Comparison of silver and molybdenum microfocus X-ray sources for single-crystal structure determination

Krause, L.; Herbst-Irmer, R.; Sheldrick, G.M.; Stalke, D.

doi:10.1107/S1600576714022985

research papers

JOURNAL OF
APPLIED
CRYSTALLOGRAPHY

ISSN: 1600-5767

Volume 48| Part 1| February 2015| Pages 3-10

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Comparison of silver and molybdenum microfocus X-ray sources for single-crystal structure determination

Lennard Krause,^a Regine Herbst-Irmer,^a George M. Sheldrick ^a and Dietmar Stalke ^a ^*

^aInstitut für Anorganische Chemie, Georg-August Universität Göttingen, Tammannstrasse 4, 37077 Göttingen, Germany
^*Correspondence e-mail: [email protected]

(Received 29 July 2014; accepted 19 October 2014)

The quality of diffraction data obtained using silver and molybdenum microsources has been compared for six model compounds with a wide range of absorption factors. The experiments were performed on two 30 W air-cooled Incoatec IµS microfocus sources with multilayer optics mounted on a Bruker D8 goniometer with a SMART APEX II CCD detector. All data were analysed, processed and refined using standard Bruker software. The results show that Ag Kα radiation can be beneficial when heavy elements are involved. A numerical absorption correction based on the positions and indices of the crystal faces is shown to be of limited use for the highly focused microsource beams, presumably because the assumption that the crystal is completely bathed in a (top-hat profile) beam of uniform intensity is no longer valid. Fortunately the empirical corrections implemented in SADABS, although originally intended as a correction for absorption, also correct rather well for the variations in the effective volume of the crystal irradiated. In three of the cases studied (two Ag and one Mo) the final SHELXL R1 against all data after application of empirical corrections implemented in SADABS was below 1%. Since such corrections are designed to optimize the agreement of the intensities of equivalent reflections with different paths through the crystal but the same Bragg 2θ angles, a further correction is required for the 2θ dependence of the absorption. For this, SADABS uses the transmission factor of a spherical crystal with a user-defined value of μr (where μ is the linear absorption coefficient and r is the effective radius of the crystal); the best results are obtained when r is biased towards the smallest crystal dimension. The results presented here suggest that the IUCr publication requirement that a numerical absorption correction must be applied for strongly absorbing crystals is in need of revision.

Keywords: microfocus X-ray sources; single-crystal structure determination; absorption correction.

CCDC references: 1029932; 1029933; 1029934; 1029935; 1029936; 1029937; 1029938; 1029939; 1029940; 1029941; 1029942; 1029943

1. Introduction

Microfocus sealed-tube X-ray sources have become standard in many laboratories because of their very low power consumption and minimal maintenance requirements (Coles & Gale, 2012 ; Schulz et al., 2009 ). Cu Kα and Mo Kα microsources are already widely used, but the more recent commercial availability of silver anode microsources raises the question as to when Ag Kα is preferable. The shorter wavelength enables a higher resolution to be achieved and results in a compressed diffraction pattern, which is particularly advantageous when the diffraction geometry is restricted, for example by a high-pressure cell (Saouane et al., 2013 ). The strength of the absorption correlates with the wavelength of the incident beam: a short wavelength is generally less prone to absorption unless it is close to an absorption edge (Hamilton, 1965 ; Becker & Coppens, 1974a ,b ). In the case of large, strongly absorbing crystals, it is possible that reduced absorption with the silver anode could more than compensate for the decrease in the absolute scattering power of the crystal (which is proportional to λ³). The question of the optimal crystal size has been investigated for weakly absorbing crystals by Görbitz (1999 ), who used a system with a sealed tube source and monochromator.

The curved mirror optics used by both Mo and Ag microsources deliver a narrow beam with a slightly anisotropic profile, making accurate sample alignment essential (Arndt, 1990 ; Coles & Hursthouse, 2004 ; Storm et al., 2004 ). The focal spot size of the beam is 110 and 90 µm for Mo Kα and Ag Kα, respectively (Hasse et al., 2010 $[Hasse, B., Wiesmann, J., Michaelsen, C., Heidorn, U., Kroth, S. & Hertlein, F. (2010). State-of-the-Art Multilayer Optics for X-ray Diffractometry. Geesthacht: Incoatec.]$ ). This highly focused beam makes a uniform homogeneous sample illumination impossible even for small crystals. In this paper, molybdenum and silver microsource data are compared for a variety of crystals with significant absorption in typical data collection situations. Although in these tests independent atom model (IAM) refinements were employed, the conclusions should also apply to data collected for charge density studies.

The SADABS program (Bruker, 2014 ) assumes that the corrected intensity is given by the product of an incident beam scale factor S(n), where n is the frame number, a diffracted beam factor P(u, v, w), where u, v and w are the direction cosines of the diffracted beam relative to crystal-fixed axes, and a spherical crystal factor Q(μr, 2θ), where μ is the linear absorption coefficient and r the effective radius of the crystal:

$[I_{{\rm corrected}} = I_{{\rm raw}}\, S(n)\, P(u,v,w)\, Q(\mu r, 2\theta). \eqno(1)]$

Similar approximations were used by Kopfmann & Huber (1968 ), North et al. (1968 ) and Huber & Kopfmann (1969 ) and in many subsequent papers and programs. There is one incident beam scale factor S(n) for each frame n, but in SADABS the values are interpolated according to the calculated rotation angle of the reflection relative to the rotation angles of the beginning and end of the frame. In addition, a restraint is applied that adjacent frames should have similar scale factors; this is essential when there are few (perhaps even zero) reflections that have their centres on a particular frame. The incident beam factor S(n) in SADABS corrects for crystal decomposition, intensity variations of the X-ray source, changes in the effective volume irradiated (possibly caused by the crystal not being accurately centred), beam inhomogeneity, and absorption by the crystal and its support. The plot of S(n) against the frame number n is a useful diagnostic (see below). The diffracted beam factor P(u, v, w) is based on spherical harmonics. Blessing (1995 ) also used spherical harmonics but applied them to both the incident and diffracted beams.

The empirical or multiscan correction involves refining the incident beam scale factors and spherical harmonic coefficients so that the intensities of equivalent reflections become more equal (Kopfmann & Huber, 1968; North et al., 1968; Blessing, 1995). This is critically dependent on there being a high multiplicity of observations involving different paths through the crystal, so in general multiple scans about different rotation axes relative to the crystal are required. In SADABS the incident beam scale factors and spherical harmonic coefficients are refined in alternate half-cycles, so that each of these full-matrix refinements is linear. This has the advantage that no starting values are required and that each half-cycle converges in one iteration. After each half-cycle the weighted mean intensity of each reflection is calculated using robust/resilient weights as described by Blessing (1997 ), and the resulting weighted mean intensities are used as observations for fitting the least-squares parameters. Several double cycles are required, but the method is robust and fast. The spherical crystal term Q(μr, 2θ) (Blessing, 1995) is applied only after the other parameters have been refined to convergence, because it has no effect on the agreement of the equivalent reflections. Since the spherical absorption factor Q(μr, 2θ) is largest at low 2θ and decreases monotonically as 2θ increases, the effect of neglecting this term would be to cause the atomic displacement parameters to become too small or even negative (Katayama, 1986 ). If the crystals faces have been indexed and their distances from a reference point in the crystal determined, a numerical absorption correction based on Gaussian integration (Busing & Levy, 1957 ) may be performed in SADABS before the refinement of the other parameters. In such a case, lower-order spherical harmonics can be used in P(u, v, w). For X-ray beams from a sealed tube source that have been shaped by slits but not focused, this procedure works well because the assumption that the crystal is completely bathed in a uniform (top-hat profile) beam is valid, and it is even possible to use it to refine the linear absorption coefficient μ. As will be shown, this approach fails for the highly focused microsource beams.

After the determination of the scaling parameters, SADABS rejects severe outliers and scales the estimated standard deviations of the intensities so that they correspond statistically to the degree of agreement between the corrected intensities of the equivalent reflections. The equation used to scale the reflection standard deviations involves two parameters, K and g, that are refined so that the weighted mean square deviation χ² is as close as possible to unity over the full range of intensities. Since there is no resolution-dependent term in this error model, plots of χ² against resolution are a particularly effective diagnostic test; in an ideal case χ² should be close to unity over the full ranges of intensity and resolution. In the work reported here, the current standard SADABS option of refining one overall g value and one K for each scan was adopted:

$[\sigma^2(I)_{\rm corrected} = [K \sigma(I)_{\rm raw}]^2 + (g I)^2. \eqno(2)]$

It should be noted that the current versions of SADABS and the programs XDS (Kabsch, 2010 ), AIMLESS (Evans & Murshudov, 2013 ) and HKL-2000 (Borek et al., 2003 ), which are very widely used for macromolecules, all use the same error model, an example of convergent evolution. This error model is justified by the fact that it results in values of χ² that are close to unity throughout the full range of intensity and resolution, except sometimes for a small rise at very low resolution that is clearly indicative of a residual systematic error. This can be seen later in Fig. 5 (see §3.1) and for many thousands of data sets processed by SADABS. It is remarkable that this is achieved by the refinement of only two parameters, K and g. However recent versions of SADABS also allow these parameters to be held fixed (e.g. at 1 and 0, respectively), refined as overall values for all scans or refined separately for each scan. Here we have adopted the default SADABS option of refining separate K values for each scan (because they may be influenced by different scan speeds etc.) but only one overall g value. This error model has been criticized by Henn & Meindl (2010 ) and Jørgensen et al. (2012 ), who, however, do not explain why they prefer to ignore the standard statistical criterion that χ² should be close to unity. A direct consequence of this error model is the characteristic shape of the Diederichs plot (Diederichs, 2010 ), a scatter plot of I/σ against log(I) for the unmerged data to assess the influence of systematic errors, shown later in Fig. 6 (§3.1), which has a limiting maximum value of I/σ given by 1/g.

2. Experimental

2.1. Test crystals

Scandium platinate, 1 (Harmening et al., 2010 ), murdochite, 2 (Dubler et al., 1983 ), sodium tungstate, 3 (Farrugia, 2007 ), and scandium cobalt carbide, 4 (Rohrmoser et al., 2007 ; Scherer et al., 2010 ; Eickerling et al., 2013 ), were used to represent inorganic compounds and minerals with medium to high absorption coefficients. Small crystals were chosen for this investigation in order to match the highly focused beams of the two microsources. Less strongly absorbing test crystals included a dibromoacridine derivative, 5 (Visscher, unpublished), and an inorganic cobalt complex, 6 (Azhakar et al., 2013 ). See Fig. 1 and Table 1 for detailed information on each sample.

Table 1
Experimental setup and sample characteristics

	Space group	Crystal dimensions (mm)	r (mm)	Source	μ (mm⁻¹)	μr	Spherical harmonics	Maximum resolution (Å)	Reflections: measured/unique
1	Pbam	0.06/0.04/0.02	0.014	Ag	65.25	0.919	8/7	0.33	88135/6527
1	Pbam	0.06/0.04/0.02	0.014	Mo	121.02	1.705	8/7	0.43	51469/3183
2	F $[m\bar 3m]$	0.12/0.11/0.09	0.049	Ag	20.50	1.009	8/7	0.31	14474/770
2	F $[m\bar 3m]$	0.12/0.11/0.09	0.049	Mo	38.25	1.876	8/7	0.43	10420/313
3	Pbca	0.03/0.05/0.11	0.021	Ag	10.16	0.214	8/7	0.40	154303/10927
3	Pbca	0.03/0.05/0.11	0.021	Mo	18.84	0.397	8/7	0.44	84934/8314
4	Immm	0.08/0.05/0.05	0.026	Ag	5.02	0.129	8/7	0.33	25448/1590
4	Immm	0.08/0.05/0.05	0.026	Mo	9.78	0.251	8/7	0.43	11127/704
5	P2₁/n	0.20/0.16/0.15	0.078	Ag	3.16	0.246	6/3	0.79	55453/3161
5	P2₁/n	0.20/0.16/0.15	0.078	Mo	5.90	0.459	6/3	0.79	35888/3130
6	P2₁/n	0.08/0.06/0.02	0.018	Ag	1.53	0.027	8/5	0.79	62614/8300
6	P2₁/n	0.08/0.06/0.02	0.018	Mo	2.87	0.051	8/5	0.79	96806/8338

Figure 1
Test crystals.

2.2. Diffractometer setup and data acquisition

All experiments were performed on Bruker SMART APEX II systems based on D8 three-circle goniometers with Incoatec microfocus X-ray sources (IµS) and Incoatec QUAZAR mirror optics (Schulz et al., 2009). The data were collected at 100 K crystal temperature (Mo source: Bruker CRYOFLEX; Ag source: Oxford Cryosystems CRYOSTREAM 700), 50 kV and 600 µA for both machines with an appropriate 0.5° ω scan strategy for the wavelength in question. Since no radiation damage to the crystals was expected, the same crystals were used to collect data successively on both diffractometers. Differences in scattering power and resolution for the two wavelengths led to differences in the data collection strategy and in the exposure times. Both diffractometers are equipped with Bruker APEX II area detectors that use Fairchild CCD6161 sensors. The only difference is the thickness of the scintillation phosphor, which results in a characteristic quantum yield of 160 e per X-ray photon for Mo Kα and 204 e per X-ray photon for Ag Kα. The detector on the Ag source uses a slightly thicker scintillation phosphor in order to compensate for the smaller gain caused by the shorter wavelength. A thicker scintillation phosphor increases the sensitivity but also increases the point spread function, which significantly broadens the reflection profiles (Gruner et al., 2002 ), as can be seen in Fig. 2.

Figure 2
Reflection profiles as recorded by the scintillation phosphor for Mo Kα (left) and Ag Kα (right). 4 × 4 binning mode was used for both sources.

2.3. Data processing

Data reduction was performed with SAINT (version 7.68A; Bruker, 2009 ) from the program package APEX2 (version 2.2012.2-0; Bruker, 2009). The SAINT data reduction program uses either a predetermined or an internally derived and refined box size for the integration steps. The dimensions of this box are expected to be primarily determined by the mosaicity of the crystal, the point spread function of the detector and, where applicable, the Kα₁/Kα₂ splitting. As the same crystals were used with both sources, no changes in mosaicity were expected. However, in order to minimize systematic errors due to imprecise or improperly determined box sizes, the box size was always determined and refined by SAINT using a standard procedure. Data were collected up to a maximum resolution (max.) that was limited either by the scattering power of the sample or by the 2θ limit of the experimental setup. These limits are roughly 0.43 and 0.31 Å for the Mo and Ag sources, respectively, and are solely due to the different wavelengths since both sources were mounted on identical goniometers. The data for each crystal were then integrated to different resolution shells (1.00, 0.83, 0.79, 0.60, 0.43 and max. Å). This was done to facilitate the detection of resolution-dependent differences.

2.4. Scaling and `absorption' corrections

SADABS (version 2014/4) was employed for the incident beam scaling, determination of the spherical harmonic coefficients, outlier rejection and determination of the error model parameters. Additional tests were required to see if the empirical absorption correction method was a suitable treatment for the highly absorbing crystals, since the numerical correction requires well defined crystal faces. It was almost impossible to index the faces of the tiny crystals of 1 and 4 reliably, so the numerical and empirical absorption corrections were compared for the crystals of 2, 3 and 5, since these were larger than the width of the beam and had high linear absorption coefficients μ. It was anticipated that the numerical absorption correction would provide the best correction and that for the empirical correction it might be difficult to estimate the effective radius r for the additional spherical crystal correction. The validation of this correction involved a stepwise increase of the μr value, followed by a comparison of the principal mean square atomic displacements of selected atoms with the values obtained by the numerical method. Satisfactory results were achieved when r was chosen so that it is biased towards the smallest crystal dimension; e.g. for a crystal with dimensions 0.1 × 0.2 × 0.3 mm and μ = 10 mm⁻¹, 0.07 mm would be a good value for r, giving 0.7 for μr.

2.5. Structure refinement

All the structures were solved by either Patterson or direct methods with SHELXS (Sheldrick, 2008 ). They were refined by full-matrix least squares against F² using SHELXL-2014/3 with the help of the SHELXle graphical user interface (Hübschle et al., 2011 ). All non-H atoms were refined with anisotropic displacement parameters (ADPs). The H atoms were set to idealized positions and refined using a riding model with their isotropic displacement parameters constrained to be 1.5 times the equivalent isotropic displacements of the atoms to which they were attached for methyl H atoms and 1.2 times for all other H atoms. The bromine/chlorine disorder in 2 was treated with EADP/EXYZ constraints in SHELXL-2014/3. In compound 6 the chlorine/bromine disorder and the rotational disorder of the tertiary butyl group attached to N1 were refined using distance and ADP restraints.

3. Results

3.1. Quality of the processed data

Table 2 shows the quality indicators after scaling and correction. For this table the data were truncated to the highest common resolution, but if the crystal diffracted further with Ag Kα than could be achieved with Mo Kα and the experimental geometry employed, these Ag Kα data are also reported. The data collection strategies were optimized for the wavelength in question, which resulted in only slightly longer total data collection times for Ag Kα. To some extent, the larger number of reflections recorded per frame for Ag Kα and the corresponding reduction in the number of different detector 2θ settings required compensates for the higher Mo Kα flux. To reduce the influence of the multiplicity on the quality indicators, the multiplicity-independent R_r.i.m. and R_p.i.m. (Weiss, 2001 ) are shown. Except for sample 6, which gave the weakest diffraction and would probably have benefited from a longer total data collection time with Ag Kα radiation, these R values and 〈I/σ〉 for the merged data are very comparable for the two sources for data to the same resolution. The broader reflection profile for Ag Kα (Fig. 2) requires the use of slightly larger integration boxes and hence involves a larger contribution from the background noise. However, this appears to have had little influence on the data from these relatively strongly diffracting crystals.

Table 2
Data quality indicators

	Source	Resolution (Å)	Completeness (%)	Multiplicity	〈I/σ〉	R_r.i.m.	R_p.i.m.	Exposure time	Unmerged I/σ limit	Reflections per second
1	Ag	0.33	97.6	13.06	27.97	0.0718	0.0181	60–120	16.4	0.18
		0.43	99.4	18.93	40.02	0.0619	0.0143		18.1	0.05
		0.83	99.8	12.88	45.42	0.0403	0.0113		21.3	0.04
	Mo	0.43	100	15.92	39.12	0.0491	0.0120	15–90	17.0	0.02
	Mo	0.83	100	14.80	40.76	0.0464	0.0125	15–90	17.8	0.07
2	Ag	0.31	99.1	18.63	81.63	0.0298	0.0061	5–60	33.6	0.23
		0.43	100	25.27	112.20	0.0255	0.0051		40.1	0.17
		0.83	100	34.14	196.24	0.0214	0.0045		56.5	0.13
	Mo	0.43	100	33.19	125.77	0.0361	0.0071	5–60	29.1	0.09
	Mo	0.83	100	30.43	127.70	0.0370	0.0084	5–60	27.6	0.04
3	Ag	0.40	99.9	14.10	48.46	0.0301	0.0072	20–120	43.9	1.06
		0.44	99.9	14.87	58.00	0.0282	0.0066		49.3	0.87
		0.83	100	25.96	105.23	0.0247	0.0049		44.8	0.01
	Mo	0.44	99.4	10.15	45.04	0.0316	0.0086	10–60	37.1	0.49
	Mo	0.83	100	15.09	81.89	0.0241	0.0062	10–60	48.1	0.02
4	Ag	0.33	83.3	13.34	61.51	0.0274	0.0059	20–60	54.9	0.11
		0.43	100	25.58	112.10	0.0247	0.0050		64.7	0.10
		0.83	100	21.39	194.77	0.0160	0.0038		82.5	0.16
	Mo	0.43	99.7	15.73	122.91	0.0208	0.0040	20–60	66.1	0.04
	Mo	0.83	100	30.71	215.43	0.0216	0.0037	20–60	56.8	0.16
5	Ag	0.79	99.8	17.49	56.22	0.0323	0.0072	10	36.1	1.28
	Ag	0.83	100	18.35	60.84	0.0312	0.0068	10	36.4	0.92
	Mo	0.79	100	11.45	63.01	0.0242	0.0067	10	44.2	0.75
	Mo	0.83	100	11.92	67.22	0.0234	0.0064	10	44.0	0.74
6	Ag	0.79	99.5	7.51	29.94	0.0407	0.0145	30–40	34.4	0.73
	Ag	0.83	99.5	7.71	33.01	0.0388	0.0136	30–40	38.0	0.68
	Mo	0.79	99.8	11.56	44.49	0.0290	0.0075	30	33.6	0.80
	Mo	0.83	99.8	12.43	49.87	0.0279	0.0070	30	34.4	0.75

Table 2 also shows the asymptotic limiting value of I/σ for infinite intensity (calculated by SADABS as 1/g from its error model) and the average number of reflections collected per second. This is calculated by dividing the total time required for the data collection by the number of reflections measured, which in most of the cases is higher for the Ag Kα data.

As shown in Fig. 3, the variations in the incident beam correction factor S(n) can be substantial, even for Ag Kα radiation. Despite this, the R_r.i.m. and R_p.i.m. values after correction (red lines in Fig. 4) are low and show little systematic variation with resolution. The corresponding values for Mo Kα (blue lines in Fig. 4) are similar at higher resolution but increase significantly at low resolutions, indicating that the empirical absorption correction is less effective at correcting for the even higher absorption with molybdenum radiation. The χ² plots for the same experiments in Fig. 5 again show a more pronounced rise at low resolutions for the molybdenum data; however, these plots also demonstrate that the corrections have been very effective for both sources, even for this highly absorbing sample. Since the error model has not been fitted as a function of the resolution, a flat curve close to a χ² of unity for the full resolution range is a particularly good validation of the quality of the corrected data. Convincing χ² plots were obtained in all the analyses reported here (see supporting information¹).

Figure 3
Incident beam scale factor S(n) and merging R_int as output by SADABS for the strongly absorbing crystal 2 with Ag Kα radiation. It should be noted that the smoothing algorithm for the R_int plots was changed in SADABS 2014/4 to make these plots more informative.

Figure 4
R_r.i.m. (upper curves) and R_p.i.m. (lower) after correction as a function of the resolution in ångström for Ag (red) and Mo (blue) for the strongly absorbing crystal 2. This figure was prepared with the XPREP (Bruker, 2014

) program.

Figure 5
χ² after applying corrections and deriving the error model for crystal 2. Ag (left) and Mo (right) radiation. χ² = mean{N∑(I − 〈I〉)²/(N − 1)∑[s.u.²(I)]} (N equivalents).

Fig. 6 shows the Diederichs plot prepared using SADABS for the Ag Kα data to 0.43 Å resolution for sample 4. A limiting value greater than 30 for I/σ at infinite intensity is regarded as good for synchrotron data and is taken to indicate that the data are relatively free from systematic errors. With the exception of the highly absorbing sample 1, the values reported here are all higher than 30.

Figure 6
Diederichs plot of I/σ against log(I) for sample 4 for Ag Kα data to 0.43 Å.

The limiting I/σ values for the unmerged data are relatively constant for the same sample and do not vary much with the resolution threshold, supporting the idea that this is a robust indication of the extent of systematic error for a given crystal and experimental arrangement. On the other hand, the mean 〈I/σ〉 values for the merged data are clearly correlated with the multiplicity, which tends to decrease at the highest resolution. For the strongly absorbing sample 2, the merging R values are lower for the Ag Kα data, but the opposite is true for the less strongly absorbing sample 6. Overall the precision of the Ag Kα and Mo Kα data is comparable.

3.2. Comparison of model quality

After the full structure refinement, the R1 value calculated using all data, the wR2 value (minimized in the full-matrix least-squares refinement) and the residual electron density Δρ were compared at both the maximum resolution achieved and the standard resolution of 0.83 Å. Δρ was calculated as the difference between the highest and lowest residual density in a weighted difference Fourier map.

For crystals 2, 3 and 5 it proved possible to index the crystal faces and compare the numerical and empirical absorption corrections. However the attempts to refine the absorption coefficient μ, although this works well for conventional sealed tube sources without focusing optics, were not satisfactory. Especially for the Ag Kα data, μ refined to unreasonably small values or even to zero. This problem may be attributed to the use of highly focused beams, the Ag Kα source having the most highly focused beam. When the numerical correction is combined with lower-order spherical harmonics (even/odd orders 4/1), the merging R values and the R1 values for the SHELXL refinement (shown in Table 3) were extremely similar to those obtained using no numerical correction but higher-order spherical harmonics (specified in Table 1) plus a spherical crystal correction Q(μr, 2θ). In both cases the incident beam term S(n) is responsible for about half the correction. It is thus debatable whether the numerical correction is justified. In practice an effective crystal radius r for the spherical correction Q(μr, 2θ) biased towards half the smallest crystal diameter gives an adequate spherical crystal correction.

Table 3
Selected quality criteria after structure refinement

	Resolution (Å)	Source	R1 (all data)	wR2	Δρ (e Å⁻³)	Data/parameter	R1†
1	0.83	Ag	0.0133	0.0283	2.64	10.64	–
	0.83	Mo	0.0216	0.0665	4.43	10.60	–
	0.43	Ag	0.0219	0.0391	7.34	71.93	–
	0.43	Mo	0.0262	0.0678	13.15	70.86	–
2	0.83	Ag	0.0170	0.0566	1.68	5.27	0.0166
	0.83	Mo	0.0138	0.0360	1.33	5.27	0.0128
	0.43	Ag	0.0201	0.0469	9.69	28.55	0.0201
	0.43	Mo	0.0196	0.0451	7.07	28.45	0.0193
3	0.83	Ag	0.0080	0.0193	0.80	11.87	0.0081
	0.83	Mo	0.0094	0.0215	0.98	11.91	0.0092
	0.44	Ag	0.0151	0.0228	4.01	79.87	0.0151
	0.44	Mo	0.0172	0.0326	5.34	79.83	0.0165
4	0.83	Ag	0.0129	0.0354	0.77	6.33	–
	0.83	Mo	0.0157	0.0408	1.21	6.33	–
	0.43	Ag	0.0099	0.0254	1.25	39.11	–
	0.43	Mo	0.0121	0.0327	1.70	39.11	–
5	0.83	Ag	0.0193	0.0470	1.21	14.62	0.0193
	0.83	Mo	0.0197	0.0491	1.34	14.52	0.0198
	0.79	Ag	0.0206	0.0488	1.47	16.94	0.0205
	0.79	Mo	0.0211	0.0541	1.37	16.77	0.0211
6	0.83	Ag	0.0237	0.0488	0.54	16.00	–
	0.83	Mo	0.0252	0.0572	0.63	16.07	–
	0.79	Ag	0.0260	0.0506	0.66	18.55	–
	0.79	Mo	0.0278	0.0593	0.65	18.64	–

†R1 values for the refined structure after application of a numerical absorption correction based on the measured crystal faces and the absorption coefficient μ calculated from the known unit-cell contents. The other R values in this table were obtained using the empirical correction.

For ten of the 12 combinations of crystal and resolution cutoff shown in Table 3, both R1 and wR2 were lower for the Ag Kα data. The residual density values show a similar trend but are not quite as decisive. The R1 and wR2 values are significantly lower for Ag (average values R1 0.0178, wR2 0.0398) than for Mo (R1 0.0197, wR2 0.0485). Thus, although the data precision (Table 2) is comparable for the two sources, the Ag data are clearly more accurate (Table 3). These low R factors (three of the R1 values for all data are below 1%) confirm that the empirical corrections have performed remarkably well, despite the unfavourable combination of highly focused beams and relatively high absorption.

For the refinement of structures 2 and 4 against data truncated to the standard (Acta Crystallographica) requirement of 0.83 Å, the data-to-parameter ratios are low (5.27 and 6.33, respectively). Since the scattering is dominated by the Pb and Br atoms in the case of 2, the O atoms cannot reliably be refined. However, with data to 0.43 Å the data-to-parameter ratio is 28.55 and there are no problems refining the O atoms. It should be standard practice to collect data to the highest possible resolution when both heavy and light atoms are present.

4. Conclusions

The empirical correction employed in SADABS performed remarkably well for strongly absorbing crystals despite the highly focused microsource beams, leading to very low R factors for the refined structures. While the precision of the corrected intensities was comparable for both Ag Kα and Mo Kα microsources, their accuracy was higher for the silver source because of the reduced absorption. For strongly absorbing crystals the Ag Kα microsource data were in general less affected by systematic errors than the Mo Kα data. The application of a numerical absorption correction did not improve the results. Clearly, the assumption that the crystal is completely bathed in a uniform X-ray beam is not valid for highly focused X-ray optics. However, when the empirical approach is used it is important to obtain a good estimate of the effective crystal radius for the correction term Q(μr, 2θ). An estimate of r biased towards half the smallest crystal diameter is an adequate approximation.

Supporting information

CCDC references: 1029932; 1029933; 1029934; 1029935; 1029936; 1029937; 1029938; 1029939; 1029940; 1029941; 1029942; 1029943

Crystal structure: contains datablocks global, 1-(Ag), 1-(Mo), 2-(Ag), 2-(Mo), 3-(Ag), 3-(Mo), 4-(Ag), 4-(Mo), 5-(Ag), 5-(Mo), 6-(Ag), 6-(Mo). DOI: https://doi.org/10.1107/S1600576714022985/aj5242sup1.cif

Structure factors: contains datablock 1-(Ag). DOI: https://doi.org/10.1107/S1600576714022985/aj52421-Agsup2.hkl

Structure factors: contains datablock 1-(Mo). DOI: https://doi.org/10.1107/S1600576714022985/aj52421-Mosup3.hkl

Structure factors: contains datablock 2-(Ag). DOI: https://doi.org/10.1107/S1600576714022985/aj52422-Agsup4.hkl

Structure factors: contains datablock 2-(Mo). DOI: https://doi.org/10.1107/S1600576714022985/aj52422-Mosup5.hkl

Structure factors: contains datablock 3-(Ag). DOI: https://doi.org/10.1107/S1600576714022985/aj52423-Agsup6.hkl

Structure factors: contains datablock 3-(Mo). DOI: https://doi.org/10.1107/S1600576714022985/aj52423-Mosup7.hkl

Structure factors: contains datablock 4-(Ag). DOI: https://doi.org/10.1107/S1600576714022985/aj52424-Agsup8.hkl

Structure factors: contains datablock 4-(Mo). DOI: https://doi.org/10.1107/S1600576714022985/aj52424-Mosup9.hkl

Structure factors: contains datablock 5-(Ag). DOI: https://doi.org/10.1107/S1600576714022985/aj52425-Agsup10.hkl

Structure factors: contains datablock 5-(Mo). DOI: https://doi.org/10.1107/S1600576714022985/aj52425-Mosup11.hkl

Structure factors: contains datablock 6-(Ag). DOI: https://doi.org/10.1107/S1600576714022985/aj52426-Agsup12.hkl

Structure factors: contains datablock 6-(Mo). DOI: https://doi.org/10.1107/S1600576714022985/aj52426-Mosup13.hkl

Supporting information file. DOI: https://doi.org/10.1107/S1600576714022985/aj5242sup14.pdf

Computing details top

For all compounds, data collection: APEX2 v2012.2. Cell refinement: SAINT V7.68A for 1-(Ag), 1-(Mo), 2-(Ag), 2-(Mo), 4-(Ag), 4-(Mo), 5-(Ag), 5-(Mo), 6-(Ag), 6-(Mo); SAINT V8.30C for 3-(Ag), 3-(Mo). Data reduction: SAINT V7.68A for 1-(Ag), 1-(Mo), 2-(Ag), 2-(Mo), 4-(Ag), 4-(Mo), 5-(Ag), 5-(Mo), 6-(Ag), 6-(Mo); SAINT V8.30C for 3-(Ag), 3-(Mo). For all compounds, program(s) used to solve structure: SHELXS2012 (Sheldrick, 2012). Program(s) used to refine structure: SHELXL2014 (Sheldrick, 2014) for 1-(Ag), 1-(Mo), 3-(Ag), 3-(Mo), 4-(Ag), 4-(Mo), 5-(Ag), 5-(Mo), 6-(Ag), 6-(Mo); SHELXL2014/7 (Sheldrick, 2014) for 2-(Ag), 2-(Mo). Molecular graphics: Mercury CSD 3.3 (Build RC5) for 2-(Ag), 2-(Mo). Software used to prepare material for publication: Mercury CSD 3.3 (Build RC5) for 2-(Ag), 2-(Mo).

1-(Ag) top

Crystal data top

Pt₇Sc₄Si₂	F(000) = 1316
M_r = 1601.65	D_x = 12.783 Mg m⁻³
Orthorhombic, Pbam	Ag Kα radiation, λ = 0.56086 Å
a = 6.462 (2) Å	Cell parameters from 9935 reflections
b = 16.147 (3) Å	θ = 2.7–57.2°
c = 3.988 (2) Å	µ = 65.26 mm⁻¹
V = 416.1 (3) Å³	T = 100 K
Z = 2	0.06 × 0.04 × 0.02 mm

Data collection top

Bruker Smart APEX II Quazar diffractometer	5353 reflections with I > 2σ(I)
Radiation source: INCOATEC Microsource	R_int = 0.072
ω scans	θ_max = 57.8°, θ_min = 2.0°
Absorption correction: multi-scan SADABS-2014/4	h = −18→19
T_min = 0.146, T_max = 0.331	k = −48→47
84931 measured reflections	l = −11→11
6207 independent reflections

Refinement top

Refinement on F²	41 parameters
Least-squares matrix: full	0 restraints
R[F² > 2σ(F²)] = 0.024	w = 1/[σ²(F_o²) + (0.0096P)² + 0.9879P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.047	(Δ/σ)_max = 0.003
S = 1.24	Δρ_max = 4.55 e Å⁻³
6207 reflections	Δρ_min = −10.52 e Å⁻³

Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Pt01	0.5000	0.5000	0.0000	0.00274 (1)
Pt02	−0.09659 (2)	0.42139 (2)	−1.0000	0.00290 (1)
Pt03	0.59273 (2)	0.38255 (2)	−0.5000	0.00266 (1)
Pt04	0.28692 (2)	0.33330 (2)	−1.0000	0.00293 (1)
Sc01	0.21412 (6)	0.46091 (2)	−0.5000	0.00351 (4)
Sc02	0.97516 (6)	0.29091 (2)	−0.5000	0.00361 (4)
Si1	0.66076 (12)	0.30680 (5)	−1.0000	0.00353 (8)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Pt01	0.00268 (2)	0.00287 (2)	0.00266 (3)	0.00033 (2)	0.000	0.000
Pt02	0.00243 (2)	0.00299 (2)	0.00330 (2)	−0.00010 (1)	0.000	0.000
Pt03	0.00256 (2)	0.00294 (2)	0.00246 (2)	0.00014 (1)	0.000	0.000
Pt04	0.00238 (2)	0.00307 (2)	0.00332 (2)	0.00001 (1)	0.000	0.000
Sc01	0.00302 (9)	0.00355 (9)	0.00395 (10)	0.00011 (7)	0.000	0.000
Sc02	0.00364 (9)	0.00333 (9)	0.00385 (10)	0.00027 (7)	0.000	0.000
Si1	0.00361 (18)	0.00386 (18)	0.00313 (19)	−0.00025 (14)	0.000	0.000

Geometric parameters (Å, º) top

Pt01—Sc01	2.7906 (9)	Pt04—Si1^xi	2.4046 (9)
Pt01—Sc01ⁱ	2.7906 (9)	Pt04—Si1	2.4533 (11)
Pt01—Sc01ⁱⁱ	2.7906 (9)	Pt04—Sc01^ix	2.9057 (8)
Pt01—Sc01ⁱⁱⁱ	2.7906 (9)	Pt04—Sc01	2.9057 (8)
Pt01—Pt03	2.8164 (7)	Pt04—Sc02^viii	2.9160 (9)
Pt01—Pt03ⁱ	2.8164 (7)	Pt04—Sc02^vi	2.9160 (9)
Pt01—Pt03ⁱⁱⁱ	2.8164 (7)	Pt04—Pt03^ix	2.9178 (8)
Pt01—Pt03ⁱⁱ	2.8164 (7)	Pt04—Pt01^ix	3.0234 (5)
Pt01—Pt02^iv	2.8994 (7)	Pt04—Sc02^xii	3.0786 (8)
Pt01—Pt02^v	2.8994 (7)	Pt04—Sc02^xi	3.0786 (8)
Pt01—Pt04ⁱⁱⁱ	3.0235 (5)	Sc01—Pt01^ix	2.7906 (9)
Pt01—Pt04ⁱⁱ	3.0235 (5)	Sc01—Pt03ⁱⁱ	2.8191 (6)
Pt02—Si1^vi	2.4253 (9)	Sc01—Pt02^v	2.8574 (8)
Pt02—Pt02^vii	2.8289 (5)	Sc01—Pt02^vii	2.8574 (8)
Pt02—Sc01^v	2.8574 (8)	Sc01—Pt02ⁱⁱⁱ	2.9008 (9)
Pt02—Sc01^vii	2.8574 (8)	Sc01—Pt04ⁱⁱⁱ	2.9057 (8)
Pt02—Pt04	2.8575 (7)	Sc01—Sc01^v	3.0416 (11)
Pt02—Pt03^viii	2.8983 (8)	Sc01—Sc02^vi	3.1495 (7)
Pt02—Pt03^vi	2.8983 (8)	Sc02—Si1^xiii	2.8113 (10)
Pt02—Pt01^viii	2.8994 (7)	Sc02—Si1^xiv	2.8113 (10)
Pt02—Sc01^ix	2.9007 (9)	Sc02—Si1	2.8582 (10)
Pt02—Sc01	2.9008 (9)	Sc02—Si1ⁱⁱⁱ	2.8582 (10)
Pt02—Sc02^viii	2.9377 (8)	Sc02—Pt03^xiii	2.9020 (6)
Pt02—Sc02^vi	2.9377 (8)	Sc02—Pt04^iv	2.9160 (9)
Pt03—Si1ⁱⁱⁱ	2.3802 (9)	Sc02—Pt04^x	2.9160 (9)
Pt03—Si1	2.3802 (9)	Sc02—Pt02^iv	2.9377 (8)
Pt03—Sc01	2.7544 (8)	Sc02—Pt02^x	2.9377 (8)
Pt03—Pt01^ix	2.8164 (8)	Sc02—Pt04^xiii	3.0786 (8)
Pt03—Sc01ⁱⁱ	2.8192 (6)	Sc02—Pt04^xiv	3.0786 (8)
Pt03—Sc02	2.8804 (8)	Si1—Pt03^ix	2.3802 (9)
Pt03—Pt02^iv	2.8983 (8)	Si1—Pt04^xiii	2.4046 (9)
Pt03—Pt02^x	2.8983 (8)	Si1—Pt02^x	2.4254 (9)
Pt03—Sc02^xi	2.9020 (6)	Si1—Sc02^xii	2.8113 (10)
Pt03—Pt04	2.9178 (8)	Si1—Sc02^xi	2.8113 (10)
Pt03—Pt04ⁱⁱⁱ	2.9178 (8)	Si1—Sc02^ix	2.8582 (10)

Sc01—Pt01—Sc01ⁱ	180.0	Sc01^ix—Pt04—Sc02^vi	121.59 (2)
Sc01—Pt01—Sc01ⁱⁱ	88.79 (3)	Sc01—Pt04—Sc02^vi	65.50 (2)
Sc01ⁱ—Pt01—Sc01ⁱⁱ	91.21 (4)	Sc02^viii—Pt04—Sc02^vi	86.28 (3)
Sc01—Pt01—Sc01ⁱⁱⁱ	91.21 (3)	Si1^xi—Pt04—Pt03	119.079 (15)
Sc01ⁱ—Pt01—Sc01ⁱⁱⁱ	88.79 (4)	Si1—Pt04—Pt03	51.731 (17)
Sc01ⁱⁱ—Pt01—Sc01ⁱⁱⁱ	180.000 (15)	Pt02—Pt04—Pt03	116.855 (15)
Sc01—Pt01—Pt03	58.84 (2)	Sc01^ix—Pt04—Pt03	112.67 (2)
Sc01ⁱ—Pt01—Pt03	121.16 (2)	Sc01—Pt04—Pt03	56.456 (19)
Sc01ⁱⁱ—Pt01—Pt03	60.368 (19)	Sc02^viii—Pt04—Pt03	177.698 (8)
Sc01ⁱⁱⁱ—Pt01—Pt03	119.632 (19)	Sc02^vi—Pt04—Pt03	93.70 (3)
Sc01—Pt01—Pt03ⁱ	121.16 (2)	Si1^xi—Pt04—Pt03^ix	119.079 (14)
Sc01ⁱ—Pt01—Pt03ⁱ	58.84 (2)	Si1—Pt04—Pt03^ix	51.731 (17)
Sc01ⁱⁱ—Pt01—Pt03ⁱ	119.632 (19)	Pt02—Pt04—Pt03^ix	116.855 (15)
Sc01ⁱⁱⁱ—Pt01—Pt03ⁱ	60.368 (19)	Sc01^ix—Pt04—Pt03^ix	56.46 (2)
Pt03—Pt01—Pt03ⁱ	180.0	Sc01—Pt04—Pt03^ix	112.67 (2)
Sc01—Pt01—Pt03ⁱⁱⁱ	119.632 (19)	Sc02^viii—Pt04—Pt03^ix	93.70 (3)
Sc01ⁱ—Pt01—Pt03ⁱⁱⁱ	60.37 (2)	Sc02^vi—Pt04—Pt03^ix	177.698 (8)
Sc01ⁱⁱ—Pt01—Pt03ⁱⁱⁱ	121.16 (2)	Pt03—Pt04—Pt03^ix	86.22 (3)
Sc01ⁱⁱⁱ—Pt01—Pt03ⁱⁱⁱ	58.84 (2)	Si1^xi—Pt04—Pt01^ix	172.727 (19)
Pt03—Pt01—Pt03ⁱⁱⁱ	90.15 (3)	Si1—Pt04—Pt01^ix	72.95 (2)
Pt03ⁱ—Pt01—Pt03ⁱⁱⁱ	89.85 (3)	Pt02—Pt04—Pt01^ix	87.237 (18)
Sc01—Pt01—Pt03ⁱⁱ	60.37 (2)	Sc01^ix—Pt04—Pt01^ix	56.112 (14)
Sc01ⁱ—Pt01—Pt03ⁱⁱ	119.632 (19)	Sc01—Pt04—Pt01^ix	56.111 (15)
Sc01ⁱⁱ—Pt01—Pt03ⁱⁱ	58.84 (2)	Sc02^viii—Pt04—Pt01^ix	121.575 (12)
Sc01ⁱⁱⁱ—Pt01—Pt03ⁱⁱ	121.16 (2)	Sc02^vi—Pt04—Pt01^ix	121.575 (13)
Pt03—Pt01—Pt03ⁱⁱ	89.85 (3)	Pt03—Pt04—Pt01^ix	56.560 (10)
Pt03ⁱ—Pt01—Pt03ⁱⁱ	90.15 (3)	Pt03^ix—Pt04—Pt01^ix	56.560 (10)
Pt03ⁱⁱⁱ—Pt01—Pt03ⁱⁱ	180.0	Si1^xi—Pt04—Sc02^xii	61.386 (19)
Sc01—Pt01—Pt02^iv	119.748 (17)	Si1—Pt04—Sc02^xii	59.823 (16)
Sc01ⁱ—Pt01—Pt02^iv	60.252 (17)	Pt02—Pt04—Sc02^xii	131.833 (14)
Sc01ⁱⁱ—Pt01—Pt02^iv	60.252 (17)	Sc01^ix—Pt04—Sc02^xii	94.67 (3)
Sc01ⁱⁱⁱ—Pt01—Pt02^iv	119.748 (17)	Sc01—Pt04—Sc02^xii	166.026 (12)
Pt03—Pt01—Pt02^iv	60.917 (9)	Sc02^viii—Pt04—Sc02^xii	71.16 (2)
Pt03ⁱ—Pt01—Pt02^iv	119.083 (9)	Sc02^vi—Pt04—Sc02^xii	124.259 (17)
Pt03ⁱⁱⁱ—Pt01—Pt02^iv	60.917 (9)	Pt03—Pt04—Sc02^xii	110.65 (2)
Pt03ⁱⁱ—Pt01—Pt02^iv	119.083 (9)	Pt03^ix—Pt04—Sc02^xii	57.813 (18)
Sc01—Pt01—Pt02^v	60.252 (17)	Pt01^ix—Pt04—Sc02^xii	113.581 (16)
Sc01ⁱ—Pt01—Pt02^v	119.748 (17)	Si1^xi—Pt04—Sc02^xi	61.386 (19)
Sc01ⁱⁱ—Pt01—Pt02^v	119.748 (17)	Si1—Pt04—Sc02^xi	59.823 (16)
Sc01ⁱⁱⁱ—Pt01—Pt02^v	60.252 (17)	Pt02—Pt04—Sc02^xi	131.833 (14)
Pt03—Pt01—Pt02^v	119.083 (9)	Sc01^ix—Pt04—Sc02^xi	166.027 (12)
Pt03ⁱ—Pt01—Pt02^v	60.917 (9)	Sc01—Pt04—Sc02^xi	94.67 (3)
Pt03ⁱⁱⁱ—Pt01—Pt02^v	119.083 (9)	Sc02^viii—Pt04—Sc02^xi	124.260 (16)
Pt03ⁱⁱ—Pt01—Pt02^v	60.917 (9)	Sc02^vi—Pt04—Sc02^xi	71.16 (2)
Pt02^iv—Pt01—Pt02^v	180.0	Pt03—Pt04—Sc02^xi	57.813 (19)
Sc01—Pt01—Pt04ⁱⁱⁱ	59.811 (12)	Pt03^ix—Pt04—Sc02^xi	110.65 (2)
Sc01ⁱ—Pt01—Pt04ⁱⁱⁱ	120.190 (13)	Pt01^ix—Pt04—Sc02^xi	113.581 (16)
Sc01ⁱⁱ—Pt01—Pt04ⁱⁱⁱ	120.190 (13)	Sc02^xii—Pt04—Sc02^xi	80.74 (3)
Sc01ⁱⁱⁱ—Pt01—Pt04ⁱⁱⁱ	59.810 (13)	Pt03—Sc01—Pt01	61.045 (16)
Pt03—Pt01—Pt04ⁱⁱⁱ	59.826 (13)	Pt03—Sc01—Pt01^ix	61.045 (16)
Pt03ⁱ—Pt01—Pt04ⁱⁱⁱ	120.174 (13)	Pt01—Sc01—Pt01^ix	91.21 (3)
Pt03ⁱⁱⁱ—Pt01—Pt04ⁱⁱⁱ	59.826 (13)	Pt03—Sc01—Pt03ⁱⁱ	91.07 (2)
Pt03ⁱⁱ—Pt01—Pt04ⁱⁱⁱ	120.174 (13)	Pt01—Sc01—Pt03ⁱⁱ	60.269 (12)
Pt02^iv—Pt01—Pt04ⁱⁱⁱ	91.129 (17)	Pt01^ix—Sc01—Pt03ⁱⁱ	60.269 (12)
Pt02^v—Pt01—Pt04ⁱⁱⁱ	88.871 (17)	Pt03—Sc01—Pt02^v	122.793 (14)
Sc01—Pt01—Pt04ⁱⁱ	120.189 (12)	Pt01—Sc01—Pt02^v	61.76 (2)
Sc01ⁱ—Pt01—Pt04ⁱⁱ	59.810 (13)	Pt01^ix—Sc01—Pt02^v	121.61 (2)
Sc01ⁱⁱ—Pt01—Pt04ⁱⁱ	59.810 (13)	Pt03ⁱⁱ—Sc01—Pt02^v	61.400 (15)
Sc01ⁱⁱⁱ—Pt01—Pt04ⁱⁱ	120.190 (13)	Pt03—Sc01—Pt02^vii	122.793 (14)
Pt03—Pt01—Pt04ⁱⁱ	120.174 (13)	Pt01—Sc01—Pt02^vii	121.61 (2)
Pt03ⁱ—Pt01—Pt04ⁱⁱ	59.826 (13)	Pt01^ix—Sc01—Pt02^vii	61.76 (2)
Pt03ⁱⁱⁱ—Pt01—Pt04ⁱⁱ	120.174 (13)	Pt03ⁱⁱ—Sc01—Pt02^vii	61.400 (15)
Pt03ⁱⁱ—Pt01—Pt04ⁱⁱ	59.826 (13)	Pt02^v—Sc01—Pt02^vii	88.51 (3)
Pt02^iv—Pt01—Pt04ⁱⁱ	88.871 (17)	Pt03—Sc01—Pt02	120.915 (17)
Pt02^v—Pt01—Pt04ⁱⁱ	91.129 (17)	Pt01—Sc01—Pt02	177.648 (12)
Pt04ⁱⁱⁱ—Pt01—Pt04ⁱⁱ	180.0	Pt01^ix—Sc01—Pt02	90.96 (3)
Si1^vi—Pt02—Pt02^vii	165.908 (19)	Pt03ⁱⁱ—Sc01—Pt02	120.244 (13)
Si1^vi—Pt02—Sc01^v	109.610 (19)	Pt02^v—Sc01—Pt02	116.23 (2)
Pt02^vii—Pt02—Sc01^v	61.343 (15)	Pt02^vii—Sc01—Pt02	58.845 (18)
Si1^vi—Pt02—Sc01^vii	109.61 (2)	Pt03—Sc01—Pt02ⁱⁱⁱ	120.916 (17)
Pt02^vii—Pt02—Sc01^vii	61.343 (15)	Pt01—Sc01—Pt02ⁱⁱⁱ	90.96 (3)
Sc01^v—Pt02—Sc01^vii	88.51 (3)	Pt01^ix—Sc01—Pt02ⁱⁱⁱ	177.648 (12)
Si1^vi—Pt02—Pt04	100.42 (3)	Pt03ⁱⁱ—Sc01—Pt02ⁱⁱⁱ	120.244 (13)
Pt02^vii—Pt02—Pt04	93.667 (17)	Pt02^v—Sc01—Pt02ⁱⁱⁱ	58.844 (18)
Sc01^v—Pt02—Pt04	124.166 (13)	Pt02^vii—Sc01—Pt02ⁱⁱⁱ	116.23 (2)
Sc01^vii—Pt02—Pt04	124.166 (13)	Pt02—Sc01—Pt02ⁱⁱⁱ	86.85 (3)
Si1^vi—Pt02—Pt03^viii	52.198 (16)	Pt03—Sc01—Pt04	61.993 (11)
Pt02^vii—Pt02—Pt03^viii	119.993 (10)	Pt01—Sc01—Pt04	122.93 (2)
Sc01^v—Pt02—Pt03^viii	116.10 (2)	Pt01^ix—Sc01—Pt04	64.078 (19)
Sc01^vii—Pt02—Pt03^viii	58.650 (19)	Pt03ⁱⁱ—Sc01—Pt04	124.343 (16)
Pt04—Pt02—Pt03^viii	119.540 (15)	Pt02^v—Sc01—Pt04	173.500 (16)
Si1^vi—Pt02—Pt03^vi	52.198 (16)	Pt02^vii—Sc01—Pt04	92.05 (3)
Pt02^vii—Pt02—Pt03^vi	119.993 (10)	Pt02—Sc01—Pt04	58.960 (19)
Sc01^v—Pt02—Pt03^vi	58.650 (19)	Pt02ⁱⁱⁱ—Sc01—Pt04	115.33 (2)
Sc01^vii—Pt02—Pt03^vi	116.10 (2)	Pt03—Sc01—Pt04ⁱⁱⁱ	61.993 (11)
Pt04—Pt02—Pt03^vi	119.540 (15)	Pt01—Sc01—Pt04ⁱⁱⁱ	64.078 (19)
Pt03^viii—Pt02—Pt03^vi	86.94 (3)	Pt01^ix—Sc01—Pt04ⁱⁱⁱ	122.93 (2)
Si1^vi—Pt02—Pt01^viii	75.68 (3)	Pt03ⁱⁱ—Sc01—Pt04ⁱⁱⁱ	124.343 (16)
Pt02^vii—Pt02—Pt01^viii	90.225 (17)	Pt02^v—Sc01—Pt04ⁱⁱⁱ	92.05 (3)
Sc01^v—Pt02—Pt01^viii	57.986 (12)	Pt02^vii—Sc01—Pt04ⁱⁱⁱ	173.500 (16)
Sc01^vii—Pt02—Pt01^viii	57.986 (12)	Pt02—Sc01—Pt04ⁱⁱⁱ	115.33 (2)
Pt04—Pt02—Pt01^viii	176.108 (4)	Pt02ⁱⁱⁱ—Sc01—Pt04ⁱⁱⁱ	58.961 (19)
Pt03^viii—Pt02—Pt01^viii	58.127 (15)	Pt04—Sc01—Pt04ⁱⁱⁱ	86.67 (3)
Pt03^vi—Pt02—Pt01^viii	58.127 (15)	Pt03—Sc01—Sc01^v	177.18 (2)
Si1^vi—Pt02—Sc01^ix	127.973 (17)	Pt01—Sc01—Sc01^v	120.558 (19)
Pt02^vii—Pt02—Sc01^ix	59.812 (12)	Pt01^ix—Sc01—Sc01^v	120.558 (19)
Sc01^v—Pt02—Sc01^ix	121.155 (18)	Pt03ⁱⁱ—Sc01—Sc01^v	91.76 (2)
Sc01^vii—Pt02—Sc01^ix	63.77 (2)	Pt02^v—Sc01—Sc01^v	58.811 (13)
Pt04—Pt02—Sc01^ix	60.606 (17)	Pt02^vii—Sc01—Sc01^v	58.811 (13)
Pt03^viii—Pt02—Sc01^ix	93.10 (3)	Pt02—Sc01—Sc01^v	57.424 (18)
Pt03^vi—Pt02—Sc01^ix	179.792 (8)	Pt02ⁱⁱⁱ—Sc01—Sc01^v	57.423 (18)
Pt01^viii—Pt02—Sc01^ix	121.737 (17)	Pt04—Sc01—Sc01^v	116.209 (15)
Si1^vi—Pt02—Sc01	127.974 (17)	Pt04ⁱⁱⁱ—Sc01—Sc01^v	116.209 (16)
Pt02^vii—Pt02—Sc01	59.812 (12)	Pt03—Sc01—Sc02^vi	92.01 (2)
Sc01^v—Pt02—Sc01	63.77 (2)	Pt01—Sc01—Sc02^vi	121.447 (14)
Sc01^vii—Pt02—Sc01	121.155 (18)	Pt01^ix—Sc01—Sc02^vi	121.447 (14)
Pt04—Pt02—Sc01	60.606 (17)	Pt03ⁱⁱ—Sc01—Sc02^vi	176.921 (17)
Pt03^viii—Pt02—Sc01	179.792 (8)	Pt02^v—Sc01—Sc02^vi	116.704 (17)
Pt03^vi—Pt02—Sc01	93.10 (3)	Pt02^vii—Sc01—Sc02^vi	116.704 (17)
Pt01^viii—Pt02—Sc01	121.737 (17)	Pt02—Sc01—Sc02^vi	57.922 (14)
Sc01^ix—Pt02—Sc01	86.85 (3)	Pt02ⁱⁱⁱ—Sc01—Sc02^vi	57.923 (13)
Si1^vi—Pt02—Sc02^viii	63.569 (19)	Pt04—Sc01—Sc02^vi	57.408 (15)
Pt02^vii—Pt02—Sc02^viii	125.025 (15)	Pt04ⁱⁱⁱ—Sc01—Sc02^vi	57.407 (15)
Sc01^v—Pt02—Sc02^viii	173.043 (12)	Sc01^v—Sc01—Sc02^vi	85.16 (2)
Sc01^vii—Pt02—Sc02^viii	92.60 (3)	Si1^xiii—Sc02—Si1^xiv	90.35 (4)
Pt04—Pt02—Sc02^viii	60.403 (12)	Si1^xiii—Sc02—Si1	81.88 (3)
Pt03^viii—Pt02—Sc02^viii	59.14 (2)	Si1^xiv—Sc02—Si1	148.04 (2)
Pt03^vi—Pt02—Sc02^viii	114.90 (2)	Si1^xiii—Sc02—Si1ⁱⁱⁱ	148.04 (2)
Pt01^viii—Pt02—Sc02^viii	117.121 (11)	Si1^xiv—Sc02—Si1ⁱⁱⁱ	81.88 (3)
Sc01^ix—Pt02—Sc02^viii	65.29 (2)	Si1—Sc02—Si1ⁱⁱⁱ	88.48 (4)
Sc01—Pt02—Sc02^viii	121.00 (2)	Si1^xiii—Sc02—Pt03	130.87 (2)
Si1^vi—Pt02—Sc02^vi	63.569 (19)	Si1^xiv—Sc02—Pt03	130.87 (2)
Pt02^vii—Pt02—Sc02^vi	125.025 (15)	Si1—Sc02—Pt03	49.01 (2)
Sc01^v—Pt02—Sc02^vi	92.60 (3)	Si1ⁱⁱⁱ—Sc02—Pt03	49.01 (2)
Sc01^vii—Pt02—Sc02^vi	173.043 (12)	Si1^xiii—Sc02—Pt03^xiii	49.209 (19)
Pt04—Pt02—Sc02^vi	60.403 (12)	Si1^xiv—Sc02—Pt03^xiii	49.209 (18)
Pt03^viii—Pt02—Sc02^vi	114.90 (2)	Si1—Sc02—Pt03^xiii	105.827 (19)
Pt03^vi—Pt02—Sc02^vi	59.14 (2)	Si1ⁱⁱⁱ—Sc02—Pt03^xiii	105.828 (19)
Pt01^viii—Pt02—Sc02^vi	117.121 (11)	Pt03—Sc02—Pt03^xiii	136.088 (15)
Sc01^ix—Pt02—Sc02^vi	121.00 (2)	Si1^xiii—Sc02—Pt04^iv	108.78 (3)
Sc01—Pt02—Sc02^vi	65.29 (2)	Si1^xiv—Sc02—Pt04^iv	49.61 (2)
Sc02^viii—Pt02—Sc02^vi	85.49 (3)	Si1—Sc02—Pt04^iv	161.27 (2)
Si1ⁱⁱⁱ—Pt03—Si1	113.81 (4)	Si1ⁱⁱⁱ—Sc02—Pt04^iv	89.60 (3)
Si1ⁱⁱⁱ—Pt03—Sc01	113.59 (2)	Pt03—Sc02—Pt04^iv	118.175 (18)
Si1—Pt03—Sc01	113.59 (2)	Pt03^xiii—Sc02—Pt04^iv	92.617 (13)
Si1ⁱⁱⁱ—Pt03—Pt01	78.01 (3)	Si1^xiii—Sc02—Pt04^x	49.61 (2)
Si1—Pt03—Pt01	168.088 (16)	Si1^xiv—Sc02—Pt04^x	108.78 (3)
Sc01—Pt03—Pt01	60.111 (10)	Si1—Sc02—Pt04^x	89.60 (3)
Si1ⁱⁱⁱ—Pt03—Pt01^ix	168.087 (16)	Si1ⁱⁱⁱ—Sc02—Pt04^x	161.27 (2)
Si1—Pt03—Pt01^ix	78.01 (3)	Pt03—Sc02—Pt04^x	118.175 (18)
Sc01—Pt03—Pt01^ix	60.111 (10)	Pt03^xiii—Sc02—Pt04^x	92.617 (13)
Pt01—Pt03—Pt01^ix	90.15 (3)	Pt04^iv—Sc02—Pt04^x	86.28 (3)
Si1ⁱⁱⁱ—Pt03—Sc01ⁱⁱ	112.27 (2)	Si1^xiii—Sc02—Pt02^iv	162.03 (2)
Si1—Pt03—Sc01ⁱⁱ	112.27 (2)	Si1^xiv—Sc02—Pt02^iv	89.34 (3)
Sc01—Pt03—Sc01ⁱⁱ	88.93 (2)	Si1—Sc02—Pt02^iv	107.27 (3)
Pt01—Pt03—Sc01ⁱⁱ	59.363 (14)	Si1ⁱⁱⁱ—Sc02—Pt02^iv	49.45 (2)
Pt01^ix—Pt03—Sc01ⁱⁱ	59.363 (13)	Pt03—Sc02—Pt02^iv	59.745 (12)
Si1ⁱⁱⁱ—Pt03—Sc02	65.01 (2)	Pt03^xiii—Sc02—Pt02^iv	137.182 (16)
Si1—Pt03—Sc02	65.01 (2)	Pt04^iv—Sc02—Pt02^iv	58.437 (18)
Sc01—Pt03—Sc02	176.435 (11)	Pt04^x—Sc02—Pt02^iv	113.88 (2)
Pt01—Pt03—Sc02	121.902 (11)	Si1^xiii—Sc02—Pt02^x	89.34 (3)
Pt01^ix—Pt03—Sc02	121.902 (11)	Si1^xiv—Sc02—Pt02^x	162.03 (2)
Sc01ⁱⁱ—Pt03—Sc02	94.63 (2)	Si1—Sc02—Pt02^x	49.45 (2)
Si1ⁱⁱⁱ—Pt03—Pt02^iv	53.62 (2)	Si1ⁱⁱⁱ—Sc02—Pt02^x	107.27 (3)
Si1—Pt03—Pt02^iv	124.03 (3)	Pt03—Sc02—Pt02^x	59.745 (11)
Sc01—Pt03—Pt02^iv	121.054 (16)	Pt03^xiii—Sc02—Pt02^x	137.182 (16)
Pt01—Pt03—Pt02^iv	60.96 (2)	Pt04^iv—Sc02—Pt02^x	113.88 (2)
Pt01^ix—Pt03—Pt02^iv	119.257 (18)	Pt04^x—Sc02—Pt02^x	58.437 (19)
Sc01ⁱⁱ—Pt03—Pt02^iv	59.950 (11)	Pt02^iv—Sc02—Pt02^x	85.49 (3)
Sc02—Pt03—Pt02^iv	61.111 (16)	Si1^xiii—Sc02—Pt04^xiii	48.97 (2)
Si1ⁱⁱⁱ—Pt03—Pt02^x	124.03 (3)	Si1^xiv—Sc02—Pt04^xiii	105.21 (3)
Si1—Pt03—Pt02^x	53.62 (2)	Si1—Sc02—Pt04^xiii	47.61 (2)
Sc01—Pt03—Pt02^x	121.054 (16)	Si1ⁱⁱⁱ—Sc02—Pt04^xiii	103.27 (3)
Pt01—Pt03—Pt02^x	119.257 (18)	Pt03—Sc02—Pt04^xiii	89.752 (17)
Pt01^ix—Pt03—Pt02^x	60.96 (2)	Pt03^xiii—Sc02—Pt04^xiii	58.312 (14)
Sc01ⁱⁱ—Pt03—Pt02^x	59.950 (11)	Pt04^iv—Sc02—Pt04^xiii	150.317 (16)
Sc02—Pt03—Pt02^x	61.111 (16)	Pt04^x—Sc02—Pt04^xiii	89.02 (3)
Pt02^iv—Pt03—Pt02^x	86.94 (3)	Pt02^iv—Sc02—Pt04^xiii	147.617 (19)
Si1ⁱⁱⁱ—Pt03—Sc02^xi	63.41 (2)	Pt02^x—Sc02—Pt04^xiii	88.01 (3)
Si1—Pt03—Sc02^xi	63.41 (2)	Si1^xiii—Sc02—Pt04^xiv	105.21 (3)
Sc01—Pt03—Sc02^xi	102.170 (18)	Si1^xiv—Sc02—Pt04^xiv	48.97 (2)
Pt01—Pt03—Sc02^xi	126.456 (13)	Si1—Sc02—Pt04^xiv	103.27 (3)
Pt01^ix—Pt03—Sc02^xi	126.456 (13)	Si1ⁱⁱⁱ—Sc02—Pt04^xiv	47.61 (2)
Sc01ⁱⁱ—Pt03—Sc02^xi	168.896 (12)	Pt03—Sc02—Pt04^xiv	89.752 (17)
Sc02—Pt03—Sc02^xi	74.265 (16)	Pt03^xiii—Sc02—Pt04^xiv	58.312 (14)
Pt02^iv—Pt03—Sc02^xi	112.969 (9)	Pt04^iv—Sc02—Pt04^xiv	89.02 (3)
Pt02^x—Pt03—Sc02^xi	112.969 (9)	Pt04^x—Sc02—Pt04^xiv	150.317 (16)
Si1ⁱⁱⁱ—Pt03—Pt04	123.89 (3)	Pt02^iv—Sc02—Pt04^xiv	88.01 (3)
Si1—Pt03—Pt04	54.02 (3)	Pt02^x—Sc02—Pt04^xiv	147.617 (19)
Sc01—Pt03—Pt04	61.551 (16)	Pt04^xiii—Sc02—Pt04^xiv	80.74 (3)
Pt01—Pt03—Pt04	121.55 (2)	Pt03^ix—Si1—Pt03	113.81 (4)
Pt01^ix—Pt03—Pt04	63.614 (18)	Pt03^ix—Si1—Pt04^xiii	123.10 (2)
Sc01ⁱⁱ—Pt03—Pt04	122.972 (11)	Pt03—Si1—Pt04^xiii	123.10 (2)
Sc02—Pt03—Pt04	116.172 (16)	Pt03^ix—Si1—Pt02^x	74.18 (2)
Pt02^iv—Pt03—Pt04	176.656 (4)	Pt03—Si1—Pt02^x	74.18 (2)
Pt02^x—Pt03—Pt04	93.32 (3)	Pt04^xiii—Si1—Pt02^x	119.90 (4)
Sc02^xi—Pt03—Pt04	63.875 (9)	Pt03^ix—Si1—Pt04	74.25 (2)
Si1ⁱⁱⁱ—Pt03—Pt04ⁱⁱⁱ	54.02 (3)	Pt03—Si1—Pt04	74.25 (2)
Si1—Pt03—Pt04ⁱⁱⁱ	123.89 (3)	Pt04^xiii—Si1—Pt04	119.86 (3)
Sc01—Pt03—Pt04ⁱⁱⁱ	61.551 (17)	Pt02^x—Si1—Pt04	120.23 (3)
Pt01—Pt03—Pt04ⁱⁱⁱ	63.614 (19)	Pt03^ix—Si1—Sc02^xii	67.38 (3)
Pt01^ix—Pt03—Pt04ⁱⁱⁱ	121.55 (2)	Pt03—Si1—Sc02^xii	143.49 (4)
Sc01ⁱⁱ—Pt03—Pt04ⁱⁱⁱ	122.973 (11)	Pt04^xiii—Si1—Sc02^xii	67.46 (2)
Sc02—Pt03—Pt04ⁱⁱⁱ	116.171 (16)	Pt02^x—Si1—Sc02^xii	134.74 (2)
Pt02^iv—Pt03—Pt04ⁱⁱⁱ	93.32 (3)	Pt04—Si1—Sc02^xii	71.20 (2)
Pt02^x—Pt03—Pt04ⁱⁱⁱ	176.655 (4)	Pt03^ix—Si1—Sc02^xi	143.49 (4)
Sc02^xi—Pt03—Pt04ⁱⁱⁱ	63.874 (9)	Pt03—Si1—Sc02^xi	67.38 (3)
Pt04—Pt03—Pt04ⁱⁱⁱ	86.22 (3)	Pt04^xiii—Si1—Sc02^xi	67.46 (2)
Si1^xi—Pt04—Si1	99.77 (2)	Pt02^x—Si1—Sc02^xi	134.74 (2)
Si1^xi—Pt04—Pt02	100.04 (2)	Pt04—Si1—Sc02^xi	71.20 (2)
Si1—Pt04—Pt02	160.191 (19)	Sc02^xii—Si1—Sc02^xi	90.35 (4)
Si1^xi—Pt04—Sc01^ix	127.750 (17)	Pt03^ix—Si1—Sc02^ix	65.98 (3)
Si1—Pt04—Sc01^ix	106.447 (15)	Pt03—Si1—Sc02^ix	139.63 (3)
Pt02—Pt04—Sc01^ix	60.433 (12)	Pt04^xiii—Si1—Sc02^ix	71.01 (2)
Si1^xi—Pt04—Sc01	127.750 (17)	Pt02^x—Si1—Sc02^ix	66.98 (2)
Si1—Pt04—Sc01	106.447 (15)	Pt04—Si1—Sc02^ix	135.69 (2)
Pt02—Pt04—Sc01	60.434 (11)	Sc02^xii—Si1—Sc02^ix	76.00 (3)
Sc01^ix—Pt04—Sc01	86.67 (3)	Sc02^xi—Si1—Sc02^ix	138.39 (3)
Si1^xi—Pt04—Sc02^viii	62.931 (16)	Pt03^ix—Si1—Sc02	139.63 (3)
Si1—Pt04—Sc02^viii	129.743 (18)	Pt03—Si1—Sc02	65.98 (3)
Pt02—Pt04—Sc02^viii	61.161 (17)	Pt04^xiii—Si1—Sc02	71.01 (2)
Sc01^ix—Pt04—Sc02^viii	65.50 (2)	Pt02^x—Si1—Sc02	66.98 (2)
Sc01—Pt04—Sc02^viii	121.59 (2)	Pt04—Si1—Sc02	135.69 (2)
Si1^xi—Pt04—Sc02^vi	62.931 (16)	Sc02^xii—Si1—Sc02	138.39 (3)
Si1—Pt04—Sc02^vi	129.743 (18)	Sc02^xi—Si1—Sc02	76.00 (3)
Pt02—Pt04—Sc02^vi	61.161 (17)	Sc02^ix—Si1—Sc02	88.48 (4)

Symmetry codes: (i) −x+1, −y+1, −z; (ii) −x+1, −y+1, −z−1; (iii) x, y, z+1; (iv) x+1, y, z+1; (v) −x, −y+1, −z−1; (vi) x−1, y, z; (vii) −x, −y+1, −z−2; (viii) x−1, y, z−1; (ix) x, y, z−1; (x) x+1, y, z; (xi) x−1/2, −y+1/2, z; (xii) x−1/2, −y+1/2, z−1; (xiii) x+1/2, −y+1/2, z; (xiv) x+1/2, −y+1/2, z+1.

1-(Mo) top

Crystal data top

Pt₇Sc₄Si₂	F(000) = 1316
M_r = 1601.65	D_x = 12.853 Mg m⁻³
Orthorhombic, Pbam	Mo Kα radiation, λ = 0.71073 Å
a = 6.447 (2) Å	Cell parameters from 9937 reflections
b = 16.121 (3) Å	θ = 2.5–55.8°
c = 3.982 (2) Å	µ = 121.04 mm⁻¹
V = 413.9 (3) Å³	T = 100 K
Z = 2	0.06 × 0.04 × 0.02 mm

Data collection top

Bruker Smart APEX II Quazar diffractometer	2933 reflections with I > 2σ(I)
Radiation source: INCOATEC Microsource	R_int = 0.047
ω scans	θ_max = 56.1°, θ_min = 2.5°
Absorption correction: multi-scan SADABS-2014/4	h = −13→15
T_min = 0.040, T_max = 0.176	k = −37→37
48679 measured reflections	l = −9→8
2976 independent reflections

Refinement top

Refinement on F²	0 restraints
Least-squares matrix: full	w = 1/[σ²(F_o²) + (0.0265P)² + 6.503P] where P = (F_o² + 2F_c²)/3
R[F² > 2σ(F²)] = 0.026	(Δ/σ)_max = 0.001
wR(F²) = 0.068	Δρ_max = 8.77 e Å⁻³
S = 1.29	Δρ_min = −4.38 e Å⁻³
2976 reflections	Extinction correction: SHELXL, Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
42 parameters	Extinction coefficient: 0.00051 (8)

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Pt4	0.59272 (2)	0.38257 (2)	0.5000	0.00442 (3)
Pt3	0.28687 (2)	0.33332 (2)	0.0000	0.00475 (3)
Pt1	−0.09655 (2)	0.42142 (2)	0.0000	0.00467 (3)
Pt2	0.5000	0.5000	1.0000	0.00450 (3)
Sc2	0.97528 (12)	0.29097 (5)	0.5000	0.00528 (8)
Sc1	0.21425 (12)	0.46092 (5)	0.5000	0.00532 (9)
Si1	0.6605 (2)	0.30686 (9)	0.0000	0.00506 (16)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Pt4	0.00328 (4)	0.00504 (5)	0.00492 (4)	0.00017 (3)	0.000	0.000
Pt3	0.00314 (4)	0.00531 (5)	0.00580 (5)	0.00005 (3)	0.000	0.000
Pt1	0.00313 (4)	0.00510 (5)	0.00578 (5)	−0.00012 (3)	0.000	0.000
Pt2	0.00332 (5)	0.00505 (6)	0.00514 (6)	0.00038 (4)	0.000	0.000
Sc2	0.0048 (2)	0.00506 (19)	0.0060 (2)	0.00031 (16)	0.000	0.000
Sc1	0.00358 (18)	0.0064 (2)	0.0060 (2)	0.00005 (16)	0.000	0.000
Si1	0.0040 (4)	0.0059 (4)	0.0053 (4)	−0.0008 (3)	0.000	0.000

Geometric parameters (Å, º) top

Pt4—Si1ⁱ	2.3759 (12)	Pt2—Sc1ⁱⁱⁱ	2.7847 (10)
Pt4—Si1	2.3759 (12)	Pt2—Sc1ⁱ	2.7847 (10)
Pt4—Sc1	2.7475 (10)	Pt2—Sc1	2.7847 (10)
Pt4—Pt2	2.8117 (8)	Pt2—Pt4^xii	2.8116 (8)
Pt4—Pt2ⁱⁱ	2.8117 (8)	Pt2—Pt4ⁱⁱⁱ	2.8116 (8)
Pt4—Sc1ⁱⁱⁱ	2.8133 (9)	Pt2—Pt4ⁱ	2.8116 (8)
Pt4—Sc2	2.8746 (10)	Pt2—Pt1^iv	2.8931 (7)
Pt4—Pt1^iv	2.8930 (8)	Pt2—Pt1^xi	2.8931 (7)
Pt4—Pt1^v	2.8930 (8)	Pt2—Pt3ⁱⁱⁱ	3.0181 (5)
Pt4—Sc2^vi	2.8982 (10)	Pt2—Pt3ⁱ	3.0181 (5)
Pt4—Pt3	2.9125 (8)	Sc2—Si1^xiii	2.8068 (14)
Pt4—Pt3ⁱ	2.9125 (8)	Sc2—Si1^xiv	2.8068 (14)
Pt3—Si1^vi	2.4021 (15)	Sc2—Si1ⁱ	2.8543 (14)
Pt3—Si1	2.4465 (16)	Sc2—Si1	2.8543 (14)
Pt3—Pt1	2.8509 (7)	Sc2—Pt4^xiii	2.8983 (10)
Pt3—Sc1	2.9008 (9)	Sc2—Pt3^iv	2.9096 (10)
Pt3—Sc1ⁱⁱ	2.9009 (9)	Sc2—Pt3^v	2.9096 (10)
Pt3—Sc2^vii	2.9096 (10)	Sc2—Pt1^iv	2.9327 (9)
Pt3—Sc2^viii	2.9096 (10)	Sc2—Pt1^v	2.9327 (9)
Pt3—Pt4ⁱⁱ	2.9125 (8)	Sc2—Pt3^xiii	3.0747 (9)
Pt3—Pt2ⁱⁱ	3.0180 (5)	Sc2—Pt3^xiv	3.0747 (9)
Pt3—Sc2^ix	3.0747 (9)	Sc1—Pt2ⁱⁱ	2.7847 (10)
Pt3—Sc2^vi	3.0747 (9)	Sc1—Pt4ⁱⁱⁱ	2.8133 (9)
Pt1—Si1^viii	2.4213 (15)	Sc1—Pt1^xi	2.8527 (9)
Pt1—Pt1^x	2.8230 (6)	Sc1—Pt1^x	2.8527 (9)
Pt1—Sc1^xi	2.8527 (9)	Sc1—Pt1ⁱ	2.8956 (10)
Pt1—Sc1^x	2.8527 (9)	Sc1—Pt3ⁱ	2.9009 (9)
Pt1—Pt4^vii	2.8930 (8)	Sc1—Sc1^xi	3.0364 (17)
Pt1—Pt4^viii	2.8930 (8)	Sc1—Sc2^viii	3.1432 (12)
Pt1—Pt2^vii	2.8931 (8)	Si1—Pt4ⁱⁱ	2.3759 (12)
Pt1—Sc1	2.8956 (10)	Si1—Pt3^xiii	2.4020 (15)
Pt1—Sc1ⁱⁱ	2.8956 (10)	Si1—Pt1^v	2.4214 (15)
Pt1—Sc2^vii	2.9327 (9)	Si1—Sc2^ix	2.8068 (14)
Pt1—Sc2^viii	2.9327 (9)	Si1—Sc2^vi	2.8068 (14)
Pt2—Sc1^xii	2.7847 (10)	Si1—Sc2ⁱⁱ	2.8543 (14)

Si1ⁱ—Pt4—Si1	113.86 (7)	Sc1—Pt2—Pt4ⁱ	119.64 (2)
Si1ⁱ—Pt4—Sc1	113.55 (3)	Pt4^xii—Pt2—Pt4ⁱ	89.83 (3)
Si1—Pt4—Sc1	113.55 (3)	Pt4ⁱⁱⁱ—Pt2—Pt4ⁱ	180.0
Si1ⁱ—Pt4—Pt2	77.97 (4)	Sc1^xii—Pt2—Pt4	121.20 (2)
Si1—Pt4—Pt2	168.07 (3)	Sc1ⁱⁱⁱ—Pt2—Pt4	60.36 (2)
Sc1—Pt4—Pt2	60.109 (13)	Sc1ⁱ—Pt2—Pt4	119.64 (2)
Si1ⁱ—Pt4—Pt2ⁱⁱ	168.07 (3)	Sc1—Pt2—Pt4	58.80 (2)
Si1—Pt4—Pt2ⁱⁱ	77.97 (4)	Pt4^xii—Pt2—Pt4	180.0
Sc1—Pt4—Pt2ⁱⁱ	60.109 (13)	Pt4ⁱⁱⁱ—Pt2—Pt4	89.83 (3)
Pt2—Pt4—Pt2ⁱⁱ	90.16 (3)	Pt4ⁱ—Pt2—Pt4	90.17 (3)
Si1ⁱ—Pt4—Sc1ⁱⁱⁱ	112.29 (3)	Sc1^xii—Pt2—Pt1^iv	60.28 (2)
Si1—Pt4—Sc1ⁱⁱⁱ	112.29 (3)	Sc1ⁱⁱⁱ—Pt2—Pt1^iv	60.28 (2)
Sc1—Pt4—Sc1ⁱⁱⁱ	88.88 (3)	Sc1ⁱ—Pt2—Pt1^iv	119.72 (2)
Pt2—Pt4—Sc1ⁱⁱⁱ	59.348 (16)	Sc1—Pt2—Pt1^iv	119.71 (2)
Pt2ⁱⁱ—Pt4—Sc1ⁱⁱⁱ	59.348 (16)	Pt4^xii—Pt2—Pt1^iv	119.076 (9)
Si1ⁱ—Pt4—Sc2	65.05 (3)	Pt4ⁱⁱⁱ—Pt2—Pt1^iv	119.076 (9)
Si1—Pt4—Sc2	65.05 (3)	Pt4ⁱ—Pt2—Pt1^iv	60.924 (9)
Sc1—Pt4—Sc2	176.46 (2)	Pt4—Pt2—Pt1^iv	60.924 (10)
Pt2—Pt4—Sc2	121.889 (14)	Sc1^xii—Pt2—Pt1^xi	119.72 (2)
Pt2ⁱⁱ—Pt4—Sc2	121.889 (14)	Sc1ⁱⁱⁱ—Pt2—Pt1^xi	119.72 (2)
Sc1ⁱⁱⁱ—Pt4—Sc2	94.66 (3)	Sc1ⁱ—Pt2—Pt1^xi	60.28 (2)
Si1ⁱ—Pt4—Pt1^iv	53.63 (4)	Sc1—Pt2—Pt1^xi	60.29 (2)
Si1—Pt4—Pt1^iv	124.09 (4)	Pt4^xii—Pt2—Pt1^xi	60.924 (10)
Sc1—Pt4—Pt1^iv	121.025 (19)	Pt4ⁱⁱⁱ—Pt2—Pt1^xi	60.924 (10)
Pt2—Pt4—Pt1^iv	60.93 (2)	Pt4ⁱ—Pt2—Pt1^xi	119.076 (9)
Pt2ⁱⁱ—Pt4—Pt1^iv	119.261 (19)	Pt4—Pt2—Pt1^xi	119.076 (9)
Sc1ⁱⁱⁱ—Pt4—Pt1^iv	59.970 (14)	Pt1^iv—Pt2—Pt1^xi	180.0
Sc2—Pt4—Pt1^iv	61.124 (18)	Sc1^xii—Pt2—Pt3ⁱⁱⁱ	59.828 (18)
Si1ⁱ—Pt4—Pt1^v	124.09 (4)	Sc1ⁱⁱⁱ—Pt2—Pt3ⁱⁱⁱ	59.828 (18)
Si1—Pt4—Pt1^v	53.63 (4)	Sc1ⁱ—Pt2—Pt3ⁱⁱⁱ	120.172 (18)
Sc1—Pt4—Pt1^v	121.025 (19)	Sc1—Pt2—Pt3ⁱⁱⁱ	120.173 (18)
Pt2—Pt4—Pt1^v	119.261 (19)	Pt4^xii—Pt2—Pt3ⁱⁱⁱ	59.821 (12)
Pt2ⁱⁱ—Pt4—Pt1^v	60.93 (2)	Pt4ⁱⁱⁱ—Pt2—Pt3ⁱⁱⁱ	59.821 (13)
Sc1ⁱⁱⁱ—Pt4—Pt1^v	59.970 (14)	Pt4ⁱ—Pt2—Pt3ⁱⁱⁱ	120.179 (13)
Sc2—Pt4—Pt1^v	61.124 (18)	Pt4—Pt2—Pt3ⁱⁱⁱ	120.179 (13)
Pt1^iv—Pt4—Pt1^v	86.98 (3)	Pt1^iv—Pt2—Pt3ⁱⁱⁱ	88.886 (18)
Si1ⁱ—Pt4—Sc2^vi	63.40 (3)	Pt1^xi—Pt2—Pt3ⁱⁱⁱ	91.114 (17)
Si1—Pt4—Sc2^vi	63.40 (3)	Sc1^xii—Pt2—Pt3ⁱ	120.172 (18)
Sc1—Pt4—Sc2^vi	102.23 (3)	Sc1ⁱⁱⁱ—Pt2—Pt3ⁱ	120.172 (18)
Pt2—Pt4—Sc2^vi	126.470 (15)	Sc1ⁱ—Pt2—Pt3ⁱ	59.828 (18)
Pt2ⁱⁱ—Pt4—Sc2^vi	126.470 (15)	Sc1—Pt2—Pt3ⁱ	59.827 (18)
Sc1ⁱⁱⁱ—Pt4—Sc2^vi	168.89 (2)	Pt4^xii—Pt2—Pt3ⁱ	120.179 (13)
Sc2—Pt4—Sc2^vi	74.234 (19)	Pt4ⁱⁱⁱ—Pt2—Pt3ⁱ	120.179 (13)
Pt1^iv—Pt4—Sc2^vi	112.946 (13)	Pt4ⁱ—Pt2—Pt3ⁱ	59.821 (12)
Pt1^v—Pt4—Sc2^vi	112.946 (13)	Pt4—Pt2—Pt3ⁱ	59.821 (13)
Si1ⁱ—Pt4—Pt3	123.88 (4)	Pt1^iv—Pt2—Pt3ⁱ	91.114 (17)
Si1—Pt4—Pt3	53.96 (4)	Pt1^xi—Pt2—Pt3ⁱ	88.886 (17)
Sc1—Pt4—Pt3	61.582 (19)	Pt3ⁱⁱⁱ—Pt2—Pt3ⁱ	180.0
Pt2—Pt4—Pt3	121.58 (2)	Si1^xiii—Sc2—Si1^xiv	90.36 (6)
Pt2ⁱⁱ—Pt4—Pt3	63.611 (19)	Si1^xiii—Sc2—Si1ⁱ	147.97 (4)
Sc1ⁱⁱⁱ—Pt4—Pt3	122.953 (14)	Si1^xiv—Sc2—Si1ⁱ	81.84 (4)
Sc2—Pt4—Pt3	116.157 (19)	Si1^xiii—Sc2—Si1	81.84 (4)
Pt1^iv—Pt4—Pt3	176.655 (7)	Si1^xiv—Sc2—Si1	147.97 (4)
Pt1^v—Pt4—Pt3	93.29 (3)	Si1ⁱ—Sc2—Si1	88.46 (6)
Sc2^vi—Pt4—Pt3	63.896 (13)	Si1^xiii—Sc2—Pt4	130.82 (3)
Si1ⁱ—Pt4—Pt3ⁱ	53.96 (4)	Si1^xiv—Sc2—Pt4	130.82 (3)
Si1—Pt4—Pt3ⁱ	123.88 (4)	Si1ⁱ—Sc2—Pt4	49.00 (3)
Sc1—Pt4—Pt3ⁱ	61.583 (19)	Si1—Sc2—Pt4	49.00 (3)
Pt2—Pt4—Pt3ⁱ	63.612 (19)	Si1^xiii—Sc2—Pt4^xiii	49.19 (3)
Pt2ⁱⁱ—Pt4—Pt3ⁱ	121.58 (2)	Si1^xiv—Sc2—Pt4^xiii	49.19 (3)
Sc1ⁱⁱⁱ—Pt4—Pt3ⁱ	122.954 (14)	Si1ⁱ—Sc2—Pt4^xiii	105.80 (4)
Sc2—Pt4—Pt3ⁱ	116.157 (19)	Si1—Sc2—Pt4^xiii	105.80 (4)
Pt1^iv—Pt4—Pt3ⁱ	93.29 (3)	Pt4—Sc2—Pt4^xiii	136.05 (3)
Pt1^v—Pt4—Pt3ⁱ	176.653 (7)	Si1^xiii—Sc2—Pt3^iv	108.87 (4)
Sc2^vi—Pt4—Pt3ⁱ	63.895 (13)	Si1^xiv—Sc2—Pt3^iv	49.66 (3)
Pt3—Pt4—Pt3ⁱ	86.25 (3)	Si1ⁱ—Sc2—Pt3^iv	89.57 (4)
Si1^vi—Pt3—Si1	99.78 (4)	Si1—Sc2—Pt3^iv	161.28 (4)
Si1^vi—Pt3—Pt1	100.06 (4)	Pt4—Sc2—Pt3^iv	118.16 (3)
Si1—Pt3—Pt1	160.16 (4)	Pt4^xiii—Sc2—Pt3^iv	92.64 (2)
Si1^vi—Pt3—Sc1	127.76 (3)	Si1^xiii—Sc2—Pt3^v	49.66 (3)
Si1—Pt3—Sc1	106.41 (3)	Si1^xiv—Sc2—Pt3^v	108.87 (4)
Pt1—Pt3—Sc1	60.448 (17)	Si1ⁱ—Sc2—Pt3^v	161.28 (4)
Si1^vi—Pt3—Sc1ⁱⁱ	127.76 (3)	Si1—Sc2—Pt3^v	89.57 (4)
Si1—Pt3—Sc1ⁱⁱ	106.41 (3)	Pt4—Sc2—Pt3^v	118.16 (3)
Pt1—Pt3—Sc1ⁱⁱ	60.448 (17)	Pt4^xiii—Sc2—Pt3^v	92.64 (2)
Sc1—Pt3—Sc1ⁱⁱ	86.68 (4)	Pt3^iv—Sc2—Pt3^v	86.36 (4)
Si1^vi—Pt3—Sc2^vii	62.95 (3)	Si1^xiii—Sc2—Pt1^iv	162.12 (4)
Si1—Pt3—Sc2^vii	129.71 (3)	Si1^xiv—Sc2—Pt1^iv	89.34 (4)
Pt1—Pt3—Sc2^vii	61.20 (2)	Si1ⁱ—Sc2—Pt1^iv	49.45 (3)
Sc1—Pt3—Sc2^vii	121.64 (3)	Si1—Sc2—Pt1^iv	107.28 (4)
Sc1ⁱⁱ—Pt3—Sc2^vii	65.50 (3)	Pt4—Sc2—Pt1^iv	59.747 (17)
Si1^vi—Pt3—Sc2^viii	62.95 (3)	Pt4^xiii—Sc2—Pt1^iv	137.173 (18)
Si1—Pt3—Sc2^viii	129.71 (3)	Pt3^iv—Sc2—Pt1^iv	58.41 (2)
Pt1—Pt3—Sc2^viii	61.20 (2)	Pt3^v—Sc2—Pt1^iv	113.91 (3)
Sc1—Pt3—Sc2^viii	65.50 (3)	Si1^xiii—Sc2—Pt1^v	89.34 (4)
Sc1ⁱⁱ—Pt3—Sc2^viii	121.64 (3)	Si1^xiv—Sc2—Pt1^v	162.12 (4)
Sc2^vii—Pt3—Sc2^viii	86.36 (4)	Si1ⁱ—Sc2—Pt1^v	107.27 (4)
Si1^vi—Pt3—Pt4	119.08 (2)	Si1—Sc2—Pt1^v	49.45 (3)
Si1—Pt3—Pt4	51.75 (2)	Pt4—Sc2—Pt1^v	59.747 (17)
Pt1—Pt3—Pt4	116.822 (16)	Pt4^xiii—Sc2—Pt1^v	137.173 (18)
Sc1—Pt3—Pt4	56.41 (2)	Pt3^iv—Sc2—Pt1^v	113.91 (3)
Sc1ⁱⁱ—Pt3—Pt4	112.65 (2)	Pt3^v—Sc2—Pt1^v	58.41 (2)
Sc2^vii—Pt3—Pt4	177.692 (17)	Pt1^iv—Sc2—Pt1^v	85.51 (4)
Sc2^viii—Pt3—Pt4	93.65 (3)	Si1^xiii—Sc2—Pt3^xiii	48.90 (3)
Si1^vi—Pt3—Pt4ⁱⁱ	119.08 (2)	Si1^xiv—Sc2—Pt3^xiii	105.15 (4)
Si1—Pt3—Pt4ⁱⁱ	51.75 (2)	Si1ⁱ—Sc2—Pt3^xiii	103.26 (4)
Pt1—Pt3—Pt4ⁱⁱ	116.821 (16)	Si1—Sc2—Pt3^xiii	47.62 (3)
Sc1—Pt3—Pt4ⁱⁱ	112.65 (2)	Pt4—Sc2—Pt3^xiii	89.76 (2)
Sc1ⁱⁱ—Pt3—Pt4ⁱⁱ	56.41 (2)	Pt4^xiii—Sc2—Pt3^xiii	58.278 (18)
Sc2^vii—Pt3—Pt4ⁱⁱ	93.65 (3)	Pt3^iv—Sc2—Pt3^xiii	150.31 (3)
Sc2^viii—Pt3—Pt4ⁱⁱ	177.691 (17)	Pt3^v—Sc2—Pt3^xiii	89.00 (3)
Pt4—Pt3—Pt4ⁱⁱ	86.25 (3)	Pt1^iv—Sc2—Pt3^xiii	147.62 (3)
Si1^vi—Pt3—Pt2ⁱⁱ	172.74 (3)	Pt1^v—Sc2—Pt3^xiii	88.01 (3)
Si1—Pt3—Pt2ⁱⁱ	72.96 (4)	Si1^xiii—Sc2—Pt3^xiv	105.15 (4)
Pt1—Pt3—Pt2ⁱⁱ	87.203 (18)	Si1^xiv—Sc2—Pt3^xiv	48.90 (3)
Sc1—Pt3—Pt2ⁱⁱ	56.089 (19)	Si1ⁱ—Sc2—Pt3^xiv	47.62 (3)
Sc1ⁱⁱ—Pt3—Pt2ⁱⁱ	56.088 (19)	Si1—Sc2—Pt3^xiv	103.26 (4)
Sc2^vii—Pt3—Pt2ⁱⁱ	121.550 (17)	Pt4—Sc2—Pt3^xiv	89.76 (2)
Sc2^viii—Pt3—Pt2ⁱⁱ	121.550 (18)	Pt4^xiii—Sc2—Pt3^xiv	58.278 (18)
Pt4—Pt3—Pt2ⁱⁱ	56.568 (11)	Pt3^iv—Sc2—Pt3^xiv	89.00 (3)
Pt4ⁱⁱ—Pt3—Pt2ⁱⁱ	56.568 (11)	Pt3^v—Sc2—Pt3^xiv	150.31 (3)
Si1^vi—Pt3—Sc2^ix	61.37 (3)	Pt1^iv—Sc2—Pt3^xiv	88.01 (3)
Si1—Pt3—Sc2^ix	59.83 (3)	Pt1^v—Sc2—Pt3^xiv	147.62 (3)
Pt1—Pt3—Sc2^ix	131.849 (17)	Pt3^xiii—Sc2—Pt3^xiv	80.71 (4)
Sc1—Pt3—Sc2^ix	166.00 (2)	Pt4—Sc1—Pt2	61.09 (2)
Sc1ⁱⁱ—Pt3—Sc2^ix	94.67 (3)	Pt4—Sc1—Pt2ⁱⁱ	61.09 (2)
Sc2^vii—Pt3—Sc2^ix	71.14 (3)	Pt2—Sc1—Pt2ⁱⁱ	91.28 (4)
Sc2^viii—Pt3—Sc2^ix	124.261 (19)	Pt4—Sc1—Pt4ⁱⁱⁱ	91.12 (3)
Pt4—Pt3—Sc2^ix	110.66 (3)	Pt2—Sc1—Pt4ⁱⁱⁱ	60.296 (18)
Pt4ⁱⁱ—Pt3—Sc2^ix	57.83 (2)	Pt2ⁱⁱ—Sc1—Pt4ⁱⁱⁱ	60.296 (18)
Pt2ⁱⁱ—Pt3—Sc2^ix	113.60 (2)	Pt4—Sc1—Pt1^xi	122.81 (2)
Si1^vi—Pt3—Sc2^vi	61.37 (3)	Pt2—Sc1—Pt1^xi	61.74 (2)
Si1—Pt3—Sc2^vi	59.83 (3)	Pt2ⁱⁱ—Sc1—Pt1^xi	121.64 (3)
Pt1—Pt3—Sc2^vi	131.849 (17)	Pt4ⁱⁱⁱ—Sc1—Pt1^xi	61.40 (2)
Sc1—Pt3—Sc2^vi	94.67 (3)	Pt4—Sc1—Pt1^x	122.81 (2)
Sc1ⁱⁱ—Pt3—Sc2^vi	166.00 (2)	Pt2—Sc1—Pt1^x	121.64 (3)
Sc2^vii—Pt3—Sc2^vi	124.261 (19)	Pt2ⁱⁱ—Sc1—Pt1^x	61.74 (2)
Sc2^viii—Pt3—Sc2^vi	71.14 (3)	Pt4ⁱⁱⁱ—Sc1—Pt1^x	61.40 (2)
Pt4—Pt3—Sc2^vi	57.83 (2)	Pt1^xi—Sc1—Pt1^x	88.52 (4)
Pt4ⁱⁱ—Pt3—Sc2^vi	110.66 (3)	Pt4—Sc1—Pt1	120.89 (2)
Pt2ⁱⁱ—Pt3—Sc2^vi	113.60 (2)	Pt2—Sc1—Pt1	177.63 (2)
Sc2^ix—Pt3—Sc2^vi	80.71 (4)	Pt2ⁱⁱ—Sc1—Pt1	90.91 (3)
Si1^viii—Pt1—Pt1^x	165.87 (4)	Pt4ⁱⁱⁱ—Sc1—Pt1	120.22 (2)
Si1^viii—Pt1—Pt3	100.42 (4)	Pt1^xi—Sc1—Pt1	116.23 (3)
Pt1^x—Pt1—Pt3	93.713 (19)	Pt1^x—Sc1—Pt1	58.82 (2)
Si1^viii—Pt1—Sc1^xi	109.58 (3)	Pt4—Sc1—Pt1ⁱ	120.89 (3)
Pt1^x—Pt1—Sc1^xi	61.35 (2)	Pt2—Sc1—Pt1ⁱ	90.91 (3)
Pt3—Pt1—Sc1^xi	124.188 (18)	Pt2ⁱⁱ—Sc1—Pt1ⁱ	177.63 (2)
Si1^viii—Pt1—Sc1^x	109.58 (3)	Pt4ⁱⁱⁱ—Sc1—Pt1ⁱ	120.22 (2)
Pt1^x—Pt1—Sc1^x	61.35 (2)	Pt1^xi—Sc1—Pt1ⁱ	58.82 (2)
Pt3—Pt1—Sc1^x	124.188 (18)	Pt1^x—Sc1—Pt1ⁱ	116.23 (3)
Sc1^xi—Pt1—Sc1^x	88.52 (4)	Pt1—Sc1—Pt1ⁱ	86.88 (4)
Si1^viii—Pt1—Pt4^vii	52.20 (2)	Pt4—Sc1—Pt3	62.009 (17)
Pt1^x—Pt1—Pt4^vii	119.978 (11)	Pt2—Sc1—Pt3	122.98 (3)
Pt3—Pt1—Pt4^vii	119.509 (16)	Pt2ⁱⁱ—Sc1—Pt3	64.08 (2)
Sc1^xi—Pt1—Pt4^vii	116.11 (3)	Pt4ⁱⁱⁱ—Sc1—Pt3	124.37 (2)
Sc1^x—Pt1—Pt4^vii	58.63 (2)	Pt1^xi—Sc1—Pt3	173.46 (3)
Si1^viii—Pt1—Pt4^viii	52.20 (2)	Pt1^x—Sc1—Pt3	92.03 (3)
Pt1^x—Pt1—Pt4^viii	119.978 (11)	Pt1—Sc1—Pt3	58.92 (2)
Pt3—Pt1—Pt4^viii	119.509 (16)	Pt1ⁱ—Sc1—Pt3	115.32 (3)
Sc1^xi—Pt1—Pt4^viii	58.63 (2)	Pt4—Sc1—Pt3ⁱ	62.008 (17)
Sc1^x—Pt1—Pt4^viii	116.11 (3)	Pt2—Sc1—Pt3ⁱ	64.08 (2)
Pt4^vii—Pt1—Pt4^viii	86.98 (3)	Pt2ⁱⁱ—Sc1—Pt3ⁱ	122.98 (3)
Si1^viii—Pt1—Pt2^vii	75.67 (4)	Pt4ⁱⁱⁱ—Sc1—Pt3ⁱ	124.38 (2)
Pt1^x—Pt1—Pt2^vii	90.199 (18)	Pt1^xi—Sc1—Pt3ⁱ	92.03 (3)
Pt3—Pt1—Pt2^vii	176.088 (7)	Pt1^x—Sc1—Pt3ⁱ	173.46 (3)
Sc1^xi—Pt1—Pt2^vii	57.974 (17)	Pt1—Sc1—Pt3ⁱ	115.32 (3)
Sc1^x—Pt1—Pt2^vii	57.974 (17)	Pt1ⁱ—Sc1—Pt3ⁱ	58.92 (2)
Pt4^vii—Pt1—Pt2^vii	58.146 (16)	Pt3—Sc1—Pt3ⁱ	86.68 (4)
Pt4^viii—Pt1—Pt2^vii	58.146 (16)	Pt4—Sc1—Sc1^xi	177.15 (5)
Si1^viii—Pt1—Sc1	127.97 (3)	Pt2—Sc1—Sc1^xi	120.53 (3)
Pt1^x—Pt1—Sc1	59.831 (18)	Pt2ⁱⁱ—Sc1—Sc1^xi	120.53 (3)
Pt3—Pt1—Sc1	60.63 (2)	Pt4ⁱⁱⁱ—Sc1—Sc1^xi	91.74 (4)
Sc1^xi—Pt1—Sc1	63.77 (3)	Pt1^xi—Sc1—Sc1^xi	58.81 (2)
Sc1^x—Pt1—Sc1	121.181 (19)	Pt1^x—Sc1—Sc1^xi	58.81 (2)
Pt4^vii—Pt1—Sc1	179.798 (17)	Pt1—Sc1—Sc1^xi	57.43 (2)
Pt4^viii—Pt1—Sc1	93.07 (3)	Pt1ⁱ—Sc1—Sc1^xi	57.43 (2)
Pt2^vii—Pt1—Sc1	121.72 (2)	Pt3—Sc1—Sc1^xi	116.17 (3)
Si1^viii—Pt1—Sc1ⁱⁱ	127.97 (2)	Pt3ⁱ—Sc1—Sc1^xi	116.17 (3)
Pt1^x—Pt1—Sc1ⁱⁱ	59.830 (18)	Pt4—Sc1—Sc2^viii	91.98 (3)
Pt3—Pt1—Sc1ⁱⁱ	60.63 (2)	Pt2—Sc1—Sc2^viii	121.43 (2)
Sc1^xi—Pt1—Sc1ⁱⁱ	121.18 (2)	Pt2ⁱⁱ—Sc1—Sc2^viii	121.43 (2)
Sc1^x—Pt1—Sc1ⁱⁱ	63.76 (3)	Pt4ⁱⁱⁱ—Sc1—Sc2^viii	176.90 (3)
Pt4^vii—Pt1—Sc1ⁱⁱ	93.07 (3)	Pt1^xi—Sc1—Sc2^viii	116.69 (3)
Pt4^viii—Pt1—Sc1ⁱⁱ	179.797 (17)	Pt1^x—Sc1—Sc2^viii	116.69 (3)
Pt2^vii—Pt1—Sc1ⁱⁱ	121.72 (2)	Pt1—Sc1—Sc2^viii	57.94 (2)
Sc1—Pt1—Sc1ⁱⁱ	86.88 (4)	Pt1ⁱ—Sc1—Sc2^viii	57.94 (2)
Si1^viii—Pt1—Sc2^vii	63.59 (3)	Pt3—Sc1—Sc2^viii	57.38 (2)
Pt1^x—Pt1—Sc2^vii	125.02 (2)	Pt3ⁱ—Sc1—Sc2^viii	57.38 (2)
Pt3—Pt1—Sc2^vii	60.387 (17)	Sc1^xi—Sc1—Sc2^viii	85.17 (4)
Sc1^xi—Pt1—Sc2^vii	173.03 (2)	Pt4—Si1—Pt4ⁱⁱ	113.86 (7)
Sc1^x—Pt1—Sc2^vii	92.58 (3)	Pt4—Si1—Pt3^xiii	123.07 (3)
Pt4^vii—Pt1—Sc2^vii	59.13 (2)	Pt4ⁱⁱ—Si1—Pt3^xiii	123.07 (3)
Pt4^viii—Pt1—Sc2^vii	114.92 (2)	Pt4—Si1—Pt1^v	74.17 (4)
Pt2^vii—Pt1—Sc2^vii	117.126 (17)	Pt4ⁱⁱ—Si1—Pt1^v	74.17 (4)
Sc1—Pt1—Sc2^vii	121.01 (3)	Pt3^xiii—Si1—Pt1^v	119.88 (6)
Sc1ⁱⁱ—Pt1—Sc2^vii	65.27 (3)	Pt4—Si1—Pt3	74.29 (4)
Si1^viii—Pt1—Sc2^viii	63.59 (3)	Pt4ⁱⁱ—Si1—Pt3	74.29 (4)
Pt1^x—Pt1—Sc2^viii	125.02 (2)	Pt3^xiii—Si1—Pt3	119.86 (6)
Pt3—Pt1—Sc2^viii	60.387 (17)	Pt1^v—Si1—Pt3	120.26 (6)
Sc1^xi—Pt1—Sc2^viii	92.58 (3)	Pt4—Si1—Sc2^ix	143.59 (6)
Sc1^x—Pt1—Sc2^viii	173.03 (2)	Pt4ⁱⁱ—Si1—Sc2^ix	67.41 (3)
Pt4^vii—Pt1—Sc2^viii	114.92 (2)	Pt3^xiii—Si1—Sc2^ix	67.40 (4)
Pt4^viii—Pt1—Sc2^viii	59.13 (2)	Pt1^v—Si1—Sc2^ix	134.73 (3)
Pt2^vii—Pt1—Sc2^viii	117.126 (17)	Pt3—Si1—Sc2^ix	71.27 (4)
Sc1—Pt1—Sc2^viii	65.27 (3)	Pt4—Si1—Sc2^vi	67.41 (3)
Sc1ⁱⁱ—Pt1—Sc2^viii	121.01 (3)	Pt4ⁱⁱ—Si1—Sc2^vi	143.59 (6)
Sc2^vii—Pt1—Sc2^viii	85.51 (4)	Pt3^xiii—Si1—Sc2^vi	67.40 (4)
Sc1^xii—Pt2—Sc1ⁱⁱⁱ	91.28 (4)	Pt1^v—Si1—Sc2^vi	134.73 (3)
Sc1^xii—Pt2—Sc1ⁱ	88.72 (4)	Pt3—Si1—Sc2^vi	71.27 (4)
Sc1ⁱⁱⁱ—Pt2—Sc1ⁱ	180.00 (3)	Sc2^ix—Si1—Sc2^vi	90.37 (6)
Sc1^xii—Pt2—Sc1	180.0	Pt4—Si1—Sc2	65.94 (3)
Sc1ⁱⁱⁱ—Pt2—Sc1	88.72 (4)	Pt4ⁱⁱ—Si1—Sc2	139.59 (6)
Sc1ⁱ—Pt2—Sc1	91.28 (4)	Pt3^xiii—Si1—Sc2	71.01 (4)
Sc1^xii—Pt2—Pt4^xii	58.80 (2)	Pt1^v—Si1—Sc2	66.96 (4)
Sc1ⁱⁱⁱ—Pt2—Pt4^xii	119.64 (2)	Pt3—Si1—Sc2	135.70 (3)
Sc1ⁱ—Pt2—Pt4^xii	60.36 (2)	Sc2^ix—Si1—Sc2	138.32 (6)
Sc1—Pt2—Pt4^xii	121.20 (2)	Sc2^vi—Si1—Sc2	75.95 (3)
Sc1^xii—Pt2—Pt4ⁱⁱⁱ	119.64 (2)	Pt4—Si1—Sc2ⁱⁱ	139.59 (6)
Sc1ⁱⁱⁱ—Pt2—Pt4ⁱⁱⁱ	58.80 (2)	Pt4ⁱⁱ—Si1—Sc2ⁱⁱ	65.95 (3)
Sc1ⁱ—Pt2—Pt4ⁱⁱⁱ	121.20 (2)	Pt3^xiii—Si1—Sc2ⁱⁱ	71.01 (4)
Sc1—Pt2—Pt4ⁱⁱⁱ	60.36 (2)	Pt1^v—Si1—Sc2ⁱⁱ	66.96 (4)
Pt4^xii—Pt2—Pt4ⁱⁱⁱ	90.17 (3)	Pt3—Si1—Sc2ⁱⁱ	135.70 (3)
Sc1^xii—Pt2—Pt4ⁱ	60.36 (2)	Sc2^ix—Si1—Sc2ⁱⁱ	75.95 (3)
Sc1ⁱⁱⁱ—Pt2—Pt4ⁱ	121.20 (3)	Sc2^vi—Si1—Sc2ⁱⁱ	138.32 (6)
Sc1ⁱ—Pt2—Pt4ⁱ	58.80 (2)	Sc2—Si1—Sc2ⁱⁱ	88.46 (6)

Symmetry codes: (i) x, y, z+1; (ii) x, y, z−1; (iii) −x+1, −y+1, −z+1; (iv) x+1, y, z+1; (v) x+1, y, z; (vi) x−1/2, −y+1/2, z; (vii) x−1, y, z−1; (viii) x−1, y, z; (ix) x−1/2, −y+1/2, z−1; (x) −x, −y+1, −z; (xi) −x, −y+1, −z+1; (xii) −x+1, −y+1, −z+2; (xiii) x+1/2, −y+1/2, z; (xiv) x+1/2, −y+1/2, z+1.

2-(Ag) top

Crystal data top

Br_0.09Cl_0.91Cu₆O₈Pb	Ag Kα radiation, λ = 0.56086 Å
M_r = 755.76	Cell parameters from 9932 reflections
Cubic, Fm3m	θ = 3.0–65.3°
a = 9.216 (2) Å	µ = 20.48 mm⁻¹
V = 782.8 (5) Å³	T = 100 K
Z = 4	Block, black
F(000) = 1354	0.12 × 0.11 × 0.09 mm
D_x = 6.413 Mg m⁻³

Data collection top

Bruker Smart APEX II Quazar diffractometer	770 reflections with I > 2σ(I)
Radiation source: INCOATEC Microsource	R_int = 0.029
ω scans	θ_max = 65.9°, θ_min = 3.0°
Absorption correction: multi-scan SADABS-2014/4	h = −29→18
T_min = 0.194, T_max = 0.315	k = −18→27
14473 measured reflections	l = −29→29
770 independent reflections

Refinement top

Refinement on F²	10 parameters
Least-squares matrix: full	0 restraints
R[F² > 2σ(F²)] = 0.024	w = 1/[σ²(F_o²) + (0.0381P)²] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.050	(Δ/σ)_max < 0.001
S = 1.20	Δρ_max = 14.02 e Å⁻³
770 reflections	Δρ_min = −7.01 e Å⁻³

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
Pb1	0.0000	0.0000	0.0000	0.00270 (2)
Cu1	0.2500	0.2500	0.0000	0.00337 (2)
O1	0.14257 (5)	0.14257 (5)	0.14257 (5)	0.00422 (6)
Cl1	0.0000	0.5000	0.0000	0.0142 (3)	0.911 (12)
Br1	0.0000	0.5000	0.0000	0.0142 (3)	0.089 (12)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Pb1	0.00270 (2)	0.00270 (2)	0.00270 (2)	0.000	0.000	0.000
Cu1	0.00351 (3)	0.00351 (3)	0.00308 (3)	−0.00080 (2)	0.000	0.000
O1	0.00422 (6)	0.00422 (6)	0.00422 (6)	0.00014 (6)	0.00014 (6)	0.00014 (6)
Cl1	0.0142 (3)	0.0142 (3)	0.0142 (3)	0.000	0.000	0.000
Br1	0.0142 (3)	0.0142 (3)	0.0142 (3)	0.000	0.000	0.000

Geometric parameters (Å, º) top

Pb1—O1	2.2758 (9)	Pb1—Cu1^x	3.2583 (7)
Pb1—O1ⁱ	2.2758 (9)	Pb1—Cu1^xi	3.2583 (7)
Pb1—O1ⁱⁱ	2.2758 (9)	Cu1—O1^vi	1.9201 (4)
Pb1—O1ⁱⁱⁱ	2.2758 (9)	Cu1—O1^xii	1.9201 (4)
Pb1—O1^iv	2.2758 (9)	Cu1—O1^xiii	1.9201 (4)
Pb1—O1^v	2.2758 (9)	Cu1—O1	1.9201 (4)
Pb1—O1^vi	2.2758 (9)	Cu1—Pb1^xiv	3.2583 (7)
Pb1—O1^vii	2.2758 (9)	O1—Cu1^x	1.9201 (4)
Pb1—Cu1^viii	3.2583 (7)	O1—Cu1^ix	1.9201 (4)
Pb1—Cu1^ix	3.2583 (7)

O1—Pb1—O1ⁱ	180.00 (4)	Cu1^viii—Pb1—Cu1^ix	120.0
O1—Pb1—O1ⁱⁱ	70.5	O1—Pb1—Cu1^x	35.3
O1ⁱ—Pb1—O1ⁱⁱ	109.5	O1ⁱ—Pb1—Cu1^x	144.7
O1—Pb1—O1ⁱⁱⁱ	109.5	O1ⁱⁱ—Pb1—Cu1^x	90.0
O1ⁱ—Pb1—O1ⁱⁱⁱ	70.5	O1ⁱⁱⁱ—Pb1—Cu1^x	90.0
O1ⁱⁱ—Pb1—O1ⁱⁱⁱ	180.000 (18)	O1^iv—Pb1—Cu1^x	35.3
O1—Pb1—O1^iv	70.5	O1^v—Pb1—Cu1^x	144.7
O1ⁱ—Pb1—O1^iv	109.5	O1^vi—Pb1—Cu1^x	90.0
O1ⁱⁱ—Pb1—O1^iv	109.5	O1^vii—Pb1—Cu1^x	90.0
O1ⁱⁱⁱ—Pb1—O1^iv	70.5	Cu1^viii—Pb1—Cu1^x	120.0
O1—Pb1—O1^v	109.5	Cu1^ix—Pb1—Cu1^x	60.0
O1ⁱ—Pb1—O1^v	70.5	O1—Pb1—Cu1^xi	144.7
O1ⁱⁱ—Pb1—O1^v	70.5	O1ⁱ—Pb1—Cu1^xi	35.3
O1ⁱⁱⁱ—Pb1—O1^v	109.5	O1ⁱⁱ—Pb1—Cu1^xi	90.0
O1^iv—Pb1—O1^v	180.000 (18)	O1ⁱⁱⁱ—Pb1—Cu1^xi	90.0
O1—Pb1—O1^vi	70.5	O1^iv—Pb1—Cu1^xi	144.7
O1ⁱ—Pb1—O1^vi	109.5	O1^v—Pb1—Cu1^xi	35.3
O1ⁱⁱ—Pb1—O1^vi	109.5	O1^vi—Pb1—Cu1^xi	90.0
O1ⁱⁱⁱ—Pb1—O1^vi	70.5	O1^vii—Pb1—Cu1^xi	90.0
O1^iv—Pb1—O1^vi	109.5	Cu1^viii—Pb1—Cu1^xi	60.0
O1^v—Pb1—O1^vi	70.5	Cu1^ix—Pb1—Cu1^xi	120.0
O1—Pb1—O1^vii	109.5	Cu1^x—Pb1—Cu1^xi	180.0
O1ⁱ—Pb1—O1^vii	70.529 (1)	O1^vi—Cu1—O1^xii	180.0
O1ⁱⁱ—Pb1—O1^vii	70.5	O1^vi—Cu1—O1^xiii	93.64 (4)
O1ⁱⁱⁱ—Pb1—O1^vii	109.5	O1^xii—Cu1—O1^xiii	86.36 (4)
O1^iv—Pb1—O1^vii	70.5	O1^vi—Cu1—O1	86.36 (4)
O1^v—Pb1—O1^vii	109.5	O1^xii—Cu1—O1	93.64 (4)
O1^vi—Pb1—O1^vii	180.00 (4)	O1^xiii—Cu1—O1	180.0
O1—Pb1—Cu1^viii	144.7	O1^vi—Cu1—Pb1	43.18 (2)
O1ⁱ—Pb1—Cu1^viii	35.3	O1^xii—Cu1—Pb1	136.82 (2)
O1ⁱⁱ—Pb1—Cu1^viii	90.0	O1^xiii—Cu1—Pb1	136.82 (2)
O1ⁱⁱⁱ—Pb1—Cu1^viii	90.0	O1—Cu1—Pb1	43.18 (2)
O1^iv—Pb1—Cu1^viii	90.0	O1^vi—Cu1—Pb1^xiv	136.82 (2)
O1^v—Pb1—Cu1^viii	90.0	O1^xii—Cu1—Pb1^xiv	43.18 (2)
O1^vi—Pb1—Cu1^viii	144.7	O1^xiii—Cu1—Pb1^xiv	43.18 (2)
O1^vii—Pb1—Cu1^viii	35.3	O1—Cu1—Pb1^xiv	136.82 (2)
O1—Pb1—Cu1^ix	35.3	Pb1—Cu1—Pb1^xiv	180.0
O1ⁱ—Pb1—Cu1^ix	144.7	Cu1^x—O1—Cu1	116.091 (14)
O1ⁱⁱ—Pb1—Cu1^ix	35.3	Cu1^x—O1—Cu1^ix	116.091 (14)
O1ⁱⁱⁱ—Pb1—Cu1^ix	144.7	Cu1—O1—Cu1^ix	116.091 (14)
O1^iv—Pb1—Cu1^ix	90.0	Cu1^x—O1—Pb1	101.56 (2)
O1^v—Pb1—Cu1^ix	90.0	Cu1—O1—Pb1	101.56 (2)
O1^vi—Pb1—Cu1^ix	90.0	Cu1^ix—O1—Pb1	101.56 (2)
O1^vii—Pb1—Cu1^ix	90.0

Symmetry codes: (i) −x, −y, −z; (ii) −x, y, z; (iii) x, −y, −z; (iv) x, −y, z; (v) −x, y, −z; (vi) x, y, −z; (vii) −x, −y, z; (viii) x−1/2, y−1/2, z; (ix) z, x, y; (x) y, z, x; (xi) y−1/2, z, x−1/2; (xii) −x+1/2, −y+1/2, z; (xiii) −x+1/2, −y+1/2, −z; (xiv) x+1/2, y+1/2, z.

2-(Mo) top

Crystal data top

Br_0.10Cl_0.90Cu₆O₈Pb	Mo Kα radiation, λ = 0.71073 Å
M_r = 756.41	Cell parameters from 9919 reflections
Cubic, Fm3m	θ = 3.8–55.7°
a = 9.2164 (2) Å	µ = 38.25 mm⁻¹
V = 782.86 (5) Å³	T = 100 K
Z = 4	Block, black
F(000) = 1355	0.12 × 0.11 × 0.09 mm
D_x = 6.418 Mg m⁻³

Data collection top

Bruker Smart APEX II Quazar diffractometer	313 reflections with I > 2σ(I)
Radiation source: INCOATEC Microsource	R_int = 0.035
ω scans	θ_max = 55.7°, θ_min = 3.8°
Absorption correction: multi-scan SADABS-2014/4	h = −20→20
T_min = 0.062, T_max = 0.158	k = −21→19
10388 measured reflections	l = −20→20
313 independent reflections

Refinement top

Refinement on F²	0 restraints
Least-squares matrix: full	w = 1/[σ²(F_o²) + (0.0319P)² + 1.8322P] where P = (F_o² + 2F_c²)/3
R[F² > 2σ(F²)] = 0.020	(Δ/σ)_max < 0.001
wR(F²) = 0.045	Δρ_max = 4.40 e Å⁻³
S = 1.22	Δρ_min = −2.67 e Å⁻³
313 reflections	Extinction correction: SHELXL-2014/7 (Sheldrick 2014, Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
11 parameters	Extinction coefficient: 0.00051 (9)

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
Pb1	0.5000	0.0000	0.5000	0.00397 (5)
Cu1	0.5000	0.2500	0.2500	0.00419 (7)
O1	0.35715 (9)	0.14285 (9)	0.35715 (9)	0.00493 (14)
Cl1	0.5000	0.5000	0.5000	0.0151 (4)	0.897 (12)
Br1	0.5000	0.5000	0.5000	0.0151 (4)	0.103 (12)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Pb1	0.00397 (5)	0.00397 (5)	0.00397 (5)	0.000	0.000	0.000
Cu1	0.00387 (8)	0.00436 (7)	0.00436 (7)	0.000	0.000	0.00092 (5)
O1	0.00493 (14)	0.00493 (14)	0.00493 (14)	0.00010 (18)	−0.00010 (18)	0.00010 (18)
Cl1	0.0151 (4)	0.0151 (4)	0.0151 (4)	0.000	0.000	0.000
Br1	0.0151 (4)	0.0151 (4)	0.0151 (4)	0.000	0.000	0.000

Geometric parameters (Å, º) top

Pb1—O1ⁱ	2.2804 (15)	Pb1—Cu1^ix	3.2585 (1)
Pb1—O1ⁱⁱ	2.2804 (15)	Pb1—Cu1^x	3.2585 (1)
Pb1—O1ⁱⁱⁱ	2.2804 (15)	Cu1—O1	1.9193 (3)
Pb1—O1^iv	2.2804 (15)	Cu1—O1ⁱⁱⁱ	1.9193 (3)
Pb1—O1^v	2.2804 (15)	Cu1—O1^xi	1.9193 (3)
Pb1—O1^vi	2.2804 (15)	Cu1—O1^xii	1.9193 (3)
Pb1—O1^vii	2.2804 (15)	Cu1—Pb1^xiii	3.2585 (1)
Pb1—O1	2.2804 (15)	O1—Cu1^ix	1.9193 (3)
Pb1—Cu1^vi	3.2585 (1)	O1—Cu1^xiv	1.9193 (3)
Pb1—Cu1^viii	3.2585 (1)

O1ⁱ—Pb1—O1ⁱⁱ	180.00 (3)	Cu1^vi—Pb1—Cu1^viii	120.0
O1ⁱ—Pb1—O1ⁱⁱⁱ	109.5	O1ⁱ—Pb1—Cu1^ix	35.3
O1ⁱⁱ—Pb1—O1ⁱⁱⁱ	70.5	O1ⁱⁱ—Pb1—Cu1^ix	144.7
O1ⁱ—Pb1—O1^iv	70.5	O1ⁱⁱⁱ—Pb1—Cu1^ix	90.0
O1ⁱⁱ—Pb1—O1^iv	109.5	O1^iv—Pb1—Cu1^ix	90.0
O1ⁱⁱⁱ—Pb1—O1^iv	180.0	O1^v—Pb1—Cu1^ix	90.0
O1ⁱ—Pb1—O1^v	109.5	O1^vi—Pb1—Cu1^ix	90.0
O1ⁱⁱ—Pb1—O1^v	70.5	O1^vii—Pb1—Cu1^ix	144.7
O1ⁱⁱⁱ—Pb1—O1^v	109.5	O1—Pb1—Cu1^ix	35.3
O1^iv—Pb1—O1^v	70.5	Cu1^vi—Pb1—Cu1^ix	60.0
O1ⁱ—Pb1—O1^vi	70.5	Cu1^viii—Pb1—Cu1^ix	180.0
O1ⁱⁱ—Pb1—O1^vi	109.5	O1ⁱ—Pb1—Cu1^x	144.7
O1ⁱⁱⁱ—Pb1—O1^vi	70.5	O1ⁱⁱ—Pb1—Cu1^x	35.3
O1^iv—Pb1—O1^vi	109.5	O1ⁱⁱⁱ—Pb1—Cu1^x	90.0
O1^v—Pb1—O1^vi	180.0	O1^iv—Pb1—Cu1^x	90.0
O1ⁱ—Pb1—O1^vii	109.5	O1^v—Pb1—Cu1^x	35.3
O1ⁱⁱ—Pb1—O1^vii	70.5	O1^vi—Pb1—Cu1^x	144.7
O1ⁱⁱⁱ—Pb1—O1^vii	109.471 (1)	O1^vii—Pb1—Cu1^x	90.0
O1^iv—Pb1—O1^vii	70.5	O1—Pb1—Cu1^x	90.0
O1^v—Pb1—O1^vii	109.471 (1)	Cu1^vi—Pb1—Cu1^x	180.0
O1^vi—Pb1—O1^vii	70.5	Cu1^viii—Pb1—Cu1^x	60.0
O1ⁱ—Pb1—O1	70.5	Cu1^ix—Pb1—Cu1^x	120.0
O1ⁱⁱ—Pb1—O1	109.471 (1)	O1—Cu1—O1ⁱⁱⁱ	86.62 (9)
O1ⁱⁱⁱ—Pb1—O1	70.5	O1—Cu1—O1^xi	93.38 (9)
O1^iv—Pb1—O1	109.5	O1ⁱⁱⁱ—Cu1—O1^xi	180.0
O1^v—Pb1—O1	70.5	O1—Cu1—O1^xii	180.0
O1^vi—Pb1—O1	109.5	O1ⁱⁱⁱ—Cu1—O1^xii	93.38 (9)
O1^vii—Pb1—O1	180.0	O1^xi—Cu1—O1^xii	86.62 (9)
O1ⁱ—Pb1—Cu1^vi	35.3	O1—Cu1—Pb1	43.31 (4)
O1ⁱⁱ—Pb1—Cu1^vi	144.7	O1ⁱⁱⁱ—Cu1—Pb1	43.31 (4)
O1ⁱⁱⁱ—Pb1—Cu1^vi	90.0	O1^xi—Cu1—Pb1	136.69 (4)
O1^iv—Pb1—Cu1^vi	90.0	O1^xii—Cu1—Pb1	136.69 (4)
O1^v—Pb1—Cu1^vi	144.7	O1—Cu1—Pb1^xiii	136.69 (4)
O1^vi—Pb1—Cu1^vi	35.3	O1ⁱⁱⁱ—Cu1—Pb1^xiii	136.69 (4)
O1^vii—Pb1—Cu1^vi	90.0	O1^xi—Cu1—Pb1^xiii	43.31 (4)
O1—Pb1—Cu1^vi	90.0	O1^xii—Cu1—Pb1^xiii	43.31 (4)
O1ⁱ—Pb1—Cu1^viii	144.7	Pb1—Cu1—Pb1^xiii	180.0
O1ⁱⁱ—Pb1—Cu1^viii	35.3	Cu1^ix—O1—Cu1^xiv	116.18 (3)
O1ⁱⁱⁱ—Pb1—Cu1^viii	90.0	Cu1^ix—O1—Cu1	116.18 (3)
O1^iv—Pb1—Cu1^viii	90.0	Cu1^xiv—O1—Cu1	116.18 (3)
O1^v—Pb1—Cu1^viii	90.0	Cu1^ix—O1—Pb1	101.42 (4)
O1^vi—Pb1—Cu1^viii	90.0	Cu1^xiv—O1—Pb1	101.42 (4)
O1^vii—Pb1—Cu1^viii	35.3	Cu1—O1—Pb1	101.42 (4)
O1—Pb1—Cu1^viii	144.7

Symmetry codes: (i) x, −y, z; (ii) −x+1, y, −z+1; (iii) −x+1, y, z; (iv) x, −y, −z+1; (v) x, y, −z+1; (vi) −x+1, −y, z; (vii) −x+1, −y, −z+1; (viii) z+1/2, −x+1/2, −y+1; (ix) z, −x+1/2, −y+1/2; (x) −x+1, −y+1/2, z+1/2; (xi) x, −y+1/2, −z+1/2; (xii) −x+1, −y+1/2, −z+1/2; (xiii) x, y+1/2, z−1/2; (xiv) y, z, x.

3-(Ag) top

Crystal data top

O₄W·2(H₂O)·2(Na)	F(000) = 1184
M_r = 329.86	D_x = 3.562 Mg m⁻³
Orthorhombic, Pbca	Ag Kα radiation, λ = 0.56086 Å
a = 8.439 (2) Å	Cell parameters from 9695 reflections
b = 10.559 (2) Å	θ = 2.3–44.4°
c = 13.807 (3) Å	µ = 10.16 mm⁻¹
V = 1230.3 (5) Å³	T = 100 K
Z = 8	0.10 × 0.06 × 0.03 mm

Data collection top

Bruker Smart APEX II Quazar diffractometer	8783 reflections with I > 2σ(I)
Radiation source: INCOATEC Microsource	R_int = 0.029
ω scans	θ_max = 44.5°, θ_min = 2.3°
Absorption correction: multi-scan SADABS-2014/4	h = −21→21
T_min = 0.567, T_max = 0.734	k = −26→26
146508 measured reflections	l = −34→34
10047 independent reflections

Refinement top

Refinement on F²	Hydrogen site location: difference Fourier map
Least-squares matrix: full	Only H-atom coordinates refined
R[F² > 2σ(F²)] = 0.014	w = 1/[σ²(F_o²) + (0.0046P)² + 0.8512P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.025	(Δ/σ)_max = 0.006
S = 1.16	Δρ_max = 1.81 e Å⁻³
10047 reflections	Δρ_min = −3.04 e Å⁻³
95 parameters	Extinction correction: SHELXL, Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
84 restraints	Extinction coefficient: 0.00107 (3)

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
W1	0.48649 (2)	0.30163 (2)	0.47725 (2)	0.00383 (1)
Na1	0.75923 (4)	0.45111 (3)	0.64771 (2)	0.00736 (4)
Na2	0.84444 (4)	0.49551 (3)	0.41430 (2)	0.00734 (4)
O1	0.55242 (6)	0.32269 (5)	0.59925 (4)	0.00723 (6)
O2	0.63150 (6)	0.35114 (5)	0.39028 (4)	0.00762 (6)
O3	0.31247 (6)	0.39264 (5)	0.46244 (4)	0.00817 (6)
O4	0.44310 (6)	0.13853 (5)	0.45833 (4)	0.00671 (6)
O5	0.77221 (7)	0.35953 (6)	0.79899 (4)	0.00911 (7)
H51	0.863 (2)	0.3544 (16)	0.8221 (13)	0.014*
H52	0.728 (2)	0.2944 (16)	0.8201 (13)	0.014*
O6	0.96253 (7)	0.59201 (6)	0.69974 (4)	0.00978 (7)
H61	0.945 (2)	0.6616 (17)	0.6718 (13)	0.015*
H62	0.942 (2)	0.6028 (16)	0.7555 (13)	0.015*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
W1	0.00425 (1)	0.00337 (1)	0.00388 (1)	0.00000 (1)	0.00015 (1)	−0.00008 (1)
Na1	0.00747 (10)	0.00789 (11)	0.00671 (10)	−0.00050 (8)	−0.00054 (8)	0.00051 (9)
Na2	0.00754 (10)	0.00692 (11)	0.00757 (10)	−0.00073 (8)	−0.00024 (8)	0.00028 (9)
O1	0.00758 (14)	0.00816 (16)	0.00596 (14)	−0.00064 (12)	−0.00099 (11)	−0.00058 (12)
O2	0.00810 (14)	0.00793 (16)	0.00684 (14)	−0.00197 (12)	0.00159 (11)	0.00022 (13)
O3	0.00798 (14)	0.00774 (16)	0.00880 (15)	0.00276 (12)	−0.00055 (11)	0.00060 (13)
O4	0.00741 (14)	0.00465 (14)	0.00808 (14)	−0.00081 (11)	−0.00005 (11)	−0.00037 (11)
O5	0.00954 (16)	0.00957 (18)	0.00820 (16)	−0.00075 (13)	−0.00137 (12)	0.00183 (14)
O6	0.01269 (18)	0.00836 (17)	0.00830 (16)	−0.00015 (14)	0.00120 (13)	−0.00029 (14)

Geometric parameters (Å, º) top

W1—O3	1.7669 (6)	Na2—O4^iv	2.4061 (7)
W1—O4	1.7800 (6)	Na2—O5^vii	2.4179 (8)
W1—O1	1.7879 (6)	Na2—O4^viii	2.4217 (7)
W1—O2	1.7924 (6)	Na2—O6^v	2.4468 (7)
W1—Na2ⁱ	3.6385 (7)	Na2—O3ⁱⁱⁱ	2.4586 (7)
W1—Na1	3.6508 (6)	Na2—Na1^v	3.4982 (9)
W1—Na2ⁱⁱ	3.6774 (6)	Na2—Na2^v	3.5360 (9)
W1—Na1ⁱⁱ	3.7116 (6)	Na2—W1^viii	3.6385 (7)
Na1—O5	2.3042 (8)	Na2—W1^iv	3.6774 (6)
Na1—O1	2.3091 (7)	Na2—Na1^vii	3.8250 (9)
Na1—O3ⁱⁱⁱ	2.3241 (7)	O3—Na1ⁱⁱⁱ	2.3241 (7)
Na1—O4^iv	2.3339 (7)	O3—Na2ⁱⁱⁱ	2.4586 (7)
Na1—O6	2.3818 (8)	O4—Na1ⁱⁱ	2.3339 (7)
Na1—Na2	3.3352 (8)	O4—Na2ⁱⁱ	2.4061 (7)
Na1—Na2^v	3.4982 (9)	O4—Na2ⁱ	2.4217 (7)
Na1—W1^iv	3.7117 (6)	O5—Na2^vi	2.4180 (8)
Na1—Na2^vi	3.8250 (9)	O6—Na2^v	2.4467 (8)
Na2—O2	2.3797 (7)

O3—W1—O4	109.77 (3)	O2—Na2—O4^viii	173.47 (2)
O3—W1—O1	107.46 (3)	O4^iv—Na2—O4^viii	85.82 (2)
O4—W1—O1	108.82 (2)	O5^vii—Na2—O4^viii	94.13 (3)
O3—W1—O2	109.35 (3)	O2—Na2—O6^v	99.85 (3)
O4—W1—O2	108.92 (2)	O4^iv—Na2—O6^v	91.02 (3)
O1—W1—O2	112.48 (3)	O5^vii—Na2—O6^v	94.96 (3)
O3—W1—Na2ⁱ	141.39 (2)	O4^viii—Na2—O6^v	84.50 (3)
O4—W1—Na2ⁱ	35.52 (2)	O2—Na2—O3ⁱⁱⁱ	89.86 (3)
O1—W1—Na2ⁱ	102.330 (19)	O4^iv—Na2—O3ⁱⁱⁱ	87.88 (3)
O2—W1—Na2ⁱ	80.29 (2)	O5^vii—Na2—O3ⁱⁱⁱ	86.13 (3)
O3—W1—Na1	111.31 (2)	O4^viii—Na2—O3ⁱⁱⁱ	85.72 (3)
O4—W1—Na1	129.986 (18)	O6^v—Na2—O3ⁱⁱⁱ	170.21 (2)
O1—W1—Na1	30.977 (18)	O2—Na2—Na1	83.209 (18)
O2—W1—Na1	82.84 (2)	O4^iv—Na2—Na1	44.407 (17)
Na2ⁱ—W1—Na1	106.908 (13)	O5^vii—Na2—Na1	129.60 (2)
O3—W1—Na2ⁱⁱ	103.90 (2)	O4^viii—Na2—Na1	90.270 (19)
O4—W1—Na2ⁱⁱ	33.614 (19)	O6^v—Na2—Na1	135.42 (2)
O1—W1—Na2ⁱⁱ	79.86 (2)	O3ⁱⁱⁱ—Na2—Na1	44.152 (17)
O2—W1—Na2ⁱⁱ	138.089 (19)	O2—Na2—Na1^v	142.29 (2)
Na2ⁱ—W1—Na2ⁱⁱ	57.803 (15)	O4^iv—Na2—Na1^v	86.721 (19)
Na1—W1—Na2ⁱⁱ	108.171 (13)	O5^vii—Na2—Na1^v	97.24 (2)
O3—W1—Na1ⁱⁱ	84.71 (2)	O4^viii—Na2—Na1^v	41.676 (16)
O4—W1—Na1ⁱⁱ	29.523 (18)	O6^v—Na2—Na1^v	42.846 (18)
O1—W1—Na1ⁱⁱ	133.487 (18)	O3ⁱⁱⁱ—Na2—Na1^v	127.37 (2)
O2—W1—Na1ⁱⁱ	104.54 (2)	Na1—Na2—Na1^v	117.729 (11)
Na2ⁱ—W1—Na1ⁱⁱ	56.830 (15)	O2—Na2—Na2^v	132.15 (2)
Na1—W1—Na1ⁱⁱ	159.435 (4)	O4^iv—Na2—Na2^v	43.082 (16)
Na2ⁱⁱ—W1—Na1ⁱⁱ	53.659 (14)	O5^vii—Na2—Na2^v	136.55 (2)
O5—Na1—O1	92.99 (2)	O4^viii—Na2—Na2^v	42.737 (16)
O5—Na1—O3ⁱⁱⁱ	154.62 (3)	O6^v—Na2—Na2^v	86.93 (3)
O1—Na1—O3ⁱⁱⁱ	91.75 (3)	O3ⁱⁱⁱ—Na2—Na2^v	85.63 (2)
O5—Na1—O4^iv	111.52 (3)	Na1—Na2—Na2^v	61.127 (17)
O1—Na1—O4^iv	94.74 (3)	Na1^v—Na2—Na2^v	56.602 (17)
O3ⁱⁱⁱ—Na1—O4^iv	92.89 (3)	O2—Na2—W1^viii	153.959 (19)
O5—Na1—O6	87.39 (2)	O4^iv—Na2—W1^viii	102.25 (2)
O1—Na1—O6	176.97 (3)	O5^vii—Na2—W1^viii	75.79 (2)
O3ⁱⁱⁱ—Na1—O6	86.64 (3)	O4^viii—Na2—W1^viii	25.279 (13)
O4^iv—Na1—O6	87.91 (3)	O6^v—Na2—W1^viii	103.19 (2)
O5—Na1—Na2	157.61 (2)	O3ⁱⁱⁱ—Na2—W1^viii	67.611 (19)
O1—Na1—Na2	88.024 (19)	Na1—Na2—W1^viii	88.774 (12)
O3ⁱⁱⁱ—Na1—Na2	47.466 (17)	Na1^v—Na2—W1^viii	62.638 (9)
O4^iv—Na1—Na2	46.170 (16)	Na2^v—Na2—W1^viii	61.649 (11)
O6—Na1—Na2	92.77 (2)	O2—Na2—W1^iv	75.90 (2)
O5—Na1—Na2^v	104.123 (19)	O4^iv—Na2—W1^iv	24.175 (13)
O1—Na1—Na2^v	138.27 (2)	O5^vii—Na2—W1^iv	160.206 (19)
O3ⁱⁱⁱ—Na1—Na2^v	88.531 (19)	O4^viii—Na2—W1^iv	100.86 (2)
O4^iv—Na1—Na2^v	43.625 (17)	O6^v—Na2—W1^iv	73.90 (2)
O6—Na1—Na2^v	44.312 (18)	O3ⁱⁱⁱ—Na2—W1^iv	107.67 (2)
Na2—Na1—Na2^v	62.271 (11)	Na1—Na2—W1^iv	63.695 (10)
O5—Na1—W1	115.65 (2)	Na1^v—Na2—W1^iv	85.725 (12)
O1—Na1—W1	23.486 (14)	Na2^v—Na2—W1^iv	60.546 (12)
O3ⁱⁱⁱ—Na1—W1	73.79 (2)	W1^viii—Na2—W1^iv	122.196 (15)
O4^iv—Na1—W1	80.76 (2)	O2—Na2—Na1^vii	77.739 (17)
O6—Na1—W1	156.722 (19)	O4^iv—Na2—Na1^vii	150.364 (19)
Na2—Na1—W1	64.769 (14)	O5^vii—Na2—Na1^vii	34.916 (16)
Na2^v—Na1—W1	120.974 (16)	O4^viii—Na2—Na1^vii	108.603 (18)
O5—Na1—W1^iv	95.46 (2)	O6^v—Na2—Na1^vii	65.71 (2)
O1—Na1—W1^iv	80.43 (2)	O3ⁱⁱⁱ—Na2—Na1^vii	118.17 (2)
O3ⁱⁱⁱ—Na1—W1^iv	109.92 (2)	Na1—Na2—Na1^vii	154.324 (13)
O4^iv—Na1—W1^iv	22.074 (13)	Na1^v—Na2—Na1^vii	87.674 (12)
O6—Na1—W1^iv	102.54 (2)	Na2^v—Na2—Na1^vii	144.087 (16)
Na2—Na1—W1^iv	62.645 (11)	W1^viii—Na2—Na1^vii	100.874 (11)
Na2^v—Na1—W1^iv	60.531 (12)	W1^iv—Na2—Na1^vii	126.308 (11)
W1—Na1—W1^iv	73.456 (15)	W1—O1—Na1	125.54 (3)
O5—Na1—Na2^vi	36.915 (19)	W1—O2—Na2	127.52 (3)
O1—Na1—Na2^vi	101.098 (19)	W1—O3—Na1ⁱⁱⁱ	132.71 (3)
O3ⁱⁱⁱ—Na1—Na2^vi	117.75 (2)	W1—O3—Na2ⁱⁱⁱ	128.96 (3)
O4^iv—Na1—Na2^vi	144.634 (19)	Na1ⁱⁱⁱ—O3—Na2ⁱⁱⁱ	88.38 (3)
O6—Na1—Na2^vi	77.439 (19)	W1—O4—Na1ⁱⁱ	128.40 (3)
Na2—Na1—Na2^vi	163.426 (12)	W1—O4—Na2ⁱⁱ	122.21 (3)
Na2^v—Na1—Na2^vi	115.496 (12)	Na1ⁱⁱ—O4—Na2ⁱⁱ	89.42 (2)
W1—Na1—Na2^vi	122.676 (16)	W1—O4—Na2ⁱ	119.20 (3)
W1^iv—Na1—Na2^vi	132.178 (11)	Na1ⁱⁱ—O4—Na2ⁱ	94.70 (3)
O2—Na2—O4^iv	89.22 (2)	Na2ⁱⁱ—O4—Na2ⁱ	94.18 (2)
O2—Na2—O5^vii	90.37 (3)	Na1—O5—Na2^vi	108.17 (3)
O4^iv—Na2—O5^vii	173.99 (2)	Na1—O6—Na2^v	92.84 (3)

Symmetry codes: (i) −x+3/2, y−1/2, z; (ii) x−1/2, −y+1/2, −z+1; (iii) −x+1, −y+1, −z+1; (iv) x+1/2, −y+1/2, −z+1; (v) −x+2, −y+1, −z+1; (vi) −x+3/2, −y+1, z+1/2; (vii) −x+3/2, −y+1, z−1/2; (viii) −x+3/2, y+1/2, z.

3-(Mo) top

Crystal data top

O₄W·2(H₂O)·2(Na)	F(000) = 1184
M_r = 329.86	D_x = 3.555 Mg m⁻³
Orthorhombic, Pbca	Mo Kα radiation, λ = 0.71073 Å
a = 8.442 (2) Å	Cell parameters from 9598 reflections
b = 10.569 (2) Å	θ = 3.4–54.1°
c = 13.816 (3) Å	µ = 18.84 mm⁻¹
V = 1232.7 (5) Å³	T = 100 K
Z = 8	0.11 × 0.05 × 0.03 mm

Data collection top

Bruker Smart APEX II Quazar diffractometer	7024 reflections with I > 2σ(I)
Radiation source: INCOATEC Microsource	R_int = 0.030
ω scans	θ_max = 54.1°, θ_min = 3.0°
Absorption correction: multi-scan SADABS-2014/4	h = −19→18
T_min = 0.416, T_max = 0.580	k = −23→23
80496 measured reflections	l = −29→30
7584 independent reflections

Refinement top

Refinement on F²	Hydrogen site location: difference Fourier map
Least-squares matrix: full	Only H-atom coordinates refined
R[F² > 2σ(F²)] = 0.015	w = 1/[σ²(F_o²) + (0.0103P)² + 1.1388P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.033	(Δ/σ)_max = 0.011
S = 1.18	Δρ_max = 2.64 e Å⁻³
7584 reflections	Δρ_min = −2.70 e Å⁻³
95 parameters	Extinction correction: SHELXL, Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
84 restraints	Extinction coefficient: 0.00164 (4)

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
W1	0.51352 (2)	0.30163 (2)	0.52276 (2)	0.00396 (1)
Na2	0.15563 (5)	0.49545 (4)	0.58567 (3)	0.00754 (6)
Na1	0.24079 (5)	0.45107 (4)	0.35226 (3)	0.00759 (6)
O1	0.44747 (9)	0.32286 (7)	0.40073 (5)	0.00745 (8)
O2	0.36862 (9)	0.35113 (7)	0.60982 (5)	0.00779 (9)
O3	0.68756 (9)	0.39260 (7)	0.53761 (5)	0.00844 (9)
O4	0.55707 (9)	0.13864 (6)	0.54168 (5)	0.00685 (8)
O5	0.22785 (9)	0.35952 (7)	0.20105 (6)	0.00921 (9)
H51	0.141 (3)	0.356 (2)	0.1785 (17)	0.014*
H52	0.268 (3)	0.294 (2)	0.1780 (17)	0.014*
O6	0.03752 (10)	0.59210 (7)	0.30019 (6)	0.01004 (10)
H61	0.061 (3)	0.656 (2)	0.3270 (18)	0.015*
H62	0.063 (3)	0.603 (2)	0.2419 (18)	0.015*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
W1	0.00433 (1)	0.00344 (1)	0.00410 (1)	0.00001 (1)	0.00014 (1)	0.00008 (1)
Na2	0.00776 (15)	0.00714 (14)	0.00773 (14)	0.00070 (11)	−0.00028 (11)	−0.00044 (11)
Na1	0.00765 (15)	0.00804 (14)	0.00709 (14)	0.00043 (11)	−0.00063 (11)	−0.00056 (11)
O1	0.0078 (2)	0.0083 (2)	0.0062 (2)	0.00078 (16)	−0.00116 (16)	0.00078 (15)
O2	0.0081 (2)	0.0082 (2)	0.0070 (2)	0.00181 (16)	0.00158 (16)	−0.00012 (16)
O3	0.0085 (2)	0.0078 (2)	0.0090 (2)	−0.00282 (17)	−0.00058 (17)	−0.00065 (17)
O4	0.0076 (2)	0.00462 (18)	0.0083 (2)	0.00078 (15)	−0.00003 (16)	0.00059 (15)
O5	0.0091 (2)	0.0101 (2)	0.0085 (2)	0.00075 (18)	−0.00142 (18)	−0.00177 (18)
O6	0.0130 (3)	0.0087 (2)	0.0084 (2)	0.0003 (2)	0.00140 (19)	0.00022 (18)

Geometric parameters (Å, º) top

W1—O3	1.7678 (8)	Na2—W1ⁱⁱⁱ	3.6799 (7)
W1—O4	1.7807 (7)	Na2—Na1^iv	3.8275 (10)
W1—O1	1.7900 (8)	Na1—O5	2.3049 (10)
W1—O2	1.7936 (7)	Na1—O1	2.3085 (9)
W1—Na2ⁱ	3.6423 (7)	Na1—O3^vii	2.3261 (9)
W1—Na1	3.6531 (7)	Na1—O4ⁱⁱⁱ	2.3349 (9)
W1—Na2ⁱⁱ	3.6799 (7)	Na1—O6	2.3841 (10)
W1—Na1ⁱⁱ	3.7143 (7)	Na1—Na2^vi	3.5006 (10)
Na2—O2	2.3814 (9)	Na1—W1ⁱⁱⁱ	3.7143 (7)
Na2—O4ⁱⁱⁱ	2.4076 (9)	Na1—Na2^viii	3.8275 (10)
Na2—O5^iv	2.4204 (10)	O3—Na1^vii	2.3262 (9)
Na2—O4^v	2.4257 (9)	O3—Na2^vii	2.4604 (9)
Na2—O6^vi	2.4498 (10)	O4—Na1ⁱⁱ	2.3349 (9)
Na2—O3^vii	2.4605 (9)	O4—Na2ⁱⁱ	2.4075 (9)
Na2—Na1	3.3372 (9)	O4—Na2ⁱ	2.4257 (9)
Na2—Na1^vi	3.5006 (10)	O5—Na2^viii	2.4205 (10)
Na2—Na2^vi	3.5380 (11)	O6—Na2^vi	2.4498 (10)
Na2—W1^v	3.6423 (7)

O3—W1—O4	109.73 (4)	O4^v—Na2—W1ⁱⁱⁱ	100.89 (2)
O3—W1—O1	107.46 (3)	O6^vi—Na2—W1ⁱⁱⁱ	73.91 (2)
O4—W1—O1	108.90 (3)	O3^vii—Na2—W1ⁱⁱⁱ	107.69 (3)
O3—W1—O2	109.29 (4)	Na1—Na2—W1ⁱⁱⁱ	63.700 (12)
O4—W1—O2	108.94 (3)	Na1^vi—Na2—W1ⁱⁱⁱ	85.747 (15)
O1—W1—O2	112.50 (4)	Na2^vi—Na2—W1ⁱⁱⁱ	60.574 (14)
O3—W1—Na2ⁱ	141.38 (3)	W1^v—Na2—W1ⁱⁱⁱ	122.214 (17)
O4—W1—Na2ⁱ	35.55 (3)	O2—Na2—Na1^iv	77.72 (2)
O1—W1—Na2ⁱ	102.36 (2)	O4ⁱⁱⁱ—Na2—Na1^iv	150.36 (2)
O2—W1—Na2ⁱ	80.32 (3)	O5^iv—Na2—Na1^iv	34.90 (2)
O3—W1—Na1	111.31 (3)	O4^v—Na2—Na1^iv	108.55 (2)
O4—W1—Na1	130.02 (2)	O6^vi—Na2—Na1^iv	65.70 (3)
O1—W1—Na1	30.91 (2)	O3^vii—Na2—Na1^iv	118.18 (3)
O2—W1—Na1	82.90 (3)	Na1—Na2—Na1^iv	154.348 (16)
Na2ⁱ—W1—Na1	106.915 (15)	Na1^vi—Na2—Na1^iv	87.641 (15)
O3—W1—Na2ⁱⁱ	103.91 (3)	Na2^vi—Na2—Na1^iv	144.05 (2)
O4—W1—Na2ⁱⁱ	33.60 (3)	W1^v—Na2—Na1^iv	100.837 (14)
O1—W1—Na2ⁱⁱ	79.92 (3)	W1ⁱⁱⁱ—Na2—Na1^iv	126.316 (15)
O2—W1—Na2ⁱⁱ	138.10 (2)	O5—Na1—O1	93.00 (3)
Na2ⁱ—W1—Na2ⁱⁱ	57.785 (17)	O5—Na1—O3^vii	154.61 (3)
Na1—W1—Na2ⁱⁱ	108.172 (15)	O1—Na1—O3^vii	91.76 (3)
O3—W1—Na1ⁱⁱ	84.71 (3)	O5—Na1—O4ⁱⁱⁱ	111.52 (3)
O4—W1—Na1ⁱⁱ	29.48 (2)	O1—Na1—O4ⁱⁱⁱ	94.68 (3)
O1—W1—Na1ⁱⁱ	133.55 (2)	O3^vii—Na1—O4ⁱⁱⁱ	92.90 (3)
O2—W1—Na1ⁱⁱ	104.49 (3)	O5—Na1—O6	87.41 (3)
Na2ⁱ—W1—Na1ⁱⁱ	56.819 (16)	O1—Na1—O6	176.92 (4)
Na1—W1—Na1ⁱⁱ	159.432 (5)	O3^vii—Na1—O6	86.59 (3)
Na2ⁱⁱ—W1—Na1ⁱⁱ	53.655 (16)	O4ⁱⁱⁱ—Na1—O6	88.00 (3)
O2—Na2—O4ⁱⁱⁱ	89.22 (3)	O5—Na1—Na2	157.62 (3)
O2—Na2—O5^iv	90.37 (3)	O1—Na1—Na2	88.00 (2)
O4ⁱⁱⁱ—Na2—O5^iv	174.01 (3)	O3^vii—Na1—Na2	47.48 (2)
O2—Na2—O4^v	173.54 (3)	O4ⁱⁱⁱ—Na1—Na2	46.17 (2)
O4ⁱⁱⁱ—Na2—O4^v	85.89 (3)	O6—Na1—Na2	92.79 (3)
O5^iv—Na2—O4^v	94.06 (3)	O5—Na1—Na2^vi	104.15 (3)
O2—Na2—O6^vi	99.81 (3)	O1—Na1—Na2^vi	138.27 (3)
O4ⁱⁱⁱ—Na2—O6^vi	91.04 (3)	O3^vii—Na1—Na2^vi	88.49 (3)
O5^iv—Na2—O6^vi	94.92 (3)	O4ⁱⁱⁱ—Na1—Na2^vi	43.68 (2)
O4^v—Na2—O6^vi	84.51 (3)	O6—Na1—Na2^vi	44.35 (2)
O2—Na2—O3^vii	89.93 (3)	Na2—Na1—Na2^vi	62.265 (15)
O4ⁱⁱⁱ—Na2—O3^vii	87.88 (3)	O5—Na1—W1	115.65 (3)
O5^iv—Na2—O3^vii	86.14 (3)	O1—Na1—W1	23.476 (19)
O4^v—Na2—O3^vii	85.68 (3)	O3^vii—Na1—W1	73.82 (3)
O6^vi—Na2—O3^vii	170.18 (3)	O4ⁱⁱⁱ—Na1—W1	80.70 (3)
O2—Na2—Na1	83.26 (2)	O6—Na1—W1	156.71 (3)
O4ⁱⁱⁱ—Na2—Na1	44.40 (2)	Na2—Na1—W1	64.748 (16)
O5^iv—Na2—Na1	129.63 (3)	Na2^vi—Na1—W1	120.955 (19)
O4^v—Na2—Na1	90.29 (2)	O5—Na1—W1ⁱⁱⁱ	95.45 (3)
O6^vi—Na2—Na1	135.43 (3)	O1—Na1—W1ⁱⁱⁱ	80.41 (3)
O3^vii—Na2—Na1	44.17 (2)	O3^vii—Na1—W1ⁱⁱⁱ	109.94 (3)
O2—Na2—Na1^vi	142.27 (3)	O4ⁱⁱⁱ—Na1—W1ⁱⁱⁱ	22.046 (17)
O4ⁱⁱⁱ—Na2—Na1^vi	86.77 (2)	O6—Na1—W1ⁱⁱⁱ	102.59 (3)
O5^iv—Na2—Na1^vi	97.18 (3)	Na2—Na1—W1ⁱⁱⁱ	62.646 (14)
O4^v—Na2—Na1^vi	41.67 (2)	Na2^vi—Na1—W1ⁱⁱⁱ	60.554 (14)
O6^vi—Na2—Na1^vi	42.86 (2)	W1—Na1—W1ⁱⁱⁱ	73.433 (17)
O3^vii—Na2—Na1^vi	127.32 (3)	O5—Na1—Na2^viii	36.93 (2)
Na1—Na2—Na1^vi	117.734 (15)	O1—Na1—Na2^viii	101.14 (3)
O2—Na2—Na2^vi	132.22 (3)	O3^vii—Na1—Na2^viii	117.72 (3)
O4ⁱⁱⁱ—Na2—Na2^vi	43.14 (2)	O4ⁱⁱⁱ—Na1—Na2^viii	144.65 (3)
O5^iv—Na2—Na2^vi	136.49 (3)	O6—Na1—Na2^viii	77.39 (2)
O4^v—Na2—Na2^vi	42.74 (2)	Na2—Na1—Na2^viii	163.411 (15)
O6^vi—Na2—Na2^vi	86.94 (3)	Na2^vi—Na1—Na2^viii	115.487 (16)
O3^vii—Na2—Na2^vi	85.60 (3)	W1—Na1—Na2^viii	122.709 (18)
Na1—Na2—Na2^vi	61.13 (2)	W1ⁱⁱⁱ—Na1—Na2^viii	132.188 (15)
Na1^vi—Na2—Na2^vi	56.60 (2)	W1—O1—Na1	125.61 (4)
O2—Na2—W1^v	153.96 (3)	W1—O2—Na2	127.43 (4)
O4ⁱⁱⁱ—Na2—W1^v	102.30 (2)	W1—O3—Na1^vii	132.71 (4)
O5^iv—Na2—W1^v	75.75 (2)	W1—O3—Na2^vii	128.93 (4)
O4^v—Na2—W1^v	25.268 (17)	Na1^vii—O3—Na2^vii	88.36 (3)
O6^vi—Na2—W1^v	103.19 (3)	W1—O4—Na1ⁱⁱ	128.47 (4)
O3^vii—Na2—W1^v	67.57 (2)	W1—O4—Na2ⁱⁱ	122.24 (4)
Na1—Na2—W1^v	88.779 (15)	Na1ⁱⁱ—O4—Na2ⁱⁱ	89.43 (3)
Na1^vi—Na2—W1^v	62.627 (11)	W1—O4—Na2ⁱ	119.18 (4)
Na2^vi—Na2—W1^v	61.640 (14)	Na1ⁱⁱ—O4—Na2ⁱ	94.65 (3)
O2—Na2—W1ⁱⁱⁱ	75.92 (2)	Na2ⁱⁱ—O4—Na2ⁱ	94.11 (3)
O4ⁱⁱⁱ—Na2—W1ⁱⁱⁱ	24.160 (17)	Na1—O5—Na2^viii	108.17 (4)
O5^iv—Na2—W1ⁱⁱⁱ	160.21 (2)	Na1—O6—Na2^vi	92.79 (3)

Symmetry codes: (i) −x+1/2, y−1/2, z; (ii) x+1/2, −y+1/2, −z+1; (iii) x−1/2, −y+1/2, −z+1; (iv) −x+1/2, −y+1, z+1/2; (v) −x+1/2, y+1/2, z; (vi) −x, −y+1, −z+1; (vii) −x+1, −y+1, −z+1; (viii) −x+1/2, −y+1, z−1/2.

4-(Ag) top

Crystal data top

C₄CoSc₃	F(000) = 228
M_r = 241.85	D_x = 4.511 Mg m⁻³
Orthorhombic, Immm	Ag Kα radiation, λ = 0.56086 Å
a = 3.394 (2) Å	Cell parameters from 9877 reflections
b = 4.374 (2) Å	θ = 2.7–66.4°
c = 11.995 (3) Å	µ = 5.02 mm⁻¹
V = 178.07 (14) Å³	T = 100 K
Z = 2	0.08 × 0.05 × 0.05 mm

Data collection top

Bruker Smart APEX II Quazar diffractometer	1463 reflections with I > 2σ(I)
Radiation source: INCOATEC Microsource	R_int = 0.027
ω scans	θ_max = 67.6°, θ_min = 2.7°
Absorption correction: multi-scan SADABS-2014/4	h = −10→9
T_min = 0.738, T_max = 0.830	k = −12→12
25448 measured reflections	l = −39→33
1590 independent reflections

Refinement top

Refinement on F²	0 restraints
Least-squares matrix: full	w = 1/[σ²(F_o²) + (0.0156P)² + 0.0264P] where P = (F_o² + 2F_c²)/3
R[F² > 2σ(F²)] = 0.015	(Δ/σ)_max = 0.002
wR(F²) = 0.032	Δρ_max = 1.18 e Å⁻³
S = 1.10	Δρ_min = −1.05 e Å⁻³
1590 reflections	Extinction correction: SHELXL, Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
18 parameters	Extinction coefficient: 0.067 (3)

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Co	0.5000	0.0000	0.0000	0.00452 (1)
Sc1	0.0000	0.5000	0.0000	0.00408 (1)
Sc2	0.5000	0.5000	0.31199 (2)	0.00376 (1)
C	0.5000	0.33380 (7)	0.12484 (2)	0.00485 (3)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Co	0.00678 (2)	0.00344 (2)	0.00332 (2)	0.000	0.000	0.000
Sc1	0.00390 (2)	0.00428 (3)	0.00408 (2)	0.000	0.000	0.000
Sc2	0.00400 (2)	0.00364 (2)	0.00366 (2)	0.000	0.000	0.000
C	0.00560 (6)	0.00438 (7)	0.00456 (6)	0.000	0.000	0.00033 (5)

Geometric parameters (Å, º) top

Co—C	2.0914 (6)	Sc1—Co^xv	2.7682 (10)
Co—Cⁱ	2.0914 (6)	Sc1—Co^xvii	2.7682 (10)
Co—Cⁱⁱ	2.0914 (6)	Sc1—Co^xviii	2.7682 (10)
Co—Cⁱⁱⁱ	2.0914 (6)	Sc2—C^xii	2.3596 (6)
Co—Sc1^iv	2.7682 (10)	Sc2—C	2.3596 (6)
Co—Sc1^v	2.7682 (10)	Sc2—C^xix	2.3634 (9)
Co—Sc1^vi	2.7682 (10)	Sc2—C^ix	2.3634 (9)
Co—Sc1	2.7682 (10)	Sc2—C^viii	2.3634 (9)
Co—Sc2^vii	2.8224 (8)	Sc2—C^xx	2.3634 (9)
Co—Sc2^viii	2.8224 (8)	Sc2—Co^xxi	2.8224 (8)
Co—Sc2^ix	2.8224 (8)	Sc2—Co^xxii	2.8224 (8)
Co—Sc2^x	2.8224 (8)	Sc2—Sc1^xxi	3.1415 (8)
Sc1—C	2.3771 (8)	Sc2—Sc1^xxiii	3.1415 (8)
Sc1—C^xi	2.3771 (8)	Sc2—Sc2^ix	3.1423 (9)
Sc1—C^xii	2.3771 (8)	Sc2—Sc2^xxiv	3.1423 (9)
Sc1—C^xiii	2.3771 (8)	C—C^xii	1.4540 (9)
Sc1—C^xiv	2.3771 (8)	C—Sc2^ix	2.3634 (9)
Sc1—C^xv	2.3771 (8)	C—Sc2^viii	2.3634 (9)
Sc1—Cⁱⁱ	2.3771 (8)	C—Sc1^v	2.3771 (8)
Sc1—C^xvi	2.3771 (8)

C—Co—Cⁱ	180.0	Co^xv—Sc1—Co^xvii	180.0
C—Co—Cⁱⁱ	91.45 (3)	C—Sc1—Co	47.214 (15)
Cⁱ—Co—Cⁱⁱ	88.55 (3)	C^xi—Sc1—Co	101.30 (3)
C—Co—Cⁱⁱⁱ	88.55 (3)	C^xii—Sc1—Co	78.70 (3)
Cⁱ—Co—Cⁱⁱⁱ	91.45 (3)	C^xiii—Sc1—Co	132.786 (15)
Cⁱⁱ—Co—Cⁱⁱⁱ	180.000 (16)	C^xiv—Sc1—Co	78.70 (3)
C—Co—Sc1^iv	123.473 (19)	C^xv—Sc1—Co	101.30 (3)
Cⁱ—Co—Sc1^iv	56.528 (19)	Cⁱⁱ—Sc1—Co	47.214 (15)
Cⁱⁱ—Co—Sc1^iv	123.472 (19)	C^xvi—Sc1—Co	132.786 (15)
Cⁱⁱⁱ—Co—Sc1^iv	56.528 (19)	Co^xv—Sc1—Co	75.62 (4)
C—Co—Sc1^v	56.527 (19)	Co^xvii—Sc1—Co	104.38 (4)
Cⁱ—Co—Sc1^v	123.472 (19)	C—Sc1—Co^xviii	132.786 (16)
Cⁱⁱ—Co—Sc1^v	56.528 (19)	C^xi—Sc1—Co^xviii	78.70 (3)
Cⁱⁱⁱ—Co—Sc1^v	123.472 (19)	C^xii—Sc1—Co^xviii	101.30 (3)
Sc1^iv—Co—Sc1^v	180.0	C^xiii—Sc1—Co^xviii	47.214 (15)
C—Co—Sc1^vi	123.473 (19)	C^xiv—Sc1—Co^xviii	101.30 (3)
Cⁱ—Co—Sc1^vi	56.528 (19)	C^xv—Sc1—Co^xviii	78.70 (3)
Cⁱⁱ—Co—Sc1^vi	123.472 (19)	Cⁱⁱ—Sc1—Co^xviii	132.786 (15)
Cⁱⁱⁱ—Co—Sc1^vi	56.528 (19)	C^xvi—Sc1—Co^xviii	47.214 (15)
Sc1^iv—Co—Sc1^vi	75.62 (4)	Co^xv—Sc1—Co^xviii	104.38 (4)
Sc1^v—Co—Sc1^vi	104.38 (4)	Co^xvii—Sc1—Co^xviii	75.62 (4)
C—Co—Sc1	56.527 (19)	Co—Sc1—Co^xviii	180.0
Cⁱ—Co—Sc1	123.472 (19)	C^xii—Sc2—C	35.89 (2)
Cⁱⁱ—Co—Sc1	56.528 (19)	C^xii—Sc2—C^xix	96.586 (16)
Cⁱⁱⁱ—Co—Sc1	123.472 (19)	C—Sc2—C^xix	119.693 (13)
Sc1^iv—Co—Sc1	104.38 (4)	C^xii—Sc2—C^ix	119.694 (13)
Sc1^v—Co—Sc1	75.62 (4)	C—Sc2—C^ix	96.587 (16)
Sc1^vi—Co—Sc1	180.0	C^xix—Sc2—C^ix	142.60 (2)
C—Co—Sc2^vii	124.898 (16)	C^xii—Sc2—C^viii	119.694 (13)
Cⁱ—Co—Sc2^vii	55.102 (16)	C—Sc2—C^viii	96.587 (16)
Cⁱⁱ—Co—Sc2^vii	55.102 (16)	C^xix—Sc2—C^viii	76.31 (4)
Cⁱⁱⁱ—Co—Sc2^vii	124.898 (16)	C^ix—Sc2—C^viii	91.78 (4)
Sc1^iv—Co—Sc2^vii	68.371 (19)	C^xii—Sc2—C^xx	96.586 (16)
Sc1^v—Co—Sc2^vii	111.629 (19)	C—Sc2—C^xx	119.693 (13)
Sc1^vi—Co—Sc2^vii	111.629 (18)	C^xix—Sc2—C^xx	91.78 (4)
Sc1—Co—Sc2^vii	68.371 (18)	C^ix—Sc2—C^xx	76.31 (4)
C—Co—Sc2^viii	55.102 (16)	C^viii—Sc2—C^xx	142.60 (2)
Cⁱ—Co—Sc2^viii	124.898 (16)	C^xii—Sc2—Co^xxi	139.480 (16)
Cⁱⁱ—Co—Sc2^viii	124.898 (16)	C—Sc2—Co^xxi	139.480 (16)
Cⁱⁱⁱ—Co—Sc2^viii	55.102 (16)	C^xix—Sc2—Co^xxi	46.534 (17)
Sc1^iv—Co—Sc2^viii	111.629 (19)	C^ix—Sc2—Co^xxi	100.11 (3)
Sc1^v—Co—Sc2^viii	68.371 (19)	C^viii—Sc2—Co^xxi	46.534 (17)
Sc1^vi—Co—Sc2^viii	68.371 (18)	C^xx—Sc2—Co^xxi	100.11 (3)
Sc1—Co—Sc2^viii	111.629 (18)	C^xii—Sc2—Co^xxii	139.480 (16)
Sc2^vii—Co—Sc2^viii	180.0	C—Sc2—Co^xxii	139.480 (17)
C—Co—Sc2^ix	55.102 (16)	C^xix—Sc2—Co^xxii	100.11 (3)
Cⁱ—Co—Sc2^ix	124.898 (16)	C^ix—Sc2—Co^xxii	46.534 (17)
Cⁱⁱ—Co—Sc2^ix	124.898 (16)	C^viii—Sc2—Co^xxii	100.11 (3)
Cⁱⁱⁱ—Co—Sc2^ix	55.102 (16)	C^xx—Sc2—Co^xxii	46.534 (17)
Sc1^iv—Co—Sc2^ix	68.371 (18)	Co^xxi—Sc2—Co^xxii	73.92 (4)
Sc1^v—Co—Sc2^ix	111.629 (18)	C^xii—Sc2—Sc1^xxi	117.94 (2)
Sc1^vi—Co—Sc2^ix	111.629 (18)	C—Sc2—Sc1^xxi	153.824 (10)
Sc1—Co—Sc2^ix	68.371 (18)	C^xix—Sc2—Sc1^xxi	48.682 (19)
Sc2^vii—Co—Sc2^ix	106.08 (4)	C^ix—Sc2—Sc1^xxi	101.53 (2)
Sc2^viii—Co—Sc2^ix	73.92 (4)	C^viii—Sc2—Sc1^xxi	101.53 (2)
C—Co—Sc2^x	124.898 (16)	C^xx—Sc2—Sc1^xxi	48.682 (19)
Cⁱ—Co—Sc2^x	55.102 (16)	Co^xxi—Sc2—Sc1^xxi	54.997 (15)
Cⁱⁱ—Co—Sc2^x	55.102 (16)	Co^xxii—Sc2—Sc1^xxi	54.997 (15)
Cⁱⁱⁱ—Co—Sc2^x	124.898 (16)	C^xii—Sc2—Sc1^xxiii	153.825 (10)
Sc1^iv—Co—Sc2^x	111.629 (18)	C—Sc2—Sc1^xxiii	117.94 (2)
Sc1^v—Co—Sc2^x	68.371 (18)	C^xix—Sc2—Sc1^xxiii	101.53 (2)
Sc1^vi—Co—Sc2^x	68.371 (18)	C^ix—Sc2—Sc1^xxiii	48.682 (18)
Sc1—Co—Sc2^x	111.629 (18)	C^viii—Sc2—Sc1^xxiii	48.682 (19)
Sc2^vii—Co—Sc2^x	73.92 (4)	C^xx—Sc2—Sc1^xxiii	101.53 (2)
Sc2^viii—Co—Sc2^x	106.08 (4)	Co^xxi—Sc2—Sc1^xxiii	54.997 (15)
Sc2^ix—Co—Sc2^x	180.0	Co^xxii—Sc2—Sc1^xxiii	54.997 (15)
C—Sc1—C^xi	144.38 (2)	Sc1^xxi—Sc2—Sc1^xxiii	88.24 (3)
C—Sc1—C^xii	35.62 (2)	C^xii—Sc2—Sc2^ix	76.362 (19)
C^xi—Sc1—C^xii	180.000 (10)	C—Sc2—Sc2^ix	48.345 (11)
C—Sc1—C^xiii	180.0	C^xix—Sc2—Sc2^ix	165.802 (7)
C^xi—Sc1—C^xiii	35.62 (2)	C^ix—Sc2—Sc2^ix	48.242 (19)
C^xii—Sc1—C^xiii	144.38 (2)	C^viii—Sc2—Sc2^ix	96.29 (4)
C—Sc1—C^xiv	88.90 (4)	C^xx—Sc2—Sc2^ix	101.18 (4)
C^xi—Sc1—C^xiv	101.91 (3)	Co^xxi—Sc2—Sc2^ix	134.656 (16)
C^xii—Sc1—C^xiv	78.09 (3)	Co^xxii—Sc2—Sc2^ix	93.06 (3)
C^xiii—Sc1—C^xiv	91.10 (4)	Sc1^xxi—Sc2—Sc2^ix	145.513 (17)
C—Sc1—C^xv	91.10 (4)	Sc1^xxiii—Sc2—Sc2^ix	81.68 (2)
C^xi—Sc1—C^xv	78.09 (3)	C^xii—Sc2—Sc2^xxiv	48.344 (11)
C^xii—Sc1—C^xv	101.91 (3)	C—Sc2—Sc2^xxiv	76.362 (19)
C^xiii—Sc1—C^xv	88.90 (4)	C^xix—Sc2—Sc2^xxiv	48.242 (19)
C^xiv—Sc1—C^xv	180.0	C^ix—Sc2—Sc2^xxiv	165.802 (6)
C—Sc1—Cⁱⁱ	78.09 (3)	C^viii—Sc2—Sc2^xxiv	101.18 (4)
C^xi—Sc1—Cⁱⁱ	91.10 (4)	C^xx—Sc2—Sc2^xxiv	96.29 (3)
C^xii—Sc1—Cⁱⁱ	88.90 (4)	Co^xxi—Sc2—Sc2^xxiv	93.06 (3)
C^xiii—Sc1—Cⁱⁱ	101.91 (3)	Co^xxii—Sc2—Sc2^xxiv	134.656 (16)
C^xiv—Sc1—Cⁱⁱ	35.62 (2)	Sc1^xxi—Sc2—Sc2^xxiv	81.68 (3)
C^xv—Sc1—Cⁱⁱ	144.38 (2)	Sc1^xxiii—Sc2—Sc2^xxiv	145.513 (17)
C—Sc1—C^xvi	101.91 (3)	Sc2^ix—Sc2—Sc2^xxiv	123.51 (2)
C^xi—Sc1—C^xvi	88.90 (4)	C^xii—C—Co	134.276 (17)
C^xii—Sc1—C^xvi	91.10 (4)	C^xii—C—Sc2	72.055 (11)
C^xiii—Sc1—C^xvi	78.09 (3)	Co—C—Sc2	153.669 (16)
C^xiv—Sc1—C^xvi	144.38 (2)	C^xii—C—Sc2^ix	128.15 (2)
C^xv—Sc1—C^xvi	35.62 (2)	Co—C—Sc2^ix	78.36 (2)
Cⁱⁱ—Sc1—C^xvi	180.000 (14)	Sc2—C—Sc2^ix	83.414 (16)
C—Sc1—Co^xv	101.30 (3)	C^xii—C—Sc2^viii	128.15 (2)
C^xi—Sc1—Co^xv	47.214 (15)	Co—C—Sc2^viii	78.36 (2)
C^xii—Sc1—Co^xv	132.786 (15)	Sc2—C—Sc2^viii	83.414 (16)
C^xiii—Sc1—Co^xv	78.70 (3)	Sc2^ix—C—Sc2^viii	91.78 (4)
C^xiv—Sc1—Co^xv	132.786 (15)	C^xii—C—Sc1	72.193 (12)
C^xv—Sc1—Co^xv	47.214 (15)	Co—C—Sc1	76.26 (2)
Cⁱⁱ—Sc1—Co^xv	101.30 (3)	Sc2—C—Sc1	120.336 (18)
C^xvi—Sc1—Co^xv	78.70 (3)	Sc2^ix—C—Sc1	83.01 (3)
C—Sc1—Co^xvii	78.70 (3)	Sc2^viii—C—Sc1	154.622 (16)
C^xi—Sc1—Co^xvii	132.786 (15)	C^xii—C—Sc1^v	72.193 (12)
C^xii—Sc1—Co^xvii	47.214 (15)	Co—C—Sc1^v	76.26 (2)
C^xiii—Sc1—Co^xvii	101.30 (3)	Sc2—C—Sc1^v	120.336 (18)
C^xiv—Sc1—Co^xvii	47.214 (15)	Sc2^ix—C—Sc1^v	154.622 (16)
C^xv—Sc1—Co^xvii	132.786 (15)	Sc2^viii—C—Sc1^v	83.01 (3)
Cⁱⁱ—Sc1—Co^xvii	78.70 (3)	Sc1—C—Sc1^v	91.11 (4)
C^xvi—Sc1—Co^xvii	101.30 (3)

Symmetry codes: (i) −x+1, −y, −z; (ii) x, y, −z; (iii) −x+1, −y, z; (iv) x, y−1, z; (v) x+1, y, z; (vi) x+1, y−1, z; (vii) x−1/2, y−1/2, z−1/2; (viii) −x+3/2, −y+1/2, −z+1/2; (ix) −x+1/2, −y+1/2, −z+1/2; (x) x+1/2, y−1/2, z−1/2; (xi) x−1, y, −z; (xii) −x+1, −y+1, z; (xiii) −x, −y+1, −z; (xiv) −x+1, −y+1, −z; (xv) x−1, y, z; (xvi) −x, −y+1, z; (xvii) x, y+1, z; (xviii) x−1, y+1, z; (xix) x+1/2, y+1/2, −z+1/2; (xx) x−1/2, y+1/2, −z+1/2; (xxi) x+1/2, y+1/2, z+1/2; (xxii) x−1/2, y+1/2, z+1/2; (xxiii) x+1/2, y−1/2, z+1/2; (xxiv) −x+3/2, −y+3/2, −z+1/2.

4-(Mo) top

Crystal data top

C₄CoSc₃	F(000) = 228
M_r = 241.85	D_x = 4.499 Mg m⁻³
Orthorhombic, Immm	Mo Kα radiation, λ = 0.71073 Å
a = 3.398 (2) Å	Cell parameters from 9548 reflections
b = 4.377 (2) Å	θ = 3.4–55.8°
c = 12.003 (3) Å	µ = 9.79 mm⁻¹
V = 178.52 (14) Å³	T = 100 K
Z = 2	0.08 × 0.05 × 0.05 mm

Data collection top

Bruker Smart APEX II Quazar diffractometer	699 reflections with I > 2σ(I)
Radiation source: INCOATEC Microsource	R_int = 0.020
ω scans	θ_max = 55.8°, θ_min = 3.4°
Absorption correction: multi-scan SADABS-2014/4	h = −7→7
T_min = 0.576, T_max = 0.701	k = −10→9
11104 measured reflections	l = −27→27
704 independent reflections

Refinement top

Refinement on F²	0 restraints
Least-squares matrix: full	w = 1/[σ²(F_o²) + (0.0174P)² + 0.0528P] where P = (F_o² + 2F_c²)/3
R[F² > 2σ(F²)] = 0.012	(Δ/σ)_max = 0.002
wR(F²) = 0.033	Δρ_max = 0.96 e Å⁻³
S = 1.28	Δρ_min = −0.74 e Å⁻³
704 reflections	Extinction correction: SHELXL, Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
18 parameters	Extinction coefficient: 0.046 (3)

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Co	0.5000	0.0000	0.0000	0.00478 (3)
Sc1	0.0000	0.5000	0.0000	0.00436 (3)
Sc2	0.5000	0.5000	0.31198 (2)	0.00404 (3)
C	0.5000	0.33377 (11)	0.12480 (4)	0.00511 (5)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Co	0.00724 (5)	0.00349 (4)	0.00362 (4)	0.000	0.000	0.000
Sc1	0.00431 (5)	0.00439 (5)	0.00439 (5)	0.000	0.000	0.000
Sc2	0.00444 (4)	0.00370 (4)	0.00399 (4)	0.000	0.000	0.000
C	0.00601 (12)	0.00438 (12)	0.00494 (12)	0.000	0.000	0.00030 (9)

Geometric parameters (Å, º) top

Co—Cⁱ	2.0924 (7)	Sc1—Co^xv	2.7706 (10)
Co—Cⁱⁱ	2.0924 (7)	Sc1—Co^xvii	2.7706 (10)
Co—Cⁱⁱⁱ	2.0924 (7)	Sc1—Co^xviii	2.7706 (10)
Co—C	2.0924 (7)	Sc2—C	2.3616 (7)
Co—Sc1^iv	2.7706 (10)	Sc2—C^xii	2.3616 (7)
Co—Sc1^v	2.7706 (10)	Sc2—C^xix	2.3657 (9)
Co—Sc1^vi	2.7706 (10)	Sc2—C^x	2.3657 (9)
Co—Sc1	2.7706 (10)	Sc2—C^xx	2.3657 (9)
Co—Sc2^vii	2.8248 (8)	Sc2—C^viii	2.3657 (9)
Co—Sc2^viii	2.8248 (8)	Sc2—Co^xxi	2.8249 (8)
Co—Sc2^ix	2.8248 (8)	Sc2—Co^xxii	2.8249 (8)
Co—Sc2^x	2.8248 (8)	Sc2—Sc1^xxi	3.1437 (8)
Sc1—C^xi	2.3791 (8)	Sc2—Sc1^xxiii	3.1437 (8)
Sc1—C^xii	2.3791 (8)	Sc2—Sc2^x	3.1448 (9)
Sc1—C^xiii	2.3791 (8)	Sc2—Sc2^xxiv	3.1448 (9)
Sc1—C^xiv	2.3791 (8)	C—C^xii	1.4552 (11)
Sc1—C^xv	2.3791 (8)	C—Sc2^x	2.3657 (9)
Sc1—Cⁱⁱ	2.3791 (8)	C—Sc2^viii	2.3657 (9)
Sc1—C^xvi	2.3791 (8)	C—Sc1^v	2.3791 (8)
Sc1—C	2.3791 (8)

Cⁱ—Co—Cⁱⁱ	88.56 (4)	Co^xv—Sc1—Co^xvii	180.0
Cⁱ—Co—Cⁱⁱⁱ	91.44 (4)	C^xi—Sc1—Co	101.32 (3)
Cⁱⁱ—Co—Cⁱⁱⁱ	180.00 (2)	C^xii—Sc1—Co	78.68 (3)
Cⁱ—Co—C	180.000 (17)	C^xiii—Sc1—Co	132.806 (17)
Cⁱⁱ—Co—C	91.44 (4)	C^xiv—Sc1—Co	78.68 (3)
Cⁱⁱⁱ—Co—C	88.56 (4)	C^xv—Sc1—Co	101.32 (3)
Cⁱ—Co—Sc1^iv	56.53 (2)	Cⁱⁱ—Sc1—Co	47.194 (18)
Cⁱⁱ—Co—Sc1^iv	123.47 (2)	C^xvi—Sc1—Co	132.806 (17)
Cⁱⁱⁱ—Co—Sc1^iv	56.53 (2)	C—Sc1—Co	47.194 (18)
C—Co—Sc1^iv	123.47 (2)	Co^xv—Sc1—Co	75.65 (4)
Cⁱ—Co—Sc1^v	123.47 (2)	Co^xvii—Sc1—Co	104.35 (4)
Cⁱⁱ—Co—Sc1^v	56.53 (2)	C^xi—Sc1—Co^xviii	78.68 (3)
Cⁱⁱⁱ—Co—Sc1^v	123.47 (2)	C^xii—Sc1—Co^xviii	101.32 (3)
C—Co—Sc1^v	56.53 (2)	C^xiii—Sc1—Co^xviii	47.194 (17)
Sc1^iv—Co—Sc1^v	180.0	C^xiv—Sc1—Co^xviii	101.32 (3)
Cⁱ—Co—Sc1^vi	56.53 (2)	C^xv—Sc1—Co^xviii	78.68 (3)
Cⁱⁱ—Co—Sc1^vi	123.47 (2)	Cⁱⁱ—Sc1—Co^xviii	132.806 (17)
Cⁱⁱⁱ—Co—Sc1^vi	56.53 (2)	C^xvi—Sc1—Co^xviii	47.194 (18)
C—Co—Sc1^vi	123.47 (2)	C—Sc1—Co^xviii	132.806 (17)
Sc1^iv—Co—Sc1^vi	75.65 (4)	Co^xv—Sc1—Co^xviii	104.35 (4)
Sc1^v—Co—Sc1^vi	104.35 (4)	Co^xvii—Sc1—Co^xviii	75.65 (4)
Cⁱ—Co—Sc1	123.47 (2)	Co—Sc1—Co^xviii	180.0
Cⁱⁱ—Co—Sc1	56.53 (2)	C—Sc2—C^xii	35.89 (3)
Cⁱⁱⁱ—Co—Sc1	123.47 (2)	C—Sc2—C^xix	119.697 (15)
C—Co—Sc1	56.53 (2)	C^xii—Sc2—C^xix	96.597 (18)
Sc1^iv—Co—Sc1	104.35 (4)	C—Sc2—C^x	96.597 (18)
Sc1^v—Co—Sc1	75.65 (4)	C^xii—Sc2—C^x	119.697 (15)
Sc1^vi—Co—Sc1	180.0	C^xix—Sc2—C^x	142.58 (3)
Cⁱ—Co—Sc2^vii	55.113 (17)	C—Sc2—C^xx	119.697 (16)
Cⁱⁱ—Co—Sc2^vii	55.113 (17)	C^xii—Sc2—C^xx	96.597 (19)
Cⁱⁱⁱ—Co—Sc2^vii	124.887 (17)	C^xix—Sc2—C^xx	91.81 (4)
C—Co—Sc2^vii	124.887 (17)	C^x—Sc2—C^xx	76.27 (4)
Sc1^iv—Co—Sc2^vii	68.357 (18)	C—Sc2—C^viii	96.597 (19)
Sc1^v—Co—Sc2^vii	111.643 (19)	C^xii—Sc2—C^viii	119.697 (15)
Sc1^vi—Co—Sc2^vii	111.643 (18)	C^xix—Sc2—C^viii	76.27 (4)
Sc1—Co—Sc2^vii	68.357 (18)	C^x—Sc2—C^viii	91.81 (4)
Cⁱ—Co—Sc2^viii	124.887 (17)	C^xx—Sc2—C^viii	142.58 (3)
Cⁱⁱ—Co—Sc2^viii	124.887 (17)	C—Sc2—Co^xxi	139.468 (16)
Cⁱⁱⁱ—Co—Sc2^viii	55.113 (17)	C^xii—Sc2—Co^xxi	139.468 (17)
C—Co—Sc2^viii	55.113 (17)	C^xix—Sc2—Co^xxi	46.512 (19)
Sc1^iv—Co—Sc2^viii	111.643 (19)	C^x—Sc2—Co^xxi	100.12 (3)
Sc1^v—Co—Sc2^viii	68.357 (18)	C^xx—Sc2—Co^xxi	100.12 (3)
Sc1^vi—Co—Sc2^viii	68.357 (18)	C^viii—Sc2—Co^xxi	46.512 (19)
Sc1—Co—Sc2^viii	111.643 (18)	C—Sc2—Co^xxii	139.468 (17)
Sc2^vii—Co—Sc2^viii	180.0	C^xii—Sc2—Co^xxii	139.468 (17)
Cⁱ—Co—Sc2^ix	55.113 (17)	C^xix—Sc2—Co^xxii	100.12 (3)
Cⁱⁱ—Co—Sc2^ix	55.113 (17)	C^x—Sc2—Co^xxii	46.512 (19)
Cⁱⁱⁱ—Co—Sc2^ix	124.887 (17)	C^xx—Sc2—Co^xxii	46.512 (19)
C—Co—Sc2^ix	124.887 (17)	C^viii—Sc2—Co^xxii	100.12 (3)
Sc1^iv—Co—Sc2^ix	111.643 (18)	Co^xxi—Sc2—Co^xxii	73.95 (4)
Sc1^v—Co—Sc2^ix	68.357 (18)	C—Sc2—Sc1^xxi	153.825 (13)
Sc1^vi—Co—Sc2^ix	68.357 (18)	C^xii—Sc2—Sc1^xxi	117.94 (3)
Sc1—Co—Sc2^ix	111.643 (18)	C^xix—Sc2—Sc1^xxi	48.69 (2)
Sc2^vii—Co—Sc2^ix	73.95 (4)	C^x—Sc2—Sc1^xxi	101.52 (2)
Sc2^viii—Co—Sc2^ix	106.05 (4)	C^xx—Sc2—Sc1^xxi	48.69 (2)
Cⁱ—Co—Sc2^x	124.887 (17)	C^viii—Sc2—Sc1^xxi	101.52 (2)
Cⁱⁱ—Co—Sc2^x	124.887 (17)	Co^xxi—Sc2—Sc1^xxi	55.003 (15)
Cⁱⁱⁱ—Co—Sc2^x	55.113 (17)	Co^xxii—Sc2—Sc1^xxi	55.003 (15)
C—Co—Sc2^x	55.113 (17)	C—Sc2—Sc1^xxiii	117.94 (3)
Sc1^iv—Co—Sc2^x	68.357 (18)	C^xii—Sc2—Sc1^xxiii	153.826 (13)
Sc1^v—Co—Sc2^x	111.643 (18)	C^xix—Sc2—Sc1^xxiii	101.52 (2)
Sc1^vi—Co—Sc2^x	111.643 (18)	C^x—Sc2—Sc1^xxiii	48.69 (2)
Sc1—Co—Sc2^x	68.357 (18)	C^xx—Sc2—Sc1^xxiii	101.52 (2)
Sc2^vii—Co—Sc2^x	106.05 (4)	C^viii—Sc2—Sc1^xxiii	48.69 (2)
Sc2^viii—Co—Sc2^x	73.95 (4)	Co^xxi—Sc2—Sc1^xxiii	55.003 (15)
Sc2^ix—Co—Sc2^x	180.0	Co^xxii—Sc2—Sc1^xxiii	55.003 (15)
C^xi—Sc1—C^xii	180.000 (16)	Sc1^xxi—Sc2—Sc1^xxiii	88.24 (3)
C^xi—Sc1—C^xiii	35.62 (3)	C—Sc2—Sc2^x	48.354 (12)
C^xii—Sc1—C^xiii	144.38 (3)	C^xii—Sc2—Sc2^x	76.37 (2)
C^xi—Sc1—C^xiv	101.95 (4)	C^xix—Sc2—Sc2^x	165.811 (10)
C^xii—Sc1—C^xiv	78.05 (4)	C^x—Sc2—Sc2^x	48.24 (2)
C^xiii—Sc1—C^xiv	91.15 (4)	C^xx—Sc2—Sc2^x	101.16 (4)
C^xi—Sc1—C^xv	78.05 (4)	C^viii—Sc2—Sc2^x	96.32 (4)
C^xii—Sc1—C^xv	101.95 (4)	Co^xxi—Sc2—Sc2^x	134.662 (16)
C^xiii—Sc1—C^xv	88.85 (4)	Co^xxii—Sc2—Sc2^x	93.04 (3)
C^xiv—Sc1—C^xv	180.0	Sc1^xxi—Sc2—Sc2^x	145.498 (16)
C^xi—Sc1—Cⁱⁱ	91.15 (4)	Sc1^xxiii—Sc2—Sc2^x	81.67 (2)
C^xii—Sc1—Cⁱⁱ	88.85 (4)	C—Sc2—Sc2^xxiv	76.37 (2)
C^xiii—Sc1—Cⁱⁱ	101.95 (4)	C^xii—Sc2—Sc2^xxiv	48.354 (13)
C^xiv—Sc1—Cⁱⁱ	35.62 (3)	C^xix—Sc2—Sc2^xxiv	48.24 (2)
C^xv—Sc1—Cⁱⁱ	144.38 (3)	C^x—Sc2—Sc2^xxiv	165.811 (10)
C^xi—Sc1—C^xvi	88.85 (4)	C^xx—Sc2—Sc2^xxiv	96.32 (4)
C^xii—Sc1—C^xvi	91.15 (4)	C^viii—Sc2—Sc2^xxiv	101.16 (4)
C^xiii—Sc1—C^xvi	78.05 (4)	Co^xxi—Sc2—Sc2^xxiv	93.04 (3)
C^xiv—Sc1—C^xvi	144.38 (3)	Co^xxii—Sc2—Sc2^xxiv	134.662 (16)
C^xv—Sc1—C^xvi	35.62 (3)	Sc1^xxi—Sc2—Sc2^xxiv	81.67 (2)
Cⁱⁱ—Sc1—C^xvi	180.00 (2)	Sc1^xxiii—Sc2—Sc2^xxiv	145.498 (17)
C^xi—Sc1—C	144.38 (3)	Sc2^x—Sc2—Sc2^xxiv	123.53 (2)
C^xii—Sc1—C	35.62 (3)	C^xii—C—Co	134.281 (19)
C^xiii—Sc1—C	180.0	C^xii—C—Sc2	72.055 (14)
C^xiv—Sc1—C	88.85 (4)	Co—C—Sc2	153.66 (2)
C^xv—Sc1—C	91.15 (4)	C^xii—C—Sc2^x	128.14 (2)
Cⁱⁱ—Sc1—C	78.05 (4)	Co—C—Sc2^x	78.37 (2)
C^xvi—Sc1—C	101.95 (4)	Sc2—C—Sc2^x	83.404 (19)
C^xi—Sc1—Co^xv	47.194 (17)	C^xii—C—Sc2^viii	128.14 (2)
C^xii—Sc1—Co^xv	132.806 (18)	Co—C—Sc2^viii	78.37 (2)
C^xiii—Sc1—Co^xv	78.68 (3)	Sc2—C—Sc2^viii	83.404 (19)
C^xiv—Sc1—Co^xv	132.806 (17)	Sc2^x—C—Sc2^viii	91.81 (4)
C^xv—Sc1—Co^xv	47.194 (18)	C^xii—C—Sc1	72.191 (14)
Cⁱⁱ—Sc1—Co^xv	101.32 (3)	Co—C—Sc1	76.28 (2)
C^xvi—Sc1—Co^xv	78.68 (3)	Sc2—C—Sc1	120.32 (2)
C—Sc1—Co^xv	101.32 (3)	Sc2^x—C—Sc1	82.99 (3)
C^xi—Sc1—Co^xvii	132.806 (18)	Sc2^viii—C—Sc1	154.65 (2)
C^xii—Sc1—Co^xvii	47.194 (18)	C^xii—C—Sc1^v	72.191 (15)
C^xiii—Sc1—Co^xvii	101.32 (3)	Co—C—Sc1^v	76.28 (2)
C^xiv—Sc1—Co^xvii	47.194 (18)	Sc2—C—Sc1^v	120.32 (2)
C^xv—Sc1—Co^xvii	132.806 (17)	Sc2^x—C—Sc1^v	154.65 (2)
Cⁱⁱ—Sc1—Co^xvii	78.68 (3)	Sc2^viii—C—Sc1^v	82.99 (3)
C^xvi—Sc1—Co^xvii	101.32 (3)	Sc1—C—Sc1^v	91.15 (4)
C—Sc1—Co^xvii	78.68 (3)

Symmetry codes: (i) −x+1, −y, −z; (ii) x, y, −z; (iii) −x+1, −y, z; (iv) x, y−1, z; (v) x+1, y, z; (vi) x+1, y−1, z; (vii) x−1/2, y−1/2, z−1/2; (viii) −x+3/2, −y+1/2, −z+1/2; (ix) x+1/2, y−1/2, z−1/2; (x) −x+1/2, −y+1/2, −z+1/2; (xi) x−1, y, −z; (xii) −x+1, −y+1, z; (xiii) −x, −y+1, −z; (xiv) −x+1, −y+1, −z; (xv) x−1, y, z; (xvi) −x, −y+1, z; (xvii) x, y+1, z; (xviii) x−1, y+1, z; (xix) x+1/2, y+1/2, −z+1/2; (xx) x−1/2, y+1/2, −z+1/2; (xxi) x+1/2, y+1/2, z+1/2; (xxii) x−1/2, y+1/2, z+1/2; (xxiii) x+1/2, y−1/2, z+1/2; (xxiv) −x+3/2, −y+3/2, −z+1/2.

5-(Ag) top

Crystal data top

C₁₆H₁₃Br₂N	F(000) = 744
M_r = 379.09	D_x = 1.835 Mg m⁻³
Monoclinic, P2₁/n	Ag Kα radiation, λ = 0.56086 Å
a = 9.601 (2) Å	Cell parameters from 9896 reflections
b = 8.377 (2) Å	θ = 2.6–20.9°
c = 17.201 (3) Å	µ = 3.16 mm⁻¹
β = 97.35 (2)°	T = 100 K
V = 1372.1 (5) Å³	0.20 × 0.16 × 0.15 mm
Z = 4

Data collection top

Bruker Smart APEX II Quazar diffractometer	2736 reflections with I > 2σ(I)
Radiation source: INCOATEC Microsource	R_int = 0.032
ω scans	θ_max = 20.9°, θ_min = 1.8°
Absorption correction: multi-scan SADABS-2014/4	h = −12→12
T_min = 0.648, T_max = 0.697	k = −10→10
53103 measured reflections	l = −21→21
2948 independent reflections

Refinement top

Refinement on F²	0 restraints
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.019	H-atom parameters constrained
wR(F²) = 0.049	w = 1/[σ²(F_o²) + (0.0233P)² + 1.4071P] where P = (F_o² + 2F_c²)/3
S = 1.07	(Δ/σ)_max = 0.002
2948 reflections	Δρ_max = 0.85 e Å⁻³
173 parameters	Δρ_min = −0.63 e Å⁻³

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Br1	0.49008 (2)	−0.01220 (2)	0.69965 (2)	0.02045 (6)
Br2	0.42857 (2)	−0.29652 (3)	0.48081 (2)	0.02535 (6)
N1	0.16189 (15)	−0.08661 (17)	0.57962 (9)	0.0136 (3)
C4	0.0234 (2)	0.0336 (2)	0.79109 (11)	0.0208 (4)
H4	−0.0054	0.0628	0.8400	0.025*
C3	0.1511 (2)	0.0952 (2)	0.76984 (11)	0.0188 (4)
H00E	0.2062	0.1653	0.8047	0.023*
C1	0.11300 (17)	−0.0517 (2)	0.64724 (10)	0.0132 (3)
C2	0.19582 (18)	0.0553 (2)	0.70021 (11)	0.0155 (3)
C7	−0.09670 (18)	−0.2165 (2)	0.61497 (11)	0.0151 (3)
C6	−0.01674 (18)	−0.1142 (2)	0.66830 (10)	0.0140 (3)
C5	−0.05846 (19)	−0.0666 (2)	0.74244 (11)	0.0180 (4)
H5	−0.1440	−0.1056	0.7575	0.022*
C8	−0.04826 (18)	−0.2483 (2)	0.54252 (11)	0.0143 (3)
C9	−0.12454 (19)	−0.3433 (2)	0.48222 (11)	0.0181 (4)
H00F	−0.2121	−0.3886	0.4905	0.022*
C10	−0.0730 (2)	−0.3696 (2)	0.41308 (11)	0.0204 (4)
H00H	−0.1256	−0.4317	0.3734	0.024*
C11	0.0583 (2)	−0.3050 (2)	0.39988 (11)	0.0197 (4)
H00G	0.0926	−0.3252	0.3514	0.024*
C12	0.13676 (19)	−0.2144 (2)	0.45524 (11)	0.0160 (4)
C13	0.08391 (18)	−0.1815 (2)	0.52841 (10)	0.0135 (3)
C14	−0.23209 (19)	−0.2891 (2)	0.63433 (12)	0.0195 (4)
H14	−0.3115	−0.2235	0.6115	0.029*
H00K	−0.2306	−0.2937	0.6914	0.029*
H00L	−0.2421	−0.3973	0.6126	0.029*
C15	0.32514 (18)	0.1282 (2)	0.67560 (11)	0.0179 (4)
H00A	0.3438	0.2315	0.7029	0.021*
H15	0.3096	0.1495	0.6185	0.021*
C16	0.27561 (19)	−0.1482 (2)	0.44095 (11)	0.0194 (4)
H16	0.2909	−0.0437	0.4676	0.023*
H00D	0.2763	−0.1311	0.3840	0.023*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Br1	0.01288 (9)	0.02093 (10)	0.02761 (11)	0.00163 (7)	0.00282 (7)	0.00626 (7)
Br2	0.01582 (10)	0.03085 (12)	0.02905 (11)	0.00623 (7)	0.00162 (7)	0.00327 (8)
N1	0.0109 (7)	0.0112 (7)	0.0182 (7)	0.0012 (5)	−0.0001 (5)	0.0029 (6)
C4	0.0213 (9)	0.0209 (9)	0.0208 (9)	0.0089 (8)	0.0048 (8)	−0.0007 (8)
C3	0.0196 (9)	0.0124 (8)	0.0227 (9)	0.0043 (7)	−0.0037 (7)	−0.0027 (7)
C1	0.0103 (8)	0.0107 (8)	0.0179 (8)	0.0028 (6)	−0.0008 (6)	0.0021 (7)
C2	0.0119 (8)	0.0108 (8)	0.0225 (9)	0.0024 (6)	−0.0024 (7)	0.0008 (7)
C7	0.0100 (8)	0.0114 (8)	0.0233 (9)	0.0025 (6)	−0.0006 (7)	0.0047 (7)
C6	0.0111 (8)	0.0115 (8)	0.0191 (9)	0.0033 (6)	0.0010 (6)	0.0029 (7)
C5	0.0133 (8)	0.0182 (9)	0.0230 (9)	0.0041 (7)	0.0042 (7)	0.0032 (7)
C8	0.0121 (8)	0.0095 (8)	0.0204 (9)	0.0019 (6)	−0.0018 (7)	0.0039 (7)
C9	0.0141 (8)	0.0127 (8)	0.0257 (10)	0.0001 (7)	−0.0042 (7)	0.0031 (7)
C10	0.0220 (9)	0.0152 (9)	0.0210 (9)	0.0030 (7)	−0.0091 (7)	−0.0009 (7)
C11	0.0234 (10)	0.0185 (9)	0.0159 (9)	0.0072 (7)	−0.0025 (7)	0.0014 (7)
C12	0.0155 (8)	0.0146 (8)	0.0173 (9)	0.0039 (7)	−0.0002 (7)	0.0047 (7)
C13	0.0116 (8)	0.0108 (8)	0.0174 (8)	0.0036 (6)	−0.0012 (6)	0.0037 (6)
C14	0.0127 (8)	0.0186 (9)	0.0266 (10)	−0.0010 (7)	0.0006 (7)	0.0012 (8)
C15	0.0146 (8)	0.0126 (8)	0.0251 (9)	0.0000 (7)	−0.0027 (7)	0.0018 (7)
C16	0.0171 (9)	0.0221 (10)	0.0192 (9)	0.0045 (7)	0.0033 (7)	0.0062 (7)

Geometric parameters (Å, º) top

Br1—C15	1.9736 (18)	C8—C9	1.432 (3)
Br2—C16	1.9782 (19)	C8—C13	1.436 (2)
N1—C1	1.341 (2)	C9—C10	1.363 (3)
N1—C13	1.341 (2)	C9—H00F	0.9500
C4—C5	1.362 (3)	C10—C11	1.416 (3)
C4—C3	1.420 (3)	C10—H00H	0.9500
C4—H4	0.9500	C11—C12	1.366 (3)
C3—C2	1.365 (3)	C11—H00G	0.9500
C3—H00E	0.9500	C12—C13	1.443 (3)
C1—C6	1.440 (2)	C12—C16	1.493 (3)
C1—C2	1.442 (2)	C14—H14	0.9800
C2—C15	1.493 (3)	C14—H00K	0.9800
C7—C6	1.409 (3)	C14—H00L	0.9800
C7—C8	1.410 (3)	C15—H00A	0.9900
C7—C14	1.510 (2)	C15—H15	0.9900
C6—C5	1.441 (3)	C16—H16	0.9900
C5—H5	0.9500	C16—H00D	0.9900

C1—N1—C13	118.09 (15)	C9—C10—H00H	119.7
C5—C4—C3	121.00 (18)	C11—C10—H00H	119.7
C5—C4—H4	119.5	C12—C11—C10	121.54 (18)
C3—C4—H4	119.5	C12—C11—H00G	119.2
C2—C3—C4	121.07 (17)	C10—C11—H00G	119.2
C2—C3—H00E	119.5	C11—C12—C13	119.35 (17)
C4—C3—H00E	119.5	C11—C12—C16	121.08 (17)
N1—C1—C6	123.29 (16)	C13—C12—C16	119.57 (16)
N1—C1—C2	117.24 (16)	N1—C13—C8	123.45 (16)
C6—C1—C2	119.47 (16)	N1—C13—C12	117.20 (16)
C3—C2—C1	119.76 (17)	C8—C13—C12	119.34 (16)
C3—C2—C15	121.03 (17)	C7—C14—H14	109.5
C1—C2—C15	119.11 (16)	C7—C14—H00K	109.5
C6—C7—C8	118.45 (16)	H14—C14—H00K	109.5
C6—C7—C14	120.94 (17)	C7—C14—H00L	109.5
C8—C7—C14	120.61 (16)	H14—C14—H00L	109.5
C7—C6—C1	118.32 (16)	H00K—C14—H00L	109.5
C7—C6—C5	123.66 (16)	C2—C15—Br1	111.78 (12)
C1—C6—C5	118.01 (16)	C2—C15—H00A	109.3
C4—C5—C6	120.69 (17)	Br1—C15—H00A	109.3
C4—C5—H5	119.7	C2—C15—H15	109.3
C6—C5—H5	119.7	Br1—C15—H15	109.3
C7—C8—C9	123.31 (17)	H00A—C15—H15	107.9
C7—C8—C13	118.32 (16)	C12—C16—Br2	110.38 (13)
C9—C8—C13	118.38 (17)	C12—C16—H16	109.6
C10—C9—C8	120.83 (17)	Br2—C16—H16	109.6
C10—C9—H00F	119.6	C12—C16—H00D	109.6
C8—C9—H00F	119.6	Br2—C16—H00D	109.6
C9—C10—C11	120.54 (17)	H16—C16—H00D	108.1

5-(Mo) top

Crystal data top

C₁₆H₁₃Br₂N	F(000) = 744
M_r = 379.09	D_x = 1.836 Mg m⁻³
Monoclinic, P2₁/n	Mo Kα radiation, λ = 0.71073 Å
a = 9.599 (2) Å	Cell parameters from 9736 reflections
b = 8.378 (2) Å	θ = 2.3–26.8°
c = 17.194 (3) Å	µ = 5.90 mm⁻¹
β = 97.32 (2)°	T = 100 K
V = 1371.5 (5) Å³	0.20 × 0.16 × 0.15 mm
Z = 4

Data collection top

Bruker Smart APEX II Quazar diffractometer	2754 reflections with I > 2σ(I)
Radiation source: INCOATEC Microsource	R_int = 0.023
ω scans	θ_max = 26.8°, θ_min = 2.3°
Absorption correction: multi-scan SADABS-2014/4	h = −12→12
T_min = 0.452, T_max = 0.519	k = −10→10
34451 measured reflections	l = −21→21
2918 independent reflections

Refinement top

Refinement on F²	0 restraints
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.020	H-atom parameters constrained
wR(F²) = 0.054	w = 1/[σ²(F_o²) + (0.026P)² + 1.6275P] where P = (F_o² + 2F_c²)/3
S = 1.08	(Δ/σ)_max < 0.001
2918 reflections	Δρ_max = 0.79 e Å⁻³
173 parameters	Δρ_min = −0.59 e Å⁻³

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Br1	−0.00996 (2)	0.01221 (2)	0.19965 (2)	0.02202 (7)
Br2	−0.07147 (2)	0.29647 (3)	−0.01920 (2)	0.02705 (7)
N01	−0.33788 (16)	0.08678 (19)	0.07965 (9)	0.0150 (3)
C004	−0.3042 (2)	−0.0555 (2)	0.20016 (12)	0.0171 (4)
C005	−0.41590 (19)	0.1815 (2)	0.02838 (11)	0.0150 (4)
C006	−0.38696 (19)	0.0517 (2)	0.14726 (11)	0.0148 (4)
C007	−0.3632 (2)	0.2145 (2)	−0.04472 (11)	0.0175 (4)
C008	−0.5586 (2)	0.0667 (2)	0.24237 (12)	0.0197 (4)
H008	−0.6443	0.1054	0.2574	0.024*
C009	−0.51671 (19)	0.1143 (2)	0.16839 (11)	0.0157 (4)
C00A	−0.54823 (19)	0.2482 (2)	0.04254 (11)	0.0158 (4)
C00B	−0.1749 (2)	−0.1282 (2)	0.17557 (12)	0.0194 (4)
H00A	−0.1904	−0.1494	0.1185	0.023*
H00B	−0.1563	−0.2315	0.2029	0.023*
C00C	−0.2247 (2)	0.1480 (3)	−0.05908 (12)	0.0209 (4)
H00C	−0.2241	0.1310	−0.1160	0.025*
H00D	−0.2095	0.0436	−0.0324	0.025*
C00D	−0.6245 (2)	0.3434 (2)	−0.01772 (12)	0.0195 (4)
H00E	−0.7121	0.3887	−0.0094	0.023*
C00E	−0.4417 (2)	0.3050 (2)	−0.10020 (12)	0.0213 (4)
H00F	−0.4075	0.3249	−0.1488	0.026*
C00F	−0.3490 (2)	−0.0950 (2)	0.26977 (12)	0.0202 (4)
H00G	−0.2938	−0.1649	0.3046	0.024*
C00G	−0.5729 (2)	0.3696 (2)	−0.08683 (12)	0.0223 (4)
H00H	−0.6254	0.4319	−0.1264	0.027*
C00H	−0.5967 (2)	0.2165 (2)	0.11492 (12)	0.0169 (4)
C00I	−0.4767 (2)	−0.0335 (3)	0.29113 (12)	0.0219 (4)
H00I	−0.5053	−0.0626	0.3401	0.026*
C00J	−0.7321 (2)	0.2890 (2)	0.13425 (13)	0.0213 (4)
H00J	−0.7426	0.3967	0.1121	0.032*
H00K	−0.7302	0.2946	0.1913	0.032*
H00L	−0.8114	0.2227	0.1119	0.032*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Br1	0.01422 (10)	0.02267 (11)	0.02919 (12)	−0.00169 (7)	0.00287 (8)	−0.00642 (8)
Br2	0.01727 (11)	0.03276 (13)	0.03074 (13)	−0.00650 (8)	0.00164 (8)	−0.00341 (9)
N01	0.0119 (7)	0.0130 (7)	0.0195 (8)	−0.0014 (6)	0.0001 (6)	−0.0029 (6)
C004	0.0134 (8)	0.0127 (8)	0.0242 (10)	−0.0027 (7)	−0.0016 (7)	−0.0008 (7)
C005	0.0138 (8)	0.0126 (8)	0.0179 (9)	−0.0037 (7)	−0.0008 (7)	−0.0035 (7)
C006	0.0121 (8)	0.0116 (8)	0.0199 (9)	−0.0027 (7)	−0.0004 (7)	−0.0027 (7)
C007	0.0167 (9)	0.0169 (9)	0.0184 (9)	−0.0042 (7)	−0.0004 (7)	−0.0042 (7)
C008	0.0150 (9)	0.0204 (9)	0.0241 (10)	−0.0045 (8)	0.0044 (7)	−0.0028 (8)
C009	0.0125 (8)	0.0136 (8)	0.0208 (9)	−0.0034 (7)	0.0010 (7)	−0.0028 (7)
C00A	0.0130 (8)	0.0119 (8)	0.0213 (9)	−0.0023 (7)	−0.0027 (7)	−0.0033 (7)
C00B	0.0157 (9)	0.0146 (9)	0.0266 (10)	0.0002 (7)	−0.0024 (7)	−0.0013 (8)
C00C	0.0184 (9)	0.0239 (10)	0.0208 (10)	−0.0042 (8)	0.0040 (8)	−0.0054 (8)
C00D	0.0153 (9)	0.0139 (9)	0.0275 (10)	−0.0004 (7)	−0.0041 (8)	−0.0026 (8)
C00E	0.0248 (10)	0.0206 (10)	0.0170 (9)	−0.0072 (8)	−0.0027 (8)	−0.0009 (8)
C00F	0.0203 (9)	0.0147 (9)	0.0240 (10)	−0.0042 (7)	−0.0037 (8)	0.0031 (8)
C00G	0.0230 (10)	0.0179 (9)	0.0228 (10)	−0.0032 (8)	−0.0089 (8)	0.0010 (8)
C00H	0.0119 (8)	0.0133 (8)	0.0247 (10)	−0.0017 (7)	−0.0002 (7)	−0.0047 (7)
C00I	0.0224 (10)	0.0222 (10)	0.0217 (10)	−0.0081 (8)	0.0050 (8)	0.0005 (8)
C00J	0.0142 (9)	0.0199 (10)	0.0293 (11)	0.0005 (7)	0.0011 (8)	−0.0001 (8)

Geometric parameters (Å, º) top

Br1—C00B	1.9738 (19)	C007—C00C	1.491 (3)
Br2—C00C	1.980 (2)	C008—C00I	1.363 (3)
N01—C006	1.341 (2)	C008—C009	1.438 (3)
N01—C005	1.341 (2)	C009—C00H	1.410 (3)
C004—C00F	1.363 (3)	C00A—C00H	1.408 (3)
C004—C006	1.442 (3)	C00A—C00D	1.433 (3)
C004—C00B	1.491 (3)	C00D—C00G	1.362 (3)
C005—C00A	1.437 (3)	C00E—C00G	1.416 (3)
C005—C007	1.440 (3)	C00F—C00I	1.420 (3)
C006—C009	1.440 (3)	C00H—C00J	1.510 (3)
C007—C00E	1.367 (3)

C006—N01—C005	118.07 (16)	C00H—C009—C006	118.22 (17)
C00F—C004—C006	119.68 (18)	C008—C009—C006	118.09 (17)
C00F—C004—C00B	121.10 (18)	C00H—C00A—C00D	123.25 (18)
C006—C004—C00B	119.13 (18)	C00H—C00A—C005	118.36 (17)
N01—C005—C00A	123.39 (17)	C00D—C00A—C005	118.39 (18)
N01—C005—C007	117.27 (17)	C004—C00B—Br1	111.81 (13)
C00A—C005—C007	119.33 (18)	C007—C00C—Br2	110.28 (14)
N01—C006—C009	123.35 (17)	C00G—C00D—C00A	120.75 (19)
N01—C006—C004	117.18 (17)	C007—C00E—C00G	121.41 (19)
C009—C006—C004	119.46 (17)	C004—C00F—C00I	121.19 (19)
C00E—C007—C005	119.44 (18)	C00D—C00G—C00E	120.65 (19)
C00E—C007—C00C	121.03 (19)	C00A—C00H—C009	118.51 (17)
C005—C007—C00C	119.52 (18)	C00A—C00H—C00J	120.61 (18)
C00I—C008—C009	120.65 (18)	C009—C00H—C00J	120.87 (18)
C00H—C009—C008	123.68 (17)	C008—C00I—C00F	120.92 (19)

6-(Ag) top

Crystal data top

C₃₀H₄₆Br₂Cl₂CoN₄Si₂	F(000) = 1652
M_r = 808.54	D_x = 1.461 Mg m⁻³
Monoclinic, P2₁/n	Ag Kα radiation, λ = 0.56086 Å
a = 18.568 (3) Å	Cell parameters from 9912 reflections
b = 9.504 (2) Å	θ = 2.6–20.8°
c = 21.378 (3) Å	µ = 1.53 mm⁻¹
β = 102.95 (2)°	T = 100 K
V = 3676.6 (11) Å³	0.08 × 0.06 × 0.02 mm
Z = 4

Data collection top

Bruker Smart APEX II Quazar diffractometer	6882 reflections with I > 2σ(I)
Radiation source: INCOATEC Microsource	R_int = 0.038
ω scans	θ_max = 20.8°, θ_min = 1.5°
Absorption correction: multi-scan SADABS-2014/4	h = −23→23
T_min = 0.841, T_max = 0.960	k = −12→12
60559 measured reflections	l = −27→27
7811 independent reflections

Refinement top

Refinement on F²	79 restraints
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.020	H-atom parameters constrained
wR(F²) = 0.051	w = 1/[σ²(F_o²) + (0.0225P)² + 1.990P] where P = (F_o² + 2F_c²)/3
S = 1.02	(Δ/σ)_max = 0.001
7811 reflections	Δρ_max = 0.41 e Å⁻³
420 parameters	Δρ_min = −0.25 e Å⁻³

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
Co1	0.03359 (2)	0.56713 (2)	0.27668 (2)	0.01389 (5)
Br1	0.10445 (2)	0.77476 (2)	0.28356 (2)	0.02096 (6)	0.9736 (8)
Cl1B	0.0799 (13)	0.779 (2)	0.2769 (12)	0.02096 (6)	0.0264 (8)
Br2	0.07057 (2)	0.49224 (2)	0.38454 (2)	0.02330 (6)	0.9736 (8)
Cl2B	0.0782 (13)	0.461 (3)	0.3686 (9)	0.02330 (6)	0.0264 (8)
Si1	0.03220 (2)	0.54932 (5)	0.17408 (2)	0.01487 (9)
Si2	−0.06621 (2)	0.44281 (5)	0.27142 (2)	0.01473 (9)
Cl1	−0.01344 (6)	0.38328 (15)	0.11392 (7)	0.0258 (2)	0.9736 (8)
Br1C	−0.0267 (11)	0.381 (3)	0.1166 (12)	0.0258 (2)	0.0264 (8)
Cl2	−0.15454 (6)	0.42642 (11)	0.19043 (5)	0.02511 (17)	0.9736 (8)
Br2C	−0.1617 (10)	0.402 (2)	0.1952 (9)	0.02511 (17)	0.0264 (8)
N2	0.02298 (7)	0.69982 (15)	0.12014 (6)	0.0167 (3)
N3	−0.06660 (7)	0.27216 (14)	0.30928 (6)	0.0163 (3)
N4	−0.11687 (7)	0.45964 (15)	0.33466 (6)	0.0178 (3)
C1	0.09426 (8)	0.68819 (18)	0.11746 (7)	0.0163 (3)
N1	0.11945 (7)	0.57260 (15)	0.15020 (6)	0.0174 (3)
C2	0.19081 (9)	0.49658 (18)	0.16081 (8)	0.0198 (3)
C3	0.2580 (4)	0.5936 (8)	0.1683 (5)	0.0324 (15)	0.56 (2)
H3A	0.3032	0.5368	0.1751	0.049*	0.56 (2)
H3B	0.2538	0.6503	0.1293	0.049*	0.56 (2)
H3C	0.2602	0.6559	0.2052	0.049*	0.56 (2)
C4	0.1908 (7)	0.4013 (12)	0.1030 (5)	0.0288 (18)	0.56 (2)
H4A	0.2379	0.3506	0.1097	0.043*	0.56 (2)
H4B	0.1501	0.3335	0.0982	0.043*	0.56 (2)
H4C	0.1843	0.4588	0.0640	0.043*	0.56 (2)
C5	0.1938 (8)	0.4071 (13)	0.2198 (5)	0.041 (2)	0.56 (2)
H5A	0.2401	0.3537	0.2294	0.061*	0.56 (2)
H5B	0.1913	0.4679	0.2563	0.061*	0.56 (2)
H5C	0.1519	0.3418	0.2119	0.061*	0.56 (2)
C3A	0.2533 (5)	0.5921 (10)	0.1942 (9)	0.041 (3)	0.44 (2)
H3A1	0.3003	0.5410	0.2010	0.061*	0.44 (2)
H3A2	0.2555	0.6750	0.1674	0.061*	0.44 (2)
H3A3	0.2445	0.6220	0.2357	0.061*	0.44 (2)
C4A	0.2015 (11)	0.4354 (17)	0.0985 (6)	0.037 (3)	0.44 (2)
H4A1	0.2488	0.3853	0.1060	0.055*	0.44 (2)
H4A2	0.1612	0.3696	0.0816	0.055*	0.44 (2)
H4A3	0.2014	0.5113	0.0675	0.055*	0.44 (2)
C5A	0.1858 (10)	0.3759 (15)	0.2069 (7)	0.037 (3)	0.44 (2)
H5A1	0.2320	0.3222	0.2154	0.056*	0.44 (2)
H5A2	0.1775	0.4142	0.2473	0.056*	0.44 (2)
H5A3	0.1446	0.3139	0.1876	0.056*	0.44 (2)
C6	−0.03355 (9)	0.80599 (18)	0.09232 (8)	0.0190 (3)
C7	−0.04532 (11)	0.8055 (2)	0.01940 (8)	0.0315 (4)
H7A	−0.0860	0.8692	0.0008	0.047*
H7B	−0.0575	0.7099	0.0032	0.047*
H7C	0.0000	0.8370	0.0073	0.047*
C8	−0.01139 (11)	0.9523 (2)	0.11873 (9)	0.0305 (4)
H8A	0.0312	0.9851	0.1028	0.046*
H8B	0.0017	0.9488	0.1657	0.046*
H8C	−0.0528	1.0173	0.1047	0.046*
C9	−0.10376 (10)	0.7593 (2)	0.11194 (11)	0.0370 (5)
H9A	−0.1439	0.8251	0.0944	0.055*
H9B	−0.0952	0.7581	0.1589	0.055*
H9C	−0.1174	0.6647	0.0952	0.055*
C10	0.13825 (9)	0.78651 (19)	0.08709 (8)	0.0203 (3)
C11	0.17443 (10)	0.8989 (2)	0.12244 (9)	0.0265 (4)
H11	0.1678	0.9166	0.1645	0.032*
C12	0.22007 (11)	0.9849 (2)	0.09610 (11)	0.0357 (5)
H12	0.2454	1.0609	0.1204	0.043*
C13	0.22877 (11)	0.9602 (3)	0.03455 (11)	0.0438 (6)
H13	0.2601	1.0194	0.0166	0.053*
C14	0.19231 (11)	0.8507 (3)	−0.00082 (10)	0.0430 (6)
H14	0.1983	0.8352	−0.0433	0.052*
C15	0.14673 (10)	0.7623 (2)	0.02487 (8)	0.0304 (4)
H15	0.1217	0.6864	0.0003	0.036*
C16	−0.10367 (8)	0.32501 (18)	0.35097 (7)	0.0169 (3)
C17	−0.16234 (9)	0.56885 (18)	0.35680 (8)	0.0211 (4)
C18	−0.16415 (15)	0.6923 (2)	0.31120 (12)	0.0515 (7)
H18A	−0.1877	0.6629	0.2675	0.077*
H18B	−0.1136	0.7236	0.3125	0.077*
H18C	−0.1923	0.7698	0.3243	0.077*
C19	−0.12719 (11)	0.6159 (2)	0.42487 (10)	0.0350 (5)
H19A	−0.0762	0.6458	0.4271	0.052*
H19B	−0.1274	0.5375	0.4546	0.052*
H19C	−0.1554	0.6948	0.4368	0.052*
C20	−0.24004 (10)	0.5136 (2)	0.35197 (11)	0.0372 (5)
H20A	−0.2592	0.4752	0.3089	0.056*
H20B	−0.2720	0.5906	0.3599	0.056*
H20C	−0.2391	0.4395	0.3840	0.056*
C21	−0.02628 (9)	0.13691 (17)	0.30850 (8)	0.0197 (3)
C22	0.03268 (10)	0.16586 (19)	0.27051 (9)	0.0241 (4)
H22A	0.0091	0.2021	0.2279	0.036*
H22B	0.0590	0.0784	0.2659	0.036*
H22C	0.0678	0.2357	0.2933	0.036*
C23	−0.08000 (11)	0.0267 (2)	0.27371 (10)	0.0319 (4)
H23A	−0.1180	0.0086	0.2980	0.048*
H23B	−0.0532	−0.0606	0.2700	0.048*
H23C	−0.1034	0.0611	0.2307	0.048*
C24	0.01131 (12)	0.0868 (2)	0.37563 (9)	0.0335 (5)
H24A	0.0447	0.0086	0.3724	0.050*
H24B	−0.0262	0.0552	0.3982	0.050*
H24C	0.0396	0.1644	0.3995	0.050*
C25	−0.12520 (9)	0.24780 (18)	0.40419 (8)	0.0188 (3)
C26	−0.18171 (10)	0.1489 (2)	0.39064 (8)	0.0241 (4)
H26	−0.2080	0.1343	0.3476	0.029*
C27	−0.19967 (11)	0.0714 (2)	0.44003 (9)	0.0308 (4)
H27	−0.2383	0.0038	0.4309	0.037*
C28	−0.16099 (11)	0.0930 (2)	0.50267 (9)	0.0321 (4)
H28	−0.1727	0.0388	0.5364	0.039*
C29	−0.10548 (12)	0.1928 (2)	0.51648 (8)	0.0307 (4)
H29	−0.0798	0.2080	0.5596	0.037*
C30	−0.08733 (10)	0.27045 (19)	0.46741 (8)	0.0244 (4)
H30	−0.0492	0.3390	0.4768	0.029*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Co1	0.01348 (10)	0.01527 (11)	0.01304 (10)	−0.00228 (8)	0.00321 (8)	−0.00187 (8)
Br1	0.02282 (11)	0.01803 (9)	0.02184 (9)	−0.00764 (9)	0.00462 (9)	−0.00273 (7)
Cl1B	0.02282 (11)	0.01803 (9)	0.02184 (9)	−0.00764 (9)	0.00462 (9)	−0.00273 (7)
Br2	0.02393 (10)	0.02937 (12)	0.01439 (10)	−0.00656 (8)	−0.00035 (7)	0.00056 (7)
Cl2B	0.02393 (10)	0.02937 (12)	0.01439 (10)	−0.00656 (8)	−0.00035 (7)	0.00056 (7)
Si1	0.0141 (2)	0.0166 (2)	0.01422 (19)	0.00006 (17)	0.00368 (16)	−0.00155 (17)
Si2	0.0132 (2)	0.0154 (2)	0.0157 (2)	−0.00007 (17)	0.00342 (16)	0.00192 (17)
Cl1	0.0283 (5)	0.0275 (2)	0.0221 (3)	−0.0068 (4)	0.0072 (3)	−0.01013 (19)
Br1C	0.0283 (5)	0.0275 (2)	0.0221 (3)	−0.0068 (4)	0.0072 (3)	−0.01013 (19)
Cl2	0.0167 (3)	0.0336 (5)	0.0225 (3)	−0.0060 (3)	−0.0010 (2)	0.0081 (3)
Br2C	0.0167 (3)	0.0336 (5)	0.0225 (3)	−0.0060 (3)	−0.0010 (2)	0.0081 (3)
N2	0.0141 (7)	0.0210 (7)	0.0157 (6)	0.0022 (5)	0.0047 (5)	0.0026 (5)
N3	0.0158 (7)	0.0149 (7)	0.0180 (6)	−0.0008 (5)	0.0034 (5)	0.0019 (5)
N4	0.0159 (7)	0.0173 (7)	0.0219 (7)	0.0026 (5)	0.0082 (5)	0.0041 (6)
C1	0.0142 (7)	0.0229 (9)	0.0116 (7)	0.0004 (6)	0.0026 (6)	−0.0028 (6)
N1	0.0144 (7)	0.0220 (8)	0.0161 (6)	0.0033 (6)	0.0044 (5)	0.0004 (6)
C2	0.0146 (8)	0.0211 (9)	0.0237 (8)	0.0058 (7)	0.0042 (6)	−0.0015 (7)
C3	0.018 (2)	0.027 (2)	0.049 (4)	0.0034 (15)	0.001 (2)	−0.014 (3)
C4	0.027 (3)	0.026 (4)	0.034 (3)	0.003 (3)	0.010 (2)	−0.008 (3)
C5	0.039 (4)	0.053 (5)	0.033 (3)	0.032 (4)	0.012 (3)	0.017 (3)
C3A	0.016 (3)	0.030 (3)	0.067 (7)	0.005 (2)	−0.011 (4)	−0.016 (4)
C4A	0.045 (7)	0.037 (6)	0.034 (3)	0.020 (5)	0.019 (3)	0.003 (3)
C5A	0.036 (5)	0.043 (5)	0.039 (5)	0.018 (3)	0.019 (4)	0.014 (4)
C6	0.0149 (8)	0.0242 (9)	0.0182 (8)	0.0056 (7)	0.0042 (6)	0.0042 (7)
C7	0.0278 (10)	0.0466 (13)	0.0176 (8)	0.0146 (9)	−0.0006 (7)	0.0008 (8)
C8	0.0341 (11)	0.0256 (10)	0.0298 (9)	0.0092 (8)	0.0027 (8)	−0.0008 (8)
C9	0.0193 (9)	0.0405 (12)	0.0542 (13)	0.0115 (8)	0.0150 (9)	0.0191 (10)
C10	0.0123 (8)	0.0291 (10)	0.0196 (8)	0.0045 (7)	0.0042 (6)	0.0064 (7)
C11	0.0229 (9)	0.0287 (10)	0.0278 (9)	0.0001 (8)	0.0056 (7)	0.0066 (8)
C12	0.0218 (9)	0.0331 (11)	0.0507 (13)	−0.0032 (8)	0.0051 (9)	0.0143 (10)
C13	0.0220 (10)	0.0635 (16)	0.0476 (13)	−0.0003 (10)	0.0113 (9)	0.0316 (12)
C14	0.0273 (11)	0.0785 (18)	0.0262 (10)	0.0058 (11)	0.0123 (8)	0.0198 (11)
C15	0.0205 (9)	0.0532 (13)	0.0179 (8)	0.0029 (8)	0.0049 (7)	0.0063 (8)
C16	0.0125 (7)	0.0192 (8)	0.0177 (7)	−0.0029 (6)	0.0003 (6)	0.0011 (6)
C17	0.0206 (8)	0.0209 (9)	0.0243 (8)	0.0058 (7)	0.0102 (7)	0.0015 (7)
C18	0.0750 (17)	0.0338 (12)	0.0608 (15)	0.0332 (12)	0.0471 (14)	0.0231 (11)
C19	0.0322 (11)	0.0299 (11)	0.0398 (11)	0.0042 (9)	0.0017 (9)	−0.0135 (9)
C20	0.0191 (9)	0.0484 (13)	0.0460 (12)	0.0031 (9)	0.0114 (8)	−0.0177 (10)
C21	0.0214 (8)	0.0142 (8)	0.0231 (8)	0.0018 (7)	0.0041 (7)	−0.0004 (7)
C22	0.0228 (9)	0.0174 (9)	0.0332 (9)	0.0025 (7)	0.0088 (7)	−0.0014 (7)
C23	0.0317 (10)	0.0213 (10)	0.0451 (11)	−0.0081 (8)	0.0134 (9)	−0.0089 (8)
C24	0.0435 (12)	0.0280 (11)	0.0279 (10)	0.0167 (9)	0.0055 (8)	0.0068 (8)
C25	0.0192 (8)	0.0198 (9)	0.0173 (7)	−0.0001 (6)	0.0040 (6)	0.0031 (6)
C26	0.0212 (9)	0.0296 (10)	0.0205 (8)	−0.0054 (7)	0.0023 (7)	0.0051 (7)
C27	0.0285 (10)	0.0332 (11)	0.0311 (10)	−0.0100 (8)	0.0078 (8)	0.0074 (8)
C28	0.0410 (11)	0.0338 (11)	0.0243 (9)	−0.0010 (9)	0.0133 (8)	0.0117 (8)
C29	0.0437 (11)	0.0296 (11)	0.0166 (8)	0.0007 (9)	0.0021 (8)	0.0038 (7)
C30	0.0289 (9)	0.0210 (9)	0.0208 (8)	−0.0036 (7)	0.0001 (7)	0.0001 (7)

Geometric parameters (Å, º) top

Co1—Si2	2.1792 (6)	C7—H7C	0.9800
Co1—Cl1B	2.19 (2)	C8—H8A	0.9800
Co1—Si1	2.1942 (6)	C8—H8B	0.9800
Co1—Cl2B	2.196 (19)	C8—H8C	0.9800
Co1—Br1	2.3580 (5)	C9—H9A	0.9800
Co1—Br2	2.3633 (5)	C9—H9B	0.9800
Si1—N1	1.8179 (14)	C9—H9C	0.9800
Si1—N2	1.8213 (14)	C10—C11	1.391 (3)
Si1—Cl1	2.0913 (13)	C10—C15	1.393 (2)
Si1—Br1C	2.159 (19)	C11—C12	1.385 (3)
Si1—C1	2.2716 (17)	C11—H11	0.9500
Si2—N3	1.8133 (14)	C12—C13	1.381 (3)
Si2—N4	1.8188 (14)	C12—H12	0.9500
Si2—Cl2	2.1070 (12)	C13—C14	1.373 (4)
Si2—Br2C	2.156 (17)	C13—H13	0.9500
Si2—C16	2.2713 (16)	C14—C15	1.390 (3)
N2—C1	1.342 (2)	C14—H14	0.9500
N2—C6	1.481 (2)	C15—H15	0.9500
N3—C16	1.340 (2)	C16—C25	1.482 (2)
N3—C21	1.490 (2)	C17—C20	1.517 (3)
N4—C16	1.334 (2)	C17—C18	1.521 (3)
N4—C17	1.481 (2)	C17—C19	1.523 (3)
C1—N1	1.330 (2)	C18—H18A	0.9800
C1—C10	1.483 (2)	C18—H18B	0.9800
N1—C2	1.481 (2)	C18—H18C	0.9800
C2—C4A	1.506 (9)	C19—H19A	0.9800
C2—C5	1.511 (8)	C19—H19B	0.9800
C2—C3A	1.520 (7)	C19—H19C	0.9800
C2—C5A	1.529 (9)	C20—H20A	0.9800
C2—C3	1.531 (6)	C20—H20B	0.9800
C2—C4	1.533 (7)	C20—H20C	0.9800
C3—H3A	0.9800	C21—C23	1.521 (2)
C3—H3B	0.9800	C21—C24	1.525 (2)
C3—H3C	0.9800	C21—C22	1.527 (2)
C4—H4A	0.9800	C22—H22A	0.9800
C4—H4B	0.9800	C22—H22B	0.9800
C4—H4C	0.9800	C22—H22C	0.9800
C5—H5A	0.9800	C23—H23A	0.9800
C5—H5B	0.9800	C23—H23B	0.9800
C5—H5C	0.9800	C23—H23C	0.9800
C3A—H3A1	0.9800	C24—H24A	0.9800
C3A—H3A2	0.9800	C24—H24B	0.9800
C3A—H3A3	0.9800	C24—H24C	0.9800
C4A—H4A1	0.9800	C25—C26	1.390 (2)
C4A—H4A2	0.9800	C25—C30	1.393 (2)
C4A—H4A3	0.9800	C26—C27	1.388 (2)
C5A—H5A1	0.9800	C26—H26	0.9500
C5A—H5A2	0.9800	C27—C28	1.386 (3)
C5A—H5A3	0.9800	C27—H27	0.9500
C6—C9	1.522 (2)	C28—C29	1.383 (3)
C6—C8	1.523 (3)	C28—H28	0.9500
C6—C7	1.525 (2)	C29—C30	1.385 (3)
C7—H7A	0.9800	C29—H29	0.9500
C7—H7B	0.9800	C30—H30	0.9500

Si2—Co1—Cl1B	145.9 (7)	C8—C6—C7	110.29 (15)
Si2—Co1—Si1	95.01 (2)	C6—C7—H7A	109.5
Cl1B—Co1—Si1	89.4 (7)	C6—C7—H7B	109.5
Si2—Co1—Cl2B	86.8 (6)	H7A—C7—H7B	109.5
Cl1B—Co1—Cl2B	110.5 (9)	C6—C7—H7C	109.5
Si1—Co1—Cl2B	140.9 (6)	H7A—C7—H7C	109.5
Si2—Co1—Br1	155.933 (17)	H7B—C7—H7C	109.5
Si1—Co1—Br1	90.479 (18)	C6—C8—H8A	109.5
Si2—Co1—Br2	86.83 (2)	C6—C8—H8B	109.5
Si1—Co1—Br2	152.597 (17)	H8A—C8—H8B	109.5
Br1—Co1—Br2	98.922 (17)	C6—C8—H8C	109.5
N1—Si1—N2	71.93 (6)	H8A—C8—H8C	109.5
N1—Si1—Cl1	100.54 (5)	H8B—C8—H8C	109.5
N2—Si1—Cl1	103.63 (7)	C6—C9—H9A	109.5
N1—Si1—Br1C	107.4 (5)	C6—C9—H9B	109.5
N2—Si1—Br1C	105.0 (8)	H9A—C9—H9B	109.5
N1—Si1—Co1	117.37 (5)	C6—C9—H9C	109.5
N2—Si1—Co1	123.42 (5)	H9A—C9—H9C	109.5
Cl1—Si1—Co1	125.82 (4)	H9B—C9—H9C	109.5
Br1C—Si1—Co1	121.1 (6)	C11—C10—C15	120.09 (17)
N1—Si1—C1	35.83 (6)	C11—C10—C1	119.49 (15)
N2—Si1—C1	36.21 (6)	C15—C10—C1	120.33 (17)
Cl1—Si1—C1	107.14 (5)	C12—C11—C10	119.83 (18)
Br1C—Si1—C1	112.3 (6)	C12—C11—H11	120.1
Co1—Si1—C1	126.45 (4)	C10—C11—H11	120.1
N3—Si2—N4	72.09 (6)	C13—C12—C11	120.0 (2)
N3—Si2—Cl2	102.73 (5)	C13—C12—H12	120.0
N4—Si2—Cl2	100.39 (6)	C11—C12—H12	120.0
N3—Si2—Br2C	95.3 (5)	C14—C13—C12	120.33 (19)
N4—Si2—Br2C	95.9 (5)	C14—C13—H13	119.8
N3—Si2—Co1	123.39 (5)	C12—C13—H13	119.8
N4—Si2—Co1	119.30 (5)	C13—C14—C15	120.63 (19)
Cl2—Si2—Co1	125.36 (3)	C13—C14—H14	119.7
Br2C—Si2—Co1	133.0 (4)	C15—C14—H14	119.7
N3—Si2—C16	36.15 (6)	C14—C15—C10	119.1 (2)
N4—Si2—C16	35.97 (6)	C14—C15—H15	120.4
Cl2—Si2—C16	105.44 (5)	C10—C15—H15	120.4
Br2C—Si2—C16	98.0 (4)	N4—C16—N3	106.11 (14)
Co1—Si2—C16	128.91 (5)	N4—C16—C25	127.58 (15)
C1—N2—C6	131.00 (14)	N3—C16—C25	126.31 (15)
C1—N2—Si1	90.50 (10)	N4—C16—Si2	53.19 (8)
C6—N2—Si1	138.31 (11)	N3—C16—Si2	52.96 (8)
C16—N3—C21	131.71 (14)	C25—C16—Si2	177.87 (12)
C16—N3—Si2	90.89 (10)	N4—C17—C20	109.72 (15)
C21—N3—Si2	135.61 (11)	N4—C17—C18	105.55 (14)
C16—N4—C17	132.30 (14)	C20—C17—C18	109.83 (18)
C16—N4—Si2	90.83 (10)	N4—C17—C19	110.99 (14)
C17—N4—Si2	136.55 (11)	C20—C17—C19	111.36 (16)
N1—C1—N2	106.23 (14)	C18—C17—C19	109.22 (18)
N1—C1—C10	125.98 (14)	C17—C18—H18A	109.5
N2—C1—C10	127.73 (15)	C17—C18—H18B	109.5
N1—C1—Si1	53.15 (8)	H18A—C18—H18B	109.5
N2—C1—Si1	53.29 (8)	C17—C18—H18C	109.5
C10—C1—Si1	173.86 (12)	H18A—C18—H18C	109.5
C1—N1—C2	132.88 (14)	H18B—C18—H18C	109.5
C1—N1—Si1	91.02 (10)	C17—C19—H19A	109.5
C2—N1—Si1	136.09 (11)	C17—C19—H19B	109.5
N1—C2—C4A	110.1 (7)	H19A—C19—H19B	109.5
N1—C2—C5	105.5 (6)	C17—C19—H19C	109.5
N1—C2—C3A	110.1 (4)	H19A—C19—H19C	109.5
C4A—C2—C3A	114.1 (6)	H19B—C19—H19C	109.5
N1—C2—C5A	106.4 (7)	C17—C20—H20A	109.5
C4A—C2—C5A	108.6 (7)	C17—C20—H20B	109.5
C3A—C2—C5A	107.2 (7)	H20A—C20—H20B	109.5
N1—C2—C3	113.7 (3)	C17—C20—H20C	109.5
C5—C2—C3	112.0 (6)	H20A—C20—H20C	109.5
N1—C2—C4	109.0 (5)	H20B—C20—H20C	109.5
C5—C2—C4	109.5 (6)	N3—C21—C23	108.89 (14)
C3—C2—C4	107.0 (4)	N3—C21—C24	112.59 (14)
C2—C3—H3A	109.5	C23—C21—C24	110.92 (16)
C2—C3—H3B	109.5	N3—C21—C22	105.81 (13)
H3A—C3—H3B	109.5	C23—C21—C22	109.50 (15)
C2—C3—H3C	109.5	C24—C21—C22	108.98 (15)
H3A—C3—H3C	109.5	C21—C22—H22A	109.5
H3B—C3—H3C	109.5	C21—C22—H22B	109.5
C2—C4—H4A	109.5	H22A—C22—H22B	109.5
C2—C4—H4B	109.5	C21—C22—H22C	109.5
H4A—C4—H4B	109.5	H22A—C22—H22C	109.5
C2—C4—H4C	109.5	H22B—C22—H22C	109.5
H4A—C4—H4C	109.5	C21—C23—H23A	109.5
H4B—C4—H4C	109.5	C21—C23—H23B	109.5
C2—C5—H5A	109.5	H23A—C23—H23B	109.5
C2—C5—H5B	109.5	C21—C23—H23C	109.5
H5A—C5—H5B	109.5	H23A—C23—H23C	109.5
C2—C5—H5C	109.5	H23B—C23—H23C	109.5
H5A—C5—H5C	109.5	C21—C24—H24A	109.5
H5B—C5—H5C	109.5	C21—C24—H24B	109.5
C2—C3A—H3A1	109.5	H24A—C24—H24B	109.5
C2—C3A—H3A2	109.5	C21—C24—H24C	109.5
H3A1—C3A—H3A2	109.5	H24A—C24—H24C	109.5
C2—C3A—H3A3	109.5	H24B—C24—H24C	109.5
H3A1—C3A—H3A3	109.5	C26—C25—C30	119.99 (16)
H3A2—C3A—H3A3	109.5	C26—C25—C16	119.71 (14)
C2—C4A—H4A1	109.5	C30—C25—C16	120.25 (15)
C2—C4A—H4A2	109.5	C27—C26—C25	119.95 (16)
H4A1—C4A—H4A2	109.5	C27—C26—H26	120.0
C2—C4A—H4A3	109.5	C25—C26—H26	120.0
H4A1—C4A—H4A3	109.5	C28—C27—C26	119.71 (18)
H4A2—C4A—H4A3	109.5	C28—C27—H27	120.1
C2—C5A—H5A1	109.5	C26—C27—H27	120.1
C2—C5A—H5A2	109.5	C29—C28—C27	120.53 (17)
H5A1—C5A—H5A2	109.5	C29—C28—H28	119.7
C2—C5A—H5A3	109.5	C27—C28—H28	119.7
H5A1—C5A—H5A3	109.5	C28—C29—C30	120.01 (17)
H5A2—C5A—H5A3	109.5	C28—C29—H29	120.0
N2—C6—C9	105.35 (14)	C30—C29—H29	120.0
N2—C6—C8	111.41 (14)	C29—C30—C25	119.79 (17)
C9—C6—C8	109.93 (16)	C29—C30—H30	120.1
N2—C6—C7	109.54 (14)	C25—C30—H30	120.1
C9—C6—C7	110.21 (16)

6-(Mo) top

Crystal data top

C₃₀H₄₆Br₂Cl₂CoN₄Si₂	F(000) = 1652
M_r = 808.54	D_x = 1.455 Mg m⁻³
Monoclinic, P2₁/n	Mo Kα radiation, λ = 0.71073 Å
a = 18.588 (2) Å	Cell parameters from 9773 reflections
b = 9.518 (2) Å	θ = 2.3–26.7°
c = 21.403 (3) Å	µ = 2.87 mm⁻¹
β = 102.95 (2)°	T = 100 K
V = 3690.3 (11) Å³	0.08 × 0.06 × 0.02 mm
Z = 4

Data collection top

Bruker Smart APEX II Quazar diffractometer	6936 reflections with I > 2σ(I)
Radiation source: INCOATEC Microsource	R_int = 0.028
ω scans	θ_max = 26.8°, θ_min = 1.3°
Absorption correction: multi-scan SADABS-2014/4	h = −23→23
T_min = 0.821, T_max = 0.927	k = −11→12
92677 measured reflections	l = −27→27
7847 independent reflections

Refinement top

Refinement on F²	79 restraints
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.022	H-atom parameters constrained
wR(F²) = 0.059	w = 1/[σ²(F_o²) + (0.027P)² + 2.4392P] where P = (F_o² + 2F_c²)/3
S = 1.10	(Δ/σ)_max = 0.001
7847 reflections	Δρ_max = 0.43 e Å⁻³
420 parameters	Δρ_min = −0.25 e Å⁻³

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
Co1	0.03357 (2)	0.56689 (3)	0.27669 (2)	0.01584 (6)
Br1	0.10426 (2)	0.77457 (2)	0.28346 (2)	0.02326 (7)	0.9787 (9)
Cl1B	0.0739 (17)	0.777 (2)	0.2754 (14)	0.02326 (7)	0.0213 (9)
Br2	0.07063 (2)	0.49209 (2)	0.38446 (2)	0.02587 (7)	0.9787 (9)
Cl2B	0.0819 (14)	0.454 (3)	0.3626 (13)	0.02587 (7)	0.0213 (9)
Si1	0.03215 (3)	0.54896 (5)	0.17417 (2)	0.01693 (10)
Si2	−0.06629 (3)	0.44261 (5)	0.27149 (2)	0.01667 (10)
Cl1	−0.01356 (4)	0.38262 (12)	0.11416 (5)	0.02775 (19)	0.9787 (9)
Br1C	−0.0291 (12)	0.388 (3)	0.1171 (13)	0.02775 (19)	0.0213 (9)
Cl2	−0.15473 (5)	0.42619 (9)	0.19056 (4)	0.02705 (18)	0.9787 (9)
Br2C	−0.1589 (12)	0.396 (2)	0.1968 (10)	0.02705 (18)	0.0213 (9)
N2	0.02289 (8)	0.69936 (16)	0.12018 (7)	0.0190 (3)
N3	−0.06661 (8)	0.27190 (16)	0.30937 (7)	0.0183 (3)
N4	−0.11686 (8)	0.45953 (16)	0.33457 (7)	0.0200 (3)
C1	0.09431 (9)	0.6876 (2)	0.11740 (8)	0.0186 (4)
N1	0.11932 (8)	0.57209 (16)	0.15023 (7)	0.0190 (3)
C2	0.19098 (10)	0.4961 (2)	0.16110 (9)	0.0223 (4)
C3	0.2569 (5)	0.5955 (10)	0.1676 (7)	0.033 (2)	0.51 (3)
H3A	0.3026	0.5406	0.1747	0.050*	0.51 (3)
H3B	0.2517	0.6509	0.1283	0.050*	0.51 (3)
H3C	0.2585	0.6586	0.2041	0.050*	0.51 (3)
C4	0.1897 (8)	0.4018 (15)	0.1026 (6)	0.031 (2)	0.51 (3)
H4A	0.2364	0.3504	0.1086	0.047*	0.51 (3)
H4B	0.1488	0.3348	0.0979	0.047*	0.51 (3)
H4C	0.1830	0.4600	0.0639	0.047*	0.51 (3)
C5	0.1979 (9)	0.4053 (18)	0.2197 (7)	0.046 (3)	0.51 (3)
H5A	0.2449	0.3544	0.2276	0.069*	0.51 (3)
H5B	0.1963	0.4645	0.2569	0.069*	0.51 (3)
H5C	0.1570	0.3379	0.2129	0.069*	0.51 (3)
C3A	0.2549 (6)	0.5889 (12)	0.1942 (10)	0.051 (3)	0.49 (3)
H3A1	0.3011	0.5357	0.2006	0.077*	0.49 (3)
H3A2	0.2578	0.6714	0.1675	0.077*	0.49 (3)
H3A3	0.2469	0.6195	0.2358	0.077*	0.49 (3)
C4A	0.2026 (11)	0.4325 (19)	0.1000 (6)	0.043 (3)	0.49 (3)
H4A1	0.2500	0.3831	0.1084	0.064*	0.49 (3)
H4A2	0.1627	0.3659	0.0834	0.064*	0.49 (3)
H4A3	0.2026	0.5069	0.0684	0.064*	0.49 (3)
C5A	0.1827 (9)	0.3808 (16)	0.2088 (8)	0.042 (3)	0.49 (3)
H5A1	0.2279	0.3243	0.2190	0.062*	0.49 (3)
H5A2	0.1741	0.4238	0.2481	0.062*	0.49 (3)
H5A3	0.1407	0.3205	0.1898	0.062*	0.49 (3)
C6	−0.03365 (10)	0.8055 (2)	0.09222 (9)	0.0212 (4)
C7	−0.04547 (12)	0.8046 (3)	0.01963 (10)	0.0349 (5)
H7A	−0.0862	0.8680	0.0010	0.052*
H7B	−0.0576	0.7091	0.0036	0.052*
H7C	−0.0003	0.8360	0.0075	0.052*
C8	−0.01133 (12)	0.9518 (2)	0.11850 (11)	0.0332 (5)
H8A	0.0303	0.9854	0.1015	0.050*
H8B	0.0032	0.9479	0.1654	0.050*
H8C	−0.0532	1.0162	0.1055	0.050*
C9	−0.10380 (12)	0.7597 (3)	0.11210 (13)	0.0402 (6)
H9A	−0.1439	0.8252	0.0944	0.060*
H9B	−0.0952	0.7594	0.1590	0.060*
H9C	−0.1175	0.6650	0.0957	0.060*
C10	0.13821 (10)	0.7861 (2)	0.08686 (9)	0.0224 (4)
C11	0.17437 (11)	0.8981 (2)	0.12216 (10)	0.0290 (4)
H11	0.1678	0.9157	0.1642	0.035*
C12	0.22006 (12)	0.9841 (3)	0.09583 (12)	0.0386 (6)
H12	0.2454	1.0600	0.1200	0.046*
C13	0.22866 (12)	0.9594 (3)	0.03451 (13)	0.0465 (7)
H13	0.2601	1.0181	0.0166	0.056*
C14	0.19205 (12)	0.8502 (3)	−0.00079 (11)	0.0458 (7)
H14	0.1979	0.8347	−0.0432	0.055*
C15	0.14643 (11)	0.7617 (3)	0.02499 (10)	0.0329 (5)
H15	0.1214	0.6858	0.0006	0.039*
C16	−0.10350 (9)	0.3249 (2)	0.35105 (9)	0.0188 (4)
C17	−0.16214 (10)	0.5689 (2)	0.35699 (10)	0.0242 (4)
C18	−0.16426 (17)	0.6918 (3)	0.31112 (14)	0.0557 (8)
H18A	−0.1874	0.6618	0.2674	0.084*
H18B	−0.1138	0.7240	0.3126	0.084*
H18C	−0.1929	0.7689	0.3238	0.084*
C19	−0.12701 (13)	0.6158 (3)	0.42478 (11)	0.0379 (5)
H19A	−0.0759	0.6450	0.4270	0.057*
H19B	−0.1275	0.5377	0.4545	0.057*
H19C	−0.1549	0.6950	0.4366	0.057*
C20	−0.24010 (11)	0.5136 (3)	0.35220 (12)	0.0394 (6)
H20A	−0.2589	0.4731	0.3096	0.059*
H20B	−0.2723	0.5910	0.3591	0.059*
H20C	−0.2393	0.4412	0.3849	0.059*
C21	−0.02644 (10)	0.13684 (19)	0.30848 (9)	0.0219 (4)
C22	0.03252 (11)	0.1656 (2)	0.27052 (10)	0.0270 (4)
H22A	0.0091	0.2031	0.2282	0.040*
H22B	0.0583	0.0780	0.2654	0.040*
H22C	0.0680	0.2343	0.2936	0.040*
C23	−0.08016 (12)	0.0270 (2)	0.27365 (12)	0.0349 (5)
H23A	−0.1178	0.0081	0.2981	0.052*
H23B	−0.0533	−0.0599	0.2695	0.052*
H23C	−0.1039	0.0619	0.2309	0.052*
C24	0.01126 (14)	0.0869 (2)	0.37555 (11)	0.0367 (5)
H24A	0.0438	0.0075	0.3723	0.055*
H24B	−0.0262	0.0573	0.3985	0.055*
H24C	0.0405	0.1639	0.3990	0.055*
C25	−0.12493 (10)	0.2477 (2)	0.40422 (9)	0.0213 (4)
C26	−0.18177 (11)	0.1489 (2)	0.39071 (9)	0.0264 (4)
H26	−0.2081	0.1344	0.3477	0.032*
C27	−0.19975 (12)	0.0718 (2)	0.44008 (11)	0.0331 (5)
H27	−0.2384	0.0045	0.4310	0.040*
C28	−0.16106 (13)	0.0932 (2)	0.50266 (10)	0.0349 (5)
H28	−0.1727	0.0390	0.5363	0.042*
C29	−0.10558 (13)	0.1929 (2)	0.51646 (10)	0.0332 (5)
H29	−0.0800	0.2084	0.5596	0.040*
C30	−0.08741 (11)	0.2704 (2)	0.46722 (10)	0.0270 (4)
H30	−0.0493	0.3390	0.4766	0.032*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Co1	0.01383 (11)	0.01789 (13)	0.01645 (12)	−0.00248 (9)	0.00478 (9)	−0.00214 (9)
Br1	0.02365 (12)	0.02069 (10)	0.02575 (11)	−0.00797 (9)	0.00621 (9)	−0.00288 (8)
Cl1B	0.02365 (12)	0.02069 (10)	0.02575 (11)	−0.00797 (9)	0.00621 (9)	−0.00288 (8)
Br2	0.02453 (11)	0.03315 (13)	0.01809 (11)	−0.00704 (8)	0.00088 (8)	0.00079 (9)
Cl2B	0.02453 (11)	0.03315 (13)	0.01809 (11)	−0.00704 (8)	0.00088 (8)	0.00079 (9)
Si1	0.0143 (2)	0.0196 (2)	0.0175 (2)	−0.00021 (19)	0.00493 (18)	−0.00194 (19)
Si2	0.0131 (2)	0.0181 (2)	0.0194 (2)	−0.00038 (18)	0.00484 (18)	0.00186 (19)
Cl1	0.0285 (5)	0.0305 (3)	0.0253 (3)	−0.0063 (4)	0.0083 (3)	−0.0110 (2)
Br1C	0.0285 (5)	0.0305 (3)	0.0253 (3)	−0.0063 (4)	0.0083 (3)	−0.0110 (2)
Cl2	0.0168 (3)	0.0361 (5)	0.0258 (3)	−0.0055 (3)	−0.0003 (2)	0.0086 (3)
Br2C	0.0168 (3)	0.0361 (5)	0.0258 (3)	−0.0055 (3)	−0.0003 (2)	0.0086 (3)
N2	0.0144 (7)	0.0239 (8)	0.0197 (7)	0.0027 (6)	0.0060 (6)	0.0018 (6)
N3	0.0165 (7)	0.0176 (8)	0.0208 (8)	−0.0008 (6)	0.0041 (6)	0.0016 (6)
N4	0.0174 (7)	0.0198 (8)	0.0251 (8)	0.0022 (6)	0.0097 (6)	0.0034 (6)
C1	0.0147 (8)	0.0266 (10)	0.0147 (8)	0.0005 (7)	0.0040 (7)	−0.0034 (7)
N1	0.0148 (7)	0.0242 (8)	0.0190 (8)	0.0031 (6)	0.0061 (6)	−0.0004 (6)
C2	0.0142 (8)	0.0253 (10)	0.0276 (10)	0.0054 (7)	0.0048 (7)	−0.0017 (8)
C3	0.013 (2)	0.028 (3)	0.050 (5)	0.0059 (18)	−0.009 (3)	−0.006 (3)
C4	0.023 (4)	0.032 (4)	0.040 (4)	0.001 (3)	0.010 (2)	−0.014 (3)
C5	0.026 (6)	0.075 (6)	0.040 (4)	0.020 (4)	0.012 (4)	0.023 (4)
C3A	0.027 (3)	0.031 (3)	0.081 (8)	0.003 (2)	−0.020 (5)	−0.009 (5)
C4A	0.042 (7)	0.050 (7)	0.039 (4)	0.020 (5)	0.016 (4)	−0.002 (4)
C5A	0.016 (5)	0.054 (5)	0.054 (6)	0.020 (3)	0.007 (4)	0.026 (5)
C6	0.0150 (8)	0.0274 (10)	0.0217 (9)	0.0059 (7)	0.0052 (7)	0.0040 (8)
C7	0.0278 (11)	0.0511 (14)	0.0229 (10)	0.0143 (10)	−0.0005 (8)	0.0013 (10)
C8	0.0337 (12)	0.0306 (11)	0.0337 (12)	0.0105 (9)	0.0038 (9)	−0.0004 (9)
C9	0.0206 (10)	0.0423 (13)	0.0619 (16)	0.0109 (9)	0.0182 (10)	0.0188 (12)
C10	0.0124 (8)	0.0337 (11)	0.0217 (9)	0.0040 (8)	0.0051 (7)	0.0055 (8)
C11	0.0236 (10)	0.0320 (11)	0.0322 (11)	−0.0004 (9)	0.0079 (8)	0.0070 (9)
C12	0.0223 (10)	0.0372 (13)	0.0551 (15)	−0.0043 (9)	0.0061 (10)	0.0142 (11)
C13	0.0220 (11)	0.0682 (18)	0.0521 (15)	−0.0009 (11)	0.0140 (11)	0.0321 (14)
C14	0.0263 (11)	0.085 (2)	0.0301 (12)	0.0062 (12)	0.0136 (10)	0.0209 (13)
C15	0.0209 (10)	0.0581 (15)	0.0206 (10)	0.0022 (10)	0.0065 (8)	0.0057 (10)
C16	0.0124 (8)	0.0217 (9)	0.0212 (9)	−0.0035 (7)	0.0011 (7)	0.0016 (7)
C17	0.0213 (9)	0.0233 (10)	0.0312 (10)	0.0055 (8)	0.0130 (8)	0.0021 (8)
C18	0.079 (2)	0.0367 (14)	0.0683 (18)	0.0350 (14)	0.0524 (16)	0.0245 (13)
C19	0.0336 (12)	0.0329 (12)	0.0446 (13)	0.0052 (10)	0.0035 (10)	−0.0143 (10)
C20	0.0180 (10)	0.0532 (15)	0.0489 (14)	0.0021 (10)	0.0116 (10)	−0.0173 (12)
C21	0.0228 (9)	0.0154 (9)	0.0275 (10)	0.0019 (7)	0.0059 (8)	0.0000 (7)
C22	0.0231 (10)	0.0202 (10)	0.0389 (12)	0.0031 (8)	0.0096 (9)	−0.0006 (8)
C23	0.0329 (12)	0.0249 (11)	0.0503 (14)	−0.0083 (9)	0.0167 (10)	−0.0091 (10)
C24	0.0462 (13)	0.0298 (12)	0.0332 (12)	0.0169 (10)	0.0072 (10)	0.0066 (9)
C25	0.0187 (9)	0.0232 (10)	0.0221 (9)	0.0005 (7)	0.0050 (7)	0.0037 (7)
C26	0.0214 (9)	0.0339 (11)	0.0237 (10)	−0.0063 (8)	0.0046 (8)	0.0045 (8)
C27	0.0279 (11)	0.0375 (12)	0.0348 (12)	−0.0098 (9)	0.0089 (9)	0.0092 (10)
C28	0.0411 (13)	0.0378 (12)	0.0294 (11)	−0.0006 (10)	0.0157 (10)	0.0119 (10)
C29	0.0456 (13)	0.0330 (12)	0.0192 (10)	0.0007 (10)	0.0034 (9)	0.0047 (9)
C30	0.0304 (11)	0.0238 (10)	0.0248 (10)	−0.0044 (8)	0.0019 (8)	0.0009 (8)

Geometric parameters (Å, º) top

Co1—Cl1B	2.14 (2)	C7—H7C	0.9800
Co1—Cl2B	2.14 (2)	C8—H8A	0.9800
Co1—Si2	2.1828 (6)	C8—H8B	0.9800
Co1—Si1	2.1953 (6)	C8—H8C	0.9800
Co1—Br1	2.3600 (5)	C9—H9A	0.9800
Co1—Br2	2.3642 (5)	C9—H9B	0.9800
Si1—N1	1.8190 (15)	C9—H9C	0.9800
Si1—N2	1.8234 (16)	C10—C15	1.386 (3)
Si1—Cl1	2.0950 (11)	C10—C11	1.390 (3)
Si1—Br1C	2.12 (2)	C11—C12	1.387 (3)
Si1—C1	2.2763 (19)	C11—H11	0.9500
Si2—N3	1.8164 (16)	C12—C13	1.377 (4)
Si2—N4	1.8168 (16)	C12—H12	0.9500
Si2—Cl2	2.1099 (11)	C13—C14	1.372 (4)
Si2—Br2C	2.12 (2)	C13—H13	0.9500
Si2—C16	2.2715 (19)	C14—C15	1.394 (3)
N2—C1	1.347 (2)	C14—H14	0.9500
N2—C6	1.484 (2)	C15—H15	0.9500
N3—C16	1.340 (2)	C16—C25	1.482 (3)
N3—C21	1.489 (2)	C17—C19	1.519 (3)
N4—C16	1.337 (2)	C17—C18	1.522 (3)
N4—C17	1.484 (2)	C17—C20	1.523 (3)
C1—N1	1.331 (2)	C18—H18A	0.9800
C1—C10	1.487 (3)	C18—H18B	0.9800
N1—C2	1.488 (2)	C18—H18C	0.9800
C2—C4A	1.499 (9)	C19—H19A	0.9800
C2—C5	1.505 (9)	C19—H19B	0.9800
C2—C3A	1.522 (8)	C19—H19C	0.9800
C2—C3	1.529 (7)	C20—H20A	0.9800
C2—C5A	1.530 (9)	C20—H20B	0.9800
C2—C4	1.537 (8)	C20—H20C	0.9800
C3—H3A	0.9800	C21—C23	1.521 (3)
C3—H3B	0.9800	C21—C24	1.525 (3)
C3—H3C	0.9800	C21—C22	1.528 (3)
C4—H4A	0.9800	C22—H22A	0.9800
C4—H4B	0.9800	C22—H22B	0.9800
C4—H4C	0.9800	C22—H22C	0.9800
C5—H5A	0.9800	C23—H23A	0.9800
C5—H5B	0.9800	C23—H23B	0.9800
C5—H5C	0.9800	C23—H23C	0.9800
C3A—H3A1	0.9800	C24—H24A	0.9800
C3A—H3A2	0.9800	C24—H24B	0.9800
C3A—H3A3	0.9800	C24—H24C	0.9800
C4A—H4A1	0.9800	C25—C30	1.389 (3)
C4A—H4A2	0.9800	C25—C26	1.396 (3)
C4A—H4A3	0.9800	C26—C27	1.388 (3)
C5A—H5A1	0.9800	C26—H26	0.9500
C5A—H5A2	0.9800	C27—C28	1.386 (3)
C5A—H5A3	0.9800	C27—H27	0.9500
C6—C7	1.520 (3)	C28—C29	1.384 (3)
C6—C9	1.523 (3)	C28—H28	0.9500
C6—C8	1.524 (3)	C29—C30	1.389 (3)
C7—H7A	0.9800	C29—H29	0.9500
C7—H7B	0.9800	C30—H30	0.9500

Cl1B—Co1—Cl2B	113.5 (11)	C9—C6—C8	109.75 (17)
Cl1B—Co1—Si2	143.4 (8)	C6—C7—H7A	109.5
Cl2B—Co1—Si2	87.8 (7)	C6—C7—H7B	109.5
Cl1B—Co1—Si1	89.2 (8)	H7A—C7—H7B	109.5
Cl2B—Co1—Si1	136.7 (9)	C6—C7—H7C	109.5
Si2—Co1—Si1	95.01 (3)	H7A—C7—H7C	109.5
Si2—Co1—Br1	155.844 (19)	H7B—C7—H7C	109.5
Si1—Co1—Br1	90.479 (19)	C6—C8—H8A	109.5
Si2—Co1—Br2	86.85 (2)	C6—C8—H8B	109.5
Si1—Co1—Br2	152.552 (19)	H8A—C8—H8B	109.5
Br1—Co1—Br2	98.967 (17)	C6—C8—H8C	109.5
N1—Si1—N2	71.94 (7)	H8A—C8—H8C	109.5
N1—Si1—Cl1	100.56 (6)	H8B—C8—H8C	109.5
N2—Si1—Cl1	103.72 (7)	C6—C9—H9A	109.5
N1—Si1—Br1C	108.7 (6)	C6—C9—H9B	109.5
N2—Si1—Br1C	103.9 (8)	H9A—C9—H9B	109.5
N1—Si1—Co1	117.39 (6)	C6—C9—H9C	109.5
N2—Si1—Co1	123.41 (5)	H9A—C9—H9C	109.5
Cl1—Si1—Co1	125.73 (4)	H9B—C9—H9C	109.5
Br1C—Si1—Co1	121.1 (7)	C15—C10—C11	120.30 (19)
N1—Si1—C1	35.78 (7)	C15—C10—C1	120.20 (19)
N2—Si1—C1	36.27 (6)	C11—C10—C1	119.40 (17)
Cl1—Si1—C1	107.19 (6)	C12—C11—C10	119.8 (2)
Br1C—Si1—C1	112.4 (7)	C12—C11—H11	120.1
Co1—Si1—C1	126.48 (5)	C10—C11—H11	120.1
N3—Si2—N4	72.16 (7)	C13—C12—C11	119.9 (2)
N3—Si2—Cl2	102.72 (6)	C13—C12—H12	120.1
N4—Si2—Cl2	100.31 (6)	C11—C12—H12	120.1
N3—Si2—Br2C	93.8 (5)	C14—C13—C12	120.3 (2)
N4—Si2—Br2C	96.3 (7)	C14—C13—H13	119.8
N3—Si2—Co1	123.35 (5)	C12—C13—H13	119.8
N4—Si2—Co1	119.33 (6)	C13—C14—C15	120.7 (2)
Cl2—Si2—Co1	125.40 (3)	C13—C14—H14	119.7
Br2C—Si2—Co1	133.7 (5)	C15—C14—H14	119.7
N3—Si2—C16	36.14 (7)	C10—C15—C14	118.9 (2)
N4—Si2—C16	36.06 (7)	C10—C15—H15	120.5
Cl2—Si2—C16	105.47 (5)	C14—C15—H15	120.5
Br2C—Si2—C16	97.5 (5)	N4—C16—N3	106.13 (15)
Co1—Si2—C16	128.85 (5)	N4—C16—C25	127.69 (17)
C1—N2—C6	130.91 (16)	N3—C16—C25	126.17 (17)
C1—N2—Si1	90.50 (11)	N4—C16—Si2	53.10 (9)
C6—N2—Si1	138.41 (12)	N3—C16—Si2	53.09 (9)
C16—N3—C21	131.82 (15)	C25—C16—Si2	177.91 (13)
C16—N3—Si2	90.77 (11)	N4—C17—C19	111.20 (16)
C21—N3—Si2	135.63 (12)	N4—C17—C18	105.38 (15)
C16—N4—C17	132.21 (16)	C19—C17—C18	109.5 (2)
C16—N4—Si2	90.84 (11)	N4—C17—C20	109.62 (17)
C17—N4—Si2	136.69 (13)	C19—C17—C20	111.40 (18)
N1—C1—N2	106.05 (15)	C18—C17—C20	109.6 (2)
N1—C1—C10	126.26 (16)	C17—C18—H18A	109.5
N2—C1—C10	127.63 (17)	C17—C18—H18B	109.5
N1—C1—Si1	53.03 (9)	H18A—C18—H18B	109.5
N2—C1—Si1	53.23 (9)	C17—C18—H18C	109.5
C10—C1—Si1	173.88 (13)	H18A—C18—H18C	109.5
C1—N1—C2	132.74 (15)	H18B—C18—H18C	109.5
C1—N1—Si1	91.19 (11)	C17—C19—H19A	109.5
C2—N1—Si1	136.07 (13)	C17—C19—H19B	109.5
N1—C2—C4A	111.0 (7)	H19A—C19—H19B	109.5
N1—C2—C5	108.4 (7)	C17—C19—H19C	109.5
N1—C2—C3A	111.6 (5)	H19A—C19—H19C	109.5
C4A—C2—C3A	113.0 (6)	H19B—C19—H19C	109.5
N1—C2—C3	112.6 (4)	C17—C20—H20A	109.5
C5—C2—C3	111.2 (6)	C17—C20—H20B	109.5
N1—C2—C5A	103.4 (6)	H20A—C20—H20B	109.5
C4A—C2—C5A	110.3 (8)	C17—C20—H20C	109.5
C3A—C2—C5A	106.9 (7)	H20A—C20—H20C	109.5
N1—C2—C4	107.9 (7)	H20B—C20—H20C	109.5
C5—C2—C4	109.1 (8)	N3—C21—C23	108.90 (16)
C3—C2—C4	107.6 (5)	N3—C21—C24	112.52 (16)
C2—C3—H3A	109.5	C23—C21—C24	111.09 (18)
C2—C3—H3B	109.5	N3—C21—C22	105.87 (15)
H3A—C3—H3B	109.5	C23—C21—C22	109.45 (17)
C2—C3—H3C	109.5	C24—C21—C22	108.86 (17)
H3A—C3—H3C	109.5	C21—C22—H22A	109.5
H3B—C3—H3C	109.5	C21—C22—H22B	109.5
C2—C4—H4A	109.5	H22A—C22—H22B	109.5
C2—C4—H4B	109.5	C21—C22—H22C	109.5
H4A—C4—H4B	109.5	H22A—C22—H22C	109.5
C2—C4—H4C	109.5	H22B—C22—H22C	109.5
H4A—C4—H4C	109.5	C21—C23—H23A	109.5
H4B—C4—H4C	109.5	C21—C23—H23B	109.5
C2—C5—H5A	109.5	H23A—C23—H23B	109.5
C2—C5—H5B	109.5	C21—C23—H23C	109.5
H5A—C5—H5B	109.5	H23A—C23—H23C	109.5
C2—C5—H5C	109.5	H23B—C23—H23C	109.5
H5A—C5—H5C	109.5	C21—C24—H24A	109.5
H5B—C5—H5C	109.5	C21—C24—H24B	109.5
C2—C3A—H3A1	109.5	H24A—C24—H24B	109.5
C2—C3A—H3A2	109.5	C21—C24—H24C	109.5
H3A1—C3A—H3A2	109.5	H24A—C24—H24C	109.5
C2—C3A—H3A3	109.5	H24B—C24—H24C	109.5
H3A1—C3A—H3A3	109.5	C30—C25—C26	119.87 (18)
H3A2—C3A—H3A3	109.5	C30—C25—C16	120.35 (17)
C2—C4A—H4A1	109.5	C26—C25—C16	119.75 (17)
C2—C4A—H4A2	109.5	C27—C26—C25	119.94 (19)
H4A1—C4A—H4A2	109.5	C27—C26—H26	120.0
C2—C4A—H4A3	109.5	C25—C26—H26	120.0
H4A1—C4A—H4A3	109.5	C28—C27—C26	119.8 (2)
H4A2—C4A—H4A3	109.5	C28—C27—H27	120.1
C2—C5A—H5A1	109.5	C26—C27—H27	120.1
C2—C5A—H5A2	109.5	C29—C28—C27	120.51 (19)
H5A1—C5A—H5A2	109.5	C29—C28—H28	119.7
C2—C5A—H5A3	109.5	C27—C28—H28	119.7
H5A1—C5A—H5A3	109.5	C28—C29—C30	119.9 (2)
H5A2—C5A—H5A3	109.5	C28—C29—H29	120.0
N2—C6—C7	109.59 (15)	C30—C29—H29	120.0
N2—C6—C9	105.40 (15)	C29—C30—C25	119.97 (19)
C7—C6—C9	110.31 (18)	C29—C30—H30	120.0
N2—C6—C8	111.32 (15)	C25—C30—H30	120.0
C7—C6—C8	110.36 (17)

Footnotes

¹Supporting information is available from the IUCr electronic archives (Reference: AJ5242).

Acknowledgements

We thank the Danish National Research Foundation (DNRF93) funded Centre for Materials Crystallography (CMC) for support. GMS thanks the Volkswagen Stiftung for a Niedersachsen (emeritus) Professorship. The authors thank INCOATEC, Geesthacht, for providing the crystals of 1 and 2, Professor Scherer, Augsburg, and Professor Pöttgen, Münster, for sample 4, and Visscher MSc, Göttingen, for sample 5.

References

Arndt, U. W. (1990). J. Appl. Cryst. 23, 161–168. CrossRef Web of Science IUCr Journals Google Scholar
Azhakar, R., Ghadwal, R. S., Roesky, H. W., Hey, J., Krause, L. & Stalke, D. (2013). Dalton Trans. 42, 10277–10281. Web of Science CSD CrossRef CAS PubMed Google Scholar
Becker, P. J. & Coppens, P. (1974a). Acta Cryst. A30, 129–147. CrossRef IUCr Journals Web of Science Google Scholar
Becker, P. J. & Coppens, P. (1974b). Acta Cryst. A30, 148–153. CrossRef IUCr Journals Web of Science Google Scholar
Blessing, R. H. (1995). Acta Cryst. A51, 33–38. CrossRef CAS Web of Science IUCr Journals Google Scholar
Blessing, R. H. (1997). J. Appl. Cryst. 30, 421–426. CrossRef CAS Web of Science IUCr Journals Google Scholar
Borek, D., Minor, W. & Otwinowski, Z. (2003). Acta Cryst. D59, 2031–2038. Web of Science CrossRef CAS IUCr Journals Google Scholar
Bruker (2009). APEX2 (Version 2.2012.2 0) and SAINT (Version 7.68A). Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Bruker (2014). XPREP (Version 2014/2) and SADABS (Version 2014/4). Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Busing, W. R. & Levy, H. A. (1957). Acta Cryst. 10, 180–182. CrossRef CAS IUCr Journals Web of Science Google Scholar
Coles, S. J. & Gale, P. A. (2012). Chem. Sci. 3, 683–689. Web of Science CSD CrossRef CAS Google Scholar
Coles, S. J. & Hursthouse, M. B. (2004). J. Appl. Cryst. 37, 988–992. Web of Science CSD CrossRef CAS IUCr Journals Google Scholar
Diederichs, K. (2010). Acta Cryst. D66, 733–740. Web of Science CrossRef CAS IUCr Journals Google Scholar
Dubler, E., Vedani, A. & Oswald, H. R. (1983). Acta Cryst. C39, 1143–1146. CrossRef CAS Web of Science IUCr Journals Google Scholar
Eickerling, G., Hauf, C., Scheidt, E.-W., Reichardt, L., Schneider, C., Muñoz, A., Lopez-Moreno, S., Humberto Romero, A., Porcher, F., André, G., Pöttgen, R. & Scherer, W. (2013). Z. Anorg. Allg. Chem. 639, 1985–1995. Web of Science CrossRef CAS Google Scholar
Evans, P. R. & Murshudov, G. N. (2013). Acta Cryst. D69, 1204–1214. Web of Science CrossRef CAS IUCr Journals Google Scholar
Farrugia, L. J. (2007). Acta Cryst. E63, i142. Web of Science CrossRef IUCr Journals Google Scholar
Görbitz, C. H. (1999). Acta Cryst. B55, 1090–1098. Web of Science CSD CrossRef IUCr Journals Google Scholar
Gruner, S. M., Tate, M. W. & Eikenberry, E. F. (2002). Rev. Sci. Instrum. 73, 2815–2842. Web of Science CrossRef CAS Google Scholar
Hamilton, W. C. (1965). Acta Cryst. 18, 502–510. CrossRef CAS IUCr Journals Web of Science Google Scholar
Harmening, T., van Wüllen, L., Eckert, H., Rodewald, U. C. & Pöttgen, R. (2010). Z. Anorg. Allg. Chem. 636, 972–976. Web of Science CrossRef CAS Google Scholar
Hasse, B., Wiesmann, J., Michaelsen, C., Heidorn, U., Kroth, S. & Hertlein, F. (2010). State-of-the-Art Multilayer Optics for X-ray Diffractometry. Geesthacht: Incoatec. Google Scholar
Henn, J. & Meindl, K. (2010). Acta Cryst. A66, 676–684. Web of Science CrossRef CAS IUCr Journals Google Scholar
Huber, R. & Kopfmann, G. (1969). Acta Cryst. A25, 143–152. CrossRef CAS IUCr Journals Web of Science Google Scholar
Hübschle, C. B., Sheldrick, G. M. & Dittrich, B. (2011). J. Appl. Cryst. 44, 1281–1284. Web of Science CrossRef IUCr Journals Google Scholar
Jørgensen, M. R. V., Svendsen, H., Schmøkel, M. S., Overgaard, J. & Iversen, B. B. (2012). Acta Cryst. A68, 301–303. Web of Science CrossRef IUCr Journals Google Scholar
Kabsch, W. (2010). Acta Cryst. D66, 133–144. Web of Science CrossRef CAS IUCr Journals Google Scholar
Katayama, C. (1986). Acta Cryst. A42, 19–23. CrossRef CAS Web of Science IUCr Journals Google Scholar
Kopfmann, G. & Huber, R. (1968). Acta Cryst. A24, 348–351. CrossRef IUCr Journals Web of Science Google Scholar
North, A. C. T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351–359. CrossRef IUCr Journals Web of Science Google Scholar
Rohrmoser, B., Eickerling, G., Presnitz, M., Scherer, W., Eyert, V., Hoffmann, R.-D., Rodewald, U. C., Vogt, C. & Pöttgen, R. (2007). J. Am. Chem. Soc. 129, 9356–9365. Web of Science CSD CrossRef PubMed CAS Google Scholar
Saouane, S., Norman, S. E., Hardacre, C. & Fabbiani, F. P. A. (2013). Chem. Sci. 4, 1270–1280. Web of Science CSD CrossRef CAS Google Scholar
Scherer, W., Hauf, C., Presnitz, M., Scheidt, E.-W., Eickerling, G., Eyert, V., Hoffmann, R.-D., Rodewald, U. C., Hammerschmidt, A., Vogt, C. & Pöttgen, R. (2010). Angew. Chem. 122, 1623–1627. CrossRef Google Scholar
Schulz, T., Meindl, K., Leusser, D., Stern, D., Graf, J., Michaelsen, C., Ruf, M., Sheldrick, G. M. & Stalke, D. (2009). J. Appl. Cryst. 42, 885–891. Web of Science CSD CrossRef CAS IUCr Journals Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Storm, A. B., Michaelsen, C., Oehr, A. & Hoffmann, C. (2004). Proc. SPIE, 5557, 177–181. CrossRef Google Scholar
Weiss, M. S. (2001). J. Appl. Cryst. 34, 130–135. Web of Science CrossRef CAS IUCr Journals Google Scholar

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