INSTRUMENTATION AND EXPERIMENTAL TECHNIQUES

structures determination and for application of the Rietveld method in P.01.08.9

quantitative phase analysis. The utilization of this instrument is open Acta Cryst. (2005). A61, C144
for the brazilian and latin-american scientific and technological Design of a High Resolution Macromolecular Neutron
communities. Diffractometer (MaNDi) for Structural Biology Research at the
The authors acknowledge the financial supports given by SNS
Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP), Pappannan Thiyagarajan1, A. J. Schultz1, C. Rehm2, J. P. Hodges2,
under project no. 95/05173-0, and Ministério da Ciência e Tecnologia D.A. Myles3, P. A. Langan4, A.D. Mesecar5, 1IPNS, Argonne National
(MCT), under project no. 62.00007/98-2. Laboratory, Argonne, IL 60439. 2SNS, ORNL. 3CSMB, ORNL.
4
Keywords: neutron diffractometer, PSD detector, focusing Biology Division, LANL. 5University of Illinois, Department of
monochromator Medicinal Chemistry and Pharmacognosy, Chicago. E-mail:
[email protected]
P.01.08.7
Acta Cryst. (2005). A61, C144 With the advent of third-generation synchrotron X-ray sources, it
The new Single Crystal Diffractometer HEiDi at the FRM-II and was envisioned that ultra-high resolution macromolecular
its Applications crystallography (UHRXMC) at resolutions of 0.5 Å to 1.0 Å would
Martin Mevena, Vladimir Hutanua,b, Gernot Hegerb, aZWE FRM-II, provide detailed information on the positions of critical hydrogen
TU München, Germany. bInstitut für Kristallographie, RWTH Aachen, atoms within the active sites of enzymes. To date, in about 82
Germany. E-mail: [email protected] structures in the PDB in this resolution range, significant numbers of
hydrogen atoms including those in the active sites could not be
HEiDi, one of the new single crystal diffractometers of the identified. Furthermore, only about 0.5% of all macromolecular
research neutron source FRM-II, was designed to cover a wide area of structures in the PDB are amenable to UHRXMC and hence other
scientific applications in crystal structure analysis. It uses the high complementary techniques are needed for the identification of critical
flux of fast neutrons with short wavelengths from the hot source of the hydrogen atoms involved in the catalytic mechanisms in a majority of
FRM-II. The enlargement of the visible reciprocal space (=Q-space) enzyme systems.
allows very accurate determinations of nuclear positions in single Neutron Macromolecular Crystallography (NMC) has been shown
crystals as well as more detailed quantitative informations about mean to provide accurate proton positions, protonation states and hydration
square displacements and vacancies which is of interest in reference to states, as well as hydrogen/deuterium exchange, in macromolecular
static or dynamic disorder effects and phase transitions. The Q- crystals even at moderate 2 Å to 2.5 Å resolution. One major
dependences of the magnetic and the nuclear cross sections of bottleneck that severely constrains the productivity of NMC is the
neutrons are quite different. This can be used to determine the limited flux at the current sources and the requirement of large
magnetic and the nuclear order in a crystal separately. Other crystals. The advent of the Spallation Neutron Source (SNS), with
advantages of shorter neutron wavelengths (1.4 Å down to 0.3 Å) are over an order of magnitude increase in neutron flux, the advances in
the significant reduction of absorption effects in compounds with neutron optics and detectors, as well as advances in structure
highly absorbing elements (e.g. Sm, Gd) and the reduction of genomics and deuteration. provide an exciting opportunity to push the
extinction effects. NMC field to new horizons. Hence we propose to develop a dedicated
During the nuclear commissioning of the FRM-II in 2004 started world-class high resolution time-of-flight single crystal
the adjustment and characterization of HEiDi with neutron radiation. macromolecular neutron diffractometer (MaNDi) for structural
First experimental results are quite promising, e.g. an excellent biology research at the SNS. MaNDi has been designed to be able to
resolution function (<0.1° at min.) or a perfect alignment between the collect a full hemisphere of Bragg data with a resolution of 1.5 to 2 Å
calculated and the measured gain factor of 2.5 of the monochromator on a crystal with a lattice constant up to 150 Å in 1 to 7 days. The
focussing unit. Further experimental results from the instrument and higher throughput and resolution are accomplished by the use of a
typical applications like structural phase transitions, local disorder (H wide wavelength bandwidth of cold neutrons (1.8 Å < Ȝ < 4.5 Å)
bonds in RDP) or magnetism will be presented on the conference. sorted into a large number of high resolution wavelength channels by
Keywords: neutron and X-ray diffractometry, single crystal time-of-flight and by an array of high resolution position-sensitive
structure analysis, neutron instrumentation area detectors covering a large solid angle. We envision that the
unprecedented high data rates and resolution with MaNDi will open
P.01.08.8 up new avenues and greatly advance the field of structural biology,
Acta Cryst. (2005). A61, C144 enzymology and protein dynamics.
The Italian Neutron Experimental Station (INES) at ISIS: Status Work at IPNS was funded by the U.S. DOE, BES-Materials Science, under
and Development Contract W-31-109-ENG-38 to U. Chicago, and at SNS by the U.S. DOE,
Francesco Grazzi, Ubaldo Bafile, Milva Celli, Daniele Colognesi, BES-MS. under contract DE-AC05-00OR22725UT-Battelle, LLC and ORAU.
Marco Zoppi, ISC-CNR, Florence, Italy. E-mail: [email protected] Keywords: neutron macromolecular crystallography, time-of-
flight single crystal diffractometer, structural biology
The INES project concerns the realization of a multipurpose
experimental station, built by CNR at the ISIS pulsed neutron source P.01.08.10
(Rutherford Appleton Laboratory, UK). This instrument is mainly Acta Cryst. (2005). A61, C144-C145
intended to operate as test and training facility for the Italian neutron- Advances in Neutron Single Crystal Diffraction towards a Smaller
scattering community. The experimental station is equipped with a Sample Sizes
multipurpose time-of-flight neutron diffractometer, presently under Christina Hoffmanna, Alexandru Stoicaa, Arthur Schultzb, Paula
commissioning. This is located downstream a water moderator of the Piccolib, Robert Bauc, Thomas Koetzleb, aSpallation Neutron Source
neutron source, with an excellent time-resolution. In the present Oak Ridge National Laboratory, USA. bIntense Pulsed Neutron
configuration the INES diffractometer contains a highly-efficient large Source, Argonne National Laboratory, USA. cDepartment of
detector area covering a range of about 170o on the horizontal plane. Chemisty, University of Southern California, Los Angeles, USA. E-
Moreover it offers a large sample volume (about 0.25 m3), allowing mail: [email protected]
the study of almost any kind of object, including bulky archaeological
artifacts. The possibility to separately analyze each single detector Single crystal diffraction has been used as a tool for structure
makes texture analysis also possible. The opportunity to operate analysis since the discovery of neutron scattering. Complementary to
experiments in particular thermodynamic conditions (i.e. high X-ray radiation neutron radiation is especially useful to locate ‘light’
pressure, high and low temperatures) is also under investigation. elements like hydrogen next to ‘heavy’ elements like metals.
Keywords: neutron istrumentation, texture analysis, Furthermore, neutrons are much “gentler” to organic crystals. A major
archaeometry obstacle for neutron diffraction is the moderate flux and therefore the
significantly larger single crystal sizes and longer data collection
times needed for a decent data set.

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