Successful protein cryocooling for powder diffraction

2007 ◽  
Vol 40 (1) ◽  
pp. 121-124 ◽  
Author(s):  
Mark J. Jenner ◽  
Jonathan P. Wright ◽  
Irene Margiolaki ◽  
Andrew N. Fitch
Keyword(s):  
Powder Diffraction ◽  
Room Temperature ◽  
Egg White ◽  
Powder Diffraction Data ◽  
High Quality ◽  
X Ray ◽  
Egg White Lysozyme ◽  
Diffraction Peaks ◽  
Better Than

It is shown that samples of microcrystalline tetragonal chicken egg white lysozyme can be effectively cryoprotected for high-resolution synchrotron X-ray powder diffraction studies at 100 K. The survival of the powder in the beam is increased by a factor of around 30. Thus, a high-quality powder diffraction pattern could be collected at 100 K, which attains a resolution ofdmin≃ 2.6 Å, significantly better than the previous limit of ∼3.27 Å at room temperature, despite a smaller volume of sample. Systematic variations of the concentration and type of cryoprotectant agent show that the lattice microstrains that accompany cooling, and degrade the quality of the powder diffraction data by broadening the diffraction peaks, are caused by a collapse in the volume of the crystalline unit cell.

Rietveld Structure Refinement of Metastable Lithium Disilicate Using Synchrotron X-Ray Powder Diffraction Data From the Daresbury SRS 8.3 Diffractometer

1990 ◽  
Vol 5 (3) ◽  
pp. 137-143 ◽  
Author(s):  
R.I. Smith ◽  
A.R. West ◽  
I. Abrahams ◽  
P.G. Bruce
Keyword(s):  
Crystal Structure ◽  
Powder Diffraction ◽  
Diffraction Data ◽  
Rietveld Method ◽  
Structure Refinement ◽  
Powder Diffraction Data ◽  
X Ray ◽  
New Instrument ◽  
Diffraction Peaks

AbstractThe crystal structure of metastable Li2Si2O5, Fw = 150.05, has been refined by the Rietveld method using high resolution X-ray powder diffraction data recorded at the Daresbury Synchrotron Radiation Source on the new 8.3 diffractometer. Li2Si2O5, in keeping with many compounds of interest to the materials scientist, exhibits relatively broad diffraction peaks. It is important to establish the quality of crystal structure data that may be obtained from such materials on this new instrument. Various functions were used to model the peak shape from this instrument; a split-Pearson VII function appeared to be marginally superior to Pearson VII or Pseudo-Voigt functions. Refinement was carried out using the split-Pearson VII in the space group Pbcn (60) and terminated with a = 5.6871(6), b = 4.7846(5), c = 14.645(1) Å, V = 398.50 Å3, Z=4, Dc= 2.502 gcm−3, Rwp = 17.06, Rex = 14.48 and Χ2 = 1.39. The refined parameters are compared with those obtained from a previous single crystal X-ray determination.

Improvement of X-ray powder diffraction patterns of the spin transition polymer [Fe(Htrz)3](ClO4)2⋅1.85H2O

2001 ◽  
Vol 16 (1) ◽  
pp. 37-41 ◽  
Author(s):  
E. Smit ◽  
B. Manoun ◽  
S. M. C. Verryn ◽  
D. de Waal
Keyword(s):  
Powder Diffraction ◽  
Diffraction Data ◽  
Spin Transition ◽  
Powder Diffraction Data ◽  
High Quality ◽  
Monoclinic System ◽  
X Ray ◽  
Cell Parameters ◽  
Diffraction Patterns

The effects of proper drying and grinding of [Fe(Htrz)3](ClO4)2⋅1.85H2O specimens on the quality of X-ray powder patterns are illustrated (Htrz=1H-1,2,4-Triazole). A procedure is suggested to achieve high-quality, reproducible X-ray powder patterns of the compound. The observed powder diffraction data of the compound are reported together with preliminary indices calculated for a monoclinic system with cell parameters a=15.8160 Å, b=20.6134 Å, c=13.0321 Å, β=103.83° and Volume=4125.633 Å3, with reliability factors: M15=10.4, F15=22.0 (0.0100; 68) and space group P21/m. This compound is very similar to the compound [Cu(Hyetrz)3](ClO4)2⋅3H2O and a comparison is made between the cell parameters of the two compounds

Crystal structure of the anticancer drug carmustine determined by X-ray powder diffraction

2021 ◽  
pp. 1-3
Author(s):  
Carina Schlesinger ◽  
Edith Alig ◽  
Martin U. Schmidt
Keyword(s):  
Crystal Structure ◽  
Anticancer Drug ◽  
Powder Diffraction ◽  
Room Temperature ◽  
Powder Diffraction Data ◽  
Orthorhombic Space Group ◽  
Commercial Sample ◽  
One Dimensional ◽  
X Ray ◽  
Hydrogen Bond Pattern

The structure of the anticancer drug carmustine (1,3-bis(2-chloroethyl)-1-nitrosourea, C5H9Cl2N3O2) was successfully determined from laboratory X-ray powder diffraction data recorded at 278 K and at 153 K. Carmustine crystallizes in the orthorhombic space group P212121 with Z = 4. The lattice parameters are a = 19.6935(2) Å, b = 9.8338(14) Å, c = 4.63542(6) Å, V = 897.71(2) ų at 153 K, and a = 19.8522(2) Å, b = 9.8843(15) Å, c = 4.69793(6) Å, V = 921.85(2) ų at 278 K. The Rietveld fits are very good, with low R-values and smooth difference curves of calculated and experimental powder data. The molecules form a one-dimensional hydrogen bond pattern. At room temperature, the investigated commercial sample of carmustine was amorphous.

The crystal structures of solvent-free alkali-metal squarates from powder diffraction data

2005 ◽  
Vol 220 (11) ◽  
Author(s):  
Robert E. Dinnebier ◽  
Hanne Nuss ◽  
Martin Jansen
Keyword(s):  
High Resolution ◽  
Alkali Metal ◽  
Crystal Structures ◽  
Powder Diffraction ◽  
Diffraction Data ◽  
Room Temperature ◽  
Solvent Free ◽  
Crystallographic Data ◽  
Powder Diffraction Data ◽  
X Ray

AbstractThe crystal structures of solvent-free lithium, sodium, rubidium, and cesium squarates have been determined from high resolution synchrotron and X-ray laboratory powder patterns. Crystallographic data at room temperature of Li

High Quality Hydrothermal ZnO Crystals

1998 ◽  
Vol 537 ◽  
Author(s):  
M. Suscavage ◽  
M. Harris ◽  
D. Bliss ◽  
P. Yip ◽  
S.-Q. Wang ◽  
...  
Keyword(s):  
Zinc Oxide ◽  
Liquid Helium ◽  
Room Temperature ◽  
Surface Preparation ◽  
Critical Factor ◽  
High Quality ◽  
Rocking Curve ◽  
X Ray ◽  
Oxide Crystals

AbstractZinc Oxide crystals have historically been grown in hydrothermal autoclaves with a basic mineralizer; however, doubts have been raised about the quality of such crystals because they have often exhibited large x-ray rocking curve widths and low photoluminescence (PL) yield with large linewidths. Several ZnO crystals were grown hydrothermally and sliced parallel to the c-plane. This resulted in opposite surfaces (the C+ and C-) exhibiting pronounced chemical and mechanical differences. Different surface treatments were investigated and compared by PL both at room temperature and liquid helium temperatures, and by double axis X-ray rocking curve measurements. The high quality of hydrothermally-grown ZnO is substantiated by the narrow rocking curve widths and sharp PL peaks obtained. A critical factor in obtaining these results was found to be surface preparation.

X-ray powder diffraction data for compound DyNiSn

1997 ◽  
Vol 12 (3) ◽  
pp. 134-135
Author(s):  
Liangqin Nong ◽  
Lingmin Zeng ◽  
Jianmin Hao
Keyword(s):  
Powder Diffraction ◽  
Diffraction Data ◽  
Figure Of Merit ◽  
Room Temperature ◽  
Unit Cell ◽  
Powder Diffraction Data ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Diffraction Patterns

The compound DyNiSn has been studied by X-ray powder diffraction. The X-ray diffraction patterns for this compound at room temperature are reported. DyNiSn is orthorhombic with lattice parameters a=7.1018(1) Å, b=7.6599(2) Å, c=4.4461(2) Å, space group Pna21 and 4 formula units of DyNiSn in unit cell. The Smith and Snyder Figure-of-Merit F30 for this powder pattern is 26.7(0.0178,63).

Synthesis and structure of the ternary nitride Li6WN4

2005 ◽  
Vol 20 (1) ◽  
pp. 18-21 ◽  
Author(s):  
W. X. Yuan ◽  
J. W. Hu ◽  
Y. T. Song ◽  
W. J. Wang ◽  
Y. P. Xu
Keyword(s):  
Crystal Structure ◽  
Thermal Stability ◽  
Room Temperature ◽  
Powder Diffraction Data ◽  
High Quality ◽  
X Ray ◽  
Cell Parameters ◽  
Tetragonal System ◽  
Ternary Nitride ◽  
Stability Measurements

The ternary nitridotungstate Li6WN4 has been synthesized via the solid state reaction of lithium subnitride, Li3N, with W under nitrogen. High quality X-ray powder diffraction data were collected for the crystal-structure determination. Li6WN4 crystallizes in the tetragonal system, space group P42∕nmc, with cell parameters a=6.6759(3) Å and c=4.9280(3) Å, Z=2. Preliminary thermal stability measurements of Li6WN4 show that it is sensitive to moisture, even at room temperature, and decomposes at high temperatures below 1000 °C under flowing nitrogen.

X-ray powder diffraction data for ErH2−xDx

2008 ◽  
Vol 23 (3) ◽  
pp. 259-264 ◽  
Author(s):  
Mark A. Rodriguez ◽  
Robert M. Ferrizz ◽  
Clark S. Snow ◽  
James F. Browning
Keyword(s):  
Powder Diffraction ◽  
Diffraction Data ◽  
Room Temperature ◽  
Lattice Parameter ◽  
Powder Diffraction Data ◽  
Mole Percent ◽  
X Ray ◽  
Cubic Lattice ◽  
Fluorite Type ◽  
Hydrogen Deuterium

X-ray powder diffraction data for ErH2−xDx formed by hydrogen (i.e., protium)–deuterium loading of Er metal are reported. Lattice parameters for the varying hydrogen–deuterium compositions followed Vergard’s law behavior. The cubic lattice parameter at room temperature for ErH2−xDx obeys a linear relationship according to the formula a=5.1287−1.1120×10−4⋅x, where a is the lattice parameter of the fluorite-type structure and x is the mole percent of deuterium. Microstrain measurements suggest a possible ordering of hydrogen and deuterium in the composition ErH1D1.

X-ray powder diffraction data of anilinium trimolybdate tetrahydrate and anilinium trimolybdate dihydrate

1999 ◽  
Vol 14 (4) ◽  
pp. 280-283 ◽  
Author(s):  
A. Rafalska-Łasocha ◽  
W. Łasocha ◽  
M. Michalec
Keyword(s):  
Powder Diffraction ◽  
Diffraction Data ◽  
Room Temperature ◽  
Unit Cell ◽  
Powder Diffraction Data ◽  
Unit Cell Parameters ◽  
Space Group ◽  
X Ray ◽  
Cell Parameters ◽  
Diffraction Patterns

The X-ray powder diffraction patterns of anilinium trimolybdate tetrahydrate, (C6H5NH3)2Mo3O10·4H2O, and anilinium trimolybdate dihyhydrate, (C6H5NH3)2Mo3O10·2H2O, have been measured in room temperature. The unit cell parameters were refined to a=11.0670(7) Å, b=7.6116(8) Å, c=25.554(3) Å, space group Pnma(62) and a=17.560(2) Å, b=7.5621(6) Å, c=16.284(2) Å, β=108.54(1)°, space group P21(4) or P21/m(11) for orthorhombic anilinium trimolybdate tetrahydrate and monoclinic anilinium trimolybdate dihydrate, respectively.

X-ray powder diffraction data of lapatinib ditosylate monohydrate

2009 ◽  
Vol 24 (3) ◽  
pp. 250-253 ◽  
Author(s):  
Peter Varlashkin
Keyword(s):  
Breast Cancer ◽  
Powder Diffraction ◽  
Diffraction Data ◽  
Room Temperature ◽  
Powder Diffraction Data ◽  
X Ray Diffraction ◽  
Unit Cell Parameters ◽  
X Ray ◽  
Cell Parameters ◽  
Diffraction Structure

The room temperature powder pattern of lapatinib ditosylate monohydrate (active ingredient in Tykerb used to treat refractory breast cancer) was indexed and the cell from the single crystal X-ray diffraction structure was refined using the experimental capillary data. Unit-cell parameters for the orthorhombic compound with space group Pbca refined from powder diffraction data are a=9.6850±0.0009 Å, b=29.364±0.003 Å, and c=30.733±0.003 Å, α=β=γ=90°, z=8, V=8740.1 Å3. Values of 2θ, d, I, and Miller indices are reported.

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