Considerations in the Maintenance and Dissemination of the Powder Diffraction File Database

2009 ◽  
pp. 117-117-10
Author(s):  
R Jenkins ◽  
MM Fornoff ◽  
MA Holomany ◽  
MM King
Keyword(s):  
Powder Diffraction ◽  
Powder Diffraction File

Crystal structure of pomalidomide Form I, C13H11N3O4

2021 ◽  
pp. 1-6
Author(s):  
James A. Kaduk ◽  
Amy M. Gindhart ◽  
Thomas N. Blanton
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Powder Diffraction ◽  
Density Functional ◽  
Double Layers ◽  
Carbonyl Groups ◽  
Hydrogen Atoms ◽  
Powder Diffraction File ◽  
Functional Theory ◽  
Amine Hydrogen

The crystal structure of pomalidomide Form I has been solved and refined using synchrotron X-ray powder diffraction data and optimized using density functional theory techniques. Pomalidomide Form I crystallizes in the space group P-1 (#2) with a = 7.04742(9), b = 7.89103(27), c = 11.3106(6) Å, α = 73.2499(13), β = 80.9198(9), γ = 88.5969(6)°, V = 594.618(8) Å3, and Z = 2. The crystal structure is characterized by the parallel stacking of planes parallel to the bc-plane. Hydrogen bonds link the molecules into double layers also parallel to the bc-plane. Each of the amine hydrogen atoms acts as a donor to a carbonyl group in an N–H⋯O hydrogen bond, but only two of the four carbonyl groups act as acceptors in such hydrogen bonds. Other carbonyl groups participate in C–H⋯O hydrogen bonds. The powder pattern has been submitted to ICDD® for inclusion in the Powder Diffraction File™ (PDF®).

Crystal structure of tamsulosin hydrochloride, C20H29N2O5SCl

2021 ◽  
pp. 1-7
Author(s):  
Nilan V. Patel ◽  
Joseph T. Golab ◽  
James A. Kaduk ◽  
Amy M. Gindhart ◽  
Thomas N. Blanton
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bond ◽  
Hydrogen Atom ◽  
Powder Diffraction ◽  
Density Functional ◽  
Carbon Chain ◽  
Strong Hydrogen Bond ◽  
Powder Diffraction File ◽  
Ether Oxygen ◽  
Sulfonamide Group

The crystal structure of tamsulosin hydrochloride has been solved and refined using synchrotron X-ray powder diffraction data and optimized using density functional techniques. Tamsulosin hydrochloride crystallizes in space group P21 (#4) with a = 7.62988(2), b = 9.27652(2), c = 31.84996(12) Å, β = 93.2221(2)°, V = 2250.734(7) Å3, and Z = 4. In the crystal structure, two arene rings are connected by a carbon chain oriented roughly parallel to the c-axis. The crystal structure is characterized by two slabs of tamsulosin hydrochloride molecules perpendicular to the c-axis. As expected, each of the hydrogens on the protonated nitrogen atoms makes a strong hydrogen bond to one of the chloride anions. The result is to link the cations and anions into columns along the b-axis. One hydrogen atom of each sulfonamide group also makes a hydrogen bond to a chloride anion. The other hydrogen atom of each sulfonamide group forms bifurcated hydrogen bonds to two ether oxygen atoms. The powder pattern is included in the Powder Diffraction File™ as entry 00-065-1415.

scholarly journals Crystal structure of pimecrolimus Form B, C43H68ClNO11

2021 ◽  
Vol 36 (1) ◽  
pp. 35-42
Author(s):  
Shivang Bhaskar ◽  
Joseph T. Golab ◽  
James A. Kaduk ◽  
Amy M. Gindhart ◽  
Thomas N. Blanton
Keyword(s):  
Crystal Structure ◽  
Powder Diffraction ◽  
Density Functional ◽  
Van Der Waals Interactions ◽  
Powder Diffraction File ◽  
X Ray ◽  
Weak Intermolecular Interactions ◽  
Significant Difference ◽  
Atomic Coordinates ◽  
Solid State Conformation

The crystal structure of pimecrolimus Form B has been solved and refined using synchrotron X-ray powder diffraction data and optimized using density functional techniques. Pimecrolimus crystallizes in the space group P21 (#4) with a = 15.28864(7), b = 13.31111(4), c = 10.95529(5) Å, β = 96.1542(3)°, V = 2216.649(9) Å3, and Z = 2. Although there are an intramolecular six-ring hydrogen bond and some larger chain and ring patterns, the crystal structure is dominated by van der Waals interactions. There is a significant difference between the conformation of the Rietveld-refined and the DFT-optimized structures in one portion of the macrocyclic ring. Although weak, intermolecular interactions are apparently important in determining the solid-state conformation. The powder pattern is included in the Powder Diffraction File™ (PDF®) as entry 00-066-1619. This study provides the atomic coordinates to be added to the PDF entry.

Crystal structure of donepezil hydrochloride form III, C24H29NO3⋅HCl

2021 ◽  
pp. 1-8
Author(s):  
Joel W. Reid ◽  
James A. Kaduk
Keyword(s):  
Crystal Structure ◽  
Density Functional Theory ◽  
Powder Diffraction ◽  
Density Functional ◽  
Chloride Anion ◽  
Powder Diffraction Data ◽  
Powder Diffraction File ◽  
Functional Theory ◽  
Monoclinic Lattice ◽  
Donepezil Hydrochloride

The crystal structure of donepezil hydrochloride, form III, has been solved with FOX using laboratory powder diffraction data previously submitted to and published in the Powder Diffraction File. Rietveld refinement with GSAS yielded monoclinic lattice parameters of a = 14.3662(9) Å, b = 11.8384(6) Å, c = 13.5572(7) Å, and β = 107.7560(26)° (C24H30ClNO3, Z = 4, space group P21/c). The Rietveld-refined structure was compared to a density functional theory (DFT)-optimized structure, and the structures exhibit excellent agreement. Layers of donepezil molecules parallel to the (101) planes are maintained by columns of chloride anions along the b-axis, where each chloride anion hydrogen bonds to three donepezil molecules each.

Crystal structure of ziprasidone hydrochloride monohydrate, C21H22Cl2N4OS(H2O)

2015 ◽  
Vol 30 (3) ◽  
pp. 192-198
Author(s):  
James A. Kaduk ◽  
Kai Zhong ◽  
Amy M. Gindhart ◽  
Thomas N. Blanton
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bond ◽  
Powder Diffraction ◽  
Density Functional ◽  
Minimum Energy ◽  
Strong Hydrogen Bond ◽  
Powder Diffraction File ◽  
X Ray ◽  
Hydrochloride Monohydrate ◽  
Positively Charged

The crystal structure of ziprasidone hydrochloride monohydrate has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional techniques. Ziprasidone hydrochloride monohydrate crystallizes in space group P-1 (#2) with a = 7.250 10(3), b = 10.986 66(8), c = 14.071 87(14) Å, α = 83.4310(4), β = 80.5931(6), γ = 87.1437(6)°, V = 1098.00(1) Å3, and Z = 2. The ziprasidone conformation in the solid state is very close to the minimum energy conformation. The positively-charged nitrogen in the ziprasidone makes a strong hydrogen bond with the chloride anion. The water molecule makes two weaker bonds to the chloride, and acts as an acceptor in an N–H⋯O hydrogen bond. The powder pattern is included in the Powder Diffraction File™ as entry 00-064-1492.

Crystal structure of oxybutynin hydrochloride hemihydrate, C22H32NO3Cl(H2O)0.5

2019 ◽  
Vol 34 (1) ◽  
pp. 50-58
Author(s):  
James A. Kaduk ◽  
Nicholas C. Boaz ◽  
Amy M. Gindhart ◽  
Thomas N. Blanton
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Powder Diffraction ◽  
Density Functional ◽  
Hydroxyl Group ◽  
Layered Crystal ◽  
Powder Diffraction File ◽  
X Ray ◽  
Layered Crystal Structure ◽  
Oxybutynin Hydrochloride

The crystal structure of oxybutynin hydrochloride hemihydrate has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional techniques. Oxybutynin hydrochloride hemihydrate crystallizes in space group I2/a (#15) with a = 14.57266(8), b = 8.18550(6), c = 37.16842(26) Å, β = 91.8708(4)°, V = 4421.25(7) Å3, and Z = 8. The compound exhibits X-ray-induced photoreduction of the triple bond. Prominent in the layered crystal structure is the N–H⋅⋅⋅Cl hydrogen bond between the cation and anion, as well as O–H⋅⋅⋅Cl hydrogen bonds from the water molecule and hydroxyl group of the oxybutynin cation. C–H⋅⋅⋅Cl hydrogen bonds also contribute to the crystal energy, and help determine the conformation of the cation. The powder pattern is included in the Powder Diffraction File™ as entry 00-068-1305.

Reference materials for the study of polymorphism and crystallinity in cellulosics

2013 ◽  
Vol 28 (1) ◽  
pp. 18-31 ◽  
Author(s):  
T. G. Fawcett ◽  
C. E. Crowder ◽  
S. N. Kabekkodu ◽  
F. Needham ◽  
J. A. Kaduk ◽  
...  
Keyword(s):  
Powder Diffraction ◽  
Reference Materials ◽  
Reference Data ◽  
Powder Diffraction File ◽  
Material Identification ◽  
Cellulosic Materials ◽  
Chemical Substitution

Eighty specimens of cellulosic materials were analyzed over a period of several years to study the diffraction characteristics resulting from polymorphism, crystallinity, and chemical substitution. The aim of the study was to produce and verify the quality of reference data useful for the diffraction analyses of cellulosic materials. These reference data can be used for material identification, polymorphism, and crystallinity measurements. Overall 13 new references have been characterized for publication in the Powder Diffraction File (PDF) and several others are in the process of publication.

Qualitative phase analysis system for crystalline mixtures based on X-ray powder diffraction file

2004 ◽  
Vol 19 (4) ◽  
pp. 340-346
Author(s):  
YuanYuan Qiao ◽  
YunFei Xi ◽  
DongTao Zhuo ◽  
Ji Jun Wang ◽  
ShaoFan Lin
Keyword(s):  
Phase Analysis ◽  
Powder Diffraction ◽  
Identification System ◽  
Phase Identification ◽  
Powder Diffraction File ◽  
X Ray ◽  
Analysis System ◽  
Qualitative Phase ◽  
Full Peak

A qualitative phase identification system for crystalline mixtures is presented. The system provides up to five-phase qualitative identification using up to nine-peak filtration, and additive full peak matching based on the powder diffraction file of ICDD. It was implemented using Microsoft Visual C++, and runs under most common Windows systems. Screenshots and examples are included.

Crystal structure of osimertinib mesylate Form B (Tagrisso), (C28H34N7O2)(CH3O3S)

2021 ◽  
pp. 1-9
Author(s):  
James A. Kaduk ◽  
Nicholas C. Boaz ◽  
Emma L. Markun ◽  
Amy M. Gindhart ◽  
Thomas N. Blanton
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bond ◽  
Hydrogen Bonds ◽  
Powder Diffraction ◽  
Density Functional ◽  
Amino Nitrogen ◽  
Strong Hydrogen Bond ◽  
Powder Diffraction File ◽  
Dimethylamino Group ◽  
Intramolecular Hydrogen

The crystal structure of osimertinib mesylate Form B has been solved and refined using synchrotron X-ray powder diffraction data and optimized using density functional techniques. Osimertinib mesylate Form B crystallizes in space group P-1 (#2) with a = 11.42912(17), b = 11.72274(24), c = 13.32213(22) Å, α = 69.0265(5), β = 74.5914(4), γ = 66.4007(4)°, V = 1511.557(12) Å3, and Z = 2. The crystal structure is characterized by alternating layers of cation–anion and parallel stacking interactions parallel to the ab-planes. The cation is protonated at the nitrogen atom of the dimethylamino group, which forms a strong hydrogen bond between the cation and the anion. That hydrogen atom also participates in a weaker intramolecular hydrogen bond to an amino nitrogen. There are two additional N–H⋅⋅⋅O hydrogen bonds between the cation and the anion. Several C–H⋅⋅⋅O hydrogen bonds also link the cations and anions. The powder pattern has been submitted to ICDD® for inclusion in the Powder Diffraction File™.

Crystal structure of minocycline hydrochloride dihydrate form A, C23H28N3O7Cl (H2O)2

2018 ◽  
Vol 34 (1) ◽  
pp. 59-65
Author(s):  
Austin M. Wheatley ◽  
James A. Kaduk ◽  
Amy M. Gindhart ◽  
Thomas N. Blanton
Keyword(s):  
Crystal Structure ◽  
Powder Diffraction ◽  
Density Functional ◽  
Hydroxyl Group ◽  
Water Molecules ◽  
Powder Diffraction File ◽  
X Ray ◽  
Dimethyl Amine ◽  
Minocycline Hydrochloride ◽  
Amine Groups

The crystal structure of minocycline hydrochloride dihydrate has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional techniques. Minocycline hydrochloride dihydrate crystallizes in space groupP212121(#19) witha= 7.40772(1),b= 14.44924(3),c= 22.33329(4) Å,V= 2390.465(12) Å3, andZ= 4. The minocycline cation is a zwitterion: both dimethylamino groups are protonated and one hydroxyl group is ionized. A potential ambiguity in the orientation of the amide group was resolved by considering Rietveld refinement residuals and displacement coefficients, as well as DFT energies. The crystal structure is dominated by hydrogen bonds. Both water molecules and a hydroxyl group act as donors to the chloride anion. Both protonated dimethyl amine groups act as donors to the ionized hydroxyl group. Several intramolecular O–H···O hydrogen groups help determine the conformation of the cation. The powder pattern is included in the Powder Diffraction File™ as entry 00-066-1606.

Sign in / Sign up

Export Citation Format

Share Document