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Title: Crystal structure of hydrocortisone acetate, C23H32O6

Abstract

The crystal structure of hydrocortisone acetate has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional techniques. Hydrocortisone acetate crystallizes in space groupP2 1(#4) witha= 8.85173(3) Å,b= 13.53859(3) Å,c= 8.86980(4) Å,β= 101.5438(3)°,V= 1041.455(6) Å 3, andZ= 2. Both hydroxyl groups form hydrogen bonds to the ketone oxygen atom on the steroid ring system, resulting in a three-dimensional hydrogen bond network. The powder pattern has been submitted to ICDD for inclusion in the Powder Diffraction File™.

Authors:
; ;
Publication Date:
Research Org.:
Argonne National Lab. (ANL), Argonne, IL (United States). Advanced Photon Source (APS)
Sponsoring Org.:
INDUSTRY
OSTI Identifier:
1351327
Resource Type:
Journal Article
Resource Relation:
Journal Name: Powder Diffraction; Journal Volume: 32; Journal Issue: 01
Country of Publication:
United States
Language:
ENGLISH

Citation Formats

Kaduk, James A., Gindhart, Amy M., and Blanton, Thomas N.. Crystal structure of hydrocortisone acetate, C23H32O6. United States: N. p., 2017. Web. doi:10.1017/S0885715616000713.
Kaduk, James A., Gindhart, Amy M., & Blanton, Thomas N.. Crystal structure of hydrocortisone acetate, C23H32O6. United States. doi:10.1017/S0885715616000713.
Kaduk, James A., Gindhart, Amy M., and Blanton, Thomas N.. Wed . "Crystal structure of hydrocortisone acetate, C23H32O6". United States. doi:10.1017/S0885715616000713.
@article{osti_1351327,
title = {Crystal structure of hydrocortisone acetate, C23H32O6},
author = {Kaduk, James A. and Gindhart, Amy M. and Blanton, Thomas N.},
abstractNote = {The crystal structure of hydrocortisone acetate has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional techniques. Hydrocortisone acetate crystallizes in space groupP21(#4) witha= 8.85173(3) Å,b= 13.53859(3) Å,c= 8.86980(4) Å,β= 101.5438(3)°,V= 1041.455(6) Å3, andZ= 2. Both hydroxyl groups form hydrogen bonds to the ketone oxygen atom on the steroid ring system, resulting in a three-dimensional hydrogen bond network. The powder pattern has been submitted to ICDD for inclusion in the Powder Diffraction File™.},
doi = {10.1017/S0885715616000713},
journal = {Powder Diffraction},
number = 01,
volume = 32,
place = {United States},
year = {Wed Jan 11 00:00:00 EST 2017},
month = {Wed Jan 11 00:00:00 EST 2017}
}
  • Sodium uranyl acetate, NaUO/sub 2/(O/sub 2/CCH/sub 3/)a, is cubic with space group P2/sub 1/3 and alpha = 10.688 plus or minus 0.002 A. The positions of all atoms were deduced from precisely measured x-ray-diffraction intensities. In the collinear uranyl group U-O = 1.71 plus or minus 0.04 A. Normal to the uranyl axis are six secondary bonds from uranium to acetate oxygens with U-O = 2.49 plus or minus 0.02 A. Sodium is bonded to six acetate oxygens with Na-O = 2.37 plus or minus 0.04 A. The bond lengths within the acetate group are C-C == 1.52 plus ormore » minus 0.05A, C--O=1.26 plus or minus 0.05A,and 1.28 plus or minus 0.04A, and 121 deg is found for the carboxyl bond angle. A revised bond length versus bond strength curve for U/sup VI/-O bonds is presented. (auth)« less
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  • The crystal structure of cobalt(II) acetate tetrahydrate, Co(C{sub 2}H{sub 3}O{sub 2}){center_dot}4H{sub 2}O, has been refined using single-crystal, laboratory powder, and synchrotron powder diffraction data, both individually and in various combinations. The compound crystallizes in the monoclinic space group P2{sub 1}/c, with a=4.80688(3), b=11.92012(7), c=8.45992(5) {Angstrom}, {beta}=94.3416(4){degree} at 27{degree}C, and Z=2. The crystal structure consists of discrete centrosymmetric {ital trans}-Co(C{sub 2}H{sub 3}O{sub 2})(H{sub 2}O){sub 4} complexes, linked by a three-dimensional network of hydrogen bonds. Each complex participates in 14 hydrogen bonds, 12 intermolecular, and 2 intramolecular. Compared to the single-crystal refinement, refinement of laboratory powder data yielded an average difference inmore » bond distances of 0.02 {Angstrom}, in bond angles of 3{degree}, and in root mean square atomic displacements of 0.07 {Angstrom}. The standard uncertainties of the bond distances were 0.01 {Angstrom}, compared to the 0.001{endash}0.002 {Angstrom} in the single-crystal refinement. Refinement of the synchrotron powder data yielded improved accuracy and precision. It proved impossible to locate or refine hydrogen positions using a single-powder dataset, but the hydrogens could be refined using rigid groups in a joint refinement of the two powder datasets. Even from powder refinements, it is possible to obtain suitable accuracy and precision to distinguish C{endash}O and C=O bonds, and to examine details of chemical bonding. {copyright} {ital 1997 International Center for Diffraction Data.}« less