Crystal structure determination by combined synchrotron powder X-ray diffraction and crystal structure prediction: 1: 1 L-ephedrine D-tartrate

被引：12

作者：

Wu, Han ^{[1
]}

Habgood, Matthew ^{[2
]}

Parker, Julia E. ^{[3
]}

Reeves-McLaren, Nik ^{[4
]}

Cockcroft, Jeremy K. ^{[2
]}

Vickers, Martin ^{[2
]}

West, Anthony R. ^{[4
]}

Jones, Alan G. ^{[1
]}

机构：

[1] UCL, Dept Chem Engn, London WC1E 7JE, England

[2] UCL, Dept Chem, London WC1H 0AJ, England

[3] Diamond Light Source, Didcot OX11 0DE, Oxon, England

[4] Univ Sheffield, Dept Mat Sci & Engn, Sheffield S1 3JD, S Yorkshire, England

来源：

CRYSTENGCOMM | 2013年 / 15卷 / 10期

基金：

英国工程与自然科学研究理事会;

关键词：

RESOLVING AGENTS; SALT; MINIMIZATION; POLYMORPHISM; CHALLENGES; STABILITY; MOLECULES; EXAMPLE; DESIGN; MODEL;

D O I：

10.1039/c2ce26097b

中图分类号：

O6 [化学];

学科分类号：

0703 ;

摘要：

The crystal structure of the diastereomeric salt 1 : 1 L-ephedrine D-tartrate (1 : 1 LD, C10H16NO+center dot C4H5O6-) was determined from high-resolution synchrotron powder X-ray diffraction (PXRD) data using global optimization in direct space (parallel tempering) together with computational modelling to locate hydrogen positions and refined by the Rietveld method. The structure is monoclinic, space group P2(1), with a = 18.82810(3) angstrom, b = 7.19429(2) angstrom, c = 5.73035(1) angstrom, beta = 95.9613(1)degrees, V = 772.006(3) angstrom(3), and Z = 2. Computational prediction of organic salt structures, especially hydrogen positions, is a valuable complementary technique to PXRD for the final stages of structure determination.

引用

页码：1853 / 1859

页数：7

共 46 条

[1] TABLES OF BOND LENGTHS DETERMINED BY X-RAY AND NEUTRON-DIFFRACTION .1. BOND LENGTHS IN ORGANIC-COMPOUNDS [J].

ALLEN, FH ;

KENNARD, O ;

WATSON, DG ;

BRAMMER, L ;

ORPEN, AG ;

TAYLOR, R .

JOURNAL OF THE CHEMICAL SOCIETY-PERKIN TRANSACTIONS 2, 1987, (12) :S1-S19

[2]

[Anonymous], 1998, RIETICA A VISUAL RIE

[3] Towards crystal structure prediction of complex organic compounds - a report on the fifth blind test [J].

Bardwell, David A. ;

Adjiman, Claire S. ;

Arnautova, Yelena A. ;

Bartashevich, Ekaterina ;

Boerrigter, Stephan X. M. ;

Braun, Doris E. ;

Cruz-Cabeza, Aurora J. ;

Day, Graeme M. ;

Della Valle, Raffaele G. ;

Desiraju, Gautam R. ;

van Eijck, Bouke P. ;

Facelli, Julio C. ;

Ferraro, Marta B. ;

Grillo, Damian ;

Habgood, Matthew ;

Hofmann, Detlef W. M. ;

Hofmann, Fridolin ;

Jose, K. V. Jovan ;

Karamertzanis, Panagiotis G. ;

Kazantsev, Andrei V. ;

Kendrick, John ;

Kuleshova, Liudmila N. ;

Leusen, Frank J. J. ;

Maleev, Andrey V. ;

Misquitta, Alston J. ;

Mohamed, Sharmarke ;

Needs, Richard J. ;

Neumann, Marcus A. ;

Nikylov, Denis ;

Orendt, Anita M. ;

Pal, Rumpa ;

Pantelides, Constantinos C. ;

Pickard, Chris J. ;

Price, Louise S. ;

Price, Sarah L. ;

Scheraga, Harold A. ;

van de Streek, Jacco ;

Thakur, Tejender S. ;

Tiwari, Siddharth ;

Venuti, Elisabetta ;

Zhitkov, Ilia K. .

ACTA CRYSTALLOGRAPHICA SECTION B-STRUCTURAL SCIENCE CRYSTAL ENGINEERING AND MATERIALS, 2011, 67 :535-551

[4] Ritonavir: An extraordinary example of conformational polymorphism [J].

Bauer, J ;

Spanton, S ;

Henry, R ;

Quick, J ;

Dziki, W ;

Porter, W ;

Morris, J .

PHARMACEUTICAL RESEARCH, 2001, 18 (06) :859-866

[5] Structure determinations of three fluorescent organic pigments by powder diffraction and micro-crystal structure analysis [J].

Bruening, Juergen ;

Alig, Edith ;

Meents, Alke ;

van de Streek, Jacco ;

Schmidt, Martin U. .

ZEITSCHRIFT FUR KRISTALLOGRAPHIE, 2009, 224 (11) :556-562

[6] COMPACK:: a program for identifying crystal structure similarity using distances [J].

Chisholm, JA ;

Motherwell, S .

JOURNAL OF APPLIED CRYSTALLOGRAPHY, 2005, 38 :228-231

[7]

Cockcroft JK, 2008, POWDER DIFFRACTION: THEORY AND PRACTICE, P20, DOI 10.1039/9781847558237-00020

[8] THE STRUCTURES OF CRYSTALLINE HYDROGEN BROMIDE [J].

COCKCROFT, JK ;

SIMON, A ;

ZIEBECK, KRA .

ZEITSCHRIFT FUR KRISTALLOGRAPHIE, 1988, 184 (3-4) :229-246

[9]

Coelho A. A., 2006, TOPAS USER MANUAL VE

[10] 17 salts of ephedrine: crystal structures and packing analysis [J].

Collier, Edwin A. ;

Davey, Roger J. ;

Black, Simon N. ;

Roberts, Ron J. .

ACTA CRYSTALLOGRAPHICA SECTION B-STRUCTURAL SCIENCE CRYSTAL ENGINEERING AND MATERIALS, 2006, 62 :498-505

← 1 2 3 4 5 →