Indexing Non-merohedrally Twinned Crystals by Bruker’s APEX2 and Agilent’s CrysAlisPRO.an Example of a Crystal Structure That Can Be Refined through Either the PLATON Route or the 'Kklf 5' Route,and, Simultaneous Data Collection of Two Crystals in a Two-in-one Run

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摘要 The first part of this report describes the data reduction of non-merohedrally twinned crystals measured on Bruker and Agilent area-detector diffractometers. The image frames of methyl-2-aminopyrazine-3-carboxylate were processed with APEX2 to furnish a set of overlapping diffraction indices that were used for solution and refinement. CrysAlis^PRO was used for processing the frames of bis(diethyldicarbamato)nickel, which exists in monoclinic and tetragonal polymorphs, and in untwinned and twinned forms. In the second part, the crystal structure of [(3-formyl-4- hydroxyphenyl)methyl]triphenylphosphanium chloride was refined through the ‘HKLF 5’ (based on a combined set of diffraction indices) and PLATON (based on one set of diffraction indices) routes to give identical outcomes because the amount of overlap of the twin domains is small. For the third part, in a proof-of-concept investigation, the diffraction pattern of untwinned and twinned 4-{(E)-(4-aminophenyl)diazenyl]phenylamine was recorded simultaneously in one run; the three domains could be indexed and the crystal structure satisfactorily refined. The refinement was identical to those derived from independent measurements; the crystal structure features two independent centrosymmetric molecules, one of which is ordered and the other whole-molecule-disordered. This two-in-one run opens up the possibility that two or more crystals having different atomic compositions can be measured simultaneously if their reciprocal lattices do not overlap significantly.

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	NG Seik Weng

关键词 ： merohedral, non-merohedral twin, APEX2, CrysAlisPRO, two-in-one data collection

Abstract：The first part of this report describes the data reduction of non-merohedrally twinned crystals measured on Bruker and Agilent area-detector diffractometers. The image frames of methyl-2-aminopyrazine-3-carboxylate were processed with APEX2 to furnish a set of overlapping diffraction indices that were used for solution and refinement. CrysAlis^PRO was used for processing the frames of bis(diethyldicarbamato)nickel, which exists in monoclinic and tetragonal polymorphs, and in untwinned and twinned forms. In the second part, the crystal structure of [(3-formyl-4- hydroxyphenyl)methyl]triphenylphosphanium chloride was refined through the ‘HKLF 5’ (based on a combined set of diffraction indices) and PLATON (based on one set of diffraction indices) routes to give identical outcomes because the amount of overlap of the twin domains is small. For the third part, in a proof-of-concept investigation, the diffraction pattern of untwinned and twinned 4-{(E)-(4-aminophenyl)diazenyl]phenylamine was recorded simultaneously in one run; the three domains could be indexed and the crystal structure satisfactorily refined. The refinement was identical to those derived from independent measurements; the crystal structure features two independent centrosymmetric molecules, one of which is ordered and the other whole-molecule-disordered. This two-in-one run opens up the possibility that two or more crystals having different atomic compositions can be measured simultaneously if their reciprocal lattices do not overlap significantly.

Key words： merohedral non-merohedral twin APEX2 CrysAlisPRO two-in-one data collection

收稿日期: 2013-07-11 出版日期: 2013-09-17

通讯作者: NG Seik Weng:seikweng@um.edu.my E-mail: seikweng@um.edu.my

作者简介: NG Seik Weng:seikweng@um.edu.my

引用本文:

NG Seik Weng. Indexing Non-merohedrally Twinned Crystals by Bruker’s APEX2 and Agilent’s CrysAlis^PRO.an Example of a Crystal Structure That Can Be Refined through Either the PLATON Route or the 'Kklf 5' Route,and, Simultaneous Data Collection of Two Crystals in a Two-in-one Run[J]. 结构化学, 2014, 33(2): 294-303.
NG Seik Weng. Indexing Non-merohedrally Twinned Crystals by Bruker’s APEX2 and Agilent’s CrysAlis^PRO.an Example of a Crystal Structure That Can Be Refined through Either the PLATON Route or the 'Kklf 5' Route,and, Simultaneous Data Collection of Two Crystals in a Two-in-one Run. CHINESE JOURNAL OF STRUCTURAL CHEMISTRY, 2014, 33(2): 294-303.

链接本文:

http://manu30.magtech.com.cn/jghx/CN/ 或 http://manu30.magtech.com.cn/jghx/CN/Y2014/V33/I2/294

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