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 we...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. CrysAlisPRO 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.展开更多
The title compound, [Cu2（CH3COO）4（C8H10N2）]n·nCH3CN 1 （C8H10N2, 4,4＇-bipy = 4,4＇-bipyridine）, has been solvothermally synthesized in CH3CN and characterized by X-ray diffraction. The crystal is of monocli...The title compound, [Cu2（CH3COO）4（C8H10N2）]n·nCH3CN 1 （C8H10N2, 4,4＇-bipy = 4,4＇-bipyridine）, has been solvothermally synthesized in CH3CN and characterized by X-ray diffraction. The crystal is of monoclinic, space group Cc with α = 22.626（6）, b = 14.012（4）, c = 15.106（4） ]A, β = 107.610（3）°, V = 4565（2） ]A^3, C20H23Cu2N3O8, Mr = 560.49, Z = 8, Dc = 1.631 g/cm^3,μ = 1.914 mm^-1, Flack parameter = 0.48（1）, F（000） = 2288, R = 0.042 and wR = 0.098 for 8887 observed reflections （I 〉 20（I））. It consists of nearly linear one-dimensional chains [Cu2（CH3COO）4（C8H10N2）]n derived from paddle-wheel [Cu2（CH3COO）4] unit linked by 4,4＇-bipy, and CH3CN as guest molecule regularly decorates between the chains.展开更多
The compound described as [Cu(OH)2(H2O)2(4-C5H4NCOOH)2] in Chin. J. Struct. Chem., 2001, 20: 478-480 is instead the compound [Cu(H2O)4(4-C5H4NCOO)2], whose crystal structure has already been published elsewhere.
The two component molecules of the co-crystal 0.69（C18H2ON206）.0.31（C18H18N2O6） lie on a center-of-inversion that exists midway along the ethylene chain connecting the two aromatic rings. The two molecules are sup...The two component molecules of the co-crystal 0.69（C18H2ON206）.0.31（C18H18N2O6） lie on a center-of-inversion that exists midway along the ethylene chain connecting the two aromatic rings. The two molecules are superimposed. The crystal is also a non-morohedral twin with a minor 37.7（2）% component. The refinement of this twinned and disordered crystal structure is detailed. Crystal data： C18H19.38N2O6, monoclinic, P21/c, a = 17.1687（8）, b = 5.4389（2）, c = 9.3261（4） A, b = 95.270（5）° and V= 867.18（6） A3 at -173 ℃.展开更多
The space group of [(H2O)(C3H4N2)(O2CCH=CHCO2Zn)]n, which was originally described in the acentric Pc space group (Liu et al., Chin. J. Struct. Chem. 2004, 23, 160～163), is re-described in the centric P21/c space g...The space group of [(H2O)(C3H4N2)(O2CCH=CHCO2Zn)]n, which was originally described in the acentric Pc space group (Liu et al., Chin. J. Struct. Chem. 2004, 23, 160～163), is re-described in the centric P21/c space group.展开更多
The two independent cations of the salt, [HO-C6H4-CH=NH-C6H4-OH]·1/2OH·1/2Cl, are both disordered about an axis connecting the two oxygen atoms at the para-positions of the aromatic rings, the disorder being...The two independent cations of the salt, [HO-C6H4-CH=NH-C6H4-OH]·1/2OH·1/2Cl, are both disordered about an axis connecting the two oxygen atoms at the para-positions of the aromatic rings, the disorder being in a 83：17 ratio in one cation and 91：9 in the other. The hydroxide and chloride anions are ordered. The treatment of the nearly ‘whole-molecule disorder’ by employing a small number of restraints is described. Crystal data： C13H12.5Cl0.5NO2.5, triclinic, P , a = 9.1731（4）, b = 9.2048（4）, c = 15.9144（7） , α = 104.822（1）, β = 90.077（1）, γ = 118.641（1）o and V = 1127.86（9） 3 at –173 K.展开更多
The molecule of 4-tricyanovinyl-N,N-diethylaniline is disordered about an axis that is close to the axis passing through the 1,4-carbon atoms. The disorder is a 1：1 type of disorder that involves only part of the mol...The molecule of 4-tricyanovinyl-N,N-diethylaniline is disordered about an axis that is close to the axis passing through the 1,4-carbon atoms. The disorder is a 1：1 type of disorder that involves only part of the molecule as the diethylamino substitutent and the three nitrogen atoms of the tricyanovinyl substituent are ordered. The treatment of the nearly ‘whole-molecule disorder’ by employing a small number of restraints is described. Crystal data： C15H14N4, triclinic, P , a = 7.1996（5）, b = 7.7232（5）, c = 12.4171（8） , α = 99.350（1）, β = 94.647（1）, γ = 103.312（1）o and V = 657.90（8） 3 at –173 K.展开更多
This note explains the relationship (as well as the absence of a relationship) between chiral space groups and chiral molecules (which have absolute configurations). For a chiral molecule, which must crystallize in a ...This note explains the relationship (as well as the absence of a relationship) between chiral space groups and chiral molecules (which have absolute configurations). For a chiral molecule, which must crystallize in a chiral space group, the outcome of the absolute configuration determination must be linked to some other properties of the chiral crystal such as its optical activity for the observation to the relevant.展开更多
文摘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. CrysAlisPRO 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.
基金The work was supported by the Zhejiang Key Laboratory for Reactive Chemistry on Solid Surfaces (No. 0506) and the University of Malaya (F0712/2005c)
文摘The title compound, [Cu2（CH3COO）4（C8H10N2）]n·nCH3CN 1 （C8H10N2, 4,4＇-bipy = 4,4＇-bipyridine）, has been solvothermally synthesized in CH3CN and characterized by X-ray diffraction. The crystal is of monoclinic, space group Cc with α = 22.626（6）, b = 14.012（4）, c = 15.106（4） ]A, β = 107.610（3）°, V = 4565（2） ]A^3, C20H23Cu2N3O8, Mr = 560.49, Z = 8, Dc = 1.631 g/cm^3,μ = 1.914 mm^-1, Flack parameter = 0.48（1）, F（000） = 2288, R = 0.042 and wR = 0.098 for 8887 observed reflections （I 〉 20（I））. It consists of nearly linear one-dimensional chains [Cu2（CH3COO）4（C8H10N2）]n derived from paddle-wheel [Cu2（CH3COO）4] unit linked by 4,4＇-bipy, and CH3CN as guest molecule regularly decorates between the chains.
文摘The compound described as [Cu(OH)2(H2O)2(4-C5H4NCOOH)2] in Chin. J. Struct. Chem., 2001, 20: 478-480 is instead the compound [Cu(H2O)4(4-C5H4NCOO)2], whose crystal structure has already been published elsewhere.
基金the University of Malaya (grant No. UM.C/HIR/MOHE/SC/12) for supporting this study
文摘The two component molecules of the co-crystal 0.69（C18H2ON206）.0.31（C18H18N2O6） lie on a center-of-inversion that exists midway along the ethylene chain connecting the two aromatic rings. The two molecules are superimposed. The crystal is also a non-morohedral twin with a minor 37.7（2）% component. The refinement of this twinned and disordered crystal structure is detailed. Crystal data： C18H19.38N2O6, monoclinic, P21/c, a = 17.1687（8）, b = 5.4389（2）, c = 9.3261（4） A, b = 95.270（5）° and V= 867.18（6） A3 at -173 ℃.
文摘The space group of [(H2O)(C3H4N2)(O2CCH=CHCO2Zn)]n, which was originally described in the acentric Pc space group (Liu et al., Chin. J. Struct. Chem. 2004, 23, 160～163), is re-described in the centric P21/c space group.
文摘The two independent cations of the salt, [HO-C6H4-CH=NH-C6H4-OH]·1/2OH·1/2Cl, are both disordered about an axis connecting the two oxygen atoms at the para-positions of the aromatic rings, the disorder being in a 83：17 ratio in one cation and 91：9 in the other. The hydroxide and chloride anions are ordered. The treatment of the nearly ‘whole-molecule disorder’ by employing a small number of restraints is described. Crystal data： C13H12.5Cl0.5NO2.5, triclinic, P , a = 9.1731（4）, b = 9.2048（4）, c = 15.9144（7） , α = 104.822（1）, β = 90.077（1）, γ = 118.641（1）o and V = 1127.86（9） 3 at –173 K.
文摘The molecule of 4-tricyanovinyl-N,N-diethylaniline is disordered about an axis that is close to the axis passing through the 1,4-carbon atoms. The disorder is a 1：1 type of disorder that involves only part of the molecule as the diethylamino substitutent and the three nitrogen atoms of the tricyanovinyl substituent are ordered. The treatment of the nearly ‘whole-molecule disorder’ by employing a small number of restraints is described. Crystal data： C15H14N4, triclinic, P , a = 7.1996（5）, b = 7.7232（5）, c = 12.4171（8） , α = 99.350（1）, β = 94.647（1）, γ = 103.312（1）o and V = 657.90（8） 3 at –173 K.
文摘This note explains the relationship (as well as the absence of a relationship) between chiral space groups and chiral molecules (which have absolute configurations). For a chiral molecule, which must crystallize in a chiral space group, the outcome of the absolute configuration determination must be linked to some other properties of the chiral crystal such as its optical activity for the observation to the relevant.
