Pub Date : 2013-02-01DOI: 10.1107/S2052519212050439
F. Dumitru, Y. Legrand, M. Barboiu, Arie Lee
The synthesis and characterization of a series of halogen-substituted pseudoterpyridine ZnII homoleptic mononuclear complexes, based on ligands L11–L44 [2,6-pyridinedicarboxaldehydebis(p-R-phenylimines), R = F, Cl, Br, I] are reported. Neither of the structures contain relatively strong classical hydrogen bonds (OH⋯O, NH⋯O, OH⋯N, NH⋯N) and the structure packing is thus determined by a subtle interplay of weaker interactions. Isostructurality of the four halogen analogues is very rare, and in this study —Br, —Cl and —F are found to be isostructural in different degrees, whereas —I is not. Interestingly, although it is closely isostructural to the —Cl and —Br compounds, the F analogue is shown not to form F⋯O bonds, while the Cl and the Br analogues do form Hal⋯O bonds. This raises an important question on the role of Hal⋯O bonds in the structuration of the crystal packing, particularly the stabilization effect. Similarly, while the CH⋯Hal interaction seems to give one-dimensional cohesion in the —Cl and —Br analogues, this feature is absent in the —F analogue, despite its close isostructurality. CH⋯O interactions appear to dominate to a first degree the cohesion between the anionic trifluoromethanesulfonate network and the cationic Zn-pyridinedicarboxaldehydebis(p-R-phenylimines) network. The analysis of these interactions is corroborated by reduced density gradient calculations based on promolecular densities.
{"title":"Weak intermolecular hydrogen and halogen interactions in an isomorphous halogen series of pseudoterpyridine ZnII complexes","authors":"F. Dumitru, Y. Legrand, M. Barboiu, Arie Lee","doi":"10.1107/S2052519212050439","DOIUrl":"https://doi.org/10.1107/S2052519212050439","url":null,"abstract":"The synthesis and characterization of a series of halogen-substituted pseudoterpyridine ZnII homoleptic mononuclear complexes, based on ligands L11–L44 [2,6-pyridinedicarboxaldehydebis(p-R-phenylimines), R = F, Cl, Br, I] are reported. Neither of the structures contain relatively strong classical hydrogen bonds (OH⋯O, NH⋯O, OH⋯N, NH⋯N) and the structure packing is thus determined by a subtle interplay of weaker interactions. Isostructurality of the four halogen analogues is very rare, and in this study —Br, —Cl and —F are found to be isostructural in different degrees, whereas —I is not. Interestingly, although it is closely isostructural to the —Cl and —Br compounds, the F analogue is shown not to form F⋯O bonds, while the Cl and the Br analogues do form Hal⋯O bonds. This raises an important question on the role of Hal⋯O bonds in the structuration of the crystal packing, particularly the stabilization effect. Similarly, while the CH⋯Hal interaction seems to give one-dimensional cohesion in the —Cl and —Br analogues, this feature is absent in the —F analogue, despite its close isostructurality. CH⋯O interactions appear to dominate to a first degree the cohesion between the anionic trifluoromethanesulfonate network and the cationic Zn-pyridinedicarboxaldehydebis(p-R-phenylimines) network. The analysis of these interactions is corroborated by reduced density gradient calculations based on promolecular densities.","PeriodicalId":6887,"journal":{"name":"Acta Crystallographica Section B Structural Crystallography and Crystal Chemistry","volume":"45 1","pages":"43-54"},"PeriodicalIF":0.0,"publicationDate":"2013-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"75582368","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2010-09-20DOI: 10.1111/J.1600-5740.1974.TB00014.X
S. D̂uroviĉ
The term ‘OD packet’ is defined as the smallest continuous part of an OD structure consisting of M > 1 kinds of layers which is periodical in two dimensions and which completely represents its composition. The properties of OD packets in the four categories are discussed and their application to kaolinite-type and MoS2 polytypes is shown.
{"title":"Notion of ‘Packets' in the Theory of OD Structures of M > 1 Kinds of Layers. Examples: Kaolinites and MoS2","authors":"S. D̂uroviĉ","doi":"10.1111/J.1600-5740.1974.TB00014.X","DOIUrl":"https://doi.org/10.1111/J.1600-5740.1974.TB00014.X","url":null,"abstract":"The term ‘OD packet’ is defined as the smallest continuous part of an OD structure consisting of M > 1 kinds of layers which is periodical in two dimensions and which completely represents its composition. The properties of OD packets in the four categories are discussed and their application to kaolinite-type and MoS2 polytypes is shown.","PeriodicalId":6887,"journal":{"name":"Acta Crystallographica Section B Structural Crystallography and Crystal Chemistry","volume":"30 1","pages":"76-78"},"PeriodicalIF":0.0,"publicationDate":"2010-09-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"74107698","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2006-04-01DOI: 10.1107/S0108768106006604
C. Lehmann
{"title":"Crystalline Molecular Complexes and Compounds. Vol. 1 and 2. By F. H. Herbstein. Pp. xxviii + 1273. Oxford: Oxford University Press, 2005. Price (hardback) GBP 125.00. ISBN 0-19-852660-1.","authors":"C. Lehmann","doi":"10.1107/S0108768106006604","DOIUrl":"https://doi.org/10.1107/S0108768106006604","url":null,"abstract":"","PeriodicalId":6887,"journal":{"name":"Acta Crystallographica Section B Structural Crystallography and Crystal Chemistry","volume":"8 6","pages":"338-339"},"PeriodicalIF":0.0,"publicationDate":"2006-04-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"72568881","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 1997-06-01DOI: 10.1107/S0108768196012529
C. Weidenthaler, R. Fischer, L. Abrams, A. Hewat
Samples of two differently prepared zeolite rho loaded with different amounts of dimethylamine (DMA) were studied in their hydrated forms by X-ray diffraction. Both zeolites are partially dealuminated, as indicated by nonframework A1 which is assumed to be Al2O3 or AlOOH. Series I was prepared from dry-calcined NHn-rho at 873 K, series II from steam-calcined NHn-rho at 773 K. The samples were loaded with different amounts of DMA. Rietveld refinements yielded the following results for series I: (1) H3.8(H-DMA)5Cs0.2Al9Si39O96.Al2O3.21H2O, X-ray data collection at room temperature, Imoverline 3m, a = 15.0590 (2) A, Rwp = 0.089; (2) (H-DMA)8.8Cs0.2Al9Si39O96.Al2O3.18H2O, X-ray data collection at room temperature, Imoverline 3m, a = 15.0680 (2) A, Rwp = 0.091. Series II: (3) H0.3(H-DMA)5Cs0.7Al6Si42O96.2.5Al2O3.24H2O, X-ray data collection at room temperature, Imoverline 3m, a = 15.0596 (2) A, Rwp = 0.120. DMA resides on the center axis through the alpha-cage with the N atoms pointing to the single eight-ring and the two methyl groups oriented towards the center of the alpha-cage.
用x射线衍射法对两种不同制备的沸石样品进行了水合形式的研究。两种沸石都部分脱铝，如非骨架A1所示，假定为Al2O3或AlOOH。系列1由873 K下干烧NHn-rho制得，系列2由773 K下蒸汽烧NHn-rho制得。这些样品被装载了不同数量的DMA。系列1的Rietveld细化得到如下结果:(1)H3.8(H-DMA)5Cs0.2Al9Si39O96.Al2O3.21H2O，室温下x射线数据采集，Im overline 3m, a = 15.0590 (2) a, Rwp = 0.089;(2) (H-DMA)8.8Cs0.2Al9Si39O96.Al2O3.18H2O，室温下x射线数据采集，Im overline 3m, a = 15.0680 (2) a, Rwp = 0.091。系列II:(3) H0.3(H-DMA)5Cs0.7Al6Si42O96.2.5Al2O3.24H2O, x射线数据在室温下采集，Im overline 3m, a = 15.0596 (2) a, Rwp = 0.120。DMA通过alpha -笼位于中心轴上，N原子指向单个八环，两个甲基指向alpha -笼的中心。
{"title":"Zeolite Rho Loaded with Methylamines. III. Trimethylamine Loadings","authors":"C. Weidenthaler, R. Fischer, L. Abrams, A. Hewat","doi":"10.1107/S0108768196012529","DOIUrl":"https://doi.org/10.1107/S0108768196012529","url":null,"abstract":"Samples of two differently prepared zeolite rho loaded with different amounts of dimethylamine (DMA) were studied in their hydrated forms by X-ray diffraction. Both zeolites are partially dealuminated, as indicated by nonframework A1 which is assumed to be Al2O3 or AlOOH. Series I was prepared from dry-calcined NHn-rho at 873 K, series II from steam-calcined NHn-rho at 773 K. The samples were loaded with different amounts of DMA. Rietveld refinements yielded the following results for series I: (1) H3.8(H-DMA)5Cs0.2Al9Si39O96.Al2O3.21H2O, X-ray data collection at room temperature, Imoverline 3m, a = 15.0590 (2) A, Rwp = 0.089; (2) (H-DMA)8.8Cs0.2Al9Si39O96.Al2O3.18H2O, X-ray data collection at room temperature, Imoverline 3m, a = 15.0680 (2) A, Rwp = 0.091. Series II: (3) H0.3(H-DMA)5Cs0.7Al6Si42O96.2.5Al2O3.24H2O, X-ray data collection at room temperature, Imoverline 3m, a = 15.0596 (2) A, Rwp = 0.120. DMA resides on the center axis through the alpha-cage with the N atoms pointing to the single eight-ring and the two methyl groups oriented towards the center of the alpha-cage.","PeriodicalId":6887,"journal":{"name":"Acta Crystallographica Section B Structural Crystallography and Crystal Chemistry","volume":"30 1","pages":"429-439"},"PeriodicalIF":0.0,"publicationDate":"1997-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"75900087","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 1997-04-01DOI: 10.1107/S0108768197099680
P. Maitlis
{"title":"Metallomesogens - synthesis, properties and applications edited by J. L. Serrano","authors":"P. Maitlis","doi":"10.1107/S0108768197099680","DOIUrl":"https://doi.org/10.1107/S0108768197099680","url":null,"abstract":"","PeriodicalId":6887,"journal":{"name":"Acta Crystallographica Section B Structural Crystallography and Crystal Chemistry","volume":"67 1","pages":"323-324"},"PeriodicalIF":0.0,"publicationDate":"1997-04-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"83861680","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 1995-06-01DOI: 10.1107/S0108768194011407
S. T. Howard, M. Hursthouse, C. Lehmann, E. A. Poyner
(2S)-3-(3',4'-Dihydroxyphenyl)alanine (L-dopa), C 9 H 11 NO 4 , M r =197.19, monoclinic, P2 1 , a=13.619(6), b = 5.232(2), c = 6.062 (3) A, β = 97.56 (4)°, V = 428.191A 3 , Z = 2, D x = 1.529 g cm -3 , D m = 1.515 g cm -3 (T = 293 K), λ(MoKα) = 0.71069 A, μ = 1.2 cm- 1 , F(000) = 208, T=173K, R(F) = 0.017 for 4208 reflections with sin θ/λ < 1.078 A- 1 . The electron distribution has been determined by multipole refinement with the Hansen/Coppens aspherical scattering factor expansion, including multipole terms up to octopoles for C, N and O and up to dipoles for H. The molecular dipole moment was determined as 12(2)D, within an e.s.d. of the ab initio value reported here of 11 D. The bond critical-point properties of the total electron density were determined, giving negative values for ⊇ 2 ρ c consistent with covalent bonds, and are in fair agreement with the ab initio results. An analysis of the hydrogen-bond critical points gave small positive ⊇ 2 ρ values, consistent with ionic, closed-shell interactions between the participating atoms. A set of theoretical structure factors was generated from the ab initio charge distribution and subjected to multipole refinement, to enable a more detailed comparison with experiment.
(2) 3 -(3’,4’-Dihydroxyphenyl)丙氨酸(左旋多巴),C 9 H 11 4号,M r = 197.19,单斜,P2 1 = 13.619 (6), b = 5.232 (2), C = 6.062(3),β= 97.56(4)°,428.191 V = 3, Z = 2, 3 D x = 1.529 g厘米,g D M = 1.515厘米3 (T = 293 K),λ(MoKα)= 0.71069,- 1μ= 1.2厘米,F (000) = 208 T = 173 K, r (F) = 0.017 4208反射sinθ/λ< 1.078 - 1。用Hansen/Coppens非球面散射因子展开法确定了电子分布，包括C、N和O的多极项和h的偶极项，确定了分子偶极矩为12(2)D，在本文报道的从头计算值11 D的e.s.d范围内。确定了总电子密度的键临界点性质，得到与共价键一致的负值。并且与从头算的结果基本一致。对氢键临界点的分析给出了小的正ρ值，与参与原子之间的离子、闭壳相互作用一致。通过从头计算得到了一组理论结构因子，并对其进行了多极精化，以便与实验结果进行更详细的比较。
{"title":"Experimental and theoretical determination of electronic properties in l-dopa","authors":"S. T. Howard, M. Hursthouse, C. Lehmann, E. A. Poyner","doi":"10.1107/S0108768194011407","DOIUrl":"https://doi.org/10.1107/S0108768194011407","url":null,"abstract":"(2S)-3-(3',4'-Dihydroxyphenyl)alanine (L-dopa), C 9 H 11 NO 4 , M r =197.19, monoclinic, P2 1 , a=13.619(6), b = 5.232(2), c = 6.062 (3) A, β = 97.56 (4)°, V = 428.191A 3 , Z = 2, D x = 1.529 g cm -3 , D m = 1.515 g cm -3 (T = 293 K), λ(MoKα) = 0.71069 A, μ = 1.2 cm- 1 , F(000) = 208, T=173K, R(F) = 0.017 for 4208 reflections with sin θ/λ < 1.078 A- 1 . The electron distribution has been determined by multipole refinement with the Hansen/Coppens aspherical scattering factor expansion, including multipole terms up to octopoles for C, N and O and up to dipoles for H. The molecular dipole moment was determined as 12(2)D, within an e.s.d. of the ab initio value reported here of 11 D. The bond critical-point properties of the total electron density were determined, giving negative values for ⊇ 2 ρ c consistent with covalent bonds, and are in fair agreement with the ab initio results. An analysis of the hydrogen-bond critical points gave small positive ⊇ 2 ρ values, consistent with ionic, closed-shell interactions between the participating atoms. A set of theoretical structure factors was generated from the ab initio charge distribution and subjected to multipole refinement, to enable a more detailed comparison with experiment.","PeriodicalId":6887,"journal":{"name":"Acta Crystallographica Section B Structural Crystallography and Crystal Chemistry","volume":"126 1","pages":"328-337"},"PeriodicalIF":0.0,"publicationDate":"1995-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"77810444","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 1994-06-01DOI: 10.1107/S0108768193013989
U. Burkhardt, Y. Grin, M. Ellner, K. Peters
Diiron pentaaluminide, Fe 2 Al 5 , M r =268.8, orthorhombic, Cmcm (No. 63), a=7.6559(8), b=6.4154(6), c=4.2184 (4) A, V=207. 19 (6) A 3 , Z=2, D x =4.23 (2), D m =4.20 (1) Mg m -3 , Mo Kα radiation, μ=8.2 mm -1 , F(000)=249.6, T=293 K, R=0.0229, wR=0.0270 for 137 unique reflections. The refined structure differs from the approximate structure proposed previously by an additional partially occupied atomic position
五铝二铁，fe2al5, M r =268.8，正交，Cmcm (No. 63)， a=7.6559(8)， b=6.4154(6)， c=4.2184 (4)， a, V=207。19 (6) A 3, Z=2, D x =4.23 (2)， D m =4.20 (1)， Mg m -3, Mo Kα辐射μ=8.2 mm -1, F(000)=249.6, T=293 K, R=0.0229, wR=0.0270。这种精炼的结构与先前提出的近似结构不同，因为它增加了一个部分占据的原子位置
{"title":"Structure refinement of the iron–aluminium phase with the approximate composition Fe2Al5","authors":"U. Burkhardt, Y. Grin, M. Ellner, K. Peters","doi":"10.1107/S0108768193013989","DOIUrl":"https://doi.org/10.1107/S0108768193013989","url":null,"abstract":"Diiron pentaaluminide, Fe 2 Al 5 , M r =268.8, orthorhombic, Cmcm (No. 63), a=7.6559(8), b=6.4154(6), c=4.2184 (4) A, V=207. 19 (6) A 3 , Z=2, D x =4.23 (2), D m =4.20 (1) Mg m -3 , Mo Kα radiation, μ=8.2 mm -1 , F(000)=249.6, T=293 K, R=0.0229, wR=0.0270 for 137 unique reflections. The refined structure differs from the approximate structure proposed previously by an additional partially occupied atomic position","PeriodicalId":6887,"journal":{"name":"Acta Crystallographica Section B Structural Crystallography and Crystal Chemistry","volume":"59 1","pages":"313-316"},"PeriodicalIF":0.0,"publicationDate":"1994-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"81171124","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 1994-06-01DOI: 10.1107/S0108768193011656
A. Lehmann, P. Luger, C. Lehmann, R. Ibberson
Deuterated oxalic acid dihydrate, C 2 D 4 .2D 2 O, M r =132.10, monoclinic, P2 1 /n, Z=2. At 100 K, a=6.13338 (6), b=3.50018 (1), c=11.98334 (3) A, β= 106.0599 (2) o , V=247.218 A 3 , D x =1.694 g cm -3 , χ 2 =1.93. At 15 K, a=6.13661 (4), b=3.47501 (1), c=11.97044 (2) A, β=105.9778 (1) o , V=245.406 A 3 , D x =1.706 g cm -3 , χ 2 =2.59. High-resolution neutron powder diffraction data have been recorded at temperatures of 15 and 100 K on fully deuterated oxalic acid dihydrate, which has been widely used as a crystallographic standard, in order to assess in particular the potential use of neutron powder diffraction data for charge-density studies
二水合氘化草酸，c2d4 . 2d2o, M r =132.10，单斜，P2 1 /n, Z=2。在100 K时，a=6.13338 (6)， b=3.50018 (1)， c=11.98334 (3) a， β= 106.0599 (2) o, V=247.218 a 3, x =1.694 g cm -3， χ 2 =1.93。15 K时，a=6.13661 (4)， b=3.47501 (1)， c=11.97044 (2) a， β=105.9778 (1) o, V=245.406 a 3, x =1.706 g cm -3， χ 2 =2.59。在15和100 K的温度下，用完全氘化的二水合草酸记录了高分辨率的中子粉末衍射数据，该数据已被广泛用作晶体学标准，以评估中子粉末衍射数据在电荷密度研究中的潜在用途
{"title":"Oxalic acid dihydrate - an accurate low-temperature structural study using high-resolution neutron powder diffraction","authors":"A. Lehmann, P. Luger, C. Lehmann, R. Ibberson","doi":"10.1107/S0108768193011656","DOIUrl":"https://doi.org/10.1107/S0108768193011656","url":null,"abstract":"Deuterated oxalic acid dihydrate, C 2 D 4 .2D 2 O, M r =132.10, monoclinic, P2 1 /n, Z=2. At 100 K, a=6.13338 (6), b=3.50018 (1), c=11.98334 (3) A, β= 106.0599 (2) o , V=247.218 A 3 , D x =1.694 g cm -3 , χ 2 =1.93. At 15 K, a=6.13661 (4), b=3.47501 (1), c=11.97044 (2) A, β=105.9778 (1) o , V=245.406 A 3 , D x =1.706 g cm -3 , χ 2 =2.59. High-resolution neutron powder diffraction data have been recorded at temperatures of 15 and 100 K on fully deuterated oxalic acid dihydrate, which has been widely used as a crystallographic standard, in order to assess in particular the potential use of neutron powder diffraction data for charge-density studies","PeriodicalId":6887,"journal":{"name":"Acta Crystallographica Section B Structural Crystallography and Crystal Chemistry","volume":"2 1","pages":"344-348"},"PeriodicalIF":0.0,"publicationDate":"1994-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"90214697","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Structure of Monoclinic Papain at 1.60 Angstroms Resolution","authors":"R. Pickersgill, G. Harris, E. Garman","doi":"10.2210/PDB1PPN/PDB","DOIUrl":"https://doi.org/10.2210/PDB1PPN/PDB","url":null,"abstract":"","PeriodicalId":6887,"journal":{"name":"Acta Crystallographica Section B Structural Crystallography and Crystal Chemistry","volume":"20 10","pages":"59-67"},"PeriodicalIF":0.0,"publicationDate":"1994-01-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"91418572","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 1990-12-01DOI: 10.1107/S010876819000622X
Å. Oskarsson, B. Norén, C. Svensson, L. I. Elding
Crystals of trans-diiodobis(tetrahydrothiophene)-palladium(II) and trans-diiodobis(tetrahydrothiophene)platinum(II) were prepared by dissolving the appropriate metal iodide in tetrahydrothiophene at 353 K and cooling to room temperature. Crystal data at room temperature (Mo K-alpha, lambda = 0.7107-angstrom) are: [PdI2(C4H8S)2], M(r) = 536.54, triclinic, P1BAR, a = 8.4920 (8), b = 8.8248 (1), c = 9.4580 (11) angstrom, alpha = 97.595 (9), beta = 91.963 (9), gamma = 99.482 (9)-degrees, V = 691.8 (1) angstrom-3, Z = 2, D(x) = 2.576 Mg m-3, mu = 5.997 mm-1, F(000) = 496, R = 0.028 for 2090 unique reflections with I > 3-sigma-(I); [PtI2(C4H8S)2], M(r) = 625.24, triclinic, P1BAR, a = 7.889 (2), b = 8.676 (1), c = 10.616 (2) angstrom, alpha = 103.75 (1), beta = 90.36 (1), gamma = 94.70 (2)-degrees, V = 703.2 (2) angstrom-3, Z = 2, D(x) = 2.953 Mg m-3, mu = 14.67 mm-1, F(000) = 560, R = 0.024 for 3988 reflections with I > 3-sigma-(I). Both compounds consist of van-der-Waals-packed mononuclear trans-[MI2(C4H8S)2] complexes. There are two centrosymmetric metal complexes in the asymmetric unit of the Pt compound but only one pseudoplanar complex in the Pd compound. The acceptor-donor distances are Pd-I 2.603 (1), 2.625 (1); Pd-S 2.316 (2), 2.329 (2); Pt-I 2.606 (1), 2.616 (1); and Pt-S 2.309 (1), 2.310 (1) angstrom. A literature survey of compounds in which ligand-I or -S (in thioethers) atoms are trans to themselves shows average M-I and M-S distances of Pd-I 2.605 (20), Pd-S 2.324 (15), Pt-I 2.609 (9) and Pt-S 2.313 (13) angstrom. The spread of the M-I and M-S distances is significantly increased if complexes are included where I or S are not trans to themselves, indicating that for some donor atoms the trans influence dominates over other factors such as the cis influence and packing forces. (Less)
{"title":"trans influence on bond distances. Structures of trans-diiodobis(tetrahydrothiophene)palladium(II) and trans-diiodobis(tetrahydrothiophene)platinum(II)","authors":"Å. Oskarsson, B. Norén, C. Svensson, L. I. Elding","doi":"10.1107/S010876819000622X","DOIUrl":"https://doi.org/10.1107/S010876819000622X","url":null,"abstract":"Crystals of trans-diiodobis(tetrahydrothiophene)-palladium(II) and trans-diiodobis(tetrahydrothiophene)platinum(II) were prepared by dissolving the appropriate metal iodide in tetrahydrothiophene at 353 K and cooling to room temperature. Crystal data at room temperature (Mo K-alpha, lambda = 0.7107-angstrom) are: [PdI2(C4H8S)2], M(r) = 536.54, triclinic, P1BAR, a = 8.4920 (8), b = 8.8248 (1), c = 9.4580 (11) angstrom, alpha = 97.595 (9), beta = 91.963 (9), gamma = 99.482 (9)-degrees, V = 691.8 (1) angstrom-3, Z = 2, D(x) = 2.576 Mg m-3, mu = 5.997 mm-1, F(000) = 496, R = 0.028 for 2090 unique reflections with I > 3-sigma-(I); [PtI2(C4H8S)2], M(r) = 625.24, triclinic, P1BAR, a = 7.889 (2), b = 8.676 (1), c = 10.616 (2) angstrom, alpha = 103.75 (1), beta = 90.36 (1), gamma = 94.70 (2)-degrees, V = 703.2 (2) angstrom-3, Z = 2, D(x) = 2.953 Mg m-3, mu = 14.67 mm-1, F(000) = 560, R = 0.024 for 3988 reflections with I > 3-sigma-(I). Both compounds consist of van-der-Waals-packed mononuclear trans-[MI2(C4H8S)2] complexes. There are two centrosymmetric metal complexes in the asymmetric unit of the Pt compound but only one pseudoplanar complex in the Pd compound. The acceptor-donor distances are Pd-I 2.603 (1), 2.625 (1); Pd-S 2.316 (2), 2.329 (2); Pt-I 2.606 (1), 2.616 (1); and Pt-S 2.309 (1), 2.310 (1) angstrom. A literature survey of compounds in which ligand-I or -S (in thioethers) atoms are trans to themselves shows average M-I and M-S distances of Pd-I 2.605 (20), Pd-S 2.324 (15), Pt-I 2.609 (9) and Pt-S 2.313 (13) angstrom. The spread of the M-I and M-S distances is significantly increased if complexes are included where I or S are not trans to themselves, indicating that for some donor atoms the trans influence dominates over other factors such as the cis influence and packing forces. (Less)","PeriodicalId":6887,"journal":{"name":"Acta Crystallographica Section B Structural Crystallography and Crystal Chemistry","volume":"1 1","pages":"748-752"},"PeriodicalIF":0.0,"publicationDate":"1990-12-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"78163161","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
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