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Five-co-ordination with ‘hybrid’ ligands. Part VII. Cobalt(II) and nickel(II) complexes with asymmetric tripod ligands having N2OP, N2SP, and NOAs2 donor sets 与“杂化”配体的五配位。第七部分。钴(II)和镍(II)配合物具有N2OP、N2SP和NOAs2供体集的不对称三脚架配体
Pub Date : 1971-01-01 DOI: 10.1039/J19710001487
R. Morassi, L. Sacconi
The asymmetric ‘tripod’ ligands N-[2-(diphenylphosphino)ethyl]-N-(2-methoxyethyl)-N′N′- diethylthylenediamine (I; donor set N2OP) and N-[2-(diphenylphosphino)ethyl)-N-[2-(methylthio)ethyl]-N′N′-diethylethylenediamine (II; donor set N2SP) form cobalt(II) and nickel(II) complexes with general formula [MLX]BPh4(X = halogen or NCS). The cobalt(II) complexes are high-spin and five-co-ordinate, probably trigonal bipyramidal, both in the solid state and in solution. The [NiLX]BPh4 complexes with L =(I), X = l or NCS are low-spin and probably five-co-ordinate in the solid state with a distorted square-pyramidal stereochemistry. All the other nickel complexes are thought to have a square-planar structure with the ligand L being terdentate with an NNP donor set. The complex [Ni(NOAs2)l]BPh4 derived from the ligand NN-bis-(2-diphenylarsinoethyl)-2-methoxyethylamine (III; donor set NOAs2) is accorded a five-co-ordinate, ‘elongated’ square-pyramidal structure.
不对称“三脚架”配体N-[2-(二苯基膦)乙基]-N-(2-甲氧基乙基)-N ' N ' -二乙二胺(I;N-[2-(二苯基膦)乙基]-N -[2-(甲基硫)乙基]-N ' N ' -二乙基乙二胺(II);用通式[MLX]BPh4(X =卤素或NCS)形成钴(II)和镍(II)配合物。钴(II)配合物在固体和溶液中都是高自旋和五坐标的,可能是三角双锥体。L =(I), X = L或NCS的[NiLX]BPh4配合物具有低自旋和可能的五坐标固相,具有扭曲的方锥体立体化学。所有其他的镍配合物被认为具有方形平面结构,配体L与NNP给体集是三齿合的。配合物[Ni(NOAs2) 1]BPh4由配体nn -二-(2-二苯larsinethyl)-2-甲氧基乙胺(III;供体集NOAs2)被赋予一个五坐标,“拉长”的方形金字塔结构。
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引用次数: 5
The vibrational spectra of silane and germane derivatives. Part V. The infrared and Raman spectra of dihalogeno(methyl)germanes 硅烷和锗衍生物的振动谱。第五部分:二卤基(甲基)日耳曼的红外光谱和拉曼光谱
Pub Date : 1971-01-01 DOI: 10.1039/J19710003291
G. K. Barker, J. Drake, R. Hemmings, B. Rapp
The i.r. and Raman spectra of the series of dihalogeno(methyl)germanes, MeGeHX2(X = F, Cl, Br, I) and their specifically deuteriated analogues, MeGeDX2, are recorded. A normal co-ordinate treatment based on a modified valence force field confirms the assignment of 17 of the 18 fundamental frequencies for each molecule. The torsional mode is not observed. The transferability of the force constants between the protonated and deuteriated species is tested.
记录了一系列二卤代(甲基)日耳曼化合物MeGeHX2(X = F, Cl, Br, I)及其特殊氘化类似物MeGeDX2的红外光谱和拉曼光谱。基于修正价力场的标准坐标处理确认了每个分子18个基本频率中的17个。没有观察到扭转模态。测试了质子化和氘化物质之间力常数的可转移性。
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引用次数: 3
Molecular complexes. Part X. The crystal and molecular structure of the 1 : 1 complex of 8-hydroxyquinoline and 1,3,5-trinitrobenzene 分子复合物。第十部分:8-羟基喹啉与1,3,5-三硝基苯1:1配合物的晶体和分子结构
Pub Date : 1971-01-01 DOI: 10.1039/J19710000550
E. Castellano, C. Prout
The crystal structure of the 1 : 1 complex of 8-hydroxyquinoline and 1,3,5-trinitrobenzene has been determined by three-dimensional X-ray methods. It is a plane-to-plane π–π* electron donor–acceptor complex formed from dimeric 8-hydroxyquinoline molecules as electron donors and 1,3,5-trinitrobenzene molecules as acceptors. In the stacks of alternating donor and acceptor molecules, each 1,3,5-trinitrobenzene molecule is located in the position of maximum π–π* overlap with respect to one of its neighbouring 8-hydroxyquinoline molecules and somewhat shifted from that position with respect to the other.The 8-hydroxyquinoline dimer is held together by a bifurcated hydrogen-bond system similar to that in the 8-hydroxyquinoline–chloranil complex.
用三维x射线法测定了8-羟基喹啉与1,3,5-三硝基苯1:1配合物的晶体结构。它是由二聚体8-羟基喹啉分子为电子供体,1,3,5-三硝基苯分子为受体形成的平面对平面π -π *电子供体-受体配合物。在供体和受体交替排列的分子堆中,每个1,3,5-三硝基苯分子相对于相邻的8-羟基喹啉分子中的一个分子位于最大π -π *重叠的位置,并且相对于另一个分子在一定程度上发生了移位。8-羟基喹啉二聚体是由一个类似于8-羟基喹啉-氯胺配合物的分叉氢键系统结合在一起的。
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引用次数: 15
Solvent extraction from halide solutions. Part V. Temperature-dependence and dissociation of ion pairs 卤化物溶液的溶剂萃取。第五部分:离子对的温度依赖性和解离
Pub Date : 1971-01-01 DOI: 10.1039/J19710000650
Z. Maksimović, A. Maddock
The temperature-dependence of the extraction coefficients of different organic solvents for metals, such as gallium and iron, from aqueous hydrochloric acid solutions, has been shown to depend on the metal concentration. The data have been analysed to yield entropies and enthalpies of dissociation of the extracting acids in the organic phase. The peculiarities of the values obtained are discussed.
从盐酸水溶液中提取金属(如镓和铁)的不同有机溶剂萃取系数的温度依赖性已被证明取决于金属浓度。对这些数据进行了分析,得出了萃取酸在有机相中的解离熵和解离焓。讨论了所得值的特殊性。
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引用次数: 0
Far-infrared reflectance spectra of A2CuCl4,2H2O (A = NH4, K, or Rb) single crystals: copper–chlorine vibrations of the distorted octahedral aquochlorocuprate(II) anion A2CuCl4,2H2O (A = NH4, K,或Rb)单晶的远红外反射光谱:畸变八面体水氯酸盐(II)阴离子的铜-氯振动
Pub Date : 1971-01-01 DOI: 10.1039/J19710002724
J. Dunsmuir, A. Lane
The polarised far-i.r. reflectance spectra of A2CuCl4,2H2O (A = NH4, K, or Rb) single crystals have been recorded in the region 40–400 cm–1. These have permitted the observation and assignment of most of the predicted bands, including one at ca. 180 cm–1 due predominantly to the ‘long’ Cu–Cl stretching mode. Anomalies in the reflectance spectra of (111) faces of these crystals are discussed.
偏振的远红外线。A2CuCl4,2H2O (A = NH4, K,或Rb)单晶的反射光谱在40-400 cm-1范围内。这使得大多数预测波段的观测和分配成为可能,包括一个大约180 cm-1的波段,主要是由于“长”Cu-Cl拉伸模式。讨论了这些晶体(111)面反射光谱中的异常现象。
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引用次数: 3
Metal–metal bonding in co-ordination complexes. Part XI. Crystal and molecular structure of di[(benzenesulphinato)-µ-hydroxo-phenylstannio]-tetracarbonyldi-π-cyclopentadienyl-di-iron 配位配合物中的金属-金属键。二[(苯磺酸)-µ-羟基苯基锡]-四羰基二π-环戊二烯基二铁的晶体和分子结构
Pub Date : 1971-01-01 DOI: 10.1039/J19710003364
R. Restivo, R. Bryan
The compound previously formulated as (π-C5H5)Fe(CO)2Sn(Ph)(OSOPh)(OH) has been shown, by X-ray analysis, to be a centrosymmetric dimer with two five-co-ordinate tin atoms linked by a dihydroxo-bridge. The Sn–O bond lengths are 2·054(2)A and the O–Sn–O and Sn–O–Sn bond angles are 70·8(1) and 109·2(1)°, respectively. The Sn–Fe bond distance of 2·499(1)A is ca. 0·03 A longer than the limiting value for this bond type and is presumed to be a σ-bond. Other bond distances of interest are Sn–O(non-bridging) 2·206(2), Sn–C 2·146(3), Fe–C(carbonyl) 1·765(4), Fe–C(ring) 2·093(4), CO 1·142(5), S–O 1·539(3), SO 1·499(3), and S–C 1·808(4)A.Crystals of the dimer are monoclinic with cell dimensions a= 9·698(2)b= 18·097(3), c= 13·516(4)A, β= 123·44(3)°, space group P21/c, and Z= 2. The structure analysis, based on 2592 independent intensities measured by counter diffractometry, was carried out by the heavy-atom method and refinement was by least-squares techniques to a final R of 0·024.
x射线分析表明,先前分子式为(π-C5H5)Fe(CO)2Sn(Ph)(OSOPh)(OH)的化合物是由两个五配位锡原子通过二羟基桥连接的中心对称二聚体。Sn-O键长为2.054 (2)A, O-Sn-O键角为70·8(1)°,Sn-O - sn键角为109·2(1)°。Sn-Fe键距为2·499(1)A,比该键的极限值长约0.03 A,推测为σ-键。其他感兴趣的键距有Sn-O(非桥接)2·206(2)、Sn-C 2·146(3)、Fe-C(羰基)1·765(4)、Fe-C(环)2·093(4)、CO 1·142(5)、S-O 1·539(3)、SO 1·499(3)和S-C 1·808(4)A。二聚体晶体呈单斜晶型,细胞尺寸a= 9·698(2)b= 18·097(3),c= 13·516(4)a, β= 123·44(3)°,空间群P21/c, Z= 2。采用重原子法对2592个独立的反衍射强度进行了结构分析,并采用最小二乘技术进行了细化,最终R为0·024。
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引用次数: 12
Unstable intermediates. Part LXXXVIII. Alkali-metal interaction with trapped hydrogen atoms in barium sulphate 不稳定的中间体。LXXXVIII一部分。碱金属与困在硫酸钡中的氢原子的相互作用
Pub Date : 1971-01-01 DOI: 10.1039/J19710000833
M. Bloom, R. Eachus, M. Symons
Barium sulphate doped with various alkali-metal salts gave, on exposure to 60Co γ-rays at 77 K, two types of trapped hydrogen atoms, one of which had e.s.r. spectra characterised by hyperfine coupling to the alkali-metal cations. For example, the species NaH+ had gav= 2·0013, a‖(1H)= 513·2 G, a⊥(1H)= 510·7 G, a‖(23Na)= 21·4 G and a⊥(23Na)= 15·1 G.These results, together with data for other host crystals, are discussed in terms of the structure of the adducts and their stability.
掺入各种碱金属盐的硫酸钡,在77 K的60Co γ射线下暴露后,有两种类型的氢原子被捕获,其中一种具有与碱金属阳离子超精细耦合的e.s.r.光谱。例如,物种NaH+具有gav= 2·0013,a‖(1H)= 513·2g, a⊥(1H)= 510·7 G, a‖(23Na)= 21·4 G和a⊥(23Na)= 15·1 G。这些结果以及其他宿主晶体的数据都是根据加合物的结构及其稳定性进行讨论的。
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引用次数: 1
Metal carbonyl chemistry. Part XV. Reactions of the dicarbonylbis-(triphenylphosphine)rhodate anion, [Rh(CO)2(PPh3)2]–, with some perfluoroaromatic compounds 金属羰基化学。十五。二羰基双-(三苯基膦)铑阴离子[Rh(CO)2(PPh3)2] -与一些全氟芳香化合物的反应
Pub Date : 1971-01-01 DOI: 10.1039/J19710000927
B. Booth, R. Haszeldine, Ian Perkins
The carbonylmetal anion [Rh(CO)2(PPh3)2]– has been shown to be a strong nucleophile of similar power to that of [(π-C5H5)Fe(CO)2]– or [(π-C5H5)Ru(CO)2]–. Its reactions with the compounds C6F6, C6F5X (X = CN or CO2Et), (NC)2C6F4, C5F5N, and 2-(NC)C5F4N to afford some new perfluoroaromatic rhodium(l) complexes are discussed.
羰基金属阴离子[Rh(CO)2(PPh3)2] -是与[(π-C5H5)Fe(CO)2] -或[(π-C5H5)Ru(CO)2] -相似的强亲核试剂。讨论了它与化合物C6F6、C6F5X (X = CN或CO2Et)、(NC)2C6F4、C5F5N和2-(NC)C5F4N反应生成一些新的全氟芳香铑(l)配合物。
{"title":"Metal carbonyl chemistry. Part XV. Reactions of the dicarbonylbis-(triphenylphosphine)rhodate anion, [Rh(CO)2(PPh3)2]–, with some perfluoroaromatic compounds","authors":"B. Booth, R. Haszeldine, Ian Perkins","doi":"10.1039/J19710000927","DOIUrl":"https://doi.org/10.1039/J19710000927","url":null,"abstract":"The carbonylmetal anion [Rh(CO)2(PPh3)2]– has been shown to be a strong nucleophile of similar power to that of [(π-C5H5)Fe(CO)2]– or [(π-C5H5)Ru(CO)2]–. Its reactions with the compounds C6F6, C6F5X (X = CN or CO2Et), (NC)2C6F4, C5F5N, and 2-(NC)C5F4N to afford some new perfluoroaromatic rhodium(l) complexes are discussed.","PeriodicalId":17321,"journal":{"name":"Journal of The Chemical Society A: Inorganic, Physical, Theoretical","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"1971-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"72909877","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}
引用次数: 6
Solutions in acetone. Part II. Transference numbers of potassium thiocyanate and ionic conductances in acetone at 25 °C 丙酮溶液。第二部分。25℃时硫氰酸钾在丙酮中的转移数和离子电导
Pub Date : 1971-01-01 DOI: 10.1039/J19710002415
H. Brookes, M. Hotz, A. Spong
Transport numbers for the thiocyanate anion constituent of KCNS in anhydrous acetone have been measured by a conductimetric moving-boundary method at 25 °C. The limiting transport number obtained is t°CNS–= 0·6237 ± 0·0009. Limiting ion conductances in acetone have been calculated and discussed.
用电导移动边界法测定了KCNS中硫氰酸盐阴离子组分在无水丙酮中的输运数。得到的极限输运数为t°CNS - = 0.6237±0.0009。对丙酮中的极限离子电导进行了计算和讨论。
{"title":"Solutions in acetone. Part II. Transference numbers of potassium thiocyanate and ionic conductances in acetone at 25 °C","authors":"H. Brookes, M. Hotz, A. Spong","doi":"10.1039/J19710002415","DOIUrl":"https://doi.org/10.1039/J19710002415","url":null,"abstract":"Transport numbers for the thiocyanate anion constituent of KCNS in anhydrous acetone have been measured by a conductimetric moving-boundary method at 25 °C. The limiting transport number obtained is t°CNS–= 0·6237 ± 0·0009. Limiting ion conductances in acetone have been calculated and discussed.","PeriodicalId":17321,"journal":{"name":"Journal of The Chemical Society A: Inorganic, Physical, Theoretical","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"1971-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"73182208","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}
引用次数: 8
Mössbauer spectra and structures of organotin compounds. The relationship between quadrupole splitting and intermolecular association Mössbauer有机锡化合物的光谱和结构。四极分裂与分子间缔合的关系
Pub Date : 1971-01-01 DOI: 10.1039/J19710001191
A. Maddock, R. H. Platt
The Mossbauer spectra of cyclohexyltin derivatives and of the compounds Ph2Sn(X)·[CH2]4·Sn(X)Ph2(X = I, OH, O·CO·Me, or Ph), BunSn(O·CO·Me)4–n(n= 2 or 3), and Bu2Sn maleate have been recorded. These data are used to define the range of quadrupole splittings associated with tetrahedral organotin compounds. It is shown that the simple point-charge model does not account for the quadrupole splittings of compounds with differing co-ordination numbers. Quadrupole splitting data are used empirically to discuss intermolecular association in organotin compounds.
记录了环己基锡衍生物和化合物Ph2Sn(X)·[CH2]4·Sn(X)Ph2(X = I、OH、O·CO·Me或Ph)、BunSn(O·CO·Me)4 - n(n= 2或3)和Bu2Sn马来酸盐的穆斯堡尔光谱。这些数据用于确定与四面体有机锡化合物有关的四极分裂的范围。结果表明,简单点电荷模型不能解释具有不同配位数的化合物的四极分裂。四极分裂数据用于经验讨论有机锡化合物的分子间结合。
{"title":"Mössbauer spectra and structures of organotin compounds. The relationship between quadrupole splitting and intermolecular association","authors":"A. Maddock, R. H. Platt","doi":"10.1039/J19710001191","DOIUrl":"https://doi.org/10.1039/J19710001191","url":null,"abstract":"The Mossbauer spectra of cyclohexyltin derivatives and of the compounds Ph2Sn(X)·[CH2]4·Sn(X)Ph2(X = I, OH, O·CO·Me, or Ph), BunSn(O·CO·Me)4–n(n= 2 or 3), and Bu2Sn maleate have been recorded. These data are used to define the range of quadrupole splittings associated with tetrahedral organotin compounds. It is shown that the simple point-charge model does not account for the quadrupole splittings of compounds with differing co-ordination numbers. Quadrupole splitting data are used empirically to discuss intermolecular association in organotin compounds.","PeriodicalId":17321,"journal":{"name":"Journal of The Chemical Society A: Inorganic, Physical, Theoretical","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"1971-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"80117209","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}
引用次数: 16
期刊
Journal of The Chemical Society A: Inorganic, Physical, Theoretical
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