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首页> 外文期刊>Zeitschrift fur Anorganische und Allgemeine Chemie >1 : 1 adducts of copper(I) and silver(I) halides with the olefinic phosphane tri(1-cyclohepta-2,4,6-trienyl)phosphane. Molecular structures of CuX[P(C7H7)(3)] (X = Cl, Br), AgCl[P(C7H7)(3)] and {Cu(mu(3)-I)[P(C7H7)(3)]}(4)
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1 : 1 adducts of copper(I) and silver(I) halides with the olefinic phosphane tri(1-cyclohepta-2,4,6-trienyl)phosphane. Molecular structures of CuX[P(C7H7)(3)] (X = Cl, Br), AgCl[P(C7H7)(3)] and {Cu(mu(3)-I)[P(C7H7)(3)]}(4)

机译：卤化铜（I）和卤化银（I）与烯属膦三（1-环庚-2,4,6-三烯基）膦的1：1加合物。 CuX [P（C7H7）（3）]（X = Cl，Br），AgCl [P（C7H7）（3）]和{Cu（mu（3）-I）[P（C7H7）（3）]的分子结构]}（4）

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摘要

A suspension of CuX (X = Cl, Br) or AgCl in organic solvents (such as CH2Cl2) reacts with P(C7H7)(3) (1) in a molar ratio 1:1 to give the mononuclear adducts CuX[P(C7H7)(3)] (X = Cl (2a), Br (2b)) and AgCl[P(C7H7)(3)] (3a) which crystallize as isotypic compounds in the orthorhombic space group Pnma (Z = 4). In the crystal, two (of the three) cyclohepta-2,4,6-trienyl substituents are present in the boat conformation, thus establishing a loose long-distance interaction between the central double bond and the metal atom. A distorted pseudo-tetrahedral coordination sphere is assumed to exist around the metal atom, with large P-M-X angles of 165.49(8)degrees (2a), 162.07(7)degrees (2b) and 168.54(3)degrees (3a), respectively. The tetrameric 1:1 adduct {Cu(mu(3)-I)[P(C7H7)(3)]}(4)(2c) which was obtained from CuI and 1 in boiling ethanol, has also been characterized by X-ray crystallography (monoclinic space group P2(1), Z = 4); it contains all 12 cyclohepta-2,4,6-trienyl substituents in the chair conformation. The NMR spectra (H-1, C-13, P-31) of the new complexes 2a-c and 3a indicate non-rigid structures in solution. At room temperature, the P-31 NMR signal of 3a appears as a doublet with an averaged coupling constant, (1)J(Ag,P), of 700.1 Hz, whereas at -45 degreesC the two expected doublets are clearly discernible with coupling constants (1)J(Ag-107, P-31) = 671.0 Hz and (1)J(Ag-109, P-31) = 774.4 Hz, respectively. [References: 54]
机译：CuX（X = Cl，Br）或AgCl在有机溶剂（例如CH2Cl2）中的悬浮液与P（C7H7）（3）（1）的摩尔比为1：1，得到单核加合物CuX [P（C7H7） ）（3）]（X = Cl（2a），Br（2b））和AgCl [P（C7H7）（3）]（3a）结晶成正交晶体空间群Pnma（Z = 4）中的同型化合物。在晶体中，舟形中存在两个（三个）环庚-2,4,6-三烯基取代基，因此在中心双键和金属原子之间建立了松散的长距离相互作用。假定金属原子周围存在变形的伪四面体配位球，其大P-M-X角分别为165.49（8）度（2a），162.07（7）度（2b）和168.54（3）度（3a）。由CuI和1在沸腾的乙醇中获得的四聚体1：1加合物{Cu（mu（3）-I）[P（C7H7）（3）]}（4）（2c）的特征还在于X-射线晶体学（单斜空间群P2（1）/ n，Z = 4）;它在椅子构象中包含所有12个环庚2,4,6-三烯基取代基。新配合物2a-c和3a的NMR光谱（H-1，C-13，P-31）表明溶液中存在非刚性结构。在室温下，3a的P-31 NMR信号为双峰，平均偶联常数（1）J（Ag，P）为700.1 Hz，而在-45摄氏度时，通过偶联可清楚地识别出两个预期的双峰常数（1）J（Ag-107，P-31）= 671.0 Hz和（1）J（Ag-109，P-31）= 774.4 Hz。 [参考：54]

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