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首页> 外文期刊>Dalton transactions: An international journal of inorganic chemistry >Spectroscopy and structures of two complete families, one mononuclear, theother binuclear, of 1: 2 CuX : dptu stoichiometry (X = Cl, Br, I; 'dptu' =N,N'-diphenylthiourea)
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Spectroscopy and structures of two complete families, one mononuclear, theother binuclear, of 1: 2 CuX : dptu stoichiometry (X = Cl, Br, I; 'dptu' =N,N'-diphenylthiourea)

机译：两个完整家族的光谱学和结构：一个单核，另一个双核，1：2 CuX：dptu化学计量比（X = Cl，Br，I;'dptu'= N，N'-二苯基硫脲）

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摘要

Crystallization of the copper(I) halides (CuX; X = Cl, Br, I) with N,N'-diphenylthiourea ('dptu' =(PhNH)_2,CS) in I : 2 ratio from acetonitrile solution in ambient conditions yields a mononuclearisomorphous series of complexes of the form [XCu(dptu)_2].H_2Oan unusually complete array, with thecentral copper atoms in quasi-trigonal planar environments, as shown by single crystal X-ray studies, inturn providing a platform for comparative spectroscopic studies. Under anhydrous conditions,anhydrous compounds may be obtained, a full series again being accessible, but now of the binuclearform [(dptu)XCu(μ-S-dptu)_2CuX(dptu)], the chloride being a bis(acetonitrile) solvate, the isomorphousbromide and iodide pair being unsolvated. A (solvated) sulfate salt is found to be of the form[Cu(dptu)_2]_2(SO_4), providing a novel example of a copper(I) atom being (quasi-)linearly coordinated bythe pair of unidentate (dptu) sulfur ligands, Cu-S 2.1770(5), 2.1811(5) A, S-Cu-S 162.18(2)°. Thev(CuX) vibrational frequencies are assigned in the far-IR spectra of [XCu(dptu)_2].H_2O(X = Cl, Br, I)at 274, 207, and 190 cm~(-1)respectively. The broadline static~(65)Cu NMR spectra of [Cl_2Cu_2(dptu)_4].2CH_3CN and [X_2Cu_2(dptu)_4] (X = Br, I) have been recorded at 9.4 and 7.05 T, and the spectra havebeen analysed to yield the~ (65)Cu nuclear quadrupole coupling and chemical shift parameters. The ~(63.65)Cunuclear quadrupole resonance frequencies of [XCu(dptu)_2].H_2O(X = Cl, Br, I) have also beenmeasured, and the resulting ~(65)Cu quadrupole coupling constants areca.4x those of the dimeric[X_2Cu_2(dptu)_4] compounds.
机译：用N：N'-二苯基硫脲（'dptu'=（PhNH）_2，CS）以I：2的比例从环境中的乙腈溶液中结晶出卤化铜（I）（CuX; X = Cl，Br，I） [XCu（dptu）_2]形式的单核同构配合物系列。H_2O具有非常完整的阵列，在准三角形平面环境中具有中心铜原子，如单晶X射线研究所示，这反过来又为比较光谱研究提供了平台。在无水条件下，可以获得无水化合物，但仍可得到全系列化合物，但现在是双核形式的[（dptu）XCu（μ-S-dptu）_2CuX（dptu）]，氯化物为双（乙腈）溶剂化物，异溴化物和碘化物对未被溶剂化。发现（溶剂化）硫酸盐的形式为[Cu（dptu）_2] _2（SO_4），提供了一个铜（I）原子被一对未鉴定的（dptu）线性（准）线性配位的新实例硫配体，Cu-S 2.1770（5），2.1811（5）A，S-Cu-S 162.18（2）°。在[XCu（dptu）_2] .H_2O（X = Cl，Br，I）的远红外光谱中分别在274、207和190 cm〜（-1）处分配了v（CuX）振动频率。 [Cl_2Cu_2（dptu）_4] .2CH_3CN和[X_2Cu_2（dptu）_4]（X = Br，I）的宽线静态〜（65）Cu NMR光谱已在9.4和7.05 T记录下来，并进行了分析得到〜（65）Cu核四极偶合和化学位移参数。还测量了[XCu（dptu）_2] .H_2O（X = Cl，Br，I）的〜（63.65）核四极共振频率，所得〜（65）Cu四极耦合常数约为二聚体常数的4倍。 [X_2Cu_2（dptu）_4]化合物。

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