| 新型氧桥和多硫基杂桥联的双核钼硫亚硝基化合物〔(CH_3)_4N〕_2K〔Mo_2OS_2(NO)_2(S_2)_2S_5)·H_2O的合成和晶体结构 |
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| 引用本文： | 吴新涛,王兵.新型氧桥和多硫基杂桥联的双核钼硫亚硝基化合物〔(CH_3)_4N〕_2K〔Mo_2OS_2(NO)_2(S_2)_2S_5)·H_2O的合成和晶体结构[J].结构化学,1983(1). |
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| 作者姓名： | 吴新涛 王兵 |
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| 作者单位： | 中国科学院福建物质结构研究所
(吴新涛)，中国科学院福建物质结构研究所(王兵) |
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| 摘 要： | 本文报导(CH_3)_4N]_2KMo_2OS_2(NO)_2(S_2)S_5]·H_2O的合成和晶体结构。该化合物晶体属于单斜晶系,所属的空间群为P2_1/c。晶胞参数为:a=13.320(2),b=17.377(2),c=13.269(3),β=107.93(2)°,Z=4。在CAD—4四圆衍射仪上,用MoKα射线收录了3576个独立衍射数据(I≥3σ(I))。晶体结构用直接法解出,经Fourier合成和全矩阵最小二乘方修正,最后偏离因子R=0.045。结构分析表明,晶体中Mo—Mo间距为3.421,二钼原子间未成键。Mo原子周围呈近似五角双锥的七配位构型。本结构的特征在于二Mo原子间除双硫桥外还存在氧桥。
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The Synthesis and Structure of a Novel Dineuclear Molybdenum Compound [(CH_3)_4N]_2K[Mo_2OS_2(NO)_2(S_2)_2S_5]·H_2O |
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| Abstract: | Reported here is a novel dineuclear molybdenum-sulfur complex with two different bridge-ligands, {(CH3)4N}2K{MO2OS2NO)2(S2)2S5} H2O(1).The reaction of molybdate ions with potassinum polysulfide in aqueous solution in the presence of hydroxylamine hydrochloride leads to the formation of the dark orange-red crystalline compound (1), which was characterized not only by elemental analysis, 1R spectrum and powder X-ray diffraction, but by single-crystal X-ray structure analysis as well. The complex (1) shows principal IR absorptions (cm-1) at ca. 1550(br. vs) {v(NO)}, 600(m) { δ(MoN)}, 790,415(m) {v(MoOMo)}, 516 ,525 { v (SS)} , 450(m) { v(MoSMo)} ,and 320, 330(m) { v(MoS)}.The compound (1) crystallizes with a=13.3201(22), b=17.3772(23)., c=13.2686(34)A, β = 107.9339(16) in the monoclinic space group P21/c and Z=4. 3576 independent reflections are collected on our CAD-4 diffractometer with Sinθ/λ<0.595A-1, MoKa and refined to R=0 0448,The detail structural data of the molecule and crystal has also been given in this paper |
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