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本文合成了钼硫原子簇新化合物(NH_4)_4[Mo_3(NO)_4S_(13)]·3H_2O,并用X射线单晶衍射法测定了晶体结构.晶体属三斜晶系,空间群C_i~1—P_1~-,晶胞参数:a=9.535(2)A,b=9.740(2)A,C=15.795(4)A,a=89.85(2)°,β=91.80(2)°,r=99.37(1)°,V=1446.6A~3,Z=2.1903个衍射点参与修正,最终偏差因子R=0.075,R_ω=0.074.此化合物中硫和钼的结合状态是多种多样的.中心两个硫原子分别和三个钼成键,构成三角双锥.除了过硫配位基S_2~(-2)外,还有三个硫原子组成的多硫链.钼原子的配位数为7,采用稍有畸变的五角双锥构型.和钼配位的三个NO基,Mo—N—O是直线型的;和多硫链结合的NO基,S—N—O是弯曲型的。
In this paper, a new compound (NH_4) _4 [Mo_3 (NO) _4S_ (13)) · 3H_2O was synthesized and its crystal structure was determined by X-ray single crystal diffraction.The crystal belongs to the triclinic system with space group C_i ~ 1- P_1 ~ -, cell parameters: a = 9.535 (2) A, b = 9.740 (2) A, C = 15.795 (4) A, a = 89.85 (2) °, β = 91.80 99.37 (1) °, V = 1446.6A ~ 3 and Z = 2.1903 diffraction points, the final deviation factor R = 0.075 and R_ω = 0.074. The binding states of sulfur and molybdenum in this compound are diverse. A sulfur atom and three molybdenum bond, forming a triangular double cone.In addition to the over-sulfur ligand S_2 ~ (-2), there are three sulfur atoms composed of polysulfide chain.Molybdenum atoms with a coordination number of 7, Using a slightly distorted pentagonal bipyramidal configuration with three NO moieties coordinated to molybdenum, Mo-N-O being linear; and a polysulphide-bonded NO group with S-N-O being curved.