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本文报道具有松散配位的三核钼簇合物{Mo_3(μ_3-S)(μ-S)_3[S_2P(OEt)_2]_4·L’(L’=H_2O,1;C_3H_3ON,2)和SbCl_3在HCl-EtOH中的加合反应及其产物{Mo_3(μ_3-S)[(μ-S)_3·SbCl_3]·[S_2P(OEt)_2]_4(C_2H_5OH)}(C_2H_5OH)(3)和{Mo_3(μ_3-S)[(μ-S)_3·SbCl_3][S_2P(OEt)_2]_3[SXP(OEt)_2]·(C_3H_3ON)}(X=S,O)(4)的晶体结构.晶体3空间群属P2_1/n,晶胞参数为α=13.250(3),6=17.296(4),c=23.223(9)A,β=92.4l(3)°,D_(?)=1.844g·cm~(-3);晶体4空间群属PI,晶胞参数为α=10.342(3),b=11.994(3),c=21.352(4)A,α=76.27(2),β=88.55(2),γ=73.26(2)°,D_=1.947g·cm~(-3).晶体3、4的最终结构偏离因子分别为0.078和0.068.结构测定结果表明,这两个加合物的分子由{Mo_3(μ_3-S)(μ-S)_3[S_2P(OEt)_2]_4·L(L=C_2H_5OH,C_3H_3ON)通过三个(μ-S)联结SbCl_3而成,从而获得了{Mo_3SbS_4}的类立方烷簇胳构型,Sb—S之间存在较弱的配位键.由此推断,若加合的金属原子的轨道和电子组态适宜,有可能通过这种[3+1]的成簇模式获得四核的同核或异核簇合物.
In this paper, we report the existence and distribution of the tri-nuclear molybdenum clusters {Mo_3 (μ_3-S) (μ-S) _3 [S_2P (OEt) _2] _4 · L ’(L’ = H_2O, 1; C_3H_3ON, 2) The Addition of SbCl_3 in HCl-EtOH and Its Products {Mo_3 (μ_3-S) [(μ-S) _3 · SbCl_3] · [S_2P (OEt) _2] _4 (C_2H_5OH) (C_2H_5OH) The crystal structure of {Mo_3 (μ_3-S) [(μ-S) _3 · SbCl_3] [S_2P (OEt) _2] _3 [SXP (OEt) _2] · (C_3H_3ON)} (X = S, O) . The crystal 3 space group P2_1 / n has the unit cell parameters of α = 13.250 (3), 6 = 17.296 (4), c = 23.223 (9) A, β = 92.41 (3) °, 1.844g · cm -3. For the crystal 4 space group PI, the unit cell parameters are α = 10.342 (3), b = 11.994 (3), c = 21.352 (4) A and α = 76.27 β = 88.55 (2), γ = 73.26 (2) °, D_ = 1.947g · cm -3 .The final structure deviation factors of crystal 3,4 were 0.078 and 0.068, respectively.The results of structure determination showed that the two Adduct molecules are composed of three (μ-S) bonds of SbCl_3 from {Mo_3 (μ_3-S) (μ-S) _3 [S_2P (OEt) _2] _4 · L (L = C_2H_5OH, C_3H_3ON) The cubic Cuban cluster structure of {Mo_3SbS_4} is obtained, and there is a weak coordinate bond between Sb-S, so it can be deduced that if the orbital and electronic configurations of the added metal atoms are suitable, [3 + 1] clustering pattern We have homonuclear or heteronuclear quad-core clusters.