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本文报道了两个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·(C_3H_3ON)}·CH_3GN(Ⅰ)、{Mo_3(μ_3—O)(μ—S)_3[S_2P(OEt)_2]_4(C_3H_3ON)}(Ⅱ)的合成和晶体结构。簇合物(Ⅰ)属单斜晶系,空间群为P2_2/n,晶胞参数为a=16.579(3),b=16.959(2),c=16.867(2);β=94.44(1)°;v=4728 3;Z=4;D_c=1.778g·cm~(-3),用Patterson法解出结构,最终偏离因子R=0.045。簇合物(Ⅱ)属三斜晶系,空间群为P1,晶胞参数为a=13.175(4),b=13.372(6),c=16.656(3);α=117.87(4)°,β=60.09(3)°,γ=109.03(3)°;ν=2231 3;Z=2;D_c=1.798g·cm~(-3),用直接法解出结构,最终偏离因子R=0.066。两个簇合物均为以具有一个松散配位为特征的单帽三核簇,而且松散配位上均被一嘿唑五员环所占据,其主要差别在于簇合物(Ⅰ)的簇胳为Mo_3S_4,而簇合物(Ⅱ)则为一Mo_3OS_3·文中对这一“松散”配位的三核钼簇合物的活泼性进行了讨论。
In this paper, we report the synthesis of two tetranuclear molybdenum clusters {Mo_3 (μ_3-S) (μ-S) _3 [S_2P (OEt) _2] _4 · (C_3H_3ON)} CH_3GN (Ⅰ) The synthesis and crystal structure of (μ_3-O) (μ-S) _3 [S_2P (OEt) _2] _4 (C_3H_3ON)} (Ⅱ) The cluster (Ⅰ) belongs to the monoclinic system with a space group of P2_2 / n with unit cell parameters of a = 16.579 (3), b = 16.959 (2), c = 16.867 The structure was solved by Patterson method and the final deviation factor was R = 0.045. The cluster (Ⅱ) belongs to the triclinic system with the space group P1 and the unit cell parameters a = 13.175 (4), b = 13.372 (6) and c = 16.656 The structure was solved by the direct method with the final deviation factor of R = 0.066 (β = 60.09 (3) °, γ = 109.03 (3) °; ν = 2231 3; Z = 2; D_c = 1.798g · cm -3) . Both clusters are single-capped triple-core clusters characterized by a loose coordination, and are loosely coordinated by a five-membered ring. The main difference is that the clusters Mo 3 S 4 as the cluster, and Mo 3 OS 3 as the cluster (II). The activity of this “loosely coordinated” ternary molybdenum cluster was discussed.