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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。 相似文献
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<正> {Mo4S4(μ-OAc)2(dtp)4H}3,(dtp=S2P(OEt)2),Mr=1371.60,Or-thorhombic, space group Pcab, a = 18. 90 (2) ,b = 21. 678 (4 ) , c = 24. 491 (4 ) A , V = 10031(7)A3,Z=8,Dc=1.818g/cm-3,F(000)=5464,λ(MoKa)=0.71073A,finalR= 0. 069 for 3738 independent reflections. This is a successful example of the formation of [Mo4S4]5+ from[3+1] reaction mode. The results of the structure determination indicate that the configuration of the title compound exhibits a tetranuclear cubane-type core [Mo4S4]5+ with six Mo - Mo distances in the range 2. 685~2. 969A and is very similar to that of the previously characterized compound {Mo4S4(μ-OAc)2(dtp)4}2, [Mo4S4]6+, which was obtained directly by the reaction of MoCl3·3H2O with dtp. Some notable differences, however, can be found when six Mo - Mo bond distances and bonding parameters of the four terminal bidentate ligands (dtp) are compared between these two compounds , That can be attributed to the difference in the oxidation state of these two clusters . 相似文献
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用x射线衍射法测定了四核钼原子簇化合物Mo4(μ3-S)3(μ3-O)[μ-S2P(OEt)2]3[S2P(OEt)3]的晶体结构。晶体属三种晶系。晶胞参数为a=13.387(3),b=13.997(4),c=16.281(3)Å,α=72.84(2)°,β=87.92(2)°,γ=84.87(2)°;z=2;空间群P1。由直接法(MULTAN—80)求得原子坐标。所有非氢原子坐标和热参数经全矩阵最小二乘方精修,最后偏离因子R=0.092。研究表明,在这一中性配位分子中,簇胳中心为[Mo4S3O]类立方烷构型,加上桥式和端式两种[S2P(OEt)2]-配体,每个Mo原子周期都满足了畸变六配位八面体的要求。本文还讨论了两种[S2P(OEt)2]-配体在结构参数上的差别。 相似文献
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本文报道了具有局部松散配位的三核钼原子簇{Mo3(μ3-S)(μ-S)[S2P(OEt)2]4.P(C6H5)3}.(0.86CH2Cl2)的合成和晶体结构.在CAD-4四圆衍射仪上用Mo Kα射线收集到I≥2σ(I)的衍射点4840个.采用重原子法和差电子密度法解出结构,并用全矩阵最小二乘法修正,最终偏离因子为0.058.簇分子的Mo-Mo键为2.731(1),2.748(1),2.753(1)A,Mo原子和三苯基膦的P原子配位键长为Mo-P2.647(3)A,显著长于一般的Mo-P共价单键.三苯基膦基团在Mo的配位多面体中处于三重桥S原子的对位,表现出与其他此类簇合物的松散配位体配位位置不同.文中概括了此类簇合物的Mo-Mo键和Mo-L的成键情况. 相似文献
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The oxidation-reduction reaction of the molybdenum cluster compound Mo_3(μ_3-S)(μ-S)_2-[μ-SOP(OEt)_2] [S_2P(OEt)_2]_3(O)_2 with CuCl_2·2H_2O has been investigated and the chemical components of its product, Cu_8Cl_2[S_2P(OEt)_2]_6, were confirmed. The crystal belongs to the triclinic system and the space group is P with the following unit cell parameters: a=11.578 (5), b=12.663 (3), c=14.317 (4); α=55.54 (2)°, β=57.35 (3)°, γ=72.23 (3)°; Z=1; D_(calc)=1.926 g·cm~(-3). Final discrepancy factor of R is 0.075 for 3573 unique reflections with I≥3σ(I). The results of investigation show that the crystal structure consists of molecular chains with Cu_8Cl_2[S_2P(OEt)_2]_6 as structural unit, in which eight Cu atoms form a cube-shaped cage. The coordination sphere of each Cu atom is a tetrahedron configuration. The distances between Cu atoms are 3.018-3.437, which indicates that there are no metal-metal bonds between Cu atoms. It is worthwhile to study further the phenomenon how Cu(+2) captures the 相似文献
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When trinuclear molybdenum cluster compound with "loose coordination site", Mo_3(μ_3-S)(μ-S)_3(μ-dtp)(dtp)_3·H_2O(A) (dtp=diethyldithiophos-phinato anion), is reacted with an excess of imidazole, the H_2O ligand and the bidentate bridging ligand μ-dtp are found to be simultaneously substituted by the imidazole to form the title compound. The title crystal belongs to the space group P(?), Z =2, with the following unit cell parameters: a=14.465(2), b=14.653(4), c=14.886(6), α=99.36(3),β=93.11(2),γ=114.29(2),V=2812(3). The crystalline compound consists of an ordered array of the cluster cation and dtp anion with acetone as packed molecule. The cation possesses a symmetry of C_3. Three Mo atoms form basically an equilateral triangle with three Mo—Mo bond lengths of 2.763 (1), 2.762(1), 2.756(1) respectively. 相似文献
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通过配基置换反应合成出两个新的三核钼簇合物[Mo3S4(DTC)4(DMF)](EtOH)(1)和[Mo3S4-(DTC)4(Py)](Py)2(H2O)(2). 用X射线衍射法测定了这两个簇合物的晶体结构.簇合物1的空间群为PT, 晶胞参数: A=10.624(5), b=11.373(2), c=19.216(5)埃;α=87.92(2), β=79.89(3), γ=69.44(3)°; Z=2. 簇合物2的空间群为PT, 晶胞参数:a=11.505(2), b=11.945(1), c=18.974(2)埃; α=99.18(1), β=94.82(1), γ=93.84(1)°; Z=2, 结构分析结果表明, 两个簇合物的簇胳均是{Mo3S4}^4^+的三核钼原子簇, 对簇合物中配基对Mo-Mo键的影响以及配基置换反应的规律性进行了讨论. 相似文献
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二硫代乙酰丙酮和某些金属离子络合反应的研究 总被引:1,自引:0,他引:1
报导CH3COCH2COCH3/H-2S/C2H5OH-HCl体系和十六种金属离子以及Fe(CO)5的反应,用X射线衍射法测定了九种反应产物的分子和晶体结构.本文结果总结出了该反应的规律性.研究表明,在该反应条件下,钼是唯一能够形成原子簇化合物的元素. 相似文献
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