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报道了四种二苄基二硫代氨基甲酸金属配合物 [Cd(DBTC) 2 ] 2 ( 1) ,[Hg(DBTC) 2 ] ( 2 ) ,[Nd(DBTC) 3 ·2H2 O]和 [Nd (DBTC) 3 (HMPA) 2 ] ( 3 ) (DBTC =N ,N 二苄基二硫代氨基甲酸 ;HMPA =六次甲基磷酰胺 )的合成及其红外光谱 .配合物 1~3的晶体结构用X射线晶体衍射分析确定 .配合物 1,C3 0 H2 8N2 CdS4,Mr=65 7.18,单斜晶系 ,空间群P2 1/n ,a =1.110 98( 4 )nm ,b =1.5 63 2 5 ( 5 )nm ,c =1.66695 ( 5 )nm ,β =97.92 2 0 ( 10 )° ,Z =4,R =0 .0 44 ,wR1=0 .0 91.2 ,C3 0 H2 8N2 HgS4,Mr=745 3 7,正交晶系 ,空间群Pbcn ,a =1.64 73 8( 1)nm ,b =1.864 18( 14 )nm ,c =0 .940 0 0 ( 6)nm ,Z =4,R =0 .0 3 87,wR1=0 0 965 .3 ,C57H78N9NdO2 P2 S6,Mr=13 19.82 ,单斜晶系 ,空间群P2 1/c ,a =1.3 0 3 89( 9)nm ,b =3 .470 8( 3 )nm ,c=3 .12 10 ( 2 )nm ,β =96.5 2 7( 2 )° ,Z =8,R =0 .10 2 3 ,wR1=0 .2 2 0 3 .1为二聚体 ,中心离子的配位结构为扭曲的四方锥 ;2和 3均为单核配合物 ,但中心离子的配位结构不同 ,2为扭曲的四面体 ,而 3则为变形的十二面体 .配合物的热重分析结果表明配合物 1,2在加热失重的过程中可能伴随有升华现象 ,有望作为MOCVD的前驱物
Four metal complexes of dibenzyl dithiocarbamate [Cd (DBTC) 2] 2 (1), [Hg (DBTC) 2] (2), [Nd (DBTC) 3 · 2H 2 O] The synthesis and infrared spectra of Nd (DBTC) 3 (HMPA) 2] (DBTC = N, N dibenzyldithiocarbamic acid and HMPA = hexamethylphosphoramide) The crystal structure was confirmed by X-ray crystallography. Complex 1, C3 0 H2 8N2 CdS4, Mr = 65 7.18, monoclinic system, space group P2 1 / n, a = 1.11098 (4) nm, b = 1.563 2 5 (5) nm, c = 1.66695 (5) nm, β = 97.92 2 0 (10) °, Z = 4, R = 0.044, wR1 = 0.091.2, C3 0 H2 8N2 HgS4, Mr = 745 3 7, orthorhombic space group Pbcn, a = 1.64 73 8 (1) nm, b = 1.864 18 (14) nm, c = 0.940 0 0 (6) nm, Z = 4, R = 0 0 3 87, wR1 = 0 0 965 .3, C57H78N9NdO2 P2 S6, Mr = 13 19.82, monoclinic space group P2 1 / c, a = 1.3 0 3 89 (9) nm, b = 3 .470 8 (3) nm, c = 3.12 10 (2) nm, β = 96.5 2 7 (2) °, Z = 8, R = 0.10 2 3, wR1 = 0.2203. 1 is a dimer, the coordination structure of the central ion is a distorted tetragon; 2 and 3 are mononuclear complexes, but the coordination structure of the central ion is different, 2 is a distorted tetra While the third is the deformed dodecahedron.The thermogravimetric analysis of the complexes showed that complexes 1 and 2 may be accompanied by sublimation in the process of weightlessness heating and are expected to be precursors of MOCVD