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化学学报
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化学学报 ›› 2003, Vol. 61 ›› Issue (11): 1828-1833. 上一篇    下一篇

研究论文

锌二硫代氨基甲酸配合物的合成、晶体结构及其热稳定性研究

钟昀;章伟光;张启交;谭民裕;王素兰   

  1. 兰州大学化学化工学院;华南师范大学化学系;国立清华大学化学系
  • 发布日期:2003-11-15

Synthesis, Struture and Thermal Stability of Zinc Complexes with Dithiocarbamate

Zhong Yun;Zhang Weiguang;Zhang Qijiao;Tan Minyu;Wang Sulan   

  1. Department of Chemistry, Lanzhou University;Department of Chemistry, South China Normal University;Department of Chemistry, National Tsinghua University
  • Published:2003-11-15

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814

被引次数

20 | 5

合成了3个二硫代氨基甲酸锌配合物[Zn_2(S_2CNBu_2~n)_4]，[Zn(S_2CNBy_2) _2](2)和[Zn(S_2CNBy_2)_2Py] (3) (Bu~n = 正丁基，By=苄基，Py=吡啶)。测定 了它们的晶体结构，红外光谱和热稳定性。1为单斜晶系，空间群C2/c，晶胞参数 a=2.3329(3)nm, b=1.7090(2)nm, c=1.6115(2)nm. α=90 °β=127.560(10) °, γ=90 °.2为正交晶系，空间群Pbcn，晶胞参数a=1.62193(11)nm, b=1.90010(12) nm, c=0.93795(6)nm. α=90 °,β=90 °,γ=90 °.3为三斜晶系，空间群P-1， 晶胞参数a=0.86418(6)nm, b=1.31156(9)nm, c=1.66238(11)nm. α=106.398(1) °,β=92.633(1) °,γ=107.461(1) °.1为二聚体，属典型的荒氨酸金属配合物 结构类型。2为一单核匹配位化合物，而在荒氨酸金属配合物中（除Ln,Ac系外）该 结构类型非常少见。2中引入吡啶环得到3，3为一五配位化合物，吡啶环的引入说 明2的中心离子处于配位不饱和状态，这与以往报道相吻合。1的热稳定性质研究发 现其在251 ℃有升华现象，可作为MOCVD的前驱物。

关键词: 锌络合物, 二硫代氨基甲酸 P, 晶体结构, 热稳定性, 吡啶 P, 红外分光光度法

Three zinc complexes with dithiocarbamate were synthesized. They are [Zn2 (S2CNB112 )4] (1), [Zn-(S2CNBy2)2] (2) and [Zn(S2CNBy2)2Py] (3) (where By = benzyl, Py = pyridine). Their crystal structure, IR spectra and theimal stability were determined. 1 is monoclinic, space group C2/c, with a =2.3329(3) nm, b = 1.7090(2) nm, c = 1.6115(2) nm. a =90°, /?= 127.560(10)°, 7 = 90°. 2 is orthorhombic, space group Phcn, with a = 1.6219(11) nm, 6 = 1.9001(12) nm, c = 0.9376(6) nm. a = 90°, /? = 90°, 7 = 90°. 3 is triclinic, space group P-l, with a = 0.8642(6) nm, 6 = 1.3116(9) nm, c = 1.6624(11) nm. a = 106.398(1)° , ￡ = 92.633(1)°, 7 = 107.461(1)°. Compound 1 is dimeric, which belongs to the typical structure of metal dithiocarbamate complexes. 2 is monomeric which is seldom appeared in metal (except Ln, Ac series) complexes with dithiocarbamate. 2 could coordinate with pyridine to form 3. 3 is a five-coordinated complex. It is indicated that the center metal ion of 2 is unsaturated, which is the same as some in the existed reports. The thermal stability of 1 shows that it could sublime at 251 °C , so 1 may be precursor for MOCVD.

Key words: ZINC COMPLEX, CARBAMODITHIOIC ACID P, CRYSTAL STRUCTURE, THERMAL STABILITY, PYRIDINE P, IR

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