Solvothermal Syntheses of (H_2en)_2Sn_2S_6·en and[(H_2hmda)_3(Hhmda)_2](Sn_2S_6)_2Using SnCl_4 and S_8 as Starting Materials  

作　　者：JIA Ding-Xian DAI Jie ZHU Qin-Yu LU Wen GUO Wen-Juan 

机构地区：[1]Department of Chemistry and Chemical Engineering, Suzhou University, Suzhou 215006, China [2]State Key Laboratory of Coordination Chemistry, Nanjing University, Nanjing 210093, China

出　　处：《Chinese Journal of Structural Chemistry》2005年第10期1157-1163,共7页结构化学（英文）

基　　金：Supported by the NNSFC (20071024, 20371033) and the Key Laboratory of Organic Synthesis of Jiangsu Province, Suzhou University

摘　　要：Three thiostannates （H2en）2Sn2S6· en 1, （Hen）4Sn2S6 2 （en = ethylenediamine, a known compound）and [（H2hmda）3（Hhmda）2]（Sn2S6）2 3 （hmda = hexamethylenediamine） were prepared using SnCl4.5H2O and S8 as starting materials in alkylenediamine solutions under mild solvothermal conditions. Compound 1 crystallizes in the triclinic system, space group P1^- with a = 8.7491（17）, b = 10.704（2）, c = 12.2031（19） A, a = 74.888（13）, β= 72.998（12）, γ= 89.032（15）°, V = 1052.9（3） A^3, Mr = 614.08, Z= 2, De = 1.937 g/cm^3, p = 2.966 mm^-1, F（000） = 604, S = 1.211, R = 0.0579 and wR = 0.0770 for 3999 observed reβections with I 〉 2σ（I）; while 3 crystallizes in the triclinic system, space group P1^- with a = 9.8075（13）, b = 10.8266（16）, c = 14.303（2） A, a = 88.611 （10）, β = 81.030（9）, γ = 74.609（9）°, V = 1446.1 （4） A^3, Mr = 1448.78, Z = 1, Dc = 1.664 g/cm^3, μ = 2.173 mm^-1, F（000） = 730, S = 1.173, R = 0.0457 and wR = 0.0667 for 5738 observed reβections with I 〉 2σ（I）. The compounds are composed of dimeric [Sn2S6]^4- anions and protohated alkylenediamine cations.Three thiostannates （H2en）2Sn2S6· en 1, （Hen）4Sn2S6 2 （en = ethylenediamine, a known compound）and [（H2hmda）3（Hhmda）2]（Sn2S6）2 3 （hmda = hexamethylenediamine） were prepared using SnCl4.5H2O and S8 as starting materials in alkylenediamine solutions under mild solvothermal conditions. Compound 1 crystallizes in the triclinic system, space group P1^- with a = 8.7491（17）, b = 10.704（2）, c = 12.2031（19） A, a = 74.888（13）, β= 72.998（12）, γ= 89.032（15）°, V = 1052.9（3） A^3, Mr = 614.08, Z= 2, De = 1.937 g/cm^3, p = 2.966 mm^-1, F（000） = 604, S = 1.211, R = 0.0579 and wR = 0.0770 for 3999 observed reβections with I 〉 2σ（I）; while 3 crystallizes in the triclinic system, space group P1^- with a = 9.8075（13）, b = 10.8266（16）, c = 14.303（2） A, a = 88.611 （10）, β = 81.030（9）, γ = 74.609（9）°, V = 1446.1 （4） A^3, Mr = 1448.78, Z = 1, Dc = 1.664 g/cm^3, μ = 2.173 mm^-1, F（000） = 730, S = 1.173, R = 0.0457 and wR = 0.0667 for 5738 observed reβections with I 〉 2σ（I）. The compounds are composed of dimeric [Sn2S6]^4- anions and protohated alkylenediamine cations.

关 键 词：solvothermal synthesis thiostannate crystal structure hydrogen bond DIAMINE 

分 类 号：O623.731[理学—有机化学]