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...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.展开更多
基金Supported by the NNSFC (20071024, 20371033) and the Key Laboratory of Organic Synthesis of Jiangsu Province, Suzhou University
文摘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.