Solvothermal Syntheses of (H_2en)_2Sn_2S_6·en and[(H_2hmda)_3(Hhmda)_2](Sn_2S_6)_2Using SnCl_4 and S

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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) ?, α = 74.888(13), β = 72.998(12), γ = 89.032(15)°, V = 1052.9(3) ?3, Mr = 614.08, Z = 2, Dc = 1.937 g/cm3, μ = 2.966 mm-1, F(000) = 604, S = 1.211, R = 0.0579 and wR = 0.0770 for 3999 observed reflections 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) ?, α = 88.611(10), β = 81.030(9), γ = 74.609(9)°, V = 1446.1(4) ?3, Mr = 1448.78, Z = 1, Dc = 1.664 g/cm3, μ = 2.173 mm?1, F(000) = 730, S = 1.173, R = 0.0457 and wR = 0.0667 for 5738 observed reflections with I > 2σ(I). The compounds are composed of dimeric [Sn2S6]4– anions and proto- nated alkylenediamine cations. Three thiostannates (H2en) 2Sn2S6? En1, (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 the 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 = 74.888 (13), β = 72.998 (12), γ = 89.032 (15) ° and V = 1052.9 (3)? 3, Mr = 614.08, Z = 2, Dc = 1.937 g / cm3, , F (000) = 604, S = 1.211, R = 0.0579 and wR = 0.0770 for 3999 at reflections with I> 2σ (I); while 3 crystallizes in the triclinic system, space group P1 with a = 9.8075 α = 88.611 (10), β = 81.030 (9), γ = 74.609 (9) °, V = 1446.1 (4)? 3, Mr = 1448.78, F = (000) = 730, S = 1.173, R = 0.0457 and wR = 0.0667 for 5738 at refs with I> 2σ (I) for Z = 1, Dc = 1.664 g / cm3, μ = are composed of dim eric [Sn2S6] 4-anions and proto- nated alkylenediamine cations.
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