【摘 要】
：
The reaction of [Et4N]2WOS3 with three equiv, of CuI and dmpzm in MeCN afforded [WOS3Cu3I(dmpzm)2]·2(MeCN)0.5 (1·2(MeCN)0.5)while that of [PPh4]2WS4 with four
【机 构】
：
Key Laboratory of Organic Synthesis of Jiangsu Province
论文部分内容阅读
The reaction of [Et4N]2WOS3 with three equiv, of CuI and dmpzm in MeCN afforded [WOS3Cu3I(dmpzm)2]·2(MeCN)0.5 (1·2(MeCN)0.5)while that of [PPh4]2WS4 with four equiv, of CuI in DMF/MeCN followed by the addition of two equiv, of dmpzm in MeOH gave rise to [WS4Cu4I2(dmpzm)2]·DMF(2·DMF). Both compounds were characterized by elemental analysis, IR, and single-crystal X-ray diffraction analysis. 1·2(MeCH)0.5 crystallizes in triclinic, space group P1 with a = 11.4552(5), b = 11.6735(3), c = 16.2278(9)A, α = 99.537(9), β = 101.986(2), γ = 118.464(13)°, V = 1775.5(3)A3, Z = 2,μ= 6.080 mm-1, Dc = 1.983 Mg/m3, T = 193(2)K, C24H35Cu3IN9OS3W, Mr = 1063.22, F(00G)= 1018, S =1.060, R = 0.0376 and wR = 0.0870. 2·DMF belongs to the orthorhombic system, space group Pmn21 with a = 22.145(4), b = 11.464(2), c = 7.7370(15)A, V = 1964.2(6)A3, Z = 2,μ = 6.865 mm-1, Dc = 2.189 Mg/m3, T = 193(2)K, C25H39Cu4I2N9OS4W, Mr= 1301.72, F(000)= 1226, R = 0.0632, wR = 0.1706 and S = 1.130. 1·2(MeCN)0.5 consists of one CuI and two [Cu(dmpzm)]+ fragments that are linked by [WOS3]2- species via six Cu-S bonds, forming a hide-like [WS3Cu3] core. 2-DMF contains a saddle-shaped [WS4Cu4] core With two iodides coordinated at two Cu centers in a cis position and two dmpzm ligands being chelated at another two Cu centers in a cis position.
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