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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(MeCN)0.5 crystallizes in triclinic,space group P1-with a = 11.4552(5),b = 11.6735(3),c = 16.2278(9) ,α = 99.537(9),β = 101.986(2),γ = 118.464(13)o,V = 1775.5(3)3,Z = 2,μ = 6.080 mm-1,Dc = 1.983 Mg/m3,T = 193(2) K,C24H35Cu3IN9OS3W,Mr = 1063.22,F(000) = 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) ,V = 1964.2(6)3,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 nido-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.
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 (MeCN) 0.5 crystallizes in triclinic, space group P1-with a = 11.4552 (5), b = 11.6735 (3), c = 16.2278 , β = 101.986 (2), γ = 118.464 (13) o, V = 1775.5 (3) 3, Z = 2, μ = 6.080 mm-1, Dc = 1.983 Mg / m3, T = 193 K = C24H35Cu3IN9OS3W, Mr = 1063.22, F (000) = 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 = (2), c = 7.7370 (15) , V = 1964.2 (6) 3, 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 nido-like [WS3Cu3] core.2 DMF containing 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.