摘要：

The reactions of Mo(CO)6, W(CO)6 and Re(CO)6Br with the ligand l-thia-4,7-diazacyclononane (C6H14N2S = L) yield crystals of LMo(CO)3 (4a), LW(CO)3 (4b) and LRe(CO)3Br (5). A n improved synthesis of L has been developed, and the structures of 4a and 5 have been determined. Crystal data: 4a, monoclinic, space group P21/n, a = 791.3(4), b - 1332.6(4), c = 1149.2(6) pm, β - 98.96(4)°, Z = 4.1841 reflexions, R = 0.045. 5, orthorhombic, space group Pbca, a = 1413.4(5), b = 1398.0(5), c = 1409.5(5) pm, Z = 8.2619 reflexions, R = 0.038. Both crystals contain pseudooctahedral LM(CO)3 moieties, with facial coordination of the CO molecules. The Re - N bond lengths (average 220.3(4) pm) are rather short. The structure of L 'Mo(CO)3 (3) with the acyclic ligand 1,7-diaza-4-thiaheptane (C4H10N2S = L') was also determined. Crystal data: monoclinic, space group P21/c, a = 682.8(2), b = 1213.0(3), c = 1253.0(3), β = 99.74°, Z = 4.1889 reflexions, R = 0.023.

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