Abstract
The quadruply bonded heterobimetallic complex MoWCl[sub 4](dmpm)[sub 2] (1) and the homobimetallic complexes Mo[sub 2]X[sub 4](dmpm)[sub 2] (X = Br, I,) were synthesized and their structures determined. The crystals of compound 1 exhibit the typical disorder for heteronuclear systems, namely, the random orientation of the M-M[prime] vector, with each metal atom appearing as 50% Mo and 50% W. The structural refinement in the space group P4 resulted in lower residuals, with R = 0.048 and R[sub W] = 0.067, than in the space group P4/m. For complexes 2 and 3, crystals obtained from THF solutions are monoclinic, with space groups P2[sub 1]/c and P2[sub 1]/n for 2 and 3, respectively. The quadruple bond distances are 2.193(2), 2.1271(8), and 2.132(2) [angstrom] for 1, 2, and 3, respectively. In addition, each complex has been characterized using UV-visible, [sup 31]P[[sup 1]H] NMR, and [sup 1]H NMR spectroscopies. The average magnetic anisotropy of the Mo-Mo quadruple bond in complexes 2 and 3 has been calculated from [sup 1]H NMR data as [minus]4450 [times] 10[sup [minus]36] m[sup 3] molecule[sup [minus]1]. The crystal structures of complexes 1-3 are fully described, and their crystallographic data are as follows: (1) space group P4 with a = b =more » 9.083(2) [angstrom], c = 8.092(2) [angstrom], V = 667.5(5) [angstrom][sup 3], and Z = 2; (2) space group P2[sub 1]/n with a = 8.694(1) [angstrom], b = 8.695(2) [angstrom], c = 15.369(2) [angstrom], [beta] = 100.70(1)[degrees], V = 1141.6(6) [angstrom][sup 3], and Z = 2; (3) space group P2[sub 1]/c with a = 9.076(2) [angstrom], b = 16.813(7) [angstrom], c = 16.654(5) [angstrom], [beta] = 102.4(1)[degrees], V = 2481(4) [angstrom][sup 3], and Z = 4.« less
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