摘要:
The gallium phosphide [(Me3CCH2)Ga(PPh2)2]2 has been prepared from [(Me3CCH2)ClGaPPh2]3 and Li(CMe3) in an Et2O/C6H6 mixture at 0-degrees-C and fully characterized by elemental analyses, physical ProPerties, H-1 NMR, P-31 NMR, and IR spectroscopic data, and an X-ray structural study. The identity of the gallium Phosphide was confirmed by its independent synthesis from [(Me3CCH2)BrGaPPh273 and KPPh2 in Et2O/C6H6. The dimeric molecule crystallizes in the monoclinic spacegroup P1BAR with cell dimensions of a = 10.106 (2) angstrom, b = 11.146 (6) angstrom, c = 12.266 (2) angstrom, alpha = 93.91 (2)-degrees, beta = 101.39 (1)-degrees, gamma = 95.81 (4)-degrees, V = 1342.0 angstrom3, and Z = 1. Diffraction data were collected on an Enraf-Nonius CAD-4 diffractometer, and the structure was refined to R = 3.8% and R(w) - 3.8% for those 3561 unique data with F0 greater-than-or-equal-to 5sigma(F0). The four-membered Ga2P2 ring has a planar conformation. The neopentyl groups are arranged trans to each other across the ring. The bridging Ga-P bond distances are 2.4568 (9) and 2.4689 (9) angstrom. The terminal Ga-P bond distance is 2.351 (1) angstrom.