Crystals of fac-[dimethylbis(1-pyrazolyl)gallato-N,N′](triphenylphosphine)tricarbonylrhenium(I) are triclinic, a = 9.479(2), b = 16.258(4), c = 20.412(6) Å, α = 110.06(1), β = 95.46(1), γ = 92.65(2)°, Z = 4, space group [Formula: see text] The structure was solved by conventional heavy-atom methods and was refined by full-matrix least-squares procedures to R = 0.027 and Rw = 0.031 for 5965 reflections with I ≥ 3σ(I). The two crystallographically independent molecules have nearly identical structures. The coordination about Re is distorted fac-octahedral with mean bond lengths: Re—P = 2.538(4), Re—N = 2.201(5), Re—CO(trans to P) = 1.931(1), and Re—CO(trans to N) = 1.913(9) Å. The ReGaN4 chelate rings have twisted boat conformations with cross-ring [Formula: see text] separations of 3.9396(7) and 3.8981(8) Å.
