Joint x-ray and neutron diffraction structure analysis of [(μ-H) 3Re 3(CO) 8{(EtO) 2POP(OEt) 2} 2

Abstract

The compound [(μ-H) 3Re 3(CO) 8{(EtO) 2POP(OEt) 2} 2] crystallises in the monoclinic space group P2 1/ c with a 18.053(6), b 16.211(5), c 14.800(3) Å, β = 102.41(2)°, and Z = 4. Simultaneous refinement of a single parameter set to fit 3212 X-Ray (sin θ/λ) > 0.352 Å −1 and 1480 neutron data has led to final weighted residuals R w ( F) of 0.096 (X-Ray) and 0.095 (neutron). The molecule exhibits noncrystallographic C 2 symmetry, with two edges of the Re 3 triangle bridged by (OEt) 2POP(OEt) 2 ligands. The hydride ligands lie close to the trimetal plane with each hydride bridging an ReRe vector. Average molecular parameters involving the hydride ligands are ReH 1.812(17), ReRe 3.282(17) Å, ReHRe 130(3) and HReH 107.6(27)/dg. All eight carbonyl ligands are terminal, the ligand polyhedron being derived from that in H 3Re 3(CO) 12 by substitution of four axial carbonyls by two bidentate phosphite ligands.