Neutron diffraction study of HFeCo/sub 3/(CO)/sub 9/(P(OCH/sub 3/)/sub 3/)/sub 3/, a metal cluster complex with a triply bridging hydride ligand

We wish to report the first accurate neutron diffraction study of a transition metal structure with a triply bridging hydride ligand, the cluster HFeCo/sub 3/(CO)/sub 9/(P(OCH/sub 3/)/sub 3/)/sub 3/. The compound crystallizes in the space group P2/sub 1//c, Z = 4. The cell constants at 90 K are a = 15.957 (8) A, b = 10.611 (5) A/sub 9/ c = 18.383 (9) A, ..beta.. = 98.70 (2)/sup 0/. The structure was refined, based on the measured intensities of 8229 reflections; the final discrepancy factors for all reflections are R/sub F/sup 2// = 0.087, R/sub wF/sup 2// = 0.066. The four metal atoms form a tetrahedron with the apical Fe atom additionally bonded to three terminal carbonyl groups. Each Co atom is further bonded to one terminal and two bridging carbonyl ligands, as well as one phosphite group and the hydride ligand. The hydride ligand is located outside the metal cluster, 0.978 (3) A from the Co/sub 3/ face. This result confirms that of an earlier x-ray investigation by Huie, Knobler, and Kaesz. The Co--H distances are 1.724 (3), 1.731 (3), and 1.728 (3) A, and Co--H--Co angles are 92.1 (1), 91.7 (1), and 91.5 (1)/sup 0/.