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Synthesis, characterization, low-temperature (50 K) neutron diffraction structure, and reactivity of chlorodihydridotetrakis(trimethylphosphine)tantalum (III)

Journal Article · · Inorg. Chem.; (United States)
DOI:https://doi.org/10.1021/ic00262a019· OSTI ID:5572148

Dichlorodihydridotetrakis(trimethylphosphine)tantalum(IV), TaCl/sub 2/H/sub 2/(PMe/sub 3/)/sub 4/, is reduced under argon by sodium amalgam in the presence of PMe/sub 3/ to give green TaClH/sub 2/(PMe/sub 3/)/sub 4/ (1a) in 70% yield. 1a has been characterized by spectroscopy, variable-temperature /sup 1/H and /sup 31/P(/sup 1/H) NMR spectroscopy, and low-temperature (50K) neutron crystallography. In the solid state, 1a is a slightly distorted pentagonal bipyramid with two axial phosphines. The hydride ligands are coordinated in a cis configuration in the pentagonal plane with a H-Ta-H angle of 66.2 (6)/sup 0/ and Ta-H distances of 1.79 (1) and 1.80 (1) A. 1a reacts readily with Me/sub 2/PCH/sub 2/CH/sub 2/PMe/sub 2/ (dmpe) to give TaClH/sub 2/(dmpe)/sub 2/ (2) and with ethylene to give TaCL(C/sub 2/H/sub 4/)(PMe/sub 3/)/sub 4/ (3). It also reacts with dinitrogen to given the ..mu..-dinitrogen complex (TaClH/sub 2/(PMe/sub 3/)/sub 3/)/sub 2/(..mu..-N/sub 2/) (4a) and with carbon monoxide to provide TaCl(CO)/sub 3/(PMe/sub 3/)/sub 3/ (5). The latter complex has been characterized by low-temperature (-160/sup 0/C) X-ray crystallography. In the solid state, 5 is a capped (by Cl) trigonal prism with three PMe/sub 3/ ligands and one CO on the capped quadrilateral face and two CO ligands on the remaining edge. Crystal data for 1a (at 50 K) and for 5 are presented. 25 references, 5 figures, 6 tables.

Research Organization:
Univ. of Michigan, Ann Arbor
DOE Contract Number:
W-31109-ENG-38
OSTI ID:
5572148
Journal Information:
Inorg. Chem.; (United States), Journal Name: Inorg. Chem.; (United States) Vol. 26:15; ISSN INOCA
Country of Publication:
United States
Language:
English