Abstract
The chemistry leading to the isolation of Mo 3HI 7L 3 compounds has been reexamined. Although yields of the species with L = THF could not be improved, crystalline samples of compounds with L = PPh 3 ( 1) and PEt 3 ( 2) have been obtained and characterized by X-ray crystallography and 1H NMR spectra. The NMR spectra (1,3,3,1 quartets for 1H) provide conclusive evidence for the presence of the μ 3-H ligand. The principal crystallographic data are: ( 1): orthorhombic space group Pnma, a = 20.726(3), b = 21.704(1), c = 20.05(1)A˚; V = 9020A˚ 3; Z = 4; d calc, 1.672 g cm −3; R = 0.0361, R w = 0.053 3 for 423 parameters and 4935 observed data [ F o 2ρ3σ( F o 2]. 2: orthorhombic space group Pbca, a = 20.877(8), b = 16.951(5), c = 24.007(4)A˚; V = 8495A˚ 3; Z = 8; d calc = 2.508 g cm −3; R = 0.0343, R w = 0.0495 for 296 parameters and 4655 observed data [ F o 2 > 3σ( F o 2]. NMR ( 1H in C 6D 6) data: ( 1) δ = −5.01, 2 J(HP) = 36 Hz; ( 2) δ = −2.26, 2 J(HP) = 39 Hz.
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