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Preparation and Characterization of a Heteronuclear μ‐Alkyne Complex; X‐Ray Crystal Structure of MoCo(CO) 4 (PPh 3 ){μ‐HCCSiMe 3 )(η 5 ‐C 5 H 5 )
Author(s) -
Hong FungE,
Hung ChangKu,
Lin ChuChieh
Publication year - 1997
Publication title -
journal of the chinese chemical society
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.329
H-Index - 45
eISSN - 2192-6549
pISSN - 0009-4536
DOI - 10.1002/jccs.199700007
Subject(s) - chemistry , acetylene , triphenylphosphine , heteronuclear molecule , triclinic crystal system , crystal structure , crystallography , alkyne , molecule , x ray crystallography , ligand (biochemistry) , tetrahydrofuran , phenylacetylene , nuclear magnetic resonance spectroscopy , stereochemistry , diffraction , solvent , organic chemistry , physics , catalysis , biochemistry , receptor , optics
Reaction of MoCo(CO) 5 (PPh 3 ) 2 (η 5 ‐C 5 H 5 ) (1a) with trimethylsilylacetylene in tetrahydrofuran at 58° C yielded two acetylene bridged heterobimetallic compounds, MoCo(CO) 4 (PPh 3 ){μ‐HCCSiMe 3 }(η 5 ‐C 5 H 5 ) (4) and MoCo (CO) 5 {μ‐HCCSiMe 3 }(η 5 ‐C 5 H 5 )(5). (4) was characterized by mass, infrared, 1 H, 13 C and 31 P NMR spectra. The X‐ray crystal structure of (4) was determined:triclinic, P‐1, a=8.821(1) Å, b=11.315(3) Å, c=17.029(2) Å, α=70.73(1)°, β=78 .72(1)°, γ=86.10(2)°,V =1573.4(6) Å 3 , Z=2, R = 3.92%,R w = 6.06% for 4285 (F > 4σ (F)) observed reflections. The core of this molecule is a quasi‐tetrahedron containing Mo, Co and two carbons of acetylene. The triphenylphosphine ligand is attached to cobalt rather than molybdenum center.