TY - JOUR
T1 - Preparation and crystal and molecular structure of [MoO(SCH2CH2PPh2)2]
AU - Chatt, Joseph
AU - Dilworth, Jonathan R.
AU - Schmutz, James A.
AU - Zubieta, Jon A.
N1 - Funding Information:
There are nosignificant intermolecular interactions as shown in theunit-cell packing stereogram (Figure 2).The structural investigation was supported by a grant(number GM22566A) from the National Institutes ofHealth (to J , A.
Copyright:
Copyright 2007 Elsevier B.V., All rights reserved.
PY - 1979
Y1 - 1979
N2 - The title complex has been prepared by reaction of [MoO2(acac)2] (acac = pentane-2,4-dionate) with an excess of Ph2PCH2CH2SH in methanol or toluene. The oxo-group can be protonated with anhydrous HBF4 in benzene to give [Mo(OH2)(SCH2CH2PPh2) 2][BF4]2 but does not undergo condensation-type reactions with hydrazines even under forcing conditions. The complex [MoO(SCH2CH2PPh2)2] crystallises in the orthorhombic space group P212121 with four molecules in a unit cell of dimensions a = 10.263(3), b = 10.246(1), and c = 26.657(5) Å. The structure has been solved using 2 179 symmetry-independent reflections with I > 2.58σ(I) collected by counter techniques using Cu-Kα radiation. Refinement by full-matrix least squares, using anisotropic temperature factors for all non-carbon and non-hydrogen atoms, gives a final R factor of 0.063. The co-ordination polyhedron is intermediate between trigonal-bipyramidal and square-pyramidal geometries. The bond distances to Mo are Mo-O 1.733(9), Mo-S(av.) 2.360(4), and Mo-P(av.) 2.484(4) Å.
AB - The title complex has been prepared by reaction of [MoO2(acac)2] (acac = pentane-2,4-dionate) with an excess of Ph2PCH2CH2SH in methanol or toluene. The oxo-group can be protonated with anhydrous HBF4 in benzene to give [Mo(OH2)(SCH2CH2PPh2) 2][BF4]2 but does not undergo condensation-type reactions with hydrazines even under forcing conditions. The complex [MoO(SCH2CH2PPh2)2] crystallises in the orthorhombic space group P212121 with four molecules in a unit cell of dimensions a = 10.263(3), b = 10.246(1), and c = 26.657(5) Å. The structure has been solved using 2 179 symmetry-independent reflections with I > 2.58σ(I) collected by counter techniques using Cu-Kα radiation. Refinement by full-matrix least squares, using anisotropic temperature factors for all non-carbon and non-hydrogen atoms, gives a final R factor of 0.063. The co-ordination polyhedron is intermediate between trigonal-bipyramidal and square-pyramidal geometries. The bond distances to Mo are Mo-O 1.733(9), Mo-S(av.) 2.360(4), and Mo-P(av.) 2.484(4) Å.
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U2 - 10.1039/DT9790001595
DO - 10.1039/DT9790001595
M3 - Article
AN - SCOPUS:37049106636
SN - 1472-7773
SP - 1595
EP - 1599
JO - Journal of the Chemical Society, Dalton Transactions
JF - Journal of the Chemical Society, Dalton Transactions
IS - 10
ER -