TY - JOUR
T1 - Iron-molybdenum and iron-tungsten sulphido clusters containing hydrazido(2-) ligands. The synthesis and X-ray crystal and molecular structure of [{Fe(CO)3(μ3-S)}2Mo(NNMe2)2(PPh3)](Fe-Fe) · CH2Cl2
AU - Bishop, Peter T.
AU - Dilworth, Jonathan R.
AU - Morton, Stephen
AU - Zubieta, Jon A.
N1 - Copyright:
Copyright 2014 Elsevier B.V., All rights reserved.
PY - 1988/3/1
Y1 - 1988/3/1
N2 - Treatment of [MCl(NNRR′2(PPh3)2]Cl (M = Mo or W; R,R′ = Me2 or Me, Ph) with [{Fe(CO)3(μ2-SLi)}2](Fe-Fe) gives the trinuclear clusters [{Fe(CO)3(μ3-S)}2M(NNRR′)2(PPh3)](Fe-Fe) in good yield. The X-ray crystal structure of [{Fe(CO)3(μ3-S)}2Mo(NNMe2)2(PPh3)] · CH2Cl2 (space group P212121,; a 15.089(4), b 15.569(5), c 16.983(4) Å; Z = 4; R = 0.061 for 1915 observed reflections) confirms the absence of iron-molybdenum bonding, and the complexes generally show similar Mössbauer parameters. Analogous coordination environments at molybdenum are obtained in [Mo(NNMePh)2(C7H6S2)(PPh3)] (C7H6(SH)2 = 3,4-dimercaptotoluene) and in the dimeric species [{Mo(NNMePh)2-(μ2-S)(PPh3)}2]. These are prepared by reaction of [MoCl(NNMePh)2(PPh3)2]Cl with 3,4-dimercaptotoluene and S(SiMe3)2, respectively.
AB - Treatment of [MCl(NNRR′2(PPh3)2]Cl (M = Mo or W; R,R′ = Me2 or Me, Ph) with [{Fe(CO)3(μ2-SLi)}2](Fe-Fe) gives the trinuclear clusters [{Fe(CO)3(μ3-S)}2M(NNRR′)2(PPh3)](Fe-Fe) in good yield. The X-ray crystal structure of [{Fe(CO)3(μ3-S)}2Mo(NNMe2)2(PPh3)] · CH2Cl2 (space group P212121,; a 15.089(4), b 15.569(5), c 16.983(4) Å; Z = 4; R = 0.061 for 1915 observed reflections) confirms the absence of iron-molybdenum bonding, and the complexes generally show similar Mössbauer parameters. Analogous coordination environments at molybdenum are obtained in [Mo(NNMePh)2(C7H6S2)(PPh3)] (C7H6(SH)2 = 3,4-dimercaptotoluene) and in the dimeric species [{Mo(NNMePh)2-(μ2-S)(PPh3)}2]. These are prepared by reaction of [MoCl(NNMePh)2(PPh3)2]Cl with 3,4-dimercaptotoluene and S(SiMe3)2, respectively.
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U2 - 10.1016/0022-328X(88)89092-2
DO - 10.1016/0022-328X(88)89092-2
M3 - Article
AN - SCOPUS:0000539282
SN - 0022-328X
VL - 341
SP - 373
EP - 380
JO - Journal of Organometallic Chemistry
JF - Journal of Organometallic Chemistry
IS - 1-3
ER -