A convenient route to complexes of the type [MoO(SR)4]-(R = aryl) and [MoO{S(CH2)nS}2]- (n = 2 or 3) preparation and crystal structure of [PPh4][Mo(NNMe2)O(SC6H5) 3]·(C2H5)2O

R. J. Burt; J. R. Dilworth; G. J. Leigh; J. A. Zubieta

doi:10.1039/DT9820002295

A convenient route to complexes of the type [MoO(SR)₄]^-(R = aryl) and [MoO{S(CH₂)_nS}₂]^- (n = 2 or 3) preparation and crystal structure of [PPh₄][Mo(NNMe₂)O(SC₆H₅) ₃]·(C₂H₅)₂O

R. J. Burt, J. R. Dilworth, G. J. Leigh, J. A. Zubieta

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Abstract

The complexes [MoO(SR)₄]^- (R = aryl) and [MoO{S(CH₂)_nS}₂]^- (n = 2 or 3) can be prepared by reaction of an Mo^VI butanediolato-complex with thiolate anion in methanol. The complexes [MoO(SPh)₄]^- react with R′₂NNH₂ [R′₂ = Me₂ or (CH₂)₅] in refluxing CH₃CN to give [Mo(NNR′₂)O(SPh)₃]^-. Crystal Data for [PPh₄] [Mo(NNMe₂)O(SC₆H₅)₃]·(C ₂H₅)₂O: space group Pbca, a = 12.789(4), b = 19.375(3), c = 36.941(3) Å, Z = 8.3 225 Independent reflections with I > 3σ(I) gave R = 0.076. The geometry is essentially square-pyramidal with an apical oxo-group and the NNMe₂ group in the basal plane. Although the MO-N and N-N distances of 1.821(9) and 1.292(14) Å respectively are analogous to other hydrazido(2-) complexes, the Mo-N-NMe₂ system is anomalously bent with MO-N-N = 152.5(10)°.

Original language	English (US)
Pages (from-to)	2295-2298
Number of pages	4
Journal	Journal of the Chemical Society, Dalton Transactions
Issue number	11
DOIs	https://doi.org/10.1039/DT9820002295
State	Published - 1982
Externally published	Yes

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A convenient route to complexes of the type [MoO(SR)₄]^-(R = aryl) and [MoO{S(CH₂)_nS}₂]^- (n = 2 or 3) preparation and crystal structure of [PPh₄][Mo(NNMe₂)O(SC₆H₅) ₃]·(C₂H₅)₂O. / Burt, R. J.; Dilworth, J. R.; Leigh, G. J. et al.
In: Journal of the Chemical Society, Dalton Transactions, No. 11, 1982, p. 2295-2298.

Research output: Contribution to journal › Article › peer-review

@article{9116463a196e401db6b8eda3053706e7,

title = "A convenient route to complexes of the type [MoO(SR)4]-(R = aryl) and [MoO{S(CH2)nS}2]- (n = 2 or 3) preparation and crystal structure of [PPh4][Mo(NNMe2)O(SC6H5) 3]·(C2H5)2O",

abstract = "The complexes [MoO(SR)4]- (R = aryl) and [MoO{S(CH2)nS}2]- (n = 2 or 3) can be prepared by reaction of an MoVI butanediolato-complex with thiolate anion in methanol. The complexes [MoO(SPh)4]- react with R′2NNH2 [R′2 = Me2 or (CH2)5] in refluxing CH3CN to give [Mo(NNR′2)O(SPh)3]-. Crystal Data for [PPh4] [Mo(NNMe2)O(SC6H5)3]·(C 2H5)2O: space group Pbca, a = 12.789(4), b = 19.375(3), c = 36.941(3) {\AA}, Z = 8.3 225 Independent reflections with I > 3σ(I) gave R = 0.076. The geometry is essentially square-pyramidal with an apical oxo-group and the NNMe2 group in the basal plane. Although the MO-N and N-N distances of 1.821(9) and 1.292(14) {\AA} respectively are analogous to other hydrazido(2-) complexes, the Mo-N-NMe2 system is anomalously bent with MO-N-N = 152.5(10)°.",

author = "Burt, {R. J.} and Dilworth, {J. R.} and Leigh, {G. J.} and Zubieta, {J. A.}",

year = "1982",

doi = "10.1039/DT9820002295",

language = "English (US)",

pages = "2295--2298",

journal = "Journal of the Chemical Society, Dalton Transactions",

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T1 - A convenient route to complexes of the type [MoO(SR)4]-(R = aryl) and [MoO{S(CH2)nS}2]- (n = 2 or 3) preparation and crystal structure of [PPh4][Mo(NNMe2)O(SC6H5) 3]·(C2H5)2O

AU - Burt, R. J.

AU - Dilworth, J. R.

AU - Leigh, G. J.

AU - Zubieta, J. A.

PY - 1982

Y1 - 1982

N2 - The complexes [MoO(SR)4]- (R = aryl) and [MoO{S(CH2)nS}2]- (n = 2 or 3) can be prepared by reaction of an MoVI butanediolato-complex with thiolate anion in methanol. The complexes [MoO(SPh)4]- react with R′2NNH2 [R′2 = Me2 or (CH2)5] in refluxing CH3CN to give [Mo(NNR′2)O(SPh)3]-. Crystal Data for [PPh4] [Mo(NNMe2)O(SC6H5)3]·(C 2H5)2O: space group Pbca, a = 12.789(4), b = 19.375(3), c = 36.941(3) Å, Z = 8.3 225 Independent reflections with I > 3σ(I) gave R = 0.076. The geometry is essentially square-pyramidal with an apical oxo-group and the NNMe2 group in the basal plane. Although the MO-N and N-N distances of 1.821(9) and 1.292(14) Å respectively are analogous to other hydrazido(2-) complexes, the Mo-N-NMe2 system is anomalously bent with MO-N-N = 152.5(10)°.

AB - The complexes [MoO(SR)4]- (R = aryl) and [MoO{S(CH2)nS}2]- (n = 2 or 3) can be prepared by reaction of an MoVI butanediolato-complex with thiolate anion in methanol. The complexes [MoO(SPh)4]- react with R′2NNH2 [R′2 = Me2 or (CH2)5] in refluxing CH3CN to give [Mo(NNR′2)O(SPh)3]-. Crystal Data for [PPh4] [Mo(NNMe2)O(SC6H5)3]·(C 2H5)2O: space group Pbca, a = 12.789(4), b = 19.375(3), c = 36.941(3) Å, Z = 8.3 225 Independent reflections with I > 3σ(I) gave R = 0.076. The geometry is essentially square-pyramidal with an apical oxo-group and the NNMe2 group in the basal plane. Although the MO-N and N-N distances of 1.821(9) and 1.292(14) Å respectively are analogous to other hydrazido(2-) complexes, the Mo-N-NMe2 system is anomalously bent with MO-N-N = 152.5(10)°.

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A convenient route to complexes of the type [MoO(SR)₄]^-(R = aryl) and [MoO{S(CH₂)_nS}₂]^- (n = 2 or 3) preparation and crystal structure of [PPh₄][Mo(NNMe₂)O(SC₆H₅) ₃]·(C₂H₅)₂O

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