The effects of steric hindrance on the chemistry of rhenium and molybdenum nitrosyl thiolato-complexes. The structures of[Mo(SC6H2Pr3i)3(NH3(NO)] and [Re(SC6H3Pr2i)4(NO)]

P. J. Blower; P. T. Bishop; J. R. Dilworth; T. C. Hsieh; J. Hutchinson; T. Nicholson; Jon Zubieta

doi:10.1016/S0020-1693(00)85626-1

The effects of steric hindrance on the chemistry of rhenium and molybdenum nitrosyl thiolato-complexes. The structures of[Mo(SC₆H₂Pr₃ⁱ)₃(NH₃(NO)] and [Re(SC₆H₃Pr₂ⁱ)₄(NO)]

P. J. Blower, P. T. Bishop, J. R. Dilworth, T. C. Hsieh, J. Hutchinson, T. Nicholson, Jon Zubieta

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

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Abstract

The Re(II) nitrosyl complex [ReCl₂(OMe)(NO)(PPh₃)2] reacts with excess 2,6-Pr₂ⁱC₆H₃S^-(DIPT^-) in methanol to give the Re(III) complex [Re(DIPT)₄(NO)] (I) whereas thiophenolate gives a thiolatobridged Re(II) dimer. Crystal data for(I): crystallizes in the orthorhombic space group Pbca, a = 13.218(6) Å, b = 19.534(9) Å, c = 38.115(13) Å, V = 9841.3(6) Å³ to give D_calc = 1.35 g cm^-3 for Z = 8. Structure solution and refinement are based on 3047 reflections with I_o>3σ|I_o| and yielded a final R value of 0.064. The overall geometry about Re is trigonal bipyramidal with an apical NO group with a nearly linear ReNO system (ReNO, 173.6(14)°). The polymeric species '{Mo(NO)(NH₂O)}_n' reacts with excess 2,4,6-Pr₃ⁱC₆H₂S^-(TIPT^- to give[Mo(TIPT)₃(NH₃)(NO)]·C₅H₁₂ (II) (C₅H₁₂ = n-pentane) whereas thiophenolate anion gives [Mo(SPh)₄(NO)]^-. Crystal data for (II): space group P2₁/n with a = 10.477(3) Å, b = 26.359(5) Å, c = 20.124(4) Å, β = 87.21(1)°, with V = 5550.9(12) Å³ to give D_calc = 1.05 g cm^-3 for Z = 4. Structure refinement was based on 1040 reflections with I_o>3σ|I_o| and yielded a final R value of 0.079. The geometry about Mo is again trigonal bipyramidal with apical NO and NH₃ groups and again an essentially linear MoNO system (MNO = 174.2(3)°).

Original language	English (US)
Pages (from-to)	63-65
Number of pages	3
Journal	Inorganica Chimica Acta
Volume	101
Issue number	1
DOIs	https://doi.org/10.1016/S0020-1693(00)85626-1
State	Published - Jun 17 1985
Externally published	Yes

ASJC Scopus subject areas

Physical and Theoretical Chemistry
Inorganic Chemistry
Materials Chemistry

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10.1016/S0020-1693(00)85626-1

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Blower, P. J., Bishop, P. T., Dilworth, J. R., Hsieh, T. C., Hutchinson, J., Nicholson, T., & Zubieta, J. (1985). The effects of steric hindrance on the chemistry of rhenium and molybdenum nitrosyl thiolato-complexes. The structures of[Mo(SC₆H₂Pr₃ⁱ)₃(NH₃(NO)] and [Re(SC₆H₃Pr₂ⁱ)₄(NO)]. Inorganica Chimica Acta, 101(1), 63-65. https://doi.org/10.1016/S0020-1693(00)85626-1

@article{921a7d2c482c49ff9ca80912b22f7eb1,

title = "The effects of steric hindrance on the chemistry of rhenium and molybdenum nitrosyl thiolato-complexes. The structures of[Mo(SC6H2Pr3i)3(NH3(NO)] and [Re(SC6H3Pr2i)4(NO)]",

abstract = "The Re(II) nitrosyl complex [ReCl2(OMe)(NO)(PPh3)2] reacts with excess 2,6-Pr2iC6H3S-(DIPT-) in methanol to give the Re(III) complex [Re(DIPT)4(NO)] (I) whereas thiophenolate gives a thiolatobridged Re(II) dimer. Crystal data for(I): crystallizes in the orthorhombic space group Pbca, a = 13.218(6) {\AA}, b = 19.534(9) {\AA}, c = 38.115(13) {\AA}, V = 9841.3(6) {\AA}3 to give Dcalc = 1.35 g cm-3 for Z = 8. Structure solution and refinement are based on 3047 reflections with Io>3σ|Io| and yielded a final R value of 0.064. The overall geometry about Re is trigonal bipyramidal with an apical NO group with a nearly linear ReNO system (ReNO, 173.6(14)°). The polymeric species '{Mo(NO)(NH2O)}n' reacts with excess 2,4,6-Pr3iC6H2S-(TIPT- to give[Mo(TIPT)3(NH3)(NO)]·C5H12 (II) (C5H12 = n-pentane) whereas thiophenolate anion gives [Mo(SPh)4(NO)]-. Crystal data for (II): space group P21/n with a = 10.477(3) {\AA}, b = 26.359(5) {\AA}, c = 20.124(4) {\AA}, β = 87.21(1)°, with V = 5550.9(12) {\AA}3 to give Dcalc = 1.05 g cm-3 for Z = 4. Structure refinement was based on 1040 reflections with Io>3σ|Io| and yielded a final R value of 0.079. The geometry about Mo is again trigonal bipyramidal with apical NO and NH3 groups and again an essentially linear MoNO system (MNO = 174.2(3)°).",

author = "Blower, {P. J.} and Bishop, {P. T.} and Dilworth, {J. R.} and Hsieh, {T. C.} and J. Hutchinson and T. Nicholson and Jon Zubieta",

year = "1985",

month = jun,

day = "17",

doi = "10.1016/S0020-1693(00)85626-1",

language = "English (US)",

volume = "101",

pages = "63--65",

journal = "Inorganica Chimica Acta",

issn = "0020-1693",

publisher = "Elsevier",

number = "1",

}

TY - JOUR

T1 - The effects of steric hindrance on the chemistry of rhenium and molybdenum nitrosyl thiolato-complexes. The structures of[Mo(SC6H2Pr3i)3(NH3(NO)] and [Re(SC6H3Pr2i)4(NO)]

AU - Blower, P. J.

AU - Bishop, P. T.

AU - Dilworth, J. R.

AU - Hsieh, T. C.

AU - Hutchinson, J.

AU - Nicholson, T.

AU - Zubieta, Jon

PY - 1985/6/17

Y1 - 1985/6/17

N2 - The Re(II) nitrosyl complex [ReCl2(OMe)(NO)(PPh3)2] reacts with excess 2,6-Pr2iC6H3S-(DIPT-) in methanol to give the Re(III) complex [Re(DIPT)4(NO)] (I) whereas thiophenolate gives a thiolatobridged Re(II) dimer. Crystal data for(I): crystallizes in the orthorhombic space group Pbca, a = 13.218(6) Å, b = 19.534(9) Å, c = 38.115(13) Å, V = 9841.3(6) Å3 to give Dcalc = 1.35 g cm-3 for Z = 8. Structure solution and refinement are based on 3047 reflections with Io>3σ|Io| and yielded a final R value of 0.064. The overall geometry about Re is trigonal bipyramidal with an apical NO group with a nearly linear ReNO system (ReNO, 173.6(14)°). The polymeric species '{Mo(NO)(NH2O)}n' reacts with excess 2,4,6-Pr3iC6H2S-(TIPT- to give[Mo(TIPT)3(NH3)(NO)]·C5H12 (II) (C5H12 = n-pentane) whereas thiophenolate anion gives [Mo(SPh)4(NO)]-. Crystal data for (II): space group P21/n with a = 10.477(3) Å, b = 26.359(5) Å, c = 20.124(4) Å, β = 87.21(1)°, with V = 5550.9(12) Å3 to give Dcalc = 1.05 g cm-3 for Z = 4. Structure refinement was based on 1040 reflections with Io>3σ|Io| and yielded a final R value of 0.079. The geometry about Mo is again trigonal bipyramidal with apical NO and NH3 groups and again an essentially linear MoNO system (MNO = 174.2(3)°).

AB - The Re(II) nitrosyl complex [ReCl2(OMe)(NO)(PPh3)2] reacts with excess 2,6-Pr2iC6H3S-(DIPT-) in methanol to give the Re(III) complex [Re(DIPT)4(NO)] (I) whereas thiophenolate gives a thiolatobridged Re(II) dimer. Crystal data for(I): crystallizes in the orthorhombic space group Pbca, a = 13.218(6) Å, b = 19.534(9) Å, c = 38.115(13) Å, V = 9841.3(6) Å3 to give Dcalc = 1.35 g cm-3 for Z = 8. Structure solution and refinement are based on 3047 reflections with Io>3σ|Io| and yielded a final R value of 0.064. The overall geometry about Re is trigonal bipyramidal with an apical NO group with a nearly linear ReNO system (ReNO, 173.6(14)°). The polymeric species '{Mo(NO)(NH2O)}n' reacts with excess 2,4,6-Pr3iC6H2S-(TIPT- to give[Mo(TIPT)3(NH3)(NO)]·C5H12 (II) (C5H12 = n-pentane) whereas thiophenolate anion gives [Mo(SPh)4(NO)]-. Crystal data for (II): space group P21/n with a = 10.477(3) Å, b = 26.359(5) Å, c = 20.124(4) Å, β = 87.21(1)°, with V = 5550.9(12) Å3 to give Dcalc = 1.05 g cm-3 for Z = 4. Structure refinement was based on 1040 reflections with Io>3σ|Io| and yielded a final R value of 0.079. The geometry about Mo is again trigonal bipyramidal with apical NO and NH3 groups and again an essentially linear MoNO system (MNO = 174.2(3)°).

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U2 - 10.1016/S0020-1693(00)85626-1

DO - 10.1016/S0020-1693(00)85626-1

M3 - Article

AN - SCOPUS:21244448278

SN - 0020-1693

VL - 101

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EP - 65

JO - Inorganica Chimica Acta

JF - Inorganica Chimica Acta

IS - 1

ER -

The effects of steric hindrance on the chemistry of rhenium and molybdenum nitrosyl thiolato-complexes. The structures of[Mo(SC₆H₂Pr₃ⁱ)₃(NH₃(NO)] and [Re(SC₆H₃Pr₂ⁱ)₄(NO)]

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