Mononuclear oxo- and sulfidomolybdenum(IV) complexes

Syntheses and crystal structures of {HB(Me2C3N2H)3}MoE(S 2CNEt2) (E = O, S) and related complexes

Charles G. Young, Sue A Roberts, Richard B. Ortega, John H. Enemark

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Abstract

The syntheses, structures, and properties of mononuclear oxo- and sulfidomolybdenum(IV) complexes with hydrotris(3,5-dimethyl-1-pyrazolyl)borate, HB(Me2pz)3-, and dithiocarbamate ligands are described. The reactions of MoO-(S2CNR2)2 (R = Me, Et, n-Pr, n-Bu) with K{HB(Me2pz)3} in refluxing toluene yield the green, diamagnetic, air-stable complexes {HB(Me2pz)3}MoO(S2CNR2). The complex {HB(Me2pz)3}MoO(S2CNEt2) crystallizes in the monoclinic space group P21/c with a - 8.303 (2) Å, b = 21.710 (4) Å, c = 14.475 (3) Å, β = 100.75 (2)°, Z = 4. The molybdenum atom is in a distorted octahedral coordination environment composed of fac-tridentate HB(Me2pz)31, terminal oxo (Mo=O = 1.669 (3) Å), and bidentate S2CNEt2- ligands. The reaction of these oxo complexes with boron sulfide in dichloromethane yields the gold-yellow, diamagnetic sulfido analogues {HB(Me2pz)3}MoS(S2CNR2). The compound {HB(Me2pz)3}MoS(S2CNEt 2)·CH2Cl2 crystallizes in the orthorhombic space group P212121 with a = 7.967 (3) Å, b = 14.314 (5) Å, c = 26.15 (1) Å, Z = 4. The coordination geometry is similar to that of the oxo analogue, with Mo=S = 2.129 (2) Å.

Original languageEnglish (US)
Pages (from-to)2938-2946
Number of pages9
JournalJournal of the American Chemical Society
Volume109
Issue number10
StatePublished - 1987

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Crystal structure
Ligands
Borates
Boron
Molybdenum
Methylene Chloride
Dichloromethane
Toluene
Sulfides
Gold
Air
Atoms
Geometry
HB-compound

ASJC Scopus subject areas

  • Chemistry(all)

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Mononuclear oxo- and sulfidomolybdenum(IV) complexes : Syntheses and crystal structures of {HB(Me2C3N2H)3}MoE(S 2CNEt2) (E = O, S) and related complexes. / Young, Charles G.; Roberts, Sue A; Ortega, Richard B.; Enemark, John H.

In: Journal of the American Chemical Society, Vol. 109, No. 10, 1987, p. 2938-2946.

Research output: Contribution to journalArticle

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title = "Mononuclear oxo- and sulfidomolybdenum(IV) complexes: Syntheses and crystal structures of {HB(Me2C3N2H)3}MoE(S 2CNEt2) (E = O, S) and related complexes",
abstract = "The syntheses, structures, and properties of mononuclear oxo- and sulfidomolybdenum(IV) complexes with hydrotris(3,5-dimethyl-1-pyrazolyl)borate, HB(Me2pz)3-, and dithiocarbamate ligands are described. The reactions of MoO-(S2CNR2)2 (R = Me, Et, n-Pr, n-Bu) with K{HB(Me2pz)3} in refluxing toluene yield the green, diamagnetic, air-stable complexes {HB(Me2pz)3}MoO(S2CNR2). The complex {HB(Me2pz)3}MoO(S2CNEt2) crystallizes in the monoclinic space group P21/c with a - 8.303 (2) {\AA}, b = 21.710 (4) {\AA}, c = 14.475 (3) {\AA}, β = 100.75 (2)°, Z = 4. The molybdenum atom is in a distorted octahedral coordination environment composed of fac-tridentate HB(Me2pz)31, terminal oxo (Mo=O = 1.669 (3) {\AA}), and bidentate S2CNEt2- ligands. The reaction of these oxo complexes with boron sulfide in dichloromethane yields the gold-yellow, diamagnetic sulfido analogues {HB(Me2pz)3}MoS(S2CNR2). The compound {HB(Me2pz)3}MoS(S2CNEt 2)·CH2Cl2 crystallizes in the orthorhombic space group P212121 with a = 7.967 (3) {\AA}, b = 14.314 (5) {\AA}, c = 26.15 (1) {\AA}, Z = 4. The coordination geometry is similar to that of the oxo analogue, with Mo=S = 2.129 (2) {\AA}.",
author = "Young, {Charles G.} and Roberts, {Sue A} and Ortega, {Richard B.} and Enemark, {John H.}",
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T2 - Syntheses and crystal structures of {HB(Me2C3N2H)3}MoE(S 2CNEt2) (E = O, S) and related complexes

AU - Young, Charles G.

AU - Roberts, Sue A

AU - Ortega, Richard B.

AU - Enemark, John H.

PY - 1987

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N2 - The syntheses, structures, and properties of mononuclear oxo- and sulfidomolybdenum(IV) complexes with hydrotris(3,5-dimethyl-1-pyrazolyl)borate, HB(Me2pz)3-, and dithiocarbamate ligands are described. The reactions of MoO-(S2CNR2)2 (R = Me, Et, n-Pr, n-Bu) with K{HB(Me2pz)3} in refluxing toluene yield the green, diamagnetic, air-stable complexes {HB(Me2pz)3}MoO(S2CNR2). The complex {HB(Me2pz)3}MoO(S2CNEt2) crystallizes in the monoclinic space group P21/c with a - 8.303 (2) Å, b = 21.710 (4) Å, c = 14.475 (3) Å, β = 100.75 (2)°, Z = 4. The molybdenum atom is in a distorted octahedral coordination environment composed of fac-tridentate HB(Me2pz)31, terminal oxo (Mo=O = 1.669 (3) Å), and bidentate S2CNEt2- ligands. The reaction of these oxo complexes with boron sulfide in dichloromethane yields the gold-yellow, diamagnetic sulfido analogues {HB(Me2pz)3}MoS(S2CNR2). The compound {HB(Me2pz)3}MoS(S2CNEt 2)·CH2Cl2 crystallizes in the orthorhombic space group P212121 with a = 7.967 (3) Å, b = 14.314 (5) Å, c = 26.15 (1) Å, Z = 4. The coordination geometry is similar to that of the oxo analogue, with Mo=S = 2.129 (2) Å.

AB - The syntheses, structures, and properties of mononuclear oxo- and sulfidomolybdenum(IV) complexes with hydrotris(3,5-dimethyl-1-pyrazolyl)borate, HB(Me2pz)3-, and dithiocarbamate ligands are described. The reactions of MoO-(S2CNR2)2 (R = Me, Et, n-Pr, n-Bu) with K{HB(Me2pz)3} in refluxing toluene yield the green, diamagnetic, air-stable complexes {HB(Me2pz)3}MoO(S2CNR2). The complex {HB(Me2pz)3}MoO(S2CNEt2) crystallizes in the monoclinic space group P21/c with a - 8.303 (2) Å, b = 21.710 (4) Å, c = 14.475 (3) Å, β = 100.75 (2)°, Z = 4. The molybdenum atom is in a distorted octahedral coordination environment composed of fac-tridentate HB(Me2pz)31, terminal oxo (Mo=O = 1.669 (3) Å), and bidentate S2CNEt2- ligands. The reaction of these oxo complexes with boron sulfide in dichloromethane yields the gold-yellow, diamagnetic sulfido analogues {HB(Me2pz)3}MoS(S2CNR2). The compound {HB(Me2pz)3}MoS(S2CNEt 2)·CH2Cl2 crystallizes in the orthorhombic space group P212121 with a = 7.967 (3) Å, b = 14.314 (5) Å, c = 26.15 (1) Å, Z = 4. The coordination geometry is similar to that of the oxo analogue, with Mo=S = 2.129 (2) Å.

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