Mononuclear Oxo- and Sulfidomolybdenum(IV) Complexes. Syntheses and Crystal Structures of {HB(Me2c3n2h)3}Moe(s2CNEt2) (E = O, S) and Related Complexes

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

doi:10.1021/ja00244a015

Mononuclear Oxo- and Sulfidomolybdenum(IV) Complexes. Syntheses and Crystal Structures of {HB(Me₂c₃n₂h)₃}Moe(s₂CNEt₂) (E = O, S) and Related Complexes

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

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

72 Scopus citations

Abstract

The syntheses, structures, and properties of mononuclear oxo- and sulfidomolybdenum(IV) complexes with hy-drotris(3,5-dimethyl-l-pyrazolyl)borate, HB(Me₂pz)₃~, and dithiocarbamate ligands are described. The reactions of MoO-(S₂CNR₂)₂(R = Me, Et, n-Pr, «-Bu) with K{HB(Me₂pz)₃(in refluxing toluene yield the green, diamagnetic, air-stable complexes| HB(Me₂pz)₃]MoO(S₂CNR₂). The complex jHB(Me₂pz)₃)MoO(S₂CNEt₂) crystallizes in the monoclinic space group P2Jc 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/aotridentate HB(Me₂pz)₃“, terminal oxo (Mo=0 = 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(S₂CNEt₂)•CH₂Cl₂crystallizes in the orthorhombic space group P2₁2₁2₁with 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 language	English (US)
Pages (from-to)	2938-2946
Number of pages	9
Journal	Journal of the American Chemical Society
Volume	109
Issue number	10
DOIs	https://doi.org/10.1021/ja00244a015
State	Published - May 1 1987
Externally published	Yes

ASJC Scopus subject areas

Catalysis
General Chemistry
Biochemistry
Colloid and Surface Chemistry

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10.1021/ja00244a015

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Mononuclear Oxo- and Sulfidomolybdenum(IV) Complexes. Syntheses and Crystal Structures of {HB(Me₂c₃n₂h)₃}Moe(s₂CNEt₂) (E = O, S) and Related Complexes. / Young, Charles G.; Roberts, Sue A.; Ortega, Richard B. et al.
In: Journal of the American Chemical Society, Vol. 109, No. 10, 01.05.1987, p. 2938-2946.

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

@article{940a8ccf6fe54f4fa5b3cf6092eca292,

title = "Mononuclear Oxo- and Sulfidomolybdenum(IV) Complexes. Syntheses and Crystal Structures of \{HB(Me2c3n2h)3\}Moe(s2CNEt2) (E = O, S) and Related Complexes",

abstract = "The syntheses, structures, and properties of mononuclear oxo- and sulfidomolybdenum(IV) complexes with hy-drotris(3,5-dimethyl-l-pyrazolyl)borate, HB(Me2pz)3\textasciitilde{}, and dithiocarbamate ligands are described. The reactions of MoO-(S2CNR2)2(R = Me, Et, n-Pr, «-Bu) with K\{HB(Me2pz)3(in refluxing toluene yield the green, diamagnetic, air-stable complexes| HB(Me2pz)3]MoO(S2CNR2). The complex jHB(Me2pz)3)MoO(S2CNEt2) crystallizes in the monoclinic space group P2Jc 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/aotridentate HB(Me2pz)3“, terminal oxo (Mo=0 = 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(S2CNEt2)•CH2Cl2crystallizes in the orthorhombic space group P212121with 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.\}",

year = "1987",

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T1 - Mononuclear Oxo- and Sulfidomolybdenum(IV) Complexes. Syntheses and Crystal Structures of {HB(Me2c3n2h)3}Moe(s2CNEt2) (E = O, S) and Related Complexes

AU - Young, Charles G.

AU - Roberts, Sue A.

AU - Ortega, Richard B.

AU - Enemark, John H.

PY - 1987/5/1

Y1 - 1987/5/1

N2 - The syntheses, structures, and properties of mononuclear oxo- and sulfidomolybdenum(IV) complexes with hy-drotris(3,5-dimethyl-l-pyrazolyl)borate, HB(Me2pz)3~, and dithiocarbamate ligands are described. The reactions of MoO-(S2CNR2)2(R = Me, Et, n-Pr, «-Bu) with K{HB(Me2pz)3(in refluxing toluene yield the green, diamagnetic, air-stable complexes| HB(Me2pz)3]MoO(S2CNR2). The complex jHB(Me2pz)3)MoO(S2CNEt2) crystallizes in the monoclinic space group P2Jc 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/aotridentate HB(Me2pz)3“, terminal oxo (Mo=0 = 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(S2CNEt2)•CH2Cl2crystallizes in the orthorhombic space group P212121with 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 hy-drotris(3,5-dimethyl-l-pyrazolyl)borate, HB(Me2pz)3~, and dithiocarbamate ligands are described. The reactions of MoO-(S2CNR2)2(R = Me, Et, n-Pr, «-Bu) with K{HB(Me2pz)3(in refluxing toluene yield the green, diamagnetic, air-stable complexes| HB(Me2pz)3]MoO(S2CNR2). The complex jHB(Me2pz)3)MoO(S2CNEt2) crystallizes in the monoclinic space group P2Jc 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/aotridentate HB(Me2pz)3“, terminal oxo (Mo=0 = 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(S2CNEt2)•CH2Cl2crystallizes in the orthorhombic space group P212121with 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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U2 - 10.1021/ja00244a015

DO - 10.1021/ja00244a015

M3 - Article

SN - 0002-7863

VL - 109

SP - 2938

EP - 2946

JO - Journal of the American Chemical Society

JF - Journal of the American Chemical Society

IS - 10

ER -

Mononuclear Oxo- and Sulfidomolybdenum(IV) Complexes. Syntheses and Crystal Structures of {HB(Me₂c₃n₂h)₃}Moe(s₂CNEt₂) (E = O, S) and Related Complexes

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