Preparation and characterization of bis(dialkyldithiocarbamato)[hydrotris(3,5-dimethyl-1-pyrazolyl)borato] molybdenum(III) complexes produced by the oxidative decarbonylation of [{HB(3,5-Me2C3N2H)3}Mo(CO) 3]- by tetraalkylthiuram bisulfides. Crystal structure of {HB(3,5-Me2C3 ...

Charles G. Young, Sue A Roberts, John H. Enemark

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Abstract

Full title: Preparation and characterization of bis(dialkyldithiocarbamato)[hydrotris(3,5-dimethyl-1-pyrazolyl)borato] molybdenum(III) complexes produced by the oxidative decarbonylation of [{HB(3,5-Me2C3N2H)3}Mo(CO) 3]- by tetraalkylthiuram bisulfides. Crystal structure of {HB(3,5-Me2C3N2H)3}Mo(η 2-S2CNEt2)(η1-S 2CNEt2). The reactions of Et4N[{HB(Me2pz)3}Mo(CO)3] [HB(Me2pz)3- = hydrotris(3,5-dimethyl-1-pyrazolyl)borate anion] and tetra-alkylthiuram disulfides in refluxing acetonitrile produce the yellow or orange, air-sensitive compounds {HB(Me2pz)3}Mo(η2-S2CNR 2)(η1-S2CNR2) (1, R = Me; 2, R = Et). The compounds are monomeric, paramagnetic (μeff: 1, 3.93 μB; 2, 3.84 μB) and exhibit infrared bands characteristic of both mono- and bidentate dithiocarbamate ligands. Complex 2 crystallizes in triclinic space group P1 with a = 10.162 (4) Å, b = 11.089 (4) Å, c = 31.10 (1) Å, α = 88.49 (3)°, β = 86.34 (3)°, γ = 68.37 (3)°, V = 3251 (3) Å3, and Z = 4. The structure was solved by Patterson and Fourier methods, followed by least-squares refinement, using 5547 reflections, to a conventional R value of 0.043 (Rw = 0.049). The complex possesses a distorted octahedral fac-N3-fac-S3 coordination sphere composed of tridentate HB(Me2pz)3-, bidentate S2CNEt2-, and monodentate S2CNEt2- ligands. Structural comparison of the two dithiocarbamate ligands indicates considerable thioureide character in the η1-ligand framework.

Original languageEnglish (US)
Pages (from-to)3667-3671
Number of pages5
JournalInorganic Chemistry
Volume25
Issue number20
StatePublished - 1986

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Molybdenum
Carbon Monoxide
molybdenum
Crystal structure
Ligands
preparation
ligands
crystal structure
Borates
disulfides
borates
Disulfides
acetonitrile
Anions
anions
Infrared radiation
air
Air

ASJC Scopus subject areas

  • Inorganic Chemistry

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@article{b6fe8c55108148808ce1ae314bc500e5,
title = "Preparation and characterization of bis(dialkyldithiocarbamato)[hydrotris(3,5-dimethyl-1-pyrazolyl)borato] molybdenum(III) complexes produced by the oxidative decarbonylation of [{HB(3,5-Me2C3N2H)3}Mo(CO) 3]- by tetraalkylthiuram bisulfides. Crystal structure of {HB(3,5-Me2C3 ...",
abstract = "Full title: Preparation and characterization of bis(dialkyldithiocarbamato)[hydrotris(3,5-dimethyl-1-pyrazolyl)borato] molybdenum(III) complexes produced by the oxidative decarbonylation of [{HB(3,5-Me2C3N2H)3}Mo(CO) 3]- by tetraalkylthiuram bisulfides. Crystal structure of {HB(3,5-Me2C3N2H)3}Mo(η 2-S2CNEt2)(η1-S 2CNEt2). The reactions of Et4N[{HB(Me2pz)3}Mo(CO)3] [HB(Me2pz)3- = hydrotris(3,5-dimethyl-1-pyrazolyl)borate anion] and tetra-alkylthiuram disulfides in refluxing acetonitrile produce the yellow or orange, air-sensitive compounds {HB(Me2pz)3}Mo(η2-S2CNR 2)(η1-S2CNR2) (1, R = Me; 2, R = Et). The compounds are monomeric, paramagnetic (μeff: 1, 3.93 μB; 2, 3.84 μB) and exhibit infrared bands characteristic of both mono- and bidentate dithiocarbamate ligands. Complex 2 crystallizes in triclinic space group P1 with a = 10.162 (4) {\AA}, b = 11.089 (4) {\AA}, c = 31.10 (1) {\AA}, α = 88.49 (3)°, β = 86.34 (3)°, γ = 68.37 (3)°, V = 3251 (3) {\AA}3, and Z = 4. The structure was solved by Patterson and Fourier methods, followed by least-squares refinement, using 5547 reflections, to a conventional R value of 0.043 (Rw = 0.049). The complex possesses a distorted octahedral fac-N3-fac-S3 coordination sphere composed of tridentate HB(Me2pz)3-, bidentate S2CNEt2-, and monodentate S2CNEt2- ligands. Structural comparison of the two dithiocarbamate ligands indicates considerable thioureide character in the η1-ligand framework.",
author = "Young, {Charles G.} and Roberts, {Sue A} and Enemark, {John H.}",
year = "1986",
language = "English (US)",
volume = "25",
pages = "3667--3671",
journal = "Inorganic Chemistry",
issn = "0020-1669",
publisher = "American Chemical Society",
number = "20",

}

TY - JOUR

T1 - Preparation and characterization of bis(dialkyldithiocarbamato)[hydrotris(3,5-dimethyl-1-pyrazolyl)borato] molybdenum(III) complexes produced by the oxidative decarbonylation of [{HB(3,5-Me2C3N2H)3}Mo(CO) 3]- by tetraalkylthiuram bisulfides. Crystal structure of {HB(3,5-Me2C3 ...

AU - Young, Charles G.

AU - Roberts, Sue A

AU - Enemark, John H.

PY - 1986

Y1 - 1986

N2 - Full title: Preparation and characterization of bis(dialkyldithiocarbamato)[hydrotris(3,5-dimethyl-1-pyrazolyl)borato] molybdenum(III) complexes produced by the oxidative decarbonylation of [{HB(3,5-Me2C3N2H)3}Mo(CO) 3]- by tetraalkylthiuram bisulfides. Crystal structure of {HB(3,5-Me2C3N2H)3}Mo(η 2-S2CNEt2)(η1-S 2CNEt2). The reactions of Et4N[{HB(Me2pz)3}Mo(CO)3] [HB(Me2pz)3- = hydrotris(3,5-dimethyl-1-pyrazolyl)borate anion] and tetra-alkylthiuram disulfides in refluxing acetonitrile produce the yellow or orange, air-sensitive compounds {HB(Me2pz)3}Mo(η2-S2CNR 2)(η1-S2CNR2) (1, R = Me; 2, R = Et). The compounds are monomeric, paramagnetic (μeff: 1, 3.93 μB; 2, 3.84 μB) and exhibit infrared bands characteristic of both mono- and bidentate dithiocarbamate ligands. Complex 2 crystallizes in triclinic space group P1 with a = 10.162 (4) Å, b = 11.089 (4) Å, c = 31.10 (1) Å, α = 88.49 (3)°, β = 86.34 (3)°, γ = 68.37 (3)°, V = 3251 (3) Å3, and Z = 4. The structure was solved by Patterson and Fourier methods, followed by least-squares refinement, using 5547 reflections, to a conventional R value of 0.043 (Rw = 0.049). The complex possesses a distorted octahedral fac-N3-fac-S3 coordination sphere composed of tridentate HB(Me2pz)3-, bidentate S2CNEt2-, and monodentate S2CNEt2- ligands. Structural comparison of the two dithiocarbamate ligands indicates considerable thioureide character in the η1-ligand framework.

AB - Full title: Preparation and characterization of bis(dialkyldithiocarbamato)[hydrotris(3,5-dimethyl-1-pyrazolyl)borato] molybdenum(III) complexes produced by the oxidative decarbonylation of [{HB(3,5-Me2C3N2H)3}Mo(CO) 3]- by tetraalkylthiuram bisulfides. Crystal structure of {HB(3,5-Me2C3N2H)3}Mo(η 2-S2CNEt2)(η1-S 2CNEt2). The reactions of Et4N[{HB(Me2pz)3}Mo(CO)3] [HB(Me2pz)3- = hydrotris(3,5-dimethyl-1-pyrazolyl)borate anion] and tetra-alkylthiuram disulfides in refluxing acetonitrile produce the yellow or orange, air-sensitive compounds {HB(Me2pz)3}Mo(η2-S2CNR 2)(η1-S2CNR2) (1, R = Me; 2, R = Et). The compounds are monomeric, paramagnetic (μeff: 1, 3.93 μB; 2, 3.84 μB) and exhibit infrared bands characteristic of both mono- and bidentate dithiocarbamate ligands. Complex 2 crystallizes in triclinic space group P1 with a = 10.162 (4) Å, b = 11.089 (4) Å, c = 31.10 (1) Å, α = 88.49 (3)°, β = 86.34 (3)°, γ = 68.37 (3)°, V = 3251 (3) Å3, and Z = 4. The structure was solved by Patterson and Fourier methods, followed by least-squares refinement, using 5547 reflections, to a conventional R value of 0.043 (Rw = 0.049). The complex possesses a distorted octahedral fac-N3-fac-S3 coordination sphere composed of tridentate HB(Me2pz)3-, bidentate S2CNEt2-, and monodentate S2CNEt2- ligands. Structural comparison of the two dithiocarbamate ligands indicates considerable thioureide character in the η1-ligand framework.

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