Synthesis of Early Transition Metal Porphyrin Halide Complexes: First Structural Characterization of a Vanadium(III) Porphyrin Complex

Lisa M. Berreau; J. Alan Hays; Victor G. Young; L. Keith Woo

doi:10.1021/ic00079a020

Synthesis of Early Transition Metal Porphyrin Halide Complexes: First Structural Characterization of a Vanadium(III) Porphyrin Complex

Lisa M. Berreau, J. Alan Hays, Victor G. Young, L. Keith Woo

Chemistry (Twin Cities)

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Abstract

A general method for the preparation of early transition metal porphyrin halide complexes using a porphyrin dianion, (THF)₂Li₂(POR) (POR = OEP, TTP; OEP = octaethylporphyrinato, TTP = meso-tetra-p-tolylporphyrinato), and the appropriate metal halide complex, MX_n (MX_n = VCl₃(THF)₃, TiCl₄(THF)₂, TiCl₃(THF)₃, MoCl₄(CH₃CN)₂, WCl₄), is described. The structure of (TTP)V^IIICl•THF (2•THF) has been determined by single-crystal X-ray diffraction analysis. Complex 2-THF crystallizes in the centrosymmetric space group P2₁/m with a = 11.968(2) Å, b = 17.072(3) Å, c = 12.649(2) Å, β = 98.62(2)°, V= 2555.2(8) Å³, Z = 2, R = 4.6%, and R_w = 6.7%. The V-Cl bond length is 2.272(1) Å, the V-N bond lengths range from 2.040(4) to 2.050(3) Å, and the V-O bond distance is 2.141(3) Å.

Original language	English (US)
Pages (from-to)	105-108
Number of pages	4
Journal	Inorganic chemistry
Volume	33
Issue number	1
DOIs	https://doi.org/10.1021/ic00079a020
State	Published - Jan 1 1994

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@article{9f530efe1c7742d2a3defa7209131fd7,

title = "Synthesis of Early Transition Metal Porphyrin Halide Complexes: First Structural Characterization of a Vanadium(III) Porphyrin Complex",

abstract = "A general method for the preparation of early transition metal porphyrin halide complexes using a porphyrin dianion, (THF)2Li2(POR) (POR = OEP, TTP; OEP = octaethylporphyrinato, TTP = meso-tetra-p-tolylporphyrinato), and the appropriate metal halide complex, MXn (MXn = VCl3(THF)3, TiCl4(THF)2, TiCl3(THF)3, MoCl4(CH3CN)2, WCl4), is described. The structure of (TTP)VIIICl•THF (2•THF) has been determined by single-crystal X-ray diffraction analysis. Complex 2-THF crystallizes in the centrosymmetric space group P21/m with a = 11.968(2) {\AA}, b = 17.072(3) {\AA}, c = 12.649(2) {\AA}, β = 98.62(2)°, V= 2555.2(8) {\AA}3, Z = 2, R = 4.6%, and Rw = 6.7%. The V-Cl bond length is 2.272(1) {\AA}, the V-N bond lengths range from 2.040(4) to 2.050(3) {\AA}, and the V-O bond distance is 2.141(3) {\AA}.",

author = "Berreau, {Lisa M.} and Hays, {J. Alan} and Young, {Victor G.} and Woo, {L. Keith}",

year = "1994",

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doi = "10.1021/ic00079a020",

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pages = "105--108",

journal = "Inorganic chemistry",

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TY - JOUR

T1 - Synthesis of Early Transition Metal Porphyrin Halide Complexes

T2 - First Structural Characterization of a Vanadium(III) Porphyrin Complex

AU - Berreau, Lisa M.

AU - Hays, J. Alan

AU - Young, Victor G.

AU - Woo, L. Keith

PY - 1994/1/1

Y1 - 1994/1/1

N2 - A general method for the preparation of early transition metal porphyrin halide complexes using a porphyrin dianion, (THF)2Li2(POR) (POR = OEP, TTP; OEP = octaethylporphyrinato, TTP = meso-tetra-p-tolylporphyrinato), and the appropriate metal halide complex, MXn (MXn = VCl3(THF)3, TiCl4(THF)2, TiCl3(THF)3, MoCl4(CH3CN)2, WCl4), is described. The structure of (TTP)VIIICl•THF (2•THF) has been determined by single-crystal X-ray diffraction analysis. Complex 2-THF crystallizes in the centrosymmetric space group P21/m with a = 11.968(2) Å, b = 17.072(3) Å, c = 12.649(2) Å, β = 98.62(2)°, V= 2555.2(8) Å3, Z = 2, R = 4.6%, and Rw = 6.7%. The V-Cl bond length is 2.272(1) Å, the V-N bond lengths range from 2.040(4) to 2.050(3) Å, and the V-O bond distance is 2.141(3) Å.

AB - A general method for the preparation of early transition metal porphyrin halide complexes using a porphyrin dianion, (THF)2Li2(POR) (POR = OEP, TTP; OEP = octaethylporphyrinato, TTP = meso-tetra-p-tolylporphyrinato), and the appropriate metal halide complex, MXn (MXn = VCl3(THF)3, TiCl4(THF)2, TiCl3(THF)3, MoCl4(CH3CN)2, WCl4), is described. The structure of (TTP)VIIICl•THF (2•THF) has been determined by single-crystal X-ray diffraction analysis. Complex 2-THF crystallizes in the centrosymmetric space group P21/m with a = 11.968(2) Å, b = 17.072(3) Å, c = 12.649(2) Å, β = 98.62(2)°, V= 2555.2(8) Å3, Z = 2, R = 4.6%, and Rw = 6.7%. The V-Cl bond length is 2.272(1) Å, the V-N bond lengths range from 2.040(4) to 2.050(3) Å, and the V-O bond distance is 2.141(3) Å.

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Synthesis of Early Transition Metal Porphyrin Halide Complexes: First Structural Characterization of a Vanadium(III) Porphyrin Complex

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