Studies of the oxovanadium(IV)-oxalate system: Syntheses and crystal structures of binuclear (Ph4P)2[(VO)2(H2O) 2(C2O4)3]·4H2O and of the one-dimensional chain material, (Ph4P) [VOCl(C2O4)]

José Salta; Charles J. O'Connor; Sichu Li; Jon Zubieta

doi:10.1016/s0020-1693(96)05239-5

Studies of the oxovanadium(IV)-oxalate system: Syntheses and crystal structures of binuclear (Ph₄P)₂[(VO)₂(H₂O) ₂(C₂O₄)3]·4H₂O and of the one-dimensional chain material, (Ph₄P) [VOCl(C₂O₄)]

José Salta, Charles J. O'Connor, Sichu Li, Jon Zubieta

Department of Chemistry

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

31 Scopus citations

Abstract

The hydrothermal reactions of (Ph₄P)[VO₂Cl₂] and H₂C₂O₄ at 150 and 125 °C yield (Ph₄P)₂[V₂O₂(H₂O) ₂(C₂O₄)₃]·4H₂O (1) and (Ph₄P) [VOCl(C₂O₄)] (2), respectively. The structure of the molecular anion of 1 consists of a binuclear unit of oxovanadium(IV) octahedra bridged by a bisbidentate oxalate group. The {VO₆} coordination geometry at each vanadium site is defined by a terminal oxo group, an aquo ligand, and four oxygen donors - two from the bisbidentate bridging oxalate and two from the terminal bidentate oxalate. The structure of 2 consists of discrete Ph₄P⁺ cations occupying regions between {[VOCl(C₂O₄)]^-}_∝ spiral chains. The structure of the one-dimensional anionic chain exhibits V(IV) octahedra bridged by bisbidentate oxalate groups. Crystal data: 1·4H₂O, monoclinic P2₁/n, a=12.694(3), b=12.531 (3), c=17.17(3) Å, β=106.32(2)°, V=2621.3(13) Å³,Z=2,D_calc=1.501 g cm^-3, structure solution and refinement converged at a conventional residual of 0.0518; 2, tetragonal P4₃, a=12.145(2), c=15.991(3) Å, V=2358.7(12) Å³, Z=4, R=0.0452.

Original language	English (US)
Pages (from-to)	303-310
Number of pages	8
Journal	Inorganica Chimica Acta
Volume	250
Issue number	1-2 PART I
DOIs	https://doi.org/10.1016/s0020-1693(96)05239-5
State	Published - Sep 1996

Keywords

Crystal structures
Hydrothermal synthesis
One-dimensional chain complexes
Oxalate complexes
Oxovanadium complexes

ASJC Scopus subject areas

Physical and Theoretical Chemistry
Inorganic Chemistry
Materials Chemistry

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10.1016/s0020-1693(96)05239-5

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Studies of the oxovanadium(IV)-oxalate system: Syntheses and crystal structures of binuclear (Ph₄P)₂[(VO)₂(H₂O) ₂(C₂O₄)3]·4H₂O and of the one-dimensional chain material, (Ph₄P) [VOCl(C₂O₄)]. / Salta, José; O'Connor, Charles J.; Li, Sichu et al.
In: Inorganica Chimica Acta, Vol. 250, No. 1-2 PART I, 09.1996, p. 303-310.

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

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title = "Studies of the oxovanadium(IV)-oxalate system: Syntheses and crystal structures of binuclear (Ph4P)2[(VO)2(H2O) 2(C2O4)3]·4H2O and of the one-dimensional chain material, (Ph4P) [VOCl(C2O4)]",

abstract = "The hydrothermal reactions of (Ph4P)[VO2Cl2] and H2C2O4 at 150 and 125 °C yield (Ph4P)2[V2O2(H2O) 2(C2O4)3]·4H2O (1) and (Ph4P) [VOCl(C2O4)] (2), respectively. The structure of the molecular anion of 1 consists of a binuclear unit of oxovanadium(IV) octahedra bridged by a bisbidentate oxalate group. The {VO6} coordination geometry at each vanadium site is defined by a terminal oxo group, an aquo ligand, and four oxygen donors - two from the bisbidentate bridging oxalate and two from the terminal bidentate oxalate. The structure of 2 consists of discrete Ph4P+ cations occupying regions between {[VOCl(C2O4)]-}∝ spiral chains. The structure of the one-dimensional anionic chain exhibits V(IV) octahedra bridged by bisbidentate oxalate groups. Crystal data: 1·4H2O, monoclinic P21/n, a=12.694(3), b=12.531 (3), c=17.17(3) {\AA}, β=106.32(2)°, V=2621.3(13) {\AA}3,Z=2,Dcalc=1.501 g cm-3, structure solution and refinement converged at a conventional residual of 0.0518; 2, tetragonal P43, a=12.145(2), c=15.991(3) {\AA}, V=2358.7(12) {\AA}3, Z=4, R=0.0452.",

keywords = "Crystal structures, Hydrothermal synthesis, One-dimensional chain complexes, Oxalate complexes, Oxovanadium complexes",

author = "Jos{\'e} Salta and O'Connor, {Charles J.} and Sichu Li and Jon Zubieta",

note = "Funding Information: This work was supported by NSF Grant CHE 9318824.",

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doi = "10.1016/s0020-1693(96)05239-5",

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T1 - Studies of the oxovanadium(IV)-oxalate system

T2 - Syntheses and crystal structures of binuclear (Ph4P)2[(VO)2(H2O) 2(C2O4)3]·4H2O and of the one-dimensional chain material, (Ph4P) [VOCl(C2O4)]

AU - Salta, José

AU - O'Connor, Charles J.

AU - Li, Sichu

AU - Zubieta, Jon

N1 - Funding Information: This work was supported by NSF Grant CHE 9318824.

PY - 1996/9

Y1 - 1996/9

N2 - The hydrothermal reactions of (Ph4P)[VO2Cl2] and H2C2O4 at 150 and 125 °C yield (Ph4P)2[V2O2(H2O) 2(C2O4)3]·4H2O (1) and (Ph4P) [VOCl(C2O4)] (2), respectively. The structure of the molecular anion of 1 consists of a binuclear unit of oxovanadium(IV) octahedra bridged by a bisbidentate oxalate group. The {VO6} coordination geometry at each vanadium site is defined by a terminal oxo group, an aquo ligand, and four oxygen donors - two from the bisbidentate bridging oxalate and two from the terminal bidentate oxalate. The structure of 2 consists of discrete Ph4P+ cations occupying regions between {[VOCl(C2O4)]-}∝ spiral chains. The structure of the one-dimensional anionic chain exhibits V(IV) octahedra bridged by bisbidentate oxalate groups. Crystal data: 1·4H2O, monoclinic P21/n, a=12.694(3), b=12.531 (3), c=17.17(3) Å, β=106.32(2)°, V=2621.3(13) Å3,Z=2,Dcalc=1.501 g cm-3, structure solution and refinement converged at a conventional residual of 0.0518; 2, tetragonal P43, a=12.145(2), c=15.991(3) Å, V=2358.7(12) Å3, Z=4, R=0.0452.

AB - The hydrothermal reactions of (Ph4P)[VO2Cl2] and H2C2O4 at 150 and 125 °C yield (Ph4P)2[V2O2(H2O) 2(C2O4)3]·4H2O (1) and (Ph4P) [VOCl(C2O4)] (2), respectively. The structure of the molecular anion of 1 consists of a binuclear unit of oxovanadium(IV) octahedra bridged by a bisbidentate oxalate group. The {VO6} coordination geometry at each vanadium site is defined by a terminal oxo group, an aquo ligand, and four oxygen donors - two from the bisbidentate bridging oxalate and two from the terminal bidentate oxalate. The structure of 2 consists of discrete Ph4P+ cations occupying regions between {[VOCl(C2O4)]-}∝ spiral chains. The structure of the one-dimensional anionic chain exhibits V(IV) octahedra bridged by bisbidentate oxalate groups. Crystal data: 1·4H2O, monoclinic P21/n, a=12.694(3), b=12.531 (3), c=17.17(3) Å, β=106.32(2)°, V=2621.3(13) Å3,Z=2,Dcalc=1.501 g cm-3, structure solution and refinement converged at a conventional residual of 0.0518; 2, tetragonal P43, a=12.145(2), c=15.991(3) Å, V=2358.7(12) Å3, Z=4, R=0.0452.

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KW - One-dimensional chain complexes

KW - Oxalate complexes

KW - Oxovanadium complexes

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