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New niobium complexes with alkynes. 2. Tetranuclear compounds with Nb-Nb bonds, an unprecedented type of tetracarbon ligand, and oxygen in a rectangular environment

Journal Article · · Journal of the American Chemical Society; (USA)
DOI:https://doi.org/10.1021/ja00160a043· OSTI ID:6725848
;  [1]
  1. Texas A M Univ., College Station (USA)
+ Show Author Affiliations
Three compounds containing the tetranuclear anion (Nb{sub 4}OCl{sub 8}((PhC){sub 4}){sub 2}){sup 2{minus}} have been prepared by (1) reduction by NbCl{sub 4}(THF){sub 2} with Mg in the presence of PhCCPh, (2) by reduction of NbCl{sub 3}(PhCCPh)(THF){sub 2} with Na/Hg, and (3) by reduction of NbCl{sub 3}(PhCCPh)(THF){sub 2} with Na/Hg in the presence of PEt{sub 3}. Crystallographic data for the three compounds are as follows: (1) (Mg{sub 2}Cl{sub 3}(THF){sub 6}){sub 2}(Nb{sub 4}OCl{sub 8}((PhC){sub 4}){sub 2}){center dot}6THF, space group P{bar 1}, a = 15.200 (3) {angstrom}, b = 15.515 (4) {angstrom}, c = 16.306 (3) {angstrom}, {alpha} = 98.93 (2){degree}, {beta} = 106.90 (2){degree}, {gamma} = 102.97 (2){degree}, V = 3484 (3) {angstrom}{sup 3}, Z = 1; (2) Na{sub 2}(Nb{sub 4}OCl{sub 8}((PhC){sub 4}){sub 2}){center dot}(THF){sub 6}(C{sub 6}H{sub 6}){sub 2}, space group P{bar 1}, a = 11.802 (3) {angstrom}, b = 17.311 (2) {angstrom}, c = 22.966 (4) {angstrom}, {alpha} = 98.91 (1){degree}, {beta} = 91.61 (1){degree}, {gamma} = 103.55 (1){degree}, V = 4496 (3) {angstrom}, Z = 2; (3) (HPEt{sub 3}){sub 2}(Nb{sub 4}OCl{sub 8}((PhC){sub 4}){sub 2}){center dot}2C{sub 6}H{sub 6}, space group P{bar 1}, a = 12.831 (1) {angstrom}, b = 13.194 (1) {angstrom}, c = 14.219 (1) {angstrom}, {alpha} = 68.040 (8){degree}, {beta} = 66.616 (7){degree}, {gamma} = 66.704 (7){degree}, V = 1961.0 (4) {angstrom}{sup 3}, Z = 1.
OSTI ID:
6725848
Journal Information:
Journal of the American Chemical Society; (USA), Journal Name: Journal of the American Chemical Society; (USA) Vol. 112:4; ISSN 0002-7863; ISSN JACSA
Country of Publication:
United States
Language:
English

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Related Subjects

36 MATERIALS SCIENCE
360102* -- Metals & Alloys-- Structure & Phase Studies
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
400201 -- Chemical & Physicochemical Properties
ALKYNES
CALCULATION METHODS
COMPLEXES
CRYSTAL STRUCTURE
DATA ANALYSIS
HYDROCARBONS
LIGANDS
MEASURING INSTRUMENTS
MEASURING METHODS
NIOBIUM COMPLEXES
ORGANIC COMPOUNDS
SYNTHESIS
TRANSITION ELEMENT COMPLEXES