EIGHT-COORDINATE CHELATE COMPLEXES OF ZIRCONIUM(IV) AND NIOBIUM(IV) : X-RAY DIFFRACTOMETRIC AND EPR INVESTIGATIONS
作者： Fausto Calderazzo , Ulli Englertb , Cäcilia Maichle-Mössmer , Fabio Marchetti , Guido Pampaloni
DOI: 10.1016/S0020-1693(97)05838-6
关键词: Monoclinic crystal system 、 Zirconium 、 Niobium 、 Electron paramagnetic resonance 、 Chemistry 、 Solid solution 、 Crystallography 、 Square antiprismatic molecular geometry 、 Orthorhombic crystal system 、 Paramagnetism
摘要: Abstract The N,N -diethylcarbamato derivative of zirconium(IV), Zr(O 2 CNEt ) 4 has been studied by X-ray crystallography. Crystal data: C 20 H 40 Na O 8 Zr, monoclinic, space group 2/ c , a = 14.057(1), b 12.168(1), 16.746(2) A, β 108.071(4)°, Z 4, D 1.356, F(000) 1168, T 213 K. compound is isotypic with the corresponding niobium(IV) dodecahedral coordination at zirconium atom. By reaction NbCl (THF) Tl(hfacac), hexafluoroacetylacetonato niobium (IV), Nb(hfacac) prepared and structurally characterized. crystallizes in orthorhombic Pna 1 following cell constants: 10.399(4), 15.852(9), 119.073(1) A. It not zirconium(IV) derivative, Zr(hfacac) . F 24 P / n 11.974(4), 20.451(6), 13.140(3) 104.487(11)°, 1.960, 1776, 223 Although both compounds central metal atom shows square antiprismatic coordination, mode ligands different slight deviations from (llll) (llss) ideal geometries have observed case zirconium, respectively. An EPR study performed on Nb(IV) derivatives as diluted solid solutions frozen organic solvents or diamagnetic matrix compound. spectra confirmed presence non-interacting paramagnets and, Nb(O point symmetry paramagnetic centre found to be agreement results investigation. spectrum rhombic for when THF solution
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