X-RAY DIFFRACTION STRUCTURAL INVESTIGATION OF TWO HAFNIUM(IV) COMPLEXES WITH DIPIVALOYLMETHANE
K. V. Zherikova, I. A. Baidina, N. B. Morozova, N. V. Kuratieva, I. K. Igumenov
Keywords: hafnium(IV) ОІ-diketonates, synthesis, single crystal X-ray diffraction, mononuclear complex, mass-spectrometry study
Pages: 1137-1142
Abstract
Synthesis and single crystal X-ray diffraction study of hafnium(IV) dipivaloylmethanate Hf(dpm)4 and chloro-tris-(dipivaloylmethanato)hafnium(IV) Hf(dpm)3Cl have been carried out. Crystal data: a =
22.6606(5) Å, b = 11.3990(4) Å, c = 19.8513(7) Å, β = 106.458(1)°, Рс, Z = 4, dcalc = 1.231 g/cm3, R = 0.075 for C44H76HfO8; a = 10.6376(13) Å, b = 10.6701(10) Å, c = 19.4400(22) Å, α = 74.970(3)°, β = 75.672(3)°, γ = 61.725(2)°, P-1, Z = 2, dcalc = 1.366 g/cm3, R = 0.031 for C33H57ClHfO6. The structures are molecular and are built from discrete mononuclear complexes joined by van der Waals interactions. Disordering of carbon atoms preserving at low temperature is observed for the compound Hf(dpm)4. It has been found out that the structure contains two crystallographically unique complexes of hafnium(IV) with central atoms coordinated with eight oxygen atoms of four dipivaloylmethane ligands, bond lengths Hf-O fall within 2.084-2.222 Å, the distances Hf…Hf between the molecules are 10.07-13.87 Å. In Hf(dpm)3Cl the hafnium atom is seven-coordinated with six oxygen atoms of three β-diketonate ligands and one chlorine atom, the distances Hf-O fall within 2.087-2.179 Å, the lengths of the bond Hf-Cl for two crystallographically independent molecules Hf(1) and Hf(2) are 2.466 Å and 2.442 Å, respectively.
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