Synthesis and Structure of Cyclopentadienyl Diferrocenoylacetonatozirconium Chloride С5H5[С10H9FeC(O)CHC(O)CF3]2ZrCl

Abstract

Interaction of zirconocene dichloride with ferrocenoyltrifluoroacetylacetone in benzene solution led to synthesis of a trans-isomer of cyclopentadienyl diferrocenoylacetonatozirconium chloride, the structure of which was proved by X-ray diffraction analysis. According to the X-ray analysis performed at 293 K on an automatic four-circle diffractometer D8 QuestBruker (MoCA radiation, λ = 0.71073 Å, graphite monochromator), the zirconium atoms in the trans-isomer of complex 1 have a distorted octahedral configuration [C₃₃H₂₅F₆ClFe₂ZrO₄ (1), M 837.90; the crystal structure is triclinic, the symmetry group P ; crystal unit cell parameters: a = 10.16(3),
b = 12.39(3), c = 13.44 (3) Å; α= 95.70(10)º, β = 102.62(14)º, γ = 93.77(2)° ; V = 1635 (6) ų; crystal size 0.16 × 0.09 × 0.08 mm³; reflection index intervals –12 ≤ h ≤ 12, –15 ≤ k ≤ 15,
–17 ≤ l ≤ 17; total reflections 23770; independent reflections 7090; R_int = 0.3164; GOOF = 1.054; R₁ = 0.1601, wR₂ = 0.3121; residual electron density 1.41/–1.80 e/ų. In the IR spectrum of compound 1 the bands are observed at 808, 1007, 1055, 1409, 2855, 2926, 3099 cm^–1, which can be attributed to fluctuations in the bonds of the ferrocene substituent. The intense vibration band at 1298 cm^–1 corresponds to the vibrations of the CF₃ groups. Valence vibrations of the Zr-O bonds appear in the IR spectrum as a series of bands in the region of 400–1000 cm^–1. According to the X-ray diffraction analysis, the packing of complex 1 molecules into layers is possible due to short contacts С···С (3.323 Å). Each of the layers is formed by reference contacts Н···С (2.850 Å). Complete tables of atomic coordinates, bond lengths, and valence angles are deposited in the Cambridge structural data Bank (No. 1988379 for 1; deposit@ccdc.cam.ac.uk; http://www.ccdc.cam.ac.uk).