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- ItemCrystal structure of bis{μ2-[(2-iminocyclopentylidene)methylidene]azanido-κ2 N:N'}bis[(η5-pentamethylcyclopentadienyl)zirconium(IV)] hexane monosolvate(Chester : International Union of Crystallography, 2015) Becker, Lisanne; Spannenberg, Anke; Arndt, Perdita; Rosenthal, UweThe title compound, [Zr2(C10H15)4(C6H6N2)2]·C6H14, was obtained by the stoichiometric reaction of adiponitrile with [Zr(C10H15)2([eta]2-Me3SiC2SiMe3)]. Intramolecular nitrile-nitrile couplings and deprotonation of the substrate produced the (1-imino-2-enimino)cyclopentane ligand, which functions as a five-membered bridge between the two metal atoms. The ZrIV atom exhibits a distorted tetrahedral coordination sphere defined by two pentamethylcyclopentadienyl ligands, by the imino unit of one (1-imino-2-enimino)cyclopentane and by the enimino unit of the second (1-imino-2-enimino)cyclopentane. The cyclopentane ring of the ligand shows an envelope conformation. The asymmetric unit contains one half of the complex and one half of the hexane solvent molecule, both being completed by the application of inversion symmetry. One of the pentamethylcyclopentadienyl ligands is disordered over two sets of sites with a refined occupancy ratio of 0.8111 (3):0.189 (3). In the crystal, the complex molecules are packed into rods extending along [100], with the solvent molecules located in between. The rods are arranged in a distorted hexagonal packing.
- ItemSynthesis and crystallographic characterization of [2,2-bis(η5-pentamethylcyclopentadienyl)-3,4-bis(trimethylsilyl)-2-zirconafuran-5-one-κO5]triisobutylaluminium(Chester : International Union of Crystallography, 2018-3-27) Burlakov, Vladimir V.; Bogdanov, Vyacheslav S.; Arndt, Perdita; Spannenberg, Anke; Rosenthal, Uwe; Beweries, Torsten; Shur, Vladimir B.The crystal structure of the title zwitterionic zirconocene complex containing a furanone unit, [AlZr(C10H15)2(C4H9)3(C9H18O2Si2)], is reported. On reacting a zirconafuranone with two equivalents of HAl(i-Bu)2, disproportionation of the Lewis acid results in the formation of a triisobutylaluminium fragment, Al(i-Bu)3, which coordinates to the exocyclic carbonyl O atom of the zirconafuranone ring. Single-crystal X-ray diffraction reveals that the zirconafuranone ring remains intact with coordination of the aluminium to the exocyclic O atom. One of the i-butyl groups is disordered over two sets of sites, with an occupancy ratio of 0.731 (3):0.269 (3).