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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 adipoÂnitrile with [Zr(C10H15)2([eta]2-Me3SiC2SiMe3)]. IntraÂmolecular nitrile-nitrile couplings and deprotonation of the substrate produced the (1-imino-2-enimino)ÂcycloÂpentane ligand, which functions as a five-membered bridge between the two metal atoms. The ZrIV atom exhibits a distorted tetraÂhedral coordination sphere defined by two pentaÂmethylÂcycloÂpentaÂdienyl ligands, by the imino unit of one (1-imino-2-enimino)ÂcycloÂpentane and by the enimino unit of the second (1-imino-2-enimino)ÂcycloÂpentane. The cycloÂpentane ring of the ligand shows an envelope conformation. The asymmetric unit contains one half of the complex and one half of the hexane solvent molÂecule, both being completed by the application of inversion symmetry. One of the pentaÂmethylÂcycloÂpentaÂdienyl 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 molÂecules are packed into rods extending along [100], with the solvent molÂecules located in between. The rods are arranged in a distorted hexaÂgonal packing.
- ItemSynthesis and crystallographic characterization of [2,2-bisÂ(η5-pentaÂmethylÂcycloÂpentaÂdienÂyl)-3,4-bis(triÂmethylÂsilÂyl)-2-zirconaÂfuran-5-one-κO5]triisobutylÂaluminium(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 furanÂone unit, [AlZr(C10H15)2(C4H9)3(C9H18O2Si2)], is reported. On reacting a zirconaÂfuranÂone with two equivalents of HAl(i-Bu)2, disproportionation of the Lewis acid results in the formation of a triisoÂbutylÂaluminium fragment, Al(i-Bu)3, which coordinates to the exocyclic carbonyl O atom of the zirconaÂfuranÂone ring. Single-crystal X-ray diffraction reveals that the zirconaÂfuranÂone 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).