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Pyrrolyl, hydroxo, and carbonate organometallic derivatives of nickel(II). Crystal and molecular structure of [Ni(CH2C6H4-o-Me)(PMe 3)(μ-OH)]2·2,5-HNC4H 2Me2

Pyrrolyl-organometallic derivatives of Ni(II), of composition Ni(R)(NC4H2X2)(PMe3)2 (X = H (1a-5a), 2,5-Me (1b-5b); R = Me (1), CH2SiMe3 (2), CH2CMe3 (3), CH2CMe2Ph (4), 2,4,6-C6H2Me3 (5)), have been obtained by treatment of the complexes trans-Ni(R)Cl(PMe3)2 with the sodium salt of the pyrrolyl ligand. The action of wet CO2 upon solutions of 2a,b provides the carbonate Ni2(CH2SiMe3)2(CO 3)(PMe3)3 (10), possibly through the intermediacy of a dimeric hydroxide, [Ni(CH2SiMe3)-(PMe3)(μ-OH)]2 (6). Hydroxides related to 6, [Ni(R)(PMe3)(μ-OH)]2 (R = CH2CMe2Ph (7), CH2C6H5 (8)), have been produced by reacting the corresponding monoalkyl chlorides with powdered NaOH and have been shown to react with CO2 with formation of carbonates analogous to 10, Ni2R2(CO3)(PMe3)3 (R = CH3 (9), CH2SiMe3 (10), CH2C6H5 (11), C6H5 (12)). The hydroxides readily form solid-state adducts, when crystallized in the presence of pyrrole or 2,5-dimethylpyrrole. NMR studies show these adducts are completely dissociated in solution, but an O?H-N hydrogen-bonding interaction exists in the solid state, as revealed by the results of an X-ray structural determination, carried out with the o-methylbenzyl complex [Ni(CH2C6H4-o-Me)-(PMe 3)(μ-OH)]2·2,5-HNC4H 2Me2. The crystals are monoclinic, space group C2/c, with cell dimensions a = 15.598 (6) A?, b = 12.655 (7) A?, c = 17.705 (6) A?, β = 111.72 (4)°, V = 3243.7 A?3, and Z = 4. The structure consists of dinuclear Ni2(η1-CH2C6H 4-o-Me)2(PMe3)2(μ-OH)2 molecules and of 2,5-dimethylpyrrole molecules of crystallization, all of them showing crystallographic 2-fold symmetry. The Ni dimers have dihedral geometry, with the Ni atoms situated in a distorted square-planar environment.

Synthesis and X-ray Structure of the Nickelabenzocyclopentene Complex . Reactivity Toward Simple, Unsaturated Molecules and the Crystal and Molecular Structure of the Cyclic Carboxylate

Facile cyclometalation to the nickelacyclopentene complex (1) occurs upon alkylation of NiCl2(PMe3)2 with 2 equiv of Mg(CH2CMe2Ph)Cl, in the presence of traces I(1-).Compound 1 has been fully characterized by spectroscopic and X-ray studies.Its

Intrazeolite Chemistry of Nickel(0) Complexes and Ni(0,II) Clusters Studied by EXAFS, Solid-State NMR, and FT-IR Spectroscopy

Adsorption, thermal decomposition, and reactivity of Ni(CO)4 in the cage system of dehydrated zeolite Y has been studied with EXAFS and near-edge spectroscopies, in particular monitoring changes in oxidation states and Ni ligation.Ni(CO)4 is adsorbed as an intact molecule in cation-free zeolite Y, LiY, and NaY.Symmetry changes of the molecule in LiY and NaY are assigned to the formation of cation--OC-Ni bridges.Thermal treatment of the Ni(CO)4/NaY adduct leads to loss of CO concomitant with the formation of a bimodal Ni phase.A major part of the Ni forms small clusters (approximately 0.5 to 1.5 nm), in addition to larger crystallites (5-30 nm), sticking at the outer surface of the zeolite crystals.Oxidation of Ni(CO)4/NaY to NiO/NaY with molecular oxygen occurs almost to completion below 295 K.The small NiO particles are stable to sintering up to 670 K.Nickel-phosphine/NaY adducts have been prepared by direct adsorption from solution , and by synthesis inside the NaY supercage x>.The NaY/Ni(CO)3(PPh2CHMe2) adduct is a ship-in-a-bottle complex, i.e., the Ni complex is too large to exit the zeolite supercage.The substitution of carbonyl ligands by phosphines was monitored in the near-edge and EXAFS modulations as well as with (31)P MAS NMR.EXAFS is an excellent method to monitor ligand coordination and provides information that is complimentary to IR spectroscopy.

Electrochemical Syntheses, V. Phosphane Substituted Metal Carbonyls of the Iron Group Elements

The electrochemical synthesis of iron, cobalt, and nickel carbonyl derivatives with phosphane ligands from metal anodes is described. - Keywords: Electrochemical Synthesis, Metal Carbonyls, Phosphane Ligands