1271-28-9Relevant academic research and scientific papers
HETEROMETALL-ZWEIKERNKOMPLEXE AUS DEN TRIPELDECKERSANDWICH-VERBINDUNGEN BF4 UND CYCLOPENTADIENYLMETALLBISTHIOLATEN. KRISTALLSTRUKTUR UND SPIN-CROSSOVER-VERHALTEN VON t)2Ni(C5H4R)>BF4
Werner, H.,Ulrich, B.,Schubert, U.,Hoffmann, P.,Zimmer-Gasser, B.
, p. 27 - 42 (1985)
The tripledecker sandwich complex BF4 (I) reacts with (C5H5)2Ti(SR)2 (R=Me, Ph) and (C5H5)2Mo(SR)2 (R=Me, Ph, But) to produce the dinuclear heterometallic compounds BF4 (V, VI, XI-XIII).The temperature dependence of the 1H NMR spectra of the Ti-Ni complexes V, VI is best explained by an inversion at the sulfur atoms of the bridging SR units which, above +35 deg C, occurs rapidly.The chemical shifts of the 1H and 13C NMR signals of the cyclopentadienyl ligand coordinated to nickel in the compounds t)2Ni(C5H4R)>BF4 (XIII: R=H, XIV: R=Me) are also strongly temperature-dependent presumably due to an equilibrium between a diamagnetic low-spin and a paramagnetic high-spin isomer.Molecular orbital calculations indicate that the spin crossover is probably a consequence of a flattening at the sulfur atoms caused by the t-butyl substituents.The X-ray structural analysis of XIII shows the presence of a folded four-membered MoS2Ni ring having the t-butyl groups on the inside.In accordance with the MO calculatins, the sulfur atoms are less pyramidal than in analogous complexes.The NMR spectrum of the compound BF4 (XXIII) which is prepared from C5H5(PMe3)Co(SPh)2 and I, does not vary with the temperature.
Two nickelocenes and ferrocene in a rigid cis/trans chain
Herker, Martin,K?hler, Frank H.,Schwaiger, Markus,Weber, Bernd
, p. 266 - 273 (2002)
With the aim of studying the conformation of bridged paramagnetic metallocenes and the conformation-dependent electron spin delocalization therein, a trimetallic model compound was synthesized. First, a nickelocene bonded to cyclopentadienyl (Cp) anion by
Triple-decker complexes XIV. Reactions of iron carbonyls with the triple-decker sandwich complexes (η5-C5H5)Ni(μ,η5-C2B2C)M(η5-C5H5), (M = Co, Ni). Replacement of (η5-C5H5)Ni by and insertion of the Fe(CO)3 fragment into the (η5-C5H5)-Ni bond
Edwin, Joseph,Whiteley, Mark W.,Herter, Wilfried,Siebert, Walter
, p. 329 - 338 (1990)
The reactions of Fe2(CO)9 with triple-decker sandwich complexes containing the 2-methyl-1,3,4,5-tetraethyl or the 4,5-diethyl-1,3-dimethyl derivatives of the 2,3-dihydro-1,3-diborole heterocycle C2B2C (4a,b) as a bridging ligand have been investigated.The paramagnetic triple-deckers, 32 valence electron (VE) 5-C5H5)Ni(μ,η5-C2B2C)5-C5H5)> (8a) and 33 VE 5-C5H5)Ni(μ,η5-C2B2C)Ni(η5-C5H5)> (9b) react with Fe2(CO)3, or insertion of Fe(CO)3 into the (η5-C5H5)-Ni bond.Thus, reaction of 8a with Fe2(CO)9 proceeds via Fe(CO)3 insertion into the (η5-C5H5)-Ni bond to yield th'etrinuclear carbonyl-bridged complex 5-C5H5)FeCO(μ-CO)2Ni(μ,η5-C2B2C)Co(η5-C5H5)> (10a), and subsequently the tetranuclear 5-C5H5)Co(μ,η5-C2B2C)Ni(μ-CO)>2> (12a), and also via replacement of (η5-C5H5)Ni to give the triple-decker 5-C5H5)Co(μ,η5-C2B2C)Fe(CO)3> (13a). 33 VE 9b reacts with Fe2(CO)9 to give initially 5-C5H5)Ni(μ,η5-C2B2C)Fe(CO)3> (14b); subsequent reactions lead to the carbonyl-bridged 5-C5H5)Fe(CO)(μ-CO)2Ni(μ,η5-C2B2C)Fe(CO)3> (15b), the tetra-decker 5-C2B2C)>2Ni> (16b), and the triple-decker 5-C5H5)Fe(μ,η5-C2B2C)Fe(CO)3> (17b).The unsymmetrical triple-decker complexes 14a and 14b have been made independently by stacking the Ni-sandwich complexes 20a and 20b with an Fe(CO)3 fragment.A close chemical relationship between 32 VE 8a and 20 VE nickelocene has been established, and may be rationalised by consideration of electronic structures.
Photolytisch induzierte Erzeugung und komplexchemische Stabilisierung eines Molybdaen-Arsen-Dreifachbindungssystems; Roentgenstrukturanalysen der Cluster μ3-AsCp3Mo2Ni(CO)4, As2Cp6Mo4Ni2(CO)7 und μ3-AsCpMoPt2(CO)4(PPh3)2
Gorzellik, Marc,Nuber, Bernhard,Bohn, Thomas,Ziegler, Manfred L.
, p. 173 - 186 (1992)
Cophotolysis of μ3-AsCp3Mo3(CO)6 (1) and Cp2Ni2(CO)2 (2) yields the clusters μ3-AsCp3Mo2Ni(CO)4 (3) and As2Cp6Mo4Ni2(CO)7 (4).Cophotolysis of 1 with Pt(C2H4)(PPh3)2 (5) leads to the butterfly cluster μ3-AsCpMoPt2(CO)4(PPh3
ZUR REAKTIVITAET KOMPLEXGEBUNDENER CARBOCYCLEN XV. NEUE WEGE ZU INDENYL-DIOLEFIN-KOMPLEXEN VON COBALT UND RHODIUM
Salzer, A.,Taeschler, C.
, p. 261 - 266 (1985)
The formation of (indenyl)rhodium(diolefin) complexes is described, using bis(indenyl) magnesium.On protonation of these complexes an η5-η6 shift of the indenyl ligand is observed.The corresponding cobalt complexes are obtained by li
Transition metal azolates from metallocenes. Part 3: Polymeric manganese(II) and nickel(II) pyrazolates; synthesis, characterization, and magnetochemistry
Storr, Alan,Summers, David A.,Thompson, Robert C.
, p. 1130 - 1137 (1998)
Direct reactions of nickelocene and manganocene with molten pyrazoles in an inert atmosphere or under vacuum have led to the isolation of the following metal pyrazolate compounds: [Ni(4-Xpz)2](x) (where X = H, Cl and pz = pyrazolate); [M(4-Xdmp
Some reactions of Ni-Mo and Ni-W propargylic cations with nucleophiles
Chetcuti, Michael J.,McDonald, Steven R.
, p. 1882 - 1889 (2004)
Preliminary reactions of the metal stabilized carbocationic species [(η-C5H5)Ni(μ-η2(Ni), η3(Mo)-HC2CMe2)Mo (CO)2(η-C5H4Me)]+ BF4
Chemistry of the interaction of some metal carbonyl clusters with metal oxide surfaces. [CpFe(CO)]4, Cp3Ni3(CO)2, and [CpNi(CO)]2 on alumina
Tessier-Youngs, Claire,Correa, Fernando,Pioch, Daniel,Burwell Jr., Robert L.,Shriver, Duward F.
, p. 898 - 903 (1983)
The nature of the interactions between [CpFe(CO)]4, Cp3Ni3(CO)2, and [CpNi(CO)]2 with nearly fully dehydroxylated alumina were investigated by infrared spectroscopy, gas evolution, and other chemical means. A donor-acceptor interaction occurs between a carbonyl oxygen and the surface Al3+ in the case of [CpFe(CO)]4 and Cp3Ni3(CO)2 and possibly in the case of [CpNi(CO)]2. The stability of these simple surfaces adducts increases in the order [CpNi(CO)]2 3Ni3(CO)2 4 with the γ-Al2O3-[CpFe(CO)]4 adduct being stable for weeks and the adduct with [CpNi(CO)]2 rapidly decomposing to Ni(CO)4, CO, and other products. The chemistry of these metal clusters with an active alumina surface strongly parallels the reactions with aluminum bromide.
Electrochemical synthesis of ?-cyclopentadienyl(nitrosyl)nickel complexes
Shirokii, V. L.,Knizhnikov, V. A.,Sutormin, A. B.,Maier, N. A.,Andrianov, Yu. A.,Sedova, L. G.
, p. 1061 - 1062 (1994)
The dependence of the yield of ?-cyclopentadienyl(nitrosyl)nickel on the conditions of its electrochemical synthesis from cyclopentadiene under an atmosphere of nitric oxide has been studied with the use of a nickel anode. the general character of the reaction has been demonstrated by its extention to monosubstituted ethyl-, isopropyl-, and benzoylcyclopentadienes. - Key words: cyclopentadienyl(nitrosyl)nickel, electrochemical synthesis; nickelocene.
Synthesis method of nickelocene
-
Paragraph 0010; 0011; 0012, (2019/08/12)
The invention discloses a synthesis method of nickelocene. The synthesis method of nickelocene comprises the following steps: step 1, dissolving 140-160 g of nickel chloride hexahydrate in 400-600 mlof ammonia water, and carrying out a reaction for 8-10 hours by stirring; step 2, after the reaction in the step 1 is ended, filtering the substances obtained in the reaction, carrying out drying by suction, carrying out washing with ethyl alcohol or n-hexane, and carrying out drying to obtain 70-90 g of a product hexamine nickel dichloride; step 3, putting 15-19 g of sodium metal into 400-600 mlof tetrahydrofuran for a reaction, carrying out cooling, then dropwise adding 50-60 g of cyclopentadiene monomers, and adding 70-90 g of the hexamine nickel dichloride obtained in the step 2 after dropwise adding is completed, and carrying out refluxing for 8-10 hours; and step 4, evaporating the reactant obtained after refluxing, removing the solvent evaporating, carrying out a sublimating reaction to obtain 60-80 g of dark green nickelocene crystals, and carrying out closed storage. The synthesis method disclosed by the invention has the advantages that types of the raw materials required for reactions are few, operation is relatively simple and convenient, purity is high, and strict requirements of electronic chemicals on product quality are well met.
