Synthesis and structure of a terminal dinitrogen complex of nickel

2005 ◽  
Vol 83 (4) ◽  
pp. 328-331 ◽  
Author(s):  
Rory Waterman ◽  
Gregory L Hillhouse
Keyword(s):  
Crystal Structure ◽  
Petroleum Ether ◽  
Key Words ◽  
X Ray ◽  
Dinitrogen Complex

Reaction of petroleum ether solutions of [(dtbpe)Ni]2(η2,µ-C6H6) (1, dtbpe = 1,2-bis(di-tert-butylphosphino)ethane) with triphenylphosphine under a dinitrogen atmosphere gives the Ni(0) dinitrogen adduct (dtbpe)Ni(N2)(PPh3) (2), which can be isolated as dark red crystals in 87% yield. The X-ray crystal structure of 2 reveals pseudotetrahedral geometry about Ni and a terminal dinitrogen ligand with Ni—N(1) = 1.830(2) Å, N(1)—N(2) = 1.112(2) Å, and Ni-N(1)-N(2) = 177.5(2)°. Key words: dinitrogen, nickel, X-ray.

The Reaction of Bis[bis(trimethylsilyl)amino]germylene with Bromocyanogen and the Crystal Structure of Bis[bis(trimethylsilyl)amino]bromocyanogermane

1998 ◽  
Vol 53 (1) ◽  
pp. 9-12 ◽  
Author(s):  
Svetlana N. Nikolaeva ◽  
Evgeni V. Avtomonov ◽  
Jörg Lorberth ◽  
Valery S. Petrosyan
Keyword(s):  
Crystal Structure ◽  
Nmr Spectroscopy ◽  
Petroleum Ether ◽  
X Ray

Bis[bis(trimethylsilyl)amino)]germylene (1) reacts with bromocyanogen to give bis[bis(trimethylsilyl)amino]bromocyanogermane (2). 2 crystallises from petroleum ether as a colourless solid which has been characterised by IR, 1H, 13C, 29Si NMR spectroscopy, ele­mental analysis and X-ray diffractometry.

The structure of the tetrachlorohydroxotellurate(IV) anion in KTeCl4(OH)•0.5H2O and KTeCl4(OH)

1991 ◽  
Vol 69 (4) ◽  
pp. 648-652 ◽  
Author(s):  
J. B. Milne ◽  
E. J. Gabe ◽  
C. Bensimon
Keyword(s):  
Crystal Structure ◽  
Key Words ◽  
Vibrational Spectroscopy ◽  
X Ray ◽  
Hydroxo Group

Three compounds containing the tetrachlorohydroxotellurate(IV) anion, [Formula: see text] K[TeCl4(OH)]•0.5H2O, and K[TeCl4(OH)], have been prepared. The crystal structure of K[TeCl4(OH)]•0.5H2O has been determined. The structure contains isolated square pyramidal TeCl4(OH)− anions with OH axial. Vibrational spectroscopy shows that [Formula: see text] and K[TeCl4(OH)]•0.5H2O both contain isolated anions but that, in K[TeCl4(OH)], the anion is polymerized with chloride bridging. The hydroxo group, like the fluoro group, acts to hinder coordination at the site trans to it on Te(IV). Key words: tellurium(IV) complexes, chlorotellurate(IV), X-ray structure, vibrational spectroscopy.

Geminal bis(hypersilyl) compounds — the synthesis and structure of bis[tris(trimethylsilyl)silyl]silanes

2000 ◽  
Vol 78 (11) ◽  
pp. 1399-1404
Author(s):  
Thoralf Gross ◽  
Helmut Reinke ◽  
Hartmut Oehme
Keyword(s):  
Crystal Structure ◽  
Key Words ◽  
Trifluoromethanesulfonic Acid ◽  
Molar Ratio ◽  
Coupling Reactions ◽  
Subsequent Reaction ◽  
X Ray ◽  
A Value ◽  
Spatial Demand

Protodesilylation of diphenylsilane with trifluoromethanesulfonic acid and subsequent reaction of the obtained bis(trifluoromethanesulfonyloxy)silane with tris(trimethylsilyl)silyllithium (1) (molar ratio 1:2) afforded bis[tris(trimethylsilyl)silyl]silane (8). Methyl-bis[tris(trimethylsilyl)silyl]silane (3) and phenyl-bis[tris(trimethylsilyl)silyl]silane (10) were obtained by coupling reactions of 1 with MeHSiCl2 or PhHSiCl2, respectively, (2:1). By treatment with HCBr3, the H-silanes 3, 8, and10 were converted into the bromosilanes [(Me3Si)3Si]2SiR1R2 (9: R1 = R2 = Br; 11: R1 = Me, R2 = Br; 12: R1 = Ph, R2 = Br). X-ray crystal structure analyses, performed for 3, 10 and 12, confirmed the expected distortions of the molecular skeletons of the compounds. Thus, e.g., in 10, the spatial demand of the two extended hemispherical hypersilyl groups forces a widening of the Si-Si-Si angle at the central Si atom to a value of 128.3°.Key words: silanes, sterically congested, bis(hypersilyl)silanes, hypersilylsilanes, bis(hypersilyl)germanes, tris(trimethylsilyl)silylsilanes.

Crystal structure and ferromagnetic behavior of a cis-Co(II) complex with nitronyl nitroxide

2000 ◽  
Vol 78 (3) ◽  
pp. 322-327
Author(s):  
Bai-Wang Sun ◽  
Qi-Hua Zhao ◽  
Dai-Zheng Liao ◽  
Zong-Hui Jiang ◽  
Shi-Ping Yan ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Magnetic Property ◽  
Charge Transfer ◽  
Key Words ◽  
Nitroxide Radical ◽  
Ferromagnetic Behavior ◽  
Nitronyl Nitroxide ◽  
X Ray ◽  
Ferromagnetic Exchange ◽  
A Charge

Bis(hexafluoroacetylacetonate)cobalt(II), Co(hfac)2, reacted with the nitronyl nitroxide radical 2-(4-methylphenyl)-4,4,5,5-tetramethylimidazoline-1-oxyl-3-oxide, NITPhMe, to yield an octahedral adduct of formula Co(hfac)2(NITPhMe)2. The X-ray crystal structure shows that it crystallizes in the space group P1, with a = 9.837(3), b = 11.618(3), c = 20.502(4) Å, α = 81.22(2), β = 87.93(2), γ = 72.24(3)º, V = 2205(1) Å3, Z = 2. The mechanism of ferromagnetic exchange between cobalt(II) and the radical can be qualitatively understood in terms of a charge-transfer interaction (J being 25.7 cm-1, the Hamiltonian is written in the form H = -2J(SRad1·SCo + SCo·SRad2)).Key words: crystal structure, cobalt(II) complex, nitronyl nitroxide, magnetic property.

Synthesis and X-ray crystal structure determination of 3,4-diphenyl-6-(diphenylmethyl)-1,5-dioxa-2-thiane-2-oxide

1991 ◽  
Vol 69 (2) ◽  
pp. 185-188 ◽  
Author(s):  
L. Breau ◽  
N. K. Sharma ◽  
I. R. Butler ◽  
T Durst
Keyword(s):  
Crystal Structure ◽  
Key Words ◽  
Structure Determination ◽  
Title Compound ◽  
Heterocyclic Ring ◽  
Ring System ◽  
Sulfuryl Chloride ◽  
Similar Treatment ◽  
X Ray

Erythro and threo-1,2-diphenyl-2-tert-butylsulfinylethanols 5 and 8 were prepared from the condensation of the α-lithio derivative of benzyl-tert-butyl sulfoxide with benzaldehyde. Reaction of 5 with sulfuryl chloride gave the title compound, (2R*,3S*,4R*,6R*)-3,4-diphenyl-6-(diphenylmethyl)-1,5-dioxa-2-thiane-2-oxide 6, the first representative of a new heterocyclic ring system. Similar treatment of 8 resulted in the formation of 7, a stereoisomer of 6. This same compound was also obtained by photolysis of 6. In both 6 and 7 the S=O bond is in an axial orientation. Key words: sulfuryl chloride, reaction with β-hydroxy sulfoxides; 1,2-diphenyl-tert-butylsulfinylethanol; β-hydroxysulfoxides; β-sultines; N-chlorosuccinimide, reaction with β-hydroxysulfoxides.

The selective complexation of adamantane nitriles by tungsten pentacarbonyl

1996 ◽  
Vol 74 (1) ◽  
pp. 107-113 ◽  
Author(s):  
Valerie J. Jefford ◽  
Melbourne J. Schriver ◽  
Michael J. Zaworotko
Keyword(s):  
Crystal Structure ◽  
Key Words ◽  
Crystal Data ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
X Ray ◽  
Pure Compounds ◽  
Semi Empirical ◽  
Oxygen Atoms ◽  
Selective Complexation

Adamantyl-1,3,4-oxathiazol-2-one is usually prepared as a mixture with 1-adamantanecarbonitrile. To separate these two compounds the mixture is reacted with thf•W(CO)5, which selectively forms a complex with the nitrile. The resulting mixture can then be readily separated into pure compounds by sublimation. Characterization data are presented, including the X-ray crystal structure of the nitrile complex, which can be prepared directly from the reaction of the adamantyl nitrile and thf•W(CO)5. (Crystal data for C16H15NO5W: orthorhombic, space group Pmcn, a = 10.5869(19) Å, b = 14.0622(22) Å, c = 23.342(4) Å, V = 3475.0(11) Å, Z = 8, R = 0.042.) The nitrile can be recovered from the complex by reaction with P(C6H5)3 followed with separation by sublimation. The reaction of the related 1-cyano-3-(1,3,4-oxathiazol-2-on-5-yl)-adamantane with thf•W(CO)5 yields a complex in which the site of coordination is shown spectroscopically to be the nitrile moiety. Semi-empirical calculations at the PM3 level indicate that the oxathiazolone heterocycle may be a poor ligand due to the influence of the exo- and endo-cyclic oxygen atoms. Key words: oxathiazolone, nitrile, tungsten, complexation, selectivity, adamantane.not available

scholarly journals Bipyridylacetylenes 1: the synthesis of some bipyridylacetylenes via the palladium-catalyzed coupling of acetylenes with 2,2′-dibromobipyridyl, and the single crystal X-ray structure of 6,6′-bisphenylethynyl-2,2′-bipyridine

1991 ◽  
Vol 69 (7) ◽  
pp. 1117-1123 ◽  
Author(s):  
Ian R. Butler ◽  
Chantal Soucy-Breau
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Key Words ◽  
Dihedral Angle ◽  
Palladium Catalysis ◽  
Crystal Data ◽  
X Ray ◽  
Acetylenic Bond ◽  
Palladium Catalyzed

The synthesis of a series of 6,6′-diethynyl-2,2′-bipyridyls from the palladium-catalyzed coupling of 6,6′-dibromo-2,2′-bipyridine with a series of arylacetylenes is reported. The single crystal X-ray structure of 6,6′-phenylethynyl-2,2′-bipyridyl was determined. Crystal data: monoclinic, A2/a, with cell constants a = 10.0385(4), b = 9.2166(4), c = 21.4130(8) Å, and β = 102.981(3)°; Dcalc. = 1.226 g cm−3, Z = 4, Rf = 0.045, S = 1.22, using 886 reflections of the 1443 unique reflections. The packing diagram indicates essentially that the molecules pack in a layered assembly with the nitrogen atoms of the dipyridyl groups on opposite sides and with a dihedral angle of 59.85(16)° between the pyridyl and phenyl groups. The acetylenic bond distances are normal. Key words: acetylene, palladium, catalysis, coupling, monomers, crystal structure.

The crystal structure of W(CO)5piperidine: Implications for photoreactivity of W(CO)5L complexes

1991 ◽  
Vol 69 (12) ◽  
pp. 2033-2037 ◽  
Author(s):  
Carol Moralejo ◽  
Cooper H. Langford ◽  
Peter H. Bird
Keyword(s):  
Crystal Structure ◽  
Bond Length ◽  
Key Words ◽  
Triplet Excitation ◽  
X Ray ◽  
Bond Lengths ◽  
Model Based ◽  
Equatorial Bond ◽  
Reverse Trend ◽  
Back Donation

The X-ray crystal structure of W(CO)5piperidine is reported and assignments are given for the LF and CT band of W(CO)5piperidine and W(CO)5pyridine. The [Formula: see text](axial), and [Formula: see text] (equatorial) bond lengths for W(CO)5pip are 2.330(5), 1,963(6), and 2.04(7), respectively. The longer [Formula: see text] bond length in W(CO)5pip compared to W(CO)5pyr corresponds to greater photoreactivity observed under LF triplet excitation for W(CO)5pip but cannot account for the reverse trend observed under LF singlet irradiation. The structure also fails to support a model based on differences in π back donation from W. It is concluded that differences between singlet and triplet photoreaction originate in the relative rates of radiationless decay. Key words: W(CO)5piperidine, photoreactivity, crystal structure.

The life, death, and ROMP activity of ruthenium complexes containing the basic, chelating diphosphine bis(dicyclohexyl)-1,4-phosphinobutane

2001 ◽  
Vol 79 (5-6) ◽  
pp. 958-963 ◽  
Author(s):  
Dino Amoroso ◽  
Glenn PA Yap ◽  
Deryn E Fogg
Keyword(s):  
Crystal Structure ◽  
Key Words ◽  
Ring Opening ◽  
Chlorinated Solvents ◽  
Metathesis Polymerization ◽  
Space Group ◽  
X Ray ◽  
Vacuum Atmosphere ◽  
Benzylidene Derivative

Reaction of RuCl2(PPh3)3 with bis(dicyclohexyl)-1,4-phosphinobutane (dcypb) under N2 affords access to a formerly elusive family of dcypb complexes based on the RuCl2(PP) core. Under Ar or vacuum atmosphere, decomposition occurs via Ru-promoted dehydrogenation of the dcypb ligand. While the N2-stabilized species [RuCl2(dcypb)]2(N2) (4a) is easily handled under N2 in nonchlorinated solvents, reaction with chlorinated solvents rapidly yields paramagnetic Ru2Cl5(dcypb)2 (5). The N2 ligand within 4a is readily displaced under H2 or CO atmosphere, yielding Ru2Cl4(dcypb)2(H2) (6) or RuCl2(dcypb)(CO)2, the latter as a mixture of ccc-(7) and tcc-(8) isomers. Benzylidene derivative RuCl2(dcypb)(CHPh) (1a), prepared in situ by reaction of 4a with PhCHN2, proves exceptionally active in ring-opening metathesis polymerization (ROMP) of norbornene. The X-ray crystal structure of 5 is reported: triclinic, a = 13.390(2), b = 15.726(2), c = 19.524(2) Å, α = 77.325(2), β = 70.964(2), γ = 73.478(2)°, with space group P[Formula: see text] and Z = 2.Key words: ruthenium, alkylphosphine, dehydrogenation, carbene, metathesis, crystal structure.

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