X-ray crystal structure of the clathrate compound tetrakis[(benzonitrile)(triphenylphosphorane)nickel(0)] · 2 toluene · ~1 n-hexane · ~1 cycloocta-1,5-diene

作者: I.W. Bassi , C. Benedicenti , M. Calcaterra , R. Intrito , G. Rucci

DOI: 10.1016/S0022-328X(00)84165-0

关键词: Double bondRing (chemistry)BenzonitrileMonoclinic crystal systemCyclohexane conformationMoleculeClathrate compoundChemistryCrystal structureCrystallography

摘要: Abstract The preparation and the chemical properties of clathrate compound tetrakis[(benzonitrile)(triphenylphosphorane)nickel(0)] · 2 toluene ~1 n-hexane cycloocta-1,5-diene are described. crystal molecular structure this were determined from X-ray diffractometer data. was solved by direct Fourier methods refined least-squares techniques to R = 0.117 for 3441 independent reflections. crystals monoclinic, space group P21, with Z 2, in a unit cell dimensions 14.680(7), b 28.198(18), c 15.482(8) A, β 118.43(8)°. Eight (NiP(C6H5)3 NCC6H5) formula units present as two tetrameric molecules cell. Each Ni atom tetramer is linked σ bonds P N π NC another benzonitrile molecule. coordination nickel atoms roughly trigonal. form an eight-membered ring boat conformation. NCC groups residues bent NC distances indicate high degree double bond character all these bonds. triphenylphosphorane adopt “propeller”-like Four solvent toluene, 1 n-hexane, per asymmetric

参考文章(14)
F. H. Moore, Analytic constants for atomic scattering factors Acta Crystallographica. ,vol. 16, pp. 1169- 1175 ,(1963) , 10.1107/S0365110X63003054
P.W. Jolly, K. Jonas, C. Krüger, Y.-H. Tsay, The preparation, reactions and structure of bis[bis(tricyclohexylphosphine)nickel] dinitrogen, {[(C6H11)3P]2Ni}2N2 Journal of Organometallic Chemistry. ,vol. 33, pp. 109- 122 ,(1971) , 10.1016/S0022-328X(00)80809-8
Ron S. Dickson, James A. Ibers, .pi.-Bonded azo-transition metal complex. Structure of bis(tert-butyl isocyanide) (azobenzene)nickel(0) Journal of the American Chemical Society. ,vol. 94, pp. 2988- 2993 ,(1972) , 10.1021/JA00764A015
I.W. Bassi, M. Calcaterra, X-ray crystal structure of racemic bis(ethyl fumarate) (acetonitrile)nickel(0) Journal of Organometallic Chemistry. ,vol. 110, pp. 129- 137 ,(1976) , 10.1016/S0022-328X(00)90166-9
G. Germain, P. Main, M. M. Woolfson, The application of phase relationships to complex structures. III. The optimum use of phase relationships Acta Crystallographica Section A. ,vol. 27, pp. 368- 376 ,(1971) , 10.1107/S0567739471000822
I.W. Bassi, C. Benedicenti, M. Calcaterra, G. Rucci, Preparation and x-ray crystal structure of (benzonitrile)tris(triphenylphosphorane)nickel(0) Journal of Organometallic Chemistry. ,vol. 117, pp. 285- 295 ,(1976) , 10.1016/S0022-328X(00)91899-0
G. Wilke, G. Herrmann, Bis-triphenylphosphin-nickel-äthylen und analoge Komplexe Angewandte Chemie. ,vol. 74, pp. 693- 694 ,(1962) , 10.1002/ANGE.19620741705
V. Vand, P. F. Eiland, R. Pepinsky, Analytical representation of atomic scattering factors Acta Crystallographica. ,vol. 10, pp. 303- 306 ,(1957) , 10.1107/S0365110X57000882
K. Jonas, P. Heimbach, G. Wilke, 1,5,9‐Cyclododecatrien‐Komplexe mit Nickel(0) Angewandte Chemie. ,vol. 80, pp. 1033- 1033 ,(1968) , 10.1002/ANGE.19680802411
Karl Fischer, Klaus Jonas, Günther Wilke, Tris(äthylen)nickel(0) Angewandte Chemie. ,vol. 85, pp. 620- 621 ,(1973) , 10.1002/ANGE.19730851408