Abstract
A new compound comprising a Ni(III) di-carbollide cluster anion [H(Phen)2][Ni(B9C2H11)2], Phen = 1,10-phenanthroline, has been prepared and structurally characterized. Crystal data: C28H39B18N6Ni, M = 684.92, monoclinic, space group P21/n; unit cell parameters: a = 19.337(3) Å, b = 6.9968(8) Å, c = 25.630(4) Å; β = 101.69(1)°; V = 3395.8(9) Å3, Z = 4, d calc = 1.340 g/cm3, T = 293 K, F(000) = 1412, μ = 0.602 mm−1. The structure was solved by the direct and Fourier methods and refined in the full-matrix anisotropic approximation (isotropic for hydrogen atoms) to final agreement factors R 1 = 0.0372, wR 2 = 0.0887 for 4136 I hkl ⩾ 2σI from 5445 measured I hkl (an Enraf-Nonius CAD-4 diffractometer, λMoK α , graphite monochromator, ω-scanning). The structure is built from [H(Phen)2]+ cations and [Ni(C2B9H11)2]− anions. The anions have a usual for commo-metal carboranes sandwich structure consisting of two icosahedra {NiC2B9} sharing a common Ni vertex. EPR technique shows that nickel ion has the electron state 3d 7 with S = 1/2. The angular dependence of single-crystal EPR spectra was used to calculate g-factors (g 1 = 2.0803, g 2 = 2.0229 and g 3 = 1.9810) and to assign principal values of the g-tensor to the directions in the crystal structure, in accord with which g 1 is directed along the Cb-Ni-Cb axis, while the direction and the value of g 2 is determined by a distortion introduced by the cation. The compound has been characterized by IR and Raman spectroscopy.
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V. V. Volkov, E. A. Il’inchik, B. A. Kolesov, et al., Zh. Strukt. Khim., 37, No. 6, 1060–1071 (1996).
V. V. Volkov, T. M. Polyanskaya, C. Price, et al., Khimiya v interesakh ustoichivogo razvitiya, 8, Nos. 1/2, 229–236 (2000).
T. M. Polyanskaya, V. V. Volkov, and M. K. Drozdova, Zh. Strukt. Khim., 44, No. 4, 690–700 (2003).
V. V. Volkov, V. N. Ikorskii, M. K. Drozdova, et al., ibid., No. 5, 890–896.
T. M. Polyanskaya, V. V. Volkov, and M. K. Drozdova, ibid., 46, No. 4, 730–740 (2005).
R. Hoffmann and W. N. Lipscomb, J. Chem. Phys., 36, No. 12, 3489–3493 (1962).
J. Aihara, J. Am. Chem. Soc., 100, No. 11, 3339–3342 (1978).
M. F. Hawthorne, D. C. Young, T. D. Andrews, et al., ibid., 90, No. 4, 879–896 (1968).
E. L. Muetterties (ed.), Boron Hydride Chemistry, Academic Press, New York (1975).
V. A. Nadolinnyi, T. M. Polyanskaya, V. V. Volkov, et al., Koordinats. Khim., 31, No. 6, 403–414 (2005).
A. Altomare, M. C. Burla, M. Camalli, et al., J. Appl. Crystallogr., 32, 115–119 (1999).
G. M. Sheldrick, SHELXL-97, Release 97-2, Univ. Göttingen, Germany (1998).
J. S. Strukl and J. L. Walter, Spectrochim. Acta (A), 27, No. 2, 209–221 (1971).
E. König and K. Madeja, ibid., 23, No. 1, 45–54 (1967).
R. Krishnakumar, G. Aravamudan, M. R. Udupa, et al., J. Chem. Soc., Dalton Trans., No. 11, 2253–2259 (1996).
L. Maresca, G. Natile, and F. P. Fanizzi, J. Am. Chem. Soc., 111, No. 4, 1492/1493 (1989).
K. Hensen, F. Gebhardt, and M. Bolte, Acta Crystallogr., C54, No. 3, 359–361 (1998).
S. Nishigaki, H. Yoshioka, and K. Nakatsu, ibid., B34, No. 3, 875–879 (1978).
F. V. Hansen, R. G. Hazell, C. Hyatt, et al., Acta Chem. Scand., 27, No. 4, 1210–1218 (1973).
P. A. Chetcuti, W. Hofherr, A. Liegard, et al., Organometallics, 14, No. 2, 666–675 (1995).
R. E. Robertson and H. M. McConnell, J. Phys. Chem., 64, No. 1, 70–77 (1960).
Y.-H. Huang, J.-B. Park, M. W. W. Adams, et al., Inorg. Chem., 32, No. 4, 375/376 (1993).
R. J. Wiersema and M. F. Hawthorne, J. Am. Chem. Soc., 96, No. 3, 761–770 (1974).
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Original Russian Text Copyright © 2006 by T. M. Polyanskaya, V. A. Nadolinnyi, V. V. Volkov, E. A. Il’inchik, and M. K. Drozdova
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Translated from Zhurnal Strukturnoi Khimii, Vol. 47, No. 5, pp. 905–916, September–October, 2006.
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Polyanskaya, T.M., Nadolinnyi, V.A., Volkov, V.V. et al. Synthesis, X-ray structural and spectroscopic study of [bis(1,10-phenanthrolinium)](1+) {3,3′-commo-bis-[η5-1,2-dicarba-(3)-nickel(III)-closo-dodecaborate]}(1-), [H(1,10-C12H8N2)2]+{NiIII[η5-(3)-1,2-B9C2H11]2}− . J Struct Chem 47, 894–905 (2006). https://doi.org/10.1007/s10947-006-0406-5
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DOI: https://doi.org/10.1007/s10947-006-0406-5