A. Babai, G. B. Deacon, A. P. Erven, G. Meyer
[3] A. Babai, G. B. Deacon, G. Meyer, Z. Anorg. Allg. Chem.
2004, 630, 399.
[4] G. B. Deacon, I. L. Grayson, Transition Met. Chem. 1982,
X-ray-crystal structure determinations
For all compounds, a hemisphere of data (1° frames in phi and
omega) were collected at 123(1) K using an Enraf-Nonius CCD
area-detector diffractometer (monochromatic Mo-Kα radiation,
7, 97.
[5] D. P. Buxton, G. B. Gatehouse, B. M. Gatehouse, I. L. Gray-
son, S. C. Ney, Aust. J. Chem. 1988, 41, 943.
˚
λ ϭ 0.71073 A), yielding Ntotal collected reflections after inte-
gration and scaling using the DENZO SMN software package [17].
Each data set was merged to N unique reflections (N0 (I>2σ(I))
‘observed’).
[6] G. B. Deacon, K. T. Nelson-Reed, J. Organomet. Chem. 1981,
322; T. W. Hambley, A. R. Battle, G. B. Deacon, E. T.
Lawrenz, G. D. Fallon, B. M. Gatehouse, L. K. Webster, S.
Rainone, J. Inorg. Biochem. 1991, 77, 3; C. Cullinane, G. B.
Deacon, P. R. Dragon, T. W. Hambley, K. T. Nelson, L. K.
Webster, J. Inorg. Biochem. 2002, 89, 293.
[7] (C37 H22 F10 P2 Pt): monoclinic, P21/c, a ϭ 18.214(4), b ϭ
9.9320(13), c ϭ 19.529(4), β ϭ 104.48(2)°, R1 ϭ 0.0357 (0.2548
all data), wR2 ϭ 0.0526 (0.1108 all data), Rint ϭ 0.3586,
GooF ϭ 0.468.
[8] S. J. Dossett, A. Gillon, A. G. Orpen, J. S. Fleming, P. G.
Pringle, D. F. Wass, M. D. Jones, Chem. Commun. 2001, 699.
[9] a) D. H. Farar, G. Ferguson, J.Cryst. Spec. Res. 1982, 12, 465;
b) B. Bovio, F. Bonati, G. Banditelli, Gazz. Chim. Ital. 1985,
115, 613; L. M. Engelhardt, J. M. Patrick, C. L. Raston, P.
Twiss, A. H. White, Aust. J. Chem. 1984, 37, 2193.
[10] R.D. Shannon, Acta Crystallogr. 1980, 12, 180.
[11] T. Appleton, H. C. Clark, L. E. Manzer, Coord. Chem. Rev.
1973, 10, 335.
The structures were solved using Direct Methods and refinedwith
anisotropic thermal parameters for the non-hydrogen atoms by full
matrix least-squares on all F2 data using the SHELX97 [18] and
XSEED [19] software packages. For all compounds hydrogen
atoms were placed geometrically and refined isotropically using the
riding model. A numerical absorption correction was applied to
the data by the programs XϪRED and XϪSHAPE [20, 21]. Crys-
tallographic data and refinement details are given in Table 1.
Although the cis-[Pt(dppm)Cl2] (1) crystals had a regular shape and
showed no signs for twinning under polarized light and in the first
patterns, several crystals had to be measured to obtain a solvable
diffraction data set. Because of weak packing forces, 10 % of the
molecules are disordered, which may explain why a crystal struc-
ture of the well known cis-[Pt(dppm)Cl2] has not been reported
previously. In the Table 2 and Figure 1a, 1b only one of the mol-
ecule-orientations is reported.
[12] L. Pauling, The Nature of the Chemical Bond 3rd Ed., Cornell
Univ. Press, New York 1960.
[13] G. B. Deacon, K. T. Nelson, E. R. T. Tiekink, Acta Crys-
tallogr. 1991, C47, 955.
[14] G. B. Deacon, K. T. Nelson-Reed, J. Organomet. Chem. 1987,
Crystallographic data for the structures have been deposited with
the Cambridge Crystallographic Data Centre, CCDC 291797-
291802. Copies of the data can be obtained free of charge on
application to The Director CCDC, 12 Union Road, Cam-
bridge CB2 1EZ, UK (Fax: ϩ44 (1223)336-033; e-mail for
322, 257.
[15] A. R. Sanger, J. Chem. Soc., Dalton Trans. 1977, 1971.
[16] A. D. Westland, J. Chem. Soc. 1965, 3060.
[17] S. Mackay, C. F. Gilmore, C. Edwards, M. Tremayne, N.
Stewart, K. Shankland, maXus, University of Glasgow, Scot-
land UK, Nonius BV, Delft, The Netherlands and MacScience
Co. Ltd., Yokohama, Japan 1998.
[18] G. M. Sheldrick, SHELXϪ97, Program for the Solution of
Crystal Structures and for the Refinement of Crystal Struc-
tures from Diffraction Data, Göttingen (D), 1997.
[19] L. J. Barbour, XϪSeed v1.5 Ϫ A Software Tool for Supra-
molecular Crystallography, J. Supramol. Chem. 2001, 1, 189.
[20] STOE & Cie GmbH, XϪRed 1.08a: “Data reduction for
STADI4 and IPDS“, Darmstadt, 1996.
inquiry:
deposit@ccdc.cam.ac.uk).
fileserv@ccdc.cam.ac.uk;
email
for
deposition:
Crystal and refinement details for each compound are listed in
Table 1, with selected bond distances and angles in Table 2.
References
[1] G. B. Deacon, P. W. Elliott, A. P. Erven, G. Meyer, Z. Anorg.
Allg. Chem. 2005, 631, 643.
´
[2] R. Uson, J. Fornies, P. Espinet, R. Navarro, L. Fortuno, J.
[21] STOE & Cie GmbH, XϪShape 1.06: “Crystal optimisation
Chem. Soc., Dalton Trans. 1987, 2001.
for numerical absorption correction“, Darmstadt, 1999.
644
zaac.wiley-vch.de
2006 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim
Z. Anorg. Allg. Chem. 2006, 639Ϫ644