M. Barret et al. / Journal of Organometallic Chemistry 587 (1999) 101–103
103
dimethylpyrazol-1-yl) [13] and Ba2(DAP)3[N(SiMe3)2]
(DAP=diazapentadienyl) [14] which also incorporate
p-interactions with cyclic or acyclic conjugated C, N
ligands.
F2 data with Fo\4|(Fo), 281 parameters] R1=0.0487
and wR2=0.1276. Goodness of fit=1.046. The max.
and min. residual densities were 1.211 and −1.171 e
A
−3, respectively. The asymmetric unit (shown in Fig.
,
1, along with the labelling scheme used) was produced
using ORTEX [18].
1. Experimental
Spectra were recorded on the following instruments:
Jeol GX270 (1H-, 13C-NMR), GX400 (209Pb-NMR),
Perkin–Elmer 599B (IR; Nujol mull on KBr plates).
2. Supplementary material
Crystallographic data for the structural analysis have
been deposited with the Cambridge Crystallographic
Data Centre, CCDC No. 118701 for compound 1.
Copies of this information may be obtained free of
charge from The Director, CCDC, 12, Union Road,
Cambridge CB2 1EZ (Fax: +44-1223-336-033 or e-
1.1. Synthesis of 1
Ph3PbCl (0.95 g, 2.0 mmol) in methanol (240 ml) was
added dropwise to
a
well-stirred solution of
[NH4][SCN4Ph] (0.48 g, 2.4 mmol) also in methanol (30
ml). The solution was then refluxed for 3 h, the solvent
removed in vacuo and the residue extracted into ace-
tone. After separation of insolubles, the acetone was
evaporated and the remaining solid recrystallised from
hot methanol to yield 1 (0.84 g, 68%; m.p. 156–8°C).
Anal. Calc. for C25H20N4PbS: C, 48.8 (48.8); H, 3.27
mail:
or
http://
www.ccdc.cam.ac.uk).
References
[1] M. Hill, M.F. Mahon, J.G. McGinley, K.C. Molloy, J. Chem.
Soc. Dalton Trans. (1996) 835.
[2] S. Bhandari, PhD Thesis; University of Bath, Bath, 1998.
[3] D.S. Moore, S.D. Robinson, Adv. Inorg. Chem. 32 (1988) 171.
[4] E.O. John, R.D. Willett, B. Scott, R.L. Kirchmeier, J.M.
Shreeve, Inorg. Chem. 28 (1989) 893.
1
(3.25), N, 8.89 (9.10)%. H-NMR (CDCl3): 7.40–7.86
(m, 20H, C6H5); 13C-NMR: 159.0 (CN4), 136.3, 134.7,
129.9, 129.3, 129.2, 124.5 (C6H5); 207Pb-NMR (100°C;
relation to Et4Pb): 172.2 ppm.
[5] C. Gaffney, P.G. Harrison, J. Chem. Soc. Dalton Trans. (1982)
1055.
1.2. Crystallography
[6] R. Allmann, A. Waskowska, R. Hohlfeld, J. Lorbeth, J.
Organomet. Chem. 198 (1980) 155.
[7] H.O. van der Kooi, W.H. den Brinker, A.J. de Kok, Acta
Crystallogr. Sect. C 41 (1985) 869.
[8] R. Cea-Olivares, O. Jimenez-Sandoval, G. Espinosa-Perez, C.
Silvestru, J. Organomet. Chem. 484 (1994) 33.
[9] R. Cea-Olivares, O. Jiminez-Sandoval, G. Espinosa-Perez, C.
Silvestru, Polyhedron 13 (1994) 2809.
A colourless crystal of approximate dimensions
0.2×0.2×0.2 mm was used for data collection.
Crystal data: C25H20N4PbS, M=615.70, monoclinic,
,
a=11.116(2), b=16.270(3), c=13.055(2) A, i=
3
,
100.49(2)°, U=2321.6(7) A , space group P21/n, Z=4,
D
calc. =1.762 g cm−3, v(Mo–Ka)=7.376 mm−1. Crys-
tallographic measurements were made at 293(2) K on a
CAD4 automatic four-circle diffractometer in the range
[10] A. Goodger; M. Hill, M.F. Mahon, J.G. McGinley, K.C. Mol-
loy J. Chem. Soc. Dalton Trans. (1996) 847.
[11] M. Hill, M.F. Mahon, K.C. Molloy J. Chem. Soc. Dalton Trans.
(1996) 1857.
,
2.02BqB23.92° (u=0.71069 A). Data (3634 indepen-
dent reflections) were corrected for Lorentz and polari-
sation and also for absorption [15]. (Max. and min.
absorption corrections; 1.000, 0.336, respectively). In
the final least squares cycles all atoms were allowed to
vibrate anisotropically. Hydrogen atoms were included
at calculated positions where relevant. The solution of
the structure (SHELX86) and refinement (SHELX93)
[16,17] converged to a conventional [i.e. based on 2532
[12] D. Britton, J.D. Dunitz, J. Am. Chem. Soc. 102 (1981) 2971.
[13] A. Steiner, D. Stalke, Inorg. Chem. 34 (1995) 4846.
[14] W. Clegg, S.J. Coles, E.K. Cope, F.S. Mair, Angew. Chem. Int.
Ed. Eng. 37 (1998) 796.
[15] N. Walker, D. Stewart, Acta Crystallogr. Sect. A 39 (1983) 158.
[16] G.M. Sheldrick, Acta Crystallogr. Sect. A 46 (1990) 467–473.
[17] G.M. Sheldrick, SHELXL, a computer program for crystal struc-
ture refinement, University of Go¨ttingen, 1993.
[18] P. McArdle, J. Appl. Cryst. 27 (1994) 438.
.