A. Akkari et al. / Journal of Organometallic Chemistry 622 (2001) 190–198
197
Organometallics 18 (1999) 1482. (c) S. Benet, C.J. Cardin, D.J.
Cardin, S.P. Constantine, P. Heath, M.G.B. Drew, H. Rashid, S.
Teixeira, J.H. Thorpe, A.K. Todd, Organometallics 18 (1999)
389. (d) R.S. Foley, Y. Zhou, G.P.A. Yap, D.R. Richeson,
Inorg. Chem. 39 (2000) 924. (e) A. Filippou, P. Portius, G.
Kociok-ko¨hn, V. Albrecht, J. Chem. Soc., Dalton Trans. (2000)
1759. Sn: (b–d). (f) B.G. Mc Burnett, A.J. Cowley, Chem.
Commun. (1999). (g) D. Agustin, G. Rima, H. Gornitzka, J.
Barrau, Main Group Met. Chem. 22 (1999) 703. (h) R.S. Foley,
G.P.A. Yap, D.R. Richeson, Organometallics 18 (1999) 4700. (i)
M.C. Kuchta, J.M. Hahn, G. Parkin, J. Chem. Soc., Dalton
Trans. (1999) 3559. (j) S. Wingerter, H. Gornitzka, R. Berter-
mann, S.K. Pandey, J. Rocha, D. Stalke, Organometallics 19
(2000) 3890. (k) C. Eaborn, M.S. Hill, P.B. Hitchcock, D. Patel,
J.D. Smith, S. Zhang, Organometallics 19 (2000) 49. (l) C. Drest,
P.B. Hitchcock, M.F. Lappert, Angew. Chem. 111 (1999) 1185;
Angew. Chem. Int. Ed. 38 (1999) 1113. (m) P.B. Hitchcock,
M.F. Lappert, G.A. Lawless, G.M. de Lima, L.J.-M. Pierssens,
J. Organomet. Chem. 601 (2000) 142. Pb: (c), (i), (j). (n) M.
Stu¨rmann, W. Saak, M. Weidenbruch, K.W. Klinkhammer, Eur.
J. Inorg. Chem. (1999) 579. (o) W.J. Evans, R.D. Clark, K.J.
Forrestal, J.W. Ziller, Organometallics 18 (1999) 2401. (p) M.
Seidel, K. Jacob, A.A.H. Van der Zeiden, H. Menge, K.
Merzweiler, C. Wagner, Organometallics 19 (2000) 1438.
[3] H.V.R. Dias, W. Jin, J. Am. Chem. Soc. 118 (1996) 9123.
[4] H.V.R. Dias, W. Jin, Inorg. Chem. 35 (1996) 6546.
[5] H.V.R. Dias, Z. Wang, J. Am. Chem. Soc. 119 (1997) 4650.
[6] Y. Zhou, D.S. Richeson, J. Am. Chem. Soc. 118 (1996) 10850.
[7] S.R. Foley, C. Bensimon, D.S. Richeson, J. Am. Chem. Soc. 119
(1997) 10359.
4.21. Crystal data for 2
C17H17ClN2Sn, Mr=403.47, monoclinic, C2/c, a=
29.477(2), b=8.6530(6), c=14.6554(10) A, i=
,
3
,
112.065(1)°, V=3464.3(4) A , Z=8, zcalc 1.547 Mg
m−3 F(000)=1600, u=0.71073 A, T=193(2) K, v
,
(Mo–Ka)=1.624 mm−1, crystal size 0.4×0.5×0.8
mm, 5.21=[=23.25°, 12957 reflections (5321 inde-
pendent) were collected at low temperatures using an
oil-coated shock-cooled crystal on a Bruker-AXS CCD
1000 diffractometer. At the beginning of the refinement,
we were blocked at R1=0.2 and the Difference Fourier
gave a high rest electron density peak, which gave no
chemical sense. By using the program package GEMINI
[32], we found two orientation matrices [A1=0.01414
−0.10611 0.00493, −0.00767 0.00020 −0.07252,
0.03287 0.04569 0.01175 and A2=0.01407 0.10624
0.01652, −0.00733 −0.00090 0.06130, 0.03300 −
0.04552 0.03735] corresponding to a non-meroheral
twin formed by rotation of 180° around the reciprocal
vector 100 (for more information about twinned sys-
tems have a look at [33,34]). The reflection intensities
for each twin component were integrated. The structure
was solved by direct methods (SHELXS-97) [35] and 199
parameters were refined using the least-squares method
on F2 [36]. All non-hydrogen atoms were refined an-
isotropically. The hydrogen atoms of the molecules
[8] J. Barrau, G. Rima, T. El Amraoui, Organometallics 17 (1998)
607.
[9] J. Barrau, G. Rima, T. El Amraoui, J. Organomet. Chem. 570
(1998) 163.
[10] J. Barrau, G. Rima, T. El Amraoui, J. Organomet. Chem. 561
(1998) 167.
[11] D. Agustin, G. Rima, H. Gornitzka, J. Barrau, J. Organomet.
Chem. 592 (1999) 1.
were geometrically idealized and refined using a riding
model. Largest electron density residue: 0.971 e A
−3
,
,
R1 (for F\2|(F))=0.0663 and wR2=0.1743 (all data)
with R1=SꢀꢀFoꢀ−ꢀFcꢀꢀ/SꢀFoꢀ and wR2=(Sw(F2o−Fc2)2/
Sw(F2o)2)0.5
.
[12] D. Agustin, G. Rima, H. Gornitzka, J. Barrau, Eur. J. Inorg.
Chem. (2000) 693 and references quoted there in.
[13] D. Agustin, G. Rima, H. Gornitzka, J. Barrau, Inorg. Chem. 39
(2000) 5492 and references quoted therein.
5. Supplementary material
[14] D. Agustin, G. Rima, H. Gornitzka, J. Barrau, Organometallics
19 (2000) 4276.
[15] M. Rahim, N.J. Taylor, S. Xin, S. Collins, Organometallics 17
(1998) 1315.
[16] B. Qian, D.L. Ward, N.R. Smith, Organometallics 17 (1998)
3070.
Crystallographic data (excluding structure factors)
have been deposited with the Cambridge Crystallo-
graphic Data Centre, CCDC no. 151 236. Copies of the
data can be obtained free of charge from The Director,
CCDC, 12 Union Road, Cambridge CB2 1EZ, UK
[17] W.-K. Kim, M.J. Fevola, L.M. Liable-Sauds, A.L. Rheingold,
K.H. Theopold, Organometallics 17 (1998) 4541.
[18] F. Cosledan, P.B. Hitchcock, M.F. Lappert, Chem. Commun.
(1999) 707.
(fax:
+44-1223-336033;
e-mail:
deposit@ccdc.
cam.ac.uk or www: http://www.ccdc.cam.ac.uk).
[19] D.L. Reger, S.J. Knox, M.F. Huff, A.L. Rheingold, B.S. Hag-
gerty, Inorg. Chem. 30 (1991) 1754.
[20] C.F. Caro, P.B. Hitchcock, M.F. Lappert, Chem. Comm. (1999)
1433.
[21] P.B. Hitchcock, M.F. Lappert, S. Tian, J. Chem. Soc. Dalton
Trans. (1997) 1945.
[22] P.B. Hitchcock, M.F. Lappert, M. Layh, D.-S. Liu, R. Sablong,
S. Tian, J. Chem. Soc. Dalton Trans. (2000) 2301 and references
quoted there in.
References
[1] Recent reviews: (a) J. Barrau, G. Rima, Coord. Chem. Rev.
Part. I: 178–180 (1998) 593. (b) M. Driess, H. Gru¨tzmacher,
Angew. Chem. 108 (1996) 900; Angew Chem. Ed. Engl. 35
(1996) 827. (c) W.P. Neumann, Chem. Rev. 91 (1991) 311. (d)
M.F. Lappert, R.S. Rowe, Coord. Chem. Rev. 100 (1990) 267.
(e) J. Satge´, J. Organomet. Chem. 400 (1990) 121.
[23] P.B. Hitchcock, J. Hu, M.F. Lappert, M. Layh, D.-S. Liu, J.R.
Severn, S. Tian, An. Quim. Int. Ed. Engl. 92 (1996) 186.
[24] C.E. Holloway, M. Melnik, Main Group Met. Chem. 21 (1998)
371.
[2] For structurally characterized compounds for the last 2 years,
see: Ge: (a) P. Jutzi, S. Keitemeyer, B. Neumann, H.-G. Stamm-
ler, Organometallics 18 (1999) 4778. (b) W.-P. Leung, L.-H.
Weng, W.-H. Kwok, Z.Y. Zhou, Z.Y. Zhang, T.C.W. Mak,