Bis(phosphido)-Bridged Dinuclear Carbonyls of Platinum(I)
Arif, J. A. Gladysz, Organometallics 1992, 11, 2673–2685; d)
D. Scott Bohle, G. R. Clark, C. E. F. Rickard, W. R. Roper, J.
Organomet. Chem. 1990, 393, 243–285; e) W. Malish, R.
Maisch, I. J. Colquhoun, W. McFarlane, J. Organomet. Chem.
1981, 220, C1–C6; f) V. Gallo, M. Latronico, P. Mastrorilli,
C. F. Nobile, G. Ciccarella, U. Englert, Eur. J. Inorg. Chem.
2006, 2634–2641; g) E. J. Derrah, D. A. Pantazis, R. McDon-
ald, L. Rosenberg, Organometallics 2007, 26, 1473–1482; h)
G. L. Geoffroy, S. Rosenberg, P. M. Schulman, R. R. Whittle,
J. Am. Chem. Soc. 1984, 106, 1519–1521.
a) C. Archambault, R. Bender, P. Braunstein, Y. Dusausoy, J.
Chem. Soc., Dalton Trans. 2002, 4084–4090; b) H.-C. Bottcher,
M. Graf, K. Merzweiler, C. Wagner, J. Organomet. Chem. 2001,
628, 144–150; c) P. Braunstein, E. de Jesus, A. Dedieu, M. Lan-
franchi, A. Tiripicchio, Inorg. Chem. 1992, 31, 399–410; d) J.
Powell, J. F. Sawyer, S. J. Smith, J. Chem. Soc., Dalton Trans.
1992, 2793–2801; e) J. A. Cabeza, F. J. Lahoz, A. Martin, Orga-
nometallics 1992, 11, 2754–2756; f) R. Walther, H. Hartung,
H.-C. Böttcher, U. Baumeister, U. Böhland, J. Rheinold, J. Si-
eler, J. Ladriere, H.-M. Schiebel, Polyhedron 1991, 10, 2423–
2435; g) J. Powell, E. Fuchs, M. R. Gregg, J. Phillips, M. V. R.
Stainer, Organometallics 1990, 9, 387–393; h) T. Adatia, M.
McPartlin, M. J. Mays, M. J. Morris, P. R. Raithby, J. Chem.
Soc., Dalton Trans. 1989, 1555–1564; i) J. Powell, J. F. Sawyer,
M. V. R. Stainer, Inorg. Chem. 1989, 28, 4461–4470; j) T. Blum,
P. Braunstein, Organometallics 1989, 8, 2497–2503; k) B. Kling-
ert, H. Werner, J. Organomet. Chem. 1987, 333, 119–128; l) L.
Chen, D. J. Kountz, D. W. Meek, Organometallics 1985, 4, 598–
601; m) H. Werner, W. Hofmann, R. Zolk, L. F. Dahl, J. Kocal,
A. Kühn, J. Organomet. Chem. 1985, 289, 173–188.
a) P. Leoni, M. Sommovigo, M. Pasquali, P. Sabatino, D.
Braga, J. Organomet. Chem. 1992, 423, 263–270; b) P. Leoni,
M. Pasquali, M. Sommovigo, F. Laschi, P. Zanello, A. Albin-
ati, F. Lianza, P. S. Pregosin, H. Rüegger, Organometallics
1993, 12, 1702–1713; c) P. Leoni, G. Pieri, M. Pasquali, J.
Chem. Soc., Dalton Trans. 1998, 657–662; d) P. Leoni, M. Pas-
quali, G. Pieri, A. Albinati, P. S. Pregosin, H. Rüegger, Organo-
metallics 1995, 14, 3143–3145; e) P. Leoni, M. Pasquali, M.
Sommovigo, A. Albinati, F. Lianza, P. S. Pregosin, H. Rüegger,
Organometallics 1993, 12, 4503–4508; f) P. Leoni, E. Vichi, S.
Lencioni, M. Pasquali, E. Chiarentin, A. Albinati, Organome-
tallics 2000, 19, 3062–3068.
a) P. Leoni, M. Pasquali, A. Fortunelli, G. Germano, A. Albin-
ati, J. Am. Chem. Soc. 1998, 120, 9564–9673; b) P. Leoni, G.
Chiaradonna, M. Pasquali, F. Marchetti, Inorg. Chem. 1999,
38, 253–259; c) P. Leoni, M. Pasquali, V. Cittadini, A. For-
tunelli, M. Selmi, Inorg. Chem. 1999, 38, 5257–5265; d) V. Cit-
tadini, P. Leoni, L. Marchetti, M. Pasquali, A. Albinati, Inorg.
Chim. Acta 2002, 330, 25; e) P. Leoni, F. Marchetti, L. March-
etti, V. Passarelli, Chem. Commun. 2004, 2346–2347.
collection. The data were collected by using ω scans, in steps of 0.3°.
For each of the collected frames, counting time was 30 s. The least-
squares refinement was carried out by using anisotropic displace-
ment parameters for the P and C atoms of the phosphido-bridged
moiety. The remaining atoms were treated isotropically. The large
values of the displacement parameters of some atoms suggest the
presence of structural disorder. The latter can be due to the higher
crystallographic symmetry imposed on a less symmetric molecule,
thus leading to positional disorder. An attempt to improve the re-
fined model, by treating all atoms anisotropically, did not yield any
significant improvement of the fit; therefore, the model with less pa-
rameters was retained. The contribution of the H atoms, in their
calculated positions [C–H 0.96[Å], B(H) = 1.5ϫ B(Cbonded)(Å2)],
was included in the refinement by using a riding model.
[2]
Structural Study of [Pt(µ-PtBu2)(PPh3)]2 (19): The space group was
determined from the systematic absences. Cell constants were re-
fined by least-squares at the end of the data collection. The data
were collected by using ω scans, in steps of 0.3°. For each of the
1800 collected frames, counting time was 20 s. The Fourier differ-
ence maps revealed a clathrated toluene molecule that was included
in the refinement. The least-squares refinement was carried out by
using anisotropic displacement parameters for all non-hydrogen
atoms, whereas the H atoms were included in the refinement as
described above [C–H 0.96(Å), B(H) = aB(Cbonded)(Å2), a = 1.4 for
CH3 groups and 1.2 for the other H atoms].
Structural Study of [Pt2(µ-PtBu2)2(H)(PPh3)2]CF3SO3 (21): The
values of the cell parameters were refined at the end of the data
collection. The data were collected by using ω scans, in steps of
0.3°. For each of the 1800 collected frames, counting time was 20 s.
The space group assignment was confirmed by the successful re-
finement. Due to the crystallographic symmetry the asymmetric
unit is half of the dimer; therefore, the counterion site occupancy
factor (SOF) has to be 0.5. Refinement of the SOFs for the
[3]
–
CF3SO3 atoms confirmed this assumption. Refining the structure
in the noncentrosymmetric space group P1 (thus almost doubling
the number of refined parameters) did not yield a better fit or mo-
lecular geometry. It proved impossible to locate the hydride ligand
(see the discussion of the structure). As often the case, the triflate
show large amplitude motions for the atoms as a consequence of
disorder that proved impossible to model satisfactorily. The least-
squares refinement and H atoms treatment was carried out as de-
scribed above.
[4]
CCDC-656030 (for 9), -684894 (for 9·210), -656031 (for 18),
-656032 (for 19) and -656033 (for 21) contain the supplementary
crystallographic data for this publication. These data can be ob-
tained free of charge from the Cambridge Crystallographic Data
Centre via www.ccdc.cam.ac.uk/data_request/cif.
[5]
[6]
P. Leoni, S. Manetti, M. Pasquali, A. Albinati, Inorg. Chem.
1996, 35, 6045–6052.
M. P. Brown, R. J. Puddephatt, M. Rashidi, K. R. Seddon, J.
Chem. Soc., Dalton Trans. 1978, 516–522.
[7]
[8]
P. E. Garrou, Chem. Rev. 1981, 81, 229–266.
a) Ni2[µ-P(SiMe3)2](PMe3)2: B. Deppisch, H. Schafer, Z.
Anorg. Allg. Chem. 1982, 490, 129–135; b) Ni2(µ-PtBu2)
2(PMe3)2: R. A. Jones, A. L. Stuart, J. L. Atwood, W. E.
Hunter, R. D. Rogers, Organometallics 1982, 1, 1721–1723; c)
Ni2(µ-PCy2)2(η2-CH2=CH2)2: B. L. Barnett, C. Kruger, Cryst.
Struct. Commun. 1973, 2, 85; d) Ni2(µ-PCy2)2(PMeCy2)2: C. E.
Krilley, C. J. Woolley, M. K. Krepps, E. M. Popa, P. E. Fan-
wick, I. P. Rothwell, Inorg. Chim. Acta 2000, 300, 200–205.
a) Pd2(µ-PtBu2)2(PMe3)2: A. M. Arif, D. E. Heaton, R. A.
Jones, C. M. Nunn, Inorg. Chem. 1987, 26, 4228–4231; b)
Pd2(µ-PCy2)2[P(OPh)Cy2]2: M. Sommovigo, M. Pasquali, P.
Leoni, U. Englert, Inorg. Chem. 1994, 33, 2686–2688; c) Pd2(µ-
PtBu2)2(PEt3)2: U. Englert, E. Matern, J. Olkowska-Oetzel, J.
Pikies, Acta Crystallogr., Sect. E: Struct. Rep. Online 2003, 59,
m376–m377.
Acknowledgments
This work was supported by the Ministero dellЈIstruzione,
dellЈUniversità e della Ricerca (MIUR), Programmi di Rilevante
Interesse Nazionale, PRIN 2006-2007 and by the University of Pisa
(Progetti di Ricerca 2006 – Scienze e tecnologie dei nano/microsis-
temi).
[9]
[1] a) J. Giver Planas, F. Hampel, J. A. Gladysz, Chem. Eur. J.
2005, 11, 1402–1416; b) D. K. Wicht, S. N. Paisner, B. M. Lew,
D. S. Glueck, G. P. A. Yap, L. M. Liable-Sands, A. Rheingold,
C. M. Haar, S. P. Nolan, Organometallics 1998, 17, 652–660; c)
B. D. Zwick, M. A. Dewey, D. A. Knight, W. E. Buhro, A. M.
Eur. J. Inorg. Chem. 2008, 4092–4100
© 2008 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim
www.eurjic.org
4099