18
T. Kanbara, T. Yamamoto / Journal of Organometallic Chemistry 688 (2003) 15Á19
/
and washed with MeOH, water, and ether to give a
bright yellow powder of 2 (48 mg, 72% yield).
(I ꢀ
R1ꢀ
/
3s(I), 334 valuable parameters) with factors of
0.089, Rwꢀ0.139, GOFꢀ0.98.
/
/
/
3.3.2. Procedure B
4. Supplementary material
A mixture of 1 (53 mg, 0.1 mmol), PdCl2(PhCN)2 (38
mg, 0.1 mmol), and CH3CN (10 ml) was heated at 65 8C
for 24 h under N2. The resulting yellow precipitate was
filtered and washed with CH3CN, MeOH, water, and
ether to give a yellow powder of 2 (44 mg, 65% yield).
Crystallographic data for the structural analysis have
been deposited with the Cambridge Crystallographic
Data Center, CCDC nos. 209322 (2) and 209323 (3).
Copies of this information may be obtained free of
charge from The Director, CCDC, 12 Union Road,
Cambridge CB2 1EZ, UK (Fax: ꢂ44-1223-336033; e-
mail: deposit@ccdc.cam.ac.uk or www: http://
1H-NMR (400 MHz, Me2SO-d6): d 7.82Á
/
7.72 (m,
12H), 7.70Á
/
7.63 (m, 8H), 7.20 (d, 2H, Jꢀ
/
11.7 Hz), 2.16
(s, 3H). 31P-NMR (160 MHz, Me2SO-d6): d 56.5. Anal.
Found: C, 55.59; H, 3.96; Cl, 4.91; S, 9.51. Calc. for
C31H25ClP2PdS2: C, 55.95; H, 3.79; Cl, 5.33; S, 9.64%.
/
3.4. Pt(1-H)Cl (3)
Acknowledgements
The procedure A for 2 was adopted using K2PtCl4 (42
mg, 0.1 mmol) to afford a yellow powder of 3 (67 mg,
89% yield).
The authors are grateful to Dr. Hiromitsu Ogawa and
Tetsushi Inoue of TDK Corporation for experimental
support.
1H-NMR (400 MHz, Me2SO-d6): d 7.82Á
/
7.73 (m,
12H), 7.70Á
/
7.63 (m, 8H), 7.19 (d, 2H, Jꢀ
/
11.7 Hz), 2.09
(s, 3H). 31P-NMR (160 MHz, Me2SO-d6): d 58.0. Anal.
Found: C, 49.26; H, 3.50; Cl, 4.59; S, 8.42. Calc. for
C31H25ClP2PtS2: C, 49.37; H, 3.34; Cl, 4.70; S, 8.50%.
References
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3.5. Crystal data for 2 and 3
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The diffraction data were collected with a Rigaku
Saturn CCD diffractometer using a graphite monochro-
˚
(d) J.T. Singleton, Tetrahedron 59 (2003) 1837.
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mated MoÁ
/
Ka (lꢀ
/
0.71070 A) at ꢁ160 8C. The data
/
were corrected for Lorentz and polarization effects, and
an absorption correction was applied. The structure was
solved by direct methods (SIR 92), and expanded using
Fourier techniques. The non-hydrogen atoms were
refined anisotropically. Hydrogen atoms were located
by assuming the ideal geometry and included in the
structure calculation without further refinement of the
parameters.
(b) S.-W. Lai, M.C.-W. Chan, T.-C. Cheung, S.-M. Peng, C.-M.
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[3] (a) T.S. Lobana, in: F.R. Hartley (Ed.), The Chemistry of
2: C31H25ClP2Pd2S2, Mꢀ
/
665.46, orthorhombic,
Organophosphorus Compounds, vol.
Chichester, 1992, p. 409 (Chapter 8);
2 (Chapter 8), Wiley,
space group P212121 (No. 19), aꢀ
/
9.890(6), bꢀ
/
3
(b) B. Walther, Coord. Chem. Rev. 60 (1984) 67.
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Organometallics 21 (2002) 2785.
˚
˚
14.959(8), cꢀ
Dcalc 1.559
F(000)ꢀ1344. A total of 79 603 reflections were mea-
/
19.160(11) A, Vꢀ
/
2834.5(27) A , Zꢀ
Ka)ꢀ ,
/4,
ꢀ
/
g
cmꢁ3
,
m(MoÁ
/
/
10.30 cmꢁ1
/
sured, 3582 unique. The final cycle of full-matrix least-
squares refinement on F was based on 3079 observed
[5] (a) O. Herd, A. Heßler, M. Hingst, M. Tepper, O. Stelzer, J.
Organomet. Chem. 522 (1996) 69;
(b) P. Machnitzki, T. Nickel, O. Stelzer, C. Landgrafe, Eur. J.
Inorg. Chem. (1998) 1029;
reflections (I ꢀ
factors of R1ꢀ0.070, Rwꢀ
3: C31H25ClP2Pt2S2, Mꢀ754.15, orthorhombic, space
group P212121 (No. 19), aꢀ9.832(6), bꢀ14.978(10),
2811.2(31) A , Zꢀ4, Dcalc
1.782 g cmꢁ3, m(MoÁ 53.49 cmꢁ1, F(000)ꢀ
Ka)ꢀ
/
3s(I), 334 valuable parameters) with
/
/
0.118, GOFꢀ0.94.
/
(c) T. Kanbara, S. Takase, R. Hayashi, S. Kagaya, K. Hasegawa,
T. Yamamoto, J. Polym. Sci.: Part A: Polym. Chem. 40 (2002)
2637.
/
/
/
3
˚
˚
[6] (a) A.D. Ryabov, Inorg. Chem. 26 (1987) 1252;
(b) D.J. Ca´rdenas, A.M. Echavarren, Organometallics 18 (1999)
3337;
cꢀ
/
19.090(12) A, Vꢀ
/
/
ꢀ
/
/
/
/
1472. A total of 20 235 reflections were measured,
3222 unique. The final cycle of full-matrix least-squares
refinement on F was based on 3022 observed reflections
(c) E. D´ıez-Barra, J. Guerra, I. Lo´pez-Solera, S. Merino, J.
Rodor´ıguez-Lo´pez, P. Sa´nchez-Verdu´, J. Tejeda, Organometallics
22 (2003) 541.