2906
P.-C. Zhang et al. / Journal of Organometallic Chemistry 693 (2008) 2903–2906
4H PhS), 6.23 (d, 4H PhS), 1.04 (s, 30H, Cp*). 13C NMR (125 MHz,
CDCl3, ppm): d 176.54, 149.57, 135.51, 126.10, 117.13 (2-PyS),
130.32–126.62 (PhS), 91.53, 10.64 (Cp*).
Table 1
X-ray crystallographic data and processing parameters for 3 and 5
Complex
3
5
Empirical formula
Formula weight
Crystal system
Space group
a (Å)
C
20H24CoN2S2I
C38H46Cl2Co2INS3
928.65
Monoclinic
P21/n
13.735(4)
16.530(5)
17.583(6)
90
91.517(4)
90
4.6. Crystal structure determinations
542.39
Monoclinic
P21/c
18.149(6)
7.260(3)
18.226(6)
90
115.757(4)
90
Crystals of 3 and 5 suitable for X-ray crystallography were
grown by slow diffusion of hexane into CH2Cl2 solution. Diffraction
data of 3 and 5 were collected on a Bruker Smart APEX CCD diffrac-
b (Å)
c (Å)
tometer (Mo K
a radiation). The structures were solved by direct
a
(°)
methods and subsequently refined on F2 by using full-matrix
least-squares techniques (SHELXL-97), all non-hydrogen atoms were
refined anisotropically, and hydrogen atoms were located at calcu-
lated positions (see Table 1).
b (°)
c
(°)
Volume (Å3)
2162.8(13)
4
2.421
3991(2)
4
1.923
Z
l
(mmÀ1
)
Crystal size (mm)
Dcalc. (mg/m3)
F(000)
0.30 Â 0.10 Â 0.10
0.20 Â 0.15 Â 0.10
1.666
1.546
Acknowledgment
1080
1880
h Range (°)
h, k, l Collected
2.241–23.451
À22, 23; À6, 9;
À21, 23
1.69–27.13
17; À15, 21;
À22, 21
Financial support by Shanghai Leading Academic Discipline Pro-
ject, Project No.: B108 is gratefully acknowledged.
Reflections collected/unique
10419/4775 (0.0578)
19539/8667 (0.0663)
(Rint
)
Appendix A. Supplementary material
Data/restraints/parameters
4775/18/278
0.976
8667/0/434
0.893
Goodness-of-fit on F2
Supplementary data associated with this article can be found, in
Final R indices [I > 2
r
(I)]
R1 = 0.0518,
wR2 = 0.1136
R1 = 0.0797,
wR2 = 0.1255
1.167 and À0.857
R1 = 0.0647,
wR2 = 0.1679
R1 = 0.1397,
wR2 = 0.1995
1.641 and À0.743
R indices (all data)
Largest difference in peak
and hole (e ÅÀ3
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C, 58.56; H, 5.63. N, 6.88%. IR (KBr): 2955, 1619, 1441, 1261,
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C
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(500 MHz, CDCl3, ppm): d 8.47 (d, 1H, 2-PyS), 7.97 (t, 1H, 2-PyS),
6.71 (t, 1H, 2-PyS), 6.43 (d, 1H, 2-PyS), 8.51 (d, 2H, 4-PyS), 7.38
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To an Et2O (10 mL) solution of benzenethiol (22 mg, 0.2 mmol)
was added a solution of n-BuLi (1.6 M, 0.14 mL, 0.22 mmol) in hex-
ane dropwise at 0 °C. A white precipitate was formed immediately.
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in 20 mL THF at À78 °C, and the mixture was stirred overnight.
The solvent was removed under reduced pressure and the residue
was redissolved in 10 mL CH2Cl2. The brown filtrate was collected.
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brown solid (54 mg, 58%). Anal. Calc. for C37H44Co2INS3 Á CH2Cl2
(928.65 g/mol): C, 49.15; H, 4.99; N, 1.51. Found: C, 49.03; H,
4.86; N, 1.52%. IR (KBr): 2970, 2907, 1633, 1576, 1440, 1415,
1376, 1255, 1134, 1087, 1023, 800, 760, 734 cmÀ1 1H NMR
.
(500 MHz, CDCl3, ppm): d 7.78 (d, 1H, 2-PyS), 7.20 (d, 1H, 2-PyS),
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