(IUCr) Decacarbonyl-1[kappa]3C,2[kappa]3C,3[kappa]4C-[mu]-hydrido-1:2[kappa]2H:H-([mu]-quinoline-2-thiolato-1:2[kappa]2S:S)diosmium(I)osmium(0)(3 Os-Os)

Volume 64
Part 5
Page m608
May 2008

Received 14 January 2008
Accepted 20 February 2008
Online 2 April 2008

Key indicators
Single-crystal X-ray study
T = 223 K
Mean (C-C) = 0.009 Å
R = 0.024
wR = 0.052
Data-to-parameter ratio = 14.3
Details

Decacarbonyl-1³C,2³C,3⁴C--hydrido-1:2²H:H-(-quinoline-2-thiolato-1:2²S:S)diosmium(I)osmium(0)(3 Os-Os)

Yu Sun,^a ^* Xiu-Bing Li ^b and Bai-Wang Sun ^a

^aOrdered Matter Science Research Center, College of Chemistry and Chemical Engineering, Southeast University, Nanjing 210096, People's Republic of China, and ^bKey Laboratory of Medicinal Chemistry for Natural Resources, Ministry of Education and Department of Chemistry, Yunnan University, Kunming 650091, People's Republic of China
Correspondence e-mail: chmsunbw@seu.edu.cn

The title compound, [Os₃(C₉H₆NS)H(CO)₁₀], contains a nearly equilateral triangle of Os atoms. Two of the Os atoms are bridged by an S atom of the quinoline-2-thiolate ligand. Ten carbonyl groups complete the cluster, resulting in a distorted octahedral geometry for each Os atom. The hydride atom, which was located in a difference Fourier map and refined isotropically, bridges the shortest Os-Os edge.

Related literature

For related literature, see: Begum et al. (2007); Fan et al. (2004); Miyake et al. (2007); Zeller et al. (2003).

Experimental

Crystal data

[Os₃(C₉H₆NS)H(CO)₁₀]
M_r = 1012.02
Monoclinic, P 2₁ /n
a = 9.3593 (5) Å
b = 9.4129 (5) Å
c = 25.7433 (14) Å
= 93.045 (1)°
V = 2264.7 (2) Å³
Z = 4
Mo K radiation
= 16.94 mm^-1
T = 223 (2) K
0.18 × 0.16 × 0.14 mm

Data collection

Rigaku SCXMini 1K CCD area-detector diffractometer
Absorption correction: multi-scan (CrystalClear; Rigaku, 2005) T_min = 0.058, T_max = 0.092
13690 measured reflections
4446 independent reflections
4162 reflections with I > 2(I)
R_int = 0.032

Refinement

R[F² > 2(F²)] = 0.024
wR(F²) = 0.052
S = 1.14
4446 reflections
311 parameters
1 restraint
H atoms treated by a mixture of independent and constrained refinement
_max = 0.75 e Å^-3
_min = -1.24 e Å^-3

Table 1
Selected bond lengths (Å)

Os1-C11	1.892 (6)
Os1-C12	1.900 (6)
Os1-C13	1.922 (6)
Os1-S1	2.4154 (14)
Os1-Os2	2.8399 (3)
Os1-Os3	2.8559 (3)
Os1-H1	1.87 (6)
Os2-C23	1.896 (6)
Os2-C22	1.901 (6)
Os2-C21	1.926 (6)
Os2-S1	2.4144 (13)
Os2-Os3	2.8516 (3)
Os2-H1	1.86 (6)
Os3-C33	1.897 (6)
Os3-C34	1.929 (6)
Os3-C31	1.941 (6)
Os3-C32	1.970 (6)

Data collection: CrystalClear (Rigaku, 2005); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL.

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: HY2117 ).

References

Begum, N., Das, U. K., Hassan, M., Hogarth, G., Kabir, S. E., Nordlander, E., Rahman, M. A. & Tocher, D. A. (2007). Organometallics, 26, 6462-6472.
Fan, W., Zhang, R., Leong, W. K. & Yan, Y. K. (2004). Inorg. Chim. Acta, 357, 2441-2450.
Miyake, Y., Nomaguchi, Y., Yuki, M. & Nishibayashi, Y. (2007). Organometallics, 26, 3611-3613.
Rigaku (2005). CrystalClear. Rigaku Corporation, Tokyo, Japan.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Zeller, M., Hunter, A. D., Regula, J. L. & Szalay, P. S. (2003). Acta Cryst. E59, m975-m976.

metal-organic compounds

Decacarbonyl-13C,23C,34C--hydrido-1:22H:H-(-quinoline-2-thiolato-1:22S:S)diosmium(I)osmium(0)(3 Os-Os)