Decacarbonyl-1κ3C,2κ3C,3κ4C-μ-hydrido-1:2κ2H:H-(μ-quinoline-2-thiol­ato-1:2κ2S:S)diosmium(I)osmium(0)(3 Os—Os)

Sun, Y.; Li, X.-B.; Sun, B.-W.

doi:10.1107/S1600536808004881

metal-organic compounds

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ISSN: 2056-9890

Volume 64| Part 5| May 2008| Page m608

doi:10.1107/S1600536808004881

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Decacarbonyl-1κ³C,2κ³C,3κ⁴C-μ-hydrido-1:2κ²H:H-(μ-quinoline-2-thiolato-1:2κ²S: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

(Received 14 January 2008; accepted 20 February 2008; online 2 April 2008)

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
β = 93.045 (1)°
V = 2264.7 (2) Å³
Z = 4
Mo Kα radiation
μ = 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 > 2σ(I)
R_int = 0.032

Refinement

R[F² > 2σ(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
Δρ_max = 0.75 e Å⁻³
Δρ_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.

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536808004881/hy2117sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536808004881/hy2117Isup2.hkl

checkCIF report

Comment top

In recent years, transition metal–carbonyl clusters have received considerable attention owing to their important role in catalytic reactions (Miyake et al., 2007; Zeller et al., 2003) as well as the preparation of materials with novel magnetic properties (Fan et al., 2004). Different organic ligands containing O and S atoms can stabilize the metal cluster framework by means of chelating and bridging (Begum et al., 2007). We report here the synthesis and structure of the title compound containing a triangle of Os atoms and an organic quinoline-2-thiol ligand.

The S atom of the ligand acts as a bidentate bridge connecting two Os atoms [Os1—S1 = 2.4154 (14) and Os2—S1 = 2.4144 (13) Å]. The molecule of the title compound (Fig. 1) consists of an Os₃ triangle with ten terminal CO ligands and a substituted quinoline-2-thiol ligand. Each Os atom is in a distorted octahedral geometry, with Os3 bonded to four terminal carbonyl ligands and Os1 and Os2 bonded to three terminal carbonyl ligands and one bridging S atom from the quinoline-2-thiol ligand, respectively. The hydride H atom was crystallographically located and refined and it is found to bridge across the shortest Os1—Os2 edge.

Related literature top

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

Experimental top

[Os₃(CO)₁₀(MeCN)₂] (0.120 g, 0.1 mmol) was added to a MeCN solution (10 ml) of quinoline-2-thiol (0.015 g, 0.1 mmol) and the mixture was stirred at room temperature for one hour. Crystals suitable for crystallographic analysis were obtained after two weeks.

Computing details top

Data collection: CrystalClear (Rigaku, 2005); cell refinement: CrystalClear (Rigaku, 2005); data reduction: CrystalClear (Rigaku, 2005); 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 (Sheldrick, 2008).

Figures top

Fig. 1. The molecular structure of the title compound. Displacement ellipsoids are drawn at the 30% probability level.

Decacarbonyl-1κ³C,2κ³C,3κ⁴C-µ-hydrido-1:2κ²H:H-(µ- quinoline-2-thiolato-1:2κ²S:S)diosmium(I)osmium(0)(3 Os—Os) top

Crystal data top

[Os₃(C₉H₆NS)H(CO)₁₀]	F(000) = 1808
M_r = 1012.02	D_x = 2.968 Mg m⁻³
Monoclinic, P2₁/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 4762 reflections
a = 9.3593 (5) Å	θ = 3.0–26.1°
b = 9.4129 (5) Å	µ = 16.94 mm⁻¹
c = 25.7433 (14) Å	T = 223 K
β = 93.045 (1)°	Block, colourless
V = 2264.7 (2) Å³	0.18 × 0.16 × 0.14 mm
Z = 4

Data collection top

Rigaku Scxmini 1K CCD area-detector diffractometer	4446 independent reflections
Radiation source: fine-focus sealed tube	4162 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.032
ω scans	θ_max = 26.0°, θ_min = 2.3°
Absorption correction: multi-scan (CrystalClear; Rigaku, 2005)	h = −10→11
T_min = 0.058, T_max = 0.092	k = −11→8
13690 measured reflections	l = −31→31

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.024	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.052	H atoms treated by a mixture of independent and constrained refinement
S = 1.14	w = 1/[σ²(F_o²) + (0.0163P)² + 2.1547P] where P = (F_o² + 2F_c²)/3
4446 reflections	(Δ/σ)_max = 0.001
311 parameters	Δρ_max = 0.75 e Å⁻³
1 restraint	Δρ_min = −1.24 e Å⁻³

Crystal data top

[Os₃(C₉H₆NS)H(CO)₁₀]	V = 2264.7 (2) Å³
M_r = 1012.02	Z = 4
Monoclinic, P2₁/n	Mo Kα radiation
a = 9.3593 (5) Å	µ = 16.94 mm⁻¹
b = 9.4129 (5) Å	T = 223 K
c = 25.7433 (14) Å	0.18 × 0.16 × 0.14 mm
β = 93.045 (1)°

Data collection top

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

Refinement top

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

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Os1	0.76242 (2)	0.01890 (2)	0.169927 (8)	0.01740 (6)
Os2	0.97667 (2)	−0.15956 (2)	0.130925 (8)	0.01676 (6)
Os3	1.04641 (2)	0.12428 (2)	0.161547 (8)	0.01774 (6)
N1	0.5984 (5)	−0.2445 (5)	0.08694 (18)	0.0239 (11)
S1	0.79273 (14)	−0.03585 (15)	0.07951 (5)	0.0200 (3)
O11	0.6461 (5)	0.3150 (5)	0.1487 (2)	0.0434 (12)
O12	0.7862 (5)	0.0836 (5)	0.28569 (17)	0.0401 (11)
O13	0.4768 (5)	−0.1310 (5)	0.18287 (19)	0.0414 (12)
O21	0.8805 (5)	−0.4583 (5)	0.09893 (18)	0.0402 (11)
O22	1.1990 (5)	−0.1242 (5)	0.0512 (2)	0.0465 (13)
O23	1.1859 (5)	−0.2826 (5)	0.21235 (18)	0.0426 (12)
O31	1.1025 (5)	−0.0142 (5)	0.26916 (17)	0.0384 (11)
O32	0.9894 (5)	0.2326 (5)	0.04959 (18)	0.0426 (12)
O33	1.3613 (5)	0.1450 (6)	0.1407 (2)	0.0605 (17)
O34	1.0082 (6)	0.4241 (5)	0.20439 (19)	0.0471 (13)
H1	0.851 (7)	−0.156 (8)	0.184 (3)	0.09 (3)*
C1	0.6572 (5)	−0.1579 (6)	0.0552 (2)	0.0183 (11)
C2	0.6192 (6)	−0.1465 (6)	0.0019 (2)	0.0227 (12)
H2A	0.6674	−0.0837	−0.0195	0.027*
C3	0.5099 (6)	−0.2299 (7)	−0.0178 (2)	0.0281 (13)
H3A	0.4821	−0.2252	−0.0534	0.034*
C4	0.3199 (6)	−0.4058 (7)	−0.0022 (3)	0.0304 (14)
H4A	0.2871	−0.4038	−0.0374	0.036*
C5	0.2526 (6)	−0.4889 (7)	0.0322 (3)	0.0349 (16)
H5A	0.1730	−0.5436	0.0207	0.042*
C6	0.3013 (7)	−0.4935 (7)	0.0844 (3)	0.0374 (16)
H6A	0.2530	−0.5506	0.1078	0.045*
C7	0.4172 (7)	−0.4170 (7)	0.1020 (3)	0.0332 (15)
H7A	0.4499	−0.4231	0.1371	0.040*
C8	0.4886 (5)	−0.3279 (6)	0.0673 (2)	0.0197 (12)
C9	0.4392 (5)	−0.3222 (6)	0.0148 (2)	0.0213 (12)
C11	0.6869 (6)	0.2026 (7)	0.1567 (2)	0.0267 (13)
C12	0.7783 (6)	0.0587 (7)	0.2424 (2)	0.0268 (13)
C13	0.5842 (6)	−0.0799 (7)	0.1754 (2)	0.0279 (13)
C21	0.9088 (6)	−0.3461 (6)	0.1112 (2)	0.0251 (13)
C22	1.1165 (6)	−0.1414 (6)	0.0804 (2)	0.0276 (14)
C23	1.1095 (6)	−0.2351 (6)	0.1818 (2)	0.0245 (13)
C31	1.0809 (6)	0.0373 (6)	0.2294 (2)	0.0243 (13)
C32	1.0046 (6)	0.1898 (7)	0.0897 (2)	0.0259 (13)
C33	1.2440 (6)	0.1335 (7)	0.1489 (3)	0.0311 (15)
C34	1.0190 (6)	0.3122 (7)	0.1892 (2)	0.0263 (13)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Os1	0.01208 (11)	0.01895 (12)	0.02128 (12)	−0.00154 (8)	0.00173 (8)	−0.00144 (8)
Os2	0.01364 (11)	0.01579 (11)	0.02091 (12)	−0.00091 (8)	0.00137 (8)	−0.00040 (8)
Os3	0.01302 (11)	0.01713 (11)	0.02298 (12)	−0.00306 (8)	0.00002 (8)	−0.00002 (8)
N1	0.021 (2)	0.027 (3)	0.023 (3)	−0.005 (2)	−0.0013 (19)	0.002 (2)
S1	0.0181 (6)	0.0206 (7)	0.0212 (7)	−0.0043 (5)	−0.0009 (5)	0.0022 (5)
O11	0.038 (3)	0.031 (3)	0.061 (3)	0.006 (2)	−0.006 (2)	−0.006 (2)
O12	0.048 (3)	0.050 (3)	0.023 (2)	0.001 (2)	0.005 (2)	−0.007 (2)
O13	0.028 (2)	0.046 (3)	0.051 (3)	−0.017 (2)	0.013 (2)	−0.009 (2)
O21	0.051 (3)	0.023 (2)	0.045 (3)	−0.008 (2)	−0.011 (2)	−0.008 (2)
O22	0.045 (3)	0.037 (3)	0.061 (3)	0.005 (2)	0.036 (3)	−0.001 (2)
O23	0.041 (3)	0.042 (3)	0.044 (3)	0.013 (2)	−0.014 (2)	0.005 (2)
O31	0.046 (3)	0.041 (3)	0.027 (2)	−0.008 (2)	−0.011 (2)	0.002 (2)
O32	0.050 (3)	0.042 (3)	0.035 (3)	−0.017 (2)	−0.004 (2)	0.015 (2)
O33	0.019 (3)	0.075 (4)	0.089 (4)	−0.004 (2)	0.005 (3)	0.034 (3)
O34	0.072 (4)	0.027 (3)	0.043 (3)	0.001 (3)	0.005 (3)	−0.009 (2)
C1	0.012 (2)	0.021 (3)	0.021 (3)	−0.001 (2)	−0.006 (2)	−0.002 (2)
C2	0.023 (3)	0.024 (3)	0.022 (3)	−0.005 (2)	0.000 (2)	0.001 (2)
C3	0.028 (3)	0.032 (3)	0.024 (3)	−0.001 (3)	−0.003 (2)	0.000 (3)
C4	0.026 (3)	0.026 (3)	0.038 (4)	−0.001 (3)	−0.005 (3)	−0.009 (3)
C5	0.017 (3)	0.031 (4)	0.055 (4)	−0.012 (3)	−0.002 (3)	−0.004 (3)
C6	0.035 (4)	0.030 (4)	0.048 (4)	−0.010 (3)	0.012 (3)	0.007 (3)
C7	0.033 (3)	0.035 (4)	0.032 (4)	−0.015 (3)	0.001 (3)	0.006 (3)
C8	0.015 (3)	0.022 (3)	0.023 (3)	−0.003 (2)	0.002 (2)	0.001 (2)
C9	0.013 (3)	0.023 (3)	0.028 (3)	0.001 (2)	0.002 (2)	−0.003 (2)
C11	0.017 (3)	0.030 (4)	0.033 (3)	0.003 (3)	−0.005 (2)	−0.007 (3)
C12	0.022 (3)	0.025 (3)	0.034 (4)	−0.002 (3)	0.009 (3)	−0.003 (3)
C13	0.026 (3)	0.030 (3)	0.028 (3)	−0.004 (3)	0.004 (3)	−0.002 (3)
C21	0.021 (3)	0.027 (3)	0.027 (3)	0.001 (2)	−0.004 (2)	−0.001 (3)
C22	0.023 (3)	0.026 (3)	0.035 (3)	0.005 (3)	0.004 (3)	−0.003 (3)
C23	0.026 (3)	0.018 (3)	0.029 (3)	0.003 (2)	0.000 (3)	−0.003 (2)
C31	0.019 (3)	0.025 (3)	0.028 (3)	−0.007 (2)	−0.001 (2)	0.000 (3)
C32	0.020 (3)	0.029 (3)	0.030 (3)	−0.008 (2)	0.002 (2)	0.002 (3)
C33	0.021 (3)	0.030 (3)	0.041 (4)	0.000 (3)	−0.005 (3)	0.012 (3)
C34	0.026 (3)	0.028 (3)	0.025 (3)	−0.001 (3)	0.001 (2)	−0.001 (3)

Geometric parameters (Å, º) top

Os1—C11	1.892 (6)	O21—C21	1.130 (7)
Os1—C12	1.900 (6)	O22—C22	1.118 (7)
Os1—C13	1.922 (6)	O23—C23	1.127 (7)
Os1—S1	2.4154 (14)	O31—C31	1.140 (7)
Os1—Os2	2.8399 (3)	O32—C32	1.110 (7)
Os1—Os3	2.8559 (3)	O33—C33	1.134 (7)
Os1—H1	1.87 (6)	O34—C34	1.130 (7)
Os2—C23	1.896 (6)	C1—C2	1.404 (8)
Os2—C22	1.901 (6)	C2—C3	1.366 (8)
Os2—C21	1.926 (6)	C2—H2A	0.9400
Os2—S1	2.4144 (13)	C3—C9	1.399 (8)
Os2—Os3	2.8516 (3)	C3—H3A	0.9400
Os2—H1	1.86 (6)	C4—C5	1.361 (9)
Os3—C33	1.897 (6)	C4—C9	1.417 (8)
Os3—C34	1.929 (6)	C4—H4A	0.9400
Os3—C31	1.941 (6)	C5—C6	1.397 (9)
Os3—C32	1.970 (6)	C5—H5A	0.9400
N1—C1	1.297 (7)	C6—C7	1.360 (9)
N1—C8	1.369 (7)	C6—H6A	0.9400
S1—C1	1.799 (5)	C7—C8	1.418 (8)
O11—C11	1.140 (7)	C7—H7A	0.9400
O12—C12	1.138 (7)	C8—C9	1.406 (8)
O13—C13	1.139 (7)

C11—Os1—C12	90.3 (3)	C34—Os3—Os2	158.16 (17)
C11—Os1—C13	97.9 (3)	C31—Os3—Os2	83.02 (17)
C12—Os1—C13	92.6 (2)	C32—Os3—Os2	90.14 (18)
C11—Os1—S1	94.81 (18)	C33—Os3—Os1	161.6 (2)
C12—Os1—S1	168.73 (17)	C34—Os3—Os1	98.51 (17)
C13—Os1—S1	96.58 (18)	C31—Os3—Os1	84.06 (16)
C11—Os1—Os2	137.83 (19)	C32—Os3—Os1	92.31 (16)
C12—Os1—Os2	116.33 (18)	Os2—Os3—Os1	59.679 (7)
C13—Os1—Os2	111.83 (19)	C1—N1—C8	117.6 (5)
S1—Os1—Os2	53.97 (3)	C1—S1—Os2	110.59 (18)
C11—Os1—Os3	90.53 (17)	C1—S1—Os1	110.76 (19)
C12—Os1—Os3	88.91 (17)	Os2—S1—Os1	72.03 (4)
C13—Os1—Os3	171.38 (19)	N1—C1—C2	124.7 (5)
S1—Os1—Os3	81.02 (3)	N1—C1—S1	119.8 (4)
Os2—Os1—Os3	60.085 (8)	C2—C1—S1	115.4 (4)
C11—Os1—H1	176 (3)	C3—C2—C1	117.7 (5)
C12—Os1—H1	88 (2)	C3—C2—H2A	121.1
C13—Os1—H1	86 (2)	C1—C2—H2A	121.1
S1—Os1—H1	86 (2)	C2—C3—C9	120.2 (5)
Os2—Os1—H1	40 (2)	C2—C3—H3A	119.9
Os3—Os1—H1	85 (2)	C9—C3—H3A	119.9
C23—Os2—C22	93.2 (3)	C5—C4—C9	120.1 (6)
C23—Os2—C21	92.0 (2)	C5—C4—H4A	119.9
C22—Os2—C21	97.5 (3)	C9—C4—H4A	119.9
C23—Os2—S1	169.10 (18)	C4—C5—C6	120.4 (6)
C22—Os2—S1	94.50 (18)	C4—C5—H5A	119.8
C21—Os2—S1	94.56 (17)	C6—C5—H5A	119.8
C23—Os2—Os1	115.27 (17)	C7—C6—C5	121.2 (6)
C22—Os2—Os1	135.51 (18)	C7—C6—H6A	119.4
C21—Os2—Os1	113.78 (17)	C5—C6—H6A	119.4
S1—Os2—Os1	54.00 (3)	C6—C7—C8	119.8 (6)
C23—Os2—Os3	91.62 (17)	C6—C7—H7A	120.1
C22—Os2—Os3	87.07 (18)	C8—C7—H7A	120.1
C21—Os2—Os3	173.95 (17)	N1—C8—C9	122.3 (5)
S1—Os2—Os3	81.12 (3)	N1—C8—C7	118.5 (5)
Os1—Os2—Os3	60.236 (8)	C9—C8—C7	119.1 (5)
C23—Os2—H1	85 (2)	C3—C9—C8	117.3 (5)
C22—Os2—H1	172 (3)	C3—C9—C4	123.3 (5)
C21—Os2—H1	90 (2)	C8—C9—C4	119.3 (5)
S1—Os2—H1	86 (2)	O11—C11—Os1	177.7 (5)
Os1—Os2—H1	41 (2)	O12—C12—Os1	179.1 (6)
Os3—Os2—H1	86 (2)	O13—C13—Os1	173.5 (5)
C33—Os3—C34	99.9 (3)	O21—C21—Os2	174.3 (5)
C33—Os3—C31	93.3 (2)	O22—C22—Os2	176.8 (6)
C34—Os3—C31	94.2 (2)	O23—C23—Os2	178.2 (6)
C33—Os3—C32	88.3 (2)	O31—C31—Os3	179.3 (6)
C34—Os3—C32	92.1 (3)	O32—C32—Os3	175.0 (5)
C31—Os3—C32	173.2 (2)	O33—C33—Os3	177.1 (6)
C33—Os3—Os2	101.9 (2)	O34—C34—Os3	177.0 (6)

C11—Os1—Os2—C23	128.2 (3)	S1—Os1—Os3—C31	−138.78 (18)
C12—Os1—Os2—C23	4.5 (3)	Os2—Os1—Os3—C31	−85.37 (18)
C13—Os1—Os2—C23	−100.2 (3)	C11—Os1—Os3—C32	−59.4 (3)
S1—Os1—Os2—C23	177.8 (2)	C12—Os1—Os3—C32	−149.7 (3)
Os3—Os1—Os2—C23	76.47 (19)	S1—Os1—Os3—C32	35.40 (19)
C11—Os1—Os2—C22	3.5 (4)	Os2—Os1—Os3—C32	88.80 (18)
C12—Os1—Os2—C22	−120.2 (3)	C11—Os1—Os3—Os2	−148.20 (18)
C13—Os1—Os2—C22	135.1 (3)	C12—Os1—Os3—Os2	121.52 (19)
S1—Os1—Os2—C22	53.1 (3)	S1—Os1—Os3—Os2	−53.41 (3)
Os3—Os1—Os2—C22	−48.2 (3)	C23—Os2—S1—C1	−116.8 (10)
C11—Os1—Os2—C21	−127.3 (3)	C22—Os2—S1—C1	108.1 (3)
C12—Os1—Os2—C21	109.0 (3)	C21—Os2—S1—C1	10.2 (3)
C13—Os1—Os2—C21	4.3 (3)	Os1—Os2—S1—C1	−106.0 (2)
S1—Os1—Os2—C21	−77.71 (19)	Os3—Os2—S1—C1	−165.5 (2)
Os3—Os1—Os2—C21	−179.00 (19)	C23—Os2—S1—Os1	−10.7 (10)
C11—Os1—Os2—S1	−49.6 (3)	C22—Os2—S1—Os1	−145.81 (18)
C12—Os1—Os2—S1	−173.3 (2)	C21—Os2—S1—Os1	116.24 (18)
C13—Os1—Os2—S1	82.0 (2)	Os3—Os2—S1—Os1	−59.50 (2)
Os3—Os1—Os2—S1	−101.29 (4)	C11—Os1—S1—C1	−105.0 (3)
C11—Os1—Os2—Os3	51.7 (2)	C12—Os1—S1—C1	138.3 (10)
C12—Os1—Os2—Os3	−72.0 (2)	C13—Os1—S1—C1	−6.5 (3)
C13—Os1—Os2—Os3	−176.69 (19)	Os2—Os1—S1—C1	105.81 (19)
S1—Os1—Os2—Os3	101.29 (4)	Os3—Os1—S1—C1	165.19 (19)
C23—Os2—Os3—C33	60.7 (3)	C11—Os1—S1—Os2	149.15 (17)
C22—Os2—Os3—C33	−32.5 (3)	C12—Os1—S1—Os2	32.5 (10)
S1—Os2—Os3—C33	−127.50 (19)	C13—Os1—S1—Os2	−112.27 (19)
Os1—Os2—Os3—C33	179.09 (19)	Os3—Os1—S1—Os2	59.38 (2)
C23—Os2—Os3—C34	−115.1 (5)	C8—N1—C1—C2	−2.0 (8)
C22—Os2—Os3—C34	151.7 (5)	C8—N1—C1—S1	175.3 (4)
S1—Os2—Os3—C34	56.7 (5)	Os2—S1—C1—N1	51.1 (5)
Os1—Os2—Os3—C34	3.3 (5)	Os1—S1—C1—N1	−26.7 (5)
C23—Os2—Os3—C31	−31.2 (2)	Os2—S1—C1—C2	−131.3 (4)
C22—Os2—Os3—C31	−124.4 (2)	Os1—S1—C1—C2	150.8 (4)
S1—Os2—Os3—C31	140.59 (17)	N1—C1—C2—C3	1.9 (9)
Os1—Os2—Os3—C31	87.18 (17)	S1—C1—C2—C3	−175.6 (4)
C23—Os2—Os3—C32	149.0 (2)	C1—C2—C3—C9	0.3 (9)
C22—Os2—Os3—C32	55.8 (2)	C9—C4—C5—C6	−0.5 (10)
S1—Os2—Os3—C32	−39.19 (17)	C4—C5—C6—C7	−0.8 (11)
Os1—Os2—Os3—C32	−92.60 (17)	C5—C6—C7—C8	1.6 (10)
C23—Os2—Os3—Os1	−118.41 (18)	C1—N1—C8—C9	0.1 (8)
C22—Os2—Os3—Os1	148.44 (18)	C1—N1—C8—C7	−176.2 (6)
S1—Os2—Os3—Os1	53.42 (3)	C6—C7—C8—N1	175.4 (6)
C11—Os1—Os3—C33	−151.0 (6)	C6—C7—C8—C9	−1.0 (9)
C12—Os1—Os3—C33	118.7 (6)	C2—C3—C9—C8	−2.0 (8)
S1—Os1—Os3—C33	−56.2 (6)	C2—C3—C9—C4	176.3 (6)
Os2—Os1—Os3—C33	−2.8 (6)	N1—C8—C9—C3	1.9 (8)
C11—Os1—Os3—C34	33.0 (3)	C7—C8—C9—C3	178.2 (6)
C12—Os1—Os3—C34	−57.3 (3)	N1—C8—C9—C4	−176.5 (5)
S1—Os1—Os3—C34	127.82 (18)	C7—C8—C9—C4	−0.2 (8)
Os2—Os1—Os3—C34	−178.77 (17)	C5—C4—C9—C3	−177.3 (6)
C11—Os1—Os3—C31	126.4 (3)	C5—C4—C9—C8	1.0 (9)
C12—Os1—Os3—C31	36.1 (3)

Experimental details

Crystal data
Chemical formula	[Os₃(C₉H₆NS)H(CO)₁₀]
M_r	1012.02
Crystal system, space group	Monoclinic, P2₁/n
Temperature (K)	223
a, b, c (Å)	9.3593 (5), 9.4129 (5), 25.7433 (14)
β (°)	93.045 (1)
V (Å³)	2264.7 (2)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	16.94
Crystal size (mm)	0.18 × 0.16 × 0.14

Data collection
Diffractometer	Rigaku Scxmini 1K CCD area-detector diffractometer
Absorption correction	Multi-scan (CrystalClear; Rigaku, 2005)
T_min, T_max	0.058, 0.092
No. of measured, independent and observed [I > 2σ(I)] reflections	13690, 4446, 4162
R_int	0.032
(sin θ/λ)_max (Å⁻¹)	0.617

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.024, 0.052, 1.14
No. of reflections	4446
No. of parameters	311
No. of restraints	1
H-atom treatment	H atoms treated by a mixture of independent and constrained refinement
Δρ_max, Δρ_min (e Å⁻³)	0.75, −1.24

Computer programs: CrystalClear (Rigaku, 2005), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

Selected bond lengths (Å) top

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

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. Web of Science CSD CrossRef CAS Google Scholar
Fan, W., Zhang, R., Leong, W. K. & Yan, Y. K. (2004). Inorg. Chim. Acta, 357, 2441–2450. Web of Science CSD CrossRef CAS Google Scholar
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Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Zeller, M., Hunter, A. D., Regula, J. L. & Szalay, P. S. (2003). Acta Cryst. E59, m975–m976. Web of Science CSD CrossRef IUCr Journals Google Scholar

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