metal-organic compounds
Decacarbonyl-1κ3C,2κ3C,3κ4C-μ-hydrido-1:2κ2H:H-(μ-quinoline-2-thiolato-1:2κ2S:S)diosmium(I)osmium(0)(3 Os—Os)
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
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Refinement
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Data collection: CrystalClear (Rigaku, 2005); cell 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
10.1107/S1600536808004881/hy2117sup1.cif
contains datablocks I, global. DOI:Structure factors: contains datablock I. DOI: 10.1107/S1600536808004881/hy2117Isup2.hkl
[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.
H atoms bound to C were positioned geometrically and refined as riding atoms, with C—H = 0.94Å and Uiso(H) = 1.2Ueq(C). The hydride H atom was located from a difference Fourier map and refined isotropically.
Data collection: CrystalClear (Rigaku, 2005); cell
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).Fig. 1. The molecular structure of the title compound. Displacement ellipsoids are drawn at the 30% probability level. |
[Os3(C9H6NS)H(CO)10] | F(000) = 1808 |
Mr = 1012.02 | Dx = 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 |
Rigaku Scxmini 1K CCD area-detector diffractometer | 4446 independent reflections |
Radiation source: fine-focus sealed tube | 4162 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.032 |
ω scans | θmax = 26.0°, θmin = 2.3° |
Absorption correction: multi-scan (CrystalClear; Rigaku, 2005) | h = −10→11 |
Tmin = 0.058, Tmax = 0.092 | k = −11→8 |
13690 measured reflections | l = −31→31 |
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(Fo2) + (0.0163P)2 + 2.1547P] where P = (Fo2 + 2Fc2)/3 |
4446 reflections | (Δ/σ)max = 0.001 |
311 parameters | Δρmax = 0.75 e Å−3 |
1 restraint | Δρmin = −1.24 e Å−3 |
[Os3(C9H6NS)H(CO)10] | V = 2264.7 (2) Å3 |
Mr = 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)° |
Rigaku Scxmini 1K CCD area-detector diffractometer | 4446 independent reflections |
Absorption correction: multi-scan (CrystalClear; Rigaku, 2005) | 4162 reflections with I > 2σ(I) |
Tmin = 0.058, Tmax = 0.092 | Rint = 0.032 |
13690 measured reflections |
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 | Δρmax = 0.75 e Å−3 |
4446 reflections | Δρmin = −1.24 e Å−3 |
311 parameters |
x | y | z | Uiso*/Ueq | ||
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) |
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) |
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] |
Mr | 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) |
Tmin, Tmax | 0.058, 0.092 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 13690, 4446, 4162 |
Rint | 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 |
Δρmax, Δρmin (e Å−3) | 0.75, −1.24 |
Computer programs: CrystalClear (Rigaku, 2005), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).
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
Miyake, Y., Nomaguchi, Y., Yuki, M. & Nishibayashi, Y. (2007). Organometallics, 26, 3611–3613. Web of Science CSD CrossRef CAS Google Scholar
Rigaku (2005). CrystalClear. Rigaku Corporation, Tokyo, Japan. Google Scholar
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
This is an open-access article distributed under the terms of the Creative Commons Attribution (CC-BY) Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.
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.