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Acta Crystallogr Sect E Struct Rep Online. 2008 May 1; 64(Pt 5): m608.
Published online 2008 April 2. doi:  10.1107/S1600536808004881
PMCID: PMC2961200

Decacarbonyl-1κ3 C,2κ3 C,3κ4 C-μ-hydrido-1:2κ2 H:H-(μ-quinoline-2-thiol­ato-1:2κ2 S:S)diosmium(I)osmium(0)(3 OsOs)

Abstract

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 [triangle]); Fan et al. (2004 [triangle]); Miyake et al. (2007 [triangle]); Zeller et al. (2003 [triangle]).

An external file that holds a picture, illustration, etc.
Object name is e-64-0m608-scheme1.jpg

Experimental

Crystal data

  • [Os3(C9H6NS)H(CO)10]
  • M r = 1012.02
  • Monoclinic, An external file that holds a picture, illustration, etc.
Object name is e-64-0m608-efi1.jpg
  • 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 [triangle]) 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[F 2 > 2σ(F 2)] = 0.024
  • wR(F 2) = 0.052
  • S = 1.14
  • 4446 reflections
  • 311 parameters
  • 1 restraint
  • H atoms treated by a mixture of independent and constrained refinement
  • Δρmax = 0.75 e Å−3
  • Δρmin = −1.24 e Å−3

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

Table 1
Selected bond lengths (Å)

Supplementary Material

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

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

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

supplementary crystallographic information

Comment

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.

Experimental

[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.

Refinement

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.

Figures

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

Crystal data

[Os3(C9H6NS)H(CO)10]F000 = 1808
Mr = 1012.02Dx = 2.968 Mg m3
Monoclinic, P21/nMo Kα radiation λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 4762 reflections
a = 9.3593 (5) Åθ = 3.0–26.1º
b = 9.4129 (5) ŵ = 16.94 mm1
c = 25.7433 (14) ÅT = 223 (2) K
β = 93.045 (1)ºBlock, colourless
V = 2264.7 (2) Å30.18 × 0.16 × 0.14 mm
Z = 4

Data collection

Rigaku Scxmini 1K CCD area-detector diffractometer4446 independent reflections
Radiation source: fine-focus sealed tube4162 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.032
T = 223(2) Kθmax = 26.0º
ω scansθmin = 2.3º
Absorption correction: multi-scan(CrystalClear; Rigaku, 2005)h = −10→11
Tmin = 0.058, Tmax = 0.092k = −11→8
13690 measured reflectionsl = −31→31

Refinement

Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.024H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.052  w = 1/[σ2(Fo2) + (0.0163P)2 + 2.1547P] where P = (Fo2 + 2Fc2)/3
S = 1.14(Δ/σ)max = 0.001
4446 reflectionsΔρmax = 0.75 e Å3
311 parametersΔρmin = −1.24 e Å3
1 restraintExtinction correction: none
Primary atom site location: structure-invariant direct methods

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

xyzUiso*/Ueq
Os10.76242 (2)0.01890 (2)0.169927 (8)0.01740 (6)
Os20.97667 (2)−0.15956 (2)0.130925 (8)0.01676 (6)
Os31.04641 (2)0.12428 (2)0.161547 (8)0.01774 (6)
N10.5984 (5)−0.2445 (5)0.08694 (18)0.0239 (11)
S10.79273 (14)−0.03585 (15)0.07951 (5)0.0200 (3)
O110.6461 (5)0.3150 (5)0.1487 (2)0.0434 (12)
O120.7862 (5)0.0836 (5)0.28569 (17)0.0401 (11)
O130.4768 (5)−0.1310 (5)0.18287 (19)0.0414 (12)
O210.8805 (5)−0.4583 (5)0.09893 (18)0.0402 (11)
O221.1990 (5)−0.1242 (5)0.0512 (2)0.0465 (13)
O231.1859 (5)−0.2826 (5)0.21235 (18)0.0426 (12)
O311.1025 (5)−0.0142 (5)0.26916 (17)0.0384 (11)
O320.9894 (5)0.2326 (5)0.04959 (18)0.0426 (12)
O331.3613 (5)0.1450 (6)0.1407 (2)0.0605 (17)
O341.0082 (6)0.4241 (5)0.20439 (19)0.0471 (13)
H10.851 (7)−0.156 (8)0.184 (3)0.09 (3)*
C10.6572 (5)−0.1579 (6)0.0552 (2)0.0183 (11)
C20.6192 (6)−0.1465 (6)0.0019 (2)0.0227 (12)
H2A0.6674−0.0837−0.01950.027*
C30.5099 (6)−0.2299 (7)−0.0178 (2)0.0281 (13)
H3A0.4821−0.2252−0.05340.034*
C40.3199 (6)−0.4058 (7)−0.0022 (3)0.0304 (14)
H4A0.2871−0.4038−0.03740.036*
C50.2526 (6)−0.4889 (7)0.0322 (3)0.0349 (16)
H5A0.1730−0.54360.02070.042*
C60.3013 (7)−0.4935 (7)0.0844 (3)0.0374 (16)
H6A0.2530−0.55060.10780.045*
C70.4172 (7)−0.4170 (7)0.1020 (3)0.0332 (15)
H7A0.4499−0.42310.13710.040*
C80.4886 (5)−0.3279 (6)0.0673 (2)0.0197 (12)
C90.4392 (5)−0.3222 (6)0.0148 (2)0.0213 (12)
C110.6869 (6)0.2026 (7)0.1567 (2)0.0267 (13)
C120.7783 (6)0.0587 (7)0.2424 (2)0.0268 (13)
C130.5842 (6)−0.0799 (7)0.1754 (2)0.0279 (13)
C210.9088 (6)−0.3461 (6)0.1112 (2)0.0251 (13)
C221.1165 (6)−0.1414 (6)0.0804 (2)0.0276 (14)
C231.1095 (6)−0.2351 (6)0.1818 (2)0.0245 (13)
C311.0809 (6)0.0373 (6)0.2294 (2)0.0243 (13)
C321.0046 (6)0.1898 (7)0.0897 (2)0.0259 (13)
C331.2440 (6)0.1335 (7)0.1489 (3)0.0311 (15)
C341.0190 (6)0.3122 (7)0.1892 (2)0.0263 (13)

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
Os10.01208 (11)0.01895 (12)0.02128 (12)−0.00154 (8)0.00173 (8)−0.00144 (8)
Os20.01364 (11)0.01579 (11)0.02091 (12)−0.00091 (8)0.00137 (8)−0.00040 (8)
Os30.01302 (11)0.01713 (11)0.02298 (12)−0.00306 (8)0.00002 (8)−0.00002 (8)
N10.021 (2)0.027 (3)0.023 (3)−0.005 (2)−0.0013 (19)0.002 (2)
S10.0181 (6)0.0206 (7)0.0212 (7)−0.0043 (5)−0.0009 (5)0.0022 (5)
O110.038 (3)0.031 (3)0.061 (3)0.006 (2)−0.006 (2)−0.006 (2)
O120.048 (3)0.050 (3)0.023 (2)0.001 (2)0.005 (2)−0.007 (2)
O130.028 (2)0.046 (3)0.051 (3)−0.017 (2)0.013 (2)−0.009 (2)
O210.051 (3)0.023 (2)0.045 (3)−0.008 (2)−0.011 (2)−0.008 (2)
O220.045 (3)0.037 (3)0.061 (3)0.005 (2)0.036 (3)−0.001 (2)
O230.041 (3)0.042 (3)0.044 (3)0.013 (2)−0.014 (2)0.005 (2)
O310.046 (3)0.041 (3)0.027 (2)−0.008 (2)−0.011 (2)0.002 (2)
O320.050 (3)0.042 (3)0.035 (3)−0.017 (2)−0.004 (2)0.015 (2)
O330.019 (3)0.075 (4)0.089 (4)−0.004 (2)0.005 (3)0.034 (3)
O340.072 (4)0.027 (3)0.043 (3)0.001 (3)0.005 (3)−0.009 (2)
C10.012 (2)0.021 (3)0.021 (3)−0.001 (2)−0.006 (2)−0.002 (2)
C20.023 (3)0.024 (3)0.022 (3)−0.005 (2)0.000 (2)0.001 (2)
C30.028 (3)0.032 (3)0.024 (3)−0.001 (3)−0.003 (2)0.000 (3)
C40.026 (3)0.026 (3)0.038 (4)−0.001 (3)−0.005 (3)−0.009 (3)
C50.017 (3)0.031 (4)0.055 (4)−0.012 (3)−0.002 (3)−0.004 (3)
C60.035 (4)0.030 (4)0.048 (4)−0.010 (3)0.012 (3)0.007 (3)
C70.033 (3)0.035 (4)0.032 (4)−0.015 (3)0.001 (3)0.006 (3)
C80.015 (3)0.022 (3)0.023 (3)−0.003 (2)0.002 (2)0.001 (2)
C90.013 (3)0.023 (3)0.028 (3)0.001 (2)0.002 (2)−0.003 (2)
C110.017 (3)0.030 (4)0.033 (3)0.003 (3)−0.005 (2)−0.007 (3)
C120.022 (3)0.025 (3)0.034 (4)−0.002 (3)0.009 (3)−0.003 (3)
C130.026 (3)0.030 (3)0.028 (3)−0.004 (3)0.004 (3)−0.002 (3)
C210.021 (3)0.027 (3)0.027 (3)0.001 (2)−0.004 (2)−0.001 (3)
C220.023 (3)0.026 (3)0.035 (3)0.005 (3)0.004 (3)−0.003 (3)
C230.026 (3)0.018 (3)0.029 (3)0.003 (2)0.000 (3)−0.003 (2)
C310.019 (3)0.025 (3)0.028 (3)−0.007 (2)−0.001 (2)0.000 (3)
C320.020 (3)0.029 (3)0.030 (3)−0.008 (2)0.002 (2)0.002 (3)
C330.021 (3)0.030 (3)0.041 (4)0.000 (3)−0.005 (3)0.012 (3)
C340.026 (3)0.028 (3)0.025 (3)−0.001 (3)0.001 (2)−0.001 (3)

Geometric parameters (Å, °)

Os1—C111.892 (6)O21—C211.130 (7)
Os1—C121.900 (6)O22—C221.118 (7)
Os1—C131.922 (6)O23—C231.127 (7)
Os1—S12.4154 (14)O31—C311.140 (7)
Os1—Os22.8399 (3)O32—C321.110 (7)
Os1—Os32.8559 (3)O33—C331.134 (7)
Os1—H11.87 (6)O34—C341.130 (7)
Os2—C231.896 (6)C1—C21.404 (8)
Os2—C221.901 (6)C2—C31.366 (8)
Os2—C211.926 (6)C2—H2A0.9400
Os2—S12.4144 (13)C3—C91.399 (8)
Os2—Os32.8516 (3)C3—H3A0.9400
Os2—H11.86 (6)C4—C51.361 (9)
Os3—C331.897 (6)C4—C91.417 (8)
Os3—C341.929 (6)C4—H4A0.9400
Os3—C311.941 (6)C5—C61.397 (9)
Os3—C321.970 (6)C5—H5A0.9400
N1—C11.297 (7)C6—C71.360 (9)
N1—C81.369 (7)C6—H6A0.9400
S1—C11.799 (5)C7—C81.418 (8)
O11—C111.140 (7)C7—H7A0.9400
O12—C121.138 (7)C8—C91.406 (8)
O13—C131.139 (7)
C11—Os1—C1290.3 (3)C34—Os3—Os2158.16 (17)
C11—Os1—C1397.9 (3)C31—Os3—Os283.02 (17)
C12—Os1—C1392.6 (2)C32—Os3—Os290.14 (18)
C11—Os1—S194.81 (18)C33—Os3—Os1161.6 (2)
C12—Os1—S1168.73 (17)C34—Os3—Os198.51 (17)
C13—Os1—S196.58 (18)C31—Os3—Os184.06 (16)
C11—Os1—Os2137.83 (19)C32—Os3—Os192.31 (16)
C12—Os1—Os2116.33 (18)Os2—Os3—Os159.679 (7)
C13—Os1—Os2111.83 (19)C1—N1—C8117.6 (5)
S1—Os1—Os253.97 (3)C1—S1—Os2110.59 (18)
C11—Os1—Os390.53 (17)C1—S1—Os1110.76 (19)
C12—Os1—Os388.91 (17)Os2—S1—Os172.03 (4)
C13—Os1—Os3171.38 (19)N1—C1—C2124.7 (5)
S1—Os1—Os381.02 (3)N1—C1—S1119.8 (4)
Os2—Os1—Os360.085 (8)C2—C1—S1115.4 (4)
C11—Os1—H1176 (3)C3—C2—C1117.7 (5)
C12—Os1—H188 (2)C3—C2—H2A121.1
C13—Os1—H186 (2)C1—C2—H2A121.1
S1—Os1—H186 (2)C2—C3—C9120.2 (5)
Os2—Os1—H140 (2)C2—C3—H3A119.9
Os3—Os1—H185 (2)C9—C3—H3A119.9
C23—Os2—C2293.2 (3)C5—C4—C9120.1 (6)
C23—Os2—C2192.0 (2)C5—C4—H4A119.9
C22—Os2—C2197.5 (3)C9—C4—H4A119.9
C23—Os2—S1169.10 (18)C4—C5—C6120.4 (6)
C22—Os2—S194.50 (18)C4—C5—H5A119.8
C21—Os2—S194.56 (17)C6—C5—H5A119.8
C23—Os2—Os1115.27 (17)C7—C6—C5121.2 (6)
C22—Os2—Os1135.51 (18)C7—C6—H6A119.4
C21—Os2—Os1113.78 (17)C5—C6—H6A119.4
S1—Os2—Os154.00 (3)C6—C7—C8119.8 (6)
C23—Os2—Os391.62 (17)C6—C7—H7A120.1
C22—Os2—Os387.07 (18)C8—C7—H7A120.1
C21—Os2—Os3173.95 (17)N1—C8—C9122.3 (5)
S1—Os2—Os381.12 (3)N1—C8—C7118.5 (5)
Os1—Os2—Os360.236 (8)C9—C8—C7119.1 (5)
C23—Os2—H185 (2)C3—C9—C8117.3 (5)
C22—Os2—H1172 (3)C3—C9—C4123.3 (5)
C21—Os2—H190 (2)C8—C9—C4119.3 (5)
S1—Os2—H186 (2)O11—C11—Os1177.7 (5)
Os1—Os2—H141 (2)O12—C12—Os1179.1 (6)
Os3—Os2—H186 (2)O13—C13—Os1173.5 (5)
C33—Os3—C3499.9 (3)O21—C21—Os2174.3 (5)
C33—Os3—C3193.3 (2)O22—C22—Os2176.8 (6)
C34—Os3—C3194.2 (2)O23—C23—Os2178.2 (6)
C33—Os3—C3288.3 (2)O31—C31—Os3179.3 (6)
C34—Os3—C3292.1 (3)O32—C32—Os3175.0 (5)
C31—Os3—C32173.2 (2)O33—C33—Os3177.1 (6)
C33—Os3—Os2101.9 (2)O34—C34—Os3177.0 (6)
C11—Os1—Os2—C23128.2 (3)S1—Os1—Os3—C31−138.78 (18)
C12—Os1—Os2—C234.5 (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—C23177.8 (2)C12—Os1—Os3—C32−149.7 (3)
Os3—Os1—Os2—C2376.47 (19)S1—Os1—Os3—C3235.40 (19)
C11—Os1—Os2—C223.5 (4)Os2—Os1—Os3—C3288.80 (18)
C12—Os1—Os2—C22−120.2 (3)C11—Os1—Os3—Os2−148.20 (18)
C13—Os1—Os2—C22135.1 (3)C12—Os1—Os3—Os2121.52 (19)
S1—Os1—Os2—C2253.1 (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—C1108.1 (3)
C12—Os1—Os2—C21109.0 (3)C21—Os2—S1—C110.2 (3)
C13—Os1—Os2—C214.3 (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—Os1116.24 (18)
C13—Os1—Os2—S182.0 (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—Os351.7 (2)C12—Os1—S1—C1138.3 (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—C1105.81 (19)
S1—Os1—Os2—Os3101.29 (4)Os3—Os1—S1—C1165.19 (19)
C23—Os2—Os3—C3360.7 (3)C11—Os1—S1—Os2149.15 (17)
C22—Os2—Os3—C33−32.5 (3)C12—Os1—S1—Os232.5 (10)
S1—Os2—Os3—C33−127.50 (19)C13—Os1—S1—Os2−112.27 (19)
Os1—Os2—Os3—C33179.09 (19)Os3—Os1—S1—Os259.38 (2)
C23—Os2—Os3—C34−115.1 (5)C8—N1—C1—C2−2.0 (8)
C22—Os2—Os3—C34151.7 (5)C8—N1—C1—S1175.3 (4)
S1—Os2—Os3—C3456.7 (5)Os2—S1—C1—N151.1 (5)
Os1—Os2—Os3—C343.3 (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—C2150.8 (4)
S1—Os2—Os3—C31140.59 (17)N1—C1—C2—C31.9 (9)
Os1—Os2—Os3—C3187.18 (17)S1—C1—C2—C3−175.6 (4)
C23—Os2—Os3—C32149.0 (2)C1—C2—C3—C90.3 (9)
C22—Os2—Os3—C3255.8 (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—C81.6 (10)
C23—Os2—Os3—Os1−118.41 (18)C1—N1—C8—C90.1 (8)
C22—Os2—Os3—Os1148.44 (18)C1—N1—C8—C7−176.2 (6)
S1—Os2—Os3—Os153.42 (3)C6—C7—C8—N1175.4 (6)
C11—Os1—Os3—C33−151.0 (6)C6—C7—C8—C9−1.0 (9)
C12—Os1—Os3—C33118.7 (6)C2—C3—C9—C8−2.0 (8)
S1—Os1—Os3—C33−56.2 (6)C2—C3—C9—C4176.3 (6)
Os2—Os1—Os3—C33−2.8 (6)N1—C8—C9—C31.9 (8)
C11—Os1—Os3—C3433.0 (3)C7—C8—C9—C3178.2 (6)
C12—Os1—Os3—C34−57.3 (3)N1—C8—C9—C4−176.5 (5)
S1—Os1—Os3—C34127.82 (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—C31126.4 (3)C5—C4—C9—C81.0 (9)
C12—Os1—Os3—C3136.1 (3)

Footnotes

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

References

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