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metal-organic compounds
The title compound, [Os3(C6F5NHNH2)(CO)10], contains a near regular triangle of Os atoms. Two of the metal atoms are bridged by the hydrazine group of the C6F5NHNH2 ligand. Ten carbonyl groups complete the cluster, resulting in a distorted octahedral coordination for each Os atom.
Supporting information
 | Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805034471/hb6290sup1.cif |
 | Structure factor file (CIF format) https://doi.org/10.1107/S1600536805034471/hb6290Isup2.hkl |
CCDC reference: 289760
Key indicators
- Single-crystal X-ray study
- T = 285 K
- Mean
![[sigma]](//journals.iucr.org/logos/entities/sigma_rmgif.gif)
(C-C) = 0.013 Å - R factor = 0.040
- wR factor = 0.112
- Data-to-parameter ratio = 19.3
![[sigma]](http://journals.iucr.org/logos/entities/sigma_rmgif.gif){kind=small}
(C-C) = 0.013 ÅcheckCIF/PLATON results
No syntax errors found
Alert level C PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ? PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Os1 - N2 .. 5.25 su PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 13 PLAT431_ALERT_2_C Short Inter HL..A Contact F2 .. O7 .. 2.97 Ang. PLAT431_ALERT_2_C Short Inter HL..A Contact F3 .. O2 .. 2.91 Ang. PLAT431_ALERT_2_C Short Inter HL..A Contact F3 .. O8 .. 2.92 Ang. PLAT432_ALERT_2_C Short Inter X...Y Contact O5 .. C13 .. 3.01 Ang.
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 7 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 5 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion
Alert level C
Computing details top
Data collection: SMART (Bruker, 1998); cell refinement: SAINT (Bruker, 1998); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1998); software used to prepare material for publication: SHELXTL.
Crystal data top
| [Os3(C6H3F5N2)(CO)10] | Z = 4 |
| Mr = 1048.80 | F(000) = 1864 |
| Monoclinic, P21/c | Dx = 3.223 Mg m−3 |
| Hall symbol: -P 2ybc | Mo Kα radiation, λ = 0.71073 Å |
| a = 14.816 (3) Å | θ = 1.4–30.0° |
| b = 7.6177 (15) Å | µ = 17.69 mm−1 |
| c = 19.153 (4) Å | T = 285 K |
| β = 90.46 (3)° | Block, yellow |
| V = 2161.6 (7) Å3 | 0.18 × 0.16 × 0.15 mm |
Data collection top
| Bruker SMART CCD diffractometer | 6269 independent reflections |
| Radiation source: fine-focus sealed tube | 5341 reflections with I > 2σ(I) |
| Graphite monochromator | Rint = 0.060 |
| φ and ω scans | θmax = 30.0°, θmin = 1.4° |
| Absorption correction: multi-scan (SADABS; Bruker, 1998) | h = −20→13 |
| Tmin = 0.056, Tmax = 0.069 | k = −10→10 |
| 17316 measured reflections | l = −26→22 |
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)] = 0.040 | Hydrogen site location: inferred from neighbouring sites |
| wR(F2) = 0.112 | H-atom parameters constrained |
| S = 1.06 | w = 1/[σ2(Fo2) + (0.0533P)2] where P = (Fo2 + 2Fc2)/3 |
| 6269 reflections | (Δ/σ)max = 0.001 |
| 325 parameters | Δρmax = 2.48 e Å−3 |
| 0 restraints | Δρmin = −3.03 e Å−3 |
Special details top
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
| x | y | z | Uiso*/Ueq | ||
| Os1 | 0.16952 (2) | 0.80121 (3) | 0.425824 (13) | 0.02339 (9) | |
| C1 | 0.1793 (5) | 0.5965 (11) | 0.4852 (4) | 0.0319 (17) | |
| O1 | 0.1789 (5) | 0.4813 (9) | 0.5215 (3) | 0.0481 (17) | |
| F1 | 0.4437 (4) | 0.5676 (7) | 0.4334 (3) | 0.0434 (12) | |
| N2 | 0.3057 (5) | 0.8552 (9) | 0.4511 (4) | 0.0350 (15) | |
| H1A | 0.3096 | 0.9581 | 0.4740 | 0.042* | |
| H1B | 0.3279 | 0.7704 | 0.4791 | 0.042* | |
| Os2 | 0.27955 (2) | 0.82455 (4) | 0.302177 (13) | 0.02404 (9) | |
| C2 | 0.1246 (6) | 0.9441 (10) | 0.4999 (4) | 0.0303 (15) | |
| O2 | 0.0976 (5) | 1.0269 (9) | 0.5436 (3) | 0.0444 (15) | |
| F2 | 0.6254 (4) | 0.5552 (8) | 0.4388 (3) | 0.0555 (15) | |
| N1 | 0.3497 (5) | 0.8623 (9) | 0.3972 (3) | 0.0308 (14) | |
| H2A | 0.3452 | 0.9813 | 0.3945 | 0.037* | |
| Os3 | 0.15871 (2) | 1.10302 (4) | 0.338609 (14) | 0.02473 (9) | |
| C3 | 0.0506 (6) | 0.7332 (10) | 0.3951 (4) | 0.0293 (15) | |
| O3 | −0.0183 (5) | 0.6844 (8) | 0.3756 (4) | 0.0452 (16) | |
| F3 | 0.7228 (4) | 0.8516 (10) | 0.4181 (3) | 0.0610 (17) | |
| C9 | 0.0688 (6) | 1.2325 (11) | 0.3882 (4) | 0.0347 (17) | |
| O9 | 0.0184 (5) | 1.3084 (8) | 0.4204 (4) | 0.0475 (16) | |
| F4 | 0.6384 (4) | 1.1539 (9) | 0.3841 (3) | 0.0549 (15) | |
| C10 | 0.0656 (6) | 0.9857 (10) | 0.2828 (4) | 0.0338 (17) | |
| O10 | 0.0096 (5) | 0.9245 (10) | 0.2517 (4) | 0.0535 (19) | |
| F5 | 0.4587 (4) | 1.1655 (8) | 0.3715 (4) | 0.0563 (15) | |
| C8 | 0.1846 (6) | 1.2661 (11) | 0.2646 (4) | 0.0345 (17) | |
| O6 | 0.1656 (6) | 0.7494 (12) | 0.1723 (4) | 0.066 (2) | |
| C7 | 0.2540 (6) | 1.1994 (10) | 0.3997 (4) | 0.0320 (16) | |
| O7 | 0.3053 (5) | 1.2648 (9) | 0.4339 (4) | 0.0463 (16) | |
| C6 | 0.2078 (7) | 0.7790 (13) | 0.2204 (4) | 0.040 (2) | |
| O8 | 0.1997 (6) | 1.3637 (10) | 0.2216 (4) | 0.059 (2) | |
| C5 | 0.3483 (7) | 0.9950 (12) | 0.2529 (4) | 0.0397 (19) | |
| O5 | 0.3893 (6) | 1.0922 (11) | 0.2221 (4) | 0.067 (2) | |
| C4 | 0.3549 (6) | 0.6262 (11) | 0.2832 (4) | 0.0335 (17) | |
| O4 | 0.3998 (5) | 0.5087 (10) | 0.2696 (4) | 0.0535 (18) | |
| C11 | 0.4462 (6) | 0.8671 (12) | 0.4062 (4) | 0.0332 (16) | |
| C12 | 0.4909 (6) | 0.7113 (11) | 0.4233 (4) | 0.0321 (16) | |
| C13 | 0.5835 (6) | 0.7080 (13) | 0.4265 (4) | 0.0389 (19) | |
| C14 | 0.6328 (6) | 0.8587 (14) | 0.4144 (4) | 0.0392 (19) | |
| C15 | 0.5908 (6) | 1.0103 (12) | 0.3986 (4) | 0.0367 (19) | |
| C16 | 0.4986 (7) | 1.0133 (12) | 0.3920 (5) | 0.0398 (19) |
Atomic displacement parameters (Å2) top
| U11 | U22 | U33 | U12 | U13 | U23 | |
| Os1 | 0.01940 (15) | 0.02428 (15) | 0.02647 (14) | 0.00152 (10) | −0.00063 (11) | 0.00087 (8) |
| C1 | 0.019 (4) | 0.042 (5) | 0.035 (4) | 0.000 (3) | 0.000 (3) | 0.004 (3) |
| O1 | 0.044 (4) | 0.041 (4) | 0.059 (4) | 0.013 (3) | −0.001 (3) | 0.025 (3) |
| F1 | 0.036 (3) | 0.041 (3) | 0.053 (3) | −0.001 (2) | −0.012 (2) | 0.007 (2) |
| N2 | 0.035 (4) | 0.030 (3) | 0.040 (3) | 0.005 (3) | 0.001 (3) | 0.004 (3) |
| Os2 | 0.02091 (15) | 0.02988 (17) | 0.02127 (13) | 0.00283 (11) | −0.00440 (10) | −0.00093 (8) |
| C2 | 0.024 (4) | 0.033 (4) | 0.033 (3) | −0.007 (3) | −0.005 (3) | −0.006 (3) |
| O2 | 0.039 (4) | 0.052 (4) | 0.042 (3) | 0.002 (3) | 0.004 (3) | −0.017 (3) |
| F2 | 0.035 (3) | 0.066 (4) | 0.066 (4) | 0.023 (3) | −0.013 (3) | 0.012 (3) |
| N1 | 0.034 (4) | 0.034 (3) | 0.024 (3) | 0.001 (3) | −0.011 (3) | −0.002 (2) |
| Os3 | 0.02070 (15) | 0.02300 (16) | 0.03038 (14) | 0.00107 (10) | −0.00712 (11) | 0.00137 (9) |
| C3 | 0.022 (4) | 0.029 (4) | 0.037 (4) | 0.005 (3) | 0.001 (3) | 0.000 (3) |
| O3 | 0.031 (4) | 0.039 (4) | 0.066 (4) | −0.007 (3) | −0.006 (3) | −0.008 (3) |
| F3 | 0.020 (3) | 0.106 (5) | 0.057 (3) | 0.001 (3) | −0.006 (3) | 0.014 (3) |
| C9 | 0.026 (4) | 0.034 (4) | 0.043 (4) | −0.006 (4) | −0.010 (3) | 0.005 (3) |
| O9 | 0.036 (4) | 0.037 (4) | 0.071 (4) | 0.005 (3) | 0.009 (3) | −0.008 (3) |
| F4 | 0.037 (3) | 0.075 (4) | 0.053 (3) | −0.029 (3) | 0.001 (3) | 0.008 (3) |
| C10 | 0.030 (4) | 0.028 (4) | 0.043 (4) | −0.006 (3) | −0.017 (3) | 0.001 (3) |
| O10 | 0.038 (4) | 0.065 (5) | 0.058 (4) | −0.011 (3) | −0.027 (3) | 0.007 (3) |
| F5 | 0.045 (4) | 0.042 (3) | 0.082 (4) | −0.003 (3) | −0.009 (3) | 0.016 (3) |
| C8 | 0.031 (4) | 0.030 (4) | 0.042 (4) | −0.004 (3) | −0.009 (3) | 0.003 (3) |
| O6 | 0.070 (6) | 0.078 (5) | 0.049 (4) | 0.015 (5) | −0.028 (4) | −0.012 (4) |
| C7 | 0.029 (4) | 0.028 (4) | 0.039 (4) | −0.004 (3) | −0.004 (3) | −0.005 (3) |
| O7 | 0.036 (4) | 0.043 (4) | 0.059 (4) | −0.002 (3) | −0.014 (3) | −0.017 (3) |
| C6 | 0.037 (5) | 0.053 (5) | 0.030 (4) | 0.015 (4) | −0.013 (3) | −0.009 (3) |
| O8 | 0.067 (6) | 0.057 (4) | 0.053 (4) | −0.009 (4) | 0.000 (4) | 0.018 (3) |
| C5 | 0.038 (5) | 0.047 (5) | 0.034 (4) | −0.003 (4) | −0.001 (3) | 0.003 (3) |
| O5 | 0.060 (6) | 0.078 (6) | 0.063 (5) | −0.012 (4) | 0.017 (4) | 0.018 (4) |
| C4 | 0.030 (4) | 0.037 (4) | 0.033 (4) | 0.005 (4) | −0.002 (3) | −0.001 (3) |
| O4 | 0.047 (4) | 0.053 (4) | 0.061 (4) | 0.020 (4) | 0.000 (3) | −0.010 (3) |
| C11 | 0.022 (4) | 0.044 (4) | 0.034 (4) | 0.003 (4) | 0.002 (3) | −0.001 (3) |
| C12 | 0.023 (4) | 0.041 (4) | 0.031 (3) | 0.001 (3) | −0.005 (3) | 0.004 (3) |
| C13 | 0.028 (4) | 0.055 (5) | 0.033 (4) | 0.008 (4) | −0.008 (3) | −0.002 (3) |
| C14 | 0.022 (4) | 0.070 (6) | 0.026 (3) | 0.000 (4) | −0.003 (3) | −0.001 (3) |
| C15 | 0.033 (5) | 0.050 (5) | 0.028 (3) | −0.016 (4) | 0.001 (3) | 0.000 (3) |
| C16 | 0.032 (5) | 0.038 (5) | 0.049 (4) | 0.002 (4) | 0.002 (4) | 0.007 (3) |
Geometric parameters (Å, º) top
| Os1—Os3 | 2.8456 (6) | Os3—C8 | 1.925 (8) |
| Os1—Os2 | 2.8912 (9) | Os3—C10 | 1.955 (8) |
| Os2—Os3 | 2.8657 (6) | Os3—C7 | 1.969 (8) |
| Os1—N2 | 2.112 (8) | C3—O3 | 1.146 (10) |
| Os2—N1 | 2.108 (6) | F3—C14 | 1.337 (10) |
| Os1—C2 | 1.912 (8) | C9—O9 | 1.131 (11) |
| Os1—C3 | 1.924 (8) | F4—C15 | 1.332 (10) |
| Os1—C1 | 1.935 (8) | C10—O10 | 1.119 (10) |
| C1—O1 | 1.119 (9) | F5—C16 | 1.358 (10) |
| F1—C12 | 1.314 (10) | C8—O8 | 1.134 (10) |
| N2—N1 | 1.226 (9) | O6—C6 | 1.132 (10) |
| N2—H1A | 0.9000 | C7—O7 | 1.117 (10) |
| N2—H1B | 0.9000 | C5—O5 | 1.127 (11) |
| Os2—C5 | 1.906 (9) | C4—O4 | 1.146 (10) |
| Os2—C4 | 1.916 (8) | C11—C16 | 1.386 (13) |
| Os2—C6 | 1.917 (8) | C11—C12 | 1.397 (12) |
| C2—O2 | 1.124 (9) | C12—C13 | 1.374 (12) |
| F2—C13 | 1.339 (10) | C13—C14 | 1.381 (14) |
| N1—C11 | 1.440 (10) | C14—C15 | 1.345 (14) |
| N1—H2A | 0.9100 | C15—C16 | 1.371 (12) |
| Os3—C9 | 1.916 (9) | ||
| Os1—Os3—Os2 | 60.82 (2) | C11—N1—H2A | 93.0 |
| Os3—Os1—Os2 | 59.93 (3) | Os2—N1—H2A | 93.0 |
| Os3—Os2—Os1 | 59.244 (16) | C9—Os3—C8 | 100.1 (4) |
| C2—Os1—C3 | 93.3 (3) | C9—Os3—C10 | 90.9 (4) |
| C2—Os1—C1 | 92.7 (3) | C8—Os3—C10 | 92.1 (3) |
| C3—Os1—C1 | 91.6 (3) | C9—Os3—C7 | 90.7 (3) |
| C2—Os1—N2 | 93.2 (3) | C8—Os3—C7 | 92.9 (3) |
| C3—Os1—N2 | 173.5 (3) | C10—Os3—C7 | 174.4 (3) |
| C1—Os1—N2 | 87.4 (3) | C9—Os3—Os1 | 99.3 (2) |
| C2—Os1—Os3 | 87.5 (2) | C8—Os3—Os1 | 160.5 (3) |
| C3—Os1—Os3 | 89.5 (2) | C10—Os3—Os1 | 89.3 (2) |
| C1—Os1—Os3 | 178.9 (2) | C7—Os3—Os1 | 85.2 (2) |
| N2—Os1—Os3 | 91.50 (19) | C9—Os3—Os2 | 160.1 (2) |
| C2—Os1—Os2 | 140.8 (2) | C8—Os3—Os2 | 99.8 (3) |
| C3—Os1—Os2 | 106.7 (2) | C10—Os3—Os2 | 88.2 (3) |
| C1—Os1—Os2 | 119.4 (2) | C7—Os3—Os2 | 88.5 (2) |
| N2—Os1—Os2 | 68.39 (18) | O3—C3—Os1 | 176.3 (7) |
| O1—C1—Os1 | 174.9 (8) | O9—C9—Os3 | 176.5 (8) |
| N1—N2—Os1 | 109.2 (6) | O10—C10—Os3 | 176.8 (9) |
| N1—N2—H1A | 109.8 | O8—C8—Os3 | 179.2 (9) |
| Os1—N2—H1A | 109.8 | O7—C7—Os3 | 175.3 (8) |
| N1—N2—H1B | 109.8 | O6—C6—Os2 | 178.9 (9) |
| Os1—N2—H1B | 109.8 | O5—C5—Os2 | 177.9 (9) |
| H1A—N2—H1B | 108.3 | O4—C4—Os2 | 177.9 (7) |
| C5—Os2—C4 | 97.4 (4) | C16—C11—C12 | 117.7 (8) |
| C5—Os2—C6 | 90.8 (4) | C16—C11—N1 | 123.6 (8) |
| C4—Os2—C6 | 91.3 (4) | C12—C11—N1 | 118.4 (8) |
| C5—Os2—N1 | 94.2 (3) | F1—C12—C13 | 120.7 (8) |
| C4—Os2—N1 | 89.3 (3) | F1—C12—C11 | 119.4 (8) |
| C6—Os2—N1 | 174.9 (4) | C13—C12—C11 | 119.8 (8) |
| C5—Os2—Os3 | 87.4 (3) | F2—C13—C12 | 119.0 (8) |
| C4—Os2—Os3 | 175.2 (3) | F2—C13—C14 | 120.5 (9) |
| C6—Os2—Os3 | 89.4 (3) | C12—C13—C14 | 120.5 (8) |
| N1—Os2—Os3 | 89.62 (19) | F3—C14—C15 | 120.4 (9) |
| C5—Os2—Os1 | 139.0 (3) | F3—C14—C13 | 119.1 (9) |
| C4—Os2—Os1 | 116.1 (2) | C15—C14—C13 | 120.5 (8) |
| C6—Os2—Os1 | 110.2 (3) | F4—C15—C14 | 120.5 (9) |
| N1—Os2—Os1 | 65.1 (2) | F4—C15—C16 | 119.7 (9) |
| O2—C2—Os1 | 179.3 (8) | C14—C15—C16 | 119.6 (8) |
| N2—N1—C11 | 115.8 (6) | F5—C16—C15 | 118.2 (8) |
| N2—N1—Os2 | 117.4 (6) | F5—C16—C11 | 120.0 (8) |
| C11—N1—Os2 | 126.1 (5) | C15—C16—C11 | 121.8 (8) |
| N2—N1—H2A | 93.0 |
