Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680502338X/ng6168sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S160053680502338X/ng6168Isup2.hkl |
CCDC reference: 282550
Key indicators
- Single-crystal X-ray study
- T = 100 K
- Mean (C-C) = 0.009 Å
- R factor = 0.028
- wR factor = 0.067
- Data-to-parameter ratio = 13.6
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT029_ALERT_3_B _diffrn_measured_fraction_theta_full Low ....... 0.96 PLAT220_ALERT_2_B Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.84 Ratio
Alert level C PLAT066_ALERT_1_C Predicted and Reported Transmissions Identical . ? PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ? PLAT141_ALERT_4_C su on a - Axis Small or Missing (x 100000) ..... 10 Ang. PLAT142_ALERT_4_C su on b - Axis Small or Missing (x 100000) ..... 10 Ang. PLAT143_ALERT_4_C su on c - Axis Small or Missing (x 100000) ..... 20 Ang. PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.67 Ratio PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.33 Ratio PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Os1 - C1 .. 5.02 su PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 9
0 ALERT level A = In general: serious problem 2 ALERT level B = Potentially serious problem 9 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 3 ALERT type 2 Indicator that the structure model may be wrong or deficient 3 ALERT type 3 Indicator that the structure quality may be low 4 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Bruker, 2001); cell refinement: SAINT (Bruker, 2001); 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, 2001); software used to prepare material for publication: SHELXTL.
[Os3(C5H10NS2)H(CO)9] | F(000) = 3472 |
Mr = 971.96 | Dx = 3.026 Mg m−3 |
Monoclinic, P21/c | Cu Kα radiation, λ = 1.54178 Å |
a = 15.0412 (1) Å | Cell parameters from 9424 reflections |
b = 12.5376 (1) Å | θ = 3.9–70.6° |
c = 23.2430 (2) Å | µ = 35.26 mm−1 |
β = 103.191 (1)° | T = 100 K |
V = 4267.53 (6) Å3 | Prism, orange |
Z = 8 | 0.06 × 0.03 × 0.02 mm |
Bruker CCD area-detector diffractometer | 7285 independent reflections |
Radiation source: Rotating Anode | 7049 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.053 |
φ and ω scans | θmax = 67.1°, θmin = 3.0° |
Absorption correction: multi-scan (SADABS; Bruker, 2001) | h = −17→17 |
Tmin = 0.323, Tmax = 0.494 | k = −14→13 |
31582 measured reflections | l = −26→23 |
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)] = 0.028 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.067 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.18 | w = 1/[σ2(Fo2) + (0.024P)2 + 5.3186P] where P = (Fo2 + 2Fc2)/3 |
7285 reflections | (Δ/σ)max = 0.001 |
535 parameters | Δρmax = 1.66 e Å−3 |
0 restraints | Δρmin = −2.39 e Å−3 |
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. |
x | y | z | Uiso*/Ueq | ||
Os1 | 0.39914 (2) | 0.11178 (2) | 0.33180 (1) | 0.00756 (7) | |
Os2 | 0.43099 (2) | 0.33332 (2) | 0.33896 (1) | 0.00834 (7) | |
Os3 | 0.25089 (2) | 0.25918 (2) | 0.30690 (1) | 0.00869 (7) | |
Os4 | 0.15349 (2) | 0.67688 (2) | 0.45815 (1) | 0.00776 (7) | |
Os5 | 0.21186 (2) | 0.89019 (2) | 0.46096 (1) | 0.00789 (7) | |
Os6 | 0.02197 (2) | 0.84023 (2) | 0.42908 (1) | 0.01006 (7) | |
S1 | 0.43659 (10) | 0.33551 (11) | 0.23461 (6) | 0.0131 (3) | |
S2 | 0.30474 (9) | 0.15297 (10) | 0.23471 (6) | 0.0098 (3) | |
S3 | 0.16182 (10) | 0.66197 (10) | 0.35420 (6) | 0.0103 (3) | |
S4 | 0.11560 (9) | 0.89636 (10) | 0.36178 (6) | 0.0102 (3) | |
C1 | 0.5106 (4) | 0.1021 (4) | 0.3052 (2) | 0.0145 (13) | |
C2 | 0.3585 (4) | −0.0342 (5) | 0.3214 (2) | 0.0117 (12) | |
C3 | 0.4605 (4) | 0.0989 (4) | 0.4122 (3) | 0.0132 (12) | |
C4 | 0.5619 (4) | 0.3376 (4) | 0.3585 (2) | 0.0120 (12) | |
C5 | 0.4073 (4) | 0.4848 (5) | 0.3371 (2) | 0.0115 (12) | |
C6 | 0.4267 (4) | 0.3266 (4) | 0.4200 (3) | 0.0153 (13) | |
C7 | 0.2189 (4) | 0.3798 (5) | 0.2579 (3) | 0.0191 (14) | |
C8 | 0.2281 (4) | 0.3334 (5) | 0.3733 (3) | 0.0182 (14) | |
C9 | 0.1347 (4) | 0.1878 (5) | 0.2904 (3) | 0.0150 (12) | |
C10 | 0.3785 (4) | 0.2298 (4) | 0.1998 (2) | 0.0084 (11) | |
C11 | 0.3345 (4) | 0.1077 (5) | 0.1138 (3) | 0.0183 (13) | |
H11A | 0.3120 | 0.0608 | 0.1417 | 0.022* | |
H11B | 0.3768 | 0.0655 | 0.0958 | 0.022* | |
C12 | 0.2541 (5) | 0.1441 (6) | 0.0655 (3) | 0.0333 (18) | |
H12A | 0.2145 | 0.1906 | 0.0826 | 0.050* | |
H12B | 0.2193 | 0.0817 | 0.0475 | 0.050* | |
H12C | 0.2766 | 0.1834 | 0.0353 | 0.050* | |
C13 | 0.4456 (4) | 0.2584 (5) | 0.1157 (3) | 0.0176 (13) | |
H13A | 0.4593 | 0.2125 | 0.0842 | 0.021* | |
H13B | 0.5039 | 0.2738 | 0.1441 | 0.021* | |
C14 | 0.4045 (5) | 0.3622 (5) | 0.0885 (3) | 0.0274 (16) | |
H14A | 0.3494 | 0.3471 | 0.0579 | 0.041* | |
H14B | 0.4489 | 0.3996 | 0.0709 | 0.041* | |
H14C | 0.3885 | 0.4070 | 0.1192 | 0.041* | |
C15 | 0.2699 (4) | 0.6073 (4) | 0.4785 (3) | 0.0143 (13) | |
C16 | 0.0756 (4) | 0.5549 (5) | 0.4469 (2) | 0.0131 (12) | |
C17 | 0.1477 (4) | 0.6903 (5) | 0.5384 (3) | 0.0132 (12) | |
C18 | 0.3188 (4) | 0.8297 (5) | 0.4439 (3) | 0.0150 (13) | |
C19 | 0.2339 (4) | 1.0418 (5) | 0.4568 (2) | 0.0139 (12) | |
C20 | 0.2654 (4) | 0.8836 (4) | 0.5428 (3) | 0.0103 (12) | |
C21 | −0.0469 (4) | 0.7345 (5) | 0.3795 (3) | 0.0206 (14) | |
C22 | −0.0284 (4) | 0.8041 (5) | 0.4949 (3) | 0.0148 (12) | |
C23 | −0.0532 (4) | 0.9646 (5) | 0.4084 (3) | 0.0188 (13) | |
C24 | 0.1364 (4) | 0.7813 (4) | 0.3203 (2) | 0.0079 (11) | |
C25 | 0.1415 (4) | 0.7064 (5) | 0.2246 (2) | 0.0105 (11) | |
H25A | 0.1013 | 0.7171 | 0.1849 | 0.013* | |
H25B | 0.1236 | 0.6389 | 0.2409 | 0.013* | |
C26 | 0.2398 (4) | 0.6990 (5) | 0.2194 (2) | 0.0131 (12) | |
H26A | 0.2575 | 0.7658 | 0.2031 | 0.020* | |
H26B | 0.2463 | 0.6398 | 0.1931 | 0.020* | |
H26C | 0.2794 | 0.6866 | 0.2585 | 0.020* | |
C27 | 0.1131 (4) | 0.9007 (4) | 0.2336 (2) | 0.0103 (11) | |
H27A | 0.1435 | 0.9019 | 0.2000 | 0.012* | |
H27B | 0.1406 | 0.9577 | 0.2615 | 0.012* | |
C28 | 0.0117 (4) | 0.9235 (5) | 0.2107 (3) | 0.0190 (13) | |
H28A | −0.0151 | 0.8693 | 0.1815 | 0.029* | |
H28B | 0.0038 | 0.9942 | 0.1923 | 0.029* | |
H28C | −0.0188 | 0.9215 | 0.2437 | 0.029* | |
N1 | 0.3846 (3) | 0.1992 (4) | 0.1467 (2) | 0.0128 (10) | |
N2 | 0.1297 (3) | 0.7965 (4) | 0.26368 (19) | 0.0078 (9) | |
O1 | 0.5747 (3) | 0.0979 (3) | 0.28766 (19) | 0.0183 (9) | |
O2 | 0.3366 (3) | −0.1207 (3) | 0.31398 (19) | 0.0196 (10) | |
O3 | 0.4980 (3) | 0.0921 (4) | 0.4609 (2) | 0.0250 (10) | |
O4 | 0.6401 (3) | 0.3418 (3) | 0.3710 (2) | 0.0237 (10) | |
O5 | 0.3962 (3) | 0.5734 (4) | 0.3397 (2) | 0.0248 (10) | |
O6 | 0.4246 (3) | 0.3246 (4) | 0.4686 (2) | 0.0238 (10) | |
O7 | 0.1982 (3) | 0.4515 (4) | 0.2268 (2) | 0.0300 (11) | |
O8 | 0.2116 (3) | 0.3768 (4) | 0.4128 (2) | 0.0242 (10) | |
O9 | 0.0623 (3) | 0.1520 (4) | 0.2817 (2) | 0.0264 (11) | |
O10 | 0.3400 (3) | 0.5664 (4) | 0.4918 (2) | 0.0257 (10) | |
O11 | 0.0288 (3) | 0.4805 (4) | 0.4404 (2) | 0.0271 (11) | |
O12 | 0.1432 (3) | 0.6960 (4) | 0.58689 (18) | 0.0190 (9) | |
O13 | 0.3841 (3) | 0.7927 (4) | 0.43514 (19) | 0.0200 (9) | |
O14 | 0.2503 (3) | 1.1302 (3) | 0.45687 (19) | 0.0211 (10) | |
O15 | 0.3003 (3) | 0.8828 (4) | 0.59223 (18) | 0.0203 (10) | |
O16 | −0.0878 (3) | 0.6702 (4) | 0.3497 (2) | 0.0293 (12) | |
O17 | −0.0583 (3) | 0.7841 (4) | 0.5343 (2) | 0.0268 (11) | |
O18 | −0.1014 (3) | 1.0374 (4) | 0.3956 (2) | 0.0278 (11) | |
H1 | 0.284 (6) | 0.140 (7) | 0.357 (3) | 0.04 (2)* | |
H2 | 0.090 (7) | 0.948 (9) | 0.479 (5) | 0.04 (3)* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Os1 | 0.00375 (13) | 0.00858 (13) | 0.01046 (13) | 0.00045 (9) | 0.00182 (10) | 0.00111 (8) |
Os2 | 0.00527 (13) | 0.00917 (13) | 0.00994 (13) | −0.00104 (9) | 0.00039 (10) | −0.00092 (8) |
Os3 | 0.00334 (13) | 0.00961 (13) | 0.01298 (14) | 0.00107 (9) | 0.00153 (10) | 0.00063 (8) |
Os4 | 0.00518 (13) | 0.01040 (13) | 0.00765 (13) | 0.00082 (9) | 0.00138 (9) | 0.00055 (8) |
Os5 | 0.00498 (13) | 0.01014 (13) | 0.00831 (13) | 0.00039 (9) | 0.00104 (10) | −0.00093 (8) |
Os6 | 0.00359 (13) | 0.01591 (14) | 0.01025 (13) | 0.00326 (9) | 0.00071 (10) | −0.00290 (8) |
S1 | 0.0145 (7) | 0.0143 (7) | 0.0103 (7) | −0.0065 (5) | 0.0028 (6) | −0.0010 (4) |
S2 | 0.0060 (7) | 0.0108 (6) | 0.0119 (7) | −0.0019 (5) | 0.0006 (5) | 0.0007 (4) |
S3 | 0.0114 (7) | 0.0099 (6) | 0.0104 (7) | 0.0043 (5) | 0.0037 (5) | 0.0005 (4) |
S4 | 0.0100 (7) | 0.0123 (7) | 0.0077 (7) | 0.0038 (5) | 0.0010 (5) | −0.0006 (4) |
C1 | 0.019 (4) | 0.013 (3) | 0.009 (3) | 0.002 (2) | −0.001 (3) | −0.002 (2) |
C2 | 0.007 (3) | 0.013 (3) | 0.016 (3) | 0.000 (2) | 0.003 (2) | 0.005 (2) |
C3 | 0.009 (3) | 0.010 (3) | 0.020 (3) | 0.002 (2) | 0.003 (3) | −0.001 (2) |
C4 | 0.011 (3) | 0.011 (3) | 0.012 (3) | 0.001 (2) | 0.000 (2) | −0.0009 (19) |
C5 | 0.007 (3) | 0.015 (3) | 0.010 (3) | −0.001 (2) | −0.003 (2) | 0.000 (2) |
C6 | 0.010 (3) | 0.013 (3) | 0.020 (4) | 0.003 (2) | −0.003 (3) | −0.002 (2) |
C7 | 0.015 (3) | 0.020 (3) | 0.023 (3) | −0.003 (3) | 0.004 (3) | −0.002 (2) |
C8 | 0.013 (3) | 0.015 (3) | 0.024 (4) | −0.002 (2) | −0.001 (3) | 0.001 (2) |
C9 | 0.014 (3) | 0.011 (3) | 0.023 (3) | 0.002 (2) | 0.009 (3) | −0.002 (2) |
C10 | 0.003 (3) | 0.013 (3) | 0.009 (3) | 0.003 (2) | 0.000 (2) | 0.0017 (19) |
C11 | 0.021 (4) | 0.015 (3) | 0.019 (3) | −0.010 (3) | 0.006 (3) | −0.006 (2) |
C12 | 0.018 (4) | 0.043 (4) | 0.036 (4) | −0.011 (3) | 0.001 (3) | −0.022 (3) |
C13 | 0.014 (3) | 0.027 (3) | 0.013 (3) | −0.009 (3) | 0.007 (3) | 0.002 (2) |
C14 | 0.034 (4) | 0.025 (3) | 0.023 (4) | −0.010 (3) | 0.004 (3) | 0.008 (3) |
C15 | 0.019 (4) | 0.012 (3) | 0.012 (3) | −0.003 (2) | 0.003 (3) | 0.001 (2) |
C16 | 0.014 (3) | 0.016 (3) | 0.010 (3) | 0.001 (3) | 0.004 (2) | 0.000 (2) |
C17 | 0.009 (3) | 0.011 (3) | 0.019 (4) | −0.002 (2) | 0.001 (2) | −0.001 (2) |
C18 | 0.012 (3) | 0.019 (3) | 0.013 (3) | −0.005 (2) | −0.001 (2) | 0.001 (2) |
C19 | 0.010 (3) | 0.018 (4) | 0.013 (3) | −0.001 (2) | 0.002 (2) | −0.001 (2) |
C20 | 0.005 (3) | 0.009 (3) | 0.018 (3) | −0.002 (2) | 0.004 (2) | −0.0011 (19) |
C21 | 0.010 (3) | 0.035 (4) | 0.020 (3) | 0.002 (3) | 0.009 (3) | −0.004 (3) |
C22 | 0.005 (3) | 0.020 (3) | 0.018 (3) | 0.004 (2) | −0.001 (2) | −0.001 (2) |
C23 | 0.016 (3) | 0.028 (4) | 0.013 (3) | 0.002 (3) | 0.006 (3) | −0.009 (2) |
C24 | 0.003 (3) | 0.016 (3) | 0.005 (3) | 0.001 (2) | 0.002 (2) | 0.0007 (19) |
C25 | 0.009 (3) | 0.016 (3) | 0.006 (3) | 0.000 (2) | 0.001 (2) | 0.000 (2) |
C26 | 0.006 (3) | 0.021 (3) | 0.013 (3) | −0.001 (2) | 0.003 (2) | −0.003 (2) |
C27 | 0.010 (3) | 0.012 (3) | 0.008 (3) | −0.001 (2) | 0.000 (2) | 0.0018 (19) |
C28 | 0.014 (3) | 0.016 (3) | 0.026 (3) | 0.006 (3) | 0.002 (3) | 0.004 (2) |
N1 | 0.011 (3) | 0.013 (2) | 0.014 (3) | −0.001 (2) | 0.002 (2) | −0.0009 (18) |
N2 | 0.002 (2) | 0.010 (2) | 0.010 (2) | 0.0019 (18) | −0.0006 (18) | 0.0018 (17) |
O1 | 0.007 (2) | 0.023 (2) | 0.026 (2) | −0.0008 (17) | 0.0086 (19) | −0.0048 (17) |
O2 | 0.015 (2) | 0.015 (2) | 0.026 (2) | −0.0038 (18) | −0.0019 (19) | 0.0014 (16) |
O3 | 0.031 (3) | 0.024 (2) | 0.016 (2) | 0.004 (2) | −0.004 (2) | 0.0016 (16) |
O4 | 0.009 (3) | 0.023 (2) | 0.037 (3) | 0.0001 (18) | 0.003 (2) | −0.0070 (18) |
O5 | 0.031 (3) | 0.016 (3) | 0.024 (2) | 0.006 (2) | 0.000 (2) | −0.0015 (17) |
O6 | 0.030 (3) | 0.028 (3) | 0.013 (3) | 0.004 (2) | 0.005 (2) | −0.0014 (16) |
O7 | 0.034 (3) | 0.021 (2) | 0.033 (3) | 0.009 (2) | 0.003 (2) | 0.0124 (19) |
O8 | 0.023 (3) | 0.025 (2) | 0.025 (3) | 0.005 (2) | 0.005 (2) | −0.0083 (19) |
O9 | 0.011 (3) | 0.020 (2) | 0.048 (3) | −0.0027 (19) | 0.007 (2) | −0.0078 (19) |
O10 | 0.014 (3) | 0.030 (3) | 0.032 (3) | 0.012 (2) | 0.002 (2) | 0.0064 (19) |
O11 | 0.029 (3) | 0.025 (3) | 0.029 (3) | −0.014 (2) | 0.011 (2) | −0.0058 (19) |
O12 | 0.018 (2) | 0.029 (2) | 0.011 (2) | −0.0049 (19) | 0.0059 (18) | −0.0027 (16) |
O13 | 0.007 (2) | 0.033 (3) | 0.021 (2) | 0.0027 (19) | 0.0058 (18) | −0.0011 (18) |
O14 | 0.031 (3) | 0.015 (2) | 0.019 (2) | −0.005 (2) | 0.009 (2) | 0.0007 (16) |
O15 | 0.016 (2) | 0.030 (3) | 0.012 (2) | −0.0070 (19) | −0.0031 (19) | 0.0006 (16) |
O16 | 0.016 (3) | 0.042 (3) | 0.026 (3) | 0.000 (2) | −0.005 (2) | −0.020 (2) |
O17 | 0.020 (3) | 0.041 (3) | 0.024 (3) | 0.002 (2) | 0.015 (2) | 0.0022 (19) |
O18 | 0.027 (3) | 0.030 (3) | 0.026 (3) | 0.019 (2) | 0.003 (2) | −0.0001 (19) |
Os1—C3 | 1.892 (6) | C5—O5 | 1.127 (8) |
Os1—C1 | 1.919 (7) | C6—O6 | 1.138 (8) |
Os1—C2 | 1.927 (6) | C7—O7 | 1.152 (8) |
Os1—S2 | 2.4318 (13) | C8—O8 | 1.140 (8) |
Os1—Os2 | 2.8171 (3) | C9—O9 | 1.152 (8) |
Os1—Os3 | 2.8519 (3) | C10—N1 | 1.316 (7) |
Os1—H1 | 1.98 (8) | C11—N1 | 1.486 (7) |
Os2—C6 | 1.902 (7) | C11—C12 | 1.520 (10) |
Os2—C4 | 1.917 (6) | C11—H11A | 0.9900 |
Os2—C5 | 1.932 (6) | C11—H11B | 0.9900 |
Os2—S1 | 2.4461 (14) | C12—H12A | 0.9800 |
Os2—Os3 | 2.7993 (3) | C12—H12B | 0.9800 |
Os3—C7 | 1.888 (6) | C12—H12C | 0.9800 |
Os3—C8 | 1.900 (7) | C13—N1 | 1.488 (8) |
Os3—C9 | 1.922 (6) | C13—C14 | 1.516 (9) |
Os3—S2 | 2.4218 (14) | C13—H13A | 0.9900 |
Os3—H1 | 1.90 (8) | C13—H13B | 0.9900 |
Os4—C17 | 1.894 (6) | C14—H14A | 0.9800 |
Os4—C16 | 1.907 (6) | C14—H14B | 0.9800 |
Os4—C15 | 1.917 (6) | C14—H14C | 0.9800 |
Os4—S3 | 2.4548 (13) | C15—O10 | 1.149 (8) |
Os4—Os5 | 2.8110 (3) | C16—O11 | 1.158 (7) |
Os4—Os6 | 2.8203 (3) | C17—O12 | 1.147 (7) |
Os5—C20 | 1.891 (6) | C18—O13 | 1.147 (8) |
Os5—C18 | 1.900 (6) | C19—O14 | 1.135 (7) |
Os5—C19 | 1.936 (6) | C20—O15 | 1.149 (7) |
Os5—H2 | 2.10 (11) | C21—O16 | 1.146 (8) |
Os5—S4 | 2.4276 (13) | C22—O17 | 1.136 (8) |
Os5—Os6 | 2.8519 (3) | C23—O18 | 1.161 (8) |
Os5—H2 | 2.10 (11) | C24—N2 | 1.311 (7) |
Os6—C21 | 1.901 (7) | C25—N2 | 1.486 (7) |
Os6—C22 | 1.911 (6) | C25—C26 | 1.514 (8) |
Os6—C23 | 1.922 (7) | C25—H25A | 0.9900 |
Os6—H2 | 1.93 (11) | C25—H25B | 0.9900 |
Os6—S4 | 2.4353 (14) | C26—H26A | 0.9800 |
Os6—H2 | 1.93 (11) | C26—H26B | 0.9800 |
S1—C10 | 1.689 (6) | C26—H26C | 0.9800 |
S2—C10 | 1.796 (6) | C27—N2 | 1.476 (7) |
S3—C24 | 1.694 (5) | C27—C28 | 1.523 (8) |
S4—C24 | 1.801 (5) | C27—H27A | 0.9900 |
C1—O1 | 1.130 (8) | C27—H27B | 0.9900 |
C2—O2 | 1.135 (7) | C28—H28A | 0.9800 |
C3—O3 | 1.147 (7) | C28—H28B | 0.9800 |
C4—O4 | 1.147 (7) | C28—H28C | 0.9800 |
C3—Os1—C1 | 92.7 (2) | C22—Os6—S4 | 167.46 (18) |
C3—Os1—C2 | 96.5 (2) | C23—Os6—S4 | 89.90 (19) |
C1—Os1—C2 | 100.0 (2) | H2—Os6—S4 | 83 (3) |
C3—Os1—S2 | 169.83 (18) | C21—Os6—Os4 | 83.9 (2) |
C1—Os1—S2 | 94.70 (17) | C22—Os6—Os4 | 91.20 (17) |
C2—Os1—S2 | 89.06 (17) | C23—Os6—Os4 | 171.74 (19) |
C3—Os1—Os2 | 89.28 (17) | H2—Os6—Os4 | 97 (3) |
C1—Os1—Os2 | 86.12 (17) | S4—Os6—Os4 | 83.50 (3) |
C2—Os1—Os2 | 171.31 (17) | C21—Os6—Os5 | 133.30 (18) |
S2—Os1—Os2 | 84.31 (3) | C22—Os6—Os5 | 113.62 (17) |
C3—Os1—Os3 | 116.00 (17) | C23—Os6—Os5 | 112.58 (19) |
C1—Os1—Os3 | 132.51 (17) | H2—Os6—Os5 | 48 (3) |
C2—Os1—Os3 | 112.27 (17) | S4—Os6—Os5 | 53.97 (3) |
S2—Os1—Os3 | 53.85 (3) | Os4—Os6—Os5 | 59.411 (8) |
Os2—Os1—Os3 | 59.176 (8) | C21—Os6—H2 | 179 (3) |
C3—Os1—H1 | 89 (2) | C22—Os6—H2 | 86 (3) |
C1—Os1—H1 | 173 (2) | C23—Os6—H2 | 77 (3) |
C2—Os1—H1 | 86 (2) | H2—Os6—H2 | 0 (7) |
S2—Os1—H1 | 83 (2) | S4—Os6—H2 | 83 (3) |
Os2—Os1—H1 | 87 (2) | Os4—Os6—H2 | 97 (3) |
Os3—Os1—H1 | 42 (2) | Os5—Os6—H2 | 48 (3) |
C6—Os2—C4 | 91.8 (3) | C10—S1—Os2 | 109.5 (2) |
C6—Os2—C5 | 91.0 (2) | C10—S2—Os3 | 110.90 (18) |
C4—Os2—C5 | 98.8 (2) | C10—S2—Os1 | 104.06 (18) |
C6—Os2—S1 | 178.09 (17) | Os3—S2—Os1 | 71.97 (4) |
C4—Os2—S1 | 88.22 (17) | C24—S3—Os4 | 109.49 (19) |
C5—Os2—S1 | 90.85 (17) | C24—S4—Os5 | 110.11 (17) |
C6—Os2—Os3 | 89.95 (18) | C24—S4—Os6 | 107.99 (18) |
C4—Os2—Os3 | 162.02 (16) | Os5—S4—Os6 | 71.81 (4) |
C5—Os2—Os3 | 99.09 (17) | O1—C1—Os1 | 177.6 (5) |
S1—Os2—Os3 | 89.43 (3) | O2—C2—Os1 | 177.6 (5) |
C6—Os2—Os1 | 88.32 (17) | O3—C3—Os1 | 179.4 (5) |
C4—Os2—Os1 | 101.13 (16) | O4—C4—Os2 | 178.6 (5) |
C5—Os2—Os1 | 160.10 (17) | O5—C5—Os2 | 175.5 (5) |
S1—Os2—Os1 | 89.79 (3) | O6—C6—Os2 | 178.6 (5) |
Os3—Os2—Os1 | 61.032 (8) | O7—C7—Os3 | 178.1 (6) |
C7—Os3—C8 | 91.7 (3) | O8—C8—Os3 | 177.8 (6) |
C7—Os3—C9 | 99.0 (3) | O9—C9—Os3 | 174.9 (5) |
C8—Os3—C9 | 93.8 (3) | N1—C10—S1 | 122.6 (4) |
C7—Os3—S2 | 95.9 (2) | N1—C10—S2 | 116.7 (4) |
C8—Os3—S2 | 169.53 (19) | S1—C10—S2 | 120.7 (3) |
C9—Os3—S2 | 92.18 (18) | N1—C11—C12 | 111.9 (5) |
C7—Os3—Os2 | 89.60 (19) | N1—C11—H11A | 109.2 |
C8—Os3—Os2 | 87.93 (19) | C12—C11—H11A | 109.2 |
C9—Os3—Os2 | 171.14 (18) | N1—C11—H11B | 109.2 |
S2—Os3—Os2 | 84.87 (3) | C12—C11—H11B | 109.2 |
C7—Os3—Os1 | 136.2 (2) | H11A—C11—H11B | 107.9 |
C8—Os3—Os1 | 115.47 (18) | C11—C12—H12A | 109.5 |
C9—Os3—Os1 | 111.83 (17) | C11—C12—H12B | 109.5 |
S2—Os3—Os1 | 54.18 (3) | H12A—C12—H12B | 109.5 |
Os2—Os3—Os1 | 59.792 (8) | C11—C12—H12C | 109.5 |
C7—Os3—H1 | 179 (3) | H12A—C12—H12C | 109.5 |
C8—Os3—H1 | 87 (2) | H12B—C12—H12C | 109.5 |
C9—Os3—H1 | 82 (3) | N1—C13—C14 | 113.1 (5) |
S2—Os3—H1 | 85 (2) | N1—C13—H13A | 109.0 |
Os2—Os3—H1 | 90 (3) | C14—C13—H13A | 109.0 |
Os1—Os3—H1 | 44 (2) | N1—C13—H13B | 109.0 |
C17—Os4—C16 | 92.4 (2) | C14—C13—H13B | 109.0 |
C17—Os4—C15 | 92.4 (2) | H13A—C13—H13B | 107.8 |
C16—Os4—C15 | 99.6 (2) | C13—C14—H14A | 109.5 |
C17—Os4—S3 | 179.21 (18) | C13—C14—H14B | 109.5 |
C16—Os4—S3 | 88.35 (17) | H14A—C14—H14B | 109.5 |
C15—Os4—S3 | 87.68 (18) | C13—C14—H14C | 109.5 |
C17—Os4—Os5 | 88.66 (17) | H14A—C14—H14C | 109.5 |
C16—Os4—Os5 | 160.85 (18) | H14B—C14—H14C | 109.5 |
C15—Os4—Os5 | 99.48 (17) | O10—C15—Os4 | 178.7 (5) |
S3—Os4—Os5 | 90.54 (3) | O11—C16—Os4 | 179.4 (6) |
C17—Os4—Os6 | 89.07 (18) | O12—C17—Os4 | 178.3 (5) |
C16—Os4—Os6 | 100.03 (18) | O13—C18—Os5 | 178.2 (5) |
C15—Os4—Os6 | 160.26 (17) | O14—C19—Os5 | 176.6 (5) |
S3—Os4—Os6 | 90.58 (3) | O15—C20—Os5 | 177.3 (5) |
Os5—Os4—Os6 | 60.855 (8) | O16—C21—Os6 | 179.4 (6) |
C20—Os5—C18 | 90.3 (2) | O17—C22—Os6 | 179.1 (6) |
C20—Os5—C19 | 93.1 (2) | O18—C23—Os6 | 177.5 (6) |
C18—Os5—C19 | 102.6 (2) | N2—C24—S3 | 123.5 (4) |
C20—Os5—H2 | 90 (3) | N2—C24—S4 | 116.0 (4) |
C18—Os5—H2 | 177 (3) | S3—C24—S4 | 120.5 (3) |
C19—Os5—H2 | 81 (3) | N2—C25—C26 | 110.6 (5) |
C20—Os5—S4 | 169.01 (17) | N2—C25—H25A | 109.5 |
C18—Os5—S4 | 99.46 (18) | C26—C25—H25A | 109.5 |
C19—Os5—S4 | 89.64 (17) | N2—C25—H25B | 109.5 |
H2—Os5—S4 | 80 (3) | C26—C25—H25B | 109.5 |
C20—Os5—Os4 | 92.36 (16) | H25A—C25—H25B | 108.1 |
C18—Os5—Os4 | 83.70 (17) | C25—C26—H26A | 109.5 |
C19—Os5—Os4 | 171.62 (17) | C25—C26—H26B | 109.5 |
H2—Os5—Os4 | 93 (3) | H26A—C26—H26B | 109.5 |
S4—Os5—Os4 | 83.84 (3) | C25—C26—H26C | 109.5 |
C20—Os5—Os6 | 115.05 (17) | H26A—C26—H26C | 109.5 |
C18—Os5—Os6 | 134.70 (17) | H26B—C26—H26C | 109.5 |
C19—Os5—Os6 | 112.07 (17) | N2—C27—C28 | 112.2 (5) |
H2—Os5—Os6 | 42 (3) | N2—C27—H27A | 109.2 |
S4—Os5—Os6 | 54.22 (3) | C28—C27—H27A | 109.2 |
Os4—Os5—Os6 | 59.734 (8) | N2—C27—H27B | 109.2 |
C20—Os5—H2 | 90 (3) | C28—C27—H27B | 109.2 |
C18—Os5—H2 | 177 (3) | H27A—C27—H27B | 107.9 |
C19—Os5—H2 | 81 (3) | C27—C28—H28A | 109.5 |
H2—Os5—H2 | 0 (5) | C27—C28—H28B | 109.5 |
S4—Os5—H2 | 80 (3) | H28A—C28—H28B | 109.5 |
Os4—Os5—H2 | 93 (3) | C27—C28—H28C | 109.5 |
Os6—Os5—H2 | 42 (3) | H28A—C28—H28C | 109.5 |
C21—Os6—C22 | 93.4 (3) | H28B—C28—H28C | 109.5 |
C21—Os6—C23 | 101.9 (3) | C10—N1—C11 | 125.0 (5) |
C22—Os6—C23 | 94.3 (3) | C10—N1—C13 | 119.5 (5) |
C21—Os6—H2 | 179 (3) | C11—N1—C13 | 115.6 (5) |
C22—Os6—H2 | 86 (3) | C24—N2—C27 | 124.8 (5) |
C23—Os6—H2 | 77 (3) | C24—N2—C25 | 120.8 (4) |
C21—Os6—S4 | 97.32 (19) | C27—N2—C25 | 114.4 (4) |
C3—Os1—Os2—C6 | −30.3 (3) | C20—Os5—Os6—C21 | −120.8 (3) |
C1—Os1—Os2—C6 | −123.1 (2) | C18—Os5—Os6—C21 | −2.6 (4) |
S2—Os1—Os2—C6 | 141.76 (19) | C19—Os5—Os6—C21 | 134.5 (3) |
Os3—Os1—Os2—C6 | 90.87 (18) | H2—Os5—Os6—C21 | 180 (4) |
C3—Os1—Os2—C4 | 61.2 (3) | S4—Os5—Os6—C21 | 62.0 (3) |
C1—Os1—Os2—C4 | −31.6 (2) | Os4—Os5—Os6—C21 | −43.5 (3) |
S2—Os1—Os2—C4 | −126.71 (18) | C20—Os5—Os6—C22 | −0.7 (3) |
Os3—Os1—Os2—C4 | −177.61 (17) | C18—Os5—Os6—C22 | 117.4 (3) |
C3—Os1—Os2—C5 | −118.7 (5) | C19—Os5—Os6—C22 | −105.4 (3) |
C1—Os1—Os2—C5 | 148.5 (5) | H2—Os5—Os6—C22 | −60 (4) |
S2—Os1—Os2—C5 | 53.4 (5) | S4—Os5—Os6—C22 | −177.9 (2) |
Os3—Os1—Os2—C5 | 2.5 (5) | Os4—Os5—Os6—C22 | 76.58 (19) |
C3—Os1—Os2—S1 | 149.34 (18) | C20—Os5—Os6—C23 | 104.9 (3) |
C1—Os1—Os2—S1 | 56.55 (17) | C18—Os5—Os6—C23 | −136.9 (3) |
S2—Os1—Os2—S1 | −38.57 (5) | C19—Os5—Os6—C23 | 0.3 (3) |
Os3—Os1—Os2—S1 | −89.46 (4) | H2—Os5—Os6—C23 | 46 (4) |
C3—Os1—Os2—Os3 | −121.20 (18) | S4—Os5—Os6—C23 | −72.26 (19) |
C1—Os1—Os2—Os3 | 146.01 (17) | Os4—Os5—Os6—C23 | −177.77 (19) |
S2—Os1—Os2—Os3 | 50.89 (3) | C20—Os5—Os6—H2 | 59 (4) |
C6—Os2—Os3—C7 | 124.9 (3) | C18—Os5—Os6—H2 | 178 (4) |
C4—Os2—Os3—C7 | −139.4 (6) | C19—Os5—Os6—H2 | −45 (4) |
C5—Os2—Os3—C7 | 33.8 (3) | S4—Os5—Os6—H2 | −118 (4) |
S1—Os2—Os3—C7 | −57.0 (2) | Os4—Os5—Os6—H2 | 137 (4) |
Os1—Os2—Os3—C7 | −147.0 (2) | C20—Os5—Os6—S4 | 177.20 (18) |
C6—Os2—Os3—C8 | 33.2 (2) | C18—Os5—Os6—S4 | −64.7 (2) |
C4—Os2—Os3—C8 | 128.9 (6) | C19—Os5—Os6—S4 | 72.51 (19) |
C5—Os2—Os3—C8 | −57.9 (2) | H2—Os5—Os6—S4 | 118 (4) |
S1—Os2—Os3—C8 | −148.65 (18) | Os4—Os5—Os6—S4 | −105.52 (4) |
Os1—Os2—Os3—C8 | 121.27 (18) | C20—Os5—Os6—Os4 | −77.28 (18) |
C6—Os2—Os3—S2 | −139.23 (17) | C18—Os5—Os6—Os4 | 40.9 (2) |
C4—Os2—Os3—S2 | −43.5 (6) | C19—Os5—Os6—Os4 | 178.03 (18) |
C5—Os2—Os3—S2 | 129.73 (17) | H2—Os5—Os6—Os4 | −137 (4) |
S1—Os2—Os3—S2 | 38.97 (5) | S4—Os5—Os6—Os4 | 105.52 (4) |
Os1—Os2—Os3—S2 | −51.12 (3) | C4—Os2—S1—C10 | 124.8 (3) |
C6—Os2—Os3—Os1 | −88.11 (17) | C5—Os2—S1—C10 | −136.5 (3) |
C4—Os2—Os3—Os1 | 7.6 (6) | Os3—Os2—S1—C10 | −37.4 (2) |
C5—Os2—Os3—Os1 | −179.15 (16) | Os1—Os2—S1—C10 | 23.6 (2) |
S1—Os2—Os3—Os1 | 90.08 (3) | C7—Os3—S2—C10 | 46.6 (3) |
C3—Os1—Os3—C7 | 123.9 (3) | C8—Os3—S2—C10 | −89.3 (10) |
C1—Os1—Os3—C7 | 2.6 (4) | C9—Os3—S2—C10 | 145.9 (3) |
C2—Os1—Os3—C7 | −126.5 (3) | Os2—Os3—S2—C10 | −42.51 (18) |
S2—Os1—Os3—C7 | −55.2 (3) | Os1—Os3—S2—C10 | −98.58 (19) |
Os2—Os1—Os3—C7 | 51.8 (3) | C7—Os3—S2—Os1 | 145.13 (19) |
C3—Os1—Os3—C8 | 1.0 (3) | C8—Os3—S2—Os1 | 9.3 (10) |
C1—Os1—Os3—C8 | −120.3 (3) | C9—Os3—S2—Os1 | −115.57 (18) |
C2—Os1—Os3—C8 | 110.6 (3) | Os2—Os3—S2—Os1 | 56.06 (2) |
S2—Os1—Os3—C8 | −178.1 (2) | C3—Os1—S2—C10 | 103.3 (10) |
Os2—Os1—Os3—C8 | −71.1 (2) | C1—Os1—S2—C10 | −33.5 (3) |
C3—Os1—Os3—C9 | −104.7 (3) | C2—Os1—S2—C10 | −133.5 (2) |
C1—Os1—Os3—C9 | 134.0 (3) | Os2—Os1—S2—C10 | 52.16 (18) |
C2—Os1—Os3—C9 | 4.9 (3) | Os3—Os1—S2—C10 | 107.77 (19) |
S2—Os1—Os3—C9 | 76.2 (2) | C3—Os1—S2—Os3 | −4.4 (10) |
Os2—Os1—Os3—C9 | −176.79 (19) | C1—Os1—S2—Os3 | −141.23 (17) |
C3—Os1—Os3—S2 | 179.1 (2) | C2—Os1—S2—Os3 | 118.77 (17) |
C1—Os1—Os3—S2 | 57.9 (2) | Os2—Os1—S2—Os3 | −55.61 (2) |
C2—Os1—Os3—S2 | −71.27 (18) | C16—Os4—S3—C24 | 128.6 (3) |
Os2—Os1—Os3—S2 | 107.02 (4) | C15—Os4—S3—C24 | −131.8 (3) |
C3—Os1—Os3—Os2 | 72.1 (2) | Os5—Os4—S3—C24 | −32.3 (2) |
C1—Os1—Os3—Os2 | −49.2 (2) | Os6—Os4—S3—C24 | 28.6 (2) |
C2—Os1—Os3—Os2 | −178.30 (18) | C20—Os5—S4—C24 | −116.5 (9) |
S2—Os1—Os3—Os2 | −107.02 (4) | C18—Os5—S4—C24 | 36.3 (3) |
C17—Os4—Os5—C20 | 28.1 (2) | C19—Os5—S4—C24 | 139.1 (3) |
C16—Os4—Os5—C20 | 121.6 (5) | H2—Os5—S4—C24 | −140 (3) |
C15—Os4—Os5—C20 | −64.1 (2) | Os4—Os5—S4—C24 | −46.22 (19) |
S3—Os4—Os5—C20 | −151.83 (17) | Os6—Os5—S4—C24 | −103.05 (19) |
Os6—Os4—Os5—C20 | 117.82 (17) | C20—Os5—S4—Os6 | −13.4 (9) |
C17—Os4—Os5—C18 | 118.2 (2) | C18—Os5—S4—Os6 | 139.37 (18) |
C16—Os4—Os5—C18 | −148.3 (5) | C19—Os5—S4—Os6 | −117.88 (18) |
C15—Os4—Os5—C18 | 26.0 (3) | H2—Os5—S4—Os6 | −37 (3) |
S3—Os4—Os5—C18 | −61.75 (18) | Os4—Os5—S4—Os6 | 56.83 (2) |
Os6—Os4—Os5—C18 | −152.10 (18) | C21—Os6—S4—C24 | −33.7 (3) |
C17—Os4—Os5—H2 | −62 (3) | C22—Os6—S4—C24 | 114.8 (8) |
C16—Os4—Os5—H2 | 31 (3) | C23—Os6—S4—C24 | −135.7 (3) |
C15—Os4—Os5—H2 | −154 (3) | H2—Os6—S4—C24 | 147 (3) |
S3—Os4—Os5—H2 | 118 (3) | Os4—Os6—S4—C24 | 49.30 (18) |
Os6—Os4—Os5—H2 | 28 (3) | Os5—Os6—S4—C24 | 105.90 (18) |
C17—Os4—Os5—S4 | −141.52 (18) | C21—Os6—S4—Os5 | −139.6 (2) |
C16—Os4—Os5—S4 | −48.0 (5) | C22—Os6—S4—Os5 | 8.9 (8) |
C15—Os4—Os5—S4 | 126.26 (18) | C23—Os6—S4—Os5 | 118.43 (18) |
S3—Os4—Os5—S4 | 38.52 (5) | H2—Os6—S4—Os5 | 41 (3) |
Os6—Os4—Os5—S4 | −51.83 (3) | Os4—Os6—S4—Os5 | −56.60 (2) |
C17—Os4—Os5—Os6 | −89.68 (18) | Os2—S1—C10—N1 | −166.6 (4) |
C16—Os4—Os5—Os6 | 3.8 (5) | Os2—S1—C10—S2 | 13.2 (4) |
C15—Os4—Os5—Os6 | 178.09 (18) | Os3—S2—C10—N1 | −154.9 (4) |
S3—Os4—Os5—Os6 | 90.36 (3) | Os1—S2—C10—N1 | 129.3 (4) |
C17—Os4—Os6—C21 | −121.3 (3) | Os3—S2—C10—S1 | 25.2 (4) |
C16—Os4—Os6—C21 | −29.0 (3) | Os1—S2—C10—S1 | −50.5 (3) |
C15—Os4—Os6—C21 | 144.2 (5) | Os4—S3—C24—N2 | −175.6 (4) |
S3—Os4—Os6—C21 | 59.5 (2) | Os4—S3—C24—S4 | 3.8 (4) |
Os5—Os4—Os6—C21 | 149.76 (19) | Os5—S4—C24—N2 | −146.0 (4) |
C17—Os4—Os6—C22 | −28.0 (3) | Os6—S4—C24—N2 | 137.3 (4) |
C16—Os4—Os6—C22 | 64.3 (2) | Os5—S4—C24—S3 | 34.6 (4) |
C15—Os4—Os6—C22 | −122.5 (5) | Os6—S4—C24—S3 | −42.1 (4) |
S3—Os4—Os6—C22 | 152.75 (18) | S1—C10—N1—C11 | −179.3 (4) |
Os5—Os4—Os6—C22 | −116.95 (18) | S2—C10—N1—C11 | 0.8 (7) |
C17—Os4—Os6—H2 | 58 (3) | S1—C10—N1—C13 | 0.7 (7) |
C16—Os4—Os6—H2 | 151 (3) | S2—C10—N1—C13 | −179.1 (4) |
C15—Os4—Os6—H2 | −36 (3) | C12—C11—N1—C10 | 103.5 (7) |
S3—Os4—Os6—H2 | −121 (3) | C12—C11—N1—C13 | −76.6 (7) |
Os5—Os4—Os6—H2 | −31 (3) | C14—C13—N1—C10 | −78.4 (7) |
C17—Os4—Os6—S4 | 140.64 (18) | C14—C13—N1—C11 | 101.7 (6) |
C16—Os4—Os6—S4 | −127.08 (17) | S3—C24—N2—C27 | −176.2 (4) |
C15—Os4—Os6—S4 | 46.1 (5) | S4—C24—N2—C27 | 4.4 (7) |
S3—Os4—Os6—S4 | −38.65 (5) | S3—C24—N2—C25 | 2.0 (7) |
Os5—Os4—Os6—S4 | 51.65 (3) | S4—C24—N2—C25 | −177.4 (4) |
C17—Os4—Os6—Os5 | 88.99 (17) | C28—C27—N2—C24 | −90.2 (6) |
C16—Os4—Os6—Os5 | −178.73 (17) | C28—C27—N2—C25 | 91.5 (6) |
C15—Os4—Os6—Os5 | −5.6 (5) | C26—C25—N2—C24 | −92.8 (6) |
S3—Os4—Os6—Os5 | −90.30 (3) | C26—C25—N2—C27 | 85.6 (5) |
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