Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804001047/hg6017sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536804001047/hg6017Isup2.hkl |
CCDC reference: 234819
Key indicators
- Single-crystal X-ray study
- T = 120 K
- Mean (S-C) = 0.003 Å
- R factor = 0.029
- wR factor = 0.064
- Data-to-parameter ratio = 27.2
checkCIF/PLATON results
No syntax errors found
Alert level C PLAT061_ALERT_3_C Tmax/Tmin Range Test RR' too Large ............. 0.89
Alert level G REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is correct. If it is not, please give the correct count in the _publ_section_exptl_refinement section of the submitted CIF. From the CIF: _diffrn_reflns_theta_max 27.49 From the CIF: _reflns_number_total 3263 Count of symmetry unique reflns 1772 Completeness (_total/calc) 184.14% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 1491 Fraction of Friedel pairs measured 0.841 Are heavy atom types Z>Si present yes
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 1 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 0 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 1 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997); cell refinement: COLLECT and DENZO; data reduction: COLLECT and DENZO; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976).
[RuCl3(C2H6S)3] | F(000) = 788 |
Mr = 393.80 | Dx = 1.783 Mg m−3 |
Orthorhombic, Pna21 | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: P 2c -2n | Cell parameters from 5262 reflections |
a = 16.391 (2) Å | θ = 2.9–27.5° |
b = 8.540 (1) Å | µ = 2.00 mm−1 |
c = 10.4825 (10) Å | T = 120 K |
V = 1467.3 (3) Å3 | Block, red |
Z = 4 | 0.18 × 0.18 × 0.10 mm |
Nonius KappaCCD area-detector diffractometer | 3263 independent reflections |
Radiation source: Nonius rotating anode | 2912 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.058 |
φ and ω scans | θmax = 27.5°, θmin = 3.1° |
Absorption correction: multi-scan SORTAV, R H Blessing, J. Appl. Cryst., 1997, 30, 421-426. | h = −21→21 |
Tmin = 0.629, Tmax = 0.818 | k = −11→10 |
11276 measured reflections | l = −12→13 |
Refinement on F2 | Hydrogen site location: inferred from neighbouring sites |
Least-squares matrix: full | H-atom parameters constrained |
R[F2 > 2σ(F2)] = 0.029 | w = 1/[σ2(Fo2) + (0.0171P)2 + 0.0078P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.064 | (Δ/σ)max = 0.001 |
S = 1.04 | Δρmax = 0.79 e Å−3 |
3263 reflections | Δρmin = −0.65 e Å−3 |
120 parameters | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
1 restraint | Extinction coefficient: 0.0045 (3) |
Primary atom site location: structure-invariant direct methods | Absolute structure: Flack (1983), 0000 Friedel pairs |
Secondary atom site location: difference Fourier map | Absolute structure parameter: −0.04 (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. The H atoms are in calculated positions with a common refined isotropic adp. |
x | y | z | Uiso*/Ueq | ||
Ru1 | 0.138500 (16) | 0.74481 (2) | 0.33416 (3) | 0.01249 (9) | |
Cl1 | 0.25315 (6) | 0.77875 (10) | 0.20423 (9) | 0.0224 (2) | |
Cl2 | 0.02346 (5) | 0.74323 (9) | 0.46717 (9) | 0.0186 (2) | |
Cl3 | 0.14814 (5) | 0.46959 (8) | 0.33899 (11) | 0.02330 (19) | |
S1 | 0.05396 (6) | 0.72744 (10) | 0.14917 (10) | 0.0198 (2) | |
S2 | 0.23383 (6) | 0.77039 (11) | 0.50511 (10) | 0.0205 (2) | |
S3 | 0.12723 (4) | 1.02262 (8) | 0.32995 (11) | 0.01613 (17) | |
C1 | −0.0287 (2) | 0.5952 (4) | 0.1815 (3) | 0.0269 (8) | |
H1A | −0.0648 | 0.6412 | 0.2460 | 0.043 (3)* | |
H1B | −0.0068 | 0.4958 | 0.2133 | 0.043 (3)* | |
H1C | −0.0596 | 0.5765 | 0.1029 | 0.043 (3)* | |
C2 | 0.1072 (2) | 0.6144 (5) | 0.0318 (4) | 0.0329 (10) | |
H2A | 0.1554 | 0.6723 | 0.0029 | 0.043 (3)* | |
H2B | 0.0711 | 0.5945 | −0.0409 | 0.043 (3)* | |
H2C | 0.1243 | 0.5145 | 0.0693 | 0.043 (3)* | |
C3 | 0.3097 (2) | 0.6181 (4) | 0.4915 (4) | 0.0321 (10) | |
H3A | 0.3400 | 0.6314 | 0.4117 | 0.043 (3)* | |
H3B | 0.2829 | 0.5156 | 0.4918 | 0.043 (3)* | |
H3C | 0.3475 | 0.6247 | 0.5638 | 0.043 (3)* | |
C4 | 0.1894 (2) | 0.7178 (4) | 0.6556 (3) | 0.0284 (9) | |
H4A | 0.1460 | 0.7922 | 0.6770 | 0.043 (3)* | |
H4B | 0.2315 | 0.7205 | 0.7220 | 0.043 (3)* | |
H4C | 0.1665 | 0.6120 | 0.6500 | 0.043 (3)* | |
C5 | 0.1292 (2) | 1.0949 (4) | 0.4900 (3) | 0.0276 (9) | |
H5A | 0.1824 | 1.0721 | 0.5284 | 0.043 (3)* | |
H5B | 0.0862 | 1.0438 | 0.5398 | 0.043 (3)* | |
H5C | 0.1201 | 1.2083 | 0.4894 | 0.043 (3)* | |
C6 | 0.0248 (2) | 1.0823 (4) | 0.2899 (4) | 0.0275 (8) | |
H6A | 0.0125 | 1.0513 | 0.2020 | 0.043 (3)* | |
H6B | 0.0201 | 1.1962 | 0.2980 | 0.043 (3)* | |
H6C | −0.0139 | 1.0317 | 0.3481 | 0.043 (3)* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ru1 | 0.01246 (14) | 0.01152 (15) | 0.01350 (14) | −0.00008 (8) | 0.00046 (14) | 0.00110 (12) |
Cl1 | 0.0191 (5) | 0.0259 (5) | 0.0222 (5) | 0.0018 (4) | 0.0088 (4) | 0.0028 (5) |
Cl2 | 0.0157 (5) | 0.0206 (5) | 0.0195 (5) | −0.0018 (3) | 0.0050 (4) | 0.0028 (3) |
Cl3 | 0.0264 (4) | 0.0114 (4) | 0.0321 (5) | 0.0013 (3) | −0.0004 (5) | 0.0020 (5) |
S1 | 0.0233 (5) | 0.0179 (4) | 0.0181 (4) | −0.0002 (3) | −0.0061 (4) | −0.0028 (4) |
S2 | 0.0180 (5) | 0.0218 (5) | 0.0216 (5) | −0.0031 (4) | −0.0060 (4) | 0.0060 (4) |
S3 | 0.0215 (4) | 0.0115 (4) | 0.0154 (4) | −0.0005 (3) | 0.0022 (5) | 0.0013 (5) |
C1 | 0.0217 (18) | 0.026 (2) | 0.033 (2) | −0.0032 (15) | −0.0036 (17) | −0.0058 (15) |
C2 | 0.036 (2) | 0.039 (3) | 0.024 (2) | 0.0018 (17) | 0.0032 (17) | −0.0141 (17) |
C3 | 0.0198 (19) | 0.043 (3) | 0.033 (2) | 0.0051 (17) | −0.0004 (17) | 0.0110 (17) |
C4 | 0.028 (2) | 0.037 (2) | 0.0200 (18) | 0.0023 (17) | −0.0049 (17) | 0.0044 (17) |
C5 | 0.043 (2) | 0.018 (2) | 0.022 (2) | −0.0004 (17) | −0.0059 (17) | −0.0062 (14) |
C6 | 0.029 (2) | 0.0217 (18) | 0.032 (2) | 0.0082 (15) | −0.0097 (16) | −0.0001 (15) |
Ru1—Cl1 | 2.3389 (10) | C2—H2A | 0.9800 |
Ru1—Cl2 | 2.3451 (9) | C2—H2B | 0.9800 |
Ru1—Cl3 | 2.3562 (8) | C2—H2C | 0.9800 |
Ru1—S1 | 2.3879 (10) | C3—H3A | 0.9800 |
Ru1—S2 | 2.3876 (11) | C3—H3B | 0.9800 |
Ru1—S3 | 2.3801 (8) | C3—H3C | 0.9800 |
S1—C1 | 1.796 (3) | C4—H4A | 0.9800 |
S1—C2 | 1.791 (4) | C4—H4B | 0.9800 |
S2—C4 | 1.795 (4) | C4—H4C | 0.9800 |
S2—C3 | 1.806 (4) | C5—H5A | 0.9800 |
S3—C5 | 1.787 (4) | C5—H5B | 0.9800 |
S3—C6 | 1.805 (3) | C5—H5C | 0.9800 |
C1—H1A | 0.9800 | C6—H6A | 0.9800 |
C1—H1B | 0.9800 | C6—H6B | 0.9800 |
C1—H1C | 0.9800 | C6—H6C | 0.9800 |
Cl1—Ru1—Cl2 | 173.19 (3) | S1—C2—H2A | 109.5 |
Cl1—Ru1—Cl3 | 94.72 (3) | S1—C2—H2B | 109.5 |
Cl2—Ru1—Cl3 | 92.03 (3) | H2A—C2—H2B | 109.5 |
Cl1—Ru1—S3 | 85.87 (3) | S1—C2—H2C | 109.5 |
Cl2—Ru1—S3 | 87.39 (3) | H2A—C2—H2C | 109.5 |
Cl3—Ru1—S3 | 179.37 (3) | H2B—C2—H2C | 109.5 |
Cl1—Ru1—S2 | 84.26 (4) | S2—C3—H3A | 109.5 |
Cl2—Ru1—S2 | 94.62 (4) | S2—C3—H3B | 109.5 |
Cl3—Ru1—S2 | 91.79 (3) | H3A—C3—H3B | 109.5 |
S3—Ru1—S2 | 88.48 (3) | S2—C3—H3C | 109.5 |
Cl1—Ru1—S1 | 90.06 (4) | H3A—C3—H3C | 109.5 |
Cl2—Ru1—S1 | 90.91 (4) | H3B—C3—H3C | 109.5 |
Cl3—Ru1—S1 | 89.68 (3) | S2—C4—H4A | 109.5 |
S3—Ru1—S1 | 90.10 (3) | S2—C4—H4B | 109.5 |
S2—Ru1—S1 | 174.22 (4) | H4A—C4—H4B | 109.5 |
C2—S1—C1 | 99.11 (17) | S2—C4—H4C | 109.5 |
C2—S1—Ru1 | 107.96 (13) | H4A—C4—H4C | 109.5 |
C1—S1—Ru1 | 108.87 (12) | H4B—C4—H4C | 109.5 |
C4—S2—C3 | 99.71 (17) | S3—C5—H5A | 109.5 |
C4—S2—Ru1 | 111.80 (13) | S3—C5—H5B | 109.5 |
C3—S2—Ru1 | 109.02 (13) | H5A—C5—H5B | 109.5 |
C5—S3—C6 | 97.90 (17) | S3—C5—H5C | 109.5 |
C5—S3—Ru1 | 108.98 (12) | H5A—C5—H5C | 109.5 |
C6—S3—Ru1 | 110.97 (11) | H5B—C5—H5C | 109.5 |
S1—C1—H1A | 109.5 | S3—C6—H6A | 109.5 |
S1—C1—H1B | 109.5 | S3—C6—H6B | 109.5 |
H1A—C1—H1B | 109.5 | H6A—C6—H6B | 109.5 |
S1—C1—H1C | 109.5 | S3—C6—H6C | 109.5 |
H1A—C1—H1C | 109.5 | H6A—C6—H6C | 109.5 |
H1B—C1—H1C | 109.5 | H6B—C6—H6C | 109.5 |
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