Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805014157/hb6194sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536805014157/hb6194Isup2.hkl |
CCDC reference: 274406
Key indicators
- Single-crystal X-ray study
- T = 173 K
- Mean (C-C) = 0.006 Å
- R factor = 0.023
- wR factor = 0.079
- Data-to-parameter ratio = 17.1
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT029_ALERT_3_B _diffrn_measured_fraction_theta_full Low ....... 0.94 PLAT213_ALERT_2_B Atom C5 has ADP max/min Ratio ............. 4.60 oblate
Alert level C PLAT022_ALERT_3_C Ratio Unique / Expected Reflections too Low .... 0.94 PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT061_ALERT_3_C Tmax/Tmin Range Test RR' too Large ............. 0.89 PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.93 PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Ru - C5 .. 6.70 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Ru - Cl1_a .. 5.94 su PLAT330_ALERT_2_C Large Average Phenyl C-C Dist. C1 -C6 1.41 Ang. PLAT431_ALERT_2_C Short Inter HL..A Contact Cl2 .. Cl3 .. 3.35 Ang. PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 2 C H Cl3
Alert level G ABSTM02_ALERT_3_G When printed, the submitted absorption T values will be replaced by the scaled T values. Since the ratio of scaled T's is identical to the ratio of reported T values, the scaling does not imply a change to the absorption corrections used in the study. Ratio of Tmax expected/reported 0.925 Tmax scaled 0.734 Tmin scaled 0.367
0 ALERT level A = In general: serious problem 2 ALERT level B = Potentially serious problem 9 ALERT level C = Check and explain 1 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 4 ALERT type 3 Indicator that the structure quality may be low 2 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: EXPOSE in IPDS Software (Stoe & Cie, 2000); cell refinement: CELL in IPDS Software; data reduction: INTEGRATE in IPDS Software; program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: SHELXL97.
[Ru2Cl4(C6H6)2]·2CHCl3 | Z = 1 |
Mr = 738.90 | F(000) = 356 |
Triclinic, P1 | Dx = 2.219 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 7.9951 (10) Å | Cell parameters from 5113 reflections |
b = 8.1835 (11) Å | θ = 2.4–25.9° |
c = 9.6545 (13) Å | µ = 2.57 mm−1 |
α = 69.312 (15)° | T = 173 K |
β = 69.676 (15)° | Block, orange |
γ = 86.164 (16)° | 0.35 × 0.23 × 0.12 mm |
V = 553.03 (15) Å3 |
Stoe IPDS diffractometer | 2014 independent reflections |
Radiation source: fine-focus sealed tube | 1817 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.032 |
Detector resolution: 0.81Å pixels mm-1 | θmax = 25.9°, θmin = 2.4° |
φ oscillation scans | h = −9→9 |
Absorption correction: part of the refinement model (ΔF) (DIFABS; Walker & Stuart, 1983) | k = −10→10 |
Tmin = 0.397, Tmax = 0.794 | l = −11→11 |
4350 measured reflections |
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)] = 0.023 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.079 | H-atom parameters constrained |
S = 1.20 | w = 1/[σ2(Fo2) + (0.0458P)2 + 0.223P] where P = (Fo2 + 2Fc2)/3 |
2014 reflections | (Δ/σ)max < 0.001 |
118 parameters | Δρmax = 0.59 e Å−3 |
12 restraints | Δρmin = −0.88 e Å−3 |
Experimental. A crystal was mounted at 173 K on a Stoe Image Plate Diffraction System (Stoe & Cie, 2000) using Mo Kα graphite monochromated radiation. Image plate distance 70 mm, φ oscillation scans 0 - 186°, step Δφ = 2.0°, 3 minutes per frame. |
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 | ||
C1 | 0.2122 (6) | 0.2228 (5) | 0.2522 (5) | 0.0271 (8) | |
H1 | 0.1615 | 0.1106 | 0.2845 | 0.033* | |
C2 | 0.3108 (5) | 0.2615 (5) | 0.3346 (5) | 0.0269 (8) | |
H2 | 0.3237 | 0.1736 | 0.4223 | 0.032* | |
C3 | 0.3894 (5) | 0.4295 (6) | 0.2869 (5) | 0.0255 (8) | |
H3 | 0.4564 | 0.4527 | 0.3403 | 0.031* | |
C4 | 0.3646 (5) | 0.5637 (5) | 0.1552 (5) | 0.0261 (8) | |
H4 | 0.4128 | 0.6766 | 0.1244 | 0.031* | |
C5 | 0.2683 (5) | 0.5279 (5) | 0.0710 (4) | 0.0234 (7) | |
H5 | 0.2550 | 0.6161 | −0.0164 | 0.028* | |
C6 | 0.1918 (5) | 0.3578 (5) | 0.1196 (5) | 0.0253 (8) | |
H6 | 0.1276 | 0.3339 | 0.0643 | 0.030* | |
C7 | −0.2831 (6) | −0.0814 (5) | 0.2244 (5) | 0.0264 (9) | |
H7 | −0.2017 | −0.1735 | 0.2481 | 0.032* | |
Cl1 | 0.05653 (12) | 0.70373 (10) | 0.39911 (10) | 0.0197 (2) | |
Cl2 | −0.18041 (12) | 0.48946 (12) | 0.28739 (12) | 0.0244 (2) | |
Cl3 | −0.23396 (14) | 0.09486 (12) | 0.27166 (12) | 0.0287 (2) | |
Cl4 | −0.50274 (15) | −0.16644 (15) | 0.33707 (16) | 0.0401 (3) | |
Cl5 | −0.2489 (2) | −0.00924 (15) | 0.01980 (14) | 0.0488 (3) | |
Ru | 0.10494 (4) | 0.44595 (3) | 0.31870 (3) | 0.01443 (12) |
U11 | U22 | U33 | U12 | U13 | U23 | |
C1 | 0.029 (2) | 0.0220 (16) | 0.033 (2) | 0.0088 (16) | −0.0071 (19) | −0.0168 (14) |
C2 | 0.022 (2) | 0.0311 (16) | 0.027 (2) | 0.0162 (15) | −0.0102 (18) | −0.0103 (15) |
C3 | 0.0095 (19) | 0.0422 (19) | 0.028 (2) | 0.0066 (15) | −0.0045 (18) | −0.0186 (16) |
C4 | 0.016 (2) | 0.0256 (17) | 0.030 (2) | −0.0009 (15) | 0.0026 (18) | −0.0114 (14) |
C5 | 0.020 (2) | 0.0308 (16) | 0.0063 (15) | 0.0034 (15) | 0.0075 (15) | −0.0031 (14) |
C6 | 0.025 (2) | 0.0344 (17) | 0.0242 (18) | 0.0090 (16) | −0.0077 (18) | −0.0206 (15) |
C7 | 0.030 (2) | 0.0234 (19) | 0.031 (2) | 0.0068 (17) | −0.013 (2) | −0.0135 (17) |
Cl1 | 0.0218 (5) | 0.0169 (4) | 0.0186 (4) | 0.0003 (3) | −0.0037 (4) | −0.0074 (3) |
Cl2 | 0.0194 (5) | 0.0270 (5) | 0.0345 (5) | 0.0063 (4) | −0.0151 (5) | −0.0149 (4) |
Cl3 | 0.0377 (6) | 0.0223 (5) | 0.0294 (5) | −0.0014 (4) | −0.0147 (5) | −0.0095 (4) |
Cl4 | 0.0276 (6) | 0.0352 (6) | 0.0631 (8) | 0.0008 (5) | −0.0135 (6) | −0.0258 (6) |
Cl5 | 0.0843 (10) | 0.0392 (6) | 0.0313 (6) | 0.0131 (6) | −0.0246 (7) | −0.0194 (5) |
Ru | 0.0132 (2) | 0.01639 (17) | 0.01456 (18) | 0.00278 (12) | −0.00453 (14) | −0.00703 (12) |
C1—C2 | 1.415 (6) | C5—C6 | 1.409 (6) |
C1—C6 | 1.416 (5) | C5—Ru | 2.165 (4) |
C1—Ru | 2.172 (4) | C5—H5 | 0.9300 |
C1—H1 | 0.9300 | C6—Ru | 2.164 (4) |
C2—C3 | 1.402 (6) | C6—H6 | 0.9300 |
C2—Ru | 2.166 (3) | C7—Cl4 | 1.747 (4) |
C2—H2 | 0.9300 | C7—Cl3 | 1.763 (4) |
C3—C4 | 1.422 (6) | C7—Cl5 | 1.774 (4) |
C3—Ru | 2.188 (4) | C7—H7 | 0.9800 |
C3—H3 | 0.9300 | Ru—Cl1 | 2.4580 (9) |
C4—C5 | 1.404 (6) | Ru—Cl2 | 2.3911 (9) |
C4—Ru | 2.156 (4) | Ru—Cl1i | 2.4495 (11) |
C4—H4 | 0.9300 | ||
C2—C1—C6 | 119.0 (4) | Cl3—C7—H7 | 108.7 |
C2—C1—Ru | 70.7 (2) | Cl5—C7—H7 | 108.7 |
C6—C1—Ru | 70.6 (2) | Rui—Cl1—Ru | 98.22 (3) |
C2—C1—H1 | 120.5 | C4—Ru—C6 | 68.53 (15) |
C6—C1—H1 | 120.5 | C4—Ru—C5 | 37.93 (15) |
Ru—C1—H1 | 130.7 | C6—Ru—C5 | 37.99 (16) |
C3—C2—C1 | 121.3 (3) | C4—Ru—C2 | 68.41 (16) |
C3—C2—Ru | 72.1 (2) | C6—Ru—C2 | 68.58 (14) |
C1—C2—Ru | 71.2 (2) | C5—Ru—C2 | 81.11 (15) |
C3—C2—H2 | 119.3 | C4—Ru—C1 | 81.37 (16) |
C1—C2—H2 | 119.3 | C6—Ru—C1 | 38.13 (15) |
Ru—C2—H2 | 130.0 | C5—Ru—C1 | 68.86 (15) |
C2—C3—C4 | 118.7 (3) | C2—Ru—C1 | 38.07 (15) |
C2—C3—Ru | 70.4 (2) | C4—Ru—C3 | 38.21 (15) |
C4—C3—Ru | 69.7 (2) | C6—Ru—C3 | 81.15 (15) |
C2—C3—H3 | 120.6 | C5—Ru—C3 | 68.76 (15) |
C4—C3—H3 | 120.6 | C2—Ru—C3 | 37.56 (16) |
Ru—C3—H3 | 132.1 | C1—Ru—C3 | 68.56 (15) |
C5—C4—C3 | 120.9 (4) | C4—Ru—Cl2 | 129.55 (11) |
C5—C4—Ru | 71.4 (2) | C6—Ru—Cl2 | 88.33 (10) |
C3—C4—Ru | 72.1 (2) | C5—Ru—Cl2 | 97.81 (11) |
C5—C4—H4 | 119.6 | C2—Ru—Cl2 | 143.88 (12) |
C3—C4—H4 | 119.6 | C1—Ru—Cl2 | 107.71 (11) |
Ru—C4—H4 | 129.3 | C3—Ru—Cl2 | 166.56 (11) |
C4—C5—C6 | 119.6 (3) | C4—Ru—Cl1i | 141.50 (11) |
C4—C5—Ru | 70.7 (2) | C6—Ru—Cl1i | 132.60 (12) |
C6—C5—Ru | 70.9 (2) | C5—Ru—Cl1i | 168.60 (10) |
C4—C5—H5 | 120.2 | C2—Ru—Cl1i | 88.83 (11) |
C6—C5—H5 | 120.2 | C1—Ru—Cl1i | 99.88 (12) |
Ru—C5—H5 | 130.9 | C3—Ru—Cl1i | 106.13 (11) |
C5—C6—C1 | 120.4 (3) | Cl2—Ru—Cl1i | 87.14 (4) |
C5—C6—Ru | 71.1 (2) | C4—Ru—Cl1 | 88.58 (10) |
C1—C6—Ru | 71.2 (2) | C6—Ru—Cl1 | 144.88 (11) |
C5—C6—H6 | 119.8 | C5—Ru—Cl1 | 108.68 (11) |
C1—C6—H6 | 119.8 | C2—Ru—Cl1 | 128.41 (11) |
Ru—C6—H6 | 130.6 | C1—Ru—Cl1 | 165.79 (11) |
Cl4—C7—Cl3 | 110.4 (2) | C3—Ru—Cl1 | 97.37 (11) |
Cl4—C7—Cl5 | 110.8 (2) | Cl2—Ru—Cl1 | 86.43 (3) |
Cl3—C7—Cl5 | 109.4 (2) | Cl1i—Ru—Cl1 | 81.78 (3) |
Cl4—C7—H7 | 108.7 | ||
C6—C1—C2—C3 | −0.6 (6) | C6—C5—Ru—Cl2 | −77.1 (2) |
Ru—C1—C2—C3 | −54.0 (3) | C4—C5—Ru—Cl1i | −94.4 (6) |
C6—C1—C2—Ru | 53.4 (3) | C6—C5—Ru—Cl1i | 38.1 (7) |
C1—C2—C3—C4 | 1.6 (6) | C4—C5—Ru—Cl1 | 61.6 (2) |
Ru—C2—C3—C4 | −52.0 (3) | C6—C5—Ru—Cl1 | −165.94 (19) |
C1—C2—C3—Ru | 53.6 (3) | C3—C2—Ru—C4 | 29.3 (2) |
C2—C3—C4—C5 | −2.1 (6) | C1—C2—Ru—C4 | −104.1 (3) |
Ru—C3—C4—C5 | −54.4 (3) | C3—C2—Ru—C6 | 103.8 (3) |
C2—C3—C4—Ru | 52.3 (3) | C1—C2—Ru—C6 | −29.6 (3) |
C3—C4—C5—C6 | 1.4 (6) | C3—C2—Ru—C5 | 66.5 (2) |
Ru—C4—C5—C6 | −53.3 (3) | C1—C2—Ru—C5 | −66.9 (3) |
C3—C4—C5—Ru | 54.7 (3) | C3—C2—Ru—C1 | 133.4 (4) |
C4—C5—C6—C1 | −0.3 (6) | C1—C2—Ru—C3 | −133.4 (4) |
Ru—C5—C6—C1 | −53.4 (3) | C3—C2—Ru—Cl2 | 157.62 (18) |
C4—C5—C6—Ru | 53.2 (3) | C1—C2—Ru—Cl2 | 24.2 (3) |
C2—C1—C6—C5 | −0.2 (6) | C3—C2—Ru—Cl1i | −118.8 (2) |
Ru—C1—C6—C5 | 53.3 (3) | C1—C2—Ru—Cl1i | 107.7 (2) |
C2—C1—C6—Ru | −53.5 (3) | C3—C2—Ru—Cl1 | −40.3 (3) |
C5—C4—Ru—C6 | 29.2 (2) | C1—C2—Ru—Cl1 | −173.7 (2) |
C3—C4—Ru—C6 | −103.4 (2) | C2—C1—Ru—C4 | 65.8 (3) |
C3—C4—Ru—C5 | −132.6 (3) | C6—C1—Ru—C4 | −66.0 (3) |
C5—C4—Ru—C2 | 103.7 (2) | C2—C1—Ru—C6 | 131.9 (4) |
C3—C4—Ru—C2 | −28.9 (2) | C2—C1—Ru—C5 | 103.0 (3) |
C5—C4—Ru—C1 | 66.5 (2) | C6—C1—Ru—C5 | −28.8 (2) |
C3—C4—Ru—C1 | −66.1 (2) | C6—C1—Ru—C2 | −131.9 (4) |
C5—C4—Ru—C3 | 132.6 (3) | C2—C1—Ru—C3 | 28.4 (2) |
C5—C4—Ru—Cl2 | −39.4 (3) | C6—C1—Ru—C3 | −103.5 (3) |
C3—C4—Ru—Cl2 | −172.00 (17) | C2—C1—Ru—Cl2 | −165.3 (2) |
C5—C4—Ru—Cl1i | 161.55 (17) | C6—C1—Ru—Cl2 | 62.8 (3) |
C3—C4—Ru—Cl1i | 28.9 (3) | C2—C1—Ru—Cl1i | −75.2 (2) |
C5—C4—Ru—Cl1 | −123.6 (2) | C6—C1—Ru—Cl1i | 153.0 (2) |
C3—C4—Ru—Cl1 | 103.8 (2) | C2—C1—Ru—Cl1 | 20.4 (6) |
C5—C6—Ru—C4 | −29.1 (2) | C6—C1—Ru—Cl1 | −111.5 (4) |
C1—C6—Ru—C4 | 103.9 (3) | C2—C3—Ru—C4 | −132.5 (3) |
C1—C6—Ru—C5 | 133.0 (4) | C2—C3—Ru—C6 | −66.2 (2) |
C5—C6—Ru—C2 | −103.5 (3) | C4—C3—Ru—C6 | 66.4 (2) |
C1—C6—Ru—C2 | 29.6 (3) | C2—C3—Ru—C5 | −103.5 (2) |
C5—C6—Ru—C1 | −133.0 (4) | C4—C3—Ru—C5 | 29.0 (2) |
C5—C6—Ru—C3 | −66.6 (2) | C4—C3—Ru—C2 | 132.5 (3) |
C1—C6—Ru—C3 | 66.4 (3) | C2—C3—Ru—C1 | −28.8 (2) |
C5—C6—Ru—Cl2 | 105.0 (2) | C4—C3—Ru—C1 | 103.8 (3) |
C1—C6—Ru—Cl2 | −122.0 (2) | C2—C3—Ru—Cl2 | −105.0 (5) |
C5—C6—Ru—Cl1i | −170.47 (17) | C4—C3—Ru—Cl2 | 27.5 (6) |
C1—C6—Ru—Cl1i | −37.4 (3) | C2—C3—Ru—Cl1i | 65.7 (2) |
C5—C6—Ru—Cl1 | 23.6 (3) | C4—C3—Ru—Cl1i | −161.73 (19) |
C1—C6—Ru—Cl1 | 156.6 (2) | C2—C3—Ru—Cl1 | 149.3 (2) |
C6—C5—Ru—C4 | 132.5 (3) | C4—C3—Ru—Cl1 | −78.2 (2) |
C4—C5—Ru—C6 | −132.5 (3) | Rui—Cl1—Ru—C4 | −142.61 (11) |
C4—C5—Ru—C2 | −66.1 (2) | Rui—Cl1—Ru—C6 | 169.59 (18) |
C6—C5—Ru—C2 | 66.4 (2) | Rui—Cl1—Ru—C5 | −175.34 (11) |
C4—C5—Ru—C1 | −103.6 (2) | Rui—Cl1—Ru—C2 | −81.91 (15) |
C6—C5—Ru—C1 | 28.9 (2) | Rui—Cl1—Ru—C1 | −97.8 (5) |
C4—C5—Ru—C3 | −29.2 (2) | Rui—Cl1—Ru—C3 | −105.33 (11) |
C6—C5—Ru—C3 | 103.3 (2) | Rui—Cl1—Ru—Cl2 | 87.62 (4) |
C4—C5—Ru—Cl2 | 150.4 (2) | Rui—Cl1—Ru—Cl1i | 0.0 |
Symmetry code: (i) −x, −y+1, −z+1. |
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