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The title compound, [Ru2Cl3(C10H14)2]2[Hg2Cl6], contains two [{Ru(C10H14)}2(μ-Cl)3]+ cations and one [Hg2Cl6]2− anion. In the cation, two [Ru(η6-p-cymene)] fragments are linked by three bridging Cl atoms. The anion lies on a twofold rotation axis. The coordination geometry of ruthenium is pseudo-octahedral, while the coordination around mercury is highly distorted tetrahedral. The average Ru—Cl bond length is 2.435 Å. The average bridging and terminal Hg—Cl distances are 2.664 and 2.435 Å, respectively.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804007214/cf6331sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804007214/cf6331Isup2.hkl
Contains datablock I

CCDC reference: 238685

Key indicators

  • Single-crystal X-ray study
  • T = 100 K
  • Mean [sigma](C-C) = 0.006 Å
  • R factor = 0.033
  • wR factor = 0.084
  • Data-to-parameter ratio = 22.8

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT029_ALERT_3_B _diffrn_measured_fraction_theta_full Low ....... 0.95 PLAT432_ALERT_2_B Short Inter X...Y Contact C5 .. C5 .. 3.06 Ang.
Alert level C PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 2.00 Ratio PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ? PLAT233_ALERT_4_C Hirshfeld (M-X Solvent) Hg1 - Cl6_a .. 13.59 su PLAT432_ALERT_2_C Short Inter X...Y Contact C5 .. C6 .. 3.17 Ang.
0 ALERT level A = In general: serious problem 2 ALERT level B = Potentially serious problem 6 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 2 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 2 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: SMART (Bruker, 1998); cell refinement: SMART; data reduction: SAINT (Bruker, 1998); program(s) used to solve structure: SHELXTL (Sheldrick, 1997b); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

(I) top
Crystal data top
[Ru2Cl3(C10H14)2]2[Hg2Cl6]F(000) = 3344
Mr = 1767.71Dx = 2.318 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
a = 20.0879 (13) ÅCell parameters from 6323 reflections
b = 11.1018 (7) Åθ = 2.3–28.2°
c = 23.7560 (15) ŵ = 7.87 mm1
β = 107.055 (1)°T = 100 K
V = 5064.9 (6) Å3Bar, orange
Z = 40.40 × 0.08 × 0.08 mm
Data collection top
Bruker SMART CCD area-detector
diffractometer
5982 independent reflections
Radiation source: fine-focus sealed tube5361 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.030
φ and ω scansθmax = 28.3°, θmin = 1.8°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1997a)
h = 2526
Tmin = 0.245, Tmax = 0.533k = 1413
15246 measured reflectionsl = 1831
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.033Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.084H-atom parameters constrained
S = 1.04 w = 1/[σ2(Fo2) + (0.0484P)2 + 1.6219P]
where P = (Fo2 + 2Fc2)/3
5982 reflections(Δ/σ)max = 0.001
262 parametersΔρmax = 1.81 e Å3
0 restraintsΔρmin = 1.06 e Å3
Special details top

Experimental. The data collection covered over a hemisphere of reciprocal space by a combination of three sets of exposures; each set had a different φ angle (0, 88 and 180°) for the crystal and each exposure of 20 s covered 0.3° in ω. The crystal-to-detector distance was 4 cm and the detector swing a ngle was -35°. Coverage of the unique set is over 99% complete. Crystal decay was monitored by repeating fifty initial frames at the end of data collection and analysing the duplicate reflections, and was found to be negligible.

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
xyzUiso*/Ueq
Hg10.464140 (10)0.477956 (16)0.312927 (8)0.02548 (7)
Ru10.321938 (17)0.41019 (3)0.452154 (15)0.01445 (8)
Ru20.181318 (17)0.43091 (3)0.339847 (15)0.01481 (8)
Cl10.29670 (6)0.51480 (9)0.35862 (5)0.0219 (2)
Cl20.25173 (5)0.25863 (9)0.38649 (4)0.0176 (2)
Cl30.20515 (6)0.48478 (9)0.44368 (5)0.0198 (2)
Cl40.46131 (6)0.66008 (9)0.36508 (5)0.0228 (2)
Cl50.45867 (7)0.26697 (10)0.32880 (5)0.0289 (3)
Cl60.40629 (6)0.51303 (10)0.20250 (5)0.0240 (2)
C10.4049 (2)0.2805 (4)0.49114 (19)0.0200 (9)
C20.3669 (2)0.3061 (4)0.53171 (19)0.0195 (9)
H2A0.34770.24170.54820.023*
C30.3575 (2)0.4254 (4)0.5478 (2)0.0215 (9)
H3A0.33250.43970.57550.026*
C40.3843 (2)0.5253 (4)0.5236 (2)0.0206 (9)
C50.4205 (2)0.4985 (4)0.4823 (2)0.0183 (8)
H5A0.43820.56300.46460.022*
C60.4312 (2)0.3793 (4)0.46645 (19)0.0205 (9)
H6A0.45640.36500.43890.025*
C70.4144 (2)0.1546 (4)0.4727 (2)0.0251 (10)
H7A0.45710.12060.49930.038*
H7B0.41780.15510.43240.038*
H7C0.37440.10550.47420.038*
C80.3758 (3)0.6539 (4)0.5414 (2)0.0287 (11)
H8A0.41930.67330.57350.034*
C90.3173 (3)0.6704 (4)0.5679 (2)0.0328 (12)
H9A0.32160.61100.59930.049*
H9B0.27270.65910.53750.049*
H9C0.31930.75170.58430.049*
C100.3733 (3)0.7437 (5)0.4916 (3)0.0383 (13)
H10A0.41260.72880.47600.057*
H10B0.37610.82610.50700.057*
H10C0.32950.73360.46010.057*
C140.1567 (2)0.4303 (4)0.24458 (19)0.0187 (8)
C130.1401 (2)0.5452 (4)0.2642 (2)0.0194 (9)
H13A0.15860.61570.25180.023*
C120.0975 (2)0.5568 (4)0.3012 (2)0.0215 (9)
H12A0.08750.63460.31330.026*
C110.0691 (2)0.4524 (4)0.3209 (2)0.0207 (9)
C160.0837 (2)0.3381 (4)0.3006 (2)0.0192 (9)
H16A0.06400.26760.31180.023*
C150.1278 (2)0.3280 (4)0.26340 (19)0.0197 (9)
H15A0.13780.25050.25110.024*
C170.0278 (3)0.4647 (4)0.3635 (2)0.0248 (10)
H17A0.02160.47340.34190.037*
H17B0.04360.53590.38820.037*
H17C0.03440.39280.38850.037*
C180.2087 (2)0.4258 (4)0.2096 (2)0.0217 (9)
H18A0.24150.49510.22250.026*
C190.2517 (3)0.3107 (4)0.2193 (2)0.0295 (11)
H19A0.27590.30130.26130.044*
H19D0.28600.31510.19730.044*
H19B0.22100.24150.20550.044*
C200.1696 (3)0.4441 (6)0.1444 (2)0.0377 (13)
H20D0.14250.51880.13960.057*
H20A0.13810.37600.13030.057*
H20B0.20300.44930.12170.057*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Hg10.03277 (12)0.01778 (10)0.02336 (12)0.00108 (7)0.00430 (9)0.00106 (6)
Ru10.01507 (17)0.01389 (15)0.01445 (17)0.00107 (12)0.00441 (14)0.00038 (12)
Ru20.01443 (16)0.01199 (15)0.01695 (18)0.00084 (12)0.00292 (13)0.00114 (12)
Cl10.0182 (5)0.0242 (5)0.0209 (5)0.0053 (4)0.0020 (4)0.0071 (4)
Cl20.0177 (5)0.0142 (4)0.0195 (5)0.0006 (3)0.0035 (4)0.0006 (4)
Cl30.0185 (5)0.0190 (5)0.0218 (6)0.0011 (4)0.0057 (4)0.0030 (4)
Cl40.0275 (6)0.0205 (5)0.0223 (6)0.0031 (4)0.0102 (5)0.0011 (4)
Cl50.0437 (7)0.0174 (5)0.0264 (6)0.0020 (5)0.0116 (5)0.0004 (4)
Cl60.0241 (6)0.0261 (5)0.0200 (6)0.0005 (4)0.0036 (5)0.0020 (4)
C10.018 (2)0.024 (2)0.016 (2)0.0010 (17)0.0014 (17)0.0002 (17)
C20.022 (2)0.019 (2)0.017 (2)0.0025 (17)0.0054 (18)0.0035 (16)
C30.024 (2)0.023 (2)0.018 (2)0.0031 (17)0.0080 (19)0.0003 (17)
C40.021 (2)0.023 (2)0.017 (2)0.0045 (16)0.0032 (19)0.0019 (16)
C50.014 (2)0.022 (2)0.016 (2)0.0051 (16)0.0002 (17)0.0009 (16)
C60.017 (2)0.029 (2)0.015 (2)0.0002 (17)0.0036 (17)0.0011 (17)
C70.025 (2)0.024 (2)0.025 (2)0.0049 (18)0.005 (2)0.0002 (18)
C80.038 (3)0.020 (2)0.029 (3)0.004 (2)0.012 (2)0.0059 (19)
C90.046 (3)0.021 (2)0.034 (3)0.007 (2)0.015 (3)0.001 (2)
C100.059 (4)0.022 (2)0.043 (3)0.000 (2)0.030 (3)0.001 (2)
C140.017 (2)0.019 (2)0.018 (2)0.0004 (16)0.0013 (17)0.0030 (16)
C130.015 (2)0.0172 (19)0.023 (2)0.0002 (16)0.0006 (18)0.0052 (17)
C120.023 (2)0.017 (2)0.022 (2)0.0032 (17)0.0020 (19)0.0013 (17)
C110.016 (2)0.022 (2)0.022 (2)0.0007 (16)0.0032 (18)0.0027 (18)
C160.016 (2)0.0160 (19)0.023 (2)0.0038 (16)0.0029 (18)0.0027 (16)
C150.021 (2)0.0167 (19)0.019 (2)0.0004 (16)0.0008 (18)0.0040 (16)
C170.021 (2)0.022 (2)0.032 (3)0.0005 (17)0.009 (2)0.0027 (19)
C180.021 (2)0.022 (2)0.022 (2)0.0001 (17)0.0061 (19)0.0028 (17)
C190.036 (3)0.022 (2)0.034 (3)0.005 (2)0.016 (2)0.002 (2)
C200.034 (3)0.054 (3)0.027 (3)0.009 (3)0.012 (2)0.010 (3)
Geometric parameters (Å, º) top
Hg1—Cl52.3801 (11)C7—H7B0.980
Hg1—Cl42.3807 (11)C7—H7C0.980
Hg1—Cl62.5681 (12)C8—C91.499 (7)
Hg1—Cl6i2.7605 (12)C8—C101.537 (7)
Ru1—C52.136 (4)C8—H8A1.000
Ru1—C62.148 (4)C9—H9A0.980
Ru1—C22.173 (4)C9—H9B0.980
Ru1—C32.179 (5)C9—H9C0.980
Ru1—C12.192 (4)C10—H10A0.980
Ru1—C42.200 (4)C10—H10B0.980
Ru1—Cl12.4253 (11)C10—H10C0.980
Ru1—Cl32.4399 (11)C14—C151.407 (6)
Ru1—Cl22.4420 (10)C14—C131.431 (6)
Ru2—C152.148 (4)C14—C181.516 (6)
Ru2—C132.156 (4)C13—C121.400 (6)
Ru2—C162.169 (4)C13—H13A0.950
Ru2—C142.170 (4)C12—C111.430 (6)
Ru2—C122.173 (4)C12—H12A0.950
Ru2—C112.179 (4)C11—C161.418 (6)
Ru2—Cl12.4151 (11)C11—C171.492 (6)
Ru2—Cl22.4428 (10)C16—C151.426 (6)
Ru2—Cl32.4451 (12)C16—H16A0.950
Cl6—Hg1i2.7605 (12)C15—H15A0.950
C1—C61.417 (6)C17—H17A0.980
C1—C21.423 (6)C17—H17B0.980
C1—C71.494 (6)C17—H17C0.980
C2—C31.406 (6)C18—C191.522 (6)
C2—H2A0.950C18—C201.530 (7)
C3—C41.426 (6)C18—H18A1.000
C3—H3A0.950C19—H19A0.980
C4—C51.414 (6)C19—H19D0.980
C4—C81.513 (6)C19—H19B0.980
C5—C61.410 (6)C20—H20D0.980
C5—H5A0.950C20—H20A0.980
C6—H6A0.950C20—H20B0.980
C7—H7A0.980
Cl5—Hg1—Cl4138.08 (4)C5—C4—C8121.0 (4)
Cl5—Hg1—Cl6106.44 (4)C3—C4—C8122.3 (4)
Cl4—Hg1—Cl6109.27 (4)C5—C4—Ru168.6 (2)
Cl5—Hg1—Cl6i104.42 (4)C3—C4—Ru170.2 (3)
Cl4—Hg1—Cl6i96.70 (4)C8—C4—Ru1132.7 (3)
Cl6—Hg1—Cl6i90.27 (4)C6—C5—C4122.2 (4)
C5—Ru1—C638.42 (17)C6—C5—Ru171.3 (2)
C5—Ru1—C281.05 (16)C4—C5—Ru173.4 (2)
C6—Ru1—C268.45 (16)C6—C5—H5A118.9
C5—Ru1—C368.11 (17)C4—C5—H5A118.9
C6—Ru1—C380.83 (17)Ru1—C5—H5A128.9
C2—Ru1—C337.69 (16)C5—C6—C1120.8 (4)
C5—Ru1—C169.19 (16)C5—C6—Ru170.3 (2)
C6—Ru1—C138.10 (16)C1—C6—Ru172.6 (2)
C2—Ru1—C138.04 (15)C5—C6—H6A119.6
C3—Ru1—C168.55 (16)C1—C6—H6A119.6
C5—Ru1—C438.03 (16)Ru1—C6—H6A130.0
C6—Ru1—C469.28 (17)C1—C7—H7A109.5
C2—Ru1—C468.90 (16)C1—C7—H7B109.5
C3—Ru1—C438.01 (16)H7A—C7—H7B109.5
C1—Ru1—C482.24 (17)C1—C7—H7C109.5
C5—Ru1—Cl190.65 (12)H7A—C7—H7C109.5
C6—Ru1—Cl198.66 (12)H7B—C7—H7C109.5
C2—Ru1—Cl1166.73 (12)C9—C8—C4113.5 (4)
C3—Ru1—Cl1146.59 (12)C9—C8—C10113.1 (4)
C1—Ru1—Cl1129.08 (11)C4—C8—C10112.2 (4)
C4—Ru1—Cl1110.35 (12)C9—C8—H8A105.7
C5—Ru1—Cl3130.25 (12)C4—C8—H8A105.7
C6—Ru1—Cl3168.67 (13)C10—C8—H8A105.7
C2—Ru1—Cl3113.37 (12)C8—C9—H9A109.5
C3—Ru1—Cl394.17 (12)C8—C9—H9B109.5
C1—Ru1—Cl3148.37 (12)H9A—C9—H9B109.5
C4—Ru1—Cl3100.54 (12)C8—C9—H9C109.5
Cl1—Ru1—Cl379.89 (4)H9A—C9—H9C109.5
C5—Ru1—Cl2146.65 (12)H9B—C9—H9C109.5
C6—Ru1—Cl2111.28 (12)C8—C10—H10A109.5
C2—Ru1—Cl2101.78 (12)C8—C10—H10B109.5
C3—Ru1—Cl2132.10 (12)H10A—C10—H10B109.5
C1—Ru1—Cl292.43 (12)C8—C10—H10C109.5
C4—Ru1—Cl2170.05 (12)H10A—C10—H10C109.5
Cl1—Ru1—Cl279.54 (4)H10B—C10—H10C109.5
Cl3—Ru1—Cl279.63 (3)C15—C14—C13117.3 (4)
C15—Ru2—C1368.52 (16)C15—C14—C18124.3 (4)
C15—Ru2—C1638.58 (16)C13—C14—C18118.2 (4)
C13—Ru2—C1681.00 (16)C15—C14—Ru270.1 (2)
C15—Ru2—C1438.01 (16)C13—C14—Ru270.2 (3)
C13—Ru2—C1438.61 (16)C18—C14—Ru2126.1 (3)
C16—Ru2—C1469.45 (16)C12—C13—C14122.0 (4)
C15—Ru2—C1281.44 (17)C12—C13—Ru271.8 (3)
C13—Ru2—C1237.74 (16)C14—C13—Ru271.2 (2)
C16—Ru2—C1268.50 (16)C12—C13—H13A119.0
C14—Ru2—C1269.51 (17)C14—C13—H13A119.0
C15—Ru2—C1169.63 (17)Ru2—C13—H13A130.9
C13—Ru2—C1169.04 (16)C13—C12—C11120.4 (4)
C16—Ru2—C1138.08 (16)C13—C12—Ru270.5 (3)
C14—Ru2—C1183.04 (17)C11—C12—Ru271.0 (2)
C12—Ru2—C1138.38 (16)C13—C12—H12A119.8
C15—Ru2—Cl1125.22 (12)C11—C12—H12A119.8
C13—Ru2—Cl192.29 (12)Ru2—C12—H12A131.6
C16—Ru2—Cl1163.80 (12)C16—C11—C12118.2 (4)
C14—Ru2—Cl196.14 (12)C16—C11—C17121.6 (4)
C12—Ru2—Cl1114.36 (12)C12—C11—C17120.2 (4)
C11—Ru2—Cl1151.03 (12)C16—C11—Ru270.6 (2)
C15—Ru2—Cl292.69 (12)C12—C11—Ru270.6 (2)
C13—Ru2—Cl2150.26 (12)C17—C11—Ru2128.1 (3)
C16—Ru2—Cl298.81 (11)C11—C16—C15120.6 (4)
C14—Ru2—Cl2113.28 (12)C11—C16—Ru271.3 (2)
C12—Ru2—Cl2165.66 (12)C15—C16—Ru269.9 (2)
C11—Ru2—Cl2127.29 (12)C11—C16—H16A119.7
Cl1—Ru2—Cl279.72 (4)C15—C16—H16A119.7
C15—Ru2—Cl3152.16 (12)Ru2—C16—H16A132.0
C13—Ru2—Cl3127.61 (12)C14—C15—C16121.5 (4)
C16—Ru2—Cl3115.79 (12)C14—C15—Ru271.8 (3)
C14—Ru2—Cl3165.95 (12)C16—C15—Ru271.5 (2)
C12—Ru2—Cl399.62 (12)C14—C15—H15A119.2
C11—Ru2—Cl393.82 (13)C16—C15—H15A119.2
Cl1—Ru2—Cl379.98 (4)Ru2—C15—H15A130.1
Cl2—Ru2—Cl379.51 (3)C11—C17—H17A109.5
Ru2—Cl1—Ru185.18 (3)C11—C17—H17B109.5
Ru1—Cl2—Ru284.22 (3)H17A—C17—H17B109.5
Ru1—Cl3—Ru284.22 (3)C11—C17—H17C109.5
Hg1—Cl6—Hg1i87.27 (4)H17A—C17—H17C109.5
C6—C1—C2117.7 (4)H17B—C17—H17C109.5
C6—C1—C7120.5 (4)C14—C18—C19113.4 (4)
C2—C1—C7121.7 (4)C14—C18—C20108.5 (4)
C6—C1—Ru169.3 (2)C19—C18—C20111.4 (4)
C2—C1—Ru170.3 (2)C14—C18—H18A107.8
C7—C1—Ru1129.6 (3)C19—C18—H18A107.8
C3—C2—C1121.0 (4)C20—C18—H18A107.8
C3—C2—Ru171.4 (3)C18—C19—H19A109.5
C1—C2—Ru171.7 (2)C18—C19—H19D109.5
C3—C2—H2A119.5H19A—C19—H19D109.5
C1—C2—H2A119.5C18—C19—H19B109.5
Ru1—C2—H2A130.0H19A—C19—H19B109.5
C2—C3—C4121.7 (4)H19D—C19—H19B109.5
C2—C3—Ru170.9 (3)C18—C20—H20D109.5
C4—C3—Ru171.8 (3)C18—C20—H20A109.5
C2—C3—H3A119.1H20D—C20—H20A109.5
C4—C3—H3A119.1C18—C20—H20B109.5
Ru1—C3—H3A131.1H20D—C20—H20B109.5
C5—C4—C3116.6 (4)H20A—C20—H20B109.5
Symmetry code: (i) x+1, y, z+1/2.
 

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