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A new (third) polymorph of the title complex, [Ru4(C10H15)4Cl4] or [Cp*Ru(μ3-Cl)]4 [Cp* = η5-C5(CH3)5], crystallizes in the tetra­gonal system, with imposed \overline{4} symmetry. The complex contains a distorted cubic array of Ru and Cl atoms. The structure is an inversion twin.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680702627X/bt2380sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S160053680702627X/bt2380Isup2.hkl
Contains datablock I

CCDC reference: 654688

Key indicators

  • Single-crystal X-ray study
  • T = 133 K
  • Mean [sigma](C-C) = 0.004 Å
  • R factor = 0.024
  • wR factor = 0.049
  • Data-to-parameter ratio = 28.8

checkCIF/PLATON results

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Alert level C ABSTM02_ALERT_3_C The ratio of expected to reported Tmax/Tmin(RR') is < 0.90 Tmin and Tmax reported: 0.530 0.736 Tmin(prime) and Tmax expected: 0.607 0.722 RR(prime) = 0.856 Please check that your absorption correction is appropriate. STRVA01_ALERT_4_C Flack test results are ambiguous. From the CIF: _refine_ls_abs_structure_Flack 0.430 From the CIF: _refine_ls_abs_structure_Flack_su 0.030 PLAT048_ALERT_1_C MoietyFormula Not Given ........................ ? PLAT061_ALERT_3_C Tmax/Tmin Range Test RR' too Large ............. 0.84 PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.98 PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.57 PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ? PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Ru - Cl .. 9.58 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Ru - Cl_a .. 6.04 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Ru - Cl_c .. 9.18 su PLAT601_ALERT_2_C Structure Contains Solvent Accessible VOIDS of . 54.00 A   3 PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.11 Ratio
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 30.52 From the CIF: _reflns_number_total 3314 Count of symmetry unique reflns 1741 Completeness (_total/calc) 190.35% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 1573 Fraction of Friedel pairs measured 0.904 Are heavy atom types Z>Si present yes PLAT033_ALERT_2_G Flack Parameter Value Deviates 2 * su from zero. 0.43
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 12 ALERT level C = Check and explain 2 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 6 ALERT type 2 Indicator that the structure model may be wrong or deficient 2 ALERT type 3 Indicator that the structure quality may be low 5 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Comment top

Fagan et al. (1990) reported two polymorphs of the title complex (I) [Cp*Ru(µ3-Cl)]4. At 201 K the crystal is triclinic with space group P1 (a = 11.281 (5), b = 11.354 (4), c = 18.846 (5) Å, α = 82.20 (2)°, β = 82.03 (3)°, γ = 65.45 (4) °; V = 2166.3 Å3) whereas at room temperature it adopts a monoclinic cell (a = 19.040; b = 12.240; c = 18.850 Å; β = 99.38°; V = 4334.2 Å3). Only the structure of the triclinic form was solved and refined; its Cambridge refcode (Allen, 2002) is JERTIJ.

Here we report the structure of a new, tetragonal polymorph of (I), which crystallizes in space group I4 (a = b = 12.0733 (8), c = 14.9611 (15) Å; V = 2180.8 (3) Å3). It is noteworthy that the new form has a significantly larger cell volume then the triclinic form despite the lower temperature. The tetrameric complex possesses imposed 4 symmetry (Fig. 1) and consists, as does the triclinic form, of a distorted cubic array of four Ru and Cl atoms, with angles at ruthenium ca 82° and angles at chlorine ca 97°. Each Ru atom in the complex adopts an 18-electron configuration in a pseudooctahedral environment. The C5Me5 ligand coordinates in η5 fashion to the Ru atom with a Cp* (centroid)—Ru distance of 1.727 Å, which is slightly longer than the average Cp*—Ru distance (1.720 Å) reported by Fagan et al. The C2—centroid vector eclipses the bond Ru···Cl (torsion angle 2.1°). The structure of the complex is closely similar to that of the triclinic form; a least-squares fit of the Ru4Cl4 core for one of the many possible atom permutations gave a r.m.s. deviation of 0.019 Å. In detail, the Ru—Cl bond lengths (av. 2.534 Å) are also slightly longer than in the triclinic form (av. 2.524 Å). The Ru···Ru distances are 3.8286 (4) to Ruii, 3.7920 (4) Å to Rui and Ruiii, cf. 3.776 (2)–3.821 Å (av. 3.797 Å) in the triclinic form. The thermal parameters of the Cp* rings are normal, but were high in the triclinic form; this and the above-mentioned bond lengthening effects (presumably attributable to reduced libration) may be a result of the lower measurement temperature of the current structure.

Related literature top

For related literature, see: Allen (2002); Fagan et al. (1990).

Experimental top

The reaction between the title compound and four equivalents of the lithium salt of an imidazoline-2-imine in hexane afforded the new polymorph of the ruthenium starting complex as unreacted material, dark red-brown crystals of which were obtained by re-crystallization from hexane solution at -35 °C.

Refinement top

Methyl hydrogen atoms were located in a difference synthesis; the methyl groups were idealized and refined as rigid groups allowed to rotate but not tip, with C—H 0.98 Å, H—C—H 109.5°. U(H) values were fixed at 1.2Ueq(C). The structure was refined as a racemic twin, with components 0.57, 0.43 (3). The twinning (Flack) parameter is based on 1573 Friedel pairs.

Structure description top

Fagan et al. (1990) reported two polymorphs of the title complex (I) [Cp*Ru(µ3-Cl)]4. At 201 K the crystal is triclinic with space group P1 (a = 11.281 (5), b = 11.354 (4), c = 18.846 (5) Å, α = 82.20 (2)°, β = 82.03 (3)°, γ = 65.45 (4) °; V = 2166.3 Å3) whereas at room temperature it adopts a monoclinic cell (a = 19.040; b = 12.240; c = 18.850 Å; β = 99.38°; V = 4334.2 Å3). Only the structure of the triclinic form was solved and refined; its Cambridge refcode (Allen, 2002) is JERTIJ.

Here we report the structure of a new, tetragonal polymorph of (I), which crystallizes in space group I4 (a = b = 12.0733 (8), c = 14.9611 (15) Å; V = 2180.8 (3) Å3). It is noteworthy that the new form has a significantly larger cell volume then the triclinic form despite the lower temperature. The tetrameric complex possesses imposed 4 symmetry (Fig. 1) and consists, as does the triclinic form, of a distorted cubic array of four Ru and Cl atoms, with angles at ruthenium ca 82° and angles at chlorine ca 97°. Each Ru atom in the complex adopts an 18-electron configuration in a pseudooctahedral environment. The C5Me5 ligand coordinates in η5 fashion to the Ru atom with a Cp* (centroid)—Ru distance of 1.727 Å, which is slightly longer than the average Cp*—Ru distance (1.720 Å) reported by Fagan et al. The C2—centroid vector eclipses the bond Ru···Cl (torsion angle 2.1°). The structure of the complex is closely similar to that of the triclinic form; a least-squares fit of the Ru4Cl4 core for one of the many possible atom permutations gave a r.m.s. deviation of 0.019 Å. In detail, the Ru—Cl bond lengths (av. 2.534 Å) are also slightly longer than in the triclinic form (av. 2.524 Å). The Ru···Ru distances are 3.8286 (4) to Ruii, 3.7920 (4) Å to Rui and Ruiii, cf. 3.776 (2)–3.821 Å (av. 3.797 Å) in the triclinic form. The thermal parameters of the Cp* rings are normal, but were high in the triclinic form; this and the above-mentioned bond lengthening effects (presumably attributable to reduced libration) may be a result of the lower measurement temperature of the current structure.

For related literature, see: Allen (2002); Fagan et al. (1990).

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: XP (Siemens, 1994); software used to prepare material for publication: SHELXL97.

Figures top
[Figure 1] Fig. 1. The molecule of the title compound in the crystal. Ellipsoids represent 30% probability levels. Symmetry operators are those of Table 1.
tetra-µ3-chlorido-[tetrakis(η5-pentamethylcyclopentadienyl)ruthenium(II)] top
Crystal data top
[Ru4(C10H15)4Cl4]Dx = 1.655 Mg m3
Mr = 1086.96Mo Kα radiation, λ = 0.71073 Å
Tetragonal, I4Cell parameters from 5126 reflections
a = 12.0733 (8) Åθ = 2–30°
c = 14.9611 (15) ŵ = 1.63 mm1
V = 2180.8 (3) Å3T = 133 K
Z = 2Tablet, dark red
F(000) = 10880.30 × 0.22 × 0.20 mm
Data collection top
Bruker SMART 1000 CCD
diffractometer
3314 independent reflections
Radiation source: fine-focus sealed tube3068 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.034
Detector resolution: 8.192 pixels mm-1θmax = 30.5°, θmin = 2.2°
ω and φ scansh = 1617
Absorption correction: multi-scan
(SADABS; Bruker, 1998)
k = 1617
Tmin = 0.530, Tmax = 0.736l = 2121
13332 measured reflections
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.024H-atom parameters constrained
wR(F2) = 0.049 w = 1/[σ2(Fo2) + (0.0202P)2 + 1.4509P]
where P = (Fo2 + 2Fc2)/3
S = 1.07(Δ/σ)max = 0.003
3314 reflectionsΔρmax = 0.84 e Å3
115 parametersΔρmin = 0.33 e Å3
0 restraintsAbsolute structure: Flack (1983), 1573 Friedel pairs
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.43 (3)
Crystal data top
[Ru4(C10H15)4Cl4]Z = 2
Mr = 1086.96Mo Kα radiation
Tetragonal, I4µ = 1.63 mm1
a = 12.0733 (8) ÅT = 133 K
c = 14.9611 (15) Å0.30 × 0.22 × 0.20 mm
V = 2180.8 (3) Å3
Data collection top
Bruker SMART 1000 CCD
diffractometer
3314 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 1998)
3068 reflections with I > 2σ(I)
Tmin = 0.530, Tmax = 0.736Rint = 0.034
13332 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.024H-atom parameters constrained
wR(F2) = 0.049Δρmax = 0.84 e Å3
S = 1.07Δρmin = 0.33 e Å3
3314 reflectionsAbsolute structure: Flack (1983), 1573 Friedel pairs
115 parametersAbsolute structure parameter: 0.43 (3)
0 restraints
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
xyzUiso*/Ueq
Ru0.418223 (15)0.864161 (15)0.661262 (12)0.01407 (5)
C10.4531 (2)0.7131 (2)0.59544 (18)0.0208 (5)
C20.4159 (2)0.7947 (2)0.53127 (18)0.0231 (5)
C30.3056 (2)0.8280 (2)0.55638 (18)0.0223 (5)
C40.2743 (2)0.7683 (2)0.63523 (18)0.0220 (5)
C50.3659 (2)0.69705 (19)0.6597 (2)0.0205 (5)
C60.5628 (3)0.6547 (3)0.5945 (2)0.0344 (7)
H6A0.57720.62280.65350.041*
H6B0.62140.70770.57950.041*
H6C0.56130.59550.54960.041*
C70.4806 (3)0.8323 (3)0.4508 (2)0.0405 (8)
H7A0.47300.77750.40290.049*
H7B0.55890.84000.46690.049*
H7C0.45190.90390.43030.049*
C80.2339 (3)0.9097 (3)0.5071 (2)0.0447 (9)
H8A0.18930.87050.46240.054*
H8B0.28090.96450.47710.054*
H8C0.18490.94730.54950.054*
C90.1638 (2)0.7708 (3)0.6811 (2)0.0391 (8)
H9A0.12910.84330.67180.047*
H9B0.17390.75790.74520.047*
H9C0.11610.71280.65610.047*
C100.3684 (3)0.6195 (2)0.7381 (2)0.0333 (7)
H10A0.33440.54880.72120.040*
H10B0.32700.65210.78790.040*
H10C0.44530.60690.75640.040*
Cl0.38208 (4)1.06982 (5)0.67020 (3)0.01539 (10)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ru0.01418 (10)0.01413 (9)0.01390 (7)0.00059 (7)0.00012 (8)0.00179 (8)
C10.0205 (13)0.0188 (13)0.0230 (13)0.0005 (10)0.0001 (10)0.0097 (10)
C20.0288 (14)0.0238 (14)0.0166 (11)0.0085 (11)0.0025 (10)0.0060 (10)
C30.0248 (14)0.0214 (13)0.0208 (12)0.0013 (10)0.0061 (10)0.0066 (10)
C40.0173 (12)0.0229 (13)0.0258 (13)0.0043 (9)0.0012 (9)0.0082 (10)
C50.0264 (12)0.0163 (11)0.0188 (11)0.0017 (8)0.0010 (11)0.0056 (11)
C60.0236 (15)0.0338 (17)0.0459 (19)0.0055 (12)0.0031 (13)0.0193 (14)
C70.060 (2)0.0366 (18)0.0250 (16)0.0154 (16)0.0137 (15)0.0080 (13)
C80.052 (2)0.0400 (19)0.0420 (19)0.0067 (16)0.0282 (17)0.0007 (16)
C90.0246 (15)0.0455 (19)0.047 (2)0.0093 (13)0.0071 (13)0.0194 (15)
C100.054 (2)0.0184 (14)0.0277 (15)0.0075 (12)0.0030 (14)0.0014 (11)
Cl0.0146 (2)0.0162 (2)0.0154 (2)0.00040 (17)0.0002 (2)0.0005 (2)
Geometric parameters (Å, º) top
Ru—C12.115 (3)Cl—Ruiii2.5349 (6)
Ru—C22.118 (3)Cl—Ruii2.5428 (6)
Ru—C32.122 (3)C6—H6A0.9800
Ru—C42.124 (3)C6—H6B0.9800
Ru—C52.114 (2)C6—H6C0.9800
Ru—Cl2.5245 (6)C7—H7A0.9800
Ru—Cli2.5350 (6)C7—H7B0.9800
Ru—Clii2.5427 (6)C7—H7C0.9800
C1—C51.439 (4)C8—H8A0.9800
C1—C21.447 (4)C8—H8B0.9800
C1—C61.500 (4)C8—H8C0.9800
C2—C31.440 (4)C9—H9A0.9800
C2—C71.504 (4)C9—H9B0.9800
C3—C41.433 (4)C9—H9C0.9800
C3—C81.506 (4)C10—H10A0.9800
C4—C51.448 (4)C10—H10B0.9800
C4—C91.500 (4)C10—H10C0.9800
C5—C101.502 (4)
C5—Ru—C139.77 (10)C3—C4—C5107.7 (2)
C5—Ru—C266.93 (11)C3—C4—C9127.0 (3)
C1—Ru—C239.99 (11)C5—C4—C9125.1 (3)
C5—Ru—C366.64 (10)C3—C4—Ru70.17 (15)
C1—Ru—C366.76 (11)C5—C4—Ru69.66 (14)
C2—Ru—C339.73 (11)C9—C4—Ru129.3 (2)
C5—Ru—C439.95 (10)C1—C5—C4108.1 (2)
C1—Ru—C466.90 (10)C1—C5—C10126.2 (3)
C2—Ru—C466.75 (10)C4—C5—C10125.7 (3)
C3—Ru—C439.45 (11)C1—C5—Ru70.13 (14)
C5—Ru—Cl152.55 (7)C4—C5—Ru70.39 (14)
C1—Ru—Cl155.12 (8)C10—C5—Ru125.47 (19)
C2—Ru—Cl115.82 (8)Ru—Cl—Ruiii97.092 (19)
C3—Ru—Cl97.53 (7)Ru—Cl—Ruii98.145 (18)
C4—Ru—Cl113.84 (8)Ruiii—Cl—Ruii96.627 (19)
C5—Ru—Cli96.30 (8)C1—C6—H6A109.5
C1—Ru—Cli121.70 (8)C1—C6—H6B109.5
C2—Ru—Cli161.43 (8)H6A—C6—H6B109.5
C3—Ru—Cli142.17 (8)C1—C6—H6C109.5
C4—Ru—Cli105.99 (7)H6A—C6—H6C109.5
Cl—Ru—Cli82.715 (19)H6B—C6—H6C109.5
C5—Ru—Clii125.67 (7)C2—C7—H7A109.5
C1—Ru—Clii96.09 (8)C2—C7—H7B109.5
C2—Ru—Clii100.65 (7)H7A—C7—H7B109.5
C3—Ru—Clii135.31 (8)C2—C7—H7C109.5
C4—Ru—Clii162.99 (7)H7A—C7—H7C109.5
Cl—Ru—Clii81.533 (18)H7B—C7—H7C109.5
Cli—Ru—Clii82.354 (19)C3—C8—H8A109.5
C5—C1—C2107.9 (2)C3—C8—H8B109.5
C5—C1—C6126.1 (3)H8A—C8—H8B109.5
C2—C1—C6126.0 (3)C3—C8—H8C109.5
C5—C1—Ru70.10 (13)H8A—C8—H8C109.5
C2—C1—Ru70.12 (15)H8B—C8—H8C109.5
C6—C1—Ru125.85 (19)C4—C9—H9A109.5
C3—C2—C1107.6 (2)C4—C9—H9B109.5
C3—C2—C7127.2 (3)H9A—C9—H9B109.5
C1—C2—C7125.1 (3)C4—C9—H9C109.5
C3—C2—Ru70.27 (15)H9A—C9—H9C109.5
C1—C2—Ru69.89 (14)H9B—C9—H9C109.5
C7—C2—Ru127.5 (2)C5—C10—H10A109.5
C4—C3—C2108.6 (2)C5—C10—H10B109.5
C4—C3—C8125.5 (3)H10A—C10—H10B109.5
C2—C3—C8125.9 (3)C5—C10—H10C109.5
C4—C3—Ru70.37 (15)H10A—C10—H10C109.5
C2—C3—Ru70.00 (15)H10B—C10—H10C109.5
C8—C3—Ru126.5 (2)
C2—Ru—C1—C5118.6 (2)Ru—C3—C4—C559.79 (17)
C3—Ru—C1—C580.87 (17)C2—C3—C4—C9175.4 (3)
C4—Ru—C1—C537.79 (16)C8—C3—C4—C93.3 (4)
Cl—Ru—C1—C5134.95 (17)Ru—C3—C4—C9124.8 (3)
Cli—Ru—C1—C557.29 (17)C2—C3—C4—Ru59.79 (18)
Clii—Ru—C1—C5142.05 (14)C8—C3—C4—Ru121.5 (3)
C5—Ru—C1—C2118.6 (2)C5—Ru—C4—C3118.6 (2)
C3—Ru—C1—C237.76 (16)C1—Ru—C4—C380.99 (17)
C4—Ru—C1—C280.84 (17)C2—Ru—C4—C337.32 (15)
Cl—Ru—C1—C216.3 (3)Cl—Ru—C4—C371.86 (15)
Cli—Ru—C1—C2175.93 (12)Cli—Ru—C4—C3160.85 (13)
Clii—Ru—C1—C299.32 (14)Clii—Ru—C4—C381.5 (3)
C5—Ru—C1—C6120.8 (3)C1—Ru—C4—C537.62 (16)
C2—Ru—C1—C6120.6 (3)C2—Ru—C4—C581.29 (17)
C3—Ru—C1—C6158.4 (3)C3—Ru—C4—C5118.6 (2)
C4—Ru—C1—C6158.6 (3)Cl—Ru—C4—C5169.53 (13)
Cl—Ru—C1—C6104.3 (3)Cli—Ru—C4—C580.54 (15)
Cli—Ru—C1—C663.5 (3)Clii—Ru—C4—C537.1 (4)
Clii—Ru—C1—C621.3 (3)C5—Ru—C4—C9119.3 (4)
C5—C1—C2—C30.3 (3)C1—Ru—C4—C9157.0 (3)
C6—C1—C2—C3179.1 (2)C2—Ru—C4—C9159.4 (3)
Ru—C1—C2—C360.42 (18)C3—Ru—C4—C9122.1 (3)
C5—C1—C2—C7177.5 (3)Cl—Ru—C4—C950.2 (3)
C6—C1—C2—C71.9 (4)Cli—Ru—C4—C938.8 (3)
Ru—C1—C2—C7122.3 (3)Clii—Ru—C4—C9156.4 (2)
C5—C1—C2—Ru60.17 (17)C2—C1—C5—C40.3 (3)
C6—C1—C2—Ru120.5 (3)C6—C1—C5—C4179.1 (2)
C5—Ru—C2—C380.69 (16)Ru—C1—C5—C460.43 (17)
C1—Ru—C2—C3118.3 (2)C2—C1—C5—C10179.8 (2)
C4—Ru—C2—C337.07 (16)C6—C1—C5—C100.4 (4)
Cl—Ru—C2—C369.24 (15)Ru—C1—C5—C10120.0 (3)
Cli—Ru—C2—C3107.4 (2)C2—C1—C5—Ru60.18 (17)
Clii—Ru—C2—C3154.91 (14)C6—C1—C5—Ru120.5 (3)
C5—Ru—C2—C137.61 (15)C3—C4—C5—C10.2 (3)
C3—Ru—C2—C1118.3 (2)C9—C4—C5—C1175.4 (2)
C4—Ru—C2—C181.24 (17)Ru—C4—C5—C160.27 (17)
Cl—Ru—C2—C1172.45 (13)C3—C4—C5—C10179.7 (2)
Cli—Ru—C2—C110.9 (3)C9—C4—C5—C104.2 (4)
Clii—Ru—C2—C186.78 (15)Ru—C4—C5—C10120.2 (3)
C5—Ru—C2—C7157.0 (3)C3—C4—C5—Ru60.12 (18)
C1—Ru—C2—C7119.4 (4)C9—C4—C5—Ru124.4 (3)
C3—Ru—C2—C7122.3 (3)C2—Ru—C5—C137.81 (16)
C4—Ru—C2—C7159.3 (3)C3—Ru—C5—C181.21 (18)
Cl—Ru—C2—C753.0 (3)C4—Ru—C5—C1118.6 (2)
Cli—Ru—C2—C7130.4 (3)Cl—Ru—C5—C1139.76 (16)
Clii—Ru—C2—C732.6 (3)Cli—Ru—C5—C1133.92 (15)
C1—C2—C3—C40.2 (3)Clii—Ru—C5—C148.83 (18)
C7—C2—C3—C4177.3 (3)C1—Ru—C5—C4118.6 (2)
Ru—C2—C3—C460.02 (18)C2—Ru—C5—C480.82 (17)
C1—C2—C3—C8178.6 (3)C3—Ru—C5—C437.42 (16)
C7—C2—C3—C81.4 (5)Cl—Ru—C5—C421.1 (3)
Ru—C2—C3—C8121.3 (3)Cli—Ru—C5—C4107.45 (15)
C1—C2—C3—Ru60.18 (18)Clii—Ru—C5—C4167.46 (12)
C7—C2—C3—Ru122.6 (3)C1—Ru—C5—C10121.0 (3)
C5—Ru—C3—C437.88 (15)C2—Ru—C5—C10158.8 (3)
C1—Ru—C3—C481.36 (17)C3—Ru—C5—C10157.8 (3)
C2—Ru—C3—C4119.4 (2)C4—Ru—C5—C10120.4 (3)
Cl—Ru—C3—C4118.75 (14)Cl—Ru—C5—C1099.3 (3)
Cli—Ru—C3—C430.9 (2)Cli—Ru—C5—C1013.0 (2)
Clii—Ru—C3—C4155.70 (12)Clii—Ru—C5—C1072.1 (3)
C5—Ru—C3—C281.48 (16)C5—Ru—Cl—Ruiii81.26 (18)
C1—Ru—C3—C238.00 (16)C1—Ru—Cl—Ruiii177.91 (18)
C4—Ru—C3—C2119.4 (2)C2—Ru—Cl—Ruiii170.52 (8)
Cl—Ru—C3—C2121.89 (14)C3—Ru—Cl—Ruiii133.45 (8)
Cli—Ru—C3—C2150.30 (13)C4—Ru—Cl—Ruiii95.92 (8)
Clii—Ru—C3—C236.34 (19)Cli—Ru—Cl—Ruiii8.388 (18)
C5—Ru—C3—C8158.1 (3)Clii—Ru—Cl—Ruiii91.693 (16)
C1—Ru—C3—C8158.4 (3)C5—Ru—Cl—Ruii179.04 (17)
C2—Ru—C3—C8120.4 (4)C1—Ru—Cl—Ruii80.13 (18)
C4—Ru—C3—C8120.2 (3)C2—Ru—Cl—Ruii91.70 (8)
Cl—Ru—C3—C81.5 (3)C3—Ru—Cl—Ruii128.78 (8)
Cli—Ru—C3—C889.3 (3)C4—Ru—Cl—Ruii166.30 (8)
Clii—Ru—C3—C884.1 (3)Cli—Ru—Cl—Ruii89.387 (18)
C2—C3—C4—C50.0 (3)Clii—Ru—Cl—Ruii6.08 (2)
C8—C3—C4—C5178.7 (3)
Symmetry codes: (i) y+3/2, x+1/2, z+3/2; (ii) x+1, y+2, z; (iii) y1/2, x+3/2, z+3/2.

Experimental details

Crystal data
Chemical formula[Ru4(C10H15)4Cl4]
Mr1086.96
Crystal system, space groupTetragonal, I4
Temperature (K)133
a, c (Å)12.0733 (8), 14.9611 (15)
V3)2180.8 (3)
Z2
Radiation typeMo Kα
µ (mm1)1.63
Crystal size (mm)0.30 × 0.22 × 0.20
Data collection
DiffractometerBruker SMART 1000 CCD
Absorption correctionMulti-scan
(SADABS; Bruker, 1998)
Tmin, Tmax0.530, 0.736
No. of measured, independent and
observed [I > 2σ(I)] reflections
13332, 3314, 3068
Rint0.034
(sin θ/λ)max1)0.715
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.024, 0.049, 1.07
No. of reflections3314
No. of parameters115
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.84, 0.33
Absolute structureFlack (1983), 1573 Friedel pairs
Absolute structure parameter0.43 (3)

Computer programs: SMART (Bruker, 1998), SAINT (Bruker, 1998), SAINT, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), XP (Siemens, 1994), SHELXL97.

Selected geometric parameters (Å, º) top
Ru—C12.115 (3)Ru—C52.114 (2)
Ru—C22.118 (3)Ru—Cl2.5245 (6)
Ru—C32.122 (3)Ru—Cli2.5350 (6)
Ru—C42.124 (3)Ru—Clii2.5427 (6)
Cl—Ru—Cli82.715 (19)Ru—Cl—Ruiii97.092 (19)
Cl—Ru—Clii81.533 (18)Ru—Cl—Ruii98.145 (18)
Cli—Ru—Clii82.354 (19)Ruiii—Cl—Ruii96.627 (19)
Symmetry codes: (i) y+3/2, x+1/2, z+3/2; (ii) x+1, y+2, z; (iii) y1/2, x+3/2, z+3/2.
 

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