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In the cation of the title compound, [Rh2Cl3(C10H15)2]BF4, two Rh(η5-C5Me5) fragments are linked by three bridging Cl atoms. Each rhodium center has a pseudo-octahedral coordination geometry, with a C5Me5 group occupying three positions and three Cl atoms completing the coordination. The average Rh—Cl bond length is 2.450 Å and the average Rh—Cl—Rh bond angle is 81.6°.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804007226/cf6332sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804007226/cf6332Isup2.hkl
Contains datablock I

CCDC reference: 238686

Key indicators

  • Single-crystal X-ray study
  • T = 296 K
  • Mean [sigma](C-C) = 0.007 Å
  • R factor = 0.042
  • wR factor = 0.084
  • Data-to-parameter ratio = 20.4

checkCIF/PLATON results

No syntax errors found



Alert level A PLAT029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.89
Alert level B REFLT03_ALERT_3_B Reflection count < 90% complete (theta max?) From the CIF: _diffrn_reflns_theta_max 28.33 From the CIF: _diffrn_reflns_theta_full 0.00 From the CIF: _reflns_number_total 5533 TEST2: Reflns within _diffrn_reflns_theta_max Count of symmetry unique reflns 6183 Completeness (_total/calc) 89.49%
Alert level C PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ? PLAT380_ALERT_4_C Incorrectly Oriented X(sp2)-Methyl Moiety ...... C8 PLAT380_ALERT_4_C Incorrectly Oriented X(sp2)-Methyl Moiety ...... C20
1 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 3 ALERT level C = Check and explain 0 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 2 ALERT type 3 Indicator that the structure quality may be low 3 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
[Rh2Cl3(C10H15)2]BF4Z = 2
Mr = 669.42F(000) = 664
Triclinic, P1Dx = 1.791 Mg m3
a = 8.1768 (16) ÅMo Kα radiation, λ = 0.71073 Å
b = 11.858 (2) ÅCell parameters from 1788 reflections
c = 14.007 (3) Åθ = 2.5–27.9°
α = 67.534 (3)°µ = 1.69 mm1
β = 82.032 (3)°T = 296 K
γ = 89.421 (4)°Block, orange
V = 1241.6 (4) Å30.35 × 0.30 × 0.28 mm
Data collection top
Bruker SMART CCD area-detector
diffractometer
5533 independent reflections
Radiation source: fine-focus sealed tube3807 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.038
φ and ω scansθmax = 28.3°, θmin = 1.6°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1997a)
h = 1010
Tmin = 0.542, Tmax = 0.629k = 1015
7407 measured reflectionsl = 1817
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)] = 0.042Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.084H-atom parameters constrained
S = 0.96 w = 1/[σ2(Fo2)]
5533 reflections(Δ/σ)max < 0.001
271 parametersΔρmax = 0.92 e Å3
0 restraintsΔρmin = 0.97 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
Rh10.20814 (5)0.14363 (4)0.23180 (3)0.01512 (11)
Rh20.37519 (5)0.10983 (4)0.25781 (3)0.01539 (11)
Cl10.13945 (15)0.01536 (12)0.17194 (10)0.0209 (3)
Cl20.25000 (18)0.03223 (13)0.38781 (10)0.0297 (3)
Cl30.49262 (14)0.10214 (12)0.17235 (10)0.0194 (3)
C10.1998 (6)0.3305 (4)0.1333 (4)0.0160 (11)
C20.2495 (6)0.3193 (5)0.2321 (4)0.0196 (12)
C30.1159 (6)0.2562 (5)0.3130 (4)0.0166 (11)
C40.0118 (6)0.2260 (5)0.2654 (4)0.0175 (11)
C50.0391 (6)0.2752 (4)0.1542 (4)0.0170 (11)
C60.3012 (7)0.3934 (5)0.0296 (4)0.0264 (13)
H6A0.27350.47750.00110.040*
H6B0.27960.35450.01650.040*
H6C0.41630.38880.03730.040*
C70.4081 (6)0.3690 (5)0.2454 (4)0.0279 (14)
H7A0.39420.45050.24280.042*
H7B0.49310.37020.19030.042*
H7C0.43910.31810.31160.042*
C80.1134 (7)0.2275 (5)0.4263 (4)0.0247 (13)
H8A0.06560.29290.44330.037*
H8B0.22440.21790.44240.037*
H8C0.04880.15310.46630.037*
C90.1764 (6)0.1630 (5)0.3220 (4)0.0234 (13)
H9A0.25410.22290.32580.035*
H9B0.16380.10790.39130.035*
H9C0.21610.11800.28490.035*
C100.0619 (7)0.2672 (5)0.0766 (4)0.0255 (13)
H10A0.12770.33760.05460.038*
H10B0.13290.19460.10770.038*
H10C0.00970.26430.01720.038*
C110.5553 (6)0.1943 (5)0.1860 (4)0.0184 (12)
C120.3981 (6)0.2535 (5)0.2023 (4)0.0183 (11)
C130.3376 (6)0.3009 (5)0.3128 (4)0.0175 (11)
C140.4601 (6)0.2734 (5)0.3638 (4)0.0177 (11)
C150.5947 (6)0.2056 (5)0.2866 (4)0.0182 (11)
C160.6654 (6)0.1312 (5)0.0846 (4)0.0258 (13)
H16A0.73640.18910.06960.039*
H16B0.73120.06750.08940.039*
H16C0.59910.09650.02980.039*
C170.3105 (7)0.2662 (5)0.1207 (4)0.0278 (14)
H17A0.34330.33880.10980.042*
H17B0.33820.19630.05660.042*
H17C0.19330.27150.14280.042*
C180.1801 (6)0.3748 (5)0.3651 (4)0.0276 (14)
H18A0.19950.45990.38230.041*
H18B0.09840.35030.31890.041*
H18C0.14130.36180.42790.041*
C190.4529 (7)0.3085 (5)0.4784 (4)0.0278 (13)
H19A0.49900.38690.50820.042*
H19B0.33990.31240.50980.042*
H19C0.51510.24870.49110.042*
C200.7495 (6)0.1606 (5)0.3069 (4)0.0275 (13)
H20A0.82950.22240.31730.041*
H20B0.72710.14210.36830.041*
H20C0.79210.08820.24820.041*
B10.8133 (8)0.5211 (7)0.2550 (5)0.0297 (16)
F10.6539 (4)0.5380 (3)0.2912 (3)0.0448 (10)
F20.8939 (4)0.4538 (3)0.3385 (2)0.0331 (8)
F30.8075 (5)0.4559 (3)0.1913 (3)0.0444 (10)
F40.8956 (4)0.6331 (3)0.1992 (3)0.0426 (9)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Rh10.0131 (2)0.0157 (2)0.0140 (2)0.00076 (16)0.00170 (16)0.00412 (17)
Rh20.0137 (2)0.0158 (2)0.0137 (2)0.00077 (16)0.00272 (16)0.00392 (17)
Cl10.0131 (6)0.0201 (7)0.0307 (8)0.0018 (5)0.0029 (5)0.0111 (6)
Cl20.0423 (9)0.0267 (8)0.0131 (7)0.0107 (6)0.0039 (6)0.0030 (6)
Cl30.0115 (6)0.0193 (7)0.0253 (7)0.0024 (5)0.0012 (5)0.0075 (6)
C10.019 (3)0.009 (3)0.013 (3)0.004 (2)0.003 (2)0.002 (2)
C20.017 (3)0.019 (3)0.023 (3)0.002 (2)0.001 (2)0.010 (2)
C30.020 (3)0.015 (3)0.013 (3)0.002 (2)0.001 (2)0.003 (2)
C40.019 (3)0.016 (3)0.019 (3)0.005 (2)0.005 (2)0.008 (2)
C50.018 (3)0.011 (3)0.017 (3)0.004 (2)0.002 (2)0.001 (2)
C60.030 (3)0.018 (3)0.021 (3)0.003 (2)0.006 (2)0.001 (2)
C70.021 (3)0.022 (3)0.039 (4)0.004 (2)0.003 (3)0.011 (3)
C80.025 (3)0.029 (3)0.018 (3)0.004 (2)0.003 (2)0.007 (3)
C90.015 (3)0.032 (4)0.021 (3)0.006 (2)0.003 (2)0.010 (3)
C100.029 (3)0.025 (3)0.019 (3)0.003 (2)0.004 (2)0.005 (3)
C110.021 (3)0.015 (3)0.018 (3)0.005 (2)0.000 (2)0.005 (2)
C120.020 (3)0.013 (3)0.021 (3)0.003 (2)0.001 (2)0.007 (2)
C130.016 (3)0.014 (3)0.019 (3)0.004 (2)0.001 (2)0.003 (2)
C140.017 (3)0.014 (3)0.015 (3)0.004 (2)0.002 (2)0.000 (2)
C150.017 (3)0.013 (3)0.022 (3)0.003 (2)0.001 (2)0.005 (2)
C160.018 (3)0.036 (4)0.021 (3)0.001 (2)0.008 (2)0.012 (3)
C170.029 (3)0.030 (4)0.031 (3)0.001 (3)0.006 (3)0.018 (3)
C180.023 (3)0.026 (3)0.030 (3)0.012 (2)0.004 (2)0.009 (3)
C190.027 (3)0.027 (3)0.020 (3)0.000 (3)0.003 (2)0.000 (3)
C200.019 (3)0.027 (3)0.031 (3)0.001 (2)0.000 (2)0.007 (3)
B10.030 (4)0.026 (4)0.028 (4)0.007 (3)0.002 (3)0.006 (3)
F10.025 (2)0.035 (2)0.068 (3)0.0050 (16)0.0039 (18)0.016 (2)
F20.035 (2)0.031 (2)0.0274 (19)0.0001 (15)0.0075 (15)0.0035 (16)
F30.059 (3)0.045 (3)0.038 (2)0.0163 (19)0.0164 (18)0.0233 (19)
F40.036 (2)0.035 (2)0.040 (2)0.0121 (17)0.0032 (17)0.0030 (17)
Geometric parameters (Å, º) top
Rh1—C22.116 (5)C9—H9A0.960
Rh1—C42.119 (5)C9—H9B0.960
Rh1—C12.123 (5)C9—H9C0.960
Rh1—C32.132 (5)C10—H10A0.960
Rh1—C52.146 (5)C10—H10B0.960
Rh1—Cl12.4358 (13)C10—H10C0.960
Rh1—Cl22.4396 (15)C11—C121.418 (6)
Rh1—Cl32.4697 (13)C11—C151.446 (7)
Rh2—C132.106 (5)C11—C161.494 (6)
Rh2—C152.117 (5)C12—C131.444 (6)
Rh2—C122.123 (5)C12—C171.484 (7)
Rh2—C142.123 (5)C13—C141.416 (7)
Rh2—C112.125 (5)C13—C181.495 (6)
Rh2—Cl22.4403 (13)C14—C151.432 (6)
Rh2—Cl12.4468 (14)C14—C191.488 (6)
Rh2—Cl32.4705 (13)C15—C201.482 (6)
C1—C51.416 (6)C16—H16A0.960
C1—C21.454 (7)C16—H16B0.960
C1—C61.484 (6)C16—H16C0.960
C2—C31.436 (6)C17—H17A0.960
C2—C71.493 (6)C17—H17B0.960
C3—C41.430 (7)C17—H17C0.960
C3—C81.488 (6)C18—H18A0.960
C4—C51.439 (6)C18—H18B0.960
C4—C91.506 (6)C18—H18C0.960
C5—C101.484 (7)C19—H19A0.960
C6—H6A0.960C19—H19B0.960
C6—H6B0.960C19—H19C0.960
C6—H6C0.960C20—H20A0.960
C7—H7A0.960C20—H20B0.960
C7—H7B0.960C20—H20C0.960
C7—H7C0.960B1—F11.373 (7)
C8—H8A0.960B1—F41.381 (7)
C8—H8B0.960B1—F21.389 (8)
C8—H8C0.960B1—F31.392 (7)
C2—Rh1—C466.43 (19)H6A—C6—H6C109.5
C2—Rh1—C140.14 (18)H6B—C6—H6C109.5
C4—Rh1—C166.14 (19)C2—C7—H7A109.5
C2—Rh1—C339.51 (17)C2—C7—H7B109.5
C4—Rh1—C339.31 (18)H7A—C7—H7B109.5
C1—Rh1—C366.37 (18)C2—C7—H7C109.5
C2—Rh1—C566.08 (19)H7A—C7—H7C109.5
C4—Rh1—C539.44 (17)H7B—C7—H7C109.5
C1—Rh1—C538.75 (17)C3—C8—H8A109.5
C3—Rh1—C565.77 (19)C3—C8—H8B109.5
C2—Rh1—Cl1160.24 (15)H8A—C8—H8B109.5
C4—Rh1—Cl1108.98 (14)C3—C8—H8C109.5
C1—Rh1—Cl1120.10 (14)H8A—C8—H8C109.5
C3—Rh1—Cl1145.65 (14)H8B—C8—H8C109.5
C5—Rh1—Cl197.79 (14)C4—C9—H9A109.5
C2—Rh1—Cl2117.46 (15)C4—C9—H9B109.5
C4—Rh1—Cl2108.77 (14)H9A—C9—H9B109.5
C1—Rh1—Cl2157.60 (14)C4—C9—H9C109.5
C3—Rh1—Cl295.53 (14)H9A—C9—H9C109.5
C5—Rh1—Cl2146.59 (13)H9B—C9—H9C109.5
Cl1—Rh1—Cl282.30 (5)C5—C10—H10A109.5
C2—Rh1—Cl399.87 (14)C5—C10—H10B109.5
C4—Rh1—Cl3165.35 (14)H10A—C10—H10B109.5
C1—Rh1—Cl3100.22 (13)C5—C10—H10C109.5
C3—Rh1—Cl3131.77 (14)H10A—C10—H10C109.5
C5—Rh1—Cl3131.58 (13)H10B—C10—H10C109.5
Cl1—Rh1—Cl382.07 (4)C12—C11—C15107.9 (4)
Cl2—Rh1—Cl381.70 (5)C12—C11—C16127.6 (5)
C13—Rh2—C1566.41 (19)C15—C11—C16124.4 (5)
C13—Rh2—C1239.93 (17)C12—C11—Rh270.4 (3)
C15—Rh2—C1266.19 (19)C15—C11—Rh269.8 (3)
C13—Rh2—C1439.11 (18)C16—C11—Rh2125.5 (4)
C15—Rh2—C1439.49 (18)C11—C12—C13108.2 (4)
C12—Rh2—C1466.0 (2)C11—C12—C17126.3 (4)
C13—Rh2—C1166.44 (19)C13—C12—C17125.5 (5)
C15—Rh2—C1139.85 (18)C11—C12—Rh270.6 (3)
C12—Rh2—C1139.00 (17)C13—C12—Rh269.4 (3)
C14—Rh2—C1166.21 (19)C17—C12—Rh2126.2 (4)
C13—Rh2—Cl2110.98 (13)C14—C13—C12107.9 (4)
C15—Rh2—Cl2117.32 (14)C14—C13—C18125.8 (5)
C12—Rh2—Cl2149.36 (14)C12—C13—C18126.2 (5)
C14—Rh2—Cl296.96 (14)C14—C13—Rh271.1 (3)
C11—Rh2—Cl2157.02 (15)C12—C13—Rh270.7 (3)
C13—Rh2—Cl1108.26 (14)C18—C13—Rh2127.5 (4)
C15—Rh2—Cl1160.62 (14)C13—C14—C15108.6 (4)
C12—Rh2—Cl197.43 (15)C13—C14—C19126.5 (4)
C14—Rh2—Cl1144.66 (14)C15—C14—C19124.9 (5)
C11—Rh2—Cl1120.80 (15)C13—C14—Rh269.8 (3)
Cl2—Rh2—Cl182.06 (5)C15—C14—Rh270.0 (3)
C13—Rh2—Cl3164.42 (13)C19—C14—Rh2126.1 (4)
C15—Rh2—Cl3100.08 (14)C14—C15—C11107.4 (4)
C12—Rh2—Cl3128.76 (14)C14—C15—C20126.1 (5)
C14—Rh2—Cl3133.22 (14)C11—C15—C20126.4 (5)
C11—Rh2—Cl398.31 (14)C14—C15—Rh270.5 (3)
Cl2—Rh2—Cl381.67 (5)C11—C15—Rh270.3 (3)
Cl1—Rh2—Cl381.83 (4)C20—C15—Rh2126.7 (4)
Rh1—Cl1—Rh281.94 (4)C11—C16—H16A109.5
Rh1—Cl2—Rh282.00 (4)C11—C16—H16B109.5
Rh1—Cl3—Rh280.79 (4)H16A—C16—H16B109.5
C5—C1—C2108.1 (4)C11—C16—H16C109.5
C5—C1—C6127.3 (5)H16A—C16—H16C109.5
C2—C1—C6124.5 (5)H16B—C16—H16C109.5
C5—C1—Rh171.5 (3)C12—C17—H17A109.5
C2—C1—Rh169.7 (3)C12—C17—H17B109.5
C6—C1—Rh1126.0 (4)H17A—C17—H17B109.5
C3—C2—C1107.3 (4)C12—C17—H17C109.5
C3—C2—C7126.8 (5)H17A—C17—H17C109.5
C1—C2—C7125.8 (4)H17B—C17—H17C109.5
C3—C2—Rh170.8 (3)C13—C18—H18A109.5
C1—C2—Rh170.2 (3)C13—C18—H18B109.5
C7—C2—Rh1125.9 (4)H18A—C18—H18B109.5
C4—C3—C2108.1 (4)C13—C18—H18C109.5
C4—C3—C8126.6 (4)H18A—C18—H18C109.5
C2—C3—C8125.3 (5)H18B—C18—H18C109.5
C4—C3—Rh169.9 (3)C14—C19—H19A109.5
C2—C3—Rh169.6 (3)C14—C19—H19B109.5
C8—C3—Rh1125.9 (4)H19A—C19—H19B109.5
C3—C4—C5108.1 (4)C14—C19—H19C109.5
C3—C4—C9125.5 (4)H19A—C19—H19C109.5
C5—C4—C9126.3 (4)H19B—C19—H19C109.5
C3—C4—Rh170.8 (3)C15—C20—H20A109.5
C5—C4—Rh171.3 (3)C15—C20—H20B109.5
C9—C4—Rh1127.4 (4)H20A—C20—H20B109.5
C1—C5—C4108.3 (4)C15—C20—H20C109.5
C1—C5—C10126.9 (4)H20A—C20—H20C109.5
C4—C5—C10124.8 (4)H20B—C20—H20C109.5
C1—C5—Rh169.7 (3)F1—B1—F4109.7 (6)
C4—C5—Rh169.3 (3)F1—B1—F2109.7 (5)
C10—C5—Rh1126.3 (4)F4—B1—F2110.1 (5)
C1—C6—H6A109.5F1—B1—F3108.2 (5)
C1—C6—H6B109.5F4—B1—F3110.3 (5)
H6A—C6—H6B109.5F2—B1—F3108.9 (6)
C1—C6—H6C109.5
 

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