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Acta Crystallogr Sect E Struct Rep Online. 2010 November 1; 66(Pt 11): m1370.
Published online 2010 October 9. doi:  10.1107/S1600536810039577
PMCID: PMC3008980

(+)-{1,2-Bis[(2R,5R)-2,5-diethyl­phospho­lan-1-yl]ethane-κ 2 P,P′}(η 4-cyclo­octa-1,5-diene)rhodium(I) tetra­fluoridoborate

Abstract

The title compound, [Rh(C8H12)(C18H36P2)]BF4, exhibits a rhodium(I) complex cation with a bidentate bis­phosphine ligand and a bidentate η 2,η 2-coordinated cyclo­octa-1,5-diene ligand. The ligands form a slightly distorted square-planar coordination environment for the Rh(I) atom. An intra­molecular P–Rh–P bite angle of 83.91 (2)° is observed. The dihedral angle between the P—Rh—P and the X—Rh—X planes (X is the centroid of a double bond) is 14.0 (1)°. The BF4 anion is disordered over two positions in a 0.515 (7):0.485 (7) ratio.

Related literature

For general synthetic aspects and different related structures of cationic rhodium bis­phosphine diolefin complexes, see: Schulz et al. (2010 [triangle]) and references cited therein. For applications of the Et-BPE ligand {Et-BPE (1,2-bis[(2R,5R)-2,5-diethylphospholan-1-yl]ethane)} in catalytic reactions, see: Axtell et al. (2005 [triangle]); Jerphagnon et al. (2003 [triangle]); Burk et al. (1998 [triangle]). For related structures, see: Burk et al. (1990 [triangle]); Drexler et al. (2001 [triangle], 2004 [triangle]).

An external file that holds a picture, illustration, etc.
Object name is e-66-m1370-scheme1.jpg

Experimental

Crystal data

  • [Rh(C8H12)(C18H36P2)]BF4
  • M r = 612.32
  • Orthorhombic, An external file that holds a picture, illustration, etc.
Object name is e-66-m1370-efi1.jpg
  • a = 8.8374 (18) Å
  • b = 16.218 (3) Å
  • c = 19.946 (4) Å
  • V = 2858.7 (10) Å3
  • Z = 4
  • Mo Kα radiation
  • μ = 0.75 mm−1
  • T = 200 K
  • 0.50 × 0.43 × 0.40 mm

Data collection

  • STOE IPDS 2 diffractometer
  • Absorption correction: numerical (X-SHAPE; Stoe & Cie, 2005) T min = 0.728, T max = 0.858
  • 36650 measured reflections
  • 6075 independent reflections
  • 5779 reflections with I > 2σ(I)
  • R int = 0.035

Refinement

  • R[F 2 > 2σ(F 2)] = 0.027
  • wR(F 2) = 0.073
  • S = 1.06
  • 6075 reflections
  • 305 parameters
  • 21 restraints
  • H-atom parameters constrained
  • Δρmax = 0.95 e Å−3
  • Δρmin = −0.34 e Å−3
  • Absolute structure: Flack (1983 [triangle]), 2621 Friedel pairs
  • Flack parameter: −0.02 (2)

Data collection: X-AREA (Stoe & Cie, 2005) [triangle]; cell refinement: X-AREA [triangle]; data reduction: X-RED32 (Stoe & Cie, 2005) [triangle]; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 [triangle]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 [triangle]); molecular graphics: SHELXTL (Sheldrick, 2008 [triangle]); software used to prepare material for publication: SHELXTL.

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536810039577/si2281sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536810039577/si2281Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Acknowledgments

This work was supported by the Leibniz-Institut für Katalyse e. V. an der Universität Rostock.

supplementary crystallographic information

Comment

The geometry of the cation of the title compound is comparable with the three independent complexes described in Schulz et al. (2010): the dihedral angle between the planes P1,Rh1,P2 and X1,Rh1,X2 (X = centroid of the double bond) of 14.0 (1)° corresponds to those in the Me-BPE complexes (14.7 (1)°, 14.8 (1)° and 15.3 (1)°). Furthermore, the dihedral angle is not the value found for the corresponding Et-DuPhos complex [Rh((R,R)-Et-DuPhos)COD]BF4 (21.1 (1)°) (Drexler et al., 2001) or for the complex [Rh((R,R)-Me-BPE)COD]SbF6 (19.4°) (Burk et al., 1990; Drexler et al., 2004). The cationic rhodium bisphosphine diolefine complexes build up five-membered ring chelates with rhodium (Fig. 1). For the title compound the molecular structure shows a δ-conformation of the backbone of the bisphosphine. The COD is η2,η2-coordinated and is orientated in an anticlockwise twist manner. An intramolecular P1—Rh1—P2 angle of 83.91 (2)° is obtained. This is in the same range of corresponding complexes already described in the literature Schulz et al. (2010) and literature therein. The bonds Rh1—P1 and Rh1—P2 show bond lengths of 2.2754 (8) Å and 2.2702 (8) Å, respectively. Applications of the ligand Et-BPE in catalytic reactions are reported by Axtell et al. (2005); Jerphagnon et al. (2003) and Burk et al. (1998).

Experimental

By overlaying a solution of [Rh((R,R)-Et-BPE)COD)]BF4 in dichloromethane with MTBE (methyl-tert-butylether) red single crystals suitable for X-ray analysis are obtained. 31P NMR (CD2Cl2, 298 K, 162 MHz) [p.p.m.]: 73.5 (d, JP—Rh = 145.5 Hz).

Refinement

All non-hydrogen atoms are refined anisotropically, except not fully occupied fluorine atoms of the anion. All H atoms were placed in idealized positions with d(C—H) = 0.98(CH), 0.97 (CH2) and 0.96 (CH3) Å and refined using a riding model with Uiso(H) fixed at 1.5 Ueq(C) for CH3 and 1.2 Ueq(C) for CH2 and CH. The absolute configuration indicators 2R,5R for the title compound were determined by using 2621 Friedel pairs in the refinement. The Flack parameter at convergence was -0.02 (2).

Figures

Fig. 1.
Perspective view and numbering scheme of the cation [Rh((R,R)-Et-BPE)COD]+. All H atoms and the anion have been omitted for clarity. Thermal ellipsoids are drawn at the 30% probability level.

Crystal data

[Rh(C8H12)(C18H36P2)]BF4F(000) = 1280
Mr = 612.32Dx = 1.423 Mg m3
Orthorhombic, P212121Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2ac 2abCell parameters from 54003 reflections
a = 8.8374 (18) Åθ = 1.6–27.2°
b = 16.218 (3) ŵ = 0.75 mm1
c = 19.946 (4) ÅT = 200 K
V = 2858.7 (10) Å3Part of block, red
Z = 40.50 × 0.43 × 0.40 mm

Data collection

STOE IPDS 2 diffractometer6075 independent reflections
Radiation source: fine-focus sealed tube5779 reflections with I > 2σ(I)
graphiteRint = 0.035
Detector resolution: 6.67 pixels mm-1θmax = 26.8°, θmin = 1.6°
rotation method scansh = −11→11
Absorption correction: numerical (X-SHAPE; Stoe & Cie, 2005)k = −20→20
Tmin = 0.728, Tmax = 0.858l = −25→25
36650 measured reflections

Refinement

Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.027H-atom parameters constrained
wR(F2) = 0.073w = 1/[σ2(Fo2) + (0.0545P)2 + 0.2291P] where P = (Fo2 + 2Fc2)/3
S = 1.06(Δ/σ)max = 0.002
6075 reflectionsΔρmax = 0.95 e Å3
305 parametersΔρmin = −0.34 e Å3
21 restraintsAbsolute structure: Flack (1983), 2621 Friedel pairs
Primary atom site location: structure-invariant direct methodsFlack parameter: −0.02 (2)

Special details

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)

xyzUiso*/UeqOcc. (<1)
Rh10.55265 (2)0.179334 (12)0.820495 (9)0.02703 (6)
P10.62151 (8)0.15079 (4)0.71305 (3)0.02599 (13)
P20.62220 (8)0.04667 (4)0.83972 (3)0.02676 (13)
C10.5242 (4)0.31550 (18)0.80272 (15)0.0417 (7)
H1A0.56630.33480.76000.050*
C20.3872 (4)0.2772 (2)0.79692 (15)0.0431 (7)
H2A0.35020.27490.75060.052*
C30.2629 (5)0.2709 (3)0.8481 (2)0.0656 (11)
H3A0.19690.22540.83620.079*
H3B0.20320.32110.84700.079*
C40.3214 (6)0.2576 (3)0.9195 (2)0.0721 (13)
H4A0.34890.31060.93840.087*
H4B0.24010.23510.94660.087*
C50.4564 (6)0.2006 (2)0.92417 (14)0.0550 (10)
H5A0.43800.15000.94990.066*
C60.6040 (6)0.2249 (2)0.92248 (16)0.0555 (11)
H6A0.67200.18880.94790.067*
C70.6635 (7)0.3112 (2)0.91348 (19)0.0689 (13)
H7A0.76850.30790.89950.083*
H7B0.66120.33890.95660.083*
C80.5783 (6)0.3636 (2)0.86315 (19)0.0667 (13)
H8A0.49160.38830.88520.080*
H8B0.64370.40800.84810.080*
C90.6456 (3)0.03874 (18)0.70368 (13)0.0333 (6)
H9A0.54780.01220.69880.040*
H9B0.70570.02670.66420.040*
C100.7254 (3)0.00717 (18)0.76640 (13)0.0340 (6)
H10A0.82940.02640.76720.041*
H10B0.7259−0.05260.76680.041*
C110.5147 (3)0.18501 (18)0.63828 (12)0.0309 (5)
H11A0.48300.24210.64620.037*
C120.6369 (4)0.1865 (2)0.58392 (14)0.0435 (7)
H12A0.66050.13080.56960.052*
H12B0.60180.21740.54530.052*
C130.7764 (4)0.2272 (2)0.61365 (17)0.0484 (8)
H13A0.76100.28630.61610.058*
H13B0.86310.21680.58500.058*
C140.8070 (3)0.19301 (18)0.68390 (14)0.0364 (6)
H14A0.87730.14660.67930.044*
C150.3730 (4)0.1352 (2)0.62165 (15)0.0414 (7)
H15A0.30830.13280.66090.050*
H15B0.40200.07930.61020.050*
C160.2847 (4)0.1727 (3)0.56339 (17)0.0522 (8)
H16A0.19600.14020.55490.078*
H16B0.34730.17350.52410.078*
H16C0.25530.22800.57460.078*
C170.8803 (4)0.2564 (3)0.7303 (2)0.0556 (9)
H17A0.81190.30260.73620.067*
H17B0.89710.23160.77390.067*
C181.0305 (5)0.2877 (3)0.7027 (3)0.0729 (12)
H18A1.07300.32720.73330.109*
H18B1.01400.31350.66000.109*
H18C1.09910.24230.69750.109*
C190.7298 (3)0.01375 (18)0.91399 (14)0.0338 (6)
H19A0.69110.04510.95230.041*
C200.6821 (4)−0.07572 (19)0.92375 (17)0.0449 (7)
H20A0.7293−0.11080.89030.054*
H20B0.7111−0.09510.96790.054*
C210.5106 (4)−0.07681 (19)0.91604 (16)0.0428 (7)
H21A0.4637−0.04990.95420.051*
H21B0.4747−0.13330.91430.051*
C220.4677 (3)−0.03148 (17)0.85109 (14)0.0345 (6)
H22A0.4750−0.07110.81410.041*
C230.3065 (4)0.0006 (2)0.85289 (17)0.0448 (7)
H23A0.30000.04360.88650.054*
H23B0.2402−0.04390.86680.054*
C240.2487 (4)0.0349 (3)0.7865 (2)0.0622 (10)
H24A0.14660.05400.79200.093*
H24B0.2513−0.00760.75300.093*
H24C0.31180.08000.77270.093*
C250.9010 (4)0.0292 (2)0.91028 (17)0.0456 (7)
H25A0.9430−0.00310.87380.055*
H25B0.91860.08690.90030.055*
C260.9818 (5)0.0075 (4)0.9735 (2)0.0775 (13)
H26A1.08790.01840.96830.116*
H26B0.9669−0.04990.98320.116*
H26C0.94250.04011.00970.116*
B10.5008 (3)0.0287 (2)0.09541 (15)0.0521 (9)
F10.4824 (5)0.0657 (3)0.15617 (16)0.1419 (18)
F20.4003 (6)0.0460 (4)0.0449 (2)0.0663 (15)*0.515 (7)
F30.6464 (5)0.0467 (4)0.0748 (3)0.0791 (18)*0.515 (7)
F40.4794 (10)−0.0470 (4)0.1253 (4)0.125 (3)*0.515 (7)
F2'0.3620 (5)0.0229 (4)0.0636 (3)0.0655 (15)*0.485 (7)
F3'0.5818 (10)0.0895 (5)0.0629 (4)0.111 (3)*0.485 (7)
F4'0.5614 (7)−0.0489 (3)0.0851 (3)0.0781 (19)*0.485 (7)

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
Rh10.03754 (10)0.02407 (10)0.01948 (9)0.00346 (8)−0.00143 (7)−0.00007 (7)
P10.0289 (3)0.0278 (3)0.0213 (3)0.0005 (2)0.0010 (2)0.0001 (2)
P20.0317 (3)0.0240 (3)0.0246 (3)0.0016 (3)−0.0005 (2)0.0006 (2)
C10.0641 (19)0.0273 (13)0.0336 (13)0.0106 (14)−0.0043 (12)0.0059 (11)
C20.0526 (17)0.0443 (17)0.0324 (13)0.0261 (15)0.0063 (13)0.0056 (12)
C30.062 (2)0.076 (3)0.059 (2)0.030 (2)0.0252 (19)0.006 (2)
C40.107 (4)0.065 (3)0.044 (2)0.028 (2)0.037 (2)0.0032 (18)
C50.104 (3)0.0408 (18)0.0198 (12)0.0109 (19)0.0115 (17)0.0005 (11)
C60.111 (3)0.0291 (16)0.0265 (14)0.0103 (18)−0.0235 (17)−0.0037 (12)
C70.126 (4)0.0322 (18)0.0481 (19)−0.002 (2)−0.034 (2)−0.0029 (15)
C80.124 (4)0.0303 (17)0.0455 (18)0.002 (2)−0.015 (2)0.0045 (14)
C90.0405 (15)0.0334 (14)0.0260 (12)0.0011 (11)0.0036 (10)−0.0019 (11)
C100.0411 (15)0.0310 (14)0.0299 (13)0.0040 (11)0.0038 (11)−0.0001 (11)
C110.0391 (14)0.0326 (13)0.0210 (10)0.0000 (11)−0.0007 (9)0.0014 (10)
C120.0479 (17)0.057 (2)0.0253 (12)0.0031 (16)0.0055 (11)0.0059 (13)
C130.0458 (17)0.061 (2)0.0386 (16)−0.0046 (15)0.0080 (13)0.0160 (15)
C140.0327 (13)0.0392 (15)0.0371 (14)0.0000 (10)0.0009 (11)0.0051 (12)
C150.0480 (17)0.0448 (17)0.0314 (14)−0.0022 (14)−0.0072 (12)0.0045 (12)
C160.0573 (19)0.057 (2)0.0426 (16)−0.0054 (18)−0.0188 (14)0.0081 (17)
C170.0420 (17)0.063 (2)0.062 (2)−0.0173 (17)0.0009 (16)−0.0054 (18)
C180.047 (2)0.085 (3)0.087 (3)−0.024 (2)−0.0018 (19)0.002 (2)
C190.0390 (15)0.0329 (15)0.0294 (13)0.0031 (11)−0.0023 (11)0.0043 (11)
C200.060 (2)0.0308 (15)0.0440 (17)0.0067 (14)−0.0009 (15)0.0087 (13)
C210.0573 (19)0.0299 (14)0.0412 (15)−0.0087 (13)0.0024 (13)0.0082 (12)
C220.0418 (16)0.0282 (13)0.0335 (12)−0.0061 (12)0.0032 (11)−0.0025 (10)
C230.0369 (16)0.0483 (18)0.0491 (18)−0.0052 (13)0.0065 (13)0.0055 (15)
C240.0378 (18)0.083 (3)0.066 (2)−0.0052 (18)−0.0062 (16)0.014 (2)
C250.0435 (17)0.0484 (19)0.0450 (17)0.0009 (13)−0.0045 (13)0.0088 (14)
C260.066 (3)0.106 (4)0.061 (3)−0.001 (2)−0.012 (2)0.010 (2)
B10.061 (2)0.045 (2)0.050 (2)−0.0017 (17)−0.0056 (17)0.0075 (17)
F10.118 (3)0.241 (5)0.0664 (18)−0.026 (3)0.0212 (19)−0.049 (3)

Geometric parameters (Å, °)

Rh1—C22.209 (3)C13—H13B0.9700
Rh1—C62.211 (3)C14—C171.528 (5)
Rh1—C12.251 (3)C14—H14A0.9800
Rh1—C52.262 (3)C15—C161.526 (4)
Rh1—P22.2702 (8)C15—H15A0.9700
Rh1—P12.2754 (8)C15—H15B0.9700
P1—C91.839 (3)C16—H16A0.9600
P1—C111.850 (3)C16—H16B0.9600
P1—C141.869 (3)C16—H16C0.9600
P2—C101.839 (3)C17—C181.524 (5)
P2—C191.840 (3)C17—H17A0.9700
P2—C221.877 (3)C17—H17B0.9700
C1—C21.366 (5)C18—H18A0.9600
C1—C81.514 (5)C18—H18B0.9600
C1—H1A0.9800C18—H18C0.9600
C2—C31.503 (5)C19—C201.523 (4)
C2—H2A0.9800C19—C251.536 (5)
C3—C41.531 (6)C19—H19A0.9800
C3—H3A0.9700C20—C211.524 (5)
C3—H3B0.9700C20—H20A0.9700
C4—C51.511 (6)C20—H20B0.9700
C4—H4A0.9700C21—C221.537 (4)
C4—H4B0.9700C21—H21A0.9700
C5—C61.363 (7)C21—H21B0.9700
C5—H5A0.9800C22—C231.517 (4)
C6—C71.506 (5)C22—H22A0.9800
C6—H6A0.9800C23—C241.524 (5)
C7—C81.516 (5)C23—H23A0.9700
C7—H7A0.9700C23—H23B0.9700
C7—H7B0.9700C24—H24A0.9600
C8—H8A0.9700C24—H24B0.9600
C8—H8B0.9700C24—H24C0.9600
C9—C101.525 (4)C25—C261.491 (5)
C9—H9A0.9700C25—H25A0.9700
C9—H9B0.9700C25—H25B0.9700
C10—H10A0.9700C26—H26A0.9600
C10—H10B0.9700C26—H26B0.9600
C11—C151.526 (4)C26—H26C0.9600
C11—C121.531 (4)B1—F11.362 (3)
C11—H11A0.9800B1—F21.372 (4)
C12—C131.518 (5)B1—F41.377 (4)
C12—H12A0.9700B1—F3'1.381 (4)
C12—H12B0.9700B1—F31.382 (4)
C13—C141.531 (4)B1—F4'1.383 (4)
C13—H13A0.9700B1—F2'1.384 (4)
C2—Rh1—C695.24 (13)C14—C13—H13A109.6
C2—Rh1—C135.65 (13)C12—C13—H13B109.6
C6—Rh1—C180.79 (11)C14—C13—H13B109.6
C2—Rh1—C580.57 (12)H13A—C13—H13B108.2
C6—Rh1—C535.46 (17)C17—C14—C13112.7 (3)
C1—Rh1—C587.29 (11)C17—C14—P1115.5 (2)
C2—Rh1—P2153.68 (10)C13—C14—P1105.2 (2)
C6—Rh1—P296.08 (9)C17—C14—H14A107.7
C1—Rh1—P2170.65 (9)C13—C14—H14A107.7
C5—Rh1—P295.26 (9)P1—C14—H14A107.7
C2—Rh1—P197.05 (8)C11—C15—C16112.0 (3)
C6—Rh1—P1151.59 (13)C11—C15—H15A109.2
C1—Rh1—P194.65 (8)C16—C15—H15A109.2
C5—Rh1—P1172.93 (13)C11—C15—H15B109.2
P2—Rh1—P183.91 (2)C16—C15—H15B109.2
C9—P1—C11105.88 (13)H15A—C15—H15B107.9
C9—P1—C14103.23 (13)C15—C16—H16A109.5
C11—P1—C1494.99 (12)C15—C16—H16B109.5
C9—P1—Rh1109.13 (9)H16A—C16—H16B109.5
C11—P1—Rh1124.17 (9)C15—C16—H16C109.5
C14—P1—Rh1116.93 (10)H16A—C16—H16C109.5
C10—P2—C19106.43 (13)H16B—C16—H16C109.5
C10—P2—C22102.82 (13)C18—C17—C14112.0 (3)
C19—P2—C2294.75 (13)C18—C17—H17A109.2
C10—P2—Rh1109.28 (9)C14—C17—H17A109.2
C19—P2—Rh1123.44 (10)C18—C17—H17B109.2
C22—P2—Rh1117.61 (10)C14—C17—H17B109.2
C2—C1—C8125.6 (3)H17A—C17—H17B107.9
C2—C1—Rh170.51 (16)C17—C18—H18A109.5
C8—C1—Rh1110.2 (2)C17—C18—H18B109.5
C2—C1—H1A114.1H18A—C18—H18B109.5
C8—C1—H1A114.1C17—C18—H18C109.5
Rh1—C1—H1A114.1H18A—C18—H18C109.5
C1—C2—C3128.4 (3)H18B—C18—H18C109.5
C1—C2—Rh173.84 (17)C20—C19—C25115.7 (3)
C3—C2—Rh1106.9 (2)C20—C19—P2103.7 (2)
C1—C2—H2A113.2C25—C19—P2115.0 (2)
C3—C2—H2A113.2C20—C19—H19A107.3
Rh1—C2—H2A113.2C25—C19—H19A107.3
C2—C3—C4113.2 (4)P2—C19—H19A107.3
C2—C3—H3A108.9C21—C20—C19105.9 (3)
C4—C3—H3A108.9C21—C20—H20A110.6
C2—C3—H3B108.9C19—C20—H20A110.6
C4—C3—H3B108.9C21—C20—H20B110.6
H3A—C3—H3B107.7C19—C20—H20B110.6
C5—C4—C3114.2 (3)H20A—C20—H20B108.7
C5—C4—H4A108.7C20—C21—C22109.0 (3)
C3—C4—H4A108.7C20—C21—H21A109.9
C5—C4—H4B108.7C22—C21—H21A109.9
C3—C4—H4B108.7C20—C21—H21B109.9
H4A—C4—H4B107.6C22—C21—H21B109.9
C6—C5—C4125.2 (4)H21A—C21—H21B108.3
C6—C5—Rh170.2 (2)C23—C22—C21112.1 (3)
C4—C5—Rh1109.5 (2)C23—C22—P2117.0 (2)
C6—C5—H5A114.4C21—C22—P2104.2 (2)
C4—C5—H5A114.4C23—C22—H22A107.7
Rh1—C5—H5A114.4C21—C22—H22A107.7
C5—C6—C7127.3 (4)P2—C22—H22A107.7
C5—C6—Rh174.32 (19)C22—C23—C24114.8 (3)
C7—C6—Rh1105.8 (2)C22—C23—H23A108.6
C5—C6—H6A113.7C24—C23—H23A108.6
C7—C6—H6A113.7C22—C23—H23B108.6
Rh1—C6—H6A113.7C24—C23—H23B108.6
C6—C7—C8115.2 (4)H23A—C23—H23B107.5
C6—C7—H7A108.5C23—C24—H24A109.5
C8—C7—H7A108.5C23—C24—H24B109.5
C6—C7—H7B108.5H24A—C24—H24B109.5
C8—C7—H7B108.5C23—C24—H24C109.5
H7A—C7—H7B107.5H24A—C24—H24C109.5
C1—C8—C7113.3 (3)H24B—C24—H24C109.5
C1—C8—H8A108.9C26—C25—C19113.1 (3)
C7—C8—H8A108.9C26—C25—H25A109.0
C1—C8—H8B108.9C19—C25—H25A109.0
C7—C8—H8B108.9C26—C25—H25B109.0
H8A—C8—H8B107.7C19—C25—H25B109.0
C10—C9—P1107.57 (19)H25A—C25—H25B107.8
C10—C9—H9A110.2C25—C26—H26A109.5
P1—C9—H9A110.2C25—C26—H26B109.5
C10—C9—H9B110.2H26A—C26—H26B109.5
P1—C9—H9B110.2C25—C26—H26C109.5
H9A—C9—H9B108.5H26A—C26—H26C109.5
C9—C10—P2107.82 (19)H26B—C26—H26C109.5
C9—C10—H10A110.1F1—B1—F2119.1 (4)
P2—C10—H10A110.1F1—B1—F489.5 (5)
C9—C10—H10B110.1F2—B1—F4114.3 (5)
P2—C10—H10B110.1F1—B1—F3'99.5 (4)
H10A—C10—H10B108.5F2—B1—F3'81.1 (5)
C15—C11—C12115.7 (2)F4—B1—F3'155.6 (6)
C15—C11—P1115.8 (2)F1—B1—F3106.4 (4)
C12—C11—P1102.44 (19)F2—B1—F3109.9 (4)
C15—C11—H11A107.5F4—B1—F3116.4 (5)
C12—C11—H11A107.5F1—B1—F4'125.4 (4)
P1—C11—H11A107.5F2—B1—F4'109.1 (4)
C13—C12—C11107.6 (2)F4—B1—F4'46.1 (4)
C13—C12—H12A110.2F3'—B1—F4'112.3 (5)
C11—C12—H12A110.2F3—B1—F4'77.7 (4)
C13—C12—H12B110.2F1—B1—F2'109.4 (4)
C11—C12—H12B110.2F4—B1—F2'90.9 (5)
H12A—C12—H12B108.5F3'—B1—F2'107.0 (5)
C12—C13—C14110.1 (3)F3—B1—F2'134.7 (4)
C12—C13—H13A109.6F4'—B1—F2'102.3 (4)

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: SI2281).

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