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Acta Crystallogr Sect E Struct Rep Online. 2010 June 1; 66(Pt 6): m721–m722.
Published online 2010 May 29. doi:  10.1107/S1600536810019859
PMCID: PMC2979608

(+)-{1,2-Bis[(2R,5R)-2,5-dimethyl­phospho­lan-1-yl]ethane-κ2 P,P′}(η4-cyclo­octa-1,5-diene)rhodium(I) tetra­fluorido­borate

Abstract

The title compound, [Rh(C8H12)(C14H28P2)]BF4, exhibits a rhodium(I) complex cation with a bidentate bis­phosphine ligand and a bidentate η22-coordinated cyclo­octa-1,5-diene. Together the ligands create a slightly distorted square-planar cordination environment for the Rh(I) atom. There are three mol­ecules in the asymmetric unit and intra­molecular P—Rh—P bite angles of 82.78 (5), 82.97 (6) and 83.09 (5)° are observed. The dihedral angles between the P—Rh—P and the X—Rh—X planes (X is the centroid of a double bond) are 14.7 (1), 14.8 (1) and 15.3 (1)°. The structure exhibits disorder of one cyclo­octa­diene ligand as well as one BF4 anion.

Related literature

For general synthetic procedures for cationic rhodium bis­phosphine diolefin complexes, see: Schrock & Osborn (1971 [triangle]); Fennis et al. (1990 [triangle]); Fernandez et al. (2000 [triangle]). For a discussion on the structures of cationic rhodium bis­phosphine diolefin complexes in general, see: Drexler et al. (2004 [triangle]) and for the different stereoisomers of [Rh(Me-BPE)COD]BF4, see: Fox & McCague (2005 [triangle]). For the structures of related complexes, see: Burk et al. (1990 [triangle]); Burk (1991 [triangle]); Drexler et al. (2004 [triangle]); Burk et al. (1993 [triangle]). For applications of related ligands in catalytic reactions, see: Axtell et al. (2005 [triangle]); Burk et al. (1995 [triangle]); Heller et al. (2002 [triangle]); Schäffner et al. (2008 [triangle]).

An external file that holds a picture, illustration, etc.
Object name is e-66-0m721-scheme1.jpg

Experimental

Crystal data

  • [Rh(C8H12)(C14H28P2)]BF4
  • M r = 556.20
  • Orthorhombic, An external file that holds a picture, illustration, etc.
Object name is e-66-0m721-efi1.jpg
  • a = 10.224 (2) Å
  • b = 14.771 (3) Å
  • c = 50.158 (10) Å
  • V = 7575 (3) Å3
  • Z = 12
  • Mo Kα radiation
  • μ = 0.84 mm−1
  • T = 200 K
  • 0.20 × 0.13 × 0.10 mm

Data collection

  • Stoe IPDS 2 diffractometer
  • Absorption correction: numerical (X-SHAPE and X-RED32; Stoe & Cie, 2005 [triangle]) T min = 0.853, T max = 0.945
  • 67186 measured reflections
  • 13252 independent reflections
  • 9566 reflections with I > 2σ(I)
  • R int = 0.055

Refinement

  • R[F 2 > 2σ(F 2)] = 0.032
  • wR(F 2) = 0.046
  • S = 0.87
  • 13252 reflections
  • 804 parameters
  • 77 restraints
  • H-atom parameters constrained
  • Δρmax = 0.37 e Å−3
  • Δρmin = −0.28 e Å−3
  • Absolute structure: Flack (1983 [triangle]), 5822 Friedel pairs
  • Flack parameter: −0.03 (2)

Data collection: X-AREA (Stoe & Cie, 2005 [triangle]); cell refinement: X-AREA; 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/S1600536810019859/im2198sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536810019859/im2198Isup2.hkl

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

supplementary crystallographic information

Comment

In the course of our studies on structures of cationic rhodium bisphosphine diolefin complexes (Drexler et al., 2004), we became interested in the chiral ligand family of 1,2-bis(2,5-dialkylphospholano)ethane, that build up five-membered ring chelates with rhodium (see: figure 1).

The title compound [Rh((R,R)-Me-BPE)COD)]BF4 can be easily synthesized by an cycloocta-1,5-diene (COD) exchange of [Rh(COD)2]BF4 with the chiral bisphosphine ligand (R,R)-Me-BPE (Schrock & Osborn, 1971) or an exchange of acetylacetonate (acac) by the bisphosphine in the presence of HBF4 starting from the precursor [Rh(acac)(COD)] (Fennis et al., 1990).

Usually, the five-membered ring chelate is flexible and λ- or δ-conformers would be anticipated (Fernandez et al., 2000). For the title compound the molecular structure of the three molecules in the asymmetric unit exclusively show δ-conformation of the bisphosphine backbones. COD ligands are η2,η2-coordinated and are orientated in an anticlockwise twist manner for all molecules (see: figure 2). This means that the double bonds of COD are not coordinated perpendicular to the P,Rh,P plane. The dihedral angles between the planes of P,Rh,P and of X,Rh,X (X = centroid of the double bond) are 14.8 (1)° (Rh1), 14.7 (1)° (Rh2) and 15.3 (1)° (Rh3). These dihedral angles are comparable to those in the corresponding Me-BPE complex [Rh((R,R)-Me-BPE)COD]SbF6 (19.4°) (Burk et al., 1990; Drexler et al., 2004) or for the Me-DuPhos complexes ([Rh((S,S)-Me-DuPhos)COD]BF4: 16.4°, Drexler et al., 2004; [Rh((S,S)-Me-DuPhos)COD]SbF6: 17.8°, Drexler et al., 2004; Burk et al., 1993).

Intramolecular P—Rh—P angles of 82.78 (5)°, 82.97 (6)° and 83.09 (5)° were obtained. They are in the same range as those of corresponding complexes already described in the literature ([Rh((R,R)-Me-BPE)COD]SbF6: 83.25 (6)°, Burk et al., 1990; [Rh((R,R)-Et-DuPhos)COD]BF4: 85.32 (6)°, Drexler et al., 2001) exclusively for the complex [Rh((R,R)-iPr-BPE)COD]SbF6 with an bite angle of 95.18 (9)° (Burk et al., 1991).

Experimental

By overlaying a solution of [Rh((R,R)-Me-BPE)COD]BF4 in dichloromethane with MTBE (methyl-tert-butylether) red-orange single crystals suitable for X-ray analysis are obtained. 31P NMR (CD2Cl2, 298 K, 122 MHz) [ppm]: 77.0 (d, JP—Rh = 146.0 Hz).

Refinement

All non-hydrogen atoms are refined anisotropically, except not fully occupied non-hydrogen atoms of one anion and one COD, which are disordered. Distance restraints were used to improve the geometry of the respective anions and COD ligands. All H atoms were placed in idealized positions with d(C—H) = 0.99 (CH2), 0.98 (CH3) and 1.0 Å (CH) 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.

Figures

Fig. 1.
Perspective view and numbering scheme of the three cations [Rh((R,R)-Me-BPE)COD]+ in the asymmetric unit (30% probability displacement ellipsoids). All hydrogens and anions have been omitted for clarity.
Fig. 2.
Front view, perspective diagram of one cation [Rh((R,R)-Me-BPE)COD]+ showing the anticlockwise twist of the cycloocta-1,5-diene ligand.

Crystal data

[Rh(C8H12)(C14H28P2)]BF4F(000) = 3456
Mr = 556.20Dx = 1.463 Mg m3
Orthorhombic, P212121Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2ac 2abCell parameters from 35629 reflections
a = 10.224 (2) Åθ = 1.4–26.1°
b = 14.771 (3) ŵ = 0.84 mm1
c = 50.158 (10) ÅT = 200 K
V = 7575 (3) Å3Part of rod, red
Z = 120.20 × 0.13 × 0.10 mm

Data collection

Stoe IPDS 2 diffractometer13252 independent reflections
Radiation source: fine-focus sealed tube9566 reflections with I > 2σ(I)
graphiteRint = 0.055
Detector resolution: 6.67 pixels mm-1θmax = 25.0°, θmin = 1.4°
rotation method scansh = −12→12
Absorption correction: numerical (X-SHAPE and X-RED32; Stoe & Cie, 2005)k = −17→17
Tmin = 0.853, Tmax = 0.945l = −59→59
67186 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)] = 0.032H-atom parameters constrained
wR(F2) = 0.046w = 1/[σ2(Fo2) + (0.P)2] where P = (Fo2 + 2Fc2)/3
S = 0.87(Δ/σ)max = 0.005
13252 reflectionsΔρmax = 0.37 e Å3
804 parametersΔρmin = −0.28 e Å3
77 restraintsAbsolute structure: Flack (1983), 5822 Friedel pairs
Primary atom site location: structure-invariant direct methodsFlack parameter: −0.03 (2)

Special details

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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)
Rh10.82592 (3)0.50648 (3)0.225528 (7)0.03098 (9)
Rh20.68473 (4)0.17120 (3)0.070150 (7)0.03643 (10)
Rh30.30533 (4)0.65212 (3)0.096621 (7)0.03681 (10)
P10.86072 (10)0.52268 (9)0.27014 (3)0.0334 (3)
P20.61906 (11)0.47364 (9)0.23907 (3)0.0376 (3)
P210.68588 (15)0.12890 (9)0.11366 (3)0.0398 (3)
P220.90416 (12)0.17094 (11)0.07562 (3)0.0387 (4)
P310.11683 (12)0.73359 (10)0.09291 (3)0.0398 (4)
P320.32525 (15)0.68615 (9)0.05279 (2)0.0372 (3)
C11.0259 (5)0.4697 (4)0.21284 (11)0.0443 (15)
H1A1.07600.44080.22770.053*0.50
H1B1.07890.43820.22620.053*0.50
C21.0220 (5)0.5638 (4)0.21560 (12)0.0462 (16)
H2A1.07220.58860.23110.055*0.50
H2B1.06960.58690.23110.055*0.50
C31.0234 (9)0.6181 (9)0.1923 (2)0.045 (4)*0.50
H3A1.06270.58340.17750.053*0.50
H3B1.07830.67220.19550.053*0.50
C40.8848 (8)0.6481 (8)0.1845 (2)0.042 (3)*0.50
H4A0.88550.67060.16590.051*0.50
H4B0.85700.69840.19620.051*0.50
C3'0.9846 (14)0.6392 (10)0.1936 (3)0.065 (5)*0.50
H3C0.95000.69320.20290.078*0.50
H3D1.06540.65760.18420.078*0.50
C4'0.8841 (10)0.6086 (9)0.1729 (2)0.060 (4)*0.50
H4C0.85010.66150.16290.072*0.50
H4D0.92480.56620.16000.072*0.50
C50.7798 (5)0.5645 (5)0.18707 (12)0.0626 (19)
H5A0.68730.58630.18620.075*0.50
H5B0.69280.59150.18500.075*0.50
C60.7889 (5)0.4703 (5)0.18289 (11)0.063 (2)
H6A0.70770.43590.17830.076*0.50
H6B0.70140.44400.18100.076*0.50
C70.9149 (9)0.4465 (8)0.1687 (2)0.043 (3)*0.50
H7A0.95480.50150.16090.052*0.50
H7B0.89750.40280.15410.052*0.50
C81.0077 (12)0.4043 (9)0.1895 (2)0.048 (4)*0.50
H8A0.97070.34640.19600.058*0.50
H8B1.09350.39140.18110.058*0.50
C7'0.8969 (8)0.3997 (8)0.1755 (2)0.040 (3)*0.50
H7C0.87480.34030.18350.048*0.50
H7D0.90020.39220.15590.048*0.50
C8'1.0314 (9)0.4306 (9)0.1857 (2)0.037 (4)*0.50
H8C1.09170.37810.18580.045*0.50
H8D1.06740.47640.17330.045*0.50
C90.7140 (4)0.4873 (4)0.28857 (9)0.0419 (13)
H9A0.71410.42080.29100.050*
H9B0.71280.51610.30640.050*
C100.5960 (4)0.5158 (4)0.27287 (10)0.0389 (13)
H10A0.58790.58250.27280.047*
H10B0.51570.48970.28080.047*
C111.0028 (5)0.4737 (4)0.28699 (11)0.0421 (14)
H11A1.07660.47490.27390.051*
C121.0378 (5)0.5388 (4)0.30895 (12)0.0560 (17)
H12A1.12880.52880.31500.067*
H12B0.97840.53100.32440.067*
C131.0227 (5)0.6331 (4)0.29706 (13)0.0573 (17)
H13A1.09450.64500.28430.069*
H13B1.02680.67920.31140.069*
C140.8908 (5)0.6387 (3)0.28275 (10)0.0425 (13)
H14A0.82360.65020.29680.051*
C150.9866 (6)0.3764 (4)0.29560 (13)0.064 (2)
H15A1.06750.35530.30400.096*
H15B0.96730.33880.28000.096*
H15C0.91440.37200.30840.096*
C160.8791 (5)0.7152 (3)0.26294 (12)0.0620 (16)
H16A0.89680.77280.27190.093*
H16B0.79050.71610.25550.093*
H16C0.94250.70630.24850.093*
C170.4699 (4)0.4987 (5)0.21980 (11)0.0554 (16)
H17A0.49490.50090.20050.067*
C180.3837 (5)0.4154 (5)0.22387 (14)0.070 (2)
H18A0.33790.41930.24120.084*
H18B0.31720.41170.20960.084*
C190.4703 (5)0.3331 (5)0.22324 (13)0.0680 (18)
H19A0.50050.32150.20480.082*
H19B0.42120.27940.22950.082*
C200.5874 (4)0.3504 (4)0.24144 (11)0.0518 (15)
H20A0.55940.33720.26010.062*
C210.4052 (6)0.5867 (4)0.22654 (14)0.075 (2)
H21A0.32790.59490.21520.113*
H21B0.46670.63650.22350.113*
H21C0.37870.58630.24530.113*
C220.7015 (6)0.2899 (3)0.23517 (13)0.0694 (17)
H22A0.67530.22650.23730.104*
H22B0.77380.30340.24740.104*
H22C0.72990.30040.21680.104*
C310.4901 (5)0.2375 (4)0.06897 (12)0.0472 (15)
H31A0.45950.25870.08680.057*
C320.4687 (4)0.1448 (4)0.06465 (12)0.0498 (17)
H32A0.42550.11220.07970.060*
C330.4467 (5)0.1042 (5)0.03785 (14)0.083 (2)
H33A0.39550.14760.02700.099*
H33B0.39290.04900.04000.099*
C340.5688 (6)0.0794 (6)0.02254 (15)0.094 (3)
H34A0.59130.01590.02690.113*
H34B0.54800.08170.00330.113*
C350.6846 (6)0.1354 (4)0.02726 (10)0.0585 (16)
H35A0.76800.10700.02100.070*
C360.6906 (7)0.2298 (4)0.02921 (10)0.0593 (16)
H36A0.77720.25610.02410.071*
C370.5777 (6)0.2910 (5)0.02433 (13)0.090 (3)
H37A0.52020.26310.01070.109*
H37B0.61060.34880.01700.109*
C380.4976 (7)0.3108 (5)0.04901 (12)0.082 (2)
H38A0.53460.36510.05780.098*
H38B0.40750.32600.04330.098*
C390.8513 (4)0.1388 (4)0.12698 (10)0.0460 (15)
H39A0.87020.20250.13180.055*
H39B0.86090.10110.14320.055*
C400.9448 (5)0.1068 (4)0.10544 (11)0.0418 (15)
H40A0.93380.04110.10220.050*
H40B1.03660.11830.11080.050*
C410.5772 (5)0.1797 (4)0.13869 (11)0.0475 (15)
H41A0.49280.19370.12950.057*
C420.5498 (6)0.1038 (5)0.15788 (13)0.068 (2)
H42A0.62500.09480.17000.082*
H42B0.47140.11770.16870.082*
C430.5273 (5)0.0211 (5)0.14145 (14)0.071 (2)
H43A0.44360.02650.13160.086*
H43B0.5223−0.03290.15310.086*
C440.6406 (4)0.0110 (4)0.12176 (11)0.0540 (15)
H44A0.7155−0.01570.13190.065*
C450.6241 (6)0.2667 (4)0.15108 (12)0.073 (2)
H45A0.55900.28830.16390.110*
H45B0.63650.31230.13710.110*
H45C0.70740.25610.16020.110*
C460.6139 (6)−0.0510 (4)0.09844 (15)0.076 (2)
H46A0.5921−0.11160.10500.115*
H46B0.6919−0.05440.08710.115*
H46C0.5405−0.02720.08800.115*
C471.0193 (5)0.1383 (5)0.04934 (12)0.0551 (17)
H47A0.97690.15150.03180.066*
C481.1320 (6)0.2034 (5)0.05267 (15)0.081 (2)
H48A1.19010.18320.06730.097*
H48B1.18380.20690.03600.097*
C491.0735 (7)0.2941 (5)0.05912 (15)0.081 (3)
H49A1.14320.33690.06450.098*
H49B1.02880.31900.04320.098*
C500.9773 (5)0.2826 (4)0.08145 (12)0.0561 (17)
H50A1.02960.27760.09820.067*
C511.0593 (6)0.0383 (5)0.04937 (14)0.075 (2)
H51A1.11930.02680.03450.113*
H51B0.98120.00040.04740.113*
H51C1.10280.02380.06620.113*
C520.8835 (7)0.3609 (4)0.08534 (14)0.085 (2)
H52A0.93310.41650.08860.127*
H52B0.82660.34840.10060.127*
H52C0.82990.36830.06930.127*
C610.2458 (6)0.5608 (4)0.12921 (12)0.0613 (18)
H61A0.14880.55430.13100.074*
C620.2952 (6)0.6401 (4)0.14108 (11)0.0612 (17)
H62A0.22760.67940.14970.073*
C630.4270 (6)0.6461 (6)0.15322 (12)0.086 (2)
H63A0.45060.58620.16060.103*
H63B0.42410.68970.16820.103*
C640.5324 (6)0.6755 (6)0.13371 (12)0.087 (2)
H64A0.53670.74240.13380.105*
H64B0.61760.65270.14030.105*
C650.5158 (5)0.6449 (5)0.10556 (12)0.0596 (19)
H65A0.57230.67770.09250.072*
C660.4782 (6)0.5581 (4)0.09725 (14)0.0636 (18)
H66A0.51120.54100.07920.076*
C670.4544 (6)0.4795 (5)0.11517 (14)0.086 (2)
H67A0.51530.48350.13050.104*
H67B0.47500.42320.10530.104*
C680.3148 (7)0.4730 (4)0.12582 (14)0.091 (2)
H68A0.26310.43480.11350.109*
H68B0.31710.44180.14330.109*
C690.0849 (5)0.7563 (4)0.05786 (11)0.0496 (16)
H69A0.04490.70270.04930.060*
H69B0.02400.80800.05600.060*
C700.2147 (5)0.7783 (4)0.04481 (12)0.0558 (16)
H70A0.24950.83620.05170.067*
H70B0.20400.78360.02530.067*
C71−0.0378 (5)0.6989 (4)0.10800 (11)0.0463 (15)
H71A−0.01540.66740.12500.056*
C72−0.1042 (5)0.7865 (4)0.11559 (13)0.0587 (18)
H72A−0.14370.81530.09970.070*
H72B−0.17400.77520.12890.070*
C73−0.0009 (5)0.8454 (4)0.12709 (12)0.0633 (16)
H73A0.02640.82180.14470.076*
H73B−0.03530.90750.12960.076*
C740.1158 (5)0.8475 (4)0.10829 (12)0.0570 (16)
H74A0.09340.89120.09380.068*
C75−0.1210 (5)0.6336 (5)0.09196 (15)0.088 (3)
H75A−0.20000.61830.10210.131*
H75B−0.07090.57830.08840.131*
H75C−0.14590.66190.07500.131*
C760.2408 (6)0.8800 (4)0.12044 (16)0.092 (3)
H76A0.22820.94100.12760.138*
H76B0.30940.88130.10680.138*
H76C0.26680.83890.13480.138*
C770.4794 (5)0.7060 (4)0.03511 (12)0.0466 (15)
H77A0.54830.66860.04400.056*
C780.4552 (5)0.6657 (4)0.00776 (11)0.0618 (16)
H78A0.40070.7070−0.00310.074*
H78B0.53910.6557−0.00160.074*
C790.3853 (6)0.5768 (4)0.01195 (13)0.0663 (19)
H79A0.44550.53200.02000.080*
H79B0.35400.5527−0.00530.080*
C800.2696 (4)0.5941 (4)0.03052 (11)0.0470 (15)
H80A0.19580.61790.01950.056*
C810.5255 (6)0.8022 (4)0.03515 (14)0.074 (2)
H81A0.60940.80620.02580.111*
H81B0.53650.82280.05360.111*
H81C0.46090.84040.02610.111*
C820.2231 (5)0.5091 (4)0.04417 (11)0.0670 (17)
H82A0.19490.46510.03070.101*
H82B0.14950.52360.05590.101*
H82C0.29470.48330.05470.101*
B10.7819 (5)0.7243 (5)0.35410 (13)0.0457 (17)
F10.7859 (3)0.6327 (2)0.35020 (7)0.0892 (12)
F20.7065 (3)0.7637 (2)0.33541 (6)0.0820 (11)
F30.9076 (2)0.7578 (2)0.35287 (7)0.0726 (11)
F40.7329 (3)0.7410 (2)0.37907 (6)0.0874 (12)
B30.6346 (7)0.8352 (6)0.19316 (15)0.061 (2)
F90.7009 (3)0.8256 (3)0.16969 (6)0.0978 (12)
F100.5025 (3)0.8416 (3)0.18800 (7)0.0834 (11)
F110.6560 (4)0.7609 (3)0.20857 (9)0.1390 (19)
F120.6746 (4)0.9104 (3)0.20584 (8)0.1192 (17)
B20.7930 (8)0.5482 (7)0.02251 (15)0.100 (4)
F50.9082 (5)0.5195 (5)0.03039 (12)0.090 (3)*0.618 (7)
F60.7925 (6)0.6469 (3)0.02415 (12)0.104 (3)*0.618 (7)
F70.6990 (6)0.5245 (4)0.04215 (11)0.073 (3)*0.618 (7)
F80.7524 (7)0.5256 (5)−0.00082 (11)0.125 (4)*0.618 (7)
F5'0.8285 (11)0.4399 (5)0.0204 (2)0.126 (5)*0.382 (7)
F6'0.9221 (9)0.5735 (7)0.0278 (2)0.094 (4)*0.382 (7)
F7'0.7174 (11)0.5484 (9)0.0412 (2)0.107 (6)*0.382 (7)
F8'0.7640 (8)0.5615 (7)−0.00230 (17)0.072 (4)*0.382 (7)

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
Rh10.02789 (17)0.0373 (2)0.02778 (19)0.0001 (2)0.00228 (18)0.00123 (18)
Rh20.0306 (2)0.0494 (3)0.0293 (2)0.0028 (2)−0.0029 (2)−0.0004 (2)
Rh30.0333 (2)0.0494 (3)0.0278 (2)0.0021 (2)0.00166 (19)0.00467 (19)
P10.0351 (6)0.0387 (8)0.0264 (8)−0.0014 (6)−0.0027 (5)−0.0014 (6)
P20.0310 (6)0.0492 (10)0.0325 (8)−0.0029 (6)0.0030 (6)−0.0011 (7)
P210.0333 (7)0.0506 (9)0.0355 (8)−0.0013 (8)−0.0026 (8)0.0032 (6)
P220.0322 (7)0.0491 (10)0.0349 (9)−0.0039 (7)−0.0032 (6)0.0045 (8)
P310.0339 (7)0.0499 (10)0.0357 (9)0.0022 (7)0.0049 (6)0.0023 (7)
P320.0340 (7)0.0477 (8)0.0299 (7)0.0041 (8)0.0038 (7)0.0052 (6)
C10.028 (3)0.061 (4)0.044 (4)0.006 (3)−0.005 (2)−0.002 (3)
C20.034 (3)0.065 (5)0.040 (4)−0.011 (3)0.009 (2)−0.002 (3)
C50.037 (4)0.107 (6)0.043 (4)0.002 (4)−0.001 (3)0.027 (4)
C60.030 (3)0.127 (6)0.033 (4)0.018 (4)−0.004 (2)−0.014 (4)
C90.051 (3)0.046 (3)0.029 (3)−0.002 (3)0.002 (2)−0.004 (2)
C100.036 (2)0.046 (4)0.035 (3)0.001 (3)0.011 (2)0.000 (3)
C110.041 (3)0.043 (4)0.042 (3)0.004 (3)−0.005 (2)−0.007 (3)
C120.050 (3)0.062 (4)0.057 (4)0.002 (3)−0.018 (3)−0.016 (3)
C130.058 (4)0.046 (4)0.068 (5)−0.005 (3)−0.013 (3)−0.006 (3)
C140.052 (3)0.040 (3)0.036 (3)0.001 (3)−0.001 (2)−0.003 (2)
C150.081 (5)0.059 (5)0.053 (5)0.019 (4)−0.021 (3)0.009 (3)
C160.080 (4)0.040 (4)0.066 (5)0.001 (3)0.007 (4)−0.007 (3)
C170.033 (3)0.087 (5)0.046 (4)−0.001 (4)0.001 (2)−0.007 (4)
C180.042 (3)0.110 (6)0.059 (5)−0.015 (4)0.000 (3)−0.010 (4)
C190.052 (3)0.088 (5)0.064 (4)−0.027 (4)0.008 (3)−0.026 (4)
C200.051 (3)0.058 (4)0.047 (4)−0.012 (3)0.017 (3)−0.005 (3)
C210.057 (4)0.102 (6)0.066 (5)0.023 (4)−0.009 (4)0.012 (4)
C220.077 (4)0.044 (3)0.087 (5)−0.006 (3)0.015 (4)−0.008 (3)
C310.041 (3)0.063 (4)0.038 (4)0.023 (3)−0.001 (3)−0.002 (3)
C320.021 (3)0.080 (5)0.048 (4)0.004 (3)−0.001 (2)−0.010 (4)
C330.051 (4)0.137 (7)0.060 (5)−0.014 (4)−0.007 (3)−0.036 (5)
C340.065 (5)0.149 (8)0.068 (6)−0.011 (5)0.014 (4)−0.052 (5)
C350.037 (3)0.106 (5)0.033 (3)0.000 (4)0.000 (3)−0.015 (3)
C360.051 (3)0.096 (5)0.031 (3)0.010 (4)−0.004 (3)0.019 (3)
C370.076 (5)0.134 (7)0.061 (5)0.046 (5)0.006 (4)0.036 (5)
C380.093 (5)0.095 (6)0.057 (5)0.047 (4)−0.002 (4)0.022 (4)
C390.044 (3)0.064 (4)0.029 (3)0.000 (3)−0.003 (2)0.014 (3)
C400.027 (3)0.053 (4)0.045 (4)−0.007 (3)−0.002 (2)0.009 (3)
C410.039 (3)0.067 (4)0.037 (3)0.002 (3)0.000 (2)0.005 (3)
C420.054 (4)0.101 (6)0.049 (5)0.000 (4)0.009 (3)0.021 (4)
C430.056 (4)0.074 (5)0.085 (6)−0.008 (4)0.013 (3)0.030 (4)
C440.037 (3)0.060 (4)0.065 (4)0.006 (3)−0.002 (2)0.013 (3)
C450.073 (4)0.104 (6)0.044 (4)−0.003 (4)0.001 (3)−0.015 (4)
C460.065 (4)0.041 (4)0.124 (7)−0.011 (3)−0.012 (4)0.015 (4)
C470.038 (3)0.088 (5)0.040 (4)0.001 (3)0.000 (2)0.006 (3)
C480.041 (4)0.124 (7)0.078 (6)−0.009 (4)0.005 (3)0.022 (5)
C490.067 (4)0.103 (7)0.075 (6)−0.033 (4)−0.009 (4)0.042 (5)
C500.055 (4)0.057 (4)0.057 (4)−0.015 (3)−0.008 (3)0.022 (3)
C510.060 (4)0.111 (7)0.055 (5)0.017 (4)0.005 (3)−0.021 (4)
C520.107 (6)0.047 (4)0.100 (7)−0.003 (4)−0.015 (4)−0.004 (4)
C610.067 (4)0.070 (5)0.047 (4)−0.003 (3)0.015 (3)0.025 (3)
C620.064 (4)0.087 (5)0.032 (3)−0.008 (4)0.006 (3)0.009 (3)
C630.086 (5)0.138 (7)0.034 (4)−0.009 (5)−0.004 (3)0.001 (4)
C640.058 (4)0.149 (8)0.055 (5)−0.010 (5)−0.018 (3)0.012 (5)
C650.034 (3)0.097 (6)0.048 (4)0.005 (4)−0.011 (3)0.007 (4)
C660.064 (4)0.074 (5)0.053 (5)0.028 (4)0.008 (3)0.011 (4)
C670.113 (6)0.077 (6)0.069 (5)0.049 (5)0.011 (4)0.025 (4)
C680.103 (5)0.063 (5)0.106 (6)0.015 (5)0.004 (5)0.024 (4)
C690.043 (3)0.070 (5)0.037 (4)0.011 (3)0.002 (3)0.009 (3)
C700.064 (4)0.063 (4)0.041 (4)0.014 (3)0.009 (3)0.020 (3)
C710.037 (3)0.053 (4)0.049 (4)0.007 (3)0.008 (2)−0.003 (3)
C720.041 (3)0.081 (5)0.055 (4)0.022 (3)0.018 (3)0.005 (3)
C730.073 (4)0.063 (4)0.054 (4)0.014 (4)0.016 (3)−0.002 (4)
C740.056 (3)0.044 (4)0.071 (5)−0.002 (3)0.009 (3)0.005 (3)
C750.047 (4)0.113 (7)0.103 (7)−0.010 (4)0.019 (4)−0.039 (5)
C760.077 (5)0.067 (5)0.132 (8)−0.012 (4)−0.004 (4)−0.041 (4)
C770.044 (3)0.047 (4)0.048 (4)−0.001 (3)0.003 (3)−0.003 (3)
C780.064 (4)0.078 (5)0.043 (4)0.000 (4)0.020 (3)0.004 (4)
C790.063 (4)0.090 (5)0.046 (4)−0.011 (4)0.014 (3)−0.025 (4)
C800.036 (3)0.069 (4)0.037 (4)−0.004 (3)−0.002 (2)−0.004 (3)
C810.073 (4)0.075 (5)0.074 (5)−0.014 (4)0.023 (4)−0.002 (4)
C820.076 (4)0.068 (4)0.058 (4)−0.011 (4)−0.003 (3)−0.009 (4)
B10.035 (4)0.062 (5)0.040 (4)0.000 (3)−0.002 (3)0.013 (3)
F10.090 (3)0.073 (3)0.104 (3)−0.003 (2)−0.010 (2)−0.001 (2)
F20.066 (2)0.110 (3)0.070 (3)0.011 (2)−0.019 (2)0.023 (2)
F30.0399 (19)0.110 (3)0.068 (3)−0.004 (2)0.0011 (17)0.032 (2)
F40.068 (2)0.142 (4)0.052 (3)−0.012 (2)0.0107 (17)−0.010 (2)
B30.059 (5)0.076 (6)0.049 (5)0.010 (5)0.007 (3)0.006 (5)
F90.095 (2)0.145 (4)0.053 (2)0.026 (3)0.021 (2)−0.015 (2)
F100.070 (2)0.092 (3)0.089 (3)0.008 (2)0.0092 (19)−0.009 (2)
F110.136 (4)0.138 (4)0.143 (5)0.039 (4)0.004 (3)0.062 (3)
F120.073 (3)0.151 (4)0.133 (4)−0.025 (3)0.021 (3)−0.068 (3)
B20.073 (6)0.194 (12)0.034 (5)0.046 (6)0.002 (4)−0.024 (5)

Geometric parameters (Å, °)

Rh1—C52.163 (6)C35—C361.399 (4)
Rh1—C12.209 (5)C35—H35A1.0000
Rh1—C22.232 (5)C36—C371.486 (8)
Rh1—C62.236 (5)C36—H36A1.0000
Rh1—P22.2737 (13)C37—C381.513 (4)
Rh1—P12.2786 (14)C37—H37A0.9900
Rh2—C352.215 (5)C37—H37B0.9900
Rh2—C312.218 (5)C38—H38A0.9900
Rh2—C362.229 (5)C38—H38B0.9900
Rh2—C322.259 (5)C39—C401.518 (7)
Rh2—P222.2602 (14)C39—H39A0.9900
Rh2—P212.2702 (15)C39—H39B0.9900
Rh3—C652.200 (5)C40—H40A0.9900
Rh3—C612.205 (5)C40—H40B0.9900
Rh3—C622.239 (5)C41—C421.503 (8)
Rh3—C662.249 (6)C41—C451.506 (8)
Rh3—P322.2642 (14)C41—H41A1.0000
Rh3—P312.2797 (14)C42—C431.491 (9)
P1—C111.830 (5)C42—H42A0.9900
P1—C91.837 (4)C42—H42B0.9900
P1—C141.853 (5)C43—C441.530 (7)
P2—C101.821 (5)C43—H43A0.9900
P2—C171.843 (5)C43—H43B0.9900
P2—C201.852 (6)C44—C461.510 (8)
P21—C391.825 (5)C44—H44A1.0000
P21—C411.837 (5)C45—H45A0.9800
P21—C441.847 (6)C45—H45B0.9800
P22—C401.819 (5)C45—H45C0.9800
P22—C471.832 (6)C46—H46A0.9800
P22—C501.834 (6)C46—H46B0.9800
P31—C691.820 (6)C46—H46C0.9800
P31—C711.826 (5)C47—C481.510 (8)
P31—C741.850 (6)C47—C511.533 (8)
P32—C701.814 (5)C47—H47A1.0000
P32—C771.832 (5)C48—C491.502 (9)
P32—C801.850 (5)C48—H48A0.9900
C1—C21.398 (4)C48—H48B0.9900
C1—C8'1.479 (12)C49—C501.500 (8)
C1—C81.530 (13)C49—H49A0.9900
C1—H1A1.0000C49—H49B0.9900
C1—H1B1.0000C50—C521.515 (8)
C2—C31.416 (12)C50—H50A1.0000
C2—C3'1.614 (14)C51—H51A0.9800
C2—H2A1.0000C51—H51B0.9800
C2—H2B1.0000C51—H51C0.9800
C3—C41.535 (5)C52—H52A0.9800
C3—H3A0.9900C52—H52B0.9800
C3—H3B0.9900C52—H52C0.9800
C4—C51.641 (12)C61—C621.409 (4)
C4—H4A0.9900C61—C681.486 (7)
C4—H4B0.9900C61—H61A1.0000
C3'—C4'1.529 (5)C62—C631.481 (8)
C3'—H3C0.9900C62—H62A1.0000
C3'—H3D0.9900C63—C641.520 (4)
C4'—C51.439 (12)C63—H63A0.9900
C4'—H4C0.9900C63—H63B0.9900
C4'—H4D0.9900C64—C651.492 (8)
C5—C61.410 (4)C64—H64A0.9900
C5—H5A1.0000C64—H64B0.9900
C5—H5B1.0000C65—C661.402 (5)
C6—C71.514 (11)C65—H65A1.0000
C6—C7'1.564 (11)C66—C671.488 (8)
C6—H6A1.0000C66—H66A1.0000
C6—H6B1.0000C67—C681.527 (5)
C7—C81.542 (5)C67—H67A0.9900
C7—H7A0.9900C67—H67B0.9900
C7—H7B0.9900C68—H68A0.9900
C8—H8A0.9900C68—H68B0.9900
C8—H8B0.9900C69—C701.515 (7)
C7'—C8'1.536 (5)C69—H69A0.9900
C7'—H7C0.9900C69—H69B0.9900
C7'—H7D0.9900C70—H70A0.9900
C8'—H8C0.9900C70—H70B0.9900
C8'—H8D0.9900C71—C721.509 (7)
C9—C101.501 (6)C71—C751.517 (7)
C9—H9A0.9900C71—H71A1.0000
C9—H9B0.9900C72—C731.486 (8)
C10—H10A0.9900C72—H72A0.9900
C10—H10B0.9900C72—H72B0.9900
C11—C121.506 (7)C73—C741.521 (7)
C11—C151.509 (8)C73—H73A0.9900
C11—H11A1.0000C73—H73B0.9900
C12—C131.523 (8)C74—C761.496 (7)
C12—H12A0.9900C74—H74A1.0000
C12—H12B0.9900C75—H75A0.9800
C13—C141.529 (7)C75—H75B0.9800
C13—H13A0.9900C75—H75C0.9800
C13—H13B0.9900C76—H76A0.9800
C14—C161.509 (7)C76—H76B0.9800
C14—H14A1.0000C76—H76C0.9800
C15—H15A0.9800C77—C811.497 (7)
C15—H15B0.9800C77—C781.516 (8)
C15—H15C0.9800C77—H77A1.0000
C16—H16A0.9800C78—C791.509 (8)
C16—H16B0.9800C78—H78A0.9900
C16—H16C0.9800C78—H78B0.9900
C17—C211.497 (8)C79—C801.527 (7)
C17—C181.527 (8)C79—H79A0.9900
C17—H17A1.0000C79—H79B0.9900
C18—C191.505 (8)C80—C821.507 (7)
C18—H18A0.9900C80—H80A1.0000
C18—H18B0.9900C81—H81A0.9800
C19—C201.528 (7)C81—H81B0.9800
C19—H19A0.9900C81—H81C0.9800
C19—H19B0.9900C82—H82A0.9800
C20—C221.503 (7)C82—H82B0.9800
C20—H20A1.0000C82—H82C0.9800
C21—H21A0.9800B1—F21.346 (6)
C21—H21B0.9800B1—F11.368 (7)
C21—H21C0.9800B1—F41.371 (7)
C22—H22A0.9800B1—F31.379 (6)
C22—H22B0.9800B3—F121.344 (8)
C22—H22C0.9800B3—F111.360 (8)
C31—C321.403 (4)B3—F91.366 (7)
C31—C381.476 (8)B3—F101.378 (7)
C31—H31A1.0000B2—F7'1.213 (10)
C32—C331.489 (7)B2—F81.285 (9)
C32—H32A1.0000B2—F8'1.294 (11)
C33—C341.510 (4)B2—F51.313 (9)
C33—H33A0.9900B2—F6'1.398 (11)
C33—H33B0.9900B2—F71.419 (9)
C34—C351.464 (8)B2—F61.460 (10)
C34—H34A0.9900B2—F5'1.644 (12)
C34—H34B0.9900
C5—Rh1—C192.4 (2)C32—C33—H33B108.4
C5—Rh1—C281.2 (2)C34—C33—H33B108.4
C1—Rh1—C236.70 (12)H33A—C33—H33B107.4
C5—Rh1—C637.33 (13)C35—C34—C33116.7 (5)
C1—Rh1—C679.8 (2)C35—C34—H34A108.1
C2—Rh1—C691.7 (2)C33—C34—H34A108.1
C5—Rh1—P298.51 (15)C35—C34—H34B108.1
C1—Rh1—P2153.42 (15)C33—C34—H34B108.1
C2—Rh1—P2169.37 (14)H34A—C34—H34B107.3
C6—Rh1—P294.43 (15)C36—C35—C34127.6 (7)
C5—Rh1—P1150.27 (19)C36—C35—Rh272.2 (3)
C1—Rh1—P199.46 (15)C34—C35—Rh2107.0 (4)
C2—Rh1—P192.23 (15)C36—C35—H35A113.7
C6—Rh1—P1172.15 (19)C34—C35—H35A113.7
P2—Rh1—P182.78 (5)Rh2—C35—H35A113.7
C35—Rh2—C3194.5 (2)C35—C36—C37124.1 (7)
C35—Rh2—C3636.70 (12)C35—C36—Rh271.1 (3)
C31—Rh2—C3680.1 (2)C37—C36—Rh2111.5 (4)
C35—Rh2—C3280.8 (2)C35—C36—H36A114.2
C31—Rh2—C3236.52 (12)C37—C36—H36A114.2
C36—Rh2—C3288.9 (2)Rh2—C36—H36A114.2
C35—Rh2—P2296.78 (17)C36—C37—C38113.8 (5)
C31—Rh2—P22153.41 (15)C36—C37—H37A108.8
C36—Rh2—P2294.91 (18)C38—C37—H37A108.8
C32—Rh2—P22169.96 (15)C36—C37—H37B108.8
C35—Rh2—P21150.21 (16)C38—C37—H37B108.8
C31—Rh2—P2198.74 (16)H37A—C37—H37B107.7
C36—Rh2—P21172.88 (16)C31—C38—C37116.2 (5)
C32—Rh2—P2194.30 (16)C31—C38—H38A108.2
P22—Rh2—P2182.97 (6)C37—C38—H38A108.2
C65—Rh3—C6195.1 (2)C31—C38—H38B108.2
C65—Rh3—C6280.7 (2)C37—C38—H38B108.2
C61—Rh3—C6236.95 (13)H38A—C38—H38B107.4
C65—Rh3—C6636.71 (13)C40—C39—P21107.4 (4)
C61—Rh3—C6680.1 (2)C40—C39—H39A110.2
C62—Rh3—C6688.5 (2)P21—C39—H39A110.2
C65—Rh3—P3296.94 (17)C40—C39—H39B110.2
C61—Rh3—P32151.68 (16)P21—C39—H39B110.2
C62—Rh3—P32171.30 (16)H39A—C39—H39B108.5
C66—Rh3—P3294.59 (18)C39—C40—P22106.2 (4)
C65—Rh3—P31150.34 (18)C39—C40—H40A110.5
C61—Rh3—P3198.63 (16)P22—C40—H40A110.5
C62—Rh3—P3194.82 (17)C39—C40—H40B110.5
C66—Rh3—P31172.70 (18)P22—C40—H40B110.5
P32—Rh3—P3183.09 (5)H40A—C40—H40B108.7
C11—P1—C9107.7 (2)C42—C41—C45115.5 (5)
C11—P1—C1494.4 (2)C42—C41—P21104.2 (4)
C9—P1—C14103.1 (2)C45—C41—P21115.9 (4)
C11—P1—Rh1122.41 (18)C42—C41—H41A106.8
C9—P1—Rh1109.67 (15)C45—C41—H41A106.8
C14—P1—Rh1117.27 (17)P21—C41—H41A106.8
C10—P2—C17108.2 (2)C43—C42—C41106.6 (6)
C10—P2—C20104.7 (2)C43—C42—H42A110.4
C17—P2—C2095.0 (3)C41—C42—H42A110.4
C10—P2—Rh1109.00 (15)C43—C42—H42B110.4
C17—P2—Rh1124.76 (19)C41—C42—H42B110.4
C20—P2—Rh1113.03 (15)H42A—C42—H42B108.6
C39—P21—C41106.2 (3)C42—C43—C44108.7 (5)
C39—P21—C44103.2 (2)C42—C43—H43A110.0
C41—P21—C4494.8 (3)C44—C43—H43A110.0
C39—P21—Rh2109.54 (17)C42—C43—H43B110.0
C41—P21—Rh2122.78 (19)C44—C43—H43B110.0
C44—P21—Rh2118.00 (19)H43A—C43—H43B108.3
C40—P22—C47107.9 (3)C46—C44—C43115.0 (5)
C40—P22—C50104.1 (3)C46—C44—P21116.5 (4)
C47—P22—C5095.1 (3)C43—C44—P21103.9 (4)
C40—P22—Rh2109.13 (16)C46—C44—H44A107.0
C47—P22—Rh2123.43 (19)C43—C44—H44A107.0
C50—P22—Rh2115.00 (19)P21—C44—H44A107.0
C69—P31—C71107.3 (3)C41—C45—H45A109.5
C69—P31—C74103.5 (3)C41—C45—H45B109.5
C71—P31—C7494.4 (2)H45A—C45—H45B109.5
C69—P31—Rh3109.15 (18)C41—C45—H45C109.5
C71—P31—Rh3123.37 (19)H45A—C45—H45C109.5
C74—P31—Rh3116.79 (19)H45B—C45—H45C109.5
C70—P32—C77108.0 (3)C44—C46—H46A109.5
C70—P32—C80103.1 (3)C44—C46—H46B109.5
C77—P32—C8095.1 (2)H46A—C46—H46B109.5
C70—P32—Rh3108.96 (18)C44—C46—H46C109.5
C77—P32—Rh3125.7 (2)H46A—C46—H46C109.5
C80—P32—Rh3113.30 (19)H46B—C46—H46C109.5
C2—C1—C8'118.7 (7)C48—C47—C51114.2 (5)
C2—C1—C8134.5 (7)C48—C47—P22104.1 (4)
C2—C1—Rh172.6 (3)C51—C47—P22115.1 (4)
C8'—C1—Rh1113.4 (4)C48—C47—H47A107.7
C8—C1—Rh1105.3 (5)C51—C47—H47A107.7
C2—C1—H1A111.4P22—C47—H47A107.7
C8'—C1—H1A120.0C49—C48—C47106.7 (5)
C8—C1—H1A111.4C49—C48—H48A110.4
Rh1—C1—H1A111.4C47—C48—H48A110.4
C2—C1—H1B114.7C49—C48—H48B110.4
C8'—C1—H1B115.1C47—C48—H48B110.4
C8—C1—H1B107.1H48A—C48—H48B108.6
Rh1—C1—H1B115.5C50—C49—C48108.7 (5)
C1—C2—C3118.8 (8)C50—C49—H49A110.0
C1—C2—C3'128.7 (7)C48—C49—H49A110.0
C1—C2—Rh170.8 (3)C50—C49—H49B110.0
C3—C2—Rh1114.1 (5)C48—C49—H49B109.9
C3'—C2—Rh1101.6 (6)H49A—C49—H49B108.3
C1—C2—H2A115.3C49—C50—C52115.1 (5)
C3—C2—H2A115.3C49—C50—P22104.5 (5)
C3'—C2—H2A113.6C52—C50—P22116.6 (4)
Rh1—C2—H2A115.3C49—C50—H50A106.6
C1—C2—H2B114.3C52—C50—H50A106.6
C3—C2—H2B116.9P22—C50—H50A106.6
Rh1—C2—H2B113.6C47—C51—H51A109.5
C2—C3—C4111.4 (8)C47—C51—H51B109.5
C2—C3—H3A109.4H51A—C51—H51B109.5
C4—C3—H3A109.4C47—C51—H51C109.5
C2—C3—H3B109.4H51A—C51—H51C109.5
C4—C3—H3B109.4H51B—C51—H51C109.5
H3A—C3—H3B108.0C50—C52—H52A109.5
C3—C4—C5111.6 (8)C50—C52—H52B109.5
C3—C4—H4A109.3H52A—C52—H52B109.5
C5—C4—H4A109.3C50—C52—H52C109.5
C3—C4—H4B109.3H52A—C52—H52C109.5
C5—C4—H4B109.3H52B—C52—H52C109.5
H4A—C4—H4B108.0C62—C61—C68127.2 (6)
C4'—C3'—C2114.9 (10)C62—C61—Rh372.8 (3)
C4'—C3'—H3C108.6C68—C61—Rh3108.5 (4)
C2—C3'—H3C108.6C62—C61—H61A113.4
C4'—C3'—H3D108.6C68—C61—H61A113.4
C2—C3'—H3D108.6Rh3—C61—H61A113.4
H3C—C3'—H3D107.5C61—C62—C63123.4 (6)
C5—C4'—C3'107.2 (10)C61—C62—Rh370.2 (3)
C5—C4'—H4C110.3C63—C62—Rh3111.3 (4)
C3'—C4'—H4C110.3C61—C62—H62A114.6
C5—C4'—H4D110.3C63—C62—H62A114.6
C3'—C4'—H4D110.3Rh3—C62—H62A114.6
H4C—C4'—H4D108.5C62—C63—C64113.4 (5)
C6—C5—C4'108.9 (8)C62—C63—H63A108.9
C6—C5—C4133.4 (6)C64—C63—H63A108.9
C6—C5—Rh174.2 (3)C62—C63—H63B108.9
C4—C5—Rh1103.0 (5)C64—C63—H63B108.9
C6—C5—H5A111.9H63A—C63—H63B107.7
C4'—C5—H5A122.2C65—C64—C63116.2 (6)
C4—C5—H5A111.9C65—C64—H64A108.2
Rh1—C5—H5A111.9C63—C64—H64A108.2
C6—C5—H5B116.4C65—C64—H64B108.2
C4'—C5—H5B115.8C63—C64—H64B108.2
C4—C5—H5B106.3H64A—C64—H64B107.4
Rh1—C5—H5B117.1C66—C65—C64126.2 (6)
C5—C6—C7110.8 (7)C66—C65—Rh373.5 (3)
C5—C6—C7'137.7 (7)C64—C65—Rh3106.9 (4)
C5—C6—Rh168.5 (3)C66—C65—H65A114.0
C7—C6—Rh1111.2 (5)C64—C65—H65A114.0
C7'—C6—Rh1105.4 (5)Rh3—C65—H65A114.0
C5—C6—H6A118.7C65—C66—C67125.3 (7)
C7—C6—H6A118.7C65—C66—Rh369.8 (3)
C7'—C6—H6A101.2C67—C66—Rh3111.2 (4)
Rh1—C6—H6A118.7C65—C66—H66A114.0
C5—C6—H6B110.3C67—C66—H66A114.0
C7—C6—H6B129.6Rh3—C66—H66A114.0
C7'—C6—H6B110.9C66—C67—C68114.4 (5)
Rh1—C6—H6B110.1C66—C67—H67A108.7
C6—C7—C8107.4 (9)C68—C67—H67A108.7
C6—C7—H7A110.2C66—C67—H67B108.7
C8—C7—H7A110.2C68—C67—H67B108.7
C6—C7—H7B110.2H67A—C67—H67B107.6
C8—C7—H7B110.2C61—C68—C67115.4 (5)
H7A—C7—H7B108.5C61—C68—H68A108.4
C1—C8—C7109.7 (9)C67—C68—H68A108.4
C1—C8—H8A109.7C61—C68—H68B108.4
C7—C8—H8A109.7C67—C68—H68B108.4
C1—C8—H8B109.7H68A—C68—H68B107.5
C7—C8—H8B109.7C70—C69—P31107.4 (4)
H8A—C8—H8B108.2C70—C69—H69A110.2
C8'—C7'—C6110.8 (8)P31—C69—H69A110.2
C8'—C7'—H7C109.5C70—C69—H69B110.2
C6—C7'—H7C109.5P31—C69—H69B110.2
C8'—C7'—H7D109.5H69A—C69—H69B108.5
C6—C7'—H7D109.5C69—C70—P32106.9 (4)
H7C—C7'—H7D108.1C69—C70—H70A110.3
C1—C8'—C7'112.8 (8)P32—C70—H70A110.3
C1—C8'—H8C109.0C69—C70—H70B110.3
C7'—C8'—H8C109.0P32—C70—H70B110.3
C1—C8'—H8D109.0H70A—C70—H70B108.6
C7'—C8'—H8D109.0C72—C71—C75115.3 (5)
H8C—C8'—H8D107.8C72—C71—P31104.7 (4)
C10—C9—P1108.2 (3)C75—C71—P31116.4 (4)
C10—C9—H9A110.1C72—C71—H71A106.6
P1—C9—H9A110.1C75—C71—H71A106.6
C10—C9—H9B110.1P31—C71—H71A106.6
P1—C9—H9B110.1C73—C72—C71106.3 (4)
H9A—C9—H9B108.4C73—C72—H72A110.5
C9—C10—P2106.8 (3)C71—C72—H72A110.5
C9—C10—H10A110.4C73—C72—H72B110.5
P2—C10—H10A110.4C71—C72—H72B110.5
C9—C10—H10B110.4H72A—C72—H72B108.7
P2—C10—H10B110.4C72—C73—C74109.2 (5)
H10A—C10—H10B108.6C72—C73—H73A109.8
C12—C11—C15115.2 (5)C74—C73—H73A109.8
C12—C11—P1105.9 (4)C72—C73—H73B109.8
C15—C11—P1114.9 (4)C74—C73—H73B109.8
C12—C11—H11A106.8H73A—C73—H73B108.3
C15—C11—H11A106.8C76—C74—C73115.1 (5)
P1—C11—H11A106.8C76—C74—P31117.2 (4)
C11—C12—C13105.9 (5)C73—C74—P31104.2 (4)
C11—C12—H12A110.6C76—C74—H74A106.5
C13—C12—H12A110.6C73—C74—H74A106.5
C11—C12—H12B110.6P31—C74—H74A106.5
C13—C12—H12B110.6C71—C75—H75A109.5
H12A—C12—H12B108.7C71—C75—H75B109.5
C12—C13—C14108.8 (4)H75A—C75—H75B109.5
C12—C13—H13A109.9C71—C75—H75C109.5
C14—C13—H13A109.9H75A—C75—H75C109.5
C12—C13—H13B109.9H75B—C75—H75C109.5
C14—C13—H13B109.9C74—C76—H76A109.5
H13A—C13—H13B108.3C74—C76—H76B109.5
C16—C14—C13114.8 (4)H76A—C76—H76B109.5
C16—C14—P1117.0 (4)C74—C76—H76C109.5
C13—C14—P1104.8 (4)H76A—C76—H76C109.5
C16—C14—H14A106.5H76B—C76—H76C109.5
C13—C14—H14A106.5C81—C77—C78115.2 (5)
P1—C14—H14A106.5C81—C77—P32115.0 (4)
C11—C15—H15A109.5C78—C77—P32103.6 (4)
C11—C15—H15B109.5C81—C77—H77A107.6
H15A—C15—H15B109.5C78—C77—H77A107.6
C11—C15—H15C109.5P32—C77—H77A107.6
H15A—C15—H15C109.5C79—C78—C77107.0 (5)
H15B—C15—H15C109.5C79—C78—H78A110.3
C14—C16—H16A109.5C77—C78—H78A110.3
C14—C16—H16B109.5C79—C78—H78B110.3
H16A—C16—H16B109.5C77—C78—H78B110.3
C14—C16—H16C109.5H78A—C78—H78B108.6
H16A—C16—H16C109.5C78—C79—C80107.9 (5)
H16B—C16—H16C109.5C78—C79—H79A110.1
C21—C17—C18114.4 (4)C80—C79—H79A110.1
C21—C17—P2114.9 (4)C78—C79—H79B110.1
C18—C17—P2104.2 (4)C80—C79—H79B110.1
C21—C17—H17A107.6H79A—C79—H79B108.4
C18—C17—H17A107.6C82—C80—C79112.5 (5)
P2—C17—H17A107.6C82—C80—P32115.8 (4)
C19—C18—C17107.9 (5)C79—C80—P32104.7 (3)
C19—C18—H18A110.1C82—C80—H80A107.8
C17—C18—H18A110.1C79—C80—H80A107.8
C19—C18—H18B110.1P32—C80—H80A107.8
C17—C18—H18B110.1C77—C81—H81A109.5
H18A—C18—H18B108.4C77—C81—H81B109.5
C18—C19—C20108.3 (5)H81A—C81—H81B109.5
C18—C19—H19A110.0C77—C81—H81C109.5
C20—C19—H19A110.0H81A—C81—H81C109.5
C18—C19—H19B110.0H81B—C81—H81C109.5
C20—C19—H19B110.0C80—C82—H82A109.5
H19A—C19—H19B108.4C80—C82—H82B109.5
C22—C20—C19112.6 (5)H82A—C82—H82B109.5
C22—C20—P2115.8 (3)C80—C82—H82C109.5
C19—C20—P2105.3 (4)H82A—C82—H82C109.5
C22—C20—H20A107.6H82B—C82—H82C109.5
C19—C20—H20A107.6F2—B1—F1110.2 (5)
P2—C20—H20A107.6F2—B1—F4110.4 (5)
C17—C21—H21A109.5F1—B1—F4108.6 (5)
C17—C21—H21B109.5F2—B1—F3110.3 (5)
H21A—C21—H21B109.5F1—B1—F3108.7 (5)
C17—C21—H21C109.5F4—B1—F3108.5 (5)
H21A—C21—H21C109.5F12—B3—F11110.4 (6)
H21B—C21—H21C109.5F12—B3—F9110.0 (6)
C20—C22—H22A109.5F11—B3—F9109.1 (6)
C20—C22—H22B109.5F12—B3—F10109.3 (6)
H22A—C22—H22B109.5F11—B3—F10108.7 (6)
C20—C22—H22C109.5F9—B3—F10109.3 (5)
H22A—C22—H22C109.5F7'—B2—F8'126.5 (9)
H22B—C22—H22C109.5F7'—B2—F5109.9 (9)
C32—C31—C38128.2 (6)F8—B2—F5118.7 (7)
C32—C31—Rh273.3 (3)F8'—B2—F5122.9 (8)
C38—C31—Rh2107.2 (4)F7'—B2—F6'116.9 (8)
C32—C31—H31A113.3F8'—B2—F6'111.1 (8)
C38—C31—H31A113.3F8—B2—F7110.5 (8)
Rh2—C31—H31A113.3F8'—B2—F7123.4 (8)
C31—C32—C33123.8 (6)F5—B2—F7108.6 (7)
C31—C32—Rh270.1 (3)F6'—B2—F7124.9 (7)
C33—C32—Rh2109.1 (3)F8—B2—F6108.0 (7)
C31—C32—H32A115.0F5—B2—F6107.9 (7)
C33—C32—H32A115.0F7—B2—F6101.8 (5)
Rh2—C32—H32A115.0F7'—B2—F5'101.2 (8)
C32—C33—C34115.6 (5)F8'—B2—F5'97.8 (7)
C32—C33—H33A108.4F6'—B2—F5'93.6 (6)
C34—C33—H33A108.4

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: IM2198).

References

  • Axtell, A. T., Cobley, C. J., Klosin, J., Whiteker, G. T., Zanotti-Gerosa, A. & Abboud, K. A. (2005). Angew. Chem. Int. Ed.44, 5834–5838. [PubMed]
  • Burk, M. J. (1991). J. Am. Chem. Soc.113, 8518–8519.
  • Burk, J. M., Feaster, J. E. & Harlow, R. L. (1990). Organometallics, 9, 2653–2655.
  • Burk, M. J., Feaster, J. E., Nugent, W. A. & Harlow, R. L. (1993). J. Am. Chem. Soc.115, 10125–10138.
  • Burk, J. M., Gross, M. F. & Martinez, J. P. (1995). J. Am. Chem. Soc.117, 9376–9376.
  • Drexler, H.-J., Zhang, S., Sun, A., Spannenberg, A., Arrieta, A., Preetz, A. & Heller, D. (2004). Tetrahedron Asymmetry, 15, 2139–2150.
  • Fennis, P. J., Budzelaar, P. H. M., Frijns, J. H. G. & Orpen, A. G. (1990). J. Organomet. Chem.393, 287–298.
  • Fernandez, E., Gillon, A., Heslop, K., Horwood, E., Hyett, D. J., Orpen, A. G. & Pringle, P. G. (2000). Chem. Commun. pp. 1663–1664.
  • Flack, H. D. (1983). Acta Cryst. A39, 876–881.
  • Fox, M. E. & McCague, R. (2005). Chirality, 17, 177–185. [PubMed]
  • Heller, D., Holz, J., Komarov, I., Drexler, H.-J., You, J., Drauz, K. & Börner, A. (2002). Tetrahedron Asymmetry, 13, 2735–2741.
  • Schäffner, B., Andrushko, V., Holz, J., Verevkin, S. P. & Börner, A. (2008). ChemSusChem, 1, 934–940. [PubMed]
  • Schrock, R. R. & Osborn, J. A. (1971). J. Am. Chem. Soc.93, 2397–2407.
  • Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. [PubMed]
  • Stoe & Cie (2005). X-AREA, X-RED32 and X-SHAPE Stoe & Cie, Darmstadt, Germany.

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