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Acta Crystallographica Section E: Structure Reports Online logoLink to Acta Crystallographica Section E: Structure Reports Online
. 2012 Mar 28;68(Pt 4):m488. doi: 10.1107/S1600536812011786

Dicarbonyl­{3,3′-di-tert-butyl-5,5′-di­meth­oxy-2,2′-bis­[(4,4,5,5-tetra­phenyl-1,3,2-dioxa­phospho­lan-2-yl)­oxy-κP]biphen­yl}hydridorhodium(I) diethyl ether monosolvate

Detlef Selent a,*, Anke Spannenberg a, Armin Börner a
PMCID: PMC3343872  PMID: 22589846

Abstract

In the title compound, [Rh(C74H68O8P2)H(CO)2]·C4H10O, the C2HP2 coordination set at the RhI ion is arranged in a distorted trigonal–planar geometry with one P atom of the diphosphite mol­ecule and the H atom adopting the axial coordination sites.

Related literature  

For another crystal structure of a dicarbonyl hydrido complex of rhodium(I), see: Van Rooy et al. (1995, 1996). The title compound has recently been studied in solution, see: Selent et al. (2011). Structural information on this labile compound class is usually obtained by spectroscopy, see, for example: Dieleman et al. (2001); Axet et al. (2007).graphic file with name e-68-0m488-scheme1.jpg

Experimental  

Crystal data  

  • [Rh(C74H68O8P2)H(CO)2]·C4H10O

  • M r = 1381.28

  • Monoclinic, Inline graphic

  • a = 11.1489 (2) Å

  • b = 25.8458 (4) Å

  • c = 12.5941 (3) Å

  • β = 110.263 (2)°

  • V = 3404.43 (11) Å3

  • Z = 2

  • Mo Kα radiation

  • μ = 0.36 mm−1

  • T = 200 K

  • 0.40 × 0.35 × 0.15 mm

Data collection  

  • Stoe IPDS II diffractometer

  • Absorption correction: numerical (X-SHAPE and X-RED32; Stoe & Cie, 2005) T min = 0.835, T max = 0.959

  • 59171 measured reflections

  • 16262 independent reflections

  • 14238 reflections with I > 2σ(I)

  • R int = 0.026

Refinement  

  • R[F 2 > 2σ(F 2)] = 0.028

  • wR(F 2) = 0.063

  • S = 0.94

  • 16262 reflections

  • 834 parameters

  • 35 restraints

  • H atoms treated by a mixture of independent and constrained refinement

  • Δρmax = 0.66 e Å−3

  • Δρmin = −0.47 e Å−3

  • Absolute structure: Flack (1983), 7944 Friedel pairs

  • Flack parameter: −0.026 (11)

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

Supplementary Material

Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536812011786/bt5848sup1.cif

e-68-0m488-sup1.cif (41KB, cif)

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536812011786/bt5848Isup2.hkl

e-68-0m488-Isup2.hkl (794.8KB, hkl)

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

supplementary crystallographic information

Comment

The reaction of a mixture of dicarbonyl(acetylacetonato-κO,O')rhodium(I) and 3,3'-di-tert-butyl-5,5'-dimethoxy-2,2'-bis[(4,4,5,5-tetraphenyl-1,3,2-dioxaphospholan-2-yl)oxy]biphenyl under an atmosphere of hydrogen and carbon monoxide in toluene affords the elimination of acetylacetone and the formation of the rhodium hydrido complex which, after recrystallization, gives the title compound (figure 1). The distances Rh1—P1 = 2.3045 (5) Å and Rh1—P2 = 2.2913 (5) Å and the angle P1—Rh1—P2 = 109.66 (2)° do significantly differ from those (Rh1—P1 = 2.255 (3), Rh1—P2 = 2.239 (3) Å, P1—Rh1—P2 = 115.95 (9)°) found in the only molecular structure of a similar rhodium complex known to date (Van Rooy et al. 1995, 1996). In the solid state, the phosphorus atoms of the diphosphite molecule adopt formally different axial and equatorial sites of the idealized trigonal bipyramidal geometry around the rhodium center which is in contrast to the bisequatorial arrangement determined for both, the solution and the theoretical gas phase structure (Selent et al., 2011). The hydride could be found from difference Fourier map; the Rh1—H1 distance was refined to 1.42 (3) Å.

Experimental

A mixture of dicarbonyl(acetylacetonato-κO,O')rhodium(I) (0.5161 g, 2 mmol) and 3,3'-di-tert-butyl-5,5'-dimethoxy-2,2'-bis[(4,4,5,5-tetraphenyl-1,3,2-dioxaphospholan-2-yl)oxy]biphenyl (2.524 g, 2.2 mmol) was dissolved in toluene (50 ml). The resulting solution was transferred to an autoclave and then stirred under an atmosphere of carbon monoxide and hydrogen (1:1, 2.0 MPa) at 70°C for 2 h. The clear, pale yellow solution obtained after cooling and depressurization was evaporated to dryness in vacuo. The residue was crystallized from diethyl ether to give 2.108 g (1.613 mmol, 81%) of the title compound. 1H-NMR(toluene-D8): -10.00 (d, 1JHRh = 3.4 Hz) p.p.m.. 31P-NMR (toluene-D8): 166.1 (d, 1JPRh = 235 Hz) p.p.m.. Elemental analysis (calc. for C76H69O10P2Rh = 1307.229 g/mol): C, 69.75 (69.83); H, 5.48 (5.32); P, 4.56 (4.74); Rh, 7.73(7.87) %. ESI-TOF/HRMS: m/e 1317.3097 (M—CO+K)+, 1249.34397 (M-2CO)+. Crystals suitable for X-ray analysis were obtained by recrystallization from diethyl ether.

Refinement

H1 was found from difference Fourier map and refined freely. All other H atoms were placed in idealized positions with d(C—H) = 0.95 Å (CH), 0.99 Å (CH2) and 0.98 Å (CH3) and refined using a riding model with Uiso(H) fixed at 1.2 Ueq(C) for CH, CH2 and 1.5 Ueq(C) for CH3. The solvent atoms were only isotropically refined.

Figures

Fig. 1.

Fig. 1.

The molecular structure of the title compound; displacement ellipsoids are drawn at the 30% probability level. Hydrogen atoms except H1 are omitted for clarity.

Crystal data

[Rh(C74H68O8P2)H(CO)2]·C4H10O F(000) = 1444
Mr = 1381.28 Dx = 1.347 Mg m3
Monoclinic, P21 Mo Kα radiation, λ = 0.71073 Å
a = 11.1489 (2) Å Cell parameters from 15841 reflections
b = 25.8458 (4) Å θ = 1.7–28.4°
c = 12.5941 (3) Å µ = 0.36 mm1
β = 110.263 (2)° T = 200 K
V = 3404.43 (11) Å3 Prism, colourless
Z = 2 0.40 × 0.35 × 0.15 mm

Data collection

Stoe IPDS II diffractometer 16262 independent reflections
Radiation source: fine-focus sealed tube 14238 reflections with I > 2σ(I)
Graphite monochromator Rint = 0.026
ω scans θmax = 27.9°, θmin = 1.6°
Absorption correction: numerical (X-SHAPE and X-RED32; Stoe & Cie, 2005) h = −14→14
Tmin = 0.835, Tmax = 0.959 k = −34→34
59171 measured reflections l = −16→16

Refinement

Refinement on F2 Secondary atom site location: difference Fourier map
Least-squares matrix: full Hydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.028 H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.063 w = 1/[σ2(Fo2) + (0.0377P)2] where P = (Fo2 + 2Fc2)/3
S = 0.94 (Δ/σ)max = 0.001
16262 reflections Δρmax = 0.66 e Å3
834 parameters Δρmin = −0.47 e Å3
35 restraints Absolute structure: Flack (1983), 7944 Friedel pairs
Primary atom site location: structure-invariant direct methods Flack parameter: −0.026 (11)

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)

x y z Uiso*/Ueq
C77 1.0804 (4) 0.91333 (17) 0.5094 (3) 0.0878 (11)*
H77A 1.1508 0.9343 0.5030 0.132*
H77B 1.1042 0.8767 0.5147 0.132*
H77C 1.0626 0.9236 0.5774 0.132*
C78 0.9699 (5) 0.9212 (2) 0.4129 (4) 0.1113 (15)*
H78A 0.9490 0.9586 0.4077 0.134*
H78B 0.9908 0.9120 0.3449 0.134*
C79 0.7521 (5) 0.9016 (2) 0.3186 (4) 0.1172 (17)*
H79A 0.7315 0.8699 0.2715 0.141*
H79B 0.7635 0.9304 0.2713 0.141*
C80 0.6510 (6) 0.9131 (3) 0.3584 (6) 0.147 (2)*
H80A 0.5718 0.9181 0.2938 0.221*
H80B 0.6711 0.9449 0.4037 0.221*
H80C 0.6401 0.8845 0.4052 0.221*
O11 0.8631 (3) 0.89420 (13) 0.4096 (3) 0.1138 (10)*
C1 0.5785 (3) 0.53367 (10) 0.6920 (2) 0.0518 (7)
C2 0.5159 (2) 0.59995 (12) 0.9031 (2) 0.0456 (6)
C3 0.37567 (19) 0.72557 (7) 0.53935 (15) 0.0230 (4)
C4 0.44781 (18) 0.75555 (7) 0.65556 (16) 0.0248 (4)
C5 0.4165 (2) 0.73789 (8) 0.43790 (16) 0.0287 (4)
C6 0.3402 (2) 0.72021 (9) 0.33200 (16) 0.0377 (5)
H6 0.2633 0.7022 0.3239 0.045*
C7 0.3749 (2) 0.72856 (10) 0.23819 (19) 0.0507 (7)
H7 0.3217 0.7161 0.1664 0.061*
C8 0.4858 (2) 0.75483 (11) 0.24739 (19) 0.0573 (8)
H8 0.5071 0.7620 0.1821 0.069*
C9 0.5654 (3) 0.77058 (10) 0.35312 (17) 0.0522 (7)
H9 0.6438 0.7874 0.3610 0.063*
C10 0.5319 (2) 0.76214 (9) 0.44750 (19) 0.0375 (5)
H10 0.5879 0.7729 0.5198 0.045*
C11 0.23051 (19) 0.72664 (7) 0.50856 (15) 0.0242 (4)
C12 0.1685 (2) 0.68911 (8) 0.54920 (17) 0.0297 (4)
H12 0.2158 0.6610 0.5922 0.036*
C13 0.0377 (2) 0.69246 (9) 0.52739 (19) 0.0346 (5)
H13 −0.0041 0.6662 0.5544 0.042*
C14 −0.0318 (2) 0.73353 (9) 0.46688 (18) 0.0347 (5)
H14 −0.1209 0.7360 0.4534 0.042*
C15 0.0287 (2) 0.77076 (8) 0.42623 (17) 0.0338 (5)
H15 −0.0188 0.7992 0.3846 0.041*
C16 0.1582 (2) 0.76722 (8) 0.44540 (16) 0.0289 (4)
H16 0.1984 0.7928 0.4151 0.035*
C17 0.37177 (18) 0.75349 (6) 0.73659 (15) 0.0268 (4)
C18 0.27163 (19) 0.78775 (8) 0.72410 (17) 0.0316 (4)
H18 0.2514 0.8130 0.6657 0.038*
C19 0.2012 (2) 0.78574 (9) 0.79491 (17) 0.0406 (5)
H19 0.1335 0.8096 0.7850 0.049*
C20 0.2282 (3) 0.74940 (9) 0.8798 (2) 0.0542 (7)
H20 0.1775 0.7471 0.9266 0.065*
C21 0.3298 (3) 0.71647 (12) 0.8955 (2) 0.0654 (9)
H21 0.3513 0.6921 0.9557 0.078*
C22 0.4007 (3) 0.71839 (10) 0.82517 (19) 0.0470 (6)
H22 0.4705 0.6953 0.8375 0.056*
C23 0.4872 (2) 0.81179 (7) 0.65172 (18) 0.0287 (4)
C24 0.4264 (2) 0.84704 (7) 0.5669 (2) 0.0407 (5)
H24 0.3584 0.8356 0.5019 0.049*
C25 0.4628 (3) 0.89834 (8) 0.5752 (2) 0.0495 (6)
H25 0.4194 0.9218 0.5163 0.059*
C26 0.5618 (2) 0.91583 (9) 0.66831 (19) 0.0506 (7)
H26 0.5870 0.9511 0.6740 0.061*
C27 0.6238 (2) 0.88133 (7) 0.7529 (2) 0.0505 (7)
H27 0.6930 0.8928 0.8170 0.061*
C28 0.5857 (2) 0.83023 (8) 0.7449 (2) 0.0377 (5)
H28 0.6282 0.8071 0.8048 0.045*
C29 0.75300 (19) 0.63414 (7) 0.60830 (16) 0.0236 (4)
C30 0.75663 (16) 0.59539 (10) 0.53180 (14) 0.0268 (3)
C31 0.8683 (2) 0.56572 (7) 0.56195 (17) 0.0298 (4)
H31 0.8735 0.5385 0.5130 0.036*
C32 0.9723 (2) 0.57425 (8) 0.66043 (18) 0.0282 (4)
C33 0.96708 (19) 0.61368 (7) 0.73284 (16) 0.0253 (4)
H33 1.0380 0.6202 0.7998 0.030*
C34 0.85706 (19) 0.64382 (7) 0.70688 (16) 0.0225 (4)
C35 0.85814 (18) 0.68962 (7) 0.77842 (16) 0.0241 (4)
C36 0.85984 (19) 0.68565 (7) 0.88844 (16) 0.0240 (4)
C37 0.8629 (2) 0.72994 (8) 0.95425 (16) 0.0260 (4)
C38 0.8742 (2) 0.77697 (8) 0.90746 (17) 0.0285 (4)
H38 0.8807 0.8074 0.9516 0.034*
C39 0.8764 (2) 0.78185 (7) 0.79794 (18) 0.0277 (4)
C40 0.86457 (19) 0.73841 (7) 0.73202 (17) 0.0256 (4)
H40 0.8608 0.7414 0.6557 0.031*
C41 0.65315 (19) 0.58828 (10) 0.41376 (16) 0.0347 (5)
C42 0.6587 (4) 0.63533 (12) 0.3432 (2) 0.0581 (8)
H42A 0.6297 0.6659 0.3735 0.087*
H42B 0.6031 0.6298 0.2646 0.087*
H42C 0.7468 0.6406 0.3462 0.087*
C43 0.5178 (2) 0.58264 (12) 0.4152 (2) 0.0536 (8)
H43A 0.4934 0.6144 0.4453 0.080*
H43B 0.5143 0.5533 0.4633 0.080*
H43C 0.4585 0.5767 0.3381 0.080*
C44 0.6792 (3) 0.53988 (12) 0.3542 (2) 0.0529 (8)
H44A 0.6122 0.5363 0.2797 0.079*
H44B 0.6794 0.5092 0.4000 0.079*
H44C 0.7625 0.5432 0.3449 0.079*
C45 1.1894 (2) 0.55561 (10) 0.7650 (2) 0.0428 (5)
H45A 1.2151 0.5911 0.7556 0.064*
H45B 1.2572 0.5316 0.7643 0.064*
H45C 1.1751 0.5526 0.8372 0.064*
C46 0.8585 (2) 0.72778 (9) 1.07566 (17) 0.0338 (5)
C47 0.7439 (3) 0.69620 (10) 1.0791 (2) 0.0415 (6)
H47A 0.7534 0.6602 1.0588 0.062*
H47B 0.6651 0.7107 1.0252 0.062*
H47C 0.7399 0.6975 1.1556 0.062*
C48 0.9848 (3) 0.70463 (10) 1.15472 (19) 0.0438 (6)
H48A 0.9823 0.7021 1.2316 0.066*
H48B 1.0560 0.7269 1.1552 0.066*
H48C 0.9965 0.6701 1.1279 0.066*
C49 0.8440 (3) 0.78176 (9) 1.11995 (19) 0.0455 (6)
H49A 0.8371 0.7787 1.1952 0.068*
H49B 0.7667 0.7983 1.0681 0.068*
H49C 0.9188 0.8028 1.1249 0.068*
C50 0.8673 (3) 0.83944 (9) 0.6481 (2) 0.0445 (6)
H50A 0.9270 0.8189 0.6237 0.067*
H50B 0.8783 0.8762 0.6349 0.067*
H50C 0.7794 0.8290 0.6047 0.067*
C51 0.8631 (2) 0.51759 (7) 1.06368 (16) 0.0272 (4)
C52 0.9253 (2) 0.50443 (7) 0.96605 (16) 0.0258 (4)
C53 0.9628 (2) 0.52742 (7) 1.17970 (17) 0.0333 (5)
C54 0.9590 (3) 0.57220 (9) 1.23876 (18) 0.0436 (6)
H54 0.8948 0.5974 1.2056 0.052*
C55 1.0473 (3) 0.58061 (11) 1.3451 (2) 0.0635 (8)
H55 1.0434 0.6115 1.3845 0.076*
C56 1.1416 (3) 0.54451 (14) 1.3952 (2) 0.0684 (9)
H56 1.2029 0.5508 1.4681 0.082*
C57 1.1457 (3) 0.49955 (12) 1.3383 (2) 0.0553 (7)
H57 1.2091 0.4742 1.3722 0.066*
C58 1.0572 (2) 0.49143 (9) 1.23184 (19) 0.0410 (5)
H58 1.0609 0.4603 1.1930 0.049*
C59 0.7618 (2) 0.47876 (8) 1.06974 (19) 0.0297 (5)
C60 0.7693 (2) 0.45389 (8) 1.1700 (2) 0.0407 (5)
H60 0.8376 0.4619 1.2379 0.049*
C61 0.6786 (2) 0.41769 (9) 1.1717 (2) 0.0525 (7)
H61 0.6854 0.4009 1.2406 0.063*
C62 0.5784 (3) 0.40585 (10) 1.07396 (18) 0.0524 (7)
H62 0.5181 0.3800 1.0746 0.063*
C63 0.5666 (2) 0.43203 (9) 0.9752 (2) 0.0488 (6)
H63 0.4963 0.4250 0.9081 0.059*
C64 0.6570 (2) 0.46836 (8) 0.9739 (2) 0.0382 (5)
H64 0.6470 0.4866 0.9059 0.046*
C65 1.0696 (2) 0.51295 (9) 1.00494 (17) 0.0320 (5)
C66 1.1212 (2) 0.56104 (10) 1.04461 (18) 0.0391 (5)
H66 1.0658 0.5888 1.0457 0.047*
C67 1.25186 (18) 0.56925 (11) 1.0827 (2) 0.0546 (7)
H67 1.2854 0.6024 1.1102 0.065*
C68 1.3338 (3) 0.52943 (10) 1.0807 (2) 0.0651 (9)
H68 1.4237 0.5348 1.1078 0.078*
C69 1.2832 (2) 0.48177 (11) 1.0386 (2) 0.0635 (9)
H69 1.3387 0.4544 1.0355 0.076*
C70 1.1525 (2) 0.47359 (10) 1.0011 (2) 0.0458 (6)
H70 1.1191 0.4406 0.9724 0.055*
C71 0.8872 (2) 0.45146 (8) 0.91157 (18) 0.0300 (4)
C72 0.9014 (2) 0.40673 (8) 0.9771 (2) 0.0355 (5)
H72 0.9386 0.4089 1.0572 0.043*
C73 0.8617 (3) 0.35940 (9) 0.9266 (2) 0.0446 (6)
H73 0.8711 0.3293 0.9722 0.053*
C74 0.8087 (3) 0.35539 (10) 0.8108 (3) 0.0591 (8)
H74 0.7785 0.3230 0.7761 0.071*
C75 0.7999 (4) 0.39903 (10) 0.7457 (2) 0.0620 (8)
H75 0.7664 0.3964 0.6655 0.074*
C76 0.8393 (3) 0.44637 (9) 0.79552 (19) 0.0419 (6)
H76 0.8334 0.4760 0.7492 0.050*
O1 0.41561 (13) 0.67214 (5) 0.57154 (11) 0.0249 (3)
O2 0.56444 (13) 0.72564 (5) 0.70404 (11) 0.0258 (3)
O3 0.64584 (13) 0.66599 (5) 0.58506 (11) 0.0265 (3)
O4 0.87143 (14) 0.63686 (5) 0.93978 (11) 0.0266 (3)
O5 0.79305 (14) 0.56579 (5) 1.02459 (11) 0.0285 (3)
O6 0.86838 (14) 0.54274 (5) 0.87786 (11) 0.0258 (3)
O7 0.5764 (3) 0.49777 (8) 0.6399 (2) 0.0890 (9)
O8 0.4804 (2) 0.60351 (9) 0.97680 (18) 0.0691 (6)
O9 1.07528 (16) 0.54333 (6) 0.67518 (14) 0.0421 (4)
O10 0.89204 (16) 0.83106 (5) 0.76520 (13) 0.0341 (3)
P1 0.55672 (5) 0.66565 (2) 0.66426 (4) 0.02305 (10)
P2 0.78003 (5) 0.586778 (19) 0.90123 (4) 0.02370 (10)
Rh1 0.574142 (14) 0.594078 (6) 0.777762 (12) 0.02906 (4)
H1 0.444 (3) 0.5921 (15) 0.708 (2) 0.062 (7)*

Atomic displacement parameters (Å2)

U11 U22 U33 U12 U13 U23
C1 0.0549 (18) 0.0355 (13) 0.0473 (15) −0.0018 (12) −0.0045 (13) 0.0005 (12)
C2 0.0323 (11) 0.0520 (15) 0.0581 (13) 0.0060 (12) 0.0228 (10) 0.0182 (13)
C3 0.0249 (10) 0.0200 (8) 0.0234 (9) 0.0035 (7) 0.0074 (7) 0.0006 (7)
C4 0.0210 (10) 0.0247 (9) 0.0263 (9) 0.0047 (7) 0.0052 (7) −0.0008 (7)
C5 0.0339 (12) 0.0267 (9) 0.0273 (10) 0.0069 (8) 0.0129 (9) 0.0036 (8)
C6 0.0387 (13) 0.0452 (13) 0.0293 (11) 0.0082 (10) 0.0117 (9) 0.0003 (9)
C7 0.0610 (18) 0.0641 (17) 0.0280 (11) 0.0204 (14) 0.0166 (11) 0.0042 (11)
C8 0.076 (2) 0.0670 (17) 0.0435 (14) 0.0223 (16) 0.0392 (15) 0.0192 (13)
C9 0.0569 (17) 0.0479 (14) 0.0683 (18) 0.0032 (12) 0.0427 (15) 0.0115 (12)
C10 0.0402 (13) 0.0351 (11) 0.0430 (12) 0.0011 (10) 0.0215 (11) 0.0007 (9)
C11 0.0260 (10) 0.0246 (9) 0.0206 (8) 0.0017 (8) 0.0063 (7) −0.0038 (7)
C12 0.0292 (11) 0.0289 (10) 0.0298 (10) 0.0006 (8) 0.0086 (8) −0.0012 (8)
C13 0.0319 (12) 0.0392 (11) 0.0353 (11) −0.0044 (9) 0.0148 (9) −0.0018 (9)
C14 0.0250 (11) 0.0433 (12) 0.0345 (11) 0.0029 (9) 0.0084 (9) −0.0090 (9)
C15 0.0284 (11) 0.0361 (11) 0.0297 (10) 0.0103 (9) 0.0010 (8) −0.0031 (8)
C16 0.0299 (11) 0.0272 (10) 0.0268 (10) 0.0024 (8) 0.0062 (8) 0.0006 (7)
C17 0.0279 (11) 0.0267 (9) 0.0242 (9) 0.0002 (8) 0.0069 (8) −0.0060 (7)
C18 0.0301 (11) 0.0311 (10) 0.0324 (11) 0.0047 (9) 0.0092 (9) −0.0064 (8)
C19 0.0338 (13) 0.0451 (13) 0.0468 (13) 0.0075 (10) 0.0189 (10) −0.0047 (10)
C20 0.0677 (19) 0.0566 (16) 0.0576 (16) 0.0150 (14) 0.0463 (15) 0.0055 (13)
C21 0.093 (2) 0.0676 (18) 0.0553 (17) 0.0359 (18) 0.0504 (17) 0.0264 (14)
C22 0.0567 (16) 0.0516 (14) 0.0386 (12) 0.0277 (12) 0.0241 (12) 0.0081 (10)
C23 0.0251 (11) 0.0271 (9) 0.0362 (11) −0.0006 (8) 0.0136 (9) −0.0079 (8)
C24 0.0422 (14) 0.0289 (10) 0.0471 (13) −0.0032 (10) 0.0106 (11) 0.0014 (9)
C25 0.0583 (18) 0.0297 (11) 0.0613 (16) −0.0021 (11) 0.0217 (14) 0.0027 (11)
C26 0.0515 (17) 0.0288 (11) 0.0818 (19) −0.0114 (11) 0.0359 (15) −0.0152 (12)
C27 0.0357 (14) 0.0423 (13) 0.0729 (18) −0.0080 (11) 0.0179 (13) −0.0277 (13)
C28 0.0309 (12) 0.0329 (11) 0.0449 (12) 0.0017 (9) 0.0076 (10) −0.0102 (9)
C29 0.0230 (10) 0.0228 (8) 0.0267 (9) 0.0005 (7) 0.0108 (8) 0.0015 (7)
C30 0.0261 (8) 0.0258 (8) 0.0289 (8) 0.0002 (11) 0.0098 (7) −0.0012 (10)
C31 0.0312 (11) 0.0252 (10) 0.0340 (10) 0.0036 (8) 0.0126 (9) −0.0061 (8)
C32 0.0262 (11) 0.0260 (9) 0.0347 (10) 0.0041 (8) 0.0135 (8) 0.0000 (8)
C33 0.0219 (10) 0.0274 (8) 0.0265 (9) −0.0022 (7) 0.0083 (8) 0.0014 (7)
C34 0.0249 (10) 0.0205 (8) 0.0254 (9) −0.0012 (7) 0.0127 (8) 0.0005 (7)
C35 0.0199 (10) 0.0258 (9) 0.0259 (9) −0.0003 (7) 0.0070 (7) −0.0029 (7)
C36 0.0223 (10) 0.0243 (9) 0.0259 (9) −0.0024 (7) 0.0089 (8) 0.0004 (7)
C37 0.0220 (10) 0.0302 (10) 0.0233 (9) −0.0022 (8) 0.0045 (8) −0.0037 (8)
C38 0.0255 (11) 0.0278 (10) 0.0298 (10) −0.0024 (8) 0.0066 (8) −0.0080 (8)
C39 0.0271 (11) 0.0231 (9) 0.0341 (10) −0.0015 (8) 0.0123 (9) 0.0018 (8)
C40 0.0256 (11) 0.0255 (9) 0.0266 (9) −0.0002 (8) 0.0101 (8) 0.0005 (7)
C41 0.0315 (10) 0.0393 (12) 0.0298 (9) 0.0041 (11) 0.0061 (7) −0.0084 (10)
C42 0.069 (2) 0.0575 (17) 0.0351 (14) −0.0011 (15) 0.0024 (13) −0.0005 (12)
C43 0.0320 (12) 0.081 (2) 0.0413 (12) −0.0052 (13) 0.0050 (9) −0.0233 (13)
C44 0.0440 (17) 0.0582 (17) 0.0421 (14) 0.0096 (13) −0.0032 (12) −0.0272 (12)
C45 0.0266 (12) 0.0497 (13) 0.0498 (14) 0.0097 (10) 0.0102 (10) 0.0030 (11)
C46 0.0405 (13) 0.0381 (11) 0.0235 (9) −0.0011 (9) 0.0117 (9) −0.0047 (8)
C47 0.0504 (16) 0.0441 (14) 0.0369 (13) −0.0003 (12) 0.0238 (12) −0.0023 (10)
C48 0.0474 (15) 0.0489 (14) 0.0285 (11) 0.0017 (11) 0.0049 (10) −0.0038 (10)
C49 0.0662 (18) 0.0410 (12) 0.0310 (11) 0.0029 (12) 0.0191 (11) −0.0073 (9)
C50 0.0620 (17) 0.0319 (11) 0.0430 (13) −0.0021 (11) 0.0225 (12) 0.0072 (9)
C51 0.0318 (11) 0.0258 (9) 0.0262 (9) 0.0054 (8) 0.0128 (8) 0.0046 (7)
C52 0.0262 (11) 0.0271 (9) 0.0250 (9) 0.0050 (8) 0.0103 (8) 0.0060 (7)
C53 0.0379 (13) 0.0385 (11) 0.0250 (10) 0.0000 (9) 0.0127 (9) 0.0043 (8)
C54 0.0526 (16) 0.0460 (12) 0.0314 (11) 0.0057 (11) 0.0136 (10) −0.0014 (9)
C55 0.084 (2) 0.062 (2) 0.0370 (12) 0.0020 (15) 0.0107 (13) −0.0136 (12)
C56 0.072 (2) 0.089 (2) 0.0295 (13) 0.0022 (18) −0.0022 (13) −0.0054 (14)
C57 0.0528 (17) 0.0710 (19) 0.0356 (13) 0.0133 (14) 0.0069 (12) 0.0103 (12)
C58 0.0445 (14) 0.0481 (13) 0.0293 (11) 0.0094 (11) 0.0112 (10) 0.0067 (10)
C59 0.0369 (13) 0.0248 (10) 0.0343 (11) 0.0063 (9) 0.0211 (10) 0.0057 (8)
C60 0.0554 (16) 0.0352 (11) 0.0409 (12) 0.0044 (11) 0.0287 (12) 0.0091 (10)
C61 0.071 (2) 0.0415 (13) 0.0588 (16) 0.0022 (13) 0.0407 (16) 0.0163 (12)
C62 0.0511 (17) 0.0388 (13) 0.081 (2) −0.0036 (12) 0.0399 (16) 0.0117 (13)
C63 0.0361 (14) 0.0475 (14) 0.0645 (17) −0.0049 (11) 0.0196 (13) 0.0049 (12)
C64 0.0335 (13) 0.0384 (12) 0.0461 (13) 0.0018 (10) 0.0180 (11) 0.0111 (10)
C65 0.0288 (11) 0.0412 (12) 0.0262 (10) 0.0039 (9) 0.0098 (8) 0.0104 (8)
C66 0.0323 (12) 0.0510 (13) 0.0320 (11) −0.0076 (10) 0.0084 (9) 0.0029 (10)
C67 0.0355 (14) 0.0747 (18) 0.0444 (14) −0.0131 (13) 0.0023 (11) 0.0148 (13)
C68 0.0260 (14) 0.100 (2) 0.0613 (17) −0.0023 (15) 0.0052 (12) 0.0395 (17)
C69 0.0347 (15) 0.081 (2) 0.081 (2) 0.0246 (15) 0.0285 (15) 0.0445 (17)
C70 0.0333 (13) 0.0500 (14) 0.0572 (15) 0.0129 (11) 0.0196 (11) 0.0210 (12)
C71 0.0294 (12) 0.0295 (10) 0.0356 (11) 0.0037 (8) 0.0170 (9) 0.0009 (8)
C72 0.0394 (13) 0.0304 (11) 0.0401 (12) 0.0096 (9) 0.0180 (10) 0.0074 (9)
C73 0.0563 (16) 0.0260 (10) 0.0588 (15) 0.0044 (10) 0.0294 (13) 0.0051 (10)
C74 0.083 (2) 0.0314 (12) 0.0650 (18) −0.0071 (13) 0.0281 (17) −0.0115 (12)
C75 0.096 (3) 0.0431 (14) 0.0418 (14) −0.0058 (15) 0.0176 (16) −0.0098 (11)
C76 0.0628 (17) 0.0309 (11) 0.0324 (11) 0.0014 (11) 0.0169 (11) 0.0003 (9)
O1 0.0233 (7) 0.0216 (6) 0.0277 (7) 0.0013 (5) 0.0060 (5) −0.0010 (5)
O2 0.0208 (7) 0.0273 (7) 0.0261 (6) 0.0041 (5) 0.0041 (5) −0.0031 (5)
O3 0.0251 (7) 0.0269 (6) 0.0270 (7) 0.0056 (6) 0.0084 (6) −0.0006 (5)
O4 0.0296 (8) 0.0247 (7) 0.0222 (7) −0.0006 (6) 0.0047 (6) 0.0021 (5)
O5 0.0336 (8) 0.0256 (7) 0.0291 (7) 0.0061 (6) 0.0145 (6) 0.0048 (5)
O6 0.0300 (8) 0.0251 (7) 0.0225 (6) 0.0036 (6) 0.0092 (6) 0.0038 (5)
O7 0.115 (2) 0.0415 (11) 0.0759 (15) 0.0036 (13) −0.0104 (14) −0.0194 (11)
O8 0.0672 (13) 0.0842 (17) 0.0769 (13) 0.0133 (12) 0.0514 (11) 0.0264 (12)
O9 0.0313 (9) 0.0427 (9) 0.0463 (9) 0.0127 (7) 0.0056 (7) −0.0105 (7)
O10 0.0423 (9) 0.0219 (7) 0.0406 (8) −0.0021 (6) 0.0176 (7) 0.0014 (6)
P1 0.0218 (3) 0.0234 (2) 0.0234 (2) 0.0023 (2) 0.0071 (2) 0.00024 (19)
P2 0.0243 (2) 0.0229 (3) 0.0240 (2) 0.0010 (2) 0.00854 (17) 0.00250 (18)
Rh1 0.02251 (7) 0.02832 (7) 0.03357 (7) −0.00073 (8) 0.00617 (5) 0.00755 (8)

Geometric parameters (Å, º)

C77—C78 1.414 (5) C41—C42 1.520 (4)
C77—H77A 0.9800 C41—C43 1.523 (3)
C77—H77B 0.9800 C41—C44 1.537 (3)
C77—H77C 0.9800 C42—H42A 0.9800
C78—O11 1.369 (4) C42—H42B 0.9800
C78—H78A 0.9900 C42—H42C 0.9800
C78—H78B 0.9900 C43—H43A 0.9800
C79—O11 1.377 (4) C43—H43B 0.9800
C79—C80 1.415 (5) C43—H43C 0.9800
C79—H79A 0.9900 C44—H44A 0.9800
C79—H79B 0.9900 C44—H44B 0.9800
C80—H80A 0.9800 C44—H44C 0.9800
C80—H80B 0.9800 C45—O9 1.415 (3)
C80—H80C 0.9800 C45—H45A 0.9800
C1—O7 1.132 (3) C45—H45B 0.9800
C1—Rh1 1.909 (3) C45—H45C 0.9800
C2—O8 1.133 (3) C46—C47 1.529 (4)
C2—Rh1 1.909 (2) C46—C49 1.532 (3)
C3—O1 1.464 (2) C46—C48 1.536 (3)
C3—C11 1.528 (3) C47—H47A 0.9800
C3—C5 1.531 (3) C47—H47B 0.9800
C3—C4 1.604 (3) C47—H47C 0.9800
C4—O2 1.453 (2) C48—H48A 0.9800
C4—C23 1.524 (3) C48—H48B 0.9800
C4—C17 1.537 (3) C48—H48C 0.9800
C5—C6 1.388 (3) C49—H49A 0.9800
C5—C10 1.398 (3) C49—H49B 0.9800
C6—C7 1.3814 (18) C49—H49C 0.9800
C6—H6 0.9500 C50—O10 1.421 (3)
C7—C8 1.3797 (19) C50—H50A 0.9800
C7—H7 0.9500 C50—H50B 0.9800
C8—C9 1.3811 (19) C50—H50C 0.9800
C8—H8 0.9500 C51—O5 1.462 (2)
C9—C10 1.3811 (18) C51—C53 1.520 (3)
C9—H9 0.9500 C51—C59 1.532 (3)
C10—H10 0.9500 C51—C52 1.643 (3)
C11—C12 1.387 (3) C52—O6 1.459 (2)
C11—C16 1.392 (3) C52—C71 1.524 (3)
C12—C13 1.390 (3) C52—C65 1.527 (3)
C12—H12 0.9500 C53—C54 1.385 (2)
C13—C14 1.378 (3) C53—C58 1.387 (2)
C13—H13 0.9500 C54—C55 1.377 (4)
C14—C15 1.372 (3) C54—H54 0.9500
C14—H14 0.9500 C55—C56 1.384 (4)
C15—C16 1.382 (3) C55—H55 0.9500
C15—H15 0.9500 C56—C57 1.374 (4)
C16—H16 0.9500 C56—H56 0.9500
C17—C22 1.386 (2) C57—C58 1.378 (4)
C17—C18 1.391 (2) C57—H57 0.9500
C18—C19 1.3779 (18) C58—H58 0.9500
C18—H18 0.9500 C59—C64 1.385 (3)
C19—C20 1.3754 (18) C59—C60 1.393 (3)
C19—H19 0.9500 C60—C61 1.3835 (19)
C20—C21 1.3751 (18) C60—H60 0.9500
C20—H20 0.9500 C61—C62 1.3805 (19)
C21—C22 1.3778 (18) C61—H61 0.9500
C21—H21 0.9500 C62—C63 1.3817 (19)
C22—H22 0.9500 C62—H62 0.9500
C23—C28 1.385 (3) C63—C64 1.3814 (19)
C23—C24 1.389 (3) C63—H63 0.9500
C24—C25 1.3800 (18) C64—H64 0.9500
C24—H24 0.9500 C65—C70 1.386 (3)
C25—C26 1.3791 (18) C65—C66 1.388 (3)
C25—H25 0.9500 C66—C67 1.3835 (19)
C26—C27 1.3775 (18) C66—H66 0.9500
C26—H26 0.9500 C67—C68 1.3823 (19)
C27—C28 1.3802 (18) C67—H67 0.9500
C27—H27 0.9500 C68—C69 1.382 (2)
C28—H28 0.9500 C68—H68 0.9500
C29—O3 1.396 (2) C69—C70 1.3840 (19)
C29—C34 1.397 (3) C69—H69 0.9500
C29—C30 1.400 (3) C70—H70 0.9500
C30—C31 1.398 (3) C71—C76 1.378 (3)
C30—C41 1.545 (2) C71—C72 1.397 (3)
C31—C32 1.391 (3) C72—C73 1.379 (3)
C31—H31 0.9500 C72—H72 0.9500
C32—O9 1.358 (2) C73—C74 1.375 (4)
C32—C33 1.382 (3) C73—H73 0.9500
C33—C34 1.393 (3) C74—C75 1.378 (4)
C33—H33 0.9500 C74—H74 0.9500
C34—C35 1.485 (3) C75—C76 1.376 (3)
C35—C36 1.383 (3) C75—H75 0.9500
C35—C40 1.402 (3) C76—H76 0.9500
C36—O4 1.403 (2) O1—P1 1.6106 (14)
C36—C37 1.407 (3) O2—P1 1.6224 (14)
C37—C38 1.375 (3) O3—P1 1.6336 (14)
C37—C46 1.548 (3) O4—P2 1.6146 (14)
C38—C39 1.394 (3) O5—P2 1.6039 (14)
C38—H38 0.9500 O6—P2 1.5979 (14)
C39—O10 1.367 (2) P1—Rh1 2.3045 (5)
C39—C40 1.375 (3) P2—Rh1 2.2913 (5)
C40—H40 0.9500 Rh1—H1 1.42 (3)
C78—C77—H77A 109.5 H43A—C43—H43B 109.5
C78—C77—H77B 109.5 C41—C43—H43C 109.5
H77A—C77—H77B 109.5 H43A—C43—H43C 109.5
C78—C77—H77C 109.5 H43B—C43—H43C 109.5
H77A—C77—H77C 109.5 C41—C44—H44A 109.5
H77B—C77—H77C 109.5 C41—C44—H44B 109.5
O11—C78—C77 116.2 (4) H44A—C44—H44B 109.5
O11—C78—H78A 108.2 C41—C44—H44C 109.5
C77—C78—H78A 108.2 H44A—C44—H44C 109.5
O11—C78—H78B 108.2 H44B—C44—H44C 109.5
C77—C78—H78B 108.2 O9—C45—H45A 109.5
H78A—C78—H78B 107.4 O9—C45—H45B 109.5
O11—C79—C80 109.3 (5) H45A—C45—H45B 109.5
O11—C79—H79A 109.8 O9—C45—H45C 109.5
C80—C79—H79A 109.8 H45A—C45—H45C 109.5
O11—C79—H79B 109.8 H45B—C45—H45C 109.5
C80—C79—H79B 109.8 C47—C46—C49 106.3 (2)
H79A—C79—H79B 108.3 C47—C46—C48 111.1 (2)
C79—C80—H80A 109.5 C49—C46—C48 107.92 (19)
C79—C80—H80B 109.5 C47—C46—C37 111.10 (18)
H80A—C80—H80B 109.5 C49—C46—C37 111.75 (18)
C79—C80—H80C 109.5 C48—C46—C37 108.60 (18)
H80A—C80—H80C 109.5 C46—C47—H47A 109.5
H80B—C80—H80C 109.5 C46—C47—H47B 109.5
C78—O11—C79 118.4 (4) H47A—C47—H47B 109.5
O7—C1—Rh1 177.5 (3) C46—C47—H47C 109.5
O8—C2—Rh1 179.4 (2) H47A—C47—H47C 109.5
O1—C3—C11 106.33 (15) H47B—C47—H47C 109.5
O1—C3—C5 106.10 (14) C46—C48—H48A 109.5
C11—C3—C5 112.30 (15) C46—C48—H48B 109.5
O1—C3—C4 101.22 (13) H48A—C48—H48B 109.5
C11—C3—C4 112.02 (15) C46—C48—H48C 109.5
C5—C3—C4 117.43 (16) H48A—C48—H48C 109.5
O2—C4—C23 107.17 (16) H48B—C48—H48C 109.5
O2—C4—C17 108.77 (14) C46—C49—H49A 109.5
C23—C4—C17 106.57 (15) C46—C49—H49B 109.5
O2—C4—C3 102.67 (14) H49A—C49—H49B 109.5
C23—C4—C3 119.38 (16) C46—C49—H49C 109.5
C17—C4—C3 111.80 (16) H49A—C49—H49C 109.5
C6—C5—C10 118.05 (19) H49B—C49—H49C 109.5
C6—C5—C3 118.22 (19) O10—C50—H50A 109.5
C10—C5—C3 123.49 (18) O10—C50—H50B 109.5
C7—C6—C5 120.7 (2) H50A—C50—H50B 109.5
C7—C6—H6 119.6 O10—C50—H50C 109.5
C5—C6—H6 119.6 H50A—C50—H50C 109.5
C8—C7—C6 120.9 (2) H50B—C50—H50C 109.5
C8—C7—H7 119.6 O5—C51—C53 107.98 (15)
C6—C7—H7 119.6 O5—C51—C59 104.95 (16)
C7—C8—C9 118.9 (2) C53—C51—C59 111.58 (17)
C7—C8—H8 120.5 O5—C51—C52 103.82 (14)
C9—C8—H8 120.5 C53—C51—C52 113.35 (17)
C10—C9—C8 120.6 (2) C59—C51—C52 114.28 (16)
C10—C9—H9 119.7 O6—C52—C71 106.68 (16)
C8—C9—H9 119.7 O6—C52—C65 106.17 (15)
C9—C10—C5 120.7 (2) C71—C52—C65 111.83 (17)
C9—C10—H10 119.6 O6—C52—C51 104.14 (14)
C5—C10—H10 119.6 C71—C52—C51 113.51 (16)
C12—C11—C16 118.27 (19) C65—C52—C51 113.65 (16)
C12—C11—C3 120.83 (17) C54—C53—C58 117.7 (2)
C16—C11—C3 120.76 (17) C54—C53—C51 120.52 (18)
C11—C12—C13 120.4 (2) C58—C53—C51 121.69 (17)
C11—C12—H12 119.8 C55—C54—C53 120.6 (2)
C13—C12—H12 119.8 C55—C54—H54 119.7
C14—C13—C12 120.5 (2) C53—C54—H54 119.7
C14—C13—H13 119.7 C54—C55—C56 120.8 (2)
C12—C13—H13 119.7 C54—C55—H55 119.6
C15—C14—C13 119.4 (2) C56—C55—H55 119.6
C15—C14—H14 120.3 C57—C56—C55 119.3 (3)
C13—C14—H14 120.3 C57—C56—H56 120.3
C14—C15—C16 120.5 (2) C55—C56—H56 120.3
C14—C15—H15 119.8 C56—C57—C58 119.6 (3)
C16—C15—H15 119.8 C56—C57—H57 120.2
C15—C16—C11 120.9 (2) C58—C57—H57 120.2
C15—C16—H16 119.6 C57—C58—C53 121.9 (2)
C11—C16—H16 119.6 C57—C58—H58 119.0
C22—C17—C18 117.48 (19) C53—C58—H58 119.0
C22—C17—C4 121.93 (16) C64—C59—C60 117.9 (2)
C18—C17—C4 120.58 (15) C64—C59—C51 119.84 (18)
C19—C18—C17 121.18 (18) C60—C59—C51 122.2 (2)
C19—C18—H18 119.4 C61—C60—C59 120.8 (2)
C17—C18—H18 119.4 C61—C60—H60 119.6
C20—C19—C18 120.6 (2) C59—C60—H60 119.6
C20—C19—H19 119.7 C62—C61—C60 120.4 (2)
C18—C19—H19 119.7 C62—C61—H61 119.8
C21—C20—C19 118.8 (2) C60—C61—H61 119.8
C21—C20—H20 120.6 C61—C62—C63 119.3 (2)
C19—C20—H20 120.6 C61—C62—H62 120.4
C20—C21—C22 120.8 (2) C63—C62—H62 120.4
C20—C21—H21 119.6 C64—C63—C62 120.1 (2)
C22—C21—H21 119.6 C64—C63—H63 120.0
C21—C22—C17 121.1 (2) C62—C63—H63 120.0
C21—C22—H22 119.5 C63—C64—C59 121.3 (2)
C17—C22—H22 119.5 C63—C64—H64 119.3
C28—C23—C24 117.27 (19) C59—C64—H64 119.3
C28—C23—C4 117.01 (18) C70—C65—C66 118.1 (2)
C24—C23—C4 125.52 (18) C70—C65—C52 121.6 (2)
C25—C24—C23 121.3 (2) C66—C65—C52 120.26 (19)
C25—C24—H24 119.3 C67—C66—C65 121.2 (2)
C23—C24—H24 119.3 C67—C66—H66 119.4
C26—C25—C24 120.5 (2) C65—C66—H66 119.4
C26—C25—H25 119.8 C68—C67—C66 120.2 (3)
C24—C25—H25 119.8 C68—C67—H67 119.9
C27—C26—C25 119.0 (2) C66—C67—H67 119.9
C27—C26—H26 120.5 C69—C68—C67 119.1 (2)
C25—C26—H26 120.5 C69—C68—H68 120.5
C26—C27—C28 120.2 (2) C67—C68—H68 120.5
C26—C27—H27 119.9 C68—C69—C70 120.6 (3)
C28—C27—H27 119.9 C68—C69—H69 119.7
C27—C28—C23 121.7 (2) C70—C69—H69 119.7
C27—C28—H28 119.2 C69—C70—C65 120.8 (2)
C23—C28—H28 119.2 C69—C70—H70 119.6
O3—C29—C34 117.88 (16) C65—C70—H70 119.6
O3—C29—C30 120.28 (16) C76—C71—C72 118.1 (2)
C34—C29—C30 121.78 (17) C76—C71—C52 120.57 (19)
C31—C30—C29 116.15 (16) C72—C71—C52 121.4 (2)
C31—C30—C41 119.61 (18) C73—C72—C71 120.6 (2)
C29—C30—C41 123.87 (18) C73—C72—H72 119.7
C32—C31—C30 122.95 (18) C71—C72—H72 119.7
C32—C31—H31 118.5 C74—C73—C72 120.5 (2)
C30—C31—H31 118.5 C74—C73—H73 119.8
O9—C32—C33 124.77 (19) C72—C73—H73 119.8
O9—C32—C31 115.64 (17) C73—C74—C75 119.0 (2)
C33—C32—C31 119.53 (18) C73—C74—H74 120.5
C32—C33—C34 119.48 (18) C75—C74—H74 120.5
C32—C33—H33 120.3 C76—C75—C74 120.7 (3)
C34—C33—H33 120.3 C76—C75—H75 119.6
C33—C34—C29 120.07 (17) C74—C75—H75 119.6
C33—C34—C35 118.81 (17) C75—C76—C71 120.9 (2)
C29—C34—C35 120.77 (17) C75—C76—H76 119.5
C36—C35—C40 119.96 (17) C71—C76—H76 119.5
C36—C35—C34 122.90 (17) C3—O1—P1 115.21 (11)
C40—C35—C34 117.05 (17) C4—O2—P1 115.76 (11)
C35—C36—O4 119.71 (16) C29—O3—P1 121.75 (12)
C35—C36—C37 121.26 (18) C36—O4—P2 129.38 (13)
O4—C36—C37 118.72 (17) C51—O5—P2 118.22 (12)
C38—C37—C36 117.00 (18) C52—O6—P2 118.46 (12)
C38—C37—C46 119.60 (18) C32—O9—C45 117.47 (17)
C36—C37—C46 123.37 (18) C39—O10—C50 117.12 (16)
C37—C38—C39 122.65 (18) O1—P1—O2 93.35 (7)
C37—C38—H38 118.7 O1—P1—O3 101.81 (7)
C39—C38—H38 118.7 O2—P1—O3 101.83 (7)
O10—C39—C40 124.98 (18) O1—P1—Rh1 112.62 (5)
O10—C39—C38 115.50 (17) O2—P1—Rh1 126.26 (5)
C40—C39—C38 119.52 (18) O3—P1—Rh1 116.40 (5)
C39—C40—C35 119.39 (18) O6—P2—O5 94.75 (7)
C39—C40—H40 120.3 O6—P2—O4 105.15 (8)
C35—C40—H40 120.3 O5—P2—O4 98.27 (7)
C42—C41—C43 109.0 (2) O6—P2—Rh1 118.05 (6)
C42—C41—C44 108.3 (2) O5—P2—Rh1 114.74 (6)
C43—C41—C44 106.5 (2) O4—P2—Rh1 121.17 (5)
C42—C41—C30 107.4 (2) C1—Rh1—C2 127.99 (13)
C43—C41—C30 114.37 (17) C1—Rh1—P2 95.80 (9)
C44—C41—C30 111.23 (19) C2—Rh1—P2 89.60 (7)
C41—C42—H42A 109.5 C1—Rh1—P1 108.58 (9)
C41—C42—H42B 109.5 C2—Rh1—P1 117.99 (9)
H42A—C42—H42B 109.5 P2—Rh1—P1 109.662 (19)
C41—C42—H42C 109.5 C1—Rh1—H1 80.9 (14)
H42A—C42—H42C 109.5 C2—Rh1—H1 86.9 (10)
H42B—C42—H42C 109.5 P2—Rh1—H1 172.1 (14)
C41—C43—H43A 109.5 P1—Rh1—H1 78.3 (14)
C41—C43—H43B 109.5

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: BT5848).

References

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Associated Data

This section collects any data citations, data availability statements, or supplementary materials included in this article.

Supplementary Materials

Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536812011786/bt5848sup1.cif

e-68-0m488-sup1.cif (41KB, cif)

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536812011786/bt5848Isup2.hkl

e-68-0m488-Isup2.hkl (794.8KB, hkl)

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


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