(Acetyl­acetonato-κ2O,O′)carbon­yl[tris­(naphthalen-1-yl)phosphane-κP]rhodium(I) acetone hemisolvate

Ogutu, H.; Meijboom, R.

doi:10.1107/S1600536812008148

metal-organic compounds

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ISSN: 2056-9890

Volume 68| Part 4| April 2012| Page m394

doi:10.1107/S1600536812008148

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(Acetylacetonato-κ²O,O′)carbonyl[tris(naphthalen-1-yl)phosphane-κP]rhodium(I) acetone hemisolvate

Hezron Ogutu ^a and Reinout Meijboom ^a ^*

^aResearch Centre for Synthesis and Catalysis, Department of Chemistry, University of Johannesburg, PO Box 524, Auckland Park, 2006 Johannesburg, South Africa
^*Correspondence e-mail: rmeijboom@uj.ac.za

(Received 17 February 2012; accepted 23 February 2012; online 10 March 2012)

The title compound, [Rh(C₅H₇O₂)(C₃₀H₂₁P)(CO)]·0.5C₃H₆O, has two different complex molecules in the asymmetric unit, with the Rh^I atoms in slightly distorted square-planar coordination environments. The molecules are packed as two monomeric molecules with one acetone solvent molecule sitting at the centre.

Related literature

For related literature on the catalytic activities of rhodium phosphine adducts, see: Carraz et al. (2000 ); Moloy & Wegman (1989 ). For related complexes, see: Bonati & Wilkinson (1964 ); Brink et al. (2007 ); Leipoldt et al. (1978 ); Janse van Rensburg et al. (2006 ).

Experimental

Crystal data

[Rh(C₅H₇O₂)(C₃₀H₂₁P)(CO)]·0.5C₃H₆O
M_r = 671.51
Monoclinic, P 2₁ /c
a = 19.8780 (5) Å
b = 16.9350 (5) Å
c = 18.8060 (4) Å
β = 102.916 (1)°
V = 6170.6 (3) Å³
Z = 8
Cu Kα radiation
μ = 5.27 mm⁻¹
T = 173 K
0.15 × 0.09 × 0.04 mm

Data collection

Bruker APEXII CCD diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2007 ) T_min = 0.505, T_max = 0.817
105322 measured reflections
10278 independent reflections
9730 reflections with I > 2σ(I)
R_int = 0.043

Refinement

R[F² > 2σ(F²)] = 0.028
wR(F²) = 0.068
S = 1.08
10278 reflections
745 parameters
240 restraints
H-atom parameters constrained
Δρ_max = 1.56 e Å⁻³
Δρ_min = −0.59 e Å⁻³

Data collection: APEX2 (Bruker, 2007); cell refinement: SAINT-Plus (Bruker, 2007); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL.

Supporting information

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536812008148/hg5181sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536812008148/hg5181Isup2.hkl

checkCIF report

Comment top

Acetylacetonate has two O-donor atoms with equivalent σ-electron donor capabilities. The high symmetry of dicarbonyl(acetylacetonate)rhodium(I) complexes promotes easy carbonyl displacement of either carbonyl group with a variety of phosphines, phosphites and arsines. (Bonati & Wilkinson, 1964). This work is part of an ongoing investigation aimed at determing the steric effects induced by various phosphine ligands on a rhodium(I) metal centre. Previous work illustrating the catalytic importance of the rhodium(I) square- planar moieties has been conducted on rhodium mono- and di-phosphine complexes containing the symmetrical bidentate ligand, acac (acac = acetylacetonate) (Moloy & Wegman, 1989). Symmetrical di-phosphine ligands result in the production of acetaldehyde, whereas unsymmetrical di-phosphine ligands are more stable and efficient catalysts for the carbonylation of methanol to acetic acid (Carraz et al., 2000).

In the title compound, the Rh lies at the base of acetylacetonato ring. The coordination polyhedron around the Rh atom shows a slightly distorted square-planar arrangement. A larger trans influence of the phosphine ligand with respect to the carbonyl ligand is indicated by the longer Rh—O2 2.0633 (17) Å) bond compared to Rh—O3 2.0380 (17) Å) bond which is trans to the carbonyl ligand. The steric demand of the phosphine is indicated by the smaller O3—Rh1—P1 angle, 92.78 (5)°), compared to the carbonyl ligand (O2—Rh1—C1 = 90.07 (9)°). Similar geometries have been observed for related complexes [Brink et al. (2007); Leipoldt et al. (1978); Janse van Rensburg et al. (2006)].

Spectroscopic characteristics of the current compound are similar to that reported previously by Brink et al. (2007), and we refer at Brink et al. (2007) for additional discussion on the spectroscopy of these types of compounds.

Related literature top

For related literature on the catalytic activities of rhodium phosphine adducts, see: Carraz et al. (2000); Moloy & Wegman (1989). For related complexes, see: Bonati & Wilkinson (1964); Brink et al. (2007); Leipoldt et al. (1978); Janse van Rensburg et al. (2006).

Experimental top

A solution of [Rh(acac)(CO)₂] (25.8 mg, 0.1 mmol) in acetone (5 cm³) was slowly added to a solution of [P(C₁₀H₇)] (41.2 mg, 0.1 mmol) in acetone (5 cm³) at room temperature, the mixture was then stirred for 10 min. Slow evaporation of the solvent afforded the title compound as a yellow crystalline solid.Spectroscopic analysis: ³¹P{H} NMR (CDCl₃, 161.99 MHz, p.p.m.):46.42 [d, ¹J(Rh—P) = 179.81 Hz]; IR ν(CO): 1971.2 cm^-1; (CD₂Cl₂) ν(CO): 1982.8 cm^-1.

Structure description top

For related literature on the catalytic activities of rhodium phosphine adducts, see: Carraz et al. (2000); Moloy & Wegman (1989). For related complexes, see: Bonati & Wilkinson (1964); Brink et al. (2007); Leipoldt et al. (1978); Janse van Rensburg et al. (2006).

Computing details top

Data collection: APEX2 (Bruker, 2007); cell refinement: SAINT-Plus (Bruker, 2007); data reduction: SAINT-Plus (Bruker, 2007); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Figures top

Fig. 1. Molecular structure of the title compound showing 50% probability displacement ellipsoids.

(Acetylacetonato-κ²O,O')carbonyl[tris(naphthalen- 1-yl)phosphane-κP]rhodium(I) acetone hemisolvate top

Crystal data top

[Rh(C₅H₇O₂)(C₃₀H₂₁P)(CO)]·0.5C₃H₆O	F(000) = 2752
M_r = 671.51	D_x = 1.446 Mg m⁻³
Monoclinic, P2₁/c	Cu Kα radiation, λ = 1.54184 Å
Hall symbol: -P 2ybc	Cell parameters from 9789 reflections
a = 19.8780 (5) Å	θ = 3.9–64.9°
b = 16.9350 (5) Å	µ = 5.27 mm⁻¹
c = 18.8060 (4) Å	T = 173 K
β = 102.916 (1)°	Plate, yellow
V = 6170.6 (3) Å³	0.15 × 0.09 × 0.04 mm
Z = 8

Data collection top

Bruker APEXII CCD diffractometer	9730 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.043
φ and ω scans	θ_max = 64.9°, θ_min = 3.9°
Absorption correction: multi-scan (SADABS; Bruker, 2007)	h = −23→23
T_min = 0.505, T_max = 0.817	k = −19→19
105322 measured reflections	l = −21→16
10278 independent reflections

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.028	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.068	H-atom parameters constrained
S = 1.08	w = 1/[σ²(F_o²) + (0.0274P)² + 9.4181P] where P = (F_o² + 2F_c²)/3
10278 reflections	(Δ/σ)_max = 0.003
745 parameters	Δρ_max = 1.56 e Å⁻³
240 restraints	Δρ_min = −0.59 e Å⁻³

Crystal data top

[Rh(C₅H₇O₂)(C₃₀H₂₁P)(CO)]·0.5C₃H₆O	V = 6170.6 (3) Å³
M_r = 671.51	Z = 8
Monoclinic, P2₁/c	Cu Kα radiation
a = 19.8780 (5) Å	µ = 5.27 mm⁻¹
b = 16.9350 (5) Å	T = 173 K
c = 18.8060 (4) Å	0.15 × 0.09 × 0.04 mm
β = 102.916 (1)°

Data collection top

Bruker APEXII CCD diffractometer	10278 independent reflections
Absorption correction: multi-scan (SADABS; Bruker, 2007)	9730 reflections with I > 2σ(I)
T_min = 0.505, T_max = 0.817	R_int = 0.043
105322 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.028	240 restraints
wR(F²) = 0.068	H-atom parameters constrained
S = 1.08	Δρ_max = 1.56 e Å⁻³
10278 reflections	Δρ_min = −0.59 e Å⁻³
745 parameters

Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F² against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F², conventional R-factors R are based on F, with F set to zero for negative F². The threshold expression of F² > σ(F²) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F² are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Rh2	0.534136 (9)	0.265488 (10)	0.656237 (9)	0.01388 (5)
Rh1	0.900894 (9)	0.212742 (10)	0.226138 (10)	0.01600 (6)
P2	0.44700 (3)	0.20502 (3)	0.69398 (3)	0.01280 (12)
P1	0.97479 (3)	0.14922 (3)	0.31614 (3)	0.01495 (13)
O2	0.82855 (9)	0.26594 (10)	0.14433 (10)	0.0245 (4)
O1	0.89175 (12)	0.06892 (12)	0.13498 (11)	0.0399 (5)
O4	0.61587 (9)	0.11875 (11)	0.68514 (11)	0.0290 (4)
O1S	0.69700 (11)	0.22018 (13)	0.40521 (13)	0.0419 (5)
O3	0.90469 (9)	0.31368 (10)	0.28592 (9)	0.0206 (4)
O5	0.61765 (9)	0.32029 (10)	0.62888 (10)	0.0244 (4)
O6	0.47819 (9)	0.36556 (9)	0.62588 (9)	0.0182 (4)
C11	1.00411 (14)	0.30098 (16)	0.49516 (16)	0.0283 (2)
C37	0.58290 (13)	0.17534 (15)	0.67555 (13)	0.0192 (5)
C50	0.41440 (12)	0.01493 (15)	0.45279 (13)	0.0202 (5)
H50	0.4079	−0.004	0.4042	0.024*
C52	0.43376 (12)	0.12415 (14)	0.53699 (13)	0.0160 (5)
H52	0.4409	0.1791	0.5459	0.019*
C72	0.33769 (13)	0.16760 (15)	0.79961 (13)	0.0206 (5)
H72	0.3247	0.1646	0.7479	0.025*
C53	0.43128 (11)	0.07298 (14)	0.59626 (13)	0.0143 (5)
C56	0.25310 (13)	0.24601 (15)	0.56476 (14)	0.0198 (5)
H56	0.2216	0.2173	0.5285	0.024*
C10	0.97019 (15)	0.25843 (18)	0.54138 (15)	0.0308 (6)
H10	0.9658	0.2812	0.5863	0.037*
C3S	0.7913 (2)	0.3101 (2)	0.4286 (2)	0.0613 (11)
H3S1	0.7927	0.2979	0.4798	0.092*
H3S2	0.7811	0.3663	0.4195	0.092*
H3S3	0.8362	0.2978	0.4177	0.092*
C18	0.99601 (12)	−0.01346 (14)	0.31244 (13)	0.0180 (5)
H18	1.0412	0.001	0.3084	0.022*
C64	0.45917 (12)	0.20529 (13)	0.79421 (13)	0.0147 (5)
C48	0.42152 (11)	−0.00937 (14)	0.58107 (13)	0.0155 (5)
C34	1.17054 (14)	0.05419 (16)	0.47784 (15)	0.0262 (6)
H34	1.1644	0.0295	0.5213	0.031*
C44	0.43700 (11)	0.09951 (13)	0.67017 (12)	0.0138 (5)
C22	0.79677 (13)	−0.08122 (15)	0.32964 (14)	0.0213 (5)
H22	0.7855	−0.1357	0.3302	0.026*
C20	0.91353 (13)	−0.11548 (15)	0.31596 (14)	0.0219 (5)
H20	0.9019	−0.1699	0.3152	0.026*
C68	0.42456 (13)	0.18990 (14)	0.91148 (13)	0.0174 (5)
C27	1.06450 (12)	0.14510 (14)	0.30637 (13)	0.0169 (5)
C55	0.31566 (12)	0.21079 (14)	0.60119 (13)	0.0162 (5)
H55	0.326	0.1586	0.5885	0.019*
C51	0.42607 (12)	0.09599 (15)	0.46746 (13)	0.0187 (5)
H51	0.4286	0.1313	0.4289	0.022*
C45	0.43799 (12)	0.04421 (14)	0.72423 (13)	0.0158 (5)
H45	0.444	0.0614	0.7733	0.019*
C7	0.97909 (12)	0.19186 (15)	0.40698 (13)	0.0187 (5)
C62	0.39025 (13)	0.37353 (15)	0.72987 (13)	0.0198 (5)
H62	0.4324	0.3512	0.756	0.024*
C25	0.82850 (13)	0.07842 (15)	0.32955 (14)	0.0205 (5)
H25	0.8385	0.1333	0.3297	0.025*
C15	1.04497 (14)	0.31208 (16)	0.38265 (16)	0.0283 (2)
H15	1.0497	0.2912	0.3371	0.034*
C61	0.37271 (14)	0.44802 (15)	0.74651 (14)	0.0253 (6)
H61	0.4027	0.4767	0.7841	0.03*
C65	0.52473 (13)	0.22282 (13)	0.83309 (13)	0.0172 (5)
H65	0.5593	0.2351	0.8072	0.021*
C57	0.23786 (13)	0.32114 (15)	0.58155 (14)	0.0215 (5)
H57	0.196	0.3448	0.5563	0.026*
C54	0.36217 (12)	0.25042 (14)	0.65473 (12)	0.0145 (5)
C21	0.86374 (13)	−0.05871 (15)	0.32365 (13)	0.0191 (5)
C40	0.56711 (14)	0.44663 (15)	0.59914 (14)	0.0253 (6)
H40	0.5769	0.4987	0.5857	0.03*
C35	1.11436 (13)	0.08241 (15)	0.42834 (14)	0.0215 (5)
H35	1.0698	0.0781	0.4385	0.026*
C58	0.28366 (13)	0.36425 (15)	0.63605 (14)	0.0207 (5)
C71	0.28949 (14)	0.15189 (16)	0.83948 (14)	0.0253 (6)
H71	0.2437	0.1387	0.8152	0.03*
C26	0.88095 (12)	0.02320 (14)	0.32458 (13)	0.0172 (5)
C32	1.24612 (14)	0.09633 (16)	0.40218 (16)	0.0289 (6)
H32	1.2914	0.1019	0.3941	0.035*
C70	0.30738 (15)	0.15521 (16)	0.91627 (15)	0.0276 (6)
H70	0.2736	0.1448	0.9437	0.033*
C30	1.19871 (13)	0.15532 (15)	0.28205 (16)	0.0258 (6)
H30	1.2441	0.1606	0.2741	0.031*
C3	0.82824 (13)	0.39243 (15)	0.19905 (15)	0.0245 (6)
H3	0.8103	0.4444	0.1901	0.029*
C17	0.94997 (12)	0.04497 (14)	0.32094 (13)	0.0159 (5)
C69	0.37318 (14)	0.17335 (15)	0.95109 (14)	0.0232 (6)
H69	0.385	0.175	1.0029	0.028*
C46	0.43032 (12)	−0.03718 (14)	0.70854 (13)	0.0179 (5)
H46	0.4317	−0.074	0.747	0.022*
C12	1.03281 (14)	0.37690 (16)	0.51546 (16)	0.0283 (2)
H12	1.0285	0.3996	0.5604	0.034*
C28	1.07644 (13)	0.17322 (14)	0.24157 (14)	0.0211 (5)
H28	1.0384	0.1901	0.2045	0.025*
C24	0.76388 (13)	0.05461 (15)	0.33411 (14)	0.0230 (5)
H24	0.7296	0.0928	0.3369	0.028*
C1	0.89609 (14)	0.12360 (16)	0.17148 (14)	0.0249 (6)
C36	1.12161 (12)	0.11787 (14)	0.36217 (14)	0.0185 (5)
C31	1.18918 (13)	0.12442 (15)	0.34891 (15)	0.0223 (5)
C4	0.87534 (13)	0.37951 (15)	0.26451 (14)	0.0215 (5)
C19	0.97786 (13)	−0.09378 (15)	0.30967 (14)	0.0209 (5)
H19	1.0104	−0.1328	0.3034	0.025*
C47	0.42097 (12)	−0.06313 (14)	0.63843 (13)	0.0180 (5)
H47	0.414	−0.1178	0.628	0.022*
C42	0.44669 (15)	0.49561 (16)	0.59086 (15)	0.0288 (6)
H42A	0.4047	0.4754	0.5583	0.043*
H42B	0.4645	0.5404	0.5676	0.043*
H42C	0.4359	0.5129	0.6368	0.043*
C2	0.80491 (13)	0.33581 (16)	0.14513 (15)	0.0249 (6)
C66	0.54236 (13)	0.22314 (14)	0.91011 (13)	0.0196 (5)
H66	0.5883	0.2345	0.9353	0.024*
C49	0.41249 (12)	−0.03627 (15)	0.50793 (13)	0.0181 (5)
H49	0.405	−0.0909	0.4975	0.022*
C73	0.40621 (13)	0.18809 (13)	0.83337 (13)	0.0165 (5)
C16	1.00927 (14)	0.26749 (16)	0.42584 (16)	0.0283 (2)
C23	0.74805 (13)	−0.02628 (16)	0.33467 (14)	0.0229 (6)
H23	0.7033	−0.0426	0.3386	0.027*
C8	0.94860 (13)	0.15189 (16)	0.45579 (14)	0.0228 (5)
H8	0.9305	0.1005	0.4436	0.027*
C14	1.07306 (14)	0.38447 (16)	0.40426 (15)	0.0283 (2)
H14	1.0972	0.4126	0.374	0.034*
C63	0.34676 (12)	0.32891 (14)	0.67429 (13)	0.0175 (5)
C29	1.14352 (14)	0.17767 (15)	0.22877 (15)	0.0249 (6)
H29	1.1503	0.1962	0.1832	0.03*
C67	0.49302 (13)	0.20703 (14)	0.94805 (13)	0.0199 (5)
H67	0.5049	0.2073	0.9999	0.024*
C59	0.26762 (14)	0.44216 (16)	0.65436 (15)	0.0267 (6)
H59	0.2262	0.4663	0.6284	0.032*
C60	0.31056 (15)	0.48312 (16)	0.70851 (16)	0.0293 (6)
H60	0.2988	0.535	0.7206	0.035*
C6	0.89517 (15)	0.44618 (16)	0.31812 (16)	0.0283 (6)
H6A	0.8835	0.432	0.3645	0.042*
H6B	0.87	0.494	0.2986	0.042*
H6C	0.9449	0.4558	0.3262	0.042*
C39	0.50023 (14)	0.43147 (15)	0.60603 (13)	0.0221 (5)
C9	0.94373 (14)	0.18528 (18)	0.52279 (15)	0.0288 (6)
H9	0.922	0.1569	0.555	0.035*
C5	0.74708 (16)	0.35524 (19)	0.08127 (17)	0.0391 (7)
H5A	0.7645	0.3553	0.0365	0.059*
H5B	0.7285	0.4075	0.0884	0.059*
H5C	0.7105	0.3156	0.0772	0.059*
C41	0.62120 (14)	0.39225 (16)	0.61022 (15)	0.0268 (6)
C13	1.06635 (14)	0.41745 (16)	0.47135 (15)	0.0283 (2)
H13	1.0853	0.468	0.4857	0.034*
C33	1.23727 (14)	0.06142 (17)	0.46478 (15)	0.0300 (6)
H33	1.276	0.042	0.4995	0.036*
C43	0.69125 (17)	0.4173 (2)	0.5994 (2)	0.0498 (9)
H43A	0.7222	0.427	0.647	0.075*
H43B	0.6865	0.4657	0.5702	0.075*
H43C	0.7105	0.3753	0.574	0.075*
C2S	0.73211 (17)	0.2659 (2)	0.3004 (2)	0.0435 (8)
H2S1	0.6964	0.2295	0.2749	0.065*
H2S2	0.7768	0.2512	0.2903	0.065*
H2S3	0.7203	0.3199	0.2833	0.065*
C1S	0.73633 (15)	0.26151 (17)	0.38060 (19)	0.0367 (7)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Rh2	0.01668 (10)	0.01180 (9)	0.01356 (9)	−0.00149 (7)	0.00425 (7)	0.00001 (6)
Rh1	0.01686 (10)	0.01368 (10)	0.01775 (10)	0.00225 (7)	0.00450 (7)	0.00181 (7)
P2	0.0158 (3)	0.0106 (3)	0.0122 (3)	−0.0007 (2)	0.0036 (2)	−0.0006 (2)
P1	0.0148 (3)	0.0131 (3)	0.0174 (3)	0.0005 (2)	0.0046 (2)	0.0009 (2)
O2	0.0267 (10)	0.0234 (10)	0.0221 (9)	0.0063 (8)	0.0025 (7)	0.0047 (7)
O1	0.0626 (15)	0.0242 (11)	0.0292 (11)	0.0057 (10)	0.0025 (10)	−0.0073 (9)
O4	0.0255 (10)	0.0184 (10)	0.0418 (12)	0.0030 (8)	0.0045 (8)	−0.0021 (8)
O1S	0.0375 (12)	0.0398 (13)	0.0526 (14)	−0.0048 (10)	0.0188 (11)	0.0013 (10)
O3	0.0216 (9)	0.0162 (9)	0.0243 (9)	0.0037 (7)	0.0058 (7)	0.0008 (7)
O5	0.0237 (9)	0.0228 (10)	0.0293 (10)	−0.0043 (7)	0.0114 (8)	0.0035 (8)
O6	0.0246 (9)	0.0131 (8)	0.0178 (9)	−0.0013 (7)	0.0063 (7)	0.0023 (7)
C11	0.0264 (6)	0.0219 (6)	0.0326 (6)	0.0041 (4)	−0.0020 (5)	−0.0034 (5)
C37	0.0202 (13)	0.0176 (13)	0.0206 (13)	−0.0052 (11)	0.0059 (10)	−0.0028 (10)
C50	0.0191 (13)	0.0259 (14)	0.0144 (12)	0.0005 (10)	0.0015 (10)	−0.0068 (10)
C52	0.0150 (12)	0.0149 (12)	0.0183 (12)	0.0002 (9)	0.0042 (9)	0.0000 (9)
C72	0.0254 (13)	0.0217 (13)	0.0153 (12)	−0.0024 (10)	0.0060 (10)	−0.0018 (10)
C53	0.0103 (11)	0.0151 (12)	0.0166 (12)	0.0004 (9)	0.0011 (9)	−0.0013 (9)
C56	0.0179 (12)	0.0212 (13)	0.0210 (13)	−0.0013 (10)	0.0056 (10)	0.0012 (10)
C10	0.0325 (15)	0.0394 (17)	0.0190 (14)	0.0095 (13)	0.0023 (11)	−0.0049 (12)
C3S	0.051 (2)	0.046 (2)	0.080 (3)	−0.0113 (18)	0.000 (2)	0.005 (2)
C18	0.0180 (12)	0.0187 (12)	0.0178 (12)	0.0004 (10)	0.0051 (10)	0.0020 (10)
C64	0.0230 (12)	0.0084 (11)	0.0132 (11)	−0.0005 (9)	0.0051 (9)	−0.0011 (9)
C48	0.0112 (11)	0.0146 (12)	0.0204 (12)	0.0004 (9)	0.0025 (9)	−0.0009 (9)
C34	0.0270 (14)	0.0260 (14)	0.0222 (14)	0.0041 (11)	−0.0017 (11)	−0.0055 (11)
C44	0.0124 (11)	0.0121 (11)	0.0166 (12)	−0.0002 (9)	0.0023 (9)	−0.0022 (9)
C22	0.0256 (13)	0.0175 (13)	0.0207 (13)	−0.0050 (10)	0.0050 (10)	0.0004 (10)
C20	0.0288 (14)	0.0137 (12)	0.0239 (13)	−0.0023 (10)	0.0074 (11)	−0.0004 (10)
C68	0.0272 (13)	0.0098 (11)	0.0163 (12)	0.0030 (10)	0.0075 (10)	−0.0007 (9)
C27	0.0175 (12)	0.0124 (12)	0.0216 (13)	−0.0004 (9)	0.0060 (10)	−0.0006 (9)
C55	0.0182 (12)	0.0143 (12)	0.0173 (12)	0.0003 (9)	0.0065 (9)	0.0007 (9)
C51	0.0161 (12)	0.0237 (13)	0.0154 (12)	0.0003 (10)	0.0019 (9)	0.0012 (10)
C45	0.0145 (12)	0.0166 (12)	0.0167 (12)	0.0006 (9)	0.0040 (9)	−0.0006 (9)
C7	0.0175 (12)	0.0209 (13)	0.0173 (12)	0.0061 (10)	0.0035 (9)	0.0008 (10)
C62	0.0247 (13)	0.0177 (13)	0.0184 (13)	0.0014 (10)	0.0079 (10)	−0.0010 (10)
C25	0.0209 (13)	0.0159 (12)	0.0253 (13)	0.0008 (10)	0.0064 (10)	0.0034 (10)
C15	0.0264 (6)	0.0219 (6)	0.0326 (6)	0.0041 (4)	−0.0020 (5)	−0.0034 (5)
C61	0.0334 (15)	0.0204 (13)	0.0237 (14)	0.0002 (11)	0.0095 (11)	−0.0052 (11)
C65	0.0235 (13)	0.0112 (11)	0.0175 (12)	−0.0006 (9)	0.0062 (10)	−0.0011 (9)
C57	0.0185 (12)	0.0246 (14)	0.0226 (13)	0.0041 (10)	0.0076 (10)	0.0055 (10)
C54	0.0187 (12)	0.0141 (11)	0.0120 (11)	−0.0004 (9)	0.0061 (9)	0.0026 (9)
C21	0.0208 (12)	0.0198 (13)	0.0165 (12)	−0.0019 (10)	0.0038 (10)	0.0009 (10)
C40	0.0393 (16)	0.0168 (13)	0.0225 (14)	−0.0074 (11)	0.0127 (12)	0.0016 (10)
C35	0.0199 (13)	0.0217 (13)	0.0218 (13)	0.0013 (10)	0.0023 (10)	−0.0046 (10)
C58	0.0233 (13)	0.0185 (13)	0.0228 (13)	0.0034 (10)	0.0105 (10)	0.0027 (10)
C71	0.0249 (14)	0.0293 (15)	0.0240 (14)	−0.0037 (11)	0.0101 (11)	−0.0024 (11)
C26	0.0174 (12)	0.0193 (12)	0.0142 (12)	−0.0005 (10)	0.0022 (9)	0.0031 (9)
C32	0.0170 (13)	0.0281 (15)	0.0399 (16)	0.0000 (11)	0.0027 (11)	−0.0127 (12)
C70	0.0339 (15)	0.0284 (15)	0.0258 (14)	−0.0035 (12)	0.0181 (12)	−0.0013 (11)
C30	0.0193 (13)	0.0185 (13)	0.0432 (16)	−0.0013 (10)	0.0146 (12)	−0.0034 (12)
C3	0.0260 (14)	0.0164 (13)	0.0338 (15)	0.0056 (11)	0.0120 (11)	0.0068 (11)
C17	0.0189 (12)	0.0144 (12)	0.0147 (12)	−0.0005 (9)	0.0040 (9)	0.0001 (9)
C69	0.0345 (15)	0.0218 (13)	0.0158 (12)	0.0006 (11)	0.0110 (11)	−0.0037 (10)
C46	0.0199 (12)	0.0140 (12)	0.0201 (12)	0.0011 (10)	0.0049 (10)	0.0038 (10)
C12	0.0264 (6)	0.0219 (6)	0.0326 (6)	0.0041 (4)	−0.0020 (5)	−0.0034 (5)
C28	0.0238 (13)	0.0136 (12)	0.0271 (14)	0.0024 (10)	0.0085 (11)	0.0028 (10)
C24	0.0184 (13)	0.0235 (13)	0.0272 (14)	0.0037 (10)	0.0052 (11)	0.0028 (11)
C1	0.0273 (14)	0.0235 (14)	0.0220 (13)	0.0043 (11)	0.0013 (11)	0.0052 (11)
C36	0.0175 (12)	0.0135 (12)	0.0238 (13)	−0.0004 (9)	0.0035 (10)	−0.0055 (10)
C31	0.0193 (13)	0.0170 (13)	0.0306 (14)	−0.0007 (10)	0.0055 (11)	−0.0077 (11)
C4	0.0201 (13)	0.0169 (13)	0.0308 (14)	0.0019 (10)	0.0127 (11)	0.0025 (11)
C19	0.0246 (13)	0.0163 (12)	0.0222 (13)	0.0032 (10)	0.0063 (10)	−0.0003 (10)
C47	0.0149 (12)	0.0127 (12)	0.0258 (13)	−0.0003 (9)	0.0034 (10)	−0.0008 (10)
C42	0.0420 (17)	0.0197 (14)	0.0247 (14)	0.0031 (12)	0.0077 (12)	0.0033 (11)
C2	0.0245 (14)	0.0239 (14)	0.0271 (14)	0.0067 (11)	0.0073 (11)	0.0084 (11)
C66	0.0245 (13)	0.0135 (12)	0.0186 (13)	0.0015 (10)	−0.0001 (10)	−0.0007 (10)
C49	0.0154 (12)	0.0161 (12)	0.0210 (13)	0.0003 (9)	0.0007 (10)	−0.0066 (10)
C73	0.0236 (13)	0.0097 (11)	0.0170 (12)	0.0018 (9)	0.0064 (10)	0.0005 (9)
C16	0.0264 (6)	0.0219 (6)	0.0326 (6)	0.0041 (4)	−0.0020 (5)	−0.0034 (5)
C23	0.0174 (12)	0.0288 (14)	0.0223 (13)	−0.0038 (11)	0.0042 (10)	0.0036 (11)
C8	0.0203 (13)	0.0258 (14)	0.0219 (13)	0.0020 (11)	0.0041 (10)	−0.0004 (11)
C14	0.0264 (6)	0.0219 (6)	0.0326 (6)	0.0041 (4)	−0.0020 (5)	−0.0034 (5)
C63	0.0205 (12)	0.0172 (12)	0.0175 (12)	0.0012 (10)	0.0099 (10)	0.0021 (10)
C29	0.0280 (14)	0.0190 (13)	0.0325 (15)	0.0022 (11)	0.0169 (12)	0.0030 (11)
C67	0.0316 (14)	0.0138 (12)	0.0136 (12)	0.0032 (10)	0.0033 (10)	−0.0003 (9)
C59	0.0264 (14)	0.0228 (14)	0.0326 (15)	0.0088 (11)	0.0100 (11)	0.0015 (11)
C60	0.0360 (16)	0.0179 (13)	0.0365 (16)	0.0057 (12)	0.0135 (13)	−0.0035 (12)
C6	0.0340 (15)	0.0192 (14)	0.0343 (16)	0.0053 (11)	0.0131 (12)	0.0004 (11)
C39	0.0371 (15)	0.0170 (13)	0.0122 (12)	−0.0020 (11)	0.0052 (10)	−0.0001 (10)
C9	0.0291 (15)	0.0376 (16)	0.0207 (14)	0.0041 (12)	0.0078 (11)	0.0031 (12)
C5	0.0415 (18)	0.0333 (17)	0.0362 (17)	0.0142 (14)	−0.0046 (13)	0.0048 (13)
C41	0.0331 (15)	0.0257 (15)	0.0244 (14)	−0.0103 (12)	0.0127 (11)	0.0007 (11)
C13	0.0264 (6)	0.0219 (6)	0.0326 (6)	0.0041 (4)	−0.0020 (5)	−0.0034 (5)
C33	0.0237 (14)	0.0321 (16)	0.0283 (15)	0.0064 (12)	−0.0067 (11)	−0.0101 (12)
C43	0.0402 (19)	0.0377 (19)	0.079 (3)	−0.0101 (15)	0.0301 (18)	0.0112 (18)
C2S	0.0336 (17)	0.0380 (18)	0.061 (2)	0.0113 (14)	0.0142 (15)	0.0200 (16)
C1S	0.0233 (15)	0.0247 (15)	0.062 (2)	0.0047 (12)	0.0091 (14)	0.0078 (14)

Geometric parameters (Å, º) top

Rh2—C37	1.801 (3)	C15—C16	1.411 (4)
Rh2—O6	2.0374 (16)	C15—H15	0.95
Rh2—O5	2.0649 (17)	C61—C60	1.413 (4)
Rh2—P2	2.2588 (6)	C61—H61	0.95
Rh1—C1	1.817 (3)	C65—C66	1.412 (3)
Rh1—O3	2.0380 (17)	C65—H65	0.95
Rh1—O2	2.0633 (17)	C57—C58	1.412 (4)
Rh1—P1	2.2513 (6)	C57—H57	0.95
P2—C44	1.842 (2)	C54—C63	1.431 (3)
P2—C64	1.846 (2)	C21—C26	1.428 (3)
P2—C54	1.850 (2)	C40—C39	1.388 (4)
P1—C27	1.835 (2)	C40—C41	1.396 (4)
P1—C7	1.839 (2)	C40—H40	0.95
P1—C17	1.841 (2)	C35—C36	1.418 (4)
O2—C2	1.274 (3)	C35—H35	0.95
O1—C1	1.144 (3)	C58—C59	1.418 (4)
O4—C37	1.152 (3)	C58—C63	1.430 (3)
O1S—C1S	1.215 (4)	C71—C70	1.409 (4)
O3—C4	1.281 (3)	C71—H71	0.95
O5—C41	1.274 (3)	C26—C17	1.437 (3)
O6—C39	1.285 (3)	C32—C33	1.364 (4)
C11—C10	1.411 (4)	C32—C31	1.416 (4)
C11—C12	1.424 (4)	C32—H32	0.95
C11—C16	1.446 (4)	C70—C69	1.361 (4)
C50—C49	1.359 (4)	C70—H70	0.95
C50—C51	1.409 (4)	C30—C29	1.363 (4)
C50—H50	0.95	C30—C31	1.413 (4)
C52—C51	1.368 (3)	C30—H30	0.95
C52—C53	1.421 (3)	C3—C4	1.387 (4)
C52—H52	0.95	C3—C2	1.397 (4)
C72—C71	1.368 (4)	C3—H3	0.95
C72—C73	1.411 (4)	C69—H69	0.95
C72—H72	0.95	C46—C47	1.362 (4)
C53—C48	1.428 (3)	C46—H46	0.95
C53—C44	1.441 (3)	C12—C13	1.361 (4)
C56—C57	1.361 (4)	C12—H12	0.95
C56—C55	1.411 (3)	C28—C29	1.409 (4)
C56—H56	0.95	C28—H28	0.95
C10—C9	1.361 (4)	C24—C23	1.406 (4)
C10—H10	0.95	C24—H24	0.95
C3S—C1S	1.498 (5)	C36—C31	1.424 (3)
C3S—H3S1	0.98	C4—C6	1.506 (4)
C3S—H3S2	0.98	C19—H19	0.95
C3S—H3S3	0.98	C47—H47	0.95
C18—C17	1.381 (3)	C42—C39	1.503 (4)
C18—C19	1.405 (3)	C42—H42A	0.98
C18—H18	0.95	C42—H42B	0.98
C64—C65	1.377 (3)	C42—H42C	0.98
C64—C73	1.443 (3)	C2—C5	1.502 (4)
C48—C47	1.414 (3)	C66—C67	1.363 (4)
C48—C49	1.422 (3)	C66—H66	0.95
C34—C35	1.370 (4)	C49—H49	0.95
C34—C33	1.407 (4)	C23—H23	0.95
C34—H34	0.95	C8—C9	1.404 (4)
C44—C45	1.379 (3)	C8—H8	0.95
C22—C23	1.361 (4)	C14—C13	1.413 (4)
C22—C21	1.413 (4)	C14—H14	0.95
C22—H22	0.95	C29—H29	0.95
C20—C19	1.361 (4)	C67—H67	0.95
C20—C21	1.410 (4)	C59—C60	1.363 (4)
C20—H20	0.95	C59—H59	0.95
C68—C67	1.411 (4)	C60—H60	0.95
C68—C69	1.420 (4)	C6—H6A	0.98
C68—C73	1.433 (3)	C6—H6B	0.98
C27—C28	1.377 (4)	C6—H6C	0.98
C27—C36	1.439 (3)	C9—H9	0.95
C55—C54	1.380 (3)	C5—H5A	0.98
C55—H55	0.95	C5—H5B	0.98
C51—H51	0.95	C5—H5C	0.98
C45—C46	1.411 (3)	C41—C43	1.512 (4)
C45—H45	0.95	C13—H13	0.95
C7—C8	1.385 (4)	C33—H33	0.95
C7—C16	1.425 (4)	C43—H43A	0.98
C62—C61	1.364 (4)	C43—H43B	0.98
C62—C63	1.417 (4)	C43—H43C	0.98
C62—H62	0.95	C2S—C1S	1.494 (5)
C25—C24	1.367 (4)	C2S—H2S1	0.98
C25—C26	1.419 (3)	C2S—H2S2	0.98
C25—H25	0.95	C2S—H2S3	0.98
C15—C14	1.370 (4)

C37—Rh2—O6	175.48 (9)	C33—C32—C31	121.3 (3)
C37—Rh2—O5	90.28 (9)	C33—C32—H32	119.3
O6—Rh2—O5	88.58 (7)	C31—C32—H32	119.3
C37—Rh2—P2	88.18 (8)	C69—C70—C71	119.8 (2)
O6—Rh2—P2	93.22 (5)	C69—C70—H70	120.1
O5—Rh2—P2	176.14 (5)	C71—C70—H70	120.1
C1—Rh1—O3	178.85 (10)	C29—C30—C31	120.7 (2)
C1—Rh1—O2	90.07 (9)	C29—C30—H30	119.6
O3—Rh1—O2	88.78 (7)	C31—C30—H30	119.6
C1—Rh1—P1	88.35 (8)	C4—C3—C2	125.8 (2)
O3—Rh1—P1	92.78 (5)	C4—C3—H3	117.1
O2—Rh1—P1	176.45 (5)	C2—C3—H3	117.1
C44—P2—C64	103.47 (10)	C18—C17—C26	119.1 (2)
C44—P2—C54	105.48 (10)	C18—C17—P1	119.32 (18)
C64—P2—C54	107.83 (11)	C26—C17—P1	121.17 (18)
C44—P2—Rh2	114.33 (8)	C70—C69—C68	121.3 (2)
C64—P2—Rh2	112.65 (8)	C70—C69—H69	119.4
C54—P2—Rh2	112.38 (7)	C68—C69—H69	119.4
C27—P1—C7	105.28 (11)	C47—C46—C45	120.2 (2)
C27—P1—C17	104.22 (11)	C47—C46—H46	119.9
C7—P1—C17	106.77 (11)	C45—C46—H46	119.9
C27—P1—Rh1	115.36 (8)	C13—C12—C11	120.9 (3)
C7—P1—Rh1	113.44 (8)	C13—C12—H12	119.5
C17—P1—Rh1	110.99 (8)	C11—C12—H12	119.5
C2—O2—Rh1	126.44 (17)	C27—C28—C29	121.8 (2)
C4—O3—Rh1	126.77 (16)	C27—C28—H28	119.1
C41—O5—Rh2	126.54 (17)	C29—C28—H28	119.1
C39—O6—Rh2	127.15 (16)	C25—C24—C23	120.2 (2)
C10—C11—C12	120.9 (3)	C25—C24—H24	119.9
C10—C11—C16	119.7 (3)	C23—C24—H24	119.9
C12—C11—C16	119.4 (3)	O1—C1—Rh1	177.6 (2)
O4—C37—Rh2	176.4 (2)	C35—C36—C31	118.1 (2)
C49—C50—C51	120.2 (2)	C35—C36—C27	123.9 (2)
C49—C50—H50	119.9	C31—C36—C27	117.9 (2)
C51—C50—H50	119.9	C30—C31—C32	120.6 (2)
C51—C52—C53	121.4 (2)	C30—C31—C36	120.2 (2)
C51—C52—H52	119.3	C32—C31—C36	119.1 (2)
C53—C52—H52	119.3	O3—C4—C3	125.9 (2)
C71—C72—C73	121.7 (2)	O3—C4—C6	114.2 (2)
C71—C72—H72	119.2	C3—C4—C6	120.0 (2)
C73—C72—H72	119.2	C20—C19—C18	119.8 (2)
C52—C53—C48	117.7 (2)	C20—C19—H19	120.1
C52—C53—C44	123.9 (2)	C18—C19—H19	120.1
C48—C53—C44	118.4 (2)	C46—C47—C48	120.5 (2)
C57—C56—C55	120.0 (2)	C46—C47—H47	119.7
C57—C56—H56	120	C48—C47—H47	119.7
C55—C56—H56	120	C39—C42—H42A	109.5
C9—C10—C11	121.1 (3)	C39—C42—H42B	109.5
C9—C10—H10	119.4	H42A—C42—H42B	109.5
C11—C10—H10	119.4	C39—C42—H42C	109.5
C1S—C3S—H3S1	109.5	H42A—C42—H42C	109.5
C1S—C3S—H3S2	109.5	H42B—C42—H42C	109.5
H3S1—C3S—H3S2	109.5	O2—C2—C3	125.6 (2)
C1S—C3S—H3S3	109.5	O2—C2—C5	114.4 (2)
H3S1—C3S—H3S3	109.5	C3—C2—C5	120.0 (2)
H3S2—C3S—H3S3	109.5	C67—C66—C65	119.6 (2)
C17—C18—C19	121.8 (2)	C67—C66—H66	120.2
C17—C18—H18	119.1	C65—C66—H66	120.2
C19—C18—H18	119.1	C50—C49—C48	121.0 (2)
C65—C64—C73	119.0 (2)	C50—C49—H49	119.5
C65—C64—P2	115.81 (18)	C48—C49—H49	119.5
C73—C64—P2	125.21 (18)	C72—C73—C68	117.7 (2)
C47—C48—C49	120.7 (2)	C72—C73—C64	124.1 (2)
C47—C48—C53	120.0 (2)	C68—C73—C64	118.1 (2)
C49—C48—C53	119.2 (2)	C15—C16—C7	125.1 (3)
C35—C34—C33	120.5 (3)	C15—C16—C11	117.1 (2)
C35—C34—H34	119.7	C7—C16—C11	117.8 (3)
C33—C34—H34	119.7	C22—C23—C24	120.1 (2)
C45—C44—C53	119.0 (2)	C22—C23—H23	119.9
C45—C44—P2	119.77 (18)	C24—C23—H23	119.9
C53—C44—P2	121.19 (17)	C7—C8—C9	121.8 (3)
C23—C22—C21	121.2 (2)	C7—C8—H8	119.1
C23—C22—H22	119.4	C9—C8—H8	119.1
C21—C22—H22	119.4	C15—C14—C13	120.3 (3)
C19—C20—C21	121.3 (2)	C15—C14—H14	119.8
C19—C20—H20	119.4	C13—C14—H14	119.8
C21—C20—H20	119.4	C62—C63—C58	118.0 (2)
C67—C68—C69	120.9 (2)	C62—C63—C54	123.7 (2)
C67—C68—C73	120.1 (2)	C58—C63—C54	118.3 (2)
C69—C68—C73	119.0 (2)	C30—C29—C28	119.8 (2)
C28—C27—C36	119.5 (2)	C30—C29—H29	120.1
C28—C27—P1	116.04 (18)	C28—C29—H29	120.1
C36—C27—P1	124.42 (18)	C66—C67—C68	121.0 (2)
C54—C55—C56	121.5 (2)	C66—C67—H67	119.5
C54—C55—H55	119.2	C68—C67—H67	119.5
C56—C55—H55	119.2	C60—C59—C58	121.2 (3)
C52—C51—C50	120.3 (2)	C60—C59—H59	119.4
C52—C51—H51	119.8	C58—C59—H59	119.4
C50—C51—H51	119.8	C59—C60—C61	119.6 (2)
C44—C45—C46	121.8 (2)	C59—C60—H60	120.2
C44—C45—H45	119.1	C61—C60—H60	120.2
C46—C45—H45	119.1	C4—C6—H6A	109.5
C8—C7—C16	119.8 (2)	C4—C6—H6B	109.5
C8—C7—P1	119.18 (19)	H6A—C6—H6B	109.5
C16—C7—P1	120.9 (2)	C4—C6—H6C	109.5
C61—C62—C63	121.2 (2)	H6A—C6—H6C	109.5
C61—C62—H62	119.4	H6B—C6—H6C	109.5
C63—C62—H62	119.4	O6—C39—C40	125.7 (2)
C24—C25—C26	121.6 (2)	O6—C39—C42	114.2 (2)
C24—C25—H25	119.2	C40—C39—C42	120.1 (2)
C26—C25—H25	119.2	C10—C9—C8	119.8 (3)
C14—C15—C16	122.1 (3)	C10—C9—H9	120.1
C14—C15—H15	118.9	C8—C9—H9	120.1
C16—C15—H15	118.9	C2—C5—H5A	109.5
C62—C61—C60	120.8 (3)	C2—C5—H5B	109.5
C62—C61—H61	119.6	H5A—C5—H5B	109.5
C60—C61—H61	119.6	C2—C5—H5C	109.5
C64—C65—C66	122.3 (2)	H5A—C5—H5C	109.5
C64—C65—H65	118.9	H5B—C5—H5C	109.5
C66—C65—H65	118.9	O5—C41—C40	125.7 (2)
C56—C57—C58	120.7 (2)	O5—C41—C43	114.5 (3)
C56—C57—H57	119.6	C40—C41—C43	119.8 (3)
C58—C57—H57	119.6	C12—C13—C14	120.1 (3)
C55—C54—C63	119.5 (2)	C12—C13—H13	119.9
C55—C54—P2	119.44 (18)	C14—C13—H13	119.9
C63—C54—P2	120.80 (18)	C32—C33—C34	119.8 (3)
C20—C21—C22	121.3 (2)	C32—C33—H33	120.1
C20—C21—C26	119.5 (2)	C34—C33—H33	120.1
C22—C21—C26	119.2 (2)	C41—C43—H43A	109.5
C39—C40—C41	125.9 (2)	C41—C43—H43B	109.5
C39—C40—H40	117.1	H43A—C43—H43B	109.5
C41—C40—H40	117.1	C41—C43—H43C	109.5
C34—C35—C36	121.1 (2)	H43A—C43—H43C	109.5
C34—C35—H35	119.4	H43B—C43—H43C	109.5
C36—C35—H35	119.4	C1S—C2S—H2S1	109.5
C57—C58—C59	120.9 (2)	C1S—C2S—H2S2	109.5
C57—C58—C63	119.9 (2)	H2S1—C2S—H2S2	109.5
C59—C58—C63	119.1 (2)	C1S—C2S—H2S3	109.5
C72—C71—C70	120.4 (2)	H2S1—C2S—H2S3	109.5
C72—C71—H71	119.8	H2S2—C2S—H2S3	109.5
C70—C71—H71	119.8	O1S—C1S—C2S	121.2 (3)
C25—C26—C21	117.6 (2)	O1S—C1S—C3S	122.1 (3)
C25—C26—C17	123.9 (2)	C2S—C1S—C3S	116.7 (3)
C21—C26—C17	118.5 (2)

C37—Rh2—P2—C44	−36.07 (11)	Rh1—P1—C17—C26	−51.6 (2)
O6—Rh2—P2—C44	139.63 (9)	C71—C70—C69—C68	0.6 (4)
C37—Rh2—P2—C64	81.68 (11)	C67—C68—C69—C70	−178.7 (2)
O6—Rh2—P2—C64	−102.61 (9)	C73—C68—C69—C70	0.6 (4)
C37—Rh2—P2—C54	−156.28 (11)	C44—C45—C46—C47	−0.6 (4)
O6—Rh2—P2—C54	19.43 (9)	C10—C11—C12—C13	179.1 (3)
C1—Rh1—P1—C27	80.66 (12)	C16—C11—C12—C13	−1.5 (4)
O3—Rh1—P1—C27	−99.52 (10)	C36—C27—C28—C29	−1.3 (4)
C1—Rh1—P1—C7	−157.77 (12)	P1—C27—C28—C29	176.3 (2)
O3—Rh1—P1—C7	22.04 (10)	C26—C25—C24—C23	0.6 (4)
C1—Rh1—P1—C17	−37.57 (12)	C34—C35—C36—C31	−0.9 (4)
O3—Rh1—P1—C17	142.25 (9)	C34—C35—C36—C27	176.8 (2)
C1—Rh1—O2—C2	−179.8 (2)	C28—C27—C36—C35	−175.0 (2)
O3—Rh1—O2—C2	0.3 (2)	P1—C27—C36—C35	7.6 (3)
O2—Rh1—O3—C4	−7.33 (19)	C28—C27—C36—C31	2.6 (3)
P1—Rh1—O3—C4	175.86 (19)	P1—C27—C36—C31	−174.75 (18)
C37—Rh2—O5—C41	−177.5 (2)	C29—C30—C31—C32	175.7 (2)
O6—Rh2—O5—C41	6.9 (2)	C29—C30—C31—C36	−1.4 (4)
O5—Rh2—O6—C39	−5.34 (19)	C33—C32—C31—C30	−175.5 (3)
P2—Rh2—O6—C39	171.24 (18)	C33—C32—C31—C36	1.7 (4)
C51—C52—C53—C48	1.0 (3)	C35—C36—C31—C30	176.5 (2)
C51—C52—C53—C44	−178.1 (2)	C27—C36—C31—C30	−1.3 (3)
C12—C11—C10—C9	−178.9 (3)	C35—C36—C31—C32	−0.7 (3)
C16—C11—C10—C9	1.8 (4)	C27—C36—C31—C32	−178.5 (2)
C44—P2—C64—C65	108.30 (18)	Rh1—O3—C4—C3	8.3 (4)
C54—P2—C64—C65	−140.27 (18)	Rh1—O3—C4—C6	−172.57 (16)
Rh2—P2—C64—C65	−15.7 (2)	C2—C3—C4—O3	−0.2 (4)
C44—P2—C64—C73	−71.1 (2)	C2—C3—C4—C6	−179.2 (2)
C54—P2—C64—C73	40.3 (2)	C21—C20—C19—C18	1.4 (4)
Rh2—P2—C64—C73	164.92 (17)	C17—C18—C19—C20	−0.5 (4)
C52—C53—C48—C47	177.9 (2)	C45—C46—C47—C48	2.5 (4)
C44—C53—C48—C47	−3.0 (3)	C49—C48—C47—C46	179.3 (2)
C52—C53—C48—C49	−2.1 (3)	C53—C48—C47—C46	−0.6 (3)
C44—C53—C48—C49	177.0 (2)	Rh1—O2—C2—C3	6.3 (4)
C52—C53—C44—C45	−176.2 (2)	Rh1—O2—C2—C5	−173.66 (19)
C48—C53—C44—C45	4.7 (3)	C4—C3—C2—O2	−7.8 (4)
C52—C53—C44—P2	0.9 (3)	C4—C3—C2—C5	172.1 (3)
C48—C53—C44—P2	−178.12 (16)	C64—C65—C66—C67	−1.2 (4)
C64—P2—C44—C45	1.7 (2)	C51—C50—C49—C48	0.6 (4)
C54—P2—C44—C45	−111.41 (19)	C47—C48—C49—C50	−178.6 (2)
Rh2—P2—C44—C45	124.61 (17)	C53—C48—C49—C50	1.3 (3)
C64—P2—C44—C53	−175.38 (18)	C71—C72—C73—C68	1.7 (4)
C54—P2—C44—C53	71.5 (2)	C71—C72—C73—C64	−180.0 (2)
Rh2—P2—C44—C53	−52.5 (2)	C67—C68—C73—C72	177.6 (2)
C7—P1—C27—C28	−132.80 (19)	C69—C68—C73—C72	−1.7 (3)
C17—P1—C27—C28	115.01 (19)	C67—C68—C73—C64	−0.9 (3)
Rh1—P1—C27—C28	−6.9 (2)	C69—C68—C73—C64	179.8 (2)
C7—P1—C27—C36	44.7 (2)	C65—C64—C73—C72	−178.5 (2)
C17—P1—C27—C36	−67.5 (2)	P2—C64—C73—C72	0.9 (3)
Rh1—P1—C27—C36	170.53 (17)	C65—C64—C73—C68	−0.2 (3)
C57—C56—C55—C54	0.8 (4)	P2—C64—C73—C68	179.21 (17)
C53—C52—C51—C50	0.9 (4)	C14—C15—C16—C7	−179.7 (3)
C49—C50—C51—C52	−1.7 (4)	C14—C15—C16—C11	−0.8 (4)
C53—C44—C45—C46	−3.0 (3)	C8—C7—C16—C15	176.4 (2)
P2—C44—C45—C46	179.81 (18)	P1—C7—C16—C15	−7.7 (4)
C27—P1—C7—C8	−126.3 (2)	C8—C7—C16—C11	−2.5 (4)
C17—P1—C7—C8	−15.9 (2)	P1—C7—C16—C11	173.38 (19)
Rh1—P1—C7—C8	106.65 (19)	C10—C11—C16—C15	−178.8 (2)
C27—P1—C7—C16	57.8 (2)	C12—C11—C16—C15	1.9 (4)
C17—P1—C7—C16	168.2 (2)	C10—C11—C16—C7	0.2 (4)
Rh1—P1—C7—C16	−69.2 (2)	C12—C11—C16—C7	−179.1 (2)
C63—C62—C61—C60	−0.2 (4)	C21—C22—C23—C24	−0.1 (4)
C73—C64—C65—C66	1.2 (3)	C25—C24—C23—C22	−0.9 (4)
P2—C64—C65—C66	−178.21 (18)	C16—C7—C8—C9	2.8 (4)
C55—C56—C57—C58	−0.9 (4)	P1—C7—C8—C9	−173.1 (2)
C56—C55—C54—C63	0.3 (3)	C16—C15—C14—C13	−0.6 (4)
C56—C55—C54—P2	−173.95 (18)	C61—C62—C63—C58	−0.1 (4)
C44—P2—C54—C55	−17.9 (2)	C61—C62—C63—C54	−179.6 (2)
C64—P2—C54—C55	−127.92 (19)	C57—C58—C63—C62	−178.3 (2)
Rh2—P2—C54—C55	107.34 (18)	C59—C58—C63—C62	0.8 (3)
C44—P2—C54—C63	167.93 (18)	C57—C58—C63—C54	1.2 (3)
C64—P2—C54—C63	57.9 (2)	C59—C58—C63—C54	−179.7 (2)
Rh2—P2—C54—C63	−66.87 (19)	C55—C54—C63—C62	178.2 (2)
C19—C20—C21—C22	179.5 (2)	P2—C54—C63—C62	−7.6 (3)
C19—C20—C21—C26	0.3 (4)	C55—C54—C63—C58	−1.3 (3)
C23—C22—C21—C20	−177.8 (2)	P2—C54—C63—C58	172.89 (17)
C23—C22—C21—C26	1.4 (4)	C31—C30—C29—C28	2.8 (4)
C33—C34—C35—C36	1.4 (4)	C27—C28—C29—C30	−1.4 (4)
C56—C57—C58—C59	−179.2 (2)	C65—C66—C67—C68	0.1 (4)
C56—C57—C58—C63	−0.1 (4)	C69—C68—C67—C66	−179.8 (2)
C73—C72—C71—C70	−0.5 (4)	C73—C68—C67—C66	0.9 (4)
C24—C25—C26—C21	0.7 (4)	C57—C58—C59—C60	177.9 (3)
C24—C25—C26—C17	−178.9 (2)	C63—C58—C59—C60	−1.3 (4)
C20—C21—C26—C25	177.6 (2)	C58—C59—C60—C61	0.9 (4)
C22—C21—C26—C25	−1.7 (3)	C62—C61—C60—C59	−0.2 (4)
C20—C21—C26—C17	−2.8 (3)	Rh2—O6—C39—C40	2.2 (4)
C22—C21—C26—C17	177.9 (2)	Rh2—O6—C39—C42	−176.84 (16)
C72—C71—C70—C69	−0.7 (4)	C41—C40—C39—O6	2.3 (4)
C19—C18—C17—C26	−2.1 (4)	C41—C40—C39—C42	−178.7 (2)
C19—C18—C17—P1	−174.75 (19)	C11—C10—C9—C8	−1.5 (4)
C25—C26—C17—C18	−176.7 (2)	C7—C8—C9—C10	−0.8 (4)
C21—C26—C17—C18	3.7 (3)	Rh2—O5—C41—C40	−5.3 (4)
C25—C26—C17—P1	−4.2 (3)	Rh2—O5—C41—C43	175.1 (2)
C21—C26—C17—P1	176.18 (17)	C39—C40—C41—O5	−0.5 (4)
C27—P1—C17—C18	−3.9 (2)	C39—C40—C41—C43	179.0 (3)
C7—P1—C17—C18	−115.0 (2)	C11—C12—C13—C14	0.1 (4)
Rh1—P1—C17—C18	120.88 (18)	C15—C14—C13—C12	1.0 (4)
C27—P1—C17—C26	−176.36 (19)	C31—C32—C33—C34	−1.2 (4)
C7—P1—C17—C26	72.5 (2)	C35—C34—C33—C32	−0.4 (4)

Experimental details

Crystal data
Chemical formula	[Rh(C₅H₇O₂)(C₃₀H₂₁P)(CO)]·0.5C₃H₆O
M_r	671.51
Crystal system, space group	Monoclinic, P2₁/c
Temperature (K)	173
a, b, c (Å)	19.8780 (5), 16.9350 (5), 18.8060 (4)
β (°)	102.916 (1)
V (Å³)	6170.6 (3)
Z	8
Radiation type	Cu Kα
µ (mm⁻¹)	5.27
Crystal size (mm)	0.15 × 0.09 × 0.04

Data collection
Diffractometer	Bruker APEXII CCD
Absorption correction	Multi-scan (SADABS; Bruker, 2007)
T_min, T_max	0.505, 0.817
No. of measured, independent and observed [I > 2σ(I)] reflections	105322, 10278, 9730
R_int	0.043
(sin θ/λ)_max (Å⁻¹)	0.587

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.028, 0.068, 1.08
No. of reflections	10278
No. of parameters	745
No. of restraints	240
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	1.56, −0.59

Computer programs: APEX2 (Bruker, 2007), SAINT-Plus (Bruker, 2007), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

Acknowledgements

Financial assistance from the South African National Research Foundation (SA NRF), the Research Fund of the University of Johannesburg, TESP and SASOL is gratefully acknowledged. Mr S. Enus is acknowledged for the synthesis of this compound.

References

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