metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

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ISSN: 2056-9890

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

aLeibniz-Institut für Katalyse e. V. an der Universität Rostock, Albert-Einstein-Strasse 29a, 18059 Rostock, Germany
*Correspondence e-mail: detlef.selent@catalysis.de

(Received 16 March 2012; accepted 19 March 2012; online 28 March 2012)

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[Van Rooy, A., Kamer, P. C. J., van Leeuwen, P. W. N. M., Veldman, N. & Spek, A. L. (1995). J. Organomet. Chem. 494, C15-C18.], 1996[Van Rooy, A., Kamer, P. C. J., van Leeuwen, P. W. N. M., Goubitz, K., Fraanje, J., Veldman, N. & Spek, A. L. (1996). Organometallics, 15, 835-847.]). The title compound has recently been studied in solution, see: Selent et al. (2011[Selent, D., Franke, R., Kubis, C., Spannenberg, A., Baumann, W., Kreidler, B. & Börner, A. (2011). Organometallics, 30, 4509-4514.]). Structural information on this labile compound class is usually obtained by spectroscopy, see, for example: Dieleman et al. (2001[Dieleman, C. B., Kamer, P. C. J., Reek, J. N. H. & van Leeuwen, P. W. N. M. (2001). Helv. Chim. Acta, 84, 3269-3280.]); Axet et al. (2007[Axet, M. R., Benet-Buchholz, J., Claver, C. & Castillón, S. (2007). Adv. Synth. Catal. 349, 1983-1998.]).

[Scheme 1]

Experimental

Crystal data
  • [Rh(C74H68O8P2)H(CO)2]·C4H10O

  • Mr = 1381.28

  • Monoclinic, P 21

  • 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[Stoe & Cie (2005). X-SHAPE, X-RED32 and X-AREA. Stoe & Cie, Darmstadt, Germany.]) Tmin = 0.835, Tmax = 0.959

  • 59171 measured reflections

  • 16262 independent reflections

  • 14238 reflections with I > 2σ(I)

  • Rint = 0.026

Refinement
  • R[F2 > 2σ(F2)] = 0.028

  • wR(F2) = 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[Flack, H. D. (1983). Acta Cryst. A39, 876-881.]), 7944 Friedel pairs

  • Flack parameter: −0.026 (11)

Data collection: X-AREA (Stoe & Cie, 2005[Stoe & Cie (2005). X-SHAPE, X-RED32 and X-AREA. Stoe & Cie, Darmstadt, Germany.]); cell refinement: X-AREA; data reduction: X-AREA; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: XP in SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); software used to prepare material for publication: SHELXTL.

Supporting information


Comment top

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.

Related literature top

For another solid state-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).

Experimental top

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 top

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.

Structure description top

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.

For another solid state-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).

Computing details top

Data collection: X-AREA (Stoe & Cie, 2005); cell refinement: X-AREA (Stoe & Cie, 2005); data reduction: X-AREA (Stoe & Cie, 2005); 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 (Sheldrick, 2008).

Figures top
[Figure 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.
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 top
Crystal data top
[Rh(C74H68O8P2)H(CO)2]·C4H10OF(000) = 1444
Mr = 1381.28Dx = 1.347 Mg m3
Monoclinic, P21Mo Kα radiation, λ = 0.71073 Å
a = 11.1489 (2) ÅCell parameters from 15841 reflections
b = 25.8458 (4) Åθ = 1.7–28.4°
c = 12.5941 (3) ŵ = 0.36 mm1
β = 110.263 (2)°T = 200 K
V = 3404.43 (11) Å3Prism, colourless
Z = 20.40 × 0.35 × 0.15 mm
Data collection top
Stoe IPDS II
diffractometer
16262 independent reflections
Radiation source: fine-focus sealed tube14238 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.026
ω scansθmax = 27.9°, θmin = 1.6°
Absorption correction: numerical
(X-SHAPE and X-RED32; Stoe & Cie, 2005)
h = 1414
Tmin = 0.835, Tmax = 0.959k = 3434
59171 measured reflectionsl = 1616
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.028H 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 reflectionsΔρmax = 0.66 e Å3
834 parametersΔρmin = 0.47 e Å3
35 restraintsAbsolute structure: Flack (1983), 7944 Friedel pairs
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.026 (11)
Crystal data top
[Rh(C74H68O8P2)H(CO)2]·C4H10OV = 3404.43 (11) Å3
Mr = 1381.28Z = 2
Monoclinic, P21Mo Kα radiation
a = 11.1489 (2) ŵ = 0.36 mm1
b = 25.8458 (4) ÅT = 200 K
c = 12.5941 (3) Å0.40 × 0.35 × 0.15 mm
β = 110.263 (2)°
Data collection top
Stoe IPDS II
diffractometer
16262 independent reflections
Absorption correction: numerical
(X-SHAPE and X-RED32; Stoe & Cie, 2005)
14238 reflections with I > 2σ(I)
Tmin = 0.835, Tmax = 0.959Rint = 0.026
59171 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.028H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.063Δρmax = 0.66 e Å3
S = 0.94Δρmin = 0.47 e Å3
16262 reflectionsAbsolute structure: Flack (1983), 7944 Friedel pairs
834 parametersAbsolute structure parameter: 0.026 (11)
35 restraints
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
xyzUiso*/Ueq
C771.0804 (4)0.91333 (17)0.5094 (3)0.0878 (11)*
H77A1.15080.93430.50300.132*
H77B1.10420.87670.51470.132*
H77C1.06260.92360.57740.132*
C780.9699 (5)0.9212 (2)0.4129 (4)0.1113 (15)*
H78A0.94900.95860.40770.134*
H78B0.99080.91200.34490.134*
C790.7521 (5)0.9016 (2)0.3186 (4)0.1172 (17)*
H79A0.73150.86990.27150.141*
H79B0.76350.93040.27130.141*
C800.6510 (6)0.9131 (3)0.3584 (6)0.147 (2)*
H80A0.57180.91810.29380.221*
H80B0.67110.94490.40370.221*
H80C0.64010.88450.40520.221*
O110.8631 (3)0.89420 (13)0.4096 (3)0.1138 (10)*
C10.5785 (3)0.53367 (10)0.6920 (2)0.0518 (7)
C20.5159 (2)0.59995 (12)0.9031 (2)0.0456 (6)
C30.37567 (19)0.72557 (7)0.53935 (15)0.0230 (4)
C40.44781 (18)0.75555 (7)0.65556 (16)0.0248 (4)
C50.4165 (2)0.73789 (8)0.43790 (16)0.0287 (4)
C60.3402 (2)0.72021 (9)0.33200 (16)0.0377 (5)
H60.26330.70220.32390.045*
C70.3749 (2)0.72856 (10)0.23819 (19)0.0507 (7)
H70.32170.71610.16640.061*
C80.4858 (2)0.75483 (11)0.24739 (19)0.0573 (8)
H80.50710.76200.18210.069*
C90.5654 (3)0.77058 (10)0.35312 (17)0.0522 (7)
H90.64380.78740.36100.063*
C100.5319 (2)0.76214 (9)0.44750 (19)0.0375 (5)
H100.58790.77290.51980.045*
C110.23051 (19)0.72664 (7)0.50856 (15)0.0242 (4)
C120.1685 (2)0.68911 (8)0.54920 (17)0.0297 (4)
H120.21580.66100.59220.036*
C130.0377 (2)0.69246 (9)0.52739 (19)0.0346 (5)
H130.00410.66620.55440.042*
C140.0318 (2)0.73353 (9)0.46688 (18)0.0347 (5)
H140.12090.73600.45340.042*
C150.0287 (2)0.77076 (8)0.42623 (17)0.0338 (5)
H150.01880.79920.38460.041*
C160.1582 (2)0.76722 (8)0.44540 (16)0.0289 (4)
H160.19840.79280.41510.035*
C170.37177 (18)0.75349 (6)0.73659 (15)0.0268 (4)
C180.27163 (19)0.78775 (8)0.72410 (17)0.0316 (4)
H180.25140.81300.66570.038*
C190.2012 (2)0.78574 (9)0.79491 (17)0.0406 (5)
H190.13350.80960.78500.049*
C200.2282 (3)0.74940 (9)0.8798 (2)0.0542 (7)
H200.17750.74710.92660.065*
C210.3298 (3)0.71647 (12)0.8955 (2)0.0654 (9)
H210.35130.69210.95570.078*
C220.4007 (3)0.71839 (10)0.82517 (19)0.0470 (6)
H220.47050.69530.83750.056*
C230.4872 (2)0.81179 (7)0.65172 (18)0.0287 (4)
C240.4264 (2)0.84704 (7)0.5669 (2)0.0407 (5)
H240.35840.83560.50190.049*
C250.4628 (3)0.89834 (8)0.5752 (2)0.0495 (6)
H250.41940.92180.51630.059*
C260.5618 (2)0.91583 (9)0.66831 (19)0.0506 (7)
H260.58700.95110.67400.061*
C270.6238 (2)0.88133 (7)0.7529 (2)0.0505 (7)
H270.69300.89280.81700.061*
C280.5857 (2)0.83023 (8)0.7449 (2)0.0377 (5)
H280.62820.80710.80480.045*
C290.75300 (19)0.63414 (7)0.60830 (16)0.0236 (4)
C300.75663 (16)0.59539 (10)0.53180 (14)0.0268 (3)
C310.8683 (2)0.56572 (7)0.56195 (17)0.0298 (4)
H310.87350.53850.51300.036*
C320.9723 (2)0.57425 (8)0.66043 (18)0.0282 (4)
C330.96708 (19)0.61368 (7)0.73284 (16)0.0253 (4)
H331.03800.62020.79980.030*
C340.85706 (19)0.64382 (7)0.70688 (16)0.0225 (4)
C350.85814 (18)0.68962 (7)0.77842 (16)0.0241 (4)
C360.85984 (19)0.68565 (7)0.88844 (16)0.0240 (4)
C370.8629 (2)0.72994 (8)0.95425 (16)0.0260 (4)
C380.8742 (2)0.77697 (8)0.90746 (17)0.0285 (4)
H380.88070.80740.95160.034*
C390.8764 (2)0.78185 (7)0.79794 (18)0.0277 (4)
C400.86457 (19)0.73841 (7)0.73202 (17)0.0256 (4)
H400.86080.74140.65570.031*
C410.65315 (19)0.58828 (10)0.41376 (16)0.0347 (5)
C420.6587 (4)0.63533 (12)0.3432 (2)0.0581 (8)
H42A0.62970.66590.37350.087*
H42B0.60310.62980.26460.087*
H42C0.74680.64060.34620.087*
C430.5178 (2)0.58264 (12)0.4152 (2)0.0536 (8)
H43A0.49340.61440.44530.080*
H43B0.51430.55330.46330.080*
H43C0.45850.57670.33810.080*
C440.6792 (3)0.53988 (12)0.3542 (2)0.0529 (8)
H44A0.61220.53630.27970.079*
H44B0.67940.50920.40000.079*
H44C0.76250.54320.34490.079*
C451.1894 (2)0.55561 (10)0.7650 (2)0.0428 (5)
H45A1.21510.59110.75560.064*
H45B1.25720.53160.76430.064*
H45C1.17510.55260.83720.064*
C460.8585 (2)0.72778 (9)1.07566 (17)0.0338 (5)
C470.7439 (3)0.69620 (10)1.0791 (2)0.0415 (6)
H47A0.75340.66021.05880.062*
H47B0.66510.71071.02520.062*
H47C0.73990.69751.15560.062*
C480.9848 (3)0.70463 (10)1.15472 (19)0.0438 (6)
H48A0.98230.70211.23160.066*
H48B1.05600.72691.15520.066*
H48C0.99650.67011.12790.066*
C490.8440 (3)0.78176 (9)1.11995 (19)0.0455 (6)
H49A0.83710.77871.19520.068*
H49B0.76670.79831.06810.068*
H49C0.91880.80281.12490.068*
C500.8673 (3)0.83944 (9)0.6481 (2)0.0445 (6)
H50A0.92700.81890.62370.067*
H50B0.87830.87620.63490.067*
H50C0.77940.82900.60470.067*
C510.8631 (2)0.51759 (7)1.06368 (16)0.0272 (4)
C520.9253 (2)0.50443 (7)0.96605 (16)0.0258 (4)
C530.9628 (2)0.52742 (7)1.17970 (17)0.0333 (5)
C540.9590 (3)0.57220 (9)1.23876 (18)0.0436 (6)
H540.89480.59741.20560.052*
C551.0473 (3)0.58061 (11)1.3451 (2)0.0635 (8)
H551.04340.61151.38450.076*
C561.1416 (3)0.54451 (14)1.3952 (2)0.0684 (9)
H561.20290.55081.46810.082*
C571.1457 (3)0.49955 (12)1.3383 (2)0.0553 (7)
H571.20910.47421.37220.066*
C581.0572 (2)0.49143 (9)1.23184 (19)0.0410 (5)
H581.06090.46031.19300.049*
C590.7618 (2)0.47876 (8)1.06974 (19)0.0297 (5)
C600.7693 (2)0.45389 (8)1.1700 (2)0.0407 (5)
H600.83760.46191.23790.049*
C610.6786 (2)0.41769 (9)1.1717 (2)0.0525 (7)
H610.68540.40091.24060.063*
C620.5784 (3)0.40585 (10)1.07396 (18)0.0524 (7)
H620.51810.38001.07460.063*
C630.5666 (2)0.43203 (9)0.9752 (2)0.0488 (6)
H630.49630.42500.90810.059*
C640.6570 (2)0.46836 (8)0.9739 (2)0.0382 (5)
H640.64700.48660.90590.046*
C651.0696 (2)0.51295 (9)1.00494 (17)0.0320 (5)
C661.1212 (2)0.56104 (10)1.04461 (18)0.0391 (5)
H661.06580.58881.04570.047*
C671.25186 (18)0.56925 (11)1.0827 (2)0.0546 (7)
H671.28540.60241.11020.065*
C681.3338 (3)0.52943 (10)1.0807 (2)0.0651 (9)
H681.42370.53481.10780.078*
C691.2832 (2)0.48177 (11)1.0386 (2)0.0635 (9)
H691.33870.45441.03550.076*
C701.1525 (2)0.47359 (10)1.0011 (2)0.0458 (6)
H701.11910.44060.97240.055*
C710.8872 (2)0.45146 (8)0.91157 (18)0.0300 (4)
C720.9014 (2)0.40673 (8)0.9771 (2)0.0355 (5)
H720.93860.40891.05720.043*
C730.8617 (3)0.35940 (9)0.9266 (2)0.0446 (6)
H730.87110.32930.97220.053*
C740.8087 (3)0.35539 (10)0.8108 (3)0.0591 (8)
H740.77850.32300.77610.071*
C750.7999 (4)0.39903 (10)0.7457 (2)0.0620 (8)
H750.76640.39640.66550.074*
C760.8393 (3)0.44637 (9)0.79552 (19)0.0419 (6)
H760.83340.47600.74920.050*
O10.41561 (13)0.67214 (5)0.57154 (11)0.0249 (3)
O20.56444 (13)0.72564 (5)0.70404 (11)0.0258 (3)
O30.64584 (13)0.66599 (5)0.58506 (11)0.0265 (3)
O40.87143 (14)0.63686 (5)0.93978 (11)0.0266 (3)
O50.79305 (14)0.56579 (5)1.02459 (11)0.0285 (3)
O60.86838 (14)0.54274 (5)0.87786 (11)0.0258 (3)
O70.5764 (3)0.49777 (8)0.6399 (2)0.0890 (9)
O80.4804 (2)0.60351 (9)0.97680 (18)0.0691 (6)
O91.07528 (16)0.54333 (6)0.67518 (14)0.0421 (4)
O100.89204 (16)0.83106 (5)0.76520 (13)0.0341 (3)
P10.55672 (5)0.66565 (2)0.66426 (4)0.02305 (10)
P20.78003 (5)0.586778 (19)0.90123 (4)0.02370 (10)
Rh10.574142 (14)0.594078 (6)0.777762 (12)0.02906 (4)
H10.444 (3)0.5921 (15)0.708 (2)0.062 (7)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.0549 (18)0.0355 (13)0.0473 (15)0.0018 (12)0.0045 (13)0.0005 (12)
C20.0323 (11)0.0520 (15)0.0581 (13)0.0060 (12)0.0228 (10)0.0182 (13)
C30.0249 (10)0.0200 (8)0.0234 (9)0.0035 (7)0.0074 (7)0.0006 (7)
C40.0210 (10)0.0247 (9)0.0263 (9)0.0047 (7)0.0052 (7)0.0008 (7)
C50.0339 (12)0.0267 (9)0.0273 (10)0.0069 (8)0.0129 (9)0.0036 (8)
C60.0387 (13)0.0452 (13)0.0293 (11)0.0082 (10)0.0117 (9)0.0003 (9)
C70.0610 (18)0.0641 (17)0.0280 (11)0.0204 (14)0.0166 (11)0.0042 (11)
C80.076 (2)0.0670 (17)0.0435 (14)0.0223 (16)0.0392 (15)0.0192 (13)
C90.0569 (17)0.0479 (14)0.0683 (18)0.0032 (12)0.0427 (15)0.0115 (12)
C100.0402 (13)0.0351 (11)0.0430 (12)0.0011 (10)0.0215 (11)0.0007 (9)
C110.0260 (10)0.0246 (9)0.0206 (8)0.0017 (8)0.0063 (7)0.0038 (7)
C120.0292 (11)0.0289 (10)0.0298 (10)0.0006 (8)0.0086 (8)0.0012 (8)
C130.0319 (12)0.0392 (11)0.0353 (11)0.0044 (9)0.0148 (9)0.0018 (9)
C140.0250 (11)0.0433 (12)0.0345 (11)0.0029 (9)0.0084 (9)0.0090 (9)
C150.0284 (11)0.0361 (11)0.0297 (10)0.0103 (9)0.0010 (8)0.0031 (8)
C160.0299 (11)0.0272 (10)0.0268 (10)0.0024 (8)0.0062 (8)0.0006 (7)
C170.0279 (11)0.0267 (9)0.0242 (9)0.0002 (8)0.0069 (8)0.0060 (7)
C180.0301 (11)0.0311 (10)0.0324 (11)0.0047 (9)0.0092 (9)0.0064 (8)
C190.0338 (13)0.0451 (13)0.0468 (13)0.0075 (10)0.0189 (10)0.0047 (10)
C200.0677 (19)0.0566 (16)0.0576 (16)0.0150 (14)0.0463 (15)0.0055 (13)
C210.093 (2)0.0676 (18)0.0553 (17)0.0359 (18)0.0504 (17)0.0264 (14)
C220.0567 (16)0.0516 (14)0.0386 (12)0.0277 (12)0.0241 (12)0.0081 (10)
C230.0251 (11)0.0271 (9)0.0362 (11)0.0006 (8)0.0136 (9)0.0079 (8)
C240.0422 (14)0.0289 (10)0.0471 (13)0.0032 (10)0.0106 (11)0.0014 (9)
C250.0583 (18)0.0297 (11)0.0613 (16)0.0021 (11)0.0217 (14)0.0027 (11)
C260.0515 (17)0.0288 (11)0.0818 (19)0.0114 (11)0.0359 (15)0.0152 (12)
C270.0357 (14)0.0423 (13)0.0729 (18)0.0080 (11)0.0179 (13)0.0277 (13)
C280.0309 (12)0.0329 (11)0.0449 (12)0.0017 (9)0.0076 (10)0.0102 (9)
C290.0230 (10)0.0228 (8)0.0267 (9)0.0005 (7)0.0108 (8)0.0015 (7)
C300.0261 (8)0.0258 (8)0.0289 (8)0.0002 (11)0.0098 (7)0.0012 (10)
C310.0312 (11)0.0252 (10)0.0340 (10)0.0036 (8)0.0126 (9)0.0061 (8)
C320.0262 (11)0.0260 (9)0.0347 (10)0.0041 (8)0.0135 (8)0.0000 (8)
C330.0219 (10)0.0274 (8)0.0265 (9)0.0022 (7)0.0083 (8)0.0014 (7)
C340.0249 (10)0.0205 (8)0.0254 (9)0.0012 (7)0.0127 (8)0.0005 (7)
C350.0199 (10)0.0258 (9)0.0259 (9)0.0003 (7)0.0070 (7)0.0029 (7)
C360.0223 (10)0.0243 (9)0.0259 (9)0.0024 (7)0.0089 (8)0.0004 (7)
C370.0220 (10)0.0302 (10)0.0233 (9)0.0022 (8)0.0045 (8)0.0037 (8)
C380.0255 (11)0.0278 (10)0.0298 (10)0.0024 (8)0.0066 (8)0.0080 (8)
C390.0271 (11)0.0231 (9)0.0341 (10)0.0015 (8)0.0123 (9)0.0018 (8)
C400.0256 (11)0.0255 (9)0.0266 (9)0.0002 (8)0.0101 (8)0.0005 (7)
C410.0315 (10)0.0393 (12)0.0298 (9)0.0041 (11)0.0061 (7)0.0084 (10)
C420.069 (2)0.0575 (17)0.0351 (14)0.0011 (15)0.0024 (13)0.0005 (12)
C430.0320 (12)0.081 (2)0.0413 (12)0.0052 (13)0.0050 (9)0.0233 (13)
C440.0440 (17)0.0582 (17)0.0421 (14)0.0096 (13)0.0032 (12)0.0272 (12)
C450.0266 (12)0.0497 (13)0.0498 (14)0.0097 (10)0.0102 (10)0.0030 (11)
C460.0405 (13)0.0381 (11)0.0235 (9)0.0011 (9)0.0117 (9)0.0047 (8)
C470.0504 (16)0.0441 (14)0.0369 (13)0.0003 (12)0.0238 (12)0.0023 (10)
C480.0474 (15)0.0489 (14)0.0285 (11)0.0017 (11)0.0049 (10)0.0038 (10)
C490.0662 (18)0.0410 (12)0.0310 (11)0.0029 (12)0.0191 (11)0.0073 (9)
C500.0620 (17)0.0319 (11)0.0430 (13)0.0021 (11)0.0225 (12)0.0072 (9)
C510.0318 (11)0.0258 (9)0.0262 (9)0.0054 (8)0.0128 (8)0.0046 (7)
C520.0262 (11)0.0271 (9)0.0250 (9)0.0050 (8)0.0103 (8)0.0060 (7)
C530.0379 (13)0.0385 (11)0.0250 (10)0.0000 (9)0.0127 (9)0.0043 (8)
C540.0526 (16)0.0460 (12)0.0314 (11)0.0057 (11)0.0136 (10)0.0014 (9)
C550.084 (2)0.062 (2)0.0370 (12)0.0020 (15)0.0107 (13)0.0136 (12)
C560.072 (2)0.089 (2)0.0295 (13)0.0022 (18)0.0022 (13)0.0054 (14)
C570.0528 (17)0.0710 (19)0.0356 (13)0.0133 (14)0.0069 (12)0.0103 (12)
C580.0445 (14)0.0481 (13)0.0293 (11)0.0094 (11)0.0112 (10)0.0067 (10)
C590.0369 (13)0.0248 (10)0.0343 (11)0.0063 (9)0.0211 (10)0.0057 (8)
C600.0554 (16)0.0352 (11)0.0409 (12)0.0044 (11)0.0287 (12)0.0091 (10)
C610.071 (2)0.0415 (13)0.0588 (16)0.0022 (13)0.0407 (16)0.0163 (12)
C620.0511 (17)0.0388 (13)0.081 (2)0.0036 (12)0.0399 (16)0.0117 (13)
C630.0361 (14)0.0475 (14)0.0645 (17)0.0049 (11)0.0196 (13)0.0049 (12)
C640.0335 (13)0.0384 (12)0.0461 (13)0.0018 (10)0.0180 (11)0.0111 (10)
C650.0288 (11)0.0412 (12)0.0262 (10)0.0039 (9)0.0098 (8)0.0104 (8)
C660.0323 (12)0.0510 (13)0.0320 (11)0.0076 (10)0.0084 (9)0.0029 (10)
C670.0355 (14)0.0747 (18)0.0444 (14)0.0131 (13)0.0023 (11)0.0148 (13)
C680.0260 (14)0.100 (2)0.0613 (17)0.0023 (15)0.0052 (12)0.0395 (17)
C690.0347 (15)0.081 (2)0.081 (2)0.0246 (15)0.0285 (15)0.0445 (17)
C700.0333 (13)0.0500 (14)0.0572 (15)0.0129 (11)0.0196 (11)0.0210 (12)
C710.0294 (12)0.0295 (10)0.0356 (11)0.0037 (8)0.0170 (9)0.0009 (8)
C720.0394 (13)0.0304 (11)0.0401 (12)0.0096 (9)0.0180 (10)0.0074 (9)
C730.0563 (16)0.0260 (10)0.0588 (15)0.0044 (10)0.0294 (13)0.0051 (10)
C740.083 (2)0.0314 (12)0.0650 (18)0.0071 (13)0.0281 (17)0.0115 (12)
C750.096 (3)0.0431 (14)0.0418 (14)0.0058 (15)0.0176 (16)0.0098 (11)
C760.0628 (17)0.0309 (11)0.0324 (11)0.0014 (11)0.0169 (11)0.0003 (9)
O10.0233 (7)0.0216 (6)0.0277 (7)0.0013 (5)0.0060 (5)0.0010 (5)
O20.0208 (7)0.0273 (7)0.0261 (6)0.0041 (5)0.0041 (5)0.0031 (5)
O30.0251 (7)0.0269 (6)0.0270 (7)0.0056 (6)0.0084 (6)0.0006 (5)
O40.0296 (8)0.0247 (7)0.0222 (7)0.0006 (6)0.0047 (6)0.0021 (5)
O50.0336 (8)0.0256 (7)0.0291 (7)0.0061 (6)0.0145 (6)0.0048 (5)
O60.0300 (8)0.0251 (7)0.0225 (6)0.0036 (6)0.0092 (6)0.0038 (5)
O70.115 (2)0.0415 (11)0.0759 (15)0.0036 (13)0.0104 (14)0.0194 (11)
O80.0672 (13)0.0842 (17)0.0769 (13)0.0133 (12)0.0514 (11)0.0264 (12)
O90.0313 (9)0.0427 (9)0.0463 (9)0.0127 (7)0.0056 (7)0.0105 (7)
O100.0423 (9)0.0219 (7)0.0406 (8)0.0021 (6)0.0176 (7)0.0014 (6)
P10.0218 (3)0.0234 (2)0.0234 (2)0.0023 (2)0.0071 (2)0.00024 (19)
P20.0243 (2)0.0229 (3)0.0240 (2)0.0010 (2)0.00854 (17)0.00250 (18)
Rh10.02251 (7)0.02832 (7)0.03357 (7)0.00073 (8)0.00617 (5)0.00755 (8)
Geometric parameters (Å, º) top
C77—C781.414 (5)C41—C421.520 (4)
C77—H77A0.9800C41—C431.523 (3)
C77—H77B0.9800C41—C441.537 (3)
C77—H77C0.9800C42—H42A0.9800
C78—O111.369 (4)C42—H42B0.9800
C78—H78A0.9900C42—H42C0.9800
C78—H78B0.9900C43—H43A0.9800
C79—O111.377 (4)C43—H43B0.9800
C79—C801.415 (5)C43—H43C0.9800
C79—H79A0.9900C44—H44A0.9800
C79—H79B0.9900C44—H44B0.9800
C80—H80A0.9800C44—H44C0.9800
C80—H80B0.9800C45—O91.415 (3)
C80—H80C0.9800C45—H45A0.9800
C1—O71.132 (3)C45—H45B0.9800
C1—Rh11.909 (3)C45—H45C0.9800
C2—O81.133 (3)C46—C471.529 (4)
C2—Rh11.909 (2)C46—C491.532 (3)
C3—O11.464 (2)C46—C481.536 (3)
C3—C111.528 (3)C47—H47A0.9800
C3—C51.531 (3)C47—H47B0.9800
C3—C41.604 (3)C47—H47C0.9800
C4—O21.453 (2)C48—H48A0.9800
C4—C231.524 (3)C48—H48B0.9800
C4—C171.537 (3)C48—H48C0.9800
C5—C61.388 (3)C49—H49A0.9800
C5—C101.398 (3)C49—H49B0.9800
C6—C71.3814 (18)C49—H49C0.9800
C6—H60.9500C50—O101.421 (3)
C7—C81.3797 (19)C50—H50A0.9800
C7—H70.9500C50—H50B0.9800
C8—C91.3811 (19)C50—H50C0.9800
C8—H80.9500C51—O51.462 (2)
C9—C101.3811 (18)C51—C531.520 (3)
C9—H90.9500C51—C591.532 (3)
C10—H100.9500C51—C521.643 (3)
C11—C121.387 (3)C52—O61.459 (2)
C11—C161.392 (3)C52—C711.524 (3)
C12—C131.390 (3)C52—C651.527 (3)
C12—H120.9500C53—C541.385 (2)
C13—C141.378 (3)C53—C581.387 (2)
C13—H130.9500C54—C551.377 (4)
C14—C151.372 (3)C54—H540.9500
C14—H140.9500C55—C561.384 (4)
C15—C161.382 (3)C55—H550.9500
C15—H150.9500C56—C571.374 (4)
C16—H160.9500C56—H560.9500
C17—C221.386 (2)C57—C581.378 (4)
C17—C181.391 (2)C57—H570.9500
C18—C191.3779 (18)C58—H580.9500
C18—H180.9500C59—C641.385 (3)
C19—C201.3754 (18)C59—C601.393 (3)
C19—H190.9500C60—C611.3835 (19)
C20—C211.3751 (18)C60—H600.9500
C20—H200.9500C61—C621.3805 (19)
C21—C221.3778 (18)C61—H610.9500
C21—H210.9500C62—C631.3817 (19)
C22—H220.9500C62—H620.9500
C23—C281.385 (3)C63—C641.3814 (19)
C23—C241.389 (3)C63—H630.9500
C24—C251.3800 (18)C64—H640.9500
C24—H240.9500C65—C701.386 (3)
C25—C261.3791 (18)C65—C661.388 (3)
C25—H250.9500C66—C671.3835 (19)
C26—C271.3775 (18)C66—H660.9500
C26—H260.9500C67—C681.3823 (19)
C27—C281.3802 (18)C67—H670.9500
C27—H270.9500C68—C691.382 (2)
C28—H280.9500C68—H680.9500
C29—O31.396 (2)C69—C701.3840 (19)
C29—C341.397 (3)C69—H690.9500
C29—C301.400 (3)C70—H700.9500
C30—C311.398 (3)C71—C761.378 (3)
C30—C411.545 (2)C71—C721.397 (3)
C31—C321.391 (3)C72—C731.379 (3)
C31—H310.9500C72—H720.9500
C32—O91.358 (2)C73—C741.375 (4)
C32—C331.382 (3)C73—H730.9500
C33—C341.393 (3)C74—C751.378 (4)
C33—H330.9500C74—H740.9500
C34—C351.485 (3)C75—C761.376 (3)
C35—C361.383 (3)C75—H750.9500
C35—C401.402 (3)C76—H760.9500
C36—O41.403 (2)O1—P11.6106 (14)
C36—C371.407 (3)O2—P11.6224 (14)
C37—C381.375 (3)O3—P11.6336 (14)
C37—C461.548 (3)O4—P21.6146 (14)
C38—C391.394 (3)O5—P21.6039 (14)
C38—H380.9500O6—P21.5979 (14)
C39—O101.367 (2)P1—Rh12.3045 (5)
C39—C401.375 (3)P2—Rh12.2913 (5)
C40—H400.9500Rh1—H11.42 (3)
C78—C77—H77A109.5H43A—C43—H43B109.5
C78—C77—H77B109.5C41—C43—H43C109.5
H77A—C77—H77B109.5H43A—C43—H43C109.5
C78—C77—H77C109.5H43B—C43—H43C109.5
H77A—C77—H77C109.5C41—C44—H44A109.5
H77B—C77—H77C109.5C41—C44—H44B109.5
O11—C78—C77116.2 (4)H44A—C44—H44B109.5
O11—C78—H78A108.2C41—C44—H44C109.5
C77—C78—H78A108.2H44A—C44—H44C109.5
O11—C78—H78B108.2H44B—C44—H44C109.5
C77—C78—H78B108.2O9—C45—H45A109.5
H78A—C78—H78B107.4O9—C45—H45B109.5
O11—C79—C80109.3 (5)H45A—C45—H45B109.5
O11—C79—H79A109.8O9—C45—H45C109.5
C80—C79—H79A109.8H45A—C45—H45C109.5
O11—C79—H79B109.8H45B—C45—H45C109.5
C80—C79—H79B109.8C47—C46—C49106.3 (2)
H79A—C79—H79B108.3C47—C46—C48111.1 (2)
C79—C80—H80A109.5C49—C46—C48107.92 (19)
C79—C80—H80B109.5C47—C46—C37111.10 (18)
H80A—C80—H80B109.5C49—C46—C37111.75 (18)
C79—C80—H80C109.5C48—C46—C37108.60 (18)
H80A—C80—H80C109.5C46—C47—H47A109.5
H80B—C80—H80C109.5C46—C47—H47B109.5
C78—O11—C79118.4 (4)H47A—C47—H47B109.5
O7—C1—Rh1177.5 (3)C46—C47—H47C109.5
O8—C2—Rh1179.4 (2)H47A—C47—H47C109.5
O1—C3—C11106.33 (15)H47B—C47—H47C109.5
O1—C3—C5106.10 (14)C46—C48—H48A109.5
C11—C3—C5112.30 (15)C46—C48—H48B109.5
O1—C3—C4101.22 (13)H48A—C48—H48B109.5
C11—C3—C4112.02 (15)C46—C48—H48C109.5
C5—C3—C4117.43 (16)H48A—C48—H48C109.5
O2—C4—C23107.17 (16)H48B—C48—H48C109.5
O2—C4—C17108.77 (14)C46—C49—H49A109.5
C23—C4—C17106.57 (15)C46—C49—H49B109.5
O2—C4—C3102.67 (14)H49A—C49—H49B109.5
C23—C4—C3119.38 (16)C46—C49—H49C109.5
C17—C4—C3111.80 (16)H49A—C49—H49C109.5
C6—C5—C10118.05 (19)H49B—C49—H49C109.5
C6—C5—C3118.22 (19)O10—C50—H50A109.5
C10—C5—C3123.49 (18)O10—C50—H50B109.5
C7—C6—C5120.7 (2)H50A—C50—H50B109.5
C7—C6—H6119.6O10—C50—H50C109.5
C5—C6—H6119.6H50A—C50—H50C109.5
C8—C7—C6120.9 (2)H50B—C50—H50C109.5
C8—C7—H7119.6O5—C51—C53107.98 (15)
C6—C7—H7119.6O5—C51—C59104.95 (16)
C7—C8—C9118.9 (2)C53—C51—C59111.58 (17)
C7—C8—H8120.5O5—C51—C52103.82 (14)
C9—C8—H8120.5C53—C51—C52113.35 (17)
C10—C9—C8120.6 (2)C59—C51—C52114.28 (16)
C10—C9—H9119.7O6—C52—C71106.68 (16)
C8—C9—H9119.7O6—C52—C65106.17 (15)
C9—C10—C5120.7 (2)C71—C52—C65111.83 (17)
C9—C10—H10119.6O6—C52—C51104.14 (14)
C5—C10—H10119.6C71—C52—C51113.51 (16)
C12—C11—C16118.27 (19)C65—C52—C51113.65 (16)
C12—C11—C3120.83 (17)C54—C53—C58117.7 (2)
C16—C11—C3120.76 (17)C54—C53—C51120.52 (18)
C11—C12—C13120.4 (2)C58—C53—C51121.69 (17)
C11—C12—H12119.8C55—C54—C53120.6 (2)
C13—C12—H12119.8C55—C54—H54119.7
C14—C13—C12120.5 (2)C53—C54—H54119.7
C14—C13—H13119.7C54—C55—C56120.8 (2)
C12—C13—H13119.7C54—C55—H55119.6
C15—C14—C13119.4 (2)C56—C55—H55119.6
C15—C14—H14120.3C57—C56—C55119.3 (3)
C13—C14—H14120.3C57—C56—H56120.3
C14—C15—C16120.5 (2)C55—C56—H56120.3
C14—C15—H15119.8C56—C57—C58119.6 (3)
C16—C15—H15119.8C56—C57—H57120.2
C15—C16—C11120.9 (2)C58—C57—H57120.2
C15—C16—H16119.6C57—C58—C53121.9 (2)
C11—C16—H16119.6C57—C58—H58119.0
C22—C17—C18117.48 (19)C53—C58—H58119.0
C22—C17—C4121.93 (16)C64—C59—C60117.9 (2)
C18—C17—C4120.58 (15)C64—C59—C51119.84 (18)
C19—C18—C17121.18 (18)C60—C59—C51122.2 (2)
C19—C18—H18119.4C61—C60—C59120.8 (2)
C17—C18—H18119.4C61—C60—H60119.6
C20—C19—C18120.6 (2)C59—C60—H60119.6
C20—C19—H19119.7C62—C61—C60120.4 (2)
C18—C19—H19119.7C62—C61—H61119.8
C21—C20—C19118.8 (2)C60—C61—H61119.8
C21—C20—H20120.6C61—C62—C63119.3 (2)
C19—C20—H20120.6C61—C62—H62120.4
C20—C21—C22120.8 (2)C63—C62—H62120.4
C20—C21—H21119.6C64—C63—C62120.1 (2)
C22—C21—H21119.6C64—C63—H63120.0
C21—C22—C17121.1 (2)C62—C63—H63120.0
C21—C22—H22119.5C63—C64—C59121.3 (2)
C17—C22—H22119.5C63—C64—H64119.3
C28—C23—C24117.27 (19)C59—C64—H64119.3
C28—C23—C4117.01 (18)C70—C65—C66118.1 (2)
C24—C23—C4125.52 (18)C70—C65—C52121.6 (2)
C25—C24—C23121.3 (2)C66—C65—C52120.26 (19)
C25—C24—H24119.3C67—C66—C65121.2 (2)
C23—C24—H24119.3C67—C66—H66119.4
C26—C25—C24120.5 (2)C65—C66—H66119.4
C26—C25—H25119.8C68—C67—C66120.2 (3)
C24—C25—H25119.8C68—C67—H67119.9
C27—C26—C25119.0 (2)C66—C67—H67119.9
C27—C26—H26120.5C69—C68—C67119.1 (2)
C25—C26—H26120.5C69—C68—H68120.5
C26—C27—C28120.2 (2)C67—C68—H68120.5
C26—C27—H27119.9C68—C69—C70120.6 (3)
C28—C27—H27119.9C68—C69—H69119.7
C27—C28—C23121.7 (2)C70—C69—H69119.7
C27—C28—H28119.2C69—C70—C65120.8 (2)
C23—C28—H28119.2C69—C70—H70119.6
O3—C29—C34117.88 (16)C65—C70—H70119.6
O3—C29—C30120.28 (16)C76—C71—C72118.1 (2)
C34—C29—C30121.78 (17)C76—C71—C52120.57 (19)
C31—C30—C29116.15 (16)C72—C71—C52121.4 (2)
C31—C30—C41119.61 (18)C73—C72—C71120.6 (2)
C29—C30—C41123.87 (18)C73—C72—H72119.7
C32—C31—C30122.95 (18)C71—C72—H72119.7
C32—C31—H31118.5C74—C73—C72120.5 (2)
C30—C31—H31118.5C74—C73—H73119.8
O9—C32—C33124.77 (19)C72—C73—H73119.8
O9—C32—C31115.64 (17)C73—C74—C75119.0 (2)
C33—C32—C31119.53 (18)C73—C74—H74120.5
C32—C33—C34119.48 (18)C75—C74—H74120.5
C32—C33—H33120.3C76—C75—C74120.7 (3)
C34—C33—H33120.3C76—C75—H75119.6
C33—C34—C29120.07 (17)C74—C75—H75119.6
C33—C34—C35118.81 (17)C75—C76—C71120.9 (2)
C29—C34—C35120.77 (17)C75—C76—H76119.5
C36—C35—C40119.96 (17)C71—C76—H76119.5
C36—C35—C34122.90 (17)C3—O1—P1115.21 (11)
C40—C35—C34117.05 (17)C4—O2—P1115.76 (11)
C35—C36—O4119.71 (16)C29—O3—P1121.75 (12)
C35—C36—C37121.26 (18)C36—O4—P2129.38 (13)
O4—C36—C37118.72 (17)C51—O5—P2118.22 (12)
C38—C37—C36117.00 (18)C52—O6—P2118.46 (12)
C38—C37—C46119.60 (18)C32—O9—C45117.47 (17)
C36—C37—C46123.37 (18)C39—O10—C50117.12 (16)
C37—C38—C39122.65 (18)O1—P1—O293.35 (7)
C37—C38—H38118.7O1—P1—O3101.81 (7)
C39—C38—H38118.7O2—P1—O3101.83 (7)
O10—C39—C40124.98 (18)O1—P1—Rh1112.62 (5)
O10—C39—C38115.50 (17)O2—P1—Rh1126.26 (5)
C40—C39—C38119.52 (18)O3—P1—Rh1116.40 (5)
C39—C40—C35119.39 (18)O6—P2—O594.75 (7)
C39—C40—H40120.3O6—P2—O4105.15 (8)
C35—C40—H40120.3O5—P2—O498.27 (7)
C42—C41—C43109.0 (2)O6—P2—Rh1118.05 (6)
C42—C41—C44108.3 (2)O5—P2—Rh1114.74 (6)
C43—C41—C44106.5 (2)O4—P2—Rh1121.17 (5)
C42—C41—C30107.4 (2)C1—Rh1—C2127.99 (13)
C43—C41—C30114.37 (17)C1—Rh1—P295.80 (9)
C44—C41—C30111.23 (19)C2—Rh1—P289.60 (7)
C41—C42—H42A109.5C1—Rh1—P1108.58 (9)
C41—C42—H42B109.5C2—Rh1—P1117.99 (9)
H42A—C42—H42B109.5P2—Rh1—P1109.662 (19)
C41—C42—H42C109.5C1—Rh1—H180.9 (14)
H42A—C42—H42C109.5C2—Rh1—H186.9 (10)
H42B—C42—H42C109.5P2—Rh1—H1172.1 (14)
C41—C43—H43A109.5P1—Rh1—H178.3 (14)
C41—C43—H43B109.5

Experimental details

Crystal data
Chemical formula[Rh(C74H68O8P2)H(CO)2]·C4H10O
Mr1381.28
Crystal system, space groupMonoclinic, P21
Temperature (K)200
a, b, c (Å)11.1489 (2), 25.8458 (4), 12.5941 (3)
β (°) 110.263 (2)
V3)3404.43 (11)
Z2
Radiation typeMo Kα
µ (mm1)0.36
Crystal size (mm)0.40 × 0.35 × 0.15
Data collection
DiffractometerStoe IPDS II
Absorption correctionNumerical
(X-SHAPE and X-RED32; Stoe & Cie, 2005)
Tmin, Tmax0.835, 0.959
No. of measured, independent and
observed [I > 2σ(I)] reflections
59171, 16262, 14238
Rint0.026
(sin θ/λ)max1)0.659
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.028, 0.063, 0.94
No. of reflections16262
No. of parameters834
No. of restraints35
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)0.66, 0.47
Absolute structureFlack (1983), 7944 Friedel pairs
Absolute structure parameter0.026 (11)

Computer programs: X-AREA (Stoe & Cie, 2005), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), XP in SHELXTL (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

 

References

First citationAxet, M. R., Benet-Buchholz, J., Claver, C. & Castillón, S. (2007). Adv. Synth. Catal. 349, 1983–1998.  Web of Science CSD CrossRef CAS Google Scholar
First citationDieleman, C. B., Kamer, P. C. J., Reek, J. N. H. & van Leeuwen, P. W. N. M. (2001). Helv. Chim. Acta, 84, 3269–3280.  CrossRef CAS Google Scholar
First citationFlack, H. D. (1983). Acta Cryst. A39, 876–881.  CrossRef CAS Web of Science IUCr Journals Google Scholar
First citationSelent, D., Franke, R., Kubis, C., Spannenberg, A., Baumann, W., Kreidler, B. & Börner, A. (2011). Organometallics, 30, 4509–4514.  Web of Science CSD CrossRef CAS Google Scholar
First citationSheldrick, G. M. (2008). Acta Cryst. A64, 112–122.  Web of Science CrossRef CAS IUCr Journals Google Scholar
First citationStoe & Cie (2005). X-SHAPE, X-RED32 and X-AREA. Stoe & Cie, Darmstadt, Germany.  Google Scholar
First citationVan Rooy, A., Kamer, P. C. J., van Leeuwen, P. W. N. M., Goubitz, K., Fraanje, J., Veldman, N. & Spek, A. L. (1996). Organometallics, 15, 835–847.  CrossRef CAS Google Scholar
First citationVan Rooy, A., Kamer, P. C. J., van Leeuwen, P. W. N. M., Veldman, N. & Spek, A. L. (1995). J. Organomet. Chem. 494, C15–C18.  CAS Google Scholar

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