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The title mononuclear chromium compound, [Cr(C32H28P2)(CO)3], (I), and its rhodium complexes [CrRh(C7H8)(C32H28P2)(CO)3]BF4·0.75CH4O, (II), and [CrRh(C8H12)(C32H28P2)(CO)3]BF4·1.5CH4O, (III), prepared as a ligand and precatalysts, respectively, for application in asymmetric homogeneous hydrogenation, have been studied by single-crystal X-ray diffraction. The structures of the free and complexed ligand are compared. It was found that the backbone of the ligand remains rigid on coordination, while only minor conformational changes of its side chains are observed. Both elements of central and planar chirality seem to build a well defined chiral environment for stereoselective catalysis.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270104020773/tr1096sup1.cif
Contains datablocks global, I, II, III

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270104020773/tr1096Isup2.hkl
Contains datablock I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270104020773/tr1096IIsup3.hkl
Contains datablock II

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270104020773/tr1096IIIsup4.hkl
Contains datablock III

CCDC references: 254914; 254915; 254916

Comment top

One of our main interests lies in the field of the design, synthesis and application of new chiral ligands for asymmetric hydrogenation, including those incorporating an organometallic framework. For compound (R,R)-(I), first introduced by Uemura (Hayashi et al., 1995) in its enantiomeric form (S,S)-(I), we have recently reported an alternative synthetic route (Vasen et al., 2000; Braun et al., 2003), depicted in Scheme 1 as route (a), together with Uemura's route, (b). Uemura's method starts from the (S)-[(1-methoxymethoxy)ethyl]benzene chromium tricarbonyl complex which, after deprotonation with s-BuLi and quenching with ClPPh2, gives the ortho-substituted product in a 50% yield. Subsequent deprotection with boron trifluoride etherate (38%) and nucleophilic substitution of the hydroxy group for PPh2 with tetrafluoroboric acid and diphenylphosphine (80%) leads to the diphosphine in an overall yield of just 15%. In contrast, we employed (R)-[(1-dimethylamino)ethyl] benzene chromium tricarbonyl as the starting material. From this, ortho-substitution by a deprotonation/electrophilic addition sequence with t-BuLi and diphenyl phosphine gives the planar chiral product in almost quantitative yield (98%). The dimethylamino group is then substituted for a Cl atom employing ACE-Cl (1-chloroethyl chloroformate) with 90% yield, and this can easily be exchanged for the desired diphenylphosphine group in 83% yield. The overall yield of the synthesis of (I) is 73%, significantly higher than the aforementioned compound. \sch

For application in catalysis we have complexed (I) to NBD-Rh- and COD-Rh- fragments (NBD is norbornadiene and COD is cyclooctadiene) by standard laboratory procedures (Gladiali, 2000), forming the complexes [(NBD)Rh(PPh2/PPh2)]BF4·0.75CH4O, (II), and [(COD)Rh(PPh2/PPh2)]BF4·1.5CH4O, (III). Here, we present an X-ray crystallographic study of both the ligand and the two rhodium complexes (Figs. 1–3). Scheme 2 here.

It should be mentioned that the supplementary material associated with Uemura's original report (Hayashi et al., 1995) refers to a compound in the centrosymmetric space group P21/c, and hence to a racemic crystal rather than enantiomerically pure crystals. In the free ligand, (I), as typical for piano-stool compounds like these, the Cr tripod is oriented eclipsed with respect to the arene ring. The three carbonyl ligands are oriented synperiplanar with the respective C atoms of the benzene ring. The bond lengths and angles of the title three complexes are similar to those of the already published structures of [(NBD)Rh(PPh2/PCy2)]BF4 and [(NBD)Rh(PCy2/PPh2)]BF4 (Braun et al., 2003). The NBD complex, (II), crystallizes with two complex cations and two anions (BF4) per asymmetric unit. The superposition of the two independent complex moieties and an analysis of the torsion angles (Table 4) shows that the geometry of the two molecules is almost the same, except for the phenyl rings on the P atoms, which adopt slightly different conformations, differing by about 9° in the two independent molecules of (II).

The deviation observed from square-planar towards a tetrahedral coordination sphere is characteristic. The dihedral angles between the planes defined by P/Rh/P and MP1/Rh/MP2 (MP denotes the midpoints of the coordinated double bond) are 3.3 (1) and 6.5 (1)° for (II), and 9.8 (1)° for (III). It is also found for rhodium diolefin complexes with other bisphosphine ligands that this dihedral angle is larger in COD complexes than in NBD complexes (Drexler et al., 2001; Spannenberg et al., 2001). No substantial change is found for the important bond lengths of the uncoordinated ligand on coordination to Rh (Tables 1–3).

Selected torsion angles may be used to describe the conformation of the chelate rings of the title complexes. Table 4 shows that these torsion angles do not differ significantly for the NBD complex, (II), and the COD complex, (III). For the group incorporating the α-C atom, as expected, it can be stated that it chooses a conformation in which the small H atom faces down towards the bulky chromium tricarbonyl moiety, while the diphenylphosphine group points away from the ring plane. We have calculated in (I) a dihedral angle for P2-α-C8—C6ipso—C1ortho of 68.9 (5)°. Since the two P atoms are in close proximity, they can readily coordinate a Rh centre. This dihedral angle does not change significantly on coordination to the Rh centre, as can be seen in Table 4. Nonetheless, a twist of 30° around the P—Casymm bond takes place, due to the orientation of the P lone pair towards the Rh.

Within the ligand, the four phenyl rings of both the ortho and the α diphenylphosphine groups adopt a conformation that exhibits a sense of helicity, probably induced by the asymmetry of the backbone of the ligand, which might lead to the formation of a chiral cavity for the prochiral substrate in the rhodium complex.

Table 4. Comparison of characteristic torsion angles in (I)-(III) (°).

Experimental top

The syntheses and complete characterization of complexes (I) and (II) (including all starting materials) are given by Braun et al. (2003). Single crystals were obtained from ethanol for (I) and from methanol for (II). Complex (III) was prepared according to the following procedure. In a Schlenk flask, [CODRhCl]2 (104 mg, 0.211 mmol) and AgBF4 (82 mg, 0.423 mmol) were dissolved in tetrahydrofuran (THF; 10 ml) and the solution was stirred vigorously for 30 min at ambient temperature. The AgCl which precipitated was filtered off using a syringe equipped with a filter needle, and the clear liquid dripped into a solution of (I) (258 mg; 0.423 mmol) in THF (5 ml). After stirring for 10 min, the product was precipitated by adding Et2O. The ether solution was discarded and the solid dried in vacuo. Single crystals of (III) were obtained by recrystallization from methanol.

Refinement top

H atoms were placed in calculated positions and refined using a riding model, with C—H distances of 0.98 Å and with Uiso(H) = 1.3Ueq(C). Please check added text. The BF4 anion in complex (III) is disordered. Two sets of F atoms were refined isotropically, each set with near half occupancy. For complexes (II) and (III), the final structure models show several peaks of relatively high electron density. In agreement with the 1H NMR data, this electron density was interpreted as two MeOH molecules for (II) and 1.5 molecules for (III) per unit cell (solvent of crystallization). In the case of (II), both solvent molecules are disordered and were treated as isotropic. For one solvent molecule, the position of the hydroxyl H atom attached to atom O8 was refined using a riding model, with O—H = 0.95 Å. The choice of the H-atom position was determined by the best hydrogen bond that could be created (O8···F6). For the second MeOH molecule, no hydrogen-bond acceptor was found in the neighbourhood of atom O7 and the maximum electron density was taken as the starting position for the H atom, and it was also treated as riding, with O—H = 0.95 Å. For both hydroxy H atoms, Uiso(H) = Ueq(O). For (III), the position of one solvent molecule was only half occupied. For both MeOH molecules, the maximum electron density was taken as the starting position for the hydroxy H atom and these were treated as riding, with O—H = 0.95 Å and Uiso(H) = 1.5Ueq(O). Please check all added text.

Computing details top

Data collection: SMART (Bruker, 2001) for (I), (II); EXPOSE in IPDS (Stoe & Cie, 1995) for (III). Cell refinement: SAINT-Plus (Bruker 1999) for (I), (II); CELL in IPDS for (III). Data reduction: SAINT-Plus for (I), (II); INTEGRATE in IPDS for (III). For all compounds, program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997). Molecular graphics: PLATON (Spek, 1990) for (I), (II); XP in SHELXTL (Bruker, 1999) for (III). For all compounds, software used to prepare material for publication: SHELXL97.

Figures top
[Figure 1] Fig. 1. A view of the structure of (I), with the atom-labelling scheme. Displacement ellipsoids are drawn at the 30% probability level and most H atoms have been omitted for clarity. Please check added text.
[Figure 2] Fig. 2. A view of the [(NBD)Rh(PPh2/PPh2)]+ cation of (II), with the atom-labelling scheme. Displacement ellipsoids are drawn at the 30% probability level and most H atoms have been omitted for clarity. Please check added text. The relative orientation of the two molecules in the plot does not reflect their true orientation in the asymmetric unit.
[Figure 3] Fig. 3. A view of the [(COD)Rh(PPh2/PPh2)]+ cation of (III), with the atom-labelling scheme. Displacement ellipsoids are drawn at the 30% probability level and most H atoms have been omitted for clarity. Please check added text.
(I) (R,R)-Tricarbonyl{η6-2-[1-diphenylphosphino-1- (diphenylphosphino)ethyl]benzene}chromium(0) top
Crystal data top
[Cr(C32H28P2)(CO)3]F(000) = 1264
Mr = 610.51Dx = 1.319 Mg m3
Orthorhombic, P212121Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2ac 2abCell parameters from 8096 reflections
a = 10.6758 (12) Åθ = 2.4–25.2°
b = 13.5533 (15) ŵ = 0.51 mm1
c = 21.255 (2) ÅT = 293 K
V = 3075.4 (6) Å3Rod, yellow
Z = 40.70 × 0.20 × 0.12 mm
Data collection top
Bruker SMART APEX CCD
diffractometer
5572 independent reflections
Radiation source: fine-focus sealed tube4996 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.044
Detector resolution: 0 pixels mm-1θmax = 25.2°, θmin = 2.4°
ϕ and ω scansh = 1212
Absorption correction: multi-scan
(SADABS; Sheldrick; 1996)
k = 1616
Tmin = 0.717, Tmax = 0.941l = 2525
33737 measured reflections
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)] = 0.042H-atom parameters constrained
wR(F2) = 0.098 w = 1/[σ2(Fo2) + (0.0546P)2 + 1.0577P]
where P = (Fo2 + 2Fc2)/3
S = 1.01(Δ/σ)max = 0.001
5572 reflectionsΔρmax = 0.33 e Å3
371 parametersΔρmin = 0.16 e Å3
0 restraintsAbsolute structure: Flack (1983), 2430 Friedel pairs
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.02 (2)
Crystal data top
[Cr(C32H28P2)(CO)3]V = 3075.4 (6) Å3
Mr = 610.51Z = 4
Orthorhombic, P212121Mo Kα radiation
a = 10.6758 (12) ŵ = 0.51 mm1
b = 13.5533 (15) ÅT = 293 K
c = 21.255 (2) Å0.70 × 0.20 × 0.12 mm
Data collection top
Bruker SMART APEX CCD
diffractometer
5572 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick; 1996)
4996 reflections with I > 2σ(I)
Tmin = 0.717, Tmax = 0.941Rint = 0.044
33737 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.042H-atom parameters constrained
wR(F2) = 0.098Δρmax = 0.33 e Å3
S = 1.01Δρmin = 0.16 e Å3
5572 reflectionsAbsolute structure: Flack (1983), 2430 Friedel pairs
371 parametersAbsolute structure parameter: 0.02 (2)
0 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
Cr10.15520 (4)0.31365 (3)0.89842 (2)0.04051 (13)
P10.30442 (8)0.12244 (6)0.79891 (4)0.0441 (2)
P20.07943 (9)0.03049 (6)0.83940 (4)0.0511 (2)
C10.1711 (3)0.2012 (2)0.82331 (12)0.0376 (6)
C250.1262 (4)0.0865 (3)0.62873 (17)0.0614 (9)
H250.04090.09110.61190.080*
C20.1511 (3)0.2944 (2)0.79614 (13)0.0435 (7)
H20.21030.31880.76460.057*
C80.1061 (3)0.0665 (2)0.90104 (14)0.0464 (7)
H80.19540.06370.91170.060*
C260.1499 (3)0.1107 (2)0.69062 (14)0.0493 (7)
H260.08060.13210.71760.064*
C50.0173 (3)0.2257 (2)0.88608 (14)0.0437 (7)
H50.07850.20140.91670.057*
C90.1608 (4)0.1377 (2)0.87144 (16)0.0580 (8)
C270.4352 (3)0.2095 (2)0.79696 (15)0.0501 (8)
C210.2687 (3)0.1054 (2)0.71520 (14)0.0462 (7)
C60.0847 (3)0.1667 (2)0.87004 (12)0.0393 (6)
C340.2883 (3)0.3990 (3)0.8868 (2)0.0646 (10)
C40.0338 (3)0.3192 (2)0.85912 (14)0.0474 (7)
H40.10380.36080.87280.062*
O20.3692 (3)0.4521 (2)0.8792 (2)0.1073 (12)
O30.3038 (3)0.2077 (2)0.99631 (14)0.0919 (10)
C320.4675 (3)0.2694 (3)0.74669 (19)0.0644 (10)
H320.41480.26960.70890.084*
C150.0860 (4)0.0570 (3)0.85191 (17)0.0610 (9)
C300.6473 (4)0.3297 (4)0.8006 (3)0.0940 (15)
H300.72200.37180.80170.122*
O10.0586 (3)0.4493 (3)0.99766 (16)0.1090 (12)
C200.1687 (5)0.0038 (3)0.8204 (2)0.0838 (13)
H200.13620.05410.79160.109*
C140.1412 (4)0.2279 (3)0.8424 (2)0.0832 (13)
H140.07830.23330.80900.108*
C280.5121 (3)0.2105 (3)0.84998 (18)0.0661 (10)
H280.49230.16860.88620.086*
C230.3410 (4)0.0515 (4)0.61445 (18)0.0832 (13)
H230.40990.03070.58700.108*
C160.1340 (4)0.1299 (4)0.8918 (2)0.0846 (12)
H160.07670.17520.91340.110*
C220.3658 (4)0.0757 (3)0.67595 (18)0.0704 (11)
H220.45160.07200.69210.092*
C120.2976 (6)0.3040 (4)0.9058 (3)0.1051 (16)
H120.34260.36320.91940.137*
C240.2225 (4)0.0560 (3)0.59094 (17)0.0716 (11)
H240.20620.03740.54710.093*
C170.2613 (5)0.1383 (5)0.9009 (3)0.1145 (19)
H170.29440.18880.92940.149*
C110.3237 (6)0.2154 (4)0.9330 (3)0.1120 (19)
H110.39020.21020.96460.146*
C130.2094 (5)0.3109 (4)0.8598 (3)0.1065 (17)
H130.19390.37420.83900.138*
C70.0346 (4)0.0511 (3)0.96275 (15)0.0653 (10)
H7A0.05930.10200.99310.085*
H7B0.05440.01420.97990.085*
H7C0.05560.05570.95480.085*
C310.5720 (4)0.3288 (4)0.7486 (2)0.0834 (13)
H310.59260.37070.71250.108*
C290.6176 (4)0.2714 (4)0.8511 (2)0.0888 (15)
H290.67120.27250.88860.115*
C330.0964 (4)0.3977 (3)0.96015 (18)0.0653 (10)
C100.2559 (5)0.1326 (3)0.9158 (2)0.0876 (14)
H100.27560.06900.93540.114*
C180.3410 (5)0.0767 (6)0.8702 (4)0.125 (3)
H180.43130.08270.87740.162*
C190.2968 (6)0.0051 (5)0.8288 (3)0.119 (2)
H190.35510.03800.80610.154*
C30.0483 (3)0.3535 (2)0.81309 (14)0.0483 (8)
H30.03460.41760.79290.063*
C350.2468 (4)0.2495 (3)0.95873 (16)0.0577 (9)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cr10.0371 (2)0.0421 (2)0.0423 (2)0.0015 (2)0.0030 (2)0.0088 (2)
P10.0438 (4)0.0480 (4)0.0405 (4)0.0112 (3)0.0011 (3)0.0023 (3)
P20.0664 (6)0.0450 (4)0.0421 (4)0.0007 (4)0.0013 (4)0.0019 (4)
C10.0376 (15)0.0421 (15)0.0331 (13)0.0012 (13)0.0025 (11)0.0025 (12)
C250.069 (2)0.064 (2)0.051 (2)0.0041 (18)0.0057 (17)0.0020 (16)
C20.0442 (16)0.0469 (17)0.0393 (15)0.0028 (14)0.0010 (14)0.0003 (12)
C80.0576 (18)0.0445 (15)0.0371 (15)0.0014 (14)0.0002 (15)0.0035 (13)
C260.0521 (18)0.0531 (17)0.0427 (16)0.0064 (16)0.0030 (15)0.0043 (14)
C50.0356 (15)0.0535 (17)0.0421 (17)0.0052 (13)0.0013 (13)0.0094 (13)
C90.065 (2)0.0508 (19)0.058 (2)0.0013 (18)0.0099 (19)0.0009 (15)
C270.0391 (16)0.061 (2)0.0501 (17)0.0131 (15)0.0001 (14)0.0101 (15)
C210.0530 (19)0.0452 (17)0.0405 (16)0.0036 (14)0.0056 (14)0.0037 (13)
C60.0434 (16)0.0427 (16)0.0319 (13)0.0010 (13)0.0057 (13)0.0056 (11)
C340.053 (2)0.056 (2)0.086 (3)0.0014 (17)0.003 (2)0.0134 (19)
C40.0364 (15)0.0546 (18)0.0510 (17)0.0116 (15)0.0071 (13)0.0130 (15)
O20.0719 (19)0.076 (2)0.174 (4)0.0332 (17)0.018 (2)0.019 (2)
O30.099 (2)0.098 (2)0.0788 (18)0.0108 (19)0.0464 (17)0.0023 (17)
C320.045 (2)0.078 (2)0.069 (2)0.0001 (18)0.0003 (17)0.0061 (19)
C150.067 (2)0.061 (2)0.056 (2)0.0007 (19)0.0036 (18)0.0199 (17)
C300.051 (2)0.105 (4)0.126 (4)0.008 (3)0.012 (3)0.005 (3)
O10.112 (3)0.120 (3)0.095 (2)0.016 (2)0.003 (2)0.064 (2)
C200.083 (3)0.076 (3)0.092 (3)0.019 (2)0.019 (3)0.031 (2)
C140.072 (3)0.054 (2)0.124 (4)0.000 (2)0.010 (3)0.011 (2)
C280.049 (2)0.085 (3)0.065 (2)0.0112 (19)0.0091 (17)0.005 (2)
C230.083 (3)0.117 (4)0.050 (2)0.018 (3)0.016 (2)0.021 (2)
C160.071 (3)0.086 (3)0.096 (3)0.010 (2)0.012 (3)0.006 (3)
C220.056 (2)0.096 (3)0.059 (2)0.018 (2)0.0088 (18)0.014 (2)
C120.111 (4)0.068 (3)0.136 (5)0.032 (3)0.005 (4)0.012 (3)
C240.096 (3)0.080 (3)0.0380 (18)0.004 (2)0.002 (2)0.0108 (18)
C170.078 (3)0.124 (4)0.141 (5)0.028 (3)0.023 (4)0.032 (4)
C110.148 (5)0.086 (4)0.102 (4)0.044 (4)0.027 (4)0.007 (3)
C130.090 (3)0.057 (3)0.172 (5)0.008 (3)0.007 (4)0.017 (3)
C70.100 (3)0.059 (2)0.0369 (17)0.003 (2)0.0060 (18)0.0014 (15)
C310.051 (2)0.100 (3)0.100 (3)0.008 (2)0.005 (2)0.015 (3)
C290.052 (2)0.119 (4)0.095 (3)0.000 (2)0.026 (2)0.012 (3)
C330.066 (2)0.072 (2)0.058 (2)0.006 (2)0.0049 (19)0.0311 (19)
C100.121 (4)0.067 (3)0.074 (3)0.028 (3)0.020 (3)0.009 (2)
C180.061 (3)0.152 (6)0.161 (6)0.004 (4)0.003 (4)0.084 (5)
C190.085 (4)0.110 (4)0.162 (6)0.035 (3)0.040 (4)0.069 (4)
C30.0536 (19)0.0444 (17)0.0469 (17)0.0082 (15)0.0062 (15)0.0026 (13)
C350.062 (2)0.062 (2)0.050 (2)0.0039 (18)0.0149 (18)0.0099 (16)
Geometric parameters (Å, º) top
Cr1—C351.832 (4)C32—C311.376 (5)
Cr1—C331.847 (3)C32—H320.9800
Cr1—C341.849 (4)C15—C201.381 (6)
Cr1—C42.186 (3)C15—C161.399 (6)
Cr1—C22.190 (3)C30—C311.366 (6)
Cr1—C32.210 (3)C30—C291.371 (7)
Cr1—C52.209 (3)C30—H300.9800
Cr1—C12.214 (3)O1—C331.135 (4)
Cr1—C62.213 (3)C20—C191.384 (8)
P1—C271.828 (4)C20—H200.9800
P1—C211.834 (3)C14—C131.389 (7)
P1—C11.854 (3)C14—H140.9800
P2—C151.822 (4)C28—C291.397 (6)
P2—C91.825 (4)C28—H280.9800
P2—C81.878 (3)C23—C241.362 (6)
C1—C21.405 (4)C23—C221.373 (5)
C1—C61.434 (4)C23—H230.9800
C25—C241.369 (5)C16—C171.377 (6)
C25—C261.379 (5)C16—H160.9800
C25—H250.9800C22—H220.9800
C2—C31.406 (4)C12—C131.360 (7)
C2—H20.9800C12—C111.362 (7)
C8—C61.526 (4)C12—H120.9800
C8—C71.532 (4)C24—H240.9800
C8—H80.9800C17—C181.359 (9)
C26—C211.374 (5)C17—H170.9800
C26—H260.9800C11—C101.383 (6)
C5—C61.392 (4)C11—H110.9800
C5—C41.402 (4)C13—H130.9800
C5—H50.9800C7—H7A0.9801
C9—C141.386 (5)C7—H7B0.9801
C9—C101.387 (6)C7—H7C0.9801
C27—C321.386 (5)C31—H310.9800
C27—C281.395 (5)C29—H290.9800
C21—C221.390 (5)C10—H100.9800
C34—O21.136 (4)C18—C191.392 (9)
C4—C31.394 (4)C18—H180.9800
C4—H40.9800C19—H190.9800
O3—C351.153 (4)C3—H30.9800
C35—Cr1—C3388.68 (17)C1—C6—C8119.5 (3)
C35—Cr1—C3488.86 (17)C5—C6—Cr171.50 (16)
C33—Cr1—C3488.32 (17)C1—C6—Cr171.12 (15)
C35—Cr1—C4140.98 (15)C8—C6—Cr1129.18 (19)
C33—Cr1—C486.34 (14)O2—C34—Cr1179.2 (4)
C34—Cr1—C4129.57 (16)C3—C4—C5120.6 (3)
C35—Cr1—C2130.44 (14)C3—C4—Cr172.47 (18)
C33—Cr1—C2140.52 (15)C5—C4—Cr172.31 (17)
C34—Cr1—C287.56 (15)C3—C4—H4119.7
C4—Cr1—C266.81 (11)C5—C4—H4119.7
C35—Cr1—C3165.03 (13)Cr1—C4—H4127.6
C33—Cr1—C3104.87 (15)C31—C32—C27121.4 (4)
C34—Cr1—C397.71 (16)C31—C32—H32119.3
C4—Cr1—C336.97 (12)C27—C32—H32119.3
C2—Cr1—C337.27 (11)C20—C15—C16118.8 (4)
C35—Cr1—C5105.78 (14)C20—C15—P2115.6 (3)
C33—Cr1—C597.68 (15)C16—C15—P2125.6 (3)
C34—Cr1—C5164.22 (15)C31—C30—C29119.5 (4)
C4—Cr1—C537.21 (12)C31—C30—H30120.3
C2—Cr1—C578.52 (11)C29—C30—H30120.3
C3—Cr1—C566.67 (12)C15—C20—C19121.1 (5)
C35—Cr1—C197.88 (13)C15—C20—H20119.4
C33—Cr1—C1164.28 (15)C19—C20—H20119.4
C34—Cr1—C1106.00 (14)C9—C14—C13121.1 (5)
C4—Cr1—C179.55 (11)C9—C14—H14119.5
C2—Cr1—C137.20 (10)C13—C14—H14119.5
C3—Cr1—C167.41 (11)C27—C28—C29119.6 (4)
C5—Cr1—C166.83 (10)C27—C28—H28120.2
C35—Cr1—C686.87 (13)C29—C28—H28120.2
C33—Cr1—C6129.24 (15)C24—C23—C22121.2 (4)
C34—Cr1—C6142.02 (14)C24—C23—H23119.4
C4—Cr1—C667.20 (11)C22—C23—H23119.4
C2—Cr1—C667.37 (11)C17—C16—C15120.3 (5)
C3—Cr1—C679.66 (11)C17—C16—H16119.9
C5—Cr1—C636.70 (10)C15—C16—H16119.9
C1—Cr1—C637.80 (10)C23—C22—C21119.8 (4)
C27—P1—C21102.60 (15)C23—C22—H22120.1
C27—P1—C1102.77 (13)C21—C22—H22120.1
C21—P1—C1100.63 (13)C13—C12—C11120.4 (5)
C15—P2—C9104.50 (18)C13—C12—H12119.8
C15—P2—C8100.55 (15)C11—C12—H12119.8
C9—P2—C8102.99 (15)C23—C24—C25119.7 (3)
C2—C1—C6118.7 (3)C23—C24—H24120.1
C2—C1—P1121.3 (2)C25—C24—H24120.1
C6—C1—P1120.0 (2)C18—C17—C16120.0 (6)
C2—C1—Cr170.49 (16)C18—C17—H17120.0
C6—C1—Cr171.08 (15)C16—C17—H17120.0
P1—C1—Cr1131.08 (14)C12—C11—C10119.7 (5)
C24—C25—C26119.6 (4)C12—C11—H11120.1
C24—C25—H25120.2C10—C11—H11120.1
C26—C25—H25120.2C12—C13—C14119.9 (5)
C1—C2—C3121.7 (3)C12—C13—H13120.0
C1—C2—Cr172.31 (16)C14—C13—H13120.0
C3—C2—Cr172.14 (17)C8—C7—H7A109.5
C1—C2—H2119.1C8—C7—H7B109.5
C3—C2—H2119.1H7A—C7—H7B109.5
Cr1—C2—H2128.8C8—C7—H7C109.5
C6—C8—C7114.6 (3)H7A—C7—H7C109.5
C6—C8—P2107.39 (19)H7B—C7—H7C109.5
C7—C8—P2115.2 (2)C30—C31—C32120.5 (4)
C6—C8—H8106.3C30—C31—H31119.8
C7—C8—H8106.3C32—C31—H31119.8
P2—C8—H8106.3C30—C29—C28120.9 (4)
C21—C26—C25121.3 (3)C30—C29—H29119.5
C21—C26—H26119.3C28—C29—H29119.5
C25—C26—H26119.3O1—C33—Cr1179.0 (4)
C6—C5—C4121.2 (3)C11—C10—C9121.5 (4)
C6—C5—Cr171.80 (16)C11—C10—H10119.3
C4—C5—Cr170.47 (17)C9—C10—H10119.3
C6—C5—H5119.4C17—C18—C19121.3 (6)
C4—C5—H5119.4C17—C18—H18119.3
Cr1—C5—H5131.2C19—C18—H18119.3
C14—C9—C10117.2 (4)C20—C19—C18118.5 (6)
C14—C9—P2117.7 (3)C20—C19—H19120.8
C10—C9—P2124.3 (3)C18—C19—H19120.8
C32—C27—C28118.1 (3)C4—C3—C2118.7 (3)
C32—C27—P1125.9 (3)C4—C3—Cr170.57 (17)
C28—C27—P1115.9 (3)C2—C3—Cr170.60 (17)
C26—C21—C22118.4 (3)C4—C3—H3120.6
C26—C21—P1123.7 (2)C2—C3—H3120.6
C22—C21—P1117.6 (3)Cr1—C3—H3130.7
C5—C6—C1119.0 (3)O3—C35—Cr1178.9 (3)
C5—C6—C8121.5 (3)
C27—P1—C1—C245.1 (3)C1—P1—C27—C3285.6 (3)
C21—P1—C1—C260.6 (3)C21—P1—C27—C28157.7 (3)
C27—P1—C1—C6135.9 (2)C1—P1—C27—C2898.1 (3)
C21—P1—C1—C6118.4 (2)C25—C26—C21—C220.6 (5)
C27—P1—C1—Cr145.5 (2)C25—C26—C21—P1172.7 (3)
C21—P1—C1—Cr1151.21 (19)C27—P1—C21—C26131.8 (3)
C35—Cr1—C1—C2154.3 (2)C1—P1—C21—C2626.0 (3)
C33—Cr1—C1—C291.8 (6)C27—P1—C21—C2254.9 (3)
C34—Cr1—C1—C263.2 (2)C1—P1—C21—C22160.7 (3)
C4—Cr1—C1—C265.20 (19)C4—C5—C6—C12.4 (4)
C5—Cr1—C1—C2101.88 (19)Cr1—C5—C6—C154.8 (2)
C3—Cr1—C1—C228.65 (18)C4—C5—C6—C8177.6 (3)
C6—Cr1—C1—C2131.3 (2)Cr1—C5—C6—C8125.2 (3)
C35—Cr1—C1—C674.4 (2)C4—C5—C6—Cr152.4 (2)
C33—Cr1—C1—C639.5 (6)C2—C1—C6—C51.2 (4)
C34—Cr1—C1—C6165.51 (19)P1—C1—C6—C5177.8 (2)
C4—Cr1—C1—C666.10 (17)Cr1—C1—C6—C555.0 (2)
C2—Cr1—C1—C6131.3 (2)C2—C1—C6—C8178.8 (2)
C5—Cr1—C1—C629.42 (16)P1—C1—C6—C82.2 (3)
C3—Cr1—C1—C6102.66 (18)Cr1—C1—C6—C8125.0 (2)
C35—Cr1—C1—P139.3 (2)C2—C1—C6—Cr153.8 (2)
C33—Cr1—C1—P1153.3 (5)P1—C1—C6—Cr1127.17 (19)
C34—Cr1—C1—P151.8 (2)C7—C8—C6—C517.9 (4)
C4—Cr1—C1—P1179.8 (2)P2—C8—C6—C5111.5 (3)
C2—Cr1—C1—P1115.0 (3)C7—C8—C6—C1162.1 (3)
C5—Cr1—C1—P1143.2 (2)P2—C8—C6—C168.5 (3)
C3—Cr1—C1—P1143.6 (2)C7—C8—C6—Cr173.2 (4)
C6—Cr1—C1—P1113.7 (3)P2—C8—C6—Cr1157.43 (17)
C6—C1—C2—C30.8 (4)C6—C5—C4—C33.2 (4)
P1—C1—C2—C3178.2 (2)Cr1—C5—C4—C356.2 (3)
Cr1—C1—C2—C354.9 (3)C6—C5—C4—Cr153.0 (2)
C6—C1—C2—Cr154.1 (2)C28—C27—C32—C310.3 (5)
P1—C1—C2—Cr1126.90 (19)P1—C27—C32—C31176.4 (3)
C35—Cr1—C2—C134.4 (3)C9—P2—C15—C20167.4 (3)
C33—Cr1—C2—C1154.8 (2)C8—P2—C15—C2086.0 (3)
C34—Cr1—C2—C1120.8 (2)C9—P2—C15—C1615.0 (4)
C4—Cr1—C2—C1103.8 (2)C8—P2—C15—C1691.5 (4)
C5—Cr1—C2—C166.63 (18)C16—C15—C20—C191.4 (6)
C3—Cr1—C2—C1133.0 (3)P2—C15—C20—C19176.3 (4)
C6—Cr1—C2—C129.92 (16)C10—C9—C14—C133.7 (7)
C35—Cr1—C2—C3167.4 (2)P2—C9—C14—C13173.4 (4)
C33—Cr1—C2—C321.8 (3)C32—C27—C28—C290.4 (5)
C34—Cr1—C2—C3106.1 (2)P1—C27—C28—C29176.9 (3)
C4—Cr1—C2—C329.25 (19)C20—C15—C16—C172.1 (7)
C5—Cr1—C2—C366.40 (19)P2—C15—C16—C17175.3 (4)
C6—Cr1—C2—C3103.1 (2)C24—C23—C22—C210.1 (7)
C1—Cr1—C2—C3133.0 (3)C26—C21—C22—C230.7 (6)
C15—P2—C8—C692.3 (2)P1—C21—C22—C23172.9 (4)
C9—P2—C8—C6160.0 (2)C22—C23—C24—C251.0 (7)
C15—P2—C8—C736.7 (3)C26—C25—C24—C231.2 (6)
C9—P2—C8—C771.0 (3)C15—C16—C17—C181.0 (8)
C24—C25—C26—C210.4 (6)C13—C12—C11—C103.0 (9)
C35—Cr1—C5—C661.7 (2)C11—C12—C13—C143.0 (9)
C33—Cr1—C5—C6152.5 (2)C9—C14—C13—C120.5 (8)
C34—Cr1—C5—C695.9 (5)C29—C30—C31—C320.4 (7)
C4—Cr1—C5—C6134.0 (3)C27—C32—C31—C300.2 (7)
C2—Cr1—C5—C667.38 (17)C31—C30—C29—C280.6 (8)
C3—Cr1—C5—C6104.55 (19)C27—C28—C29—C300.6 (6)
C1—Cr1—C5—C630.25 (16)C12—C11—C10—C90.4 (9)
C35—Cr1—C5—C4164.31 (19)C14—C9—C10—C113.6 (7)
C33—Cr1—C5—C473.5 (2)P2—C9—C10—C11172.5 (4)
C34—Cr1—C5—C438.1 (5)C16—C17—C18—C190.8 (9)
C2—Cr1—C5—C466.61 (18)C15—C20—C19—C180.3 (8)
C3—Cr1—C5—C429.43 (17)C17—C18—C19—C201.5 (9)
C6—Cr1—C5—C4134.0 (3)C5—C4—C3—C22.7 (4)
C1—Cr1—C5—C4103.74 (18)Cr1—C4—C3—C253.5 (3)
C15—P2—C9—C1464.3 (4)C5—C4—C3—Cr156.2 (2)
C8—P2—C9—C14169.0 (3)C1—C2—C3—C41.5 (4)
C15—P2—C9—C10126.8 (4)Cr1—C2—C3—C453.5 (3)
C8—P2—C9—C1022.1 (4)C1—C2—C3—Cr154.9 (3)
C21—P1—C27—C3218.5 (3)
(II) (R,R)-tricarbonyl-1κ3C-{µ-1(η6):2κ2P,P'-1-(diphenylphosphino)-2-[1- (diphenylphosphino)ethyl]benzene}[2(η4)-norbornadiene]chromium(0)rhodium(I) tetrafluoroborate methanol 0.75-solvate top
Crystal data top
[CrRh(C7H8)(C32H28P2)(CO)3]·BF4·0.75CH4ODx = 1.546 Mg m3
Mr = 916.40Mo Kα radiation, λ = 0.71073 Å
Tetragonal, P43212Cell parameters from 8096 reflections
Hall symbol: P 4nw 2abwθ = 1.5–25.0°
a = 14.3886 (6) ŵ = 0.84 mm1
c = 76.056 (4) ÅT = 110 K
V = 15746.0 (13) Å3Fragment, red
Z = 160.16 × 0.10 × 0.10 mm
F(000) = 7448
Data collection top
Bruker SMART APEX CCD
diffractometer
13552 independent reflections
Radiation source: fine-focus sealed tube9225 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.105
Detector resolution: 0 pixels mm-1θmax = 25.0°, θmin = 1.5°
ϕ and ω scansh = 1716
Absorption correction: multi-scan
(SADABS; Sheldrick; 1996)
k = 1617
Tmin = 0.878, Tmax = 0.921l = 8570
72654 measured reflections
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)] = 0.071H-atom parameters constrained
wR(F2) = 0.174Calculated w = 1/[σ2(Fo2) + (0.0804P)2 + 29.8752P]
where P = (Fo2 + 2Fc2)/3
S = 1.02(Δ/σ)max = 0.001
13552 reflectionsΔρmax = 1.77 e Å3
983 parametersΔρmin = 0.90 e Å3
9 restraintsAbsolute structure: Flack (1983), 5780 Friedel pairs
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.01 (4)
Crystal data top
[CrRh(C7H8)(C32H28P2)(CO)3]·BF4·0.75CH4OZ = 16
Mr = 916.40Mo Kα radiation
Tetragonal, P43212µ = 0.84 mm1
a = 14.3886 (6) ÅT = 110 K
c = 76.056 (4) Å0.16 × 0.10 × 0.10 mm
V = 15746.0 (13) Å3
Data collection top
Bruker SMART APEX CCD
diffractometer
13552 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick; 1996)
9225 reflections with I > 2σ(I)
Tmin = 0.878, Tmax = 0.921Rint = 0.105
72654 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.071H-atom parameters constrained
wR(F2) = 0.174Δρmax = 1.77 e Å3
S = 1.02Δρmin = 0.90 e Å3
13552 reflectionsAbsolute structure: Flack (1983), 5780 Friedel pairs
983 parametersAbsolute structure parameter: 0.01 (4)
9 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*/UeqOcc. (<1)
Rh10.22302 (6)0.77146 (6)0.011497 (10)0.0312 (2)
Cr10.51228 (12)0.76647 (12)0.03666 (2)0.0329 (4)
P10.2699 (2)0.76309 (18)0.01705 (4)0.0320 (7)
P20.3574 (2)0.84285 (19)0.01953 (3)0.0301 (7)
O10.4793 (5)0.9689 (5)0.04294 (10)0.0438 (19)
O20.6970 (6)0.7915 (6)0.05386 (10)0.053 (2)
O30.4427 (5)0.7224 (6)0.07218 (10)0.048 (2)
C10.3953 (8)0.7375 (7)0.01877 (13)0.035 (3)
C20.4911 (7)0.8895 (8)0.04061 (13)0.033 (3)
C30.6271 (8)0.7826 (8)0.04724 (13)0.038 (3)
C40.4691 (7)0.7387 (8)0.05834 (15)0.035 (3)
C50.4614 (8)0.7890 (7)0.00914 (14)0.035 (3)
C60.5543 (8)0.7590 (8)0.00845 (14)0.043 (3)
H60.59810.79310.00220.051*
C70.5812 (9)0.6766 (9)0.01733 (13)0.051 (4)
H70.64350.65920.01720.062*
C80.5162 (9)0.6197 (8)0.02642 (15)0.047 (3)
H80.53310.56320.03140.056*
C90.4276 (8)0.6529 (7)0.02732 (13)0.037 (3)
H90.38470.61920.03390.045*
C100.4325 (7)0.8756 (6)0.00077 (13)0.028 (2)
H100.39300.91100.00730.034*
C110.4293 (8)0.7777 (7)0.03467 (13)0.037 (3)
C120.4081 (7)0.6844 (7)0.03731 (14)0.038 (3)
H120.36300.65550.03050.046*
C130.4557 (9)0.6340 (8)0.05045 (14)0.049 (4)
H130.44080.57210.05260.058*
C140.5244 (9)0.6772 (10)0.06001 (15)0.050 (3)
H140.55650.64390.06850.060*
C150.5462 (8)0.7685 (9)0.05715 (14)0.045 (3)
H150.59310.79690.06360.054*
C160.4973 (7)0.8190 (7)0.04439 (13)0.035 (3)
H160.51130.88130.04250.042*
C170.3307 (7)0.9495 (7)0.03106 (13)0.028 (2)
C180.3075 (7)1.0289 (8)0.02219 (15)0.038 (3)
H180.31191.03100.01000.046*
C190.2767 (8)1.1073 (8)0.03162 (19)0.052 (3)
H190.26051.16080.02550.062*
C200.2702 (7)1.1068 (8)0.04960 (17)0.044 (3)
H200.25171.15950.05580.053*
C210.2915 (7)1.0271 (8)0.05805 (16)0.044 (3)
H210.28611.02490.07020.053*
C220.3204 (8)0.9501 (7)0.04937 (14)0.038 (3)
H220.33380.89650.05570.046*
C230.5147 (7)0.9412 (7)0.00569 (13)0.039 (3)
H23A0.54900.95680.00470.059*
H23B0.49080.99690.01100.059*
H23C0.55510.91030.01390.059*
C240.2085 (7)0.6714 (7)0.02848 (13)0.031 (3)
C250.1374 (7)0.6911 (7)0.04038 (13)0.035 (3)
H250.12470.75260.04330.042*
C260.0857 (7)0.6213 (8)0.04794 (14)0.037 (3)
H260.03720.63520.05560.045*
C270.1075 (8)0.5295 (8)0.04391 (14)0.038 (3)
H270.07560.48190.04960.046*
C280.1740 (8)0.5073 (8)0.03192 (14)0.042 (3)
H280.18670.44580.02910.050*
C290.2212 (8)0.5784 (7)0.02427 (13)0.036 (3)
H290.26470.56380.01570.043*
C300.2513 (6)0.8678 (6)0.02980 (12)0.024 (2)
C310.2152 (7)0.9449 (6)0.02187 (13)0.029 (2)
H310.19810.94240.01010.035*
C320.2040 (8)1.0251 (7)0.03103 (14)0.038 (3)
H320.18051.07760.02540.045*
C330.2273 (8)1.0294 (7)0.04867 (16)0.046 (3)
H330.21941.08430.05490.055*
C340.2622 (8)0.9519 (8)0.05686 (15)0.041 (3)
H340.27870.95490.06870.050*
C350.2728 (7)0.8709 (7)0.04798 (13)0.032 (3)
H350.29400.81800.05370.039*
C360.1088 (8)0.6688 (7)0.01081 (14)0.043 (3)
H360.13440.62640.00300.051*
C370.0715 (7)0.7562 (7)0.00705 (13)0.036 (3)
H370.06710.78270.00410.043*
C380.0398 (7)0.8003 (8)0.02382 (14)0.041 (3)
H380.00410.85220.02310.049*
C390.1321 (7)0.8158 (8)0.03350 (14)0.038 (3)
H390.15930.87300.03590.046*
C400.1674 (8)0.7306 (8)0.03790 (13)0.043 (3)
H400.22270.71880.04380.052*
C410.0976 (8)0.6583 (8)0.03116 (13)0.041 (3)
H410.10080.59560.03610.049*
C420.0097 (9)0.7123 (8)0.03376 (15)0.049 (3)
H42A0.04350.68230.02830.058*
H42B0.00310.72440.04610.058*
Rh20.42814 (5)0.49305 (6)0.123562 (10)0.02484 (19)
Cr20.06623 (11)0.46824 (11)0.15045 (2)0.0277 (4)
P30.33396 (17)0.45689 (17)0.14681 (3)0.0230 (6)
P40.30543 (18)0.50008 (19)0.10521 (3)0.0271 (6)
O40.0519 (5)0.3640 (6)0.18448 (9)0.048 (2)
O50.0615 (5)0.2764 (5)0.13521 (9)0.0427 (19)
O60.1422 (5)0.4641 (6)0.15098 (10)0.049 (2)
C430.2170 (6)0.5060 (6)0.14572 (12)0.023 (2)
C440.0594 (7)0.4082 (8)0.17194 (15)0.039 (3)
C450.0635 (7)0.3524 (7)0.14077 (13)0.030 (3)
C460.0627 (8)0.4673 (8)0.15027 (14)0.039 (3)
C470.1637 (6)0.5064 (7)0.12944 (12)0.024 (2)
C480.0854 (7)0.5624 (7)0.12775 (13)0.033 (3)
H480.05380.56450.11710.040*
C490.0528 (7)0.6169 (7)0.14231 (15)0.035 (3)
H490.00050.65430.14120.042*
C500.1003 (7)0.6128 (7)0.15798 (15)0.037 (3)
H500.07810.64680.16750.045*
C510.1816 (7)0.5588 (7)0.16022 (14)0.030 (3)
H510.21190.55750.17100.036*
C520.1957 (6)0.4480 (7)0.11375 (13)0.029 (2)
H520.21270.38710.11850.035*
C530.2740 (7)0.6195 (6)0.10023 (12)0.025 (2)
C540.2120 (7)0.6455 (7)0.08720 (13)0.033 (3)
H540.18740.60140.07960.040*
C550.1874 (7)0.7379 (7)0.08569 (12)0.034 (3)
H550.14330.75490.07740.041*
C560.2265 (7)0.8060 (7)0.09628 (13)0.033 (3)
H560.21080.86820.09480.040*
C570.2897 (7)0.7797 (8)0.10918 (13)0.034 (3)
H570.31570.82430.11660.040*
C580.3137 (6)0.6883 (7)0.11102 (13)0.028 (2)
H580.35680.67130.11950.034*
C590.3280 (6)0.4360 (7)0.08522 (13)0.027 (2)
C600.3441 (6)0.4759 (7)0.06964 (12)0.027 (2)
H600.33880.54000.06850.032*
C610.3688 (7)0.4225 (9)0.05491 (14)0.044 (3)
H610.37840.45140.04410.053*
C620.3789 (8)0.3274 (8)0.05633 (15)0.043 (3)
H620.39690.29160.04670.052*
C630.3615 (7)0.2872 (8)0.07252 (15)0.044 (3)
H630.36830.22330.07380.053*
C640.3343 (7)0.3398 (8)0.08681 (13)0.035 (3)
H640.32010.31110.09740.042*
C650.1205 (6)0.4300 (8)0.10033 (12)0.033 (3)
H65A0.06600.40690.10610.050*
H65B0.14190.38490.09200.050*
H65C0.10580.48690.09430.050*
C660.3229 (6)0.3339 (7)0.14996 (12)0.023 (2)
C670.2667 (7)0.2948 (6)0.16357 (13)0.027 (2)
H670.23190.33370.17080.033*
C680.2635 (7)0.2004 (7)0.16607 (13)0.033 (3)
H680.22700.17580.17500.040*
C690.3148 (8)0.1407 (7)0.15523 (14)0.037 (3)
H690.31290.07690.15710.045*
C700.3683 (7)0.1767 (8)0.14175 (15)0.040 (3)
H700.40120.13710.13440.048*
C710.3727 (6)0.2717 (8)0.13931 (13)0.031 (3)
H710.40980.29520.13030.037*
C720.3833 (6)0.5012 (7)0.16723 (11)0.019 (2)
C730.3902 (7)0.5979 (7)0.16946 (13)0.030 (2)
H730.36200.63820.16150.036*
C740.4390 (8)0.6320 (7)0.18349 (13)0.036 (3)
H740.44170.69590.18520.043*
C750.4835 (7)0.5748 (8)0.19489 (13)0.038 (3)
H750.51700.60040.20420.045*
C760.4803 (7)0.4804 (7)0.19304 (12)0.035 (3)
H760.51140.44180.20090.041*
C770.4281 (7)0.4421 (7)0.17870 (12)0.028 (2)
H770.42450.37810.17720.033*
C780.5664 (6)0.4583 (7)0.13535 (13)0.028 (2)
H780.55070.41200.14330.033*
C790.5507 (6)0.5506 (7)0.13715 (12)0.027 (2)
H790.52080.58010.14640.032*
C800.5930 (7)0.5975 (7)0.12052 (13)0.028 (2)
H800.60610.66430.12120.034*
C810.5270 (7)0.5640 (7)0.10572 (14)0.036 (3)
H810.48680.60070.09910.044*
C820.5393 (7)0.4693 (7)0.10423 (13)0.031 (2)
H820.50790.42890.09680.037*
C830.6155 (7)0.4449 (7)0.11742 (12)0.030 (3)
H830.64720.38540.11560.036*
C840.6762 (6)0.5314 (6)0.11693 (13)0.026 (2)
H84A0.70500.54170.10560.031*
H84B0.72260.53260.12620.031*
F10.9524 (4)0.7206 (4)0.10757 (8)0.0453 (16)
F20.8952 (4)0.5737 (4)0.10725 (8)0.0449 (16)
F30.8214 (5)0.6883 (4)0.09244 (9)0.0568 (19)
F40.9599 (5)0.6339 (6)0.08279 (10)0.081 (3)
B10.9061 (8)0.6548 (9)0.09729 (17)0.034 (3)
F50.5025 (8)0.4115 (9)0.00851 (18)0.171 (5)
F60.3540 (8)0.4113 (8)0.01204 (11)0.126 (4)
B20.4178 (14)0.4178 (14)0.00000.076 (8)
F71.0039 (4)0.0890 (4)0.00967 (8)0.0509 (17)
F81.0036 (4)0.0688 (4)0.01143 (8)0.0503 (16)
B31.0074 (9)0.0074 (9)0.00000.050 (5)
C850.8702 (17)0.7547 (17)0.0273 (4)0.173 (5)*0.50
H85A0.93570.73790.02890.173 (5)*0.50
H85B0.83080.70790.03300.173 (5)*0.50
H85C0.85860.81560.03270.173 (5)*0.50
O70.8492 (17)0.7586 (17)0.0089 (4)0.173 (5)*0.50
H7A0.78330.76210.00850.173 (5)*0.50
C860.4127 (10)0.1636 (9)0.01799 (15)0.173 (5)*
H86A0.46120.21140.01780.173 (5)*
H86B0.42850.11390.00970.173 (5)*
H86C0.40780.13770.02990.173 (5)*
O80.3256 (10)0.2040 (9)0.01308 (15)0.173 (5)*
H8A0.33340.26960.01270.173 (5)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Rh10.0445 (5)0.0321 (5)0.0168 (4)0.0059 (4)0.0027 (4)0.0013 (4)
Cr10.0399 (10)0.0397 (10)0.0192 (10)0.0047 (8)0.0012 (8)0.0016 (8)
P10.0456 (16)0.0263 (14)0.0240 (16)0.0029 (13)0.0007 (13)0.0015 (12)
P20.0445 (17)0.0299 (15)0.0161 (16)0.0008 (13)0.0043 (13)0.0007 (12)
O10.044 (5)0.046 (5)0.041 (5)0.005 (4)0.009 (4)0.001 (4)
O20.051 (5)0.071 (6)0.038 (5)0.010 (4)0.005 (4)0.010 (4)
O30.051 (5)0.061 (5)0.033 (5)0.011 (4)0.002 (4)0.011 (4)
C10.055 (7)0.022 (6)0.027 (6)0.021 (5)0.011 (5)0.003 (5)
C20.036 (6)0.041 (7)0.021 (6)0.002 (5)0.007 (5)0.001 (5)
C30.040 (7)0.057 (8)0.016 (6)0.011 (6)0.012 (5)0.002 (5)
C40.037 (6)0.044 (7)0.025 (7)0.005 (5)0.000 (5)0.001 (5)
C50.052 (7)0.032 (6)0.021 (6)0.009 (5)0.000 (5)0.003 (5)
C60.046 (7)0.059 (8)0.023 (7)0.009 (6)0.000 (5)0.000 (6)
C70.072 (9)0.070 (9)0.012 (7)0.042 (8)0.004 (6)0.007 (6)
C80.066 (9)0.040 (7)0.034 (8)0.024 (6)0.006 (7)0.005 (6)
C90.060 (8)0.029 (6)0.023 (7)0.004 (6)0.001 (6)0.006 (5)
C100.032 (6)0.031 (6)0.022 (6)0.006 (4)0.007 (5)0.000 (5)
C110.052 (7)0.034 (6)0.024 (6)0.004 (6)0.006 (6)0.006 (5)
C120.041 (7)0.039 (7)0.034 (7)0.003 (5)0.018 (5)0.001 (6)
C130.075 (10)0.051 (8)0.021 (7)0.032 (7)0.020 (7)0.020 (6)
C140.049 (8)0.087 (11)0.014 (7)0.031 (7)0.007 (6)0.002 (7)
C150.054 (8)0.056 (8)0.026 (7)0.008 (7)0.003 (6)0.008 (6)
C160.039 (6)0.039 (6)0.028 (7)0.007 (6)0.009 (6)0.002 (5)
C170.027 (6)0.040 (7)0.018 (6)0.003 (5)0.002 (5)0.010 (5)
C180.038 (7)0.045 (7)0.033 (7)0.002 (5)0.005 (5)0.001 (6)
C190.029 (7)0.044 (7)0.082 (11)0.007 (6)0.007 (7)0.010 (7)
C200.028 (6)0.047 (8)0.058 (9)0.005 (6)0.009 (6)0.028 (7)
C210.031 (6)0.053 (8)0.048 (8)0.007 (5)0.005 (6)0.010 (7)
C220.058 (8)0.026 (6)0.030 (7)0.008 (5)0.009 (6)0.007 (5)
C230.041 (7)0.049 (7)0.028 (6)0.000 (5)0.007 (5)0.005 (5)
C240.051 (7)0.027 (6)0.017 (6)0.002 (5)0.002 (5)0.004 (5)
C250.043 (7)0.032 (6)0.030 (7)0.011 (5)0.011 (5)0.005 (5)
C260.027 (6)0.049 (7)0.035 (7)0.013 (5)0.007 (5)0.002 (6)
C270.045 (7)0.036 (7)0.033 (7)0.017 (5)0.016 (6)0.012 (6)
C280.060 (8)0.037 (7)0.027 (7)0.004 (6)0.017 (6)0.011 (6)
C290.049 (7)0.027 (6)0.030 (7)0.001 (5)0.001 (6)0.002 (5)
C300.030 (6)0.023 (5)0.018 (6)0.007 (4)0.004 (4)0.000 (4)
C310.039 (6)0.020 (6)0.028 (6)0.001 (5)0.006 (5)0.001 (5)
C320.063 (8)0.033 (7)0.017 (7)0.010 (5)0.004 (6)0.003 (5)
C330.046 (7)0.028 (6)0.064 (9)0.000 (5)0.018 (7)0.005 (6)
C340.047 (7)0.044 (7)0.033 (7)0.012 (6)0.001 (6)0.016 (6)
C350.036 (6)0.036 (6)0.024 (7)0.004 (5)0.002 (5)0.009 (5)
C360.078 (9)0.023 (6)0.027 (7)0.004 (5)0.003 (6)0.003 (5)
C370.042 (6)0.046 (7)0.019 (6)0.002 (5)0.006 (5)0.003 (5)
C380.033 (6)0.054 (8)0.035 (7)0.001 (5)0.007 (5)0.005 (6)
C390.037 (7)0.033 (7)0.045 (8)0.008 (5)0.014 (5)0.005 (6)
C400.045 (7)0.062 (8)0.023 (6)0.019 (6)0.001 (5)0.006 (6)
C410.051 (8)0.053 (8)0.019 (7)0.011 (6)0.010 (5)0.017 (6)
C420.062 (8)0.051 (7)0.032 (7)0.000 (7)0.016 (6)0.002 (6)
Rh20.0257 (4)0.0337 (5)0.0152 (4)0.0022 (4)0.0000 (4)0.0013 (4)
Cr20.0252 (9)0.0337 (10)0.0242 (10)0.0012 (7)0.0015 (7)0.0001 (7)
P30.0244 (14)0.0294 (15)0.0152 (15)0.0009 (11)0.0004 (11)0.0002 (11)
P40.0302 (14)0.0342 (15)0.0170 (15)0.0062 (12)0.0019 (11)0.0002 (13)
O40.061 (6)0.069 (6)0.014 (5)0.014 (4)0.003 (4)0.013 (4)
O50.049 (5)0.044 (5)0.035 (5)0.009 (4)0.005 (4)0.000 (4)
O60.026 (4)0.081 (6)0.041 (5)0.009 (4)0.000 (4)0.002 (4)
C430.025 (5)0.023 (5)0.020 (6)0.004 (4)0.002 (4)0.000 (5)
C440.032 (6)0.065 (8)0.020 (7)0.003 (6)0.004 (5)0.002 (6)
C450.032 (6)0.032 (6)0.028 (7)0.010 (5)0.001 (5)0.009 (5)
C460.037 (7)0.056 (8)0.023 (7)0.000 (6)0.001 (5)0.007 (5)
C470.020 (5)0.030 (6)0.022 (6)0.000 (4)0.002 (4)0.001 (5)
C480.037 (6)0.045 (7)0.017 (6)0.003 (5)0.011 (5)0.001 (5)
C490.029 (6)0.032 (6)0.044 (8)0.003 (5)0.005 (6)0.001 (5)
C500.028 (6)0.047 (7)0.037 (8)0.004 (5)0.000 (5)0.019 (6)
C510.029 (6)0.032 (6)0.029 (7)0.003 (5)0.002 (5)0.004 (5)
C520.028 (6)0.036 (6)0.023 (6)0.003 (4)0.007 (5)0.005 (5)
C530.030 (6)0.032 (6)0.014 (6)0.004 (5)0.003 (5)0.000 (4)
C540.040 (7)0.037 (6)0.022 (6)0.008 (5)0.002 (5)0.004 (5)
C550.043 (7)0.043 (7)0.017 (6)0.015 (5)0.007 (5)0.000 (5)
C560.037 (6)0.037 (6)0.025 (6)0.005 (5)0.006 (5)0.001 (5)
C570.037 (7)0.042 (7)0.022 (6)0.005 (5)0.003 (5)0.001 (5)
C580.019 (5)0.044 (7)0.022 (6)0.002 (5)0.002 (5)0.005 (5)
C590.020 (5)0.046 (7)0.016 (6)0.001 (5)0.007 (4)0.010 (5)
C600.036 (6)0.039 (6)0.005 (6)0.006 (5)0.003 (4)0.000 (5)
C610.044 (7)0.068 (9)0.020 (7)0.005 (6)0.002 (5)0.001 (6)
C620.059 (8)0.050 (8)0.021 (7)0.002 (6)0.000 (6)0.008 (6)
C630.040 (7)0.041 (7)0.051 (8)0.007 (5)0.002 (6)0.004 (7)
C640.038 (7)0.046 (7)0.021 (7)0.012 (5)0.004 (5)0.002 (5)
C650.022 (6)0.054 (7)0.024 (6)0.008 (5)0.007 (5)0.005 (6)
C660.024 (5)0.035 (6)0.010 (6)0.005 (4)0.003 (4)0.003 (5)
C670.030 (6)0.021 (5)0.031 (6)0.012 (4)0.012 (5)0.006 (4)
C680.037 (6)0.040 (7)0.024 (6)0.001 (5)0.004 (5)0.011 (5)
C690.054 (8)0.020 (6)0.037 (7)0.005 (5)0.027 (6)0.003 (5)
C700.026 (6)0.059 (9)0.036 (7)0.007 (5)0.002 (5)0.001 (6)
C710.020 (5)0.039 (7)0.034 (7)0.007 (5)0.005 (5)0.007 (5)
C720.017 (4)0.032 (5)0.008 (5)0.002 (4)0.001 (4)0.010 (4)
C730.044 (7)0.027 (6)0.019 (6)0.002 (5)0.010 (5)0.009 (5)
C740.060 (8)0.028 (6)0.020 (6)0.003 (5)0.000 (6)0.003 (5)
C750.033 (6)0.053 (7)0.026 (6)0.004 (6)0.003 (5)0.001 (6)
C760.041 (7)0.043 (7)0.019 (6)0.011 (5)0.005 (5)0.006 (5)
C770.032 (6)0.036 (6)0.015 (6)0.005 (5)0.003 (5)0.005 (5)
C780.022 (5)0.037 (5)0.024 (6)0.002 (4)0.001 (4)0.009 (4)
C790.029 (5)0.047 (5)0.004 (5)0.001 (4)0.001 (4)0.008 (4)
C800.029 (6)0.021 (5)0.036 (6)0.005 (4)0.011 (5)0.000 (4)
C810.024 (6)0.048 (7)0.037 (7)0.001 (5)0.000 (5)0.018 (6)
C820.037 (6)0.032 (6)0.025 (6)0.003 (4)0.006 (5)0.005 (5)
C830.025 (6)0.046 (7)0.019 (6)0.009 (5)0.006 (5)0.004 (5)
C840.021 (5)0.037 (6)0.020 (6)0.004 (4)0.002 (4)0.005 (5)
F10.050 (4)0.047 (4)0.039 (4)0.007 (3)0.005 (3)0.009 (3)
F20.039 (4)0.044 (4)0.052 (4)0.001 (3)0.005 (3)0.013 (3)
F30.055 (4)0.050 (4)0.065 (5)0.000 (3)0.016 (4)0.001 (4)
F40.076 (6)0.097 (6)0.069 (6)0.025 (5)0.041 (5)0.024 (5)
B10.026 (7)0.037 (8)0.039 (9)0.007 (5)0.010 (6)0.011 (7)
F50.112 (9)0.182 (12)0.218 (14)0.012 (9)0.060 (10)0.024 (10)
F60.152 (9)0.174 (10)0.052 (6)0.098 (8)0.053 (6)0.017 (6)
B20.060 (10)0.060 (10)0.11 (3)0.017 (13)0.002 (12)0.002 (12)
F70.062 (4)0.049 (4)0.041 (4)0.005 (3)0.015 (4)0.002 (3)
F80.058 (4)0.052 (4)0.041 (4)0.001 (3)0.010 (4)0.001 (3)
B30.053 (8)0.053 (8)0.043 (13)0.023 (10)0.012 (8)0.012 (8)
Geometric parameters (Å, º) top
Rh1—C362.210 (11)Cr2—C502.212 (11)
Rh1—C372.217 (10)Cr2—C492.235 (10)
Rh1—C392.218 (10)Cr2—C512.237 (10)
Rh1—C402.240 (10)Cr2—C432.266 (9)
Rh1—P22.273 (3)P3—C661.792 (10)
Rh1—P12.277 (3)P3—C721.823 (9)
Cr1—C41.807 (11)P3—C431.827 (9)
Cr1—C21.821 (11)P4—C591.807 (10)
Cr1—C31.852 (11)P4—C531.816 (10)
Cr1—C92.158 (11)P4—C521.865 (10)
Cr1—C72.195 (10)O4—C441.152 (12)
Cr1—C12.204 (11)O5—C451.172 (11)
Cr1—C62.232 (11)O6—C461.146 (12)
Cr1—C52.241 (11)C43—C511.432 (13)
Cr1—C82.252 (11)C43—C471.458 (12)
P1—C241.810 (10)C47—C481.390 (13)
P1—C301.812 (9)C47—C521.531 (13)
P1—C11.846 (11)C48—C491.436 (14)
P2—C171.808 (10)C48—H480.9300
P2—C111.810 (11)C49—C501.375 (14)
P2—C101.851 (10)C49—H490.9300
O1—C21.168 (11)C50—C511.415 (13)
O2—C31.133 (11)C50—H500.9300
O3—C41.143 (11)C51—H510.9300
C1—C51.411 (15)C52—C651.509 (12)
C1—C91.455 (13)C52—H520.9800
C5—C61.406 (14)C53—C541.385 (13)
C5—C101.514 (13)C53—C581.407 (13)
C6—C71.418 (15)C54—C551.380 (14)
C6—H60.9300C54—H540.9300
C7—C81.422 (17)C55—C561.388 (14)
C7—H70.9300C55—H550.9300
C8—C91.364 (15)C56—C571.390 (13)
C8—H80.9300C56—H560.9300
C9—H90.9300C57—C581.367 (13)
C10—C231.559 (13)C57—H570.9300
C10—H100.9800C58—H580.9300
C11—C161.362 (14)C59—C601.336 (13)
C11—C121.392 (14)C59—C641.393 (14)
C12—C131.412 (14)C60—C611.404 (14)
C12—H120.9300C60—H600.9300
C13—C141.375 (17)C61—C621.379 (15)
C13—H130.9300C61—H610.9300
C14—C151.368 (16)C62—C631.384 (15)
C14—H140.9300C62—H620.9300
C15—C161.402 (14)C63—C641.381 (14)
C15—H150.9300C63—H630.9300
C16—H160.9300C64—H640.9300
C17—C181.369 (14)C65—H65A0.9600
C17—C221.400 (13)C65—H65B0.9600
C18—C191.408 (15)C65—H65C0.9600
C18—H180.9300C66—C711.404 (13)
C19—C201.371 (16)C66—C671.430 (13)
C19—H190.9300C67—C681.373 (13)
C20—C211.350 (15)C67—H670.9300
C20—H200.9300C68—C691.401 (14)
C21—C221.355 (14)C68—H680.9300
C21—H210.9300C69—C701.383 (15)
C22—H220.9300C69—H690.9300
C23—H23A0.9600C70—C711.381 (14)
C23—H23B0.9600C70—H700.9300
C23—H23C0.9600C71—H710.9300
C24—C291.389 (14)C72—C771.378 (12)
C24—C251.395 (14)C72—C731.406 (13)
C25—C261.376 (13)C73—C741.368 (13)
C25—H250.9300C73—H730.9300
C26—C271.392 (15)C74—C751.356 (13)
C26—H260.9300C74—H740.9300
C27—C281.360 (15)C75—C761.366 (14)
C27—H270.9300C75—H750.9300
C28—C291.359 (14)C76—C771.434 (12)
C28—H280.9300C76—H760.9300
C29—H290.9300C77—H770.9300
C30—C311.365 (13)C78—C791.354 (13)
C30—C351.417 (13)C78—C831.548 (13)
C31—C321.359 (13)C78—H780.9300
C31—H310.9300C79—C801.557 (12)
C32—C331.384 (15)C79—H790.9300
C32—H320.9300C80—C811.549 (13)
C33—C341.372 (15)C80—C841.554 (13)
C33—H330.9300C80—H800.9800
C34—C351.355 (13)C81—C821.379 (13)
C34—H340.9300C81—H810.9300
C35—H350.9300C82—C831.527 (13)
C36—C371.396 (14)C82—H820.9300
C36—C411.563 (14)C83—C841.521 (13)
C36—H360.9300C83—H830.9800
C37—C381.496 (14)C84—H84A0.9700
C37—H370.9300C84—H84B0.9700
C38—C391.535 (14)F1—B11.396 (14)
C38—C421.537 (14)F2—B11.401 (13)
C38—H380.9800F3—B11.363 (13)
C39—C401.369 (15)F4—B11.381 (14)
C39—H390.9300F5—B21.383 (17)
C40—C411.533 (14)F6—B21.300 (16)
C40—H400.9300B2—F6i1.300 (16)
C41—C421.498 (16)B2—F5i1.383 (17)
C41—H410.9800F7—B31.387 (12)
C42—H42A0.9700F8—B31.400 (12)
C42—H42B0.9700B3—F7ii1.387 (12)
Rh2—C822.200 (10)B3—F8ii1.401 (12)
Rh2—C792.206 (9)C85—O71.4297
Rh2—C812.215 (10)C85—H85A0.9802
Rh2—C782.238 (9)C85—H85B0.9799
Rh2—P42.253 (3)C85—H85C0.9808
Rh2—P32.288 (3)O7—H7A0.9500
Cr2—C451.824 (10)C86—O81.4301
Cr2—C441.851 (12)C86—H86A0.9799
Cr2—C461.855 (11)C86—H86B0.9806
Cr2—C472.196 (9)C86—H86C0.9813
Cr2—C482.212 (10)O8—H8A0.9504
C36—Rh1—C3736.8 (4)C45—Cr2—C4688.2 (5)
C36—Rh1—C3976.8 (4)C44—Cr2—C4687.1 (5)
C37—Rh1—C3964.2 (4)C45—Cr2—C4787.0 (4)
C36—Rh1—C4065.2 (4)C44—Cr2—C47142.5 (4)
C37—Rh1—C4076.1 (4)C46—Cr2—C47129.4 (4)
C39—Rh1—C4035.8 (4)C45—Cr2—C48104.3 (4)
C36—Rh1—P2160.2 (3)C44—Cr2—C48169.0 (4)
C37—Rh1—P2157.3 (3)C46—Cr2—C4897.1 (4)
C39—Rh1—P299.7 (3)C47—Cr2—C4836.8 (3)
C40—Rh1—P2100.5 (3)C45—Cr2—C50165.7 (4)
C36—Rh1—P199.4 (3)C44—Cr2—C50102.8 (5)
C37—Rh1—P198.1 (3)C46—Cr2—C50103.3 (4)
C39—Rh1—P1155.5 (3)C47—Cr2—C5079.1 (4)
C40—Rh1—P1161.2 (3)C48—Cr2—C5066.3 (4)
P2—Rh1—P191.60 (10)C45—Cr2—C49139.6 (4)
C4—Cr1—C290.4 (5)C44—Cr2—C49133.4 (5)
C4—Cr1—C386.4 (5)C46—Cr2—C4985.3 (4)
C2—Cr1—C387.5 (5)C47—Cr2—C4967.3 (4)
C4—Cr1—C986.5 (4)C48—Cr2—C4937.7 (4)
C2—Cr1—C9134.0 (4)C50—Cr2—C4936.0 (4)
C3—Cr1—C9137.9 (5)C45—Cr2—C51133.0 (4)
C4—Cr1—C7129.5 (5)C44—Cr2—C5191.0 (4)
C2—Cr1—C7139.4 (5)C46—Cr2—C51138.5 (4)
C3—Cr1—C787.8 (5)C47—Cr2—C5167.8 (4)
C9—Cr1—C765.7 (5)C48—Cr2—C5179.1 (4)
C4—Cr1—C1105.0 (5)C50—Cr2—C5137.1 (3)
C2—Cr1—C199.1 (4)C49—Cr2—C5166.4 (4)
C3—Cr1—C1166.7 (4)C45—Cr2—C43100.1 (4)
C9—Cr1—C139.0 (4)C44—Cr2—C43107.6 (4)
C7—Cr1—C179.6 (4)C46—Cr2—C43163.4 (4)
C4—Cr1—C6163.7 (5)C47—Cr2—C4338.1 (3)
C2—Cr1—C6104.5 (4)C48—Cr2—C4367.0 (3)
C3—Cr1—C6100.5 (4)C50—Cr2—C4366.6 (3)
C9—Cr1—C678.5 (4)C49—Cr2—C4379.0 (4)
C7—Cr1—C637.4 (4)C51—Cr2—C4337.1 (3)
C1—Cr1—C666.7 (4)C66—P3—C72105.4 (4)
C4—Cr1—C5140.5 (4)C66—P3—C43107.8 (4)
C2—Cr1—C587.6 (4)C72—P3—C43105.2 (4)
C3—Cr1—C5132.8 (4)C66—P3—Rh2112.3 (3)
C9—Cr1—C567.5 (4)C72—P3—Rh2110.4 (3)
C7—Cr1—C566.9 (4)C43—P3—Rh2115.0 (3)
C1—Cr1—C537.0 (4)C59—P4—C53110.6 (5)
C6—Cr1—C536.6 (4)C59—P4—C52103.9 (4)
C4—Cr1—C896.7 (5)C53—P4—C52104.0 (5)
C2—Cr1—C8166.6 (4)C59—P4—Rh2111.0 (3)
C3—Cr1—C8104.2 (5)C53—P4—Rh2111.5 (3)
C9—Cr1—C836.0 (4)C52—P4—Rh2115.5 (3)
C7—Cr1—C837.3 (4)C51—C43—C47117.7 (8)
C1—Cr1—C868.2 (4)C51—C43—P3119.8 (7)
C6—Cr1—C867.4 (4)C47—C43—P3121.7 (7)
C5—Cr1—C879.7 (4)C51—C43—Cr270.4 (5)
C24—P1—C30106.0 (5)C47—C43—Cr268.4 (5)
C24—P1—C1107.3 (5)P3—C43—Cr2141.4 (5)
C30—P1—C1105.8 (4)O4—C44—Cr2173.7 (10)
C24—P1—Rh1110.6 (3)O5—C45—Cr2177.3 (9)
C30—P1—Rh1115.0 (3)O6—C46—Cr2176.3 (9)
C1—P1—Rh1111.6 (3)C48—C47—C43120.5 (9)
C17—P2—C11104.6 (5)C48—C47—C52119.3 (8)
C17—P2—C10106.4 (4)C43—C47—C52120.1 (8)
C11—P2—C10106.8 (5)C48—C47—Cr272.2 (6)
C17—P2—Rh1109.5 (3)C43—C47—Cr273.6 (5)
C11—P2—Rh1115.0 (4)C52—C47—Cr2128.5 (7)
C10—P2—Rh1113.9 (3)C47—C48—C49120.6 (9)
C5—C1—C9117.2 (10)C47—C48—Cr271.0 (6)
C5—C1—P1121.1 (7)C49—C48—Cr272.0 (6)
C9—C1—P1120.7 (9)C47—C48—H48119.7
C5—C1—Cr172.9 (6)C49—C48—H48119.7
C9—C1—Cr168.8 (6)Cr2—C48—H48129.8
P1—C1—Cr1138.8 (5)C50—C49—C48118.9 (10)
O1—C2—Cr1178.5 (10)C50—C49—Cr271.1 (6)
O2—C3—Cr1179.0 (9)C48—C49—Cr270.3 (6)
O3—C4—Cr1178.8 (9)C50—C49—H49120.6
C6—C5—C1119.9 (10)C48—C49—H49120.6
C6—C5—C10119.7 (10)Cr2—C49—H49130.6
C1—C5—C10120.4 (9)C49—C50—C51122.6 (10)
C6—C5—Cr171.3 (6)C49—C50—Cr272.9 (6)
C1—C5—Cr170.1 (6)C51—C50—Cr272.4 (6)
C10—C5—Cr1132.4 (7)C49—C50—H50118.7
C5—C6—C7119.9 (11)C51—C50—H50118.7
C5—C6—Cr172.0 (6)Cr2—C50—H50128.4
C7—C6—Cr169.9 (6)C50—C51—C43119.5 (9)
C5—C6—H6120.0C50—C51—Cr270.5 (6)
C7—C6—H6120.0C43—C51—Cr272.6 (6)
Cr1—C6—H6130.6C50—C51—H51120.2
C6—C7—C8122.2 (11)C43—C51—H51120.2
C6—C7—Cr172.7 (6)Cr2—C51—H51129.0
C8—C7—Cr173.5 (6)C65—C52—C47113.9 (8)
C6—C7—H7118.9C65—C52—P4116.1 (7)
C8—C7—H7118.9C47—C52—P4107.8 (6)
Cr1—C7—H7126.9C65—C52—H52106.1
C9—C8—C7115.9 (11)C47—C52—H52106.1
C9—C8—Cr168.3 (6)P4—C52—H52106.1
C7—C8—Cr169.2 (6)C54—C53—C58119.2 (9)
C9—C8—H8122.0C54—C53—P4124.4 (8)
C7—C8—H8122.0C58—C53—P4116.3 (7)
Cr1—C8—H8133.1C55—C54—C53119.1 (10)
C8—C9—C1124.7 (11)C55—C54—H54120.5
C8—C9—Cr175.8 (7)C53—C54—H54120.5
C1—C9—Cr172.2 (6)C54—C55—C56121.8 (10)
C8—C9—H9117.7C54—C55—H55119.1
C1—C9—H9117.7C56—C55—H55119.1
Cr1—C9—H9126.4C55—C56—C57118.9 (10)
C5—C10—C23114.1 (8)C55—C56—H56120.5
C5—C10—P2109.5 (7)C57—C56—H56120.5
C23—C10—P2114.4 (7)C58—C57—C56119.9 (10)
C5—C10—H10106.0C58—C57—H57120.1
C23—C10—H10106.0C56—C57—H57120.1
P2—C10—H10106.0C57—C58—C53121.1 (9)
C16—C11—C12120.0 (10)C57—C58—H58119.5
C16—C11—P2122.0 (8)C53—C58—H58119.5
C12—C11—P2117.8 (9)C60—C59—C64119.5 (9)
C11—C12—C13119.4 (11)C60—C59—P4124.0 (8)
C11—C12—H12120.3C64—C59—P4116.5 (8)
C13—C12—H12120.3C59—C60—C61121.1 (10)
C14—C13—C12119.3 (12)C59—C60—H60119.4
C14—C13—H13120.3C61—C60—H60119.4
C12—C13—H13120.3C62—C61—C60120.5 (11)
C15—C14—C13121.0 (11)C62—C61—H61119.8
C15—C14—H14119.5C60—C61—H61119.8
C13—C14—H14119.5C61—C62—C63117.7 (11)
C14—C15—C16119.5 (12)C61—C62—H62121.1
C14—C15—H15120.3C63—C62—H62121.1
C16—C15—H15120.3C64—C63—C62121.5 (11)
C11—C16—C15120.7 (11)C64—C63—H63119.3
C11—C16—H16119.7C62—C63—H63119.3
C15—C16—H16119.7C63—C64—C59119.7 (10)
C18—C17—C22117.4 (9)C63—C64—H64120.2
C18—C17—P2121.4 (8)C59—C64—H64120.2
C22—C17—P2120.7 (8)C52—C65—H65A109.5
C17—C18—C19119.6 (11)C52—C65—H65B109.5
C17—C18—H18120.2H65A—C65—H65B109.5
C19—C18—H18120.2C52—C65—H65C109.5
C20—C19—C18121.7 (12)H65A—C65—H65C109.5
C20—C19—H19119.1H65B—C65—H65C109.5
C18—C19—H19119.1C71—C66—C67117.1 (9)
C21—C20—C19117.6 (11)C71—C66—P3120.5 (7)
C21—C20—H20121.2C67—C66—P3122.4 (7)
C19—C20—H20121.2C68—C67—C66120.6 (9)
C20—C21—C22122.2 (12)C68—C67—H67119.7
C20—C21—H21118.9C66—C67—H67119.7
C22—C21—H21118.9C67—C68—C69120.5 (10)
C21—C22—C17121.5 (11)C67—C68—H68119.8
C21—C22—H22119.3C69—C68—H68119.8
C17—C22—H22119.3C70—C69—C68120.0 (10)
C10—C23—H23A109.5C70—C69—H69120.0
C10—C23—H23B109.5C68—C69—H69120.0
H23A—C23—H23B109.5C71—C70—C69119.7 (10)
C10—C23—H23C109.5C71—C70—H70120.1
H23A—C23—H23C109.5C69—C70—H70120.1
H23B—C23—H23C109.5C70—C71—C66122.0 (10)
C29—C24—C25116.2 (9)C70—C71—H71119.0
C29—C24—P1121.8 (8)C66—C71—H71119.0
C25—C24—P1121.5 (8)C77—C72—C73120.1 (9)
C26—C25—C24121.3 (10)C77—C72—P3120.4 (7)
C26—C25—H25119.4C73—C72—P3118.5 (7)
C24—C25—H25119.4C74—C73—C72119.0 (9)
C25—C26—C27118.7 (11)C74—C73—H73120.5
C25—C26—H26120.7C72—C73—H73120.5
C27—C26—H26120.7C75—C74—C73121.6 (10)
C28—C27—C26121.9 (10)C75—C74—H74119.2
C28—C27—H27119.0C73—C74—H74119.2
C26—C27—H27119.0C74—C75—C76121.4 (10)
C29—C28—C27117.5 (11)C74—C75—H75119.3
C29—C28—H28121.2C76—C75—H75119.3
C27—C28—H28121.2C75—C76—C77118.5 (10)
C28—C29—C24124.1 (11)C75—C76—H76120.7
C28—C29—H29117.9C77—C76—H76120.7
C24—C29—H29117.9C72—C77—C76119.3 (9)
C31—C30—C35119.3 (9)C72—C77—H77120.4
C31—C30—P1119.7 (7)C76—C77—H77120.4
C35—C30—P1121.1 (7)C79—C78—C83106.7 (8)
C32—C31—C30120.6 (10)C79—C78—Rh271.0 (6)
C32—C31—H31119.7C83—C78—Rh294.6 (6)
C30—C31—H31119.7C79—C78—H78126.7
C31—C32—C33120.4 (10)C83—C78—H78126.7
C31—C32—H32119.8Rh2—C78—H78101.9
C33—C32—H32119.8C78—C79—C80106.2 (8)
C34—C33—C32119.5 (10)C78—C79—Rh273.6 (6)
C34—C33—H33120.2C80—C79—Rh295.4 (5)
C32—C33—H33120.2C78—C79—H79126.9
C35—C34—C33120.9 (11)C80—C79—H79126.9
C35—C34—H34119.5Rh2—C79—H7999.0
C33—C34—H34119.5C81—C80—C8498.9 (8)
C34—C35—C30119.2 (10)C81—C80—C79102.5 (7)
C34—C35—H35120.4C84—C80—C79100.3 (8)
C30—C35—H35120.4C81—C80—H80117.4
C37—C36—C41104.5 (9)C84—C80—H80117.4
C37—C36—Rh171.9 (6)C79—C80—H80117.4
C41—C36—Rh196.7 (7)C82—C81—C80106.8 (8)
C37—C36—H36127.7C82—C81—Rh271.2 (6)
C41—C36—H36127.7C80—C81—Rh295.3 (6)
Rh1—C36—H3699.1C82—C81—H81126.6
C36—C37—C38108.9 (9)C80—C81—H81126.6
C36—C37—Rh171.4 (6)Rh2—C81—H81101.1
C38—C37—Rh197.3 (6)C81—C82—C83105.3 (9)
C36—C37—H37125.6C81—C82—Rh272.4 (6)
C38—C37—H37125.6C83—C82—Rh296.8 (6)
Rh1—C37—H3799.5C81—C82—H82127.3
C37—C38—C39102.0 (8)C83—C82—H82127.3
C37—C38—C4299.0 (9)Rh2—C82—H8298.7
C39—C38—C4297.4 (9)C84—C83—C82102.0 (8)
C37—C38—H38118.2C84—C83—C78100.5 (8)
C39—C38—H38118.2C82—C83—C78102.9 (7)
C42—C38—H38118.2C84—C83—H83116.3
C40—C39—C38107.9 (9)C82—C83—H83116.3
C40—C39—Rh173.0 (6)C78—C83—H83116.3
C38—C39—Rh196.1 (7)C83—C84—C8093.1 (7)
C40—C39—H39126.1C83—C84—H84A113.1
C38—C39—H39126.1C80—C84—H84A113.1
Rh1—C39—H3999.1C83—C84—H84B113.1
C39—C40—C41106.5 (10)C80—C84—H84B113.1
C39—C40—Rh171.2 (6)H84A—C84—H84B110.5
C41—C40—Rh196.5 (6)F3—B1—F4111.2 (10)
C39—C40—H40126.8F3—B1—F1109.8 (10)
C41—C40—H40126.8F4—B1—F1109.1 (9)
Rh1—C40—H40100.1F3—B1—F2109.9 (9)
C42—C41—C4099.1 (10)F4—B1—F2108.2 (10)
C42—C41—C3699.6 (9)F1—B1—F2108.4 (10)
C40—C41—C36101.4 (8)F6—B2—F6i113 (2)
C42—C41—H41117.8F6—B2—F5106.7 (7)
C40—C41—H41117.8F6i—B2—F5110.3 (7)
C36—C41—H41117.8F6—B2—F5i110.3 (7)
C41—C42—C3897.1 (9)F6i—B2—F5i106.7 (7)
C41—C42—H42A112.3F5—B2—F5i110 (2)
C38—C42—H42A112.3F7ii—B3—F7110.0 (14)
C41—C42—H42B112.3F7ii—B3—F8109.5 (4)
C38—C42—H42B112.3F7—B3—F8109.4 (3)
H42A—C42—H42B109.9F7ii—B3—F8ii109.4 (3)
C82—Rh2—C7977.9 (4)F7—B3—F8ii109.5 (4)
C82—Rh2—C8136.4 (4)F8—B3—F8ii109.0 (14)
C79—Rh2—C8166.4 (4)O7—C85—H85A109.3
C82—Rh2—C7865.6 (4)O7—C85—H85B109.5
C79—Rh2—C7835.5 (3)H85A—C85—H85B109.5
C81—Rh2—C7877.2 (4)O7—C85—H85C109.6
C82—Rh2—P499.4 (3)H85A—C85—H85C109.5
C79—Rh2—P4154.2 (3)H85B—C85—H85C109.4
C81—Rh2—P495.9 (3)C85—O7—H7A104.1
C78—Rh2—P4162.7 (3)O8—C86—H86A109.5
C82—Rh2—P3155.8 (3)O8—C86—H86B109.4
C79—Rh2—P3101.4 (2)H86A—C86—H86B109.7
C81—Rh2—P3163.5 (3)O8—C86—H86C109.4
C78—Rh2—P399.5 (3)H86A—C86—H86C109.4
P4—Rh2—P391.42 (9)H86B—C86—H86C109.5
C45—Cr2—C4485.9 (5)C86—O8—H8A108.0
Symmetry codes: (i) y, x, z; (ii) y+1, x1, z.
(III) (R,R)-tricarbonyl-1κ3C-{µ-1(η6):2κ2P,P'-1-(diphenylphosphino)-2-[1- (diphenylphosphino)ethyl]benzene}[2(η4)-(Z,Z)-cycloocta-1,5- diene]chromium(0)rhodium(I) tetrafluoroborate methanol 1.5-solvate top
Crystal data top
[CrRh(C8H12)(C32H28P2)(CO)3]·BF4·1.5CH4OF(000) = 978
Mr = 956.47Dx = 1.475 Mg m3
Monoclinic, P21Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2ybCell parameters from 5000 reflections
a = 11.262 (2) Åθ = 4–20°
b = 14.116 (3) ŵ = 0.77 mm1
c = 14.226 (3) ÅT = 200 K
β = 107.81 (3)°Prism, red
V = 2153.2 (7) Å30.50 × 0.30 × 0.30 mm
Z = 2
Data collection top
Stoe IPDS image-plate
diffractometer
6454 independent reflections
Radiation source: fine-focus sealed tube5511 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.035
ϕ scansθmax = 24.4°, θmin = 2.0°
Absorption correction: empirical (using intensity measurements)
(ABSCOR; Stoe & Cie, 1995)
h = 1212
Tmin = 0.700, Tmax = 0.802k = 1615
11684 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)] = 0.034H-atom parameters constrained
wR(F2) = 0.074 w = 1/[σ2(Fo2) + (0.0388P)2]
where P = (Fo2 + 2Fc2)/3
S = 0.95(Δ/σ)max = 0.009
6454 reflectionsΔρmax = 0.63 e Å3
532 parametersΔρmin = 0.34 e Å3
3 restraintsAbsolute structure: Flack (1983), 2773 Friedel pairs
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.00 (2)
Crystal data top
[CrRh(C8H12)(C32H28P2)(CO)3]·BF4·1.5CH4OV = 2153.2 (7) Å3
Mr = 956.47Z = 2
Monoclinic, P21Mo Kα radiation
a = 11.262 (2) ŵ = 0.77 mm1
b = 14.116 (3) ÅT = 200 K
c = 14.226 (3) Å0.50 × 0.30 × 0.30 mm
β = 107.81 (3)°
Data collection top
Stoe IPDS image-plate
diffractometer
6454 independent reflections
Absorption correction: empirical (using intensity measurements)
(ABSCOR; Stoe & Cie, 1995)
5511 reflections with I > 2σ(I)
Tmin = 0.700, Tmax = 0.802Rint = 0.035
11684 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.034H-atom parameters constrained
wR(F2) = 0.074Δρmax = 0.63 e Å3
S = 0.95Δρmin = 0.34 e Å3
6454 reflectionsAbsolute structure: Flack (1983), 2773 Friedel pairs
532 parametersAbsolute structure parameter: 0.00 (2)
3 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*/UeqOcc. (<1)
Rh10.48626 (3)0.63969 (2)0.77159 (2)0.02141 (10)
Cr10.34290 (8)0.25708 (6)0.71544 (6)0.0234 (2)
P10.33189 (12)0.52834 (10)0.74748 (10)0.0202 (3)
P20.63296 (12)0.52357 (10)0.81948 (10)0.0222 (3)
O10.3343 (5)0.0440 (3)0.6990 (4)0.0573 (14)
O20.0743 (3)0.2426 (3)0.7071 (3)0.0462 (9)
O30.4147 (4)0.2278 (3)0.9335 (3)0.0504 (11)
C10.3702 (4)0.4137 (3)0.7007 (3)0.0201 (10)
C20.2925 (4)0.3750 (3)0.6104 (3)0.0258 (11)
H2A0.20500.39500.58650.031*
C30.3309 (5)0.2999 (3)0.5630 (3)0.0294 (12)
H3A0.27130.26870.50650.035*
C40.4482 (5)0.2599 (4)0.6068 (3)0.0305 (11)
H4A0.46940.19990.58100.037*
C50.5255 (5)0.2944 (3)0.6964 (4)0.0267 (11)
H5A0.59880.25700.73190.032*
C60.4883 (4)0.3692 (3)0.7469 (3)0.0224 (11)
C70.5741 (4)0.4053 (3)0.8439 (3)0.0209 (11)
H7A0.52260.41600.88730.025*
C80.6765 (5)0.3348 (4)0.8969 (4)0.0321 (12)
H8A0.63900.27600.90650.048*
H8B0.72370.36030.95980.048*
H8C0.73090.32400.85750.048*
C90.3397 (5)0.1269 (5)0.7041 (3)0.0391 (14)
C100.1783 (5)0.2485 (4)0.7096 (4)0.0333 (12)
C110.3860 (5)0.2394 (3)0.8494 (4)0.0310 (12)
C120.2957 (4)0.5065 (3)0.8624 (3)0.0244 (11)
C130.3506 (5)0.5640 (3)0.9442 (3)0.0273 (11)
H13A0.40920.60930.94080.033*
C140.3186 (5)0.5541 (4)1.0299 (4)0.0373 (13)
H14A0.35600.59241.08410.045*
C150.2321 (5)0.4882 (4)1.0354 (4)0.0401 (14)
H15A0.21010.48231.09300.048*
C160.1777 (5)0.4307 (4)0.9563 (4)0.0394 (13)
H16A0.11930.38570.96080.047*
C170.2092 (5)0.4389 (4)0.8694 (4)0.0320 (12)
H17A0.17250.39930.81620.038*
C180.1834 (4)0.5623 (3)0.6595 (3)0.0214 (10)
C190.0786 (4)0.5843 (3)0.6864 (4)0.0306 (12)
H19A0.07920.57490.75120.037*
C200.0277 (4)0.6203 (4)0.6174 (4)0.0406 (15)
H20A0.09710.63600.63660.049*
C210.0302 (4)0.6326 (6)0.5222 (4)0.0463 (13)
H21A0.10280.65460.47620.056*
C220.0728 (5)0.6133 (3)0.4921 (4)0.0364 (14)
H22A0.07110.62410.42720.044*
C230.1791 (5)0.5774 (3)0.5607 (4)0.0312 (12)
H23A0.24860.56320.54110.037*
C240.6969 (4)0.4961 (3)0.7200 (4)0.0257 (11)
C250.8037 (5)0.4397 (4)0.7324 (4)0.0375 (13)
H25A0.85310.42210.79520.045*
C260.8340 (6)0.4108 (4)0.6489 (5)0.0519 (17)
H26A0.90350.37260.65600.062*
C270.7622 (6)0.4382 (5)0.5558 (5)0.0539 (17)
H27A0.78330.41780.50080.065*
C280.6621 (5)0.4942 (4)0.5440 (4)0.0405 (14)
H28A0.61580.51360.48100.049*
C290.6273 (5)0.5233 (4)0.6253 (4)0.0298 (11)
H29A0.55710.56110.61610.036*
C300.7602 (4)0.5489 (3)0.9305 (4)0.0294 (12)
C310.8741 (5)0.5863 (4)0.9282 (5)0.0412 (14)
H31A0.88980.59410.86820.049*
C320.9640 (5)0.6120 (4)1.0155 (5)0.0561 (19)
H32A1.03960.63721.01370.067*
C330.9417 (6)0.6006 (5)1.1039 (5)0.0602 (19)
H33A1.00310.61631.16230.072*
C340.8301 (6)0.5662 (4)1.1071 (4)0.0488 (16)
H34A0.81530.55941.16760.059*
C350.7393 (5)0.5416 (4)1.0219 (4)0.0372 (13)
H35A0.66270.51971.02510.045*
C360.3429 (5)0.7555 (5)0.7539 (4)0.0319 (13)
H36A0.25830.73230.74550.038*
C370.3780 (5)0.7511 (4)0.6693 (4)0.0337 (12)
H37A0.31300.72520.61240.040*
C380.4643 (6)0.8215 (4)0.6405 (4)0.0436 (15)
H38A0.45980.88200.67170.052*
H38B0.43460.83110.56960.052*
C390.6025 (6)0.7889 (4)0.6703 (4)0.0474 (16)
H39A0.61370.74640.62010.057*
H39B0.65540.84370.67300.057*
C400.6429 (5)0.7393 (4)0.7688 (4)0.0314 (13)
H40A0.72460.70860.78390.038*
C410.6073 (5)0.7600 (4)0.8505 (4)0.0295 (12)
H41A0.66890.74080.91260.035*
C420.5309 (5)0.8449 (4)0.8616 (4)0.0352 (13)
H42A0.54060.89460.81730.042*
H42B0.56290.86880.92850.042*
C430.3912 (5)0.8222 (4)0.8390 (4)0.0409 (14)
H43A0.37760.79450.89730.049*
H43B0.34410.88080.82460.049*
B10.2944 (6)0.5734 (5)0.3265 (6)0.0491 (18)
F10.3742 (5)0.5434 (5)0.2812 (4)0.125 (2)
F20.1993 (4)0.5114 (3)0.3198 (4)0.1059 (16)
F30.2351 (9)0.6544 (9)0.3038 (10)0.100 (4)*0.491 (14)
F40.3723 (9)0.5784 (8)0.4216 (6)0.068 (3)*0.491 (14)
F3'0.2441 (6)0.6425 (8)0.2476 (7)0.067 (3)*0.509 (14)
F4'0.3289 (8)0.6268 (10)0.4078 (6)0.083 (3)*0.509 (14)
O1000.0839 (4)0.3606 (3)0.3735 (4)0.0674 (13)
H1000.12030.41520.35460.088*
C1000.0335 (7)0.3835 (6)0.3807 (8)0.094 (3)
H1010.08210.41330.32090.141*
H1020.02390.42600.43530.141*
H1030.07370.32660.39140.141*
O2000.0229 (9)0.2499 (5)0.1956 (6)0.058 (2)0.50
H2000.06320.27540.25910.075*0.50
C2000.0024 (15)0.3204 (9)0.1265 (9)0.068 (4)0.50
H2010.08240.34220.12050.102*0.50
H2020.04030.37340.14690.102*0.50
H2030.04960.29620.06260.102*0.50
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Rh10.02224 (17)0.01532 (16)0.02386 (18)0.0007 (2)0.00291 (13)0.0010 (2)
Cr10.0274 (4)0.0192 (4)0.0215 (4)0.0000 (4)0.0045 (3)0.0011 (4)
P10.0190 (7)0.0165 (7)0.0220 (7)0.0016 (6)0.0018 (6)0.0001 (7)
P20.0190 (6)0.0193 (7)0.0253 (7)0.0004 (6)0.0023 (6)0.0014 (6)
O10.087 (4)0.008 (2)0.088 (4)0.001 (2)0.043 (3)0.006 (2)
O20.034 (2)0.045 (2)0.057 (2)0.0031 (19)0.0103 (18)0.001 (2)
O30.060 (3)0.063 (3)0.025 (2)0.013 (2)0.0076 (19)0.0066 (19)
C10.024 (2)0.014 (2)0.020 (2)0.0022 (19)0.003 (2)0.0015 (19)
C20.024 (2)0.023 (3)0.024 (3)0.000 (2)0.001 (2)0.003 (2)
C30.044 (3)0.022 (3)0.021 (3)0.001 (2)0.007 (2)0.003 (2)
C40.044 (3)0.021 (2)0.030 (3)0.000 (2)0.017 (2)0.007 (2)
C50.032 (3)0.021 (2)0.028 (3)0.003 (2)0.010 (2)0.002 (2)
C60.025 (3)0.018 (2)0.022 (3)0.004 (2)0.004 (2)0.001 (2)
C70.022 (3)0.020 (3)0.018 (3)0.002 (2)0.002 (2)0.006 (2)
C80.029 (3)0.025 (3)0.034 (3)0.011 (2)0.002 (2)0.007 (2)
C90.040 (3)0.050 (4)0.032 (3)0.000 (3)0.018 (2)0.000 (3)
C100.041 (3)0.024 (3)0.032 (3)0.001 (3)0.007 (2)0.001 (2)
C110.032 (3)0.018 (3)0.041 (3)0.011 (2)0.007 (2)0.000 (2)
C120.025 (2)0.021 (3)0.026 (3)0.004 (2)0.005 (2)0.004 (2)
C130.034 (3)0.022 (3)0.025 (3)0.003 (2)0.008 (2)0.003 (2)
C140.055 (4)0.030 (3)0.025 (3)0.009 (3)0.009 (3)0.003 (2)
C150.049 (3)0.042 (3)0.036 (3)0.015 (3)0.023 (3)0.010 (3)
C160.041 (3)0.044 (3)0.038 (3)0.002 (3)0.020 (3)0.004 (3)
C170.027 (3)0.037 (3)0.031 (3)0.006 (2)0.007 (2)0.000 (2)
C180.018 (2)0.015 (2)0.028 (3)0.0047 (19)0.001 (2)0.002 (2)
C190.029 (3)0.027 (3)0.033 (3)0.001 (2)0.006 (2)0.001 (2)
C200.026 (2)0.037 (4)0.052 (3)0.011 (3)0.003 (2)0.002 (3)
C210.032 (3)0.047 (3)0.044 (3)0.010 (4)0.012 (2)0.007 (4)
C220.038 (3)0.034 (4)0.027 (3)0.007 (2)0.005 (2)0.004 (2)
C230.032 (3)0.024 (3)0.034 (3)0.006 (2)0.004 (2)0.004 (2)
C240.021 (2)0.019 (2)0.036 (3)0.001 (2)0.008 (2)0.003 (2)
C250.024 (3)0.037 (3)0.054 (4)0.007 (2)0.016 (3)0.003 (3)
C260.039 (3)0.046 (4)0.079 (5)0.004 (3)0.029 (4)0.013 (4)
C270.055 (4)0.062 (4)0.055 (4)0.007 (3)0.033 (4)0.025 (4)
C280.049 (4)0.037 (3)0.037 (3)0.011 (3)0.015 (3)0.013 (3)
C290.031 (3)0.031 (3)0.029 (3)0.001 (2)0.011 (2)0.009 (2)
C300.019 (2)0.024 (3)0.037 (3)0.008 (2)0.003 (2)0.003 (2)
C310.029 (3)0.034 (3)0.057 (4)0.002 (3)0.008 (3)0.012 (3)
C320.026 (3)0.043 (4)0.083 (5)0.001 (2)0.006 (3)0.021 (3)
C330.045 (4)0.061 (4)0.050 (4)0.017 (3)0.021 (3)0.027 (3)
C340.041 (4)0.054 (4)0.038 (3)0.012 (3)0.008 (3)0.008 (3)
C350.040 (3)0.027 (3)0.041 (3)0.004 (3)0.007 (3)0.006 (3)
C360.027 (3)0.023 (3)0.042 (3)0.002 (3)0.005 (3)0.001 (3)
C370.038 (3)0.021 (3)0.032 (3)0.004 (3)0.004 (2)0.011 (2)
C380.063 (4)0.025 (3)0.039 (3)0.002 (3)0.010 (3)0.012 (3)
C390.069 (4)0.035 (3)0.041 (4)0.013 (3)0.021 (3)0.005 (3)
C400.024 (3)0.029 (3)0.043 (3)0.008 (2)0.013 (2)0.002 (3)
C410.027 (3)0.020 (2)0.037 (3)0.008 (2)0.004 (2)0.006 (3)
C420.042 (3)0.031 (3)0.032 (3)0.003 (3)0.011 (3)0.006 (3)
C430.052 (4)0.019 (3)0.052 (4)0.008 (3)0.018 (3)0.005 (3)
B10.032 (4)0.042 (4)0.070 (5)0.007 (3)0.011 (4)0.002 (4)
F10.112 (4)0.160 (6)0.125 (5)0.001 (4)0.071 (4)0.032 (4)
F20.095 (3)0.087 (3)0.131 (4)0.051 (3)0.028 (3)0.008 (3)
O1000.062 (3)0.054 (3)0.083 (3)0.007 (2)0.019 (3)0.016 (3)
C1000.051 (5)0.063 (5)0.161 (9)0.010 (4)0.023 (5)0.015 (5)
O2000.121 (8)0.026 (4)0.046 (5)0.004 (5)0.053 (5)0.003 (4)
C2000.100 (12)0.061 (9)0.040 (7)0.026 (8)0.019 (8)0.002 (7)
Geometric parameters (Å, º) top
Rh1—C372.234 (5)C22—H22A0.9300
Rh1—C412.251 (5)C23—H23A0.9300
Rh1—C362.257 (6)C24—C291.390 (7)
Rh1—C402.265 (5)C24—C251.408 (7)
Rh1—P22.2786 (15)C25—C261.394 (8)
Rh1—P12.2904 (15)C25—H25A0.9300
Cr1—C111.833 (6)C26—C271.379 (9)
Cr1—C101.833 (6)C26—H26A0.9300
Cr1—C91.844 (7)C27—C281.344 (8)
Cr1—C22.192 (5)C27—H27A0.9300
Cr1—C32.215 (5)C28—C291.392 (7)
Cr1—C42.218 (5)C28—H28A0.9300
Cr1—C52.218 (5)C29—H29A0.9300
Cr1—C62.222 (5)C30—C351.395 (7)
Cr1—C12.250 (4)C30—C311.396 (7)
P1—C181.820 (5)C31—C321.389 (8)
P1—C121.828 (5)C31—H31A0.9300
P1—C11.851 (5)C32—C331.365 (9)
P2—C301.814 (5)C32—H32A0.9300
P2—C241.815 (5)C33—C341.361 (9)
P2—C71.868 (5)C33—H33A0.9300
O1—C91.172 (8)C34—C351.370 (8)
O2—C101.164 (6)C34—H34A0.9300
O3—C111.152 (6)C35—H35A0.9300
C1—C21.424 (6)C36—C371.378 (8)
C1—C61.435 (6)C36—C431.499 (8)
C2—C31.395 (7)C36—H36A0.9800
C2—H2A0.9800C37—C381.531 (8)
C3—C41.396 (7)C37—H37A0.9800
C3—H3A0.9800C38—C391.553 (9)
C4—C51.394 (7)C38—H38A0.9700
C4—H4A0.9800C38—H38B0.9700
C5—C61.410 (7)C39—C401.507 (8)
C5—H5A0.9800C39—H39A0.9700
C6—C71.510 (6)C39—H39B0.9700
C7—C81.536 (6)C40—C411.372 (7)
C7—H7A0.9800C40—H40A0.9800
C8—H8A0.9600C41—C421.511 (7)
C8—H8B0.9600C41—H41A0.9800
C8—H8C0.9600C42—C431.540 (8)
C12—C171.390 (7)C42—H42A0.9700
C12—C131.398 (7)C42—H42B0.9700
C13—C141.381 (7)C43—H43A0.9700
C13—H13A0.9300C43—H43B0.9700
C14—C151.366 (7)B1—F31.314 (14)
C14—H14A0.9300B1—F11.326 (8)
C15—C161.371 (8)B1—F4'1.335 (12)
C15—H15A0.9300B1—F21.363 (8)
C16—C171.391 (7)B1—F41.370 (11)
C16—H16A0.9300B1—F3'1.465 (12)
C17—H17A0.9300O100—C1001.395 (8)
C18—C191.383 (6)O100—H1000.9500
C18—C231.407 (7)C100—H1010.9572
C19—C201.391 (7)C100—H1020.9608
C19—H19A0.9300C100—H1030.9565
C20—C211.358 (7)O200—C2001.369 (12)
C20—H20A0.9300O200—H2000.9500
C21—C221.381 (7)C200—H2010.9801
C21—H21A0.9300C200—H2020.9801
C22—C231.388 (7)C200—H2030.9801
C37—Rh1—C4185.4 (2)C16—C17—H17A120.1
C37—Rh1—C3635.7 (2)C19—C18—C23118.1 (4)
C41—Rh1—C3679.2 (2)C19—C18—P1123.4 (4)
C37—Rh1—C4079.9 (2)C23—C18—P1118.1 (4)
C41—Rh1—C4035.38 (18)C18—C19—C20120.7 (5)
C36—Rh1—C4094.7 (2)C18—C19—H19A119.7
C37—Rh1—P2154.47 (14)C20—C19—H19A119.7
C41—Rh1—P296.93 (14)C21—C20—C19120.1 (5)
C36—Rh1—P2169.41 (15)C21—C20—H20A120.0
C40—Rh1—P287.39 (14)C19—C20—H20A120.0
C37—Rh1—P198.48 (14)C20—C21—C22121.4 (5)
C41—Rh1—P1155.30 (14)C20—C21—H21A119.3
C36—Rh1—P189.78 (15)C22—C21—H21A119.3
C40—Rh1—P1169.31 (14)C21—C22—C23118.7 (5)
P2—Rh1—P189.94 (5)C21—C22—H22A120.7
C11—Cr1—C1088.9 (2)C23—C22—H22A120.7
C11—Cr1—C987.0 (2)C22—C23—C18121.1 (5)
C10—Cr1—C986.5 (2)C22—C23—H23A119.5
C11—Cr1—C2137.9 (2)C18—C23—H23A119.5
C10—Cr1—C288.4 (2)C29—C24—C25119.0 (5)
C9—Cr1—C2134.7 (2)C29—C24—P2117.2 (4)
C11—Cr1—C3166.4 (2)C25—C24—P2123.4 (4)
C10—Cr1—C3102.4 (2)C26—C25—C24118.8 (5)
C9—Cr1—C3101.1 (2)C26—C25—H25A120.6
C2—Cr1—C336.90 (17)C24—C25—H25A120.6
C11—Cr1—C4134.3 (2)C27—C26—C25120.8 (5)
C10—Cr1—C4135.9 (2)C27—C26—H26A119.6
C9—Cr1—C487.5 (2)C25—C26—H26A119.6
C2—Cr1—C466.04 (19)C28—C27—C26120.5 (6)
C3—Cr1—C436.70 (18)C28—C27—H27A119.8
C11—Cr1—C5101.5 (2)C26—C27—H27A119.8
C10—Cr1—C5166.4 (2)C27—C28—C29120.6 (6)
C9—Cr1—C5102.71 (19)C27—C28—H28A119.7
C2—Cr1—C578.05 (18)C29—C28—H28A119.7
C3—Cr1—C566.22 (19)C24—C29—C28120.4 (5)
C4—Cr1—C536.63 (17)C24—C29—H29A119.8
C11—Cr1—C686.73 (19)C28—C29—H29A119.8
C10—Cr1—C6136.7 (2)C35—C30—C31117.9 (5)
C9—Cr1—C6136.1 (2)C35—C30—P2118.9 (4)
C2—Cr1—C667.54 (17)C31—C30—P2122.8 (4)
C3—Cr1—C679.83 (18)C32—C31—C30120.1 (6)
C4—Cr1—C667.02 (18)C32—C31—H31A119.9
C5—Cr1—C637.03 (17)C30—C31—H31A119.9
C11—Cr1—C1103.28 (18)C33—C32—C31120.2 (6)
C10—Cr1—C1103.0 (2)C33—C32—H32A119.9
C9—Cr1—C1165.98 (19)C31—C32—H32A119.9
C2—Cr1—C137.35 (16)C34—C33—C32120.3 (5)
C3—Cr1—C167.05 (17)C34—C33—H33A119.9
C4—Cr1—C178.48 (17)C32—C33—H33A119.9
C5—Cr1—C166.22 (17)C33—C34—C35120.6 (6)
C6—Cr1—C137.42 (16)C33—C34—H34A119.7
C18—P1—C12104.5 (2)C35—C34—H34A119.7
C18—P1—C1104.4 (2)C34—C35—C30120.8 (5)
C12—P1—C1108.3 (2)C34—C35—H35A119.6
C18—P1—Rh1114.70 (15)C30—C35—H35A119.6
C12—P1—Rh1110.37 (16)C37—C36—C43127.2 (6)
C1—P1—Rh1113.84 (15)C37—C36—Rh171.2 (3)
C30—P2—C24108.9 (2)C43—C36—Rh1107.1 (4)
C30—P2—C7104.2 (2)C37—C36—H36A114.0
C24—P2—C7101.6 (2)C43—C36—H36A114.0
C30—P2—Rh1115.23 (16)Rh1—C36—H36A114.0
C24—P2—Rh1110.16 (17)C36—C37—C38125.4 (5)
C7—P2—Rh1115.62 (16)C36—C37—Rh173.0 (3)
C2—C1—C6118.3 (4)C38—C37—Rh1111.5 (3)
C2—C1—P1120.8 (3)C36—C37—H37A113.3
C6—C1—P1120.3 (3)C38—C37—H37A113.3
C2—C1—Cr169.1 (3)Rh1—C37—H37A113.3
C6—C1—Cr170.2 (3)C37—C38—C39113.6 (4)
P1—C1—Cr1140.6 (2)C37—C38—H38A108.9
C3—C2—C1122.1 (4)C39—C38—H38A108.9
C3—C2—Cr172.4 (3)C37—C38—H38B108.9
C1—C2—Cr173.5 (3)C39—C38—H38B108.9
C3—C2—H2A118.6H38A—C38—H38B107.7
C1—C2—H2A118.6C40—C39—C38112.6 (5)
Cr1—C2—H2A118.6C40—C39—H39A109.1
C2—C3—C4118.9 (4)C38—C39—H39A109.1
C2—C3—Cr170.7 (3)C40—C39—H39B109.1
C4—C3—Cr171.8 (3)C38—C39—H39B109.1
C2—C3—H3A120.1H39A—C39—H39B107.8
C4—C3—H3A120.1C41—C40—C39127.2 (5)
Cr1—C3—H3A120.1C41—C40—Rh171.7 (3)
C5—C4—C3120.5 (4)C39—C40—Rh1106.9 (3)
C5—C4—Cr171.7 (3)C41—C40—H40A114.0
C3—C4—Cr171.5 (3)C39—C40—H40A114.0
C5—C4—H4A119.2Rh1—C40—H40A114.0
C3—C4—H4A119.2C40—C41—C42125.5 (5)
Cr1—C4—H4A119.2C40—C41—Rh172.9 (3)
C4—C5—C6121.9 (4)C42—C41—Rh1111.9 (3)
C4—C5—Cr171.7 (3)C40—C41—H41A113.2
C6—C5—Cr171.6 (3)C42—C41—H41A113.2
C4—C5—H5A118.4Rh1—C41—H41A113.2
C6—C5—H5A118.4C41—C42—C43113.0 (4)
Cr1—C5—H5A118.4C41—C42—H42A109.0
C5—C6—C1118.2 (4)C43—C42—H42A109.0
C5—C6—C7120.7 (4)C41—C42—H42B109.0
C1—C6—C7121.0 (4)C43—C42—H42B109.0
C5—C6—Cr171.3 (3)H42A—C42—H42B107.8
C1—C6—Cr172.4 (3)C36—C43—C42113.2 (5)
C7—C6—Cr1130.6 (3)C36—C43—H43A108.9
C6—C7—C8113.8 (4)C42—C43—H43A108.9
C6—C7—P2107.3 (3)C36—C43—H43B108.9
C8—C7—P2114.5 (3)C42—C43—H43B108.9
C6—C7—H7A106.9H43A—C43—H43B107.7
C8—C7—H7A106.9F3—B1—F1121.8 (9)
P2—C7—H7A106.9F3—B1—F4'73.3 (8)
C7—C8—H8A109.5F1—B1—F4'122.8 (7)
C7—C8—H8B109.5F3—B1—F2102.2 (6)
H8A—C8—H8B109.5F1—B1—F2113.3 (7)
C7—C8—H8C109.5F4'—B1—F2115.9 (7)
H8A—C8—H8C109.5F3—B1—F4108.8 (8)
H8B—C8—H8C109.5F1—B1—F499.9 (7)
O1—C9—Cr1177.3 (4)F2—B1—F4110.8 (7)
O2—C10—Cr1179.1 (5)F1—B1—F3'90.0 (7)
O3—C11—Cr1179.0 (5)F4'—B1—F3'103.3 (8)
C17—C12—C13118.7 (4)F2—B1—F3'105.2 (6)
C17—C12—P1122.2 (4)F4—B1—F3'134.7 (8)
C13—C12—P1118.9 (3)C100—O100—H100109.5
C14—C13—C12120.5 (5)O100—C100—H101109.5
C14—C13—H13A119.8O100—C100—H102109.2
C12—C13—H13A119.8H101—C100—H102109.6
C15—C14—C13120.2 (5)O100—C100—H103108.8
C15—C14—H14A119.9H101—C100—H103110.0
C13—C14—H14A119.9H102—C100—H103109.7
C14—C15—C16120.3 (5)C200—O200—H200109.5
C14—C15—H15A119.9O200—C200—H201109.5
C16—C15—H15A119.9O200—C200—H202109.5
C15—C16—C17120.5 (5)H201—C200—H202109.5
C15—C16—H16A119.7O200—C200—H203109.5
C17—C16—H16A119.7H201—C200—H203109.5
C12—C17—C16119.7 (5)H202—C200—H203109.5
C12—C17—H17A120.1
C37—Rh1—P1—C180.5 (2)P1—C1—C6—Cr1137.8 (3)
C41—Rh1—P1—C1898.1 (4)C11—Cr1—C6—C5114.0 (3)
C36—Rh1—P1—C1835.3 (2)C10—Cr1—C6—C5161.1 (3)
C40—Rh1—P1—C1879.8 (8)C9—Cr1—C6—C531.7 (4)
P2—Rh1—P1—C18155.27 (17)C2—Cr1—C6—C5100.1 (3)
C37—Rh1—P1—C12117.2 (2)C3—Cr1—C6—C563.7 (3)
C41—Rh1—P1—C1219.6 (4)C4—Cr1—C6—C527.7 (3)
C36—Rh1—P1—C1282.4 (2)C1—Cr1—C6—C5129.1 (4)
C40—Rh1—P1—C12162.5 (8)C11—Cr1—C6—C1117.0 (3)
P2—Rh1—P1—C1287.03 (17)C10—Cr1—C6—C132.1 (4)
C37—Rh1—P1—C1120.8 (2)C9—Cr1—C6—C1160.8 (3)
C41—Rh1—P1—C1141.7 (4)C2—Cr1—C6—C128.9 (3)
C36—Rh1—P1—C1155.6 (2)C3—Cr1—C6—C165.3 (3)
C40—Rh1—P1—C140.4 (8)C4—Cr1—C6—C1101.4 (3)
P2—Rh1—P1—C135.04 (16)C5—Cr1—C6—C1129.1 (4)
C37—Rh1—P2—C30116.2 (4)C11—Cr1—C6—C71.0 (4)
C41—Rh1—P2—C3022.3 (2)C10—Cr1—C6—C783.9 (5)
C36—Rh1—P2—C3045.4 (9)C9—Cr1—C6—C783.2 (5)
C40—Rh1—P2—C3056.4 (2)C2—Cr1—C6—C7144.9 (5)
P1—Rh1—P2—C30133.9 (2)C3—Cr1—C6—C7178.7 (5)
C37—Rh1—P2—C247.5 (4)C4—Cr1—C6—C7142.6 (5)
C41—Rh1—P2—C24101.4 (2)C5—Cr1—C6—C7114.9 (5)
C36—Rh1—P2—C24169.2 (9)C1—Cr1—C6—C7116.0 (5)
C40—Rh1—P2—C2467.3 (2)C5—C6—C7—C820.4 (6)
P1—Rh1—P2—C24102.34 (18)C1—C6—C7—C8163.5 (4)
C37—Rh1—P2—C7122.0 (4)Cr1—C6—C7—C870.8 (6)
C41—Rh1—P2—C7144.1 (2)C5—C6—C7—P2107.3 (4)
C36—Rh1—P2—C776.3 (9)C1—C6—C7—P268.7 (5)
C40—Rh1—P2—C7178.2 (2)Cr1—C6—C7—P2161.5 (3)
P1—Rh1—P2—C712.14 (18)C30—P2—C7—C6167.3 (3)
C18—P1—C1—C23.5 (4)C24—P2—C7—C654.1 (4)
C12—P1—C1—C2114.5 (4)Rh1—P2—C7—C665.2 (3)
Rh1—P1—C1—C2122.4 (3)C30—P2—C7—C839.9 (4)
C18—P1—C1—C6174.1 (4)C24—P2—C7—C873.3 (4)
C12—P1—C1—C675.0 (4)Rh1—P2—C7—C8167.5 (3)
Rh1—P1—C1—C648.2 (4)C18—P1—C12—C1759.2 (4)
C18—P1—C1—Cr190.6 (4)C1—P1—C12—C1751.8 (5)
C12—P1—C1—Cr120.3 (4)Rh1—P1—C12—C17177.0 (4)
Rh1—P1—C1—Cr1143.5 (3)C18—P1—C12—C13116.5 (4)
C11—Cr1—C1—C2161.4 (3)C1—P1—C12—C13132.6 (4)
C10—Cr1—C1—C269.4 (3)Rh1—P1—C12—C137.3 (4)
C9—Cr1—C1—C262.3 (9)C17—C12—C13—C140.5 (7)
C3—Cr1—C1—C228.8 (3)P1—C12—C13—C14175.3 (4)
C4—Cr1—C1—C265.4 (3)C12—C13—C14—C150.4 (8)
C5—Cr1—C1—C2101.8 (3)C13—C14—C15—C160.8 (8)
C6—Cr1—C1—C2132.5 (4)C14—C15—C16—C170.3 (8)
C11—Cr1—C1—C666.1 (3)C13—C12—C17—C161.0 (7)
C10—Cr1—C1—C6158.1 (3)P1—C12—C17—C16174.7 (4)
C9—Cr1—C1—C670.2 (9)C15—C16—C17—C120.6 (8)
C2—Cr1—C1—C6132.5 (4)C12—P1—C18—C1911.9 (4)
C3—Cr1—C1—C6103.8 (3)C1—P1—C18—C19125.7 (4)
C4—Cr1—C1—C667.1 (3)Rh1—P1—C18—C19109.0 (4)
C5—Cr1—C1—C630.7 (3)C12—P1—C18—C23175.6 (4)
C11—Cr1—C1—P147.8 (4)C1—P1—C18—C2361.9 (4)
C10—Cr1—C1—P144.2 (4)Rh1—P1—C18—C2363.4 (4)
C9—Cr1—C1—P1175.9 (7)C23—C18—C19—C200.0 (7)
C2—Cr1—C1—P1113.6 (5)P1—C18—C19—C20172.5 (4)
C3—Cr1—C1—P1142.3 (4)C18—C19—C20—C211.2 (8)
C4—Cr1—C1—P1179.0 (4)C19—C20—C21—C222.4 (10)
C5—Cr1—C1—P1144.6 (4)C20—C21—C22—C232.3 (10)
C6—Cr1—C1—P1113.9 (5)C21—C22—C23—C181.1 (8)
C6—C1—C2—C34.2 (7)C19—C18—C23—C220.0 (7)
P1—C1—C2—C3166.5 (4)P1—C18—C23—C22172.9 (4)
Cr1—C1—C2—C356.2 (4)C30—P2—C24—C29146.6 (4)
C6—C1—C2—Cr151.9 (4)C7—P2—C24—C29103.8 (4)
P1—C1—C2—Cr1137.3 (3)Rh1—P2—C24—C2919.3 (4)
C11—Cr1—C2—C3160.1 (3)C30—P2—C24—C2541.2 (5)
C10—Cr1—C2—C3113.4 (3)C7—P2—C24—C2568.4 (5)
C9—Cr1—C2—C330.0 (4)Rh1—P2—C24—C25168.5 (4)
C4—Cr1—C2—C329.6 (3)C29—C24—C25—C261.8 (8)
C5—Cr1—C2—C366.1 (3)P2—C24—C25—C26170.2 (4)
C6—Cr1—C2—C3103.4 (3)C24—C25—C26—C271.2 (9)
C1—Cr1—C2—C3132.4 (4)C25—C26—C27—C280.6 (10)
C11—Cr1—C2—C127.6 (4)C26—C27—C28—C291.8 (9)
C10—Cr1—C2—C1114.2 (3)C25—C24—C29—C280.7 (7)
C9—Cr1—C2—C1162.4 (3)P2—C24—C29—C28171.8 (4)
C3—Cr1—C2—C1132.4 (4)C27—C28—C29—C241.1 (8)
C4—Cr1—C2—C1102.8 (3)C24—P2—C30—C35159.4 (4)
C5—Cr1—C2—C166.3 (3)C7—P2—C30—C3551.5 (4)
C6—Cr1—C2—C129.0 (3)Rh1—P2—C30—C3576.3 (4)
C1—C2—C3—C41.6 (7)C24—P2—C30—C3128.6 (5)
Cr1—C2—C3—C455.1 (4)C7—P2—C30—C31136.4 (4)
C1—C2—C3—Cr156.7 (4)Rh1—P2—C30—C3195.8 (4)
C11—Cr1—C3—C275.7 (10)C35—C30—C31—C322.1 (8)
C10—Cr1—C3—C270.0 (3)P2—C30—C31—C32174.3 (4)
C9—Cr1—C3—C2158.7 (3)C30—C31—C32—C330.2 (8)
C4—Cr1—C3—C2130.9 (4)C31—C32—C33—C341.7 (9)
C5—Cr1—C3—C2102.1 (3)C32—C33—C34—C350.8 (9)
C6—Cr1—C3—C265.9 (3)C33—C34—C35—C301.7 (9)
C1—Cr1—C3—C229.1 (3)C31—C30—C35—C343.1 (8)
C11—Cr1—C3—C455.2 (10)P2—C30—C35—C34175.6 (4)
C10—Cr1—C3—C4159.1 (3)C41—Rh1—C36—C3797.3 (4)
C9—Cr1—C3—C470.3 (3)C40—Rh1—C36—C3765.4 (3)
C2—Cr1—C3—C4130.9 (4)P2—Rh1—C36—C37166.6 (7)
C5—Cr1—C3—C428.8 (3)P1—Rh1—C36—C37104.9 (3)
C6—Cr1—C3—C465.0 (3)C37—Rh1—C36—C43124.3 (6)
C1—Cr1—C3—C4101.8 (3)C41—Rh1—C36—C4327.0 (4)
C2—C3—C4—C50.0 (7)C40—Rh1—C36—C4358.9 (4)
Cr1—C3—C4—C554.5 (4)P2—Rh1—C36—C4342.3 (12)
C2—C3—C4—Cr154.5 (4)P1—Rh1—C36—C43130.8 (4)
C11—Cr1—C4—C532.0 (4)C43—C36—C37—C387.1 (9)
C10—Cr1—C4—C5162.4 (3)Rh1—C36—C37—C38104.7 (5)
C9—Cr1—C4—C5115.3 (3)C43—C36—C37—Rh197.6 (6)
C2—Cr1—C4—C5102.6 (3)C41—Rh1—C37—C3677.8 (3)
C3—Cr1—C4—C5132.3 (4)C40—Rh1—C37—C36113.1 (4)
C6—Cr1—C4—C528.0 (3)P2—Rh1—C37—C36174.3 (3)
C1—Cr1—C4—C565.4 (3)P1—Rh1—C37—C3677.7 (3)
C11—Cr1—C4—C3164.3 (3)C41—Rh1—C37—C3844.2 (4)
C10—Cr1—C4—C330.0 (4)C36—Rh1—C37—C38122.0 (6)
C9—Cr1—C4—C3112.4 (3)C40—Rh1—C37—C389.0 (4)
C2—Cr1—C4—C329.8 (3)P2—Rh1—C37—C3852.3 (6)
C5—Cr1—C4—C3132.3 (4)P1—Rh1—C37—C38160.3 (4)
C6—Cr1—C4—C3104.3 (3)C36—C37—C38—C3995.7 (6)
C1—Cr1—C4—C366.9 (3)Rh1—C37—C38—C3911.7 (6)
C3—C4—C5—C61.1 (7)C37—C38—C39—C4037.8 (7)
Cr1—C4—C5—C653.3 (4)C38—C39—C40—C4136.3 (8)
C3—C4—C5—Cr154.4 (4)C38—C39—C40—Rh143.3 (5)
C11—Cr1—C5—C4157.3 (3)C37—Rh1—C40—C4196.4 (4)
C10—Cr1—C5—C463.8 (9)C36—Rh1—C40—C4163.8 (4)
C9—Cr1—C5—C467.8 (3)P2—Rh1—C40—C41105.8 (3)
C2—Cr1—C5—C465.7 (3)P1—Rh1—C40—C41178.5 (6)
C3—Cr1—C5—C428.9 (3)C37—Rh1—C40—C3928.1 (4)
C6—Cr1—C5—C4134.2 (4)C41—Rh1—C40—C39124.5 (5)
C1—Cr1—C5—C4103.1 (3)C36—Rh1—C40—C3960.7 (4)
C11—Cr1—C5—C668.6 (3)P2—Rh1—C40—C39129.7 (4)
C10—Cr1—C5—C670.4 (9)P1—Rh1—C40—C3954.1 (10)
C9—Cr1—C5—C6158.1 (3)C39—C40—C41—C427.5 (9)
C2—Cr1—C5—C668.4 (3)Rh1—C40—C41—C42105.1 (5)
C3—Cr1—C5—C6105.3 (3)C39—C40—C41—Rh197.6 (5)
C4—Cr1—C5—C6134.2 (4)C37—Rh1—C41—C4078.9 (3)
C1—Cr1—C5—C631.0 (3)C36—Rh1—C41—C40114.5 (4)
C4—C5—C6—C13.7 (7)P2—Rh1—C41—C4075.5 (3)
Cr1—C5—C6—C157.1 (4)P1—Rh1—C41—C40179.3 (3)
C4—C5—C6—C7179.9 (4)C37—Rh1—C41—C4243.1 (4)
Cr1—C5—C6—C7126.7 (4)C36—Rh1—C41—C427.6 (4)
C4—C5—C6—Cr153.3 (4)C40—Rh1—C41—C42122.0 (6)
C2—C1—C6—C55.1 (6)P2—Rh1—C41—C42162.5 (4)
P1—C1—C6—C5165.7 (3)P1—Rh1—C41—C4257.3 (6)
Cr1—C1—C6—C556.6 (4)C40—C41—C42—C4397.5 (6)
C2—C1—C6—C7178.7 (4)Rh1—C41—C42—C4313.3 (6)
P1—C1—C6—C710.5 (6)C37—C36—C43—C4235.7 (8)
Cr1—C1—C6—C7127.2 (4)Rh1—C36—C43—C4243.4 (6)
C2—C1—C6—Cr151.4 (4)C41—C42—C43—C3638.9 (7)

Experimental details

(I)(II)(III)
Crystal data
Chemical formula[Cr(C32H28P2)(CO)3][CrRh(C7H8)(C32H28P2)(CO)3]·BF4·0.75CH4O[CrRh(C8H12)(C32H28P2)(CO)3]·BF4·1.5CH4O
Mr610.51916.40956.47
Crystal system, space groupOrthorhombic, P212121Tetragonal, P43212Monoclinic, P21
Temperature (K)293110200
a, b, c (Å)10.6758 (12), 13.5533 (15), 21.255 (2)14.3886 (6), 14.3886 (6), 76.056 (4)11.262 (2), 14.116 (3), 14.226 (3)
α, β, γ (°)90, 90, 9090, 90, 9090, 107.81 (3), 90
V3)3075.4 (6)15746.0 (13)2153.2 (7)
Z4162
Radiation typeMo KαMo KαMo Kα
µ (mm1)0.510.840.77
Crystal size (mm)0.70 × 0.20 × 0.120.16 × 0.10 × 0.100.50 × 0.30 × 0.30
Data collection
DiffractometerBruker SMART APEX CCD
diffractometer
Bruker SMART APEX CCD
diffractometer
Stoe IPDS image-plate
diffractometer
Absorption correctionMulti-scan
(SADABS; Sheldrick; 1996)
Multi-scan
(SADABS; Sheldrick; 1996)
Empirical (using intensity measurements)
(ABSCOR; Stoe & Cie, 1995)
Tmin, Tmax0.717, 0.9410.878, 0.9210.700, 0.802
No. of measured, independent and
observed [I > 2σ(I)] reflections
33737, 5572, 4996 72654, 13552, 9225 11684, 6454, 5511
Rint0.0440.1050.035
(sin θ/λ)max1)0.6000.5950.581
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.042, 0.098, 1.01 0.071, 0.174, 1.02 0.034, 0.074, 0.95
No. of reflections5572135526454
No. of parameters371983532
No. of restraints093
H-atom treatmentH-atom parameters constrainedH-atom parameters constrainedH-atom parameters constrained
w = 1/[σ2(Fo2) + (0.0546P)2 + 1.0577P]
where P = (Fo2 + 2Fc2)/3
Calculated w = 1/[σ2(Fo2) + (0.0804P)2 + 29.8752P]
where P = (Fo2 + 2Fc2)/3
w = 1/[σ2(Fo2) + (0.0388P)2]
where P = (Fo2 + 2Fc2)/3
Δρmax, Δρmin (e Å3)0.33, 0.161.77, 0.900.63, 0.34
Absolute structureFlack (1983), 2430 Friedel pairsFlack (1983), 5780 Friedel pairsFlack (1983), 2773 Friedel pairs
Absolute structure parameter0.02 (2)0.01 (4)0.00 (2)

Computer programs: SMART (Bruker, 2001), EXPOSE in IPDS (Stoe & Cie, 1995), SAINT-Plus (Bruker 1999), CELL in IPDS, SAINT-Plus, INTEGRATE in IPDS, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), PLATON (Spek, 1990), XP in SHELXTL (Bruker, 1999), SHELXL97.

Selected bond distances and angles for (I) (Å, °) top
P1-C11.854 (3)P2-C81.878 (3)
Cr1-C(C6H4 ring)2.213 (4)Cr1-C(CO)1.840 (4)
C33-Cr1-C3488.3 (2)C34-Cr1-C3588.8 (2)
C35-Cr1-C3388.6 (2)
Selected distances and angles for molecule 1/molecule 2 in (II) (Å, °) top
Rh1-P12.277 (3)/2.288 (3)Rh1-P22.273 (3)/2.253 (3)
Rh1-MP12.0974 (8)/2.1141 (6)Rh1-MP22.1242 (7)/2.0962 (7)
Rh1-CC (diolefin)2.221 (10)/2.215 (9)
P1-C11.846 (11)/1.827 (9)P2-C101.851 (10)/1.865 (10)
P1-C241.810 (10)/1.823 (9)P2-C111.810 (11)/1.807 (10)
P1-C301.812 (9)/1.793 (10)P2-C171.808 (10)/1.816 (10)
Cr1-C(C6H4 ring)2.214 (11)/2.226 (10)Cr1-C(CO)1.826 (11)/1.843 (11)
P1-Rh1-P291.60 (10)/91.42 (9)MP1-Rh1-MP268.26 (3)/69.23 (2)
P1-Rh1-MP199.02 (8)/101.11 (7)P2-Rh1-MP2101.03 (7)/98.53 (7)
C2-Cr1-C387.5 (5)/85.9 (5)C3-Cr1-C486.4 (5)/87.1 (5)
C4-Cr1-C290.4 (5)/88.2 (5)
Note: MP1 and MP2 denote the midpoints of the olefinic bonds C36-C37/C78-C79 and C39-C40/C81-C82, respectively.
Selected distances and angles for (III) (Å, °) top
Rh1-P12.290 (2)Rh1-P22.279 (2)
Rh1-MP12.135 (5)Rh1-MP22.149 (5)
Rh1-CC (diolefin)2.249 (6)
P1-C11.852 (5)P2-C71.871 (5)
P1-C121.832 (5)P2-C241.815 (5)
P1-C181.823 (5)P2-C301.818 (5)
Cr1-C(C6H4 ring)2.217 (5)Cr1-C(CO)1.835 (7)
P1-Rh1-P290.0 (1)MP1-Rh1-MP284.2 (1)
P1-Rh1-MP194.4 (1)P2-Rh1-MP292.2 (1)
C9-Cr1-C1086.5 (2)C10-Cr1-C1188.9 (2)
C11-Cr1-C987.1 (2)
Comparison of characteristic torsion angles in (I)-(III) (°) top
Torsion angle(I)(II)(III)
Molecule 1/Molecule 2
Image 1-68.9 (5)-68.6 (11)/-68.5 (10)-68.9 (5)
Image 2-92.3 (2)-66.3 (8)/-56.8 (7)-54.1 (3)
Image 3-17.9 (4)-19.5 (13)/-21.4 (13)-20.0 (6)
Image 4-61.6 (2)-75.9 (9)/-83.6 (8)-75.1 (4)
 

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