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
CCDC references: 254914; 254915; 254916
(
R,
R)-Tricarbonyl{
η6-2-[1-diphenylphosphino-1-
(diphenylphosphino)ethyl]benzene}chromium(0) (I)
top
Crystal data top
[Cr(C32H28P2)(CO)3] | F(000) = 1264 |
Mr = 610.51 | Dx = 1.319 Mg m−3 |
Orthorhombic, P212121 | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: P 2ac 2ab | Cell parameters from 8096 reflections |
a = 10.6758 (12) Å | θ = 2.4–25.2° |
b = 13.5533 (15) Å | µ = 0.51 mm−1 |
c = 21.255 (2) Å | T = 293 K |
V = 3075.4 (6) Å3 | Rod, yellow |
Z = 4 | 0.70 × 0.20 × 0.12 mm |
Data collection top
Bruker SMART APEX CCD diffractometer | 5572 independent reflections |
Radiation source: fine-focus sealed tube | 4996 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.044 |
Detector resolution: 0 pixels mm-1 | θmax = 25.2°, θmin = 2.4° |
φ and ω scans | h = −12→12 |
Absorption correction: multi-scan (SADABS; Sheldrick; 1996) | k = −16→16 |
Tmin = 0.717, Tmax = 0.941 | l = −25→25 |
33737 measured reflections | |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.042 | H-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 reflections | Δρmax = 0.33 e Å−3 |
371 parameters | Δρmin = −0.16 e Å−3 |
0 restraints | Absolute structure: Flack (1983), 2430 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.02 (2) |
Special details top
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell e.s.d.'s are taken
into account individually in the estimation of e.s.d.'s in distances, angles
and torsion angles; correlations between e.s.d.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s.
planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor
wR and goodness of fit S are based on F2, conventional
R-factors R are based on F, with F set to zero for
negative F2. The threshold expression of F2 >
σ(F2) is used only for calculating R-factors(gt) etc.
and is not relevant to the choice of reflections for refinement.
R-factors based on F2 are statistically about twice as large
as those based on F, and R- factors based on ALL data will be
even larger. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Cr1 | 0.15520 (4) | 0.31365 (3) | 0.89842 (2) | 0.04051 (13) | |
P1 | 0.30442 (8) | 0.12244 (6) | 0.79891 (4) | 0.0441 (2) | |
P2 | 0.07943 (9) | −0.03049 (6) | 0.83940 (4) | 0.0511 (2) | |
C1 | 0.1711 (3) | 0.2012 (2) | 0.82331 (12) | 0.0376 (6) | |
C25 | 0.1262 (4) | 0.0865 (3) | 0.62873 (17) | 0.0614 (9) | |
H25 | 0.0409 | 0.0911 | 0.6119 | 0.080* | |
C2 | 0.1511 (3) | 0.2944 (2) | 0.79614 (13) | 0.0435 (7) | |
H2 | 0.2103 | 0.3188 | 0.7646 | 0.057* | |
C8 | 0.1061 (3) | 0.0665 (2) | 0.90104 (14) | 0.0464 (7) | |
H8 | 0.1954 | 0.0637 | 0.9117 | 0.060* | |
C26 | 0.1499 (3) | 0.1107 (2) | 0.69062 (14) | 0.0493 (7) | |
H26 | 0.0806 | 0.1321 | 0.7176 | 0.064* | |
C5 | −0.0173 (3) | 0.2257 (2) | 0.88608 (14) | 0.0437 (7) | |
H5 | −0.0785 | 0.2014 | 0.9167 | 0.057* | |
C9 | 0.1608 (4) | −0.1377 (2) | 0.87144 (16) | 0.0580 (8) | |
C27 | 0.4352 (3) | 0.2095 (2) | 0.79696 (15) | 0.0501 (8) | |
C21 | 0.2687 (3) | 0.1054 (2) | 0.71520 (14) | 0.0462 (7) | |
C6 | 0.0847 (3) | 0.1667 (2) | 0.87004 (12) | 0.0393 (6) | |
C34 | 0.2883 (3) | 0.3990 (3) | 0.8868 (2) | 0.0646 (10) | |
C4 | −0.0338 (3) | 0.3192 (2) | 0.85912 (14) | 0.0474 (7) | |
H4 | −0.1038 | 0.3608 | 0.8728 | 0.062* | |
O2 | 0.3692 (3) | 0.4521 (2) | 0.8792 (2) | 0.1073 (12) | |
O3 | 0.3038 (3) | 0.2077 (2) | 0.99631 (14) | 0.0919 (10) | |
C32 | 0.4675 (3) | 0.2694 (3) | 0.74669 (19) | 0.0644 (10) | |
H32 | 0.4148 | 0.2696 | 0.7089 | 0.084* | |
C15 | −0.0860 (4) | −0.0570 (3) | 0.85191 (17) | 0.0610 (9) | |
C30 | 0.6473 (4) | 0.3297 (4) | 0.8006 (3) | 0.0940 (15) | |
H30 | 0.7220 | 0.3718 | 0.8017 | 0.122* | |
O1 | 0.0586 (3) | 0.4493 (3) | 0.99766 (16) | 0.1090 (12) | |
C20 | −0.1687 (5) | 0.0038 (3) | 0.8204 (2) | 0.0838 (13) | |
H20 | −0.1362 | 0.0541 | 0.7916 | 0.109* | |
C14 | 0.1412 (4) | −0.2279 (3) | 0.8424 (2) | 0.0832 (13) | |
H14 | 0.0783 | −0.2333 | 0.8090 | 0.108* | |
C28 | 0.5121 (3) | 0.2105 (3) | 0.84998 (18) | 0.0661 (10) | |
H28 | 0.4923 | 0.1686 | 0.8862 | 0.086* | |
C23 | 0.3410 (4) | 0.0515 (4) | 0.61445 (18) | 0.0832 (13) | |
H23 | 0.4099 | 0.0307 | 0.5870 | 0.108* | |
C16 | −0.1340 (4) | −0.1299 (4) | 0.8918 (2) | 0.0846 (12) | |
H16 | −0.0767 | −0.1752 | 0.9134 | 0.110* | |
C22 | 0.3658 (4) | 0.0757 (3) | 0.67595 (18) | 0.0704 (11) | |
H22 | 0.4516 | 0.0720 | 0.6921 | 0.092* | |
C12 | 0.2976 (6) | −0.3040 (4) | 0.9058 (3) | 0.1051 (16) | |
H12 | 0.3426 | −0.3632 | 0.9194 | 0.137* | |
C24 | 0.2225 (4) | 0.0560 (3) | 0.59094 (17) | 0.0716 (11) | |
H24 | 0.2062 | 0.0374 | 0.5471 | 0.093* | |
C17 | −0.2613 (5) | −0.1383 (5) | 0.9009 (3) | 0.1145 (19) | |
H17 | −0.2944 | −0.1888 | 0.9294 | 0.149* | |
C11 | 0.3237 (6) | −0.2154 (4) | 0.9330 (3) | 0.1120 (19) | |
H11 | 0.3902 | −0.2102 | 0.9646 | 0.146* | |
C13 | 0.2094 (5) | −0.3109 (4) | 0.8598 (3) | 0.1065 (17) | |
H13 | 0.1939 | −0.3742 | 0.8390 | 0.138* | |
C7 | 0.0346 (4) | 0.0511 (3) | 0.96275 (15) | 0.0653 (10) | |
H7A | 0.0593 | 0.1020 | 0.9931 | 0.085* | |
H7B | 0.0544 | −0.0142 | 0.9799 | 0.085* | |
H7C | −0.0556 | 0.0557 | 0.9548 | 0.085* | |
C31 | 0.5720 (4) | 0.3288 (4) | 0.7486 (2) | 0.0834 (13) | |
H31 | 0.5926 | 0.3707 | 0.7125 | 0.108* | |
C29 | 0.6176 (4) | 0.2714 (4) | 0.8511 (2) | 0.0888 (15) | |
H29 | 0.6712 | 0.2725 | 0.8886 | 0.115* | |
C33 | 0.0964 (4) | 0.3977 (3) | 0.96015 (18) | 0.0653 (10) | |
C10 | 0.2559 (5) | −0.1326 (3) | 0.9158 (2) | 0.0876 (14) | |
H10 | 0.2756 | −0.0690 | 0.9354 | 0.114* | |
C18 | −0.3410 (5) | −0.0767 (6) | 0.8702 (4) | 0.125 (3) | |
H18 | −0.4313 | −0.0827 | 0.8774 | 0.162* | |
C19 | −0.2968 (6) | −0.0051 (5) | 0.8288 (3) | 0.119 (2) | |
H19 | −0.3551 | 0.0380 | 0.8061 | 0.154* | |
C3 | 0.0483 (3) | 0.3535 (2) | 0.81309 (14) | 0.0483 (8) | |
H3 | 0.0346 | 0.4176 | 0.7929 | 0.063* | |
C35 | 0.2468 (4) | 0.2495 (3) | 0.95873 (16) | 0.0577 (9) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Cr1 | 0.0371 (2) | 0.0421 (2) | 0.0423 (2) | 0.0015 (2) | −0.0030 (2) | −0.0088 (2) |
P1 | 0.0438 (4) | 0.0480 (4) | 0.0405 (4) | 0.0112 (3) | 0.0011 (3) | −0.0023 (3) |
P2 | 0.0664 (6) | 0.0450 (4) | 0.0421 (4) | −0.0007 (4) | −0.0013 (4) | −0.0019 (4) |
C1 | 0.0376 (15) | 0.0421 (15) | 0.0331 (13) | 0.0012 (13) | −0.0025 (11) | −0.0025 (12) |
C25 | 0.069 (2) | 0.064 (2) | 0.051 (2) | 0.0041 (18) | −0.0057 (17) | −0.0020 (16) |
C2 | 0.0442 (16) | 0.0469 (17) | 0.0393 (15) | 0.0028 (14) | 0.0010 (14) | 0.0003 (12) |
C8 | 0.0576 (18) | 0.0445 (15) | 0.0371 (15) | −0.0014 (14) | −0.0002 (15) | −0.0035 (13) |
C26 | 0.0521 (18) | 0.0531 (17) | 0.0427 (16) | 0.0064 (16) | 0.0030 (15) | −0.0043 (14) |
C5 | 0.0356 (15) | 0.0535 (17) | 0.0421 (17) | −0.0052 (13) | 0.0013 (13) | −0.0094 (13) |
C9 | 0.065 (2) | 0.0508 (19) | 0.058 (2) | 0.0013 (18) | 0.0099 (19) | −0.0009 (15) |
C27 | 0.0391 (16) | 0.061 (2) | 0.0501 (17) | 0.0131 (15) | 0.0001 (14) | −0.0101 (15) |
C21 | 0.0530 (19) | 0.0452 (17) | 0.0405 (16) | 0.0036 (14) | 0.0056 (14) | −0.0037 (13) |
C6 | 0.0434 (16) | 0.0427 (16) | 0.0319 (13) | −0.0010 (13) | −0.0057 (13) | −0.0056 (11) |
C34 | 0.053 (2) | 0.056 (2) | 0.086 (3) | −0.0014 (17) | −0.003 (2) | −0.0134 (19) |
C4 | 0.0364 (15) | 0.0546 (18) | 0.0510 (17) | 0.0116 (15) | −0.0071 (13) | −0.0130 (15) |
O2 | 0.0719 (19) | 0.076 (2) | 0.174 (4) | −0.0332 (17) | 0.018 (2) | −0.019 (2) |
O3 | 0.099 (2) | 0.098 (2) | 0.0788 (18) | 0.0108 (19) | −0.0464 (17) | 0.0023 (17) |
C32 | 0.045 (2) | 0.078 (2) | 0.069 (2) | −0.0001 (18) | 0.0003 (17) | 0.0061 (19) |
C15 | 0.067 (2) | 0.061 (2) | 0.056 (2) | −0.0007 (19) | −0.0036 (18) | −0.0199 (17) |
C30 | 0.051 (2) | 0.105 (4) | 0.126 (4) | −0.008 (3) | −0.012 (3) | 0.005 (3) |
O1 | 0.112 (3) | 0.120 (3) | 0.095 (2) | 0.016 (2) | 0.003 (2) | −0.064 (2) |
C20 | 0.083 (3) | 0.076 (3) | 0.092 (3) | 0.019 (2) | −0.019 (3) | −0.031 (2) |
C14 | 0.072 (3) | 0.054 (2) | 0.124 (4) | 0.000 (2) | −0.010 (3) | −0.011 (2) |
C28 | 0.049 (2) | 0.085 (3) | 0.065 (2) | 0.0112 (19) | −0.0091 (17) | −0.005 (2) |
C23 | 0.083 (3) | 0.117 (4) | 0.050 (2) | 0.018 (3) | 0.016 (2) | −0.021 (2) |
C16 | 0.071 (3) | 0.086 (3) | 0.096 (3) | −0.010 (2) | 0.012 (3) | −0.006 (3) |
C22 | 0.056 (2) | 0.096 (3) | 0.059 (2) | 0.018 (2) | 0.0088 (18) | −0.014 (2) |
C12 | 0.111 (4) | 0.068 (3) | 0.136 (5) | 0.032 (3) | −0.005 (4) | 0.012 (3) |
C24 | 0.096 (3) | 0.080 (3) | 0.0380 (18) | 0.004 (2) | 0.002 (2) | −0.0108 (18) |
C17 | 0.078 (3) | 0.124 (4) | 0.141 (5) | −0.028 (3) | 0.023 (4) | −0.032 (4) |
C11 | 0.148 (5) | 0.086 (4) | 0.102 (4) | 0.044 (4) | −0.027 (4) | 0.007 (3) |
C13 | 0.090 (3) | 0.057 (3) | 0.172 (5) | 0.008 (3) | 0.007 (4) | −0.017 (3) |
C7 | 0.100 (3) | 0.059 (2) | 0.0369 (17) | −0.003 (2) | 0.0060 (18) | 0.0014 (15) |
C31 | 0.051 (2) | 0.100 (3) | 0.100 (3) | −0.008 (2) | 0.005 (2) | 0.015 (3) |
C29 | 0.052 (2) | 0.119 (4) | 0.095 (3) | 0.000 (2) | −0.026 (2) | −0.012 (3) |
C33 | 0.066 (2) | 0.072 (2) | 0.058 (2) | 0.006 (2) | −0.0049 (19) | −0.0311 (19) |
C10 | 0.121 (4) | 0.067 (3) | 0.074 (3) | 0.028 (3) | −0.020 (3) | −0.009 (2) |
C18 | 0.061 (3) | 0.152 (6) | 0.161 (6) | −0.004 (4) | 0.003 (4) | −0.084 (5) |
C19 | 0.085 (4) | 0.110 (4) | 0.162 (6) | 0.035 (3) | −0.040 (4) | −0.069 (4) |
C3 | 0.0536 (19) | 0.0444 (17) | 0.0469 (17) | 0.0082 (15) | −0.0062 (15) | 0.0026 (13) |
C35 | 0.062 (2) | 0.062 (2) | 0.050 (2) | −0.0039 (18) | −0.0149 (18) | −0.0099 (16) |
Geometric parameters (Å, º) top
Cr1—C35 | 1.832 (4) | C32—C31 | 1.376 (5) |
Cr1—C33 | 1.847 (3) | C32—H32 | 0.9800 |
Cr1—C34 | 1.849 (4) | C15—C20 | 1.381 (6) |
Cr1—C4 | 2.186 (3) | C15—C16 | 1.399 (6) |
Cr1—C2 | 2.190 (3) | C30—C31 | 1.366 (6) |
Cr1—C3 | 2.210 (3) | C30—C29 | 1.371 (7) |
Cr1—C5 | 2.209 (3) | C30—H30 | 0.9800 |
Cr1—C1 | 2.214 (3) | O1—C33 | 1.135 (4) |
Cr1—C6 | 2.213 (3) | C20—C19 | 1.384 (8) |
P1—C27 | 1.828 (4) | C20—H20 | 0.9800 |
P1—C21 | 1.834 (3) | C14—C13 | 1.389 (7) |
P1—C1 | 1.854 (3) | C14—H14 | 0.9800 |
P2—C15 | 1.822 (4) | C28—C29 | 1.397 (6) |
P2—C9 | 1.825 (4) | C28—H28 | 0.9800 |
P2—C8 | 1.878 (3) | C23—C24 | 1.362 (6) |
C1—C2 | 1.405 (4) | C23—C22 | 1.373 (5) |
C1—C6 | 1.434 (4) | C23—H23 | 0.9800 |
C25—C24 | 1.369 (5) | C16—C17 | 1.377 (6) |
C25—C26 | 1.379 (5) | C16—H16 | 0.9800 |
C25—H25 | 0.9800 | C22—H22 | 0.9800 |
C2—C3 | 1.406 (4) | C12—C13 | 1.360 (7) |
C2—H2 | 0.9800 | C12—C11 | 1.362 (7) |
C8—C6 | 1.526 (4) | C12—H12 | 0.9800 |
C8—C7 | 1.532 (4) | C24—H24 | 0.9800 |
C8—H8 | 0.9800 | C17—C18 | 1.359 (9) |
C26—C21 | 1.374 (5) | C17—H17 | 0.9800 |
C26—H26 | 0.9800 | C11—C10 | 1.383 (6) |
C5—C6 | 1.392 (4) | C11—H11 | 0.9800 |
C5—C4 | 1.402 (4) | C13—H13 | 0.9800 |
C5—H5 | 0.9800 | C7—H7A | 0.9801 |
C9—C14 | 1.386 (5) | C7—H7B | 0.9801 |
C9—C10 | 1.387 (6) | C7—H7C | 0.9801 |
C27—C32 | 1.386 (5) | C31—H31 | 0.9800 |
C27—C28 | 1.395 (5) | C29—H29 | 0.9800 |
C21—C22 | 1.390 (5) | C10—H10 | 0.9800 |
C34—O2 | 1.136 (4) | C18—C19 | 1.392 (9) |
C4—C3 | 1.394 (4) | C18—H18 | 0.9800 |
C4—H4 | 0.9800 | C19—H19 | 0.9800 |
O3—C35 | 1.153 (4) | C3—H3 | 0.9800 |
| | | |
C35—Cr1—C33 | 88.68 (17) | C1—C6—C8 | 119.5 (3) |
C35—Cr1—C34 | 88.86 (17) | C5—C6—Cr1 | 71.50 (16) |
C33—Cr1—C34 | 88.32 (17) | C1—C6—Cr1 | 71.12 (15) |
C35—Cr1—C4 | 140.98 (15) | C8—C6—Cr1 | 129.18 (19) |
C33—Cr1—C4 | 86.34 (14) | O2—C34—Cr1 | 179.2 (4) |
C34—Cr1—C4 | 129.57 (16) | C3—C4—C5 | 120.6 (3) |
C35—Cr1—C2 | 130.44 (14) | C3—C4—Cr1 | 72.47 (18) |
C33—Cr1—C2 | 140.52 (15) | C5—C4—Cr1 | 72.31 (17) |
C34—Cr1—C2 | 87.56 (15) | C3—C4—H4 | 119.7 |
C4—Cr1—C2 | 66.81 (11) | C5—C4—H4 | 119.7 |
C35—Cr1—C3 | 165.03 (13) | Cr1—C4—H4 | 127.6 |
C33—Cr1—C3 | 104.87 (15) | C31—C32—C27 | 121.4 (4) |
C34—Cr1—C3 | 97.71 (16) | C31—C32—H32 | 119.3 |
C4—Cr1—C3 | 36.97 (12) | C27—C32—H32 | 119.3 |
C2—Cr1—C3 | 37.27 (11) | C20—C15—C16 | 118.8 (4) |
C35—Cr1—C5 | 105.78 (14) | C20—C15—P2 | 115.6 (3) |
C33—Cr1—C5 | 97.68 (15) | C16—C15—P2 | 125.6 (3) |
C34—Cr1—C5 | 164.22 (15) | C31—C30—C29 | 119.5 (4) |
C4—Cr1—C5 | 37.21 (12) | C31—C30—H30 | 120.3 |
C2—Cr1—C5 | 78.52 (11) | C29—C30—H30 | 120.3 |
C3—Cr1—C5 | 66.67 (12) | C15—C20—C19 | 121.1 (5) |
C35—Cr1—C1 | 97.88 (13) | C15—C20—H20 | 119.4 |
C33—Cr1—C1 | 164.28 (15) | C19—C20—H20 | 119.4 |
C34—Cr1—C1 | 106.00 (14) | C9—C14—C13 | 121.1 (5) |
C4—Cr1—C1 | 79.55 (11) | C9—C14—H14 | 119.5 |
C2—Cr1—C1 | 37.20 (10) | C13—C14—H14 | 119.5 |
C3—Cr1—C1 | 67.41 (11) | C27—C28—C29 | 119.6 (4) |
C5—Cr1—C1 | 66.83 (10) | C27—C28—H28 | 120.2 |
C35—Cr1—C6 | 86.87 (13) | C29—C28—H28 | 120.2 |
C33—Cr1—C6 | 129.24 (15) | C24—C23—C22 | 121.2 (4) |
C34—Cr1—C6 | 142.02 (14) | C24—C23—H23 | 119.4 |
C4—Cr1—C6 | 67.20 (11) | C22—C23—H23 | 119.4 |
C2—Cr1—C6 | 67.37 (11) | C17—C16—C15 | 120.3 (5) |
C3—Cr1—C6 | 79.66 (11) | C17—C16—H16 | 119.9 |
C5—Cr1—C6 | 36.70 (10) | C15—C16—H16 | 119.9 |
C1—Cr1—C6 | 37.80 (10) | C23—C22—C21 | 119.8 (4) |
C27—P1—C21 | 102.60 (15) | C23—C22—H22 | 120.1 |
C27—P1—C1 | 102.77 (13) | C21—C22—H22 | 120.1 |
C21—P1—C1 | 100.63 (13) | C13—C12—C11 | 120.4 (5) |
C15—P2—C9 | 104.50 (18) | C13—C12—H12 | 119.8 |
C15—P2—C8 | 100.55 (15) | C11—C12—H12 | 119.8 |
C9—P2—C8 | 102.99 (15) | C23—C24—C25 | 119.7 (3) |
C2—C1—C6 | 118.7 (3) | C23—C24—H24 | 120.1 |
C2—C1—P1 | 121.3 (2) | C25—C24—H24 | 120.1 |
C6—C1—P1 | 120.0 (2) | C18—C17—C16 | 120.0 (6) |
C2—C1—Cr1 | 70.49 (16) | C18—C17—H17 | 120.0 |
C6—C1—Cr1 | 71.08 (15) | C16—C17—H17 | 120.0 |
P1—C1—Cr1 | 131.08 (14) | C12—C11—C10 | 119.7 (5) |
C24—C25—C26 | 119.6 (4) | C12—C11—H11 | 120.1 |
C24—C25—H25 | 120.2 | C10—C11—H11 | 120.1 |
C26—C25—H25 | 120.2 | C12—C13—C14 | 119.9 (5) |
C1—C2—C3 | 121.7 (3) | C12—C13—H13 | 120.0 |
C1—C2—Cr1 | 72.31 (16) | C14—C13—H13 | 120.0 |
C3—C2—Cr1 | 72.14 (17) | C8—C7—H7A | 109.5 |
C1—C2—H2 | 119.1 | C8—C7—H7B | 109.5 |
C3—C2—H2 | 119.1 | H7A—C7—H7B | 109.5 |
Cr1—C2—H2 | 128.8 | C8—C7—H7C | 109.5 |
C6—C8—C7 | 114.6 (3) | H7A—C7—H7C | 109.5 |
C6—C8—P2 | 107.39 (19) | H7B—C7—H7C | 109.5 |
C7—C8—P2 | 115.2 (2) | C30—C31—C32 | 120.5 (4) |
C6—C8—H8 | 106.3 | C30—C31—H31 | 119.8 |
C7—C8—H8 | 106.3 | C32—C31—H31 | 119.8 |
P2—C8—H8 | 106.3 | C30—C29—C28 | 120.9 (4) |
C21—C26—C25 | 121.3 (3) | C30—C29—H29 | 119.5 |
C21—C26—H26 | 119.3 | C28—C29—H29 | 119.5 |
C25—C26—H26 | 119.3 | O1—C33—Cr1 | 179.0 (4) |
C6—C5—C4 | 121.2 (3) | C11—C10—C9 | 121.5 (4) |
C6—C5—Cr1 | 71.80 (16) | C11—C10—H10 | 119.3 |
C4—C5—Cr1 | 70.47 (17) | C9—C10—H10 | 119.3 |
C6—C5—H5 | 119.4 | C17—C18—C19 | 121.3 (6) |
C4—C5—H5 | 119.4 | C17—C18—H18 | 119.3 |
Cr1—C5—H5 | 131.2 | C19—C18—H18 | 119.3 |
C14—C9—C10 | 117.2 (4) | C20—C19—C18 | 118.5 (6) |
C14—C9—P2 | 117.7 (3) | C20—C19—H19 | 120.8 |
C10—C9—P2 | 124.3 (3) | C18—C19—H19 | 120.8 |
C32—C27—C28 | 118.1 (3) | C4—C3—C2 | 118.7 (3) |
C32—C27—P1 | 125.9 (3) | C4—C3—Cr1 | 70.57 (17) |
C28—C27—P1 | 115.9 (3) | C2—C3—Cr1 | 70.60 (17) |
C26—C21—C22 | 118.4 (3) | C4—C3—H3 | 120.6 |
C26—C21—P1 | 123.7 (2) | C2—C3—H3 | 120.6 |
C22—C21—P1 | 117.6 (3) | Cr1—C3—H3 | 130.7 |
C5—C6—C1 | 119.0 (3) | O3—C35—Cr1 | 178.9 (3) |
C5—C6—C8 | 121.5 (3) | | |
| | | |
C27—P1—C1—C2 | 45.1 (3) | C1—P1—C27—C32 | −85.6 (3) |
C21—P1—C1—C2 | −60.6 (3) | C21—P1—C27—C28 | −157.7 (3) |
C27—P1—C1—C6 | −135.9 (2) | C1—P1—C27—C28 | 98.1 (3) |
C21—P1—C1—C6 | 118.4 (2) | C25—C26—C21—C22 | 0.6 (5) |
C27—P1—C1—Cr1 | −45.5 (2) | C25—C26—C21—P1 | −172.7 (3) |
C21—P1—C1—Cr1 | −151.21 (19) | C27—P1—C21—C26 | −131.8 (3) |
C35—Cr1—C1—C2 | −154.3 (2) | C1—P1—C21—C26 | −26.0 (3) |
C33—Cr1—C1—C2 | 91.8 (6) | C27—P1—C21—C22 | 54.9 (3) |
C34—Cr1—C1—C2 | −63.2 (2) | C1—P1—C21—C22 | 160.7 (3) |
C4—Cr1—C1—C2 | 65.20 (19) | C4—C5—C6—C1 | −2.4 (4) |
C5—Cr1—C1—C2 | 101.88 (19) | Cr1—C5—C6—C1 | −54.8 (2) |
C3—Cr1—C1—C2 | 28.65 (18) | C4—C5—C6—C8 | 177.6 (3) |
C6—Cr1—C1—C2 | 131.3 (2) | Cr1—C5—C6—C8 | 125.2 (3) |
C35—Cr1—C1—C6 | 74.4 (2) | C4—C5—C6—Cr1 | 52.4 (2) |
C33—Cr1—C1—C6 | −39.5 (6) | C2—C1—C6—C5 | 1.2 (4) |
C34—Cr1—C1—C6 | 165.51 (19) | P1—C1—C6—C5 | −177.8 (2) |
C4—Cr1—C1—C6 | −66.10 (17) | Cr1—C1—C6—C5 | 55.0 (2) |
C2—Cr1—C1—C6 | −131.3 (2) | C2—C1—C6—C8 | −178.8 (2) |
C5—Cr1—C1—C6 | −29.42 (16) | P1—C1—C6—C8 | 2.2 (3) |
C3—Cr1—C1—C6 | −102.66 (18) | Cr1—C1—C6—C8 | −125.0 (2) |
C35—Cr1—C1—P1 | −39.3 (2) | C2—C1—C6—Cr1 | −53.8 (2) |
C33—Cr1—C1—P1 | −153.3 (5) | P1—C1—C6—Cr1 | 127.17 (19) |
C34—Cr1—C1—P1 | 51.8 (2) | C7—C8—C6—C5 | −17.9 (4) |
C4—Cr1—C1—P1 | −179.8 (2) | P2—C8—C6—C5 | 111.5 (3) |
C2—Cr1—C1—P1 | 115.0 (3) | C7—C8—C6—C1 | 162.1 (3) |
C5—Cr1—C1—P1 | −143.2 (2) | P2—C8—C6—C1 | −68.5 (3) |
C3—Cr1—C1—P1 | 143.6 (2) | C7—C8—C6—Cr1 | 73.2 (4) |
C6—Cr1—C1—P1 | −113.7 (3) | P2—C8—C6—Cr1 | −157.43 (17) |
C6—C1—C2—C3 | −0.8 (4) | C6—C5—C4—C3 | 3.2 (4) |
P1—C1—C2—C3 | 178.2 (2) | Cr1—C5—C4—C3 | 56.2 (3) |
Cr1—C1—C2—C3 | −54.9 (3) | C6—C5—C4—Cr1 | −53.0 (2) |
C6—C1—C2—Cr1 | 54.1 (2) | C28—C27—C32—C31 | −0.3 (5) |
P1—C1—C2—Cr1 | −126.90 (19) | P1—C27—C32—C31 | −176.4 (3) |
C35—Cr1—C2—C1 | 34.4 (3) | C9—P2—C15—C20 | −167.4 (3) |
C33—Cr1—C2—C1 | −154.8 (2) | C8—P2—C15—C20 | 86.0 (3) |
C34—Cr1—C2—C1 | 120.8 (2) | C9—P2—C15—C16 | 15.0 (4) |
C4—Cr1—C2—C1 | −103.8 (2) | C8—P2—C15—C16 | −91.5 (4) |
C5—Cr1—C2—C1 | −66.63 (18) | C16—C15—C20—C19 | 1.4 (6) |
C3—Cr1—C2—C1 | −133.0 (3) | P2—C15—C20—C19 | −176.3 (4) |
C6—Cr1—C2—C1 | −29.92 (16) | C10—C9—C14—C13 | 3.7 (7) |
C35—Cr1—C2—C3 | 167.4 (2) | P2—C9—C14—C13 | 173.4 (4) |
C33—Cr1—C2—C3 | −21.8 (3) | C32—C27—C28—C29 | 0.4 (5) |
C34—Cr1—C2—C3 | −106.1 (2) | P1—C27—C28—C29 | 176.9 (3) |
C4—Cr1—C2—C3 | 29.25 (19) | C20—C15—C16—C17 | −2.1 (7) |
C5—Cr1—C2—C3 | 66.40 (19) | P2—C15—C16—C17 | 175.3 (4) |
C6—Cr1—C2—C3 | 103.1 (2) | C24—C23—C22—C21 | −0.1 (7) |
C1—Cr1—C2—C3 | 133.0 (3) | C26—C21—C22—C23 | −0.7 (6) |
C15—P2—C8—C6 | −92.3 (2) | P1—C21—C22—C23 | 172.9 (4) |
C9—P2—C8—C6 | 160.0 (2) | C22—C23—C24—C25 | 1.0 (7) |
C15—P2—C8—C7 | 36.7 (3) | C26—C25—C24—C23 | −1.2 (6) |
C9—P2—C8—C7 | −71.0 (3) | C15—C16—C17—C18 | 1.0 (8) |
C24—C25—C26—C21 | 0.4 (6) | C13—C12—C11—C10 | 3.0 (9) |
C35—Cr1—C5—C6 | −61.7 (2) | C11—C12—C13—C14 | −3.0 (9) |
C33—Cr1—C5—C6 | −152.5 (2) | C9—C14—C13—C12 | −0.5 (8) |
C34—Cr1—C5—C6 | 95.9 (5) | C29—C30—C31—C32 | −0.4 (7) |
C4—Cr1—C5—C6 | 134.0 (3) | C27—C32—C31—C30 | 0.2 (7) |
C2—Cr1—C5—C6 | 67.38 (17) | C31—C30—C29—C28 | 0.6 (8) |
C3—Cr1—C5—C6 | 104.55 (19) | C27—C28—C29—C30 | −0.6 (6) |
C1—Cr1—C5—C6 | 30.25 (16) | C12—C11—C10—C9 | 0.4 (9) |
C35—Cr1—C5—C4 | 164.31 (19) | C14—C9—C10—C11 | −3.6 (7) |
C33—Cr1—C5—C4 | 73.5 (2) | P2—C9—C10—C11 | −172.5 (4) |
C34—Cr1—C5—C4 | −38.1 (5) | C16—C17—C18—C19 | 0.8 (9) |
C2—Cr1—C5—C4 | −66.61 (18) | C15—C20—C19—C18 | 0.3 (8) |
C3—Cr1—C5—C4 | −29.43 (17) | C17—C18—C19—C20 | −1.5 (9) |
C6—Cr1—C5—C4 | −134.0 (3) | C5—C4—C3—C2 | −2.7 (4) |
C1—Cr1—C5—C4 | −103.74 (18) | Cr1—C4—C3—C2 | 53.5 (3) |
C15—P2—C9—C14 | 64.3 (4) | C5—C4—C3—Cr1 | −56.2 (2) |
C8—P2—C9—C14 | 169.0 (3) | C1—C2—C3—C4 | 1.5 (4) |
C15—P2—C9—C10 | −126.8 (4) | Cr1—C2—C3—C4 | −53.5 (3) |
C8—P2—C9—C10 | −22.1 (4) | C1—C2—C3—Cr1 | 54.9 (3) |
C21—P1—C27—C32 | 18.5 (3) | | |
(
R,
R)-tricarbonyl-1
κ3C-{µ-1(
η6):2
κ2P,
P'-1-(diphenylphosphino)-2-[1-
(diphenylphosphino)ethyl]benzene}[2(
η4)-norbornadiene]chromium(0)rhodium(I)
tetrafluoroborate methanol 0.75-solvate (II)
top
Crystal data top
[CrRh(C7H8)(C32H28P2)(CO)3]·BF4·0.75CH4O | Dx = 1.546 Mg m−3 |
Mr = 916.40 | Mo Kα radiation, λ = 0.71073 Å |
Tetragonal, P43212 | Cell parameters from 8096 reflections |
Hall symbol: P 4nw 2abw | θ = 1.5–25.0° |
a = 14.3886 (6) Å | µ = 0.84 mm−1 |
c = 76.056 (4) Å | T = 110 K |
V = 15746.0 (13) Å3 | Fragment, red |
Z = 16 | 0.16 × 0.10 × 0.10 mm |
F(000) = 7448 | |
Data collection top
Bruker SMART APEX CCD diffractometer | 13552 independent reflections |
Radiation source: fine-focus sealed tube | 9225 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.105 |
Detector resolution: 0 pixels mm-1 | θmax = 25.0°, θmin = 1.5° |
φ and ω scans | h = −17→16 |
Absorption correction: multi-scan (SADABS; Sheldrick; 1996) | k = −16→17 |
Tmin = 0.878, Tmax = 0.921 | l = −85→70 |
72654 measured reflections | |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.071 | H-atom parameters constrained |
wR(F2) = 0.174 | Calculated w = 1/[σ2(Fo2) + (0.0804P)2 + 29.8752P] where P = (Fo2 + 2Fc2)/3 |
S = 1.02 | (Δ/σ)max = 0.001 |
13552 reflections | Δρmax = 1.77 e Å−3 |
983 parameters | Δρmin = −0.90 e Å−3 |
9 restraints | Absolute structure: Flack (1983), 5780 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: −0.01 (4) |
Special details top
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell e.s.d.'s are taken
into account individually in the estimation of e.s.d.'s in distances, angles
and torsion angles; correlations between e.s.d.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s.
planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor
wR and goodness of fit S are based on F2, conventional
R-factors R are based on F, with F set to zero for
negative F2. The threshold expression of F2 >
σ(F2) is used only for calculating R-factors(gt) etc.
and is not relevant to the choice of reflections for refinement.
R-factors based on F2 are statistically about twice as large
as those based on F, and R- factors based on ALL data will be
even larger. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Rh1 | 0.22302 (6) | 0.77146 (6) | −0.011497 (10) | 0.0312 (2) | |
Cr1 | 0.51228 (12) | 0.76647 (12) | 0.03666 (2) | 0.0329 (4) | |
P1 | 0.2699 (2) | 0.76309 (18) | 0.01705 (4) | 0.0320 (7) | |
P2 | 0.3574 (2) | 0.84285 (19) | −0.01953 (3) | 0.0301 (7) | |
O1 | 0.4793 (5) | 0.9689 (5) | 0.04294 (10) | 0.0438 (19) | |
O2 | 0.6970 (6) | 0.7915 (6) | 0.05386 (10) | 0.053 (2) | |
O3 | 0.4427 (5) | 0.7224 (6) | 0.07218 (10) | 0.048 (2) | |
C1 | 0.3953 (8) | 0.7375 (7) | 0.01877 (13) | 0.035 (3) | |
C2 | 0.4911 (7) | 0.8895 (8) | 0.04061 (13) | 0.033 (3) | |
C3 | 0.6271 (8) | 0.7826 (8) | 0.04724 (13) | 0.038 (3) | |
C4 | 0.4691 (7) | 0.7387 (8) | 0.05834 (15) | 0.035 (3) | |
C5 | 0.4614 (8) | 0.7890 (7) | 0.00914 (14) | 0.035 (3) | |
C6 | 0.5543 (8) | 0.7590 (8) | 0.00845 (14) | 0.043 (3) | |
H6 | 0.5981 | 0.7931 | 0.0022 | 0.051* | |
C7 | 0.5812 (9) | 0.6766 (9) | 0.01733 (13) | 0.051 (4) | |
H7 | 0.6435 | 0.6592 | 0.0172 | 0.062* | |
C8 | 0.5162 (9) | 0.6197 (8) | 0.02642 (15) | 0.047 (3) | |
H8 | 0.5331 | 0.5632 | 0.0314 | 0.056* | |
C9 | 0.4276 (8) | 0.6529 (7) | 0.02732 (13) | 0.037 (3) | |
H9 | 0.3847 | 0.6192 | 0.0339 | 0.045* | |
C10 | 0.4325 (7) | 0.8756 (6) | −0.00077 (13) | 0.028 (2) | |
H10 | 0.3930 | 0.9110 | 0.0073 | 0.034* | |
C11 | 0.4293 (8) | 0.7777 (7) | −0.03467 (13) | 0.037 (3) | |
C12 | 0.4081 (7) | 0.6844 (7) | −0.03731 (14) | 0.038 (3) | |
H12 | 0.3630 | 0.6555 | −0.0305 | 0.046* | |
C13 | 0.4557 (9) | 0.6340 (8) | −0.05045 (14) | 0.049 (4) | |
H13 | 0.4408 | 0.5721 | −0.0526 | 0.058* | |
C14 | 0.5244 (9) | 0.6772 (10) | −0.06001 (15) | 0.050 (3) | |
H14 | 0.5565 | 0.6439 | −0.0685 | 0.060* | |
C15 | 0.5462 (8) | 0.7685 (9) | −0.05715 (14) | 0.045 (3) | |
H15 | 0.5931 | 0.7969 | −0.0636 | 0.054* | |
C16 | 0.4973 (7) | 0.8190 (7) | −0.04439 (13) | 0.035 (3) | |
H16 | 0.5113 | 0.8813 | −0.0425 | 0.042* | |
C17 | 0.3307 (7) | 0.9495 (7) | −0.03106 (13) | 0.028 (2) | |
C18 | 0.3075 (7) | 1.0289 (8) | −0.02219 (15) | 0.038 (3) | |
H18 | 0.3119 | 1.0310 | −0.0100 | 0.046* | |
C19 | 0.2767 (8) | 1.1073 (8) | −0.03162 (19) | 0.052 (3) | |
H19 | 0.2605 | 1.1608 | −0.0255 | 0.062* | |
C20 | 0.2702 (7) | 1.1068 (8) | −0.04960 (17) | 0.044 (3) | |
H20 | 0.2517 | 1.1595 | −0.0558 | 0.053* | |
C21 | 0.2915 (7) | 1.0271 (8) | −0.05805 (16) | 0.044 (3) | |
H21 | 0.2861 | 1.0249 | −0.0702 | 0.053* | |
C22 | 0.3204 (8) | 0.9501 (7) | −0.04937 (14) | 0.038 (3) | |
H22 | 0.3338 | 0.8965 | −0.0557 | 0.046* | |
C23 | 0.5147 (7) | 0.9412 (7) | −0.00569 (13) | 0.039 (3) | |
H23A | 0.5490 | 0.9568 | 0.0047 | 0.059* | |
H23B | 0.4908 | 0.9969 | −0.0110 | 0.059* | |
H23C | 0.5551 | 0.9103 | −0.0139 | 0.059* | |
C24 | 0.2085 (7) | 0.6714 (7) | 0.02848 (13) | 0.031 (3) | |
C25 | 0.1374 (7) | 0.6911 (7) | 0.04038 (13) | 0.035 (3) | |
H25 | 0.1247 | 0.7526 | 0.0433 | 0.042* | |
C26 | 0.0857 (7) | 0.6213 (8) | 0.04794 (14) | 0.037 (3) | |
H26 | 0.0372 | 0.6352 | 0.0556 | 0.045* | |
C27 | 0.1075 (8) | 0.5295 (8) | 0.04391 (14) | 0.038 (3) | |
H27 | 0.0756 | 0.4819 | 0.0496 | 0.046* | |
C28 | 0.1740 (8) | 0.5073 (8) | 0.03192 (14) | 0.042 (3) | |
H28 | 0.1867 | 0.4458 | 0.0291 | 0.050* | |
C29 | 0.2212 (8) | 0.5784 (7) | 0.02427 (13) | 0.036 (3) | |
H29 | 0.2647 | 0.5638 | 0.0157 | 0.043* | |
C30 | 0.2513 (6) | 0.8678 (6) | 0.02980 (12) | 0.024 (2) | |
C31 | 0.2152 (7) | 0.9449 (6) | 0.02187 (13) | 0.029 (2) | |
H31 | 0.1981 | 0.9424 | 0.0101 | 0.035* | |
C32 | 0.2040 (8) | 1.0251 (7) | 0.03103 (14) | 0.038 (3) | |
H32 | 0.1805 | 1.0776 | 0.0254 | 0.045* | |
C33 | 0.2273 (8) | 1.0294 (7) | 0.04867 (16) | 0.046 (3) | |
H33 | 0.2194 | 1.0843 | 0.0549 | 0.055* | |
C34 | 0.2622 (8) | 0.9519 (8) | 0.05686 (15) | 0.041 (3) | |
H34 | 0.2787 | 0.9549 | 0.0687 | 0.050* | |
C35 | 0.2728 (7) | 0.8709 (7) | 0.04798 (13) | 0.032 (3) | |
H35 | 0.2940 | 0.8180 | 0.0537 | 0.039* | |
C36 | 0.1088 (8) | 0.6688 (7) | −0.01081 (14) | 0.043 (3) | |
H36 | 0.1344 | 0.6264 | −0.0030 | 0.051* | |
C37 | 0.0715 (7) | 0.7562 (7) | −0.00705 (13) | 0.036 (3) | |
H37 | 0.0671 | 0.7827 | 0.0041 | 0.043* | |
C38 | 0.0398 (7) | 0.8003 (8) | −0.02382 (14) | 0.041 (3) | |
H38 | −0.0041 | 0.8522 | −0.0231 | 0.049* | |
C39 | 0.1321 (7) | 0.8158 (8) | −0.03350 (14) | 0.038 (3) | |
H39 | 0.1593 | 0.8730 | −0.0359 | 0.046* | |
C40 | 0.1674 (8) | 0.7306 (8) | −0.03790 (13) | 0.043 (3) | |
H40 | 0.2227 | 0.7188 | −0.0438 | 0.052* | |
C41 | 0.0976 (8) | 0.6583 (8) | −0.03116 (13) | 0.041 (3) | |
H41 | 0.1008 | 0.5956 | −0.0361 | 0.049* | |
C42 | 0.0097 (9) | 0.7123 (8) | −0.03376 (15) | 0.049 (3) | |
H42A | −0.0435 | 0.6823 | −0.0283 | 0.058* | |
H42B | −0.0031 | 0.7244 | −0.0461 | 0.058* | |
Rh2 | 0.42814 (5) | 0.49305 (6) | 0.123562 (10) | 0.02484 (19) | |
Cr2 | 0.06623 (11) | 0.46824 (11) | 0.15045 (2) | 0.0277 (4) | |
P3 | 0.33396 (17) | 0.45689 (17) | 0.14681 (3) | 0.0230 (6) | |
P4 | 0.30543 (18) | 0.50008 (19) | 0.10521 (3) | 0.0271 (6) | |
O4 | 0.0519 (5) | 0.3640 (6) | 0.18448 (9) | 0.048 (2) | |
O5 | 0.0615 (5) | 0.2764 (5) | 0.13521 (9) | 0.0427 (19) | |
O6 | −0.1422 (5) | 0.4641 (6) | 0.15098 (10) | 0.049 (2) | |
C43 | 0.2170 (6) | 0.5060 (6) | 0.14572 (12) | 0.023 (2) | |
C44 | 0.0594 (7) | 0.4082 (8) | 0.17194 (15) | 0.039 (3) | |
C45 | 0.0635 (7) | 0.3524 (7) | 0.14077 (13) | 0.030 (3) | |
C46 | −0.0627 (8) | 0.4673 (8) | 0.15027 (14) | 0.039 (3) | |
C47 | 0.1637 (6) | 0.5064 (7) | 0.12944 (12) | 0.024 (2) | |
C48 | 0.0854 (7) | 0.5624 (7) | 0.12775 (13) | 0.033 (3) | |
H48 | 0.0538 | 0.5645 | 0.1171 | 0.040* | |
C49 | 0.0528 (7) | 0.6169 (7) | 0.14231 (15) | 0.035 (3) | |
H49 | 0.0005 | 0.6543 | 0.1412 | 0.042* | |
C50 | 0.1003 (7) | 0.6128 (7) | 0.15798 (15) | 0.037 (3) | |
H50 | 0.0781 | 0.6468 | 0.1675 | 0.045* | |
C51 | 0.1816 (7) | 0.5588 (7) | 0.16022 (14) | 0.030 (3) | |
H51 | 0.2119 | 0.5575 | 0.1710 | 0.036* | |
C52 | 0.1957 (6) | 0.4480 (7) | 0.11375 (13) | 0.029 (2) | |
H52 | 0.2127 | 0.3871 | 0.1185 | 0.035* | |
C53 | 0.2740 (7) | 0.6195 (6) | 0.10023 (12) | 0.025 (2) | |
C54 | 0.2120 (7) | 0.6455 (7) | 0.08720 (13) | 0.033 (3) | |
H54 | 0.1874 | 0.6014 | 0.0796 | 0.040* | |
C55 | 0.1874 (7) | 0.7379 (7) | 0.08569 (12) | 0.034 (3) | |
H55 | 0.1433 | 0.7549 | 0.0774 | 0.041* | |
C56 | 0.2265 (7) | 0.8060 (7) | 0.09628 (13) | 0.033 (3) | |
H56 | 0.2108 | 0.8682 | 0.0948 | 0.040* | |
C57 | 0.2897 (7) | 0.7797 (8) | 0.10918 (13) | 0.034 (3) | |
H57 | 0.3157 | 0.8243 | 0.1166 | 0.040* | |
C58 | 0.3137 (6) | 0.6883 (7) | 0.11102 (13) | 0.028 (2) | |
H58 | 0.3568 | 0.6713 | 0.1195 | 0.034* | |
C59 | 0.3280 (6) | 0.4360 (7) | 0.08522 (13) | 0.027 (2) | |
C60 | 0.3441 (6) | 0.4759 (7) | 0.06964 (12) | 0.027 (2) | |
H60 | 0.3388 | 0.5400 | 0.0685 | 0.032* | |
C61 | 0.3688 (7) | 0.4225 (9) | 0.05491 (14) | 0.044 (3) | |
H61 | 0.3784 | 0.4514 | 0.0441 | 0.053* | |
C62 | 0.3789 (8) | 0.3274 (8) | 0.05633 (15) | 0.043 (3) | |
H62 | 0.3969 | 0.2916 | 0.0467 | 0.052* | |
C63 | 0.3615 (7) | 0.2872 (8) | 0.07252 (15) | 0.044 (3) | |
H63 | 0.3683 | 0.2233 | 0.0738 | 0.053* | |
C64 | 0.3343 (7) | 0.3398 (8) | 0.08681 (13) | 0.035 (3) | |
H64 | 0.3201 | 0.3111 | 0.0974 | 0.042* | |
C65 | 0.1205 (6) | 0.4300 (8) | 0.10033 (12) | 0.033 (3) | |
H65A | 0.0660 | 0.4069 | 0.1061 | 0.050* | |
H65B | 0.1419 | 0.3849 | 0.0920 | 0.050* | |
H65C | 0.1058 | 0.4869 | 0.0943 | 0.050* | |
C66 | 0.3229 (6) | 0.3339 (7) | 0.14996 (12) | 0.023 (2) | |
C67 | 0.2667 (7) | 0.2948 (6) | 0.16357 (13) | 0.027 (2) | |
H67 | 0.2319 | 0.3337 | 0.1708 | 0.033* | |
C68 | 0.2635 (7) | 0.2004 (7) | 0.16607 (13) | 0.033 (3) | |
H68 | 0.2270 | 0.1758 | 0.1750 | 0.040* | |
C69 | 0.3148 (8) | 0.1407 (7) | 0.15523 (14) | 0.037 (3) | |
H69 | 0.3129 | 0.0769 | 0.1571 | 0.045* | |
C70 | 0.3683 (7) | 0.1767 (8) | 0.14175 (15) | 0.040 (3) | |
H70 | 0.4012 | 0.1371 | 0.1344 | 0.048* | |
C71 | 0.3727 (6) | 0.2717 (8) | 0.13931 (13) | 0.031 (3) | |
H71 | 0.4098 | 0.2952 | 0.1303 | 0.037* | |
C72 | 0.3833 (6) | 0.5012 (7) | 0.16723 (11) | 0.019 (2) | |
C73 | 0.3902 (7) | 0.5979 (7) | 0.16946 (13) | 0.030 (2) | |
H73 | 0.3620 | 0.6382 | 0.1615 | 0.036* | |
C74 | 0.4390 (8) | 0.6320 (7) | 0.18349 (13) | 0.036 (3) | |
H74 | 0.4417 | 0.6959 | 0.1852 | 0.043* | |
C75 | 0.4835 (7) | 0.5748 (8) | 0.19489 (13) | 0.038 (3) | |
H75 | 0.5170 | 0.6004 | 0.2042 | 0.045* | |
C76 | 0.4803 (7) | 0.4804 (7) | 0.19304 (12) | 0.035 (3) | |
H76 | 0.5114 | 0.4418 | 0.2009 | 0.041* | |
C77 | 0.4281 (7) | 0.4421 (7) | 0.17870 (12) | 0.028 (2) | |
H77 | 0.4245 | 0.3781 | 0.1772 | 0.033* | |
C78 | 0.5664 (6) | 0.4583 (7) | 0.13535 (13) | 0.028 (2) | |
H78 | 0.5507 | 0.4120 | 0.1433 | 0.033* | |
C79 | 0.5507 (6) | 0.5506 (7) | 0.13715 (12) | 0.027 (2) | |
H79 | 0.5208 | 0.5801 | 0.1464 | 0.032* | |
C80 | 0.5930 (7) | 0.5975 (7) | 0.12052 (13) | 0.028 (2) | |
H80 | 0.6061 | 0.6643 | 0.1212 | 0.034* | |
C81 | 0.5270 (7) | 0.5640 (7) | 0.10572 (14) | 0.036 (3) | |
H81 | 0.4868 | 0.6007 | 0.0991 | 0.044* | |
C82 | 0.5393 (7) | 0.4693 (7) | 0.10423 (13) | 0.031 (2) | |
H82 | 0.5079 | 0.4289 | 0.0968 | 0.037* | |
C83 | 0.6155 (7) | 0.4449 (7) | 0.11742 (12) | 0.030 (3) | |
H83 | 0.6472 | 0.3854 | 0.1156 | 0.036* | |
C84 | 0.6762 (6) | 0.5314 (6) | 0.11693 (13) | 0.026 (2) | |
H84A | 0.7050 | 0.5417 | 0.1056 | 0.031* | |
H84B | 0.7226 | 0.5326 | 0.1262 | 0.031* | |
F1 | 0.9524 (4) | 0.7206 (4) | 0.10757 (8) | 0.0453 (16) | |
F2 | 0.8952 (4) | 0.5737 (4) | 0.10725 (8) | 0.0449 (16) | |
F3 | 0.8214 (5) | 0.6883 (4) | 0.09244 (9) | 0.0568 (19) | |
F4 | 0.9599 (5) | 0.6339 (6) | 0.08279 (10) | 0.081 (3) | |
B1 | 0.9061 (8) | 0.6548 (9) | 0.09729 (17) | 0.034 (3) | |
F5 | 0.5025 (8) | 0.4115 (9) | 0.00851 (18) | 0.171 (5) | |
F6 | 0.3540 (8) | 0.4113 (8) | 0.01204 (11) | 0.126 (4) | |
B2 | 0.4178 (14) | 0.4178 (14) | 0.0000 | 0.076 (8) | |
F7 | 1.0039 (4) | 0.0890 (4) | 0.00967 (8) | 0.0509 (17) | |
F8 | 1.0036 (4) | −0.0688 (4) | 0.01143 (8) | 0.0503 (16) | |
B3 | 1.0074 (9) | 0.0074 (9) | 0.0000 | 0.050 (5) | |
C85 | 0.8702 (17) | 0.7547 (17) | 0.0273 (4) | 0.173 (5)* | 0.50 |
H85A | 0.9357 | 0.7379 | 0.0289 | 0.173 (5)* | 0.50 |
H85B | 0.8308 | 0.7079 | 0.0330 | 0.173 (5)* | 0.50 |
H85C | 0.8586 | 0.8156 | 0.0327 | 0.173 (5)* | 0.50 |
O7 | 0.8492 (17) | 0.7586 (17) | 0.0089 (4) | 0.173 (5)* | 0.50 |
H7A | 0.7833 | 0.7621 | 0.0085 | 0.173 (5)* | 0.50 |
C86 | 0.4127 (10) | 0.1636 (9) | 0.01799 (15) | 0.173 (5)* | |
H86A | 0.4612 | 0.2114 | 0.0178 | 0.173 (5)* | |
H86B | 0.4285 | 0.1139 | 0.0097 | 0.173 (5)* | |
H86C | 0.4078 | 0.1377 | 0.0299 | 0.173 (5)* | |
O8 | 0.3256 (10) | 0.2040 (9) | 0.01308 (15) | 0.173 (5)* | |
H8A | 0.3334 | 0.2696 | 0.0127 | 0.173 (5)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Rh1 | 0.0445 (5) | 0.0321 (5) | 0.0168 (4) | −0.0059 (4) | −0.0027 (4) | 0.0013 (4) |
Cr1 | 0.0399 (10) | 0.0397 (10) | 0.0192 (10) | 0.0047 (8) | −0.0012 (8) | 0.0016 (8) |
P1 | 0.0456 (16) | 0.0263 (14) | 0.0240 (16) | −0.0029 (13) | −0.0007 (13) | −0.0015 (12) |
P2 | 0.0445 (17) | 0.0299 (15) | 0.0161 (16) | 0.0008 (13) | −0.0043 (13) | −0.0007 (12) |
O1 | 0.044 (5) | 0.046 (5) | 0.041 (5) | −0.005 (4) | 0.009 (4) | −0.001 (4) |
O2 | 0.051 (5) | 0.071 (6) | 0.038 (5) | 0.010 (4) | −0.005 (4) | 0.010 (4) |
O3 | 0.051 (5) | 0.061 (5) | 0.033 (5) | −0.011 (4) | 0.002 (4) | 0.011 (4) |
C1 | 0.055 (7) | 0.022 (6) | 0.027 (6) | 0.021 (5) | −0.011 (5) | −0.003 (5) |
C2 | 0.036 (6) | 0.041 (7) | 0.021 (6) | 0.002 (5) | −0.007 (5) | −0.001 (5) |
C3 | 0.040 (7) | 0.057 (8) | 0.016 (6) | 0.011 (6) | −0.012 (5) | −0.002 (5) |
C4 | 0.037 (6) | 0.044 (7) | 0.025 (7) | −0.005 (5) | 0.000 (5) | 0.001 (5) |
C5 | 0.052 (7) | 0.032 (6) | 0.021 (6) | 0.009 (5) | 0.000 (5) | −0.003 (5) |
C6 | 0.046 (7) | 0.059 (8) | 0.023 (7) | 0.009 (6) | 0.000 (5) | 0.000 (6) |
C7 | 0.072 (9) | 0.070 (9) | 0.012 (7) | 0.042 (8) | 0.004 (6) | −0.007 (6) |
C8 | 0.066 (9) | 0.040 (7) | 0.034 (8) | 0.024 (6) | −0.006 (7) | −0.005 (6) |
C9 | 0.060 (8) | 0.029 (6) | 0.023 (7) | −0.004 (6) | −0.001 (6) | −0.006 (5) |
C10 | 0.032 (6) | 0.031 (6) | 0.022 (6) | 0.006 (4) | −0.007 (5) | 0.000 (5) |
C11 | 0.052 (7) | 0.034 (6) | 0.024 (6) | −0.004 (6) | 0.006 (6) | 0.006 (5) |
C12 | 0.041 (7) | 0.039 (7) | 0.034 (7) | 0.003 (5) | −0.018 (5) | −0.001 (6) |
C13 | 0.075 (10) | 0.051 (8) | 0.021 (7) | 0.032 (7) | −0.020 (7) | −0.020 (6) |
C14 | 0.049 (8) | 0.087 (11) | 0.014 (7) | 0.031 (7) | −0.007 (6) | −0.002 (7) |
C15 | 0.054 (8) | 0.056 (8) | 0.026 (7) | 0.008 (7) | −0.003 (6) | 0.008 (6) |
C16 | 0.039 (6) | 0.039 (6) | 0.028 (7) | 0.007 (6) | −0.009 (6) | 0.002 (5) |
C17 | 0.027 (6) | 0.040 (7) | 0.018 (6) | 0.003 (5) | −0.002 (5) | 0.010 (5) |
C18 | 0.038 (7) | 0.045 (7) | 0.033 (7) | −0.002 (5) | 0.005 (5) | −0.001 (6) |
C19 | 0.029 (7) | 0.044 (7) | 0.082 (11) | 0.007 (6) | 0.007 (7) | 0.010 (7) |
C20 | 0.028 (6) | 0.047 (8) | 0.058 (9) | −0.005 (6) | −0.009 (6) | 0.028 (7) |
C21 | 0.031 (6) | 0.053 (8) | 0.048 (8) | −0.007 (5) | −0.005 (6) | 0.010 (7) |
C22 | 0.058 (8) | 0.026 (6) | 0.030 (7) | −0.008 (5) | −0.009 (6) | 0.007 (5) |
C23 | 0.041 (7) | 0.049 (7) | 0.028 (6) | 0.000 (5) | −0.007 (5) | 0.005 (5) |
C24 | 0.051 (7) | 0.027 (6) | 0.017 (6) | −0.002 (5) | 0.002 (5) | 0.004 (5) |
C25 | 0.043 (7) | 0.032 (6) | 0.030 (7) | −0.011 (5) | −0.011 (5) | −0.005 (5) |
C26 | 0.027 (6) | 0.049 (7) | 0.035 (7) | −0.013 (5) | −0.007 (5) | 0.002 (6) |
C27 | 0.045 (7) | 0.036 (7) | 0.033 (7) | −0.017 (5) | −0.016 (6) | 0.012 (6) |
C28 | 0.060 (8) | 0.037 (7) | 0.027 (7) | −0.004 (6) | −0.017 (6) | 0.011 (6) |
C29 | 0.049 (7) | 0.027 (6) | 0.030 (7) | 0.001 (5) | −0.001 (6) | 0.002 (5) |
C30 | 0.030 (6) | 0.023 (5) | 0.018 (6) | −0.007 (4) | −0.004 (4) | 0.000 (4) |
C31 | 0.039 (6) | 0.020 (6) | 0.028 (6) | 0.001 (5) | 0.006 (5) | −0.001 (5) |
C32 | 0.063 (8) | 0.033 (7) | 0.017 (7) | 0.010 (5) | −0.004 (6) | 0.003 (5) |
C33 | 0.046 (7) | 0.028 (6) | 0.064 (9) | 0.000 (5) | 0.018 (7) | −0.005 (6) |
C34 | 0.047 (7) | 0.044 (7) | 0.033 (7) | −0.012 (6) | 0.001 (6) | −0.016 (6) |
C35 | 0.036 (6) | 0.036 (6) | 0.024 (7) | 0.004 (5) | 0.002 (5) | −0.009 (5) |
C36 | 0.078 (9) | 0.023 (6) | 0.027 (7) | −0.004 (5) | −0.003 (6) | −0.003 (5) |
C37 | 0.042 (6) | 0.046 (7) | 0.019 (6) | −0.002 (5) | −0.006 (5) | 0.003 (5) |
C38 | 0.033 (6) | 0.054 (8) | 0.035 (7) | 0.001 (5) | −0.007 (5) | 0.005 (6) |
C39 | 0.037 (7) | 0.033 (7) | 0.045 (8) | −0.008 (5) | −0.014 (5) | 0.005 (6) |
C40 | 0.045 (7) | 0.062 (8) | 0.023 (6) | −0.019 (6) | 0.001 (5) | 0.006 (6) |
C41 | 0.051 (8) | 0.053 (8) | 0.019 (7) | −0.011 (6) | −0.010 (5) | −0.017 (6) |
C42 | 0.062 (8) | 0.051 (7) | 0.032 (7) | 0.000 (7) | −0.016 (6) | −0.002 (6) |
Rh2 | 0.0257 (4) | 0.0337 (5) | 0.0152 (4) | −0.0022 (4) | 0.0000 (4) | 0.0013 (4) |
Cr2 | 0.0252 (9) | 0.0337 (10) | 0.0242 (10) | 0.0012 (7) | −0.0015 (7) | −0.0001 (7) |
P3 | 0.0244 (14) | 0.0294 (15) | 0.0152 (15) | 0.0009 (11) | −0.0004 (11) | −0.0002 (11) |
P4 | 0.0302 (14) | 0.0342 (15) | 0.0170 (15) | −0.0062 (12) | 0.0019 (11) | −0.0002 (13) |
O4 | 0.061 (6) | 0.069 (6) | 0.014 (5) | −0.014 (4) | −0.003 (4) | 0.013 (4) |
O5 | 0.049 (5) | 0.044 (5) | 0.035 (5) | −0.009 (4) | −0.005 (4) | 0.000 (4) |
O6 | 0.026 (4) | 0.081 (6) | 0.041 (5) | 0.009 (4) | 0.000 (4) | −0.002 (4) |
C43 | 0.025 (5) | 0.023 (5) | 0.020 (6) | 0.004 (4) | 0.002 (4) | 0.000 (5) |
C44 | 0.032 (6) | 0.065 (8) | 0.020 (7) | 0.003 (6) | 0.004 (5) | −0.002 (6) |
C45 | 0.032 (6) | 0.032 (6) | 0.028 (7) | −0.010 (5) | 0.001 (5) | −0.009 (5) |
C46 | 0.037 (7) | 0.056 (8) | 0.023 (7) | 0.000 (6) | 0.001 (5) | 0.007 (5) |
C47 | 0.020 (5) | 0.030 (6) | 0.022 (6) | 0.000 (4) | −0.002 (4) | 0.001 (5) |
C48 | 0.037 (6) | 0.045 (7) | 0.017 (6) | 0.003 (5) | −0.011 (5) | 0.001 (5) |
C49 | 0.029 (6) | 0.032 (6) | 0.044 (8) | 0.003 (5) | −0.005 (6) | 0.001 (5) |
C50 | 0.028 (6) | 0.047 (7) | 0.037 (8) | 0.004 (5) | 0.000 (5) | −0.019 (6) |
C51 | 0.029 (6) | 0.032 (6) | 0.029 (7) | −0.003 (5) | −0.002 (5) | 0.004 (5) |
C52 | 0.028 (6) | 0.036 (6) | 0.023 (6) | −0.003 (4) | 0.007 (5) | −0.005 (5) |
C53 | 0.030 (6) | 0.032 (6) | 0.014 (6) | −0.004 (5) | 0.003 (5) | 0.000 (4) |
C54 | 0.040 (7) | 0.037 (6) | 0.022 (6) | 0.008 (5) | 0.002 (5) | 0.004 (5) |
C55 | 0.043 (7) | 0.043 (7) | 0.017 (6) | 0.015 (5) | 0.007 (5) | 0.000 (5) |
C56 | 0.037 (6) | 0.037 (6) | 0.025 (6) | 0.005 (5) | 0.006 (5) | 0.001 (5) |
C57 | 0.037 (7) | 0.042 (7) | 0.022 (6) | 0.005 (5) | 0.003 (5) | −0.001 (5) |
C58 | 0.019 (5) | 0.044 (7) | 0.022 (6) | 0.002 (5) | −0.002 (5) | −0.005 (5) |
C59 | 0.020 (5) | 0.046 (7) | 0.016 (6) | −0.001 (5) | −0.007 (4) | −0.010 (5) |
C60 | 0.036 (6) | 0.039 (6) | 0.005 (6) | −0.006 (5) | 0.003 (4) | 0.000 (5) |
C61 | 0.044 (7) | 0.068 (9) | 0.020 (7) | 0.005 (6) | 0.002 (5) | −0.001 (6) |
C62 | 0.059 (8) | 0.050 (8) | 0.021 (7) | 0.002 (6) | 0.000 (6) | −0.008 (6) |
C63 | 0.040 (7) | 0.041 (7) | 0.051 (8) | 0.007 (5) | −0.002 (6) | −0.004 (7) |
C64 | 0.038 (7) | 0.046 (7) | 0.021 (7) | 0.012 (5) | 0.004 (5) | −0.002 (5) |
C65 | 0.022 (6) | 0.054 (7) | 0.024 (6) | −0.008 (5) | −0.007 (5) | −0.005 (6) |
C66 | 0.024 (5) | 0.035 (6) | 0.010 (6) | 0.005 (4) | −0.003 (4) | −0.003 (5) |
C67 | 0.030 (6) | 0.021 (5) | 0.031 (6) | 0.012 (4) | −0.012 (5) | −0.006 (4) |
C68 | 0.037 (6) | 0.040 (7) | 0.024 (6) | −0.001 (5) | −0.004 (5) | 0.011 (5) |
C69 | 0.054 (8) | 0.020 (6) | 0.037 (7) | 0.005 (5) | −0.027 (6) | −0.003 (5) |
C70 | 0.026 (6) | 0.059 (9) | 0.036 (7) | 0.007 (5) | 0.002 (5) | −0.001 (6) |
C71 | 0.020 (5) | 0.039 (7) | 0.034 (7) | −0.007 (5) | 0.005 (5) | 0.007 (5) |
C72 | 0.017 (4) | 0.032 (5) | 0.008 (5) | 0.002 (4) | −0.001 (4) | 0.010 (4) |
C73 | 0.044 (7) | 0.027 (6) | 0.019 (6) | 0.002 (5) | −0.010 (5) | 0.009 (5) |
C74 | 0.060 (8) | 0.028 (6) | 0.020 (6) | −0.003 (5) | 0.000 (6) | −0.003 (5) |
C75 | 0.033 (6) | 0.053 (7) | 0.026 (6) | −0.004 (6) | −0.003 (5) | 0.001 (6) |
C76 | 0.041 (7) | 0.043 (7) | 0.019 (6) | −0.011 (5) | −0.005 (5) | 0.006 (5) |
C77 | 0.032 (6) | 0.036 (6) | 0.015 (6) | −0.005 (5) | −0.003 (5) | 0.005 (5) |
C78 | 0.022 (5) | 0.037 (5) | 0.024 (6) | −0.002 (4) | 0.001 (4) | 0.009 (4) |
C79 | 0.029 (5) | 0.047 (5) | 0.004 (5) | −0.001 (4) | 0.001 (4) | −0.008 (4) |
C80 | 0.029 (6) | 0.021 (5) | 0.036 (6) | −0.005 (4) | 0.011 (5) | 0.000 (4) |
C81 | 0.024 (6) | 0.048 (7) | 0.037 (7) | 0.001 (5) | 0.000 (5) | 0.018 (6) |
C82 | 0.037 (6) | 0.032 (6) | 0.025 (6) | −0.003 (4) | −0.006 (5) | −0.005 (5) |
C83 | 0.025 (6) | 0.046 (7) | 0.019 (6) | 0.009 (5) | 0.006 (5) | −0.004 (5) |
C84 | 0.021 (5) | 0.037 (6) | 0.020 (6) | −0.004 (4) | 0.002 (4) | −0.005 (5) |
F1 | 0.050 (4) | 0.047 (4) | 0.039 (4) | −0.007 (3) | −0.005 (3) | −0.009 (3) |
F2 | 0.039 (4) | 0.044 (4) | 0.052 (4) | 0.001 (3) | −0.005 (3) | 0.013 (3) |
F3 | 0.055 (4) | 0.050 (4) | 0.065 (5) | 0.000 (3) | −0.016 (4) | 0.001 (4) |
F4 | 0.076 (6) | 0.097 (6) | 0.069 (6) | −0.025 (5) | 0.041 (5) | −0.024 (5) |
B1 | 0.026 (7) | 0.037 (8) | 0.039 (9) | −0.007 (5) | 0.010 (6) | 0.011 (7) |
F5 | 0.112 (9) | 0.182 (12) | 0.218 (14) | −0.012 (9) | −0.060 (10) | −0.024 (10) |
F6 | 0.152 (9) | 0.174 (10) | 0.052 (6) | 0.098 (8) | 0.053 (6) | 0.017 (6) |
B2 | 0.060 (10) | 0.060 (10) | 0.11 (3) | 0.017 (13) | −0.002 (12) | 0.002 (12) |
F7 | 0.062 (4) | 0.049 (4) | 0.041 (4) | −0.005 (3) | −0.015 (4) | −0.002 (3) |
F8 | 0.058 (4) | 0.052 (4) | 0.041 (4) | −0.001 (3) | 0.010 (4) | 0.001 (3) |
B3 | 0.053 (8) | 0.053 (8) | 0.043 (13) | −0.023 (10) | 0.012 (8) | −0.012 (8) |
Geometric parameters (Å, º) top
Rh1—C36 | 2.210 (11) | Cr2—C50 | 2.212 (11) |
Rh1—C37 | 2.217 (10) | Cr2—C49 | 2.235 (10) |
Rh1—C39 | 2.218 (10) | Cr2—C51 | 2.237 (10) |
Rh1—C40 | 2.240 (10) | Cr2—C43 | 2.266 (9) |
Rh1—P2 | 2.273 (3) | P3—C66 | 1.792 (10) |
Rh1—P1 | 2.277 (3) | P3—C72 | 1.823 (9) |
Cr1—C4 | 1.807 (11) | P3—C43 | 1.827 (9) |
Cr1—C2 | 1.821 (11) | P4—C59 | 1.807 (10) |
Cr1—C3 | 1.852 (11) | P4—C53 | 1.816 (10) |
Cr1—C9 | 2.158 (11) | P4—C52 | 1.865 (10) |
Cr1—C7 | 2.195 (10) | O4—C44 | 1.152 (12) |
Cr1—C1 | 2.204 (11) | O5—C45 | 1.172 (11) |
Cr1—C6 | 2.232 (11) | O6—C46 | 1.146 (12) |
Cr1—C5 | 2.241 (11) | C43—C51 | 1.432 (13) |
Cr1—C8 | 2.252 (11) | C43—C47 | 1.458 (12) |
P1—C24 | 1.810 (10) | C47—C48 | 1.390 (13) |
P1—C30 | 1.812 (9) | C47—C52 | 1.531 (13) |
P1—C1 | 1.846 (11) | C48—C49 | 1.436 (14) |
P2—C17 | 1.808 (10) | C48—H48 | 0.9300 |
P2—C11 | 1.810 (11) | C49—C50 | 1.375 (14) |
P2—C10 | 1.851 (10) | C49—H49 | 0.9300 |
O1—C2 | 1.168 (11) | C50—C51 | 1.415 (13) |
O2—C3 | 1.133 (11) | C50—H50 | 0.9300 |
O3—C4 | 1.143 (11) | C51—H51 | 0.9300 |
C1—C5 | 1.411 (15) | C52—C65 | 1.509 (12) |
C1—C9 | 1.455 (13) | C52—H52 | 0.9800 |
C5—C6 | 1.406 (14) | C53—C54 | 1.385 (13) |
C5—C10 | 1.514 (13) | C53—C58 | 1.407 (13) |
C6—C7 | 1.418 (15) | C54—C55 | 1.380 (14) |
C6—H6 | 0.9300 | C54—H54 | 0.9300 |
C7—C8 | 1.422 (17) | C55—C56 | 1.388 (14) |
C7—H7 | 0.9300 | C55—H55 | 0.9300 |
C8—C9 | 1.364 (15) | C56—C57 | 1.390 (13) |
C8—H8 | 0.9300 | C56—H56 | 0.9300 |
C9—H9 | 0.9300 | C57—C58 | 1.367 (13) |
C10—C23 | 1.559 (13) | C57—H57 | 0.9300 |
C10—H10 | 0.9800 | C58—H58 | 0.9300 |
C11—C16 | 1.362 (14) | C59—C60 | 1.336 (13) |
C11—C12 | 1.392 (14) | C59—C64 | 1.393 (14) |
C12—C13 | 1.412 (14) | C60—C61 | 1.404 (14) |
C12—H12 | 0.9300 | C60—H60 | 0.9300 |
C13—C14 | 1.375 (17) | C61—C62 | 1.379 (15) |
C13—H13 | 0.9300 | C61—H61 | 0.9300 |
C14—C15 | 1.368 (16) | C62—C63 | 1.384 (15) |
C14—H14 | 0.9300 | C62—H62 | 0.9300 |
C15—C16 | 1.402 (14) | C63—C64 | 1.381 (14) |
C15—H15 | 0.9300 | C63—H63 | 0.9300 |
C16—H16 | 0.9300 | C64—H64 | 0.9300 |
C17—C18 | 1.369 (14) | C65—H65A | 0.9600 |
C17—C22 | 1.400 (13) | C65—H65B | 0.9600 |
C18—C19 | 1.408 (15) | C65—H65C | 0.9600 |
C18—H18 | 0.9300 | C66—C71 | 1.404 (13) |
C19—C20 | 1.371 (16) | C66—C67 | 1.430 (13) |
C19—H19 | 0.9300 | C67—C68 | 1.373 (13) |
C20—C21 | 1.350 (15) | C67—H67 | 0.9300 |
C20—H20 | 0.9300 | C68—C69 | 1.401 (14) |
C21—C22 | 1.355 (14) | C68—H68 | 0.9300 |
C21—H21 | 0.9300 | C69—C70 | 1.383 (15) |
C22—H22 | 0.9300 | C69—H69 | 0.9300 |
C23—H23A | 0.9600 | C70—C71 | 1.381 (14) |
C23—H23B | 0.9600 | C70—H70 | 0.9300 |
C23—H23C | 0.9600 | C71—H71 | 0.9300 |
C24—C29 | 1.389 (14) | C72—C77 | 1.378 (12) |
C24—C25 | 1.395 (14) | C72—C73 | 1.406 (13) |
C25—C26 | 1.376 (13) | C73—C74 | 1.368 (13) |
C25—H25 | 0.9300 | C73—H73 | 0.9300 |
C26—C27 | 1.392 (15) | C74—C75 | 1.356 (13) |
C26—H26 | 0.9300 | C74—H74 | 0.9300 |
C27—C28 | 1.360 (15) | C75—C76 | 1.366 (14) |
C27—H27 | 0.9300 | C75—H75 | 0.9300 |
C28—C29 | 1.359 (14) | C76—C77 | 1.434 (12) |
C28—H28 | 0.9300 | C76—H76 | 0.9300 |
C29—H29 | 0.9300 | C77—H77 | 0.9300 |
C30—C31 | 1.365 (13) | C78—C79 | 1.354 (13) |
C30—C35 | 1.417 (13) | C78—C83 | 1.548 (13) |
C31—C32 | 1.359 (13) | C78—H78 | 0.9300 |
C31—H31 | 0.9300 | C79—C80 | 1.557 (12) |
C32—C33 | 1.384 (15) | C79—H79 | 0.9300 |
C32—H32 | 0.9300 | C80—C81 | 1.549 (13) |
C33—C34 | 1.372 (15) | C80—C84 | 1.554 (13) |
C33—H33 | 0.9300 | C80—H80 | 0.9800 |
C34—C35 | 1.355 (13) | C81—C82 | 1.379 (13) |
C34—H34 | 0.9300 | C81—H81 | 0.9300 |
C35—H35 | 0.9300 | C82—C83 | 1.527 (13) |
C36—C37 | 1.396 (14) | C82—H82 | 0.9300 |
C36—C41 | 1.563 (14) | C83—C84 | 1.521 (13) |
C36—H36 | 0.9300 | C83—H83 | 0.9800 |
C37—C38 | 1.496 (14) | C84—H84A | 0.9700 |
C37—H37 | 0.9300 | C84—H84B | 0.9700 |
C38—C39 | 1.535 (14) | F1—B1 | 1.396 (14) |
C38—C42 | 1.537 (14) | F2—B1 | 1.401 (13) |
C38—H38 | 0.9800 | F3—B1 | 1.363 (13) |
C39—C40 | 1.369 (15) | F4—B1 | 1.381 (14) |
C39—H39 | 0.9300 | F5—B2 | 1.383 (17) |
C40—C41 | 1.533 (14) | F6—B2 | 1.300 (16) |
C40—H40 | 0.9300 | B2—F6i | 1.300 (16) |
C41—C42 | 1.498 (16) | B2—F5i | 1.383 (17) |
C41—H41 | 0.9800 | F7—B3 | 1.387 (12) |
C42—H42A | 0.9700 | F8—B3 | 1.400 (12) |
C42—H42B | 0.9700 | B3—F7ii | 1.387 (12) |
Rh2—C82 | 2.200 (10) | B3—F8ii | 1.401 (12) |
Rh2—C79 | 2.206 (9) | C85—O7 | 1.4297 |
Rh2—C81 | 2.215 (10) | C85—H85A | 0.9802 |
Rh2—C78 | 2.238 (9) | C85—H85B | 0.9799 |
Rh2—P4 | 2.253 (3) | C85—H85C | 0.9808 |
Rh2—P3 | 2.288 (3) | O7—H7A | 0.9500 |
Cr2—C45 | 1.824 (10) | C86—O8 | 1.4301 |
Cr2—C44 | 1.851 (12) | C86—H86A | 0.9799 |
Cr2—C46 | 1.855 (11) | C86—H86B | 0.9806 |
Cr2—C47 | 2.196 (9) | C86—H86C | 0.9813 |
Cr2—C48 | 2.212 (10) | O8—H8A | 0.9504 |
| | | |
C36—Rh1—C37 | 36.8 (4) | C45—Cr2—C46 | 88.2 (5) |
C36—Rh1—C39 | 76.8 (4) | C44—Cr2—C46 | 87.1 (5) |
C37—Rh1—C39 | 64.2 (4) | C45—Cr2—C47 | 87.0 (4) |
C36—Rh1—C40 | 65.2 (4) | C44—Cr2—C47 | 142.5 (4) |
C37—Rh1—C40 | 76.1 (4) | C46—Cr2—C47 | 129.4 (4) |
C39—Rh1—C40 | 35.8 (4) | C45—Cr2—C48 | 104.3 (4) |
C36—Rh1—P2 | 160.2 (3) | C44—Cr2—C48 | 169.0 (4) |
C37—Rh1—P2 | 157.3 (3) | C46—Cr2—C48 | 97.1 (4) |
C39—Rh1—P2 | 99.7 (3) | C47—Cr2—C48 | 36.8 (3) |
C40—Rh1—P2 | 100.5 (3) | C45—Cr2—C50 | 165.7 (4) |
C36—Rh1—P1 | 99.4 (3) | C44—Cr2—C50 | 102.8 (5) |
C37—Rh1—P1 | 98.1 (3) | C46—Cr2—C50 | 103.3 (4) |
C39—Rh1—P1 | 155.5 (3) | C47—Cr2—C50 | 79.1 (4) |
C40—Rh1—P1 | 161.2 (3) | C48—Cr2—C50 | 66.3 (4) |
P2—Rh1—P1 | 91.60 (10) | C45—Cr2—C49 | 139.6 (4) |
C4—Cr1—C2 | 90.4 (5) | C44—Cr2—C49 | 133.4 (5) |
C4—Cr1—C3 | 86.4 (5) | C46—Cr2—C49 | 85.3 (4) |
C2—Cr1—C3 | 87.5 (5) | C47—Cr2—C49 | 67.3 (4) |
C4—Cr1—C9 | 86.5 (4) | C48—Cr2—C49 | 37.7 (4) |
C2—Cr1—C9 | 134.0 (4) | C50—Cr2—C49 | 36.0 (4) |
C3—Cr1—C9 | 137.9 (5) | C45—Cr2—C51 | 133.0 (4) |
C4—Cr1—C7 | 129.5 (5) | C44—Cr2—C51 | 91.0 (4) |
C2—Cr1—C7 | 139.4 (5) | C46—Cr2—C51 | 138.5 (4) |
C3—Cr1—C7 | 87.8 (5) | C47—Cr2—C51 | 67.8 (4) |
C9—Cr1—C7 | 65.7 (5) | C48—Cr2—C51 | 79.1 (4) |
C4—Cr1—C1 | 105.0 (5) | C50—Cr2—C51 | 37.1 (3) |
C2—Cr1—C1 | 99.1 (4) | C49—Cr2—C51 | 66.4 (4) |
C3—Cr1—C1 | 166.7 (4) | C45—Cr2—C43 | 100.1 (4) |
C9—Cr1—C1 | 39.0 (4) | C44—Cr2—C43 | 107.6 (4) |
C7—Cr1—C1 | 79.6 (4) | C46—Cr2—C43 | 163.4 (4) |
C4—Cr1—C6 | 163.7 (5) | C47—Cr2—C43 | 38.1 (3) |
C2—Cr1—C6 | 104.5 (4) | C48—Cr2—C43 | 67.0 (3) |
C3—Cr1—C6 | 100.5 (4) | C50—Cr2—C43 | 66.6 (3) |
C9—Cr1—C6 | 78.5 (4) | C49—Cr2—C43 | 79.0 (4) |
C7—Cr1—C6 | 37.4 (4) | C51—Cr2—C43 | 37.1 (3) |
C1—Cr1—C6 | 66.7 (4) | C66—P3—C72 | 105.4 (4) |
C4—Cr1—C5 | 140.5 (4) | C66—P3—C43 | 107.8 (4) |
C2—Cr1—C5 | 87.6 (4) | C72—P3—C43 | 105.2 (4) |
C3—Cr1—C5 | 132.8 (4) | C66—P3—Rh2 | 112.3 (3) |
C9—Cr1—C5 | 67.5 (4) | C72—P3—Rh2 | 110.4 (3) |
C7—Cr1—C5 | 66.9 (4) | C43—P3—Rh2 | 115.0 (3) |
C1—Cr1—C5 | 37.0 (4) | C59—P4—C53 | 110.6 (5) |
C6—Cr1—C5 | 36.6 (4) | C59—P4—C52 | 103.9 (4) |
C4—Cr1—C8 | 96.7 (5) | C53—P4—C52 | 104.0 (5) |
C2—Cr1—C8 | 166.6 (4) | C59—P4—Rh2 | 111.0 (3) |
C3—Cr1—C8 | 104.2 (5) | C53—P4—Rh2 | 111.5 (3) |
C9—Cr1—C8 | 36.0 (4) | C52—P4—Rh2 | 115.5 (3) |
C7—Cr1—C8 | 37.3 (4) | C51—C43—C47 | 117.7 (8) |
C1—Cr1—C8 | 68.2 (4) | C51—C43—P3 | 119.8 (7) |
C6—Cr1—C8 | 67.4 (4) | C47—C43—P3 | 121.7 (7) |
C5—Cr1—C8 | 79.7 (4) | C51—C43—Cr2 | 70.4 (5) |
C24—P1—C30 | 106.0 (5) | C47—C43—Cr2 | 68.4 (5) |
C24—P1—C1 | 107.3 (5) | P3—C43—Cr2 | 141.4 (5) |
C30—P1—C1 | 105.8 (4) | O4—C44—Cr2 | 173.7 (10) |
C24—P1—Rh1 | 110.6 (3) | O5—C45—Cr2 | 177.3 (9) |
C30—P1—Rh1 | 115.0 (3) | O6—C46—Cr2 | 176.3 (9) |
C1—P1—Rh1 | 111.6 (3) | C48—C47—C43 | 120.5 (9) |
C17—P2—C11 | 104.6 (5) | C48—C47—C52 | 119.3 (8) |
C17—P2—C10 | 106.4 (4) | C43—C47—C52 | 120.1 (8) |
C11—P2—C10 | 106.8 (5) | C48—C47—Cr2 | 72.2 (6) |
C17—P2—Rh1 | 109.5 (3) | C43—C47—Cr2 | 73.6 (5) |
C11—P2—Rh1 | 115.0 (4) | C52—C47—Cr2 | 128.5 (7) |
C10—P2—Rh1 | 113.9 (3) | C47—C48—C49 | 120.6 (9) |
C5—C1—C9 | 117.2 (10) | C47—C48—Cr2 | 71.0 (6) |
C5—C1—P1 | 121.1 (7) | C49—C48—Cr2 | 72.0 (6) |
C9—C1—P1 | 120.7 (9) | C47—C48—H48 | 119.7 |
C5—C1—Cr1 | 72.9 (6) | C49—C48—H48 | 119.7 |
C9—C1—Cr1 | 68.8 (6) | Cr2—C48—H48 | 129.8 |
P1—C1—Cr1 | 138.8 (5) | C50—C49—C48 | 118.9 (10) |
O1—C2—Cr1 | 178.5 (10) | C50—C49—Cr2 | 71.1 (6) |
O2—C3—Cr1 | 179.0 (9) | C48—C49—Cr2 | 70.3 (6) |
O3—C4—Cr1 | 178.8 (9) | C50—C49—H49 | 120.6 |
C6—C5—C1 | 119.9 (10) | C48—C49—H49 | 120.6 |
C6—C5—C10 | 119.7 (10) | Cr2—C49—H49 | 130.6 |
C1—C5—C10 | 120.4 (9) | C49—C50—C51 | 122.6 (10) |
C6—C5—Cr1 | 71.3 (6) | C49—C50—Cr2 | 72.9 (6) |
C1—C5—Cr1 | 70.1 (6) | C51—C50—Cr2 | 72.4 (6) |
C10—C5—Cr1 | 132.4 (7) | C49—C50—H50 | 118.7 |
C5—C6—C7 | 119.9 (11) | C51—C50—H50 | 118.7 |
C5—C6—Cr1 | 72.0 (6) | Cr2—C50—H50 | 128.4 |
C7—C6—Cr1 | 69.9 (6) | C50—C51—C43 | 119.5 (9) |
C5—C6—H6 | 120.0 | C50—C51—Cr2 | 70.5 (6) |
C7—C6—H6 | 120.0 | C43—C51—Cr2 | 72.6 (6) |
Cr1—C6—H6 | 130.6 | C50—C51—H51 | 120.2 |
C6—C7—C8 | 122.2 (11) | C43—C51—H51 | 120.2 |
C6—C7—Cr1 | 72.7 (6) | Cr2—C51—H51 | 129.0 |
C8—C7—Cr1 | 73.5 (6) | C65—C52—C47 | 113.9 (8) |
C6—C7—H7 | 118.9 | C65—C52—P4 | 116.1 (7) |
C8—C7—H7 | 118.9 | C47—C52—P4 | 107.8 (6) |
Cr1—C7—H7 | 126.9 | C65—C52—H52 | 106.1 |
C9—C8—C7 | 115.9 (11) | C47—C52—H52 | 106.1 |
C9—C8—Cr1 | 68.3 (6) | P4—C52—H52 | 106.1 |
C7—C8—Cr1 | 69.2 (6) | C54—C53—C58 | 119.2 (9) |
C9—C8—H8 | 122.0 | C54—C53—P4 | 124.4 (8) |
C7—C8—H8 | 122.0 | C58—C53—P4 | 116.3 (7) |
Cr1—C8—H8 | 133.1 | C55—C54—C53 | 119.1 (10) |
C8—C9—C1 | 124.7 (11) | C55—C54—H54 | 120.5 |
C8—C9—Cr1 | 75.8 (7) | C53—C54—H54 | 120.5 |
C1—C9—Cr1 | 72.2 (6) | C54—C55—C56 | 121.8 (10) |
C8—C9—H9 | 117.7 | C54—C55—H55 | 119.1 |
C1—C9—H9 | 117.7 | C56—C55—H55 | 119.1 |
Cr1—C9—H9 | 126.4 | C55—C56—C57 | 118.9 (10) |
C5—C10—C23 | 114.1 (8) | C55—C56—H56 | 120.5 |
C5—C10—P2 | 109.5 (7) | C57—C56—H56 | 120.5 |
C23—C10—P2 | 114.4 (7) | C58—C57—C56 | 119.9 (10) |
C5—C10—H10 | 106.0 | C58—C57—H57 | 120.1 |
C23—C10—H10 | 106.0 | C56—C57—H57 | 120.1 |
P2—C10—H10 | 106.0 | C57—C58—C53 | 121.1 (9) |
C16—C11—C12 | 120.0 (10) | C57—C58—H58 | 119.5 |
C16—C11—P2 | 122.0 (8) | C53—C58—H58 | 119.5 |
C12—C11—P2 | 117.8 (9) | C60—C59—C64 | 119.5 (9) |
C11—C12—C13 | 119.4 (11) | C60—C59—P4 | 124.0 (8) |
C11—C12—H12 | 120.3 | C64—C59—P4 | 116.5 (8) |
C13—C12—H12 | 120.3 | C59—C60—C61 | 121.1 (10) |
C14—C13—C12 | 119.3 (12) | C59—C60—H60 | 119.4 |
C14—C13—H13 | 120.3 | C61—C60—H60 | 119.4 |
C12—C13—H13 | 120.3 | C62—C61—C60 | 120.5 (11) |
C15—C14—C13 | 121.0 (11) | C62—C61—H61 | 119.8 |
C15—C14—H14 | 119.5 | C60—C61—H61 | 119.8 |
C13—C14—H14 | 119.5 | C61—C62—C63 | 117.7 (11) |
C14—C15—C16 | 119.5 (12) | C61—C62—H62 | 121.1 |
C14—C15—H15 | 120.3 | C63—C62—H62 | 121.1 |
C16—C15—H15 | 120.3 | C64—C63—C62 | 121.5 (11) |
C11—C16—C15 | 120.7 (11) | C64—C63—H63 | 119.3 |
C11—C16—H16 | 119.7 | C62—C63—H63 | 119.3 |
C15—C16—H16 | 119.7 | C63—C64—C59 | 119.7 (10) |
C18—C17—C22 | 117.4 (9) | C63—C64—H64 | 120.2 |
C18—C17—P2 | 121.4 (8) | C59—C64—H64 | 120.2 |
C22—C17—P2 | 120.7 (8) | C52—C65—H65A | 109.5 |
C17—C18—C19 | 119.6 (11) | C52—C65—H65B | 109.5 |
C17—C18—H18 | 120.2 | H65A—C65—H65B | 109.5 |
C19—C18—H18 | 120.2 | C52—C65—H65C | 109.5 |
C20—C19—C18 | 121.7 (12) | H65A—C65—H65C | 109.5 |
C20—C19—H19 | 119.1 | H65B—C65—H65C | 109.5 |
C18—C19—H19 | 119.1 | C71—C66—C67 | 117.1 (9) |
C21—C20—C19 | 117.6 (11) | C71—C66—P3 | 120.5 (7) |
C21—C20—H20 | 121.2 | C67—C66—P3 | 122.4 (7) |
C19—C20—H20 | 121.2 | C68—C67—C66 | 120.6 (9) |
C20—C21—C22 | 122.2 (12) | C68—C67—H67 | 119.7 |
C20—C21—H21 | 118.9 | C66—C67—H67 | 119.7 |
C22—C21—H21 | 118.9 | C67—C68—C69 | 120.5 (10) |
C21—C22—C17 | 121.5 (11) | C67—C68—H68 | 119.8 |
C21—C22—H22 | 119.3 | C69—C68—H68 | 119.8 |
C17—C22—H22 | 119.3 | C70—C69—C68 | 120.0 (10) |
C10—C23—H23A | 109.5 | C70—C69—H69 | 120.0 |
C10—C23—H23B | 109.5 | C68—C69—H69 | 120.0 |
H23A—C23—H23B | 109.5 | C71—C70—C69 | 119.7 (10) |
C10—C23—H23C | 109.5 | C71—C70—H70 | 120.1 |
H23A—C23—H23C | 109.5 | C69—C70—H70 | 120.1 |
H23B—C23—H23C | 109.5 | C70—C71—C66 | 122.0 (10) |
C29—C24—C25 | 116.2 (9) | C70—C71—H71 | 119.0 |
C29—C24—P1 | 121.8 (8) | C66—C71—H71 | 119.0 |
C25—C24—P1 | 121.5 (8) | C77—C72—C73 | 120.1 (9) |
C26—C25—C24 | 121.3 (10) | C77—C72—P3 | 120.4 (7) |
C26—C25—H25 | 119.4 | C73—C72—P3 | 118.5 (7) |
C24—C25—H25 | 119.4 | C74—C73—C72 | 119.0 (9) |
C25—C26—C27 | 118.7 (11) | C74—C73—H73 | 120.5 |
C25—C26—H26 | 120.7 | C72—C73—H73 | 120.5 |
C27—C26—H26 | 120.7 | C75—C74—C73 | 121.6 (10) |
C28—C27—C26 | 121.9 (10) | C75—C74—H74 | 119.2 |
C28—C27—H27 | 119.0 | C73—C74—H74 | 119.2 |
C26—C27—H27 | 119.0 | C74—C75—C76 | 121.4 (10) |
C29—C28—C27 | 117.5 (11) | C74—C75—H75 | 119.3 |
C29—C28—H28 | 121.2 | C76—C75—H75 | 119.3 |
C27—C28—H28 | 121.2 | C75—C76—C77 | 118.5 (10) |
C28—C29—C24 | 124.1 (11) | C75—C76—H76 | 120.7 |
C28—C29—H29 | 117.9 | C77—C76—H76 | 120.7 |
C24—C29—H29 | 117.9 | C72—C77—C76 | 119.3 (9) |
C31—C30—C35 | 119.3 (9) | C72—C77—H77 | 120.4 |
C31—C30—P1 | 119.7 (7) | C76—C77—H77 | 120.4 |
C35—C30—P1 | 121.1 (7) | C79—C78—C83 | 106.7 (8) |
C32—C31—C30 | 120.6 (10) | C79—C78—Rh2 | 71.0 (6) |
C32—C31—H31 | 119.7 | C83—C78—Rh2 | 94.6 (6) |
C30—C31—H31 | 119.7 | C79—C78—H78 | 126.7 |
C31—C32—C33 | 120.4 (10) | C83—C78—H78 | 126.7 |
C31—C32—H32 | 119.8 | Rh2—C78—H78 | 101.9 |
C33—C32—H32 | 119.8 | C78—C79—C80 | 106.2 (8) |
C34—C33—C32 | 119.5 (10) | C78—C79—Rh2 | 73.6 (6) |
C34—C33—H33 | 120.2 | C80—C79—Rh2 | 95.4 (5) |
C32—C33—H33 | 120.2 | C78—C79—H79 | 126.9 |
C35—C34—C33 | 120.9 (11) | C80—C79—H79 | 126.9 |
C35—C34—H34 | 119.5 | Rh2—C79—H79 | 99.0 |
C33—C34—H34 | 119.5 | C81—C80—C84 | 98.9 (8) |
C34—C35—C30 | 119.2 (10) | C81—C80—C79 | 102.5 (7) |
C34—C35—H35 | 120.4 | C84—C80—C79 | 100.3 (8) |
C30—C35—H35 | 120.4 | C81—C80—H80 | 117.4 |
C37—C36—C41 | 104.5 (9) | C84—C80—H80 | 117.4 |
C37—C36—Rh1 | 71.9 (6) | C79—C80—H80 | 117.4 |
C41—C36—Rh1 | 96.7 (7) | C82—C81—C80 | 106.8 (8) |
C37—C36—H36 | 127.7 | C82—C81—Rh2 | 71.2 (6) |
C41—C36—H36 | 127.7 | C80—C81—Rh2 | 95.3 (6) |
Rh1—C36—H36 | 99.1 | C82—C81—H81 | 126.6 |
C36—C37—C38 | 108.9 (9) | C80—C81—H81 | 126.6 |
C36—C37—Rh1 | 71.4 (6) | Rh2—C81—H81 | 101.1 |
C38—C37—Rh1 | 97.3 (6) | C81—C82—C83 | 105.3 (9) |
C36—C37—H37 | 125.6 | C81—C82—Rh2 | 72.4 (6) |
C38—C37—H37 | 125.6 | C83—C82—Rh2 | 96.8 (6) |
Rh1—C37—H37 | 99.5 | C81—C82—H82 | 127.3 |
C37—C38—C39 | 102.0 (8) | C83—C82—H82 | 127.3 |
C37—C38—C42 | 99.0 (9) | Rh2—C82—H82 | 98.7 |
C39—C38—C42 | 97.4 (9) | C84—C83—C82 | 102.0 (8) |
C37—C38—H38 | 118.2 | C84—C83—C78 | 100.5 (8) |
C39—C38—H38 | 118.2 | C82—C83—C78 | 102.9 (7) |
C42—C38—H38 | 118.2 | C84—C83—H83 | 116.3 |
C40—C39—C38 | 107.9 (9) | C82—C83—H83 | 116.3 |
C40—C39—Rh1 | 73.0 (6) | C78—C83—H83 | 116.3 |
C38—C39—Rh1 | 96.1 (7) | C83—C84—C80 | 93.1 (7) |
C40—C39—H39 | 126.1 | C83—C84—H84A | 113.1 |
C38—C39—H39 | 126.1 | C80—C84—H84A | 113.1 |
Rh1—C39—H39 | 99.1 | C83—C84—H84B | 113.1 |
C39—C40—C41 | 106.5 (10) | C80—C84—H84B | 113.1 |
C39—C40—Rh1 | 71.2 (6) | H84A—C84—H84B | 110.5 |
C41—C40—Rh1 | 96.5 (6) | F3—B1—F4 | 111.2 (10) |
C39—C40—H40 | 126.8 | F3—B1—F1 | 109.8 (10) |
C41—C40—H40 | 126.8 | F4—B1—F1 | 109.1 (9) |
Rh1—C40—H40 | 100.1 | F3—B1—F2 | 109.9 (9) |
C42—C41—C40 | 99.1 (10) | F4—B1—F2 | 108.2 (10) |
C42—C41—C36 | 99.6 (9) | F1—B1—F2 | 108.4 (10) |
C40—C41—C36 | 101.4 (8) | F6—B2—F6i | 113 (2) |
C42—C41—H41 | 117.8 | F6—B2—F5 | 106.7 (7) |
C40—C41—H41 | 117.8 | F6i—B2—F5 | 110.3 (7) |
C36—C41—H41 | 117.8 | F6—B2—F5i | 110.3 (7) |
C41—C42—C38 | 97.1 (9) | F6i—B2—F5i | 106.7 (7) |
C41—C42—H42A | 112.3 | F5—B2—F5i | 110 (2) |
C38—C42—H42A | 112.3 | F7ii—B3—F7 | 110.0 (14) |
C41—C42—H42B | 112.3 | F7ii—B3—F8 | 109.5 (4) |
C38—C42—H42B | 112.3 | F7—B3—F8 | 109.4 (3) |
H42A—C42—H42B | 109.9 | F7ii—B3—F8ii | 109.4 (3) |
C82—Rh2—C79 | 77.9 (4) | F7—B3—F8ii | 109.5 (4) |
C82—Rh2—C81 | 36.4 (4) | F8—B3—F8ii | 109.0 (14) |
C79—Rh2—C81 | 66.4 (4) | O7—C85—H85A | 109.3 |
C82—Rh2—C78 | 65.6 (4) | O7—C85—H85B | 109.5 |
C79—Rh2—C78 | 35.5 (3) | H85A—C85—H85B | 109.5 |
C81—Rh2—C78 | 77.2 (4) | O7—C85—H85C | 109.6 |
C82—Rh2—P4 | 99.4 (3) | H85A—C85—H85C | 109.5 |
C79—Rh2—P4 | 154.2 (3) | H85B—C85—H85C | 109.4 |
C81—Rh2—P4 | 95.9 (3) | C85—O7—H7A | 104.1 |
C78—Rh2—P4 | 162.7 (3) | O8—C86—H86A | 109.5 |
C82—Rh2—P3 | 155.8 (3) | O8—C86—H86B | 109.4 |
C79—Rh2—P3 | 101.4 (2) | H86A—C86—H86B | 109.7 |
C81—Rh2—P3 | 163.5 (3) | O8—C86—H86C | 109.4 |
C78—Rh2—P3 | 99.5 (3) | H86A—C86—H86C | 109.4 |
P4—Rh2—P3 | 91.42 (9) | H86B—C86—H86C | 109.5 |
C45—Cr2—C44 | 85.9 (5) | C86—O8—H8A | 108.0 |
Symmetry codes: (i) y, x, −z; (ii) y+1, x−1, −z. |
(
R,
R)-tricarbonyl-1
κ3C-{µ-1(
η6):2
κ2P,
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 (III)
top
Crystal data top
[CrRh(C8H12)(C32H28P2)(CO)3]·BF4·1.5CH4O | F(000) = 978 |
Mr = 956.47 | Dx = 1.475 Mg m−3 |
Monoclinic, P21 | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: P 2yb | Cell parameters from 5000 reflections |
a = 11.262 (2) Å | θ = 4–20° |
b = 14.116 (3) Å | µ = 0.77 mm−1 |
c = 14.226 (3) Å | T = 200 K |
β = 107.81 (3)° | Prism, red |
V = 2153.2 (7) Å3 | 0.50 × 0.30 × 0.30 mm |
Z = 2 | |
Data collection top
Stoe IPDS image-plate diffractometer | 6454 independent reflections |
Radiation source: fine-focus sealed tube | 5511 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.035 |
φ scans | θmax = 24.4°, θmin = 2.0° |
Absorption correction: empirical (using intensity measurements) (ABSCOR; Stoe & Cie, 1995) | h = −12→12 |
Tmin = 0.700, Tmax = 0.802 | k = −16→15 |
11684 measured reflections | l = −16→16 |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.034 | H-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 reflections | Δρmax = 0.63 e Å−3 |
532 parameters | Δρmin = −0.34 e Å−3 |
3 restraints | Absolute structure: Flack (1983), 2773 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.00 (2) |
Special details top
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell e.s.d.'s are taken
into account individually in the estimation of e.s.d.'s in distances, angles
and torsion angles; correlations between e.s.d.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s.
planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor
wR and goodness of fit S are based on F2, conventional
R-factors R are based on F, with F set to zero for
negative F2. The threshold expression of F2 >
σ(F2) is used only for calculating R-factors(gt) etc.
and is not relevant to the choice of reflections for refinement.
R-factors based on F2 are statistically about twice as large
as those based on F, and R- factors based on ALL data will be
even larger. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Rh1 | 0.48626 (3) | 0.63969 (2) | 0.77159 (2) | 0.02141 (10) | |
Cr1 | 0.34290 (8) | 0.25708 (6) | 0.71544 (6) | 0.0234 (2) | |
P1 | 0.33189 (12) | 0.52834 (10) | 0.74748 (10) | 0.0202 (3) | |
P2 | 0.63296 (12) | 0.52357 (10) | 0.81948 (10) | 0.0222 (3) | |
O1 | 0.3343 (5) | 0.0440 (3) | 0.6990 (4) | 0.0573 (14) | |
O2 | 0.0743 (3) | 0.2426 (3) | 0.7071 (3) | 0.0462 (9) | |
O3 | 0.4147 (4) | 0.2278 (3) | 0.9335 (3) | 0.0504 (11) | |
C1 | 0.3702 (4) | 0.4137 (3) | 0.7007 (3) | 0.0201 (10) | |
C2 | 0.2925 (4) | 0.3750 (3) | 0.6104 (3) | 0.0258 (11) | |
H2A | 0.2050 | 0.3950 | 0.5865 | 0.031* | |
C3 | 0.3309 (5) | 0.2999 (3) | 0.5630 (3) | 0.0294 (12) | |
H3A | 0.2713 | 0.2687 | 0.5065 | 0.035* | |
C4 | 0.4482 (5) | 0.2599 (4) | 0.6068 (3) | 0.0305 (11) | |
H4A | 0.4694 | 0.1999 | 0.5810 | 0.037* | |
C5 | 0.5255 (5) | 0.2944 (3) | 0.6964 (4) | 0.0267 (11) | |
H5A | 0.5988 | 0.2570 | 0.7319 | 0.032* | |
C6 | 0.4883 (4) | 0.3692 (3) | 0.7469 (3) | 0.0224 (11) | |
C7 | 0.5741 (4) | 0.4053 (3) | 0.8439 (3) | 0.0209 (11) | |
H7A | 0.5226 | 0.4160 | 0.8873 | 0.025* | |
C8 | 0.6765 (5) | 0.3348 (4) | 0.8969 (4) | 0.0321 (12) | |
H8A | 0.6390 | 0.2760 | 0.9065 | 0.048* | |
H8B | 0.7237 | 0.3603 | 0.9598 | 0.048* | |
H8C | 0.7309 | 0.3240 | 0.8575 | 0.048* | |
C9 | 0.3397 (5) | 0.1269 (5) | 0.7041 (3) | 0.0391 (14) | |
C10 | 0.1783 (5) | 0.2485 (4) | 0.7096 (4) | 0.0333 (12) | |
C11 | 0.3860 (5) | 0.2394 (3) | 0.8494 (4) | 0.0310 (12) | |
C12 | 0.2957 (4) | 0.5065 (3) | 0.8624 (3) | 0.0244 (11) | |
C13 | 0.3506 (5) | 0.5640 (3) | 0.9442 (3) | 0.0273 (11) | |
H13A | 0.4092 | 0.6093 | 0.9408 | 0.033* | |
C14 | 0.3186 (5) | 0.5541 (4) | 1.0299 (4) | 0.0373 (13) | |
H14A | 0.3560 | 0.5924 | 1.0841 | 0.045* | |
C15 | 0.2321 (5) | 0.4882 (4) | 1.0354 (4) | 0.0401 (14) | |
H15A | 0.2101 | 0.4823 | 1.0930 | 0.048* | |
C16 | 0.1777 (5) | 0.4307 (4) | 0.9563 (4) | 0.0394 (13) | |
H16A | 0.1193 | 0.3857 | 0.9608 | 0.047* | |
C17 | 0.2092 (5) | 0.4389 (4) | 0.8694 (4) | 0.0320 (12) | |
H17A | 0.1725 | 0.3993 | 0.8162 | 0.038* | |
C18 | 0.1834 (4) | 0.5623 (3) | 0.6595 (3) | 0.0214 (10) | |
C19 | 0.0786 (4) | 0.5843 (3) | 0.6864 (4) | 0.0306 (12) | |
H19A | 0.0792 | 0.5749 | 0.7512 | 0.037* | |
C20 | −0.0277 (4) | 0.6203 (4) | 0.6174 (4) | 0.0406 (15) | |
H20A | −0.0971 | 0.6360 | 0.6366 | 0.049* | |
C21 | −0.0302 (4) | 0.6326 (6) | 0.5222 (4) | 0.0463 (13) | |
H21A | −0.1028 | 0.6546 | 0.4762 | 0.056* | |
C22 | 0.0728 (5) | 0.6133 (3) | 0.4921 (4) | 0.0364 (14) | |
H22A | 0.0711 | 0.6241 | 0.4272 | 0.044* | |
C23 | 0.1791 (5) | 0.5774 (3) | 0.5607 (4) | 0.0312 (12) | |
H23A | 0.2486 | 0.5632 | 0.5411 | 0.037* | |
C24 | 0.6969 (4) | 0.4961 (3) | 0.7200 (4) | 0.0257 (11) | |
C25 | 0.8037 (5) | 0.4397 (4) | 0.7324 (4) | 0.0375 (13) | |
H25A | 0.8531 | 0.4221 | 0.7952 | 0.045* | |
C26 | 0.8340 (6) | 0.4108 (4) | 0.6489 (5) | 0.0519 (17) | |
H26A | 0.9035 | 0.3726 | 0.6560 | 0.062* | |
C27 | 0.7622 (6) | 0.4382 (5) | 0.5558 (5) | 0.0539 (17) | |
H27A | 0.7833 | 0.4178 | 0.5008 | 0.065* | |
C28 | 0.6621 (5) | 0.4942 (4) | 0.5440 (4) | 0.0405 (14) | |
H28A | 0.6158 | 0.5136 | 0.4810 | 0.049* | |
C29 | 0.6273 (5) | 0.5233 (4) | 0.6253 (4) | 0.0298 (11) | |
H29A | 0.5571 | 0.5611 | 0.6161 | 0.036* | |
C30 | 0.7602 (4) | 0.5489 (3) | 0.9305 (4) | 0.0294 (12) | |
C31 | 0.8741 (5) | 0.5863 (4) | 0.9282 (5) | 0.0412 (14) | |
H31A | 0.8898 | 0.5941 | 0.8682 | 0.049* | |
C32 | 0.9640 (5) | 0.6120 (4) | 1.0155 (5) | 0.0561 (19) | |
H32A | 1.0396 | 0.6372 | 1.0137 | 0.067* | |
C33 | 0.9417 (6) | 0.6006 (5) | 1.1039 (5) | 0.0602 (19) | |
H33A | 1.0031 | 0.6163 | 1.1623 | 0.072* | |
C34 | 0.8301 (6) | 0.5662 (4) | 1.1071 (4) | 0.0488 (16) | |
H34A | 0.8153 | 0.5594 | 1.1676 | 0.059* | |
C35 | 0.7393 (5) | 0.5416 (4) | 1.0219 (4) | 0.0372 (13) | |
H35A | 0.6627 | 0.5197 | 1.0251 | 0.045* | |
C36 | 0.3429 (5) | 0.7555 (5) | 0.7539 (4) | 0.0319 (13) | |
H36A | 0.2583 | 0.7323 | 0.7455 | 0.038* | |
C37 | 0.3780 (5) | 0.7511 (4) | 0.6693 (4) | 0.0337 (12) | |
H37A | 0.3130 | 0.7252 | 0.6124 | 0.040* | |
C38 | 0.4643 (6) | 0.8215 (4) | 0.6405 (4) | 0.0436 (15) | |
H38A | 0.4598 | 0.8820 | 0.6717 | 0.052* | |
H38B | 0.4346 | 0.8311 | 0.5696 | 0.052* | |
C39 | 0.6025 (6) | 0.7889 (4) | 0.6703 (4) | 0.0474 (16) | |
H39A | 0.6137 | 0.7464 | 0.6201 | 0.057* | |
H39B | 0.6554 | 0.8437 | 0.6730 | 0.057* | |
C40 | 0.6429 (5) | 0.7393 (4) | 0.7688 (4) | 0.0314 (13) | |
H40A | 0.7246 | 0.7086 | 0.7839 | 0.038* | |
C41 | 0.6073 (5) | 0.7600 (4) | 0.8505 (4) | 0.0295 (12) | |
H41A | 0.6689 | 0.7408 | 0.9126 | 0.035* | |
C42 | 0.5309 (5) | 0.8449 (4) | 0.8616 (4) | 0.0352 (13) | |
H42A | 0.5406 | 0.8946 | 0.8173 | 0.042* | |
H42B | 0.5629 | 0.8688 | 0.9285 | 0.042* | |
C43 | 0.3912 (5) | 0.8222 (4) | 0.8390 (4) | 0.0409 (14) | |
H43A | 0.3776 | 0.7945 | 0.8973 | 0.049* | |
H43B | 0.3441 | 0.8808 | 0.8246 | 0.049* | |
B1 | 0.2944 (6) | 0.5734 (5) | 0.3265 (6) | 0.0491 (18) | |
F1 | 0.3742 (5) | 0.5434 (5) | 0.2812 (4) | 0.125 (2) | |
F2 | 0.1993 (4) | 0.5114 (3) | 0.3198 (4) | 0.1059 (16) | |
F3 | 0.2351 (9) | 0.6544 (9) | 0.3038 (10) | 0.100 (4)* | 0.491 (14) |
F4 | 0.3723 (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) |
O100 | 0.0839 (4) | 0.3606 (3) | 0.3735 (4) | 0.0674 (13) | |
H100 | 0.1203 | 0.4152 | 0.3546 | 0.088* | |
C100 | −0.0335 (7) | 0.3835 (6) | 0.3807 (8) | 0.094 (3) | |
H101 | −0.0821 | 0.4133 | 0.3209 | 0.141* | |
H102 | −0.0239 | 0.4260 | 0.4353 | 0.141* | |
H103 | −0.0737 | 0.3266 | 0.3914 | 0.141* | |
O200 | 0.0229 (9) | 0.2499 (5) | 0.1956 (6) | 0.058 (2) | 0.50 |
H200 | 0.0632 | 0.2754 | 0.2591 | 0.075* | 0.50 |
C200 | 0.0024 (15) | 0.3204 (9) | 0.1265 (9) | 0.068 (4) | 0.50 |
H201 | 0.0824 | 0.3422 | 0.1205 | 0.102* | 0.50 |
H202 | −0.0403 | 0.3734 | 0.1469 | 0.102* | 0.50 |
H203 | −0.0496 | 0.2962 | 0.0626 | 0.102* | 0.50 |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Rh1 | 0.02224 (17) | 0.01532 (16) | 0.02386 (18) | 0.0007 (2) | 0.00291 (13) | 0.0010 (2) |
Cr1 | 0.0274 (4) | 0.0192 (4) | 0.0215 (4) | 0.0000 (4) | 0.0045 (3) | −0.0011 (4) |
P1 | 0.0190 (7) | 0.0165 (7) | 0.0220 (7) | 0.0016 (6) | 0.0018 (6) | −0.0001 (7) |
P2 | 0.0190 (6) | 0.0193 (7) | 0.0253 (7) | −0.0004 (6) | 0.0023 (6) | 0.0014 (6) |
O1 | 0.087 (4) | 0.008 (2) | 0.088 (4) | −0.001 (2) | 0.043 (3) | −0.006 (2) |
O2 | 0.034 (2) | 0.045 (2) | 0.057 (2) | −0.0031 (19) | 0.0103 (18) | −0.001 (2) |
O3 | 0.060 (3) | 0.063 (3) | 0.025 (2) | −0.013 (2) | 0.0076 (19) | 0.0066 (19) |
C1 | 0.024 (2) | 0.014 (2) | 0.020 (2) | −0.0022 (19) | 0.003 (2) | 0.0015 (19) |
C2 | 0.024 (2) | 0.023 (3) | 0.024 (3) | 0.000 (2) | −0.001 (2) | 0.003 (2) |
C3 | 0.044 (3) | 0.022 (3) | 0.021 (3) | −0.001 (2) | 0.007 (2) | −0.003 (2) |
C4 | 0.044 (3) | 0.021 (2) | 0.030 (3) | 0.000 (2) | 0.017 (2) | −0.007 (2) |
C5 | 0.032 (3) | 0.021 (2) | 0.028 (3) | 0.003 (2) | 0.010 (2) | −0.002 (2) |
C6 | 0.025 (3) | 0.018 (2) | 0.022 (3) | −0.004 (2) | 0.004 (2) | 0.001 (2) |
C7 | 0.022 (3) | 0.020 (3) | 0.018 (3) | 0.002 (2) | 0.002 (2) | 0.006 (2) |
C8 | 0.029 (3) | 0.025 (3) | 0.034 (3) | 0.011 (2) | −0.002 (2) | 0.007 (2) |
C9 | 0.040 (3) | 0.050 (4) | 0.032 (3) | 0.000 (3) | 0.018 (2) | 0.000 (3) |
C10 | 0.041 (3) | 0.024 (3) | 0.032 (3) | 0.001 (3) | 0.007 (2) | −0.001 (2) |
C11 | 0.032 (3) | 0.018 (3) | 0.041 (3) | −0.011 (2) | 0.007 (2) | 0.000 (2) |
C12 | 0.025 (2) | 0.021 (3) | 0.026 (3) | 0.004 (2) | 0.005 (2) | 0.004 (2) |
C13 | 0.034 (3) | 0.022 (3) | 0.025 (3) | 0.003 (2) | 0.008 (2) | 0.003 (2) |
C14 | 0.055 (4) | 0.030 (3) | 0.025 (3) | 0.009 (3) | 0.009 (3) | −0.003 (2) |
C15 | 0.049 (3) | 0.042 (3) | 0.036 (3) | 0.015 (3) | 0.023 (3) | 0.010 (3) |
C16 | 0.041 (3) | 0.044 (3) | 0.038 (3) | −0.002 (3) | 0.020 (3) | 0.004 (3) |
C17 | 0.027 (3) | 0.037 (3) | 0.031 (3) | −0.006 (2) | 0.007 (2) | 0.000 (2) |
C18 | 0.018 (2) | 0.015 (2) | 0.028 (3) | −0.0047 (19) | 0.001 (2) | −0.002 (2) |
C19 | 0.029 (3) | 0.027 (3) | 0.033 (3) | 0.001 (2) | 0.006 (2) | −0.001 (2) |
C20 | 0.026 (2) | 0.037 (4) | 0.052 (3) | 0.011 (3) | 0.003 (2) | 0.002 (3) |
C21 | 0.032 (3) | 0.047 (3) | 0.044 (3) | 0.010 (4) | −0.012 (2) | 0.007 (4) |
C22 | 0.038 (3) | 0.034 (4) | 0.027 (3) | 0.007 (2) | −0.005 (2) | 0.004 (2) |
C23 | 0.032 (3) | 0.024 (3) | 0.034 (3) | 0.006 (2) | 0.004 (2) | 0.004 (2) |
C24 | 0.021 (2) | 0.019 (2) | 0.036 (3) | −0.001 (2) | 0.008 (2) | −0.003 (2) |
C25 | 0.024 (3) | 0.037 (3) | 0.054 (4) | 0.007 (2) | 0.016 (3) | −0.003 (3) |
C26 | 0.039 (3) | 0.046 (4) | 0.079 (5) | 0.004 (3) | 0.029 (4) | −0.013 (4) |
C27 | 0.055 (4) | 0.062 (4) | 0.055 (4) | −0.007 (3) | 0.033 (4) | −0.025 (4) |
C28 | 0.049 (4) | 0.037 (3) | 0.037 (3) | −0.011 (3) | 0.015 (3) | −0.013 (3) |
C29 | 0.031 (3) | 0.031 (3) | 0.029 (3) | −0.001 (2) | 0.011 (2) | −0.009 (2) |
C30 | 0.019 (2) | 0.024 (3) | 0.037 (3) | 0.008 (2) | −0.003 (2) | 0.003 (2) |
C31 | 0.029 (3) | 0.034 (3) | 0.057 (4) | 0.002 (3) | 0.008 (3) | −0.012 (3) |
C32 | 0.026 (3) | 0.043 (4) | 0.083 (5) | 0.001 (2) | −0.006 (3) | −0.021 (3) |
C33 | 0.045 (4) | 0.061 (4) | 0.050 (4) | 0.017 (3) | −0.021 (3) | −0.027 (3) |
C34 | 0.041 (4) | 0.054 (4) | 0.038 (3) | 0.012 (3) | −0.008 (3) | −0.008 (3) |
C35 | 0.040 (3) | 0.027 (3) | 0.041 (3) | 0.004 (3) | 0.007 (3) | −0.006 (3) |
C36 | 0.027 (3) | 0.023 (3) | 0.042 (3) | 0.002 (3) | 0.005 (3) | 0.001 (3) |
C37 | 0.038 (3) | 0.021 (3) | 0.032 (3) | 0.004 (3) | −0.004 (2) | 0.011 (2) |
C38 | 0.063 (4) | 0.025 (3) | 0.039 (3) | 0.002 (3) | 0.010 (3) | 0.012 (3) |
C39 | 0.069 (4) | 0.035 (3) | 0.041 (4) | −0.013 (3) | 0.021 (3) | 0.005 (3) |
C40 | 0.024 (3) | 0.029 (3) | 0.043 (3) | −0.008 (2) | 0.013 (2) | −0.002 (3) |
C41 | 0.027 (3) | 0.020 (2) | 0.037 (3) | −0.008 (2) | 0.004 (2) | −0.006 (3) |
C42 | 0.042 (3) | 0.031 (3) | 0.032 (3) | 0.003 (3) | 0.011 (3) | −0.006 (3) |
C43 | 0.052 (4) | 0.019 (3) | 0.052 (4) | 0.008 (3) | 0.018 (3) | −0.005 (3) |
B1 | 0.032 (4) | 0.042 (4) | 0.070 (5) | −0.007 (3) | 0.011 (4) | 0.002 (4) |
F1 | 0.112 (4) | 0.160 (6) | 0.125 (5) | −0.001 (4) | 0.071 (4) | −0.032 (4) |
F2 | 0.095 (3) | 0.087 (3) | 0.131 (4) | −0.051 (3) | 0.028 (3) | 0.008 (3) |
O100 | 0.062 (3) | 0.054 (3) | 0.083 (3) | −0.007 (2) | 0.019 (3) | 0.016 (3) |
C100 | 0.051 (5) | 0.063 (5) | 0.161 (9) | −0.010 (4) | 0.023 (5) | −0.015 (5) |
O200 | 0.121 (8) | 0.026 (4) | 0.046 (5) | −0.004 (5) | 0.053 (5) | −0.003 (4) |
C200 | 0.100 (12) | 0.061 (9) | 0.040 (7) | 0.026 (8) | 0.019 (8) | −0.002 (7) |
Geometric parameters (Å, º) top
Rh1—C37 | 2.234 (5) | C22—H22A | 0.9300 |
Rh1—C41 | 2.251 (5) | C23—H23A | 0.9300 |
Rh1—C36 | 2.257 (6) | C24—C29 | 1.390 (7) |
Rh1—C40 | 2.265 (5) | C24—C25 | 1.408 (7) |
Rh1—P2 | 2.2786 (15) | C25—C26 | 1.394 (8) |
Rh1—P1 | 2.2904 (15) | C25—H25A | 0.9300 |
Cr1—C11 | 1.833 (6) | C26—C27 | 1.379 (9) |
Cr1—C10 | 1.833 (6) | C26—H26A | 0.9300 |
Cr1—C9 | 1.844 (7) | C27—C28 | 1.344 (8) |
Cr1—C2 | 2.192 (5) | C27—H27A | 0.9300 |
Cr1—C3 | 2.215 (5) | C28—C29 | 1.392 (7) |
Cr1—C4 | 2.218 (5) | C28—H28A | 0.9300 |
Cr1—C5 | 2.218 (5) | C29—H29A | 0.9300 |
Cr1—C6 | 2.222 (5) | C30—C35 | 1.395 (7) |
Cr1—C1 | 2.250 (4) | C30—C31 | 1.396 (7) |
P1—C18 | 1.820 (5) | C31—C32 | 1.389 (8) |
P1—C12 | 1.828 (5) | C31—H31A | 0.9300 |
P1—C1 | 1.851 (5) | C32—C33 | 1.365 (9) |
P2—C30 | 1.814 (5) | C32—H32A | 0.9300 |
P2—C24 | 1.815 (5) | C33—C34 | 1.361 (9) |
P2—C7 | 1.868 (5) | C33—H33A | 0.9300 |
O1—C9 | 1.172 (8) | C34—C35 | 1.370 (8) |
O2—C10 | 1.164 (6) | C34—H34A | 0.9300 |
O3—C11 | 1.152 (6) | C35—H35A | 0.9300 |
C1—C2 | 1.424 (6) | C36—C37 | 1.378 (8) |
C1—C6 | 1.435 (6) | C36—C43 | 1.499 (8) |
C2—C3 | 1.395 (7) | C36—H36A | 0.9800 |
C2—H2A | 0.9800 | C37—C38 | 1.531 (8) |
C3—C4 | 1.396 (7) | C37—H37A | 0.9800 |
C3—H3A | 0.9800 | C38—C39 | 1.553 (9) |
C4—C5 | 1.394 (7) | C38—H38A | 0.9700 |
C4—H4A | 0.9800 | C38—H38B | 0.9700 |
C5—C6 | 1.410 (7) | C39—C40 | 1.507 (8) |
C5—H5A | 0.9800 | C39—H39A | 0.9700 |
C6—C7 | 1.510 (6) | C39—H39B | 0.9700 |
C7—C8 | 1.536 (6) | C40—C41 | 1.372 (7) |
C7—H7A | 0.9800 | C40—H40A | 0.9800 |
C8—H8A | 0.9600 | C41—C42 | 1.511 (7) |
C8—H8B | 0.9600 | C41—H41A | 0.9800 |
C8—H8C | 0.9600 | C42—C43 | 1.540 (8) |
C12—C17 | 1.390 (7) | C42—H42A | 0.9700 |
C12—C13 | 1.398 (7) | C42—H42B | 0.9700 |
C13—C14 | 1.381 (7) | C43—H43A | 0.9700 |
C13—H13A | 0.9300 | C43—H43B | 0.9700 |
C14—C15 | 1.366 (7) | B1—F3 | 1.314 (14) |
C14—H14A | 0.9300 | B1—F1 | 1.326 (8) |
C15—C16 | 1.371 (8) | B1—F4' | 1.335 (12) |
C15—H15A | 0.9300 | B1—F2 | 1.363 (8) |
C16—C17 | 1.391 (7) | B1—F4 | 1.370 (11) |
C16—H16A | 0.9300 | B1—F3' | 1.465 (12) |
C17—H17A | 0.9300 | O100—C100 | 1.395 (8) |
C18—C19 | 1.383 (6) | O100—H100 | 0.9500 |
C18—C23 | 1.407 (7) | C100—H101 | 0.9572 |
C19—C20 | 1.391 (7) | C100—H102 | 0.9608 |
C19—H19A | 0.9300 | C100—H103 | 0.9565 |
C20—C21 | 1.358 (7) | O200—C200 | 1.369 (12) |
C20—H20A | 0.9300 | O200—H200 | 0.9500 |
C21—C22 | 1.381 (7) | C200—H201 | 0.9801 |
C21—H21A | 0.9300 | C200—H202 | 0.9801 |
C22—C23 | 1.388 (7) | C200—H203 | 0.9801 |
| | | |
C37—Rh1—C41 | 85.4 (2) | C16—C17—H17A | 120.1 |
C37—Rh1—C36 | 35.7 (2) | C19—C18—C23 | 118.1 (4) |
C41—Rh1—C36 | 79.2 (2) | C19—C18—P1 | 123.4 (4) |
C37—Rh1—C40 | 79.9 (2) | C23—C18—P1 | 118.1 (4) |
C41—Rh1—C40 | 35.38 (18) | C18—C19—C20 | 120.7 (5) |
C36—Rh1—C40 | 94.7 (2) | C18—C19—H19A | 119.7 |
C37—Rh1—P2 | 154.47 (14) | C20—C19—H19A | 119.7 |
C41—Rh1—P2 | 96.93 (14) | C21—C20—C19 | 120.1 (5) |
C36—Rh1—P2 | 169.41 (15) | C21—C20—H20A | 120.0 |
C40—Rh1—P2 | 87.39 (14) | C19—C20—H20A | 120.0 |
C37—Rh1—P1 | 98.48 (14) | C20—C21—C22 | 121.4 (5) |
C41—Rh1—P1 | 155.30 (14) | C20—C21—H21A | 119.3 |
C36—Rh1—P1 | 89.78 (15) | C22—C21—H21A | 119.3 |
C40—Rh1—P1 | 169.31 (14) | C21—C22—C23 | 118.7 (5) |
P2—Rh1—P1 | 89.94 (5) | C21—C22—H22A | 120.7 |
C11—Cr1—C10 | 88.9 (2) | C23—C22—H22A | 120.7 |
C11—Cr1—C9 | 87.0 (2) | C22—C23—C18 | 121.1 (5) |
C10—Cr1—C9 | 86.5 (2) | C22—C23—H23A | 119.5 |
C11—Cr1—C2 | 137.9 (2) | C18—C23—H23A | 119.5 |
C10—Cr1—C2 | 88.4 (2) | C29—C24—C25 | 119.0 (5) |
C9—Cr1—C2 | 134.7 (2) | C29—C24—P2 | 117.2 (4) |
C11—Cr1—C3 | 166.4 (2) | C25—C24—P2 | 123.4 (4) |
C10—Cr1—C3 | 102.4 (2) | C26—C25—C24 | 118.8 (5) |
C9—Cr1—C3 | 101.1 (2) | C26—C25—H25A | 120.6 |
C2—Cr1—C3 | 36.90 (17) | C24—C25—H25A | 120.6 |
C11—Cr1—C4 | 134.3 (2) | C27—C26—C25 | 120.8 (5) |
C10—Cr1—C4 | 135.9 (2) | C27—C26—H26A | 119.6 |
C9—Cr1—C4 | 87.5 (2) | C25—C26—H26A | 119.6 |
C2—Cr1—C4 | 66.04 (19) | C28—C27—C26 | 120.5 (6) |
C3—Cr1—C4 | 36.70 (18) | C28—C27—H27A | 119.8 |
C11—Cr1—C5 | 101.5 (2) | C26—C27—H27A | 119.8 |
C10—Cr1—C5 | 166.4 (2) | C27—C28—C29 | 120.6 (6) |
C9—Cr1—C5 | 102.71 (19) | C27—C28—H28A | 119.7 |
C2—Cr1—C5 | 78.05 (18) | C29—C28—H28A | 119.7 |
C3—Cr1—C5 | 66.22 (19) | C24—C29—C28 | 120.4 (5) |
C4—Cr1—C5 | 36.63 (17) | C24—C29—H29A | 119.8 |
C11—Cr1—C6 | 86.73 (19) | C28—C29—H29A | 119.8 |
C10—Cr1—C6 | 136.7 (2) | C35—C30—C31 | 117.9 (5) |
C9—Cr1—C6 | 136.1 (2) | C35—C30—P2 | 118.9 (4) |
C2—Cr1—C6 | 67.54 (17) | C31—C30—P2 | 122.8 (4) |
C3—Cr1—C6 | 79.83 (18) | C32—C31—C30 | 120.1 (6) |
C4—Cr1—C6 | 67.02 (18) | C32—C31—H31A | 119.9 |
C5—Cr1—C6 | 37.03 (17) | C30—C31—H31A | 119.9 |
C11—Cr1—C1 | 103.28 (18) | C33—C32—C31 | 120.2 (6) |
C10—Cr1—C1 | 103.0 (2) | C33—C32—H32A | 119.9 |
C9—Cr1—C1 | 165.98 (19) | C31—C32—H32A | 119.9 |
C2—Cr1—C1 | 37.35 (16) | C34—C33—C32 | 120.3 (5) |
C3—Cr1—C1 | 67.05 (17) | C34—C33—H33A | 119.9 |
C4—Cr1—C1 | 78.48 (17) | C32—C33—H33A | 119.9 |
C5—Cr1—C1 | 66.22 (17) | C33—C34—C35 | 120.6 (6) |
C6—Cr1—C1 | 37.42 (16) | C33—C34—H34A | 119.7 |
C18—P1—C12 | 104.5 (2) | C35—C34—H34A | 119.7 |
C18—P1—C1 | 104.4 (2) | C34—C35—C30 | 120.8 (5) |
C12—P1—C1 | 108.3 (2) | C34—C35—H35A | 119.6 |
C18—P1—Rh1 | 114.70 (15) | C30—C35—H35A | 119.6 |
C12—P1—Rh1 | 110.37 (16) | C37—C36—C43 | 127.2 (6) |
C1—P1—Rh1 | 113.84 (15) | C37—C36—Rh1 | 71.2 (3) |
C30—P2—C24 | 108.9 (2) | C43—C36—Rh1 | 107.1 (4) |
C30—P2—C7 | 104.2 (2) | C37—C36—H36A | 114.0 |
C24—P2—C7 | 101.6 (2) | C43—C36—H36A | 114.0 |
C30—P2—Rh1 | 115.23 (16) | Rh1—C36—H36A | 114.0 |
C24—P2—Rh1 | 110.16 (17) | C36—C37—C38 | 125.4 (5) |
C7—P2—Rh1 | 115.62 (16) | C36—C37—Rh1 | 73.0 (3) |
C2—C1—C6 | 118.3 (4) | C38—C37—Rh1 | 111.5 (3) |
C2—C1—P1 | 120.8 (3) | C36—C37—H37A | 113.3 |
C6—C1—P1 | 120.3 (3) | C38—C37—H37A | 113.3 |
C2—C1—Cr1 | 69.1 (3) | Rh1—C37—H37A | 113.3 |
C6—C1—Cr1 | 70.2 (3) | C37—C38—C39 | 113.6 (4) |
P1—C1—Cr1 | 140.6 (2) | C37—C38—H38A | 108.9 |
C3—C2—C1 | 122.1 (4) | C39—C38—H38A | 108.9 |
C3—C2—Cr1 | 72.4 (3) | C37—C38—H38B | 108.9 |
C1—C2—Cr1 | 73.5 (3) | C39—C38—H38B | 108.9 |
C3—C2—H2A | 118.6 | H38A—C38—H38B | 107.7 |
C1—C2—H2A | 118.6 | C40—C39—C38 | 112.6 (5) |
Cr1—C2—H2A | 118.6 | C40—C39—H39A | 109.1 |
C2—C3—C4 | 118.9 (4) | C38—C39—H39A | 109.1 |
C2—C3—Cr1 | 70.7 (3) | C40—C39—H39B | 109.1 |
C4—C3—Cr1 | 71.8 (3) | C38—C39—H39B | 109.1 |
C2—C3—H3A | 120.1 | H39A—C39—H39B | 107.8 |
C4—C3—H3A | 120.1 | C41—C40—C39 | 127.2 (5) |
Cr1—C3—H3A | 120.1 | C41—C40—Rh1 | 71.7 (3) |
C5—C4—C3 | 120.5 (4) | C39—C40—Rh1 | 106.9 (3) |
C5—C4—Cr1 | 71.7 (3) | C41—C40—H40A | 114.0 |
C3—C4—Cr1 | 71.5 (3) | C39—C40—H40A | 114.0 |
C5—C4—H4A | 119.2 | Rh1—C40—H40A | 114.0 |
C3—C4—H4A | 119.2 | C40—C41—C42 | 125.5 (5) |
Cr1—C4—H4A | 119.2 | C40—C41—Rh1 | 72.9 (3) |
C4—C5—C6 | 121.9 (4) | C42—C41—Rh1 | 111.9 (3) |
C4—C5—Cr1 | 71.7 (3) | C40—C41—H41A | 113.2 |
C6—C5—Cr1 | 71.6 (3) | C42—C41—H41A | 113.2 |
C4—C5—H5A | 118.4 | Rh1—C41—H41A | 113.2 |
C6—C5—H5A | 118.4 | C41—C42—C43 | 113.0 (4) |
Cr1—C5—H5A | 118.4 | C41—C42—H42A | 109.0 |
C5—C6—C1 | 118.2 (4) | C43—C42—H42A | 109.0 |
C5—C6—C7 | 120.7 (4) | C41—C42—H42B | 109.0 |
C1—C6—C7 | 121.0 (4) | C43—C42—H42B | 109.0 |
C5—C6—Cr1 | 71.3 (3) | H42A—C42—H42B | 107.8 |
C1—C6—Cr1 | 72.4 (3) | C36—C43—C42 | 113.2 (5) |
C7—C6—Cr1 | 130.6 (3) | C36—C43—H43A | 108.9 |
C6—C7—C8 | 113.8 (4) | C42—C43—H43A | 108.9 |
C6—C7—P2 | 107.3 (3) | C36—C43—H43B | 108.9 |
C8—C7—P2 | 114.5 (3) | C42—C43—H43B | 108.9 |
C6—C7—H7A | 106.9 | H43A—C43—H43B | 107.7 |
C8—C7—H7A | 106.9 | F3—B1—F1 | 121.8 (9) |
P2—C7—H7A | 106.9 | F3—B1—F4' | 73.3 (8) |
C7—C8—H8A | 109.5 | F1—B1—F4' | 122.8 (7) |
C7—C8—H8B | 109.5 | F3—B1—F2 | 102.2 (6) |
H8A—C8—H8B | 109.5 | F1—B1—F2 | 113.3 (7) |
C7—C8—H8C | 109.5 | F4'—B1—F2 | 115.9 (7) |
H8A—C8—H8C | 109.5 | F3—B1—F4 | 108.8 (8) |
H8B—C8—H8C | 109.5 | F1—B1—F4 | 99.9 (7) |
O1—C9—Cr1 | 177.3 (4) | F2—B1—F4 | 110.8 (7) |
O2—C10—Cr1 | 179.1 (5) | F1—B1—F3' | 90.0 (7) |
O3—C11—Cr1 | 179.0 (5) | F4'—B1—F3' | 103.3 (8) |
C17—C12—C13 | 118.7 (4) | F2—B1—F3' | 105.2 (6) |
C17—C12—P1 | 122.2 (4) | F4—B1—F3' | 134.7 (8) |
C13—C12—P1 | 118.9 (3) | C100—O100—H100 | 109.5 |
C14—C13—C12 | 120.5 (5) | O100—C100—H101 | 109.5 |
C14—C13—H13A | 119.8 | O100—C100—H102 | 109.2 |
C12—C13—H13A | 119.8 | H101—C100—H102 | 109.6 |
C15—C14—C13 | 120.2 (5) | O100—C100—H103 | 108.8 |
C15—C14—H14A | 119.9 | H101—C100—H103 | 110.0 |
C13—C14—H14A | 119.9 | H102—C100—H103 | 109.7 |
C14—C15—C16 | 120.3 (5) | C200—O200—H200 | 109.5 |
C14—C15—H15A | 119.9 | O200—C200—H201 | 109.5 |
C16—C15—H15A | 119.9 | O200—C200—H202 | 109.5 |
C15—C16—C17 | 120.5 (5) | H201—C200—H202 | 109.5 |
C15—C16—H16A | 119.7 | O200—C200—H203 | 109.5 |
C17—C16—H16A | 119.7 | H201—C200—H203 | 109.5 |
C12—C17—C16 | 119.7 (5) | H202—C200—H203 | 109.5 |
C12—C17—H17A | 120.1 | | |
| | | |
C37—Rh1—P1—C18 | 0.5 (2) | P1—C1—C6—Cr1 | 137.8 (3) |
C41—Rh1—P1—C18 | 98.1 (4) | C11—Cr1—C6—C5 | 114.0 (3) |
C36—Rh1—P1—C18 | 35.3 (2) | C10—Cr1—C6—C5 | −161.1 (3) |
C40—Rh1—P1—C18 | −79.8 (8) | C9—Cr1—C6—C5 | 31.7 (4) |
P2—Rh1—P1—C18 | −155.27 (17) | C2—Cr1—C6—C5 | −100.1 (3) |
C37—Rh1—P1—C12 | −117.2 (2) | C3—Cr1—C6—C5 | −63.7 (3) |
C41—Rh1—P1—C12 | −19.6 (4) | C4—Cr1—C6—C5 | −27.7 (3) |
C36—Rh1—P1—C12 | −82.4 (2) | C1—Cr1—C6—C5 | −129.1 (4) |
C40—Rh1—P1—C12 | 162.5 (8) | C11—Cr1—C6—C1 | −117.0 (3) |
P2—Rh1—P1—C12 | 87.03 (17) | C10—Cr1—C6—C1 | −32.1 (4) |
C37—Rh1—P1—C1 | 120.8 (2) | C9—Cr1—C6—C1 | 160.8 (3) |
C41—Rh1—P1—C1 | −141.7 (4) | C2—Cr1—C6—C1 | 28.9 (3) |
C36—Rh1—P1—C1 | 155.6 (2) | C3—Cr1—C6—C1 | 65.3 (3) |
C40—Rh1—P1—C1 | 40.4 (8) | C4—Cr1—C6—C1 | 101.4 (3) |
P2—Rh1—P1—C1 | −35.04 (16) | C5—Cr1—C6—C1 | 129.1 (4) |
C37—Rh1—P2—C30 | 116.2 (4) | C11—Cr1—C6—C7 | −1.0 (4) |
C41—Rh1—P2—C30 | 22.3 (2) | C10—Cr1—C6—C7 | 83.9 (5) |
C36—Rh1—P2—C30 | −45.4 (9) | C9—Cr1—C6—C7 | −83.2 (5) |
C40—Rh1—P2—C30 | 56.4 (2) | C2—Cr1—C6—C7 | 144.9 (5) |
P1—Rh1—P2—C30 | −133.9 (2) | C3—Cr1—C6—C7 | −178.7 (5) |
C37—Rh1—P2—C24 | −7.5 (4) | C4—Cr1—C6—C7 | −142.6 (5) |
C41—Rh1—P2—C24 | −101.4 (2) | C5—Cr1—C6—C7 | −114.9 (5) |
C36—Rh1—P2—C24 | −169.2 (9) | C1—Cr1—C6—C7 | 116.0 (5) |
C40—Rh1—P2—C24 | −67.3 (2) | C5—C6—C7—C8 | −20.4 (6) |
P1—Rh1—P2—C24 | 102.34 (18) | C1—C6—C7—C8 | 163.5 (4) |
C37—Rh1—P2—C7 | −122.0 (4) | Cr1—C6—C7—C8 | 70.8 (6) |
C41—Rh1—P2—C7 | 144.1 (2) | C5—C6—C7—P2 | 107.3 (4) |
C36—Rh1—P2—C7 | 76.3 (9) | C1—C6—C7—P2 | −68.7 (5) |
C40—Rh1—P2—C7 | 178.2 (2) | Cr1—C6—C7—P2 | −161.5 (3) |
P1—Rh1—P2—C7 | −12.14 (18) | C30—P2—C7—C6 | −167.3 (3) |
C18—P1—C1—C2 | 3.5 (4) | C24—P2—C7—C6 | −54.1 (4) |
C12—P1—C1—C2 | 114.5 (4) | Rh1—P2—C7—C6 | 65.2 (3) |
Rh1—P1—C1—C2 | −122.4 (3) | C30—P2—C7—C8 | −39.9 (4) |
C18—P1—C1—C6 | 174.1 (4) | C24—P2—C7—C8 | 73.3 (4) |
C12—P1—C1—C6 | −75.0 (4) | Rh1—P2—C7—C8 | −167.5 (3) |
Rh1—P1—C1—C6 | 48.2 (4) | C18—P1—C12—C17 | 59.2 (4) |
C18—P1—C1—Cr1 | −90.6 (4) | C1—P1—C12—C17 | −51.8 (5) |
C12—P1—C1—Cr1 | 20.3 (4) | Rh1—P1—C12—C17 | −177.0 (4) |
Rh1—P1—C1—Cr1 | 143.5 (3) | C18—P1—C12—C13 | −116.5 (4) |
C11—Cr1—C1—C2 | −161.4 (3) | C1—P1—C12—C13 | 132.6 (4) |
C10—Cr1—C1—C2 | −69.4 (3) | Rh1—P1—C12—C13 | 7.3 (4) |
C9—Cr1—C1—C2 | 62.3 (9) | C17—C12—C13—C14 | −0.5 (7) |
C3—Cr1—C1—C2 | 28.8 (3) | P1—C12—C13—C14 | 175.3 (4) |
C4—Cr1—C1—C2 | 65.4 (3) | C12—C13—C14—C15 | −0.4 (8) |
C5—Cr1—C1—C2 | 101.8 (3) | C13—C14—C15—C16 | 0.8 (8) |
C6—Cr1—C1—C2 | 132.5 (4) | C14—C15—C16—C17 | −0.3 (8) |
C11—Cr1—C1—C6 | 66.1 (3) | C13—C12—C17—C16 | 1.0 (7) |
C10—Cr1—C1—C6 | 158.1 (3) | P1—C12—C17—C16 | −174.7 (4) |
C9—Cr1—C1—C6 | −70.2 (9) | C15—C16—C17—C12 | −0.6 (8) |
C2—Cr1—C1—C6 | −132.5 (4) | C12—P1—C18—C19 | 11.9 (4) |
C3—Cr1—C1—C6 | −103.8 (3) | C1—P1—C18—C19 | 125.7 (4) |
C4—Cr1—C1—C6 | −67.1 (3) | Rh1—P1—C18—C19 | −109.0 (4) |
C5—Cr1—C1—C6 | −30.7 (3) | C12—P1—C18—C23 | −175.6 (4) |
C11—Cr1—C1—P1 | −47.8 (4) | C1—P1—C18—C23 | −61.9 (4) |
C10—Cr1—C1—P1 | 44.2 (4) | Rh1—P1—C18—C23 | 63.4 (4) |
C9—Cr1—C1—P1 | 175.9 (7) | C23—C18—C19—C20 | 0.0 (7) |
C2—Cr1—C1—P1 | 113.6 (5) | P1—C18—C19—C20 | 172.5 (4) |
C3—Cr1—C1—P1 | 142.3 (4) | C18—C19—C20—C21 | 1.2 (8) |
C4—Cr1—C1—P1 | 179.0 (4) | C19—C20—C21—C22 | −2.4 (10) |
C5—Cr1—C1—P1 | −144.6 (4) | C20—C21—C22—C23 | 2.3 (10) |
C6—Cr1—C1—P1 | −113.9 (5) | C21—C22—C23—C18 | −1.1 (8) |
C6—C1—C2—C3 | −4.2 (7) | C19—C18—C23—C22 | 0.0 (7) |
P1—C1—C2—C3 | 166.5 (4) | P1—C18—C23—C22 | −172.9 (4) |
Cr1—C1—C2—C3 | −56.2 (4) | C30—P2—C24—C29 | −146.6 (4) |
C6—C1—C2—Cr1 | 51.9 (4) | C7—P2—C24—C29 | 103.8 (4) |
P1—C1—C2—Cr1 | −137.3 (3) | Rh1—P2—C24—C29 | −19.3 (4) |
C11—Cr1—C2—C3 | 160.1 (3) | C30—P2—C24—C25 | 41.2 (5) |
C10—Cr1—C2—C3 | −113.4 (3) | C7—P2—C24—C25 | −68.4 (5) |
C9—Cr1—C2—C3 | −30.0 (4) | Rh1—P2—C24—C25 | 168.5 (4) |
C4—Cr1—C2—C3 | 29.6 (3) | C29—C24—C25—C26 | −1.8 (8) |
C5—Cr1—C2—C3 | 66.1 (3) | P2—C24—C25—C26 | 170.2 (4) |
C6—Cr1—C2—C3 | 103.4 (3) | C24—C25—C26—C27 | 1.2 (9) |
C1—Cr1—C2—C3 | 132.4 (4) | C25—C26—C27—C28 | 0.6 (10) |
C11—Cr1—C2—C1 | 27.6 (4) | C26—C27—C28—C29 | −1.8 (9) |
C10—Cr1—C2—C1 | 114.2 (3) | C25—C24—C29—C28 | 0.7 (7) |
C9—Cr1—C2—C1 | −162.4 (3) | P2—C24—C29—C28 | −171.8 (4) |
C3—Cr1—C2—C1 | −132.4 (4) | C27—C28—C29—C24 | 1.1 (8) |
C4—Cr1—C2—C1 | −102.8 (3) | C24—P2—C30—C35 | −159.4 (4) |
C5—Cr1—C2—C1 | −66.3 (3) | C7—P2—C30—C35 | −51.5 (4) |
C6—Cr1—C2—C1 | −29.0 (3) | Rh1—P2—C30—C35 | 76.3 (4) |
C1—C2—C3—C4 | 1.6 (7) | C24—P2—C30—C31 | 28.6 (5) |
Cr1—C2—C3—C4 | −55.1 (4) | C7—P2—C30—C31 | 136.4 (4) |
C1—C2—C3—Cr1 | 56.7 (4) | Rh1—P2—C30—C31 | −95.8 (4) |
C11—Cr1—C3—C2 | −75.7 (10) | C35—C30—C31—C32 | 2.1 (8) |
C10—Cr1—C3—C2 | 70.0 (3) | P2—C30—C31—C32 | 174.3 (4) |
C9—Cr1—C3—C2 | 158.7 (3) | C30—C31—C32—C33 | 0.2 (8) |
C4—Cr1—C3—C2 | −130.9 (4) | C31—C32—C33—C34 | −1.7 (9) |
C5—Cr1—C3—C2 | −102.1 (3) | C32—C33—C34—C35 | 0.8 (9) |
C6—Cr1—C3—C2 | −65.9 (3) | C33—C34—C35—C30 | 1.7 (9) |
C1—Cr1—C3—C2 | −29.1 (3) | C31—C30—C35—C34 | −3.1 (8) |
C11—Cr1—C3—C4 | 55.2 (10) | P2—C30—C35—C34 | −175.6 (4) |
C10—Cr1—C3—C4 | −159.1 (3) | C41—Rh1—C36—C37 | 97.3 (4) |
C9—Cr1—C3—C4 | −70.3 (3) | C40—Rh1—C36—C37 | 65.4 (3) |
C2—Cr1—C3—C4 | 130.9 (4) | P2—Rh1—C36—C37 | 166.6 (7) |
C5—Cr1—C3—C4 | 28.8 (3) | P1—Rh1—C36—C37 | −104.9 (3) |
C6—Cr1—C3—C4 | 65.0 (3) | C37—Rh1—C36—C43 | −124.3 (6) |
C1—Cr1—C3—C4 | 101.8 (3) | C41—Rh1—C36—C43 | −27.0 (4) |
C2—C3—C4—C5 | 0.0 (7) | C40—Rh1—C36—C43 | −58.9 (4) |
Cr1—C3—C4—C5 | −54.5 (4) | P2—Rh1—C36—C43 | 42.3 (12) |
C2—C3—C4—Cr1 | 54.5 (4) | P1—Rh1—C36—C43 | 130.8 (4) |
C11—Cr1—C4—C5 | −32.0 (4) | C43—C36—C37—C38 | −7.1 (9) |
C10—Cr1—C4—C5 | 162.4 (3) | Rh1—C36—C37—C38 | −104.7 (5) |
C9—Cr1—C4—C5 | −115.3 (3) | C43—C36—C37—Rh1 | 97.6 (6) |
C2—Cr1—C4—C5 | 102.6 (3) | C41—Rh1—C37—C36 | −77.8 (3) |
C3—Cr1—C4—C5 | 132.3 (4) | C40—Rh1—C37—C36 | −113.1 (4) |
C6—Cr1—C4—C5 | 28.0 (3) | P2—Rh1—C37—C36 | −174.3 (3) |
C1—Cr1—C4—C5 | 65.4 (3) | P1—Rh1—C37—C36 | 77.7 (3) |
C11—Cr1—C4—C3 | −164.3 (3) | C41—Rh1—C37—C38 | 44.2 (4) |
C10—Cr1—C4—C3 | 30.0 (4) | C36—Rh1—C37—C38 | 122.0 (6) |
C9—Cr1—C4—C3 | 112.4 (3) | C40—Rh1—C37—C38 | 9.0 (4) |
C2—Cr1—C4—C3 | −29.8 (3) | P2—Rh1—C37—C38 | −52.3 (6) |
C5—Cr1—C4—C3 | −132.3 (4) | P1—Rh1—C37—C38 | −160.3 (4) |
C6—Cr1—C4—C3 | −104.3 (3) | C36—C37—C38—C39 | 95.7 (6) |
C1—Cr1—C4—C3 | −66.9 (3) | Rh1—C37—C38—C39 | 11.7 (6) |
C3—C4—C5—C6 | 1.1 (7) | C37—C38—C39—C40 | −37.8 (7) |
Cr1—C4—C5—C6 | −53.3 (4) | C38—C39—C40—C41 | −36.3 (8) |
C3—C4—C5—Cr1 | 54.4 (4) | C38—C39—C40—Rh1 | 43.3 (5) |
C11—Cr1—C5—C4 | 157.3 (3) | C37—Rh1—C40—C41 | 96.4 (4) |
C10—Cr1—C5—C4 | −63.8 (9) | C36—Rh1—C40—C41 | 63.8 (4) |
C9—Cr1—C5—C4 | 67.8 (3) | P2—Rh1—C40—C41 | −105.8 (3) |
C2—Cr1—C5—C4 | −65.7 (3) | P1—Rh1—C40—C41 | 178.5 (6) |
C3—Cr1—C5—C4 | −28.9 (3) | C37—Rh1—C40—C39 | −28.1 (4) |
C6—Cr1—C5—C4 | −134.2 (4) | C41—Rh1—C40—C39 | −124.5 (5) |
C1—Cr1—C5—C4 | −103.1 (3) | C36—Rh1—C40—C39 | −60.7 (4) |
C11—Cr1—C5—C6 | −68.6 (3) | P2—Rh1—C40—C39 | 129.7 (4) |
C10—Cr1—C5—C6 | 70.4 (9) | P1—Rh1—C40—C39 | 54.1 (10) |
C9—Cr1—C5—C6 | −158.1 (3) | C39—C40—C41—C42 | −7.5 (9) |
C2—Cr1—C5—C6 | 68.4 (3) | Rh1—C40—C41—C42 | −105.1 (5) |
C3—Cr1—C5—C6 | 105.3 (3) | C39—C40—C41—Rh1 | 97.6 (5) |
C4—Cr1—C5—C6 | 134.2 (4) | C37—Rh1—C41—C40 | −78.9 (3) |
C1—Cr1—C5—C6 | 31.0 (3) | C36—Rh1—C41—C40 | −114.5 (4) |
C4—C5—C6—C1 | −3.7 (7) | P2—Rh1—C41—C40 | 75.5 (3) |
Cr1—C5—C6—C1 | −57.1 (4) | P1—Rh1—C41—C40 | −179.3 (3) |
C4—C5—C6—C7 | −179.9 (4) | C37—Rh1—C41—C42 | 43.1 (4) |
Cr1—C5—C6—C7 | 126.7 (4) | C36—Rh1—C41—C42 | 7.6 (4) |
C4—C5—C6—Cr1 | 53.3 (4) | C40—Rh1—C41—C42 | 122.0 (6) |
C2—C1—C6—C5 | 5.1 (6) | P2—Rh1—C41—C42 | −162.5 (4) |
P1—C1—C6—C5 | −165.7 (3) | P1—Rh1—C41—C42 | −57.3 (6) |
Cr1—C1—C6—C5 | 56.6 (4) | C40—C41—C42—C43 | 97.5 (6) |
C2—C1—C6—C7 | −178.7 (4) | Rh1—C41—C42—C43 | 13.3 (6) |
P1—C1—C6—C7 | 10.5 (6) | C37—C36—C43—C42 | −35.7 (8) |
Cr1—C1—C6—C7 | −127.2 (4) | Rh1—C36—C43—C42 | 43.4 (6) |
C2—C1—C6—Cr1 | −51.4 (4) | C41—C42—C43—C36 | −38.9 (7) |
Selected bond distances and angles for (I) (Å, °) topP1-C1 | 1.854 (3) | P2-C8 | 1.878 (3) |
〈Cr1-C(C6H4 ring)〉 | 2.213 (4) | 〈Cr1-C(CO)〉 | 1.840 (4) |
| | | |
C33-Cr1-C34 | 88.3 (2) | C34-Cr1-C35 | 88.8 (2) |
C35-Cr1-C33 | 88.6 (2) | | |
Selected distances and angles for molecule 1/molecule 2 in (II) (Å, °) topRh1-P1 | 2.277 (3)/2.288 (3) | Rh1-P2 | 2.273 (3)/2.253 (3) |
Rh1-MP1 | 2.0974 (8)/2.1141 (6) | Rh1-MP2 | 2.1242 (7)/2.0962 (7) |
〈Rh1-C═C (diolefin)〉 | 2.221 (10)/2.215 (9) | | |
P1-C1 | 1.846 (11)/1.827 (9) | P2-C10 | 1.851 (10)/1.865 (10) |
P1-C24 | 1.810 (10)/1.823 (9) | P2-C11 | 1.810 (11)/1.807 (10) |
P1-C30 | 1.812 (9)/1.793 (10) | P2-C17 | 1.808 (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-P2 | 91.60 (10)/91.42 (9) | MP1-Rh1-MP2 | 68.26 (3)/69.23 (2) |
P1-Rh1-MP1 | 99.02 (8)/101.11 (7) | P2-Rh1-MP2 | 101.03 (7)/98.53 (7) |
C2-Cr1-C3 | 87.5 (5)/85.9 (5) | C3-Cr1-C4 | 86.4 (5)/87.1 (5) |
C4-Cr1-C2 | 90.4 (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, °) topRh1-P1 | 2.290 (2) | Rh1-P2 | 2.279 (2) |
Rh1-MP1 | 2.135 (5) | Rh1-MP2 | 2.149 (5) |
〈Rh1-C═C (diolefin)〉 | 2.249 (6) | | |
P1-C1 | 1.852 (5) | P2-C7 | 1.871 (5) |
P1-C12 | 1.832 (5) | P2-C24 | 1.815 (5) |
P1-C18 | 1.823 (5) | P2-C30 | 1.818 (5) |
〈Cr1-C(C6H4 ring)〉 | 2.217 (5) | 〈Cr1-C(CO)〉 | 1.835 (7) |
| | | |
P1-Rh1-P2 | 90.0 (1) | MP1-Rh1-MP2 | 84.2 (1) |
P1-Rh1-MP1 | 94.4 (1) | P2-Rh1-MP2 | 92.2 (1) |
C9-Cr1-C10 | 86.5 (2) | C10-Cr1-C11 | 88.9 (2) |
C11-Cr1-C9 | 87.1 (2) | | |
Comparison of characteristic torsion angles in (I)-(III) (°) topTorsion 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) |