The complexes {bis[(2-diphenylphosphanyl)phenyl] ether-κ2P,P′}(η4-norbornadiene)rhodium(I) tetrafluoridoborate, [Rh(C7H8)(C36H28OP2)]BF4, and {bis[(2-diphenylphosphanyl)phenyl] ether-κ2P,P′}[η4-(Z,Z)-cycloocta-1,5-diene]rhodium(I) tetrafluoridoborate dichloromethane monosolvate, [Rh(C8H12)(C36H28OP2)]BF4·CH2Cl2, are applied as precatalysts in redox-neutral atomic-economic propargylic CH activation [Lumbroso et al. (2013). Angew. Chem. Int. Ed. 52, 1890–1932]. In addition, the catalytically inactive pentacoordinated 18-electron complex {bis[(2-diphenylphosphanyl)phenyl] ether-κ2P,P′}chlorido(η4-norbornadiene)rhodium(I), [RhCl(C7H8)(C36H28OP2)], was synthesized, which can form in the presence of chloride in the reaction system.
Supporting information
CCDC references: 1948472; 1948473; 1948474
For all structures, data collection: APEX2 (Bruker, 2014); cell refinement: SAINT (Bruker, 2013); data reduction: SAINT (Bruker, 2013); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL2014 (Sheldrick, 2015); molecular graphics: SHELXTL (Bruker, 2014); software used to prepare material for publication: SHELXTL (Bruker, 2014) and publCIF (Westrip, 2010).
{Bis[(2-diphenylphosphanyl)phenyl]
ether-
κ2P,
P'}(
η4-norbornadiene)rhodium(I)
tetrafluoridoborate (compI)
top
Crystal data top
[Rh(C7H8)(C36H28OP2)]BF4 | F(000) = 3344 |
Mr = 820.38 | Dx = 1.551 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
a = 21.8106 (3) Å | Cell parameters from 9800 reflections |
b = 18.0754 (2) Å | θ = 2.6–27.5° |
c = 18.1455 (2) Å | µ = 0.63 mm−1 |
β = 100.742 (1)° | T = 150 K |
V = 7028.24 (15) Å3 | Part of prism, orange |
Z = 8 | 0.50 × 0.44 × 0.32 mm |
Data collection top
Bruker APEXII CCD diffractometer | 13063 independent reflections |
Radiation source: sealed tube | 11013 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.031 |
Detector resolution: 8.33 pixels mm-1 | θmax = 25.5°, θmin = 1.6° |
φ and ω scans | h = −26→24 |
Absorption correction: multi-scan (SADABS; Bruker, 2014) | k = −21→21 |
Tmin = 0.664, Tmax = 0.746 | l = −21→20 |
68856 measured reflections | |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.037 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.105 | H-atom parameters constrained |
S = 1.07 | w = 1/[σ2(Fo2) + (0.0408P)2 + 20.3084P] where P = (Fo2 + 2Fc2)/3 |
13063 reflections | (Δ/σ)max = 0.002 |
937 parameters | Δρmax = 1.34 e Å−3 |
24 restraints | Δρmin = −1.29 e Å−3 |
Special details top
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Rh1 | 0.17316 (2) | 0.74146 (2) | 0.03877 (2) | 0.02192 (8) | |
P1 | 0.10970 (4) | 0.63622 (5) | 0.02064 (5) | 0.02198 (18) | |
P2 | 0.15520 (4) | 0.78805 (5) | −0.08330 (5) | 0.02189 (18) | |
O1 | 0.15982 (11) | 0.63852 (13) | −0.12610 (13) | 0.0264 (5) | |
C1 | 0.12308 (16) | 0.55765 (19) | −0.03872 (19) | 0.0245 (7) | |
C2 | 0.11093 (17) | 0.4849 (2) | −0.0191 (2) | 0.0294 (8) | |
H2 | 0.0903 | 0.4762 | 0.0218 | 0.035* | |
C3 | 0.12861 (19) | 0.4254 (2) | −0.0587 (2) | 0.0345 (9) | |
H3 | 0.1193 | 0.3764 | −0.0453 | 0.041* | |
C4 | 0.1594 (2) | 0.4368 (2) | −0.1172 (2) | 0.0389 (9) | |
H4 | 0.1736 | 0.3958 | −0.1421 | 0.047* | |
C5 | 0.16978 (19) | 0.5084 (2) | −0.1398 (2) | 0.0356 (9) | |
H5 | 0.1900 | 0.5167 | −0.1812 | 0.043* | |
C6 | 0.15043 (17) | 0.56718 (19) | −0.1016 (2) | 0.0270 (7) | |
C7 | 0.10860 (16) | 0.67068 (19) | −0.17231 (18) | 0.0244 (7) | |
C8 | 0.06783 (18) | 0.6312 (2) | −0.2260 (2) | 0.0307 (8) | |
H8 | 0.0725 | 0.5793 | −0.2310 | 0.037* | |
C9 | 0.02032 (18) | 0.6688 (2) | −0.2721 (2) | 0.0355 (9) | |
H9 | −0.0088 | 0.6426 | −0.3083 | 0.043* | |
C10 | 0.01517 (18) | 0.7460 (2) | −0.2654 (2) | 0.0328 (8) | |
H10 | −0.0167 | 0.7722 | −0.2980 | 0.039* | |
C11 | 0.05565 (17) | 0.7828 (2) | −0.2124 (2) | 0.0297 (8) | |
H11 | 0.0522 | 0.8351 | −0.2091 | 0.036* | |
C12 | 0.10256 (16) | 0.74620 (19) | −0.16246 (19) | 0.0236 (7) | |
C13 | 0.03055 (16) | 0.66807 (19) | −0.0145 (2) | 0.0275 (8) | |
C14 | 0.0096 (2) | 0.7288 (2) | 0.0221 (3) | 0.0411 (10) | |
H14 | 0.0361 | 0.7502 | 0.0642 | 0.049* | |
C15 | −0.0490 (2) | 0.7573 (2) | −0.0023 (4) | 0.0580 (15) | |
H15 | −0.0640 | 0.7967 | 0.0241 | 0.070* | |
C16 | −0.0857 (2) | 0.7282 (3) | −0.0657 (4) | 0.0662 (17) | |
H16 | −0.1252 | 0.7500 | −0.0844 | 0.079* | |
C17 | −0.0671 (2) | 0.6699 (3) | −0.1016 (3) | 0.0513 (12) | |
H17 | −0.0941 | 0.6501 | −0.1442 | 0.062* | |
C18 | −0.00793 (18) | 0.6376 (2) | −0.0765 (2) | 0.0363 (9) | |
H18 | 0.0052 | 0.5960 | −0.1016 | 0.044* | |
C19 | 0.10460 (19) | 0.58566 (19) | 0.10690 (19) | 0.0286 (8) | |
C20 | 0.1579 (2) | 0.5506 (2) | 0.1450 (2) | 0.0374 (9) | |
H20 | 0.1964 | 0.5570 | 0.1285 | 0.045* | |
C21 | 0.1555 (3) | 0.5060 (2) | 0.2072 (2) | 0.0494 (12) | |
H21 | 0.1917 | 0.4809 | 0.2320 | 0.059* | |
C22 | 0.0995 (3) | 0.4987 (3) | 0.2323 (2) | 0.0621 (16) | |
H22 | 0.0978 | 0.4690 | 0.2751 | 0.074* | |
C23 | 0.0466 (3) | 0.5336 (2) | 0.1964 (2) | 0.0533 (13) | |
H23 | 0.0087 | 0.5282 | 0.2144 | 0.064* | |
C24 | 0.0486 (2) | 0.5778 (2) | 0.1323 (2) | 0.0388 (10) | |
H24 | 0.0120 | 0.6019 | 0.1070 | 0.047* | |
C25 | 0.12455 (16) | 0.88152 (19) | −0.07940 (18) | 0.0247 (7) | |
C26 | 0.16272 (18) | 0.9439 (2) | −0.0717 (2) | 0.0294 (8) | |
H26 | 0.2058 | 0.9386 | −0.0731 | 0.035* | |
C27 | 0.1391 (2) | 1.0129 (2) | −0.0622 (2) | 0.0391 (10) | |
H27 | 0.1656 | 1.0550 | −0.0570 | 0.047* | |
C28 | 0.0757 (2) | 1.0204 (2) | −0.0603 (2) | 0.0442 (11) | |
H28 | 0.0586 | 1.0680 | −0.0551 | 0.053* | |
C29 | 0.0390 (2) | 0.9603 (3) | −0.0659 (2) | 0.0432 (11) | |
H29 | −0.0039 | 0.9662 | −0.0641 | 0.052* | |
C30 | 0.06193 (18) | 0.8901 (2) | −0.0742 (2) | 0.0318 (8) | |
H30 | 0.0354 | 0.8482 | −0.0764 | 0.038* | |
C31 | 0.22847 (16) | 0.79868 (19) | −0.11663 (19) | 0.0253 (7) | |
C32 | 0.23407 (18) | 0.8495 (2) | −0.1728 (2) | 0.0306 (8) | |
H32 | 0.1984 | 0.8763 | −0.1969 | 0.037* | |
C33 | 0.29141 (19) | 0.8614 (2) | −0.1940 (2) | 0.0365 (9) | |
H33 | 0.2955 | 0.8975 | −0.2308 | 0.044* | |
C34 | 0.34207 (18) | 0.8201 (2) | −0.1610 (2) | 0.0393 (10) | |
H34 | 0.3812 | 0.8277 | −0.1756 | 0.047* | |
C35 | 0.33723 (18) | 0.7690 (2) | −0.1082 (2) | 0.0355 (9) | |
H35 | 0.3729 | 0.7408 | −0.0867 | 0.043* | |
C36 | 0.28044 (17) | 0.7567 (2) | −0.0844 (2) | 0.0283 (8) | |
H36 | 0.2774 | 0.7206 | −0.0472 | 0.034* | |
C37 | 0.18969 (18) | 0.8497 (2) | 0.09314 (19) | 0.0287 (8) | |
H37 | 0.1681 | 0.8958 | 0.0717 | 0.034* | |
C38 | 0.24468 (18) | 0.8250 (2) | 0.0747 (2) | 0.0301 (8) | |
H38 | 0.2667 | 0.8519 | 0.0390 | 0.036* | |
C39 | 0.27914 (18) | 0.7824 (2) | 0.1429 (2) | 0.0330 (8) | |
H39 | 0.3247 | 0.7730 | 0.1457 | 0.040* | |
C40 | 0.23671 (18) | 0.7150 (2) | 0.1429 (2) | 0.0325 (8) | |
H40 | 0.2532 | 0.6640 | 0.1553 | 0.039* | |
C41 | 0.18204 (19) | 0.7403 (2) | 0.16146 (19) | 0.0327 (9) | |
H41 | 0.1551 | 0.7092 | 0.1881 | 0.039* | |
C42 | 0.19005 (18) | 0.8238 (2) | 0.1737 (2) | 0.0321 (8) | |
H42 | 0.1607 | 0.8490 | 0.2018 | 0.038* | |
C43 | 0.25974 (18) | 0.8287 (2) | 0.2069 (2) | 0.0345 (9) | |
H43A | 0.2709 | 0.8047 | 0.2567 | 0.041* | |
H43B | 0.2759 | 0.8800 | 0.2091 | 0.041* | |
Rh2 | 0.34749 (2) | 0.24149 (2) | 0.13032 (2) | 0.01640 (7) | |
P3 | 0.31862 (4) | 0.12588 (4) | 0.17023 (4) | 0.01692 (16) | |
P4 | 0.43984 (4) | 0.20273 (4) | 0.09510 (4) | 0.01535 (16) | |
O2 | 0.45302 (10) | 0.14927 (11) | 0.24878 (11) | 0.0169 (4) | |
C51 | 0.35412 (15) | 0.10025 (17) | 0.26661 (17) | 0.0178 (6) | |
C52 | 0.31940 (16) | 0.06760 (18) | 0.31545 (18) | 0.0237 (7) | |
H52 | 0.2769 | 0.0555 | 0.2974 | 0.028* | |
C53 | 0.34553 (17) | 0.05255 (19) | 0.38950 (18) | 0.0248 (7) | |
H53 | 0.3212 | 0.0299 | 0.4216 | 0.030* | |
C54 | 0.40723 (16) | 0.07062 (18) | 0.41651 (18) | 0.0227 (7) | |
H54 | 0.4251 | 0.0608 | 0.4674 | 0.027* | |
C55 | 0.44339 (16) | 0.10299 (17) | 0.36981 (17) | 0.0201 (7) | |
H55 | 0.4857 | 0.1158 | 0.3884 | 0.024* | |
C56 | 0.41652 (15) | 0.11616 (16) | 0.29562 (17) | 0.0171 (6) | |
C57 | 0.48303 (14) | 0.10056 (17) | 0.20741 (17) | 0.0169 (6) | |
C58 | 0.51508 (16) | 0.03914 (18) | 0.24038 (18) | 0.0230 (7) | |
H58 | 0.5176 | 0.0292 | 0.2923 | 0.028* | |
C59 | 0.54326 (16) | −0.00730 (19) | 0.19608 (19) | 0.0259 (7) | |
H59 | 0.5652 | −0.0497 | 0.2178 | 0.031* | |
C60 | 0.54000 (16) | 0.00712 (18) | 0.12047 (19) | 0.0244 (7) | |
H60 | 0.5588 | −0.0257 | 0.0904 | 0.029* | |
C61 | 0.50906 (15) | 0.06978 (18) | 0.08901 (17) | 0.0199 (6) | |
H61 | 0.5070 | 0.0797 | 0.0372 | 0.024* | |
C62 | 0.48093 (14) | 0.11840 (17) | 0.13208 (17) | 0.0165 (6) | |
C63 | 0.23535 (15) | 0.11321 (19) | 0.17163 (18) | 0.0215 (7) | |
C64 | 0.20018 (16) | 0.0566 (2) | 0.1332 (2) | 0.0299 (8) | |
H64 | 0.2190 | 0.0229 | 0.1039 | 0.036* | |
C65 | 0.13766 (18) | 0.0489 (3) | 0.1374 (2) | 0.0393 (10) | |
H65 | 0.1141 | 0.0094 | 0.1117 | 0.047* | |
C66 | 0.10938 (17) | 0.0980 (2) | 0.1784 (2) | 0.0371 (9) | |
H66 | 0.0663 | 0.0930 | 0.1801 | 0.044* | |
C67 | 0.14373 (18) | 0.1546 (2) | 0.2170 (2) | 0.0331 (8) | |
H67 | 0.1244 | 0.1887 | 0.2454 | 0.040* | |
C68 | 0.20664 (17) | 0.1616 (2) | 0.2143 (2) | 0.0285 (8) | |
H68 | 0.2304 | 0.1999 | 0.2420 | 0.034* | |
C69 | 0.33497 (14) | 0.05015 (17) | 0.11018 (17) | 0.0189 (6) | |
C70 | 0.36883 (16) | −0.01234 (18) | 0.13622 (19) | 0.0236 (7) | |
H70 | 0.3837 | −0.0188 | 0.1885 | 0.028* | |
C71 | 0.38105 (17) | −0.0657 (2) | 0.0857 (2) | 0.0295 (8) | |
H71 | 0.4046 | −0.1084 | 0.1036 | 0.035* | |
C72 | 0.35909 (17) | −0.0571 (2) | 0.0095 (2) | 0.0302 (8) | |
H72 | 0.3676 | −0.0937 | −0.0248 | 0.036* | |
C73 | 0.32472 (17) | 0.0051 (2) | −0.01648 (19) | 0.0291 (8) | |
H73 | 0.3095 | 0.0110 | −0.0687 | 0.035* | |
C74 | 0.31247 (15) | 0.05862 (19) | 0.03322 (18) | 0.0235 (7) | |
H74 | 0.2888 | 0.1012 | 0.0151 | 0.028* | |
C75 | 0.43380 (15) | 0.19761 (17) | −0.00664 (17) | 0.0184 (6) | |
C76 | 0.37537 (16) | 0.19583 (18) | −0.05217 (18) | 0.0229 (7) | |
H76 | 0.3392 | 0.1944 | −0.0301 | 0.028* | |
C77 | 0.36892 (17) | 0.19614 (19) | −0.13001 (19) | 0.0286 (8) | |
H77 | 0.3285 | 0.1936 | −0.1606 | 0.034* | |
C78 | 0.42071 (18) | 0.20018 (18) | −0.16270 (18) | 0.0271 (8) | |
H78 | 0.4163 | 0.2012 | −0.2158 | 0.032* | |
C79 | 0.47982 (18) | 0.20278 (19) | −0.11771 (19) | 0.0265 (7) | |
H79 | 0.5157 | 0.2060 | −0.1402 | 0.032* | |
C80 | 0.48660 (16) | 0.20076 (18) | −0.04019 (18) | 0.0226 (7) | |
H80 | 0.5271 | 0.2015 | −0.0098 | 0.027* | |
C81 | 0.49796 (14) | 0.27554 (17) | 0.12270 (17) | 0.0177 (6) | |
C82 | 0.50611 (16) | 0.33150 (18) | 0.07270 (18) | 0.0240 (7) | |
H82 | 0.4835 | 0.3297 | 0.0226 | 0.029* | |
C83 | 0.54665 (18) | 0.38976 (19) | 0.0948 (2) | 0.0297 (8) | |
H83 | 0.5524 | 0.4270 | 0.0598 | 0.036* | |
C84 | 0.57875 (18) | 0.3935 (2) | 0.1680 (2) | 0.0302 (8) | |
H84 | 0.6063 | 0.4336 | 0.1836 | 0.036* | |
C85 | 0.57062 (17) | 0.3388 (2) | 0.21831 (19) | 0.0268 (7) | |
H85 | 0.5927 | 0.3415 | 0.2686 | 0.032* | |
C86 | 0.53057 (15) | 0.27987 (19) | 0.19638 (18) | 0.0216 (7) | |
H86 | 0.5254 | 0.2425 | 0.2315 | 0.026* | |
C87 | 0.27633 (16) | 0.3134 (2) | 0.1663 (2) | 0.0278 (8) | |
H87 | 0.2564 | 0.3019 | 0.2103 | 0.033* | |
C88 | 0.25457 (16) | 0.2859 (2) | 0.0950 (2) | 0.0267 (7) | |
H88 | 0.2167 | 0.2539 | 0.0827 | 0.032* | |
C89 | 0.27199 (18) | 0.3433 (2) | 0.0397 (2) | 0.0308 (8) | |
H89 | 0.2494 | 0.3407 | −0.0135 | 0.037* | |
C90 | 0.34306 (17) | 0.33590 (18) | 0.0539 (2) | 0.0273 (8) | |
H90 | 0.3678 | 0.3384 | 0.0127 | 0.033* | |
C91 | 0.36514 (17) | 0.36228 (18) | 0.1250 (2) | 0.0270 (7) | |
H91 | 0.4075 | 0.3848 | 0.1403 | 0.032* | |
C92 | 0.30799 (18) | 0.3876 (2) | 0.1564 (2) | 0.0305 (8) | |
H92 | 0.3154 | 0.4221 | 0.2003 | 0.037* | |
C93 | 0.2656 (2) | 0.4155 (2) | 0.0835 (2) | 0.0380 (9) | |
H93A | 0.2222 | 0.4252 | 0.0899 | 0.046* | |
H93B | 0.2829 | 0.4592 | 0.0617 | 0.046* | |
B1 | 0.1869 (2) | 0.3042 (2) | 0.3786 (2) | 0.0455 (12) | |
F1 | 0.12523 (13) | 0.3061 (3) | 0.3543 (2) | 0.140 (2) | |
F2 | 0.20013 (15) | 0.32071 (15) | 0.45366 (14) | 0.0730 (10) | |
F3 | 0.2147 (2) | 0.3573 (2) | 0.3418 (3) | 0.145 (2) | |
F4 | 0.2133 (2) | 0.23748 (17) | 0.3685 (2) | 0.1033 (15) | |
B2 | 0.6354 (2) | 0.0976 (3) | 0.4139 (3) | 0.0543 (14) | |
F5 | 0.60486 (18) | 0.16315 (18) | 0.4017 (3) | 0.143 (2) | |
F6 | 0.59538 (13) | 0.04401 (15) | 0.42811 (15) | 0.0636 (8) | |
F7 | 0.65998 (16) | 0.0784 (2) | 0.35226 (16) | 0.0869 (11) | |
F8 | 0.68433 (16) | 0.1044 (2) | 0.47283 (19) | 0.1083 (14) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Rh1 | 0.02400 (15) | 0.02361 (14) | 0.01774 (14) | −0.00358 (10) | 0.00281 (10) | 0.00099 (10) |
P1 | 0.0256 (5) | 0.0209 (4) | 0.0201 (4) | −0.0010 (3) | 0.0058 (3) | −0.0001 (3) |
P2 | 0.0215 (4) | 0.0231 (4) | 0.0207 (4) | −0.0019 (3) | 0.0032 (3) | 0.0020 (3) |
O1 | 0.0282 (13) | 0.0272 (13) | 0.0243 (12) | 0.0014 (10) | 0.0064 (10) | 0.0014 (10) |
C1 | 0.0244 (17) | 0.0240 (17) | 0.0240 (17) | 0.0046 (14) | 0.0019 (13) | −0.0022 (13) |
C2 | 0.033 (2) | 0.0280 (19) | 0.0268 (18) | −0.0009 (15) | 0.0035 (15) | 0.0009 (14) |
C3 | 0.045 (2) | 0.0232 (18) | 0.033 (2) | 0.0034 (16) | 0.0011 (17) | −0.0025 (15) |
C4 | 0.053 (3) | 0.030 (2) | 0.033 (2) | 0.0135 (18) | 0.0062 (18) | −0.0058 (16) |
C5 | 0.041 (2) | 0.037 (2) | 0.031 (2) | 0.0094 (17) | 0.0109 (17) | −0.0024 (16) |
C6 | 0.0296 (19) | 0.0243 (17) | 0.0270 (18) | 0.0070 (14) | 0.0048 (14) | 0.0023 (14) |
C7 | 0.0252 (18) | 0.0293 (18) | 0.0200 (16) | −0.0014 (14) | 0.0073 (13) | 0.0027 (14) |
C8 | 0.038 (2) | 0.0296 (19) | 0.0260 (18) | −0.0052 (16) | 0.0092 (16) | −0.0021 (15) |
C9 | 0.035 (2) | 0.045 (2) | 0.0246 (18) | −0.0122 (18) | −0.0003 (15) | 0.0007 (16) |
C10 | 0.0256 (19) | 0.046 (2) | 0.0255 (19) | 0.0035 (16) | 0.0013 (15) | 0.0072 (16) |
C11 | 0.032 (2) | 0.0313 (19) | 0.0259 (18) | 0.0039 (16) | 0.0069 (15) | 0.0069 (15) |
C12 | 0.0222 (17) | 0.0280 (18) | 0.0205 (16) | −0.0026 (14) | 0.0042 (13) | 0.0025 (13) |
C13 | 0.0230 (18) | 0.0256 (18) | 0.035 (2) | 0.0014 (14) | 0.0096 (15) | 0.0083 (15) |
C14 | 0.036 (2) | 0.028 (2) | 0.065 (3) | −0.0003 (17) | 0.024 (2) | −0.0031 (19) |
C15 | 0.048 (3) | 0.029 (2) | 0.107 (5) | 0.012 (2) | 0.042 (3) | 0.013 (2) |
C16 | 0.025 (2) | 0.072 (4) | 0.104 (5) | 0.015 (2) | 0.020 (3) | 0.053 (4) |
C17 | 0.033 (2) | 0.066 (3) | 0.051 (3) | −0.007 (2) | −0.003 (2) | 0.024 (2) |
C18 | 0.027 (2) | 0.046 (2) | 0.035 (2) | −0.0028 (17) | 0.0065 (16) | 0.0066 (18) |
C19 | 0.047 (2) | 0.0202 (17) | 0.0202 (17) | −0.0065 (15) | 0.0099 (15) | −0.0020 (13) |
C20 | 0.057 (3) | 0.0237 (18) | 0.0270 (19) | −0.0029 (18) | −0.0025 (18) | −0.0007 (15) |
C21 | 0.083 (4) | 0.030 (2) | 0.028 (2) | −0.011 (2) | −0.008 (2) | 0.0032 (17) |
C22 | 0.121 (5) | 0.044 (3) | 0.018 (2) | −0.028 (3) | 0.008 (3) | 0.0016 (19) |
C23 | 0.095 (4) | 0.039 (2) | 0.034 (2) | −0.026 (3) | 0.033 (3) | −0.012 (2) |
C24 | 0.058 (3) | 0.030 (2) | 0.034 (2) | −0.0129 (19) | 0.0235 (19) | −0.0060 (16) |
C25 | 0.0294 (19) | 0.0244 (17) | 0.0199 (16) | −0.0004 (14) | 0.0032 (14) | 0.0010 (13) |
C26 | 0.031 (2) | 0.0310 (19) | 0.0263 (18) | −0.0057 (15) | 0.0057 (15) | 0.0006 (15) |
C27 | 0.059 (3) | 0.029 (2) | 0.028 (2) | −0.0062 (19) | 0.0027 (18) | −0.0012 (16) |
C28 | 0.060 (3) | 0.035 (2) | 0.035 (2) | 0.017 (2) | 0.003 (2) | −0.0042 (18) |
C29 | 0.035 (2) | 0.052 (3) | 0.038 (2) | 0.013 (2) | −0.0051 (18) | −0.0174 (19) |
C30 | 0.031 (2) | 0.036 (2) | 0.0281 (19) | 0.0003 (16) | 0.0034 (15) | −0.0055 (16) |
C31 | 0.0236 (17) | 0.0294 (18) | 0.0222 (17) | −0.0028 (14) | 0.0025 (13) | −0.0023 (14) |
C32 | 0.033 (2) | 0.036 (2) | 0.0233 (18) | −0.0035 (16) | 0.0063 (15) | 0.0015 (15) |
C33 | 0.040 (2) | 0.044 (2) | 0.029 (2) | −0.0108 (18) | 0.0149 (17) | −0.0062 (17) |
C34 | 0.027 (2) | 0.046 (2) | 0.048 (2) | −0.0073 (18) | 0.0147 (18) | −0.024 (2) |
C35 | 0.0236 (19) | 0.047 (2) | 0.034 (2) | 0.0073 (17) | −0.0002 (15) | −0.0206 (18) |
C36 | 0.0303 (19) | 0.0287 (18) | 0.0245 (18) | 0.0015 (15) | 0.0015 (15) | −0.0058 (14) |
C37 | 0.038 (2) | 0.0243 (18) | 0.0229 (18) | −0.0028 (15) | 0.0027 (15) | −0.0030 (14) |
C38 | 0.035 (2) | 0.0302 (19) | 0.0254 (18) | −0.0147 (16) | 0.0066 (15) | −0.0040 (15) |
C39 | 0.0255 (19) | 0.039 (2) | 0.032 (2) | −0.0026 (16) | −0.0009 (15) | −0.0066 (16) |
C40 | 0.039 (2) | 0.034 (2) | 0.0206 (17) | −0.0033 (17) | −0.0049 (15) | 0.0036 (15) |
C41 | 0.043 (2) | 0.039 (2) | 0.0161 (17) | −0.0129 (17) | 0.0064 (15) | 0.0008 (15) |
C42 | 0.037 (2) | 0.038 (2) | 0.0226 (18) | −0.0039 (17) | 0.0109 (15) | −0.0040 (15) |
C43 | 0.041 (2) | 0.039 (2) | 0.0220 (18) | −0.0088 (17) | 0.0006 (16) | −0.0014 (16) |
Rh2 | 0.01638 (13) | 0.01748 (13) | 0.01557 (13) | 0.00231 (9) | 0.00358 (9) | 0.00136 (9) |
P3 | 0.0168 (4) | 0.0194 (4) | 0.0148 (4) | −0.0001 (3) | 0.0035 (3) | 0.0002 (3) |
P4 | 0.0168 (4) | 0.0164 (4) | 0.0128 (4) | −0.0001 (3) | 0.0026 (3) | 0.0008 (3) |
O2 | 0.0205 (11) | 0.0164 (10) | 0.0150 (10) | 0.0008 (9) | 0.0063 (8) | 0.0003 (8) |
C51 | 0.0221 (16) | 0.0171 (15) | 0.0141 (14) | 0.0010 (12) | 0.0035 (12) | −0.0009 (12) |
C52 | 0.0251 (18) | 0.0240 (17) | 0.0236 (17) | 0.0011 (14) | 0.0084 (14) | 0.0010 (13) |
C53 | 0.035 (2) | 0.0243 (17) | 0.0185 (16) | 0.0024 (14) | 0.0134 (14) | 0.0019 (13) |
C54 | 0.0353 (19) | 0.0186 (16) | 0.0144 (15) | 0.0029 (14) | 0.0053 (13) | −0.0015 (12) |
C55 | 0.0265 (17) | 0.0160 (15) | 0.0171 (15) | 0.0001 (13) | 0.0023 (13) | −0.0018 (12) |
C56 | 0.0249 (17) | 0.0121 (14) | 0.0162 (15) | −0.0010 (12) | 0.0084 (12) | −0.0008 (11) |
C57 | 0.0163 (15) | 0.0167 (15) | 0.0184 (15) | −0.0006 (12) | 0.0054 (12) | −0.0026 (12) |
C58 | 0.0272 (18) | 0.0234 (17) | 0.0185 (16) | 0.0035 (14) | 0.0043 (13) | 0.0035 (13) |
C59 | 0.0294 (19) | 0.0210 (17) | 0.0270 (18) | 0.0076 (14) | 0.0048 (14) | 0.0037 (14) |
C60 | 0.0270 (18) | 0.0207 (16) | 0.0273 (18) | 0.0033 (14) | 0.0099 (14) | −0.0033 (13) |
C61 | 0.0220 (16) | 0.0219 (16) | 0.0166 (15) | −0.0011 (13) | 0.0058 (12) | −0.0004 (12) |
C62 | 0.0158 (15) | 0.0160 (15) | 0.0168 (15) | −0.0004 (12) | 0.0013 (12) | 0.0014 (12) |
C63 | 0.0186 (16) | 0.0269 (17) | 0.0188 (16) | 0.0016 (13) | 0.0032 (12) | 0.0047 (13) |
C64 | 0.0232 (18) | 0.039 (2) | 0.0280 (18) | −0.0043 (15) | 0.0072 (14) | −0.0052 (16) |
C65 | 0.025 (2) | 0.057 (3) | 0.036 (2) | −0.0117 (18) | 0.0060 (16) | −0.0096 (19) |
C66 | 0.0192 (18) | 0.060 (3) | 0.033 (2) | −0.0015 (17) | 0.0067 (15) | 0.0015 (18) |
C67 | 0.029 (2) | 0.042 (2) | 0.031 (2) | 0.0059 (16) | 0.0117 (16) | 0.0020 (16) |
C68 | 0.0290 (19) | 0.0294 (19) | 0.0287 (18) | −0.0018 (15) | 0.0097 (15) | −0.0019 (15) |
C69 | 0.0169 (15) | 0.0208 (16) | 0.0205 (16) | −0.0034 (12) | 0.0071 (12) | −0.0016 (12) |
C70 | 0.0223 (17) | 0.0236 (17) | 0.0261 (17) | −0.0037 (13) | 0.0076 (13) | −0.0018 (13) |
C71 | 0.0300 (19) | 0.0214 (17) | 0.039 (2) | −0.0008 (14) | 0.0115 (16) | −0.0028 (15) |
C72 | 0.032 (2) | 0.0289 (19) | 0.034 (2) | −0.0108 (15) | 0.0161 (16) | −0.0141 (15) |
C73 | 0.0311 (19) | 0.037 (2) | 0.0200 (17) | −0.0131 (16) | 0.0076 (14) | −0.0057 (15) |
C74 | 0.0215 (17) | 0.0283 (18) | 0.0208 (16) | −0.0056 (14) | 0.0040 (13) | −0.0025 (14) |
C75 | 0.0266 (17) | 0.0152 (15) | 0.0134 (14) | 0.0010 (12) | 0.0042 (12) | 0.0015 (11) |
C76 | 0.0277 (18) | 0.0222 (16) | 0.0188 (16) | −0.0034 (14) | 0.0043 (13) | 0.0006 (13) |
C77 | 0.033 (2) | 0.0279 (18) | 0.0211 (17) | −0.0048 (15) | −0.0042 (14) | 0.0010 (14) |
C78 | 0.048 (2) | 0.0198 (17) | 0.0139 (15) | 0.0034 (15) | 0.0077 (15) | 0.0017 (13) |
C79 | 0.038 (2) | 0.0221 (17) | 0.0228 (17) | 0.0062 (15) | 0.0154 (15) | 0.0028 (13) |
C80 | 0.0271 (18) | 0.0207 (16) | 0.0207 (16) | 0.0033 (13) | 0.0061 (13) | 0.0031 (13) |
C81 | 0.0152 (15) | 0.0183 (15) | 0.0195 (15) | 0.0002 (12) | 0.0031 (12) | −0.0009 (12) |
C82 | 0.0293 (18) | 0.0213 (16) | 0.0196 (16) | 0.0000 (14) | −0.0002 (13) | 0.0018 (13) |
C83 | 0.039 (2) | 0.0200 (17) | 0.0292 (19) | −0.0061 (15) | 0.0053 (16) | 0.0044 (14) |
C84 | 0.036 (2) | 0.0247 (18) | 0.0295 (19) | −0.0108 (15) | 0.0063 (15) | −0.0040 (15) |
C85 | 0.0302 (19) | 0.0306 (19) | 0.0187 (16) | −0.0084 (15) | 0.0021 (14) | −0.0039 (14) |
C86 | 0.0240 (17) | 0.0246 (17) | 0.0168 (15) | −0.0010 (13) | 0.0056 (13) | 0.0000 (13) |
C87 | 0.0216 (17) | 0.0322 (19) | 0.0307 (19) | 0.0079 (15) | 0.0076 (14) | 0.0002 (15) |
C88 | 0.0173 (16) | 0.0308 (19) | 0.0311 (19) | 0.0077 (14) | 0.0022 (14) | 0.0036 (15) |
C89 | 0.036 (2) | 0.0287 (19) | 0.0266 (18) | 0.0111 (16) | 0.0027 (15) | 0.0057 (15) |
C90 | 0.035 (2) | 0.0192 (16) | 0.0294 (19) | 0.0065 (14) | 0.0094 (15) | 0.0096 (14) |
C91 | 0.0304 (19) | 0.0164 (16) | 0.035 (2) | 0.0021 (14) | 0.0076 (15) | 0.0016 (14) |
C92 | 0.033 (2) | 0.0233 (18) | 0.036 (2) | 0.0074 (15) | 0.0103 (16) | −0.0045 (15) |
C93 | 0.041 (2) | 0.029 (2) | 0.043 (2) | 0.0159 (17) | 0.0072 (18) | 0.0052 (17) |
B1 | 0.045 (3) | 0.051 (3) | 0.039 (3) | 0.004 (2) | 0.004 (2) | −0.008 (2) |
F1 | 0.043 (2) | 0.258 (7) | 0.106 (3) | −0.006 (3) | −0.019 (2) | −0.042 (4) |
F2 | 0.105 (3) | 0.0474 (16) | 0.0525 (17) | 0.0172 (16) | −0.0224 (16) | −0.0148 (13) |
F3 | 0.136 (4) | 0.151 (4) | 0.174 (5) | 0.057 (3) | 0.099 (4) | 0.092 (4) |
F4 | 0.158 (4) | 0.069 (2) | 0.073 (2) | 0.030 (2) | −0.005 (2) | −0.0293 (19) |
B2 | 0.050 (3) | 0.061 (4) | 0.053 (3) | −0.008 (3) | 0.013 (3) | −0.006 (3) |
F5 | 0.087 (3) | 0.068 (3) | 0.285 (7) | 0.020 (2) | 0.062 (4) | 0.050 (3) |
F6 | 0.0629 (19) | 0.072 (2) | 0.0575 (17) | −0.0132 (15) | 0.0167 (14) | 0.0066 (15) |
F7 | 0.100 (3) | 0.102 (3) | 0.067 (2) | −0.034 (2) | 0.035 (2) | −0.0020 (19) |
F8 | 0.089 (3) | 0.128 (4) | 0.096 (3) | −0.028 (3) | −0.012 (2) | −0.042 (3) |
Geometric parameters (Å, º) top
Rh1—C40 | 2.178 (3) | Rh2—P4 | 2.3317 (8) |
Rh1—C38 | 2.182 (3) | Rh2—P3 | 2.3363 (8) |
Rh1—C37 | 2.190 (3) | P3—C69 | 1.826 (3) |
Rh1—C41 | 2.199 (3) | P3—C63 | 1.835 (3) |
Rh1—P2 | 2.3335 (9) | P3—C51 | 1.835 (3) |
Rh1—P1 | 2.3393 (9) | P4—C75 | 1.828 (3) |
P1—C13 | 1.819 (4) | P4—C62 | 1.831 (3) |
P1—C19 | 1.834 (3) | P4—C81 | 1.831 (3) |
P1—C1 | 1.838 (3) | O2—C57 | 1.397 (4) |
P2—C31 | 1.821 (4) | O2—C56 | 1.402 (4) |
P2—C25 | 1.823 (4) | C51—C56 | 1.395 (4) |
P2—C12 | 1.827 (3) | C51—C52 | 1.399 (4) |
O1—C6 | 1.391 (4) | C52—C53 | 1.385 (5) |
O1—C7 | 1.393 (4) | C52—H52 | 0.9500 |
C1—C6 | 1.394 (5) | C53—C54 | 1.383 (5) |
C1—C2 | 1.400 (5) | C53—H53 | 0.9500 |
C2—C3 | 1.388 (5) | C54—C55 | 1.390 (5) |
C2—H2 | 0.9500 | C54—H54 | 0.9500 |
C3—C4 | 1.373 (6) | C55—C56 | 1.385 (4) |
C3—H3 | 0.9500 | C55—H55 | 0.9500 |
C4—C5 | 1.389 (6) | C57—C58 | 1.387 (4) |
C4—H4 | 0.9500 | C57—C62 | 1.397 (4) |
C5—C6 | 1.377 (5) | C58—C59 | 1.383 (5) |
C5—H5 | 0.9500 | C58—H58 | 0.9500 |
C7—C12 | 1.386 (5) | C59—C60 | 1.385 (5) |
C7—C8 | 1.388 (5) | C59—H59 | 0.9500 |
C8—C9 | 1.384 (6) | C60—C61 | 1.386 (5) |
C8—H8 | 0.9500 | C60—H60 | 0.9500 |
C9—C10 | 1.406 (6) | C61—C62 | 1.392 (4) |
C9—H9 | 0.9500 | C61—H61 | 0.9500 |
C10—C11 | 1.353 (5) | C63—C64 | 1.387 (5) |
C10—H10 | 0.9500 | C63—C68 | 1.392 (5) |
C11—C12 | 1.401 (5) | C64—C65 | 1.387 (5) |
C11—H11 | 0.9500 | C64—H64 | 0.9500 |
C13—C18 | 1.387 (5) | C65—C66 | 1.376 (6) |
C13—C14 | 1.402 (5) | C65—H65 | 0.9500 |
C14—C15 | 1.373 (7) | C66—C67 | 1.380 (6) |
C14—H14 | 0.9500 | C66—H66 | 0.9500 |
C15—C16 | 1.377 (9) | C67—C68 | 1.388 (5) |
C15—H15 | 0.9500 | C67—H67 | 0.9500 |
C16—C17 | 1.341 (8) | C68—H68 | 0.9500 |
C16—H16 | 0.9500 | C69—C70 | 1.384 (5) |
C17—C18 | 1.413 (6) | C69—C74 | 1.400 (5) |
C17—H17 | 0.9500 | C70—C71 | 1.390 (5) |
C18—H18 | 0.9500 | C70—H70 | 0.9500 |
C19—C20 | 1.390 (6) | C71—C72 | 1.386 (5) |
C19—C24 | 1.390 (6) | C71—H71 | 0.9500 |
C20—C21 | 1.396 (6) | C72—C73 | 1.383 (6) |
C20—H20 | 0.9500 | C72—H72 | 0.9500 |
C21—C22 | 1.387 (8) | C73—C74 | 1.383 (5) |
C21—H21 | 0.9500 | C73—H73 | 0.9500 |
C22—C23 | 1.367 (8) | C74—H74 | 0.9500 |
C22—H22 | 0.9500 | C75—C76 | 1.384 (5) |
C23—C24 | 1.418 (6) | C75—C80 | 1.400 (5) |
C23—H23 | 0.9500 | C76—C77 | 1.393 (5) |
C24—H24 | 0.9500 | C76—H76 | 0.9500 |
C25—C26 | 1.393 (5) | C77—C78 | 1.372 (5) |
C25—C30 | 1.395 (5) | C77—H77 | 0.9500 |
C26—C27 | 1.372 (6) | C78—C79 | 1.392 (5) |
C26—H26 | 0.9500 | C78—H78 | 0.9500 |
C27—C28 | 1.396 (6) | C79—C80 | 1.387 (5) |
C27—H27 | 0.9500 | C79—H79 | 0.9500 |
C28—C29 | 1.342 (6) | C80—H80 | 0.9500 |
C28—H28 | 0.9500 | C81—C82 | 1.392 (5) |
C29—C30 | 1.383 (6) | C81—C86 | 1.395 (4) |
C29—H29 | 0.9500 | C82—C83 | 1.385 (5) |
C30—H30 | 0.9500 | C82—H82 | 0.9500 |
C31—C32 | 1.395 (5) | C83—C84 | 1.383 (5) |
C31—C36 | 1.399 (5) | C83—H83 | 0.9500 |
C32—C33 | 1.392 (5) | C84—C85 | 1.379 (5) |
C32—H32 | 0.9500 | C84—H84 | 0.9500 |
C33—C34 | 1.375 (6) | C85—C86 | 1.388 (5) |
C33—H33 | 0.9500 | C85—H85 | 0.9500 |
C34—C35 | 1.349 (6) | C86—H86 | 0.9500 |
C34—H34 | 0.9500 | C87—C88 | 1.385 (5) |
C35—C36 | 1.404 (5) | C87—C92 | 1.535 (5) |
C35—H35 | 0.9500 | C87—H87 | 1.0000 |
C36—H36 | 0.9500 | C88—C89 | 1.538 (5) |
C37—C38 | 1.378 (5) | C88—H88 | 1.0000 |
C37—C42 | 1.534 (5) | C89—C90 | 1.529 (5) |
C37—H37 | 1.0000 | C89—C93 | 1.547 (5) |
C38—C39 | 1.530 (5) | C89—H89 | 1.0000 |
C38—H38 | 1.0000 | C90—C91 | 1.375 (5) |
C39—C40 | 1.530 (5) | C90—H90 | 1.0000 |
C39—C43 | 1.554 (5) | C91—C92 | 1.534 (5) |
C39—H39 | 1.0000 | C91—H91 | 1.0000 |
C40—C41 | 1.376 (6) | C92—C93 | 1.549 (5) |
C40—H40 | 1.0000 | C92—H92 | 1.0000 |
C41—C42 | 1.530 (5) | C93—H93A | 0.9900 |
C41—H41 | 1.0000 | C93—H93B | 0.9900 |
C42—C43 | 1.530 (5) | B1—F1 | 1.336 (4) |
C42—H42 | 1.0000 | B1—F4 | 1.363 (4) |
C43—H43A | 0.9900 | B1—F2 | 1.372 (4) |
C43—H43B | 0.9900 | B1—F3 | 1.372 (5) |
Rh2—C88 | 2.163 (3) | B2—F5 | 1.356 (5) |
Rh2—C90 | 2.190 (3) | B2—F6 | 1.361 (5) |
Rh2—C87 | 2.214 (3) | B2—F8 | 1.369 (5) |
Rh2—C91 | 2.222 (3) | B2—F7 | 1.372 (5) |
| | | |
C40—Rh1—C38 | 65.71 (14) | C88—Rh2—P4 | 147.11 (10) |
C40—Rh1—C37 | 77.31 (14) | C90—Rh2—P4 | 89.94 (10) |
C38—Rh1—C37 | 36.74 (14) | C87—Rh2—P4 | 161.10 (10) |
C40—Rh1—C41 | 36.65 (15) | C91—Rh2—P4 | 96.76 (10) |
C38—Rh1—C41 | 77.34 (14) | C88—Rh2—P3 | 97.60 (10) |
C37—Rh1—C41 | 64.92 (14) | C90—Rh2—P3 | 155.61 (10) |
C40—Rh1—P2 | 150.43 (11) | C87—Rh2—P3 | 100.93 (10) |
C38—Rh1—P2 | 91.03 (10) | C91—Rh2—P3 | 162.05 (10) |
C37—Rh1—P2 | 95.15 (10) | P4—Rh2—P3 | 96.47 (3) |
C41—Rh1—P2 | 158.76 (11) | C69—P3—C63 | 102.63 (15) |
C40—Rh1—P1 | 102.00 (10) | C69—P3—C51 | 106.54 (14) |
C38—Rh1—P1 | 167.48 (10) | C63—P3—C51 | 101.43 (14) |
C37—Rh1—P1 | 146.40 (10) | C69—P3—Rh2 | 113.06 (10) |
C41—Rh1—P1 | 94.18 (10) | C63—P3—Rh2 | 116.14 (11) |
P2—Rh1—P1 | 99.77 (3) | C51—P3—Rh2 | 115.53 (10) |
C13—P1—C19 | 104.61 (17) | C75—P4—C62 | 105.43 (14) |
C13—P1—C1 | 106.44 (16) | C75—P4—C81 | 103.21 (14) |
C19—P1—C1 | 99.01 (16) | C62—P4—C81 | 103.39 (14) |
C13—P1—Rh1 | 106.86 (12) | C75—P4—Rh2 | 112.87 (11) |
C19—P1—Rh1 | 114.43 (12) | C62—P4—Rh2 | 122.58 (10) |
C1—P1—Rh1 | 123.80 (12) | C81—P4—Rh2 | 107.36 (10) |
C31—P2—C25 | 105.41 (16) | C57—O2—C56 | 115.6 (2) |
C31—P2—C12 | 104.13 (15) | C56—C51—C52 | 117.0 (3) |
C25—P2—C12 | 103.47 (16) | C56—C51—P3 | 121.1 (2) |
C31—P2—Rh1 | 110.54 (11) | C52—C51—P3 | 121.9 (2) |
C25—P2—Rh1 | 107.19 (11) | C53—C52—C51 | 121.6 (3) |
C12—P2—Rh1 | 124.51 (11) | C53—C52—H52 | 119.2 |
C6—O1—C7 | 115.4 (3) | C51—C52—H52 | 119.2 |
C6—C1—C2 | 117.0 (3) | C54—C53—C52 | 119.6 (3) |
C6—C1—P1 | 121.6 (3) | C54—C53—H53 | 120.2 |
C2—C1—P1 | 121.2 (3) | C52—C53—H53 | 120.2 |
C3—C2—C1 | 120.9 (3) | C53—C54—C55 | 120.6 (3) |
C3—C2—H2 | 119.6 | C53—C54—H54 | 119.7 |
C1—C2—H2 | 119.6 | C55—C54—H54 | 119.7 |
C4—C3—C2 | 120.4 (4) | C56—C55—C54 | 118.7 (3) |
C4—C3—H3 | 119.8 | C56—C55—H55 | 120.7 |
C2—C3—H3 | 119.8 | C54—C55—H55 | 120.7 |
C3—C4—C5 | 119.9 (4) | C55—C56—C51 | 122.5 (3) |
C3—C4—H4 | 120.0 | C55—C56—O2 | 118.5 (3) |
C5—C4—H4 | 120.0 | C51—C56—O2 | 118.9 (3) |
C6—C5—C4 | 119.2 (4) | C58—C57—O2 | 121.5 (3) |
C6—C5—H5 | 120.4 | C58—C57—C62 | 121.9 (3) |
C4—C5—H5 | 120.4 | O2—C57—C62 | 116.6 (3) |
C5—C6—O1 | 118.5 (3) | C59—C58—C57 | 118.6 (3) |
C5—C6—C1 | 122.4 (3) | C59—C58—H58 | 120.7 |
O1—C6—C1 | 119.1 (3) | C57—C58—H58 | 120.7 |
C12—C7—C8 | 122.2 (3) | C58—C59—C60 | 121.0 (3) |
C12—C7—O1 | 114.7 (3) | C58—C59—H59 | 119.5 |
C8—C7—O1 | 123.0 (3) | C60—C59—H59 | 119.5 |
C9—C8—C7 | 118.8 (4) | C59—C60—C61 | 119.5 (3) |
C9—C8—H8 | 120.6 | C59—C60—H60 | 120.2 |
C7—C8—H8 | 120.6 | C61—C60—H60 | 120.2 |
C8—C9—C10 | 119.9 (3) | C60—C61—C62 | 121.1 (3) |
C8—C9—H9 | 120.1 | C60—C61—H61 | 119.5 |
C10—C9—H9 | 120.1 | C62—C61—H61 | 119.5 |
C11—C10—C9 | 119.9 (4) | C61—C62—C57 | 117.8 (3) |
C11—C10—H10 | 120.1 | C61—C62—P4 | 123.8 (2) |
C9—C10—H10 | 120.1 | C57—C62—P4 | 118.4 (2) |
C10—C11—C12 | 121.9 (4) | C64—C63—C68 | 118.7 (3) |
C10—C11—H11 | 119.1 | C64—C63—P3 | 122.8 (3) |
C12—C11—H11 | 119.1 | C68—C63—P3 | 118.6 (3) |
C7—C12—C11 | 117.2 (3) | C65—C64—C63 | 120.2 (4) |
C7—C12—P2 | 116.6 (3) | C65—C64—H64 | 119.9 |
C11—C12—P2 | 126.1 (3) | C63—C64—H64 | 119.9 |
C18—C13—C14 | 119.6 (4) | C66—C65—C64 | 120.7 (4) |
C18—C13—P1 | 123.4 (3) | C66—C65—H65 | 119.7 |
C14—C13—P1 | 116.9 (3) | C64—C65—H65 | 119.7 |
C15—C14—C13 | 120.4 (5) | C65—C66—C67 | 119.8 (4) |
C15—C14—H14 | 119.8 | C65—C66—H66 | 120.1 |
C13—C14—H14 | 119.8 | C67—C66—H66 | 120.1 |
C14—C15—C16 | 119.2 (5) | C66—C67—C68 | 119.7 (4) |
C14—C15—H15 | 120.4 | C66—C67—H67 | 120.1 |
C16—C15—H15 | 120.4 | C68—C67—H67 | 120.1 |
C17—C16—C15 | 121.6 (4) | C67—C68—C63 | 120.9 (3) |
C17—C16—H16 | 119.2 | C67—C68—H68 | 119.6 |
C15—C16—H16 | 119.2 | C63—C68—H68 | 119.6 |
C16—C17—C18 | 120.6 (5) | C70—C69—C74 | 119.7 (3) |
C16—C17—H17 | 119.7 | C70—C69—P3 | 124.0 (2) |
C18—C17—H17 | 119.7 | C74—C69—P3 | 116.3 (2) |
C13—C18—C17 | 118.4 (4) | C69—C70—C71 | 119.8 (3) |
C13—C18—H18 | 120.8 | C69—C70—H70 | 120.1 |
C17—C18—H18 | 120.8 | C71—C70—H70 | 120.1 |
C20—C19—C24 | 119.6 (4) | C72—C71—C70 | 120.4 (3) |
C20—C19—P1 | 118.3 (3) | C72—C71—H71 | 119.8 |
C24—C19—P1 | 122.1 (3) | C70—C71—H71 | 119.8 |
C19—C20—C21 | 120.7 (4) | C73—C72—C71 | 119.7 (3) |
C19—C20—H20 | 119.6 | C73—C72—H72 | 120.1 |
C21—C20—H20 | 119.6 | C71—C72—H72 | 120.1 |
C22—C21—C20 | 119.3 (5) | C74—C73—C72 | 120.3 (3) |
C22—C21—H21 | 120.3 | C74—C73—H73 | 119.8 |
C20—C21—H21 | 120.3 | C72—C73—H73 | 119.8 |
C23—C22—C21 | 121.0 (4) | C73—C74—C69 | 120.0 (3) |
C23—C22—H22 | 119.5 | C73—C74—H74 | 120.0 |
C21—C22—H22 | 119.5 | C69—C74—H74 | 120.0 |
C22—C23—C24 | 119.9 (5) | C76—C75—C80 | 118.8 (3) |
C22—C23—H23 | 120.0 | C76—C75—P4 | 119.3 (2) |
C24—C23—H23 | 120.0 | C80—C75—P4 | 121.8 (2) |
C19—C24—C23 | 119.5 (5) | C75—C76—C77 | 120.9 (3) |
C19—C24—H24 | 120.2 | C75—C76—H76 | 119.6 |
C23—C24—H24 | 120.2 | C77—C76—H76 | 119.6 |
C26—C25—C30 | 118.5 (3) | C78—C77—C76 | 120.2 (3) |
C26—C25—P2 | 122.5 (3) | C78—C77—H77 | 119.9 |
C30—C25—P2 | 118.4 (3) | C76—C77—H77 | 119.9 |
C27—C26—C25 | 121.2 (4) | C77—C78—C79 | 119.7 (3) |
C27—C26—H26 | 119.4 | C77—C78—H78 | 120.2 |
C25—C26—H26 | 119.4 | C79—C78—H78 | 120.2 |
C26—C27—C28 | 119.2 (4) | C80—C79—C78 | 120.4 (3) |
C26—C27—H27 | 120.4 | C80—C79—H79 | 119.8 |
C28—C27—H27 | 120.4 | C78—C79—H79 | 119.8 |
C29—C28—C27 | 120.0 (4) | C79—C80—C75 | 120.1 (3) |
C29—C28—H28 | 120.0 | C79—C80—H80 | 120.0 |
C27—C28—H28 | 120.0 | C75—C80—H80 | 120.0 |
C28—C29—C30 | 121.9 (4) | C82—C81—C86 | 118.7 (3) |
C28—C29—H29 | 119.0 | C82—C81—P4 | 120.7 (2) |
C30—C29—H29 | 119.0 | C86—C81—P4 | 120.4 (2) |
C29—C30—C25 | 119.2 (4) | C83—C82—C81 | 121.0 (3) |
C29—C30—H30 | 120.4 | C83—C82—H82 | 119.5 |
C25—C30—H30 | 120.4 | C81—C82—H82 | 119.5 |
C32—C31—C36 | 119.3 (3) | C84—C83—C82 | 119.8 (3) |
C32—C31—P2 | 120.9 (3) | C84—C83—H83 | 120.1 |
C36—C31—P2 | 119.8 (3) | C82—C83—H83 | 120.1 |
C33—C32—C31 | 120.6 (4) | C85—C84—C83 | 119.8 (3) |
C33—C32—H32 | 119.7 | C85—C84—H84 | 120.1 |
C31—C32—H32 | 119.7 | C83—C84—H84 | 120.1 |
C34—C33—C32 | 119.1 (4) | C84—C85—C86 | 120.8 (3) |
C34—C33—H33 | 120.4 | C84—C85—H85 | 119.6 |
C32—C33—H33 | 120.4 | C86—C85—H85 | 119.6 |
C35—C34—C33 | 121.2 (4) | C85—C86—C81 | 119.9 (3) |
C35—C34—H34 | 119.4 | C85—C86—H86 | 120.0 |
C33—C34—H34 | 119.4 | C81—C86—H86 | 120.0 |
C34—C35—C36 | 121.2 (4) | C88—C87—C92 | 106.7 (3) |
C34—C35—H35 | 119.4 | C88—C87—Rh2 | 69.56 (19) |
C36—C35—H35 | 119.4 | C92—C87—Rh2 | 97.1 (2) |
C31—C36—C35 | 118.5 (4) | C88—C87—H87 | 123.2 |
C31—C36—H36 | 120.7 | C92—C87—H87 | 123.2 |
C35—C36—H36 | 120.7 | Rh2—C87—H87 | 123.2 |
C38—C37—C42 | 106.4 (3) | C87—C88—C89 | 106.5 (3) |
C38—C37—Rh1 | 71.3 (2) | C87—C88—Rh2 | 73.6 (2) |
C42—C37—Rh1 | 97.4 (2) | C89—C88—Rh2 | 96.4 (2) |
C38—C37—H37 | 122.9 | C87—C88—H88 | 122.7 |
C42—C37—H37 | 122.9 | C89—C88—H88 | 122.7 |
Rh1—C37—H37 | 122.9 | Rh2—C88—H88 | 122.7 |
C37—C38—C39 | 106.5 (3) | C90—C89—C88 | 101.4 (3) |
C37—C38—Rh1 | 71.9 (2) | C90—C89—C93 | 100.0 (3) |
C39—C38—Rh1 | 96.3 (2) | C88—C89—C93 | 100.2 (3) |
C37—C38—H38 | 123.0 | C90—C89—H89 | 117.4 |
C39—C38—H38 | 123.0 | C88—C89—H89 | 117.4 |
Rh1—C38—H38 | 123.0 | C93—C89—H89 | 117.4 |
C40—C39—C38 | 101.2 (3) | C91—C90—C89 | 107.1 (3) |
C40—C39—C43 | 100.4 (3) | C91—C90—Rh2 | 73.1 (2) |
C38—C39—C43 | 99.9 (3) | C89—C90—Rh2 | 95.6 (2) |
C40—C39—H39 | 117.4 | C91—C90—H90 | 122.8 |
C38—C39—H39 | 117.4 | C89—C90—H90 | 122.8 |
C43—C39—H39 | 117.4 | Rh2—C90—H90 | 122.8 |
C41—C40—C39 | 106.7 (3) | C90—C91—C92 | 106.6 (3) |
C41—C40—Rh1 | 72.5 (2) | C90—C91—Rh2 | 70.57 (19) |
C39—C40—Rh1 | 96.5 (2) | C92—C91—Rh2 | 96.8 (2) |
C41—C40—H40 | 122.8 | C90—C91—H91 | 123.1 |
C39—C40—H40 | 122.8 | C92—C91—H91 | 123.1 |
Rh1—C40—H40 | 122.8 | Rh2—C91—H91 | 123.1 |
C40—C41—C42 | 106.4 (3) | C91—C92—C87 | 101.3 (3) |
C40—C41—Rh1 | 70.8 (2) | C91—C92—C93 | 100.2 (3) |
C42—C41—Rh1 | 97.1 (2) | C87—C92—C93 | 100.0 (3) |
C40—C41—H41 | 123.0 | C91—C92—H92 | 117.4 |
C42—C41—H41 | 123.0 | C87—C92—H92 | 117.4 |
Rh1—C41—H41 | 123.0 | C93—C92—H92 | 117.4 |
C43—C42—C41 | 101.1 (3) | C89—C93—C92 | 93.9 (3) |
C43—C42—C37 | 100.7 (3) | C89—C93—H93A | 112.9 |
C41—C42—C37 | 100.5 (3) | C92—C93—H93A | 112.9 |
C43—C42—H42 | 117.2 | C89—C93—H93B | 112.9 |
C41—C42—H42 | 117.2 | C92—C93—H93B | 112.9 |
C37—C42—H42 | 117.2 | H93A—C93—H93B | 110.4 |
C42—C43—C39 | 93.6 (3) | F1—B1—F4 | 113.8 (4) |
C42—C43—H43A | 113.0 | F1—B1—F2 | 109.5 (3) |
C39—C43—H43A | 113.0 | F4—B1—F2 | 108.1 (3) |
C42—C43—H43B | 113.0 | F1—B1—F3 | 109.3 (4) |
C39—C43—H43B | 113.0 | F4—B1—F3 | 108.5 (4) |
H43A—C43—H43B | 110.4 | F2—B1—F3 | 107.5 (4) |
C88—Rh2—C90 | 66.08 (14) | F5—B2—F6 | 109.9 (4) |
C88—Rh2—C87 | 36.87 (13) | F5—B2—F8 | 109.7 (4) |
C90—Rh2—C87 | 77.21 (13) | F6—B2—F8 | 110.5 (4) |
C88—Rh2—C91 | 77.44 (14) | F5—B2—F7 | 110.0 (4) |
C90—Rh2—C91 | 36.31 (13) | F6—B2—F7 | 109.6 (4) |
C87—Rh2—C91 | 64.71 (13) | F8—B2—F7 | 107.0 (4) |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
C36—H36···F8i | 0.95 | 2.55 | 3.418 (5) | 152 |
C68—H68···F4 | 0.95 | 2.49 | 3.094 (5) | 122 |
C74—H74···F2ii | 0.95 | 2.48 | 3.395 (5) | 161 |
C86—H86···O2 | 0.95 | 2.37 | 3.152 (4) | 140 |
Symmetry codes: (i) −x+1, y+1/2, −z+1/2; (ii) x, −y+1/2, z−1/2. |
{Bis[(2-diphenylphosphanyl)phenyl]
ether-
κ2P,
P'}[
η4-(
Z,
Z)-cycloocta-1,5-\
diene]rhodium(I) tetrafluoridoborate dichloromethane monosolvate (compII)
top
Crystal data top
[Rh(C8H12)(C36H28OP2)]BF4·CH2Cl2 | Z = 2 |
Mr = 921.34 | F(000) = 940 |
Triclinic, P1 | Dx = 1.574 Mg m−3 |
a = 11.3056 (3) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 12.8231 (4) Å | Cell parameters from 9759 reflections |
c = 14.6101 (4) Å | θ = 2.2–27.3° |
α = 83.286 (1)° | µ = 0.72 mm−1 |
β = 74.695 (1)° | T = 150 K |
γ = 72.262 (1)° | Rod, orange |
V = 1944.29 (10) Å3 | 0.35 × 0.15 × 0.12 mm |
Data collection top
Bruker APEXII CCD diffractometer | 7240 independent reflections |
Radiation source: sealed tube | 6334 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.048 |
Detector resolution: 8.33 pixels mm-1 | θmax = 25.5°, θmin = 1.7° |
φ and ω scans | h = −13→13 |
Absorption correction: multi-scan (SADABS; Bruker, 2014) | k = −15→15 |
Tmin = 0.863, Tmax = 0.996 | l = −17→17 |
67143 measured reflections | |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.045 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.127 | H-atom parameters constrained |
S = 1.08 | w = 1/[σ2(Fo2) + (0.0636P)2 + 6.1906P] where P = (Fo2 + 2Fc2)/3 |
7240 reflections | (Δ/σ)max = 0.002 |
533 parameters | Δρmax = 1.53 e Å−3 |
69 restraints | Δρmin = −1.06 e Å−3 |
Special details top
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Rh1 | 0.45096 (3) | 0.19856 (2) | 0.36409 (2) | 0.01773 (11) | |
P1 | 0.47334 (9) | 0.11771 (8) | 0.21906 (7) | 0.0171 (2) | |
P2 | 0.62749 (9) | 0.27166 (8) | 0.30918 (7) | 0.0176 (2) | |
O1 | 0.7523 (2) | 0.0578 (2) | 0.23351 (18) | 0.0195 (6) | |
C1 | 0.7276 (3) | 0.2450 (3) | 0.1893 (3) | 0.0187 (8) | |
C2 | 0.7493 (4) | 0.3262 (4) | 0.1205 (3) | 0.0256 (9) | |
H2 | 0.7140 | 0.4011 | 0.1362 | 0.031* | |
C3 | 0.8218 (4) | 0.2994 (4) | 0.0294 (3) | 0.0291 (9) | |
H3 | 0.8356 | 0.3557 | −0.0169 | 0.035* | |
C4 | 0.8739 (4) | 0.1911 (4) | 0.0060 (3) | 0.0288 (9) | |
H4 | 0.9249 | 0.1730 | −0.0562 | 0.035* | |
C5 | 0.8525 (4) | 0.1086 (3) | 0.0724 (3) | 0.0237 (8) | |
H5 | 0.8878 | 0.0339 | 0.0563 | 0.028* | |
C6 | 0.7788 (4) | 0.1366 (3) | 0.1630 (3) | 0.0200 (8) | |
C7 | 0.7240 (4) | −0.0266 (3) | 0.1992 (3) | 0.0199 (8) | |
C8 | 0.8156 (4) | −0.1259 (3) | 0.1854 (3) | 0.0231 (8) | |
H8 | 0.8930 | −0.1386 | 0.2046 | 0.028* | |
C9 | 0.7941 (4) | −0.2073 (3) | 0.1433 (3) | 0.0283 (9) | |
H9 | 0.8559 | −0.2771 | 0.1344 | 0.034* | |
C10 | 0.6817 (4) | −0.1864 (4) | 0.1143 (3) | 0.0279 (9) | |
H10 | 0.6691 | −0.2401 | 0.0811 | 0.033* | |
C11 | 0.5883 (4) | −0.0887 (3) | 0.1331 (3) | 0.0233 (8) | |
H11 | 0.5106 | −0.0767 | 0.1145 | 0.028* | |
C12 | 0.6051 (4) | −0.0063 (3) | 0.1789 (3) | 0.0193 (8) | |
C13 | 0.7450 (4) | 0.2369 (3) | 0.3825 (3) | 0.0205 (8) | |
C14 | 0.8593 (4) | 0.1540 (4) | 0.3600 (3) | 0.0273 (9) | |
H14 | 0.8787 | 0.1134 | 0.3049 | 0.033* | |
C15 | 0.9463 (4) | 0.1296 (4) | 0.4178 (3) | 0.0331 (10) | |
H15 | 1.0235 | 0.0719 | 0.4023 | 0.040* | |
C16 | 0.9200 (4) | 0.1889 (4) | 0.4964 (3) | 0.0345 (10) | |
H16 | 0.9794 | 0.1729 | 0.5351 | 0.041* | |
C17 | 0.8074 (4) | 0.2720 (4) | 0.5194 (3) | 0.0338 (10) | |
H17 | 0.7896 | 0.3133 | 0.5738 | 0.041* | |
C18 | 0.7200 (4) | 0.2957 (4) | 0.4634 (3) | 0.0290 (9) | |
H18 | 0.6422 | 0.3525 | 0.4804 | 0.035* | |
C19 | 0.5799 (4) | 0.4218 (3) | 0.3056 (3) | 0.0206 (8) | |
C20 | 0.6676 (4) | 0.4788 (4) | 0.3045 (3) | 0.0267 (9) | |
H20 | 0.7510 | 0.4396 | 0.3116 | 0.032* | |
C21 | 0.6340 (5) | 0.5915 (4) | 0.2932 (3) | 0.0314 (10) | |
H21 | 0.6942 | 0.6297 | 0.2928 | 0.038* | |
C22 | 0.5132 (5) | 0.6489 (4) | 0.2825 (3) | 0.0318 (10) | |
H22 | 0.4901 | 0.7266 | 0.2750 | 0.038* | |
C23 | 0.4260 (4) | 0.5933 (4) | 0.2827 (3) | 0.0300 (9) | |
H23 | 0.3433 | 0.6329 | 0.2745 | 0.036* | |
C24 | 0.4581 (4) | 0.4807 (3) | 0.2948 (3) | 0.0237 (8) | |
H24 | 0.3971 | 0.4432 | 0.2957 | 0.028* | |
C25 | 0.4803 (4) | 0.2166 (3) | 0.1192 (3) | 0.0197 (8) | |
C26 | 0.5598 (4) | 0.1890 (3) | 0.0292 (3) | 0.0232 (8) | |
H26 | 0.6132 | 0.1162 | 0.0182 | 0.028* | |
C27 | 0.5602 (4) | 0.2688 (4) | −0.0442 (3) | 0.0290 (9) | |
H27 | 0.6161 | 0.2512 | −0.1049 | 0.035* | |
C28 | 0.4788 (4) | 0.3739 (4) | −0.0282 (3) | 0.0308 (10) | |
H28 | 0.4780 | 0.4277 | −0.0787 | 0.037* | |
C29 | 0.3987 (4) | 0.4014 (4) | 0.0603 (3) | 0.0301 (9) | |
H29 | 0.3432 | 0.4736 | 0.0706 | 0.036* | |
C30 | 0.4001 (4) | 0.3229 (3) | 0.1338 (3) | 0.0243 (8) | |
H30 | 0.3458 | 0.3416 | 0.1949 | 0.029* | |
C31 | 0.3398 (4) | 0.0673 (3) | 0.2132 (3) | 0.0205 (8) | |
C32 | 0.3212 (4) | −0.0267 (3) | 0.2661 (3) | 0.0247 (9) | |
H32 | 0.3743 | −0.0614 | 0.3081 | 0.030* | |
C33 | 0.2266 (4) | −0.0700 (4) | 0.2582 (3) | 0.0304 (10) | |
H33 | 0.2156 | −0.1344 | 0.2943 | 0.036* | |
C34 | 0.1480 (4) | −0.0198 (4) | 0.1981 (4) | 0.0353 (11) | |
H34 | 0.0826 | −0.0495 | 0.1932 | 0.042* | |
C35 | 0.1645 (4) | 0.0734 (4) | 0.1453 (3) | 0.0345 (10) | |
H35 | 0.1107 | 0.1078 | 0.1037 | 0.041* | |
C36 | 0.2596 (4) | 0.1170 (4) | 0.1529 (3) | 0.0269 (9) | |
H36 | 0.2702 | 0.1814 | 0.1167 | 0.032* | |
C37 | 0.3889 (4) | 0.3114 (4) | 0.4845 (3) | 0.0243 (9) | |
H37 | 0.4384 | 0.3660 | 0.4754 | 0.029* | |
C38 | 0.4538 (4) | 0.2081 (4) | 0.5132 (3) | 0.0271 (9) | |
H38 | 0.5402 | 0.2035 | 0.5216 | 0.033* | |
C39 | 0.3940 (4) | 0.1283 (4) | 0.5752 (3) | 0.0295 (9) | |
H39A | 0.3691 | 0.1510 | 0.6417 | 0.035* | |
H39B | 0.4583 | 0.0555 | 0.5718 | 0.035* | |
C40 | 0.2760 (4) | 0.1176 (4) | 0.5487 (3) | 0.0311 (10) | |
H40A | 0.2641 | 0.0448 | 0.5711 | 0.037* | |
H40B | 0.1992 | 0.1741 | 0.5809 | 0.037* | |
C41 | 0.2893 (4) | 0.1312 (4) | 0.4419 (3) | 0.0251 (9) | |
H41 | 0.2868 | 0.0654 | 0.4127 | 0.030* | |
C42 | 0.2416 (4) | 0.2295 (4) | 0.3951 (3) | 0.0247 (9) | |
H42 | 0.2105 | 0.2205 | 0.3393 | 0.030* | |
C43 | 0.1793 (4) | 0.3395 (4) | 0.4379 (3) | 0.0318 (10) | |
H43A | 0.0889 | 0.3447 | 0.4698 | 0.038* | |
H43B | 0.1796 | 0.3969 | 0.3863 | 0.038* | |
C44 | 0.2452 (4) | 0.3622 (4) | 0.5102 (3) | 0.0319 (10) | |
H44A | 0.2264 | 0.4423 | 0.5142 | 0.038* | |
H44B | 0.2090 | 0.3328 | 0.5737 | 0.038* | |
B1 | 0.0760 (4) | 0.6454 (3) | 0.2708 (3) | 0.0338 (12) | |
F1 | −0.0415 (3) | 0.6392 (3) | 0.2676 (3) | 0.0623 (9) | |
F2 | 0.0927 (10) | 0.7438 (6) | 0.2437 (12) | 0.091 (5) | 0.47 (2) |
F3 | 0.0881 (9) | 0.6184 (12) | 0.3629 (4) | 0.068 (4) | 0.47 (2) |
F4 | 0.1700 (5) | 0.5658 (10) | 0.2151 (9) | 0.073 (4) | 0.47 (2) |
F2' | 0.1176 (11) | 0.5802 (9) | 0.3418 (9) | 0.091 (4) | 0.53 (2) |
F3' | 0.1598 (8) | 0.6185 (16) | 0.1861 (7) | 0.129 (6) | 0.53 (2) |
F4' | 0.0652 (9) | 0.7528 (4) | 0.2872 (11) | 0.081 (4) | 0.53 (2) |
C45 | 0.0124 (7) | 0.4413 (5) | 0.1458 (5) | 0.0618 (17) | |
H45A | 0.0472 | 0.5006 | 0.1542 | 0.074* | |
H45B | −0.0773 | 0.4750 | 0.1414 | 0.074* | |
Cl1 | 0.01502 (15) | 0.35083 (15) | 0.24415 (12) | 0.0660 (4) | |
Cl2 | 0.10115 (16) | 0.37698 (15) | 0.04030 (12) | 0.0640 (4) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Rh1 | 0.01555 (16) | 0.02420 (18) | 0.01589 (17) | −0.00779 (12) | −0.00490 (11) | −0.00207 (11) |
P1 | 0.0158 (5) | 0.0208 (5) | 0.0173 (5) | −0.0072 (4) | −0.0060 (4) | −0.0009 (4) |
P2 | 0.0157 (5) | 0.0207 (5) | 0.0183 (5) | −0.0060 (4) | −0.0051 (4) | −0.0036 (4) |
O1 | 0.0208 (13) | 0.0223 (14) | 0.0190 (13) | −0.0084 (11) | −0.0070 (11) | −0.0029 (11) |
C1 | 0.0142 (17) | 0.027 (2) | 0.0187 (19) | −0.0089 (15) | −0.0058 (14) | −0.0032 (15) |
C2 | 0.023 (2) | 0.031 (2) | 0.027 (2) | −0.0112 (17) | −0.0079 (17) | −0.0039 (17) |
C3 | 0.033 (2) | 0.040 (3) | 0.022 (2) | −0.022 (2) | −0.0074 (18) | 0.0056 (18) |
C4 | 0.026 (2) | 0.041 (3) | 0.021 (2) | −0.0157 (19) | 0.0008 (17) | −0.0069 (18) |
C5 | 0.0175 (19) | 0.030 (2) | 0.025 (2) | −0.0077 (16) | −0.0032 (16) | −0.0082 (17) |
C6 | 0.0171 (18) | 0.027 (2) | 0.0209 (19) | −0.0105 (16) | −0.0091 (15) | −0.0005 (16) |
C7 | 0.0220 (19) | 0.023 (2) | 0.0173 (19) | −0.0107 (16) | −0.0043 (15) | −0.0001 (15) |
C8 | 0.0200 (19) | 0.028 (2) | 0.022 (2) | −0.0085 (16) | −0.0050 (16) | −0.0009 (16) |
C9 | 0.028 (2) | 0.023 (2) | 0.033 (2) | −0.0058 (17) | −0.0061 (18) | −0.0027 (17) |
C10 | 0.031 (2) | 0.028 (2) | 0.028 (2) | −0.0136 (18) | −0.0036 (18) | −0.0080 (18) |
C11 | 0.024 (2) | 0.029 (2) | 0.020 (2) | −0.0108 (17) | −0.0058 (16) | −0.0044 (16) |
C12 | 0.0184 (18) | 0.0219 (19) | 0.0182 (19) | −0.0070 (15) | −0.0047 (15) | 0.0010 (15) |
C13 | 0.0178 (18) | 0.026 (2) | 0.021 (2) | −0.0105 (16) | −0.0069 (15) | 0.0015 (16) |
C14 | 0.027 (2) | 0.031 (2) | 0.027 (2) | −0.0064 (18) | −0.0105 (17) | −0.0076 (18) |
C15 | 0.025 (2) | 0.037 (3) | 0.038 (3) | −0.0035 (19) | −0.0143 (19) | −0.007 (2) |
C16 | 0.028 (2) | 0.053 (3) | 0.031 (2) | −0.015 (2) | −0.0155 (19) | 0.000 (2) |
C17 | 0.029 (2) | 0.051 (3) | 0.026 (2) | −0.015 (2) | −0.0078 (18) | −0.010 (2) |
C18 | 0.023 (2) | 0.039 (2) | 0.026 (2) | −0.0076 (18) | −0.0061 (17) | −0.0077 (18) |
C19 | 0.0225 (19) | 0.0214 (19) | 0.0182 (19) | −0.0061 (16) | −0.0037 (15) | −0.0051 (15) |
C20 | 0.023 (2) | 0.029 (2) | 0.029 (2) | −0.0084 (17) | −0.0061 (17) | −0.0048 (17) |
C21 | 0.041 (3) | 0.030 (2) | 0.030 (2) | −0.018 (2) | −0.0080 (19) | −0.0065 (18) |
C22 | 0.046 (3) | 0.023 (2) | 0.025 (2) | −0.0070 (19) | −0.0069 (19) | −0.0050 (17) |
C23 | 0.031 (2) | 0.031 (2) | 0.023 (2) | −0.0008 (18) | −0.0049 (17) | −0.0036 (17) |
C24 | 0.025 (2) | 0.027 (2) | 0.020 (2) | −0.0079 (17) | −0.0057 (16) | −0.0013 (16) |
C25 | 0.0205 (19) | 0.023 (2) | 0.022 (2) | −0.0111 (15) | −0.0120 (16) | 0.0016 (15) |
C26 | 0.024 (2) | 0.029 (2) | 0.023 (2) | −0.0104 (17) | −0.0108 (16) | −0.0024 (16) |
C27 | 0.035 (2) | 0.041 (3) | 0.020 (2) | −0.022 (2) | −0.0095 (18) | 0.0023 (18) |
C28 | 0.042 (3) | 0.029 (2) | 0.033 (2) | −0.020 (2) | −0.021 (2) | 0.0100 (18) |
C29 | 0.035 (2) | 0.026 (2) | 0.036 (2) | −0.0123 (18) | −0.015 (2) | 0.0000 (18) |
C30 | 0.025 (2) | 0.028 (2) | 0.025 (2) | −0.0123 (17) | −0.0098 (17) | −0.0005 (17) |
C31 | 0.0189 (18) | 0.022 (2) | 0.0207 (19) | −0.0056 (15) | −0.0046 (15) | −0.0052 (15) |
C32 | 0.024 (2) | 0.027 (2) | 0.025 (2) | −0.0087 (17) | −0.0055 (17) | −0.0032 (17) |
C33 | 0.030 (2) | 0.030 (2) | 0.032 (2) | −0.0158 (18) | 0.0024 (18) | −0.0072 (18) |
C34 | 0.026 (2) | 0.042 (3) | 0.046 (3) | −0.018 (2) | −0.005 (2) | −0.015 (2) |
C35 | 0.026 (2) | 0.045 (3) | 0.039 (3) | −0.013 (2) | −0.015 (2) | −0.006 (2) |
C36 | 0.026 (2) | 0.028 (2) | 0.031 (2) | −0.0097 (17) | −0.0123 (18) | −0.0001 (18) |
C37 | 0.027 (2) | 0.033 (2) | 0.0152 (19) | −0.0127 (18) | −0.0007 (16) | −0.0087 (16) |
C38 | 0.028 (2) | 0.042 (3) | 0.018 (2) | −0.0164 (19) | −0.0074 (17) | −0.0050 (18) |
C39 | 0.031 (2) | 0.042 (3) | 0.018 (2) | −0.015 (2) | −0.0077 (17) | 0.0006 (18) |
C40 | 0.030 (2) | 0.042 (3) | 0.024 (2) | −0.019 (2) | −0.0033 (18) | 0.0030 (19) |
C41 | 0.021 (2) | 0.033 (2) | 0.023 (2) | −0.0113 (17) | −0.0045 (16) | −0.0020 (17) |
C42 | 0.0172 (19) | 0.035 (2) | 0.025 (2) | −0.0103 (17) | −0.0058 (16) | −0.0029 (17) |
C43 | 0.025 (2) | 0.036 (3) | 0.033 (2) | −0.0067 (19) | −0.0048 (18) | −0.0069 (19) |
C44 | 0.028 (2) | 0.035 (2) | 0.032 (2) | −0.0084 (19) | −0.0020 (18) | −0.0105 (19) |
B1 | 0.036 (3) | 0.037 (3) | 0.034 (3) | −0.011 (2) | −0.017 (2) | 0.000 (2) |
F1 | 0.0435 (18) | 0.059 (2) | 0.093 (3) | −0.0135 (16) | −0.0293 (18) | −0.0085 (19) |
F2 | 0.101 (8) | 0.061 (7) | 0.131 (11) | −0.048 (6) | −0.054 (8) | 0.042 (6) |
F3 | 0.116 (8) | 0.072 (7) | 0.039 (5) | −0.055 (6) | −0.022 (5) | −0.005 (4) |
F4 | 0.031 (4) | 0.074 (7) | 0.107 (8) | −0.026 (4) | 0.026 (4) | −0.046 (6) |
F2' | 0.148 (9) | 0.041 (5) | 0.138 (9) | −0.044 (5) | −0.123 (8) | 0.031 (5) |
F3' | 0.165 (11) | 0.193 (13) | 0.055 (6) | −0.131 (9) | 0.039 (6) | −0.044 (7) |
F4' | 0.117 (8) | 0.049 (5) | 0.118 (9) | −0.036 (5) | −0.091 (6) | 0.007 (4) |
C45 | 0.069 (4) | 0.056 (4) | 0.057 (4) | −0.015 (3) | −0.008 (3) | −0.014 (3) |
Cl1 | 0.0485 (8) | 0.0719 (11) | 0.0640 (10) | −0.0032 (7) | −0.0115 (7) | 0.0083 (8) |
Cl2 | 0.0563 (9) | 0.0741 (10) | 0.0551 (9) | 0.0005 (8) | −0.0193 (7) | −0.0150 (8) |
Geometric parameters (Å, º) top
Rh1—C38 | 2.206 (4) | C24—H24 | 0.9500 |
Rh1—C42 | 2.206 (4) | C25—C30 | 1.391 (6) |
Rh1—C37 | 2.237 (4) | C25—C26 | 1.397 (6) |
Rh1—C41 | 2.239 (4) | C26—C27 | 1.393 (6) |
Rh1—P2 | 2.3715 (10) | C26—H26 | 0.9500 |
Rh1—P1 | 2.3872 (10) | C27—C28 | 1.387 (7) |
P1—C25 | 1.820 (4) | C27—H27 | 0.9500 |
P1—C31 | 1.839 (4) | C28—C29 | 1.382 (7) |
P1—C12 | 1.845 (4) | C28—H28 | 0.9500 |
P2—C1 | 1.823 (4) | C29—C30 | 1.384 (6) |
P2—C19 | 1.832 (4) | C29—H29 | 0.9500 |
P2—C13 | 1.841 (4) | C30—H30 | 0.9500 |
O1—C7 | 1.396 (5) | C31—C36 | 1.393 (6) |
O1—C6 | 1.396 (5) | C31—C32 | 1.395 (6) |
C1—C6 | 1.391 (6) | C32—C33 | 1.380 (6) |
C1—C2 | 1.391 (6) | C32—H32 | 0.9500 |
C2—C3 | 1.386 (6) | C33—C34 | 1.380 (7) |
C2—H2 | 0.9500 | C33—H33 | 0.9500 |
C3—C4 | 1.378 (6) | C34—C35 | 1.380 (7) |
C3—H3 | 0.9500 | C34—H34 | 0.9500 |
C4—C5 | 1.383 (6) | C35—C36 | 1.388 (6) |
C4—H4 | 0.9500 | C35—H35 | 0.9500 |
C5—C6 | 1.386 (6) | C36—H36 | 0.9500 |
C5—H5 | 0.9500 | C37—C38 | 1.381 (6) |
C7—C8 | 1.371 (6) | C37—C44 | 1.515 (6) |
C7—C12 | 1.394 (5) | C37—H37 | 1.0000 |
C8—C9 | 1.383 (6) | C38—C39 | 1.486 (6) |
C8—H8 | 0.9500 | C38—H38 | 1.0000 |
C9—C10 | 1.385 (6) | C39—C40 | 1.531 (6) |
C9—H9 | 0.9500 | C39—H39A | 0.9900 |
C10—C11 | 1.372 (6) | C39—H39B | 0.9900 |
C10—H10 | 0.9500 | C40—C41 | 1.522 (6) |
C11—C12 | 1.399 (5) | C40—H40A | 0.9900 |
C11—H11 | 0.9500 | C40—H40B | 0.9900 |
C13—C14 | 1.388 (6) | C41—C42 | 1.387 (6) |
C13—C18 | 1.396 (6) | C41—H41 | 1.0000 |
C14—C15 | 1.402 (6) | C42—C43 | 1.499 (6) |
C14—H14 | 0.9500 | C42—H42 | 1.0000 |
C15—C16 | 1.368 (7) | C43—C44 | 1.541 (6) |
C15—H15 | 0.9500 | C43—H43A | 0.9900 |
C16—C17 | 1.379 (7) | C43—H43B | 0.9900 |
C16—H16 | 0.9500 | C44—H44A | 0.9900 |
C17—C18 | 1.386 (6) | C44—H44B | 0.9900 |
C17—H17 | 0.9500 | B1—F2 | 1.333 (5) |
C18—H18 | 0.9500 | B1—F2' | 1.346 (5) |
C19—C24 | 1.395 (6) | B1—F3' | 1.353 (5) |
C19—C20 | 1.396 (6) | B1—F1 | 1.367 (4) |
C20—C21 | 1.380 (6) | B1—F3 | 1.380 (5) |
C20—H20 | 0.9500 | B1—F4 | 1.381 (5) |
C21—C22 | 1.380 (7) | B1—F4' | 1.389 (5) |
C21—H21 | 0.9500 | C45—Cl1 | 1.739 (7) |
C22—C23 | 1.381 (7) | C45—Cl2 | 1.743 (6) |
C22—H22 | 0.9500 | C45—H45A | 0.9900 |
C23—C24 | 1.380 (6) | C45—H45B | 0.9900 |
C23—H23 | 0.9500 | | |
| | | |
C38—Rh1—C42 | 94.41 (16) | C30—C25—P1 | 117.7 (3) |
C38—Rh1—C37 | 36.22 (16) | C26—C25—P1 | 122.6 (3) |
C42—Rh1—C37 | 79.76 (15) | C27—C26—C25 | 119.6 (4) |
C38—Rh1—C41 | 78.44 (15) | C27—C26—H26 | 120.2 |
C42—Rh1—C41 | 36.35 (16) | C25—C26—H26 | 120.2 |
C37—Rh1—C41 | 85.81 (15) | C28—C27—C26 | 119.8 (4) |
C38—Rh1—P2 | 91.28 (11) | C28—C27—H27 | 120.1 |
C42—Rh1—P2 | 147.20 (12) | C26—C27—H27 | 120.1 |
C37—Rh1—P2 | 86.14 (11) | C29—C28—C27 | 120.9 (4) |
C41—Rh1—P2 | 169.71 (11) | C29—C28—H28 | 119.6 |
C38—Rh1—P1 | 158.62 (12) | C27—C28—H28 | 119.6 |
C42—Rh1—P1 | 89.90 (11) | C28—C29—C30 | 119.4 (4) |
C37—Rh1—P1 | 163.98 (11) | C28—C29—H29 | 120.3 |
C41—Rh1—P1 | 93.11 (11) | C30—C29—H29 | 120.3 |
P2—Rh1—P1 | 96.39 (3) | C29—C30—C25 | 120.7 (4) |
C25—P1—C31 | 102.70 (17) | C29—C30—H30 | 119.7 |
C25—P1—C12 | 105.69 (18) | C25—C30—H30 | 119.7 |
C31—P1—C12 | 98.00 (17) | C36—C31—C32 | 118.3 (4) |
C25—P1—Rh1 | 111.48 (13) | C36—C31—P1 | 121.8 (3) |
C31—P1—Rh1 | 115.73 (13) | C32—C31—P1 | 119.9 (3) |
C12—P1—Rh1 | 120.98 (13) | C33—C32—C31 | 120.8 (4) |
C1—P2—C19 | 100.57 (18) | C33—C32—H32 | 119.6 |
C1—P2—C13 | 103.07 (17) | C31—C32—H32 | 119.6 |
C19—P2—C13 | 102.02 (18) | C32—C33—C34 | 120.2 (4) |
C1—P2—Rh1 | 119.61 (12) | C32—C33—H33 | 119.9 |
C19—P2—Rh1 | 112.88 (13) | C34—C33—H33 | 119.9 |
C13—P2—Rh1 | 116.18 (13) | C35—C34—C33 | 119.9 (4) |
C7—O1—C6 | 112.7 (3) | C35—C34—H34 | 120.0 |
C6—C1—C2 | 117.8 (4) | C33—C34—H34 | 120.0 |
C6—C1—P2 | 117.8 (3) | C34—C35—C36 | 120.0 (4) |
C2—C1—P2 | 124.3 (3) | C34—C35—H35 | 120.0 |
C3—C2—C1 | 120.9 (4) | C36—C35—H35 | 120.0 |
C3—C2—H2 | 119.5 | C35—C36—C31 | 120.7 (4) |
C1—C2—H2 | 119.5 | C35—C36—H36 | 119.6 |
C4—C3—C2 | 120.0 (4) | C31—C36—H36 | 119.6 |
C4—C3—H3 | 120.0 | C38—C37—C44 | 125.9 (4) |
C2—C3—H3 | 120.0 | C38—C37—Rh1 | 70.7 (2) |
C3—C4—C5 | 120.4 (4) | C44—C37—Rh1 | 111.9 (3) |
C3—C4—H4 | 119.8 | C38—C37—H37 | 113.5 |
C5—C4—H4 | 119.8 | C44—C37—H37 | 113.5 |
C4—C5—C6 | 118.9 (4) | Rh1—C37—H37 | 113.5 |
C4—C5—H5 | 120.5 | C37—C38—C39 | 125.6 (4) |
C6—C5—H5 | 120.5 | C37—C38—Rh1 | 73.1 (2) |
C5—C6—C1 | 121.9 (4) | C39—C38—Rh1 | 110.8 (3) |
C5—C6—O1 | 122.1 (4) | C37—C38—H38 | 113.4 |
C1—C6—O1 | 116.0 (3) | C39—C38—H38 | 113.4 |
C8—C7—C12 | 122.7 (4) | Rh1—C38—H38 | 113.4 |
C8—C7—O1 | 118.4 (3) | C38—C39—C40 | 113.8 (4) |
C12—C7—O1 | 118.8 (3) | C38—C39—H39A | 108.8 |
C7—C8—C9 | 119.3 (4) | C40—C39—H39A | 108.8 |
C7—C8—H8 | 120.4 | C38—C39—H39B | 108.8 |
C9—C8—H8 | 120.4 | C40—C39—H39B | 108.8 |
C8—C9—C10 | 119.4 (4) | H39A—C39—H39B | 107.7 |
C8—C9—H9 | 120.3 | C41—C40—C39 | 111.5 (3) |
C10—C9—H9 | 120.3 | C41—C40—H40A | 109.3 |
C11—C10—C9 | 120.4 (4) | C39—C40—H40A | 109.3 |
C11—C10—H10 | 119.8 | C41—C40—H40B | 109.3 |
C9—C10—H10 | 119.8 | C39—C40—H40B | 109.3 |
C10—C11—C12 | 121.4 (4) | H40A—C40—H40B | 108.0 |
C10—C11—H11 | 119.3 | C42—C41—C40 | 124.1 (4) |
C12—C11—H11 | 119.3 | C42—C41—Rh1 | 70.5 (2) |
C7—C12—C11 | 116.3 (4) | C40—C41—Rh1 | 113.4 (3) |
C7—C12—P1 | 121.6 (3) | C42—C41—H41 | 113.8 |
C11—C12—P1 | 122.0 (3) | C40—C41—H41 | 113.8 |
C14—C13—C18 | 118.2 (4) | Rh1—C41—H41 | 113.8 |
C14—C13—P2 | 122.3 (3) | C41—C42—C43 | 126.8 (4) |
C18—C13—P2 | 119.5 (3) | C41—C42—Rh1 | 73.1 (2) |
C13—C14—C15 | 120.7 (4) | C43—C42—Rh1 | 108.3 (3) |
C13—C14—H14 | 119.7 | C41—C42—H42 | 113.6 |
C15—C14—H14 | 119.7 | C43—C42—H42 | 113.6 |
C16—C15—C14 | 120.0 (4) | Rh1—C42—H42 | 113.6 |
C16—C15—H15 | 120.0 | C42—C43—C44 | 113.6 (4) |
C14—C15—H15 | 120.0 | C42—C43—H43A | 108.8 |
C15—C16—C17 | 120.0 (4) | C44—C43—H43A | 108.8 |
C15—C16—H16 | 120.0 | C42—C43—H43B | 108.8 |
C17—C16—H16 | 120.0 | C44—C43—H43B | 108.8 |
C16—C17—C18 | 120.4 (4) | H43A—C43—H43B | 107.7 |
C16—C17—H17 | 119.8 | C37—C44—C43 | 112.8 (4) |
C18—C17—H17 | 119.8 | C37—C44—H44A | 109.0 |
C17—C18—C13 | 120.7 (4) | C43—C44—H44A | 109.0 |
C17—C18—H18 | 119.6 | C37—C44—H44B | 109.0 |
C13—C18—H18 | 119.6 | C43—C44—H44B | 109.0 |
C24—C19—C20 | 118.9 (4) | H44A—C44—H44B | 107.8 |
C24—C19—P2 | 119.9 (3) | F2'—B1—F3' | 111.1 (4) |
C20—C19—P2 | 121.0 (3) | F2—B1—F1 | 113.1 (4) |
C21—C20—C19 | 120.5 (4) | F2'—B1—F1 | 110.8 (4) |
C21—C20—H20 | 119.8 | F3'—B1—F1 | 109.6 (4) |
C19—C20—H20 | 119.8 | F2—B1—F3 | 110.5 (4) |
C20—C21—C22 | 120.1 (4) | F1—B1—F3 | 107.4 (4) |
C20—C21—H21 | 119.9 | F2—B1—F4 | 110.3 (4) |
C22—C21—H21 | 119.9 | F1—B1—F4 | 109.1 (4) |
C21—C22—C23 | 119.9 (4) | F3—B1—F4 | 106.1 (4) |
C21—C22—H22 | 120.1 | F2'—B1—F4' | 108.5 (4) |
C23—C22—H22 | 120.1 | F3'—B1—F4' | 108.1 (4) |
C24—C23—C22 | 120.5 (4) | F1—B1—F4' | 108.6 (4) |
C24—C23—H23 | 119.8 | Cl1—C45—Cl2 | 112.3 (4) |
C22—C23—H23 | 119.8 | Cl1—C45—H45A | 109.1 |
C23—C24—C19 | 120.2 (4) | Cl2—C45—H45A | 109.1 |
C23—C24—H24 | 119.9 | Cl1—C45—H45B | 109.1 |
C19—C24—H24 | 119.9 | Cl2—C45—H45B | 109.1 |
C30—C25—C26 | 119.6 (4) | H45A—C45—H45B | 107.9 |
{Bis[(2-diphenylphosphanyl)phenyl]
ether-
κ2P,
P'}chlorido(
η4-norbornadiene)rhodium(I) (compIII)
top
Crystal data top
[RhCl(C7H8)(C36H28OP2)] | Z = 2 |
Mr = 769.02 | F(000) = 788 |
Triclinic, P1 | Dx = 1.475 Mg m−3 |
a = 10.3662 (5) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 12.0008 (5) Å | Cell parameters from 9691 reflections |
c = 15.4693 (7) Å | θ = 2.6–31.2° |
α = 83.690 (1)° | µ = 0.70 mm−1 |
β = 89.763 (1)° | T = 150 K |
γ = 64.953 (1)° | Part of prism, orange |
V = 1730.97 (14) Å3 | 0.50 × 0.48 × 0.25 mm |
Data collection top
Bruker APEXII CCD diffractometer | 7974 independent reflections |
Radiation source: sealed tube | 7275 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.031 |
Detector resolution: 8.33 pixels mm-1 | θmax = 27.5°, θmin = 1.9° |
φ and ω scans | h = −13→13 |
Absorption correction: multi-scan (SADABS; Bruker, 2014) | k = −15→15 |
Tmin = 0.664, Tmax = 0.746 | l = −20→20 |
64995 measured reflections | |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.026 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.072 | H-atom parameters constrained |
S = 1.03 | w = 1/[σ2(Fo2) + (0.0413P)2 + 1.554P] where P = (Fo2 + 2Fc2)/3 |
7974 reflections | (Δ/σ)max = 0.003 |
433 parameters | Δρmax = 1.16 e Å−3 |
0 restraints | Δρmin = −0.70 e Å−3 |
Special details top
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Rh1 | 1.07989 (2) | 0.21759 (2) | 0.30726 (2) | 0.01270 (5) | |
Cl1 | 1.20283 (5) | 0.31386 (4) | 0.20391 (3) | 0.02132 (9) | |
P1 | 0.85872 (5) | 0.39646 (4) | 0.31868 (3) | 0.01297 (9) | |
P2 | 1.02150 (5) | 0.14945 (4) | 0.18453 (3) | 0.01324 (9) | |
O1 | 0.85019 (13) | 0.42711 (12) | 0.13561 (8) | 0.0162 (2) | |
C1 | 0.70458 (18) | 0.42145 (15) | 0.24915 (11) | 0.0147 (3) | |
C2 | 0.57564 (19) | 0.42547 (16) | 0.27923 (12) | 0.0184 (3) | |
H2 | 0.5593 | 0.4259 | 0.3397 | 0.022* | |
C3 | 0.4709 (2) | 0.42886 (17) | 0.22183 (13) | 0.0218 (4) | |
H3 | 0.3830 | 0.4326 | 0.2428 | 0.026* | |
C4 | 0.4952 (2) | 0.42670 (18) | 0.13420 (13) | 0.0235 (4) | |
H4 | 0.4248 | 0.4262 | 0.0953 | 0.028* | |
C5 | 0.6211 (2) | 0.42525 (17) | 0.10194 (12) | 0.0204 (4) | |
H5 | 0.6370 | 0.4248 | 0.0414 | 0.025* | |
C6 | 0.72331 (18) | 0.42441 (15) | 0.16025 (12) | 0.0153 (3) | |
C7 | 0.91518 (19) | 0.36680 (17) | 0.06443 (11) | 0.0162 (3) | |
C8 | 0.8974 (2) | 0.43709 (18) | −0.01502 (12) | 0.0210 (4) | |
H8 | 0.8366 | 0.5233 | −0.0215 | 0.025* | |
C9 | 0.9690 (2) | 0.3808 (2) | −0.08567 (13) | 0.0249 (4) | |
H9 | 0.9585 | 0.4284 | −0.1407 | 0.030* | |
C10 | 1.0556 (2) | 0.2553 (2) | −0.07520 (13) | 0.0254 (4) | |
H10 | 1.1046 | 0.2163 | −0.1233 | 0.030* | |
C11 | 1.0716 (2) | 0.18543 (18) | 0.00530 (12) | 0.0214 (4) | |
H11 | 1.1309 | 0.0990 | 0.0112 | 0.026* | |
C12 | 1.00251 (19) | 0.23973 (17) | 0.07759 (11) | 0.0159 (3) | |
C13 | 0.85892 (19) | 0.54987 (16) | 0.30641 (11) | 0.0154 (3) | |
C14 | 0.9844 (2) | 0.55985 (17) | 0.32501 (13) | 0.0204 (4) | |
H14 | 1.0706 | 0.4872 | 0.3383 | 0.024* | |
C15 | 0.9840 (2) | 0.67632 (19) | 0.32411 (14) | 0.0259 (4) | |
H15 | 1.0700 | 0.6827 | 0.3370 | 0.031* | |
C16 | 0.8595 (2) | 0.78228 (18) | 0.30454 (13) | 0.0237 (4) | |
H16 | 0.8596 | 0.8614 | 0.3046 | 0.028* | |
C17 | 0.7346 (2) | 0.77329 (17) | 0.28491 (13) | 0.0248 (4) | |
H17 | 0.6491 | 0.8462 | 0.2708 | 0.030* | |
C18 | 0.7341 (2) | 0.65761 (17) | 0.28574 (13) | 0.0217 (4) | |
H18 | 0.6480 | 0.6519 | 0.2721 | 0.026* | |
C19 | 0.78369 (18) | 0.39507 (16) | 0.42680 (11) | 0.0159 (3) | |
C20 | 0.7357 (2) | 0.49589 (17) | 0.47469 (12) | 0.0206 (4) | |
H20 | 0.7430 | 0.5698 | 0.4521 | 0.025* | |
C21 | 0.6775 (2) | 0.48946 (19) | 0.55510 (13) | 0.0247 (4) | |
H21 | 0.6460 | 0.5588 | 0.5871 | 0.030* | |
C22 | 0.6649 (2) | 0.38321 (19) | 0.58903 (13) | 0.0232 (4) | |
H22 | 0.6239 | 0.3796 | 0.6437 | 0.028* | |
C23 | 0.7126 (2) | 0.28231 (18) | 0.54261 (13) | 0.0237 (4) | |
H23 | 0.7044 | 0.2089 | 0.5654 | 0.028* | |
C24 | 0.7724 (2) | 0.28787 (18) | 0.46296 (13) | 0.0223 (4) | |
H24 | 0.8065 | 0.2172 | 0.4323 | 0.027* | |
C25 | 1.16252 (19) | −0.00107 (16) | 0.16620 (11) | 0.0175 (3) | |
C26 | 1.2977 (2) | −0.00762 (18) | 0.14854 (13) | 0.0226 (4) | |
H26 | 1.3131 | 0.0654 | 0.1442 | 0.027* | |
C27 | 1.4099 (2) | −0.1205 (2) | 0.13728 (14) | 0.0283 (4) | |
H27 | 1.5012 | −0.1242 | 0.1244 | 0.034* | |
C28 | 1.3884 (2) | −0.2278 (2) | 0.14481 (15) | 0.0326 (5) | |
H28 | 1.4651 | −0.3050 | 0.1374 | 0.039* | |
C29 | 1.2557 (2) | −0.22181 (19) | 0.16299 (16) | 0.0336 (5) | |
H29 | 1.2412 | −0.2953 | 0.1683 | 0.040* | |
C30 | 1.1426 (2) | −0.10908 (18) | 0.17367 (14) | 0.0249 (4) | |
H30 | 1.0514 | −0.1060 | 0.1861 | 0.030* | |
C31 | 0.86064 (18) | 0.12194 (15) | 0.18250 (12) | 0.0159 (3) | |
C32 | 0.8073 (2) | 0.10231 (18) | 0.10555 (13) | 0.0225 (4) | |
H32 | 0.8578 | 0.0981 | 0.0537 | 0.027* | |
C33 | 0.6809 (2) | 0.0890 (2) | 0.10472 (15) | 0.0283 (4) | |
H33 | 0.6456 | 0.0750 | 0.0524 | 0.034* | |
C34 | 0.6056 (2) | 0.09599 (19) | 0.17964 (15) | 0.0272 (4) | |
H34 | 0.5178 | 0.0887 | 0.1784 | 0.033* | |
C35 | 0.6587 (2) | 0.11357 (18) | 0.25642 (14) | 0.0243 (4) | |
H35 | 0.6080 | 0.1175 | 0.3081 | 0.029* | |
C36 | 0.78629 (19) | 0.12541 (16) | 0.25774 (12) | 0.0184 (3) | |
H36 | 0.8231 | 0.1360 | 0.3108 | 0.022* | |
C37 | 1.1239 (2) | 0.23985 (18) | 0.44560 (12) | 0.0215 (4) | |
H37 | 1.0744 | 0.3190 | 0.4718 | 0.026* | |
C38 | 1.2481 (2) | 0.20993 (19) | 0.40300 (13) | 0.0229 (4) | |
H38 | 1.2973 | 0.2660 | 0.3947 | 0.028* | |
C39 | 1.3283 (2) | 0.06891 (19) | 0.41552 (13) | 0.0247 (4) | |
H39 | 1.4327 | 0.0326 | 0.4053 | 0.030* | |
C40 | 1.2329 (2) | 0.03795 (17) | 0.35620 (12) | 0.0221 (4) | |
H40 | 1.2720 | −0.0315 | 0.3193 | 0.027* | |
C41 | 1.1022 (2) | 0.06786 (17) | 0.39951 (12) | 0.0214 (4) | |
H41 | 1.0436 | 0.0202 | 0.3959 | 0.026* | |
C42 | 1.1229 (2) | 0.11672 (19) | 0.48403 (12) | 0.0232 (4) | |
H42 | 1.0556 | 0.1199 | 0.5312 | 0.028* | |
C43 | 1.2834 (2) | 0.0384 (2) | 0.50660 (13) | 0.0275 (4) | |
H43A | 1.3205 | 0.0691 | 0.5530 | 0.033* | |
H43B | 1.3081 | −0.0509 | 0.5214 | 0.033* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Rh1 | 0.01421 (7) | 0.01120 (7) | 0.01362 (7) | −0.00617 (5) | −0.00184 (5) | −0.00199 (5) |
Cl1 | 0.0223 (2) | 0.0227 (2) | 0.0237 (2) | −0.01450 (18) | 0.00180 (17) | −0.00137 (17) |
P1 | 0.0148 (2) | 0.01177 (19) | 0.0132 (2) | −0.00625 (16) | 0.00007 (15) | −0.00252 (15) |
P2 | 0.0151 (2) | 0.01214 (19) | 0.0137 (2) | −0.00662 (16) | −0.00044 (15) | −0.00288 (15) |
O1 | 0.0166 (6) | 0.0187 (6) | 0.0158 (6) | −0.0094 (5) | 0.0012 (5) | −0.0040 (5) |
C1 | 0.0147 (8) | 0.0105 (7) | 0.0185 (8) | −0.0047 (6) | −0.0017 (6) | −0.0030 (6) |
C2 | 0.0170 (8) | 0.0158 (8) | 0.0221 (9) | −0.0063 (7) | 0.0018 (7) | −0.0037 (7) |
C3 | 0.0149 (8) | 0.0203 (9) | 0.0315 (10) | −0.0086 (7) | 0.0004 (7) | −0.0038 (8) |
C4 | 0.0198 (9) | 0.0221 (9) | 0.0289 (10) | −0.0091 (8) | −0.0078 (7) | −0.0031 (8) |
C5 | 0.0211 (9) | 0.0212 (9) | 0.0181 (9) | −0.0079 (7) | −0.0036 (7) | −0.0030 (7) |
C6 | 0.0141 (8) | 0.0110 (7) | 0.0195 (8) | −0.0041 (6) | −0.0004 (6) | −0.0016 (6) |
C7 | 0.0173 (8) | 0.0198 (8) | 0.0151 (8) | −0.0109 (7) | 0.0006 (6) | −0.0043 (7) |
C8 | 0.0239 (9) | 0.0215 (9) | 0.0202 (9) | −0.0126 (8) | −0.0029 (7) | 0.0001 (7) |
C9 | 0.0333 (11) | 0.0312 (10) | 0.0156 (9) | −0.0199 (9) | −0.0003 (7) | 0.0013 (7) |
C10 | 0.0315 (10) | 0.0330 (11) | 0.0164 (9) | −0.0174 (9) | 0.0054 (8) | −0.0070 (8) |
C11 | 0.0246 (9) | 0.0224 (9) | 0.0190 (9) | −0.0108 (8) | 0.0025 (7) | −0.0066 (7) |
C12 | 0.0188 (8) | 0.0192 (8) | 0.0128 (8) | −0.0110 (7) | −0.0011 (6) | −0.0016 (6) |
C13 | 0.0217 (9) | 0.0150 (8) | 0.0119 (8) | −0.0097 (7) | 0.0008 (6) | −0.0029 (6) |
C14 | 0.0205 (9) | 0.0181 (9) | 0.0239 (9) | −0.0092 (7) | −0.0007 (7) | −0.0032 (7) |
C15 | 0.0285 (10) | 0.0238 (10) | 0.0318 (11) | −0.0167 (8) | −0.0009 (8) | −0.0061 (8) |
C16 | 0.0377 (11) | 0.0174 (9) | 0.0213 (9) | −0.0159 (8) | 0.0018 (8) | −0.0051 (7) |
C17 | 0.0310 (10) | 0.0139 (8) | 0.0261 (10) | −0.0066 (8) | −0.0034 (8) | −0.0010 (7) |
C18 | 0.0224 (9) | 0.0168 (9) | 0.0255 (10) | −0.0082 (7) | −0.0040 (7) | −0.0020 (7) |
C19 | 0.0156 (8) | 0.0180 (8) | 0.0140 (8) | −0.0069 (7) | 0.0003 (6) | −0.0028 (6) |
C20 | 0.0246 (9) | 0.0185 (9) | 0.0202 (9) | −0.0100 (7) | 0.0028 (7) | −0.0049 (7) |
C21 | 0.0315 (10) | 0.0233 (9) | 0.0215 (9) | −0.0123 (8) | 0.0060 (8) | −0.0093 (7) |
C22 | 0.0243 (9) | 0.0262 (10) | 0.0173 (9) | −0.0091 (8) | 0.0048 (7) | −0.0027 (7) |
C23 | 0.0301 (10) | 0.0197 (9) | 0.0217 (9) | −0.0114 (8) | 0.0037 (8) | −0.0006 (7) |
C24 | 0.0295 (10) | 0.0175 (9) | 0.0209 (9) | −0.0105 (8) | 0.0047 (7) | −0.0052 (7) |
C25 | 0.0207 (9) | 0.0152 (8) | 0.0154 (8) | −0.0057 (7) | −0.0024 (7) | −0.0044 (6) |
C26 | 0.0197 (9) | 0.0233 (9) | 0.0252 (9) | −0.0082 (8) | −0.0005 (7) | −0.0074 (8) |
C27 | 0.0191 (9) | 0.0319 (11) | 0.0297 (11) | −0.0052 (8) | −0.0010 (8) | −0.0109 (9) |
C28 | 0.0280 (11) | 0.0224 (10) | 0.0371 (12) | 0.0013 (8) | −0.0063 (9) | −0.0114 (9) |
C29 | 0.0340 (12) | 0.0155 (9) | 0.0479 (14) | −0.0067 (9) | −0.0077 (10) | −0.0060 (9) |
C30 | 0.0235 (9) | 0.0170 (9) | 0.0332 (11) | −0.0078 (8) | −0.0029 (8) | −0.0027 (8) |
C31 | 0.0168 (8) | 0.0117 (7) | 0.0199 (8) | −0.0066 (6) | −0.0018 (6) | −0.0026 (6) |
C32 | 0.0246 (9) | 0.0246 (9) | 0.0224 (9) | −0.0130 (8) | 0.0001 (7) | −0.0082 (7) |
C33 | 0.0280 (10) | 0.0287 (10) | 0.0329 (11) | −0.0156 (9) | −0.0080 (8) | −0.0079 (9) |
C34 | 0.0194 (9) | 0.0222 (9) | 0.0439 (12) | −0.0125 (8) | −0.0029 (8) | −0.0042 (9) |
C35 | 0.0223 (9) | 0.0217 (9) | 0.0312 (10) | −0.0116 (8) | 0.0047 (8) | −0.0034 (8) |
C36 | 0.0196 (9) | 0.0160 (8) | 0.0212 (9) | −0.0089 (7) | 0.0002 (7) | −0.0025 (7) |
C37 | 0.0255 (9) | 0.0206 (9) | 0.0174 (9) | −0.0079 (8) | −0.0083 (7) | −0.0060 (7) |
C38 | 0.0240 (9) | 0.0256 (10) | 0.0225 (9) | −0.0138 (8) | −0.0095 (7) | −0.0022 (7) |
C39 | 0.0200 (9) | 0.0255 (10) | 0.0236 (10) | −0.0046 (8) | −0.0066 (7) | −0.0031 (8) |
C40 | 0.0267 (10) | 0.0149 (8) | 0.0194 (9) | −0.0038 (7) | −0.0077 (7) | −0.0013 (7) |
C41 | 0.0299 (10) | 0.0185 (9) | 0.0174 (9) | −0.0130 (8) | −0.0073 (7) | 0.0028 (7) |
C42 | 0.0283 (10) | 0.0274 (10) | 0.0150 (8) | −0.0136 (8) | −0.0038 (7) | −0.0001 (7) |
C43 | 0.0318 (11) | 0.0245 (10) | 0.0217 (10) | −0.0084 (8) | −0.0106 (8) | 0.0009 (8) |
Geometric parameters (Å, º) top
Rh1—C41 | 2.0990 (18) | C20—C21 | 1.389 (3) |
Rh1—C40 | 2.1196 (18) | C20—H20 | 0.9500 |
Rh1—C37 | 2.2575 (18) | C21—C22 | 1.383 (3) |
Rh1—C38 | 2.2576 (18) | C21—H21 | 0.9500 |
Rh1—P2 | 2.3258 (4) | C22—C23 | 1.381 (3) |
Rh1—P1 | 2.4101 (4) | C22—H22 | 0.9500 |
Rh1—Cl1 | 2.5176 (5) | C23—C24 | 1.385 (3) |
P1—C1 | 1.8270 (18) | C23—H23 | 0.9500 |
P1—C13 | 1.8309 (18) | C24—H24 | 0.9500 |
P1—C19 | 1.8430 (18) | C25—C30 | 1.389 (3) |
P2—C25 | 1.8313 (18) | C25—C26 | 1.398 (3) |
P2—C31 | 1.8329 (18) | C26—C27 | 1.390 (3) |
P2—C12 | 1.8378 (18) | C26—H26 | 0.9500 |
O1—C6 | 1.381 (2) | C27—C28 | 1.389 (3) |
O1—C7 | 1.395 (2) | C27—H27 | 0.9500 |
C1—C6 | 1.387 (2) | C28—C29 | 1.377 (3) |
C1—C2 | 1.397 (2) | C28—H28 | 0.9500 |
C2—C3 | 1.390 (3) | C29—C30 | 1.392 (3) |
C2—H2 | 0.9500 | C29—H29 | 0.9500 |
C3—C4 | 1.379 (3) | C30—H30 | 0.9500 |
C3—H3 | 0.9500 | C31—C36 | 1.388 (3) |
C4—C5 | 1.389 (3) | C31—C32 | 1.399 (3) |
C4—H4 | 0.9500 | C32—C33 | 1.385 (3) |
C5—C6 | 1.390 (2) | C32—H32 | 0.9500 |
C5—H5 | 0.9500 | C33—C34 | 1.385 (3) |
C7—C8 | 1.378 (3) | C33—H33 | 0.9500 |
C7—C12 | 1.397 (3) | C34—C35 | 1.385 (3) |
C8—C9 | 1.390 (3) | C34—H34 | 0.9500 |
C8—H8 | 0.9500 | C35—C36 | 1.389 (3) |
C9—C10 | 1.380 (3) | C35—H35 | 0.9500 |
C9—H9 | 0.9500 | C36—H36 | 0.9500 |
C10—C11 | 1.391 (3) | C37—C38 | 1.369 (3) |
C10—H10 | 0.9500 | C37—C42 | 1.535 (3) |
C11—C12 | 1.395 (3) | C37—H37 | 1.0000 |
C11—H11 | 0.9500 | C38—C39 | 1.527 (3) |
C13—C14 | 1.390 (3) | C38—H38 | 1.0000 |
C13—C18 | 1.394 (3) | C39—C40 | 1.534 (3) |
C14—C15 | 1.395 (3) | C39—C43 | 1.537 (3) |
C14—H14 | 0.9500 | C39—H39 | 1.0000 |
C15—C16 | 1.380 (3) | C40—C41 | 1.431 (3) |
C15—H15 | 0.9500 | C40—H40 | 1.0000 |
C16—C17 | 1.381 (3) | C41—C42 | 1.542 (3) |
C16—H16 | 0.9500 | C41—H41 | 1.0000 |
C17—C18 | 1.389 (3) | C42—C43 | 1.543 (3) |
C17—H17 | 0.9500 | C42—H42 | 1.0000 |
C18—H18 | 0.9500 | C43—H43A | 0.9900 |
C19—C20 | 1.394 (3) | C43—H43B | 0.9900 |
C19—C24 | 1.396 (3) | | |
| | | |
C41—Rh1—C40 | 39.65 (8) | C21—C20—H20 | 119.6 |
C41—Rh1—C37 | 65.27 (7) | C19—C20—H20 | 119.6 |
C40—Rh1—C37 | 77.18 (7) | C22—C21—C20 | 120.67 (18) |
C41—Rh1—C38 | 77.18 (7) | C22—C21—H21 | 119.7 |
C40—Rh1—C38 | 64.12 (7) | C20—C21—H21 | 119.7 |
C37—Rh1—C38 | 35.29 (7) | C23—C22—C21 | 119.30 (18) |
C41—Rh1—P2 | 98.93 (5) | C23—C22—H22 | 120.4 |
C40—Rh1—P2 | 93.07 (5) | C21—C22—H22 | 120.4 |
C37—Rh1—P2 | 163.76 (5) | C22—C23—C24 | 120.17 (18) |
C38—Rh1—P2 | 149.05 (5) | C22—C23—H23 | 119.9 |
C41—Rh1—P1 | 111.97 (6) | C24—C23—H23 | 119.9 |
C40—Rh1—P1 | 150.95 (6) | C23—C24—C19 | 121.42 (18) |
C37—Rh1—P1 | 84.19 (5) | C23—C24—H24 | 119.3 |
C38—Rh1—P1 | 110.71 (5) | C19—C24—H24 | 119.3 |
P2—Rh1—P1 | 99.300 (15) | C30—C25—C26 | 119.04 (17) |
C41—Rh1—Cl1 | 146.68 (6) | C30—C25—P2 | 122.88 (15) |
C40—Rh1—Cl1 | 107.43 (6) | C26—C25—P2 | 117.99 (14) |
C37—Rh1—Cl1 | 109.86 (5) | C27—C26—C25 | 120.31 (19) |
C38—Rh1—Cl1 | 82.40 (5) | C27—C26—H26 | 119.8 |
P2—Rh1—Cl1 | 85.314 (16) | C25—C26—H26 | 119.8 |
P1—Rh1—Cl1 | 99.737 (16) | C28—C27—C26 | 120.0 (2) |
C1—P1—C13 | 102.34 (8) | C28—C27—H27 | 120.0 |
C1—P1—C19 | 100.25 (8) | C26—C27—H27 | 120.0 |
C13—P1—C19 | 100.53 (8) | C29—C28—C27 | 119.79 (19) |
C1—P1—Rh1 | 119.00 (6) | C29—C28—H28 | 120.1 |
C13—P1—Rh1 | 118.74 (6) | C27—C28—H28 | 120.1 |
C19—P1—Rh1 | 112.93 (6) | C28—C29—C30 | 120.5 (2) |
C25—P2—C31 | 102.79 (8) | C28—C29—H29 | 119.7 |
C25—P2—C12 | 101.48 (8) | C30—C29—H29 | 119.7 |
C31—P2—C12 | 101.08 (8) | C25—C30—C29 | 120.3 (2) |
C25—P2—Rh1 | 110.32 (6) | C25—C30—H30 | 119.9 |
C31—P2—Rh1 | 119.29 (6) | C29—C30—H30 | 119.9 |
C12—P2—Rh1 | 119.31 (6) | C36—C31—C32 | 118.84 (17) |
C6—O1—C7 | 118.13 (13) | C36—C31—P2 | 119.77 (13) |
C6—C1—C2 | 118.07 (16) | C32—C31—P2 | 121.35 (14) |
C6—C1—P1 | 116.71 (13) | C33—C32—C31 | 120.15 (19) |
C2—C1—P1 | 124.90 (14) | C33—C32—H32 | 119.9 |
C3—C2—C1 | 120.84 (18) | C31—C32—H32 | 119.9 |
C3—C2—H2 | 119.6 | C34—C33—C32 | 120.52 (19) |
C1—C2—H2 | 119.6 | C34—C33—H33 | 119.7 |
C4—C3—C2 | 119.60 (17) | C32—C33—H33 | 119.7 |
C4—C3—H3 | 120.2 | C35—C34—C33 | 119.69 (18) |
C2—C3—H3 | 120.2 | C35—C34—H34 | 120.2 |
C3—C4—C5 | 120.98 (18) | C33—C34—H34 | 120.2 |
C3—C4—H4 | 119.5 | C34—C35—C36 | 119.94 (19) |
C5—C4—H4 | 119.5 | C34—C35—H35 | 120.0 |
C4—C5—C6 | 118.47 (17) | C36—C35—H35 | 120.0 |
C4—C5—H5 | 120.8 | C31—C36—C35 | 120.83 (18) |
C6—C5—H5 | 120.8 | C31—C36—H36 | 119.6 |
O1—C6—C1 | 114.34 (15) | C35—C36—H36 | 119.6 |
O1—C6—C5 | 123.69 (16) | C38—C37—C42 | 106.34 (17) |
C1—C6—C5 | 121.96 (17) | C38—C37—Rh1 | 72.36 (11) |
C8—C7—O1 | 118.21 (16) | C42—C37—Rh1 | 94.26 (11) |
C8—C7—C12 | 122.75 (17) | C38—C37—H37 | 123.4 |
O1—C7—C12 | 118.91 (15) | C42—C37—H37 | 123.4 |
C7—C8—C9 | 119.44 (18) | Rh1—C37—H37 | 123.4 |
C7—C8—H8 | 120.3 | C37—C38—C39 | 107.15 (17) |
C9—C8—H8 | 120.3 | C37—C38—Rh1 | 72.35 (11) |
C10—C9—C8 | 119.41 (18) | C39—C38—Rh1 | 95.68 (11) |
C10—C9—H9 | 120.3 | C37—C38—H38 | 122.9 |
C8—C9—H9 | 120.3 | C39—C38—H38 | 122.9 |
C9—C10—C11 | 120.46 (18) | Rh1—C38—H38 | 122.9 |
C9—C10—H10 | 119.8 | C38—C39—C40 | 98.95 (14) |
C11—C10—H10 | 119.8 | C38—C39—C43 | 100.92 (16) |
C10—C11—C12 | 121.37 (18) | C40—C39—C43 | 102.07 (17) |
C10—C11—H11 | 119.3 | C38—C39—H39 | 117.3 |
C12—C11—H11 | 119.3 | C40—C39—H39 | 117.3 |
C11—C12—C7 | 116.57 (16) | C43—C39—H39 | 117.3 |
C11—C12—P2 | 122.22 (14) | C41—C40—C39 | 105.71 (16) |
C7—C12—P2 | 121.20 (13) | C41—C40—Rh1 | 69.40 (10) |
C14—C13—C18 | 119.03 (16) | C39—C40—Rh1 | 101.22 (12) |
C14—C13—P1 | 119.09 (14) | C41—C40—H40 | 122.6 |
C18—C13—P1 | 121.67 (14) | C39—C40—H40 | 122.6 |
C13—C14—C15 | 120.08 (18) | Rh1—C40—H40 | 122.6 |
C13—C14—H14 | 120.0 | C40—C41—C42 | 105.23 (16) |
C15—C14—H14 | 120.0 | C40—C41—Rh1 | 70.95 (11) |
C16—C15—C14 | 120.35 (18) | C42—C41—Rh1 | 100.54 (12) |
C16—C15—H15 | 119.8 | C40—C41—H41 | 122.6 |
C14—C15—H15 | 119.8 | C42—C41—H41 | 122.6 |
C15—C16—C17 | 119.98 (18) | Rh1—C41—H41 | 122.6 |
C15—C16—H16 | 120.0 | C37—C42—C41 | 99.77 (14) |
C17—C16—H16 | 120.0 | C37—C42—C43 | 100.46 (16) |
C16—C17—C18 | 120.02 (18) | C41—C42—C43 | 101.80 (16) |
C16—C17—H17 | 120.0 | C37—C42—H42 | 117.3 |
C18—C17—H17 | 120.0 | C41—C42—H42 | 117.3 |
C17—C18—C13 | 120.53 (18) | C43—C42—H42 | 117.3 |
C17—C18—H18 | 119.7 | C39—C43—C42 | 93.92 (15) |
C13—C18—H18 | 119.7 | C39—C43—H43A | 112.9 |
C20—C19—C24 | 117.70 (17) | C42—C43—H43A | 112.9 |
C20—C19—P1 | 123.70 (14) | C39—C43—H43B | 112.9 |
C24—C19—P1 | 118.60 (14) | C42—C43—H43B | 112.9 |
C21—C20—C19 | 120.73 (18) | H43A—C43—H43B | 110.4 |
| | | |
C13—P1—C1—C6 | 78.46 (14) | C19—C20—C21—C22 | −0.5 (3) |
C19—P1—C1—C6 | −178.26 (13) | C20—C21—C22—C23 | 0.8 (3) |
Rh1—P1—C1—C6 | −54.69 (15) | C21—C22—C23—C24 | 0.0 (3) |
C13—P1—C1—C2 | −108.12 (16) | C22—C23—C24—C19 | −1.2 (3) |
C19—P1—C1—C2 | −4.84 (17) | C20—C19—C24—C23 | 1.6 (3) |
Rh1—P1—C1—C2 | 118.72 (14) | P1—C19—C24—C23 | −177.80 (16) |
C6—C1—C2—C3 | 1.8 (3) | C31—P2—C25—C30 | −14.58 (18) |
P1—C1—C2—C3 | −171.58 (14) | C12—P2—C25—C30 | −118.89 (17) |
C1—C2—C3—C4 | 0.8 (3) | Rh1—P2—C25—C30 | 113.67 (16) |
C2—C3—C4—C5 | −2.1 (3) | C31—P2—C25—C26 | 168.93 (15) |
C3—C4—C5—C6 | 0.8 (3) | C12—P2—C25—C26 | 64.63 (16) |
C7—O1—C6—C1 | 146.38 (15) | Rh1—P2—C25—C26 | −62.82 (15) |
C7—O1—C6—C5 | −34.0 (2) | C30—C25—C26—C27 | 1.0 (3) |
C2—C1—C6—O1 | 176.54 (15) | P2—C25—C26—C27 | 177.64 (15) |
P1—C1—C6—O1 | −9.57 (19) | C25—C26—C27—C28 | −0.9 (3) |
C2—C1—C6—C5 | −3.1 (3) | C26—C27—C28—C29 | 0.3 (3) |
P1—C1—C6—C5 | 170.78 (14) | C27—C28—C29—C30 | 0.2 (4) |
C4—C5—C6—O1 | −177.76 (16) | C26—C25—C30—C29 | −0.5 (3) |
C4—C5—C6—C1 | 1.9 (3) | P2—C25—C30—C29 | −176.95 (17) |
C6—O1—C7—C8 | 99.74 (19) | C28—C29—C30—C25 | −0.1 (3) |
C6—O1—C7—C12 | −84.3 (2) | C25—P2—C31—C36 | 113.61 (15) |
O1—C7—C8—C9 | 175.47 (16) | C12—P2—C31—C36 | −141.77 (14) |
C12—C7—C8—C9 | −0.3 (3) | Rh1—P2—C31—C36 | −8.78 (17) |
C7—C8—C9—C10 | 0.7 (3) | C25—P2—C31—C32 | −69.01 (16) |
C8—C9—C10—C11 | −0.2 (3) | C12—P2—C31—C32 | 35.61 (17) |
C9—C10—C11—C12 | −0.6 (3) | Rh1—P2—C31—C32 | 168.59 (13) |
C10—C11—C12—C7 | 1.0 (3) | C36—C31—C32—C33 | 1.2 (3) |
C10—C11—C12—P2 | 179.81 (15) | P2—C31—C32—C33 | −176.19 (15) |
C8—C7—C12—C11 | −0.5 (3) | C31—C32—C33—C34 | 0.5 (3) |
O1—C7—C12—C11 | −176.28 (15) | C32—C33—C34—C35 | −1.5 (3) |
C8—C7—C12—P2 | −179.34 (14) | C33—C34—C35—C36 | 0.7 (3) |
O1—C7—C12—P2 | 4.9 (2) | C32—C31—C36—C35 | −2.0 (3) |
C25—P2—C12—C11 | 8.30 (17) | P2—C31—C36—C35 | 175.42 (14) |
C31—P2—C12—C11 | −97.37 (16) | C34—C35—C36—C31 | 1.1 (3) |
Rh1—P2—C12—C11 | 129.66 (14) | C42—C37—C38—C39 | −1.29 (19) |
C25—P2—C12—C7 | −172.93 (15) | Rh1—C37—C38—C39 | −90.60 (13) |
C31—P2—C12—C7 | 81.41 (15) | C42—C37—C38—Rh1 | 89.31 (12) |
Rh1—P2—C12—C7 | −51.57 (16) | C37—C38—C39—C40 | 71.69 (18) |
C1—P1—C13—C14 | −158.47 (15) | Rh1—C38—C39—C40 | −1.56 (15) |
C19—P1—C13—C14 | 98.47 (15) | C37—C38—C39—C43 | −32.55 (19) |
Rh1—P1—C13—C14 | −25.16 (17) | Rh1—C38—C39—C43 | −105.80 (13) |
C1—P1—C13—C18 | 26.79 (17) | C38—C39—C40—C41 | −69.84 (18) |
C19—P1—C13—C18 | −76.27 (16) | C43—C39—C40—C41 | 33.44 (19) |
Rh1—P1—C13—C18 | 160.10 (13) | C38—C39—C40—Rh1 | 1.69 (16) |
C18—C13—C14—C15 | 0.9 (3) | C43—C39—C40—Rh1 | 104.97 (14) |
P1—C13—C14—C15 | −173.94 (15) | C39—C40—C41—C42 | 0.20 (19) |
C13—C14—C15—C16 | −0.2 (3) | Rh1—C40—C41—C42 | −96.12 (13) |
C14—C15—C16—C17 | −0.6 (3) | C39—C40—C41—Rh1 | 96.33 (13) |
C15—C16—C17—C18 | 0.7 (3) | C38—C37—C42—C41 | −69.55 (18) |
C16—C17—C18—C13 | 0.1 (3) | Rh1—C37—C42—C41 | 3.30 (14) |
C14—C13—C18—C17 | −0.9 (3) | C38—C37—C42—C43 | 34.50 (19) |
P1—C13—C18—C17 | 173.85 (15) | Rh1—C37—C42—C43 | 107.35 (13) |
C1—P1—C19—C20 | −100.80 (16) | C40—C41—C42—C37 | 69.34 (18) |
C13—P1—C19—C20 | 3.94 (17) | Rh1—C41—C42—C37 | −3.60 (15) |
Rh1—P1—C19—C20 | 131.50 (15) | C40—C41—C42—C43 | −33.61 (19) |
C1—P1—C19—C24 | 78.50 (16) | Rh1—C41—C42—C43 | −106.55 (14) |
C13—P1—C19—C24 | −176.75 (15) | C38—C39—C43—C42 | 50.49 (17) |
Rh1—P1—C19—C24 | −49.19 (16) | C40—C39—C43—C42 | −51.25 (17) |
C24—C19—C20—C21 | −0.7 (3) | C37—C42—C43—C39 | −51.14 (17) |
P1—C19—C20—C21 | 178.63 (15) | C41—C42—C43—C39 | 51.27 (17) |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
C26—H26···Cl1 | 0.95 | 2.96 | 3.754 (2) | 142 |