A hydroxy phosphonite was found to be unstable during the catalyst preformation routine applied towards a rhodium olefin hydroformylation catalyst. C—P bond cleavage occurred when the phosphonite was reacted with [(acac)Rh(1,5-COD)] (acac is acetyl acetate and 1,5-COD is cycloocta-1,5-diene) at 80 °C and 20 bar of CO/H2. As a result, a nearly planar six-membered ring structure consisting of two rhodium(I) cations and two bridging phosphorous acid diester anions was formed, namely bis[μ-(4,8-di-tert-butyl-2,10-dimethoxydibenzo[d,f][1,3,2]dioxaphosphepin-6-yl)oxy]-1:2κ2P:O;1:2κ2O:P-bis{[6-([1,1′-biphenyl]-2-yloxy)-4,8-di-tert-butyl-2,10-dimethoxydibenzo[d,f][1,3,2]dioxaphosphepine-κP]carbonylrhodium(I)} toluene tetrasolvate, [Rh2(C22H28O5P)2(C34H37O5P)2(CO)2]·4C7H8. Further coordination of phosphite and of carbonyl groups resulted in 16-electron rhodium centres.
Supporting information
CCDC reference: 1898827
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: XP in SHELXTL (Sheldrick, 2008).
Bis[µ-(4,8-di-
tert-butyl-2,10-dimethoxydibenzo[
d,
f]\
[1,3,2]dioxaphosphepin-6-yl)oxy]-1:2
κ2P:\
O;\
1:2
κ2O:
P-bis{[6-([1,1'-biphenyl]-2-yloxy)-4,8-di-
tert-\
butyl-2,10-dimethoxydibenzo[
d,
f][1,3,2]dioxaphosphepine-\
κP]carbonylrhodium} toluene tatrasolvate
top
Crystal data top
[Rh2(C22H28O5P)2(C34H37O5P)2(CO)2]·4C7H8 | F(000) = 2680 |
Mr = 2550.41 | Dx = 1.319 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
a = 13.4100 (5) Å | Cell parameters from 9938 reflections |
b = 15.5455 (5) Å | θ = 2.3–30.3° |
c = 31.1570 (11) Å | µ = 0.38 mm−1 |
β = 98.7430 (14)° | T = 150 K |
V = 6419.7 (4) Å3 | Prism, yellow |
Z = 2 | 0.41 × 0.34 × 0.32 mm |
Data collection top
Bruker APEXII CCD diffractometer | 15481 independent reflections |
Radiation source: fine-focus sealed tube | 13358 reflections with I > 2σ(I) |
Detector resolution: 8.3333 pixels mm-1 | Rint = 0.040 |
φ and ω scans | θmax = 28.0°, θmin = 1.6° |
Absorption correction: multi-scan (SADABS; Bruker, 2014) | h = −17→17 |
Tmin = 0.86, Tmax = 0.89 | k = −20→20 |
140325 measured reflections | l = −41→41 |
Refinement top
Refinement on F2 | 0 restraints |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.035 | H-atom parameters constrained |
wR(F2) = 0.093 | w = 1/[σ2(Fo2) + (0.0453P)2 + 5.3591P] where P = (Fo2 + 2Fc2)/3 |
S = 1.03 | (Δ/σ)max = 0.001 |
15481 reflections | Δρmax = 0.81 e Å−3 |
760 parameters | Δρmin = −0.39 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 | |
C1 | −0.05877 (14) | 1.10380 (12) | 0.15205 (6) | 0.0222 (3) | |
C2 | 0.00322 (15) | 1.14899 (13) | 0.12855 (6) | 0.0274 (4) | |
H2 | 0.0414 | 1.1195 | 0.1098 | 0.033* | |
C3 | 0.00930 (18) | 1.23754 (14) | 0.13250 (7) | 0.0342 (5) | |
H3 | 0.0526 | 1.2690 | 0.1167 | 0.041* | |
C4 | −0.04732 (19) | 1.28050 (14) | 0.15927 (7) | 0.0387 (5) | |
H4 | −0.0437 | 1.3414 | 0.1618 | 0.046* | |
C5 | −0.10935 (17) | 1.23413 (13) | 0.18239 (7) | 0.0343 (5) | |
H5 | −0.1486 | 1.2640 | 0.2005 | 0.041* | |
C6 | −0.11587 (14) | 1.14461 (12) | 0.17978 (6) | 0.0255 (4) | |
C7 | −0.17942 (15) | 1.09749 (13) | 0.20697 (6) | 0.0273 (4) | |
C8 | −0.28188 (16) | 1.11705 (15) | 0.20360 (7) | 0.0346 (5) | |
H8 | −0.3115 | 1.1573 | 0.1825 | 0.042* | |
C9 | −0.34058 (17) | 1.07785 (17) | 0.23096 (8) | 0.0427 (6) | |
H9 | −0.4104 | 1.0913 | 0.2284 | 0.051* | |
C10 | −0.29892 (18) | 1.01997 (17) | 0.26169 (8) | 0.0435 (6) | |
H10 | −0.3397 | 0.9937 | 0.2804 | 0.052* | |
C11 | −0.19711 (18) | 0.99962 (15) | 0.26553 (8) | 0.0390 (5) | |
H11 | −0.1681 | 0.9597 | 0.2869 | 0.047* | |
C12 | −0.13792 (16) | 1.03784 (14) | 0.23793 (7) | 0.0307 (4) | |
H12 | −0.0686 | 1.0231 | 0.2402 | 0.037* | |
C13 | −0.03331 (13) | 0.84098 (11) | 0.19468 (5) | 0.0199 (3) | |
C14 | −0.12566 (14) | 0.81619 (12) | 0.20717 (6) | 0.0227 (4) | |
C15 | −0.12299 (14) | 0.79805 (13) | 0.25087 (6) | 0.0263 (4) | |
H15 | −0.1840 | 0.7824 | 0.2609 | 0.032* | |
C16 | −0.03476 (15) | 0.80181 (13) | 0.28062 (6) | 0.0258 (4) | |
C17 | 0.05601 (14) | 0.81946 (12) | 0.26674 (6) | 0.0240 (4) | |
H17 | 0.1171 | 0.8184 | 0.2867 | 0.029* | |
C18 | 0.05714 (13) | 0.83903 (11) | 0.22290 (6) | 0.0208 (3) | |
C19 | 0.15755 (13) | 0.84937 (12) | 0.20853 (5) | 0.0212 (3) | |
C20 | 0.23197 (14) | 0.78886 (13) | 0.22332 (6) | 0.0252 (4) | |
H20 | 0.2171 | 0.7417 | 0.2407 | 0.030* | |
C21 | 0.32743 (15) | 0.79833 (14) | 0.21237 (6) | 0.0288 (4) | |
C22 | 0.35060 (14) | 0.87008 (14) | 0.18910 (6) | 0.0285 (4) | |
H22 | 0.4176 | 0.8766 | 0.1832 | 0.034* | |
C23 | 0.28013 (14) | 0.93226 (12) | 0.17423 (6) | 0.0242 (4) | |
C24 | 0.18141 (13) | 0.91769 (12) | 0.18293 (6) | 0.0208 (3) | |
C25 | −0.22374 (14) | 0.80187 (13) | 0.17502 (6) | 0.0259 (4) | |
C26 | −0.20636 (17) | 0.72748 (15) | 0.14487 (8) | 0.0385 (5) | |
H26A | −0.2689 | 0.7156 | 0.1251 | 0.058* | |
H26B | −0.1860 | 0.6761 | 0.1622 | 0.058* | |
H26C | −0.1530 | 0.7431 | 0.1280 | 0.058* | |
C27 | −0.25697 (16) | 0.88192 (14) | 0.14816 (7) | 0.0340 (5) | |
H27A | −0.2625 | 0.9306 | 0.1676 | 0.051* | |
H27B | −0.3226 | 0.8712 | 0.1304 | 0.051* | |
H27C | −0.2071 | 0.8952 | 0.1292 | 0.051* | |
C28 | −0.31157 (16) | 0.77680 (18) | 0.19899 (7) | 0.0414 (6) | |
H28A | −0.3218 | 0.8221 | 0.2198 | 0.062* | |
H28B | −0.2957 | 0.7225 | 0.2145 | 0.062* | |
H28C | −0.3732 | 0.7698 | 0.1779 | 0.062* | |
C29 | 0.03783 (16) | 0.79999 (15) | 0.35515 (6) | 0.0334 (5) | |
H29A | 0.0934 | 0.7618 | 0.3506 | 0.050* | |
H29B | 0.0190 | 0.7890 | 0.3838 | 0.050* | |
H29C | 0.0593 | 0.8600 | 0.3534 | 0.050* | |
C30 | 0.38639 (18) | 0.67199 (17) | 0.25083 (9) | 0.0474 (6) | |
H30A | 0.3739 | 0.6951 | 0.2788 | 0.071* | |
H30B | 0.4455 | 0.6341 | 0.2555 | 0.071* | |
H30C | 0.3273 | 0.6393 | 0.2374 | 0.071* | |
C31 | 0.31189 (15) | 1.01366 (14) | 0.15168 (7) | 0.0305 (4) | |
C32 | 0.26525 (17) | 1.01554 (16) | 0.10375 (7) | 0.0386 (5) | |
H32A | 0.1917 | 1.0199 | 0.1013 | 0.058* | |
H32B | 0.2829 | 0.9626 | 0.0896 | 0.058* | |
H32C | 0.2913 | 1.0653 | 0.0896 | 0.058* | |
C33 | 0.28132 (19) | 1.09348 (15) | 0.17499 (8) | 0.0433 (6) | |
H33A | 0.3148 | 1.0929 | 0.2052 | 0.065* | |
H33B | 0.2080 | 1.0937 | 0.1743 | 0.065* | |
H33C | 0.3016 | 1.1451 | 0.1605 | 0.065* | |
C34 | 0.42695 (17) | 1.01700 (18) | 0.15328 (9) | 0.0468 (6) | |
H34A | 0.4459 | 1.0720 | 0.1414 | 0.070* | |
H34B | 0.4484 | 0.9697 | 0.1360 | 0.070* | |
H34C | 0.4600 | 1.0114 | 0.1834 | 0.070* | |
C35 | −0.01994 (13) | 0.74019 (11) | −0.00710 (5) | 0.0190 (3) | |
C36 | −0.10642 (13) | 0.71434 (11) | 0.01005 (6) | 0.0211 (3) | |
C37 | −0.09665 (14) | 0.64049 (12) | 0.03547 (6) | 0.0242 (4) | |
H37 | −0.1521 | 0.6226 | 0.0490 | 0.029* | |
C38 | −0.00846 (15) | 0.59184 (12) | 0.04181 (6) | 0.0234 (4) | |
C39 | 0.07087 (14) | 0.61313 (11) | 0.02026 (6) | 0.0216 (3) | |
H39 | 0.1287 | 0.5772 | 0.0224 | 0.026* | |
C40 | 0.06490 (13) | 0.68827 (11) | −0.00473 (6) | 0.0191 (3) | |
C41 | 0.14602 (13) | 0.70671 (11) | −0.03120 (6) | 0.0195 (3) | |
C42 | 0.17301 (14) | 0.64030 (11) | −0.05760 (6) | 0.0222 (3) | |
H42 | 0.1406 | 0.5859 | −0.0581 | 0.027* | |
C43 | 0.24729 (14) | 0.65520 (12) | −0.08274 (6) | 0.0243 (4) | |
C44 | 0.29977 (14) | 0.73246 (12) | −0.07929 (6) | 0.0243 (4) | |
H44 | 0.3529 | 0.7402 | −0.0959 | 0.029* | |
C45 | 0.27748 (13) | 0.79902 (11) | −0.05244 (6) | 0.0202 (3) | |
C46 | 0.19454 (13) | 0.78558 (11) | −0.03043 (5) | 0.0186 (3) | |
C47 | −0.20971 (14) | 0.75849 (13) | −0.00268 (6) | 0.0255 (4) | |
C48 | −0.23840 (16) | 0.75233 (15) | −0.05224 (7) | 0.0329 (4) | |
H48A | −0.3043 | 0.7795 | −0.0611 | 0.049* | |
H48B | −0.2418 | 0.6917 | −0.0610 | 0.049* | |
H48C | −0.1874 | 0.7819 | −0.0663 | 0.049* | |
C49 | −0.20901 (16) | 0.85279 (14) | 0.01137 (8) | 0.0351 (5) | |
H49A | −0.1854 | 0.8568 | 0.0426 | 0.053* | |
H49B | −0.2774 | 0.8763 | 0.0048 | 0.053* | |
H49C | −0.1638 | 0.8856 | −0.0044 | 0.053* | |
C50 | −0.29270 (16) | 0.71236 (17) | 0.01750 (8) | 0.0392 (5) | |
H50A | −0.2764 | 0.7144 | 0.0492 | 0.059* | |
H50B | −0.2971 | 0.6523 | 0.0079 | 0.059* | |
H50C | −0.3575 | 0.7410 | 0.0083 | 0.059* | |
C51 | 0.07793 (17) | 0.46875 (13) | 0.07478 (7) | 0.0328 (4) | |
H51A | 0.0858 | 0.4419 | 0.0470 | 0.049* | |
H51B | 0.0699 | 0.4239 | 0.0961 | 0.049* | |
H51C | 0.1379 | 0.5033 | 0.0852 | 0.049* | |
C52 | 0.22870 (18) | 0.51538 (14) | −0.11391 (8) | 0.0390 (5) | |
H52A | 0.2455 | 0.4870 | −0.0857 | 0.059* | |
H52B | 0.2532 | 0.4804 | −0.1363 | 0.059* | |
H52C | 0.1553 | 0.5219 | −0.1209 | 0.059* | |
C53 | 0.34312 (14) | 0.88047 (12) | −0.04674 (6) | 0.0244 (4) | |
C54 | 0.43790 (16) | 0.87090 (14) | −0.06847 (8) | 0.0349 (5) | |
H54A | 0.4765 | 0.8206 | −0.0565 | 0.052* | |
H54B | 0.4797 | 0.9226 | −0.0630 | 0.052* | |
H54C | 0.4180 | 0.8634 | −0.0998 | 0.052* | |
C55 | 0.28377 (16) | 0.95709 (13) | −0.06802 (8) | 0.0367 (5) | |
H55A | 0.2640 | 0.9457 | −0.0991 | 0.055* | |
H55B | 0.3260 | 1.0088 | −0.0642 | 0.055* | |
H55C | 0.2232 | 0.9659 | −0.0545 | 0.055* | |
C56 | 0.37997 (18) | 0.89737 (17) | 0.00145 (7) | 0.0413 (5) | |
H56A | 0.3218 | 0.9059 | 0.0166 | 0.062* | |
H56B | 0.4223 | 0.9490 | 0.0046 | 0.062* | |
H56C | 0.4194 | 0.8480 | 0.0141 | 0.062* | |
C57 | 0.10115 (15) | 0.83262 (12) | 0.08053 (6) | 0.0259 (4) | |
C58 | 0.43179 (16) | 0.65168 (12) | 0.08541 (7) | 0.0611 (8) | |
C59 | 0.50365 (15) | 0.59332 (16) | 0.10454 (7) | 0.0776 (11) | |
H59 | 0.5499 | 0.6096 | 0.1294 | 0.093* | |
C60 | 0.50780 (16) | 0.51116 (14) | 0.08730 (9) | 0.0863 (12) | |
H60 | 0.5569 | 0.4713 | 0.1004 | 0.104* | |
C61 | 0.4401 (2) | 0.48734 (13) | 0.05094 (10) | 0.0995 (14) | |
H61 | 0.4429 | 0.4312 | 0.0392 | 0.119* | |
C62 | 0.3682 (2) | 0.54570 (17) | 0.03182 (8) | 0.1091 (16) | |
H62 | 0.3219 | 0.5294 | 0.0070 | 0.131* | |
C63 | 0.36407 (16) | 0.62787 (15) | 0.04905 (7) | 0.0756 (10) | |
H63 | 0.3150 | 0.6678 | 0.0360 | 0.091* | |
C64 | 0.4267 (3) | 0.7386 (3) | 0.10370 (13) | 0.0878 (11) | |
H64A | 0.4834 | 0.7730 | 0.0968 | 0.132* | |
H64B | 0.4302 | 0.7346 | 0.1353 | 0.132* | |
H64C | 0.3630 | 0.7659 | 0.0912 | 0.132* | |
C65 | 0.21479 (11) | 0.53242 (11) | 0.17671 (5) | 0.0518 (7) | |
C66 | 0.17226 (11) | 0.60699 (10) | 0.15723 (5) | 0.0410 (5) | |
H66 | 0.2077 | 0.6395 | 0.1386 | 0.049* | |
C67 | 0.07787 (11) | 0.63405 (9) | 0.16505 (5) | 0.0401 (5) | |
H67 | 0.0488 | 0.6850 | 0.1517 | 0.048* | |
C68 | 0.02601 (10) | 0.58654 (12) | 0.19234 (6) | 0.0534 (7) | |
H68 | −0.0385 | 0.6050 | 0.1977 | 0.064* | |
C69 | 0.06854 (13) | 0.51197 (11) | 0.21182 (6) | 0.0584 (7) | |
H69 | 0.0331 | 0.4795 | 0.2305 | 0.070* | |
C70 | 0.16293 (14) | 0.48491 (9) | 0.20400 (5) | 0.0539 (7) | |
H70 | 0.1920 | 0.4339 | 0.2173 | 0.065* | |
C71 | 0.3155 (3) | 0.5033 (3) | 0.16757 (13) | 0.1101 (18) | |
H71A | 0.3065 | 0.4573 | 0.1458 | 0.165* | |
H71B | 0.3554 | 0.4818 | 0.1944 | 0.165* | |
H71C | 0.3507 | 0.5518 | 0.1565 | 0.165* | |
O1 | −0.07102 (9) | 1.01463 (8) | 0.14786 (4) | 0.0223 (3) | |
O2 | −0.02939 (9) | 0.85920 (8) | 0.15060 (4) | 0.0199 (2) | |
O3 | 0.10367 (9) | 0.97617 (8) | 0.16894 (4) | 0.0214 (3) | |
O4 | −0.04594 (11) | 0.78438 (11) | 0.32282 (4) | 0.0363 (4) | |
O5 | 0.40458 (11) | 0.74111 (11) | 0.22297 (5) | 0.0396 (4) | |
O6 | −0.01933 (9) | 0.81766 (7) | −0.02991 (4) | 0.0185 (2) | |
O7 | 0.16567 (9) | 0.84936 (8) | −0.00312 (4) | 0.0191 (2) | |
O8 | 0.04755 (9) | 0.96021 (8) | −0.04265 (4) | 0.0205 (2) | |
O9 | −0.00905 (11) | 0.52279 (9) | 0.06893 (4) | 0.0284 (3) | |
O10 | 0.27510 (11) | 0.59780 (9) | −0.11224 (5) | 0.0327 (3) | |
O11 | 0.14861 (13) | 0.77373 (10) | 0.09226 (5) | 0.0397 (4) | |
P1 | 0.00872 (3) | 0.94829 (3) | 0.13333 (2) | 0.01749 (9) | |
P2 | 0.05519 (3) | 0.89371 (3) | −0.00705 (2) | 0.01635 (9) | |
Rh1 | 0.03018 (2) | 0.92806 (2) | 0.06248 (2) | 0.01662 (4) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
C1 | 0.0273 (9) | 0.0181 (8) | 0.0207 (8) | 0.0008 (7) | 0.0012 (7) | −0.0029 (7) |
C2 | 0.0380 (10) | 0.0240 (9) | 0.0208 (9) | 0.0007 (8) | 0.0062 (8) | −0.0004 (7) |
C3 | 0.0498 (13) | 0.0260 (10) | 0.0276 (10) | −0.0036 (9) | 0.0083 (9) | 0.0021 (8) |
C4 | 0.0599 (14) | 0.0191 (10) | 0.0373 (12) | 0.0044 (9) | 0.0083 (10) | −0.0023 (8) |
C5 | 0.0452 (12) | 0.0241 (10) | 0.0346 (11) | 0.0081 (9) | 0.0091 (9) | −0.0073 (8) |
C6 | 0.0290 (9) | 0.0238 (9) | 0.0234 (9) | 0.0042 (7) | 0.0026 (7) | −0.0028 (7) |
C7 | 0.0282 (9) | 0.0276 (10) | 0.0268 (9) | 0.0005 (8) | 0.0066 (7) | −0.0116 (8) |
C8 | 0.0303 (10) | 0.0392 (12) | 0.0338 (11) | 0.0049 (9) | 0.0029 (8) | −0.0140 (9) |
C9 | 0.0275 (10) | 0.0544 (15) | 0.0485 (14) | −0.0058 (10) | 0.0129 (10) | −0.0218 (12) |
C10 | 0.0444 (13) | 0.0458 (14) | 0.0459 (13) | −0.0115 (11) | 0.0255 (11) | −0.0144 (11) |
C11 | 0.0495 (13) | 0.0340 (12) | 0.0373 (12) | −0.0015 (10) | 0.0187 (10) | −0.0034 (9) |
C12 | 0.0311 (10) | 0.0297 (10) | 0.0330 (10) | 0.0026 (8) | 0.0105 (8) | −0.0034 (8) |
C13 | 0.0281 (9) | 0.0167 (8) | 0.0160 (8) | −0.0020 (7) | 0.0071 (6) | 0.0013 (6) |
C14 | 0.0258 (9) | 0.0206 (9) | 0.0222 (9) | −0.0035 (7) | 0.0053 (7) | 0.0025 (7) |
C15 | 0.0264 (9) | 0.0292 (10) | 0.0248 (9) | −0.0061 (8) | 0.0092 (7) | 0.0034 (8) |
C16 | 0.0320 (10) | 0.0284 (10) | 0.0180 (8) | −0.0057 (8) | 0.0070 (7) | 0.0036 (7) |
C17 | 0.0257 (9) | 0.0264 (9) | 0.0195 (8) | −0.0039 (7) | 0.0025 (7) | 0.0033 (7) |
C18 | 0.0252 (8) | 0.0187 (8) | 0.0195 (8) | −0.0033 (7) | 0.0066 (7) | 0.0012 (7) |
C19 | 0.0232 (8) | 0.0244 (9) | 0.0163 (8) | −0.0026 (7) | 0.0036 (6) | −0.0014 (7) |
C20 | 0.0276 (9) | 0.0273 (9) | 0.0206 (8) | 0.0003 (7) | 0.0033 (7) | 0.0025 (7) |
C21 | 0.0272 (9) | 0.0338 (11) | 0.0251 (9) | 0.0054 (8) | 0.0025 (7) | 0.0011 (8) |
C22 | 0.0213 (9) | 0.0395 (11) | 0.0257 (9) | −0.0033 (8) | 0.0069 (7) | −0.0007 (8) |
C23 | 0.0258 (9) | 0.0291 (10) | 0.0187 (8) | −0.0063 (7) | 0.0062 (7) | −0.0009 (7) |
C24 | 0.0227 (8) | 0.0220 (9) | 0.0175 (8) | −0.0011 (7) | 0.0028 (6) | −0.0011 (7) |
C25 | 0.0254 (9) | 0.0280 (10) | 0.0238 (9) | −0.0067 (7) | 0.0018 (7) | 0.0053 (7) |
C26 | 0.0386 (12) | 0.0345 (12) | 0.0396 (12) | −0.0088 (9) | −0.0032 (9) | −0.0058 (9) |
C27 | 0.0287 (10) | 0.0338 (11) | 0.0369 (11) | −0.0045 (8) | −0.0032 (8) | 0.0086 (9) |
C28 | 0.0277 (10) | 0.0620 (16) | 0.0335 (11) | −0.0138 (10) | 0.0012 (9) | 0.0134 (11) |
C29 | 0.0370 (11) | 0.0451 (13) | 0.0188 (9) | −0.0089 (9) | 0.0061 (8) | 0.0027 (8) |
C30 | 0.0368 (12) | 0.0439 (14) | 0.0575 (16) | 0.0082 (10) | −0.0053 (11) | 0.0154 (12) |
C31 | 0.0298 (10) | 0.0332 (11) | 0.0300 (10) | −0.0110 (8) | 0.0091 (8) | 0.0032 (8) |
C32 | 0.0410 (12) | 0.0448 (13) | 0.0311 (11) | −0.0114 (10) | 0.0087 (9) | 0.0110 (10) |
C33 | 0.0486 (14) | 0.0325 (12) | 0.0502 (14) | −0.0162 (10) | 0.0124 (11) | −0.0044 (10) |
C34 | 0.0347 (12) | 0.0576 (16) | 0.0491 (14) | −0.0167 (11) | 0.0098 (10) | 0.0127 (12) |
C35 | 0.0253 (8) | 0.0135 (8) | 0.0185 (8) | −0.0005 (6) | 0.0042 (6) | 0.0002 (6) |
C36 | 0.0237 (8) | 0.0192 (8) | 0.0214 (8) | −0.0022 (7) | 0.0070 (7) | −0.0036 (7) |
C37 | 0.0278 (9) | 0.0226 (9) | 0.0240 (9) | −0.0052 (7) | 0.0097 (7) | −0.0008 (7) |
C38 | 0.0336 (10) | 0.0170 (8) | 0.0202 (8) | −0.0058 (7) | 0.0065 (7) | 0.0000 (7) |
C39 | 0.0267 (9) | 0.0167 (8) | 0.0224 (8) | 0.0005 (7) | 0.0069 (7) | −0.0009 (7) |
C40 | 0.0229 (8) | 0.0155 (8) | 0.0199 (8) | −0.0021 (6) | 0.0069 (6) | −0.0013 (6) |
C41 | 0.0224 (8) | 0.0172 (8) | 0.0202 (8) | 0.0032 (6) | 0.0076 (6) | 0.0020 (6) |
C42 | 0.0253 (9) | 0.0159 (8) | 0.0264 (9) | 0.0021 (7) | 0.0074 (7) | −0.0008 (7) |
C43 | 0.0262 (9) | 0.0213 (9) | 0.0273 (9) | 0.0046 (7) | 0.0099 (7) | −0.0037 (7) |
C44 | 0.0245 (9) | 0.0229 (9) | 0.0281 (9) | 0.0018 (7) | 0.0120 (7) | −0.0004 (7) |
C45 | 0.0212 (8) | 0.0178 (8) | 0.0224 (8) | 0.0016 (6) | 0.0059 (7) | 0.0023 (7) |
C46 | 0.0216 (8) | 0.0156 (8) | 0.0193 (8) | 0.0047 (6) | 0.0054 (6) | 0.0002 (6) |
C47 | 0.0204 (8) | 0.0285 (10) | 0.0284 (9) | −0.0004 (7) | 0.0065 (7) | −0.0022 (8) |
C48 | 0.0305 (10) | 0.0367 (11) | 0.0304 (10) | 0.0013 (9) | 0.0012 (8) | −0.0026 (9) |
C49 | 0.0263 (10) | 0.0329 (11) | 0.0461 (12) | 0.0057 (8) | 0.0054 (9) | −0.0110 (9) |
C50 | 0.0246 (10) | 0.0507 (14) | 0.0440 (13) | −0.0022 (9) | 0.0106 (9) | 0.0073 (11) |
C51 | 0.0443 (12) | 0.0215 (9) | 0.0314 (10) | −0.0001 (8) | 0.0025 (9) | 0.0083 (8) |
C52 | 0.0471 (13) | 0.0257 (10) | 0.0499 (13) | −0.0056 (9) | 0.0254 (11) | −0.0156 (10) |
C53 | 0.0239 (9) | 0.0216 (9) | 0.0298 (9) | −0.0032 (7) | 0.0109 (7) | −0.0015 (7) |
C54 | 0.0293 (10) | 0.0316 (11) | 0.0478 (13) | −0.0071 (8) | 0.0192 (9) | −0.0056 (9) |
C55 | 0.0340 (11) | 0.0213 (10) | 0.0574 (14) | −0.0013 (8) | 0.0148 (10) | 0.0071 (9) |
C56 | 0.0382 (12) | 0.0527 (14) | 0.0340 (11) | −0.0191 (11) | 0.0092 (9) | −0.0092 (10) |
C57 | 0.0363 (10) | 0.0252 (9) | 0.0173 (8) | 0.0042 (8) | 0.0074 (7) | 0.0004 (7) |
C58 | 0.0578 (17) | 0.0594 (18) | 0.0649 (19) | −0.0025 (14) | 0.0058 (14) | 0.0092 (15) |
C59 | 0.0421 (16) | 0.085 (3) | 0.098 (3) | −0.0023 (16) | −0.0126 (16) | 0.024 (2) |
C60 | 0.0446 (17) | 0.073 (2) | 0.139 (4) | 0.0028 (16) | 0.007 (2) | 0.028 (2) |
C61 | 0.076 (3) | 0.097 (3) | 0.121 (4) | 0.009 (2) | 0.001 (2) | −0.003 (3) |
C62 | 0.105 (3) | 0.100 (3) | 0.109 (4) | 0.020 (3) | −0.028 (3) | −0.014 (3) |
C63 | 0.065 (2) | 0.081 (2) | 0.072 (2) | 0.0034 (18) | −0.0186 (17) | 0.0108 (19) |
C64 | 0.093 (3) | 0.085 (3) | 0.082 (3) | 0.014 (2) | 0.001 (2) | −0.009 (2) |
C65 | 0.0674 (17) | 0.0544 (16) | 0.0352 (12) | 0.0279 (14) | 0.0124 (12) | 0.0054 (11) |
C66 | 0.0507 (14) | 0.0354 (12) | 0.0384 (12) | 0.0080 (10) | 0.0117 (10) | 0.0022 (10) |
C67 | 0.0465 (13) | 0.0317 (11) | 0.0418 (12) | 0.0024 (10) | 0.0055 (10) | −0.0007 (10) |
C68 | 0.0394 (13) | 0.0693 (19) | 0.0519 (15) | 0.0016 (13) | 0.0081 (11) | 0.0142 (14) |
C69 | 0.0558 (16) | 0.070 (2) | 0.0484 (15) | −0.0059 (14) | 0.0047 (13) | 0.0232 (14) |
C70 | 0.0779 (19) | 0.0463 (15) | 0.0354 (13) | 0.0129 (14) | 0.0017 (12) | 0.0101 (11) |
C71 | 0.117 (3) | 0.141 (4) | 0.084 (3) | 0.095 (3) | 0.052 (2) | 0.049 (3) |
O1 | 0.0262 (6) | 0.0181 (6) | 0.0242 (6) | −0.0010 (5) | 0.0086 (5) | −0.0030 (5) |
O2 | 0.0268 (6) | 0.0177 (6) | 0.0159 (6) | −0.0029 (5) | 0.0057 (5) | 0.0026 (5) |
O3 | 0.0238 (6) | 0.0196 (6) | 0.0207 (6) | −0.0029 (5) | 0.0033 (5) | 0.0006 (5) |
O4 | 0.0340 (8) | 0.0580 (10) | 0.0177 (6) | −0.0144 (7) | 0.0062 (6) | 0.0076 (6) |
O5 | 0.0284 (7) | 0.0465 (9) | 0.0439 (9) | 0.0115 (7) | 0.0051 (6) | 0.0116 (7) |
O6 | 0.0224 (6) | 0.0143 (6) | 0.0193 (6) | 0.0003 (5) | 0.0048 (5) | 0.0004 (5) |
O7 | 0.0209 (6) | 0.0155 (6) | 0.0219 (6) | 0.0024 (5) | 0.0063 (5) | −0.0014 (5) |
O8 | 0.0286 (6) | 0.0151 (6) | 0.0194 (6) | 0.0034 (5) | 0.0088 (5) | 0.0023 (5) |
O9 | 0.0383 (7) | 0.0200 (6) | 0.0281 (7) | −0.0032 (6) | 0.0090 (6) | 0.0074 (5) |
O10 | 0.0401 (8) | 0.0234 (7) | 0.0397 (8) | −0.0024 (6) | 0.0229 (7) | −0.0100 (6) |
O11 | 0.0582 (10) | 0.0314 (8) | 0.0284 (7) | 0.0217 (7) | 0.0035 (7) | 0.0045 (6) |
P1 | 0.0217 (2) | 0.0164 (2) | 0.0153 (2) | −0.00067 (16) | 0.00582 (16) | 0.00060 (16) |
P2 | 0.0205 (2) | 0.0132 (2) | 0.01642 (19) | 0.00155 (15) | 0.00628 (15) | 0.00047 (15) |
Rh1 | 0.02171 (7) | 0.01364 (7) | 0.01554 (7) | 0.00143 (5) | 0.00610 (5) | 0.00137 (5) |
Geometric parameters (Å, º) top
C1—C2 | 1.381 (3) | C39—H39 | 0.9500 |
C1—C6 | 1.392 (3) | C40—C41 | 1.489 (2) |
C1—O1 | 1.400 (2) | C41—C46 | 1.387 (2) |
C2—C3 | 1.383 (3) | C41—C42 | 1.401 (2) |
C2—H2 | 0.9500 | C42—C43 | 1.377 (2) |
C3—C4 | 1.382 (3) | C42—H42 | 0.9500 |
C3—H3 | 0.9500 | C43—O10 | 1.373 (2) |
C4—C5 | 1.383 (3) | C43—C44 | 1.388 (3) |
C4—H4 | 0.9500 | C44—C45 | 1.391 (2) |
C5—C6 | 1.396 (3) | C44—H44 | 0.9500 |
C5—H5 | 0.9500 | C45—C46 | 1.408 (2) |
C6—C7 | 1.483 (3) | C45—C53 | 1.537 (2) |
C7—C12 | 1.392 (3) | C46—O7 | 1.399 (2) |
C7—C8 | 1.395 (3) | C47—C49 | 1.529 (3) |
C8—C9 | 1.386 (3) | C47—C48 | 1.536 (3) |
C8—H8 | 0.9500 | C47—C50 | 1.537 (3) |
C9—C10 | 1.370 (4) | C48—H48A | 0.9800 |
C9—H9 | 0.9500 | C48—H48B | 0.9800 |
C10—C11 | 1.389 (3) | C48—H48C | 0.9800 |
C10—H10 | 0.9500 | C49—H49A | 0.9800 |
C11—C12 | 1.389 (3) | C49—H49B | 0.9800 |
C11—H11 | 0.9500 | C49—H49C | 0.9800 |
C12—H12 | 0.9500 | C50—H50A | 0.9800 |
C13—C18 | 1.386 (3) | C50—H50B | 0.9800 |
C13—C14 | 1.407 (2) | C50—H50C | 0.9800 |
C13—O2 | 1.411 (2) | C51—O9 | 1.427 (3) |
C14—C15 | 1.386 (3) | C51—H51A | 0.9800 |
C14—C25 | 1.543 (3) | C51—H51B | 0.9800 |
C15—C16 | 1.389 (3) | C51—H51C | 0.9800 |
C15—H15 | 0.9500 | C52—O10 | 1.422 (2) |
C16—O4 | 1.373 (2) | C52—H52A | 0.9800 |
C16—C17 | 1.380 (3) | C52—H52B | 0.9800 |
C17—C18 | 1.402 (2) | C52—H52C | 0.9800 |
C17—H17 | 0.9500 | C53—C55 | 1.527 (3) |
C18—C19 | 1.491 (2) | C53—C56 | 1.531 (3) |
C19—C24 | 1.395 (2) | C53—C54 | 1.535 (3) |
C19—C20 | 1.398 (3) | C54—H54A | 0.9800 |
C20—C21 | 1.382 (3) | C54—H54B | 0.9800 |
C20—H20 | 0.9500 | C54—H54C | 0.9800 |
C21—O5 | 1.366 (2) | C55—H55A | 0.9800 |
C21—C22 | 1.391 (3) | C55—H55B | 0.9800 |
C22—C23 | 1.382 (3) | C55—H55C | 0.9800 |
C22—H22 | 0.9500 | C56—H56A | 0.9800 |
C23—C24 | 1.409 (2) | C56—H56B | 0.9800 |
C23—C31 | 1.539 (3) | C56—H56C | 0.9800 |
C24—O3 | 1.402 (2) | C57—O11 | 1.143 (2) |
C25—C27 | 1.528 (3) | C57—Rh1 | 1.8057 (19) |
C25—C26 | 1.530 (3) | C58—C59 | 1.3900 |
C25—C28 | 1.538 (3) | C58—C63 | 1.3900 |
C26—H26A | 0.9800 | C58—C64 | 1.472 (4) |
C26—H26B | 0.9800 | C59—C60 | 1.3900 |
C26—H26C | 0.9800 | C59—H59 | 0.9500 |
C27—H27A | 0.9800 | C60—C61 | 1.3900 |
C27—H27B | 0.9800 | C60—H60 | 0.9500 |
C27—H27C | 0.9800 | C61—C62 | 1.3900 |
C28—H28A | 0.9800 | C61—H61 | 0.9500 |
C28—H28B | 0.9800 | C62—C63 | 1.3900 |
C28—H28C | 0.9800 | C62—H62 | 0.9500 |
C29—O4 | 1.411 (2) | C63—H63 | 0.9500 |
C29—H29A | 0.9800 | C64—H64A | 0.9800 |
C29—H29B | 0.9800 | C64—H64B | 0.9800 |
C29—H29C | 0.9800 | C64—H64C | 0.9800 |
C30—O5 | 1.425 (3) | C65—C66 | 1.3900 |
C30—H30A | 0.9800 | C65—C70 | 1.3900 |
C30—H30B | 0.9800 | C65—C71 | 1.492 (3) |
C30—H30C | 0.9800 | C66—C67 | 1.3900 |
C31—C33 | 1.525 (3) | C66—H66 | 0.9500 |
C31—C32 | 1.529 (3) | C67—C68 | 1.3900 |
C31—C34 | 1.537 (3) | C67—H67 | 0.9500 |
C32—H32A | 0.9800 | C68—C69 | 1.3900 |
C32—H32B | 0.9800 | C68—H68 | 0.9500 |
C32—H32C | 0.9800 | C69—C70 | 1.3900 |
C33—H33A | 0.9800 | C69—H69 | 0.9500 |
C33—H33B | 0.9800 | C70—H70 | 0.9500 |
C33—H33C | 0.9800 | C71—H71A | 0.9800 |
C34—H34A | 0.9800 | C71—H71B | 0.9800 |
C34—H34B | 0.9800 | C71—H71C | 0.9800 |
C34—H34C | 0.9800 | O1—P1 | 1.5999 (13) |
C35—C40 | 1.388 (2) | O2—P1 | 1.5976 (12) |
C35—O6 | 1.399 (2) | O3—P1 | 1.6157 (13) |
C35—C36 | 1.407 (2) | O6—P2 | 1.6393 (13) |
C36—C37 | 1.390 (3) | O7—P2 | 1.6217 (12) |
C36—C47 | 1.543 (3) | O8—P2 | 1.5081 (12) |
C37—C38 | 1.392 (3) | O8—Rh1i | 2.0710 (12) |
C37—H37 | 0.9500 | P1—Rh1 | 2.2906 (4) |
C38—O9 | 1.367 (2) | P2—Rh1 | 2.3049 (4) |
C38—C39 | 1.382 (2) | Rh1—O8i | 2.0711 (12) |
C39—C40 | 1.399 (2) | | |
| | | |
C2—C1—C6 | 122.00 (17) | C43—C42—C41 | 118.93 (17) |
C2—C1—O1 | 121.74 (16) | C43—C42—H42 | 120.5 |
C6—C1—O1 | 116.20 (16) | C41—C42—H42 | 120.5 |
C1—C2—C3 | 119.42 (18) | O10—C43—C42 | 124.42 (17) |
C1—C2—H2 | 120.3 | O10—C43—C44 | 115.35 (16) |
C3—C2—H2 | 120.3 | C42—C43—C44 | 120.23 (17) |
C4—C3—C2 | 120.3 (2) | C43—C44—C45 | 122.50 (16) |
C4—C3—H3 | 119.9 | C43—C44—H44 | 118.7 |
C2—C3—H3 | 119.9 | C45—C44—H44 | 118.7 |
C3—C4—C5 | 119.4 (2) | C44—C45—C46 | 116.12 (16) |
C3—C4—H4 | 120.3 | C44—C45—C53 | 120.70 (15) |
C5—C4—H4 | 120.3 | C46—C45—C53 | 123.15 (15) |
C4—C5—C6 | 121.78 (19) | C41—C46—O7 | 117.70 (14) |
C4—C5—H5 | 119.1 | C41—C46—C45 | 121.73 (15) |
C6—C5—H5 | 119.1 | O7—C46—C45 | 120.21 (15) |
C1—C6—C5 | 117.08 (18) | C49—C47—C48 | 109.71 (17) |
C1—C6—C7 | 123.20 (17) | C49—C47—C50 | 107.67 (17) |
C5—C6—C7 | 119.70 (17) | C48—C47—C50 | 107.21 (17) |
C12—C7—C8 | 118.9 (2) | C49—C47—C36 | 112.74 (16) |
C12—C7—C6 | 121.40 (17) | C48—C47—C36 | 107.97 (15) |
C8—C7—C6 | 119.61 (19) | C50—C47—C36 | 111.41 (16) |
C9—C8—C7 | 120.2 (2) | C47—C48—H48A | 109.5 |
C9—C8—H8 | 119.9 | C47—C48—H48B | 109.5 |
C7—C8—H8 | 119.9 | H48A—C48—H48B | 109.5 |
C10—C9—C8 | 120.6 (2) | C47—C48—H48C | 109.5 |
C10—C9—H9 | 119.7 | H48A—C48—H48C | 109.5 |
C8—C9—H9 | 119.7 | H48B—C48—H48C | 109.5 |
C9—C10—C11 | 120.1 (2) | C47—C49—H49A | 109.5 |
C9—C10—H10 | 120.0 | C47—C49—H49B | 109.5 |
C11—C10—H10 | 120.0 | H49A—C49—H49B | 109.5 |
C10—C11—C12 | 119.7 (2) | C47—C49—H49C | 109.5 |
C10—C11—H11 | 120.1 | H49A—C49—H49C | 109.5 |
C12—C11—H11 | 120.1 | H49B—C49—H49C | 109.5 |
C11—C12—C7 | 120.5 (2) | C47—C50—H50A | 109.5 |
C11—C12—H12 | 119.7 | C47—C50—H50B | 109.5 |
C7—C12—H12 | 119.7 | H50A—C50—H50B | 109.5 |
C18—C13—C14 | 122.73 (16) | C47—C50—H50C | 109.5 |
C18—C13—O2 | 117.61 (15) | H50A—C50—H50C | 109.5 |
C14—C13—O2 | 119.25 (15) | H50B—C50—H50C | 109.5 |
C15—C14—C13 | 115.79 (17) | O9—C51—H51A | 109.5 |
C15—C14—C25 | 120.03 (16) | O9—C51—H51B | 109.5 |
C13—C14—C25 | 123.99 (16) | H51A—C51—H51B | 109.5 |
C14—C15—C16 | 122.64 (17) | O9—C51—H51C | 109.5 |
C14—C15—H15 | 118.7 | H51A—C51—H51C | 109.5 |
C16—C15—H15 | 118.7 | H51B—C51—H51C | 109.5 |
O4—C16—C17 | 124.70 (17) | O10—C52—H52A | 109.5 |
O4—C16—C15 | 115.14 (16) | O10—C52—H52B | 109.5 |
C17—C16—C15 | 120.13 (17) | H52A—C52—H52B | 109.5 |
C16—C17—C18 | 119.28 (17) | O10—C52—H52C | 109.5 |
C16—C17—H17 | 120.4 | H52A—C52—H52C | 109.5 |
C18—C17—H17 | 120.4 | H52B—C52—H52C | 109.5 |
C13—C18—C17 | 119.01 (16) | C55—C53—C56 | 111.18 (18) |
C13—C18—C19 | 123.40 (15) | C55—C53—C54 | 107.22 (16) |
C17—C18—C19 | 117.38 (16) | C56—C53—C54 | 106.48 (17) |
C24—C19—C20 | 119.12 (16) | C55—C53—C45 | 109.93 (16) |
C24—C19—C18 | 123.38 (16) | C56—C53—C45 | 110.40 (16) |
C20—C19—C18 | 117.44 (16) | C54—C53—C45 | 111.55 (15) |
C21—C20—C19 | 119.26 (18) | C53—C54—H54A | 109.5 |
C21—C20—H20 | 120.4 | C53—C54—H54B | 109.5 |
C19—C20—H20 | 120.4 | H54A—C54—H54B | 109.5 |
O5—C21—C20 | 124.53 (19) | C53—C54—H54C | 109.5 |
O5—C21—C22 | 115.29 (18) | H54A—C54—H54C | 109.5 |
C20—C21—C22 | 120.19 (18) | H54B—C54—H54C | 109.5 |
C23—C22—C21 | 122.70 (17) | C53—C55—H55A | 109.5 |
C23—C22—H22 | 118.7 | C53—C55—H55B | 109.5 |
C21—C22—H22 | 118.7 | H55A—C55—H55B | 109.5 |
C22—C23—C24 | 115.96 (17) | C53—C55—H55C | 109.5 |
C22—C23—C31 | 120.39 (17) | H55A—C55—H55C | 109.5 |
C24—C23—C31 | 123.59 (17) | H55B—C55—H55C | 109.5 |
C19—C24—O3 | 116.57 (15) | C53—C56—H56A | 109.5 |
C19—C24—C23 | 122.43 (17) | C53—C56—H56B | 109.5 |
O3—C24—C23 | 120.80 (16) | H56A—C56—H56B | 109.5 |
C27—C25—C26 | 109.77 (17) | C53—C56—H56C | 109.5 |
C27—C25—C28 | 106.94 (17) | H56A—C56—H56C | 109.5 |
C26—C25—C28 | 107.82 (18) | H56B—C56—H56C | 109.5 |
C27—C25—C14 | 112.75 (16) | O11—C57—Rh1 | 177.9 (2) |
C26—C25—C14 | 108.25 (16) | C59—C58—C63 | 120.0 |
C28—C25—C14 | 111.19 (16) | C59—C58—C64 | 120.2 (2) |
C25—C26—H26A | 109.5 | C63—C58—C64 | 119.8 (2) |
C25—C26—H26B | 109.5 | C60—C59—C58 | 120.0 |
H26A—C26—H26B | 109.5 | C60—C59—H59 | 120.0 |
C25—C26—H26C | 109.5 | C58—C59—H59 | 120.0 |
H26A—C26—H26C | 109.5 | C59—C60—C61 | 120.0 |
H26B—C26—H26C | 109.5 | C59—C60—H60 | 120.0 |
C25—C27—H27A | 109.5 | C61—C60—H60 | 120.0 |
C25—C27—H27B | 109.5 | C62—C61—C60 | 120.0 |
H27A—C27—H27B | 109.5 | C62—C61—H61 | 120.0 |
C25—C27—H27C | 109.5 | C60—C61—H61 | 120.0 |
H27A—C27—H27C | 109.5 | C61—C62—C63 | 120.0 |
H27B—C27—H27C | 109.5 | C61—C62—H62 | 120.0 |
C25—C28—H28A | 109.5 | C63—C62—H62 | 120.0 |
C25—C28—H28B | 109.5 | C62—C63—C58 | 120.0 |
H28A—C28—H28B | 109.5 | C62—C63—H63 | 120.0 |
C25—C28—H28C | 109.5 | C58—C63—H63 | 120.0 |
H28A—C28—H28C | 109.5 | C58—C64—H64A | 109.5 |
H28B—C28—H28C | 109.5 | C58—C64—H64B | 109.5 |
O4—C29—H29A | 109.5 | H64A—C64—H64B | 109.5 |
O4—C29—H29B | 109.5 | C58—C64—H64C | 109.5 |
H29A—C29—H29B | 109.5 | H64A—C64—H64C | 109.5 |
O4—C29—H29C | 109.5 | H64B—C64—H64C | 109.5 |
H29A—C29—H29C | 109.5 | C66—C65—C70 | 120.0 |
H29B—C29—H29C | 109.5 | C66—C65—C71 | 119.52 (19) |
O5—C30—H30A | 109.5 | C70—C65—C71 | 120.47 (19) |
O5—C30—H30B | 109.5 | C65—C66—C67 | 120.0 |
H30A—C30—H30B | 109.5 | C65—C66—H66 | 120.0 |
O5—C30—H30C | 109.5 | C67—C66—H66 | 120.0 |
H30A—C30—H30C | 109.5 | C68—C67—C66 | 120.0 |
H30B—C30—H30C | 109.5 | C68—C67—H67 | 120.0 |
C33—C31—C32 | 110.5 (2) | C66—C67—H67 | 120.0 |
C33—C31—C34 | 107.35 (19) | C69—C68—C67 | 120.0 |
C32—C31—C34 | 106.89 (17) | C69—C68—H68 | 120.0 |
C33—C31—C23 | 109.79 (17) | C67—C68—H68 | 120.0 |
C32—C31—C23 | 111.18 (17) | C68—C69—C70 | 120.0 |
C34—C31—C23 | 111.05 (18) | C68—C69—H69 | 120.0 |
C31—C32—H32A | 109.5 | C70—C69—H69 | 120.0 |
C31—C32—H32B | 109.5 | C69—C70—C65 | 120.0 |
H32A—C32—H32B | 109.5 | C69—C70—H70 | 120.0 |
C31—C32—H32C | 109.5 | C65—C70—H70 | 120.0 |
H32A—C32—H32C | 109.5 | C65—C71—H71A | 109.5 |
H32B—C32—H32C | 109.5 | C65—C71—H71B | 109.5 |
C31—C33—H33A | 109.5 | H71A—C71—H71B | 109.5 |
C31—C33—H33B | 109.5 | C65—C71—H71C | 109.5 |
H33A—C33—H33B | 109.5 | H71A—C71—H71C | 109.5 |
C31—C33—H33C | 109.5 | H71B—C71—H71C | 109.5 |
H33A—C33—H33C | 109.5 | C1—O1—P1 | 126.22 (11) |
H33B—C33—H33C | 109.5 | C13—O2—P1 | 124.26 (11) |
C31—C34—H34A | 109.5 | C24—O3—P1 | 120.71 (11) |
C31—C34—H34B | 109.5 | C16—O4—C29 | 117.31 (15) |
H34A—C34—H34B | 109.5 | C21—O5—C30 | 116.40 (17) |
C31—C34—H34C | 109.5 | C35—O6—P2 | 116.77 (10) |
H34A—C34—H34C | 109.5 | C46—O7—P2 | 126.12 (11) |
H34B—C34—H34C | 109.5 | P2—O8—Rh1i | 140.28 (7) |
C40—C35—O6 | 117.37 (15) | C38—O9—C51 | 117.38 (15) |
C40—C35—C36 | 122.00 (16) | C43—O10—C52 | 116.63 (15) |
O6—C35—C36 | 120.50 (15) | O2—P1—O1 | 101.63 (7) |
C37—C36—C35 | 116.15 (16) | O2—P1—O3 | 105.08 (7) |
C37—C36—C47 | 121.14 (16) | O1—P1—O3 | 97.10 (7) |
C35—C36—C47 | 122.34 (16) | O2—P1—Rh1 | 107.40 (5) |
C36—C37—C38 | 122.28 (17) | O1—P1—Rh1 | 123.27 (5) |
C36—C37—H37 | 118.9 | O3—P1—Rh1 | 119.82 (5) |
C38—C37—H37 | 118.9 | O8—P2—O7 | 107.83 (7) |
O9—C38—C39 | 124.45 (17) | O8—P2—O6 | 101.89 (7) |
O9—C38—C37 | 115.45 (16) | O7—P2—O6 | 102.46 (6) |
C39—C38—C37 | 120.06 (17) | O8—P2—Rh1 | 121.95 (5) |
C38—C39—C40 | 119.16 (17) | O7—P2—Rh1 | 106.81 (5) |
C38—C39—H39 | 120.4 | O6—P2—Rh1 | 114.16 (5) |
C40—C39—H39 | 120.4 | C57—Rh1—O8i | 178.25 (7) |
C35—C40—C39 | 119.49 (16) | C57—Rh1—P1 | 87.14 (6) |
C35—C40—C41 | 121.36 (15) | O8i—Rh1—P1 | 92.36 (3) |
C39—C40—C41 | 118.95 (15) | C57—Rh1—P2 | 87.55 (6) |
C46—C41—C42 | 119.95 (15) | O8i—Rh1—P2 | 93.00 (3) |
C46—C41—C40 | 122.74 (15) | P1—Rh1—P2 | 174.350 (16) |
C42—C41—C40 | 117.31 (16) | | |
| | | |
C6—C1—C2—C3 | 0.0 (3) | C38—C39—C40—C41 | −174.31 (16) |
O1—C1—C2—C3 | 177.22 (18) | C35—C40—C41—C46 | 54.6 (2) |
C1—C2—C3—C4 | −0.9 (3) | C39—C40—C41—C46 | −130.68 (18) |
C2—C3—C4—C5 | 0.6 (3) | C35—C40—C41—C42 | −125.56 (18) |
C3—C4—C5—C6 | 0.6 (4) | C39—C40—C41—C42 | 49.2 (2) |
C2—C1—C6—C5 | 1.1 (3) | C46—C41—C42—C43 | −0.6 (3) |
O1—C1—C6—C5 | −176.24 (17) | C40—C41—C42—C43 | 179.59 (17) |
C2—C1—C6—C7 | −177.06 (18) | C41—C42—C43—O10 | −174.92 (18) |
O1—C1—C6—C7 | 5.6 (3) | C41—C42—C43—C44 | 5.0 (3) |
C4—C5—C6—C1 | −1.4 (3) | O10—C43—C44—C45 | 176.86 (17) |
C4—C5—C6—C7 | 176.8 (2) | C42—C43—C44—C45 | −3.1 (3) |
C1—C6—C7—C12 | 59.9 (3) | C43—C44—C45—C46 | −3.3 (3) |
C5—C6—C7—C12 | −118.2 (2) | C43—C44—C45—C53 | 174.90 (18) |
C1—C6—C7—C8 | −124.3 (2) | C42—C41—C46—O7 | −179.21 (15) |
C5—C6—C7—C8 | 57.5 (3) | C40—C41—C46—O7 | 0.6 (2) |
C12—C7—C8—C9 | 0.4 (3) | C42—C41—C46—C45 | −6.1 (3) |
C6—C7—C8—C9 | −175.45 (19) | C40—C41—C46—C45 | 173.78 (16) |
C7—C8—C9—C10 | 0.3 (3) | C44—C45—C46—C41 | 7.8 (3) |
C8—C9—C10—C11 | −0.4 (4) | C53—C45—C46—C41 | −170.31 (17) |
C9—C10—C11—C12 | −0.4 (3) | C44—C45—C46—O7 | −179.22 (15) |
C10—C11—C12—C7 | 1.1 (3) | C53—C45—C46—O7 | 2.7 (3) |
C8—C7—C12—C11 | −1.2 (3) | C37—C36—C47—C49 | 123.2 (2) |
C6—C7—C12—C11 | 174.64 (19) | C35—C36—C47—C49 | −64.0 (2) |
C18—C13—C14—C15 | 6.5 (3) | C37—C36—C47—C48 | −115.40 (19) |
O2—C13—C14—C15 | 178.99 (16) | C35—C36—C47—C48 | 57.3 (2) |
C18—C13—C14—C25 | −168.51 (17) | C37—C36—C47—C50 | 2.1 (2) |
O2—C13—C14—C25 | 3.9 (3) | C35—C36—C47—C50 | 174.80 (18) |
C13—C14—C15—C16 | −1.5 (3) | C44—C45—C53—C55 | 111.1 (2) |
C25—C14—C15—C16 | 173.73 (18) | C46—C45—C53—C55 | −70.9 (2) |
C14—C15—C16—O4 | 178.17 (18) | C44—C45—C53—C56 | −125.9 (2) |
C14—C15—C16—C17 | −3.7 (3) | C46—C45—C53—C56 | 52.1 (2) |
O4—C16—C17—C18 | −177.94 (18) | C44—C45—C53—C54 | −7.7 (3) |
C15—C16—C17—C18 | 4.1 (3) | C46—C45—C53—C54 | 170.29 (18) |
C14—C13—C18—C17 | −6.2 (3) | C63—C58—C59—C60 | 0.0 |
O2—C13—C18—C17 | −178.77 (16) | C64—C58—C59—C60 | 179.6 (3) |
C14—C13—C18—C19 | 168.40 (17) | C58—C59—C60—C61 | 0.0 |
O2—C13—C18—C19 | −4.2 (3) | C59—C60—C61—C62 | 0.0 |
C16—C17—C18—C13 | 0.6 (3) | C60—C61—C62—C63 | 0.0 |
C16—C17—C18—C19 | −174.28 (17) | C61—C62—C63—C58 | 0.0 |
C13—C18—C19—C24 | 52.2 (3) | C59—C58—C63—C62 | 0.0 |
C17—C18—C19—C24 | −133.16 (19) | C64—C58—C63—C62 | −179.6 (3) |
C13—C18—C19—C20 | −130.61 (19) | C70—C65—C66—C67 | 0.0 |
C17—C18—C19—C20 | 44.1 (2) | C71—C65—C66—C67 | 179.1 (3) |
C24—C19—C20—C21 | 0.3 (3) | C65—C66—C67—C68 | 0.0 |
C18—C19—C20—C21 | −177.09 (17) | C66—C67—C68—C69 | 0.0 |
C19—C20—C21—O5 | −176.43 (18) | C67—C68—C69—C70 | 0.0 |
C19—C20—C21—C22 | 3.8 (3) | C68—C69—C70—C65 | 0.0 |
O5—C21—C22—C23 | 177.17 (18) | C66—C65—C70—C69 | 0.0 |
C20—C21—C22—C23 | −3.0 (3) | C71—C65—C70—C69 | −179.1 (3) |
C21—C22—C23—C24 | −1.8 (3) | C2—C1—O1—P1 | 26.3 (2) |
C21—C22—C23—C31 | 175.35 (18) | C6—C1—O1—P1 | −156.39 (14) |
C20—C19—C24—O3 | 179.79 (15) | C18—C13—O2—P1 | −63.9 (2) |
C18—C19—C24—O3 | −3.0 (2) | C14—C13—O2—P1 | 123.26 (15) |
C20—C19—C24—C23 | −5.4 (3) | C19—C24—O3—P1 | −69.83 (18) |
C18—C19—C24—C23 | 171.83 (17) | C23—C24—O3—P1 | 115.23 (16) |
C22—C23—C24—C19 | 6.0 (3) | C17—C16—O4—C29 | 11.4 (3) |
C31—C23—C24—C19 | −171.03 (17) | C15—C16—O4—C29 | −170.62 (19) |
C22—C23—C24—O3 | −179.34 (16) | C20—C21—O5—C30 | −6.4 (3) |
C31—C23—C24—O3 | 3.6 (3) | C22—C21—O5—C30 | 173.3 (2) |
C15—C14—C25—C27 | 126.3 (2) | C40—C35—O6—P2 | −71.52 (17) |
C13—C14—C25—C27 | −58.9 (2) | C36—C35—O6—P2 | 112.59 (15) |
C15—C14—C25—C26 | −112.1 (2) | C41—C46—O7—P2 | −63.4 (2) |
C13—C14—C25—C26 | 62.7 (2) | C45—C46—O7—P2 | 123.33 (15) |
C15—C14—C25—C28 | 6.2 (3) | C39—C38—O9—C51 | −0.8 (3) |
C13—C14—C25—C28 | −178.99 (19) | C37—C38—O9—C51 | 177.12 (17) |
C22—C23—C31—C33 | −124.4 (2) | C42—C43—O10—C52 | −5.2 (3) |
C24—C23—C31—C33 | 52.6 (3) | C44—C43—O10—C52 | 174.89 (19) |
C22—C23—C31—C32 | 113.1 (2) | C13—O2—P1—O1 | −61.60 (14) |
C24—C23—C31—C32 | −70.0 (2) | C13—O2—P1—O3 | 39.12 (14) |
C22—C23—C31—C34 | −5.8 (3) | C13—O2—P1—Rh1 | 167.75 (12) |
C24—C23—C31—C34 | 171.14 (19) | C1—O1—P1—O2 | 160.96 (13) |
C40—C35—C36—C37 | 9.9 (3) | C1—O1—P1—O3 | 53.90 (14) |
O6—C35—C36—C37 | −174.39 (15) | C1—O1—P1—Rh1 | −79.02 (14) |
C40—C35—C36—C47 | −163.16 (17) | C24—O3—P1—O2 | 49.52 (13) |
O6—C35—C36—C47 | 12.5 (3) | C24—O3—P1—O1 | 153.65 (12) |
C35—C36—C37—C38 | −3.4 (3) | C24—O3—P1—Rh1 | −71.24 (13) |
C47—C36—C37—C38 | 169.73 (17) | Rh1i—O8—P2—O7 | −156.08 (11) |
C36—C37—C38—O9 | 177.68 (16) | Rh1i—O8—P2—O6 | 96.51 (12) |
C36—C37—C38—C39 | −4.3 (3) | Rh1i—O8—P2—Rh1 | −32.11 (15) |
O9—C38—C39—C40 | −176.40 (16) | C46—O7—P2—O8 | −78.92 (14) |
C37—C38—C39—C40 | 5.8 (3) | C46—O7—P2—O6 | 28.10 (14) |
O6—C35—C40—C39 | 175.53 (15) | C46—O7—P2—Rh1 | 148.40 (12) |
C36—C35—C40—C39 | −8.6 (3) | C35—O6—P2—O8 | 172.30 (11) |
O6—C35—C40—C41 | −9.8 (2) | C35—O6—P2—O7 | 60.77 (12) |
C36—C35—C40—C41 | 166.06 (16) | C35—O6—P2—Rh1 | −54.30 (12) |
C38—C39—C40—C35 | 0.5 (3) | | |
Symmetry code: (i) −x, −y+2, −z. |