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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

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S2053229619002730/qf3023sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2053229619002730/qf3023Isup2.hkl
Contains datablock I

CCDC reference: 1898827

Computing details top

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]-1:2κ2P:\ 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} toluene tatrasolvate top
Crystal data top
[Rh2(C22H28O5P)2(C34H37O5P)2(CO)2]·4C7H8F(000) = 2680
Mr = 2550.41Dx = 1.319 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
a = 13.4100 (5) ÅCell parameters from 9938 reflections
b = 15.5455 (5) Åθ = 2.3–30.3°
c = 31.1570 (11) ŵ = 0.38 mm1
β = 98.7430 (14)°T = 150 K
V = 6419.7 (4) Å3Prism, yellow
Z = 20.41 × 0.34 × 0.32 mm
Data collection top
Bruker APEXII CCD
diffractometer
15481 independent reflections
Radiation source: fine-focus sealed tube13358 reflections with I > 2σ(I)
Detector resolution: 8.3333 pixels mm-1Rint = 0.040
φ and ω scansθmax = 28.0°, θmin = 1.6°
Absorption correction: multi-scan
(SADABS; Bruker, 2014)
h = 1717
Tmin = 0.86, Tmax = 0.89k = 2020
140325 measured reflectionsl = 4141
Refinement top
Refinement on F20 restraints
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.035H-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 reflectionsΔρmax = 0.81 e Å3
760 parametersΔρmin = 0.39 e Å3
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
xyzUiso*/Ueq
C10.05877 (14)1.10380 (12)0.15205 (6)0.0222 (3)
C20.00322 (15)1.14899 (13)0.12855 (6)0.0274 (4)
H20.04141.11950.10980.033*
C30.00930 (18)1.23754 (14)0.13250 (7)0.0342 (5)
H30.05261.26900.11670.041*
C40.04732 (19)1.28050 (14)0.15927 (7)0.0387 (5)
H40.04371.34140.16180.046*
C50.10935 (17)1.23413 (13)0.18239 (7)0.0343 (5)
H50.14861.26400.20050.041*
C60.11587 (14)1.14461 (12)0.17978 (6)0.0255 (4)
C70.17942 (15)1.09749 (13)0.20697 (6)0.0273 (4)
C80.28188 (16)1.11705 (15)0.20360 (7)0.0346 (5)
H80.31151.15730.18250.042*
C90.34058 (17)1.07785 (17)0.23096 (8)0.0427 (6)
H90.41041.09130.22840.051*
C100.29892 (18)1.01997 (17)0.26169 (8)0.0435 (6)
H100.33970.99370.28040.052*
C110.19711 (18)0.99962 (15)0.26553 (8)0.0390 (5)
H110.16810.95970.28690.047*
C120.13792 (16)1.03784 (14)0.23793 (7)0.0307 (4)
H120.06861.02310.24020.037*
C130.03331 (13)0.84098 (11)0.19468 (5)0.0199 (3)
C140.12566 (14)0.81619 (12)0.20717 (6)0.0227 (4)
C150.12299 (14)0.79805 (13)0.25087 (6)0.0263 (4)
H150.18400.78240.26090.032*
C160.03476 (15)0.80181 (13)0.28062 (6)0.0258 (4)
C170.05601 (14)0.81946 (12)0.26674 (6)0.0240 (4)
H170.11710.81840.28670.029*
C180.05714 (13)0.83903 (11)0.22290 (6)0.0208 (3)
C190.15755 (13)0.84937 (12)0.20853 (5)0.0212 (3)
C200.23197 (14)0.78886 (13)0.22332 (6)0.0252 (4)
H200.21710.74170.24070.030*
C210.32743 (15)0.79833 (14)0.21237 (6)0.0288 (4)
C220.35060 (14)0.87008 (14)0.18910 (6)0.0285 (4)
H220.41760.87660.18320.034*
C230.28013 (14)0.93226 (12)0.17423 (6)0.0242 (4)
C240.18141 (13)0.91769 (12)0.18293 (6)0.0208 (3)
C250.22374 (14)0.80187 (13)0.17502 (6)0.0259 (4)
C260.20636 (17)0.72748 (15)0.14487 (8)0.0385 (5)
H26A0.26890.71560.12510.058*
H26B0.18600.67610.16220.058*
H26C0.15300.74310.12800.058*
C270.25697 (16)0.88192 (14)0.14816 (7)0.0340 (5)
H27A0.26250.93060.16760.051*
H27B0.32260.87120.13040.051*
H27C0.20710.89520.12920.051*
C280.31157 (16)0.77680 (18)0.19899 (7)0.0414 (6)
H28A0.32180.82210.21980.062*
H28B0.29570.72250.21450.062*
H28C0.37320.76980.17790.062*
C290.03783 (16)0.79999 (15)0.35515 (6)0.0334 (5)
H29A0.09340.76180.35060.050*
H29B0.01900.78900.38380.050*
H29C0.05930.86000.35340.050*
C300.38639 (18)0.67199 (17)0.25083 (9)0.0474 (6)
H30A0.37390.69510.27880.071*
H30B0.44550.63410.25550.071*
H30C0.32730.63930.23740.071*
C310.31189 (15)1.01366 (14)0.15168 (7)0.0305 (4)
C320.26525 (17)1.01554 (16)0.10375 (7)0.0386 (5)
H32A0.19171.01990.10130.058*
H32B0.28290.96260.08960.058*
H32C0.29131.06530.08960.058*
C330.28132 (19)1.09348 (15)0.17499 (8)0.0433 (6)
H33A0.31481.09290.20520.065*
H33B0.20801.09370.17430.065*
H33C0.30161.14510.16050.065*
C340.42695 (17)1.01700 (18)0.15328 (9)0.0468 (6)
H34A0.44591.07200.14140.070*
H34B0.44840.96970.13600.070*
H34C0.46001.01140.18340.070*
C350.01994 (13)0.74019 (11)0.00710 (5)0.0190 (3)
C360.10642 (13)0.71434 (11)0.01005 (6)0.0211 (3)
C370.09665 (14)0.64049 (12)0.03547 (6)0.0242 (4)
H370.15210.62260.04900.029*
C380.00846 (15)0.59184 (12)0.04181 (6)0.0234 (4)
C390.07087 (14)0.61313 (11)0.02026 (6)0.0216 (3)
H390.12870.57720.02240.026*
C400.06490 (13)0.68827 (11)0.00473 (6)0.0191 (3)
C410.14602 (13)0.70671 (11)0.03120 (6)0.0195 (3)
C420.17301 (14)0.64030 (11)0.05760 (6)0.0222 (3)
H420.14060.58590.05810.027*
C430.24729 (14)0.65520 (12)0.08274 (6)0.0243 (4)
C440.29977 (14)0.73246 (12)0.07929 (6)0.0243 (4)
H440.35290.74020.09590.029*
C450.27748 (13)0.79902 (11)0.05244 (6)0.0202 (3)
C460.19454 (13)0.78558 (11)0.03043 (5)0.0186 (3)
C470.20971 (14)0.75849 (13)0.00268 (6)0.0255 (4)
C480.23840 (16)0.75233 (15)0.05224 (7)0.0329 (4)
H48A0.30430.77950.06110.049*
H48B0.24180.69170.06100.049*
H48C0.18740.78190.06630.049*
C490.20901 (16)0.85279 (14)0.01137 (8)0.0351 (5)
H49A0.18540.85680.04260.053*
H49B0.27740.87630.00480.053*
H49C0.16380.88560.00440.053*
C500.29270 (16)0.71236 (17)0.01750 (8)0.0392 (5)
H50A0.27640.71440.04920.059*
H50B0.29710.65230.00790.059*
H50C0.35750.74100.00830.059*
C510.07793 (17)0.46875 (13)0.07478 (7)0.0328 (4)
H51A0.08580.44190.04700.049*
H51B0.06990.42390.09610.049*
H51C0.13790.50330.08520.049*
C520.22870 (18)0.51538 (14)0.11391 (8)0.0390 (5)
H52A0.24550.48700.08570.059*
H52B0.25320.48040.13630.059*
H52C0.15530.52190.12090.059*
C530.34312 (14)0.88047 (12)0.04674 (6)0.0244 (4)
C540.43790 (16)0.87090 (14)0.06847 (8)0.0349 (5)
H54A0.47650.82060.05650.052*
H54B0.47970.92260.06300.052*
H54C0.41800.86340.09980.052*
C550.28377 (16)0.95709 (13)0.06802 (8)0.0367 (5)
H55A0.26400.94570.09910.055*
H55B0.32601.00880.06420.055*
H55C0.22320.96590.05450.055*
C560.37997 (18)0.89737 (17)0.00145 (7)0.0413 (5)
H56A0.32180.90590.01660.062*
H56B0.42230.94900.00460.062*
H56C0.41940.84800.01410.062*
C570.10115 (15)0.83262 (12)0.08053 (6)0.0259 (4)
C580.43179 (16)0.65168 (12)0.08541 (7)0.0611 (8)
C590.50365 (15)0.59332 (16)0.10454 (7)0.0776 (11)
H590.54990.60960.12940.093*
C600.50780 (16)0.51116 (14)0.08730 (9)0.0863 (12)
H600.55690.47130.10040.104*
C610.4401 (2)0.48734 (13)0.05094 (10)0.0995 (14)
H610.44290.43120.03920.119*
C620.3682 (2)0.54570 (17)0.03182 (8)0.1091 (16)
H620.32190.52940.00700.131*
C630.36407 (16)0.62787 (15)0.04905 (7)0.0756 (10)
H630.31500.66780.03600.091*
C640.4267 (3)0.7386 (3)0.10370 (13)0.0878 (11)
H64A0.48340.77300.09680.132*
H64B0.43020.73460.13530.132*
H64C0.36300.76590.09120.132*
C650.21479 (11)0.53242 (11)0.17671 (5)0.0518 (7)
C660.17226 (11)0.60699 (10)0.15723 (5)0.0410 (5)
H660.20770.63950.13860.049*
C670.07787 (11)0.63405 (9)0.16505 (5)0.0401 (5)
H670.04880.68500.15170.048*
C680.02601 (10)0.58654 (12)0.19234 (6)0.0534 (7)
H680.03850.60500.19770.064*
C690.06854 (13)0.51197 (11)0.21182 (6)0.0584 (7)
H690.03310.47950.23050.070*
C700.16293 (14)0.48491 (9)0.20400 (5)0.0539 (7)
H700.19200.43390.21730.065*
C710.3155 (3)0.5033 (3)0.16757 (13)0.1101 (18)
H71A0.30650.45730.14580.165*
H71B0.35540.48180.19440.165*
H71C0.35070.55180.15650.165*
O10.07102 (9)1.01463 (8)0.14786 (4)0.0223 (3)
O20.02939 (9)0.85920 (8)0.15060 (4)0.0199 (2)
O30.10367 (9)0.97617 (8)0.16894 (4)0.0214 (3)
O40.04594 (11)0.78438 (11)0.32282 (4)0.0363 (4)
O50.40458 (11)0.74111 (11)0.22297 (5)0.0396 (4)
O60.01933 (9)0.81766 (7)0.02991 (4)0.0185 (2)
O70.16567 (9)0.84936 (8)0.00312 (4)0.0191 (2)
O80.04755 (9)0.96021 (8)0.04265 (4)0.0205 (2)
O90.00905 (11)0.52279 (9)0.06893 (4)0.0284 (3)
O100.27510 (11)0.59780 (9)0.11224 (5)0.0327 (3)
O110.14861 (13)0.77373 (10)0.09226 (5)0.0397 (4)
P10.00872 (3)0.94829 (3)0.13333 (2)0.01749 (9)
P20.05519 (3)0.89371 (3)0.00705 (2)0.01635 (9)
Rh10.03018 (2)0.92806 (2)0.06248 (2)0.01662 (4)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.0273 (9)0.0181 (8)0.0207 (8)0.0008 (7)0.0012 (7)0.0029 (7)
C20.0380 (10)0.0240 (9)0.0208 (9)0.0007 (8)0.0062 (8)0.0004 (7)
C30.0498 (13)0.0260 (10)0.0276 (10)0.0036 (9)0.0083 (9)0.0021 (8)
C40.0599 (14)0.0191 (10)0.0373 (12)0.0044 (9)0.0083 (10)0.0023 (8)
C50.0452 (12)0.0241 (10)0.0346 (11)0.0081 (9)0.0091 (9)0.0073 (8)
C60.0290 (9)0.0238 (9)0.0234 (9)0.0042 (7)0.0026 (7)0.0028 (7)
C70.0282 (9)0.0276 (10)0.0268 (9)0.0005 (8)0.0066 (7)0.0116 (8)
C80.0303 (10)0.0392 (12)0.0338 (11)0.0049 (9)0.0029 (8)0.0140 (9)
C90.0275 (10)0.0544 (15)0.0485 (14)0.0058 (10)0.0129 (10)0.0218 (12)
C100.0444 (13)0.0458 (14)0.0459 (13)0.0115 (11)0.0255 (11)0.0144 (11)
C110.0495 (13)0.0340 (12)0.0373 (12)0.0015 (10)0.0187 (10)0.0034 (9)
C120.0311 (10)0.0297 (10)0.0330 (10)0.0026 (8)0.0105 (8)0.0034 (8)
C130.0281 (9)0.0167 (8)0.0160 (8)0.0020 (7)0.0071 (6)0.0013 (6)
C140.0258 (9)0.0206 (9)0.0222 (9)0.0035 (7)0.0053 (7)0.0025 (7)
C150.0264 (9)0.0292 (10)0.0248 (9)0.0061 (8)0.0092 (7)0.0034 (8)
C160.0320 (10)0.0284 (10)0.0180 (8)0.0057 (8)0.0070 (7)0.0036 (7)
C170.0257 (9)0.0264 (9)0.0195 (8)0.0039 (7)0.0025 (7)0.0033 (7)
C180.0252 (8)0.0187 (8)0.0195 (8)0.0033 (7)0.0066 (7)0.0012 (7)
C190.0232 (8)0.0244 (9)0.0163 (8)0.0026 (7)0.0036 (6)0.0014 (7)
C200.0276 (9)0.0273 (9)0.0206 (8)0.0003 (7)0.0033 (7)0.0025 (7)
C210.0272 (9)0.0338 (11)0.0251 (9)0.0054 (8)0.0025 (7)0.0011 (8)
C220.0213 (9)0.0395 (11)0.0257 (9)0.0033 (8)0.0069 (7)0.0007 (8)
C230.0258 (9)0.0291 (10)0.0187 (8)0.0063 (7)0.0062 (7)0.0009 (7)
C240.0227 (8)0.0220 (9)0.0175 (8)0.0011 (7)0.0028 (6)0.0011 (7)
C250.0254 (9)0.0280 (10)0.0238 (9)0.0067 (7)0.0018 (7)0.0053 (7)
C260.0386 (12)0.0345 (12)0.0396 (12)0.0088 (9)0.0032 (9)0.0058 (9)
C270.0287 (10)0.0338 (11)0.0369 (11)0.0045 (8)0.0032 (8)0.0086 (9)
C280.0277 (10)0.0620 (16)0.0335 (11)0.0138 (10)0.0012 (9)0.0134 (11)
C290.0370 (11)0.0451 (13)0.0188 (9)0.0089 (9)0.0061 (8)0.0027 (8)
C300.0368 (12)0.0439 (14)0.0575 (16)0.0082 (10)0.0053 (11)0.0154 (12)
C310.0298 (10)0.0332 (11)0.0300 (10)0.0110 (8)0.0091 (8)0.0032 (8)
C320.0410 (12)0.0448 (13)0.0311 (11)0.0114 (10)0.0087 (9)0.0110 (10)
C330.0486 (14)0.0325 (12)0.0502 (14)0.0162 (10)0.0124 (11)0.0044 (10)
C340.0347 (12)0.0576 (16)0.0491 (14)0.0167 (11)0.0098 (10)0.0127 (12)
C350.0253 (8)0.0135 (8)0.0185 (8)0.0005 (6)0.0042 (6)0.0002 (6)
C360.0237 (8)0.0192 (8)0.0214 (8)0.0022 (7)0.0070 (7)0.0036 (7)
C370.0278 (9)0.0226 (9)0.0240 (9)0.0052 (7)0.0097 (7)0.0008 (7)
C380.0336 (10)0.0170 (8)0.0202 (8)0.0058 (7)0.0065 (7)0.0000 (7)
C390.0267 (9)0.0167 (8)0.0224 (8)0.0005 (7)0.0069 (7)0.0009 (7)
C400.0229 (8)0.0155 (8)0.0199 (8)0.0021 (6)0.0069 (6)0.0013 (6)
C410.0224 (8)0.0172 (8)0.0202 (8)0.0032 (6)0.0076 (6)0.0020 (6)
C420.0253 (9)0.0159 (8)0.0264 (9)0.0021 (7)0.0074 (7)0.0008 (7)
C430.0262 (9)0.0213 (9)0.0273 (9)0.0046 (7)0.0099 (7)0.0037 (7)
C440.0245 (9)0.0229 (9)0.0281 (9)0.0018 (7)0.0120 (7)0.0004 (7)
C450.0212 (8)0.0178 (8)0.0224 (8)0.0016 (6)0.0059 (7)0.0023 (7)
C460.0216 (8)0.0156 (8)0.0193 (8)0.0047 (6)0.0054 (6)0.0002 (6)
C470.0204 (8)0.0285 (10)0.0284 (9)0.0004 (7)0.0065 (7)0.0022 (8)
C480.0305 (10)0.0367 (11)0.0304 (10)0.0013 (9)0.0012 (8)0.0026 (9)
C490.0263 (10)0.0329 (11)0.0461 (12)0.0057 (8)0.0054 (9)0.0110 (9)
C500.0246 (10)0.0507 (14)0.0440 (13)0.0022 (9)0.0106 (9)0.0073 (11)
C510.0443 (12)0.0215 (9)0.0314 (10)0.0001 (8)0.0025 (9)0.0083 (8)
C520.0471 (13)0.0257 (10)0.0499 (13)0.0056 (9)0.0254 (11)0.0156 (10)
C530.0239 (9)0.0216 (9)0.0298 (9)0.0032 (7)0.0109 (7)0.0015 (7)
C540.0293 (10)0.0316 (11)0.0478 (13)0.0071 (8)0.0192 (9)0.0056 (9)
C550.0340 (11)0.0213 (10)0.0574 (14)0.0013 (8)0.0148 (10)0.0071 (9)
C560.0382 (12)0.0527 (14)0.0340 (11)0.0191 (11)0.0092 (9)0.0092 (10)
C570.0363 (10)0.0252 (9)0.0173 (8)0.0042 (8)0.0074 (7)0.0004 (7)
C580.0578 (17)0.0594 (18)0.0649 (19)0.0025 (14)0.0058 (14)0.0092 (15)
C590.0421 (16)0.085 (3)0.098 (3)0.0023 (16)0.0126 (16)0.024 (2)
C600.0446 (17)0.073 (2)0.139 (4)0.0028 (16)0.007 (2)0.028 (2)
C610.076 (3)0.097 (3)0.121 (4)0.009 (2)0.001 (2)0.003 (3)
C620.105 (3)0.100 (3)0.109 (4)0.020 (3)0.028 (3)0.014 (3)
C630.065 (2)0.081 (2)0.072 (2)0.0034 (18)0.0186 (17)0.0108 (19)
C640.093 (3)0.085 (3)0.082 (3)0.014 (2)0.001 (2)0.009 (2)
C650.0674 (17)0.0544 (16)0.0352 (12)0.0279 (14)0.0124 (12)0.0054 (11)
C660.0507 (14)0.0354 (12)0.0384 (12)0.0080 (10)0.0117 (10)0.0022 (10)
C670.0465 (13)0.0317 (11)0.0418 (12)0.0024 (10)0.0055 (10)0.0007 (10)
C680.0394 (13)0.0693 (19)0.0519 (15)0.0016 (13)0.0081 (11)0.0142 (14)
C690.0558 (16)0.070 (2)0.0484 (15)0.0059 (14)0.0047 (13)0.0232 (14)
C700.0779 (19)0.0463 (15)0.0354 (13)0.0129 (14)0.0017 (12)0.0101 (11)
C710.117 (3)0.141 (4)0.084 (3)0.095 (3)0.052 (2)0.049 (3)
O10.0262 (6)0.0181 (6)0.0242 (6)0.0010 (5)0.0086 (5)0.0030 (5)
O20.0268 (6)0.0177 (6)0.0159 (6)0.0029 (5)0.0057 (5)0.0026 (5)
O30.0238 (6)0.0196 (6)0.0207 (6)0.0029 (5)0.0033 (5)0.0006 (5)
O40.0340 (8)0.0580 (10)0.0177 (6)0.0144 (7)0.0062 (6)0.0076 (6)
O50.0284 (7)0.0465 (9)0.0439 (9)0.0115 (7)0.0051 (6)0.0116 (7)
O60.0224 (6)0.0143 (6)0.0193 (6)0.0003 (5)0.0048 (5)0.0004 (5)
O70.0209 (6)0.0155 (6)0.0219 (6)0.0024 (5)0.0063 (5)0.0014 (5)
O80.0286 (6)0.0151 (6)0.0194 (6)0.0034 (5)0.0088 (5)0.0023 (5)
O90.0383 (7)0.0200 (6)0.0281 (7)0.0032 (6)0.0090 (6)0.0074 (5)
O100.0401 (8)0.0234 (7)0.0397 (8)0.0024 (6)0.0229 (7)0.0100 (6)
O110.0582 (10)0.0314 (8)0.0284 (7)0.0217 (7)0.0035 (7)0.0045 (6)
P10.0217 (2)0.0164 (2)0.0153 (2)0.00067 (16)0.00582 (16)0.00060 (16)
P20.0205 (2)0.0132 (2)0.01642 (19)0.00155 (15)0.00628 (15)0.00047 (15)
Rh10.02171 (7)0.01364 (7)0.01554 (7)0.00143 (5)0.00610 (5)0.00137 (5)
Geometric parameters (Å, º) top
C1—C21.381 (3)C39—H390.9500
C1—C61.392 (3)C40—C411.489 (2)
C1—O11.400 (2)C41—C461.387 (2)
C2—C31.383 (3)C41—C421.401 (2)
C2—H20.9500C42—C431.377 (2)
C3—C41.382 (3)C42—H420.9500
C3—H30.9500C43—O101.373 (2)
C4—C51.383 (3)C43—C441.388 (3)
C4—H40.9500C44—C451.391 (2)
C5—C61.396 (3)C44—H440.9500
C5—H50.9500C45—C461.408 (2)
C6—C71.483 (3)C45—C531.537 (2)
C7—C121.392 (3)C46—O71.399 (2)
C7—C81.395 (3)C47—C491.529 (3)
C8—C91.386 (3)C47—C481.536 (3)
C8—H80.9500C47—C501.537 (3)
C9—C101.370 (4)C48—H48A0.9800
C9—H90.9500C48—H48B0.9800
C10—C111.389 (3)C48—H48C0.9800
C10—H100.9500C49—H49A0.9800
C11—C121.389 (3)C49—H49B0.9800
C11—H110.9500C49—H49C0.9800
C12—H120.9500C50—H50A0.9800
C13—C181.386 (3)C50—H50B0.9800
C13—C141.407 (2)C50—H50C0.9800
C13—O21.411 (2)C51—O91.427 (3)
C14—C151.386 (3)C51—H51A0.9800
C14—C251.543 (3)C51—H51B0.9800
C15—C161.389 (3)C51—H51C0.9800
C15—H150.9500C52—O101.422 (2)
C16—O41.373 (2)C52—H52A0.9800
C16—C171.380 (3)C52—H52B0.9800
C17—C181.402 (2)C52—H52C0.9800
C17—H170.9500C53—C551.527 (3)
C18—C191.491 (2)C53—C561.531 (3)
C19—C241.395 (2)C53—C541.535 (3)
C19—C201.398 (3)C54—H54A0.9800
C20—C211.382 (3)C54—H54B0.9800
C20—H200.9500C54—H54C0.9800
C21—O51.366 (2)C55—H55A0.9800
C21—C221.391 (3)C55—H55B0.9800
C22—C231.382 (3)C55—H55C0.9800
C22—H220.9500C56—H56A0.9800
C23—C241.409 (2)C56—H56B0.9800
C23—C311.539 (3)C56—H56C0.9800
C24—O31.402 (2)C57—O111.143 (2)
C25—C271.528 (3)C57—Rh11.8057 (19)
C25—C261.530 (3)C58—C591.3900
C25—C281.538 (3)C58—C631.3900
C26—H26A0.9800C58—C641.472 (4)
C26—H26B0.9800C59—C601.3900
C26—H26C0.9800C59—H590.9500
C27—H27A0.9800C60—C611.3900
C27—H27B0.9800C60—H600.9500
C27—H27C0.9800C61—C621.3900
C28—H28A0.9800C61—H610.9500
C28—H28B0.9800C62—C631.3900
C28—H28C0.9800C62—H620.9500
C29—O41.411 (2)C63—H630.9500
C29—H29A0.9800C64—H64A0.9800
C29—H29B0.9800C64—H64B0.9800
C29—H29C0.9800C64—H64C0.9800
C30—O51.425 (3)C65—C661.3900
C30—H30A0.9800C65—C701.3900
C30—H30B0.9800C65—C711.492 (3)
C30—H30C0.9800C66—C671.3900
C31—C331.525 (3)C66—H660.9500
C31—C321.529 (3)C67—C681.3900
C31—C341.537 (3)C67—H670.9500
C32—H32A0.9800C68—C691.3900
C32—H32B0.9800C68—H680.9500
C32—H32C0.9800C69—C701.3900
C33—H33A0.9800C69—H690.9500
C33—H33B0.9800C70—H700.9500
C33—H33C0.9800C71—H71A0.9800
C34—H34A0.9800C71—H71B0.9800
C34—H34B0.9800C71—H71C0.9800
C34—H34C0.9800O1—P11.5999 (13)
C35—C401.388 (2)O2—P11.5976 (12)
C35—O61.399 (2)O3—P11.6157 (13)
C35—C361.407 (2)O6—P21.6393 (13)
C36—C371.390 (3)O7—P21.6217 (12)
C36—C471.543 (3)O8—P21.5081 (12)
C37—C381.392 (3)O8—Rh1i2.0710 (12)
C37—H370.9500P1—Rh12.2906 (4)
C38—O91.367 (2)P2—Rh12.3049 (4)
C38—C391.382 (2)Rh1—O8i2.0711 (12)
C39—C401.399 (2)
C2—C1—C6122.00 (17)C43—C42—C41118.93 (17)
C2—C1—O1121.74 (16)C43—C42—H42120.5
C6—C1—O1116.20 (16)C41—C42—H42120.5
C1—C2—C3119.42 (18)O10—C43—C42124.42 (17)
C1—C2—H2120.3O10—C43—C44115.35 (16)
C3—C2—H2120.3C42—C43—C44120.23 (17)
C4—C3—C2120.3 (2)C43—C44—C45122.50 (16)
C4—C3—H3119.9C43—C44—H44118.7
C2—C3—H3119.9C45—C44—H44118.7
C3—C4—C5119.4 (2)C44—C45—C46116.12 (16)
C3—C4—H4120.3C44—C45—C53120.70 (15)
C5—C4—H4120.3C46—C45—C53123.15 (15)
C4—C5—C6121.78 (19)C41—C46—O7117.70 (14)
C4—C5—H5119.1C41—C46—C45121.73 (15)
C6—C5—H5119.1O7—C46—C45120.21 (15)
C1—C6—C5117.08 (18)C49—C47—C48109.71 (17)
C1—C6—C7123.20 (17)C49—C47—C50107.67 (17)
C5—C6—C7119.70 (17)C48—C47—C50107.21 (17)
C12—C7—C8118.9 (2)C49—C47—C36112.74 (16)
C12—C7—C6121.40 (17)C48—C47—C36107.97 (15)
C8—C7—C6119.61 (19)C50—C47—C36111.41 (16)
C9—C8—C7120.2 (2)C47—C48—H48A109.5
C9—C8—H8119.9C47—C48—H48B109.5
C7—C8—H8119.9H48A—C48—H48B109.5
C10—C9—C8120.6 (2)C47—C48—H48C109.5
C10—C9—H9119.7H48A—C48—H48C109.5
C8—C9—H9119.7H48B—C48—H48C109.5
C9—C10—C11120.1 (2)C47—C49—H49A109.5
C9—C10—H10120.0C47—C49—H49B109.5
C11—C10—H10120.0H49A—C49—H49B109.5
C10—C11—C12119.7 (2)C47—C49—H49C109.5
C10—C11—H11120.1H49A—C49—H49C109.5
C12—C11—H11120.1H49B—C49—H49C109.5
C11—C12—C7120.5 (2)C47—C50—H50A109.5
C11—C12—H12119.7C47—C50—H50B109.5
C7—C12—H12119.7H50A—C50—H50B109.5
C18—C13—C14122.73 (16)C47—C50—H50C109.5
C18—C13—O2117.61 (15)H50A—C50—H50C109.5
C14—C13—O2119.25 (15)H50B—C50—H50C109.5
C15—C14—C13115.79 (17)O9—C51—H51A109.5
C15—C14—C25120.03 (16)O9—C51—H51B109.5
C13—C14—C25123.99 (16)H51A—C51—H51B109.5
C14—C15—C16122.64 (17)O9—C51—H51C109.5
C14—C15—H15118.7H51A—C51—H51C109.5
C16—C15—H15118.7H51B—C51—H51C109.5
O4—C16—C17124.70 (17)O10—C52—H52A109.5
O4—C16—C15115.14 (16)O10—C52—H52B109.5
C17—C16—C15120.13 (17)H52A—C52—H52B109.5
C16—C17—C18119.28 (17)O10—C52—H52C109.5
C16—C17—H17120.4H52A—C52—H52C109.5
C18—C17—H17120.4H52B—C52—H52C109.5
C13—C18—C17119.01 (16)C55—C53—C56111.18 (18)
C13—C18—C19123.40 (15)C55—C53—C54107.22 (16)
C17—C18—C19117.38 (16)C56—C53—C54106.48 (17)
C24—C19—C20119.12 (16)C55—C53—C45109.93 (16)
C24—C19—C18123.38 (16)C56—C53—C45110.40 (16)
C20—C19—C18117.44 (16)C54—C53—C45111.55 (15)
C21—C20—C19119.26 (18)C53—C54—H54A109.5
C21—C20—H20120.4C53—C54—H54B109.5
C19—C20—H20120.4H54A—C54—H54B109.5
O5—C21—C20124.53 (19)C53—C54—H54C109.5
O5—C21—C22115.29 (18)H54A—C54—H54C109.5
C20—C21—C22120.19 (18)H54B—C54—H54C109.5
C23—C22—C21122.70 (17)C53—C55—H55A109.5
C23—C22—H22118.7C53—C55—H55B109.5
C21—C22—H22118.7H55A—C55—H55B109.5
C22—C23—C24115.96 (17)C53—C55—H55C109.5
C22—C23—C31120.39 (17)H55A—C55—H55C109.5
C24—C23—C31123.59 (17)H55B—C55—H55C109.5
C19—C24—O3116.57 (15)C53—C56—H56A109.5
C19—C24—C23122.43 (17)C53—C56—H56B109.5
O3—C24—C23120.80 (16)H56A—C56—H56B109.5
C27—C25—C26109.77 (17)C53—C56—H56C109.5
C27—C25—C28106.94 (17)H56A—C56—H56C109.5
C26—C25—C28107.82 (18)H56B—C56—H56C109.5
C27—C25—C14112.75 (16)O11—C57—Rh1177.9 (2)
C26—C25—C14108.25 (16)C59—C58—C63120.0
C28—C25—C14111.19 (16)C59—C58—C64120.2 (2)
C25—C26—H26A109.5C63—C58—C64119.8 (2)
C25—C26—H26B109.5C60—C59—C58120.0
H26A—C26—H26B109.5C60—C59—H59120.0
C25—C26—H26C109.5C58—C59—H59120.0
H26A—C26—H26C109.5C59—C60—C61120.0
H26B—C26—H26C109.5C59—C60—H60120.0
C25—C27—H27A109.5C61—C60—H60120.0
C25—C27—H27B109.5C62—C61—C60120.0
H27A—C27—H27B109.5C62—C61—H61120.0
C25—C27—H27C109.5C60—C61—H61120.0
H27A—C27—H27C109.5C61—C62—C63120.0
H27B—C27—H27C109.5C61—C62—H62120.0
C25—C28—H28A109.5C63—C62—H62120.0
C25—C28—H28B109.5C62—C63—C58120.0
H28A—C28—H28B109.5C62—C63—H63120.0
C25—C28—H28C109.5C58—C63—H63120.0
H28A—C28—H28C109.5C58—C64—H64A109.5
H28B—C28—H28C109.5C58—C64—H64B109.5
O4—C29—H29A109.5H64A—C64—H64B109.5
O4—C29—H29B109.5C58—C64—H64C109.5
H29A—C29—H29B109.5H64A—C64—H64C109.5
O4—C29—H29C109.5H64B—C64—H64C109.5
H29A—C29—H29C109.5C66—C65—C70120.0
H29B—C29—H29C109.5C66—C65—C71119.52 (19)
O5—C30—H30A109.5C70—C65—C71120.47 (19)
O5—C30—H30B109.5C65—C66—C67120.0
H30A—C30—H30B109.5C65—C66—H66120.0
O5—C30—H30C109.5C67—C66—H66120.0
H30A—C30—H30C109.5C68—C67—C66120.0
H30B—C30—H30C109.5C68—C67—H67120.0
C33—C31—C32110.5 (2)C66—C67—H67120.0
C33—C31—C34107.35 (19)C69—C68—C67120.0
C32—C31—C34106.89 (17)C69—C68—H68120.0
C33—C31—C23109.79 (17)C67—C68—H68120.0
C32—C31—C23111.18 (17)C68—C69—C70120.0
C34—C31—C23111.05 (18)C68—C69—H69120.0
C31—C32—H32A109.5C70—C69—H69120.0
C31—C32—H32B109.5C69—C70—C65120.0
H32A—C32—H32B109.5C69—C70—H70120.0
C31—C32—H32C109.5C65—C70—H70120.0
H32A—C32—H32C109.5C65—C71—H71A109.5
H32B—C32—H32C109.5C65—C71—H71B109.5
C31—C33—H33A109.5H71A—C71—H71B109.5
C31—C33—H33B109.5C65—C71—H71C109.5
H33A—C33—H33B109.5H71A—C71—H71C109.5
C31—C33—H33C109.5H71B—C71—H71C109.5
H33A—C33—H33C109.5C1—O1—P1126.22 (11)
H33B—C33—H33C109.5C13—O2—P1124.26 (11)
C31—C34—H34A109.5C24—O3—P1120.71 (11)
C31—C34—H34B109.5C16—O4—C29117.31 (15)
H34A—C34—H34B109.5C21—O5—C30116.40 (17)
C31—C34—H34C109.5C35—O6—P2116.77 (10)
H34A—C34—H34C109.5C46—O7—P2126.12 (11)
H34B—C34—H34C109.5P2—O8—Rh1i140.28 (7)
C40—C35—O6117.37 (15)C38—O9—C51117.38 (15)
C40—C35—C36122.00 (16)C43—O10—C52116.63 (15)
O6—C35—C36120.50 (15)O2—P1—O1101.63 (7)
C37—C36—C35116.15 (16)O2—P1—O3105.08 (7)
C37—C36—C47121.14 (16)O1—P1—O397.10 (7)
C35—C36—C47122.34 (16)O2—P1—Rh1107.40 (5)
C36—C37—C38122.28 (17)O1—P1—Rh1123.27 (5)
C36—C37—H37118.9O3—P1—Rh1119.82 (5)
C38—C37—H37118.9O8—P2—O7107.83 (7)
O9—C38—C39124.45 (17)O8—P2—O6101.89 (7)
O9—C38—C37115.45 (16)O7—P2—O6102.46 (6)
C39—C38—C37120.06 (17)O8—P2—Rh1121.95 (5)
C38—C39—C40119.16 (17)O7—P2—Rh1106.81 (5)
C38—C39—H39120.4O6—P2—Rh1114.16 (5)
C40—C39—H39120.4C57—Rh1—O8i178.25 (7)
C35—C40—C39119.49 (16)C57—Rh1—P187.14 (6)
C35—C40—C41121.36 (15)O8i—Rh1—P192.36 (3)
C39—C40—C41118.95 (15)C57—Rh1—P287.55 (6)
C46—C41—C42119.95 (15)O8i—Rh1—P293.00 (3)
C46—C41—C40122.74 (15)P1—Rh1—P2174.350 (16)
C42—C41—C40117.31 (16)
C6—C1—C2—C30.0 (3)C38—C39—C40—C41174.31 (16)
O1—C1—C2—C3177.22 (18)C35—C40—C41—C4654.6 (2)
C1—C2—C3—C40.9 (3)C39—C40—C41—C46130.68 (18)
C2—C3—C4—C50.6 (3)C35—C40—C41—C42125.56 (18)
C3—C4—C5—C60.6 (4)C39—C40—C41—C4249.2 (2)
C2—C1—C6—C51.1 (3)C46—C41—C42—C430.6 (3)
O1—C1—C6—C5176.24 (17)C40—C41—C42—C43179.59 (17)
C2—C1—C6—C7177.06 (18)C41—C42—C43—O10174.92 (18)
O1—C1—C6—C75.6 (3)C41—C42—C43—C445.0 (3)
C4—C5—C6—C11.4 (3)O10—C43—C44—C45176.86 (17)
C4—C5—C6—C7176.8 (2)C42—C43—C44—C453.1 (3)
C1—C6—C7—C1259.9 (3)C43—C44—C45—C463.3 (3)
C5—C6—C7—C12118.2 (2)C43—C44—C45—C53174.90 (18)
C1—C6—C7—C8124.3 (2)C42—C41—C46—O7179.21 (15)
C5—C6—C7—C857.5 (3)C40—C41—C46—O70.6 (2)
C12—C7—C8—C90.4 (3)C42—C41—C46—C456.1 (3)
C6—C7—C8—C9175.45 (19)C40—C41—C46—C45173.78 (16)
C7—C8—C9—C100.3 (3)C44—C45—C46—C417.8 (3)
C8—C9—C10—C110.4 (4)C53—C45—C46—C41170.31 (17)
C9—C10—C11—C120.4 (3)C44—C45—C46—O7179.22 (15)
C10—C11—C12—C71.1 (3)C53—C45—C46—O72.7 (3)
C8—C7—C12—C111.2 (3)C37—C36—C47—C49123.2 (2)
C6—C7—C12—C11174.64 (19)C35—C36—C47—C4964.0 (2)
C18—C13—C14—C156.5 (3)C37—C36—C47—C48115.40 (19)
O2—C13—C14—C15178.99 (16)C35—C36—C47—C4857.3 (2)
C18—C13—C14—C25168.51 (17)C37—C36—C47—C502.1 (2)
O2—C13—C14—C253.9 (3)C35—C36—C47—C50174.80 (18)
C13—C14—C15—C161.5 (3)C44—C45—C53—C55111.1 (2)
C25—C14—C15—C16173.73 (18)C46—C45—C53—C5570.9 (2)
C14—C15—C16—O4178.17 (18)C44—C45—C53—C56125.9 (2)
C14—C15—C16—C173.7 (3)C46—C45—C53—C5652.1 (2)
O4—C16—C17—C18177.94 (18)C44—C45—C53—C547.7 (3)
C15—C16—C17—C184.1 (3)C46—C45—C53—C54170.29 (18)
C14—C13—C18—C176.2 (3)C63—C58—C59—C600.0
O2—C13—C18—C17178.77 (16)C64—C58—C59—C60179.6 (3)
C14—C13—C18—C19168.40 (17)C58—C59—C60—C610.0
O2—C13—C18—C194.2 (3)C59—C60—C61—C620.0
C16—C17—C18—C130.6 (3)C60—C61—C62—C630.0
C16—C17—C18—C19174.28 (17)C61—C62—C63—C580.0
C13—C18—C19—C2452.2 (3)C59—C58—C63—C620.0
C17—C18—C19—C24133.16 (19)C64—C58—C63—C62179.6 (3)
C13—C18—C19—C20130.61 (19)C70—C65—C66—C670.0
C17—C18—C19—C2044.1 (2)C71—C65—C66—C67179.1 (3)
C24—C19—C20—C210.3 (3)C65—C66—C67—C680.0
C18—C19—C20—C21177.09 (17)C66—C67—C68—C690.0
C19—C20—C21—O5176.43 (18)C67—C68—C69—C700.0
C19—C20—C21—C223.8 (3)C68—C69—C70—C650.0
O5—C21—C22—C23177.17 (18)C66—C65—C70—C690.0
C20—C21—C22—C233.0 (3)C71—C65—C70—C69179.1 (3)
C21—C22—C23—C241.8 (3)C2—C1—O1—P126.3 (2)
C21—C22—C23—C31175.35 (18)C6—C1—O1—P1156.39 (14)
C20—C19—C24—O3179.79 (15)C18—C13—O2—P163.9 (2)
C18—C19—C24—O33.0 (2)C14—C13—O2—P1123.26 (15)
C20—C19—C24—C235.4 (3)C19—C24—O3—P169.83 (18)
C18—C19—C24—C23171.83 (17)C23—C24—O3—P1115.23 (16)
C22—C23—C24—C196.0 (3)C17—C16—O4—C2911.4 (3)
C31—C23—C24—C19171.03 (17)C15—C16—O4—C29170.62 (19)
C22—C23—C24—O3179.34 (16)C20—C21—O5—C306.4 (3)
C31—C23—C24—O33.6 (3)C22—C21—O5—C30173.3 (2)
C15—C14—C25—C27126.3 (2)C40—C35—O6—P271.52 (17)
C13—C14—C25—C2758.9 (2)C36—C35—O6—P2112.59 (15)
C15—C14—C25—C26112.1 (2)C41—C46—O7—P263.4 (2)
C13—C14—C25—C2662.7 (2)C45—C46—O7—P2123.33 (15)
C15—C14—C25—C286.2 (3)C39—C38—O9—C510.8 (3)
C13—C14—C25—C28178.99 (19)C37—C38—O9—C51177.12 (17)
C22—C23—C31—C33124.4 (2)C42—C43—O10—C525.2 (3)
C24—C23—C31—C3352.6 (3)C44—C43—O10—C52174.89 (19)
C22—C23—C31—C32113.1 (2)C13—O2—P1—O161.60 (14)
C24—C23—C31—C3270.0 (2)C13—O2—P1—O339.12 (14)
C22—C23—C31—C345.8 (3)C13—O2—P1—Rh1167.75 (12)
C24—C23—C31—C34171.14 (19)C1—O1—P1—O2160.96 (13)
C40—C35—C36—C379.9 (3)C1—O1—P1—O353.90 (14)
O6—C35—C36—C37174.39 (15)C1—O1—P1—Rh179.02 (14)
C40—C35—C36—C47163.16 (17)C24—O3—P1—O249.52 (13)
O6—C35—C36—C4712.5 (3)C24—O3—P1—O1153.65 (12)
C35—C36—C37—C383.4 (3)C24—O3—P1—Rh171.24 (13)
C47—C36—C37—C38169.73 (17)Rh1i—O8—P2—O7156.08 (11)
C36—C37—C38—O9177.68 (16)Rh1i—O8—P2—O696.51 (12)
C36—C37—C38—C394.3 (3)Rh1i—O8—P2—Rh132.11 (15)
O9—C38—C39—C40176.40 (16)C46—O7—P2—O878.92 (14)
C37—C38—C39—C405.8 (3)C46—O7—P2—O628.10 (14)
O6—C35—C40—C39175.53 (15)C46—O7—P2—Rh1148.40 (12)
C36—C35—C40—C398.6 (3)C35—O6—P2—O8172.30 (11)
O6—C35—C40—C419.8 (2)C35—O6—P2—O760.77 (12)
C36—C35—C40—C41166.06 (16)C35—O6—P2—Rh154.30 (12)
C38—C39—C40—C350.5 (3)
Symmetry code: (i) x, y+2, z.
 

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