Molecules of the title compound, [Rh(C9H6NO){(C14H21O)3P}(CO)]·0.5(CH3)2CO, where (C9H6NO) = 8-hydroxyquinolinato and {(C14H21O)3P} = tris(2,4-di-tert-butylphenyl)phosphite, pack in a tail-to-tail fashion with an intermolecular quinoline ligand-to-ligand π-stacking distance of 3.312 (1) Å. The effective cone angle (ΘE) for the phosphite ligand is 192°. The bidentate oxine ligand has a bite angle of 81.00 (8)° and the Rh—P bond length is 2.1819 (6) Å.
Supporting information
CCDC reference: 627319
Key indicators
- Single-crystal X-ray study
- T = 150 K
- Mean (C-C) = 0.004 Å
- Disorder in solvent or counterion
- R factor = 0.039
- wR factor = 0.130
- Data-to-parameter ratio = 22.2
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ?
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 0.50 Ratio
PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.36
PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.18 Ratio
PLAT220_ALERT_2_C Large Non-Solvent O Ueq(max)/Ueq(min) ... 2.55 Ratio
PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.41 Ratio
PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.08
PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 25.00 Perc.
PLAT601_ALERT_2_C Structure Contains Solvent Accessible VOIDS of . 41.00 A 3
Alert level G
FORMU01_ALERT_1_G There is a discrepancy between the atom counts in the
_chemical_formula_sum and _chemical_formula_moiety. This is
usually due to the moiety formula being in the wrong format.
Atom count from _chemical_formula_sum: C53.5 H72 N1 O5.5 P1 Rh1
Atom count from _chemical_formula_moiety:
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
10 ALERT level C = Check and explain
1 ALERT level G = General alerts; check
4 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
5 ALERT type 2 Indicator that the structure model may be wrong or deficient
1 ALERT type 3 Indicator that the structure quality may be low
1 ALERT type 4 Improvement, methodology, query or suggestion
0 ALERT type 5 Informative message, check
Data collection: Apex2 (Bruker, 2005); cell refinement: SAINT-Plus (Bruker, 2004); data reduction: SAINT-Plus; program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg & Putz, 2005); software used to prepare material for publication: WinGX (Farrugia, 1999).
Carbonyl[tris(2,4-di-
tert-butylphenyl)phosphite](8-hydroxyquinolinato)
rhodium(I) acetone hemisolvate
top
Crystal data top
[Rh(C9H6NO){(C14H21O)3P}(CO)]·0.5C3H6O | F(000) = 4032 |
Mr = 951 | Dx = 1.175 Mg m−3 |
Orthorhombic, Pccn | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ab 2ac | Cell parameters from 7476 reflections |
a = 34.945 (5) Å | θ = 2.3–27.7° |
b = 17.307 (5) Å | µ = 0.39 mm−1 |
c = 17.778 (5) Å | T = 150 K |
V = 10752 (5) Å3 | Block, yellow |
Z = 8 | 0.3 × 0.28 × 0.21 mm |
Data collection top
Bruker X8 ApexII CCD diffractometer | 13332 independent reflections |
Radiation source: fine-focus sealed tube | 10688 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.043 |
ω and φ scans | θmax = 28.3°, θmin = 1.2° |
Absorption correction: multi-scan (SADABS; Bruker, 2004) | h = −45→46 |
Tmin = 0.892, Tmax = 0.922 | k = −20→23 |
86538 measured reflections | l = −23→23 |
Refinement top
Refinement on F2 | 6 restraints |
Least-squares matrix: full | H-atom parameters constrained |
R[F2 > 2σ(F2)] = 0.039 | w = 1/[σ2(Fo2) + (0.0709P)2 + 8.2813P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.130 | (Δ/σ)max = 0.002 |
S = 1.07 | Δρmax = 1.14 e Å−3 |
13332 reflections | Δρmin = −0.48 e Å−3 |
600 parameters | |
Special details top
Experimental. The intensity data was collected on a Bruker X8 Apex II 4 K Kappa CCD
diffractometer using an exposure time of 10 s/frame. A total of 1125 frames
were collected with a frame width of 0.5° covering up to θ = 28.0° with
100% completeness accomplished. |
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell e.s.d.'s are taken
into account individually in the estimation of e.s.d.'s in distances, angles
and torsion angles; correlations between e.s.d.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s.
planes. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Rh | 0.424373 (5) | 0.033301 (10) | 0.144019 (10) | 0.02034 (7) | |
P | 0.369749 (15) | −0.00206 (3) | 0.19249 (3) | 0.01656 (11) | |
N | 0.47385 (6) | 0.06700 (12) | 0.08734 (11) | 0.0256 (4) | |
O1 | 0.36793 (4) | −0.07805 (9) | 0.24404 (8) | 0.0184 (3) | |
O2 | 0.34904 (4) | 0.05015 (9) | 0.25486 (8) | 0.0204 (3) | |
O3 | 0.33881 (4) | −0.01596 (9) | 0.12782 (8) | 0.0183 (3) | |
O4 | 0.40017 (5) | 0.07404 (11) | 0.04853 (10) | 0.0324 (4) | |
O5 | 0.46625 (6) | −0.03168 (13) | 0.27429 (12) | 0.0467 (5) | |
C1 | 0.51004 (7) | 0.06073 (16) | 0.10770 (15) | 0.0316 (5) | |
H1 | 0.5157 | 0.0422 | 0.1556 | 0.038* | |
C2 | 0.54035 (8) | 0.08093 (16) | 0.05978 (17) | 0.0379 (6) | |
H2 | 0.5656 | 0.0764 | 0.0758 | 0.046* | |
C3 | 0.53236 (8) | 0.10698 (16) | −0.00967 (17) | 0.0391 (7) | |
H3 | 0.5523 | 0.1205 | −0.0417 | 0.047* | |
C4 | 0.49434 (8) | 0.11427 (15) | −0.03500 (16) | 0.0360 (6) | |
C5 | 0.48318 (10) | 0.13708 (19) | −0.10809 (18) | 0.0492 (8) | |
H5 | 0.5015 | 0.1512 | −0.1435 | 0.059* | |
C6 | 0.44525 (11) | 0.1382 (2) | −0.12614 (18) | 0.0547 (9) | |
H6 | 0.4382 | 0.1531 | −0.1745 | 0.066* | |
C7 | 0.41610 (10) | 0.11768 (19) | −0.07477 (17) | 0.0441 (7) | |
H7 | 0.3906 | 0.1192 | −0.0896 | 0.053* | |
C8 | 0.42560 (7) | 0.09532 (15) | −0.00249 (15) | 0.0316 (5) | |
C9 | 0.46522 (7) | 0.09387 (14) | 0.01664 (15) | 0.0301 (5) | |
C10 | 0.44919 (7) | −0.00647 (16) | 0.22511 (14) | 0.0293 (5) | |
C11 | 0.38862 (6) | −0.14544 (12) | 0.22824 (12) | 0.0174 (4) | |
C12 | 0.40013 (6) | −0.19175 (13) | 0.28920 (12) | 0.0190 (4) | |
C13 | 0.42247 (6) | −0.25557 (13) | 0.27062 (13) | 0.0219 (4) | |
H13 | 0.4313 | −0.2866 | 0.3096 | 0.026* | |
C14 | 0.43251 (6) | −0.27610 (13) | 0.19692 (13) | 0.0219 (4) | |
C15 | 0.41823 (6) | −0.23090 (13) | 0.13955 (12) | 0.0208 (4) | |
H15 | 0.4234 | −0.2441 | 0.0899 | 0.025* | |
C16 | 0.39619 (6) | −0.16577 (13) | 0.15497 (12) | 0.0186 (4) | |
H16 | 0.3866 | −0.136 | 0.1157 | 0.022* | |
C21 | 0.33962 (6) | 0.12834 (12) | 0.24597 (12) | 0.0199 (4) | |
C22 | 0.33843 (6) | 0.17500 (13) | 0.31064 (12) | 0.0219 (4) | |
C23 | 0.32617 (7) | 0.25056 (13) | 0.29940 (13) | 0.0245 (5) | |
H23 | 0.3251 | 0.283 | 0.3411 | 0.029* | |
C24 | 0.31537 (7) | 0.28116 (13) | 0.22976 (13) | 0.0246 (5) | |
C25 | 0.31803 (8) | 0.23292 (14) | 0.16785 (14) | 0.0292 (5) | |
H25 | 0.3117 | 0.2516 | 0.1204 | 0.035* | |
C26 | 0.33017 (7) | 0.15689 (14) | 0.17598 (13) | 0.0271 (5) | |
H26 | 0.3319 | 0.1251 | 0.134 | 0.033* | |
C31 | 0.30192 (6) | −0.04769 (12) | 0.13120 (12) | 0.0171 (4) | |
C32 | 0.28317 (6) | −0.06078 (12) | 0.06263 (11) | 0.0176 (4) | |
C33 | 0.24701 (6) | −0.09385 (12) | 0.06801 (12) | 0.0197 (4) | |
H33 | 0.2337 | −0.1029 | 0.0236 | 0.024* | |
C34 | 0.22935 (6) | −0.11438 (13) | 0.13564 (12) | 0.0193 (4) | |
C35 | 0.24899 (6) | −0.09912 (13) | 0.20151 (12) | 0.0202 (4) | |
H35 | 0.238 | −0.1116 | 0.2476 | 0.024* | |
C36 | 0.28500 (6) | −0.06537 (13) | 0.19944 (12) | 0.0194 (4) | |
H36 | 0.2978 | −0.0546 | 0.2441 | 0.023* | |
C121 | 0.38749 (7) | −0.17576 (14) | 0.37054 (12) | 0.0226 (4) | |
C122 | 0.34346 (7) | −0.17556 (17) | 0.37427 (14) | 0.0313 (5) | |
H12D | 0.3338 | −0.2242 | 0.3564 | 0.047* | |
H12E | 0.3337 | −0.1346 | 0.3434 | 0.047* | |
H12F | 0.3354 | −0.1678 | 0.4254 | 0.047* | |
C123 | 0.40335 (8) | −0.09795 (15) | 0.39843 (14) | 0.0315 (5) | |
H12G | 0.3952 | −0.0893 | 0.4493 | 0.047* | |
H12H | 0.394 | −0.0571 | 0.3669 | 0.047* | |
H12I | 0.4308 | −0.0989 | 0.3965 | 0.047* | |
C124 | 0.40158 (8) | −0.23832 (16) | 0.42436 (14) | 0.0327 (6) | |
H12A | 0.3915 | −0.2875 | 0.4091 | 0.049* | |
H12B | 0.393 | −0.2268 | 0.4744 | 0.049* | |
H12C | 0.429 | −0.24 | 0.4234 | 0.049* | |
C141 | 0.45818 (7) | −0.34663 (15) | 0.18299 (14) | 0.0293 (5) | |
C142 | 0.43893 (8) | −0.41933 (15) | 0.21416 (16) | 0.0357 (6) | |
H14G | 0.4339 | −0.4125 | 0.2668 | 0.054* | |
H14H | 0.4556 | −0.4629 | 0.2072 | 0.054* | |
H14I | 0.4153 | −0.4282 | 0.188 | 0.054* | |
C143 | 0.49685 (7) | −0.33218 (17) | 0.22240 (17) | 0.0370 (6) | |
H14A | 0.5086 | −0.2867 | 0.2018 | 0.056* | |
H14B | 0.5133 | −0.3758 | 0.2146 | 0.056* | |
H14C | 0.4927 | −0.325 | 0.2753 | 0.056* | |
C144 | 0.46588 (10) | −0.3592 (2) | 0.09924 (16) | 0.0502 (8) | |
H14D | 0.4423 | −0.3711 | 0.0741 | 0.075* | |
H14E | 0.4835 | −0.4013 | 0.093 | 0.075* | |
H14F | 0.4767 | −0.3131 | 0.078 | 0.075* | |
C221 | 0.34997 (8) | 0.14491 (14) | 0.38870 (13) | 0.0275 (5) | |
C222 | 0.39247 (8) | 0.12372 (17) | 0.38798 (17) | 0.0397 (6) | |
H22G | 0.3972 | 0.0869 | 0.3487 | 0.06* | |
H22H | 0.3994 | 0.1016 | 0.4356 | 0.06* | |
H22I | 0.4074 | 0.1693 | 0.3792 | 0.06* | |
C223 | 0.32531 (9) | 0.07527 (16) | 0.41135 (14) | 0.0367 (6) | |
H22A | 0.2987 | 0.0891 | 0.4086 | 0.055* | |
H22B | 0.3315 | 0.0601 | 0.4618 | 0.055* | |
H22C | 0.3303 | 0.033 | 0.3777 | 0.055* | |
C224 | 0.34448 (10) | 0.20674 (17) | 0.45013 (15) | 0.0434 (7) | |
H22D | 0.3602 | 0.2508 | 0.4389 | 0.065* | |
H22E | 0.3517 | 0.1858 | 0.498 | 0.065* | |
H22F | 0.3181 | 0.2222 | 0.4517 | 0.065* | |
C241 | 0.30091 (7) | 0.36482 (14) | 0.22478 (14) | 0.0281 (5) | |
C242 | 0.33288 (8) | 0.42021 (15) | 0.24880 (16) | 0.0368 (6) | |
H24G | 0.3411 | 0.4076 | 0.2989 | 0.055* | |
H24H | 0.3235 | 0.4723 | 0.2477 | 0.055* | |
H24I | 0.3541 | 0.4154 | 0.2148 | 0.055* | |
C243 | 0.26637 (8) | 0.37486 (15) | 0.27730 (15) | 0.0333 (6) | |
H24A | 0.2463 | 0.3403 | 0.2622 | 0.05* | |
H24B | 0.2574 | 0.4272 | 0.2745 | 0.05* | |
H24C | 0.2739 | 0.3634 | 0.328 | 0.05* | |
C244 | 0.28833 (10) | 0.38609 (16) | 0.14441 (15) | 0.0425 (7) | |
H24D | 0.3097 | 0.3809 | 0.1108 | 0.064* | |
H24E | 0.2793 | 0.4385 | 0.1436 | 0.064* | |
H24F | 0.2681 | 0.3521 | 0.1287 | 0.064* | |
C321 | 0.30038 (7) | −0.03819 (13) | −0.01390 (12) | 0.0221 (4) | |
C322 | 0.33906 (7) | −0.07795 (16) | −0.02720 (14) | 0.0319 (6) | |
H32D | 0.3575 | −0.0585 | 0.008 | 0.048* | |
H32E | 0.3476 | −0.0675 | −0.0775 | 0.048* | |
H32F | 0.3363 | −0.1327 | −0.0204 | 0.048* | |
C323 | 0.30552 (8) | 0.04976 (15) | −0.01789 (14) | 0.0306 (5) | |
H32A | 0.325 | 0.0654 | 0.017 | 0.046* | |
H32B | 0.2818 | 0.0746 | −0.0052 | 0.046* | |
H32C | 0.3129 | 0.0642 | −0.0679 | 0.046* | |
C324 | 0.27391 (8) | −0.06116 (18) | −0.07909 (13) | 0.0343 (6) | |
H32G | 0.2851 | −0.0451 | −0.1259 | 0.051* | |
H32H | 0.2495 | −0.0366 | −0.0728 | 0.051* | |
H32I | 0.2706 | −0.1162 | −0.0793 | 0.051* | |
C341 | 0.18999 (6) | −0.15331 (14) | 0.13420 (13) | 0.0225 (4) | |
C342 | 0.17545 (7) | −0.17148 (17) | 0.21320 (14) | 0.0324 (6) | |
H34G | 0.1929 | −0.2063 | 0.2376 | 0.049* | |
H34H | 0.1506 | −0.195 | 0.21 | 0.049* | |
H34I | 0.1737 | −0.1245 | 0.2418 | 0.049* | |
C343 | 0.19289 (7) | −0.22968 (14) | 0.09027 (15) | 0.0295 (5) | |
H34A | 0.2026 | −0.2196 | 0.0407 | 0.044* | |
H34B | 0.168 | −0.2528 | 0.0866 | 0.044* | |
H34C | 0.2099 | −0.2642 | 0.1161 | 0.044* | |
C344 | 0.16090 (7) | −0.09981 (15) | 0.09566 (14) | 0.0282 (5) | |
H34D | 0.1587 | −0.0526 | 0.1237 | 0.042* | |
H34E | 0.1364 | −0.1249 | 0.0937 | 0.042* | |
H34F | 0.1694 | −0.0885 | 0.0455 | 0.042* | |
C40A | 0.4759 (2) | 0.1840 (6) | 0.5904 (6) | 0.0378 (14) | 0.301 (3) |
H40A | 0.4901 | 0.1365 | 0.5905 | 0.057* | 0.301 (3) |
H40B | 0.4869 | 0.2191 | 0.6261 | 0.057* | 0.301 (3) |
H40C | 0.4767 | 0.2065 | 0.5411 | 0.057* | 0.301 (3) |
C41A | 0.4215 (5) | 0.2420 (9) | 0.6470 (7) | 0.0378 (14) | 0.301 (3) |
H41A | 0.4044 | 0.2688 | 0.6137 | 0.057* | 0.301 (3) |
H41B | 0.4439 | 0.2728 | 0.6552 | 0.057* | 0.301 (3) |
H41C | 0.4089 | 0.233 | 0.6942 | 0.057* | 0.301 (3) |
C42A | 0.4326 (3) | 0.1669 (7) | 0.6129 (6) | 0.0378 (14) | 0.301 (3) |
O6A | 0.4130 (3) | 0.1122 (5) | 0.6087 (5) | 0.068 (2) | 0.301 (3) |
C40B | 0.4641 (4) | 0.1836 (10) | 0.5621 (8) | 0.0378 (14) | 0.199 (3) |
H40D | 0.4717 | 0.1332 | 0.5453 | 0.057* | 0.199 (3) |
H40E | 0.4864 | 0.2152 | 0.5692 | 0.057* | 0.199 (3) |
H40F | 0.4477 | 0.2069 | 0.5251 | 0.057* | 0.199 (3) |
C41B | 0.4205 (7) | 0.2424 (14) | 0.6645 (12) | 0.0378 (14) | 0.199 (3) |
H41D | 0.3967 | 0.2236 | 0.6847 | 0.057* | 0.199 (3) |
H41E | 0.4153 | 0.2783 | 0.6245 | 0.057* | 0.199 (3) |
H41F | 0.4347 | 0.2679 | 0.7034 | 0.057* | 0.199 (3) |
C42B | 0.4431 (4) | 0.1767 (10) | 0.6348 (8) | 0.0378 (14) | 0.199 (3) |
O6B | 0.4375 (4) | 0.1196 (7) | 0.6694 (8) | 0.068 (2) | 0.199 (3) |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Rh | 0.01890 (10) | 0.02238 (10) | 0.01974 (10) | −0.00549 (6) | 0.00165 (6) | 0.00041 (7) |
P | 0.0172 (2) | 0.0169 (3) | 0.0156 (3) | −0.00137 (19) | 0.00040 (19) | 0.0007 (2) |
N | 0.0266 (10) | 0.0242 (10) | 0.0260 (10) | −0.0085 (8) | 0.0061 (8) | −0.0048 (8) |
O1 | 0.0202 (7) | 0.0181 (7) | 0.0167 (7) | 0.0010 (6) | 0.0013 (6) | 0.0018 (6) |
O2 | 0.0267 (8) | 0.0175 (7) | 0.0170 (7) | 0.0017 (6) | 0.0016 (6) | −0.0002 (6) |
O3 | 0.0169 (7) | 0.0221 (7) | 0.0160 (7) | −0.0040 (6) | −0.0004 (6) | 0.0014 (6) |
O4 | 0.0280 (9) | 0.0416 (11) | 0.0276 (9) | −0.0043 (8) | 0.0012 (7) | 0.0105 (8) |
O5 | 0.0340 (10) | 0.0632 (15) | 0.0430 (12) | −0.0134 (9) | −0.0121 (9) | 0.0193 (10) |
C1 | 0.0282 (12) | 0.0331 (13) | 0.0336 (13) | −0.0100 (10) | 0.0044 (10) | −0.0082 (11) |
C2 | 0.0298 (13) | 0.0343 (14) | 0.0497 (17) | −0.0117 (11) | 0.0094 (12) | −0.0098 (13) |
C3 | 0.0377 (14) | 0.0281 (13) | 0.0513 (17) | −0.0095 (11) | 0.0220 (13) | −0.0061 (12) |
C4 | 0.0453 (15) | 0.0246 (12) | 0.0381 (14) | −0.0056 (11) | 0.0172 (12) | 0.0006 (11) |
C5 | 0.061 (2) | 0.0446 (17) | 0.0419 (17) | −0.0003 (15) | 0.0231 (15) | 0.0155 (14) |
C6 | 0.073 (2) | 0.056 (2) | 0.0342 (16) | 0.0048 (18) | 0.0111 (16) | 0.0224 (15) |
C7 | 0.0523 (17) | 0.0459 (17) | 0.0339 (15) | 0.0020 (14) | 0.0037 (13) | 0.0142 (13) |
C8 | 0.0381 (14) | 0.0277 (13) | 0.0288 (13) | −0.0017 (10) | 0.0068 (10) | 0.0048 (10) |
C9 | 0.0369 (13) | 0.0214 (11) | 0.0321 (13) | −0.0057 (10) | 0.0105 (10) | −0.0003 (10) |
C10 | 0.0218 (11) | 0.0367 (13) | 0.0293 (13) | −0.0124 (10) | −0.0006 (9) | 0.0059 (11) |
C11 | 0.0153 (9) | 0.0158 (9) | 0.0212 (10) | −0.0013 (7) | −0.0009 (7) | 0.0007 (8) |
C12 | 0.0199 (10) | 0.0200 (10) | 0.0171 (10) | −0.0020 (8) | −0.0017 (8) | 0.0009 (8) |
C13 | 0.0236 (11) | 0.0218 (11) | 0.0204 (10) | 0.0015 (8) | −0.0034 (8) | 0.0037 (9) |
C14 | 0.0212 (10) | 0.0222 (11) | 0.0222 (11) | 0.0024 (8) | −0.0006 (8) | −0.0004 (9) |
C15 | 0.0215 (10) | 0.0225 (11) | 0.0183 (10) | −0.0014 (8) | 0.0008 (8) | −0.0025 (8) |
C16 | 0.0174 (10) | 0.0212 (10) | 0.0171 (10) | −0.0017 (8) | −0.0012 (7) | 0.0023 (8) |
C21 | 0.0226 (10) | 0.0165 (10) | 0.0206 (10) | −0.0002 (8) | 0.0020 (8) | 0.0003 (8) |
C22 | 0.0249 (11) | 0.0217 (11) | 0.0192 (10) | −0.0019 (8) | 0.0007 (8) | −0.0002 (9) |
C23 | 0.0317 (12) | 0.0202 (11) | 0.0217 (11) | −0.0008 (9) | 0.0031 (9) | −0.0040 (9) |
C24 | 0.0307 (12) | 0.0186 (10) | 0.0246 (11) | 0.0003 (9) | 0.0026 (9) | 0.0016 (9) |
C25 | 0.0453 (14) | 0.0238 (12) | 0.0185 (10) | 0.0057 (10) | 0.0017 (10) | 0.0023 (9) |
C26 | 0.0409 (13) | 0.0218 (11) | 0.0186 (11) | 0.0043 (10) | 0.0015 (10) | −0.0020 (9) |
C31 | 0.0162 (9) | 0.0166 (9) | 0.0185 (10) | 0.0001 (7) | −0.0002 (7) | 0.0012 (8) |
C32 | 0.0213 (10) | 0.0161 (9) | 0.0155 (10) | 0.0008 (8) | −0.0005 (8) | 0.0005 (8) |
C33 | 0.0217 (10) | 0.0210 (10) | 0.0163 (10) | −0.0005 (8) | −0.0026 (8) | −0.0015 (8) |
C34 | 0.0182 (10) | 0.0191 (10) | 0.0207 (10) | 0.0006 (8) | −0.0005 (8) | 0.0003 (8) |
C35 | 0.0204 (10) | 0.0246 (11) | 0.0157 (9) | −0.0006 (8) | 0.0017 (8) | 0.0015 (8) |
C36 | 0.0204 (10) | 0.0226 (10) | 0.0153 (10) | −0.0009 (8) | −0.0005 (8) | −0.0001 (8) |
C121 | 0.0273 (11) | 0.0251 (11) | 0.0154 (10) | 0.0007 (9) | −0.0007 (8) | 0.0015 (9) |
C122 | 0.0315 (13) | 0.0424 (15) | 0.0200 (11) | 0.0016 (11) | 0.0054 (9) | 0.0040 (11) |
C123 | 0.0432 (14) | 0.0307 (13) | 0.0207 (11) | −0.0023 (11) | −0.0028 (10) | −0.0034 (10) |
C124 | 0.0449 (15) | 0.0350 (14) | 0.0181 (11) | 0.0054 (11) | −0.0008 (10) | 0.0063 (10) |
C141 | 0.0310 (12) | 0.0291 (12) | 0.0277 (12) | 0.0112 (10) | −0.0019 (10) | −0.0009 (10) |
C142 | 0.0380 (14) | 0.0256 (13) | 0.0434 (15) | 0.0074 (11) | −0.0097 (12) | −0.0027 (11) |
C143 | 0.0267 (12) | 0.0364 (14) | 0.0480 (16) | 0.0080 (11) | 0.0000 (11) | 0.0087 (13) |
C144 | 0.066 (2) | 0.0520 (19) | 0.0326 (15) | 0.0326 (16) | 0.0085 (14) | −0.0033 (14) |
C221 | 0.0412 (14) | 0.0233 (11) | 0.0181 (11) | 0.0012 (10) | −0.0023 (10) | −0.0003 (9) |
C222 | 0.0430 (16) | 0.0366 (15) | 0.0395 (15) | 0.0008 (12) | −0.0156 (12) | 0.0008 (13) |
C223 | 0.0549 (17) | 0.0319 (14) | 0.0232 (12) | −0.0017 (12) | 0.0069 (11) | 0.0051 (11) |
C224 | 0.077 (2) | 0.0332 (15) | 0.0203 (12) | 0.0040 (14) | −0.0052 (13) | −0.0049 (11) |
C241 | 0.0394 (13) | 0.0188 (11) | 0.0262 (12) | 0.0039 (10) | 0.0026 (10) | 0.0015 (9) |
C242 | 0.0465 (15) | 0.0219 (12) | 0.0420 (15) | −0.0031 (11) | 0.0047 (12) | 0.0008 (11) |
C243 | 0.0374 (14) | 0.0256 (12) | 0.0368 (14) | 0.0070 (10) | 0.0011 (11) | −0.0013 (11) |
C244 | 0.071 (2) | 0.0253 (13) | 0.0314 (14) | 0.0142 (13) | −0.0055 (13) | 0.0029 (11) |
C321 | 0.0261 (11) | 0.0263 (11) | 0.0137 (10) | −0.0005 (9) | −0.0006 (8) | 0.0010 (8) |
C322 | 0.0360 (13) | 0.0388 (14) | 0.0210 (11) | 0.0057 (11) | 0.0097 (10) | 0.0012 (10) |
C323 | 0.0411 (14) | 0.0282 (12) | 0.0224 (12) | −0.0028 (10) | −0.0003 (10) | 0.0082 (10) |
C324 | 0.0388 (14) | 0.0483 (16) | 0.0157 (11) | −0.0102 (12) | −0.0022 (10) | 0.0002 (11) |
C341 | 0.0198 (10) | 0.0237 (11) | 0.0240 (11) | −0.0040 (8) | −0.0013 (8) | 0.0002 (9) |
C342 | 0.0263 (12) | 0.0421 (15) | 0.0288 (13) | −0.0124 (11) | 0.0028 (10) | 0.0030 (11) |
C343 | 0.0257 (11) | 0.0254 (12) | 0.0372 (14) | −0.0052 (9) | −0.0004 (10) | −0.0046 (10) |
C344 | 0.0213 (11) | 0.0302 (13) | 0.0331 (13) | 0.0009 (9) | −0.0036 (9) | −0.0036 (10) |
C40A | 0.028 (2) | 0.047 (2) | 0.039 (4) | 0.0012 (19) | 0.002 (2) | 0.013 (3) |
C41A | 0.028 (2) | 0.047 (2) | 0.039 (4) | 0.0012 (19) | 0.002 (2) | 0.013 (3) |
C42A | 0.028 (2) | 0.047 (2) | 0.039 (4) | 0.0012 (19) | 0.002 (2) | 0.013 (3) |
O6A | 0.100 (6) | 0.036 (3) | 0.066 (5) | 0.011 (4) | 0.040 (4) | 0.008 (4) |
C40B | 0.028 (2) | 0.047 (2) | 0.039 (4) | 0.0012 (19) | 0.002 (2) | 0.013 (3) |
C41B | 0.028 (2) | 0.047 (2) | 0.039 (4) | 0.0012 (19) | 0.002 (2) | 0.013 (3) |
C42B | 0.028 (2) | 0.047 (2) | 0.039 (4) | 0.0012 (19) | 0.002 (2) | 0.013 (3) |
O6B | 0.100 (6) | 0.036 (3) | 0.066 (5) | 0.011 (4) | 0.040 (4) | 0.008 (4) |
Geometric parameters (Å, º) top
Rh—C10 | 1.818 (3) | C141—C143 | 1.543 (4) |
Rh—O4 | 2.0234 (18) | C142—H14G | 0.96 |
Rh—N | 2.0842 (19) | C142—H14H | 0.96 |
Rh—P | 2.1819 (6) | C142—H14I | 0.96 |
P—O3 | 1.5965 (16) | C143—H14A | 0.96 |
P—O2 | 1.6030 (16) | C143—H14B | 0.96 |
P—O1 | 1.6042 (16) | C143—H14C | 0.96 |
N—C1 | 1.320 (3) | C144—H14D | 0.96 |
N—C9 | 1.374 (3) | C144—H14E | 0.96 |
O1—C11 | 1.401 (2) | C144—H14F | 0.96 |
O2—C21 | 1.402 (3) | C221—C222 | 1.530 (4) |
O3—C31 | 1.402 (2) | C221—C223 | 1.535 (4) |
O4—C8 | 1.322 (3) | C221—C224 | 1.541 (3) |
O5—C10 | 1.145 (3) | C222—H22G | 0.96 |
C1—C2 | 1.404 (4) | C222—H22H | 0.96 |
C1—H1 | 0.93 | C222—H22I | 0.96 |
C2—C3 | 1.344 (4) | C223—H22A | 0.96 |
C2—H2 | 0.93 | C223—H22B | 0.96 |
C3—C4 | 1.409 (4) | C223—H22C | 0.96 |
C3—H3 | 0.93 | C224—H22D | 0.96 |
C4—C5 | 1.413 (4) | C224—H22E | 0.96 |
C4—C9 | 1.415 (3) | C224—H22F | 0.96 |
C5—C6 | 1.364 (5) | C241—C242 | 1.533 (4) |
C5—H5 | 0.93 | C241—C243 | 1.536 (4) |
C6—C7 | 1.413 (4) | C241—C244 | 1.540 (4) |
C6—H6 | 0.93 | C242—H24G | 0.96 |
C7—C8 | 1.382 (4) | C242—H24H | 0.96 |
C7—H7 | 0.93 | C242—H24I | 0.96 |
C8—C9 | 1.426 (4) | C243—H24A | 0.96 |
C11—C16 | 1.375 (3) | C243—H24B | 0.96 |
C11—C12 | 1.407 (3) | C243—H24C | 0.96 |
C12—C13 | 1.392 (3) | C244—H24D | 0.96 |
C12—C121 | 1.537 (3) | C244—H24E | 0.96 |
C13—C14 | 1.402 (3) | C244—H24F | 0.96 |
C13—H13 | 0.93 | C321—C323 | 1.534 (3) |
C14—C15 | 1.379 (3) | C321—C322 | 1.535 (3) |
C14—C141 | 1.535 (3) | C321—C324 | 1.535 (3) |
C15—C16 | 1.392 (3) | C322—H32D | 0.96 |
C15—H15 | 0.93 | C322—H32E | 0.96 |
C16—H16 | 0.93 | C322—H32F | 0.96 |
C21—C26 | 1.379 (3) | C323—H32A | 0.96 |
C21—C22 | 1.406 (3) | C323—H32B | 0.96 |
C22—C23 | 1.391 (3) | C323—H32C | 0.96 |
C22—C221 | 1.536 (3) | C324—H32G | 0.96 |
C23—C24 | 1.398 (3) | C324—H32H | 0.96 |
C23—H23 | 0.93 | C324—H32I | 0.96 |
C24—C25 | 1.385 (3) | C341—C342 | 1.526 (3) |
C24—C241 | 1.536 (3) | C341—C344 | 1.536 (3) |
C25—C26 | 1.390 (3) | C341—C343 | 1.539 (3) |
C25—H25 | 0.93 | C342—H34G | 0.96 |
C26—H26 | 0.93 | C342—H34H | 0.96 |
C31—C36 | 1.384 (3) | C342—H34I | 0.96 |
C31—C32 | 1.402 (3) | C343—H34A | 0.96 |
C32—C33 | 1.390 (3) | C343—H34B | 0.96 |
C32—C321 | 1.538 (3) | C343—H34C | 0.96 |
C33—C34 | 1.397 (3) | C344—H34D | 0.96 |
C33—H33 | 0.93 | C344—H34E | 0.96 |
C34—C35 | 1.383 (3) | C344—H34F | 0.96 |
C34—C341 | 1.532 (3) | C40A—C42A | 1.592 (11) |
C35—C36 | 1.388 (3) | C40A—H40A | 0.96 |
C35—H35 | 0.93 | C40A—H40B | 0.96 |
C36—H36 | 0.93 | C40A—H40C | 0.96 |
C121—C124 | 1.527 (3) | C41A—C42A | 1.487 (13) |
C121—C123 | 1.538 (3) | C41A—H41A | 0.96 |
C121—C122 | 1.540 (3) | C41A—H41B | 0.96 |
C122—H12D | 0.96 | C41A—H41C | 0.96 |
C122—H12E | 0.96 | C42A—O6A | 1.171 (14) |
C122—H12F | 0.96 | C40B—C42B | 1.491 (15) |
C123—H12G | 0.96 | C40B—H40D | 0.96 |
C123—H12H | 0.96 | C40B—H40E | 0.96 |
C123—H12I | 0.96 | C40B—H40F | 0.96 |
C124—H12A | 0.96 | C41B—C42B | 1.482 (16) |
C124—H12B | 0.96 | C41B—H41D | 0.96 |
C124—H12C | 0.96 | C41B—H41E | 0.96 |
C141—C144 | 1.529 (4) | C41B—H41F | 0.96 |
C141—C142 | 1.530 (4) | C42B—O6B | 1.18 (2) |
| | | |
C10—Rh—O4 | 175.38 (10) | C141—C142—H14H | 109.5 |
C10—Rh—N | 95.37 (9) | H14G—C142—H14H | 109.5 |
O4—Rh—N | 81.00 (8) | C141—C142—H14I | 109.5 |
C10—Rh—P | 89.88 (7) | H14G—C142—H14I | 109.5 |
O4—Rh—P | 93.64 (5) | H14H—C142—H14I | 109.5 |
N—Rh—P | 174.30 (6) | C141—C143—H14A | 109.5 |
O3—P—O2 | 106.10 (8) | C141—C143—H14B | 109.5 |
O3—P—O1 | 105.13 (8) | H14A—C143—H14B | 109.5 |
O2—P—O1 | 92.81 (8) | C141—C143—H14C | 109.5 |
O3—P—Rh | 110.51 (6) | H14A—C143—H14C | 109.5 |
O2—P—Rh | 120.66 (6) | H14B—C143—H14C | 109.5 |
O1—P—Rh | 119.36 (6) | C141—C144—H14D | 109.5 |
C1—N—C9 | 119.3 (2) | C141—C144—H14E | 109.5 |
C1—N—Rh | 129.74 (18) | H14D—C144—H14E | 109.5 |
C9—N—Rh | 110.80 (16) | C141—C144—H14F | 109.5 |
C11—O1—P | 123.20 (13) | H14D—C144—H14F | 109.5 |
C21—O2—P | 124.90 (14) | H14E—C144—H14F | 109.5 |
C31—O3—P | 130.60 (14) | C222—C221—C223 | 111.0 (2) |
C8—O4—Rh | 113.06 (16) | C222—C221—C22 | 109.2 (2) |
N—C1—C2 | 122.4 (3) | C223—C221—C22 | 110.8 (2) |
N—C1—H1 | 118.8 | C222—C221—C224 | 107.0 (2) |
C2—C1—H1 | 118.8 | C223—C221—C224 | 106.8 (2) |
C3—C2—C1 | 119.0 (3) | C22—C221—C224 | 111.9 (2) |
C3—C2—H2 | 120.5 | C221—C222—H22G | 109.5 |
C1—C2—H2 | 120.5 | C221—C222—H22H | 109.5 |
C2—C3—C4 | 121.3 (2) | H22G—C222—H22H | 109.5 |
C2—C3—H3 | 119.3 | C221—C222—H22I | 109.5 |
C4—C3—H3 | 119.3 | H22G—C222—H22I | 109.5 |
C3—C4—C5 | 125.4 (3) | H22H—C222—H22I | 109.5 |
C3—C4—C9 | 116.6 (3) | C221—C223—H22A | 109.5 |
C5—C4—C9 | 117.9 (3) | C221—C223—H22B | 109.5 |
C6—C5—C4 | 119.3 (3) | H22A—C223—H22B | 109.5 |
C6—C5—H5 | 120.4 | C221—C223—H22C | 109.5 |
C4—C5—H5 | 120.4 | H22A—C223—H22C | 109.5 |
C5—C6—C7 | 123.0 (3) | H22B—C223—H22C | 109.5 |
C5—C6—H6 | 118.5 | C221—C224—H22D | 109.5 |
C7—C6—H6 | 118.5 | C221—C224—H22E | 109.5 |
C8—C7—C6 | 119.9 (3) | H22D—C224—H22E | 109.5 |
C8—C7—H7 | 120.1 | C221—C224—H22F | 109.5 |
C6—C7—H7 | 120.1 | H22D—C224—H22F | 109.5 |
O4—C8—C7 | 123.7 (3) | H22E—C224—H22F | 109.5 |
O4—C8—C9 | 119.0 (2) | C242—C241—C243 | 109.4 (2) |
C7—C8—C9 | 117.4 (2) | C242—C241—C24 | 109.5 (2) |
N—C9—C4 | 121.4 (2) | C243—C241—C24 | 109.3 (2) |
N—C9—C8 | 115.9 (2) | C242—C241—C244 | 108.5 (2) |
C4—C9—C8 | 122.6 (3) | C243—C241—C244 | 108.2 (2) |
O5—C10—Rh | 177.0 (2) | C24—C241—C244 | 111.9 (2) |
C16—C11—O1 | 120.15 (19) | C241—C242—H24G | 109.5 |
C16—C11—C12 | 121.9 (2) | C241—C242—H24H | 109.5 |
O1—C11—C12 | 117.87 (19) | H24G—C242—H24H | 109.5 |
C13—C12—C11 | 115.4 (2) | C241—C242—H24I | 109.5 |
C13—C12—C121 | 121.81 (19) | H24G—C242—H24I | 109.5 |
C11—C12—C121 | 122.7 (2) | H24H—C242—H24I | 109.5 |
C12—C13—C14 | 124.3 (2) | C241—C243—H24A | 109.5 |
C12—C13—H13 | 117.9 | C241—C243—H24B | 109.5 |
C14—C13—H13 | 117.9 | H24A—C243—H24B | 109.5 |
C15—C14—C13 | 117.2 (2) | C241—C243—H24C | 109.5 |
C15—C14—C141 | 122.9 (2) | H24A—C243—H24C | 109.5 |
C13—C14—C141 | 119.9 (2) | H24B—C243—H24C | 109.5 |
C14—C15—C16 | 120.9 (2) | C241—C244—H24D | 109.5 |
C14—C15—H15 | 119.5 | C241—C244—H24E | 109.5 |
C16—C15—H15 | 119.5 | H24D—C244—H24E | 109.5 |
C11—C16—C15 | 120.0 (2) | C241—C244—H24F | 109.5 |
C11—C16—H16 | 120 | H24D—C244—H24F | 109.5 |
C15—C16—H16 | 120 | H24E—C244—H24F | 109.5 |
C26—C21—O2 | 120.27 (19) | C323—C321—C322 | 109.5 (2) |
C26—C21—C22 | 121.7 (2) | C323—C321—C324 | 107.0 (2) |
O2—C21—C22 | 117.99 (19) | C322—C321—C324 | 107.3 (2) |
C23—C22—C21 | 115.6 (2) | C323—C321—C32 | 109.81 (18) |
C23—C22—C221 | 122.0 (2) | C322—C321—C32 | 111.51 (18) |
C21—C22—C221 | 122.4 (2) | C324—C321—C32 | 111.48 (19) |
C22—C23—C24 | 124.5 (2) | C321—C322—H32D | 109.5 |
C22—C23—H23 | 117.7 | C321—C322—H32E | 109.5 |
C24—C23—H23 | 117.7 | H32D—C322—H32E | 109.5 |
C25—C24—C23 | 117.2 (2) | C321—C322—H32F | 109.5 |
C25—C24—C241 | 123.0 (2) | H32D—C322—H32F | 109.5 |
C23—C24—C241 | 119.8 (2) | H32E—C322—H32F | 109.5 |
C24—C25—C26 | 120.6 (2) | C321—C323—H32A | 109.5 |
C24—C25—H25 | 119.7 | C321—C323—H32B | 109.5 |
C26—C25—H25 | 119.7 | H32A—C323—H32B | 109.5 |
C21—C26—C25 | 120.4 (2) | C321—C323—H32C | 109.5 |
C21—C26—H26 | 119.8 | H32A—C323—H32C | 109.5 |
C25—C26—H26 | 119.8 | H32B—C323—H32C | 109.5 |
C36—C31—O3 | 121.12 (19) | C321—C324—H32G | 109.5 |
C36—C31—C32 | 121.78 (19) | C321—C324—H32H | 109.5 |
O3—C31—C32 | 117.10 (18) | H32G—C324—H32H | 109.5 |
C33—C32—C31 | 115.55 (19) | C321—C324—H32I | 109.5 |
C33—C32—C321 | 121.40 (19) | H32G—C324—H32I | 109.5 |
C31—C32—C321 | 123.02 (19) | H32H—C324—H32I | 109.5 |
C32—C33—C34 | 124.42 (19) | C342—C341—C34 | 111.98 (19) |
C32—C33—H33 | 117.8 | C342—C341—C344 | 108.3 (2) |
C34—C33—H33 | 117.8 | C34—C341—C344 | 109.66 (19) |
C35—C34—C33 | 117.45 (19) | C342—C341—C343 | 108.2 (2) |
C35—C34—C341 | 122.94 (19) | C34—C341—C343 | 109.11 (19) |
C33—C34—C341 | 119.60 (19) | C344—C341—C343 | 109.57 (19) |
C34—C35—C36 | 120.5 (2) | C341—C342—H34G | 109.5 |
C34—C35—H35 | 119.7 | C341—C342—H34H | 109.5 |
C36—C35—H35 | 119.7 | H34G—C342—H34H | 109.5 |
C31—C36—C35 | 120.25 (19) | C341—C342—H34I | 109.5 |
C31—C36—H36 | 119.9 | H34G—C342—H34I | 109.5 |
C35—C36—H36 | 119.9 | H34H—C342—H34I | 109.5 |
C124—C121—C12 | 111.68 (19) | C341—C343—H34A | 109.5 |
C124—C121—C123 | 107.6 (2) | C341—C343—H34B | 109.5 |
C12—C121—C123 | 110.93 (19) | H34A—C343—H34B | 109.5 |
C124—C121—C122 | 107.3 (2) | C341—C343—H34C | 109.5 |
C12—C121—C122 | 109.15 (18) | H34A—C343—H34C | 109.5 |
C123—C121—C122 | 110.1 (2) | H34B—C343—H34C | 109.5 |
C121—C122—H12D | 109.5 | C341—C344—H34D | 109.5 |
C121—C122—H12E | 109.5 | C341—C344—H34E | 109.5 |
H12D—C122—H12E | 109.5 | H34D—C344—H34E | 109.5 |
C121—C122—H12F | 109.5 | C341—C344—H34F | 109.5 |
H12D—C122—H12F | 109.5 | H34D—C344—H34F | 109.5 |
H12E—C122—H12F | 109.5 | H34E—C344—H34F | 109.5 |
C121—C123—H12G | 109.5 | O6A—C42A—C41A | 125.4 (11) |
C121—C123—H12H | 109.5 | O6A—C42A—C40A | 133.7 (11) |
H12G—C123—H12H | 109.5 | C41A—C42A—C40A | 100.9 (10) |
C121—C123—H12I | 109.5 | C42B—C40B—H40D | 109.5 |
H12G—C123—H12I | 109.5 | C42B—C40B—H40E | 109.5 |
H12H—C123—H12I | 109.5 | H40D—C40B—H40E | 109.5 |
C121—C124—H12A | 109.5 | C42B—C40B—H40F | 109.5 |
C121—C124—H12B | 109.5 | H40D—C40B—H40F | 109.5 |
H12A—C124—H12B | 109.5 | H40E—C40B—H40F | 109.5 |
C121—C124—H12C | 109.5 | C42B—C41B—H41D | 109.5 |
H12A—C124—H12C | 109.5 | C42B—C41B—H41E | 109.5 |
H12B—C124—H12C | 109.5 | H41D—C41B—H41E | 109.5 |
C144—C141—C142 | 108.2 (2) | C42B—C41B—H41F | 109.5 |
C144—C141—C14 | 111.9 (2) | H41D—C41B—H41F | 109.5 |
C142—C141—C14 | 109.8 (2) | H41E—C41B—H41F | 109.5 |
C144—C141—C143 | 108.1 (2) | O6B—C42B—C41B | 111.7 (14) |
C142—C141—C143 | 110.7 (2) | O6B—C42B—C40B | 126.9 (16) |
C14—C141—C143 | 108.0 (2) | C41B—C42B—C40B | 120.6 (14) |
C141—C142—H14G | 109.5 | | |
| | | |
C10—Rh—P—O3 | −153.46 (11) | C26—C21—C22—C23 | 1.7 (3) |
O4—Rh—P—O3 | 23.54 (9) | O2—C21—C22—C23 | −175.38 (19) |
C10—Rh—P—O2 | 82.07 (11) | C26—C21—C22—C221 | −178.2 (2) |
O4—Rh—P—O2 | −100.94 (9) | O2—C21—C22—C221 | 4.8 (3) |
C10—Rh—P—O1 | −31.45 (11) | C21—C22—C23—C24 | 0.1 (3) |
O4—Rh—P—O1 | 145.55 (9) | C221—C22—C23—C24 | 179.9 (2) |
C10—Rh—N—C1 | −0.9 (2) | C22—C23—C24—C25 | −1.6 (4) |
O4—Rh—N—C1 | −178.0 (2) | C22—C23—C24—C241 | 177.8 (2) |
C10—Rh—N—C9 | 173.82 (18) | C23—C24—C25—C26 | 1.4 (4) |
O4—Rh—N—C9 | −3.28 (16) | C241—C24—C25—C26 | −178.0 (2) |
O3—P—O1—C11 | 85.52 (16) | O2—C21—C26—C25 | 175.1 (2) |
O2—P—O1—C11 | −166.97 (15) | C22—C21—C26—C25 | −1.9 (4) |
Rh—P—O1—C11 | −39.12 (17) | C24—C25—C26—C21 | 0.2 (4) |
O3—P—O2—C21 | −71.23 (18) | P—O3—C31—C36 | 7.2 (3) |
O1—P—O2—C21 | −177.86 (17) | P—O3—C31—C32 | −172.61 (15) |
Rh—P—O2—C21 | 55.29 (18) | C36—C31—C32—C33 | −1.2 (3) |
O2—P—O3—C31 | −56.34 (19) | O3—C31—C32—C33 | 178.63 (18) |
O1—P—O3—C31 | 41.18 (19) | C36—C31—C32—C321 | 177.0 (2) |
Rh—P—O3—C31 | 171.23 (16) | O3—C31—C32—C321 | −3.2 (3) |
N—Rh—O4—C8 | 4.60 (18) | C31—C32—C33—C34 | −0.5 (3) |
P—Rh—O4—C8 | −173.45 (17) | C321—C32—C33—C34 | −178.7 (2) |
C9—N—C1—C2 | 0.3 (4) | C32—C33—C34—C35 | 1.4 (3) |
Rh—N—C1—C2 | 174.70 (19) | C32—C33—C34—C341 | −177.7 (2) |
N—C1—C2—C3 | −0.6 (4) | C33—C34—C35—C36 | −0.6 (3) |
C1—C2—C3—C4 | 0.0 (4) | C341—C34—C35—C36 | 178.4 (2) |
C2—C3—C4—C5 | −176.4 (3) | O3—C31—C36—C35 | −177.84 (19) |
C2—C3—C4—C9 | 0.9 (4) | C32—C31—C36—C35 | 2.0 (3) |
C3—C4—C5—C6 | 176.9 (3) | C34—C35—C36—C31 | −1.0 (3) |
C9—C4—C5—C6 | −0.4 (5) | C13—C12—C121—C124 | −1.4 (3) |
C4—C5—C6—C7 | 0.2 (6) | C11—C12—C121—C124 | 175.6 (2) |
C5—C6—C7—C8 | 0.1 (6) | C13—C12—C121—C123 | 118.7 (2) |
Rh—O4—C8—C7 | 173.3 (2) | C11—C12—C121—C123 | −64.3 (3) |
Rh—O4—C8—C9 | −5.3 (3) | C13—C12—C121—C122 | −119.8 (2) |
C6—C7—C8—O4 | −178.8 (3) | C11—C12—C121—C122 | 57.2 (3) |
C6—C7—C8—C9 | −0.2 (4) | C15—C14—C141—C144 | 0.5 (4) |
C1—N—C9—C4 | 0.6 (4) | C13—C14—C141—C144 | −179.9 (2) |
Rh—N—C9—C4 | −174.78 (19) | C15—C14—C141—C142 | −119.7 (2) |
C1—N—C9—C8 | 177.0 (2) | C13—C14—C141—C142 | 59.9 (3) |
Rh—N—C9—C8 | 1.6 (3) | C15—C14—C141—C143 | 119.5 (2) |
C3—C4—C9—N | −1.2 (4) | C13—C14—C141—C143 | −60.9 (3) |
C5—C4—C9—N | 176.3 (2) | C23—C22—C221—C222 | −115.8 (3) |
C3—C4—C9—C8 | −177.3 (2) | C21—C22—C221—C222 | 64.0 (3) |
C5—C4—C9—C8 | 0.2 (4) | C23—C22—C221—C223 | 121.5 (2) |
O4—C8—C9—N | 2.4 (4) | C21—C22—C221—C223 | −58.6 (3) |
C7—C8—C9—N | −176.2 (2) | C23—C22—C221—C224 | 2.4 (3) |
O4—C8—C9—C4 | 178.7 (2) | C21—C22—C221—C224 | −177.7 (2) |
C7—C8—C9—C4 | 0.1 (4) | C25—C24—C241—C242 | −117.7 (3) |
P—O1—C11—C16 | −31.9 (3) | C23—C24—C241—C242 | 62.9 (3) |
P—O1—C11—C12 | 149.89 (16) | C25—C24—C241—C243 | 122.4 (3) |
C16—C11—C12—C13 | 5.4 (3) | C23—C24—C241—C243 | −56.9 (3) |
O1—C11—C12—C13 | −176.45 (18) | C25—C24—C241—C244 | 2.6 (4) |
C16—C11—C12—C121 | −171.8 (2) | C23—C24—C241—C244 | −176.8 (2) |
O1—C11—C12—C121 | 6.4 (3) | C33—C32—C321—C323 | 115.2 (2) |
C11—C12—C13—C14 | −2.0 (3) | C31—C32—C321—C323 | −62.9 (3) |
C121—C12—C13—C14 | 175.2 (2) | C33—C32—C321—C322 | −123.2 (2) |
C12—C13—C14—C15 | −1.9 (3) | C31—C32—C321—C322 | 58.7 (3) |
C12—C13—C14—C141 | 178.4 (2) | C33—C32—C321—C324 | −3.3 (3) |
C13—C14—C15—C16 | 2.8 (3) | C31—C32—C321—C324 | 178.7 (2) |
C141—C14—C15—C16 | −177.6 (2) | C35—C34—C341—C342 | 0.8 (3) |
O1—C11—C16—C15 | 177.12 (18) | C33—C34—C341—C342 | 179.9 (2) |
C12—C11—C16—C15 | −4.8 (3) | C35—C34—C341—C344 | 121.1 (2) |
C14—C15—C16—C11 | 0.4 (3) | C33—C34—C341—C344 | −59.9 (3) |
P—O2—C21—C26 | 31.7 (3) | C35—C34—C341—C343 | −118.9 (2) |
P—O2—C21—C22 | −151.18 (16) | C33—C34—C341—C343 | 60.1 (3) |
Comparative geometric data (Å, °) for
[Rh(OX)(CO)(PR3)] complexes. topPR3 | Rh—P | Rh—N | Rh—O | N—Rh—O | ΘE (°) | 1JRh—P (Hz) |
P(Obtbp)i | 2.182 (7) | 2.084 (2) | 2.023 (2) | 81.0 (1) | 192 | 279 |
P(OPh)3ii | 2.186 (1) | 2.097 (2) | 2.022 (2) | 80.8iii | 163 | 281 |
P(O2MP)3iv | 2.189 (1) | 2.088 (3) | 2.032 (3) | 81.2 (1) | 168 | 278 |
P(O2,6DMP)3v | 2.198 (1) | 2.091 (3) | 2.029 (3) | 80.3 (1) | 183 | 280 |
PPh3vi | 2.261 (2) | 2.098 (9) | 2.042 (5) | 80.0 (3) | 153 | 161 |
References and notes:
(i) this work, P(Obtbp) = tris(2,4-di-tert-butylphenyl)phosphite;
(ii) Simanko et al. (2000);
(iii) data extracted from the Cambridge Structural Database
(Version 5.26), no s.u. values (Allen, 2002);
(iv) Janse van Rensburg et al. (2005b);
(v) Janse van Rensburg et al. (2005a);
(vi) Leipoldt et al. (1981). |