The title compound, [Rh
2(C
28H
40O
3P)
2(C
2H
3N)
2(CO)
2]·∼1.5CH
2Cl
2, contains a dimeric rhodacyclic complex, having inversion symmetry. The Rh atoms are joined by bridging phosphites and additionally each is coordinated by a CO and an acetonitrile. Half of the
tert-butyl groups are rotationally disordered, but weak C—H
O interactions prevent this from occurring in the other two groups.
Supporting information
CCDC reference: 245136
Key indicators
- Single-crystal X-ray study
- T = 150 K
- Mean (C-C) = 0.006 Å
- R factor = 0.043
- wR factor = 0.098
- Data-to-parameter ratio = 17.9
checkCIF/PLATON results
No syntax errors found
Alert level A
PLAT601_ALERT_2_A Structure Contains Solvent Accessible VOIDS of . 377.00 A 3
| Author Response: See experimental section
|
Alert level B
PLAT201_ALERT_2_B Isotropic non-H Atoms in Main Residue(s) ....... 6
Alert level C
PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.69 Ratio
PLAT301_ALERT_3_C Main Residue Disorder ......................... 14.00 Perc.
1 ALERT level A = In general: serious problem
1 ALERT level B = Potentially serious problem
2 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
3 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
0 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: Collect (Nonius, 1998); cell refinement: DIRAX (Duisenberg, 1992); data reduction: HKL-2000 (Otwinowski & Minor, 1997); program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: PLATON (Spek, 2003); software used to prepare material for publication: PLATON.
{(carbonyl)(acetonitrilo)(µ
2-
O)(
P)(dibenzo-[d,f]-2,2,4,4-tetra-
tert-butyl- [1,3,2]dioxa-phosphito)}-rhodium(I)-dimer
~1.5
dichloromethane solvate
top
Crystal data top
[C62H86N2O8P2Rh2]1.5CH2Cl2 | F(000) = 2624 |
Mr = 1255.09 | Dx = 1.199 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 7134 reflections |
a = 29.2584 (4) Å | θ = 1.0–26.0° |
b = 12.4252 (2) Å | µ = 0.57 mm−1 |
c = 21.7240 (3) Å | T = 150 K |
β = 118.3548 (5)° | Needle, yellow |
V = 6950.05 (18) Å3 | 0.39 × 0.15 × 0.09 mm |
Z = 4 | |
Data collection top
Nonius KappaCCD diffractometer | 6085 independent reflections |
Radiation source: Rotating Anode | 4468 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.053 |
Detector resolution: 18.4 pixels mm-1 | θmax = 25.0°, θmin = 1.6° |
φ and ω scans | h = −34→34 |
Absorption correction: multi-scan (SADABS; Sheldrick, 1990) | k = −14→14 |
Tmin = 0.750, Tmax = 0.950 | l = −25→25 |
28137 measured reflections | |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.043 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.098 | H-atom parameters constrained |
S = 1.05 | w = 1/[σ2(Fo2) + (0.0431P)2 + 7.5648P] where P = (Fo2 + 2Fc2)/3 |
6085 reflections | (Δ/σ)max = 0.004 |
340 parameters | Δρmax = 0.68 e Å−3 |
72 restraints | Δρmin = −0.49 e Å−3 |
Special details top
Geometry. Bond distances, angles etc. have been calculated using the rounded
fractional coordinates. All su's are estimated from the variances of the
(full) variance-covariance matrix. The cell e.s.d.'s are taken into account in
the estimation of distances, angles and torsion angles |
Refinement. Refinement on F2 for ALL reflections except those flagged by the user
for potential systematic errors. Weighted R-factors wR
and all goodnesses of fit S are based on F2,
conventional R-factors R are based on F, with F
set to zero for negative F2. The observed criterion of F2 >
σ(F2) is used only for calculating -R-factor-obs
etc. and is not relevant to the choice of reflections for
refinement. R-factors based on F2 are statistically about
twice as large as those based on F, and R-factors based on ALL
data will be even larger. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Rh1 | 0.06582 (1) | 0.51980 (2) | 0.10396 (1) | 0.0245 (1) | |
P1 | 0.06371 (3) | 0.51557 (8) | 0.00106 (5) | 0.0239 (3) | |
O1 | 0.01229 (8) | 0.5151 (2) | −0.06492 (12) | 0.0307 (8) | |
O2 | 0.17690 (11) | 0.5792 (3) | 0.16739 (15) | 0.0560 (11) | |
O3 | 0.09280 (8) | 0.41436 (18) | −0.01457 (11) | 0.0252 (8) | |
O4 | 0.09740 (8) | 0.61748 (18) | −0.00192 (12) | 0.0261 (8) | |
N1 | 0.06688 (10) | 0.5281 (2) | 0.20205 (15) | 0.0267 (10) | |
C1 | 0.13352 (15) | 0.5541 (3) | 0.1417 (2) | 0.0354 (14) | |
C2 | 0.06809 (13) | 0.5423 (3) | 0.2540 (2) | 0.0289 (11) | |
C3 | 0.06957 (15) | 0.5616 (4) | 0.3214 (2) | 0.0424 (14) | |
C4 | 0.14565 (12) | 0.3957 (3) | 0.03120 (17) | 0.0242 (11) | |
C5 | 0.18136 (13) | 0.4680 (3) | 0.02949 (18) | 0.0268 (11) | |
C6 | 0.23421 (13) | 0.4507 (3) | 0.07499 (19) | 0.0282 (11) | |
C7 | 0.25157 (13) | 0.3641 (3) | 0.12039 (19) | 0.0305 (12) | |
C8 | 0.21435 (13) | 0.2905 (3) | 0.1171 (2) | 0.0319 (12) | |
C9 | 0.16100 (13) | 0.3015 (3) | 0.07208 (19) | 0.0273 (12) | |
C10 | 0.12480 (12) | 0.6265 (3) | −0.03951 (17) | 0.0252 (11) | |
C11 | 0.16614 (12) | 0.5562 (3) | −0.02352 (18) | 0.0252 (11) | |
C12 | 0.19559 (13) | 0.5697 (3) | −0.05784 (19) | 0.0275 (11) | |
C13 | 0.18562 (13) | 0.6510 (3) | −0.10648 (19) | 0.0304 (12) | |
C14 | 0.14482 (14) | 0.7210 (3) | −0.11920 (19) | 0.0316 (12) | |
C15 | 0.11371 (13) | 0.7123 (3) | −0.08699 (19) | 0.0288 (11) | |
C16 | 0.12314 (14) | 0.2095 (3) | 0.0632 (2) | 0.0347 (14) | |
C17 | 0.15116 (16) | 0.1150 (3) | 0.1130 (2) | 0.0538 (18) | |
C18 | 0.07875 (15) | 0.2439 (3) | 0.0772 (2) | 0.0463 (16) | |
C19 | 0.10086 (17) | 0.1669 (4) | −0.0117 (2) | 0.0535 (17) | |
C20 | 0.30991 (15) | 0.3472 (3) | 0.1708 (2) | 0.0423 (11) | |
C21A | 0.3211 (3) | 0.2540 (6) | 0.2182 (4) | 0.054 (2)* | 0.641 (5) |
C22A | 0.3327 (3) | 0.4492 (6) | 0.2141 (4) | 0.056 (2)* | 0.641 (5) |
C23A | 0.3369 (3) | 0.3342 (6) | 0.1242 (4) | 0.063 (2)* | 0.641 (5) |
C24 | 0.06911 (15) | 0.7942 (3) | −0.1036 (2) | 0.0374 (14) | |
C25 | 0.07432 (18) | 0.8453 (3) | −0.0361 (2) | 0.0559 (17) | |
C26 | 0.01628 (15) | 0.7392 (4) | −0.1443 (2) | 0.0520 (16) | |
C27 | 0.07082 (17) | 0.8874 (4) | −0.1498 (3) | 0.0591 (19) | |
C28 | 0.21934 (15) | 0.6628 (3) | −0.1430 (2) | 0.0363 (11) | |
C29A | 0.2141 (3) | 0.5597 (5) | −0.1850 (3) | 0.0502 (16)* | 0.740 (6) |
C30A | 0.2779 (2) | 0.6725 (5) | −0.0860 (3) | 0.0503 (17)* | 0.740 (6) |
C31A | 0.2075 (3) | 0.7612 (6) | −0.1885 (4) | 0.0630 (19)* | 0.740 (6) |
C29B | 0.2477 (8) | 0.5642 (14) | −0.1417 (11) | 0.059 (4)* | 0.260 (6) |
C30B | 0.2540 (7) | 0.7526 (15) | −0.1124 (10) | 0.060 (4)* | 0.260 (6) |
C31B | 0.1832 (6) | 0.7034 (13) | −0.2235 (8) | 0.040 (4)* | 0.260 (6) |
C22B | 0.3437 (4) | 0.4282 (9) | 0.1645 (6) | 0.039 (3)* | 0.359 (5) |
C23B | 0.3270 (5) | 0.2356 (11) | 0.1680 (8) | 0.063 (3)* | 0.359 (5) |
C21B | 0.3158 (5) | 0.3582 (11) | 0.2501 (7) | 0.065 (3)* | 0.359 (5) |
H6 | 0.25890 | 0.50000 | 0.07460 | 0.0340* | |
H8 | 0.22590 | 0.22960 | 0.14710 | 0.0390* | |
H17B | 0.17900 | 0.08850 | 0.10420 | 0.0810* | |
H17C | 0.12630 | 0.05690 | 0.10490 | 0.0810* | |
H18A | 0.09310 | 0.27120 | 0.12510 | 0.0690* | |
H18B | 0.05640 | 0.18180 | 0.07140 | 0.0690* | |
H12 | 0.22350 | 0.52160 | −0.04760 | 0.0330* | |
H14 | 0.13790 | 0.77790 | −0.15170 | 0.0380* | |
H17A | 0.16590 | 0.13960 | 0.16160 | 0.0810* | |
H3A | 0.10580 | 0.56770 | 0.35810 | 0.0640* | |
H3B | 0.05290 | 0.50150 | 0.33220 | 0.0640* | |
H3C | 0.05110 | 0.62850 | 0.31910 | 0.0640* | |
H21C | 0.35880 | 0.24540 | 0.24650 | 0.0820* | 0.641 (5) |
H22A | 0.32510 | 0.51110 | 0.18280 | 0.0830* | 0.641 (5) |
H22B | 0.37040 | 0.44110 | 0.24250 | 0.0830* | 0.641 (5) |
H22C | 0.31720 | 0.46080 | 0.24490 | 0.0830* | 0.641 (5) |
H23A | 0.33000 | 0.39800 | 0.09450 | 0.0950* | 0.641 (5) |
H23B | 0.32320 | 0.27020 | 0.09470 | 0.0950* | 0.641 (5) |
H23C | 0.37440 | 0.32640 | 0.15410 | 0.0950* | 0.641 (5) |
H25A | 0.10830 | 0.88010 | −0.01070 | 0.0840* | |
H25B | 0.07110 | 0.78930 | −0.00660 | 0.0840* | |
H25C | 0.04690 | 0.89900 | −0.04790 | 0.0840* | |
H26A | −0.01140 | 0.79150 | −0.15390 | 0.0780* | |
H26B | 0.01370 | 0.67980 | −0.11640 | 0.0780* | |
H26C | 0.01270 | 0.71120 | −0.18850 | 0.0780* | |
H27A | 0.10430 | 0.92450 | −0.12540 | 0.0880* | |
H27B | 0.04270 | 0.93840 | −0.15900 | 0.0880* | |
H27C | 0.06650 | 0.85840 | −0.19420 | 0.0880* | |
H29A | 0.22250 | 0.49710 | −0.15400 | 0.0750* | 0.740 (6) |
H29B | 0.23800 | 0.56300 | −0.20470 | 0.0750* | 0.740 (6) |
H29C | 0.17830 | 0.55330 | −0.22290 | 0.0750* | 0.740 (6) |
H30A | 0.28770 | 0.60950 | −0.05520 | 0.0750* | 0.740 (6) |
H30B | 0.28270 | 0.73790 | −0.05830 | 0.0750* | 0.740 (6) |
H30C | 0.29970 | 0.67630 | −0.10890 | 0.0750* | 0.740 (6) |
H31A | 0.23060 | 0.76330 | −0.20950 | 0.0940* | 0.740 (6) |
H31B | 0.21280 | 0.82590 | −0.16010 | 0.0940* | 0.740 (6) |
H31C | 0.17130 | 0.75840 | −0.22560 | 0.0940* | 0.740 (6) |
H18C | 0.05840 | 0.30050 | 0.04420 | 0.0690* | |
H19A | 0.07650 | 0.10820 | −0.01870 | 0.0800* | |
H19B | 0.12920 | 0.14020 | −0.01950 | 0.0800* | |
H19C | 0.08260 | 0.22510 | −0.04480 | 0.0800* | |
H21A | 0.30630 | 0.18880 | 0.19050 | 0.0820* | 0.641 (5) |
H21B | 0.30570 | 0.26610 | 0.24900 | 0.0820* | 0.641 (5) |
H21D | 0.29290 | 0.30590 | 0.25560 | 0.0970* | 0.359 (5) |
H21E | 0.30610 | 0.43110 | 0.25670 | 0.0970* | 0.359 (5) |
H21F | 0.35190 | 0.34400 | 0.28510 | 0.0970* | 0.359 (5) |
H22D | 0.37990 | 0.41310 | 0.19870 | 0.0590* | 0.359 (5) |
H22E | 0.33410 | 0.49970 | 0.17350 | 0.0590* | 0.359 (5) |
H22F | 0.33990 | 0.42600 | 0.11720 | 0.0590* | 0.359 (5) |
H23D | 0.30380 | 0.18440 | 0.17360 | 0.0940* | 0.359 (5) |
H23E | 0.36260 | 0.22520 | 0.20570 | 0.0940* | 0.359 (5) |
H23F | 0.32600 | 0.22360 | 0.12280 | 0.0940* | 0.359 (5) |
H29D | 0.26860 | 0.57760 | −0.16520 | 0.0880* | 0.260 (6) |
H29E | 0.22290 | 0.50620 | −0.16580 | 0.0880* | 0.260 (6) |
H29F | 0.27060 | 0.54310 | −0.09300 | 0.0880* | 0.260 (6) |
H30D | 0.27610 | 0.76040 | −0.13480 | 0.0900* | 0.260 (6) |
H30E | 0.27590 | 0.74000 | −0.06220 | 0.0900* | 0.260 (6) |
H30F | 0.23370 | 0.81850 | −0.11950 | 0.0900* | 0.260 (6) |
H31D | 0.20460 | 0.71110 | −0.24680 | 0.0610* | 0.260 (6) |
H31E | 0.16750 | 0.77300 | −0.22330 | 0.0610* | 0.260 (6) |
H31F | 0.15570 | 0.65050 | −0.24880 | 0.0610* | 0.260 (6) |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Rh1 | 0.0221 (2) | 0.0298 (2) | 0.0211 (2) | 0.0003 (1) | 0.0100 (1) | 0.0000 (1) |
P1 | 0.0193 (4) | 0.0312 (5) | 0.0214 (5) | 0.0000 (4) | 0.0099 (4) | 0.0000 (4) |
O1 | 0.0222 (12) | 0.0488 (16) | 0.0210 (13) | 0.0011 (12) | 0.0101 (10) | 0.0038 (12) |
O2 | 0.0361 (17) | 0.090 (2) | 0.0409 (18) | −0.0255 (17) | 0.0176 (15) | −0.0183 (17) |
O3 | 0.0209 (12) | 0.0296 (14) | 0.0238 (14) | 0.0001 (10) | 0.0096 (11) | −0.0018 (10) |
O4 | 0.0268 (13) | 0.0269 (14) | 0.0310 (14) | 0.0014 (11) | 0.0189 (11) | 0.0007 (11) |
N1 | 0.0223 (15) | 0.0338 (18) | 0.0203 (17) | −0.0016 (14) | 0.0071 (13) | −0.0029 (14) |
C1 | 0.035 (2) | 0.046 (3) | 0.028 (2) | −0.0083 (19) | 0.0172 (19) | −0.0086 (18) |
C2 | 0.0208 (18) | 0.034 (2) | 0.026 (2) | 0.0011 (16) | 0.0062 (17) | −0.0005 (17) |
C3 | 0.043 (2) | 0.060 (3) | 0.030 (2) | 0.004 (2) | 0.022 (2) | 0.002 (2) |
C4 | 0.0208 (18) | 0.028 (2) | 0.024 (2) | 0.0033 (16) | 0.0108 (16) | −0.0026 (16) |
C5 | 0.0270 (18) | 0.028 (2) | 0.029 (2) | 0.0011 (17) | 0.0163 (16) | −0.0022 (16) |
C6 | 0.0247 (19) | 0.030 (2) | 0.035 (2) | −0.0019 (16) | 0.0184 (17) | 0.0019 (17) |
C7 | 0.028 (2) | 0.031 (2) | 0.035 (2) | 0.0055 (17) | 0.0171 (18) | 0.0041 (17) |
C8 | 0.032 (2) | 0.026 (2) | 0.040 (2) | 0.0090 (17) | 0.0189 (19) | 0.0095 (17) |
C9 | 0.028 (2) | 0.027 (2) | 0.033 (2) | 0.0020 (16) | 0.0194 (18) | −0.0001 (16) |
C10 | 0.0227 (18) | 0.029 (2) | 0.023 (2) | −0.0028 (16) | 0.0102 (16) | −0.0023 (16) |
C11 | 0.0221 (18) | 0.024 (2) | 0.028 (2) | −0.0026 (15) | 0.0107 (16) | −0.0011 (15) |
C12 | 0.0247 (18) | 0.024 (2) | 0.036 (2) | −0.0003 (16) | 0.0161 (17) | −0.0024 (17) |
C13 | 0.031 (2) | 0.026 (2) | 0.033 (2) | −0.0012 (17) | 0.0143 (18) | −0.0006 (17) |
C14 | 0.037 (2) | 0.029 (2) | 0.030 (2) | −0.0018 (18) | 0.0168 (18) | 0.0062 (17) |
C15 | 0.0268 (19) | 0.027 (2) | 0.030 (2) | −0.0007 (16) | 0.0115 (17) | 0.0011 (16) |
C16 | 0.037 (2) | 0.025 (2) | 0.046 (3) | −0.0038 (17) | 0.023 (2) | −0.0011 (18) |
C17 | 0.049 (3) | 0.033 (2) | 0.077 (4) | −0.003 (2) | 0.028 (3) | 0.012 (2) |
C18 | 0.045 (2) | 0.037 (3) | 0.069 (3) | −0.009 (2) | 0.037 (2) | −0.002 (2) |
C19 | 0.056 (3) | 0.041 (3) | 0.066 (3) | −0.013 (2) | 0.031 (3) | −0.016 (2) |
C20 | 0.0335 (19) | 0.040 (2) | 0.054 (2) | 0.0069 (17) | 0.0214 (18) | 0.0137 (18) |
C24 | 0.040 (2) | 0.032 (2) | 0.044 (3) | 0.0073 (18) | 0.023 (2) | 0.0103 (18) |
C25 | 0.068 (3) | 0.040 (3) | 0.066 (3) | 0.022 (2) | 0.037 (3) | 0.001 (2) |
C26 | 0.036 (2) | 0.058 (3) | 0.058 (3) | 0.011 (2) | 0.019 (2) | 0.016 (2) |
C27 | 0.054 (3) | 0.043 (3) | 0.089 (4) | 0.021 (2) | 0.041 (3) | 0.033 (3) |
C28 | 0.0386 (19) | 0.036 (2) | 0.043 (2) | −0.0005 (17) | 0.0266 (17) | 0.0024 (17) |
Geometric parameters (Å, º) top
Rh1—P1 | 2.2074 (10) | C17—H17A | 0.9806 |
Rh1—N1 | 2.119 (3) | C17—H17B | 0.9779 |
Rh1—C1 | 1.799 (5) | C17—H17C | 0.9796 |
Rh1—O1i | 2.071 (3) | C18—H18A | 0.9794 |
P1—O1 | 1.507 (3) | C18—H18B | 0.9801 |
P1—O3 | 1.642 (3) | C18—H18C | 0.9786 |
P1—O4 | 1.625 (3) | C19—H19A | 0.9799 |
O2—C1 | 1.161 (6) | C19—H19B | 0.9797 |
O3—C4 | 1.405 (4) | C19—H19C | 0.9801 |
O4—C10 | 1.394 (5) | C21A—H21A | 0.9790 |
N1—C2 | 1.126 (5) | C21A—H21B | 0.9796 |
C2—C3 | 1.464 (6) | C21A—H21C | 0.9808 |
C4—C5 | 1.392 (6) | C21B—H21E | 0.9799 |
C4—C9 | 1.408 (5) | C21B—H21F | 0.9808 |
C5—C6 | 1.401 (6) | C21B—H21D | 0.9806 |
C5—C11 | 1.496 (5) | C22A—H22A | 0.9797 |
C6—C7 | 1.383 (5) | C22A—H22B | 0.9803 |
C7—C8 | 1.398 (6) | C22A—H22C | 0.9810 |
C7—C20 | 1.543 (6) | C22B—H22D | 0.9806 |
C8—C9 | 1.401 (6) | C22B—H22F | 0.9800 |
C9—C16 | 1.539 (6) | C22B—H22E | 0.9791 |
C10—C11 | 1.396 (5) | C23A—H23B | 0.9797 |
C10—C15 | 1.410 (5) | C23A—H23A | 0.9807 |
C11—C12 | 1.392 (6) | C23A—H23C | 0.9789 |
C12—C13 | 1.389 (5) | C23B—H23D | 0.9791 |
C13—C14 | 1.395 (6) | C23B—H23E | 0.9809 |
C13—C28 | 1.539 (6) | C23B—H23F | 0.9798 |
C14—C15 | 1.391 (6) | C25—H25C | 0.9794 |
C15—C24 | 1.556 (6) | C25—H25A | 0.9792 |
C16—C17 | 1.542 (5) | C25—H25B | 0.9803 |
C16—C18 | 1.529 (7) | C26—H26B | 0.9804 |
C16—C19 | 1.531 (6) | C26—H26C | 0.9790 |
C20—C21A | 1.479 (8) | C26—H26A | 0.9804 |
C20—C22A | 1.530 (8) | C27—H27A | 0.9797 |
C20—C23A | 1.560 (10) | C27—H27C | 0.9800 |
C20—C21B | 1.654 (14) | C27—H27B | 0.9809 |
C20—C22B | 1.462 (13) | C29A—H29A | 0.9807 |
C20—C23B | 1.485 (15) | C29A—H29C | 0.9809 |
C24—C25 | 1.538 (6) | C29A—H29B | 0.9788 |
C24—C26 | 1.530 (6) | C29B—H29E | 0.9793 |
C24—C27 | 1.549 (7) | C29B—H29F | 0.9816 |
C28—C29A | 1.538 (7) | C29B—H29D | 0.9792 |
C28—C30A | 1.571 (8) | C30A—H30A | 0.9800 |
C28—C31A | 1.506 (8) | C30A—H30C | 0.9787 |
C28—C29B | 1.47 (2) | C30A—H30B | 0.9808 |
C28—C30B | 1.44 (2) | C30B—H30E | 0.9801 |
C28—C31B | 1.635 (16) | C30B—H30F | 0.9798 |
C3—H3A | 0.9810 | C30B—H30D | 0.9814 |
C3—H3B | 0.9794 | C31A—H31A | 0.9790 |
C3—H3C | 0.9797 | C31A—H31B | 0.9798 |
C6—H6 | 0.9502 | C31A—H31C | 0.9807 |
C8—H8 | 0.9499 | C31B—H31D | 0.9790 |
C12—H12 | 0.9492 | C31B—H31E | 0.9802 |
C14—H14 | 0.9505 | C31B—H31F | 0.9805 |
| | | |
P1—Rh1—N1 | 178.42 (8) | C16—C18—H18A | 109.40 |
P1—Rh1—C1 | 87.84 (13) | C16—C18—H18B | 109.41 |
P1—Rh1—O1i | 94.91 (7) | C16—C18—H18C | 109.51 |
N1—Rh1—C1 | 92.47 (15) | H18A—C18—H18B | 109.42 |
O1i—Rh1—N1 | 84.74 (11) | H18A—C18—H18C | 109.52 |
O1i—Rh1—C1 | 176.86 (15) | H18B—C18—H18C | 109.57 |
Rh1—P1—O1 | 119.91 (11) | C16—C19—H19A | 109.47 |
Rh1—P1—O3 | 117.37 (9) | C16—C19—H19B | 109.43 |
Rh1—P1—O4 | 107.22 (10) | C16—C19—H19C | 109.46 |
O1—P1—O3 | 100.47 (13) | H19A—C19—H19B | 109.52 |
O1—P1—O4 | 108.41 (14) | H19A—C19—H19C | 109.42 |
O3—P1—O4 | 101.82 (13) | H19B—C19—H19C | 109.52 |
Rh1i—O1—P1 | 143.09 (16) | C20—C21A—H21A | 109.44 |
P1—O3—C4 | 119.0 (2) | C20—C21A—H21B | 109.50 |
P1—O4—C10 | 127.9 (2) | C20—C21A—H21C | 109.44 |
Rh1—N1—C2 | 173.7 (3) | H21A—C21A—H21B | 109.52 |
Rh1—C1—O2 | 177.5 (4) | H21A—C21A—H21C | 109.43 |
N1—C2—C3 | 179.6 (4) | H21B—C21A—H21C | 109.50 |
O3—C4—C5 | 117.6 (3) | H21E—C21B—H21F | 109.45 |
O3—C4—C9 | 119.9 (3) | C20—C21B—H21F | 109.50 |
C5—C4—C9 | 122.3 (4) | C20—C21B—H21D | 109.45 |
C4—C5—C6 | 118.2 (3) | C20—C21B—H21E | 109.56 |
C4—C5—C11 | 122.7 (3) | H21D—C21B—H21E | 109.43 |
C6—C5—C11 | 118.7 (4) | H21D—C21B—H21F | 109.44 |
C5—C6—C7 | 122.1 (4) | C20—C22A—H22B | 109.48 |
C6—C7—C8 | 117.3 (4) | C20—C22A—H22A | 109.55 |
C6—C7—C20 | 121.3 (4) | H22A—C22A—H22B | 109.52 |
C8—C7—C20 | 121.3 (3) | H22A—C22A—H22C | 109.39 |
C7—C8—C9 | 123.7 (3) | C20—C22A—H22C | 109.48 |
C4—C9—C8 | 116.0 (4) | H22B—C22A—H22C | 109.41 |
C4—C9—C16 | 122.9 (3) | C20—C22B—H22D | 109.42 |
C8—C9—C16 | 120.8 (3) | C20—C22B—H22E | 109.58 |
O4—C10—C11 | 118.4 (3) | C20—C22B—H22F | 109.51 |
O4—C10—C15 | 119.5 (3) | H22D—C22B—H22E | 109.35 |
C11—C10—C15 | 121.8 (4) | H22D—C22B—H22F | 109.45 |
C5—C11—C10 | 123.8 (3) | H22E—C22B—H22F | 109.53 |
C5—C11—C12 | 117.8 (3) | C20—C23A—H23B | 109.43 |
C10—C11—C12 | 118.4 (3) | C20—C23A—H23C | 109.45 |
C11—C12—C13 | 122.4 (4) | C20—C23A—H23A | 109.50 |
C12—C13—C14 | 117.1 (4) | H23A—C23A—H23B | 109.47 |
C12—C13—C28 | 120.5 (4) | H23A—C23A—H23C | 109.40 |
C14—C13—C28 | 122.5 (3) | H23B—C23A—H23C | 109.58 |
C13—C14—C15 | 123.7 (3) | C20—C23B—H23D | 109.56 |
C10—C15—C14 | 116.7 (4) | C20—C23B—H23E | 109.48 |
C10—C15—C24 | 122.7 (4) | C20—C23B—H23F | 109.44 |
C14—C15—C24 | 120.6 (3) | H23E—C23B—H23F | 109.34 |
C9—C16—C17 | 111.5 (3) | H23D—C23B—H23E | 109.55 |
C9—C16—C18 | 113.4 (3) | H23D—C23B—H23F | 109.46 |
C9—C16—C19 | 107.9 (3) | C24—C25—H25B | 109.48 |
C17—C16—C18 | 107.0 (3) | H25A—C25—H25C | 109.45 |
C17—C16—C19 | 107.4 (3) | C24—C25—H25C | 109.50 |
C18—C16—C19 | 109.6 (4) | H25A—C25—H25B | 109.40 |
C7—C20—C21A | 113.9 (5) | C24—C25—H25A | 109.51 |
C7—C20—C22A | 109.6 (4) | H25B—C25—H25C | 109.48 |
C7—C20—C23A | 106.5 (4) | C24—C26—H26C | 109.49 |
C7—C20—C21B | 105.1 (6) | H26A—C26—H26B | 109.40 |
C7—C20—C22B | 114.2 (5) | C24—C26—H26B | 109.41 |
C7—C20—C23B | 112.2 (7) | H26B—C26—H26C | 109.57 |
C21A—C20—C22A | 109.4 (5) | H26A—C26—H26C | 109.52 |
C21A—C20—C23A | 111.0 (5) | C24—C26—H26A | 109.43 |
C22A—C20—C23A | 106.1 (5) | C24—C27—H27A | 109.45 |
C21B—C20—C22B | 107.5 (7) | H27A—C27—H27B | 109.43 |
C21B—C20—C23B | 104.4 (8) | H27A—C27—H27C | 109.51 |
C22B—C20—C23B | 112.5 (8) | H27B—C27—H27C | 109.47 |
C15—C24—C25 | 110.9 (3) | C24—C27—H27C | 109.52 |
C15—C24—C26 | 110.4 (3) | C24—C27—H27B | 109.45 |
C15—C24—C27 | 111.0 (4) | C28—C29A—H29B | 109.51 |
C25—C24—C26 | 110.6 (4) | C28—C29A—H29A | 109.36 |
C25—C24—C27 | 106.9 (3) | H29B—C29A—H29C | 109.65 |
C26—C24—C27 | 107.1 (4) | H29A—C29A—H29C | 109.36 |
C13—C28—C29A | 108.6 (4) | C28—C29A—H29C | 109.35 |
C13—C28—C30A | 109.1 (4) | H29A—C29A—H29B | 109.60 |
C13—C28—C31A | 114.3 (5) | C28—C29B—H29F | 109.44 |
C13—C28—C29B | 113.9 (9) | H29E—C29B—H29F | 109.44 |
C13—C28—C30B | 108.6 (9) | H29D—C29B—H29E | 109.51 |
C13—C28—C31B | 109.5 (7) | H29D—C29B—H29F | 109.37 |
C29A—C28—C30A | 107.2 (5) | C28—C29B—H29E | 109.53 |
C29A—C28—C31A | 111.1 (4) | C28—C29B—H29D | 109.53 |
C30A—C28—C31A | 106.3 (5) | C28—C30A—H30A | 109.44 |
C29B—C28—C30B | 111.6 (13) | C28—C30A—H30B | 109.39 |
C29B—C28—C31B | 110.5 (10) | C28—C30A—H30C | 109.46 |
C30B—C28—C31B | 102.2 (10) | H30B—C30A—H30C | 109.51 |
C2—C3—H3A | 109.44 | H30A—C30A—H30C | 109.61 |
C2—C3—H3B | 109.46 | H30A—C30A—H30B | 109.43 |
C2—C3—H3C | 109.54 | C28—C30B—H30F | 109.48 |
H3A—C3—H3B | 109.45 | H30D—C30B—H30E | 109.33 |
H3A—C3—H3C | 109.44 | H30E—C30B—H30F | 109.62 |
H3B—C3—H3C | 109.50 | C28—C30B—H30D | 109.44 |
C5—C6—H6 | 118.94 | H30D—C30B—H30F | 109.41 |
C7—C6—H6 | 118.99 | C28—C30B—H30E | 109.55 |
C7—C8—H8 | 118.13 | H31B—C31A—H31C | 109.44 |
C9—C8—H8 | 118.18 | C28—C31A—H31A | 109.46 |
C11—C12—H12 | 118.76 | C28—C31A—H31B | 109.55 |
C13—C12—H12 | 118.86 | C28—C31A—H31C | 109.43 |
C13—C14—H14 | 118.13 | H31A—C31A—H31B | 109.49 |
C15—C14—H14 | 118.17 | H31A—C31A—H31C | 109.46 |
C16—C17—H17A | 109.47 | C28—C31B—H31D | 109.61 |
C16—C17—H17B | 109.50 | C28—C31B—H31E | 109.50 |
C16—C17—H17C | 109.45 | C28—C31B—H31F | 109.53 |
H17A—C17—H17B | 109.52 | H31D—C31B—H31E | 109.40 |
H17A—C17—H17C | 109.42 | H31D—C31B—H31F | 109.37 |
H17B—C17—H17C | 109.46 | H31E—C31B—H31F | 109.41 |
| | | |
C1—Rh1—P1—O1 | −165.70 (17) | C6—C7—C20—C23A | −60.6 (5) |
C1—Rh1—P1—O3 | 72.03 (16) | C8—C7—C20—C21A | −5.5 (6) |
C1—Rh1—P1—O4 | −41.67 (16) | C8—C7—C20—C22A | −128.5 (5) |
O1i—Rh1—P1—O1 | 12.78 (14) | C8—C7—C20—C23A | 117.2 (5) |
O1i—Rh1—P1—O3 | −109.49 (13) | C7—C8—C9—C4 | −3.0 (6) |
O1i—Rh1—P1—O4 | 136.81 (12) | C7—C8—C9—C16 | 170.8 (4) |
P1—Rh1—O1i—P1i | −18.6 (3) | C4—C9—C16—C17 | 177.8 (4) |
N1—Rh1—O1i—P1i | 159.8 (3) | C4—C9—C16—C18 | −61.4 (5) |
Rh1—P1—O1—Rh1i | −21.5 (3) | C4—C9—C16—C19 | 60.2 (5) |
O3—P1—O1—Rh1i | 108.7 (3) | C8—C9—C16—C17 | 4.5 (5) |
O4—P1—O1—Rh1i | −145.0 (2) | C8—C9—C16—C18 | 125.3 (4) |
Rh1—P1—O3—C4 | −56.6 (3) | C8—C9—C16—C19 | −113.2 (4) |
O1—P1—O3—C4 | 171.6 (2) | O4—C10—C11—C5 | 3.0 (5) |
O4—P1—O3—C4 | 60.1 (3) | O4—C10—C11—C12 | −175.9 (3) |
Rh1—P1—O4—C10 | 151.5 (2) | C15—C10—C11—C5 | 176.3 (3) |
O1—P1—O4—C10 | −77.8 (3) | C15—C10—C11—C12 | −2.5 (5) |
O3—P1—O4—C10 | 27.6 (3) | O4—C10—C15—C14 | 175.7 (3) |
P1—O3—C4—C5 | −71.7 (4) | O4—C10—C15—C24 | −4.4 (5) |
P1—O3—C4—C9 | 113.8 (3) | C11—C10—C15—C14 | 2.4 (5) |
P1—O4—C10—C11 | −62.6 (4) | C11—C10—C15—C24 | −177.7 (3) |
P1—O4—C10—C15 | 123.9 (3) | C5—C11—C12—C13 | −178.2 (3) |
O3—C4—C5—C6 | 179.8 (3) | C10—C11—C12—C13 | 0.8 (6) |
O3—C4—C5—C11 | −6.6 (5) | C11—C12—C13—C14 | 1.0 (6) |
C9—C4—C5—C6 | −5.9 (5) | C11—C12—C13—C28 | 179.9 (3) |
C9—C4—C5—C11 | 167.8 (3) | C12—C13—C14—C15 | −1.1 (6) |
O3—C4—C9—C8 | −178.9 (3) | C28—C13—C14—C15 | 180.0 (4) |
O3—C4—C9—C16 | 7.5 (5) | C12—C13—C28—C29A | 61.4 (5) |
C5—C4—C9—C8 | 6.9 (5) | C12—C13—C28—C30A | −55.1 (5) |
C5—C4—C9—C16 | −166.7 (4) | C12—C13—C28—C31A | −173.9 (4) |
C4—C5—C6—C7 | 0.7 (6) | C14—C13—C28—C29A | −119.7 (4) |
C11—C5—C6—C7 | −173.2 (3) | C14—C13—C28—C30A | 123.8 (4) |
C4—C5—C11—C10 | 48.6 (5) | C14—C13—C28—C31A | 5.0 (6) |
C4—C5—C11—C12 | −132.6 (4) | C13—C14—C15—C10 | −0.5 (6) |
C6—C5—C11—C10 | −137.8 (4) | C13—C14—C15—C24 | 179.6 (4) |
C6—C5—C11—C12 | 41.0 (5) | C10—C15—C24—C25 | 54.0 (5) |
C5—C6—C7—C8 | 3.0 (6) | C10—C15—C24—C26 | −68.9 (5) |
C5—C6—C7—C20 | −179.2 (4) | C10—C15—C24—C27 | 172.6 (4) |
C6—C7—C8—C9 | −1.8 (6) | C14—C15—C24—C25 | −126.1 (4) |
C20—C7—C8—C9 | −179.6 (4) | C14—C15—C24—C26 | 111.1 (4) |
C6—C7—C20—C21A | 176.8 (5) | C14—C15—C24—C27 | −7.5 (5) |
C6—C7—C20—C22A | 53.8 (6) | | |
Symmetry code: (i) −x, −y+1, −z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
C18—H18C···O3 | 0.98 | 2.42 | 3.067 (5) | 123 |
C19—H19C···O3 | 0.98 | 2.42 | 3.082 (5) | 124 |
C25—H25B···O4 | 0.98 | 2.26 | 2.923 (4) | 124 |
C26—H26B···O1 | 0.98 | 2.34 | 3.306 (5) | 168 |