In the title compound, [Rh(C9H6NO)(C24H27O3P)(CO)], the molecules pack in a tail-to-tail fashion, with a π–π stacking distance of 3.76 (6) Å, due to the steric effect of the phosphite ligand. The effective cone angle (ΘE) for the phosphite ligand is 183°.
Supporting information
CCDC reference: 283937
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.007 Å
- R factor = 0.046
- wR factor = 0.097
- Data-to-parameter ratio = 15.6
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ?
PLAT199_ALERT_1_C Check the Reported _cell_measurement_temperature 293 K
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Rh - N .. 5.31 su
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Rh - C10 .. 6.53 su
PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C5
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
5 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
2 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
0 ALERT type 3 Indicator that the structure quality may be low
0 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART-NT (Bruker, 1998); cell refinement: SAINT-Plus (Bruker, 1999); data reduction: SAINT-Plus and XPREP (Bruker, 1999); program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg & Berndt, 2001); software used to prepare material for publication: WinGX (Farrugia, 1999).
Carbonyl(8-hydroxyquinolinato)[tris(2,6-dimethylphenyl)phosphite]rhodium(I)
top
Crystal data top
[Rh(C9H6NO)(C24H27O3P)(CO)] | Z = 2 |
Mr = 669.49 | F(000) = 688 |
Triclinic, P1 | Dx = 1.439 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 10.580 (2) Å | Cell parameters from 925 reflections |
b = 10.944 (2) Å | θ = 5.5–45.9° |
c = 13.886 (3) Å | µ = 0.65 mm−1 |
α = 83.49 (3)° | T = 293 K |
β = 75.25 (3)° | Plate, yellow |
γ = 88.58 (3)° | 0.36 × 0.12 × 0.07 mm |
V = 1545.0 (5) Å3 | |
Data collection top
Bruker SMART CCD 1K area-detector diffractometer | 4122 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.030 |
ω scans | θmax = 26°, θmin = 1.5° |
Absorption correction: multi-scan (SADABS; Bruker, 1998) | h = −12→13 |
Tmin = 0.801, Tmax = 0.956 | k = −13→13 |
9255 measured reflections | l = −17→10 |
6014 independent reflections | |
Refinement top
Refinement on F2 | 0 restraints |
Least-squares matrix: full | H-atom parameters constrained |
R[F2 > 2σ(F2)] = 0.046 | w = 1/[σ2(Fo2) + (0.0361P)2 + 0.3605P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.097 | (Δ/σ)max < 0.001 |
S = 1.02 | Δρmax = 0.46 e Å−3 |
6014 reflections | Δρmin = −0.34 e Å−3 |
385 parameters | |
Special details top
Experimental. The intensity data were collected on a Siemens SMART CCD 1 K
diffractometer using an exposure time of 10 s/frame. A total of 1350 frames
were collected with a frame width of 0.3° covering up to θ = 26.99° with
98.5% completeness accomplished. The first 50 frames were recollected at the
end of each data collection to check for decay; none was found. |
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 | |
Rh | 0.56737 (3) | 0.28624 (3) | 0.35606 (2) | 0.04167 (12) | |
P | 0.67150 (9) | 0.41603 (9) | 0.22987 (7) | 0.0386 (3) | |
O1 | 0.8039 (2) | 0.3697 (2) | 0.15756 (19) | 0.0443 (7) | |
O2 | 0.7180 (2) | 0.5441 (2) | 0.25409 (19) | 0.0441 (7) | |
O3 | 0.5849 (2) | 0.4702 (2) | 0.15625 (18) | 0.0414 (6) | |
O4 | 0.7340 (2) | 0.2340 (2) | 0.3960 (2) | 0.0525 (7) | |
O5 | 0.3188 (3) | 0.3341 (3) | 0.2992 (3) | 0.0799 (10) | |
N | 0.4873 (3) | 0.1796 (3) | 0.4919 (2) | 0.0500 (9) | |
C1 | 0.3637 (5) | 0.1575 (4) | 0.5398 (3) | 0.0600 (12) | |
C2 | 0.3292 (6) | 0.0858 (5) | 0.6335 (4) | 0.0749 (16) | |
C3 | 0.4219 (7) | 0.0358 (5) | 0.6748 (4) | 0.0821 (17) | |
C4 | 0.5556 (6) | 0.0557 (4) | 0.6272 (3) | 0.0647 (13) | |
C5 | 0.6597 (8) | 0.0078 (5) | 0.6642 (4) | 0.094 (2) | |
C6 | 0.7849 (7) | 0.0357 (5) | 0.6113 (5) | 0.0891 (18) | |
C7 | 0.8132 (5) | 0.1125 (4) | 0.5204 (4) | 0.0729 (14) | |
C8 | 0.7139 (4) | 0.1614 (4) | 0.4813 (3) | 0.0522 (11) | |
C9 | 0.5825 (4) | 0.1315 (4) | 0.5355 (3) | 0.0504 (11) | |
C10 | 0.4162 (4) | 0.3180 (4) | 0.3204 (3) | 0.0534 (11) | |
C11 | 0.8524 (4) | 0.2477 (4) | 0.1583 (3) | 0.0449 (10) | |
C12 | 0.9587 (4) | 0.2241 (4) | 0.1981 (3) | 0.0524 (11) | |
C13 | 1.0131 (4) | 0.1072 (5) | 0.1901 (4) | 0.0696 (14) | |
C14 | 0.9627 (5) | 0.0207 (5) | 0.1455 (4) | 0.0769 (16) | |
C15 | 0.8570 (5) | 0.0473 (4) | 0.1086 (4) | 0.0676 (13) | |
C16 | 0.7977 (4) | 0.1625 (4) | 0.1137 (3) | 0.0513 (11) | |
C21 | 0.8274 (4) | 0.5806 (3) | 0.2845 (3) | 0.0448 (10) | |
C22 | 0.9303 (4) | 0.6365 (4) | 0.2111 (3) | 0.0521 (11) | |
C23 | 1.0348 (4) | 0.6764 (4) | 0.2427 (5) | 0.0715 (14) | |
C24 | 1.0346 (5) | 0.6642 (5) | 0.3413 (5) | 0.0848 (18) | |
C25 | 0.9306 (6) | 0.6123 (5) | 0.4120 (4) | 0.0781 (16) | |
C26 | 0.8222 (4) | 0.5694 (4) | 0.3861 (3) | 0.0545 (11) | |
C31 | 0.5881 (4) | 0.5912 (3) | 0.1070 (3) | 0.0414 (9) | |
C32 | 0.6524 (4) | 0.6110 (4) | 0.0066 (3) | 0.0472 (10) | |
C33 | 0.6548 (4) | 0.7302 (5) | −0.0404 (4) | 0.0652 (13) | |
C34 | 0.5952 (5) | 0.8241 (4) | 0.0119 (4) | 0.0731 (15) | |
C35 | 0.5276 (5) | 0.7997 (4) | 0.1098 (4) | 0.0663 (13) | |
C36 | 0.5200 (4) | 0.6828 (4) | 0.1608 (3) | 0.0522 (11) | |
C121 | 1.0114 (4) | 0.3166 (4) | 0.2494 (4) | 0.0708 (14) | |
C161 | 0.6827 (5) | 0.1879 (4) | 0.0712 (4) | 0.0687 (13) | |
C221 | 0.9281 (5) | 0.6562 (4) | 0.1023 (4) | 0.0721 (14) | |
C261 | 0.7060 (5) | 0.5148 (4) | 0.4639 (3) | 0.0774 (15) | |
C321 | 0.7136 (4) | 0.5068 (4) | −0.0507 (3) | 0.0638 (13) | |
C361 | 0.4395 (4) | 0.6570 (4) | 0.2666 (3) | 0.0705 (14) | |
H1 | 0.2981 | 0.1899 | 0.511 | 0.072* | |
H2 | 0.2416 | 0.0733 | 0.6666 | 0.09* | |
H3 | 0.3981 | −0.013 | 0.736 | 0.099* | |
H5 | 0.6437 | −0.0428 | 0.7245 | 0.113* | |
H6 | 0.8535 | 0.0027 | 0.6362 | 0.107* | |
H7 | 0.8997 | 0.1304 | 0.4866 | 0.088* | |
H12A | 1.026 | 0.3933 | 0.2072 | 0.106* | |
H12B | 1.0924 | 0.2875 | 0.2625 | 0.106* | |
H12C | 0.9496 | 0.3283 | 0.3115 | 0.106* | |
H13 | 1.0851 | 0.0873 | 0.2155 | 0.084* | |
H14 | 1.0012 | −0.0564 | 0.1407 | 0.092* | |
H15 | 0.8235 | −0.0124 | 0.0792 | 0.081* | |
H16A | 0.6125 | 0.2193 | 0.1207 | 0.103* | |
H16B | 0.6551 | 0.1133 | 0.0523 | 0.103* | |
H16C | 0.7062 | 0.2477 | 0.0134 | 0.103* | |
H22A | 1.0021 | 0.7054 | 0.065 | 0.108* | |
H22B | 0.849 | 0.6976 | 0.0962 | 0.108* | |
H22C | 0.9319 | 0.5781 | 0.0764 | 0.108* | |
H23 | 1.1066 | 0.7123 | 0.1955 | 0.086* | |
H24 | 1.1061 | 0.6916 | 0.3605 | 0.102* | |
H25 | 0.932 | 0.6053 | 0.4791 | 0.094* | |
H26A | 0.6291 | 0.5606 | 0.4584 | 0.116* | |
H26B | 0.7194 | 0.518 | 0.5294 | 0.116* | |
H26C | 0.695 | 0.4308 | 0.4538 | 0.116* | |
H32A | 0.7882 | 0.4771 | −0.0278 | 0.096* | |
H32B | 0.7406 | 0.5353 | −0.1209 | 0.096* | |
H32C | 0.651 | 0.4414 | −0.0401 | 0.096* | |
H33 | 0.6973 | 0.7465 | −0.1079 | 0.078* | |
H34 | 0.6008 | 0.9042 | −0.0194 | 0.088* | |
H35 | 0.4852 | 0.8639 | 0.1434 | 0.08* | |
H36A | 0.3875 | 0.5845 | 0.2727 | 0.106* | |
H36B | 0.3832 | 0.7256 | 0.2838 | 0.106* | |
H36C | 0.4961 | 0.6445 | 0.3109 | 0.106* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Rh | 0.03984 (19) | 0.0479 (2) | 0.03395 (18) | −0.00851 (13) | −0.00486 (14) | 0.00087 (14) |
P | 0.0352 (5) | 0.0447 (6) | 0.0341 (6) | −0.0049 (5) | −0.0066 (5) | −0.0007 (5) |
N | 0.054 (2) | 0.049 (2) | 0.042 (2) | −0.0127 (17) | 0.0003 (19) | −0.0095 (17) |
O1 | 0.0358 (14) | 0.0474 (17) | 0.0441 (16) | 0.0001 (12) | −0.0015 (13) | −0.0005 (13) |
O2 | 0.0401 (14) | 0.0466 (16) | 0.0471 (16) | −0.0043 (12) | −0.0141 (13) | −0.0035 (13) |
O3 | 0.0389 (14) | 0.0467 (16) | 0.0387 (15) | −0.0030 (12) | −0.0112 (13) | −0.0009 (13) |
O4 | 0.0461 (16) | 0.0620 (19) | 0.0463 (17) | −0.0075 (14) | −0.0111 (14) | 0.0073 (15) |
O5 | 0.0501 (19) | 0.112 (3) | 0.081 (3) | −0.0144 (18) | −0.0269 (19) | 0.001 (2) |
C1 | 0.067 (3) | 0.062 (3) | 0.044 (3) | −0.013 (2) | 0.004 (2) | −0.011 (2) |
C2 | 0.086 (4) | 0.074 (4) | 0.048 (3) | −0.029 (3) | 0.017 (3) | −0.009 (3) |
C3 | 0.137 (5) | 0.058 (3) | 0.041 (3) | −0.025 (4) | −0.004 (4) | 0.002 (2) |
C4 | 0.106 (4) | 0.048 (3) | 0.041 (3) | −0.010 (3) | −0.019 (3) | −0.001 (2) |
C5 | 0.175 (7) | 0.062 (4) | 0.051 (4) | −0.003 (4) | −0.045 (4) | 0.004 (3) |
C6 | 0.127 (5) | 0.076 (4) | 0.078 (4) | 0.011 (4) | −0.057 (4) | 0.002 (3) |
C7 | 0.079 (3) | 0.077 (4) | 0.069 (4) | 0.003 (3) | −0.034 (3) | 0.000 (3) |
C8 | 0.069 (3) | 0.047 (3) | 0.049 (3) | −0.001 (2) | −0.028 (3) | −0.007 (2) |
C9 | 0.067 (3) | 0.046 (3) | 0.037 (2) | −0.008 (2) | −0.010 (2) | −0.004 (2) |
C10 | 0.054 (3) | 0.065 (3) | 0.038 (2) | −0.017 (2) | −0.005 (2) | −0.002 (2) |
C11 | 0.040 (2) | 0.048 (3) | 0.038 (2) | 0.0017 (19) | 0.003 (2) | 0.005 (2) |
C12 | 0.044 (2) | 0.058 (3) | 0.047 (3) | 0.003 (2) | −0.002 (2) | 0.005 (2) |
C13 | 0.055 (3) | 0.082 (4) | 0.063 (3) | 0.014 (3) | −0.009 (3) | 0.011 (3) |
C14 | 0.083 (4) | 0.056 (3) | 0.077 (4) | 0.014 (3) | 0.005 (3) | −0.005 (3) |
C15 | 0.079 (3) | 0.057 (3) | 0.059 (3) | −0.004 (3) | −0.003 (3) | −0.007 (2) |
C16 | 0.056 (3) | 0.048 (3) | 0.042 (2) | −0.002 (2) | 0.000 (2) | −0.002 (2) |
C21 | 0.046 (2) | 0.040 (2) | 0.054 (3) | 0.0009 (19) | −0.022 (2) | −0.008 (2) |
C22 | 0.045 (2) | 0.047 (3) | 0.063 (3) | −0.006 (2) | −0.013 (2) | −0.005 (2) |
C23 | 0.051 (3) | 0.070 (3) | 0.093 (4) | −0.012 (2) | −0.015 (3) | −0.013 (3) |
C24 | 0.064 (3) | 0.096 (4) | 0.115 (5) | −0.001 (3) | −0.046 (4) | −0.042 (4) |
C25 | 0.093 (4) | 0.085 (4) | 0.080 (4) | 0.020 (3) | −0.058 (4) | −0.031 (3) |
C26 | 0.067 (3) | 0.050 (3) | 0.051 (3) | 0.008 (2) | −0.022 (3) | −0.010 (2) |
C31 | 0.040 (2) | 0.043 (2) | 0.044 (2) | −0.0044 (18) | −0.018 (2) | 0.002 (2) |
C32 | 0.042 (2) | 0.060 (3) | 0.042 (2) | −0.001 (2) | −0.016 (2) | 0.001 (2) |
C33 | 0.072 (3) | 0.071 (3) | 0.052 (3) | −0.005 (3) | −0.025 (3) | 0.018 (3) |
C34 | 0.098 (4) | 0.048 (3) | 0.077 (4) | −0.002 (3) | −0.039 (3) | 0.011 (3) |
C35 | 0.077 (3) | 0.059 (3) | 0.071 (4) | 0.017 (3) | −0.033 (3) | −0.010 (3) |
C36 | 0.054 (3) | 0.055 (3) | 0.051 (3) | 0.002 (2) | −0.020 (2) | −0.007 (2) |
C121 | 0.042 (3) | 0.079 (3) | 0.090 (4) | −0.003 (2) | −0.020 (3) | 0.001 (3) |
C161 | 0.085 (3) | 0.062 (3) | 0.061 (3) | −0.010 (3) | −0.024 (3) | −0.004 (2) |
C221 | 0.072 (3) | 0.073 (3) | 0.064 (3) | −0.022 (3) | −0.008 (3) | 0.005 (3) |
C261 | 0.117 (4) | 0.071 (3) | 0.043 (3) | 0.001 (3) | −0.015 (3) | −0.015 (3) |
C321 | 0.069 (3) | 0.075 (3) | 0.042 (3) | 0.002 (3) | −0.006 (2) | −0.002 (2) |
C361 | 0.069 (3) | 0.077 (3) | 0.060 (3) | 0.012 (3) | −0.002 (3) | −0.019 (3) |
Geometric parameters (Å, º) top
Rh—C10 | 1.805 (5) | C21—C22 | 1.388 (5) |
Rh—O4 | 2.029 (3) | C21—C26 | 1.390 (6) |
Rh—N | 2.091 (3) | C22—C23 | 1.386 (6) |
Rh—P | 2.1982 (13) | C22—C221 | 1.507 (6) |
P—O2 | 1.596 (3) | C23—C24 | 1.359 (7) |
P—O3 | 1.597 (3) | C23—H23 | 0.93 |
P—O1 | 1.610 (3) | C24—C25 | 1.361 (7) |
N—C1 | 1.322 (5) | C24—H24 | 0.93 |
N—C9 | 1.367 (5) | C25—C26 | 1.393 (6) |
O1—C11 | 1.418 (4) | C25—H25 | 0.93 |
O2—C21 | 1.409 (4) | C26—C261 | 1.500 (6) |
O3—C31 | 1.416 (4) | C31—C32 | 1.383 (5) |
O4—C8 | 1.322 (5) | C31—C36 | 1.393 (5) |
O5—C10 | 1.146 (5) | C32—C33 | 1.388 (6) |
C1—C2 | 1.408 (6) | C32—C321 | 1.504 (6) |
C1—H1 | 0.93 | C33—C34 | 1.373 (6) |
C2—C3 | 1.334 (7) | C33—H33 | 0.93 |
C2—H2 | 0.93 | C34—C35 | 1.365 (6) |
C3—C4 | 1.412 (7) | C34—H34 | 0.93 |
C3—H3 | 0.93 | C35—C36 | 1.384 (6) |
C4—C5 | 1.396 (8) | C35—H35 | 0.93 |
C4—C9 | 1.407 (6) | C36—C361 | 1.498 (6) |
C5—C6 | 1.364 (8) | C121—H12A | 0.96 |
C5—H5 | 0.93 | C121—H12B | 0.96 |
C6—C7 | 1.403 (7) | C121—H12C | 0.96 |
C6—H6 | 0.93 | C161—H16A | 0.96 |
C7—C8 | 1.372 (6) | C161—H16B | 0.96 |
C7—H7 | 0.93 | C161—H16C | 0.96 |
C8—C9 | 1.428 (6) | C221—H22A | 0.96 |
C11—C12 | 1.380 (6) | C221—H22B | 0.96 |
C11—C16 | 1.389 (5) | C221—H22C | 0.96 |
C12—C13 | 1.394 (6) | C261—H26A | 0.96 |
C12—C121 | 1.496 (6) | C261—H26B | 0.96 |
C13—C14 | 1.375 (7) | C261—H26C | 0.96 |
C13—H13 | 0.93 | C321—H32A | 0.96 |
C14—C15 | 1.356 (7) | C321—H32B | 0.96 |
C14—H14 | 0.93 | C321—H32C | 0.96 |
C15—C16 | 1.395 (6) | C361—H36A | 0.96 |
C15—H15 | 0.93 | C361—H36B | 0.96 |
C16—C161 | 1.490 (6) | C361—H36C | 0.96 |
| | | |
C10—Rh—O4 | 174.78 (15) | C23—C22—C221 | 121.2 (4) |
C10—Rh—N | 97.11 (16) | C21—C22—C221 | 122.0 (4) |
O4—Rh—N | 80.34 (13) | C24—C23—C22 | 121.5 (5) |
C10—Rh—P | 90.31 (13) | C24—C23—H23 | 119.3 |
O4—Rh—P | 92.87 (8) | C22—C23—H23 | 119.3 |
N—Rh—P | 169.17 (9) | C23—C24—C25 | 120.5 (5) |
O2—P—O3 | 97.54 (14) | C23—C24—H24 | 119.7 |
O2—P—O1 | 101.26 (13) | C25—C24—H24 | 119.7 |
O3—P—O1 | 104.99 (14) | C24—C25—C26 | 121.4 (5) |
O2—P—Rh | 118.07 (11) | C24—C25—H25 | 119.3 |
O3—P—Rh | 114.36 (10) | C26—C25—H25 | 119.3 |
O1—P—Rh | 117.80 (11) | C21—C26—C25 | 116.4 (4) |
C1—N—C9 | 118.5 (4) | C21—C26—C261 | 121.9 (4) |
C1—N—Rh | 130.0 (3) | C25—C26—C261 | 121.7 (4) |
C9—N—Rh | 111.5 (2) | C32—C31—C36 | 123.2 (4) |
C11—O1—P | 126.5 (2) | C32—C31—O3 | 118.3 (4) |
C21—O2—P | 133.6 (2) | C36—C31—O3 | 118.3 (4) |
C31—O3—P | 127.4 (2) | C31—C32—C33 | 117.5 (4) |
C8—O4—Rh | 113.7 (3) | C31—C32—C321 | 121.3 (4) |
N—C1—C2 | 121.5 (5) | C33—C32—C321 | 121.1 (4) |
N—C1—H1 | 119.3 | C34—C33—C32 | 120.7 (4) |
C2—C1—H1 | 119.3 | C34—C33—H33 | 119.6 |
C3—C2—C1 | 120.2 (5) | C32—C33—H33 | 119.6 |
C3—C2—H2 | 119.9 | C35—C34—C33 | 119.9 (5) |
C1—C2—H2 | 119.9 | C35—C34—H34 | 120 |
C2—C3—C4 | 121.0 (5) | C33—C34—H34 | 120 |
C2—C3—H3 | 119.5 | C34—C35—C36 | 122.3 (5) |
C4—C3—H3 | 119.5 | C34—C35—H35 | 118.9 |
C5—C4—C9 | 119.0 (5) | C36—C35—H35 | 118.9 |
C5—C4—C3 | 125.4 (5) | C35—C36—C31 | 116.1 (4) |
C9—C4—C3 | 115.5 (5) | C35—C36—C361 | 121.3 (4) |
C6—C5—C4 | 119.6 (5) | C31—C36—C361 | 122.6 (4) |
C6—C5—H5 | 120.2 | C12—C121—H12A | 109.5 |
C4—C5—H5 | 120.2 | C12—C121—H12B | 109.5 |
C5—C6—C7 | 122.0 (6) | H12A—C121—H12B | 109.5 |
C5—C6—H6 | 119 | C12—C121—H12C | 109.5 |
C7—C6—H6 | 119 | H12A—C121—H12C | 109.5 |
C8—C7—C6 | 120.2 (5) | H12B—C121—H12C | 109.5 |
C8—C7—H7 | 119.9 | C16—C161—H16A | 109.5 |
C6—C7—H7 | 119.9 | C16—C161—H16B | 109.5 |
O4—C8—C7 | 123.2 (4) | H16A—C161—H16B | 109.5 |
O4—C8—C9 | 118.6 (4) | C16—C161—H16C | 109.5 |
C7—C8—C9 | 118.2 (4) | H16A—C161—H16C | 109.5 |
N—C9—C4 | 123.3 (4) | H16B—C161—H16C | 109.5 |
N—C9—C8 | 115.9 (4) | C22—C221—H22A | 109.5 |
C4—C9—C8 | 120.9 (5) | C22—C221—H22B | 109.5 |
O5—C10—Rh | 177.6 (4) | H22A—C221—H22B | 109.5 |
C12—C11—C16 | 124.0 (4) | C22—C221—H22C | 109.5 |
C12—C11—O1 | 116.7 (4) | H22A—C221—H22C | 109.5 |
C16—C11—O1 | 119.1 (4) | H22B—C221—H22C | 109.5 |
C11—C12—C13 | 116.2 (4) | C26—C261—H26A | 109.5 |
C11—C12—C121 | 122.5 (4) | C26—C261—H26B | 109.5 |
C13—C12—C121 | 121.3 (4) | H26A—C261—H26B | 109.5 |
C14—C13—C12 | 121.5 (5) | C26—C261—H26C | 109.5 |
C14—C13—H13 | 119.2 | H26A—C261—H26C | 109.5 |
C12—C13—H13 | 119.2 | H26B—C261—H26C | 109.5 |
C15—C14—C13 | 120.3 (5) | C32—C321—H32A | 109.5 |
C15—C14—H14 | 119.8 | C32—C321—H32B | 109.5 |
C13—C14—H14 | 119.8 | H32A—C321—H32B | 109.5 |
C14—C15—C16 | 121.3 (5) | C32—C321—H32C | 109.5 |
C14—C15—H15 | 119.3 | H32A—C321—H32C | 109.5 |
C16—C15—H15 | 119.3 | H32B—C321—H32C | 109.5 |
C11—C16—C15 | 116.6 (4) | C36—C361—H36A | 109.5 |
C11—C16—C161 | 123.9 (4) | C36—C361—H36B | 109.5 |
C15—C16—C161 | 119.4 (4) | H36A—C361—H36B | 109.5 |
C22—C21—C26 | 123.3 (4) | C36—C361—H36C | 109.5 |
C22—C21—O2 | 117.4 (4) | H36A—C361—H36C | 109.5 |
C26—C21—O2 | 118.9 (4) | H36B—C361—H36C | 109.5 |
C23—C22—C21 | 116.8 (4) | | |
| | | |
O1—P—Rh—C10 | −130.17 (18) | O3—P—Rh—C10 | −6.13 (17) |
O2—P—Rh—C10 | 107.74 (18) | | |
Comparative geometrical data (Å, °) for [Rh(OX)(CO)(PR3)] complexes topR | Rh—P | Rh—N | Rh—O | N—Rh—O≡0 | ΘE (Å) | 1JRhP (Hz) |
O(2,6-DMP)a | 2.198 (1) | 2.091 (3) | 2.029 (3) | 80.3 (1) | 183 | 280 |
OPhb | 2.186 (1) | 2.097 (2) | 2.022 (2) | 80.8c | 154 | 281 |
Phd | 2.261 (2) | 2.098 (9) | 2.042 (5) | 80.0 (3) | 153 | 161 |
Phe | 2.317 (2) | 2.084 (7) | 2.037 (4) | 81.2 (2) | 153 | 163 |
References: (a) this work (2,6-DMP = 2,6-dimethylphenyl); (b) Simanko et al.
(2000); (c) data extracted from the Cambridge Structural Database
(Allen, 2002), no s.u. values; (d) Leipoldt et al. (1981); (v)
van Aswegen et al. (1991); RhIII iodomethane oxidative addition
product containing apical trans methyl and iodo ligands. |