The title compound, [RhCl{P(OC8H9)3}2(CO)], where P(OC8H9)3 is tris(2,6-dimethylphenyl)phosphite, crystallizes with two independent molecules, both disordered over inversion centres. The Rh1-P1 and Rh2-P2 bond distances are 2.3097 (7) and 2.2995 (7) Å, respectively. The effective cone angle for the phosphite ligands was calculated as 182°.
Supporting information
CCDC reference: 238668
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.005 Å
- R factor = 0.044
- wR factor = 0.093
- Data-to-parameter ratio = 19.5
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.64 Ratio
PLAT241_ALERT_2_C Check High U(eq) as Compared to Neighbors .... O2
PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... C22
PLAT301_ALERT_3_C Main Residue Disorder ......................... 5.00 Perc.
PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 2.30 Deg.
C1 -CL1 -RH1 1.555 1.555 1.555
PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 5.60 Deg.
CL1 -C1 -O1 1.555 1.555 1.555
PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 6.50 Deg.
CL1 -O1 -C1 1.555 1.555 1.555
PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 4.90 Deg.
C2 -CL2 -RH2 1.555 1.555 1.555
PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 6.10 Deg.
CL2 -C2 -O2 1.555 1.555 1.555
PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 6.90 Deg.
CL2 -O2 -C2 1.555 1.555 1.555
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 2
C49 H54 Cl O7 P2 Rh
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
12 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
9 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
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).
Crystal data top
[RhCl(C48H54O6P2)(CO)] | Z = 2 |
Mr = 955.22 | F(000) = 992 |
Triclinic, P1 | Dx = 1.386 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 12.3892 (5) Å | Cell parameters from 997 reflections |
b = 13.1262 (5) Å | θ = 2.3–19.9° |
c = 14.6675 (6) Å | µ = 0.55 mm−1 |
α = 83.685 (2)° | T = 293 K |
β = 89.773 (2)° | Plates, yellow |
γ = 75.016 (2)° | 0.26 × 0.12 × 0.07 mm |
V = 2289.45 (16) Å3 | |
Data collection top
Bruker SMART 1K CCD diffractometer | Rint = 0.070 |
Radiation source: fine focus sealed tube | θmax = 28.3°, θmin = 1.4° |
ω scans | h = −14→16 |
27501 measured reflections | k = −17→16 |
11343 independent reflections | l = −19→19 |
6184 reflections with I > 2σ(I) | |
Refinement top
Refinement on F2 | 0 restraints |
Least-squares matrix: full | H-atom parameters constrained |
R[F2 > 2σ(F2)] = 0.044 | w = 1/[σ2(Fo2) + (0.0332P)2] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.093 | (Δ/σ)max < 0.001 |
S = 0.91 | Δρmax = 0.35 e Å−3 |
11343 reflections | Δρmin = −0.44 e Å−3 |
583 parameters | |
Special details top
Experimental. The intensity data were collected on a Siemens SMART CCD 1 K
diffractometer using an exposure time of 20 s/frame. A total of 2231 frames were collected
with a frame width of 0.3° covering up to θ = 28.3° with 99.4% completeness
accomplished. The first 50 frames were recollected at the end of the 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 | Occ. (<1) |
Rh1 | 0 | 0 | 0.5 | 0.03602 (10) | |
Rh2 | −0.5 | −0.5 | 0 | 0.03565 (10) | |
P1 | 0.15281 (6) | 0.06726 (6) | 0.51628 (5) | 0.03622 (19) | |
Cl1 | −0.0251 (4) | 0.0747 (4) | 0.3437 (2) | 0.0517 (11) | 0.5 |
O23 | −0.34970 (15) | −0.35303 (16) | −0.10108 (12) | 0.0417 (5) | |
O13 | 0.17393 (15) | 0.14038 (15) | 0.42755 (12) | 0.0401 (5) | |
O22 | −0.32557 (15) | −0.35156 (15) | 0.06128 (12) | 0.0424 (5) | |
O12 | 0.15823 (15) | 0.14727 (15) | 0.58964 (13) | 0.0441 (5) | |
O21 | −0.22971 (15) | −0.51601 (16) | −0.00752 (12) | 0.0427 (5) | |
O11 | 0.26965 (14) | −0.02083 (15) | 0.53548 (12) | 0.0389 (5) | |
C36 | 0.1069 (3) | 0.3291 (3) | 0.4256 (2) | 0.0520 (9) | |
C62 | −0.4104 (3) | −0.1644 (3) | −0.0916 (2) | 0.0595 (9) | |
C61 | −0.3281 (3) | −0.2519 (3) | −0.11272 (19) | 0.0464 (8) | |
C31 | 0.1963 (3) | 0.2415 (3) | 0.42262 (19) | 0.0456 (8) | |
C621 | −0.5225 (3) | −0.1735 (3) | −0.0549 (3) | 0.0764 (11) | |
H62A | −0.5446 | −0.2286 | −0.082 | 0.115* | |
H62B | −0.5774 | −0.1073 | −0.07 | 0.115* | |
H62C | −0.5163 | −0.1905 | 0.0106 | 0.115* | |
C361 | −0.0112 (3) | 0.3209 (3) | 0.4347 (2) | 0.0699 (11) | |
H36A | −0.0253 | 0.274 | 0.393 | 0.105* | |
H36B | −0.0616 | 0.3899 | 0.4204 | 0.105* | |
H36C | −0.0223 | 0.2934 | 0.4964 | 0.105* | |
P2 | −0.34817 (6) | −0.42937 (6) | −0.00844 (5) | 0.0364 (2) | |
C41 | −0.2181 (2) | −0.6261 (3) | −0.0108 (2) | 0.0454 (8) | |
C32 | 0.3067 (3) | 0.2461 (3) | 0.4084 (2) | 0.0640 (10) | |
C35 | 0.1310 (4) | 0.4268 (3) | 0.4170 (2) | 0.0727 (12) | |
H35 | 0.0732 | 0.4878 | 0.4194 | 0.087* | |
C46 | −0.1805 (2) | −0.6945 (3) | 0.0688 (2) | 0.0503 (8) | |
C12 | 0.2952 (2) | −0.1688 (3) | 0.4450 (2) | 0.0462 (8) | |
C42 | −0.2366 (3) | −0.6619 (3) | −0.0935 (2) | 0.0526 (9) | |
C16 | 0.3044 (2) | −0.1973 (3) | 0.6121 (2) | 0.0439 (8) | |
C52 | −0.1648 (3) | −0.3884 (2) | 0.1626 (2) | 0.0499 (8) | |
C26 | 0.0772 (3) | 0.1476 (3) | 0.7375 (2) | 0.0565 (9) | |
C21 | 0.1727 (3) | 0.1307 (2) | 0.6854 (2) | 0.0457 (8) | |
C161 | 0.3068 (3) | −0.1562 (2) | 0.70397 (19) | 0.0540 (9) | |
H16A | 0.3127 | −0.2134 | 0.752 | 0.081* | |
H16B | 0.2393 | −0.102 | 0.7105 | 0.081* | |
H16C | 0.37 | −0.1271 | 0.7079 | 0.081* | |
C15 | 0.3256 (3) | −0.3056 (3) | 0.6065 (2) | 0.0608 (9) | |
H15 | 0.3372 | −0.3523 | 0.6602 | 0.073* | |
C421 | −0.2642 (3) | −0.5885 (3) | −0.1813 (2) | 0.0651 (10) | |
H42A | −0.3329 | −0.5357 | −0.1749 | 0.098* | |
H42B | −0.2723 | −0.6285 | −0.2306 | 0.098* | |
H42C | −0.2051 | −0.5545 | −0.1943 | 0.098* | |
C45 | −0.1668 (3) | −0.8021 (3) | 0.0637 (3) | 0.0682 (11) | |
H45 | −0.1409 | −0.8502 | 0.1152 | 0.082* | |
C121 | 0.2857 (3) | −0.0967 (3) | 0.3566 (2) | 0.0578 (9) | |
H12A | 0.2108 | −0.0522 | 0.3484 | 0.087* | |
H12B | 0.3031 | −0.1387 | 0.3062 | 0.087* | |
H12C | 0.337 | −0.0533 | 0.3586 | 0.087* | |
C56 | −0.3531 (3) | −0.3645 (3) | 0.2230 (2) | 0.0552 (9) | |
C13 | 0.3156 (3) | −0.2778 (3) | 0.4441 (2) | 0.0622 (10) | |
H13 | 0.32 | −0.3056 | 0.3881 | 0.075* | |
C51 | −0.2791 (3) | −0.3722 (2) | 0.15140 (19) | 0.0427 (7) | |
C11 | 0.2864 (2) | −0.1306 (2) | 0.5302 (2) | 0.0381 (7) | |
C53 | −0.1240 (3) | −0.4041 (3) | 0.2519 (3) | 0.0686 (11) | |
H53 | −0.0476 | −0.4162 | 0.2627 | 0.082* | |
C23 | 0.2884 (4) | 0.1007 (3) | 0.8180 (3) | 0.0896 (14) | |
H23 | 0.3586 | 0.0871 | 0.8462 | 0.108* | |
C54 | −0.1928 (4) | −0.4025 (3) | 0.3244 (3) | 0.0833 (14) | |
H54 | −0.1626 | −0.4152 | 0.3838 | 0.1* | |
C14 | 0.3296 (3) | −0.3449 (3) | 0.5234 (3) | 0.0728 (11) | |
H14 | 0.3418 | −0.4175 | 0.5212 | 0.087* | |
C44 | −0.1908 (3) | −0.8391 (3) | −0.0155 (3) | 0.0770 (12) | |
H44 | −0.1846 | −0.9111 | −0.0163 | 0.092* | |
C22 | 0.2795 (3) | 0.1117 (3) | 0.7230 (3) | 0.0597 (9) | |
C55 | −0.3053 (4) | −0.3824 (3) | 0.3113 (2) | 0.0766 (12) | |
H55 | −0.351 | −0.3805 | 0.3618 | 0.092* | |
C461 | −0.1546 (3) | −0.6529 (3) | 0.1562 (2) | 0.0662 (10) | |
H46A | −0.1233 | −0.7115 | 0.2016 | 0.099* | |
H46B | −0.2222 | −0.6098 | 0.1785 | 0.099* | |
H46C | −0.1021 | −0.6111 | 0.1439 | 0.099* | |
C521 | −0.0887 (3) | −0.3838 (3) | 0.0831 (2) | 0.0652 (10) | |
H52A | −0.0751 | −0.4487 | 0.0554 | 0.098* | |
H52B | −0.0192 | −0.3744 | 0.1045 | 0.098* | |
H52C | −0.1233 | −0.3252 | 0.0386 | 0.098* | |
C261 | −0.0375 (3) | 0.1871 (3) | 0.6939 (3) | 0.0864 (13) | |
H26A | −0.0914 | 0.1701 | 0.7361 | 0.13* | |
H26B | −0.0402 | 0.1537 | 0.6392 | 0.13* | |
H26C | −0.0543 | 0.2626 | 0.6786 | 0.13* | |
C221 | 0.3797 (3) | 0.1076 (3) | 0.6639 (3) | 0.0948 (15) | |
H22A | 0.4429 | 0.1082 | 0.7014 | 0.142* | |
H22B | 0.3642 | 0.1682 | 0.6183 | 0.142* | |
H22C | 0.3961 | 0.0438 | 0.6343 | 0.142* | |
C561 | −0.4781 (3) | −0.3294 (3) | 0.2076 (3) | 0.0842 (13) | |
H56A | −0.5017 | −0.2533 | 0.1967 | 0.126* | |
H56B | −0.514 | −0.3531 | 0.261 | 0.126* | |
H56C | −0.4983 | −0.3593 | 0.1554 | 0.126* | |
C34 | 0.2384 (5) | 0.4361 (4) | 0.4049 (3) | 0.0886 (15) | |
H34 | 0.2525 | 0.5027 | 0.3999 | 0.106* | |
C33 | 0.3241 (4) | 0.3476 (4) | 0.4003 (3) | 0.0890 (14) | |
H33 | 0.3961 | 0.3551 | 0.3915 | 0.107* | |
C64 | −0.2865 (5) | −0.0574 (4) | −0.1424 (3) | 0.1037 (19) | |
H64 | −0.271 | 0.0086 | −0.1508 | 0.124* | |
C25 | 0.0925 (4) | 0.1336 (3) | 0.8318 (3) | 0.0824 (13) | |
H25 | 0.0307 | 0.1409 | 0.8691 | 0.099* | |
C43 | −0.2233 (3) | −0.7711 (3) | −0.0925 (3) | 0.0707 (11) | |
H43 | −0.2372 | −0.7978 | −0.1462 | 0.085* | |
C63 | −0.3868 (4) | −0.0664 (3) | −0.1063 (2) | 0.0828 (13) | |
H63 | −0.4392 | −0.0061 | −0.0915 | 0.099* | |
C24 | 0.1972 (6) | 0.1093 (3) | 0.8707 (3) | 0.0989 (17) | |
H24 | 0.206 | 0.0985 | 0.9343 | 0.119* | |
C66 | −0.2277 (3) | −0.2459 (3) | −0.1522 (2) | 0.0639 (10) | |
C661 | −0.1461 (3) | −0.3421 (4) | −0.1799 (2) | 0.0890 (14) | |
H66A | −0.0863 | −0.3214 | −0.2123 | 0.133* | |
H66B | −0.1832 | −0.3771 | −0.2191 | 0.133* | |
H66C | −0.1164 | −0.3897 | −0.1262 | 0.133* | |
C65 | −0.2097 (4) | −0.1448 (4) | −0.1660 (3) | 0.0950 (16) | |
H65 | −0.1435 | −0.1367 | −0.192 | 0.114* | |
C1 | −0.0196 (13) | 0.0573 (13) | 0.3842 (7) | 0.041 (3) | 0.5 |
O1 | −0.0226 (13) | 0.0927 (12) | 0.3103 (6) | 0.051 (2) | 0.5 |
Cl2 | −0.4409 (3) | −0.5807 (3) | 0.1511 (2) | 0.0489 (9) | 0.5 |
C321 | 0.3992 (3) | 0.1479 (4) | 0.3983 (3) | 0.1006 (15) | |
H32A | 0.3941 | 0.1264 | 0.3383 | 0.151* | |
H32B | 0.3923 | 0.0918 | 0.444 | 0.151* | |
H32C | 0.4702 | 0.1629 | 0.4063 | 0.151* | |
C2 | −0.4591 (11) | −0.5573 (11) | 0.1139 (7) | 0.042 (3) | 0.5 |
O2 | −0.4347 (11) | −0.5990 (11) | 0.1859 (5) | 0.066 (3) | 0.5 |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Rh1 | 0.03006 (19) | 0.0392 (2) | 0.0387 (2) | −0.01127 (16) | 0.00322 (14) | 0.00136 (15) |
Rh2 | 0.0330 (2) | 0.0402 (2) | 0.03330 (19) | −0.01044 (16) | −0.00138 (14) | 0.00040 (15) |
P1 | 0.0312 (4) | 0.0372 (5) | 0.0396 (4) | −0.0090 (4) | 0.0034 (3) | −0.0010 (3) |
Cl1 | 0.0542 (14) | 0.068 (3) | 0.036 (3) | −0.0291 (18) | −0.001 (3) | 0.011 (3) |
O23 | 0.0489 (12) | 0.0422 (14) | 0.0351 (11) | −0.0154 (10) | −0.0016 (9) | 0.0002 (9) |
O13 | 0.0427 (12) | 0.0394 (13) | 0.0388 (11) | −0.0135 (10) | 0.0034 (9) | 0.0003 (9) |
O22 | 0.0463 (12) | 0.0404 (14) | 0.0401 (12) | −0.0104 (10) | −0.0044 (9) | −0.0053 (9) |
O12 | 0.0462 (12) | 0.0449 (14) | 0.0401 (12) | −0.0101 (10) | 0.0033 (9) | −0.0043 (9) |
O21 | 0.0363 (11) | 0.0402 (14) | 0.0515 (13) | −0.0095 (10) | 0.0006 (9) | −0.0054 (10) |
O11 | 0.0359 (11) | 0.0358 (13) | 0.0452 (12) | −0.0095 (9) | −0.0004 (9) | −0.0040 (9) |
C36 | 0.081 (3) | 0.041 (2) | 0.0352 (17) | −0.019 (2) | −0.0050 (16) | 0.0011 (15) |
C62 | 0.082 (3) | 0.046 (3) | 0.049 (2) | −0.017 (2) | −0.0172 (18) | 0.0025 (17) |
C61 | 0.060 (2) | 0.048 (2) | 0.0344 (17) | −0.0242 (18) | −0.0098 (15) | 0.0053 (15) |
C31 | 0.057 (2) | 0.046 (2) | 0.0365 (17) | −0.0220 (18) | −0.0003 (14) | 0.0049 (14) |
C621 | 0.074 (3) | 0.054 (3) | 0.091 (3) | 0.004 (2) | −0.001 (2) | −0.011 (2) |
C361 | 0.063 (2) | 0.054 (3) | 0.079 (3) | 0.0060 (19) | 0.002 (2) | −0.0013 (19) |
P2 | 0.0344 (4) | 0.0388 (5) | 0.0359 (4) | −0.0097 (4) | 0.0003 (3) | −0.0036 (3) |
C41 | 0.0336 (17) | 0.044 (2) | 0.057 (2) | −0.0066 (15) | 0.0103 (15) | −0.0096 (17) |
C32 | 0.065 (2) | 0.072 (3) | 0.066 (2) | −0.040 (2) | 0.0048 (18) | 0.002 (2) |
C35 | 0.131 (4) | 0.044 (3) | 0.044 (2) | −0.027 (3) | −0.011 (2) | −0.0035 (17) |
C46 | 0.0433 (19) | 0.047 (2) | 0.058 (2) | −0.0095 (16) | 0.0067 (16) | −0.0018 (18) |
C12 | 0.0407 (18) | 0.050 (2) | 0.0476 (19) | −0.0097 (15) | 0.0028 (14) | −0.0084 (16) |
C42 | 0.048 (2) | 0.052 (2) | 0.060 (2) | −0.0140 (17) | 0.0200 (16) | −0.0146 (18) |
C16 | 0.0410 (18) | 0.045 (2) | 0.0452 (19) | −0.0114 (15) | −0.0041 (14) | −0.0046 (15) |
C52 | 0.056 (2) | 0.042 (2) | 0.054 (2) | −0.0131 (16) | −0.0138 (17) | −0.0106 (15) |
C26 | 0.073 (3) | 0.056 (2) | 0.048 (2) | −0.0272 (19) | 0.0097 (18) | −0.0149 (17) |
C21 | 0.057 (2) | 0.037 (2) | 0.0445 (19) | −0.0140 (16) | −0.0011 (16) | −0.0061 (14) |
C161 | 0.064 (2) | 0.049 (2) | 0.0470 (19) | −0.0136 (17) | −0.0028 (16) | 0.0008 (16) |
C15 | 0.076 (3) | 0.044 (2) | 0.059 (2) | −0.0120 (19) | −0.0093 (18) | 0.0016 (18) |
C421 | 0.071 (2) | 0.077 (3) | 0.050 (2) | −0.019 (2) | 0.0115 (18) | −0.0178 (19) |
C45 | 0.075 (3) | 0.044 (3) | 0.080 (3) | −0.011 (2) | 0.017 (2) | 0.008 (2) |
C121 | 0.064 (2) | 0.062 (2) | 0.047 (2) | −0.0156 (18) | 0.0096 (16) | −0.0062 (17) |
C56 | 0.070 (3) | 0.050 (2) | 0.052 (2) | −0.0249 (19) | 0.0079 (18) | −0.0106 (17) |
C13 | 0.079 (3) | 0.054 (3) | 0.054 (2) | −0.013 (2) | 0.0001 (18) | −0.0179 (19) |
C51 | 0.059 (2) | 0.0359 (19) | 0.0355 (17) | −0.0166 (15) | −0.0019 (15) | −0.0050 (13) |
C11 | 0.0292 (15) | 0.037 (2) | 0.0482 (19) | −0.0084 (13) | −0.0026 (13) | −0.0048 (15) |
C53 | 0.082 (3) | 0.053 (3) | 0.067 (3) | −0.010 (2) | −0.033 (2) | −0.0089 (19) |
C23 | 0.111 (4) | 0.049 (3) | 0.104 (4) | −0.010 (3) | −0.057 (3) | −0.010 (3) |
C54 | 0.136 (4) | 0.061 (3) | 0.044 (2) | −0.010 (3) | −0.030 (3) | −0.0036 (19) |
C14 | 0.104 (3) | 0.038 (2) | 0.077 (3) | −0.018 (2) | −0.007 (2) | −0.012 (2) |
C44 | 0.103 (3) | 0.045 (3) | 0.087 (3) | −0.023 (2) | 0.032 (3) | −0.018 (2) |
C22 | 0.061 (2) | 0.039 (2) | 0.078 (3) | −0.0069 (17) | −0.021 (2) | −0.0134 (18) |
C55 | 0.127 (4) | 0.062 (3) | 0.044 (2) | −0.029 (3) | 0.018 (2) | −0.0074 (18) |
C461 | 0.061 (2) | 0.066 (3) | 0.070 (2) | −0.0200 (19) | −0.0186 (18) | 0.0124 (19) |
C521 | 0.048 (2) | 0.078 (3) | 0.077 (3) | −0.0265 (19) | −0.0030 (18) | −0.019 (2) |
C261 | 0.061 (3) | 0.101 (4) | 0.109 (3) | −0.026 (2) | 0.033 (2) | −0.052 (3) |
C221 | 0.047 (2) | 0.092 (4) | 0.156 (4) | −0.017 (2) | −0.014 (3) | −0.057 (3) |
C561 | 0.080 (3) | 0.092 (3) | 0.092 (3) | −0.030 (3) | 0.035 (2) | −0.039 (2) |
C34 | 0.160 (5) | 0.073 (3) | 0.055 (3) | −0.076 (4) | −0.012 (3) | 0.005 (2) |
C33 | 0.105 (4) | 0.110 (4) | 0.077 (3) | −0.076 (3) | 0.003 (3) | 0.001 (3) |
C64 | 0.181 (6) | 0.090 (4) | 0.066 (3) | −0.091 (4) | −0.029 (3) | 0.020 (3) |
C25 | 0.135 (4) | 0.073 (3) | 0.056 (3) | −0.052 (3) | 0.021 (3) | −0.017 (2) |
C43 | 0.084 (3) | 0.062 (3) | 0.073 (3) | −0.022 (2) | 0.032 (2) | −0.029 (2) |
C63 | 0.136 (4) | 0.051 (3) | 0.062 (3) | −0.032 (3) | −0.024 (3) | 0.009 (2) |
C24 | 0.181 (6) | 0.067 (3) | 0.052 (3) | −0.043 (4) | −0.020 (3) | 0.002 (2) |
C66 | 0.066 (2) | 0.091 (3) | 0.0424 (19) | −0.043 (2) | −0.0042 (17) | 0.0130 (19) |
C661 | 0.059 (3) | 0.143 (4) | 0.067 (3) | −0.037 (3) | 0.017 (2) | 0.005 (3) |
C65 | 0.123 (4) | 0.127 (5) | 0.061 (3) | −0.092 (4) | −0.010 (3) | 0.023 (3) |
C1 | 0.037 (5) | 0.046 (7) | 0.046 (8) | −0.020 (4) | 0.005 (7) | 0.000 (7) |
O1 | 0.056 (4) | 0.069 (5) | 0.033 (6) | −0.033 (3) | −0.003 (5) | 0.019 (5) |
Cl2 | 0.0547 (19) | 0.054 (3) | 0.036 (3) | −0.0192 (17) | −0.016 (2) | 0.014 (2) |
C321 | 0.053 (3) | 0.129 (4) | 0.128 (4) | −0.040 (3) | 0.027 (2) | −0.011 (3) |
C2 | 0.037 (5) | 0.051 (7) | 0.037 (7) | −0.015 (5) | −0.007 (5) | 0.011 (5) |
O2 | 0.068 (4) | 0.087 (6) | 0.041 (6) | −0.027 (4) | −0.026 (5) | 0.025 (5) |
Geometric parameters (Å, º) top
Rh1—C1 | 1.771 (9) | C15—C14 | 1.371 (4) |
Rh1—C1i | 1.771 (9) | C15—H15 | 0.93 |
Rh1—P1i | 2.3097 (7) | C421—H42A | 0.96 |
Rh1—P1 | 2.3097 (7) | C421—H42B | 0.96 |
Rh1—Cl1 | 2.380 (3) | C421—H42C | 0.96 |
Rh1—Cl1i | 2.380 (3) | C45—C44 | 1.368 (5) |
Rh2—C2ii | 1.773 (8) | C45—H45 | 0.93 |
Rh2—C2 | 1.773 (8) | C121—H12A | 0.96 |
Rh2—P2 | 2.2995 (7) | C121—H12B | 0.96 |
Rh2—P2ii | 2.2995 (7) | C121—H12C | 0.96 |
Rh2—Cl2ii | 2.379 (3) | C56—C51 | 1.387 (4) |
Rh2—Cl2 | 2.379 (3) | C56—C55 | 1.396 (5) |
P1—O13 | 1.5923 (19) | C56—C561 | 1.508 (5) |
P1—O12 | 1.597 (2) | C13—C14 | 1.363 (5) |
P1—O11 | 1.6056 (19) | C13—H13 | 0.93 |
Cl1—O1 | 0.525 (7) | C53—C54 | 1.359 (5) |
Cl1—C1 | 0.610 (8) | C53—H53 | 0.93 |
O23—C61 | 1.413 (3) | C23—C24 | 1.354 (6) |
O23—P2 | 1.5943 (19) | C23—C22 | 1.387 (5) |
O13—C31 | 1.419 (3) | C23—H23 | 0.93 |
O22—C51 | 1.414 (3) | C54—C55 | 1.360 (5) |
O22—P2 | 1.596 (2) | C54—H54 | 0.93 |
O12—C21 | 1.402 (3) | C14—H14 | 0.93 |
O21—C41 | 1.422 (3) | C44—C43 | 1.353 (5) |
O21—P2 | 1.607 (2) | C44—H44 | 0.93 |
O11—C11 | 1.413 (3) | C22—C221 | 1.504 (5) |
C36—C31 | 1.379 (4) | C55—H55 | 0.93 |
C36—C35 | 1.383 (4) | C461—H46A | 0.96 |
C36—C361 | 1.499 (4) | C461—H46B | 0.96 |
C62—C63 | 1.386 (5) | C461—H46C | 0.96 |
C62—C61 | 1.387 (4) | C521—H52A | 0.96 |
C62—C621 | 1.516 (5) | C521—H52B | 0.96 |
C61—C66 | 1.387 (4) | C521—H52C | 0.96 |
C31—C32 | 1.398 (4) | C261—H26A | 0.96 |
C621—H62A | 0.96 | C261—H26B | 0.96 |
C621—H62B | 0.96 | C261—H26C | 0.96 |
C621—H62C | 0.96 | C221—H22A | 0.96 |
C361—H36A | 0.96 | C221—H22B | 0.96 |
C361—H36B | 0.96 | C221—H22C | 0.96 |
C361—H36C | 0.96 | C561—H56A | 0.96 |
C41—C42 | 1.388 (4) | C561—H56B | 0.96 |
C41—C46 | 1.395 (4) | C561—H56C | 0.96 |
C32—C33 | 1.396 (5) | C34—C33 | 1.364 (6) |
C32—C321 | 1.509 (5) | C34—H34 | 0.93 |
C35—C34 | 1.375 (5) | C33—H33 | 0.93 |
C35—H35 | 0.93 | C64—C65 | 1.365 (6) |
C46—C45 | 1.389 (4) | C64—C63 | 1.377 (6) |
C46—C461 | 1.513 (4) | C64—H64 | 0.93 |
C12—C13 | 1.388 (4) | C25—C24 | 1.364 (6) |
C12—C11 | 1.391 (4) | C25—H25 | 0.93 |
C12—C121 | 1.504 (4) | C43—H43 | 0.93 |
C42—C43 | 1.399 (4) | C63—H63 | 0.93 |
C42—C421 | 1.504 (4) | C24—H24 | 0.93 |
C16—C15 | 1.389 (4) | C66—C65 | 1.395 (5) |
C16—C11 | 1.389 (4) | C66—C661 | 1.494 (5) |
C16—C161 | 1.508 (4) | C661—H66A | 0.96 |
C52—C53 | 1.381 (4) | C661—H66B | 0.96 |
C52—C51 | 1.383 (4) | C661—H66C | 0.96 |
C52—C521 | 1.503 (4) | C65—H65 | 0.93 |
C26—C25 | 1.383 (5) | C1—O1 | 1.128 (12) |
C26—C21 | 1.388 (4) | Cl2—O2 | 0.537 (7) |
C26—C261 | 1.500 (5) | Cl2—C2 | 0.609 (7) |
C21—C22 | 1.387 (4) | C321—H32A | 0.96 |
C161—H16A | 0.96 | C321—H32B | 0.96 |
C161—H16B | 0.96 | C321—H32C | 0.96 |
C161—H16C | 0.96 | C2—O2 | 1.139 (11) |
| | | |
C1—Rh1—C1i | 180.000 (2) | C44—C45—H45 | 119.3 |
C1—Rh1—P1i | 89.3 (5) | C46—C45—H45 | 119.3 |
C1i—Rh1—P1i | 90.7 (5) | C12—C121—H12A | 109.5 |
C1—Rh1—P1 | 90.7 (5) | C12—C121—H12B | 109.5 |
C1i—Rh1—P1 | 89.3 (5) | H12A—C121—H12B | 109.5 |
P1i—Rh1—P1 | 180.00 (4) | C12—C121—H12C | 109.5 |
C1—Rh1—Cl1 | 0.8 (6) | H12A—C121—H12C | 109.5 |
C1i—Rh1—Cl1 | 179.2 (6) | H12B—C121—H12C | 109.5 |
P1i—Rh1—Cl1 | 89.20 (11) | C51—C56—C55 | 116.0 (3) |
P1—Rh1—Cl1 | 90.80 (11) | C51—C56—C561 | 122.5 (3) |
C1—Rh1—Cl1i | 179.2 (6) | C55—C56—C561 | 121.2 (3) |
C1i—Rh1—Cl1i | 0.8 (6) | C14—C13—C12 | 121.4 (3) |
P1i—Rh1—Cl1i | 90.80 (11) | C14—C13—H13 | 119.3 |
P1—Rh1—Cl1i | 89.20 (11) | C12—C13—H13 | 119.3 |
Cl1—Rh1—Cl1i | 180.0000 (10) | C52—C51—C56 | 124.2 (3) |
C2ii—Rh2—C2 | 180.0 (9) | C52—C51—O22 | 118.4 (3) |
C2ii—Rh2—P2 | 90.0 (5) | C56—C51—O22 | 117.1 (3) |
C2—Rh2—P2 | 90.0 (5) | C16—C11—C12 | 122.6 (3) |
C2ii—Rh2—P2ii | 90.0 (5) | C16—C11—O11 | 117.4 (3) |
C2—Rh2—P2ii | 90.0 (5) | C12—C11—O11 | 119.8 (3) |
P2—Rh2—P2ii | 180 | C54—C53—C52 | 121.6 (4) |
C2ii—Rh2—Cl2ii | 1.7 (5) | C54—C53—H53 | 119.2 |
C2—Rh2—Cl2ii | 178.3 (5) | C52—C53—H53 | 119.2 |
P2—Rh2—Cl2ii | 90.39 (10) | C24—C23—C22 | 121.5 (4) |
P2ii—Rh2—Cl2ii | 89.61 (10) | C24—C23—H23 | 119.2 |
C2ii—Rh2—Cl2 | 178.3 (5) | C22—C23—H23 | 119.2 |
C2—Rh2—Cl2 | 1.7 (5) | C53—C54—C55 | 120.9 (4) |
P2—Rh2—Cl2 | 89.61 (10) | C53—C54—H54 | 119.6 |
P2ii—Rh2—Cl2 | 90.39 (10) | C55—C54—H54 | 119.6 |
Cl2ii—Rh2—Cl2 | 180.00 (19) | C13—C14—C15 | 120.1 (4) |
O13—P1—O12 | 97.30 (11) | C13—C14—H14 | 119.9 |
O13—P1—O11 | 104.23 (10) | C15—C14—H14 | 119.9 |
O12—P1—O11 | 102.13 (10) | C43—C44—C45 | 120.2 (4) |
O13—P1—Rh1 | 113.24 (8) | C43—C44—H44 | 119.9 |
O12—P1—Rh1 | 122.48 (7) | C45—C44—H44 | 119.9 |
O11—P1—Rh1 | 114.74 (8) | C23—C22—C21 | 116.4 (4) |
O1—Cl1—C1 | 168 (2) | C23—C22—C221 | 121.8 (4) |
O1—Cl1—Rh1 | 168 (2) | C21—C22—C221 | 121.7 (3) |
C1—Cl1—Rh1 | 2.3 (18) | C54—C55—C56 | 121.0 (4) |
C61—O23—P2 | 128.46 (17) | C54—C55—H55 | 119.5 |
C31—O13—P1 | 128.29 (17) | C56—C55—H55 | 119.5 |
C51—O22—P2 | 131.35 (18) | C46—C461—H46A | 109.5 |
C21—O12—P1 | 131.26 (18) | C46—C461—H46B | 109.5 |
C41—O21—P2 | 123.68 (17) | H46A—C461—H46B | 109.5 |
C11—O11—P1 | 125.21 (16) | C46—C461—H46C | 109.5 |
C31—C36—C35 | 116.5 (4) | H46A—C461—H46C | 109.5 |
C31—C36—C361 | 122.6 (3) | H46B—C461—H46C | 109.5 |
C35—C36—C361 | 120.9 (4) | C52—C521—H52A | 109.5 |
C63—C62—C61 | 117.2 (4) | C52—C521—H52B | 109.5 |
C63—C62—C621 | 120.5 (4) | H52A—C521—H52B | 109.5 |
C61—C62—C621 | 122.3 (3) | C52—C521—H52C | 109.5 |
C66—C61—C62 | 124.0 (3) | H52A—C521—H52C | 109.5 |
C66—C61—O23 | 116.8 (3) | H52B—C521—H52C | 109.5 |
C62—C61—O23 | 119.1 (3) | C26—C261—H26A | 109.5 |
C36—C31—C32 | 124.4 (3) | C26—C261—H26B | 109.5 |
C36—C31—O13 | 117.9 (3) | H26A—C261—H26B | 109.5 |
C32—C31—O13 | 117.5 (3) | C26—C261—H26C | 109.5 |
C62—C621—H62A | 109.5 | H26A—C261—H26C | 109.5 |
C62—C621—H62B | 109.5 | H26B—C261—H26C | 109.5 |
H62A—C621—H62B | 109.5 | C22—C221—H22A | 109.5 |
C62—C621—H62C | 109.5 | C22—C221—H22B | 109.5 |
H62A—C621—H62C | 109.5 | H22A—C221—H22B | 109.5 |
H62B—C621—H62C | 109.5 | C22—C221—H22C | 109.5 |
C36—C361—H36A | 109.5 | H22A—C221—H22C | 109.5 |
C36—C361—H36B | 109.5 | H22B—C221—H22C | 109.5 |
H36A—C361—H36B | 109.5 | C56—C561—H56A | 109.5 |
C36—C361—H36C | 109.5 | C56—C561—H56B | 109.5 |
H36A—C361—H36C | 109.5 | H56A—C561—H56B | 109.5 |
H36B—C361—H36C | 109.5 | C56—C561—H56C | 109.5 |
O23—P2—O22 | 97.80 (11) | H56A—C561—H56C | 109.5 |
O23—P2—O21 | 104.39 (10) | H56B—C561—H56C | 109.5 |
O22—P2—O21 | 102.43 (10) | C33—C34—C35 | 119.9 (4) |
O23—P2—Rh2 | 112.15 (8) | C33—C34—H34 | 120 |
O22—P2—Rh2 | 123.18 (8) | C35—C34—H34 | 120 |
O21—P2—Rh2 | 114.29 (8) | C34—C33—C32 | 121.9 (4) |
C42—C41—C46 | 122.9 (3) | C34—C33—H33 | 119.1 |
C42—C41—O21 | 119.3 (3) | C32—C33—H33 | 119.1 |
C46—C41—O21 | 117.6 (3) | C65—C64—C63 | 120.3 (5) |
C33—C32—C31 | 115.5 (4) | C65—C64—H64 | 119.8 |
C33—C32—C321 | 122.7 (4) | C63—C64—H64 | 119.8 |
C31—C32—C321 | 121.7 (3) | C24—C25—C26 | 120.7 (4) |
C34—C35—C36 | 121.7 (4) | C24—C25—H25 | 119.7 |
C34—C35—H35 | 119.1 | C26—C25—H25 | 119.7 |
C36—C35—H35 | 119.1 | C44—C43—C42 | 121.7 (4) |
C45—C46—C41 | 116.9 (3) | C44—C43—H43 | 119.1 |
C45—C46—C461 | 121.9 (3) | C42—C43—H43 | 119.1 |
C41—C46—C461 | 121.3 (3) | C64—C63—C62 | 120.6 (5) |
C13—C12—C11 | 117.2 (3) | C64—C63—H63 | 119.7 |
C13—C12—C121 | 120.5 (3) | C62—C63—H63 | 119.7 |
C11—C12—C121 | 122.3 (3) | C23—C24—C25 | 120.9 (4) |
C41—C42—C43 | 116.7 (3) | C23—C24—H24 | 119.6 |
C41—C42—C421 | 122.2 (3) | C25—C24—H24 | 119.6 |
C43—C42—C421 | 121.0 (3) | C61—C66—C65 | 115.8 (4) |
C15—C16—C11 | 117.2 (3) | C61—C66—C661 | 121.4 (3) |
C15—C16—C161 | 120.3 (3) | C65—C66—C661 | 122.7 (4) |
C11—C16—C161 | 122.4 (3) | C66—C661—H66A | 109.5 |
C53—C52—C51 | 116.2 (3) | C66—C661—H66B | 109.5 |
C53—C52—C521 | 121.0 (3) | H66A—C661—H66B | 109.5 |
C51—C52—C521 | 122.7 (3) | C66—C661—H66C | 109.5 |
C25—C26—C21 | 117.0 (4) | H66A—C661—H66C | 109.5 |
C25—C26—C261 | 121.1 (4) | H66B—C661—H66C | 109.5 |
C21—C26—C261 | 121.7 (3) | C64—C65—C66 | 121.9 (5) |
C22—C21—C26 | 123.1 (3) | C64—C65—H65 | 119 |
C22—C21—O12 | 118.8 (3) | C66—C65—H65 | 119 |
C26—C21—O12 | 117.5 (3) | Cl1—C1—O1 | 5.6 (9) |
C16—C161—H16A | 109.5 | Cl1—C1—Rh1 | 177 (2) |
C16—C161—H16B | 109.5 | O1—C1—Rh1 | 174.2 (19) |
H16A—C161—H16B | 109.5 | Cl1—O1—C1 | 6.5 (11) |
C16—C161—H16C | 109.5 | O2—Cl2—C2 | 167 (2) |
H16A—C161—H16C | 109.5 | O2—Cl2—Rh2 | 170.5 (18) |
H16B—C161—H16C | 109.5 | C2—Cl2—Rh2 | 4.9 (16) |
C14—C15—C16 | 121.2 (3) | C32—C321—H32A | 109.5 |
C14—C15—H15 | 119.4 | C32—C321—H32B | 109.5 |
C16—C15—H15 | 119.4 | H32A—C321—H32B | 109.5 |
C42—C421—H42A | 109.5 | C32—C321—H32C | 109.5 |
C42—C421—H42B | 109.5 | H32A—C321—H32C | 109.5 |
H42A—C421—H42B | 109.5 | H32B—C321—H32C | 109.5 |
C42—C421—H42C | 109.5 | Cl2—C2—O2 | 6.1 (9) |
H42A—C421—H42C | 109.5 | Cl2—C2—Rh2 | 173 (2) |
H42B—C421—H42C | 109.5 | O2—C2—Rh2 | 176.1 (19) |
C44—C45—C46 | 121.5 (4) | Cl2—O2—C2 | 6.9 (10) |
| | | |
Cl1—Rh1—P1—O11 | −114.49 (15) | Cl2—Rh2—P2—O21 | 66.04 (13) |
Cl1—Rh1—P1—O12 | 120.93 (15) | Cl2—Rh2—P2—O22 | −59.21 (14) |
Cl1—Rh1—P1—O13 | 5.00 (15) | Cl2—Rh2—P2—O23 | −175.41 (13) |
Symmetry codes: (i) −x, −y, −z+1; (ii) −x−1, −y−1, −z. |
Comparative X-ray data for trans-[MCl(CO)(PX3)2] complexes. topX | M-P(Å) | M-Cl(Å) | P-M-P(°) | Cl-M-C(°) | ΘE(°) | Footnote |
O(2,6DMP) | 2.3097 (7) | 2.380 (3) | 180 | 179.2 (6) | 182 | TW |
| 2.2995 (7) | 2.379 (3) | 180 | 178.3 (5) | 182 | |
O(2tBP) | 2.286 | 2.370 | 180 | 175.85 | 181 | (i) |
Bz | 2.3164 (15) | 2.3654 (15) | 177.67 (6) | 178.55 (17) | 170 | (ii) |
| 2.3156 (16) | | | | 172 | |
(TW) This work;
(i) Fernández et al., 1998;
(ii) Muller et al., 2001;
2,6DMP = 2,6-dimethylphenyl;
2tBP = 2-tert-butylphenyl;
Bz = benzyl. |