In the structure of the title compound, [Rh
2(C
7F
7S)
2(C
8H
12)
2], important geometric parameters are Rh
Rh = 2.9595 (3) Å, mean Rh—S = 2.3949 (8) Å, mean S—C = 1.764 (3) Å and mean S—Rh—S = 87.37 (3)°. The S—Rh—S planes intersect at an angle of 117.4 (3)°.
Supporting information
CCDC reference: 289881
Key indicators
- Single-crystal X-ray study
- T = 193 K
- Mean (C-C) = 0.005 Å
- R factor = 0.022
- wR factor = 0.052
- Data-to-parameter ratio = 10.2
checkCIF/PLATON results
No syntax errors found
Alert level A
PLAT027_ALERT_3_A _diffrn_reflns_theta_full (too) Low ............ 23.25 Deg.
| Author Response: Data were truncated during integration to include
strongest reflection data only
|
Alert level B
THETM01_ALERT_3_B The value of sine(theta_max)/wavelength is less than 0.575
Calculated sin(theta_max)/wavelength = 0.5554
PLAT023_ALERT_3_B Resolution (too) Low [sin(th)/Lambda < 0.6]..... 23.25 Deg.
PLAT220_ALERT_2_B Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.52 Ratio
PLAT411_ALERT_2_B Short Inter H...H Contact H2A .. H2A .. 2.04 Ang.
Alert level C
ABSTY02_ALERT_1_C An _exptl_absorpt_correction_type has been given without
a literature citation. This should be contained in the
_exptl_absorpt_process_details field.
Absorption correction given as empirical
PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ?
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Rh1 - S1 .. 6.41 su
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Rh2 - S1 .. 5.37 su
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Rh2 - S2 .. 5.20 su
PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C12
PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C15
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C30
PLAT366_ALERT_2_C Short? C(sp?)-C(sp?) Bond C1 - C2 ... 1.39 Ang.
PLAT366_ALERT_2_C Short? C(sp?)-C(sp?) Bond C5 - C6 ... 1.39 Ang.
PLAT366_ALERT_2_C Short? C(sp?)-C(sp?) Bond C9 - C10 ... 1.39 Ang.
PLAT366_ALERT_2_C Short? C(sp?)-C(sp?) Bond C13 - C14 ... 1.38 Ang.
1 ALERT level A = In general: serious problem
4 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
12 ALERT type 2 Indicator that the structure model may be wrong or deficient
3 ALERT type 3 Indicator that the structure quality may be low
1 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Bruker, 1999); cell refinement: SMART; data reduction: SAINT (Bruker, 1999); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997a); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997a); molecular graphics: SHELXTL (Sheldrick, 1997b); software used to prepare material for publication: SHELXTL.
Bis[µ-2,3,5,6-tetrafluoro-4-(trifluoromethyl)benzenethiolato]bis[(
η4-3,5-
cyclooctadiene)rhodium(I)]
top
Crystal data top
[Rh2(C7F7S)2(C8H12)2] | F(000) = 1808 |
Mr = 920.43 | Dx = 1.994 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
a = 12.5718 (6) Å | Cell parameters from 4620 reflections |
b = 19.5538 (10) Å | θ = 5.3–46.5° |
c = 13.3217 (7) Å | µ = 1.32 mm−1 |
β = 110.547 (1)° | T = 193 K |
V = 3066.5 (3) Å3 | Prism, red |
Z = 4 | 0.32 × 0.32 × 0.28 mm |
Data collection top
Bruker SMART CCD area-detector diffractometer | 4402 independent reflections |
Radiation source: fine-focus sealed tube | 3998 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.018 |
φ and ω scans | θmax = 23.3°, θmin = 1.9° |
Absorption correction: empirical (using intensity measurements) (SADABS; Blessing, 1995) | h = −11→13 |
Tmin = 0.613, Tmax = 0.691 | k = −19→21 |
13638 measured reflections | l = −14→14 |
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)] = 0.022 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.052 | H-atom parameters constrained |
S = 1.04 | w = 1/[σ2(Fo2) + (0.0245P)2 + 3.0986P] where P = (Fo2 + 2Fc2)/3 |
4402 reflections | (Δ/σ)max = 0.001 |
433 parameters | Δρmax = 0.49 e Å−3 |
0 restraints | Δρmin = −0.37 e Å−3 |
Special details top
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. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor
wR and goodness of fit S are based on F2, conventional
R-factors R are based on F, with F set to zero for
negative F2. The threshold expression of F2 >
σ(F2) is used only for calculating R-factors(gt) 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 | |
Rh1 | 0.299170 (19) | 0.063465 (11) | 0.619365 (18) | 0.02570 (8) | |
Rh2 | 0.492581 (19) | 0.155319 (12) | 0.727738 (19) | 0.02720 (8) | |
S1 | 0.37572 (6) | 0.15247 (4) | 0.54169 (6) | 0.02695 (17) | |
S2 | 0.32286 (6) | 0.13912 (4) | 0.76730 (6) | 0.02850 (17) | |
F1 | −0.00623 (17) | 0.41026 (11) | 0.37866 (19) | 0.0661 (6) | |
F2 | 0.10615 (18) | 0.45205 (10) | 0.52583 (17) | 0.0588 (6) | |
F3 | 0.14734 (18) | 0.45926 (10) | 0.38458 (18) | 0.0588 (6) | |
F4 | 0.11881 (14) | 0.16866 (9) | 0.46015 (14) | 0.0370 (4) | |
F5 | −0.00023 (14) | 0.28158 (10) | 0.41338 (15) | 0.0442 (5) | |
F6 | 0.33969 (15) | 0.41114 (8) | 0.52715 (15) | 0.0421 (5) | |
F7 | 0.45852 (13) | 0.29763 (8) | 0.57411 (14) | 0.0371 (4) | |
F8 | −0.0877 (2) | 0.35743 (13) | 0.7383 (2) | 0.0826 (8) | |
F9 | 0.0283 (2) | 0.43276 (12) | 0.7277 (2) | 0.0768 (8) | |
F10 | −0.0777 (2) | 0.38418 (13) | 0.58649 (17) | 0.0738 (7) | |
F11 | 0.06951 (15) | 0.13386 (9) | 0.67580 (16) | 0.0452 (5) | |
F12 | −0.07679 (15) | 0.23532 (11) | 0.64595 (16) | 0.0518 (5) | |
F13 | 0.22897 (16) | 0.39312 (9) | 0.75109 (15) | 0.0467 (5) | |
F14 | 0.37305 (14) | 0.29210 (9) | 0.78140 (14) | 0.0378 (4) | |
C1 | 0.2573 (3) | 0.00369 (16) | 0.4766 (3) | 0.0361 (8) | |
H1A | 0.2509 | 0.0310 | 0.4113 | 0.043* | |
C2 | 0.3683 (3) | −0.01024 (15) | 0.5413 (3) | 0.0378 (8) | |
H2A | 0.4263 | 0.0089 | 0.5135 | 0.045* | |
C3 | 0.4060 (3) | −0.07504 (18) | 0.6064 (3) | 0.0537 (10) | |
H3A | 0.4843 | −0.0863 | 0.6108 | 0.064* | |
H3B | 0.3559 | −0.1132 | 0.5690 | 0.064* | |
C4 | 0.4033 (3) | −0.06880 (18) | 0.7191 (3) | 0.0558 (10) | |
H4A | 0.3883 | −0.1145 | 0.7432 | 0.067* | |
H4B | 0.4791 | −0.0539 | 0.7678 | 0.067* | |
C5 | 0.3156 (3) | −0.01958 (16) | 0.7291 (3) | 0.0421 (8) | |
H5A | 0.3276 | −0.0051 | 0.8043 | 0.051* | |
C6 | 0.2029 (3) | −0.01634 (16) | 0.6597 (3) | 0.0400 (8) | |
H6A | 0.1491 | 0.0007 | 0.6943 | 0.048* | |
C7 | 0.1498 (3) | −0.06637 (18) | 0.5688 (3) | 0.0512 (9) | |
H7A | 0.0692 | −0.0735 | 0.5605 | 0.061* | |
H7B | 0.1892 | −0.1109 | 0.5875 | 0.061* | |
C8 | 0.1562 (3) | −0.04175 (19) | 0.4627 (3) | 0.0523 (10) | |
H8A | 0.1602 | −0.0819 | 0.4190 | 0.063* | |
H8B | 0.0859 | −0.0163 | 0.4231 | 0.063* | |
C9 | 0.5891 (3) | 0.11520 (19) | 0.8827 (3) | 0.0468 (9) | |
H9A | 0.5425 | 0.0944 | 0.9222 | 0.056* | |
C10 | 0.5940 (3) | 0.18646 (19) | 0.8861 (3) | 0.0457 (9) | |
H10A | 0.5498 | 0.2078 | 0.9273 | 0.055* | |
C11 | 0.6929 (3) | 0.2285 (2) | 0.8838 (4) | 0.0673 (12) | |
H11A | 0.6731 | 0.2774 | 0.8854 | 0.081* | |
H11B | 0.7582 | 0.2190 | 0.9501 | 0.081* | |
C12 | 0.7294 (3) | 0.2176 (3) | 0.7919 (4) | 0.0761 (14) | |
H12A | 0.7995 | 0.1896 | 0.8158 | 0.091* | |
H12B | 0.7488 | 0.2625 | 0.7686 | 0.091* | |
C13 | 0.6438 (3) | 0.18309 (18) | 0.6972 (3) | 0.0430 (8) | |
H13A | 0.6293 | 0.2073 | 0.6275 | 0.052* | |
C14 | 0.6295 (3) | 0.11306 (18) | 0.6878 (3) | 0.0462 (9) | |
H14A | 0.6058 | 0.0965 | 0.6121 | 0.055* | |
C15 | 0.6912 (4) | 0.0605 (2) | 0.7677 (5) | 0.0835 (15) | |
H15A | 0.7719 | 0.0606 | 0.7736 | 0.100* | |
H15B | 0.6594 | 0.0150 | 0.7406 | 0.100* | |
C16 | 0.6857 (3) | 0.0703 (2) | 0.8769 (4) | 0.0709 (14) | |
H16A | 0.7584 | 0.0905 | 0.9236 | 0.085* | |
H16B | 0.6788 | 0.0248 | 0.9066 | 0.085* | |
C17 | 0.2939 (2) | 0.22784 (14) | 0.5190 (2) | 0.0239 (6) | |
C18 | 0.1760 (2) | 0.22820 (15) | 0.4769 (2) | 0.0269 (7) | |
C19 | 0.1132 (2) | 0.28763 (15) | 0.4516 (2) | 0.0284 (7) | |
C20 | 0.1652 (2) | 0.35138 (15) | 0.4654 (2) | 0.0286 (7) | |
C21 | 0.2835 (2) | 0.35146 (14) | 0.5091 (2) | 0.0286 (7) | |
C22 | 0.3446 (2) | 0.29238 (15) | 0.5337 (2) | 0.0263 (7) | |
C23 | 0.1021 (3) | 0.41792 (17) | 0.4378 (3) | 0.0398 (8) | |
C24 | 0.2273 (2) | 0.20863 (15) | 0.7311 (2) | 0.0257 (6) | |
C25 | 0.1108 (3) | 0.19783 (16) | 0.6954 (2) | 0.0316 (7) | |
C26 | 0.0346 (3) | 0.25040 (17) | 0.6804 (2) | 0.0355 (7) | |
C27 | 0.0700 (3) | 0.31784 (17) | 0.7009 (2) | 0.0346 (7) | |
C28 | 0.1858 (3) | 0.32930 (15) | 0.7332 (2) | 0.0330 (7) | |
C29 | 0.2616 (2) | 0.27650 (15) | 0.7485 (2) | 0.0286 (7) | |
C30 | −0.0169 (3) | 0.3733 (2) | 0.6880 (3) | 0.0477 (9) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Rh1 | 0.02879 (14) | 0.02009 (13) | 0.03024 (14) | 0.00077 (9) | 0.01289 (10) | 0.00001 (10) |
Rh2 | 0.02216 (13) | 0.02637 (14) | 0.03125 (14) | 0.00361 (9) | 0.00709 (10) | 0.00095 (10) |
S1 | 0.0290 (4) | 0.0239 (4) | 0.0299 (4) | 0.0024 (3) | 0.0129 (3) | 0.0009 (3) |
S2 | 0.0306 (4) | 0.0273 (4) | 0.0291 (4) | 0.0036 (3) | 0.0125 (3) | 0.0003 (3) |
F1 | 0.0404 (13) | 0.0497 (13) | 0.0861 (17) | 0.0135 (10) | −0.0053 (11) | 0.0060 (12) |
F2 | 0.0737 (15) | 0.0462 (12) | 0.0602 (14) | 0.0208 (11) | 0.0282 (11) | −0.0048 (10) |
F3 | 0.0670 (14) | 0.0439 (12) | 0.0726 (14) | 0.0200 (10) | 0.0336 (12) | 0.0266 (11) |
F4 | 0.0312 (9) | 0.0308 (10) | 0.0448 (10) | −0.0084 (8) | 0.0079 (8) | 0.0001 (8) |
F5 | 0.0219 (9) | 0.0492 (12) | 0.0542 (12) | 0.0037 (8) | 0.0042 (8) | 0.0040 (9) |
F6 | 0.0429 (11) | 0.0229 (10) | 0.0552 (12) | −0.0046 (8) | 0.0107 (9) | −0.0017 (8) |
F7 | 0.0228 (9) | 0.0318 (10) | 0.0518 (11) | −0.0029 (7) | 0.0068 (8) | 0.0009 (8) |
F8 | 0.0809 (18) | 0.0835 (18) | 0.109 (2) | 0.0406 (14) | 0.0649 (16) | 0.0178 (15) |
F9 | 0.0695 (16) | 0.0514 (15) | 0.0916 (18) | 0.0285 (12) | 0.0060 (13) | −0.0173 (13) |
F10 | 0.0714 (16) | 0.0832 (17) | 0.0491 (14) | 0.0423 (13) | −0.0011 (11) | 0.0076 (12) |
F11 | 0.0334 (10) | 0.0376 (11) | 0.0630 (13) | −0.0058 (8) | 0.0151 (9) | −0.0009 (9) |
F12 | 0.0273 (10) | 0.0645 (14) | 0.0615 (13) | 0.0060 (9) | 0.0131 (9) | 0.0026 (10) |
F13 | 0.0567 (12) | 0.0277 (10) | 0.0504 (12) | 0.0038 (9) | 0.0121 (10) | −0.0051 (9) |
F14 | 0.0307 (10) | 0.0334 (10) | 0.0453 (11) | −0.0034 (8) | 0.0084 (8) | −0.0064 (8) |
C1 | 0.051 (2) | 0.0279 (17) | 0.0344 (18) | −0.0061 (15) | 0.0206 (16) | −0.0059 (14) |
C2 | 0.046 (2) | 0.0255 (17) | 0.052 (2) | 0.0038 (14) | 0.0300 (17) | −0.0033 (15) |
C3 | 0.058 (2) | 0.034 (2) | 0.072 (3) | 0.0114 (17) | 0.027 (2) | 0.0000 (18) |
C4 | 0.068 (3) | 0.0295 (19) | 0.062 (2) | 0.0120 (18) | 0.013 (2) | 0.0121 (17) |
C5 | 0.066 (2) | 0.0251 (17) | 0.0384 (19) | −0.0039 (16) | 0.0215 (18) | 0.0072 (15) |
C6 | 0.051 (2) | 0.0317 (18) | 0.048 (2) | −0.0067 (15) | 0.0301 (18) | 0.0028 (15) |
C7 | 0.054 (2) | 0.039 (2) | 0.066 (3) | −0.0150 (17) | 0.028 (2) | −0.0063 (18) |
C8 | 0.054 (2) | 0.044 (2) | 0.054 (2) | −0.0179 (18) | 0.0139 (19) | −0.0133 (18) |
C9 | 0.038 (2) | 0.055 (2) | 0.0346 (19) | −0.0015 (17) | −0.0031 (15) | 0.0148 (17) |
C10 | 0.041 (2) | 0.052 (2) | 0.0341 (19) | 0.0085 (17) | 0.0000 (15) | −0.0087 (16) |
C11 | 0.066 (3) | 0.043 (2) | 0.073 (3) | −0.014 (2) | 0.000 (2) | −0.013 (2) |
C12 | 0.040 (2) | 0.085 (3) | 0.100 (4) | −0.022 (2) | 0.021 (2) | −0.021 (3) |
C13 | 0.0245 (17) | 0.047 (2) | 0.059 (2) | 0.0020 (15) | 0.0167 (16) | 0.0057 (18) |
C14 | 0.0302 (19) | 0.049 (2) | 0.063 (2) | 0.0115 (16) | 0.0208 (17) | −0.0021 (18) |
C15 | 0.067 (3) | 0.068 (3) | 0.124 (5) | 0.035 (2) | 0.044 (3) | 0.026 (3) |
C16 | 0.062 (3) | 0.040 (2) | 0.075 (3) | 0.016 (2) | −0.021 (2) | 0.006 (2) |
C17 | 0.0258 (16) | 0.0264 (16) | 0.0196 (14) | 0.0026 (12) | 0.0081 (12) | 0.0009 (12) |
C18 | 0.0305 (17) | 0.0272 (16) | 0.0225 (15) | −0.0053 (13) | 0.0089 (13) | 0.0000 (12) |
C19 | 0.0228 (16) | 0.0367 (18) | 0.0234 (15) | 0.0012 (13) | 0.0053 (12) | 0.0016 (13) |
C20 | 0.0320 (17) | 0.0298 (17) | 0.0227 (15) | 0.0068 (13) | 0.0078 (13) | 0.0029 (13) |
C21 | 0.0339 (18) | 0.0228 (16) | 0.0290 (16) | −0.0038 (13) | 0.0109 (13) | −0.0029 (13) |
C22 | 0.0224 (16) | 0.0311 (17) | 0.0247 (15) | −0.0011 (13) | 0.0073 (12) | 0.0004 (13) |
C23 | 0.038 (2) | 0.039 (2) | 0.0404 (19) | 0.0088 (15) | 0.0114 (16) | 0.0019 (16) |
C24 | 0.0268 (16) | 0.0303 (17) | 0.0211 (14) | 0.0047 (13) | 0.0098 (12) | −0.0011 (12) |
C25 | 0.0338 (18) | 0.0337 (18) | 0.0294 (16) | −0.0011 (14) | 0.0138 (14) | 0.0001 (14) |
C26 | 0.0271 (17) | 0.049 (2) | 0.0317 (17) | 0.0056 (15) | 0.0118 (14) | 0.0023 (15) |
C27 | 0.0383 (19) | 0.039 (2) | 0.0262 (16) | 0.0129 (15) | 0.0112 (14) | 0.0024 (14) |
C28 | 0.047 (2) | 0.0266 (17) | 0.0246 (16) | 0.0034 (15) | 0.0117 (14) | −0.0019 (13) |
C29 | 0.0298 (17) | 0.0347 (18) | 0.0211 (15) | −0.0005 (14) | 0.0086 (13) | −0.0015 (13) |
C30 | 0.047 (2) | 0.054 (2) | 0.039 (2) | 0.0199 (18) | 0.0108 (18) | 0.0038 (18) |
Geometric parameters (Å, º) top
Rh1—C2 | 2.132 (3) | C6—C7 | 1.517 (5) |
Rh1—C1 | 2.135 (3) | C6—H6A | 1.0000 |
Rh1—C5 | 2.146 (3) | C7—C8 | 1.523 (5) |
Rh1—C6 | 2.155 (3) | C7—H7A | 0.9900 |
Rh1—S1 | 2.3927 (8) | C7—H7B | 0.9900 |
Rh1—S2 | 2.3977 (8) | C8—H8A | 0.9900 |
Rh1—Rh2 | 2.9595 (3) | C8—H8B | 0.9900 |
Rh2—C10 | 2.135 (3) | C9—C10 | 1.395 (5) |
Rh2—C14 | 2.138 (3) | C9—C16 | 1.523 (5) |
Rh2—C9 | 2.143 (3) | C9—H9A | 1.0000 |
Rh2—C13 | 2.149 (3) | C10—C11 | 1.499 (5) |
Rh2—S2 | 2.3917 (8) | C10—H10A | 1.0000 |
Rh2—S1 | 2.3976 (8) | C11—C12 | 1.466 (6) |
S1—C17 | 1.762 (3) | C11—H11A | 0.9900 |
S2—C24 | 1.765 (3) | C11—H11B | 0.9900 |
F1—C23 | 1.321 (4) | C12—C13 | 1.501 (5) |
F2—C23 | 1.334 (4) | C12—H12A | 0.9900 |
F3—C23 | 1.328 (4) | C12—H12B | 0.9900 |
F4—C18 | 1.345 (3) | C13—C14 | 1.381 (5) |
F5—C19 | 1.341 (3) | C13—H13A | 1.0000 |
F6—C21 | 1.342 (3) | C14—C15 | 1.486 (6) |
F7—C22 | 1.345 (3) | C14—H14A | 1.0000 |
F8—C30 | 1.324 (4) | C15—C16 | 1.493 (6) |
F9—C30 | 1.321 (4) | C15—H15A | 0.9900 |
F10—C30 | 1.317 (4) | C15—H15B | 0.9900 |
F11—C25 | 1.344 (3) | C16—H16A | 0.9900 |
F12—C26 | 1.344 (3) | C16—H16B | 0.9900 |
F13—C28 | 1.348 (3) | C17—C18 | 1.388 (4) |
F14—C29 | 1.348 (3) | C17—C22 | 1.396 (4) |
C1—C2 | 1.386 (4) | C18—C19 | 1.378 (4) |
C1—C8 | 1.507 (4) | C19—C20 | 1.389 (4) |
C1—H1A | 1.0000 | C20—C21 | 1.394 (4) |
C2—C3 | 1.514 (5) | C20—C23 | 1.501 (4) |
C2—H2A | 1.0000 | C21—C22 | 1.362 (4) |
C3—C4 | 1.519 (5) | C24—C25 | 1.388 (4) |
C3—H3A | 0.9900 | C24—C29 | 1.390 (4) |
C3—H3B | 0.9900 | C25—C26 | 1.371 (4) |
C4—C5 | 1.504 (5) | C26—C27 | 1.388 (5) |
C4—H4A | 0.9900 | C27—C28 | 1.384 (4) |
C4—H4B | 0.9900 | C27—C30 | 1.506 (4) |
C5—C6 | 1.396 (5) | C28—C29 | 1.371 (4) |
C5—H5A | 1.0000 | | |
| | | |
C2—Rh1—C1 | 37.90 (12) | C10—C9—C16 | 123.4 (3) |
C2—Rh1—C5 | 82.10 (13) | C10—C9—Rh2 | 70.65 (18) |
C1—Rh1—C5 | 97.32 (13) | C16—C9—Rh2 | 110.7 (3) |
C2—Rh1—C6 | 89.58 (13) | C10—C9—H9A | 114.6 |
C1—Rh1—C6 | 80.85 (12) | C16—C9—H9A | 114.6 |
C5—Rh1—C6 | 37.86 (12) | Rh2—C9—H9A | 114.6 |
C2—Rh1—S1 | 89.21 (9) | C9—C10—C11 | 125.1 (3) |
C1—Rh1—S1 | 91.37 (9) | C9—C10—Rh2 | 71.30 (19) |
C5—Rh1—S1 | 152.61 (10) | C11—C10—Rh2 | 110.4 (3) |
C6—Rh1—S1 | 168.74 (9) | C9—C10—H10A | 114.0 |
C2—Rh1—S2 | 149.71 (9) | C11—C10—H10A | 114.0 |
C1—Rh1—S2 | 172.16 (9) | Rh2—C10—H10A | 114.0 |
C5—Rh1—S2 | 87.26 (9) | C12—C11—C10 | 116.2 (3) |
C6—Rh1—S2 | 99.23 (9) | C12—C11—H11A | 108.2 |
S1—Rh1—S2 | 87.36 (3) | C10—C11—H11A | 108.2 |
C2—Rh1—Rh2 | 104.04 (9) | C12—C11—H11B | 108.2 |
C1—Rh1—Rh2 | 132.11 (9) | C10—C11—H11B | 108.2 |
C5—Rh1—Rh2 | 105.11 (9) | H11A—C11—H11B | 107.4 |
C6—Rh1—Rh2 | 139.02 (9) | C11—C12—C13 | 115.2 (3) |
S1—Rh1—Rh2 | 51.919 (19) | C11—C12—H12A | 108.5 |
S2—Rh1—Rh2 | 51.745 (19) | C13—C12—H12A | 108.5 |
C10—Rh2—C14 | 95.84 (14) | C11—C12—H12B | 108.5 |
C10—Rh2—C9 | 38.06 (13) | C13—C12—H12B | 108.5 |
C14—Rh2—C9 | 82.24 (14) | H12A—C12—H12B | 107.5 |
C10—Rh2—C13 | 81.58 (14) | C14—C13—C12 | 123.6 (4) |
C14—Rh2—C13 | 37.58 (13) | C14—C13—Rh2 | 70.80 (19) |
C9—Rh2—C13 | 92.04 (14) | C12—C13—Rh2 | 112.0 (3) |
C10—Rh2—S2 | 95.16 (10) | C14—C13—H13A | 114.2 |
C14—Rh2—S2 | 149.55 (10) | C12—C13—H13A | 114.2 |
C9—Rh2—S2 | 89.23 (10) | Rh2—C13—H13A | 114.2 |
C13—Rh2—S2 | 172.83 (10) | C13—C14—C15 | 127.0 (4) |
C10—Rh2—S1 | 164.74 (10) | C13—C14—Rh2 | 71.62 (19) |
C14—Rh2—S1 | 89.35 (10) | C15—C14—Rh2 | 110.6 (3) |
C9—Rh2—S1 | 157.20 (10) | C13—C14—H14A | 113.2 |
C13—Rh2—S1 | 94.12 (10) | C15—C14—H14A | 113.2 |
S2—Rh2—S1 | 87.38 (3) | Rh2—C14—H14A | 113.2 |
C10—Rh2—Rh1 | 139.35 (10) | C14—C15—C16 | 114.7 (4) |
C14—Rh2—Rh1 | 103.86 (10) | C14—C15—H15A | 108.6 |
C9—Rh2—Rh1 | 109.78 (10) | C16—C15—H15A | 108.6 |
C13—Rh2—Rh1 | 133.70 (10) | C14—C15—H15B | 108.6 |
S2—Rh2—Rh1 | 51.928 (19) | C16—C15—H15B | 108.6 |
S1—Rh2—Rh1 | 51.771 (18) | H15A—C15—H15B | 107.6 |
C17—S1—Rh1 | 112.54 (10) | C15—C16—C9 | 115.7 (3) |
C17—S1—Rh2 | 105.47 (9) | C15—C16—H16A | 108.4 |
Rh1—S1—Rh2 | 76.31 (2) | C9—C16—H16A | 108.4 |
C24—S2—Rh2 | 114.32 (10) | C15—C16—H16B | 108.4 |
C24—S2—Rh1 | 111.95 (9) | C9—C16—H16B | 108.4 |
Rh2—S2—Rh1 | 76.33 (2) | H16A—C16—H16B | 107.4 |
C2—C1—C8 | 125.6 (3) | C18—C17—C22 | 115.0 (2) |
C2—C1—Rh1 | 70.96 (18) | C18—C17—S1 | 123.3 (2) |
C8—C1—Rh1 | 111.5 (2) | C22—C17—S1 | 121.4 (2) |
C2—C1—H1A | 113.7 | F4—C18—C19 | 117.5 (2) |
C8—C1—H1A | 113.7 | F4—C18—C17 | 119.7 (3) |
Rh1—C1—H1A | 113.7 | C19—C18—C17 | 122.8 (3) |
C1—C2—C3 | 124.4 (3) | F5—C19—C18 | 117.4 (3) |
C1—C2—Rh1 | 71.14 (17) | F5—C19—C20 | 121.2 (3) |
C3—C2—Rh1 | 112.7 (2) | C18—C19—C20 | 121.4 (3) |
C1—C2—H2A | 113.7 | C19—C20—C21 | 116.1 (3) |
C3—C2—H2A | 113.7 | C19—C20—C23 | 124.2 (3) |
Rh1—C2—H2A | 113.7 | C21—C20—C23 | 119.7 (3) |
C2—C3—C4 | 112.8 (3) | F6—C21—C22 | 118.5 (3) |
C2—C3—H3A | 109.0 | F6—C21—C20 | 119.6 (3) |
C4—C3—H3A | 109.0 | C22—C21—C20 | 121.9 (3) |
C2—C3—H3B | 109.0 | F7—C22—C21 | 117.6 (2) |
C4—C3—H3B | 109.0 | F7—C22—C17 | 119.6 (2) |
H3A—C3—H3B | 107.8 | C21—C22—C17 | 122.8 (3) |
C5—C4—C3 | 114.2 (3) | F1—C23—F3 | 107.2 (3) |
C5—C4—H4A | 108.7 | F1—C23—F2 | 107.1 (3) |
C3—C4—H4A | 108.7 | F3—C23—F2 | 105.9 (3) |
C5—C4—H4B | 108.7 | F1—C23—C20 | 113.2 (3) |
C3—C4—H4B | 108.7 | F3—C23—C20 | 111.7 (3) |
H4A—C4—H4B | 107.6 | F2—C23—C20 | 111.4 (3) |
C6—C5—C4 | 125.1 (3) | C25—C24—C29 | 115.5 (3) |
C6—C5—Rh1 | 71.42 (18) | C25—C24—S2 | 120.8 (2) |
C4—C5—Rh1 | 108.8 (2) | C29—C24—S2 | 123.2 (2) |
C6—C5—H5A | 114.4 | F11—C25—C26 | 117.8 (3) |
C4—C5—H5A | 114.4 | F11—C25—C24 | 119.8 (3) |
Rh1—C5—H5A | 114.4 | C26—C25—C24 | 122.4 (3) |
C5—C6—C7 | 124.0 (3) | F12—C26—C25 | 118.5 (3) |
C5—C6—Rh1 | 70.72 (18) | F12—C26—C27 | 119.9 (3) |
C7—C6—Rh1 | 113.4 (2) | C25—C26—C27 | 121.6 (3) |
C5—C6—H6A | 113.8 | C28—C27—C26 | 116.4 (3) |
C7—C6—H6A | 113.8 | C28—C27—C30 | 124.1 (3) |
Rh1—C6—H6A | 113.8 | C26—C27—C30 | 119.5 (3) |
C6—C7—C8 | 112.7 (3) | F13—C28—C29 | 117.1 (3) |
C6—C7—H7A | 109.1 | F13—C28—C27 | 121.3 (3) |
C8—C7—H7A | 109.1 | C29—C28—C27 | 121.6 (3) |
C6—C7—H7B | 109.1 | F14—C29—C28 | 117.8 (3) |
C8—C7—H7B | 109.1 | F14—C29—C24 | 119.8 (3) |
H7A—C7—H7B | 107.8 | C28—C29—C24 | 122.4 (3) |
C1—C8—C7 | 112.9 (3) | F10—C30—F9 | 106.3 (3) |
C1—C8—H8A | 109.0 | F10—C30—F8 | 107.9 (3) |
C7—C8—H8A | 109.0 | F9—C30—F8 | 106.0 (3) |
C1—C8—H8B | 109.0 | F10—C30—C27 | 111.7 (3) |
C7—C8—H8B | 109.0 | F9—C30—C27 | 113.3 (3) |
H8A—C8—H8B | 107.8 | F8—C30—C27 | 111.3 (3) |
Selected angles (°), distances (Å) and sums of angles (mean values) about
the S atom in [Rh(µ-SR)(Ln)]2 (L1 = cod, L2 = dippe) complexes topSR, Ln | Isomer | A1a | A2b | A3b | Rh···Rh | S···S |
SC6F5, L1 | syn–endo | 311.7 | 118.4 | 87.4, 89.5 | 2.954 | 3.369c |
| | 294.3 | | | | |
SC6HF4, L1 | syn–endo | 313.0 | 117.8 | 87.6, 89.8 | 2.956 | 3.330d |
| | 296.0 | | | | |
SC7F7, L1 | syn–endo | 294.3 | 117.4 | 86.0, 91.4 | 2.960 | 3.308e |
| | 302.6 | | | | |
SH, L2 | syn–exo | 302.5 | 136.0 | 36.0 | 3.281 | 3.016f |
SCH3, L2 | bent–anti | 297.6endo | 124.6 | 83.2endo | 3.298 | 3.299f |
| | 327.7exo | | 16.9exo | | |
SC6H11, L2 | syn–endo | 306.9 | 126.4 | 86.0 | 3.238 | 3.299f |
S2C3H6, L2 | syn–endo | 289.4 | 129.1 | 80.6 | 3.243 | 3.171f |
SC6H5, L2 | planar–anti | 301.0 | 180.0 | 77.8 | 3.634 | 3.231f |
Notes: (a) A1 is the sum of X—S—X angles at S; (b) The angles are defined
as shown in the scheme; (c) Cruz-Garritz et al., (1984); (d) Cruz-Garritz et al., (1991); (e) This work; (f) Oster & Jones, (2004) |