Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804015533/hb6060sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536804015533/hb6060Isup2.hkl |
CCDC reference: 248706
Key indicators
- Single-crystal X-ray study
- T = 105 K
- Mean (C-C) = 0.004 Å
- R factor = 0.031
- wR factor = 0.071
- Data-to-parameter ratio = 23.4
checkCIF/PLATON results
No syntax errors found
Alert level C PLAT031_ALERT_4_C Refined Extinction Parameter within Range ...... 3.00 Sigma PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Rh1 - Cl2 .. 8.60 su PLAT244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors .... C1S PLAT244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors .... B1
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 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 1 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 3 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: COLLECT (Nonius, 2000); cell refinement: HKL SCALEPACK (Otwinowski & Minor, 1997); data reduction: HKL SCALEPACK and DENZO (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: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: SHELXL97.
[RhCl2(C25H40P4)]BF4·C3H6O | F(000) = 1608 |
Mr = 783.15 | Dx = 1.502 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 7957 reflections |
a = 10.595 (2) Å | θ = 2.5–28.7° |
b = 14.750 (3) Å | µ = 0.88 mm−1 |
c = 22.285 (5) Å | T = 105 K |
β = 96.186 (9)° | Tablet, pale yellow |
V = 3462.3 (12) Å3 | 0.28 × 0.23 × 0.12 mm |
Z = 4 |
Nonius KappaCCD (with an Oxford Cryosystems Cryostream cooler) diffractometer | 8837 independent reflections |
Radiation source: fine-focus sealed tube | 7230 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.027 |
ω scans with κ offsets | θmax = 28.7°, θmin = 2.7° |
Absorption correction: multi-scan (HKL SCALEPACK; Otwinowski & Minor, 1997) | h = −14→14 |
Tmin = 0.806, Tmax = 0.900 | k = −19→14 |
29400 measured reflections | l = −30→30 |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.031 | H-atom parameters constrained |
wR(F2) = 0.071 | w = 1/[σ2(Fo2) + (0.0196P)2 + 3.8331P] where P = (Fo2 + 2Fc2)/3 |
S = 1.01 | (Δ/σ)max = 0.001 |
8837 reflections | Δρmax = 0.55 e Å−3 |
377 parameters | Δρmin = −0.85 e Å−3 |
0 restraints | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0003 (1) |
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. |
x | y | z | Uiso*/Ueq | ||
Rh1 | 0.240170 (16) | 0.276057 (10) | 0.328026 (7) | 0.01309 (5) | |
Cl1 | 0.23936 (6) | 0.42713 (3) | 0.28604 (3) | 0.02114 (12) | |
Cl2 | 0.37178 (6) | 0.31683 (4) | 0.42006 (3) | 0.02430 (13) | |
P1 | 0.05890 (6) | 0.30764 (4) | 0.37706 (3) | 0.01593 (12) | |
P2 | 0.09665 (5) | 0.21664 (4) | 0.25654 (2) | 0.01393 (11) | |
P3 | 0.24355 (6) | 0.12520 (4) | 0.34310 (3) | 0.01533 (12) | |
P4 | 0.42017 (5) | 0.24879 (4) | 0.27644 (3) | 0.01605 (12) | |
C1 | −0.0752 (2) | 0.24567 (15) | 0.33734 (10) | 0.0206 (5) | |
H1A | −0.0743 | 0.1820 | 0.3515 | 0.025* | |
H1B | −0.1561 | 0.2738 | 0.3461 | 0.025* | |
C2 | −0.0656 (2) | 0.24792 (15) | 0.26921 (10) | 0.0197 (5) | |
H2A | −0.0857 | 0.3094 | 0.2532 | 0.024* | |
H2B | −0.1269 | 0.2047 | 0.2483 | 0.024* | |
C3 | 0.1180 (2) | 0.09891 (14) | 0.28204 (10) | 0.0162 (4) | |
H3A | 0.1476 | 0.0587 | 0.2508 | 0.019* | |
H3B | 0.0409 | 0.0734 | 0.2971 | 0.019* | |
C4 | 0.3914 (2) | 0.07802 (15) | 0.32167 (10) | 0.0203 (5) | |
H4A | 0.4595 | 0.0856 | 0.3553 | 0.024* | |
H4B | 0.3805 | 0.0124 | 0.3134 | 0.024* | |
C5 | 0.4291 (2) | 0.12591 (15) | 0.26539 (10) | 0.0190 (5) | |
H5A | 0.3711 | 0.1077 | 0.2296 | 0.023* | |
H5B | 0.5166 | 0.1085 | 0.2584 | 0.023* | |
C6 | 0.0082 (2) | 0.42587 (15) | 0.37108 (11) | 0.0232 (5) | |
H6A | 0.0041 | 0.4450 | 0.3283 | 0.028* | |
H6B | −0.0783 | 0.4309 | 0.3837 | 0.028* | |
C7 | 0.0971 (3) | 0.49007 (17) | 0.40978 (12) | 0.0330 (6) | |
H7A | 0.0901 | 0.4784 | 0.4526 | 0.049* | |
H7B | 0.0731 | 0.5530 | 0.4002 | 0.049* | |
H7C | 0.1848 | 0.4798 | 0.4013 | 0.049* | |
C8 | 0.0593 (2) | 0.27648 (17) | 0.45602 (10) | 0.0257 (5) | |
H8A | 0.0761 | 0.2106 | 0.4601 | 0.031* | |
H8B | 0.1300 | 0.3086 | 0.4798 | 0.031* | |
C9 | −0.0640 (3) | 0.29797 (18) | 0.48304 (12) | 0.0316 (6) | |
H9A | −0.0806 | 0.3633 | 0.4802 | 0.047* | |
H9B | −0.0559 | 0.2794 | 0.5255 | 0.047* | |
H9C | −0.1344 | 0.2650 | 0.4607 | 0.047* | |
C10 | 0.1082 (2) | 0.22870 (14) | 0.17672 (10) | 0.0169 (4) | |
C11 | 0.1516 (2) | 0.15987 (16) | 0.14130 (10) | 0.0210 (5) | |
H11 | 0.1716 | 0.1019 | 0.1582 | 0.025* | |
C12 | 0.1652 (2) | 0.17682 (18) | 0.08114 (11) | 0.0264 (5) | |
H12 | 0.1943 | 0.1300 | 0.0568 | 0.032* | |
C13 | 0.1370 (3) | 0.26139 (19) | 0.05619 (11) | 0.0306 (6) | |
H13 | 0.1473 | 0.2724 | 0.0150 | 0.037* | |
C14 | 0.0938 (3) | 0.32980 (17) | 0.09130 (11) | 0.0276 (5) | |
H14 | 0.0746 | 0.3878 | 0.0741 | 0.033* | |
C15 | 0.0785 (2) | 0.31410 (15) | 0.15130 (10) | 0.0217 (5) | |
H15 | 0.0480 | 0.3610 | 0.1752 | 0.026* | |
C16 | 0.2169 (2) | 0.06644 (15) | 0.41155 (10) | 0.0188 (5) | |
C17 | 0.1281 (2) | −0.00322 (15) | 0.41166 (11) | 0.0231 (5) | |
H17 | 0.0752 | −0.0178 | 0.3758 | 0.028* | |
C18 | 0.1172 (3) | −0.05121 (17) | 0.46453 (12) | 0.0304 (6) | |
H18 | 0.0573 | −0.0991 | 0.4645 | 0.036* | |
C19 | 0.1926 (3) | −0.02993 (18) | 0.51694 (12) | 0.0329 (6) | |
H19 | 0.1843 | −0.0629 | 0.5529 | 0.040* | |
C20 | 0.2807 (3) | 0.03973 (19) | 0.51705 (12) | 0.0349 (6) | |
H20 | 0.3326 | 0.0543 | 0.5532 | 0.042* | |
C21 | 0.2935 (3) | 0.08803 (17) | 0.46478 (11) | 0.0285 (6) | |
H21 | 0.3539 | 0.1356 | 0.4650 | 0.034* | |
C22 | 0.5723 (2) | 0.27816 (16) | 0.31822 (11) | 0.0230 (5) | |
H22A | 0.5743 | 0.2547 | 0.3599 | 0.028* | |
H22B | 0.6411 | 0.2479 | 0.2991 | 0.028* | |
C23 | 0.5980 (3) | 0.38048 (17) | 0.32073 (13) | 0.0310 (6) | |
H23A | 0.6087 | 0.4027 | 0.2801 | 0.047* | |
H23B | 0.6754 | 0.3925 | 0.3477 | 0.047* | |
H23C | 0.5262 | 0.4117 | 0.3359 | 0.047* | |
C24 | 0.4268 (2) | 0.30015 (16) | 0.20244 (10) | 0.0220 (5) | |
H24A | 0.3477 | 0.2849 | 0.1766 | 0.026* | |
H24B | 0.4295 | 0.3669 | 0.2072 | 0.026* | |
C25 | 0.5403 (3) | 0.27054 (18) | 0.17007 (12) | 0.0304 (6) | |
H25A | 0.6193 | 0.2874 | 0.1945 | 0.046* | |
H25B | 0.5365 | 0.3006 | 0.1307 | 0.046* | |
H25C | 0.5379 | 0.2047 | 0.1643 | 0.046* | |
B1 | 0.7420 (3) | 0.01968 (19) | 0.30275 (13) | 0.0247 (6) | |
F1 | 0.86574 (15) | −0.00685 (11) | 0.32240 (8) | 0.0402 (4) | |
F2 | 0.69748 (16) | 0.07493 (12) | 0.34659 (7) | 0.0410 (4) | |
F3 | 0.74176 (17) | 0.06957 (12) | 0.25002 (7) | 0.0437 (4) | |
F4 | 0.66369 (17) | −0.05409 (11) | 0.29292 (9) | 0.0515 (5) | |
O1S | 0.6663 (3) | 0.0553 (3) | 0.06315 (14) | 0.1278 (18) | |
C1S | 0.7760 (4) | 0.0822 (3) | 0.06820 (15) | 0.0664 (13) | |
C2S | 0.8077 (4) | 0.1746 (3) | 0.09012 (17) | 0.0735 (13) | |
H21S | 0.7293 | 0.2089 | 0.0928 | 0.110* | |
H22S | 0.8588 | 0.2051 | 0.0620 | 0.110* | |
H23S | 0.8561 | 0.1714 | 0.1301 | 0.110* | |
C3S | 0.8818 (5) | 0.0261 (2) | 0.04886 (16) | 0.0765 (15) | |
H31S | 0.8526 | −0.0364 | 0.0417 | 0.115* | |
H32S | 0.9534 | 0.0267 | 0.0806 | 0.115* | |
H33S | 0.9089 | 0.0512 | 0.0116 | 0.115* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Rh1 | 0.01270 (9) | 0.01110 (8) | 0.01553 (9) | −0.00076 (6) | 0.00181 (6) | −0.00109 (6) |
Cl1 | 0.0249 (3) | 0.0124 (2) | 0.0270 (3) | −0.0013 (2) | 0.0071 (2) | 0.0022 (2) |
Cl2 | 0.0220 (3) | 0.0294 (3) | 0.0209 (3) | −0.0046 (2) | 0.0001 (2) | −0.0058 (2) |
P1 | 0.0152 (3) | 0.0148 (3) | 0.0183 (3) | 0.0001 (2) | 0.0042 (2) | −0.0022 (2) |
P2 | 0.0135 (3) | 0.0120 (2) | 0.0162 (3) | 0.0000 (2) | 0.0011 (2) | −0.0009 (2) |
P3 | 0.0151 (3) | 0.0119 (3) | 0.0189 (3) | 0.0005 (2) | 0.0015 (2) | 0.0005 (2) |
P4 | 0.0130 (3) | 0.0158 (3) | 0.0196 (3) | −0.0010 (2) | 0.0029 (2) | −0.0016 (2) |
C1 | 0.0154 (11) | 0.0196 (11) | 0.0277 (12) | −0.0020 (9) | 0.0066 (9) | −0.0050 (9) |
C2 | 0.0159 (12) | 0.0189 (11) | 0.0237 (12) | 0.0024 (9) | −0.0006 (9) | −0.0033 (8) |
C3 | 0.0173 (12) | 0.0119 (10) | 0.0196 (11) | −0.0013 (8) | 0.0027 (9) | −0.0013 (8) |
C4 | 0.0176 (12) | 0.0168 (11) | 0.0264 (12) | 0.0038 (9) | 0.0015 (10) | −0.0003 (9) |
C5 | 0.0135 (11) | 0.0188 (11) | 0.0248 (12) | 0.0007 (8) | 0.0027 (9) | −0.0034 (9) |
C6 | 0.0237 (13) | 0.0176 (11) | 0.0297 (13) | 0.0038 (9) | 0.0097 (10) | −0.0026 (9) |
C7 | 0.0403 (17) | 0.0206 (12) | 0.0397 (15) | −0.0061 (11) | 0.0121 (13) | −0.0105 (11) |
C8 | 0.0275 (14) | 0.0310 (13) | 0.0199 (12) | 0.0008 (11) | 0.0083 (10) | 0.0008 (10) |
C9 | 0.0349 (16) | 0.0368 (15) | 0.0258 (13) | 0.0021 (12) | 0.0165 (12) | −0.0001 (11) |
C10 | 0.0154 (11) | 0.0181 (10) | 0.0169 (10) | −0.0041 (8) | 0.0006 (8) | 0.0000 (8) |
C11 | 0.0186 (12) | 0.0226 (11) | 0.0220 (12) | 0.0016 (9) | 0.0019 (9) | −0.0007 (9) |
C12 | 0.0228 (13) | 0.0355 (14) | 0.0213 (12) | 0.0021 (11) | 0.0037 (10) | −0.0033 (10) |
C13 | 0.0282 (14) | 0.0423 (15) | 0.0220 (12) | −0.0006 (12) | 0.0054 (10) | 0.0060 (11) |
C14 | 0.0286 (14) | 0.0256 (12) | 0.0283 (13) | −0.0017 (10) | 0.0021 (11) | 0.0080 (10) |
C15 | 0.0228 (13) | 0.0199 (11) | 0.0219 (12) | −0.0034 (9) | −0.0003 (10) | −0.0001 (9) |
C16 | 0.0204 (12) | 0.0169 (10) | 0.0192 (11) | 0.0032 (9) | 0.0033 (9) | 0.0021 (8) |
C17 | 0.0267 (14) | 0.0200 (11) | 0.0229 (12) | −0.0014 (10) | 0.0038 (10) | 0.0008 (9) |
C18 | 0.0352 (16) | 0.0262 (13) | 0.0308 (14) | −0.0078 (11) | 0.0081 (12) | 0.0061 (10) |
C19 | 0.0392 (17) | 0.0367 (15) | 0.0234 (13) | 0.0009 (12) | 0.0057 (12) | 0.0118 (11) |
C20 | 0.0387 (17) | 0.0418 (16) | 0.0223 (13) | −0.0036 (13) | −0.0049 (12) | 0.0050 (11) |
C21 | 0.0300 (15) | 0.0276 (13) | 0.0264 (13) | −0.0055 (11) | −0.0036 (11) | 0.0055 (10) |
C22 | 0.0126 (11) | 0.0271 (12) | 0.0290 (13) | −0.0026 (9) | 0.0005 (9) | −0.0063 (10) |
C23 | 0.0227 (14) | 0.0312 (14) | 0.0394 (15) | −0.0094 (11) | 0.0044 (12) | −0.0087 (11) |
C24 | 0.0187 (12) | 0.0247 (12) | 0.0233 (12) | −0.0014 (9) | 0.0061 (10) | 0.0026 (9) |
C25 | 0.0310 (15) | 0.0336 (14) | 0.0293 (13) | −0.0003 (11) | 0.0158 (11) | −0.0016 (11) |
B1 | 0.0176 (14) | 0.0256 (14) | 0.0307 (15) | 0.0004 (11) | 0.0011 (11) | −0.0011 (11) |
F1 | 0.0190 (8) | 0.0469 (10) | 0.0538 (11) | 0.0071 (7) | 0.0000 (7) | 0.0038 (8) |
F2 | 0.0368 (10) | 0.0519 (10) | 0.0331 (9) | 0.0149 (8) | −0.0021 (7) | −0.0083 (7) |
F3 | 0.0456 (11) | 0.0484 (10) | 0.0375 (9) | 0.0014 (8) | 0.0070 (8) | 0.0120 (8) |
F4 | 0.0389 (11) | 0.0364 (9) | 0.0782 (13) | −0.0200 (8) | 0.0014 (10) | −0.0046 (9) |
O1S | 0.085 (2) | 0.210 (4) | 0.078 (2) | −0.105 (3) | −0.0414 (18) | 0.082 (2) |
C1S | 0.059 (3) | 0.107 (3) | 0.0301 (17) | −0.049 (2) | −0.0126 (16) | 0.0305 (19) |
C2S | 0.033 (2) | 0.133 (4) | 0.054 (2) | −0.005 (2) | 0.0025 (17) | −0.035 (2) |
C3S | 0.146 (5) | 0.041 (2) | 0.038 (2) | −0.029 (2) | −0.009 (2) | 0.0116 (15) |
Rh1—P3 | 2.2501 (7) | C11—H11 | 0.9500 |
Rh1—P2 | 2.2574 (7) | C12—C13 | 1.385 (4) |
Rh1—P1 | 2.3563 (7) | C12—H12 | 0.9500 |
Rh1—P4 | 2.3649 (7) | C13—C14 | 1.385 (4) |
Rh1—Cl1 | 2.4164 (7) | C13—H13 | 0.9500 |
Rh1—Cl2 | 2.4282 (7) | C14—C15 | 1.384 (3) |
P1—C8 | 1.818 (2) | C14—H14 | 0.9500 |
P1—C6 | 1.825 (2) | C15—H15 | 0.9500 |
P1—C1 | 1.835 (2) | C16—C17 | 1.394 (3) |
P2—C10 | 1.805 (2) | C16—C21 | 1.400 (3) |
P2—C2 | 1.831 (2) | C17—C18 | 1.390 (3) |
P2—C3 | 1.834 (2) | C17—H17 | 0.9500 |
P3—C16 | 1.803 (2) | C18—C19 | 1.378 (4) |
P3—C4 | 1.824 (2) | C18—H18 | 0.9500 |
P3—C3 | 1.839 (2) | C19—C20 | 1.388 (4) |
P4—C24 | 1.823 (2) | C19—H19 | 0.9500 |
P4—C22 | 1.825 (2) | C20—C21 | 1.384 (3) |
P4—C5 | 1.833 (2) | C20—H20 | 0.9500 |
C1—C2 | 1.533 (3) | C21—H21 | 0.9500 |
C1—H1A | 0.9900 | C22—C23 | 1.534 (3) |
C1—H1B | 0.9900 | C22—H22A | 0.9900 |
C2—H2A | 0.9900 | C22—H22B | 0.9900 |
C2—H2B | 0.9900 | C23—H23A | 0.9800 |
C3—H3A | 0.9900 | C23—H23B | 0.9800 |
C3—H3B | 0.9900 | C23—H23C | 0.9800 |
C4—C5 | 1.529 (3) | C24—C25 | 1.532 (3) |
C4—H4A | 0.9900 | C24—H24A | 0.9900 |
C4—H4B | 0.9900 | C24—H24B | 0.9900 |
C5—H5A | 0.9900 | C25—H25A | 0.9800 |
C5—H5B | 0.9900 | C25—H25B | 0.9800 |
C6—C7 | 1.534 (3) | C25—H25C | 0.9800 |
C6—H6A | 0.9900 | B1—F4 | 1.372 (3) |
C6—H6B | 0.9900 | B1—F3 | 1.386 (3) |
C7—H7A | 0.9800 | B1—F1 | 1.392 (3) |
C7—H7B | 0.9800 | B1—F2 | 1.393 (3) |
C7—H7C | 0.9800 | O1S—C1S | 1.221 (4) |
C8—C9 | 1.529 (3) | C1S—C2S | 1.475 (6) |
C8—H8A | 0.9900 | C1S—C3S | 1.494 (6) |
C8—H8B | 0.9900 | C2S—H21S | 0.9800 |
C9—H9A | 0.9800 | C2S—H22S | 0.9800 |
C9—H9B | 0.9800 | C2S—H23S | 0.9800 |
C9—H9C | 0.9800 | C3S—H31S | 0.9800 |
C10—C11 | 1.394 (3) | C3S—H32S | 0.9800 |
C10—C15 | 1.403 (3) | C3S—H33S | 0.9800 |
C11—C12 | 1.387 (3) | ||
P3—Rh1—P2 | 73.75 (2) | C8—C9—H9A | 109.5 |
P3—Rh1—P1 | 97.29 (2) | C8—C9—H9B | 109.5 |
P2—Rh1—P1 | 83.30 (3) | H9A—C9—H9B | 109.5 |
P3—Rh1—P4 | 84.47 (2) | C8—C9—H9C | 109.5 |
P2—Rh1—P4 | 96.21 (3) | H9A—C9—H9C | 109.5 |
P1—Rh1—P4 | 177.94 (2) | H9B—C9—H9C | 109.5 |
P3—Rh1—Cl1 | 165.72 (2) | C11—C10—C15 | 119.9 (2) |
P2—Rh1—Cl1 | 96.36 (2) | C11—C10—P2 | 123.21 (17) |
P1—Rh1—Cl1 | 91.61 (2) | C15—C10—P2 | 116.77 (17) |
P4—Rh1—Cl1 | 86.45 (2) | C12—C11—C10 | 119.4 (2) |
P3—Rh1—Cl2 | 96.91 (2) | C12—C11—H11 | 120.3 |
P2—Rh1—Cl2 | 166.92 (2) | C10—C11—H11 | 120.3 |
P1—Rh1—Cl2 | 88.96 (3) | C13—C12—C11 | 120.7 (2) |
P4—Rh1—Cl2 | 91.89 (3) | C13—C12—H12 | 119.7 |
Cl1—Rh1—Cl2 | 94.38 (2) | C11—C12—H12 | 119.7 |
C8—P1—C6 | 106.39 (11) | C14—C13—C12 | 120.0 (2) |
C8—P1—C1 | 105.19 (11) | C14—C13—H13 | 120.0 |
C6—P1—C1 | 103.54 (11) | C12—C13—H13 | 120.0 |
C8—P1—Rh1 | 118.80 (8) | C15—C14—C13 | 120.3 (2) |
C6—P1—Rh1 | 113.78 (8) | C15—C14—H14 | 119.9 |
C1—P1—Rh1 | 107.77 (7) | C13—C14—H14 | 119.9 |
C10—P2—C2 | 106.94 (11) | C14—C15—C10 | 119.7 (2) |
C10—P2—C3 | 112.31 (10) | C14—C15—H15 | 120.1 |
C2—P2—C3 | 106.08 (10) | C10—C15—H15 | 120.1 |
C10—P2—Rh1 | 123.05 (7) | C17—C16—C21 | 119.7 (2) |
C2—P2—Rh1 | 111.45 (8) | C17—C16—P3 | 121.55 (18) |
C3—P2—Rh1 | 95.62 (7) | C21—C16—P3 | 118.58 (18) |
C16—P3—C4 | 104.79 (11) | C18—C17—C16 | 119.7 (2) |
C16—P3—C3 | 110.97 (11) | C18—C17—H17 | 120.2 |
C4—P3—C3 | 107.39 (11) | C16—C17—H17 | 120.2 |
C16—P3—Rh1 | 126.89 (7) | C19—C18—C17 | 120.6 (2) |
C4—P3—Rh1 | 109.79 (8) | C19—C18—H18 | 119.7 |
C3—P3—Rh1 | 95.71 (7) | C17—C18—H18 | 119.7 |
C24—P4—C22 | 104.18 (11) | C18—C19—C20 | 119.9 (2) |
C24—P4—C5 | 106.38 (11) | C18—C19—H19 | 120.0 |
C22—P4—C5 | 104.34 (11) | C20—C19—H19 | 120.0 |
C24—P4—Rh1 | 118.73 (8) | C21—C20—C19 | 120.4 (3) |
C22—P4—Rh1 | 115.21 (8) | C21—C20—H20 | 119.8 |
C5—P4—Rh1 | 106.82 (7) | C19—C20—H20 | 119.8 |
C2—C1—P1 | 109.66 (15) | C20—C21—C16 | 119.7 (2) |
C2—C1—H1A | 109.7 | C20—C21—H21 | 120.1 |
P1—C1—H1A | 109.7 | C16—C21—H21 | 120.1 |
C2—C1—H1B | 109.7 | C23—C22—P4 | 113.30 (18) |
P1—C1—H1B | 109.7 | C23—C22—H22A | 108.9 |
H1A—C1—H1B | 108.2 | P4—C22—H22A | 108.9 |
C1—C2—P2 | 108.11 (16) | C23—C22—H22B | 108.9 |
C1—C2—H2A | 110.1 | P4—C22—H22B | 108.9 |
P2—C2—H2A | 110.1 | H22A—C22—H22B | 107.7 |
C1—C2—H2B | 110.1 | C22—C23—H23A | 109.5 |
P2—C2—H2B | 110.1 | C22—C23—H23B | 109.5 |
H2A—C2—H2B | 108.4 | H23A—C23—H23B | 109.5 |
P2—C3—P3 | 94.86 (10) | C22—C23—H23C | 109.5 |
P2—C3—H3A | 112.8 | H23A—C23—H23C | 109.5 |
P3—C3—H3A | 112.8 | H23B—C23—H23C | 109.5 |
P2—C3—H3B | 112.8 | C25—C24—P4 | 114.60 (18) |
P3—C3—H3B | 112.8 | C25—C24—H24A | 108.6 |
H3A—C3—H3B | 110.2 | P4—C24—H24A | 108.6 |
C5—C4—P3 | 110.26 (15) | C25—C24—H24B | 108.6 |
C5—C4—H4A | 109.6 | P4—C24—H24B | 108.6 |
P3—C4—H4A | 109.6 | H24A—C24—H24B | 107.6 |
C5—C4—H4B | 109.6 | C24—C25—H25A | 109.5 |
P3—C4—H4B | 109.6 | C24—C25—H25B | 109.5 |
H4A—C4—H4B | 108.1 | H25A—C25—H25B | 109.5 |
C4—C5—P4 | 108.95 (15) | C24—C25—H25C | 109.5 |
C4—C5—H5A | 109.9 | H25A—C25—H25C | 109.5 |
P4—C5—H5A | 109.9 | H25B—C25—H25C | 109.5 |
C4—C5—H5B | 109.9 | F4—B1—F3 | 109.9 (2) |
P4—C5—H5B | 109.9 | F4—B1—F1 | 111.1 (2) |
H5A—C5—H5B | 108.3 | F3—B1—F1 | 109.4 (2) |
C7—C6—P1 | 113.00 (18) | F4—B1—F2 | 109.3 (2) |
C7—C6—H6A | 109.0 | F3—B1—F2 | 108.3 (2) |
P1—C6—H6A | 109.0 | F1—B1—F2 | 108.8 (2) |
C7—C6—H6B | 109.0 | O1S—C1S—C2S | 120.7 (5) |
P1—C6—H6B | 109.0 | O1S—C1S—C3S | 122.0 (5) |
H6A—C6—H6B | 107.8 | C2S—C1S—C3S | 117.1 (3) |
C6—C7—H7A | 109.5 | C1S—C2S—H21S | 109.5 |
C6—C7—H7B | 109.5 | C1S—C2S—H22S | 109.5 |
H7A—C7—H7B | 109.5 | H21S—C2S—H22S | 109.5 |
C6—C7—H7C | 109.5 | C1S—C2S—H23S | 109.5 |
H7A—C7—H7C | 109.5 | H21S—C2S—H23S | 109.5 |
H7B—C7—H7C | 109.5 | H22S—C2S—H23S | 109.5 |
C9—C8—P1 | 114.55 (18) | C1S—C3S—H31S | 109.5 |
C9—C8—H8A | 108.6 | C1S—C3S—H32S | 109.5 |
P1—C8—H8A | 108.6 | H31S—C3S—H32S | 109.5 |
C9—C8—H8B | 108.6 | C1S—C3S—H33S | 109.5 |
P1—C8—H8B | 108.6 | H31S—C3S—H33S | 109.5 |
H8A—C8—H8B | 107.6 | H32S—C3S—H33S | 109.5 |
P3—Rh1—P1—C8 | 58.51 (10) | P1—C1—C2—P2 | 48.26 (18) |
P2—Rh1—P1—C8 | 131.11 (10) | C10—P2—C2—C1 | −175.54 (15) |
Cl1—Rh1—P1—C8 | −132.68 (10) | C3—P2—C2—C1 | 64.41 (17) |
Cl2—Rh1—P1—C8 | −38.32 (10) | Rh1—P2—C2—C1 | −38.46 (16) |
P3—Rh1—P1—C6 | −175.03 (9) | C10—P2—C3—P3 | 127.09 (10) |
P2—Rh1—P1—C6 | −102.44 (9) | C2—P2—C3—P3 | −116.41 (11) |
Cl1—Rh1—P1—C6 | −6.22 (9) | Rh1—P2—C3—P3 | −2.15 (8) |
Cl2—Rh1—P1—C6 | 88.13 (9) | C16—P3—C3—P2 | 135.35 (10) |
P3—Rh1—P1—C1 | −60.84 (8) | C4—P3—C3—P2 | −110.66 (10) |
P2—Rh1—P1—C1 | 11.76 (8) | Rh1—P3—C3—P2 | 2.16 (8) |
Cl1—Rh1—P1—C1 | 107.97 (8) | C16—P3—C4—C5 | −177.08 (16) |
Cl2—Rh1—P1—C1 | −157.67 (8) | C3—P3—C4—C5 | 64.84 (18) |
P3—Rh1—P2—C10 | −119.44 (9) | Rh1—P3—C4—C5 | −38.07 (17) |
P1—Rh1—P2—C10 | 140.92 (9) | P3—C4—C5—P4 | 48.92 (19) |
P4—Rh1—P2—C10 | −37.06 (9) | C24—P4—C5—C4 | −166.13 (16) |
Cl1—Rh1—P2—C10 | 50.04 (9) | C22—P4—C5—C4 | 84.08 (18) |
Cl2—Rh1—P2—C10 | −164.96 (11) | Rh1—P4—C5—C4 | −38.38 (17) |
P3—Rh1—P2—C2 | 111.57 (8) | C8—P1—C6—C7 | 60.4 (2) |
P1—Rh1—P2—C2 | 11.93 (8) | C1—P1—C6—C7 | 171.04 (17) |
P4—Rh1—P2—C2 | −166.05 (8) | Rh1—P1—C6—C7 | −72.27 (18) |
Cl1—Rh1—P2—C2 | −78.95 (8) | C6—P1—C8—C9 | 51.5 (2) |
Cl2—Rh1—P2—C2 | 66.05 (13) | C1—P1—C8—C9 | −58.0 (2) |
P3—Rh1—P2—C3 | 1.83 (7) | Rh1—P1—C8—C9 | −178.65 (15) |
P1—Rh1—P2—C3 | −97.81 (7) | C2—P2—C10—C11 | −127.2 (2) |
P4—Rh1—P2—C3 | 84.21 (7) | C3—P2—C10—C11 | −11.2 (2) |
Cl1—Rh1—P2—C3 | 171.31 (7) | Rh1—P2—C10—C11 | 101.96 (19) |
Cl2—Rh1—P2—C3 | −43.69 (12) | C2—P2—C10—C15 | 56.7 (2) |
P2—Rh1—P3—C16 | −123.47 (10) | C3—P2—C10—C15 | 172.72 (17) |
P1—Rh1—P3—C16 | −42.67 (10) | Rh1—P2—C10—C15 | −74.13 (19) |
P4—Rh1—P3—C16 | 138.40 (10) | C15—C10—C11—C12 | 0.2 (3) |
Cl1—Rh1—P3—C16 | −170.83 (12) | P2—C10—C11—C12 | −175.81 (18) |
Cl2—Rh1—P3—C16 | 47.16 (10) | C10—C11—C12—C13 | 0.4 (4) |
P2—Rh1—P3—C4 | 108.99 (9) | C11—C12—C13—C14 | −0.5 (4) |
P1—Rh1—P3—C4 | −170.21 (8) | C12—C13—C14—C15 | −0.1 (4) |
P4—Rh1—P3—C4 | 10.86 (8) | C13—C14—C15—C10 | 0.7 (4) |
Cl1—Rh1—P3—C4 | 61.63 (13) | C11—C10—C15—C14 | −0.7 (4) |
Cl2—Rh1—P3—C4 | −80.38 (9) | P2—C10—C15—C14 | 175.52 (19) |
P2—Rh1—P3—C3 | −1.82 (7) | C4—P3—C16—C17 | −103.0 (2) |
P1—Rh1—P3—C3 | 78.98 (7) | C3—P3—C16—C17 | 12.7 (2) |
P4—Rh1—P3—C3 | −99.95 (7) | Rh1—P3—C16—C17 | 127.55 (17) |
Cl1—Rh1—P3—C3 | −49.17 (12) | C4—P3—C16—C21 | 72.9 (2) |
Cl2—Rh1—P3—C3 | 168.81 (7) | C3—P3—C16—C21 | −171.43 (18) |
P3—Rh1—P4—C24 | 132.60 (9) | Rh1—P3—C16—C21 | −56.5 (2) |
P2—Rh1—P4—C24 | 59.66 (9) | C21—C16—C17—C18 | −0.6 (4) |
Cl1—Rh1—P4—C24 | −36.36 (9) | P3—C16—C17—C18 | 175.23 (19) |
Cl2—Rh1—P4—C24 | −130.64 (9) | C16—C17—C18—C19 | 0.6 (4) |
P3—Rh1—P4—C22 | −102.87 (9) | C17—C18—C19—C20 | −0.3 (4) |
P2—Rh1—P4—C22 | −175.81 (9) | C18—C19—C20—C21 | 0.0 (4) |
Cl1—Rh1—P4—C22 | 88.17 (9) | C19—C20—C21—C16 | 0.0 (4) |
Cl2—Rh1—P4—C22 | −6.11 (9) | C17—C16—C21—C20 | 0.3 (4) |
P3—Rh1—P4—C5 | 12.49 (8) | P3—C16—C21—C20 | −175.7 (2) |
P2—Rh1—P4—C5 | −60.45 (8) | C24—P4—C22—C23 | 56.1 (2) |
Cl1—Rh1—P4—C5 | −156.47 (8) | C5—P4—C22—C23 | 167.48 (17) |
Cl2—Rh1—P4—C5 | 109.26 (8) | Rh1—P4—C22—C23 | −75.74 (19) |
C8—P1—C1—C2 | −166.14 (16) | C22—P4—C24—C25 | 56.3 (2) |
C6—P1—C1—C2 | 82.38 (17) | C5—P4—C24—C25 | −53.6 (2) |
Rh1—P1—C1—C2 | −38.47 (17) | Rh1—P4—C24—C25 | −173.98 (15) |
D—H···A | D—H | H···A | D···A | D—H···A |
C2—H2A···F4i | 0.99 | 2.37 | 3.349 (3) | 171 |
C3—H3B···F1ii | 0.99 | 2.32 | 3.302 (3) | 171 |
C17—H17···F1ii | 0.95 | 2.41 | 3.240 (3) | 146 |
Symmetry codes: (i) −x+1/2, y+1/2, −z+1/2; (ii) x−1, y, z. |
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