Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803014995/su6031sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536803014995/su6031Isup2.hkl |
CCDC reference: 221623
Data collection: COLLECT (Nonius, 2000); cell refinement: DENZO-SMN (Otwinowski & Minor, 1997); data reduction: DENZO-SMN); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); 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.
[PtBrH(C18H15P)2]·0.5C7H8 | F(000) = 1660 |
Mr = 846.61 | Dx = 1.630 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
a = 11.514 (2) Å | Cell parameters from 55096 reflections |
b = 13.447 (3) Å | θ = 2.9–27.5° |
c = 22.449 (5) Å | µ = 5.35 mm−1 |
β = 97.01 (3)° | T = 150 K |
V = 3449.8 (12) Å3 | Prism, colourless |
Z = 4 | 0.20 × 0.20 × 0.15 mm |
Nonius KappaCCD diffractometer | 7893 independent reflections |
Radiation source: fine-focus sealed tube | 6645 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.083 |
φ and ω scans to fill Ewald sphere | θmax = 27.5°, θmin = 3.0° |
Absorption correction: multi-scan (SORTAV; Blessing, 1995) | h = −14→14 |
Tmin = 0.325, Tmax = 0.461 | k = −17→17 |
55828 measured reflections | l = −29→29 |
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)] = 0.032 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.071 | w = 1/[σ2(Fo2) + (0.0246P)2 + 8.05P] where P = (Fo2 + 2Fc2)/3 |
S = 1.02 | (Δ/σ)max = 0.001 |
7893 reflections | Δρmax = 1.08 e Å−3 |
386 parameters | Δρmin = −0.97 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: 0.00126 (7) |
Experimental. The title compound was prepared by the hydrolysis of a toluene solution of trans-(Ph3P)2Pt(B(Mes)Br)Br on exposure to air. A solution containing 137 mg (0.13 mmol) of trans-(Ph3P)2Pt(B(Mes)Br)Br in ca 10 cm3 of toluene was exposed to air for a period of 9 days, at which point monitoring of the reaction mixture by 31P NMR revealed that the sole phosphorus-containing product in solution was trans-(Ph3P)2Pt(H)Br; starting material (δP 18.2 p.p.m., 1JPtP = 3469 Hz), title compound (δP 29.7 p.p.m., 1JPtP = 2986 Hz). Removal of solvent in vacuo and recrystallization from toluene/hexane (50:50) led to the isolation of the title compound as colourless crystals suitable for X-ray diffraction in yields of ca 58%. Comparison of multinuclear (1H, 13C and 31P) NMR and IR spectroscopic data with that reported previously confirmed the identity of the platinum-containing product (Carr, Shaw & Thornton-Pett, 1985). The identity of the boron-containing product was confirmed as (MesBO)3 by comparison of the multinuclear (1H, 13C and 11B) NMR data of the colourless material isolated from the supernatent solution with that reported in the literature (Anulewicz-Ostrowska, R., Luliński, S., Serwatowski, J. & Suwińska, K. (2000). Inorg. Chem. 39, 5763–5767.). |
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. The H atom, H99 attached to Pt1 centres was located from difference Fourier syntheses and refined isotropically with no restraints. Phenyl hydrogen atoms were placed in idealized positions [C—H 0.95 Å] and refined using a riding model with Uiso(H) = 1.2Ueq(C). A disordered molecule of toluene was located in the crystal lattice and found to reside on a 2-fold axis (0.5 molecule/asymmetric unit). The disorder was successfully modelled and the carbon atoms, C37—C41 refined isotropically without attached hydrogen atoms. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Pt1 | 0.812595 (12) | 0.013603 (10) | 0.220868 (6) | 0.01636 (6) | |
Br1 | 0.66361 (3) | −0.00628 (3) | 0.294337 (18) | 0.02347 (9) | |
P1 | 0.67686 (8) | 0.01202 (7) | 0.13791 (4) | 0.01567 (19) | |
P2 | 0.96458 (8) | 0.00875 (7) | 0.29576 (4) | 0.01611 (19) | |
C1 | 0.5800 (3) | −0.0948 (3) | 0.13621 (18) | 0.0198 (8) | |
C2 | 0.6188 (4) | −0.1806 (3) | 0.16774 (19) | 0.0266 (9) | |
H2 | 0.6945 | −0.1820 | 0.1899 | 0.032* | |
C3 | 0.5473 (4) | −0.2635 (3) | 0.1668 (2) | 0.0346 (11) | |
H3 | 0.5746 | −0.3217 | 0.1880 | 0.042* | |
C4 | 0.4371 (4) | −0.2621 (3) | 0.1354 (2) | 0.0355 (11) | |
H4 | 0.3882 | −0.3191 | 0.1353 | 0.043* | |
C5 | 0.3971 (4) | −0.1778 (3) | 0.1038 (2) | 0.0322 (10) | |
H5 | 0.3210 | −0.1769 | 0.0819 | 0.039* | |
C6 | 0.4693 (3) | −0.0942 (3) | 0.10417 (19) | 0.0240 (9) | |
H6 | 0.4422 | −0.0365 | 0.0823 | 0.029* | |
C7 | 0.7401 (3) | 0.0056 (3) | 0.06702 (17) | 0.0185 (8) | |
C8 | 0.7027 (3) | −0.0634 (3) | 0.02249 (17) | 0.0192 (8) | |
H8 | 0.6436 | −0.1101 | 0.0289 | 0.023* | |
C9 | 0.7511 (3) | −0.0645 (3) | −0.03121 (19) | 0.0248 (9) | |
H9 | 0.7264 | −0.1129 | −0.0609 | 0.030* | |
C10 | 0.8355 (4) | 0.0051 (3) | −0.0415 (2) | 0.0284 (9) | |
H10 | 0.8680 | 0.0053 | −0.0784 | 0.034* | |
C11 | 0.8719 (4) | 0.0744 (3) | 0.00264 (19) | 0.0274 (9) | |
H11 | 0.9296 | 0.1221 | −0.0042 | 0.033* | |
C12 | 0.8255 (3) | 0.0748 (3) | 0.05623 (19) | 0.0238 (9) | |
H12 | 0.8518 | 0.1224 | 0.0861 | 0.029* | |
C13 | 0.5788 (3) | 0.1194 (3) | 0.12629 (17) | 0.0174 (8) | |
C14 | 0.5576 (4) | 0.1677 (3) | 0.07063 (19) | 0.0262 (9) | |
H14 | 0.5953 | 0.1452 | 0.0378 | 0.031* | |
C15 | 0.4815 (4) | 0.2485 (3) | 0.0634 (2) | 0.0312 (10) | |
H15 | 0.4680 | 0.2814 | 0.0258 | 0.037* | |
C16 | 0.4259 (3) | 0.2808 (3) | 0.1108 (2) | 0.0263 (9) | |
H16 | 0.3738 | 0.3358 | 0.1059 | 0.032* | |
C17 | 0.4458 (4) | 0.2332 (3) | 0.1654 (2) | 0.0270 (9) | |
H17 | 0.4071 | 0.2554 | 0.1980 | 0.032* | |
C18 | 0.5218 (3) | 0.1532 (3) | 0.17325 (19) | 0.0235 (9) | |
H18 | 0.5350 | 0.1212 | 0.2112 | 0.028* | |
C19 | 1.1083 (3) | −0.0236 (3) | 0.27520 (18) | 0.0208 (8) | |
C20 | 1.1525 (4) | 0.0325 (3) | 0.2312 (2) | 0.0302 (9) | |
H20 | 1.1057 | 0.0836 | 0.2113 | 0.036* | |
C21 | 1.2636 (4) | 0.0153 (4) | 0.2158 (2) | 0.0386 (11) | |
H21 | 1.2933 | 0.0554 | 0.1863 | 0.046* | |
C22 | 1.3311 (4) | −0.0599 (4) | 0.2434 (2) | 0.0453 (13) | |
H22 | 1.4073 | −0.0719 | 0.2329 | 0.054* | |
C23 | 1.2881 (4) | −0.1174 (5) | 0.2859 (3) | 0.0564 (16) | |
H23 | 1.3347 | −0.1695 | 0.3047 | 0.068* | |
C24 | 1.1766 (4) | −0.1002 (4) | 0.3019 (2) | 0.0398 (12) | |
H24 | 1.1473 | −0.1410 | 0.3312 | 0.048* | |
C25 | 0.9431 (3) | −0.0782 (3) | 0.35564 (17) | 0.0192 (8) | |
C26 | 0.9211 (4) | −0.1775 (3) | 0.3413 (2) | 0.0360 (11) | |
H26 | 0.9176 | −0.1988 | 0.3008 | 0.043* | |
C27 | 0.9041 (5) | −0.2453 (3) | 0.3856 (2) | 0.0386 (12) | |
H27 | 0.8911 | −0.3133 | 0.3753 | 0.046* | |
C28 | 0.9056 (4) | −0.2162 (3) | 0.4437 (2) | 0.0321 (10) | |
H28 | 0.8964 | −0.2636 | 0.4741 | 0.038* | |
C29 | 0.9204 (5) | −0.1177 (4) | 0.4578 (2) | 0.0531 (15) | |
H29 | 0.9176 | −0.0963 | 0.4979 | 0.064* | |
C30 | 0.9397 (5) | −0.0481 (4) | 0.4137 (2) | 0.0456 (13) | |
H30 | 0.9504 | 0.0201 | 0.4241 | 0.055* | |
C31 | 0.9927 (3) | 0.1291 (3) | 0.33214 (17) | 0.0189 (8) | |
C32 | 1.0999 (4) | 0.1501 (3) | 0.36455 (19) | 0.0265 (9) | |
H32 | 1.1597 | 0.1011 | 0.3688 | 0.032* | |
C33 | 1.1200 (4) | 0.2435 (3) | 0.3910 (2) | 0.0309 (10) | |
H33 | 1.1936 | 0.2577 | 0.4133 | 0.037* | |
C34 | 1.0339 (4) | 0.3151 (3) | 0.3849 (2) | 0.0309 (10) | |
H34 | 1.0482 | 0.3784 | 0.4031 | 0.037* | |
C35 | 0.9261 (4) | 0.2946 (3) | 0.3522 (2) | 0.0349 (11) | |
H35 | 0.8667 | 0.3440 | 0.3477 | 0.042* | |
C36 | 0.9057 (4) | 0.2014 (3) | 0.32603 (19) | 0.0264 (9) | |
H36 | 0.8319 | 0.1871 | 0.3039 | 0.032* | |
C38 | 0.6767 (8) | 0.4657 (6) | 0.0342 (4) | 0.091 (2)* | |
C37 | 0.6448 (15) | 0.4650 (12) | −0.0243 (8) | 0.089 (5)* | 0.50 |
C40 | 0.4782 (7) | 0.5159 (5) | 0.0497 (4) | 0.077 (2)* | |
H99 | 0.894 (5) | 0.020 (4) | 0.180 (3) | 0.057 (16)* | |
C41 | 0.4471 (12) | 0.5151 (9) | −0.0032 (7) | 0.064 (3)* | 0.50 |
C39 | 0.6047 (16) | 0.4962 (11) | 0.0734 (8) | 0.088 (5)* | 0.50 |
U11 | U22 | U33 | U12 | U13 | U23 | |
Pt1 | 0.01457 (8) | 0.02045 (9) | 0.01384 (9) | 0.00028 (5) | 0.00079 (5) | −0.00044 (5) |
Br1 | 0.01918 (19) | 0.0317 (2) | 0.0202 (2) | −0.00030 (15) | 0.00508 (15) | 0.00233 (15) |
P1 | 0.0146 (4) | 0.0182 (4) | 0.0140 (5) | 0.0003 (3) | 0.0008 (4) | −0.0004 (4) |
P2 | 0.0149 (4) | 0.0191 (5) | 0.0141 (5) | −0.0005 (3) | 0.0008 (4) | −0.0003 (4) |
C1 | 0.0204 (19) | 0.0206 (19) | 0.020 (2) | −0.0010 (15) | 0.0070 (16) | −0.0007 (15) |
C2 | 0.033 (2) | 0.024 (2) | 0.022 (2) | −0.0006 (17) | 0.0011 (18) | −0.0008 (16) |
C3 | 0.054 (3) | 0.024 (2) | 0.025 (3) | −0.001 (2) | −0.001 (2) | 0.0054 (17) |
C4 | 0.043 (3) | 0.025 (2) | 0.039 (3) | −0.0131 (19) | 0.009 (2) | −0.0037 (19) |
C5 | 0.026 (2) | 0.035 (2) | 0.035 (3) | −0.0088 (18) | 0.002 (2) | −0.0041 (19) |
C6 | 0.019 (2) | 0.025 (2) | 0.027 (2) | −0.0013 (15) | 0.0024 (17) | −0.0002 (16) |
C7 | 0.0180 (18) | 0.0226 (19) | 0.0145 (19) | 0.0055 (14) | 0.0012 (14) | 0.0032 (14) |
C8 | 0.0146 (18) | 0.025 (2) | 0.018 (2) | 0.0046 (15) | 0.0009 (15) | 0.0026 (15) |
C9 | 0.026 (2) | 0.026 (2) | 0.022 (2) | 0.0091 (16) | 0.0027 (17) | −0.0024 (16) |
C10 | 0.030 (2) | 0.036 (2) | 0.020 (2) | 0.0087 (18) | 0.0078 (18) | 0.0030 (17) |
C11 | 0.024 (2) | 0.034 (2) | 0.025 (2) | −0.0040 (17) | 0.0067 (18) | 0.0031 (18) |
C12 | 0.021 (2) | 0.026 (2) | 0.024 (2) | −0.0020 (16) | 0.0021 (17) | −0.0015 (16) |
C13 | 0.0136 (18) | 0.0184 (18) | 0.019 (2) | −0.0022 (14) | −0.0023 (15) | −0.0042 (14) |
C14 | 0.030 (2) | 0.028 (2) | 0.021 (2) | 0.0056 (17) | 0.0037 (18) | −0.0003 (17) |
C15 | 0.037 (2) | 0.027 (2) | 0.029 (3) | 0.0074 (18) | −0.001 (2) | 0.0072 (18) |
C16 | 0.021 (2) | 0.0187 (19) | 0.038 (3) | 0.0012 (15) | 0.0009 (18) | −0.0027 (17) |
C17 | 0.028 (2) | 0.024 (2) | 0.031 (3) | 0.0027 (17) | 0.0100 (19) | −0.0033 (17) |
C18 | 0.022 (2) | 0.024 (2) | 0.025 (2) | 0.0030 (16) | 0.0054 (17) | 0.0044 (16) |
C19 | 0.0173 (18) | 0.0256 (19) | 0.020 (2) | −0.0001 (15) | 0.0034 (15) | −0.0027 (16) |
C20 | 0.025 (2) | 0.036 (2) | 0.030 (2) | −0.0019 (18) | 0.0060 (18) | −0.0006 (19) |
C21 | 0.028 (2) | 0.055 (3) | 0.036 (3) | −0.010 (2) | 0.015 (2) | −0.004 (2) |
C22 | 0.019 (2) | 0.079 (4) | 0.040 (3) | 0.001 (2) | 0.011 (2) | −0.013 (3) |
C23 | 0.025 (3) | 0.077 (4) | 0.068 (4) | 0.025 (3) | 0.009 (3) | 0.016 (3) |
C24 | 0.028 (2) | 0.054 (3) | 0.039 (3) | 0.014 (2) | 0.010 (2) | 0.013 (2) |
C25 | 0.0132 (17) | 0.025 (2) | 0.019 (2) | −0.0017 (14) | 0.0016 (15) | 0.0016 (15) |
C26 | 0.062 (3) | 0.026 (2) | 0.022 (2) | −0.008 (2) | 0.009 (2) | −0.0033 (17) |
C27 | 0.059 (3) | 0.021 (2) | 0.038 (3) | −0.009 (2) | 0.013 (2) | 0.0014 (19) |
C28 | 0.040 (3) | 0.033 (2) | 0.022 (2) | −0.0061 (19) | 0.001 (2) | 0.0099 (18) |
C29 | 0.093 (5) | 0.045 (3) | 0.021 (3) | −0.019 (3) | 0.005 (3) | −0.001 (2) |
C30 | 0.078 (4) | 0.033 (2) | 0.025 (3) | −0.019 (3) | 0.004 (2) | 0.000 (2) |
C31 | 0.0205 (19) | 0.0189 (18) | 0.018 (2) | −0.0018 (14) | 0.0034 (16) | 0.0013 (14) |
C32 | 0.023 (2) | 0.029 (2) | 0.026 (2) | −0.0011 (16) | −0.0004 (18) | −0.0024 (17) |
C33 | 0.029 (2) | 0.034 (2) | 0.031 (3) | −0.0085 (18) | 0.0063 (19) | −0.0067 (19) |
C34 | 0.038 (3) | 0.026 (2) | 0.030 (3) | −0.0093 (18) | 0.008 (2) | −0.0068 (18) |
C35 | 0.038 (3) | 0.023 (2) | 0.043 (3) | 0.0012 (18) | 0.007 (2) | −0.0043 (19) |
C36 | 0.028 (2) | 0.022 (2) | 0.029 (2) | 0.0018 (16) | 0.0002 (18) | −0.0032 (17) |
Pt1—P2 | 2.2749 (12) | C20—H20 | 0.9500 |
Pt1—P1 | 2.2805 (12) | C21—C22 | 1.375 (8) |
Pt1—Br1 | 2.5347 (8) | C21—H21 | 0.9500 |
Pt1—H99 | 1.38 (6) | C22—C23 | 1.367 (8) |
P1—C1 | 1.816 (4) | C22—H22 | 0.9500 |
P1—C7 | 1.831 (4) | C23—C24 | 1.395 (6) |
P1—C13 | 1.833 (4) | C23—H23 | 0.9500 |
P2—C25 | 1.821 (4) | C24—H24 | 0.9500 |
P2—C31 | 1.823 (4) | C25—C30 | 1.371 (6) |
P2—C19 | 1.824 (4) | C25—C26 | 1.389 (6) |
C1—C6 | 1.385 (5) | C26—C27 | 1.381 (6) |
C1—C2 | 1.398 (5) | C26—H26 | 0.9500 |
C2—C3 | 1.384 (6) | C27—C28 | 1.360 (6) |
C2—H2 | 0.9500 | C27—H27 | 0.9500 |
C3—C4 | 1.375 (7) | C28—C29 | 1.368 (7) |
C3—H3 | 0.9500 | C28—H28 | 0.9500 |
C4—C5 | 1.386 (6) | C29—C30 | 1.399 (7) |
C4—H4 | 0.9500 | C29—H29 | 0.9500 |
C5—C6 | 1.399 (6) | C30—H30 | 0.9500 |
C5—H5 | 0.9500 | C31—C32 | 1.383 (5) |
C6—H6 | 0.9500 | C31—C36 | 1.391 (5) |
C7—C8 | 1.393 (5) | C32—C33 | 1.397 (6) |
C7—C12 | 1.397 (5) | C32—H32 | 0.9500 |
C8—C9 | 1.388 (5) | C33—C34 | 1.376 (6) |
C8—H8 | 0.9500 | C33—H33 | 0.9500 |
C9—C10 | 1.389 (6) | C34—C35 | 1.392 (6) |
C9—H9 | 0.9500 | C34—H34 | 0.9500 |
C10—C11 | 1.387 (6) | C35—C36 | 1.392 (6) |
C10—H10 | 0.9500 | C35—H35 | 0.9500 |
C11—C12 | 1.374 (6) | C36—H36 | 0.9500 |
C11—H11 | 0.9500 | C38—C37 | 1.319 (18) |
C12—H12 | 0.9500 | C38—C39 | 1.345 (19) |
C13—C18 | 1.384 (5) | C38—C41i | 1.529 (15) |
C13—C14 | 1.402 (5) | C37—C41i | 1.32 (2) |
C14—C15 | 1.392 (6) | C37—C40i | 1.484 (18) |
C14—H14 | 0.9500 | C40—C41 | 1.198 (15) |
C15—C16 | 1.378 (6) | C40—C37i | 1.484 (18) |
C15—H15 | 0.9500 | C40—C41i | 1.491 (16) |
C16—C17 | 1.376 (6) | C40—C39 | 1.512 (19) |
C16—H16 | 0.9500 | C41—C41i | 1.28 (3) |
C17—C18 | 1.384 (5) | C41—C37i | 1.32 (2) |
C17—H17 | 0.9500 | C41—C40i | 1.491 (16) |
C18—H18 | 0.9500 | C41—C38i | 1.529 (15) |
C19—C24 | 1.386 (6) | C41—C39i | 1.62 (2) |
C19—C20 | 1.389 (6) | C39—C41i | 1.62 (2) |
C20—C21 | 1.385 (6) | ||
P2—Pt1—P1 | 172.73 (3) | C22—C21—C20 | 120.0 (5) |
P2—Pt1—Br1 | 92.10 (3) | C22—C21—H21 | 120.0 |
P1—Pt1—Br1 | 94.57 (3) | C20—C21—H21 | 120.0 |
P2—Pt1—H99 | 88 (2) | C23—C22—C21 | 119.8 (4) |
P1—Pt1—H99 | 85 (2) | C23—C22—H22 | 120.1 |
Br1—Pt1—H99 | 177 (2) | C21—C22—H22 | 120.1 |
C1—P1—C7 | 104.64 (17) | C22—C23—C24 | 120.6 (5) |
C1—P1—C13 | 104.72 (17) | C22—C23—H23 | 119.7 |
C7—P1—C13 | 102.54 (17) | C24—C23—H23 | 119.7 |
C1—P1—Pt1 | 112.48 (13) | C19—C24—C23 | 120.2 (5) |
C7—P1—Pt1 | 113.87 (13) | C19—C24—H24 | 119.9 |
C13—P1—Pt1 | 117.25 (12) | C23—C24—H24 | 119.9 |
C25—P2—C31 | 105.78 (17) | C30—C25—C26 | 118.6 (4) |
C25—P2—C19 | 104.02 (18) | C30—C25—P2 | 122.3 (3) |
C31—P2—C19 | 102.00 (17) | C26—C25—P2 | 118.9 (3) |
C25—P2—Pt1 | 113.74 (12) | C27—C26—C25 | 120.4 (4) |
C31—P2—Pt1 | 112.60 (13) | C27—C26—H26 | 119.8 |
C19—P2—Pt1 | 117.36 (13) | C25—C26—H26 | 119.8 |
C6—C1—C2 | 119.0 (4) | C28—C27—C26 | 120.9 (4) |
C6—C1—P1 | 122.0 (3) | C28—C27—H27 | 119.5 |
C2—C1—P1 | 119.0 (3) | C26—C27—H27 | 119.5 |
C3—C2—C1 | 120.3 (4) | C27—C28—C29 | 119.2 (4) |
C3—C2—H2 | 119.9 | C27—C28—H28 | 120.4 |
C1—C2—H2 | 119.9 | C29—C28—H28 | 120.4 |
C4—C3—C2 | 120.5 (4) | C28—C29—C30 | 120.7 (5) |
C4—C3—H3 | 119.8 | C28—C29—H29 | 119.6 |
C2—C3—H3 | 119.8 | C30—C29—H29 | 119.6 |
C3—C4—C5 | 120.1 (4) | C25—C30—C29 | 120.0 (4) |
C3—C4—H4 | 119.9 | C25—C30—H30 | 120.0 |
C5—C4—H4 | 119.9 | C29—C30—H30 | 120.0 |
C4—C5—C6 | 119.6 (4) | C32—C31—C36 | 119.6 (4) |
C4—C5—H5 | 120.2 | C32—C31—P2 | 121.0 (3) |
C6—C5—H5 | 120.2 | C36—C31—P2 | 119.3 (3) |
C1—C6—C5 | 120.5 (4) | C31—C32—C33 | 119.9 (4) |
C1—C6—H6 | 119.8 | C31—C32—H32 | 120.0 |
C5—C6—H6 | 119.8 | C33—C32—H32 | 120.0 |
C8—C7—C12 | 118.8 (4) | C34—C33—C32 | 120.4 (4) |
C8—C7—P1 | 122.3 (3) | C34—C33—H33 | 119.8 |
C12—C7—P1 | 118.8 (3) | C32—C33—H33 | 119.8 |
C9—C8—C7 | 120.6 (4) | C33—C34—C35 | 119.9 (4) |
C9—C8—H8 | 119.7 | C33—C34—H34 | 120.0 |
C7—C8—H8 | 119.7 | C35—C34—H34 | 120.0 |
C8—C9—C10 | 120.0 (4) | C36—C35—C34 | 119.7 (4) |
C8—C9—H9 | 120.0 | C36—C35—H35 | 120.2 |
C10—C9—H9 | 120.0 | C34—C35—H35 | 120.2 |
C11—C10—C9 | 119.4 (4) | C31—C36—C35 | 120.4 (4) |
C11—C10—H10 | 120.3 | C31—C36—H36 | 119.8 |
C9—C10—H10 | 120.3 | C35—C36—H36 | 119.8 |
C12—C11—C10 | 120.8 (4) | C37—C38—C39 | 122.4 (13) |
C12—C11—H11 | 119.6 | C37—C38—C41i | 54.4 (10) |
C10—C11—H11 | 119.6 | C39—C38—C41i | 68.4 (10) |
C11—C12—C7 | 120.4 (4) | C41i—C37—C38 | 71.0 (12) |
C11—C12—H12 | 119.8 | C41i—C37—C40i | 50.2 (9) |
C7—C12—H12 | 119.8 | C38—C37—C40i | 121.2 (14) |
C18—C13—C14 | 118.7 (3) | C41—C40—C37i | 57.6 (10) |
C18—C13—P1 | 119.4 (3) | C41—C40—C41i | 55.4 (11) |
C14—C13—P1 | 121.9 (3) | C37i—C40—C41i | 112.6 (11) |
C15—C14—C13 | 120.2 (4) | C41—C40—C39 | 120.5 (12) |
C15—C14—H14 | 119.9 | C37i—C40—C39 | 178.0 (12) |
C13—C14—H14 | 119.9 | C41i—C40—C39 | 65.5 (9) |
C16—C15—C14 | 120.1 (4) | C40—C41—C41i | 74.0 (13) |
C16—C15—H15 | 120.0 | C40—C41—C37i | 72.2 (12) |
C14—C15—H15 | 120.0 | C41i—C41—C37i | 145 (2) |
C17—C16—C15 | 119.9 (4) | C40—C41—C40i | 124.6 (11) |
C17—C16—H16 | 120.1 | C41i—C41—C40i | 50.6 (11) |
C15—C16—H16 | 120.1 | C37i—C41—C40i | 162.0 (15) |
C16—C17—C18 | 120.6 (4) | C40—C41—C38i | 126.8 (12) |
C16—C17—H17 | 119.7 | C41i—C41—C38i | 158.2 (19) |
C18—C17—H17 | 119.7 | C37i—C41—C38i | 54.6 (9) |
C17—C18—C13 | 120.6 (4) | C40i—C41—C38i | 108.3 (11) |
C17—C18—H18 | 119.7 | C40—C41—C39i | 173.6 (14) |
C13—C18—H18 | 119.7 | C41i—C41—C39i | 108.1 (17) |
C24—C19—C20 | 118.3 (4) | C37i—C41—C39i | 104.7 (13) |
C24—C19—P2 | 123.5 (3) | C40i—C41—C39i | 57.9 (9) |
C20—C19—P2 | 118.2 (3) | C38i—C41—C39i | 50.4 (8) |
C21—C20—C19 | 121.0 (4) | C38—C39—C40 | 117.8 (14) |
C21—C20—H20 | 119.5 | C38—C39—C41i | 61.2 (10) |
C19—C20—H20 | 119.5 | C40—C39—C41i | 56.7 (9) |
Br1—Pt1—P1—C1 | −52.33 (13) | P2—C19—C20—C21 | 176.4 (3) |
Br1—Pt1—P1—C7 | −171.16 (13) | C19—C20—C21—C22 | 1.5 (7) |
Br1—Pt1—P1—C13 | 69.17 (14) | C20—C21—C22—C23 | −0.1 (8) |
Br1—Pt1—P2—C25 | 37.45 (14) | C21—C22—C23—C24 | −0.3 (9) |
Br1—Pt1—P2—C31 | −82.87 (14) | C20—C19—C24—C23 | 2.0 (7) |
Br1—Pt1—P2—C19 | 159.16 (14) | P2—C19—C24—C23 | −176.8 (4) |
C7—P1—C1—C6 | −79.7 (4) | C22—C23—C24—C19 | −0.7 (9) |
C13—P1—C1—C6 | 27.8 (4) | C31—P2—C25—C30 | 5.5 (4) |
Pt1—P1—C1—C6 | 156.2 (3) | C19—P2—C25—C30 | 112.5 (4) |
C7—P1—C1—C2 | 99.7 (3) | Pt1—P2—C25—C30 | −118.6 (4) |
C13—P1—C1—C2 | −152.8 (3) | C31—P2—C25—C26 | −179.3 (3) |
Pt1—P1—C1—C2 | −24.4 (4) | C19—P2—C25—C26 | −72.2 (4) |
C6—C1—C2—C3 | 0.0 (6) | Pt1—P2—C25—C26 | 56.6 (4) |
P1—C1—C2—C3 | −179.4 (3) | C30—C25—C26—C27 | −4.4 (7) |
C1—C2—C3—C4 | −0.6 (7) | P2—C25—C26—C27 | −179.8 (4) |
C2—C3—C4—C5 | 0.7 (7) | C25—C26—C27—C28 | 1.7 (8) |
C3—C4—C5—C6 | −0.2 (7) | C26—C27—C28—C29 | 2.1 (8) |
C2—C1—C6—C5 | 0.5 (6) | C27—C28—C29—C30 | −3.2 (9) |
P1—C1—C6—C5 | 179.9 (3) | C26—C25—C30—C29 | 3.3 (8) |
C4—C5—C6—C1 | −0.4 (7) | P2—C25—C30—C29 | 178.6 (4) |
C1—P1—C7—C8 | 6.8 (3) | C28—C29—C30—C25 | 0.4 (9) |
C13—P1—C7—C8 | −102.3 (3) | C25—P2—C31—C32 | 75.6 (4) |
Pt1—P1—C7—C8 | 130.0 (3) | C19—P2—C31—C32 | −32.9 (4) |
C1—P1—C7—C12 | −175.8 (3) | Pt1—P2—C31—C32 | −159.6 (3) |
C13—P1—C7—C12 | 75.1 (3) | C25—P2—C31—C36 | −105.7 (3) |
Pt1—P1—C7—C12 | −52.6 (3) | C19—P2—C31—C36 | 145.8 (3) |
C12—C7—C8—C9 | 1.2 (5) | Pt1—P2—C31—C36 | 19.1 (4) |
P1—C7—C8—C9 | 178.6 (3) | C36—C31—C32—C33 | 0.1 (6) |
C7—C8—C9—C10 | −1.6 (6) | P2—C31—C32—C33 | 178.7 (3) |
C8—C9—C10—C11 | 1.0 (6) | C31—C32—C33—C34 | −0.1 (7) |
C9—C10—C11—C12 | 0.0 (6) | C32—C33—C34—C35 | −0.1 (7) |
C10—C11—C12—C7 | −0.4 (6) | C33—C34—C35—C36 | 0.4 (7) |
C8—C7—C12—C11 | −0.2 (6) | C32—C31—C36—C35 | 0.2 (6) |
P1—C7—C12—C11 | −177.7 (3) | P2—C31—C36—C35 | −178.5 (3) |
C1—P1—C13—C18 | 76.5 (3) | C34—C35—C36—C31 | −0.5 (7) |
C7—P1—C13—C18 | −174.4 (3) | C39—C38—C37—C41i | −8.6 (16) |
Pt1—P1—C13—C18 | −48.9 (3) | C39—C38—C37—C40i | −9 (2) |
C1—P1—C13—C14 | −102.2 (3) | C41i—C38—C37—C40i | −0.3 (10) |
C7—P1—C13—C14 | 6.8 (3) | C37i—C40—C41—C41i | −172.6 (17) |
Pt1—P1—C13—C14 | 132.3 (3) | C39—C40—C41—C41i | 7.5 (16) |
C18—C13—C14—C15 | 0.6 (6) | C41i—C40—C41—C37i | 172.6 (17) |
P1—C13—C14—C15 | 179.3 (3) | C39—C40—C41—C37i | −179.8 (12) |
C13—C14—C15—C16 | −0.6 (6) | C37i—C40—C41—C40i | −172.6 (17) |
C14—C15—C16—C17 | 0.2 (6) | C41i—C40—C41—C40i | 0.000 (1) |
C15—C16—C17—C18 | 0.2 (6) | C39—C40—C41—C40i | 7.5 (16) |
C16—C17—C18—C13 | −0.2 (6) | C37i—C40—C41—C38i | 0.4 (12) |
C14—C13—C18—C17 | −0.2 (6) | C41i—C40—C41—C38i | 173 (2) |
P1—C13—C18—C17 | −179.0 (3) | C39—C40—C41—C38i | −179.5 (11) |
C25—P2—C19—C24 | 1.0 (4) | C37—C38—C39—C40 | 9 (2) |
C31—P2—C19—C24 | 110.8 (4) | C41i—C38—C39—C40 | 1.4 (11) |
Pt1—P2—C19—C24 | −125.7 (4) | C37—C38—C39—C41i | 7.5 (14) |
C25—P2—C19—C20 | −177.9 (3) | C41—C40—C39—C38 | −8.3 (18) |
C31—P2—C19—C20 | −68.0 (4) | C41i—C40—C39—C38 | −1.5 (11) |
Pt1—P2—C19—C20 | 55.5 (4) | C41—C40—C39—C41i | −6.8 (15) |
C24—C19—C20—C21 | −2.5 (7) |
Symmetry code: (i) −x+1, −y+1, −z. |