Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270101007788/gd1151sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270101007788/gd1151Isup2.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270101007788/gd1151IIsup3.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270101007788/gd1151IIIsup4.hkl |
CCDC references: 170165; 170166; 170167
For related literature, see: Barton & Srivastava (1995); Boocock et al. (1981); Gaft et al. (1983); Kennedy (1986); Marshall et al. (1967); Mutterties & Knoth (1968); Paxson & Hawthorne (1975).
The synthesis of compound (I) was effected by the reaction of [RuCl2(PPh3)3] (0.38 g, 0.4 mmol), [PtCl2(PPh3)2] (0.32 g, 0.4 mmol) and (NEt4)2B10H10 (0.16 g, 0.4 mmol) in refluxing methanol (65 ml) for 68 h under dry nitrogen. The resulting mixture was filtered. The yellowish precipitate was dissolved in the minimum of dichloromethane and chromatographed using dichloromethane/light petroleum (b.p. 303–333 K) (4:1) as the eluting medium to give compound (I) (Rf = 0.72). Compounds (II) and (III) were synthesized by the reaction of [PtCl2(PPh3)2] (0.284 g, 0.35 mmol) and (NEt4)2B10H10 (0.265 g, 0.7 mmol) with i-PrOH under reflux for 132 h in an atmosphere of dry nitrogen. After filtration, the resulting solution was reduced in volume and chromatographed using dichloromethane/light petrolem (4:1) as the eluting medium to give the two compounds at Rf = 0.83 for (II) and Rf = 0.45 for (III). All three products were recrystallized from n-hexane-dichloromethane solution.
H atoms, other than the B—H—B bridging atoms, were treated as riding, with B—H(general), C—H(phenyl), C—H(—CH), C—H(—CH2) and C—H(—CH3) distances of 1.10, 0.93, 0.98, 0.97 and 0.96 Å, respectively. In all three compounds, the bridging H atoms were refined isotropically.
Data collection: MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1992) for (I), (III); CAD-4 Manual (Enraf-Nonius, 1988) for (II). Cell refinement: MSC/AFC Diffractometer Control Software for (I), (III); CAD-4 Manual for (II). Data reduction: TEXSAN (Molecular Structure Corporation, 1985) for (I), (III); SDP-Plus (Frenz, 1985) for (II). For all compounds, program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ZORTEP (Zsolnai, 1994); software used to prepare material for publication: SHELXL97.
[Pt(CH14B10O)(C18H15P)2]·0.5CH2Cl2 | F(000) = 1812 |
Mr = 912.32 | Dx = 1.426 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71069 Å |
a = 12.850 (2) Å | Cell parameters from 25 reflections |
b = 25.824 (7) Å | θ = 6.8–10.8° |
c = 13.308 (2) Å | µ = 3.47 mm−1 |
β = 105.77 (1)° | T = 293 K |
V = 4249.9 (15) Å3 | Prism, yellow |
Z = 4 | 0.3 × 0.2 × 0.2 mm |
Rigaku AFC-7R diffractometer | 5607 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.048 |
Graphite monochromator | θmax = 25°, θmin = 2.3° |
θ/2θ scans | h = 0→13 |
Absorption correction: ψ scans (North et al., 1968) | k = 0→30 |
Tmin = 0.423, Tmax = 0.544 | l = −15→15 |
7336 measured reflections | 3 standard reflections every 200 reflections |
6984 independent reflections | intensity decay: −1.3 |
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)] = 0.037 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.105 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.04 | w = 1/[σ2(Fo2) + (0.0601P)2 + 4.5436P] where P = (Fo2 + 2Fc2)/3 |
6984 reflections | (Δ/σ)max = 0.030 |
495 parameters | Δρmax = 1.98 e Å−3 |
2 restraints | Δρmin = −1.71 e Å−3 |
[Pt(CH14B10O)(C18H15P)2]·0.5CH2Cl2 | V = 4249.9 (15) Å3 |
Mr = 912.32 | Z = 4 |
Monoclinic, P21/n | Mo Kα radiation |
a = 12.850 (2) Å | µ = 3.47 mm−1 |
b = 25.824 (7) Å | T = 293 K |
c = 13.308 (2) Å | 0.3 × 0.2 × 0.2 mm |
β = 105.77 (1)° |
Rigaku AFC-7R diffractometer | 5607 reflections with I > 2σ(I) |
Absorption correction: ψ scans (North et al., 1968) | Rint = 0.048 |
Tmin = 0.423, Tmax = 0.544 | 3 standard reflections every 200 reflections |
7336 measured reflections | intensity decay: −1.3 |
6984 independent reflections |
R[F2 > 2σ(F2)] = 0.037 | 2 restraints |
wR(F2) = 0.105 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.04 | Δρmax = 1.98 e Å−3 |
6984 reflections | Δρmin = −1.71 e Å−3 |
495 parameters |
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 | Occ. (<1) | |
Pt7 | 0.699111 (18) | 0.192397 (8) | 0.859548 (16) | 0.02893 (10) | |
P1 | 0.77647 (13) | 0.14883 (6) | 0.73977 (12) | 0.0335 (3) | |
P2 | 0.61525 (14) | 0.12207 (6) | 0.91964 (13) | 0.0369 (4) | |
O1 | 0.4562 (4) | 0.21328 (18) | 0.8252 (3) | 0.0437 (11) | |
C1 | 0.3641 (6) | 0.2219 (3) | 0.7389 (6) | 0.059 (2) | |
H1A | 0.3093 | 0.1968 | 0.7401 | 0.089* | |
H1B | 0.3845 | 0.2187 | 0.6750 | 0.089* | |
H1C | 0.3364 | 0.2561 | 0.7436 | 0.089* | |
C11 | 0.7424 (5) | 0.1844 (2) | 0.6165 (5) | 0.0354 (14) | |
C12 | 0.6346 (6) | 0.1948 (2) | 0.5681 (6) | 0.0462 (16) | |
H12 | 0.5826 | 0.1868 | 0.6025 | 0.055* | |
C13 | 0.6030 (6) | 0.2167 (3) | 0.4704 (6) | 0.0541 (18) | |
H13 | 0.5300 | 0.2223 | 0.4385 | 0.065* | |
C14 | 0.6789 (7) | 0.2303 (3) | 0.4199 (6) | 0.061 (2) | |
H14 | 0.6575 | 0.2441 | 0.3529 | 0.073* | |
C15 | 0.7870 (6) | 0.2234 (3) | 0.4692 (6) | 0.060 (2) | |
H15 | 0.8389 | 0.2341 | 0.4367 | 0.072* | |
C16 | 0.8187 (6) | 0.2007 (3) | 0.5662 (6) | 0.0495 (17) | |
H16 | 0.8919 | 0.1962 | 0.5987 | 0.059* | |
C21 | 0.7404 (5) | 0.0820 (2) | 0.6954 (5) | 0.0386 (14) | |
C22 | 0.6695 (6) | 0.0703 (3) | 0.5996 (6) | 0.0526 (18) | |
H22 | 0.6372 | 0.0971 | 0.5554 | 0.063* | |
C23 | 0.6456 (7) | 0.0199 (3) | 0.5683 (7) | 0.069 (2) | |
H23 | 0.5957 | 0.0126 | 0.5049 | 0.082* | |
C24 | 0.6967 (8) | −0.0194 (3) | 0.6322 (8) | 0.080 (3) | |
H24 | 0.6818 | −0.0535 | 0.6113 | 0.096* | |
C25 | 0.7696 (8) | −0.0091 (3) | 0.7265 (7) | 0.069 (2) | |
H25 | 0.8042 | −0.0360 | 0.7692 | 0.083* | |
C26 | 0.7905 (6) | 0.0415 (3) | 0.7568 (6) | 0.0519 (18) | |
H26 | 0.8400 | 0.0486 | 0.8206 | 0.062* | |
C31 | 0.9225 (5) | 0.1433 (2) | 0.7838 (5) | 0.0394 (14) | |
C32 | 0.9807 (6) | 0.1205 (3) | 0.7199 (6) | 0.0540 (18) | |
H32 | 0.9444 | 0.1094 | 0.6531 | 0.065* | |
C33 | 1.0912 (6) | 0.1147 (3) | 0.7553 (7) | 0.065 (2) | |
H33 | 1.1290 | 0.1003 | 0.7116 | 0.079* | |
C34 | 1.1455 (6) | 0.1296 (3) | 0.8532 (8) | 0.066 (2) | |
H34 | 1.2202 | 0.1255 | 0.8760 | 0.079* | |
C35 | 1.0910 (6) | 0.1506 (3) | 0.9189 (7) | 0.060 (2) | |
H35 | 1.1282 | 0.1598 | 0.9867 | 0.072* | |
C36 | 0.9799 (6) | 0.1580 (3) | 0.8836 (5) | 0.0477 (17) | |
H36 | 0.9435 | 0.1732 | 0.9277 | 0.057* | |
C41 | 0.5037 (5) | 0.0890 (2) | 0.8277 (5) | 0.0394 (15) | |
C42 | 0.4790 (6) | 0.1019 (3) | 0.7232 (5) | 0.0468 (16) | |
H42 | 0.5198 | 0.1269 | 0.7011 | 0.056* | |
C43 | 0.3953 (6) | 0.0784 (3) | 0.6515 (6) | 0.061 (2) | |
H43 | 0.3793 | 0.0875 | 0.5814 | 0.073* | |
C44 | 0.3350 (7) | 0.0410 (4) | 0.6842 (8) | 0.075 (3) | |
H44 | 0.2791 | 0.0245 | 0.6355 | 0.090* | |
C45 | 0.3568 (8) | 0.0280 (3) | 0.7882 (8) | 0.078 (3) | |
H45 | 0.3157 | 0.0029 | 0.8098 | 0.094* | |
C46 | 0.4394 (7) | 0.0523 (3) | 0.8594 (6) | 0.062 (2) | |
H46 | 0.4530 | 0.0442 | 0.9298 | 0.075* | |
C51 | 0.7207 (6) | 0.0737 (3) | 0.9696 (6) | 0.0510 (18) | |
C52 | 0.7031 (7) | 0.0204 (3) | 0.9567 (7) | 0.066 (2) | |
H52 | 0.6352 | 0.0084 | 0.9200 | 0.079* | |
C53 | 0.7825 (10) | −0.0139 (4) | 0.9965 (9) | 0.092 (3) | |
H53 | 0.7696 | −0.0492 | 0.9862 | 0.110* | |
C54 | 0.8817 (10) | 0.0032 (5) | 1.0516 (9) | 0.104 (4) | |
H54 | 0.9361 | −0.0206 | 1.0794 | 0.124* | |
C55 | 0.9033 (8) | 0.0565 (4) | 1.0673 (8) | 0.090 (3) | |
H55 | 0.9714 | 0.0678 | 1.1049 | 0.108* | |
C56 | 0.8218 (6) | 0.0915 (3) | 1.0259 (6) | 0.063 (2) | |
H56 | 0.8344 | 0.1269 | 1.0357 | 0.075* | |
C61 | 0.5635 (5) | 0.1319 (2) | 1.0338 (5) | 0.0403 (15) | |
C62 | 0.6251 (8) | 0.1209 (4) | 1.1329 (6) | 0.089 (3) | |
H62 | 0.6954 | 0.1087 | 1.1437 | 0.106* | |
C63 | 0.5821 (10) | 0.1280 (5) | 1.2176 (7) | 0.114 (5) | |
H63 | 0.6244 | 0.1211 | 1.2849 | 0.137* | |
C64 | 0.4778 (9) | 0.1452 (4) | 1.2023 (7) | 0.095 (3) | |
H64 | 0.4488 | 0.1484 | 1.2588 | 0.114* | |
C65 | 0.4182 (8) | 0.1571 (4) | 1.1066 (7) | 0.077 (3) | |
H65 | 0.3483 | 0.1697 | 1.0966 | 0.093* | |
C66 | 0.4603 (6) | 0.1508 (3) | 1.0220 (6) | 0.058 (2) | |
H66 | 0.4180 | 0.1594 | 0.9556 | 0.070* | |
B1 | 0.7087 (7) | 0.3118 (3) | 0.9745 (7) | 0.0449 (18) | |
H1 | 0.7321 | 0.3322 | 1.0499 | 0.054* | |
B2 | 0.7851 (6) | 0.2598 (3) | 0.9467 (6) | 0.0383 (16) | |
H2 | 0.8578 | 0.2465 | 1.0058 | 0.046* | |
B3 | 0.6514 (6) | 0.2491 (3) | 0.9658 (5) | 0.0374 (16) | |
H3 | 0.6401 | 0.2295 | 1.0355 | 0.045* | |
B4 | 0.5714 (7) | 0.3031 (3) | 0.9086 (6) | 0.0429 (18) | |
H4 | 0.5079 | 0.3186 | 0.9413 | 0.052* | |
B5 | 0.6523 (7) | 0.3427 (3) | 0.8528 (6) | 0.0454 (19) | |
H5 | 0.6369 | 0.3846 | 0.8471 | 0.054* | |
B6 | 0.7867 (7) | 0.3196 (3) | 0.8829 (6) | 0.0417 (17) | |
H6 | 0.8579 | 0.3451 | 0.9003 | 0.050* | |
B8 | 0.5483 (6) | 0.2432 (3) | 0.8437 (5) | 0.0368 (16) | |
B9 | 0.5557 (7) | 0.3046 (3) | 0.7697 (6) | 0.0434 (18) | |
H9 | 0.4919 | 0.3072 | 0.6956 | 0.052* | |
B10 | 0.6993 (7) | 0.3158 (3) | 0.7552 (6) | 0.0434 (18) | |
H10 | 0.7010 | 0.3242 | 0.6746 | 0.052* | |
B11 | 0.7897 (6) | 0.2613 (3) | 0.8132 (6) | 0.0369 (16) | |
H11 | 0.8360 | 0.2456 | 0.7618 | 0.044* | |
H1U | 0.569 (5) | 0.261 (3) | 0.750 (5) | 0.053 (19)* | |
H2U | 0.718 (4) | 0.266 (2) | 0.741 (4) | 0.029 (15)* | |
Cl2 | 0.8352 (7) | 0.0758 (3) | 0.4255 (8) | 0.175 (4) | 0.50 |
Cl1 | 0.9635 (8) | 0.0140 (3) | 0.3448 (8) | 0.167 (4) | 0.50 |
C1S | 0.9467 (17) | 0.0601 (9) | 0.411 (3) | 0.170 (16) | 0.50 |
H1S | 0.9741 | 0.0903 | 0.3830 | 0.204* | 0.50 |
H2S | 0.9942 | 0.0546 | 0.4804 | 0.204* | 0.50 |
U11 | U22 | U33 | U12 | U13 | U23 | |
Pt7 | 0.03273 (16) | 0.02862 (13) | 0.02808 (13) | 0.00030 (10) | 0.01277 (9) | −0.00093 (9) |
P1 | 0.0356 (9) | 0.0338 (8) | 0.0339 (8) | 0.0007 (7) | 0.0142 (7) | −0.0043 (6) |
P2 | 0.0452 (10) | 0.0334 (8) | 0.0369 (8) | 0.0015 (7) | 0.0193 (7) | 0.0039 (6) |
O1 | 0.039 (3) | 0.050 (3) | 0.044 (3) | −0.009 (2) | 0.016 (2) | 0.003 (2) |
C1 | 0.046 (5) | 0.082 (6) | 0.048 (4) | −0.009 (4) | 0.010 (3) | 0.003 (4) |
C11 | 0.040 (4) | 0.036 (3) | 0.035 (3) | 0.001 (3) | 0.018 (3) | 0.000 (2) |
C12 | 0.041 (4) | 0.050 (4) | 0.053 (4) | −0.003 (3) | 0.024 (3) | 0.007 (3) |
C13 | 0.049 (4) | 0.058 (4) | 0.055 (4) | 0.006 (4) | 0.012 (3) | 0.009 (4) |
C14 | 0.072 (6) | 0.065 (5) | 0.049 (4) | 0.009 (4) | 0.023 (4) | 0.015 (4) |
C15 | 0.058 (5) | 0.071 (5) | 0.061 (5) | 0.004 (4) | 0.035 (4) | 0.020 (4) |
C16 | 0.043 (4) | 0.061 (4) | 0.050 (4) | 0.002 (3) | 0.021 (3) | 0.004 (3) |
C21 | 0.041 (4) | 0.035 (3) | 0.044 (3) | −0.004 (3) | 0.019 (3) | −0.012 (3) |
C22 | 0.054 (5) | 0.041 (4) | 0.057 (4) | 0.002 (3) | 0.006 (3) | −0.009 (3) |
C23 | 0.064 (5) | 0.061 (5) | 0.073 (6) | −0.009 (4) | 0.007 (4) | −0.025 (4) |
C24 | 0.106 (8) | 0.046 (5) | 0.095 (7) | −0.008 (5) | 0.039 (6) | −0.027 (5) |
C25 | 0.093 (7) | 0.047 (4) | 0.073 (6) | 0.008 (4) | 0.031 (5) | −0.005 (4) |
C26 | 0.070 (5) | 0.041 (4) | 0.049 (4) | −0.003 (3) | 0.023 (4) | −0.009 (3) |
C31 | 0.042 (4) | 0.034 (3) | 0.045 (4) | 0.004 (3) | 0.016 (3) | −0.001 (3) |
C32 | 0.046 (4) | 0.058 (4) | 0.059 (5) | 0.001 (3) | 0.015 (3) | −0.016 (4) |
C33 | 0.044 (5) | 0.065 (5) | 0.097 (7) | 0.011 (4) | 0.034 (5) | 0.002 (5) |
C34 | 0.034 (4) | 0.058 (5) | 0.102 (7) | 0.002 (4) | 0.014 (4) | 0.008 (5) |
C35 | 0.045 (5) | 0.053 (4) | 0.071 (5) | −0.003 (4) | −0.005 (4) | 0.004 (4) |
C36 | 0.052 (5) | 0.042 (4) | 0.047 (4) | 0.000 (3) | 0.010 (3) | −0.001 (3) |
C41 | 0.044 (4) | 0.033 (3) | 0.049 (4) | −0.005 (3) | 0.024 (3) | −0.003 (3) |
C42 | 0.051 (4) | 0.046 (4) | 0.046 (4) | −0.009 (3) | 0.018 (3) | −0.002 (3) |
C43 | 0.067 (5) | 0.060 (5) | 0.057 (5) | −0.008 (4) | 0.020 (4) | −0.013 (4) |
C44 | 0.066 (6) | 0.074 (6) | 0.084 (6) | −0.018 (5) | 0.017 (5) | −0.031 (5) |
C45 | 0.076 (6) | 0.067 (6) | 0.098 (7) | −0.037 (5) | 0.034 (5) | −0.012 (5) |
C46 | 0.076 (6) | 0.057 (5) | 0.062 (5) | −0.022 (4) | 0.032 (4) | 0.003 (4) |
C51 | 0.062 (5) | 0.053 (4) | 0.050 (4) | 0.018 (4) | 0.035 (4) | 0.017 (3) |
C52 | 0.077 (6) | 0.045 (4) | 0.091 (6) | 0.020 (4) | 0.048 (5) | 0.018 (4) |
C53 | 0.110 (9) | 0.068 (6) | 0.121 (9) | 0.040 (6) | 0.071 (8) | 0.038 (6) |
C54 | 0.108 (9) | 0.102 (8) | 0.119 (9) | 0.065 (8) | 0.062 (8) | 0.073 (7) |
C55 | 0.062 (6) | 0.128 (9) | 0.088 (7) | 0.044 (6) | 0.032 (5) | 0.048 (6) |
C56 | 0.061 (5) | 0.073 (5) | 0.058 (5) | 0.018 (4) | 0.023 (4) | 0.019 (4) |
C61 | 0.054 (4) | 0.033 (3) | 0.040 (3) | 0.004 (3) | 0.023 (3) | 0.002 (3) |
C62 | 0.090 (7) | 0.136 (9) | 0.044 (5) | 0.055 (6) | 0.024 (5) | 0.014 (5) |
C63 | 0.135 (10) | 0.176 (12) | 0.039 (5) | 0.070 (9) | 0.039 (6) | 0.011 (6) |
C64 | 0.113 (9) | 0.127 (9) | 0.064 (6) | 0.042 (7) | 0.057 (6) | 0.022 (6) |
C65 | 0.075 (6) | 0.101 (7) | 0.074 (6) | 0.016 (5) | 0.049 (5) | 0.021 (5) |
C66 | 0.054 (5) | 0.077 (5) | 0.051 (4) | 0.009 (4) | 0.029 (4) | 0.013 (4) |
B1 | 0.045 (5) | 0.038 (4) | 0.054 (5) | −0.001 (3) | 0.016 (4) | −0.012 (3) |
B2 | 0.043 (4) | 0.035 (4) | 0.040 (4) | −0.004 (3) | 0.016 (3) | −0.005 (3) |
B3 | 0.046 (5) | 0.035 (4) | 0.035 (4) | −0.003 (3) | 0.017 (3) | −0.002 (3) |
B4 | 0.045 (5) | 0.039 (4) | 0.048 (4) | −0.001 (3) | 0.020 (4) | −0.009 (3) |
B5 | 0.058 (5) | 0.030 (4) | 0.055 (5) | 0.001 (3) | 0.026 (4) | 0.000 (3) |
B6 | 0.044 (5) | 0.037 (4) | 0.047 (4) | −0.004 (3) | 0.017 (4) | −0.002 (3) |
B8 | 0.040 (4) | 0.041 (4) | 0.032 (3) | 0.004 (3) | 0.013 (3) | 0.004 (3) |
B9 | 0.049 (5) | 0.037 (4) | 0.047 (4) | 0.003 (3) | 0.016 (4) | 0.007 (3) |
B10 | 0.051 (5) | 0.040 (4) | 0.042 (4) | −0.001 (3) | 0.016 (4) | 0.006 (3) |
B11 | 0.041 (4) | 0.036 (4) | 0.035 (4) | −0.007 (3) | 0.013 (3) | −0.003 (3) |
Cl2 | 0.141 (7) | 0.136 (6) | 0.242 (11) | −0.038 (5) | 0.041 (7) | −0.085 (7) |
Cl1 | 0.183 (9) | 0.137 (7) | 0.213 (10) | −0.006 (6) | 0.107 (8) | −0.025 (6) |
C1S | 0.16 (3) | 0.12 (2) | 0.29 (4) | −0.089 (19) | 0.17 (3) | −0.12 (2) |
Pt7—B2 | 2.214 (7) | C51—C56 | 1.390 (11) |
Pt7—B3 | 2.234 (7) | C51—C52 | 1.397 (11) |
Pt7—B11 | 2.301 (7) | C52—C53 | 1.346 (12) |
Pt7—B8 | 2.303 (7) | C52—H52 | 0.9300 |
Pt7—P2 | 2.3595 (16) | C53—C54 | 1.360 (15) |
Pt7—P1 | 2.3783 (15) | C53—H53 | 0.9300 |
P1—C31 | 1.813 (7) | C54—C55 | 1.407 (16) |
P1—C11 | 1.827 (6) | C54—H54 | 0.9300 |
P1—C21 | 1.842 (6) | C55—C56 | 1.381 (11) |
P2—C41 | 1.824 (7) | C55—H55 | 0.9300 |
P2—C51 | 1.831 (7) | C56—H56 | 0.9300 |
P2—C61 | 1.834 (6) | C61—C62 | 1.371 (10) |
O1—B8 | 1.379 (9) | C61—C66 | 1.382 (10) |
O1—C1 | 1.425 (8) | C62—C63 | 1.396 (11) |
C1—H1A | 0.9600 | C62—H62 | 0.9300 |
C1—H1B | 0.9600 | C63—C64 | 1.373 (14) |
C1—H1C | 0.9600 | C63—H63 | 0.9300 |
C11—C12 | 1.386 (9) | C64—C65 | 1.332 (12) |
C11—C16 | 1.394 (9) | C64—H64 | 0.9300 |
C12—C13 | 1.374 (10) | C65—C66 | 1.385 (10) |
C12—H12 | 0.9300 | C65—H65 | 0.9300 |
C13—C14 | 1.372 (10) | C66—H66 | 0.9300 |
C13—H13 | 0.9300 | B1—B4 | 1.759 (12) |
C14—C15 | 1.377 (10) | B1—B2 | 1.760 (10) |
C14—H14 | 0.9300 | B1—B3 | 1.769 (10) |
C15—C16 | 1.374 (10) | B1—B5 | 1.773 (12) |
C15—H15 | 0.9300 | B1—B6 | 1.787 (11) |
C16—H16 | 0.9300 | B1—H1 | 1.1000 |
C21—C26 | 1.374 (10) | B2—B6 | 1.765 (10) |
C21—C22 | 1.384 (9) | B2—B11 | 1.793 (10) |
C22—C23 | 1.375 (10) | B2—B3 | 1.825 (10) |
C22—H22 | 0.9300 | B2—H2 | 1.1000 |
C23—C24 | 1.372 (12) | B3—B4 | 1.775 (10) |
C23—H23 | 0.9300 | B3—B8 | 1.803 (10) |
C24—C25 | 1.372 (12) | B3—H3 | 1.1000 |
C24—H24 | 0.9300 | B4—B8 | 1.756 (10) |
C25—C26 | 1.373 (10) | B4—B5 | 1.760 (11) |
C25—H25 | 0.9300 | B4—B9 | 1.804 (11) |
C26—H26 | 0.9300 | B4—H4 | 1.1000 |
C31—C36 | 1.386 (9) | B5—B10 | 1.720 (11) |
C31—C32 | 1.405 (9) | B5—B9 | 1.728 (11) |
C32—C33 | 1.378 (10) | B5—B6 | 1.766 (11) |
C32—H32 | 0.9300 | B5—H5 | 1.1000 |
C33—C34 | 1.356 (12) | B6—B10 | 1.766 (11) |
C33—H33 | 0.9300 | B6—B11 | 1.774 (10) |
C34—C35 | 1.373 (12) | B6—H6 | 1.1000 |
C34—H34 | 0.9300 | B8—B9 | 1.882 (10) |
C35—C36 | 1.389 (10) | B8—H1U | 1.43 (7) |
C35—H35 | 0.9300 | B9—B10 | 1.929 (12) |
C36—H36 | 0.9300 | B9—H9 | 1.1000 |
C41—C42 | 1.380 (9) | B9—H1U | 1.17 (7) |
C41—C46 | 1.397 (9) | B10—B11 | 1.854 (11) |
C42—C43 | 1.370 (10) | B10—H10 | 1.1000 |
C42—H42 | 0.9300 | B10—H2U | 1.33 (5) |
C43—C44 | 1.380 (12) | B11—H11 | 1.1000 |
C43—H43 | 0.9300 | B11—H2U | 1.15 (5) |
C44—C45 | 1.377 (13) | Cl2—C1S | 1.552 (16) |
C44—H44 | 0.9300 | Cl1—C1S | 1.531 (15) |
C45—C46 | 1.368 (11) | C1S—H1S | 0.9700 |
C45—H45 | 0.9300 | C1S—H2S | 0.9700 |
C46—H46 | 0.9300 | ||
B2—Pt7—B3 | 48.5 (3) | B2—B1—B6 | 59.7 (4) |
B2—Pt7—B11 | 46.8 (3) | B3—B1—B6 | 111.1 (5) |
B3—Pt7—B11 | 84.7 (3) | B5—B1—B6 | 59.5 (5) |
B2—Pt7—B8 | 83.5 (3) | B4—B1—H1 | 120.3 |
B3—Pt7—B8 | 46.8 (3) | B2—B1—H1 | 121.8 |
B11—Pt7—B8 | 90.5 (3) | B3—B1—H1 | 120.2 |
B2—Pt7—P2 | 129.56 (19) | B5—B1—H1 | 124.1 |
B3—Pt7—P2 | 93.49 (19) | B6—B1—H1 | 120.2 |
B11—Pt7—P2 | 175.72 (18) | B1—B2—B6 | 60.9 (4) |
B8—Pt7—P2 | 91.10 (18) | B1—B2—B11 | 111.2 (5) |
B2—Pt7—P1 | 118.88 (19) | B6—B2—B11 | 59.8 (4) |
B3—Pt7—P1 | 166.14 (19) | B1—B2—B3 | 59.1 (4) |
B11—Pt7—P1 | 81.51 (19) | B6—B2—B3 | 109.5 (5) |
B8—Pt7—P1 | 134.67 (18) | B11—B2—B3 | 115.2 (5) |
P2—Pt7—P1 | 100.12 (6) | B1—B2—Pt7 | 118.8 (5) |
C31—P1—C11 | 107.8 (3) | B6—B2—Pt7 | 120.4 (5) |
C31—P1—C21 | 100.2 (3) | B11—B2—Pt7 | 69.2 (3) |
C11—P1—C21 | 101.9 (3) | B3—B2—Pt7 | 66.3 (3) |
C31—P1—Pt7 | 113.9 (2) | B1—B2—H2 | 120.1 |
C11—P1—Pt7 | 108.8 (2) | B6—B2—H2 | 120.0 |
C21—P1—Pt7 | 122.9 (2) | B11—B2—H2 | 117.7 |
C41—P2—C51 | 107.1 (3) | B3—B2—H2 | 120.1 |
C41—P2—C61 | 103.0 (3) | Pt7—B2—H2 | 109.5 |
C51—P2—C61 | 101.1 (3) | B1—B3—B4 | 59.5 (4) |
C41—P2—Pt7 | 118.7 (2) | B1—B3—B8 | 109.1 (5) |
C51—P2—Pt7 | 106.7 (2) | B4—B3—B8 | 58.8 (4) |
C61—P2—Pt7 | 118.4 (2) | B1—B3—B2 | 58.6 (4) |
B8—O1—C1 | 122.7 (5) | B4—B3—B2 | 106.2 (5) |
O1—C1—H1A | 109.5 | B8—B3—B2 | 112.1 (5) |
O1—C1—H1B | 109.5 | B1—B3—Pt7 | 117.4 (4) |
H1A—C1—H1B | 109.5 | B4—B3—Pt7 | 118.0 (4) |
O1—C1—H1C | 109.5 | B8—B3—Pt7 | 68.6 (3) |
H1A—C1—H1C | 109.5 | B2—B3—Pt7 | 65.2 (3) |
H1B—C1—H1C | 109.5 | B1—B3—H3 | 120.9 |
C12—C11—C16 | 117.6 (6) | B4—B3—H3 | 121.9 |
C12—C11—P1 | 118.7 (5) | B8—B3—H3 | 119.2 |
C16—C11—P1 | 123.7 (5) | B2—B3—H3 | 122.1 |
C13—C12—C11 | 121.3 (6) | Pt7—B3—H3 | 110.7 |
C13—C12—H12 | 119.3 | B8—B4—B1 | 111.8 (5) |
C11—C12—H12 | 119.3 | B8—B4—B5 | 110.1 (5) |
C14—C13—C12 | 120.1 (7) | B1—B4—B5 | 60.5 (5) |
C14—C13—H13 | 119.9 | B8—B4—B3 | 61.4 (4) |
C12—C13—H13 | 119.9 | B1—B4—B3 | 60.1 (4) |
C13—C14—C15 | 119.5 (7) | B5—B4—B3 | 107.3 (6) |
C13—C14—H14 | 120.2 | B8—B4—B9 | 63.8 (4) |
C15—C14—H14 | 120.2 | B1—B4—B9 | 109.0 (6) |
C16—C15—C14 | 120.3 (7) | B5—B4—B9 | 58.0 (4) |
C16—C15—H15 | 119.8 | B3—B4—B9 | 110.3 (5) |
C14—C15—H15 | 119.8 | B8—B4—H4 | 118.2 |
C15—C16—C11 | 120.8 (7) | B1—B4—H4 | 120.5 |
C15—C16—H16 | 119.6 | B5—B4—H4 | 122.8 |
C11—C16—H16 | 119.6 | B3—B4—H4 | 121.5 |
C26—C21—C22 | 117.9 (6) | B9—B4—H4 | 120.6 |
C26—C21—P1 | 119.0 (5) | B10—B5—B9 | 68.0 (5) |
C22—C21—P1 | 123.0 (5) | B10—B5—B4 | 117.0 (5) |
C23—C22—C21 | 121.5 (7) | B9—B5—B4 | 62.3 (4) |
C23—C22—H22 | 119.3 | B10—B5—B6 | 60.9 (5) |
C21—C22—H22 | 119.3 | B9—B5—B6 | 116.2 (5) |
C24—C23—C22 | 118.8 (8) | B4—B5—B6 | 111.2 (5) |
C24—C23—H23 | 120.6 | B10—B5—B1 | 111.6 (6) |
C22—C23—H23 | 120.6 | B9—B5—B1 | 111.9 (5) |
C23—C24—C25 | 121.1 (8) | B4—B5—B1 | 59.7 (5) |
C23—C24—H24 | 119.4 | B6—B5—B1 | 60.7 (5) |
C25—C24—H24 | 119.4 | B10—B5—H5 | 116.0 |
C24—C25—C26 | 118.9 (8) | B9—B5—H5 | 115.5 |
C24—C25—H25 | 120.5 | B4—B5—H5 | 119.1 |
C26—C25—H25 | 120.5 | B6—B5—H5 | 119.6 |
C25—C26—C21 | 121.7 (7) | B1—B5—H5 | 121.8 |
C25—C26—H26 | 119.1 | B2—B6—B5 | 105.4 (5) |
C21—C26—H26 | 119.1 | B2—B6—B10 | 109.1 (5) |
C36—C31—C32 | 117.6 (6) | B5—B6—B10 | 58.3 (4) |
C36—C31—P1 | 121.5 (5) | B2—B6—B11 | 60.9 (4) |
C32—C31—P1 | 120.8 (5) | B5—B6—B11 | 109.1 (5) |
C33—C32—C31 | 120.5 (7) | B10—B6—B11 | 63.2 (4) |
C33—C32—H32 | 119.7 | B2—B6—B1 | 59.4 (4) |
C31—C32—H32 | 119.7 | B5—B6—B1 | 59.9 (4) |
C34—C33—C32 | 120.7 (8) | B10—B6—B1 | 108.8 (6) |
C34—C33—H33 | 119.6 | B11—B6—B1 | 110.9 (5) |
C32—C33—H33 | 119.6 | B2—B6—H6 | 122.7 |
C33—C34—C35 | 120.4 (7) | B5—B6—H6 | 123.5 |
C33—C34—H34 | 119.8 | B10—B6—H6 | 120.7 |
C35—C34—H34 | 119.8 | B11—B6—H6 | 118.9 |
C34—C35—C36 | 119.7 (8) | B1—B6—H6 | 120.8 |
C34—C35—H35 | 120.2 | O1—B8—B4 | 127.2 (6) |
C36—C35—H35 | 120.2 | O1—B8—B3 | 126.4 (5) |
C31—C36—C35 | 121.1 (7) | B4—B8—B3 | 59.8 (4) |
C31—C36—H36 | 119.5 | O1—B8—B9 | 122.8 (5) |
C35—C36—H36 | 119.5 | B4—B8—B9 | 59.4 (4) |
C42—C41—C46 | 118.3 (6) | B3—B8—B9 | 105.7 (5) |
C42—C41—P2 | 119.2 (5) | O1—B8—Pt7 | 110.9 (4) |
C46—C41—P2 | 122.5 (6) | B4—B8—Pt7 | 115.5 (5) |
C43—C42—C41 | 121.2 (7) | B3—B8—Pt7 | 64.6 (3) |
C43—C42—H42 | 119.4 | B9—B8—Pt7 | 111.5 (4) |
C41—C42—H42 | 119.4 | O1—B8—H1U | 112 (3) |
C42—C43—C44 | 119.5 (8) | B4—B8—H1U | 95 (3) |
C42—C43—H43 | 120.3 | B3—B8—H1U | 120 (3) |
C44—C43—H43 | 120.3 | B9—B8—H1U | 38 (3) |
C45—C44—C43 | 120.6 (8) | Pt7—B8—H1U | 85 (3) |
C45—C44—H44 | 119.7 | B5—B9—B4 | 59.7 (4) |
C43—C44—H44 | 119.7 | B5—B9—B8 | 105.9 (5) |
C46—C45—C44 | 119.5 (8) | B4—B9—B8 | 56.8 (4) |
C46—C45—H45 | 120.3 | B5—B9—B10 | 55.8 (4) |
C44—C45—H45 | 120.3 | B4—B9—B10 | 105.2 (5) |
C45—C46—C41 | 120.9 (8) | B8—B9—B10 | 111.4 (5) |
C45—C46—H46 | 119.5 | B5—B9—H9 | 140.3 |
C41—C46—H46 | 119.5 | B4—B9—H9 | 140.2 |
C56—C51—C52 | 119.3 (7) | B8—B9—H9 | 112.9 |
C56—C51—P2 | 117.4 (6) | B10—B9—H9 | 113.7 |
C52—C51—P2 | 123.3 (7) | B5—B9—H1U | 125 (3) |
C53—C52—C51 | 121.3 (10) | B4—B9—H1U | 103 (3) |
C53—C52—H52 | 119.4 | B8—B9—H1U | 49 (3) |
C51—C52—H52 | 119.4 | B10—B9—H1U | 85 (3) |
C52—C53—C54 | 119.8 (10) | H9—B9—H1U | 88.4 |
C52—C53—H53 | 120.1 | B5—B10—B6 | 60.9 (5) |
C54—C53—H53 | 120.1 | B5—B10—B11 | 107.5 (5) |
C53—C54—C55 | 121.1 (9) | B6—B10—B11 | 58.6 (4) |
C53—C54—H54 | 119.5 | B5—B10—B9 | 56.2 (4) |
C55—C54—H54 | 119.5 | B6—B10—B9 | 106.7 (5) |
C56—C55—C54 | 119.0 (10) | B11—B10—B9 | 110.6 (5) |
C56—C55—H55 | 120.5 | B5—B10—H10 | 139.6 |
C54—C55—H55 | 120.5 | B6—B10—H10 | 138.7 |
C55—C56—C51 | 119.6 (9) | B11—B10—H10 | 112.3 |
C55—C56—H56 | 120.2 | B9—B10—H10 | 113.6 |
C51—C56—H56 | 120.2 | B5—B10—H2U | 128 (2) |
C62—C61—C66 | 117.9 (7) | B6—B10—H2U | 96 (2) |
C62—C61—P2 | 121.6 (6) | B11—B10—H2U | 38 (2) |
C66—C61—P2 | 120.5 (5) | B9—B10—H2U | 95 (2) |
C61—C62—C63 | 119.9 (8) | H10—B10—H2U | 89.9 |
C61—C62—H62 | 120.1 | B6—B11—B2 | 59.3 (4) |
C63—C62—H62 | 120.1 | B6—B11—B10 | 58.2 (4) |
C64—C63—C62 | 120.5 (9) | B2—B11—B10 | 104.1 (5) |
C64—C63—H63 | 119.8 | B6—B11—Pt7 | 115.6 (4) |
C62—C63—H63 | 119.8 | B2—B11—Pt7 | 64.1 (3) |
C65—C64—C63 | 120.1 (8) | B10—B11—Pt7 | 113.2 (4) |
C65—C64—H64 | 120.0 | B6—B11—H11 | 137.0 |
C63—C64—H64 | 120.0 | B2—B11—H11 | 141.0 |
C64—C65—C66 | 120.0 (9) | B10—B11—H11 | 113.9 |
C64—C65—H65 | 120.0 | Pt7—B11—H11 | 106.2 |
C66—C65—H65 | 120.0 | B6—B11—H2U | 103 (3) |
C61—C66—C65 | 121.6 (7) | B2—B11—H2U | 127 (3) |
C61—C66—H66 | 119.2 | B10—B11—H2U | 45 (3) |
C65—C66—H66 | 119.2 | Pt7—B11—H2U | 88 (3) |
B4—B1—B2 | 109.8 (5) | H11—B11—H2U | 88.0 |
B4—B1—B3 | 60.4 (4) | Cl1—C1S—Cl2 | 123.6 (14) |
B2—B1—B3 | 62.3 (4) | Cl1—C1S—H1S | 106.4 |
B4—B1—B5 | 59.8 (5) | Cl2—C1S—H1S | 106.4 |
B2—B1—B5 | 105.3 (6) | Cl1—C1S—H2S | 106.5 |
B3—B1—B5 | 107.0 (5) | Cl2—C1S—H2S | 106.5 |
B4—B1—B6 | 110.3 (6) | H1S—C1S—H2S | 106.5 |
[Pt(C3H18B10O)(C18H15P)2]·CH2Cl2 | F(000) = 1960 |
Mr = 982.83 | Dx = 1.472 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
a = 11.114 (3) Å | Cell parameters from 25 reflections |
b = 21.634 (8) Å | θ = 9–13.2° |
c = 18.990 (8) Å | µ = 3.39 mm−1 |
β = 103.75 (3)° | T = 293 K |
V = 4435 (3) Å3 | Plate, yellow |
Z = 4 | 0.42 × 0.27 × 0.07 mm |
Enraf-Nonius CAD-4 diffractometer | 4066 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.081 |
Graphite monochromator | θmax = 25.1°, θmin = 1.5° |
θ/2θ scans | h = −13→12 |
Absorption correction: ψ scans (North et al., 1968) | k = 0→25 |
Tmin = 0.330, Tmax = 0.797 | l = 0→22 |
8141 measured reflections | 3 standard reflections every 200 reflections |
7894 independent reflections | intensity decay: 5.4% |
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)] = 0.069 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.238 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.38 | w = 1/[σ2(Fo2) + (0.1P)2] where P = (Fo2 + 2Fc2)/3 |
7894 reflections | (Δ/σ)max = 0.001 |
507 parameters | Δρmax = 2.19 e Å−3 |
0 restraints | Δρmin = −3.02 e Å−3 |
[Pt(C3H18B10O)(C18H15P)2]·CH2Cl2 | V = 4435 (3) Å3 |
Mr = 982.83 | Z = 4 |
Monoclinic, P21/n | Mo Kα radiation |
a = 11.114 (3) Å | µ = 3.39 mm−1 |
b = 21.634 (8) Å | T = 293 K |
c = 18.990 (8) Å | 0.42 × 0.27 × 0.07 mm |
β = 103.75 (3)° |
Enraf-Nonius CAD-4 diffractometer | 4066 reflections with I > 2σ(I) |
Absorption correction: ψ scans (North et al., 1968) | Rint = 0.081 |
Tmin = 0.330, Tmax = 0.797 | 3 standard reflections every 200 reflections |
8141 measured reflections | intensity decay: 5.4% |
7894 independent reflections |
R[F2 > 2σ(F2)] = 0.069 | 0 restraints |
wR(F2) = 0.238 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.38 | Δρmax = 2.19 e Å−3 |
7894 reflections | Δρmin = −3.02 e Å−3 |
507 parameters |
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 | ||
Pt7 | 0.94224 (5) | 0.18408 (3) | 0.80843 (3) | 0.0411 (2) | |
P1 | 0.8422 (4) | 0.25483 (19) | 0.8715 (2) | 0.0430 (9) | |
P2 | 1.1265 (4) | 0.2400 (2) | 0.8119 (2) | 0.0454 (9) | |
C1S | 0.646 (4) | 0.4630 (12) | 1.0861 (17) | 0.174 (17) | |
H1S1 | 0.5485 | 0.4492 | 1.0782 | 0.209* | |
H1S2 | 0.6975 | 0.4416 | 1.1370 | 0.209* | |
Cl1 | 0.7014 (14) | 0.4321 (6) | 1.0158 (7) | 0.236 (6) | |
Cl2 | 0.6532 (15) | 0.5307 (6) | 1.0957 (10) | 0.279 (8) | |
C11 | 0.9236 (14) | 0.3199 (7) | 0.9208 (8) | 0.051 (4) | |
C12 | 0.9385 (15) | 0.3748 (7) | 0.8838 (10) | 0.057 (4) | |
H12 | 0.9060 | 0.3762 | 0.8340 | 0.069* | |
C13 | 0.997 (2) | 0.4247 (11) | 0.9161 (14) | 0.097 (8) | |
H13 | 0.9957 | 0.4616 | 0.8910 | 0.116* | |
C14 | 1.058 (2) | 0.4198 (11) | 0.9887 (17) | 0.109 (10) | |
H14 | 1.1069 | 0.4529 | 1.0103 | 0.130* | |
C15 | 1.0510 (16) | 0.3653 (11) | 1.0324 (11) | 0.079 (6) | |
H15 | 1.0903 | 0.3626 | 1.0814 | 0.094* | |
C16 | 0.9808 (14) | 0.3184 (8) | 0.9952 (8) | 0.056 (4) | |
H16 | 0.9702 | 0.2830 | 1.0209 | 0.067* | |
C21 | 0.7894 (13) | 0.2092 (9) | 0.9390 (8) | 0.053 (4) | |
C22 | 0.8729 (14) | 0.1699 (8) | 0.9851 (9) | 0.059 (5) | |
H22 | 0.9552 | 0.1699 | 0.9819 | 0.071* | |
C23 | 0.8391 (17) | 0.1307 (9) | 1.0355 (9) | 0.069 (5) | |
H23 | 0.8932 | 0.1017 | 1.0620 | 0.083* | |
C24 | 0.7185 (19) | 0.1382 (8) | 1.0434 (9) | 0.061 (5) | |
H24 | 0.6941 | 0.1144 | 1.0784 | 0.074* | |
C25 | 0.635 (2) | 0.1772 (11) | 1.0041 (15) | 0.106 (10) | |
H25 | 0.5564 | 0.1813 | 1.0126 | 0.127* | |
C26 | 0.6714 (18) | 0.2122 (9) | 0.9486 (11) | 0.069 (5) | |
H26 | 0.6136 | 0.2375 | 0.9185 | 0.083* | |
C31 | 0.7043 (13) | 0.2914 (7) | 0.8160 (8) | 0.044 (4) | |
C32 | 0.6571 (16) | 0.2767 (9) | 0.7432 (10) | 0.070 (5) | |
H32 | 0.6944 | 0.2461 | 0.7213 | 0.084* | |
C33 | 0.5536 (17) | 0.3082 (9) | 0.7035 (10) | 0.077 (6) | |
H33 | 0.5258 | 0.2997 | 0.6543 | 0.092* | |
C34 | 0.4908 (18) | 0.3518 (9) | 0.7346 (12) | 0.078 (6) | |
H34 | 0.4161 | 0.3685 | 0.7090 | 0.093* | |
C35 | 0.5410 (18) | 0.3683 (8) | 0.8015 (11) | 0.071 (5) | |
H35 | 0.5045 | 0.4010 | 0.8207 | 0.085* | |
C36 | 0.6479 (15) | 0.3400 (8) | 0.8473 (10) | 0.063 (5) | |
H36 | 0.6788 | 0.3526 | 0.8950 | 0.075* | |
C41 | 1.2332 (14) | 0.2579 (8) | 0.8983 (8) | 0.052 (4) | |
C42 | 1.3487 (14) | 0.2859 (9) | 0.9028 (8) | 0.063 (5) | |
H42 | 1.3779 | 0.2910 | 0.8611 | 0.075* | |
C43 | 1.4201 (17) | 0.3062 (9) | 0.9697 (11) | 0.073 (6) | |
H43 | 1.4906 | 0.3301 | 0.9725 | 0.088* | |
C44 | 1.3814 (19) | 0.2891 (9) | 1.0335 (10) | 0.075 (6) | |
H44 | 1.4253 | 0.3036 | 1.0784 | 0.090* | |
C45 | 1.2811 (15) | 0.2518 (11) | 1.0296 (9) | 0.077 (6) | |
H45 | 1.2650 | 0.2354 | 1.0717 | 0.093* | |
C46 | 1.2030 (15) | 0.2383 (9) | 0.9626 (9) | 0.066 (5) | |
H46 | 1.1304 | 0.2162 | 0.9602 | 0.080* | |
C51 | 1.2261 (17) | 0.2088 (9) | 0.7569 (11) | 0.070 (5) | |
C52 | 1.2156 (17) | 0.2249 (9) | 0.6870 (9) | 0.064 (5) | |
H52 | 1.1575 | 0.2549 | 0.6673 | 0.077* | |
C53 | 1.285 (3) | 0.1999 (14) | 0.6430 (12) | 0.119 (10) | |
H53 | 1.2719 | 0.2091 | 0.5939 | 0.143* | |
C54 | 1.380 (3) | 0.1583 (12) | 0.6804 (16) | 0.106 (8) | |
H54 | 1.4308 | 0.1403 | 0.6539 | 0.127* | |
C55 | 1.3987 (19) | 0.1439 (11) | 0.7501 (13) | 0.089 (7) | |
H55 | 1.4605 | 0.1159 | 0.7708 | 0.107* | |
C56 | 1.3251 (16) | 0.1710 (8) | 0.7922 (10) | 0.065 (5) | |
H56 | 1.3412 | 0.1643 | 0.8419 | 0.078* | |
C61 | 1.0802 (13) | 0.3109 (8) | 0.7662 (7) | 0.048 (4) | |
C62 | 1.1417 (18) | 0.3676 (11) | 0.7779 (12) | 0.089 (7) | |
H62 | 1.2144 | 0.3695 | 0.8142 | 0.107* | |
C63 | 1.104 (2) | 0.4192 (10) | 0.7410 (12) | 0.094 (7) | |
H63 | 1.1508 | 0.4552 | 0.7504 | 0.113* | |
C64 | 0.995 (3) | 0.4183 (12) | 0.6887 (12) | 0.107 (8) | |
H64 | 0.9718 | 0.4534 | 0.6605 | 0.128* | |
C65 | 0.920 (2) | 0.3694 (13) | 0.6768 (13) | 0.101 (8) | |
H65 | 0.8419 | 0.3713 | 0.6455 | 0.121* | |
C66 | 0.9646 (18) | 0.3153 (9) | 0.7133 (11) | 0.076 (6) | |
H66 | 0.9165 | 0.2798 | 0.7027 | 0.092* | |
B1 | 0.867 (2) | 0.0549 (13) | 0.7068 (16) | 0.093 (9) | |
H1 | 0.8565 | 0.0364 | 0.6517 | 0.112* | |
B2 | 0.8220 (19) | 0.1309 (10) | 0.7169 (9) | 0.060 (5) | |
H2 | 0.7855 | 0.1610 | 0.6700 | 0.072* | |
B3 | 0.9944 (18) | 0.1100 (10) | 0.7439 (12) | 0.069 (6) | |
H3 | 1.0628 | 0.1276 | 0.7154 | 0.082* | |
B4 | 0.994 (2) | 0.0284 (11) | 0.7733 (13) | 0.075 (7) | |
H4 | 1.0580 | −0.0064 | 0.7613 | 0.090* | |
B5 | 0.8409 (17) | 0.0082 (10) | 0.7744 (13) | 0.068 (6) | |
H5 | 0.8130 | −0.0406 | 0.7674 | 0.081* | |
B6 | 0.7301 (18) | 0.0702 (10) | 0.7331 (9) | 0.062 (6) | |
H6 | 0.6370 | 0.0624 | 0.6984 | 0.074* | |
B8 | 1.0450 (19) | 0.0912 (7) | 0.8356 (11) | 0.056 (5) | |
B9 | 0.950 (2) | 0.0303 (12) | 0.8594 (18) | 0.093 (9) | |
H9 | 0.9833 | 0.0151 | 0.9159 | 0.112* | |
B10 | 0.775 (2) | 0.0541 (11) | 0.8289 (12) | 0.072 (6) | |
H10 | 0.7285 | 0.0473 | 0.8735 | 0.087* | |
B11 | 0.7545 (17) | 0.1324 (10) | 0.7944 (10) | 0.060 (6) | |
H11 | 0.6965 | 0.1612 | 0.8210 | 0.072* | |
H1U | 0.965 (13) | 0.088 (6) | 0.876 (7) | 0.05 (4)* | |
H2U | 0.83 (3) | 0.091 (15) | 0.875 (17) | 0.22 (14)* | |
O1 | 1.1626 (10) | 0.0994 (6) | 0.8792 (7) | 0.075 (4) | |
C1 | 1.222 (2) | 0.0542 (9) | 0.9286 (13) | 0.092 (7) | |
H1A | 1.1781 | 0.0093 | 0.9120 | 0.110* | |
C2 | 1.359 (3) | 0.0482 (14) | 0.933 (2) | 0.182 (16) | |
H2A | 1.3808 | 0.0688 | 0.8845 | 0.219* | |
H2B | 1.3854 | −0.0009 | 0.9365 | 0.219* | |
H2C | 1.4120 | 0.0725 | 0.9816 | 0.219* | |
C3 | 1.203 (3) | 0.0700 (14) | 1.0026 (15) | 0.167 (15) | |
H3A | 1.2629 | 0.1092 | 1.0253 | 0.201* | |
H3B | 1.2267 | 0.0297 | 1.0385 | 0.201* | |
H3C | 1.1056 | 0.0827 | 0.9978 | 0.201* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Pt7 | 0.0344 (3) | 0.0528 (4) | 0.0365 (3) | 0.0006 (3) | 0.0093 (2) | −0.0030 (3) |
P1 | 0.036 (2) | 0.053 (2) | 0.040 (2) | −0.0005 (17) | 0.0087 (16) | −0.0039 (18) |
P2 | 0.038 (2) | 0.061 (3) | 0.040 (2) | −0.0033 (18) | 0.0133 (17) | −0.0033 (18) |
C1S | 0.33 (5) | 0.083 (19) | 0.16 (3) | 0.09 (3) | 0.16 (3) | 0.057 (19) |
Cl1 | 0.315 (17) | 0.222 (12) | 0.200 (11) | −0.009 (12) | 0.119 (11) | −0.081 (10) |
Cl2 | 0.281 (16) | 0.181 (12) | 0.42 (2) | −0.024 (11) | 0.178 (16) | −0.140 (14) |
C11 | 0.049 (9) | 0.052 (9) | 0.054 (9) | 0.017 (8) | 0.014 (7) | −0.019 (8) |
C12 | 0.063 (11) | 0.034 (9) | 0.084 (12) | −0.001 (8) | 0.034 (9) | 0.001 (8) |
C13 | 0.099 (18) | 0.091 (17) | 0.103 (18) | −0.047 (14) | 0.030 (14) | −0.032 (14) |
C14 | 0.093 (18) | 0.089 (18) | 0.17 (3) | −0.039 (14) | 0.085 (19) | −0.068 (18) |
C15 | 0.042 (10) | 0.117 (18) | 0.070 (13) | 0.007 (11) | −0.001 (9) | −0.034 (13) |
C16 | 0.043 (8) | 0.080 (12) | 0.049 (9) | −0.022 (9) | 0.022 (7) | −0.003 (9) |
C21 | 0.032 (8) | 0.084 (12) | 0.045 (9) | −0.003 (8) | 0.011 (7) | −0.015 (8) |
C22 | 0.037 (8) | 0.082 (13) | 0.059 (10) | 0.006 (8) | 0.014 (7) | 0.026 (9) |
C23 | 0.063 (12) | 0.084 (14) | 0.055 (10) | −0.022 (10) | 0.000 (9) | 0.010 (10) |
C24 | 0.078 (13) | 0.054 (11) | 0.050 (10) | −0.004 (10) | 0.010 (9) | 0.009 (8) |
C25 | 0.090 (17) | 0.108 (19) | 0.15 (2) | −0.053 (15) | 0.093 (18) | −0.048 (18) |
C26 | 0.066 (12) | 0.059 (11) | 0.088 (14) | 0.008 (9) | 0.032 (11) | 0.002 (10) |
C31 | 0.036 (8) | 0.056 (9) | 0.044 (8) | 0.012 (7) | 0.018 (7) | −0.006 (7) |
C32 | 0.053 (11) | 0.083 (14) | 0.068 (12) | −0.007 (10) | 0.003 (9) | −0.011 (10) |
C33 | 0.071 (13) | 0.087 (15) | 0.060 (12) | 0.026 (11) | −0.007 (10) | 0.005 (10) |
C34 | 0.066 (13) | 0.072 (13) | 0.085 (14) | 0.024 (11) | −0.001 (11) | −0.003 (11) |
C35 | 0.073 (13) | 0.052 (11) | 0.094 (15) | 0.006 (10) | 0.034 (11) | 0.013 (10) |
C36 | 0.053 (10) | 0.064 (11) | 0.078 (12) | 0.001 (8) | 0.027 (9) | 0.038 (9) |
C41 | 0.040 (8) | 0.081 (12) | 0.046 (9) | −0.001 (8) | 0.027 (7) | −0.020 (8) |
C42 | 0.032 (8) | 0.117 (15) | 0.038 (8) | −0.010 (9) | 0.006 (7) | 0.004 (9) |
C43 | 0.053 (10) | 0.091 (15) | 0.076 (13) | −0.029 (10) | 0.015 (9) | −0.022 (11) |
C44 | 0.078 (14) | 0.076 (13) | 0.056 (11) | 0.020 (11) | −0.016 (10) | −0.025 (10) |
C45 | 0.039 (10) | 0.14 (2) | 0.045 (10) | −0.014 (11) | −0.004 (8) | −0.003 (11) |
C46 | 0.041 (9) | 0.103 (15) | 0.050 (10) | 0.005 (9) | 0.001 (8) | −0.028 (10) |
C51 | 0.055 (11) | 0.073 (12) | 0.088 (14) | −0.001 (9) | 0.029 (10) | 0.031 (11) |
C52 | 0.066 (12) | 0.087 (14) | 0.041 (9) | 0.002 (10) | 0.019 (8) | 0.006 (9) |
C53 | 0.14 (2) | 0.18 (3) | 0.054 (13) | 0.03 (2) | 0.047 (15) | 0.006 (15) |
C54 | 0.12 (2) | 0.111 (19) | 0.11 (2) | −0.004 (16) | 0.074 (18) | −0.040 (17) |
C55 | 0.073 (14) | 0.111 (18) | 0.094 (16) | 0.035 (13) | 0.041 (12) | −0.016 (14) |
C56 | 0.056 (11) | 0.070 (13) | 0.070 (11) | 0.000 (9) | 0.017 (9) | −0.020 (9) |
C61 | 0.033 (7) | 0.075 (11) | 0.034 (7) | 0.014 (8) | 0.007 (6) | 0.001 (8) |
C62 | 0.052 (11) | 0.095 (16) | 0.109 (17) | 0.014 (11) | −0.003 (11) | 0.048 (14) |
C63 | 0.106 (18) | 0.069 (14) | 0.090 (16) | −0.011 (13) | −0.009 (13) | 0.015 (12) |
C64 | 0.13 (2) | 0.091 (18) | 0.087 (17) | 0.010 (17) | 0.001 (16) | 0.034 (14) |
C65 | 0.081 (16) | 0.13 (2) | 0.086 (16) | −0.007 (16) | 0.008 (13) | 0.017 (16) |
C66 | 0.074 (13) | 0.073 (13) | 0.086 (14) | 0.028 (11) | 0.025 (11) | 0.033 (11) |
B1 | 0.061 (14) | 0.11 (2) | 0.11 (2) | 0.000 (14) | 0.019 (14) | −0.049 (18) |
B2 | 0.062 (12) | 0.086 (15) | 0.032 (9) | 0.013 (11) | 0.010 (8) | 0.000 (9) |
B3 | 0.047 (11) | 0.068 (13) | 0.098 (16) | 0.016 (10) | 0.031 (11) | −0.048 (12) |
B4 | 0.061 (13) | 0.072 (15) | 0.096 (17) | −0.008 (12) | 0.024 (12) | −0.035 (13) |
B5 | 0.038 (10) | 0.051 (12) | 0.112 (18) | −0.012 (9) | 0.015 (11) | −0.014 (12) |
B6 | 0.051 (12) | 0.084 (15) | 0.040 (10) | −0.005 (11) | −0.008 (9) | −0.031 (10) |
B8 | 0.067 (13) | 0.012 (7) | 0.074 (13) | 0.004 (8) | −0.014 (10) | 0.013 (8) |
B9 | 0.046 (13) | 0.087 (19) | 0.14 (2) | −0.007 (12) | 0.011 (14) | 0.038 (18) |
B10 | 0.070 (15) | 0.072 (15) | 0.072 (14) | −0.001 (12) | 0.015 (12) | −0.007 (12) |
B11 | 0.045 (10) | 0.080 (15) | 0.058 (11) | −0.039 (10) | 0.022 (9) | −0.017 (10) |
O1 | 0.044 (7) | 0.076 (9) | 0.105 (10) | 0.021 (6) | 0.020 (7) | 0.034 (8) |
C1 | 0.097 (17) | 0.048 (12) | 0.111 (18) | −0.013 (11) | −0.013 (14) | 0.017 (12) |
C2 | 0.11 (2) | 0.14 (3) | 0.27 (4) | 0.09 (2) | 0.00 (3) | 0.08 (3) |
C3 | 0.24 (4) | 0.15 (3) | 0.10 (2) | 0.08 (3) | 0.02 (2) | 0.09 (2) |
Pt7—B3 | 2.178 (16) | C51—C52 | 1.35 (2) |
Pt7—B2 | 2.24 (2) | C51—C56 | 1.41 (2) |
Pt7—B8 | 2.308 (16) | C52—C53 | 1.37 (3) |
Pt7—B11 | 2.326 (16) | C53—C54 | 1.44 (4) |
Pt7—P2 | 2.366 (4) | C54—C55 | 1.33 (3) |
Pt7—P1 | 2.376 (4) | C55—C56 | 1.40 (2) |
P1—C11 | 1.810 (16) | C61—C62 | 1.40 (3) |
P1—C31 | 1.821 (15) | C61—C66 | 1.43 (2) |
P1—C21 | 1.821 (17) | C62—C63 | 1.33 (3) |
P2—C61 | 1.776 (17) | C63—C64 | 1.37 (3) |
P2—C41 | 1.823 (16) | C64—C65 | 1.33 (3) |
P2—C51 | 1.822 (19) | C65—C66 | 1.39 (3) |
C1S—Cl2 | 1.48 (3) | B1—B5 | 1.71 (4) |
C1S—Cl1 | 1.73 (3) | B1—B6 | 1.74 (3) |
C11—C16 | 1.40 (2) | B1—B2 | 1.74 (3) |
C11—C12 | 1.41 (2) | B1—B4 | 1.75 (4) |
C12—C13 | 1.33 (2) | B1—B3 | 1.86 (3) |
C13—C14 | 1.39 (3) | B2—B6 | 1.74 (3) |
C14—C15 | 1.46 (3) | B2—B11 | 1.80 (3) |
C15—C16 | 1.37 (2) | B2—B3 | 1.92 (3) |
C21—C26 | 1.37 (2) | B3—B8 | 1.75 (3) |
C21—C22 | 1.40 (2) | B3—B4 | 1.85 (3) |
C22—C23 | 1.40 (2) | B4—B5 | 1.76 (3) |
C23—C24 | 1.39 (3) | B4—B8 | 1.80 (3) |
C24—C25 | 1.34 (3) | B4—B9 | 1.81 (4) |
C25—C26 | 1.43 (3) | B5—B10 | 1.72 (3) |
C31—C32 | 1.39 (2) | B5—B9 | 1.84 (4) |
C31—C36 | 1.42 (2) | B5—B6 | 1.86 (3) |
C32—C33 | 1.39 (2) | B6—B11 | 1.76 (3) |
C33—C34 | 1.38 (3) | B6—B10 | 1.80 (3) |
C34—C35 | 1.31 (3) | B8—O1 | 1.38 (2) |
C35—C36 | 1.43 (2) | B8—B9 | 1.81 (3) |
C41—C42 | 1.40 (2) | B9—B10 | 1.96 (3) |
C41—C46 | 1.41 (2) | B10—B11 | 1.81 (3) |
C42—C43 | 1.40 (2) | O1—C1 | 1.41 (2) |
C43—C44 | 1.43 (3) | C1—C2 | 1.51 (3) |
C44—C45 | 1.37 (3) | C1—C3 | 1.51 (3) |
C45—C46 | 1.39 (2) | ||
B3—Pt7—B2 | 51.4 (7) | B2—B1—B3 | 64.2 (13) |
B3—Pt7—B8 | 45.7 (8) | B4—B1—B3 | 61.7 (13) |
B2—Pt7—B8 | 84.2 (7) | B6—B2—B1 | 60.0 (13) |
B3—Pt7—B11 | 86.2 (8) | B6—B2—B11 | 59.5 (10) |
B2—Pt7—B11 | 46.5 (7) | B1—B2—B11 | 106.9 (16) |
B8—Pt7—B11 | 89.4 (8) | B6—B2—B3 | 111.6 (15) |
B3—Pt7—P2 | 92.7 (6) | B1—B2—B3 | 60.9 (12) |
B2—Pt7—P2 | 129.5 (5) | B11—B2—B3 | 111.7 (13) |
B8—Pt7—P2 | 93.5 (5) | B6—B2—Pt7 | 121.2 (11) |
B11—Pt7—P2 | 174.8 (5) | B1—B2—Pt7 | 115.9 (13) |
B3—Pt7—P1 | 167.6 (5) | B11—B2—Pt7 | 69.2 (8) |
B2—Pt7—P1 | 117.2 (5) | B3—B2—Pt7 | 62.6 (8) |
B8—Pt7—P1 | 135.6 (6) | B8—B3—B4 | 60.0 (12) |
B11—Pt7—P1 | 81.5 (6) | B8—B3—B1 | 105.3 (17) |
P2—Pt7—P1 | 99.33 (14) | B4—B3—B1 | 56.3 (13) |
C11—P1—C31 | 102.1 (7) | B8—B3—B2 | 112.7 (14) |
C11—P1—C21 | 105.2 (7) | B4—B3—B2 | 103.3 (15) |
C31—P1—C21 | 105.9 (7) | B1—B3—B2 | 54.9 (12) |
C11—P1—Pt7 | 121.7 (5) | B8—B3—Pt7 | 71.1 (9) |
C31—P1—Pt7 | 114.8 (5) | B4—B3—Pt7 | 120.7 (14) |
C21—P1—Pt7 | 105.9 (6) | B1—B3—Pt7 | 113.8 (12) |
C61—P2—C41 | 107.9 (8) | B2—B3—Pt7 | 66.0 (8) |
C61—P2—C51 | 100.6 (7) | B1—B4—B5 | 58.3 (14) |
C41—P2—C51 | 103.9 (8) | B1—B4—B8 | 107.6 (16) |
C61—P2—Pt7 | 106.3 (5) | B5—B4—B8 | 109.6 (15) |
C41—P2—Pt7 | 120.5 (5) | B1—B4—B9 | 107.5 (17) |
C51—P2—Pt7 | 115.7 (6) | B5—B4—B9 | 61.9 (13) |
Cl2—C1S—Cl1 | 117.3 (18) | B8—B4—B9 | 60.1 (12) |
C16—C11—C12 | 116.3 (15) | B1—B4—B3 | 62.1 (14) |
C16—C11—P1 | 123.6 (13) | B5—B4—B3 | 108.3 (16) |
C12—C11—P1 | 120.0 (13) | B8—B4—B3 | 57.1 (11) |
C13—C12—C11 | 123.7 (19) | B9—B4—B3 | 105.8 (14) |
C12—C13—C14 | 118 (2) | B1—B5—B10 | 106.5 (17) |
C13—C14—C15 | 123 (2) | B1—B5—B4 | 60.7 (14) |
C16—C15—C14 | 114.1 (19) | B10—B5—B4 | 114.6 (15) |
C15—C16—C11 | 124.6 (18) | B1—B5—B9 | 108.3 (15) |
C26—C21—C22 | 117.3 (16) | B10—B5—B9 | 66.9 (14) |
C26—C21—P1 | 123.2 (14) | B4—B5—B9 | 60.6 (13) |
C22—C21—P1 | 119.5 (11) | B1—B5—B6 | 58.1 (13) |
C23—C22—C21 | 123.4 (16) | B10—B5—B6 | 60.3 (11) |
C22—C23—C24 | 115.3 (17) | B4—B5—B6 | 111.1 (16) |
C25—C24—C23 | 124.7 (18) | B9—B5—B6 | 114.5 (15) |
C24—C25—C26 | 117.6 (18) | B2—B6—B1 | 60.2 (13) |
C21—C26—C25 | 121 (2) | B2—B6—B11 | 62.2 (11) |
C32—C31—C36 | 118.9 (15) | B1—B6—B11 | 109.2 (15) |
C32—C31—P1 | 122.7 (12) | B2—B6—B10 | 107.0 (13) |
C36—C31—P1 | 118.2 (12) | B1—B6—B10 | 101.7 (16) |
C31—C32—C33 | 119.5 (18) | B11—B6—B10 | 61.2 (11) |
C34—C33—C32 | 122.4 (18) | B2—B6—B5 | 105.1 (13) |
C35—C34—C33 | 117.2 (18) | B1—B6—B5 | 56.5 (14) |
C34—C35—C36 | 124.9 (19) | B11—B6—B5 | 106.9 (13) |
C31—C36—C35 | 116.5 (18) | B10—B6—B5 | 56.0 (12) |
C42—C41—C46 | 118.8 (15) | O1—B8—B3 | 126.9 (17) |
C42—C41—P2 | 122.4 (11) | O1—B8—B4 | 126.6 (16) |
C46—C41—P2 | 118.6 (12) | B3—B8—B4 | 62.9 (12) |
C43—C42—C41 | 120.2 (15) | O1—B8—B9 | 118.0 (15) |
C42—C43—C44 | 118.0 (16) | B3—B8—B9 | 110.5 (15) |
C45—C44—C43 | 121.0 (16) | B4—B8—B9 | 60.2 (14) |
C44—C45—C46 | 119.8 (18) | O1—B8—Pt7 | 111.7 (11) |
C45—C46—C41 | 120.4 (17) | B3—B8—Pt7 | 63.2 (7) |
C52—C51—C56 | 119.5 (18) | B4—B8—Pt7 | 116.5 (12) |
C52—C51—P2 | 123.1 (15) | B9—B8—Pt7 | 113.7 (13) |
C56—C51—P2 | 117.1 (14) | B8—B9—B4 | 59.7 (12) |
C51—C52—C53 | 125 (2) | B8—B9—B5 | 105.8 (18) |
C52—C53—C54 | 113 (2) | B4—B9—B5 | 57.6 (14) |
C55—C54—C53 | 124 (2) | B8—B9—B10 | 109.4 (15) |
C54—C55—C56 | 120 (2) | B4—B9—B10 | 101.5 (17) |
C55—C56—C51 | 117.9 (19) | B5—B9—B10 | 53.7 (11) |
C62—C61—C66 | 112.1 (16) | B5—B10—B6 | 63.8 (13) |
C62—C61—P2 | 127.4 (12) | B5—B10—B11 | 110.8 (17) |
C66—C61—P2 | 120.4 (14) | B6—B10—B11 | 58.2 (11) |
C63—C62—C61 | 124.9 (19) | B5—B10—B9 | 59.3 (14) |
C62—C63—C64 | 119 (2) | B6—B10—B9 | 111.3 (16) |
C65—C64—C63 | 123 (2) | B11—B10—B9 | 112.4 (15) |
C64—C65—C66 | 117 (2) | B6—B11—B2 | 58.3 (12) |
C65—C66—C61 | 124 (2) | B6—B11—B10 | 60.6 (12) |
B5—B1—B6 | 65.4 (14) | B2—B11—B10 | 103.8 (15) |
B5—B1—B2 | 111.9 (17) | B6—B11—Pt7 | 115.9 (12) |
B6—B1—B2 | 59.8 (13) | B2—B11—Pt7 | 64.3 (8) |
B5—B1—B4 | 61.0 (15) | B10—B11—Pt7 | 112.2 (13) |
B6—B1—B4 | 118 (2) | B8—O1—C1 | 122.5 (14) |
B2—B1—B4 | 115.6 (17) | O1—C1—C2 | 114 (2) |
B5—B1—B3 | 110.1 (18) | O1—C1—C3 | 108.4 (19) |
B6—B1—B3 | 114.2 (16) | C2—C1—C3 | 109 (2) |
[Pt(C3H18B10O)(C18H15P)2]·CH2Cl2 | F(000) = 1960 |
Mr = 982.83 | Dx = 1.459 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71069 Å |
a = 13.435 (3) Å | Cell parameters from 22 reflections |
b = 17.864 (4) Å | θ = 9.1–10.8° |
c = 19.383 (4) Å | µ = 3.36 mm−1 |
β = 105.94 (2)° | T = 293 K |
V = 4473.1 (17) Å3 | Square prism, red |
Z = 4 | 0.44 × 0.34 × 0.32 mm |
Rigaku AFC-7R diffractometer | 6198 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.048 |
Graphite monochromator | θmax = 25°, θmin = 2.3° |
θ/2θ scans | h = 0→15 |
Absorption correction: ψ scans (North et al., 1968) | k = 0→21 |
Tmin = 0.320, Tmax = 0.413 | l = −23→22 |
8222 measured reflections | 3 standard reflections every 200 reflections |
7865 independent reflections | intensity decay: 0.3% |
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)] = 0.035 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.096 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.03 | w = 1/[σ2(Fo2) + (0.0575P)2 + 0.5166P] where P = (Fo2 + 2Fc2)/3 |
7865 reflections | (Δ/σ)max = 0.002 |
549 parameters | Δρmax = 2.30 e Å−3 |
0 restraints | Δρmin = −0.99 e Å−3 |
[Pt(C3H18B10O)(C18H15P)2]·CH2Cl2 | V = 4473.1 (17) Å3 |
Mr = 982.83 | Z = 4 |
Monoclinic, P21/n | Mo Kα radiation |
a = 13.435 (3) Å | µ = 3.36 mm−1 |
b = 17.864 (4) Å | T = 293 K |
c = 19.383 (4) Å | 0.44 × 0.34 × 0.32 mm |
β = 105.94 (2)° |
Rigaku AFC-7R diffractometer | 6198 reflections with I > 2σ(I) |
Absorption correction: ψ scans (North et al., 1968) | Rint = 0.048 |
Tmin = 0.320, Tmax = 0.413 | 3 standard reflections every 200 reflections |
8222 measured reflections | intensity decay: 0.3% |
7865 independent reflections |
R[F2 > 2σ(F2)] = 0.035 | 0 restraints |
wR(F2) = 0.096 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.03 | Δρmax = 2.30 e Å−3 |
7865 reflections | Δρmin = −0.99 e Å−3 |
549 parameters |
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 | ||
Pt7 | 0.201146 (14) | 0.819610 (10) | 0.119982 (10) | 0.02727 (8) | |
P1 | 0.19465 (10) | 0.73495 (7) | 0.02513 (7) | 0.0310 (3) | |
P2 | 0.35817 (10) | 0.87605 (7) | 0.12119 (7) | 0.0303 (3) | |
O1 | −0.1650 (3) | 0.8291 (2) | 0.0655 (2) | 0.0497 (11) | |
C1 | −0.1979 (5) | 0.7704 (3) | 0.0141 (3) | 0.0497 (15) | |
H1F | −0.1408 | 0.7568 | −0.0059 | 0.060* | |
C2 | −0.2870 (6) | 0.8008 (5) | −0.0450 (4) | 0.075 (2) | |
H2A | −0.2641 | 0.8436 | −0.0665 | 0.112* | |
H2B | −0.3424 | 0.8153 | −0.0253 | 0.112* | |
H2C | −0.3111 | 0.7629 | −0.0808 | 0.112* | |
C3 | −0.2298 (6) | 0.7022 (4) | 0.0496 (5) | 0.076 (2) | |
H3A | −0.1715 | 0.6844 | 0.0867 | 0.114* | |
H3B | −0.2532 | 0.6636 | 0.0145 | 0.114* | |
H3C | −0.2847 | 0.7156 | 0.0702 | 0.114* | |
C11 | 0.2903 (4) | 0.7349 (3) | −0.0265 (3) | 0.0350 (11) | |
C12 | 0.3851 (4) | 0.6994 (3) | 0.0026 (3) | 0.0450 (14) | |
H12 | 0.3998 | 0.6786 | 0.0482 | 0.054* | |
C13 | 0.4571 (5) | 0.6951 (4) | −0.0362 (4) | 0.0598 (18) | |
H13 | 0.5203 | 0.6716 | −0.0165 | 0.072* | |
C14 | 0.4359 (5) | 0.7252 (5) | −0.1035 (4) | 0.066 (2) | |
H14 | 0.4847 | 0.7223 | −0.1294 | 0.079* | |
C15 | 0.3430 (5) | 0.7598 (4) | −0.1329 (3) | 0.0595 (17) | |
H15 | 0.3288 | 0.7802 | −0.1787 | 0.071* | |
C16 | 0.2699 (5) | 0.7646 (4) | −0.0946 (3) | 0.0482 (14) | |
H16 | 0.2067 | 0.7879 | −0.1150 | 0.058* | |
C21 | 0.0730 (4) | 0.7540 (3) | −0.0436 (3) | 0.0347 (11) | |
C22 | 0.0041 (5) | 0.6991 (3) | −0.0763 (3) | 0.0471 (15) | |
H22 | 0.0176 | 0.6492 | −0.0631 | 0.057* | |
C23 | −0.0861 (5) | 0.7180 (4) | −0.1295 (4) | 0.0608 (19) | |
H23 | −0.1321 | 0.6807 | −0.1517 | 0.073* | |
C24 | −0.1070 (5) | 0.7915 (5) | −0.1490 (3) | 0.0596 (18) | |
H24 | −0.1669 | 0.8040 | −0.1843 | 0.072* | |
C25 | −0.0389 (5) | 0.8462 (4) | −0.1159 (3) | 0.0545 (16) | |
H25 | −0.0533 | 0.8961 | −0.1285 | 0.065* | |
C26 | 0.0509 (4) | 0.8277 (3) | −0.0641 (3) | 0.0425 (13) | |
H26 | 0.0970 | 0.8652 | −0.0426 | 0.051* | |
C31 | 0.1982 (4) | 0.6356 (3) | 0.0475 (3) | 0.0401 (13) | |
C32 | 0.2066 (4) | 0.6118 (3) | 0.1176 (3) | 0.0452 (14) | |
H32 | 0.2046 | 0.6469 | 0.1527 | 0.054* | |
C33 | 0.2178 (5) | 0.5363 (4) | 0.1353 (4) | 0.066 (2) | |
H33 | 0.2245 | 0.5209 | 0.1822 | 0.079* | |
C34 | 0.2190 (7) | 0.4844 (4) | 0.0830 (5) | 0.083 (3) | |
H34 | 0.2258 | 0.4338 | 0.0946 | 0.100* | |
C35 | 0.2101 (7) | 0.5073 (4) | 0.0132 (5) | 0.078 (2) | |
H35 | 0.2105 | 0.4719 | −0.0219 | 0.093* | |
C36 | 0.2006 (5) | 0.5825 (3) | −0.0043 (4) | 0.0573 (17) | |
H36 | 0.1957 | 0.5975 | −0.0511 | 0.069* | |
C41 | 0.4049 (4) | 0.9536 (3) | 0.1838 (3) | 0.0337 (11) | |
C42 | 0.4613 (4) | 0.9378 (3) | 0.2541 (3) | 0.0476 (14) | |
H42 | 0.4744 | 0.8884 | 0.2689 | 0.057* | |
C43 | 0.4978 (5) | 0.9961 (4) | 0.3019 (4) | 0.0593 (18) | |
H43 | 0.5348 | 0.9853 | 0.3488 | 0.071* | |
C44 | 0.4800 (5) | 1.0693 (4) | 0.2808 (4) | 0.0579 (17) | |
H44 | 0.5055 | 1.1077 | 0.3132 | 0.069* | |
C45 | 0.4251 (5) | 1.0853 (3) | 0.2126 (4) | 0.0529 (16) | |
H45 | 0.4137 | 1.1350 | 0.1984 | 0.064* | |
C46 | 0.3853 (4) | 1.0282 (3) | 0.1634 (3) | 0.0404 (13) | |
H46 | 0.3459 | 1.0400 | 0.1172 | 0.048* | |
C51 | 0.4633 (4) | 0.8089 (3) | 0.1546 (3) | 0.0361 (12) | |
C52 | 0.5657 (5) | 0.8276 (4) | 0.1608 (4) | 0.0533 (16) | |
H52 | 0.5820 | 0.8747 | 0.1466 | 0.064* | |
C53 | 0.6439 (5) | 0.7758 (5) | 0.1882 (4) | 0.070 (2) | |
H53 | 0.7122 | 0.7879 | 0.1910 | 0.084* | |
C54 | 0.6203 (6) | 0.7066 (5) | 0.2113 (4) | 0.074 (2) | |
H54 | 0.6729 | 0.6721 | 0.2293 | 0.089* | |
C55 | 0.5199 (6) | 0.6886 (4) | 0.2078 (4) | 0.0569 (17) | |
H55 | 0.5043 | 0.6422 | 0.2241 | 0.068* | |
C56 | 0.4405 (5) | 0.7406 (3) | 0.1794 (3) | 0.0459 (14) | |
H56 | 0.3723 | 0.7288 | 0.1774 | 0.055* | |
C61 | 0.3659 (4) | 0.9116 (3) | 0.0348 (3) | 0.0342 (11) | |
C62 | 0.2874 (4) | 0.9593 (3) | −0.0039 (3) | 0.0462 (14) | |
H62 | 0.2330 | 0.9720 | 0.0150 | 0.055* | |
C63 | 0.2900 (5) | 0.9874 (4) | −0.0693 (3) | 0.0511 (15) | |
H63 | 0.2386 | 1.0203 | −0.0937 | 0.061* | |
C64 | 0.3670 (5) | 0.9677 (4) | −0.0988 (3) | 0.0546 (16) | |
H64 | 0.3678 | 0.9863 | −0.1434 | 0.065* | |
C65 | 0.4446 (5) | 0.9195 (4) | −0.0619 (4) | 0.0545 (16) | |
H65 | 0.4974 | 0.9059 | −0.0820 | 0.065* | |
C66 | 0.4436 (4) | 0.8919 (3) | 0.0039 (3) | 0.0434 (14) | |
H66 | 0.4958 | 0.8596 | 0.0281 | 0.052* | |
B1 | 0.0782 (5) | 0.8534 (4) | 0.2506 (4) | 0.0423 (15) | |
B2 | 0.1833 (5) | 0.8786 (3) | 0.2181 (3) | 0.0342 (13) | |
B3 | 0.1302 (5) | 0.7853 (4) | 0.2050 (3) | 0.0356 (13) | |
B4 | −0.0048 (5) | 0.7896 (4) | 0.1932 (4) | 0.0393 (14) | |
B5 | −0.0362 (5) | 0.8876 (4) | 0.1868 (4) | 0.0413 (15) | |
B6 | 0.0789 (5) | 0.9425 (4) | 0.2083 (4) | 0.0403 (15) | |
B8 | 0.0435 (5) | 0.7653 (3) | 0.1194 (3) | 0.0331 (13) | |
B9 | −0.0643 (5) | 0.8337 (3) | 0.1087 (4) | 0.0381 (14) | |
B10 | −0.0023 (5) | 0.9379 (3) | 0.1208 (4) | 0.0389 (15) | |
B11 | 0.1378 (5) | 0.9345 (3) | 0.1397 (3) | 0.0348 (13) | |
H1 | 0.087 (4) | 0.849 (3) | 0.309 (3) | 0.025 (12)* | |
H2 | 0.256 (4) | 0.891 (3) | 0.251 (3) | 0.032 (13)* | |
H3 | 0.174 (4) | 0.738 (3) | 0.226 (3) | 0.040 (15)* | |
H4 | −0.050 (5) | 0.749 (4) | 0.210 (3) | 0.059 (18)* | |
H5 | −0.104 (4) | 0.911 (3) | 0.202 (3) | 0.037 (14)* | |
H6 | 0.086 (4) | 0.998 (3) | 0.244 (3) | 0.046 (16)* | |
H8 | 0.034 (4) | 0.709 (3) | 0.098 (3) | 0.028 (13)* | |
H10 | −0.047 (4) | 0.985 (3) | 0.089 (3) | 0.031 (13)* | |
H11 | 0.175 (4) | 0.976 (3) | 0.118 (3) | 0.039 (15)* | |
H1U | 0.003 (5) | 0.810 (3) | 0.068 (4) | 0.07 (2)* | |
H2U | 0.055 (4) | 0.925 (3) | 0.094 (3) | 0.037 (14)* | |
Cl1 | 0.5410 (5) | 0.5221 (3) | 0.0903 (2) | 0.237 (3) | |
Cl2 | 0.7355 (3) | 0.4928 (4) | 0.1878 (3) | 0.226 (3) | |
C1S | 0.6056 (10) | 0.4766 (7) | 0.1599 (7) | 0.148 (5) | |
H1S | 0.5950 | 0.4235 | 0.1499 | 0.178* | |
H2S | 0.5766 | 0.4882 | 0.1993 | 0.178* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Pt7 | 0.02531 (11) | 0.02416 (11) | 0.03163 (12) | 0.00079 (8) | 0.00662 (8) | 0.00101 (8) |
P1 | 0.0315 (7) | 0.0252 (6) | 0.0357 (7) | −0.0001 (5) | 0.0080 (5) | −0.0005 (5) |
P2 | 0.0273 (6) | 0.0279 (6) | 0.0350 (7) | −0.0002 (5) | 0.0074 (5) | −0.0001 (5) |
O1 | 0.0267 (19) | 0.047 (2) | 0.069 (3) | 0.0046 (17) | 0.0014 (19) | −0.010 (2) |
C1 | 0.037 (3) | 0.050 (4) | 0.059 (4) | 0.002 (3) | 0.007 (3) | −0.011 (3) |
C2 | 0.048 (4) | 0.083 (6) | 0.080 (5) | 0.004 (4) | −0.004 (4) | 0.000 (4) |
C3 | 0.064 (5) | 0.046 (4) | 0.112 (7) | −0.012 (4) | 0.015 (5) | −0.004 (4) |
C11 | 0.034 (3) | 0.032 (3) | 0.039 (3) | 0.001 (2) | 0.010 (2) | −0.008 (2) |
C12 | 0.041 (3) | 0.045 (3) | 0.048 (3) | 0.004 (3) | 0.010 (3) | −0.007 (3) |
C13 | 0.041 (4) | 0.061 (4) | 0.080 (5) | 0.006 (3) | 0.019 (3) | −0.014 (4) |
C14 | 0.051 (4) | 0.092 (6) | 0.065 (5) | −0.011 (4) | 0.033 (4) | −0.022 (4) |
C15 | 0.055 (4) | 0.082 (5) | 0.043 (4) | −0.006 (4) | 0.015 (3) | −0.007 (3) |
C16 | 0.043 (3) | 0.058 (4) | 0.043 (3) | 0.000 (3) | 0.009 (3) | 0.000 (3) |
C21 | 0.035 (3) | 0.033 (3) | 0.036 (3) | −0.004 (2) | 0.009 (2) | −0.006 (2) |
C22 | 0.046 (3) | 0.039 (3) | 0.054 (4) | −0.009 (3) | 0.010 (3) | −0.012 (3) |
C23 | 0.041 (3) | 0.079 (5) | 0.056 (4) | −0.016 (4) | 0.001 (3) | −0.028 (4) |
C24 | 0.045 (4) | 0.082 (5) | 0.042 (4) | 0.003 (4) | −0.004 (3) | −0.004 (3) |
C25 | 0.051 (4) | 0.056 (4) | 0.046 (4) | 0.011 (3) | −0.004 (3) | 0.010 (3) |
C26 | 0.041 (3) | 0.041 (3) | 0.041 (3) | −0.002 (3) | 0.004 (3) | 0.004 (2) |
C31 | 0.042 (3) | 0.026 (3) | 0.055 (4) | 0.002 (2) | 0.018 (3) | −0.001 (2) |
C32 | 0.047 (3) | 0.039 (3) | 0.053 (4) | 0.007 (3) | 0.020 (3) | 0.007 (3) |
C33 | 0.067 (5) | 0.058 (4) | 0.077 (5) | 0.016 (4) | 0.025 (4) | 0.029 (4) |
C34 | 0.115 (7) | 0.029 (3) | 0.119 (7) | 0.013 (4) | 0.052 (6) | 0.018 (4) |
C35 | 0.116 (7) | 0.031 (3) | 0.097 (6) | 0.005 (4) | 0.048 (5) | −0.009 (4) |
C36 | 0.079 (5) | 0.033 (3) | 0.063 (4) | −0.001 (3) | 0.027 (4) | −0.006 (3) |
C41 | 0.030 (3) | 0.032 (3) | 0.038 (3) | −0.005 (2) | 0.009 (2) | −0.007 (2) |
C42 | 0.049 (3) | 0.043 (3) | 0.046 (3) | −0.002 (3) | 0.004 (3) | −0.006 (3) |
C43 | 0.062 (4) | 0.061 (4) | 0.044 (4) | −0.004 (3) | −0.002 (3) | −0.010 (3) |
C44 | 0.064 (4) | 0.048 (4) | 0.061 (4) | −0.011 (3) | 0.016 (3) | −0.025 (3) |
C45 | 0.061 (4) | 0.032 (3) | 0.067 (4) | −0.005 (3) | 0.020 (3) | −0.007 (3) |
C46 | 0.043 (3) | 0.032 (3) | 0.046 (3) | −0.001 (2) | 0.013 (3) | −0.003 (2) |
C51 | 0.032 (3) | 0.036 (3) | 0.035 (3) | 0.010 (2) | 0.000 (2) | 0.002 (2) |
C52 | 0.039 (3) | 0.052 (4) | 0.065 (4) | 0.002 (3) | 0.007 (3) | −0.005 (3) |
C53 | 0.033 (3) | 0.085 (6) | 0.081 (5) | 0.013 (4) | −0.004 (3) | −0.011 (4) |
C54 | 0.059 (5) | 0.072 (5) | 0.073 (5) | 0.030 (4) | −0.012 (4) | −0.012 (4) |
C55 | 0.069 (5) | 0.044 (4) | 0.049 (4) | 0.014 (3) | 0.001 (3) | 0.006 (3) |
C56 | 0.045 (3) | 0.043 (3) | 0.044 (3) | 0.006 (3) | 0.002 (3) | 0.001 (3) |
C61 | 0.036 (3) | 0.030 (3) | 0.036 (3) | −0.006 (2) | 0.008 (2) | 0.000 (2) |
C62 | 0.041 (3) | 0.046 (3) | 0.051 (3) | 0.003 (3) | 0.012 (3) | 0.007 (3) |
C63 | 0.049 (4) | 0.055 (4) | 0.046 (3) | 0.003 (3) | 0.007 (3) | 0.012 (3) |
C64 | 0.065 (4) | 0.057 (4) | 0.044 (3) | −0.010 (3) | 0.021 (3) | 0.009 (3) |
C65 | 0.057 (4) | 0.054 (4) | 0.062 (4) | 0.001 (3) | 0.032 (3) | 0.003 (3) |
C66 | 0.040 (3) | 0.042 (3) | 0.054 (4) | 0.002 (3) | 0.022 (3) | 0.007 (3) |
B1 | 0.046 (4) | 0.041 (4) | 0.041 (4) | 0.002 (3) | 0.012 (3) | −0.001 (3) |
B2 | 0.035 (3) | 0.033 (3) | 0.036 (3) | −0.002 (3) | 0.010 (3) | −0.004 (3) |
B3 | 0.032 (3) | 0.037 (3) | 0.039 (3) | 0.004 (3) | 0.012 (3) | 0.008 (3) |
B4 | 0.037 (3) | 0.033 (3) | 0.054 (4) | 0.000 (3) | 0.021 (3) | 0.009 (3) |
B5 | 0.034 (3) | 0.041 (4) | 0.055 (4) | 0.003 (3) | 0.022 (3) | −0.004 (3) |
B6 | 0.038 (3) | 0.035 (3) | 0.044 (4) | −0.004 (3) | 0.006 (3) | −0.006 (3) |
B8 | 0.033 (3) | 0.023 (3) | 0.043 (3) | 0.002 (2) | 0.011 (3) | 0.006 (3) |
B9 | 0.028 (3) | 0.032 (3) | 0.055 (4) | −0.002 (2) | 0.013 (3) | −0.004 (3) |
B10 | 0.029 (3) | 0.027 (3) | 0.060 (4) | 0.005 (2) | 0.012 (3) | 0.000 (3) |
B11 | 0.031 (3) | 0.029 (3) | 0.044 (3) | 0.000 (2) | 0.011 (3) | −0.005 (3) |
Cl1 | 0.348 (7) | 0.163 (4) | 0.142 (4) | 0.063 (4) | −0.032 (4) | 0.008 (3) |
Cl2 | 0.124 (3) | 0.379 (8) | 0.176 (4) | −0.042 (4) | 0.042 (3) | −0.059 (5) |
C1S | 0.185 (14) | 0.122 (10) | 0.127 (10) | −0.019 (9) | 0.025 (9) | 0.033 (8) |
Pt7—B3 | 2.205 (6) | C45—C46 | 1.398 (8) |
Pt7—B2 | 2.243 (6) | C45—H45 | 0.9300 |
Pt7—B11 | 2.294 (6) | C46—H46 | 0.9300 |
Pt7—B8 | 2.327 (6) | C51—C56 | 1.377 (8) |
Pt7—P2 | 2.3325 (14) | C51—C52 | 1.388 (8) |
Pt7—P1 | 2.3636 (14) | C52—C53 | 1.391 (9) |
P1—C31 | 1.825 (5) | C52—H52 | 0.9300 |
P1—C11 | 1.834 (5) | C53—C54 | 1.381 (11) |
P1—C21 | 1.834 (5) | C53—H53 | 0.9300 |
P2—C61 | 1.821 (5) | C54—C55 | 1.371 (11) |
P2—C51 | 1.830 (5) | C54—H54 | 0.9300 |
P2—C41 | 1.835 (5) | C55—C56 | 1.409 (8) |
O1—B9 | 1.384 (7) | C55—H55 | 0.9300 |
O1—C1 | 1.431 (7) | C56—H56 | 0.9300 |
C1—C2 | 1.514 (9) | C61—C66 | 1.383 (7) |
C1—C3 | 1.517 (9) | C61—C62 | 1.403 (7) |
C1—H1F | 0.9800 | C62—C63 | 1.375 (8) |
C2—H2A | 0.9600 | C62—H62 | 0.9300 |
C2—H2B | 0.9600 | C63—C64 | 1.359 (9) |
C2—H2C | 0.9600 | C63—H63 | 0.9300 |
C3—H3A | 0.9600 | C64—C65 | 1.388 (9) |
C3—H3B | 0.9600 | C64—H64 | 0.9300 |
C3—H3C | 0.9600 | C65—C66 | 1.371 (8) |
C11—C16 | 1.378 (8) | C65—H65 | 0.9300 |
C11—C12 | 1.395 (8) | C66—H66 | 0.9300 |
C12—C13 | 1.381 (9) | B1—B2 | 1.756 (9) |
C12—H12 | 0.9300 | B1—B3 | 1.757 (9) |
C13—C14 | 1.367 (10) | B1—B4 | 1.761 (10) |
C13—H13 | 0.9300 | B1—B6 | 1.792 (9) |
C14—C15 | 1.368 (10) | B1—B5 | 1.796 (10) |
C14—H14 | 0.9300 | B1—H1 | 1.10 (5) |
C15—C16 | 1.387 (9) | B2—B6 | 1.778 (9) |
C15—H15 | 0.9300 | B2—B11 | 1.780 (9) |
C16—H16 | 0.9300 | B2—B3 | 1.803 (9) |
C21—C22 | 1.378 (7) | B2—H2 | 1.04 (5) |
C21—C26 | 1.384 (7) | B3—B4 | 1.766 (9) |
C22—C23 | 1.400 (9) | B3—B8 | 1.781 (9) |
C22—H22 | 0.9300 | B3—H3 | 1.05 (6) |
C23—C24 | 1.373 (10) | B4—B8 | 1.779 (9) |
C23—H23 | 0.9300 | B4—B9 | 1.796 (10) |
C24—C25 | 1.371 (10) | B4—B5 | 1.797 (9) |
C24—H24 | 0.9300 | B4—H4 | 1.06 (6) |
C25—C26 | 1.382 (8) | B5—B10 | 1.724 (9) |
C25—H25 | 0.9300 | B5—B9 | 1.746 (9) |
C26—H26 | 0.9300 | B5—B6 | 1.782 (9) |
C31—C36 | 1.389 (8) | B5—H5 | 1.11 (5) |
C31—C32 | 1.398 (8) | B6—B11 | 1.730 (9) |
C32—C33 | 1.390 (9) | B6—B10 | 1.748 (9) |
C32—H32 | 0.9300 | B6—H6 | 1.20 (6) |
C33—C34 | 1.377 (11) | B8—B9 | 1.862 (8) |
C33—H33 | 0.9300 | B8—H8 | 1.08 (5) |
C34—C35 | 1.387 (11) | B8—H1U | 1.28 (7) |
C34—H34 | 0.9300 | B9—B10 | 2.025 (9) |
C35—C36 | 1.382 (9) | B9—H1U | 1.42 (7) |
C35—H35 | 0.9300 | B10—B11 | 1.818 (9) |
C36—H36 | 0.9300 | B10—H10 | 1.11 (5) |
C41—C42 | 1.393 (8) | B10—H2U | 1.07 (5) |
C41—C46 | 1.395 (7) | B11—H11 | 1.04 (5) |
C42—C43 | 1.391 (8) | B11—H2U | 1.23 (5) |
C42—H42 | 0.9300 | Cl1—C1S | 1.609 (12) |
C43—C44 | 1.370 (9) | Cl2—C1S | 1.704 (13) |
C43—H43 | 0.9300 | C1S—H1S | 0.9700 |
C44—C45 | 1.356 (9) | C1S—H2S | 0.9700 |
C44—H44 | 0.9300 | ||
B3—Pt7—B2 | 47.8 (2) | B2—B1—B4 | 111.8 (5) |
B3—Pt7—B11 | 82.4 (2) | B3—B1—B4 | 60.3 (4) |
B2—Pt7—B11 | 46.2 (2) | B2—B1—B6 | 60.1 (4) |
B3—Pt7—B8 | 46.2 (2) | B3—B1—B6 | 109.3 (5) |
B2—Pt7—B8 | 83.7 (2) | B4—B1—B6 | 111.5 (5) |
B11—Pt7—B8 | 89.7 (2) | B2—B1—B5 | 106.6 (5) |
B3—Pt7—P2 | 133.49 (17) | B3—B1—B5 | 105.8 (5) |
B2—Pt7—P2 | 95.47 (16) | B4—B1—B5 | 60.7 (4) |
B11—Pt7—P2 | 89.28 (16) | B6—B1—B5 | 59.6 (4) |
B8—Pt7—P2 | 178.97 (15) | B2—B1—H1 | 121 (2) |
B3—Pt7—P1 | 118.17 (18) | B3—B1—H1 | 121 (3) |
B2—Pt7—P1 | 165.92 (16) | B4—B1—H1 | 118 (3) |
B11—Pt7—P1 | 140.00 (16) | B6—B1—H1 | 122 (3) |
B8—Pt7—P1 | 83.72 (16) | B5—B1—H1 | 124 (2) |
P2—Pt7—P1 | 97.15 (5) | B1—B2—B6 | 60.9 (4) |
C31—P1—C11 | 98.8 (2) | B1—B2—B11 | 109.2 (4) |
C31—P1—C21 | 108.2 (3) | B6—B2—B11 | 58.2 (3) |
C11—P1—C21 | 102.8 (2) | B1—B2—B3 | 59.2 (4) |
C31—P1—Pt7 | 116.38 (19) | B6—B2—B3 | 107.9 (4) |
C11—P1—Pt7 | 122.91 (17) | B11—B2—B3 | 111.6 (4) |
C21—P1—Pt7 | 106.36 (17) | B1—B2—Pt7 | 117.9 (4) |
C61—P2—C51 | 108.7 (3) | B6—B2—Pt7 | 118.4 (4) |
C61—P2—C41 | 104.5 (2) | B11—B2—Pt7 | 68.4 (3) |
C51—P2—C41 | 99.8 (2) | B3—B2—Pt7 | 65.0 (3) |
C61—P2—Pt7 | 114.92 (17) | B1—B2—H2 | 123 (3) |
C51—P2—Pt7 | 109.18 (19) | B6—B2—H2 | 121 (3) |
C41—P2—Pt7 | 118.51 (16) | B11—B2—H2 | 117 (3) |
B9—O1—C1 | 121.9 (4) | B3—B2—H2 | 124 (3) |
O1—C1—C2 | 107.0 (5) | Pt7—B2—H2 | 109 (3) |
O1—C1—C3 | 110.2 (6) | B1—B3—B4 | 60.0 (4) |
C2—C1—C3 | 111.7 (6) | B1—B3—B8 | 111.0 (4) |
O1—C1—H1F | 109.3 | B4—B3—B8 | 60.2 (4) |
C2—C1—H1F | 109.3 | B1—B3—B2 | 59.1 (4) |
C3—C1—H1F | 109.3 | B4—B3—B2 | 109.3 (4) |
C1—C2—H2A | 109.5 | B8—B3—B2 | 116.7 (4) |
C1—C2—H2B | 109.5 | B1—B3—Pt7 | 119.8 (4) |
H2A—C2—H2B | 109.5 | B4—B3—Pt7 | 122.1 (4) |
C1—C2—H2C | 109.5 | B8—B3—Pt7 | 70.5 (3) |
H2A—C2—H2C | 109.5 | B2—B3—Pt7 | 67.2 (3) |
H2B—C2—H2C | 109.5 | B1—B3—H3 | 128 (3) |
C1—C3—H3A | 109.5 | B4—B3—H3 | 122 (3) |
C1—C3—H3B | 109.5 | B8—B3—H3 | 111 (3) |
H3A—C3—H3B | 109.5 | B2—B3—H3 | 122 (3) |
C1—C3—H3C | 109.5 | Pt7—B3—H3 | 102 (3) |
H3A—C3—H3C | 109.5 | B1—B4—B3 | 59.8 (4) |
H3B—C3—H3C | 109.5 | B1—B4—B8 | 111.0 (4) |
C16—C11—C12 | 118.8 (5) | B3—B4—B8 | 60.3 (3) |
C16—C11—P1 | 122.5 (4) | B1—B4—B9 | 109.8 (5) |
C12—C11—P1 | 118.6 (4) | B3—B4—B9 | 108.7 (4) |
C13—C12—C11 | 120.2 (6) | B8—B4—B9 | 62.8 (4) |
C13—C12—H12 | 119.9 | B1—B4—B5 | 60.6 (4) |
C11—C12—H12 | 119.9 | B3—B4—B5 | 105.3 (4) |
C14—C13—C12 | 120.2 (6) | B8—B4—B5 | 108.2 (4) |
C14—C13—H13 | 119.9 | B9—B4—B5 | 58.1 (4) |
C12—C13—H13 | 119.9 | B1—B4—H4 | 125 (3) |
C13—C14—C15 | 120.2 (6) | B3—B4—H4 | 126 (3) |
C13—C14—H14 | 119.9 | B8—B4—H4 | 117 (3) |
C15—C14—H14 | 119.9 | B9—B4—H4 | 116 (3) |
C14—C15—C16 | 120.3 (7) | B5—B4—H4 | 123 (3) |
C14—C15—H15 | 119.9 | B10—B5—B9 | 71.4 (4) |
C16—C15—H15 | 119.9 | B10—B5—B6 | 59.8 (4) |
C11—C16—C15 | 120.3 (6) | B9—B5—B6 | 118.2 (5) |
C11—C16—H16 | 119.8 | B10—B5—B1 | 109.7 (4) |
C15—C16—H16 | 119.8 | B9—B5—B1 | 110.5 (5) |
C22—C21—C26 | 118.7 (5) | B6—B5—B1 | 60.1 (4) |
C22—C21—P1 | 123.7 (4) | B10—B5—B4 | 117.0 (5) |
C26—C21—P1 | 117.6 (4) | B9—B5—B4 | 60.9 (4) |
C21—C22—C23 | 120.2 (6) | B6—B5—B4 | 110.3 (4) |
C21—C22—H22 | 119.9 | B1—B5—B4 | 58.7 (4) |
C23—C22—H22 | 119.9 | B10—B5—H5 | 114 (3) |
C24—C23—C22 | 120.3 (6) | B9—B5—H5 | 116 (3) |
C24—C23—H23 | 119.9 | B6—B5—H5 | 117 (3) |
C22—C23—H23 | 119.9 | B1—B5—H5 | 123 (3) |
C25—C24—C23 | 119.5 (6) | B4—B5—H5 | 122 (3) |
C25—C24—H24 | 120.2 | B11—B6—B10 | 63.0 (4) |
C23—C24—H24 | 120.2 | B11—B6—B2 | 61.0 (4) |
C24—C25—C26 | 120.4 (6) | B10—B6—B2 | 109.7 (4) |
C24—C25—H25 | 119.8 | B11—B6—B5 | 109.1 (4) |
C26—C25—H25 | 119.8 | B10—B6—B5 | 58.5 (4) |
C25—C26—C21 | 120.8 (6) | B2—B6—B5 | 106.3 (4) |
C25—C26—H26 | 119.6 | B11—B6—B1 | 109.9 (5) |
C21—C26—H26 | 119.6 | B10—B6—B1 | 108.8 (4) |
C36—C31—C32 | 119.0 (5) | B2—B6—B1 | 58.9 (4) |
C36—C31—P1 | 119.8 (5) | B5—B6—B1 | 60.3 (4) |
C32—C31—P1 | 121.1 (4) | B11—B6—H6 | 122 (3) |
C33—C32—C31 | 120.6 (6) | B10—B6—H6 | 122 (3) |
C33—C32—H32 | 119.7 | B2—B6—H6 | 122 (3) |
C31—C32—H32 | 119.7 | B5—B6—H6 | 121 (3) |
C34—C33—C32 | 119.6 (7) | B1—B6—H6 | 119 (3) |
C34—C33—H33 | 120.2 | B4—B8—B3 | 59.5 (4) |
C32—C33—H33 | 120.2 | B4—B8—B9 | 59.1 (4) |
C33—C34—C35 | 120.3 (6) | B3—B8—B9 | 105.2 (4) |
C33—C34—H34 | 119.8 | B4—B8—Pt7 | 115.3 (4) |
C35—C34—H34 | 119.8 | B3—B8—Pt7 | 63.3 (3) |
C36—C35—C34 | 120.2 (7) | B9—B8—Pt7 | 114.0 (3) |
C36—C35—H35 | 119.9 | B4—B8—H8 | 121 (3) |
C34—C35—H35 | 119.9 | B3—B8—H8 | 121 (3) |
C35—C36—C31 | 120.3 (7) | B9—B8—H8 | 124 (3) |
C35—C36—H36 | 119.8 | Pt7—B8—H8 | 113 (3) |
C31—C36—H36 | 119.8 | B4—B8—H1U | 108 (3) |
C42—C41—C46 | 118.7 (5) | B3—B8—H1U | 129 (3) |
C42—C41—P2 | 119.3 (4) | B9—B8—H1U | 50 (3) |
C46—C41—P2 | 122.0 (4) | Pt7—B8—H1U | 86 (3) |
C43—C42—C41 | 119.8 (6) | H8—B8—H1U | 107 (4) |
C43—C42—H42 | 120.1 | O1—B9—B5 | 120.0 (5) |
C41—C42—H42 | 120.1 | O1—B9—B4 | 129.9 (5) |
C44—C43—C42 | 121.0 (6) | B5—B9—B4 | 60.9 (4) |
C44—C43—H43 | 119.5 | O1—B9—B8 | 129.0 (5) |
C42—C43—H43 | 119.5 | B5—B9—B8 | 106.8 (4) |
C45—C44—C43 | 119.7 (6) | B4—B9—B8 | 58.2 (3) |
C45—C44—H44 | 120.2 | O1—B9—B10 | 115.3 (5) |
C43—C44—H44 | 120.2 | B5—B9—B10 | 53.8 (3) |
C44—C45—C46 | 121.0 (6) | B4—B9—B10 | 103.4 (4) |
C44—C45—H45 | 119.5 | B8—B9—B10 | 107.9 (4) |
C46—C45—H45 | 119.5 | O1—B9—H1U | 108 (3) |
C41—C46—C45 | 119.7 (5) | B5—B9—H1U | 129 (3) |
C41—C46—H46 | 120.1 | B4—B9—H1U | 101 (3) |
C45—C46—H46 | 120.1 | B8—B9—H1U | 43 (3) |
C56—C51—C52 | 119.6 (5) | B10—B9—H1U | 92 (3) |
C56—C51—P2 | 118.7 (4) | B5—B10—B6 | 61.8 (4) |
C52—C51—P2 | 121.6 (4) | B5—B10—B11 | 107.7 (5) |
C51—C52—C53 | 120.0 (6) | B6—B10—B11 | 58.0 (4) |
C51—C52—H52 | 120.0 | B5—B10—B9 | 54.8 (3) |
C53—C52—H52 | 120.0 | B6—B10—B9 | 106.5 (4) |
C54—C53—C52 | 120.2 (7) | B11—B10—B9 | 111.3 (4) |
C54—C53—H53 | 119.9 | B5—B10—H10 | 126 (3) |
C52—C53—H53 | 119.9 | B6—B10—H10 | 127 (3) |
C55—C54—C53 | 120.3 (6) | B11—B10—H10 | 121 (3) |
C55—C54—H54 | 119.8 | B9—B10—H10 | 119 (3) |
C53—C54—H54 | 119.8 | B5—B10—H2U | 128 (3) |
C54—C55—C56 | 119.6 (7) | B6—B10—H2U | 98 (3) |
C54—C55—H55 | 120.2 | B11—B10—H2U | 41 (3) |
C56—C55—H55 | 120.2 | B9—B10—H2U | 94 (3) |
C51—C56—C55 | 120.2 (6) | H10—B10—H2U | 105 (4) |
C51—C56—H56 | 119.9 | B6—B11—B2 | 60.8 (4) |
C55—C56—H56 | 119.9 | B6—B11—B10 | 59.0 (4) |
C66—C61—C62 | 118.0 (5) | B2—B11—B10 | 106.5 (4) |
C66—C61—P2 | 123.4 (4) | B6—B11—Pt7 | 118.1 (4) |
C62—C61—P2 | 118.6 (4) | B2—B11—Pt7 | 65.4 (3) |
C63—C62—C61 | 120.6 (6) | B10—B11—Pt7 | 114.0 (3) |
C63—C62—H62 | 119.7 | B6—B11—H11 | 129 (3) |
C61—C62—H62 | 119.7 | B2—B11—H11 | 131 (3) |
C64—C63—C62 | 120.5 (6) | B10—B11—H11 | 119 (3) |
C64—C63—H63 | 119.7 | Pt7—B11—H11 | 109 (3) |
C62—C63—H63 | 119.7 | B6—B11—H2U | 93 (2) |
C63—C64—C65 | 119.7 (6) | B2—B11—H2U | 124 (3) |
C63—C64—H64 | 120.1 | B10—B11—H2U | 35 (2) |
C65—C64—H64 | 120.1 | Pt7—B11—H2U | 93 (3) |
C66—C65—C64 | 120.3 (6) | H11—B11—H2U | 105 (4) |
C66—C65—H65 | 119.9 | Cl1—C1S—Cl2 | 116.7 (8) |
C64—C65—H65 | 119.9 | Cl1—C1S—H1S | 108.1 |
C65—C66—C61 | 120.8 (6) | Cl2—C1S—H1S | 108.1 |
C65—C66—H66 | 119.6 | Cl1—C1S—H2S | 108.1 |
C61—C66—H66 | 119.6 | Cl2—C1S—H2S | 108.1 |
B2—B1—B3 | 61.7 (4) | H1S—C1S—H2S | 107.3 |
Experimental details
(I) | (II) | (III) | |
Crystal data | |||
Chemical formula | [Pt(CH14B10O)(C18H15P)2]·0.5CH2Cl2 | [Pt(C3H18B10O)(C18H15P)2]·CH2Cl2 | [Pt(C3H18B10O)(C18H15P)2]·CH2Cl2 |
Mr | 912.32 | 982.83 | 982.83 |
Crystal system, space group | Monoclinic, P21/n | Monoclinic, P21/n | Monoclinic, P21/n |
Temperature (K) | 293 | 293 | 293 |
a, b, c (Å) | 12.850 (2), 25.824 (7), 13.308 (2) | 11.114 (3), 21.634 (8), 18.990 (8) | 13.435 (3), 17.864 (4), 19.383 (4) |
α, β, γ (°) | 90, 105.77 (1), 90 | 90, 103.75 (3), 90 | 90, 105.94 (2), 90 |
V (Å3) | 4249.9 (15) | 4435 (3) | 4473.1 (17) |
Z | 4 | 4 | 4 |
Radiation type | Mo Kα | Mo Kα | Mo Kα |
µ (mm−1) | 3.47 | 3.39 | 3.36 |
Crystal size (mm) | 0.3 × 0.2 × 0.2 | 0.42 × 0.27 × 0.07 | 0.44 × 0.34 × 0.32 |
Data collection | |||
Diffractometer | Rigaku AFC-7R diffractometer | Enraf-Nonius CAD-4 diffractometer | Rigaku AFC-7R diffractometer |
Absorption correction | ψ scans (North et al., 1968) | ψ scans (North et al., 1968) | ψ scans (North et al., 1968) |
Tmin, Tmax | 0.423, 0.544 | 0.330, 0.797 | 0.320, 0.413 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 7336, 6984, 5607 | 8141, 7894, 4066 | 8222, 7865, 6198 |
Rint | 0.048 | 0.081 | 0.048 |
(sin θ/λ)max (Å−1) | 0.595 | 0.597 | 0.595 |
Refinement | |||
R[F2 > 2σ(F2)], wR(F2), S | 0.037, 0.105, 1.04 | 0.069, 0.238, 1.38 | 0.035, 0.096, 1.03 |
No. of reflections | 6984 | 7894 | 7865 |
No. of parameters | 495 | 507 | 549 |
No. of restraints | 2 | 0 | 0 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement | H atoms treated by a mixture of independent and constrained refinement | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 1.98, −1.71 | 2.19, −3.02 | 2.30, −0.99 |
Computer programs: MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1992), CAD-4 Manual (Enraf-Nonius, 1988), MSC/AFC Diffractometer Control Software, CAD-4 Manual, TEXSAN (Molecular Structure Corporation, 1985), SDP-Plus (Frenz, 1985), SHELXS97 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997), ZORTEP (Zsolnai, 1994), SHELXL97.
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The polyhedral borane dianion, B10H102-, has been extensively studied due to its extreme thermal, hydrolytic, and oxidative stability (Mutterties & Knoth, 1968; Kennedy, 1986; Barton & Srivastava, 1995). Although a number of metal derivatives have been prepared, little work has been reported on the cage-opening mechanism. Marshall et al. (1967) postulated the cage opening of B10H102- in the anhydrous HCl/diethyl sulfide system as occurring via a two-proton attack process on two pairs of apex-to-equatorial B atoms. Paxson & Hawthorne (1975) studied the reaction of PtCl2(PPh3)2 and K2B10H10 in alcoholic chloroform, and obtained the alkoxy-substituted nido-[(PPh3)2PtB10H11(OC2H5)]; spectroscopic studies showed that the ethoxy group could be at various positions (i.e. 2, 3, 8, 9, 10 or 11). Gaft et al. (1983) found that the hydrogen-bridged compound [(PPh3)2PtB10H10], derived from the reaction of PtI2(PPh3)2 and Ag2B10H10 in CH3CN/CH2Cl2, could also be transformed in C2H5OH into nido-[(PPh3)2PtB10H11(OC2H5)], so that [(PPh3)2PtB10H10] could be the intermediate of the reaction system containing B10H102- and a platinum halide. However, none of these intermediates or their ultimate products have been structurally characterized. To extend the study of the cage-opening mode and the substituent effect on the cluster geometry, we have carried out the same reaction in methanol and iso-propyl alcohol, and here we report the structures of the three title platinaboranes, (I), (II) and (III). \sch
As expected, in compounds (I)-(III) the 11-vertex nido clusters are produced, the methoxy group is found to be on atom B8 in (I), and the isopropoxy groups are on atom B8 in (II) and atom B9 in (III). The intramolecular distances and angles, and even the orientations of the PPh3 ligands, are essentially the same in (I)-(III). The Pt—B distances vary in the ranges 2.214 (7)–2.303 (7) Å in (I), 2.178 (16)–2.326 (16) Å in (II), and 2.205 (6)–2.327 (6) Å in (III), which are similar to but slightly longer than those of the unsubstituted cluster [(PMe2Ph)2PtB10H12] [2.214 (5)–2.301 (6) Å; Boocock et al., 1981], probably as another consequence of the presence of the alkoxy groups. With regard to the B—O bond lengths, the present values are both close to each other and in the range of those reported for cage-B—OR groups (1.371–1.409 Å; Kennedy, 1986).
The present three structures, along with the related examples described above, suggest that the reaction of PtX2(PR3)2 in alcohols is so complex that alcohols could attack on the (opened) cage intermediates from different positions. It should be noted that a number of the 1,2-bis(diphenylphosphinoethane) and PMe2Ph relatives of the title compounds have been prepared, namely, the mono-substituted 8-OR or 9-OR compounds (R is Me or Et), but these, unfortunately, have not been structurally characterized (Kennedy, 1986).