Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807050726/kj2068sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807050726/kj2068Isup2.hkl |
CCDC reference: 667199
Equal volumes of 0.1 M Ph3P=O and CoCl2 solutions in methanol (ca 5 drops) were mixed before being syringed into a 0.7 mm diameter special glass X-ray sample tube to a depth of 4 mm. This tube was sealed in a larger sample tube containing ca 2 ml Et2O anti-solvent. The solvent level rose to the top of the 0.7 mm tube overnight (ca 30 mm), inducing the crystallization of blue plates. A suitable crystal was selected by immersing the 0.7 mm tube in fluorinated oil on a microscope slide before crushing the glass to release the crystals. It is hoped that this method of working reduced solvent loss during crystal selection and transfer to the diffractometer.
Hydrogen atoms were constrained to chemically reasonable positions. The methanol solvate molecule was treated isotropically with refined partial site occupancy, which was eventually fixed at 0.5 to allow the refinement to fully converge. Refinement of the Flack parameter indicated the prescence of a racemic twin with twin components ratio 0.60 (4):0.40 (4).
The title methanol solvate crystallized when a methanolic solution of CoCl2(OPPh3)2, contained in a 0.7 mm tube, was subjected to vapour diffusion using Et2O anti-solvent. The more common unsolvated crystals formed when a 10 mm diameter tube was used.
All unsolvated 1st row d-block MCl2(OPPh3)2 crystal structures are isostructural, crystallizing in orthorhombic space group Fdd2 with each molecule having strict crystallographic C2 symmetry In each case the O—P bonds project into the region between the two Cl ligands with a stagger angle ranging from 36.8 (2) to 42.3 (4)°, as measured by the P—O—M—Cl torsion angles. This contrasts with the situation in the only previously reported solvated structure, a Zn complex containing THF of crystallization, in which the two P atoms nearly eclipse the Zn—Cl bonds with P—O—Zn—Cl torsion angles of 8.3 (2) and 8.8 (2)°. In this case the O—P bonds project into a region just outside the range subtended by the two Cl atoms.
The four crystallographically distinct CoCl2(OPPh3)2 molecules, which comprise the title structure (Figs. 1–5), have simmilar configurations to each other but differ from the above structures. In each case one O—P bond projects into the region between the two Cl atoms (P—O—Co—Cl 21.2 (8) to 42.1 (8)°), and the other is directed away (P—O—Co—Cl 110.9 (8) to 147.4 (6)°). Comparison of the pseudo-tetrahedral geometry in the title structure with that in the unsolvated Co structures shows that the above torsional changes are accompanied by other significant bond length and angle changes (Table 1).
The lamelar nature of the title structure can be seen in the packing digrams (Fig. 6). The methanol, which semi-populates its interlayer sites and displays high vibrational amplitudes, does not form well defined interactions with the host molecules. Furthermore residual voids (total 35 Å3) in the interlayer region suggest that solvent molecules may have been lost after crystallization.
It is interesting to speculate what role the narrower crystallization container may have had in directing the formation of this lamelar solvate. As a greater depth of anti-solvent was attained in the narrower 0.7 mm crystallization tube, compared to what was achieved in the 10 mm bore tube, it would seem reasonable to suggest that the a mixed Et2O/MeOH solvate may have been formed initially, with the reported structure resulting from partial solvent loss.
Unsolvated crystal structures of the title compound have been reported previously by Cotton et al. (2002) and Marsh (1997), who re-analysed a determination by Mangion et al. (1976). These structures are identical and isostructural with the analogous complexes of Mn(II) (Tomita, 1985), Ni(II) (Moreno-Fuquen et al., 2004), Cu (II) (Bertrand & Kalyanaraman, 1971 and Weinberger et al., 1997) and Zn(II) (Rose et al., 1980 and Kosky et al., 1982). A THF solvate of the latter complex has also been reported (Zeller et al., 2001).
Data collection: COLLECT (Nonius, 1998); cell refinement: SCALEPACK (Otwinowski & Minor, 1997); data reduction: SCALEPACK and DENZO (Otwinowski & Minor 1997); program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997) and PLATON (Spek, 2003); software used to prepare material for publication: WinGX (Farrugia, 1999).
[CoCl2(C18H15OP)2]·0.125CH4O | F(000) = 5683 |
Mr = 690.13 | Dx = 1.375 Mg m−3 |
Monoclinic, Cc | Mo Kα radiation, λ = 0.71073 Å |
a = 21.3691 (3) Å | Cell parameters from 12813 reflections |
b = 37.1989 (8) Å | θ = 1.0–26.0° |
c = 19.4382 (5) Å | µ = 0.80 mm−1 |
β = 120.368 (1)° | T = 150 K |
V = 13331.4 (5) Å3 | Prism, blue |
Z = 16 | 0.22 × 0.12 × 0.05 mm |
Bruker–Nonius KappaCCD diffractometer | 9468 reflections with I > 2σ(I) |
CCD rotation images, thick slices scans | Rint = 0.095 |
Absorption correction: multi-scan (Blessing, 1995) | θmax = 26°, θmin = 3.0° |
Tmin = 0.843, Tmax = 0.961 | h = 0→26 |
13073 measured reflections | k = 0→45 |
13073 independent reflections | l = −23→20 |
Refinement on F2 | H-atom parameters constrained |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.0321P)2 + 57.6187P] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.059 | (Δ/σ)max = 0.021 |
wR(F2) = 0.133 | Δρmax = 0.63 e Å−3 |
S = 1.07 | Δρmin = −0.48 e Å−3 |
13073 reflections | Absolute structure: Flack (1983) |
1559 parameters | Absolute structure parameter: 0.40 (4) |
2 restraints |
[CoCl2(C18H15OP)2]·0.125CH4O | V = 13331.4 (5) Å3 |
Mr = 690.13 | Z = 16 |
Monoclinic, Cc | Mo Kα radiation |
a = 21.3691 (3) Å | µ = 0.80 mm−1 |
b = 37.1989 (8) Å | T = 150 K |
c = 19.4382 (5) Å | 0.22 × 0.12 × 0.05 mm |
β = 120.368 (1)° |
Bruker–Nonius KappaCCD diffractometer | 13073 independent reflections |
Absorption correction: multi-scan (Blessing, 1995) | 9468 reflections with I > 2σ(I) |
Tmin = 0.843, Tmax = 0.961 | Rint = 0.095 |
13073 measured reflections |
R[F2 > 2σ(F2)] = 0.059 | H-atom parameters constrained |
wR(F2) = 0.133 | w = 1/[σ2(Fo2) + (0.0321P)2 + 57.6187P] where P = (Fo2 + 2Fc2)/3 |
S = 1.07 | Δρmax = 0.63 e Å−3 |
13073 reflections | Δρmin = −0.48 e Å−3 |
1559 parameters | Absolute structure: Flack (1983) |
2 restraints | Absolute structure parameter: 0.40 (4) |
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. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Co1 | 0.23624 (7) | 0.03411 (3) | 0.23354 (7) | 0.0316 (3) | |
Cl1 | 0.17186 (13) | −0.01712 (6) | 0.20175 (15) | 0.0449 (6) | |
Cl2 | 0.25306 (14) | 0.06209 (7) | 0.14094 (15) | 0.0504 (6) | |
P1 | 0.19873 (12) | 0.09329 (6) | 0.33721 (14) | 0.0340 (5) | |
P2 | 0.39944 (12) | 0.00193 (6) | 0.37640 (14) | 0.0340 (5) | |
O1 | 0.1945 (3) | 0.07046 (15) | 0.2710 (4) | 0.0415 (15) | |
O2 | 0.3328 (3) | 0.02443 (15) | 0.3268 (3) | 0.0383 (14) | |
C1 | 0.1204 (4) | 0.1213 (2) | 0.2980 (5) | 0.0321 (18) | |
C2 | 0.0529 (5) | 0.1060 (2) | 0.2457 (5) | 0.037 (2) | |
H2 | 0.0504 | 0.0814 | 0.2314 | 0.045* | |
C3 | −0.0104 (5) | 0.1260 (3) | 0.2144 (6) | 0.045 (2) | |
H3 | −0.056 | 0.1151 | 0.1802 | 0.054* | |
C4 | −0.0064 (5) | 0.1618 (3) | 0.2334 (6) | 0.045 (2) | |
H4 | −0.0495 | 0.1758 | 0.21 | 0.054* | |
C5 | 0.0590 (5) | 0.1778 (2) | 0.2860 (6) | 0.045 (2) | |
H5 | 0.0605 | 0.2024 | 0.2998 | 0.053* | |
C6 | 0.1225 (5) | 0.1579 (2) | 0.3184 (6) | 0.043 (2) | |
H6 | 0.1675 | 0.1688 | 0.3545 | 0.052* | |
C7 | 0.2000 (5) | 0.0668 (2) | 0.4141 (5) | 0.036 (2) | |
C8 | 0.2302 (5) | 0.0319 (2) | 0.4279 (6) | 0.041 (2) | |
H8 | 0.2495 | 0.023 | 0.3966 | 0.049* | |
C9 | 0.2314 (6) | 0.0107 (3) | 0.4870 (6) | 0.053 (3) | |
H9 | 0.2526 | −0.0125 | 0.4971 | 0.064* | |
C10 | 0.2013 (5) | 0.0236 (3) | 0.5326 (6) | 0.047 (2) | |
H10 | 0.2 | 0.0089 | 0.5717 | 0.057* | |
C11 | 0.1742 (5) | 0.0579 (3) | 0.5192 (6) | 0.046 (2) | |
H11 | 0.1561 | 0.067 | 0.5515 | 0.056* | |
C12 | 0.1720 (5) | 0.0794 (2) | 0.4618 (5) | 0.037 (2) | |
H12 | 0.1518 | 0.1028 | 0.4537 | 0.044* | |
C13 | 0.2771 (5) | 0.1214 (2) | 0.3823 (6) | 0.043 (2) | |
C14 | 0.2986 (6) | 0.1380 (3) | 0.3327 (8) | 0.071 (4) | |
H14 | 0.2741 | 0.1324 | 0.2774 | 0.085* | |
C15 | 0.3552 (7) | 0.1624 (4) | 0.3639 (12) | 0.091 (5) | |
H15 | 0.3694 | 0.174 | 0.3303 | 0.109* | |
C16 | 0.3907 (7) | 0.1696 (3) | 0.4444 (14) | 0.102 (6) | |
H16 | 0.4289 | 0.1868 | 0.4659 | 0.122* | |
C17 | 0.3721 (7) | 0.1524 (4) | 0.4950 (10) | 0.092 (5) | |
H17 | 0.398 | 0.157 | 0.5507 | 0.11* | |
C18 | 0.3154 (6) | 0.1286 (3) | 0.4627 (7) | 0.062 (3) | |
H18 | 0.3022 | 0.1167 | 0.4968 | 0.074* | |
C19 | 0.3871 (5) | −0.0281 (2) | 0.4407 (6) | 0.038 (2) | |
C20 | 0.4251 (5) | −0.0235 (3) | 0.5235 (6) | 0.047 (2) | |
H20 | 0.4612 | −0.0054 | 0.5473 | 0.057* | |
C21 | 0.4098 (6) | −0.0458 (3) | 0.5707 (6) | 0.052 (3) | |
H21 | 0.4359 | −0.0429 | 0.627 | 0.063* | |
C22 | 0.3572 (5) | −0.0717 (3) | 0.5366 (6) | 0.047 (2) | |
H22 | 0.3464 | −0.0864 | 0.5693 | 0.057* | |
C23 | 0.3197 (5) | −0.0765 (2) | 0.4549 (7) | 0.051 (3) | |
H23 | 0.2837 | −0.0947 | 0.4316 | 0.061* | |
C24 | 0.3347 (5) | −0.0547 (2) | 0.4065 (6) | 0.042 (2) | |
H24 | 0.3091 | −0.0581 | 0.3503 | 0.051* | |
C25 | 0.4728 (4) | 0.0318 (2) | 0.4387 (5) | 0.035 (2) | |
C26 | 0.4551 (5) | 0.0652 (2) | 0.4549 (6) | 0.048 (2) | |
H26 | 0.4056 | 0.0721 | 0.4308 | 0.057* | |
C27 | 0.5091 (6) | 0.0890 (3) | 0.5063 (7) | 0.055 (3) | |
H27 | 0.497 | 0.1118 | 0.5182 | 0.066* | |
C28 | 0.5816 (5) | 0.0783 (3) | 0.5400 (6) | 0.052 (3) | |
H28 | 0.6194 | 0.0944 | 0.5737 | 0.062* | |
C29 | 0.5983 (5) | 0.0451 (3) | 0.5246 (6) | 0.053 (3) | |
H29 | 0.6478 | 0.0382 | 0.5487 | 0.064* | |
C30 | 0.5458 (5) | 0.0215 (2) | 0.4755 (6) | 0.043 (2) | |
H31 | 0.5586 | −0.0017 | 0.4664 | 0.052* | |
C31 | 0.4219 (5) | −0.0249 (2) | 0.3148 (6) | 0.041 (2) | |
C32 | 0.3928 (5) | −0.0152 (2) | 0.2352 (6) | 0.044 (2) | |
H32 | 0.3622 | 0.0052 | 0.2136 | 0.053* | |
C33 | 0.4101 (6) | −0.0365 (3) | 0.1888 (6) | 0.050 (3) | |
H33 | 0.3899 | −0.0304 | 0.1341 | 0.06* | |
C34 | 0.4545 (6) | −0.0655 (3) | 0.2173 (7) | 0.056 (3) | |
H34 | 0.4646 | −0.0794 | 0.183 | 0.067* | |
C35 | 0.4845 (6) | −0.0746 (2) | 0.2964 (6) | 0.048 (2) | |
H35 | 0.5166 | −0.0946 | 0.3173 | 0.058* | |
C36 | 0.4682 (5) | −0.0549 (2) | 0.3454 (7) | 0.048 (2) | |
H36 | 0.4882 | −0.0615 | 0.3997 | 0.057* | |
Co2 | 0.01776 (7) | 0.30892 (3) | 0.23069 (7) | 0.0365 (3) | |
Cl3 | 0.06155 (13) | 0.35607 (8) | 0.19555 (17) | 0.0569 (7) | |
Cl4 | −0.04817 (15) | 0.26942 (8) | 0.13493 (17) | 0.0672 (8) | |
P3 | 0.17372 (12) | 0.27415 (6) | 0.37669 (14) | 0.0351 (5) | |
P4 | −0.07134 (12) | 0.32353 (6) | 0.32534 (14) | 0.0345 (5) | |
O3 | 0.0947 (3) | 0.28277 (16) | 0.3247 (4) | 0.0406 (14) | |
O4 | −0.0449 (3) | 0.32921 (16) | 0.2674 (4) | 0.0430 (15) | |
C37 | 0.1849 (4) | 0.2401 (2) | 0.4476 (5) | 0.0331 (19) | |
C38 | 0.1271 (5) | 0.2343 (2) | 0.4603 (6) | 0.048 (2) | |
H38 | 0.0823 | 0.2464 | 0.4285 | 0.057* | |
C39 | 0.1356 (5) | 0.2102 (2) | 0.5207 (6) | 0.045 (2) | |
H39 | 0.0969 | 0.2065 | 0.5306 | 0.054* | |
C40 | 0.2018 (6) | 0.1919 (2) | 0.5662 (6) | 0.049 (2) | |
H40 | 0.2077 | 0.1755 | 0.6065 | 0.059* | |
C41 | 0.2579 (5) | 0.1979 (3) | 0.5521 (6) | 0.046 (2) | |
H41 | 0.3027 | 0.1856 | 0.583 | 0.055* | |
C42 | 0.2496 (5) | 0.2215 (2) | 0.4934 (6) | 0.046 (2) | |
H42 | 0.2887 | 0.2251 | 0.484 | 0.055* | |
C43 | 0.2250 (5) | 0.3121 (2) | 0.4345 (6) | 0.038 (2) | |
C44 | 0.2598 (5) | 0.3127 (2) | 0.5178 (6) | 0.042 (2) | |
H44 | 0.2603 | 0.2918 | 0.5459 | 0.05* | |
C45 | 0.2929 (5) | 0.3431 (3) | 0.5586 (7) | 0.053 (3) | |
H45 | 0.3159 | 0.3431 | 0.6151 | 0.063* | |
C46 | 0.2939 (5) | 0.3742 (3) | 0.5196 (7) | 0.050 (3) | |
H46 | 0.3156 | 0.3955 | 0.5489 | 0.06* | |
C47 | 0.2625 (6) | 0.3738 (2) | 0.4366 (7) | 0.052 (3) | |
H47 | 0.2645 | 0.3945 | 0.4091 | 0.063* | |
C48 | 0.2278 (5) | 0.3421 (2) | 0.3944 (6) | 0.043 (2) | |
H48 | 0.2061 | 0.3415 | 0.3381 | 0.052* | |
C49 | 0.2130 (5) | 0.2594 (2) | 0.3191 (5) | 0.035 (2) | |
C50 | 0.1683 (6) | 0.2418 (3) | 0.2482 (6) | 0.051 (3) | |
H50 | 0.1184 | 0.2386 | 0.2308 | 0.061* | |
C51 | 0.1966 (6) | 0.2289 (3) | 0.2020 (6) | 0.058 (3) | |
H51 | 0.1664 | 0.2161 | 0.1541 | 0.069* | |
C52 | 0.2690 (6) | 0.2347 (3) | 0.2264 (7) | 0.055 (3) | |
H52 | 0.2881 | 0.2262 | 0.1947 | 0.066* | |
C53 | 0.3138 (6) | 0.2529 (3) | 0.2971 (7) | 0.052 (3) | |
H53 | 0.3633 | 0.2569 | 0.3133 | 0.063* | |
C54 | 0.2863 (5) | 0.2651 (2) | 0.3438 (6) | 0.047 (2) | |
H55 | 0.317 | 0.2773 | 0.3925 | 0.057* | |
C55 | −0.0763 (5) | 0.2771 (2) | 0.3463 (6) | 0.042 (2) | |
C56 | −0.1099 (6) | 0.2535 (3) | 0.2799 (8) | 0.067 (3) | |
H56 | −0.1265 | 0.2622 | 0.2275 | 0.08* | |
C57 | −0.1180 (8) | 0.2177 (3) | 0.2927 (11) | 0.088 (5) | |
H57 | −0.1397 | 0.2017 | 0.2486 | 0.106* | |
C58 | −0.0958 (8) | 0.2051 (3) | 0.3663 (13) | 0.093 (6) | |
H58 | −0.103 | 0.1804 | 0.3735 | 0.112* | |
C59 | −0.0631 (7) | 0.2274 (4) | 0.4309 (10) | 0.079 (4) | |
H59 | −0.0474 | 0.2181 | 0.4827 | 0.095* | |
C60 | −0.0523 (6) | 0.2640 (3) | 0.4216 (8) | 0.063 (3) | |
H60 | −0.0289 | 0.2794 | 0.4667 | 0.076* | |
C61 | −0.1606 (5) | 0.3421 (2) | 0.2862 (5) | 0.039 (2) | |
C62 | −0.2135 (5) | 0.3264 (3) | 0.2978 (6) | 0.052 (3) | |
H62 | −0.2043 | 0.3041 | 0.3251 | 0.062* | |
C63 | −0.2791 (6) | 0.3432 (4) | 0.2699 (7) | 0.072 (4) | |
H63 | −0.3145 | 0.3326 | 0.2794 | 0.086* | |
C64 | −0.2942 (7) | 0.3742 (4) | 0.2291 (7) | 0.072 (4) | |
H64 | −0.3402 | 0.3853 | 0.2098 | 0.086* | |
C65 | −0.2426 (7) | 0.3904 (3) | 0.2151 (7) | 0.067 (3) | |
H65 | −0.2527 | 0.4125 | 0.1871 | 0.08* | |
C66 | −0.1771 (6) | 0.3736 (3) | 0.2424 (6) | 0.050 (2) | |
H66 | −0.1425 | 0.3838 | 0.2311 | 0.06* | |
C67 | −0.0137 (5) | 0.3467 (2) | 0.4187 (6) | 0.040 (2) | |
C68 | −0.0408 (5) | 0.3602 (3) | 0.4641 (6) | 0.045 (2) | |
H68 | −0.0907 | 0.3571 | 0.4469 | 0.054* | |
C69 | 0.0034 (6) | 0.3782 (3) | 0.5342 (7) | 0.058 (3) | |
H69 | −0.0154 | 0.3873 | 0.5658 | 0.069* | |
C70 | 0.0753 (6) | 0.3828 (3) | 0.5573 (7) | 0.066 (3) | |
H70 | 0.1062 | 0.3956 | 0.605 | 0.079* | |
C71 | 0.1034 (6) | 0.3690 (3) | 0.5124 (8) | 0.069 (3) | |
H71 | 0.1534 | 0.3719 | 0.5297 | 0.083* | |
C72 | 0.0586 (5) | 0.3512 (3) | 0.4426 (7) | 0.056 (3) | |
H72 | 0.0772 | 0.3421 | 0.411 | 0.067* | |
Co3 | 0.76086 (7) | 0.06559 (3) | 0.23091 (7) | 0.0396 (3) | |
Cl5 | 0.82120 (15) | 0.11451 (7) | 0.2284 (2) | 0.0675 (9) | |
Cl6 | 0.69939 (19) | 0.03291 (11) | 0.1209 (2) | 0.1013 (14) | |
P5 | 0.91512 (12) | 0.02897 (6) | 0.36261 (14) | 0.0328 (5) | |
P6 | 0.67019 (12) | 0.07520 (6) | 0.32416 (14) | 0.0355 (5) | |
O5 | 0.8341 (3) | 0.03541 (15) | 0.3196 (4) | 0.0379 (14) | |
O6 | 0.6915 (3) | 0.08228 (16) | 0.2624 (4) | 0.0420 (15) | |
C73 | 0.9351 (5) | −0.0082 (2) | 0.4286 (5) | 0.038 (2) | |
C74 | 0.8812 (6) | −0.0227 (3) | 0.4394 (6) | 0.052 (3) | |
H74 | 0.8335 | −0.0132 | 0.4095 | 0.062* | |
C75 | 0.8941 (8) | −0.0505 (3) | 0.4920 (8) | 0.074 (4) | |
H75 | 0.8563 | −0.0604 | 0.4985 | 0.089* | |
C76 | 0.9645 (9) | −0.0635 (3) | 0.5350 (7) | 0.075 (4) | |
H76 | 0.9746 | −0.0825 | 0.5719 | 0.09* | |
C77 | 1.0200 (8) | −0.0503 (3) | 0.5267 (7) | 0.072 (4) | |
H77 | 1.0675 | −0.0601 | 0.5567 | 0.086* | |
C78 | 1.0055 (6) | −0.0223 (3) | 0.4735 (7) | 0.056 (3) | |
H78 | 1.0435 | −0.0125 | 0.4675 | 0.067* | |
C79 | 0.9670 (4) | 0.0655 (2) | 0.4244 (5) | 0.0337 (19) | |
C80 | 0.9860 (5) | 0.0675 (2) | 0.5044 (5) | 0.039 (2) | |
H80 | 0.9744 | 0.0482 | 0.528 | 0.047* | |
C81 | 1.0210 (6) | 0.0969 (3) | 0.5488 (6) | 0.052 (3) | |
H81 | 1.0332 | 0.0978 | 0.603 | 0.062* | |
C82 | 1.0392 (5) | 0.1256 (2) | 0.5168 (6) | 0.046 (2) | |
H82 | 1.0649 | 0.1456 | 0.5491 | 0.055* | |
C83 | 1.0194 (5) | 0.1246 (2) | 0.4374 (6) | 0.040 (2) | |
H83 | 1.0304 | 0.1444 | 0.4145 | 0.048* | |
C84 | 0.9836 (5) | 0.0949 (2) | 0.3908 (5) | 0.038 (2) | |
H84 | 0.9703 | 0.0945 | 0.3362 | 0.046* | |
C85 | 0.9460 (5) | 0.0185 (2) | 0.2945 (5) | 0.0338 (19) | |
C86 | 0.8947 (5) | 0.0094 (3) | 0.2162 (6) | 0.046 (2) | |
H86 | 0.8445 | 0.0096 | 0.1991 | 0.055* | |
C87 | 0.9178 (6) | 0.0002 (3) | 0.1632 (6) | 0.055 (3) | |
H87 | 0.883 | −0.0063 | 0.1101 | 0.067* | |
C88 | 0.9902 (6) | 0.0004 (3) | 0.1865 (6) | 0.050 (3) | |
H88 | 1.0053 | −0.0054 | 0.1495 | 0.061* | |
C89 | 1.0407 (6) | 0.0091 (2) | 0.2641 (6) | 0.044 (2) | |
H89 | 1.0909 | 0.0082 | 0.2812 | 0.053* | |
C90 | 1.0187 (5) | 0.0191 (2) | 0.3171 (6) | 0.040 (2) | |
H90 | 1.0538 | 0.0265 | 0.3695 | 0.048* | |
C91 | 0.5798 (4) | 0.0913 (2) | 0.2897 (5) | 0.0346 (19) | |
C92 | 0.5616 (5) | 0.1253 (2) | 0.2527 (6) | 0.049 (2) | |
H92 | 0.596 | 0.1385 | 0.2455 | 0.059* | |
C93 | 0.4935 (5) | 0.1395 (2) | 0.2269 (6) | 0.045 (2) | |
H93 | 0.4812 | 0.1624 | 0.2021 | 0.054* | |
C94 | 0.4431 (5) | 0.1204 (3) | 0.2370 (6) | 0.053 (3) | |
H94 | 0.3963 | 0.1303 | 0.2191 | 0.064* | |
C95 | 0.4602 (5) | 0.0876 (3) | 0.2725 (7) | 0.057 (3) | |
H95 | 0.4252 | 0.0747 | 0.2791 | 0.069* | |
C96 | 0.5290 (5) | 0.0725 (3) | 0.2996 (6) | 0.046 (2) | |
H96 | 0.5406 | 0.0496 | 0.3247 | 0.056* | |
C97 | 0.7287 (5) | 0.0986 (3) | 0.4149 (6) | 0.043 (2) | |
C98 | 0.7045 (6) | 0.1095 (3) | 0.4662 (6) | 0.059 (3) | |
H98 | 0.6567 | 0.1037 | 0.4542 | 0.071* | |
C99 | 0.7508 (6) | 0.1289 (3) | 0.5354 (7) | 0.068 (3) | |
H99 | 0.7339 | 0.1365 | 0.5698 | 0.081* | |
C100 | 0.8202 (6) | 0.1371 (3) | 0.5540 (7) | 0.066 (3) | |
H100 | 0.8518 | 0.1497 | 0.6018 | 0.079* | |
C101 | 0.8438 (6) | 0.1268 (3) | 0.5018 (8) | 0.072 (4) | |
H101 | 0.891 | 0.1332 | 0.5131 | 0.086* | |
C102 | 0.7993 (5) | 0.1073 (3) | 0.4343 (6) | 0.051 (3) | |
H102 | 0.8169 | 0.0996 | 0.4005 | 0.061* | |
C103 | 0.6704 (5) | 0.0288 (3) | 0.3438 (7) | 0.054 (3) | |
C104 | 0.6970 (7) | 0.0140 (3) | 0.4187 (9) | 0.073 (4) | |
H104 | 0.7208 | 0.029 | 0.4644 | 0.088* | |
C105 | 0.6894 (10) | −0.0224 (5) | 0.4279 (15) | 0.123 (8) | |
H105 | 0.707 | −0.0318 | 0.4799 | 0.147* | |
C106 | 0.6571 (11) | −0.0450 (4) | 0.3638 (17) | 0.124 (9) | |
H106 | 0.6524 | −0.07 | 0.3707 | 0.149* | |
C107 | 0.6317 (8) | −0.0307 (3) | 0.2894 (13) | 0.103 (6) | |
H107 | 0.6096 | −0.0462 | 0.2444 | 0.123* | |
C108 | 0.6372 (6) | 0.0056 (3) | 0.2777 (9) | 0.069 (4) | |
H208 | 0.6187 | 0.0147 | 0.2253 | 0.083* | |
Co4 | 0.48535 (7) | 0.28576 (3) | 0.22196 (7) | 0.0389 (3) | |
Cl7 | 0.42672 (15) | 0.23383 (7) | 0.20164 (19) | 0.0641 (8) | |
Cl8 | 0.50554 (17) | 0.31232 (9) | 0.13040 (18) | 0.0708 (9) | |
P7 | 0.44717 (12) | 0.35044 (6) | 0.31112 (14) | 0.0324 (5) | |
P8 | 0.64544 (12) | 0.25569 (6) | 0.36922 (14) | 0.0354 (5) | |
O7 | 0.4355 (3) | 0.32189 (15) | 0.2500 (4) | 0.0372 (14) | |
O8 | 0.5810 (3) | 0.27918 (15) | 0.3206 (4) | 0.0392 (14) | |
C109 | 0.5199 (4) | 0.3800 (2) | 0.3309 (6) | 0.037 (2) | |
C110 | 0.5265 (5) | 0.3927 (2) | 0.2679 (6) | 0.044 (2) | |
H110 | 0.4948 | 0.384 | 0.2156 | 0.053* | |
C111 | 0.5782 (6) | 0.4178 (2) | 0.2796 (7) | 0.052 (3) | |
H111 | 0.5812 | 0.4266 | 0.2355 | 0.062* | |
C112 | 0.6262 (5) | 0.4304 (2) | 0.3560 (6) | 0.044 (2) | |
H112 | 0.6622 | 0.4477 | 0.3645 | 0.053* | |
C113 | 0.6207 (5) | 0.4176 (3) | 0.4186 (6) | 0.051 (2) | |
H113 | 0.6539 | 0.4259 | 0.4709 | 0.061* | |
C114 | 0.5688 (5) | 0.3932 (2) | 0.4082 (6) | 0.045 (2) | |
H114 | 0.5656 | 0.385 | 0.4526 | 0.054* | |
C115 | 0.3671 (5) | 0.3770 (2) | 0.2760 (5) | 0.0341 (19) | |
C116 | 0.3018 (5) | 0.3588 (3) | 0.2486 (6) | 0.051 (3) | |
H116 | 0.3011 | 0.3333 | 0.2458 | 0.061* | |
C117 | 0.2384 (5) | 0.3771 (3) | 0.2256 (6) | 0.058 (3) | |
H117 | 0.1941 | 0.3646 | 0.2084 | 0.069* | |
C118 | 0.2408 (6) | 0.4149 (4) | 0.2282 (7) | 0.068 (3) | |
H118 | 0.1973 | 0.428 | 0.2115 | 0.081* | |
C119 | 0.3041 (6) | 0.4331 (3) | 0.2540 (7) | 0.071 (4) | |
H119 | 0.3046 | 0.4586 | 0.2557 | 0.086* | |
C120 | 0.3672 (5) | 0.4142 (3) | 0.2777 (6) | 0.051 (3) | |
H120 | 0.4113 | 0.4269 | 0.2955 | 0.061* | |
C121 | 0.4630 (5) | 0.3306 (2) | 0.4026 (5) | 0.037 (2) | |
C122 | 0.4421 (6) | 0.3481 (3) | 0.4511 (6) | 0.051 (3) | |
H122 | 0.4188 | 0.3709 | 0.4355 | 0.062* | |
C123 | 0.4548 (6) | 0.3328 (3) | 0.5211 (6) | 0.059 (3) | |
H123 | 0.441 | 0.3452 | 0.5542 | 0.07* | |
C124 | 0.4875 (6) | 0.2994 (3) | 0.5439 (6) | 0.054 (3) | |
H124 | 0.4957 | 0.2888 | 0.5923 | 0.065* | |
C125 | 0.5077 (6) | 0.2819 (3) | 0.4973 (7) | 0.055 (3) | |
H125 | 0.5291 | 0.2588 | 0.5124 | 0.066* | |
C126 | 0.4972 (5) | 0.2978 (3) | 0.4272 (6) | 0.050 (2) | |
H126 | 0.5137 | 0.2858 | 0.3961 | 0.06* | |
C127 | 0.7198 (5) | 0.2838 (2) | 0.4323 (6) | 0.041 (2) | |
C128 | 0.7929 (5) | 0.2735 (3) | 0.4630 (6) | 0.049 (2) | |
H128 | 0.8041 | 0.251 | 0.4485 | 0.059* | |
C129 | 0.8482 (5) | 0.2966 (3) | 0.5148 (6) | 0.056 (3) | |
H129 | 0.8975 | 0.29 | 0.5358 | 0.067* | |
C130 | 0.8314 (6) | 0.3288 (3) | 0.5354 (7) | 0.061 (3) | |
H130 | 0.8697 | 0.3441 | 0.5712 | 0.074* | |
C131 | 0.7620 (6) | 0.3398 (3) | 0.5066 (7) | 0.058 (3) | |
H131 | 0.752 | 0.3624 | 0.5214 | 0.07* | |
C132 | 0.7050 (6) | 0.3170 (2) | 0.4546 (6) | 0.051 (3) | |
H132 | 0.6562 | 0.3242 | 0.4344 | 0.061* | |
C133 | 0.6312 (5) | 0.2253 (2) | 0.4311 (5) | 0.036 (2) | |
C134 | 0.6720 (6) | 0.2265 (3) | 0.5137 (7) | 0.057 (3) | |
H134 | 0.7114 | 0.2429 | 0.539 | 0.069* | |
C135 | 0.6555 (7) | 0.2037 (3) | 0.5608 (7) | 0.059 (3) | |
H135 | 0.6831 | 0.2048 | 0.6173 | 0.071* | |
C136 | 0.5987 (6) | 0.1799 (3) | 0.5228 (7) | 0.056 (3) | |
H136 | 0.5869 | 0.1646 | 0.5537 | 0.067* | |
C137 | 0.5591 (6) | 0.1779 (3) | 0.4420 (7) | 0.052 (3) | |
H137 | 0.5208 | 0.1609 | 0.4171 | 0.063* | |
C138 | 0.5747 (5) | 0.2006 (3) | 0.3955 (6) | 0.048 (2) | |
H138 | 0.5465 | 0.1992 | 0.339 | 0.057* | |
C139 | 0.6676 (5) | 0.2291 (2) | 0.3075 (6) | 0.041 (2) | |
C140 | 0.7062 (5) | 0.1967 (2) | 0.3335 (6) | 0.044 (2) | |
H140 | 0.7214 | 0.1878 | 0.3855 | 0.053* | |
C141 | 0.7218 (5) | 0.1778 (3) | 0.2829 (7) | 0.051 (3) | |
H141 | 0.7489 | 0.1562 | 0.3013 | 0.061* | |
C142 | 0.6994 (6) | 0.1893 (3) | 0.2076 (7) | 0.057 (3) | |
H142 | 0.7092 | 0.1754 | 0.1731 | 0.068* | |
C143 | 0.6619 (7) | 0.2216 (3) | 0.1815 (8) | 0.071 (3) | |
H143 | 0.6481 | 0.2306 | 0.13 | 0.085* | |
C144 | 0.6445 (5) | 0.2409 (3) | 0.2310 (6) | 0.052 (3) | |
H144 | 0.6165 | 0.2623 | 0.212 | 0.062* | |
O9 | 0.2083 (19) | 0.1418 (9) | 0.141 (2) | 0.182 (13)* | 0.5 |
H9B | 0.2214 | 0.1258 | 0.1203 | 0.273* | 0.5 |
C145 | 0.1384 (16) | 0.1371 (8) | 0.1174 (18) | 0.092 (9)* | 0.5 |
H145 | 0.1321 | 0.1375 | 0.164 | 0.137* | 0.5 |
H146 | 0.1219 | 0.114 | 0.09 | 0.137* | 0.5 |
H147 | 0.1099 | 0.1566 | 0.0809 | 0.137* | 0.5 |
U11 | U22 | U33 | U12 | U13 | U23 | |
Co1 | 0.0318 (6) | 0.0354 (6) | 0.0301 (7) | −0.0017 (5) | 0.0175 (6) | −0.0032 (5) |
Cl1 | 0.0483 (13) | 0.0395 (12) | 0.0559 (16) | −0.0099 (10) | 0.0330 (13) | −0.0090 (11) |
Cl2 | 0.0563 (15) | 0.0641 (15) | 0.0385 (14) | −0.0011 (12) | 0.0296 (12) | 0.0077 (12) |
P1 | 0.0358 (12) | 0.0332 (11) | 0.0361 (14) | 0.0030 (9) | 0.0205 (11) | −0.0025 (10) |
P2 | 0.0320 (12) | 0.0363 (12) | 0.0337 (13) | −0.0013 (9) | 0.0167 (11) | −0.0003 (10) |
O1 | 0.058 (4) | 0.041 (3) | 0.031 (4) | 0.008 (3) | 0.026 (3) | −0.003 (3) |
O2 | 0.036 (3) | 0.045 (3) | 0.030 (4) | 0.006 (3) | 0.014 (3) | 0.003 (3) |
C1 | 0.034 (5) | 0.026 (4) | 0.036 (5) | −0.005 (3) | 0.017 (4) | 0.000 (4) |
C2 | 0.044 (5) | 0.028 (4) | 0.036 (5) | −0.002 (4) | 0.017 (5) | 0.000 (4) |
C3 | 0.041 (5) | 0.052 (6) | 0.036 (6) | 0.001 (4) | 0.014 (5) | 0.008 (5) |
C4 | 0.032 (5) | 0.064 (6) | 0.036 (6) | 0.009 (4) | 0.016 (5) | −0.004 (5) |
C5 | 0.044 (5) | 0.041 (5) | 0.046 (6) | 0.010 (4) | 0.021 (5) | −0.009 (4) |
C6 | 0.040 (5) | 0.038 (5) | 0.051 (6) | 0.005 (4) | 0.022 (5) | −0.001 (4) |
C7 | 0.036 (5) | 0.036 (5) | 0.033 (5) | −0.003 (4) | 0.016 (4) | −0.009 (4) |
C8 | 0.040 (5) | 0.044 (5) | 0.037 (6) | 0.007 (4) | 0.019 (4) | 0.003 (4) |
C9 | 0.062 (7) | 0.054 (6) | 0.049 (7) | 0.010 (5) | 0.032 (6) | 0.011 (5) |
C10 | 0.044 (6) | 0.057 (6) | 0.038 (6) | 0.005 (5) | 0.019 (5) | 0.014 (5) |
C11 | 0.043 (5) | 0.072 (7) | 0.027 (5) | 0.007 (5) | 0.020 (5) | −0.007 (5) |
C12 | 0.036 (5) | 0.048 (5) | 0.025 (5) | −0.001 (4) | 0.015 (4) | 0.000 (4) |
C13 | 0.035 (5) | 0.034 (5) | 0.055 (7) | 0.006 (4) | 0.020 (5) | 0.000 (4) |
C14 | 0.051 (7) | 0.056 (7) | 0.090 (10) | 0.002 (5) | 0.025 (7) | 0.029 (6) |
C15 | 0.042 (7) | 0.067 (8) | 0.157 (16) | −0.002 (6) | 0.046 (9) | 0.038 (9) |
C16 | 0.049 (8) | 0.044 (7) | 0.20 (2) | −0.012 (6) | 0.058 (11) | −0.036 (10) |
C17 | 0.047 (7) | 0.093 (10) | 0.131 (14) | −0.026 (7) | 0.043 (8) | −0.063 (10) |
C18 | 0.050 (6) | 0.073 (7) | 0.070 (8) | −0.011 (5) | 0.036 (6) | −0.029 (6) |
C19 | 0.033 (5) | 0.042 (5) | 0.038 (6) | 0.001 (4) | 0.018 (4) | −0.004 (4) |
C20 | 0.055 (6) | 0.044 (5) | 0.043 (6) | −0.009 (4) | 0.026 (5) | −0.005 (4) |
C21 | 0.070 (7) | 0.049 (6) | 0.039 (6) | 0.003 (5) | 0.029 (6) | 0.007 (5) |
C22 | 0.059 (6) | 0.048 (6) | 0.045 (7) | 0.002 (5) | 0.035 (6) | 0.002 (5) |
C23 | 0.050 (6) | 0.035 (5) | 0.069 (8) | 0.004 (4) | 0.031 (6) | 0.001 (5) |
C24 | 0.034 (5) | 0.045 (5) | 0.047 (6) | 0.001 (4) | 0.020 (5) | 0.001 (4) |
C25 | 0.033 (5) | 0.033 (4) | 0.040 (5) | −0.004 (4) | 0.019 (4) | 0.002 (4) |
C26 | 0.039 (5) | 0.041 (5) | 0.053 (7) | 0.005 (4) | 0.016 (5) | −0.002 (5) |
C27 | 0.057 (7) | 0.040 (5) | 0.057 (7) | −0.002 (5) | 0.021 (6) | −0.006 (5) |
C28 | 0.041 (6) | 0.052 (6) | 0.052 (7) | −0.010 (5) | 0.015 (5) | −0.011 (5) |
C29 | 0.025 (5) | 0.070 (7) | 0.056 (7) | −0.001 (5) | 0.015 (5) | 0.008 (6) |
C30 | 0.036 (5) | 0.043 (5) | 0.054 (7) | 0.000 (4) | 0.025 (5) | −0.007 (4) |
C31 | 0.037 (5) | 0.037 (5) | 0.054 (6) | −0.004 (4) | 0.027 (5) | 0.003 (4) |
C32 | 0.056 (6) | 0.040 (5) | 0.040 (6) | −0.002 (4) | 0.027 (5) | −0.001 (4) |
C33 | 0.069 (7) | 0.051 (6) | 0.038 (6) | 0.009 (5) | 0.032 (6) | −0.003 (5) |
C34 | 0.069 (7) | 0.045 (6) | 0.077 (9) | −0.011 (5) | 0.054 (7) | −0.021 (5) |
C35 | 0.067 (7) | 0.039 (5) | 0.055 (7) | 0.008 (5) | 0.043 (6) | −0.005 (5) |
C36 | 0.052 (6) | 0.035 (5) | 0.058 (7) | −0.005 (4) | 0.029 (5) | 0.008 (4) |
Co2 | 0.0325 (6) | 0.0449 (7) | 0.0299 (7) | 0.0057 (5) | 0.0141 (6) | −0.0008 (6) |
Cl3 | 0.0447 (14) | 0.0758 (18) | 0.0555 (17) | 0.0080 (12) | 0.0293 (13) | 0.0252 (14) |
Cl4 | 0.0619 (17) | 0.0652 (17) | 0.0473 (17) | 0.0146 (14) | 0.0075 (14) | −0.0203 (14) |
P3 | 0.0319 (12) | 0.0365 (12) | 0.0332 (14) | −0.0005 (9) | 0.0138 (11) | 0.0022 (10) |
P4 | 0.0347 (12) | 0.0348 (12) | 0.0385 (14) | 0.0056 (9) | 0.0217 (11) | 0.0027 (10) |
O3 | 0.026 (3) | 0.052 (4) | 0.034 (4) | 0.006 (3) | 0.008 (3) | 0.007 (3) |
O4 | 0.041 (4) | 0.044 (4) | 0.049 (4) | 0.005 (3) | 0.027 (3) | 0.001 (3) |
C37 | 0.035 (5) | 0.028 (4) | 0.032 (5) | −0.001 (3) | 0.014 (4) | −0.003 (4) |
C38 | 0.038 (5) | 0.047 (5) | 0.055 (7) | −0.002 (4) | 0.020 (5) | 0.001 (5) |
C39 | 0.051 (6) | 0.034 (5) | 0.050 (6) | −0.007 (4) | 0.026 (5) | 0.004 (4) |
C40 | 0.060 (6) | 0.042 (5) | 0.046 (6) | 0.003 (5) | 0.028 (5) | 0.016 (5) |
C41 | 0.042 (5) | 0.049 (6) | 0.039 (6) | 0.007 (4) | 0.013 (5) | 0.006 (5) |
C42 | 0.040 (5) | 0.044 (5) | 0.060 (7) | −0.005 (4) | 0.031 (5) | 0.002 (5) |
C43 | 0.035 (5) | 0.037 (5) | 0.041 (6) | 0.002 (4) | 0.017 (4) | 0.000 (4) |
C44 | 0.045 (5) | 0.036 (5) | 0.041 (6) | −0.010 (4) | 0.019 (5) | 0.003 (4) |
C45 | 0.050 (6) | 0.055 (6) | 0.046 (7) | −0.012 (5) | 0.019 (5) | −0.001 (5) |
C46 | 0.040 (5) | 0.050 (6) | 0.055 (7) | −0.009 (4) | 0.020 (5) | −0.008 (5) |
C47 | 0.059 (6) | 0.032 (5) | 0.055 (7) | −0.003 (4) | 0.021 (6) | 0.008 (5) |
C48 | 0.048 (6) | 0.036 (5) | 0.036 (6) | −0.007 (4) | 0.014 (5) | 0.004 (4) |
C49 | 0.034 (5) | 0.033 (4) | 0.037 (5) | −0.003 (4) | 0.017 (4) | 0.008 (4) |
C50 | 0.046 (6) | 0.069 (7) | 0.033 (6) | −0.001 (5) | 0.017 (5) | 0.008 (5) |
C51 | 0.063 (7) | 0.070 (7) | 0.035 (6) | −0.003 (6) | 0.021 (6) | −0.005 (5) |
C52 | 0.074 (8) | 0.049 (6) | 0.056 (7) | 0.011 (5) | 0.044 (6) | 0.003 (5) |
C53 | 0.050 (6) | 0.059 (6) | 0.060 (7) | −0.007 (5) | 0.036 (6) | −0.006 (5) |
C54 | 0.044 (5) | 0.042 (5) | 0.052 (7) | 0.000 (4) | 0.021 (5) | −0.010 (5) |
C55 | 0.033 (5) | 0.047 (5) | 0.053 (7) | 0.012 (4) | 0.026 (5) | 0.017 (5) |
C56 | 0.068 (8) | 0.055 (7) | 0.096 (10) | −0.007 (6) | 0.056 (8) | −0.011 (6) |
C57 | 0.101 (11) | 0.034 (6) | 0.168 (17) | −0.010 (6) | 0.097 (12) | 0.000 (8) |
C58 | 0.079 (10) | 0.041 (7) | 0.19 (2) | 0.010 (7) | 0.087 (12) | 0.024 (10) |
C59 | 0.061 (8) | 0.068 (8) | 0.131 (13) | 0.031 (6) | 0.066 (9) | 0.063 (9) |
C60 | 0.047 (6) | 0.068 (7) | 0.082 (9) | 0.025 (5) | 0.039 (6) | 0.029 (6) |
C61 | 0.044 (5) | 0.036 (5) | 0.036 (6) | 0.002 (4) | 0.019 (5) | −0.006 (4) |
C62 | 0.043 (6) | 0.066 (7) | 0.055 (7) | 0.008 (5) | 0.031 (5) | 0.002 (5) |
C63 | 0.038 (6) | 0.130 (11) | 0.045 (7) | 0.031 (7) | 0.019 (5) | 0.010 (7) |
C64 | 0.061 (8) | 0.090 (9) | 0.038 (7) | 0.039 (7) | 0.005 (6) | −0.010 (6) |
C65 | 0.069 (8) | 0.050 (6) | 0.049 (8) | 0.020 (6) | 0.006 (6) | −0.001 (5) |
C66 | 0.059 (7) | 0.044 (6) | 0.036 (6) | −0.004 (5) | 0.016 (5) | −0.004 (4) |
C67 | 0.039 (5) | 0.038 (5) | 0.041 (6) | 0.009 (4) | 0.019 (5) | −0.002 (4) |
C68 | 0.035 (5) | 0.060 (6) | 0.042 (6) | −0.002 (4) | 0.021 (5) | −0.010 (5) |
C69 | 0.055 (7) | 0.068 (7) | 0.050 (7) | 0.002 (5) | 0.027 (6) | −0.003 (5) |
C70 | 0.040 (6) | 0.093 (9) | 0.053 (8) | −0.010 (6) | 0.015 (6) | −0.021 (6) |
C71 | 0.043 (6) | 0.096 (9) | 0.067 (9) | −0.005 (6) | 0.027 (6) | −0.002 (7) |
C72 | 0.037 (5) | 0.078 (7) | 0.060 (7) | −0.006 (5) | 0.029 (5) | −0.012 (6) |
Co3 | 0.0364 (7) | 0.0501 (7) | 0.0321 (7) | 0.0050 (6) | 0.0171 (6) | −0.0008 (6) |
Cl5 | 0.0636 (17) | 0.0620 (16) | 0.099 (2) | 0.0163 (13) | 0.0573 (18) | 0.0358 (16) |
Cl6 | 0.073 (2) | 0.132 (3) | 0.056 (2) | 0.029 (2) | 0.0006 (17) | −0.048 (2) |
P5 | 0.0353 (12) | 0.0311 (11) | 0.0351 (14) | 0.0003 (9) | 0.0200 (11) | 0.0017 (10) |
P6 | 0.0339 (12) | 0.0391 (12) | 0.0366 (14) | 0.0018 (9) | 0.0201 (11) | −0.0001 (10) |
O5 | 0.035 (3) | 0.039 (3) | 0.041 (4) | 0.001 (3) | 0.020 (3) | 0.002 (3) |
O6 | 0.043 (4) | 0.050 (4) | 0.038 (4) | 0.001 (3) | 0.024 (3) | −0.001 (3) |
C73 | 0.047 (5) | 0.035 (5) | 0.033 (5) | −0.006 (4) | 0.021 (5) | −0.003 (4) |
C74 | 0.063 (7) | 0.045 (6) | 0.048 (7) | −0.015 (5) | 0.028 (6) | 0.002 (5) |
C75 | 0.089 (10) | 0.071 (8) | 0.056 (8) | −0.041 (7) | 0.032 (8) | −0.002 (7) |
C76 | 0.136 (13) | 0.041 (6) | 0.046 (7) | −0.018 (7) | 0.045 (9) | 0.005 (5) |
C77 | 0.102 (10) | 0.054 (7) | 0.058 (8) | 0.032 (7) | 0.040 (8) | 0.021 (6) |
C78 | 0.060 (7) | 0.053 (6) | 0.062 (8) | 0.019 (5) | 0.036 (6) | 0.023 (5) |
C79 | 0.029 (4) | 0.035 (4) | 0.040 (5) | 0.001 (3) | 0.020 (4) | 0.001 (4) |
C80 | 0.048 (5) | 0.040 (5) | 0.035 (5) | 0.001 (4) | 0.025 (5) | 0.010 (4) |
C81 | 0.069 (7) | 0.056 (6) | 0.034 (6) | −0.008 (5) | 0.029 (5) | −0.002 (5) |
C82 | 0.055 (6) | 0.041 (5) | 0.049 (7) | −0.010 (4) | 0.031 (5) | −0.006 (4) |
C83 | 0.046 (5) | 0.033 (5) | 0.045 (6) | −0.001 (4) | 0.027 (5) | 0.001 (4) |
C84 | 0.046 (5) | 0.044 (5) | 0.031 (5) | −0.001 (4) | 0.025 (4) | −0.004 (4) |
C85 | 0.042 (5) | 0.032 (4) | 0.031 (5) | −0.006 (4) | 0.020 (4) | 0.003 (4) |
C86 | 0.045 (5) | 0.055 (6) | 0.039 (6) | 0.002 (4) | 0.023 (5) | −0.009 (5) |
C87 | 0.065 (7) | 0.066 (7) | 0.039 (6) | 0.008 (5) | 0.030 (6) | −0.012 (5) |
C88 | 0.068 (7) | 0.053 (6) | 0.046 (7) | 0.011 (5) | 0.041 (6) | 0.001 (5) |
C89 | 0.059 (6) | 0.032 (5) | 0.059 (7) | −0.002 (4) | 0.043 (6) | −0.008 (4) |
C90 | 0.040 (5) | 0.043 (5) | 0.037 (6) | −0.005 (4) | 0.019 (4) | 0.000 (4) |
C91 | 0.031 (4) | 0.043 (5) | 0.030 (5) | −0.001 (4) | 0.016 (4) | 0.001 (4) |
C92 | 0.040 (5) | 0.046 (5) | 0.055 (7) | −0.006 (4) | 0.018 (5) | −0.001 (5) |
C93 | 0.043 (5) | 0.043 (5) | 0.038 (6) | 0.010 (4) | 0.013 (5) | −0.004 (4) |
C94 | 0.038 (5) | 0.075 (7) | 0.043 (6) | 0.007 (5) | 0.018 (5) | 0.000 (5) |
C95 | 0.036 (5) | 0.089 (8) | 0.053 (7) | 0.009 (5) | 0.027 (5) | 0.006 (6) |
C96 | 0.039 (5) | 0.058 (6) | 0.042 (6) | 0.003 (4) | 0.020 (5) | 0.004 (5) |
C97 | 0.040 (5) | 0.053 (6) | 0.037 (6) | −0.001 (4) | 0.020 (5) | 0.001 (4) |
C98 | 0.047 (6) | 0.101 (9) | 0.038 (6) | −0.005 (6) | 0.028 (5) | −0.010 (6) |
C99 | 0.056 (7) | 0.104 (9) | 0.042 (7) | −0.003 (6) | 0.023 (6) | −0.024 (6) |
C100 | 0.046 (6) | 0.098 (9) | 0.037 (7) | −0.004 (6) | 0.009 (5) | −0.014 (6) |
C101 | 0.041 (6) | 0.096 (9) | 0.078 (9) | −0.009 (6) | 0.030 (6) | −0.032 (7) |
C102 | 0.036 (5) | 0.062 (6) | 0.051 (7) | −0.005 (4) | 0.019 (5) | −0.017 (5) |
C103 | 0.048 (6) | 0.056 (6) | 0.076 (8) | 0.012 (5) | 0.044 (6) | 0.014 (6) |
C104 | 0.071 (8) | 0.069 (8) | 0.104 (11) | 0.022 (6) | 0.062 (8) | 0.032 (7) |
C105 | 0.118 (14) | 0.095 (12) | 0.22 (2) | 0.063 (11) | 0.137 (17) | 0.089 (14) |
C106 | 0.137 (16) | 0.054 (9) | 0.26 (3) | 0.039 (10) | 0.16 (2) | 0.058 (14) |
C107 | 0.087 (10) | 0.042 (7) | 0.22 (2) | −0.015 (6) | 0.110 (13) | −0.043 (10) |
C108 | 0.064 (7) | 0.046 (6) | 0.119 (11) | −0.010 (5) | 0.061 (8) | −0.026 (7) |
Co4 | 0.0401 (7) | 0.0434 (7) | 0.0331 (7) | 0.0064 (5) | 0.0183 (6) | −0.0018 (6) |
Cl7 | 0.0539 (16) | 0.0477 (14) | 0.077 (2) | −0.0043 (12) | 0.0226 (15) | −0.0216 (13) |
Cl8 | 0.079 (2) | 0.096 (2) | 0.0516 (18) | 0.0331 (17) | 0.0440 (17) | 0.0305 (16) |
P7 | 0.0341 (12) | 0.0315 (11) | 0.0331 (13) | 0.0011 (9) | 0.0180 (11) | −0.0017 (9) |
P8 | 0.0328 (12) | 0.0353 (12) | 0.0384 (14) | −0.0009 (9) | 0.0181 (11) | 0.0002 (10) |
O7 | 0.036 (3) | 0.036 (3) | 0.037 (4) | 0.003 (2) | 0.017 (3) | −0.002 (3) |
O8 | 0.031 (3) | 0.047 (3) | 0.039 (4) | 0.007 (3) | 0.017 (3) | 0.003 (3) |
C109 | 0.030 (5) | 0.038 (5) | 0.042 (6) | 0.004 (4) | 0.017 (4) | −0.007 (4) |
C110 | 0.055 (6) | 0.047 (5) | 0.044 (6) | 0.000 (4) | 0.035 (5) | 0.008 (4) |
C111 | 0.066 (7) | 0.041 (5) | 0.078 (9) | −0.002 (5) | 0.058 (7) | −0.001 (5) |
C112 | 0.039 (5) | 0.043 (5) | 0.053 (7) | 0.000 (4) | 0.025 (5) | −0.002 (5) |
C113 | 0.040 (5) | 0.064 (6) | 0.035 (6) | −0.008 (5) | 0.009 (5) | 0.000 (5) |
C114 | 0.039 (5) | 0.051 (6) | 0.041 (6) | −0.007 (4) | 0.017 (5) | −0.004 (5) |
C115 | 0.037 (5) | 0.040 (5) | 0.028 (5) | 0.005 (4) | 0.019 (4) | 0.004 (4) |
C116 | 0.039 (5) | 0.060 (6) | 0.053 (7) | 0.003 (5) | 0.023 (5) | 0.009 (5) |
C117 | 0.036 (6) | 0.100 (9) | 0.040 (7) | −0.001 (6) | 0.021 (5) | −0.001 (6) |
C118 | 0.046 (7) | 0.103 (10) | 0.045 (7) | 0.022 (6) | 0.016 (6) | −0.016 (7) |
C119 | 0.065 (8) | 0.058 (7) | 0.064 (8) | 0.022 (6) | 0.012 (6) | −0.023 (6) |
C120 | 0.043 (6) | 0.052 (6) | 0.042 (6) | 0.011 (4) | 0.010 (5) | −0.011 (5) |
C121 | 0.036 (5) | 0.041 (5) | 0.037 (5) | −0.004 (4) | 0.021 (4) | 0.006 (4) |
C122 | 0.074 (7) | 0.041 (5) | 0.051 (7) | 0.014 (5) | 0.040 (6) | 0.008 (5) |
C123 | 0.083 (8) | 0.062 (7) | 0.046 (7) | 0.017 (6) | 0.043 (6) | 0.012 (5) |
C124 | 0.061 (7) | 0.074 (7) | 0.034 (6) | −0.010 (5) | 0.029 (5) | 0.011 (5) |
C125 | 0.067 (7) | 0.039 (5) | 0.061 (7) | 0.003 (5) | 0.033 (6) | 0.011 (5) |
C126 | 0.057 (6) | 0.048 (6) | 0.050 (7) | 0.006 (5) | 0.031 (5) | 0.003 (5) |
C127 | 0.042 (5) | 0.041 (5) | 0.037 (6) | 0.000 (4) | 0.018 (5) | 0.006 (4) |
C128 | 0.044 (6) | 0.059 (6) | 0.037 (6) | 0.005 (5) | 0.015 (5) | 0.007 (5) |
C129 | 0.038 (6) | 0.081 (8) | 0.042 (6) | −0.008 (5) | 0.015 (5) | −0.008 (6) |
C130 | 0.052 (7) | 0.077 (8) | 0.045 (7) | −0.028 (6) | 0.017 (6) | −0.001 (6) |
C131 | 0.067 (8) | 0.044 (6) | 0.056 (7) | −0.011 (5) | 0.025 (6) | 0.003 (5) |
C132 | 0.057 (6) | 0.036 (5) | 0.052 (7) | −0.007 (4) | 0.022 (6) | 0.000 (5) |
C133 | 0.038 (5) | 0.039 (5) | 0.033 (5) | 0.003 (4) | 0.019 (4) | 0.001 (4) |
C134 | 0.064 (7) | 0.045 (6) | 0.064 (8) | −0.015 (5) | 0.034 (6) | −0.003 (5) |
C135 | 0.096 (9) | 0.037 (5) | 0.044 (7) | −0.010 (5) | 0.035 (6) | 0.003 (5) |
C136 | 0.064 (7) | 0.047 (6) | 0.064 (8) | 0.000 (5) | 0.038 (6) | 0.010 (5) |
C137 | 0.052 (6) | 0.052 (6) | 0.056 (7) | −0.009 (5) | 0.029 (6) | 0.000 (5) |
C138 | 0.038 (5) | 0.056 (6) | 0.048 (6) | −0.008 (4) | 0.020 (5) | 0.002 (5) |
C139 | 0.042 (5) | 0.039 (5) | 0.042 (6) | 0.000 (4) | 0.022 (5) | 0.002 (4) |
C140 | 0.047 (5) | 0.037 (5) | 0.055 (7) | 0.000 (4) | 0.030 (5) | −0.001 (4) |
C141 | 0.052 (6) | 0.040 (5) | 0.073 (8) | 0.002 (4) | 0.041 (6) | 0.000 (5) |
C142 | 0.057 (6) | 0.050 (6) | 0.076 (9) | −0.003 (5) | 0.042 (6) | −0.009 (6) |
C143 | 0.082 (9) | 0.082 (9) | 0.069 (9) | 0.012 (7) | 0.053 (8) | 0.000 (7) |
C144 | 0.051 (6) | 0.053 (6) | 0.055 (7) | 0.017 (5) | 0.030 (6) | 0.007 (5) |
Co1—O1 | 1.952 (6) | Co3—Cl5 | 2.245 (3) |
Co1—O2 | 1.972 (6) | P5—O5 | 1.513 (6) |
Co1—Cl1 | 2.247 (2) | P5—C79 | 1.782 (9) |
Co1—Cl2 | 2.260 (3) | P5—C73 | 1.787 (9) |
P1—O1 | 1.506 (6) | P5—C85 | 1.795 (8) |
P1—C7 | 1.780 (9) | P6—O6 | 1.507 (6) |
P1—C1 | 1.784 (8) | P6—C103 | 1.766 (10) |
P1—C13 | 1.784 (9) | P6—C97 | 1.789 (10) |
P2—O2 | 1.507 (6) | P6—C91 | 1.796 (8) |
P2—C19 | 1.792 (9) | C73—C74 | 1.379 (13) |
P2—C31 | 1.800 (9) | C73—C78 | 1.404 (13) |
P2—C25 | 1.799 (9) | C74—C75 | 1.381 (15) |
C1—C2 | 1.398 (11) | C74—H74 | 0.95 |
C1—C6 | 1.410 (12) | C75—C76 | 1.387 (18) |
C2—C3 | 1.387 (12) | C75—H75 | 0.95 |
C2—H2 | 0.95 | C76—C77 | 1.366 (18) |
C3—C4 | 1.372 (13) | C76—H76 | 0.95 |
C3—H3 | 0.95 | C77—C78 | 1.389 (14) |
C4—C5 | 1.381 (13) | C77—H77 | 0.95 |
C4—H4 | 0.95 | C78—H78 | 0.95 |
C5—C6 | 1.386 (12) | C79—C80 | 1.398 (12) |
C5—H5 | 0.95 | C79—C84 | 1.409 (11) |
C6—H6 | 0.95 | C80—C81 | 1.357 (13) |
C7—C12 | 1.413 (12) | C80—H80 | 0.95 |
C7—C8 | 1.414 (12) | C81—C82 | 1.385 (13) |
C8—C9 | 1.381 (13) | C81—H81 | 0.95 |
C8—H8 | 0.95 | C82—C83 | 1.380 (13) |
C9—C10 | 1.416 (14) | C82—H82 | 0.95 |
C9—H9 | 0.95 | C83—C84 | 1.386 (12) |
C10—C11 | 1.370 (13) | C83—H83 | 0.95 |
C10—H10 | 0.95 | C84—H84 | 0.95 |
C11—C12 | 1.352 (13) | C85—C90 | 1.385 (12) |
C11—H11 | 0.95 | C85—C86 | 1.394 (13) |
C12—H12 | 0.95 | C86—C87 | 1.390 (13) |
C13—C18 | 1.375 (15) | C86—H86 | 0.95 |
C13—C14 | 1.402 (15) | C87—C88 | 1.375 (14) |
C14—C15 | 1.385 (17) | C87—H87 | 0.95 |
C14—H14 | 0.95 | C88—C89 | 1.376 (14) |
C15—C16 | 1.38 (2) | C88—H88 | 0.95 |
C15—H15 | 0.95 | C89—C90 | 1.382 (12) |
C16—C17 | 1.39 (2) | C89—H89 | 0.95 |
C16—H16 | 0.95 | C90—H90 | 0.95 |
C17—C18 | 1.370 (15) | C91—C96 | 1.384 (12) |
C17—H17 | 0.95 | C91—C92 | 1.412 (12) |
C18—H18 | 0.95 | C92—C93 | 1.380 (13) |
C19—C24 | 1.387 (12) | C92—H92 | 0.95 |
C19—C20 | 1.398 (13) | C93—C94 | 1.386 (14) |
C20—C21 | 1.393 (13) | C93—H93 | 0.95 |
C20—H20 | 0.95 | C94—C95 | 1.357 (15) |
C21—C22 | 1.372 (14) | C94—H94 | 0.95 |
C21—H21 | 0.95 | C95—C96 | 1.404 (13) |
C22—C23 | 1.383 (14) | C95—H95 | 0.95 |
C22—H22 | 0.95 | C96—H96 | 0.95 |
C23—C24 | 1.397 (13) | C97—C98 | 1.396 (13) |
C23—H23 | 0.95 | C97—C102 | 1.396 (13) |
C24—H24 | 0.95 | C98—C99 | 1.402 (15) |
C25—C26 | 1.382 (12) | C98—H98 | 0.95 |
C25—C30 | 1.400 (12) | C99—C100 | 1.372 (15) |
C26—C27 | 1.394 (13) | C99—H99 | 0.95 |
C26—H26 | 0.95 | C100—C101 | 1.395 (15) |
C27—C28 | 1.401 (14) | C100—H100 | 0.95 |
C27—H27 | 0.95 | C101—C102 | 1.375 (15) |
C28—C29 | 1.358 (14) | C101—H101 | 0.95 |
C28—H28 | 0.95 | C102—H102 | 0.95 |
C29—C30 | 1.364 (13) | C103—C104 | 1.382 (16) |
C29—H29 | 0.95 | C103—C108 | 1.407 (16) |
C30—H31 | 0.95 | C104—C105 | 1.39 (2) |
C31—C32 | 1.393 (13) | C104—H104 | 0.95 |
C31—C36 | 1.407 (13) | C105—C106 | 1.37 (3) |
C32—C33 | 1.384 (13) | C105—H105 | 0.95 |
C32—H32 | 0.95 | C106—C107 | 1.37 (3) |
C33—C34 | 1.358 (14) | C106—H106 | 0.95 |
C33—H33 | 0.95 | C107—C108 | 1.385 (17) |
C34—C35 | 1.375 (15) | C107—H107 | 0.95 |
C34—H34 | 0.95 | C108—H208 | 0.95 |
C35—C36 | 1.381 (13) | Co4—O7 | 1.955 (6) |
C35—H35 | 0.95 | Co4—O8 | 1.988 (6) |
C36—H36 | 0.95 | Co4—Cl7 | 2.226 (3) |
Co2—O4 | 1.959 (6) | Co4—Cl8 | 2.260 (3) |
Co2—O3 | 1.988 (6) | P7—O7 | 1.518 (6) |
Co2—Cl4 | 2.226 (3) | P7—C109 | 1.781 (9) |
Co2—Cl3 | 2.251 (3) | P7—C115 | 1.786 (8) |
P3—O3 | 1.500 (6) | P7—C121 | 1.791 (9) |
P3—C49 | 1.791 (9) | P8—O8 | 1.495 (6) |
P3—C43 | 1.793 (9) | P8—C127 | 1.777 (9) |
P3—C37 | 1.797 (9) | P8—C133 | 1.785 (9) |
P4—O4 | 1.508 (6) | P8—C139 | 1.792 (9) |
P4—C55 | 1.790 (9) | C109—C110 | 1.384 (12) |
P4—C61 | 1.796 (9) | C109—C114 | 1.415 (13) |
P4—C67 | 1.815 (10) | C110—C111 | 1.374 (13) |
C37—C38 | 1.391 (12) | C110—H110 | 0.95 |
C37—C42 | 1.394 (12) | C111—C112 | 1.391 (14) |
C38—C39 | 1.413 (13) | C111—H111 | 0.95 |
C38—H38 | 0.95 | C112—C113 | 1.367 (14) |
C39—C40 | 1.407 (13) | C112—H112 | 0.95 |
C39—H39 | 0.95 | C113—C114 | 1.367 (13) |
C40—C41 | 1.377 (13) | C113—H113 | 0.95 |
C40—H40 | 0.95 | C114—H114 | 0.95 |
C41—C42 | 1.378 (13) | C115—C120 | 1.385 (12) |
C41—H41 | 0.95 | C115—C116 | 1.392 (12) |
C42—H42 | 0.95 | C116—C117 | 1.375 (14) |
C43—C48 | 1.379 (12) | C116—H116 | 0.95 |
C43—C44 | 1.399 (13) | C117—C118 | 1.405 (16) |
C44—C45 | 1.356 (13) | C117—H117 | 0.95 |
C44—H44 | 0.95 | C118—C119 | 1.361 (16) |
C45—C46 | 1.389 (14) | C118—H118 | 0.95 |
C45—H45 | 0.95 | C119—C120 | 1.377 (14) |
C46—C47 | 1.399 (15) | C119—H119 | 0.95 |
C46—H46 | 0.95 | C120—H120 | 0.95 |
C47—C48 | 1.413 (13) | C121—C126 | 1.381 (13) |
C47—H47 | 0.95 | C121—C122 | 1.392 (13) |
C48—H48 | 0.95 | C122—C123 | 1.370 (13) |
C49—C50 | 1.381 (13) | C122—H122 | 0.95 |
C49—C54 | 1.404 (12) | C123—C124 | 1.385 (14) |
C50—C51 | 1.398 (14) | C123—H123 | 0.95 |
C50—H50 | 0.95 | C124—C125 | 1.350 (14) |
C51—C52 | 1.386 (15) | C124—H124 | 0.95 |
C51—H51 | 0.95 | C125—C126 | 1.396 (14) |
C52—C53 | 1.389 (15) | C125—H125 | 0.95 |
C52—H52 | 0.95 | C126—H126 | 0.95 |
C53—C54 | 1.384 (13) | C127—C132 | 1.394 (13) |
C53—H53 | 0.95 | C127—C128 | 1.414 (13) |
C54—H55 | 0.95 | C128—C129 | 1.397 (14) |
C55—C60 | 1.372 (14) | C128—H128 | 0.95 |
C55—C56 | 1.418 (15) | C129—C130 | 1.368 (16) |
C56—C57 | 1.384 (15) | C129—H129 | 0.95 |
C56—H56 | 0.95 | C130—C131 | 1.355 (15) |
C57—C58 | 1.34 (2) | C130—H130 | 0.95 |
C57—H57 | 0.95 | C131—C132 | 1.407 (14) |
C58—C59 | 1.37 (2) | C131—H131 | 0.95 |
C58—H58 | 0.95 | C132—H132 | 0.95 |
C59—C60 | 1.410 (16) | C133—C134 | 1.387 (14) |
C59—H59 | 0.95 | C133—C138 | 1.391 (12) |
C60—H60 | 0.95 | C134—C135 | 1.416 (14) |
C61—C66 | 1.388 (13) | C134—H134 | 0.95 |
C61—C62 | 1.389 (13) | C135—C136 | 1.378 (14) |
C62—C63 | 1.369 (13) | C135—H135 | 0.95 |
C62—H62 | 0.95 | C136—C137 | 1.357 (15) |
C63—C64 | 1.345 (17) | C136—H136 | 0.95 |
C63—H63 | 0.95 | C137—C138 | 1.396 (13) |
C64—C65 | 1.399 (18) | C137—H137 | 0.95 |
C64—H64 | 0.95 | C138—H138 | 0.95 |
C65—C66 | 1.369 (15) | C139—C144 | 1.381 (13) |
C65—H65 | 0.95 | C139—C140 | 1.403 (12) |
C66—H66 | 0.95 | C140—C141 | 1.380 (13) |
C67—C68 | 1.372 (12) | C140—H140 | 0.95 |
C67—C72 | 1.379 (13) | C141—C142 | 1.360 (15) |
C68—C69 | 1.377 (14) | C141—H141 | 0.95 |
C68—H68 | 0.95 | C142—C143 | 1.391 (15) |
C69—C70 | 1.377 (14) | C142—H142 | 0.95 |
C69—H69 | 0.95 | C143—C144 | 1.392 (14) |
C70—C71 | 1.383 (16) | C143—H143 | 0.95 |
C70—H70 | 0.95 | C144—H144 | 0.95 |
C71—C72 | 1.371 (16) | O9—C145 | 1.33 (4) |
C71—H71 | 0.95 | O9—H9B | 0.8402 |
C72—H72 | 0.95 | C145—H145 | 0.98 |
Co3—O6 | 1.968 (6) | C145—H146 | 0.98 |
Co3—O5 | 1.988 (6) | C145—H147 | 0.98 |
Co3—Cl6 | 2.221 (3) | ||
O1—Co1—O2 | 104.3 (3) | O5—Co3—Cl5 | 105.51 (19) |
O1—Co1—Cl1 | 111.0 (2) | Cl6—Co3—Cl5 | 119.28 (17) |
O2—Co1—Cl1 | 107.96 (19) | O5—P5—C79 | 113.6 (4) |
O1—Co1—Cl2 | 105.35 (19) | O5—P5—C73 | 108.1 (4) |
O2—Co1—Cl2 | 107.60 (19) | C79—P5—C73 | 105.4 (4) |
Cl1—Co1—Cl2 | 119.57 (11) | O5—P5—C85 | 111.7 (4) |
O1—P1—C7 | 112.0 (4) | C79—P5—C85 | 109.1 (4) |
O1—P1—C1 | 109.1 (4) | C73—P5—C85 | 108.6 (4) |
C7—P1—C1 | 107.1 (4) | O6—P6—C103 | 111.9 (4) |
O1—P1—C13 | 112.6 (4) | O6—P6—C97 | 111.0 (4) |
C7—P1—C13 | 107.5 (4) | C103—P6—C97 | 109.8 (5) |
C1—P1—C13 | 108.3 (4) | O6—P6—C91 | 110.2 (4) |
O2—P2—C19 | 111.6 (4) | C103—P6—C91 | 106.9 (4) |
O2—P2—C31 | 111.5 (4) | C97—P6—C91 | 106.9 (4) |
C19—P2—C31 | 107.5 (4) | P5—O5—Co3 | 138.4 (4) |
O2—P2—C25 | 107.9 (4) | P6—O6—Co3 | 140.5 (4) |
C19—P2—C25 | 107.5 (4) | C74—C73—C78 | 118.3 (9) |
C31—P2—C25 | 110.8 (4) | C74—C73—P5 | 119.9 (7) |
P1—O1—Co1 | 150.3 (4) | C78—C73—P5 | 121.7 (7) |
P2—O2—Co1 | 154.3 (4) | C75—C74—C73 | 122.5 (11) |
C2—C1—C6 | 118.2 (8) | C75—C74—H74 | 118.8 |
C2—C1—P1 | 118.1 (6) | C73—C74—H74 | 118.8 |
C6—C1—P1 | 123.6 (7) | C74—C75—C76 | 117.1 (11) |
C3—C2—C1 | 121.2 (8) | C74—C75—H75 | 121.5 |
C3—C2—H2 | 119.4 | C76—C75—H75 | 121.5 |
C1—C2—H2 | 119.4 | C77—C76—C75 | 123.2 (10) |
C4—C3—C2 | 119.3 (9) | C77—C76—H76 | 118.4 |
C4—C3—H3 | 120.3 | C75—C76—H76 | 118.4 |
C2—C3—H3 | 120.3 | C76—C77—C78 | 118.4 (12) |
C3—C4—C5 | 121.2 (9) | C76—C77—H77 | 120.8 |
C3—C4—H4 | 119.4 | C78—C77—H77 | 120.8 |
C5—C4—H4 | 119.4 | C77—C78—C73 | 120.6 (10) |
C4—C5—C6 | 119.9 (8) | C77—C78—H78 | 119.7 |
C4—C5—H5 | 120.1 | C73—C78—H78 | 119.7 |
C6—C5—H5 | 120.1 | C80—C79—C84 | 118.4 (8) |
C5—C6—C1 | 120.2 (9) | C80—C79—P5 | 121.5 (6) |
C5—C6—H6 | 119.9 | C84—C79—P5 | 119.8 (7) |
C1—C6—H6 | 119.9 | C81—C80—C79 | 120.5 (8) |
C12—C7—C8 | 118.9 (8) | C81—C80—H80 | 119.8 |
C12—C7—P1 | 122.4 (7) | C79—C80—H80 | 119.8 |
C8—C7—P1 | 118.6 (6) | C80—C81—C82 | 121.6 (9) |
C9—C8—C7 | 119.7 (9) | C80—C81—H81 | 119.2 |
C9—C8—H8 | 120.1 | C82—C81—H81 | 119.2 |
C7—C8—H8 | 120.1 | C83—C82—C81 | 119.0 (9) |
C8—C9—C10 | 120.2 (9) | C83—C82—H82 | 120.5 |
C8—C9—H9 | 119.9 | C81—C82—H82 | 120.5 |
C10—C9—H9 | 119.9 | C82—C83—C84 | 120.5 (8) |
C11—C10—C9 | 118.6 (9) | C82—C83—H83 | 119.7 |
C11—C10—H10 | 120.7 | C84—C83—H83 | 119.7 |
C9—C10—H10 | 120.7 | C83—C84—C79 | 120.0 (8) |
C12—C11—C10 | 122.7 (9) | C83—C84—H84 | 120 |
C12—C11—H11 | 118.6 | C79—C84—H84 | 120 |
C10—C11—H11 | 118.6 | C90—C85—C86 | 119.1 (8) |
C11—C12—C7 | 119.7 (8) | C90—C85—P5 | 122.2 (7) |
C11—C12—H12 | 120.1 | C86—C85—P5 | 118.7 (7) |
C7—C12—H12 | 120.1 | C87—C86—C85 | 119.4 (9) |
C18—C13—C14 | 118.8 (10) | C87—C86—H86 | 120.3 |
C18—C13—P1 | 122.9 (8) | C85—C86—H86 | 120.3 |
C14—C13—P1 | 118.2 (9) | C88—C87—C86 | 121.1 (10) |
C15—C14—C13 | 120.3 (14) | C88—C87—H87 | 119.5 |
C15—C14—H14 | 119.8 | C86—C87—H87 | 119.5 |
C13—C14—H14 | 119.8 | C89—C88—C87 | 119.4 (9) |
C16—C15—C14 | 118.9 (14) | C89—C88—H88 | 120.3 |
C16—C15—H15 | 120.6 | C87—C88—H88 | 120.3 |
C14—C15—H15 | 120.6 | C88—C89—C90 | 120.4 (9) |
C15—C16—C17 | 121.6 (12) | C88—C89—H89 | 119.8 |
C15—C16—H16 | 119.2 | C90—C89—H89 | 119.8 |
C17—C16—H16 | 119.2 | C89—C90—C85 | 120.6 (9) |
C18—C17—C16 | 118.5 (15) | C89—C90—H90 | 119.7 |
C18—C17—H17 | 120.7 | C85—C90—H90 | 119.7 |
C16—C17—H17 | 120.7 | C96—C91—C92 | 119.3 (8) |
C17—C18—C13 | 121.8 (13) | C96—C91—P6 | 123.5 (7) |
C17—C18—H18 | 119.1 | C92—C91—P6 | 117.2 (6) |
C13—C18—H18 | 119.1 | C93—C92—C91 | 119.8 (9) |
C24—C19—C20 | 119.8 (9) | C93—C92—H92 | 120.1 |
C24—C19—P2 | 118.6 (7) | C91—C92—H92 | 120.1 |
C20—C19—P2 | 121.5 (7) | C92—C93—C94 | 120.4 (9) |
C21—C20—C19 | 119.5 (9) | C92—C93—H93 | 119.8 |
C21—C20—H20 | 120.2 | C94—C93—H93 | 119.8 |
C19—C20—H20 | 120.2 | C95—C94—C93 | 120.2 (9) |
C22—C21—C20 | 120.5 (10) | C95—C94—H94 | 119.9 |
C22—C21—H21 | 119.7 | C93—C94—H94 | 119.9 |
C20—C21—H21 | 119.7 | C94—C95—C96 | 120.9 (10) |
C21—C22—C23 | 120.2 (9) | C94—C95—H95 | 119.6 |
C21—C22—H22 | 119.9 | C96—C95—H95 | 119.6 |
C23—C22—H22 | 119.9 | C91—C96—C95 | 119.5 (9) |
C22—C23—C24 | 120.2 (9) | C91—C96—H96 | 120.3 |
C22—C23—H23 | 119.9 | C95—C96—H96 | 120.3 |
C24—C23—H23 | 119.9 | C98—C97—C102 | 118.7 (9) |
C19—C24—C23 | 119.7 (10) | C98—C97—P6 | 121.2 (7) |
C19—C24—H24 | 120.1 | C102—C97—P6 | 120.0 (7) |
C23—C24—H24 | 120.1 | C97—C98—C99 | 119.9 (10) |
C26—C25—C30 | 119.4 (8) | C97—C98—H98 | 120.1 |
C26—C25—P2 | 117.6 (7) | C99—C98—H98 | 120.1 |
C30—C25—P2 | 122.8 (7) | C100—C99—C98 | 120.8 (10) |
C25—C26—C27 | 120.7 (9) | C100—C99—H99 | 119.6 |
C25—C26—H26 | 119.6 | C98—C99—H99 | 119.6 |
C27—C26—H26 | 119.6 | C99—C100—C101 | 119.1 (10) |
C26—C27—C28 | 118.4 (9) | C99—C100—H100 | 120.4 |
C26—C27—H27 | 120.8 | C101—C100—H100 | 120.4 |
C28—C27—H27 | 120.8 | C102—C101—C100 | 120.7 (10) |
C29—C28—C27 | 120.4 (9) | C102—C101—H101 | 119.7 |
C29—C28—H28 | 119.8 | C100—C101—H101 | 119.7 |
C27—C28—H28 | 119.8 | C101—C102—C97 | 120.7 (10) |
C28—C29—C30 | 121.6 (9) | C101—C102—H102 | 119.6 |
C28—C29—H29 | 119.2 | C97—C102—H102 | 119.6 |
C30—C29—H29 | 119.2 | C104—C103—C108 | 117.7 (11) |
C29—C30—C25 | 119.5 (9) | C104—C103—P6 | 124.9 (10) |
C29—C30—H31 | 120.3 | C108—C103—P6 | 117.3 (9) |
C25—C30—H31 | 120.3 | C103—C104—C105 | 120.9 (16) |
C32—C31—C36 | 119.9 (9) | C103—C104—H104 | 119.6 |
C32—C31—P2 | 118.4 (7) | C105—C104—H104 | 119.6 |
C36—C31—P2 | 121.7 (8) | C106—C105—C104 | 121.5 (19) |
C33—C32—C31 | 117.3 (9) | C106—C105—H105 | 119.3 |
C33—C32—H32 | 121.3 | C104—C105—H105 | 119.3 |
C31—C32—H32 | 121.3 | C105—C106—C107 | 118.1 (16) |
C34—C33—C32 | 123.4 (10) | C105—C106—H106 | 120.9 |
C34—C33—H33 | 118.3 | C107—C106—H106 | 120.9 |
C32—C33—H33 | 118.3 | C106—C107—C108 | 122.1 (17) |
C33—C34—C35 | 119.2 (9) | C106—C107—H107 | 119 |
C33—C34—H34 | 120.4 | C108—C107—H107 | 119 |
C35—C34—H34 | 120.4 | C107—C108—C103 | 119.7 (15) |
C34—C35—C36 | 120.1 (9) | C107—C108—H208 | 120.2 |
C34—C35—H35 | 119.9 | C103—C108—H208 | 120.2 |
C36—C35—H35 | 119.9 | O7—Co4—O8 | 104.8 (2) |
C35—C36—C31 | 120.0 (10) | O7—Co4—Cl7 | 108.01 (19) |
C35—C36—H36 | 120 | O8—Co4—Cl7 | 106.05 (19) |
C31—C36—H36 | 120 | O7—Co4—Cl8 | 105.44 (19) |
O4—Co2—O3 | 104.7 (3) | O8—Co4—Cl8 | 107.5 (2) |
O4—Co2—Cl4 | 107.4 (2) | Cl7—Co4—Cl8 | 123.64 (14) |
O3—Co2—Cl4 | 109.0 (2) | O7—P7—C109 | 112.3 (4) |
O4—Co2—Cl3 | 106.02 (19) | O7—P7—C115 | 110.0 (4) |
O3—Co2—Cl3 | 112.52 (19) | C109—P7—C115 | 107.7 (4) |
Cl4—Co2—Cl3 | 116.42 (13) | O7—P7—C121 | 111.3 (4) |
O3—P3—C49 | 111.6 (4) | C109—P7—C121 | 109.5 (4) |
O3—P3—C43 | 112.2 (4) | C115—P7—C121 | 105.7 (4) |
C49—P3—C43 | 107.5 (4) | O8—P8—C127 | 108.0 (4) |
O3—P3—C37 | 109.5 (4) | O8—P8—C133 | 112.4 (4) |
C49—P3—C37 | 110.0 (4) | C127—P8—C133 | 107.8 (4) |
C43—P3—C37 | 105.8 (4) | O8—P8—C139 | 111.7 (4) |
O4—P4—C55 | 113.1 (4) | C127—P8—C139 | 109.9 (4) |
O4—P4—C61 | 110.4 (4) | C133—P8—C139 | 107.1 (4) |
C55—P4—C61 | 107.1 (4) | P7—O7—Co4 | 143.4 (4) |
O4—P4—C67 | 111.0 (4) | P8—O8—Co4 | 148.3 (4) |
C55—P4—C67 | 108.6 (5) | C110—C109—C114 | 118.1 (8) |
C61—P4—C67 | 106.3 (4) | C110—C109—P7 | 119.3 (7) |
P3—O3—Co2 | 148.2 (4) | C114—C109—P7 | 122.5 (7) |
P4—O4—Co2 | 143.2 (4) | C111—C110—C109 | 121.2 (10) |
C38—C37—C42 | 119.5 (8) | C111—C110—H110 | 119.4 |
C38—C37—P3 | 117.4 (7) | C109—C110—H110 | 119.4 |
C42—C37—P3 | 122.9 (7) | C110—C111—C112 | 120.2 (9) |
C37—C38—C39 | 119.5 (9) | C110—C111—H111 | 119.9 |
C37—C38—H38 | 120.2 | C112—C111—H111 | 119.9 |
C39—C38—H38 | 120.2 | C113—C112—C111 | 118.9 (9) |
C40—C39—C38 | 119.7 (9) | C113—C112—H112 | 120.5 |
C40—C39—H39 | 120.2 | C111—C112—H112 | 120.5 |
C38—C39—H39 | 120.2 | C112—C113—C114 | 121.9 (9) |
C41—C40—C39 | 119.8 (9) | C112—C113—H113 | 119 |
C41—C40—H40 | 120.1 | C114—C113—H113 | 119 |
C39—C40—H40 | 120.1 | C113—C114—C109 | 119.7 (9) |
C40—C41—C42 | 120.4 (9) | C113—C114—H114 | 120.2 |
C40—C41—H41 | 119.8 | C109—C114—H114 | 120.2 |
C42—C41—H41 | 119.8 | C120—C115—C116 | 119.0 (8) |
C41—C42—C37 | 121.1 (8) | C120—C115—P7 | 123.7 (7) |
C41—C42—H42 | 119.5 | C116—C115—P7 | 117.3 (7) |
C37—C42—H42 | 119.5 | C117—C116—C115 | 121.0 (10) |
C48—C43—C44 | 119.4 (8) | C117—C116—H116 | 119.5 |
C48—C43—P3 | 118.1 (7) | C115—C116—H116 | 119.5 |
C44—C43—P3 | 122.5 (7) | C116—C117—C118 | 118.1 (10) |
C45—C44—C43 | 120.4 (9) | C116—C117—H117 | 120.9 |
C45—C44—H44 | 119.8 | C118—C117—H117 | 120.9 |
C43—C44—H44 | 119.8 | C119—C118—C117 | 121.6 (10) |
C44—C45—C46 | 121.4 (10) | C119—C118—H118 | 119.2 |
C44—C45—H45 | 119.3 | C117—C118—H118 | 119.2 |
C46—C45—H45 | 119.3 | C118—C119—C120 | 119.4 (11) |
C45—C46—C47 | 119.3 (9) | C118—C119—H119 | 120.3 |
C45—C46—H46 | 120.3 | C120—C119—H119 | 120.3 |
C47—C46—H46 | 120.3 | C119—C120—C115 | 120.8 (10) |
C46—C47—C48 | 118.9 (9) | C119—C120—H120 | 119.6 |
C46—C47—H47 | 120.5 | C115—C120—H120 | 119.6 |
C48—C47—H47 | 120.5 | C126—C121—C122 | 118.3 (9) |
C43—C48—C47 | 120.5 (9) | C126—C121—P7 | 120.6 (7) |
C43—C48—H48 | 119.8 | C122—C121—P7 | 121.1 (7) |
C47—C48—H48 | 119.8 | C123—C122—C121 | 120.6 (9) |
C50—C49—C54 | 120.1 (9) | C123—C122—H122 | 119.7 |
C50—C49—P3 | 117.6 (7) | C121—C122—H122 | 119.7 |
C54—C49—P3 | 122.3 (7) | C122—C123—C124 | 120.4 (9) |
C49—C50—C51 | 120.0 (9) | C122—C123—H123 | 119.8 |
C49—C50—H50 | 120 | C124—C123—H123 | 119.8 |
C51—C50—H50 | 120 | C125—C124—C123 | 119.8 (9) |
C52—C51—C50 | 119.7 (10) | C125—C124—H124 | 120.1 |
C52—C51—H51 | 120.2 | C123—C124—H124 | 120.1 |
C50—C51—H51 | 120.2 | C124—C125—C126 | 120.3 (9) |
C51—C52—C53 | 120.5 (10) | C124—C125—H125 | 119.8 |
C51—C52—H52 | 119.8 | C126—C125—H125 | 119.8 |
C53—C52—H52 | 119.8 | C121—C126—C125 | 120.5 (9) |
C54—C53—C52 | 120.0 (9) | C121—C126—H126 | 119.8 |
C54—C53—H53 | 120 | C125—C126—H126 | 119.8 |
C52—C53—H53 | 120 | C132—C127—C128 | 119.1 (9) |
C53—C54—C49 | 119.8 (9) | C132—C127—P8 | 118.1 (7) |
C53—C54—H55 | 120.1 | C128—C127—P8 | 122.8 (7) |
C49—C54—H55 | 120.1 | C129—C128—C127 | 119.1 (10) |
C60—C55—C56 | 119.8 (10) | C129—C128—H128 | 120.4 |
C60—C55—P4 | 123.5 (9) | C127—C128—H128 | 120.4 |
C56—C55—P4 | 116.7 (8) | C130—C129—C128 | 119.9 (10) |
C57—C56—C55 | 119.0 (13) | C130—C129—H129 | 120 |
C57—C56—H56 | 120.5 | C128—C129—H129 | 120 |
C55—C56—H56 | 120.5 | C131—C130—C129 | 122.4 (10) |
C58—C57—C56 | 121.2 (15) | C131—C130—H130 | 118.8 |
C58—C57—H57 | 119.4 | C129—C130—H130 | 118.8 |
C56—C57—H57 | 119.4 | C130—C131—C132 | 119.0 (11) |
C57—C58—C59 | 120.5 (13) | C130—C131—H131 | 120.5 |
C57—C58—H58 | 119.7 | C132—C131—H131 | 120.5 |
C59—C58—H58 | 119.7 | C127—C132—C131 | 120.4 (10) |
C58—C59—C60 | 120.7 (13) | C127—C132—H132 | 119.8 |
C58—C59—H59 | 119.7 | C131—C132—H132 | 119.8 |
C60—C59—H59 | 119.7 | C134—C133—C138 | 118.4 (9) |
C55—C60—C59 | 118.8 (13) | C134—C133—P8 | 122.5 (7) |
C55—C60—H60 | 120.6 | C138—C133—P8 | 118.9 (7) |
C59—C60—H60 | 120.6 | C133—C134—C135 | 120.8 (10) |
C66—C61—C62 | 118.6 (9) | C133—C134—H134 | 119.6 |
C66—C61—P4 | 118.1 (7) | C135—C134—H134 | 119.6 |
C62—C61—P4 | 123.3 (7) | C136—C135—C134 | 118.6 (11) |
C63—C62—C61 | 119.9 (10) | C136—C135—H135 | 120.7 |
C63—C62—H62 | 120 | C134—C135—H135 | 120.7 |
C61—C62—H62 | 120 | C137—C136—C135 | 121.3 (10) |
C64—C63—C62 | 121.2 (12) | C137—C136—H136 | 119.3 |
C64—C63—H63 | 119.4 | C135—C136—H136 | 119.3 |
C62—C63—H63 | 119.4 | C136—C137—C138 | 120.2 (10) |
C63—C64—C65 | 120.3 (10) | C136—C137—H137 | 119.9 |
C63—C64—H64 | 119.8 | C138—C137—H137 | 119.9 |
C65—C64—H64 | 119.8 | C133—C138—C137 | 120.6 (10) |
C66—C65—C64 | 118.8 (11) | C133—C138—H138 | 119.7 |
C66—C65—H65 | 120.6 | C137—C138—H138 | 119.7 |
C64—C65—H65 | 120.6 | C144—C139—C140 | 119.1 (9) |
C65—C66—C61 | 121.0 (10) | C144—C139—P8 | 118.3 (7) |
C65—C66—H66 | 119.5 | C140—C139—P8 | 122.5 (7) |
C61—C66—H66 | 119.5 | C141—C140—C139 | 119.3 (10) |
C68—C67—C72 | 120.1 (9) | C141—C140—H140 | 120.3 |
C68—C67—P4 | 121.5 (7) | C139—C140—H140 | 120.3 |
C72—C67—P4 | 118.3 (7) | C142—C141—C140 | 121.9 (10) |
C67—C68—C69 | 120.9 (9) | C142—C141—H141 | 119 |
C67—C68—H68 | 119.5 | C140—C141—H141 | 119 |
C69—C68—H68 | 119.5 | C141—C142—C143 | 119.2 (10) |
C70—C69—C68 | 118.4 (10) | C141—C142—H142 | 120.4 |
C70—C69—H69 | 120.8 | C143—C142—H142 | 120.4 |
C68—C69—H69 | 120.8 | C142—C143—C144 | 120.0 (12) |
C69—C70—C71 | 121.1 (11) | C142—C143—H143 | 120 |
C69—C70—H70 | 119.4 | C144—C143—H143 | 120 |
C71—C70—H70 | 119.4 | C139—C144—C143 | 120.4 (10) |
C72—C71—C70 | 119.6 (10) | C139—C144—H144 | 119.8 |
C72—C71—H71 | 120.2 | C143—C144—H144 | 119.8 |
C70—C71—H71 | 120.2 | C145—O9—H9B | 109.2 |
C71—C72—C67 | 119.7 (10) | O9—C145—H145 | 109.5 |
C71—C72—H72 | 120.1 | O9—C145—H146 | 109.4 |
C67—C72—H72 | 120.1 | H145—C145—H146 | 109.5 |
O6—Co3—O5 | 107.2 (2) | O9—C145—H147 | 109.5 |
O6—Co3—Cl6 | 107.5 (2) | H145—C145—H147 | 109.5 |
O5—Co3—Cl6 | 110.4 (2) | H146—C145—H147 | 109.5 |
O6—Co3—Cl5 | 106.4 (2) | ||
C7—P1—O1—Co1 | −62.7 (9) | C79—P5—O5—Co3 | 71.1 (6) |
C1—P1—O1—Co1 | 178.9 (7) | C73—P5—O5—Co3 | −172.3 (5) |
C13—P1—O1—Co1 | 58.7 (9) | C85—P5—O5—Co3 | −52.9 (6) |
O2—Co1—O1—P1 | −5.1 (9) | O6—Co3—O5—P5 | −140.3 (5) |
Cl1—Co1—O1—P1 | 110.9 (8) | Cl5—Co3—O5—P5 | −27.2 (6) |
Cl2—Co1—O1—P1 | −118.3 (8) | Cl6—Co3—O5—P5 | 102.9 (5) |
C19—P2—O2—Co1 | −85.6 (9) | C103—P6—O6—Co3 | −40.4 (8) |
C31—P2—O2—Co1 | 34.6 (10) | C97—P6—O6—Co3 | 82.6 (7) |
C25—P2—O2—Co1 | 156.5 (8) | C91—P6—O6—Co3 | −159.3 (6) |
O1—Co1—O2—P2 | 156.5 (9) | O5—Co3—O6—P6 | −12.5 (7) |
Cl1—Co1—O2—P2 | 38.4 (9) | Cl5—Co3—O6—P6 | −125.0 (6) |
Cl2—Co1—O2—P2 | −91.9 (9) | Cl6—Co3—O6—P6 | 106.2 (6) |
O1—P1—C1—C2 | 43.9 (8) | O5—P5—C73—C74 | −7.3 (9) |
C7—P1—C1—C2 | −77.5 (8) | C79—P5—C73—C74 | 114.5 (8) |
C13—P1—C1—C2 | 166.8 (7) | C85—P5—C73—C74 | −128.7 (8) |
O1—P1—C1—C6 | −137.7 (8) | O5—P5—C73—C78 | 175.9 (8) |
C7—P1—C1—C6 | 100.8 (8) | C79—P5—C73—C78 | −62.3 (9) |
C13—P1—C1—C6 | −14.8 (9) | C85—P5—C73—C78 | 54.5 (9) |
C6—C1—C2—C3 | 0.1 (13) | C78—C73—C74—C75 | −0.5 (15) |
P1—C1—C2—C3 | 178.6 (7) | P5—C73—C74—C75 | −177.4 (9) |
C1—C2—C3—C4 | 1.8 (14) | C73—C74—C75—C76 | 0.5 (17) |
C2—C3—C4—C5 | −3.0 (14) | C74—C75—C76—C77 | −0.7 (19) |
C3—C4—C5—C6 | 2.1 (15) | C75—C76—C77—C78 | 0.9 (19) |
C4—C5—C6—C1 | −0.1 (14) | C76—C77—C78—C73 | −0.9 (18) |
C2—C1—C6—C5 | −1.0 (13) | C74—C73—C78—C77 | 0.7 (16) |
P1—C1—C6—C5 | −179.4 (7) | P5—C73—C78—C77 | 177.5 (9) |
O1—P1—C7—C12 | −151.0 (7) | O5—P5—C79—C80 | 90.4 (8) |
C1—P1—C7—C12 | −31.4 (8) | C73—P5—C79—C80 | −27.7 (8) |
C13—P1—C7—C12 | 84.7 (8) | C85—P5—C79—C80 | −144.2 (7) |
O1—P1—C7—C8 | 29.1 (8) | O5—P5—C79—C84 | −83.4 (7) |
C1—P1—C7—C8 | 148.7 (7) | C73—P5—C79—C84 | 158.5 (7) |
C13—P1—C7—C8 | −95.2 (7) | C85—P5—C79—C84 | 42.0 (8) |
C12—C7—C8—C9 | 0.4 (13) | C84—C79—C80—C81 | −1.3 (13) |
P1—C7—C8—C9 | −179.7 (8) | P5—C79—C80—C81 | −175.2 (7) |
C7—C8—C9—C10 | 1.3 (15) | C79—C80—C81—C82 | −0.3 (15) |
C8—C9—C10—C11 | −2.9 (15) | C80—C81—C82—C83 | 1.9 (16) |
C9—C10—C11—C12 | 3.0 (15) | C81—C82—C83—C84 | −1.8 (14) |
C10—C11—C12—C7 | −1.3 (14) | C82—C83—C84—C79 | 0.2 (13) |
C8—C7—C12—C11 | −0.4 (13) | C80—C79—C84—C83 | 1.4 (12) |
P1—C7—C12—C11 | 179.7 (7) | P5—C79—C84—C83 | 175.4 (6) |
O1—P1—C13—C18 | −142.7 (8) | O5—P5—C85—C90 | 165.8 (7) |
C7—P1—C13—C18 | −18.8 (9) | C79—P5—C85—C90 | 39.4 (8) |
C1—P1—C13—C18 | 96.6 (9) | C73—P5—C85—C90 | −75.1 (8) |
O1—P1—C13—C14 | 40.1 (9) | O5—P5—C85—C86 | −14.1 (8) |
C7—P1—C13—C14 | 164.0 (7) | C79—P5—C85—C86 | −140.5 (7) |
C1—P1—C13—C14 | −80.6 (8) | C73—P5—C85—C86 | 105.0 (7) |
C18—C13—C14—C15 | −2.9 (15) | C90—C85—C86—C87 | 1.9 (14) |
P1—C13—C14—C15 | 174.4 (9) | P5—C85—C86—C87 | −178.1 (8) |
C13—C14—C15—C16 | 1.0 (18) | C85—C86—C87—C88 | −1.1 (16) |
C14—C15—C16—C17 | 1 (2) | C86—C87—C88—C89 | 1.5 (16) |
C15—C16—C17—C18 | −2 (2) | C87—C88—C89—C90 | −2.9 (15) |
C16—C17—C18—C13 | 0.1 (18) | C88—C89—C90—C85 | 3.9 (13) |
C14—C13—C18—C17 | 2.3 (16) | C86—C85—C90—C89 | −3.3 (13) |
P1—C13—C18—C17 | −174.9 (9) | P5—C85—C90—C89 | 176.7 (7) |
O2—P2—C19—C24 | 63.9 (8) | O6—P6—C91—C96 | 138.2 (8) |
C31—P2—C19—C24 | −58.6 (8) | C103—P6—C91—C96 | 16.3 (9) |
C25—P2—C19—C24 | −177.9 (7) | C97—P6—C91—C96 | −101.1 (8) |
O2—P2—C19—C20 | −111.3 (8) | O6—P6—C91—C92 | −43.7 (8) |
C31—P2—C19—C20 | 126.2 (8) | C103—P6—C91—C92 | −165.5 (8) |
C25—P2—C19—C20 | 6.9 (9) | C97—P6—C91—C92 | 77.0 (8) |
C24—C19—C20—C21 | −0.2 (14) | C96—C91—C92—C93 | 0.0 (14) |
P2—C19—C20—C21 | 175.0 (7) | P6—C91—C92—C93 | −178.3 (8) |
C19—C20—C21—C22 | −0.8 (15) | C91—C92—C93—C94 | −0.1 (15) |
C20—C21—C22—C23 | 1.2 (15) | C92—C93—C94—C95 | 0.1 (16) |
C21—C22—C23—C24 | −0.7 (14) | C93—C94—C95—C96 | 0.1 (17) |
C20—C19—C24—C23 | 0.7 (13) | C92—C91—C96—C95 | 0.3 (14) |
P2—C19—C24—C23 | −174.6 (7) | P6—C91—C96—C95 | 178.4 (8) |
C22—C23—C24—C19 | −0.2 (13) | C94—C95—C96—C91 | −0.3 (16) |
O2—P2—C25—C26 | 23.1 (8) | O6—P6—C97—C98 | 151.8 (8) |
C19—P2—C25—C26 | −97.4 (8) | C103—P6—C97—C98 | −84.0 (9) |
C31—P2—C25—C26 | 145.4 (7) | C91—P6—C97—C98 | 31.6 (10) |
O2—P2—C25—C30 | −161.8 (7) | O6—P6—C97—C102 | −26.2 (10) |
C19—P2—C25—C30 | 77.6 (8) | C103—P6—C97—C102 | 98.0 (9) |
C31—P2—C25—C30 | −39.5 (9) | C91—P6—C97—C102 | −146.4 (8) |
C30—C25—C26—C27 | 1.2 (15) | C102—C97—C98—C99 | 0.4 (17) |
P2—C25—C26—C27 | 176.4 (8) | P6—C97—C98—C99 | −177.6 (9) |
C25—C26—C27—C28 | 1.0 (16) | C97—C98—C99—C100 | −0.8 (19) |
C26—C27—C28—C29 | −2.1 (16) | C98—C99—C100—C101 | 2 (2) |
C27—C28—C29—C30 | 1.0 (17) | C99—C100—C101—C102 | −3 (2) |
C28—C29—C30—C25 | 1.2 (16) | C100—C101—C102—C97 | 2.4 (19) |
C26—C25—C30—C29 | −2.3 (14) | C98—C97—C102—C101 | −1.2 (16) |
P2—C25—C30—C29 | −177.3 (8) | P6—C97—C102—C101 | 176.8 (9) |
O2—P2—C31—C32 | 18.6 (8) | O6—P6—C103—C104 | 138.1 (8) |
C19—P2—C31—C32 | 141.1 (7) | C97—P6—C103—C104 | 14.4 (10) |
C25—P2—C31—C32 | −101.7 (8) | C91—P6—C103—C104 | −101.1 (9) |
O2—P2—C31—C36 | −162.1 (7) | O6—P6—C103—C108 | −45.8 (9) |
C19—P2—C31—C36 | −39.5 (8) | C97—P6—C103—C108 | −169.4 (7) |
C25—P2—C31—C36 | 77.7 (8) | C91—P6—C103—C108 | 75.0 (8) |
C36—C31—C32—C33 | 1.3 (13) | C108—C103—C104—C105 | −1.7 (15) |
P2—C31—C32—C33 | −179.3 (7) | P6—C103—C104—C105 | 174.5 (9) |
C31—C32—C33—C34 | −1.1 (15) | C103—C104—C105—C106 | 2 (2) |
C32—C33—C34—C35 | −0.4 (16) | C104—C105—C106—C107 | 0 (2) |
C33—C34—C35—C36 | 1.6 (15) | C105—C106—C107—C108 | −1 (2) |
C34—C35—C36—C31 | −1.4 (14) | C106—C107—C108—C103 | 0.6 (18) |
C32—C31—C36—C35 | −0.1 (13) | C104—C103—C108—C107 | 0.6 (14) |
P2—C31—C36—C35 | −179.5 (7) | P6—C103—C108—C107 | −175.8 (8) |
C49—P3—O3—Co2 | −51.2 (9) | C109—P7—O7—Co4 | 49.4 (7) |
C43—P3—O3—Co2 | 69.5 (9) | C115—P7—O7—Co4 | 169.3 (6) |
C37—P3—O3—Co2 | −173.2 (7) | C121—P7—O7—Co4 | −73.9 (7) |
O4—Co2—O3—P3 | −135.9 (7) | O8—Co4—O7—P7 | 15.7 (7) |
Cl3—Co2—O3—P3 | −21.2 (8) | Cl7—Co4—O7—P7 | 128.4 (6) |
Cl4—Co2—O3—P3 | 109.5 (7) | Cl8—Co4—O7—P7 | −97.6 (6) |
C55—P4—O4—Co2 | −30.7 (8) | C127—P8—O8—Co4 | 155.8 (7) |
C61—P4—O4—Co2 | −150.8 (6) | C133—P8—O8—Co4 | −85.5 (8) |
C67—P4—O4—Co2 | 91.7 (7) | C139—P8—O8—Co4 | 34.9 (8) |
O3—Co2—O4—P4 | −28.3 (7) | O7—Co4—O8—P8 | 156.3 (7) |
Cl3—Co2—O4—P4 | −147.4 (6) | Cl7—Co4—O8—P8 | 42.1 (8) |
Cl4—Co2—O4—P4 | 87.5 (7) | Cl8—Co4—O8—P8 | −91.9 (7) |
O3—P3—C37—C38 | −17.4 (8) | O7—P7—C109—C110 | 43.1 (8) |
C49—P3—C37—C38 | −140.4 (7) | C115—P7—C109—C110 | −78.2 (7) |
C43—P3—C37—C38 | 103.7 (7) | C121—P7—C109—C110 | 167.3 (7) |
O3—P3—C37—C42 | 167.1 (7) | O7—P7—C109—C114 | −141.5 (7) |
C49—P3—C37—C42 | 44.1 (9) | C115—P7—C109—C114 | 97.2 (8) |
C43—P3—C37—C42 | −71.8 (8) | C121—P7—C109—C114 | −17.2 (8) |
C42—C37—C38—C39 | 1.6 (14) | C114—C109—C110—C111 | −1.0 (13) |
P3—C37—C38—C39 | −174.1 (7) | P7—C109—C110—C111 | 174.7 (7) |
C37—C38—C39—C40 | −1.3 (14) | C109—C110—C111—C112 | 1.3 (14) |
C38—C39—C40—C41 | 0.7 (15) | C110—C111—C112—C113 | −0.3 (14) |
C39—C40—C41—C42 | −0.4 (15) | C111—C112—C113—C114 | −1.0 (15) |
C40—C41—C42—C37 | 0.6 (15) | C112—C113—C114—C109 | 1.3 (15) |
C38—C37—C42—C41 | −1.2 (14) | C110—C109—C114—C113 | −0.3 (13) |
P3—C37—C42—C41 | 174.2 (7) | P7—C109—C114—C113 | −175.8 (7) |
O3—P3—C43—C48 | −62.5 (8) | O7—P7—C115—C120 | −132.3 (8) |
C49—P3—C43—C48 | 60.5 (8) | C109—P7—C115—C120 | −9.6 (9) |
C37—P3—C43—C48 | 178.0 (7) | C121—P7—C115—C120 | 107.4 (8) |
O3—P3—C43—C44 | 115.1 (8) | O7—P7—C115—C116 | 50.4 (8) |
C49—P3—C43—C44 | −121.8 (8) | C109—P7—C115—C116 | 173.1 (7) |
C37—P3—C43—C44 | −4.3 (9) | C121—P7—C115—C116 | −69.9 (8) |
C48—C43—C44—C45 | 3.2 (14) | C120—C115—C116—C117 | −1.8 (14) |
P3—C43—C44—C45 | −174.4 (8) | P7—C115—C116—C117 | 175.6 (8) |
C43—C44—C45—C46 | −0.5 (15) | C115—C116—C117—C118 | 1.9 (15) |
C44—C45—C46—C47 | −2.5 (15) | C116—C117—C118—C119 | −1.2 (17) |
C45—C46—C47—C48 | 2.8 (15) | C117—C118—C119—C120 | 0.5 (18) |
C44—C43—C48—C47 | −2.8 (14) | C118—C119—C120—C115 | −0.3 (18) |
P3—C43—C48—C47 | 174.9 (7) | C116—C115—C120—C119 | 1.0 (15) |
C46—C47—C48—C43 | −0.2 (15) | P7—C115—C120—C119 | −176.2 (9) |
O3—P3—C49—C50 | −29.7 (8) | O7—P7—C121—C126 | 31.2 (9) |
C43—P3—C49—C50 | −153.1 (7) | C109—P7—C121—C126 | −93.6 (8) |
C37—P3—C49—C50 | 92.1 (8) | C115—P7—C121—C126 | 150.6 (8) |
O3—P3—C49—C54 | 150.5 (7) | O7—P7—C121—C122 | −149.6 (8) |
C43—P3—C49—C54 | 27.1 (9) | C109—P7—C121—C122 | 85.6 (8) |
C37—P3—C49—C54 | −87.7 (8) | C115—P7—C121—C122 | −30.2 (9) |
C54—C49—C50—C51 | 1.7 (14) | C126—C121—C122—C123 | −0.5 (15) |
P3—C49—C50—C51 | −178.2 (8) | P7—C121—C122—C123 | −179.7 (9) |
C49—C50—C51—C52 | −2.0 (16) | C121—C122—C123—C124 | −1.1 (17) |
C50—C51—C52—C53 | 1.0 (16) | C122—C123—C124—C125 | 0.6 (17) |
C51—C52—C53—C54 | 0.4 (16) | C123—C124—C125—C126 | 1.5 (16) |
C52—C53—C54—C49 | −0.8 (15) | C122—C121—C126—C125 | 2.6 (14) |
C50—C49—C54—C53 | −0.3 (14) | P7—C121—C126—C125 | −178.2 (8) |
P3—C49—C54—C53 | 179.6 (7) | C124—C125—C126—C121 | −3.1 (16) |
O4—P4—C55—C60 | 135.9 (8) | O8—P8—C127—C132 | 27.2 (9) |
C61—P4—C55—C60 | −102.2 (8) | C133—P8—C127—C132 | −94.4 (8) |
C67—P4—C55—C60 | 12.2 (9) | C139—P8—C127—C132 | 149.2 (8) |
O4—P4—C55—C56 | −46.9 (8) | O8—P8—C127—C128 | −155.2 (8) |
C61—P4—C55—C56 | 75.0 (8) | C133—P8—C127—C128 | 83.2 (9) |
C67—P4—C55—C56 | −170.6 (7) | C139—P8—C127—C128 | −33.2 (9) |
C60—C55—C56—C57 | 0.2 (15) | C132—C127—C128—C129 | 0.2 (14) |
P4—C55—C56—C57 | −177.1 (8) | P8—C127—C128—C129 | −177.4 (8) |
C55—C56—C57—C58 | 1.1 (18) | C127—C128—C129—C130 | 0.1 (16) |
C56—C57—C58—C59 | −1.5 (19) | C128—C129—C130—C131 | −0.6 (17) |
C57—C58—C59—C60 | 0.4 (18) | C129—C130—C131—C132 | 0.9 (17) |
C56—C55—C60—C59 | −1.2 (14) | C128—C127—C132—C131 | 0.1 (15) |
P4—C55—C60—C59 | 175.9 (7) | P8—C127—C132—C131 | 177.8 (8) |
C58—C59—C60—C55 | 0.9 (15) | C130—C131—C132—C127 | −0.6 (16) |
O4—P4—C61—C66 | −36.3 (8) | O8—P8—C133—C134 | −116.4 (8) |
C55—P4—C61—C66 | −159.9 (7) | C127—P8—C133—C134 | 2.5 (9) |
C67—P4—C61—C66 | 84.2 (8) | C139—P8—C133—C134 | 120.6 (8) |
O4—P4—C61—C62 | 143.8 (8) | O8—P8—C133—C138 | 60.1 (8) |
C55—P4—C61—C62 | 20.2 (9) | C127—P8—C133—C138 | 179.0 (7) |
C67—P4—C61—C62 | −95.8 (9) | C139—P8—C133—C138 | −62.9 (8) |
C66—C61—C62—C63 | −3.5 (15) | C138—C133—C134—C135 | −1.3 (15) |
P4—C61—C62—C63 | 176.5 (8) | P8—C133—C134—C135 | 175.2 (8) |
C61—C62—C63—C64 | 1.9 (18) | C133—C134—C135—C136 | 0.8 (16) |
C62—C63—C64—C65 | −0.6 (19) | C134—C135—C136—C137 | 0.5 (16) |
C63—C64—C65—C66 | 1.1 (18) | C135—C136—C137—C138 | −1.2 (16) |
C64—C65—C66—C61 | −2.8 (16) | C134—C133—C138—C137 | 0.6 (14) |
C62—C61—C66—C65 | 4.0 (14) | P8—C133—C138—C137 | −176.1 (7) |
P4—C61—C66—C65 | −175.9 (8) | C136—C137—C138—C133 | 0.7 (15) |
O4—P4—C67—C68 | 148.7 (8) | O8—P8—C139—C144 | 22.5 (9) |
C55—P4—C67—C68 | −86.3 (8) | C127—P8—C139—C144 | −97.2 (8) |
C61—P4—C67—C68 | 28.7 (9) | C133—P8—C139—C144 | 146.0 (8) |
O4—P4—C67—C72 | −29.8 (9) | O8—P8—C139—C140 | −156.2 (7) |
C55—P4—C67—C72 | 95.2 (9) | C127—P8—C139—C140 | 84.0 (8) |
C61—P4—C67—C72 | −149.9 (8) | C133—P8—C139—C140 | −32.8 (9) |
C72—C67—C68—C69 | −0.5 (15) | C144—C139—C140—C141 | 1.8 (14) |
P4—C67—C68—C69 | −179.0 (8) | P8—C139—C140—C141 | −179.5 (7) |
C67—C68—C69—C70 | 0.8 (16) | C139—C140—C141—C142 | −1.6 (15) |
C68—C69—C70—C71 | −1.3 (18) | C140—C141—C142—C143 | 2.3 (16) |
C69—C70—C71—C72 | 1.4 (19) | C141—C142—C143—C144 | −3.2 (17) |
C70—C71—C72—C67 | −1.1 (18) | C140—C139—C144—C143 | −2.7 (15) |
C68—C67—C72—C71 | 0.6 (16) | P8—C139—C144—C143 | 178.5 (8) |
P4—C67—C72—C71 | 179.2 (9) | C142—C143—C144—C139 | 3.5 (17) |
Experimental details
Crystal data | |
Chemical formula | [CoCl2(C18H15OP)2]·0.125CH4O |
Mr | 690.13 |
Crystal system, space group | Monoclinic, Cc |
Temperature (K) | 150 |
a, b, c (Å) | 21.3691 (3), 37.1989 (8), 19.4382 (5) |
β (°) | 120.368 (1) |
V (Å3) | 13331.4 (5) |
Z | 16 |
Radiation type | Mo Kα |
µ (mm−1) | 0.80 |
Crystal size (mm) | 0.22 × 0.12 × 0.05 |
Data collection | |
Diffractometer | Bruker–Nonius KappaCCD |
Absorption correction | Multi-scan (Blessing, 1995) |
Tmin, Tmax | 0.843, 0.961 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 13073, 13073, 9468 |
Rint | 0.095 |
(sin θ/λ)max (Å−1) | 0.617 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.059, 0.133, 1.07 |
No. of reflections | 13073 |
No. of parameters | 1559 |
No. of restraints | 2 |
H-atom treatment | H-atom parameters constrained |
w = 1/[σ2(Fo2) + (0.0321P)2 + 57.6187P] where P = (Fo2 + 2Fc2)/3 | |
Δρmax, Δρmin (e Å−3) | 0.63, −0.48 |
Absolute structure | Flack (1983) |
Absolute structure parameter | 0.40 (4) |
Computer programs: COLLECT (Nonius, 1998), SCALEPACK (Otwinowski & Minor, 1997), SCALEPACK and DENZO (Otwinowski & Minor 1997), SIR97 (Altomare et al., 1999), SHELXL97 (Sheldrick, 1997), ORTEP-3 for Windows (Farrugia, 1997) and PLATON (Spek, 2003), WinGX (Farrugia, 1999).
Cl1—Co1—O1—P1 | 110.9 (8) | Cl5—Co3—O5—P5 | −27.2 (6) |
Cl2—Co1—O1—P1 | −118.3 (8) | Cl6—Co3—O5—P5 | 102.9 (5) |
Cl1—Co1—O2—P2 | 38.4 (9) | Cl5—Co3—O6—P6 | −125.0 (6) |
Cl2—Co1—O2—P2 | −91.9 (9) | Cl6—Co3—O6—P6 | 106.2 (6) |
Cl3—Co2—O3—P3 | −21.2 (8) | Cl7—Co4—O7—P7 | 128.4 (6) |
Cl4—Co2—O3—P3 | 109.5 (7) | Cl8—Co4—O7—P7 | −97.6 (6) |
Cl3—Co2—O4—P4 | −147.4 (6) | Cl7—Co4—O8—P8 | 42.1 (8) |
Cl4—Co2—O4—P4 | 87.5 (7) | Cl8—Co4—O8—P8 | −91.9 (7) |
(I)* range | (I) average | (IIa) | (IIb) | |
Co-Cl (Å) | 2.221 (3)-2.260 (3) | 2.242 | 2.227 (1) | 2.203 (3) |
Co-O (Å) | 1.952 (6)-1.988 (6) | 1.971 | 1.971 (2) | 1.998 (7) |
Cl-Co-Cl (°) | 116.4 (1)-123.6 (1) | 119.7 | 112.76 (6) | 114.1 (1) |
O-Co-O (°) | 104.3 (3)-107.2 (2) | 105.3 | 97.9 (2) | 96.3 (3) |
Co-O-P (°) | 138.4 (4)-154.3 (4) | 145.8 | 153.6 (2) | 152.6 (5) |
*(I) refers to the title structure and (II) to the usolvated complex, (IIa) Cotton et al. (2002) and (IIb) Marsh (1997) with e.s.ds taken from Mangion et al. (1976) |
The title methanol solvate crystallized when a methanolic solution of CoCl2(OPPh3)2, contained in a 0.7 mm tube, was subjected to vapour diffusion using Et2O anti-solvent. The more common unsolvated crystals formed when a 10 mm diameter tube was used.
All unsolvated 1st row d-block MCl2(OPPh3)2 crystal structures are isostructural, crystallizing in orthorhombic space group Fdd2 with each molecule having strict crystallographic C2 symmetry In each case the O—P bonds project into the region between the two Cl ligands with a stagger angle ranging from 36.8 (2) to 42.3 (4)°, as measured by the P—O—M—Cl torsion angles. This contrasts with the situation in the only previously reported solvated structure, a Zn complex containing THF of crystallization, in which the two P atoms nearly eclipse the Zn—Cl bonds with P—O—Zn—Cl torsion angles of 8.3 (2) and 8.8 (2)°. In this case the O—P bonds project into a region just outside the range subtended by the two Cl atoms.
The four crystallographically distinct CoCl2(OPPh3)2 molecules, which comprise the title structure (Figs. 1–5), have simmilar configurations to each other but differ from the above structures. In each case one O—P bond projects into the region between the two Cl atoms (P—O—Co—Cl 21.2 (8) to 42.1 (8)°), and the other is directed away (P—O—Co—Cl 110.9 (8) to 147.4 (6)°). Comparison of the pseudo-tetrahedral geometry in the title structure with that in the unsolvated Co structures shows that the above torsional changes are accompanied by other significant bond length and angle changes (Table 1).
The lamelar nature of the title structure can be seen in the packing digrams (Fig. 6). The methanol, which semi-populates its interlayer sites and displays high vibrational amplitudes, does not form well defined interactions with the host molecules. Furthermore residual voids (total 35 Å3) in the interlayer region suggest that solvent molecules may have been lost after crystallization.
It is interesting to speculate what role the narrower crystallization container may have had in directing the formation of this lamelar solvate. As a greater depth of anti-solvent was attained in the narrower 0.7 mm crystallization tube, compared to what was achieved in the 10 mm bore tube, it would seem reasonable to suggest that the a mixed Et2O/MeOH solvate may have been formed initially, with the reported structure resulting from partial solvent loss.