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
Key indicators
- Single-crystal X-ray study
- T = 150 K
- Mean (C-C) = 0.017 Å
- Disorder in solvent or counterion
- R factor = 0.059
- wR factor = 0.133
- Data-to-parameter ratio = 8.4
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT220_ALERT_2_B Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.62 Ratio PLAT341_ALERT_3_B Low Bond Precision on C-C Bonds (x 1000) Ang ... 17
Alert level C STRVA01_ALERT_4_C Flack test results are ambiguous. From the CIF: _refine_ls_abs_structure_Flack 0.400 From the CIF: _refine_ls_abs_structure_Flack_su 0.040 PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 0.12 Ratio PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ? PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ? PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.12 Ratio PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.88 Ratio PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.24 Ratio PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C105 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C143 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Co2 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Co3 PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 50.00 Perc.
Alert level G REFLT03_ALERT_4_G WARNING: Large fraction of Friedel related reflns may be needed to determine absolute structure From the CIF: _diffrn_reflns_theta_max 26.00 From the CIF: _reflns_number_total 13073 Count of symmetry unique reflns 13112 Completeness (_total/calc) 99.70% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 0 Fraction of Friedel pairs measured 0.000 Are heavy atom types Z>Si present yes PLAT033_ALERT_2_G Flack Parameter Value Deviates 2 * su from zero. 0.40 PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 2
0 ALERT level A = In general: serious problem 2 ALERT level B = Potentially serious problem 14 ALERT level C = Check and explain 3 ALERT level G = General alerts; check 4 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 8 ALERT type 2 Indicator that the structure model may be wrong or deficient 3 ALERT type 3 Indicator that the structure quality may be low 4 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
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).
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) |
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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.