Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536801010893/bt6052sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536801010893/bt6052Isup2.hkl |
CCDC reference: 170863
Complex (1) (220 mg, 0.203 mmol) was suspended in benzene (20 ml) and the suspension stirred under an atmosphere of dry nitrogen. IR monitoring of the reaction revealed a gradual increase in intensity of the ν(N≡N) and ν(C≡O) absorption of the product (2) at 2071 and 1801 cm-1, respectively, and of the ν(C═O) absorption of uncoordinated DMF at 1684 cm-1. After approximately 10 h, all starting material had dissolved and the colour of the solution had changed from red to orange. Pentane (25 ml) was then added to the solution to precipitate complex (2) as an orange solid, which was washed with pentane (2 x 5 ml) and dried in vacuo at 253 K. The supernatant solution was combined with the pentane washings and allowed to stand for one day at ambient temperature to afford yellow crystals of (3a). IR of the crystals (KBr, cm-1): 1852 (versus), 1778 (versus) [ν(C≡O)]; (THF, cm-1): 1857 (versus), 1795 (s) [ν(C≡O]; (C6H6, cm-1): 1857(versus), 1795 (s) [ν(C≡O)]. During data collection the crystal was in cold N2 gas of the Cryostream cooler (Oxford Cryosystems, 1992) mounted on a φ-axis diffractometer supplied with an area detector.
Reaction of the germylenes Cp*GeX (Cp* = C5Me5; X = Cl, Br, I) with the bis-dinitrogen complex trans-[W(dppe)2(N2)2] has been recently shown to provide a convenient route to the complexes trans-[X(dppe)2W≡Ge(η1-Cp*)] (X = Cl, Br, I) bearing a transition metal–germanium triple bond (Filippou et al., 2000). In order to test the influence of a carbonyl ligand on the course of this reaction, the dinitrogen complex trans-[W(CO)(N2)(dppe)2], (2), was prepared from trans-[W(CO)(DMF)(dppe)2] (DMF is N,N'-dimethylformamide), (1) (Ishida et al., 1991). Yellow single crystals of the title compound, (3), as benzene sesquisolvate (1.5C6H6), (3a), were obtained from the washing solution after the isolation of complex (2).
Complex (3) was first prepared by Chatt & Watson (1961), however, its molecular structure in the solid state was unknown to this day. Two distorted octahedral molecules with marginally different bonding parameters and three molecules of benzene are present in the asymmetric unit of the cell. The W—P bonds trans to the carbonyl ligands have an average value of 2.5490 (9) Å, which is considerably larger than that of the W—P bonds cis to the carbonyl ligands [2.4525 (9) Å] indicating the strong trans influence of the CO groups.
Data collection: IPDS2.87 (Stoe & Cie, 1997); cell refinement: IPDS2.87; data reduction: IPDS2.87; program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 1996); software used to prepare material for publication: SHELXL97.
[W(CO)2(C26H24P2)2]·1.5C6H6 | Z = 4 |
Mr = 1153.82 | F(000) = 2340 |
Triclinic, P1 | Dx = 1.486 Mg m−3 |
a = 12.675 (2) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 18.259 (3) Å | Cell parameters from 5000 reflections |
c = 22.864 (4) Å | θ = 2.5–25.0° |
α = 89.15 (2)° | µ = 2.41 mm−1 |
β = 87.73 (2)° | T = 180 K |
γ = 77.31 (2)° | Block, yellow |
V = 5158.1 (16) Å3 | 0.40 × 0.24 × 0.12 mm |
Stoe IPDS diffractometer | 18050 independent reflections |
Radiation source: fine-focus sealed X-ray tube | 15173 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.034 |
Detector resolution: 6.667 pixels mm-1 | θmax = 25.5°, θmin = 2.2° |
φ–oscillat., φ–incr. = 1.1°, 218 exposures scans | h = −15→15 |
Absorption correction: numerical (NUMABS32 in X-RED1.08; Stoe & Cie, 1997) | k = −22→22 |
Tmin = 0.446, Tmax = 0.761 | l = −27→27 |
47419 measured reflections |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.022 | H-atom parameters not refined |
wR(F2) = 0.053 | w = 1/[σ2(Fo2) + (0.0344P)2] where P = (Fo2 + 2Fc2)/3 |
S = 0.94 | (Δ/σ)max = 0.020 |
18050 reflections | Δρmax = 0.70 e Å−3 |
1262 parameters | Δρmin = −1.27 e Å−3 |
0 restraints | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.00038 (5) |
[W(CO)2(C26H24P2)2]·1.5C6H6 | γ = 77.31 (2)° |
Mr = 1153.82 | V = 5158.1 (16) Å3 |
Triclinic, P1 | Z = 4 |
a = 12.675 (2) Å | Mo Kα radiation |
b = 18.259 (3) Å | µ = 2.41 mm−1 |
c = 22.864 (4) Å | T = 180 K |
α = 89.15 (2)° | 0.40 × 0.24 × 0.12 mm |
β = 87.73 (2)° |
Stoe IPDS diffractometer | 18050 independent reflections |
Absorption correction: numerical (NUMABS32 in X-RED1.08; Stoe & Cie, 1997) | 15173 reflections with I > 2σ(I) |
Tmin = 0.446, Tmax = 0.761 | Rint = 0.034 |
47419 measured reflections |
R[F2 > 2σ(F2)] = 0.022 | 0 restraints |
wR(F2) = 0.053 | H-atom parameters not refined |
S = 0.94 | Δρmax = 0.70 e Å−3 |
18050 reflections | Δρmin = −1.27 e Å−3 |
1262 parameters |
Experimental. Crystal faces were indexed by microscope on the diffractometer. After that a numerical absorption correction basing on Gaussian integration was applied. NUMABS32 is implemented in X-RED1.08 (Stoe, 1997). Recrystallized from benzene/pentane. |
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
x | y | z | Uiso*/Ueq | ||
C1 | 0.0567 (2) | 0.08281 (14) | 0.00638 (13) | 0.0207 (6) | |
H1A | 0.0912 | 0.0421 | −0.0208 | 0.025* | |
H1B | 0.0054 | 0.0635 | 0.0330 | 0.025* | |
C2 | −0.0045 (2) | 0.15016 (15) | −0.02841 (13) | 0.0218 (6) | |
H2A | −0.0644 | 0.1360 | −0.0488 | 0.026* | |
H2B | 0.0451 | 0.1658 | −0.0582 | 0.026* | |
C3 | 0.0797 (2) | 0.41255 (14) | 0.01953 (12) | 0.0178 (6) | |
H3A | 0.1127 | 0.4481 | −0.0041 | 0.021* | |
H3B | 0.0073 | 0.4133 | 0.0044 | 0.021* | |
C4 | 0.0687 (2) | 0.43615 (13) | 0.08380 (12) | 0.0177 (6) | |
H4A | 0.0152 | 0.4844 | 0.0880 | 0.021* | |
H4B | 0.1391 | 0.4436 | 0.0968 | 0.021* | |
C5 | 0.2212 (2) | 0.21815 (14) | 0.13778 (12) | 0.0204 (6) | |
C6 | 0.0211 (2) | 0.20042 (14) | 0.15866 (13) | 0.0184 (6) | |
C7 | 0.2809 (2) | 0.09249 (14) | −0.00053 (12) | 0.0193 (6) | |
C8 | 0.3761 (2) | 0.10931 (16) | 0.01877 (13) | 0.0260 (7) | |
H8 | 0.3771 | 0.1298 | 0.0567 | 0.031* | |
C9 | 0.4693 (3) | 0.09624 (19) | −0.01714 (16) | 0.0354 (8) | |
H9 | 0.5336 | 0.1075 | −0.0033 | 0.042* | |
C10 | 0.4699 (3) | 0.06689 (17) | −0.07299 (15) | 0.0332 (7) | |
H10 | 0.5336 | 0.0590 | −0.0975 | 0.040* | |
C11 | 0.3770 (3) | 0.04948 (16) | −0.09217 (14) | 0.0294 (7) | |
H11 | 0.3766 | 0.0287 | −0.1300 | 0.035* | |
C12 | 0.2837 (2) | 0.06221 (15) | −0.05641 (13) | 0.0257 (7) | |
H12 | 0.2201 | 0.0500 | −0.0703 | 0.031* | |
C13 | 0.1974 (2) | 0.02836 (14) | 0.09817 (13) | 0.0220 (6) | |
C14 | 0.2278 (2) | −0.04351 (15) | 0.07374 (15) | 0.0295 (7) | |
H14 | 0.2327 | −0.0493 | 0.0324 | 0.035* | |
C15 | 0.2510 (3) | −0.10671 (17) | 0.11016 (18) | 0.0381 (9) | |
H15 | 0.2716 | −0.1553 | 0.0934 | 0.046* | |
C16 | 0.2441 (3) | −0.09905 (18) | 0.17042 (18) | 0.0405 (9) | |
H16 | 0.2591 | −0.1423 | 0.1949 | 0.049* | |
C17 | 0.2154 (3) | −0.02848 (18) | 0.19474 (16) | 0.0358 (8) | |
H17 | 0.2116 | −0.0230 | 0.2361 | 0.043* | |
C18 | 0.1919 (2) | 0.03520 (16) | 0.15853 (14) | 0.0281 (7) | |
H18 | 0.1720 | 0.0836 | 0.1756 | 0.034* | |
C19 | 0.2981 (2) | 0.34186 (14) | 0.02100 (13) | 0.0206 (6) | |
C20 | 0.3365 (2) | 0.34696 (15) | 0.07702 (14) | 0.0249 (6) | |
H20 | 0.2995 | 0.3309 | 0.1101 | 0.030* | |
C21 | 0.4286 (2) | 0.37544 (17) | 0.08486 (16) | 0.0322 (8) | |
H21 | 0.4534 | 0.3793 | 0.1231 | 0.039* | |
C22 | 0.4836 (3) | 0.39792 (17) | 0.03703 (17) | 0.0362 (8) | |
H22 | 0.5461 | 0.4175 | 0.0423 | 0.043* | |
C23 | 0.4478 (3) | 0.39197 (19) | −0.01862 (17) | 0.0396 (8) | |
H23 | 0.4864 | 0.4066 | −0.0517 | 0.048* | |
C24 | 0.3548 (3) | 0.36448 (18) | −0.02630 (15) | 0.0323 (7) | |
H24 | 0.3300 | 0.3613 | −0.0647 | 0.039* | |
C25 | 0.1674 (2) | 0.30082 (14) | −0.06597 (13) | 0.0209 (6) | |
C26 | 0.2468 (3) | 0.24288 (16) | −0.09088 (14) | 0.0293 (7) | |
H26 | 0.2994 | 0.2131 | −0.0668 | 0.035* | |
C27 | 0.2493 (3) | 0.22869 (18) | −0.15056 (15) | 0.0408 (9) | |
H27 | 0.3031 | 0.1888 | −0.1668 | 0.049* | |
C28 | 0.1745 (3) | 0.27201 (18) | −0.18664 (14) | 0.0414 (9) | |
H28 | 0.1774 | 0.2623 | −0.2274 | 0.050* | |
C29 | 0.0963 (3) | 0.32897 (18) | −0.16305 (14) | 0.0351 (8) | |
H29 | 0.0449 | 0.3590 | −0.1876 | 0.042* | |
C30 | 0.0918 (3) | 0.34320 (15) | −0.10273 (13) | 0.0249 (6) | |
H30 | 0.0364 | 0.3823 | −0.0867 | 0.030* | |
C31 | −0.1257 (2) | 0.30292 (15) | −0.02895 (13) | 0.0218 (6) | |
C32 | −0.1301 (3) | 0.29034 (18) | −0.08864 (14) | 0.0313 (7) | |
H32 | −0.0964 | 0.2427 | −0.1044 | 0.038* | |
C33 | −0.1837 (3) | 0.34719 (19) | −0.12579 (15) | 0.0393 (9) | |
H33 | −0.1853 | 0.3382 | −0.1665 | 0.047* | |
C34 | −0.2343 (3) | 0.41665 (18) | −0.10284 (16) | 0.0390 (9) | |
H34 | −0.2707 | 0.4553 | −0.1279 | 0.047* | |
C35 | −0.2316 (3) | 0.42948 (16) | −0.04326 (16) | 0.0323 (8) | |
H35 | −0.2672 | 0.4767 | −0.0275 | 0.039* | |
C36 | −0.1769 (2) | 0.37336 (15) | −0.00637 (14) | 0.0249 (7) | |
H36 | −0.1743 | 0.3829 | 0.0342 | 0.030* | |
C37 | −0.1807 (2) | 0.19977 (14) | 0.05331 (13) | 0.0197 (6) | |
C38 | −0.2846 (2) | 0.22993 (15) | 0.03403 (14) | 0.0261 (7) | |
H38 | −0.2944 | 0.2673 | 0.0042 | 0.031* | |
C39 | −0.3734 (2) | 0.20602 (17) | 0.05780 (16) | 0.0336 (8) | |
H39 | −0.4437 | 0.2277 | 0.0447 | 0.040* | |
C40 | −0.3604 (3) | 0.15053 (18) | 0.10079 (16) | 0.0362 (8) | |
H40 | −0.4214 | 0.1339 | 0.1168 | 0.043* | |
C41 | −0.2578 (3) | 0.11967 (18) | 0.12008 (15) | 0.0333 (7) | |
H41 | −0.2482 | 0.0813 | 0.1491 | 0.040* | |
C42 | −0.1693 (2) | 0.14455 (15) | 0.09729 (13) | 0.0244 (6) | |
H42 | −0.0996 | 0.1239 | 0.1116 | 0.029* | |
C43 | −0.1228 (2) | 0.40100 (15) | 0.14248 (12) | 0.0196 (6) | |
C44 | −0.1702 (2) | 0.47767 (15) | 0.14474 (13) | 0.0248 (6) | |
H44 | −0.1258 | 0.5132 | 0.1396 | 0.030* | |
C45 | −0.2808 (3) | 0.50274 (18) | 0.15430 (15) | 0.0350 (8) | |
H45 | −0.3116 | 0.5551 | 0.1555 | 0.042* | |
C46 | −0.3460 (3) | 0.45221 (19) | 0.16202 (15) | 0.0365 (8) | |
H46 | −0.4219 | 0.4695 | 0.1682 | 0.044* | |
C47 | −0.3005 (3) | 0.37595 (19) | 0.16080 (15) | 0.0341 (8) | |
H47 | −0.3454 | 0.3409 | 0.1667 | 0.041* | |
C48 | −0.1898 (2) | 0.35059 (16) | 0.15104 (14) | 0.0265 (7) | |
H48 | −0.1594 | 0.2982 | 0.1502 | 0.032* | |
C49 | 0.0672 (2) | 0.38774 (14) | 0.20284 (12) | 0.0182 (6) | |
C50 | 0.0819 (2) | 0.33411 (15) | 0.24794 (12) | 0.0228 (6) | |
H50 | 0.0764 | 0.2842 | 0.2400 | 0.027* | |
C51 | 0.1045 (3) | 0.35286 (16) | 0.30442 (13) | 0.0287 (7) | |
H51 | 0.1144 | 0.3158 | 0.3345 | 0.034* | |
C52 | 0.1126 (3) | 0.42533 (16) | 0.31644 (14) | 0.0300 (7) | |
H52 | 0.1263 | 0.4384 | 0.3550 | 0.036* | |
C53 | 0.1009 (3) | 0.47881 (16) | 0.27235 (14) | 0.0312 (8) | |
H53 | 0.1081 | 0.5283 | 0.2804 | 0.037* | |
C54 | 0.0785 (2) | 0.45995 (15) | 0.21605 (13) | 0.0263 (7) | |
H54 | 0.0708 | 0.4970 | 0.1860 | 0.032* | |
C55 | 0.3289 (3) | 0.0429 (2) | −0.25960 (15) | 0.0408 (9) | |
H55 | 0.2581 | 0.0681 | −0.2697 | 0.049* | |
C56 | 0.3534 (3) | −0.0336 (2) | −0.25133 (17) | 0.0478 (10) | |
H56 | 0.2996 | −0.0617 | −0.2565 | 0.057* | |
C57 | 0.4564 (4) | −0.0699 (2) | −0.23546 (18) | 0.0527 (11) | |
H57 | 0.4731 | −0.1227 | −0.2296 | 0.063* | |
C58 | 0.5336 (3) | −0.0297 (2) | −0.22824 (17) | 0.0473 (10) | |
H58 | 0.6040 | −0.0544 | −0.2170 | 0.057* | |
C59 | 0.5094 (3) | 0.0471 (2) | −0.23737 (15) | 0.0374 (8) | |
H59 | 0.5632 | 0.0752 | −0.2327 | 0.045* | |
C60 | 0.4077 (3) | 0.08256 (19) | −0.25310 (15) | 0.0352 (8) | |
H60 | 0.3915 | 0.1353 | −0.2596 | 0.042* | |
C64 | 0.0622 (2) | 0.06863 (13) | 0.51810 (12) | 0.0174 (6) | |
H64A | −0.0079 | 0.0915 | 0.5008 | 0.021* | |
H64B | 0.0963 | 0.0232 | 0.4954 | 0.021* | |
C65 | 0.0443 (2) | 0.04766 (14) | 0.58212 (12) | 0.0178 (6) | |
H65A | 0.1137 | 0.0206 | 0.5981 | 0.021* | |
H65B | −0.0072 | 0.0140 | 0.5849 | 0.021* | |
C66 | 0.0627 (2) | 0.40574 (14) | 0.50395 (13) | 0.0196 (6) | |
H66A | 0.0112 | 0.4432 | 0.5279 | 0.024* | |
H66B | 0.1074 | 0.4329 | 0.4790 | 0.024* | |
C67 | 0.0002 (2) | 0.36402 (15) | 0.46533 (13) | 0.0221 (6) | |
H67A | 0.0506 | 0.3343 | 0.4359 | 0.026* | |
H67B | −0.0546 | 0.4008 | 0.4442 | 0.026* | |
C68 | −0.0245 (2) | 0.30023 (14) | 0.64989 (13) | 0.0217 (6) | |
C69 | 0.1780 (2) | 0.22006 (13) | 0.64331 (12) | 0.0186 (6) | |
C70 | 0.2775 (2) | 0.06683 (14) | 0.53169 (12) | 0.0176 (6) | |
C71 | 0.3289 (2) | 0.06565 (16) | 0.58430 (14) | 0.0273 (7) | |
H71 | 0.3058 | 0.1056 | 0.6113 | 0.033* | |
C72 | 0.4146 (3) | 0.00592 (19) | 0.59785 (14) | 0.0350 (8) | |
H72 | 0.4499 | 0.0058 | 0.6337 | 0.042* | |
C73 | 0.4480 (2) | −0.05278 (17) | 0.55915 (15) | 0.0324 (8) | |
H73 | 0.5049 | −0.0939 | 0.5689 | 0.039* | |
C74 | 0.3982 (2) | −0.05153 (16) | 0.50626 (15) | 0.0301 (7) | |
H74 | 0.4218 | −0.0915 | 0.4794 | 0.036* | |
C75 | 0.3144 (2) | 0.00773 (15) | 0.49241 (14) | 0.0246 (6) | |
H75 | 0.2814 | 0.0084 | 0.4558 | 0.029* | |
C76 | 0.1744 (2) | 0.14707 (13) | 0.43603 (12) | 0.0173 (6) | |
C77 | 0.1037 (2) | 0.13361 (14) | 0.39429 (13) | 0.0215 (6) | |
H77 | 0.0373 | 0.1211 | 0.4066 | 0.026* | |
C78 | 0.1294 (3) | 0.13829 (15) | 0.33421 (13) | 0.0277 (7) | |
H78 | 0.0804 | 0.1291 | 0.3063 | 0.033* | |
C79 | 0.2251 (3) | 0.15604 (16) | 0.31569 (13) | 0.0301 (7) | |
H79 | 0.2430 | 0.1582 | 0.2751 | 0.036* | |
C80 | 0.2957 (3) | 0.17075 (16) | 0.35656 (14) | 0.0288 (7) | |
H80 | 0.3615 | 0.1837 | 0.3438 | 0.035* | |
C81 | 0.2705 (2) | 0.16667 (15) | 0.41636 (13) | 0.0231 (6) | |
H81 | 0.3191 | 0.1773 | 0.4440 | 0.028* | |
C82 | −0.1197 (2) | 0.25116 (14) | 0.45073 (13) | 0.0210 (6) | |
C83 | −0.1128 (2) | 0.26995 (16) | 0.39135 (13) | 0.0278 (7) | |
H83 | −0.0814 | 0.3108 | 0.3798 | 0.033* | |
C84 | −0.1514 (3) | 0.22957 (18) | 0.34889 (15) | 0.0369 (8) | |
H84 | −0.1454 | 0.2428 | 0.3088 | 0.044* | |
C85 | −0.1981 (3) | 0.17070 (19) | 0.36474 (16) | 0.0399 (9) | |
H85 | −0.2229 | 0.1425 | 0.3357 | 0.048* | |
C86 | −0.2089 (2) | 0.15275 (17) | 0.42388 (16) | 0.0328 (8) | |
H86 | −0.2433 | 0.1132 | 0.4352 | 0.039* | |
C87 | −0.1695 (2) | 0.19239 (15) | 0.46638 (14) | 0.0260 (7) | |
H87 | −0.1766 | 0.1793 | 0.5065 | 0.031* | |
C88 | −0.1951 (2) | 0.36705 (14) | 0.53337 (13) | 0.0202 (6) | |
C89 | −0.2944 (2) | 0.36600 (16) | 0.51039 (14) | 0.0273 (7) | |
H89 | −0.2989 | 0.3296 | 0.4818 | 0.033* | |
C90 | −0.3881 (3) | 0.41777 (17) | 0.52870 (16) | 0.0348 (8) | |
H90 | −0.4556 | 0.4161 | 0.5127 | 0.042* | |
C91 | −0.3828 (3) | 0.47109 (17) | 0.56977 (15) | 0.0347 (8) | |
H91 | −0.4462 | 0.5067 | 0.5818 | 0.042* | |
C92 | −0.2840 (3) | 0.47250 (16) | 0.59344 (15) | 0.0293 (7) | |
H92 | −0.2799 | 0.5093 | 0.6217 | 0.035* | |
C93 | −0.1915 (2) | 0.42066 (15) | 0.57620 (13) | 0.0238 (6) | |
H93 | −0.1248 | 0.4213 | 0.5935 | 0.029* | |
C94 | 0.1848 (2) | 0.40720 (14) | 0.60417 (13) | 0.0199 (6) | |
C95 | 0.1554 (2) | 0.40619 (16) | 0.66344 (14) | 0.0279 (7) | |
H95 | 0.1217 | 0.3678 | 0.6784 | 0.034* | |
C96 | 0.1749 (3) | 0.46077 (18) | 0.70117 (15) | 0.0346 (8) | |
H96 | 0.1544 | 0.4593 | 0.7415 | 0.042* | |
C97 | 0.2235 (3) | 0.51665 (17) | 0.68011 (16) | 0.0346 (8) | |
H97 | 0.2360 | 0.5541 | 0.7057 | 0.042* | |
C98 | 0.2543 (3) | 0.51797 (17) | 0.62115 (16) | 0.0360 (8) | |
H98 | 0.2881 | 0.5564 | 0.6065 | 0.043* | |
C99 | 0.2359 (3) | 0.46323 (15) | 0.58350 (14) | 0.0291 (7) | |
H99 | 0.2584 | 0.4641 | 0.5434 | 0.035* | |
C100 | 0.2806 (2) | 0.31550 (13) | 0.51004 (13) | 0.0189 (6) | |
C101 | 0.3709 (2) | 0.27392 (15) | 0.53816 (14) | 0.0251 (7) | |
H101 | 0.3642 | 0.2585 | 0.5777 | 0.030* | |
C102 | 0.4702 (2) | 0.25534 (16) | 0.50807 (15) | 0.0305 (7) | |
H102 | 0.5315 | 0.2279 | 0.5275 | 0.037* | |
C103 | 0.4814 (3) | 0.27612 (17) | 0.45033 (15) | 0.0324 (7) | |
H103 | 0.5497 | 0.2625 | 0.4300 | 0.039* | |
C104 | 0.3921 (2) | 0.31720 (16) | 0.42196 (14) | 0.0287 (7) | |
H104 | 0.3991 | 0.3320 | 0.3822 | 0.034* | |
C105 | 0.2926 (2) | 0.33646 (15) | 0.45204 (13) | 0.0242 (6) | |
H105 | 0.2318 | 0.3645 | 0.4325 | 0.029* | |
C106 | 0.0211 (2) | 0.09898 (14) | 0.70056 (12) | 0.0185 (6) | |
C107 | 0.0392 (2) | 0.02238 (15) | 0.71493 (13) | 0.0233 (6) | |
H107 | 0.0395 | −0.0132 | 0.6850 | 0.028* | |
C108 | 0.0567 (2) | −0.00221 (16) | 0.77250 (14) | 0.0291 (7) | |
H108 | 0.0687 | −0.0543 | 0.7815 | 0.035* | |
C109 | 0.0565 (3) | 0.04919 (17) | 0.81662 (14) | 0.0297 (7) | |
H109 | 0.0673 | 0.0326 | 0.8559 | 0.036* | |
C110 | 0.0406 (3) | 0.12476 (17) | 0.80302 (14) | 0.0312 (7) | |
H110 | 0.0423 | 0.1600 | 0.8329 | 0.037* | |
C111 | 0.0221 (2) | 0.14937 (15) | 0.74560 (13) | 0.0251 (7) | |
H111 | 0.0099 | 0.2016 | 0.7370 | 0.030* | |
C112 | −0.1572 (2) | 0.13844 (15) | 0.62982 (12) | 0.0185 (6) | |
C113 | −0.2295 (2) | 0.20760 (17) | 0.62562 (14) | 0.0286 (7) | |
H113 | −0.2028 | 0.2518 | 0.6187 | 0.034* | |
C114 | −0.3401 (3) | 0.21248 (19) | 0.63138 (16) | 0.0385 (8) | |
H114 | −0.3886 | 0.2600 | 0.6282 | 0.046* | |
C115 | −0.3799 (3) | 0.1493 (2) | 0.64160 (16) | 0.0379 (8) | |
H115 | −0.4558 | 0.1530 | 0.6455 | 0.046* | |
C116 | −0.3092 (2) | 0.07998 (18) | 0.64617 (14) | 0.0308 (7) | |
H116 | −0.3365 | 0.0361 | 0.6536 | 0.037* | |
C117 | −0.1991 (2) | 0.07481 (16) | 0.63996 (13) | 0.0249 (6) | |
H117 | −0.1511 | 0.0271 | 0.6426 | 0.030* | |
C118 | 0.3829 (3) | 0.3607 (2) | 0.24672 (16) | 0.0421 (9) | |
H118 | 0.3154 | 0.3673 | 0.2285 | 0.050* | |
C119 | 0.4170 (3) | 0.4222 (2) | 0.26757 (17) | 0.0425 (9) | |
H119 | 0.3728 | 0.4711 | 0.2638 | 0.051* | |
C120 | 0.5155 (3) | 0.4120 (2) | 0.29381 (17) | 0.0420 (9) | |
H120 | 0.5394 | 0.4542 | 0.3077 | 0.050* | |
C121 | 0.5789 (3) | 0.3412 (2) | 0.29997 (17) | 0.0428 (9) | |
H121 | 0.6463 | 0.3343 | 0.3184 | 0.051* | |
C122 | 0.5445 (3) | 0.2800 (2) | 0.27924 (19) | 0.0483 (10) | |
H122 | 0.5883 | 0.2309 | 0.2835 | 0.058* | |
C123 | 0.4472 (3) | 0.2900 (2) | 0.25258 (18) | 0.0466 (9) | |
H123 | 0.4242 | 0.2478 | 0.2381 | 0.056* | |
C124 | −0.4182 (6) | 0.3112 (3) | −0.1971 (3) | 0.103 (2) | |
H124 | −0.3752 | 0.2960 | −0.1641 | 0.124* | |
C125 | −0.3828 (6) | 0.3547 (4) | −0.2418 (3) | 0.118 (3) | |
H125 | −0.3145 | 0.3677 | −0.2400 | 0.141* | |
C126 | −0.4465 (5) | 0.3778 (3) | −0.2874 (3) | 0.0836 (17) | |
H126 | −0.4232 | 0.4088 | −0.3167 | 0.100* | |
C127 | −0.5429 (4) | 0.3582 (3) | −0.2927 (2) | 0.0693 (14) | |
H127 | −0.5862 | 0.3739 | −0.3255 | 0.083* | |
C128 | −0.5753 (4) | 0.3155 (3) | −0.2497 (3) | 0.0844 (17) | |
H128 | −0.6426 | 0.3011 | −0.2523 | 0.101* | |
C129 | −0.5119 (5) | 0.2919 (3) | −0.2014 (3) | 0.0929 (19) | |
H129 | −0.5363 | 0.2620 | −0.1717 | 0.111* | |
O1 | 0.29683 (17) | 0.20155 (12) | 0.16661 (10) | 0.0333 (5) | |
O2 | −0.01867 (18) | 0.18177 (11) | 0.20206 (9) | 0.0274 (5) | |
O3 | −0.07439 (19) | 0.33201 (11) | 0.68894 (10) | 0.0328 (5) | |
O4 | 0.24602 (18) | 0.21534 (11) | 0.67749 (9) | 0.0330 (5) | |
P1 | 0.16134 (5) | 0.11139 (3) | 0.04946 (3) | 0.01610 (14) | |
P2 | 0.16596 (5) | 0.31656 (3) | 0.01343 (3) | 0.01513 (14) | |
P3 | −0.05951 (5) | 0.22916 (4) | 0.02246 (3) | 0.01666 (15) | |
P4 | 0.02454 (5) | 0.36378 (3) | 0.13046 (3) | 0.01466 (14) | |
P5 | 0.15145 (5) | 0.13630 (3) | 0.51568 (3) | 0.01438 (14) | |
P6 | −0.06789 (5) | 0.30062 (4) | 0.50950 (3) | 0.01712 (15) | |
P7 | 0.15107 (5) | 0.33925 (3) | 0.55260 (3) | 0.01510 (14) | |
P8 | −0.01016 (5) | 0.13389 (3) | 0.62530 (3) | 0.01491 (14) | |
W1 | 0.092175 (8) | 0.237475 (5) | 0.090426 (4) | 0.01303 (4) | |
W2 | 0.063529 (8) | 0.239684 (5) | 0.587227 (4) | 0.01369 (4) |
U11 | U22 | U33 | U12 | U13 | U23 | |
C1 | 0.0218 (14) | 0.0192 (13) | 0.0226 (16) | −0.0069 (10) | −0.0026 (13) | −0.0053 (11) |
C2 | 0.0208 (14) | 0.0253 (14) | 0.0207 (15) | −0.0072 (11) | −0.0040 (12) | −0.0019 (11) |
C3 | 0.0197 (13) | 0.0169 (12) | 0.0177 (15) | −0.0062 (10) | −0.0007 (12) | 0.0019 (10) |
C4 | 0.0195 (13) | 0.0144 (12) | 0.0196 (15) | −0.0049 (10) | 0.0010 (12) | −0.0022 (10) |
C5 | 0.0294 (15) | 0.0146 (12) | 0.0181 (15) | −0.0074 (10) | 0.0021 (13) | −0.0017 (10) |
C6 | 0.0232 (14) | 0.0139 (12) | 0.0193 (16) | −0.0055 (10) | −0.0043 (13) | −0.0030 (11) |
C7 | 0.0231 (14) | 0.0154 (12) | 0.0199 (15) | −0.0049 (10) | −0.0018 (12) | 0.0018 (11) |
C8 | 0.0247 (15) | 0.0325 (15) | 0.0220 (16) | −0.0078 (12) | −0.0041 (13) | −0.0053 (12) |
C9 | 0.0226 (16) | 0.0487 (19) | 0.036 (2) | −0.0107 (14) | −0.0030 (15) | −0.0049 (15) |
C10 | 0.0285 (17) | 0.0375 (17) | 0.0324 (19) | −0.0059 (13) | 0.0084 (15) | −0.0030 (14) |
C11 | 0.0342 (17) | 0.0303 (15) | 0.0231 (17) | −0.0061 (13) | 0.0027 (14) | −0.0054 (13) |
C12 | 0.0289 (16) | 0.0267 (14) | 0.0234 (16) | −0.0096 (12) | −0.0010 (14) | −0.0057 (12) |
C13 | 0.0183 (14) | 0.0199 (13) | 0.0288 (17) | −0.0062 (10) | −0.0030 (13) | 0.0052 (11) |
C14 | 0.0335 (17) | 0.0203 (14) | 0.0356 (19) | −0.0069 (12) | −0.0071 (15) | 0.0013 (12) |
C15 | 0.0358 (18) | 0.0200 (15) | 0.060 (3) | −0.0083 (12) | −0.0117 (18) | 0.0071 (15) |
C16 | 0.0330 (18) | 0.0320 (17) | 0.057 (3) | −0.0088 (13) | −0.0124 (18) | 0.0254 (16) |
C17 | 0.0326 (18) | 0.0431 (19) | 0.0295 (19) | −0.0043 (14) | −0.0025 (16) | 0.0157 (15) |
C18 | 0.0252 (15) | 0.0265 (15) | 0.0302 (18) | −0.0008 (12) | −0.0039 (14) | 0.0070 (13) |
C19 | 0.0207 (14) | 0.0188 (13) | 0.0222 (16) | −0.0042 (10) | 0.0009 (13) | 0.0002 (11) |
C20 | 0.0218 (15) | 0.0273 (14) | 0.0272 (17) | −0.0090 (11) | −0.0014 (13) | 0.0033 (12) |
C21 | 0.0223 (15) | 0.0399 (17) | 0.038 (2) | −0.0123 (13) | −0.0078 (15) | 0.0021 (14) |
C22 | 0.0234 (16) | 0.0355 (17) | 0.054 (2) | −0.0155 (13) | −0.0048 (17) | 0.0040 (16) |
C23 | 0.0335 (18) | 0.049 (2) | 0.042 (2) | −0.0225 (15) | 0.0093 (17) | 0.0088 (16) |
C24 | 0.0322 (17) | 0.0410 (18) | 0.0270 (18) | −0.0160 (14) | 0.0018 (15) | 0.0069 (14) |
C25 | 0.0317 (16) | 0.0162 (12) | 0.0168 (15) | −0.0102 (11) | 0.0021 (13) | 0.0007 (11) |
C26 | 0.0411 (18) | 0.0255 (15) | 0.0205 (16) | −0.0067 (13) | 0.0062 (15) | −0.0022 (12) |
C27 | 0.066 (2) | 0.0320 (17) | 0.0220 (18) | −0.0074 (16) | 0.0117 (17) | −0.0074 (14) |
C28 | 0.076 (3) | 0.0399 (19) | 0.0130 (16) | −0.0236 (17) | −0.0001 (18) | −0.0038 (13) |
C29 | 0.052 (2) | 0.0356 (17) | 0.0213 (17) | −0.0173 (15) | −0.0071 (16) | 0.0046 (13) |
C30 | 0.0353 (17) | 0.0232 (14) | 0.0178 (15) | −0.0099 (12) | −0.0026 (14) | 0.0005 (11) |
C31 | 0.0189 (14) | 0.0263 (14) | 0.0231 (16) | −0.0104 (11) | −0.0080 (13) | 0.0060 (12) |
C32 | 0.0340 (17) | 0.0376 (17) | 0.0232 (17) | −0.0090 (13) | −0.0073 (15) | 0.0024 (13) |
C33 | 0.045 (2) | 0.051 (2) | 0.0238 (18) | −0.0133 (16) | −0.0157 (17) | 0.0115 (15) |
C34 | 0.0396 (19) | 0.0384 (18) | 0.042 (2) | −0.0129 (14) | −0.0210 (18) | 0.0223 (15) |
C35 | 0.0291 (16) | 0.0254 (15) | 0.045 (2) | −0.0098 (12) | −0.0121 (16) | 0.0103 (14) |
C36 | 0.0265 (15) | 0.0257 (14) | 0.0256 (17) | −0.0115 (11) | −0.0068 (14) | 0.0029 (12) |
C37 | 0.0197 (14) | 0.0193 (13) | 0.0219 (15) | −0.0073 (10) | −0.0015 (12) | −0.0043 (11) |
C38 | 0.0232 (15) | 0.0232 (14) | 0.0330 (18) | −0.0069 (11) | −0.0058 (14) | 0.0024 (12) |
C39 | 0.0212 (15) | 0.0329 (16) | 0.048 (2) | −0.0093 (12) | −0.0043 (15) | 0.0025 (15) |
C40 | 0.0285 (17) | 0.0412 (18) | 0.044 (2) | −0.0196 (14) | 0.0055 (16) | 0.0016 (15) |
C41 | 0.0360 (18) | 0.0374 (17) | 0.0307 (19) | −0.0168 (14) | −0.0036 (16) | 0.0070 (14) |
C42 | 0.0217 (14) | 0.0280 (14) | 0.0258 (17) | −0.0099 (11) | −0.0057 (13) | 0.0029 (12) |
C43 | 0.0198 (14) | 0.0273 (14) | 0.0114 (14) | −0.0043 (11) | −0.0009 (12) | −0.0019 (11) |
C44 | 0.0243 (15) | 0.0243 (14) | 0.0244 (16) | −0.0032 (11) | 0.0027 (13) | −0.0026 (12) |
C45 | 0.0307 (17) | 0.0369 (17) | 0.0319 (19) | 0.0037 (14) | 0.0023 (15) | 0.0026 (14) |
C46 | 0.0213 (16) | 0.054 (2) | 0.0308 (19) | −0.0011 (14) | 0.0033 (15) | −0.0004 (16) |
C47 | 0.0244 (16) | 0.0479 (19) | 0.033 (2) | −0.0152 (14) | 0.0017 (15) | 0.0007 (15) |
C48 | 0.0236 (15) | 0.0292 (15) | 0.0276 (17) | −0.0080 (12) | 0.0026 (14) | −0.0020 (12) |
C49 | 0.0158 (13) | 0.0210 (13) | 0.0172 (14) | −0.0020 (10) | −0.0013 (12) | −0.0045 (11) |
C50 | 0.0316 (16) | 0.0225 (14) | 0.0155 (15) | −0.0080 (11) | −0.0021 (13) | −0.0033 (11) |
C51 | 0.0408 (18) | 0.0299 (15) | 0.0160 (16) | −0.0083 (13) | −0.0051 (14) | 0.0011 (12) |
C52 | 0.0352 (17) | 0.0323 (16) | 0.0208 (16) | −0.0016 (13) | −0.0088 (14) | −0.0102 (13) |
C53 | 0.0394 (18) | 0.0220 (14) | 0.0314 (18) | −0.0025 (12) | −0.0114 (15) | −0.0085 (13) |
C54 | 0.0340 (17) | 0.0184 (13) | 0.0251 (17) | −0.0017 (11) | −0.0074 (14) | −0.0012 (12) |
C55 | 0.0304 (18) | 0.064 (2) | 0.0246 (19) | −0.0026 (16) | −0.0005 (16) | 0.0027 (16) |
C56 | 0.052 (2) | 0.068 (3) | 0.031 (2) | −0.031 (2) | 0.0083 (19) | −0.0064 (18) |
C57 | 0.073 (3) | 0.0353 (19) | 0.045 (2) | −0.0029 (18) | 0.015 (2) | −0.0018 (17) |
C58 | 0.0314 (19) | 0.058 (2) | 0.042 (2) | 0.0119 (17) | 0.0049 (18) | 0.0015 (18) |
C59 | 0.0306 (17) | 0.054 (2) | 0.0283 (19) | −0.0117 (15) | 0.0050 (16) | 0.0002 (16) |
C60 | 0.0406 (19) | 0.0377 (17) | 0.0240 (18) | −0.0021 (14) | 0.0037 (16) | 0.0002 (14) |
C64 | 0.0196 (13) | 0.0153 (12) | 0.0176 (14) | −0.0040 (10) | −0.0021 (12) | −0.0021 (10) |
C65 | 0.0211 (14) | 0.0163 (12) | 0.0170 (14) | −0.0071 (10) | 0.0021 (12) | −0.0004 (10) |
C66 | 0.0195 (14) | 0.0145 (12) | 0.0239 (16) | −0.0020 (10) | 0.0010 (12) | 0.0030 (11) |
C67 | 0.0217 (14) | 0.0227 (13) | 0.0206 (15) | −0.0020 (11) | −0.0030 (13) | 0.0049 (11) |
C68 | 0.0283 (15) | 0.0190 (13) | 0.0189 (15) | −0.0082 (11) | −0.0008 (13) | 0.0068 (11) |
C69 | 0.0258 (15) | 0.0140 (12) | 0.0154 (14) | −0.0034 (10) | 0.0029 (12) | −0.0028 (10) |
C70 | 0.0160 (13) | 0.0191 (13) | 0.0168 (14) | −0.0028 (10) | 0.0035 (12) | 0.0020 (11) |
C71 | 0.0214 (15) | 0.0328 (15) | 0.0238 (17) | 0.0030 (12) | −0.0006 (13) | −0.0041 (13) |
C72 | 0.0258 (16) | 0.0489 (19) | 0.0239 (17) | 0.0061 (14) | −0.0044 (14) | 0.0035 (14) |
C73 | 0.0215 (15) | 0.0303 (16) | 0.038 (2) | 0.0093 (12) | 0.0035 (15) | 0.0074 (14) |
C74 | 0.0283 (16) | 0.0224 (14) | 0.0351 (19) | 0.0028 (12) | 0.0067 (15) | −0.0015 (13) |
C75 | 0.0251 (15) | 0.0213 (13) | 0.0259 (17) | −0.0019 (11) | −0.0015 (13) | −0.0010 (12) |
C76 | 0.0228 (14) | 0.0108 (11) | 0.0160 (14) | 0.0011 (10) | 0.0011 (12) | −0.0007 (10) |
C77 | 0.0223 (14) | 0.0204 (13) | 0.0207 (15) | −0.0024 (10) | −0.0016 (13) | 0.0024 (11) |
C78 | 0.0361 (18) | 0.0257 (14) | 0.0199 (16) | −0.0031 (12) | −0.0060 (14) | 0.0019 (12) |
C79 | 0.0430 (19) | 0.0312 (16) | 0.0132 (15) | −0.0029 (13) | 0.0035 (14) | 0.0022 (12) |
C80 | 0.0295 (16) | 0.0302 (15) | 0.0253 (17) | −0.0053 (12) | 0.0070 (14) | 0.0025 (13) |
C81 | 0.0249 (15) | 0.0229 (14) | 0.0211 (16) | −0.0044 (11) | 0.0012 (13) | 0.0004 (11) |
C82 | 0.0181 (13) | 0.0198 (13) | 0.0229 (16) | 0.0015 (10) | −0.0058 (12) | −0.0040 (11) |
C83 | 0.0300 (16) | 0.0292 (15) | 0.0229 (17) | −0.0034 (12) | −0.0035 (14) | 0.0006 (12) |
C84 | 0.0386 (19) | 0.0427 (19) | 0.0253 (18) | 0.0019 (15) | −0.0106 (16) | −0.0066 (14) |
C85 | 0.0344 (18) | 0.0402 (18) | 0.043 (2) | 0.0008 (14) | −0.0193 (17) | −0.0162 (16) |
C86 | 0.0262 (16) | 0.0283 (15) | 0.045 (2) | −0.0052 (12) | −0.0087 (15) | −0.0077 (14) |
C87 | 0.0224 (15) | 0.0247 (14) | 0.0289 (17) | −0.0008 (11) | −0.0038 (14) | −0.0013 (12) |
C88 | 0.0215 (14) | 0.0174 (13) | 0.0207 (15) | −0.0029 (10) | 0.0006 (12) | 0.0050 (11) |
C89 | 0.0257 (15) | 0.0238 (14) | 0.0310 (18) | −0.0018 (11) | −0.0043 (14) | −0.0021 (12) |
C90 | 0.0235 (16) | 0.0356 (17) | 0.042 (2) | 0.0007 (13) | −0.0042 (15) | −0.0008 (15) |
C91 | 0.0283 (17) | 0.0301 (16) | 0.040 (2) | 0.0052 (13) | 0.0042 (15) | −0.0007 (14) |
C92 | 0.0323 (17) | 0.0216 (14) | 0.0320 (18) | −0.0027 (12) | 0.0037 (15) | −0.0037 (12) |
C93 | 0.0235 (15) | 0.0217 (14) | 0.0257 (17) | −0.0039 (11) | −0.0010 (13) | 0.0008 (12) |
C94 | 0.0223 (14) | 0.0164 (12) | 0.0212 (15) | −0.0044 (10) | −0.0030 (12) | −0.0025 (11) |
C95 | 0.0301 (16) | 0.0295 (15) | 0.0269 (18) | −0.0129 (12) | 0.0028 (14) | −0.0060 (13) |
C96 | 0.0389 (18) | 0.0427 (18) | 0.0253 (18) | −0.0156 (14) | 0.0052 (16) | −0.0153 (14) |
C97 | 0.0383 (18) | 0.0281 (16) | 0.040 (2) | −0.0098 (13) | −0.0069 (16) | −0.0133 (14) |
C98 | 0.047 (2) | 0.0267 (16) | 0.040 (2) | −0.0196 (14) | −0.0122 (17) | 0.0040 (14) |
C99 | 0.0434 (19) | 0.0240 (14) | 0.0233 (17) | −0.0138 (13) | −0.0054 (15) | 0.0022 (12) |
C100 | 0.0208 (14) | 0.0142 (12) | 0.0221 (15) | −0.0045 (10) | −0.0009 (12) | −0.0023 (10) |
C101 | 0.0279 (16) | 0.0233 (14) | 0.0227 (16) | −0.0016 (11) | −0.0055 (13) | 0.0013 (12) |
C102 | 0.0220 (15) | 0.0295 (15) | 0.038 (2) | −0.0007 (12) | −0.0041 (15) | −0.0015 (14) |
C103 | 0.0237 (16) | 0.0319 (16) | 0.041 (2) | −0.0066 (12) | 0.0068 (15) | −0.0082 (14) |
C104 | 0.0310 (16) | 0.0303 (15) | 0.0244 (17) | −0.0074 (12) | 0.0058 (14) | 0.0003 (13) |
C105 | 0.0226 (15) | 0.0251 (14) | 0.0236 (16) | −0.0031 (11) | 0.0002 (13) | 0.0044 (12) |
C106 | 0.0181 (13) | 0.0222 (13) | 0.0161 (14) | −0.0064 (10) | 0.0007 (12) | 0.0018 (11) |
C107 | 0.0268 (15) | 0.0216 (13) | 0.0241 (16) | −0.0105 (11) | −0.0045 (13) | 0.0032 (11) |
C108 | 0.0314 (17) | 0.0268 (15) | 0.0314 (18) | −0.0110 (12) | −0.0084 (15) | 0.0119 (13) |
C109 | 0.0334 (17) | 0.0404 (17) | 0.0176 (16) | −0.0130 (13) | −0.0054 (14) | 0.0105 (13) |
C110 | 0.0434 (19) | 0.0325 (16) | 0.0190 (16) | −0.0109 (14) | −0.0004 (15) | −0.0021 (13) |
C111 | 0.0363 (17) | 0.0215 (14) | 0.0177 (15) | −0.0073 (12) | −0.0001 (14) | 0.0028 (11) |
C112 | 0.0185 (13) | 0.0267 (14) | 0.0105 (14) | −0.0053 (11) | 0.0012 (11) | 0.0004 (11) |
C113 | 0.0263 (16) | 0.0297 (15) | 0.0288 (18) | −0.0042 (12) | 0.0009 (14) | 0.0033 (13) |
C114 | 0.0239 (16) | 0.0437 (19) | 0.042 (2) | 0.0049 (14) | −0.0024 (16) | 0.0016 (16) |
C115 | 0.0193 (16) | 0.060 (2) | 0.034 (2) | −0.0090 (15) | 0.0035 (15) | 0.0013 (17) |
C116 | 0.0290 (17) | 0.0443 (18) | 0.0238 (17) | −0.0190 (14) | 0.0023 (14) | 0.0016 (14) |
C117 | 0.0268 (15) | 0.0286 (15) | 0.0204 (16) | −0.0088 (12) | −0.0009 (13) | 0.0028 (12) |
C118 | 0.0359 (19) | 0.060 (2) | 0.030 (2) | −0.0098 (16) | −0.0018 (17) | 0.0007 (17) |
C119 | 0.043 (2) | 0.0421 (19) | 0.040 (2) | −0.0055 (15) | 0.0084 (18) | 0.0002 (16) |
C120 | 0.042 (2) | 0.050 (2) | 0.038 (2) | −0.0206 (16) | 0.0073 (18) | −0.0062 (17) |
C121 | 0.0305 (18) | 0.060 (2) | 0.039 (2) | −0.0124 (16) | 0.0009 (17) | −0.0013 (18) |
C122 | 0.043 (2) | 0.044 (2) | 0.055 (3) | −0.0024 (16) | −0.002 (2) | −0.0023 (18) |
C123 | 0.052 (2) | 0.049 (2) | 0.043 (2) | −0.0176 (17) | −0.0019 (19) | −0.0112 (17) |
C124 | 0.120 (5) | 0.096 (4) | 0.115 (5) | −0.061 (4) | −0.063 (5) | 0.043 (4) |
C125 | 0.124 (5) | 0.121 (5) | 0.138 (6) | −0.084 (4) | −0.078 (5) | 0.053 (5) |
C126 | 0.117 (5) | 0.056 (3) | 0.086 (4) | −0.034 (3) | −0.032 (4) | 0.015 (3) |
C127 | 0.059 (3) | 0.062 (3) | 0.077 (4) | 0.011 (2) | −0.013 (3) | −0.011 (3) |
C128 | 0.054 (3) | 0.104 (4) | 0.094 (5) | −0.016 (3) | −0.005 (3) | −0.003 (4) |
C129 | 0.082 (4) | 0.108 (5) | 0.096 (5) | −0.039 (3) | −0.008 (4) | 0.028 (4) |
O1 | 0.0321 (12) | 0.0384 (12) | 0.0308 (13) | −0.0085 (9) | −0.0188 (11) | 0.0073 (10) |
O2 | 0.0380 (12) | 0.0298 (11) | 0.0173 (12) | −0.0155 (9) | 0.0055 (10) | 0.0034 (9) |
O3 | 0.0442 (13) | 0.0253 (11) | 0.0265 (12) | −0.0047 (9) | 0.0135 (11) | −0.0078 (9) |
O4 | 0.0388 (13) | 0.0332 (11) | 0.0254 (12) | −0.0016 (9) | −0.0150 (11) | −0.0031 (9) |
P1 | 0.0188 (3) | 0.0137 (3) | 0.0166 (4) | −0.0049 (2) | −0.0021 (3) | −0.0009 (3) |
P2 | 0.0192 (3) | 0.0145 (3) | 0.0125 (3) | −0.0056 (2) | −0.0001 (3) | 0.0008 (2) |
P3 | 0.0184 (3) | 0.0173 (3) | 0.0154 (4) | −0.0057 (2) | −0.0049 (3) | 0.0003 (3) |
P4 | 0.0178 (3) | 0.0138 (3) | 0.0127 (3) | −0.0041 (2) | −0.0007 (3) | −0.0009 (2) |
P5 | 0.0161 (3) | 0.0131 (3) | 0.0135 (3) | −0.0021 (2) | −0.0009 (3) | −0.0006 (2) |
P6 | 0.0180 (3) | 0.0162 (3) | 0.0166 (4) | −0.0023 (2) | −0.0013 (3) | −0.0001 (3) |
P7 | 0.0192 (3) | 0.0117 (3) | 0.0143 (4) | −0.0034 (2) | −0.0006 (3) | 0.0014 (2) |
P8 | 0.0186 (3) | 0.0133 (3) | 0.0133 (3) | −0.0044 (2) | 0.0006 (3) | 0.0001 (2) |
W1 | 0.01676 (6) | 0.01236 (5) | 0.01092 (6) | −0.00498 (4) | −0.00204 (4) | 0.00010 (4) |
W2 | 0.01794 (6) | 0.01075 (5) | 0.01221 (6) | −0.00287 (4) | 0.00012 (4) | −0.00031 (4) |
C1—C2 | 1.532 (4) | C68—W2 | 1.974 (3) |
C1—P1 | 1.850 (3) | C69—O4 | 1.175 (3) |
C2—P3 | 1.861 (3) | C69—W2 | 1.945 (3) |
C3—C4 | 1.530 (4) | C70—C71 | 1.388 (4) |
C3—P2 | 1.855 (3) | C70—C75 | 1.401 (4) |
C4—P4 | 1.853 (3) | C70—P5 | 1.854 (3) |
C5—O1 | 1.167 (3) | C71—C72 | 1.401 (4) |
C5—W1 | 1.961 (3) | C72—C73 | 1.382 (5) |
C6—O2 | 1.175 (4) | C73—C74 | 1.383 (5) |
C6—W1 | 1.956 (3) | C74—C75 | 1.382 (4) |
C7—C12 | 1.396 (4) | C76—C77 | 1.395 (4) |
C7—C8 | 1.398 (4) | C76—C81 | 1.400 (4) |
C7—P1 | 1.835 (3) | C76—P5 | 1.847 (3) |
C8—C9 | 1.390 (5) | C77—C78 | 1.405 (4) |
C9—C10 | 1.391 (5) | C78—C79 | 1.372 (5) |
C10—C11 | 1.375 (4) | C79—C80 | 1.387 (4) |
C11—C12 | 1.389 (4) | C80—C81 | 1.396 (4) |
C13—C18 | 1.385 (4) | C82—C87 | 1.396 (4) |
C13—C14 | 1.402 (4) | C82—C83 | 1.399 (4) |
C13—P1 | 1.853 (3) | C82—P6 | 1.849 (3) |
C14—C15 | 1.398 (4) | C83—C84 | 1.394 (4) |
C15—C16 | 1.385 (5) | C84—C85 | 1.374 (5) |
C16—C17 | 1.379 (5) | C85—C86 | 1.395 (5) |
C17—C18 | 1.402 (4) | C86—C87 | 1.391 (4) |
C19—C24 | 1.382 (5) | C88—C89 | 1.388 (4) |
C19—C20 | 1.399 (4) | C88—C93 | 1.404 (4) |
C19—P2 | 1.848 (3) | C88—P6 | 1.860 (3) |
C20—C21 | 1.398 (4) | C89—C90 | 1.399 (4) |
C21—C22 | 1.379 (5) | C90—C91 | 1.377 (5) |
C22—C23 | 1.382 (5) | C91—C92 | 1.390 (4) |
C23—C24 | 1.397 (5) | C92—C93 | 1.383 (4) |
C25—C30 | 1.394 (4) | C94—C95 | 1.392 (4) |
C25—C26 | 1.401 (4) | C94—C99 | 1.394 (4) |
C25—P2 | 1.841 (3) | C94—P7 | 1.851 (3) |
C26—C27 | 1.390 (4) | C95—C96 | 1.396 (4) |
C27—C28 | 1.385 (5) | C96—C97 | 1.375 (5) |
C28—C29 | 1.370 (5) | C97—C98 | 1.390 (5) |
C29—C30 | 1.404 (4) | C98—C99 | 1.392 (4) |
C31—C32 | 1.393 (4) | C100—C105 | 1.387 (4) |
C31—C36 | 1.403 (4) | C100—C101 | 1.401 (4) |
C31—P3 | 1.853 (3) | C100—P7 | 1.845 (3) |
C32—C33 | 1.404 (4) | C101—C102 | 1.387 (4) |
C33—C34 | 1.390 (5) | C102—C103 | 1.379 (5) |
C34—C35 | 1.389 (5) | C103—C104 | 1.391 (4) |
C35—C36 | 1.397 (4) | C104—C105 | 1.389 (4) |
C37—C38 | 1.398 (4) | C106—C111 | 1.393 (4) |
C37—C42 | 1.402 (4) | C106—C107 | 1.403 (4) |
C37—P3 | 1.846 (3) | C106—P8 | 1.853 (3) |
C38—C39 | 1.384 (5) | C107—C108 | 1.395 (4) |
C39—C40 | 1.389 (5) | C108—C109 | 1.388 (4) |
C40—C41 | 1.386 (5) | C109—C110 | 1.383 (4) |
C41—C42 | 1.380 (5) | C110—C111 | 1.393 (4) |
C43—C48 | 1.390 (4) | C112—C117 | 1.392 (4) |
C43—C44 | 1.398 (4) | C112—C113 | 1.392 (4) |
C43—P4 | 1.852 (3) | C112—P8 | 1.846 (3) |
C44—C45 | 1.386 (4) | C113—C114 | 1.385 (5) |
C45—C46 | 1.372 (5) | C114—C115 | 1.371 (5) |
C46—C47 | 1.385 (5) | C115—C116 | 1.386 (4) |
C47—C48 | 1.388 (4) | C116—C117 | 1.380 (4) |
C49—C54 | 1.396 (4) | C118—C123 | 1.374 (5) |
C49—C50 | 1.401 (4) | C118—C119 | 1.386 (5) |
C49—P4 | 1.849 (3) | C119—C120 | 1.380 (5) |
C50—C51 | 1.397 (4) | C120—C121 | 1.373 (5) |
C51—C52 | 1.382 (4) | C121—C122 | 1.382 (5) |
C52—C53 | 1.382 (5) | C122—C123 | 1.372 (5) |
C53—C54 | 1.393 (4) | C124—C129 | 1.318 (8) |
C55—C60 | 1.369 (5) | C124—C125 | 1.404 (9) |
C55—C56 | 1.376 (5) | C125—C126 | 1.349 (7) |
C56—C57 | 1.388 (6) | C126—C127 | 1.357 (7) |
C57—C58 | 1.362 (6) | C127—C128 | 1.353 (8) |
C58—C59 | 1.382 (5) | C128—C129 | 1.397 (8) |
C59—C60 | 1.369 (5) | P1—W1 | 2.4613 (9) |
C64—C65 | 1.528 (4) | P2—W1 | 2.5391 (9) |
C64—P5 | 1.848 (3) | P3—W1 | 2.5508 (8) |
C65—P8 | 1.856 (3) | P4—W1 | 2.4542 (8) |
C66—C67 | 1.526 (4) | P5—W2 | 2.5502 (9) |
C66—P7 | 1.851 (3) | P6—W2 | 2.5560 (9) |
C67—P6 | 1.855 (3) | P7—W2 | 2.4367 (9) |
C68—O3 | 1.159 (4) | P8—W2 | 2.4577 (9) |
C2—C1—P1 | 109.81 (18) | C97—C96—C95 | 120.2 (3) |
C1—C2—P3 | 109.37 (19) | C96—C97—C98 | 119.6 (3) |
C4—C3—P2 | 109.13 (17) | C97—C98—C99 | 120.3 (3) |
C3—C4—P4 | 110.74 (17) | C98—C99—C94 | 120.5 (3) |
O1—C5—W1 | 175.2 (2) | C105—C100—C101 | 118.8 (3) |
O2—C6—W1 | 175.1 (2) | C105—C100—P7 | 123.4 (2) |
C12—C7—C8 | 117.6 (3) | C101—C100—P7 | 117.8 (2) |
C12—C7—P1 | 124.6 (2) | C102—C101—C100 | 119.8 (3) |
C8—C7—P1 | 117.7 (2) | C103—C102—C101 | 121.0 (3) |
C9—C8—C7 | 120.4 (3) | C102—C103—C104 | 119.6 (3) |
C8—C9—C10 | 121.0 (3) | C105—C104—C103 | 119.6 (3) |
C11—C10—C9 | 119.1 (3) | C100—C105—C104 | 121.2 (3) |
C10—C11—C12 | 120.2 (3) | C111—C106—C107 | 117.8 (3) |
C11—C12—C7 | 121.7 (3) | C111—C106—P8 | 120.2 (2) |
C18—C13—C14 | 118.8 (3) | C107—C106—P8 | 121.9 (2) |
C18—C13—P1 | 121.6 (2) | C108—C107—C106 | 120.9 (3) |
C14—C13—P1 | 119.6 (2) | C109—C108—C107 | 120.1 (3) |
C15—C14—C13 | 120.0 (3) | C110—C109—C108 | 119.6 (3) |
C16—C15—C14 | 120.5 (3) | C109—C110—C111 | 120.2 (3) |
C17—C16—C15 | 119.8 (3) | C106—C111—C110 | 121.3 (3) |
C16—C17—C18 | 120.1 (3) | C117—C112—C113 | 118.2 (3) |
C13—C18—C17 | 120.8 (3) | C117—C112—P8 | 122.0 (2) |
C24—C19—C20 | 118.3 (3) | C113—C112—P8 | 119.7 (2) |
C24—C19—P2 | 122.1 (2) | C114—C113—C112 | 120.5 (3) |
C20—C19—P2 | 119.1 (2) | C115—C114—C113 | 120.5 (3) |
C21—C20—C19 | 120.7 (3) | C114—C115—C116 | 119.8 (3) |
C22—C21—C20 | 120.0 (3) | C117—C116—C115 | 119.9 (3) |
C21—C22—C23 | 119.9 (3) | C116—C117—C112 | 121.1 (3) |
C22—C23—C24 | 120.0 (4) | C123—C118—C119 | 119.7 (3) |
C19—C24—C23 | 121.1 (3) | C120—C119—C118 | 119.8 (3) |
C30—C25—C26 | 118.0 (3) | C121—C120—C119 | 120.3 (3) |
C30—C25—P2 | 123.1 (2) | C120—C121—C122 | 119.8 (3) |
C26—C25—P2 | 118.9 (2) | C123—C122—C121 | 120.1 (3) |
C27—C26—C25 | 120.4 (3) | C122—C123—C118 | 120.4 (3) |
C28—C27—C26 | 120.8 (3) | C129—C124—C125 | 119.1 (6) |
C29—C28—C27 | 119.5 (3) | C126—C125—C124 | 119.6 (6) |
C28—C29—C30 | 120.3 (3) | C125—C126—C127 | 122.0 (6) |
C25—C30—C29 | 120.9 (3) | C128—C127—C126 | 117.7 (5) |
C32—C31—C36 | 118.8 (3) | C127—C128—C129 | 121.4 (5) |
C32—C31—P3 | 122.6 (2) | C124—C129—C128 | 120.1 (6) |
C36—C31—P3 | 118.5 (2) | C7—P1—C1 | 102.98 (13) |
C31—C32—C33 | 120.8 (3) | C7—P1—C13 | 98.97 (13) |
C34—C33—C32 | 119.8 (3) | C1—P1—C13 | 99.83 (13) |
C35—C34—C33 | 119.8 (3) | C7—P1—W1 | 120.74 (9) |
C34—C35—C36 | 120.4 (3) | C1—P1—W1 | 110.39 (9) |
C35—C36—C31 | 120.3 (3) | C13—P1—W1 | 120.71 (10) |
C38—C37—C42 | 118.0 (3) | C25—P2—C19 | 101.09 (14) |
C38—C37—P3 | 122.5 (2) | C25—P2—C3 | 101.31 (12) |
C42—C37—P3 | 119.5 (2) | C19—P2—C3 | 97.66 (12) |
C39—C38—C37 | 120.9 (3) | C25—P2—W1 | 124.46 (9) |
C38—C39—C40 | 120.3 (3) | C19—P2—W1 | 121.28 (9) |
C41—C40—C39 | 119.5 (3) | C3—P2—W1 | 106.21 (10) |
C42—C41—C40 | 120.3 (3) | C37—P3—C31 | 99.22 (13) |
C41—C42—C37 | 121.0 (3) | C37—P3—C2 | 100.54 (13) |
C48—C43—C44 | 118.0 (3) | C31—P3—C2 | 101.38 (13) |
C48—C43—P4 | 118.8 (2) | C37—P3—W1 | 118.78 (9) |
C44—C43—P4 | 123.2 (2) | C31—P3—W1 | 126.42 (9) |
C45—C44—C43 | 121.1 (3) | C2—P3—W1 | 106.55 (9) |
C46—C45—C44 | 120.2 (3) | C49—P4—C43 | 97.63 (12) |
C45—C46—C47 | 119.7 (3) | C49—P4—C4 | 100.68 (12) |
C46—C47—C48 | 120.3 (3) | C43—P4—C4 | 103.80 (12) |
C47—C48—C43 | 120.8 (3) | C49—P4—W1 | 120.12 (8) |
C54—C49—C50 | 117.6 (2) | C43—P4—W1 | 120.20 (9) |
C54—C49—P4 | 122.2 (2) | C4—P4—W1 | 111.47 (9) |
C50—C49—P4 | 120.1 (2) | C76—P5—C64 | 101.57 (12) |
C51—C50—C49 | 121.1 (3) | C76—P5—C70 | 99.06 (12) |
C52—C51—C50 | 119.9 (3) | C64—P5—C70 | 96.01 (12) |
C51—C52—C53 | 120.1 (3) | C76—P5—W2 | 126.55 (8) |
C52—C53—C54 | 119.9 (3) | C64—P5—W2 | 105.40 (9) |
C53—C54—C49 | 121.4 (3) | C70—P5—W2 | 122.44 (9) |
C60—C55—C56 | 119.4 (3) | C82—P6—C67 | 100.46 (14) |
C55—C56—C57 | 120.1 (4) | C82—P6—C88 | 99.81 (12) |
C58—C57—C56 | 120.0 (4) | C67—P6—C88 | 100.76 (12) |
C57—C58—C59 | 119.8 (3) | C82—P6—W2 | 126.08 (8) |
C60—C59—C58 | 119.9 (3) | C67—P6—W2 | 107.07 (9) |
C55—C60—C59 | 120.8 (3) | C88—P6—W2 | 118.68 (9) |
C65—C64—P5 | 108.02 (17) | C100—P7—C66 | 103.15 (13) |
C64—C65—P8 | 109.74 (17) | C100—P7—C94 | 99.15 (13) |
C67—C66—P7 | 110.55 (17) | C66—P7—C94 | 99.15 (12) |
C66—C67—P6 | 111.2 (2) | C100—P7—W2 | 119.86 (8) |
O3—C68—W2 | 175.8 (2) | C66—P7—W2 | 111.28 (9) |
O4—C69—W2 | 173.7 (2) | C94—P7—W2 | 121.02 (10) |
C71—C70—C75 | 118.5 (2) | C112—P8—C106 | 97.90 (13) |
C71—C70—P5 | 122.5 (2) | C112—P8—C65 | 103.34 (12) |
C75—C70—P5 | 118.5 (2) | C106—P8—C65 | 100.96 (12) |
C70—C71—C72 | 120.4 (3) | C112—P8—W2 | 121.56 (9) |
C73—C72—C71 | 120.2 (3) | C106—P8—W2 | 119.08 (9) |
C72—C73—C74 | 119.8 (3) | C65—P8—W2 | 111.01 (9) |
C75—C74—C73 | 120.2 (3) | C6—W1—C5 | 85.14 (12) |
C74—C75—C70 | 120.9 (3) | C6—W1—P4 | 86.79 (7) |
C77—C76—C81 | 118.1 (3) | C5—W1—P4 | 93.28 (8) |
C77—C76—P5 | 123.8 (2) | C6—W1—P1 | 93.86 (7) |
C81—C76—P5 | 118.0 (2) | C5—W1—P1 | 86.65 (8) |
C76—C77—C78 | 120.8 (3) | P4—W1—P1 | 179.34 (3) |
C79—C78—C77 | 120.3 (3) | C6—W1—P2 | 165.95 (7) |
C78—C79—C80 | 119.7 (3) | C5—W1—P2 | 95.55 (9) |
C79—C80—C81 | 120.4 (3) | P4—W1—P2 | 79.16 (3) |
C80—C81—C76 | 120.6 (3) | P1—W1—P2 | 100.19 (3) |
C87—C82—C83 | 118.0 (3) | C6—W1—P3 | 93.74 (8) |
C87—C82—P6 | 118.3 (2) | C5—W1—P3 | 166.09 (7) |
C83—C82—P6 | 123.6 (2) | P4—W1—P3 | 100.51 (3) |
C84—C83—C82 | 121.0 (3) | P1—W1—P3 | 79.58 (3) |
C85—C84—C83 | 120.4 (3) | P2—W1—P3 | 88.89 (3) |
C84—C85—C86 | 119.4 (3) | C69—W2—C68 | 85.48 (11) |
C87—C86—C85 | 120.4 (3) | C69—W2—P7 | 84.13 (9) |
C86—C87—C82 | 120.7 (3) | C68—W2—P7 | 94.94 (8) |
C89—C88—C93 | 118.1 (3) | C69—W2—P8 | 91.53 (9) |
C89—C88—P6 | 122.5 (2) | C68—W2—P8 | 86.68 (8) |
C93—C88—P6 | 119.3 (2) | P7—W2—P8 | 175.23 (2) |
C88—C89—C90 | 120.9 (3) | C69—W2—P5 | 96.46 (8) |
C91—C90—C89 | 120.2 (3) | C68—W2—P5 | 165.38 (8) |
C90—C91—C92 | 119.5 (3) | P7—W2—P5 | 99.68 (3) |
C93—C92—C91 | 120.5 (3) | P8—W2—P5 | 78.80 (3) |
C92—C93—C88 | 120.7 (3) | C69—W2—P6 | 163.43 (8) |
C95—C94—C99 | 118.5 (3) | C68—W2—P6 | 91.79 (8) |
C95—C94—P7 | 121.4 (2) | P7—W2—P6 | 79.82 (3) |
C99—C94—P7 | 120.1 (2) | P8—W2—P6 | 104.65 (3) |
C94—C95—C96 | 120.9 (3) | P5—W2—P6 | 90.30 (3) |
P1—C1—C2—P3 | −54.7 (2) | C48—C43—P4—W1 | 25.0 (3) |
P2—C3—C4—P4 | −51.8 (2) | C44—C43—P4—W1 | −156.5 (2) |
C12—C7—C8—C9 | 0.3 (4) | C3—C4—P4—C49 | 159.78 (18) |
P1—C7—C8—C9 | −180.0 (2) | C3—C4—P4—C43 | −99.54 (19) |
C7—C8—C9—C10 | 0.5 (5) | C3—C4—P4—W1 | 31.24 (19) |
C8—C9—C10—C11 | −1.2 (5) | C77—C76—P5—C64 | 24.3 (2) |
C9—C10—C11—C12 | 0.9 (5) | C81—C76—P5—C64 | −152.83 (19) |
C10—C11—C12—C7 | −0.1 (5) | C77—C76—P5—C70 | 122.4 (2) |
C8—C7—C12—C11 | −0.5 (4) | C81—C76—P5—C70 | −54.7 (2) |
P1—C7—C12—C11 | 179.8 (2) | C77—C76—P5—W2 | −95.0 (2) |
C18—C13—C14—C15 | 0.6 (4) | C81—C76—P5—W2 | 87.9 (2) |
P1—C13—C14—C15 | −177.4 (2) | C65—C64—P5—C76 | 174.53 (16) |
C13—C14—C15—C16 | 0.0 (5) | C65—C64—P5—C70 | 73.97 (18) |
C14—C15—C16—C17 | −0.8 (5) | C65—C64—P5—W2 | −52.08 (17) |
C15—C16—C17—C18 | 0.8 (5) | C71—C70—P5—C76 | 147.0 (3) |
C14—C13—C18—C17 | −0.5 (5) | C75—C70—P5—C76 | −41.3 (3) |
P1—C13—C18—C17 | 177.5 (2) | C71—C70—P5—C64 | −110.3 (3) |
C16—C17—C18—C13 | −0.2 (5) | C75—C70—P5—C64 | 61.5 (3) |
C24—C19—C20—C21 | 1.1 (4) | C71—C70—P5—W2 | 2.3 (3) |
P2—C19—C20—C21 | −171.5 (2) | C75—C70—P5—W2 | 174.0 (2) |
C19—C20—C21—C22 | −0.9 (4) | C87—C82—P6—C67 | 174.6 (2) |
C20—C21—C22—C23 | −0.3 (5) | C83—C82—P6—C67 | −6.2 (3) |
C21—C22—C23—C24 | 1.2 (5) | C87—C82—P6—C88 | −82.5 (2) |
C20—C19—C24—C23 | −0.2 (4) | C83—C82—P6—C88 | 96.7 (2) |
P2—C19—C24—C23 | 172.2 (2) | C87—C82—P6—W2 | 54.3 (2) |
C22—C23—C24—C19 | −1.0 (5) | C83—C82—P6—W2 | −126.5 (2) |
C30—C25—C26—C27 | 0.0 (5) | C66—C67—P6—C82 | −173.17 (18) |
P2—C25—C26—C27 | 179.0 (3) | C66—C67—P6—C88 | 84.6 (2) |
C25—C26—C27—C28 | 0.9 (6) | C66—C67—P6—W2 | −40.08 (19) |
C26—C27—C28—C29 | −0.8 (6) | C89—C88—P6—C82 | 4.2 (3) |
C27—C28—C29—C30 | −0.2 (6) | C93—C88—P6—C82 | −175.7 (2) |
C26—C25—C30—C29 | −1.0 (4) | C89—C88—P6—C67 | 106.9 (3) |
P2—C25—C30—C29 | −180.0 (2) | C93—C88—P6—C67 | −73.0 (2) |
C28—C29—C30—C25 | 1.1 (5) | C89—C88—P6—W2 | −136.7 (2) |
C36—C31—C32—C33 | 0.7 (5) | C93—C88—P6—W2 | 43.4 (3) |
P3—C31—C32—C33 | 178.2 (3) | C105—C100—P7—C66 | −9.2 (3) |
C31—C32—C33—C34 | −0.8 (5) | C101—C100—P7—C66 | 171.0 (2) |
C32—C33—C34—C35 | 0.0 (5) | C105—C100—P7—C94 | −110.9 (2) |
C33—C34—C35—C36 | 1.0 (5) | C101—C100—P7—C94 | 69.3 (2) |
C34—C35—C36—C31 | −1.2 (5) | C105—C100—P7—W2 | 115.1 (2) |
C32—C31—C36—C35 | 0.3 (4) | C101—C100—P7—W2 | −64.7 (2) |
P3—C31—C36—C35 | −177.3 (2) | C67—C66—P7—C100 | 92.2 (2) |
C42—C37—C38—C39 | 0.1 (4) | C67—C66—P7—C94 | −166.1 (2) |
P3—C37—C38—C39 | 179.4 (2) | C67—C66—P7—W2 | −37.6 (2) |
C37—C38—C39—C40 | −1.0 (5) | C95—C94—P7—C100 | −137.1 (2) |
C38—C39—C40—C41 | 0.5 (5) | C99—C94—P7—C100 | 46.0 (2) |
C39—C40—C41—C42 | 0.8 (5) | C95—C94—P7—C66 | 117.8 (2) |
C40—C41—C42—C37 | −1.7 (5) | C99—C94—P7—C66 | −59.0 (2) |
C38—C37—C42—C41 | 1.2 (4) | C95—C94—P7—W2 | −3.9 (3) |
P3—C37—C42—C41 | −178.1 (2) | C99—C94—P7—W2 | 179.30 (19) |
C48—C43—C44—C45 | −1.0 (4) | C117—C112—P8—C106 | −61.8 (3) |
P4—C43—C44—C45 | −179.5 (2) | C113—C112—P8—C106 | 115.4 (2) |
C43—C44—C45—C46 | 0.3 (5) | C117—C112—P8—C65 | 41.5 (3) |
C44—C45—C46—C47 | 0.6 (5) | C113—C112—P8—C65 | −141.3 (2) |
C45—C46—C47—C48 | −0.9 (5) | C117—C112—P8—W2 | 166.9 (2) |
C46—C47—C48—C43 | 0.1 (5) | C113—C112—P8—W2 | −16.0 (3) |
C44—C43—C48—C47 | 0.8 (4) | C111—C106—P8—C112 | −92.9 (3) |
P4—C43—C48—C47 | 179.3 (2) | C107—C106—P8—C112 | 83.9 (3) |
C54—C49—C50—C51 | 1.5 (4) | C111—C106—P8—C65 | 161.8 (2) |
P4—C49—C50—C51 | −174.2 (2) | C107—C106—P8—C65 | −21.4 (3) |
C49—C50—C51—C52 | 0.0 (5) | C111—C106—P8—W2 | 40.1 (3) |
C50—C51—C52—C53 | −1.5 (5) | C107—C106—P8—W2 | −143.1 (2) |
C51—C52—C53—C54 | 1.4 (5) | C64—C65—P8—C112 | 98.2 (2) |
C52—C53—C54—C49 | 0.2 (5) | C64—C65—P8—C106 | −160.90 (18) |
C50—C49—C54—C53 | −1.6 (4) | C64—C65—P8—W2 | −33.7 (2) |
P4—C49—C54—C53 | 174.0 (2) | O2—C6—W1—C5 | 51 (3) |
C60—C55—C56—C57 | 1.2 (6) | O2—C6—W1—P4 | −43 (3) |
C55—C56—C57—C58 | −0.2 (6) | O2—C6—W1—P1 | 137 (3) |
C56—C57—C58—C59 | −0.7 (6) | O2—C6—W1—P2 | −43 (3) |
C57—C58—C59—C60 | 0.6 (6) | O2—C6—W1—P3 | −143 (3) |
C56—C55—C60—C59 | −1.3 (5) | O1—C5—W1—C6 | 52 (3) |
C58—C59—C60—C55 | 0.4 (5) | O1—C5—W1—P4 | 139 (3) |
P5—C64—C65—P8 | 55.6 (2) | O1—C5—W1—P1 | −42 (3) |
P7—C66—C67—P6 | 50.3 (2) | O1—C5—W1—P2 | −142 (3) |
C75—C70—C71—C72 | −1.0 (5) | O1—C5—W1—P3 | −34 (3) |
P5—C70—C71—C72 | 170.8 (3) | C49—P4—W1—C6 | 61.34 (13) |
C70—C71—C72—C73 | −0.7 (5) | C43—P4—W1—C6 | −59.68 (13) |
C71—C72—C73—C74 | 1.6 (5) | C4—P4—W1—C6 | 178.63 (12) |
C72—C73—C74—C75 | −0.9 (5) | C49—P4—W1—C5 | −23.60 (14) |
C73—C74—C75—C70 | −0.8 (5) | C43—P4—W1—C5 | −144.62 (14) |
C71—C70—C75—C74 | 1.7 (5) | C4—P4—W1—C5 | 93.69 (13) |
P5—C70—C75—C74 | −170.3 (2) | C49—P4—W1—P1 | −107 (2) |
C81—C76—C77—C78 | 1.2 (4) | C43—P4—W1—P1 | 132 (2) |
P5—C76—C77—C78 | −175.93 (19) | C4—P4—W1—P1 | 10 (2) |
C76—C77—C78—C79 | 0.2 (4) | C49—P4—W1—P2 | −118.62 (11) |
C77—C78—C79—C80 | −1.2 (4) | C43—P4—W1—P2 | 120.36 (11) |
C78—C79—C80—C81 | 0.8 (4) | C4—P4—W1—P2 | −1.33 (9) |
C79—C80—C81—C76 | 0.6 (4) | C49—P4—W1—P3 | 154.56 (11) |
C77—C76—C81—C80 | −1.5 (4) | C43—P4—W1—P3 | 33.54 (11) |
P5—C76—C81—C80 | 175.7 (2) | C4—P4—W1—P3 | −88.15 (9) |
C87—C82—C83—C84 | −2.1 (4) | C7—P1—W1—C6 | −155.89 (12) |
P6—C82—C83—C84 | 178.7 (2) | C1—P1—W1—C6 | 84.11 (13) |
C82—C83—C84—C85 | 0.7 (5) | C13—P1—W1—C6 | −31.53 (13) |
C83—C84—C85—C86 | 1.5 (5) | C7—P1—W1—C5 | −70.99 (13) |
C84—C85—C86—C87 | −2.1 (5) | C1—P1—W1—C5 | 169.01 (14) |
C85—C86—C87—C82 | 0.6 (4) | C13—P1—W1—C5 | 53.37 (14) |
C83—C82—C87—C86 | 1.4 (4) | C7—P1—W1—P4 | 13 (2) |
P6—C82—C87—C86 | −179.3 (2) | C1—P1—W1—P4 | −107 (2) |
C93—C88—C89—C90 | 1.1 (5) | C13—P1—W1—P4 | 137 (2) |
P6—C88—C89—C90 | −178.8 (3) | C7—P1—W1—P2 | 24.05 (10) |
C88—C89—C90—C91 | 0.4 (5) | C1—P1—W1—P2 | −95.95 (11) |
C89—C90—C91—C92 | −0.8 (5) | C13—P1—W1—P2 | 148.40 (11) |
C90—C91—C92—C93 | −0.3 (5) | C7—P1—W1—P3 | 111.01 (10) |
C91—C92—C93—C88 | 1.8 (5) | C1—P1—W1—P3 | −8.99 (11) |
C89—C88—C93—C92 | −2.1 (4) | C13—P1—W1—P3 | −124.64 (11) |
P6—C88—C93—C92 | 177.8 (2) | C25—P2—W1—C6 | −139.1 (3) |
C99—C94—C95—C96 | 1.2 (4) | C19—P2—W1—C6 | 87.2 (3) |
P7—C94—C95—C96 | −175.7 (2) | C3—P2—W1—C6 | −22.6 (3) |
C94—C95—C96—C97 | 0.1 (5) | C25—P2—W1—C5 | 128.72 (13) |
C95—C96—C97—C98 | −0.7 (5) | C19—P2—W1—C5 | −4.90 (12) |
C96—C97—C98—C99 | 0.2 (5) | C3—P2—W1—C5 | −114.72 (12) |
C97—C98—C99—C94 | 1.1 (5) | C25—P2—W1—P4 | −138.99 (11) |
C95—C94—C99—C98 | −1.7 (4) | C19—P2—W1—P4 | 87.39 (10) |
P7—C94—C99—C98 | 175.2 (2) | C3—P2—W1—P4 | −22.43 (9) |
C105—C100—C101—C102 | 0.8 (4) | C25—P2—W1—P1 | 41.14 (11) |
P7—C100—C101—C102 | −179.4 (2) | C19—P2—W1—P1 | −92.48 (10) |
C100—C101—C102—C103 | −1.1 (4) | C3—P2—W1—P1 | 157.70 (9) |
C101—C102—C103—C104 | 0.9 (5) | C25—P2—W1—P3 | −38.07 (11) |
C102—C103—C104—C105 | −0.3 (4) | C19—P2—W1—P3 | −171.69 (10) |
C101—C100—C105—C104 | −0.3 (4) | C3—P2—W1—P3 | 78.49 (9) |
P7—C100—C105—C104 | 179.9 (2) | C37—P3—W1—C6 | 3.04 (12) |
C103—C104—C105—C100 | 0.1 (4) | C31—P3—W1—C6 | 132.28 (15) |
C111—C106—C107—C108 | 0.5 (4) | C2—P3—W1—C6 | −109.35 (13) |
P8—C106—C107—C108 | −176.4 (2) | C37—P3—W1—C5 | 88.0 (4) |
C106—C107—C108—C109 | −0.1 (5) | C31—P3—W1—C5 | −142.8 (4) |
C107—C108—C109—C110 | −1.0 (5) | C2—P3—W1—C5 | −24.4 (4) |
C108—C109—C110—C111 | 1.6 (5) | C37—P3—W1—P4 | −84.38 (10) |
C107—C106—C111—C110 | 0.2 (5) | C31—P3—W1—P4 | 44.85 (13) |
P8—C106—C111—C110 | 177.1 (3) | C2—P3—W1—P4 | 163.22 (10) |
C109—C110—C111—C106 | −1.2 (5) | C37—P3—W1—P1 | 96.28 (10) |
C117—C112—C113—C114 | 0.0 (4) | C31—P3—W1—P1 | −134.48 (13) |
P8—C112—C113—C114 | −177.3 (3) | C2—P3—W1—P1 | −16.11 (10) |
C112—C113—C114—C115 | 0.3 (5) | C37—P3—W1—P2 | −163.14 (9) |
C113—C114—C115—C116 | 0.0 (5) | C31—P3—W1—P2 | −33.91 (13) |
C114—C115—C116—C117 | −0.5 (5) | C2—P3—W1—P2 | 84.46 (11) |
C115—C116—C117—C112 | 0.8 (5) | O4—C69—W2—C68 | −57 (2) |
C113—C112—C117—C116 | −0.5 (4) | O4—C69—W2—P7 | 38 (2) |
P8—C112—C117—C116 | 176.6 (2) | O4—C69—W2—P8 | −144 (2) |
C123—C118—C119—C120 | 0.3 (6) | O4—C69—W2—P5 | 138 (2) |
C118—C119—C120—C121 | −0.8 (6) | O4—C69—W2—P6 | 24 (3) |
C119—C120—C121—C122 | 0.7 (6) | O3—C68—W2—C69 | −52 (4) |
C120—C121—C122—C123 | 0.0 (6) | O3—C68—W2—P7 | −136 (4) |
C121—C122—C123—C118 | −0.6 (6) | O3—C68—W2—P8 | 40 (4) |
C119—C118—C123—C122 | 0.4 (6) | O3—C68—W2—P5 | 46 (4) |
C129—C124—C125—C126 | 2.1 (12) | O3—C68—W2—P6 | 145 (4) |
C124—C125—C126—C127 | −2.4 (11) | C100—P7—W2—C69 | 73.81 (13) |
C125—C126—C127—C128 | 1.5 (9) | C66—P7—W2—C69 | −165.86 (12) |
C126—C127—C128—C129 | −0.2 (8) | C94—P7—W2—C69 | −50.19 (12) |
C125—C124—C129—C128 | −0.9 (11) | C100—P7—W2—C68 | 158.74 (13) |
C127—C128—C129—C124 | −0.1 (10) | C66—P7—W2—C68 | −80.93 (13) |
C12—C7—P1—C1 | −1.1 (3) | C94—P7—W2—C68 | 34.75 (12) |
C8—C7—P1—C1 | 179.1 (2) | C100—P7—W2—P8 | 49.1 (3) |
C12—C7—P1—C13 | 101.2 (2) | C66—P7—W2—P8 | 169.5 (3) |
C8—C7—P1—C13 | −78.5 (2) | C94—P7—W2—P8 | −74.8 (3) |
C12—C7—P1—W1 | −124.7 (2) | C100—P7—W2—P5 | −21.77 (10) |
C8—C7—P1—W1 | 55.5 (2) | C66—P7—W2—P5 | 98.56 (10) |
C2—C1—P1—C7 | −90.8 (2) | C94—P7—W2—P5 | −145.77 (10) |
C2—C1—P1—C13 | 167.5 (2) | C100—P7—W2—P6 | −110.33 (10) |
C2—C1—P1—W1 | 39.4 (2) | C66—P7—W2—P6 | 10.00 (10) |
C18—C13—P1—C7 | 130.7 (3) | C94—P7—W2—P6 | 125.68 (10) |
C14—C13—P1—C7 | −51.3 (3) | C112—P8—W2—C69 | 143.71 (13) |
C18—C13—P1—C1 | −124.3 (3) | C106—P8—W2—C69 | 21.97 (13) |
C14—C13—P1—C1 | 53.6 (3) | C65—P8—W2—C69 | −94.56 (12) |
C18—C13—P1—W1 | −3.4 (3) | C112—P8—W2—C68 | 58.32 (13) |
C14—C13—P1—W1 | 174.59 (19) | C106—P8—W2—C68 | −63.42 (13) |
C30—C25—P2—C19 | −118.2 (3) | C65—P8—W2—C68 | −179.94 (12) |
C26—C25—P2—C19 | 62.8 (3) | C112—P8—W2—P7 | 168.2 (3) |
C30—C25—P2—C3 | −18.0 (3) | C106—P8—W2—P7 | 46.5 (3) |
C26—C25—P2—C3 | 163.1 (2) | C65—P8—W2—P7 | −70.0 (3) |
C30—C25—P2—W1 | 100.9 (2) | C112—P8—W2—P5 | −120.00 (11) |
C26—C25—P2—W1 | −78.1 (3) | C106—P8—W2—P5 | 118.26 (10) |
C24—C19—P2—C25 | 17.7 (3) | C65—P8—W2—P5 | 1.73 (9) |
C20—C19—P2—C25 | −170.0 (2) | C112—P8—W2—P6 | −32.65 (11) |
C24—C19—P2—C3 | −85.5 (2) | C106—P8—W2—P6 | −154.39 (10) |
C20—C19—P2—C3 | 86.8 (2) | C65—P8—W2—P6 | 89.08 (9) |
C24—C19—P2—W1 | 160.3 (2) | C76—P5—W2—C69 | −128.37 (14) |
C20—C19—P2—W1 | −27.5 (2) | C64—P5—W2—C69 | 114.04 (12) |
C4—C3—P2—C25 | −179.99 (19) | C70—P5—W2—C69 | 6.35 (14) |
C4—C3—P2—C19 | −77.0 (2) | C76—P5—W2—C68 | 134.7 (3) |
C4—C3—P2—W1 | 48.78 (19) | C64—P5—W2—C68 | 17.1 (3) |
C38—C37—P3—C31 | 3.0 (3) | C70—P5—W2—C68 | −90.6 (3) |
C42—C37—P3—C31 | −177.8 (2) | C76—P5—W2—P7 | −43.25 (11) |
C38—C37—P3—C2 | −100.6 (2) | C64—P5—W2—P7 | −160.84 (8) |
C42—C37—P3—C2 | 78.7 (2) | C70—P5—W2—P7 | 91.47 (11) |
C38—C37—P3—W1 | 143.8 (2) | C76—P5—W2—P8 | 141.35 (11) |
C42—C37—P3—W1 | −37.0 (2) | C64—P5—W2—P8 | 23.75 (8) |
C32—C31—P3—C37 | −99.6 (3) | C70—P5—W2—P8 | −83.94 (11) |
C36—C31—P3—C37 | 77.9 (2) | C76—P5—W2—P6 | 36.47 (11) |
C32—C31—P3—C2 | 3.2 (3) | C64—P5—W2—P6 | −81.12 (9) |
C36—C31—P3—C2 | −179.3 (2) | C70—P5—W2—P6 | 171.19 (11) |
C32—C31—P3—W1 | 123.8 (2) | C82—P6—W2—C69 | 145.0 (3) |
C36—C31—P3—W1 | −58.7 (3) | C67—P6—W2—C69 | 27.6 (3) |
C1—C2—P3—C37 | −79.5 (2) | C88—P6—W2—C69 | −85.3 (3) |
C1—C2—P3—C31 | 178.8 (2) | C82—P6—W2—C68 | −134.92 (15) |
C1—C2—P3—W1 | 45.0 (2) | C67—P6—W2—C68 | 107.77 (13) |
C54—C49—P4—C43 | −80.4 (3) | C88—P6—W2—C68 | −5.21 (13) |
C50—C49—P4—C43 | 95.1 (2) | C82—P6—W2—P7 | 130.38 (13) |
C54—C49—P4—C4 | 25.3 (3) | C67—P6—W2—P7 | 13.08 (10) |
C50—C49—P4—C4 | −159.3 (2) | C88—P6—W2—P7 | −99.91 (11) |
C54—C49—P4—W1 | 148.0 (2) | C82—P6—W2—P8 | −47.89 (13) |
C50—C49—P4—W1 | −36.6 (3) | C67—P6—W2—P8 | −165.19 (10) |
C48—C43—P4—C49 | −106.6 (2) | C88—P6—W2—P8 | 81.82 (11) |
C44—C43—P4—C49 | 71.9 (3) | C82—P6—W2—P5 | 30.60 (13) |
C48—C43—P4—C4 | 150.4 (2) | C67—P6—W2—P5 | −86.70 (10) |
C44—C43—P4—C4 | −31.1 (3) | C88—P6—W2—P5 | 160.31 (10) |
Experimental details
Crystal data | |
Chemical formula | [W(CO)2(C26H24P2)2]·1.5C6H6 |
Mr | 1153.82 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 180 |
a, b, c (Å) | 12.675 (2), 18.259 (3), 22.864 (4) |
α, β, γ (°) | 89.15 (2), 87.73 (2), 77.31 (2) |
V (Å3) | 5158.1 (16) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 2.41 |
Crystal size (mm) | 0.40 × 0.24 × 0.12 |
Data collection | |
Diffractometer | Stoe IPDS |
Absorption correction | Numerical (NUMABS32 in X-RED1.08; Stoe & Cie, 1997) |
Tmin, Tmax | 0.446, 0.761 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 47419, 18050, 15173 |
Rint | 0.034 |
(sin θ/λ)max (Å−1) | 0.606 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.022, 0.053, 0.94 |
No. of reflections | 18050 |
No. of parameters | 1262 |
H-atom treatment | H-atom parameters not refined |
Δρmax, Δρmin (e Å−3) | 0.70, −1.27 |
Computer programs: IPDS2.87 (Stoe & Cie, 1997), IPDS2.87, SHELXS97 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997), DIAMOND (Brandenburg, 1996), SHELXL97.
Reaction of the germylenes Cp*GeX (Cp* = C5Me5; X = Cl, Br, I) with the bis-dinitrogen complex trans-[W(dppe)2(N2)2] has been recently shown to provide a convenient route to the complexes trans-[X(dppe)2W≡Ge(η1-Cp*)] (X = Cl, Br, I) bearing a transition metal–germanium triple bond (Filippou et al., 2000). In order to test the influence of a carbonyl ligand on the course of this reaction, the dinitrogen complex trans-[W(CO)(N2)(dppe)2], (2), was prepared from trans-[W(CO)(DMF)(dppe)2] (DMF is N,N'-dimethylformamide), (1) (Ishida et al., 1991). Yellow single crystals of the title compound, (3), as benzene sesquisolvate (1.5C6H6), (3a), were obtained from the washing solution after the isolation of complex (2).
Complex (3) was first prepared by Chatt & Watson (1961), however, its molecular structure in the solid state was unknown to this day. Two distorted octahedral molecules with marginally different bonding parameters and three molecules of benzene are present in the asymmetric unit of the cell. The W—P bonds trans to the carbonyl ligands have an average value of 2.5490 (9) Å, which is considerably larger than that of the W—P bonds cis to the carbonyl ligands [2.4525 (9) Å] indicating the strong trans influence of the CO groups.