Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806041419/lh2200sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536806041419/lh2200Isup2.hkl |
CCDC reference: 627988
Key indicators
- Single-crystal X-ray study
- T = 173 K
- Mean (C-C)= 0.005 Å
- R factor = 0.054
- wR factor = 0.139
- Data-to-parameter ratio = 21.2
checkCIF/PLATON results
No syntax errors found No errors found in this datablock
Data collection: COLLECT (Nonius, 1999); cell refinement: DIRAX/LSQ (Duisenberg et al., 2000); data reduction: EVALCCD (Duisenberg et al., 2003); 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); software used to prepare material for publication: WinGX (Farrugia, 1999).
[Ti2(C3H7O)2(C23H30O2S2)2O] | F(000) = 2200 |
Mr = 1035.15 | Dx = 1.260 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 211 reflections |
a = 13.809 (3) Å | θ = 3.2–20.4° |
b = 22.381 (7) Å | µ = 0.49 mm−1 |
c = 21.435 (7) Å | T = 173 K |
β = 124.53 (2)° | Prism, yellow |
V = 5458 (3) Å3 | 0.38 × 0.20 × 0.13 mm |
Z = 4 |
Bruker Nonius KappaCCD area-detector diffractometer | 12358 independent reflections |
Radiation source: fine-focus sealed tube | 7100 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.063 |
Detector resolution: 9 pixels mm-1 | θmax = 27.5°, θmin = 3.1° |
φ scans, and ω scans with κ offsets | h = −17→17 |
Absorption correction: multi-scan (SADABS; Bruker Nonius, 2002) | k = −29→27 |
Tmin = 0.835, Tmax = 0.939 | l = −27→27 |
41182 measured reflections |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.054 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.139 | H-atom parameters constrained |
S = 0.97 | w = 1/[σ2(Fo2) + (0.0655P)2 + 1.7819P] where P = (Fo2 + 2Fc2)/3 |
12358 reflections | (Δ/σ)max = 0.001 |
584 parameters | Δρmax = 0.72 e Å−3 |
4 restraints | Δρmin = −0.50 e Å−3 |
Experimental. All operations were performed under a nitrogen atmosphere using standard Schlenk-line or glove-box techniques. Solvents were purified, dried and distilled under nitrogen using standard techniques. 2-Hydroxy-3-tert-butyl-5-methylbenzenethiol was prepared according to published procedures (Pastor & Denney, 1988). All other chemicals were commercially available and used after appropriate purification. NMR spectra were recorded on a Bruker DRX 400 spectrometer (1H, 400 MHz; 13C, 101 MHz) in CDCl3 at 298 K, unless otherwise stated. Chemical shifts for 1H and 13C spectra were referenced internally using the residual protio solvent resonances and reported relative to tetramethylsilane. The first intermediate compound, 2,2'-(methylenedithio)bis(4-methyl-6-tert-butylphenol), (II), was prepared as follows. Into a 500 ml two-necked flask equipped with magnetic stirrer and condenser were introduced sequentially 3-tert-butyl-2-hydroxy-5-methylbenzenethiol (42.09 g, 0.184 mol), methanol (80 ml) and sodium hydroxyde (7.36 g, 0.184 mol). The resulting mixture was heated [To what temperature?] under magnetic stirring until complete dissolution of the sodium hydroxyde. Dibromomethane (16.02 g, 92.2 mmol) was then added carefully and the reaction mixture kept under reflux for 2 h. The solvent was then removed under reduced pressure and the residue was extracted with diethyl ether (3 × 200 ml). The organic layers were collected, washed with water and dried over magnesium sulfate. Removal of the solvent under reduced pressure and recrystallization from acetone afforded the product as white needles (15.5 g, 36% yield). 1H NMR (CDCl3, 298 K, δ, p.p.m.): 1.39 (tBu, s, 18H), 2.25 (CH3, s, 6H), 3.92 (CH2, s, 4H), 6.76 (OH, s, 2H), 7.11 (ArH, s, 4H); 13C NMR (CDCl3, 25% C, δ, p.p.m.): 20.5 (4-CH3), 29.2 [C(CH3)], 34.8 [C(CH3)], 44.6 (S—CH2), 118.0 (C2), 128.9 (C4), 130.0(C5), 133.4 (C3), 135.9 (C6), 153.0 (C1). The second intermediate compound, diisopropoxy[2,2'-(methylenedithio)bis(4-methyl-6-tert- butylphenolato)]titanium, (III), was prepared as follows. Compound (II) (0.63 g, 1.55 mmol), toluene (15 ml) and titanium isopropoxide (0.44 g, 1.55 mmol) were introduced sequentially into a 100 ml glass flask. The mixture was stirred magnetically for 2 h at room temperature. Removal of the solvent under vacuum and washing with pentane gave the product as a yellow powder (0.8 g, 91% yield). 1H NMR (CDCl3, 298 K, δ, p.p.m.): 1.18 [CH(CH3)2, d, 12H], 1.47 (tBu, s, 18H), 2.22 (CH3, s, 6H), 4.05 (CH2, s, 4H), 4.76 [CH (CH3)2, m, 2H], 7.00–7.07 (ArH, m, 4H). 13C NMR (CDCl3, 25% C, δ, p.p.m.): 20.6 (4-CH3), 26.1 [CH(CH3)2], 29.4 [C (CH3)3], 35.1 [C (CH3)3], 51.0 (S—CH2), 80.4 [O—CH(CH3)2], 122.8 (C2), 127.0 (C4), 130.1 [C5 (C3)], 131.0 [C3 (C5)], 137.1 (C6), 165.4 (C1). Attempts to crystallize (III) from hexane afforded the title complex, (I), as yellow crystals. X-ray data were recorded at 173 K by means of an Oxford Cryostream 700 apparatus. |
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Ti1 | 0.69566 (4) | 0.26456 (2) | 0.27376 (3) | 0.02601 (15) | |
Ti2 | 0.88757 (4) | 0.26273 (2) | 0.47548 (3) | 0.02561 (14) | |
S1 | 0.49118 (7) | 0.29808 (3) | 0.13867 (4) | 0.0291 (2) | |
S2 | 0.52724 (7) | 0.31532 (3) | 0.29149 (4) | 0.02811 (19) | |
S3 | 0.94851 (7) | 0.22886 (4) | 0.61727 (5) | 0.0319 (2) | |
S4 | 0.70786 (7) | 0.20294 (3) | 0.47408 (5) | 0.0296 (2) | |
O1 | 0.71460 (17) | 0.34698 (9) | 0.25738 (11) | 0.0277 (5) | |
O2 | 0.60027 (17) | 0.20093 (8) | 0.26771 (11) | 0.0282 (5) | |
O3 | 0.74803 (19) | 0.23043 (10) | 0.22399 (13) | 0.0392 (6) | |
O4 | 0.81017 (16) | 0.26087 (9) | 0.37318 (11) | 0.0320 (5) | |
O5 | 0.95788 (17) | 0.18494 (9) | 0.49482 (11) | 0.0298 (5) | |
O6 | 0.79855 (17) | 0.32180 (8) | 0.48513 (11) | 0.0290 (5) | |
O7 | 1.01420 (17) | 0.30618 (9) | 0.51142 (13) | 0.0392 (6) | |
C1 | 0.6779 (2) | 0.37211 (13) | 0.19050 (16) | 0.0242 (7) | |
C2 | 0.7457 (3) | 0.41467 (13) | 0.18291 (17) | 0.0266 (7) | |
C3 | 0.6981 (3) | 0.43675 (13) | 0.11010 (18) | 0.0334 (8) | |
H3 | 0.7423 | 0.4657 | 0.1040 | 0.033* | |
C4 | 0.5903 (3) | 0.41935 (14) | 0.04579 (17) | 0.0344 (8) | |
C5 | 0.5244 (3) | 0.37831 (13) | 0.05517 (17) | 0.0298 (7) | |
H5 | 0.4494 | 0.3663 | 0.0129 | 0.030* | |
C6 | 0.5677 (3) | 0.35481 (13) | 0.12625 (16) | 0.0266 (7) | |
C7 | 0.8671 (3) | 0.43471 (14) | 0.25125 (18) | 0.0334 (8) | |
C8 | 0.8532 (3) | 0.46502 (16) | 0.30954 (19) | 0.0444 (9) | |
H8A | 0.8149 | 0.4375 | 0.3247 | 0.044* | |
H8B | 0.8050 | 0.5010 | 0.2872 | 0.044* | |
H8C | 0.9308 | 0.4761 | 0.3541 | 0.044* | |
C9 | 0.9482 (3) | 0.38024 (16) | 0.28709 (19) | 0.0439 (9) | |
H9A | 0.9171 | 0.3532 | 0.3077 | 0.044* | |
H9B | 1.0271 | 0.3935 | 0.3280 | 0.044* | |
H9C | 0.9523 | 0.3592 | 0.2485 | 0.044* | |
C10 | 0.9264 (3) | 0.47847 (17) | 0.2280 (2) | 0.0524 (10) | |
H10A | 0.9360 | 0.4596 | 0.1906 | 0.052* | |
H10B | 1.0037 | 0.4896 | 0.2727 | 0.052* | |
H10C | 0.8776 | 0.5143 | 0.2059 | 0.052* | |
C11 | 0.5483 (3) | 0.44302 (15) | −0.03136 (18) | 0.0440 (9) | |
H11A | 0.4638 | 0.4514 | −0.0598 | 0.044* | |
H11B | 0.5628 | 0.4131 | −0.0585 | 0.044* | |
H11C | 0.5908 | 0.4798 | −0.0260 | 0.044* | |
C12 | 0.4451 (3) | 0.33738 (14) | 0.19257 (16) | 0.0308 (7) | |
H12A | 0.4549 | 0.3809 | 0.1896 | 0.031* | |
H12B | 0.3606 | 0.3296 | 0.1690 | 0.031* | |
C13 | 0.5122 (2) | 0.19467 (13) | 0.27633 (15) | 0.0229 (7) | |
C14 | 0.4687 (2) | 0.13725 (13) | 0.27596 (15) | 0.0249 (7) | |
C15 | 0.3762 (3) | 0.13518 (14) | 0.28447 (17) | 0.0325 (8) | |
H15 | 0.3456 | 0.0971 | 0.2843 | 0.032* | |
C16 | 0.3257 (3) | 0.18535 (15) | 0.29327 (19) | 0.0360 (8) | |
C17 | 0.3697 (3) | 0.24078 (14) | 0.29378 (17) | 0.0308 (7) | |
H17 | 0.3369 | 0.2758 | 0.2997 | 0.031* | |
C18 | 0.4624 (2) | 0.24519 (13) | 0.28555 (16) | 0.0247 (7) | |
C19 | 0.5221 (3) | 0.08122 (13) | 0.26593 (17) | 0.0298 (7) | |
C20 | 0.4673 (3) | 0.02338 (14) | 0.27034 (19) | 0.0404 (9) | |
H20A | 0.5024 | −0.0109 | 0.2616 | 0.040* | |
H20B | 0.3824 | 0.0240 | 0.2317 | 0.040* | |
H20C | 0.4821 | 0.0201 | 0.3206 | 0.040* | |
C21 | 0.6550 (3) | 0.07826 (14) | 0.32870 (17) | 0.0334 (8) | |
H21A | 0.6898 | 0.0442 | 0.3194 | 0.033* | |
H21B | 0.6667 | 0.0734 | 0.3780 | 0.033* | |
H21C | 0.6929 | 0.1153 | 0.3286 | 0.033* | |
C22 | 0.5015 (3) | 0.08341 (14) | 0.18777 (17) | 0.0374 (8) | |
H22A | 0.5399 | 0.0491 | 0.1821 | 0.037* | |
H22B | 0.5347 | 0.1205 | 0.1830 | 0.037* | |
H22C | 0.4170 | 0.0821 | 0.1483 | 0.037* | |
C23 | 0.2244 (3) | 0.17876 (18) | 0.3017 (3) | 0.0617 (12) | |
H23A | 0.2317 | 0.1407 | 0.3266 | 0.062* | |
H23B | 0.1500 | 0.1795 | 0.2515 | 0.062* | |
H23C | 0.2261 | 0.2118 | 0.3323 | 0.062* | |
C24 | 0.8123 (4) | 0.18753 (19) | 0.2110 (3) | 0.0621 (12) | |
H24 | 0.8010 | 0.1980 | 0.1620 | 0.062* | |
C25 | 0.7695 (4) | 0.1269 (2) | 0.2043 (3) | 0.0824 (15) | |
H25A | 0.6879 | 0.1243 | 0.1601 | 0.082* | |
H25B | 0.7733 | 0.1163 | 0.2500 | 0.082* | |
H25C | 0.8184 | 0.0992 | 0.1980 | 0.082* | |
C26 | 0.9402 (3) | 0.1967 (2) | 0.2730 (3) | 0.0807 (16) | |
H26A | 0.9649 | 0.2366 | 0.2685 | 0.081* | |
H26B | 0.9873 | 0.1664 | 0.2685 | 0.081* | |
H26C | 0.9519 | 0.1928 | 0.3224 | 0.081* | |
C27 | 1.0365 (2) | 0.15640 (13) | 0.55948 (16) | 0.0246 (7) | |
C28 | 1.1113 (2) | 0.11112 (13) | 0.56304 (16) | 0.0247 (7) | |
C29 | 1.1871 (2) | 0.08437 (13) | 0.63365 (17) | 0.0281 (7) | |
H29 | 1.2372 | 0.0535 | 0.6371 | 0.028* | |
C30 | 1.1948 (3) | 0.09929 (14) | 0.69919 (17) | 0.0291 (7) | |
C31 | 1.1230 (3) | 0.14429 (13) | 0.69443 (17) | 0.0285 (7) | |
H31 | 1.1273 | 0.1565 | 0.7384 | 0.028* | |
C32 | 1.0445 (2) | 0.17175 (13) | 0.62566 (16) | 0.0260 (7) | |
C33 | 1.1112 (3) | 0.09474 (14) | 0.49364 (17) | 0.0306 (7) | |
C34 | 1.1974 (3) | 0.04412 (16) | 0.51056 (19) | 0.0476 (10) | |
H34A | 1.1943 | 0.0348 | 0.4648 | 0.048* | |
H34B | 1.1759 | 0.0086 | 0.5269 | 0.048* | |
H34C | 1.2773 | 0.0566 | 0.5509 | 0.048* | |
C35 | 1.1490 (3) | 0.14903 (16) | 0.46955 (19) | 0.0420 (9) | |
H35A | 1.1493 | 0.1389 | 0.4252 | 0.042* | |
H35B | 1.2282 | 0.1613 | 0.5112 | 0.042* | |
H35C | 1.0939 | 0.1819 | 0.4568 | 0.042* | |
C36 | 0.9883 (3) | 0.07429 (15) | 0.42800 (18) | 0.0401 (9) | |
H36A | 0.9897 | 0.0646 | 0.3839 | 0.040* | |
H36B | 0.9317 | 0.1065 | 0.4148 | 0.040* | |
H36C | 0.9651 | 0.0388 | 0.4434 | 0.040* | |
C37 | 1.2807 (3) | 0.06718 (16) | 0.77341 (18) | 0.0459 (9) | |
H37A | 1.2714 | 0.0823 | 0.8127 | 0.046* | |
H37B | 1.3612 | 0.0745 | 0.7886 | 0.046* | |
H37C | 1.2647 | 0.0242 | 0.7668 | 0.046* | |
C38 | 0.8114 (3) | 0.18638 (14) | 0.57367 (18) | 0.0352 (8) | |
H38A | 0.8299 | 0.1432 | 0.5796 | 0.035* | |
H38B | 0.7742 | 0.1954 | 0.6008 | 0.035* | |
C39 | 0.7027 (2) | 0.32310 (13) | 0.48614 (16) | 0.0238 (7) | |
C40 | 0.6562 (3) | 0.37823 (13) | 0.49089 (16) | 0.0261 (7) | |
C41 | 0.5543 (3) | 0.37524 (14) | 0.48916 (17) | 0.0326 (8) | |
H41 | 0.5219 | 0.4116 | 0.4923 | 0.033* | |
C42 | 0.4962 (3) | 0.32204 (15) | 0.48309 (18) | 0.0344 (8) | |
C43 | 0.5440 (3) | 0.26911 (14) | 0.47998 (17) | 0.0284 (7) | |
H43 | 0.5076 | 0.2322 | 0.4770 | 0.028* | |
C44 | 0.6466 (2) | 0.26989 (13) | 0.48121 (16) | 0.0258 (7) | |
C45 | 0.7136 (3) | 0.43741 (13) | 0.49450 (18) | 0.0341 (8) | |
C46 | 0.8438 (3) | 0.43846 (16) | 0.5621 (2) | 0.0503 (10) | |
H46A | 0.8800 | 0.4760 | 0.5617 | 0.050* | |
H46B | 0.8852 | 0.4047 | 0.5582 | 0.050* | |
H46C | 0.8488 | 0.4354 | 0.6095 | 0.050* | |
C47 | 0.7071 (3) | 0.44559 (14) | 0.42106 (19) | 0.0407 (9) | |
H47A | 0.7445 | 0.4835 | 0.4231 | 0.041* | |
H47B | 0.6247 | 0.4460 | 0.3777 | 0.041* | |
H47C | 0.7481 | 0.4125 | 0.4155 | 0.041* | |
C48 | 0.6523 (4) | 0.49092 (14) | 0.5025 (2) | 0.0557 (11) | |
H48A | 0.6897 | 0.5280 | 0.5021 | 0.056* | |
H48B | 0.6589 | 0.4878 | 0.5504 | 0.056* | |
H48C | 0.5691 | 0.4912 | 0.4603 | 0.056* | |
C49 | 0.3845 (3) | 0.32339 (17) | 0.4808 (2) | 0.0540 (11) | |
H49A | 0.3969 | 0.3481 | 0.5225 | 0.054* | |
H49B | 0.3640 | 0.2826 | 0.4860 | 0.054* | |
H49C | 0.3204 | 0.3403 | 0.4325 | 0.054* | |
C50A | 1.1222 (7) | 0.3366 (4) | 0.5614 (6) | 0.045 (3)* | 0.398 (9) |
H50A | 1.1333 | 0.3499 | 0.6096 | 0.045* | 0.398 (9) |
C51A | 1.2224 (9) | 0.2984 (5) | 0.5734 (8) | 0.049 (4)* | 0.398 (9) |
H51A | 1.2220 | 0.2655 | 0.6034 | 0.049* | 0.398 (9) |
H51B | 1.2962 | 0.3208 | 0.6041 | 0.049* | 0.398 (9) |
H51C | 1.2155 | 0.2823 | 0.5285 | 0.049* | 0.398 (9) |
C52A | 1.1245 (8) | 0.3875 (4) | 0.5152 (5) | 0.039 (3)* | 0.398 (9) |
H52A | 1.0962 | 0.3732 | 0.4643 | 0.039* | 0.398 (9) |
H52B | 1.2054 | 0.4020 | 0.5405 | 0.039* | 0.398 (9) |
H52C | 1.0740 | 0.4201 | 0.5114 | 0.039* | 0.398 (9) |
C50B | 1.1207 (5) | 0.3292 (2) | 0.5222 (3) | 0.047 (2)* | 0.602 (9) |
H50B | 1.1224 | 0.3267 | 0.4763 | 0.047* | 0.602 (9) |
C51B | 1.2194 (5) | 0.2954 (3) | 0.5906 (4) | 0.037 (2)* | 0.602 (9) |
H51D | 1.2195 | 0.2545 | 0.5744 | 0.037* | 0.602 (9) |
H51E | 1.2144 | 0.2944 | 0.6344 | 0.037* | 0.602 (9) |
H51F | 1.2921 | 0.3157 | 0.6046 | 0.037* | 0.602 (9) |
C52B | 1.1199 (8) | 0.3926 (3) | 0.5475 (6) | 0.100 (3)* | 0.602 (9) |
H52D | 1.0502 | 0.4142 | 0.5074 | 0.100* | 0.602 (9) |
H52E | 1.1909 | 0.4136 | 0.5595 | 0.100* | 0.602 (9) |
H52F | 1.1191 | 0.3906 | 0.5928 | 0.100* | 0.602 (9) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ti1 | 0.0203 (3) | 0.0268 (3) | 0.0319 (3) | 0.0052 (2) | 0.0155 (2) | 0.0083 (3) |
Ti2 | 0.0204 (3) | 0.0222 (3) | 0.0334 (3) | 0.0036 (2) | 0.0148 (2) | 0.0077 (3) |
S1 | 0.0257 (4) | 0.0251 (4) | 0.0304 (4) | −0.0014 (3) | 0.0123 (3) | −0.0007 (3) |
S2 | 0.0271 (4) | 0.0219 (4) | 0.0334 (4) | 0.0005 (3) | 0.0160 (4) | −0.0014 (3) |
S3 | 0.0340 (4) | 0.0277 (4) | 0.0363 (5) | 0.0077 (4) | 0.0214 (4) | 0.0030 (4) |
S4 | 0.0314 (4) | 0.0186 (4) | 0.0412 (5) | 0.0015 (3) | 0.0221 (4) | 0.0023 (4) |
O1 | 0.0272 (11) | 0.0287 (11) | 0.0244 (11) | −0.0031 (9) | 0.0130 (9) | 0.0035 (9) |
O2 | 0.0290 (11) | 0.0205 (11) | 0.0430 (13) | 0.0033 (9) | 0.0252 (10) | 0.0027 (10) |
O3 | 0.0384 (13) | 0.0412 (14) | 0.0507 (14) | 0.0106 (11) | 0.0329 (12) | 0.0063 (12) |
O4 | 0.0244 (11) | 0.0338 (12) | 0.0343 (12) | 0.0069 (10) | 0.0146 (10) | 0.0134 (10) |
O5 | 0.0314 (12) | 0.0300 (12) | 0.0279 (11) | 0.0110 (10) | 0.0167 (10) | 0.0068 (10) |
O6 | 0.0268 (11) | 0.0185 (11) | 0.0436 (13) | 0.0016 (9) | 0.0210 (10) | 0.0056 (10) |
O7 | 0.0215 (11) | 0.0377 (13) | 0.0542 (14) | −0.0031 (10) | 0.0189 (11) | 0.0041 (11) |
C1 | 0.0269 (16) | 0.0227 (16) | 0.0233 (16) | 0.0052 (13) | 0.0144 (14) | 0.0032 (13) |
C2 | 0.0302 (17) | 0.0227 (16) | 0.0295 (17) | 0.0008 (14) | 0.0186 (14) | 0.0014 (14) |
C3 | 0.043 (2) | 0.0220 (17) | 0.046 (2) | 0.0051 (15) | 0.0320 (18) | 0.0073 (16) |
C4 | 0.050 (2) | 0.0280 (18) | 0.0284 (18) | 0.0136 (16) | 0.0241 (17) | 0.0066 (15) |
C5 | 0.0319 (17) | 0.0272 (17) | 0.0255 (16) | 0.0054 (15) | 0.0134 (14) | 0.0012 (14) |
C6 | 0.0277 (16) | 0.0227 (16) | 0.0294 (17) | 0.0039 (13) | 0.0161 (14) | 0.0031 (14) |
C7 | 0.0321 (18) | 0.0359 (19) | 0.0380 (19) | −0.0094 (15) | 0.0235 (16) | −0.0038 (16) |
C8 | 0.039 (2) | 0.049 (2) | 0.046 (2) | −0.0162 (18) | 0.0246 (17) | −0.0175 (18) |
C9 | 0.0275 (18) | 0.058 (2) | 0.044 (2) | −0.0022 (18) | 0.0188 (17) | −0.0009 (19) |
C10 | 0.047 (2) | 0.061 (3) | 0.054 (2) | −0.021 (2) | 0.0309 (19) | −0.008 (2) |
C11 | 0.064 (2) | 0.038 (2) | 0.0369 (19) | 0.0111 (19) | 0.0332 (19) | 0.0084 (17) |
C12 | 0.0264 (16) | 0.0285 (17) | 0.0371 (18) | 0.0074 (14) | 0.0177 (15) | 0.0077 (15) |
C13 | 0.0198 (15) | 0.0265 (17) | 0.0225 (15) | 0.0011 (13) | 0.0120 (13) | 0.0019 (13) |
C14 | 0.0227 (15) | 0.0271 (17) | 0.0210 (15) | −0.0017 (13) | 0.0101 (13) | 0.0001 (13) |
C15 | 0.0294 (17) | 0.0301 (18) | 0.0361 (18) | −0.0038 (15) | 0.0174 (15) | 0.0031 (15) |
C16 | 0.0277 (17) | 0.045 (2) | 0.042 (2) | 0.0019 (16) | 0.0238 (16) | 0.0046 (17) |
C17 | 0.0289 (17) | 0.0318 (18) | 0.0361 (18) | 0.0098 (15) | 0.0211 (15) | 0.0034 (15) |
C18 | 0.0224 (15) | 0.0241 (16) | 0.0258 (16) | −0.0001 (13) | 0.0125 (13) | 0.0018 (13) |
C19 | 0.0335 (18) | 0.0214 (16) | 0.0316 (18) | 0.0014 (14) | 0.0167 (15) | 0.0010 (14) |
C20 | 0.050 (2) | 0.0284 (18) | 0.042 (2) | −0.0055 (17) | 0.0250 (18) | −0.0058 (16) |
C21 | 0.0405 (19) | 0.0268 (17) | 0.0356 (18) | 0.0078 (15) | 0.0230 (16) | 0.0046 (15) |
C22 | 0.041 (2) | 0.0321 (19) | 0.0343 (19) | 0.0050 (16) | 0.0189 (16) | −0.0012 (15) |
C23 | 0.054 (2) | 0.058 (3) | 0.102 (3) | 0.001 (2) | 0.061 (3) | 0.007 (2) |
C24 | 0.055 (3) | 0.060 (3) | 0.084 (3) | 0.014 (2) | 0.047 (3) | 0.012 (2) |
C25 | 0.102 (4) | 0.069 (3) | 0.098 (4) | 0.017 (3) | 0.070 (3) | −0.012 (3) |
C26 | 0.049 (3) | 0.106 (4) | 0.100 (4) | 0.033 (3) | 0.050 (3) | 0.047 (3) |
C27 | 0.0227 (15) | 0.0207 (16) | 0.0276 (16) | 0.0017 (13) | 0.0127 (14) | 0.0048 (13) |
C28 | 0.0199 (15) | 0.0210 (16) | 0.0305 (17) | 0.0007 (13) | 0.0127 (14) | 0.0028 (14) |
C29 | 0.0239 (16) | 0.0225 (16) | 0.0353 (18) | 0.0069 (13) | 0.0152 (14) | 0.0043 (14) |
C30 | 0.0271 (17) | 0.0296 (17) | 0.0282 (17) | 0.0031 (14) | 0.0143 (14) | 0.0066 (14) |
C31 | 0.0277 (16) | 0.0341 (18) | 0.0241 (16) | −0.0021 (15) | 0.0150 (14) | 0.0015 (14) |
C32 | 0.0245 (16) | 0.0216 (16) | 0.0311 (17) | 0.0020 (13) | 0.0154 (14) | 0.0025 (14) |
C33 | 0.0284 (17) | 0.0300 (17) | 0.0302 (17) | 0.0067 (14) | 0.0147 (15) | 0.0007 (15) |
C34 | 0.050 (2) | 0.056 (2) | 0.0363 (19) | 0.0267 (19) | 0.0241 (18) | 0.0041 (18) |
C35 | 0.042 (2) | 0.053 (2) | 0.0364 (19) | 0.0033 (18) | 0.0256 (17) | 0.0012 (17) |
C36 | 0.041 (2) | 0.036 (2) | 0.0349 (18) | 0.0010 (17) | 0.0163 (16) | −0.0058 (16) |
C37 | 0.048 (2) | 0.050 (2) | 0.036 (2) | 0.0181 (19) | 0.0218 (18) | 0.0120 (18) |
C38 | 0.0318 (18) | 0.0307 (18) | 0.049 (2) | 0.0089 (15) | 0.0267 (16) | 0.0160 (16) |
C39 | 0.0228 (15) | 0.0211 (16) | 0.0255 (16) | 0.0033 (13) | 0.0126 (13) | 0.0032 (13) |
C40 | 0.0302 (17) | 0.0230 (16) | 0.0267 (16) | 0.0024 (14) | 0.0171 (14) | 0.0012 (13) |
C41 | 0.043 (2) | 0.0237 (17) | 0.0400 (19) | 0.0108 (15) | 0.0288 (17) | 0.0052 (15) |
C42 | 0.0305 (18) | 0.038 (2) | 0.0398 (19) | 0.0076 (16) | 0.0229 (16) | 0.0089 (16) |
C43 | 0.0254 (16) | 0.0252 (17) | 0.0358 (17) | −0.0023 (14) | 0.0181 (14) | 0.0030 (15) |
C44 | 0.0247 (16) | 0.0193 (16) | 0.0319 (17) | −0.0001 (13) | 0.0151 (14) | −0.0002 (14) |
C45 | 0.043 (2) | 0.0208 (16) | 0.044 (2) | −0.0001 (15) | 0.0280 (17) | −0.0012 (15) |
C46 | 0.054 (2) | 0.038 (2) | 0.052 (2) | −0.0201 (19) | 0.026 (2) | −0.0089 (19) |
C47 | 0.060 (2) | 0.0202 (17) | 0.052 (2) | 0.0009 (16) | 0.0374 (19) | 0.0065 (16) |
C48 | 0.088 (3) | 0.0223 (18) | 0.086 (3) | −0.001 (2) | 0.067 (3) | −0.004 (2) |
C49 | 0.047 (2) | 0.046 (2) | 0.091 (3) | 0.0125 (19) | 0.052 (2) | 0.015 (2) |
Ti1—O3 | 1.766 (2) | C24—C25 | 1.454 (6) |
Ti1—O4 | 1.797 (2) | C24—C26 | 1.506 (6) |
Ti1—O2 | 1.894 (2) | C24—H24 | 1.0000 |
Ti1—O1 | 1.923 (2) | C25—H25A | 0.9800 |
Ti1—S1 | 2.7660 (13) | C25—H25B | 0.9801 |
Ti1—S2 | 2.8011 (11) | C25—H25C | 0.9800 |
Ti2—O7 | 1.752 (2) | C26—H26A | 0.9800 |
Ti2—O4 | 1.815 (2) | C26—H26B | 0.9800 |
Ti2—O6 | 1.895 (2) | C26—H26C | 0.9800 |
Ti2—O5 | 1.921 (2) | C27—C32 | 1.402 (4) |
Ti2—S3 | 2.7605 (14) | C27—C28 | 1.418 (4) |
Ti2—S4 | 2.8046 (11) | C28—C29 | 1.396 (4) |
S1—C6 | 1.766 (3) | C28—C33 | 1.531 (4) |
S1—C12 | 1.829 (3) | C29—C30 | 1.388 (4) |
S2—C18 | 1.776 (3) | C29—H29 | 0.9500 |
S2—C12 | 1.816 (3) | C30—C31 | 1.376 (4) |
S3—C32 | 1.776 (3) | C30—C37 | 1.521 (4) |
S3—C38 | 1.832 (3) | C31—C32 | 1.383 (4) |
S4—C44 | 1.770 (3) | C31—H31 | 0.9500 |
S4—C38 | 1.811 (3) | C33—C35 | 1.524 (4) |
O1—C1 | 1.343 (3) | C33—C34 | 1.531 (4) |
O2—C13 | 1.337 (3) | C33—C36 | 1.537 (4) |
O3—C24 | 1.437 (4) | C34—H34A | 0.9799 |
O5—C27 | 1.342 (3) | C34—H34B | 0.9800 |
O6—C39 | 1.336 (3) | C34—H34C | 0.9800 |
O7—C50A | 1.423 (9) | C35—H35A | 0.9800 |
O7—C50B | 1.447 (7) | C35—H35B | 0.9800 |
C1—C2 | 1.408 (4) | C35—H35C | 0.9800 |
C1—C6 | 1.409 (4) | C36—H36A | 0.9800 |
C2—C3 | 1.396 (4) | C36—H36B | 0.9800 |
C2—C7 | 1.541 (4) | C36—H36C | 0.9800 |
C3—C4 | 1.393 (4) | C37—H37A | 0.9800 |
C3—H3 | 0.9500 | C37—H37B | 0.9800 |
C4—C5 | 1.386 (4) | C37—H37C | 0.9800 |
C4—C11 | 1.505 (4) | C38—H38A | 0.9900 |
C5—C6 | 1.386 (4) | C38—H38B | 0.9900 |
C5—H5 | 0.9500 | C39—C44 | 1.392 (4) |
C7—C8 | 1.526 (4) | C39—C40 | 1.421 (4) |
C7—C10 | 1.530 (4) | C40—C41 | 1.389 (4) |
C7—C9 | 1.535 (5) | C40—C45 | 1.523 (4) |
C8—H8A | 0.9800 | C41—C42 | 1.400 (4) |
C8—H8B | 0.9800 | C41—H41 | 0.9500 |
C8—H8C | 0.9800 | C42—C43 | 1.376 (4) |
C9—H9A | 0.9800 | C42—C49 | 1.515 (4) |
C9—H9B | 0.9800 | C43—C44 | 1.402 (4) |
C9—H9C | 0.9800 | C43—H43 | 0.9500 |
C10—H10A | 0.9800 | C45—C48 | 1.531 (4) |
C10—H10B | 0.9800 | C45—C47 | 1.536 (5) |
C10—H10C | 0.9800 | C45—C46 | 1.542 (4) |
C11—H11A | 0.9800 | C46—H46A | 0.9800 |
C11—H11B | 0.9800 | C46—H46B | 0.9800 |
C11—H11C | 0.9800 | C46—H46C | 0.9800 |
C12—H12A | 0.9900 | C47—H47A | 0.9800 |
C12—H12B | 0.9900 | C47—H47B | 0.9800 |
C13—C18 | 1.395 (4) | C47—H47C | 0.9800 |
C13—C14 | 1.417 (4) | C48—H48A | 0.9800 |
C14—C15 | 1.389 (4) | C48—H48B | 0.9800 |
C14—C19 | 1.530 (4) | C48—H48C | 0.9800 |
C15—C16 | 1.390 (4) | C49—H49A | 0.9800 |
C15—H15 | 0.9500 | C49—H49B | 0.9800 |
C16—C17 | 1.379 (4) | C49—H49C | 0.9800 |
C16—C23 | 1.515 (4) | C50A—C51A | 1.5202 (11) |
C17—C18 | 1.390 (4) | C50A—C52A | 1.5209 (11) |
C17—H17 | 0.9500 | C50A—H50A | 1.0000 |
C19—C20 | 1.528 (4) | C51A—H51A | 0.9800 |
C19—C22 | 1.533 (4) | C51A—H51B | 0.9800 |
C19—C21 | 1.544 (4) | C51A—H51C | 0.9800 |
C20—H20A | 0.9800 | C52A—H52A | 0.9800 |
C20—H20B | 0.9800 | C52A—H52B | 0.9800 |
C20—H20C | 0.9800 | C52A—H52C | 0.9800 |
C21—H21A | 0.9800 | C50B—C51B | 1.5209 (11) |
C21—H21B | 0.9800 | C50B—C52B | 1.5212 (11) |
C21—H21C | 0.9800 | C50B—H50B | 1.0000 |
C22—H22A | 0.9800 | C51B—H51D | 0.9800 |
C22—H22B | 0.9800 | C51B—H51E | 0.9800 |
C22—H22C | 0.9800 | C51B—H51F | 0.9800 |
C23—H23A | 0.9800 | C52B—H52D | 0.9800 |
C23—H23B | 0.9800 | C52B—H52E | 0.9800 |
C23—H23C | 0.9800 | C52B—H52F | 0.9800 |
O3—Ti1—O4 | 108.07 (10) | C28—C29—H29 | 117.4 |
O3—Ti1—O2 | 98.07 (10) | C31—C30—C29 | 117.5 (3) |
O4—Ti1—O2 | 99.04 (9) | C31—C30—C37 | 121.7 (3) |
O3—Ti1—O1 | 99.20 (10) | C29—C30—C37 | 120.8 (3) |
O4—Ti1—O1 | 98.12 (9) | C30—C31—C32 | 120.0 (3) |
O2—Ti1—O1 | 150.47 (9) | C30—C31—H31 | 120.0 |
O3—Ti1—S1 | 90.54 (8) | C32—C31—H31 | 120.0 |
O4—Ti1—S1 | 160.72 (8) | C31—C32—C27 | 122.3 (3) |
O2—Ti1—S1 | 82.80 (7) | C31—C32—S3 | 121.1 (2) |
O1—Ti1—S1 | 73.29 (6) | C27—C32—S3 | 116.6 (2) |
O3—Ti1—S2 | 155.94 (8) | C35—C33—C34 | 107.5 (3) |
O4—Ti1—S2 | 95.62 (8) | C35—C33—C28 | 109.1 (3) |
O2—Ti1—S2 | 73.47 (6) | C34—C33—C28 | 112.0 (3) |
O1—Ti1—S2 | 81.09 (7) | C35—C33—C36 | 109.9 (3) |
S1—Ti1—S2 | 66.34 (3) | C34—C33—C36 | 107.7 (3) |
O7—Ti2—O4 | 107.54 (11) | C28—C33—C36 | 110.7 (3) |
O7—Ti2—O6 | 96.45 (10) | C33—C34—H34A | 109.5 |
O4—Ti2—O6 | 100.01 (9) | C33—C34—H34B | 109.5 |
O7—Ti2—O5 | 98.73 (10) | H34A—C34—H34B | 109.5 |
O4—Ti2—O5 | 96.85 (9) | C33—C34—H34C | 109.5 |
O6—Ti2—O5 | 152.71 (9) | H34A—C34—H34C | 109.5 |
O7—Ti2—S3 | 93.61 (8) | H34B—C34—H34C | 109.5 |
O4—Ti2—S3 | 157.96 (7) | C33—C35—H35A | 109.5 |
O6—Ti2—S3 | 83.29 (7) | C33—C35—H35B | 109.5 |
O5—Ti2—S3 | 73.27 (6) | H35A—C35—H35B | 109.5 |
O7—Ti2—S4 | 157.82 (9) | C33—C35—H35C | 109.4 |
O4—Ti2—S4 | 93.71 (7) | H35A—C35—H35C | 109.5 |
O6—Ti2—S4 | 73.10 (7) | H35B—C35—H35C | 109.5 |
O5—Ti2—S4 | 84.59 (7) | C33—C36—H36A | 109.5 |
S3—Ti2—S4 | 66.19 (3) | C33—C36—H36B | 109.4 |
C6—S1—C12 | 101.63 (14) | H36A—C36—H36B | 109.5 |
C6—S1—Ti1 | 90.57 (10) | C33—C36—H36C | 109.6 |
C12—S1—Ti1 | 89.04 (10) | H36A—C36—H36C | 109.5 |
C18—S2—C12 | 101.59 (14) | H36B—C36—H36C | 109.5 |
C18—S2—Ti1 | 93.19 (10) | C30—C37—H37A | 109.4 |
C12—S2—Ti1 | 88.21 (10) | C30—C37—H37B | 109.4 |
C32—S3—C38 | 100.05 (14) | H37A—C37—H37B | 109.5 |
C32—S3—Ti2 | 93.06 (10) | C30—C37—H37C | 109.6 |
C38—S3—Ti2 | 89.94 (11) | H37A—C37—H37C | 109.5 |
C44—S4—C38 | 99.69 (15) | H37B—C37—H37C | 109.5 |
C44—S4—Ti2 | 93.37 (10) | S4—C38—S3 | 113.10 (17) |
C38—S4—Ti2 | 88.99 (10) | S4—C38—H38A | 109.0 |
C1—O1—Ti1 | 126.04 (17) | S3—C38—H38A | 109.0 |
C13—O2—Ti1 | 136.15 (18) | S4—C38—H38B | 109.0 |
C24—O3—Ti1 | 156.2 (2) | S3—C38—H38B | 109.0 |
Ti1—O4—Ti2 | 162.05 (13) | H38A—C38—H38B | 107.8 |
C27—O5—Ti2 | 131.93 (18) | O6—C39—C44 | 119.6 (3) |
C39—O6—Ti2 | 136.62 (18) | O6—C39—C40 | 120.8 (3) |
C50A—O7—Ti2 | 162.8 (4) | C44—C39—C40 | 119.6 (3) |
C50B—O7—Ti2 | 159.7 (3) | C41—C40—C39 | 116.6 (3) |
O1—C1—C2 | 122.2 (3) | C41—C40—C45 | 122.3 (3) |
O1—C1—C6 | 118.2 (3) | C39—C40—C45 | 121.1 (3) |
C2—C1—C6 | 119.6 (3) | C40—C41—C42 | 124.2 (3) |
C3—C2—C1 | 116.5 (3) | C40—C41—H41 | 117.9 |
C3—C2—C7 | 121.9 (3) | C42—C41—H41 | 117.9 |
C1—C2—C7 | 121.6 (3) | C43—C42—C41 | 118.1 (3) |
C4—C3—C2 | 124.7 (3) | C43—C42—C49 | 121.5 (3) |
C4—C3—H3 | 117.7 | C41—C42—C49 | 120.3 (3) |
C2—C3—H3 | 117.7 | C42—C43—C44 | 119.7 (3) |
C5—C4—C3 | 117.6 (3) | C42—C43—H43 | 120.1 |
C5—C4—C11 | 121.1 (3) | C44—C43—H43 | 120.1 |
C3—C4—C11 | 121.3 (3) | C39—C44—C43 | 121.7 (3) |
C4—C5—C6 | 120.1 (3) | C39—C44—S4 | 117.2 (2) |
C4—C5—H5 | 120.0 | C43—C44—S4 | 121.0 (2) |
C6—C5—H5 | 120.0 | C40—C45—C48 | 112.4 (3) |
C5—C6—C1 | 121.6 (3) | C40—C45—C47 | 109.0 (3) |
C5—C6—S1 | 121.1 (2) | C48—C45—C47 | 107.9 (3) |
C1—C6—S1 | 117.2 (2) | C40—C45—C46 | 110.9 (3) |
C8—C7—C10 | 108.7 (3) | C48—C45—C46 | 107.8 (3) |
C8—C7—C9 | 109.7 (3) | C47—C45—C46 | 108.7 (3) |
C10—C7—C9 | 107.3 (3) | C45—C46—H46A | 109.5 |
C8—C7—C2 | 109.5 (3) | C45—C46—H46B | 109.5 |
C10—C7—C2 | 111.8 (3) | H46A—C46—H46B | 109.5 |
C9—C7—C2 | 109.7 (3) | C45—C46—H46C | 109.4 |
C7—C8—H8A | 109.5 | H46A—C46—H46C | 109.5 |
C7—C8—H8B | 109.4 | H46B—C46—H46C | 109.5 |
H8A—C8—H8B | 109.5 | C45—C47—H47A | 109.5 |
C7—C8—H8C | 109.5 | C45—C47—H47B | 109.5 |
H8A—C8—H8C | 109.5 | H47A—C47—H47B | 109.5 |
H8B—C8—H8C | 109.5 | C45—C47—H47C | 109.4 |
C7—C9—H9A | 109.5 | H47A—C47—H47C | 109.5 |
C7—C9—H9B | 109.4 | H47B—C47—H47C | 109.5 |
H9A—C9—H9B | 109.5 | C45—C48—H48A | 109.5 |
C7—C9—H9C | 109.5 | C45—C48—H48B | 109.4 |
H9A—C9—H9C | 109.5 | H48A—C48—H48B | 109.5 |
H9B—C9—H9C | 109.5 | C45—C48—H48C | 109.5 |
C7—C10—H10A | 109.6 | H48A—C48—H48C | 109.5 |
C7—C10—H10B | 109.4 | H48B—C48—H48C | 109.5 |
H10A—C10—H10B | 109.5 | C42—C49—H49A | 109.5 |
C7—C10—H10C | 109.4 | C42—C49—H49B | 109.4 |
H10A—C10—H10C | 109.5 | H49A—C49—H49B | 109.5 |
H10B—C10—H10C | 109.5 | C42—C49—H49C | 109.5 |
C4—C11—H11A | 109.5 | H49A—C49—H49C | 109.5 |
C4—C11—H11B | 109.3 | H49B—C49—H49C | 109.5 |
H11A—C11—H11B | 109.5 | O7—C50A—C51A | 108.8 (8) |
C4—C11—H11C | 109.6 | O7—C50A—C52A | 105.5 (7) |
H11A—C11—H11C | 109.5 | C51A—C50A—C52A | 100.2 (8) |
H11B—C11—H11C | 109.5 | O7—C50A—H50A | 113.7 |
S2—C12—S1 | 113.34 (16) | C51A—C50A—H50A | 113.7 |
S2—C12—H12A | 108.9 | C52A—C50A—H50A | 113.7 |
S1—C12—H12A | 108.9 | O7—C50A—H52F | 118.2 |
S2—C12—H12B | 108.9 | C51A—C50A—H52F | 132.8 |
S1—C12—H12B | 108.9 | C52A—C50A—H52F | 71.6 |
H12A—C12—H12B | 107.7 | C50A—C51A—H51A | 100.9 |
O2—C13—C18 | 119.7 (3) | C50A—C51A—H51B | 109.1 |
O2—C13—C14 | 120.7 (3) | H51A—C51A—H51B | 109.5 |
C18—C13—C14 | 119.6 (3) | C50A—C51A—H51C | 118.0 |
C15—C14—C13 | 116.6 (3) | H51A—C51A—H51C | 109.5 |
C15—C14—C19 | 122.9 (3) | H51B—C51A—H51C | 109.5 |
C13—C14—C19 | 120.5 (3) | C50A—C51A—H51D | 121.3 |
C14—C15—C16 | 124.1 (3) | H51B—C51A—H51D | 122.4 |
C14—C15—H15 | 118.0 | H51C—C51A—H51D | 70.8 |
C16—C15—H15 | 118.0 | C50A—C51A—H51E | 68.9 |
C17—C16—C15 | 118.4 (3) | H51A—C51A—H51E | 45.1 |
C17—C16—C23 | 121.3 (3) | H51B—C51A—H51E | 90.5 |
C15—C16—C23 | 120.4 (3) | H51C—C51A—H51E | 153.2 |
C16—C17—C18 | 119.7 (3) | H51D—C51A—H51E | 83.5 |
C16—C17—H17 | 120.1 | C50A—C51A—H51F | 112.1 |
C18—C17—H17 | 120.1 | H51A—C51A—H51F | 103.8 |
C17—C18—C13 | 121.6 (3) | H51C—C51A—H51F | 111.2 |
C17—C18—S2 | 121.1 (2) | H51D—C51A—H51F | 117.2 |
C13—C18—S2 | 117.2 (2) | H51E—C51A—H51F | 87.0 |
C20—C19—C14 | 113.0 (3) | C50A—C52A—H52A | 109.8 |
C20—C19—C22 | 107.6 (3) | C50A—C52A—H52B | 109.0 |
C14—C19—C22 | 108.8 (2) | H52A—C52A—H52B | 109.5 |
C20—C19—C21 | 107.2 (3) | C50A—C52A—H52C | 109.6 |
C14—C19—C21 | 110.0 (2) | H52A—C52A—H52C | 109.5 |
C22—C19—C21 | 110.2 (3) | H52B—C52A—H52C | 109.5 |
C19—C20—H20A | 109.7 | C50A—C52A—H52D | 98.2 |
C19—C20—H20B | 109.4 | H52A—C52A—H52D | 104.8 |
H20A—C20—H20B | 109.5 | H52B—C52A—H52D | 124.6 |
C19—C20—H20C | 109.3 | C50A—C52A—H52E | 99.1 |
H20A—C20—H20C | 109.5 | H52A—C52A—H52E | 141.5 |
H20B—C20—H20C | 109.5 | H52C—C52A—H52E | 82.9 |
C19—C21—H21A | 109.5 | H52D—C52A—H52E | 95.4 |
C19—C21—H21B | 109.4 | O7—C50B—C51B | 104.6 (5) |
H21A—C21—H21B | 109.5 | O7—C50B—C52B | 100.2 (6) |
C19—C21—H21C | 109.5 | C51B—C50B—C52B | 107.7 (6) |
H21A—C21—H21C | 109.5 | O7—C50B—H52A | 112.2 |
H21B—C21—H21C | 109.5 | C51B—C50B—H52A | 143.2 |
C19—C22—H22A | 109.4 | C52B—C50B—H52A | 68.2 |
C19—C22—H22B | 109.4 | O7—C50B—H50B | 114.3 |
H22A—C22—H22B | 109.5 | C51B—C50B—H50B | 114.3 |
C19—C22—H22C | 109.6 | C52B—C50B—H50B | 114.3 |
H22A—C22—H22C | 109.5 | H52A—C50B—H50B | 47.8 |
H22B—C22—H22C | 109.5 | C50B—C51B—H51A | 131.0 |
C16—C23—H23A | 109.5 | C50B—C51B—H51B | 101.7 |
C16—C23—H23B | 109.5 | H51A—C51B—H51B | 123.7 |
H23A—C23—H23B | 109.5 | C50B—C51B—H51C | 68.9 |
C16—C23—H23C | 109.5 | H51A—C51B—H51C | 98.1 |
H23A—C23—H23C | 109.5 | H51B—C51B—H51C | 82.1 |
H23B—C23—H23C | 109.5 | C50B—C51B—H51D | 107.6 |
O3—C24—C25 | 112.5 (3) | H51B—C51B—H51D | 112.6 |
O3—C24—C26 | 106.4 (4) | H51C—C51B—H51D | 56.4 |
C25—C24—C26 | 114.9 (4) | C50B—C51B—H51E | 115.1 |
O3—C24—H24 | 107.6 | H51A—C51B—H51E | 68.1 |
C25—C24—H24 | 107.6 | H51B—C51B—H51E | 110.2 |
C26—C24—H24 | 107.6 | H51C—C51B—H51E | 165.0 |
C24—C25—H25A | 109.3 | H51D—C51B—H51E | 109.5 |
C24—C25—H25B | 109.8 | C50B—C51B—H51F | 105.6 |
H25A—C25—H25B | 109.5 | H51A—C51B—H51F | 119.6 |
C24—C25—H25C | 109.4 | H51C—C51B—H51F | 82.1 |
H25A—C25—H25C | 109.5 | H51D—C51B—H51F | 109.5 |
H25B—C25—H25C | 109.5 | H51E—C51B—H51F | 109.5 |
C24—C26—H26A | 109.6 | C50B—C52B—H52B | 85.4 |
C24—C26—H26B | 109.3 | C50B—C52B—H52C | 118.2 |
H26A—C26—H26B | 109.5 | H52B—C52B—H52C | 92.0 |
C24—C26—H26C | 109.5 | C50B—C52B—H52D | 110.5 |
H26A—C26—H26C | 109.5 | H52B—C52B—H52D | 109.1 |
H26B—C26—H26C | 109.5 | C50B—C52B—H52E | 109.5 |
O5—C27—C32 | 118.8 (3) | H52C—C52B—H52E | 90.6 |
O5—C27—C28 | 122.3 (3) | H52D—C52B—H52E | 109.5 |
C32—C27—C28 | 118.9 (3) | C50B—C52B—H52F | 108.5 |
C29—C28—C27 | 116.1 (3) | H52B—C52B—H52F | 130.5 |
C29—C28—C33 | 122.6 (3) | H52C—C52B—H52F | 118.8 |
C27—C28—C33 | 121.3 (3) | H52D—C52B—H52F | 109.5 |
C30—C29—C28 | 125.1 (3) | H52E—C52B—H52F | 109.5 |
C30—C29—H29 | 117.4 | ||
O3—Ti1—S1—C6 | −74.63 (12) | C1—C2—C7—C8 | −62.7 (4) |
O4—Ti1—S1—C6 | 90.5 (2) | C3—C2—C7—C10 | −1.9 (4) |
O2—Ti1—S1—C6 | −172.69 (12) | C1—C2—C7—C10 | 176.8 (3) |
O1—Ti1—S1—C6 | 24.82 (12) | C3—C2—C7—C9 | −120.9 (3) |
S2—Ti1—S1—C6 | 112.24 (10) | C1—C2—C7—C9 | 57.8 (4) |
O3—Ti1—S1—C12 | −176.24 (13) | C18—S2—C12—S1 | −76.63 (19) |
O4—Ti1—S1—C12 | −11.1 (2) | Ti1—S2—C12—S1 | 16.26 (15) |
O2—Ti1—S1—C12 | 85.69 (12) | C6—S1—C12—S2 | −106.85 (18) |
O1—Ti1—S1—C12 | −76.80 (12) | Ti1—S1—C12—S2 | −16.46 (15) |
S2—Ti1—S1—C12 | 10.62 (10) | Ti1—O2—C13—C18 | 7.6 (4) |
O3—Ti1—S2—C18 | 73.8 (2) | Ti1—O2—C13—C14 | −172.6 (2) |
O4—Ti1—S2—C18 | −96.24 (12) | O2—C13—C14—C15 | −179.3 (3) |
O2—Ti1—S2—C18 | 1.54 (11) | C18—C13—C14—C15 | 0.5 (4) |
O1—Ti1—S2—C18 | 166.39 (11) | O2—C13—C14—C19 | 0.2 (4) |
S1—Ti1—S2—C18 | 90.81 (10) | C18—C13—C14—C19 | 180.0 (3) |
O3—Ti1—S2—C12 | −27.7 (2) | C13—C14—C15—C16 | −0.1 (5) |
O4—Ti1—S2—C12 | 162.25 (12) | C19—C14—C15—C16 | −179.6 (3) |
O2—Ti1—S2—C12 | −99.96 (12) | C14—C15—C16—C17 | −0.1 (5) |
O1—Ti1—S2—C12 | 64.88 (12) | C14—C15—C16—C23 | 179.6 (3) |
S1—Ti1—S2—C12 | −10.70 (10) | C15—C16—C17—C18 | 0.0 (5) |
O7—Ti2—S3—C32 | −81.33 (12) | C23—C16—C17—C18 | −179.7 (3) |
O4—Ti2—S3—C32 | 82.5 (2) | C16—C17—C18—C13 | 0.3 (5) |
O6—Ti2—S3—C32 | −177.41 (11) | C16—C17—C18—S2 | −176.2 (2) |
O5—Ti2—S3—C32 | 16.71 (11) | O2—C13—C18—C17 | 179.2 (3) |
S4—Ti2—S3—C32 | 108.14 (10) | C14—C13—C18—C17 | −0.6 (4) |
O7—Ti2—S3—C38 | 178.61 (13) | O2—C13—C18—S2 | −4.1 (4) |
O4—Ti2—S3—C38 | −17.6 (2) | C14—C13—C18—S2 | 176.1 (2) |
O6—Ti2—S3—C38 | 82.53 (12) | C12—S2—C18—C17 | −93.6 (3) |
O5—Ti2—S3—C38 | −83.35 (12) | Ti1—S2—C18—C17 | 177.5 (2) |
S4—Ti2—S3—C38 | 8.08 (10) | C12—S2—C18—C13 | 89.7 (2) |
O7—Ti2—S4—C44 | 65.7 (2) | Ti1—S2—C18—C13 | 0.8 (2) |
O4—Ti2—S4—C44 | −97.91 (12) | C15—C14—C19—C20 | −2.9 (4) |
O6—Ti2—S4—C44 | 1.43 (11) | C13—C14—C19—C20 | 177.6 (3) |
O5—Ti2—S4—C44 | 165.55 (11) | C15—C14—C19—C22 | 116.6 (3) |
S3—Ti2—S4—C44 | 91.47 (10) | C13—C14—C19—C22 | −62.9 (3) |
O7—Ti2—S4—C38 | −34.0 (2) | C15—C14—C19—C21 | −122.7 (3) |
O4—Ti2—S4—C38 | 162.45 (13) | C13—C14—C19—C21 | 57.8 (4) |
O6—Ti2—S4—C38 | −98.21 (13) | Ti1—O3—C24—C25 | 63.2 (7) |
O5—Ti2—S4—C38 | 65.90 (12) | Ti1—O3—C24—C26 | −63.5 (7) |
S3—Ti2—S4—C38 | −8.18 (11) | Ti2—O5—C27—C32 | 26.1 (4) |
O3—Ti1—O1—C1 | 49.2 (2) | Ti2—O5—C27—C28 | −154.2 (2) |
O4—Ti1—O1—C1 | 159.1 (2) | O5—C27—C28—C29 | −178.7 (3) |
O2—Ti1—O1—C1 | −75.9 (3) | C32—C27—C28—C29 | 1.0 (4) |
S1—Ti1—O1—C1 | −38.6 (2) | O5—C27—C28—C33 | 3.6 (4) |
S2—Ti1—O1—C1 | −106.4 (2) | C32—C27—C28—C33 | −176.7 (3) |
O3—Ti1—O2—C13 | −162.2 (3) | C27—C28—C29—C30 | −0.8 (4) |
O4—Ti1—O2—C13 | 88.0 (3) | C33—C28—C29—C30 | 176.9 (3) |
O1—Ti1—O2—C13 | −36.8 (4) | C28—C29—C30—C31 | −0.5 (5) |
S1—Ti1—O2—C13 | −72.6 (3) | C28—C29—C30—C37 | 180.0 (3) |
S2—Ti1—O2—C13 | −5.2 (2) | C29—C30—C31—C32 | 1.7 (4) |
O4—Ti1—O3—C24 | 36.3 (6) | C37—C30—C31—C32 | −178.8 (3) |
O2—Ti1—O3—C24 | −66.0 (6) | C30—C31—C32—C27 | −1.5 (5) |
O1—Ti1—O3—C24 | 138.0 (6) | C30—C31—C32—S3 | 178.7 (2) |
S1—Ti1—O3—C24 | −148.8 (6) | O5—C27—C32—C31 | 179.8 (3) |
S2—Ti1—O3—C24 | −133.2 (5) | C28—C27—C32—C31 | 0.1 (4) |
O3—Ti1—O4—Ti2 | −164.4 (4) | O5—C27—C32—S3 | −0.4 (4) |
O2—Ti1—O4—Ti2 | −62.8 (4) | C28—C27—C32—S3 | 179.9 (2) |
O1—Ti1—O4—Ti2 | 93.1 (4) | C38—S3—C32—C31 | −102.4 (3) |
S1—Ti1—O4—Ti2 | 31.2 (6) | Ti2—S3—C32—C31 | 167.1 (2) |
S2—Ti1—O4—Ti2 | 11.3 (4) | C38—S3—C32—C27 | 77.7 (3) |
O7—Ti2—O4—Ti1 | −132.2 (4) | Ti2—S3—C32—C27 | −12.8 (2) |
O6—Ti2—O4—Ti1 | −32.1 (4) | C29—C28—C33—C35 | −115.6 (3) |
O5—Ti2—O4—Ti1 | 126.4 (4) | C27—C28—C33—C35 | 62.1 (3) |
S3—Ti2—O4—Ti1 | 64.8 (5) | C29—C28—C33—C34 | 3.3 (4) |
S4—Ti2—O4—Ti1 | 41.4 (4) | C27—C28—C33—C34 | −179.1 (3) |
O7—Ti2—O5—C27 | 64.8 (3) | C29—C28—C33—C36 | 123.4 (3) |
O4—Ti2—O5—C27 | 173.8 (2) | C27—C28—C33—C36 | −58.9 (4) |
O6—Ti2—O5—C27 | −58.3 (3) | C44—S4—C38—S3 | −80.9 (2) |
S3—Ti2—O5—C27 | −26.4 (2) | Ti2—S4—C38—S3 | 12.31 (16) |
S4—Ti2—O5—C27 | −93.1 (2) | C32—S3—C38—S4 | −105.60 (19) |
O7—Ti2—O6—C39 | −162.3 (3) | Ti2—S3—C38—S4 | −12.51 (17) |
O4—Ti2—O6—C39 | 88.6 (3) | Ti2—O6—C39—C44 | 2.1 (4) |
O5—Ti2—O6—C39 | −38.7 (4) | Ti2—O6—C39—C40 | −176.8 (2) |
S3—Ti2—O6—C39 | −69.4 (3) | O6—C39—C40—C41 | 178.0 (3) |
S4—Ti2—O6—C39 | −2.3 (2) | C44—C39—C40—C41 | −0.9 (4) |
O4—Ti2—O7—C50A | −178.4 (12) | O6—C39—C40—C45 | 0.4 (4) |
O6—Ti2—O7—C50A | 79.0 (12) | C44—C39—C40—C45 | −178.6 (3) |
O5—Ti2—O7—C50A | −78.3 (12) | C39—C40—C41—C42 | 0.0 (5) |
S3—Ti2—O7—C50A | −4.7 (12) | C45—C40—C41—C42 | 177.6 (3) |
S4—Ti2—O7—C50A | 18.8 (13) | C40—C41—C42—C43 | 1.2 (5) |
O4—Ti2—O7—C50B | −45.3 (7) | C40—C41—C42—C49 | −179.3 (3) |
O6—Ti2—O7—C50B | −148.0 (7) | C41—C42—C43—C44 | −1.4 (5) |
O5—Ti2—O7—C50B | 54.8 (7) | C49—C42—C43—C44 | 179.1 (3) |
S3—Ti2—O7—C50B | 128.4 (7) | O6—C39—C44—C43 | −178.3 (3) |
S4—Ti2—O7—C50B | 151.9 (6) | C40—C39—C44—C43 | 0.7 (4) |
Ti1—O1—C1—C2 | −140.1 (2) | O6—C39—C44—S4 | 0.2 (4) |
Ti1—O1—C1—C6 | 39.9 (4) | C40—C39—C44—S4 | 179.1 (2) |
O1—C1—C2—C3 | 179.2 (3) | C42—C43—C44—C39 | 0.5 (5) |
C6—C1—C2—C3 | −0.7 (4) | C42—C43—C44—S4 | −177.8 (2) |
O1—C1—C2—C7 | 0.5 (4) | C38—S4—C44—C39 | 88.4 (3) |
C6—C1—C2—C7 | −179.5 (3) | Ti2—S4—C44—C39 | −1.2 (2) |
C1—C2—C3—C4 | −0.4 (5) | C38—S4—C44—C43 | −93.2 (3) |
C7—C2—C3—C4 | 178.3 (3) | Ti2—S4—C44—C43 | 177.3 (2) |
C2—C3—C4—C5 | 1.7 (5) | C41—C40—C45—C48 | 4.7 (4) |
C2—C3—C4—C11 | −176.8 (3) | C39—C40—C45—C48 | −177.8 (3) |
C3—C4—C5—C6 | −1.8 (4) | C41—C40—C45—C47 | −114.8 (3) |
C11—C4—C5—C6 | 176.7 (3) | C39—C40—C45—C47 | 62.7 (4) |
C4—C5—C6—C1 | 0.7 (5) | C41—C40—C45—C46 | 125.5 (3) |
C4—C5—C6—S1 | −174.9 (2) | C39—C40—C45—C46 | −56.9 (4) |
O1—C1—C6—C5 | −179.4 (3) | C50B—O7—C50A—C51A | −55.0 (9) |
C2—C1—C6—C5 | 0.6 (4) | Ti2—O7—C50A—C51A | 98.2 (15) |
O1—C1—C6—S1 | −3.6 (4) | C50B—O7—C50A—C52A | 51.8 (6) |
C2—C1—C6—S1 | 176.4 (2) | Ti2—O7—C50A—C52A | −155.0 (9) |
C12—S1—C6—C5 | −112.4 (3) | C50A—O7—C50B—C51B | 61.0 (8) |
Ti1—S1—C6—C5 | 158.5 (2) | Ti2—O7—C50B—C51B | −96.5 (9) |
C12—S1—C6—C1 | 71.8 (3) | C50A—O7—C50B—C52B | −50.5 (7) |
Ti1—S1—C6—C1 | −17.3 (2) | Ti2—O7—C50B—C52B | 152.0 (7) |
C3—C2—C7—C8 | 118.6 (3) |
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