Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806002492/lh6581sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536806002492/lh6581Isup2.hkl |
CCDC reference: 298497
Data collection: COLLECT (Nonius, 2001); cell refinement: DENZO-SMN (Otwinowski & Minor, 1997); data reduction: DENZO-SMN; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL/PC (Sheldrick, 2001); software used to prepare material for publication: SHELXTL/PC.
[Ti6(C2H3O2)6(C3H7O)6O6] | Z = 2 |
Mr = 1092.18 | F(000) = 1128 |
Triclinic, P1 | Dx = 1.480 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 10.2466 (14) Å | Cell parameters from 20933 reflections |
b = 12.2908 (12) Å | θ = 1.7–25.0° |
c = 20.225 (3) Å | µ = 1.01 mm−1 |
α = 89.861 (8)° | T = 298 K |
β = 83.883 (6)° | Plate, colourless |
γ = 75.461 (7)° | 0.20 × 0.17 × 0.05 mm |
V = 2450.7 (5) Å3 |
Bruker–Nonius KappaCCD diffractometer | 7905 independent reflections |
Radiation source: fine-focus sealed tube | 2994 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.091 |
φ scans, and ω scans with κ offsets | θmax = 25.0°, θmin = 2.6° |
Absorption correction: multi-scan (SORTAV; Blessing, 1995) | h = −12→12 |
Tmin = 0.811, Tmax = 0.949 | k = −14→14 |
13625 measured reflections | l = −19→24 |
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)] = 0.076 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.195 | H-atom parameters constrained |
S = 0.96 | w = 1/[σ2(Fo2) + (0.0734P)2] where P = (Fo2 + 2Fc2)/3 |
7905 reflections | (Δ/σ)max < 0.001 |
560 parameters | Δρmax = 0.35 e Å−3 |
483 restraints | Δρmin = −0.40 e Å−3 |
Experimental. FTIR Spectrum (KBr ν): 2972 (m), 2933 (m), 2875 (m), 1604 (s), 1543 (s), 1458 (s), 1375 (w), 1361 (w), 1348 (w), 1327 (w), 1165 (m), 1132 (s), 1016 (s), 858 (m),727 (s), 658 (s), 627 (s), 611 (s).cm-1. 1H NMR (deuterochloroform, 400 MHz): δ 5.07 (sept., JH—H = 6.2 Hz), δ 1.97 (s), δ 1.35 (d, JH—H = 6.2 Hz). 13C NMR (deuterochloroform, 101 MHz): δ 177.9, δ 82.0, δ 24.9, δ 23.1. |
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 | 0.57920 (15) | 0.41884 (11) | 0.09764 (8) | 0.0586 (5) | |
Ti2 | 0.69757 (15) | 0.37779 (11) | −0.05126 (8) | 0.0596 (5) | |
Ti3 | 0.36725 (16) | 0.36982 (11) | 0.00942 (8) | 0.0592 (5) | |
O1 | 0.5573 (5) | 0.3382 (4) | 0.0058 (2) | 0.0534 (13) | |
O2 | 0.6734 (5) | 0.4899 (4) | 0.0336 (3) | 0.0539 (13) | |
O3 | 0.3948 (5) | 0.4859 (4) | 0.0845 (2) | 0.0504 (13) | |
O11 | 0.5840 (5) | 0.4947 (4) | 0.1695 (3) | 0.0653 (15) | |
C12 | 0.5324 (11) | 0.5625 (8) | 0.2269 (5) | 0.084 (3) | |
H12A | 0.5171 | 0.6411 | 0.2137 | 0.101* | |
C13 | 0.6371 (12) | 0.5423 (9) | 0.2752 (5) | 0.128 (4) | |
H13A | 0.7196 | 0.5561 | 0.2541 | 0.192* | |
H13B | 0.6541 | 0.4658 | 0.2892 | 0.192* | |
H13C | 0.6045 | 0.5921 | 0.3132 | 0.192* | |
C14 | 0.4018 (11) | 0.5461 (9) | 0.2569 (5) | 0.126 (4) | |
H14A | 0.3376 | 0.5612 | 0.2247 | 0.189* | |
H14B | 0.3687 | 0.5964 | 0.2946 | 0.189* | |
H14C | 0.4139 | 0.4699 | 0.2709 | 0.189* | |
O15 | 0.5137 (6) | 0.2929 (4) | 0.1481 (3) | 0.0650 (15) | |
C16 | 0.4372 (10) | 0.2323 (7) | 0.1313 (5) | 0.067 (3) | |
C17 | 0.4267 (10) | 0.1364 (7) | 0.1733 (5) | 0.101 (4) | |
H17A | 0.3652 | 0.0987 | 0.1564 | 0.151* | |
H17B | 0.3936 | 0.1628 | 0.2181 | 0.151* | |
H17C | 0.5145 | 0.0849 | 0.1728 | 0.151* | |
O18 | 0.3733 (6) | 0.2501 (4) | 0.0811 (3) | 0.0705 (17) | |
O21 | 0.7067 (5) | 0.2809 (4) | −0.1164 (3) | 0.0657 (16) | |
C22 | 0.7231 (14) | 0.1737 (8) | −0.1439 (6) | 0.118 (4) | |
H22A | 0.6359 | 0.1753 | −0.1601 | 0.142* | |
C23 | 0.7377 (15) | 0.0891 (8) | −0.0916 (7) | 0.168 (6) | |
H23A | 0.7438 | 0.0165 | −0.1110 | 0.252* | |
H23B | 0.6603 | 0.1086 | −0.0587 | 0.252* | |
H23C | 0.8185 | 0.0870 | −0.0711 | 0.252* | |
C24 | 0.8159 (19) | 0.1476 (11) | −0.1987 (8) | 0.242 (10) | |
H24A | 0.7952 | 0.2052 | −0.2309 | 0.363* | |
H24B | 0.8129 | 0.0769 | −0.2177 | 0.363* | |
H24C | 0.9050 | 0.1424 | −0.1862 | 0.363* | |
O25 | 0.8367 (5) | 0.2657 (4) | −0.0027 (3) | 0.0680 (16) | |
C26 | 0.8428 (10) | 0.2498 (7) | 0.0594 (6) | 0.069 (3) | |
C27 | 0.9642 (10) | 0.1607 (8) | 0.0784 (5) | 0.122 (4) | |
H27A | 0.9574 | 0.1542 | 0.1259 | 0.182* | |
H27B | 1.0462 | 0.1819 | 0.0632 | 0.182* | |
H27C | 0.9658 | 0.0898 | 0.0581 | 0.182* | |
O28 | 0.7553 (6) | 0.2998 (4) | 0.1044 (3) | 0.0669 (16) | |
O31 | 0.3428 (6) | 0.2787 (4) | −0.0523 (3) | 0.0689 (16) | |
C32 | 0.2819 (16) | 0.2026 (9) | −0.0791 (6) | 0.140 (5) | |
H32A | 0.1882 | 0.2350 | −0.0598 | 0.168* | |
C33 | 0.3077 (15) | 0.0984 (8) | −0.0441 (6) | 0.166 (6) | |
H33A | 0.2604 | 0.0490 | −0.0621 | 0.249* | |
H33B | 0.2766 | 0.1131 | 0.0022 | 0.249* | |
H33C | 0.4033 | 0.0636 | −0.0492 | 0.249* | |
C34 | 0.2619 (14) | 0.2092 (10) | −0.1447 (6) | 0.160 (6) | |
H34A | 0.2343 | 0.2867 | −0.1564 | 0.240* | |
H34B | 0.1925 | 0.1724 | −0.1526 | 0.240* | |
H34C | 0.3448 | 0.1731 | −0.1713 | 0.240* | |
O35 | 0.1690 (6) | 0.4030 (5) | 0.0496 (3) | 0.0698 (16) | |
C36 | 0.0938 (10) | 0.4905 (9) | 0.0808 (5) | 0.066 (2) | |
C37 | −0.0405 (9) | 0.4813 (7) | 0.1144 (5) | 0.094 (3) | |
H37A | −0.0508 | 0.4069 | 0.1070 | 0.142* | |
H37B | −0.1120 | 0.5352 | 0.0963 | 0.142* | |
H37C | −0.0446 | 0.4959 | 0.1613 | 0.142* | |
O38 | 0.1266 (5) | 0.5817 (5) | 0.0858 (3) | 0.0708 (18) | |
Ti4 | 0.85058 (16) | 0.97592 (12) | 0.42432 (8) | 0.0640 (5) | |
Ti5 | 1.14293 (16) | 0.83775 (12) | 0.44706 (8) | 0.0619 (5) | |
Ti6 | 0.87059 (16) | 0.90903 (12) | 0.57209 (8) | 0.0638 (5) | |
O4 | 0.9639 (5) | 0.8543 (4) | 0.4889 (3) | 0.0597 (13) | |
O5 | 1.0323 (5) | 0.9886 (4) | 0.4041 (3) | 0.0580 (14) | |
O6 | 0.8024 (5) | 1.0489 (4) | 0.5083 (3) | 0.0567 (14) | |
O41 | 0.7680 (5) | 1.0798 (4) | 0.3729 (3) | 0.0697 (16) | |
C42 | 0.7333 (13) | 1.1448 (10) | 0.3173 (6) | 0.113 (4) | |
H42A | 0.7902 | 1.1982 | 0.3157 | 0.136* | |
C43 | 0.7820 (14) | 1.0741 (10) | 0.2553 (6) | 0.158 (6) | |
H43A | 0.8775 | 1.0405 | 0.2542 | 0.237* | |
H43B | 0.7653 | 1.1203 | 0.2172 | 0.237* | |
H43C | 0.7345 | 1.0161 | 0.2546 | 0.237* | |
C44 | 0.5998 (15) | 1.2127 (11) | 0.3254 (6) | 0.192 (7) | |
H44A | 0.5867 | 1.2592 | 0.3648 | 0.288* | |
H44B | 0.5373 | 1.1659 | 0.3294 | 0.288* | |
H44C | 0.5842 | 1.2593 | 0.2874 | 0.288* | |
O45 | 0.8901 (6) | 0.8487 (5) | 0.3536 (3) | 0.0740 (17) | |
C46 | 0.9880 (12) | 0.7631 (8) | 0.3436 (5) | 0.077 (3) | |
C47 | 0.9774 (10) | 0.6747 (7) | 0.2949 (5) | 0.107 (4) | |
H47A | 0.8923 | 0.6976 | 0.2766 | 0.160* | |
H47B | 0.9829 | 0.6049 | 0.3171 | 0.160* | |
H47C | 1.0504 | 0.6652 | 0.2597 | 0.160* | |
O48 | 1.0950 (6) | 0.7473 (4) | 0.3717 (3) | 0.0699 (16) | |
O51 | 1.2222 (5) | 0.7169 (4) | 0.4875 (3) | 0.0713 (17) | |
C52 | 1.2379 (19) | 0.6085 (10) | 0.5057 (7) | 0.155 (6) | |
H52A | 1.2735 | 0.6105 | 0.5486 | 0.186* | 0.447 (19) |
H52B | 1.1404 | 0.6156 | 0.5159 | 0.186* | 0.553 (19) |
C53A | 1.358 (3) | 0.548 (2) | 0.465 (2) | 0.188 (15) | 0.447 (19) |
H53A | 1.3760 | 0.4694 | 0.4751 | 0.282* | 0.447 (19) |
H53B | 1.4334 | 0.5763 | 0.4737 | 0.282* | 0.447 (19) |
H53C | 1.3437 | 0.5570 | 0.4189 | 0.282* | 0.447 (19) |
C54A | 1.122 (3) | 0.571 (3) | 0.525 (2) | 0.26 (2) | 0.447 (19) |
H54A | 1.0615 | 0.6240 | 0.5559 | 0.387* | 0.447 (19) |
H54B | 1.1469 | 0.4991 | 0.5449 | 0.387* | 0.447 (19) |
H54C | 1.0767 | 0.5642 | 0.4861 | 0.387* | 0.447 (19) |
C53B | 1.286 (4) | 0.5732 (18) | 0.5655 (12) | 0.215 (16) | 0.553 (19) |
H53D | 1.2159 | 0.5997 | 0.6013 | 0.322* | 0.553 (19) |
H53E | 1.3626 | 0.6027 | 0.5714 | 0.322* | 0.553 (19) |
H53F | 1.3136 | 0.4925 | 0.5652 | 0.322* | 0.553 (19) |
C54B | 1.240 (5) | 0.5288 (18) | 0.4563 (14) | 0.221 (15) | 0.553 (19) |
H54D | 1.1484 | 0.5248 | 0.4520 | 0.331* | 0.553 (19) |
H54E | 1.2921 | 0.4566 | 0.4681 | 0.331* | 0.553 (19) |
H54F | 1.2792 | 0.5502 | 0.4147 | 0.331* | 0.553 (19) |
O55 | 1.3055 (6) | 0.8311 (4) | 0.3771 (3) | 0.0677 (16) | |
C56 | 1.3478 (11) | 0.9105 (9) | 0.3508 (5) | 0.075 (3) | |
C57 | 1.4807 (10) | 0.8835 (7) | 0.3066 (5) | 0.093 (3) | |
H57A | 1.5177 | 0.8035 | 0.3039 | 0.139* | |
H57B | 1.5432 | 0.9184 | 0.3250 | 0.139* | |
H57C | 1.4658 | 0.9113 | 0.2630 | 0.139* | |
O58 | 1.2876 (6) | 1.0142 (5) | 0.3595 (3) | 0.0750 (18) | |
O61 | 0.9248 (6) | 0.7968 (4) | 0.6258 (3) | 0.0719 (17) | |
C62 | 0.8836 (17) | 0.7341 (12) | 0.6780 (7) | 0.156 (5) | |
H62A | 0.7954 | 0.7872 | 0.6899 | 0.188* | |
C63 | 0.9325 (17) | 0.7454 (18) | 0.7368 (8) | 0.275 (10) | |
H63A | 0.8915 | 0.7053 | 0.7704 | 0.412* | |
H63B | 0.9114 | 0.8235 | 0.7496 | 0.412* | |
H63C | 1.0291 | 0.7152 | 0.7320 | 0.412* | |
C64 | 0.8327 (18) | 0.6487 (12) | 0.6614 (9) | 0.249 (9) | |
H64A | 0.7993 | 0.6167 | 0.7011 | 0.374* | |
H64B | 0.9025 | 0.5922 | 0.6366 | 0.374* | |
H64C | 0.7597 | 0.6759 | 0.6348 | 0.374* | |
O65 | 0.7139 (6) | 0.8451 (5) | 0.5477 (3) | 0.0748 (17) | |
C66 | 0.6578 (9) | 0.8550 (7) | 0.4936 (6) | 0.067 (2) | |
C67 | 0.5409 (9) | 0.8009 (8) | 0.4916 (6) | 0.105 (4) | |
H67A | 0.5061 | 0.8135 | 0.4492 | 0.158* | |
H67B | 0.4705 | 0.8333 | 0.5263 | 0.158* | |
H67C | 0.5720 | 0.7215 | 0.4979 | 0.158* | |
O68 | 0.6875 (6) | 0.9067 (5) | 0.4442 (3) | 0.0738 (17) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ti1 | 0.0623 (11) | 0.0565 (9) | 0.0591 (11) | −0.0156 (8) | −0.0145 (9) | −0.0050 (8) |
Ti2 | 0.0588 (11) | 0.0575 (10) | 0.0622 (12) | −0.0118 (8) | −0.0120 (9) | −0.0077 (9) |
Ti3 | 0.0653 (11) | 0.0559 (10) | 0.0616 (12) | −0.0227 (8) | −0.0119 (9) | −0.0060 (8) |
O1 | 0.056 (3) | 0.047 (3) | 0.057 (3) | −0.011 (2) | −0.009 (3) | −0.006 (2) |
O2 | 0.052 (3) | 0.053 (3) | 0.061 (3) | −0.019 (2) | −0.011 (3) | −0.001 (2) |
O3 | 0.052 (3) | 0.047 (3) | 0.055 (4) | −0.015 (2) | −0.007 (3) | −0.002 (2) |
O11 | 0.070 (4) | 0.071 (3) | 0.056 (3) | −0.019 (3) | −0.010 (3) | −0.017 (3) |
C12 | 0.103 (8) | 0.083 (7) | 0.061 (7) | −0.012 (6) | −0.006 (5) | −0.012 (5) |
C13 | 0.170 (11) | 0.148 (10) | 0.079 (8) | −0.048 (9) | −0.052 (8) | −0.008 (7) |
C14 | 0.106 (8) | 0.156 (10) | 0.091 (9) | −0.008 (8) | 0.034 (6) | −0.020 (8) |
O15 | 0.083 (4) | 0.063 (3) | 0.056 (4) | −0.029 (3) | −0.017 (3) | 0.006 (3) |
C16 | 0.082 (7) | 0.057 (6) | 0.065 (7) | −0.026 (5) | −0.008 (5) | −0.001 (5) |
C17 | 0.140 (10) | 0.090 (7) | 0.094 (8) | −0.066 (7) | −0.025 (7) | 0.030 (6) |
O18 | 0.090 (5) | 0.066 (4) | 0.067 (4) | −0.036 (3) | −0.019 (4) | 0.005 (3) |
O21 | 0.076 (4) | 0.054 (3) | 0.066 (4) | −0.015 (3) | −0.007 (3) | −0.014 (3) |
C22 | 0.165 (11) | 0.072 (6) | 0.100 (9) | −0.002 (8) | −0.004 (8) | −0.025 (5) |
C23 | 0.265 (17) | 0.064 (6) | 0.185 (12) | −0.044 (9) | −0.063 (12) | 0.015 (7) |
C24 | 0.32 (2) | 0.136 (11) | 0.204 (15) | −0.008 (13) | 0.133 (15) | −0.083 (9) |
O25 | 0.065 (4) | 0.065 (4) | 0.067 (4) | −0.002 (3) | −0.012 (3) | −0.007 (3) |
C26 | 0.065 (6) | 0.061 (6) | 0.076 (6) | −0.004 (4) | −0.023 (5) | −0.006 (5) |
C27 | 0.098 (8) | 0.127 (9) | 0.105 (9) | 0.040 (6) | −0.023 (7) | 0.019 (7) |
O28 | 0.064 (4) | 0.066 (4) | 0.068 (4) | −0.009 (3) | −0.013 (3) | 0.000 (3) |
O31 | 0.093 (4) | 0.065 (3) | 0.062 (4) | −0.038 (3) | −0.020 (3) | −0.005 (3) |
C32 | 0.262 (15) | 0.089 (7) | 0.105 (9) | −0.092 (9) | −0.064 (10) | −0.008 (7) |
C33 | 0.307 (19) | 0.089 (7) | 0.138 (11) | −0.106 (10) | −0.048 (12) | 0.004 (7) |
C34 | 0.246 (16) | 0.164 (11) | 0.109 (10) | −0.098 (11) | −0.086 (11) | −0.012 (8) |
O35 | 0.061 (3) | 0.070 (4) | 0.085 (5) | −0.026 (3) | −0.016 (3) | −0.005 (3) |
C36 | 0.060 (6) | 0.088 (6) | 0.057 (7) | −0.025 (5) | −0.021 (5) | 0.008 (5) |
C37 | 0.062 (6) | 0.109 (7) | 0.116 (9) | −0.030 (5) | −0.003 (6) | −0.005 (7) |
O38 | 0.059 (4) | 0.072 (4) | 0.082 (5) | −0.017 (3) | −0.008 (4) | −0.005 (4) |
Ti4 | 0.0650 (12) | 0.0633 (10) | 0.0665 (12) | −0.0156 (8) | −0.0214 (10) | 0.0006 (9) |
Ti5 | 0.0630 (11) | 0.0575 (10) | 0.0656 (12) | −0.0121 (8) | −0.0158 (9) | −0.0023 (9) |
Ti6 | 0.0680 (12) | 0.0604 (10) | 0.0658 (12) | −0.0184 (9) | −0.0146 (10) | 0.0023 (9) |
O4 | 0.066 (3) | 0.051 (3) | 0.066 (3) | −0.020 (2) | −0.015 (3) | −0.002 (2) |
O5 | 0.066 (3) | 0.056 (3) | 0.054 (4) | −0.017 (2) | −0.016 (3) | −0.001 (3) |
O6 | 0.055 (3) | 0.057 (3) | 0.060 (3) | −0.015 (2) | −0.015 (3) | −0.004 (2) |
O41 | 0.080 (4) | 0.069 (3) | 0.065 (4) | −0.018 (3) | −0.031 (3) | 0.009 (3) |
C42 | 0.133 (9) | 0.127 (10) | 0.072 (7) | −0.017 (7) | −0.017 (8) | 0.030 (6) |
C43 | 0.201 (14) | 0.170 (12) | 0.079 (7) | 0.001 (10) | −0.025 (9) | 0.008 (8) |
C44 | 0.211 (14) | 0.174 (12) | 0.132 (12) | 0.083 (10) | −0.070 (10) | 0.015 (10) |
O45 | 0.085 (4) | 0.070 (4) | 0.071 (4) | −0.018 (3) | −0.026 (3) | −0.012 (3) |
C46 | 0.092 (8) | 0.069 (6) | 0.080 (8) | −0.030 (5) | −0.025 (6) | −0.001 (5) |
C47 | 0.128 (10) | 0.079 (6) | 0.115 (10) | −0.015 (6) | −0.043 (7) | −0.035 (6) |
O48 | 0.075 (4) | 0.065 (3) | 0.072 (4) | −0.018 (3) | −0.016 (3) | −0.014 (3) |
O51 | 0.075 (4) | 0.051 (3) | 0.085 (4) | −0.007 (3) | −0.017 (3) | 0.006 (3) |
C52 | 0.253 (17) | 0.061 (6) | 0.138 (12) | −0.010 (8) | −0.042 (12) | 0.013 (6) |
C53A | 0.16 (2) | 0.055 (15) | 0.33 (4) | 0.013 (15) | −0.06 (2) | −0.02 (2) |
C54A | 0.42 (4) | 0.11 (2) | 0.21 (4) | −0.09 (2) | 0.19 (4) | 0.03 (3) |
C53B | 0.44 (5) | 0.071 (15) | 0.14 (2) | −0.04 (2) | −0.12 (3) | 0.039 (12) |
C54B | 0.40 (4) | 0.089 (12) | 0.24 (3) | −0.11 (2) | −0.20 (3) | 0.022 (14) |
O55 | 0.072 (4) | 0.062 (4) | 0.068 (4) | −0.017 (3) | −0.005 (3) | −0.010 (3) |
C56 | 0.081 (7) | 0.089 (6) | 0.055 (7) | −0.021 (5) | −0.008 (5) | −0.006 (6) |
C57 | 0.090 (7) | 0.086 (7) | 0.092 (8) | −0.015 (5) | 0.018 (6) | −0.009 (6) |
O58 | 0.071 (4) | 0.074 (4) | 0.075 (5) | −0.014 (3) | 0.004 (4) | −0.002 (4) |
O61 | 0.086 (4) | 0.065 (4) | 0.069 (4) | −0.021 (3) | −0.020 (4) | 0.014 (3) |
C62 | 0.246 (16) | 0.145 (11) | 0.096 (10) | −0.082 (10) | −0.024 (9) | 0.050 (8) |
C63 | 0.210 (17) | 0.55 (3) | 0.124 (12) | −0.181 (19) | −0.078 (13) | 0.163 (16) |
C64 | 0.29 (2) | 0.159 (14) | 0.35 (2) | −0.148 (13) | −0.042 (18) | 0.107 (15) |
O65 | 0.068 (4) | 0.079 (4) | 0.084 (5) | −0.028 (3) | −0.014 (3) | 0.005 (4) |
C66 | 0.055 (6) | 0.057 (6) | 0.090 (8) | −0.014 (4) | −0.007 (5) | −0.013 (5) |
C67 | 0.082 (8) | 0.108 (8) | 0.149 (11) | −0.055 (6) | −0.043 (7) | 0.028 (7) |
O68 | 0.071 (4) | 0.076 (4) | 0.085 (5) | −0.030 (3) | −0.031 (3) | 0.010 (3) |
Ti1—O11 | 1.740 (6) | Ti4—O4 | 2.175 (5) |
Ti1—O2 | 1.876 (5) | Ti4—Ti6 | 3.112 (2) |
Ti1—O3 | 1.909 (5) | Ti4—Ti5 | 3.131 (2) |
Ti1—O28 | 2.035 (6) | Ti5—O51 | 1.751 (5) |
Ti1—O15 | 2.063 (5) | Ti5—O6ii | 1.891 (5) |
Ti1—O1 | 2.166 (5) | Ti5—O4 | 1.899 (5) |
Ti1—Ti2 | 3.117 (2) | Ti5—O55 | 2.052 (6) |
Ti1—Ti3 | 3.123 (2) | Ti5—O48 | 2.061 (6) |
Ti2—O21 | 1.758 (5) | Ti5—O5 | 2.150 (5) |
Ti2—O3i | 1.867 (5) | Ti5—Ti6ii | 3.106 (2) |
Ti2—O1 | 1.904 (5) | Ti6—O61 | 1.768 (5) |
Ti2—O38i | 2.041 (6) | Ti6—O4 | 1.880 (6) |
Ti2—O25 | 2.050 (5) | Ti6—O5ii | 1.882 (5) |
Ti2—O2 | 2.158 (5) | Ti6—O58ii | 2.048 (6) |
Ti2—Ti3i | 3.105 (2) | Ti6—O65 | 2.060 (6) |
Ti3—O31 | 1.758 (5) | Ti6—O6 | 2.165 (5) |
Ti3—O1 | 1.881 (5) | Ti6—Ti5ii | 3.106 (2) |
Ti3—O2i | 1.901 (5) | O5—Ti6ii | 1.882 (5) |
Ti3—O35 | 2.046 (6) | O6—Ti5ii | 1.891 (5) |
Ti3—O18 | 2.058 (6) | O41—C42 | 1.402 (10) |
Ti3—O3 | 2.173 (5) | C42—C44 | 1.405 (14) |
Ti3—Ti2i | 3.105 (2) | C42—C43 | 1.494 (14) |
O2—Ti3i | 1.901 (5) | C42—H42A | 0.9800 |
O3—Ti2i | 1.867 (5) | C43—H43A | 0.9600 |
O11—C12 | 1.405 (10) | C43—H43B | 0.9600 |
C12—C14 | 1.470 (13) | C43—H43C | 0.9600 |
C12—C13 | 1.501 (12) | C44—H44A | 0.9600 |
C12—H12A | 0.9800 | C44—H44B | 0.9600 |
C13—H13A | 0.9600 | C44—H44C | 0.9600 |
C13—H13B | 0.9600 | O45—C46 | 1.259 (10) |
C13—H13C | 0.9600 | C46—O48 | 1.258 (10) |
C14—H14A | 0.9600 | C46—C47 | 1.500 (12) |
C14—H14B | 0.9600 | C47—H47A | 0.9600 |
C14—H14C | 0.9600 | C47—H47B | 0.9600 |
O15—C16 | 1.279 (9) | C47—H47C | 0.9600 |
C16—O18 | 1.256 (10) | O51—C52 | 1.355 (12) |
C16—C17 | 1.470 (11) | C52—C53B | 1.384 (15) |
C17—H17A | 0.9600 | C52—C54B | 1.398 (16) |
C17—H17B | 0.9600 | C52—C54A | 1.398 (17) |
C17—H17C | 0.9600 | C52—C53A | 1.439 (17) |
O21—C22 | 1.394 (10) | C52—H52A | 0.9800 |
C22—C24 | 1.364 (15) | C52—H52B | 0.9800 |
C22—C23 | 1.475 (14) | C53A—H53A | 0.9600 |
C22—H22A | 0.9800 | C53A—H53B | 0.9600 |
C23—H23A | 0.9600 | C53A—H53C | 0.9600 |
C23—H23B | 0.9600 | C54A—H52B | 0.6428 |
C23—H23C | 0.9600 | C54A—H54A | 0.9600 |
C24—H24A | 0.9600 | C54A—H54B | 0.9600 |
C24—H24B | 0.9600 | C54A—H54C | 0.9600 |
C24—H24C | 0.9600 | C53B—H53D | 0.9600 |
O25—C26 | 1.275 (10) | C53B—H53E | 0.9600 |
C26—O28 | 1.249 (10) | C53B—H53F | 0.9600 |
C26—C27 | 1.520 (11) | C54B—H54D | 0.9600 |
C27—H27A | 0.9600 | C54B—H54E | 0.9600 |
C27—H27B | 0.9600 | C54B—H54F | 0.9600 |
C27—H27C | 0.9600 | O55—C56 | 1.259 (10) |
O31—C32 | 1.388 (11) | C56—O58 | 1.273 (10) |
C32—C34 | 1.362 (13) | C56—C57 | 1.508 (12) |
C32—C33 | 1.442 (13) | C57—H57A | 0.9600 |
C32—H32A | 0.9800 | C57—H57B | 0.9600 |
C33—H33A | 0.9600 | C57—H57C | 0.9600 |
C33—H33B | 0.9600 | O58—Ti6ii | 2.048 (6) |
C33—H33C | 0.9600 | O61—C62 | 1.397 (12) |
C34—H34A | 0.9600 | C62—C64 | 1.343 (17) |
C34—H34B | 0.9600 | C62—C63 | 1.359 (17) |
C34—H34C | 0.9600 | C62—H62A | 0.9800 |
O35—C36 | 1.277 (10) | C63—H63A | 0.9600 |
C36—O38 | 1.256 (10) | C63—H63B | 0.9600 |
C36—C37 | 1.498 (11) | C63—H63C | 0.9600 |
C37—H37A | 0.9600 | C64—H64A | 0.9600 |
C37—H37B | 0.9600 | C64—H64B | 0.9600 |
C37—H37C | 0.9600 | C64—H64C | 0.9600 |
O38—Ti2i | 2.041 (6) | O65—C66 | 1.280 (10) |
Ti4—O41 | 1.751 (5) | C66—O68 | 1.235 (10) |
Ti4—O6 | 1.882 (5) | C66—C67 | 1.513 (11) |
Ti4—O5 | 1.908 (5) | C67—H67A | 0.9600 |
Ti4—O45 | 2.055 (6) | C67—H67B | 0.9600 |
Ti4—O68 | 2.060 (6) | C67—H67C | 0.9600 |
O11—Ti1—O2 | 101.3 (2) | O6—Ti4—Ti6 | 43.20 (14) |
O11—Ti1—O3 | 97.5 (2) | O5—Ti4—Ti6 | 97.35 (16) |
O2—Ti1—O3 | 102.0 (2) | O45—Ti4—Ti6 | 117.78 (17) |
O11—Ti1—O28 | 96.4 (2) | O68—Ti4—Ti6 | 78.05 (18) |
O2—Ti1—O28 | 88.5 (2) | O4—Ti4—Ti6 | 36.52 (14) |
O3—Ti1—O28 | 160.5 (2) | O41—Ti4—Ti5 | 140.5 (2) |
O11—Ti1—O15 | 94.3 (2) | O6—Ti4—Ti5 | 98.05 (15) |
O2—Ti1—O15 | 160.0 (2) | O5—Ti4—Ti5 | 42.42 (14) |
O3—Ti1—O15 | 88.1 (2) | O45—Ti4—Ti5 | 77.16 (17) |
O28—Ti1—O15 | 77.3 (2) | O68—Ti4—Ti5 | 120.36 (17) |
O11—Ti1—O1 | 174.3 (2) | O4—Ti4—Ti5 | 36.64 (14) |
O2—Ti1—O1 | 77.6 (2) | Ti6—Ti4—Ti5 | 68.13 (5) |
O3—Ti1—O1 | 77.4 (2) | O51—Ti5—O6ii | 101.8 (2) |
O28—Ti1—O1 | 89.1 (2) | O51—Ti5—O4 | 98.0 (2) |
O15—Ti1—O1 | 88.0 (2) | O6ii—Ti5—O4 | 101.5 (2) |
O11—Ti1—Ti2 | 143.2 (2) | O51—Ti5—O55 | 94.7 (2) |
O2—Ti1—Ti2 | 42.82 (15) | O6ii—Ti5—O55 | 87.3 (2) |
O3—Ti1—Ti2 | 98.19 (16) | O4—Ti5—O55 | 162.7 (2) |
O28—Ti1—Ti2 | 78.24 (18) | O51—Ti5—O48 | 93.3 (2) |
O15—Ti1—Ti2 | 119.20 (17) | O6ii—Ti5—O48 | 160.6 (2) |
O1—Ti1—Ti2 | 37.03 (13) | O4—Ti5—O48 | 88.2 (2) |
O11—Ti1—Ti3 | 139.45 (19) | O55—Ti5—O48 | 79.4 (2) |
O2—Ti1—Ti3 | 98.04 (16) | O51—Ti5—O5 | 175.2 (2) |
O3—Ti1—Ti3 | 43.33 (15) | O6ii—Ti5—O5 | 77.7 (2) |
O28—Ti1—Ti3 | 119.46 (17) | O4—Ti5—O5 | 77.5 (2) |
O15—Ti1—Ti3 | 77.37 (16) | O55—Ti5—O5 | 90.0 (2) |
O1—Ti1—Ti3 | 36.29 (13) | O48—Ti5—O5 | 88.3 (2) |
Ti2—Ti1—Ti3 | 68.24 (5) | O51—Ti5—Ti6ii | 144.11 (19) |
O21—Ti2—O3i | 103.3 (2) | O6ii—Ti5—Ti6ii | 43.40 (15) |
O21—Ti2—O1 | 97.6 (2) | O4—Ti5—Ti6ii | 97.90 (14) |
O3i—Ti2—O1 | 101.8 (2) | O55—Ti5—Ti6ii | 78.14 (16) |
O21—Ti2—O38i | 94.7 (3) | O48—Ti5—Ti6ii | 119.13 (16) |
O3i—Ti2—O38i | 87.4 (2) | O5—Ti5—Ti6ii | 36.57 (14) |
O1—Ti2—O38i | 162.5 (2) | O51—Ti5—Ti4 | 139.4 (2) |
O21—Ti2—O25 | 92.7 (2) | O6ii—Ti5—Ti4 | 98.26 (15) |
O3i—Ti2—O25 | 159.5 (2) | O4—Ti5—Ti4 | 43.13 (15) |
O1—Ti2—O25 | 88.6 (2) | O55—Ti5—Ti4 | 121.35 (17) |
O38i—Ti2—O25 | 78.4 (2) | O48—Ti5—Ti4 | 77.30 (16) |
O21—Ti2—O2 | 174.8 (2) | O5—Ti5—Ti4 | 36.77 (14) |
O3i—Ti2—O2 | 78.4 (2) | Ti6ii—Ti5—Ti4 | 68.25 (5) |
O1—Ti2—O2 | 77.2 (2) | O61—Ti6—O4 | 103.5 (2) |
O38i—Ti2—O2 | 90.2 (2) | O61—Ti6—O5ii | 101.9 (2) |
O25—Ti2—O2 | 86.8 (2) | O4—Ti6—O5ii | 101.5 (2) |
O21—Ti2—Ti3i | 145.76 (18) | O61—Ti6—O58ii | 91.8 (3) |
O3i—Ti2—Ti3i | 43.57 (15) | O4—Ti6—O58ii | 158.7 (2) |
O1—Ti2—Ti3i | 97.96 (15) | O5ii—Ti6—O58ii | 89.5 (2) |
O38i—Ti2—Ti3i | 78.28 (16) | O61—Ti6—O65 | 91.8 (2) |
O25—Ti2—Ti3i | 117.98 (17) | O4—Ti6—O65 | 87.8 (2) |
O2—Ti2—Ti3i | 37.15 (13) | O5ii—Ti6—O65 | 161.0 (2) |
O21—Ti2—Ti1 | 138.73 (19) | O58ii—Ti6—O65 | 76.8 (2) |
O3i—Ti2—Ti1 | 98.54 (16) | O61—Ti6—O6 | 178.7 (3) |
O1—Ti2—Ti1 | 43.23 (15) | O4—Ti6—O6 | 77.7 (2) |
O38i—Ti2—Ti1 | 121.13 (18) | O5ii—Ti6—O6 | 77.5 (2) |
O25—Ti2—Ti1 | 76.82 (18) | O58ii—Ti6—O6 | 87.1 (2) |
O2—Ti2—Ti1 | 36.22 (13) | O65—Ti6—O6 | 88.6 (2) |
Ti3i—Ti2—Ti1 | 68.21 (5) | O61—Ti6—Ti5ii | 142.18 (19) |
O31—Ti3—O1 | 102.9 (2) | O4—Ti6—Ti5ii | 98.17 (15) |
O31—Ti3—O2i | 101.3 (2) | O5ii—Ti6—Ti5ii | 42.90 (14) |
O1—Ti3—O2i | 101.4 (2) | O58ii—Ti6—Ti5ii | 77.44 (17) |
O31—Ti3—O35 | 92.8 (3) | O65—Ti6—Ti5ii | 119.89 (17) |
O1—Ti3—O35 | 159.0 (2) | O6—Ti6—Ti5ii | 36.87 (13) |
O2i—Ti3—O35 | 88.9 (2) | O61—Ti6—Ti4 | 144.8 (2) |
O31—Ti3—O18 | 92.4 (2) | O4—Ti6—Ti4 | 43.51 (15) |
O1—Ti3—O18 | 87.6 (2) | O5ii—Ti6—Ti4 | 97.90 (16) |
O2i—Ti3—O18 | 161.3 (2) | O58ii—Ti6—Ti4 | 117.37 (17) |
O35—Ti3—O18 | 77.7 (2) | O65—Ti6—Ti4 | 77.43 (18) |
O31—Ti3—O3 | 178.6 (2) | O6—Ti6—Ti4 | 36.51 (14) |
O1—Ti3—O3 | 77.8 (2) | Ti5ii—Ti6—Ti4 | 68.23 (5) |
O2i—Ti3—O3 | 77.36 (19) | Ti6—O4—Ti5 | 135.5 (3) |
O35—Ti3—O3 | 86.9 (2) | Ti6—O4—Ti4 | 100.0 (2) |
O18—Ti3—O3 | 88.9 (2) | Ti5—O4—Ti4 | 100.2 (2) |
O31—Ti3—Ti2i | 142.29 (18) | Ti6ii—O5—Ti4 | 134.8 (3) |
O1—Ti3—Ti2i | 97.86 (14) | Ti6ii—O5—Ti5 | 100.5 (2) |
O2i—Ti3—Ti2i | 43.27 (16) | Ti4—O5—Ti5 | 100.8 (2) |
O35—Ti3—Ti2i | 77.10 (16) | Ti4—O6—Ti5ii | 135.1 (3) |
O18—Ti3—Ti2i | 119.81 (17) | Ti4—O6—Ti6 | 100.3 (2) |
O3—Ti3—Ti2i | 36.31 (12) | Ti5ii—O6—Ti6 | 99.7 (2) |
O31—Ti3—Ti1 | 144.0 (2) | C42—O41—Ti4 | 162.5 (7) |
O1—Ti3—Ti1 | 42.96 (15) | O41—C42—C44 | 113.2 (10) |
O2i—Ti3—Ti1 | 97.90 (15) | O41—C42—C43 | 109.6 (9) |
O35—Ti3—Ti1 | 117.95 (18) | C44—C42—C43 | 119.1 (12) |
O18—Ti3—Ti1 | 77.55 (17) | O41—C42—H42A | 104.4 |
O3—Ti3—Ti1 | 37.06 (12) | C44—C42—H42A | 104.4 |
Ti2i—Ti3—Ti1 | 68.13 (5) | C43—C42—H42A | 104.4 |
Ti3—O1—Ti2 | 135.2 (3) | C42—C43—H43A | 109.5 |
Ti3—O1—Ti1 | 100.7 (2) | C42—C43—H43B | 109.5 |
Ti2—O1—Ti1 | 99.7 (2) | H43A—C43—H43B | 109.5 |
Ti1—O2—Ti3i | 134.9 (3) | C42—C43—H43C | 109.5 |
Ti1—O2—Ti2 | 101.0 (2) | H43A—C43—H43C | 109.5 |
Ti3i—O2—Ti2 | 99.6 (2) | H43B—C43—H43C | 109.5 |
Ti2i—O3—Ti1 | 134.9 (3) | C42—C44—H44A | 109.5 |
Ti2i—O3—Ti3 | 100.1 (2) | C42—C44—H44B | 109.5 |
Ti1—O3—Ti3 | 99.6 (2) | H44A—C44—H44B | 109.5 |
C12—O11—Ti1 | 157.2 (6) | C42—C44—H44C | 109.5 |
O11—C12—C14 | 112.5 (9) | H44A—C44—H44C | 109.5 |
O11—C12—C13 | 109.3 (8) | H44B—C44—H44C | 109.5 |
C14—C12—C13 | 112.2 (9) | C46—O45—Ti4 | 130.6 (6) |
O11—C12—H12A | 107.5 | O48—C46—O45 | 124.0 (9) |
C14—C12—H12A | 107.5 | O48—C46—C47 | 117.9 (9) |
C13—C12—H12A | 107.5 | O45—C46—C47 | 118.1 (9) |
C12—C13—H13A | 109.5 | C46—C47—H47A | 109.5 |
C12—C13—H13B | 109.5 | C46—C47—H47B | 109.5 |
H13A—C13—H13B | 109.5 | H47A—C47—H47B | 109.5 |
C12—C13—H13C | 109.5 | C46—C47—H47C | 109.5 |
H13A—C13—H13C | 109.5 | H47A—C47—H47C | 109.5 |
H13B—C13—H13C | 109.5 | H47B—C47—H47C | 109.5 |
C12—C14—H14A | 109.5 | C46—O48—Ti5 | 130.3 (6) |
C12—C14—H14B | 109.5 | C52—O51—Ti5 | 153.3 (8) |
H14A—C14—H14B | 109.5 | O51—C52—C53B | 120.7 (15) |
C12—C14—H14C | 109.5 | O51—C52—C54B | 117.7 (15) |
H14A—C14—H14C | 109.5 | C53B—C52—C54B | 119.5 (18) |
H14B—C14—H14C | 109.5 | O51—C52—C54A | 118.4 (19) |
C16—O15—Ti1 | 130.1 (6) | C53B—C52—C54A | 90 (2) |
O18—C16—O15 | 123.4 (8) | C54B—C52—C54A | 76 (2) |
O18—C16—C17 | 119.4 (9) | O51—C52—C53A | 104.4 (17) |
O15—C16—C17 | 117.2 (9) | C53B—C52—C53A | 95 (2) |
C16—C17—H17A | 109.5 | C54B—C52—C53A | 55.4 (17) |
C16—C17—H17B | 109.5 | C54A—C52—C53A | 127 (2) |
H17A—C17—H17B | 109.5 | O51—C52—H52A | 100.9 |
C16—C17—H17C | 109.5 | C53B—C52—H52A | 19.8 |
H17A—C17—H17C | 109.5 | C54B—C52—H52A | 137.8 |
H17B—C17—H17C | 109.5 | C54A—C52—H52A | 100.9 |
C16—O18—Ti3 | 130.9 (6) | C53A—C52—H52A | 100.9 |
C22—O21—Ti2 | 154.5 (6) | O51—C52—H52B | 94.4 |
C24—C22—O21 | 114.8 (12) | C53B—C52—H52B | 101.9 |
C24—C22—C23 | 115.5 (12) | C54B—C52—H52B | 88.2 |
O21—C22—C23 | 110.5 (10) | C54A—C52—H52B | 24.1 |
C24—C22—H22A | 104.9 | C53A—C52—H52B | 143.5 |
O21—C22—H22A | 104.9 | H52A—C52—H52B | 106.0 |
C23—C22—H22A | 104.9 | C52—C53A—H53A | 109.5 |
C22—C23—H23A | 109.5 | C52—C53A—H53B | 109.5 |
C22—C23—H23B | 109.5 | H53A—C53A—H53B | 109.5 |
H23A—C23—H23B | 109.5 | C52—C53A—H53C | 109.5 |
C22—C23—H23C | 109.5 | H53A—C53A—H53C | 109.5 |
H23A—C23—H23C | 109.5 | H53B—C53A—H53C | 109.5 |
H23B—C23—H23C | 109.5 | C52—C54A—H52B | 38.4 |
C22—C24—H24A | 109.5 | C52—C54A—H54A | 109.5 |
C22—C24—H24B | 109.5 | H52B—C54A—H54A | 80.8 |
H24A—C24—H24B | 109.5 | C52—C54A—H54B | 109.5 |
C22—C24—H24C | 109.5 | H52B—C54A—H54B | 145.6 |
H24A—C24—H24C | 109.5 | H54A—C54A—H54B | 109.5 |
H24B—C24—H24C | 109.5 | C52—C54A—H54C | 109.5 |
C26—O25—Ti2 | 130.3 (6) | H52B—C54A—H54C | 96.8 |
O28—C26—O25 | 124.7 (8) | H54A—C54A—H54C | 109.5 |
O28—C26—C27 | 118.9 (9) | H54B—C54A—H54C | 109.5 |
O25—C26—C27 | 116.4 (9) | C52—C53B—H53D | 109.5 |
C26—C27—H27A | 109.5 | C52—C53B—H53E | 109.5 |
C26—C27—H27B | 109.5 | H53D—C53B—H53E | 109.5 |
H27A—C27—H27B | 109.5 | C52—C53B—H53F | 109.5 |
C26—C27—H27C | 109.5 | H53D—C53B—H53F | 109.5 |
H27A—C27—H27C | 109.5 | H53E—C53B—H53F | 109.5 |
H27B—C27—H27C | 109.5 | C52—C54B—H54D | 109.5 |
C26—O28—Ti1 | 129.8 (6) | C52—C54B—H54E | 109.5 |
C32—O31—Ti3 | 155.3 (7) | H54D—C54B—H54E | 109.5 |
C34—C32—O31 | 118.7 (11) | C52—C54B—H54F | 109.5 |
C34—C32—C33 | 123.2 (11) | H54D—C54B—H54F | 109.5 |
O31—C32—C33 | 111.3 (10) | H54E—C54B—H54F | 109.5 |
C34—C32—H32A | 98.7 | C56—O55—Ti5 | 129.2 (6) |
O31—C32—H32A | 98.7 | O55—C56—O58 | 124.6 (10) |
C33—C32—H32A | 98.7 | O55—C56—C57 | 119.0 (9) |
C32—C33—H33A | 109.5 | O58—C56—C57 | 116.4 (9) |
C32—C33—H33B | 109.5 | C56—C57—H57A | 109.5 |
H33A—C33—H33B | 109.5 | C56—C57—H57B | 109.5 |
C32—C33—H33C | 109.5 | H57A—C57—H57B | 109.5 |
H33A—C33—H33C | 109.5 | C56—C57—H57C | 109.5 |
H33B—C33—H33C | 109.5 | H57A—C57—H57C | 109.5 |
C32—C34—H34A | 109.5 | H57B—C57—H57C | 109.5 |
C32—C34—H34B | 109.5 | C56—O58—Ti6ii | 129.7 (6) |
H34A—C34—H34B | 109.5 | C62—O61—Ti6 | 144.9 (8) |
C32—C34—H34C | 109.5 | C64—C62—C63 | 124.8 (15) |
H34A—C34—H34C | 109.5 | C64—C62—O61 | 116.7 (14) |
H34B—C34—H34C | 109.5 | C63—C62—O61 | 115.9 (14) |
C36—O35—Ti3 | 130.3 (6) | C64—C62—H62A | 95.4 |
O38—C36—O35 | 124.1 (9) | C63—C62—H62A | 95.4 |
O38—C36—C37 | 118.8 (9) | O61—C62—H62A | 95.4 |
O35—C36—C37 | 117.1 (9) | C62—C63—H63A | 109.5 |
C36—C37—H37A | 109.5 | C62—C63—H63B | 109.5 |
C36—C37—H37B | 109.5 | H63A—C63—H63B | 109.5 |
H37A—C37—H37B | 109.5 | C62—C63—H63C | 109.5 |
C36—C37—H37C | 109.5 | H63A—C63—H63C | 109.5 |
H37A—C37—H37C | 109.5 | H63B—C63—H63C | 109.5 |
H37B—C37—H37C | 109.5 | C62—C64—H64A | 109.5 |
C36—O38—Ti2i | 129.7 (6) | C62—C64—H64B | 109.5 |
O41—Ti4—O6 | 101.4 (2) | H64A—C64—H64B | 109.5 |
O41—Ti4—O5 | 99.6 (2) | C62—C64—H64C | 109.5 |
O6—Ti4—O5 | 101.5 (2) | H64A—C64—H64C | 109.5 |
O41—Ti4—O45 | 94.8 (2) | H64B—C64—H64C | 109.5 |
O6—Ti4—O45 | 158.9 (2) | C66—O65—Ti6 | 128.7 (6) |
O5—Ti4—O45 | 88.8 (2) | O68—C66—O65 | 126.3 (9) |
O41—Ti4—O68 | 94.6 (2) | O68—C66—C67 | 117.4 (10) |
O6—Ti4—O68 | 87.8 (2) | O65—C66—C67 | 116.2 (10) |
O5—Ti4—O68 | 161.0 (2) | C66—C67—H67A | 109.5 |
O45—Ti4—O68 | 77.4 (3) | C66—C67—H67B | 109.5 |
O41—Ti4—O4 | 175.8 (2) | H67A—C67—H67B | 109.5 |
O6—Ti4—O4 | 77.4 (2) | C66—C67—H67C | 109.5 |
O5—Ti4—O4 | 76.7 (2) | H67A—C67—H67C | 109.5 |
O45—Ti4—O4 | 87.3 (2) | H67B—C67—H67C | 109.5 |
O68—Ti4—O4 | 89.4 (2) | C66—O68—Ti4 | 128.6 (6) |
O41—Ti4—Ti6 | 143.4 (2) |
Symmetry codes: (i) −x+1, −y+1, −z; (ii) −x+2, −y+2, −z+1. |