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
Key indicators
- Single-crystal X-ray study
- T = 298 K
- Mean (C-C) = 0.016 Å
- Disorder in main residue
- R factor = 0.076
- wR factor = 0.195
- Data-to-parameter ratio = 14.1
checkCIF/PLATON results
No syntax errors found
Alert level A PLAT029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.91
Author Response: see _publ_section_exptl_refinement |
Alert level B PLAT026_ALERT_3_B Ratio Observed / Unique Reflections too Low .... 38 Perc. PLAT213_ALERT_2_B Atom C54A has ADP max/min Ratio ............. 4.30 prolat PLAT220_ALERT_2_B Large Non-Solvent C Ueq(max)/Ueq(min) ... 4.10 Ratio PLAT220_ALERT_2_B Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.65 Ratio PLAT242_ALERT_2_B Check Low Ueq as Compared to Neighbors for O51 PLAT242_ALERT_2_B Check Low Ueq as Compared to Neighbors for O61 PLAT242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C52 PLAT242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C62 PLAT242_ALERT_2_B Check Low Ueq as Compared to Neighbors for O31 PLAT242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C22 PLAT341_ALERT_3_B Low Bond Precision on C-C bonds (x 1000) Ang ... 16
Alert level C REFLT03_ALERT_3_C Reflection count < 95% complete From the CIF: _diffrn_reflns_theta_max 25.03 From the CIF: _diffrn_reflns_theta_full 25.03 From the CIF: _reflns_number_total 7905 TEST2: Reflns within _diffrn_reflns_theta_max Count of symmetry unique reflns 8662 Completeness (_total/calc) 91.26% PLAT022_ALERT_3_C Ratio Unique / Expected Reflections too Low .... 0.91 PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ? PLAT213_ALERT_2_C Atom C54B has ADP max/min Ratio ............. 3.20 prolat PLAT213_ALERT_2_C Atom C24 has ADP max/min Ratio ............. 3.10 prolat PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.03 Ratio PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.59 Ratio PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for O41 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C42 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C66 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for O21 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C12 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C26 PLAT301_ALERT_3_C Main Residue Disorder ......................... 3.00 Perc. PLAT360_ALERT_2_C Short C(sp3)-C(sp3) Bond C42 - C44 ... 1.41 Ang. PLAT360_ALERT_2_C Short C(sp3)-C(sp3) Bond C62 - C63 ... 1.36 Ang. PLAT360_ALERT_2_C Short C(sp3)-C(sp3) Bond C62 - C64 ... 1.34 Ang. PLAT360_ALERT_2_C Short C(sp3)-C(sp3) Bond C22 - C24 ... 1.36 Ang. PLAT360_ALERT_2_C Short C(sp3)-C(sp3) Bond C32 - C34 ... 1.36 Ang. PLAT380_ALERT_4_C Check Incorrectly? Oriented X(sp2)-Methyl Moiety C67 PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.19 Ratio PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 19.80 Deg. C53B -C52 -H52A 1.555 1.555 1.555 PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 24.10 Deg. C54A -C52 -H52B 1.555 1.555 1.555 PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 38.40 Deg. C52 -C54A -H52B 1.555 1.555 1.555
1 ALERT level A = In general: serious problem 11 ALERT level B = Potentially serious problem 24 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 25 ALERT type 2 Indicator that the structure model may be wrong or deficient 8 ALERT type 3 Indicator that the structure quality may be low 2 ALERT type 4 Improvement, methodology, query or suggestion
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. |