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The title compound, [Ti6(C2H3O2)6(C3H7O)6O6], was pre­pared by the stoichiometric reaction of acetic acid with titanium isopropoxide in supercritical CO2. There are two independent half-mol­ecules in the asymmetric unit. The symmetry-complete hexa­prismatic mol­ecules are centro­symmetric.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806002492/lh6581sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806002492/lh6581Isup2.hkl
Contains datablock I

CCDC reference: 298497

Key indicators

  • Single-crystal X-ray study
  • T = 298 K
  • Mean [sigma](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

Computing details top

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.

Hexakis(µ-acetato-κ2O,O')hexaisopropoxyhexa-µ3-oxo-hexatitanium top
Crystal data top
[Ti6(C2H3O2)6(C3H7O)6O6]Z = 2
Mr = 1092.18F(000) = 1128
Triclinic, P1Dx = 1.480 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 10.2466 (14) ÅCell parameters from 20933 reflections
b = 12.2908 (12) Åθ = 1.7–25.0°
c = 20.225 (3) ŵ = 1.01 mm1
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
Data collection top
Bruker–Nonius KappaCCD
diffractometer
7905 independent reflections
Radiation source: fine-focus sealed tube2994 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.091
φ scans, and ω scans with κ offsetsθmax = 25.0°, θmin = 2.6°
Absorption correction: multi-scan
(SORTAV; Blessing, 1995)
h = 1212
Tmin = 0.811, Tmax = 0.949k = 1414
13625 measured reflectionsl = 1924
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.076Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.195H-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 parametersΔρmax = 0.35 e Å3
483 restraintsΔρmin = 0.40 e Å3
Special details top

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Ti10.57920 (15)0.41884 (11)0.09764 (8)0.0586 (5)
Ti20.69757 (15)0.37779 (11)0.05126 (8)0.0596 (5)
Ti30.36725 (16)0.36982 (11)0.00942 (8)0.0592 (5)
O10.5573 (5)0.3382 (4)0.0058 (2)0.0534 (13)
O20.6734 (5)0.4899 (4)0.0336 (3)0.0539 (13)
O30.3948 (5)0.4859 (4)0.0845 (2)0.0504 (13)
O110.5840 (5)0.4947 (4)0.1695 (3)0.0653 (15)
C120.5324 (11)0.5625 (8)0.2269 (5)0.084 (3)
H12A0.51710.64110.21370.101*
C130.6371 (12)0.5423 (9)0.2752 (5)0.128 (4)
H13A0.71960.55610.25410.192*
H13B0.65410.46580.28920.192*
H13C0.60450.59210.31320.192*
C140.4018 (11)0.5461 (9)0.2569 (5)0.126 (4)
H14A0.33760.56120.22470.189*
H14B0.36870.59640.29460.189*
H14C0.41390.46990.27090.189*
O150.5137 (6)0.2929 (4)0.1481 (3)0.0650 (15)
C160.4372 (10)0.2323 (7)0.1313 (5)0.067 (3)
C170.4267 (10)0.1364 (7)0.1733 (5)0.101 (4)
H17A0.36520.09870.15640.151*
H17B0.39360.16280.21810.151*
H17C0.51450.08490.17280.151*
O180.3733 (6)0.2501 (4)0.0811 (3)0.0705 (17)
O210.7067 (5)0.2809 (4)0.1164 (3)0.0657 (16)
C220.7231 (14)0.1737 (8)0.1439 (6)0.118 (4)
H22A0.63590.17530.16010.142*
C230.7377 (15)0.0891 (8)0.0916 (7)0.168 (6)
H23A0.74380.01650.11100.252*
H23B0.66030.10860.05870.252*
H23C0.81850.08700.07110.252*
C240.8159 (19)0.1476 (11)0.1987 (8)0.242 (10)
H24A0.79520.20520.23090.363*
H24B0.81290.07690.21770.363*
H24C0.90500.14240.18620.363*
O250.8367 (5)0.2657 (4)0.0027 (3)0.0680 (16)
C260.8428 (10)0.2498 (7)0.0594 (6)0.069 (3)
C270.9642 (10)0.1607 (8)0.0784 (5)0.122 (4)
H27A0.95740.15420.12590.182*
H27B1.04620.18190.06320.182*
H27C0.96580.08980.05810.182*
O280.7553 (6)0.2998 (4)0.1044 (3)0.0669 (16)
O310.3428 (6)0.2787 (4)0.0523 (3)0.0689 (16)
C320.2819 (16)0.2026 (9)0.0791 (6)0.140 (5)
H32A0.18820.23500.05980.168*
C330.3077 (15)0.0984 (8)0.0441 (6)0.166 (6)
H33A0.26040.04900.06210.249*
H33B0.27660.11310.00220.249*
H33C0.40330.06360.04920.249*
C340.2619 (14)0.2092 (10)0.1447 (6)0.160 (6)
H34A0.23430.28670.15640.240*
H34B0.19250.17240.15260.240*
H34C0.34480.17310.17130.240*
O350.1690 (6)0.4030 (5)0.0496 (3)0.0698 (16)
C360.0938 (10)0.4905 (9)0.0808 (5)0.066 (2)
C370.0405 (9)0.4813 (7)0.1144 (5)0.094 (3)
H37A0.05080.40690.10700.142*
H37B0.11200.53520.09630.142*
H37C0.04460.49590.16130.142*
O380.1266 (5)0.5817 (5)0.0858 (3)0.0708 (18)
Ti40.85058 (16)0.97592 (12)0.42432 (8)0.0640 (5)
Ti51.14293 (16)0.83775 (12)0.44706 (8)0.0619 (5)
Ti60.87059 (16)0.90903 (12)0.57209 (8)0.0638 (5)
O40.9639 (5)0.8543 (4)0.4889 (3)0.0597 (13)
O51.0323 (5)0.9886 (4)0.4041 (3)0.0580 (14)
O60.8024 (5)1.0489 (4)0.5083 (3)0.0567 (14)
O410.7680 (5)1.0798 (4)0.3729 (3)0.0697 (16)
C420.7333 (13)1.1448 (10)0.3173 (6)0.113 (4)
H42A0.79021.19820.31570.136*
C430.7820 (14)1.0741 (10)0.2553 (6)0.158 (6)
H43A0.87751.04050.25420.237*
H43B0.76531.12030.21720.237*
H43C0.73451.01610.25460.237*
C440.5998 (15)1.2127 (11)0.3254 (6)0.192 (7)
H44A0.58671.25920.36480.288*
H44B0.53731.16590.32940.288*
H44C0.58421.25930.28740.288*
O450.8901 (6)0.8487 (5)0.3536 (3)0.0740 (17)
C460.9880 (12)0.7631 (8)0.3436 (5)0.077 (3)
C470.9774 (10)0.6747 (7)0.2949 (5)0.107 (4)
H47A0.89230.69760.27660.160*
H47B0.98290.60490.31710.160*
H47C1.05040.66520.25970.160*
O481.0950 (6)0.7473 (4)0.3717 (3)0.0699 (16)
O511.2222 (5)0.7169 (4)0.4875 (3)0.0713 (17)
C521.2379 (19)0.6085 (10)0.5057 (7)0.155 (6)
H52A1.27350.61050.54860.186*0.447 (19)
H52B1.14040.61560.51590.186*0.553 (19)
C53A1.358 (3)0.548 (2)0.465 (2)0.188 (15)0.447 (19)
H53A1.37600.46940.47510.282*0.447 (19)
H53B1.43340.57630.47370.282*0.447 (19)
H53C1.34370.55700.41890.282*0.447 (19)
C54A1.122 (3)0.571 (3)0.525 (2)0.26 (2)0.447 (19)
H54A1.06150.62400.55590.387*0.447 (19)
H54B1.14690.49910.54490.387*0.447 (19)
H54C1.07670.56420.48610.387*0.447 (19)
C53B1.286 (4)0.5732 (18)0.5655 (12)0.215 (16)0.553 (19)
H53D1.21590.59970.60130.322*0.553 (19)
H53E1.36260.60270.57140.322*0.553 (19)
H53F1.31360.49250.56520.322*0.553 (19)
C54B1.240 (5)0.5288 (18)0.4563 (14)0.221 (15)0.553 (19)
H54D1.14840.52480.45200.331*0.553 (19)
H54E1.29210.45660.46810.331*0.553 (19)
H54F1.27920.55020.41470.331*0.553 (19)
O551.3055 (6)0.8311 (4)0.3771 (3)0.0677 (16)
C561.3478 (11)0.9105 (9)0.3508 (5)0.075 (3)
C571.4807 (10)0.8835 (7)0.3066 (5)0.093 (3)
H57A1.51770.80350.30390.139*
H57B1.54320.91840.32500.139*
H57C1.46580.91130.26300.139*
O581.2876 (6)1.0142 (5)0.3595 (3)0.0750 (18)
O610.9248 (6)0.7968 (4)0.6258 (3)0.0719 (17)
C620.8836 (17)0.7341 (12)0.6780 (7)0.156 (5)
H62A0.79540.78720.68990.188*
C630.9325 (17)0.7454 (18)0.7368 (8)0.275 (10)
H63A0.89150.70530.77040.412*
H63B0.91140.82350.74960.412*
H63C1.02910.71520.73200.412*
C640.8327 (18)0.6487 (12)0.6614 (9)0.249 (9)
H64A0.79930.61670.70110.374*
H64B0.90250.59220.63660.374*
H64C0.75970.67590.63480.374*
O650.7139 (6)0.8451 (5)0.5477 (3)0.0748 (17)
C660.6578 (9)0.8550 (7)0.4936 (6)0.067 (2)
C670.5409 (9)0.8009 (8)0.4916 (6)0.105 (4)
H67A0.50610.81350.44920.158*
H67B0.47050.83330.52630.158*
H67C0.57200.72150.49790.158*
O680.6875 (6)0.9067 (5)0.4442 (3)0.0738 (17)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ti10.0623 (11)0.0565 (9)0.0591 (11)0.0156 (8)0.0145 (9)0.0050 (8)
Ti20.0588 (11)0.0575 (10)0.0622 (12)0.0118 (8)0.0120 (9)0.0077 (9)
Ti30.0653 (11)0.0559 (10)0.0616 (12)0.0227 (8)0.0119 (9)0.0060 (8)
O10.056 (3)0.047 (3)0.057 (3)0.011 (2)0.009 (3)0.006 (2)
O20.052 (3)0.053 (3)0.061 (3)0.019 (2)0.011 (3)0.001 (2)
O30.052 (3)0.047 (3)0.055 (4)0.015 (2)0.007 (3)0.002 (2)
O110.070 (4)0.071 (3)0.056 (3)0.019 (3)0.010 (3)0.017 (3)
C120.103 (8)0.083 (7)0.061 (7)0.012 (6)0.006 (5)0.012 (5)
C130.170 (11)0.148 (10)0.079 (8)0.048 (9)0.052 (8)0.008 (7)
C140.106 (8)0.156 (10)0.091 (9)0.008 (8)0.034 (6)0.020 (8)
O150.083 (4)0.063 (3)0.056 (4)0.029 (3)0.017 (3)0.006 (3)
C160.082 (7)0.057 (6)0.065 (7)0.026 (5)0.008 (5)0.001 (5)
C170.140 (10)0.090 (7)0.094 (8)0.066 (7)0.025 (7)0.030 (6)
O180.090 (5)0.066 (4)0.067 (4)0.036 (3)0.019 (4)0.005 (3)
O210.076 (4)0.054 (3)0.066 (4)0.015 (3)0.007 (3)0.014 (3)
C220.165 (11)0.072 (6)0.100 (9)0.002 (8)0.004 (8)0.025 (5)
C230.265 (17)0.064 (6)0.185 (12)0.044 (9)0.063 (12)0.015 (7)
C240.32 (2)0.136 (11)0.204 (15)0.008 (13)0.133 (15)0.083 (9)
O250.065 (4)0.065 (4)0.067 (4)0.002 (3)0.012 (3)0.007 (3)
C260.065 (6)0.061 (6)0.076 (6)0.004 (4)0.023 (5)0.006 (5)
C270.098 (8)0.127 (9)0.105 (9)0.040 (6)0.023 (7)0.019 (7)
O280.064 (4)0.066 (4)0.068 (4)0.009 (3)0.013 (3)0.000 (3)
O310.093 (4)0.065 (3)0.062 (4)0.038 (3)0.020 (3)0.005 (3)
C320.262 (15)0.089 (7)0.105 (9)0.092 (9)0.064 (10)0.008 (7)
C330.307 (19)0.089 (7)0.138 (11)0.106 (10)0.048 (12)0.004 (7)
C340.246 (16)0.164 (11)0.109 (10)0.098 (11)0.086 (11)0.012 (8)
O350.061 (3)0.070 (4)0.085 (5)0.026 (3)0.016 (3)0.005 (3)
C360.060 (6)0.088 (6)0.057 (7)0.025 (5)0.021 (5)0.008 (5)
C370.062 (6)0.109 (7)0.116 (9)0.030 (5)0.003 (6)0.005 (7)
O380.059 (4)0.072 (4)0.082 (5)0.017 (3)0.008 (4)0.005 (4)
Ti40.0650 (12)0.0633 (10)0.0665 (12)0.0156 (8)0.0214 (10)0.0006 (9)
Ti50.0630 (11)0.0575 (10)0.0656 (12)0.0121 (8)0.0158 (9)0.0023 (9)
Ti60.0680 (12)0.0604 (10)0.0658 (12)0.0184 (9)0.0146 (10)0.0023 (9)
O40.066 (3)0.051 (3)0.066 (3)0.020 (2)0.015 (3)0.002 (2)
O50.066 (3)0.056 (3)0.054 (4)0.017 (2)0.016 (3)0.001 (3)
O60.055 (3)0.057 (3)0.060 (3)0.015 (2)0.015 (3)0.004 (2)
O410.080 (4)0.069 (3)0.065 (4)0.018 (3)0.031 (3)0.009 (3)
C420.133 (9)0.127 (10)0.072 (7)0.017 (7)0.017 (8)0.030 (6)
C430.201 (14)0.170 (12)0.079 (7)0.001 (10)0.025 (9)0.008 (8)
C440.211 (14)0.174 (12)0.132 (12)0.083 (10)0.070 (10)0.015 (10)
O450.085 (4)0.070 (4)0.071 (4)0.018 (3)0.026 (3)0.012 (3)
C460.092 (8)0.069 (6)0.080 (8)0.030 (5)0.025 (6)0.001 (5)
C470.128 (10)0.079 (6)0.115 (10)0.015 (6)0.043 (7)0.035 (6)
O480.075 (4)0.065 (3)0.072 (4)0.018 (3)0.016 (3)0.014 (3)
O510.075 (4)0.051 (3)0.085 (4)0.007 (3)0.017 (3)0.006 (3)
C520.253 (17)0.061 (6)0.138 (12)0.010 (8)0.042 (12)0.013 (6)
C53A0.16 (2)0.055 (15)0.33 (4)0.013 (15)0.06 (2)0.02 (2)
C54A0.42 (4)0.11 (2)0.21 (4)0.09 (2)0.19 (4)0.03 (3)
C53B0.44 (5)0.071 (15)0.14 (2)0.04 (2)0.12 (3)0.039 (12)
C54B0.40 (4)0.089 (12)0.24 (3)0.11 (2)0.20 (3)0.022 (14)
O550.072 (4)0.062 (4)0.068 (4)0.017 (3)0.005 (3)0.010 (3)
C560.081 (7)0.089 (6)0.055 (7)0.021 (5)0.008 (5)0.006 (6)
C570.090 (7)0.086 (7)0.092 (8)0.015 (5)0.018 (6)0.009 (6)
O580.071 (4)0.074 (4)0.075 (5)0.014 (3)0.004 (4)0.002 (4)
O610.086 (4)0.065 (4)0.069 (4)0.021 (3)0.020 (4)0.014 (3)
C620.246 (16)0.145 (11)0.096 (10)0.082 (10)0.024 (9)0.050 (8)
C630.210 (17)0.55 (3)0.124 (12)0.181 (19)0.078 (13)0.163 (16)
C640.29 (2)0.159 (14)0.35 (2)0.148 (13)0.042 (18)0.107 (15)
O650.068 (4)0.079 (4)0.084 (5)0.028 (3)0.014 (3)0.005 (4)
C660.055 (6)0.057 (6)0.090 (8)0.014 (4)0.007 (5)0.013 (5)
C670.082 (8)0.108 (8)0.149 (11)0.055 (6)0.043 (7)0.028 (7)
O680.071 (4)0.076 (4)0.085 (5)0.030 (3)0.031 (3)0.010 (3)
Geometric parameters (Å, º) top
Ti1—O111.740 (6)Ti4—O42.175 (5)
Ti1—O21.876 (5)Ti4—Ti63.112 (2)
Ti1—O31.909 (5)Ti4—Ti53.131 (2)
Ti1—O282.035 (6)Ti5—O511.751 (5)
Ti1—O152.063 (5)Ti5—O6ii1.891 (5)
Ti1—O12.166 (5)Ti5—O41.899 (5)
Ti1—Ti23.117 (2)Ti5—O552.052 (6)
Ti1—Ti33.123 (2)Ti5—O482.061 (6)
Ti2—O211.758 (5)Ti5—O52.150 (5)
Ti2—O3i1.867 (5)Ti5—Ti6ii3.106 (2)
Ti2—O11.904 (5)Ti6—O611.768 (5)
Ti2—O38i2.041 (6)Ti6—O41.880 (6)
Ti2—O252.050 (5)Ti6—O5ii1.882 (5)
Ti2—O22.158 (5)Ti6—O58ii2.048 (6)
Ti2—Ti3i3.105 (2)Ti6—O652.060 (6)
Ti3—O311.758 (5)Ti6—O62.165 (5)
Ti3—O11.881 (5)Ti6—Ti5ii3.106 (2)
Ti3—O2i1.901 (5)O5—Ti6ii1.882 (5)
Ti3—O352.046 (6)O6—Ti5ii1.891 (5)
Ti3—O182.058 (6)O41—C421.402 (10)
Ti3—O32.173 (5)C42—C441.405 (14)
Ti3—Ti2i3.105 (2)C42—C431.494 (14)
O2—Ti3i1.901 (5)C42—H42A0.9800
O3—Ti2i1.867 (5)C43—H43A0.9600
O11—C121.405 (10)C43—H43B0.9600
C12—C141.470 (13)C43—H43C0.9600
C12—C131.501 (12)C44—H44A0.9600
C12—H12A0.9800C44—H44B0.9600
C13—H13A0.9600C44—H44C0.9600
C13—H13B0.9600O45—C461.259 (10)
C13—H13C0.9600C46—O481.258 (10)
C14—H14A0.9600C46—C471.500 (12)
C14—H14B0.9600C47—H47A0.9600
C14—H14C0.9600C47—H47B0.9600
O15—C161.279 (9)C47—H47C0.9600
C16—O181.256 (10)O51—C521.355 (12)
C16—C171.470 (11)C52—C53B1.384 (15)
C17—H17A0.9600C52—C54B1.398 (16)
C17—H17B0.9600C52—C54A1.398 (17)
C17—H17C0.9600C52—C53A1.439 (17)
O21—C221.394 (10)C52—H52A0.9800
C22—C241.364 (15)C52—H52B0.9800
C22—C231.475 (14)C53A—H53A0.9600
C22—H22A0.9800C53A—H53B0.9600
C23—H23A0.9600C53A—H53C0.9600
C23—H23B0.9600C54A—H52B0.6428
C23—H23C0.9600C54A—H54A0.9600
C24—H24A0.9600C54A—H54B0.9600
C24—H24B0.9600C54A—H54C0.9600
C24—H24C0.9600C53B—H53D0.9600
O25—C261.275 (10)C53B—H53E0.9600
C26—O281.249 (10)C53B—H53F0.9600
C26—C271.520 (11)C54B—H54D0.9600
C27—H27A0.9600C54B—H54E0.9600
C27—H27B0.9600C54B—H54F0.9600
C27—H27C0.9600O55—C561.259 (10)
O31—C321.388 (11)C56—O581.273 (10)
C32—C341.362 (13)C56—C571.508 (12)
C32—C331.442 (13)C57—H57A0.9600
C32—H32A0.9800C57—H57B0.9600
C33—H33A0.9600C57—H57C0.9600
C33—H33B0.9600O58—Ti6ii2.048 (6)
C33—H33C0.9600O61—C621.397 (12)
C34—H34A0.9600C62—C641.343 (17)
C34—H34B0.9600C62—C631.359 (17)
C34—H34C0.9600C62—H62A0.9800
O35—C361.277 (10)C63—H63A0.9600
C36—O381.256 (10)C63—H63B0.9600
C36—C371.498 (11)C63—H63C0.9600
C37—H37A0.9600C64—H64A0.9600
C37—H37B0.9600C64—H64B0.9600
C37—H37C0.9600C64—H64C0.9600
O38—Ti2i2.041 (6)O65—C661.280 (10)
Ti4—O411.751 (5)C66—O681.235 (10)
Ti4—O61.882 (5)C66—C671.513 (11)
Ti4—O51.908 (5)C67—H67A0.9600
Ti4—O452.055 (6)C67—H67B0.9600
Ti4—O682.060 (6)C67—H67C0.9600
O11—Ti1—O2101.3 (2)O6—Ti4—Ti643.20 (14)
O11—Ti1—O397.5 (2)O5—Ti4—Ti697.35 (16)
O2—Ti1—O3102.0 (2)O45—Ti4—Ti6117.78 (17)
O11—Ti1—O2896.4 (2)O68—Ti4—Ti678.05 (18)
O2—Ti1—O2888.5 (2)O4—Ti4—Ti636.52 (14)
O3—Ti1—O28160.5 (2)O41—Ti4—Ti5140.5 (2)
O11—Ti1—O1594.3 (2)O6—Ti4—Ti598.05 (15)
O2—Ti1—O15160.0 (2)O5—Ti4—Ti542.42 (14)
O3—Ti1—O1588.1 (2)O45—Ti4—Ti577.16 (17)
O28—Ti1—O1577.3 (2)O68—Ti4—Ti5120.36 (17)
O11—Ti1—O1174.3 (2)O4—Ti4—Ti536.64 (14)
O2—Ti1—O177.6 (2)Ti6—Ti4—Ti568.13 (5)
O3—Ti1—O177.4 (2)O51—Ti5—O6ii101.8 (2)
O28—Ti1—O189.1 (2)O51—Ti5—O498.0 (2)
O15—Ti1—O188.0 (2)O6ii—Ti5—O4101.5 (2)
O11—Ti1—Ti2143.2 (2)O51—Ti5—O5594.7 (2)
O2—Ti1—Ti242.82 (15)O6ii—Ti5—O5587.3 (2)
O3—Ti1—Ti298.19 (16)O4—Ti5—O55162.7 (2)
O28—Ti1—Ti278.24 (18)O51—Ti5—O4893.3 (2)
O15—Ti1—Ti2119.20 (17)O6ii—Ti5—O48160.6 (2)
O1—Ti1—Ti237.03 (13)O4—Ti5—O4888.2 (2)
O11—Ti1—Ti3139.45 (19)O55—Ti5—O4879.4 (2)
O2—Ti1—Ti398.04 (16)O51—Ti5—O5175.2 (2)
O3—Ti1—Ti343.33 (15)O6ii—Ti5—O577.7 (2)
O28—Ti1—Ti3119.46 (17)O4—Ti5—O577.5 (2)
O15—Ti1—Ti377.37 (16)O55—Ti5—O590.0 (2)
O1—Ti1—Ti336.29 (13)O48—Ti5—O588.3 (2)
Ti2—Ti1—Ti368.24 (5)O51—Ti5—Ti6ii144.11 (19)
O21—Ti2—O3i103.3 (2)O6ii—Ti5—Ti6ii43.40 (15)
O21—Ti2—O197.6 (2)O4—Ti5—Ti6ii97.90 (14)
O3i—Ti2—O1101.8 (2)O55—Ti5—Ti6ii78.14 (16)
O21—Ti2—O38i94.7 (3)O48—Ti5—Ti6ii119.13 (16)
O3i—Ti2—O38i87.4 (2)O5—Ti5—Ti6ii36.57 (14)
O1—Ti2—O38i162.5 (2)O51—Ti5—Ti4139.4 (2)
O21—Ti2—O2592.7 (2)O6ii—Ti5—Ti498.26 (15)
O3i—Ti2—O25159.5 (2)O4—Ti5—Ti443.13 (15)
O1—Ti2—O2588.6 (2)O55—Ti5—Ti4121.35 (17)
O38i—Ti2—O2578.4 (2)O48—Ti5—Ti477.30 (16)
O21—Ti2—O2174.8 (2)O5—Ti5—Ti436.77 (14)
O3i—Ti2—O278.4 (2)Ti6ii—Ti5—Ti468.25 (5)
O1—Ti2—O277.2 (2)O61—Ti6—O4103.5 (2)
O38i—Ti2—O290.2 (2)O61—Ti6—O5ii101.9 (2)
O25—Ti2—O286.8 (2)O4—Ti6—O5ii101.5 (2)
O21—Ti2—Ti3i145.76 (18)O61—Ti6—O58ii91.8 (3)
O3i—Ti2—Ti3i43.57 (15)O4—Ti6—O58ii158.7 (2)
O1—Ti2—Ti3i97.96 (15)O5ii—Ti6—O58ii89.5 (2)
O38i—Ti2—Ti3i78.28 (16)O61—Ti6—O6591.8 (2)
O25—Ti2—Ti3i117.98 (17)O4—Ti6—O6587.8 (2)
O2—Ti2—Ti3i37.15 (13)O5ii—Ti6—O65161.0 (2)
O21—Ti2—Ti1138.73 (19)O58ii—Ti6—O6576.8 (2)
O3i—Ti2—Ti198.54 (16)O61—Ti6—O6178.7 (3)
O1—Ti2—Ti143.23 (15)O4—Ti6—O677.7 (2)
O38i—Ti2—Ti1121.13 (18)O5ii—Ti6—O677.5 (2)
O25—Ti2—Ti176.82 (18)O58ii—Ti6—O687.1 (2)
O2—Ti2—Ti136.22 (13)O65—Ti6—O688.6 (2)
Ti3i—Ti2—Ti168.21 (5)O61—Ti6—Ti5ii142.18 (19)
O31—Ti3—O1102.9 (2)O4—Ti6—Ti5ii98.17 (15)
O31—Ti3—O2i101.3 (2)O5ii—Ti6—Ti5ii42.90 (14)
O1—Ti3—O2i101.4 (2)O58ii—Ti6—Ti5ii77.44 (17)
O31—Ti3—O3592.8 (3)O65—Ti6—Ti5ii119.89 (17)
O1—Ti3—O35159.0 (2)O6—Ti6—Ti5ii36.87 (13)
O2i—Ti3—O3588.9 (2)O61—Ti6—Ti4144.8 (2)
O31—Ti3—O1892.4 (2)O4—Ti6—Ti443.51 (15)
O1—Ti3—O1887.6 (2)O5ii—Ti6—Ti497.90 (16)
O2i—Ti3—O18161.3 (2)O58ii—Ti6—Ti4117.37 (17)
O35—Ti3—O1877.7 (2)O65—Ti6—Ti477.43 (18)
O31—Ti3—O3178.6 (2)O6—Ti6—Ti436.51 (14)
O1—Ti3—O377.8 (2)Ti5ii—Ti6—Ti468.23 (5)
O2i—Ti3—O377.36 (19)Ti6—O4—Ti5135.5 (3)
O35—Ti3—O386.9 (2)Ti6—O4—Ti4100.0 (2)
O18—Ti3—O388.9 (2)Ti5—O4—Ti4100.2 (2)
O31—Ti3—Ti2i142.29 (18)Ti6ii—O5—Ti4134.8 (3)
O1—Ti3—Ti2i97.86 (14)Ti6ii—O5—Ti5100.5 (2)
O2i—Ti3—Ti2i43.27 (16)Ti4—O5—Ti5100.8 (2)
O35—Ti3—Ti2i77.10 (16)Ti4—O6—Ti5ii135.1 (3)
O18—Ti3—Ti2i119.81 (17)Ti4—O6—Ti6100.3 (2)
O3—Ti3—Ti2i36.31 (12)Ti5ii—O6—Ti699.7 (2)
O31—Ti3—Ti1144.0 (2)C42—O41—Ti4162.5 (7)
O1—Ti3—Ti142.96 (15)O41—C42—C44113.2 (10)
O2i—Ti3—Ti197.90 (15)O41—C42—C43109.6 (9)
O35—Ti3—Ti1117.95 (18)C44—C42—C43119.1 (12)
O18—Ti3—Ti177.55 (17)O41—C42—H42A104.4
O3—Ti3—Ti137.06 (12)C44—C42—H42A104.4
Ti2i—Ti3—Ti168.13 (5)C43—C42—H42A104.4
Ti3—O1—Ti2135.2 (3)C42—C43—H43A109.5
Ti3—O1—Ti1100.7 (2)C42—C43—H43B109.5
Ti2—O1—Ti199.7 (2)H43A—C43—H43B109.5
Ti1—O2—Ti3i134.9 (3)C42—C43—H43C109.5
Ti1—O2—Ti2101.0 (2)H43A—C43—H43C109.5
Ti3i—O2—Ti299.6 (2)H43B—C43—H43C109.5
Ti2i—O3—Ti1134.9 (3)C42—C44—H44A109.5
Ti2i—O3—Ti3100.1 (2)C42—C44—H44B109.5
Ti1—O3—Ti399.6 (2)H44A—C44—H44B109.5
C12—O11—Ti1157.2 (6)C42—C44—H44C109.5
O11—C12—C14112.5 (9)H44A—C44—H44C109.5
O11—C12—C13109.3 (8)H44B—C44—H44C109.5
C14—C12—C13112.2 (9)C46—O45—Ti4130.6 (6)
O11—C12—H12A107.5O48—C46—O45124.0 (9)
C14—C12—H12A107.5O48—C46—C47117.9 (9)
C13—C12—H12A107.5O45—C46—C47118.1 (9)
C12—C13—H13A109.5C46—C47—H47A109.5
C12—C13—H13B109.5C46—C47—H47B109.5
H13A—C13—H13B109.5H47A—C47—H47B109.5
C12—C13—H13C109.5C46—C47—H47C109.5
H13A—C13—H13C109.5H47A—C47—H47C109.5
H13B—C13—H13C109.5H47B—C47—H47C109.5
C12—C14—H14A109.5C46—O48—Ti5130.3 (6)
C12—C14—H14B109.5C52—O51—Ti5153.3 (8)
H14A—C14—H14B109.5O51—C52—C53B120.7 (15)
C12—C14—H14C109.5O51—C52—C54B117.7 (15)
H14A—C14—H14C109.5C53B—C52—C54B119.5 (18)
H14B—C14—H14C109.5O51—C52—C54A118.4 (19)
C16—O15—Ti1130.1 (6)C53B—C52—C54A90 (2)
O18—C16—O15123.4 (8)C54B—C52—C54A76 (2)
O18—C16—C17119.4 (9)O51—C52—C53A104.4 (17)
O15—C16—C17117.2 (9)C53B—C52—C53A95 (2)
C16—C17—H17A109.5C54B—C52—C53A55.4 (17)
C16—C17—H17B109.5C54A—C52—C53A127 (2)
H17A—C17—H17B109.5O51—C52—H52A100.9
C16—C17—H17C109.5C53B—C52—H52A19.8
H17A—C17—H17C109.5C54B—C52—H52A137.8
H17B—C17—H17C109.5C54A—C52—H52A100.9
C16—O18—Ti3130.9 (6)C53A—C52—H52A100.9
C22—O21—Ti2154.5 (6)O51—C52—H52B94.4
C24—C22—O21114.8 (12)C53B—C52—H52B101.9
C24—C22—C23115.5 (12)C54B—C52—H52B88.2
O21—C22—C23110.5 (10)C54A—C52—H52B24.1
C24—C22—H22A104.9C53A—C52—H52B143.5
O21—C22—H22A104.9H52A—C52—H52B106.0
C23—C22—H22A104.9C52—C53A—H53A109.5
C22—C23—H23A109.5C52—C53A—H53B109.5
C22—C23—H23B109.5H53A—C53A—H53B109.5
H23A—C23—H23B109.5C52—C53A—H53C109.5
C22—C23—H23C109.5H53A—C53A—H53C109.5
H23A—C23—H23C109.5H53B—C53A—H53C109.5
H23B—C23—H23C109.5C52—C54A—H52B38.4
C22—C24—H24A109.5C52—C54A—H54A109.5
C22—C24—H24B109.5H52B—C54A—H54A80.8
H24A—C24—H24B109.5C52—C54A—H54B109.5
C22—C24—H24C109.5H52B—C54A—H54B145.6
H24A—C24—H24C109.5H54A—C54A—H54B109.5
H24B—C24—H24C109.5C52—C54A—H54C109.5
C26—O25—Ti2130.3 (6)H52B—C54A—H54C96.8
O28—C26—O25124.7 (8)H54A—C54A—H54C109.5
O28—C26—C27118.9 (9)H54B—C54A—H54C109.5
O25—C26—C27116.4 (9)C52—C53B—H53D109.5
C26—C27—H27A109.5C52—C53B—H53E109.5
C26—C27—H27B109.5H53D—C53B—H53E109.5
H27A—C27—H27B109.5C52—C53B—H53F109.5
C26—C27—H27C109.5H53D—C53B—H53F109.5
H27A—C27—H27C109.5H53E—C53B—H53F109.5
H27B—C27—H27C109.5C52—C54B—H54D109.5
C26—O28—Ti1129.8 (6)C52—C54B—H54E109.5
C32—O31—Ti3155.3 (7)H54D—C54B—H54E109.5
C34—C32—O31118.7 (11)C52—C54B—H54F109.5
C34—C32—C33123.2 (11)H54D—C54B—H54F109.5
O31—C32—C33111.3 (10)H54E—C54B—H54F109.5
C34—C32—H32A98.7C56—O55—Ti5129.2 (6)
O31—C32—H32A98.7O55—C56—O58124.6 (10)
C33—C32—H32A98.7O55—C56—C57119.0 (9)
C32—C33—H33A109.5O58—C56—C57116.4 (9)
C32—C33—H33B109.5C56—C57—H57A109.5
H33A—C33—H33B109.5C56—C57—H57B109.5
C32—C33—H33C109.5H57A—C57—H57B109.5
H33A—C33—H33C109.5C56—C57—H57C109.5
H33B—C33—H33C109.5H57A—C57—H57C109.5
C32—C34—H34A109.5H57B—C57—H57C109.5
C32—C34—H34B109.5C56—O58—Ti6ii129.7 (6)
H34A—C34—H34B109.5C62—O61—Ti6144.9 (8)
C32—C34—H34C109.5C64—C62—C63124.8 (15)
H34A—C34—H34C109.5C64—C62—O61116.7 (14)
H34B—C34—H34C109.5C63—C62—O61115.9 (14)
C36—O35—Ti3130.3 (6)C64—C62—H62A95.4
O38—C36—O35124.1 (9)C63—C62—H62A95.4
O38—C36—C37118.8 (9)O61—C62—H62A95.4
O35—C36—C37117.1 (9)C62—C63—H63A109.5
C36—C37—H37A109.5C62—C63—H63B109.5
C36—C37—H37B109.5H63A—C63—H63B109.5
H37A—C37—H37B109.5C62—C63—H63C109.5
C36—C37—H37C109.5H63A—C63—H63C109.5
H37A—C37—H37C109.5H63B—C63—H63C109.5
H37B—C37—H37C109.5C62—C64—H64A109.5
C36—O38—Ti2i129.7 (6)C62—C64—H64B109.5
O41—Ti4—O6101.4 (2)H64A—C64—H64B109.5
O41—Ti4—O599.6 (2)C62—C64—H64C109.5
O6—Ti4—O5101.5 (2)H64A—C64—H64C109.5
O41—Ti4—O4594.8 (2)H64B—C64—H64C109.5
O6—Ti4—O45158.9 (2)C66—O65—Ti6128.7 (6)
O5—Ti4—O4588.8 (2)O68—C66—O65126.3 (9)
O41—Ti4—O6894.6 (2)O68—C66—C67117.4 (10)
O6—Ti4—O6887.8 (2)O65—C66—C67116.2 (10)
O5—Ti4—O68161.0 (2)C66—C67—H67A109.5
O45—Ti4—O6877.4 (3)C66—C67—H67B109.5
O41—Ti4—O4175.8 (2)H67A—C67—H67B109.5
O6—Ti4—O477.4 (2)C66—C67—H67C109.5
O5—Ti4—O476.7 (2)H67A—C67—H67C109.5
O45—Ti4—O487.3 (2)H67B—C67—H67C109.5
O68—Ti4—O489.4 (2)C66—O68—Ti4128.6 (6)
O41—Ti4—Ti6143.4 (2)
Symmetry codes: (i) x+1, y+1, z; (ii) x+2, y+2, z+1.
 

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