Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805021276/cf6434sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536805021276/cf6434Isup2.hkl |
CCDC reference: 282262
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.009 Å
- H-atom completeness 53%
- Disorder in solvent or counterion
- R factor = 0.063
- wR factor = 0.170
- Data-to-parameter ratio = 12.6
checkCIF/PLATON results
No syntax errors found
Alert level A PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) ....... O11W
Author Response: We did not find any H-atom for water oxygen O11W. |
Alert level B PLAT220_ALERT_2_B Large Non-Solvent O Ueq(max)/Ueq(min) ... 3.71 Ratio PLAT430_ALERT_2_B Short Inter D...A Contact O7W .. O10A .. 2.83 Ang. PLAT430_ALERT_2_B Short Inter D...A Contact O9W .. O11W .. 2.76 Ang.
Alert level C CHEMW01_ALERT_1_C The ratio of given/expected molecular weight as calculated from the _chemical_formula_sum lies outside the range 0.99 <> 1.01 Calculated formula weight = 1202.5671 Formula weight given = 1180.3700 CHEMW01_ALERT_1_C The difference between the given and expected weight for compound is greater 1 mass unit. Check that all hydrogen atoms have been taken into account. PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.25 PLAT199_ALERT_1_C Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_C Check the Reported _diffrn_ambient_temperature . 293 K PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 33.00 Perc. PLAT311_ALERT_2_C Isolated Disordered Oxygen Atom (No H's ?) ..... >O10B PLAT311_ALERT_2_C Isolated Disordered Oxygen Atom (No H's ?) ..... <O10A PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 9 PLAT430_ALERT_2_C Short Inter D...A Contact O7W .. O10B .. 2.86 Ang. PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 2
Alert level G FORMU01_ALERT_1_G There is a discrepancy between the atom counts in the _chemical_formula_sum and _chemical_formula_moiety. This is usually due to the moiety formula being in the wrong format. Atom count from _chemical_formula_sum: C42 H46 Na4 O29 Ti2 Atom count from _chemical_formula_moiety:C42 H24 Na4 O18 Ti2 FORMU01_ALERT_2_G There is a discrepancy between the atom counts in the _chemical_formula_sum and the formula from the _atom_site* data. Atom count from _chemical_formula_sum:C42 H46 Na4 O29 Ti2 Atom count from the _atom_site data: C42 H24 Na4 O29 Ti2 CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected. CELLZ01_ALERT_1_G WARNING: H atoms missing from atom site list. Is this intentional? From the CIF: _cell_formula_units_Z 4 From the CIF: _chemical_formula_sum C42 H46 Na4 O29 Ti2 TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff C 168.00 168.00 0.00 H 184.00 96.00 88.00 Na 16.00 16.00 0.00 O 116.00 116.00 0.00 Ti 8.00 8.00 0.00
1 ALERT level A = In general: serious problem 3 ALERT level B = Potentially serious problem 13 ALERT level C = Check and explain 4 ALERT level G = General alerts; check 9 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 9 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 2 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: XDS (Kabsch, 1988); cell refinement: XDS; data reduction: XDS; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997; program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 2005); software used to prepare material for publication: PLATON (Spek, 2003).
Na4[Ti(C7H4O3)3]2·11H2O | F(000) = 2384 |
Mr = 1180.37 | Dx = 1.555 Mg m−3 Dm = 1.60 Mg m−3 Dm measured by flotation in benzene/bromoform |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 25 reflections |
a = 17.572 (3) Å | θ = 2.2–25.0° |
b = 9.588 (5) Å | µ = 0.45 mm−1 |
c = 30.126 (3) Å | T = 293 K |
β = 96.60 (2)° | Rhombic, yellow |
V = 5042 (3) Å3 | 0.25 × 0.20 × 0.15 mm |
Z = 4 |
Enraf–Nonius CAD-4 diffractometer | Rint = 0.030 |
Radiation source: fine-focus sealed tube | θmax = 25.0°, θmin = 2.2° |
Graphite monochromator | h = −20→20 |
ω–2θ scans | k = 0→11 |
9046 measured reflections | l = 0→35 |
8865 independent reflections | 3 standard reflections every 120 min |
4399 reflections with I > 2σ(I) | intensity decay: none |
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)] = 0.063 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.170 | H-atom parameters constrained |
S = 0.93 | w = 1/[σ2(Fo2) + (0.083P)2] where P = (Fo2 + 2Fc2)/3 |
8865 reflections | (Δ/σ)max < 0.001 |
706 parameters | Δρmax = 0.85 e Å−3 |
30 restraints | Δρmin = −0.38 e Å−3 |
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) | |
TiA | 0.18895 (5) | 0.54240 (11) | 0.39115 (3) | 0.0263 (3) | |
TiB | −0.19990 (5) | 0.53002 (11) | 0.10507 (3) | 0.0247 (2) | |
Na1 | −0.16491 (12) | 0.5293 (2) | 0.28684 (7) | 0.0359 (5) | |
Na2 | 0.30317 (13) | 0.1739 (3) | 0.23632 (7) | 0.0386 (6) | |
Na3 | 0.13705 (13) | 0.2949 (3) | 0.28485 (8) | 0.0463 (7) | |
Na4 | −0.16003 (15) | 0.8723 (3) | 0.24697 (8) | 0.0511 (7) | |
O1A | 0.1450 (2) | 0.4162 (4) | 0.42682 (12) | 0.0336 (10) | |
O2A | 0.08239 (19) | 0.5402 (4) | 0.35334 (12) | 0.0335 (9) | |
O4A | 0.2068 (2) | 0.6886 (4) | 0.34463 (11) | 0.0338 (10) | |
O3A | 0.1748 (2) | 0.6957 (4) | 0.42763 (11) | 0.0302 (9) | |
O6A | 0.2173 (2) | 0.4080 (4) | 0.34447 (12) | 0.0354 (10) | |
O5A | 0.29180 (19) | 0.5235 (4) | 0.41497 (12) | 0.0343 (10) | |
O7A | −0.0385 (2) | 0.4880 (4) | 0.33163 (13) | 0.0412 (11) | |
O8A | 0.2173 (2) | 0.8877 (5) | 0.31055 (13) | 0.0467 (12) | |
O9A | 0.2806 (2) | 0.2855 (5) | 0.29957 (13) | 0.0458 (11) | |
C1A | 0.0725 (3) | 0.3979 (6) | 0.43678 (18) | 0.0311 (13) | |
C2A | 0.0606 (4) | 0.3414 (7) | 0.4777 (2) | 0.0428 (16) | |
H2A | 0.1025 | 0.3131 | 0.4974 | 0.051* | |
C3A | −0.0127 (4) | 0.3264 (7) | 0.4899 (2) | 0.0500 (18) | |
H3A | −0.0197 | 0.2902 | 0.5177 | 0.060* | |
C4A | −0.0752 (4) | 0.3652 (7) | 0.4605 (2) | 0.0540 (19) | |
H4A | −0.1245 | 0.3566 | 0.4686 | 0.065* | |
C5A | −0.0642 (4) | 0.4159 (7) | 0.4200 (2) | 0.0459 (17) | |
H5A | −0.1068 | 0.4387 | 0.4000 | 0.055* | |
C6A | 0.0085 (3) | 0.4355 (6) | 0.40674 (19) | 0.0345 (14) | |
C7A | 0.0175 (3) | 0.4893 (6) | 0.36133 (18) | 0.0309 (14) | |
C14A | 0.2146 (3) | 0.8231 (7) | 0.34586 (18) | 0.0323 (14) | |
C13A | 0.2202 (3) | 0.8949 (6) | 0.38907 (18) | 0.0274 (13) | |
C12A | 0.2430 (3) | 1.0348 (7) | 0.3920 (2) | 0.0398 (15) | |
H12A | 0.2552 | 1.0799 | 0.3664 | 0.048* | |
C11A | 0.2477 (4) | 1.1074 (7) | 0.4316 (2) | 0.0449 (17) | |
H11A | 0.2631 | 1.2003 | 0.4328 | 0.054* | |
C10A | 0.2293 (3) | 1.0404 (7) | 0.4694 (2) | 0.0440 (16) | |
H10A | 0.2325 | 1.0889 | 0.4962 | 0.053* | |
C9A | 0.2061 (3) | 0.9031 (6) | 0.46809 (19) | 0.0299 (13) | |
H9A | 0.1941 | 0.8597 | 0.4940 | 0.036* | |
C8A | 0.2008 (3) | 0.8291 (6) | 0.42804 (17) | 0.0256 (13) | |
C21A | 0.2813 (3) | 0.3562 (6) | 0.33387 (19) | 0.0320 (14) | |
C20A | 0.3530 (3) | 0.3799 (6) | 0.36400 (18) | 0.0313 (14) | |
C19A | 0.4208 (3) | 0.3164 (7) | 0.3536 (2) | 0.0468 (17) | |
H19A | 0.4201 | 0.2589 | 0.3287 | 0.056* | |
C18A | 0.4891 (4) | 0.3401 (8) | 0.3808 (3) | 0.059 (2) | |
H18A | 0.5342 | 0.2998 | 0.3737 | 0.071* | |
C17A | 0.4904 (4) | 0.4222 (8) | 0.4181 (2) | 0.058 (2) | |
H17A | 0.5362 | 0.4365 | 0.4362 | 0.069* | |
C16A | 0.4243 (3) | 0.4833 (7) | 0.4286 (2) | 0.0439 (17) | |
H16A | 0.4260 | 0.5398 | 0.4538 | 0.053* | |
C15A | 0.3556 (3) | 0.4630 (6) | 0.40276 (18) | 0.0314 (13) | |
O2B | −0.2350 (2) | 0.3895 (4) | 0.14944 (12) | 0.0304 (9) | |
O1B | −0.29985 (18) | 0.5124 (4) | 0.07624 (12) | 0.0333 (10) | |
O3B | −0.1767 (2) | 0.6814 (4) | 0.07020 (11) | 0.0298 (9) | |
O4B | −0.2268 (2) | 0.6763 (4) | 0.14936 (12) | 0.0328 (9) | |
O5B | −0.1517 (2) | 0.4056 (4) | 0.07074 (12) | 0.0297 (9) | |
O6B | −0.10039 (19) | 0.5237 (4) | 0.14735 (11) | 0.0292 (9) | |
O7B | −0.3075 (2) | 0.2559 (4) | 0.18693 (13) | 0.0366 (10) | |
O8B | −0.2469 (2) | 0.8781 (4) | 0.18091 (13) | 0.0420 (11) | |
O9B | 0.0162 (2) | 0.4631 (6) | 0.17464 (14) | 0.0622 (15) | |
C7B | −0.3007 (3) | 0.3365 (6) | 0.15548 (17) | 0.0256 (12) | |
C6B | −0.3700 (3) | 0.3769 (6) | 0.12475 (18) | 0.0273 (13) | |
C5B | −0.4416 (3) | 0.3287 (6) | 0.1336 (2) | 0.0374 (15) | |
H5B | −0.4446 | 0.2683 | 0.1575 | 0.045* | |
C4B | −0.5072 (3) | 0.3674 (7) | 0.1082 (2) | 0.0481 (18) | |
H4B | −0.5544 | 0.3350 | 0.1150 | 0.058* | |
C3B | −0.5032 (3) | 0.4567 (7) | 0.0716 (2) | 0.0456 (17) | |
H3B | −0.5479 | 0.4860 | 0.0546 | 0.055* | |
C2B | −0.4329 (3) | 0.5008 (6) | 0.0608 (2) | 0.0399 (16) | |
H2B | −0.4300 | 0.5571 | 0.0359 | 0.048* | |
C1B | −0.3666 (3) | 0.4615 (6) | 0.08708 (17) | 0.0274 (12) | |
C14B | −0.2326 (3) | 0.8111 (6) | 0.14769 (17) | 0.0288 (13) | |
C13B | −0.2218 (3) | 0.8850 (6) | 0.10549 (18) | 0.0276 (13) | |
C8B | −0.1977 (3) | 0.8158 (6) | 0.06870 (16) | 0.0242 (12) | |
C9B | −0.1954 (3) | 0.8897 (6) | 0.02876 (18) | 0.0322 (14) | |
H9B | −0.1814 | 0.8435 | 0.0038 | 0.039* | |
C10B | −0.2134 (4) | 1.0294 (7) | 0.0257 (2) | 0.0443 (16) | |
H10B | −0.2118 | 1.0769 | −0.0011 | 0.053* | |
C11B | −0.2338 (4) | 1.0986 (7) | 0.0629 (2) | 0.0475 (17) | |
H11B | −0.2443 | 1.1937 | 0.0614 | 0.057* | |
C12B | −0.2387 (4) | 1.0267 (7) | 0.1022 (2) | 0.0417 (16) | |
H12B | −0.2535 | 1.0736 | 0.1268 | 0.050* | |
C21B | −0.0343 (3) | 0.4717 (7) | 0.14229 (18) | 0.0337 (14) | |
C20B | −0.0182 (3) | 0.4250 (6) | 0.09775 (18) | 0.0337 (14) | |
C15B | −0.0775 (3) | 0.3896 (6) | 0.06392 (18) | 0.0308 (13) | |
C16B | −0.0587 (4) | 0.3392 (7) | 0.0234 (2) | 0.0433 (16) | |
H16B | −0.0975 | 0.3130 | 0.0014 | 0.052* | |
C17B | 0.0163 (4) | 0.3274 (7) | 0.0153 (2) | 0.0526 (19) | |
H17B | 0.0283 | 0.2948 | −0.0122 | 0.063* | |
C18B | 0.0742 (4) | 0.3647 (8) | 0.0485 (2) | 0.057 (2) | |
H18B | 0.1250 | 0.3598 | 0.0427 | 0.069* | |
C19B | 0.0583 (3) | 0.4078 (8) | 0.0889 (2) | 0.0506 (19) | |
H19B | 0.0982 | 0.4264 | 0.1112 | 0.061* | |
O1W | 0.1570 (2) | 0.4647 (4) | 0.22722 (13) | 0.0416 (10) | |
O2W | 0.4414 (2) | 0.2163 (5) | 0.22657 (14) | 0.0485 (12) | |
O3W | 0.0075 (2) | 0.3553 (5) | 0.25771 (14) | 0.0561 (13) | |
O4W | −0.1514 (2) | 0.3234 (4) | 0.23677 (13) | 0.0441 (11) | |
O5W | −0.2773 (2) | 0.5801 (4) | 0.23243 (12) | 0.0359 (10) | |
O6W | −0.0946 (2) | 0.6620 (4) | 0.23287 (13) | 0.0377 (10) | |
O7W | 0.1683 (2) | 0.0975 (5) | 0.23980 (16) | 0.0560 (13) | |
O8W | −0.0321 (4) | 0.9879 (7) | 0.2588 (2) | 0.108 (2) | |
O9W | 0.0853 (4) | 0.1635 (7) | 0.3406 (2) | 0.106 (2) | |
O10A | 0.065 (2) | 0.173 (4) | 0.1648 (12) | 0.064 (11) | 0.26 (5) |
O10B | 0.0317 (13) | 0.1370 (15) | 0.1796 (6) | 0.094 (5) | 0.74 (5) |
O11W | −0.0724 (4) | 0.1780 (8) | 0.3346 (2) | 0.127 (3) |
U11 | U22 | U33 | U12 | U13 | U23 | |
TiA | 0.0264 (5) | 0.0297 (6) | 0.0226 (5) | 0.0009 (5) | 0.0028 (4) | −0.0015 (5) |
TiB | 0.0228 (5) | 0.0284 (6) | 0.0232 (5) | 0.0008 (5) | 0.0034 (4) | 0.0002 (5) |
Na1 | 0.0406 (12) | 0.0303 (13) | 0.0370 (13) | −0.0004 (11) | 0.0055 (10) | −0.0033 (11) |
Na2 | 0.0472 (14) | 0.0427 (15) | 0.0271 (12) | 0.0082 (12) | 0.0089 (10) | 0.0031 (11) |
Na3 | 0.0372 (13) | 0.0520 (17) | 0.0486 (15) | 0.0012 (12) | 0.0007 (11) | −0.0015 (13) |
Na4 | 0.0628 (16) | 0.0535 (18) | 0.0369 (14) | 0.0184 (14) | 0.0052 (12) | −0.0014 (13) |
O1A | 0.039 (2) | 0.031 (2) | 0.032 (2) | 0.0000 (19) | 0.0064 (18) | 0.0065 (18) |
O2A | 0.027 (2) | 0.042 (3) | 0.031 (2) | −0.003 (2) | 0.0014 (16) | 0.002 (2) |
O4A | 0.045 (2) | 0.036 (3) | 0.021 (2) | −0.006 (2) | 0.0068 (17) | −0.0031 (19) |
O3A | 0.033 (2) | 0.036 (3) | 0.023 (2) | −0.0009 (18) | 0.0069 (16) | 0.0023 (18) |
O6A | 0.032 (2) | 0.040 (3) | 0.034 (2) | 0.0047 (19) | 0.0027 (18) | −0.011 (2) |
O5A | 0.0239 (19) | 0.047 (3) | 0.031 (2) | 0.0038 (19) | −0.0002 (16) | −0.005 (2) |
O7A | 0.031 (2) | 0.055 (3) | 0.036 (2) | 0.000 (2) | −0.0025 (18) | −0.003 (2) |
O8A | 0.068 (3) | 0.047 (3) | 0.026 (2) | −0.010 (2) | 0.007 (2) | 0.010 (2) |
O9A | 0.046 (3) | 0.053 (3) | 0.038 (2) | 0.003 (2) | 0.006 (2) | −0.017 (2) |
C1A | 0.038 (3) | 0.024 (3) | 0.032 (3) | −0.003 (3) | 0.009 (3) | −0.003 (3) |
C2A | 0.054 (4) | 0.039 (4) | 0.036 (4) | −0.003 (3) | 0.009 (3) | 0.003 (3) |
C3A | 0.069 (5) | 0.048 (5) | 0.036 (4) | −0.012 (4) | 0.017 (4) | −0.001 (4) |
C4A | 0.052 (4) | 0.054 (5) | 0.061 (5) | −0.020 (4) | 0.030 (4) | −0.004 (4) |
C5A | 0.042 (4) | 0.051 (4) | 0.047 (4) | −0.002 (3) | 0.013 (3) | −0.002 (3) |
C6A | 0.038 (3) | 0.033 (4) | 0.033 (3) | −0.006 (3) | 0.007 (3) | −0.006 (3) |
C7A | 0.032 (3) | 0.030 (4) | 0.030 (3) | −0.001 (3) | 0.000 (2) | −0.005 (3) |
C14A | 0.032 (3) | 0.037 (4) | 0.029 (3) | −0.007 (3) | 0.010 (3) | −0.004 (3) |
C13A | 0.030 (3) | 0.023 (3) | 0.029 (3) | 0.004 (3) | 0.004 (2) | 0.003 (3) |
C12A | 0.049 (4) | 0.037 (4) | 0.033 (3) | −0.005 (3) | 0.004 (3) | 0.004 (3) |
C11A | 0.057 (4) | 0.024 (4) | 0.051 (4) | −0.003 (3) | −0.001 (3) | −0.001 (3) |
C10A | 0.046 (4) | 0.045 (4) | 0.039 (4) | 0.008 (3) | −0.001 (3) | −0.009 (4) |
C9A | 0.033 (3) | 0.028 (3) | 0.028 (3) | 0.005 (3) | 0.000 (2) | −0.002 (3) |
C8A | 0.020 (3) | 0.027 (3) | 0.030 (3) | 0.002 (2) | 0.005 (2) | −0.003 (3) |
C21A | 0.037 (3) | 0.026 (3) | 0.033 (3) | −0.001 (3) | 0.004 (3) | −0.001 (3) |
C20A | 0.038 (3) | 0.030 (4) | 0.027 (3) | 0.004 (3) | 0.010 (3) | 0.009 (3) |
C19A | 0.040 (4) | 0.051 (4) | 0.049 (4) | 0.008 (3) | 0.007 (3) | −0.014 (4) |
C18A | 0.040 (4) | 0.057 (5) | 0.079 (5) | 0.015 (4) | 0.003 (4) | −0.004 (4) |
C17A | 0.034 (4) | 0.066 (5) | 0.070 (5) | 0.012 (4) | −0.008 (3) | −0.004 (4) |
C16A | 0.035 (3) | 0.056 (5) | 0.038 (3) | 0.004 (3) | −0.004 (3) | −0.016 (3) |
C15A | 0.031 (3) | 0.033 (3) | 0.029 (3) | 0.005 (3) | −0.002 (2) | 0.000 (3) |
O2B | 0.026 (2) | 0.038 (2) | 0.027 (2) | 0.0015 (18) | 0.0016 (16) | 0.0087 (19) |
O1B | 0.0196 (18) | 0.051 (3) | 0.029 (2) | −0.0001 (18) | 0.0014 (15) | 0.0122 (19) |
O3B | 0.036 (2) | 0.028 (2) | 0.027 (2) | 0.0011 (18) | 0.0105 (17) | 0.0032 (18) |
O4B | 0.046 (2) | 0.027 (2) | 0.026 (2) | 0.007 (2) | 0.0110 (18) | 0.0020 (19) |
O5B | 0.027 (2) | 0.031 (2) | 0.032 (2) | −0.0006 (17) | 0.0045 (16) | −0.0058 (18) |
O6B | 0.0242 (19) | 0.037 (2) | 0.0258 (19) | 0.0030 (18) | 0.0020 (15) | −0.0064 (18) |
O7B | 0.040 (2) | 0.035 (2) | 0.035 (2) | −0.0057 (19) | 0.0068 (18) | 0.011 (2) |
O8B | 0.064 (3) | 0.035 (3) | 0.029 (2) | 0.012 (2) | 0.015 (2) | −0.002 (2) |
O9B | 0.038 (2) | 0.110 (4) | 0.035 (2) | 0.021 (3) | −0.010 (2) | −0.006 (3) |
C7B | 0.029 (3) | 0.022 (3) | 0.027 (3) | −0.001 (2) | 0.004 (2) | 0.001 (3) |
C6B | 0.027 (3) | 0.025 (3) | 0.030 (3) | −0.001 (2) | 0.004 (2) | −0.001 (3) |
C5B | 0.035 (3) | 0.034 (4) | 0.042 (4) | −0.003 (3) | 0.002 (3) | 0.005 (3) |
C4B | 0.021 (3) | 0.062 (5) | 0.061 (4) | −0.012 (3) | 0.004 (3) | −0.005 (4) |
C3B | 0.024 (3) | 0.057 (5) | 0.054 (4) | 0.002 (3) | −0.007 (3) | 0.006 (4) |
C2B | 0.033 (3) | 0.051 (5) | 0.034 (3) | −0.001 (3) | −0.007 (3) | 0.009 (3) |
C1B | 0.027 (3) | 0.031 (3) | 0.024 (3) | −0.003 (3) | 0.003 (2) | 0.000 (3) |
C14B | 0.030 (3) | 0.034 (4) | 0.022 (3) | 0.001 (3) | 0.004 (2) | −0.003 (3) |
C13B | 0.033 (3) | 0.024 (3) | 0.026 (3) | −0.002 (3) | 0.005 (2) | −0.004 (3) |
C8B | 0.019 (3) | 0.033 (4) | 0.021 (3) | −0.001 (2) | 0.001 (2) | −0.002 (3) |
C9B | 0.036 (3) | 0.037 (4) | 0.024 (3) | −0.010 (3) | 0.006 (2) | −0.003 (3) |
C10B | 0.063 (4) | 0.035 (4) | 0.034 (3) | −0.011 (4) | 0.003 (3) | 0.006 (3) |
C11B | 0.064 (4) | 0.028 (4) | 0.049 (4) | 0.003 (3) | 0.004 (3) | −0.005 (3) |
C12B | 0.065 (4) | 0.028 (4) | 0.034 (3) | 0.001 (3) | 0.012 (3) | −0.001 (3) |
C21B | 0.034 (3) | 0.038 (4) | 0.028 (3) | −0.002 (3) | 0.003 (3) | 0.002 (3) |
C20B | 0.032 (3) | 0.040 (4) | 0.030 (3) | 0.002 (3) | 0.004 (2) | −0.001 (3) |
C15B | 0.026 (3) | 0.032 (4) | 0.034 (3) | 0.003 (3) | 0.005 (2) | −0.001 (3) |
C16B | 0.049 (4) | 0.049 (4) | 0.032 (3) | 0.001 (3) | 0.006 (3) | −0.006 (3) |
C17B | 0.056 (4) | 0.050 (5) | 0.057 (4) | 0.009 (4) | 0.031 (4) | −0.005 (4) |
C18B | 0.030 (3) | 0.073 (6) | 0.072 (5) | −0.001 (4) | 0.025 (4) | −0.010 (4) |
C19B | 0.027 (3) | 0.073 (5) | 0.052 (4) | 0.008 (3) | 0.003 (3) | −0.020 (4) |
O1W | 0.043 (2) | 0.036 (2) | 0.045 (2) | −0.001 (2) | −0.0009 (19) | −0.003 (2) |
O2W | 0.030 (2) | 0.069 (3) | 0.046 (3) | 0.003 (2) | 0.0001 (19) | 0.001 (2) |
O3W | 0.039 (2) | 0.075 (4) | 0.056 (3) | 0.003 (3) | 0.009 (2) | −0.001 (3) |
O4W | 0.046 (3) | 0.041 (3) | 0.044 (2) | −0.004 (2) | −0.002 (2) | 0.000 (2) |
O5W | 0.047 (2) | 0.027 (2) | 0.034 (2) | −0.0036 (19) | 0.0068 (18) | 0.0018 (18) |
O6W | 0.031 (2) | 0.043 (3) | 0.039 (2) | 0.0030 (19) | 0.0049 (18) | −0.006 (2) |
O7W | 0.048 (3) | 0.052 (3) | 0.069 (3) | 0.004 (2) | 0.010 (2) | −0.006 (3) |
O8W | 0.108 (4) | 0.086 (5) | 0.135 (5) | −0.026 (4) | 0.037 (4) | −0.026 (4) |
O9W | 0.109 (5) | 0.096 (5) | 0.116 (5) | 0.008 (4) | 0.028 (4) | 0.032 (4) |
O10A | 0.062 (14) | 0.058 (13) | 0.068 (13) | 0.019 (8) | −0.005 (8) | −0.009 (8) |
O10B | 0.103 (9) | 0.080 (7) | 0.094 (7) | 0.013 (6) | −0.009 (6) | −0.008 (5) |
O11W | 0.119 (5) | 0.132 (6) | 0.127 (5) | −0.016 (5) | 0.009 (4) | 0.005 (5) |
TiA—O1A | 1.846 (4) | C10A—C9A | 1.377 (8) |
TiA—O3A | 1.869 (4) | C10A—H10A | 0.930 |
TiA—O5A | 1.875 (4) | C9A—C8A | 1.394 (7) |
TiA—O6A | 2.011 (4) | C9A—H9A | 0.930 |
TiA—O4A | 2.032 (4) | C21A—C20A | 1.484 (8) |
TiA—O2A | 2.077 (4) | C20A—C19A | 1.406 (8) |
TiB—O5B | 1.847 (4) | C20A—C15A | 1.410 (8) |
TiB—O3B | 1.864 (4) | C19A—C18A | 1.392 (9) |
TiB—O1B | 1.875 (3) | C19A—H19A | 0.930 |
TiB—O4B | 2.029 (4) | C18A—C17A | 1.368 (10) |
TiB—O6B | 2.042 (3) | C18A—H18A | 0.930 |
TiB—O2B | 2.042 (4) | C17A—C16A | 1.371 (8) |
Na1—O7Bi | 2.381 (5) | C17A—H17A | 0.930 |
Na1—O8Bii | 2.407 (4) | C16A—C15A | 1.373 (7) |
Na1—O5W | 2.466 (4) | C16A—H16A | 0.930 |
Na1—O7A | 2.494 (4) | O2B—C7B | 1.293 (6) |
Na1—O6W | 2.500 (4) | O1B—C1B | 1.345 (6) |
Na1—O4W | 2.512 (5) | O3B—C8B | 1.340 (6) |
Na2—O9A | 2.260 (4) | O4B—C14B | 1.296 (7) |
Na2—O1Wiii | 2.354 (5) | O5B—C15B | 1.352 (6) |
Na2—O4Aiii | 2.429 (4) | O6B—C21B | 1.290 (6) |
Na2—O8Aiii | 2.492 (5) | O7B—C7B | 1.239 (6) |
Na2—O7W | 2.494 (5) | O7B—Na1ii | 2.381 (5) |
Na2—O2W | 2.513 (5) | O7B—Na4ii | 2.408 (5) |
Na3—O9W | 2.364 (6) | O8B—C14B | 1.239 (6) |
Na3—O3W | 2.400 (5) | O8B—Na1i | 2.407 (4) |
Na3—O6A | 2.410 (4) | O9B—C21B | 1.242 (6) |
Na3—O7W | 2.428 (5) | C7B—C6B | 1.494 (7) |
Na3—O1W | 2.435 (5) | C6B—C5B | 1.395 (7) |
Na3—O9A | 2.512 (5) | C6B—C1B | 1.402 (7) |
Na4—O8B | 2.366 (5) | C5B—C4B | 1.360 (8) |
Na4—O6W | 2.383 (5) | C5B—H5B | 0.930 |
Na4—O5Wi | 2.392 (5) | C4B—C3B | 1.404 (9) |
Na4—O7Bi | 2.408 (5) | C4B—H4B | 0.930 |
Na4—O8W | 2.495 (7) | C3B—C2B | 1.379 (8) |
O1A—C1A | 1.353 (6) | C3B—H3B | 0.930 |
O2A—C7A | 1.288 (6) | C2B—C1B | 1.383 (7) |
O4A—C14A | 1.297 (7) | C2B—H2B | 0.930 |
O4A—Na2iv | 2.429 (4) | C14B—C13B | 1.487 (7) |
O3A—C8A | 1.358 (6) | C13B—C12B | 1.392 (8) |
O6A—C21A | 1.302 (6) | C13B—C8B | 1.398 (7) |
O5A—C15A | 1.349 (6) | C8B—C9B | 1.401 (7) |
O7A—C7A | 1.252 (6) | C9B—C10B | 1.377 (8) |
O8A—C14A | 1.237 (6) | C9B—H9B | 0.930 |
O8A—Na2iv | 2.492 (5) | C10B—C11B | 1.384 (8) |
O9A—C21A | 1.235 (6) | C10B—H10B | 0.930 |
C1A—C2A | 1.384 (8) | C11B—C12B | 1.381 (8) |
C1A—C6A | 1.407 (8) | C11B—H11B | 0.930 |
C2A—C3A | 1.387 (9) | C12B—H12B | 0.930 |
C2A—H2A | 0.930 | C21B—C20B | 1.472 (8) |
C3A—C4A | 1.380 (9) | C20B—C15B | 1.413 (7) |
C3A—H3A | 0.930 | C20B—C19B | 1.410 (8) |
C4A—C5A | 1.349 (9) | C15B—C16B | 1.386 (8) |
C4A—H4A | 0.930 | C16B—C17B | 1.373 (8) |
C5A—C6A | 1.394 (8) | C16B—H16B | 0.930 |
C5A—H5A | 0.930 | C17B—C18B | 1.390 (9) |
C6A—C7A | 1.487 (8) | C17B—H17B | 0.930 |
C14A—C13A | 1.466 (7) | C18B—C19B | 1.345 (9) |
C13A—C12A | 1.399 (8) | C18B—H18B | 0.930 |
C13A—C8A | 1.409 (7) | C19B—H19B | 0.930 |
C12A—C11A | 1.375 (8) | O1W—Na2iv | 2.354 (5) |
C12A—H12A | 0.930 | O5W—Na4ii | 2.392 (5) |
C11A—C10A | 1.378 (9) | O10A—O10B | 0.84 (3) |
C11A—H11A | 0.930 | ||
O1A—TiA—O3A | 94.62 (17) | O8A—C14A—O4A | 119.2 (5) |
O1A—TiA—O5A | 99.42 (17) | O8A—C14A—C13A | 121.5 (6) |
O3A—TiA—O5A | 92.20 (17) | O4A—C14A—C13A | 119.2 (5) |
O1A—TiA—O6A | 98.09 (18) | C12A—C13A—C8A | 118.2 (5) |
O3A—TiA—O6A | 167.20 (17) | C12A—C13A—C14A | 119.7 (5) |
O5A—TiA—O6A | 84.29 (16) | C8A—C13A—C14A | 122.1 (5) |
O1A—TiA—O4A | 164.15 (17) | C11A—C12A—C13A | 121.9 (6) |
O3A—TiA—O4A | 84.52 (16) | C11A—C12A—H12A | 119.1 |
O5A—TiA—O4A | 96.44 (17) | C13A—C12A—H12A | 119.1 |
O6A—TiA—O4A | 83.65 (16) | C12A—C11A—C10A | 118.9 (6) |
O1A—TiA—O2A | 84.32 (16) | C12A—C11A—H11A | 120.5 |
O3A—TiA—O2A | 99.10 (16) | C10A—C11A—H11A | 120.5 |
O5A—TiA—O2A | 167.80 (16) | C9A—C10A—C11A | 121.3 (6) |
O6A—TiA—O2A | 83.69 (15) | C9A—C10A—H10A | 119.3 |
O4A—TiA—O2A | 80.20 (16) | C11A—C10A—H10A | 119.3 |
O5B—TiB—O3B | 92.47 (17) | C10A—C9A—C8A | 120.1 (6) |
O5B—TiB—O1B | 98.47 (17) | C10A—C9A—H9A | 120.0 |
O3B—TiB—O1B | 93.62 (17) | C8A—C9A—H9A | 120.0 |
O5B—TiB—O4B | 166.24 (16) | O3A—C8A—C9A | 118.5 (5) |
O3B—TiB—O4B | 85.12 (16) | O3A—C8A—C13A | 121.9 (5) |
O1B—TiB—O4B | 95.20 (17) | C9A—C8A—C13A | 119.6 (5) |
O5B—TiB—O6B | 85.14 (15) | O9A—C21A—O6A | 119.3 (5) |
O3B—TiB—O6B | 98.48 (16) | O9A—C21A—C20A | 121.4 (5) |
O1B—TiB—O6B | 167.23 (16) | O6A—C21A—C20A | 119.2 (5) |
O4B—TiB—O6B | 81.83 (15) | C19A—C20A—C15A | 118.8 (5) |
O5B—TiB—O2B | 97.64 (17) | C19A—C20A—C21A | 118.7 (5) |
O3B—TiB—O2B | 169.89 (16) | C15A—C20A—C21A | 122.5 (5) |
O1B—TiB—O2B | 84.63 (15) | C18A—C19A—C20A | 119.5 (6) |
O4B—TiB—O2B | 85.13 (15) | C18A—C19A—H19A | 120.2 |
O6B—TiB—O2B | 82.74 (15) | C20A—C19A—H19A | 120.2 |
O7Bi—Na1—O8Bii | 104.50 (16) | C17A—C18A—C19A | 120.7 (6) |
O7Bi—Na1—O5W | 82.07 (14) | C17A—C18A—H18A | 119.7 |
O8Bii—Na1—O5W | 83.31 (15) | C19A—C18A—H18A | 119.7 |
O7Bi—Na1—O7A | 99.66 (15) | C18A—C17A—C16A | 120.0 (6) |
O8Bii—Na1—O7A | 105.11 (16) | C18A—C17A—H17A | 120.0 |
O5W—Na1—O7A | 170.51 (16) | C16A—C17A—H17A | 120.0 |
O7Bi—Na1—O6W | 83.46 (15) | C17A—C16A—C15A | 121.5 (6) |
O8Bii—Na1—O6W | 163.38 (16) | C17A—C16A—H16A | 119.3 |
O5W—Na1—O6W | 83.39 (14) | C15A—C16A—H16A | 119.3 |
O7A—Na1—O6W | 87.53 (14) | O5A—C15A—C16A | 119.2 (5) |
O7Bi—Na1—O4W | 162.43 (17) | O5A—C15A—C20A | 121.3 (5) |
O8Bii—Na1—O4W | 83.04 (15) | C16A—C15A—C20A | 119.5 (5) |
O5W—Na1—O4W | 83.11 (14) | C7B—O2B—TiB | 133.9 (3) |
O7A—Na1—O4W | 93.46 (15) | C1B—O1B—TiB | 135.8 (3) |
O6W—Na1—O4W | 85.51 (15) | C8B—O3B—TiB | 133.7 (3) |
O9A—Na2—O1Wiii | 94.67 (17) | C14B—O4B—TiB | 133.4 (3) |
O9A—Na2—O4Aiii | 145.05 (18) | C15B—O5B—TiB | 132.1 (4) |
O1Wiii—Na2—O4Aiii | 120.09 (17) | C21B—O6B—TiB | 131.0 (3) |
O9A—Na2—O8Aiii | 93.45 (17) | C7B—O7B—Na1ii | 149.8 (4) |
O1Wiii—Na2—O8Aiii | 168.87 (17) | C7B—O7B—Na4ii | 113.3 (4) |
O4Aiii—Na2—O8Aiii | 52.72 (14) | Na1ii—O7B—Na4ii | 94.12 (15) |
O9A—Na2—O7W | 81.02 (16) | C14B—O8B—Na4 | 119.7 (4) |
O1Wiii—Na2—O7W | 87.87 (16) | C14B—O8B—Na1i | 146.9 (4) |
O4Aiii—Na2—O7W | 95.74 (17) | Na4—O8B—Na1i | 93.31 (16) |
O8Aiii—Na2—O7W | 100.91 (17) | O7B—C7B—O2B | 121.2 (5) |
O9A—Na2—O2W | 106.71 (17) | O7B—C7B—C6B | 119.5 (5) |
O1Wiii—Na2—O2W | 87.31 (16) | O2B—C7B—C6B | 119.2 (5) |
O4Aiii—Na2—O2W | 80.36 (15) | C5B—C6B—C1B | 118.0 (5) |
O8Aiii—Na2—O2W | 83.07 (16) | C5B—C6B—C7B | 119.0 (5) |
O7W—Na2—O2W | 171.20 (19) | C1B—C6B—C7B | 123.0 (5) |
O9W—Na3—O3W | 86.8 (2) | C4B—C5B—C6B | 121.9 (6) |
O9W—Na3—O6A | 87.1 (2) | C4B—C5B—H5B | 119.1 |
O3W—Na3—O6A | 126.58 (18) | C6B—C5B—H5B | 119.1 |
O9W—Na3—O7W | 96.4 (2) | C5B—C4B—C3B | 119.5 (6) |
O3W—Na3—O7W | 105.35 (18) | C5B—C4B—H4B | 120.3 |
O6A—Na3—O7W | 128.08 (17) | C3B—C4B—H4B | 120.3 |
O9W—Na3—O1W | 164.1 (2) | C2B—C3B—C4B | 119.9 (5) |
O3W—Na3—O1W | 78.73 (16) | C2B—C3B—H3B | 120.0 |
O6A—Na3—O1W | 96.35 (16) | C4B—C3B—H3B | 120.0 |
O7W—Na3—O1W | 93.56 (17) | C3B—C2B—C1B | 120.0 (6) |
O9W—Na3—O9A | 108.4 (2) | C3B—C2B—H2B | 120.0 |
O3W—Na3—O9A | 164.33 (19) | C1B—C2B—H2B | 120.0 |
O6A—Na3—O9A | 52.78 (14) | O1B—C1B—C2B | 117.6 (5) |
O7W—Na3—O9A | 77.49 (16) | O1B—C1B—C6B | 121.7 (5) |
O1W—Na3—O9A | 85.74 (16) | C2B—C1B—C6B | 120.6 (5) |
O8B—Na4—O6W | 98.48 (16) | O8B—C14B—O4B | 120.5 (5) |
O8B—Na4—O5Wi | 85.81 (15) | O8B—C14B—C13B | 120.1 (5) |
O6W—Na4—O5Wi | 175.27 (17) | O4B—C14B—C13B | 119.4 (5) |
O8B—Na4—O7Bi | 121.01 (18) | C12B—C13B—C8B | 119.2 (5) |
O6W—Na4—O7Bi | 85.42 (16) | C12B—C13B—C14B | 118.6 (5) |
O5Wi—Na4—O7Bi | 90.67 (16) | C8B—C13B—C14B | 122.1 (5) |
O8B—Na4—O8W | 126.4 (2) | O3B—C8B—C9B | 118.7 (5) |
O6W—Na4—O8W | 87.5 (2) | O3B—C8B—C13B | 122.5 (5) |
O5Wi—Na4—O8W | 91.6 (2) | C9B—C8B—C13B | 118.8 (5) |
O7Bi—Na4—O8W | 112.6 (2) | C10B—C9B—C8B | 121.3 (6) |
C1A—O1A—TiA | 133.0 (4) | C10B—C9B—H9B | 119.3 |
C7A—O2A—TiA | 131.6 (4) | C8B—C9B—H9B | 119.3 |
C14A—O4A—TiA | 133.7 (4) | C9B—C10B—C11B | 119.5 (6) |
C14A—O4A—Na2iv | 94.7 (3) | C9B—C10B—H10B | 120.3 |
TiA—O4A—Na2iv | 130.8 (2) | C11B—C10B—H10B | 120.3 |
C8A—O3A—TiA | 132.8 (3) | C12B—C11B—C10B | 120.1 (6) |
C21A—O6A—TiA | 134.9 (4) | C12B—C11B—H11B | 120.0 |
C21A—O6A—Na3 | 95.3 (3) | C10B—C11B—H11B | 120.0 |
TiA—O6A—Na3 | 129.70 (19) | C11B—C12B—C13B | 121.0 (6) |
C15A—O5A—TiA | 137.0 (3) | C11B—C12B—H12B | 119.5 |
C7A—O7A—Na1 | 164.4 (4) | C13B—C12B—H12B | 119.5 |
C14A—O8A—Na2iv | 93.3 (4) | O9B—C21B—O6B | 120.3 (5) |
C21A—O9A—Na2 | 168.5 (4) | O9B—C21B—C20B | 120.0 (5) |
C21A—O9A—Na3 | 92.3 (3) | O6B—C21B—C20B | 119.7 (5) |
Na2—O9A—Na3 | 97.94 (17) | C15B—C20B—C19B | 118.5 (5) |
O1A—C1A—C2A | 119.4 (5) | C15B—C20B—C21B | 121.8 (5) |
O1A—C1A—C6A | 121.8 (5) | C19B—C20B—C21B | 119.6 (5) |
C2A—C1A—C6A | 118.8 (5) | O5B—C15B—C16B | 120.4 (5) |
C3A—C2A—C1A | 121.0 (6) | O5B—C15B—C20B | 120.5 (5) |
C3A—C2A—H2A | 119.5 | C16B—C15B—C20B | 119.1 (5) |
C1A—C2A—H2A | 119.5 | C17B—C16B—C15B | 121.2 (6) |
C4A—C3A—C2A | 119.9 (6) | C17B—C16B—H16B | 119.4 |
C4A—C3A—H3A | 120.0 | C15B—C16B—H16B | 119.4 |
C2A—C3A—H3A | 120.0 | C16B—C17B—C18B | 119.2 (6) |
C5A—C4A—C3A | 119.3 (6) | C16B—C17B—H17B | 120.4 |
C5A—C4A—H4A | 120.3 | C18B—C17B—H17B | 120.4 |
C3A—C4A—H4A | 120.3 | C19B—C18B—C17B | 121.4 (6) |
C4A—C5A—C6A | 122.7 (7) | C19B—C18B—H18B | 119.3 |
C4A—C5A—H5A | 118.7 | C17B—C18B—H18B | 119.3 |
C6A—C5A—H5A | 118.7 | C18B—C19B—C20B | 120.5 (6) |
C5A—C6A—C1A | 118.2 (6) | C18B—C19B—H19B | 119.7 |
C5A—C6A—C7A | 120.5 (6) | C20B—C19B—H19B | 119.7 |
C1A—C6A—C7A | 121.3 (5) | Na2iv—O1W—Na3 | 107.24 (17) |
O7A—C7A—O2A | 120.7 (5) | Na4ii—O5W—Na1 | 91.17 (15) |
O7A—C7A—C6A | 119.8 (5) | Na4—O6W—Na1 | 91.74 (15) |
O2A—C7A—C6A | 119.5 (5) | Na3—O7W—Na2 | 94.12 (18) |
O3A—TiA—O1A—C1A | 67.8 (5) | TiA—O5A—C15A—C20A | −5.7 (9) |
O5A—TiA—O1A—C1A | 160.8 (5) | C17A—C16A—C15A—O5A | 178.8 (6) |
O6A—TiA—O1A—C1A | −113.7 (5) | C17A—C16A—C15A—C20A | −1.3 (10) |
O4A—TiA—O1A—C1A | −18.4 (9) | C19A—C20A—C15A—O5A | −178.3 (5) |
O2A—TiA—O1A—C1A | −30.9 (5) | C21A—C20A—C15A—O5A | 1.4 (9) |
O1A—TiA—O2A—C7A | 11.4 (5) | C19A—C20A—C15A—C16A | 1.9 (9) |
O3A—TiA—O2A—C7A | −82.4 (5) | C21A—C20A—C15A—C16A | −178.4 (6) |
O5A—TiA—O2A—C7A | 119.9 (9) | O5B—TiB—O2B—C7B | −106.8 (5) |
O6A—TiA—O2A—C7A | 110.2 (5) | O3B—TiB—O2B—C7B | 71.5 (11) |
O4A—TiA—O2A—C7A | −165.2 (5) | O1B—TiB—O2B—C7B | −9.0 (5) |
O1A—TiA—O4A—C14A | 96.1 (8) | O4B—TiB—O2B—C7B | 86.7 (5) |
O3A—TiA—O4A—C14A | 8.5 (5) | O6B—TiB—O2B—C7B | 169.1 (5) |
O5A—TiA—O4A—C14A | −83.1 (5) | O5B—TiB—O1B—C1B | 112.6 (5) |
O6A—TiA—O4A—C14A | −166.6 (5) | O3B—TiB—O1B—C1B | −154.4 (5) |
O2A—TiA—O4A—C14A | 108.7 (5) | O4B—TiB—O1B—C1B | −69.0 (5) |
O1A—TiA—O4A—Na2iv | −70.5 (7) | O6B—TiB—O1B—C1B | 6.9 (12) |
O3A—TiA—O4A—Na2iv | −158.1 (3) | O2B—TiB—O1B—C1B | 15.6 (5) |
O5A—TiA—O4A—Na2iv | 110.3 (3) | O5B—TiB—O3B—C8B | 171.6 (5) |
O6A—TiA—O4A—Na2iv | 26.8 (2) | O1B—TiB—O3B—C8B | 72.9 (5) |
O2A—TiA—O4A—Na2iv | −57.9 (2) | O4B—TiB—O3B—C8B | −22.0 (4) |
O1A—TiA—O3A—C8A | 170.0 (4) | O6B—TiB—O3B—C8B | −103.0 (5) |
O5A—TiA—O3A—C8A | 70.4 (4) | O2B—TiB—O3B—C8B | −6.8 (12) |
O6A—TiA—O3A—C8A | −3.4 (10) | O5B—TiB—O4B—C14B | 88.0 (9) |
O4A—TiA—O3A—C8A | −25.9 (4) | O3B—TiB—O4B—C14B | 7.6 (5) |
O2A—TiA—O3A—C8A | −105.0 (4) | O1B—TiB—O4B—C14B | −85.6 (5) |
O1A—TiA—O6A—C21A | −108.7 (5) | O6B—TiB—O4B—C14B | 106.9 (5) |
O3A—TiA—O6A—C21A | 64.7 (10) | O2B—TiB—O4B—C14B | −169.7 (5) |
O5A—TiA—O6A—C21A | −9.9 (5) | O3B—TiB—O5B—C15B | 65.8 (5) |
O4A—TiA—O6A—C21A | 87.2 (5) | O1B—TiB—O5B—C15B | 159.8 (5) |
O2A—TiA—O6A—C21A | 168.0 (5) | O4B—TiB—O5B—C15B | −13.7 (10) |
O1A—TiA—O6A—Na3 | 74.8 (3) | O6B—TiB—O5B—C15B | −32.5 (5) |
O3A—TiA—O6A—Na3 | −111.9 (7) | O2B—TiB—O5B—C15B | −114.5 (5) |
O5A—TiA—O6A—Na3 | 173.6 (3) | O5B—TiB—O6B—C21B | 11.1 (5) |
O4A—TiA—O6A—Na3 | −89.3 (3) | O3B—TiB—O6B—C21B | −80.7 (5) |
O2A—TiA—O6A—Na3 | −8.5 (3) | O1B—TiB—O6B—C21B | 118.2 (8) |
O9W—Na3—O6A—C21A | 113.0 (4) | O4B—TiB—O6B—C21B | −164.4 (5) |
O3W—Na3—O6A—C21A | −163.1 (3) | O2B—TiB—O6B—C21B | 109.5 (5) |
O7W—Na3—O6A—C21A | 17.1 (4) | O6W—Na4—O8B—C14B | −20.8 (5) |
O1W—Na3—O6A—C21A | −82.5 (3) | O5Wi—Na4—O8B—C14B | 161.2 (4) |
O9A—Na3—O6A—C21A | −2.8 (3) | O7Bi—Na4—O8B—C14B | −110.5 (4) |
O9W—Na3—O6A—TiA | −69.4 (3) | O8W—Na4—O8B—C14B | 72.4 (5) |
O3W—Na3—O6A—TiA | 14.4 (4) | O6W—Na4—O8B—Na1i | 158.56 (16) |
O7W—Na3—O6A—TiA | −165.4 (2) | O5Wi—Na4—O8B—Na1i | −19.45 (16) |
O1W—Na3—O6A—TiA | 95.0 (3) | O7Bi—Na4—O8B—Na1i | 68.8 (2) |
O9A—Na3—O6A—TiA | 174.8 (3) | O8W—Na4—O8B—Na1i | −108.3 (2) |
O1A—TiA—O5A—C15A | 105.0 (6) | Na1ii—O7B—C7B—O2B | −114.2 (7) |
O3A—TiA—O5A—C15A | −160.0 (6) | Na4ii—O7B—C7B—O2B | 92.1 (5) |
O6A—TiA—O5A—C15A | 7.7 (6) | Na1ii—O7B—C7B—C6B | 67.7 (9) |
O4A—TiA—O5A—C15A | −75.3 (6) | Na4ii—O7B—C7B—C6B | −86.0 (5) |
O2A—TiA—O5A—C15A | −2.0 (12) | TiB—O2B—C7B—O7B | −176.6 (4) |
O7Bi—Na1—O7A—C7A | 27.8 (15) | TiB—O2B—C7B—C6B | 1.5 (8) |
O8Bii—Na1—O7A—C7A | −80.2 (15) | O7B—C7B—C6B—C5B | 3.4 (8) |
O6W—Na1—O7A—C7A | 110.7 (15) | O2B—C7B—C6B—C5B | −174.8 (5) |
O4W—Na1—O7A—C7A | −164.0 (15) | O7B—C7B—C6B—C1B | −176.5 (5) |
O1Wiii—Na2—O9A—C21A | 97 (2) | O2B—C7B—C6B—C1B | 5.4 (8) |
O4Aiii—Na2—O9A—C21A | −89 (2) | C1B—C6B—C5B—C4B | −3.5 (9) |
O8Aiii—Na2—O9A—C21A | −76 (2) | C7B—C6B—C5B—C4B | 176.6 (6) |
O7W—Na2—O9A—C21A | −176 (2) | C6B—C5B—C4B—C3B | 1.0 (10) |
O2W—Na2—O9A—C21A | 8 (2) | C5B—C4B—C3B—C2B | 2.0 (10) |
O1Wiii—Na2—O9A—Na3 | −110.15 (18) | C4B—C3B—C2B—C1B | −2.4 (10) |
O4Aiii—Na2—O9A—Na3 | 64.1 (3) | TiB—O1B—C1B—C2B | 162.9 (4) |
O8Aiii—Na2—O9A—Na3 | 77.46 (18) | TiB—O1B—C1B—C6B | −14.1 (9) |
O7W—Na2—O9A—Na3 | −23.05 (17) | C3B—C2B—C1B—O1B | −177.2 (6) |
O2W—Na2—O9A—Na3 | 161.26 (17) | C3B—C2B—C1B—C6B | −0.1 (9) |
O9W—Na3—O9A—C21A | −68.5 (4) | C5B—C6B—C1B—O1B | 180.0 (5) |
O3W—Na3—O9A—C21A | 96.5 (7) | C7B—C6B—C1B—O1B | −0.2 (9) |
O6A—Na3—O9A—C21A | 2.9 (3) | C5B—C6B—C1B—C2B | 3.0 (9) |
O7W—Na3—O9A—C21A | −161.2 (4) | C7B—C6B—C1B—C2B | −177.1 (5) |
O1W—Na3—O9A—C21A | 104.2 (4) | Na4—O8B—C14B—O4B | 62.2 (6) |
O9W—Na3—O9A—Na2 | 116.7 (2) | Na1i—O8B—C14B—O4B | −116.6 (7) |
O3W—Na3—O9A—Na2 | −78.3 (7) | Na4—O8B—C14B—C13B | −117.6 (5) |
O6A—Na3—O9A—Na2 | −171.9 (2) | Na1i—O8B—C14B—C13B | 63.6 (9) |
O7W—Na3—O9A—Na2 | 24.01 (18) | TiB—O4B—C14B—O8B | −176.7 (4) |
O1W—Na3—O9A—Na2 | −70.60 (18) | TiB—O4B—C14B—C13B | 3.2 (8) |
TiA—O1A—C1A—C2A | −150.8 (5) | O8B—C14B—C13B—C12B | −9.1 (8) |
TiA—O1A—C1A—C6A | 28.9 (8) | O4B—C14B—C13B—C12B | 171.1 (5) |
O1A—C1A—C2A—C3A | 177.4 (6) | O8B—C14B—C13B—C8B | 173.1 (5) |
C6A—C1A—C2A—C3A | −2.3 (9) | O4B—C14B—C13B—C8B | −6.7 (8) |
C1A—C2A—C3A—C4A | 1.4 (10) | TiB—O3B—C8B—C9B | −155.2 (4) |
C2A—C3A—C4A—C5A | 0.8 (11) | TiB—O3B—C8B—C13B | 24.9 (7) |
C3A—C4A—C5A—C6A | −2.2 (11) | C12B—C13B—C8B—O3B | 176.5 (5) |
C4A—C5A—C6A—C1A | 1.3 (10) | C14B—C13B—C8B—O3B | −5.7 (8) |
C4A—C5A—C6A—C7A | 178.9 (6) | C12B—C13B—C8B—C9B | −3.5 (8) |
O1A—C1A—C6A—C5A | −178.7 (5) | C14B—C13B—C8B—C9B | 174.3 (5) |
C2A—C1A—C6A—C5A | 1.0 (9) | O3B—C8B—C9B—C10B | −177.4 (5) |
O1A—C1A—C6A—C7A | 3.7 (9) | C13B—C8B—C9B—C10B | 2.6 (8) |
C2A—C1A—C6A—C7A | −176.6 (5) | C8B—C9B—C10B—C11B | 0.3 (9) |
Na1—O7A—C7A—O2A | −115.6 (14) | C9B—C10B—C11B—C12B | −2.3 (10) |
Na1—O7A—C7A—C6A | 62.6 (17) | C10B—C11B—C12B—C13B | 1.3 (10) |
TiA—O2A—C7A—O7A | −173.0 (4) | C8B—C13B—C12B—C11B | 1.6 (9) |
TiA—O2A—C7A—C6A | 8.8 (8) | C14B—C13B—C12B—C11B | −176.3 (6) |
C5A—C6A—C7A—O7A | −15.9 (9) | TiB—O6B—C21B—O9B | −170.5 (5) |
C1A—C6A—C7A—O7A | 161.6 (5) | TiB—O6B—C21B—C20B | 10.7 (8) |
C5A—C6A—C7A—O2A | 162.4 (6) | O9B—C21B—C20B—C15B | 159.0 (6) |
C1A—C6A—C7A—O2A | −20.1 (8) | O6B—C21B—C20B—C15B | −22.2 (9) |
Na2iv—O8A—C14A—O4A | 2.7 (6) | O9B—C21B—C20B—C19B | −17.6 (10) |
Na2iv—O8A—C14A—C13A | −177.5 (5) | O6B—C21B—C20B—C19B | 161.1 (6) |
TiA—O4A—C14A—O8A | −172.7 (4) | TiB—O5B—C15B—C16B | −149.2 (5) |
Na2iv—O4A—C14A—O8A | −2.8 (6) | TiB—O5B—C15B—C20B | 30.3 (8) |
TiA—O4A—C14A—C13A | 7.5 (8) | C19B—C20B—C15B—O5B | −179.4 (6) |
Na2iv—O4A—C14A—C13A | 177.4 (4) | C21B—C20B—C15B—O5B | 3.9 (9) |
O8A—C14A—C13A—C12A | −11.8 (8) | C19B—C20B—C15B—C16B | 0.1 (9) |
O4A—C14A—C13A—C12A | 168.0 (5) | C21B—C20B—C15B—C16B | −176.6 (6) |
O8A—C14A—C13A—C8A | 165.8 (5) | O5B—C15B—C16B—C17B | 177.4 (6) |
O4A—C14A—C13A—C8A | −14.4 (8) | C20B—C15B—C16B—C17B | −2.1 (10) |
C8A—C13A—C12A—C11A | 1.0 (8) | C15B—C16B—C17B—C18B | 1.0 (11) |
C14A—C13A—C12A—C11A | 178.8 (6) | C16B—C17B—C18B—C19B | 2.2 (12) |
C13A—C12A—C11A—C10A | −0.2 (9) | C17B—C18B—C19B—C20B | −4.2 (12) |
C12A—C11A—C10A—C9A | −0.2 (9) | C15B—C20B—C19B—C18B | 3.0 (10) |
C11A—C10A—C9A—C8A | −0.2 (9) | C21B—C20B—C19B—C18B | 179.8 (7) |
TiA—O3A—C8A—C9A | −155.1 (4) | O9W—Na3—O1W—Na2iv | 80.1 (8) |
TiA—O3A—C8A—C13A | 26.6 (7) | O3W—Na3—O1W—Na2iv | 104.23 (19) |
C10A—C9A—C8A—O3A | −177.4 (5) | O6A—Na3—O1W—Na2iv | −21.87 (19) |
C10A—C9A—C8A—C13A | 1.0 (8) | O7W—Na3—O1W—Na2iv | −150.82 (18) |
C12A—C13A—C8A—O3A | 176.9 (5) | O9A—Na3—O1W—Na2iv | −73.66 (18) |
C14A—C13A—C8A—O3A | −0.8 (8) | O7Bi—Na1—O5W—Na4ii | −124.39 (16) |
C12A—C13A—C8A—C9A | −1.3 (8) | O8Bii—Na1—O5W—Na4ii | −18.67 (15) |
C14A—C13A—C8A—C9A | −179.0 (5) | O6W—Na1—O5W—Na4ii | 151.33 (16) |
Na2—O9A—C21A—O6A | 148.3 (18) | O4W—Na1—O5W—Na4ii | 65.08 (15) |
Na3—O9A—C21A—O6A | −4.9 (6) | O8B—Na4—O6W—Na1 | −103.78 (16) |
Na2—O9A—C21A—C20A | −34 (2) | O7Bi—Na4—O6W—Na1 | 16.93 (14) |
Na3—O9A—C21A—C20A | 173.2 (5) | O8W—Na4—O6W—Na1 | 129.8 (2) |
TiA—O6A—C21A—O9A | −172.2 (4) | O7Bi—Na1—O6W—Na4 | −17.18 (15) |
Na3—O6A—C21A—O9A | 5.1 (6) | O8Bii—Na1—O6W—Na4 | 102.6 (6) |
TiA—O6A—C21A—C20A | 9.6 (8) | O5W—Na1—O6W—Na4 | 65.55 (15) |
Na3—O6A—C21A—C20A | −173.0 (5) | O7A—Na1—O6W—Na4 | −117.21 (16) |
O9A—C21A—C20A—C19A | −1.9 (9) | O4W—Na1—O6W—Na4 | 149.12 (15) |
O6A—C21A—C20A—C19A | 176.2 (5) | O9W—Na3—O7W—Na2 | −129.0 (2) |
O9A—C21A—C20A—C15A | 178.4 (6) | O3W—Na3—O7W—Na2 | 142.64 (18) |
O6A—C21A—C20A—C15A | −3.5 (9) | O6A—Na3—O7W—Na2 | −37.6 (3) |
C15A—C20A—C19A—C18A | −1.9 (9) | O1W—Na3—O7W—Na2 | 63.36 (18) |
C21A—C20A—C19A—C18A | 178.4 (6) | O9A—Na3—O7W—Na2 | −21.48 (16) |
C20A—C19A—C18A—C17A | 1.3 (11) | O9A—Na2—O7W—Na3 | 23.72 (18) |
C19A—C18A—C17A—C16A | −0.7 (12) | O1Wiii—Na2—O7W—Na3 | 118.79 (18) |
C18A—C17A—C16A—C15A | 0.7 (12) | O4Aiii—Na2—O7W—Na3 | −121.18 (17) |
TiA—O5A—C15A—C16A | 174.2 (5) | O8Aiii—Na2—O7W—Na3 | −68.09 (18) |
Symmetry codes: (i) −x−1/2, y+1/2, −z+1/2; (ii) −x−1/2, y−1/2, −z+1/2; (iii) −x+1/2, y−1/2, −z+1/2; (iv) −x+1/2, y+1/2, −z+1/2. |
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