Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806054547/bt2222sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536806054547/bt22222sup2.hkl |
CCDC reference: 636159
Data collection: SMART (Bruker, 1998); cell refinement: SMART; data reduction: SAINT (Bruker, 1998); program(s) used to solve structure: SHELXTL (Sheldrick, 2000); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.
[Ti(C6F5)2(C14H42O2Si7)] | F(000) = 1696 |
Mr = 821.13 | Dx = 1.306 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 8815 reflections |
a = 11.3299 (2) Å | θ = 2.7–37.2° |
b = 19.1104 (3) Å | µ = 0.47 mm−1 |
c = 19.7235 (4) Å | T = 173 K |
β = 102.039 (1)° | Prism, orange |
V = 4176.58 (13) Å3 | 0.60 × 0.48 × 0.45 mm |
Z = 4 |
Bruker X8-APEX CCD diffractometer | 6528 reflections with I > 2σ(I) |
Radiation source: sealed tube | Rint = 0.027 |
Graphite monochromator | θmax = 25.0°, θmin = 2.1° |
φ and ω scans | h = −13→13 |
45244 measured reflections | k = −22→22 |
7359 independent reflections | l = −23→21 |
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)] = 0.036 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.099 | H-atom parameters constrained |
S = 1.08 | w = 1/[σ2(Fo2) + (0.0379P)2 + 3.8726P] where P = (Fo2 + 2Fc2)/3 |
7359 reflections | (Δ/σ)max = 0.001 |
429 parameters | Δρmax = 0.59 e Å−3 |
0 restraints | Δρmin = −0.55 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 | ||
Ti1 | 0.27295 (3) | 0.512686 (19) | 0.23102 (2) | 0.03294 (11) | |
Si1 | 0.41862 (7) | 0.74991 (4) | 0.27561 (4) | 0.04606 (17) | |
Si2 | 0.27059 (5) | 0.68266 (3) | 0.20236 (3) | 0.03057 (14) | |
Si3 | 0.07561 (7) | 0.69010 (3) | 0.22993 (5) | 0.0511 (2) | |
Si4 | 0.00705 (5) | 0.57465 (3) | 0.24422 (3) | 0.03239 (14) | |
Si5 | −0.14650 (6) | 0.53884 (4) | 0.15109 (3) | 0.04102 (16) | |
Si6 | 0.27251 (7) | 0.70754 (4) | 0.08555 (3) | 0.04375 (17) | |
Si7 | −0.03101 (6) | 0.55274 (4) | 0.35522 (3) | 0.04411 (17) | |
F1 | 0.10949 (19) | 0.37976 (10) | 0.15847 (12) | 0.0863 (6) | |
F2 | 0.1349 (2) | 0.28910 (9) | 0.05826 (11) | 0.0870 (6) | |
F3 | 0.32395 (19) | 0.30126 (10) | −0.00461 (9) | 0.0775 (5) | |
F4 | 0.48586 (18) | 0.40658 (12) | 0.03042 (11) | 0.0893 (6) | |
F5 | 0.45982 (15) | 0.49815 (10) | 0.12999 (10) | 0.0730 (5) | |
F6 | 0.22304 (18) | 0.39474 (11) | 0.33595 (15) | 0.1071 (9) | |
F7 | 0.3459 (2) | 0.34675 (14) | 0.45957 (15) | 0.1243 (10) | |
F8 | 0.5698 (2) | 0.39617 (12) | 0.51351 (10) | 0.0908 (7) | |
F9 | 0.66876 (19) | 0.49429 (13) | 0.44520 (12) | 0.1002 (7) | |
F10 | 0.54701 (15) | 0.54297 (11) | 0.32243 (10) | 0.0834 (6) | |
O1 | 0.31779 (13) | 0.59759 (7) | 0.21466 (8) | 0.0364 (3) | |
O2 | 0.12400 (13) | 0.51898 (7) | 0.24056 (8) | 0.0361 (3) | |
C1 | 0.3980 (3) | 0.84267 (14) | 0.24688 (17) | 0.0621 (8) | |
H1A | 0.4495 | 0.8729 | 0.2809 | 0.093* | |
H1B | 0.3134 | 0.8561 | 0.2429 | 0.093* | |
H1C | 0.4204 | 0.8479 | 0.2017 | 0.093* | |
C2 | 0.5723 (3) | 0.7211 (2) | 0.2679 (3) | 0.1003 (15) | |
H2A | 0.5829 | 0.7293 | 0.2205 | 0.150* | |
H2B | 0.5819 | 0.6712 | 0.2787 | 0.150* | |
H2C | 0.6330 | 0.7478 | 0.3004 | 0.150* | |
C3 | 0.4065 (5) | 0.7422 (3) | 0.36862 (18) | 0.128 (2) | |
H3A | 0.3972 | 0.6929 | 0.3800 | 0.192* | |
H3B | 0.3362 | 0.7687 | 0.3760 | 0.192* | |
H3C | 0.4797 | 0.7611 | 0.3985 | 0.192* | |
C4 | 0.0820 (5) | 0.7412 (2) | 0.3122 (3) | 0.127 (2) | |
H4A | 0.1112 | 0.7887 | 0.3064 | 0.190* | |
H4B | 0.1370 | 0.7180 | 0.3505 | 0.190* | |
H4C | 0.0011 | 0.7437 | 0.3225 | 0.190* | |
C5 | −0.0335 (3) | 0.73686 (19) | 0.1581 (3) | 0.1117 (18) | |
H5A | −0.1145 | 0.7363 | 0.1684 | 0.168* | |
H5B | −0.0352 | 0.7130 | 0.1140 | 0.168* | |
H5C | −0.0073 | 0.7854 | 0.1550 | 0.168* | |
C6 | −0.0898 (3) | 0.54608 (17) | 0.06869 (14) | 0.0577 (7) | |
H6A | −0.0168 | 0.5176 | 0.0723 | 0.086* | |
H6B | −0.0710 | 0.5951 | 0.0608 | 0.086* | |
H6C | −0.1519 | 0.5293 | 0.0299 | 0.086* | |
C7 | −0.2845 (3) | 0.59348 (19) | 0.14792 (19) | 0.0724 (9) | |
H7A | −0.3474 | 0.5790 | 0.1084 | 0.109* | |
H7B | −0.2647 | 0.6429 | 0.1428 | 0.109* | |
H7C | −0.3137 | 0.5872 | 0.1909 | 0.109* | |
C8 | −0.1847 (3) | 0.44521 (16) | 0.16234 (16) | 0.0669 (8) | |
H8A | −0.2151 | 0.4399 | 0.2051 | 0.100* | |
H8B | −0.1122 | 0.4164 | 0.1652 | 0.100* | |
H8C | −0.2467 | 0.4301 | 0.1227 | 0.100* | |
C9 | 0.4336 (3) | 0.7204 (2) | 0.07805 (18) | 0.0803 (10) | |
H9A | 0.4798 | 0.6778 | 0.0933 | 0.120* | |
H9B | 0.4685 | 0.7598 | 0.1073 | 0.120* | |
H9C | 0.4366 | 0.7303 | 0.0297 | 0.120* | |
C10 | 0.1902 (4) | 0.7900 (2) | 0.0557 (2) | 0.0998 (14) | |
H10A | 0.2083 | 0.8043 | 0.0113 | 0.150* | |
H10B | 0.2158 | 0.8269 | 0.0902 | 0.150* | |
H10C | 0.1032 | 0.7822 | 0.0500 | 0.150* | |
C11 | 0.2112 (4) | 0.6325 (2) | 0.02962 (17) | 0.0899 (12) | |
H11A | 0.1254 | 0.6268 | 0.0298 | 0.135* | |
H11B | 0.2550 | 0.5898 | 0.0473 | 0.135* | |
H11C | 0.2210 | 0.6413 | −0.0179 | 0.135* | |
C12 | −0.1428 (3) | 0.61560 (19) | 0.37747 (19) | 0.0753 (9) | |
H12A | −0.2196 | 0.6108 | 0.3441 | 0.113* | |
H12B | −0.1124 | 0.6635 | 0.3758 | 0.113* | |
H12C | −0.1551 | 0.6056 | 0.4242 | 0.113* | |
C13 | −0.0880 (4) | 0.46124 (17) | 0.35791 (17) | 0.0810 (11) | |
H13A | −0.0904 | 0.4488 | 0.4058 | 0.122* | |
H13B | −0.0341 | 0.4290 | 0.3403 | 0.122* | |
H13C | −0.1694 | 0.4579 | 0.3290 | 0.122* | |
C14 | 0.1156 (3) | 0.5602 (2) | 0.41908 (17) | 0.0862 (11) | |
H14A | 0.1027 | 0.5509 | 0.4658 | 0.129* | |
H14B | 0.1480 | 0.6076 | 0.4173 | 0.129* | |
H14C | 0.1731 | 0.5262 | 0.4076 | 0.129* | |
C15 | 0.2837 (2) | 0.44308 (12) | 0.14786 (12) | 0.0399 (5) | |
C16 | 0.2040 (3) | 0.38830 (13) | 0.12766 (14) | 0.0500 (6) | |
C17 | 0.2159 (3) | 0.34076 (13) | 0.07700 (15) | 0.0532 (7) | |
C18 | 0.3112 (3) | 0.34706 (14) | 0.04469 (13) | 0.0534 (7) | |
C19 | 0.3925 (2) | 0.40064 (16) | 0.06223 (14) | 0.0534 (7) | |
C20 | 0.3768 (2) | 0.44675 (14) | 0.11308 (13) | 0.0465 (6) | |
C21 | 0.3792 (2) | 0.47195 (12) | 0.32502 (13) | 0.0408 (5) | |
C22 | 0.3336 (3) | 0.42099 (14) | 0.36217 (17) | 0.0598 (7) | |
C23 | 0.3954 (3) | 0.39551 (16) | 0.42515 (18) | 0.0693 (9) | |
C24 | 0.5081 (3) | 0.42040 (16) | 0.45225 (15) | 0.0605 (8) | |
C25 | 0.5585 (3) | 0.46968 (16) | 0.41739 (15) | 0.0578 (7) | |
C26 | 0.4933 (2) | 0.49431 (14) | 0.35503 (13) | 0.0477 (6) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ti1 | 0.0330 (2) | 0.02330 (19) | 0.0428 (2) | 0.00182 (15) | 0.00847 (16) | 0.00002 (16) |
Si1 | 0.0514 (4) | 0.0360 (4) | 0.0459 (4) | −0.0133 (3) | −0.0011 (3) | −0.0023 (3) |
Si2 | 0.0352 (3) | 0.0234 (3) | 0.0334 (3) | −0.0036 (2) | 0.0079 (2) | −0.0011 (2) |
Si3 | 0.0509 (4) | 0.0229 (3) | 0.0894 (6) | −0.0002 (3) | 0.0375 (4) | −0.0043 (3) |
Si4 | 0.0332 (3) | 0.0260 (3) | 0.0396 (3) | −0.0012 (2) | 0.0114 (2) | −0.0017 (2) |
Si5 | 0.0355 (3) | 0.0460 (4) | 0.0406 (3) | −0.0001 (3) | 0.0058 (3) | 0.0016 (3) |
Si6 | 0.0601 (4) | 0.0380 (4) | 0.0351 (3) | 0.0045 (3) | 0.0144 (3) | 0.0019 (3) |
Si7 | 0.0520 (4) | 0.0445 (4) | 0.0372 (3) | −0.0034 (3) | 0.0125 (3) | −0.0055 (3) |
F1 | 0.1026 (15) | 0.0578 (11) | 0.1187 (16) | −0.0358 (10) | 0.0695 (13) | −0.0305 (11) |
F2 | 0.1187 (16) | 0.0491 (10) | 0.0991 (14) | −0.0303 (10) | 0.0361 (12) | −0.0273 (10) |
F3 | 0.1083 (15) | 0.0663 (11) | 0.0589 (10) | 0.0154 (10) | 0.0197 (10) | −0.0228 (9) |
F4 | 0.0729 (12) | 0.1179 (17) | 0.0889 (14) | −0.0025 (11) | 0.0444 (11) | −0.0327 (12) |
F5 | 0.0476 (9) | 0.0852 (13) | 0.0911 (13) | −0.0191 (9) | 0.0259 (9) | −0.0299 (10) |
F6 | 0.0682 (12) | 0.0710 (13) | 0.168 (2) | −0.0215 (10) | −0.0089 (13) | 0.0595 (14) |
F7 | 0.1099 (18) | 0.1068 (18) | 0.160 (2) | 0.0086 (14) | 0.0364 (16) | 0.0951 (18) |
F8 | 0.1114 (16) | 0.0997 (16) | 0.0574 (11) | 0.0368 (13) | 0.0086 (10) | 0.0326 (11) |
F9 | 0.0705 (13) | 0.1227 (19) | 0.0878 (15) | −0.0117 (12) | −0.0282 (11) | 0.0281 (13) |
F10 | 0.0484 (9) | 0.1080 (15) | 0.0864 (13) | −0.0187 (10) | −0.0031 (9) | 0.0479 (12) |
O1 | 0.0348 (8) | 0.0276 (8) | 0.0467 (9) | 0.0004 (6) | 0.0081 (7) | 0.0010 (6) |
O2 | 0.0365 (8) | 0.0249 (7) | 0.0479 (9) | 0.0007 (6) | 0.0108 (7) | −0.0014 (6) |
C1 | 0.0713 (19) | 0.0361 (14) | 0.081 (2) | −0.0106 (13) | 0.0200 (16) | −0.0120 (14) |
C2 | 0.0481 (18) | 0.082 (3) | 0.154 (4) | 0.0123 (17) | −0.019 (2) | −0.031 (3) |
C3 | 0.181 (5) | 0.145 (4) | 0.0438 (18) | −0.100 (4) | −0.007 (2) | 0.004 (2) |
C4 | 0.171 (4) | 0.065 (2) | 0.191 (5) | −0.060 (3) | 0.144 (4) | −0.078 (3) |
C5 | 0.0511 (18) | 0.058 (2) | 0.229 (5) | 0.0173 (16) | 0.035 (3) | 0.069 (3) |
C6 | 0.0584 (16) | 0.0695 (19) | 0.0452 (14) | 0.0037 (14) | 0.0109 (12) | 0.0041 (13) |
C7 | 0.0422 (15) | 0.090 (2) | 0.085 (2) | 0.0132 (15) | 0.0126 (15) | 0.0036 (19) |
C8 | 0.077 (2) | 0.0615 (19) | 0.0599 (17) | −0.0279 (16) | 0.0090 (15) | −0.0091 (14) |
C9 | 0.080 (2) | 0.104 (3) | 0.068 (2) | −0.007 (2) | 0.0405 (18) | −0.0020 (19) |
C10 | 0.144 (4) | 0.089 (3) | 0.073 (2) | 0.058 (3) | 0.037 (2) | 0.036 (2) |
C11 | 0.135 (3) | 0.088 (3) | 0.0498 (18) | −0.038 (2) | 0.026 (2) | −0.0243 (17) |
C12 | 0.077 (2) | 0.077 (2) | 0.085 (2) | 0.0054 (18) | 0.0461 (19) | −0.0098 (18) |
C13 | 0.136 (3) | 0.0573 (19) | 0.0563 (18) | −0.024 (2) | 0.036 (2) | 0.0046 (15) |
C14 | 0.079 (2) | 0.118 (3) | 0.0522 (18) | 0.009 (2) | −0.0076 (16) | −0.0223 (19) |
C15 | 0.0440 (13) | 0.0301 (11) | 0.0456 (13) | 0.0082 (10) | 0.0096 (10) | 0.0008 (10) |
C16 | 0.0607 (16) | 0.0331 (13) | 0.0608 (16) | −0.0004 (11) | 0.0236 (13) | −0.0003 (11) |
C17 | 0.0713 (18) | 0.0295 (12) | 0.0572 (15) | −0.0019 (12) | 0.0100 (14) | −0.0028 (11) |
C18 | 0.0722 (18) | 0.0454 (15) | 0.0405 (13) | 0.0197 (13) | 0.0069 (12) | −0.0040 (11) |
C19 | 0.0479 (14) | 0.0645 (18) | 0.0494 (15) | 0.0133 (13) | 0.0140 (12) | −0.0031 (13) |
C20 | 0.0390 (13) | 0.0489 (15) | 0.0498 (14) | 0.0069 (11) | 0.0052 (11) | −0.0038 (11) |
C21 | 0.0431 (13) | 0.0321 (12) | 0.0476 (13) | 0.0082 (10) | 0.0103 (10) | 0.0019 (10) |
C22 | 0.0491 (15) | 0.0399 (14) | 0.089 (2) | 0.0033 (12) | 0.0114 (14) | 0.0200 (14) |
C23 | 0.076 (2) | 0.0523 (17) | 0.086 (2) | 0.0154 (15) | 0.0309 (18) | 0.0359 (16) |
C24 | 0.0701 (19) | 0.0622 (18) | 0.0496 (15) | 0.0270 (15) | 0.0133 (14) | 0.0146 (13) |
C25 | 0.0534 (16) | 0.0645 (18) | 0.0511 (15) | 0.0087 (14) | 0.0008 (13) | 0.0054 (14) |
C26 | 0.0470 (14) | 0.0498 (15) | 0.0467 (14) | 0.0057 (11) | 0.0106 (11) | 0.0083 (11) |
Ti1—O2 | 1.7408 (15) | C4—H4A | 0.9800 |
Ti1—O1 | 1.7503 (15) | C4—H4B | 0.9800 |
Ti1—C15 | 2.135 (2) | C4—H4C | 0.9800 |
Ti1—C21 | 2.136 (2) | C5—H5A | 0.9800 |
Si1—C1 | 1.861 (3) | C5—H5B | 0.9800 |
Si1—C2 | 1.862 (4) | C5—H5C | 0.9800 |
Si1—C3 | 1.874 (4) | C6—H6A | 0.9800 |
Si1—Si2 | 2.3540 (8) | C6—H6B | 0.9800 |
Si2—O1 | 1.7127 (15) | C6—H6C | 0.9800 |
Si2—Si6 | 2.3571 (8) | C7—H7A | 0.9800 |
Si2—Si3 | 2.3869 (9) | C7—H7B | 0.9800 |
Si3—C4 | 1.882 (4) | C7—H7C | 0.9800 |
Si3—C5 | 1.898 (4) | C8—H8A | 0.9800 |
Si3—Si4 | 2.3753 (9) | C8—H8B | 0.9800 |
Si4—O2 | 1.7125 (15) | C8—H8C | 0.9800 |
Si4—Si5 | 2.3528 (9) | C9—H9A | 0.9800 |
Si4—Si7 | 2.3554 (9) | C9—H9B | 0.9800 |
Si5—C8 | 1.865 (3) | C9—H9C | 0.9800 |
Si5—C7 | 1.870 (3) | C10—H10A | 0.9800 |
Si5—C6 | 1.873 (3) | C10—H10B | 0.9800 |
Si6—C11 | 1.853 (3) | C10—H10C | 0.9800 |
Si6—C10 | 1.863 (3) | C11—H11A | 0.9800 |
Si6—C9 | 1.877 (3) | C11—H11B | 0.9800 |
Si7—C12 | 1.863 (3) | C11—H11C | 0.9800 |
Si7—C13 | 1.869 (3) | C12—H12A | 0.9800 |
Si7—C14 | 1.869 (3) | C12—H12B | 0.9800 |
F1—C16 | 1.347 (3) | C12—H12C | 0.9800 |
F2—C17 | 1.346 (3) | C13—H13A | 0.9800 |
F3—C18 | 1.338 (3) | C13—H13B | 0.9800 |
F4—C19 | 1.343 (3) | C13—H13C | 0.9800 |
F5—C20 | 1.353 (3) | C14—H14A | 0.9800 |
F6—C22 | 1.349 (3) | C14—H14B | 0.9800 |
F7—C23 | 1.342 (3) | C14—H14C | 0.9800 |
F8—C24 | 1.346 (3) | C15—C20 | 1.374 (3) |
F9—C25 | 1.340 (3) | C15—C16 | 1.386 (4) |
F10—C26 | 1.346 (3) | C16—C17 | 1.378 (4) |
C1—H1A | 0.9800 | C17—C18 | 1.369 (4) |
C1—H1B | 0.9800 | C18—C19 | 1.373 (4) |
C1—H1C | 0.9800 | C19—C20 | 1.374 (4) |
C2—H2A | 0.9800 | C21—C26 | 1.373 (4) |
C2—H2B | 0.9800 | C21—C22 | 1.381 (4) |
C2—H2C | 0.9800 | C22—C23 | 1.381 (4) |
C3—H3A | 0.9800 | C23—C24 | 1.363 (5) |
C3—H3B | 0.9800 | C24—C25 | 1.360 (4) |
C3—H3C | 0.9800 | C25—C26 | 1.379 (4) |
O2—Ti1—O1 | 106.33 (7) | H6B—C6—H6C | 109.5 |
O2—Ti1—C15 | 109.77 (8) | Si5—C7—H7A | 109.5 |
O1—Ti1—C15 | 111.75 (8) | Si5—C7—H7B | 109.5 |
O2—Ti1—C21 | 108.35 (8) | H7A—C7—H7B | 109.5 |
O1—Ti1—C21 | 111.43 (8) | Si5—C7—H7C | 109.5 |
C15—Ti1—C21 | 109.12 (9) | H7A—C7—H7C | 109.5 |
C1—Si1—C2 | 108.45 (18) | H7B—C7—H7C | 109.5 |
C1—Si1—C3 | 110.0 (2) | Si5—C8—H8A | 109.5 |
C2—Si1—C3 | 108.5 (2) | Si5—C8—H8B | 109.5 |
C1—Si1—Si2 | 107.78 (10) | H8A—C8—H8B | 109.5 |
C2—Si1—Si2 | 110.33 (12) | Si5—C8—H8C | 109.5 |
C3—Si1—Si2 | 111.68 (13) | H8A—C8—H8C | 109.5 |
O1—Si2—Si1 | 105.66 (6) | H8B—C8—H8C | 109.5 |
O1—Si2—Si6 | 105.29 (6) | Si6—C9—H9A | 109.5 |
Si1—Si2—Si6 | 109.82 (3) | Si6—C9—H9B | 109.5 |
O1—Si2—Si3 | 107.50 (6) | H9A—C9—H9B | 109.5 |
Si1—Si2—Si3 | 113.73 (4) | Si6—C9—H9C | 109.5 |
Si6—Si2—Si3 | 114.10 (4) | H9A—C9—H9C | 109.5 |
C4—Si3—C5 | 107.5 (2) | H9B—C9—H9C | 109.5 |
C4—Si3—Si4 | 109.55 (13) | Si6—C10—H10A | 109.5 |
C5—Si3—Si4 | 110.34 (12) | Si6—C10—H10B | 109.5 |
C4—Si3—Si2 | 110.86 (14) | H10A—C10—H10B | 109.5 |
C5—Si3—Si2 | 110.37 (13) | Si6—C10—H10C | 109.5 |
Si4—Si3—Si2 | 108.23 (3) | H10A—C10—H10C | 109.5 |
O2—Si4—Si5 | 103.83 (6) | H10B—C10—H10C | 109.5 |
O2—Si4—Si7 | 102.83 (6) | Si6—C11—H11A | 109.5 |
Si5—Si4—Si7 | 115.15 (3) | Si6—C11—H11B | 109.5 |
O2—Si4—Si3 | 107.28 (6) | H11A—C11—H11B | 109.5 |
Si5—Si4—Si3 | 112.60 (4) | Si6—C11—H11C | 109.5 |
Si7—Si4—Si3 | 113.78 (4) | H11A—C11—H11C | 109.5 |
C8—Si5—C7 | 109.07 (16) | H11B—C11—H11C | 109.5 |
C8—Si5—C6 | 107.70 (15) | Si7—C12—H12A | 109.5 |
C7—Si5—C6 | 111.43 (15) | Si7—C12—H12B | 109.5 |
C8—Si5—Si4 | 109.76 (10) | H12A—C12—H12B | 109.5 |
C7—Si5—Si4 | 109.91 (12) | Si7—C12—H12C | 109.5 |
C6—Si5—Si4 | 108.92 (10) | H12A—C12—H12C | 109.5 |
C11—Si6—C10 | 111.4 (2) | H12B—C12—H12C | 109.5 |
C11—Si6—C9 | 107.68 (18) | Si7—C13—H13A | 109.5 |
C10—Si6—C9 | 107.2 (2) | Si7—C13—H13B | 109.5 |
C11—Si6—Si2 | 110.31 (12) | H13A—C13—H13B | 109.5 |
C10—Si6—Si2 | 111.92 (12) | Si7—C13—H13C | 109.5 |
C9—Si6—Si2 | 108.10 (12) | H13A—C13—H13C | 109.5 |
C12—Si7—C13 | 109.93 (18) | H13B—C13—H13C | 109.5 |
C12—Si7—C14 | 110.12 (17) | Si7—C14—H14A | 109.5 |
C13—Si7—C14 | 108.5 (2) | Si7—C14—H14B | 109.5 |
C12—Si7—Si4 | 111.69 (12) | H14A—C14—H14B | 109.5 |
C13—Si7—Si4 | 108.91 (10) | Si7—C14—H14C | 109.5 |
C14—Si7—Si4 | 107.65 (13) | H14A—C14—H14C | 109.5 |
Si2—O1—Ti1 | 144.29 (10) | H14B—C14—H14C | 109.5 |
Si4—O2—Ti1 | 145.44 (9) | C20—C15—C16 | 114.6 (2) |
Si1—C1—H1A | 109.5 | C20—C15—Ti1 | 121.64 (18) |
Si1—C1—H1B | 109.5 | C16—C15—Ti1 | 123.58 (18) |
H1A—C1—H1B | 109.5 | F1—C16—C17 | 117.0 (2) |
Si1—C1—H1C | 109.5 | F1—C16—C15 | 119.6 (2) |
H1A—C1—H1C | 109.5 | C17—C16—C15 | 123.4 (2) |
H1B—C1—H1C | 109.5 | F2—C17—C18 | 119.7 (2) |
Si1—C2—H2A | 109.5 | F2—C17—C16 | 121.3 (3) |
Si1—C2—H2B | 109.5 | C18—C17—C16 | 119.0 (3) |
H2A—C2—H2B | 109.5 | F3—C18—C17 | 119.7 (3) |
Si1—C2—H2C | 109.5 | F3—C18—C19 | 120.2 (3) |
H2A—C2—H2C | 109.5 | C17—C18—C19 | 120.1 (2) |
H2B—C2—H2C | 109.5 | F4—C19—C18 | 119.9 (2) |
Si1—C3—H3A | 109.5 | F4—C19—C20 | 121.4 (3) |
Si1—C3—H3B | 109.5 | C18—C19—C20 | 118.7 (2) |
H3A—C3—H3B | 109.5 | F5—C20—C15 | 118.7 (2) |
Si1—C3—H3C | 109.5 | F5—C20—C19 | 117.1 (2) |
H3A—C3—H3C | 109.5 | C15—C20—C19 | 124.1 (2) |
H3B—C3—H3C | 109.5 | C26—C21—C22 | 114.4 (2) |
Si3—C4—H4A | 109.5 | C26—C21—Ti1 | 124.77 (18) |
Si3—C4—H4B | 109.5 | C22—C21—Ti1 | 120.82 (19) |
H4A—C4—H4B | 109.5 | F6—C22—C23 | 118.0 (3) |
Si3—C4—H4C | 109.5 | F6—C22—C21 | 118.6 (3) |
H4A—C4—H4C | 109.5 | C23—C22—C21 | 123.4 (3) |
H4B—C4—H4C | 109.5 | F7—C23—C24 | 120.0 (3) |
Si3—C5—H5A | 109.5 | F7—C23—C22 | 120.9 (3) |
Si3—C5—H5B | 109.5 | C24—C23—C22 | 119.1 (3) |
H5A—C5—H5B | 109.5 | F8—C24—C25 | 119.9 (3) |
Si3—C5—H5C | 109.5 | F8—C24—C23 | 120.1 (3) |
H5A—C5—H5C | 109.5 | C25—C24—C23 | 120.1 (3) |
H5B—C5—H5C | 109.5 | F9—C25—C24 | 119.3 (3) |
Si5—C6—H6A | 109.5 | F9—C25—C26 | 121.7 (3) |
Si5—C6—H6B | 109.5 | C24—C25—C26 | 118.9 (3) |
H6A—C6—H6B | 109.5 | F10—C26—C21 | 119.2 (2) |
Si5—C6—H6C | 109.5 | F10—C26—C25 | 116.7 (2) |
H6A—C6—H6C | 109.5 | C21—C26—C25 | 124.0 (3) |
C1—Si1—Si2—O1 | 163.80 (12) | O1—Ti1—O2—Si4 | −4.4 (2) |
C2—Si1—Si2—O1 | 45.56 (18) | C15—Ti1—O2—Si4 | −125.46 (17) |
C3—Si1—Si2—O1 | −75.2 (2) | C21—Ti1—O2—Si4 | 115.47 (18) |
C1—Si1—Si2—Si6 | 50.72 (11) | O2—Ti1—C15—C20 | 156.52 (19) |
C2—Si1—Si2—Si6 | −67.52 (18) | O1—Ti1—C15—C20 | 38.8 (2) |
C3—Si1—Si2—Si6 | 171.7 (2) | C21—Ti1—C15—C20 | −84.9 (2) |
C1—Si1—Si2—Si3 | −78.52 (11) | O2—Ti1—C15—C16 | −28.0 (2) |
C2—Si1—Si2—Si3 | 163.24 (17) | O1—Ti1—C15—C16 | −145.7 (2) |
C3—Si1—Si2—Si3 | 42.5 (2) | C21—Ti1—C15—C16 | 90.6 (2) |
O1—Si2—Si3—C4 | 110.27 (18) | C20—C15—C16—F1 | 179.9 (2) |
Si1—Si2—Si3—C4 | −6.33 (18) | Ti1—C15—C16—F1 | 4.1 (4) |
Si6—Si2—Si3—C4 | −133.38 (18) | C20—C15—C16—C17 | 0.2 (4) |
O1—Si2—Si3—C5 | −130.74 (17) | Ti1—C15—C16—C17 | −175.6 (2) |
Si1—Si2—Si3—C5 | 112.66 (16) | F1—C16—C17—F2 | 1.4 (4) |
Si6—Si2—Si3—C5 | −14.38 (16) | C15—C16—C17—F2 | −178.8 (3) |
O1—Si2—Si3—Si4 | −9.90 (7) | F1—C16—C17—C18 | −179.5 (3) |
Si1—Si2—Si3—Si4 | −126.50 (4) | C15—C16—C17—C18 | 0.3 (4) |
Si6—Si2—Si3—Si4 | 106.45 (4) | F2—C17—C18—F3 | −0.9 (4) |
C4—Si3—Si4—O2 | −114.16 (19) | C16—C17—C18—F3 | 180.0 (2) |
C5—Si3—Si4—O2 | 127.68 (18) | F2—C17—C18—C19 | 178.4 (3) |
Si2—Si3—Si4—O2 | 6.83 (7) | C16—C17—C18—C19 | −0.8 (4) |
C4—Si3—Si4—Si5 | 132.22 (19) | F3—C18—C19—F4 | −0.8 (4) |
C5—Si3—Si4—Si5 | 14.06 (17) | C17—C18—C19—F4 | 180.0 (3) |
Si2—Si3—Si4—Si5 | −106.79 (4) | F3—C18—C19—C20 | −180.0 (2) |
C4—Si3—Si4—Si7 | −1.14 (19) | C17—C18—C19—C20 | 0.8 (4) |
C5—Si3—Si4—Si7 | −119.30 (17) | C16—C15—C20—F5 | −179.2 (2) |
Si2—Si3—Si4—Si7 | 119.85 (4) | Ti1—C15—C20—F5 | −3.4 (3) |
O2—Si4—Si5—C8 | 58.96 (13) | C16—C15—C20—C19 | −0.2 (4) |
Si7—Si4—Si5—C8 | −52.65 (12) | Ti1—C15—C20—C19 | 175.7 (2) |
Si3—Si4—Si5—C8 | 174.66 (12) | F4—C19—C20—F5 | −0.4 (4) |
O2—Si4—Si5—C7 | 178.92 (13) | C18—C19—C20—F5 | 178.8 (2) |
Si7—Si4—Si5—C7 | 67.31 (13) | F4—C19—C20—C15 | −179.5 (3) |
Si3—Si4—Si5—C7 | −65.37 (13) | C18—C19—C20—C15 | −0.3 (4) |
O2—Si4—Si5—C6 | −58.74 (12) | O2—Ti1—C21—C26 | −140.2 (2) |
Si7—Si4—Si5—C6 | −170.34 (11) | O1—Ti1—C21—C26 | −23.6 (2) |
Si3—Si4—Si5—C6 | 56.97 (11) | C15—Ti1—C21—C26 | 100.3 (2) |
O1—Si2—Si6—C11 | 41.81 (17) | O2—Ti1—C21—C22 | 37.4 (2) |
Si1—Si2—Si6—C11 | 155.13 (16) | O1—Ti1—C21—C22 | 154.1 (2) |
Si3—Si2—Si6—C11 | −75.82 (16) | C15—Ti1—C21—C22 | −82.1 (2) |
O1—Si2—Si6—C10 | 166.51 (19) | C26—C21—C22—F6 | −178.6 (3) |
Si1—Si2—Si6—C10 | −80.17 (18) | Ti1—C21—C22—F6 | 3.5 (4) |
Si3—Si2—Si6—C10 | 48.87 (18) | C26—C21—C22—C23 | 1.6 (4) |
O1—Si2—Si6—C9 | −75.69 (15) | Ti1—C21—C22—C23 | −176.2 (2) |
Si1—Si2—Si6—C9 | 37.63 (14) | F6—C22—C23—F7 | −0.9 (5) |
Si3—Si2—Si6—C9 | 166.68 (14) | C21—C22—C23—F7 | 178.9 (3) |
O2—Si4—Si7—C12 | 172.53 (14) | F6—C22—C23—C24 | 179.0 (3) |
Si5—Si4—Si7—C12 | −75.27 (13) | C21—C22—C23—C24 | −1.2 (5) |
Si3—Si4—Si7—C12 | 56.86 (13) | F7—C23—C24—F8 | −0.1 (5) |
O2—Si4—Si7—C13 | −65.87 (16) | C22—C23—C24—F8 | −179.9 (3) |
Si5—Si4—Si7—C13 | 46.33 (15) | F7—C23—C24—C25 | 179.8 (3) |
Si3—Si4—Si7—C13 | 178.46 (15) | C22—C23—C24—C25 | 0.0 (5) |
O2—Si4—Si7—C14 | 51.53 (15) | F8—C24—C25—F9 | −1.0 (4) |
Si5—Si4—Si7—C14 | 163.72 (14) | C23—C24—C25—F9 | 179.1 (3) |
Si3—Si4—Si7—C14 | −64.14 (15) | F8—C24—C25—C26 | −179.4 (3) |
Si1—Si2—O1—Ti1 | 131.30 (15) | C23—C24—C25—C26 | 0.7 (5) |
Si6—Si2—O1—Ti1 | −112.49 (16) | C22—C21—C26—F10 | 178.8 (3) |
Si3—Si2—O1—Ti1 | 9.52 (18) | Ti1—C21—C26—F10 | −3.5 (4) |
O2—Ti1—O1—Si2 | −2.55 (19) | C22—C21—C26—C25 | −0.9 (4) |
C15—Ti1—O1—Si2 | 117.21 (17) | Ti1—C21—C26—C25 | 176.9 (2) |
C21—Ti1—O1—Si2 | −120.41 (17) | F9—C25—C26—F10 | 1.8 (4) |
Si5—Si4—O2—Ti1 | 119.87 (17) | C24—C25—C26—F10 | −179.9 (3) |
Si7—Si4—O2—Ti1 | −119.80 (17) | F9—C25—C26—C21 | −178.6 (3) |
Si3—Si4—O2—Ti1 | 0.45 (19) | C24—C25—C26—C21 | −0.3 (5) |