Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270199012718/bk1495sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270199012718/bk1495Isup2.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270199012718/bk1495IIsup3.hkl |
CCDC references: 140939; 140940
Compounds (I) and (II) were generated by slow hydrolysis of the corresponding alkoxysilane precursor in CH2Cl2. Red needle-like crystals of both (I) and (II) were obtained by slow evaporation of an ethyl acetate solution at ambient temperature.
Only data up to 2θmax = 48.0° could be used for (I) as the crystals were very weak diffractors (mean I/σ = 1.8 for a resolution of 0.90 Å). For (I), intensity data were collected using a longer exposure time of 60 s per frame to improve data quality.
For both compounds, data collection: SMART (Bruker, 1997a); cell refinement: SMART; data reduction: SAINT (Bruker, 1997a); program(s) used to solve structure: SHELXTL-Plus (Sheldrick, 1999); program(s) used to refine structure: SHELXTL-Plus; molecular graphics: SHELXTL (Bruker, 1997b); software used to prepare material for publication: SHELXTL.
[TiCl2(C5H5)(C7H10Si)]2O·CH2Cl2 | F(000) = 1456 |
Mr = 713.19 | Dx = 1.504 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
a = 13.6494 (2) Å | Cell parameters from 4922 reflections |
b = 12.8573 (2) Å | θ = 2–24° |
c = 18.4995 (3) Å | µ = 1.11 mm−1 |
β = 103.977 (1)° | T = 223 K |
V = 3150.44 (8) Å3 | Needle, red |
Z = 4 | 0.40 × 0.18 × 0.10 mm |
Bruker CCD area detector diffractometer | 4950 independent reflections |
Radiation source: normal-focus sealed tube | 2810 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.13 |
ϕ and ω scans | θmax = 24°, θmin = 1.5° |
Absorption correction: empirical (using intensity measurements) (SADABS; Blessing, 1995) | h = −15→15 |
Tmin = 0.67, Tmax = 0.90 | k = −14→14 |
27882 measured reflections | l = −21→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)] = 0.070 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.179 | H-atom parameters constrained |
S = 1.05 | w = 1/[σ2(Fo2) + (0.0647P)2 + 10.5834P] where P = (Fo2 + 2Fc2)/3 |
4950 reflections | (Δ/σ)max = 0.001 |
325 parameters | Δρmax = 0.77 e Å−3 |
0 restraints | Δρmin = −0.66 e Å−3 |
[TiCl2(C5H5)(C7H10Si)]2O·CH2Cl2 | V = 3150.44 (8) Å3 |
Mr = 713.19 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 13.6494 (2) Å | µ = 1.11 mm−1 |
b = 12.8573 (2) Å | T = 223 K |
c = 18.4995 (3) Å | 0.40 × 0.18 × 0.10 mm |
β = 103.977 (1)° |
Bruker CCD area detector diffractometer | 4950 independent reflections |
Absorption correction: empirical (using intensity measurements) (SADABS; Blessing, 1995) | 2810 reflections with I > 2σ(I) |
Tmin = 0.67, Tmax = 0.90 | Rint = 0.13 |
27882 measured reflections | θmax = 24° |
R[F2 > 2σ(F2)] = 0.070 | 0 restraints |
wR(F2) = 0.179 | H-atom parameters constrained |
S = 1.05 | w = 1/[σ2(Fo2) + (0.0647P)2 + 10.5834P] where P = (Fo2 + 2Fc2)/3 |
4950 reflections | Δρmax = 0.77 e Å−3 |
325 parameters | Δρmin = −0.66 e Å−3 |
Experimental. Data were collected by the double-pass method using the CCD area detector system. The first 50 frames of data were re-collected at the end of data collection and no crystal decay was observed for either compound. |
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. The structures were solved by the Patterson method and refined successfully in the monoclinic space groups P21/c and P21/n. Full matrix least-squares refinement was carried out by minimizing w(Fo2-Fc2)2. The non-H atoms were refined anisotropically to convergence. H atoms were treated using appropriate riding models [SHELXTL-Plus command AFIX = m3 (Sheldrick, 1999)], where the atomic position of the H atom rides on the coordinates of the non-H atom to which it is attached and the displacement parameters are fixed at 1.2 times those of the parent atom. |
x | y | z | Uiso*/Ueq | ||
Ti1 | 0.72111 (9) | 0.89568 (10) | 0.01272 (8) | 0.0321 (4) | |
Ti2 | 1.21117 (9) | 0.60279 (10) | −0.01995 (8) | 0.0337 (4) | |
Cl1 | 0.65521 (15) | 1.01670 (16) | −0.08251 (11) | 0.0456 (6) | |
Cl2 | 0.72088 (16) | 1.01740 (16) | 0.10911 (12) | 0.0482 (6) | |
Cl3 | 1.13817 (14) | 0.47371 (15) | −0.10729 (11) | 0.0435 (5) | |
Cl4 | 1.23535 (14) | 0.48462 (16) | 0.08196 (11) | 0.0453 (5) | |
Si1 | 0.82779 (17) | 0.87783 (19) | −0.16077 (13) | 0.0451 (6) | |
Si2 | 1.00345 (17) | 0.72606 (18) | −0.17783 (13) | 0.0429 (6) | |
O | 0.9291 (4) | 0.8254 (4) | −0.1775 (3) | 0.0528 (15) | |
C1 | 0.8477 (5) | 0.8740 (6) | −0.0569 (4) | 0.0350 (19) | |
C2 | 0.8492 (5) | 0.7850 (6) | −0.0116 (4) | 0.036 (2) | |
H2 | 0.8389 | 0.7125 | −0.0301 | 0.043* | |
C3 | 0.8767 (5) | 0.8146 (7) | 0.0640 (5) | 0.043 (2) | |
H3 | 0.8913 | 0.7668 | 0.1073 | 0.052* | |
C4 | 0.8986 (5) | 0.9214 (7) | 0.0659 (5) | 0.047 (2) | |
H4 | 0.9282 | 0.9625 | 0.1112 | 0.056* | |
C5 | 0.8792 (5) | 0.9577 (6) | −0.0065 (5) | 0.038 (2) | |
H5 | 0.8921 | 1.0296 | −0.0211 | 0.045* | |
C6 | 0.8239 (7) | 1.0134 (7) | −0.1946 (5) | 0.059 (3) | |
H6A | 0.8135 | 1.0135 | −0.2483 | 0.089* | |
H6B | 0.8872 | 1.0477 | −0.1721 | 0.089* | |
H6C | 0.7688 | 1.0502 | −0.1811 | 0.089* | |
C7 | 0.7155 (7) | 0.8014 (8) | −0.2078 (5) | 0.075 (3) | |
H7A | 0.7073 | 0.8049 | −0.2613 | 0.112* | |
H7B | 0.6560 | 0.8297 | −0.1951 | 0.112* | |
H7C | 0.7244 | 0.7295 | −0.1917 | 0.112* | |
C8 | 1.0928 (6) | 0.7687 (7) | −0.2336 (5) | 0.058 (2) | |
H8A | 1.0564 | 0.7781 | −0.2851 | 0.087* | |
H8B | 1.1447 | 0.7163 | −0.2308 | 0.087* | |
H8C | 1.1239 | 0.8340 | −0.2140 | 0.087* | |
C9 | 0.9298 (6) | 0.6120 (7) | −0.2181 (5) | 0.058 (2) | |
H9A | 0.8984 | 0.6250 | −0.2702 | 0.087* | |
H9B | 0.8780 | 0.5984 | −0.1915 | 0.087* | |
H9C | 0.9741 | 0.5521 | −0.2139 | 0.087* | |
C10 | 1.0660 (5) | 0.7055 (6) | −0.0771 (4) | 0.0343 (19) | |
C11 | 1.1382 (5) | 0.7707 (5) | −0.0324 (5) | 0.037 (2) | |
H11 | 1.1680 | 0.8328 | −0.0506 | 0.044* | |
C12 | 1.1548 (6) | 0.7411 (6) | 0.0444 (5) | 0.042 (2) | |
H12 | 1.1949 | 0.7793 | 0.0881 | 0.050* | |
C13 | 1.0875 (6) | 0.6586 (6) | 0.0454 (5) | 0.039 (2) | |
H13 | 1.0756 | 0.6255 | 0.0908 | 0.047* | |
C14 | 1.0370 (5) | 0.6349 (6) | −0.0261 (4) | 0.0345 (19) | |
H14 | 0.9825 | 0.5825 | −0.0399 | 0.041* | |
C15 | 1.3511 (6) | 0.7164 (7) | −0.0068 (7) | 0.060 (3) | |
H15 | 1.3569 | 0.7867 | 0.0156 | 0.072* | |
C16 | 1.3172 (7) | 0.6940 (9) | −0.0805 (7) | 0.066 (3) | |
H16 | 1.2943 | 0.7461 | −0.1204 | 0.079* | |
C17 | 1.3332 (7) | 0.5913 (11) | −0.0921 (7) | 0.078 (4) | |
H17 | 1.3237 | 0.5567 | −0.1411 | 0.094* | |
C18 | 1.3758 (7) | 0.5468 (8) | −0.0234 (8) | 0.071 (3) | |
H18 | 1.4021 | 0.4749 | −0.0148 | 0.085* | |
C19 | 1.3884 (6) | 0.6252 (10) | 0.0295 (6) | 0.070 (3) | |
H19 | 1.4246 | 0.6189 | 0.0826 | 0.084* | |
C20 | 0.6674 (7) | 0.7321 (6) | 0.0457 (7) | 0.060 (3) | |
H20 | 0.7120 | 0.6755 | 0.0708 | 0.072* | |
C21 | 0.6211 (7) | 0.8042 (7) | 0.0799 (5) | 0.054 (2) | |
H21 | 0.6276 | 0.8092 | 0.1343 | 0.065* | |
C22 | 0.5554 (6) | 0.8621 (7) | 0.0262 (6) | 0.057 (3) | |
H22 | 0.5071 | 0.9148 | 0.0356 | 0.068* | |
C23 | 0.5592 (7) | 0.8231 (8) | −0.0425 (6) | 0.058 (3) | |
H23 | 0.5146 | 0.8432 | −0.0911 | 0.069* | |
C24 | 0.6303 (7) | 0.7428 (7) | −0.0304 (6) | 0.058 (3) | |
H24 | 0.6439 | 0.6952 | −0.0690 | 0.070* | |
C1S | 1.5728 (9) | 0.4814 (9) | −0.2543 (5) | 0.092 (4) | |
H1SA | 1.6399 | 0.5129 | −0.2384 | 0.110* | |
H1SB | 1.5466 | 0.4979 | −0.3072 | 0.110* | |
Cl1S | 1.4992 (3) | 0.5352 (4) | −0.2076 (2) | 0.1503 (18) | |
Cl2S | 1.5860 (3) | 0.3417 (4) | −0.2446 (2) | 0.1600 (18) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ti1 | 0.0282 (7) | 0.0270 (8) | 0.0448 (9) | 0.0026 (6) | 0.0157 (6) | 0.0008 (7) |
Ti2 | 0.0270 (7) | 0.0279 (8) | 0.0488 (9) | 0.0003 (6) | 0.0144 (6) | −0.0004 (7) |
Cl1 | 0.0422 (12) | 0.0438 (12) | 0.0549 (14) | 0.0125 (10) | 0.0197 (10) | 0.0123 (10) |
Cl2 | 0.0545 (13) | 0.0422 (12) | 0.0560 (14) | −0.0040 (10) | 0.0291 (11) | −0.0103 (11) |
Cl3 | 0.0415 (12) | 0.0356 (11) | 0.0549 (13) | 0.0021 (9) | 0.0145 (10) | −0.0094 (10) |
Cl4 | 0.0425 (12) | 0.0411 (12) | 0.0516 (13) | 0.0026 (10) | 0.0103 (10) | 0.0083 (10) |
Si1 | 0.0433 (13) | 0.0508 (15) | 0.0425 (14) | 0.0127 (12) | 0.0130 (11) | 0.0014 (12) |
Si2 | 0.0439 (14) | 0.0456 (14) | 0.0433 (14) | 0.0082 (11) | 0.0188 (11) | 0.0007 (12) |
O | 0.056 (4) | 0.057 (4) | 0.050 (4) | 0.025 (3) | 0.022 (3) | 0.004 (3) |
C1 | 0.028 (4) | 0.035 (5) | 0.047 (5) | 0.004 (4) | 0.017 (4) | 0.002 (4) |
C2 | 0.025 (4) | 0.037 (5) | 0.050 (6) | 0.013 (4) | 0.019 (4) | −0.009 (4) |
C3 | 0.034 (5) | 0.056 (6) | 0.040 (5) | 0.017 (4) | 0.010 (4) | 0.015 (4) |
C4 | 0.027 (4) | 0.069 (7) | 0.046 (6) | −0.002 (4) | 0.014 (4) | −0.007 (5) |
C5 | 0.029 (4) | 0.037 (5) | 0.054 (6) | −0.006 (4) | 0.023 (4) | −0.002 (4) |
C6 | 0.073 (6) | 0.065 (6) | 0.046 (6) | 0.019 (5) | 0.026 (5) | 0.020 (5) |
C7 | 0.070 (7) | 0.105 (9) | 0.048 (6) | −0.006 (6) | 0.013 (5) | −0.022 (6) |
C8 | 0.059 (6) | 0.065 (6) | 0.059 (6) | 0.005 (5) | 0.029 (5) | −0.005 (5) |
C9 | 0.054 (6) | 0.075 (7) | 0.046 (5) | −0.005 (5) | 0.010 (4) | −0.006 (5) |
C10 | 0.029 (4) | 0.030 (4) | 0.048 (5) | 0.006 (4) | 0.018 (4) | 0.002 (4) |
C11 | 0.033 (4) | 0.016 (4) | 0.066 (6) | 0.002 (3) | 0.022 (4) | −0.006 (4) |
C12 | 0.044 (5) | 0.034 (5) | 0.048 (6) | 0.006 (4) | 0.013 (4) | −0.014 (4) |
C13 | 0.041 (5) | 0.038 (5) | 0.042 (5) | 0.010 (4) | 0.019 (4) | 0.005 (4) |
C14 | 0.029 (4) | 0.027 (4) | 0.052 (6) | 0.005 (3) | 0.020 (4) | 0.000 (4) |
C15 | 0.034 (5) | 0.045 (6) | 0.105 (9) | −0.010 (5) | 0.022 (5) | −0.014 (6) |
C16 | 0.044 (6) | 0.073 (8) | 0.090 (9) | 0.001 (5) | 0.037 (6) | 0.032 (7) |
C17 | 0.035 (6) | 0.122 (11) | 0.091 (9) | −0.026 (7) | 0.040 (6) | −0.038 (9) |
C18 | 0.028 (5) | 0.041 (6) | 0.151 (12) | 0.003 (4) | 0.035 (6) | 0.002 (7) |
C19 | 0.017 (5) | 0.112 (10) | 0.076 (7) | −0.025 (6) | 0.000 (4) | 0.016 (7) |
C20 | 0.048 (6) | 0.024 (5) | 0.112 (9) | −0.002 (4) | 0.026 (6) | 0.016 (5) |
C21 | 0.060 (6) | 0.050 (6) | 0.061 (6) | −0.015 (5) | 0.033 (5) | 0.010 (5) |
C22 | 0.027 (5) | 0.045 (6) | 0.108 (9) | 0.003 (4) | 0.036 (5) | 0.016 (6) |
C23 | 0.047 (6) | 0.058 (7) | 0.063 (7) | −0.026 (5) | 0.005 (5) | 0.014 (5) |
C24 | 0.051 (6) | 0.048 (6) | 0.081 (8) | −0.022 (5) | 0.029 (5) | −0.021 (6) |
C1S | 0.114 (10) | 0.106 (10) | 0.046 (6) | 0.003 (8) | 0.002 (6) | −0.028 (7) |
Cl1S | 0.095 (3) | 0.250 (5) | 0.106 (3) | 0.023 (3) | 0.024 (2) | −0.001 (3) |
Cl2S | 0.142 (4) | 0.234 (6) | 0.105 (3) | −0.020 (4) | 0.030 (3) | −0.047 (3) |
Ti1—C3 | 2.351 (7) | Si1—C1 | 1.876 (8) |
Ti1—C20 | 2.356 (8) | Si2—O | 1.633 (5) |
Ti1—C24 | 2.358 (8) | Si2—C9 | 1.832 (9) |
Ti1—Cl1 | 2.360 (2) | Si2—C8 | 1.861 (8) |
Ti1—C21 | 2.369 (8) | Si2—C10 | 1.872 (8) |
Ti1—Cl2 | 2.373 (2) | C1—C2 | 1.415 (10) |
Ti1—C22 | 2.374 (7) | C1—C5 | 1.421 (10) |
Ti1—C2 | 2.381 (7) | C2—C3 | 1.411 (10) |
Ti1—C23 | 2.389 (8) | C3—C4 | 1.404 (11) |
Ti1—C5 | 2.406 (7) | C4—C5 | 1.383 (11) |
Ti1—C1 | 2.408 (7) | C10—C11 | 1.402 (10) |
Ti1—C4 | 2.408 (8) | C10—C14 | 1.432 (10) |
Ti2—C16 | 2.347 (8) | C11—C12 | 1.436 (11) |
Ti2—Cl3 | 2.362 (2) | C12—C13 | 1.405 (10) |
Ti2—C11 | 2.366 (7) | C13—C14 | 1.370 (10) |
Ti2—C15 | 2.370 (8) | C15—C16 | 1.361 (13) |
Ti2—C12 | 2.370 (7) | C15—C19 | 1.386 (13) |
Ti2—C18 | 2.376 (8) | C16—C17 | 1.363 (14) |
Ti2—C17 | 2.378 (9) | C17—C18 | 1.388 (14) |
Ti2—Cl4 | 2.381 (2) | C18—C19 | 1.386 (14) |
Ti2—C14 | 2.389 (7) | C20—C21 | 1.362 (12) |
Ti2—C19 | 2.388 (8) | C20—C24 | 1.383 (13) |
Ti2—C10 | 2.403 (7) | C21—C22 | 1.383 (11) |
Ti2—C13 | 2.411 (7) | C22—C23 | 1.379 (12) |
Si1—O | 1.633 (5) | C23—C24 | 1.398 (12) |
Si1—C6 | 1.849 (8) | C1S—Cl1S | 1.629 (11) |
Si1—C7 | 1.852 (9) | C1S—Cl2S | 1.810 (12) |
C3—Ti1—C20 | 78.9 (3) | C12—Ti2—C19 | 98.0 (4) |
C3—Ti1—C24 | 96.7 (3) | C18—Ti2—C19 | 33.8 (3) |
C20—Ti1—C24 | 34.1 (3) | C17—Ti2—C19 | 56.0 (4) |
C3—Ti1—Cl1 | 137.6 (2) | Cl4—Ti2—C19 | 80.8 (3) |
C20—Ti1—Cl1 | 134.1 (3) | C14—Ti2—C19 | 154.4 (4) |
C24—Ti1—Cl1 | 102.9 (3) | C16—Ti2—C10 | 93.1 (3) |
C3—Ti1—C21 | 98.5 (3) | Cl3—Ti2—C10 | 85.31 (19) |
C20—Ti1—C21 | 33.5 (3) | C11—Ti2—C10 | 34.2 (2) |
C24—Ti1—C21 | 56.0 (3) | C15—Ti2—C10 | 105.4 (3) |
Cl1—Ti1—C21 | 123.7 (2) | C12—Ti2—C10 | 58.4 (3) |
C3—Ti1—Cl2 | 98.9 (2) | C18—Ti2—C10 | 147.1 (4) |
C20—Ti1—Cl2 | 109.7 (3) | C17—Ti2—C10 | 113.7 (4) |
C24—Ti1—Cl2 | 135.1 (2) | Cl4—Ti2—C10 | 129.83 (18) |
Cl1—Ti1—Cl2 | 93.25 (9) | C14—Ti2—C10 | 34.8 (2) |
C21—Ti1—Cl2 | 80.1 (2) | C19—Ti2—C10 | 138.9 (4) |
C3—Ti1—C22 | 131.9 (3) | C16—Ti2—C13 | 132.7 (4) |
C20—Ti1—C22 | 56.4 (3) | Cl3—Ti2—C13 | 108.7 (2) |
C24—Ti1—C22 | 56.5 (3) | C11—Ti2—C13 | 56.5 (3) |
Cl1—Ti1—C22 | 89.8 (2) | C15—Ti2—C13 | 114.2 (3) |
C21—Ti1—C22 | 33.9 (3) | C12—Ti2—C13 | 34.2 (3) |
Cl2—Ti1—C22 | 82.4 (3) | C18—Ti2—C13 | 152.3 (4) |
C3—Ti1—C2 | 34.7 (3) | C17—Ti2—C13 | 166.0 (4) |
C20—Ti1—C2 | 78.7 (3) | Cl4—Ti2—C13 | 76.9 (2) |
C24—Ti1—C2 | 77.7 (3) | C14—Ti2—C13 | 33.2 (2) |
Cl1—Ti1—C2 | 114.7 (2) | C19—Ti2—C13 | 122.6 (4) |
C21—Ti1—C2 | 110.2 (3) | C10—Ti2—C13 | 56.9 (3) |
Cl2—Ti1—C2 | 132.1 (2) | O—Si1—C6 | 106.4 (4) |
C22—Ti1—C2 | 132.3 (3) | O—Si1—C7 | 109.5 (4) |
C3—Ti1—C23 | 130.7 (3) | C6—Si1—C7 | 112.9 (4) |
C20—Ti1—C23 | 56.5 (3) | O—Si1—C1 | 105.2 (3) |
C24—Ti1—C23 | 34.3 (3) | C6—Si1—C1 | 110.9 (4) |
Cl1—Ti1—C23 | 78.0 (2) | C7—Si1—C1 | 111.5 (4) |
C21—Ti1—C23 | 55.9 (3) | O—Si2—C9 | 110.4 (4) |
Cl2—Ti1—C23 | 114.2 (3) | O—Si2—C8 | 105.2 (4) |
C22—Ti1—C23 | 33.6 (3) | C9—Si2—C8 | 112.3 (4) |
C2—Ti1—C23 | 109.4 (3) | O—Si2—C10 | 103.9 (3) |
C3—Ti1—C5 | 56.7 (3) | C9—Si2—C10 | 111.4 (4) |
C20—Ti1—C5 | 132.9 (3) | C8—Si2—C10 | 113.1 (4) |
C24—Ti1—C5 | 130.0 (3) | Si2—O—Si1 | 151.5 (4) |
Cl1—Ti1—C5 | 82.2 (2) | C2—C1—C5 | 105.5 (7) |
C21—Ti1—C5 | 153.3 (3) | C2—C1—Si1 | 127.2 (6) |
Cl2—Ti1—C5 | 93.2 (2) | C5—C1—Si1 | 126.7 (6) |
C22—Ti1—C5 | 170.7 (3) | C2—C1—Ti1 | 71.8 (4) |
C2—Ti1—C5 | 56.2 (3) | C5—C1—Ti1 | 72.8 (4) |
C23—Ti1—C5 | 146.7 (3) | Si1—C1—Ti1 | 126.8 (4) |
C3—Ti1—C1 | 57.9 (3) | C3—C2—C1 | 109.3 (7) |
C20—Ti1—C1 | 110.1 (3) | C3—C2—Ti1 | 71.5 (4) |
C24—Ti1—C1 | 96.2 (3) | C1—C2—Ti1 | 73.9 (4) |
Cl1—Ti1—C1 | 82.57 (19) | C4—C3—C2 | 107.0 (7) |
C21—Ti1—C1 | 143.3 (3) | C4—C3—Ti1 | 75.1 (5) |
Cl2—Ti1—C1 | 127.6 (2) | C2—C3—Ti1 | 73.8 (4) |
C22—Ti1—C1 | 149.3 (3) | C5—C4—C3 | 108.5 (8) |
C2—Ti1—C1 | 34.4 (2) | C5—C4—Ti1 | 73.3 (4) |
C23—Ti1—C1 | 115.8 (3) | C3—C4—Ti1 | 70.6 (4) |
C5—Ti1—C1 | 34.3 (2) | C4—C5—C1 | 109.6 (7) |
C3—Ti1—C4 | 34.3 (3) | C4—C5—Ti1 | 73.4 (4) |
C20—Ti1—C4 | 111.2 (3) | C1—C5—Ti1 | 72.9 (4) |
C24—Ti1—C4 | 130.4 (3) | C11—C10—C14 | 104.9 (7) |
Cl1—Ti1—C4 | 112.3 (2) | C11—C10—Si2 | 126.1 (6) |
C21—Ti1—C4 | 120.3 (3) | C14—C10—Si2 | 127.8 (6) |
Cl2—Ti1—C4 | 77.7 (2) | C11—C10—Ti2 | 71.5 (4) |
C22—Ti1—C4 | 150.7 (3) | C14—C10—Ti2 | 72.0 (4) |
C2—Ti1—C4 | 56.4 (3) | Si2—C10—Ti2 | 130.1 (4) |
C23—Ti1—C4 | 164.6 (3) | C10—C11—C12 | 110.2 (7) |
C5—Ti1—C4 | 33.4 (3) | C10—C11—Ti2 | 74.4 (4) |
C1—Ti1—C4 | 56.8 (3) | C12—C11—Ti2 | 72.5 (4) |
C16—Ti2—Cl3 | 103.4 (3) | C13—C12—C11 | 105.4 (7) |
C16—Ti2—C11 | 78.0 (3) | C13—C12—Ti2 | 74.5 (4) |
Cl3—Ti2—C11 | 118.4 (2) | C11—C12—Ti2 | 72.2 (4) |
C16—Ti2—C15 | 33.5 (3) | C14—C13—C12 | 109.5 (7) |
Cl3—Ti2—C15 | 134.4 (3) | C14—C13—Ti2 | 72.5 (4) |
C11—Ti2—C15 | 76.0 (3) | C12—C13—Ti2 | 71.3 (4) |
C16—Ti2—C12 | 100.3 (4) | C13—C14—C10 | 109.9 (7) |
Cl3—Ti2—C12 | 137.4 (2) | C13—C14—Ti2 | 74.3 (4) |
C11—Ti2—C12 | 35.3 (3) | C10—C14—Ti2 | 73.2 (4) |
C15—Ti2—C12 | 80.7 (3) | C16—C15—C19 | 107.7 (9) |
C16—Ti2—C18 | 56.1 (3) | C16—C15—Ti2 | 72.3 (5) |
Cl3—Ti2—C18 | 90.8 (3) | C19—C15—Ti2 | 73.8 (5) |
C11—Ti2—C18 | 130.8 (3) | C15—C16—C17 | 109.5 (10) |
C15—Ti2—C18 | 56.3 (3) | C15—C16—Ti2 | 74.1 (5) |
C12—Ti2—C18 | 131.7 (4) | C17—C16—Ti2 | 74.5 (5) |
C16—Ti2—C17 | 33.5 (3) | C16—C17—C18 | 107.6 (10) |
Cl3—Ti2—C17 | 79.0 (3) | C16—C17—Ti2 | 72.0 (5) |
C11—Ti2—C17 | 109.7 (4) | C18—C17—Ti2 | 72.9 (6) |
C15—Ti2—C17 | 55.9 (3) | C19—C18—C17 | 107.5 (9) |
C12—Ti2—C17 | 133.3 (4) | C19—C18—Ti2 | 73.6 (5) |
C18—Ti2—C17 | 33.9 (3) | C17—C18—Ti2 | 73.1 (5) |
C16—Ti2—Cl4 | 135.5 (3) | C18—C19—C15 | 107.7 (9) |
Cl3—Ti2—Cl4 | 92.76 (8) | C18—C19—Ti2 | 72.6 (5) |
C11—Ti2—Cl4 | 129.3 (2) | C15—C19—Ti2 | 72.3 (5) |
C15—Ti2—Cl4 | 111.0 (3) | C21—C20—C24 | 108.0 (9) |
C12—Ti2—Cl4 | 94.6 (2) | C21—C20—Ti1 | 73.8 (5) |
C18—Ti2—Cl4 | 82.9 (3) | C24—C20—Ti1 | 73.0 (5) |
C17—Ti2—Cl4 | 115.0 (4) | C20—C21—C22 | 109.0 (9) |
C16—Ti2—C14 | 127.8 (3) | C20—C21—Ti1 | 72.7 (5) |
Cl3—Ti2—C14 | 80.7 (2) | C22—C21—Ti1 | 73.3 (5) |
C11—Ti2—C14 | 56.4 (2) | C23—C22—C21 | 107.7 (8) |
C15—Ti2—C14 | 131.8 (3) | C23—C22—Ti1 | 73.7 (5) |
C12—Ti2—C14 | 56.9 (3) | C21—C22—Ti1 | 72.8 (4) |
C18—Ti2—C14 | 171.3 (3) | C22—C23—C24 | 107.5 (9) |
C17—Ti2—C14 | 143.9 (4) | C22—C23—Ti1 | 72.6 (5) |
Cl4—Ti2—C14 | 95.39 (19) | C24—C23—Ti1 | 71.7 (5) |
C16—Ti2—C19 | 55.8 (3) | C20—C24—C23 | 107.8 (9) |
Cl3—Ti2—C19 | 124.6 (3) | C20—C24—Ti1 | 72.9 (5) |
C11—Ti2—C19 | 106.9 (4) | C23—C24—Ti1 | 74.1 (5) |
C15—Ti2—C19 | 33.9 (3) | Cl1S—C1S—Cl2S | 115.3 (8) |
C9—Si2—O—Si1 | 47.0 (9) | Ti2—C13—C14—C10 | −65.1 (5) |
C8—Si2—O—Si1 | 168.3 (8) | C12—C13—C14—Ti2 | 62.1 (5) |
C10—Si2—O—Si1 | −72.6 (9) | C11—C10—C14—C13 | 1.4 (8) |
C6—Si1—O—Si2 | −175.9 (8) | Si2—C10—C14—C13 | −166.9 (5) |
C7—Si1—O—Si2 | −53.6 (9) | Ti2—C10—C14—C13 | 65.8 (5) |
C1—Si1—O—Si2 | 66.4 (9) | C11—C10—C14—Ti2 | −64.4 (5) |
O—Si1—C1—C2 | −69.2 (7) | Si2—C10—C14—Ti2 | 127.3 (6) |
C6—Si1—C1—C2 | 176.2 (6) | C16—Ti2—C14—C13 | −112.5 (6) |
C7—Si1—C1—C2 | 49.5 (8) | Cl3—Ti2—C14—C13 | 147.8 (5) |
O—Si1—C1—C5 | 100.7 (7) | C11—Ti2—C14—C13 | −78.7 (5) |
C6—Si1—C1—C5 | −13.9 (8) | C15—Ti2—C14—C13 | −68.7 (7) |
C7—Si1—C1—C5 | −140.6 (7) | C12—Ti2—C14—C13 | −36.1 (5) |
O—Si1—C1—Ti1 | −163.7 (4) | C18—Ti2—C14—C13 | 134 (3) |
C6—Si1—C1—Ti1 | 81.7 (5) | C17—Ti2—C14—C13 | −155.8 (7) |
C7—Si1—C1—Ti1 | −45.0 (6) | Cl4—Ti2—C14—C13 | 55.9 (5) |
C3—Ti1—C1—C2 | 36.6 (4) | C19—Ti2—C14—C13 | −24.0 (10) |
C20—Ti1—C1—C2 | −25.2 (6) | C10—Ti2—C14—C13 | −117.0 (7) |
C24—Ti1—C1—C2 | −57.4 (5) | C16—Ti2—C14—C10 | 4.5 (7) |
Cl1—Ti1—C1—C2 | −159.6 (4) | Cl3—Ti2—C14—C10 | −95.2 (4) |
C21—Ti1—C1—C2 | −20.0 (7) | C11—Ti2—C14—C10 | 38.3 (4) |
Cl2—Ti1—C1—C2 | 112.0 (4) | C15—Ti2—C14—C10 | 48.3 (7) |
C22—Ti1—C1—C2 | −82.6 (7) | C12—Ti2—C14—C10 | 80.8 (5) |
C23—Ti1—C1—C2 | −86.8 (5) | C18—Ti2—C14—C10 | −109 (3) |
C5—Ti1—C1—C2 | 113.3 (6) | C17—Ti2—C14—C10 | −38.8 (8) |
C4—Ti1—C1—C2 | 77.6 (5) | Cl4—Ti2—C14—C10 | 172.9 (4) |
C3—Ti1—C1—C5 | −76.7 (5) | C19—Ti2—C14—C10 | 93.0 (8) |
C20—Ti1—C1—C5 | −138.6 (5) | C13—Ti2—C14—C10 | 117.0 (7) |
C24—Ti1—C1—C5 | −170.7 (5) | Cl3—Ti2—C15—C16 | 27.0 (8) |
Cl1—Ti1—C1—C5 | 87.1 (4) | C11—Ti2—C15—C16 | −89.3 (7) |
C21—Ti1—C1—C5 | −133.3 (6) | C12—Ti2—C15—C16 | −125.1 (7) |
Cl2—Ti1—C1—C5 | −1.3 (5) | C18—Ti2—C15—C16 | 78.0 (7) |
C22—Ti1—C1—C5 | 164.1 (6) | C17—Ti2—C15—C16 | 36.8 (6) |
C2—Ti1—C1—C5 | −113.3 (6) | Cl4—Ti2—C15—C16 | 143.5 (6) |
C23—Ti1—C1—C5 | 159.8 (5) | C14—Ti2—C15—C16 | −97.9 (7) |
C4—Ti1—C1—C5 | −35.7 (4) | C19—Ti2—C15—C16 | 115.1 (9) |
C3—Ti1—C1—Si1 | 160.0 (6) | C10—Ti2—C15—C16 | −71.7 (6) |
C20—Ti1—C1—Si1 | 98.1 (5) | C13—Ti2—C15—C16 | −131.9 (6) |
C24—Ti1—C1—Si1 | 65.9 (5) | C16—Ti2—C15—C19 | −115.1 (9) |
Cl1—Ti1—C1—Si1 | −36.3 (4) | Cl3—Ti2—C15—C19 | −88.1 (8) |
C21—Ti1—C1—Si1 | 103.4 (6) | C11—Ti2—C15—C19 | 155.6 (8) |
Cl2—Ti1—C1—Si1 | −124.7 (4) | C12—Ti2—C15—C19 | 119.8 (7) |
C22—Ti1—C1—Si1 | 40.7 (8) | C18—Ti2—C15—C19 | −37.1 (6) |
C2—Ti1—C1—Si1 | 123.3 (7) | C17—Ti2—C15—C19 | −78.3 (7) |
C23—Ti1—C1—Si1 | 36.5 (6) | Cl4—Ti2—C15—C19 | 28.4 (7) |
C5—Ti1—C1—Si1 | −123.4 (7) | C14—Ti2—C15—C19 | 147.0 (6) |
C4—Ti1—C1—Si1 | −159.1 (6) | C10—Ti2—C15—C19 | 173.2 (7) |
C5—C1—C2—C3 | 2.4 (8) | C13—Ti2—C15—C19 | 113.0 (7) |
Si1—C1—C2—C3 | 174.0 (5) | C19—C15—C16—C17 | −0.8 (10) |
Ti1—C1—C2—C3 | −63.1 (5) | Ti2—C15—C16—C17 | −66.7 (6) |
C5—C1—C2—Ti1 | 65.5 (5) | C19—C15—C16—Ti2 | 65.9 (6) |
Si1—C1—C2—Ti1 | −122.9 (6) | Cl3—Ti2—C16—C15 | −160.5 (6) |
C20—Ti1—C2—C3 | −86.7 (6) | C11—Ti2—C16—C15 | 82.7 (7) |
C24—Ti1—C2—C3 | −121.6 (6) | C12—Ti2—C16—C15 | 55.2 (7) |
Cl1—Ti1—C2—C3 | 139.7 (4) | C18—Ti2—C16—C15 | −78.7 (7) |
C21—Ti1—C2—C3 | −75.2 (5) | C17—Ti2—C16—C15 | −116.1 (9) |
Cl2—Ti1—C2—C3 | 19.7 (6) | Cl4—Ti2—C16—C15 | −52.3 (8) |
C22—Ti1—C2—C3 | −105.8 (6) | C14—Ti2—C16—C15 | 111.0 (6) |
C23—Ti1—C2—C3 | −134.9 (5) | C19—Ti2—C16—C15 | −37.6 (6) |
C5—Ti1—C2—C3 | 78.9 (5) | C10—Ti2—C16—C15 | 113.5 (6) |
C1—Ti1—C2—C3 | 117.4 (7) | C13—Ti2—C16—C15 | 67.5 (7) |
C4—Ti1—C2—C3 | 38.5 (5) | Cl3—Ti2—C16—C17 | −44.5 (8) |
C3—Ti1—C2—C1 | −117.4 (7) | C11—Ti2—C16—C17 | −161.2 (8) |
C20—Ti1—C2—C1 | 155.9 (5) | C15—Ti2—C16—C17 | 116.1 (9) |
C24—Ti1—C2—C1 | 121.0 (5) | C12—Ti2—C16—C17 | 171.2 (8) |
Cl1—Ti1—C2—C1 | 22.4 (5) | C18—Ti2—C16—C17 | 37.3 (6) |
C21—Ti1—C2—C1 | 167.4 (5) | Cl4—Ti2—C16—C17 | 63.7 (10) |
Cl2—Ti1—C2—C1 | −97.7 (5) | C14—Ti2—C16—C17 | −133.0 (7) |
C22—Ti1—C2—C1 | 136.8 (5) | C19—Ti2—C16—C17 | 78.5 (7) |
C23—Ti1—C2—C1 | 107.7 (5) | C10—Ti2—C16—C17 | −130.4 (8) |
C5—Ti1—C2—C1 | −38.5 (4) | C13—Ti2—C16—C17 | −176.4 (7) |
C4—Ti1—C2—C1 | −78.9 (5) | C15—C16—C17—C18 | 1.7 (10) |
C1—C2—C3—C4 | −3.7 (8) | Ti2—C16—C17—C18 | −64.7 (6) |
Ti1—C2—C3—C4 | −68.3 (5) | C15—C16—C17—Ti2 | 66.5 (6) |
C1—C2—C3—Ti1 | 64.7 (5) | Cl3—Ti2—C17—C16 | 136.0 (8) |
C20—Ti1—C3—C4 | −160.7 (6) | C11—Ti2—C17—C16 | 19.5 (8) |
C24—Ti1—C3—C4 | 170.0 (5) | C15—Ti2—C17—C16 | −36.8 (6) |
Cl1—Ti1—C3—C4 | 52.6 (6) | C12—Ti2—C17—C16 | −11.9 (10) |
C21—Ti1—C3—C4 | −133.4 (5) | C18—Ti2—C17—C16 | −115.7 (9) |
Cl2—Ti1—C3—C4 | −52.2 (5) | Cl4—Ti2—C17—C16 | −136.1 (7) |
C22—Ti1—C3—C4 | −139.9 (6) | C14—Ti2—C17—C16 | 79.2 (8) |
C2—Ti1—C3—C4 | 113.1 (7) | C19—Ti2—C17—C16 | −78.0 (7) |
C23—Ti1—C3—C4 | 174.8 (5) | C10—Ti2—C17—C16 | 56.2 (8) |
C5—Ti1—C3—C4 | 35.8 (5) | C13—Ti2—C17—C16 | 10.9 (19) |
C1—Ti1—C3—C4 | 76.9 (5) | C16—Ti2—C17—C18 | 115.7 (9) |
C20—Ti1—C3—C2 | 86.2 (5) | Cl3—Ti2—C17—C18 | −108.3 (7) |
C24—Ti1—C3—C2 | 56.9 (5) | C11—Ti2—C17—C18 | 135.2 (7) |
Cl1—Ti1—C3—C2 | −60.5 (6) | C15—Ti2—C17—C18 | 78.8 (6) |
C21—Ti1—C3—C2 | 113.5 (5) | C12—Ti2—C17—C18 | 103.7 (9) |
Cl2—Ti1—C3—C2 | −165.3 (4) | Cl4—Ti2—C17—C18 | −20.4 (8) |
C22—Ti1—C3—C2 | 107.0 (6) | C14—Ti2—C17—C18 | −165.2 (6) |
C23—Ti1—C3—C2 | 61.7 (6) | C19—Ti2—C17—C18 | 37.6 (6) |
C5—Ti1—C3—C2 | −77.3 (5) | C10—Ti2—C17—C18 | 171.8 (6) |
C1—Ti1—C3—C2 | −36.3 (4) | C13—Ti2—C17—C18 | 126.6 (15) |
C4—Ti1—C3—C2 | −113.1 (7) | C16—C17—C18—C19 | −2.0 (10) |
C2—C3—C4—C5 | 3.5 (8) | Ti2—C17—C18—C19 | −66.1 (6) |
Ti1—C3—C4—C5 | −63.9 (5) | C16—C17—C18—Ti2 | 64.1 (6) |
C2—C3—C4—Ti1 | 67.5 (5) | C16—Ti2—C18—C19 | 77.7 (7) |
C3—Ti1—C4—C5 | 117.1 (7) | Cl3—Ti2—C18—C19 | −176.7 (7) |
C20—Ti1—C4—C5 | 137.5 (5) | C11—Ti2—C18—C19 | 53.4 (10) |
C24—Ti1—C4—C5 | 104.1 (6) | C15—Ti2—C18—C19 | 37.1 (6) |
Cl1—Ti1—C4—C5 | −27.5 (5) | C12—Ti2—C18—C19 | 5.9 (10) |
C21—Ti1—C4—C5 | 173.5 (5) | C17—Ti2—C18—C19 | 114.6 (9) |
Cl2—Ti1—C4—C5 | −115.9 (5) | Cl4—Ti2—C18—C19 | −84.0 (7) |
C22—Ti1—C4—C5 | −163.9 (6) | C14—Ti2—C18—C19 | −163 (2) |
C2—Ti1—C4—C5 | 78.2 (5) | C10—Ti2—C18—C19 | 100.7 (10) |
C23—Ti1—C4—C5 | 102.3 (13) | C13—Ti2—C18—C19 | −40.8 (10) |
C1—Ti1—C4—C5 | 36.8 (4) | C16—Ti2—C18—C17 | −36.9 (6) |
C20—Ti1—C4—C3 | 20.3 (6) | Cl3—Ti2—C18—C17 | 68.7 (7) |
C24—Ti1—C4—C3 | −13.0 (7) | C11—Ti2—C18—C17 | −61.2 (9) |
Cl1—Ti1—C4—C3 | −144.6 (4) | C15—Ti2—C18—C17 | −77.5 (7) |
C21—Ti1—C4—C3 | 56.3 (6) | C12—Ti2—C18—C17 | −108.7 (8) |
Cl2—Ti1—C4—C3 | 126.9 (5) | Cl4—Ti2—C18—C17 | 161.4 (7) |
C22—Ti1—C4—C3 | 78.9 (8) | C14—Ti2—C18—C17 | 82 (2) |
C2—Ti1—C4—C3 | −38.9 (5) | C19—Ti2—C18—C17 | −114.6 (9) |
C23—Ti1—C4—C3 | −14.9 (14) | C10—Ti2—C18—C17 | −13.9 (11) |
C5—Ti1—C4—C3 | −117.1 (7) | C13—Ti2—C18—C17 | −155.4 (8) |
C1—Ti1—C4—C3 | −80.4 (5) | C17—C18—C19—C15 | 1.5 (10) |
C3—C4—C5—C1 | −2.1 (8) | Ti2—C18—C19—C15 | −64.3 (6) |
Ti1—C4—C5—C1 | −64.4 (5) | C17—C18—C19—Ti2 | 65.8 (6) |
C3—C4—C5—Ti1 | 62.2 (5) | C16—C15—C19—C18 | −0.5 (10) |
C2—C1—C5—C4 | −0.2 (8) | Ti2—C15—C19—C18 | 64.4 (6) |
Si1—C1—C5—C4 | −171.8 (5) | C16—C15—C19—Ti2 | −64.9 (6) |
Ti1—C1—C5—C4 | 64.7 (5) | C16—Ti2—C19—C18 | −78.6 (7) |
C2—C1—C5—Ti1 | −64.8 (5) | Cl3—Ti2—C19—C18 | 4.1 (8) |
Si1—C1—C5—Ti1 | 123.5 (6) | C11—Ti2—C19—C18 | −140.5 (7) |
C3—Ti1—C5—C4 | −36.8 (5) | C15—Ti2—C19—C18 | −115.7 (9) |
C20—Ti1—C5—C4 | −59.3 (7) | C12—Ti2—C19—C18 | −175.6 (7) |
C24—Ti1—C5—C4 | −105.2 (6) | C17—Ti2—C19—C18 | −37.8 (6) |
Cl1—Ti1—C5—C4 | 154.5 (5) | Cl4—Ti2—C19—C18 | 91.0 (7) |
C21—Ti1—C5—C4 | −12.6 (9) | C14—Ti2—C19—C18 | 174.2 (7) |
Cl2—Ti1—C5—C4 | 61.6 (5) | C10—Ti2—C19—C18 | −125.7 (8) |
C22—Ti1—C5—C4 | 123 (2) | C13—Ti2—C19—C18 | 158.9 (6) |
C2—Ti1—C5—C4 | −78.8 (5) | C16—Ti2—C19—C15 | 37.2 (6) |
C23—Ti1—C5—C4 | −151.8 (6) | Cl3—Ti2—C19—C15 | 119.8 (7) |
C1—Ti1—C5—C4 | −117.3 (7) | C11—Ti2—C19—C15 | −24.8 (8) |
C3—Ti1—C5—C1 | 80.5 (5) | C12—Ti2—C19—C15 | −59.8 (7) |
C20—Ti1—C5—C1 | 58.0 (7) | C18—Ti2—C19—C15 | 115.7 (9) |
C24—Ti1—C5—C1 | 12.1 (7) | C17—Ti2—C19—C15 | 78.0 (7) |
Cl1—Ti1—C5—C1 | −88.2 (4) | Cl4—Ti2—C19—C15 | −153.2 (7) |
C21—Ti1—C5—C1 | 104.7 (7) | C14—Ti2—C19—C15 | −70.1 (10) |
Cl2—Ti1—C5—C1 | 179.0 (4) | C10—Ti2—C19—C15 | −10.0 (10) |
C22—Ti1—C5—C1 | −120 (2) | C13—Ti2—C19—C15 | −85.4 (7) |
C2—Ti1—C5—C1 | 38.6 (4) | C3—Ti1—C20—C21 | 124.7 (7) |
C23—Ti1—C5—C1 | −34.5 (8) | C24—Ti1—C20—C21 | −115.1 (8) |
C4—Ti1—C5—C1 | 117.3 (7) | Cl1—Ti1—C20—C21 | −86.4 (7) |
O—Si2—C10—C11 | −70.4 (7) | Cl2—Ti1—C20—C21 | 29.2 (7) |
C9—Si2—C10—C11 | 170.8 (6) | C22—Ti1—C20—C21 | −36.8 (6) |
C8—Si2—C10—C11 | 43.2 (7) | C2—Ti1—C20—C21 | 160.1 (7) |
O—Si2—C10—C14 | 95.6 (7) | C23—Ti1—C20—C21 | −77.4 (6) |
C9—Si2—C10—C14 | −23.2 (7) | C5—Ti1—C20—C21 | 143.7 (5) |
C8—Si2—C10—C14 | −150.8 (6) | C1—Ti1—C20—C21 | 174.3 (6) |
O—Si2—C10—Ti2 | −166.1 (4) | C4—Ti1—C20—C21 | 113.2 (6) |
C9—Si2—C10—Ti2 | 75.1 (5) | C3—Ti1—C20—C24 | −120.2 (6) |
C8—Si2—C10—Ti2 | −52.5 (6) | Cl1—Ti1—C20—C24 | 28.8 (7) |
C16—Ti2—C10—C11 | −63.2 (6) | C21—Ti1—C20—C24 | 115.1 (8) |
Cl3—Ti2—C10—C11 | −166.4 (4) | Cl2—Ti1—C20—C24 | 144.3 (5) |
C15—Ti2—C10—C11 | −31.5 (5) | C22—Ti1—C20—C24 | 78.4 (6) |
C12—Ti2—C10—C11 | 37.0 (4) | C2—Ti1—C20—C24 | −84.8 (6) |
C18—Ti2—C10—C11 | −82.1 (8) | C23—Ti1—C20—C24 | 37.7 (5) |
C17—Ti2—C10—C11 | −90.5 (5) | C5—Ti1—C20—C24 | −101.2 (6) |
Cl4—Ti2—C10—C11 | 104.0 (4) | C1—Ti1—C20—C24 | −70.6 (6) |
C14—Ti2—C10—C11 | 113.2 (6) | C4—Ti1—C20—C24 | −131.7 (6) |
C19—Ti2—C10—C11 | −25.7 (7) | C24—C20—C21—C22 | −0.7 (9) |
C13—Ti2—C10—C11 | 77.7 (5) | Ti1—C20—C21—C22 | 64.8 (6) |
C16—Ti2—C10—C14 | −176.4 (5) | C24—C20—C21—Ti1 | −65.5 (6) |
Cl3—Ti2—C10—C14 | 80.4 (4) | C3—Ti1—C21—C20 | −54.6 (7) |
C11—Ti2—C10—C14 | −113.2 (6) | C24—Ti1—C21—C20 | 37.8 (6) |
C15—Ti2—C10—C14 | −144.7 (5) | Cl1—Ti1—C21—C20 | 120.5 (6) |
C12—Ti2—C10—C14 | −76.3 (5) | Cl2—Ti1—C21—C20 | −152.2 (6) |
C18—Ti2—C10—C14 | 164.6 (6) | C22—Ti1—C21—C20 | 116.7 (9) |
C17—Ti2—C10—C14 | 156.2 (5) | C2—Ti1—C21—C20 | −20.8 (7) |
Cl4—Ti2—C10—C14 | −9.3 (5) | C23—Ti1—C21—C20 | 79.4 (6) |
C19—Ti2—C10—C14 | −139.0 (6) | C5—Ti1—C21—C20 | −75.0 (9) |
C13—Ti2—C10—C14 | −35.6 (4) | C1—Ti1—C21—C20 | −9.0 (9) |
C16—Ti2—C10—Si2 | 58.8 (6) | C4—Ti1—C21—C20 | −82.9 (7) |
Cl3—Ti2—C10—Si2 | −44.4 (4) | C3—Ti1—C21—C22 | −171.4 (6) |
C11—Ti2—C10—Si2 | 122.0 (7) | C20—Ti1—C21—C22 | −116.7 (9) |
C15—Ti2—C10—Si2 | 90.5 (5) | C24—Ti1—C21—C22 | −78.9 (6) |
C12—Ti2—C10—Si2 | 158.9 (6) | Cl1—Ti1—C21—C22 | 3.8 (7) |
C18—Ti2—C10—Si2 | 39.9 (9) | Cl2—Ti1—C21—C22 | 91.1 (6) |
C17—Ti2—C10—Si2 | 31.4 (6) | C2—Ti1—C21—C22 | −137.5 (6) |
Cl4—Ti2—C10—Si2 | −134.1 (4) | C23—Ti1—C21—C22 | −37.3 (5) |
C14—Ti2—C10—Si2 | −124.8 (7) | C5—Ti1—C21—C22 | 168.3 (6) |
C19—Ti2—C10—Si2 | 96.2 (6) | C1—Ti1—C21—C22 | −125.7 (7) |
C13—Ti2—C10—Si2 | −160.4 (6) | C4—Ti1—C21—C22 | 160.3 (6) |
C14—C10—C11—C12 | 0.6 (8) | C20—C21—C22—C23 | 1.6 (9) |
Si2—C10—C11—C12 | 169.2 (5) | Ti1—C21—C22—C23 | 66.0 (6) |
Ti2—C10—C11—C12 | −64.2 (5) | C20—C21—C22—Ti1 | −64.4 (6) |
C14—C10—C11—Ti2 | 64.8 (5) | C3—Ti1—C22—C23 | −103.5 (7) |
Si2—C10—C11—Ti2 | −126.7 (5) | C20—Ti1—C22—C23 | −78.7 (6) |
C16—Ti2—C11—C10 | 114.3 (5) | C24—Ti1—C22—C23 | −37.4 (6) |
Cl3—Ti2—C11—C10 | 15.5 (5) | Cl1—Ti1—C22—C23 | 68.2 (6) |
C15—Ti2—C11—C10 | 148.7 (5) | C21—Ti1—C22—C23 | −115.0 (8) |
C12—Ti2—C11—C10 | −117.6 (6) | Cl2—Ti1—C22—C23 | 161.5 (6) |
C18—Ti2—C11—C10 | 134.8 (6) | C2—Ti1—C22—C23 | −56.1 (7) |
C17—Ti2—C11—C10 | 103.5 (5) | C5—Ti1—C22—C23 | 99 (2) |
Cl4—Ti2—C11—C10 | −105.5 (4) | C1—Ti1—C22—C23 | −6.9 (9) |
C14—Ti2—C11—C10 | −39.0 (4) | C4—Ti1—C22—C23 | −151.4 (7) |
C19—Ti2—C11—C10 | 162.6 (5) | C3—Ti1—C22—C21 | 11.5 (8) |
C13—Ti2—C11—C10 | −79.0 (5) | C20—Ti1—C22—C21 | 36.3 (5) |
C16—Ti2—C11—C12 | −128.0 (5) | C24—Ti1—C22—C21 | 77.5 (6) |
Cl3—Ti2—C11—C12 | 133.2 (4) | Cl1—Ti1—C22—C21 | −176.9 (6) |
C15—Ti2—C11—C12 | −93.6 (5) | Cl2—Ti1—C22—C21 | −83.6 (6) |
C18—Ti2—C11—C12 | −107.6 (6) | C2—Ti1—C22—C21 | 58.9 (8) |
C17—Ti2—C11—C12 | −138.9 (5) | C23—Ti1—C22—C21 | 115.0 (8) |
Cl4—Ti2—C11—C12 | 12.2 (5) | C5—Ti1—C22—C21 | −145.7 (19) |
C14—Ti2—C11—C12 | 78.7 (5) | C1—Ti1—C22—C21 | 108.1 (8) |
C19—Ti2—C11—C12 | −79.7 (5) | C4—Ti1—C22—C21 | −36.5 (9) |
C10—Ti2—C11—C12 | 117.6 (6) | C21—C22—C23—C24 | −1.8 (9) |
C13—Ti2—C11—C12 | 38.6 (4) | Ti1—C22—C23—C24 | 63.6 (6) |
C10—C11—C12—C13 | −2.4 (8) | C21—C22—C23—Ti1 | −65.4 (6) |
Ti2—C11—C12—C13 | −67.7 (5) | C3—Ti1—C23—C22 | 107.3 (6) |
C10—C11—C12—Ti2 | 65.4 (5) | C20—Ti1—C23—C22 | 78.2 (6) |
C16—Ti2—C12—C13 | 163.7 (5) | C24—Ti1—C23—C22 | 115.8 (8) |
Cl3—Ti2—C12—C13 | 40.8 (6) | Cl1—Ti1—C23—C22 | −108.4 (6) |
C11—Ti2—C12—C13 | 112.2 (6) | C21—Ti1—C23—C22 | 37.6 (5) |
C15—Ti2—C12—C13 | −168.9 (6) | Cl2—Ti1—C23—C22 | −20.2 (6) |
C18—Ti2—C12—C13 | −143.0 (6) | C2—Ti1—C23—C22 | 139.4 (6) |
C17—Ti2—C12—C13 | 170.4 (6) | C5—Ti1—C23—C22 | −163.1 (5) |
Cl4—Ti2—C12—C13 | −58.4 (5) | C1—Ti1—C23—C22 | 176.1 (5) |
C14—Ti2—C12—C13 | 35.1 (4) | C4—Ti1—C23—C22 | 118.3 (13) |
C19—Ti2—C12—C13 | −139.7 (5) | C3—Ti1—C23—C24 | −8.5 (8) |
C10—Ti2—C12—C13 | 76.5 (5) | C20—Ti1—C23—C24 | −37.6 (5) |
C16—Ti2—C12—C11 | 51.5 (5) | Cl1—Ti1—C23—C24 | 135.8 (6) |
Cl3—Ti2—C12—C11 | −71.4 (5) | C21—Ti1—C23—C24 | −78.2 (6) |
C15—Ti2—C12—C11 | 78.9 (5) | Cl2—Ti1—C23—C24 | −136.0 (6) |
C18—Ti2—C12—C11 | 104.8 (6) | C22—Ti1—C23—C24 | −115.8 (8) |
C17—Ti2—C12—C11 | 58.2 (7) | C2—Ti1—C23—C24 | 23.6 (7) |
Cl4—Ti2—C12—C11 | −170.6 (4) | C5—Ti1—C23—C24 | 81.0 (8) |
C14—Ti2—C12—C11 | −77.2 (5) | C1—Ti1—C23—C24 | 60.3 (7) |
C19—Ti2—C12—C11 | 108.1 (5) | C4—Ti1—C23—C24 | 2.5 (16) |
C10—Ti2—C12—C11 | −35.8 (4) | C21—C20—C24—C23 | −0.4 (10) |
C13—Ti2—C12—C11 | −112.2 (6) | Ti1—C20—C24—C23 | −66.4 (6) |
C11—C12—C13—C14 | 3.2 (8) | C21—C20—C24—Ti1 | 66.0 (6) |
Ti2—C12—C13—C14 | −62.9 (5) | C22—C23—C24—C20 | 1.3 (9) |
C11—C12—C13—Ti2 | 66.1 (5) | Ti1—C23—C24—C20 | 65.6 (6) |
C16—Ti2—C13—C14 | 96.4 (6) | C22—C23—C24—Ti1 | −64.2 (6) |
Cl3—Ti2—C13—C14 | −33.7 (5) | C3—Ti1—C24—C20 | 58.7 (6) |
C11—Ti2—C13—C14 | 78.5 (5) | Cl1—Ti1—C24—C20 | −159.2 (5) |
C15—Ti2—C13—C14 | 130.5 (5) | C21—Ti1—C24—C20 | −37.1 (5) |
C12—Ti2—C13—C14 | 118.4 (7) | Cl2—Ti1—C24—C20 | −51.1 (7) |
C18—Ti2—C13—C14 | −166.4 (6) | C22—Ti1—C24—C20 | −78.1 (6) |
C17—Ti2—C13—C14 | 88.3 (15) | C2—Ti1—C24—C20 | 87.9 (6) |
Cl4—Ti2—C13—C14 | −122.2 (5) | C23—Ti1—C24—C20 | −114.9 (8) |
C19—Ti2—C13—C14 | 168.0 (5) | C5—Ti1—C24—C20 | 110.2 (6) |
C10—Ti2—C13—C14 | 37.3 (4) | C1—Ti1—C24—C20 | 117.0 (6) |
C16—Ti2—C13—C12 | −22.0 (7) | C4—Ti1—C24—C20 | 66.0 (7) |
Cl3—Ti2—C13—C12 | −152.2 (4) | C3—Ti1—C24—C23 | 173.5 (6) |
C11—Ti2—C13—C12 | −39.9 (4) | C20—Ti1—C24—C23 | 114.9 (8) |
C15—Ti2—C13—C12 | 12.0 (6) | Cl1—Ti1—C24—C23 | −44.4 (6) |
C18—Ti2—C13—C12 | 75.1 (8) | C21—Ti1—C24—C23 | 77.8 (6) |
C17—Ti2—C13—C12 | −30.2 (16) | Cl2—Ti1—C24—C23 | 63.8 (8) |
Cl4—Ti2—C13—C12 | 119.4 (5) | C22—Ti1—C24—C23 | 36.7 (5) |
C14—Ti2—C13—C12 | −118.4 (7) | C2—Ti1—C24—C23 | −157.3 (7) |
C19—Ti2—C13—C12 | 49.5 (6) | C5—Ti1—C24—C23 | −135.0 (6) |
C10—Ti2—C13—C12 | −81.1 (5) | C1—Ti1—C24—C23 | −128.1 (6) |
C12—C13—C14—C10 | −3.0 (8) | C4—Ti1—C24—C23 | −179.1 (5) |
[TiCl2(C10H15)(C7H10Si)]2O | F(000) = 1608 |
Mr = 768.52 | Dx = 1.313 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
a = 8.1319 (1) Å | Cell parameters from 8192 reflections |
b = 22.2503 (3) Å | θ = 2–25° |
c = 21.6970 (3) Å | µ = 0.77 mm−1 |
β = 97.97 (1)° | T = 223 K |
V = 3887.84 (9) Å3 | Plate, brown |
Z = 4 | 0.38 × 0.20 × 0.10 mm |
Bruker CCD area detector diffractometer | 6849 independent reflections |
Radiation source: normal-focus sealed tube | 4852 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.11 |
ϕ and ω scans | θmax = 25°, θmin = 1.3° |
Absorption correction: empirical (using intensity measurements) (SADABS; Blessing, 1995) | h = −9→9 |
Tmin = 0.76, Tmax = 0.93 | k = −26→26 |
62999 measured reflections | l = −25→25 |
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)] = 0.051 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.122 | H-atom parameters constrained |
S = 1.02 | w = 1/[σ2(Fo2) + (0.0451P)2 + 6.1721P] where P = (Fo2 + 2Fc2)/3 |
6849 reflections | (Δ/σ)max < 0.001 |
388 parameters | Δρmax = 0.72 e Å−3 |
0 restraints | Δρmin = −0.51 e Å−3 |
[TiCl2(C10H15)(C7H10Si)]2O | V = 3887.84 (9) Å3 |
Mr = 768.52 | Z = 4 |
Monoclinic, P21/n | Mo Kα radiation |
a = 8.1319 (1) Å | µ = 0.77 mm−1 |
b = 22.2503 (3) Å | T = 223 K |
c = 21.6970 (3) Å | 0.38 × 0.20 × 0.10 mm |
β = 97.97 (1)° |
Bruker CCD area detector diffractometer | 6849 independent reflections |
Absorption correction: empirical (using intensity measurements) (SADABS; Blessing, 1995) | 4852 reflections with I > 2σ(I) |
Tmin = 0.76, Tmax = 0.93 | Rint = 0.11 |
62999 measured reflections |
R[F2 > 2σ(F2)] = 0.051 | 0 restraints |
wR(F2) = 0.122 | H-atom parameters constrained |
S = 1.02 | Δρmax = 0.72 e Å−3 |
6849 reflections | Δρmin = −0.51 e Å−3 |
388 parameters |
Experimental. Data were collected by the double-pass method using the CCD area detector system. The first 50 frames of data were re-collected at the end of data collection and no crystal decay was observed for either compound. |
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. The structures were solved by the Patterson method and refined successfully in the monoclinic space groups P21/c and P21/n. Full matrix least-squares refinement was carried out by minimizing w(Fo2-Fc2)2. The non-H atoms were refined anisotropically to convergence. H atoms were treated using appropriate riding models [SHELXTL-Plus command AFIX = m3 (Sheldrick, 1999)], where the atomic position of the H atom rides on the coordinates of the non-H atom to which it is attached and the displacement parameters are fixed at 1.2 times those of the parent atom. |
x | y | z | Uiso*/Ueq | ||
Ti1 | 0.09992 (8) | 0.23619 (3) | 0.56643 (3) | 0.02936 (17) | |
Ti2 | 0.24721 (8) | −0.02970 (3) | 0.22787 (3) | 0.02984 (17) | |
Cl1 | 0.16455 (17) | 0.24427 (5) | 0.46548 (5) | 0.0614 (3) | |
Cl2 | 0.37801 (13) | 0.22898 (6) | 0.61567 (6) | 0.0628 (3) | |
Cl3 | −0.00893 (12) | −0.07319 (5) | 0.24167 (5) | 0.0500 (3) | |
Cl4 | 0.13230 (18) | 0.06215 (5) | 0.19172 (5) | 0.0646 (4) | |
Si1 | 0.23902 (14) | 0.08699 (5) | 0.49426 (5) | 0.0378 (3) | |
Si2 | 0.11684 (16) | 0.08288 (5) | 0.34899 (5) | 0.0451 (3) | |
O | 0.1351 (4) | 0.08264 (13) | 0.42481 (12) | 0.0513 (7) | |
C1 | 0.0997 (4) | 0.12825 (15) | 0.54177 (17) | 0.0340 (8) | |
C2 | −0.0584 (5) | 0.15257 (17) | 0.5210 (2) | 0.0428 (10) | |
H2 | −0.1144 | 0.1510 | 0.4776 | 0.051* | |
C3 | −0.1311 (5) | 0.17388 (17) | 0.5715 (2) | 0.0454 (10) | |
H3 | −0.2475 | 0.1873 | 0.5702 | 0.054* | |
C4 | −0.0169 (5) | 0.16387 (17) | 0.6255 (2) | 0.0474 (11) | |
H4 | −0.0396 | 0.1690 | 0.6688 | 0.057* | |
C5 | 0.1211 (5) | 0.13468 (16) | 0.60723 (18) | 0.0410 (9) | |
H5 | 0.2163 | 0.1188 | 0.6360 | 0.049* | |
C6 | 0.2655 (6) | 0.00979 (19) | 0.5272 (2) | 0.0604 (13) | |
H6A | 0.3372 | −0.0133 | 0.5038 | 0.091* | |
H6B | 0.1580 | −0.0097 | 0.5244 | 0.091* | |
H6C | 0.3151 | 0.0121 | 0.5704 | 0.091* | |
C7 | 0.4443 (5) | 0.1224 (2) | 0.4932 (3) | 0.0643 (14) | |
H7A | 0.5086 | 0.0984 | 0.4677 | 0.096* | |
H7B | 0.5024 | 0.1246 | 0.5353 | 0.096* | |
H7C | 0.4295 | 0.1625 | 0.4759 | 0.096* | |
C8 | −0.1016 (6) | 0.0623 (2) | 0.3222 (2) | 0.0623 (13) | |
H8A | −0.1743 | 0.0934 | 0.3343 | 0.093* | |
H8B | −0.1269 | 0.0244 | 0.3410 | 0.093* | |
H8C | −0.1183 | 0.0582 | 0.2773 | 0.093* | |
C9 | 0.1717 (8) | 0.1581 (2) | 0.3219 (2) | 0.087 (2) | |
H9A | 0.0932 | 0.1875 | 0.3334 | 0.131* | |
H9B | 0.1678 | 0.1576 | 0.2771 | 0.131* | |
H9C | 0.2828 | 0.1686 | 0.3412 | 0.131* | |
C10 | 0.2673 (5) | 0.02466 (16) | 0.32742 (16) | 0.0361 (9) | |
C11 | 0.4158 (5) | 0.0329 (2) | 0.30025 (18) | 0.0481 (11) | |
H11 | 0.4611 | 0.0724 | 0.2900 | 0.058* | |
C12 | 0.4979 (5) | −0.0221 (2) | 0.29673 (19) | 0.0501 (11) | |
H12 | 0.6112 | −0.0279 | 0.2860 | 0.060* | |
C13 | 0.3986 (5) | −0.0665 (2) | 0.32073 (18) | 0.0472 (11) | |
H13 | 0.4307 | −0.1090 | 0.3292 | 0.057* | |
C14 | 0.2627 (5) | −0.03741 (17) | 0.34053 (16) | 0.0384 (9) | |
H14 | 0.1784 | −0.0572 | 0.3625 | 0.046* | |
C15 | 0.2905 (5) | −0.02847 (17) | 0.11831 (17) | 0.0370 (9) | |
C16 | 0.1763 (5) | −0.07428 (18) | 0.12539 (17) | 0.0389 (9) | |
C17 | 0.2602 (5) | −0.11872 (17) | 0.16513 (18) | 0.0408 (10) | |
C18 | 0.4253 (5) | −0.09906 (17) | 0.18274 (18) | 0.0397 (9) | |
C19 | 0.4415 (4) | −0.04183 (17) | 0.15572 (17) | 0.0359 (9) | |
C20 | 0.1447 (6) | 0.34273 (18) | 0.5823 (2) | 0.0559 (13) | |
C21 | 0.0982 (5) | 0.3183 (2) | 0.6381 (2) | 0.0525 (12) | |
C22 | −0.0682 (5) | 0.29836 (17) | 0.62398 (18) | 0.0390 (9) | |
C23 | −0.1180 (5) | 0.30941 (17) | 0.56017 (19) | 0.0413 (10) | |
C24 | 0.0110 (6) | 0.33824 (18) | 0.5357 (2) | 0.0510 (11) | |
C25 | −0.2910 (6) | 0.3024 (2) | 0.5251 (2) | 0.0682 (14) | |
H25A | −0.3548 | 0.3385 | 0.5300 | 0.102* | |
H25B | −0.3450 | 0.2682 | 0.5414 | 0.102* | |
H25C | −0.2842 | 0.2961 | 0.4813 | 0.102* | |
C26 | −0.1821 (6) | 0.2808 (2) | 0.6702 (2) | 0.0609 (13) | |
H26A | −0.2319 | 0.3166 | 0.6851 | 0.091* | |
H26B | −0.1189 | 0.2599 | 0.7049 | 0.091* | |
H26C | −0.2687 | 0.2545 | 0.6501 | 0.091* | |
C27 | 0.1952 (7) | 0.3200 (3) | 0.7022 (3) | 0.100 (2) | |
H27A | 0.1743 | 0.3577 | 0.7221 | 0.150* | |
H27B | 0.3128 | 0.3165 | 0.6992 | 0.150* | |
H27C | 0.1612 | 0.2869 | 0.7266 | 0.150* | |
C28 | 0.3088 (7) | 0.3733 (2) | 0.5762 (3) | 0.100 (2) | |
H28A | 0.2999 | 0.4160 | 0.5845 | 0.150* | |
H28B | 0.3353 | 0.3676 | 0.5344 | 0.150* | |
H28C | 0.3959 | 0.3560 | 0.6060 | 0.150* | |
C29 | −0.0034 (8) | 0.3663 (2) | 0.4714 (3) | 0.087 (2) | |
H29A | −0.0418 | 0.4075 | 0.4733 | 0.131* | |
H29B | −0.0819 | 0.3435 | 0.4428 | 0.131* | |
H29C | 0.1044 | 0.3659 | 0.4571 | 0.131* | |
C30 | 0.2629 (6) | 0.0230 (2) | 0.0728 (2) | 0.0615 (13) | |
H30A | 0.2905 | 0.0103 | 0.0327 | 0.092* | |
H30B | 0.3330 | 0.0566 | 0.0881 | 0.092* | |
H30C | 0.1474 | 0.0353 | 0.0683 | 0.092* | |
C31 | 0.0027 (5) | −0.0781 (3) | 0.0914 (2) | 0.0687 (15) | |
H31A | 0.0044 | −0.0976 | 0.0516 | 0.103* | |
H31B | −0.0427 | −0.0379 | 0.0849 | 0.103* | |
H31C | −0.0659 | −0.1012 | 0.1160 | 0.103* | |
C32 | 0.1937 (7) | −0.17945 (19) | 0.1789 (3) | 0.0712 (15) | |
H32A | 0.2143 | −0.2076 | 0.1467 | 0.107* | |
H32B | 0.0751 | −0.1766 | 0.1801 | 0.107* | |
H32C | 0.2486 | −0.1934 | 0.2189 | 0.107* | |
C33 | 0.5640 (6) | −0.1379 (2) | 0.2145 (2) | 0.0600 (13) | |
H33A | 0.6121 | −0.1609 | 0.1834 | 0.090* | |
H33B | 0.5203 | −0.1652 | 0.2431 | 0.090* | |
H33C | 0.6487 | −0.1126 | 0.2373 | 0.090* | |
C34 | 0.5985 (5) | −0.0058 (2) | 0.1549 (2) | 0.0584 (12) | |
H34A | 0.6553 | −0.0195 | 0.1211 | 0.088* | |
H34B | 0.6704 | −0.0111 | 0.1941 | 0.088* | |
H34C | 0.5707 | 0.0364 | 0.1491 | 0.088* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ti1 | 0.0277 (3) | 0.0269 (3) | 0.0346 (4) | −0.0016 (3) | 0.0080 (3) | −0.0030 (3) |
Ti2 | 0.0316 (3) | 0.0288 (3) | 0.0286 (4) | 0.0009 (3) | 0.0020 (3) | 0.0002 (3) |
Cl1 | 0.1001 (9) | 0.0443 (6) | 0.0483 (7) | 0.0088 (6) | 0.0396 (6) | 0.0034 (5) |
Cl2 | 0.0336 (6) | 0.0637 (7) | 0.0877 (9) | −0.0020 (5) | −0.0039 (6) | −0.0093 (7) |
Cl3 | 0.0349 (5) | 0.0729 (8) | 0.0427 (6) | −0.0091 (5) | 0.0070 (4) | −0.0054 (5) |
Cl4 | 0.1140 (10) | 0.0410 (6) | 0.0389 (6) | 0.0304 (6) | 0.0109 (6) | 0.0043 (5) |
Si1 | 0.0444 (6) | 0.0309 (6) | 0.0388 (6) | 0.0026 (5) | 0.0078 (5) | −0.0049 (5) |
Si2 | 0.0692 (8) | 0.0336 (6) | 0.0340 (6) | −0.0006 (6) | 0.0124 (6) | −0.0021 (5) |
O | 0.073 (2) | 0.0480 (17) | 0.0329 (16) | −0.0034 (15) | 0.0091 (14) | −0.0074 (13) |
C1 | 0.037 (2) | 0.0240 (19) | 0.040 (2) | −0.0014 (16) | 0.0038 (17) | −0.0041 (16) |
C2 | 0.037 (2) | 0.034 (2) | 0.056 (3) | −0.0100 (18) | −0.0026 (19) | −0.0104 (19) |
C3 | 0.033 (2) | 0.033 (2) | 0.072 (3) | −0.0104 (17) | 0.015 (2) | −0.004 (2) |
C4 | 0.066 (3) | 0.033 (2) | 0.049 (3) | −0.005 (2) | 0.027 (2) | 0.0013 (19) |
C5 | 0.053 (2) | 0.030 (2) | 0.040 (2) | 0.0025 (18) | 0.0068 (19) | 0.0037 (17) |
C6 | 0.074 (3) | 0.044 (3) | 0.064 (3) | 0.017 (2) | 0.010 (3) | 0.001 (2) |
C7 | 0.053 (3) | 0.047 (3) | 0.097 (4) | 0.001 (2) | 0.024 (3) | −0.011 (3) |
C8 | 0.066 (3) | 0.077 (3) | 0.043 (3) | 0.017 (3) | 0.005 (2) | −0.008 (2) |
C9 | 0.170 (6) | 0.041 (3) | 0.060 (3) | −0.013 (3) | 0.048 (4) | −0.005 (2) |
C10 | 0.046 (2) | 0.036 (2) | 0.026 (2) | −0.0096 (18) | 0.0009 (17) | −0.0043 (16) |
C11 | 0.050 (3) | 0.057 (3) | 0.036 (2) | −0.024 (2) | 0.0035 (19) | −0.010 (2) |
C12 | 0.032 (2) | 0.074 (3) | 0.040 (2) | −0.002 (2) | −0.0067 (18) | −0.011 (2) |
C13 | 0.052 (3) | 0.051 (3) | 0.033 (2) | 0.011 (2) | −0.0087 (19) | 0.0044 (19) |
C14 | 0.048 (2) | 0.040 (2) | 0.025 (2) | −0.0042 (19) | −0.0011 (17) | 0.0009 (17) |
C15 | 0.045 (2) | 0.036 (2) | 0.031 (2) | 0.0046 (18) | 0.0118 (18) | −0.0012 (17) |
C16 | 0.041 (2) | 0.046 (2) | 0.030 (2) | 0.0000 (19) | 0.0054 (17) | −0.0109 (18) |
C17 | 0.051 (2) | 0.030 (2) | 0.045 (2) | −0.0051 (18) | 0.018 (2) | −0.0083 (18) |
C18 | 0.044 (2) | 0.037 (2) | 0.040 (2) | 0.0107 (18) | 0.0117 (18) | 0.0019 (18) |
C19 | 0.034 (2) | 0.038 (2) | 0.037 (2) | −0.0009 (17) | 0.0107 (17) | −0.0049 (17) |
C20 | 0.059 (3) | 0.028 (2) | 0.090 (4) | −0.009 (2) | 0.043 (3) | −0.020 (2) |
C21 | 0.054 (3) | 0.047 (3) | 0.056 (3) | 0.006 (2) | 0.006 (2) | −0.028 (2) |
C22 | 0.045 (2) | 0.034 (2) | 0.042 (2) | 0.0027 (18) | 0.0182 (19) | −0.0029 (18) |
C23 | 0.042 (2) | 0.033 (2) | 0.052 (3) | 0.0129 (18) | 0.0197 (19) | 0.0040 (19) |
C24 | 0.064 (3) | 0.032 (2) | 0.063 (3) | 0.009 (2) | 0.031 (3) | 0.007 (2) |
C25 | 0.054 (3) | 0.077 (4) | 0.071 (3) | 0.025 (3) | 0.001 (2) | 0.020 (3) |
C26 | 0.077 (3) | 0.054 (3) | 0.060 (3) | 0.007 (2) | 0.040 (3) | −0.002 (2) |
C27 | 0.088 (4) | 0.130 (6) | 0.076 (4) | 0.009 (4) | −0.008 (3) | −0.062 (4) |
C28 | 0.072 (4) | 0.049 (3) | 0.191 (7) | −0.024 (3) | 0.065 (4) | −0.031 (4) |
C29 | 0.125 (5) | 0.059 (3) | 0.093 (4) | 0.034 (3) | 0.069 (4) | 0.036 (3) |
C30 | 0.084 (3) | 0.064 (3) | 0.040 (3) | 0.019 (3) | 0.021 (2) | 0.017 (2) |
C31 | 0.048 (3) | 0.109 (4) | 0.047 (3) | −0.011 (3) | 0.000 (2) | −0.028 (3) |
C32 | 0.088 (4) | 0.033 (2) | 0.101 (4) | −0.013 (2) | 0.045 (3) | −0.007 (3) |
C33 | 0.061 (3) | 0.057 (3) | 0.064 (3) | 0.026 (2) | 0.015 (2) | 0.011 (2) |
C34 | 0.045 (3) | 0.066 (3) | 0.066 (3) | −0.009 (2) | 0.018 (2) | 0.003 (3) |
Ti1—Cl1 | 2.3291 (12) | Si2—C10 | 1.885 (4) |
Ti1—C4 | 2.339 (4) | C1—C2 | 1.410 (5) |
Ti1—C3 | 2.349 (4) | C1—C5 | 1.414 (5) |
Ti1—Cl2 | 2.3687 (12) | C2—C3 | 1.397 (6) |
Ti1—C2 | 2.395 (4) | C3—C4 | 1.408 (6) |
Ti1—C23 | 2.397 (4) | C4—C5 | 1.401 (5) |
Ti1—C21 | 2.399 (4) | C10—C14 | 1.412 (5) |
Ti1—C22 | 2.411 (4) | C10—C11 | 1.427 (5) |
Ti1—C20 | 2.416 (4) | C11—C12 | 1.401 (6) |
Ti1—C5 | 2.423 (4) | C12—C13 | 1.420 (6) |
Ti1—C24 | 2.447 (4) | C13—C14 | 1.399 (5) |
Ti1—C1 | 2.461 (3) | C15—C16 | 1.402 (5) |
Ti2—Cl4 | 2.3369 (12) | C15—C19 | 1.406 (5) |
Ti2—Cl3 | 2.3532 (12) | C15—C30 | 1.509 (5) |
Ti2—C13 | 2.358 (4) | C16—C17 | 1.422 (5) |
Ti2—C12 | 2.360 (4) | C16—C31 | 1.501 (6) |
Ti2—C11 | 2.385 (4) | C17—C18 | 1.414 (5) |
Ti2—C19 | 2.389 (4) | C17—C32 | 1.501 (5) |
Ti2—C17 | 2.414 (4) | C18—C19 | 1.416 (5) |
Ti2—C18 | 2.415 (4) | C18—C33 | 1.509 (5) |
Ti2—C16 | 2.430 (4) | C19—C34 | 1.509 (5) |
Ti2—C14 | 2.436 (4) | C20—C24 | 1.382 (7) |
Ti2—C15 | 2.451 (4) | C20—C21 | 1.425 (6) |
Ti2—C10 | 2.461 (4) | C20—C28 | 1.520 (6) |
Si1—O | 1.625 (3) | C21—C22 | 1.416 (6) |
Si1—C7 | 1.849 (4) | C21—C27 | 1.501 (7) |
Si1—C6 | 1.861 (4) | C22—C23 | 1.409 (6) |
Si1—C1 | 1.874 (4) | C22—C26 | 1.507 (5) |
Si2—O | 1.631 (3) | C23—C24 | 1.396 (6) |
Si2—C8 | 1.848 (5) | C23—C25 | 1.512 (6) |
Si2—C9 | 1.848 (5) | C24—C29 | 1.518 (6) |
Cl1—Ti1—C4 | 136.89 (11) | Cl4—Ti2—C10 | 80.77 (9) |
Cl1—Ti1—C3 | 112.05 (12) | Cl3—Ti2—C10 | 92.45 (9) |
C4—Ti1—C3 | 34.96 (15) | C13—Ti2—C10 | 57.14 (14) |
Cl1—Ti1—Cl2 | 95.94 (5) | C12—Ti2—C10 | 57.51 (14) |
C4—Ti1—Cl2 | 98.12 (12) | C11—Ti2—C10 | 34.20 (13) |
C3—Ti1—Cl2 | 131.18 (12) | C19—Ti2—C10 | 131.39 (13) |
Cl1—Ti1—C2 | 81.48 (11) | C17—Ti2—C10 | 153.55 (13) |
C4—Ti1—C2 | 56.97 (15) | C18—Ti2—C10 | 134.37 (13) |
C3—Ti1—C2 | 34.22 (14) | C16—Ti2—C10 | 169.15 (13) |
Cl2—Ti1—C2 | 123.90 (10) | C14—Ti2—C10 | 33.50 (12) |
Cl1—Ti1—C23 | 98.96 (10) | C15—Ti2—C10 | 147.64 (13) |
C4—Ti1—C23 | 98.35 (14) | O—Si1—C7 | 111.6 (2) |
C3—Ti1—C23 | 79.28 (14) | O—Si1—C6 | 108.56 (19) |
Cl2—Ti1—C23 | 136.36 (11) | C7—Si1—C6 | 109.9 (2) |
C2—Ti1—C23 | 98.84 (14) | O—Si1—C1 | 105.25 (16) |
Cl1—Ti1—C21 | 124.94 (13) | C7—Si1—C1 | 114.48 (19) |
C4—Ti1—C21 | 97.43 (16) | C6—Si1—C1 | 106.71 (19) |
C3—Ti1—C21 | 110.02 (15) | O—Si2—C8 | 105.38 (19) |
Cl2—Ti1—C21 | 81.40 (11) | O—Si2—C9 | 109.3 (2) |
C2—Ti1—C21 | 143.75 (15) | C8—Si2—C9 | 112.9 (3) |
C23—Ti1—C21 | 56.54 (15) | O—Si2—C10 | 106.07 (16) |
Cl1—Ti1—C22 | 131.35 (10) | C8—Si2—C10 | 112.35 (19) |
C4—Ti1—C22 | 78.96 (13) | C9—Si2—C10 | 110.5 (2) |
C3—Ti1—C22 | 78.47 (14) | Si1—O—Si2 | 153.9 (2) |
Cl2—Ti1—C22 | 112.31 (11) | C2—C1—C5 | 105.1 (3) |
C2—Ti1—C22 | 110.34 (14) | C2—C1—Si1 | 127.3 (3) |
C23—Ti1—C22 | 34.08 (13) | C5—C1—Si1 | 127.1 (3) |
C21—Ti1—C22 | 34.23 (14) | C2—C1—Ti1 | 70.6 (2) |
Cl1—Ti1—C20 | 90.51 (12) | C5—C1—Ti1 | 71.7 (2) |
C4—Ti1—C20 | 131.44 (15) | Si1—C1—Ti1 | 127.99 (18) |
C3—Ti1—C20 | 132.71 (14) | C3—C2—C1 | 110.3 (4) |
Cl2—Ti1—C20 | 83.49 (13) | C3—C2—Ti1 | 71.1 (2) |
C2—Ti1—C20 | 151.96 (17) | C1—C2—Ti1 | 75.7 (2) |
C23—Ti1—C20 | 55.73 (15) | C2—C3—C4 | 107.2 (4) |
C21—Ti1—C20 | 34.44 (16) | C2—C3—Ti1 | 74.7 (2) |
C22—Ti1—C20 | 56.53 (13) | C4—C3—Ti1 | 72.1 (2) |
Cl1—Ti1—C5 | 113.68 (10) | C5—C4—C3 | 107.4 (4) |
C4—Ti1—C5 | 34.15 (13) | C5—C4—Ti1 | 76.2 (2) |
C3—Ti1—C5 | 56.63 (14) | C3—C4—Ti1 | 72.9 (2) |
Cl2—Ti1—C5 | 75.93 (10) | C4—C5—C1 | 109.8 (4) |
C2—Ti1—C5 | 55.47 (14) | C4—C5—Ti1 | 69.6 (2) |
C23—Ti1—C5 | 131.96 (14) | C1—C5—Ti1 | 74.6 (2) |
C21—Ti1—C5 | 118.64 (15) | C14—C10—C11 | 104.9 (4) |
C22—Ti1—C5 | 111.24 (13) | C14—C10—Si2 | 125.9 (3) |
C20—Ti1—C5 | 149.42 (17) | C11—C10—Si2 | 129.1 (3) |
Cl1—Ti1—C24 | 76.64 (11) | C14—C10—Ti2 | 72.3 (2) |
C4—Ti1—C24 | 131.32 (14) | C11—C10—Ti2 | 70.0 (2) |
C3—Ti1—C24 | 110.62 (15) | Si2—C10—Ti2 | 126.09 (18) |
Cl2—Ti1—C24 | 114.42 (13) | C12—C11—C10 | 110.3 (4) |
C2—Ti1—C24 | 119.15 (16) | C12—C11—Ti2 | 71.9 (2) |
C23—Ti1—C24 | 33.47 (13) | C10—C11—Ti2 | 75.8 (2) |
C21—Ti1—C24 | 56.10 (16) | C11—C12—C13 | 106.8 (4) |
C22—Ti1—C24 | 56.05 (13) | C11—C12—Ti2 | 73.8 (2) |
C20—Ti1—C24 | 33.00 (16) | C13—C12—Ti2 | 72.4 (2) |
C5—Ti1—C24 | 165.38 (14) | C14—C13—C12 | 107.7 (4) |
Cl1—Ti1—C1 | 82.20 (9) | C14—C13—Ti2 | 76.1 (2) |
C4—Ti1—C1 | 57.29 (13) | C12—C13—Ti2 | 72.6 (2) |
C3—Ti1—C1 | 57.16 (13) | C13—C14—C10 | 110.3 (4) |
Cl2—Ti1—C1 | 90.21 (9) | C13—C14—Ti2 | 70.0 (2) |
C2—Ti1—C1 | 33.72 (12) | C10—C14—Ti2 | 74.2 (2) |
C23—Ti1—C1 | 132.29 (13) | C16—C15—C19 | 108.8 (3) |
C21—Ti1—C1 | 152.11 (15) | C16—C15—C30 | 125.7 (4) |
C22—Ti1—C1 | 133.57 (13) | C19—C15—C30 | 125.2 (4) |
C20—Ti1—C1 | 169.84 (13) | C16—C15—Ti2 | 72.5 (2) |
C5—Ti1—C1 | 33.65 (12) | C19—C15—Ti2 | 70.7 (2) |
C24—Ti1—C1 | 148.78 (15) | C30—C15—Ti2 | 127.9 (3) |
Cl4—Ti2—Cl3 | 94.74 (5) | C15—C16—C17 | 107.6 (3) |
Cl4—Ti2—C13 | 136.71 (11) | C15—C16—C31 | 125.4 (4) |
Cl3—Ti2—C13 | 96.59 (11) | C17—C16—C31 | 126.7 (4) |
Cl4—Ti2—C12 | 114.83 (12) | C15—C16—Ti2 | 74.1 (2) |
Cl3—Ti2—C12 | 130.60 (12) | C17—C16—Ti2 | 72.3 (2) |
C13—Ti2—C12 | 35.03 (15) | C31—C16—Ti2 | 124.0 (3) |
Cl4—Ti2—C11 | 82.94 (12) | C18—C17—C16 | 107.8 (3) |
Cl3—Ti2—C11 | 126.47 (10) | C18—C17—C32 | 125.4 (4) |
C13—Ti2—C11 | 57.03 (15) | C16—C17—C32 | 126.2 (4) |
C12—Ti2—C11 | 34.34 (15) | C18—C17—Ti2 | 73.0 (2) |
Cl4—Ti2—C19 | 98.56 (10) | C16—C17—Ti2 | 73.5 (2) |
Cl3—Ti2—C19 | 135.60 (10) | C32—C17—Ti2 | 125.5 (3) |
C13—Ti2—C19 | 101.91 (14) | C17—C18—C19 | 107.8 (3) |
C12—Ti2—C19 | 80.28 (14) | C17—C18—C33 | 124.6 (4) |
C11—Ti2—C19 | 97.21 (13) | C19—C18—C33 | 126.7 (4) |
Cl4—Ti2—C17 | 125.10 (11) | C17—C18—Ti2 | 72.9 (2) |
Cl3—Ti2—C17 | 80.96 (10) | C19—C18—Ti2 | 71.8 (2) |
C13—Ti2—C17 | 97.95 (15) | C33—C18—Ti2 | 129.3 (3) |
C12—Ti2—C17 | 108.31 (15) | C15—C19—C18 | 107.8 (3) |
C11—Ti2—C17 | 141.66 (15) | C15—C19—C34 | 123.6 (4) |
C19—Ti2—C17 | 56.85 (13) | C18—C19—C34 | 127.6 (4) |
Cl4—Ti2—C18 | 131.08 (10) | C15—C19—Ti2 | 75.6 (2) |
Cl3—Ti2—C18 | 112.34 (10) | C18—C19—Ti2 | 73.9 (2) |
C13—Ti2—C18 | 81.54 (14) | C34—C19—Ti2 | 125.8 (3) |
C12—Ti2—C18 | 77.78 (15) | C24—C20—C21 | 108.6 (4) |
C11—Ti2—C18 | 108.52 (15) | C24—C20—C28 | 125.5 (5) |
C19—Ti2—C18 | 34.27 (13) | C21—C20—C28 | 125.7 (5) |
C17—Ti2—C18 | 34.05 (13) | C24—C20—Ti1 | 74.8 (2) |
Cl4—Ti2—C16 | 90.96 (10) | C21—C20—Ti1 | 72.2 (2) |
Cl3—Ti2—C16 | 81.18 (10) | C28—C20—Ti1 | 123.0 (3) |
C13—Ti2—C16 | 132.04 (14) | C22—C21—C20 | 107.1 (4) |
C12—Ti2—C16 | 133.07 (14) | C22—C21—C27 | 124.9 (5) |
C11—Ti2—C16 | 151.97 (14) | C20—C21—C27 | 127.6 (5) |
C19—Ti2—C16 | 56.55 (13) | C22—C21—Ti1 | 73.3 (2) |
C17—Ti2—C16 | 34.15 (13) | C20—C21—Ti1 | 73.4 (2) |
C18—Ti2—C16 | 56.48 (13) | C27—C21—Ti1 | 124.7 (3) |
Cl4—Ti2—C14 | 111.16 (10) | C23—C22—C21 | 107.1 (4) |
Cl3—Ti2—C14 | 76.52 (10) | C23—C22—C26 | 125.4 (4) |
C13—Ti2—C14 | 33.88 (13) | C21—C22—C26 | 126.5 (4) |
C12—Ti2—C14 | 56.63 (14) | C23—C22—Ti1 | 72.4 (2) |
C11—Ti2—C14 | 55.63 (13) | C21—C22—Ti1 | 72.4 (2) |
C19—Ti2—C14 | 134.65 (13) | C26—C22—Ti1 | 129.8 (3) |
C17—Ti2—C14 | 120.51 (13) | C24—C23—C22 | 109.0 (4) |
C18—Ti2—C14 | 114.29 (13) | C24—C23—C25 | 123.5 (4) |
C16—Ti2—C14 | 149.54 (13) | C22—C23—C25 | 126.7 (4) |
Cl4—Ti2—C15 | 76.66 (9) | C24—C23—Ti1 | 75.2 (2) |
Cl3—Ti2—C15 | 112.14 (10) | C22—C23—Ti1 | 73.5 (2) |
C13—Ti2—C15 | 134.78 (14) | C25—C23—Ti1 | 126.0 (3) |
C12—Ti2—C15 | 112.67 (14) | C20—C24—C23 | 108.2 (4) |
C11—Ti2—C15 | 119.03 (14) | C20—C24—C29 | 126.5 (4) |
C19—Ti2—C15 | 33.75 (12) | C23—C24—C29 | 124.9 (5) |
C17—Ti2—C15 | 55.87 (13) | C20—C24—Ti1 | 72.2 (2) |
C18—Ti2—C15 | 55.87 (13) | C23—C24—Ti1 | 71.3 (2) |
C16—Ti2—C15 | 33.38 (13) | C29—C24—Ti1 | 127.9 (3) |
C14—Ti2—C15 | 168.37 (13) | ||
C7—Si1—O—Si2 | 18.4 (5) | C11—Ti2—C16—C17 | 101.8 (4) |
C6—Si1—O—Si2 | −103.0 (5) | C19—Ti2—C16—C17 | 78.8 (2) |
C1—Si1—O—Si2 | 143.1 (4) | C18—Ti2—C16—C17 | 37.5 (2) |
C8—Si2—O—Si1 | 173.2 (4) | C14—Ti2—C16—C17 | −43.7 (4) |
C9—Si2—O—Si1 | −65.3 (5) | C15—Ti2—C16—C17 | 114.9 (3) |
C10—Si2—O—Si1 | 53.9 (5) | C10—Ti2—C16—C17 | −141.4 (6) |
O—Si1—C1—C2 | −2.5 (4) | Cl4—Ti2—C16—C31 | −58.7 (4) |
C7—Si1—C1—C2 | 120.4 (4) | Cl3—Ti2—C16—C31 | 35.9 (4) |
C6—Si1—C1—C2 | −117.7 (4) | C13—Ti2—C16—C31 | 126.8 (4) |
O—Si1—C1—C5 | 168.5 (3) | C12—Ti2—C16—C31 | 175.1 (4) |
C7—Si1—C1—C5 | −68.6 (4) | C11—Ti2—C16—C31 | −135.4 (4) |
C6—Si1—C1—C5 | 53.3 (4) | C19—Ti2—C16—C31 | −158.4 (4) |
O—Si1—C1—Ti1 | −96.2 (2) | C17—Ti2—C16—C31 | 122.8 (5) |
C7—Si1—C1—Ti1 | 26.7 (3) | C18—Ti2—C16—C31 | 160.2 (4) |
C6—Si1—C1—Ti1 | 148.5 (2) | C14—Ti2—C16—C31 | 79.1 (5) |
Cl1—Ti1—C1—C2 | −86.3 (2) | C15—Ti2—C16—C31 | −122.3 (5) |
C4—Ti1—C1—C2 | 78.2 (3) | C10—Ti2—C16—C31 | −18.6 (9) |
C3—Ti1—C1—C2 | 36.3 (2) | C15—C16—C17—C18 | 0.8 (4) |
Cl2—Ti1—C1—C2 | 177.7 (2) | C31—C16—C17—C18 | 174.9 (4) |
C23—Ti1—C1—C2 | 8.7 (3) | Ti2—C16—C17—C18 | −65.5 (3) |
C21—Ti1—C1—C2 | 105.9 (3) | C15—C16—C17—C32 | −171.4 (4) |
C22—Ti1—C1—C2 | 55.9 (3) | C31—C16—C17—C32 | 2.7 (7) |
C20—Ti1—C1—C2 | −130.8 (9) | Ti2—C16—C17—C32 | 122.3 (4) |
C5—Ti1—C1—C2 | 114.1 (3) | C15—C16—C17—Ti2 | 66.3 (3) |
C24—Ti1—C1—C2 | −38.8 (4) | C31—C16—C17—Ti2 | −119.6 (4) |
Cl1—Ti1—C1—C5 | 159.6 (2) | Cl4—Ti2—C17—C18 | 113.2 (2) |
C4—Ti1—C1—C5 | −35.9 (2) | Cl3—Ti2—C17—C18 | −157.3 (2) |
C3—Ti1—C1—C5 | −77.8 (3) | C13—Ti2—C17—C18 | −61.8 (2) |
Cl2—Ti1—C1—C5 | 63.6 (2) | C12—Ti2—C17—C18 | −27.4 (3) |
C2—Ti1—C1—C5 | −114.1 (3) | C11—Ti2—C17—C18 | −17.0 (3) |
C23—Ti1—C1—C5 | −105.4 (3) | C19—Ti2—C17—C18 | 37.2 (2) |
C21—Ti1—C1—C5 | −8.1 (4) | C16—Ti2—C17—C18 | 115.1 (3) |
C22—Ti1—C1—C5 | −58.2 (3) | C14—Ti2—C17—C18 | −88.9 (2) |
C20—Ti1—C1—C5 | 115.1 (9) | C15—Ti2—C17—C18 | 78.0 (2) |
C24—Ti1—C1—C5 | −152.9 (3) | C10—Ti2—C17—C18 | −80.2 (4) |
Cl1—Ti1—C1—Si1 | 36.4 (2) | Cl4—Ti2—C17—C16 | −1.9 (3) |
C4—Ti1—C1—Si1 | −159.1 (3) | Cl3—Ti2—C17—C16 | 87.6 (2) |
C3—Ti1—C1—Si1 | 159.1 (3) | C13—Ti2—C17—C16 | −177.0 (2) |
Cl2—Ti1—C1—Si1 | −59.6 (2) | C12—Ti2—C17—C16 | −142.5 (2) |
C2—Ti1—C1—Si1 | 122.7 (4) | C11—Ti2—C17—C16 | −132.1 (3) |
C23—Ti1—C1—Si1 | 131.5 (2) | C19—Ti2—C17—C16 | −77.9 (2) |
C21—Ti1—C1—Si1 | −131.3 (3) | C18—Ti2—C17—C16 | −115.1 (3) |
C22—Ti1—C1—Si1 | 178.61 (19) | C14—Ti2—C17—C16 | 156.0 (2) |
C20—Ti1—C1—Si1 | −8.1 (11) | C15—Ti2—C17—C16 | −37.1 (2) |
C5—Ti1—C1—Si1 | −123.2 (3) | C10—Ti2—C17—C16 | 164.7 (3) |
C24—Ti1—C1—Si1 | 83.9 (3) | Cl4—Ti2—C17—C32 | −125.0 (4) |
C5—C1—C2—C3 | 0.7 (4) | Cl3—Ti2—C17—C32 | −35.5 (4) |
Si1—C1—C2—C3 | 173.3 (3) | C13—Ti2—C17—C32 | 59.9 (4) |
Ti1—C1—C2—C3 | −63.2 (3) | C12—Ti2—C17—C32 | 94.4 (4) |
C5—C1—C2—Ti1 | 63.9 (3) | C11—Ti2—C17—C32 | 104.7 (4) |
Si1—C1—C2—Ti1 | −123.5 (3) | C19—Ti2—C17—C32 | 159.0 (4) |
Cl1—Ti1—C2—C3 | −153.5 (3) | C18—Ti2—C17—C32 | 121.8 (5) |
C4—Ti1—C2—C3 | 38.5 (2) | C16—Ti2—C17—C32 | −123.1 (5) |
Cl2—Ti1—C2—C3 | 115.0 (2) | C14—Ti2—C17—C32 | 32.9 (4) |
C23—Ti1—C2—C3 | −55.7 (3) | C15—Ti2—C17—C32 | −160.2 (5) |
C21—Ti1—C2—C3 | −12.7 (4) | C10—Ti2—C17—C32 | 41.6 (6) |
C22—Ti1—C2—C3 | −22.5 (3) | C16—C17—C18—C19 | 2.0 (4) |
C20—Ti1—C2—C3 | −78.7 (4) | C32—C17—C18—C19 | 174.3 (4) |
C5—Ti1—C2—C3 | 79.9 (3) | Ti2—C17—C18—C19 | −63.8 (3) |
C24—Ti1—C2—C3 | −84.1 (3) | C16—C17—C18—C33 | −167.8 (4) |
C1—Ti1—C2—C3 | 117.8 (4) | C32—C17—C18—C33 | 4.5 (6) |
Cl1—Ti1—C2—C1 | 88.7 (2) | Ti2—C17—C18—C33 | 126.4 (4) |
C4—Ti1—C2—C1 | −79.2 (3) | C16—C17—C18—Ti2 | 65.8 (3) |
C3—Ti1—C2—C1 | −117.8 (4) | C32—C17—C18—Ti2 | −121.9 (4) |
Cl2—Ti1—C2—C1 | −2.8 (3) | Cl4—Ti2—C18—C17 | −94.1 (2) |
C23—Ti1—C2—C1 | −173.5 (2) | Cl3—Ti2—C18—C17 | 24.3 (2) |
C21—Ti1—C2—C1 | −130.5 (3) | C13—Ti2—C18—C17 | 118.0 (2) |
C22—Ti1—C2—C1 | −140.2 (2) | C12—Ti2—C18—C17 | 153.4 (3) |
C20—Ti1—C2—C1 | 163.5 (3) | C11—Ti2—C18—C17 | 169.0 (2) |
C5—Ti1—C2—C1 | −37.9 (2) | C19—Ti2—C18—C17 | −115.9 (3) |
C24—Ti1—C2—C1 | 158.1 (2) | C16—Ti2—C18—C17 | −37.6 (2) |
C1—C2—C3—C4 | 0.8 (4) | C14—Ti2—C18—C17 | 109.1 (2) |
Ti1—C2—C3—C4 | −65.3 (3) | C15—Ti2—C18—C17 | −78.0 (2) |
C1—C2—C3—Ti1 | 66.1 (3) | C10—Ti2—C18—C17 | 142.1 (2) |
Cl1—Ti1—C3—C2 | 28.4 (3) | Cl4—Ti2—C18—C19 | 21.8 (3) |
C4—Ti1—C3—C2 | −114.3 (4) | Cl3—Ti2—C18—C19 | 140.2 (2) |
Cl2—Ti1—C3—C2 | −91.8 (3) | C13—Ti2—C18—C19 | −126.1 (2) |
C23—Ti1—C3—C2 | 123.8 (3) | C12—Ti2—C18—C19 | −90.6 (2) |
C21—Ti1—C3—C2 | 172.0 (2) | C11—Ti2—C18—C19 | −75.1 (2) |
C22—Ti1—C3—C2 | 158.5 (3) | C17—Ti2—C18—C19 | 115.9 (3) |
C20—Ti1—C3—C2 | 141.1 (3) | C16—Ti2—C18—C19 | 78.3 (2) |
C5—Ti1—C3—C2 | −76.2 (3) | C14—Ti2—C18—C19 | −135.0 (2) |
C24—Ti1—C3—C2 | 111.8 (3) | C15—Ti2—C18—C19 | 37.9 (2) |
C1—Ti1—C3—C2 | −35.8 (2) | C10—Ti2—C18—C19 | −101.9 (2) |
Cl1—Ti1—C3—C4 | 142.7 (2) | Cl4—Ti2—C18—C33 | 144.8 (3) |
Cl2—Ti1—C3—C4 | 22.5 (3) | Cl3—Ti2—C18—C33 | −96.7 (4) |
C2—Ti1—C3—C4 | 114.3 (4) | C13—Ti2—C18—C33 | −3.1 (4) |
C23—Ti1—C3—C4 | −121.9 (3) | C12—Ti2—C18—C33 | 32.4 (4) |
C21—Ti1—C3—C4 | −73.7 (3) | C11—Ti2—C18—C33 | 47.9 (4) |
C22—Ti1—C3—C4 | −87.2 (2) | C19—Ti2—C18—C33 | 123.0 (5) |
C20—Ti1—C3—C4 | −104.6 (3) | C17—Ti2—C18—C33 | −121.1 (5) |
C5—Ti1—C3—C4 | 38.1 (2) | C16—Ti2—C18—C33 | −158.6 (4) |
C24—Ti1—C3—C4 | −133.9 (2) | C14—Ti2—C18—C33 | −12.0 (4) |
C1—Ti1—C3—C4 | 78.5 (2) | C15—Ti2—C18—C33 | 160.9 (4) |
C2—C3—C4—C5 | −2.0 (4) | C10—Ti2—C18—C33 | 21.1 (5) |
Ti1—C3—C4—C5 | −69.0 (3) | C16—C15—C19—C18 | 4.6 (4) |
C2—C3—C4—Ti1 | 67.0 (3) | C30—C15—C19—C18 | −169.2 (4) |
Cl1—Ti1—C4—C5 | 58.1 (3) | Ti2—C15—C19—C18 | 67.4 (3) |
C3—Ti1—C4—C5 | 113.5 (4) | C16—C15—C19—C34 | 173.5 (4) |
Cl2—Ti1—C4—C5 | −49.6 (2) | C30—C15—C19—C34 | −0.3 (6) |
C2—Ti1—C4—C5 | 75.8 (3) | Ti2—C15—C19—C34 | −123.6 (4) |
C23—Ti1—C4—C5 | 170.9 (3) | C16—C15—C19—Ti2 | −62.9 (3) |
C21—Ti1—C4—C5 | −132.0 (3) | C30—C15—C19—Ti2 | 123.3 (4) |
C22—Ti1—C4—C5 | −160.9 (3) | C17—C18—C19—C15 | −4.0 (4) |
C20—Ti1—C4—C5 | −138.1 (3) | C33—C18—C19—C15 | 165.5 (4) |
C24—Ti1—C4—C5 | 177.4 (2) | Ti2—C18—C19—C15 | −68.6 (3) |
C1—Ti1—C4—C5 | 35.4 (2) | C17—C18—C19—C34 | −172.4 (4) |
Cl1—Ti1—C4—C3 | −55.3 (3) | C33—C18—C19—C34 | −2.9 (7) |
Cl2—Ti1—C4—C3 | −163.1 (2) | Ti2—C18—C19—C34 | 123.1 (4) |
C2—Ti1—C4—C3 | −37.7 (2) | C17—C18—C19—Ti2 | 64.6 (3) |
C23—Ti1—C4—C3 | 57.5 (3) | C33—C18—C19—Ti2 | −125.9 (4) |
C21—Ti1—C4—C3 | 114.6 (2) | Cl4—Ti2—C19—C15 | −49.8 (2) |
C22—Ti1—C4—C3 | 85.6 (2) | Cl3—Ti2—C19—C15 | 56.0 (3) |
C20—Ti1—C4—C3 | 108.4 (3) | C13—Ti2—C19—C15 | 168.5 (2) |
C5—Ti1—C4—C3 | −113.5 (3) | C12—Ti2—C19—C15 | −163.7 (2) |
C24—Ti1—C4—C3 | 64.0 (3) | C11—Ti2—C19—C15 | −133.7 (2) |
C1—Ti1—C4—C3 | −78.1 (2) | C17—Ti2—C19—C15 | 76.8 (2) |
C3—C4—C5—C1 | 2.5 (4) | C18—Ti2—C19—C15 | 113.8 (3) |
Ti1—C4—C5—C1 | −64.2 (3) | C16—Ti2—C19—C15 | 35.6 (2) |
C3—C4—C5—Ti1 | 66.8 (3) | C14—Ti2—C19—C15 | 178.7 (2) |
C2—C1—C5—C4 | −2.0 (4) | C10—Ti2—C19—C15 | −135.0 (2) |
Si1—C1—C5—C4 | −174.6 (3) | Cl4—Ti2—C19—C18 | −163.6 (2) |
Ti1—C1—C5—C4 | 61.1 (3) | Cl3—Ti2—C19—C18 | −57.7 (3) |
C2—C1—C5—Ti1 | −63.1 (2) | C13—Ti2—C19—C18 | 54.8 (3) |
Si1—C1—C5—Ti1 | 124.3 (3) | C12—Ti2—C19—C18 | 82.5 (2) |
Cl1—Ti1—C5—C4 | −140.7 (2) | C11—Ti2—C19—C18 | 112.5 (2) |
C3—Ti1—C5—C4 | −39.0 (2) | C17—Ti2—C19—C18 | −37.0 (2) |
Cl2—Ti1—C5—C4 | 129.0 (3) | C16—Ti2—C19—C18 | −78.1 (2) |
C2—Ti1—C5—C4 | −80.5 (3) | C14—Ti2—C19—C18 | 65.0 (3) |
C23—Ti1—C5—C4 | −12.1 (3) | C15—Ti2—C19—C18 | −113.8 (3) |
C21—Ti1—C5—C4 | 57.2 (3) | C10—Ti2—C19—C18 | 111.2 (2) |
C22—Ti1—C5—C4 | 20.1 (3) | Cl4—Ti2—C19—C34 | 71.4 (3) |
C20—Ti1—C5—C4 | 79.8 (4) | Cl3—Ti2—C19—C34 | 177.3 (3) |
C24—Ti1—C5—C4 | −7.7 (7) | C13—Ti2—C19—C34 | −70.2 (4) |
C1—Ti1—C5—C4 | −118.5 (4) | C12—Ti2—C19—C34 | −42.5 (4) |
Cl1—Ti1—C5—C1 | −22.2 (2) | C11—Ti2—C19—C34 | −12.5 (4) |
C4—Ti1—C5—C1 | 118.5 (4) | C17—Ti2—C19—C34 | −162.0 (4) |
C3—Ti1—C5—C1 | 79.5 (2) | C18—Ti2—C19—C34 | −125.0 (4) |
Cl2—Ti1—C5—C1 | −112.5 (2) | C16—Ti2—C19—C34 | 156.9 (4) |
C2—Ti1—C5—C1 | 38.0 (2) | C14—Ti2—C19—C34 | −60.0 (4) |
C23—Ti1—C5—C1 | 106.4 (3) | C15—Ti2—C19—C34 | 121.2 (4) |
C21—Ti1—C5—C1 | 175.7 (2) | C10—Ti2—C19—C34 | −13.8 (4) |
C22—Ti1—C5—C1 | 138.6 (2) | Cl1—Ti1—C20—C24 | 64.0 (2) |
C20—Ti1—C5—C1 | −161.7 (3) | C4—Ti1—C20—C24 | −104.9 (3) |
C24—Ti1—C5—C1 | 110.8 (6) | C3—Ti1—C20—C24 | −57.2 (3) |
O—Si2—C10—C14 | 61.9 (4) | Cl2—Ti1—C20—C24 | 160.0 (3) |
C8—Si2—C10—C14 | −52.8 (4) | C2—Ti1—C20—C24 | −8.6 (5) |
C9—Si2—C10—C14 | −179.8 (3) | C23—Ti1—C20—C24 | −36.5 (2) |
O—Si2—C10—C11 | −111.9 (3) | C21—Ti1—C20—C24 | −115.8 (4) |
C8—Si2—C10—C11 | 133.4 (4) | C22—Ti1—C20—C24 | −77.8 (3) |
C9—Si2—C10—C11 | 6.4 (4) | C5—Ti1—C20—C24 | −152.4 (3) |
O—Si2—C10—Ti2 | 155.44 (19) | C1—Ti1—C20—C24 | 108.0 (9) |
C8—Si2—C10—Ti2 | 40.8 (3) | Cl1—Ti1—C20—C21 | 179.8 (3) |
C9—Si2—C10—Ti2 | −86.2 (3) | C4—Ti1—C20—C21 | 10.8 (4) |
Cl4—Ti2—C10—C14 | 155.2 (2) | C3—Ti1—C20—C21 | 58.5 (4) |
Cl3—Ti2—C10—C14 | 60.8 (2) | Cl2—Ti1—C20—C21 | −84.3 (3) |
C13—Ti2—C10—C14 | −35.4 (2) | C2—Ti1—C20—C21 | 107.2 (4) |
C12—Ti2—C10—C14 | −77.3 (3) | C23—Ti1—C20—C21 | 79.3 (3) |
C11—Ti2—C10—C14 | −113.8 (4) | C22—Ti1—C20—C21 | 38.0 (2) |
C19—Ti2—C10—C14 | −111.4 (2) | C5—Ti1—C20—C21 | −36.7 (4) |
C17—Ti2—C10—C14 | −13.7 (4) | C24—Ti1—C20—C21 | 115.8 (4) |
C18—Ti2—C10—C14 | −64.2 (3) | C1—Ti1—C20—C21 | −136.3 (8) |
C16—Ti2—C10—C14 | 114.5 (7) | Cl1—Ti1—C20—C28 | −58.7 (5) |
C15—Ti2—C10—C14 | −158.6 (2) | C4—Ti1—C20—C28 | 132.3 (4) |
Cl4—Ti2—C10—C11 | −91.0 (2) | C3—Ti1—C20—C28 | −180.0 (4) |
Cl3—Ti2—C10—C11 | 174.6 (2) | Cl2—Ti1—C20—C28 | 37.2 (5) |
C13—Ti2—C10—C11 | 78.3 (3) | C2—Ti1—C20—C28 | −131.3 (5) |
C12—Ti2—C10—C11 | 36.4 (3) | C23—Ti1—C20—C28 | −159.2 (6) |
C19—Ti2—C10—C11 | 2.3 (3) | C21—Ti1—C20—C28 | 121.5 (6) |
C17—Ti2—C10—C11 | 100.1 (4) | C22—Ti1—C20—C28 | 159.5 (6) |
C18—Ti2—C10—C11 | 49.6 (3) | C5—Ti1—C20—C28 | 84.8 (5) |
C16—Ti2—C10—C11 | −131.8 (7) | C24—Ti1—C20—C28 | −122.7 (6) |
C14—Ti2—C10—C11 | 113.8 (4) | C1—Ti1—C20—C28 | −14.8 (13) |
C15—Ti2—C10—C11 | −44.9 (4) | C24—C20—C21—C22 | 0.3 (5) |
Cl4—Ti2—C10—Si2 | 33.4 (2) | C28—C20—C21—C22 | 175.7 (4) |
Cl3—Ti2—C10—Si2 | −61.1 (2) | Ti1—C20—C21—C22 | −66.1 (3) |
C13—Ti2—C10—Si2 | −157.3 (3) | C24—C20—C21—C27 | −172.1 (4) |
C12—Ti2—C10—Si2 | 160.8 (3) | C28—C20—C21—C27 | 3.2 (7) |
C11—Ti2—C10—Si2 | 124.4 (4) | Ti1—C20—C21—C27 | 121.4 (5) |
C19—Ti2—C10—Si2 | 126.7 (2) | C24—C20—C21—Ti1 | 66.5 (3) |
C17—Ti2—C10—Si2 | −135.6 (3) | C28—C20—C21—Ti1 | −118.2 (4) |
C18—Ti2—C10—Si2 | 173.92 (18) | Cl1—Ti1—C21—C22 | 113.9 (2) |
C16—Ti2—C10—Si2 | −7.4 (8) | C4—Ti1—C21—C22 | −57.6 (3) |
C14—Ti2—C10—Si2 | −121.9 (3) | C3—Ti1—C21—C22 | −24.0 (3) |
C15—Ti2—C10—Si2 | 79.5 (3) | Cl2—Ti1—C21—C22 | −154.8 (3) |
C14—C10—C11—C12 | 0.2 (4) | C2—Ti1—C21—C22 | −16.4 (4) |
Si2—C10—C11—C12 | 175.1 (3) | C23—Ti1—C21—C22 | 37.5 (2) |
Ti2—C10—C11—C12 | −64.2 (3) | C20—Ti1—C21—C22 | 114.2 (4) |
C14—C10—C11—Ti2 | 64.4 (2) | C5—Ti1—C21—C22 | −86.0 (3) |
Si2—C10—C11—Ti2 | −120.8 (3) | C24—Ti1—C21—C22 | 78.0 (3) |
Cl4—Ti2—C11—C12 | −158.7 (3) | C1—Ti1—C21—C22 | −80.9 (4) |
Cl3—Ti2—C11—C12 | 110.6 (2) | Cl1—Ti1—C21—C20 | −0.3 (3) |
C13—Ti2—C11—C12 | 38.7 (2) | C4—Ti1—C21—C20 | −171.8 (3) |
C19—Ti2—C11—C12 | −60.9 (3) | C3—Ti1—C21—C20 | −138.2 (3) |
C17—Ti2—C11—C12 | −17.7 (4) | Cl2—Ti1—C21—C20 | 91.0 (3) |
C18—Ti2—C11—C12 | −27.6 (3) | C2—Ti1—C21—C20 | −130.6 (3) |
C16—Ti2—C11—C12 | −80.0 (4) | C23—Ti1—C21—C20 | −76.7 (3) |
C14—Ti2—C11—C12 | 79.6 (3) | C22—Ti1—C21—C20 | −114.2 (4) |
C15—Ti2—C11—C12 | −88.2 (3) | C5—Ti1—C21—C20 | 159.8 (3) |
C10—Ti2—C11—C12 | 117.4 (4) | C24—Ti1—C21—C20 | −36.2 (3) |
Cl4—Ti2—C11—C10 | 84.0 (2) | C1—Ti1—C21—C20 | 164.9 (3) |
Cl3—Ti2—C11—C10 | −6.7 (3) | Cl1—Ti1—C21—C27 | −124.8 (4) |
C13—Ti2—C11—C10 | −78.7 (3) | C4—Ti1—C21—C27 | 63.6 (5) |
C12—Ti2—C11—C10 | −117.4 (4) | C3—Ti1—C21—C27 | 97.3 (5) |
C19—Ti2—C11—C10 | −178.2 (2) | Cl2—Ti1—C21—C27 | −33.6 (4) |
C17—Ti2—C11—C10 | −135.0 (3) | C2—Ti1—C21—C27 | 104.8 (5) |
C18—Ti2—C11—C10 | −145.0 (2) | C23—Ti1—C21—C27 | 158.7 (5) |
C16—Ti2—C11—C10 | 162.6 (3) | C22—Ti1—C21—C27 | 121.2 (6) |
C14—Ti2—C11—C10 | −37.7 (2) | C20—Ti1—C21—C27 | −124.6 (6) |
C15—Ti2—C11—C10 | 154.4 (2) | C5—Ti1—C21—C27 | 35.2 (5) |
C10—C11—C12—C13 | 1.3 (4) | C24—Ti1—C21—C27 | −160.8 (5) |
Ti2—C11—C12—C13 | −65.4 (3) | C1—Ti1—C21—C27 | 40.3 (6) |
C10—C11—C12—Ti2 | 66.7 (3) | C20—C21—C22—C23 | 1.6 (4) |
Cl4—Ti2—C12—C11 | 23.4 (3) | C27—C21—C22—C23 | 174.3 (4) |
Cl3—Ti2—C12—C11 | −97.7 (3) | Ti1—C21—C22—C23 | −64.6 (3) |
C13—Ti2—C12—C11 | −114.0 (4) | C20—C21—C22—C26 | −166.9 (4) |
C19—Ti2—C12—C11 | 118.4 (3) | C27—C21—C22—C26 | 5.8 (7) |
C17—Ti2—C12—C11 | 168.6 (2) | Ti1—C21—C22—C26 | 126.9 (4) |
C18—Ti2—C12—C11 | 153.3 (3) | C20—C21—C22—Ti1 | 66.2 (3) |
C16—Ti2—C12—C11 | 140.7 (2) | C27—C21—C22—Ti1 | −121.1 (5) |
C14—Ti2—C12—C11 | −76.4 (3) | Cl1—Ti1—C22—C23 | 21.5 (3) |
C15—Ti2—C12—C11 | 108.7 (3) | C4—Ti1—C22—C23 | −123.5 (3) |
C10—Ti2—C12—C11 | −36.3 (2) | C3—Ti1—C22—C23 | −87.9 (2) |
Cl4—Ti2—C12—C13 | 137.5 (2) | Cl2—Ti1—C22—C23 | 142.1 (2) |
Cl3—Ti2—C12—C13 | 16.4 (3) | C2—Ti1—C22—C23 | −75.2 (3) |
C11—Ti2—C12—C13 | 114.0 (4) | C21—Ti1—C22—C23 | 115.1 (4) |
C19—Ti2—C12—C13 | −127.5 (3) | C20—Ti1—C22—C23 | 76.9 (3) |
C17—Ti2—C12—C13 | −77.4 (3) | C5—Ti1—C22—C23 | −134.9 (2) |
C18—Ti2—C12—C13 | −92.7 (3) | C24—Ti1—C22—C23 | 36.9 (2) |
C16—Ti2—C12—C13 | −105.3 (3) | C1—Ti1—C22—C23 | −104.5 (3) |
C14—Ti2—C12—C13 | 37.6 (2) | Cl1—Ti1—C22—C21 | −93.6 (3) |
C15—Ti2—C12—C13 | −137.2 (2) | C4—Ti1—C22—C21 | 121.4 (3) |
C10—Ti2—C12—C13 | 77.8 (3) | C3—Ti1—C22—C21 | 157.1 (3) |
C11—C12—C13—C14 | −2.4 (4) | Cl2—Ti1—C22—C21 | 27.1 (3) |
Ti2—C12—C13—C14 | −68.7 (3) | C2—Ti1—C22—C21 | 169.8 (3) |
C11—C12—C13—Ti2 | 66.3 (3) | C23—Ti1—C22—C21 | −115.1 (4) |
Cl4—Ti2—C13—C14 | 50.5 (3) | C20—Ti1—C22—C21 | −38.2 (3) |
Cl3—Ti2—C13—C14 | −53.6 (2) | C5—Ti1—C22—C21 | 110.1 (3) |
C12—Ti2—C13—C14 | 113.9 (4) | C24—Ti1—C22—C21 | −78.1 (3) |
C11—Ti2—C13—C14 | 76.0 (3) | C1—Ti1—C22—C21 | 140.4 (3) |
C19—Ti2—C13—C14 | 167.0 (2) | Cl1—Ti1—C22—C26 | 143.2 (4) |
C17—Ti2—C13—C14 | −135.4 (2) | C4—Ti1—C22—C26 | −1.8 (4) |
C18—Ti2—C13—C14 | −165.3 (3) | C3—Ti1—C22—C26 | 33.9 (4) |
C16—Ti2—C13—C14 | −137.7 (2) | Cl2—Ti1—C22—C26 | −96.1 (4) |
C15—Ti2—C13—C14 | 175.9 (2) | C2—Ti1—C22—C26 | 46.6 (4) |
C10—Ti2—C13—C14 | 35.0 (2) | C23—Ti1—C22—C26 | 121.7 (5) |
Cl4—Ti2—C13—C12 | −63.4 (3) | C21—Ti1—C22—C26 | −123.2 (5) |
Cl3—Ti2—C13—C12 | −167.5 (2) | C20—Ti1—C22—C26 | −161.4 (5) |
C11—Ti2—C13—C12 | −37.9 (2) | C5—Ti1—C22—C26 | −13.1 (4) |
C19—Ti2—C13—C12 | 53.0 (3) | C24—Ti1—C22—C26 | 158.7 (5) |
C17—Ti2—C13—C12 | 110.7 (3) | C1—Ti1—C22—C26 | 17.2 (5) |
C18—Ti2—C13—C12 | 80.8 (3) | C21—C22—C23—C24 | −2.9 (4) |
C16—Ti2—C13—C12 | 108.4 (3) | C26—C22—C23—C24 | 165.7 (4) |
C14—Ti2—C13—C12 | −113.9 (4) | Ti1—C22—C23—C24 | −67.5 (3) |
C15—Ti2—C13—C12 | 62.0 (3) | C21—C22—C23—C25 | −172.5 (4) |
C10—Ti2—C13—C12 | −78.9 (3) | C26—C22—C23—C25 | −3.8 (6) |
C12—C13—C14—C10 | 2.6 (4) | Ti1—C22—C23—C25 | 122.9 (4) |
Ti2—C13—C14—C10 | −63.7 (3) | C21—C22—C23—Ti1 | 64.6 (3) |
C12—C13—C14—Ti2 | 66.3 (3) | C26—C22—C23—Ti1 | −126.8 (4) |
C11—C10—C14—C13 | −1.8 (4) | Cl1—Ti1—C23—C24 | −48.5 (3) |
Si2—C10—C14—C13 | −176.8 (3) | C4—Ti1—C23—C24 | 171.1 (3) |
Ti2—C10—C14—C13 | 61.1 (3) | C3—Ti1—C23—C24 | −159.4 (3) |
C11—C10—C14—Ti2 | −62.8 (2) | Cl2—Ti1—C23—C24 | 60.0 (3) |
Si2—C10—C14—Ti2 | 122.2 (3) | C2—Ti1—C23—C24 | −131.2 (3) |
Cl4—Ti2—C14—C13 | −145.4 (2) | C21—Ti1—C23—C24 | 77.7 (3) |
Cl3—Ti2—C14—C13 | 124.7 (2) | C22—Ti1—C23—C24 | 115.4 (4) |
C12—Ti2—C14—C13 | −38.9 (3) | C20—Ti1—C23—C24 | 36.0 (3) |
C11—Ti2—C14—C13 | −80.6 (3) | C5—Ti1—C23—C24 | 178.0 (3) |
C19—Ti2—C14—C13 | −18.1 (3) | C1—Ti1—C23—C24 | −136.1 (3) |
C17—Ti2—C14—C13 | 53.9 (3) | Cl1—Ti1—C23—C22 | −163.9 (2) |
C18—Ti2—C14—C13 | 16.0 (3) | C4—Ti1—C23—C22 | 55.8 (3) |
C16—Ti2—C14—C13 | 80.6 (4) | C3—Ti1—C23—C22 | 85.2 (2) |
C15—Ti2—C14—C13 | −14.6 (8) | Cl2—Ti1—C23—C22 | −55.4 (3) |
C10—Ti2—C14—C13 | −119.1 (4) | C2—Ti1—C23—C22 | 113.5 (2) |
Cl4—Ti2—C14—C10 | −26.3 (2) | C21—Ti1—C23—C22 | −37.6 (2) |
Cl3—Ti2—C14—C10 | −116.2 (2) | C20—Ti1—C23—C22 | −79.4 (3) |
C13—Ti2—C14—C10 | 119.1 (4) | C5—Ti1—C23—C22 | 62.6 (3) |
C12—Ti2—C14—C10 | 80.2 (3) | C24—Ti1—C23—C22 | −115.4 (4) |
C11—Ti2—C14—C10 | 38.6 (2) | C1—Ti1—C23—C22 | 108.6 (3) |
C19—Ti2—C14—C10 | 101.0 (3) | Cl1—Ti1—C23—C25 | 72.4 (4) |
C17—Ti2—C14—C10 | 173.0 (2) | C4—Ti1—C23—C25 | −68.0 (4) |
C18—Ti2—C14—C10 | 135.1 (2) | C3—Ti1—C23—C25 | −38.5 (4) |
C16—Ti2—C14—C10 | −160.3 (3) | Cl2—Ti1—C23—C25 | −179.1 (3) |
C15—Ti2—C14—C10 | 104.5 (6) | C2—Ti1—C23—C25 | −10.3 (4) |
Cl4—Ti2—C15—C16 | −113.0 (2) | C21—Ti1—C23—C25 | −161.4 (4) |
Cl3—Ti2—C15—C16 | −23.3 (2) | C22—Ti1—C23—C25 | −123.7 (5) |
C13—Ti2—C15—C16 | 102.0 (3) | C20—Ti1—C23—C25 | 156.9 (4) |
C12—Ti2—C15—C16 | 135.3 (2) | C5—Ti1—C23—C25 | −61.1 (4) |
C11—Ti2—C15—C16 | 173.0 (2) | C24—Ti1—C23—C25 | 120.9 (5) |
C19—Ti2—C15—C16 | 117.9 (3) | C1—Ti1—C23—C25 | −15.2 (4) |
C17—Ti2—C15—C16 | 38.0 (2) | C21—C20—C24—C23 | −2.1 (5) |
C18—Ti2—C15—C16 | 79.4 (2) | C28—C20—C24—C23 | −177.5 (4) |
C14—Ti2—C15—C16 | 113.4 (6) | Ti1—C20—C24—C23 | 62.6 (3) |
C10—Ti2—C15—C16 | −160.0 (2) | C21—C20—C24—C29 | 170.8 (4) |
Cl4—Ti2—C15—C19 | 129.1 (2) | C28—C20—C24—C29 | −4.5 (7) |
Cl3—Ti2—C15—C19 | −141.2 (2) | Ti1—C20—C24—C29 | −124.4 (4) |
C13—Ti2—C15—C19 | −15.9 (3) | C21—C20—C24—Ti1 | −64.8 (3) |
C12—Ti2—C15—C19 | 17.4 (3) | C28—C20—C24—Ti1 | 119.9 (4) |
C11—Ti2—C15—C19 | 55.1 (3) | C22—C23—C24—C20 | 3.1 (5) |
C17—Ti2—C15—C19 | −79.9 (2) | C25—C23—C24—C20 | 173.1 (4) |
C18—Ti2—C15—C19 | −38.5 (2) | Ti1—C23—C24—C20 | −63.2 (3) |
C16—Ti2—C15—C19 | −117.9 (3) | C22—C23—C24—C29 | −169.9 (4) |
C14—Ti2—C15—C19 | −4.5 (8) | C25—C23—C24—C29 | 0.0 (7) |
C10—Ti2—C15—C19 | 82.1 (3) | Ti1—C23—C24—C29 | 123.7 (4) |
Cl4—Ti2—C15—C30 | 8.9 (4) | C22—C23—C24—Ti1 | 66.4 (3) |
Cl3—Ti2—C15—C30 | 98.7 (4) | C25—C23—C24—Ti1 | −123.7 (4) |
C13—Ti2—C15—C30 | −136.0 (4) | Cl1—Ti1—C24—C20 | −112.5 (3) |
C12—Ti2—C15—C30 | −102.7 (4) | C4—Ti1—C24—C20 | 105.3 (3) |
C11—Ti2—C15—C30 | −65.0 (4) | C3—Ti1—C24—C20 | 138.7 (3) |
C19—Ti2—C15—C30 | −120.1 (5) | Cl2—Ti1—C24—C20 | −22.0 (3) |
C17—Ti2—C15—C30 | 159.9 (4) | C2—Ti1—C24—C20 | 175.4 (2) |
C18—Ti2—C15—C30 | −158.6 (4) | C23—Ti1—C24—C20 | 117.0 (4) |
C16—Ti2—C15—C30 | 122.0 (5) | C21—Ti1—C24—C20 | 37.9 (2) |
C14—Ti2—C15—C30 | −124.6 (6) | C22—Ti1—C24—C20 | 79.4 (3) |
C10—Ti2—C15—C30 | −38.1 (5) | C5—Ti1—C24—C20 | 111.1 (6) |
C19—C15—C16—C17 | −3.3 (4) | C1—Ti1—C24—C20 | −161.1 (3) |
C30—C15—C16—C17 | 170.4 (4) | Cl1—Ti1—C24—C23 | 130.5 (3) |
Ti2—C15—C16—C17 | −65.1 (3) | C4—Ti1—C24—C23 | −11.7 (4) |
C19—C15—C16—C31 | −177.5 (4) | C3—Ti1—C24—C23 | 21.7 (3) |
C30—C15—C16—C31 | −3.7 (6) | Cl2—Ti1—C24—C23 | −139.0 (2) |
Ti2—C15—C16—C31 | 120.8 (4) | C2—Ti1—C24—C23 | 58.4 (3) |
C19—C15—C16—Ti2 | 61.7 (3) | C21—Ti1—C24—C23 | −79.2 (3) |
C30—C15—C16—Ti2 | −124.5 (4) | C22—Ti1—C24—C23 | −37.6 (2) |
Cl4—Ti2—C16—C15 | 63.6 (2) | C20—Ti1—C24—C23 | −117.0 (4) |
Cl3—Ti2—C16—C15 | 158.2 (2) | C5—Ti1—C24—C23 | −6.0 (8) |
C13—Ti2—C16—C15 | −110.8 (3) | C1—Ti1—C24—C23 | 81.9 (3) |
C12—Ti2—C16—C15 | −62.6 (3) | Cl1—Ti1—C24—C29 | 10.3 (4) |
C11—Ti2—C16—C15 | −13.1 (4) | C4—Ti1—C24—C29 | −131.9 (4) |
C19—Ti2—C16—C15 | −36.0 (2) | C3—Ti1—C24—C29 | −98.5 (5) |
C17—Ti2—C16—C15 | −114.9 (3) | Cl2—Ti1—C24—C29 | 100.9 (5) |
C18—Ti2—C16—C15 | −77.4 (2) | C2—Ti1—C24—C29 | −61.8 (5) |
C14—Ti2—C16—C15 | −158.6 (3) | C23—Ti1—C24—C29 | −120.2 (6) |
C10—Ti2—C16—C15 | 103.7 (7) | C21—Ti1—C24—C29 | 160.7 (5) |
Cl4—Ti2—C16—C17 | 178.5 (2) | C22—Ti1—C24—C29 | −157.8 (5) |
Cl3—Ti2—C16—C17 | −86.9 (2) | C20—Ti1—C24—C29 | 122.8 (6) |
C13—Ti2—C16—C17 | 4.1 (3) | C5—Ti1—C24—C29 | −126.1 (6) |
C12—Ti2—C16—C17 | 52.3 (3) | C1—Ti1—C24—C29 | −38.3 (6) |
Experimental details
(I) | (II) | |
Crystal data | ||
Chemical formula | [TiCl2(C5H5)(C7H10Si)]2O·CH2Cl2 | [TiCl2(C10H15)(C7H10Si)]2O |
Mr | 713.19 | 768.52 |
Crystal system, space group | Monoclinic, P21/c | Monoclinic, P21/n |
Temperature (K) | 223 | 223 |
a, b, c (Å) | 13.6494 (2), 12.8573 (2), 18.4995 (3) | 8.1319 (1), 22.2503 (3), 21.6970 (3) |
β (°) | 103.977 (1) | 97.97 (1) |
V (Å3) | 3150.44 (8) | 3887.84 (9) |
Z | 4 | 4 |
Radiation type | Mo Kα | Mo Kα |
µ (mm−1) | 1.11 | 0.77 |
Crystal size (mm) | 0.40 × 0.18 × 0.10 | 0.38 × 0.20 × 0.10 |
Data collection | ||
Diffractometer | Bruker CCD area detector diffractometer | Bruker CCD area detector diffractometer |
Absorption correction | Empirical (using intensity measurements) (SADABS; Blessing, 1995) | Empirical (using intensity measurements) (SADABS; Blessing, 1995) |
Tmin, Tmax | 0.67, 0.90 | 0.76, 0.93 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 27882, 4950, 2810 | 62999, 6849, 4852 |
Rint | 0.13 | 0.11 |
θmax (°) | 24 | 25 |
(sin θ/λ)max (Å−1) | 0.572 | 0.595 |
Refinement | ||
R[F2 > 2σ(F2)], wR(F2), S | 0.070, 0.179, 1.05 | 0.051, 0.122, 1.02 |
No. of reflections | 4950 | 6849 |
No. of parameters | 325 | 388 |
H-atom treatment | H-atom parameters constrained | H-atom parameters constrained |
w = 1/[σ2(Fo2) + (0.0647P)2 + 10.5834P] where P = (Fo2 + 2Fc2)/3 | w = 1/[σ2(Fo2) + (0.0451P)2 + 6.1721P] where P = (Fo2 + 2Fc2)/3 | |
Δρmax, Δρmin (e Å−3) | 0.77, −0.66 | 0.72, −0.51 |
Computer programs: SMART (Bruker, 1997a), SMART, SAINT (Bruker, 1997a), SHELXTL-Plus (Sheldrick, 1999), SHELXTL-Plus, SHELXTL (Bruker, 1997b), SHELXTL.
Ti1—Cl1 | 2.360 (2) | Si1—C1 | 1.876 (8) |
Ti1—Cl2 | 2.373 (2) | C1—C2 | 1.415 (10) |
Si1—O | 1.633 (5) | C2—C3 | 1.411 (10) |
Si1—C6 | 1.849 (8) | C3—C4 | 1.404 (11) |
Si1—C7 | 1.852 (9) | ||
Cl1—Ti1—Cl2 | 93.25 (9) | C2—C1—C5 | 105.5 (7) |
C6—Si1—C7 | 112.9 (4) | C3—C2—C1 | 109.3 (7) |
Si2—O—Si1 | 151.5 (4) | C4—C3—C2 | 107.0 (7) |
Ti1—Cl1 | 2.3291 (12) | Si1—C1 | 1.874 (4) |
Ti1—Cl2 | 2.3687 (12) | C1—C2 | 1.410 (5) |
Si1—O | 1.625 (3) | C2—C3 | 1.397 (6) |
Si1—C7 | 1.849 (4) | C3—C4 | 1.408 (6) |
Si1—C6 | 1.861 (4) | ||
Cl1—Ti1—Cl2 | 95.94 (5) | C2—C1—C5 | 105.1 (3) |
C7—Si1—C6 | 109.9 (2) | C3—C2—C1 | 110.3 (4) |
Si1—O—Si2 | 153.9 (2) | C2—C3—C4 | 107.2 (4) |
The title compounds, (I) and (II), were obtained as byproducts in the synthesis of [η5-(dimethylfenchoxysilyl)cyclopentadienyl](η5-cyclopentadienyl) titanium dichloride, (C10H17OSiMe2C5H4)C5H5TiCl2 (Grimmond & Corey, 1998) and [η5-(dimethylfenchoxysilyl)cyclopentadienyl](η5-pentamethyl cyclopentadienyl)titanium dichloride, (C10H17OSiMe2C5H4)C5Me5TiCl2, respectively, upon crystallization from ethyl acetate at 298 K. A Cambridge Database search indicated that these substituted metallocenes are the first crystallographically characterized examples of bimetallic siloxy-bridged titanocenes, although other structures of cyclopentadienyl transition metal complexes involving siloxane bridges are known (Schubert & Grubert, 1998; Ciruelos et al., 1998). The synthesis of compound (I) by alternative means has also been described by Noh et al. (1996). There is one CH2Cl2 molecule of solvation per molecule for metallocene (I) and no solvation for (II). Neither structure exhibits molecular disorder. For both compounds, there are no significant intermolecular close contacts resulting from crystal packing. Selected bond lengths and angles for (I) and (II) are listed in Tables 1 and 2, and perspective views of the two metallocenes are presented in Figs. 1 and 2.
In compounds (I) and (II), the cyclopentadienyl rings are planar within experimental error and adopt η5 bonding modes with respect to each Ti atom. The following geometric parameters described for (I) are compared in parentheses with the corresponding values for the parent titanocene dichloride (Clearfield et al., 1975). The average Cpcentroid—Ti distance is 2.06 (2.06 Å) and the Cpcentroid—Ti—Cpcentroid angle is 130.70 (130.98°). Additionally, compound (I) has a mean Ti—Cl bond length of 2.37 (2.36 Å) with a Cl—Ti—Cl angle of 93.25 (94.52°), indicating that all major aspects of the substituted metallocene architecture compare well with those of titanocene dichloride.
A similar comparison of (II) with the parent mixed titanocene dichloride Cp*CpTiCl2 (Cp* = C5Me5) indicated no significant deviations in the geometry of (II) from the base structure. The following geometric parameters described for (II) are compared in parentheses with the corresponding values for the parent mixed titanocene dichloride (Rodgers et al., 1985). The average Cpcentroid—Ti distance is 2.07 (2.07 Å), while the mean Cp*centroid-Ti distance is 2.10 (2.10 Å). The Cp*centroid-Ti—Cpcentroid angle is 132.60 (131.98°). Additionally, compound (II) has a mean Ti—Cl bond length of 2.35 (2.35 Å) with a slightly extended Cl—Ti—Cl angle of 95.94 (94.44°).
The conformations of the siloxy chains within (I) and (II) are different. The conformational geometry of the siloxy linkage in (I) is cisoid, in contrast to the transoid siloxy conformation observed in (II). In (I), a nearly eclipsed geometry for the Si1—O—Si2 linkage is observed in the crystal structure and this is highlighted by the C6—Si1···Si2—C8 torsion angle of 8.30°. Indeed, the C5H4 groups are also disposed in a periplanar or cis conformation with respect to one another, and the C1—Si1···Si2—C10 torsion angle of 6.20° emphasizes the nearly ideal eclipsed conformation of the silicon substituents. However, for (II), a staggered geometry of the substituents about the Si1—O—Si2 linkage is observed in the crystal structure in the solid state, which is highlighted by the C6—Si1···Si2—C9 torsion angle of 160.1°. The C5H4 groups are also disposed in an antiperiplanar or trans conformation with respect to one another, and the C1—Si1···Si2—C10 torsion angle is 168.3°, further emphasizing the staggered conformation of the Si substituents.
In compound (I), the two monosubstituted C5 planes are aligned in a nearly parallel fashion with a C5H4-centroid–C5H4-centroid distance of 3.86 Å, suggesting that a small degree of π-stacking may also be responsible for the observed geometry. However, in (II), a staggered conformation of the Si1—O—Si2 bridge substituents appeared to be a conformational energy minimum. Presumably, the steric repulsion of the Cp* ligands was too great to allow the cis conformation of the siloxane substituents which was observed for (I). It is also possible that net packing forces contributed to the opposing conformations observed between (I) and (II). For (I) and (II), all Si—C bond lengths approximate to the average Sisp3—Cspn (n = 2 or 3) distance within the margins of experimental error (Orpen et al., 1989).
All other cases of metallocenes that involve the same siloxane bridging unit are ansa-metallocenes, wherein both Cp units of the same ligand are bound to the same metal (Curtis et al., 1983; Angelokos et al., 1994; Ciruelos et al., 1995). For such ansa-metallocenes, the siloxane methyl substituents are constrained to be eclipsed in order to accommodate the metal center and so do not offer a legitimate comparison to the title compounds where free rotation about the Si1—O—Si2 axis is possible.