Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807000827/ci2256sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807000827/ci2256Isup2.hkl |
CCDC reference: 621958
Key indicators
- Single-crystal X-ray study
- T = 298 K
- R factor = 0.045
- wR factor = 0.126
- Data-to-parameter ratio = 12.1
checkCIF/PLATON results
No syntax errors found No errors found in this datablock
Data collection: SMART (Bruker, 2004); cell refinement: SAINT (Bruker, 2004); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997a); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997a); molecular graphics: SHELXTL (Sheldrick, 1997b); software used to prepare material for publication: SHELXTL.
[Ti(C6H7)2(C13H7O3)] | Z = 2 |
Mr = 525.25 | F(000) = 532 |
Triclinic, P1 | Dx = 1.551 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 7.834 (3) Å | Cell parameters from 2293 reflections |
b = 7.922 (3) Å | θ = 2.8–26.9° |
c = 19.867 (7) Å | µ = 2.19 mm−1 |
α = 89.999 (4)° | T = 298 K |
β = 79.003 (4)° | Plate, brown |
γ = 68.763 (4)° | 0.48 × 0.45 × 0.16 mm |
V = 1124.9 (7) Å3 |
Bruker SMART CCD area-detector diffractometer | 3892 independent reflections |
Radiation source: fine-focus sealed tube | 2797 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.033 |
φ and ω scans | θmax = 25.0°, θmin = 2.1° |
Absorption correction: multi-scan (SADABS; Bruker, 2004) | h = −7→9 |
Tmin = 0.420, Tmax = 0.721 | k = −7→9 |
5879 measured reflections | l = −23→23 |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.046 | H-atom parameters constrained |
wR(F2) = 0.126 | w = 1/[σ2(Fo2) + (0.063P)2 + 0.039P] where P = (Fo2 + 2Fc2)/3 |
S = 1.02 | (Δ/σ)max = 0.001 |
3892 reflections | Δρmax = 0.45 e Å−3 |
321 parameters | Δρmin = −0.43 e Å−3 |
43 restraints | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.013 (2) |
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Ti1 | 0.22353 (7) | 0.68722 (7) | 0.12537 (3) | 0.0308 (2) | |
Br1 | 0.8526 (2) | −0.8344 (3) | 0.4605 (3) | 0.0886 (10) | 0.677 (13) |
Br1' | 0.8535 (5) | −0.7732 (19) | 0.4929 (6) | 0.115 (3) | 0.323 (13) |
N1 | 0.5236 (6) | −0.0499 (6) | 0.3219 (2) | 0.0467 (15) | 0.781 (11) |
N2 | 0.4940 (6) | −0.0564 (6) | 0.3856 (2) | 0.0581 (16) | 0.781 (11) |
N1' | 0.440 (2) | 0.0191 (16) | 0.3600 (6) | 0.042 (5) | 0.219 (11) |
N2' | 0.530 (2) | −0.1409 (17) | 0.3354 (6) | 0.055 (6) | 0.219 (11) |
O1 | 0.4724 (3) | 0.4984 (3) | 0.11229 (11) | 0.0413 (6) | |
O2 | 0.6535 (3) | 0.2085 (3) | 0.10534 (14) | 0.0600 (7) | |
O3 | 0.1836 (3) | 0.6251 (3) | 0.21962 (11) | 0.0402 (6) | |
C1 | 0.5250 (4) | 0.3391 (4) | 0.13712 (18) | 0.0381 (8) | |
C2 | 0.4265 (4) | 0.3264 (4) | 0.20761 (17) | 0.0371 (8) | |
C3 | 0.2655 (5) | 0.4683 (4) | 0.24543 (17) | 0.0379 (8) | |
C4 | 0.1902 (5) | 0.4412 (5) | 0.31304 (19) | 0.0526 (9) | |
H4 | 0.0856 | 0.5325 | 0.3386 | 0.063* | |
C5 | 0.2718 (7) | 0.2782 (7) | 0.3419 (2) | 0.0635 (12) | |
H5 | 0.2220 | 0.2620 | 0.3867 | 0.076* | |
C6 | 0.4275 (6) | 0.1393 (5) | 0.3038 (2) | 0.0545 (10) | |
C7 | 0.4993 (5) | 0.1642 (5) | 0.2388 (2) | 0.0478 (9) | |
H7 | 0.6015 | 0.0695 | 0.2137 | 0.057* | |
C8 | 0.5835 (6) | −0.2494 (6) | 0.3960 (3) | 0.0729 (13) | |
C9 | 0.5823 (6) | −0.3990 (6) | 0.3608 (2) | 0.0656 (12) | |
H9 | 0.5290 | −0.3848 | 0.3221 | 0.079* | |
C10 | 0.6607 (6) | −0.5702 (6) | 0.3832 (2) | 0.0646 (11) | |
H10 | 0.6584 | −0.6720 | 0.3605 | 0.078* | |
C11 | 0.7408 (6) | −0.5862 (6) | 0.4388 (2) | 0.0642 (12) | |
C12 | 0.7395 (7) | −0.4416 (8) | 0.4738 (3) | 0.0871 (16) | |
H12 | 0.7945 | −0.4570 | 0.5120 | 0.105* | |
C13 | 0.6590 (7) | −0.2737 (7) | 0.4539 (3) | 0.0953 (18) | |
H13 | 0.6544 | −0.1734 | 0.4796 | 0.114* | |
C14 | 0.1531 (5) | 0.9762 (4) | 0.18613 (19) | 0.0457 (9) | |
C15 | 0.3473 (5) | 0.8835 (5) | 0.1729 (2) | 0.0484 (10) | |
H15 | 0.4197 | 0.8416 | 0.2058 | 0.058* | |
C16 | 0.4131 (5) | 0.8650 (5) | 0.1024 (2) | 0.0526 (10) | |
H16 | 0.5380 | 0.8122 | 0.0802 | 0.063* | |
C17 | 0.2620 (6) | 0.9384 (5) | 0.0702 (2) | 0.0554 (10) | |
H17 | 0.2671 | 0.9412 | 0.0231 | 0.066* | |
C18 | 0.1011 (5) | 1.0073 (4) | 0.1222 (2) | 0.0507 (10) | |
H18 | −0.0204 | 1.0644 | 0.1154 | 0.061* | |
C19 | 0.0265 (7) | 1.0284 (6) | 0.2557 (2) | 0.0798 (14) | |
H19A | 0.0744 | 0.9386 | 0.2867 | 0.120* | |
H19B | −0.0966 | 1.0357 | 0.2522 | 0.120* | |
H19C | 0.0204 | 1.1443 | 0.2726 | 0.120* | |
C20 | −0.0270 (4) | 0.5733 (5) | 0.12637 (18) | 0.0421 (8) | |
C21 | 0.1386 (5) | 0.4445 (5) | 0.0898 (2) | 0.0523 (10) | |
H21 | 0.1983 | 0.3275 | 0.1019 | 0.063* | |
C22 | 0.1999 (6) | 0.5241 (7) | 0.0308 (2) | 0.0648 (13) | |
H22 | 0.3068 | 0.4677 | −0.0029 | 0.078* | |
C23 | 0.0748 (6) | 0.6989 (7) | 0.0320 (2) | 0.0648 (12) | |
H23 | 0.0806 | 0.7805 | −0.0012 | 0.078* | |
C24 | −0.0627 (5) | 0.7322 (5) | 0.0918 (2) | 0.0514 (10) | |
H24 | −0.1616 | 0.8418 | 0.1062 | 0.062* | |
C25 | −0.1473 (6) | 0.5488 (7) | 0.1909 (2) | 0.0719 (13) | |
H25A | −0.2000 | 0.6599 | 0.2198 | 0.108* | |
H25B | −0.0728 | 0.4535 | 0.2148 | 0.108* | |
H25C | −0.2461 | 0.5171 | 0.1794 | 0.108* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ti1 | 0.0298 (3) | 0.0255 (3) | 0.0376 (4) | −0.0091 (2) | −0.0103 (2) | 0.0047 (2) |
Br1 | 0.0938 (7) | 0.0526 (8) | 0.100 (2) | −0.0065 (5) | −0.0161 (8) | 0.0396 (9) |
Br1' | 0.1047 (16) | 0.105 (4) | 0.098 (4) | 0.0016 (18) | −0.0176 (18) | 0.061 (4) |
N1 | 0.054 (3) | 0.056 (3) | 0.031 (2) | −0.018 (3) | −0.016 (2) | 0.021 (2) |
N2 | 0.074 (3) | 0.051 (3) | 0.048 (3) | −0.017 (2) | −0.021 (2) | 0.005 (2) |
N1' | 0.044 (7) | 0.054 (8) | 0.030 (8) | −0.016 (6) | −0.024 (6) | 0.031 (6) |
N2' | 0.067 (9) | 0.047 (8) | 0.053 (10) | −0.022 (7) | −0.014 (6) | 0.031 (7) |
O1 | 0.0329 (12) | 0.0343 (13) | 0.0490 (14) | −0.0048 (10) | −0.0052 (10) | 0.0098 (10) |
O2 | 0.0468 (14) | 0.0400 (15) | 0.0726 (19) | 0.0038 (12) | −0.0032 (13) | 0.0058 (13) |
O3 | 0.0410 (12) | 0.0357 (13) | 0.0367 (13) | −0.0079 (10) | −0.0038 (10) | 0.0039 (10) |
C1 | 0.0298 (17) | 0.0336 (19) | 0.050 (2) | −0.0084 (15) | −0.0129 (15) | 0.0052 (16) |
C2 | 0.0412 (18) | 0.0292 (17) | 0.046 (2) | −0.0126 (15) | −0.0209 (15) | 0.0076 (14) |
C3 | 0.0481 (19) | 0.0361 (19) | 0.0363 (19) | −0.0198 (16) | −0.0164 (15) | 0.0096 (15) |
C4 | 0.062 (2) | 0.059 (2) | 0.039 (2) | −0.025 (2) | −0.0103 (18) | 0.0048 (18) |
C5 | 0.094 (3) | 0.084 (3) | 0.042 (2) | −0.059 (3) | −0.031 (2) | 0.031 (2) |
C6 | 0.071 (3) | 0.047 (2) | 0.065 (3) | −0.032 (2) | −0.041 (2) | 0.024 (2) |
C7 | 0.054 (2) | 0.036 (2) | 0.061 (3) | −0.0180 (17) | −0.0297 (19) | 0.0154 (17) |
C8 | 0.064 (3) | 0.046 (3) | 0.108 (4) | −0.017 (2) | −0.023 (3) | 0.038 (3) |
C9 | 0.073 (3) | 0.079 (3) | 0.055 (3) | −0.032 (2) | −0.027 (2) | 0.029 (2) |
C10 | 0.074 (3) | 0.052 (3) | 0.067 (3) | −0.029 (2) | −0.003 (2) | 0.005 (2) |
C11 | 0.056 (2) | 0.056 (3) | 0.064 (3) | −0.006 (2) | −0.002 (2) | 0.027 (2) |
C12 | 0.085 (3) | 0.095 (4) | 0.067 (3) | −0.008 (3) | −0.033 (3) | 0.004 (3) |
C13 | 0.092 (4) | 0.064 (3) | 0.127 (5) | −0.012 (3) | −0.049 (4) | −0.013 (3) |
C14 | 0.051 (2) | 0.0274 (18) | 0.061 (3) | −0.0147 (16) | −0.0152 (18) | −0.0027 (16) |
C15 | 0.046 (2) | 0.035 (2) | 0.072 (3) | −0.0178 (17) | −0.028 (2) | −0.0006 (18) |
C16 | 0.046 (2) | 0.043 (2) | 0.075 (3) | −0.0253 (18) | −0.007 (2) | 0.0018 (19) |
C17 | 0.083 (3) | 0.041 (2) | 0.056 (2) | −0.034 (2) | −0.023 (2) | 0.0190 (18) |
C18 | 0.054 (2) | 0.0264 (18) | 0.075 (3) | −0.0111 (17) | −0.030 (2) | 0.0087 (18) |
C19 | 0.086 (3) | 0.066 (3) | 0.077 (3) | −0.025 (3) | 0.001 (3) | −0.027 (2) |
C20 | 0.0356 (18) | 0.050 (2) | 0.051 (2) | −0.0253 (17) | −0.0131 (16) | 0.0039 (17) |
C21 | 0.046 (2) | 0.036 (2) | 0.080 (3) | −0.0208 (17) | −0.015 (2) | −0.0080 (19) |
C22 | 0.063 (3) | 0.092 (4) | 0.050 (3) | −0.047 (3) | 0.000 (2) | −0.030 (2) |
C23 | 0.085 (3) | 0.091 (4) | 0.049 (3) | −0.056 (3) | −0.037 (2) | 0.022 (2) |
C24 | 0.048 (2) | 0.053 (2) | 0.068 (3) | −0.0244 (18) | −0.033 (2) | 0.0121 (19) |
C25 | 0.059 (3) | 0.101 (4) | 0.070 (3) | −0.050 (3) | −0.007 (2) | 0.017 (3) |
Ti1—O3 | 1.932 (2) | C9—C10 | 1.384 (6) |
Ti1—O1 | 1.949 (2) | C9—H9 | 0.93 |
Ti1—C22 | 2.353 (4) | C10—C11 | 1.357 (6) |
Ti1—C23 | 2.357 (4) | C10—H10 | 0.93 |
Ti1—C17 | 2.358 (4) | C11—C12 | 1.336 (7) |
Ti1—C24 | 2.365 (3) | C12—C13 | 1.345 (7) |
Ti1—C18 | 2.370 (3) | C12—H12 | 0.93 |
Ti1—C16 | 2.378 (4) | C13—H13 | 0.93 |
Ti1—C15 | 2.386 (3) | C14—C15 | 1.400 (5) |
Ti1—C21 | 2.397 (3) | C14—C18 | 1.402 (5) |
Ti1—C14 | 2.415 (3) | C14—C19 | 1.498 (6) |
Ti1—C20 | 2.436 (3) | C15—C16 | 1.385 (5) |
Br1—C11 | 1.927 (4) | C15—H15 | 0.93 |
Br1'—C11 | 1.882 (5) | C16—C17 | 1.393 (5) |
N1—N2 | 1.247 (6) | C16—H16 | 0.93 |
N1—C6 | 1.493 (5) | C17—C18 | 1.399 (5) |
N2—C8 | 1.466 (5) | C17—H17 | 0.93 |
N1'—N2' | 1.250 (10) | C18—H18 | 0.93 |
N1'—C6 | 1.461 (8) | C19—H19A | 0.96 |
N2'—C8 | 1.515 (8) | C19—H19B | 0.96 |
O1—C1 | 1.306 (4) | C19—H19C | 0.96 |
O2—C1 | 1.219 (4) | C20—C21 | 1.390 (5) |
O3—C3 | 1.329 (4) | C20—C24 | 1.398 (5) |
C1—C2 | 1.487 (5) | C20—C25 | 1.496 (5) |
C2—C7 | 1.402 (4) | C21—C22 | 1.416 (6) |
C2—C3 | 1.424 (5) | C21—H21 | 0.93 |
C3—C4 | 1.410 (5) | C22—C23 | 1.373 (6) |
C4—C5 | 1.395 (6) | C22—H22 | 0.93 |
C4—H4 | 0.93 | C23—C24 | 1.395 (6) |
C5—C6 | 1.395 (6) | C23—H23 | 0.93 |
C5—H5 | 0.93 | C24—H24 | 0.93 |
C6—C7 | 1.352 (5) | C25—H25A | 0.96 |
C7—H7 | 0.93 | C25—H25B | 0.96 |
C8—C13 | 1.374 (7) | C25—H25C | 0.96 |
C8—C9 | 1.381 (6) | ||
O3—Ti1—O1 | 87.36 (9) | C13—C8—C9 | 118.9 (4) |
O3—Ti1—C22 | 124.83 (14) | C13—C8—N2 | 111.8 (5) |
O1—Ti1—C22 | 83.00 (14) | C9—C8—N2 | 128.8 (4) |
O3—Ti1—C23 | 135.76 (13) | C13—C8—N2' | 150.7 (8) |
O1—Ti1—C23 | 113.92 (14) | C9—C8—N2' | 88.2 (7) |
C22—Ti1—C23 | 33.91 (15) | N2—C8—N2' | 44.5 (6) |
O3—Ti1—C17 | 135.18 (12) | C8—C9—C10 | 119.8 (4) |
O1—Ti1—C17 | 106.23 (13) | C8—C9—H9 | 120.1 |
C22—Ti1—C17 | 99.47 (16) | C10—C9—H9 | 120.1 |
C23—Ti1—C17 | 77.82 (15) | C11—C10—C9 | 118.5 (4) |
O3—Ti1—C24 | 104.26 (12) | C11—C10—H10 | 120.8 |
O1—Ti1—C24 | 137.55 (12) | C9—C10—H10 | 120.8 |
C22—Ti1—C24 | 56.63 (15) | C12—C11—C10 | 121.9 (4) |
C23—Ti1—C24 | 34.37 (14) | C12—C11—Br1' | 100.9 (7) |
C17—Ti1—C24 | 93.93 (14) | C10—C11—Br1' | 137.0 (7) |
O3—Ti1—C18 | 109.43 (12) | C12—C11—Br1 | 125.0 (4) |
O1—Ti1—C18 | 135.81 (12) | C10—C11—Br1 | 113.1 (4) |
C22—Ti1—C18 | 114.98 (16) | Br1'—C11—Br1 | 24.5 (4) |
C23—Ti1—C18 | 82.58 (15) | C11—C12—C13 | 120.3 (5) |
C17—Ti1—C18 | 34.43 (13) | C11—C12—H12 | 119.8 |
C24—Ti1—C18 | 79.07 (13) | C13—C12—H12 | 119.8 |
O3—Ti1—C16 | 114.12 (13) | C12—C13—C8 | 120.5 (5) |
O1—Ti1—C16 | 79.39 (12) | C12—C13—H13 | 119.8 |
C22—Ti1—C16 | 117.05 (15) | C8—C13—H13 | 119.8 |
C23—Ti1—C16 | 107.92 (15) | C15—C14—C18 | 106.9 (3) |
C17—Ti1—C16 | 34.20 (13) | C15—C14—C19 | 126.0 (4) |
C24—Ti1—C16 | 128.11 (14) | C18—C14—C19 | 127.1 (4) |
C18—Ti1—C16 | 56.42 (13) | C15—C14—Ti1 | 71.89 (19) |
O3—Ti1—C15 | 82.02 (12) | C18—C14—Ti1 | 71.20 (19) |
O1—Ti1—C15 | 87.61 (11) | C19—C14—Ti1 | 121.4 (3) |
C22—Ti1—C15 | 150.82 (15) | C16—C15—C14 | 108.3 (3) |
C23—Ti1—C15 | 134.13 (15) | C16—C15—Ti1 | 72.8 (2) |
C17—Ti1—C15 | 56.90 (14) | C14—C15—Ti1 | 74.20 (19) |
C24—Ti1—C15 | 133.95 (13) | C16—C15—H15 | 125.8 |
C18—Ti1—C15 | 56.52 (12) | C14—C15—H15 | 125.8 |
C16—Ti1—C15 | 33.79 (13) | Ti1—C15—H15 | 119.0 |
O3—Ti1—C21 | 90.33 (13) | C15—C16—C17 | 108.9 (3) |
O1—Ti1—C21 | 83.41 (11) | C15—C16—Ti1 | 73.4 (2) |
C22—Ti1—C21 | 34.68 (14) | C17—C16—Ti1 | 72.1 (2) |
C23—Ti1—C21 | 56.83 (15) | C15—C16—H16 | 125.5 |
C17—Ti1—C21 | 132.85 (15) | C17—C16—H16 | 125.5 |
C24—Ti1—C21 | 56.35 (13) | Ti1—C16—H16 | 120.7 |
C18—Ti1—C21 | 134.74 (13) | C16—C17—C18 | 107.0 (4) |
C16—Ti1—C21 | 149.10 (14) | C16—C17—Ti1 | 73.7 (2) |
C15—Ti1—C21 | 168.47 (13) | C18—C17—Ti1 | 73.2 (2) |
O3—Ti1—C14 | 79.19 (12) | C16—C17—H17 | 126.5 |
O1—Ti1—C14 | 120.96 (11) | C18—C17—H17 | 126.5 |
C22—Ti1—C14 | 148.84 (16) | Ti1—C17—H17 | 118.6 |
C23—Ti1—C14 | 115.41 (15) | C17—C18—C14 | 108.8 (3) |
C17—Ti1—C14 | 56.98 (14) | C17—C18—Ti1 | 72.3 (2) |
C24—Ti1—C14 | 101.40 (13) | C14—C18—Ti1 | 74.73 (19) |
C18—Ti1—C14 | 34.07 (12) | C17—C18—H18 | 125.6 |
C16—Ti1—C14 | 56.20 (13) | C14—C18—H18 | 125.6 |
C15—Ti1—C14 | 33.91 (12) | Ti1—C18—H18 | 119.1 |
C21—Ti1—C14 | 152.48 (13) | C14—C19—H19A | 109.5 |
O3—Ti1—C20 | 79.65 (11) | C14—C19—H19B | 109.5 |
O1—Ti1—C20 | 114.25 (11) | H19A—C19—H19B | 109.5 |
C22—Ti1—C20 | 56.39 (13) | C14—C19—H19C | 109.5 |
C23—Ti1—C20 | 56.47 (14) | H19A—C19—H19C | 109.5 |
C17—Ti1—C20 | 127.68 (13) | H19B—C19—H19C | 109.5 |
C24—Ti1—C20 | 33.81 (12) | C21—C20—C24 | 107.5 (3) |
C18—Ti1—C20 | 108.97 (12) | C21—C20—C25 | 126.9 (4) |
C16—Ti1—C20 | 161.88 (13) | C24—C20—C25 | 125.6 (4) |
C15—Ti1—C20 | 150.52 (13) | C21—C20—Ti1 | 71.73 (19) |
C21—Ti1—C20 | 33.43 (12) | C24—C20—Ti1 | 70.30 (18) |
C14—Ti1—C20 | 119.08 (12) | C25—C20—Ti1 | 123.5 (2) |
N2—N1—C6 | 109.9 (4) | C20—C21—C22 | 107.5 (4) |
N1—N2—C8 | 104.4 (4) | C20—C21—Ti1 | 74.85 (19) |
N2'—N1'—C6 | 108.7 (9) | C22—C21—Ti1 | 71.0 (2) |
N1'—N2'—C8 | 105.5 (9) | C20—C21—H21 | 126.2 |
C1—O1—Ti1 | 129.3 (2) | C22—C21—H21 | 126.2 |
C3—O3—Ti1 | 128.4 (2) | Ti1—C21—H21 | 119.8 |
O2—C1—O1 | 121.8 (3) | C23—C22—C21 | 108.4 (4) |
O2—C1—C2 | 121.3 (3) | C23—C22—Ti1 | 73.2 (2) |
O1—C1—C2 | 116.8 (3) | C21—C22—Ti1 | 74.4 (2) |
C7—C2—C3 | 118.3 (3) | C23—C22—H22 | 125.8 |
C7—C2—C1 | 117.3 (3) | C21—C22—H22 | 125.8 |
C3—C2—C1 | 124.4 (3) | Ti1—C22—H22 | 118.5 |
O3—C3—C4 | 118.7 (3) | C22—C23—C24 | 107.9 (4) |
O3—C3—C2 | 122.7 (3) | C22—C23—Ti1 | 72.9 (2) |
C4—C3—C2 | 118.6 (3) | C24—C23—Ti1 | 73.1 (2) |
C5—C4—C3 | 120.4 (4) | C22—C23—H23 | 126.1 |
C5—C4—H4 | 119.8 | C24—C23—H23 | 126.1 |
C3—C4—H4 | 119.8 | Ti1—C23—H23 | 119.8 |
C6—C5—C4 | 120.4 (4) | C23—C24—C20 | 108.6 (4) |
C6—C5—H5 | 119.8 | C23—C24—Ti1 | 72.5 (2) |
C4—C5—H5 | 119.8 | C20—C24—Ti1 | 75.88 (18) |
C7—C6—C5 | 119.5 (3) | C23—C24—H24 | 125.7 |
C7—C6—N1' | 147.4 (7) | C20—C24—H24 | 125.7 |
C5—C6—N1' | 93.1 (6) | Ti1—C24—H24 | 117.8 |
C7—C6—N1 | 111.3 (4) | C20—C25—H25A | 109.5 |
C5—C6—N1 | 129.0 (4) | C20—C25—H25B | 109.5 |
N1'—C6—N1 | 36.4 (6) | H25A—C25—H25B | 109.5 |
C6—C7—C2 | 122.9 (4) | C20—C25—H25C | 109.5 |
C6—C7—H7 | 118.6 | H25A—C25—H25C | 109.5 |
C2—C7—H7 | 118.6 | H25B—C25—H25C | 109.5 |
C6—N1—N2—C8 | 176.1 (4) | C22—Ti1—C17—C18 | 120.9 (2) |
C6—N1'—N2'—C8 | 164.7 (10) | C23—Ti1—C17—C18 | 94.7 (2) |
O3—Ti1—O1—C1 | 38.4 (3) | C24—Ti1—C17—C18 | 64.1 (2) |
C22—Ti1—O1—C1 | −87.1 (3) | C16—Ti1—C17—C18 | −114.0 (3) |
C23—Ti1—O1—C1 | −101.4 (3) | C15—Ti1—C17—C18 | −77.7 (2) |
C17—Ti1—O1—C1 | 175.0 (3) | C21—Ti1—C17—C18 | 110.2 (2) |
C24—Ti1—O1—C1 | −69.9 (3) | C14—Ti1—C17—C18 | −36.9 (2) |
C18—Ti1—O1—C1 | 153.9 (3) | C20—Ti1—C17—C18 | 66.4 (3) |
C16—Ti1—O1—C1 | 153.6 (3) | C16—C17—C18—C14 | −0.1 (4) |
C15—Ti1—O1—C1 | 120.5 (3) | Ti1—C17—C18—C14 | 66.4 (2) |
C21—Ti1—O1—C1 | −52.2 (3) | C16—C17—C18—Ti1 | −66.5 (2) |
C14—Ti1—O1—C1 | 114.1 (3) | C15—C14—C18—C17 | −1.4 (4) |
C20—Ti1—O1—C1 | −39.0 (3) | C19—C14—C18—C17 | 179.6 (4) |
O1—Ti1—O3—C3 | −25.1 (3) | Ti1—C14—C18—C17 | −64.9 (2) |
C22—Ti1—O3—C3 | 54.5 (3) | C15—C14—C18—Ti1 | 63.5 (2) |
C23—Ti1—O3—C3 | 97.2 (3) | C19—C14—C18—Ti1 | −115.6 (4) |
C17—Ti1—O3—C3 | −135.6 (3) | O3—Ti1—C18—C17 | 144.7 (2) |
C24—Ti1—O3—C3 | 113.5 (3) | O1—Ti1—C18—C17 | 37.7 (3) |
C18—Ti1—O3—C3 | −163.2 (2) | C22—Ti1—C18—C17 | −69.0 (2) |
C16—Ti1—O3—C3 | −102.2 (3) | C23—Ti1—C18—C17 | −79.3 (2) |
C15—Ti1—O3—C3 | −113.0 (3) | C24—Ti1—C18—C17 | −113.9 (2) |
C21—Ti1—O3—C3 | 58.3 (3) | C16—Ti1—C18—C17 | 38.1 (2) |
C14—Ti1—O3—C3 | −147.3 (3) | C15—Ti1—C18—C17 | 78.9 (2) |
C20—Ti1—O3—C3 | 90.2 (3) | C21—Ti1—C18—C17 | −104.3 (3) |
Ti1—O1—C1—O2 | 147.6 (3) | C14—Ti1—C18—C17 | 115.9 (3) |
Ti1—O1—C1—C2 | −35.2 (4) | C20—Ti1—C18—C17 | −129.9 (2) |
O2—C1—C2—C7 | 6.4 (5) | O3—Ti1—C18—C14 | 28.8 (2) |
O1—C1—C2—C7 | −170.8 (3) | O1—Ti1—C18—C14 | −78.3 (3) |
O2—C1—C2—C3 | −174.4 (3) | C22—Ti1—C18—C14 | 175.1 (2) |
O1—C1—C2—C3 | 8.4 (5) | C23—Ti1—C18—C14 | 164.8 (2) |
Ti1—O3—C3—C4 | −168.0 (2) | C17—Ti1—C18—C14 | −115.9 (3) |
Ti1—O3—C3—C2 | 12.1 (4) | C24—Ti1—C18—C14 | 130.2 (2) |
C7—C2—C3—O3 | −178.2 (3) | C16—Ti1—C18—C14 | −77.9 (2) |
C1—C2—C3—O3 | 2.6 (5) | C15—Ti1—C18—C14 | −37.0 (2) |
C7—C2—C3—C4 | 1.8 (5) | C21—Ti1—C18—C14 | 139.8 (2) |
C1—C2—C3—C4 | −177.4 (3) | C20—Ti1—C18—C14 | 114.2 (2) |
O3—C3—C4—C5 | 179.7 (3) | O3—Ti1—C20—C21 | −106.7 (2) |
C2—C3—C4—C5 | −0.3 (5) | O1—Ti1—C20—C21 | −24.4 (3) |
C3—C4—C5—C6 | −0.7 (5) | C22—Ti1—C20—C21 | 38.2 (3) |
C4—C5—C6—C7 | 0.2 (6) | C23—Ti1—C20—C21 | 79.2 (3) |
C4—C5—C6—N1' | 179.8 (7) | C17—Ti1—C20—C21 | 112.9 (3) |
C4—C5—C6—N1 | −173.3 (4) | C24—Ti1—C20—C21 | 117.0 (3) |
N2'—N1'—C6—C7 | −22 (2) | C18—Ti1—C20—C21 | 146.1 (2) |
N2'—N1'—C6—C5 | 158.5 (12) | C16—Ti1—C20—C21 | 112.2 (5) |
N2'—N1'—C6—N1 | −12.5 (10) | C15—Ti1—C20—C21 | −159.1 (3) |
N2—N1—C6—C7 | 161.6 (4) | C14—Ti1—C20—C21 | −178.1 (2) |
N2—N1—C6—C5 | −24.4 (6) | O3—Ti1—C20—C24 | 136.3 (2) |
N2—N1—C6—N1' | −12.8 (10) | O1—Ti1—C20—C24 | −141.4 (2) |
C5—C6—C7—C2 | 1.4 (5) | C22—Ti1—C20—C24 | −78.8 (3) |
N1'—C6—C7—C2 | −177.9 (11) | C23—Ti1—C20—C24 | −37.8 (2) |
N1—C6—C7—C2 | 176.0 (3) | C17—Ti1—C20—C24 | −4.1 (3) |
C3—C2—C7—C6 | −2.4 (5) | C18—Ti1—C20—C24 | 29.1 (3) |
C1—C2—C7—C6 | 176.9 (3) | C16—Ti1—C20—C24 | −4.8 (5) |
N1—N2—C8—C13 | 145.4 (5) | C15—Ti1—C20—C24 | 83.9 (3) |
N1—N2—C8—C9 | −42.2 (6) | C21—Ti1—C20—C24 | −117.0 (3) |
N1—N2—C8—N2' | −13.4 (11) | C14—Ti1—C20—C24 | 64.9 (3) |
N1'—N2'—C8—C13 | −50 (2) | O3—Ti1—C20—C25 | 16.0 (3) |
N1'—N2'—C8—C9 | 151.6 (13) | O1—Ti1—C20—C25 | 98.3 (3) |
N1'—N2'—C8—N2 | −6.3 (8) | C22—Ti1—C20—C25 | 161.0 (4) |
C13—C8—C9—C10 | −1.6 (7) | C23—Ti1—C20—C25 | −158.1 (4) |
N2—C8—C9—C10 | −173.6 (4) | C17—Ti1—C20—C25 | −124.3 (3) |
N2'—C8—C9—C10 | 166.7 (8) | C24—Ti1—C20—C25 | −120.3 (4) |
C8—C9—C10—C11 | −1.4 (6) | C18—Ti1—C20—C25 | −91.1 (3) |
C9—C10—C11—C12 | 2.6 (7) | C16—Ti1—C20—C25 | −125.0 (5) |
C9—C10—C11—Br1' | 176.3 (4) | C15—Ti1—C20—C25 | −36.4 (5) |
C9—C10—C11—Br1 | −177.4 (3) | C21—Ti1—C20—C25 | 122.7 (4) |
C10—C11—C12—C13 | −0.7 (8) | C14—Ti1—C20—C25 | −55.3 (4) |
Br1'—C11—C12—C13 | −176.3 (5) | C24—C20—C21—C22 | −2.3 (4) |
Br1—C11—C12—C13 | 179.4 (4) | C25—C20—C21—C22 | 177.5 (3) |
C11—C12—C13—C8 | −2.5 (8) | Ti1—C20—C21—C22 | −63.9 (2) |
C9—C8—C13—C12 | 3.6 (8) | C24—C20—C21—Ti1 | 61.6 (2) |
N2—C8—C13—C12 | 176.9 (5) | C25—C20—C21—Ti1 | −118.6 (4) |
N2'—C8—C13—C12 | −151.9 (14) | O3—Ti1—C21—C20 | 70.4 (2) |
O3—Ti1—C14—C15 | 91.8 (2) | O1—Ti1—C21—C20 | 157.7 (2) |
O1—Ti1—C14—C15 | 11.5 (3) | C22—Ti1—C21—C20 | −115.1 (4) |
C22—Ti1—C14—C15 | −124.3 (3) | C23—Ti1—C21—C20 | −78.0 (3) |
C23—Ti1—C14—C15 | −132.5 (2) | C17—Ti1—C21—C20 | −96.2 (3) |
C17—Ti1—C14—C15 | −78.4 (3) | C24—Ti1—C21—C20 | −36.6 (2) |
C24—Ti1—C14—C15 | −165.7 (2) | C18—Ti1—C21—C20 | −47.9 (3) |
C18—Ti1—C14—C15 | −115.8 (3) | C16—Ti1—C21—C20 | −145.9 (3) |
C16—Ti1—C14—C15 | −37.2 (2) | C15—Ti1—C21—C20 | 118.7 (7) |
C21—Ti1—C14—C15 | 161.1 (3) | C14—Ti1—C21—C20 | 3.7 (4) |
C20—Ti1—C14—C15 | 163.4 (2) | O3—Ti1—C21—C22 | −174.5 (3) |
O3—Ti1—C14—C18 | −152.5 (2) | O1—Ti1—C21—C22 | −87.2 (3) |
O1—Ti1—C14—C18 | 127.3 (2) | C23—Ti1—C21—C22 | 37.1 (2) |
C22—Ti1—C14—C18 | −8.6 (4) | C17—Ti1—C21—C22 | 18.8 (3) |
C23—Ti1—C14—C18 | −16.7 (3) | C24—Ti1—C21—C22 | 78.5 (3) |
C17—Ti1—C14—C18 | 37.3 (2) | C18—Ti1—C21—C22 | 67.2 (3) |
C24—Ti1—C14—C18 | −49.9 (2) | C16—Ti1—C21—C22 | −30.8 (4) |
C16—Ti1—C14—C18 | 78.6 (2) | C15—Ti1—C21—C22 | −126.3 (7) |
C15—Ti1—C14—C18 | 115.8 (3) | C14—Ti1—C21—C22 | 118.7 (3) |
C21—Ti1—C14—C18 | −83.2 (4) | C20—Ti1—C21—C22 | 115.1 (4) |
C20—Ti1—C14—C18 | −80.9 (2) | C20—C21—C22—C23 | 0.6 (4) |
O3—Ti1—C14—C19 | −29.9 (3) | Ti1—C21—C22—C23 | −65.8 (3) |
O1—Ti1—C14—C19 | −110.2 (3) | C20—C21—C22—Ti1 | 66.5 (2) |
C22—Ti1—C14—C19 | 114.0 (4) | O3—Ti1—C22—C23 | 122.0 (3) |
C23—Ti1—C14—C19 | 105.9 (3) | O1—Ti1—C22—C23 | −156.2 (3) |
C17—Ti1—C14—C19 | 159.9 (4) | C17—Ti1—C22—C23 | −50.8 (3) |
C24—Ti1—C14—C19 | 72.6 (3) | C24—Ti1—C22—C23 | 37.6 (2) |
C18—Ti1—C14—C19 | 122.6 (4) | C18—Ti1—C22—C23 | −18.5 (3) |
C16—Ti1—C14—C19 | −158.9 (4) | C16—Ti1—C22—C23 | −81.9 (3) |
C15—Ti1—C14—C19 | −121.7 (4) | C15—Ti1—C22—C23 | −84.0 (4) |
C21—Ti1—C14—C19 | 39.4 (5) | C21—Ti1—C22—C23 | 115.3 (4) |
C20—Ti1—C14—C19 | 41.7 (4) | C14—Ti1—C22—C23 | −13.2 (4) |
C18—C14—C15—C16 | 2.3 (4) | C20—Ti1—C22—C23 | 78.5 (3) |
C19—C14—C15—C16 | −178.6 (3) | O3—Ti1—C22—C21 | 6.7 (3) |
Ti1—C14—C15—C16 | 65.3 (2) | O1—Ti1—C22—C21 | 88.5 (2) |
C18—C14—C15—Ti1 | −63.0 (2) | C23—Ti1—C22—C21 | −115.3 (4) |
C19—C14—C15—Ti1 | 116.1 (4) | C17—Ti1—C22—C21 | −166.1 (2) |
O3—Ti1—C15—C16 | 162.1 (2) | C24—Ti1—C22—C21 | −77.6 (2) |
O1—Ti1—C15—C16 | 74.4 (2) | C18—Ti1—C22—C21 | −133.8 (2) |
C22—Ti1—C15—C16 | 3.4 (4) | C16—Ti1—C22—C21 | 162.8 (2) |
C23—Ti1—C15—C16 | −47.3 (3) | C15—Ti1—C22—C21 | 160.7 (2) |
C17—Ti1—C15—C16 | −36.8 (2) | C14—Ti1—C22—C21 | −128.5 (3) |
C24—Ti1—C15—C16 | −95.8 (3) | C20—Ti1—C22—C21 | −36.8 (2) |
C18—Ti1—C15—C16 | −78.2 (2) | C21—C22—C23—C24 | 1.3 (4) |
C21—Ti1—C15—C16 | 113.2 (7) | Ti1—C22—C23—C24 | −65.3 (3) |
C14—Ti1—C15—C16 | −115.5 (3) | C21—C22—C23—Ti1 | 66.6 (3) |
C20—Ti1—C15—C16 | −146.0 (3) | O3—Ti1—C23—C22 | −86.5 (3) |
O3—Ti1—C15—C14 | −82.5 (2) | O1—Ti1—C23—C22 | 26.0 (3) |
O1—Ti1—C15—C14 | −170.1 (2) | C17—Ti1—C23—C22 | 128.5 (3) |
C22—Ti1—C15—C14 | 118.8 (3) | C24—Ti1—C23—C22 | −115.4 (4) |
C23—Ti1—C15—C14 | 68.2 (3) | C18—Ti1—C23—C22 | 163.1 (3) |
C17—Ti1—C15—C14 | 78.7 (3) | C16—Ti1—C23—C22 | 112.1 (3) |
C24—Ti1—C15—C14 | 19.7 (3) | C15—Ti1—C23—C22 | 137.5 (3) |
C18—Ti1—C15—C14 | 37.2 (2) | C21—Ti1—C23—C22 | −37.9 (2) |
C16—Ti1—C15—C14 | 115.5 (3) | C14—Ti1—C23—C22 | 172.5 (2) |
C21—Ti1—C15—C14 | −131.3 (6) | C20—Ti1—C23—C22 | −78.2 (3) |
C20—Ti1—C15—C14 | −30.6 (4) | O3—Ti1—C23—C24 | 28.8 (3) |
C14—C15—C16—C17 | −2.4 (4) | O1—Ti1—C23—C24 | 141.4 (2) |
Ti1—C15—C16—C17 | 63.8 (3) | C22—Ti1—C23—C24 | 115.4 (4) |
C14—C15—C16—Ti1 | −66.2 (2) | C17—Ti1—C23—C24 | −116.1 (3) |
O3—Ti1—C16—C15 | −19.5 (2) | C18—Ti1—C23—C24 | −81.5 (3) |
O1—Ti1—C16—C15 | −101.7 (2) | C16—Ti1—C23—C24 | −132.5 (2) |
C22—Ti1—C16—C15 | −178.2 (2) | C15—Ti1—C23—C24 | −107.1 (3) |
C23—Ti1—C16—C15 | 146.4 (2) | C21—Ti1—C23—C24 | 77.5 (3) |
C17—Ti1—C16—C15 | 116.9 (3) | C14—Ti1—C23—C24 | −72.1 (3) |
C24—Ti1—C16—C15 | 114.4 (2) | C20—Ti1—C23—C24 | 37.2 (2) |
C18—Ti1—C16—C15 | 78.5 (2) | C22—C23—C24—C20 | −2.8 (4) |
C21—Ti1—C16—C15 | −159.0 (2) | Ti1—C23—C24—C20 | −67.9 (2) |
C14—Ti1—C16—C15 | 37.3 (2) | C22—C23—C24—Ti1 | 65.1 (3) |
C20—Ti1—C16—C15 | 117.8 (4) | C21—C20—C24—C23 | 3.2 (4) |
O3—Ti1—C16—C17 | −136.4 (2) | C25—C20—C24—C23 | −176.6 (3) |
O1—Ti1—C16—C17 | 141.4 (3) | Ti1—C20—C24—C23 | 65.7 (2) |
C22—Ti1—C16—C17 | 65.0 (3) | C21—C20—C24—Ti1 | −62.5 (2) |
C23—Ti1—C16—C17 | 29.5 (3) | C25—C20—C24—Ti1 | 117.7 (3) |
C24—Ti1—C16—C17 | −2.4 (3) | O3—Ti1—C24—C23 | −159.7 (2) |
C18—Ti1—C16—C17 | −38.3 (2) | O1—Ti1—C24—C23 | −57.7 (3) |
C15—Ti1—C16—C17 | −116.9 (3) | C22—Ti1—C24—C23 | −37.1 (3) |
C21—Ti1—C16—C17 | 84.1 (3) | C17—Ti1—C24—C23 | 61.6 (3) |
C14—Ti1—C16—C17 | −79.5 (3) | C18—Ti1—C24—C23 | 92.8 (3) |
C20—Ti1—C16—C17 | 1.0 (6) | C16—Ti1—C24—C23 | 63.0 (3) |
C15—C16—C17—C18 | 1.5 (4) | C15—Ti1—C24—C23 | 107.7 (3) |
Ti1—C16—C17—C18 | 66.2 (2) | C21—Ti1—C24—C23 | −79.0 (3) |
C15—C16—C17—Ti1 | −64.7 (3) | C14—Ti1—C24—C23 | 118.7 (3) |
O3—Ti1—C17—C16 | 63.3 (3) | C20—Ti1—C24—C23 | −115.1 (4) |
O1—Ti1—C17—C16 | −39.7 (3) | O3—Ti1—C24—C20 | −44.6 (2) |
C22—Ti1—C17—C16 | −125.1 (3) | O1—Ti1—C24—C20 | 57.4 (3) |
C23—Ti1—C17—C16 | −151.4 (3) | C22—Ti1—C24—C20 | 78.0 (3) |
C24—Ti1—C17—C16 | 178.1 (3) | C23—Ti1—C24—C20 | 115.1 (4) |
C18—Ti1—C17—C16 | 114.0 (3) | C17—Ti1—C24—C20 | 176.8 (2) |
C15—Ti1—C17—C16 | 36.3 (2) | C18—Ti1—C24—C20 | −152.0 (3) |
C21—Ti1—C17—C16 | −135.8 (2) | C16—Ti1—C24—C20 | 178.1 (2) |
C14—Ti1—C17—C16 | 77.1 (3) | C15—Ti1—C24—C20 | −137.2 (2) |
C20—Ti1—C17—C16 | −179.6 (2) | C21—Ti1—C24—C20 | 36.1 (2) |
O3—Ti1—C17—C18 | −50.7 (3) | C14—Ti1—C24—C20 | −126.2 (2) |
O1—Ti1—C17—C18 | −153.7 (2) |
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