Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807002188/ng2208sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807002188/ng2208Isup2.hkl |
CCDC reference: 627344
Key indicators
- Single-crystal X-ray study
- T = 296 K
- Mean (C-C) = 0.003 Å
- R factor = 0.036
- wR factor = 0.098
- Data-to-parameter ratio = 12.3
checkCIF/PLATON results
No syntax errors found
Alert level C PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ? PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Ti1 PLAT380_ALERT_4_C Check Incorrectly? Oriented X(sp2)-Methyl Moiety C19
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 3 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 1 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
Data collection: SMART (Bruker, 2004); cell refinement: SMART; data reduction: SHELXTL (Sheldrick, 1997b) and SAINT (Bruker, 2004); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997a); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997a); molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.
[Ti(C6H7)2(C7H2N2O7)] | F(000) = 888 |
Mr = 432.21 | Dx = 1.575 Mg m−3 |
Monoclinic, P21/c | Melting point: 427 K |
Hall symbol: -P 2ybc | Mo Kα radiation, λ = 0.71073 Å |
a = 7.9457 (9) Å | Cell parameters from 4471 reflections |
b = 8.1111 (9) Å | θ = 2.5–27.8° |
c = 28.409 (3) Å | µ = 0.52 mm−1 |
β = 95.394 (1)° | T = 296 K |
V = 1822.8 (4) Å3 | Prism, red |
Z = 4 | 0.38 × 0.28 × 0.17 mm |
Bruker SMART CCD area-detector diffractometer | 3254 independent reflections |
Radiation source: fine-focus sealed tube | 2837 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.027 |
φ and ω scans | θmax = 25.1°, θmin = 2.6° |
Absorption correction: multi-scan (SADABS; Bruker, 1999) | h = −9→4 |
Tmin = 0.827, Tmax = 0.920 | k = −9→8 |
8884 measured reflections | l = −30→33 |
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)] = 0.036 | H-atom parameters constrained |
wR(F2) = 0.098 | w = 1/[σ2(Fo2) + (0.0512P)2 + 0.7525P] where P = (Fo2 + 2Fc2)/3 |
S = 1.03 | (Δ/σ)max = 0.001 |
3254 reflections | Δρmax = 0.30 e Å−3 |
265 parameters | Δρmin = −0.31 e Å−3 |
0 restraints | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0093 (10) |
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
x | y | z | Uiso*/Ueq | ||
Ti1 | 0.34649 (4) | 0.17727 (4) | 0.397551 (12) | 0.03589 (15) | |
N1 | 0.6283 (2) | 0.2063 (2) | 0.25882 (6) | 0.0464 (4) | |
C7 | 0.6239 (3) | −0.0668 (2) | 0.41892 (7) | 0.0400 (5) | |
O1 | 0.6341 (3) | 0.3458 (2) | 0.27505 (7) | 0.0727 (6) | |
O2 | 0.6001 (3) | 0.1765 (2) | 0.21668 (6) | 0.0711 (5) | |
O3 | 0.9854 (3) | −0.2933 (3) | 0.25484 (7) | 0.0783 (6) | |
O4 | 0.9698 (3) | −0.4203 (2) | 0.32068 (7) | 0.0744 (6) | |
O5 | 0.6959 (3) | −0.1663 (2) | 0.44586 (6) | 0.0689 (5) | |
O6 | 0.51792 (17) | 0.04184 (17) | 0.43284 (4) | 0.0421 (3) | |
O7 | 0.49918 (18) | 0.18278 (16) | 0.34715 (5) | 0.0416 (3) | |
C1 | 0.6664 (2) | 0.0672 (2) | 0.29111 (6) | 0.0355 (4) | |
C2 | 0.6036 (2) | 0.0680 (2) | 0.33647 (6) | 0.0341 (4) | |
C3 | 0.6617 (2) | −0.0601 (2) | 0.36799 (6) | 0.0353 (4) | |
C4 | 0.7681 (2) | −0.1813 (2) | 0.35315 (7) | 0.0385 (4) | |
H4 | 0.8075 | −0.2641 | 0.3740 | 0.046* | |
C5 | 0.8160 (2) | −0.1799 (2) | 0.30776 (7) | 0.0383 (4) | |
C6 | 0.7667 (2) | −0.0555 (2) | 0.27609 (7) | 0.0381 (4) | |
H6 | 0.8006 | −0.0553 | 0.2456 | 0.046* | |
N2 | 0.9310 (2) | −0.3071 (2) | 0.29335 (7) | 0.0508 (5) | |
C8 | 0.1864 (3) | 0.0247 (3) | 0.33668 (8) | 0.0573 (6) | |
H8 | 0.2111 | 0.0174 | 0.3036 | 0.069* | |
C9 | 0.2362 (3) | −0.0878 (3) | 0.37185 (8) | 0.0509 (6) | |
H9 | 0.3043 | −0.1866 | 0.3677 | 0.061* | |
C10 | 0.1593 (3) | −0.0467 (3) | 0.41325 (8) | 0.0506 (5) | |
C11 | 0.0632 (3) | 0.0951 (3) | 0.40245 (9) | 0.0551 (6) | |
H11 | −0.0152 | 0.1457 | 0.4229 | 0.066* | |
C12 | 0.0819 (3) | 0.1415 (3) | 0.35527 (9) | 0.0601 (6) | |
H12 | 0.0167 | 0.2269 | 0.3372 | 0.072* | |
C13 | 0.1752 (4) | −0.1373 (4) | 0.45930 (10) | 0.0766 (8) | |
H13A | 0.2023 | −0.0607 | 0.4847 | 0.115* | |
H13B | 0.2633 | −0.2182 | 0.4591 | 0.115* | |
H13C | 0.0702 | −0.1911 | 0.4637 | 0.115* | |
C14 | 0.2315 (4) | 0.4414 (3) | 0.40745 (10) | 0.0656 (7) | |
H14 | 0.1230 | 0.4816 | 0.3925 | 0.079* | |
C15 | 0.2586 (3) | 0.3693 (3) | 0.45222 (9) | 0.0572 (6) | |
H15 | 0.1721 | 0.3504 | 0.4740 | 0.069* | |
C16 | 0.4317 (3) | 0.3520 (3) | 0.46302 (8) | 0.0488 (5) | |
H16 | 0.4863 | 0.3144 | 0.4935 | 0.059* | |
C17 | 0.5172 (3) | 0.4099 (3) | 0.42527 (8) | 0.0505 (5) | |
C18 | 0.3902 (4) | 0.4654 (3) | 0.39038 (8) | 0.0630 (7) | |
H18 | 0.4103 | 0.5233 | 0.3612 | 0.076* | |
C19 | 0.7039 (3) | 0.4093 (4) | 0.42307 (12) | 0.0761 (8) | |
H19A | 0.7505 | 0.5115 | 0.4353 | 0.114* | |
H19B | 0.7285 | 0.3964 | 0.3908 | 0.114* | |
H19C | 0.7529 | 0.3195 | 0.4416 | 0.114* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ti1 | 0.0421 (2) | 0.0347 (2) | 0.0309 (2) | 0.00616 (14) | 0.00362 (15) | −0.00294 (13) |
N1 | 0.0491 (10) | 0.0508 (11) | 0.0404 (10) | 0.0066 (8) | 0.0107 (8) | 0.0110 (8) |
C7 | 0.0472 (11) | 0.0381 (10) | 0.0348 (10) | 0.0048 (9) | 0.0036 (8) | 0.0026 (8) |
O1 | 0.1152 (16) | 0.0438 (10) | 0.0625 (11) | 0.0127 (9) | 0.0269 (11) | 0.0111 (8) |
O2 | 0.0965 (14) | 0.0788 (13) | 0.0367 (9) | 0.0038 (10) | −0.0011 (9) | 0.0139 (8) |
O3 | 0.0912 (14) | 0.0965 (14) | 0.0504 (10) | 0.0446 (11) | 0.0241 (9) | −0.0035 (10) |
O4 | 0.0949 (14) | 0.0617 (11) | 0.0670 (11) | 0.0412 (10) | 0.0092 (10) | 0.0039 (9) |
O5 | 0.0995 (14) | 0.0678 (11) | 0.0412 (9) | 0.0411 (10) | 0.0155 (9) | 0.0177 (8) |
O6 | 0.0499 (8) | 0.0459 (8) | 0.0306 (7) | 0.0112 (7) | 0.0048 (6) | −0.0009 (6) |
O7 | 0.0521 (8) | 0.0380 (8) | 0.0362 (7) | 0.0125 (6) | 0.0112 (6) | 0.0046 (6) |
C1 | 0.0365 (10) | 0.0377 (10) | 0.0320 (10) | −0.0003 (8) | 0.0018 (8) | 0.0034 (8) |
C2 | 0.0358 (10) | 0.0334 (10) | 0.0330 (9) | −0.0002 (8) | 0.0021 (7) | −0.0008 (8) |
C3 | 0.0386 (10) | 0.0339 (10) | 0.0330 (10) | 0.0020 (8) | 0.0021 (8) | −0.0005 (8) |
C4 | 0.0434 (11) | 0.0354 (10) | 0.0360 (10) | 0.0031 (8) | −0.0005 (8) | 0.0000 (8) |
C5 | 0.0376 (10) | 0.0387 (11) | 0.0386 (11) | 0.0051 (8) | 0.0030 (8) | −0.0069 (8) |
C6 | 0.0365 (10) | 0.0450 (11) | 0.0332 (10) | −0.0010 (8) | 0.0048 (8) | −0.0032 (8) |
N2 | 0.0514 (11) | 0.0546 (12) | 0.0455 (11) | 0.0151 (9) | 0.0001 (8) | −0.0101 (9) |
C8 | 0.0584 (14) | 0.0670 (15) | 0.0446 (12) | −0.0094 (12) | −0.0043 (10) | −0.0117 (11) |
C9 | 0.0500 (12) | 0.0446 (12) | 0.0575 (14) | −0.0027 (10) | 0.0011 (10) | −0.0152 (10) |
C10 | 0.0492 (12) | 0.0488 (12) | 0.0536 (13) | −0.0059 (10) | 0.0037 (10) | −0.0022 (10) |
C11 | 0.0419 (12) | 0.0581 (14) | 0.0656 (15) | 0.0006 (10) | 0.0069 (10) | −0.0094 (12) |
C12 | 0.0530 (14) | 0.0616 (15) | 0.0616 (15) | 0.0022 (12) | −0.0157 (11) | −0.0010 (12) |
C13 | 0.092 (2) | 0.0722 (18) | 0.0664 (17) | −0.0137 (16) | 0.0092 (15) | 0.0163 (14) |
C14 | 0.0740 (18) | 0.0494 (14) | 0.0703 (17) | 0.0273 (13) | −0.0086 (14) | −0.0180 (12) |
C15 | 0.0664 (15) | 0.0553 (14) | 0.0512 (14) | 0.0073 (12) | 0.0131 (11) | −0.0181 (11) |
C16 | 0.0659 (14) | 0.0432 (12) | 0.0371 (11) | 0.0000 (10) | 0.0038 (10) | −0.0115 (9) |
C17 | 0.0655 (14) | 0.0329 (11) | 0.0542 (13) | −0.0027 (10) | 0.0114 (11) | −0.0083 (10) |
C18 | 0.115 (2) | 0.0283 (11) | 0.0464 (13) | 0.0112 (12) | 0.0086 (13) | 0.0010 (10) |
C19 | 0.0716 (18) | 0.0607 (17) | 0.099 (2) | −0.0170 (14) | 0.0234 (16) | −0.0163 (15) |
Ti1—O6 | 1.9520 (13) | C5—N2 | 1.462 (2) |
Ti1—O7 | 1.9622 (14) | C6—H6 | 0.9300 |
Ti1—C12 | 2.339 (2) | C8—C9 | 1.383 (3) |
Ti1—C15 | 2.352 (2) | C8—C12 | 1.396 (4) |
Ti1—C14 | 2.357 (2) | C8—H8 | 0.9800 |
Ti1—C11 | 2.364 (2) | C9—C10 | 1.415 (3) |
Ti1—C18 | 2.374 (2) | C9—H9 | 0.9800 |
Ti1—C16 | 2.385 (2) | C10—C11 | 1.399 (3) |
Ti1—C8 | 2.393 (2) | C10—C13 | 1.495 (4) |
Ti1—C9 | 2.409 (2) | C11—C12 | 1.414 (4) |
Ti1—C17 | 2.412 (2) | C11—H11 | 0.9800 |
Ti1—C10 | 2.416 (2) | C12—H12 | 0.9800 |
N1—O2 | 1.221 (2) | C13—H13A | 0.9600 |
N1—O1 | 1.221 (2) | C13—H13B | 0.9600 |
N1—C1 | 1.467 (3) | C13—H13C | 0.9600 |
C7—O5 | 1.217 (2) | C14—C15 | 1.398 (4) |
C7—O6 | 1.305 (2) | C14—C18 | 1.406 (4) |
C7—C3 | 1.506 (3) | C14—H14 | 0.9800 |
O3—N2 | 1.219 (3) | C15—C16 | 1.388 (3) |
O4—N2 | 1.223 (2) | C15—H15 | 0.9800 |
O7—C2 | 1.302 (2) | C16—C17 | 1.403 (3) |
C1—C6 | 1.369 (3) | C16—H16 | 0.9800 |
C1—C2 | 1.425 (3) | C17—C18 | 1.420 (3) |
C2—C3 | 1.420 (3) | C17—C19 | 1.490 (4) |
C3—C4 | 1.387 (3) | C18—H18 | 0.9800 |
C4—C5 | 1.378 (3) | C19—H19A | 0.9600 |
C4—H4 | 0.9300 | C19—H19B | 0.9600 |
C5—C6 | 1.383 (3) | C19—H19C | 0.9600 |
O6—Ti1—O7 | 86.45 (6) | C5—C4—H4 | 119.7 |
O6—Ti1—C12 | 138.07 (8) | C3—C4—H4 | 119.7 |
O7—Ti1—C12 | 102.45 (8) | C4—C5—C6 | 121.89 (17) |
O6—Ti1—C15 | 105.65 (7) | C4—C5—N2 | 119.39 (18) |
O7—Ti1—C15 | 135.17 (8) | C6—C5—N2 | 118.60 (18) |
C12—Ti1—C15 | 96.49 (9) | C1—C6—C5 | 117.73 (18) |
O6—Ti1—C14 | 135.24 (8) | C1—C6—H6 | 121.1 |
O7—Ti1—C14 | 109.85 (9) | C5—C6—H6 | 121.1 |
C12—Ti1—C14 | 80.47 (9) | O3—N2—O4 | 123.28 (19) |
C15—Ti1—C14 | 34.55 (9) | O3—N2—C5 | 118.07 (19) |
O6—Ti1—C11 | 115.68 (8) | O4—N2—C5 | 118.63 (19) |
O7—Ti1—C11 | 134.98 (8) | C9—C8—C12 | 108.3 (2) |
C12—Ti1—C11 | 34.97 (9) | C9—C8—Ti1 | 73.88 (12) |
C15—Ti1—C11 | 78.71 (9) | C12—C8—Ti1 | 70.75 (13) |
C14—Ti1—C11 | 82.38 (10) | C9—C8—H8 | 125.7 |
O6—Ti1—C18 | 119.83 (8) | C12—C8—H8 | 125.7 |
O7—Ti1—C18 | 79.03 (8) | Ti1—C8—H8 | 125.7 |
C12—Ti1—C18 | 102.10 (10) | C8—C9—C10 | 109.2 (2) |
C15—Ti1—C18 | 57.29 (9) | C8—C9—Ti1 | 72.64 (13) |
C14—Ti1—C18 | 34.58 (10) | C10—C9—Ti1 | 73.23 (13) |
C11—Ti1—C18 | 115.48 (10) | C8—C9—H9 | 125.3 |
O6—Ti1—C16 | 78.50 (7) | C10—C9—H9 | 125.3 |
O7—Ti1—C16 | 113.94 (7) | Ti1—C9—H9 | 125.3 |
C12—Ti1—C16 | 130.52 (9) | C11—C10—C9 | 106.3 (2) |
C15—Ti1—C16 | 34.06 (8) | C11—C10—C13 | 126.5 (2) |
C14—Ti1—C16 | 56.73 (8) | C9—C10—C13 | 127.2 (2) |
C11—Ti1—C16 | 108.88 (8) | C11—C10—Ti1 | 70.96 (13) |
C18—Ti1—C16 | 56.56 (8) | C9—C10—Ti1 | 72.65 (13) |
O6—Ti1—C8 | 112.21 (8) | C13—C10—Ti1 | 121.87 (17) |
O7—Ti1—C8 | 78.90 (8) | C10—C11—C12 | 108.8 (2) |
C12—Ti1—C8 | 34.28 (9) | C10—C11—Ti1 | 75.04 (13) |
C15—Ti1—C8 | 130.48 (9) | C12—C11—Ti1 | 71.55 (14) |
C14—Ti1—C8 | 111.76 (9) | C10—C11—H11 | 125.4 |
C11—Ti1—C8 | 56.80 (9) | C12—C11—H11 | 125.4 |
C18—Ti1—C8 | 121.27 (9) | Ti1—C11—H11 | 125.4 |
C16—Ti1—C8 | 164.45 (9) | C8—C12—C11 | 107.3 (2) |
O6—Ti1—C9 | 82.52 (7) | C8—C12—Ti1 | 74.97 (13) |
O7—Ti1—C9 | 91.79 (7) | C11—C12—Ti1 | 73.48 (13) |
C12—Ti1—C9 | 56.62 (8) | C8—C12—H12 | 125.9 |
C15—Ti1—C9 | 132.01 (9) | C11—C12—H12 | 125.9 |
C14—Ti1—C9 | 135.53 (9) | Ti1—C12—H12 | 125.9 |
C11—Ti1—C9 | 56.30 (8) | C10—C13—H13A | 109.5 |
C18—Ti1—C9 | 154.75 (8) | C10—C13—H13B | 109.5 |
C16—Ti1—C9 | 146.63 (8) | H13A—C13—H13B | 109.5 |
C8—Ti1—C9 | 33.48 (8) | C10—C13—H13C | 109.5 |
O6—Ti1—C17 | 85.91 (7) | H13A—C13—H13C | 109.5 |
O7—Ti1—C17 | 81.56 (7) | H13B—C13—H13C | 109.5 |
C12—Ti1—C17 | 135.67 (9) | C15—C14—C18 | 107.8 (2) |
C15—Ti1—C17 | 57.25 (9) | C15—C14—Ti1 | 72.53 (13) |
C14—Ti1—C17 | 57.47 (9) | C18—C14—Ti1 | 73.39 (13) |
C11—Ti1—C17 | 135.27 (8) | C15—C14—H14 | 125.9 |
C18—Ti1—C17 | 34.50 (8) | C18—C14—H14 | 125.9 |
C16—Ti1—C17 | 34.01 (8) | Ti1—C14—H14 | 125.9 |
C8—Ti1—C17 | 152.22 (9) | C16—C15—C14 | 107.9 (2) |
C9—Ti1—C17 | 167.00 (8) | C16—C15—Ti1 | 74.30 (12) |
O6—Ti1—C10 | 83.91 (7) | C14—C15—Ti1 | 72.92 (13) |
O7—Ti1—C10 | 125.83 (7) | C16—C15—H15 | 125.7 |
C12—Ti1—C10 | 57.47 (9) | C14—C15—H15 | 125.7 |
C15—Ti1—C10 | 98.62 (9) | Ti1—C15—H15 | 125.7 |
C14—Ti1—C10 | 114.17 (10) | C15—C16—C17 | 109.8 (2) |
C11—Ti1—C10 | 34.01 (8) | C15—C16—Ti1 | 71.64 (12) |
C18—Ti1—C10 | 148.60 (9) | C17—C16—Ti1 | 74.05 (12) |
C16—Ti1—C10 | 115.94 (8) | C15—C16—H16 | 125.0 |
C8—Ti1—C10 | 56.62 (8) | C17—C16—H16 | 125.0 |
C9—Ti1—C10 | 34.12 (8) | Ti1—C16—H16 | 125.0 |
C17—Ti1—C10 | 149.88 (8) | C16—C17—C18 | 106.0 (2) |
O2—N1—O1 | 123.42 (19) | C16—C17—C19 | 125.9 (2) |
O2—N1—C1 | 117.94 (18) | C18—C17—C19 | 128.1 (2) |
O1—N1—C1 | 118.55 (18) | C16—C17—Ti1 | 71.94 (12) |
O5—C7—O6 | 122.37 (19) | C18—C17—Ti1 | 71.27 (13) |
O5—C7—C3 | 120.21 (18) | C19—C17—Ti1 | 120.99 (16) |
O6—C7—C3 | 117.36 (16) | C14—C18—C17 | 108.5 (2) |
C7—O6—Ti1 | 131.53 (12) | C14—C18—Ti1 | 72.04 (14) |
C2—O7—Ti1 | 127.25 (12) | C17—C18—Ti1 | 74.24 (12) |
C6—C1—C2 | 123.29 (17) | C14—C18—H18 | 125.5 |
C6—C1—N1 | 117.15 (17) | C17—C18—H18 | 125.5 |
C2—C1—N1 | 119.52 (17) | Ti1—C18—H18 | 125.5 |
O7—C2—C3 | 123.56 (17) | C17—C19—H19A | 109.5 |
O7—C2—C1 | 119.94 (16) | C17—C19—H19B | 109.5 |
C3—C2—C1 | 116.50 (17) | H19A—C19—H19B | 109.5 |
C4—C3—C2 | 119.86 (18) | C17—C19—H19C | 109.5 |
C4—C3—C7 | 116.67 (17) | H19A—C19—H19C | 109.5 |
C2—C3—C7 | 123.32 (17) | H19B—C19—H19C | 109.5 |
C5—C4—C3 | 120.54 (18) | ||
O5—C7—O6—Ti1 | −163.09 (17) | C10—Ti1—C11—C12 | −116.2 (2) |
C3—C7—O6—Ti1 | 19.8 (3) | C9—C8—C12—C11 | −2.1 (3) |
O7—Ti1—O6—C7 | −33.19 (18) | Ti1—C8—C12—C11 | −66.91 (16) |
C12—Ti1—O6—C7 | 71.5 (2) | C9—C8—C12—Ti1 | 64.83 (16) |
C15—Ti1—O6—C7 | −169.29 (18) | C10—C11—C12—C8 | 1.6 (3) |
C14—Ti1—O6—C7 | −148.07 (19) | Ti1—C11—C12—C8 | 67.92 (16) |
C11—Ti1—O6—C7 | 105.92 (18) | C10—C11—C12—Ti1 | −66.33 (16) |
C18—Ti1—O6—C7 | −108.39 (19) | O6—Ti1—C12—C8 | −51.0 (2) |
C16—Ti1—O6—C7 | −148.50 (19) | O7—Ti1—C12—C8 | 47.65 (16) |
C8—Ti1—O6—C7 | 43.3 (2) | C15—Ti1—C12—C8 | −173.23 (16) |
C9—Ti1—O6—C7 | 59.09 (18) | C14—Ti1—C12—C8 | 156.04 (18) |
C17—Ti1—O6—C7 | −114.96 (19) | C11—Ti1—C12—C8 | −113.6 (2) |
C10—Ti1—O6—C7 | 93.43 (18) | C18—Ti1—C12—C8 | 128.90 (16) |
O6—Ti1—O7—C2 | 31.90 (16) | C16—Ti1—C12—C8 | −175.02 (14) |
C12—Ti1—O7—C2 | −106.65 (16) | C9—Ti1—C12—C8 | −36.21 (15) |
C15—Ti1—O7—C2 | 140.62 (16) | C17—Ti1—C12—C8 | 138.27 (15) |
C14—Ti1—O7—C2 | 169.12 (15) | C10—Ti1—C12—C8 | −77.12 (16) |
C11—Ti1—O7—C2 | −91.59 (18) | O6—Ti1—C12—C11 | 62.62 (19) |
C18—Ti1—O7—C2 | 153.21 (17) | O7—Ti1—C12—C11 | 161.29 (14) |
C16—Ti1—O7—C2 | 107.66 (16) | C15—Ti1—C12—C11 | −59.58 (16) |
C8—Ti1—O7—C2 | −81.55 (16) | C14—Ti1—C12—C11 | −90.31 (16) |
C9—Ti1—O7—C2 | −50.48 (16) | C18—Ti1—C12—C11 | −117.45 (15) |
C17—Ti1—O7—C2 | 118.29 (16) | C16—Ti1—C12—C11 | −61.38 (18) |
C10—Ti1—O7—C2 | −47.97 (18) | C8—Ti1—C12—C11 | 113.6 (2) |
O2—N1—C1—C6 | 39.7 (3) | C9—Ti1—C12—C11 | 77.44 (16) |
O1—N1—C1—C6 | −137.0 (2) | C17—Ti1—C12—C11 | −108.09 (16) |
O2—N1—C1—C2 | −142.4 (2) | C10—Ti1—C12—C11 | 36.52 (14) |
O1—N1—C1—C2 | 41.0 (3) | O6—Ti1—C14—C15 | −37.9 (2) |
Ti1—O7—C2—C3 | −19.7 (3) | O7—Ti1—C14—C15 | −143.62 (16) |
Ti1—O7—C2—C1 | 160.63 (13) | C12—Ti1—C14—C15 | 116.49 (18) |
C6—C1—C2—O7 | −175.19 (18) | C11—Ti1—C14—C15 | 81.16 (17) |
N1—C1—C2—O7 | 7.0 (3) | C18—Ti1—C14—C15 | −115.3 (2) |
C6—C1—C2—C3 | 5.1 (3) | C16—Ti1—C14—C15 | −37.42 (15) |
N1—C1—C2—C3 | −172.71 (17) | C8—Ti1—C14—C15 | 130.74 (16) |
O7—C2—C3—C4 | 177.58 (18) | C9—Ti1—C14—C15 | 101.83 (18) |
C1—C2—C3—C4 | −2.7 (3) | C17—Ti1—C14—C15 | −78.17 (16) |
O7—C2—C3—C7 | −6.8 (3) | C10—Ti1—C14—C15 | 68.79 (18) |
C1—C2—C3—C7 | 172.84 (17) | O6—Ti1—C14—C18 | 77.40 (19) |
O5—C7—C3—C4 | 5.9 (3) | O7—Ti1—C14—C18 | −28.30 (17) |
O6—C7—C3—C4 | −176.96 (17) | C12—Ti1—C14—C18 | −128.19 (17) |
O5—C7—C3—C2 | −169.8 (2) | C15—Ti1—C14—C18 | 115.3 (2) |
O6—C7—C3—C2 | 7.3 (3) | C11—Ti1—C14—C18 | −163.52 (16) |
C2—C3—C4—C5 | −1.0 (3) | C16—Ti1—C14—C18 | 77.90 (16) |
C7—C3—C4—C5 | −176.86 (18) | C8—Ti1—C14—C18 | −113.94 (15) |
C3—C4—C5—C6 | 2.8 (3) | C9—Ti1—C14—C18 | −142.85 (15) |
C3—C4—C5—N2 | 178.77 (18) | C17—Ti1—C14—C18 | 37.15 (14) |
C2—C1—C6—C5 | −3.5 (3) | C10—Ti1—C14—C18 | −175.89 (14) |
N1—C1—C6—C5 | 174.37 (17) | C18—C14—C15—C16 | 1.2 (3) |
C4—C5—C6—C1 | −0.6 (3) | Ti1—C14—C15—C16 | 66.61 (16) |
N2—C5—C6—C1 | −176.57 (17) | C18—C14—C15—Ti1 | −65.45 (17) |
C4—C5—N2—O3 | −172.4 (2) | O6—Ti1—C15—C16 | 38.39 (16) |
C6—C5—N2—O3 | 3.7 (3) | O7—Ti1—C15—C16 | −62.59 (18) |
C4—C5—N2—O4 | 6.5 (3) | C12—Ti1—C15—C16 | −177.57 (15) |
C6—C5—N2—O4 | −177.4 (2) | C14—Ti1—C15—C16 | −114.9 (2) |
O6—Ti1—C8—C9 | 29.28 (16) | C11—Ti1—C15—C16 | 152.16 (16) |
O7—Ti1—C8—C9 | 110.76 (15) | C18—Ti1—C15—C16 | −77.33 (16) |
C12—Ti1—C8—C9 | −116.6 (2) | C8—Ti1—C15—C16 | 177.42 (14) |
C15—Ti1—C8—C9 | −107.73 (17) | C9—Ti1—C15—C16 | 132.42 (14) |
C14—Ti1—C8—C9 | −142.13 (15) | C17—Ti1—C15—C16 | −36.05 (14) |
C11—Ti1—C8—C9 | −77.72 (16) | C10—Ti1—C15—C16 | 124.44 (15) |
C18—Ti1—C8—C9 | −179.49 (15) | O6—Ti1—C15—C14 | 153.29 (16) |
C16—Ti1—C8—C9 | −102.3 (3) | O7—Ti1—C15—C14 | 52.3 (2) |
C17—Ti1—C8—C9 | 156.86 (17) | C12—Ti1—C15—C14 | −62.67 (18) |
C10—Ti1—C8—C9 | −36.77 (14) | C11—Ti1—C15—C14 | −92.94 (17) |
O6—Ti1—C8—C12 | 145.86 (15) | C18—Ti1—C15—C14 | 37.57 (16) |
O7—Ti1—C8—C12 | −132.66 (17) | C16—Ti1—C15—C14 | 114.9 (2) |
C15—Ti1—C8—C12 | 8.9 (2) | C8—Ti1—C15—C14 | −67.7 (2) |
C14—Ti1—C8—C12 | −25.54 (19) | C9—Ti1—C15—C14 | −112.68 (18) |
C11—Ti1—C8—C12 | 38.87 (15) | C17—Ti1—C15—C14 | 78.85 (18) |
C18—Ti1—C8—C12 | −62.91 (19) | C10—Ti1—C15—C14 | −120.66 (17) |
C16—Ti1—C8—C12 | 14.2 (4) | C14—C15—C16—C17 | −1.0 (3) |
C9—Ti1—C8—C12 | 116.6 (2) | Ti1—C15—C16—C17 | 64.73 (15) |
C17—Ti1—C8—C12 | −86.6 (2) | C14—C15—C16—Ti1 | −65.69 (16) |
C10—Ti1—C8—C12 | 79.82 (17) | O6—Ti1—C16—C15 | −142.39 (16) |
C12—C8—C9—C10 | 1.8 (3) | O7—Ti1—C16—C15 | 136.78 (14) |
Ti1—C8—C9—C10 | 64.60 (16) | C12—Ti1—C16—C15 | 3.2 (2) |
C12—C8—C9—Ti1 | −62.79 (16) | C14—Ti1—C16—C15 | 37.97 (16) |
O6—Ti1—C9—C8 | −152.83 (15) | C11—Ti1—C16—C15 | −28.95 (17) |
O7—Ti1—C9—C8 | −66.65 (15) | C18—Ti1—C16—C15 | 79.66 (17) |
C12—Ti1—C9—C8 | 37.10 (15) | C8—Ti1—C16—C15 | −7.3 (4) |
C15—Ti1—C9—C8 | 102.82 (17) | C9—Ti1—C16—C15 | −85.8 (2) |
C14—Ti1—C9—C8 | 54.5 (2) | C17—Ti1—C16—C15 | 117.7 (2) |
C11—Ti1—C9—C8 | 79.36 (16) | C10—Ti1—C16—C15 | −65.05 (16) |
C18—Ti1—C9—C8 | 1.0 (3) | O6—Ti1—C16—C17 | 99.87 (14) |
C16—Ti1—C9—C8 | 151.57 (16) | O7—Ti1—C16—C17 | 19.04 (15) |
C17—Ti1—C9—C8 | −125.5 (3) | C12—Ti1—C16—C17 | −114.56 (16) |
C10—Ti1—C9—C8 | 117.0 (2) | C15—Ti1—C16—C17 | −117.7 (2) |
O6—Ti1—C9—C10 | 90.18 (13) | C14—Ti1—C16—C17 | −79.77 (16) |
O7—Ti1—C9—C10 | 176.37 (13) | C11—Ti1—C16—C17 | −146.69 (14) |
C12—Ti1—C9—C10 | −79.89 (15) | C18—Ti1—C16—C17 | −38.08 (15) |
C15—Ti1—C9—C10 | −14.16 (18) | C8—Ti1—C16—C17 | −125.1 (3) |
C14—Ti1—C9—C10 | −62.50 (18) | C9—Ti1—C16—C17 | 156.47 (15) |
C11—Ti1—C9—C10 | −37.62 (13) | C10—Ti1—C16—C17 | 177.20 (13) |
C18—Ti1—C9—C10 | −116.0 (2) | C15—C16—C17—C18 | 0.4 (2) |
C16—Ti1—C9—C10 | 34.6 (2) | Ti1—C16—C17—C18 | 63.57 (15) |
C8—Ti1—C9—C10 | −117.0 (2) | C15—C16—C17—C19 | −178.8 (2) |
C17—Ti1—C9—C10 | 117.5 (4) | Ti1—C16—C17—C19 | −115.6 (2) |
C8—C9—C10—C11 | −0.8 (3) | C15—C16—C17—Ti1 | −63.20 (16) |
Ti1—C9—C10—C11 | 63.42 (15) | O6—Ti1—C17—C16 | −75.44 (14) |
C8—C9—C10—C13 | 178.6 (2) | O7—Ti1—C17—C16 | −162.46 (14) |
Ti1—C9—C10—C13 | −117.2 (2) | C12—Ti1—C17—C16 | 98.34 (17) |
C8—C9—C10—Ti1 | −64.22 (16) | C15—Ti1—C17—C16 | 36.11 (14) |
O6—Ti1—C10—C11 | 159.60 (15) | C14—Ti1—C17—C16 | 77.42 (16) |
O7—Ti1—C10—C11 | −119.24 (14) | C11—Ti1—C17—C16 | 47.60 (19) |
C12—Ti1—C10—C11 | −37.59 (14) | C18—Ti1—C17—C16 | 114.7 (2) |
C15—Ti1—C10—C11 | 54.64 (15) | C8—Ti1—C17—C16 | 151.91 (18) |
C14—Ti1—C10—C11 | 22.31 (17) | C9—Ti1—C17—C16 | −102.6 (4) |
C18—Ti1—C10—C11 | 17.8 (2) | C10—Ti1—C17—C16 | −5.0 (2) |
C16—Ti1—C10—C11 | 85.55 (16) | O6—Ti1—C17—C18 | 169.90 (16) |
C8—Ti1—C10—C11 | −78.70 (16) | O7—Ti1—C17—C18 | 82.89 (15) |
C9—Ti1—C10—C11 | −114.8 (2) | C12—Ti1—C17—C18 | −16.3 (2) |
C17—Ti1—C10—C11 | 88.7 (2) | C15—Ti1—C17—C18 | −78.54 (16) |
O6—Ti1—C10—C9 | −85.64 (13) | C14—Ti1—C17—C18 | −37.24 (15) |
O7—Ti1—C10—C9 | −4.48 (16) | C11—Ti1—C17—C18 | −67.06 (19) |
C12—Ti1—C10—C9 | 77.17 (15) | C16—Ti1—C17—C18 | −114.7 (2) |
C15—Ti1—C10—C9 | 169.40 (14) | C8—Ti1—C17—C18 | 37.3 (3) |
C14—Ti1—C10—C9 | 137.07 (14) | C9—Ti1—C17—C18 | 142.7 (3) |
C11—Ti1—C10—C9 | 114.8 (2) | C10—Ti1—C17—C18 | −119.67 (19) |
C18—Ti1—C10—C9 | 132.60 (17) | O6—Ti1—C17—C19 | 46.1 (2) |
C16—Ti1—C10—C9 | −159.69 (13) | O7—Ti1—C17—C19 | −40.9 (2) |
C8—Ti1—C10—C9 | 36.06 (13) | C12—Ti1—C17—C19 | −140.1 (2) |
C17—Ti1—C10—C9 | −156.57 (16) | C15—Ti1—C17—C19 | 157.7 (2) |
O6—Ti1—C10—C13 | 37.8 (2) | C14—Ti1—C17—C19 | −161.0 (2) |
O7—Ti1—C10—C13 | 118.9 (2) | C11—Ti1—C17—C19 | 169.2 (2) |
C12—Ti1—C10—C13 | −159.4 (2) | C18—Ti1—C17—C19 | −123.8 (3) |
C15—Ti1—C10—C13 | −67.2 (2) | C16—Ti1—C17—C19 | 121.6 (3) |
C14—Ti1—C10—C13 | −99.5 (2) | C8—Ti1—C17—C19 | −86.5 (3) |
C11—Ti1—C10—C13 | −121.8 (3) | C9—Ti1—C17—C19 | 19.0 (5) |
C18—Ti1—C10—C13 | −104.0 (2) | C10—Ti1—C17—C19 | 116.5 (2) |
C16—Ti1—C10—C13 | −36.3 (2) | C15—C14—C18—C17 | −0.9 (3) |
C8—Ti1—C10—C13 | 159.5 (3) | Ti1—C14—C18—C17 | −65.82 (16) |
C9—Ti1—C10—C13 | 123.4 (3) | C15—C14—C18—Ti1 | 64.88 (17) |
C17—Ti1—C10—C13 | −33.1 (3) | C16—C17—C18—C14 | 0.4 (2) |
C9—C10—C11—C12 | −0.5 (3) | C19—C17—C18—C14 | 179.5 (2) |
C13—C10—C11—C12 | −179.9 (2) | Ti1—C17—C18—C14 | 64.38 (17) |
Ti1—C10—C11—C12 | 64.07 (17) | C16—C17—C18—Ti1 | −64.02 (15) |
C9—C10—C11—Ti1 | −64.56 (15) | C19—C17—C18—Ti1 | 115.1 (2) |
C13—C10—C11—Ti1 | 116.1 (2) | O6—Ti1—C18—C14 | −127.61 (15) |
O6—Ti1—C11—C10 | −22.62 (16) | O7—Ti1—C18—C14 | 152.98 (16) |
O7—Ti1—C11—C10 | 89.93 (16) | C12—Ti1—C18—C14 | 52.44 (17) |
C12—Ti1—C11—C10 | 116.2 (2) | C15—Ti1—C18—C14 | −37.54 (15) |
C15—Ti1—C11—C10 | −124.69 (15) | C11—Ti1—C18—C14 | 18.14 (18) |
C14—Ti1—C11—C10 | −159.55 (16) | C16—Ti1—C18—C14 | −78.45 (16) |
C18—Ti1—C11—C10 | −169.82 (13) | C8—Ti1—C18—C14 | 83.30 (17) |
C16—Ti1—C11—C10 | −108.64 (14) | C9—Ti1—C18—C14 | 82.6 (3) |
C8—Ti1—C11—C10 | 78.13 (15) | C17—Ti1—C18—C14 | −116.0 (2) |
C9—Ti1—C11—C10 | 37.75 (13) | C10—Ti1—C18—C14 | 7.2 (2) |
C17—Ti1—C11—C10 | −134.52 (14) | O6—Ti1—C18—C17 | −11.63 (18) |
O6—Ti1—C11—C12 | −138.82 (14) | O7—Ti1—C18—C17 | −91.04 (15) |
O7—Ti1—C11—C12 | −26.28 (19) | C12—Ti1—C18—C17 | 168.42 (15) |
C15—Ti1—C11—C12 | 119.10 (16) | C15—Ti1—C18—C17 | 78.44 (15) |
C14—Ti1—C11—C12 | 84.25 (16) | C14—Ti1—C18—C17 | 116.0 (2) |
C18—Ti1—C11—C12 | 73.98 (16) | C11—Ti1—C18—C17 | 134.12 (15) |
C16—Ti1—C11—C12 | 135.15 (15) | C16—Ti1—C18—C17 | 37.53 (14) |
C8—Ti1—C11—C12 | −38.07 (14) | C8—Ti1—C18—C17 | −160.73 (14) |
C9—Ti1—C11—C12 | −78.45 (16) | C9—Ti1—C18—C17 | −161.38 (18) |
C17—Ti1—C11—C12 | 109.27 (17) | C10—Ti1—C18—C17 | 123.18 (18) |