metal-organic compounds
In the title compound, (C4H12N2)[Ti(C7H4O3)3]·H2O·C3H7NO, the TiIV atom is chelated by three salicylate ligands in an octahedral geometry, the complex anion being the fac isomer. The cations, complex anions and solvent molecules are linked by hydrogen bonds into a layer structure.
Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805024761/ob6557sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536805024761/ob6557Isup2.hkl |
CCDC reference: 283971
Computing details top
Data collection: SMART (Bruker, 2002); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.
Crystal data top
(C4H12N2)[Ti(C7H4O3)3]·H2O·C3H7NO | Z = 2 |
Mr = 635.47 | F(000) = 664 |
Triclinic, P1 | Dx = 1.455 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 9.021 (1) Å | Cell parameters from 1049 reflections |
b = 11.072 (1) Å | θ = 2.3–20.1° |
c = 15.067 (2) Å | µ = 0.36 mm−1 |
α = 75.545 (2)° | T = 295 K |
β = 84.830 (2)° | Rod, yellow |
γ = 87.146 (3)° | 0.21 × 0.13 × 0.08 mm |
V = 1450.8 (3) Å3 |
Data collection top
Bruker APEX area-detector diffractometer | 5700 independent reflections |
Radiation source: fine-focus sealed tube | 3379 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.033 |
φ and ω scans | θmax = 26.3°, θmin = 1.4° |
Absorption correction: multi-scan SADABS (Sheldrick, 1996) | h = −9→11 |
Tmin = 0.383, Tmax = 0.972 | k = −13→11 |
8209 measured reflections | l = −18→18 |
Refinement top
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)] = 0.076 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.234 | H-atom parameters constrained |
S = 1.01 | w = 1/[σ2(Fo2) + (0.1201P)2] where P = (Fo2 + 2Fc2)/3 |
5700 reflections | (Δ/σ)max = 0.001 |
351 parameters | Δρmax = 0.40 e Å−3 |
0 restraints | Δρmin = −0.34 e Å−3 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
x | y | z | Uiso*/Ueq | ||
Ti1 | 0.68425 (10) | 0.70907 (8) | 0.76743 (5) | 0.0373 (3) | |
O1 | 0.8372 (4) | 0.5901 (3) | 0.7973 (2) | 0.043 (1) | |
O2 | 0.6641 (4) | 0.6313 (3) | 0.6624 (2) | 0.043 (1) | |
O3 | 0.7000 (4) | 0.5208 (3) | 0.5595 (2) | 0.052 (1) | |
O4 | 0.5342 (3) | 0.6200 (3) | 0.8461 (2) | 0.042 (1) | |
O5 | 0.5203 (4) | 0.8248 (3) | 0.7118 (2) | 0.052 (1) | |
O6 | 0.3011 (4) | 0.9165 (3) | 0.6881 (2) | 0.059 (1) | |
O7 | 0.7228 (4) | 0.8041 (3) | 0.8496 (2) | 0.047 (1) | |
O8 | 0.8203 (4) | 0.8280 (3) | 0.6757 (2) | 0.046 (1) | |
O9 | 0.9521 (4) | 0.9901 (3) | 0.6038 (2) | 0.051 (1) | |
O10 | 0.5505 (7) | 0.2756 (5) | 0.6833 (3) | 0.110 (2) | |
O1w | 1.1510 (5) | 1.1854 (4) | 0.5174 (3) | 0.080 (1) | |
N1 | 0.4565 (5) | 0.6807 (4) | 0.5027 (3) | 0.043 (1) | |
N2 | 0.2382 (5) | 0.8687 (4) | 0.5268 (3) | 0.048 (1) | |
N3 | 0.5014 (6) | 0.2220 (4) | 0.8347 (3) | 0.057 (1) | |
C1 | 0.9257 (3) | 0.5253 (3) | 0.7478 (2) | 0.037 (1) | |
C2 | 1.0602 (3) | 0.4776 (3) | 0.7823 (2) | 0.045 (1) | |
C3 | 1.1540 (3) | 0.4060 (3) | 0.7361 (2) | 0.054 (1) | |
C4 | 1.1133 (3) | 0.3820 (3) | 0.6555 (2) | 0.053 (1) | |
C5 | 0.9788 (4) | 0.4297 (3) | 0.6210 (2) | 0.045 (1) | |
C6 | 0.8851 (3) | 0.5013 (3) | 0.6672 (2) | 0.036 (1) | |
C7 | 0.7427 (6) | 0.5520 (4) | 0.6271 (3) | 0.040 (1) | |
C8 | 0.7951 (4) | 0.9103 (3) | 0.8413 (2) | 0.041 (1) | |
C9 | 0.7931 (4) | 0.9542 (3) | 0.9202 (2) | 0.059 (3) | |
C10 | 0.8613 (5) | 1.0652 (4) | 0.9169 (2) | 0.078 (2) | |
C11 | 0.9316 (5) | 1.1324 (3) | 0.8348 (3) | 0.076 (2) | |
C12 | 0.9336 (4) | 1.0885 (3) | 0.7559 (2) | 0.059 (2) | |
C13 | 0.8653 (4) | 0.9775 (3) | 0.7592 (2) | 0.036 (1) | |
C14 | 0.8822 (5) | 0.9296 (4) | 0.6756 (3) | 0.036 (1) | |
C15 | 0.3928 (2) | 0.6491 (2) | 0.8723 (2) | 0.035 (1) | |
C16 | 0.3235 (3) | 0.5711 (2) | 0.9503 (2) | 0.043 (1) | |
C17 | 0.1786 (3) | 0.5984 (3) | 0.9807 (2) | 0.057 (2) | |
C18 | 0.1030 (3) | 0.7038 (3) | 0.9331 (2) | 0.058 (2) | |
C19 | 0.1722 (3) | 0.7818 (3) | 0.8551 (2) | 0.058 (2) | |
C20 | 0.3171 (3) | 0.7544 (2) | 0.8247 (2) | 0.038 (1) | |
C21 | 0.3818 (4) | 0.8408 (3) | 0.7344 (2) | 0.045 (1) | |
C22 | 0.4950 (6) | 0.8129 (5) | 0.4840 (4) | 0.049 (1) | |
C23 | 0.3621 (6) | 0.8941 (5) | 0.4549 (3) | 0.050 (1) | |
C24 | 0.1994 (6) | 0.7356 (5) | 0.5508 (4) | 0.057 (2) | |
C25 | 0.3340 (6) | 0.6516 (5) | 0.5759 (3) | 0.052 (1) | |
C26 | 0.5546 (8) | 0.2947 (6) | 0.7591 (4) | 0.078 (2) | |
C27 | 0.4252 (9) | 0.1120 (6) | 0.8325 (5) | 0.089 (2) | |
C28 | 0.5131 (10) | 0.2510 (7) | 0.9218 (4) | 0.100 (3) | |
H1w1 | 1.0761 | 1.1396 | 0.5379 | 0.096* | |
H1w2 | 1.1952 | 1.1623 | 0.4715 | 0.096* | |
H1a | 0.5369 | 0.6320 | 0.5200 | 0.051* | |
H1b | 0.4288 | 0.6644 | 0.4510 | 0.051* | |
H2a | 0.1581 | 0.9160 | 0.5069 | 0.057* | |
H2b | 0.2639 | 0.8894 | 0.5773 | 0.057* | |
H2 | 1.0874 | 0.4937 | 0.8362 | 0.054* | |
H3 | 1.2439 | 0.3741 | 0.7591 | 0.065* | |
H4 | 1.1761 | 0.3341 | 0.6246 | 0.064* | |
H5 | 0.9516 | 0.4136 | 0.5671 | 0.054* | |
H9 | 0.7461 | 0.9092 | 0.9752 | 0.071* | |
H10 | 0.8600 | 1.0945 | 0.9697 | 0.093* | |
H11 | 0.9772 | 1.2066 | 0.8326 | 0.091* | |
H12 | 0.9805 | 1.1334 | 0.7010 | 0.071* | |
H16 | 0.3742 | 0.5006 | 0.9821 | 0.052* | |
H17 | 0.1323 | 0.5462 | 1.0329 | 0.068* | |
H18 | 0.0060 | 0.7221 | 0.9535 | 0.070* | |
H19 | 0.1216 | 0.8523 | 0.8233 | 0.069* | |
H22a | 0.5755 | 0.8307 | 0.4358 | 0.058* | |
H22b | 0.5284 | 0.8300 | 0.5389 | 0.058* | |
H23a | 0.3881 | 0.9811 | 0.4425 | 0.060* | |
H23b | 0.3314 | 0.8792 | 0.3986 | 0.060* | |
H24a | 0.1578 | 0.7162 | 0.4990 | 0.068* | |
H24b | 0.1242 | 0.7201 | 0.6023 | 0.068* | |
H25a | 0.3670 | 0.6622 | 0.6329 | 0.062* | |
H25b | 0.3072 | 0.5653 | 0.5855 | 0.062* | |
H26 | 0.5994 | 0.3671 | 0.7627 | 0.094* | |
H27a | 0.3268 | 0.1350 | 0.8134 | 0.133* | |
H27b | 0.4186 | 0.0563 | 0.8927 | 0.133* | |
H27c | 0.4793 | 0.0712 | 0.7898 | 0.133* | |
H28a | 0.5753 | 0.3216 | 0.9130 | 0.150* | |
H28b | 0.5560 | 0.1805 | 0.9634 | 0.150* | |
H28c | 0.4158 | 0.2703 | 0.9470 | 0.150* |
Atomic displacement parameters (Å2) top
U11 | U22 | U33 | U12 | U13 | U23 | |
Ti1 | 0.0443 (6) | 0.0359 (5) | 0.0300 (5) | −0.0038 (4) | −0.0002 (4) | −0.0056 (4) |
O1 | 0.044 (2) | 0.053 (2) | 0.035 (2) | 0.005 (2) | −0.009 (2) | −0.013 (2) |
O2 | 0.053 (2) | 0.040 (2) | 0.039 (2) | −0.001 (2) | −0.011 (2) | −0.011 (2) |
O3 | 0.070 (3) | 0.050 (2) | 0.043 (2) | −0.005 (2) | −0.018 (2) | −0.018 (2) |
O4 | 0.038 (2) | 0.041 (2) | 0.041 (2) | −0.001 (2) | 0.001 (2) | 0.001 (2) |
O5 | 0.065 (3) | 0.038 (2) | 0.042 (2) | 0.010 (2) | 0.002 (2) | 0.003 (2) |
O6 | 0.082 (3) | 0.055 (2) | 0.040 (2) | 0.028 (2) | −0.028 (2) | −0.005 (2) |
O7 | 0.059 (2) | 0.050 (2) | 0.033 (2) | −0.015 (2) | 0.013 (2) | −0.015 (2) |
O8 | 0.062 (2) | 0.047 (2) | 0.029 (2) | −0.016 (2) | 0.007 (2) | −0.011 (2) |
O9 | 0.050 (2) | 0.064 (2) | 0.035 (2) | −0.020 (2) | 0.008 (2) | −0.007 (2) |
O10 | 0.164 (6) | 0.130 (4) | 0.034 (2) | −0.048 (4) | 0.002 (3) | −0.011 (3) |
O1w | 0.088 (3) | 0.096 (3) | 0.061 (3) | −0.042 (3) | 0.011 (2) | −0.030 (2) |
N1 | 0.049 (3) | 0.045 (2) | 0.037 (2) | 0.0035 (19) | −0.014 (2) | −0.011 (2) |
N2 | 0.043 (3) | 0.055 (3) | 0.047 (3) | 0.006 (2) | −0.013 (2) | −0.013 (2) |
N3 | 0.075 (3) | 0.056 (3) | 0.041 (3) | −0.012 (3) | −0.001 (2) | −0.013 (2) |
C1 | 0.041 (3) | 0.036 (3) | 0.034 (3) | −0.004 (2) | 0.003 (2) | −0.008 (2) |
C2 | 0.040 (3) | 0.051 (3) | 0.043 (3) | −0.004 (2) | −0.003 (2) | −0.009 (2) |
C3 | 0.041 (3) | 0.055 (4) | 0.060 (4) | 0.004 (3) | −0.001 (3) | −0.005 (3) |
C4 | 0.062 (4) | 0.043 (3) | 0.053 (3) | −0.003 (3) | 0.014 (3) | −0.015 (3) |
C5 | 0.057 (3) | 0.041 (3) | 0.036 (3) | −0.013 (2) | 0.004 (2) | −0.009 (2) |
C6 | 0.046 (3) | 0.032 (3) | 0.029 (2) | −0.012 (2) | −0.001 (2) | −0.003 (2) |
C7 | 0.058 (3) | 0.030 (3) | 0.032 (3) | −0.016 (2) | −0.001 (2) | −0.004 (2) |
C8 | 0.042 (3) | 0.045 (3) | 0.041 (3) | 0.001 (2) | 0.004 (2) | −0.021 (2) |
C9 | 0.073 (4) | 0.066 (4) | 0.041 (3) | −0.010 (3) | 0.010 (3) | −0.021 (3) |
C10 | 0.095 (5) | 0.080 (5) | 0.075 (4) | −0.018 (4) | 0.006 (4) | −0.052 (4) |
C11 | 0.103 (6) | 0.057 (4) | 0.073 (4) | −0.026 (4) | 0.009 (4) | −0.028 (3) |
C12 | 0.076 (4) | 0.053 (4) | 0.046 (3) | −0.017 (3) | 0.005 (3) | −0.010 (3) |
C13 | 0.040 (3) | 0.039 (3) | 0.027 (2) | 0.002 (2) | −0.004 (2) | −0.003 (2) |
C14 | 0.031 (3) | 0.040 (3) | 0.030 (2) | 0.003 (2) | −0.004 (2) | 0.002 (2) |
C15 | 0.036 (3) | 0.040 (3) | 0.033 (2) | −0.007 (2) | −0.008 (2) | −0.012 (2) |
C16 | 0.039 (3) | 0.049 (3) | 0.041 (3) | −0.006 (2) | −0.007 (2) | −0.008 (2) |
C17 | 0.045 (3) | 0.081 (4) | 0.048 (3) | −0.017 (3) | 0.004 (3) | −0.021 (3) |
C18 | 0.042 (3) | 0.081 (4) | 0.049 (3) | 0.009 (3) | −0.003 (3) | −0.014 (3) |
C19 | 0.055 (4) | 0.056 (4) | 0.063 (4) | 0.019 (3) | −0.017 (3) | −0.016 (3) |
C20 | 0.044 (3) | 0.035 (3) | 0.037 (3) | 0.007 (2) | −0.014 (2) | −0.010 (2) |
C21 | 0.070 (4) | 0.032 (3) | 0.037 (3) | 0.001 (3) | −0.010 (3) | −0.017 (2) |
C22 | 0.048 (3) | 0.052 (3) | 0.044 (3) | −0.007 (3) | −0.008 (2) | −0.007 (2) |
C23 | 0.057 (3) | 0.051 (3) | 0.040 (3) | −0.004 (3) | −0.006 (3) | −0.005 (2) |
C24 | 0.049 (3) | 0.068 (4) | 0.053 (3) | −0.012 (3) | −0.003 (3) | −0.015 (3) |
C25 | 0.073 (4) | 0.038 (3) | 0.044 (3) | −0.018 (3) | −0.003 (3) | −0.009 (2) |
C26 | 0.091 (5) | 0.088 (5) | 0.056 (4) | −0.039 (4) | 0.010 (4) | −0.018 (4) |
C27 | 0.119 (6) | 0.065 (4) | 0.082 (5) | −0.021 (4) | 0.007 (5) | −0.022 (4) |
C28 | 0.147 (8) | 0.104 (6) | 0.060 (4) | −0.023 (5) | 0.001 (5) | −0.040 (4) |
Geometric parameters (Å, º) top
Ti1—O1 | 1.864 (3) | C17—C18 | 1.3900 |
Ti1—O2 | 2.007 (3) | C18—C19 | 1.3900 |
Ti1—O4 | 1.863 (3) | C19—C20 | 1.3900 |
Ti1—O5 | 2.008 (4) | C20—C21 | 1.5390 |
Ti1—O7 | 1.878 (3) | C22—C23 | 1.494 (7) |
Ti1—O8 | 2.024 (3) | C24—C25 | 1.508 (8) |
O1—C1 | 1.345 (4) | O1w—H1w1 | 0.85 |
O2—C7 | 1.288 (5) | O1w—H1w2 | 0.86 |
O3—C7 | 1.251 (5) | N1—H1a | 0.90 |
O4—C15 | 1.348 (4) | N1—H1b | 0.90 |
O5—C21 | 1.280 (5) | N2—H2a | 0.90 |
O6—C21 | 1.207 (5) | N2—H2b | 0.90 |
O7—C8 | 1.346 (4) | C2—H2 | 0.93 |
O8—C14 | 1.279 (5) | C3—H3 | 0.93 |
O9—C14 | 1.254 (5) | C4—H4 | 0.93 |
O10—C26 | 1.215 (7) | C5—H5 | 0.93 |
N1—C22 | 1.473 (6) | C9—H9 | 0.93 |
N1—C25 | 1.477 (6) | C10—H10 | 0.93 |
N2—C23 | 1.471 (6) | C11—H11 | 0.93 |
N2—C24 | 1.479 (7) | C12—H12 | 0.93 |
N3—C26 | 1.288 (7) | C16—H16 | 0.93 |
N3—C27 | 1.437 (7) | C17—H17 | 0.93 |
N3—C28 | 1.441 (7) | C18—H18 | 0.93 |
C1—C2 | 1.3900 | C19—H19 | 0.93 |
C1—C6 | 1.3900 | C22—H22a | 0.97 |
C2—C3 | 1.3900 | C22—H22b | 0.97 |
C3—C4 | 1.3900 | C23—H23a | 0.97 |
C4—C5 | 1.3900 | C23—H23b | 0.97 |
C5—C6 | 1.3900 | C24—H24a | 0.97 |
C6—C7 | 1.493 (6) | C24—H24b | 0.97 |
C8—C9 | 1.3900 | C25—H25a | 0.97 |
C8—C13 | 1.3900 | C25—H25b | 0.97 |
C9—C10 | 1.3900 | C26—H26 | 0.93 |
C10—C11 | 1.3900 | C27—H27a | 0.96 |
C11—C12 | 1.3900 | C27—H27b | 0.96 |
C12—C13 | 1.3900 | C27—H27c | 0.96 |
C13—C14 | 1.477 (5) | C28—H28a | 0.96 |
C15—C16 | 1.3900 | C28—H28b | 0.96 |
C15—C20 | 1.3900 | C28—H28c | 0.96 |
C16—C17 | 1.3900 | ||
O1—Ti1—O2 | 84.7 (1) | H1w1—O1w—H1w2 | 108.7 |
O1—Ti1—O4 | 97.0 (1) | C22—N1—H1a | 109.5 |
O1—Ti1—O5 | 168.3 (1) | C25—N1—H1a | 109.5 |
O1—Ti1—O7 | 96.9 (2) | C22—N1—H1b | 109.5 |
O1—Ti1—O8 | 92.6 (2) | C25—N1—H1b | 109.5 |
O2—Ti1—O4 | 96.2 (1) | H1a—N1—H1b | 108.1 |
O2—Ti1—O5 | 83.7 (1) | C23—N2—H2a | 109.4 |
O2—Ti1—O7 | 169.5 (1) | C24—N2—H2a | 109.4 |
O2—Ti1—O8 | 84.5 (1) | C23—N2—H2b | 109.4 |
O4—Ti1—O5 | 86.0 (1) | C24—N2—H2b | 109.4 |
O4—Ti1—O7 | 93.9 (1) | H2a—N2—H2b | 108.0 |
O4—Ti1—O8 | 170.4 (2) | C1—C2—H2 | 120.0 |
O5—Ti1—O7 | 94.2 (2) | C3—C2—H2 | 120.0 |
O5—Ti1—O8 | 84.6 (1) | C4—C3—H3 | 120.0 |
O7—Ti1—O8 | 85.1 (1) | C2—C3—H3 | 120.0 |
C1—O1—Ti1 | 133.1 (2) | C5—C4—H4 | 120.0 |
C7—O2—Ti1 | 134.6 (3) | C3—C4—H4 | 120.0 |
C15—O4—Ti1 | 133.6 (2) | C4—C5—H5 | 120.0 |
C21—O5—Ti1 | 135.0 (2) | C6—C5—H5 | 120.0 |
C8—O7—Ti1 | 134.2 (2) | C10—C9—H9 | 120.0 |
C14—O8—Ti1 | 134.6 (3) | C8—C9—H9 | 120.0 |
C22—N1—C25 | 110.6 (4) | C11—C10—H10 | 120.0 |
C23—N2—C24 | 111.3 (4) | C9—C10—H10 | 120.0 |
C26—N3—C27 | 119.8 (5) | C10—C11—H11 | 120.0 |
C26—N3—C28 | 121.0 (5) | C12—C11—H11 | 120.0 |
C27—N3—C28 | 119.2 (5) | C13—C12—H12 | 120.0 |
O1—C1—C2 | 117.3 (2) | C11—C12—H12 | 120.0 |
O1—C1—C6 | 122.6 (2) | C17—C16—H16 | 120.0 |
C2—C1—C6 | 120.0 | C15—C16—H16 | 120.0 |
C1—C2—C3 | 120.0 | C16—C17—H17 | 120.0 |
C4—C3—C2 | 120.0 | C18—C17—H17 | 120.0 |
C5—C4—C3 | 120.0 | C17—C18—H18 | 120.0 |
C4—C5—C6 | 120.0 | C19—C18—H18 | 120.0 |
C5—C6—C1 | 120.0 | C20—C19—H19 | 120.0 |
C5—C6—C7 | 118.2 (3) | C18—C19—H19 | 120.0 |
C1—C6—C7 | 121.8 (3) | N1—C22—H22a | 109.7 |
O3—C7—O2 | 119.7 (5) | C23—C22—H22a | 109.7 |
O3—C7—C6 | 121.5 (4) | N1—C22—H22b | 109.7 |
O2—C7—C6 | 118.7 (4) | C23—C22—H22b | 109.7 |
O7—C8—C9 | 116.3 (2) | H22a—C22—H22b | 108.2 |
O7—C8—C13 | 123.7 (2) | N2—C23—H23a | 109.5 |
C9—C8—C13 | 120.0 | C22—C23—H23a | 109.5 |
C10—C9—C8 | 120.0 | N2—C23—H23b | 109.5 |
C11—C10—C9 | 120.0 | C22—C23—H23b | 109.5 |
C10—C11—C12 | 120.0 | H23a—C23—H23b | 108.1 |
C13—C12—C11 | 120.0 | N2—C24—H24a | 109.4 |
C12—C13—C8 | 120.0 | C25—C24—H24a | 109.4 |
C12—C13—C14 | 117.7 (3) | N2—C24—H24b | 109.4 |
C8—C13—C14 | 122.1 (3) | C25—C24—H24b | 109.4 |
O9—C14—O8 | 120.1 (4) | H24a—C24—H24b | 108.0 |
O9—C14—C13 | 120.4 (4) | N1—C25—H25a | 109.4 |
O8—C14—C13 | 119.5 (4) | C24—C25—H25a | 109.4 |
O4—C15—C16 | 118.0 (2) | N1—C25—H25b | 109.4 |
O4—C15—C20 | 122.0 (2) | C24—C25—H25b | 109.4 |
C16—C15—C20 | 120.0 | H25a—C25—H25b | 108.0 |
C17—C16—C15 | 120.0 | O10—C26—H26 | 117.7 |
C16—C17—C18 | 120.0 | N3—C26—H26 | 117.7 |
C17—C18—C19 | 120.0 | N3—C27—H27a | 109.5 |
C20—C19—C18 | 120.0 | N3—C27—H27b | 109.5 |
C19—C20—C15 | 120.0 | H27a—C27—H27b | 109.5 |
C19—C20—C21 | 116.6 | N3—C27—H27c | 109.5 |
C15—C20—C21 | 123.2 | H27a—C27—H27c | 109.5 |
O6—C21—O5 | 123.7 (3) | H27b—C27—H27c | 109.5 |
O6—C21—C20 | 119.6 (3) | N3—C28—H28a | 109.5 |
O5—C21—C20 | 116.7 (2) | N3—C28—H28b | 109.5 |
N1—C22—C23 | 109.8 (4) | H28a—C28—H28b | 109.5 |
N2—C23—C22 | 110.8 (4) | N3—C28—H28c | 109.5 |
N2—C24—C25 | 111.4 (4) | H28a—C28—H28c | 109.5 |
N1—C25—C24 | 111.0 (4) | H28b—C28—H28c | 109.5 |
O10—C26—N3 | 124.7 (6) | ||
O4—Ti1—O1—C1 | 119.4 (3) | C1—C6—C7—O3 | −173.3 (3) |
O7—Ti1—O1—C1 | −145.8 (3) | C5—C6—C7—O2 | −171.2 (3) |
O2—Ti1—O1—C1 | 23.8 (3) | C1—C6—C7—O2 | 8.0 (5) |
O5—Ti1—O1—C1 | 15.2 (9) | Ti1—O7—C8—C9 | 177.2 (3) |
O8—Ti1—O1—C1 | −60.5 (3) | Ti1—O7—C8—C13 | −0.8 (6) |
O4—Ti1—O2—C7 | −107.4 (4) | O7—C8—C9—C10 | −178.1 (4) |
O1—Ti1—O2—C7 | −10.9 (4) | C11—C12—C13—C14 | −174.7 (3) |
O7—Ti1—O2—C7 | 88.6 (9) | O7—C8—C13—C12 | 178.0 (4) |
O5—Ti1—O2—C7 | 167.4 (4) | O7—C8—C13—C14 | −7.6 (4) |
O8—Ti1—O2—C7 | 82.3 (4) | C9—C8—C13—C14 | 174.5 (4) |
O1—Ti1—O4—C15 | 171.2 (3) | Ti1—O8—C14—O9 | −173.5 (3) |
O7—Ti1—O4—C15 | 73.7 (4) | Ti1—O8—C14—C13 | 3.9 (7) |
O2—Ti1—O4—C15 | −103.4 (3) | C12—C13—C14—O9 | −2.2 (5) |
O5—Ti1—O4—C15 | −20.2 (4) | C8—C13—C14—O9 | −176.8 (3) |
O4—Ti1—O5—C21 | 12.0 (4) | C12—C13—C14—O8 | −179.6 (3) |
O1—Ti1—O5—C21 | 117.3 (7) | C8—C13—C14—O8 | 5.8 (6) |
O7—Ti1—O5—C21 | −81.6 (4) | Ti1—O4—C15—C16 | −163.3 (2) |
O2—Ti1—O5—C21 | 108.7 (4) | Ti1—O4—C15—C20 | 15.6 (5) |
O8—Ti1—O5—C21 | −166.2 (4) | O4—C15—C16—C17 | 179.0 (3) |
O4—Ti1—O7—C8 | −163.7 (4) | C18—C19—C20—C21 | 176.2 |
O1—Ti1—O7—C8 | 98.8 (4) | O4—C15—C20—C19 | −178.9 (3) |
O2—Ti1—O7—C8 | 0.5 (11) | O4—C15—C20—C21 | 5.2 (3) |
O5—Ti1—O7—C8 | −77.4 (4) | C16—C15—C20—C21 | −175.9 |
O8—Ti1—O7—C8 | 6.7 (4) | Ti1—O5—C21—O6 | −178.2 (3) |
O1—Ti1—O8—C14 | −105.2 (5) | Ti1—O5—C21—C20 | 0.0 (5) |
O7—Ti1—O8—C14 | −8.5 (5) | C19—C20—C21—O6 | −9.6 (3) |
O2—Ti1—O8—C14 | 170.4 (5) | C15—C20—C21—O6 | 166.5 (3) |
O5—Ti1—O8—C14 | 86.2 (5) | C19—C20—C21—O5 | 172.1 (3) |
Ti1—O1—C1—C2 | 157.9 (2) | C15—C20—C21—O5 | −11.9 (3) |
Ti1—O1—C1—C6 | −24.5 (4) | C25—N1—C22—C23 | −59.4 (5) |
O1—C1—C2—C3 | 177.7 (3) | C24—N2—C23—C22 | −56.6 (6) |
C4—C5—C6—C7 | 179.2 (3) | N1—C22—C23—N2 | 59.3 (5) |
O1—C1—C6—C5 | −177.5 (3) | C23—N2—C24—C25 | 53.6 (6) |
O1—C1—C6—C7 | 3.3 (4) | C22—N1—C25—C24 | 56.7 (5) |
C2—C1—C6—C7 | −179.2 (3) | N2—C24—C25—N1 | −53.6 (6) |
Ti1—O2—C7—O3 | −179.8 (3) | C27—N3—C26—O10 | −2.8 (12) |
Ti1—O2—C7—C6 | −1.0 (6) | C28—N3—C26—O10 | 179.1 (7) |
C5—C6—C7—O3 | 7.5 (5) |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1w—H1w1···O9 | 0.85 | 2.05 | 2.855 (5) | 161 |
O1w—H1w2···O8i | 0.86 | 2.21 | 2.939 (5) | 144 |
N1—H1a···O3 | 0.90 | 1.91 | 2.808 (5) | 177 |
N1—H1b···O10ii | 0.90 | 1.96 | 2.728 (6) | 142 |
N2—H2b···O6 | 0.90 | 1.83 | 2.726 (5) | 174 |
N2—H2a···O9iii | 0.90 | 2.04 | 2.840 (6) | 147 |
Symmetry codes: (i) −x+2, −y+2, −z+1; (ii) −x+1, −y+1, −z+1; (iii) −x+1, −y+2, −z+1. |