The title compound, [Ti2(η5-C5H5)4(N3)2O], is a dinuclear oxo-bridged azido complex with two titanocene fragments connected through the oxygen bridge. The environment around each Ti atom can be considered as a distorted tetrahedron.
Supporting information
CCDC reference: 248724
Key indicators
- Single-crystal X-ray study
- T = 150 K
- Mean (C-C) = 0.003 Å
- R factor = 0.034
- wR factor = 0.087
- Data-to-parameter ratio = 17.2
checkCIF/PLATON results
No syntax errors found
Alert level B
PLAT230_ALERT_2_B Hirshfeld Test Diff for N1 - N2 .. 10.61 su
Alert level C
PLAT230_ALERT_2_C Hirshfeld Test Diff for N2 - N3 .. 5.10 su
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Ti2 - N4 .. 8.57 su
0 ALERT level A = In general: serious problem
1 ALERT level B = Potentially serious problem
2 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
3 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
0 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997); cell refinement: COLLECT and DENZO; data reduction: COLLECT and DENZO; program(s) used to solve structure: SIR92 (Altomare et al., 1994); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: PLATON (Spek, 2003); software used to prepare material for publication: SHELXL97.
µ-Oxo-bis[azidobis(
η5-cyclopentadienyl)titanium(IV)]
top
Crystal data top
[Ti2(C5H5)4(N3)2O] | F(000) = 936 |
Mr = 456.22 | Dx = 1.540 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 4685 reflections |
a = 15.2860 (4) Å | θ = 1–27.5° |
b = 8.3620 (2) Å | µ = 0.84 mm−1 |
c = 15.6900 (4) Å | T = 150 K |
β = 101.0860 (16)° | Block, yellow |
V = 1968.10 (9) Å3 | 0.3 × 0.27 × 0.2 mm |
Z = 4 | |
Data collection top
Nonius KappaCCD area-detector diffractometer | 3429 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.047 |
Graphite monochromator | θmax = 27.5°, θmin = 2.7° |
Detector resolution: 9.091 pixels mm-1 | h = −19→19 |
φ and ω scans to fill the Ewald sphere | k = −10→10 |
28006 measured reflections | l = −20→20 |
4508 independent reflections | |
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)] = 0.034 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.087 | H-atom parameters constrained |
S = 1.03 | w = 1/[σ2(Fo2) + (0.041P)2 + 0.7094P] where P = (Fo2 + 2Fc2)/3 |
4508 reflections | (Δ/σ)max = 0.001 |
262 parameters | Δρmax = 0.36 e Å−3 |
0 restraints | Δρmin = −0.44 e Å−3 |
Special details top
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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Ti1 | 0.33269 (2) | 0.05934 (4) | 0.32027 (2) | 0.01948 (10) | |
Ti2 | 0.15424 (2) | −0.13263 (4) | 0.40785 (2) | 0.01953 (10) | |
O1 | 0.24461 (8) | −0.04949 (15) | 0.36006 (8) | 0.0226 (3) | |
C1 | 0.46707 (16) | −0.0964 (3) | 0.35669 (15) | 0.0420 (6) | |
H1 | 0.5040 | −0.0846 | 0.4108 | 0.050* | |
C2 | 0.39866 (16) | −0.2051 (3) | 0.33600 (15) | 0.0372 (6) | |
H2 | 0.3816 | −0.2796 | 0.3737 | 0.045* | |
C3 | 0.35932 (16) | −0.1844 (3) | 0.24870 (15) | 0.0342 (5) | |
H3 | 0.3107 | −0.2410 | 0.2185 | 0.041* | |
C4 | 0.40542 (15) | −0.0648 (3) | 0.21496 (14) | 0.0334 (5) | |
H4 | 0.3943 | −0.0298 | 0.1576 | 0.040* | |
C5 | 0.47158 (15) | −0.0058 (3) | 0.28190 (16) | 0.0382 (6) | |
H5 | 0.5110 | 0.0773 | 0.2778 | 0.046* | |
C6 | 0.20309 (14) | 0.2108 (3) | 0.25652 (14) | 0.0310 (5) | |
H6 | 0.1459 | 0.1740 | 0.2576 | 0.037* | |
C7 | 0.25229 (14) | 0.1777 (3) | 0.19171 (13) | 0.0315 (5) | |
H7 | 0.2346 | 0.1117 | 0.1438 | 0.038* | |
C8 | 0.33341 (15) | 0.2628 (2) | 0.21228 (13) | 0.0304 (5) | |
H8 | 0.3777 | 0.2657 | 0.1791 | 0.037* | |
C9 | 0.33556 (15) | 0.3416 (2) | 0.29089 (14) | 0.0309 (5) | |
H9 | 0.3818 | 0.4050 | 0.3200 | 0.037* | |
C10 | 0.25424 (14) | 0.3074 (2) | 0.31865 (14) | 0.0296 (5) | |
H10 | 0.2382 | 0.3437 | 0.3695 | 0.036* | |
C11 | 0.02101 (15) | −0.2803 (3) | 0.35727 (13) | 0.0346 (5) | |
H11 | −0.0199 | −0.2898 | 0.3939 | 0.042* | |
C12 | 0.09235 (15) | −0.3827 (3) | 0.35465 (13) | 0.0318 (5) | |
H12 | 0.1065 | −0.4742 | 0.3881 | 0.038* | |
C13 | 0.13915 (15) | −0.3235 (3) | 0.29270 (13) | 0.0318 (5) | |
H13 | 0.1906 | −0.3671 | 0.2788 | 0.038* | |
C14 | 0.09437 (15) | −0.1872 (3) | 0.25565 (13) | 0.0330 (5) | |
H14 | 0.1105 | −0.1250 | 0.2120 | 0.040* | |
C15 | 0.02172 (15) | −0.1605 (3) | 0.29502 (14) | 0.0364 (5) | |
H15 | −0.0193 | −0.0776 | 0.2823 | 0.044* | |
C16 | 0.22973 (15) | −0.3075 (3) | 0.51646 (12) | 0.0312 (5) | |
H16 | 0.2485 | −0.4053 | 0.4982 | 0.037* | |
C17 | 0.27908 (15) | −0.1656 (3) | 0.52637 (12) | 0.0307 (5) | |
H17 | 0.3374 | −0.1538 | 0.5183 | 0.037* | |
C18 | 0.22612 (15) | −0.0458 (3) | 0.55036 (12) | 0.0326 (5) | |
H18 | 0.2419 | 0.0612 | 0.5592 | 0.039* | |
C19 | 0.14388 (16) | −0.1144 (3) | 0.55912 (13) | 0.0339 (5) | |
H19 | 0.0964 | −0.0609 | 0.5755 | 0.041* | |
C20 | 0.14648 (16) | −0.2758 (3) | 0.53901 (13) | 0.0337 (5) | |
H20 | 0.1013 | −0.3498 | 0.5402 | 0.040* | |
N1 | 0.39630 (12) | 0.1419 (2) | 0.44242 (11) | 0.0300 (4) | |
N2 | 0.38763 (13) | 0.2629 (3) | 0.47710 (11) | 0.0387 (5) | |
N3 | 0.38211 (19) | 0.3815 (3) | 0.51434 (15) | 0.0690 (8) | |
N4 | 0.08360 (12) | 0.0818 (2) | 0.40632 (12) | 0.0315 (4) | |
N5 | 0.09907 (11) | 0.1920 (2) | 0.44889 (11) | 0.0282 (4) | |
N6 | 0.11234 (15) | 0.3099 (2) | 0.49174 (13) | 0.0455 (5) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ti1 | 0.01831 (19) | 0.02130 (19) | 0.01871 (17) | 0.00224 (14) | 0.00328 (13) | 0.00283 (14) |
Ti2 | 0.02191 (19) | 0.02018 (19) | 0.01691 (17) | 0.00008 (14) | 0.00476 (13) | 0.00117 (14) |
O1 | 0.0225 (7) | 0.0239 (7) | 0.0219 (7) | 0.0023 (6) | 0.0056 (5) | 0.0052 (6) |
C1 | 0.0334 (13) | 0.0570 (16) | 0.0320 (12) | 0.0275 (12) | −0.0031 (10) | −0.0068 (11) |
C2 | 0.0490 (15) | 0.0291 (12) | 0.0385 (12) | 0.0201 (11) | 0.0207 (11) | 0.0100 (10) |
C3 | 0.0360 (13) | 0.0311 (12) | 0.0380 (12) | 0.0025 (10) | 0.0139 (10) | −0.0098 (10) |
C4 | 0.0386 (13) | 0.0392 (13) | 0.0255 (11) | 0.0113 (11) | 0.0139 (9) | 0.0029 (10) |
C5 | 0.0247 (12) | 0.0391 (13) | 0.0556 (15) | 0.0030 (10) | 0.0201 (11) | −0.0068 (12) |
C6 | 0.0203 (11) | 0.0295 (11) | 0.0412 (12) | 0.0060 (9) | 0.0010 (9) | 0.0171 (10) |
C7 | 0.0360 (13) | 0.0313 (11) | 0.0235 (10) | 0.0009 (10) | −0.0032 (9) | 0.0100 (9) |
C8 | 0.0322 (12) | 0.0294 (11) | 0.0307 (11) | 0.0015 (10) | 0.0088 (9) | 0.0122 (9) |
C9 | 0.0312 (12) | 0.0214 (11) | 0.0395 (12) | 0.0005 (9) | 0.0056 (10) | 0.0063 (9) |
C10 | 0.0295 (12) | 0.0233 (10) | 0.0367 (12) | 0.0082 (9) | 0.0082 (9) | 0.0060 (9) |
C11 | 0.0286 (12) | 0.0495 (15) | 0.0250 (10) | −0.0153 (11) | 0.0034 (9) | −0.0057 (10) |
C12 | 0.0396 (13) | 0.0250 (11) | 0.0269 (11) | −0.0079 (10) | −0.0037 (9) | −0.0002 (9) |
C13 | 0.0352 (13) | 0.0291 (11) | 0.0314 (11) | −0.0055 (10) | 0.0074 (9) | −0.0113 (9) |
C14 | 0.0448 (14) | 0.0346 (12) | 0.0181 (10) | −0.0124 (11) | 0.0028 (9) | 0.0001 (9) |
C15 | 0.0348 (13) | 0.0376 (13) | 0.0306 (11) | 0.0009 (10) | −0.0090 (10) | −0.0025 (10) |
C16 | 0.0466 (14) | 0.0282 (11) | 0.0167 (9) | 0.0090 (10) | 0.0010 (9) | 0.0044 (8) |
C17 | 0.0282 (12) | 0.0444 (13) | 0.0178 (9) | 0.0014 (10) | 0.0002 (8) | 0.0057 (9) |
C18 | 0.0473 (14) | 0.0294 (12) | 0.0184 (10) | −0.0042 (11) | −0.0005 (9) | −0.0029 (9) |
C19 | 0.0407 (14) | 0.0445 (14) | 0.0185 (10) | 0.0073 (11) | 0.0110 (9) | 0.0016 (9) |
C20 | 0.0421 (14) | 0.0381 (13) | 0.0205 (10) | −0.0073 (11) | 0.0051 (9) | 0.0090 (9) |
N1 | 0.0290 (10) | 0.0281 (10) | 0.0293 (9) | 0.0046 (8) | −0.0031 (8) | −0.0027 (8) |
N2 | 0.0390 (12) | 0.0510 (13) | 0.0244 (9) | 0.0093 (10) | 0.0019 (8) | −0.0001 (10) |
N3 | 0.098 (2) | 0.0632 (16) | 0.0406 (12) | 0.0296 (15) | 0.0016 (13) | −0.0217 (12) |
N4 | 0.0267 (10) | 0.0368 (11) | 0.0308 (10) | 0.0060 (8) | 0.0047 (8) | 0.0027 (9) |
N5 | 0.0299 (10) | 0.0266 (10) | 0.0319 (10) | 0.0078 (8) | 0.0156 (8) | 0.0119 (9) |
N6 | 0.0694 (16) | 0.0300 (11) | 0.0392 (11) | 0.0002 (11) | 0.0159 (10) | 0.0004 (9) |
Geometric parameters (Å, º) top
Ti1—O1 | 1.8315 (13) | C6—C10 | 1.386 (3) |
Ti1—N1 | 2.0925 (17) | C6—C7 | 1.404 (3) |
Ti1—C7 | 2.3676 (19) | C6—H6 | 0.9300 |
Ti1—C5 | 2.379 (2) | C7—C8 | 1.412 (3) |
Ti1—C10 | 2.394 (2) | C7—H7 | 0.9300 |
Ti1—C4 | 2.398 (2) | C8—C9 | 1.393 (3) |
Ti1—C3 | 2.400 (2) | C8—H8 | 0.9300 |
Ti1—C6 | 2.401 (2) | C9—C10 | 1.423 (3) |
Ti1—C8 | 2.402 (2) | C9—H9 | 0.9300 |
Ti1—C1 | 2.406 (2) | C10—H10 | 0.9300 |
Ti1—C9 | 2.407 (2) | C11—C12 | 1.393 (3) |
Ti1—C2 | 2.424 (2) | C11—C15 | 1.401 (3) |
Ti2—O1 | 1.8309 (13) | C11—H11 | 0.9300 |
Ti2—N4 | 2.0907 (19) | C12—C13 | 1.403 (3) |
Ti2—C16 | 2.370 (2) | C12—H12 | 0.9300 |
Ti2—C12 | 2.379 (2) | C13—C14 | 1.397 (3) |
Ti2—C11 | 2.383 (2) | C13—H13 | 0.9300 |
Ti2—C13 | 2.389 (2) | C14—C15 | 1.389 (3) |
Ti2—C20 | 2.403 (2) | C14—H14 | 0.9300 |
Ti2—C18 | 2.406 (2) | C15—H15 | 0.9300 |
Ti2—C17 | 2.411 (2) | C16—C17 | 1.398 (3) |
Ti2—C19 | 2.414 (2) | C16—C20 | 1.410 (3) |
Ti2—C14 | 2.431 (2) | C16—H16 | 0.9300 |
Ti2—C15 | 2.432 (2) | C17—C18 | 1.385 (3) |
C1—C2 | 1.377 (4) | C17—H17 | 0.9300 |
C1—C5 | 1.409 (3) | C18—C19 | 1.412 (3) |
C1—H1 | 0.9300 | C18—H18 | 0.9300 |
C2—C3 | 1.397 (3) | C19—C20 | 1.388 (3) |
C2—H2 | 0.9300 | C19—H19 | 0.9300 |
C3—C4 | 1.386 (3) | C20—H20 | 0.9300 |
C3—H3 | 0.9300 | N1—N2 | 1.169 (3) |
C4—C5 | 1.400 (3) | N2—N3 | 1.162 (3) |
C4—H4 | 0.9300 | N4—N5 | 1.136 (2) |
C5—H5 | 0.9300 | N5—N6 | 1.188 (3) |
| | | |
O1—Ti1—N1 | 95.41 (7) | C17—Ti2—C15 | 167.36 (8) |
O1—Ti1—C7 | 101.71 (7) | C19—Ti2—C15 | 121.26 (8) |
N1—Ti1—C7 | 135.73 (8) | C14—Ti2—C15 | 33.19 (8) |
O1—Ti1—C5 | 136.29 (7) | Ti2—O1—Ti1 | 172.03 (8) |
N1—Ti1—C5 | 91.56 (8) | C2—C1—C5 | 108.4 (2) |
C7—Ti1—C5 | 102.86 (8) | C2—C1—Ti1 | 74.13 (13) |
O1—Ti1—C10 | 91.99 (6) | C5—C1—Ti1 | 71.80 (12) |
N1—Ti1—C10 | 82.38 (7) | C2—C1—H1 | 125.8 |
C7—Ti1—C10 | 56.75 (8) | C5—C1—H1 | 125.8 |
C5—Ti1—C10 | 131.72 (8) | Ti1—C1—H1 | 120.0 |
O1—Ti1—C4 | 119.23 (7) | C1—C2—C3 | 108.3 (2) |
N1—Ti1—C4 | 125.35 (8) | C1—C2—Ti1 | 72.75 (13) |
C7—Ti1—C4 | 80.07 (8) | C3—C2—Ti1 | 72.23 (12) |
C5—Ti1—C4 | 34.09 (8) | C1—C2—H2 | 125.9 |
C10—Ti1—C4 | 131.73 (7) | C3—C2—H2 | 125.9 |
O1—Ti1—C3 | 86.53 (7) | Ti1—C2—H2 | 120.9 |
N1—Ti1—C3 | 128.17 (8) | C4—C3—C2 | 108.0 (2) |
C7—Ti1—C3 | 93.64 (8) | C4—C3—Ti1 | 73.15 (13) |
C5—Ti1—C3 | 56.42 (8) | C2—C3—Ti1 | 74.11 (12) |
C10—Ti1—C3 | 149.43 (8) | C4—C3—H3 | 126.0 |
C4—Ti1—C3 | 33.58 (8) | C2—C3—H3 | 126.0 |
O1—Ti1—C6 | 78.60 (7) | Ti1—C3—H3 | 118.7 |
N1—Ti1—C6 | 114.11 (7) | C3—C4—C5 | 108.3 (2) |
C7—Ti1—C6 | 34.22 (7) | C3—C4—Ti1 | 73.27 (12) |
C5—Ti1—C6 | 136.09 (8) | C5—C4—Ti1 | 72.20 (12) |
C10—Ti1—C6 | 33.61 (7) | C3—C4—H4 | 125.8 |
C4—Ti1—C6 | 113.33 (8) | C5—C4—H4 | 125.8 |
C3—Ti1—C6 | 116.98 (8) | Ti1—C4—H4 | 120.5 |
O1—Ti1—C8 | 134.08 (7) | C4—C5—C1 | 106.9 (2) |
N1—Ti1—C8 | 110.37 (7) | C4—C5—Ti1 | 73.71 (12) |
C7—Ti1—C8 | 34.42 (7) | C1—C5—Ti1 | 73.94 (12) |
C5—Ti1—C8 | 81.86 (8) | C4—C5—H5 | 126.5 |
C10—Ti1—C8 | 56.57 (7) | C1—C5—H5 | 126.5 |
C4—Ti1—C8 | 75.82 (8) | Ti1—C5—H5 | 117.9 |
C3—Ti1—C8 | 104.32 (8) | C10—C6—C7 | 108.40 (19) |
C6—Ti1—C8 | 56.51 (7) | C10—C6—Ti1 | 72.91 (12) |
O1—Ti1—C1 | 107.47 (8) | C7—C6—Ti1 | 71.58 (11) |
N1—Ti1—C1 | 74.68 (8) | C10—C6—H6 | 125.8 |
C7—Ti1—C1 | 135.09 (8) | C7—C6—H6 | 125.8 |
C5—Ti1—C1 | 34.25 (8) | Ti1—C6—H6 | 121.4 |
C10—Ti1—C1 | 150.98 (9) | C6—C7—C8 | 107.75 (19) |
C4—Ti1—C1 | 56.06 (8) | C6—C7—Ti1 | 74.20 (11) |
C3—Ti1—C1 | 55.77 (8) | C8—C7—Ti1 | 74.14 (11) |
C6—Ti1—C1 | 169.26 (8) | C6—C7—H7 | 126.1 |
C8—Ti1—C1 | 115.54 (8) | C8—C7—H7 | 126.1 |
O1—Ti1—C9 | 126.46 (7) | Ti1—C7—H7 | 117.6 |
N1—Ti1—C9 | 80.19 (7) | C9—C8—C7 | 108.10 (19) |
C7—Ti1—C9 | 56.79 (8) | C9—C8—Ti1 | 73.33 (12) |
C5—Ti1—C9 | 97.25 (8) | C7—C8—Ti1 | 71.44 (11) |
C10—Ti1—C9 | 34.48 (7) | C9—C8—H8 | 125.9 |
C4—Ti1—C9 | 105.35 (8) | C7—C8—H8 | 125.9 |
C3—Ti1—C9 | 137.09 (8) | Ti1—C8—H8 | 121.0 |
C6—Ti1—C9 | 56.43 (7) | C8—C9—C10 | 107.6 (2) |
C8—Ti1—C9 | 33.68 (7) | C8—C9—Ti1 | 72.99 (12) |
C1—Ti1—C9 | 122.00 (9) | C10—C9—Ti1 | 72.28 (12) |
O1—Ti1—C2 | 80.25 (7) | C8—C9—H9 | 126.2 |
N1—Ti1—C2 | 95.55 (8) | C10—C9—H9 | 126.2 |
C7—Ti1—C2 | 127.30 (8) | Ti1—C9—H9 | 120.4 |
C5—Ti1—C2 | 56.12 (8) | C6—C10—C9 | 108.03 (19) |
C10—Ti1—C2 | 171.77 (8) | C6—C10—Ti1 | 73.48 (12) |
C4—Ti1—C2 | 55.67 (7) | C9—C10—Ti1 | 73.25 (12) |
C3—Ti1—C2 | 33.66 (8) | C6—C10—H10 | 126.0 |
C6—Ti1—C2 | 144.83 (8) | C9—C10—H10 | 126.0 |
C8—Ti1—C2 | 131.28 (8) | Ti1—C10—H10 | 119.2 |
C1—Ti1—C2 | 33.12 (8) | C12—C11—C15 | 107.9 (2) |
C9—Ti1—C2 | 153.11 (8) | C12—C11—Ti2 | 72.82 (12) |
O1—Ti2—N4 | 95.64 (7) | C15—C11—Ti2 | 74.99 (13) |
O1—Ti2—C16 | 103.14 (7) | C12—C11—H11 | 126.0 |
N4—Ti2—C16 | 135.75 (7) | C15—C11—H11 | 126.0 |
O1—Ti2—C12 | 118.06 (7) | Ti2—C11—H11 | 118.1 |
N4—Ti2—C12 | 125.45 (8) | C11—C12—C13 | 108.1 (2) |
C16—Ti2—C12 | 79.39 (8) | C11—C12—Ti2 | 73.16 (12) |
O1—Ti2—C11 | 136.38 (7) | C13—C12—Ti2 | 73.26 (12) |
N4—Ti2—C11 | 91.95 (8) | C11—C12—H12 | 126.0 |
C16—Ti2—C11 | 100.76 (8) | C13—C12—H12 | 126.0 |
C12—Ti2—C11 | 34.02 (8) | Ti2—C12—H12 | 119.5 |
O1—Ti2—C13 | 85.11 (7) | C14—C13—C12 | 107.5 (2) |
N4—Ti2—C13 | 126.14 (8) | C14—C13—Ti2 | 74.81 (12) |
C16—Ti2—C13 | 95.42 (8) | C12—C13—Ti2 | 72.51 (12) |
C12—Ti2—C13 | 34.23 (7) | C14—C13—H13 | 126.2 |
C11—Ti2—C13 | 56.63 (8) | C12—C13—H13 | 126.2 |
O1—Ti2—C20 | 134.85 (7) | Ti2—C13—H13 | 118.4 |
N4—Ti2—C20 | 109.06 (8) | C15—C14—C13 | 108.42 (19) |
C16—Ti2—C20 | 34.35 (8) | C15—C14—Ti2 | 73.44 (12) |
C12—Ti2—C20 | 77.35 (8) | C13—C14—Ti2 | 71.50 (11) |
C11—Ti2—C20 | 81.23 (8) | C15—C14—H14 | 125.8 |
C13—Ti2—C20 | 107.54 (8) | C13—C14—H14 | 125.8 |
O1—Ti2—C18 | 91.17 (7) | Ti2—C14—H14 | 121.0 |
N4—Ti2—C18 | 83.94 (8) | C14—C15—C11 | 108.0 (2) |
C16—Ti2—C18 | 56.35 (7) | C14—C15—Ti2 | 73.37 (12) |
C12—Ti2—C18 | 132.15 (7) | C11—C15—Ti2 | 71.21 (12) |
C11—Ti2—C18 | 132.38 (7) | C14—C15—H15 | 126.0 |
C13—Ti2—C18 | 149.89 (8) | C11—C15—H15 | 126.0 |
C20—Ti2—C18 | 56.19 (7) | Ti2—C15—H15 | 121.2 |
O1—Ti2—C17 | 79.15 (7) | C17—C16—C20 | 107.8 (2) |
N4—Ti2—C17 | 115.95 (8) | C17—C16—Ti2 | 74.59 (12) |
C16—Ti2—C17 | 34.00 (7) | C20—C16—Ti2 | 74.11 (12) |
C12—Ti2—C17 | 111.87 (8) | C17—C16—H16 | 126.1 |
C11—Ti2—C17 | 134.16 (8) | C20—C16—H16 | 126.1 |
C13—Ti2—C17 | 117.00 (8) | Ti2—C16—H16 | 117.3 |
C20—Ti2—C17 | 56.26 (8) | C18—C17—C16 | 108.2 (2) |
C18—Ti2—C17 | 33.42 (7) | C18—C17—Ti2 | 73.11 (12) |
O1—Ti2—C19 | 125.17 (7) | C16—C17—Ti2 | 71.41 (11) |
N4—Ti2—C19 | 79.96 (7) | C18—C17—H17 | 125.9 |
C16—Ti2—C19 | 56.43 (7) | C16—C17—H17 | 125.9 |
C12—Ti2—C19 | 107.68 (8) | Ti2—C17—H17 | 121.3 |
C11—Ti2—C19 | 98.44 (8) | C17—C18—C19 | 108.1 (2) |
C13—Ti2—C19 | 140.45 (8) | C17—C18—Ti2 | 73.47 (11) |
C20—Ti2—C19 | 33.50 (8) | C19—C18—Ti2 | 73.26 (11) |
C18—Ti2—C19 | 34.08 (8) | C17—C18—H18 | 126.0 |
C17—Ti2—C19 | 55.99 (8) | C19—C18—H18 | 126.0 |
O1—Ti2—C14 | 80.80 (7) | Ti2—C18—H18 | 119.2 |
N4—Ti2—C14 | 93.07 (8) | C20—C19—C18 | 107.9 (2) |
C16—Ti2—C14 | 129.04 (8) | C20—C19—Ti2 | 72.83 (12) |
C12—Ti2—C14 | 56.02 (7) | C18—C19—Ti2 | 72.67 (11) |
C11—Ti2—C14 | 55.90 (7) | C20—C19—H19 | 126.0 |
C13—Ti2—C14 | 33.70 (8) | C18—C19—H19 | 126.0 |
C20—Ti2—C14 | 132.57 (8) | Ti2—C19—H19 | 120.3 |
C18—Ti2—C14 | 171.13 (8) | C19—C20—C16 | 107.9 (2) |
C17—Ti2—C14 | 146.00 (8) | C19—C20—Ti2 | 73.66 (12) |
C19—Ti2—C14 | 153.44 (8) | C16—C20—Ti2 | 71.53 (11) |
O1—Ti2—C15 | 109.06 (7) | C19—C20—H20 | 126.1 |
N4—Ti2—C15 | 73.59 (8) | C16—C20—H20 | 126.1 |
C16—Ti2—C15 | 133.37 (8) | Ti2—C20—H20 | 120.5 |
C12—Ti2—C15 | 56.01 (8) | N2—N1—Ti1 | 129.62 (15) |
C11—Ti2—C15 | 33.80 (8) | N3—N2—N1 | 177.1 (2) |
C13—Ti2—C15 | 55.91 (8) | N5—N4—Ti2 | 129.81 (15) |
C20—Ti2—C15 | 113.85 (8) | N4—N5—N6 | 177.5 (2) |
C18—Ti2—C15 | 150.82 (8) | | |
Selected geometric parameters (Å, °) topCg1—Ti1 | 2.0884 (12) | Ti1—O1 | 1.8310 (14) |
Cg2—Ti1 | 2.0752 (11) | Ti2—O1 | 1.8311 (14) |
Cg3—Ti2 | 2.0890 (11) | Ti1—N1 | 2.0926 (19) |
Cg4—Ti2 | 2.0850 (10) | Ti2—N4 | 2.091 (2) |
| | | |
Cg1—Ti1—Cg2 | 131.08 (4) | O1—Ti1—N1 | 95.39 (7) |
Cg3—Ti2—Cg4 | 131.67 (5) | O1—Ti2—N4 | 95.57 (7) |
| | | |
N1—N2 | 1.171 (3) | Ti1—N1—N2 | 129.60 (16) |
N2—N3 | 1.160 (3) | Ti2—N4—N5 | 129.81 (17) |
N4—N5 | 1.138 (3) | N1—N2—N3 | 177.1 (3) |
N5—N6 | 1.187 (3) | N4—N5—N6 | 177.6 (2) |
Notes: Cg1 = centroid of atoms C1–C5, Cg2 = centroid of atoms C6–C10,
Cg3 = centroid of atoms C11-C15 and Cg4 = centroid of atoms C16–C20. |