Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680200781X/ob6129sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S160053680200781X/ob6129Isup2.hkl |
CCDC reference: 189290
Key indicators
- Single-crystal X-ray study
- T = 149 K
- Mean (C-C) = 0.006 Å
- R factor = 0.044
- wR factor = 0.097
- Data-to-parameter ratio = 11.4
checkCIF results
No syntax errors found ADDSYM reports no extra symmetry
Alert Level A:
REFLT_03 From the CIF: _diffrn_reflns_theta_max 26.33 From the CIF: _reflns_number_total 2551 TEST2: Reflns within _diffrn_reflns_theta_max Count of symmetry unique reflns 3497 Completeness (_total/calc) 72.95% Alert A: < 85% complete (theta max?)
Author response: Normally a full hemisphere of data with a lot of redundancy is collected. In this case excessive buildup of ice, and subsequent loss of the crystal, restricted the collection to the first 360 degree run. There was still enough redundancy to permit adequate absorption corrections but the missed hour-glass (shaped) reciprocal-space region contains about 10-15% of the reflections. There was also an error in the indices range given for the l index. Thus the data set statistics show around 73% completeness. We believe that this has very little effect on final refined parameters, or the correctness of the structure solution. It is a small omission indeed compared with regions missed in older film methods or, indeed , in multiple run area detector experiments using Cu or other long wavelength radiation. Unfortunately, it is not possible to recollect the data. |
General Notes
REFLT_03 From the CIF: _diffrn_reflns_theta_max 26.33 From the CIF: _reflns_number_total 2551 From the CIF: _diffrn_reflns_limit_ max hkl 9. 23. 10. From the CIF: _diffrn_reflns_limit_ min hkl -9. -23. -12. TEST1: Expected hkl limits for theta max Calculated maximum hkl 9. 23. 14. Calculated minimum hkl -9. -23. -14. ALERT: Expected hkl max differ from CIF values
1 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
0 Alert Level C = Please check
Data collection: SMART (Siemens, 1996); cell refinement: SMART; data reduction: SAINT (Siemens, 1996) and SADABS (Sheldrick, 1996); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 in WinGX (Farrugia, 1997, 1999); software used to prepare material for publication: SHELXL97.
[TiCl(C5H5)(C14H15NO2S)] | F(000) = 848 |
Mr = 409.77 | Dx = 1.585 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 8192 reflections |
a = 7.9620 (18) Å | θ = 2.9–24.4° |
b = 18.734 (2) Å | µ = 0.79 mm−1 |
c = 11.6482 (15) Å | T = 149 K |
β = 98.678 (11)° | Needle, yellow |
V = 1717.5 (5) Å3 | 0.40 × 0.10 × 0.04 mm |
Z = 4 |
Siemens CCD area-detector diffractometer | 2551 independent reflections |
Radiation source: fine-focus sealed tube | 1746 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.062 |
Detector resolution: 8.192 pixels mm-1 | θmax = 26.3°, θmin = 2.1° |
φ and ω scans | h = −9→9 |
Absorption correction: multi-scan (Blessing, 1995) | k = −23→23 |
Tmin = 0.743, Tmax = 0.969 | l = −12→10 |
6268 measured reflections |
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)] = 0.044 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.097 | H-atom parameters constrained |
S = 0.97 | w = 1/[σ2(Fo2) + (0.039P)2] where P = (Fo2 + 2Fc2)/3 |
2551 reflections | (Δ/σ)max < 0.001 |
223 parameters | Δρmax = 0.29 e Å−3 |
0 restraints | Δρmin = −0.31 e Å−3 |
Experimental. Crystal decay was monitored by repeating the initial 10 frames at the end of the data collection and analyzing duplicate reflections. The standard 0.8 mm diameter collimator was used. |
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 | 0.11412 (8) | 0.20138 (3) | 0.54913 (7) | 0.0167 (2) | |
S1 | 0.23702 (13) | 0.06887 (5) | 0.73139 (11) | 0.0267 (4) | |
Cl1 | 0.22131 (13) | 0.28288 (5) | 0.69214 (11) | 0.0324 (4) | |
O1 | 0.2129 (4) | 0.12205 (15) | 0.8168 (3) | 0.0399 (9) | |
O2 | 0.1155 (3) | 0.01115 (14) | 0.7159 (3) | 0.0415 (10) | |
N1 | 0.2529 (4) | 0.10901 (15) | 0.6121 (3) | 0.0168 (9) | |
C1 | 0.4354 (5) | 0.02685 (18) | 0.7801 (4) | 0.0194 (11) | |
C2 | 0.4319 (5) | −0.03487 (19) | 0.8447 (4) | 0.0228 (12) | |
H2 | 0.3266 | −0.0557 | 0.8553 | 0.027* | |
C3 | 0.5827 (5) | −0.06577 (19) | 0.8936 (4) | 0.0246 (12) | |
H3 | 0.5798 | −0.1068 | 0.9411 | 0.030* | |
C4 | 0.7394 (5) | −0.03852 (18) | 0.8753 (4) | 0.0199 (11) | |
C5 | 0.7376 (5) | 0.02341 (19) | 0.8103 (4) | 0.0219 (11) | |
H5 | 0.8426 | 0.0436 | 0.7975 | 0.026* | |
C6 | 0.5882 (5) | 0.05680 (18) | 0.7632 (4) | 0.0217 (11) | |
H6 | 0.5907 | 0.0997 | 0.7200 | 0.026* | |
C7 | 0.9014 (5) | −0.07584 (19) | 0.9244 (4) | 0.0234 (11) | |
H7A | 0.9984 | −0.0496 | 0.9027 | 0.035* | |
H7B | 0.9005 | −0.1244 | 0.8932 | 0.035* | |
H7C | 0.9110 | −0.0778 | 1.0092 | 0.035* | |
C8 | 0.2905 (5) | 0.05928 (19) | 0.5193 (4) | 0.0250 (12) | |
H8A | 0.1838 | 0.0429 | 0.4719 | 0.030* | |
H8B | 0.3536 | 0.0171 | 0.5540 | 0.030* | |
C9 | 0.3973 (5) | 0.1009 (2) | 0.4451 (4) | 0.0285 (12) | |
H9A | 0.5135 | 0.1081 | 0.4874 | 0.034* | |
H9B | 0.4054 | 0.0747 | 0.3723 | 0.034* | |
C10 | 0.3107 (5) | 0.1711 (2) | 0.4188 (4) | 0.0225 (12) | |
C11 | 0.1469 (5) | 0.1818 (2) | 0.3542 (4) | 0.0260 (12) | |
H11 | 0.0821 | 0.1463 | 0.3007 | 0.031* | |
C12 | 0.1049 (5) | 0.2542 (2) | 0.3632 (4) | 0.0249 (12) | |
H12 | 0.0045 | 0.2787 | 0.3180 | 0.030* | |
C13 | 0.2379 (5) | 0.2875 (2) | 0.4355 (4) | 0.0258 (12) | |
H13 | 0.2476 | 0.3399 | 0.4519 | 0.031* | |
C14 | 0.3625 (5) | 0.2366 (2) | 0.4711 (4) | 0.0243 (12) | |
H14 | 0.4763 | 0.2466 | 0.5175 | 0.029* | |
C15 | −0.1163 (5) | 0.1254 (2) | 0.5748 (4) | 0.0204 (11) | |
H15 | −0.1097 | 0.0725 | 0.5850 | 0.024* | |
C16 | −0.1588 (4) | 0.1610 (2) | 0.4695 (4) | 0.0238 (12) | |
H16 | −0.1900 | 0.1379 | 0.3918 | 0.029* | |
C17 | −0.1758 (5) | 0.2345 (2) | 0.4938 (4) | 0.0241 (12) | |
H17 | −0.2192 | 0.2723 | 0.4363 | 0.029* | |
C18 | −0.1418 (5) | 0.2428 (2) | 0.6134 (4) | 0.0248 (13) | |
H18 | −0.1535 | 0.2884 | 0.6562 | 0.030* | |
C19 | −0.1014 (5) | 0.1759 (2) | 0.6652 (4) | 0.0237 (12) | |
H19 | −0.0831 | 0.1653 | 0.7503 | 0.028* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ti1 | 0.0152 (3) | 0.0183 (3) | 0.0158 (6) | −0.0004 (3) | −0.0008 (4) | 0.0002 (3) |
S1 | 0.0233 (6) | 0.0282 (6) | 0.0301 (10) | 0.0083 (4) | 0.0089 (6) | 0.0129 (5) |
Cl1 | 0.0375 (6) | 0.0278 (5) | 0.0266 (9) | 0.0052 (4) | −0.0123 (6) | −0.0082 (5) |
O1 | 0.059 (2) | 0.0439 (18) | 0.021 (3) | 0.0340 (16) | 0.0196 (18) | 0.0102 (16) |
O2 | 0.0207 (15) | 0.0433 (17) | 0.061 (3) | 0.0032 (13) | 0.0075 (17) | 0.0289 (17) |
N1 | 0.0199 (16) | 0.0218 (16) | 0.011 (3) | 0.0051 (13) | 0.0093 (17) | 0.0016 (15) |
C1 | 0.020 (2) | 0.0194 (19) | 0.019 (3) | 0.0042 (15) | 0.004 (2) | −0.0018 (18) |
C2 | 0.022 (2) | 0.021 (2) | 0.026 (3) | 0.0020 (15) | 0.005 (2) | 0.0042 (19) |
C3 | 0.030 (2) | 0.0173 (19) | 0.027 (3) | 0.0019 (16) | 0.005 (2) | 0.0057 (19) |
C4 | 0.026 (2) | 0.0168 (18) | 0.016 (3) | 0.0013 (15) | 0.001 (2) | −0.0053 (18) |
C5 | 0.021 (2) | 0.028 (2) | 0.019 (3) | −0.0047 (16) | 0.010 (2) | 0.001 (2) |
C6 | 0.029 (2) | 0.0177 (18) | 0.019 (3) | −0.0001 (15) | 0.006 (2) | 0.0026 (18) |
C7 | 0.024 (2) | 0.030 (2) | 0.016 (3) | 0.0018 (17) | 0.001 (2) | 0.0036 (19) |
C8 | 0.027 (2) | 0.022 (2) | 0.025 (4) | 0.0033 (16) | 0.002 (2) | −0.005 (2) |
C9 | 0.026 (2) | 0.043 (2) | 0.018 (4) | 0.0067 (19) | 0.007 (2) | −0.006 (2) |
C10 | 0.019 (2) | 0.037 (2) | 0.014 (3) | 0.0030 (17) | 0.011 (2) | 0.001 (2) |
C11 | 0.022 (2) | 0.043 (2) | 0.014 (4) | −0.0023 (17) | 0.008 (2) | 0.001 (2) |
C12 | 0.020 (2) | 0.041 (2) | 0.015 (4) | 0.0003 (17) | 0.008 (2) | 0.012 (2) |
C13 | 0.025 (2) | 0.027 (2) | 0.027 (4) | −0.0029 (16) | 0.009 (2) | 0.012 (2) |
C14 | 0.0125 (19) | 0.036 (2) | 0.026 (4) | −0.0065 (16) | 0.007 (2) | 0.007 (2) |
C15 | 0.017 (2) | 0.027 (2) | 0.017 (3) | −0.0023 (16) | 0.006 (2) | 0.005 (2) |
C16 | 0.013 (2) | 0.039 (2) | 0.019 (3) | −0.0059 (16) | −0.001 (2) | 0.003 (2) |
C17 | 0.014 (2) | 0.033 (2) | 0.027 (4) | 0.0053 (16) | 0.006 (2) | 0.011 (2) |
C18 | 0.022 (2) | 0.031 (2) | 0.026 (4) | 0.0081 (16) | 0.017 (3) | 0.000 (2) |
C19 | 0.019 (2) | 0.037 (2) | 0.019 (4) | 0.0010 (17) | 0.012 (2) | 0.005 (2) |
Ti1—N1 | 2.123 (3) | C7—H7A | 0.9800 |
Ti1—Cl1 | 2.3250 (13) | C7—H7B | 0.9800 |
Ti1—C11 | 2.353 (5) | C7—H7C | 0.9800 |
Ti1—C16 | 2.355 (4) | C8—C9 | 1.517 (6) |
Ti1—C12 | 2.371 (4) | C8—H8A | 0.9900 |
Ti1—C15 | 2.376 (4) | C8—H8B | 0.9900 |
Ti1—C17 | 2.383 (4) | C9—C10 | 1.496 (5) |
Ti1—C19 | 2.387 (4) | C9—H9A | 0.9900 |
Ti1—C14 | 2.390 (4) | C9—H9B | 0.9900 |
Ti1—C13 | 2.391 (4) | C10—C14 | 1.404 (5) |
Ti1—C18 | 2.403 (4) | C10—C11 | 1.418 (5) |
Ti1—C10 | 2.406 (4) | C11—C12 | 1.403 (5) |
S1—O1 | 1.441 (3) | C11—H11 | 1.0000 |
S1—O2 | 1.444 (3) | C12—C13 | 1.397 (5) |
S1—N1 | 1.602 (4) | C12—H12 | 1.0000 |
S1—C1 | 1.779 (4) | C13—C14 | 1.393 (5) |
N1—C8 | 1.491 (5) | C13—H13 | 1.0000 |
C1—C6 | 1.381 (5) | C14—H14 | 1.0000 |
C1—C2 | 1.382 (5) | C15—C16 | 1.393 (6) |
C2—C3 | 1.376 (5) | C15—C19 | 1.407 (6) |
C2—H2 | 0.9500 | C15—H15 | 1.0000 |
C3—C4 | 1.394 (5) | C16—C17 | 1.415 (5) |
C3—H3 | 0.9500 | C16—H16 | 1.0000 |
C4—C5 | 1.384 (5) | C17—C18 | 1.388 (6) |
C4—C7 | 1.502 (5) | C17—H17 | 1.0000 |
C5—C6 | 1.382 (5) | C18—C19 | 1.407 (5) |
C5—H5 | 0.9500 | C18—H18 | 1.0000 |
C6—H6 | 0.9500 | C19—H19 | 1.0000 |
N1—Ti1—Cl1 | 99.91 (9) | C3—C4—C7 | 120.6 (3) |
N1—Ti1—C11 | 94.53 (14) | C6—C5—C4 | 122.2 (4) |
Cl1—Ti1—C11 | 135.35 (11) | C6—C5—H5 | 118.9 |
N1—Ti1—C16 | 106.01 (13) | C4—C5—H5 | 118.9 |
Cl1—Ti1—C16 | 135.25 (12) | C1—C6—C5 | 119.0 (4) |
C11—Ti1—C16 | 78.45 (15) | C1—C6—H6 | 120.5 |
N1—Ti1—C12 | 126.73 (14) | C5—C6—H6 | 120.5 |
Cl1—Ti1—C12 | 109.75 (10) | C4—C7—H7A | 109.5 |
C11—Ti1—C12 | 34.55 (13) | C4—C7—H7B | 109.5 |
C16—Ti1—C12 | 82.78 (14) | H7A—C7—H7B | 109.5 |
N1—Ti1—C15 | 80.80 (13) | C4—C7—H7C | 109.5 |
Cl1—Ti1—C15 | 120.66 (12) | H7A—C7—H7C | 109.5 |
C11—Ti1—C15 | 103.21 (15) | H7B—C7—H7C | 109.5 |
C16—Ti1—C15 | 34.24 (13) | N1—C8—C9 | 106.5 (3) |
C12—Ti1—C15 | 116.51 (14) | N1—C8—H8A | 110.4 |
N1—Ti1—C17 | 137.56 (13) | C9—C8—H8A | 110.4 |
Cl1—Ti1—C17 | 105.00 (11) | N1—C8—H8B | 110.4 |
C11—Ti1—C17 | 91.32 (16) | C9—C8—H8B | 110.4 |
C16—Ti1—C17 | 34.75 (13) | H8A—C8—H8B | 108.6 |
C12—Ti1—C17 | 75.46 (15) | C10—C9—C8 | 106.7 (3) |
C15—Ti1—C17 | 56.98 (13) | C10—C9—H9A | 110.4 |
N1—Ti1—C19 | 91.30 (13) | C8—C9—H9A | 110.4 |
Cl1—Ti1—C19 | 86.73 (11) | C10—C9—H9B | 110.4 |
C11—Ti1—C19 | 135.17 (15) | C8—C9—H9B | 110.4 |
C16—Ti1—C19 | 57.30 (16) | H9A—C9—H9B | 108.6 |
C12—Ti1—C19 | 132.41 (14) | C14—C10—C11 | 107.0 (3) |
C15—Ti1—C19 | 34.36 (14) | C14—C10—C9 | 125.7 (4) |
C17—Ti1—C19 | 57.02 (15) | C11—C10—C9 | 126.3 (4) |
N1—Ti1—C14 | 86.51 (13) | C14—C10—Ti1 | 72.4 (2) |
Cl1—Ti1—C14 | 81.70 (11) | C11—C10—Ti1 | 70.6 (2) |
C11—Ti1—C14 | 57.16 (14) | C9—C10—Ti1 | 113.7 (3) |
C16—Ti1—C14 | 134.90 (16) | C12—C11—C10 | 107.9 (4) |
C12—Ti1—C14 | 56.72 (14) | C12—C11—Ti1 | 73.4 (3) |
C15—Ti1—C14 | 155.79 (15) | C10—C11—Ti1 | 74.7 (3) |
C17—Ti1—C14 | 130.41 (15) | C12—C11—H11 | 125.7 |
C19—Ti1—C14 | 167.66 (15) | C10—C11—H11 | 125.7 |
N1—Ti1—C13 | 120.30 (13) | Ti1—C11—H11 | 125.7 |
Cl1—Ti1—C13 | 79.40 (12) | C13—C12—C11 | 108.0 (3) |
C11—Ti1—C13 | 57.04 (14) | C13—C12—Ti1 | 73.7 (3) |
C16—Ti1—C13 | 115.54 (14) | C11—C12—Ti1 | 72.0 (3) |
C12—Ti1—C13 | 34.11 (13) | C13—C12—H12 | 125.8 |
C15—Ti1—C13 | 149.78 (14) | C11—C12—H12 | 125.8 |
C17—Ti1—C13 | 97.91 (14) | Ti1—C12—H12 | 125.8 |
C19—Ti1—C13 | 147.08 (13) | C14—C13—C12 | 108.3 (4) |
C14—Ti1—C13 | 33.88 (12) | C14—C13—Ti1 | 73.0 (2) |
N1—Ti1—C18 | 125.26 (14) | C12—C13—Ti1 | 72.2 (2) |
Cl1—Ti1—C18 | 78.55 (11) | C14—C13—H13 | 125.7 |
C11—Ti1—C18 | 124.99 (15) | C12—C13—H13 | 125.7 |
C16—Ti1—C18 | 56.70 (15) | Ti1—C13—H13 | 125.7 |
C12—Ti1—C18 | 103.81 (15) | C13—C14—C10 | 108.6 (4) |
C15—Ti1—C18 | 56.43 (14) | C13—C14—Ti1 | 73.1 (2) |
C17—Ti1—C18 | 33.70 (14) | C10—C14—Ti1 | 73.6 (2) |
C19—Ti1—C18 | 34.16 (13) | C13—C14—H14 | 125.5 |
C14—Ti1—C18 | 144.89 (13) | C10—C14—H14 | 125.5 |
C13—Ti1—C18 | 113.19 (14) | Ti1—C14—H14 | 125.5 |
N1—Ti1—C10 | 70.84 (14) | C16—C15—C19 | 108.6 (4) |
Cl1—Ti1—C10 | 113.79 (10) | C16—C15—Ti1 | 72.1 (2) |
C11—Ti1—C10 | 34.65 (13) | C19—C15—Ti1 | 73.2 (2) |
C16—Ti1—C10 | 108.97 (15) | C16—C15—H15 | 125.5 |
C12—Ti1—C10 | 57.03 (14) | C19—C15—H15 | 125.5 |
C15—Ti1—C10 | 121.76 (14) | Ti1—C15—H15 | 125.5 |
C17—Ti1—C10 | 125.88 (16) | C15—C16—C17 | 107.9 (4) |
C19—Ti1—C10 | 154.36 (13) | C15—C16—Ti1 | 73.7 (2) |
C14—Ti1—C10 | 34.04 (13) | C17—C16—Ti1 | 73.7 (2) |
C13—Ti1—C10 | 56.53 (13) | C15—C16—H16 | 125.7 |
C18—Ti1—C10 | 159.26 (16) | C17—C16—H16 | 125.7 |
O1—S1—O2 | 116.6 (2) | Ti1—C16—H16 | 125.7 |
O1—S1—N1 | 108.08 (17) | C18—C17—C16 | 107.5 (4) |
O2—S1—N1 | 112.48 (19) | C18—C17—Ti1 | 73.9 (2) |
O1—S1—C1 | 106.87 (19) | C16—C17—Ti1 | 71.5 (2) |
O2—S1—C1 | 104.75 (17) | C18—C17—H17 | 126.0 |
N1—S1—C1 | 107.56 (18) | C16—C17—H17 | 126.0 |
C8—N1—S1 | 112.7 (2) | Ti1—C17—H17 | 126.0 |
C8—N1—Ti1 | 114.2 (3) | C17—C18—C19 | 109.1 (4) |
S1—N1—Ti1 | 125.25 (19) | C17—C18—Ti1 | 72.4 (2) |
C6—C1—C2 | 120.5 (3) | C19—C18—Ti1 | 72.3 (2) |
C6—C1—S1 | 122.3 (3) | C17—C18—H18 | 125.3 |
C2—C1—S1 | 117.0 (3) | C19—C18—H18 | 125.3 |
C3—C2—C1 | 119.3 (4) | Ti1—C18—H18 | 125.3 |
C3—C2—H2 | 120.4 | C15—C19—C18 | 106.8 (4) |
C1—C2—H2 | 120.4 | C15—C19—Ti1 | 72.4 (2) |
C2—C3—C4 | 121.9 (4) | C18—C19—Ti1 | 73.6 (2) |
C2—C3—H3 | 119.1 | C15—C19—H19 | 126.3 |
C4—C3—H3 | 119.1 | C18—C19—H19 | 126.3 |
C5—C4—C3 | 117.1 (3) | Ti1—C19—H19 | 126.3 |
C5—C4—C7 | 122.4 (3) | ||
O1—S1—N1—C8 | 176.0 (3) | C19—Ti1—C13—C12 | −86.1 (4) |
O2—S1—N1—C8 | −53.9 (3) | C14—Ti1—C13—C12 | 116.3 (4) |
C1—S1—N1—C8 | 60.9 (3) | C18—Ti1—C13—C12 | −80.2 (3) |
O1—S1—N1—Ti1 | −36.9 (3) | C10—Ti1—C13—C12 | 79.2 (3) |
O2—S1—N1—Ti1 | 93.2 (2) | C12—C13—C14—C10 | 1.6 (5) |
C1—S1—N1—Ti1 | −151.96 (19) | Ti1—C13—C14—C10 | 65.6 (3) |
Cl1—Ti1—N1—C8 | −148.6 (2) | C12—C13—C14—Ti1 | −64.0 (3) |
C11—Ti1—N1—C8 | −11.0 (3) | C11—C10—C14—C13 | −2.7 (5) |
C16—Ti1—N1—C8 | 68.3 (3) | C9—C10—C14—C13 | −172.1 (4) |
C12—Ti1—N1—C8 | −24.7 (3) | Ti1—C10—C14—C13 | −65.2 (3) |
C15—Ti1—N1—C8 | 91.7 (3) | C11—C10—C14—Ti1 | 62.5 (3) |
C17—Ti1—N1—C8 | 85.9 (3) | C9—C10—C14—Ti1 | −106.9 (4) |
C19—Ti1—N1—C8 | 124.5 (3) | N1—Ti1—C14—C13 | 176.1 (3) |
C14—Ti1—N1—C8 | −67.7 (3) | Cl1—Ti1—C14—C13 | −83.3 (3) |
C13—Ti1—N1—C8 | −65.2 (3) | C11—Ti1—C14—C13 | 78.5 (3) |
C18—Ti1—N1—C8 | 128.5 (3) | C16—Ti1—C14—C13 | 66.9 (3) |
C10—Ti1—N1—C8 | −36.7 (2) | C12—Ti1—C14—C13 | 37.0 (3) |
Cl1—Ti1—N1—S1 | 64.7 (2) | C15—Ti1—C14—C13 | 117.9 (4) |
C11—Ti1—N1—S1 | −157.7 (2) | C17—Ti1—C14—C13 | 19.3 (3) |
C16—Ti1—N1—S1 | −78.5 (2) | C19—Ti1—C14—C13 | −103.8 (6) |
C12—Ti1—N1—S1 | −171.39 (18) | C18—Ti1—C14—C13 | −27.1 (4) |
C15—Ti1—N1—S1 | −55.1 (2) | C10—Ti1—C14—C13 | 115.9 (4) |
C17—Ti1—N1—S1 | −60.8 (3) | N1—Ti1—C14—C10 | 60.2 (2) |
C19—Ti1—N1—S1 | −22.2 (2) | Cl1—Ti1—C14—C10 | 160.7 (2) |
C14—Ti1—N1—S1 | 145.6 (2) | C11—Ti1—C14—C10 | −37.5 (2) |
C13—Ti1—N1—S1 | 148.1 (2) | C16—Ti1—C14—C10 | −49.0 (3) |
C18—Ti1—N1—S1 | −18.2 (3) | C12—Ti1—C14—C10 | −79.0 (3) |
C10—Ti1—N1—S1 | 176.6 (2) | C15—Ti1—C14—C10 | 1.9 (5) |
O1—S1—C1—C6 | −81.1 (4) | C17—Ti1—C14—C10 | −96.6 (3) |
O2—S1—C1—C6 | 154.7 (4) | C19—Ti1—C14—C10 | 140.3 (6) |
N1—S1—C1—C6 | 34.8 (4) | C13—Ti1—C14—C10 | −115.9 (4) |
O1—S1—C1—C2 | 93.7 (3) | C18—Ti1—C14—C10 | −143.1 (3) |
O2—S1—C1—C2 | −30.6 (4) | N1—Ti1—C15—C16 | −137.3 (3) |
N1—S1—C1—C2 | −150.5 (3) | Cl1—Ti1—C15—C16 | 126.6 (2) |
C6—C1—C2—C3 | 0.8 (6) | C11—Ti1—C15—C16 | −44.7 (3) |
S1—C1—C2—C3 | −174.0 (3) | C12—Ti1—C15—C16 | −10.7 (3) |
C1—C2—C3—C4 | −3.1 (7) | C17—Ti1—C15—C16 | 38.1 (2) |
C2—C3—C4—C5 | 3.1 (6) | C19—Ti1—C15—C16 | 116.6 (3) |
C2—C3—C4—C7 | −176.6 (4) | C14—Ti1—C15—C16 | −78.0 (4) |
C3—C4—C5—C6 | −1.0 (6) | C13—Ti1—C15—C16 | 0.2 (4) |
C7—C4—C5—C6 | 178.6 (4) | C18—Ti1—C15—C16 | 78.7 (3) |
C2—C1—C6—C5 | 1.1 (6) | C10—Ti1—C15—C16 | −76.7 (3) |
S1—C1—C6—C5 | 175.7 (3) | N1—Ti1—C15—C19 | 106.1 (2) |
C4—C5—C6—C1 | −1.0 (6) | Cl1—Ti1—C15—C19 | 10.0 (3) |
S1—N1—C8—C9 | −148.1 (3) | C11—Ti1—C15—C19 | −161.4 (2) |
Ti1—N1—C8—C9 | 61.0 (3) | C16—Ti1—C15—C19 | −116.6 (3) |
N1—C8—C9—C10 | −47.5 (4) | C12—Ti1—C15—C19 | −127.3 (2) |
C8—C9—C10—C14 | 103.9 (5) | C17—Ti1—C15—C19 | −78.5 (3) |
C8—C9—C10—C11 | −63.5 (6) | C14—Ti1—C15—C19 | 165.4 (3) |
C8—C9—C10—Ti1 | 19.2 (4) | C13—Ti1—C15—C19 | −116.4 (3) |
N1—Ti1—C10—C14 | −113.5 (3) | C18—Ti1—C15—C19 | −37.9 (2) |
Cl1—Ti1—C10—C14 | −20.9 (3) | C10—Ti1—C15—C19 | 166.7 (2) |
C11—Ti1—C10—C14 | 116.0 (3) | C19—C15—C16—C17 | −1.7 (4) |
C16—Ti1—C10—C14 | 145.6 (2) | Ti1—C15—C16—C17 | −66.3 (3) |
C12—Ti1—C10—C14 | 78.0 (3) | C19—C15—C16—Ti1 | 64.6 (3) |
C15—Ti1—C10—C14 | −179.1 (2) | N1—Ti1—C16—C15 | 44.2 (3) |
C17—Ti1—C10—C14 | 111.0 (3) | Cl1—Ti1—C16—C15 | −78.8 (3) |
C19—Ti1—C10—C14 | −161.6 (3) | C11—Ti1—C16—C15 | 135.6 (3) |
C13—Ti1—C10—C14 | 36.9 (2) | C12—Ti1—C16—C15 | 170.4 (3) |
C18—Ti1—C10—C14 | 102.6 (4) | C17—Ti1—C16—C15 | −114.8 (4) |
N1—Ti1—C10—C11 | 130.5 (2) | C19—Ti1—C16—C15 | −36.8 (2) |
Cl1—Ti1—C10—C11 | −136.9 (2) | C14—Ti1—C16—C15 | 145.5 (2) |
C16—Ti1—C10—C11 | 29.6 (3) | C13—Ti1—C16—C15 | −179.9 (2) |
C12—Ti1—C10—C11 | −38.0 (2) | C18—Ti1—C16—C15 | −77.8 (3) |
C15—Ti1—C10—C11 | 65.0 (3) | C10—Ti1—C16—C15 | 119.0 (3) |
C17—Ti1—C10—C11 | −5.0 (3) | N1—Ti1—C16—C17 | 158.9 (3) |
C19—Ti1—C10—C11 | 82.4 (4) | Cl1—Ti1—C16—C17 | 36.0 (3) |
C14—Ti1—C10—C11 | −116.0 (3) | C11—Ti1—C16—C17 | −109.6 (3) |
C13—Ti1—C10—C11 | −79.0 (2) | C12—Ti1—C16—C17 | −74.9 (3) |
C18—Ti1—C10—C11 | −13.4 (5) | C15—Ti1—C16—C17 | 114.8 (4) |
N1—Ti1—C10—C9 | 8.4 (3) | C19—Ti1—C16—C17 | 77.9 (3) |
Cl1—Ti1—C10—C9 | 101.1 (3) | C14—Ti1—C16—C17 | −99.7 (3) |
C11—Ti1—C10—C9 | −122.1 (4) | C13—Ti1—C16—C17 | −65.1 (3) |
C16—Ti1—C10—C9 | −92.5 (3) | C18—Ti1—C16—C17 | 36.9 (2) |
C12—Ti1—C10—C9 | −160.1 (3) | C10—Ti1—C16—C17 | −126.3 (3) |
C15—Ti1—C10—C9 | −57.1 (3) | C15—C16—C17—C18 | 0.6 (4) |
C17—Ti1—C10—C9 | −127.0 (3) | Ti1—C16—C17—C18 | −65.7 (3) |
C19—Ti1—C10—C9 | −39.6 (5) | C15—C16—C17—Ti1 | 66.3 (3) |
C14—Ti1—C10—C9 | 122.0 (4) | N1—Ti1—C17—C18 | 84.4 (3) |
C13—Ti1—C10—C9 | 158.9 (4) | Cl1—Ti1—C17—C18 | −39.5 (2) |
C18—Ti1—C10—C9 | −135.5 (4) | C11—Ti1—C17—C18 | −177.4 (2) |
C14—C10—C11—C12 | 2.8 (5) | C16—Ti1—C17—C18 | 115.2 (4) |
C9—C10—C11—C12 | 172.2 (4) | C12—Ti1—C17—C18 | −146.4 (3) |
Ti1—C10—C11—C12 | 66.5 (3) | C15—Ti1—C17—C18 | 77.6 (3) |
C14—C10—C11—Ti1 | −63.7 (3) | C19—Ti1—C17—C18 | 36.4 (2) |
C9—C10—C11—Ti1 | 105.7 (5) | C14—Ti1—C17—C18 | −131.3 (3) |
N1—Ti1—C11—C12 | −160.5 (2) | C13—Ti1—C17—C18 | −120.5 (2) |
Cl1—Ti1—C11—C12 | −51.5 (3) | C10—Ti1—C17—C18 | −174.6 (2) |
C16—Ti1—C11—C12 | 94.0 (2) | N1—Ti1—C17—C16 | −30.8 (4) |
C15—Ti1—C11—C12 | 117.9 (2) | Cl1—Ti1—C17—C16 | −154.6 (2) |
C17—Ti1—C11—C12 | 61.6 (2) | C11—Ti1—C17—C16 | 67.4 (3) |
C19—Ti1—C11—C12 | 103.0 (3) | C12—Ti1—C17—C16 | 98.4 (3) |
C14—Ti1—C11—C12 | −77.6 (2) | C15—Ti1—C17—C16 | −37.5 (3) |
C13—Ti1—C11—C12 | −37.0 (2) | C19—Ti1—C17—C16 | −78.8 (3) |
C18—Ti1—C11—C12 | 59.8 (3) | C14—Ti1—C17—C16 | 113.5 (3) |
C10—Ti1—C11—C12 | −114.4 (3) | C13—Ti1—C17—C16 | 124.3 (3) |
N1—Ti1—C11—C10 | −46.1 (2) | C18—Ti1—C17—C16 | −115.2 (4) |
Cl1—Ti1—C11—C10 | 62.9 (3) | C10—Ti1—C17—C16 | 70.2 (3) |
C16—Ti1—C11—C10 | −151.5 (2) | C16—C17—C18—C19 | 0.8 (4) |
C12—Ti1—C11—C10 | 114.4 (3) | Ti1—C17—C18—C19 | −63.4 (3) |
C15—Ti1—C11—C10 | −127.7 (2) | C16—C17—C18—Ti1 | 64.1 (3) |
C17—Ti1—C11—C10 | 176.0 (2) | N1—Ti1—C18—C17 | −124.7 (2) |
C19—Ti1—C11—C10 | −142.5 (2) | Cl1—Ti1—C18—C17 | 141.2 (2) |
C14—Ti1—C11—C10 | 36.8 (2) | C11—Ti1—C18—C17 | 3.1 (3) |
C13—Ti1—C11—C10 | 77.4 (2) | C16—Ti1—C18—C17 | −38.1 (2) |
C18—Ti1—C11—C10 | 174.3 (2) | C12—Ti1—C18—C17 | 33.4 (3) |
C10—C11—C12—C13 | −1.9 (5) | C15—Ti1—C18—C17 | −79.4 (3) |
Ti1—C11—C12—C13 | 65.4 (3) | C19—Ti1—C18—C17 | −117.6 (4) |
C10—C11—C12—Ti1 | −67.4 (3) | C14—Ti1—C18—C17 | 84.2 (3) |
N1—Ti1—C12—C13 | −91.2 (3) | C13—Ti1—C18—C17 | 68.1 (3) |
Cl1—Ti1—C12—C13 | 28.5 (3) | C10—Ti1—C18—C17 | 12.4 (5) |
C11—Ti1—C12—C13 | −115.7 (3) | N1—Ti1—C18—C19 | −7.1 (3) |
C16—Ti1—C12—C13 | 164.2 (3) | Cl1—Ti1—C18—C19 | −101.2 (3) |
C15—Ti1—C12—C13 | 170.2 (2) | C11—Ti1—C18—C19 | 120.7 (3) |
C17—Ti1—C12—C13 | 129.5 (3) | C16—Ti1—C18—C19 | 79.4 (3) |
C19—Ti1—C12—C13 | 132.8 (2) | C12—Ti1—C18—C19 | 151.0 (3) |
C14—Ti1—C12—C13 | −36.7 (2) | C15—Ti1—C18—C19 | 38.1 (3) |
C18—Ti1—C12—C13 | 111.1 (3) | C17—Ti1—C18—C19 | 117.6 (4) |
C10—Ti1—C12—C13 | −77.6 (3) | C14—Ti1—C18—C19 | −158.3 (3) |
N1—Ti1—C12—C11 | 24.5 (3) | C13—Ti1—C18—C19 | −174.3 (3) |
Cl1—Ti1—C12—C11 | 144.2 (2) | C10—Ti1—C18—C19 | 129.9 (4) |
C16—Ti1—C12—C11 | −80.1 (2) | C16—C15—C19—C18 | 2.2 (4) |
C15—Ti1—C12—C11 | −74.1 (3) | Ti1—C15—C19—C18 | 66.0 (3) |
C17—Ti1—C12—C11 | −114.8 (3) | C16—C15—C19—Ti1 | −63.8 (3) |
C19—Ti1—C12—C11 | −111.5 (3) | C17—C18—C19—C15 | −1.8 (4) |
C14—Ti1—C12—C11 | 79.0 (2) | Ti1—C18—C19—C15 | −65.2 (3) |
C13—Ti1—C12—C11 | 115.7 (3) | C17—C18—C19—Ti1 | 63.4 (3) |
C18—Ti1—C12—C11 | −133.2 (2) | N1—Ti1—C19—C15 | −71.5 (2) |
C10—Ti1—C12—C11 | 38.1 (2) | Cl1—Ti1—C19—C15 | −171.4 (2) |
C11—C12—C13—C14 | 0.2 (5) | C11—Ti1—C19—C15 | 26.2 (3) |
Ti1—C12—C13—C14 | 64.6 (3) | C16—Ti1—C19—C15 | 36.7 (2) |
C11—C12—C13—Ti1 | −64.3 (3) | C12—Ti1—C19—C15 | 74.6 (3) |
N1—Ti1—C13—C14 | −4.5 (3) | C17—Ti1—C19—C15 | 78.4 (3) |
Cl1—Ti1—C13—C14 | 90.9 (3) | C14—Ti1—C19—C15 | −151.1 (6) |
C11—Ti1—C13—C14 | −78.8 (3) | C13—Ti1—C19—C15 | 123.9 (3) |
C16—Ti1—C13—C14 | −133.8 (3) | C18—Ti1—C19—C15 | 114.3 (4) |
C12—Ti1—C13—C14 | −116.3 (4) | C10—Ti1—C19—C15 | −26.9 (5) |
C15—Ti1—C13—C14 | −133.9 (3) | N1—Ti1—C19—C18 | 174.2 (3) |
C17—Ti1—C13—C14 | −165.2 (3) | Cl1—Ti1—C19—C18 | 74.3 (3) |
C19—Ti1—C13—C14 | 157.6 (3) | C11—Ti1—C19—C18 | −88.0 (3) |
C18—Ti1—C13—C14 | 163.4 (3) | C16—Ti1—C19—C18 | −77.5 (3) |
C10—Ti1—C13—C14 | −37.1 (2) | C12—Ti1—C19—C18 | −39.6 (3) |
N1—Ti1—C13—C12 | 111.9 (2) | C15—Ti1—C19—C18 | −114.3 (4) |
Cl1—Ti1—C13—C12 | −152.8 (2) | C17—Ti1—C19—C18 | −35.9 (2) |
C11—Ti1—C13—C12 | 37.5 (2) | C14—Ti1—C19—C18 | 94.6 (7) |
C16—Ti1—C13—C12 | −17.4 (3) | C13—Ti1—C19—C18 | 9.7 (4) |
C15—Ti1—C13—C12 | −17.6 (4) | C10—Ti1—C19—C18 | −141.1 (3) |
C17—Ti1—C13—C12 | −48.9 (3) |
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