Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270100020527/ta1309sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270100020527/ta1309Isup2.hkl |
CCDC reference: 163885
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: PLATON (Spek, 1990) and WinGX (Farrugia, 1999).
[Ti2(CF3O3S)4(C14H15NO2S)2]·2CH2Cl2 | F(000) = 1392 |
Mr = 1384.6 | Dx = 1.739 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
a = 11.551 (4) Å | Cell parameters from 5304 reflections |
b = 15.068 (5) Å | θ = 2.2–25.2° |
c = 15.218 (5) Å | µ = 0.85 mm−1 |
β = 93.233 (5)° | T = 173 K |
V = 2644.4 (16) Å3 | Block, orange |
Z = 2 | 0.36 × 0.28 × 0.24 mm |
Siemens SMART CCD area-detector diffractometer | 5361 independent reflections |
Radiation source: fine-focus sealed tube | 3085 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.091 |
Detector resolution: 8.192 pixels mm-1 | θmax = 26.4°, θmin = 2.2° |
φ and ω scans | h = −14→11 |
Absorption correction: multi-scan (Blessing, 1995) | k = −18→18 |
Tmin = 0.736, Tmax = 0.816 | l = −18→18 |
31967 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)] = 0.056 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.139 | H-atom parameters constrained |
S = 1.05 | w = 1/[σ2(Fo2) + (0.0371P)2 + 7.19P] where P = (Fo2 + 2Fc2)/3 |
5361 reflections | (Δ/σ)max = 0.003 |
355 parameters | Δρmax = 1.08 e Å−3 |
0 restraints | Δρmin = −0.63 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. |
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 | 0.83851 (6) | 0.01528 (6) | 0.11056 (5) | 0.0285 (2) | |
Cl2 | 0.98422 (18) | 0.65322 (15) | 0.14334 (14) | 0.0947 (7) | |
Cl3 | 1.21642 (17) | 0.71809 (15) | 0.18596 (16) | 0.1016 (7) | |
S1 | 1.07958 (9) | −0.01810 (8) | 0.10549 (7) | 0.0285 (3) | |
S2 | 0.79252 (11) | −0.10265 (10) | 0.29089 (9) | 0.0419 (3) | |
O1 | 0.9924 (2) | −0.0887 (2) | 0.0968 (2) | 0.0308 (7) | |
O2 | 1.1510 (2) | −0.0063 (2) | 0.0297 (2) | 0.0362 (8) | |
O3 | 0.8536 (2) | −0.0405 (2) | 0.2347 (2) | 0.0324 (8) | |
O4 | 0.6699 (3) | −0.0949 (4) | 0.2808 (3) | 0.0790 (15) | |
O5 | 0.8443 (4) | −0.1885 (3) | 0.2936 (3) | 0.0753 (14) | |
O6 | 0.7381 (2) | −0.0942 (2) | 0.0814 (2) | 0.0331 (8) | |
N5 | 0.9998 (3) | 0.0645 (3) | 0.1229 (3) | 0.0315 (9) | |
F1 | 0.7902 (4) | 0.0254 (3) | 0.4072 (2) | 0.0984 (15) | |
F2 | 0.9400 (3) | −0.0564 (3) | 0.4203 (2) | 0.0881 (13) | |
F3 | 0.7791 (3) | −0.1052 (3) | 0.4615 (2) | 0.0757 (11) | |
F5 | 0.6605 (5) | −0.2705 (3) | 0.1181 (3) | 0.1167 (18) | |
F6 | 0.5431 (5) | −0.2764 (3) | 0.0037 (3) | 0.1216 (18) | |
C1 | 1.1787 (4) | −0.0356 (3) | 0.1957 (3) | 0.0312 (11) | |
C2 | 1.2966 (4) | −0.0402 (3) | 0.1862 (3) | 0.0390 (13) | |
H2 | 1.3270 | −0.0326 | 0.1300 | 0.047* | |
C3 | 1.3704 (4) | −0.0560 (4) | 0.2598 (3) | 0.0394 (13) | |
H3 | 1.4513 | −0.0607 | 0.2527 | 0.047* | |
C4 | 1.3301 (4) | −0.0651 (4) | 0.3424 (3) | 0.0390 (12) | |
C5 | 1.2108 (4) | −0.0590 (5) | 0.3511 (3) | 0.0605 (18) | |
H5 | 1.1807 | −0.0647 | 0.4076 | 0.073* | |
C6 | 1.1353 (4) | −0.0449 (5) | 0.2782 (3) | 0.0572 (18) | |
H6 | 1.0542 | −0.0415 | 0.2849 | 0.069* | |
C7 | 1.4110 (4) | −0.0789 (4) | 0.4229 (3) | 0.0515 (15) | |
H7A | 1.4915 | −0.0736 | 0.4064 | 0.077* | |
H7B | 1.3985 | −0.1381 | 0.4472 | 0.077* | |
H7C | 1.3955 | −0.0338 | 0.4672 | 0.077* | |
C8 | 1.0435 (4) | 0.1579 (4) | 0.1282 (4) | 0.0513 (15) | |
H8A | 1.0520 | 0.1827 | 0.0686 | 0.062* | |
H8B | 1.1194 | 0.1608 | 0.1616 | 0.062* | |
C9 | 0.9526 (5) | 0.2077 (4) | 0.1752 (5) | 0.072 (2) | |
H9A | 0.9549 | 0.2715 | 0.1598 | 0.086* | |
H9B | 0.9672 | 0.2018 | 0.2396 | 0.086* | |
C10 | 0.8343 (4) | 0.1688 (3) | 0.1472 (4) | 0.0458 (14) | |
C11 | 0.7878 (5) | 0.1600 (4) | 0.0605 (4) | 0.0520 (15) | |
H11 | 0.8175 | 0.1900 | 0.0076 | 0.062* | |
C12 | 0.6870 (5) | 0.1105 (4) | 0.0621 (4) | 0.0534 (16) | |
H12 | 0.6316 | 0.0995 | 0.0103 | 0.064* | |
C13 | 0.6683 (4) | 0.0874 (4) | 0.1490 (4) | 0.0486 (15) | |
H13 | 0.5974 | 0.0583 | 0.1704 | 0.058* | |
C14 | 0.7611 (4) | 0.1239 (3) | 0.2024 (4) | 0.0430 (13) | |
H14 | 0.7675 | 0.1241 | 0.2682 | 0.052* | |
C15 | 0.8282 (5) | −0.0569 (4) | 0.4004 (4) | 0.0537 (15) | |
C17 | 1.07462 (14) | 0.70718 (12) | 0.22095 (13) | 0.079 (2) | |
H17A | 1.0768 | 0.6734 | 0.2768 | 0.095* | |
H17B | 1.0428 | 0.7668 | 0.2323 | 0.095* | |
S3A | 0.62669 (14) | −0.12168 (12) | 0.03894 (13) | 0.0375 (7) | 0.633 (4) |
O7A | 0.59481 (14) | −0.08620 (12) | −0.04203 (13) | 0.057 (2) | 0.633 (4) |
O8A | 0.53096 (14) | −0.10674 (12) | 0.08949 (13) | 0.064 (2) | 0.633 (4) |
F4A | 0.73983 (14) | −0.26102 (12) | −0.00672 (13) | 0.114 (3) | 0.633 (4) |
C16A | 0.65148 (14) | −0.24094 (12) | 0.03861 (13) | 0.060 (3) | 0.633 (4) |
S3B | 0.66565 (14) | −0.14196 (12) | 0.00526 (13) | 0.0462 (14) | 0.367 (4) |
O7B | 0.73007 (14) | −0.20564 (12) | −0.05202 (13) | 0.077 (5) | 0.367 (4) |
O8B | 0.62735 (14) | −0.11432 (12) | −0.06406 (13) | 0.068 (4) | 0.367 (4) |
F4B | 0.51622 (14) | −0.17130 (12) | 0.11759 (13) | 0.070 (3) | 0.367 (4) |
C16B | 0.58562 (14) | −0.21747 (12) | 0.06659 (13) | 0.054 (5)* | 0.367 (4) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ti1 | 0.0172 (4) | 0.0350 (5) | 0.0332 (5) | 0.0014 (4) | 0.0006 (3) | 0.0002 (4) |
Cl2 | 0.0852 (14) | 0.1100 (17) | 0.0861 (14) | 0.0010 (12) | −0.0194 (11) | −0.0298 (12) |
Cl3 | 0.0699 (13) | 0.0981 (16) | 0.136 (2) | 0.0004 (11) | −0.0033 (12) | 0.0263 (14) |
S1 | 0.0157 (5) | 0.0393 (7) | 0.0302 (6) | −0.0001 (5) | −0.0012 (4) | 0.0026 (6) |
S2 | 0.0331 (7) | 0.0511 (9) | 0.0421 (8) | −0.0083 (6) | 0.0087 (6) | 0.0022 (7) |
O1 | 0.0212 (16) | 0.040 (2) | 0.0314 (17) | −0.0021 (14) | 0.0010 (13) | 0.0007 (15) |
O2 | 0.0178 (15) | 0.061 (2) | 0.0299 (17) | −0.0002 (15) | −0.0004 (13) | 0.0083 (16) |
O3 | 0.0217 (15) | 0.045 (2) | 0.0308 (18) | 0.0011 (14) | 0.0037 (13) | 0.0004 (15) |
O4 | 0.031 (2) | 0.152 (5) | 0.055 (3) | −0.021 (3) | 0.0088 (19) | 0.020 (3) |
O5 | 0.104 (4) | 0.042 (3) | 0.082 (3) | 0.000 (2) | 0.034 (3) | 0.006 (2) |
O6 | 0.0197 (16) | 0.044 (2) | 0.0357 (18) | −0.0018 (14) | −0.0011 (13) | 0.0021 (16) |
N5 | 0.0200 (19) | 0.034 (2) | 0.039 (2) | 0.0003 (17) | −0.0041 (16) | 0.0044 (19) |
F1 | 0.168 (4) | 0.074 (3) | 0.055 (2) | 0.030 (3) | 0.020 (3) | −0.009 (2) |
F2 | 0.056 (2) | 0.157 (4) | 0.050 (2) | −0.018 (2) | −0.0075 (18) | 0.007 (2) |
F3 | 0.086 (3) | 0.098 (3) | 0.046 (2) | −0.007 (2) | 0.0214 (19) | 0.016 (2) |
F5 | 0.153 (4) | 0.071 (3) | 0.119 (4) | −0.022 (3) | −0.047 (3) | 0.053 (3) |
F6 | 0.144 (4) | 0.078 (3) | 0.137 (4) | −0.062 (3) | −0.037 (3) | −0.014 (3) |
C1 | 0.022 (2) | 0.040 (3) | 0.031 (3) | 0.001 (2) | −0.0051 (19) | 0.004 (2) |
C2 | 0.023 (2) | 0.058 (4) | 0.036 (3) | −0.003 (2) | 0.002 (2) | 0.010 (3) |
C3 | 0.021 (2) | 0.057 (3) | 0.039 (3) | 0.002 (2) | −0.002 (2) | 0.008 (3) |
C4 | 0.027 (3) | 0.054 (3) | 0.036 (3) | 0.005 (2) | −0.004 (2) | −0.003 (3) |
C5 | 0.029 (3) | 0.127 (6) | 0.026 (3) | 0.007 (3) | 0.001 (2) | −0.001 (3) |
C6 | 0.024 (3) | 0.114 (6) | 0.034 (3) | 0.008 (3) | 0.000 (2) | −0.001 (3) |
C7 | 0.036 (3) | 0.083 (5) | 0.033 (3) | 0.009 (3) | −0.008 (2) | −0.003 (3) |
C8 | 0.028 (3) | 0.042 (3) | 0.084 (4) | −0.007 (2) | −0.002 (3) | 0.002 (3) |
C9 | 0.051 (4) | 0.040 (4) | 0.124 (6) | −0.007 (3) | 0.005 (4) | −0.016 (4) |
C10 | 0.035 (3) | 0.030 (3) | 0.073 (4) | 0.009 (2) | 0.005 (3) | −0.005 (3) |
C11 | 0.048 (4) | 0.042 (3) | 0.067 (4) | 0.017 (3) | 0.009 (3) | 0.016 (3) |
C12 | 0.034 (3) | 0.062 (4) | 0.062 (4) | 0.028 (3) | −0.015 (3) | −0.004 (3) |
C13 | 0.022 (3) | 0.049 (4) | 0.077 (4) | 0.007 (2) | 0.014 (3) | −0.008 (3) |
C14 | 0.038 (3) | 0.037 (3) | 0.055 (3) | 0.015 (2) | 0.006 (3) | −0.009 (3) |
C15 | 0.056 (4) | 0.060 (4) | 0.046 (4) | 0.006 (3) | 0.012 (3) | 0.005 (3) |
C17 | 0.078 (5) | 0.084 (5) | 0.074 (5) | −0.019 (4) | 0.007 (4) | −0.019 (4) |
S3A | 0.0243 (12) | 0.0412 (14) | 0.0465 (15) | −0.0019 (10) | −0.0036 (10) | −0.0077 (11) |
O7A | 0.051 (4) | 0.069 (5) | 0.048 (4) | −0.023 (4) | −0.033 (3) | 0.025 (4) |
O8A | 0.019 (3) | 0.088 (6) | 0.084 (5) | −0.001 (3) | 0.008 (3) | −0.038 (4) |
F4A | 0.078 (5) | 0.090 (6) | 0.175 (9) | 0.026 (4) | 0.013 (5) | −0.062 (6) |
C16A | 0.052 (6) | 0.056 (7) | 0.071 (7) | −0.016 (5) | −0.008 (5) | 0.000 (6) |
S3B | 0.036 (2) | 0.056 (3) | 0.046 (3) | −0.010 (2) | −0.005 (2) | 0.003 (2) |
O7B | 0.042 (7) | 0.125 (13) | 0.067 (9) | 0.004 (8) | 0.029 (6) | −0.036 (9) |
O8B | 0.082 (9) | 0.085 (10) | 0.037 (7) | −0.016 (8) | 0.000 (7) | 0.013 (7) |
F4B | 0.054 (6) | 0.097 (9) | 0.060 (6) | −0.007 (6) | 0.020 (5) | −0.012 (6) |
Ti1—N5 | 2.004 (4) | F5—C16A | 1.288 (5) |
Ti1—O6 | 2.051 (3) | F5—C16B | 1.387 (4) |
Ti1—O3 | 2.066 (3) | F6—C16B | 1.376 (4) |
Ti1—O2i | 2.149 (3) | F6—C16A | 1.435 (4) |
Ti1—C13 | 2.349 (5) | C1—C2 | 1.380 (6) |
Ti1—C12 | 2.350 (5) | C1—C6 | 1.384 (7) |
Ti1—C14 | 2.360 (5) | C2—C3 | 1.389 (6) |
Ti1—C11 | 2.372 (5) | C3—C4 | 1.372 (7) |
Ti1—C10 | 2.381 (5) | C4—C5 | 1.395 (7) |
Ti1—O1 | 2.388 (3) | C4—C7 | 1.512 (7) |
Ti1—S1 | 2.8350 (16) | C5—C6 | 1.388 (7) |
Cl2—C17 | 1.734 (2) | C8—C9 | 1.504 (8) |
Cl3—C17 | 1.758 (3) | C9—C10 | 1.525 (8) |
S1—O2 | 1.466 (3) | C10—C14 | 1.401 (7) |
S1—O1 | 1.467 (3) | C10—C11 | 1.402 (8) |
S1—N5 | 1.579 (4) | C11—C12 | 1.384 (8) |
S1—C1 | 1.758 (4) | C12—C13 | 1.397 (8) |
S2—O4 | 1.421 (4) | C13—C14 | 1.418 (7) |
S2—O5 | 1.425 (4) | S3A—O7A | 1.3742 |
S2—O3 | 1.474 (3) | S3A—O8A | 1.4004 |
S2—C15 | 1.829 (6) | S3A—C16A | 1.8196 |
O2—Ti1i | 2.149 (3) | F4A—C16A | 1.2994 |
O6—S3A | 1.467 (3) | S3B—O8B | 1.1956 |
O6—S3B | 1.565 (3) | S3B—O7B | 1.5189 |
N5—C8 | 1.497 (6) | S3B—C16B | 1.7657 |
F1—C15 | 1.321 (7) | O7B—O8B | 1.8193 |
F2—C15 | 1.310 (7) | F4B—C16B | 1.3413 |
F3—C15 | 1.333 (6) | ||
N5—Ti1—O6 | 146.02 (15) | S2—O3—Ti1 | 140.35 (19) |
N5—Ti1—O3 | 92.00 (14) | S3A—O6—S3B | 28.98 (6) |
O6—Ti1—O3 | 83.59 (13) | S3A—O6—Ti1 | 142.6 (2) |
N5—Ti1—O2i | 90.67 (14) | S3B—O6—Ti1 | 143.3 (2) |
O6—Ti1—O2i | 78.31 (12) | C8—N5—S1 | 123.5 (3) |
O3—Ti1—O2i | 151.16 (14) | C8—N5—Ti1 | 131.5 (3) |
N5—Ti1—C13 | 126.31 (18) | S1—N5—Ti1 | 103.9 (2) |
O6—Ti1—C13 | 87.43 (16) | C16A—F5—C16B | 41.85 (13) |
O3—Ti1—C13 | 89.39 (18) | C16B—F6—C16A | 39.87 (12) |
O2i—Ti1—C13 | 111.80 (18) | C2—C1—C6 | 120.0 (4) |
N5—Ti1—C12 | 118.4 (2) | C2—C1—S1 | 121.9 (4) |
O6—Ti1—C12 | 91.22 (18) | C6—C1—S1 | 118.1 (3) |
O3—Ti1—C12 | 123.98 (18) | C1—C2—C3 | 119.2 (4) |
O2i—Ti1—C12 | 78.99 (17) | C4—C3—C2 | 122.1 (4) |
C13—Ti1—C12 | 34.59 (19) | C3—C4—C5 | 117.9 (4) |
N5—Ti1—C14 | 93.99 (17) | C3—C4—C7 | 122.0 (4) |
O6—Ti1—C14 | 117.21 (16) | C5—C4—C7 | 120.1 (5) |
O3—Ti1—C14 | 75.88 (16) | C6—C5—C4 | 120.9 (5) |
O2i—Ti1—C14 | 132.54 (17) | C1—C6—C5 | 119.8 (5) |
C13—Ti1—C14 | 35.05 (18) | N5—C8—C9 | 104.6 (4) |
C12—Ti1—C14 | 57.5 (2) | C8—C9—C10 | 108.3 (5) |
N5—Ti1—C11 | 84.34 (18) | C14—C10—C11 | 107.8 (5) |
O6—Ti1—C11 | 122.93 (18) | C14—C10—C9 | 125.5 (6) |
O3—Ti1—C11 | 132.39 (18) | C11—C10—C9 | 126.1 (6) |
O2i—Ti1—C11 | 76.45 (18) | C14—C10—Ti1 | 72.0 (3) |
C13—Ti1—C11 | 57.3 (2) | C11—C10—Ti1 | 72.5 (3) |
C12—Ti1—C11 | 34.08 (19) | C9—C10—Ti1 | 114.1 (3) |
C14—Ti1—C11 | 57.2 (2) | C12—C11—C10 | 108.3 (5) |
N5—Ti1—C10 | 69.49 (17) | C12—C11—Ti1 | 72.1 (3) |
O6—Ti1—C10 | 144.46 (15) | C10—C11—Ti1 | 73.2 (3) |
O3—Ti1—C10 | 100.56 (18) | C11—C12—C13 | 109.0 (5) |
O2i—Ti1—C10 | 107.25 (18) | C11—C12—Ti1 | 73.9 (3) |
C13—Ti1—C10 | 57.57 (18) | C13—C12—Ti1 | 72.7 (3) |
C12—Ti1—C10 | 57.0 (2) | C12—C13—C14 | 107.1 (5) |
C14—Ti1—C10 | 34.36 (18) | C12—C13—Ti1 | 72.7 (3) |
C11—Ti1—C10 | 34.3 (2) | C14—C13—Ti1 | 72.9 (3) |
N5—Ti1—O1 | 63.80 (13) | C10—C14—C13 | 107.8 (5) |
O6—Ti1—O1 | 82.39 (12) | C10—C14—Ti1 | 73.6 (3) |
O3—Ti1—O1 | 77.77 (11) | C13—C14—Ti1 | 72.0 (3) |
O2i—Ti1—O1 | 77.73 (11) | F2—C15—F1 | 107.7 (6) |
C13—Ti1—O1 | 164.39 (17) | F2—C15—F3 | 107.1 (5) |
C12—Ti1—O1 | 156.66 (17) | F1—C15—F3 | 107.5 (5) |
C14—Ti1—O1 | 144.67 (15) | F2—C15—S2 | 112.5 (4) |
C11—Ti1—O1 | 138.31 (16) | F1—C15—S2 | 111.5 (4) |
C10—Ti1—O1 | 133.12 (15) | F3—C15—S2 | 110.3 (4) |
N5—Ti1—S1 | 32.73 (11) | Cl2—C17—Cl3 | 111.90 (16) |
O6—Ti1—S1 | 113.31 (9) | O7A—S3A—O8A | 104.5 |
O3—Ti1—S1 | 85.42 (9) | O7A—S3A—O6 | 117.98 (14) |
O2i—Ti1—S1 | 81.45 (8) | O8A—S3A—O6 | 114.40 (15) |
C13—Ti1—S1 | 157.81 (15) | O7A—S3A—C16A | 114.6 |
C12—Ti1—S1 | 144.59 (17) | O8A—S3A—C16A | 106.8 |
C14—Ti1—S1 | 123.00 (13) | O6—S3A—C16A | 98.37 (15) |
C11—Ti1—S1 | 112.30 (14) | F5—C16A—F4A | 113.2 (3) |
C10—Ti1—S1 | 102.22 (13) | F5—C16A—F6 | 104.0 (3) |
O1—Ti1—S1 | 31.14 (8) | F4A—C16A—F6 | 114.3 (2) |
O2—S1—O1 | 115.52 (19) | F5—C16A—S3A | 110.1 (2) |
O2—S1—N5 | 113.3 (2) | F4A—C16A—S3A | 111.1 |
O1—S1—N5 | 100.53 (19) | F6—C16A—S3A | 103.6 (2) |
O2—S1—C1 | 105.22 (19) | O8B—S3B—O7B | 83.3 |
O1—S1—C1 | 112.1 (2) | O8B—S3B—O6 | 130.44 (13) |
N5—S1—C1 | 110.4 (2) | O7B—S3B—O6 | 117.15 (13) |
O2—S1—Ti1 | 126.65 (13) | O8B—S3B—C16B | 120.8 |
O1—S1—Ti1 | 57.34 (12) | O7B—S3B—C16B | 100.6 |
N5—S1—Ti1 | 43.33 (14) | O6—S3B—C16B | 100.31 (13) |
C1—S1—Ti1 | 127.06 (16) | S3B—O7B—O8B | 40.7 |
O4—S2—O5 | 119.5 (3) | S3B—O8B—O7B | 56.0 |
O4—S2—O3 | 113.1 (2) | F4B—C16B—F6 | 122.4 (3) |
O5—S2—O3 | 112.3 (2) | F4B—C16B—F5 | 110.2 (3) |
O4—S2—C15 | 103.9 (3) | F6—C16B—F5 | 102.0 (3) |
O5—S2—C15 | 104.1 (3) | F4B—C16B—S3B | 108.6 |
O3—S2—C15 | 101.4 (2) | F6—C16B—S3B | 103.0 (2) |
S1—O1—Ti1 | 91.52 (16) | F5—C16B—S3B | 110.0 (2) |
S1—O2—Ti1i | 147.09 (19) | ||
N5—Ti1—S1—O2 | −86.0 (3) | O6—Ti1—C10—C9 | 170.7 (4) |
O6—Ti1—S1—O2 | 92.1 (2) | O3—Ti1—C10—C9 | 77.0 (5) |
O3—Ti1—S1—O2 | 173.1 (2) | O2i—Ti1—C10—C9 | −95.3 (5) |
O2i—Ti1—S1—O2 | 18.9 (3) | C13—Ti1—C10—C9 | 159.4 (6) |
C13—Ti1—S1—O2 | −109.9 (5) | C12—Ti1—C10—C9 | −159.2 (6) |
C12—Ti1—S1—O2 | −38.1 (3) | C14—Ti1—C10—C9 | 121.5 (6) |
C14—Ti1—S1—O2 | −117.0 (3) | C11—Ti1—C10—C9 | −122.4 (6) |
C11—Ti1—S1—O2 | −52.6 (3) | O1—Ti1—C10—C9 | −6.1 (6) |
C10—Ti1—S1—O2 | −87.1 (2) | S1—Ti1—C10—C9 | −10.6 (5) |
O1—Ti1—S1—O2 | 99.3 (2) | C14—C10—C11—C12 | 0.2 (6) |
N5—Ti1—S1—O1 | 174.8 (3) | C9—C10—C11—C12 | 171.5 (5) |
O6—Ti1—S1—O1 | −7.14 (18) | Ti1—C10—C11—C12 | 64.0 (4) |
O3—Ti1—S1—O1 | 73.85 (17) | C14—C10—C11—Ti1 | −63.8 (4) |
O2i—Ti1—S1—O1 | −80.40 (17) | C9—C10—C11—Ti1 | 107.5 (5) |
C13—Ti1—S1—O1 | 150.9 (4) | N5—Ti1—C11—C12 | −177.6 (4) |
C12—Ti1—S1—O1 | −137.4 (3) | O6—Ti1—C11—C12 | 24.2 (4) |
C14—Ti1—S1—O1 | 143.7 (2) | O3—Ti1—C11—C12 | −90.1 (4) |
C11—Ti1—S1—O1 | −151.9 (2) | O2i—Ti1—C11—C12 | 90.3 (4) |
C10—Ti1—S1—O1 | 173.7 (2) | C13—Ti1—C11—C12 | −37.2 (3) |
O6—Ti1—S1—N5 | 178.1 (2) | C14—Ti1—C11—C12 | −79.1 (4) |
O3—Ti1—S1—N5 | −100.9 (2) | C10—Ti1—C11—C12 | −116.2 (5) |
O2i—Ti1—S1—N5 | 104.8 (2) | O1—Ti1—C11—C12 | 143.5 (3) |
C13—Ti1—S1—N5 | −23.9 (5) | S1—Ti1—C11—C12 | 165.0 (3) |
C12—Ti1—S1—N5 | 47.8 (3) | N5—Ti1—C11—C10 | −61.4 (3) |
C14—Ti1—S1—N5 | −31.0 (3) | O6—Ti1—C11—C10 | 140.4 (3) |
C11—Ti1—S1—N5 | 33.4 (3) | O3—Ti1—C11—C10 | 26.2 (4) |
C10—Ti1—S1—N5 | −1.1 (3) | O2i—Ti1—C11—C10 | −153.4 (3) |
O1—Ti1—S1—N5 | −174.8 (3) | C13—Ti1—C11—C10 | 79.1 (4) |
N5—Ti1—S1—C1 | 80.5 (3) | C12—Ti1—C11—C10 | 116.2 (5) |
O6—Ti1—S1—C1 | −101.4 (2) | C14—Ti1—C11—C10 | 37.1 (3) |
O3—Ti1—S1—C1 | −20.4 (2) | O1—Ti1—C11—C10 | −100.2 (4) |
O2i—Ti1—S1—C1 | −174.7 (2) | S1—Ti1—C11—C10 | −78.7 (3) |
C13—Ti1—S1—C1 | 56.6 (5) | C10—C11—C12—C13 | 0.0 (6) |
C12—Ti1—S1—C1 | 128.3 (3) | Ti1—C11—C12—C13 | 64.7 (4) |
C14—Ti1—S1—C1 | 49.4 (3) | C10—C11—C12—Ti1 | −64.7 (4) |
C11—Ti1—S1—C1 | 113.8 (3) | N5—Ti1—C12—C11 | 2.7 (4) |
C10—Ti1—S1—C1 | 79.4 (3) | O6—Ti1—C12—C11 | −159.9 (4) |
O1—Ti1—S1—C1 | −94.3 (3) | O3—Ti1—C12—C11 | 117.0 (4) |
O2—S1—O1—Ti1 | −118.67 (17) | O2i—Ti1—C12—C11 | −82.0 (4) |
N5—S1—O1—Ti1 | 3.65 (18) | C13—Ti1—C12—C11 | 116.4 (5) |
C1—S1—O1—Ti1 | 120.85 (19) | C14—Ti1—C12—C11 | 78.2 (4) |
N5—Ti1—O1—S1 | −3.15 (16) | C10—Ti1—C12—C11 | 37.1 (3) |
O6—Ti1—O1—S1 | 173.39 (16) | O1—Ti1—C12—C11 | −86.4 (5) |
O3—Ti1—O1—S1 | −101.57 (16) | S1—Ti1—C12—C11 | −24.4 (5) |
O2i—Ti1—O1—S1 | 93.77 (16) | N5—Ti1—C12—C13 | −113.7 (4) |
C13—Ti1—O1—S1 | −136.9 (6) | O6—Ti1—C12—C13 | 83.7 (3) |
C12—Ti1—O1—S1 | 98.2 (5) | O3—Ti1—C12—C13 | 0.6 (4) |
C14—Ti1—O1—S1 | −59.1 (3) | O2i—Ti1—C12—C13 | 161.5 (4) |
C11—Ti1—O1—S1 | 41.0 (3) | C14—Ti1—C12—C13 | −38.2 (3) |
C10—Ti1—O1—S1 | −8.5 (3) | C11—Ti1—C12—C13 | −116.4 (5) |
O1—S1—O2—Ti1i | 31.0 (5) | C10—Ti1—C12—C13 | −79.4 (4) |
N5—S1—O2—Ti1i | −84.2 (4) | O1—Ti1—C12—C13 | 157.1 (4) |
C1—S1—O2—Ti1i | 155.1 (4) | S1—Ti1—C12—C13 | −140.8 (3) |
Ti1—S1—O2—Ti1i | −36.0 (5) | C11—C12—C13—C14 | −0.1 (6) |
O4—S2—O3—Ti1 | −37.3 (4) | Ti1—C12—C13—C14 | 65.3 (3) |
O5—S2—O3—Ti1 | 101.5 (4) | C11—C12—C13—Ti1 | −65.5 (4) |
C15—S2—O3—Ti1 | −147.9 (3) | N5—Ti1—C13—C12 | 88.5 (4) |
N5—Ti1—O3—S2 | −169.4 (3) | O6—Ti1—C13—C12 | −95.9 (4) |
O6—Ti1—O3—S2 | −23.2 (3) | O3—Ti1—C13—C12 | −179.5 (4) |
O2i—Ti1—O3—S2 | −74.4 (4) | O2i—Ti1—C13—C12 | −19.6 (4) |
C13—Ti1—O3—S2 | 64.2 (3) | C14—Ti1—C13—C12 | 114.7 (5) |
C12—Ti1—O3—S2 | 63.9 (4) | C11—Ti1—C13—C12 | 36.6 (3) |
C14—Ti1—O3—S2 | 96.9 (3) | C10—Ti1—C13—C12 | 77.6 (4) |
C11—Ti1—O3—S2 | 106.4 (4) | O1—Ti1—C13—C12 | −145.1 (5) |
C10—Ti1—O3—S2 | 121.1 (3) | S1—Ti1—C13—C12 | 104.3 (5) |
O1—Ti1—O3—S2 | −106.8 (3) | N5—Ti1—C13—C14 | −26.2 (4) |
S1—Ti1—O3—S2 | −137.4 (3) | O6—Ti1—C13—C14 | 149.4 (3) |
N5—Ti1—O6—S3A | −144.1 (3) | O3—Ti1—C13—C14 | 65.8 (3) |
O3—Ti1—O6—S3A | 131.9 (4) | O2i—Ti1—C13—C14 | −134.3 (3) |
O2i—Ti1—O6—S3A | −70.7 (3) | C12—Ti1—C13—C14 | −114.7 (5) |
C13—Ti1—O6—S3A | 42.2 (4) | C11—Ti1—C13—C14 | −78.1 (4) |
C12—Ti1—O6—S3A | 7.8 (4) | C10—Ti1—C13—C14 | −37.1 (3) |
C14—Ti1—O6—S3A | 61.4 (4) | O1—Ti1—C13—C14 | 100.2 (6) |
C11—Ti1—O6—S3A | −5.5 (4) | S1—Ti1—C13—C14 | −10.4 (6) |
C10—Ti1—O6—S3A | 32.7 (5) | C11—C10—C14—C13 | −0.3 (6) |
O1—Ti1—O6—S3A | −149.7 (4) | C9—C10—C14—C13 | −171.7 (5) |
S1—Ti1—O6—S3A | −145.9 (3) | Ti1—C10—C14—C13 | −64.4 (3) |
N5—Ti1—O6—S3B | −95.0 (4) | C11—C10—C14—Ti1 | 64.1 (4) |
O3—Ti1—O6—S3B | −179.1 (3) | C9—C10—C14—Ti1 | −107.3 (5) |
O2i—Ti1—O6—S3B | −21.6 (3) | C12—C13—C14—C10 | 0.2 (6) |
C13—Ti1—O6—S3B | 91.3 (4) | Ti1—C13—C14—C10 | 65.5 (3) |
C12—Ti1—O6—S3B | 56.9 (4) | C12—C13—C14—Ti1 | −65.2 (4) |
C14—Ti1—O6—S3B | 110.4 (3) | N5—Ti1—C14—C10 | 43.6 (3) |
C11—Ti1—O6—S3B | 43.6 (4) | O6—Ti1—C14—C10 | −150.4 (3) |
C10—Ti1—O6—S3B | 81.7 (4) | O3—Ti1—C14—C10 | 134.6 (3) |
O1—Ti1—O6—S3B | −100.6 (3) | O2i—Ti1—C14—C10 | −51.0 (4) |
S1—Ti1—O6—S3B | −96.9 (3) | C13—Ti1—C14—C10 | −115.5 (5) |
O2—S1—N5—C8 | −49.9 (5) | C12—Ti1—C14—C10 | −77.8 (4) |
O1—S1—N5—C8 | −173.8 (4) | C11—Ti1—C14—C10 | −37.0 (3) |
C1—S1—N5—C8 | 67.8 (5) | O1—Ti1—C14—C10 | 91.8 (4) |
Ti1—S1—N5—C8 | −169.3 (5) | S1—Ti1—C14—C10 | 59.8 (4) |
O2—S1—N5—Ti1 | 119.38 (19) | N5—Ti1—C14—C13 | 159.1 (3) |
O1—S1—N5—Ti1 | −4.5 (2) | O6—Ti1—C14—C13 | −34.8 (4) |
C1—S1—N5—Ti1 | −122.9 (2) | O3—Ti1—C14—C13 | −109.8 (3) |
O6—Ti1—N5—C8 | 165.0 (4) | O2i—Ti1—C14—C13 | 64.5 (4) |
O3—Ti1—N5—C8 | −113.6 (5) | C12—Ti1—C14—C13 | 37.7 (3) |
O2i—Ti1—N5—C8 | 95.2 (5) | C11—Ti1—C14—C13 | 78.5 (4) |
C13—Ti1—N5—C8 | −22.9 (5) | C10—Ti1—C14—C13 | 115.5 (5) |
C12—Ti1—N5—C8 | 17.3 (5) | O1—Ti1—C14—C13 | −152.7 (3) |
C14—Ti1—N5—C8 | −37.6 (5) | S1—Ti1—C14—C13 | 175.3 (3) |
C11—Ti1—N5—C8 | 18.8 (5) | O4—S2—C15—F2 | −178.2 (5) |
C10—Ti1—N5—C8 | −13.0 (5) | O5—S2—C15—F2 | 56.0 (5) |
O1—Ti1—N5—C8 | 171.1 (5) | O3—S2—C15—F2 | −60.7 (5) |
S1—Ti1—N5—C8 | 168.1 (6) | O4—S2—C15—F1 | −57.1 (5) |
O6—Ti1—N5—S1 | −3.1 (4) | O5—S2—C15—F1 | 177.1 (4) |
O3—Ti1—N5—S1 | 78.3 (2) | O3—S2—C15—F1 | 60.4 (5) |
O2i—Ti1—N5—S1 | −72.9 (2) | O4—S2—C15—F3 | 62.3 (5) |
C13—Ti1—N5—S1 | 169.0 (2) | O5—S2—C15—F3 | −63.5 (5) |
C12—Ti1—N5—S1 | −150.8 (2) | O3—S2—C15—F3 | 179.8 (4) |
C14—Ti1—N5—S1 | 154.3 (2) | S3B—O6—S3A—O7A | −65.23 (9) |
C11—Ti1—N5—S1 | −149.3 (2) | Ti1—O6—S3A—O7A | 46.2 (4) |
C10—Ti1—N5—S1 | 178.9 (3) | S3B—O6—S3A—O8A | 171.3 |
O1—Ti1—N5—S1 | 3.01 (15) | Ti1—O6—S3A—O8A | −77.3 (3) |
O2—S1—C1—C2 | −2.9 (5) | S3B—O6—S3A—C16A | 58.4 |
O1—S1—C1—C2 | 123.4 (4) | Ti1—O6—S3A—C16A | 169.9 (3) |
N5—S1—C1—C2 | −125.4 (4) | C16B—F5—C16A—F4A | 174.8 |
Ti1—S1—C1—C2 | −171.6 (3) | C16B—F5—C16A—F6 | −60.6 (3) |
O2—S1—C1—C6 | 177.0 (5) | C16B—F5—C16A—S3A | 49.79 (13) |
O1—S1—C1—C6 | −56.7 (5) | C16B—F6—C16A—F5 | 66.1 (3) |
N5—S1—C1—C6 | 54.5 (5) | C16B—F6—C16A—F4A | −170.0 |
Ti1—S1—C1—C6 | 8.3 (5) | C16B—F6—C16A—S3A | −48.95 (14) |
C6—C1—C2—C3 | 1.4 (8) | O7A—S3A—C16A—F5 | −168.6 (3) |
S1—C1—C2—C3 | −178.7 (4) | O8A—S3A—C16A—F5 | −53.5 (3) |
C1—C2—C3—C4 | −1.7 (8) | O6—S3A—C16A—F5 | 65.3 (3) |
C2—C3—C4—C5 | 0.8 (9) | O7A—S3A—C16A—F4A | 65.2 |
C2—C3—C4—C7 | −177.7 (5) | O8A—S3A—C16A—F4A | −179.6 |
C3—C4—C5—C6 | 0.4 (10) | O6—S3A—C16A—F4A | −60.91 (15) |
C7—C4—C5—C6 | 178.9 (6) | O7A—S3A—C16A—F6 | −58.0 (2) |
C2—C1—C6—C5 | −0.2 (9) | O8A—S3A—C16A—F6 | 57.2 (2) |
S1—C1—C6—C5 | 179.8 (5) | O6—S3A—C16A—F6 | 175.9 (3) |
C4—C5—C6—C1 | −0.7 (10) | S3A—O6—S3B—O8B | 90.82 (12) |
S1—N5—C8—C9 | −161.0 (4) | Ti1—O6—S3B—O8B | −17.8 (4) |
Ti1—N5—C8—C9 | 32.9 (7) | S3A—O6—S3B—O7B | −163.9 |
N5—C8—C9—C10 | −35.3 (7) | Ti1—O6—S3B—O7B | 87.5 (3) |
C8—C9—C10—C14 | 114.7 (6) | S3A—O6—S3B—C16B | −56.21 (7) |
C8—C9—C10—C11 | −55.1 (8) | Ti1—O6—S3B—C16B | −164.8 (3) |
C8—C9—C10—Ti1 | 30.3 (7) | O6—S3B—O7B—O8B | −132.32 (15) |
N5—Ti1—C10—C14 | −132.8 (4) | C16B—S3B—O7B—O8B | 120.2 |
O6—Ti1—C10—C14 | 49.2 (5) | O6—S3B—O8B—O7B | 120.19 (17) |
O3—Ti1—C10—C14 | −44.6 (3) | C16B—S3B—O8B—O7B | −98.4 |
O2i—Ti1—C10—C14 | 143.2 (3) | C16A—F6—C16B—F4B | 179.01 (7) |
C13—Ti1—C10—C14 | 37.9 (3) | C16A—F6—C16B—F5 | −57.4 (3) |
C12—Ti1—C10—C14 | 79.3 (4) | C16A—F6—C16B—S3B | 56.66 (11) |
C11—Ti1—C10—C14 | 116.1 (5) | C16A—F5—C16B—F4B | −164.1 |
O1—Ti1—C10—C14 | −127.7 (3) | C16A—F5—C16B—F6 | 64.4 (3) |
S1—Ti1—C10—C14 | −132.1 (3) | C16A—F5—C16B—S3B | −44.42 (17) |
N5—Ti1—C10—C11 | 111.2 (4) | O8B—S3B—C16B—F4B | −87.4 |
O6—Ti1—C10—C11 | −66.9 (5) | O7B—S3B—C16B—F4B | −175.8 |
O3—Ti1—C10—C11 | −160.6 (3) | O6—S3B—C16B—F4B | 63.79 (14) |
O2i—Ti1—C10—C11 | 27.1 (3) | O8B—S3B—C16B—F6 | 43.8 (3) |
C13—Ti1—C10—C11 | −78.2 (4) | O7B—S3B—C16B—F6 | −44.6 (3) |
C12—Ti1—C10—C11 | −36.8 (3) | O6—S3B—C16B—F6 | −165.0 (3) |
C14—Ti1—C10—C11 | −116.1 (5) | O8B—S3B—C16B—F5 | 151.9 (3) |
O1—Ti1—C10—C11 | 116.3 (3) | O7B—S3B—C16B—F5 | 63.5 (3) |
S1—Ti1—C10—C11 | 111.8 (3) | O6—S3B—C16B—F5 | −56.9 (3) |
N5—Ti1—C10—C9 | −11.2 (4) |
Symmetry code: (i) −x+2, −y, −z. |
Subscribe to Acta Crystallographica Section C: Structural Chemistry
The full text of this article is available to subscribers to the journal.
- Information on subscribing
- Sample issue
- Purchase subscription
- Reduced-price subscriptions
- If you have already subscribed, you may need to register