Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805017095/hb6211sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536805017095/hb6211Isup2.hkl |
CCDC reference: 277261
Key indicators
- Single-crystal X-ray study
- T = 150 K
- Mean (C-C)= 0.002 Å
- R factor = 0.030
- wR factor = 0.087
- Data-to-parameter ratio = 16.9
checkCIF/PLATON results
No syntax errors found No errors found in this datablock
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.
[Ti(C13H14)F2] | F(000) = 528 |
Mr = 256.14 | Dx = 1.577 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 2549 reflections |
a = 7.9700 (2) Å | θ = 1–27.5° |
b = 14.3740 (3) Å | µ = 0.79 mm−1 |
c = 9.5750 (2) Å | T = 150 K |
β = 100.3350 (15)° | Prism, orange |
V = 1079.12 (4) Å3 | 0.25 × 0.25 × 0.14 mm |
Z = 4 |
Nonius KappaCCD area-detector diffractometer | 2163 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.030 |
Graphite monochromator | θmax = 27.5°, θmin = 2.6° |
Detector resolution: 9.091 pixels mm-1 | h = −10→10 |
φ and ω scans to fill the Ewald sphere | k = −18→18 |
17813 measured reflections | l = −12→12 |
2478 independent 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)] = 0.030 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.087 | H-atom parameters constrained |
S = 0.99 | w = 1/[σ2(Fo2) + (0.0526P)2 + 0.5257P] where P = (Fo2 + 2Fc2)/3 |
2478 reflections | (Δ/σ)max = 0.001 |
147 parameters | Δρmax = 0.35 e Å−3 |
0 restraints | Δρmin = −0.43 e Å−3 |
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 | 0.28927 (3) | −0.004903 (17) | 0.20313 (3) | 0.01659 (11) | |
F1 | 0.49923 (12) | −0.06172 (7) | 0.26205 (11) | 0.0276 (2) | |
F2 | 0.21765 (12) | −0.07025 (6) | 0.03474 (9) | 0.0225 (2) | |
C1 | 0.24140 (19) | 0.15229 (10) | 0.23886 (16) | 0.0181 (3) | |
C2 | 0.4208 (2) | 0.13866 (10) | 0.26719 (18) | 0.0228 (3) | |
H2 | 0.4908 | 0.1435 | 0.3557 | 0.027* | |
C3 | 0.4752 (2) | 0.11658 (11) | 0.1387 (2) | 0.0274 (4) | |
H3 | 0.5870 | 0.1055 | 0.1277 | 0.033* | |
C4 | 0.3317 (2) | 0.11435 (11) | 0.03067 (18) | 0.0255 (3) | |
H4 | 0.3315 | 0.1018 | −0.0646 | 0.031* | |
C5 | 0.1865 (2) | 0.13451 (10) | 0.09170 (16) | 0.0201 (3) | |
H5 | 0.0742 | 0.1359 | 0.0436 | 0.024* | |
C6 | 0.11436 (19) | 0.04372 (10) | 0.36068 (16) | 0.0178 (3) | |
C7 | 0.2419 (2) | −0.01386 (11) | 0.43924 (16) | 0.0209 (3) | |
H7 | 0.3277 | 0.0055 | 0.5125 | 0.025* | |
C8 | 0.2161 (2) | −0.10609 (11) | 0.38693 (17) | 0.0241 (3) | |
H8 | 0.2812 | −0.1577 | 0.4207 | 0.029* | |
C9 | 0.0757 (2) | −0.10586 (10) | 0.27569 (17) | 0.0228 (3) | |
H9 | 0.0311 | −0.1574 | 0.2231 | 0.027* | |
C10 | 0.0132 (2) | −0.01344 (10) | 0.25701 (17) | 0.0203 (3) | |
H10 | −0.0780 | 0.0063 | 0.1889 | 0.024* | |
C11 | 0.1261 (2) | 0.14966 (10) | 0.34971 (16) | 0.0187 (3) | |
C12 | −0.0471 (2) | 0.19505 (11) | 0.29601 (18) | 0.0248 (3) | |
H12A | −0.0314 | 0.2601 | 0.2799 | 0.037* | |
H12B | −0.1190 | 0.1875 | 0.3656 | 0.037* | |
H12C | −0.0997 | 0.1660 | 0.2088 | 0.037* | |
C13 | 0.2107 (2) | 0.19457 (11) | 0.48930 (17) | 0.0252 (3) | |
H13A | 0.3179 | 0.1646 | 0.5233 | 0.038* | |
H13B | 0.1378 | 0.1879 | 0.5583 | 0.038* | |
H13C | 0.2296 | 0.2594 | 0.4740 | 0.038* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ti1 | 0.01849 (17) | 0.01446 (15) | 0.01660 (17) | 0.00030 (9) | 0.00254 (11) | −0.00073 (9) |
F1 | 0.0235 (5) | 0.0268 (5) | 0.0311 (5) | 0.0064 (4) | 0.0014 (4) | 0.0005 (4) |
F2 | 0.0280 (5) | 0.0204 (4) | 0.0190 (4) | −0.0014 (4) | 0.0039 (4) | −0.0028 (3) |
C1 | 0.0234 (7) | 0.0105 (6) | 0.0202 (7) | −0.0014 (5) | 0.0036 (6) | 0.0006 (5) |
C2 | 0.0219 (8) | 0.0175 (7) | 0.0281 (8) | −0.0036 (6) | 0.0023 (6) | −0.0024 (6) |
C3 | 0.0253 (8) | 0.0208 (7) | 0.0390 (10) | −0.0045 (6) | 0.0135 (7) | −0.0012 (7) |
C4 | 0.0342 (9) | 0.0196 (7) | 0.0257 (8) | −0.0040 (6) | 0.0134 (7) | 0.0004 (6) |
C5 | 0.0260 (8) | 0.0159 (7) | 0.0185 (7) | −0.0004 (6) | 0.0038 (6) | 0.0027 (5) |
C6 | 0.0202 (7) | 0.0192 (7) | 0.0151 (7) | −0.0008 (6) | 0.0059 (6) | 0.0002 (5) |
C7 | 0.0266 (8) | 0.0210 (7) | 0.0143 (7) | −0.0002 (6) | 0.0019 (6) | 0.0019 (6) |
C8 | 0.0338 (9) | 0.0170 (7) | 0.0219 (8) | 0.0019 (6) | 0.0065 (7) | 0.0042 (6) |
C9 | 0.0312 (8) | 0.0174 (7) | 0.0213 (8) | −0.0056 (6) | 0.0085 (6) | −0.0005 (6) |
C10 | 0.0208 (8) | 0.0206 (7) | 0.0200 (8) | −0.0035 (6) | 0.0054 (6) | 0.0006 (6) |
C11 | 0.0231 (7) | 0.0155 (7) | 0.0175 (7) | 0.0009 (5) | 0.0036 (6) | −0.0007 (5) |
C12 | 0.0258 (8) | 0.0237 (8) | 0.0258 (8) | 0.0052 (6) | 0.0072 (6) | 0.0025 (6) |
C13 | 0.0335 (9) | 0.0206 (7) | 0.0215 (8) | −0.0009 (6) | 0.0049 (7) | −0.0035 (6) |
Ti1—F1 | 1.8565 (9) | C4—H4 | 0.9300 |
Ti1—F2 | 1.8648 (9) | C5—H5 | 0.9300 |
Ti1—C1 | 2.3270 (14) | C6—C7 | 1.418 (2) |
Ti1—C6 | 2.3371 (15) | C6—C10 | 1.422 (2) |
Ti1—C2 | 2.3456 (15) | C6—C11 | 1.530 (2) |
Ti1—C5 | 2.3477 (15) | C7—C8 | 1.419 (2) |
Ti1—C10 | 2.3513 (16) | C7—H7 | 0.9300 |
Ti1—C7 | 2.3614 (16) | C8—C9 | 1.399 (2) |
Ti1—C9 | 2.4308 (16) | C8—H8 | 0.9300 |
Ti1—C8 | 2.4333 (16) | C9—C10 | 1.419 (2) |
Ti1—C3 | 2.4400 (16) | C9—H9 | 0.9300 |
Ti1—C4 | 2.4453 (16) | C10—H10 | 0.9300 |
C1—C2 | 1.420 (2) | C11—C13 | 1.528 (2) |
C1—C5 | 1.422 (2) | C11—C12 | 1.531 (2) |
C1—C11 | 1.524 (2) | C12—H12A | 0.9600 |
C2—C3 | 1.412 (2) | C12—H12B | 0.9600 |
C2—H2 | 0.9300 | C12—H12C | 0.9600 |
C3—C4 | 1.398 (2) | C13—H13A | 0.9600 |
C3—H3 | 0.9300 | C13—H13B | 0.9600 |
C4—C5 | 1.417 (2) | C13—H13C | 0.9600 |
F1—Ti1—F2 | 99.24 (4) | C3—C2—C1 | 108.68 (14) |
F1—Ti1—C1 | 123.03 (5) | C3—C2—Ti1 | 76.53 (9) |
F2—Ti1—C1 | 125.69 (5) | C1—C2—Ti1 | 71.59 (8) |
F1—Ti1—C6 | 123.02 (5) | C3—C2—H2 | 125.7 |
F2—Ti1—C6 | 125.68 (5) | C1—C2—H2 | 125.7 |
C1—Ti1—C6 | 58.82 (5) | Ti1—C2—H2 | 118.1 |
F1—Ti1—C2 | 88.36 (5) | C4—C3—C2 | 108.15 (15) |
F2—Ti1—C2 | 136.25 (5) | C4—C3—Ti1 | 73.58 (9) |
C1—Ti1—C2 | 35.38 (5) | C2—C3—Ti1 | 69.21 (9) |
C6—Ti1—C2 | 81.86 (6) | C4—C3—H3 | 125.9 |
F1—Ti1—C5 | 137.35 (5) | C2—C3—H3 | 125.9 |
F2—Ti1—C5 | 90.53 (5) | Ti1—C3—H3 | 122.9 |
C1—Ti1—C5 | 35.41 (5) | C3—C4—C5 | 108.10 (15) |
C6—Ti1—C5 | 80.69 (5) | C3—C4—Ti1 | 73.17 (9) |
C2—Ti1—C5 | 58.06 (6) | C5—C4—Ti1 | 69.07 (8) |
F1—Ti1—C10 | 137.58 (5) | C3—C4—H4 | 126.0 |
F2—Ti1—C10 | 90.58 (5) | C5—C4—H4 | 126.0 |
C1—Ti1—C10 | 80.44 (5) | Ti1—C4—H4 | 123.4 |
C6—Ti1—C10 | 35.32 (5) | C4—C5—C1 | 108.46 (14) |
C2—Ti1—C10 | 112.35 (5) | C4—C5—Ti1 | 76.62 (9) |
C5—Ti1—C10 | 83.13 (5) | C1—C5—Ti1 | 71.50 (8) |
F1—Ti1—C7 | 88.58 (5) | C4—C5—H5 | 125.8 |
F2—Ti1—C7 | 136.35 (5) | C1—C5—H5 | 125.8 |
C1—Ti1—C7 | 81.58 (5) | Ti1—C5—H5 | 118.0 |
C6—Ti1—C7 | 35.12 (5) | C7—C6—C10 | 107.20 (13) |
C2—Ti1—C7 | 86.46 (6) | C7—C6—C11 | 124.77 (14) |
C5—Ti1—C7 | 112.27 (5) | C10—C6—C11 | 124.12 (14) |
C10—Ti1—C7 | 58.03 (6) | C7—C6—Ti1 | 73.38 (9) |
F1—Ti1—C9 | 106.84 (5) | C10—C6—Ti1 | 72.89 (9) |
F2—Ti1—C9 | 79.92 (5) | C11—C6—Ti1 | 101.67 (9) |
C1—Ti1—C9 | 113.33 (5) | C6—C7—C8 | 108.26 (14) |
C6—Ti1—C9 | 57.64 (5) | C6—C7—Ti1 | 71.50 (9) |
C2—Ti1—C9 | 138.88 (6) | C8—C7—Ti1 | 75.58 (9) |
C5—Ti1—C9 | 115.74 (5) | C6—C7—H7 | 125.9 |
C10—Ti1—C9 | 34.46 (5) | C8—C7—H7 | 125.9 |
C7—Ti1—C9 | 56.87 (5) | Ti1—C7—H7 | 118.9 |
F1—Ti1—C8 | 80.63 (5) | C9—C8—C7 | 108.18 (14) |
F2—Ti1—C8 | 104.38 (5) | C9—C8—Ti1 | 73.18 (9) |
C1—Ti1—C8 | 114.03 (6) | C7—C8—Ti1 | 70.03 (9) |
C6—Ti1—C8 | 57.57 (5) | C9—C8—H8 | 125.9 |
C2—Ti1—C8 | 119.38 (6) | C7—C8—H8 | 125.9 |
C5—Ti1—C8 | 136.85 (6) | Ti1—C8—H8 | 122.5 |
C10—Ti1—C8 | 56.97 (6) | C8—C9—C10 | 108.23 (14) |
C7—Ti1—C8 | 34.39 (5) | C8—C9—Ti1 | 73.38 (9) |
C9—Ti1—C8 | 33.44 (6) | C10—C9—Ti1 | 69.70 (9) |
F1—Ti1—C3 | 80.60 (5) | C8—C9—H9 | 125.9 |
F2—Ti1—C3 | 104.32 (5) | C10—C9—H9 | 125.9 |
C1—Ti1—C3 | 57.67 (5) | Ti1—C9—H9 | 122.7 |
C6—Ti1—C3 | 114.13 (6) | C9—C10—C6 | 108.10 (14) |
C2—Ti1—C3 | 34.26 (6) | C9—C10—Ti1 | 75.83 (9) |
C5—Ti1—C3 | 56.79 (6) | C6—C10—Ti1 | 71.79 (9) |
C10—Ti1—C3 | 136.67 (6) | C9—C10—H10 | 126.0 |
C7—Ti1—C3 | 119.33 (6) | C6—C10—H10 | 126.0 |
C9—Ti1—C3 | 170.95 (5) | Ti1—C10—H10 | 118.3 |
C8—Ti1—C3 | 147.78 (6) | C1—C11—C13 | 111.85 (13) |
F1—Ti1—C4 | 106.70 (5) | C1—C11—C6 | 97.16 (11) |
F2—Ti1—C4 | 80.05 (5) | C13—C11—C6 | 112.54 (13) |
C1—Ti1—C4 | 57.64 (5) | C1—C11—C12 | 112.07 (13) |
C6—Ti1—C4 | 113.39 (5) | C13—C11—C12 | 110.11 (13) |
C2—Ti1—C4 | 56.67 (6) | C6—C11—C12 | 112.61 (13) |
C5—Ti1—C4 | 34.31 (6) | C11—C12—H12A | 109.5 |
C10—Ti1—C4 | 115.65 (6) | C11—C12—H12B | 109.5 |
C7—Ti1—C4 | 138.58 (5) | H12A—C12—H12B | 109.5 |
C9—Ti1—C4 | 143.14 (6) | C11—C12—H12C | 109.5 |
C8—Ti1—C4 | 170.93 (5) | H12A—C12—H12C | 109.5 |
C3—Ti1—C4 | 33.25 (6) | H12B—C12—H12C | 109.5 |
C2—C1—C5 | 106.56 (14) | C11—C13—H13A | 109.5 |
C2—C1—C11 | 125.14 (14) | C11—C13—H13B | 109.5 |
C5—C1—C11 | 124.69 (13) | H13A—C13—H13B | 109.5 |
C2—C1—Ti1 | 73.03 (8) | C11—C13—H13C | 109.5 |
C5—C1—Ti1 | 73.09 (8) | H13A—C13—H13C | 109.5 |
C11—C1—Ti1 | 102.33 (9) | H13B—C13—H13C | 109.5 |
Ti1-Cg1 | 2.0558 (7) | Cg1-Ti1-Cg2 | 121.50 (3) |
Ti1-Cg2 | 2.0567 (8) | F1-Ti1-F2 | 99.24 (4) |
Ti1-F1 | 1.8565 (10) | C1-C11-C6 | 97.15 (12) |
Ti1-F2 | 1.8648 (9) | C12-C11-C13 | 110.11 (13) |
Pr1-C1-C11 | 15.14 (10) | Pr2-C6-C11 | 16.31 (10) |
Pr1-Cg1-Ti1 | 85.99 (7) | Pr2-Cg2-Ti1 | 86.74 (7) |
Pr1-Pr2 | 65.76 (9) |
a) Cg1 is the centroid of the cyclopentadienyl ring C1-C5. b) Cg2 is the centroid of the cyclopentadienyl ring C6-C10. c) Pr1 is the ring plane defined by atoms C1-C5. d) Pr2 is the ring plane defined by atoms C5-C10. |
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