Highly Fluorinated (σ-Aryl)-Chelating Titanium(IV) Post-Metallocene: Characterization and Scalar [C–H···F–C] Coupling
Liu, Cham-Chuen; So, Loi-Chi; Lo, Jerry C. Y.; Chan, Michael C. W.; Kaneyoshi, Hiromu; Makio, Haruyuki; Organometallics 31 (2012) 5274–; doi:10.1021/om3002334

data_4078654
_publ_section_title
;
 Highly Fluorinated (\s-Aryl)-Chelating Titanium(IV) Post-Metallocene:
 Characterization and Scalar [C--H&#x00B7;&#x00B7;&#x00B7;F--C] Coupling
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              5274
_journal_paper_doi               10.1021/om3002334
_journal_volume                  31
_journal_year                    2012
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C20 H10 F9 N O'
_chemical_formula_sum            'C20 H10 F9 N O'
_chemical_formula_weight         451.29
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   4.66648(7)
_cell_length_b                   18.4940(2)
_cell_length_c                   20.8415(3)
_cell_measurement_reflns_used    8573
_cell_measurement_temperature    233(2)
_cell_measurement_theta_max      71.3298
_cell_measurement_theta_min      4.2391
_cell_volume                     1798.66(4)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_molecular_graphics
;
OLEX2: a complete structure solution, refinement and analysis program. Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341
;
_computing_publication_material
;
OLEX2: a complete structure solution, refinement and analysis program. Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      233.0
_diffrn_detector_area_resol_mean 16.127
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
1 omega  -32.00    1.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
-        0.0000  -56.0000   72.0000 33

2 omega   -2.00   27.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
-        0.0000 -118.0000 -104.0000 29

3 omega -125.00  -94.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
-      -55.0000 -157.0000 -135.0000 31

4 omega   79.00  126.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
-       55.0000  125.0000  -60.0000 47

5 omega   32.00  127.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
-       55.0000   37.0000  -90.0000 95

6 omega  -72.00  -42.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
-      -64.0000  -50.0000    0.0000 30

7 omega   37.00   62.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -25.0000   30.0000 25

8 omega   37.00   63.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -25.0000 -180.0000 26

9 omega   39.00   72.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -25.0000  -60.0000 33

10 omega   38.00   66.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -25.0000   90.0000 28

11 omega  109.00  140.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000   50.0000 -150.0000 31

12 omega   44.00   70.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -50.0000  150.0000 26

13 omega   41.00   83.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -50.0000    0.0000 42

14 omega   37.00   62.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -25.0000  120.0000 25

15 omega   96.00  170.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  111.0000   60.0000 74

16 omega  -21.00   69.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
-        0.0000   56.0000   34.0000 90

17 omega -125.00  -25.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
-      -55.0000  -77.0000  150.0000 100

18 omega -125.00  -25.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
-      -55.0000  -77.0000   90.0000 100

19 omega  -15.00   85.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
-       55.0000  -77.0000    0.0000 100

20 omega -134.00  -81.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
-      -64.0000  -50.0000  -30.0000 53

21 omega   88.00  178.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000   50.0000    0.0000 90

22 omega   80.00  178.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000   77.0000  120.0000 98

23 omega   79.00  178.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  111.0000  -90.0000 99
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.1783667
_diffrn_orient_matrix_UB_12      -0.0385072
_diffrn_orient_matrix_UB_13      -0.0519921
_diffrn_orient_matrix_UB_21      0.130575
_diffrn_orient_matrix_UB_22      0.0730585
_diffrn_orient_matrix_UB_23      -0.02004
_diffrn_orient_matrix_UB_31      0.245202
_diffrn_orient_matrix_UB_32      -0.0109798
_diffrn_orient_matrix_UB_33      0.0485553
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0189
_diffrn_reflns_av_sigmaI/netI    0.0136
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            9434
_diffrn_reflns_theta_full        66.99
_diffrn_reflns_theta_max         66.99
_diffrn_reflns_theta_min         4.24
_exptl_absorpt_coefficient_mu    1.504
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.6077
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.667
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.122
_refine_diff_density_min         -0.176
_refine_diff_density_rms         0.038
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.13(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         3175
_refine_ls_number_restraints     282
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0318
_refine_ls_R_factor_gt           0.0304
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
calc w=1/[\s^2^(Fo^2^)+(0.0533P)^2^+0.1980P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0794
_refine_ls_wR_factor_ref         0.0804
_reflns_number_gt                3031
_reflns_number_total             3175
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om3002334_si_002.cif
_cod_data_source_block           102110A_BEN
_cod_original_cell_volume        1798.65(4)
_cod_database_code               4078654