FLP behaviour of cationic titanium complexes with tridentate Cp,O,N-ligands: highly efficient syntheses and activation reactions of C-X bonds (X = Cl, F).
Fischer, Malte; Schwitalla, Kevin; Baues, Svenja; Schmidtmann, Marc; Beckhaus, Ruediger; Dalton transactions (Cambridge, England : 2003) 48 (2019) 1516–1523; doi:10.1039/c8dt04707c

data_7048456
_publ_section_title
;
 FLP behaviour of cationic titanium complexes with tridentate
 Cp,O,N-ligands: highly efficient syntheses and activation reactions of
 C-X bonds (X = Cl, F).
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1516
_journal_page_last               1523
_journal_paper_doi               10.1039/c8dt04707c
_journal_volume                  48
_journal_year                    2019
_chemical_formula_structural
'[TiCl(C10H15)(C34H41NOCl)] [B(CH3)(C6F5)3] *0.5C6H5Br'
_chemical_formula_sum            'C66 H61.5 B Br0.5 Cl2 F15 N O Ti'
_chemical_formula_weight         1339.22
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2018-10-04 deposited with the CCDC.
2019-01-08 downloaded from the CCDC.
;
_cell_angle_alpha                71.5865(18)
_cell_angle_beta                 78.1350(19)
_cell_angle_gamma                80.585(2)
_cell_formula_units_Z            2
_cell_length_a                   11.9091(9)
_cell_length_b                   14.5982(11)
_cell_length_c                   18.1227(13)
_cell_measurement_reflns_used    9969
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.99
_cell_measurement_theta_min      2.29
_cell_volume                     2908.9(4)
_computing_cell_refinement       'Bruker SAINT V8.37A'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT V8.37A'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_unetI/netI     0.0267
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            125582
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.032
_diffrn_reflns_theta_min         1.479
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.677
_exptl_absorpt_correction_T_max  0.9260
_exptl_absorpt_correction_T_min  0.8559
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS-2016/2 (Sheldrick)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_description       block
_exptl_crystal_F_000             1372
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.140
_refine_diff_density_max         0.589
_refine_diff_density_min         -0.617
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     867
_refine_ls_number_reflns         20249
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0553
_refine_ls_R_factor_gt           0.0389
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+1.1000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0968
_refine_ls_wR_factor_ref         0.1046
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16019
_reflns_number_total             20249
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04707c2.cif
_cod_data_source_block           5c
_cod_depositor_comments
'Adding full bibliography for 7048452--7048457.cif.'
_cod_original_formula_sum        'C66 H61.50 B Br0.50 Cl2 F15 N O Ti'
_cod_database_code               7048456
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.833
_shelx_estimated_absorpt_t_max   0.911
_exptl_absorpt_special_details
;
 numerical absorption correction followed by correction based on
 symmetry-related measurements (multi-scan)
;
_shelx_res_checksum              54939