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_7048454
_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_absolute_configuration ad
_chemical_formula_structural     Ti(CH3)(C10H15)(C23H35NO)
_chemical_formula_sum            'C34 H53 N O Ti'
_chemical_formula_weight         539.67
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2018-10-04 deposited with the CCDC.
2019-01-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5804(3)
_cell_length_b                   13.5510(4)
_cell_length_c                   18.5297(5)
_cell_measurement_reflns_used    9985
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.22
_cell_measurement_theta_min      2.20
_cell_volume                     2907.79(14)
_computing_cell_refinement       'Bruker SAINT V8.37A'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT V8.37A'
_computing_structure_refinement  'SHELXL-2018/1 (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  0.0384
_diffrn_reflns_av_unetI/netI     0.0206
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            150848
_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         36.311
_diffrn_reflns_theta_min         1.862
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.321
_exptl_absorpt_correction_T_max  0.9676
_exptl_absorpt_correction_T_min  0.8987
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS-2016/2 (Sheldrick)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.233
_exptl_crystal_description       block
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.358
_refine_diff_density_min         -0.175
_refine_diff_density_rms         0.048
_refine_ls_abs_structure_details
;
 Flack x determined using 5761 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.007(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         14105
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0255
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0350P)^2^+0.3500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0643
_refine_ls_wR_factor_ref         0.0664
_reflns_Friedel_coverage         0.828
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                13243
_reflns_number_total             14105
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04707c2.cif
_cod_data_source_block           3a
_cod_depositor_comments
'Adding full bibliography for 7048452--7048457.cif.'
_cod_database_code               7048454
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.893
_shelx_estimated_absorpt_t_max   0.962
_exptl_absorpt_special_details
;
 numerical absorption correction followed by correction based on
 symmetry-related measurements (multi-scan)
;
_shelx_res_checksum              83906