Syntheses and coordination chemistry of thiosemicarbazone-based titanium complexes
Schwitalla, Kevin; Claußen, Marie; Schmidtmann, Marc; Beckhaus, Rüdiger; New Journal of Chemistry 48 (2024) 18066–18074; doi:10.1039/D4NJ04061A

data_7063458
_publ_section_title
;
 Syntheses and coordination chemistry of thiosemicarbazone-based titanium
 complexes
;
_journal_issue                   42
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              18066
_journal_page_last               18074
_journal_paper_doi               10.1039/D4NJ04061A
_journal_volume                  48
_journal_year                    2024
_chemical_formula_structural     Ti(C15H18)(C15H19)(C9H9N3HS)
_chemical_formula_sum            'C39 H47 N3 S Ti'
_chemical_formula_weight         637.75
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        '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
;
2024-08-15 deposited with the CCDC.	2024-09-27 downloaded from the CCDC.
;
_cell_angle_alpha                92.218(3)
_cell_angle_beta                 107.971(3)
_cell_angle_gamma                109.627(2)
_cell_formula_units_Z            2
_cell_length_a                   11.6805(6)
_cell_length_b                   12.0032(6)
_cell_length_c                   12.9169(7)
_cell_measurement_reflns_used    9814
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      40.25
_cell_measurement_theta_min      2.27
_cell_volume                     1601.95(15)
_computing_cell_refinement       'Bruker SAINT V8.40B'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT V8.40B'
_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  0.0243
_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       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            100842
_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         40.248
_diffrn_reflns_theta_min         1.679
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.366
_exptl_absorpt_correction_T_max  0.9319
_exptl_absorpt_correction_T_min  0.8918
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS-2016/2 (Sheldrick)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.322
_exptl_crystal_description       block
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.250
_refine_diff_density_max         0.604
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     402
_refine_ls_number_reflns         20177
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0357
_refine_ls_R_factor_gt           0.0283
_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^)+(0.0400P)^2^+0.3000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0773
_refine_ls_wR_factor_ref         0.0812
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17407
_reflns_number_total             20177
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj04061a2.cif
_cod_data_source_block           Ti1a
_cod_depositor_comments
'Adding full bibliography for 7063456--7063460.cif.'
_cod_database_code               7063458
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.868
_shelx_estimated_absorpt_t_max   0.914
_exptl_absorpt_special_details
;
 numerical absorption correction followed by scaling based on
 symmetry-related measurements (multi-scan)
;
_shelx_res_checksum              9812
_shelx_hkl_checksum              40454