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_7063456
_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(C15H19)(C24H28N3OS)
_chemical_formula_sum            'C39 H47 N3 O S Ti'
_chemical_formula_weight         653.75
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2024-08-15 deposited with the CCDC.	2024-09-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.8642(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.0547(3)
_cell_length_b                   11.8933(3)
_cell_length_c                   22.4765(5)
_cell_measurement_reflns_used    9817
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.46
_cell_measurement_theta_min      4.02
_cell_volume                     3153.62(13)
_computing_cell_refinement       'Bruker SAINT V8.40B'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT V8.40B'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker Photon III CPAD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0440
_diffrn_reflns_av_unetI/netI     0.0237
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            54536
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.469
_diffrn_reflns_theta_min         3.871
_diffrn_source                   'I\mS microfocus'
_exptl_absorpt_coefficient_mu    3.200
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9074
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2016/2 (Sheldrick)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_description       block
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.515
_refine_diff_density_min         -0.260
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         6406
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0315
_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^)+(0.0450P)^2^+1.5500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0818
_refine_ls_wR_factor_ref         0.0847
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5846
_reflns_number_total             6406
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj04061a2.cif
_cod_data_source_block           Ti1d
_cod_depositor_comments
'Adding full bibliography for 7063456--7063460.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7063456
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.831
_shelx_estimated_absorpt_t_max   0.910
_shelx_res_checksum              86704
_shelx_hkl_checksum              87322