Synthesis and Coordination Behaviour of 1H-1,2,3-Triazole-4,5-Dithiolates
Schallenberg, David; Pardemann, Nils; Villinger, Alexander; Seidel, Wolfram Willy; Dalton Transactions  (2022) –; doi:10.1039/D2DT00410K

data_7711002
_publ_section_title
;
 Synthesis and Coordination Behaviour of 1H-1,2,3-Triazole-4,5-Dithiolates
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00410K
_journal_year                    2022
_chemical_formula_moiety         'C20 H19 N3 S2 Ti'
_chemical_formula_sum            'C20 H19 N3 S2 Ti'
_chemical_formula_weight         413.40
_chemical_name_systematic
'[Bis(\h5-cyclopentadienyl)(1-(2,6-dimethylphenyl)-1H-1,2,3-triazole-4,5-dithiolato)- titanium(IV)]'
_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   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2022-01-28 deposited with the CCDC.	2022-08-17 downloaded from the CCDC.
;
_cell_angle_alpha                99.292(3)
_cell_angle_beta                 102.649(3)
_cell_angle_gamma                93.060(3)
_cell_formula_units_Z            2
_cell_length_a                   7.7274(5)
_cell_length_b                   8.8234(5)
_cell_length_c                   14.3988(8)
_cell_measurement_reflns_used    6655
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.20
_cell_measurement_theta_min      2.35
_cell_volume                     941.32(10)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Apex Kappa-II-CCD-diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0457
_diffrn_reflns_av_unetI/netI     0.0535
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            26305
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.499
_diffrn_reflns_theta_min         2.541
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.685
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.6894
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_description       block
_exptl_crystal_F_000             428
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: n-pentane / dichloromethane'
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.356
_refine_diff_density_min         -0.328
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         5722
_refine_ls_number_restraints     278
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0727
_refine_ls_R_factor_gt           0.0371
_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^)+(0.0326P)^2^+0.3197P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0738
_refine_ls_wR_factor_ref         0.0858
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3910
_reflns_number_total             5722
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00410k2.cif
_cod_data_source_block           is_schal159
_cod_database_code               7711002
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.842
_shelx_estimated_absorpt_t_max   0.954
_shelx_res_checksum              5883
_shelx_hkl_checksum              99255