Stabilization of titanium(IV) and indium(III) complexes by coordination of [MoO3(1,4,7-triazacyclononane)] metalloligand in aqueous solution
Sugiarto,; Kazakami, Shota; Kawamoto, Keisuke; Hayashi, Yoshihito; Inorganica Chimica Acta 509 (2020) 119691–; doi:10.1016/j.ica.2020.119691

data_1564485
_publ_section_title
;
 Stabilization of titanium(IV) and indium(III) complexes by coordination
 of [MoO3(1,4,7-triazacyclononane)] metalloligand in aqueous solution
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119691
_journal_paper_doi               10.1016/j.ica.2020.119691
_journal_volume                  509
_journal_year                    2020
_chemical_formula_sum            'C40 H102 Cl5.01 F0 Mo6 N19 O38.04 Ti'
_chemical_formula_weight         2259.18
_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_Hall           'R 3'
_space_group_name_H-M_alt        'R 3 :H'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   21.4608(4)
_cell_length_b                   21.4608(4)
_cell_length_c                   14.8972(3)
_cell_measurement_reflns_used    9969
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      72.60
_cell_measurement_theta_min      3.80
_cell_volume                     5941.9(2)
_computing_cell_refinement       'SAINT (Bruker AXS)'
_computing_data_collection       'APEX3 (Bruker AXS)'
_computing_data_reduction        'SAINT (Bruker AXS)'
_computing_molecular_graphics    'ShelXle (H?bschle et al., 2011)'
_computing_publication_material  'APEX3 (Bruker AXS)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      93(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 goniometer'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0557
_diffrn_reflns_av_unetI/netI     0.0520
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16867
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.591
_diffrn_reflns_theta_min         3.803
_diffrn_source                   'rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    10.768
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.5950
_exptl_absorpt_correction_type   'Multi-scan (SADABS; Bruker, 2015)'
_exptl_absorpt_process_details
;
The wR2 (int) value was improved from 
0.1356 to 0.0589 after the absorption corrections by using SADABS program.
;
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.894
_exptl_crystal_description       block
_exptl_crystal_F_000             3415
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.651
_refine_diff_density_min         -1.738
_refine_diff_density_rms         0.150
_refine_ls_abs_structure_details
;
 Flack x determined using 2141 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.045(10)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         5112
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0480
_refine_ls_R_factor_gt           0.0442
_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^)+(0.0631P)^2^+66.2093P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1117
_refine_ls_wR_factor_ref         0.1140
_reflns_Friedel_coverage         0.942
_reflns_Friedel_fraction_full    0.954
_reflns_Friedel_fraction_max     0.940
_reflns_number_gt                4839
_reflns_number_total             5112
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-509-119691.cif
_cod_data_source_block           TMA1
_cod_original_cell_volume        5941.9(3)
_cod_database_code               1564485
_shelx_res_checksum              28286
_shelx_hkl_checksum              61093