Synthesis of titanium-oxo macrocyles and their catalytic properties for oxidative desulfurization.
Lv, Hai-Ting; Cui, Ying; Zou, Guo-Dong; Li, Na; Yang, Pei; Fan, Yang; Dalton transactions (Cambridge, England : 2003) 48 (2019) 14044–14048; doi:10.1039/c9dt03057c

data_7701598
_publ_section_title
;
 Synthesis of titanium-oxo macrocyles and their catalytic properties for
 oxidative desulfurization.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14044
_journal_page_last               14048
_journal_paper_doi               10.1039/c9dt03057c
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C204 H456 N0 O172 Ti32'
_chemical_formula_sum            'C204 H456 N0 O172 Ti32'
_chemical_formula_weight         7194.46
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2019-08-23 deposited with the CCDC.	2019-08-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 119.823(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   51.758(4)
_cell_length_b                   14.9948(11)
_cell_length_c                   47.346(3)
_cell_measurement_reflns_used    9976
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.27
_cell_measurement_theta_min      2.39
_cell_volume                     31879(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0851
_diffrn_reflns_av_unetI/netI     0.0761
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       63
_diffrn_reflns_limit_h_min       -63
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       58
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            150653
_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         26.000
_diffrn_reflns_theta_min         2.221
_exptl_absorpt_coefficient_mu    0.850
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5172
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 The following wavelength and cell were deduced by SADABS from the
 direction cosines etc. They are given here for emergency use only:
 CELL 0.71112   51.829   15.014   47.377   90.059  119.736   90.052
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_description       block
_exptl_crystal_F_000             15040
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.775
_refine_diff_density_min         -1.069
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1886
_refine_ls_number_reflns         31311
_refine_ls_number_restraints     696
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.1548
_refine_ls_R_factor_gt           0.1064
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1474P)^2^+461.5608P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2837
_refine_ls_wR_factor_ref         0.3229
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19415
_reflns_number_total             31311
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03057c2.cif
_cod_data_source_block           Ti32DMBTA
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7701598
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              25904
_shelx_fab_checksum              17564