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_7701597
_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         'C160 H408 N0 O188 Ti32'
_chemical_formula_sum            'C160 H408 N0 O188 Ti32'
_chemical_formula_weight         6873.64
_space_group_crystal_system      tetragonal
_space_group_IT_number           85
_space_group_name_Hall           '-P 4a'
_space_group_name_H-M_alt        'P 4/n :2'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   33.635(3)
_cell_length_b                   33.635(3)
_cell_length_c                   13.0634(12)
_cell_measurement_reflns_used    9137
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.89
_cell_measurement_theta_min      2.42
_cell_volume                     14779(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_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  0.0717
_diffrn_reflns_av_unetI/netI     0.0481
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            84405
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.316
_exptl_absorpt_coefficient_mu    0.916
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5679
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.545
_exptl_crystal_description       block
_exptl_crystal_F_000             7152
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.991
_refine_diff_density_min         -1.445
_refine_diff_density_rms         0.189
_refine_ls_extinction_coef       0.00170(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.156
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     839
_refine_ls_number_reflns         12977
_refine_ls_number_restraints     144
_refine_ls_restrained_S_all      1.154
_refine_ls_R_factor_all          0.1377
_refine_ls_R_factor_gt           0.1297
_refine_ls_shift/su_max          0.084
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0547P)^2^+429.1424P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3005
_refine_ls_wR_factor_ref         0.3048
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11687
_reflns_number_total             12977
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03057c2.cif
_cod_data_source_block           Ti32BTA
_cod_original_cell_volume        14779(3)
_cod_original_sg_symbol_H-M      'P 4/n'
_cod_database_code               7701597
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              17143
_shelx_fab_checksum              24045