Titanium complexes bearing oxa- and azacalix[4, 6]arenes: structural studies and use in the ring opening homo-/co-polymerization of cyclic esters.
Xing, Tian; Prior, Timothy J.; Chen, Kai; Redshaw, Carl; Dalton transactions (Cambridge, England : 2003) 50 (2021) 4396–4407; doi:10.1039/d1dt00189b

data_7706774
_publ_section_title
;
 Titanium complexes bearing oxa- and azacalix[4, 6]arenes: structural
 studies and use in the ring opening homo-/co-polymerization of cyclic
 esters.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4396
_journal_page_last               4407
_journal_paper_doi               10.1039/d1dt00189b
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety
;   
 C54 H59 F14 N3 O6 Ti4 [+ solvent]
;
_chemical_formula_sum            'C54 H59 F14 N3 O6 Ti4'
_chemical_formula_weight         1303.64
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-02-24 deposited with the CCDC.	2021-03-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.3810(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.1213(2)
_cell_length_b                   22.8130(2)
_cell_length_c                   17.0185(2)
_cell_measurement_reflns_used    28774
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.168
_cell_measurement_theta_min      3.388
_cell_volume                     6113.42(12)
_computing_cell_refinement       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2; Mercury'
_computing_publication_material  'CIFTAB, WinGX'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'XtaLAB AFC11 (RCD3): quarter-chi single'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0415
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            55456
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.413
_diffrn_reflns_theta_min         3.938
_diffrn_source                   'Rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    5.091
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.6143
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.416
_exptl_crystal_description       block
_exptl_crystal_F_000             2664
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.050
_platon_squeeze_details
;
140e per cell equates to about 6 MeCN per cell. 
Thus 1.5 per formula unit.
;
_refine_diff_density_max         1.499
_refine_diff_density_min         -0.518
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     741
_refine_ls_number_reflns         11386
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0705
_refine_ls_R_factor_gt           0.0637
_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^)+(0.1262P)^2^+4.0039P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1701
_refine_ls_wR_factor_ref         0.1784
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9819
_reflns_number_total             11386
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00189b2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7706773--7706779.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7706774
_shelx_shelxl_version_number     2018/3
_platon_squeeze_void_probe_radius 1.20
_shelx_estimated_absorpt_t_min   0.516
_shelx_estimated_absorpt_t_max   0.785
_shelx_res_checksum              48614
_shelx_hkl_checksum              26418
_shelx_fab_checksum              68013