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_7706777
_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
;
 C52 H60 Br4 N2 O9 Ti2, 2(C2 H3 N) [+ 2.5MeCN] 
;
_chemical_formula_sum            'C56 H66 Br4 N4 O9 Ti2'
_chemical_formula_weight         1354.56
_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   mixed
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2021-02-24 deposited with the CCDC.	2021-03-05 downloaded from the CCDC.
;
_cell_angle_alpha                111.546(5)
_cell_angle_beta                 94.299(6)
_cell_angle_gamma                96.876(5)
_cell_formula_units_Z            2
_cell_length_a                   12.8059(9)
_cell_length_b                   14.7294(9)
_cell_length_c                   18.6847(13)
_cell_measurement_reflns_used    18942
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.55
_cell_measurement_theta_min      1.50
_cell_volume                     3227.4(4)
_computing_cell_refinement       'Stoe X-AREA'
_computing_data_collection       'Stoe X-AREA'
_computing_data_reduction        'Stoe X-AREA'
_computing_molecular_graphics    'Olex2; Mercury'
_computing_publication_material  'CIFTAB, WinGX'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Stoe IPDS2'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0792
_diffrn_reflns_av_unetI/netI     0.1022
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            25790
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.373
_diffrn_reflns_theta_min         1.520
_diffrn_source                   'fine-fosu sealed tube'
_exptl_absorpt_coefficient_mu    2.775
_exptl_absorpt_correction_T_max  0.825
_exptl_absorpt_correction_T_min  0.625
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
Face index absorption correction within 
Stoe X-AREA (Tompa method)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_description       block
_exptl_crystal_F_000             1372
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.200
_platon_squeeze_details
;

Solvent is MeCN (22 electrons) 110 electrons in the cell
equates to 5 MeCN and hence 2.5 per asym unit. 
;
_refine_diff_density_max         0.894
_refine_diff_density_min         -0.841
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.859
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     699
_refine_ls_number_reflns         13079
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      0.859
_refine_ls_R_factor_all          0.0765
_refine_ls_R_factor_gt           0.0458
_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^)+(0.0511P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0995
_refine_ls_wR_factor_ref         0.1066
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8355
_reflns_number_total             13079
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00189b2.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 7706773--7706779.cif.'
_cod_database_code               7706777
_platon_squeeze_void_probe_radius 1.20
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.435
_shelx_estimated_absorpt_t_max   0.607
_shelx_res_checksum              26625
_shelx_hkl_checksum              33735
_shelx_fab_checksum              14956