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_7706773
_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
;
C76 H99 N O10 Ti2, 3(C2 H3 N) [+ 0.5 MeCN]
;
_chemical_formula_sum            'C82 H108 N4 O10 Ti2'
_chemical_formula_weight         1405.52
_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-2016/6
_audit_update_record
;
2021-02-24 deposited with the CCDC.	2021-03-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.2370(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.0347(2)
_cell_length_b                   28.3198(4)
_cell_length_c                   24.5367(3)
_cell_measurement_reflns_used    30751
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.028
_cell_measurement_theta_min      3.177
_cell_volume                     8140.4(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_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      100(2)
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'XtaLAB AFC11 (RCD3): quarter-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0521
_diffrn_reflns_av_unetI/netI     0.0292
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            75678
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        66.600
_diffrn_reflns_theta_max         66.600
_diffrn_reflns_theta_min         2.420
_diffrn_source                   'Rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    2.112
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.69725
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.147
_exptl_crystal_description       plate
_exptl_crystal_F_000             3008
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.040
_platon_squeeze_details
;
Two sensible pockets each capable of containing 22e.  CH3CN is 22e electrons. 
As Z = 4 this equates to 0.5 MeCN per Ti2 complex. 
;
_refine_diff_density_max         1.961
_refine_diff_density_min         -0.795
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.675
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     870
_refine_ls_number_reflns         14383
_refine_ls_number_restraints     58
_refine_ls_restrained_S_all      1.677
_refine_ls_R_factor_all          0.1260
_refine_ls_R_factor_gt           0.1169
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3558
_refine_ls_wR_factor_ref         0.3681
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12259
_reflns_number_total             14383
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00189b2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7706773--7706779.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7706773
_platon_squeeze_void_probe_radius 1.20
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.677
_shelx_estimated_absorpt_t_max   0.920
_shelx_res_checksum              93073
_shelx_hkl_checksum              78419
_shelx_fab_checksum              71971