INSIGHTS into the structures adopted by titanocalix[6 and 8]arenes and their use in the ring opening polymerization of cyclic esters.
Santoro, Orlando; Elsegood, Mark R. J.; Bedwell, Elizabeth V.; Pryce, Jake A.; Redshaw, Carl; Dalton transactions (Cambridge, England : 2003) 49 (2020) 11978–11996; doi:10.1039/d0dt02130j

data_7705093
_publ_section_title
;
 INSIGHTS into the structures adopted by titanocalix[6 and 8]arenes and
 their use in the ring opening polymerization of cyclic esters.
;
_journal_issue                   34
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11978
_journal_page_last               11996
_journal_paper_doi               10.1039/d0dt02130j
_journal_volume                  49
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C92 H110 Cl4 N2 O10 Ti4, 1.5(C2 H3 N)'
_chemical_formula_sum            'C95 H114.5 Cl4 N3.5 O10 Ti4'
_chemical_formula_weight         1798.79
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2020-07-08 deposited with the CCDC.	2020-08-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.7623(3)
_cell_length_b                   19.3331(3)
_cell_length_c                   26.9512(3)
_cell_measurement_reflns_used    33046
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      69.9290
_cell_measurement_theta_min      2.8520
_cell_volume                     9776.1(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'hybrid pixel detector'
_diffrn_detector_area_resol_mean 10
_diffrn_detector_type            'Rigaku, HyPix 6000'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RCD3): quarter-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_collimation    'Varimax focusing mirrors'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0486
_diffrn_reflns_av_unetI/netI     0.0356
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            94785
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.243
_diffrn_reflns_theta_min         3.279
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku 007 HF'
_exptl_absorpt_coefficient_mu    4.125
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.724
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_diffrn    1.222
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3780
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile'
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.935
_refine_diff_density_min         -0.477
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details
; 
 Flack x determined using 5884 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.000(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1175
_refine_ls_number_reflns         17801
_refine_ls_number_restraints     546
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0763
_refine_ls_R_factor_gt           0.0632
_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^)+(0.1117P)^2^+11.1740P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1690
_refine_ls_wR_factor_ref         0.1803
_reflns_Friedel_coverage         0.836
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.991
_reflns_number_gt                15039
_reflns_number_total             17801
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02130j2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7705091--7705102.cif.'
_cod_original_formula_sum        'C95 H114.50 Cl4 N3.50 O10 Ti4'
_cod_database_code               7705093
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.683
_shelx_estimated_absorpt_t_max   0.922
_shelx_res_checksum              95709