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_7705097
_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_formula_moiety         'C98 H123 Br6 N5 O9 Ti3, 7.5(C2 H3 N)'
_chemical_formula_sum            'C113 H145.5 Br6 N12.5 O9 Ti3'
_chemical_formula_weight         2446.07
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-07-08 deposited with the CCDC.	2020-08-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.7763(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.5584(2)
_cell_length_b                   26.9199(3)
_cell_length_c                   21.6443(2)
_cell_measurement_reflns_used    45430
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.33
_cell_measurement_theta_min      2.67
_cell_volume                     12497.5(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-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'hybrid pixel detector'
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details 'Rigaku, AFC11 quarter \c goniometer'
_diffrn_measurement_device_type
; 
Rigaku 007HF equipped with Varimax confocal mirrors and an AFC11
goniometer and HyPix 6000 detector 
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0542
_diffrn_reflns_av_unetI/netI     0.0384
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            126455
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.244
_diffrn_reflns_theta_min         2.628
_diffrn_source                   'Rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    4.278
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53911
_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 red'
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             5036
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile'
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.010
_refine_diff_density_max         2.764
_refine_diff_density_min         -1.424
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1293
_refine_ls_number_reflns         22797
_refine_ls_number_restraints     363
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1066
_refine_ls_R_factor_gt           0.0907
_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^)+(0.1934P)^2^+23.8835P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2771
_refine_ls_wR_factor_ref         0.2932
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17330
_reflns_number_total             22797
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02130j2.cif
_cod_data_source_block           7
_cod_depositor_comments
'Adding full bibliography for 7705091--7705102.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C113 H145.50 Br6 N12.50 O9 Ti3'
_cod_database_code               7705097
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.497
_shelx_estimated_absorpt_t_max   0.958
_shelx_res_checksum              37107
_shelx_fab_checksum              39528