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_7705099
_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         'C92 H110 I4 N2 O10 Ti4, 7.25(C H2 Cl2)'
_chemical_formula_sum            'C99.25 H124.5 Cl14.5 I4 N2 O10 Ti4'
_chemical_formula_weight         2718.73
_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
_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                 103.0731(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.2721(4)
_cell_length_b                   9.52188(14)
_cell_length_c                   43.6988(6)
_cell_measurement_reflns_used    40748
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.05
_cell_measurement_theta_min      3.07
_cell_volume                     11864.3(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46b (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46b (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46b (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_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       'four-circle diffractometer'
_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_collimation    0.3
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1519
_diffrn_reflns_av_unetI/netI     0.0744
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            103662
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.245
_diffrn_reflns_theta_min         2.292
_diffrn_source                   'Rotating anode'
_exptl_absorpt_coefficient_mu    13.798
_exptl_absorpt_correction_T_max  0.708
_exptl_absorpt_correction_T_min  0.241
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.40.47a (Rigaku Oxford Diffraction, 2019) 
Numerical absorption correction based on gaussian integration over 
   a multifaceted crystal model 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5442
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane'
_exptl_crystal_size_max          0.165
_exptl_crystal_size_mid          0.044
_exptl_crystal_size_min          0.033
_refine_diff_density_max         1.558
_refine_diff_density_min         -1.886
_refine_diff_density_rms         0.162
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1290
_refine_ls_number_reflns         21509
_refine_ls_number_restraints     669
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1149
_refine_ls_R_factor_gt           0.0986
_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^)+(0.1349P)^2^+99.1414P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2616
_refine_ls_wR_factor_ref         0.2746
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16795
_reflns_number_total             21509
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02130j2.cif
_cod_data_source_block           11
_cod_depositor_comments
'Adding full bibliography for 7705091--7705102.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C99.25 H124.50 Cl14.50 I4 N2 O10 Ti4'
_cod_database_code               7705099
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.209
_shelx_estimated_absorpt_t_max   0.659
_shelx_res_checksum              18899
_shelx_fab_checksum              45013