Use of titanocalix[4]arenes in the ring opening polymerization of cyclic esters
Sun, Ziyue; Zhao, Yanxia; Santoro, Orlando; Elsegood, Mark R. J.; Bedwell, Elizabeth V.; Zahra, Khadisha; Walton, Alex; Redshaw, Carl; Catalysis Science & Technology 10 (2020) 1619–1639; doi:10.1039/C9CY02571E

data_1557162
_publ_section_title
;
 Use of titanocalix[4]arenes in the ring opening polymerization of cyclic
 esters
;
_journal_issue                   6
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_page_first              1619
_journal_page_last               1639
_journal_paper_doi               10.1039/C9CY02571E
_journal_volume                  10
_journal_year                    2020
_chemical_formula_moiety         'C98 H127 Cl O9 Ti2, 7.5(C2 H3 N) '
_chemical_formula_sum            'C113 H149.5 Cl N7.5 O9 Ti2'
_chemical_formula_weight         1888.14
_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   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-09-19 deposited with the CCDC.	2020-01-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.6220(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.6007(4)
_cell_length_b                   13.18235(14)
_cell_length_c                   32.7812(5)
_cell_measurement_reflns_used    39501
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.5170
_cell_measurement_theta_min      1.5800
_cell_volume                     11122.7(3)
_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-2014/5 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details 'Rigaku, AFC12 \k goniometer'
_diffrn_measurement_device_type
; 
Rigaku FRE+ equipped with VHF Varimax confocal mirrors and an AFC12 
goniometer and HyPix 6000 detector 
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_collimation    0.2
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0519
_diffrn_reflns_av_unetI/netI     0.0383
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            167629
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         1.582
_diffrn_source                   'Rotating anode'
_exptl_absorpt_coefficient_mu    0.224
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.574
_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            red
_exptl_crystal_density_diffrn    1.128
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4052
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile'
_exptl_crystal_size_max          0.900
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.404
_refine_diff_density_min         -0.640
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1323
_refine_ls_number_reflns         25491
_refine_ls_number_restraints     617
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0944
_refine_ls_R_factor_gt           0.0754
_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^)+(0.0825P)^2^+22.0195P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1944
_refine_ls_wR_factor_ref         0.2043
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20319
_reflns_number_total             25491
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cy02571e2.cif
_cod_data_source_block           7
_cod_depositor_comments
;Adding full bibliography for 1557155--1557164.cif.

 Adding full bibliography for 1557155--1557164.cif.
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C113 H149.50 Cl N7.50 O9 Ti2'
_cod_database_code               1557162
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.824
_shelx_estimated_absorpt_t_max   0.996
_shelx_res_checksum              61308