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_1557156
_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_absolute_configuration ad
_chemical_formula_moiety         'C30 H44 Cl2 O2 Ti'
_chemical_formula_sum            'C30 H44 Cl2 O2 Ti'
_chemical_formula_weight         555.45
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-11-29 deposited with the CCDC.	2020-01-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.131(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.0509(2)
_cell_length_b                   9.69430(18)
_cell_length_c                   14.8668(3)
_cell_measurement_reflns_used    28467
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.02
_cell_measurement_theta_min      2.05
_cell_volume                     1513.61(5)
_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    '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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
;
Rigaku FRE+ diffractometer equipped with VHF Varimax confocal 
mirrors and an AFC12 goniometer and HyPix 6000HE 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  0.0225
_diffrn_reflns_av_unetI/netI     0.0166
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            34809
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.482
_diffrn_reflns_theta_min         2.548
_diffrn_source                   'Rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    0.483
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.432
_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            orange
_exptl_crystal_density_diffrn    1.219
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             592
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: hexane'
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.275
_refine_diff_density_min         -0.402
_refine_diff_density_rms         0.038
_refine_ls_abs_structure_details
; 
 Classical Flack method preferred over Parsons because s.u. lower. 
;
_refine_ls_abs_structure_Flack   0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     329
_refine_ls_number_reflns         6818
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0297
_refine_ls_R_factor_gt           0.0293
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0529P)^2^+0.3564P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0762
_refine_ls_wR_factor_ref         0.0765
_reflns_Friedel_coverage         0.854
_reflns_Friedel_fraction_full    0.975
_reflns_Friedel_fraction_max     0.962
_reflns_number_gt                6713
_reflns_number_total             6818
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cy02571e2.cif
_cod_data_source_block           12
_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'
_cod_database_code               1557156
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.918
_shelx_estimated_absorpt_t_max   0.981
_shelx_res_checksum              21441