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_1557163
_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         'C47 H58 Cl N O4 Ti, C2 H3 N'
_chemical_formula_sum            'C49 H61 Cl N2 O4 Ti'
_chemical_formula_weight         825.34
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2019-09-19 deposited with the CCDC.	2020-01-27 downloaded from the CCDC.
;
_cell_angle_alpha                95.2564(9)
_cell_angle_beta                 105.3553(9)
_cell_angle_gamma                90.2869(9)
_cell_formula_units_Z            4
_cell_length_a                   12.14575(13)
_cell_length_b                   18.0271(2)
_cell_length_c                   21.0909(2)
_cell_measurement_reflns_used    31277
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.3030
_cell_measurement_theta_min      7.2830
_cell_volume                     4432.27(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_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                 'CCD plate'
_diffrn_detector_area_resol_mean 10
_diffrn_detector_type            'Rigaku, HyPix 6000'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'XtaLAB AFC11 (RCD3): quarter-chi single'
_diffrn_measurement_device_type
;  
Rigaku 007HF equipped with an AFC11 goniometer and HyPix 6000 detector. 
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_monochromator  'Varimax focusing mirrors'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0539
_diffrn_reflns_av_unetI/netI     0.0159
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            68296
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.271
_diffrn_reflns_theta_min         3.445
_diffrn_source                   'Rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    2.540
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.929
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.34b (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1760
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile'
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.130
_refine_diff_density_max         0.524
_refine_diff_density_min         -0.507
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1058
_refine_ls_number_reflns         31744
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0386
_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^)+(0.0748P)^2^+0.5665P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1092
_refine_ls_wR_factor_ref         0.1107
_reflns_Friedel_coverage         0.000
_reflns_number_gt                29425
_reflns_number_total             31744
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 179.9788\% 
 around [0.91 -0.01 -0.42] (reciprocal) or [1.00 -0.00 -0.00] (direct)
;
_cod_data_source_file            c9cy02571e2.cif
_cod_data_source_block           5
_cod_depositor_comments
;Adding full bibliography for 1557155--1557164.cif.

 Adding full bibliography for 1557155--1557164.cif.
;
_cod_database_code               1557163
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.547
_shelx_estimated_absorpt_t_max   0.734
_shelx_res_checksum              61617