Lithium calix[4]arenes: structural studies and use in the ring opening polymerization of cyclic esters
Santoro, Orlando; Elsegood, Mark R. J.; Teat, Simon J.; Yamato, Takehiko; Redshaw, Carl; RSC Advances 11 (2021) 11304–11317; doi:10.1039/D1RA00175B

data_7242425
_publ_section_title
;
 Lithium calix[4]arenes: structural studies and use in the ring opening
 polymerization of cyclic esters
;
_journal_issue                   19
_journal_name_full               'RSC Advances'
_journal_page_first              11304
_journal_page_last               11317
_journal_paper_doi               10.1039/D1RA00175B
_journal_volume                  11
_journal_year                    2021
_chemical_formula_moiety         'C96 H120 Li8 O12 S8, 5(C4 H8 O)'
_chemical_formula_sum            'C116 H160 Li8 O17 S8'
_chemical_formula_weight         2138.43
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-03-03 deposited with the CCDC.	2021-03-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.218(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.323(13)
_cell_length_b                   17.655(9)
_cell_length_c                   26.894(14)
_cell_measurement_reflns_used    439
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      15.01
_cell_measurement_theta_min      2.31
_cell_volume                     11602(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX 2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX 2 CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2304
_diffrn_reflns_av_unetI/netI     0.2227
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            35870
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        22.500
_diffrn_reflns_theta_max         22.500
_diffrn_reflns_theta_min         1.667
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.216
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_correction_T_min  0.950
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2008/1, Sheldrick, G.M., (2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.224
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4576
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: tetrahydrofuran'
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.406
_refine_diff_density_min         -0.320
_refine_diff_density_rms         0.076
_refine_ls_extinction_coef       0.00046(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   0.929
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     748
_refine_ls_number_reflns         7584
_refine_ls_number_restraints     689
_refine_ls_restrained_S_all      0.902
_refine_ls_R_factor_all          0.2183
_refine_ls_R_factor_gt           0.0982
_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^)+(0.1183P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2165
_refine_ls_wR_factor_ref         0.2721
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2884
_reflns_number_total             7584
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ra00175b2.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_database_code               7242425
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.950
_shelx_estimated_absorpt_t_max   0.981
_shelx_res_checksum              87410