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_7242419
_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         'C94 H122 Li6 O10, C6 H14'
_chemical_formula_sum            'C100 H136 Li6 O10'
_chemical_formula_weight         1539.72
_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   mixed
_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                102.6019(11)
_cell_angle_beta                 91.2345(12)
_cell_angle_gamma                93.5123(12)
_cell_formula_units_Z            1
_cell_length_a                   10.5688(9)
_cell_length_b                   13.1163(11)
_cell_length_c                   17.2651(14)
_cell_measurement_reflns_used    6645
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      33.13
_cell_measurement_theta_min      2.92
_cell_volume                     2329.8(3)
_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 0.995
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker APEX 2 CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.0613
_diffrn_reflns_av_unetI/netI     0.0879
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            34077
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        27.706
_diffrn_reflns_theta_max         33.619
_diffrn_reflns_theta_min         2.914
_diffrn_source                   'ALS Station 11.3.1'
_exptl_absorpt_coefficient_mu    0.080
_exptl_absorpt_correction_T_max  0.993
_exptl_absorpt_correction_T_min  0.990
_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    1.097
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             834
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: hexane'
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.659
_refine_diff_density_min         -0.363
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     561
_refine_ls_number_reflns         13962
_refine_ls_number_restraints     77
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0995
_refine_ls_R_factor_gt           0.0717
_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^)+(0.1157P)^2^+0.3793P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2039
_refine_ls_wR_factor_ref         0.2283
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9552
_reflns_number_total             13962
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ra00175b2.cif
_cod_data_source_block           9
_cod_database_code               7242419
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.988
_shelx_estimated_absorpt_t_max   0.992
_shelx_res_checksum              31034