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_7242422
_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_absolute_configuration unk
_chemical_formula_moiety         'C48 H66 Li2 O7, 3(C4 H8 O)'
_chemical_formula_sum            'C60 H90 Li2 O10'
_chemical_formula_weight         985.19
_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   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                90
_cell_angle_beta                 96.406(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.763(14)
_cell_length_b                   36.82(4)
_cell_length_c                   13.119(16)
_cell_measurement_reflns_used    11272
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.7
_cell_measurement_theta_min      1.9
_cell_volume                     5647(11)
_computing_cell_refinement
; 
Rigaku CrystalClear-SM Expert 2.0 r13 
;
_computing_data_collection
; 
Rigaku CrystalClear-SM Expert 2.0 r13 
;
_computing_data_reduction
; 
Rigaku CrystalClear-SM Expert 2.0 r13 
;
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'four-circle \k goniometer'
_diffrn_measurement_device_type  CrystalLogic
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_collimation    'Confocal mirrors'
_diffrn_radiation_monochromator  'double crystal silicon'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.1333
_diffrn_reflns_av_unetI/netI     0.1766
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            37790
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        22.498
_diffrn_reflns_theta_max         22.498
_diffrn_reflns_theta_min         2.393
_diffrn_source                   'DLS beamline I19'
_exptl_absorpt_coefficient_mu    0.075
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.340
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.159
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Platelet
_exptl_crystal_F_000             2144
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: tetrahydrofuran'
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.557
_refine_diff_density_min         -0.488
_refine_diff_density_rms         0.119
_refine_ls_abs_structure_details
; 
 Flack x determined using 1974 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.8(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1333
_refine_ls_number_reflns         15742
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.1922
_refine_ls_R_factor_gt           0.1497
_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^)+(0.2878P)^2^+5.8000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4003
_refine_ls_wR_factor_ref         0.4514
_reflns_Friedel_coverage         0.915
_reflns_Friedel_fraction_full    0.944
_reflns_Friedel_fraction_max     0.944
_reflns_number_gt                9255
_reflns_number_total             15742
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ra00175b2.cif
_cod_data_source_block           7
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7242422
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.995
_shelx_estimated_absorpt_t_max   0.998
_shelx_res_checksum              1458