Lower rim dimerization of a calixarene through the encapsulation of sodium ions
Martins, Felipe Terra; da Silva, Cleiton Moreira; Vasconcelos, Géssica Adriana; Gontijo Vaz, Boniek; Vieira, Tarcisio da Silva; Queiroz Júnior, Luiz Henrique Keng; de Fátima, Ângelo; CrystEngComm 18 (2016) 6987–; doi:10.1039/C6CE01387B

data_7226358
_publ_section_title
;
 Lower rim dimerization of a calixarene through the encapsulation of
 sodium ions
;
_journal_issue                   37
_journal_name_full               CrystEngComm
_journal_page_first              6987
_journal_paper_doi               10.1039/C6CE01387B
_journal_volume                  18
_journal_year                    2016
_chemical_formula_sum            'C76 H72 Na4 O26 S2'
_chemical_formula_weight         1557.42
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           106
_space_group_name_Hall           'P 4c -2ab'
_space_group_name_H-M_alt        'P 42 b c'
_symmetry_space_group_name_Hall  'P 4c -2ab'
_symmetry_space_group_name_H-M   'P 42 b c'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2016-07-19 deposited with the CCDC.
2016-08-24 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.041(4)
_cell_length_b                   21.041(4)
_cell_length_c                   16.456(3)
_cell_measurement_reflns_used    41778
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.13
_cell_measurement_theta_min      1.94
_cell_volume                     7285(2)
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  KappaCCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2484
_diffrn_reflns_av_unetI/netI     0.1843
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            41778
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.135
_diffrn_reflns_theta_min         1.936
_exptl_absorpt_coefficient_mu    0.181
_exptl_absorpt_correction_T_max  0.991
_exptl_absorpt_correction_T_min  0.913
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Blessing, R. H. (1995) Acta Cryst., A51, 33-38'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3248
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.258
_refine_diff_density_min         -0.311
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details
;
 Flack x determined using 959 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.23(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.973
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     490
_refine_ls_number_reflns         6333
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.973
_refine_ls_R_factor_all          0.1946
_refine_ls_R_factor_gt           0.0689
_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^)+(0.0581P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1234
_refine_ls_wR_factor_ref         0.1666
_reflns_Friedel_coverage         0.880
_reflns_Friedel_fraction_full    0.957
_reflns_Friedel_fraction_max     0.946
_reflns_number_gt                2947
_reflns_number_total             6333
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce01387b2.cif
_cod_data_source_block           pol_calix4tube_3
_cod_depositor_comments
'Adding full bibliography for 7226356--7226359.cif.'
_cod_original_cell_volume        7286(3)
_cod_database_code               7226358
_shelxl_version_number           2014-3
_shelx_res_checksum              87430