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_7226359
_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            'C78 H74 N2 Na4 O26'
_chemical_formula_weight         1547.35
_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
;
2016-08-10 deposited with the CCDC.
2016-08-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.0771(7)
_cell_length_b                   21.0771(7)
_cell_length_c                   16.6303(5)
_cell_measurement_reflns_used    24382
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.40
_cell_measurement_theta_min      2.29
_cell_volume                     7387.9(4)
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.1284
_diffrn_reflns_av_unetI/netI     0.1274
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            24383
_diffrn_reflns_point_group_measured_fraction_full 0.868
_diffrn_reflns_point_group_measured_fraction_max 0.862
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.404
_diffrn_reflns_theta_min         2.288
_exptl_absorpt_coefficient_mu    0.124
_exptl_absorpt_correction_T_max  0.991
_exptl_absorpt_correction_T_min  0.933
_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    1.391
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3232
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.325
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.101
_refine_ls_abs_structure_details
;
 Flack x determined using 858 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.6(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     497
_refine_ls_number_reflns         5868
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.1725
_refine_ls_R_factor_gt           0.0662
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0975P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1548
_refine_ls_wR_factor_ref         0.2141
_reflns_Friedel_coverage         0.664
_reflns_Friedel_fraction_full    0.725
_reflns_Friedel_fraction_max     0.716
_reflns_number_gt                2790
_reflns_number_total             5868
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce01387b2.cif
_cod_data_source_block           pol_calix4tube_4
_cod_depositor_comments
'Adding full bibliography for 7226356--7226359.cif.'
_cod_original_cell_volume        7387.9(5)
_cod_database_code               7226359
_shelxl_version_number           2014-3
_shelx_res_checksum              15885