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_7226356
_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            'C73 H67 Na3 O26'
_chemical_formula_weight         1429.24
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_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
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.174(4)
_cell_length_b                   18.194(5)
_cell_length_c                   26.052(6)
_cell_measurement_reflns_used    48173
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.60
_cell_measurement_theta_min      1.56
_cell_volume                     6718(3)
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.952
_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  0.1126
_diffrn_reflns_av_unetI/netI     0.1235
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            48173
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.930
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.600
_diffrn_reflns_theta_min         1.563
_exptl_absorpt_coefficient_mu    0.124
_exptl_absorpt_correction_T_max  0.993
_exptl_absorpt_correction_T_min  0.895
_exptl_absorpt_process_details
'Blessing, R. H. (1995) Acta Cryst., A51, 33-38'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2984
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.377
_refine_diff_density_min         -0.643
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details
;
 Flack x determined using 2016 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.3(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     909
_refine_ls_number_reflns         13078
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.1782
_refine_ls_R_factor_gt           0.0677
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1021P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1638
_refine_ls_wR_factor_ref         0.2110
_reflns_Friedel_coverage         0.786
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.905
_reflns_number_gt                5959
_reflns_number_total             13078
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce01387b2.cif
_cod_data_source_block           free_calix4tube_1
_cod_depositor_comments
'Adding full bibliography for 7226356--7226359.cif.'
_cod_database_code               7226356
_shelxl_version_number           2014-3
_shelx_res_checksum              47850