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_7226357
_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            'C72 H61.5 Na3 O24.25'
_chemical_formula_weight         1383.68
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2016-08-19 deposited with the CCDC.
2016-08-24 downloaded from the CCDC.
;
_cell_angle_alpha                79.663(11)
_cell_angle_beta                 86.268(11)
_cell_angle_gamma                82.469(12)
_cell_formula_units_Z            4
_cell_length_a                   14.840(2)
_cell_length_b                   17.911(3)
_cell_length_c                   31.010(5)
_cell_measurement_reflns_used    45357
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.39
_cell_measurement_theta_min      1.39
_cell_volume                     8031(2)
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.939
_diffrn_measured_fraction_theta_max 0.924
_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  0.1181
_diffrn_reflns_av_unetI/netI     0.3544
_diffrn_reflns_Laue_measured_fraction_full 0.939
_diffrn_reflns_Laue_measured_fraction_max 0.924
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            45357
_diffrn_reflns_point_group_measured_fraction_full 0.939
_diffrn_reflns_point_group_measured_fraction_max 0.924
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.391
_diffrn_reflns_theta_min         1.385
_exptl_absorpt_coefficient_mu    0.100
_exptl_absorpt_correction_T_max  0.994
_exptl_absorpt_correction_T_min  0.903
_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    1.144
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2882
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_platon_squeeze_details
;
The unit cell contains an unknown number of solvent molecules (most probably water and methanol) which have been treated as a diffuse contribution to the overall scattering without specific atom positions by SQUEEZE/PLATON. 
;
_refine_diff_density_max         0.498
_refine_diff_density_min         -0.872
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.878
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1735
_refine_ls_number_reflns         27303
_refine_ls_number_restraints     1992
_refine_ls_restrained_S_all      0.931
_refine_ls_R_factor_all          0.3084
_refine_ls_R_factor_gt           0.1435
_refine_ls_shift/su_max          0.024
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1511P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3559
_refine_ls_wR_factor_ref         0.4050
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5220
_reflns_number_total             27303
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce01387b2.cif
_cod_data_source_block           free_calix4tube_2
_cod_depositor_comments
;
Adding full bibliography for 7226356--7226359.cif.

2023-11-23
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C288 H246 Na12 O97'
_cod_original_formula_weight         5534.74
_cod_original_formula_units_Z            1
_cod_original_cell_volume        8032(2)
_cod_database_code               7226357
_shelxl_version_number           2014-3
_shelx_res_checksum              23801