Tetranitro- and Tetraamino- dibenzo[18]crown-6-ether Derivatives: Complexes for Alkali Metal Ions, Redox Potentials, Crystal Structures, Molecular Sorption, and Proton Conducting Behaviors.
Shimizu, Yuta; Takeda, Takashi; Hoshino, Norihisa; Akutagawa, Tomoyuki; CrystEngComm  (2022) –; doi:10.1039/D2CE00582D

data_7245115
_publ_section_title
;
 Tetranitro- and Tetraamino- dibenzo[18]crown-6-ether Derivatives:
 Complexes for Alkali Metal Ions, Redox Potentials, Crystal Structures,
 Molecular Sorption, and Proton Conducting Behaviors.
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00582D
_journal_year                    2022
_chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk'
_chemical_formula_moiety         'C40 H88 N8 Na Ne0.5 O46 S6'
_chemical_formula_sum            'C40 H88 N8 Na Ne0.5 O46 S6'
_chemical_formula_weight         1642.60
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2022-04-26 deposited with the CCDC.	2022-06-28 downloaded from the CCDC.
;
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            2
_cell_length_a                   34.7439(9)
_cell_length_b                   8.1437(2)
_cell_length_c                   23.0281(6)
_cell_measurement_reflns_used    35594
_cell_measurement_temperature    296
_cell_measurement_theta_max      68.11
_cell_measurement_theta_min      3.19
_cell_volume                     6515.7(3)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.3'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2019)'
_computing_structure_refinement  'SHELXL Version 2018/3 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT Version 2018/2 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0805
_diffrn_reflns_av_unetI/netI     0.0772
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            71878
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         68.229
_diffrn_reflns_theta_min         3.187
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.547
_exptl_absorpt_correction_T_max  0.857
_exptl_absorpt_correction_T_min  0.527
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.837
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1728.00
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.66
_refine_diff_density_min         -0.44
_refine_ls_abs_structure_details
;
 Flack x determined using 2447 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.065(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     910
_refine_ls_number_reflns         11887
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1296
_refine_ls_R_factor_gt           0.0861
_refine_ls_shift/su_max          0.547
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1512P)^2^+2.2430P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2255
_refine_ls_wR_factor_ref         0.2615
_reflns_Friedel_coverage         0.943
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                7407
_reflns_number_total             11887
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            d2ce00582d2.cif
_cod_data_source_block           210616
_cod_database_code               7245115
_shelx_res_checksum              67164
_shelx_hkl_checksum              69534