Mobility of hydrated alkali metal ions in metallosupramolecular ionic crystals
Yoshinari, Nobuto; Yamashita, Satoshi; Fukuda, Yosuke; Nakazawa, Yasuhiro; Konno, Takumi; Chemical Science  (2019) –; doi:10.1039/C8SC04204G

data_1550127
_publ_section_title
;
 Mobility of hydrated alkali metal ions in metallosupramolecular ionic
 crystals
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C8SC04204G
_journal_year                    2019
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C36 H60 N12 Na O31 Rh4 S12 Zn4, 48(O)'
_chemical_formula_sum            'C36 H60 N12 Na O79 Rh4 S12 Zn4'
_chemical_formula_weight         3005.79
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      cubic
_space_group_IT_number           198
_space_group_name_Hall           'P 2ac 2ab 3'
_space_group_name_H-M_alt        'P 21 3'
_symmetry_space_group_name_Hall  'P 2ac 2ab 3'
_symmetry_space_group_name_H-M   'P 21 3'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2017-10-10 deposited with the CCDC.
2018-10-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.574(7)
_cell_length_b                   23.574(7)
_cell_length_c                   23.574(7)
_cell_measurement_reflns_used    33353
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.01
_cell_measurement_theta_min      0.85
_cell_volume                     13101(7)
_computing_cell_refinement       'RAPID-AUTO (Rigaku Corporation)'
_computing_data_collection       'RAPID-AUTO (Rigaku Corporation)'
_computing_data_reduction        'RAPID-AUTO (Rigaku Corporation)'
_computing_molecular_graphics
'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)'
_computing_publication_material
'Yadokari-XG 2009 (Wakita, Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 14.69
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Rigaku Mercury2CCD detector'
_diffrn_measurement_method       /w
_diffrn_radiation_monochromator  Si(311)
_diffrn_radiation_source         'SPring-8 BL02B1 bending magnet'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7009
_diffrn_reflns_av_R_equivalents  0.2080
_diffrn_reflns_av_unetI/netI     0.1167
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            42555
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.869
_diffrn_reflns_theta_max         27.021
_diffrn_reflns_theta_min         1.475
_exptl_absorpt_coefficient_mu    1.434
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.1407
_exptl_absorpt_correction_type   multi-scans
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_description       block
_exptl_crystal_F_000             5980
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.896
_refine_diff_density_min         -1.058
_refine_diff_density_rms         0.190
_refine_ls_abs_structure_details
;
 Flack x determined using 2927 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.09(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     366
_refine_ls_number_reflns         10000
_refine_ls_number_restraints     90
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.1254
_refine_ls_R_factor_gt           0.1054
_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^)+(0.1512P)^2^+74.9188P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2571
_refine_ls_wR_factor_ref         0.2820
_reflns_Friedel_coverage         0.865
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                8103
_reflns_number_total             10000
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc04204g2.cif
_cod_data_source_block           Na6-1
_cod_original_cell_volume        13102(11)
_cod_database_code               1550127
_shelx_estimated_absorpt_t_min   0.870
_shelx_estimated_absorpt_t_max   0.870
_shelxl_version_number           2014-3
_shelx_res_checksum              98106