Selective isolation of Keggin ions using self-assembled superanion capsules †
Drljaca, Alexander; Hardie, Michaele J.; Raston, Colin L.; Journal of the Chemical Society, Dalton Transactions  (1999) 3639–; doi:10.1039/a905436g

data_7027672
_publ_section_title
;
 Selective isolation of Keggin ions using self-assembled superanion
 capsules&#x200A;&#x2020;
;
_journal_issue                   20
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3639
_journal_paper_doi               10.1039/a905436g
_journal_year                    1999
_chemical_formula_sum            'C124 H325 Al26 Na O210 S16'
_chemical_formula_weight         6414.28
_chemical_name_common
;
[Al13O4(OH)36(H2O)12][(sodium-(18-
crown-6)-dihydrate).
bis(p-sulfonatocalix[4]arene)]0.5[p-sulfonatocalix[4]arene](H20)29 
;
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                117.4770(10)
_cell_angle_beta                 109.0250(10)
_cell_angle_gamma                91.3820(10)
_cell_formula_units_Z            1
_cell_length_a                   17.5361(5)
_cell_length_b                   20.2736(6)
_cell_length_c                   21.7395(6)
_cell_measurement_temperature    123(1)
_cell_volume                     6340.5(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(1)
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  CCD
_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  0.055
_diffrn_reflns_av_sigmaI/netI    0.0774
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            44510
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.96
_exptl_absorpt_coefficient_mu    0.36
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.68
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3354
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.487
_refine_diff_density_min         -1.340
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1735
_refine_ls_number_reflns         21506
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.1415
_refine_ls_R_factor_gt           0.0928
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1169P)^2^+57.8316P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2293
_refine_ls_wR_factor_ref         0.2721
_reflns_number_gt                14135
_reflns_number_total             21506
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            905436Gsup1.cif
_cod_data_source_block           1
_cod_depositor_comments
;

2023-11-21
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_weight         3207.14
_cod_original_formula_units_Z            2
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C62 H162.5 Al13 Na0.50 O105 S8'
_cod_database_code               7027672