Charge "mis-matched" hydrogen bonded frameworks for cation exchange and dye sorption.
Muang-Non, Phonlakrit; Markwell-Heys, Adrian W; Doonan, Christian J.; White, Nicholas G.; Chemical communications (Cambridge, England) 59 (2023) 4059–4062; doi:10.1039/d3cc00553d

data_7131433
_publ_section_title
;
 Charge "mis-matched" hydrogen bonded frameworks for cation exchange and
 dye sorption.
;
_journal_issue                   27
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              4059
_journal_page_last               4062
_journal_paper_doi               10.1039/d3cc00553d
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         'C28 H16 B O8, 2(C14 H16 N4), 10(H2 O), H4 N'
_chemical_formula_sum            'C56 H72 B N9 O18'
_chemical_formula_weight         1170.04
_space_group_crystal_system      tetragonal
_space_group_IT_number           85
_space_group_name_Hall           '-P 4a'
_space_group_name_H-M_alt        'P 4/n :2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2023-01-12
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-03-06 deposited with the CCDC.	2023-03-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.6061(8)
_cell_length_b                   19.6061(8)
_cell_length_c                   15.0982(9)
_cell_measurement_reflns_used    1116
_cell_measurement_temperature    150
_cell_measurement_theta_max      72.8770
_cell_measurement_theta_min      4.4730
_cell_volume                     5803.7(5)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1297
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     32.00  59.00   1.00   20.00    --   36.34  57.00-120.00   27
  2  \w     31.00  90.00   1.00   20.00    --   36.34-125.00   0.00   59
  3  \w     67.00  94.00   1.00   20.00    --   36.34  57.00-120.00   27
  4  \w     20.00 101.00   1.00   20.00    --   36.34  57.00 -60.00   81
  5  \w     46.00 109.00   1.00   80.00    --  109.99-111.00  60.00   63
  6  \w    104.00 178.00   1.00   80.00    --  109.99 111.00-150.00   74
  7  \w    104.00 167.00   1.00   80.00    --  109.99 111.00-180.00   63
  8  \w     89.00 114.00   1.00   80.00    --  109.99  15.00 -30.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0563219000
_diffrn_orient_matrix_UB_12      -0.0368353000
_diffrn_orient_matrix_UB_13      -0.0527152000
_diffrn_orient_matrix_UB_21      -0.0276274000
_diffrn_orient_matrix_UB_22      -0.0313878000
_diffrn_orient_matrix_UB_23      0.0864538000
_diffrn_orient_matrix_UB_31      -0.0474339000
_diffrn_orient_matrix_UB_32      0.0618585000
_diffrn_orient_matrix_UB_33      0.0122538000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0592
_diffrn_reflns_av_unetI/netI     0.0994
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            10575
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.349
_diffrn_reflns_theta_min         3.695
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.838
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52236
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_description       needle
_exptl_crystal_F_000             2480
_exptl_crystal_recrystallization_method
'Crystallised using diphenylbisamidinium.2Cl with TBA5.tetraboratecarboxylate in 50% EtOH. Final concentration = 2 mM. The crystal obtained was incubated in 1 M NH4Cl at 1 mg/mL.'
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.679
_refine_diff_density_min         -0.426
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     473
_refine_ls_number_reflns         5603
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.1526
_refine_ls_R_factor_gt           0.0878
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0797P)^2^+12.9580P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1973
_refine_ls_wR_factor_ref         0.2460
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3237
_reflns_number_total             5603
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc00553d2.cif
_cod_data_source_block           nh4_2_b
_cod_depositor_comments
'Adding full bibliography for 7131429--7131437.cif.'
_cod_original_cell_volume        5803.7(6)
_cod_original_sg_symbol_H-M      'P 4/n'
_cod_database_code               7131433
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.992
_shelx_estimated_absorpt_t_min   0.661
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 H10C-N100
 0.88 with sigma of 0.01
 N110-H11C
 0.88 with sigma of 0.02
 H11D-N110
 0.87 with sigma of 0.02
 H10D-N100
 0.87 with sigma of 0.02
3. Others
 Fixed Sof: H10C(0.75) H11C(0.75)
4.a Free rotating group:
 O110(H11A,H11B), O120(H12A,H12B), O100(H10A,H10B), O130(H13A,H13B)
4.b Aromatic/amide H refined with riding coordinates:
 C13(H13)
4.c X=CH2 refined with riding coordinates:
 N4(H4A,H4B)
;
_shelx_res_checksum              11359
_shelx_hkl_checksum              42563
_olex2_submission_special_instructions 'No special instructions were received'