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_7131435
_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
'2(C28 H16 B O8), 4(C14 H16 N4), H12 Mg O6, 16(H2 O)'
_chemical_formula_sum            'C112 H140 B2 Mg N16 O38'
_chemical_formula_weight         2364.33
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2023-01-09
_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            2
_cell_length_a                   19.5332(5)
_cell_length_b                   19.5332(5)
_cell_length_c                   15.1579(4)
_cell_measurement_reflns_used    1311
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      72.7180
_cell_measurement_theta_min      5.8160
_cell_volume                     5783.4(3)
_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      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1297
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.972
_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    -29.00  62.00   1.00   20.00    --   37.05 -19.00 120.00   91
  2  \w     37.00  90.00   1.00   20.00    --   37.05-125.00  60.00   53
  3  \w     43.00 128.00   1.00   80.00    --  111.00 -50.00-150.00   85
  4  \w     48.00  90.00   1.00   80.00    --  111.00 -92.00  60.00   42
  5  \w     47.00 104.00   1.00   80.00    --  111.00-111.00-150.00   57
  6  \w     42.00 100.00   1.00   80.00    --  111.00 -92.00-120.00   58
;
_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      0.0475325000
_diffrn_orient_matrix_UB_12      0.0627621000
_diffrn_orient_matrix_UB_13      -0.0049732000
_diffrn_orient_matrix_UB_21      -0.0524940000
_diffrn_orient_matrix_UB_22      0.0421431000
_diffrn_orient_matrix_UB_23      0.0531053000
_diffrn_orient_matrix_UB_31      0.0348042000
_diffrn_orient_matrix_UB_32      -0.0222514000
_diffrn_orient_matrix_UB_33      0.0865525000
_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  0.0540
_diffrn_reflns_av_unetI/netI     0.1176
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            10335
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.737
_diffrn_reflns_theta_min         3.691
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.905
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87218
_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    1.358
_exptl_crystal_description       needle
_exptl_crystal_F_000             2500
_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 MgCl2 at 1 mg/mL'
_exptl_crystal_size_max          0.71
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.725
_refine_diff_density_min         -0.409
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     410
_refine_ls_number_reflns         5706
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1287
_refine_ls_R_factor_gt           0.0753
_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^)+(0.0654P)^2^+4.4294P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1711
_refine_ls_wR_factor_ref         0.2033
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3396
_reflns_number_total             5706
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc00553d2.cif
_cod_data_source_block           Mg_2_B
_cod_depositor_comments
'Adding full bibliography for 7131429--7131437.cif.'
_cod_original_sg_symbol_H-M      'P 4/n'
_cod_database_code               7131435
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C50H50N50O50B25Mg10Cl10
_shelx_estimated_absorpt_t_max   0.956
_shelx_estimated_absorpt_t_min   0.566
_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. Others
 Fixed Sof: H20C(0.25) H20D(0.25) H20E(0.25) H20F(0.25) O100(0.5) H10A(0.5)
 H10B(0.5) O101(0.5) H10C(0.5) H10D(0.5)
3.a Free rotating group:
 O120(H12A,H12B), O130(H13A,H13B), O110(H11A,H11B), O100(H10A,H10B), O101(H10C,
 H10D)
3.b Rotating group:
 O201(H20A,H20B), O202(H20C,H20D), O200(H20E,H20F)
3.c Aromatic/amide H refined with riding coordinates:
 C35(H35), C32(H32), C33(H33), C25(H25), C7(H7), C26(H26), C36(H36), C6(H6),
 C23(H23), C3(H3), C4(H4), C22(H22), C12(H12), C13(H13), C9(H9), C10(H10)
3.d X=CH2 refined with riding coordinates:
 N2(H2A,H2B), N4(H4A,H4B), N3(H3A,H3B), N1(H1A,H1B)
;
_shelx_res_checksum              55331
_shelx_hkl_checksum              3605
_ins_header
;
TITL PMN-C-21-addMgCl2-repro in P4/n 
REM P4/n (#85 in standard setting)
CELL 1.54184  19.533248  19.533248  15.157906  90.0000  90.0000  90.0000
ZERR    2.00   0.000498   0.000498   0.000435   0.0000   0.0000   0.0000
LATT  1
SYMM -x+1/2,-y+1/2, z 
SYMM -y+1/2, x, z 
SYMM  y,-x+1/2, z 
SFAC C H B N O Mg Cl
UNIT 100.00 100.00 50.00 100.00 100.00 20.00 20.00
REM  CrysAlisPro recorded range (K): Min=150.0; max=150.1; aver:150.0
TEMP -123
SIZE 0.05 0.08 0.71
TREF
HKLF 4
END
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.217
_oxdiff_exptl_absorpt_empirical_full_min 0.672