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_7131434
_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 Ca O6, 16(H2 O)'
_chemical_formula_sum            'C112 H140 B2 Ca N16 O38'
_chemical_formula_weight         2380.08
_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             2023-01-11
_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                   19.5879(12)
_cell_length_b                   19.5879(12)
_cell_length_c                   15.0908(14)
_cell_measurement_reflns_used    242
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      43.2990
_cell_measurement_theta_min      3.7000
_cell_volume                     5790.1(7)
_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 0.990
_diffrn_measured_fraction_theta_max 0.990
_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    -87.00  -9.00   1.00   35.00    --  -36.28 125.00  60.00   78
  2  \w     27.00  60.00   1.00   35.00    --   36.28-125.00  90.00   33
  3  \w    122.00 155.00   1.00  140.00    --   85.03 111.00 120.00   33
  4  \w    105.00 155.00   1.00  140.00    --   85.03 111.00 -60.00   50
  5  \w     14.00 122.00   1.00  140.00    --   85.03 -15.00-120.00  108
;
_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      0.0540676000
_diffrn_orient_matrix_UB_12      0.0162839000
_diffrn_orient_matrix_UB_13      -0.0709283000
_diffrn_orient_matrix_UB_21      -0.0292544000
_diffrn_orient_matrix_UB_22      0.0725324000
_diffrn_orient_matrix_UB_23      -0.0098339000
_diffrn_orient_matrix_UB_31      0.0490796000
_diffrn_orient_matrix_UB_32      0.0255097000
_diffrn_orient_matrix_UB_33      0.0728363000
_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  0.1567
_diffrn_reflns_av_unetI/netI     0.2388
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8219
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        58.914
_diffrn_reflns_theta_max         58.914
_diffrn_reflns_theta_min         3.697
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.239
_exptl_absorpt_correction_T_max  0.64751
_exptl_absorpt_correction_T_min  0.62855
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Spherical absorption correction
using equivalent radius and absorption coefficient.
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    1.365
_exptl_crystal_description       needle
_exptl_crystal_F_000             2516
_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 CaCl2 at 1 mg/mL.'
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_exptl_crystal_size_rad          0.044
_refine_diff_density_max         0.346
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.963
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     408
_refine_ls_number_reflns         4134
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.967
_refine_ls_R_factor_all          0.2630
_refine_ls_R_factor_gt           0.1038
_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^)+(0.1203P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2393
_refine_ls_wR_factor_ref         0.3546
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1297
_reflns_number_total             4134
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc00553d2.cif
_cod_data_source_block           Ca_2_B
_cod_depositor_comments
'Adding full bibliography for 7131429--7131437.cif.'
_cod_original_cell_volume        5790.1(9)
_cod_original_sg_symbol_H-M      'P 4/n'
_cod_database_code               7131434
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C50 H50 N50 O50 B25 Ca10 Cl10'
_shelx_estimated_absorpt_t_max   0.964
_shelx_estimated_absorpt_t_min   0.631
_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
 C7-C2
 1.39 with sigma of 0.01
 C30-O11
 1.21 with sigma of 0.02
 C20-C21
 1.39 with sigma of 0.02
3. Others
 Fixed Sof: H10A(0.25) H10B(0.25) O106(0.75) H10M(0.75) H10N(0.75) H10E(0.25)
 H10F(0.25) O107(0.25) H10O(0.25) H10P(0.25)
4.a Free rotating group:
 O104(H10G,H10H), O105(H10I,H10J), O100(H10K,H10L), O106(H10M,H10N), O107(H10O,
 H10P)
4.b Rotating group:
 O101(H10C,H10D)
4.c Aromatic/amide H refined with riding coordinates:
 C36(H36), C35(H35), C33(H33), C12(H12), C13(H13), C32(H32), C22(H22),
 C23(H23), C9(H9), C10(H10), C25(H25), C26(H26), C6(H6), C7(H7), C3(H3), C4(H4)
4.d X=CH2 refined with riding coordinates:
 O102(H10A,H10B), N2(H2A,H2B), N4(H4A,H4B), N1(H1A,H1B), N3(H3A,H3B),
 O103(H10E,H10F)
;
_shelx_res_checksum              0
_shelx_hkl_checksum              9184
_ins_header
;
TITL PMN-C-21-CaCl2-repro-090 in P4/n 
REM P4/n (#85 in standard setting)
CELL 1.54184  19.587876  19.587876  15.090794  90.0000  90.0000  90.0000
ZERR    2.00   0.001174   0.001174   0.001408   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 Cl Ca
UNIT 100.00 100.00 50.00 100.00 100.00 20.00 20.00
REM  CrysAlisPro recorded range (K): Min=150.0; max=150.0; aver:150.0
TEMP -123
SIZE 0.03 0.03 0.41
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 1.329
_oxdiff_exptl_absorpt_empirical_full_min 0.593