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_7131436
_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, 5(H2 O), 2.5(C14 H16 N4)'
_chemical_formula_sum            'C63 H66 B N10 O13'
_chemical_formula_weight         1182.06
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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
;
2023-01-31 deposited with the CCDC.	2023-03-09 downloaded from the CCDC.
;
_cell_angle_alpha                110.045(3)
_cell_angle_beta                 110.898(3)
_cell_angle_gamma                96.920(2)
_cell_formula_units_Z            2
_cell_length_a                   14.1697(4)
_cell_length_b                   14.5406(4)
_cell_length_c                   16.0657(5)
_cell_measurement_reflns_used    14684
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      60.9630
_cell_measurement_theta_min      3.5720
_cell_volume                     2791.70(18)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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   -107.00  -7.00   1.00    1.00    --  -36.03 -19.00 -90.00  100
  2  \w    -86.00  -6.00   1.00    1.00    --  -36.03 125.00   0.00   80
  3  \w   -103.00 -19.00   1.00    1.00    --  -36.03 -57.00-150.00   84
  4  \w    103.00 153.00   1.00    6.00    --   85.19  77.00 -30.00   50
  5  \w     17.00 103.00   1.00    6.00    --   85.19 -45.00-120.00   86
  6  \w     18.00 103.00   1.00    6.00    --   85.19 -61.00  60.00   85
  7  \w     16.00 106.00   1.00    6.00    --   85.19 -95.00 -90.00   90
  8  \w     16.00 106.00   1.00    6.00    --   85.19 -95.00-180.00   90
  9  \w     15.00 107.00   1.00    6.00    --   85.19 -30.00 -60.00   92
 10  \w     18.00 112.00   1.00    6.00    --   85.19 -77.00-150.00   94
 11  \w     16.00 106.00   1.00    6.00    --   85.19 -95.00  30.00   90
 12  \w     16.00 154.00   1.00    6.00    --   85.19   0.00 -30.00  138
 13  \w   -103.00 -19.00   1.00    1.00    --  -36.03 -57.00 120.00   84
 14  \w   -103.00 -19.00   1.00    1.00    --  -36.03 -57.00  60.00   84
 15  \w    -53.00  31.00   1.00    1.00    --  -36.03  57.00-120.00   84
 16  \w     67.00 152.00   1.00    6.00    --   85.19  61.00   0.00   85
 17  \w     67.00 152.00   1.00    6.00    --   85.19  61.00 150.00   85
 18  \w     67.00 152.00   1.00    6.00    --   85.19  61.00-180.00   85
 19  \w     64.00 155.00   1.00    6.00    --   85.19  30.00 150.00   91
 20  \w     67.00 152.00   1.00    6.00    --   85.19  61.00  90.00   85
 21  \w     68.00 154.00   1.00    6.00    --   85.19  45.00-120.00   86
 22  \w     68.00 154.00   1.00    6.00    --   85.19  45.00 -30.00   86
 23  \w     67.00 152.00   1.00    6.00    --   85.19  61.00 -90.00   85
 24  \w     68.00 154.00   1.00    6.00    --   85.19  45.00  60.00   86
 25  \w   -103.00 -19.00   1.00    1.00    --  -36.03 -57.00 150.00   84
 26  \w   -103.00 -19.00   1.00    1.00    --  -36.03 -57.00   0.00   84
 27  \w   -103.00 -19.00   1.00    1.00    --  -36.03 -57.00 -60.00   84
 28  \w     67.00 152.00   1.00    6.00    --   85.19  61.00  60.00   85
 29  \w     67.00 152.00   1.00    6.00    --   85.19  61.00-120.00   85
 30  \w     67.00 152.00   1.00    6.00    --   85.19  61.00 -30.00   85
 31  \w     67.00 152.00   1.00    6.00    --   85.19  61.00 120.00   85
 32  \w     67.00 152.00   1.00    6.00    --   85.19  61.00  30.00   85
;
_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      0.0648795000
_diffrn_orient_matrix_UB_12      0.0649099000
_diffrn_orient_matrix_UB_13      -0.0296206000
_diffrn_orient_matrix_UB_21      0.0423661000
_diffrn_orient_matrix_UB_22      0.0878169000
_diffrn_orient_matrix_UB_23      0.1025652000
_diffrn_orient_matrix_UB_31      0.0930676000
_diffrn_orient_matrix_UB_32      -0.0429877000
_diffrn_orient_matrix_UB_33      0.0366383000
_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  0.0417
_diffrn_reflns_av_unetI/netI     0.0294
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            40019
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        58.935
_diffrn_reflns_theta_max         58.935
_diffrn_reflns_theta_min         3.474
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.819
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94016
_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    1.406
_exptl_crystal_description       block
_exptl_crystal_F_000             1246
_exptl_crystal_recrystallization_method
'Crystallised using diphenylbisamidinium.2Cl with TBA5.tetraboratecarboxylate in H2O. Final concentration = 2 mM.'
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.391
_refine_diff_density_min         -0.491
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     799
_refine_ls_number_reflns         8003
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0388
_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^)+(0.0488P)^2^+1.5095P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0950
_refine_ls_wR_factor_ref         0.1006
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6891
_reflns_number_total             8003
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc00553d2.cif
_cod_data_source_block           2_B
_cod_depositor_comments
'Adding full bibliography for 7131429--7131437.cif.'
_cod_original_cell_volume        2791.70(16)
_cod_database_code               7131436
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C50H50N50O50B25
_shelx_estimated_absorpt_t_max   0.908
_shelx_estimated_absorpt_t_min   0.828
_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.a Free rotating group:
 O100(H10C,H10D), O130(H13C,H13D), O140(H14A,H14B), O120(H12C,H12D), O110(H11C,
 H11D)
2.b Aromatic/amide H refined with riding coordinates:
 C53(H53), C70(H70), C62(H62), C52(H52), C59(H59), C76(H76), C73(H73),
 C66(H66), C67(H67), C60(H60), C55(H55), C32(H32), C74(H74), C77(H77), C56(H56),
  C69(H69), C63(H63), C45(H45), C31(H31), C25(H25), C46(H46), C9(H9), C3(H3),
 C22(H22), C12(H12), C4(H4), C26(H26), C10(H10), C6(H6), C29(H29), C28(H28),
 C43(H43), C13(H13), C23(H23), C42(H42), C7(H7)
2.c X=CH2 refined with riding coordinates:
 N20(H20A,H20B), N21(H21A,H21B), N12(H12A,H12B), N13(H13A,H13B), N3(H3A,H3B),
 N4(H4A,H4B), N11(H11A,H11B), N10(H10A,H10B), N2(H2A,H2B), N1(H1A,H1B)
;
_shelx_res_checksum              79116
_shelx_hkl_checksum              17236
_ins_header
;
TITL PMN-C-21-H2O-repro in P-1 
REM P-1 (#2 in standard setting)
CELL 1.54184  14.169663  14.540633  16.065734 110.0445 110.8977  96.9201
ZERR    1.00   0.000397   0.000406   0.000456   0.0026   0.0026   0.0023
LATT  1
SFAC C H B N O
UNIT 50.00 50.00 25.00 50.00 50.00
REM  CrysAlisPro recorded range (K): Min=150.0; max=150.0; aver:150.0
TEMP -123
SIZE 0.12 0.18 0.24
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 1.227
_oxdiff_exptl_absorpt_empirical_full_min 0.763