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_7131437
_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), H20 K2 O10, 10(H2 O)'
_chemical_formula_sum            'C112 H136 B2 K2 N16 O36'
_chemical_formula_weight         2382.16
_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                   19.618(3)
_cell_length_b                   19.618(3)
_cell_length_c                   14.977(3)
_cell_measurement_reflns_used    644
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      23.62
_cell_measurement_theta_min      2.63
_cell_volume                     5764.1(17)
_computing_cell_refinement       'XDS (Kabsch, 2010)'
_computing_data_collection       'AS QEGUI'
_computing_data_reduction        'XDS (Kabsch, 2010)'
_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_temperature      100.0(2)
_diffrn_detector_area_resol_mean 13.3
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'MX2 Beamline Australian Synchrotron'
_diffrn_measurement_method       'Omega Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1038
_diffrn_reflns_av_unetI/netI     0.0407
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            77857
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.379
_diffrn_reflns_theta_min         1.360
_diffrn_source                   'MX2 Beamline Australian Synchrotron'
_exptl_absorpt_coefficient_mu    0.172
_exptl_absorpt_correction_T_max  0.8623
_exptl_absorpt_correction_T_min  0.6423
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.2088 before and 0.0604 after correction.
The Ratio of minimum to maximum transmission is 0.7449.
The \l/2 correction factor is 0.0015.
;
_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    1.373
_exptl_crystal_description       needle
_exptl_crystal_F_000             2512
_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 KCl at 1 mg/mL.'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.734
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     400
_refine_ls_number_reflns         5864
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0710
_refine_ls_R_factor_gt           0.0591
_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^)+(0.1021P)^2^+3.7042P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1674
_refine_ls_wR_factor_ref         0.1799
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4752
_reflns_number_total             5864
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc00553d2.cif
_cod_data_source_block           K_2_B
_cod_depositor_comments
'Adding full bibliography for 7131429--7131437.cif.'
_cod_original_cell_volume        5764(2)
_cod_original_sg_symbol_H-M      'P 4/n'
_cod_database_code               7131437
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.997
_shelx_estimated_absorpt_t_min   0.966
_diffrn_measurement_detector_type 'Dectris Eiger 16M'
_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: O104(0.5) HP(0.5) HQ(0.5) O3(0.5) HR(0.5) HS(0.5)
3.a Free rotating group:
 O101(H,HA), O100(HD,HE), O104(HP,HQ)
3.b Rotating group:
 O102(HB,HC), O3(HR,HS)
3.c Secondary CH2 refined with riding coordinates:
 O103(HF,HG)
3.d Aromatic/amide H refined with riding coordinates:
 C35(HH), C36(HI), C3(H3), C4(H4), C32(HJ), C33(HK), C7(H7), C6(H6), C22(HL),
 C23(HM), C9(H9), C10(H10), C26(HN), C12(H12), C25(HO), C13(H13)
3.e X=CH2 refined with riding coordinates:
 N2(H2A,H2B), N4(H4A,H4B), N3(H3A,H3B), N1(H1A,H1B)
;
_shelx_res_checksum              593
_shelx_hkl_checksum              34613
_olex2_submission_special_instructions 'No special instructions were received'