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_7131431
_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), 2(C16 H36 N)'
_chemical_formula_sum            'C144 H168 B2 N18 O16'
_chemical_formula_weight         2428.57
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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
;
2023-01-31 deposited with the CCDC.	2023-03-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.209(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.0407(7)
_cell_length_b                   39.4728(15)
_cell_length_c                   18.8173(12)
_cell_measurement_reflns_used    5868
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      60.8800
_cell_measurement_theta_min      4.1380
_cell_volume                     20276.8(16)
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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   -102.00 -21.00   1.00   15.00    --  -36.03 -57.00-150.00   81
  2  \w     34.00  80.00   1.00   15.00    --   36.03-125.00  30.00   46
  3  \w      6.00  69.00   1.00   15.00    --   36.03 -99.00 150.00   63
  4  \w     18.00  89.00   1.00   60.00    --   85.19 -61.00 -30.00   71
  5  \w     15.00  93.00   1.00   60.00    --   85.19 -30.00  60.00   78
  6  \w     67.00 152.00   1.00   60.00    --   85.19  61.00  60.00   85
  7  \w     26.00 105.00   1.00   60.00    --   85.19 -77.00 -90.00   79
  8  \w     47.00 105.00   1.00   60.00    --   85.19 -15.00-150.00   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      -0.0157095000
_diffrn_orient_matrix_UB_12      0.0363119000
_diffrn_orient_matrix_UB_13      -0.0251366000
_diffrn_orient_matrix_UB_21      -0.0059739000
_diffrn_orient_matrix_UB_22      -0.0109133000
_diffrn_orient_matrix_UB_23      -0.0801240000
_diffrn_orient_matrix_UB_31      -0.0538513000
_diffrn_orient_matrix_UB_32      -0.0093688000
_diffrn_orient_matrix_UB_33      -0.0039088000
_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  0.0701
_diffrn_reflns_av_unetI/netI     0.0995
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            55310
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        58.934
_diffrn_reflns_theta_max         58.934
_diffrn_reflns_theta_min         3.729
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.417
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78306
_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    0.796
_exptl_crystal_description       needle
_exptl_crystal_F_000             5184
_exptl_crystal_recrystallization_method
'Crystallised using diphenylbisamidinium.2Cl with TBA5.tetraboratecarboxylate in 50% EtOH. Final concentration = 2 mM.'
_exptl_crystal_size_max          0.9
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.602
_refine_diff_density_min         -0.315
_refine_diff_density_rms         0.061
_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     1639
_refine_ls_number_reflns         28883
_refine_ls_number_restraints     83
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.1611
_refine_ls_R_factor_gt           0.1052
_refine_ls_shift/su_max          0.030
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3097
_refine_ls_wR_factor_ref         0.3633
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13406
_reflns_number_total             28883
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc00553d2.cif
_cod_data_source_block           TBA_2_B
_cod_depositor_comments
'Adding full bibliography for 7131429--7131437.cif.'
_cod_database_code               7131431
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C50H50N25O50B20
_shelx_estimated_absorpt_t_max   0.971
_shelx_estimated_absorpt_t_min   0.706
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C202-C200
 2.54 with sigma of 0.02
 C150-C151
 1.34 with sigma of 0.01
 C50-C53
 1.34 with sigma of 0.01
 C201-C200
 1.54 with sigma of 0.01
 C230-C231
 1.54 with sigma of 0.01
 C321-C320
 1.51 with sigma of 0.01
 C231-C230
 1.51 with sigma of 0.01
 C211-C210
 1.51 with sigma of 0.01
 C210-C211
 1.51 with sigma of 0.01
 C330-C331
 1.51 with sigma of 0.01
 C201-C15
 1.51 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C202 \\sim C201 \\sim C200 \\sim C203 \\sim C223 \\sim C222 \\sim C221 \\sim
C220 \\sim C213 \\sim C212 \\sim C211 \\sim C210 \\sim C233 \\sim C232 \\sim
C231 \\sim C230: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 1.7A
4. Others
 Fixed Sof: C200(0.5) H20E(0.5) H20F(0.5) H20G(0.5) H20J(0.5) H20K(0.5)
 H20H(0.5) H20I(0.5) C15(0.5) H15A(0.5) H15B(0.5) H15C(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C223(H22A,H22B), C233(H23A,H23B), C221(H22C,H22D), C213(H21A,H21B), C203(H20A,
 H20B), C222(H22E,H22F), C202(H20C,H20D), C211(H21C,H21D), C323(H32A,H32B),
 C232(H23C,H23D), C212(H21E,H21F), C322(H32C,H32D), C333(H33A,H33B), C332(H33C,
 H33D), C313(H31A,H31B), C303(H30A,H30B), C321(H32E,H32F), C231(H23E,H23F),
 C331(H33E,H33F), C302(H30C,H30D), C301(H30E,H30F), C311(H31C,H31D), C312(H31E,
 H31F), C201(H20J,H20K), C201(H20H,H20I)
5.b Aromatic/amide H refined with riding coordinates:
 C145(H145), C173(H173), C172(H172), C146(H146), C13(H13), C163(H163),
 C176(H176), C143(H143), C62(H62), C63(H63), C9(H9), C156(H156), C175(H175),
 C132(H132), C165(H165), C166(H166), C153(H153), C102(H102), C103(H103),
 C155(H155), C142(H142), C12(H12), C136(H136), C68(H68), C72(H72), C162(H162),
 C65(H65), C112(H112), C69(H69), C133(H133), C135(H135), C4(H4), C152(H152),
 C10(H10), C66(H66), C113(H113), C3(H3), C28(H28), C6(H6), C106(H106), C7(H7),
 C71(H71), C115(H115), C125(H125), C29(H29), C123(H123), C25(H25), C105(H105),
 C26(H26), C31(H31), C116(H116), C32(H32), C23(H23), C122(H122), C22(H22),
 C43(H43), C126(H126), C51(H51), C42(H42), C52(H52), C45(H45), C46(H46),
 C49(H49), C48(H48)
5.c X=CH2 refined with riding coordinates:
 N3(H3A,H3B), N63(H63A,H63B), N60(H60A,H60B), N61(H61A,H61B), N4(H4A,H4B),
 N62(H62A,H62B), N23(H23J,H23K), N21(H21J,H21K), N40(H40A,H40B), N20(H20L,H20M),
  N22(H22J,H22K), N2(H2A,H2B), N1(H1A,H1B), N41(H41A,H41B), N42(H42A,H42B),
 N43(H43A,H43B)
5.d Idealised Me refined as rotating group:
 C220(H22G,H22H,H22I), C210(H21G,H21H,H21I), C320(H32G,H32H,H32I), C300(H30G,
 H30H,H30I), C230(H23G,H23H,H23I), C310(H31G,H31H,H31I), C330(H33G,H33H,H33I),
 C200(H20E,H20F,H20G), C15(H15A,H15B,H15C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              49628
_shelx_hkl_checksum              38401
_shelx_fab_checksum              71389
_ins_header
;
TITL PMN-C-21-repro in P2(1)/c 
REM P2(1)/c (#14 in standard setting)
CELL 1.54184  28.040691  39.472837  18.817325  90.0000 103.2091  90.0000
ZERR    8.00   0.000708   0.001514   0.001173   0.0000   0.0042   0.0000
LATT  1
SYMM -x, y+1/2,-z+1/2 
SFAC C H B N O
UNIT 400.00 400.00 160.00 200.00 400.00
REM  CrysAlisPro recorded range (K): Min=150.0; max=150.0; aver:150.0
TEMP -123
SIZE 0.07 0.11 0.90
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 1.426
_oxdiff_exptl_absorpt_empirical_full_min 0.614