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_7131430
_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
'H12 Na O6, C28 H16 B O8, 4(H2 O), 2(C14 H16 N4)'
_chemical_formula_sum            'C56 H68 B N8 Na O18'
_chemical_formula_weight         1174.98
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                90
_cell_angle_beta                 92.871(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.2633(6)
_cell_length_b                   14.7730(5)
_cell_length_c                   19.7937(7)
_cell_measurement_reflns_used    4137
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      60.8430
_cell_measurement_theta_min      3.7460
_cell_volume                     5625.8(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      150.00(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    -85.00  -6.00   1.00   15.00    --  -36.63 125.00-150.00   79
  2  \w   -100.00 -21.00   1.00   15.00    --  -36.63 -57.00  60.00   79
  3  \w    110.00 150.00   1.00   80.00    --   84.58  77.00-150.00   40
  4  \w     19.00  99.00   1.00   80.00    --   84.58 -61.00 -30.00   80
  5  \w    112.00 152.00   1.00   80.00    --   84.58  77.00 -60.00   40
  6  \w     99.00 133.00   1.00   80.00    --   84.58 125.00 150.00   34
  7  \w    102.00 144.00   1.00   80.00    --   84.58 125.00-150.00   42
  8  \w    104.00 154.00   1.00   80.00    --   84.58 125.00  60.00   50
  9  \w    103.00 149.00   1.00   80.00    --   84.58  77.00  60.00   46
 10  \w     76.00 154.00   1.00   80.00    --   84.58  30.00-150.00   78
;
_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      0.0337851000
_diffrn_orient_matrix_UB_12      0.0860578000
_diffrn_orient_matrix_UB_13      0.0309160000
_diffrn_orient_matrix_UB_21      -0.0703809000
_diffrn_orient_matrix_UB_22      0.0282446000
_diffrn_orient_matrix_UB_23      0.0269918000
_diffrn_orient_matrix_UB_31      0.0177683000
_diffrn_orient_matrix_UB_32      -0.0516804000
_diffrn_orient_matrix_UB_33      0.0662635000
_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  0.0418
_diffrn_reflns_av_unetI/netI     0.0522
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15878
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        58.932
_diffrn_reflns_theta_max         58.932
_diffrn_reflns_theta_min         3.735
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.933
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73137
_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    1.387
_exptl_crystal_description       needle
_exptl_crystal_F_000             2480
_exptl_crystal_recrystallization_method
'Crystallised using diphenylbisamidinium.2Cl with TBA5.tetraboratecarboxylate in 50% EtOH with 100 equivalent of NaCl. Final concentration = 2 mM.'
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.855
_refine_diff_density_min         -0.689
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     836
_refine_ls_number_reflns         8008
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.1028
_refine_ls_R_factor_gt           0.0804
_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^)+(0.0947P)^2^+14.1103P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2017
_refine_ls_wR_factor_ref         0.2196
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6149
_reflns_number_total             8008
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc00553d2.cif
_cod_data_source_block           Na_2_B
_cod_depositor_comments
'Adding full bibliography for 7131429--7131437.cif.'
_cod_database_code               7131430
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C50H50B20N25O50
_shelx_estimated_absorpt_t_max   0.955
_shelx_estimated_absorpt_t_min   0.668
_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
 O130-H13C = O130-H13D
 0.87 with sigma of 0.02
 O150-H15A = O150-H15B
 0.87 with sigma of 0.02
 O140-H14A = O140-H14B
 0.87 with sigma of 0.02
 H13C-H13D
 1.38 with sigma of 0.04
 H15A-H15B
 1.38 with sigma of 0.04
 H14A-H14B
 1.38 with sigma of 0.04
 Na1-H16A \\sim Na1-H16B
 with sigma of 0.02
 Na1-H15A \\sim Na1-H15B
 with sigma of 0.02
 Na1-H14A \\sim Na1-H14B
 with sigma of 0.02
3. Others
 Fixed Sof: O100(0.5) H10C(0.5) H10D(0.5) O150(0.6666) H15A(0.6666)
 H15B(0.6666) O110(0.5) H11C(0.5) H11D(0.5) O160(0.33333) H16A(0.33333)
 H16B(0.33333) O130(0.75) H13C(0.75) H13D(0.75) O9(0.25) H9A(0.25) H9B(0.25)
 O10(0.5) H10E(0.5) H10F(0.5) O11(0.5) H11E(0.5) H11F(0.5)
4.a Free rotating group:
 O120(H12C,H12D), O200(H20A,H20B), O110(H11C,H11D), O160(H16A,H16B), O9(H9A,
 H9B), O10(H10E,H10F), O11(H11E,H11F)
4.b Rotating group:
 O180(H18A,H18B), O190(H19A,H19B), O170(H17A,H17B), O100(H10C,H10D)
4.c Aromatic/amide H refined with riding coordinates:
 C53(H53), C52(H52), C43(H43), C50(H50), C59(H59), C56(H56), C57(H57), C7(H7),
 C6(H6), C64(H64), C9(H9), C49(H49), C42(H42), C67(H67), C12(H12), C10(H10),
 C45(H45), C14(H14), C63(H63), C66(H66), C60(H60), C3(H3), C4(H4), C46(H46),
 C31(H31), C22(H22), C32(H32), C23(H23), C26(H26), C25(H25), C28(H28), C29(H29)
4.d X=CH2 refined with riding coordinates:
 N4(H4A,H4B), N3(H3A,H3B), N11(H11A,H11B), N1(H1A,H1B), N10(H10A,H10B), N2(H2A,
 H2B), N13(H13A,H13B), N12(H12A,H12B)
;
_shelx_res_checksum              73132
_shelx_hkl_checksum              97155
_ins_header
;
TITL PMN-C-21-NaCl-repro in P2(1)/n 
REM P2(1)/n (#14 in standard setting)
CELL 1.54184  19.263310  14.773009  19.793722  90.0000  92.8710  90.0000
ZERR    2.00   0.000620   0.000452   0.000744   0.0000   0.0034   0.0000
LATT  1
SYMM -x+1/2, y+1/2,-z+1/2 
SFAC C H B N O
UNIT 100.00 100.00 40.00 50.00 100.00
REM  CrysAlisPro recorded range (K): Min=150.0; max=150.0; aver:150.0
TEMP -123
SIZE 0.05 0.10 0.47
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 1.469
_oxdiff_exptl_absorpt_empirical_full_min 0.681