Weak Links To Differentiate Weak Bonds: Size-Selective Response of π-Conjugated Macrocycle Gels to Ammonium Ions.
Kang, Suk-Il; Lee, Milim; Lee, Dongwhan; Journal of the American Chemical Society 141 (2019) 5980–5986; doi:10.1021/jacs.9b01002

data_4128407
_publ_section_title
;
 Weak Links To Differentiate Weak Bonds: Size-Selective Response of
 \p-Conjugated Macrocycle Gels to Ammonium Ions.
;
_journal_issue                   14
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5980
_journal_page_last               5986
_journal_paper_doi               10.1021/jacs.9b01002
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C30 H28 N6 O4, H2 O'
_chemical_formula_sum            'C30 H30 N6 O5'
_chemical_formula_weight         554.61
_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'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-01-08
_audit_creation_method
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Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
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_cell_length_b                   21.5727(10)
_cell_length_c                   14.8041(7)
_cell_measurement_reflns_used    4516
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      29.1010
_cell_measurement_theta_min      3.9550
_cell_volume                     2685.6(2)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
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_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4525
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.9930
_diffrn_measured_fraction_theta_max 0.8195
_diffrn_measurement_details
;
  1 omega   35.00  100.00   1.0000  127.8750
omega____ theta____ kappa____ phi______ frames
    -       11.5133  178.0000  120.0000 65

  2 omega  -57.00   37.00   1.0000  127.8750
omega____ theta____ kappa____ phi______ frames
    -       11.5133  -77.0000  -90.0000 94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0107354000
_diffrn_orient_matrix_UB_12      0.0236400000
_diffrn_orient_matrix_UB_13      -0.0318190000
_diffrn_orient_matrix_UB_21      0.0563779000
_diffrn_orient_matrix_UB_22      0.0147035000
_diffrn_orient_matrix_UB_23      0.0334973000
_diffrn_orient_matrix_UB_31      0.0617606000
_diffrn_orient_matrix_UB_32      -0.0175087000
_diffrn_orient_matrix_UB_33      -0.0147845000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0277
_diffrn_reflns_av_unetI/netI     0.0479
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            11390
_diffrn_reflns_theta_full        25.0000
_diffrn_reflns_theta_max         29.66
_diffrn_reflns_theta_min         3.40
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.096
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89329
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.3716
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1168.5612
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.5230
_refine_diff_density_min         -0.4344
_refine_diff_density_rms         0.0957
_refine_ls_d_res_high            0.7180
_refine_ls_d_res_low             5.9970
_refine_ls_goodness_of_fit_ref   1.0581
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    44
_refine_ls_number_parameters     386
_refine_ls_number_reflns         6229
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0581
_refine_ls_R_factor_all          0.0699
_refine_ls_R_factor_gt           0.0487
_refine_ls_shift/su_max          0.0005
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0685P)^2^+0.6597P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1253
_refine_ls_wR_factor_ref         0.1391
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              29
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_reflns_limit_l_min              0
_reflns_number_gt                4782
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_cod_data_source_file            ja9b01002_si_002.cif
_cod_data_source_block           ML2-113
_cod_database_code               4128407
_chemical_oxdiff_formula         C24H20O4N6
_reflns_odcompleteness_completeness 98.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C14(H14), C22(H22), C26(H26), C27(H27), C28(H28), C32(H32), C34(H34), C35(H35)
2.b Idealised Me refined as rotating group:
 C36(H36a,H36b,H36c), C37(H37a,H37b,H37c), C38(H38a,H38b,H38c), C39(H39a,H39b,
 H39c), C40(H40a,H40b,H40c), C41(H41a,H41b,H41c)
2.c Idealised tetrahedral OH refined as rotating group:
 O1(H1), O3(H3)
;
_olex2_date_sample_data_collection 1442373292.74
_olex2_submission_special_instructions 'No special instructions were received'