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_4128408
_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         'C22 H16 Br2 N6 O3'
_chemical_formula_sum            'C22 H16 Br2 N6 O3'
_chemical_formula_weight         572.22
_chemical_name_systematic
(2^1E,2^8E)-1^5,3^5-dibromo-2^2,2^7-dihydro-4,7,10-trioxa-2(2,7)-benzo[1,2-d:3,4-d']bis([1,2,3]triazole)a-1,3(1,2)-dibenzenacyclodecaphane
_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
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
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_cell_length_b                   26.1510(8)
_cell_length_c                   18.5287(7)
_cell_measurement_reflns_used    12706
_cell_measurement_temperature    100.1(8)
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_cell_measurement_theta_min      4.1300
_cell_volume                     2037.77(13)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_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      100.1(8)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2262
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.9835
_diffrn_measured_fraction_theta_max 0.9835
_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    -66.00  33.00   1.00   11.12    --  -41.24  38.00 -30.00   99
  2  \w   -116.00 -17.00   1.00   11.12    --  -41.24 -38.00 150.00   99
  3  \w    -69.00  32.00   1.00   11.12    --  -41.24  57.00  60.00  101
  4  \w    -96.00  -2.00   1.00   11.12    --  -41.24 125.00  60.00   94
  5  \w     36.00 116.00   1.00   21.92    --  112.00-111.00 120.00   80
  6  \w     36.00 140.00   1.00   21.92    --  112.00 -30.00 -60.00  104
  7  \w     36.00 116.00   1.00   21.92    --  112.00-111.00-150.00   80
  8  \w     36.00 140.00   1.00   21.92    --  112.00 -30.00-150.00  104
  9  \w     86.00 178.00   1.00   21.92    --  112.00  45.00 -90.00   92
 10  \w     36.00 145.00   1.00   21.92    --  112.00 -77.00  90.00  109
 11  \w     36.00 116.00   1.00   21.92    --  112.00-111.00  60.00   80
 12  \w     36.00 140.00   1.00   21.92    --  112.00 -30.00  90.00  104
 13  \w     36.00 145.00   1.00   21.92    --  112.00 -77.00-120.00  109
 14  \w   -113.00 -13.00   1.00   11.12    --  -41.24 -57.00  60.00  100
 15  \w   -113.00 -13.00   1.00   11.12    --  -41.24 -57.00-120.00  100
 16  \w   -113.00 -13.00   1.00   11.12    --  -41.24 -57.00 -30.00  100
 17  \w      1.00  82.00   1.00   11.12    --   41.24 -99.00-150.00   81
 18  \w     59.00 137.00   1.00   21.92    --  112.00  15.00  60.00   78
 19  \w      9.00 118.00   1.00    8.37    --   41.49  77.00 -30.00  109
 20  \w      9.00 118.00   1.00    8.37    --   41.49  77.00  90.00  109
 21  \w     13.00  86.00   1.00    8.37    --   41.49  57.00 -90.00   73
 22  \w      9.00 118.00   1.00    8.37    --   41.49  77.00-180.00  109
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1620018000
_diffrn_orient_matrix_UB_12      -0.0285138000
_diffrn_orient_matrix_UB_13      0.0665730000
_diffrn_orient_matrix_UB_21      -0.0142215000
_diffrn_orient_matrix_UB_22      -0.0501759000
_diffrn_orient_matrix_UB_23      -0.0438378000
_diffrn_orient_matrix_UB_31      0.3282360000
_diffrn_orient_matrix_UB_32      0.0118663000
_diffrn_orient_matrix_UB_33      -0.0252042000
_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  0.0406
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -3
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            22960
_diffrn_reflns_theta_full        76.4645
_diffrn_reflns_theta_max         76.46
_diffrn_reflns_theta_min         4.15
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.405
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55442
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43d (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.8650
_exptl_crystal_description       needle
_exptl_crystal_F_000             1133.5105
_exptl_crystal_recrystallization_method
'obtained by vapor diffusion of cyclohexane into a CHCl3 solution of this material.'
_exptl_crystal_size_max          0.299
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.025
_refine_diff_density_max         0.4898
_refine_diff_density_min         -0.6239
_refine_diff_density_rms         0.0890
_refine_ls_d_res_high            0.7929
_refine_ls_d_res_low             10.6647
_refine_ls_goodness_of_fit_ref   1.0490
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     361
_refine_ls_number_reflns         4229
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0490
_refine_ls_R_factor_all          0.0322
_refine_ls_R_factor_gt           0.0297
_refine_ls_shift/su_max          0.0007
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0420P)^2^+2.6930P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0775
_refine_ls_wR_factor_ref         0.0797
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              5
_reflns_limit_h_min              -5
_reflns_limit_k_max              32
_reflns_limit_k_min              0
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                3943
_reflns_number_total             4229
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            ja9b01002_si_003.cif
_cod_data_source_block           exp_377
_cod_original_cell_volume        2037.77(12)
_cod_database_code               4128408
_chemical_oxdiff_formula         C22H16Br2N6O3
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_olex2_refinement_description
;
;
_olex2_date_sample_data_collection 2016-06-28
_olex2_exptl_crystal_mounting_method
'placed onto a nylon loop with Paratone-N oil and mounted'
_olex2_submission_original_sample_id SIK-3-34A
_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 2.165
_oxdiff_exptl_absorpt_empirical_full_min 0.591