Fascinating Supramolecular Assembly through Noncovalent Interactions Involving Anions in Organic Ionic Crystals
Hu, Chen; Wang, Meiyi; Han, Xiao; Fan, Jingyi; Wei, Donghui; Ding, Jie; Ma, Zhiwei; Xiao, Guanjun; Zou, Bo; Hou, Hongwei; The Journal of Physical Chemistry C 125 (2021) 22346–22353; doi:10.1021/acs.jpcc.1c07151

data_1565120
_publ_section_title
;
 Fascinating Supramolecular Assembly through Noncovalent Interactions
 Involving Anions in Organic Ionic Crystals
;
_journal_issue                   40
_journal_name_full               'The Journal of Physical Chemistry C'
_journal_page_first              22346
_journal_page_last               22353
_journal_paper_doi               10.1021/acs.jpcc.1c07151
_journal_volume                  125
_journal_year                    2021
_chemical_formula_moiety         '0.25(C16 H14 N6 S), 0.25(N2 O6)'
_chemical_formula_sum            'C4 H3.5 N2 O1.5 S0.25'
_chemical_formula_weight         111.60
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-10-08
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                77.895(2)
_cell_angle_beta                 76.682(2)
_cell_angle_gamma                68.795(2)
_cell_formula_units_Z            8
_cell_length_a                   8.3523(2)
_cell_length_b                   8.8031(2)
_cell_length_c                   13.6886(4)
_cell_measurement_reflns_used    4414
_cell_measurement_temperature    199.99(10)
_cell_measurement_theta_max      73.6160
_cell_measurement_theta_min      5.7550
_cell_volume                     904.19(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      199.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.959
_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    -22.00  30.00   0.50    0.50    --    0.00 -77.00  30.00  104
  2  \w     17.00  43.00   0.50    0.50    --    0.00  38.00-150.00   52
  3  \w    -27.00  31.00   0.50    0.50    --    0.00 -82.00-150.00  116
  4  \w    -88.00 -40.00   0.50    0.50    --    0.00 -77.00  30.00   96
  5  \w    -87.00 -35.00   0.50    0.50    --    0.00 -82.00-150.00  104
  6  \w      7.00 128.00   0.50    0.90    --   95.20 -82.00  60.00  242
  7  \w      7.00 119.00   0.50    0.90    --   95.20 -61.00-150.00  224
  8  \w     22.00  81.00   0.50    0.90    --   95.20 -77.00 -30.00  118
  9  \w     74.00 124.00   0.50    0.90    --   95.20 -82.00-150.00  100
 10  \w     27.00  53.00   0.50    0.90    --   95.20 -82.00-150.00   52
 11  \w     31.00  81.00   0.50    0.90    --   95.20 -45.00 -60.00  100
 12  \w     85.00 111.00   0.50    0.90    --   95.20 -45.00  60.00   52
 13  \w     78.00 123.00   0.50    0.90    --   95.20 -15.00  60.00   90
 14  \w     11.00 108.00   0.50    0.90    --   95.20 -61.00  60.00  194
 15  \w      9.00  75.00   0.50    0.90    --   95.20 -77.00  30.00  132
 16  \w     93.00 183.00   0.50    0.90    --   95.20  15.00 -60.00  180
 17  \w     71.00 103.00   0.50    0.90    --   95.20 -82.00 150.00   64
 18  \w      8.00  60.00   0.50    0.90    --   95.20 -15.00  60.00  104
 19  \w     82.00 118.00   0.50    0.90    --   95.20 -82.00 -60.00   72
 20  \w     94.00 121.00   0.50    0.90    --   95.20 -82.00   0.00   54
 21  \w      8.00 108.00   0.50    0.90    --   95.20 -30.00 150.00  200
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1679086000
_diffrn_orient_matrix_UB_12      -0.0099560000
_diffrn_orient_matrix_UB_13      -0.0779221000
_diffrn_orient_matrix_UB_21      0.0776238000
_diffrn_orient_matrix_UB_22      0.0448191000
_diffrn_orient_matrix_UB_23      0.0773417000
_diffrn_orient_matrix_UB_31      0.0779813000
_diffrn_orient_matrix_UB_32      -0.1839166000
_diffrn_orient_matrix_UB_33      0.0398348000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0260
_diffrn_reflns_av_unetI/netI     0.0386
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8409
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.050
_diffrn_reflns_theta_min         3.351
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.129
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81443
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.640
_exptl_crystal_description       block
_exptl_crystal_F_000             460
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.385
_refine_diff_density_min         -0.372
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         3515
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0641
_refine_ls_R_factor_gt           0.0574
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0765P)^2^+0.7718P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1510
_refine_ls_wR_factor_ref         0.1562
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3090
_reflns_number_total             3515
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jp1c07151_si_002.cif
_cod_data_source_block           20191208b1
_cod_original_formula_sum        'C4 H3.50 N2 O1.50 S0.25'
_cod_database_code               1565120
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C H O N S Ag F'
_chemical_oxdiff_usercomment     ' '
_shelx_estimated_absorpt_t_max   0.701
_shelx_estimated_absorpt_t_min   0.675
_reflns_odcompleteness_completeness 99.54
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Others
 Fixed Sof: O3(0.5) O6(0.5) O4(0.5) O5(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 N5(H5), N3(H3), N6(H6), N4(H4), C4(H4A), C13(H13), C7(H7), C16(H16), C8(H8),
 C15(H15), C14(H14), C3(H3A), C1(H1), C2(H2)
;
_shelx_res_checksum              89770
_shelx_hkl_checksum              64733
_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 1.324
_oxdiff_exptl_absorpt_empirical_full_min 0.796