Assembly and Adsorption Properties of Seven Supramolecular Compounds with Heteromacrocycle Imidazolium.
Li, Yuan-Yuan; Wang, Fu-Rong; Li, Zi-Yan; Yan, Zhen-Ning; Niu, Yun-Yin; ACS omega 4 (2019) 8926–8934; doi:10.1021/acsomega.9b00669

data_4515002
_publ_section_title
;
 Assembly and Adsorption Properties of Seven Supramolecular Compounds with
 Heteromacrocycle Imidazolium.
;
_journal_issue                   5
_journal_name_full               'ACS omega'
_journal_page_first              8926
_journal_page_last               8934
_journal_paper_doi               10.1021/acsomega.9b00669
_journal_volume                  4
_journal_year                    2019
_chemical_formula_moiety         'Ag3 I5, Ag4 I6, 2(C18 H22 N4)'
_chemical_formula_sum            'C36 H44 Ag7 I11 N8'
_chemical_formula_weight         2739.78
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_audit_creation_date             2019-04-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 94.5111(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.6146(4)
_cell_length_b                   11.5003(2)
_cell_length_c                   23.0399(4)
_cell_measurement_reflns_used    8303
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.4950
_cell_measurement_theta_min      3.6160
_cell_volume                     5973.53(18)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41k (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41k (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41k (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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2312
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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     13.60  85.00   0.70   16.50    --   17.91  57.00 -30.00  102
  2  \w    -47.00  44.00   0.70   16.50    --   17.91 -19.00-150.00  130
  3  \w      2.00  42.60   0.70   16.50    --   17.91  77.00-120.00   58
  4  \w    -50.00  -3.80   0.70   16.50    --   17.91 -77.00  30.00   66
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0236747000
_diffrn_orient_matrix_UB_12      -0.0078872000
_diffrn_orient_matrix_UB_13      -0.0180533000
_diffrn_orient_matrix_UB_21      -0.0207344000
_diffrn_orient_matrix_UB_22      -0.0088280000
_diffrn_orient_matrix_UB_23      -0.0243308000
_diffrn_orient_matrix_UB_31      0.0000558000
_diffrn_orient_matrix_UB_32      0.0605430000
_diffrn_orient_matrix_UB_33      -0.0059064000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0373
_diffrn_reflns_av_unetI/netI     0.0549
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            29680
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.414
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    7.965
_exptl_absorpt_correction_T_max  0.688
_exptl_absorpt_correction_T_min  0.366
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41k (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.046
_exptl_crystal_description       plate
_exptl_crystal_F_000             4912
_exptl_crystal_size_max          0.244
_exptl_crystal_size_mid          0.074
_exptl_crystal_size_min          0.061
_refine_diff_density_max         3.486
_refine_diff_density_min         -3.351
_refine_diff_density_rms         0.252
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     576
_refine_ls_number_reflns         12188
_refine_ls_number_restraints     220
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0995
_refine_ls_R_factor_gt           0.0686
_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^)+(0.0872P)^2^+91.2824P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1745
_refine_ls_wR_factor_ref         0.1984
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8413
_reflns_number_total             12188
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao9b00669_si_002.cif
_cod_data_source_block           2
_cod_original_cell_volume        5973.52(18)
_cod_database_code               4515002
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C36H44N8I11Ag7
_reflns_odcompleteness_completeness 99.65
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 N5-C20 \\sim N6-C21 \\sim N8-C27 \\sim N7-C28 \\sim N3-C3 \\sim N4-C2 \\sim
N2-C10 \\sim N1-C9
 with sigma of 0.02
 N5-C19 \\sim N6-C19 \\sim N8-C26 \\sim N7-C26 \\sim N3-C1 \\sim N4-C1 \\sim
N1-C8 \\sim N2-C8
 with sigma of 0.02
 C7-C6 \\sim C6-C5 \\sim C5-C4 \\sim C25-C24 \\sim C24-C23 \\sim C23-C22
 with sigma of 0.02
 N1-C11 \\sim N2-C7 \\sim N3-C4 \\sim N4-C18 \\sim N7-C25 \\sim N8-C26 \\sim
N6-C22 \\sim N5-C36
 with sigma of 0.02
 C36-C33 \\sim C30-C29 \\sim C12-C11 \\sim C18-C15
 with sigma of 0.02
 C17-C12 \\sim C17-C16 \\sim C16-C15 \\sim C15-C14 \\sim C14-C13 \\sim C13-C12
\\sim C34-C33 \\sim C35-C34
 \\sim C35-C30 \\sim C31-C30 \\sim C32-C31 \\sim C33-C32
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Ag1) = Uanis(Ag1A)
Uanis(Ag4) = Uanis(Ag4A)
Uanis(Ag5) = Uanis(Ag5A)
Uanis(Ag7) = Uanis(Ag7A)
Uanis(Ag3) = Uanis(Ag3A)
4. Others
 Sof(Ag1A)=Sof(Ag4A)=Sof(Ag5A)=Sof(Ag7A)=1-FVAR(1)
 Sof(Ag1)=Sof(Ag4)=Sof(Ag5)=Sof(Ag7)=FVAR(1)
 Sof(Ag3A)=1-FVAR(2)
 Sof(Ag3)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C11(H11A,H11B), C18(H18A,
 H18B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B),
 C29(H29A,H29B), C36(H36A,H36B)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C8(H8), C9(H9), C10(H10), C13(H13), C14(H14),
 C16(H16), C17(H17), C19(H19), C20(H20), C21(H21), C26(H26), C27(H27), C28(H28),
  C31(H31), C32(H32), C34(H34), C35(H35)
;
_olex2_date_sample_data_collection 2017-09-08
_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 1.190
_oxdiff_exptl_absorpt_empirical_full_min 0.826
_oxdiff_exptl_absorpt_spherical_max 0.484
_oxdiff_exptl_absorpt_spherical_min 0.477