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_4515003
_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 I7, 2(C18 H22 N4), C2 H3 N'
_chemical_formula_sum            'C38 H47 Ag3 I7 N9'
_chemical_formula_weight         1841.75
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-11-14
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                70.132(5)
_cell_angle_beta                 80.175(3)
_cell_angle_gamma                75.172(4)
_cell_formula_units_Z            2
_cell_length_a                   11.5869(3)
_cell_length_b                   13.6244(8)
_cell_length_c                   17.7757(6)
_cell_measurement_reflns_used    4952
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.3720
_cell_measurement_theta_min      3.8420
_cell_volume                     2540.4(2)
_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    'SIR2004 (Burla et al., 2007)'
_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 0.990
_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    -25.00  24.00   0.50   14.50    --  -15.18 -99.00 -30.00   98
  2  \w    -25.00  24.00   0.50   14.50    --  -15.18 -99.00 120.00   98
  3  \w     -1.00  62.00   0.50   14.50    --   17.91  37.00 -30.00  126
  4  \w    -46.00  35.00   0.50   14.50    --   17.91 -57.00-180.00  162
  5  \w     -5.00  35.00   0.50   14.50    --   17.91 -57.00 -60.00   80
  6  \w    -42.00   6.00   0.50   14.50    --   17.91 -57.00 120.00   96
  7  \w      1.00  70.00   0.50   14.50    --   17.91  57.00  90.00  138
;
_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      -0.0227192000
_diffrn_orient_matrix_UB_12      0.0540769000
_diffrn_orient_matrix_UB_13      -0.0014212000
_diffrn_orient_matrix_UB_21      -0.0551273000
_diffrn_orient_matrix_UB_22      -0.0127777000
_diffrn_orient_matrix_UB_23      0.0201573000
_diffrn_orient_matrix_UB_31      0.0221141000
_diffrn_orient_matrix_UB_32      -0.0110987000
_diffrn_orient_matrix_UB_33      0.0375126000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0740
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            16404
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.392
_diffrn_reflns_theta_min         3.375
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.435
_exptl_absorpt_correction_T_max  0.808
_exptl_absorpt_correction_T_min  0.530
_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    2.408
_exptl_crystal_description       plate
_exptl_crystal_F_000             1700
_exptl_crystal_size_max          0.159
_exptl_crystal_size_mid          0.133
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.372
_refine_diff_density_min         -1.316
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     535
_refine_ls_number_reflns         16404
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0747
_refine_ls_R_factor_gt           0.0405
_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^)+(0.0215P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0651
_refine_ls_wR_factor_ref         0.0683
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9954
_reflns_number_total             16404
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao9b00669_si_002.cif
_cod_data_source_block           3
_cod_database_code               4515003
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C38H47N9I7Ag3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.7112(4)
 0.2888(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C37A-N5A
 1 with sigma of 0.02
 N5-C37
 1 with sigma of 0.02
 C37-C38 = C37A-C38A
 1.55 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(N5A) \\sim Ueq, Uanis(N5) \\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C38)
\\sim Ueq, Uanis(C37A) \\sim Ueq, Uanis(C38A) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(Ag3) = Uanis(Ag3A)
Uanis(Ag2) = Uanis(Ag2A)
Uanis(N5) = Uanis(N5A)
Uanis(C38) = Uanis(C38A)
Uanis(C37) = Uanis(C37A)
5. Others
 Sof(Ag3A)=1-FVAR(1)
 Sof(Ag3)=FVAR(1)
 Sof(Ag2A)=1-FVAR(2)
 Sof(Ag2)=FVAR(2)
 Sof(N5A)=Sof(C38A)=Sof(H38D)=Sof(H38E)=Sof(H38F)=Sof(C37A)=1-FVAR(3)
 Sof(C37)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(H38C)=Sof(N5)=FVAR(3)
6.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C29(H29A,H29B), C23(H23A,H23B), C11(H11A,H11B), C22(H22A,H22B),
 C25(H25A,H25B), C5(H5A,H5B), C6(H6A,H6B), C24(H24A,H24B), C4(H4A,H4B),
 C18(H18A,H18B), C36(H36A,H36B)
6.b Aromatic/amide H refined with riding coordinates:
 C21(H21), C13(H13), C10(H10), C28(H28), C31(H31), C19(H19), C34(H34), C9(H9),
 C20(H20), C8(H8), C33(H33), C32(H32), C27(H27), C26(H26), C16(H16), C15(H15),
 C14(H14), C2(H2), C3(H3), C1(H1)
6.c Idealised Me refined as rotating group:
 C38(H38A,H38B,H38C), C38A(H38D,H38E,H38F)
;
_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 1.126
_oxdiff_exptl_absorpt_empirical_full_min 0.909
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2
_twin_special_details
;
Component 2 rotated by -179.9804\% 
 around [0.00 1.00 -0.00] (reciprocal) or [-0.23 0.95 -0.22] (direct)
;