Synthesis of two tetra-azolium salts and the recognition performance for guests
Zhao, Zhi-Xiang; Hu, Lin-Hai; Yu, Shao-Cong; Liu, Qing-Xiang; New Journal of Chemistry 46 (2022) 22108–22116; doi:10.1039/D2NJ04255J

data_7062064
_publ_section_title
;
 Synthesis of two tetra-azolium salts and the recognition performance for
 guests
;
_journal_issue                   46
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              22108
_journal_page_last               22116
_journal_paper_doi               10.1039/D2NJ04255J
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety         'C62 H54 N12, 4(F6 P)'
_chemical_formula_sum            'C62 H54 F24 N12 P4'
_chemical_formula_weight         1547.05
_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
_audit_creation_date             2019-12-23
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2022-03-23 deposited with the CCDC.	2022-10-21 downloaded from the CCDC.
;
_cell_angle_alpha                74.284(5)
_cell_angle_beta                 69.199(5)
_cell_angle_gamma                79.296(4)
_cell_formula_units_Z            1
_cell_length_a                   11.7095(6)
_cell_length_b                   12.1400(6)
_cell_length_c                   12.8528(8)
_cell_measurement_reflns_used    4632
_cell_measurement_temperature    149.7(9)
_cell_measurement_theta_max      27.3830
_cell_measurement_theta_min      2.1340
_cell_volume                     1635.97(17)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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      149.7(9)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2740
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -15.00  77.00   1.00    7.49    --   11.16  57.00  30.00   92
  2  \w    -62.00  35.00   1.00    7.49    --   11.16 -57.00-120.00   97
  3  \w    -15.00  21.00   1.00    7.49    --  -11.24 -99.00 150.00   36
  4  \w    -78.00  -4.00   1.00    7.49    --  -11.24 -77.00 120.00   74
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0176546000
_diffrn_orient_matrix_UB_12      -0.0151246000
_diffrn_orient_matrix_UB_13      -0.0413030000
_diffrn_orient_matrix_UB_21      0.0624401000
_diffrn_orient_matrix_UB_22      -0.0054181000
_diffrn_orient_matrix_UB_23      -0.0344826000
_diffrn_orient_matrix_UB_31      0.0055051000
_diffrn_orient_matrix_UB_32      -0.0588448000
_diffrn_orient_matrix_UB_33      0.0277958000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0309
_diffrn_reflns_av_unetI/netI     0.0503
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11506
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.006
_diffrn_reflns_theta_max         25.006
_diffrn_reflns_theta_min         1.870
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.236
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80925
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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    1.570
_exptl_crystal_description       block
_exptl_crystal_F_000             786
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.819
_refine_diff_density_min         -0.483
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         5748
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0791
_refine_ls_R_factor_gt           0.0587
_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^)+(0.0750P)^2^+1.7330P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1489
_refine_ls_wR_factor_ref         0.1654
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4385
_reflns_number_total             5748
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj04255j2.cif
_cod_data_source_block           a191223a
_cod_depositor_comments          'Adding full bibliography for 7062064.cif.'
_cod_database_code               7062064
_reflns_odcompleteness_completeness 99.97
_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.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C14(H14A,H14B), C18(H18A,H18B), C26(H26A,H26B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C10(H10), C11(H11), C12(H12),
 C13(H13), C17(H17), C19(H19), C22(H22), C23(H23), C24(H24), C25(H25), C28(H28),
  C29(H29), C30(H30), C31(H31)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2019-12-23
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.360
_oxdiff_exptl_absorpt_empirical_full_min 0.780