Towards hydrogen and halogen bonded frameworks based on 3,5-bis(triazolyl)pyridinium motifs
Foyle, Émer M.; Tay, Hui Min; White, Nicholas G.; CrystEngComm  (2022) –; doi:10.1039/D2CE00273F

data_7244729
_publ_section_title
;
 Towards hydrogen and halogen bonded frameworks based on
 3,5-bis(triazolyl)pyridinium motifs
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00273F
_journal_year                    2022
_chemical_absolute_configuration ad
_chemical_compound_source        synthesized
_chemical_formula_moiety         'C23 H19 N7'
_chemical_formula_sum            'C23 H19 N7'
_chemical_formula_weight         393.45
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_update_record
;
2021-12-22 deposited with the CCDC.	2022-03-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.4367(18)
_cell_length_b                   4.3516(2)
_cell_length_c                   28.1754(15)
_cell_measurement_reflns_used    2250
_cell_measurement_temperature    150
_cell_measurement_theta_max      72.01
_cell_measurement_theta_min      5.13
_cell_volume                     4222.2(4)
_computing_cell_refinement       'CrysAlisPro, (Agilent, 2011)'
_computing_data_collection       'CrysAlisPro, (Agilent, 2011'
_computing_data_reduction        'CrysAlisPro, (Agilent, 2011)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction Supernova'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.052
_diffrn_reflns_av_unetI/netI     0.068
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            13159
_diffrn_reflns_theta_full        66.443
_diffrn_reflns_theta_max         65.211
_diffrn_reflns_theta_min         5.138
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.624
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.72
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlisPro, (Agilent, 2011)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.238
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1648
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Water/methanol'
_exptl_crystal_size_max          0.87
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.42
_refine_diff_density_min         -0.37
_refine_ls_abs_structure_details
; 
 Parsons, Flack & Wagner (2013), 
 1915 Friedel Pairs 
;
_refine_ls_abs_structure_Flack   0.61(15)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     542
_refine_ls_number_reflns         6204
_refine_ls_number_restraints     147
_refine_ls_R_factor_all          0.0999
_refine_ls_R_factor_gt           0.0844
_refine_ls_shift/su_max          0.0004211
_refine_ls_shift/su_mean         0.0000355
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.14P)^2^ + 3.10P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2416
_refine_ls_wR_factor_gt          0.2219
_refine_ls_wR_factor_ref         0.2410
_reflns_limit_h_max              40
_reflns_limit_h_min              0
_reflns_limit_k_max              5
_reflns_limit_k_min              0
_reflns_limit_l_max              33
_reflns_limit_l_min              -33
_reflns_number_gt                4876
_reflns_number_total             6614
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.75
_oxford_diffrn_Wilson_scale      7.91
_oxford_refine_ls_scale          0.3747(10)
_cod_data_source_file            d2ce00273f2.cif
_cod_data_source_block           1H_Bn
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_sg_symbol_H-M      'P c a 21 '
_cod_database_code               7244729
_oxford_refine_reflns_threshold_expression I>-3.0\s(I)
_refine_ls_r_factor_ref          0.0998
_reflns_number_all               6206
_oxford_hooft_y                  0.7(2)
_oxford_bijvoet_difference       0.61(15)
_oxford_refined_flack_x          0.9(7)
_platon_squeeze_void_probe_radius 1.20