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_7244731
_publ_section_title
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 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_formula_moiety         '2(Cl), C52 H42 N14, C H4 O'
_chemical_formula_sum            'C53 H46 Cl2 N14 O'
_chemical_formula_weight         965.94
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-09-20
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-12-22 deposited with the CCDC.	2022-03-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.77(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.9910(14)
_cell_length_b                   24.531(5)
_cell_length_c                   30.593(6)
_cell_measurement_reflns_used    3443
_cell_measurement_temperature    100
_cell_measurement_theta_max      20.824
_cell_measurement_theta_min      1.064
_cell_volume                     5240.5(18)
_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_temperature      100
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'MX2 beamline at the Australian Synchrotron'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1549
_diffrn_reflns_av_unetI/netI     0.0828
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            35769
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        20.824
_diffrn_reflns_theta_max         20.824
_diffrn_reflns_theta_min         1.064
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.176
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.224
_exptl_crystal_description       needle
_exptl_crystal_F_000             2016
_exptl_crystal_preparation       Synthesised
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Methanol/diethyl ether'
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.331
_refine_diff_density_min         -0.290
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     633
_refine_ls_number_reflns         5426
_refine_ls_number_restraints     63
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1210
_refine_ls_R_factor_gt           0.0814
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1671P)^2^+1.1610P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2245
_refine_ls_wR_factor_ref         0.2577
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3443
_reflns_number_total             5426
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00273f2.cif
_cod_data_source_block           7H_2Cl
_cod_original_cell_volume        5240.4(18)
_cod_database_code               7244731
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.998
_shelx_estimated_absorpt_t_min   0.979
_olex2_refinement_description
;
1. 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, All O(H) groups
2. Restrained distances
 C33-C34
 1.39 with sigma of 0.02
 C34-C35
 1.39 with sigma of 0.02
 N11-C43
 1.35 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C21 \\sim C20 \\sim C19 \\sim C22 \\sim C23 \\sim C18: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
C34 \\sim C33 \\sim C32 \\sim C31 \\sim C30: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
4.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C36(H36A,H36B), C46(H46A,H46B), C17(H17A,H17B)
4.b Aromatic/amide H refined with riding coordinates:
 C28(H28), C29(H29), C39(H39), C25(H25), C26(H26), C13(H13), C43(H43),
 C10(H10), C12(H12), C8(H8), C41(H41), C16(H16), C45(H45), C37(H37), C34(H34),
 C5(H5), C51(H51), C1(H1), C3(H3), C2(H2), C50(H50), C52(H52), C4(H4), C33(H33),
  C21(H21), C48(H48), C19(H19), C49(H49), C23(H23), C30(H30), C32(H32),
 C22(H22), C20(H20), C31(H31)
4.c Idealised Me refined as rotating group:
 C53(H53A,H53B,H53C)
4.d Idealised tetrahedral OH refined as rotating group:
 O1(H1A)
;
_shelx_res_checksum              28657
_shelx_hkl_checksum              8048
_shelx_fab_checksum              8307
_olex2_submission_special_instructions 'No special instructions were received'