Anion templated crystal engineering of halogen bonding tripodal tris(halopyridinium) compounds
Foyle, Émer M.; White, Nicholas G.; CrystEngComm  (2020) –; doi:10.1039/D0CE00241K

data_7240171
_publ_section_title
;
 Anion templated crystal engineering of halogen bonding tripodal
 tris(halopyridinium) compounds
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE00241K
_journal_year                    2020
_chemical_formula_moiety         'C42 H57 I3 N3 O3, 3(Br), 0.33(C6 H9 N3)'
_chemical_formula_sum            'C44 H60 Br3 I3 N4 O3'
_chemical_formula_weight         1313.42
_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_Hall           '-P 3'
_space_group_name_H-M_alt        'P -3'
_symmetry_Int_Tables_number      147
_atom_sites_solution_primary     dual
_audit_creation_date             2020-01-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-02-18 deposited with the CCDC.	2020-03-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   16.639(2)
_cell_length_b                   16.639(2)
_cell_length_c                   10.570(2)
_cell_measurement_reflns_used    33692
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.21
_cell_measurement_theta_min      1.41
_cell_volume                     2534.3(6)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.8500
_diffrn_measured_fraction_theta_max 0.8500
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0654
_diffrn_reflns_av_unetI/netI     0.0257
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            33692
_diffrn_reflns_theta_full        29.2114
_diffrn_reflns_theta_max         29.21
_diffrn_reflns_theta_min         1.41
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.254
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.7210
_exptl_crystal_description       needle
_exptl_crystal_F_000             1276.3711
_exptl_crystal_recrystallization_method
'receptor dissolved in DMF:MeCN with 3 equiv of TBA.I. Then acetone was diffused into the solution'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.3287
_refine_diff_density_min         -1.3881
_refine_diff_density_rms         0.1508
_refine_ls_d_res_high            0.7282
_refine_ls_d_res_low             14.4101
_refine_ls_goodness_of_fit_ref   1.0414
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    34
_refine_ls_number_parameters     174
_refine_ls_number_reflns         3893
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0414
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0427
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0389P)^2^+14.3235P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1059
_refine_ls_wR_factor_ref         0.1070
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              19
_reflns_limit_h_min              0
_reflns_limit_k_max              19
_reflns_limit_k_min              0
_reflns_limit_l_max              13
_reflns_limit_l_min              -13
_reflns_number_gt                3710
_reflns_number_total             3893
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d0ce00241k2.cif
_cod_data_source_block           EMF4_86e
_cod_original_cell_volume        2534.4(7)
_cod_database_code               7240171
_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
2. Others
 Fixed Sof: H16a(0.33333) H16b(0.33333) H16c(0.33333) H16a(0.33333)
 H16b(0.33333) H16c(0.33333)
3.a Secondary CH2 refined with riding coordinates:
 C6(H6a,H6b), C9(H9a,H9b), C10(H10a,H10b), C11(H11a,H11b), C12(H12a,H12b),
 C13(H13a,H13b)
3.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C1(H1), C2(H2), C3(H3)
3.c Idealised Me refined as rotating group:
 C16(H16a,H16b,H16c), C14(H14a,H14b,H14c)
;
_olex2_submission_special_instructions 'No special instructions were received'