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

data_7240173
_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, 1.5(Br), 1.5(F6 P)'
_chemical_formula_sum            'C42 H57 Br1.5 F9 I3 N3 O3 P1.5'
_chemical_formula_weight         1369.95
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_symmetry_Int_Tables_number      13
_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                 101.26(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.671(5)
_cell_length_b                   8.8760(18)
_cell_length_c                   23.946(5)
_cell_measurement_reflns_used    65940
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.12
_cell_measurement_theta_min      0.84
_cell_volume                     5142.8(19)
_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 0.7958
_diffrn_measured_fraction_theta_max 0.7958
_diffrn_measurement_device_type  'MX1 beamline at the Australian Synchrotron'
_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  0.1756
_diffrn_reflns_av_unetI/netI     0.1089
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            65940
_diffrn_reflns_theta_full        29.1234
_diffrn_reflns_theta_max         29.12
_diffrn_reflns_theta_min         0.84
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.107
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.7692
_exptl_crystal_description       needle
_exptl_crystal_F_000             2671.4284
_exptl_crystal_recrystallization_method
'Disslove receptor in methanol with  1.5 eq of TBA.Br. Diffuse diethyl ether into the soltion.'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         3.6855
_refine_diff_density_min         -1.6341
_refine_diff_density_rms         0.3473
_refine_ls_d_res_high            0.7302
_refine_ls_d_res_low             24.1961
_refine_ls_goodness_of_fit_ref   1.0269
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    90
_refine_ls_number_parameters     571
_refine_ls_number_reflns         11004
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.0246
_refine_ls_R_factor_all          0.1829
_refine_ls_R_factor_gt           0.0812
_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^)+(0.1426P)^2^+1.2357P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2165
_refine_ls_wR_factor_ref         0.2833
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              29
_reflns_limit_h_min              -30
_reflns_limit_k_max              10
_reflns_limit_k_min              0
_reflns_limit_l_max              29
_reflns_limit_l_min              0
_reflns_number_gt                4936
_reflns_number_total             11004
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d0ce00241k2.cif
_cod_data_source_block           EMF458E_0149
_cod_database_code               7240173
_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. Restrained distances
 C23-C24
 1.53 with sigma of 0.01
 C24-C25
 1.53 with sigma of 0.01
 C25-C26
 1.53 with sigma of 0.01
 C26-C27
 1.53 with sigma of 0.01
 C27-C28
 1.53 with sigma of 0.01
 C23-C25
 2.55 with sigma of 0.02
 C24-C26
 2.55 with sigma of 0.02
 C25-C27
 2.55 with sigma of 0.02
 C26-C28
 2.55 with sigma of 0.02
3. Rigid bond restraints
 C23, C24, C25, C26, C27, C28
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4. Uiso/Uaniso restraints and constraints
C23 \\sim C24 \\sim C25 \\sim C26 \\sim C27 \\sim C28: within 1.7A with sigma
of 0.02 and sigma for terminal atoms of 0.04
5.a Secondary CH2 refined with riding coordinates:
 C10(H10a,H10b), C9(H9a,H9b), C37(H37a,H37b), C11(H11a,H11b), C30(H30a,H30b),
 C16(H16a,H16b), C6(H6a,H6b), C38(H38a,H38b), C13(H13a,H13b), C12(H12a,H12b),
 C23(H23a,H23b), C24(H24a,H24b), C41(H41a,H41b), C39(H39a,H39b), C40(H40a,H40b),
  C25(H25a,H25b), C27(H27a,H27b), C26(H26a,H26b)
5.b Me refined with riding coordinates:
 C28(H28a,H28b,H28c)
5.c Aromatic/amide H refined with riding coordinates:
 C31(H31), C5(H5), C17(H17), C35(H35), C21(H21), C3(H3), C1(H1), C34(H34),
 C33(H33), C4(H4), C20(H20), C19(H19)
5.d Idealised Me refined as rotating group:
 C14(H14a,H14b,H14c), C42(H42a,H42b,H42c)
;
_olex2_submission_original_sample_id 'EMF-4-58 E'
_olex2_submission_special_instructions 'No special instructions were received'