C–H hydrogen bond and halogen bond directed self-assembly of ethereal podands and C–X⋯F−/HF2− halogen bonding in solution
Dutta, Dipjyoti; Gogoi, Anamika; Dutta, Rupjyoti; Harmalkar, Sarvesh S.; Lama, Prem; Dey, Sandeep Kumar; CrystEngComm 25 (2023) 5650–5659; doi:10.1039/D3CE00599B

data_7247316
_publ_section_title
;
 C--H hydrogen bond and halogen bond directed self-assembly of ethereal
 podands and C--X&#x22EF;F&#x2212;/HF2&#x2212; halogen bonding in solution
;
_journal_issue                   40
_journal_name_full               CrystEngComm
_journal_page_first              5650
_journal_page_last               5659
_journal_paper_doi               10.1039/D3CE00599B
_journal_volume                  25
_journal_year                    2023
_chemical_formula_sum            'C33 H27 N3 O3'
_chemical_formula_weight         513.57
_chemical_melting_point          573
_chemical_name_systematic        1,3,5-tris(4-cyano-phenoxymethyl)mesitylene
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/2
_audit_update_record
;
2023-06-09 deposited with the CCDC.	2023-09-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 119.415(11)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   30.916(10)
_cell_length_b                   8.682(3)
_cell_length_c                   25.527(8)
_cell_measurement_reflns_used    4985
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      23.15
_cell_measurement_theta_min      2.46
_cell_volume                     5968(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-III detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0776
_diffrn_reflns_av_unetI/netI     0.0617
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            24223
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.465
_exptl_absorpt_coefficient_mu    0.074
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.143
_exptl_crystal_description       block
_exptl_crystal_F_000             2160
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetone acetonitrile'
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.210
_exptl_transmission_factor_max   0.7453
_exptl_transmission_factor_min   0.6011
_refine_diff_density_max         0.299
_refine_diff_density_min         -0.232
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     364
_refine_ls_number_reflns         5245
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.1527
_refine_ls_R_factor_gt           0.0999
_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^)+(0.0899P)^2^+11.2321P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2278
_refine_ls_wR_factor_ref         0.2567
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3224
_reflns_number_total             5245
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00599b2.cif
_cod_data_source_block           POD_CN
_cod_depositor_comments
'Adding full bibliography for 7247314--7247317.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7247316
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_min   0.982
_shelx_estimated_absorpt_t_max   0.985
_shelx_res_checksum              63822
_shelx_fab_checksum              60219