Novel hydrogen- and halogen-bonding anion receptors based on 3-iodopyridinium units
Amendola, Valeria; Bergamaschi, Greta; Boiocchi, Massimo; Fusco, Nadia; La Rocca, Mario Vincenzo; Linati, Laura; Lo Presti, Eliana; Mella, Massimo; Metrangolo, Pierangelo; Miljkovic, Ana; RSC Adv.  (2016) –; doi:10.1039/C6RA14703H

data_7225894
_publ_section_title
;
 Novel hydrogen- and halogen-bonding anion receptors based on
 3-iodopyridinium units
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C6RA14703H
_journal_year                    2016
_chemical_formula_moiety         'C27 H27 I3 N3, F6 P, 2(N O3)'
_chemical_formula_sum            'C27 H27 F6 I3 N5 O6 P'
_chemical_formula_weight         1043.21
_chemical_name_systematic
;
1,3,5-tris(3-iodo-1-pyridiniomethyl)-2,4,6-trimethylbenzene nitrate
 hexafluorophosphate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-04-26 deposited with the CCDC.
2016-07-11 downloaded from the CCDC.
;
_cell_angle_alpha                118.339(4)
_cell_angle_beta                 101.442(4)
_cell_angle_gamma                99.631(4)
_cell_formula_units_Z            2
_cell_length_a                   11.352(2)
_cell_length_b                   13.844(3)
_cell_length_c                   14.366(3)
_cell_measurement_reflns_used    5210
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     1856.0(7)
_computing_cell_refinement       'SAINT (Bruker-Axs Inc)'
_computing_data_collection       'SMART (Bruker-Axs Inc)'
_computing_data_reduction        'SAINT (Bruker-Axs Inc)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2008)'
_computing_structure_solution    'SIR-97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker-Axs Smart-Apex CCD'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_av_unetI/netI     0.0415
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19857
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.223
_diffrn_reflns_theta_max         25.223
_diffrn_reflns_theta_min         1.683
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    2.643
_exptl_absorpt_correction_T_max  0.982
_exptl_absorpt_correction_T_min  0.605
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.867
_exptl_crystal_description       prism
_exptl_crystal_F_000             1000
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.605
_refine_diff_density_min         -1.139
_refine_diff_density_rms         0.184
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         6663
_refine_ls_number_restraints     122
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0926
_refine_ls_R_factor_gt           0.0730
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1514P)^2^+4.9621P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2343
_refine_ls_wR_factor_ref         0.2561
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4891
_reflns_number_total             6663
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ra14703h2.cif
_cod_data_source_block           2_NO3_PF6
_cod_database_code               7225894
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              46181
_solvent_exptl_crystal_recrystallization_method acetonitrile