Tripodal halogen bonding iodo-azolium receptors for anion recognition
Ruiz-Botella, Sheila; Vidossich, Pietro; Ujaque, Gregori; Peris, Eduardo; Beer, Paul D.; RSC Adv. 7 (2017) 11253–; doi:10.1039/C6RA28082J

data_7227682
_publ_section_title
;
 Tripodal halogen bonding iodo-azolium receptors for anion recognition
;
_journal_issue                   19
_journal_name_full               'RSC Adv.'
_journal_page_first              11253
_journal_paper_doi               10.1039/C6RA28082J
_journal_volume                  7
_journal_year                    2017
_chemical_formula_moiety
'2(C21 H22 I3 N6), 3(C H Cl3), 4(B F4), 2(Cl)'
_chemical_formula_sum            'C45 H47 B4 Cl11 F16 I6 N12'
_chemical_formula_weight         2254.53
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2017-01-18
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2017-01-18 deposited with the CCDC.
2017-01-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.6312(2)
_cell_length_b                   23.5061(4)
_cell_length_c                   24.2909(4)
_cell_measurement_reflns_used    27477
_cell_measurement_temperature    200.00(14)
_cell_measurement_theta_max      28.2550
_cell_measurement_theta_min      3.3910
_cell_volume                     7783.2(2)
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      200.00(14)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_unetI/netI     0.0236
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            77836
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.916
_diffrn_reflns_theta_min         2.837
_exptl_absorpt_coefficient_mu    2.851
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76376
_exptl_absorpt_correction_type   gaussian
_exptl_crystal_colour            'clear whiteish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.924
_exptl_crystal_description       prism
_exptl_crystal_F_000             4280
_exptl_crystal_preparation       'slow evaporation'
_exptl_crystal_size_max          24.2909
_exptl_crystal_size_mid          23.5061
_exptl_crystal_size_min          13.6312
_refine_diff_density_max         1.679
_refine_diff_density_min         -0.922
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     481
_refine_ls_number_reflns         9735
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0596
_refine_ls_R_factor_gt           0.0408
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0504P)^2^+27.7610P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1060
_refine_ls_wR_factor_ref         0.1209
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7597
_reflns_number_total             9735
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ra28082j2.cif
_cod_data_source_block           ov_str1867
_cod_database_code               7227682
_shelx_shelxl_version_number     2016/4
_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: Cl2(0.5) Cl4(0.5) C23(0.5) H23(0.5) F7(0.5) F8(0.5) F1(0.5)
 F5(0.5) F3(0.5) F6(0.5) F4(0.5) F2(0.5) Cl3(0.5)
3.a Rotating group:
 C9(H9A,H9B)
3.b Ternary CH refined with riding coordinates:
 C22(H22), C23(H23)
3.c Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C10(H10A,H10B), C15(H15A,H15B)
3.d Aromatic/amide H refined with riding coordinates:
 C21(H21), C17(H17), C19(H19), C2(H2), C8(H8), C3(H3), C7(H7), C13(H13)
3.e Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C4(H4A,H4B,H4C)
;
_shelx_res_checksum              97677
_olex2_submission_special_instructions 'No special instructions were received'