Calix[6]arenes with halogen bond donor groups as selective and efficient anion transporters
Singh, Anurag; Torres-Huerta, Aaron; Vanderlinden, Tom; Renier, Nathan; Martínez-Crespo, Luis; Tumanov, Nikolay; Wouters, Johan; Bartik, Kristin; Jabin, Ivan; Valkenier, Hennie; Chemical Communications  (2022) –; doi:10.1039/D2CC00847E

data_7130065
_publ_section_title
;
 Calix[6]arenes with halogen bond donor groups as selective and efficient
 anion transporters
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC00847E
_journal_year                    2022
_chemical_formula_moiety
'C105 H108 F18 I3 N9 O6, 0.723(C H2 Cl2), 0.443(H2 O)'
_chemical_formula_sum            'C105.72 H109.11 Cl1.44 F18 I3 N9 O6.45'
_chemical_formula_weight         2382.62
_chemical_name_common
'5,11,17,23,29,35-hexa-t-butyl-37,39,41-trimethoxy-38,40,42-tris(2-(4-(3,5-bis(trifluoromethyl)phenyl)-5-iodo-1,2,3-triazolyl)ethoxy)calix(6)arenehydrate dichloromethane solvate'
_chemical_name_systematic
'1,1',1''-(((15,35,55,75,95,115-hexa-tert-butyl-32,72,112-trimethoxy-1,3,5,7,9,11(1,3)-hexabenzenacyclododecaphane-12,52,92-triyl)tris(oxy))tris(ethane-2,1-diyl))tris(4-(3,5-bis(trifluoromethyl)phenyl)-5-iodo-1H-1,2,3-triazole) hydrate dichloromethane solvate'
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-12-14 deposited with the CCDC.	2022-04-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            12
_cell_length_a                   23.1570(3)
_cell_length_b                   23.1570(3)
_cell_length_c                   68.8908(12)
_cell_measurement_reflns_used    12016
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      66.0360
_cell_measurement_theta_min      3.3770
_cell_volume                     31993.1(8)
_computing_cell_refinement       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 10.3712
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type
;
Oxford Diffraction Xcalibur Gemini Ultra R
;
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       81
_diffrn_reflns_limit_l_min       -69
_diffrn_reflns_number            39791
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.140
_diffrn_reflns_theta_max         67.140
_diffrn_reflns_theta_min         2.549
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    7.995
_exptl_absorpt_correction_T_max  0.357
_exptl_absorpt_correction_T_min  0.197
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_description       block
_exptl_crystal_F_000             14442
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.220
_refine_diff_density_max         0.746
_refine_diff_density_min         -0.864
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     840
_refine_ls_number_reflns         6343
_refine_ls_number_restraints     780
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0758
_refine_ls_R_factor_gt           0.0724
_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^)+(0.0547P)^2^+311.8214P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1766
_refine_ls_wR_factor_ref         0.1786
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5880
_reflns_number_total             6343
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc00847e2.cif
_cod_data_source_block           nt0945_AS32_DCM-MeOH
_cod_original_cell_volume        31993.0(10)
_cod_database_code               7130065
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.166
_shelx_estimated_absorpt_t_max   0.272
_shelx_res_checksum              30520
_shelx_hkl_checksum              99216