Unexpected halide anion binding modes in meso-bis-ethynyl picket-calix[4]pyrroles: effects of meso-π (ethynyl) extension.
Dutta, Ranjan; Firmansyah, Dikhi; Kim, Jihoon; Jo, Hongil; Ok, Kang Min; Lee, Chang-Hee; Chemical communications (Cambridge, England) 54 (2018) 7936–7939; doi:10.1039/c8cc04393k

data_7121862
_publ_section_title
;
 Unexpected halide anion binding modes in meso-bis-ethynyl
 picket-calix[4]pyrroles: effects of meso-\p (ethynyl) extension.
;
_journal_issue                   57
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              7936
_journal_page_last               7939
_journal_paper_doi               10.1039/c8cc04393k
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety
'C42 H38 F2 N4, C16 H36 N, C2 H3 N, F, 0.294(O)'
_chemical_formula_sum            'C60 H77 F3 N6 O0.29'
_chemical_formula_weight         943.98
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_creation_date             2018-05-29T14:19:00-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2018-06-01 deposited with the CCDC.
2018-06-21 downloaded from the CCDC.
;
_cell_angle_alpha                80.990(3)
_cell_angle_beta                 73.141(3)
_cell_angle_gamma                82.786(4)
_cell_formula_units_Z            2
_cell_length_a                   11.5785(7)
_cell_length_b                   13.3678(9)
_cell_length_c                   19.1989(10)
_cell_measurement_reflns_used    8501
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      27.89
_cell_measurement_theta_min      2.3
_cell_measurement_wavelength     0.71073
_cell_volume                     2798.7(3)
_computing_cell_refinement       'SAINT V8.34A integration software'
_computing_data_collection       'Bruker APEX2 software'
_computing_data_reduction        'Bruker APEX2 software'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      203(2)
_diffrn_detector                 'APEX-II CCD'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       '\f or \w oscillation scans'
_diffrn_orient_matrix_type       'x-axis to radiation source'
_diffrn_orient_matrix_UB_11      0.038184
_diffrn_orient_matrix_UB_12      -0.03355
_diffrn_orient_matrix_UB_13      0.039181
_diffrn_orient_matrix_UB_21      -0.001076
_diffrn_orient_matrix_UB_22      0.067557
_diffrn_orient_matrix_UB_23      0.016429
_diffrn_orient_matrix_UB_31      -0.082134
_diffrn_orient_matrix_UB_32      -0.009337
_diffrn_orient_matrix_UB_33      0.034656
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0759
_diffrn_reflns_av_unetI/netI     0.0685
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.99
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            35518
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.99
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.121
_diffrn_reflns_theta_min         2.233
_diffrn_source                   'sealed x-ray tube'
_exptl_absorpt_coefficient_mu    0.073
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.658
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.119
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1016.7
_exptl_crystal_size_max          0.661
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.333
_refine_diff_density_max         0.31
_refine_diff_density_min         -0.237
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     643
_refine_ls_number_reflns         12241
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0942
_refine_ls_R_factor_gt           0.0522
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0656P)^2^+0.1909P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1287
_refine_ls_wR_factor_ref         0.1497
_reflns_Friedel_coverage         0
_reflns_number_gt                7453
_reflns_number_total             12241
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc04393k2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7121861--7121863.cif.'
_cod_database_code               7121862
_shelx_estimated_absorpt_t_min   0.953
_shelx_estimated_absorpt_t_max   0.976