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_7121861
_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 H40 N4'
_chemical_formula_sum            'C42 H40 N4'
_chemical_formula_weight         600.78
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      148
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2017-12-15T21:11:57-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2018-03-02 deposited with the CCDC.
2018-06-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   26.1757(5)
_cell_length_b                   26.1757(5)
_cell_length_c                   31.6025(9)
_cell_measurement_reflns_used    4635
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      28.1
_cell_measurement_theta_min      2.21
_cell_measurement_wavelength     0.71073
_cell_volume                     18752.0(7)
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2008)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.188
_diffrn_reflns_av_unetI/netI     0.1253
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 1
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            61985
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 1
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.385
_diffrn_reflns_theta_min         1.105
_exptl_absorpt_coefficient_mu    0.056
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6621
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS(Blessing, 1995) 
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    0.958
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5760
_exptl_crystal_size_max          0.312
_exptl_crystal_size_mid          0.265
_exptl_crystal_size_min          0.195
_platon_squeeze_details
;
TITL shelx     R -3 :h      R = 0.13
CELL   26.1757   26.1757   31.6025     90.00     90.00    120.00
SPGR R-3
C101 1.000 0.998 0.609 !       1.26 eA-3
C102 0.446 0.578 0.094 !       1.15 eA-3
C103 0.554 0.759 0.236 !       1.13 eA-3
C104 0.781 0.253 0.755 !       1.10 eA-3
C105 0.548 0.095 0.883 !       1.08 eA-3
C106 0.039 0.874 0.501 !       1.08 eA-3
C107 0.328 0.622 0.274 !       1.06 eA-3
C108 0.260 0.516 0.226 !       1.06 eA-3
C109 0.967 0.962 0.593 !       1.05 eA-3
C110 0.290 0.626 0.233 !       1.04 eA-3
C111 0.945 0.133 0.562 !       1.03 eA-3
C112 0.822 0.219 0.767 !       1.03 eA-3
C113 0.639 0.327 0.953 !       1.02 eA-3
C114 0.521 0.766 0.212 !       1.00 eA-3
C115 0.811 0.882 0.377 !       0.99 eA-3
C116 0.073 0.232 0.436 !       0.98 eA-3
C117 0.828 0.438 0.912 !       0.98 eA-3
C118 0.109 0.850 0.439 !       0.98 eA-3
C119 0.811 0.902 0.455 !       0.98 eA-3
C120 0.899 0.764 0.585 !       0.98 eA-3
C121 0.960 0.960 0.625 !       0.97 eA-3
C122 0.839 0.987 0.451 !       0.96 eA-3
C123 0.329 0.702 0.087 !       0.96 eA-3
C124 0.251 0.640 0.099 !       0.95 eA-3
C125 0.268 0.640 0.256 !       0.94 eA-3
C126 0.099 0.114 0.398 !       0.93 eA-3
C127 0.174 0.459 0.223 !       0.93 eA-3
C128 0.537 0.739 0.259 !       0.93 eA-3
C129 0.266 0.784 0.197 !       0.93 eA-3
C130 0.271 0.767 0.252 !       0.93 eA-3
C131 0.953 0.821 0.546 !       0.93 eA-3
C132 0.139 0.219 0.462 !       0.93 eA-3
C133 0.046 0.940 0.383 !       0.92 eA-3
C134 0.009 0.937 0.399 !       0.91 eA-3
C135 0.991 0.063 0.601 !       0.91 eA-3
C136 0.273 0.523 0.303 !       0.91 eA-3
C137 0.337 0.589 0.039 !       0.91 eA-3
C138 0.336 0.500 0.157 !       0.90 eA-3
C139 0.892 0.991 0.514 !       0.90 eA-3
C140 0.056 0.116 0.421 !       0.89 eA-3
C141 0.253 0.467 0.274 !       0.89 eA-3
C142 0.594 0.290 0.751 !       0.89 eA-3
C143 0.605 0.188 0.965 !       0.87 eA-3
C144 1.000 1.005 0.577 !       0.86 eA-3
C145 0.287 0.766 0.209 !       0.86 eA-3
C146 0.640 0.203 0.865 !       0.86 eA-3
C147 0.672 0.407 0.906 !       0.85 eA-3
C148 0.304 0.553 0.291 !       0.85 eA-3
C149 0.936 0.100 0.618 !       0.84 eA-3
C150 0.861 0.154 0.562 !       0.84 eA-3
C151 0.427 0.674 0.213 !       0.84 eA-3
C152 0.220 0.437 0.274 !       0.84 eA-3
C153 0.414 0.655 0.078 !       0.83 eA-3
C154 0.320 0.602 0.133 !       0.83 eA-3
C155 0.422 0.258 0.788 !       0.83 eA-3
C156 0.917 0.008 0.585 !       0.82 eA-3
C157 0.396 0.624 0.158 !       0.80 eA-3
C158 0.734 0.381 0.971 !       0.80 eA-3
C159 0.748 0.484 0.729 !       0.80 eA-3
C160 0.360 0.695 0.217 !       0.79 eA-3
Q161 0.538 0.093 0.766 !       0.79 eA-3
C162 0.259 0.748 0.186 !       0.78 eA-3
C163 0.080 0.232 0.467 !       0.78 eA-3
C164 0.258 0.703 0.236 !       0.77 eA-3
C165 0.194 0.718 0.251 !       0.77 eA-3
C166 0.920 0.937 0.446 !       0.77 eA-3
C167 0.345 0.734 0.173 !       0.76 eA-3
C168 0.167 0.427 0.234 !       0.75 eA-3
C169 0.302 0.796 0.276 !       0.75 eA-3
C170 0.525 0.359 0.810 !       0.75 eA-3
C171 0.088 0.126 0.493 !       0.75 eA-3
C172 0.912 0.874 0.507 !       0.75 eA-3
C173 0.671 0.258 0.937 !       0.74 eA-3
Q174 0.264 0.344 0.813 !       0.74 eA-3
C175 0.593 0.305 0.812 !       0.74 eA-3
Q176 0.445 0.501 0.143 !       0.74 eA-3
C177 0.414 0.626 0.195 !       0.74 eA-3
C178 0.367 0.620 0.210 !       0.73 eA-3
C179 0.204 0.117 0.521 !       0.73 eA-3
C180 0.384 0.751 0.211 !       0.73 eA-3
C181 0.187 0.664 0.188 !       0.73 eA-3
C182 0.279 0.729 0.205 !       0.72 eA-3
C183 0.476 0.813 0.187 !       0.72 eA-3
C184 0.920 0.970 0.548 !       0.72 eA-3
C185 0.776 0.928 0.482 !       0.72 eA-3
C186 0.822 0.791 0.522 !       0.72 eA-3
C187 0.122 0.032 0.578 !       0.72 eA-3
C188 0.999 0.172 0.577 !       0.72 eA-3
C189 0.117 0.139 0.477 !       0.72 eA-3
Q190 0.796 0.575 0.902 !       0.71 eA-3
Q191 0.014 0.186 0.752 !       0.71 eA-3
C192 0.189 0.037 0.590 !       0.70 eA-3
C193 0.713 0.406 0.884 !       0.69 eA-3
C194 0.079 0.133 0.522 !       0.69 eA-3
C195 0.844 0.885 0.389 !       0.68 eA-3
C196 0.422 0.694 0.148 !       0.68 eA-3
Q197 0.822 0.478 0.242 !       0.68 eA-3
C198 0.594 0.175 0.827 !       0.67 eA-3
C199 0.398 0.155 0.793 !       0.67 eA-3
;
_refine_diff_density_max         0.388
_refine_diff_density_min         -0.304
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       0.00060(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/1 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     416
_refine_ls_number_reflns         7673
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1929
_refine_ls_R_factor_gt           0.1056
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1572P)^2^+8.0400P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2558
_refine_ls_wR_factor_ref         0.3099
_reflns_Friedel_coverage         0
_reflns_number_gt                3686
_reflns_number_total             7673
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc04393k2.cif
_cod_data_source_block           C42H40N4
_cod_depositor_comments
'Adding full bibliography for 7121861--7121863.cif.'
_cod_original_cell_volume        18752.0(9)
_cod_database_code               7121861
_shelx_estimated_absorpt_t_min   0.983
_shelx_estimated_absorpt_t_max   0.989
_shelx_res_checksum              48349
_platon_squeeze_void_probe_radius 1.20
_shelx_fab_checksum              46972