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_7121863
_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, 2(C2 H3 N)'
_chemical_formula_sum            'C46 H46 N6'
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_space_group_name_H-M_alt        'P 1 21/c 1'
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_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
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_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                 114.23(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.270(2)
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_cell_length_c                   12.708(3)
_cell_measurement_reflns_used    19788
_cell_measurement_temperature    100(2)
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_cell_measurement_wavelength     0.7
_cell_volume                     1938.7(8)
_computing_cell_refinement       'HKL3000sm (Otwinowski & Miinor, 1997)'
_computing_data_collection       'PAL BL2D-SMDC program (Shin et. al, 2016)'
_computing_data_reduction        'HKL3000sm (Otwinowski & Miinor, 1997)'
_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 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
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_diffrn_measured_fraction_theta_max 0.678
_diffrn_measurement_device_type  'ADSC Q210 CCD area detector'
_diffrn_measurement_method       '\w scan'
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_diffrn_radiation_source         'PLSII 2D bending magnet'
_diffrn_radiation_type           synchrotron
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_diffrn_reflns_av_R_equivalents  0.0582
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_diffrn_reflns_Laue_measured_fraction_full 0.926
_diffrn_reflns_Laue_measured_fraction_max 0.678
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
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_diffrn_reflns_point_group_measured_fraction_full 0.926
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_exptl_absorpt_process_details
; 
 HKL3000sm Scalepack (Otwinowski & Minor, 1997)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.17
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.218
_exptl_crystal_size_mid          0.081
_exptl_crystal_size_min          0.011
_refine_diff_density_max         0.393
_refine_diff_density_min         -0.368
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_refine_ls_extinction_coef       0.101(6)
_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   0.952
_refine_ls_hydrogen_treatment    refall
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_refine_ls_number_constraints    0
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_refine_ls_number_reflns         5214
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.952
_refine_ls_R_factor_all          0.0998
_refine_ls_R_factor_gt           0.0531
_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^)+(0.0897P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1269
_refine_ls_wR_factor_ref         0.1483
_reflns_Friedel_coverage         0
_reflns_number_gt                3163
_reflns_number_total             5214
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc04393k2.cif
_cod_data_source_block           C42H40N4_2(CH3CN)
_cod_depositor_comments
'Adding full bibliography for 7121861--7121863.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7121863
_shelx_estimated_absorpt_t_min   0.986
_shelx_estimated_absorpt_t_max   0.999