meso-Bis(ethynyl) Versus meso-Bis(aryl) Calix[4]pyrroles: Dimensionally Well-Modulated Receptors That Can Regulate the Anion Binding Domains.
Dutta, Ranjan; Samala, Srinivas; Jo, Hongil; Ok, Kang Min; Lee, Chang-Hee; The Journal of organic chemistry 84 (2019) 6851–6857; doi:10.1021/acs.joc.9b00639

data_4034630
_publ_section_title
;
 meso-Bis(ethynyl) Versus meso-Bis(aryl) Calix[4]pyrroles: Dimensionally
 Well-Modulated Receptors That Can Regulate the Anion Binding Domains.
;
_journal_issue                   11
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              6851
_journal_page_last               6857
_journal_paper_doi               10.1021/acs.joc.9b00639
_journal_volume                  84
_journal_year                    2019
_chemical_formula_moiety         'C30 H32 N4, C H2 Cl2'
_chemical_formula_sum            'C31 H34 Cl2 N4'
_chemical_formula_weight         533.52
_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   mixed
_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      2.4.5
_audit_creation_date             2018-09-07T10:40:18-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                71.411(2)
_cell_angle_beta                 82.811(3)
_cell_angle_gamma                60.942(2)
_cell_formula_units_Z            2
_cell_length_a                   10.3734(5)
_cell_length_b                   10.4862(5)
_cell_length_c                   16.0455(7)
_cell_measurement_reflns_used    48
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.31
_cell_measurement_theta_min      5.26
_cell_measurement_wavelength     0.71073
_cell_volume                     1445.17(12)
_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-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-2013/2 (Sheldrick, 2013)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector                 'APEX-II CCD'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.976
_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      0.085457
_diffrn_orient_matrix_UB_12      0.018509
_diffrn_orient_matrix_UB_13      0.000943
_diffrn_orient_matrix_UB_21      0.067336
_diffrn_orient_matrix_UB_22      -0.097626
_diffrn_orient_matrix_UB_23      -0.013761
_diffrn_orient_matrix_UB_31      -0.017173
_diffrn_orient_matrix_UB_32      0.055887
_diffrn_orient_matrix_UB_33      -0.064272
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_unetI/netI     0.0455
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            23926
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.445
_diffrn_reflns_theta_min         2.247
_diffrn_source                   'sealed x-ray tube'
_exptl_absorpt_coefficient_mu    0.251
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6121
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        SADABS-2014/2 - Bruker AXS area detector scaling and absorption correcti
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.226
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             564
_exptl_crystal_size_max          0.492
_exptl_crystal_size_mid          0.244
_exptl_crystal_size_min          0.221
_refine_diff_density_max         0.415
_refine_diff_density_min         -0.413
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     356
_refine_ls_number_reflns         7104
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0962
_refine_ls_R_factor_gt           0.0572
_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^)+(0.0436P)^2^+0.6894P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1194
_refine_ls_wR_factor_ref         0.1393
_reflns_Friedel_coverage         0
_reflns_number_gt                4548
_reflns_number_total             7104
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo9b00639_si_003.cif
_cod_data_source_block           shelx
_cod_database_code               4034630
_shelx_estimated_absorpt_t_min   0.887
_shelx_estimated_absorpt_t_max   0.947
_shelx_shelxl_version_number     2018/3