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_4034631
_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         'C36 H48 N4 Si2, C3 H6 O'
_chemical_formula_sum            'C39 H54 N4 O Si2'
_chemical_formula_weight         651.04
_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
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
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_audit_creation_date             2018-06-14T16:49:52-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                69.53(3)
_cell_angle_beta                 87.69(3)
_cell_angle_gamma                81.67(3)
_cell_formula_units_Z            2
_cell_length_a                   10.509(2)
_cell_length_b                   14.050(3)
_cell_length_c                   14.974(3)
_cell_measurement_reflns_used    33336
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      33.548
_cell_measurement_theta_min      0.361
_cell_measurement_wavelength     0.63000
_cell_volume                     2049.3(8)
_computing_cell_refinement       'HKL3000sm (Otwinowski & Minor, 1997)'
_computing_data_collection       'PAL BL2D-SMDC Program (Shin et. al, 2016)'
_computing_data_reduction        'HKL3000sm (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Rayonix MX225HS CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.63000
_diffrn_reflns_av_R_equivalents  0.0383
_diffrn_reflns_av_unetI/netI     0.0446
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            32162
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        22.21
_diffrn_reflns_theta_max         29.999
_diffrn_reflns_theta_min         2.15
_diffrn_source                   'PLSII 2D bending magnet'
_exptl_absorpt_coefficient_mu    0.088
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.931
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'HKL3000sm Scalepack(Otwinowski et.al,2003)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.055
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             704
_exptl_crystal_size_max          0.926
_exptl_crystal_size_mid          0.356
_exptl_crystal_size_min          0.256
_refine_diff_density_max         0.624
_refine_diff_density_min         -0.45
_refine_diff_density_rms         0.123
_refine_ls_extinction_coef       0.230(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     446
_refine_ls_number_reflns         17087
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0816
_refine_ls_R_factor_gt           0.0710
_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^)+(0.1481P)^2^+0.0820P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2227
_refine_ls_wR_factor_ref         0.2346
_reflns_Friedel_coverage         0
_reflns_number_gt                13573
_reflns_number_total             17087
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo9b00639_si_002.cif
_cod_data_source_block           shelx
_cod_database_code               4034631
_shelx_estimated_absorpt_t_min   0.923
_shelx_estimated_absorpt_t_max   0.978