Anion Binding Modes in meso-Substituted Hexapyrrolic Calix[4]pyrrole Isomers.
Chang, Kai-Chi; Minami, Tsuyoshi; Koutnik, Petr; Savechenkov, Pavel Y.; Liu, Yuanli; Anzenbacher, Jr, Pavel; Journal of the American Chemical Society 136 (2014) 1520–1525; doi:10.1021/ja411391c

data_4120490
_publ_section_title
;
 Anion Binding Modes in meso-Substituted Hexapyrrolic Calix[4]pyrrole
 Isomers.
;
_journal_issue                   4
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1520
_journal_page_last               1525
_journal_paper_doi               10.1021/ja411391c
_journal_volume                  136
_journal_year                    2014
_chemical_formula_sum            'C52 H36 N6 O6'
_chemical_formula_weight         840.86
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_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_creation_method           SHELXL-97
_cell_angle_alpha                103.891(2)
_cell_angle_beta                 106.045(2)
_cell_angle_gamma                107.1360(10)
_cell_formula_units_Z            2
_cell_length_a                   10.4590(2)
_cell_length_b                   14.6430(4)
_cell_length_c                   18.3230(5)
_cell_measurement_temperature    153(2)
_cell_volume                     2414.07(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_av_sigmaI/netI    0.0848
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13201
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.55
_exptl_absorpt_coefficient_mu    0.093
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             972
_refine_diff_density_max         0.763
_refine_diff_density_min         -0.585
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.624
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     573
_refine_ls_number_reflns         8448
_refine_ls_number_restraints     372
_refine_ls_restrained_S_all      1.660
_refine_ls_R_factor_all          0.1270
_refine_ls_R_factor_gt           0.0710
_refine_ls_shift/su_max          0.073
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1239
_refine_ls_wR_factor_ref         0.1340
_reflns_number_gt                5202
_reflns_number_total             8448
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja411391c_si_002.cif
_cod_data_source_block           spa242
_cod_original_cell_volume        2414.06(10)
_cod_database_code               4120490