Calix[4]pyrroles bearing proximally meso-meso linking straps: synthesis and anion binding properties
Ja-Young Park; Kamil Skonieczny; Naoki Aratani; Atsuhiro Osuka; Daniel T. Gryko; Chang-Hee Lee; Chem.Commun. 48 (2012) 8060–; doi:10.1039/c2cc33537a

data_7108135
_publ_section_title
;
 Calix[4]pyrroles bearing proximally meso-meso linking straps: synthesis
 and anion binding properties
;
_journal_name_full               Chem.Commun.
_journal_page_first              8060
_journal_paper_doi               10.1039/c2cc33537a
_journal_volume                  48
_journal_year                    2012
_chemical_formula_moiety         'C54 H68 N4 O4, C O '
_chemical_formula_sum            'C55 H68 N4 O5'
_chemical_formula_weight         865.13
_space_group_IT_number           56
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      56
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   34.4374(8)
_cell_length_b                   10.2869(2)
_cell_length_c                   13.5539(3)
_cell_measurement_reflns_used    26811
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      68.18
_cell_measurement_theta_min      3.26
_cell_volume                     4801.52(18)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 10.0
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0676
_diffrn_reflns_av_sigmaI/netI    0.0502
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            47801
_diffrn_reflns_theta_full        68.24
_diffrn_reflns_theta_max         68.24
_diffrn_reflns_theta_min         5.14
_exptl_absorpt_coefficient_mu    0.600
_exptl_absorpt_correction_T_max  0.9706
_exptl_absorpt_correction_T_min  0.9424
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.197
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1864
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.286
_refine_diff_density_min         -0.257
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         4347
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.1136
_refine_ls_R_factor_gt           0.0642
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0943P)^2^+0.7386P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1634
_refine_ls_wR_factor_ref         0.2029
_reflns_number_gt                2512
_reflns_number_total             4347
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc33537a.txt
_cod_data_source_block           01211chl
_cod_original_sg_symbol_H-M      'P ccn'
_cod_database_code               7108135