Synthesis, Crystal Structures, and Supramolecular Assemblies of Pyrrole-Based Anion Receptors Bearing Modified Pyrrole β-Substituents
Yohei Haketa; Shohei Sakamoto; Kengo Chigusa; Takashi Nakanishi; Hiromitsu Maeda; Journal of Organic Chemistry 76 (2011) 5177–5184; doi:10.1021/jo2008687

data_4026441
_publ_section_title
;
 Synthesis, Crystal Structures, and Supramolecular Assemblies of
 Pyrrole-Based Anion Receptors Bearing Modified Pyrrole \b-Substituents
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              5177
_journal_page_last               5184
_journal_paper_doi               10.1021/jo2008687
_journal_volume                  76
_journal_year                    2011
_chemical_formula_sum            'C27 H25 B F2 N2 O2'
_chemical_formula_weight         458.30
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                109.518(12)
_cell_angle_beta                 101.221(13)
_cell_angle_gamma                95.073(12)
_cell_formula_units_Z            4
_cell_length_a                   8.236(3)
_cell_length_b                   16.744(6)
_cell_length_c                   17.667(7)
_cell_measurement_temperature    123(2)
_cell_volume                     2221.2(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK?
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0574
_diffrn_reflns_av_sigmaI/netI    0.0927
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            21375
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.01
_exptl_absorpt_coefficient_mu    0.098
_exptl_absorpt_correction_T_max  0.9902
_exptl_absorpt_correction_T_min  0.9711
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_description       prism
_exptl_crystal_F_000             972
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.289
_refine_diff_density_min         -0.392
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.980
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     621
_refine_ls_number_reflns         9822
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.980
_refine_ls_R_factor_all          0.1312
_refine_ls_R_factor_gt           0.0624
_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/[?^2^(Fo^2^)+(0.0955P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1527
_refine_ls_wR_factor_ref         0.1881
_reflns_number_gt                5194
_reflns_number_total             9822
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo2008687_si_002_1.cif
_cod_data_source_block           91127mae
_cod_original_cell_volume        2221.4(13)
_cod_database_code               4026441