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_4026443
_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            'C40 H53 B Cl2 F2 N3 O2.26'
_chemical_formula_weight         731.75
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_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                 113.294(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.897(3)
_cell_length_b                   23.457(2)
_cell_length_c                   21.571(2)
_cell_measurement_temperature    123(2)
_cell_volume                     7852.8(17)
_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
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0612
_diffrn_reflns_av_sigmaI/netI    0.0669
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            117426
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.08
_exptl_absorpt_coefficient_mu    0.213
_exptl_absorpt_correction_T_max  0.9586
_exptl_absorpt_correction_T_min  0.9196
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.238
_exptl_crystal_description       prism
_exptl_crystal_F_000             3113
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.850
_refine_diff_density_min         -0.567
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1843
_refine_ls_number_reflns         34687
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0851
_refine_ls_R_factor_gt           0.0597
_refine_ls_shift/su_max          0.037
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[?^2^(Fo^2^)+(0.0817P)^2^+1.1909P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1451
_refine_ls_wR_factor_ref         0.1573
_reflns_number_gt                25552
_reflns_number_total             34687
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo2008687_si_002_3.cif
_cod_data_source_block           90105mae
_cod_original_cell_volume        7852.6(16)
_cod_database_code               4026443