First Cryptand-Like Calixpyrrole: Synthesis, X-ray Structure, and Anion Binding Properties of a Bicyclic[3,3,3]nonapyrrole
Christophe Bucher; Rebecca S. Zimmerman; Vincent Lynch; Jonathan L. Sessler; Journal of the American Chemical Society 123 (2001) 9716–9717; doi:10.1021/ja016629z

data_4115710
_publ_section_title
;
 First Cryptand-Like Calixpyrrole: Synthesis, X-ray Structure, and Anion
 Binding Properties of a Bicyclic[3,3,3]nonapyrrole
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9716
_journal_page_last               9717
_journal_paper_doi               10.1021/ja016629z
_journal_volume                  123
_journal_year                    2001
_chemical_formula_sum            'C57 H73 Cl2 N9 O3'
_chemical_formula_weight         1003.14
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 94.062(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.0515(6)
_cell_length_b                   22.1214(13)
_cell_length_c                   20.1491(9)
_cell_measurement_temperature    153(2)
_cell_volume                     5358.2(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1550
_diffrn_reflns_av_sigmaI/netI    0.2096
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            17190
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.94
_exptl_absorpt_coefficient_mu    0.174
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'faint orange'
_exptl_crystal_density_diffrn    1.244
_exptl_crystal_description       prisms
_exptl_crystal_F_000             2144
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.661
_refine_diff_density_min         -0.499
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.209
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     640
_refine_ls_number_reflns         9313
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.209
_refine_ls_R_factor_all          0.2458
_refine_ls_R_factor_gt           0.1187
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0430P)^2^+4.5200P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1778
_refine_ls_wR_factor_ref         0.2061
_reflns_number_gt                4253
_reflns_number_total             9313
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja016629z_s2.cif
_cod_data_source_block           1
_cod_database_code               4115710