Synthesis, structure, anion binding, and sensing by calix[4]pyrrole isomers.
Nishiyabu, Ryuhei; Palacios, Manuel A; Dehaen, Wim; Anzenbacher, Jr, Pavel; Journal of the American Chemical Society 128 (2006) 11496–11504; doi:10.1021/ja0622150

data_4101570
_publ_section_title
;
 Synthesis, structure, anion binding, and sensing by calix[4]pyrrole
 isomers.
;
_journal_issue                   35
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11496
_journal_page_last               11504
_journal_paper_doi               10.1021/ja0622150
_journal_volume                  128
_journal_year                    2006
_chemical_formula_sum            'C36 H42 N6 O2'
_chemical_formula_weight         590.76
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_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                 99.4240(18)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   25.3520(10)
_cell_length_b                   10.2210(4)
_cell_length_c                   26.3470(13)
_cell_measurement_temperature    293(2)
_cell_volume                     6735.0(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.947
_diffrn_measured_fraction_theta_max 0.947
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.5671
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            11044
_diffrn_reflns_theta_full        24.85
_diffrn_reflns_theta_max         24.85
_diffrn_reflns_theta_min         3.08
_exptl_absorpt_coefficient_mu    0.074
_exptl_crystal_density_diffrn    1.165
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2528
_refine_diff_density_max         0.856
_refine_diff_density_min         -0.473
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.888
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         11044
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.888
_refine_ls_R_factor_all          0.4852
_refine_ls_R_factor_gt           0.2051
_refine_ls_shift/su_max          0.221
_refine_ls_shift/su_mean         0.017
_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          0.2580
_refine_ls_wR_factor_ref         0.3176
_reflns_number_gt                3177
_reflns_number_total             11044
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0622150si20060417_022603.cif
_cod_data_source_block           calx3
_cod_database_code               4101570