Fluoride-Selective Binding in a New Deep Cavity Calix[4]pyrrole: Experiment and Theory
Christopher J. Woods; Salvatore Camiolo; Mark E. Light; Simon J. Coles; Michael B. Hursthouse; Michael A. King; Philip A. Gale; Jonathan W. Essex; Journal of the American Chemical Society 124 (2002) 8644–8652; doi:10.1021/ja025572t

data_4114964
_publ_section_title
;
 Fluoride-Selective Binding in a New Deep Cavity Calix[4]pyrrole:
 Experiment and Theory
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8644
_journal_page_last               8652
_journal_paper_doi               10.1021/ja025572t
_journal_volume                  124
_journal_year                    2002
_chemical_formula_sum            'C62 H61 N7 O8'
_chemical_formula_weight         1032.18
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           85
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a'
_symmetry_space_group_name_H-M   'P 4/n :2'
_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            2
_cell_length_a                   11.3723(16)
_cell_length_b                   11.3723(16)
_cell_length_c                   21.020(4)
_cell_measurement_temperature    150(2)
_cell_volume                     2718.5(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0917
_diffrn_reflns_av_sigmaI/netI    0.0612
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            23657
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.19
_exptl_absorpt_coefficient_mu    0.084
_exptl_absorpt_correction_T_max  0.9975
_exptl_absorpt_correction_T_min  0.9916
_exptl_crystal_density_diffrn    1.261
_exptl_crystal_F_000             1092
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.289
_refine_diff_density_min         -0.261
_refine_diff_density_rms         0.053
_refine_ls_extinction_coef       0.0043(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         3120
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0990
_refine_ls_R_factor_gt           0.0518
_refine_ls_shift/su_max          0.441
_refine_ls_shift/su_mean         0.024
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0823P)^2^+0.1320P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1258
_refine_ls_wR_factor_ref         0.1511
_reflns_number_gt                1918
_reflns_number_total             3120
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja025572t_s1_2.cif
_cod_data_source_block           s93
_cod_original_cell_volume        2718.4(8)
_cod_original_sg_symbol_H-M      'P 4/n'
_cod_database_code               4114964