A Highly Efficient, Preorganized Macrobicyclic Receptor for Halides Based on CH... and NH...Anion Interactions
Christos A. Ilioudis; Derek A. Tocher; Jonathan W. Steed; Journal of the American Chemical Society 126 (2004) 12395–12402; doi:10.1021/ja047070g

data_4112997
_publ_section_title
;
 A Highly Efficient, Preorganized Macrobicyclic Receptor for Halides Based
 on CH... and NH...Anion Interactions
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12395
_journal_page_last               12402
_journal_paper_doi               10.1021/ja047070g
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C69 H87 Cl6 N7 O12 S6'
_chemical_formula_weight         1611.61
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           146
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :H'
_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                120.00
_cell_formula_units_Z            3
_cell_length_a                   16.3404(23)
_cell_length_b                   16.3404(23)
_cell_length_c                   28.0178(27)
_cell_measurement_temperature    120(2)
_cell_volume                     6478.7(14)
_computing_cell_refinement       'DENZO SMN'
_computing_data_collection       'NONIUS COLLECT'
_computing_data_reduction        'DENZO SMN'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.940
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measurement_device_type  'KAPPA CCD'
_diffrn_measurement_method       '2o phi frames'
_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  0.1939
_diffrn_reflns_av_sigmaI/netI    0.3169
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            10189
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         2.97
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.400
_exptl_absorpt_correction_type   scalepack
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_description       plate
_exptl_crystal_F_000             2514
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.515
_refine_diff_density_min         -0.669
_refine_diff_density_rms         0.169
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.7(2)
_refine_ls_extinction_coef       0.0021(6)
_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   1.498
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         5656
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      1.496
_refine_ls_R_factor_all          0.2773
_refine_ls_R_factor_gt           0.2118
_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/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3166
_refine_ls_wR_factor_ref         0.3388
_reflns_number_gt                3732
_reflns_number_total             5656
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja047070gsi20040519_073146.cif
_cod_data_source_block           c:\structs\chris\tc2\rhomt2
_cod_original_cell_volume        6479.0(18)
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               4112997