A Macrobicyclic Receptor with Versatile Recognition Properties: Simultaneous Binding of an Ion Pair and Selective Complexation of Dimethylsulfoxide
Martin J. Deetz; Maoyu Shang; Bradley D. Smith; Journal of the American Chemical Society 122 (2000) 6201–6207; doi:10.1021/ja994487r

data_4116075
_publ_section_title
;
 A Macrobicyclic Receptor with Versatile Recognition Properties:
 Simultaneous Binding of an Ion Pair and Selective Complexation of
 Dimethylsulfoxide
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6201
_journal_page_last               6207
_journal_paper_doi               10.1021/ja994487r
_journal_volume                  122
_journal_year                    2000
_chemical_formula_sum            'C47 H55 N4 O13.5 S1.5'
_chemical_formula_weight         940.04
_chemical_name_systematic
; 
(dicarboxamidedibenzocrown).2.0H2O.1.5Me2SO
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 102.880(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   38.531(3)
_cell_length_b                   14.1236(10)
_cell_length_c                   17.5199(17)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      2
_cell_volume                     9294.4(13)
_computing_cell_refinement       MADNES
_computing_data_collection       MADNES
_computing_data_reduction        'MADNES (Messerschmitt & Pflugrath, 1987)'
_computing_molecular_graphics    'ORTEP-III for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXTL-v5 (Siemens, 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      220(2)
_diffrn_detector_area_resol_mean 8.2/10.9
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Enraf-Nonius FAST area-detector'
_diffrn_measurement_method       'Ellipsoid-mask fitting'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0659
_diffrn_reflns_av_sigmaI/netI    0.0541
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            23008
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.87
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.163
_exptl_absorpt_correction_T_max  0.9919
_exptl_absorpt_correction_T_min  0.9348
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_description       plate-like
_exptl_crystal_F_000             3976
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.860
_refine_diff_density_min         -0.913
_refine_diff_density_rms         0.075
_refine_ls_extinction_coef       0.0013(2)
_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   0.989
_refine_ls_hydrogen_treatment
;
 Hydron atoms from amide and water groups were refined with riding
thermal parameters, while the rest were idealized with riding models.
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         8059
_refine_ls_number_restraints     87
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.1256
_refine_ls_R_factor_gt           0.0856
_refine_ls_shift/su_max          0.069
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1224P)^2^+38.0955P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2165
_refine_ls_wR_factor_ref         0.2462
_reflns_number_gt                5419
_reflns_number_total             8059
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja994487r_2.cif
_cod_data_source_block           for_compound_1a.DMSO
_cod_original_formula_sum        'C47 H55 N4 O13.50 S1.50'
_cod_database_code               4116075