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_4116074
_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            'C48.48 H53.24 Cl8.86 N4 Na O12.14'
_chemical_formula_weight         1223.29
_chemical_name_systematic
; 
 Na(H2O)(bicyclicbenzocrown)Cl.(2.62CHCl3).(0.31C6H14).(1.14H2O) 
;
_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                 106.455(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.075(2)
_cell_length_b                   17.906(7)
_cell_length_c                   23.885(3)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      23
_cell_measurement_theta_min      0
_cell_volume                     5773(3)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0718
_diffrn_reflns_av_sigmaI/netI    0.0601
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            23227
_diffrn_reflns_theta_full        23.00
_diffrn_reflns_theta_max         23.00
_diffrn_reflns_theta_min         1.89
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.498
_exptl_absorpt_correction_T_max  0.9660
_exptl_absorpt_correction_T_min  0.9070
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_description       plate-like
_exptl_crystal_F_000             2523
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.827
_refine_diff_density_min         -0.455
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    'idealized with riding models'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     724
_refine_ls_number_reflns         8009
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.1393
_refine_ls_R_factor_gt           0.0925
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1414P)^2^+13.9441P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2408
_refine_ls_wR_factor_ref         0.2782
_reflns_number_gt                5166
_reflns_number_total             8009
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja994487r_1.cif
_cod_data_source_block           for_compound_1a.Na.CHCl3.Cl
_cod_database_code               4116074