Molecular Recognition of Trigonal Oxyanions Using a Ditopic Salt Receptor: Evidence for Anisotropic Shielding Surface around Nitrate Anion
Joseph M. Mahoney; Kenneth A. Stucker; Hua Jiang; Ian Carmichael; Nicole R. Brinkmann; Alicia M. Beatty; Bruce C. Noll; Bradley D. Smith; Journal of the American Chemical Society 127 (2005) 2922–2928; doi:10.1021/ja0440295

data_4111493
_publ_section_title
;
 Molecular Recognition of Trigonal Oxyanions Using a Ditopic Salt
 Receptor: Evidence for Anisotropic Shielding Surface around Nitrate Anion
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2922
_journal_page_last               2928
_journal_paper_doi               10.1021/ja0440295
_journal_volume                  127
_journal_year                    2005
_chemical_compound_source        synthesized
_chemical_formula_moiety         'C38 H50 N5 Na O8, 0.68(C4 H8 O2)'
_chemical_formula_sum            'C40.72 H55.46 N5 Na O9.37'
_chemical_formula_weight         787.89
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                76.996(1)
_cell_angle_beta                 77.410(1)
_cell_angle_gamma                72.797(1)
_cell_formula_units_Z            4
_cell_length_a                   13.1842(2)
_cell_length_b                   13.3913(2)
_cell_length_c                   25.3011(5)
_cell_measurement_reflns_used    7863
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.40
_cell_measurement_theta_min      2.52
_cell_volume                     4102.34(12)
_computing_cell_refinement       'Bruker APEX2/SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT/SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_av_sigmaI/netI    0.0252
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            73842
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         0.84
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Siemens KFFMO2K-90'
_exptl_absorpt_coefficient_mu    0.100
_exptl_absorpt_correction_T_max  0.9682
_exptl_absorpt_correction_T_min  0.9467
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Blessing, R. H. Acta Cryst. (1995) A51, 33-38.'
_exptl_crystal_colour            'clear colorless'
_exptl_crystal_density_diffrn    1.276
_exptl_crystal_density_meas      0
_exptl_crystal_description       block
_exptl_crystal_F_000             1683
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.52
_exptl_crystal_size_min          0.33
_platon_squeeze_details
;There are two badly disordered solvent sites in the asymmetric unit. 
The only solvent used to prepare the crystals was ethyl acetate. SQUEEZE was 
used to model these sites. The volumes found by SQUEEZE are suitable for
this solvent. The electron count is equivalent to 1.36 molecules of ethyl 
acetate in the asymmetric unit.
;
_refine_diff_density_max         1.677
_refine_diff_density_min         -0.606
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     989
_refine_ls_number_reflns         14452
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0904
_refine_ls_R_factor_gt           0.0821
_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^)+(0.1184P)^2^+5.2575P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2232
_refine_ls_wR_factor_ref         0.2307
_reflns_number_gt                12225
_reflns_number_total             14452
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0440295si20040930_061247.cif
_cod_data_source_block           bcn62sq
_cod_database_code               4111493