Solution Phase Measurement of Both Weak σ and C-H...X-Hydrogen Bonding Interactions in Synthetic Anion Receptors
Orion B. Berryman; Aaron C. Sather; Benjamin P. Hay; Jeffrey S. Meisner; Darren W. Johnson; Journal of the American Chemical Society 130 (2008) 10895–10897; doi:10.1021/ja8035652

data_4108211
_publ_section_title
;
 Solution Phase Measurement of Both Weak \s and C-H...X-Hydrogen Bonding
 Interactions in Synthetic Anion Receptors
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10895
_journal_page_last               10897
_journal_paper_doi               10.1021/ja8035652
_journal_volume                  130
_journal_year                    2008
_chemical_formula_sum            'C42 H48 N6 O21 S3'
_chemical_formula_weight         1069.04
_chemical_name_systematic
; 
 ? 
;
_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                 110.669(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   28.272(12)
_cell_length_b                   5.075(2)
_cell_length_c                   37.126(15)
_cell_measurement_reflns_used    1811
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      19.28
_cell_measurement_theta_min      2.31
_cell_volume                     4984(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0953
_diffrn_reflns_av_sigmaI/netI    0.1162
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            33339
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         0.79
_exptl_absorpt_coefficient_mu    0.233
_exptl_absorpt_correction_T_max  0.9953
_exptl_absorpt_correction_T_min  0.8352
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_description       needle
_exptl_crystal_F_000             2232
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.616
_refine_diff_density_min         -0.332
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.946
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     544
_refine_ls_number_reflns         8731
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.946
_refine_ls_R_factor_all          0.1736
_refine_ls_R_factor_gt           0.0857
_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^)+(0.1240P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2289
_refine_ls_wR_factor_ref         0.2637
_reflns_number_gt                3582
_reflns_number_total             8731
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8035652-file001.cif
_cod_data_source_block           ob148
_cod_database_code               4108211