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_4108212
_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            'C36 H30 N6 O18'
_chemical_formula_weight         834.66
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                84.106(4)
_cell_angle_beta                 85.278(5)
_cell_angle_gamma                81.873(5)
_cell_formula_units_Z            4
_cell_length_a                   5.6949(12)
_cell_length_b                   19.833(4)
_cell_length_c                   33.883(7)
_cell_measurement_reflns_used    3502
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.99
_cell_measurement_theta_min      2.31
_cell_volume                     3759.6(13)
_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 0.902
_diffrn_measured_fraction_theta_max 0.902
_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  0.0312
_diffrn_reflns_av_sigmaI/netI    0.0792
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            23621
_diffrn_reflns_theta_full        28.01
_diffrn_reflns_theta_max         28.01
_diffrn_reflns_theta_min         1.04
_exptl_absorpt_coefficient_mu    0.121
_exptl_absorpt_correction_T_max  0.9904
_exptl_absorpt_correction_T_min  0.9096
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_description       needle
_exptl_crystal_F_000             1728
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.308
_refine_diff_density_min         -0.236
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1321
_refine_ls_number_reflns         16401
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.1090
_refine_ls_R_factor_gt           0.0566
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0560P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1135
_refine_ls_wR_factor_ref         0.1436
_reflns_number_gt                9669
_reflns_number_total             16401
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8035652-file002.cif
_cod_data_source_block           ob145
_cod_original_cell_volume        3759.6(14)
_cod_database_code               4108212