Molecular Structure of the Solvated Proton in Isolated Salts. Short, Strong, Low Barrier (SSLB) H-bonds
Daniel Stasko; Stephan P. Hoffmann; Kee-Chan Kim; Nathanael L. P. Fackler; Anna S. Larsen; Tatiana Drovetskaya; Fook S. Tham; Christopher A. Reed; Clifton E. F. Rickard; Peter D. W. Boyd; Evgenii S. Stoyanov; Journal of the American Chemical Society 124 (2002) 13869–13876; doi:10.1021/ja012671i

data_4115294
_publ_section_title
;
 Molecular Structure of the Solvated Proton in Isolated Salts. Short,
 Strong, Low Barrier (SSLB) H-bonds
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13869
_journal_page_last               13876
_journal_paper_doi               10.1021/ja012671i
_journal_volume                  124
_journal_year                    2002
_chemical_formula_sum            'C9 H27 B11 Cl6 O2'
_chemical_formula_weight         498.92
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 90.7730(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.6777(4)
_cell_length_b                   23.5020(13)
_cell_length_c                   13.5215(7)
_cell_measurement_temperature    198(2)
_cell_volume                     2439.6(2)
_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  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      198(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         'Normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0405
_diffrn_reflns_av_sigmaI/netI    0.0444
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22221
_diffrn_reflns_theta_full        30.50
_diffrn_reflns_theta_max         30.50
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    0.709
_exptl_absorpt_correction_T_max  0.9860
_exptl_absorpt_correction_T_min  0.6756
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_density_meas      0
_exptl_crystal_description       'Thin Needle'
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.649
_refine_diff_density_min         -0.219
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         7421
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0666
_refine_ls_R_factor_gt           0.0409
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0555P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0949
_refine_ls_wR_factor_ref         0.1055
_reflns_number_gt                5294
_reflns_number_total             7421
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja012671i_1.cif
_cod_data_source_block           ucr221m
_cod_database_code               4115294