Structural characterization of protonated benzeneseleninic acid, the dihydroxyselenonium ion
Sørensen, Henning Osholm; Stuhr-Hansen, Nicolai; Henriksen, Lars; Larsen, Sine; Acta Crystallographica Section B 56 (2000) 1029–1034; doi:10.1107/S0108768100010697

data_2102202
_publ_section_title
;
 Structural characterization of protonated benzeneseleninic acid, the
 dihydroxyselenonium ion
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              1029
_journal_page_last               1034
_journal_paper_doi               10.1107/S0108768100010697
_journal_volume                  56
_journal_year                    2000
_chemical_formula_moiety         'C6 H7 O2 Se1 +,C6 H5 O3 S1 -'
_chemical_formula_sum            'C12 H12 O5 S Se'
_chemical_formula_weight         347.24
_chemical_name_systematic
; 
 dihydroxy phenylselenonium benzene sulfonate 
;
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   40.641(5)
_cell_length_b                   22.268(3)
_cell_length_c                   5.7881(13)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    122.0(5)
_cell_measurement_theta_max      40.64
_cell_measurement_theta_min      39.13
_cell_volume                     5238.2(15)
_computing_cell_refinement       'Enraf-Nonius XPRESS'
_computing_data_collection       'Enraf-Nonius XPRESS'
_computing_data_reduction        'DREADD (Blessing, 1987)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      122.0(5)
_diffrn_measured_fraction_theta_full 0.254
_diffrn_measured_fraction_theta_max 0.254
_diffrn_measurement_device_type  'Enraf Nonius CAD-4'
_diffrn_measurement_method       '\w - 2\q'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0383
_diffrn_reflns_av_sigmaI/netI    0.0204
_diffrn_reflns_limit_h_max       50
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            5592
_diffrn_reflns_theta_full        74.93
_diffrn_reflns_theta_max         74.93
_diffrn_reflns_theta_min         4.35
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  166.7
_diffrn_standards_number         4
_exptl_absorpt_coefficient_mu    5.521
_exptl_absorpt_correction_T_max  0.737
_exptl_absorpt_correction_T_min  0.361
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(DeTitta, 1985)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.761
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       needle
_exptl_crystal_F_000             2784
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.188
_refine_diff_density_min         -1.131
_refine_diff_density_rms         0.149
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   5.839
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         2669
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      5.891
_refine_ls_R_factor_all          0.0772
_refine_ls_R_factor_gt           0.0737
_refine_ls_shift/su_max          0.036
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     w=1/[\s^2^(Fo^2^)]
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.1416
_refine_ls_wR_factor_ref         0.1425
_reflns_number_gt                2552
_reflns_number_total             2669
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            os0057.cif
_cod_data_source_block           BEN
_cod_original_cell_volume        5238.4(15)
_cod_database_code               2102202
_cod_database_fobs_code          2102202