Bis[3-(dihydroxyboryl)anilinium] sulfate
Vega, Araceli; Luna, Rolando; Tlahuext, Hugo; Höpfl, Herbert; Acta Crystallographica Section E 66 (2010) o1035–o1036; doi:10.1107/S1600536810012092

data_2225995
_publ_section_title
;
 Bis[3-(dihydroxyboryl)anilinium] sulfate
;
_journal_coeditor_code           TK2649
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1035
_journal_page_last               o1036
_journal_paper_doi               10.1107/S1600536810012092
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '2C6 H9 B N O2 +, S O4 2-'
_chemical_formula_moiety         '2C6 H9 B N O2 +, O4 S 2-'
_chemical_formula_sum            'C12 H18 B2 N2 O8 S'
_chemical_formula_weight         371.96
_chemical_melting_point_gt       573
_chemical_name_systematic
;
3-(Dihydroxyboryl)anilinium hemisulfate
;
_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                 101.423(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.3589(9)
_cell_length_b                   15.695(3)
_cell_length_c                   20.489(3)
_cell_measurement_reflns_used    1721
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      19.99
_cell_measurement_theta_min      2.59
_cell_volume                     1689.2(5)
_computing_cell_refinement       'SAINT-Plus NT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT-Plus NT (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL-NT (Sheldrick, 2008)'
_computing_publication_material
;
PLATON (Spek, 2009) and publCIF (Westrip, 2010)
;
_computing_structure_refinement  'SHELXTL-NT (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL-NT (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 8.3
_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       '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  0.0957
_diffrn_reflns_av_sigmaI/netI    0.0818
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            18634
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.65
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.235
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.83
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular prism'
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.358
_refine_diff_density_min         -0.366
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         3675
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.1131
_refine_ls_R_factor_gt           0.0777
_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^)+(0.0357P)^2^+2.0612P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1330
_refine_ls_wR_factor_ref         0.1454
_reflns_number_gt                2642
_reflns_number_total             3675
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            tk2649.cif
_cod_data_source_block           I
_cod_original_cell_volume        1689.1(5)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2225995
_cod_database_fobs_code          2225995