2,6-Dihydroxy-4-oxo-2-(pyridin-1-ium-3-yl)-4<i>H</i>-1,3,2-benzodioxaborinin-2-ide 0.67-hydrate
Garcia-Grajeda, Blanca A.; Höpfl, Herbert; Guerrero-Alvarez, Jorge A.; Campos-Gaxiola, José J.; Cruz-Enríquez, Adriana; Acta Crystallographica Section E 70 (2014) o388–o389; doi:10.1107/S1600536814004267

data_2239232
_publ_section_title
;
 2,6-Dihydroxy-4-oxo-2-(pyridin-1-ium-3-yl)-4<i>H</i>-1,3,2-benzodioxaborinin-2-ide
 0.67-hydrate
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o388
_journal_page_last               o389
_journal_paper_doi               10.1107/S1600536814004267
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          'C12 H10 B N O5, 0.67H2 O'
_chemical_formula_moiety         'C12 H10 B N O5, 0.67(H2 O)'
_chemical_formula_sum            'C12 H11.33 B N O5.67'
_chemical_formula_weight         271.03
_chemical_name_systematic
'2,6-Dihydroxy-4-oxo-2-(pyridin-1-ium-3-yl)-4<i>H</i>-1,3,2-benzodioxaborinin-2-ide 0.67-hydrate'
_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                65.785(4)
_cell_angle_beta                 73.421(4)
_cell_angle_gamma                87.213(5)
_cell_formula_units_Z            6
_cell_length_a                   10.350(2)
_cell_length_b                   13.916(3)
_cell_length_c                   14.340(3)
_cell_measurement_reflns_used    1641
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.15
_cell_measurement_theta_min      2.51
_cell_volume                     1799.8(6)
_computing_cell_refinement       '<i>SAINT-Plus-NT</i> (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        '<i>SAINT-Plus-NT</i> (Bruker, 2001)'
_computing_molecular_graphics
'ORTEP-3 for Windows (Farrugia, 2012) and Mercury (Macrae <i>et al.</i>, 2008)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXTL-NT (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL-NT (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker 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  0.0920
_diffrn_reflns_av_sigmaI/netI    0.1394
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            18938
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    0.118
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.95
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             844
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.710
_refine_diff_density_min         -0.260
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     571
_refine_ls_number_reflns         7051
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.1153
_refine_ls_R_factor_gt           0.0530
_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^)+(0.0125P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0855
_refine_ls_wR_factor_ref         0.0920
_reflns_number_gt                3529
_reflns_number_total             7051
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            is5341sup1.cf
_cod_data_source_block           I
_cod_original_cell_volume        1799.8(7)
_cod_database_code               2239232
_cod_database_fobs_code          2239232