4,9,12,15-Tetraoxa-3,5,8,10,14,16-hexaazatetracyclo[11.3.0.0^2,6^.0^7,11^]hexadeca-1(16),2,5,7,10,13-hexaen-3-ium-3-olate monohydrate
Zhou, Yan-Shui; Wang, Bo-Zhou; Xu, Kang-Zhen; Acta Crystallographica Section E 68 (2012) o869–; doi:10.1107/S160053681200774X

data_2234012
_publ_section_title
;
 4,9,12,15-Tetraoxa-3,5,8,10,14,16-hexaazatetracyclo[11.3.0.0^2,6^.0^7,11^]hexadeca-1(16),2,5,7,10,13-hexaen-3-ium-3-olate
 monohydrate
;
_journal_coeditor_code           TK5030
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o869
_journal_paper_doi               10.1107/S160053681200774X
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C6 N6 O5, H2 O'
_chemical_formula_moiety         'C6 N6 O5, H2 O'
_chemical_formula_sum            'C6 H2 N6 O6'
_chemical_formula_weight         254.14
_chemical_name_common
;
bifurazano[3,4-<i>b</i>:3',4'-<i>f</i>]furoxano[3'',4''-
<i>d</i>]oxacyclohetpatriene
;
_chemical_name_systematic
;
4,9,12,15-Tetraoxa-3,5,8,10,14,16-
hexaazatetracyclo[11.3.0.0^2,6^.0^7,11^]hexadeca-
1(16),2,5,7,10,13-hexaen-3-ium-3-olate monohydrate
;
_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                 106.305(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.324(4)
_cell_length_b                   9.727(4)
_cell_length_c                   10.391(4)
_cell_measurement_reflns_used    3631
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.09
_cell_measurement_theta_min      2.93
_cell_volume                     904.5(6)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w 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  0.0246
_diffrn_reflns_av_sigmaI/netI    0.0255
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5058
_diffrn_reflns_theta_full        28.16
_diffrn_reflns_theta_max         28.16
_diffrn_reflns_theta_min         2.28
_exptl_absorpt_coefficient_mu    0.169
_exptl_absorpt_correction_T_max  0.9750
_exptl_absorpt_correction_T_min  0.9621
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.866
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             512
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.262
_refine_diff_density_min         -0.180
_refine_ls_extinction_coef       0.009(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         2146
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0364
_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^)+(0.0389P)^2^+0.3369P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0913
_refine_ls_wR_factor_ref         0.0972
_reflns_number_gt                1808
_reflns_number_total             2146
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            tk5030.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2234012
_cod_database_fobs_code          2234012