Bis(3,5-diamino-4<i>H</i>-1,2,4-triazol-1-ium) 3,4-dioxocyclobutane-1,2-diolate
Fun, Hoong-Kun; Loh, Wan-Sin; Johnson, Atim; Yousuf, Sammer; Eno, Ededet; Acta Crystallographica Section E 69 (2013) o353–o354; doi:10.1107/S160053681300322X

data_2237549
_publ_section_title
;
 Bis(3,5-diamino-4<i>H</i>-1,2,4-triazol-1-ium)
 3,4-dioxocyclobutane-1,2-diolate
;
_journal_coeditor_code           RZ5040
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o353
_journal_page_last               o354
_journal_paper_doi               10.1107/S160053681300322X
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '2C2 H6 N5 +, C4 O4 2-'
_chemical_formula_moiety         '2(C2 H6 N5 +), C4 O4 2-'
_chemical_formula_sum            'C8 H12 N10 O4'
_chemical_formula_weight         312.28
_chemical_name_systematic
;
bis(3,5-diamino-4<i>H</i>-1,2,4-triazol-1-ium)
3,4-dioxocyclobutane-1,2-diolate
;
_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                 91.7340(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.7186(2)
_cell_length_b                   11.6533(2)
_cell_length_c                   6.86180(10)
_cell_measurement_reflns_used    7050
_cell_measurement_temperature    100.0(10)
_cell_measurement_theta_max      33.66
_cell_measurement_theta_min      2.18
_cell_volume                     1256.32(3)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
;
SHELXTL (Sheldrick, 2008) and PLATON (Spek, 2009)
;
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.00(10)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type
;
Bruker SMART APEXII CCD area-detector
;
_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  0.0281
_diffrn_reflns_av_sigmaI/netI    0.0316
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            19113
_diffrn_reflns_theta_full        33.67
_diffrn_reflns_theta_max         33.67
_diffrn_reflns_theta_min         1.30
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.135
_exptl_absorpt_correction_T_max  0.9817
_exptl_absorpt_correction_T_min  0.9434
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>SADABS</i>; Bruker, 2009)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.651
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.430
_refine_diff_density_min         -0.321
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         4965
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0396
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0597P)^2^+0.1328P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0985
_refine_ls_wR_factor_ref         0.1081
_reflns_number_gt                3911
_reflns_number_total             4965
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            rz5040.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2237549
_cod_database_fobs_code          2237549