(<i>E</i>)-3,3'-(Diazene-1,2-diyl)bis(1-methyl-1,4,5,6-tetrahydropyrrolo[3,4-<i>c</i>]pyrazol-5-ium) dinitrate dihydrate
Chen, Jin-Mei; Zhao, Hong; Acta Crystallographica Section E 68 (2012) o151–; doi:10.1107/S1600536811053347

data_2233286
_publ_section_title
;
 (<i>E</i>)-3,3'-(Diazene-1,2-diyl)bis(1-methyl-1,4,5,6-tetrahydropyrrolo[3,4-<i>c</i>]pyrazol-5-ium)
 dinitrate dihydrate
;
_journal_coeditor_code           RZ2680
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o151
_journal_paper_doi               10.1107/S1600536811053347
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C12 H18 N8 2+, 2N O3 -, 2H2 O'
_chemical_formula_moiety         'C12 H18 N8 2+, 2(N O3 -), 2(H2 O)'
_chemical_formula_sum            'C12 H22 N10 O8'
_chemical_formula_weight         434.40
_chemical_name_systematic
;
(<i>E</i>)-3,3'-(Diazene-1,2-diyl)bis(1-methyl-1,4,5,6-
tetrahydropyrrolo[3,4-<i>c</i>]pyrazol-5-ium) dinitrate dihydrate
;
_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                99.56(3)
_cell_angle_beta                 92.49(3)
_cell_angle_gamma                92.84(3)
_cell_formula_units_Z            1
_cell_length_a                   6.2344(12)
_cell_length_b                   7.7725(16)
_cell_length_c                   9.7071(19)
_cell_measurement_reflns_used    4309
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.24
_cell_measurement_theta_min      3.11
_cell_volume                     462.64(17)
_computing_cell_refinement       'CrystalClear (Rigaku, 2005)'
_computing_data_collection       'CrystalClear (Rigaku, 2005)'
_computing_data_reduction        'CrystalClear (Rigaku, 2005)'
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL/PC (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku SCXmini'
_diffrn_measurement_method       CCD_Profile_fitting
_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  0.0336
_diffrn_reflns_av_sigmaI/netI    0.0401
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4322
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         3.12
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.131
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.559
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             228
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.280
_refine_diff_density_min         -0.213
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         1811
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0598
_refine_ls_R_factor_gt           0.0483
_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^)+(0.0600P)^2^+0.1401P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1238
_refine_ls_wR_factor_ref         0.1305
_reflns_number_gt                1479
_reflns_number_total             1811
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            rz2680.cif
_cod_data_source_block           I
_cod_original_cell_volume        462.64(16)
_cod_database_code               2233286
_cod_database_fobs_code          2233286