Preparation and characterization of 3,5-dinitro-1H-1,2,4-triazole.
Haiges, R.; Bélanger-Chabot, G; Kaplan, S. M.; Christe, K. O.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 7586–7594; doi:10.1039/c5dt00888c

data_7034621
_publ_section_title
;
 Preparation and characterization of 3,5-dinitro-1H-1,2,4-triazole.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7586
_journal_page_last               7594
_journal_paper_doi               10.1039/c5dt00888c
_journal_volume                  44
_journal_year                    2015
_chemical_formula_sum            'C38 H30 N6.51 O3.49 P2'
_chemical_formula_weight         695.60
_chemical_name_common            PNPDNT/PNPazidonitrotriazolate
_chemical_name_systematic
'Mixed bis (triphenylphosphoranylidene)ammonium 3,5-dinitro-1,2,4-triazolate /bis (triphenylphosphoranylidene)ammonium 5-azido-3-nitro-1,2,4-triazolate'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_audit_update_record
;
2015-01-24 deposited with the CCDC.
2015-03-26 downloaded from the CCDC.
;
_cell_angle_alpha                67.1350(10)
_cell_angle_beta                 89.7880(10)
_cell_angle_gamma                76.1090(10)
_cell_formula_units_Z            2
_cell_length_a                   10.8448(6)
_cell_length_b                   11.9539(7)
_cell_length_c                   14.4364(8)
_cell_measurement_reflns_used    9922
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      30.8041
_cell_measurement_theta_min      2.3483
_cell_volume                     1665.59(16)
_computing_cell_refinement       'APEX2 v2014.11-0 (Bruker AXS, 2014)'
_computing_data_collection
'Bruker Instrument Service v2012.12.0.3 (Bruker AXS, 2012)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS, 2013)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXTL XT 2014/4 (Bruker AXS, 2014)'
_diffrn_ambient_temperature      100.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'omega- and phi-scans'
_diffrn_radiation_monochromator  'TRIUMPH curved-crystal'
_diffrn_radiation_type           'MoK\a '
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0367
_diffrn_reflns_av_unetI/netI     0.0356
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            42188
_diffrn_reflns_theta_full        31.12
_diffrn_reflns_theta_max         31.12
_diffrn_reflns_theta_min         1.54
_diffrn_source                   'fine-focus tube'
_exptl_absorpt_coefficient_mu    0.182
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.85
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5 (Bruker AXS, 2014)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.387
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             723
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetone'
_exptl_crystal_size_max          0.630
_exptl_crystal_size_mid          0.290
_exptl_crystal_size_min          0.265
_refine_diff_density_max         0.430
_refine_diff_density_min         -0.346
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.900
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     659
_refine_ls_number_reflns         10304
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.900
_refine_ls_R_factor_all          0.0516
_refine_ls_R_factor_gt           0.0377
_refine_ls_shift/su_max          0.027
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0530P)^2^+1.0479P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0931
_refine_ls_wR_factor_ref         0.1019
_reflns_number_gt                8327
_reflns_number_total             10304
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt00888c2.cif
_cod_data_source_block           DisorderedPNPDNT-azidonitrotriazole
_cod_depositor_comments
'Adding full bibliography for 7034616--7034621.cif.'
_cod_database_code               7034621
_shelx_res_checksum              40733