Energetic High-Nitrogen Compounds: 5-(Trinitromethyl)-2H-tetrazole and -tetrazolates, Preparation, Characterization, and Conversion into 5-(Dinitromethyl)tetrazoles
Ralf Haiges; Karl O. Christe; Inorganic Chemistry 52 (2013) 7249–7260; doi:10.1021/ic400919n

data_4335263
_publ_contact_author_address
;
University of Southern California
Loker Hydrocarbon Research Institute and Department of Chemistry
Los Angeles, CA 90089
USA
;
_publ_contact_author_email       haiges@usc.edu
_publ_contact_author_name        'Ralf Haiges'
_publ_contact_author_phone       '+1 (213) 740-3197'
_publ_section_title
;
 Energetic High-Nitrogen Compounds: 5-(Trinitromethyl)-2H-tetrazole and
 -tetrazolates, Preparation, Characterization, and Conversion into
 5-(Dinitromethyl)tetrazoles
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7249
_journal_page_last               7260
_journal_paper_doi               10.1021/ic400919n
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C2 N7 O6, N H4'
_chemical_formula_sum            'C2 H4 N8 O6'
_chemical_formula_weight         236.13
_chemical_name_common            'ammonium 5-trinitromethyltetrazolate'
_chemical_name_systematic        NH4TNTz
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                104.8260(10)
_cell_angle_beta                 91.8040(10)
_cell_angle_gamma                109.1510(10)
_cell_formula_units_Z            2
_cell_length_a                   7.0369(3)
_cell_length_b                   7.3590(3)
_cell_length_c                   9.1760(4)
_cell_measurement_temperature    100.(2)
_cell_volume                     430.45(3)
_computing_cell_refinement       'APEX2 v2012.4-3 (Bruker AXS)'
_computing_data_collection       'Bruker Instrument Service v2012.6-0'
_computing_data_reduction        'SAINT V8.18C (Bruker AXS, 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.979
_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  0.0262
_diffrn_reflns_av_sigmaI/netI    0.0241
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10695
_diffrn_reflns_theta_full        29.00
_diffrn_reflns_theta_max         30.58
_diffrn_reflns_theta_min         2.31
_diffrn_source                   'fine-focus tube'
_exptl_absorpt_coefficient_mu    0.175
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.94
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS V2008/1'
_exptl_crystal_density_diffrn    1.822
_exptl_crystal_F_000             240
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.140
_refine_diff_density_max         0.391
_refine_diff_density_min         -0.290
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     159
_refine_ls_number_reflns         2585
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0318
_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^)+(0.0390P)^2^+0.1028P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0777
_refine_ls_wR_factor_ref         0.0819
_reflns_number_gt                2168
_reflns_number_total             2585
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400919n_si_001_3.cif
_cod_data_source_block           NH4TNTz
_cod_database_code               4335263