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_4335267
_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         'C12 Ag4 N42 O36, 2(Ag H6 N2)'
_chemical_formula_sum            'C12 H12 Ag6 N46 O36'
_chemical_formula_weight         2023.90
_chemical_name_common            AgTNTz
_chemical_name_systematic        'Silver 5-trinitromethyltetrazolate amine'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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
_cell_angle_alpha                90
_cell_angle_beta                 91.600(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.7121(19)
_cell_length_b                   22.171(4)
_cell_length_c                   21.479(3)
_cell_measurement_temperature    100.(2)
_cell_volume                     5575.3(16)
_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 1.000
_diffrn_measured_fraction_theta_max 0.986
_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  0.0701
_diffrn_reflns_av_sigmaI/netI    0.0457
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            130059
_diffrn_reflns_theta_full        29.00
_diffrn_reflns_theta_max         30.50
_diffrn_reflns_theta_min         1.32
_diffrn_source                   'fine-focus tube'
_exptl_absorpt_coefficient_mu    2.208
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.48
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS V2008/1'
_exptl_crystal_density_diffrn    2.411
_exptl_crystal_F_000             3904
_exptl_crystal_size_max          0.487
_exptl_crystal_size_mid          0.188
_exptl_crystal_size_min          0.106
_refine_diff_density_max         1.408
_refine_diff_density_min         -4.710
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     908
_refine_ls_number_reflns         16785
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0803
_refine_ls_R_factor_gt           0.0494
_refine_ls_shift/su_max          0.028
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0525P)^2^+45.0309P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1223
_refine_ls_wR_factor_ref         0.1380
_reflns_number_gt                11975
_reflns_number_total             16785
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400919n_si_001_7.cif
_cod_data_source_block           AgTNTz
_cod_original_cell_volume        5575.3(15)
_cod_database_code               4335267