Energetic Bis(3,5-dinitro-1H-1,2,4-triazolyl)dihydro- and dichloroborates and Bis(5-nitro-2H-tetrazolyl)-, Bis(5-(trinitromethyl)-2H-tetrazolyl)-, and Bis(5-(fluorodinitromethyl)-2H-tetrazolyl)dihydroborate
Ralf Haiges; C. Bigler Jones; Karl O. Christe; Inorganic Chemistry 52 (2013) 5551–5558; doi:10.1021/ic400504h

data_4334780
_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        'Haiges, Ralf'
_publ_contact_author_phone       '+1 (213) 740-3197'
_publ_section_title
;
 Energetic Bis(3,5-dinitro-1H-1,2,4-triazolyl)dihydro- and dichloroborates
 and Bis(5-nitro-2H-tetrazolyl)-, Bis(5-(trinitromethyl)-2H-tetrazolyl)-,
 and Bis(5-(fluorodinitromethyl)-2H-tetrazolyl)dihydroborate
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5551
_journal_page_last               5558
_journal_paper_doi               10.1021/ic400504h
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C4 H2 B N10 O8, C4 H12 N'
_chemical_formula_sum            'C8 H14 B N11 O8'
_chemical_formula_weight         403.11
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                85.815(2)
_cell_angle_beta                 86.127(2)
_cell_angle_gamma                79.409(2)
_cell_formula_units_Z            4
_cell_length_a                   11.4579(5)
_cell_length_b                   12.0559(6)
_cell_length_c                   13.0552(6)
_cell_measurement_reflns_used    3698
_cell_measurement_temperature    163.(2)
_cell_measurement_theta_max      27.1879
_cell_measurement_theta_min      2.3294
_cell_volume                     1765.24(14)
_computing_cell_refinement       'APEX2 v2012.10-0 (Bruker AXS)'
_computing_data_collection       'Bruker SMART V5.632'
_computing_data_reduction        'SAINT V8.27B (Bruker AXS, 2009)'
_computing_structure_refinement  'SHELXL 2012-4 (Sheldrick, 2012)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      163.(2)
_diffrn_detector_area_resol_mean 8.3660
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.936
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       'omega- and phi-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'MoK\a '
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0208
_diffrn_reflns_av_sigmaI/netI    0.0436
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10932
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         1.57
_diffrn_source                   'fine-focus tube'
_exptl_absorpt_coefficient_mu    0.132
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.89
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS V2012/1'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.517
_exptl_crystal_description       blade
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.461
_refine_diff_density_min         -0.231
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     529
_refine_ls_number_reflns         7604
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0854
_refine_ls_R_factor_gt           0.0552
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
w=1/[\s^2^(Fo^2^)+(0.0802P)^2^+0.2997P]
where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1407
_refine_ls_wR_factor_ref         0.1615
_reflns_number_gt                4953
_reflns_number_total             7604
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic400504h_si_002_3.cif
_cod_data_source_block           TMABH2DNT2
_cod_database_code               4334780