Pushing the limits of energetic materials – the synthesis and characterization of dihydroxylammonium 5,5′-bistetrazole-1,1′-diolate
Fischer, Niko; Fischer, Dennis; Klapötke, Thomas M.; Piercey, Davin G.; Stierstorfer, Jörg; Journal of Materials Chemistry 22 (2012) 20418–; doi:10.1039/c2jm33646d

data_7215087
_publ_section_title
;
 Pushing the limits of energetic materials -- the synthesis and
 characterization of dihydroxylammonium
 5,5&#x2032;-bistetrazole-1,1&#x2032;-diolate
;
_journal_issue                   38
_journal_name_full               'Journal of Materials Chemistry'
_journal_page_first              20418
_journal_paper_doi               10.1039/c2jm33646d
_journal_volume                  22
_journal_year                    2012
_chemical_formula_moiety         'C2 H N8 O2, C2 H8 N '
_chemical_formula_sum            'C4 H9 N9 O2'
_chemical_formula_weight         215.20
_chemical_name_common
'dimethylammonium 5-(1-hydroxytetrazolyl)-5-(1-oxidotetrazolate'
_chemical_name_systematic
'dimethylammonium 5-(1-hydroxytetrazolyl)-5-(1-oxidotetrazolate'
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date
;
'Wed Oct 05 14:09:39 2011'
;
_audit_creation_method
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   11.660(2)
_cell_length_b                   8.7050(17)
_cell_length_c                   18.028(3)
_cell_measurement_reflns_used    1508
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      33.5921
_cell_measurement_theta_min      4.1131
_cell_volume                     1829.8(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_molecular_graphics
;
'ORTEP (M. N. Burnett, C. K. Johnson, ORTEP-III: Oak Ridge Thermal Ellipsoid
;
_computing_publication_material
'PLATON (A. L. Spek, Acta Crystallogr, Sect. A, 1990, 46, C34, 1995 version).'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-92
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 15.9809
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0060932000
_diffrn_orient_matrix_UB_12      -0.0477377000
_diffrn_orient_matrix_UB_13      0.0316979000
_diffrn_orient_matrix_UB_21      0.0085199000
_diffrn_orient_matrix_UB_22      0.0657278000
_diffrn_orient_matrix_UB_23      0.0224875000
_diffrn_orient_matrix_UB_31      -0.0599423000
_diffrn_orient_matrix_UB_32      0.0042120000
_diffrn_orient_matrix_UB_33      0.0065216000
_diffrn_radiation_collimation    0.5
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0625
_diffrn_reflns_av_sigmaI/netI    0.0528
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            8586
_diffrn_reflns_theta_full        25.75
_diffrn_reflns_theta_max         25.75
_diffrn_reflns_theta_min         4.16
_diffrn_source_current           40
_diffrn_source_type              'Spellman generator'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.128
_exptl_absorpt_correction_T_max  0.99999
_exptl_absorpt_correction_T_min  0.84718
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.562
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.241
_refine_diff_density_min         -0.200
_refine_diff_density_rms         0.054
_refine_ls_extinction_coef       0.0049(11)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         1741
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0706
_refine_ls_R_factor_gt           0.0437
_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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0993
_refine_ls_wR_factor_ref         0.1201
_reflns_number_gt                1244
_reflns_number_total             1741
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2jm33646d.txt
_cod_data_source_block           gx563_Me2NH2_1BTO
_cod_original_sg_symbol_Hall     '-P 2ac 2ab '
_cod_original_sg_symbol_H-M      'P bca'
_cod_database_code               7215087