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_7215085
_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_sum            'C2 H8 N10 O4'
_chemical_formula_weight         236.18
_chemical_name_common            ' bishydroxylammonium bis-1N-oxidotetrazolate'
_chemical_name_systematic        'bishydroxylammonium bis-1N-oxidotetrazolate'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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
_audit_creation_date
;
'Thu Feb 16 13:31:57 2012'
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_audit_creation_method
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
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_audit_update_record             16.02.2012
_cell_angle_alpha                90.00
_cell_angle_beta                 95.071(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   5.4408(6)
_cell_length_b                   11.7514(13)
_cell_length_c                   6.5612(9)
_cell_measurement_reflns_used    591
_cell_measurement_temperature    298
_cell_measurement_theta_max      32.2092
_cell_measurement_theta_min      4.1325
_cell_volume                     417.86(9)
_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
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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      298
_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      0.0856469000
_diffrn_orient_matrix_UB_12      -0.0426779000
_diffrn_orient_matrix_UB_13      -0.0228091000
_diffrn_orient_matrix_UB_21      0.0969899000
_diffrn_orient_matrix_UB_22      0.0404453000
_diffrn_orient_matrix_UB_23      0.0120308000
_diffrn_orient_matrix_UB_31      0.0193773000
_diffrn_orient_matrix_UB_32      -0.0136924000
_diffrn_orient_matrix_UB_33      0.1054354000
_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  0.0171
_diffrn_reflns_av_sigmaI/netI    0.0311
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            1798
_diffrn_reflns_theta_full        26.99
_diffrn_reflns_theta_max         26.99
_diffrn_reflns_theta_min         4.66
_diffrn_source_current           40
_diffrn_source_type              'Spellman generator'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.169
_exptl_absorpt_correction_T_max  0.9833
_exptl_absorpt_correction_T_min  0.9353
_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    1.877
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             244
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.233
_refine_diff_density_min         -0.224
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     89
_refine_ls_number_reflns         911
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0344
_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^)+(0.0516P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0835
_refine_ls_wR_factor_ref         0.0915
_reflns_number_gt                729
_reflns_number_total             911
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2jm33646d.txt
_cod_data_source_block           hx089_2
_cod_original_sg_symbol_Hall     -P2ybc
_cod_database_code               7215085