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_7215086
_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 H2 N8 O2, 2(C H4 O)'
_chemical_formula_sum            'C4 H10 N8 O4'
_chemical_formula_weight         234.20
_chemical_name_common            '5,5-bis(1-hydroxy-tetrazole) dimethanolate'
_chemical_name_systematic        '5,5-bis(1-hydroxy-tetrazole) dimethanolate'
_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
;
'Thu May 26 23:52:59 2011'
;
_audit_creation_method           SHELXL-97
_audit_update_record             30.05.2011
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.6818(10)
_cell_length_b                   6.7692(12)
_cell_length_c                   18.884(3)
_cell_measurement_reflns_used    851
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      35.1422
_cell_measurement_theta_min      4.1362
_cell_volume                     982.0(3)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.27p5 beta (release 01-04-2005 CrysAlis171 .NET)
(compiled Apr 1 2005,17:53:34)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.27p5 beta (release 01-04-2005 CrysAlis171 .NET)
(compiled Apr 1 2005,17:53:34)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.27p5 beta (release 01-04-2005 CrysAlis171 .NET)
(compiled Apr 1 2005,17:53:34)
;
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       omega-scan
_diffrn_orient_matrix_UB_11      -0.0720624875
_diffrn_orient_matrix_UB_12      0.0604957715
_diffrn_orient_matrix_UB_13      0.0119501115
_diffrn_orient_matrix_UB_21      0.0243713148
_diffrn_orient_matrix_UB_22      -0.0200182066
_diffrn_orient_matrix_UB_23      0.0356519630
_diffrn_orient_matrix_UB_31      0.0725655716
_diffrn_orient_matrix_UB_32      0.0669855519
_diffrn_orient_matrix_UB_33      -0.0000773298
_diffrn_radiation_collimation    0.5
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0678
_diffrn_reflns_av_sigmaI/netI    0.0705
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4803
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         4.16
_diffrn_source_current           40
_diffrn_source_type              'Spellman generator'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.138
_exptl_absorpt_correction_T_max  0.99999
_exptl_absorpt_correction_T_min  0.88533
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;SCALE3 ABSPACK - An Oxford Diffraction program (1.0.4,gui:1.0.3)
(C) 2005 Oxford Diffraction Ltd.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.584
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             488
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.31
_refine_diff_density_max         0.293
_refine_diff_density_min         -0.219
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.841
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     93
_refine_ls_number_reflns         968
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.841
_refine_ls_R_factor_all          0.0767
_refine_ls_R_factor_gt           0.0404
_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          0.0827
_refine_ls_wR_factor_ref         0.0891
_reflns_number_gt                555
_reflns_number_total             968
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2jm33646d.txt
_cod_data_source_block           gx320
_cod_original_sg_symbol_Hall     ' -P 2ac 2ab'
_cod_original_sg_symbol_H-M      'P bca'
_cod_database_code               7215086