Nitrotetrazolate-2N-oxides and the Strategy of N-Oxide Introduction
Michael Göbel; Konstantin Karaghiosoff; Thomas M. Klapötke; Davin G. Piercey; Jörg Stierstorfer; Journal of the American Chemical Society 132 (2010) 17216–17226; doi:10.1021/ja106892a

data_4103603
_publ_contact_author_address
;
Department Chemie
Ludwig-Maximilians Universit\"at
Butenandtstra\&se 5-13 (Haus D)
D-81377 M\"unchen
Bundesrepublik Deutschland
;
_publ_contact_author_email       tmk@cup.uni-muenchen.de
_publ_contact_author_fax         +49-89-2180-77491
_publ_contact_author_name        'Thomas M. Klapo\"tke'
_publ_contact_author_phone       +49-89-2180-77492
_publ_section_title
;
 Nitrotetrazolate-2N-oxides and the Strategy of N-Oxide Introduction
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17216
_journal_page_last               17226
_journal_paper_doi               10.1021/ja106892a
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C H8 N5, C N5 O3'
_chemical_formula_sum            'C2 H8 N10 O3'
_chemical_formula_weight         220.18
_chemical_name_common
'1,3-diaminoguanidinium 5-nitrotetrazolate-N-oxide'
_chemical_name_systematic
'1,3-diaminoguanidinium 5-nitrotetrazolate-N-oxide'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_author_name               'Joerg Stierstorfer'
_audit_creation_date
;
'Sat Jun 19 15:32:00 2010'
;
_audit_creation_method           SHELXL-97
_audit_update_record             29.07.2010
_cell_angle_alpha                90.218(7)
_cell_angle_beta                 94.461(7)
_cell_angle_gamma                97.519(7)
_cell_formula_units_Z            2
_cell_length_a                   6.4344(6)
_cell_length_b                   8.0055(7)
_cell_length_c                   8.5160(8)
_cell_measurement_reflns_used    1061
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.4443
_cell_measurement_theta_min      4.1418
_cell_volume                     433.53(7)
_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 0.945
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_device       'CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       omega-scan
_diffrn_orient_matrix_UB_11      -0.0399114014
_diffrn_orient_matrix_UB_12      0.0399756412
_diffrn_orient_matrix_UB_13      0.0643106041
_diffrn_orient_matrix_UB_21      -0.0783841373
_diffrn_orient_matrix_UB_22      -0.0705655712
_diffrn_orient_matrix_UB_23      0.0060073036
_diffrn_orient_matrix_UB_31      0.0693889655
_diffrn_orient_matrix_UB_32      -0.0379041386
_diffrn_orient_matrix_UB_33      0.0536194120
_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  0.0193
_diffrn_reflns_av_sigmaI/netI    0.0566
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            2989
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         4.15
_diffrn_source_current           40
_diffrn_source_type              'Spellman generator'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.148
_exptl_absorpt_correction_T_max  0.99000
_exptl_absorpt_correction_T_min  0.96689
_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    1.687
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             228
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.220
_refine_diff_density_min         -0.171
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.885
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         1889
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      0.898
_refine_ls_R_factor_all          0.0810
_refine_ls_R_factor_gt           0.0409
_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          0.0932
_refine_ls_wR_factor_ref         0.1035
_reflns_number_gt                1106
_reflns_number_total             1889
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja106892a_si_008.cif
_cod_data_source_block           fx239
_cod_database_code               4103603