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_4103597
_publ_contact_author_address
;
Ludwig-Maximilian University,
Department of Chemistry,
Butenandtstrasse 5-13 (Haus D), 
D-81377 Munich
;
_publ_contact_author_name        'Thomas M. Klap\"otke'
_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 H N5 O3'
_chemical_formula_sum            'C H N5 O3'
_chemical_formula_weight         131.07
_chemical_name_common            2-hydroxy-5-Nitrotetrazole
_chemical_name_systematic
;
 5-nitro-2H-tetrazol-2-ol
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.584(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.9946(6)
_cell_length_b                   9.1402(6)
_cell_length_c                   6.2269(4)
_cell_measurement_reflns_used    3947
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.10
_cell_measurement_theta_min      4.45
_cell_volume                     448.66(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur3 CCD'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0341
_diffrn_reflns_av_sigmaI/netI    0.0271
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            3947
_diffrn_reflns_theta_full        30.10
_diffrn_reflns_theta_max         30.10
_diffrn_reflns_theta_min         4.45
_exptl_absorpt_coefficient_mu    0.185
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.940
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             264
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.144
_refine_diff_density_min         -0.175
_refine_diff_density_rms         0.035
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -10(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.921
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     86
_refine_ls_number_reflns         660
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.920
_refine_ls_R_factor_all          0.0270
_refine_ls_R_factor_gt           0.0220
_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^)+(0.0263P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0428
_refine_ls_wR_factor_ref         0.0437
_reflns_number_gt                582
_reflns_number_total             660
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja106892a_si_002.cif
_cod_data_source_block           fx245
_cod_database_code               4103597