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#$Date: 2016-03-21 17:24:09 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178781 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/35/4103598.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4103598
loop_
_publ_author_name
'Michael Göbel'
'Konstantin Karaghiosoff'
'Thomas M. Klapötke'
'Davin G. Piercey'
'Jörg Stierstorfer'
_publ_contact_author_address
;
Ludwig-Maximilian University,
Department of Chemistry,
Butenandtstrasse 5-13 (Haus D), 
D-81377 Munich
;
_publ_contact_author_name        'Thomas M. Klapötke'
_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         'N1 O1 H4, C1 N5 O3'
_chemical_formula_sum            'C H4 N6 O4'
_chemical_formula_weight         164.10
_chemical_name_common            HNTX
_chemical_name_systematic
;
 hydroxylammonium 5-nitro-2H-tetrazol-2-olate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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_method           SHELXL-97
_audit_update_record
;
2010-07-06 # Formatted by publCIF
;
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 91.221(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            4
_cell_length_a                   8.489(5)
_cell_length_b                   12.341(5)
_cell_length_c                   5.626(5)
_cell_measurement_reflns_used    7252
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.12
_cell_measurement_theta_min      4.61
_cell_volume                     589.3(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0282
_diffrn_reflns_av_sigmaI/netI    0.0235
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            7252
_diffrn_reflns_theta_full        26.12
_diffrn_reflns_theta_max         26.12
_diffrn_reflns_theta_min         4.61
_exptl_absorpt_coefficient_mu    0.178
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.850
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             336
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.141
_refine_diff_density_min         -0.207
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.928
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     116
_refine_ls_number_reflns         1165
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.928
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0246
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0394P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0571
_refine_ls_wR_factor_ref         0.0592
_reflns_number_gt                906
_reflns_number_total             1165
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            ja106892a_si_003.cif
_cod_data_source_block           fx203
_cod_database_code               4103598
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
C1 C 0.86750(13) 0.12919(9) 0.0128(2) 0.0178(3) Uani 1 1 d
N1 N 0.98909(11) 0.18189(7) -0.07657(17) 0.0190(2) Uani 1 1 d
N2 N 1.09911(11) 0.15220(7) 0.07883(17) 0.0172(2) Uani 1 1 d
N3 N 1.05141(11) 0.08617(8) 0.25013(18) 0.0199(2) Uani 1 1 d
N4 N 0.89773(11) 0.07104(7) 0.20622(18) 0.0198(2) Uani 1 1 d
N5 N 0.71268(11) 0.13432(8) -0.09777(18) 0.0212(2) Uani 1 1 d
N6 N 0.66342(12) -0.09441(10) 0.38723(18) 0.0199(2) Uani 1 1 d
O1 O 1.24566(8) 0.18335(6) 0.06476(14) 0.0209(2) Uani 1 1 d
O2 O 0.60730(9) 0.08274(7) -0.00371(15) 0.0271(2) Uani 1 1 d
O3 O 0.69504(11) 0.18821(8) -0.27720(17) 0.0381(3) Uani 1 1 d
O4 O 0.58689(10) -0.08244(8) 0.60555(16) 0.0311(2) Uani 1 1 d
H4 H 0.6504(17) -0.1203(12) 0.716(3) 0.044(4) Uiso 1 1 d
H6A H 0.5845(17) -0.0837(11) 0.271(3) 0.036(4) Uiso 1 1 d
H6B H 0.7005(15) -0.1626(14) 0.368(3) 0.035(4) Uiso 1 1 d
H6C H 0.7425(16) -0.0439(12) 0.369(2) 0.038(4) Uiso 1 1 d
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0224(6) 0.0145(6) 0.0165(6) -0.0016(5) 0.0025(5) -0.0016(5)
N1 0.0229(5) 0.0174(5) 0.0167(5) 0.0001(4) 0.0009(4) -0.0001(4)
N2 0.0210(5) 0.0154(5) 0.0152(5) -0.0010(4) 0.0024(4) -0.0003(4)
N3 0.0242(5) 0.0174(5) 0.0183(5) 0.0020(4) 0.0031(4) -0.0006(4)
N4 0.0234(5) 0.0172(5) 0.0190(5) 0.0003(4) 0.0025(4) -0.0004(4)
N5 0.0254(6) 0.0177(5) 0.0205(6) 0.0000(4) 0.0003(4) -0.0034(4)
N6 0.0215(6) 0.0228(6) 0.0155(5) 0.0007(4) 0.0026(4) 0.0015(5)
O1 0.0184(4) 0.0226(5) 0.0218(5) 0.0007(4) 0.0022(3) -0.0022(3)
O2 0.0238(5) 0.0312(5) 0.0265(5) 0.0014(4) 0.0025(4) -0.0084(4)
O3 0.0364(5) 0.0422(6) 0.0352(6) 0.0201(5) -0.0117(4) -0.0111(4)
O4 0.0325(5) 0.0442(6) 0.0169(5) 0.0052(4) 0.0072(4) 0.0158(4)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
N4 C1 N1 115.98(11)
N4 C1 N5 122.46(10)
N1 C1 N5 121.55(11)
N2 N1 C1 99.11(10)
O1 N2 N1 122.72(9)
O1 N2 N3 121.92(9)
N1 N2 N3 115.35(9)
N2 N3 N4 105.22(9)
C1 N4 N3 104.34(9)
O3 N5 O2 124.34(10)
O3 N5 C1 118.48(10)
O2 N5 C1 117.19(10)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1 N4 1.3240(17)
C1 N1 1.3278(15)
C1 N5 1.4435(16)
N1 N2 1.3176(14)
N2 O1 1.3061(13)
N2 N3 1.3317(15)
N3 N4 1.3357(15)
N5 O3 1.2155(15)
N5 O2 1.2270(13)
N6 O4 1.4094(16)
