#------------------------------------------------------------------------------
#$Date: 2016-03-21 17:25:37 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178782 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/36/4103602.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_4103602
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         'C1 H4 N6 O3'
_chemical_formula_sum            'C H4 N6 O3'
_chemical_formula_weight         148.10
_chemical_name_common            ANTX
_chemical_name_systematic
;
 ammonium 5-nitro-2H-tetrazol-2-olate
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_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_method           SHELXL-97
_audit_update_record
;
2010-07-05 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   9.3989(4)
_cell_length_b                   7.9263(3)
_cell_length_c                   15.2618(6)
_cell_measurement_reflns_used    3035
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      4.29
_cell_volume                     1136.98(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0191
_diffrn_reflns_av_sigmaI/netI    0.0236
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            3035
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         4.29
_exptl_absorpt_coefficient_mu    0.161
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.730
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.170
_refine_diff_density_min         -0.247
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.958
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     107
_refine_ls_number_reflns         1108
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.958
_refine_ls_R_factor_all          0.0336
_refine_ls_R_factor_gt           0.0259
_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/[σ²(Fo²)+(0.0426P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0638
_refine_ls_wR_factor_ref         0.0659
_reflns_number_gt                894
_reflns_number_total             1108
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            ja106892a_si_007.cif
_cod_data_source_block           test
_cod_database_code               4103602
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, 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 0.62467(12) -0.08646(13) 0.71317(8) 0.0132(3) Uani 1 1 d
N1 N 0.67931(11) -0.05727(11) 0.79219(7) 0.0147(2) Uani 1 1 d
N2 N 0.58957(10) -0.14727(11) 0.84033(7) 0.0137(2) Uani 1 1 d
N3 N 0.48753(11) -0.22575(12) 0.79513(7) 0.0165(3) Uani 1 1 d
N4 N 0.51096(10) -0.18475(11) 0.71151(7) 0.0155(2) Uani 1 1 d
N5 N 0.68475(11) -0.01706(12) 0.63394(7) 0.0157(3) Uani 1 1 d
N6 N 0.37236(13) -0.29954(14) 0.54759(8) 0.0161(2) Uani 1 1 d
O1 O 0.59830(9) -0.15555(9) 0.92532(5) 0.0175(2) Uani 1 1 d
O2 O 0.62057(10) -0.04430(10) 0.56524(6) 0.0222(2) Uani 1 1 d
O3 O 0.79517(9) 0.06382(11) 0.63993(6) 0.0232(2) Uani 1 1 d
H6A H 0.3670(15) -0.4178(16) 0.5505(9) 0.023(4) Uiso 1 1 d
H6B H 0.4133(17) -0.2598(18) 0.5994(11) 0.027(4) Uiso 1 1 d
H6C H 0.4298(19) -0.2761(17) 0.5029(12) 0.032(4) Uiso 1 1 d
H6D H 0.288(2) -0.255(2) 0.5448(11) 0.039(5) 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 0.0143(6) 0.0119(5) 0.0135(6) -0.0010(4) 0.0011(5) 0.0023(5)
N1 0.0144(5) 0.0154(5) 0.0142(5) 0.0007(4) 0.0018(4) 0.0001(4)
N2 0.0140(5) 0.0142(5) 0.0128(5) 0.0007(4) 0.0003(4) 0.0016(4)
N3 0.0170(5) 0.0175(5) 0.0150(6) -0.0005(4) 0.0002(4) -0.0017(4)
N4 0.0162(5) 0.0160(5) 0.0144(5) -0.0016(4) 0.0012(4) 0.0003(4)
N5 0.0181(6) 0.0140(5) 0.0150(6) -0.0003(4) 0.0020(4) 0.0016(4)
N6 0.0156(6) 0.0192(6) 0.0135(6) -0.0001(4) 0.0007(5) 0.0003(5)
O1 0.0199(5) 0.0218(4) 0.0109(5) 0.0014(3) 0.0003(4) 0.0019(4)
O2 0.0291(5) 0.0248(5) 0.0128(5) -0.0004(3) -0.0020(4) -0.0039(4)
O3 0.0201(5) 0.0252(5) 0.0244(6) 0.0024(4) 0.0026(4) -0.0083(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 115.56(10)
N4 C1 N5 121.63(10)
N1 C1 N5 122.81(10)
N2 N1 C1 99.38(9)
O1 N2 N1 122.62(9)
O1 N2 N3 122.46(9)
N1 N2 N3 114.90(10)
N2 N3 N4 105.18(9)
C1 N4 N3 104.97(9)
O3 N5 O2 124.91(11)
O3 N5 C1 117.97(10)
O2 N5 C1 117.12(10)
H6A N6 H6B 108.6(12)
H6A N6 H6C 106.1(12)
H6B N6 H6C 109.2(14)
H6A N6 H6D 110.7(13)
H6B N6 H6D 106.5(14)
H6C N6 H6D 115.7(14)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1 N4 1.3228(15)
C1 N1 1.3310(15)
C1 N5 1.4435(15)
N1 N2 1.3267(14)
N2 O1 1.3015(13)
N2 N3 1.3351(14)
N3 N4 1.3352(14)
N5 O3 1.2233(13)
N5 O2 1.2288(13)
N6 H6A 0.940(13)
N6 H6B 0.934(17)
N6 H6C 0.889(19)
N6 H6D 0.872(19)
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
N4 C1 N1 N2 0.28(12)
N5 C1 N1 N2 -179.41(10)
C1 N1 N2 O1 -178.62(9)
C1 N1 N2 N3 -0.07(11)
O1 N2 N3 N4 178.40(9)
N1 N2 N3 N4 -0.16(12)
N1 C1 N4 N3 -0.39(13)
N5 C1 N4 N3 179.31(9)
N2 N3 N4 C1 0.30(11)
N4 C1 N5 O3 -175.39(10)
N1 C1 N5 O3 4.28(16)
N4 C1 N5 O2 4.50(15)
N1 C1 N5 O2 -175.83(10)
