#------------------------------------------------------------------------------
#$Date: 2021-10-24 20:53:08 +0300 (Sun, 24 Oct 2021) $
#$Revision: 270074 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/51/44/4514422.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_4514422
loop_
_publ_author_name
'Zhao, Gang'
'Kumar, Dheeraj'
'Hu, Lu'
'Shreeve, Jean’ne M.'
_publ_section_title
;
 A Safe and Scaled-Up Route to Inert Ammonia Oxide Hydroxylammonium Azide
 (H7N5O2), Hydrazinium Azide (H5N5), and Ammonium Azide (H4N4)
;
_journal_issue                   9
_journal_name_full               'ACS Applied Energy Materials'
_journal_page_first              6919
_journal_paper_doi               10.1021/acsaem.9b01447
_journal_volume                  2
_journal_year                    2019
_chemical_formula_moiety         'H4 N, N3'
_chemical_formula_sum            'H4 N4'
_chemical_formula_weight         60.07
_space_group_crystal_system      orthorhombic
_space_group_IT_number           53
_space_group_name_Hall           '-P 2ac 2'
_space_group_name_H-M_alt        'P m n a'
_symmetry_space_group_name_Hall  '-P 2ac 2'
_symmetry_space_group_name_H-M   'P m n a'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2019-01-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.9331(10)
_cell_length_b                   3.7824(4)
_cell_length_c                   8.6519(10)
_cell_measurement_reflns_used    3093
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      3.28
_cell_volume                     292.34(6)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'COSMO (BRUKER, V1.61, 2009)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
'SHELXL (Sheldrick, Acta Cryst. A64 2008, 112-122)'
_computing_structure_solution
'SHELXT (Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 8.36
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0276
_diffrn_reflns_av_unetI/netI     0.0118
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4901
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.482
_diffrn_reflns_theta_min         3.278
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.111
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6885
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0510 before and 0.0428 after correction. The Ratio of minimum to maximum transmission is 0.9234. The λ/2 correction factor is 0.00150.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_description       block
_exptl_crystal_F_000             128
_exptl_crystal_recrystallization_method 'used as received'
_exptl_crystal_size_max          0.273
_exptl_crystal_size_mid          0.184
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.202
_refine_diff_density_min         -0.171
_refine_diff_density_rms         0.044
_refine_ls_extinction_coef       0.16(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.179
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     34
_refine_ls_number_reflns         357
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.179
_refine_ls_R_factor_all          0.0284
_refine_ls_R_factor_gt           0.0261
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0437P)²+0.0246P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0714
_refine_ls_wR_factor_ref         0.0748
_reflns_Friedel_coverage         0.000
_reflns_number_gt                318
_reflns_number_total             357
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ae9b01447_si_002.cif
_cod_data_source_block           js119a
_cod_depositor_comments
;

2021-10-24
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'H8 N8'
_cod_original_formula_weight         120.14
_cod_original_formula_moiety         '2(H4 N), 4(N1.5)'
_cod_original_formula_units_Z            2
_cod_database_code               4514422
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.989
_shelx_estimated_absorpt_t_min   0.970
_olex2_refinement_description
;
;
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a nylon loop with paratone oil'
_olex2_submission_original_sample_id 'JS  Gang Zhao NH5 N3'
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x+1/2, y, -z+1/2'
'x, -y, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x-1/2, -y, z-1/2'
'-x, y, z'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
N1 N 0.750000 0.4555(3) 0.250000 0.0203(3) Uani 1 2 d S T P
H1A H 0.7161(10) 0.330(3) 0.3248(11) 0.033(2) Uiso 1 1 d . . .
H1B H 0.6754(11) 0.594(3) 0.2153(10) 0.035(3) Uiso 1 1 d . . .
N2 N 0.63183(10) 0.000000 0.500000 0.0269(3) Uani 1 2 d S T P
N3 N 0.500000 0.000000 0.500000 0.0191(3) Uani 1 4 d S T P
N4 N 0.500000 0.1098(3) 0.87246(10) 0.0257(3) Uani 1 2 d S T P
N5 N 0.500000 0.000000 1.000000 0.0190(3) Uani 1 4 d S T P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
H1A N1 H1A 112.8(14) . 3_655
H1A N1 H1B 109.3(9) . 3_655
H1A N1 H1B 108.2(9) . .
H1A N1 H1B 108.2(9) 3_655 3_655
H1B N1 H1A 109.3(9) . 3_655
H1B N1 H1B 108.9(13) . 3_655
N2 N3 N2 180.0 . 5_656
N4 N5 N4 180.0 . 5_657
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
N1 H1A 0.857(10) .
N1 H1A 0.857(10) 3_655
N1 H1B 0.899(10) 3_655
N1 H1B 0.899(10) .
N2 N3 1.1777(9) .
N4 N5 1.1790(8) .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N1 H1A N2 0.857(10) 2.103(10) 2.9598(7) 177.0(9) . yes
N1 H1B N4 0.899(10) 2.071(10) 2.9690(8) 177.0(9) 4_566 yes
