A Safe and Scaled-Up Route to Inert Ammonia Oxide Hydroxylammonium Azide (H7N5O2), Hydrazinium Azide (H5N5), and Ammonium Azide (H4N4)
Zhao, Gang; Kumar, Dheeraj; Hu, Lu; Shreeve, Jean’ne M.; ACS Applied Energy Materials 2 (2019) 6919–; doi:10.1021/acsaem.9b01447

data_4514421
_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_absolute_configuration unk
_chemical_formula_moiety         'H7 N2 O2, N3'
_chemical_formula_sum            'H7 N5 O2'
_chemical_formula_weight         109.11
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-02-08
_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            12
_cell_length_a                   19.9594(4)
_cell_length_b                   3.55530(10)
_cell_length_c                   19.0219(3)
_cell_measurement_reflns_used    2831
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      71.44
_cell_measurement_theta_min      8.28
_cell_volume                     1349.83(5)
_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 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w and \f'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0715
_diffrn_reflns_av_unetI/netI     0.0414
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            12824
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.127
_diffrn_reflns_theta_min         4.649
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.314
_exptl_absorpt_correction_T_max  0.7535
_exptl_absorpt_correction_T_min  0.6613
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0778 before and 0.0672 after correction. The Ratio of minimum to maximum transmission is 0.8776. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.611
_exptl_crystal_description       Needle
_exptl_crystal_F_000             696
_exptl_crystal_recrystallization_method 'used as received'
_exptl_crystal_size_max          0.292
_exptl_crystal_size_mid          0.089
_exptl_crystal_size_min          0.022
_refine_diff_density_max         0.196
_refine_diff_density_min         -0.215
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details
;
 Flack x determined using 803 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.4(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         2583
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.0585
_refine_ls_R_factor_gt           0.0402
_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/[\s^2^(Fo^2^)+(0.0548P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0930
_refine_ls_wR_factor_ref         0.1025
_reflns_Friedel_coverage         0.885
_reflns_Friedel_fraction_full    0.966
_reflns_Friedel_fraction_max     0.940
_reflns_number_gt                2035
_reflns_number_total             2583
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ae9b01447_si_004.cif
_cod_data_source_block           js219a
_cod_database_code               4514421
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.972
_shelx_estimated_absorpt_t_min   0.700
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H,H) groups
2.a Idealised Me refined as rotating group:
 N10(H10A,H10B,H10C), N15(H15A,H15B,H15C), N11(H11A,H11B,H11C), N13(H13A,H13B,
 H13C), N12(H12A,H12B,H12C), N14(H14A,H14B,H14C)
;
_shelx_res_checksum              15708
_shelx_hkl_checksum              28528
_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 GANG-42
_olex2_submission_special_instructions 'No special instructions were received'