Improving the anti-hygroscopicity and safety of hydroxylamine pentazolate salt (NH3OH+N5−) by cocrystallization
Chen, Lei; Shen, Zhili; Kong, Deren; Zhang, Chong; Hu, Bingcheng; Gao, Chao; CrystEngComm 27 (2025) 5312–5318; doi:10.1039/D5CE00437C

data_7250683
_publ_section_title
;
 Improving the anti-hygroscopicity and safety of hydroxylamine pentazolate
 salt (NH3OH+N5&#x2212;) by cocrystallization
;
_journal_issue                   31
_journal_name_full               CrystEngComm
_journal_page_first              5312
_journal_page_last               5318
_journal_paper_doi               10.1039/D5CE00437C
_journal_volume                  27
_journal_year                    2025
_chemical_formula_moiety         'H4 N O, N5'
_chemical_formula_sum            'H4 N6 O'
_chemical_formula_weight         104.09
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2025-04-08
_audit_creation_method
;
Olex2 1.5
(compiled 2025.03.04 svn.red2d20d0 for OlexSys, GUI svn.r7188)
;
_audit_update_record
;
2025-04-23 deposited with the CCDC.	2025-07-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.582(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   3.7631(2)
_cell_length_b                   14.7655(7)
_cell_length_c                   7.6847(4)
_cell_measurement_reflns_used    2755
_cell_measurement_temperature    193.00
_cell_measurement_theta_max      27.34
_cell_measurement_theta_min      3.00
_cell_volume                     424.18(4)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      193.00
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0596
_diffrn_reflns_av_unetI/netI     0.0249
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            10009
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.508
_diffrn_reflns_theta_min         2.759
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.144
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7048
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1189 before and 0.0600 after correction.
The Ratio of minimum to maximum transmission is 0.9453.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.630
_exptl_crystal_description       block
_exptl_crystal_F_000             216
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.158
_refine_diff_density_min         -0.195
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     70
_refine_ls_number_reflns         968
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0293
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0412P)^2^+0.0754P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0781
_refine_ls_wR_factor_ref         0.0813
_reflns_Friedel_coverage         0.000
_reflns_number_gt                821
_reflns_number_total             968
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00437c1.cif
_cod_data_source_block           mo_20250407_ys_nlg_qa_aeo_0m
_cod_depositor_comments
'Adding full bibliography for 7250682--7250683.cif.'
_cod_database_code               7250683
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.984
_shelx_estimated_absorpt_t_min   0.979
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups, All O(H) groups
2.a Rotating group:
 O1(H1), N6(H6A,H6B)
;
_shelx_res_checksum              68032
_olex2_submission_special_instructions 'No special instructions were received'