Constructing high-performance and insensitive energetic salts through increased hydrogen bonds
Chen, Luyao; Hu, Wei; Lei, Caijin; Tang, Jie; Xiao, Chuan; Cheng, Guangbin; Yang, Hongwei; CrystEngComm 27 (2025) 4976–4984; doi:10.1039/D5CE00504C

data_7250587
_publ_section_title
;
 Constructing high-performance and insensitive energetic salts through
 increased hydrogen bonds
;
_journal_issue                   29
_journal_name_full               CrystEngComm
_journal_page_first              4976
_journal_page_last               4984
_journal_paper_doi               10.1039/D5CE00504C
_journal_volume                  27
_journal_year                    2025
_chemical_formula_moiety         'C4 H8 N5 O, C N3 O6'
_chemical_formula_sum            'C5 H8 N8 O7'
_chemical_formula_weight         292.19
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2025-06-06
_audit_creation_method
;
Olex2 1.5
(compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6410)
;
_audit_update_record
;
2025-06-16 deposited with the CCDC.	2025-06-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.7340(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.3547(2)
_cell_length_b                   17.5020(4)
_cell_length_c                   8.7636(2)
_cell_measurement_reflns_used    8875
_cell_measurement_temperature    213.00
_cell_measurement_theta_max      68.203
_cell_measurement_theta_min      2.525
_cell_volume                     1061.82(5)
_computing_cell_refinement       'SAINT V8.41 (Bruker AXS LLC)'
_computing_data_collection       'APEX5 V2023.9-2 (Bruker, 2023)'
_computing_data_reduction        'SAINT V8.41 (Bruker AXS LLC)'
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      213.00
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0299
_diffrn_reflns_av_unetI/netI     0.0199
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            12759
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.219
_diffrn_reflns_theta_min         5.054
_diffrn_source_current           1.1
_diffrn_source_power             0.05500000000000001
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.494
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.6304
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1384 before and 0.0472 after correction.
The Ratio of minimum to maximum transmission is 0.8371.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'metallic light colourless'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.828
_exptl_crystal_description       block
_exptl_crystal_F_000             600
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.476
_refine_diff_density_min         -0.438
_refine_diff_density_rms         0.048
_refine_ls_extinction_coef       0.0026(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         1925
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0311
_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^)+(0.0415P)^2^+0.5140P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0833
_refine_ls_wR_factor_ref         0.0840
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1832
_reflns_number_total             1925
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00504c2.cif
_cod_data_source_block           cu_20250214_zzh_nlg_cly_2025_1
_cod_depositor_comments
'Adding full bibliography for 7250585--7250588.cif.'
_cod_database_code               7250587
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.853
_shelx_estimated_absorpt_t_min   0.807
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups, All N(H,H) groups, All N(H,H,H) groups
2. Restrained distances
 O6_$1-O6
 2.86 with sigma of 0.001
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
3.b Aromatic/amide H refined with riding coordinates:
 N3(H3)
3.c X=CH2 refined with riding coordinates:
 N5(H5A,H5B)
3.d Idealised Me refined as rotating group:
 N1(H1C,H1D,H1E)
;
_shelx_res_checksum              43532
_olex2_submission_special_instructions 'No special instructions were received'