N-Methylene-C bridged tetrazole and 1,2,4-triazole energetic salts as promising primary explosives
Zhang, Lingfeng; Wang, Yu; Wang, Yefeng; Liu, Shuai; Zhang, Na; Yang, Mingmin; Ma, Haixia; Guo, Zhaoqi; CrystEngComm 26 (2024) 143–152; doi:10.1039/D3CE01051A

data_7247757
_publ_section_title
;
 N-Methylene-C bridged tetrazole and 1,2,4-triazole energetic salts as
 promising primary explosives
;
_journal_issue                   2
_journal_name_full               CrystEngComm
_journal_page_first              143
_journal_page_last               152
_journal_paper_doi               10.1039/D3CE01051A
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C4 H3 N11 O4, H4 N O, 2(H2 O)'
_chemical_formula_sum            'C4 H11 N12 O7'
_chemical_formula_weight         339.25
_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   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-03-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-05-20 deposited with the CCDC.	2023-11-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.162(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   3.8946(11)
_cell_length_b                   14.070(4)
_cell_length_c                   23.813(7)
_cell_measurement_reflns_used    3100
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      22.41
_cell_measurement_theta_min      2.90
_cell_volume                     1304.0(6)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      179.97
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1808
_diffrn_reflns_av_unetI/netI     0.1088
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            16456
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.600
_diffrn_reflns_theta_min         2.896
_exptl_absorpt_coefficient_mu    0.158
_exptl_absorpt_correction_T_max  0.7448
_exptl_absorpt_correction_T_min  0.4168
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1680 before and 0.1069 after correction.
The Ratio of minimum to maximum transmission is 0.5596.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.728
_exptl_crystal_description       cube
_exptl_crystal_F_000             700
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.459
_refine_diff_density_min         -0.478
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         2418
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.1721
_refine_ls_R_factor_gt           0.1056
_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^)+(0.0888P)^2^+6.8840P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2375
_refine_ls_wR_factor_ref         0.2709
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1424
_reflns_number_total             2418
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce01051a2.cif
_cod_data_source_block           a_a
_cod_depositor_comments
'Adding full bibliography for 7247754--7247757.cif.'
_cod_original_cell_volume        1303.9(6)
_cod_database_code               7247757
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.997
_shelx_estimated_absorpt_t_min   0.984
_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
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2.a Free rotating group:
 O7(H7A,H7B), O6(H6A,H6B)
2.b Rotating group:
 N12(H12A,H12B)
2.c Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B)
2.d Aromatic/amide H refined with riding coordinates:
 N1(H1)
2.e Idealised tetrahedral OH refined as rotating group:
 O8(H8)
;
_shelx_res_checksum              25131
_olex2_submission_special_instructions 'No special instructions were received'