Synthesis of novel insensitive heat-resistant explosives based on a fused-tricyclic skeleton
Jin, Gan; Lei, Caijin; Cheng, Guangbin; Yang, Hongwei; New Journal of Chemistry 48 (2024) 18120–18127; doi:10.1039/D4NJ03802A

data_7063477
_publ_section_title
;
 Synthesis of novel insensitive heat-resistant explosives based on a
 fused-tricyclic skeleton
;
_journal_issue                   42
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              18120
_journal_page_last               18127
_journal_paper_doi               10.1039/D4NJ03802A
_journal_volume                  48
_journal_year                    2024
_chemical_formula_moiety         'C6 H6 N8 O2'
_chemical_formula_sum            'C6 H6 N8 O2'
_chemical_formula_weight         222.19
_chemical_name_systematic        123
_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   mixed
_audit_creation_date             2022-12-16
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-01-19 deposited with the CCDC.	2024-10-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 117.847(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.5643(12)
_cell_length_b                   9.3620(8)
_cell_length_c                   15.0278(11)
_cell_measurement_reflns_used    2067
_cell_measurement_temperature    193.00
_cell_measurement_theta_max      24.52
_cell_measurement_theta_min      2.66
_cell_volume                     1811.8(3)
_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 0.998
_diffrn_measured_fraction_theta_max 0.995
_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  0.0839
_diffrn_reflns_av_unetI/netI     0.0658
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19688
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.496
_diffrn_reflns_theta_min         2.661
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.130
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6504
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1310 before and 0.0651 after correction.
The Ratio of minimum to maximum transmission is 0.8723.
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    1.629
_exptl_crystal_description       block
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.305
_refine_diff_density_min         -0.250
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         4141
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.1051
_refine_ls_R_factor_gt           0.0556
_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^)+(0.0658P)^2^+0.5659P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1333
_refine_ls_wR_factor_ref         0.1605
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2455
_reflns_number_total             4141
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj03802a2.cif
_cod_data_source_block           mo_20221215_zm_nlg_jg_65_0m
_cod_depositor_comments
'Adding full bibliography for 7063476--7063479.cif.'
_cod_database_code               7063477
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.986
_shelx_estimated_absorpt_t_min   0.983
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Restrained distances
 C8A-H9B
 1.6 with sigma of 0.002
 N12-C7A \\sim N12-C7
 with sigma of 0.02
 C9-C7A \\sim C9-C7
 with sigma of 0.04
 C9-C8 \\sim C9-C8A
 with sigma of 0.02
 N12-C8 \\sim N12-C8A
 with sigma of 0.04
 C7A-C8 \\sim C7-C8A
 with sigma of 0.02
 C9-H9A \\sim C9-H9B
 with sigma of 0.02
3. Others
 Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=1-FVAR(1)
 Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(C8)=Sof(H8A)=Sof(H8B)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C7A(H7AA,H7AB), C7(H7A,H7B), C8A(H8AA,H8AB), C8(H8A,H8B), C1(H1A,H1B), C2(H2A,
 H2B), C3(H3A,H3B)
;
_shelx_res_checksum              45522
_olex2_submission_special_instructions 'No special instructions were received'