<i>N</i>-Methylene-C-linked nitropyrazoles and 1,2,4-triazol-3-one: thermally stable energetic materials with reduced sensitivity.
Pandey, Krishna; Das, Priyanka; Khatri, Meera; Kumar, Dheeraj; Dalton transactions (Cambridge, England : 2003) 53 (2024) 17179–17189; doi:10.1039/d4dt02494j

data_7717200
_publ_section_title
;
 <i>N</i>-Methylene-C-linked nitropyrazoles and 1,2,4-triazol-3-one:
 thermally stable energetic materials with reduced sensitivity.
;
_journal_issue                   42
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17179
_journal_page_last               17189
_journal_paper_doi               10.1039/d4dt02494j
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C6 H6 N8 O6'
_chemical_formula_sum            'C6 H6 N8 O6'
_chemical_formula_weight         286.19
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-02-11
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-09-01 deposited with the CCDC.	2024-10-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.420(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.4322(6)
_cell_length_b                   6.1733(4)
_cell_length_c                   10.2585(7)
_cell_measurement_reflns_used    8012
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.71
_cell_measurement_theta_min      2.48
_cell_volume                     519.42(6)
_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 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_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  0.0397
_diffrn_reflns_av_unetI/netI     0.0214
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            13652
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.815
_diffrn_reflns_theta_min         2.041
_exptl_absorpt_coefficient_mu    0.163
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6723
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1369 before and 0.0495 after correction.
The Ratio of minimum to maximum transmission is 0.9019.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.830
_exptl_crystal_description       plate
_exptl_crystal_F_000             292
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.144
_refine_diff_density_max         0.238
_refine_diff_density_min         -0.171
_refine_diff_density_rms         0.040
_refine_ls_abs_structure_details
;
 Flack x determined using 963 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.3(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         2208
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0266
_refine_ls_R_factor_gt           0.0259
_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^)+(0.0388P)^2^+0.0750P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0638
_refine_ls_wR_factor_ref         0.0642
_reflns_Friedel_coverage         0.825
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.991
_reflns_number_gt                2173
_reflns_number_total             2208
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02494j2.cif
_cod_data_source_block           dk_kp_tzno_0666_0m
_cod_depositor_comments
'Adding full bibliography for 7717200--7717201.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7717200
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.977
_shelx_estimated_absorpt_t_min   0.911
_olex2_refinement_description
;
1.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B)
1.b Aromatic/amide H refined with riding coordinates:
 N6(H6)
;
_shelx_res_checksum              4476
_shelx_hkl_checksum              83137
_olex2_submission_special_instructions 'No special instructions were received'