<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_7717201
_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 H7 N9 O5'
_chemical_formula_sum            'C6 H7 N9 O5'
_chemical_formula_weight         285.21
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2024-07-03
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   7.2377(4)
_cell_length_b                   7.5343(4)
_cell_length_c                   38.309(2)
_cell_measurement_reflns_used    6314
_cell_measurement_temperature    108(2)
_cell_measurement_theta_max      25.93
_cell_measurement_theta_min      3.19
_cell_volume                     2089.03(19)
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      108.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0671
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            29940
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.110
_diffrn_reflns_theta_min         2.126
_exptl_absorpt_coefficient_mu    0.158
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6708
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0875 before and 0.0626 after correction.
The Ratio of minimum to maximum transmission is 0.8998.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            gold
_exptl_crystal_density_diffrn    1.814
_exptl_crystal_description       plate
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.104
_exptl_crystal_size_min          0.047
_refine_diff_density_max         0.275
_refine_diff_density_min         -0.255
_refine_diff_density_rms         0.053
_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     190
_refine_ls_number_reflns         2311
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0480
_refine_ls_R_factor_gt           0.0352
_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^+0.8158P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0807
_refine_ls_wR_factor_ref         0.0874
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1912
_reflns_number_total             2311
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02494j2.cif
_cod_data_source_block           dk_kp_cdnphy_0464_0m
_cod_depositor_comments
'Adding full bibliography for 7717200--7717201.cif.'
_cod_original_cell_volume        2089.0(2)
_cod_database_code               7717201
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.993
_shelx_estimated_absorpt_t_min   0.975
_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
2.a Rotating group:
 N9(H9A)
2.b Secondary CH2 refined with riding coordinates:
 C4(H4C,H4D)
2.c X=CH2 refined with riding coordinates:
 N4(H4A,H4B)
;
_shelx_res_checksum              38832
_shelx_hkl_checksum              89411
_olex2_submission_special_instructions 'No special instructions were received'