Synthesis and detonation characters of 3,4,5-1<i>H</i>-trinitropyrazole and its nitrogen-rich energetic salts.
Lin, Chenchen; Yi, Pingping; Yi, Xiaoyi; He, Piao; Wang, Tingwei; Zhang, Jianguo; Dalton transactions (Cambridge, England : 2003) 53 (2024) 1430–1433; doi:10.1039/d3dt03683a

data_7714849
_publ_section_title
;
 Synthesis and detonation characters of 3,4,5-1<i>H</i>-trinitropyrazole
 and its nitrogen-rich energetic salts.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1430
_journal_page_last               1433
_journal_paper_doi               10.1039/d3dt03683a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C3 N5 O6, C2 H6 N5'
_chemical_formula_sum            'C5 H6 N10 O6'
_chemical_formula_weight         302.20
_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     dual
_audit_creation_date             2022-12-03
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2023-02-09 deposited with the CCDC.	2023-12-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.974(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.1145(5)
_cell_length_b                   8.7498(8)
_cell_length_c                   21.6564(19)
_cell_measurement_reflns_used    3642
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      25.26
_cell_measurement_theta_min      2.51
_cell_volume                     1154.27(17)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.992
_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  0.0355
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            14294
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.538
_diffrn_reflns_theta_min         1.888
_diffrn_source_current           30.0
_diffrn_source_power             1.35
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.157
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6714
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0936 before and 0.0414 after correction.
The Ratio of minimum to maximum transmission is 0.9005.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_density_diffrn    1.739
_exptl_crystal_description       block
_exptl_crystal_F_000             616
_refine_diff_density_max         0.220
_refine_diff_density_min         -0.237
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         2635
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0562
_refine_ls_R_factor_gt           0.0382
_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^)+(0.0478P)^2^+0.3363P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0921
_refine_ls_wR_factor_ref         0.1021
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2007
_reflns_number_total             2635
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03683a2.cif
_cod_data_source_block           lcc
_cod_depositor_comments          'Adding full bibliography for 7714849.cif.'
_cod_database_code               7714849
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H) groups
2.a Riding coordinates:
 N00B(H00B), N00C(H00A,H00C), N00M(H00D,H00E)
2.b Aromatic/amide H refined with riding coordinates:
 C015(H015)
;
_shelx_res_checksum              70076
_olex2_submission_special_instructions 'No special instructions were received'