Synthesis of high-performance insensitive energetic materials based on nitropyrazole and 1,2,4-triazole
Xu, Minxian; Cheng, Guangbin; Xiong, Hualin; Wang, Bohan; Ju, Xuehai; Yang, Hongwei; New Journal of Chemistry 43 (2019) 11157–; doi:10.1039/C9NJ01445D

data_7058479
_publ_section_title
;
 Synthesis of high-performance insensitive energetic materials based on
 nitropyrazole and 1,2,4-triazole
;
_journal_issue                   28
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              11157
_journal_paper_doi               10.1039/C9NJ01445D
_journal_volume                  43
_journal_year                    2019
_chemical_formula_moiety         'C7 H5 N13 O6, H2 O'
_chemical_formula_sum            'C7 H7 N13 O7'
_chemical_formula_weight         385.26
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2019-06-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-06-04 deposited with the CCDC.    2019-06-13 downloaded from the CCDC.
;
_cell_angle_alpha                83.380(5)
_cell_angle_beta                 66.139(5)
_cell_angle_gamma                76.502(5)
_cell_formula_units_Z            2
_cell_length_a                   8.6518(13)
_cell_length_b                   8.7863(13)
_cell_length_c                   9.9600(14)
_cell_measurement_reflns_used    1461
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.23
_cell_measurement_theta_min      3.17
_cell_volume                     673.11(17)
_computing_cell_refinement       'SCALE3 ABSPACK'
_computing_data_collection       crysalispro
_computing_data_reduction        'SCALE3 ABSPACK'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      172.9
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0812
_diffrn_reflns_av_unetI/netI     0.0966
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            5838
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.021
_diffrn_reflns_theta_max         25.021
_diffrn_reflns_theta_min         3.167
_exptl_absorpt_coefficient_mu    0.169
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6123
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.901
_exptl_crystal_description       block
_exptl_crystal_F_000             392
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.414
_refine_diff_density_min         -0.413
_refine_diff_density_rms         0.090
_refine_ls_extinction_coef       0.019(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         2337
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.1323
_refine_ls_R_factor_gt           0.0706
_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^)+(0.0753P)^2^+1.1053P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1505
_refine_ls_wR_factor_ref         0.1850
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1438
_reflns_number_total             2337
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj01445d2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7058479--7058480.cif.'
_cod_database_code               7058479
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.992
_shelx_estimated_absorpt_t_min   0.985
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 N4-H4 \\sim N5-H5 \\sim N1-H1 \\sim N10-H10 \\sim N11-H11
 with sigma of 0.02
3.a Free rotating group:
 O7(H7A,H7B)
;
_olex2_submission_special_instructions 'No special instructions were received'