Combining 1,2,4-triazole and pyrazole frameworks for new insensitive energetic materials
Dai, Changhao; Chen, Jieyi; Tang, Jie; Cheng, Guangbin; Yang, Hongwei; New Journal of Chemistry 45 (2021) 17960–17965; doi:10.1039/D1NJ03433B

data_7060947
_publ_section_title
;
 Combining 1,2,4-triazole and pyrazole frameworks for new insensitive
 energetic materials
;
_journal_issue                   38
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              17960
_journal_page_last               17965
_journal_paper_doi               10.1039/D1NJ03433B
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety         '2(Cl O4), 3(H2 O), C7 H10 N10'
_chemical_formula_sum            'C7 H16 Cl2 N10 O11'
_chemical_formula_weight         487.20
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-08-20
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-08-20 deposited with the CCDC.	2021-08-24 downloaded from the CCDC.
;
_cell_angle_alpha                88.990(3)
_cell_angle_beta                 81.510(2)
_cell_angle_gamma                86.431(2)
_cell_formula_units_Z            2
_cell_length_a                   4.9672(3)
_cell_length_b                   12.7852(10)
_cell_length_c                   14.3081(13)
_cell_measurement_reflns_used    2267
_cell_measurement_temperature    170
_cell_measurement_theta_max      26.267
_cell_measurement_theta_min      3.195
_cell_volume                     896.93(12)
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_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      170.0
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0772
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2957
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        24.708
_diffrn_reflns_theta_max         24.708
_diffrn_reflns_theta_min         2.158
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.446
_exptl_absorpt_correction_T_max  0.745373
_exptl_absorpt_correction_T_min  0.364216
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.

Final HKLF 4 output contains 13275 reflections, Rint = 0.0794
 (7172 with I > 3sig(I), Rint = 0.0632)
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.804
_exptl_crystal_description       block
_exptl_crystal_F_000             500
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.521
_refine_diff_density_min         -0.554
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         2957
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0934
_refine_ls_R_factor_gt           0.0694
_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^)+(0.1220P)^2^+0.8247P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1758
_refine_ls_wR_factor_ref         0.1968
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2321
_reflns_number_total             2957
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj03433b2.cif
_cod_data_source_block           22020923tj_0m_4
_cod_depositor_comments          'Adding full bibliography for 7060947.cif.'
_cod_database_code               7060947
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.982
_shelx_estimated_absorpt_t_min   0.948
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.796(3)
 0.204(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
3. Restrained distances
 H6A-H5B
 2.2 with sigma of 0.02
 H6A-H6A_$1
 2.2 with sigma of 0.02
4.a Free rotating group:
 O7(H7A,H7B), O5(H5A,H5B), O6(H6A,H6B)
4.b Aromatic/amide H refined with riding coordinates:
 N7(H7), N2(H2), N5(H5), N9(H9), N3(H3), C4(H4)
4.c X=CH2 refined with riding coordinates:
 N10(H10A,H10B), N1(H1A,H1B)
;
_shelx_res_checksum              10554
_olex2_submission_special_instructions 'No special instructions were received'