Advanced tetracyclic heat-resistant energetic materials based on bis(4-nitropyrazole) bridged 1,2,4-triazole.
Chen, Luyao; Hu, Wei; Lei, Caijin; Zhu, Teng; Li, Chengchuang; Tang, Jie; Cheng, Guangbin; Xiao, Chuan; Yang, Hongwei; Dalton transactions (Cambridge, England : 2003) 53 (2024) 12641–12648; doi:10.1039/d4dt01627k

data_7716531
_publ_section_title
;
 Advanced tetracyclic heat-resistant energetic materials based on
 bis(4-nitropyrazole) bridged 1,2,4-triazole.
;
_journal_issue                   30
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12641
_journal_page_last               12648
_journal_paper_doi               10.1039/d4dt01627k
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         '2(Cl O4), C10 H12 N16 O4, 3(H2 O)'
_chemical_formula_sum            'C10 H18 Cl2 N16 O15'
_chemical_formula_weight         673.30
_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             2022-08-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-11-09 deposited with the CCDC.	2024-07-02 downloaded from the CCDC.
;
_cell_angle_alpha                100.454(2)
_cell_angle_beta                 98.960(2)
_cell_angle_gamma                93.903(2)
_cell_formula_units_Z            2
_cell_length_a                   6.4237(4)
_cell_length_b                   11.3648(8)
_cell_length_c                   17.0298(12)
_cell_measurement_reflns_used    2520
_cell_measurement_temperature    170
_cell_measurement_theta_max      26.261
_cell_measurement_theta_min      2.400
_cell_volume                     1201.74(14)
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_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
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0593
_diffrn_reflns_av_unetI/netI     0.0781
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13836
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.460
_diffrn_reflns_theta_min         1.999
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.380
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6891
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0973 before and 0.0576 after correction. The Ratio of minimum to maximum transmission is 0.9245. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.861
_exptl_crystal_description       block
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.850
_refine_diff_density_min         -0.746
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     427
_refine_ls_number_reflns         4909
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.1375
_refine_ls_R_factor_gt           0.0847
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0916P)^2^+5.2254P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1985
_refine_ls_wR_factor_ref         0.2377
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3101
_reflns_number_total             4909
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01627k2.cif
_cod_data_source_block           mo_2022853_0m
_cod_depositor_comments
'Adding full bibliography for 7716530--7716531.cif.'
_cod_database_code               7716531
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.981
_shelx_estimated_absorpt_t_min   0.956
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 N10-H10
 0.87 with sigma of 0.02
 N3-H3A = N3-H3B
 0.87 with sigma of 0.02
 O10-H10B = O11-H11B
 0.87 with sigma of 0.02
 H11A-H11B
 1.46 with sigma of 0.02
 H10A-H14
 2.15 with sigma of 0.02
 H14-H10A
 2.2 with sigma of 0.02
 H10B-H11B
 2.2 with sigma of 0.02
3. Others
 Fixed Sof: O12(0.5) O16(0.5)
4.a Free rotating group:
 O11(H11A), O10(H10A), O9(H9A,H9B)
4.b Rotating group:
 N16(H16A,H16B)
4.c Aromatic/amide H refined with riding coordinates:
 N7(H7), N4(H4), N14(H14)
4.d X=CH2 refined with riding coordinates:
 N1(H1A,H1B), N15(H15A,H15B)
;
_olex2_submission_special_instructions 'No special instructions were received'