Synthesis of Thermally Stable and Insensitive Energetic Materials by Incorporating the Tetrazole Functionality into Fused Ring 3,6-Dinitropyrazolo-[4,3-c]Pyrazole Framework.
Xia, Honglei; Zhang, Wenquan; Jin, Yunhe; Song, Siwei; Wang, Kangcai; Zhang, Qinghua; ACS applied materials & interfaces  (2019) –; doi:10.1021/acsami.9b17384

data_4517126
_publ_section_title
;
 Synthesis of Thermally Stable and Insensitive Energetic Materials by
 Incorporating the Tetrazole Functionality into Fused Ring
 3,6-Dinitropyrazolo-[4,3-c]Pyrazole Framework.
;
_journal_name_full               'ACS applied materials &amp; interfaces'
_journal_paper_doi               10.1021/acsami.9b17384
_journal_year                    2019
_chemical_formula_moiety         '0.17(C36 K12 N84 O24)'
_chemical_formula_sum            'C6 K2 N14 O4'
_chemical_formula_weight         410.40
_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_primary     dual
_audit_creation_date             2019-05-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 94.088(2)
_cell_angle_gamma                90
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_cell_length_b                   9.8628(6)
_cell_length_c                   33.219(2)
_cell_measurement_reflns_used    2622
_cell_measurement_temperature    173
_cell_measurement_theta_max      27.372
_cell_measurement_theta_min      3.499
_cell_volume                     1983.6(2)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 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      173
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_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  0.0823
_diffrn_reflns_av_unetI/netI     0.0678
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            23060
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.505
_diffrn_reflns_theta_min         2.403
_exptl_absorpt_coefficient_mu    0.778
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6407
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0970 before and 0.0586 after correction. The Ratio of minimum to maximum transmission is 0.8593. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear whiteish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.061
_exptl_crystal_description       block
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.444
_refine_diff_density_min         -0.368
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         4527
_refine_ls_number_restraints     399
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.1514
_refine_ls_R_factor_gt           0.0486
_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^)+(0.0372P)^2^+5.2636P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1078
_refine_ls_wR_factor_ref         0.1512
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1297
_reflns_number_total             4527
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            am9b17384_si_003.cif
_cod_data_source_block           22019575_0m
_cod_database_code               4517126
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.873
_shelx_estimated_absorpt_t_min   0.847
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(O2) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(N3) \\sim
Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
;
_shelx_res_checksum              33095
_shelx_hkl_checksum              70960
_olex2_submission_special_instructions 'No special instructions were received'