Concise synthesis of a fused energetic pyrazolotriazine with good performance
Shi, Haichuan; Wang, Yuqing; Wang, Xinyu; Zhang, Xiaotian; Huang, Ming; Yang, Haijun; Luo, Zhenghang; New Journal of Chemistry 48 (2024) 1212–1216; doi:10.1039/D3NJ04391F

data_7062908
_publ_section_title
;
 Concise synthesis of a fused energetic pyrazolotriazine with good
 performance
;
_journal_issue                   3
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1212
_journal_page_last               1216
_journal_paper_doi               10.1039/D3NJ04391F
_journal_volume                  48
_journal_year                    2024
_chemical_formula_moiety         'C5 H3 N7 O4, H4 O2'
_chemical_formula_sum            'C5 H7 N7 O6'
_chemical_formula_weight         261.18
_chemical_name_systematic
4-amino-3,8-dinitro-pyrazolo[5,1-c][1,2,4]triazine
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-12-01
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-12-02 deposited with the CCDC.	2023-12-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.864(16)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.2737(13)
_cell_length_b                   6.2094(8)
_cell_length_c                   9.4529(12)
_cell_measurement_reflns_used    1710
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.7260
_cell_measurement_theta_min      4.0690
_cell_volume                     493.88(13)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.909
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0383
_diffrn_reflns_av_unetI/netI     0.0966
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.909
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6317
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.909
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.146
_diffrn_reflns_theta_min         4.043
_exptl_absorpt_coefficient_mu    0.160
_exptl_absorpt_correction_T_max  0.994
_exptl_absorpt_correction_T_min  0.910
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.115a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.756
_exptl_crystal_description       block
_exptl_crystal_F_000             270
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.706
_refine_diff_density_min         -0.224
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.947
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         1318
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.947
_refine_ls_R_factor_all          0.1584
_refine_ls_R_factor_gt           0.0837
_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^)+(0.0841P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1914
_refine_ls_wR_factor_ref         0.2129
_reflns_Friedel_coverage         0.000
_reflns_number_gt                560
_reflns_number_total             1318
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj04391f2.cif
_cod_data_source_block           2022_2b_autored
_cod_depositor_comments
'Adding full bibliography for 7062908--7062909.cif.'
_cod_database_code               7062908
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.972
_shelx_estimated_absorpt_t_min   0.966
_olex2_refinement_description
;
1. Others
 Fixed Sof: H5A(0.5) H5B(0.5) H6C(0.5) H6D(0.5)
2.a Riding coordinates:
 O5(H5A,H5B), O6(H6C,H6D)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5)
2.c X=CH2 refined with riding coordinates:
 N6(H6A,H6B)
;
_shelx_res_checksum              62523
_olex2_submission_special_instructions 'No special instructions were received'