Design, synthesis and characterization of a carbonyl-containing high-density pyrazolotriazine-based energetic compound.
Sun, Huanyu; Zeng, Zhiwei; Chen, Chunhui; Mai, Xiancheng; Wang, Jia; Huang, Wei; Tang, Yongxing; Liu, Yuji; Organic & biomolecular chemistry 23 (2025) 9652–9657; doi:10.1039/d5ob01264c

data_7160787
_publ_section_title
;
 Design, synthesis and characterization of a carbonyl-containing
 high-density pyrazolotriazine-based energetic compound.
;
_journal_issue                   42
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              9652
_journal_page_last               9657
_journal_paper_doi               10.1039/d5ob01264c
_journal_volume                  23
_journal_year                    2025
_chemical_formula_moiety         'C42 H60 Si4 Sn'
_chemical_formula_sum            'C42 H60 Si4 Sn'
_chemical_formula_weight         795.95
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2025-03-10
_audit_creation_method           'CIF-fill 1.4w (K.Radacki, 2005-23)'
_audit_update_record
;
2025-06-19 deposited with the CCDC.	2025-10-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.3440(10)
_cell_angle_gamma                90
_cell_formula_units_Z            32
_cell_length_a                   27.8616(3)
_cell_length_b                   27.8832(3)
_cell_length_c                   44.8177(7)
_cell_measurement_reflns_used    29648
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.9920
_cell_measurement_theta_min      1.9940
_cell_volume                     34355.6(8)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)''
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 HPA
_diffrn_detector_area_resol_mean 10.0
_diffrn_detector_type            'HyPix Arc150'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
 List of Runs (angles in degrees, time in seconds):
 --------------------------------------------------------------------------
  1  \w     17.00  43.40   0.60    5.00    --   57.08-114.00  74.00   44
  2  \w     41.00  95.00   0.60    5.00    --   69.95-114.00  74.00   90
  3  \w     61.00 106.00   0.60    5.00    --   84.13-114.00  74.00   75
  4  \w     62.00  87.80   0.60    5.00    --   57.08  45.00  30.00   43
  5  \w     56.00  83.00   0.60    5.00    --   57.08-125.00-150.00   45
  6  \w      4.00  29.20   0.60    5.00    --   57.08 -30.00-120.00   42
  7  \w     23.00  49.40   0.60    5.00    --   69.95 -45.00-120.00   44
  8  \w     20.00  46.40   0.60    5.00    --   69.95 -45.00 -60.00   44
  9  \w     19.00  49.00   0.60    5.00    --   69.95 -45.00 -90.00   50
 10  \w     26.00  83.00   0.60    5.00    --   69.95 -95.00 150.00   95
 11  \w     21.00  51.60   0.60    5.00    --   69.95 -45.00 150.00   51
 12  \w     23.00  49.40   0.60    5.00    --   69.95 -45.00 -30.00   44
 13  \w     76.00 112.00   0.60    5.00    --   69.95  45.00-120.00   60
 14  \w     22.00  48.40   0.60    5.00    --   69.95 -45.00  60.00   44
 15  \w     24.00  50.40   0.60    5.00    --   69.95 -45.00-150.00   44
 16  \w     53.00  80.00   0.60    5.00    --   84.13-111.00-120.00   45
 17  \w     56.00  95.00   0.60    5.00    --   84.13 -95.00 120.00   65
 18  \w     88.00 136.00   0.60    5.00    --   84.13  30.00 -60.00   80
 19  \w     54.00 103.80   0.60    5.00    --   84.13-111.00-180.00   83
 20  \w     43.00  71.80   0.60    5.00    --   84.13 -61.00 150.00   48
 21  \w    100.00 125.80   0.60    5.00    --   84.13  45.00 -60.00   43
 22  \w     58.00  88.00   0.60    5.00    --   84.13 -77.00 -30.00   50
 23  \w     80.00 137.00   0.60    5.00    --   84.13  30.00  30.00   95
 24  \w     97.00 136.00   0.60    5.00    --   84.13  30.00-120.00   65
 25  \w     94.00 133.00   0.60    5.00    --   84.13  45.00-180.00   65
 26  \w     43.00  67.60   0.60    5.00    --   84.13 -61.00  60.00   41
 27  \w     39.00  64.80   0.60    5.00    --   84.13 -61.00 -60.00   43
 28  \w     91.00 119.80   0.60    5.00    --   84.13  45.00  60.00   48
 29  \w     39.00  63.60   0.60    5.00    --   84.13 -61.00  90.00   41
 30  \w     92.00 116.60   0.60    5.00    --   84.13  45.00  90.00   41
 31  \w    100.00 124.60   0.60    5.00    --   84.13  45.00 150.00   41
 32  \w     42.00  45.60   0.60    5.00    --   57.08-172.00-158.00    6
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy-R'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
;
 CrysAlisPro convention (1999,Acta A55,543-557)
;
_diffrn_orient_matrix_UB_11      0.0114274000
_diffrn_orient_matrix_UB_12      0.0272001000
_diffrn_orient_matrix_UB_13      0.0302373000
_diffrn_orient_matrix_UB_21      0.0174874000
_diffrn_orient_matrix_UB_22      -0.0470610000
_diffrn_orient_matrix_UB_23      0.0162387000
_diffrn_orient_matrix_UB_31      0.0519938000
_diffrn_orient_matrix_UB_32      0.0098557000
_diffrn_orient_matrix_UB_33      -0.0060048000
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_xray_symbol    K-L~2,3~
_diffrn_reflns_av_R_equivalents  0.0907
_diffrn_reflns_av_unetI/netI     0.0744
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            132993
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.251
_diffrn_reflns_theta_min         1.998
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet-R X-ray Source'
_exptl_absorpt_coefficient_mu    5.989
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.142
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
 CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022) Numerical 
 absorption correction based on gaussian integration over a multifaceted 
 crystal model Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.231
_exptl_crystal_description       plate
_exptl_crystal_F_000             13376
_exptl_crystal_preparation
;
 For data collection the crystal was immersed in a film of perfluoropolyether 
 oil, mounted on a polyimide loop and transferred to stream of cold nitrogen 
 (Oxford Cryostream 800).
;
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.010
_refine_diff_density_max         1.974
_refine_diff_density_min         -1.847
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2151
_refine_ls_number_reflns         31387
_refine_ls_number_restraints     2536
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1007
_refine_ls_R_factor_gt           0.0732
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0588P)^2^+492.2424P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1795
_refine_ls_wR_factor_ref         0.1920
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22389
_reflns_number_total             31387
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ob01264c2.cif
_cod_data_source_block           095ammd25_a
_cod_depositor_comments
'Adding full bibliography for 7160786--7160787.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7160787
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.295
_shelx_estimated_absorpt_t_max   0.943
_shelx_res_checksum              60487