Synthesis and characterization of potential polycyclic energetic materials using bicyclic triazole and azetidine structures as building blocks
Yang, Xin-bo; Jia, Chen-hui; Miao, Xiang-yan; Li, Yu-chuan; Pang, Si-ping; RSC Advances 13 (2023) 2600–2610; doi:10.1039/D2RA06646G

data_7246152
_publ_section_title
;
 Synthesis and characterization of potential polycyclic energetic
 materials using bicyclic triazole and azetidine structures as building
 blocks
;
_journal_issue                   4
_journal_name_full               'RSC Advances'
_journal_page_first              2600
_journal_page_last               2610
_journal_paper_doi               10.1039/D2RA06646G
_journal_volume                  13
_journal_year                    2023
_chemical_formula_moiety         'C10 H8 Cl2 F4 N10'
_chemical_formula_sum            'C10 H8 Cl2 F4 N10'
_chemical_formula_weight         415.16
_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_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-07-27
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5370)
;
_audit_update_record
;
2017-12-08 deposited with the CCDC.	2022-12-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.03(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.950(2)
_cell_length_b                   7.2595(15)
_cell_length_c                   9.6370(19)
_cell_measurement_reflns_used    2497
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      27.4739
_cell_measurement_theta_min      2.1293
_cell_volume                     760.3(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      153.15
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_unetI/netI     0.0311
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5728
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.487
_diffrn_reflns_theta_min         3.375
_exptl_absorpt_coefficient_mu    0.494
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8187
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.813
_exptl_crystal_description       plate
_exptl_crystal_F_000             416
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.539
_refine_diff_density_min         -0.268
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     147
_refine_ls_number_reflns         1726
_refine_ls_number_restraints     62
_refine_ls_restrained_S_all      1.137
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0469
_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^)+(0.0331P)^2^+0.9628P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1049
_refine_ls_wR_factor_ref         0.1062
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1662
_reflns_number_total             1726
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ra06646g2.cif
_cod_data_source_block           201707-31a
_cod_database_code               7246152
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.952
_shelx_estimated_absorpt_t_min   0.895
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Restrained distances
 C5-C4 = C5-C4A = C5-C3A = C5-C3
 1.54 with sigma of 0.02
 N5-C4A = N5-C4 = N5-C3 = N5-C3A
 1.47 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
F2A \\sim F2 \\sim C3 \\sim C3A \\sim C4A \\sim C4: within 1.7A with sigma of
0.01 and sigma for terminal atoms of 0.01
Uanis(C3) \\sim Ueq, Uanis(C3A) \\sim Ueq, Uanis(C4A) \\sim Ueq, Uanis(C4)
\\sim Ueq, Uanis(F2A) \\sim Ueq, Uanis(F2) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.01
4. Others
 Sof(F2A)=1-FVAR(1)
 Sof(F2)=FVAR(1)
 Sof(C4A)=Sof(H4AA)=Sof(H4AB)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=1-FVAR(2)
 Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(C4)=Sof(H4A)=Sof(H4B)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C4A(H4AA,H4AB), C3A(H3AA,H3AB)
;
_olex2_submission_special_instructions 'No special instructions were received'