Exploring the reactive chemistry of FOX-7: synthesis of cyclic triazinane-based energetic materials featuring the FOX-7 backbone
Yan, Chao; Cheng, Guangbin; Wang, Kangcai; Liu, Tianlin; Jin, Yunhe; Yang, Hongwei; Zhang, Qinghua; New Journal of Chemistry 43 (2019) 10429–; doi:10.1039/C9NJ01932D

data_7058458
_publ_section_title
;
 Exploring the reactive chemistry of FOX-7: synthesis of cyclic
 triazinane-based energetic materials featuring the FOX-7 backbone
;
_journal_issue                   26
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              10429
_journal_paper_doi               10.1039/C9NJ01932D
_journal_volume                  43
_journal_year                    2019
_chemical_formula_moiety         '4(C7 H14 Cl N2), 4(C5 H4 N7 O8), H2 O'
_chemical_formula_sum            'C48 H74 Cl4 N36 O33'
_chemical_formula_weight         1825.23
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-02-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-05-15 deposited with the CCDC.    2019-06-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.238(4)
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   13.790(2)
_cell_length_b                   7.0973(11)
_cell_length_c                   19.700(3)
_cell_measurement_reflns_used    1026
_cell_measurement_temperature    173
_cell_measurement_theta_max      20.488
_cell_measurement_theta_min      2.985
_cell_volume                     1908.2(5)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEX 3'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0854
_diffrn_reflns_av_unetI/netI     0.0788
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            16374
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.404
_diffrn_reflns_theta_min         1.940
_exptl_absorpt_coefficient_mu    0.267
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6499
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0656 before and 0.0514 after correction.
The Ratio of minimum to maximum transmission is 0.8718.
The \l/2 correction factor is 0.00150.
;
_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    1.588
_exptl_crystal_description       block
_exptl_crystal_F_000             946
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.424
_refine_diff_density_min         -0.485
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         4304
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.1216
_refine_ls_R_factor_gt           0.0606
_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^)+(0.0663P)^2^+0.0748P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1345
_refine_ls_wR_factor_ref         0.1666
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2402
_reflns_number_total             4304
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj01932d2.cif
_cod_data_source_block           a
_cod_depositor_comments
'Adding full bibliography for 7058456--7058460.cif.'
_cod_original_cell_volume        1908.3(5)
_cod_database_code               7058458
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O3A) \\sim Ueq, Uanis(N2A) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(N2)
\\sim Ueq, Uanis(O4A) \\sim Ueq, Uanis(O4) \\sim Ueq: with sigma of 0.02 and
sigma for terminal atoms of 0.04
3. Rigid body (RIGU) restrains
 O3A, O3, N2A, N2, O4A, O4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(O3A)=Sof(N2A)=Sof(O4A)=1-FVAR(1)
 Sof(N2)=Sof(O4)=Sof(O3)=FVAR(1)
 Fixed Sof: O1W(0.25) H1WA(0.25) H1WB(0.25)
5.a Free rotating group:
 O1W(H1WA,H1WB)
5.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C9(H9A,H9B), C6(H6A,H6B), C8(H8A,H8B), C12(H12A,H12B), C7(H7A,
 H7B), C11(H11A,H11B), C3(H3A,H3B)
5.c Aromatic/amide H refined with riding coordinates:
 N5(H5), N3(H3)
;
_shelx_res_checksum              92131
_olex2_submission_special_instructions 'No special instructions were received'