An advanced furoxan-bridged heat-resistant explosive.
Li, Chengchuang; Zhu, Teng; Tang, Jie; Lei, Caijin; Yu, Guoyang; Yang, Yanqiang; Yang, Hongwei; Xiao, Chuan; Cheng, Guangbin; Materials horizons 11 (2024) 5701–5708; doi:10.1039/d4mh00999a

data_1572392
_publ_section_title
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 An advanced furoxan-bridged heat-resistant explosive.
;
_journal_issue                   22
_journal_name_full               'Materials horizons'
_journal_page_first              5701
_journal_page_last               5708
_journal_paper_doi               10.1039/d4mh00999a
_journal_volume                  11
_journal_year                    2024
_chemical_formula_moiety         'C12 H4 N16 O10, 1.75(C2 H3 N)'
_chemical_formula_sum            'C15.5 H9.25 N17.75 O10'
_chemical_formula_weight         604.16
_chemical_name_systematic        123
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-08-10
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
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_audit_update_record
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2024-08-12 deposited with the CCDC.	2024-08-22 downloaded from the CCDC.
;
_cell_angle_alpha                71.0000(10)
_cell_angle_beta                 81.949(2)
_cell_angle_gamma                88.8700(10)
_cell_formula_units_Z            2
_cell_length_a                   6.4781(2)
_cell_length_b                   13.5834(3)
_cell_length_c                   14.1528(4)
_cell_measurement_reflns_used    5200
_cell_measurement_temperature    193.00
_cell_measurement_theta_max      67.978
_cell_measurement_theta_min      3.336
_cell_volume                     1165.47(6)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      193.00
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0620
_diffrn_reflns_av_unetI/netI     0.0592
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15540
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.075
_diffrn_reflns_theta_min         3.336
_diffrn_source_current           1.1
_diffrn_source_power             0.05500000000000001
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.289
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.6664
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1052 before and 0.0462 after correction.
The Ratio of minimum to maximum transmission is 0.8849.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.722
_exptl_crystal_description       block
_exptl_crystal_F_000             613
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.486
_refine_diff_density_min         -0.490
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     437
_refine_ls_number_reflns         4229
_refine_ls_number_restraints     52
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0701
_refine_ls_R_factor_gt           0.0406
_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^)+(0.0592P)^2^+0.2332P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1022
_refine_ls_wR_factor_ref         0.1104
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3319
_reflns_number_total             4229
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4mh00999a2.cif
_cod_data_source_block           cu_20230427_zm_nlg_a_3_2_0m
_cod_depositor_comments
'Adding full bibliography for 1572391--1572394.cif.'
_cod_original_formula_sum        'C15.50 H9.25 N17.75 O10'
_cod_database_code               1572392
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.871
_shelx_estimated_absorpt_t_min   0.850
_olex2_refinement_description
;
1. Restrained distances
 N18-C15
 1.14 with sigma of 0.02
 C15-N18
 1.137 with sigma of 0.01
 C15-C16
 1.456 with sigma of 0.01
 C16-N18
 2.593 with sigma of 0.02
 N19-C17
 1.14 with sigma of 0.02
 C17-N19
 1.137 with sigma of 0.01
 C17-C18
 1.456 with sigma of 0.01
 C18-N19
 2.593 with sigma of 0.02
 N18-C16
 2.59 with sigma of 0.04
 N19-C18
 2.59 with sigma of 0.04
2. Uiso/Uaniso restraints and constraints
N18 \\sim C15 \\sim C16: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
N19 \\sim C17 \\sim C18: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
3. Rigid body (RIGU) restrains
 N18, C15, C16
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N19, C17, C18
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(O7A)=1-FVAR(1)
 Sof(O7)=FVAR(1)
 Fixed Sof: N18(0.25) C15(0.25) C16(0.25) H16A(0.25) H16B(0.25) H16C(0.25)
 N19(0.5) C17(0.5) C18(0.5) H18A(0.5) H18B(0.5) H18C(0.5)
5.a X=CH2 refined with riding coordinates:
 N5(H5A,H5B), N13(H13A,H13B)
5.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C)
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_shelx_res_checksum              8545
_shelx_hkl_checksum              1110
_olex2_submission_special_instructions 'No special instructions were received'