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_1572391
_publ_section_title
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 An advanced furoxan-bridged heat-resistant explosive.
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_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, C H4 O, H2 O'
_chemical_formula_sum            'C13 H10 N16 O12'
_chemical_formula_weight         582.37
_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   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-08-12
_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.
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_cell_angle_alpha                98.143(12)
_cell_angle_beta                 95.040(12)
_cell_angle_gamma                94.764(12)
_cell_formula_units_Z            2
_cell_length_a                   7.0832(19)
_cell_length_b                   11.664(3)
_cell_length_c                   13.430(4)
_cell_measurement_reflns_used    241
_cell_measurement_temperature    193.00
_cell_measurement_theta_max      49.535
_cell_measurement_theta_min      6.833
_cell_volume                     1089.0(5)
_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 0.978
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0781
_diffrn_reflns_av_unetI/netI     0.0699
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12122
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.678
_diffrn_reflns_theta_min         3.341
_diffrn_source_current           1.1
_diffrn_source_power             0.05500000000000001
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.394
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.6442
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0994 before and 0.0648 after correction.
The Ratio of minimum to maximum transmission is 0.8554.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.776
_exptl_crystal_description       block
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.295
_refine_diff_density_min         -0.286
_refine_diff_density_rms         0.075
_refine_ls_extinction_coef       0.0034(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   0.954
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     390
_refine_ls_number_reflns         3915
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      0.953
_refine_ls_R_factor_all          0.1020
_refine_ls_R_factor_gt           0.0597
_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^)+(0.1008P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1494
_refine_ls_wR_factor_ref         0.1794
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2311
_reflns_number_total             3915
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4mh00999a2.cif
_cod_data_source_block           cu_20230525_zh_nlg_lcc_a_3_y_0
_cod_depositor_comments
'Adding full bibliography for 1572391--1572394.cif.'
_cod_original_cell_volume        1089.1(5)
_cod_database_code               1572391
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.873
_shelx_estimated_absorpt_t_min   0.829
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O5A-N9
 1.2 with sigma of 0.02
 O11-H11B
 0.88 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O5A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(O5A)=1-FVAR(1)
 Sof(O5)=FVAR(1)
5.a Free rotating group:
 O11(H11A)
5.b X=CH2 refined with riding coordinates:
 N4(H4A,H4B), N15(H15A,H15B)
5.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C)
5.d Idealised tetrahedral OH refined as rotating group:
 O12(H12)
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_shelx_res_checksum              38261
_shelx_hkl_checksum              53
_olex2_submission_special_instructions 'No special instructions were received'