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_1572394
_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, 4(C H4 O)'
_chemical_formula_sum            'C16 H20 N16 O14'
_chemical_formula_weight         660.48
_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             2024-08-20
_audit_creation_method
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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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2024-08-20 deposited with the CCDC.	2024-08-22 downloaded from the CCDC.
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_cell_angle_alpha                105.307(4)
_cell_angle_beta                 91.114(4)
_cell_angle_gamma                99.187(4)
_cell_formula_units_Z            2
_cell_length_a                   9.2092(11)
_cell_length_b                   10.8368(13)
_cell_length_c                   14.1420(16)
_cell_measurement_reflns_used    2209
_cell_measurement_temperature    198.00
_cell_measurement_theta_max      20.945
_cell_measurement_theta_min      2.245
_cell_volume                     1341.0(3)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'Bruker APEX4'
_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      198.00
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0901
_diffrn_reflns_av_unetI/netI     0.0803
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            18604
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_min         1.977
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.144
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6496
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0841 before and 0.0681 after correction.
The Ratio of minimum to maximum transmission is 0.8712.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.636
_exptl_crystal_description       block
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.371
_refine_diff_density_min         -0.380
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     470
_refine_ls_number_reflns         4856
_refine_ls_number_restraints     112
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.1079
_refine_ls_R_factor_gt           0.0626
_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^)+(0.0659P)^2^+0.9288P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1452
_refine_ls_wR_factor_ref         0.1751
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2967
_reflns_number_total             4856
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4mh00999a3.cif
_cod_data_source_block           mo_20230228_ys_nlg_lcc_a321_0m
_cod_depositor_comments
'Adding full bibliography for 1572391--1572394.cif.'
_cod_database_code               1572394
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.986
_shelx_estimated_absorpt_t_min   0.982
_olex2_refinement_description
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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
 C8-C9 \\sim C8-C9A
 with sigma of 0.02
 C9-C10 \\sim C9A-C10
 with sigma of 0.02
 C9-N14 \\sim C9A-N14A
 with sigma of 0.02
 N14-O7 \\sim N14A-O7A
 with sigma of 0.02
 N14-O8 \\sim N14A-O8A
 with sigma of 0.02
 C8-N14 \\sim C8-N14A
 with sigma of 0.04
 C9-O7 \\sim C9A-O7A
 with sigma of 0.04
 C9-O8 \\sim C9A-O8A
 with sigma of 0.04
 C10-N14 \\sim C10-N14A
 with sigma of 0.04
 O7-O8 \\sim O7A-O8A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
O8: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
O8A \\sim N14 \\sim O8 \\sim N14A \\sim O7A \\sim O7 \\sim C9 \\sim C9A: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(O6A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(N14A)=Sof(O8A)=Sof(O7A)=Sof(C9A)=1-FVAR(1)
 Sof(C9)=Sof(N14)=Sof(O7)=Sof(O8)=FVAR(1)
 Sof(O6A)=1-FVAR(2)
 Sof(O6)=FVAR(2)
5.a X=CH2 refined with riding coordinates:
 N11(H11A,H11B), N16(H16A,H16B)
5.b Idealised Me refined as rotating group:
 C16(H16C,H16D,H16E), C15(H15A,H15B,H15C), C13(H13A,H13B,H13C), C14(H14A,H14B,
 H14C)
5.c Idealised tetrahedral OH refined as rotating group:
 O14(H14), O12(H12), O11(H11), O13(H13)
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_shelx_res_checksum              84632
_shelx_hkl_checksum              1642
_olex2_submission_special_instructions 'No special instructions were received'