Negative linear compressibility and structural stability of the energetic material trans-hexanitrostilbene under pressure
Deng, Xinglong; Li, Dong; Fu, Boyang; Liu, Yu; He, Weilong; Li, Shourui; Cai, Weizhao; Physical Chemistry Chemical Physics  (2024) –; doi:10.1039/D4CP04470C

data_7249813
_publ_section_title
;
 Negative linear compressibility and structural stability of the energetic
 material trans-hexanitrostilbene under pressure
;
_journal_name_full               'Physical Chemistry Chemical Physics'
_journal_paper_doi               10.1039/D4CP04470C
_journal_year                    2024
_chemical_formula_moiety         '2(C7 H3 N3 O6)'
_chemical_formula_sum            'C14 H6 N6 O12'
_chemical_formula_weight         450.25
_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   difmap
_audit_creation_date             2024-10-28
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-10-28 deposited with the CCDC.	2025-01-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.52(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.443(11)
_cell_length_b                   4.6447(6)
_cell_length_c                   14.546(2)
_cell_measurement_reflns_used    809
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      23.12
_cell_measurement_theta_min      4.51
_cell_volume                     1309.6(8)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.130
_diffrn_measured_fraction_theta_max 0.120
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0907
_diffrn_reflns_av_unetI/netI     0.0644
_diffrn_reflns_Laue_measured_fraction_full 0.130
_diffrn_reflns_Laue_measured_fraction_max 0.120
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            2227
_diffrn_reflns_point_group_measured_fraction_full 0.130
_diffrn_reflns_point_group_measured_fraction_max 0.120
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.208
_diffrn_reflns_theta_min         2.803
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.205
_exptl_absorpt_correction_T_max  0.9907
_exptl_absorpt_correction_T_min  0.9595
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.284
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.2042
_exptl_crystal_size_mid          0.145
_exptl_crystal_size_min          0.046
_refine_diff_density_max         0.143
_refine_diff_density_min         -0.160
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         317
_refine_ls_number_restraints     266
_refine_ls_restrained_S_all      0.593
_refine_ls_R_factor_all          0.0991
_refine_ls_R_factor_gt           0.0752
_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^)+(0.1718P)^2^+25.8674P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1802
_refine_ls_wR_factor_ref         0.2049
_reflns_Friedel_coverage         0.000
_reflns_number_gt                234
_reflns_number_total             317
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cp04470c2.cif
_cod_data_source_block           a
_cod_database_code               7249813
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.9906
_shelx_estimated_absorpt_t_min   0.9593
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H3 of C5, H5 of C10, H2 of C3, H4 of C12
 At 1.5 times of:
  H1 of C7, H6 of C14
2. Restrained distances
 O5-H1_$7
 2.37541 with sigma of 0.005
 O4-H2_$7
 2.38523 with sigma of 0.005
 O4-H4_$7
 2.01239 with sigma of 0.005
 O3-H4_$7
 2.15806 with sigma of 0.005
 O11_$7-H6
 2.30465 with sigma of 0.005
 O10_$7-H5
 2.49321 with sigma of 0.005
 O7_$9-H6
 2.38721 with sigma of 0.005
 O1_$10-H2
 2.59 with sigma of 0.005
 O1-H1_$11
 2.05158 with sigma of 0.005
 O11_$2-H5
 2.25366 with sigma of 0.005
 O12_$2-H5
 2.45354 with sigma of 0.005
 O10_$3-H3
 2.517 with sigma of 0.005
 O5_$4-H2
 2.54564 with sigma of 0.005
 O9_$5-H3
 1.98761 with sigma of 0.005
 C7-C7_$1
 1.315 with sigma of 0.005
 C14_$6-C14
 1.3 with sigma of 0.005
 C3-C2
 1.387 with sigma of 0.005
 C3-C4
 1.369 with sigma of 0.005
 C4-C5
 1.369 with sigma of 0.005
 C5-C6
 1.373 with sigma of 0.005
 C6-C1
 1.391 with sigma of 0.005
 C1-C2
 1.401 with sigma of 0.005
 C1-C7
 1.485 with sigma of 0.005
 C2-N1
 1.476 with sigma of 0.005
 N2-C4
 1.47 with sigma of 0.005
 C6-N3
 1.47 with sigma of 0.005
 N1-O1
 1.206 with sigma of 0.005
 O3-N2
 1.228 with sigma of 0.005
 O4-N2
 1.217 with sigma of 0.005
 N3-O6
 1.22 with sigma of 0.005
 N3-O5
 1.22 with sigma of 0.005
 C8-C13
 1.394 with sigma of 0.005
 C13-C12
 1.38 with sigma of 0.005
 C12-C11
 1.371 with sigma of 0.005
 C11-C10
 1.38 with sigma of 0.005
 C10-C9
 1.385 with sigma of 0.005
 C9-C8
 1.397 with sigma of 0.005
 C8-C14
 1.486 with sigma of 0.005
 C9-N4
 1.473 with sigma of 0.005
 C13-N6
 1.469 with sigma of 0.005
 C11-N5
 1.471 with sigma of 0.005
 N5-O10
 1.22 with sigma of 0.005
 N5-O9
 1.214 with sigma of 0.005
 N6-O11
 1.223 with sigma of 0.005
 N6-O12
 1.214 with sigma of 0.005
 N4-O7
 1.208 with sigma of 0.005
 N4-O8
 1.212 with sigma of 0.005
 O1-C2
 2.311 with sigma of 0.005
 C2-O2
 2.298 with sigma of 0.005
 O3-C4
 2.301 with sigma of 0.005
 C4-O4
 2.3 with sigma of 0.005
 O5-C6
 2.305 with sigma of 0.005
 O6-C6
 2.303 with sigma of 0.005
 O12-C13
 2.296 with sigma of 0.005
 O11-C13
 2.306 with sigma of 0.005
 O10-C11
 2.294 with sigma of 0.005
 O9-C11
 2.305 with sigma of 0.005
 O8-C9
 2.304 with sigma of 0.005
 O7-C9
 2.304 with sigma of 0.005
3. Restrained planarity
 C8, C9, C10, C11, C12, N4, N5, N6
 with sigma of 0.05
 C1, C2, C3, C4, C5, C6, N1, N2, N3, C7
 with sigma of 0.05
 C9, C10, C8, O7, N4, O8
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C9) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C10) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.005 and
sigma for terminal atoms of 0.01
Uanis(O3) \\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.006
Uanis(C2) \\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.006
5.a Everything fixed:
 C7, H1, C3, H2, C5, H3, C12, H4, C10, H5, C14, H6
;
_shelx_res_checksum              57261
_olex2_submission_special_instructions 'No special instructions were received'