High-pressure structural studies and pressure-induced sensitisation of 3,4,5-trinitro-1<i>H</i>-pyrazole.
Atceken, Nurunnisa; Hemingway, Jack; Bull, Craig L.; Liu, Xiaojiao; Michalchuk, Adam A. L.; Konar, Sumit; Morrison, Carole A.; Pulham, Colin R.; Physical chemistry chemical physics : PCCP 25 (2023) 31646–31654; doi:10.1039/d3cp04526a

data_7247695
_publ_section_title
;
 High-pressure structural studies and pressure-induced sensitisation of
 3,4,5-trinitro-1<i>H</i>-pyrazole.
;
_journal_issue                   46
_journal_name_full               'Physical chemistry chemical physics : PCCP'
_journal_page_first              31646
_journal_page_last               31654
_journal_paper_doi               10.1039/d3cp04526a
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         'C3 N5 O6'
_chemical_formula_sum            'C3 N5 O6'
_chemical_formula_weight         202.08
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc29gp8r
_audit_creation_date             2021-12-16
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2021-12-16 deposited with the CCDC.	2023-11-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 127.623(5)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   19.319(2)
_cell_length_b                   7.5668(13)
_cell_length_c                   14.458(3)
_cell_measurement_reflns_used    1713
_cell_measurement_temperature    287.2
_cell_measurement_theta_max      24.47
_cell_measurement_theta_min      2.86
_cell_volume                     1674.0(5)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      287.2
_diffrn_measured_fraction_theta_full 0.550
_diffrn_measured_fraction_theta_max 0.550
_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  0.0320
_diffrn_reflns_av_unetI/netI     0.0488
_diffrn_reflns_Laue_measured_fraction_full 0.550
_diffrn_reflns_Laue_measured_fraction_max 0.550
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            3579
_diffrn_reflns_point_group_measured_fraction_full 0.506
_diffrn_reflns_point_group_measured_fraction_max 0.505
_diffrn_reflns_theta_full        25.022
_diffrn_reflns_theta_max         25.022
_diffrn_reflns_theta_min         2.662
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.235
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6076
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.405
_exptl_crystal_description       block
_exptl_crystal_F_000             1212
_refine_diff_density_max         0.227
_refine_diff_density_min         -0.259
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details
;
 Flack x determined using 539 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -2.4(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         1493
_refine_ls_number_restraints     317
_refine_ls_restrained_S_all      0.920
_refine_ls_R_factor_all          0.0522
_refine_ls_R_factor_gt           0.0416
_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^)+(0.0927P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1072
_refine_ls_wR_factor_ref         0.1137
_reflns_Friedel_coverage         0.836
_reflns_Friedel_fraction_full    0.461
_reflns_Friedel_fraction_max     0.461
_reflns_number_gt                1292
_reflns_number_total             1493
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cp04526a2.cif
_cod_data_source_block           2tnp_p10_h
_cod_depositor_comments
;
Adding full bibliography for 7247689--7247697.cif.

2024-11-08
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C18 N30 O36'
_cod_original_formula_weight         1212.48
_cod_original_formula_moiety         '6(C3 N5 O6)'
_cod_original_formula_units_Z            2
_cod_database_code               7247695
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Restrained distances
 C00W-C00M \\sim C00W-C00I
 with sigma of 0.02
 N4-C00M \\sim N00A-C00I
 with sigma of 0.02
 C00M-N4 \\sim C00I-N00A
 with sigma of 0.02
 C00I-N00A \\sim N4-C00M
 with sigma of 0.05
 N4-C00M \\sim N9-C00V
 with sigma of 0.02
 N00A-C00I \\sim N4-C00M
 with sigma of 0.1
 C00W-C00I \\sim C00W-C00M
 with sigma of 0.1
2. Restrained planarity
 N00A, C00I, C00W, C00M, N4
 with sigma of 0.1
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
;
_shelx_res_checksum              28772
_shelx_hkl_checksum              25486
_olex2_submission_special_instructions 'No special instructions were received'