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_7247697
_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 H N5 O6'
_chemical_formula_sum            'C3 H N5 O6'
_chemical_formula_weight         203.09
_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
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc29gp7q
_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                 92.197(3)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   14.2569(7)
_cell_length_b                   7.6573(6)
_cell_length_c                   16.6118(8)
_cell_measurement_reflns_used    3466
_cell_measurement_temperature    298.4
_cell_measurement_theta_max      24.19
_cell_measurement_theta_min      2.79
_cell_volume                     1812.17(19)
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      298.4
_diffrn_measured_fraction_theta_full 0.549
_diffrn_measured_fraction_theta_max 0.508
_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  0.0409
_diffrn_reflns_av_unetI/netI     0.0378
_diffrn_reflns_Laue_measured_fraction_full 0.549
_diffrn_reflns_Laue_measured_fraction_max 0.508
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10484
_diffrn_reflns_point_group_measured_fraction_full 0.549
_diffrn_reflns_point_group_measured_fraction_max 0.508
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.286
_diffrn_reflns_theta_min         2.454
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.217
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6715
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0553 before and 0.0469 after correction.
The Ratio of minimum to maximum transmission is 0.9009.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.233
_exptl_crystal_description       block
_exptl_crystal_F_000             1224
_refine_diff_density_max         0.176
_refine_diff_density_min         -0.177
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         1871
_refine_ls_number_restraints     306
_refine_ls_restrained_S_all      0.960
_refine_ls_R_factor_all          0.0546
_refine_ls_R_factor_gt           0.0366
_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^)+(0.0665P)^2^+1.0412P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0969
_refine_ls_wR_factor_ref         0.1071
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1468
_reflns_number_total             1871
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cp04526a2.cif
_cod_data_source_block           2tnp_p07
_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            'C9 H3 N15 O18'
_cod_original_formula_weight         609.26
_cod_original_formula_moiety         '3(C3 H N5 O6)'
_cod_original_formula_units_Z            4
_cod_database_code               7247697
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. 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              12770
_shelx_hkl_checksum              13117
_olex2_submission_special_instructions 'No special instructions were received'