Halogenated PETN derivatives: interplay between physical and chemical factors in explosive sensitivity.
Lease, Nicholas; Spielvogel, Kyle D.; Davis, Jack V.; Tisdale, Jeremy T.; Klamborowski, Lisa M.; Cawkwell, M. J.; Manner, Virginia W.; Chemical science 14 (2023) 7044–7056; doi:10.1039/d3sc01627g

data_1569022
_publ_section_title
;
 Halogenated PETN derivatives: interplay between physical and chemical
 factors in explosive sensitivity.
;
_journal_issue                   25
_journal_name_full               'Chemical science'
_journal_page_first              7044
_journal_page_last               7056
_journal_paper_doi               10.1039/d3sc01627g
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C5 H8 Br3 N O3'
_chemical_formula_sum            'C5 H8 Br3 N O3'
_chemical_formula_weight         369.85
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-09-22
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-03-27 deposited with the CCDC.	2023-05-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 118.747(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.0321(3)
_cell_length_b                   11.3862(5)
_cell_length_c                   7.2912(3)
_cell_measurement_reflns_used    3322
_cell_measurement_temperature    296.00
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      3.187
_cell_volume                     511.85(4)
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296.00
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker D8 Venture Duo'
_diffrn_measurement_method       'Phi and Omega Scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0819
_diffrn_reflns_av_unetI/netI     0.0726
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            17964
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.505
_diffrn_reflns_theta_min         3.187
_exptl_absorpt_coefficient_mu    11.792
_exptl_absorpt_correction_T_max  0.748
_exptl_absorpt_correction_T_min  0.585
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.105 before and 0.0658 after correction.
The Ratio of minimum to maximum transmission is 0.7829.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.400
_exptl_crystal_description       plate-like
_exptl_crystal_F_000             348
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Ethanol'
_exptl_crystal_size_max          0.053
_exptl_crystal_size_mid          0.051
_exptl_crystal_size_min          0.046
_refine_diff_density_max         0.353
_refine_diff_density_min         -0.395
_refine_diff_density_rms         0.078
_refine_ls_abs_structure_details
;
 Flack x determined using 800 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.007(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         3376
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0881
_refine_ls_R_factor_gt           0.0355
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0126P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0577
_refine_ls_wR_factor_ref         0.0672
_reflns_Friedel_coverage         0.914
_reflns_Friedel_fraction_full    0.982
_reflns_Friedel_fraction_max     0.990
_reflns_number_gt                2125
_reflns_number_total             3376
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc01627g2.cif
_cod_data_source_block           mo_petn_br3_c_0m
_cod_depositor_comments
'Adding full bibliography for 1569019--1569028.cif.'
_cod_database_code               1569022
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.590
_shelx_estimated_absorpt_t_min   0.590
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C1(H1A,H1B), C2(H2A,H2B)
;
_shelx_res_checksum              93225
_olex2_submission_special_instructions 'No special instructions were received'