Bis(dinitropyrazolyl)methanes spruced up with hydroxyl group: High performance energetic salts with reduced sensitivity
Bhatia, Prachi; Pandey, Krishna; Das, Priyanka; Kumar, Dheeraj; Chemical Communications  (2023) –; doi:10.1039/D3CC04445A

data_7132247
_publ_section_title
;
 Bis(dinitropyrazolyl)methanes spruced up with hydroxyl group: High
 performance energetic salts with reduced sensitivity
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D3CC04445A
_journal_year                    2023
_chemical_formula_moiety         'C7 H2 N8 O10, 2(C2 H7 N6)'
_chemical_formula_sum            'C11 H16 N20 O10'
_chemical_formula_weight         588.379
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_Int_Tables_number      15
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-08-18
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-09-07 deposited with the CCDC.	2023-10-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 121.034(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   32.034(3)
_cell_length_b                   5.3339(5)
_cell_length_c                   29.714(3)
_cell_measurement_reflns_used    6858
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      24.4746
_cell_measurement_theta_min      2.5442
_cell_volume                     4350.4(7)
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.00
_diffrn_detector_area_resol_mean 7.3910
_diffrn_measured_fraction_theta_full 0.9997
_diffrn_measured_fraction_theta_max 0.9968
_diffrn_measurement_device_type  'Bruker D8 QUEST Photon III C7'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0713
_diffrn_reflns_av_unetI/netI     0.0393
_diffrn_reflns_Laue_measured_fraction_full 0.9997
_diffrn_reflns_Laue_measured_fraction_max 0.9968
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            45335
_diffrn_reflns_point_group_measured_fraction_full 0.9997
_diffrn_reflns_point_group_measured_fraction_max 0.9968
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         26.08
_diffrn_reflns_theta_min         1.48
_exptl_absorpt_coefficient_mu    0.157
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.7170
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.797
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2418.274
_exptl_crystal_size_max          0.212
_exptl_crystal_size_mid          0.181
_exptl_crystal_size_min          0.163
_refine_diff_density_max         0.5234
_refine_diff_density_min         -0.4047
_refine_diff_density_rms         0.0771
_refine_ls_d_res_high            0.8083
_refine_ls_d_res_low             13.7243
_refine_ls_goodness_of_fit_ref   1.0708
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    17
_refine_ls_number_parameters     415
_refine_ls_number_reflns         4306
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.0702
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0418
_refine_ls_shift/su_max          0.0003
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0440P)^2^+5.8154P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0958
_refine_ls_wR_factor_ref         0.1082
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              33
_reflns_limit_h_min              -39
_reflns_limit_k_max              6
_reflns_limit_k_min              0
_reflns_limit_l_max              36
_reflns_limit_l_min              0
_reflns_number_gt                3382
_reflns_number_total             4306
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3cc04445a2.cif
_cod_data_source_block           DK_PB_PSTOT_0249
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 
;
_cod_original_cell_volume        4350.3(7)
_cod_database_code               7132247
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H) groups, H16 of N16, All N(H,H) groups
 At 1.2 times of:
  H11 of N11
2. Restrained distances
 N19-H19a
 0.89 with sigma of 0.02
 N19-H19b
 0.89 with sigma of 0.02
 H19a-H19b
 1.5 with sigma of 0.04
 C10-H19a = C10-H19b
 2 with sigma of 0.04
3.a Aromatic/amide H refined with riding coordinates:
 N11(H11)
;
_olex2_submission_special_instructions 'No special instructions were received'