Synthesis and characterization of three pyrazolate inner diazonium salts: green, powerful and stable primary explosives
Du, Yao; Zhang, Ji-Chuan; peng, Panpan; Su, Hui; Li, Sheng-Hua; Pang, Si-Ping; New J. Chem. 41 (2017) 9244–9249; doi:10.1039/C7NJ00876G

data_7056436
_publ_section_title
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 Synthesis and characterization of three pyrazolate inner diazonium salts:
 green, powerful and stable primary explosives
;
_journal_issue                   17
_journal_name_full               'New J. Chem.'
_journal_page_first              9244
_journal_page_last               9249
_journal_paper_doi               10.1039/C7NJ00876G
_journal_volume                  41
_journal_year                    2017
_chemical_formula_sum            'C3 H0 N6 O4'
_chemical_formula_weight         184.09
_chemical_name_systematic        4-diazo-3,5-dinitropyrazole
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
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2017-01-05 deposited with the CCDC.
2017-07-12 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 109.625(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   11.382(3)
_cell_length_b                   10.234(2)
_cell_length_c                   12.054(3)
_cell_measurement_reflns_used    4515
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      29.131
_cell_measurement_theta_min      2.680
_cell_volume                     1322.5(5)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  AFC10/Saturn724+
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_av_sigmaI/netI    0.0329
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13874
_diffrn_reflns_theta_full        29.13
_diffrn_reflns_theta_max         29.13
_diffrn_reflns_theta_min         2.68
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.171
_exptl_absorpt_correction_T_max  0.9538
_exptl_absorpt_correction_T_min  0.9195
_exptl_absorpt_correction_type   Multi-scans
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.849
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Chunk
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.276
_refine_diff_density_min         -0.185
_refine_diff_density_rms         0.044
_refine_ls_extinction_coef       0.007(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         3539
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0368
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0569P)^2^+0.1130P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0949
_refine_ls_wR_factor_ref         0.1018
_reflns_number_gt                3021
_reflns_number_total             3539
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7nj00876g2.cif
_cod_data_source_block           bo2541
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_cell_volume        1322.4(5)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7056436