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_7056437
_publ_section_title
;
 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_moiety         'C3 H N5 O3'
_chemical_formula_sum            'C3 H N5 O3'
_chemical_formula_weight         155.09
_chemical_name_common            NCDAP
_chemical_name_systematic
'3-nitro-5-carbonyl-4-diazopyrazolate zwitterion'
_chemical_properties_physical    Heat-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
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Olex2 1.2
(compiled 2014.02.17 svn.r2891 for OlexSys, GUI svn.r4779)
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_audit_update_record
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2014-08-07 deposited with the CCDC.
2017-07-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.852(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.5357(4)
_cell_length_b                   9.1337(7)
_cell_length_c                   11.5261(8)
_cell_measurement_reflns_used    1494
_cell_measurement_temperature    293(2)
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_cell_volume                     582.47(7)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
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_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
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_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.901
_diffrn_measurement_device       'four-circle diffractometer'
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_diffrn_orient_matrix_UB_31      -0.1035527000
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_diffrn_orient_matrix_UB_33      0.0332280000
_diffrn_radiation_monochromator  graphite
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_diffrn_radiation_type           MoK\a
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_diffrn_reflns_av_unetI/netI     0.0341
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_diffrn_reflns_limit_k_min       -12
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_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5344
_diffrn_reflns_point_group_measured_fraction_full 0.998
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_diffrn_reflns_theta_max         29.570
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_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.158
_exptl_absorpt_correction_T_max  1.00000
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_exptl_absorpt_correction_type   multi-scan
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.769
_exptl_crystal_F_000             312
_exptl_crystal_size_max          0.24
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_refine_diff_density_max         0.249
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_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
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_refine_ls_R_factor_all          0.0749
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_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^)+(0.0547P)^2^+0.0045P]
 where P=(Fo^2^+2Fc^2^)/3
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_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0985
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_reflns_number_gt                995
_reflns_number_total             1468
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj00876g2.cif
_cod_data_source_block           3oh54
_cod_database_code               7056437
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'C1 H1 O1 N1'
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N8(H8)
;
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_computing_structure_solution_long 'ShelXS (Sheldrick, 2008)'