Synthesis and properties of 3,4,5-trinitropyrazole-1-ol and its energetic salts
Zhang, Yanqiang; Parrish, Damon A.; Shreeve, Jean'ne M.; Journal of Materials Chemistry 22 (2012) 12659–; doi:10.1039/c2jm31535a

data_7208041
_publ_section_title
;
 Synthesis and properties of 3,4,5-trinitropyrazole-1-ol and its energetic
 salts
;
_journal_issue                   25
_journal_name_full               'Journal of Materials Chemistry'
_journal_page_first              12659
_journal_paper_doi               10.1039/c2jm31535a
_journal_volume                  22
_journal_year                    2012
_chemical_formula_moiety         'N1 H4 1+, C3 N5 O7 1-, C4 H8 O2'
_chemical_formula_sum            'C7 H12 N6 O9'
_chemical_formula_weight         324.23
_chemical_name_systematic
;
ammonium 3,4,5-trinitro-1H-pyrazol-1-olate ethyl acetate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2011-05-10
_audit_creation_method
'from SHELXTL CIF, local template and enCIFer'
_cell_angle_alpha                80.849(5)
_cell_angle_beta                 84.181(5)
_cell_angle_gamma                78.460(6)
_cell_formula_units_Z            2
_cell_length_a                   4.9047(19)
_cell_length_b                   10.001(4)
_cell_length_c                   14.952(6)
_cell_measurement_temperature    296(2)
_cell_volume                     707.6(5)
_computing_cell_refinement       'Bruker APEX2 v2010.3-0 (Bruker, 2009)'
_computing_data_collection       'Bruker APEX2 v2010.3-0 (Bruker, 2009)'
_computing_data_reduction
;
Bruker SAINT v7.68A (Bruker, 2009), Bruker XPREP v2008/2 (Bruker, 2008)
;
_computing_molecular_graphics    'Bruker SHELXTL v2008/4 (Bruker, 2008)'
_computing_publication_material  'Bruker SHELXTL v2008/4 (Bruker, 2008)'
_computing_structure_refinement  'Bruker SHELXTL v2008/4 (Bruker, 2008)'
_computing_structure_solution    'Bruker SHELXTL v2008/4 (Bruker, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0178
_diffrn_reflns_av_sigmaI/netI    0.0224
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6393
_diffrn_reflns_theta_full        26.46
_diffrn_reflns_theta_max         26.46
_diffrn_reflns_theta_min         2.10
_exptl_absorpt_coefficient_mu    0.141
_exptl_absorpt_correction_T_max  0.9643
_exptl_absorpt_correction_T_min  0.8993
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2008/1 (Bruker, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             336
_exptl_crystal_size_max          0.77
_exptl_crystal_size_mid          0.56
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.229
_refine_diff_density_min         -0.219
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     213
_refine_ls_number_reflns         2863
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0441
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0651P)^2^+0.1589P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1178
_refine_ls_wR_factor_ref         0.1243
_reflns_number_gt                2354
_reflns_number_total             2863
_reflns_threshold_expression     I>2\s(I)
_cod_duplicate_entry             7208039
_cod_data_source_file            c2jm31535a.txt
_cod_data_source_block           shrv162
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7208041