3,4,5-Trinitro-1-(nitromethyl)-1H-pyrazole (TNNMP): a perchlorate free high energy density oxidizer with high thermal stability
Kumar, Dheeraj; Imler, Gregory H.; Parrish, Damon A.; Shreeve, Jean'ne M.; Journal of Materials Chemistry A 5 (2017) 10437–; doi:10.1039/C7TA02585H

data_7236579
_publ_section_title
;
 3,4,5-Trinitro-1-(nitromethyl)-1H-pyrazole (TNNMP): a perchlorate free
 high energy density oxidizer with high thermal stability
;
_journal_issue                   21
_journal_name_full               'Journal of Materials Chemistry A'
_journal_page_first              10437
_journal_paper_doi               10.1039/C7TA02585H
_journal_volume                  5
_journal_year                    2017
_chemical_formula_moiety         'C4 H4 N6 O6'
_chemical_formula_sum            'C4 H4 N6 O6'
_chemical_formula_weight         232.13
_chemical_melting_point          165
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-03-07 deposited with the CCDC.
2017-05-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.282(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.7081(2)
_cell_length_b                   13.8115(5)
_cell_length_c                   9.3931(3)
_cell_measurement_reflns_used    4640
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      74.480
_cell_measurement_theta_min      3.200
_cell_volume                     858.87(5)
_computing_cell_refinement       'Bruker APEX3 v2015.5-2 (Bruker, 2015)'
_computing_data_collection       'Bruker APEX3 v2015.5-2 (Bruker, 2015)'
_computing_data_reduction
;
Bruker SAINT v8.34A (Bruker, 2013), Bruker XPREP v2014/2 (Bruker, 2014)
;
_computing_molecular_graphics    'Bruker SHELXTL v2014/7 (Bruker, 2014)'
_computing_publication_material  'Bruker SHELXTL v2014/7 (Bruker, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL v2014/7 (Bruker, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.931
_diffrn_measured_fraction_theta_max 0.905
_diffrn_measurement_device_type  'Photon 100'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'HELIOS multilayer optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_unetI/netI     0.0247
_diffrn_reflns_Laue_measured_fraction_full 0.931
_diffrn_reflns_Laue_measured_fraction_max 0.905
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            5110
_diffrn_reflns_point_group_measured_fraction_full 0.931
_diffrn_reflns_point_group_measured_fraction_max 0.905
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.471
_diffrn_reflns_theta_min         5.748
_diffrn_source                   '1uS microfocus'
_exptl_absorpt_coefficient_mu    1.502
_exptl_absorpt_correction_T_max  0.7538
_exptl_absorpt_correction_T_min  0.6215
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2014/5 (Bruker, 2008)'
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_density_diffrn    1.795
_exptl_crystal_description       block
_exptl_crystal_F_000             472
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile/methanol'
_exptl_crystal_size_max          0.364
_exptl_crystal_size_mid          0.247
_exptl_crystal_size_min          0.053
_refine_diff_density_max         0.273
_refine_diff_density_min         -0.248
_refine_diff_density_rms         0.047
_refine_ls_extinction_coef       0.0148(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     146
_refine_ls_number_reflns         1592
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0333
_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^)+(0.0429P)^2^+0.4885P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0835
_refine_ls_wR_factor_ref         0.0859
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1478
_reflns_number_total             1592
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ta02585h2.cif
_cod_data_source_block           compd2
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7236579
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.611
_shelx_estimated_absorpt_t_max   0.925