3,4-Dinitro-1<i>H</i>-pyrazole benzene 0.25-solvate
Li, Yong-Xiang; Du, Shan; Wang, Jian-Long; Acta Crystallographica Section E 67 (2011) o1369–; doi:10.1107/S1600536811015996

data_2230560
_publ_section_title
;
 3,4-Dinitro-1<i>H</i>-pyrazole benzene 0.25-solvate
;
_journal_coeditor_code           ZS2110
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1369
_journal_paper_doi               10.1107/S1600536811015996
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '2C3 H2 N4 O4, 0.5C6 H6'
_chemical_formula_moiety         '2(C3 H2 N4 O4), 0.5(C6 H6)'
_chemical_formula_sum            'C9 H7 N8 O8'
_chemical_formula_weight         355.23
_chemical_name_common            '3,4-dinitropyrazole benzene 0.25-solvate'
_chemical_name_systematic
;
3,4-Dinitro-1<i>H</i>-pyrazole benzene 0.25-solvate
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.87(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.4579(15)
_cell_length_b                   9.787(2)
_cell_length_c                   19.534(4)
_cell_measurement_reflns_used    3256
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.09
_cell_volume                     1420.6(5)
_computing_cell_refinement       'RAPID-AUTO (Rigaku, 2000)'
_computing_data_collection       'RAPID-AUTO (Rigaku, 2000)'
_computing_data_reduction        'CrystalStructure (Rigaku, 2000)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID IP'
_diffrn_measurement_method       \w
_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  0.0839
_diffrn_reflns_av_sigmaI/netI    0.1445
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            3256
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.09
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.148
_exptl_absorpt_correction_T_max  0.9711
_exptl_absorpt_correction_T_min  0.9570
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.661
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             724
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.273
_refine_diff_density_min         -0.328
_refine_ls_extinction_coef       0.0081(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   0.918
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         3256
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.918
_refine_ls_R_factor_all          0.1350
_refine_ls_R_factor_gt           0.0601
_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^)+(0.0000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0955
_refine_ls_wR_factor_ref         0.1046
_reflns_number_gt                1267
_reflns_number_total             3256
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            zs2110.cif
_cod_data_source_block           I
_cod_original_cell_volume        1420.7(5)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2230560
_cod_database_fobs_code          2230560