A monoclinic polymorph with <i>Z</i> = 4 of (<i>E</i>)-2,4-dihydroxyacetophenone 2,4-dinitrophenylhydrazone <i>N</i>,<i>N</i>-dimethylformamide monosolvate
Han, Hongfei; Liu, Yaohua; Acta Crystallographica Section E 67 (2011) o3434–; doi:10.1107/S1600536811050161

data_2232584
_publ_section_title
;
 A monoclinic polymorph with <i>Z</i> = 4 of
 (<i>E</i>)-2,4-dihydroxyacetophenone 2,4-dinitrophenylhydrazone
 <i>N</i>,<i>N</i>-dimethylformamide monosolvate
;
_journal_coeditor_code           BT5693
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3434
_journal_paper_doi               10.1107/S1600536811050161
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C14 H12 N4 O6, C3 H7 N O'
_chemical_formula_moiety         'C14 H12 N4 O6, C3 H7 N O'
_chemical_formula_sum            'C17 H19 N5 O7'
_chemical_formula_weight         405.37
_chemical_name_common
;
(<i>E</i>)-2,4-dihydroxyacetophenone 2,4-dinitrophenylhydrazone
<i>N</i>,<i>N</i>-dimethylformamide monosolvate
;
_chemical_name_systematic
;
4-{(1<i>E</i>)-1-[2-(2,4-dinitrophenyl)hydrazin-1-ylidene]ethyl}benzene-1,3-diol
<i>N</i>,<i>N</i>-dimethylformamide monosolvate
;
_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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.7720(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.7546(6)
_cell_length_b                   20.9647(18)
_cell_length_c                   13.3508(13)
_cell_measurement_reflns_used    1386
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      21.892
_cell_measurement_theta_min      3.033
_cell_volume                     1863.2(3)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'SMART (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       'phi and omega 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  0.0577
_diffrn_reflns_av_sigmaI/netI    0.0584
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9407
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.48
_exptl_absorpt_coefficient_mu    0.114
_exptl_absorpt_correction_T_max  0.9731
_exptl_absorpt_correction_T_min  0.9525
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.445
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.252
_refine_diff_density_min         -0.230
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.880
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         3280
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.880
_refine_ls_R_factor_all          0.1073
_refine_ls_R_factor_gt           0.0522
_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^)+(0.0687P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1188
_refine_ls_wR_factor_ref         0.1418
_reflns_number_gt                1642
_reflns_number_total             3280
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bt5693.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2232584
_cod_database_fobs_code          2232584