Crystal structure of (<i>E</i>,<i>E</i>)-2',4'-dihydroxyacetophenone azine dimethylformamide disolvate
Li, Wen-Juan; Han, Hong-Fei; Acta Crystallographica Section E 72 (2016) 467–469; doi:10.1107/S2056989016003686

data_2241596
_publ_section_title
;
 Crystal structure of (<i>E</i>,<i>E</i>)-2',4'-dihydroxyacetophenone
 azine dimethylformamide disolvate
;
_journal_coeditor_code           XU5885
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              467
_journal_page_last               469
_journal_paper_doi               10.1107/S2056989016003686
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac          'C16 H16 N2 O4, 2C3 H7 N O'
_chemical_formula_moiety         'C16 H16 N2 O4, 2(C3 H7 N O)'
_chemical_formula_sum            'C22 H30 N4 O6'
_chemical_formula_weight         446.50
_chemical_name_common
;
(<i>E</i>,<i>E</i>)-2',4'-Dihydroxyacetophenone azine
dimethylformamide disolvate
;
_chemical_name_systematic
;
4,4'-[1,1'-(Hydrazinediylidene)bis(ethan-1-yl-1-ylidene)]bis(benzene-1,3-diol)
;
_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_method           SHELXL-97
_cell_angle_alpha                96.7710(10)
_cell_angle_beta                 103.049(2)
_cell_angle_gamma                96.6070(10)
_cell_formula_units_Z            1
_cell_length_a                   6.1616(7)
_cell_length_b                   7.3109(8)
_cell_length_c                   13.4537(15)
_cell_measurement_reflns_used    1119
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.535
_cell_measurement_theta_min      3.032
_cell_volume                     579.96(11)
_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 0.983
_diffrn_measured_fraction_theta_max 0.983
_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  0.0259
_diffrn_reflns_av_sigmaI/netI    0.0479
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            2902
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.03
_exptl_absorpt_coefficient_mu    0.094
_exptl_absorpt_correction_T_max  0.9805
_exptl_absorpt_correction_T_min  0.9563
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 1996)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             238
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.284
_refine_diff_density_min         -0.248
_refine_ls_extinction_coef       0.17(2)
_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   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     149
_refine_ls_number_reflns         2001
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0825
_refine_ls_R_factor_gt           0.0554
_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^)+(0.1079P)^2^+0.0859P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1551
_refine_ls_wR_factor_ref         0.1874
_reflns_number_gt                1313
_reflns_number_total             2001
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            xu5885sup1.cif
_cod_data_source_block           I
_cod_database_code               2241596
_cod_database_fobs_code          2241596