3-(2,4-Difluoroanilino)-9-nitrodibenzo[<i>b</i>,<i>e</i>]oxepin-11(6<i>H</i>)-one
Baur, Benjamin; Schollmeyer, Dieter; Laufer, Stefan; Acta Crystallographica Section E 67 (2011) o555–; doi:10.1107/S1600536811002881

data_2229410
_publ_section_title
;
 3-(2,4-Difluoroanilino)-9-nitrodibenzo[<i>b</i>,<i>e</i>]oxepin-11(6<i>H</i>)-one
;
_journal_coeditor_code           IM2261
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o555
_journal_paper_doi               10.1107/S1600536811002881
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C20 H12 F2 N2 O4'
_chemical_formula_moiety         'C20 H12 F2 N2 O4'
_chemical_formula_sum            'C20 H12 F2 N2 O4'
_chemical_formula_weight         382.32
_chemical_name_systematic
;
3-(2,4-Difluoroanilino)-9-nitrodibenzo[<i>b</i>,<i>e</i>]oxepin-
11(6<i>H</i>)-one
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   27.0813(15)
_cell_length_b                   13.0411(8)
_cell_length_c                   4.5998(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      69
_cell_measurement_theta_min      65
_cell_volume                     1624.51(15)
_computing_cell_refinement       '<i>CAD-4 Software</i> (Enraf--Nonius, 1989)'
_computing_data_collection       '<i>CAD-4 Software</i> (Enraf--Nonius, 1989)'
_computing_data_reduction        'CORINC (Dr\"ager & Gattow, 1971)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>, 1999)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf--Nonius CAD-4'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0505
_diffrn_reflns_av_sigmaI/netI    0.0272
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            3417
_diffrn_reflns_theta_full        69.84
_diffrn_reflns_theta_max         69.84
_diffrn_reflns_theta_min         3.26
_diffrn_standards_decay_%        3
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.075
_exptl_absorpt_correction_T_max  0.882
_exptl_absorpt_correction_T_min  0.721
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(CORINC; Dr\"ager & Gattow, 1971)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.563
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.173
_refine_diff_density_min         -0.202
_refine_ls_abs_structure_details 'Flack, (1983), 1270 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.22(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         3010
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0473
_refine_ls_shift/su_max          0.023
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0989P)^2^+0.3414P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.1255
_refine_ls_wR_factor_ref         0.1267
_reflns_number_gt                2924
_reflns_number_total             3010
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            im2261.cif
_cod_data_source_block           I
_cod_database_code               2229410
_cod_database_fobs_code          2229410