Ethyl 2-[(2,4-difluorophenyl)hydrazinylidene]-3-oxobutanoate
Fun, Hoong-Kun; Quah, Ching Kheng; Shetty, Shobhitha; Kalluraya, Balakrishna; Acta Crystallographica Section E 68 (2012) o422–; doi:10.1107/S1600536812000803

data_2233479
_publ_section_title
;
 Ethyl 2-[(2,4-difluorophenyl)hydrazinylidene]-3-oxobutanoate
;
_journal_coeditor_code           HB6590
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o422
_journal_paper_doi               10.1107/S1600536812000803
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C12 H12 F2 N2 O3'
_chemical_formula_moiety         'C12 H12 F2 N2 O3'
_chemical_formula_sum            'C12 H12 F2 N2 O3'
_chemical_formula_weight         270.24
_chemical_name_systematic
;
Ethyl 2-[(2,4-difluorophenyl)hydrazinylidene]-3-oxobutanoate
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c 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            8
_cell_length_a                   21.814(4)
_cell_length_b                   9.0079(15)
_cell_length_c                   13.188(2)
_cell_measurement_reflns_used    3499
_cell_measurement_temperature    296
_cell_measurement_theta_max      29.80
_cell_measurement_theta_min      2.26
_cell_volume                     2591.4(8)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
'SHELXTL (Sheldrick, 2008) and PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      296
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker SMART APEXII DUO CCD'
_diffrn_measurement_method       '\f and \w 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  0.0583
_diffrn_reflns_av_sigmaI/netI    0.0562
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14829
_diffrn_reflns_theta_full        29.88
_diffrn_reflns_theta_max         29.88
_diffrn_reflns_theta_min         1.87
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.119
_exptl_absorpt_correction_T_max  0.9637
_exptl_absorpt_correction_T_min  0.9565
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>SADABS</i>; Bruker, 2009)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.377
_exptl_crystal_size_mid          0.324
_exptl_crystal_size_min          0.313
_refine_diff_density_max         0.218
_refine_diff_density_min         -0.236
_refine_ls_abs_structure_details 'Flack (1983), 3406 Friedel pairs'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         3855
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.1416
_refine_ls_R_factor_gt           0.0648
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1013P)^2^+0.7683P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1660
_refine_ls_wR_factor_ref         0.2191
_reflns_number_gt                1903
_reflns_number_total             3855
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb6590.cif
_cod_data_source_block           I
_cod_database_code               2233479
_cod_database_fobs_code          2233479