Ethyl 2-[2-(3-methoxyphenyl)hydrazinylidene]-3-oxobutanoate
Fun, Hoong-Kun; Asik, Safra Izuani Jama; Razak, Ibrahim Abdul; Shetty, Shobhitha; Kalluraya, Balakrishna; Acta Crystallographica Section E 67 (2011) o2809–; doi:10.1107/S1600536811039444

data_2231904
_publ_section_title
;
 Ethyl 2-[2-(3-methoxyphenyl)hydrazinylidene]-3-oxobutanoate
;
_journal_coeditor_code           HB6413
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2809
_journal_paper_doi               10.1107/S1600536811039444
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C13 H16 N2 O4'
_chemical_formula_moiety         'C13 H16 N2 O4'
_chemical_formula_sum            'C13 H16 N2 O4'
_chemical_formula_weight         264.28
_chemical_name_systematic
;
Ethyl 2-[2-(3-methoxyphenyl)hydrazinylidene]-3-oxobutanoate
;
_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                77.956(2)
_cell_angle_beta                 89.394(2)
_cell_angle_gamma                72.547(2)
_cell_formula_units_Z            2
_cell_length_a                   5.7796(4)
_cell_length_b                   7.4691(5)
_cell_length_c                   16.9842(11)
_cell_measurement_reflns_used    5306
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      31.02
_cell_measurement_theta_min      2.92
_cell_volume                     682.97(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(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX DUO CCD'
_diffrn_measurement_method       '\f and \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  0.0213
_diffrn_reflns_av_sigmaI/netI    0.0198
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            11969
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.23
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.096
_exptl_absorpt_correction_T_max  0.9767
_exptl_absorpt_correction_T_min  0.9417
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>SADABS</i>; Bruker, 2009)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             280
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.223
_refine_diff_density_min         -0.203
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         3108
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0497
_refine_ls_shift/su_max_lt       0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1108P)^2^+0.0852P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1578
_refine_ls_wR_factor_ref         0.1803
_reflns_number_gt                2419
_reflns_number_total             3108
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb6413.cif
_cod_data_source_block           I
_cod_database_code               2231904
_cod_database_fobs_code          2231904