Diethyl (<i>E</i>)-2,3-bis[(<i>E</i>)-(2-methyl-2-phenylhydrazin-1-ylidene)methyl]but-2-enedioate
Liu, Peng; Yuan, Libin; Song, Xiuqing; Yan, Hong; Acta Crystallographica Section E 70 (2014) o723–; doi:10.1107/S1600536814011970

data_2239616
_publ_section_title
;
 Diethyl
 (<i>E</i>)-2,3-bis[(<i>E</i>)-(2-methyl-2-phenylhydrazin-1-ylidene)methyl]but-2-enedioate
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o723
_journal_paper_doi               10.1107/S1600536814011970
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          'C24 H28 N4 O4'
_chemical_formula_moiety         'C24 H28 N4 O4'
_chemical_formula_sum            'C24 H28 N4 O4'
_chemical_formula_weight         436.50
_chemical_name_systematic
'Diethyl (<i>E</i>)-2,3-bis[(<i>E</i>)-(2-methyl-2-phenylhydrazin-1-ylidene)methyl]but-2-enedioate'
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                   15.922(3)
_cell_length_b                   8.0335(16)
_cell_length_c                   18.655(4)
_cell_measurement_reflns_used    6374
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.890
_cell_measurement_theta_min      2.183
_cell_volume                     2386.1(8)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC, 2005)'
_computing_data_collection       'CrystalClear (Rigaku/MSC, 2005)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC, 2005)'
_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      113(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku Saturn CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  multilayer
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0341
_diffrn_reflns_av_sigmaI/netI    0.0202
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -15
_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            14849
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.53
_exptl_absorpt_coefficient_mu    0.084
_exptl_absorpt_correction_T_max  0.9933
_exptl_absorpt_correction_T_min  0.9834
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrystalClear; Rigaku/MSC, 2005)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.215
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.181
_refine_diff_density_min         -0.163
_refine_ls_extinction_coef       0.063(4)
_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   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     168
_refine_ls_number_reflns         2093
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0411
_refine_ls_R_factor_gt           0.0377
_refine_ls_shift/su_max          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^)+(0.0585P)^2^+0.3730P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0961
_refine_ls_wR_factor_ref         0.0989
_reflns_number_gt                1925
_reflns_number_total             2093
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb7226sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        2386.2(8)
_cod_database_code               2239616
_cod_database_fobs_code          2239616