Crystal structure of ethyl (<i>E</i>)-4-(4-chlorophenyl)-4-methoxy-2-oxobut-3-enoate
Flores, Darlene Correia; de Vicenti, Juliano Rosa; Pereira, Bruna Ávila; da Silva, Gabriele Marques Dias; Zambiazi, Priscilla Jussiane; Acta Crystallographica Section E 70 (2014) o1025–; doi:10.1107/S1600536814017280

data_2239902
_publ_section_title
;
 Crystal structure of ethyl
 (<i>E</i>)-4-(4-chlorophenyl)-4-methoxy-2-oxobut-3-enoate
;
_journal_coeditor_code           TK5332
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1025
_journal_paper_doi               10.1107/S1600536814017280
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          'C13 H13 Cl O4'
_chemical_formula_moiety         'C13 H13 Cl O4'
_chemical_formula_sum            'C13 H13 Cl O4'
_chemical_formula_weight         268.68
_chemical_melting_point          358
_chemical_name_systematic
;
Ethyl (<i>E</i>)-4-(4-chlorophenyl)-4-methoxy-2-oxobut-3-enoate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 105.644(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.4557(4)
_cell_length_b                   16.6411(7)
_cell_length_c                   8.4319(3)
_cell_measurement_reflns_used    9103
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.32
_cell_measurement_theta_min      2.24
_cell_volume                     1277.64(9)
_computing_cell_refinement       '<i>SAINT</i> (Bruker, 2009)'
_computing_data_collection       '<i>APEX2</i> (Bruker, 2009)'
_computing_data_reduction        '<i>SAINT</i> (Bruker, 2009)'
_computing_molecular_graphics    '<i>DIAMOND</i> (Brandenburg, 2006)'
_computing_publication_material  '<i>publCIF</i> (Westrip, 2010)'
_computing_structure_refinement  '<i>SHELXL97</i> (Sheldrick, 2008)'
_computing_structure_solution    '<i>SHELXS97</i> (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  'Graphite monochromator'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0227
_diffrn_reflns_av_sigmaI/netI    0.0109
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            30885
_diffrn_reflns_theta_full        28.33
_diffrn_reflns_theta_max         28.33
_diffrn_reflns_theta_min         2.24
_exptl_absorpt_coefficient_mu    0.302
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6667
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
(XPREP; Bruker, 2009)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             560
_exptl_crystal_size_max          0.764
_exptl_crystal_size_mid          0.665
_exptl_crystal_size_min          0.592
_refine_diff_density_max         0.400
_refine_diff_density_min         -0.237
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     167
_refine_ls_number_reflns         3130
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0536
_refine_ls_R_factor_gt           0.0450
_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^)+(0.0697P)^2^+0.4231P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1256
_refine_ls_wR_factor_ref         0.1354
_reflns_number_gt                2613
_reflns_number_total             3130
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            tk5332sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2239902
_cod_database_fobs_code          2239902