Ethyl (2<i>Z</i>)-3-oxo-2-(3,4,5-trimethoxybenzylidene)butanoate
Zukerman-Schpector, Julio; Hino, Camila Lury; Moran, Paulo J. S.; de Paula, Bruno R. S.; Ng, Seik Weng; Tiekink, Edward R. T.; Acta Crystallographica Section E 69 (2013) o1474–; doi:10.1107/S1600536813023374

data_2238518
_publ_section_title
;
 Ethyl (2<i>Z</i>)-3-oxo-2-(3,4,5-trimethoxybenzylidene)butanoate
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1474
_journal_paper_doi               10.1107/S1600536813023374
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          'C16 H20 O6'
_chemical_formula_moiety         'C16 H20 O6'
_chemical_formula_sum            'C16 H20 O6'
_chemical_formula_weight         308.32
_chemical_melting_point_gt       381.2
_chemical_melting_point_lt       381.7
_chemical_name_systematic
;
Ethyl (2<i>Z</i>)-3-oxo-2-(3,4,5-trimethoxybenzylidene)butanoate
;
_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                61.130(5)
_cell_angle_beta                 77.450(4)
_cell_angle_gamma                82.534(4)
_cell_formula_units_Z            2
_cell_length_a                   8.3432(4)
_cell_length_b                   10.2446(5)
_cell_length_c                   10.4543(5)
_cell_measurement_reflns_used    3721
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.818
_cell_measurement_theta_min      5.064
_cell_volume                     763.48(7)
_computing_cell_refinement       'CrysAlis PRO (Agilent, 2013)'
_computing_data_collection       'CrysAlis PRO (Agilent, 2013)'
_computing_data_reduction        'CrysAlis PRO (Agilent, 2013)'
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012), DIAMOND (Brandenburg,
2006) and
MarvinSketch (ChemAxon, 2010)
;
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>, 1999)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4041
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Agilent SuperNova (Dual, Cu at zero, Atlas)'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0123
_diffrn_reflns_av_sigmaI/netI    0.0162
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5294
_diffrn_reflns_theta_full        76.01
_diffrn_reflns_theta_max         76.01
_diffrn_reflns_theta_min         5.07
_exptl_absorpt_coefficient_mu    0.858
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.63085
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrysAlis PRO; Agilent, 2013)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             328
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.318
_refine_diff_density_min         -0.252
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     204
_refine_ls_number_reflns         3101
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0340
_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^)+(0.0524P)^2^+0.2494P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0935
_refine_ls_wR_factor_ref         0.0948
_reflns_number_gt                2943
_reflns_number_total             3101
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            kj2231.cif
_cod_data_source_block           I
_cod_database_code               2238518
_cod_database_fobs_code          2238518