The polyfunctionalized enaminone ethyl [(<i>Z</i>)-2-(2,2-dimethyl-4,6-dioxo-1,3-dioxan-5-ylidenemethyl)-1-methyl-3-oxo-but-1-enylamino]acetate
Vencato, Ivo; Cunha, Silvio; Ferrari, Jailton; Napolitano, Hamilton B.; Lariucci, Carlito; Acta Crystallographica Section E 60 (2004) o2479–o2481; doi:10.1107/S1600536804030211

data_2204730
_publ_section_title
;The polyfunctionalized enaminone ethyl
 [(<i>Z</i>)-2-(2,2-dimethyl-4,6-dioxo-1,3-dioxan-5-ylidenemethyl)-1-methyl-3-oxo-but-1-enylamino]acetate
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2479
_journal_page_last               o2481
_journal_paper_doi               10.1107/S1600536804030211
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          'C16 H21 N O7'
_chemical_formula_moiety         'C16 H21 N O7'
_chemical_formula_sum            'C16 H21 N O7'
_chemical_formula_weight         339.34
_chemical_melting_point          413.5(15)
_chemical_name_systematic
;
ethyl [(Z)-2-(2,2-dimethyl-4,6-dioxo-1,3-dioxan-5-ylidenemethyl)-
1-methyl-3-oxo-but-1-enylamino]acetate
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 103.690(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.324(2)
_cell_length_b                   9.4780(10)
_cell_length_c                   11.062(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.7
_cell_measurement_theta_min      13.1
_cell_volume                     1662.9(4)
_computing_cell_refinement       CAD-4/PC
_computing_data_collection       'CAD-4/PC (Enraf--Nonius, 1993)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics
;
 Ortep-3 for Windows (Farrugia, 1997)
;
_computing_publication_material
;
WinGX (Farrugia, 1999)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Enraf--Nonius CAD-4'
_diffrn_measurement_method       \w--2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.044
_diffrn_reflns_av_sigmaI/netI    0.025
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3072
_diffrn_reflns_theta_full        67.2
_diffrn_reflns_theta_max         67.2
_diffrn_reflns_theta_min         2.79
_diffrn_standards_decay_%        <1.0
_diffrn_standards_interval_time  129
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.903
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.27
_refine_diff_density_min         -0.27
_refine_ls_extinction_coef       0.0100(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         2978
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0759
_refine_ls_R_factor_gt           0.0561
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1046P)^2^+0.187P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1475
_refine_ls_wR_factor_ref         0.1625
_reflns_number_gt                2304
_reflns_number_total             2978
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            kp6019.cif
_cod_data_source_block           IIIc
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '412--415' was changed to '413.5(15)'
- the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_chemical_melting_point' value '412--415' was changed to '413.5(15)'
- the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2204730
_cod_database_fobs_code          2204730