Ethyl 2,2-dimethyl-4-oxo-6-phenyl-3,4-dihydro-2<i>H</i>-pyran-5-carboxylate
Sharmila, N.; Sundar, T. V.; Sakthivel, P.; Venkatesan, P.; IUCrData 1 (2016) x161924–; doi:10.1107/S2414314616019246

data_1544765
_publ_section_title
;
 Ethyl
 2,2-dimethyl-4-oxo-6-phenyl-3,4-dihydro-2<i>H</i>-pyran-5-carboxylate
;
_journal_coeditor_code           BV4006
_journal_issue                   12
_journal_name_full               IUCrData
_journal_page_first              x161924
_journal_paper_doi               10.1107/S2414314616019246
_journal_volume                  1
_journal_year                    2016
_chemical_formula_iupac          'C16 H18 O4'
_chemical_formula_moiety         'C16 H18 O4'
_chemical_formula_sum            'C16 H18 O4'
_chemical_formula_weight         274.30
_chemical_melting_point          353
_chemical_name_systematic
;
Ethyl 2,2-dimethyl-4-oxo-6-phenyl-3,4-dihydro-2<i>H</i>-pyran-5-carboxylate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 97.4600(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.4566(2)
_cell_length_b                   5.98210(10)
_cell_length_c                   12.2040(3)
_cell_measurement_reflns_used    4503
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.14
_cell_measurement_theta_min      2.75
_cell_volume                     756.93(3)
_computing_cell_refinement
;
SAINT (Bruker, 2008)
;
_computing_data_collection
;
SMART (Bruker, 2008)
;
_computing_data_reduction
;
SAINT (Bruker, 2008)
;
_computing_molecular_graphics
;
<i>QMOL</i> (Gans & Shalloway, 2001), Mercury (Macrae <i>et al.</i>,
2008), ORTEPIII (Burnett & Johnson, 1996)
and <i>MOPAC</i> (Stewart, 2012)
;
_computing_publication_material
;
WinGX (Farrugia, 2012) and PLATON (Spek, 2009)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type  'Bruker SMART CCD area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  Graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0215
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9344
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.248
_diffrn_reflns_theta_min         1.683
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.204
_exptl_crystal_description       prism
_exptl_crystal_F_000             292
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.166
_refine_diff_density_min         -0.178
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 1007 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.3(4)
_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     181
_refine_ls_number_reflns         4067
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0638
_refine_ls_R_factor_gt           0.0420
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0573P)^2^+0.0653P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1075
_refine_ls_wR_factor_ref         0.1215
_reflns_number_gt                2956
_reflns_number_total             4067
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            bv4006sup1.cif
_cod_data_source_block           I
_cod_database_code               1544765
_cod_database_fobs_code          1544765
_shelx_estimated_absorpt_t_min   0.985
_shelx_estimated_absorpt_t_max   0.991
_shelx_hkl_checksum              34607
_shelx_res_checksum              9471
_shelxl_version_number           2.014