Ethyl 6-(4-chlorophenyl)-2,2-dimethyl-4-oxo-3,4-dihydro-2<i>H</i>-pyran-5-carboxylate
Sharmila, N.; Sundar, T. V.; Sakthivel, P.; Venkatesan, P.; IUCrData 2 (2017) x170034–; doi:10.1107/S2414314617000347

data_1545041
_publ_section_title
;
 Ethyl
 6-(4-chlorophenyl)-2,2-dimethyl-4-oxo-3,4-dihydro-2<i>H</i>-pyran-5-carboxylate
;
_journal_coeditor_code           TK4027
_journal_issue                   1
_journal_name_full               IUCrData
_journal_page_first              x170034
_journal_paper_doi               10.1107/S2414314617000347
_journal_volume                  2
_journal_year                    2017
_chemical_formula_moiety         'C16 H17 Cl O4'
_chemical_formula_sum            'C16 H17 Cl O4'
_chemical_formula_weight         308.74
_chemical_melting_point          356
_chemical_name_common
'Ethyl 2,2-dimethyl-4-oxo-6-phenyl-2,3-dihydro-4H-pyran-5-carboxylate'
_chemical_name_systematic
'Ethyl 2,2-dimethyl-4-oxo-6-phenyl-2,3-dihydro-4H-pyran-5-carboxylate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 102.311(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4412(3)
_cell_length_b                   7.6959(2)
_cell_length_c                   20.2651(5)
_cell_measurement_reflns_used    3995
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.427
_cell_measurement_theta_min      1.996
_cell_volume                     1590.95(7)
_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)
and ORTEPIII
(Burnett
& Johnson, 1996)
;
_computing_publication_material
;
WinGX publication routines (Farrugia, 2012) and PLATON (Spek,
2009)
;
_computing_structure_refinement
;
SHELXL-2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Smart  CCD Area-detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0184
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            15125
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.427
_diffrn_reflns_theta_min         1.996
_exptl_absorpt_coefficient_mu    0.252
_exptl_absorpt_correction_T_max  0.845
_exptl_absorpt_correction_T_min  0.746
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Bruker, 2008)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_description       block
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.280
_refine_diff_density_min         -0.259
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         3995
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0531
_refine_ls_R_factor_gt           0.0369
_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^)+(0.0484P)^2^+0.3683P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0969
_refine_ls_wR_factor_ref         0.1084
_reflns_number_gt                2978
_reflns_number_total             3995
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            tk4027sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        1590.94(7)
_cod_database_code               1545041
_cod_database_fobs_code          1545041
_shelx_estimated_absorpt_t_min   0.940
_shelx_estimated_absorpt_t_max   0.970
_shelx_hkl_checksum              24819
_shelx_res_checksum              76348