Ethyl (<i>E</i>)-2-(2,7-dimethyl-5-oxo-4<i>H</i>,5<i>H</i>-pyrano[4,3-<i>b</i>]pyran-4-ylidene)acetate
Bassou, Oulemda; Chicha, Hakima; Bouissane, Latifa; Rakib, El Mostapha; Saadi, Mohamed; El Ammari, Lahcen; IUCrData 2 (2017) x170208–; doi:10.1107/S2414314617002085

data_1545481
_publ_section_title
;
 Ethyl
 (<i>E</i>)-2-(2,7-dimethyl-5-oxo-4<i>H</i>,5<i>H</i>-pyrano[4,3-<i>b</i>]pyran-4-ylidene)acetate
;
_journal_issue                   2
_journal_name_full               IUCrData
_journal_page_first              x170208
_journal_paper_doi               10.1107/S2414314617002085
_journal_volume                  2
_journal_year                    2017
_chemical_formula_iupac          'C14 H14 O5'
_chemical_formula_moiety         'C14 H14 O5'
_chemical_formula_sum            'C14 H14 O5'
_chemical_formula_weight         262.25
_chemical_melting_point          376
_chemical_name_systematic
'Ethyl (<i>E</i>)-2-(2,7-dimethyl-5-oxo-4<i>H</i>,5<i>H</i>-pyrano[4,3-<i>b</i>]pyran-4-ylidene)acetate'
_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                 108.257(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.5679(12)
_cell_length_b                   11.4330(13)
_cell_length_c                   12.7993(15)
_cell_measurement_reflns_used    2939
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.102
_cell_measurement_theta_min      2.446
_cell_volume                     1329.6(3)
_computing_cell_refinement
;
SAINT (Bruker, 2009)
;
_computing_data_collection
;
APEX2 (Bruker, 2009)
;
_computing_data_reduction
;
SAINT (Bruker, 2009)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012) and Mercury (Macrae <i>et al.</i>,
2008)
;
_computing_publication_material
;
PLATON (Spek, 2009) and publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2014 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker X8 APEX'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0367
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            16353
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.102
_diffrn_reflns_theta_min         2.446
_exptl_absorpt_coefficient_mu    0.100
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.6627
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>, 2015)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_description       block
_exptl_crystal_F_000             552
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.210
_refine_diff_density_max         0.169
_refine_diff_density_min         -0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     180
_refine_ls_number_reflns         2939
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0762
_refine_ls_R_factor_gt           0.0432
_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^)+(0.0699P)^2^+0.1184P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1183
_refine_ls_wR_factor_ref         0.1370
_reflns_number_gt                1909
_reflns_number_total             2939
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            su4128sup1.cif
_cod_data_source_block           I
_cod_database_code               1545481
_cod_database_fobs_code          1545481
_shelx_hkl_checksum              37590
_shelx_res_checksum              6045