2-Ethyl-8-methoxymethyl-4-oxo-4<i>H</i>-chromen-7-yl (1<i>S</i>,4<i>R</i>)-4,7,7-trimethyl-3-oxo-2-oxabicyclo[2.2.1]heptane-1-carboxylate
Qiu, Ya; Chen, Ying; Xia, Peng; Acta Crystallographica Section E 66 (2010) o1459–; doi:10.1107/S1600536810018921

data_2226042
_publ_section_title
;
 2-Ethyl-8-methoxymethyl-4-oxo-4<i>H</i>-chromen-7-yl
 (1<i>S</i>,4<i>R</i>)-4,7,7-trimethyl-3-oxo-2-oxabicyclo[2.2.1]heptane-1-carboxylate
;
_journal_coeditor_code           BH2283
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1459
_journal_paper_doi               10.1107/S1600536810018921
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C23 H26 O7'
_chemical_formula_moiety         'C23 H26 O7'
_chemical_formula_sum            'C23 H26 O7'
_chemical_formula_weight         414.44
_chemical_name_systematic
;
2-Ethyl-8-methoxymethyl-4-oxo-4<i>H</i>-chromen-7-yl
(1<i>S</i>,4<i>R</i>)-4,7,7-trimethyl-3-oxo-2-oxabicyclo[2.2.1]heptane-
1-carboxylate
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_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           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 109.240(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.632(3)
_cell_length_b                   14.159(6)
_cell_length_c                   10.579(4)
_cell_measurement_reflns_used    755
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.228
_cell_measurement_theta_min      2.495
_cell_volume                     1079.3(7)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area-detector'
_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  0.0558
_diffrn_reflns_av_sigmaI/netI    0.0465
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            4560
_diffrn_reflns_theta_full        25.20
_diffrn_reflns_theta_max         25.20
_diffrn_reflns_theta_min         2.04
_exptl_absorpt_coefficient_mu    0.094
_exptl_absorpt_correction_T_max  0.9953
_exptl_absorpt_correction_T_min  0.9796
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             440
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.220
_refine_diff_density_min         -0.224
_refine_ls_extinction_coef       0.013(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   0.964
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     277
_refine_ls_number_reflns         2016
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.964
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0460
_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^)+(0.0832P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1136
_refine_ls_wR_factor_ref         0.1196
_reflns_number_gt                1713
_reflns_number_total             2016
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bh2283.cif
_cod_data_source_block           I
_cod_original_cell_volume        1079.3(8)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2226042
_cod_database_fobs_code          2226042