Diethyl 1,8-bis(4-methylphenyl)-11-oxatricyclo[6.2.1.0^2,7^]undeca-2,4,6-triene-9,10-dicarboxylate
Balakrishnan, B.; Nandakumar, Meganathan; Seshadri, Pandamangalam R.; Mohanakrishnan, Arasambattu K.; Acta Crystallographica Section E 69 (2013) o500–; doi:10.1107/S1600536813005291

data_2237645
_publ_section_title
;
 Diethyl
 1,8-bis(4-methylphenyl)-11-oxatricyclo[6.2.1.0^2,7^]undeca-2,4,6-triene-9,10-dicarboxylate
;
_journal_coeditor_code           IM2419
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o500
_journal_paper_doi               10.1107/S1600536813005291
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          'C30 H30 O5'
_chemical_formula_moiety         'C30 H30 O5'
_chemical_formula_sum            'C30 H30 O5'
_chemical_formula_weight         470.54
_chemical_name_common            'Diels-Alder Adduct'
_chemical_name_systematic
'Diethyl 1,8-bis(4-methylphenyl)-11-oxatricyclo[6.2.1.0^2,7^]undeca-2,4,6-triene-9,10-dicarboxylate'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                109.3190(10)
_cell_angle_beta                 105.0450(10)
_cell_angle_gamma                90.3740(10)
_cell_formula_units_Z            2
_cell_length_a                   9.8722(3)
_cell_length_b                   10.7413(3)
_cell_length_c                   13.3081(3)
_cell_measurement_reflns_used    7905
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.0
_cell_volume                     1279.46(6)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_computing_molecular_graphics
'ORTEP-3 for Windows (Farrugia, 2012) and PLATON (Spek, 2009)'
_computing_publication_material
'SHELXL97 (Sheldrick, 2008), PLATON (Spek, 2009) and publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Kappa APEXII CCD'
_diffrn_measurement_method       '\w and \f scan'
_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  0.0266
_diffrn_reflns_av_sigmaI/netI    0.0196
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            21475
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.02
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.082
_exptl_absorpt_correction_T_max  0.953
_exptl_absorpt_correction_T_min  0.951
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.221
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             500
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.230
_refine_diff_density_min         -0.175
_refine_ls_extinction_coef       0.028(3)
_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   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         4505
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0383
_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^)+(0.0574P)^2^+0.3047P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1021
_refine_ls_wR_factor_ref         0.1119
_reflns_number_gt                3754
_reflns_number_total             4505
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            im2419.cif
_cod_data_source_block           I
_cod_original_cell_volume        1279.45(6)
_cod_database_code               2237645
_cod_database_fobs_code          2237645