Ethyl 1,3,10,12-tetraphenyl-19,20-dioxahexacyclo[10.6.1.1^3,10^.0^2,11^.0^4,9^.0^13,18^]icosa-4(9),5,7,13(18),14,16-hexaene-2-carboxylate
Narayanan, P.; Sethusankar, K.; Nandhakumar, Meganathan; Mohanakrishnan, Arasambattu K.; Acta Crystallographica Section E 66 (2010) o3155–; doi:10.1107/S1600536810045873

data_2228530
_publ_section_title
;
 Ethyl
 1,3,10,12-tetraphenyl-19,20-dioxahexacyclo[10.6.1.1^3,10^.0^2,11^.0^4,9^.0^13,18^]icosa-4(9),5,7,13(18),14,16-hexaene-2-carboxylate
;
_journal_coeditor_code           RK2244
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3155
_journal_paper_doi               10.1107/S1600536810045873
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C45 H34 O4'
_chemical_formula_moiety         'C45 H34 O4'
_chemical_formula_sum            'C45 H34 O4'
_chemical_formula_weight         638.72
_chemical_melting_point_gt       451
_chemical_melting_point_lt       453
_chemical_name_common            'Diels--Alder Adduct of ethyl propiolate'
_chemical_name_systematic
;
Ethyl 1,3,10,12-tetraphenyl-19,20-
dioxahexacyclo[10.6.1.1^3,10^.0^2,11^.0^4,9^.0^13,18^]icosa-
4(9),5,7,13(18),14,16-hexaene-2-carboxylate
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.2498(4)
_cell_length_b                   12.5137(3)
_cell_length_c                   15.4118(5)
_cell_measurement_reflns_used    5474
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      26.89
_cell_measurement_theta_min      0.999
_cell_volume                     3326.77(15)
_computing_cell_refinement       '<i>SAINT</i> (Bruker, 2004)'
_computing_data_collection       '<i>APEX2</i> (Bruker, 2004)'
_computing_data_reduction        '<i>SAINT</i> (Bruker, 2004)'
_computing_molecular_graphics    '<i>ORTEP-3</i> (Farrugia, 1997)'
_computing_publication_material
'<i>SHELXL97</i> (Sheldrick, 2008) and <i>PLATON</i> (Spek, 2009)'
_computing_structure_refinement  '<i>SHELXL97</i> (Sheldrick, 2008)'
_computing_structure_solution    '<i>SHELXS97</i> (Sheldrick, 2008)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Kappa APEXII CCD'
_diffrn_measurement_method       \w
_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  0.0413
_diffrn_reflns_av_sigmaI/netI    0.0385
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            19378
_diffrn_reflns_theta_full        26.89
_diffrn_reflns_theta_max         26.89
_diffrn_reflns_theta_min         2.41
_exptl_absorpt_coefficient_mu    0.080
_exptl_absorpt_correction_T_max  0.989
_exptl_absorpt_correction_T_min  0.962
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>SADABS</i>; Sheldrick, 1996)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.161
_refine_diff_density_min         -0.165
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         5474
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0544
_refine_ls_R_factor_gt           0.0375
_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^)+(0.0491P)^2^+0.1034P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0829
_refine_ls_wR_factor_ref         0.0921
_reflns_number_gt                4366
_reflns_number_total             5474
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            rk2244.cif
_cod_data_source_block           I
_cod_database_code               2228530
_cod_database_fobs_code          2228530