Dimethyl 1-(4-methylphenyl)-8-(thiophen-2-yl)-11-oxatricyclo[6.2.1.0^2,7^]undeca-2,4,6,9-tetraene-9,10-dicarboxylate
Balakrishnan, B.; Nandakumar, Meganathan; Seshadri, Pandamangalam R.; Mohanakrishnan, Arasambattu K.; Acta Crystallographica Section E 69 (2013) o498–o499; doi:10.1107/S1600536813005308

data_2237646
_publ_section_title
;
 Dimethyl
 1-(4-methylphenyl)-8-(thiophen-2-yl)-11-oxatricyclo[6.2.1.0^2,7^]undeca-2,4,6,9-tetraene-9,10-dicarboxylate
;
_journal_coeditor_code           IM2420
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o498
_journal_page_last               o499
_journal_paper_doi               10.1107/S1600536813005308
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          'C25 H20 O5 S'
_chemical_formula_moiety         'C25 H20 O5 S'
_chemical_formula_sum            'C25 H20 O5 S'
_chemical_formula_weight         432.47
_chemical_name_systematic
'Dimethyl 1-(4-methylphenyl)-8-(thiophen-2-yl)-11-oxatricyclo[6.2.1.0^2,7^]undeca-2,4,6,9-tetraene-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                91.339(5)
_cell_angle_beta                 93.456(4)
_cell_angle_gamma                100.129(5)
_cell_formula_units_Z            2
_cell_length_a                   7.5966(15)
_cell_length_b                   10.877(2)
_cell_length_c                   13.515(3)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.46
_cell_measurement_theta_min      1.51
_cell_volume                     1096.7(4)
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_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 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker Kappa APEXII CCD'
_diffrn_measurement_method       '\w and \f 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  0.0240
_diffrn_reflns_av_sigmaI/netI    0.0240
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            19981
_diffrn_reflns_theta_full        28.46
_diffrn_reflns_theta_max         28.46
_diffrn_reflns_theta_min         1.51
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.181
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             452
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.251
_refine_diff_density_min         -0.160
_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     321
_refine_ls_number_reflns         5464
_refine_ls_number_restraints     52
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0413
_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^)+(0.0648P)^2^+0.1968P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1161
_refine_ls_wR_factor_ref         0.1290
_reflns_number_gt                4142
_reflns_number_total             5464
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            im2420.cif
_cod_data_source_block           I
_cod_original_cell_volume        1096.6(4)
_cod_database_code               2237646
_cod_database_fobs_code          2237646