Tetramethyl 1,4-dimethyl-13,14-dioxapentacyclo[8.2.1.1^4,7^.0^2,9^.0^3,8^]tetradeca-5,11-diene-5,6,11,12-tetracarboxylate
Lough, Alan J.; Jack, Kelsey; Tam, William; Acta Crystallographica Section E 68 (2012) o2961–; doi:10.1107/S1600536812039219

data_2236283
_publ_section_title
;
 Tetramethyl
 1,4-dimethyl-13,14-dioxapentacyclo[8.2.1.1^4,7^.0^2,9^.0^3,8^]tetradeca-5,11-diene-5,6,11,12-tetracarboxylate
;
_journal_coeditor_code           HB6952
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2961
_journal_paper_doi               10.1107/S1600536812039219
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C22 H24 O10'
_chemical_formula_moiety         'C22 H24 O10'
_chemical_formula_sum            'C22 H24 O10'
_chemical_formula_weight         448.41
_chemical_name_systematic
;
Tetramethyl
1,4-dimethyl-13,14-dioxapentacyclo[8.2.1.1^4,7^.0^2,9^.0^3,8^]tetradeca-
5,11-diene-5,6,11,12-tetracarboxylate
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   11.5170(14)
_cell_length_b                   13.9586(15)
_cell_length_c                   26.413(3)
_cell_measurement_reflns_used    5611
_cell_measurement_temperature    147(2)
_cell_measurement_theta_max      27.40
_cell_measurement_theta_min      2.42
_cell_volume                     4246.2(8)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      147(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Kappa APEX DUO CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Bruker Triumph'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0545
_diffrn_reflns_av_sigmaI/netI    0.0635
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            19411
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    0.112
_exptl_absorpt_correction_T_max  0.9933
_exptl_absorpt_correction_T_min  0.9641
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2007)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1888
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.259
_refine_diff_density_min         -0.200
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.895
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         4850
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      0.893
_refine_ls_R_factor_all          0.0799
_refine_ls_R_factor_gt           0.0415
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0451P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0854
_refine_ls_wR_factor_ref         0.0957
_reflns_number_gt                2974
_reflns_number_total             4850
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb6952.cif
_cod_data_source_block           I
_cod_original_cell_volume        4246.1(8)
_cod_database_code               2236283
_cod_database_fobs_code          2236283