Hexamethyl 13,14-dioxapentacyclo[8.2.1.1^4,7^.0^2,9^.0^3,8^]tetradeca-5,11-diene-1,4,5,6,11,12-hexacarboxylate
Lough, Alan J.; Jack, Kelsey; Tam, William; Acta Crystallographica Section E 68 (2012) o2963–; doi:10.1107/S1600536812039232

data_2236285
_publ_section_title
;
 Hexamethyl
 13,14-dioxapentacyclo[8.2.1.1^4,7^.0^2,9^.0^3,8^]tetradeca-5,11-diene-1,4,5,6,11,12-hexacarboxylate
;
_journal_coeditor_code           HB6954
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2963
_journal_paper_doi               10.1107/S1600536812039232
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C24 H24 O14'
_chemical_formula_moiety         'C24 H24 O14'
_chemical_formula_sum            'C24 H24 O14'
_chemical_formula_weight         536.43
_chemical_name_systematic
;
Hexamethyl
13,14-dioxapentacyclo[8.2.1.1^4,7^.0^2,9^.0^3,8^]tetradeca-
5,11-diene-1,4,5,6,11,12-hexacarboxylate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 95.430(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.1309(18)
_cell_length_b                   10.0840(7)
_cell_length_c                   9.5922(7)
_cell_measurement_reflns_used    6078
_cell_measurement_temperature    147(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.99
_cell_volume                     2419.9(3)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0277
_diffrn_reflns_av_sigmaI/netI    0.0240
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            11038
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         1.63
_exptl_absorpt_coefficient_mu    0.123
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7111
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2007)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.419
_refine_diff_density_min         -0.251
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         2787
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0351
_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^)+(0.0518P)^2^+1.6228P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0924
_refine_ls_wR_factor_ref         0.0976
_reflns_number_gt                2366
_reflns_number_total             2787
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb6954.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2236285
_cod_database_fobs_code          2236285