Diethyl 7,8,18,19-tetramethyl-2,13-dioxohexacyclo[10.10.2.0^3,24^.0^5,10^.0^14,23^.0^16,21^]tetracosa-5,7,9,16,18,20-hexaene-23,24-dicarboxylate
Wang, Jungang; Xiang, Jiacheng; Cao, Liping; Acta Crystallographica Section E 66 (2010) o1681–; doi:10.1107/S1600536810022038

data_2226394
_publ_section_title
;
 Diethyl
 7,8,18,19-tetramethyl-2,13-dioxohexacyclo[10.10.2.0^3,24^.0^5,10^.0^14,23^.0^16,21^]tetracosa-5,7,9,16,18,20-hexaene-23,24-dicarboxylate
;
_journal_coeditor_code           CV2719
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1681
_journal_paper_doi               10.1107/S1600536810022038
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C30 H34 N4 O6'
_chemical_formula_moiety         'C30 H34 N4 O6'
_chemical_formula_sum            'C30 H34 N4 O6'
_chemical_formula_weight         546.61
_chemical_name_systematic
;
Diethyl 7,8,18,19-tetramethyl-2,13-
dioxohexacyclo[10.10.2.0^3,24^.0^5,10^.0^14,23^.0^16,21^]tetracosa-
5,7,9,16,18,20-hexaene-23,24-dicarboxylate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 107.1450(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   23.4988(12)
_cell_length_b                   11.6005(6)
_cell_length_c                   21.2685(11)
_cell_measurement_reflns_used    8852
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      22.27
_cell_measurement_theta_min      2.27
_cell_volume                     5540.1(5)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        'SAINT (Bruker, 1999)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART 4K CCD area-detector'
_diffrn_measurement_method       'phi and omega 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  0.0515
_diffrn_reflns_av_sigmaI/netI    0.0569
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            67299
_diffrn_reflns_theta_full        28.32
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    0.092
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2320
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.168
_refine_diff_density_min         -0.181
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.860
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     809
_refine_ls_number_reflns         13767
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      0.883
_refine_ls_R_factor_all          0.1045
_refine_ls_R_factor_gt           0.0468
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0539P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0997
_refine_ls_wR_factor_ref         0.1159
_reflns_number_gt                6896
_reflns_number_total             13767
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            cv2719.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2226394
_cod_database_fobs_code          2226394