Crystal structure of 3,13-dimethoxy-5,6,10,11-tetrahydrofuro[3,4-<i>i</i>][5]helicene-7,9-dione
Sooksimuang, Thanasat; Kamtonwong, Siriporn; Parnchan, Waraporn; Kangkaew, Laongdao; Sahasithiwat, Somboon; Acta Crystallographica Section E 70 (2014) 418–420; doi:10.1107/S1600536814023137

data_2240140
_publ_section_title
;
 Crystal structure of
 3,13-dimethoxy-5,6,10,11-tetrahydrofuro[3,4-<i>i</i>][5]helicene-7,9-dione
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              418
_journal_page_last               420
_journal_paper_doi               10.1107/S1600536814023137
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          'C26 H20 O5'
_chemical_formula_moiety         'C26 H20 O5'
_chemical_formula_sum            'C26 H20 O5'
_chemical_formula_weight         412.42
_chemical_name_systematic
;
3,13-dimethoxy-5,6,10,11-tetrahydrofuro[3,4-<i>i</i>][5]helicene-7,9-dione
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                61.695(3)
_cell_angle_beta                 84.535(3)
_cell_angle_gamma                84.460(3)
_cell_formula_units_Z            4
_cell_length_a                   8.7570(9)
_cell_length_b                   15.9008(16)
_cell_length_c                   16.2987(16)
_cell_measurement_reflns_used    5829
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      21.34
_cell_measurement_theta_min      2.34
_cell_volume                     1985.6(4)
_computing_cell_refinement
;
SAINT (Bruker, 2013)
;
_computing_data_collection
;
APEX2 (Bruker, 2008)
;
_computing_data_reduction
;
SAINT (Bruker, 2013)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012) and Mercury
(Macrae <i>et al.</i>,  2006)
;
_computing_publication_material
;
WinGX (Farrugia, 2012) and publCIF
(Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2013 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS2013 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0487
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            33986
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.122
_diffrn_reflns_theta_min         2.468
_exptl_absorpt_coefficient_mu    0.095
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.67
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2012)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_description       block
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.340
_exptl_crystal_size_min          0.160
_refine_diff_density_max         0.546
_refine_diff_density_min         -0.285
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         7072
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0913
_refine_ls_R_factor_gt           0.0489
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0675P)^2^+0.2937P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1162
_refine_ls_wR_factor_ref         0.1395
_reflns_number_gt                4457
_reflns_number_total             7072
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            nr2055sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        1985.6(3)
_cod_database_code               2240140
_cod_database_fobs_code          2240140
_shelx_estimated_absorpt_t_min   0.961
_shelx_estimated_absorpt_t_max   0.985
_shelx_hkl_checksum              71783
_shelx_res_checksum              78350
_shelxl_version_number           .2013