1,5,7,8',11-Pentamethoxy-13<i>H</i>-spiro[dibenzo[<i>a</i>,<i>g</i>]fluorene-13,1'(4'<i>H</i>)-naphthalen]-4'-one toluene monosolvate
Takeuchi, Ryo; Nagasawa, Atsushi; Okamoto, Akiko; Yonezawa, Noriyuki; Acta Crystallographica Section E 68 (2012) o2919–; doi:10.1107/S160053681203824X

data_2236597
_publ_section_title
;
 1,5,7,8',11-Pentamethoxy-13<i>H</i>-spiro[dibenzo[<i>a</i>,<i>g</i>]fluorene-13,1'(4'<i>H</i>)-naphthalen]-4'-one
 toluene monosolvate
;
_journal_coeditor_code           RZ2797
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2919
_journal_paper_doi               10.1107/S160053681203824X
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C35 H28 O6, C7 H8'
_chemical_formula_moiety         'C35 H28 O6, C7 H8'
_chemical_formula_sum            'C42 H36 O6'
_chemical_formula_weight         636.71
_chemical_name_systematic
;
1,5,7,8',11-Pentamethoxy-13<i>H</i>-spiro[dibenzo[<i>a</i>,<i>g</i>]fluorene-
13,1'(4'<i>H</i>)-naphthalen]-4'-one toluene monosolvate
;
_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                 97.319(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.4106(6)
_cell_length_b                   12.4974(7)
_cell_length_c                   21.4941(11)
_cell_measurement_reflns_used    17422
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      68.27
_cell_measurement_theta_min      3.54
_cell_volume                     3306.6(3)
_computing_cell_refinement       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC, 2004)'
_computing_molecular_graphics    'ORTEPIII (Burnett & Johnson, 1996)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla <i>et al.</i>, 2005)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0865
_diffrn_reflns_av_sigmaI/netI    0.0884
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            48937
_diffrn_reflns_theta_full        68.24
_diffrn_reflns_theta_max         68.24
_diffrn_reflns_theta_min         3.59
_exptl_absorpt_coefficient_mu    0.680
_exptl_absorpt_correction_T_max  0.8759
_exptl_absorpt_correction_T_min  0.7725
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(NUMABS; Higashi, 1999)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.279
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.196
_refine_diff_density_min         -0.176
_refine_ls_extinction_coef       0.00363(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   0.962
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     440
_refine_ls_number_reflns         6036
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.962
_refine_ls_R_factor_all          0.0731
_refine_ls_R_factor_gt           0.0426
_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^)+(0.0516P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1080
_refine_ls_wR_factor_ref         0.1243
_reflns_number_gt                3696
_reflns_number_total             6036
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            rz2797.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2236597
_cod_database_fobs_code          2236597