3,10,14,21-Tetrakis(4-methoxyphenyl)pentacyclo[11.8.0.0^2,11^.0^4,9^.0^15,20^]henicosa-1(21),2,4(9),5,7,10,13,15(20),16,18-decaen-12-one chloroform monosolvate
Gopinath, S.; Narayanan, P.; Sethusankar, K.; Nandakumar, Meganathan; Mohanakrishnan, Arasambattu K.; Acta Crystallographica Section E 70 (2014) o873–o874; doi:10.1107/S1600536814016389

data_2239803
_publ_section_title
;
 3,10,14,21-Tetrakis(4-methoxyphenyl)pentacyclo[11.8.0.0^2,11^.0^4,9^.0^15,20^]henicosa-1(21),2,4(9),5,7,10,13,15(20),16,18-decaen-12-one
 chloroform monosolvate
;
_journal_coeditor_code           TK5322
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o873
_journal_page_last               o874
_journal_paper_doi               10.1107/S1600536814016389
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          'C49 H36 O5, C H Cl3'
_chemical_formula_moiety         'C49 H36 O5, C H Cl3'
_chemical_formula_sum            'C50 H37 Cl3 O5'
_chemical_formula_weight         824.15
_chemical_name_systematic
;3,10,14,21-Tetrakis(4-methoxyphenyl)pentacyclo[11.8.0.0^2,11^.0^4,9^.0^15,20^]henicosa-1(21),2,4(9),5,7,10,13,15(20),16,18-decaen-12-one chloroform
monosolvate
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 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                 93.9470(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.7720(4)
_cell_length_b                   12.0351(4)
_cell_length_c                   17.3162(6)
_cell_measurement_reflns_used    3474
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.75
_cell_measurement_theta_min      1.69
_cell_volume                     2031.68(13)
_computing_cell_refinement       'APEX2 (Bruker, 2008)'
_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_molecular_graphics
'ORTEP-3 for Windows (Farrugia, 2012) and Mercury (Macrae, <i>et al.</i>, 2008)'
_computing_publication_material
'SHELXL97 (Sheldrick, 2008) and PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Kappa APEXII CCD'
_diffrn_measurement_method       '\w &\f 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  0.0252
_diffrn_reflns_av_sigmaI/netI    0.0198
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            20614
_diffrn_reflns_theta_full        24.75
_diffrn_reflns_theta_max         24.75
_diffrn_reflns_theta_min         1.69
_exptl_absorpt_coefficient_mu    0.275
_exptl_absorpt_correction_T_max  0.934
_exptl_absorpt_correction_T_min  0.892
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             740
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_platon_squeeze_details
;
The void in the crystal contains a highly disordered molecule of
chloroform which has been removed from the intensity data using the
program SQUEEZE in PLATON(Spek, 2004). The electron count from the
SQUEEZE result confirms the removed solvent is chloroform. There are
two molecules of chloroform in the unit cell. The chloroform is included
in the chemical formula.
;
_refine_diff_density_max         0.130
_refine_diff_density_min         -0.147
_refine_ls_extinction_coef       0.0041(10)
_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   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         3474
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0397
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0692P)^2^+0.1579P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1173
_refine_ls_wR_factor_ref         0.1248
_reflns_number_gt                2664
_reflns_number_total             3474
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            tk5322sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 2/n'
_cod_database_code               2239803
_cod_database_fobs_code          2239803