Concise, aromatization-based approach to an elaborate C2-symmetric pyrenophane
Penchal Reddy Nandaluru; Prateek Dongare; Christina M. Kraml; Robert A. Pascal; Louise N. Dawe; David W. Thompson; Graham J. Bodwell; Chem.Commun. 48 (2012) 7747–; doi:10.1039/c2cc33611a

data_7108085
_publ_section_title
;
 Concise, aromatization-based approach to an elaborate C2-symmetric
 pyrenophane
;
_journal_name_full               Chem.Commun.
_journal_page_first              7747
_journal_paper_doi               10.1039/c2cc33611a
_journal_volume                  48
_journal_year                    2012
_chemical_formula_moiety         'C40 H36 O2'
_chemical_formula_sum            'C40 H36 O2'
_chemical_formula_weight         548.69
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                104.045(8)
_cell_angle_beta                 107.143(4)
_cell_angle_gamma                106.279(6)
_cell_formula_units_Z            2
_cell_length_a                   9.395(5)
_cell_length_b                   12.771(6)
_cell_length_c                   13.799(7)
_cell_measurement_reflns_used    4969
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      30.6839
_cell_measurement_theta_min      1.6517
_cell_volume                     1420.0(12)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_data_collection       'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_molecular_graphics    'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL-97 (Acta Cryst.2008, A64, 112-122)'
_computing_structure_solution    'SHELXS-97 (Acta Cryst.2008, A64, 112-122)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 14.63
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'graphite - Rigaku SHINE'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0590
_diffrn_reflns_av_sigmaI/netI    0.0763
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13837
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         2.74
_exptl_absorpt_coefficient_mu    0.077
_exptl_absorpt_correction_T_max  0.9985
_exptl_absorpt_correction_T_min  0.9930
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'T. Higashi, 2000'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.283
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             584
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.211
_refine_diff_density_min         -0.246
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.150
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         5859
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.150
_refine_ls_R_factor_all          0.1271
_refine_ls_R_factor_gt           0.0884
_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^)+(0.0562P)^2^+0.6960P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1702
_refine_ls_wR_factor_ref         0.1924
_reflns_number_gt                4112
_reflns_number_total             5859
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc33611a.txt
_cod_data_source_block           11
_cod_original_cell_volume        1419.9(12)
_cod_database_code               7108085