Bicyclo[2.2.2]octene-Based "Crab-like" Molecules: Synthesis, Complexation, Luminescence Properties, and Solid-State Structures
Teh-Chang Chou; Ching-Lun Hwa; Jin-Ju Lin; Kung-Ching Liao; Jui-Chang Tseng; Journal of Organic Chemistry 70 (2005) 9717–9726; doi:10.1021/jo051006f

data_4020669
_publ_section_title
;
 Bicyclo[2.2.2]octene-Based "Crab-like" Molecules:
 Synthesis, Complexation, Luminescence Properties,
 and Solid-State Structures
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              9717
_journal_page_last               9726
_journal_paper_doi               10.1021/jo051006f
_journal_volume                  70
_journal_year                    2005
_chemical_formula_sum            'C132 H126 O12'
_chemical_formula_weight         1904.33
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                114.94(3)
_cell_angle_beta                 90.12(3)
_cell_angle_gamma                106.06(3)
_cell_formula_units_Z            2
_cell_length_a                   12.119(2)
_cell_length_b                   21.628(4)
_cell_length_c                   21.812(4)
_cell_measurement_reflns_used    64
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      23
_cell_measurement_theta_min      -23
_cell_volume                     4935.7(17)
_computing_cell_refinement       'BRUKER SMART'
_computing_data_collection       'BRUKER SMART'
_computing_data_reduction        'BRUKER SAINT'
_computing_molecular_graphics    Ortep-3
_computing_publication_material  'Wingx publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.954
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device_type  'Bruker Smart Apex'
_diffrn_measurement_method       'phi-omega scan'
_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  0.0249
_diffrn_reflns_av_sigmaI/netI    0.0380
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            59277
_diffrn_reflns_theta_full        28.34
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_min         1.04
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_T_max  0.9731
_exptl_absorpt_correction_T_min  0.9586
_exptl_absorpt_correction_type   Empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.281
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chuncky
_exptl_crystal_F_000             2028
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.34
_refine_diff_density_max         2.499
_refine_diff_density_min         -1.245
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.518
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1303
_refine_ls_number_reflns         23497
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      2.518
_refine_ls_R_factor_all          0.2508
_refine_ls_R_factor_gt           0.1973
_refine_ls_shift/su_max          0.871
_refine_ls_shift/su_mean         0.068
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.5862
_refine_ls_wR_factor_ref         0.6238
_reflns_number_gt                14211
_reflns_number_total             23497
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo051006fsi20050810_110723.cif
_cod_data_source_block           compound21
_cod_database_code               4020669