Unusual [2+4] and [2+2] Cycloadditions of Arenes in the Confined Cavity of Self-Assembled Cages
Yuki Nishioka; Takumi Yamaguchi; Michito Yoshizawa; Makoto Fujita; Journal of the American Chemical Society 129 (2007) 7000–7001; doi:10.1021/ja071591x

data_4109486
_publ_contact_author             'Makoto Fujita'
_publ_contact_author_email       mfujita@appchem.t.u-tokyo.ac.jp
_publ_section_title
;
 Unusual [2+4] and [2+2] Cycloadditions of Arenes in the Confined Cavity
 of Self-Assembled Cages
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7000
_journal_page_last               7001
_journal_paper_doi               10.1021/ja071591x
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C134 H167 N43 O111.5 Pd6'
_chemical_formula_weight         4802.51
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.2759(19)
_cell_length_b                   26.2759(19)
_cell_length_c                   31.734(5)
_cell_measurement_reflns_used    13917
_cell_measurement_temperature    80(2)
_cell_measurement_theta_max      28.97
_cell_measurement_theta_min      1.69
_cell_volume                     21910(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      80(2)
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0568
_diffrn_reflns_av_sigmaI/netI    0.0414
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            127788
_diffrn_reflns_theta_full        28.97
_diffrn_reflns_theta_max         28.97
_diffrn_reflns_theta_min         1.69
_exptl_absorpt_coefficient_mu    0.589
_exptl_absorpt_correction_T_max  0.9982
_exptl_absorpt_correction_T_min  0.9982
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_density_meas      0
_exptl_crystal_description       block
_exptl_crystal_F_000             9760
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.374
_refine_diff_density_min         -0.884
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     683
_refine_ls_number_reflns         13917
_refine_ls_number_restraints     168
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.1076
_refine_ls_R_factor_gt           0.0712
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1177P)^2^+188.1454P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2021
_refine_ls_wR_factor_ref         0.2419
_reflns_number_gt                9332
_reflns_number_total             13917
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja071591xsi20070315_024606.cif
_cod_data_source_block           i41a
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_original_formula_sum        'C134 H167 N43 O111.50 Pd6'
_cod_database_code               4109486