Naphthalene Diels-Alder in a Self-Assembled Molecular Flask
Takashi Murase; Shinnosuke Horiuchi; Makoto Fujita; Journal of the American Chemical Society 132 (2010) 2866–2867; doi:10.1021/ja9107275

data_4102029
_publ_contact_author             'Makoto Fujita'
_publ_contact_author_email       mfujita@appchem.t.u-tokyo.ac.jp
_publ_section_title
;
 Naphthalene Diels-Alder in a Self-Assembled Molecular Flask
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2866
_journal_page_last               2867
_journal_paper_doi               10.1021/ja9107275
_journal_volume                  132
_journal_year                    2010
_chemical_formula_sum            'C132 H173 N48.9 O92.89 Pd6'
_chemical_formula_weight         4569.32
_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                   26.222(3)
_cell_length_b                   26.222(3)
_cell_length_c                   31.650(6)
_cell_measurement_reflns_used    8826
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      29.442
_cell_measurement_theta_min      3.741
_cell_volume                     21762(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX-II'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker XP'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_monochromator  'focusing mirror'
_diffrn_radiation_source         'fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0588
_diffrn_reflns_av_sigmaI/netI    0.0405
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            137545
_diffrn_reflns_theta_full        30.48
_diffrn_reflns_theta_max         30.48
_diffrn_reflns_theta_min         3.66
_exptl_absorpt_coefficient_mu    0.584
_exptl_absorpt_correction_T_max  0.9439
_exptl_absorpt_correction_T_min  0.9386
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             9305
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.797
_refine_diff_density_min         -0.822
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     666
_refine_ls_number_reflns         15908
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.1109
_refine_ls_R_factor_gt           0.0655
_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^)+(0.0816P)^2^+128.4617P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1725
_refine_ls_wR_factor_ref         0.2122
_reflns_number_gt                10187
_reflns_number_total             15908
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9107275_si_002.cif
_cod_data_source_block           i41a
_cod_original_cell_volume        21763(5)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_original_formula_sum        'C132 H173 N48.90 O92.89 Pd6'
_cod_database_code               4102029