Synthesis, Structure, and Transannular π-π Interaction of Multilayered [3.3]Metacyclophanes
Masahiko Shibahara; Motonori Watanabe; Tetsuo Iwanaga; Keiko Ideta; Teruo Shinmyozu; Journal of Organic Chemistry 72 (2007) 2865–2877; doi:10.1021/jo062220m

data_4022707
_publ_section_title
;
 Synthesis, Structure, and Transannular \p-\p Interaction
 of Multilayered [3.3]Metacyclophanes
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              2865
_journal_page_last               2877
_journal_paper_doi               10.1021/jo062220m
_journal_volume                  72
_journal_year                    2007
_chemical_formula_moiety         'C42 H48 '
_chemical_formula_sum            'C42 H48'
_chemical_formula_weight         552.84
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_audit_creation_date             'Thu Dec 16 13:29:13 2004'
_audit_creation_method           'by teXsan'
_cell_angle_alpha                90
_cell_angle_beta                 18.4827(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.2281
_cell_length_b                   11.3490(1)
_cell_length_c                   29.1340
_cell_measurement_reflns_used    28735
_cell_measurement_temperature    123.2
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      2.2
_cell_volume                     3063.67(5)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_publication_material  'teXsan Ver. 1.11'
_computing_structure_refinement  'teXsan Ver. 1.10'
_computing_structure_solution    SIR97
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.9970
_diffrn_measured_fraction_theta_max 0.9970
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.040
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            27817
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_exptl_absorpt_coefficient_mu    0.067
_exptl_absorpt_correction_T_max  0.993
_exptl_absorpt_correction_T_min  0.783
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Higashi, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.198
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.380
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.33
_refine_diff_density_min         -0.25
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.399
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     379
_refine_ls_number_reflns         6981
_refine_ls_R_factor_gt           0.0424
_refine_ls_shift/su_max          0.0004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^) + (0.05000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1215
_reflns_number_gt                5591
_reflns_number_total             6981
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            jo062220msi20061026_030224.cif
_cod_data_source_block           b
_cod_original_sg_symbol_H-M      'P 21/a'
_cod_original_formula_sum        'C42 H48 '
_cod_database_code               4022707