An Alternative Synthetic Route of [35](1,2,3,4,5)Cyclophane, and Structural Properties of Multibridged [3n]Cyclophanes and Their Charge-Transfer Complexes in the Solid State1
Mikio Yasutake; Toru Koga; Youichi Sakamoto; Shingo Komatsu; Ming Zhou; Katsuya Sako; Hitoshi Tatemitsu; Satoru Onaka; Yoshio Aso; Shinobu Inoue; Teruo Shinmyozu; Journal of the American Chemical Society 124 (2002) 10136–10145; doi:10.1021/ja012363k

data_4115064
_publ_section_title
;
 An Alternative Synthetic Route of [35](1,2,3,4,5)Cyclophane, and
 Structural Properties of Multibridged [3n]Cyclophanes and Their
 Charge-Transfer Complexes in the Solid State1
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10136
_journal_page_last               10145
_journal_paper_doi               10.1021/ja012363k
_journal_volume                  124
_journal_year                    2002
_chemical_formula_moiety         'C27 H28 O '
_chemical_formula_sum            'C27 H28 O'
_chemical_formula_weight         368.52
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90
_cell_angle_beta                 102.874(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.4439(5)
_cell_length_b                   14.3564(6)
_cell_length_c                   19.5718(9)
_cell_measurement_reflns_used    34001
_cell_measurement_temperature    93.2
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      1.7
_cell_volume                     3682.5(3)
_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  SHELXL97
_computing_structure_solution    SIR92
_diffrn_detector_area_resol_mean 10.00
_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  0.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            30303
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    0.078
_exptl_absorpt_correction_T_max  0.984
_exptl_absorpt_correction_T_min  0.666
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Higashi, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_description       prism
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.46
_refine_diff_density_min         -0.29
_refine_ls_extinction_coef       0.0084
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.969
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     515
_refine_ls_number_reflns         5832
_refine_ls_R_factor_gt           0.0488
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^) + (0.0895P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1433
_reflns_number_gt                5832
_reflns_number_total             8388
_reflns_threshold_expression     >2.0sigma(I)
_cod_data_source_file            ja012363k_14.cif
_cod_data_source_block           34CPeno-18
_cod_original_formula_sum        'C27 H28 O '
_cod_database_code               4115064