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_4115052
_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         'C21 H24 '
_chemical_formula_sum            'C21 H24'
_chemical_formula_weight         276.42
_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'
_cell_angle_alpha                90
_cell_angle_beta                 93.041(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.8714(7)
_cell_length_b                   11.905(1)
_cell_length_c                   13.335(1)
_cell_measurement_reflns_used    7494
_cell_measurement_temperature    93.2
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      2.3
_cell_volume                     1564.9(2)
_computing_cell_refinement       PROCESS
_computing_data_collection       PROCESS
_computing_data_reduction        'teXsan Ver. 1.10'
_computing_publication_material  'teXsan Ver. 1.10'
_computing_structure_refinement  'teXsan Ver. 1.10'
_computing_structure_solution    SHELXS97
_diffrn_measured_fraction_theta_full 0.9941
_diffrn_measured_fraction_theta_max 0.9941
_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  0.039
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            3556
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    0.065
_exptl_absorpt_correction_T_max  0.993
_exptl_absorpt_correction_T_min  0.886
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Higashi, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.173
_exptl_crystal_description       prism
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.44
_refine_diff_density_min         -0.26
_refine_ls_extinction_coef       0.012(9)
_refine_ls_extinction_method     'Zachariasen(1967) type 2 gaussian isotropic'
_refine_ls_goodness_of_fit_ref   1.461
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     200
_refine_ls_number_reflns         1426
_refine_ls_R_factor_gt           0.0687
_refine_ls_shift/su_max          0.0003
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00331|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1031
_reflns_number_gt                1426
_reflns_number_total             3556
_reflns_threshold_expression     F^2^>3.0\s(F^2^)
_cod_data_source_file            ja012363k_02.cif
_cod_data_source_block           33CP-6
_cod_original_formula_sum        'C21 H24 '
_cod_database_code               4115052