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_4115055
_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_sum            'C33 H24 F4 N4'
_chemical_formula_weight         552.57
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_cell_angle_alpha                90
_cell_angle_beta                 144.662(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.664(2)
_cell_length_b                   8.2817(5)
_cell_length_c                   21.057(1)
_cell_measurement_reflns_used    12965
_cell_measurement_temperature    93.2
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.7
_cell_volume                     2588.6(3)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        'teXsan Ver. 1.10'
_computing_publication_material  'teXsan Ver. 1.10'
_computing_structure_refinement  'teXsan Ver. 1.10'
_computing_structure_solution    MITHRIL90
_diffrn_measured_fraction_theta_full 0.9889
_diffrn_measured_fraction_theta_max 0.9889
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
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_diffrn_reflns_av_R_equivalents  0.029
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
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_diffrn_reflns_theta_max         27.49
_exptl_absorpt_coefficient_mu    0.105
_exptl_absorpt_correction_T_max  0.992
_exptl_absorpt_correction_T_min  0.878
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Higashi, 1995)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_description       prism
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_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.45
_refine_diff_density_min         -0.33
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     246
_refine_ls_number_reflns         2029
_refine_ls_R_factor_gt           0.0414
_refine_ls_shift/su_max          0.0616
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00212|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0765
_reflns_number_gt                2029
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_reflns_threshold_expression     F^2^>3.0\s(F^2^)
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_cod_original_formula_sum        'C33 H24 F4 N4 '
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