One-pot synthesis of cyclophane-type macrocycles using manganese(III)-mediated oxidative radical cyclization.
Ito, Yosuke; Tomiyasu, Yuichi; Kawanabe, Takahiro; Uemura, Keisuke; Ushimizu, Yuu; Nishino, Hiroshi; Organic & biomolecular chemistry 9 (2011) 1491–1507; doi:10.1039/c0ob00683a

data_7153081
_publ_section_title
;
 One-pot synthesis of cyclophane-type macrocycles using
 manganese(III)-mediated oxidative radical cyclization.
;
_journal_issue                   5
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              1491
_journal_page_last               1507
_journal_paper_doi               10.1039/c0ob00683a
_journal_volume                  9
_journal_year                    2011
_chemical_formula_moiety         'C54 H56 O8 '
_chemical_formula_sum            'C54 H56 O8'
_chemical_formula_weight         833.03
_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                90.0000
_cell_angle_beta                 118.413(8)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   14.5489(17)
_cell_length_b                   31.423(9)
_cell_length_c                   11.6090(13)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298.1
_cell_measurement_theta_max      17.1
_cell_measurement_theta_min      15.1
_cell_volume                     4668.0(16)
_computing_cell_refinement       WinAFC
_computing_data_collection       WinAFC
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    SIR92
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku AFC7R'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_av_R_equivalents  0.124
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_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6419
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_standards_decay_%        -36.48
_diffrn_standards_interval_count 0
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.078
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_exptl_absorpt_correction_T_min  0.735
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1776.00
_exptl_crystal_size_max          0.90
_exptl_crystal_size_mid          0.80
_exptl_crystal_size_min          0.70
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_refine_diff_density_min         -0.77
_refine_ls_extinction_coef       245(18)
_refine_ls_extinction_method
'Larson (1970) Crystallographic Computing eq. 22'
_refine_ls_goodness_of_fit_ref   4.749
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     309
_refine_ls_number_reflns         2891
_refine_ls_R_factor_gt           0.0878
_refine_ls_shift/su_max          0.0010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w = 1/\s^2^(Fo^2^)'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_ref         0.1042
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_cod_original_cell_volume        4668.0(15)
_cod_original_formula_sum        'C54 H56 O8 '
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