Stereoselective Wittig Olefination as a Macrocyclization Tool. Synthesis of Large Carbazolophanes.
Myśliwiec, Damian; Lis, Tadeusz; Gregoliński, Janusz; Stępień, Marcin; The Journal of organic chemistry 80 (2015) 6300–6312; doi:10.1021/acs.joc.5b00745

data_4031087
_publ_section_title
;
 Stereoselective Wittig Olefination as a Macrocyclization Tool. Synthesis
 of Large Carbazolophanes.
;
_journal_issue                   12
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              6300
_journal_page_last               6312
_journal_paper_doi               10.1021/acs.joc.5b00745
_journal_volume                  80
_journal_year                    2015
_chemical_formula_moiety         'C108 H90 Br12 N6'
_chemical_formula_sum            'C108 H90 Br12 N6'
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_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_cell_angle_beta                 74.45(4)
_cell_angle_gamma                88.09(4)
_cell_formula_units_Z            2
_cell_length_a                   14.207(5)
_cell_length_b                   18.011(6)
_cell_length_c                   20.025(7)
_cell_measurement_reflns_used    3471
_cell_measurement_temperature    80(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      2
_cell_volume                     4934(3)
_computing_cell_refinement       'CrysAlis RED; Oxford-Diffraction Poland, 2003'
_computing_data_collection       'CrysAlis CCD; Oxford-Diffraction Poland, 2003'
_computing_data_reduction        'CrysAlis RED; Oxford-Diffraction Poland, 2003'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      80(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Xcalibur with Ruby CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1382
_diffrn_reflns_av_sigmaI/netI    0.2602
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
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_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            45303
_diffrn_reflns_theta_full        25.50
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_exptl_absorpt_coefficient_mu    4.922
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_exptl_absorpt_correction_T_min  0.662
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   '(CrysAlis RED; Oxford Diffraction, 2003)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.636
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2400
_exptl_crystal_size_max          0.13
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_refine_ls_extinction_method     none
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_refine_ls_number_reflns         18763
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_refine_ls_R_factor_all          0.2613
_refine_ls_R_factor_gt           0.1124
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.055P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1938
_refine_ls_wR_factor_ref         0.2360
_reflns_number_gt                7209
_reflns_number_total             18763
_reflns_threshold_expression     >2sigma(I)
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_cod_depositor_comments
'Adding full bibliography for 4031087--4031094.cif.'
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4031087