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_4031092
_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_sum            'C72 H76 N4'
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_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
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_cell_angle_beta                 86.61(4)
_cell_angle_gamma                67.97(5)
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_cell_length_b                   10.853(3)
_cell_length_c                   16.733(4)
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_cell_measurement_temperature    95(2)
_cell_measurement_theta_max      31
_cell_measurement_theta_min      2
_cell_volume                     1403.2(8)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2003)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2003)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      95(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.882
_diffrn_measurement_device_type
'Xcalibur R \k-geometry diffractometer with a Ruby CCD camera'
_diffrn_measurement_method       '\w '
_diffrn_radiation_monochromator  graphite
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_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            10999
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         30.27
_diffrn_reflns_theta_min         2.83
_exptl_absorpt_coefficient_mu    0.068
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            YELLOW
_exptl_crystal_density_diffrn    1.180
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       NEEDLE
_exptl_crystal_F_000             536
_exptl_crystal_size_max          0.30
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_refine_diff_density_max         0.34
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_refine_ls_extinction_method     none
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_refine_ls_number_parameters     356
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_refine_ls_R_factor_all          0.0931
_refine_ls_R_factor_gt           0.0576
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0426P)^2^+0.4017P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1117
_refine_ls_wR_factor_ref         0.1268
_reflns_number_gt                5179
_reflns_number_total             7392
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo5b00745_si_009.cif
_cod_data_source_block           mysl08r
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'TRICLINIC' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

'_exptl_absorpt_correction_type' value 'NONE' changed to 'none'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

'_refine_ls_hydrogen_treatment' value 'CONSTR' changed to 'constr'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 4031087--4031094.cif.
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4031092