Rh-Catalyzed Oxidative Coupling between Primary and Secondary Benzamides and Alkynes: Synthesis of Polycyclic Amides
Guoyong Song; Dan Chen; Cheng-Ling Pan; Robert H. Crabtree; Xingwei Li; Journal of Organic Chemistry 75 (2010) 7487–7490; doi:10.1021/jo101596d

data_4025772
_publ_section_title
;
 Rh-Catalyzed Oxidative Coupling between Primary and Secondary Benzamides
 and Alkynes: Synthesis of Polycyclic Amides
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              7487
_journal_page_last               7490
_journal_paper_doi               10.1021/jo101596d
_journal_volume                  75
_journal_year                    2010
_chemical_formula_moiety         'C35 H23 N O'
_chemical_formula_sum            'C35 H23 N O'
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_chemical_melting_point          ?
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_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
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_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_cell_angle_alpha                90.00
_cell_angle_beta                 107.127(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
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_cell_length_c                   12.965(2)
_cell_measurement_temperature    293(2)
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_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT software (Bruker, 1999)'
_computing_molecular_graphics    'SHELXTL-PLUS (Sheldrick, 1990)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       '\w scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
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_exptl_absorpt_coefficient_mu    0.077
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_exptl_absorpt_correction_T_min  0.9773
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            coloursess
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       square
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_refine_ls_extinction_method     none
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_refine_ls_restrained_S_all      0.992
_refine_ls_R_factor_all          0.0764
_refine_ls_R_factor_gt           0.0414
_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^)+(0.0484P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0877
_refine_ls_wR_factor_ref         0.1070
_reflns_number_gt                1885
_reflns_number_total             2828
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo101596d_si_004.cif
_cod_data_source_block           m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        2441.9(8)
_cod_database_code               4025772