Palladium/Copper-catalyzed aerobic intermolecular cyclization of enediyne compounds and alkynes: interrupting cycloaromatization for (4 + 2) cross-benzannulation.
Ling, Fei; Li, Zexiang; Zheng, Chenguang; Liu, Xiang; Ma, Cheng; Journal of the American Chemical Society 136 (2014) 10914–10917; doi:10.1021/ja506795u

data_4122337
_publ_section_title
;
 Palladium/Copper-catalyzed aerobic intermolecular cyclization of enediyne
 compounds and alkynes: interrupting cycloaromatization for (4 + 2)
 cross-benzannulation.
;
_journal_issue                   31
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10914
_journal_page_last               10917
_journal_paper_doi               10.1021/ja506795u
_journal_volume                  136
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C41 H30 N2 O8 S'
_chemical_formula_sum            'C41 H30 N2 O8 S'
_chemical_formula_weight         710.73
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.1363(5)
_cell_length_b                   21.1151(17)
_cell_length_c                   23.2821(18)
_cell_measurement_reflns_used    4967
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.5598
_cell_measurement_theta_min      2.8486
_cell_volume                     3508.2(5)
_computing_cell_refinement       'CrysAlis PRO (Agilent Technologies, 2011)'
_computing_data_collection       'CrysAlis PRO'
_computing_data_reduction        'CrysAlis PRO'
_computing_molecular_graphics    'OLEX2 (Dolomanov et al., 2009)'
_computing_publication_material  OLEX2
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.3592
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_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  0.0996
_diffrn_reflns_av_sigmaI/netI    0.0697
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            22840
_diffrn_reflns_theta_full        25.34
_diffrn_reflns_theta_max         25.34
_diffrn_reflns_theta_min         2.99
_exptl_absorpt_coefficient_mu    0.151
_exptl_absorpt_correction_T_max  0.9705
_exptl_absorpt_correction_T_min  0.9394
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis PRO (Agilent Technologies, 2011) 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1480
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.330
_refine_diff_density_min         -0.293
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details 'Flack (1983), 2772 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.07(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     482
_refine_ls_number_reflns         6425
_refine_ls_number_restraints     90
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0863
_refine_ls_R_factor_gt           0.0648
_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^)+(0.0787P)^2^+0.1454P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1501
_refine_ls_wR_factor_ref         0.1714
_reflns_number_gt                4889
_reflns_number_total             6425
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja506795u_si_002.cif
_cod_data_source_block           130905_lzx0905_(4ak)
_cod_depositor_comments
'Adding full bibliography for 4122337--4122339.cif.'
_cod_database_code               4122337