Cationic Pd(II)-Catalyzed Highly Enantioselective Arylative Cyclization of Alkyne-Tethered Enals or Enones Initiated by Carbopalladation of Alkynes with Arylboronic Acids.
Shen, Kun; Han, Xiuling; Lu, Xiyan; Organic letters 14 (2012) 1756–1759; doi:10.1021/ol3003546

data_1507570
_publ_section_title
;
 Cationic Pd(II)-Catalyzed Highly Enantioselective Arylative Cyclization
 of Alkyne-Tethered Enals or Enones Initiated by Carbopalladation of
 Alkynes with Arylboronic Acids.
;
_journal_issue                   7
_journal_name_full               'Organic letters'
_journal_page_first              1756
_journal_page_last               1759
_journal_paper_doi               10.1021/ol3003546
_journal_volume                  14
_journal_year                    2012
_chemical_formula_sum            'C25 H25 Br N4 O8'
_chemical_formula_weight         589.40
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
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_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                97.301(3)
_cell_angle_beta                 94.058(3)
_cell_angle_gamma                99.077(3)
_cell_formula_units_Z            2
_cell_length_a                   7.0491(12)
_cell_length_b                   11.375(2)
_cell_length_c                   16.904(3)
_cell_measurement_reflns_used    3190
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.05
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_cell_volume                     1321.9(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \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  0.0221
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_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            8905
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.22
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.610
_exptl_absorpt_correction_T_max  0.9238
_exptl_absorpt_correction_T_min  0.6026
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.481
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             604
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.918
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_refine_ls_extinction_method     none
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_refine_ls_number_reflns         5149
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_refine_ls_R_factor_all          0.0969
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_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1558P)^2^+0.4509P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2062
_refine_ls_wR_factor_ref         0.2419
_reflns_number_gt                3407
_reflns_number_total             5149
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol3003546_si_002.cif
_cod_data_source_block           mo_dm1182_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1321.8(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1507570