AntiCarbocyanative Cyclization of Enynes under Nickel Catalysis
Tomohiro Igarashi; Shigeru Arai; Atsushi Nishida; Journal of Organic Chemistry 78 (2013) 4366–4372; doi:10.1021/jo400342y

data_4028205
_publ_section_title
;
 AntiCarbocyanative Cyclization of Enynes under Nickel Catalysis
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              4366
_journal_page_last               4372
_journal_paper_doi               10.1021/jo400342y
_journal_volume                  78
_journal_year                    2013
_chemical_formula_sum            'C28 H35 N O5 S2 Si2'
_chemical_formula_weight         585.87
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
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_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
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_cell_angle_beta                 92.2980(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   11.6475(11)
_cell_length_b                   18.5320(18)
_cell_length_c                   23.269(2)
_cell_measurement_reflns_used    3511
_cell_measurement_temperature    173
_cell_measurement_theta_max      26.70
_cell_measurement_theta_min      2.27
_cell_volume                     5018.6(8)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_molecular_graphics    'XSHEL (Bruker AXS,2002)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
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_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            27907
_diffrn_reflns_theta_full        27.54
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         1.41
_exptl_absorpt_coefficient_mu    0.352
_exptl_absorpt_correction_T_max  0.9656
_exptl_absorpt_correction_T_min  0.8719
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS Sheldrick 1996
;
_exptl_crystal_colour            colorless
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_exptl_crystal_description       prismatic
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_refine_ls_extinction_method     none
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_refine_ls_matrix_type           full
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_refine_ls_number_reflns         11303
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.928
_refine_ls_R_factor_all          0.1073
_refine_ls_R_factor_gt           0.0513
_refine_ls_shift/su_max          1.463
_refine_ls_shift/su_mean         0.020
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0861P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1357
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_reflns_number_gt                6330
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_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo400342y_Z-2b.cif
_cod_data_source_block           hoshi111205x6-m
_cod_original_cell_volume        5018.7(8)
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_database_code               4028205