Cobalt(II)-Catalyzed Aerobic Oxidation of Terminal-Capped Alkynyl α-Cyano Alkanone Systems. An Oxygen-Mediated Radical Chain Reaction.
Huang, Jing-Kai; Wong, Ying-Chieh; Kao, Tzu-Ting; Tseng, Chen-Tso; Shia, Kak-Shan; The Journal of organic chemistry 81 (2016) 10759–10768; doi:10.1021/acs.joc.6b01837

data_4037250
_publ_section_title
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 Cobalt(II)-Catalyzed Aerobic Oxidation of Terminal-Capped Alkynyl
 \a-Cyano Alkanone Systems. An Oxygen-Mediated Radical Chain Reaction.
;
_journal_issue                   22
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              10759
_journal_page_last               10768
_journal_paper_doi               10.1021/acs.joc.6b01837
_journal_volume                  81
_journal_year                    2016
_chemical_formula_sum            'C16 H23 N O2 Si'
_chemical_formula_weight         289.44
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                109.016(18)
_cell_angle_beta                 90.043(17)
_cell_angle_gamma                101.568(17)
_cell_formula_units_Z            4
_cell_length_a                   11.211(10)
_cell_length_b                   12.349(11)
_cell_length_c                   12.562(11)
_cell_measurement_reflns_used    1799
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.3963
_cell_measurement_theta_min      2.8613
_cell_volume                     1607(2)
_computing_cell_refinement       'SAINT V7.68A (Bruker AXS, 2009)'
_computing_data_collection       'APEX2 (Bruker AXS, 2010)'
_computing_data_reduction        'SAINT V7.68A (Bruker AXS, 2009)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
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_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.856
_diffrn_measured_fraction_theta_max 0.856
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
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_diffrn_radiation_type           MoK\a
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_diffrn_reflns_limit_h_min       -14
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_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -15
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_exptl_absorpt_coefficient_mu    0.148
_exptl_absorpt_correction_T_max  0.7454
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_exptl_absorpt_correction_type   multi-scan
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_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.196
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Columnar
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_refine_ls_number_reflns         6252
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.1585
_refine_ls_R_factor_gt           0.1046
_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^)+(0.1885P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_refine_ls_wR_factor_ref         0.2993
_reflns_number_gt                3772
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_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo6b01837_si_008.cif
_cod_data_source_block           t5
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
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_cod_original_cell_volume        1607(3)
_cod_database_code               4037250