Assembling Contiguous Quaternary Carbon Atoms: Regio- and Stereoselective Rearrangements in Cobalt-Directed Radical Reactions of 1,4-Enynes
Melikyan, Gagik G.; Hughes, Rhoda; Rivas, Bianca; Duncan, Kellyanne; Sahakyan, Nare; Organometallics 34 (2015) 242–; doi:10.1021/om501096x

data_4085314
_publ_section_title
;
 Assembling Contiguous Quaternary Carbon Atoms: Regio- and Stereoselective
 Rearrangements in Cobalt-Directed Radical Reactions of 1,4-Enynes
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              242
_journal_paper_doi               10.1021/om501096x
_journal_volume                  34
_journal_year                    2015
_chemical_formula_sum            'C32 H34 Co4 O12 Si2'
_chemical_formula_weight         902.49
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_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                88.433(11)
_cell_angle_beta                 86.353(10)
_cell_angle_gamma                77.394(10)
_cell_formula_units_Z            1
_cell_length_a                   8.0780(9)
_cell_length_b                   8.1647(11)
_cell_length_c                   15.667(2)
_cell_measurement_reflns_used    753
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      53.36
_cell_measurement_theta_min      5.55
_cell_volume                     1006.3(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_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      173(2)
_diffrn_measured_fraction_theta_full 0.886
_diffrn_measured_fraction_theta_max 0.886
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1113
_diffrn_reflns_av_sigmaI/netI    0.1734
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7970
_diffrn_reflns_theta_full        67.39
_diffrn_reflns_theta_max         67.39
_diffrn_reflns_theta_min         5.55
_exptl_absorpt_coefficient_mu    13.723
_exptl_absorpt_correction_T_max  0.4931
_exptl_absorpt_correction_T_min  0.1191
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             458
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.672
_refine_diff_density_min         -0.762
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         3214
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.1379
_refine_ls_R_factor_gt           0.0882
_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^)+(0.1084P)^2^+0.6188P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2236
_refine_ls_wR_factor_ref         0.2563
_reflns_number_gt                1959
_reflns_number_total             3214
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om501096x_si_002.cif
_cod_data_source_block           br_81s
_cod_original_cell_volume        1006.2(2)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4085314