Radical Reactions of 1,4-Alkadiynes: Metal Coordination as an Effective Tool for Controlling the Regio- and Stereoselectivity of the C‒C Bond Formation
Melikyan, Gagik G.; Anker, Bryan; Organometallics 34 (2015) 4194–; doi:10.1021/acs.organomet.5b00480

data_4087669
_publ_section_title
;
 Radical Reactions of 1,4-Alkadiynes: Metal Coordination as an Effective
 Tool for Controlling the Regio- and Stereoselectivity of the C--C Bond
 Formation
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              4194
_journal_paper_doi               10.1021/acs.organomet.5b00480
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C34 H38 Co4 O12 Si4'
_chemical_formula_sum            'C34 H38 Co4 O12 Si4'
_chemical_formula_weight         986.72
_chemical_name_common            BA-24
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                90
_cell_angle_beta                 118.044(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   28.8065(14)
_cell_length_b                   12.4472(6)
_cell_length_c                   28.8024(14)
_cell_measurement_reflns_used    4563
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      30.913
_cell_measurement_theta_min      2.324
_cell_volume                     9114.8(8)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       'APEX2 v2011.2-4 (Bruker, 2011)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type
'Bruker D8 diffractometer with APEX2 detector'
_diffrn_measurement_method       '\f and \w scans with a narrow frame width'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0695
_diffrn_reflns_av_unetI/netI     0.0678
_diffrn_reflns_Laue_measured_fraction_full 1.0000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            86706
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        27.485
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         1.415
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.587
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.5763
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 2:
 wR2(int) was 0.0945 before and 0.0851 after correction.
 The Ratio of minimum to maximum transmission is 0.77.
 The \l/2 correction factor is Not present
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_description       plate
_exptl_crystal_F_000             4015
_exptl_crystal_size_max          0.429
_exptl_crystal_size_mid          0.301
_exptl_crystal_size_min          0.164
_refine_diff_density_max         2.672
_refine_diff_density_min         -0.668
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     993
_refine_ls_number_reflns         20913
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0847
_refine_ls_R_factor_gt           0.0635
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0552P)^2^+26.6814P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1483
_refine_ls_wR_factor_ref         0.1572
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15668
_reflns_number_total             20913
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00480_si_002.cif
_cod_data_source_block           twin4t
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4087669
_shelx_estimated_absorpt_t_min   0.549
_shelx_estimated_absorpt_t_max   0.781
_shelxl_version_number           2012-9
_shelx_res_checksum              86969
_shelx_hkl_checksum              6566