Radical Reactions of the Cobalt-Complexed Propargyl Acetals: Inter- and Intramolecular Variants
Melikyan, Gagik G.; Voorhees, Erin; Sepanian, Ruth; Organometallics 33 (2014) 69–; doi:10.1021/om400718w

data_4082509
_publ_section_title
;
 Radical Reactions of the Cobalt-Complexed Propargyl Acetals: Inter- and
 Intramolecular Variants
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              69
_journal_paper_doi               10.1021/om400718w
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C28 H30 Co4 O14 Si2'
_chemical_formula_sum            'C28 H30 Co4 O14 Si2'
_chemical_formula_weight         882.42
_chemical_name_systematic
;
 ?
;
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2013-10-21
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2013.10.21 svn.r2790 for OlexSys, GUI svn.r4645)
;
_audit_update_record
;
2013-10-21 # Formatted by publCIF

;
_cell_angle_alpha                90
_cell_angle_beta                 100.008(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.7878(12)
_cell_length_b                   12.6131(6)
_cell_length_c                   17.4643(10)
_cell_measurement_reflns_used    894
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      45.34
_cell_measurement_theta_min      2.52
_cell_volume                     3858.7(4)
_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    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 0.932
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.3130
_diffrn_reflns_av_unetI/netI     0.3073
_diffrn_reflns_Laue_measured_fraction_full 0.932
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            23957
_diffrn_reflns_point_group_measured_fraction_full 0.932
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         65.081
_diffrn_reflns_theta_min         2.522
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    14.340
_exptl_absorpt_correction_T_max  0.7533
_exptl_absorpt_correction_T_min  0.3915
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1494 before and 0.0717 after correction.
The Ratio of minimum to maximum transmission is 0.5197.
The \l/2 correction factor is 0.0000.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_description       plate
_exptl_crystal_F_000             1784
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.094
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.072
_refine_diff_density_min         -0.608
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.902
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         6500
_refine_ls_number_restraints     87
_refine_ls_restrained_S_all      0.898
_refine_ls_R_factor_all          0.2723
_refine_ls_R_factor_gt           0.0965
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0872P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1930
_refine_ls_wR_factor_ref         0.2703
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1968
_reflns_number_total             6500
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om400718w_si_001.cif
_cod_data_source_block           ev124
_cod_database_code               4082509
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.762
_shelx_estimated_absorpt_t_min   0.222
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 Co4, C26, O10
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 Co4, C27, O11
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 Co4, C28, O12
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 Co1, C17, O1
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 Co1, C2, C1, Co2
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C3, C4
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 Co1, C18, O2
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 Co2, C21, O5
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C22, O6, Co2
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C19, O3
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
3.a Ternary CH refined with riding coordinates:
 C3(H3), C4(H4)
3.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C15(H15A,H15B)
3.c Me refined with riding coordinates:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C),
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C16(H16A,H16B,
 H16C)
;
_shelx_res_checksum              68088
_shelx_hkl_checksum              84714