Mechanism of Cobalt-Catalyzed Heterodimerization of Acrylates and 1,3-Dienes. A Potential Role of Cationic Cobalt(I) Intermediates
Gray, Montgomery; Hines, Michael T.; Parsutkar, Mahesh M.; Wahlstrom, A. J.; Brunelli, Nicholas A.; RajanBabu, T. V.; ACS Catalysis 10 (2020) 4337–4348; doi:10.1021/acscatal.9b05455

data_4517513
_publ_section_title
;
 Mechanism of Cobalt-Catalyzed Heterodimerization of Acrylates and
 1,3-Dienes. A Potential Role of Cationic Cobalt(I) Intermediates
;
_journal_issue                   7
_journal_name_full               'ACS Catalysis'
_journal_page_first              4337
_journal_page_last               4348
_journal_paper_doi               10.1021/acscatal.9b05455
_journal_volume                  10
_journal_year                    2020
_chemical_formula_moiety         'C54 H52 Co P4, C32 H12 B F24'
_chemical_formula_sum            'C86 H64 B Co F24 P4'
_chemical_formula_weight         1746.99
_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     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-08-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
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_cell_angle_gamma                90
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_cell_length_a                   16.6366(7)
_cell_length_b                   12.7954(6)
_cell_length_c                   37.4749(17)
_cell_measurement_reflns_used    9872
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      26.342
_cell_measurement_theta_min      2.420
_cell_volume                     7826.2(6)
_computing_cell_refinement       'SAINT v8.38A (Bruker, 2017)'
_computing_data_collection       'APEX3 v2017.3-0 (Bruker, 2017)'
_computing_data_reduction        'SAINT v8.38A (Bruker, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker APEX-II CCD'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Nonius Kappa APEX II'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0438
_diffrn_reflns_av_unetI/netI     0.0180
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            231454
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.379
_diffrn_reflns_theta_min         1.248
_diffrn_source                   'sealed tube'
_diffrn_source_type              fine-focus
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.405
_exptl_absorpt_correction_T_max  0.2602
_exptl_absorpt_correction_T_min  0.2187
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0566 before and 0.0496 after correction. The Ratio of minimum to maximum transmission is 0.8405. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'Dark Bluish Green'
_exptl_crystal_colour_lustre     Dark
_exptl_crystal_colour_modifier   bluish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_description       Block
_exptl_crystal_F_000             3552
_exptl_crystal_size_max          0.357
_exptl_crystal_size_mid          0.313
_exptl_crystal_size_min          0.268
_refine_diff_density_max         0.503
_refine_diff_density_min         -0.332
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1144
_refine_ls_number_reflns         15955
_refine_ls_number_restraints     144
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0348
_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^)+(0.0485P)^2^+4.8587P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0881
_refine_ls_wR_factor_ref         0.0921
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13748
_reflns_number_total             15955
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs9b05455_si_003.cif
_cod_data_source_block           RBabu_MP-05-007
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

data item '_exptl_crystal_colour_modifier' value 'Bluish' was changed
to 'bluish' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

data item '_exptl_crystal_colour_primary' value 'Green' was changed
to 'green' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 4517513--4517514.cif.

 Adding full bibliography for 4517513--4517514.cif.
;
_cod_database_code               4517513
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.899
_shelx_estimated_absorpt_t_min   0.869
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(F23B) = Uanis(F24)
Uanis(F13B) = Uanis(F13)
3. Rigid body (RIGU) restrains
 F13, F13B, F14, F14B, F15, F15B, C77
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 F10, F10B, F11, F11B, F12, F12B, C70
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 F22, F22B, F23, F23B, F24, F24B, C86
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 F16, F16B, F17, F18, F18B, C78
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 F16, F16B, F17, F17B, F18, F18B, C78
 with sigma for 1-2 distances of 0.0005 and sigma for 1-3 distances of 0.0005
4. Others
 Sof(F13B)=Sof(F14B)=Sof(F15B)=1-FVAR(1)
 Sof(F13)=Sof(F14)=Sof(F15)=FVAR(1)
 Sof(F10B)=Sof(F11B)=Sof(F12B)=1-FVAR(2)
 Sof(F10)=Sof(F11)=Sof(F12)=FVAR(2)
 Sof(F22B)=Sof(F23B)=Sof(F24B)=1-FVAR(3)
 Sof(F22)=Sof(F23)=Sof(F24)=FVAR(3)
 Fixed Sof: F16(0.5) F16B(0.5) F17(0.5) F17B(0.5) F18(0.5) F18B(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B)
5.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C14(H14), C15(H15), C16(H16),
 C17(H17), C18(H18), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C26(H26),
  C27(H27), C28(H28), C29(H29), C30(H30), C32(H32), C33(H33), C34(H34),
 C35(H35), C36(H36), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42), C44(H44),
  C45(H45), C46(H46), C47(H47), C48(H48), C50(H50), C51(H51), C52(H52),
 C53(H53), C54(H54), C56(H56), C58(H58), C60(H60), C64(H64), C66(H66), C68(H68),
  C72(H72), C74(H74), C76(H76), C80(H80), C82(H82), C84(H84)
;
_shelx_res_checksum              42309
_shelx_hkl_checksum              77053
_olex2_submission_special_instructions 'No special instructions were received'