Activator-free single-component Co(i)-catalysts for regio- and enantioselective heterodimerization and hydroacylation reactions of 1,3-dienes. New reduction procedures for synthesis of [L]Co(i)-complexes and comparison to in situ generated catalysts
Parsutkar, Mahesh M.; Moore, Curtis E.; RajanBabu, T. V.; Dalton Transactions  (2022) –; doi:10.1039/D2DT01484J

data_7710555
_publ_section_title
;
 Activator-free single-component Co(i)-catalysts for regio- and
 enantioselective heterodimerization and hydroacylation reactions of
 1,3-dienes. New reduction procedures for synthesis of [L]Co(i)-complexes
 and comparison to in situ generated catalysts
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01484J
_journal_year                    2022
_chemical_formula_moiety         'C78 H72 Cl2 Co2 P6, 2(C4 H8 O)'
_chemical_formula_sum            'C86 H88 Cl2 Co2 O2 P6'
_chemical_formula_weight         1528.27
_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_Int_Tables_number      14
_audit_creation_date             2019-10-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-11-18 deposited with the CCDC.	2022-06-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.074(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.7933(14)
_cell_length_b                   13.2529(11)
_cell_length_c                   19.5680(19)
_cell_measurement_reflns_used    9229
_cell_measurement_temperature    100
_cell_measurement_theta_max      23.037
_cell_measurement_theta_min      2.293
_cell_volume                     3751.5(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  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 0.9987
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Nonius Kappa APEX II'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0910
_diffrn_reflns_av_unetI/netI     0.0726
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            56953
_diffrn_reflns_theta_full        25.0000
_diffrn_reflns_theta_max         25.37
_diffrn_reflns_theta_min         1.41
_exptl_absorpt_coefficient_mu    0.690
_exptl_absorpt_correction_T_max  0.2590
_exptl_absorpt_correction_T_min  0.2226
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0640 before and 0.0596 after correction. The Ratio of minimum to maximum transmission is 0.8595. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            Green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.3528
_exptl_crystal_description       Block
_exptl_crystal_F_000             1599.7282
_exptl_crystal_size_max          0.113
_exptl_crystal_size_mid          0.089
_exptl_crystal_size_min          0.074
_refine_diff_density_max         0.7787
_refine_diff_density_min         -0.7499
_refine_diff_density_rms         0.1436
_refine_ls_d_res_high            0.8293
_refine_ls_d_res_low             14.4660
_refine_ls_goodness_of_fit_ref   1.0351
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    93
_refine_ls_number_parameters     449
_refine_ls_number_reflns         6870
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.0348
_refine_ls_R_factor_all          0.0973
_refine_ls_R_factor_gt           0.0508
_refine_ls_shift/su_max          0.3432
_refine_ls_shift/su_mean         0.0111
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0586P)^2^+3.4881P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1148
_refine_ls_wR_factor_ref         0.1349
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              17
_reflns_limit_h_min              -17
_reflns_limit_k_max              15
_reflns_limit_k_min              0
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                4470
_reflns_number_total             6870
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d2dt01484j2.cif
_cod_data_source_block           RBabu_MP-05-076
_cod_depositor_comments
;
The following automatic conversions were performed:

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/RSC/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 
;
_cod_database_code               7710555
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
 C1SB-O1SB
 1.45 with sigma of 0.02
 O1SB-C2S
 1.45 with sigma of 0.02
 C4S-C1SB
 1.54 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C1SB) = Uanis(O1S)
Uanis(C1S) = Uanis(O1SB)
4. Rigid body (RIGU) restrains
 O1S, O1SB, C1S, C1SB, C2S, C3S, C4S
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Sof(O1SB)=Sof(C1SB)=Sof(H1Sc)=Sof(H1Sd)=Sof(H2Sc)=Sof(H2Sd)=Sof(H4Sc)=
 Sof(H4Sd)=1-FVAR(1)
 Sof(O1S)=Sof(C1S)=Sof(H1Sa)=Sof(H1Sb)=Sof(H2Sa)=Sof(H2Sb)=Sof(H4Sa)=Sof(H4Sb)=
 FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1a,H1b), C2(H2a,H2b), C3(H3a,H3b), C1S(H1Sa,H1Sb), C1SB(H1Sc,H1Sd),
 C2S(H2Sa,H2Sb), C2S(H2Sc,H2Sd), C3S(H3Sa,H3Sb), C4S(H4Sc,H4Sd), C4S(H4Sa,H4Sb)
6.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C11(H11), C12(H12), C13(H13),
 C14(H14), C15(H15), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C23(H23),
  C24(H24), C25(H25), C26(H26), C27(H27), C29(H29), C30(H30), C31(H31),
 C32(H32), C33(H33), C35(H35), C36(H36), C37(H37), C38(H38), C39(H39)
;
_olex2_submission_special_instructions 'No special instructions were received'