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_7710554
_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_absolute_configuration ad
_chemical_formula_moiety         'C68 H72 Br2 Co2 P4'
_chemical_formula_sum            'C68 H72 Br2 Co2 P4'
_chemical_formula_weight         1290.81
_space_group_crystal_system      tetragonal
_space_group_IT_number           96
_space_group_name_Hall           'P 4nw 2abw'
_space_group_name_H-M_alt        'P 43 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-08-16
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   21.2718(9)
_cell_length_b                   21.2718(9)
_cell_length_c                   52.873(2)
_cell_measurement_reflns_used    9995
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      23.233
_cell_measurement_theta_min      2.175
_cell_volume                     23924.5(17)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.1535
_diffrn_reflns_av_unetI/netI     0.0650
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       58
_diffrn_reflns_limit_l_min       -58
_diffrn_reflns_number            319126
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        23.291
_diffrn_reflns_theta_max         23.291
_diffrn_reflns_theta_min         1.032
_diffrn_source                   'sealed tube'
_diffrn_source_type              fine-focus
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.039
_exptl_absorpt_correction_T_max  0.0243
_exptl_absorpt_correction_T_min  0.0078
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0910 before and 0.0759 after correction. The Ratio of minimum to maximum transmission is 0.3210. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'Dark Green'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_description       Block
_exptl_crystal_F_000             10624
_exptl_crystal_size_max          0.157
_exptl_crystal_size_mid          0.146
_exptl_crystal_size_min          0.092
_refine_diff_density_max         1.797
_refine_diff_density_min         -0.525
_refine_diff_density_rms         0.118
_refine_ls_abs_structure_details
;
 Flack x determined using 4481 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.006(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1369
_refine_ls_number_reflns         17222
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0982
_refine_ls_R_factor_gt           0.0693
_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^)+(0.0654P)^2^+81.9447P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1500
_refine_ls_wR_factor_ref         0.1638
_reflns_Friedel_coverage         0.789
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                13008
_reflns_number_total             17222
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01484j2.cif
_cod_data_source_block           RBabu_MP-05-066
_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/RSC/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 'Dark' was changed
to 'dark' 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.

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_original_cell_volume        23925(2)
_cod_database_code               7710554
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.835
_shelx_estimated_absorpt_t_min   0.740
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Ternary CH refined with riding coordinates:
 C3(H3), C6(H6), C19(H19), C22(H22), C37(H37), C40(H40), C53(H53), C56(H56),
 C3'(H3'), C6'(H6'), C19'(H19'), C22'(H22'), C37'(H37'), C40'(H40'), C53'(H53'),
  C56'(H56')
2.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C4(H4A,H4B), C5(H5A,H5B), C20(H20A,H20B), C21(H21A,
 H21B), C35(H35A,H35B), C36(H36A,H36B), C38(H38A,H38B), C39(H39A,H39B),
 C54(H54A,H54B), C55(H55A,H55B), C1'(H1'A,H1'B), C2'(H2'A,H2'B), C4'(H4'A,H4'B),
  C5'(H5'A,H5'B), C20'(H20C,H20D), C21'(H21C,H21D), C35'(H35C,H35D), C36'(H36C,
 H36D), C38'(H38C,H38D), C39'(H39C,H39D), C54'(H54C,H54D), C55'(H55C,H55D)
2.c 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), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28), C30(H30),
  C31(H31), C32(H32), C33(H33), C34(H34), C42(H42), C43(H43), C44(H44),
 C45(H45), C46(H46), C48(H48), C49(H49), C50(H50), C51(H51), C52(H52), C58(H58),
  C59(H59), C60(H60), C61(H61), C62(H62), C64(H64), C65(H65), C66(H66),
 C67(H67), C68(H68), C8'(H8'), C9'(H9'), C10'(H10'), C11'(H11'), C12'(H12'),
 C14'(H14'), C15'(H15'), C16'(H16'), C17'(H17'), C18'(H18'), C24'(H24'),
 C25'(H25'), C26'(H26'), C27'(H27'), C28'(H28'), C30'(H30'), C31'(H31'),
 C32'(H32'), C33'(H33'), C34'(H34'), C42'(H42'), C43'(H43'), C44'(H44'),
 C45'(H45'), C46'(H46'), C48'(H48'), C49'(H49'), C50'(H50'), C51'(H51'),
 C52'(H52'), C58'(H58'), C59'(H59'), C60'(H60'), C61'(H61'), C62'(H62'),
 C64'(H64'), C65'(H65'), C66'(H66'), C67'(H67'), C68'(H68')
;
_shelx_res_checksum              6494
_shelx_hkl_checksum              27874
_olex2_submission_special_instructions 'No special instructions were received'