An Aryl Diimine Cobalt(I) Catalyst for Carbonyl Hydrosilylation
Sharma, Anuja; So, Sangho; Kim, Jun-Hyeong; MacMillan, Samantha N.; Baik, Mu-Hyun; Trovitch, Ryan J.; Chemical Communications  (2022) –; doi:10.1039/D2CC04089A

data_7130601
_publ_section_title
;
 An Aryl Diimine Cobalt(I) Catalyst for Carbonyl Hydrosilylation
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC04089A
_journal_year                    2022
_chemical_formula_moiety         'C40 H41 Co N2 P2'
_chemical_formula_sum            'C40 H41 Co N2 P2'
_chemical_formula_weight         670.62
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-04-09
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.03.28 svn.rd84adfe8 for Rigaku Oxford Diffraction, GUI svn.r6032)
;
_audit_update_record
;
2022-06-02 deposited with the CCDC.	2022-08-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.7683(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.46782(6)
_cell_length_b                   20.13749(9)
_cell_length_c                   19.21388(7)
_cell_measurement_reflns_used    60125
_cell_measurement_temperature    100.0(6)
_cell_measurement_theta_max      77.0670
_cell_measurement_theta_min      3.1580
_cell_volume                     6750.75(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(6)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -25.00  18.00   0.50    2.51    --  -50.09  19.00 120.00   86
  2  \w    -20.00  20.00   0.50    2.51    --  -50.09  19.00 -30.00   80
  3  \w    -25.00  22.00   0.50    2.51    --  -50.09  19.00-120.00   94
  4  \w    -40.00 -12.00   0.50   10.05    --  -82.50  45.00 -30.00   56
  5  \w    -87.00 -31.00   0.50    2.51    --  -50.09 127.00 119.00  112
  6  \w    -20.00  25.00   0.50    2.51    --   50.09 -19.00 -90.00   90
  7  \w     42.00  72.00   0.50   10.05    --  104.00 -94.00 -90.00   60
  8  \w     77.00 104.00   0.50   10.05    --  104.00 -94.00 -90.00   54
  9  \w     76.00 104.00   0.50   10.05    --  104.00 -77.00 -90.00   56
 10  \w     76.00 106.00   0.50   10.05    --  104.00 -94.00-120.00   60
 11  \w     76.00 102.00   0.50   10.05    --  104.00-142.00-125.00   52
 12  \w     50.00  75.00   0.50    2.51    --   50.09-142.00-125.00   50
 13  \w     66.00 101.00   0.50   10.05    --  104.00 -94.00 -30.00   70
 14  \w     76.00 105.00   0.50   10.05    --  104.00-102.00  18.16   58
 15  \w     80.00 105.00   0.50   10.05    --  104.00 -94.00  90.00   50
 16  \w     83.00 111.00   0.50   10.05    --  104.00 -78.00 104.15   56
 17  \w     68.00 104.00   0.50   10.05    --  104.00 -94.00 120.00   72
 18  \w     61.00 112.00   0.50   10.05    --  104.00-125.00  60.00  102
 19  \w     49.00 107.00   0.50   10.05    --  104.00-107.00 108.47  116
 20  \w     37.00  67.00   0.50    2.51    --   50.09-127.00  44.00   60
 21  \w     37.00  90.00   0.50   10.05    --  104.00-127.00  44.00  106
 22  \w     36.00  68.00   0.50   10.05    --  104.00 -77.00  30.00   64
 23  \w     36.00 101.00   0.50   10.05    --  104.00 -94.00  30.00  130
 24  \w     34.00  60.00   0.50   10.05    --  104.00 -77.00 150.00   52
 25  \w     36.00  71.00   0.50   10.05    --  104.00 -61.00 120.00   70
 26  \w     33.00  58.00   0.50   10.05    --  104.00 -77.00 120.00   50
 27  \w     33.00  65.00   0.50   10.05    --  104.00 -61.00  90.00   64
 28  \w     67.00  92.00   0.50   10.05    --  104.00   0.00  30.00   50
 29  \w    100.00 149.00   0.50   10.05    --  104.00  15.00   0.00   98
 30  \w    132.00 176.00   0.50   10.05    --  104.00  15.00  30.00   88
 31  \w    147.00 173.00   0.50   10.05    --  104.00  69.00 -66.11   52
 32  \w    122.00 174.00   0.50   10.05    --  104.00 122.00  44.62  104
 33  \w    118.00 144.00   0.50   10.05    --  104.00 127.00 119.00   52
 34  \w    116.00 176.00   0.50   10.05    --  104.00  94.00 124.32  120
 35  \w    129.00 170.00   0.50   10.05    --  104.00  86.00 163.33   82
 36  \w    108.00 154.00   0.50   10.05    --  104.00  30.00 120.00   92
 37  \w    106.00 150.00   0.50   10.05    --  104.00  30.00  60.00   88
 38  \w    100.00 140.00   0.50   10.05    --  104.00  15.00 120.00   80
 39  \w     92.00 136.00   0.50   10.05    --  104.00  61.00  60.00   88
 40  \w    118.00 144.00   0.50   10.05    --  104.00 125.00 -30.00   52
 41  \w    104.00 129.00   0.50   10.05    --  104.00 142.00 -69.00   50
 42  \w     91.00 117.00   0.50   10.05    --  104.00  69.00 -66.11   52
 43  \w    102.00 128.00   0.50   10.05    --  104.00  15.00-150.00   52
 44  \w     85.00 175.00   0.50   10.05    --  104.00  77.00 -60.00  180
 45  \w     81.00 107.00   0.50   10.05    --  104.00   0.00 -60.00   52
 46  \w     58.00 111.00   0.50   10.05    --  104.00   0.00-180.00  106
 47  \w     46.00  72.00   0.50   10.05    --  104.00 -94.00-180.00   52
 48  \w     52.00 100.00   0.50   10.05    --  104.00-125.00-150.00   96
 49  \w     36.00 100.00   0.50   10.05    --  104.00-125.00-180.00  128
 50  \w     32.00  68.00   0.50   10.05    --  104.00 -61.00-150.00   72
 51  \w    -16.00  25.00   0.50    2.51    --   50.09 -19.00  60.00   82
 52  \w   -100.00 -73.00   0.50    2.51    --  -50.09-127.00  44.00   54
 53  \w   -103.00 -69.00   0.50    2.51    --  -50.09-142.00-125.00   68
 54  \w   -132.00-107.00   0.50   10.05    --  -82.50-142.00-125.00   50
 55  \w   -128.00-103.00   0.50   10.05    --  -82.50-127.00  44.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0215051000
_diffrn_orient_matrix_UB_12      0.0104354000
_diffrn_orient_matrix_UB_13      -0.0779861000
_diffrn_orient_matrix_UB_21      0.0075764000
_diffrn_orient_matrix_UB_22      0.0756942000
_diffrn_orient_matrix_UB_23      0.0097851000
_diffrn_orient_matrix_UB_31      0.0852514000
_diffrn_orient_matrix_UB_32      -0.0040619000
_diffrn_orient_matrix_UB_33      -0.0164694000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0332
_diffrn_reflns_av_unetI/netI     0.0203
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            108237
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.243
_diffrn_reflns_theta_min         3.181
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.111
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.254
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.81a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear brown'
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_description       block
_exptl_crystal_F_000             2816
_exptl_crystal_size_max          0.323
_exptl_crystal_size_mid          0.135
_exptl_crystal_size_min          0.082
_refine_diff_density_max         0.287
_refine_diff_density_min         -0.476
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     815
_refine_ls_number_reflns         14138
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0336
_refine_ls_R_factor_gt           0.0309
_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^)+(0.0452P)^2^+2.8508P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0809
_refine_ls_wR_factor_ref         0.0827
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13178
_reflns_number_total             14138
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc04089a2.cif
_cod_data_source_block           ras1_abs
_cod_original_cell_volume        6750.75(4)
_cod_database_code               7130601
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C79H82Co2N5P4
_chemical_oxdiff_usercomment     'Crystallized from toluene/ether.'
_reflns_odcompleteness_completeness 97.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     77.83
_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.a Secondary CH2 refined with riding coordinates:
 C11A(H11A,H11B), C12A(H12A,H12B), C13A(H13A,H13B), C26A(H26A,H26B), C27A(H27A,
 H27B), C28A(H28A,H28B), C11B(H11C,H11D), C12B(H12C,H12D), C13B(H13C,H13D),
 C26B(H26C,H26D), C27B(H27C,H27D), C28B(H28C,H28D)
2.b Aromatic/amide H refined with riding coordinates:
 C4A(H4A), C5A(H5A), C6A(H6A), C15A(H15A), C16A(H16A), C17A(H17A), C18A(H18A),
 C19A(H19A), C21A(H21A), C22A(H22A), C23A(H23A), C24A(H24A), C25A(H25A),
 C30A(H30A), C31A(H31A), C32A(H32A), C33A(H33A), C34A(H34A), C36A(H36A),
 C37A(H37A), C38A(H38A), C39A(H39A), C40A(H40A), C4B(H4B), C5B(H5B), C6B(H6B),
 C15B(H15B), C16B(H16B), C17B(H17B), C18B(H18B), C19B(H19B), C21B(H21B),
 C22B(H22B), C23B(H23B), C24B(H24B), C25B(H25B), C30B(H30B), C31B(H31B),
 C32B(H32B), C33B(H33B), C34B(H34B), C36B(H36B), C37B(H37B), C38B(H38B),
 C39B(H39B), C40B(H40B)
2.c Idealised Me refined as rotating group:
 C1A(H1AA,H1AB,H1AC), C9A(H9AA,H9AB,H9AC), C1B(H1BA,H1BB,H1BC), C9B(H9BA,H9BB,
 H9BC)
;
_shelx_res_checksum              34434
_shelx_hkl_checksum              24536
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.367
_oxdiff_exptl_absorpt_empirical_full_min 0.768