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_7130600
_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 Cl Co N2 P2, Cl3 Co'
_chemical_formula_sum            'C40 H41 Cl4 Co2 N2 P2'
_chemical_formula_weight         871.35
_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             2021-05-27
_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                 100.2250(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.21000(10)
_cell_length_b                   15.25040(10)
_cell_length_c                   17.82880(10)
_cell_measurement_reflns_used    24377
_cell_measurement_temperature    103(6)
_cell_measurement_theta_max      76.5680
_cell_measurement_theta_min      3.8360
_cell_volume                     3802.29(4)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      103(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 0.999
_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    -40.00  15.00   0.50    8.18    --  -49.84  37.00  23.00  110
  2  \w    -42.00 -17.00   0.50   32.72    --  -82.50  37.00  23.00   50
  3  \w    -34.00  22.00   0.50    8.18    --  -49.84  37.00 150.00  112
  4  \w     46.00  89.00   0.50    8.18    --   49.84  37.00  23.00   86
  5  \w    118.00 169.00   0.50   32.72    --  104.00  37.00  23.00  102
  6  \w    149.00 175.00   0.50   32.72    --  104.00  61.00   0.00   52
  7  \w    137.00 174.00   0.50   32.72    --  104.00  77.00 -90.00   74
  8  \w    104.00 131.00   0.50   32.72    --  104.00  15.00 -30.00   54
  9  \w    102.00 137.00   0.50   32.72    --  104.00  45.00 -30.00   70
 10  \w    113.00 139.00   0.50   32.72    --  104.00  61.00   0.00   52
 11  \w    111.00 137.00   0.50   32.72    --  104.00  45.00   0.00   52
 12  \w     91.00 117.00   0.50   32.72    --  104.00  77.00 -90.00   52
 13  \w     97.00 123.00   0.50   32.72    --  104.00  45.00 -90.00   52
 14  \w     99.00 159.00   0.50   32.72    --  104.00  30.00-120.00  120
 15  \w     85.00 110.00   0.50   32.72    --  104.00   0.00  60.00   50
 16  \w    127.00 176.00   0.50   32.72    --  104.00  15.00 120.00   98
 17  \w    149.00 175.00   0.50   32.72    --  104.00  61.00  90.00   52
 18  \w    114.00 140.00   0.50   32.72    --  104.00  61.00  90.00   52
 19  \w     96.00 171.00   0.50   32.72    --  104.00 125.00 150.00  150
 20  \w     40.00  65.00   0.50   32.72    --  104.00 -61.00  90.00   50
 21  \w     35.00  69.00   0.50   32.72    --  104.00 -61.00 150.00   68
 22  \w     40.00  95.00   0.50   32.72    --  104.00 -77.00 120.00  110
 23  \w     57.00  83.00   0.50   32.72    --  104.00-104.00  38.62   52
 24  \w     40.00  95.00   0.50   32.72    --  104.00 -94.00  60.00  110
 25  \w     41.00  70.00   0.50   32.72    --  104.00 -61.00 120.00   58
 26  \w     48.00  74.00   0.50   32.72    --  104.00 -73.00 129.64   52
 27  \w     52.00  78.00   0.50   32.72    --  104.00-115.00 158.76   52
 28  \w     42.00  70.00   0.50   32.72    --  104.00-125.00 120.00   56
 29  \w     33.00  83.00   0.50   32.72    --  104.00-105.00 154.01  100
 30  \w     38.00  71.00   0.50   32.72    --  104.00 -61.00  60.00   66
 31  \w     34.00  96.00   0.50   32.72    --  104.00  -2.00  87.28  124
 32  \w     35.00  70.00   0.50   32.72    --  104.00 -61.00 -30.00   70
 33  \w     60.00 104.00   0.50   32.72    --  104.00 -77.00 -60.00   88
 34  \w     49.00  75.00   0.50   32.72    --  104.00-115.00-159.99   52
 35  \w     78.00 108.00   0.50   32.72    --  104.00-115.00-159.99   60
 36  \w     61.00 105.00   0.50   32.72    --  104.00 -77.00-180.00   88
 37  \w     61.00  86.00   0.50   32.72    --  104.00   0.00-180.00   50
 38  \w     43.00  68.00   0.50   32.72    --  104.00 -61.00-180.00   50
 39  \w     45.00  84.00   0.50   32.72    --  104.00 -94.00-120.00   78
 40  \w     41.00  69.00   0.50   32.72    --  104.00 -61.00 -90.00   56
 41  \w     32.00  69.00   0.50   32.72    --  104.00 -61.00-120.00   74
 42  \w     33.00  59.00   0.50   32.72    --  104.00-109.00-179.64   52
 43  \w     34.00  79.00   0.50   32.72    --  104.00 -94.00 -90.00   90
 44  \w    -14.00  11.00   0.50    8.18    --   49.84 -37.00-132.00   50
 45  \w     -8.00  25.00   0.50    8.18    --   49.84 -19.00  90.00   66
 46  \w   -121.00 -52.00   0.50    8.18    --  -49.84 -37.00-132.00  138
 47  \w   -116.00 -86.00   0.50    8.18    --  -49.84-125.00  30.00   60
 48  \w   -140.00-115.00   0.50   32.72    --  -82.50 -37.00-132.00   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      -0.0111362000
_diffrn_orient_matrix_UB_12      -0.0277380000
_diffrn_orient_matrix_UB_13      -0.0841920000
_diffrn_orient_matrix_UB_21      -0.1019959000
_diffrn_orient_matrix_UB_22      0.0382831000
_diffrn_orient_matrix_UB_23      -0.0154095000
_diffrn_orient_matrix_UB_31      0.0401717000
_diffrn_orient_matrix_UB_32      0.0892580000
_diffrn_orient_matrix_UB_33      -0.0195931000
_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  0.0447
_diffrn_reflns_av_unetI/netI     0.0292
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            50524
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.499
_diffrn_reflns_theta_min         3.676
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.466
_exptl_absorpt_correction_T_max  0.709
_exptl_absorpt_correction_T_min  0.398
_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 green'
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_description       block
_exptl_crystal_F_000             1788
_exptl_crystal_size_max          0.138
_exptl_crystal_size_mid          0.068
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.665
_refine_diff_density_min         -0.405
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     453
_refine_ls_number_reflns         7755
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0413
_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^)+(0.0728P)^2^+2.3461P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1142
_refine_ls_wR_factor_ref         0.1173
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7069
_reflns_number_total             7755
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc04089a2.cif
_cod_data_source_block           ras2_abs
_cod_original_cell_volume        3802.28(4)
_cod_database_code               7130600
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C40H41Cl4N2P2Co2
_chemical_oxdiff_usercomment     'Crystallized from chloroform.'
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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:
 C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C26(H26A,H26B), C27(H27A,
 H27B), C28(H28A,H28B)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19),
 C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C30(H30), C31(H31), C32(H32),
  C33(H33), C34(H34), C36(H36), C37(H37), C38(H38), C39(H39), C40(H40)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C9(H9A,H9B,H9C)
;
_shelx_res_checksum              78654
_shelx_hkl_checksum              76504
_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 1.353
_oxdiff_exptl_absorpt_empirical_full_min 0.766