Square-planar imido complexes of cobalt: synthesis, reactivity and computational study.
Reyna, Jackson A.; Krishnan, V. Mahesh; Silva Villatoro, Roberto; Arman, Hadi D.; Stoian, Sebastian A.; Tonzetich, Zachary J.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 12128–12137; doi:10.1039/d4dt01483a

data_7716573
_publ_section_title
;
 Square-planar imido complexes of cobalt: synthesis, reactivity and
 computational study.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12128
_journal_page_last               12137
_journal_paper_doi               10.1039/d4dt01483a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C31 H54 Co N2 P2'
_chemical_formula_sum            'C31 H54 Co N2 P2'
_chemical_formula_weight         575.63
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-03-10
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-02-23 deposited with the CCDC.	2024-06-25 downloaded from the CCDC.
;
_cell_angle_alpha                82.9900(10)
_cell_angle_beta                 87.941(2)
_cell_angle_gamma                78.642(2)
_cell_formula_units_Z            2
_cell_length_a                   8.2605(2)
_cell_length_b                   12.7200(2)
_cell_length_c                   15.1520(3)
_cell_measurement_reflns_used    19587
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      77.1340
_cell_measurement_theta_min      2.9220
_cell_volume                     1549.11(6)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_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 0.955
_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    -96.00 -20.00   0.50    0.29    --  -46.90 139.00 -43.00  152
  2  \w   -119.00 -70.00   0.50    0.29    --  -46.90-130.00  69.00   98
  3  \w    -89.00 -16.00   0.50    0.29    --  -46.90 130.00 142.00  146
  4  \w   -119.00 -64.00   0.50    0.29    --  -46.90-139.00-104.00  110
  5  \w     42.00 104.00   0.50    0.29    --   46.90-139.00-104.00  124
  6  \w     37.00  98.00   0.50    0.29    --   46.90-130.00  69.00  122
  7  \w   -164.00 -70.00   0.50    1.15    --  -91.75-130.00  69.00  188
  8  \w    -96.00 -20.00   0.50    1.15    --  -91.75 139.00 -43.00  152
  9  \w   -158.00 -64.00   0.50    1.15    --  -91.75-139.00-104.00  188
 10  \w    -89.00 -19.00   0.50    1.15    --  -91.75 130.00 142.00  140
 11  \w     86.00 174.00   0.50    1.15    --  109.48 139.00 -43.00  176
 12  \w     37.00 115.00   0.50    1.15    --  109.48-130.00  69.00  156
 13  \w     92.00 178.00   0.50    1.15    --  109.48 130.00 142.00  172
 14  \w     42.00 122.00   0.50    1.15    --  109.48-139.00-104.00  160
 15  \w   -119.00 -83.00   0.50    0.29    --  -46.90 -57.00-120.00   72
 16  \w   -119.00 -83.00   0.50    0.29    --  -46.90 -57.00-180.00   72
 17  \w   -119.00 -87.00   0.50    0.29    --  -46.90-125.00 -90.00   64
 18  \w   -119.00 -83.00   0.50    0.29    --  -46.90 -57.00 -60.00   72
 19  \w   -119.00 -83.00   0.50    0.29    --  -46.90 -57.00 -30.00   72
 20  \w   -119.00 -83.00   0.50    0.29    --  -46.90 -57.00-150.00   72
 21  \w     83.00 120.00   0.50    0.29    --   46.90  57.00 150.00   74
 22  \w     83.00 120.00   0.50    0.29    --   46.90  57.00   0.00   74
 23  \w   -164.00-101.00   0.50    1.15    --  -91.75 -77.00   0.00  126
 24  \w    -54.00 -19.00   0.50    1.15    --  -91.75  45.00   0.00   70
 25  \w    -54.00 -19.00   0.50    1.15    --  -91.75  45.00 -90.00   70
 26  \w    -74.00 -19.00   0.50    1.15    --  -91.75  61.00 -60.00  110
 27  \w   -164.00 -77.00   0.50    1.15    --  -91.75 -45.00 120.00  174
 28  \w    -54.00 -19.00   0.50    1.15    --  -91.75  45.00 120.00   70
 29  \w   -164.00-101.00   0.50    1.15    --  -91.75 -77.00 -90.00  126
 30  \w    -54.00 -19.00   0.50    1.15    --  -91.75  45.00  90.00   70
 31  \w    101.00 178.00   0.50    1.15    --  109.48  77.00 -30.00  154
 32  \w     37.00 105.00   0.50    1.15    --  109.48 -94.00 -90.00  136
 33  \w     37.00  98.00   0.50    1.15    --  109.48 -77.00  90.00  122
 34  \w     92.00 178.00   0.50    1.15    --  109.48  15.00 120.00  172
 35  \w     37.00  68.00   0.50    1.15    --  109.48 -61.00 -90.00   62
 36  \w     37.00 105.00   0.50    1.15    --  109.48 -94.00-180.00  136
 37  \w     37.00  68.00   0.50    1.15    --  109.48 -61.00-120.00   62
 38  \w     92.00 178.00   0.50    1.15    --  109.48  15.00  30.00  172
 39  \w     95.00 178.00   0.50    1.15    --  109.48  45.00-120.00  166
 40  \w     37.00 111.00   0.50    1.15    --  109.48-125.00  90.00  148
 41  \w     37.00  68.00   0.50    1.15    --  109.48 -61.00  90.00   62
 42  \w     95.00 178.00   0.50    1.15    --  109.48 125.00  90.00  166
 43  \w     37.00  98.00   0.50    1.15    --  109.48 -77.00 120.00  122
 44  \w     37.00  68.00   0.50    1.15    --  109.48 -61.00 -60.00   62
 45  \w   -121.00 -32.00   0.50    0.29    --  -46.90 -37.00  90.00  178
 46  \w   -121.00 -32.00   0.50    0.29    --  -46.90 -37.00 -90.00  178
 47  \w   -121.00 -32.00   0.50    0.29    --  -46.90 -37.00-180.00  178
 48  \w   -121.00 -32.00   0.50    0.29    --  -46.90 -37.00 -30.00  178
 49  \w   -121.00 -32.00   0.50    0.29    --  -46.90 -37.00  60.00  178
 50  \w   -121.00 -32.00   0.50    0.29    --  -46.90 -37.00-120.00  178
 51  \w   -121.00 -32.00   0.50    0.29    --  -46.90 -37.00 150.00  178
 52  \w   -121.00 -32.00   0.50    0.29    --  -46.90 -37.00   0.00  178
;
_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      0.0634192000
_diffrn_orient_matrix_UB_12      -0.1133109000
_diffrn_orient_matrix_UB_13      -0.0283178000
_diffrn_orient_matrix_UB_21      0.0095238000
_diffrn_orient_matrix_UB_22      -0.0484089000
_diffrn_orient_matrix_UB_23      0.0983948000
_diffrn_orient_matrix_UB_31      -0.1791021000
_diffrn_orient_matrix_UB_32      -0.0170473000
_diffrn_orient_matrix_UB_33      -0.0034658000
_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  0.0462
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            35236
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.957
_diffrn_reflns_theta_min         2.939
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.465
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76217
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear greenish violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_description       plank
_exptl_crystal_F_000             622
_exptl_crystal_size_max          0.162
_exptl_crystal_size_mid          0.052
_exptl_crystal_size_min          0.046
_refine_diff_density_max         0.529
_refine_diff_density_min         -0.489
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         6334
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0352
_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^)+(0.0454P)^2^+0.8357P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0887
_refine_ls_wR_factor_ref         0.0894
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6084
_reflns_number_total             6334
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01483a2.cif
_cod_data_source_block           hpd636_auto
_cod_depositor_comments
'Adding full bibliography for 7716570--7716574.cif.'
_cod_database_code               7716573
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Ni C H N O P'
_chemical_oxdiff_usercomment     'Ni(PNP) JR'
_shelx_estimated_absorpt_t_max   0.787
_shelx_estimated_absorpt_t_min   0.471
_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:
 C14(H14A,H14B), C5(H5A,H5B)
2.b Aromatic/amide H refined with riding coordinates:
 C25(H25), C3(H3), C2(H2A), C27(H27)
2.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C34(H34A,H34B,H34C), C9(H9A,H9B,H9C), C8(H8A,H8B,H8C),
 C29(H29A,H29B,H29C), C13(H13A,H13B,H13C), C21(H21A,H21B,H21C), C20(H20A,H20B,
 H20C), C17(H17A,H17B,H17C), C22(H22A,H22B,H22C), C12(H12A,H12B,H12C), C11(H11A,
 H11B,H11C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C30(H30A,H30B,H30C)
;
_shelx_res_checksum              32036
_shelx_hkl_checksum              24052
_olex2_exptl_crystal_mounting_method 'nylon loop'
_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 1.466
_oxdiff_exptl_absorpt_empirical_full_min 0.823