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_7716570
_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 H53 Co N2 P2'
_chemical_formula_sum            'C31 H53 Co N2 P2'
_chemical_formula_weight         574.62
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-12-02
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.10.09 svn.r3662 for Rigaku Oxford Diffraction, GUI svn.r5959)
;
_audit_update_record
;
2024-02-23 deposited with the CCDC.	2024-06-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.5770(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.46810(10)
_cell_length_b                   15.3341(2)
_cell_length_c                   19.6726(2)
_cell_measurement_reflns_used    20219
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.0940
_cell_measurement_theta_min      3.6660
_cell_volume                     3082.05(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.63a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.63a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.63a (Rigaku OD, 2019)'
_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 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT n/a (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 0.999
_diffrn_measured_fraction_theta_max 0.968
_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    -42.00  27.00   0.50    0.70    --  -46.87  36.00  -6.00  138
  2  \w    -42.00 -14.00   0.50    2.80    --  -88.50  36.00  -6.00   56
  3  \w    -71.00 -15.00   0.50    2.80    --  -88.50  61.00  90.00  112
  4  \w    -30.00  29.00   0.50    0.70    --  -46.87  19.00 120.00  118
  5  \w    -51.00 -16.00   0.50    2.80    --  -88.50  45.00 150.00   70
  6  \w   -121.00 -32.00   0.50    0.70    --  -46.87 -37.00 -60.00  178
  7  \w    -51.00 -16.00   0.50    2.80    --  -88.50  45.00-180.00   70
  8  \w    -51.00 -16.00   0.50    2.80    --  -88.50  45.00-150.00   70
  9  \w   -121.00 -32.00   0.50    0.70    --  -46.87 -36.00-162.00  178
 10  \w    -27.00  42.00   0.50    0.70    --   46.87 -36.00-162.00  138
 11  \w     32.00 121.00   0.50    0.70    --   46.87  37.00-180.00  178
 12  \w     32.00 121.00   0.50    0.70    --   46.87  36.00  -6.00  178
 13  \w     92.00 178.00   0.50    2.80    --  106.69  36.00  -6.00  172
 14  \w     91.00 178.00   0.50    2.80    --  106.69  61.00  90.00  174
 15  \w     34.00  71.00   0.50    2.80    --  106.69 -61.00  60.00   74
 16  \w     34.00  71.00   0.50    2.80    --  106.69 -61.00   0.00   74
 17  \w     34.00  71.00   0.50    2.80    --  106.69 -61.00 -60.00   74
 18  \w     34.00  71.00   0.50    2.80    --  106.69 -61.00 -90.00   74
 19  \w     34.00  71.00   0.50    2.80    --  106.69 -61.00-120.00   74
 20  \w     34.00  71.00   0.50    2.80    --  106.69 -61.00-180.00   74
 21  \w     34.00 101.00   0.50    2.80    --  106.69 -77.00-180.00  134
 22  \w     34.00  71.00   0.50    2.80    --  106.69 -61.00-150.00   74
 23  \w     34.00 105.00   0.50    2.80    --  106.69 -94.00   0.00  142
 24  \w     34.00 105.00   0.50    2.80    --  106.69 -94.00  60.00  142
 25  \w     34.00  71.00   0.50    2.80    --  106.69 -61.00 120.00   74
 26  \w     32.00 121.00   0.50    0.70    --   46.87  37.00  90.00  178
 27  \w   -120.00 -87.00   0.50    0.70    --  -46.87-125.00 -90.00   66
 28  \w   -120.00 -87.00   0.50    0.70    --  -46.87-125.00 -30.00   66
 29  \w   -162.00 -73.00   0.50    2.80    --  -88.50 -36.00-162.00  178
 30  \w   -160.00-100.00   0.50    2.80    --  -88.50 -94.00 -60.00  120
;
_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      -0.0686992000
_diffrn_orient_matrix_UB_12      0.0047411000
_diffrn_orient_matrix_UB_13      -0.0775791000
_diffrn_orient_matrix_UB_21      0.1177196000
_diffrn_orient_matrix_UB_22      -0.0464099000
_diffrn_orient_matrix_UB_23      -0.0195847000
_diffrn_orient_matrix_UB_31      -0.0646019000
_diffrn_orient_matrix_UB_32      -0.0889306000
_diffrn_orient_matrix_UB_33      0.0060443000
_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  0.0335
_diffrn_reflns_av_unetI/netI     0.0226
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            35706
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.558
_diffrn_reflns_theta_min         3.689
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.493
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.760
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.63a (Rigaku Oxford Diffraction, 2019)
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 red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.238
_exptl_crystal_description       plate
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.124
_exptl_crystal_size_mid          0.099
_exptl_crystal_size_min          0.043
_refine_diff_density_max         0.282
_refine_diff_density_min         -0.294
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         6280
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0343
_refine_ls_R_factor_gt           0.0322
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0358P)^2^+1.8377P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0776
_refine_ls_wR_factor_ref         0.0787
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5946
_reflns_number_total             6280
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01483a2.cif
_cod_data_source_block           hpd045
_cod_depositor_comments
'Adding full bibliography for 7716570--7716574.cif.'
_cod_database_code               7716570
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         Co1N1P2C30H20
_chemical_oxdiff_usercomment     'Co(PNP)t-butyl mesityl'
_shelx_estimated_absorpt_t_max   0.798
_shelx_estimated_absorpt_t_min   0.549
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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:
 C27(H27), C25(H25), C2(H2), C3(H3)
2.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C9(H9A,H9B,H9C), C29(H29A,H29B,H29C), C12(H12A,H12B,
 H12C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C22(H22A,H22B,H22C), C31(H31A,H31B,
 H31C), C13(H13A,H13B,H13C), C30(H30A,H30B,H30C), C17(H17A,H17B,H17C), C16(H16A,
 H16B,H16C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C)
;
_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 1.389
_oxdiff_exptl_absorpt_empirical_full_min 0.780