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_7716574
_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         'C34 H52 Co N5 P2, C6 H6'
_chemical_formula_sum            'C40 H58 Co N5 P2'
_chemical_formula_weight         729.78
_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             2023-05-30
_audit_creation_method
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_audit_update_record
;
2024-02-23 deposited with the CCDC.	2024-06-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.9130(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.1588(3)
_cell_length_b                   9.92290(10)
_cell_length_c                   20.4294(2)
_cell_measurement_reflns_used    15704
_cell_measurement_temperature    100.01(13)
_cell_measurement_theta_max      74.3830
_cell_measurement_theta_min      2.3440
_cell_volume                     3874.80(8)
_computing_cell_refinement       'CrysAlisPro 1.171.42.79a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.79a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.79a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-024 (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      100.01(13)
_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 0.943
_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   -120.00 -26.00   0.50    2.39    --  -45.30 -42.00  36.00  188
  2  \w    -48.00  29.00   0.50    2.39    --  -45.30  42.00-171.00  154
  3  \w    -29.00  48.00   0.50    2.39    --   45.30 -42.00  36.00  154
  4  \w     27.00 120.00   0.50    2.39    --   45.30  42.00-171.00  186
  5  \w   -168.00 -74.00   0.50    9.54    --  -93.75 -42.00  36.00  188
  6  \w    -48.00 -19.00   0.50    9.54    --  -93.75  42.00-171.00   58
  7  \w     88.00 178.00   0.50    9.54    --  107.26  42.00-171.00  180
  8  \w    -86.00 -13.00   0.50    2.39    --  -45.30 125.00-120.00  146
  9  \w     34.00  94.00   0.50    2.39    --   45.30-125.00  30.00  120
 10  \w     83.00 119.00   0.50    2.39    --   45.30  57.00 120.00   72
 11  \w    -51.00 -20.00   0.50    9.54    --  -93.75  45.00-150.00   62
 12  \w    -51.00 -20.00   0.50    9.54    --  -93.75  45.00 -90.00   62
 13  \w   -101.00 -20.00   0.50    9.54    --  -93.75  77.00  30.00  162
 14  \w    -51.00 -20.00   0.50    9.54    --  -93.75  45.00   0.00   62
 15  \w   -167.00-100.00   0.50    9.54    --  -93.75 -94.00 150.00  134
 16  \w    -51.00 -20.00   0.50    9.54    --  -93.75  45.00 150.00   62
 17  \w    -71.00 -20.00   0.50    9.54    --  -93.75  61.00   0.00  102
 18  \w    -51.00 -20.00   0.50    9.54    --  -93.75  45.00 120.00   62
 19  \w    -51.00 -20.00   0.50    9.54    --  -93.75  45.00  30.00   62
 20  \w   -167.00-101.00   0.50    9.54    --  -93.75 -77.00 -30.00  132
 21  \w     89.00 178.00   0.50    9.54    --  107.26  45.00-120.00  178
 22  \w     34.00  71.00   0.50    9.54    --  107.26 -61.00 -60.00   74
 23  \w     34.00  71.00   0.50    9.54    --  107.26 -61.00  30.00   74
 24  \w     34.00 101.00   0.50    9.54    --  107.26 -77.00 120.00  134
 25  \w     34.00  71.00   0.50    9.54    --  107.26 -61.00 -90.00   74
 26  \w     34.00  71.00   0.50    9.54    --  107.26 -61.00-120.00   74
 27  \w   -119.00 -83.00   0.50    2.39    --  -45.30 -57.00 150.00   72
 28  \w   -119.00 -27.00   0.50    2.39    --  -45.30 -54.00-122.17  184
 29  \w   -119.00 -28.00   0.50    2.39    --  -45.30 -52.00 154.29  182
 30  \w   -119.00 -27.00   0.50    2.39    --  -45.30 -54.00 -49.69  184
;
_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      0.0765605000
_diffrn_orient_matrix_UB_12      0.0314432000
_diffrn_orient_matrix_UB_13      -0.0132358000
_diffrn_orient_matrix_UB_21      -0.0093087000
_diffrn_orient_matrix_UB_22      -0.0760232000
_diffrn_orient_matrix_UB_23      -0.0658210000
_diffrn_orient_matrix_UB_31      -0.0234444000
_diffrn_orient_matrix_UB_32      0.1316539000
_diffrn_orient_matrix_UB_33      -0.0347022000
_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  0.0533
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.943
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            44268
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.943
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.356
_diffrn_reflns_theta_min         2.312
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.507
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.787
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.79a (Rigaku Oxford Diffraction, 2022)
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 dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.251
_exptl_crystal_description       plate
_exptl_crystal_F_000             1560
_exptl_crystal_size_max          0.128
_exptl_crystal_size_mid          0.061
_exptl_crystal_size_min          0.031
_refine_diff_density_max         0.456
_refine_diff_density_min         -0.389
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         7672
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_gt           0.0435
_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^)+(0.0371P)^2^+2.9000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0966
_refine_ls_wR_factor_ref         0.0992
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6904
_reflns_number_total             7672
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01483a2.cif
_cod_data_source_block           hpd711_auto
_cod_depositor_comments
'Adding full bibliography for 7716570--7716574.cif.'
_cod_database_code               7716574
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Co C H N O P'
_chemical_oxdiff_usercomment     'Jackson Sample'
_shelx_estimated_absorpt_t_max   0.873
_shelx_estimated_absorpt_t_min   0.596
_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:
 C5(H5A,H5B), C14(H14A,H14B)
2.b Aromatic/amide H refined with riding coordinates:
 C34(H34), C30(H30), C33(H33), C3(H3), C31(H31), C27(H27), C32(H32), C2(H2),
 C28(H28), C26(H26), C25(H25), C24(H24), C40(H40), C35(H35), C36(H36), C37(H37),
  C38(H38), C39(H39)
2.c Fitted hexagon refined as free rotating group:
 C40(C35,C36,C37,C38,C39)
2.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C12(H12A,H12B,H12C), C7(H7A,H7B,H7C), C20(H20A,H20B,
 H20C), C18(H18A,H18B,H18C), C8(H8A,H8B,H8C), C11(H11A,H11B,H11C), C17(H17A,
 H17B,H17C), C9(H9A,H9B,H9C), C22(H22A,H22B,H22C), C13(H13A,H13B,H13C),
 C21(H21A,H21B,H21C)
;
_shelx_res_checksum              16731
_shelx_hkl_checksum              96777
_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
- Detector area scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.730
_oxdiff_exptl_absorpt_empirical_full_min 0.758