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_7716572
_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         'C28 H48 Co N2 P2'
_chemical_formula_sum            'C28 H48 Co N2 P2'
_chemical_formula_weight         533.55
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-05-05
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2024-02-23 deposited with the CCDC.	2024-06-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.876(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4942(3)
_cell_length_b                   13.3791(4)
_cell_length_c                   20.8730(6)
_cell_measurement_reflns_used    6852
_cell_measurement_temperature    98.0
_cell_measurement_theta_max      31.8920
_cell_measurement_theta_min      1.8230
_cell_volume                     2887.20(15)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      98.0
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -68.00  55.00   0.50   40.00    --  -35.00  70.00 270.00  246
  2  \w    -68.00  48.00   0.50   40.00    --  -35.00  70.00  90.00  232
  3  \w   -125.00 -80.00   0.50   40.00    --  -35.00   0.00 180.00   90
  4  \w    -71.00 -34.00   0.50   40.00    --  -35.00   0.00  90.00   74
  5  \w    -47.00 -20.00   0.50   40.00    --  -35.00  70.00   0.00   54
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0569983000
_diffrn_orient_matrix_UB_12      0.0188743000
_diffrn_orient_matrix_UB_13      0.0096169000
_diffrn_orient_matrix_UB_21      0.0292590000
_diffrn_orient_matrix_UB_22      -0.0043175000
_diffrn_orient_matrix_UB_23      0.0331232000
_diffrn_orient_matrix_UB_31      0.0244565000
_diffrn_orient_matrix_UB_32      0.0493440000
_diffrn_orient_matrix_UB_33      -0.0008113000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0531
_diffrn_reflns_av_unetI/netI     0.0511
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            20631
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.500
_diffrn_reflns_theta_min         1.816
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.723
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91839
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
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    1.227
_exptl_crystal_description       plate
_exptl_crystal_F_000             1148
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.557
_refine_diff_density_min         -0.361
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     313
_refine_ls_number_reflns         5983
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.137
_refine_ls_R_factor_all          0.0622
_refine_ls_R_factor_gt           0.0536
_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^)+(0.0410P)^2^+2.1890P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1107
_refine_ls_wR_factor_ref         0.1157
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5335
_reflns_number_total             5983
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01483a2.cif
_cod_data_source_block           cd1572a
_cod_depositor_comments
'Adding full bibliography for 7716570--7716574.cif.'
_cod_database_code               7716572
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Co1 N3 P2 C40 H20'
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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:
 C28(H28), C24(H24), C25(H25), C26(H26), C27(H27), C3(H3), C2(H2A)
2.c Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C17(H17A,H17B,H17C), C21(H21A,H21B,H21C), C16(H16A,H16B,
 H16C), C18(H18A,H18B,H18C), C7(H7A,H7B,H7C), C12(H12A,H12B,H12C), C20(H20A,
 H20B,H20C), C9(H9A,H9B,H9C), C8(H8A,H8B,H8C), C11(H11A,H11B,H11C), C13(H13A,
 H13B,H13C)
;
_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 1.173
_oxdiff_exptl_absorpt_empirical_full_min 0.894