Synthesis and electronic structure elucidation of bioinspired heterobimetallic nickel complexes.
Patterson, Claire R.; Oyala, Paul H.; Buss, Joshua A.; Chemical communications (Cambridge, England) 61 (2025) 12345–12348; doi:10.1039/d5cc03435c

data_7134944
_publ_section_title
;
 Synthesis and electronic structure elucidation of bioinspired
 heterobimetallic nickel complexes.
;
_journal_issue                   66
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              12345
_journal_page_last               12348
_journal_paper_doi               10.1039/d5cc03435c
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C40 H45 Co N6 Ni O5, C F3 O3 S, C2 H3 N'
_chemical_formula_sum            'C43 H48 Co F3 N7 Ni O8 S'
_chemical_formula_weight         997.58
_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             2025-05-28
_audit_creation_method
;
Olex2 1.5
(compiled 2025.05.22 svn.r631f81ec for OlexSys, GUI svn.r7248)
;
_audit_update_record
;
2025-05-29 deposited with the CCDC.	2025-07-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.2680(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.48850(10)
_cell_length_b                   21.9395(2)
_cell_length_c                   19.6735(2)
_cell_measurement_reflns_used    19986
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      69.2150
_cell_measurement_theta_min      3.0130
_cell_volume                     4500.05(8)
_computing_cell_refinement       'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.978
_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   -110.00  70.00   1.00    1.00    --  -20.00   0.00-180.00  180
  2  \w    -45.00   0.00   1.00    1.00    --  -20.00  72.00   0.00   45
  3  \w    -45.00   0.00   1.00    1.00    --  -20.00  72.00   0.00   45
  4  \w    -25.00  43.00   1.00    1.00    --  -20.00  36.00 120.00   68
  5  \w    -45.00   0.00   1.00    1.00    --  -20.00  72.00-180.00   45
  6  \w   -173.00-128.00   1.00    8.00    --  -92.00 -36.00 120.00   45
  7  \w   -133.00 -88.00   1.00    8.00    --  -92.00 -36.00 -60.00   45
  8  \w   -104.00 -59.00   1.00    8.00    --  -92.00  36.00  60.00   45
  9  \w   -122.00 -77.00   1.00    8.00    --  -92.00 -72.00  60.00   45
 10  \w   -174.00 -78.00   1.00    8.00    --  -92.00 -72.00-120.00   96
 11  \w    -93.00 -35.00   1.00    8.00    --  -92.00  36.00-120.00   58
 12  \w   -176.00 -77.00   1.00    8.00    --  -92.00 -72.00 -60.00   99
 13  \w   -147.00 -75.00   1.00    8.00    --  -92.00 -72.00-180.00   72
 14  \w   -176.00 -77.00   1.00    8.00    --  -92.00 -72.00 120.00   99
 15  \w   -177.00-116.00   1.00    8.00    --  -92.00 -36.00  60.00   61
 16  \w    -87.00  -9.00   1.00    8.00    --  -92.00  36.00 -60.00   78
 17  \w   -102.00 -14.00   1.00    8.00    --  -92.00  36.00   0.00   88
 18  \w   -102.00 -21.00   1.00    8.00    --  -92.00  72.00 120.00   81
 19  \w   -175.00-104.00   1.00    8.00    --  -92.00 -36.00   0.00   71
 20  \w   -104.00 -52.00   1.00    8.00    --  -92.00  72.00  60.00   52
 21  \w   -109.00 -14.00   1.00    8.00    --  -92.00  72.00-120.00   95
 22  \w   -105.00 -24.00   1.00    8.00    --  -92.00  36.00-120.00   81
 23  \w   -105.00  -2.00   1.00    8.00    --  -92.00  36.00-180.00  103
 24  \w   -106.00  -2.00   1.00    8.00    --  -92.00  72.00 -60.00  104
 25  \w   -106.00  -2.00   1.00    8.00    --  -92.00  72.00 -60.00  104
 26  \w   -107.00 -29.00   1.00    8.00    --  -92.00  72.00   0.00   78
 27  \w   -117.00 -72.00   1.00    8.00    --  -92.00  72.00 180.00   45
;
_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      -0.1460985000
_diffrn_orient_matrix_UB_12      0.0046079000
_diffrn_orient_matrix_UB_13      -0.0194320000
_diffrn_orient_matrix_UB_21      0.0198427000
_diffrn_orient_matrix_UB_22      -0.0052877000
_diffrn_orient_matrix_UB_23      -0.0762525000
_diffrn_orient_matrix_UB_31      -0.0111771000
_diffrn_orient_matrix_UB_32      -0.0697865000
_diffrn_orient_matrix_UB_33      0.0045201000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0680
_diffrn_reflns_av_unetI/netI     0.0389
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            64845
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         69.344
_diffrn_reflns_theta_min         3.027
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.459
_exptl_absorpt_correction_T_max  0.51754
_exptl_absorpt_correction_T_min  0.47851
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.93a (Rigaku Oxford Diffraction, 2023)
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_description       plate
_exptl_crystal_F_000             2068
_exptl_crystal_size_max          0.146
_exptl_crystal_size_mid          0.073
_exptl_crystal_size_min          0.045
_exptl_crystal_size_rad          0.400
_refine_diff_density_max         0.398
_refine_diff_density_min         -0.638
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     583
_refine_ls_number_reflns         8257
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0454
_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^)+(0.0447P)^2^+6.4019P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1057
_refine_ls_wR_factor_ref         0.1194
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7056
_reflns_number_total             8257
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc03435c2.cif
_cod_data_source_block           cp199
_cod_database_code               7134944
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         C42H45CoF6N7NiO9S2
_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:
 C24(H24A,H24B), C11(H11A,H11B), C25(H25A,H25B), C12(H12A,H12B), C31(H31A,
 H31B), C18(H18A,H18B)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C17(H17), C3(H3), C14(H14), C16(H16), C15(H15), C27(H27), C36(H36),
 C33(H33), C30(H30), C23(H23), C20(H20), C35(H35), C29(H29), C22(H22), C34(H34),
  C28(H28), C21(H21)
2.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C38(H38A,H38B,H38C),
 C40(H40A,H40B,H40C), C43(H43A,H43B,H43C)
;
_shelx_res_checksum              26394
_shelx_hkl_checksum              44930
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 2.023
_oxdiff_exptl_absorpt_empirical_full_min 0.589