Nickel-ruthenium heterobimetallic complexes of a dinucleating unsymmetrical pincer ligand.
Ngwenya, Vuyelwa; Stevens, Michael A.; Gardiner, Michael G.; Colebatch, Annie L.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 11935–11942; doi:10.1039/d5dt01568e

data_7719102
_publ_section_title
;
 Nickel-ruthenium heterobimetallic complexes of a dinucleating
 unsymmetrical pincer ligand.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11935
_journal_page_last               11942
_journal_paper_doi               10.1039/d5dt01568e
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C23 H30 Cl3 Fe N4 Ni P'
_chemical_formula_sum            'C23 H30 Cl3 Fe N4 Ni P'
_chemical_formula_weight         614.39
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-03-27
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2025-04-17 deposited with the CCDC.	2025-07-15 downloaded from the CCDC.
;
_cell_angle_alpha                82.628(2)
_cell_angle_beta                 79.561(2)
_cell_angle_gamma                89.335(2)
_cell_formula_units_Z            4
_cell_length_a                   8.1249(2)
_cell_length_b                   16.7989(5)
_cell_length_c                   19.9915(6)
_cell_measurement_reflns_used    16716
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      77.5280
_cell_measurement_theta_min      2.2920
_cell_volume                     2661.09(13)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.962
_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    4.00    --  -46.57  56.00 -62.00  138
  2  \w    -24.00  56.00   0.50    4.00    --   46.57 -56.00 155.00  160
  3  \w     45.00 116.00   0.50    4.00    --   46.57  56.00 -62.00  142
  4  \w     96.00 133.00   0.50   15.00    --  107.75  56.00 -62.00   74
  5  \w    140.00 166.00   0.50   15.00    --  107.75  56.00 -62.00   52
  6  \w     36.00  62.00   0.50   15.00    --  107.75 -56.00 155.00   52
  7  \w     -7.00  24.00   0.50    4.00    --  -46.57  19.00-150.00   62
  8  \w     -1.00  25.00   0.50    4.00    --  -46.57  19.00-120.00   52
  9  \w   -117.00 -42.00   0.50    4.00    --  -46.57 -56.00 155.00  150
 10  \w      0.00  29.00   0.50    4.00    --  -46.57  19.00  60.00   58
 11  \w     -4.00  22.00   0.50    4.00    --  -46.57  19.00  90.00   52
 12  \w     -1.00  76.00   0.50    4.00    --   46.57 -99.00  60.00  154
 13  \w     33.00  93.00   0.50    4.00    --   46.57-125.00  30.00  120
 14  \w     33.00  58.00   0.50   15.00    --  107.75 -30.00 -60.00   50
 15  \w     37.00 110.00   0.50   15.00    --  107.75-125.00 150.00  146
 16  \w     40.00  72.00   0.50   15.00    --  107.75 -45.00  30.00   64
 17  \w     32.00  57.00   0.50   15.00    --  107.75 -30.00-120.00   50
 18  \w    105.00 174.00   0.50   15.00    --  107.75  30.00  30.00  138
 19  \w     34.00  63.00   0.50   15.00    --  107.75 -77.00 -90.00   58
 20  \w     67.00  93.00   0.50   15.00    --  107.75 -77.00 -90.00   52
 21  \w     71.00 109.00   0.50   15.00    --  107.75-125.00-120.00   76
 22  \w     33.00  59.00   0.50   15.00    --  107.75 -30.00 150.00   52
 23  \w     32.00  57.00   0.50   15.00    --  107.75 -30.00   0.00   50
 24  \w     34.00  60.00   0.50   15.00    --  107.75 -61.00  30.00   52
 25  \w     65.00  91.00   0.50   15.00    --  107.75 -61.00  30.00   52
 26  \w     33.00  59.00   0.50   15.00    --  107.75 -30.00 120.00   52
 27  \w     35.00  72.00   0.50   15.00    --  107.75 -45.00 -60.00   74
 28  \w     33.00  58.00   0.50   15.00    --  107.75 -30.00  30.00   50
 29  \w     64.00 102.00   0.50   15.00    --  107.75 -95.00   0.00   76
 30  \w     38.00  68.00   0.50   15.00    --  107.75 -45.00-180.00   60
 31  \w     32.00  57.00   0.50   15.00    --  107.75 -30.00 -90.00   50
 32  \w     95.00 121.00   0.50   15.00    --  107.75  45.00 150.00   52
 33  \w    148.00 177.00   0.50   15.00    --  107.75  45.00 150.00   58
 34  \w    106.00 132.00   0.50   15.00    --  107.75  30.00-120.00   52
 35  \w    143.00 177.00   0.50   15.00    --  107.75  30.00-120.00   68
 36  \w     94.00 168.00   0.50   15.00    --  107.75  45.00 120.00  148
 37  \w     63.00 106.00   0.50   15.00    --  107.75 -95.00-150.00   86
 38  \w     80.00 106.00   0.50   15.00    --  107.75 -95.00  30.00   52
 39  \w     34.00  59.00   0.50   15.00    --  107.75 -30.00-180.00   50
 40  \w     39.00  73.00   0.50   15.00    --  107.75 -45.00-150.00   68
 41  \w     38.00 105.00   0.50   15.00    --  107.75 -95.00 -90.00  134
 42  \w     35.00  60.00   0.50   15.00    --  107.75 -45.00  60.00   50
 43  \w     40.00  67.00   0.50   15.00    --  107.75 -45.00 150.00   54
 44  \w     40.00  70.00   0.50   15.00    --  107.75 -45.00 120.00   60
 45  \w     98.00 129.00   0.50   15.00    --  107.75-148.00  68.71   62
 46  \w     60.00 106.00   0.50   15.00    --  107.75 -95.00 120.00   92
 47  \w     49.00  93.00   0.50   15.00    --  107.75 -61.00 -30.00   88
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1330440000
_diffrn_orient_matrix_UB_12      -0.0629355000
_diffrn_orient_matrix_UB_13      0.0372337000
_diffrn_orient_matrix_UB_21      -0.0095241000
_diffrn_orient_matrix_UB_22      0.0381472000
_diffrn_orient_matrix_UB_23      0.0666626000
_diffrn_orient_matrix_UB_31      -0.1392331000
_diffrn_orient_matrix_UB_32      0.0559993000
_diffrn_orient_matrix_UB_33      -0.0203110000
_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  0.0470
_diffrn_reflns_av_unetI/netI     0.0443
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            32624
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.289
_diffrn_reflns_theta_min         2.266
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.739
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43518
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic dark red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.534
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1264
_exptl_crystal_recrystallization_method MeCN/Ether
_exptl_crystal_size_max          0.183
_exptl_crystal_size_mid          0.096
_exptl_crystal_size_min          0.045
_refine_diff_density_max         0.939
_refine_diff_density_min         -0.635
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.143
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     609
_refine_ls_number_reflns         11004
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.143
_refine_ls_R_factor_all          0.0675
_refine_ls_R_factor_gt           0.0594
_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^)+(0.0561P)^2^+9.6358P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1599
_refine_ls_wR_factor_ref         0.1636
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9738
_reflns_number_total             11004
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01568e2.cif
_cod_data_source_block           nife
_cod_depositor_comments
'Adding full bibliography for 7719100--7719106.cif.'
_cod_database_code               7719102
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         NiFeC50H50N8O2P2
_chemical_oxdiff_usercomment     'From MeCn/Ether'
_olex2_refinement_description
;
1.a Secondary CH2 refined with riding coordinates:
 C38(H38A,H38B), C15(H15A,H15B)
1.b Aromatic/amide H refined with riding coordinates:
 C28(H28), C26(H26), C31(H31), C36(H36), C34(H34), C4(H4), C35(H35), C27(H27),
 C3(H3), C11(H11), C5(H5), C8(H8), C13(H13), C12(H12)
1.c Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C22(H22A,H22B,H22C), C17(H17A,H17B,H17C), C19(H19A,H19B,
 H19C), C21(H21A,H21B,H21C), C1(H1A,H1B,H1C), C46(H46A,H46B,H46C), C23(H23A,
 H23B,H23C), C45(H45A,H45B,H45C), C18(H18A,H18B,H18C), C44(H44A,H44B,H44C),
 C40(H40A,H40B,H40C), C42(H42A,H42B,H42C), C41(H41A,H41B,H41C)
;
_shelx_res_checksum              82045
_shelx_hkl_checksum              82130
_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 1.986
_oxdiff_exptl_absorpt_empirical_full_min 0.558