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_7719103
_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         'C60 H62 N4 O P3 Ru, Cl'
_chemical_formula_sum            'C60 H62 Cl N4 O P3 Ru'
_chemical_formula_weight         1084.56
_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   mixed
_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                71.9050(10)
_cell_angle_beta                 84.4030(10)
_cell_angle_gamma                76.9080(10)
_cell_formula_units_Z            2
_cell_length_a                   10.6692(2)
_cell_length_b                   16.4671(3)
_cell_length_c                   18.7338(3)
_cell_measurement_reflns_used    22222
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      77.6920
_cell_measurement_theta_min      4.2500
_cell_volume                     3045.94(10)
_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 0.999
_diffrn_measured_fraction_theta_max 0.964
_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    -89.00 -32.00   0.50    2.00    --  -46.57 -16.00 -83.00  114
  2  \w   -120.00 -94.00   0.50    2.00    --  -46.57 -16.00 -83.00   52
  3  \w     42.00 108.00   0.50    2.00    --   46.57  16.00  86.00  132
  4  \w    -25.00  51.00   0.50    2.00    --   46.57 -16.00 -83.00  152
  5  \w    118.00 144.00   0.50    6.00    --  107.75  16.00  86.00   52
  6  \w     -7.00  18.00   0.50    2.00    --  -46.57  16.00  86.00   50
  7  \w    -52.00 -14.00   0.50    2.00    --  -46.57 125.00   0.00   76
  8  \w     -7.00  28.00   0.50    2.00    --  -46.57  19.00-120.00   70
  9  \w     -4.00  29.00   0.50    2.00    --  -46.57  19.00 150.00   66
 10  \w     -5.00  27.00   0.50    2.00    --  -46.57  19.00 -60.00   64
 11  \w     -6.00  19.00   0.50    2.00    --  -46.57  19.00   0.00   50
 12  \w      2.00  27.00   0.50    2.00    --  -46.57  19.00 -90.00   50
 13  \w    -87.00 -39.00   0.50    2.00    --  -46.57 125.00-180.00   96
 14  \w     50.00  92.00   0.50    2.00    --   46.57-125.00-150.00   84
 15  \w     59.00  93.00   0.50    2.00    --   46.57-125.00   0.00   68
 16  \w     35.00  72.00   0.50    6.00    --  107.75 -45.00  60.00   74
 17  \w     33.00  59.00   0.50    6.00    --  107.75 -30.00 150.00   52
 18  \w     35.00  73.00   0.50    6.00    --  107.75 -45.00  90.00   76
 19  \w    108.00 173.00   0.50    6.00    --  107.75  30.00   0.00  130
 20  \w     96.00 122.00   0.50    6.00    --  107.75  30.00  90.00   52
 21  \w     36.00  62.00   0.50    6.00    --  107.75 -45.00-150.00   52
 22  \w     35.00  65.00   0.50    6.00    --  107.75 -45.00 -90.00   60
 23  \w     72.00 109.00   0.50    6.00    --  107.75-125.00 -30.00   74
 24  \w     35.00  69.00   0.50    6.00    --  107.75 -95.00-150.00   68
 25  \w     33.00  58.00   0.50    6.00    --  107.75 -30.00-150.00   50
 26  \w     61.00 106.00   0.50    6.00    --  107.75 -95.00 150.00   90
 27  \w     68.00  93.00   0.50    6.00    --  107.75 -61.00 -60.00   50
 28  \w     34.00  59.00   0.50    6.00    --  107.75 -30.00 -30.00   50
 29  \w    137.00 163.00   0.50    6.00    --  107.75  30.00  90.00   52
 30  \w     32.00  59.00   0.50    6.00    --  107.75 -30.00 120.00   54
 31  \w     32.00  57.00   0.50    6.00    --  107.75 -30.00-120.00   50
 32  \w     32.00  58.00   0.50    6.00    --  107.75 -30.00 -90.00   52
 33  \w     94.00 119.00   0.50    6.00    --  107.75  30.00 150.00   50
 34  \w    133.00 175.00   0.50    6.00    --  107.75  30.00 150.00   84
 35  \w     64.00 105.00   0.50    6.00    --  107.75 -95.00 -60.00   82
 36  \w     32.00  57.00   0.50    6.00    --  107.75 -30.00-180.00   50
 37  \w     36.00  61.00   0.50    6.00    --  107.75 -45.00 -60.00   50
 38  \w     37.00  63.00   0.50    6.00    --  107.75 -45.00-120.00   52
 39  \w     67.00  93.00   0.50    6.00    --  107.75 -61.00  60.00   52
 40  \w     36.00 104.00   0.50    6.00    --  107.75 -77.00  30.00  136
 41  \w     39.00  69.00   0.50    6.00    --  107.75 -45.00-180.00   60
 42  \w     34.00  60.00   0.50    6.00    --  107.75 -95.00-180.00   52
 43  \w     67.00  99.00   0.50    6.00    --  107.75 -95.00-180.00   64
 44  \w     32.00  57.00   0.50    6.00    --  107.75 -30.00   0.00   50
 45  \w     66.00 106.00   0.50    6.00    --  107.75 -95.00  60.00   80
 46  \w     33.00  59.00   0.50    6.00    --  107.75 -30.00 -60.00   52
 47  \w     32.00  59.00   0.50    6.00    --  107.75 -30.00  90.00   54
 48  \w     80.00 106.00   0.50    6.00    --  107.75 -95.00-150.00   52
 49  \w     68.00  93.00   0.50    6.00    --  107.75 -95.00 -30.00   50
 50  \w    100.00 152.00   0.50    6.00    --  107.75 125.00-150.00  104
 51  \w     34.00  99.00   0.50    6.00    --  107.75 -95.00  30.00  130
;
_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      -0.1064769000
_diffrn_orient_matrix_UB_12      -0.0534695000
_diffrn_orient_matrix_UB_13      0.0181242000
_diffrn_orient_matrix_UB_21      -0.1014342000
_diffrn_orient_matrix_UB_22      0.0828720000
_diffrn_orient_matrix_UB_23      0.0007309000
_diffrn_orient_matrix_UB_31      -0.0192284000
_diffrn_orient_matrix_UB_32      0.0198874000
_diffrn_orient_matrix_UB_33      -0.0846281000
_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  0.0709
_diffrn_reflns_av_unetI/netI     0.0583
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            37719
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.115
_diffrn_reflns_theta_min         3.198
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.533
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61762
_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 light orange'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_description       plate
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.298
_exptl_crystal_size_mid          0.102
_exptl_crystal_size_min          0.044
_refine_diff_density_max         1.038
_refine_diff_density_min         -1.280
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     642
_refine_ls_number_reflns         12592
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0509
_refine_ls_R_factor_gt           0.0475
_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^)+(0.0710P)^2^+2.2999P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1326
_refine_ls_wR_factor_ref         0.1351
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11390
_reflns_number_total             12592
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01568e2.cif
_cod_data_source_block           ruh(nn)_3
_cod_depositor_comments
'Adding full bibliography for 7719100--7719106.cif.'
_cod_database_code               7719103
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C60 H32 N4 P3 Ru O'
_shelx_estimated_absorpt_t_max   0.860
_shelx_estimated_absorpt_t_min   0.419
_olex2_refinement_description
;
1.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B)
1.b Aromatic/amide H refined with riding coordinates:
 N3(H3), C8(H8), C28(H28), C29(H29), C35(H35), C31(H31), C34(H34), C25(H25),
 C11(H11), C33(H33), C13(H13), C27(H27), C32(H32), C26(H26), C41(H41), C37(H37),
  C5(H5), C3(H3A), C4(H4), C55(H55), C12(H12), C43(H43), C39(H39), C40(H40),
 C59(H59), C38(H38), C58(H58), C49(H49), C56(H56), C47(H47), C44(H44), C45(H45),
  C46(H46), C53(H53), C57(H57), C50(H50), C52(H52), C51(H51)
1.c Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C1(H1A,H1B,H1C), C23(H23A,H23B,H23C), C21(H21A,H21B,
 H21C), C19(H19A,H19B,H19C), C18(H18A,H18B,H18C), C17(H17A,H17B,H17C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              97413
_shelx_hkl_checksum              460
_shelx_fab_checksum              78465
_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 2.544
_oxdiff_exptl_absorpt_empirical_full_min 0.541