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_7719104
_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 H61 Cl N4 Ni O P3 Ru, Cl, 5(C H Cl3)'
_chemical_formula_sum            'C65 H66 Cl17 N4 Ni O P3 Ru'
_chemical_formula_weight         1774.55
_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
_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                83.112(2)
_cell_angle_beta                 85.950(2)
_cell_angle_gamma                70.585(2)
_cell_formula_units_Z            2
_cell_length_a                   11.6620(3)
_cell_length_b                   15.6659(4)
_cell_length_c                   22.5432(5)
_cell_measurement_reflns_used    23072
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      76.9720
_cell_measurement_theta_min      3.4080
_cell_volume                     3854.23(17)
_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_temperature      150.00(10)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.961
_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   -112.00 -87.00   0.50    2.00    --  -46.57-150.00-167.00   50
  2  \w    -85.00 -15.00   0.50    2.00    --  -46.57 123.00  75.00  140
  3  \w   -103.00 -29.00   0.50    2.00    --  -46.57 150.00-122.00  148
  4  \w     67.00 110.00   0.50    2.00    --   46.57-150.00-167.00   86
  5  \w     62.00  87.00   0.50    2.00    --   46.57-123.00  -5.00   50
  6  \w     68.00 110.00   0.50    7.00    --  106.49-123.00  -5.00   84
  7  \w     79.00 113.00   0.50    7.00    --  106.49 150.00-122.00   68
  8  \w    108.00 135.00   0.50    7.00    --  106.49 123.00  75.00   54
  9  \w     80.00 128.00   0.50    7.00    --  106.49-150.00-167.00   96
 10  \w    -21.00  19.00   0.50    2.00    --  -46.57  38.00 -30.00   80
 11  \w     -7.00  30.00   0.50    2.00    --  -46.57  19.00-120.00   74
 12  \w     -7.00  28.00   0.50    2.00    --  -46.57  19.00-180.00   70
 13  \w    -21.00  27.00   0.50    2.00    --  -46.57  38.00 -60.00   96
 14  \w     -1.00  24.00   0.50    2.00    --  -46.57  19.00  90.00   50
 15  \w   -119.00 -23.00   0.50    2.00    --  -46.57 -77.00-180.00  192
 16  \w     -7.00  29.00   0.50    2.00    --  -46.57  19.00-150.00   72
 17  \w     -7.00  29.00   0.50    2.00    --  -46.57  19.00 -90.00   72
 18  \w     51.00  77.00   0.50    2.00    --   46.57  77.00 -60.00   52
 19  \w     44.00  71.00   0.50    7.00    --  106.49 -45.00   0.00   54
 20  \w     33.00  71.00   0.50    7.00    --  106.49 -61.00 -30.00   76
 21  \w     39.00  73.00   0.50    7.00    --  106.49 -45.00  60.00   68
 22  \w     43.00 110.00   0.50    7.00    --  106.49-125.00 -30.00  134
 23  \w     39.00  72.00   0.50    7.00    --  106.49 -45.00 120.00   66
 24  \w     33.00  58.00   0.50    7.00    --  106.49 -30.00  90.00   50
 25  \w     32.00  58.00   0.50    7.00    --  106.49 -30.00  30.00   52
 26  \w     34.00  60.00   0.50    7.00    --  106.49 -95.00-150.00   52
 27  \w     63.00 106.00   0.50    7.00    --  106.49 -95.00  60.00   86
 28  \w     31.00  59.00   0.50    7.00    --  106.49 -30.00-120.00   56
 29  \w     31.00  58.00   0.50    7.00    --  106.49 -30.00 120.00   54
 30  \w     96.00 155.00   0.50    7.00    --  106.49 125.00  60.00  118
 31  \w     32.00  59.00   0.50    7.00    --  106.49 -30.00 -90.00   54
 32  \w     89.00 119.00   0.50    7.00    --  106.49  61.00 -30.00   60
 33  \w    134.00 160.00   0.50    7.00    --  106.49  61.00 -30.00   52
 34  \w    110.00 176.00   0.50    7.00    --  106.49  30.00-120.00  132
 35  \w     45.00 107.00   0.50    7.00    --  106.49-102.00-127.88  124
 36  \w     36.00  61.00   0.50    7.00    --  106.49 -45.00  30.00   50
 37  \w     42.00  67.00   0.50    7.00    --  106.49 -45.00-150.00   50
 38  \w     42.00  93.00   0.50    7.00    --  106.49 -61.00   0.00  102
 39  \w     36.00  61.00   0.50    7.00    --  106.49 -95.00 120.00   50
 40  \w     97.00 134.00   0.50    7.00    --  106.49 125.00 -90.00   74
 41  \w     40.00  65.00   0.50    7.00    --  106.49 -45.00 -60.00   50
 42  \w     81.00 106.00   0.50    7.00    --  106.49 -95.00 120.00   50
 43  \w     55.00  98.00   0.50    7.00    --  106.49 -95.00-180.00   86
 44  \w     31.00  59.00   0.50    7.00    --  106.49 -30.00 -30.00   56
 45  \w     80.00 106.00   0.50    7.00    --  106.49 -95.00 -30.00   52
 46  \w     34.00  92.00   0.50    7.00    --  106.49 -61.00-180.00  116
 47  \w     98.00 177.00   0.50    7.00    --  106.49  15.00-150.00  158
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0526
_diffrn_reflns_av_unetI/netI     0.0506
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            48559
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.590
_diffrn_reflns_theta_min         3.007
_exptl_absorpt_coefficient_mu    8.244
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50077
_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 orangish orange'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_description       plate
_exptl_crystal_F_000             1796
_exptl_crystal_size_max          0.238
_exptl_crystal_size_mid          0.142
_exptl_crystal_size_min          0.114
_refine_diff_density_max         0.993
_refine_diff_density_min         -0.961
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     840
_refine_ls_number_reflns         15782
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0587
_refine_ls_R_factor_gt           0.0482
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0541P)^2^+6.5870P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1206
_refine_ls_wR_factor_ref         0.1261
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13193
_reflns_number_total             15782
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01568e2.cif
_cod_data_source_block           niruh
_cod_depositor_comments
'Adding full bibliography for 7719100--7719106.cif.'
_cod_database_code               7719104
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.453
_shelx_estimated_absorpt_t_min   0.244
_olex2_refinement_description
;
1.a Ternary CH refined with riding coordinates:
 C02G(H02G), C02H(H02H), C02I(H02I), C02J(H02J), C02K(H02K)
1.b Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B)
1.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C26(H26), C42(H42), C6(H6), C51(H51), C27(H27), C36(H36), C61(H61),
 C48(H48), C28(H28), C44(H44), C37(H37), C57(H57), C40(H40), C39(H39), C30(H30),
  C55(H55), C47(H47), C32(H32), C38(H38), C14(H14), C29(H29), C46(H46),
 C45(H45), C52(H52), C60(H60), C5(H5), C12(H12), C33(H33), C4(H4), C53(H53),
 C59(H59), C54(H54), C13(H13), C58(H58), C34(H34), C35(H35)
1.d Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C23(H23A,H23B,
 H23C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C19(H19A,H19B,H19C)
;
_shelx_res_checksum              15291
_shelx_hkl_checksum              90778
_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
;