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_7719106
_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         '2(C59 H61 Cl2 N4 P3 Ru), 2(C H2 Cl2)'
_chemical_formula_sum            'C120 H126 Cl8 N8 P6 Ru2'
_chemical_formula_weight         2351.84
_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             2025-04-07
_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                90
_cell_angle_beta                 91.4455(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.61625(15)
_cell_length_b                   10.04885(6)
_cell_length_c                   46.1456(3)
_cell_measurement_reflns_used    36757
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      77.8580
_cell_measurement_theta_min      3.2970
_cell_volume                     11411.17(12)
_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 0.996
_diffrn_measured_fraction_theta_max 0.963
_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    -40.00  27.00   0.50    3.00    --  -46.45  55.00 122.00  134
  2  \w    -74.00 -46.00   0.50    3.00    --  -46.45 -55.00 -20.00   56
  3  \w   -118.00 -83.00   0.50    3.00    --  -46.45 -55.00 -20.00   70
  4  \w     21.00  58.00   0.50    3.00    --   46.45 -55.00 -20.00   74
  5  \w     35.00  64.00   0.50    9.00    --  107.75 -55.00 -20.00   58
  6  \w     99.00 177.00   0.50    9.00    --  107.75  55.00 122.00  156
  7  \w    -21.00  27.00   0.50    3.00    --  -46.45  38.00-120.00   96
  8  \w     -8.00  17.00   0.50    3.00    --  -46.45  19.00 120.00   50
  9  \w    -21.00  17.00   0.50    3.00    --  -46.45  38.00 -90.00   76
 10  \w     -8.00  30.00   0.50    3.00    --  -46.45  19.00  30.00   76
 11  \w     -5.00  21.00   0.50    3.00    --  -46.45  19.00 -90.00   52
 12  \w     51.00  76.00   0.50    3.00    --   46.45  55.00 122.00   50
 13  \w     32.00  58.00   0.50    9.00    --  107.75 -30.00 150.00   52
 14  \w     34.00  59.00   0.50    9.00    --  107.75 -30.00  30.00   50
 15  \w     32.00  57.00   0.50    9.00    --  107.75 -30.00-180.00   50
 16  \w     33.00  58.00   0.50    9.00    --  107.75 -30.00 -30.00   50
 17  \w     37.00  63.00   0.50    9.00    --  107.75 -45.00-180.00   52
 18  \w     36.00  67.00   0.50    9.00    --  107.75 -45.00  30.00   62
 19  \w     43.00  68.00   0.50    9.00    --  107.75-125.00   0.00   50
 20  \w     80.00 106.00   0.50    9.00    --  107.75-125.00   0.00   52
 21  \w     59.00  92.00   0.50    9.00    --  107.75 -61.00  90.00   66
 22  \w     33.00  58.00   0.50    9.00    --  107.75 -30.00 120.00   50
 23  \w    151.00 177.00   0.50    9.00    --  107.75  30.00  90.00   52
 24  \w    104.00 145.00   0.50    9.00    --  107.75  30.00  90.00   82
 25  \w     41.00  68.00   0.50    9.00    --  107.75 -45.00  60.00   54
 26  \w     36.00  69.00   0.50    9.00    --  107.75 -45.00-150.00   66
 27  \w     35.00  64.00   0.50    9.00    --  107.75 -45.00   0.00   58
 28  \w     32.00  59.00   0.50    9.00    --  107.75 -30.00   0.00   54
 29  \w     33.00  58.00   0.50    9.00    --  107.75 -30.00 -90.00   50
 30  \w     33.00  58.00   0.50    9.00    --  107.75 -30.00  60.00   50
 31  \w     32.00  58.00   0.50    9.00    --  107.75 -30.00-150.00   52
 32  \w     44.00  72.00   0.50    9.00    --  107.75 -45.00 -60.00   56
 33  \w     35.00  60.00   0.50    9.00    --  107.75 -45.00 150.00   50
;
_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      0.0461821000
_diffrn_orient_matrix_UB_12      0.0634705000
_diffrn_orient_matrix_UB_13      0.0184509000
_diffrn_orient_matrix_UB_21      -0.0421392000
_diffrn_orient_matrix_UB_22      0.0792847000
_diffrn_orient_matrix_UB_23      0.0170761000
_diffrn_orient_matrix_UB_31      -0.0036673000
_diffrn_orient_matrix_UB_32      -0.1147546000
_diffrn_orient_matrix_UB_33      0.0219858000
_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  0.0379
_diffrn_reflns_av_unetI/netI     0.0370
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       57
_diffrn_reflns_limit_l_min       -55
_diffrn_reflns_number            78762
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.011
_diffrn_reflns_theta_min         3.350
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.064
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50148
_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    1.369
_exptl_crystal_description       needle
_exptl_crystal_F_000             4864
_exptl_crystal_size_max          0.317
_exptl_crystal_size_mid          0.091
_exptl_crystal_size_min          0.071
_refine_diff_density_max         0.852
_refine_diff_density_min         -1.618
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1315
_refine_ls_number_reflns         23526
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0543
_refine_ls_R_factor_gt           0.0464
_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^)+(0.0711P)^2^+15.2230P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1279
_refine_ls_wR_factor_ref         0.1340
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19953
_reflns_number_total             23526
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01568e2.cif
_cod_data_source_block           vn63
_cod_depositor_comments
'Adding full bibliography for 7719100--7719106.cif.'
_cod_original_cell_volume        11411.16(12)
_cod_database_code               7719106
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C59 H61 Cl2 N4 P3 Ru'
_chemical_oxdiff_usercomment     ????
_shelx_estimated_absorpt_t_max   0.715
_shelx_estimated_absorpt_t_min   0.297
_olex2_refinement_description
;
1.a Secondary CH2 refined with riding coordinates:
 C74(H74A,H74B), C15(H15A,H15B), C120(H12A,H12B), C119(H11A,H11B)
1.b Aromatic/amide H refined with riding coordinates:
 N3(H3), C64(H64), C62(H62), C3(H3A), C53(H53), C5(H5), C31(H31), C118(H118),
 C67(H67), C115(H115), C59(H59), C8(H8), C116(H116), C4(H4), C108(H108),
 C63(H63), C32(H32), C112(H112), C42(H42), C90(H90), C46(H46), C106(H106),
 C51(H51), C114(H114), C117(H117), C110(H110), C37(H37), C102(H102), C25(H25),
 C109(H109), C52(H52), C35(H35), C72(H72), C43(H43), C55(H55), C49(H49),
 C33(H33), C50(H50), C96(H96), C38(H38), C70(H70), C111(H111), C29(H29),
 C94(H94), C71(H71), C103(H103), C39(H39), C34(H34), C11(H11), C58(H58),
 C41(H41), C44(H44), C92(H92), C105(H105), C13(H13), C28(H28), C93(H93),
 C100(H100), C45(H45), C84(H84), C104(H104), C12(H12), C97(H97), C88(H88),
 C26(H26), C27(H27), C40(H40), C91(H91), C56(H56), C85(H85), C57(H57), C87(H87),
  C86(H86), C98(H98), C99(H99)
1.c Idealised Me refined as rotating group:
 C60(H60A,H60B,H60C), C1(H1A,H1B,H1C), C78(H78A,H78B,H78C), C76(H76A,H76B,
 H76C), C77(H77A,H77B,H77C), C19(H19A,H19B,H19C), C17(H17A,H17B,H17C), C18(H18A,
 H18B,H18C), C20(H20A,H20B,H20C), C23(H23A,H23B,H23C), C22(H22A,H22B,H22C),
 C82(H82A,H82B,H82C), C81(H81A,H81B,H81C), C80(H80A,H80B,H80C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              54089
_shelx_hkl_checksum              33933
_shelx_fab_checksum              18634
_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 2.245
_oxdiff_exptl_absorpt_empirical_full_min 0.590