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_7719105
_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         'C59 H60 Cl2 N4 Ni P3 Ru, C H2 Cl2'
_chemical_formula_sum            'C60 H62 Cl4 N4 Ni P3 Ru'
_chemical_formula_weight         1233.62
_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   geom
_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                90
_cell_angle_beta                 110.145(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.1699(2)
_cell_length_b                   36.2536(3)
_cell_length_c                   15.8549(2)
_cell_measurement_reflns_used    15183
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      75.7630
_cell_measurement_theta_min      3.2010
_cell_volume                     6567.28(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 0.999
_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   -121.00 -33.00   0.50   20.00    --  -46.45 -33.00 176.00  176
  2  \w    -10.00  27.00   0.50   20.00    --  -46.45  33.00 -25.00   74
  3  \w      6.00  32.00   0.50   20.00    --   46.45 -33.00 176.00   52
  4  \w     66.00  92.00   0.50   20.00    --   46.45  33.00 -25.00   52
  5  \w     33.00  59.00   0.50   70.00    --  107.75 -33.00 176.00   52
  6  \w    103.00 169.00   0.50   70.00    --  107.75  33.00 -25.00  132
  7  \w     -8.00  26.00   0.50   20.00    --  -46.45  19.00 120.00   68
  8  \w    -84.00 -22.00   0.50   20.00    --  -46.45 125.00 -30.00  124
  9  \w     34.00  74.00   0.50   20.00    --   46.45-125.00  30.00   80
 10  \w     33.00  59.00   0.50   70.00    --  107.75 -30.00   0.00   52
 11  \w     32.00  59.00   0.50   70.00    --  107.75 -30.00-120.00   54
 12  \w     33.00  59.00   0.50   70.00    --  107.75 -30.00 150.00   52
 13  \w     41.00 102.00   0.50   70.00    --  107.75 -95.00   0.00  122
 14  \w     35.00  67.00   0.50   70.00    --  107.75 -45.00   0.00   64
 15  \w     40.00  68.00   0.50   70.00    --  107.75 -45.00-150.00   56
 16  \w     32.00  57.00   0.50   70.00    --  107.75 -30.00  90.00   50
 17  \w    102.00 144.00   0.50   70.00    --  107.75 125.00-150.00   84
 18  \w     32.00  58.00   0.50   70.00    --  107.75 -30.00 -30.00   52
 19  \w     36.00  69.00   0.50   70.00    --  107.75 -45.00 -60.00   66
 20  \w     42.00  72.00   0.50   70.00    --  107.75 -45.00-180.00   60
 21  \w     32.00  58.00   0.50   70.00    --  107.75 -30.00  30.00   52
 22  \w     34.00  59.00   0.50   70.00    --  107.75 -30.00  60.00   50
 23  \w     35.00  60.00   0.50   70.00    --  107.75 -45.00-120.00   50
 24  \w     72.00 105.00   0.50   70.00    --  107.75 -95.00  30.00   66
 25  \w     39.00  72.00   0.50   70.00    --  107.75 -45.00 -90.00   66
 26  \w     36.00  63.00   0.50   70.00    --  107.75 -45.00 -30.00   54
 27  \w     40.00  69.00   0.50   70.00    --  107.75 -45.00  30.00   58
;
_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  0.0445
_diffrn_reflns_av_unetI/netI     0.0454
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            43899
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.119
_diffrn_reflns_theta_min         3.210
_exptl_absorpt_coefficient_mu    4.689
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86933
_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    1.248
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2540
_exptl_crystal_size_max          0.092
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.023
_refine_diff_density_max         1.274
_refine_diff_density_min         -1.442
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     665
_refine_ls_number_reflns         13553
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0641
_refine_ls_R_factor_gt           0.0532
_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^)+(0.0728P)^2^+8.2976P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1350
_refine_ls_wR_factor_ref         0.1409
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11258
_reflns_number_total             13553
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01568e2.cif
_cod_data_source_block           niclru
_cod_depositor_comments
'Adding full bibliography for 7719100--7719106.cif.'
_cod_database_code               7719105
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.900
_shelx_estimated_absorpt_t_min   0.672
_olex2_refinement_description
;
1.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C60(H60A,H60B)
1.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C57(H57), C55(H55), C43(H43), C56(H56), C31(H31), C47(H47), C34(H34),
 C5(H5), C32(H32), C35(H35), C45(H45), C49(H49), C33(H33), C59(H59), C41(H41),
 C37(H37), C50(H50), C25(H25), C53(H53), C11(H11), C51(H51), C58(H58), C3(H3),
 C38(H38), C44(H44), C29(H29), C40(H40), C46(H46), C39(H39), C12(H12), C4(H4),
 C27(H27), C26(H26), C13(H13), C52(H52), C28(H28)
1.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C18(H18A,H18B,H18C), C17(H17A,H17B,H17C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C19(H19A,H19B,H19C), C21(H21A,H21B,H21C)
;
_shelx_res_checksum              47039
_shelx_hkl_checksum              17549
_shelx_fab_checksum              36212
_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
;