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_7719101
_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 H31 N4 P'
_chemical_formula_sum            'C23 H31 N4 P'
_chemical_formula_weight         394.49
_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                70.890(3)
_cell_angle_beta                 84.826(3)
_cell_angle_gamma                84.255(2)
_cell_formula_units_Z            4
_cell_length_a                   8.3272(3)
_cell_length_b                   14.4208(4)
_cell_length_c                   19.5888(6)
_cell_measurement_reflns_used    7918
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      75.9250
_cell_measurement_theta_min      3.2400
_cell_volume                     2207.40(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 0.996
_diffrn_measured_fraction_theta_max 0.955
_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    -81.00 -55.00   0.50    3.00    --  -46.45-160.00  23.00   52
  2  \w   -110.00 -52.00   0.50    3.00    --  -46.45 160.00  54.00  116
  3  \w    -77.00 -10.00   0.50    3.00    --  -46.45 118.00 -98.00  134
  4  \w     71.00  96.00   0.50    3.00    --   46.45 160.00  54.00   50
  5  \w     74.00 100.00   0.50    3.00    --   46.45-160.00  23.00   52
  6  \w     43.00  88.00   0.50    3.00    --   46.45-118.00 175.00   90
  7  \w     64.00 110.00   0.50   12.00    --  107.75-118.00 175.00   92
  8  \w    115.00 141.00   0.50   12.00    --  107.75 118.00 -98.00   52
  9  \w     89.00 134.00   0.50   12.00    --  107.75-160.00  23.00   90
 10  \w     71.00 109.00   0.50   12.00    --  107.75 160.00  54.00   76
 11  \w     -7.00  20.00   0.50    3.00    --  -46.45  19.00-120.00   54
 12  \w     -7.00  29.00   0.50    3.00    --  -46.45  19.00-150.00   72
 13  \w     -6.00  28.00   0.50    3.00    --  -46.45  19.00  90.00   68
 14  \w     -7.00  30.00   0.50    3.00    --  -46.45  19.00-180.00   74
 15  \w      2.00  27.00   0.50    3.00    --  -46.45  19.00  30.00   50
 16  \w     -7.00  30.00   0.50    3.00    --  -46.45  19.00 -60.00   74
 17  \w     -6.00  30.00   0.50    3.00    --  -46.45  19.00   0.00   72
 18  \w     -7.00  28.00   0.50    3.00    --  -46.45  19.00 -90.00   70
 19  \w     -7.00  30.00   0.50    3.00    --  -46.45  19.00  60.00   74
 20  \w     -7.00  28.00   0.50    3.00    --  -46.45  19.00 150.00   70
 21  \w     42.00  73.00   0.50   12.00    --  107.75 -45.00  30.00   62
 22  \w     38.00  73.00   0.50   12.00    --  107.75 -45.00 -60.00   70
 23  \w     35.00  70.00   0.50   12.00    --  107.75 -45.00-150.00   70
 24  \w     94.00 155.00   0.50   12.00    --  107.75 125.00 -90.00  122
 25  \w     95.00 128.00   0.50   12.00    --  107.75 125.00-150.00   66
 26  \w     36.00  67.00   0.50   12.00    --  107.75 -45.00 120.00   62
 27  \w     62.00  93.00   0.50   12.00    --  107.75 -61.00   0.00   62
 28  \w     33.00  59.00   0.50   12.00    --  107.75 -30.00  60.00   52
 29  \w     44.00  72.00   0.50   12.00    --  107.75 -45.00-120.00   56
 30  \w    135.00 161.00   0.50   12.00    --  107.75  45.00 150.00   52
 31  \w     40.00  72.00   0.50   12.00    --  107.75 -45.00  60.00   64
 32  \w     39.00  69.00   0.50   12.00    --  107.75 -45.00-180.00   60
 33  \w     95.00 120.00   0.50   12.00    --  107.75  45.00 150.00   50
 34  \w    151.00 177.00   0.50   12.00    --  107.75 125.00-150.00   52
 35  \w     51.00 108.00   0.50   12.00    --  107.75-125.00   0.00  114
 36  \w    102.00 176.00   0.50   12.00    --  107.75  45.00-150.00  148
 37  \w     34.00  59.00   0.50   12.00    --  107.75 -30.00 -90.00   50
 38  \w     81.00 106.00   0.50   12.00    --  107.75 -95.00  30.00   50
 39  \w     42.00  68.00   0.50   12.00    --  107.75-125.00-120.00   52
 40  \w    117.00 178.00   0.50   12.00    --  107.75 125.00 150.00  122
 41  \w     35.00  64.00   0.50   12.00    --  107.75 -95.00  30.00   58
 42  \w     32.00  59.00   0.50   12.00    --  107.75 -30.00-120.00   54
 43  \w     74.00 112.00   0.50   12.00    --  107.75-125.00-120.00   76
 44  \w     34.00  59.00   0.50   12.00    --  107.75 -30.00-150.00   50
 45  \w     33.00  58.00   0.50   12.00    --  107.75 -30.00 -60.00   50
 46  \w     80.00 107.00   0.50   12.00    --  107.75-100.00 166.61   54
 47  \w     81.00 106.00   0.50   12.00    --  107.75 -95.00 -30.00   50
 48  \w     39.00 108.00   0.50   12.00    --  107.75-104.00-122.97  138
 49  \w     97.00 176.00   0.50   12.00    --  107.75  61.00-180.00  158
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0511015000
_diffrn_orient_matrix_UB_12      -0.0271075000
_diffrn_orient_matrix_UB_13      -0.0643104000
_diffrn_orient_matrix_UB_21      0.0427508000
_diffrn_orient_matrix_UB_22      0.1017360000
_diffrn_orient_matrix_UB_23      -0.0517954000
_diffrn_orient_matrix_UB_31      0.1739622000
_diffrn_orient_matrix_UB_32      -0.0420692000
_diffrn_orient_matrix_UB_33      -0.0116157000
_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  0.0781
_diffrn_reflns_av_unetI/netI     0.0773
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            25249
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.043
_diffrn_reflns_theta_min         3.253
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.207
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74432
_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 yellow'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.187
_exptl_crystal_description       plate
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.526
_exptl_crystal_size_mid          0.215
_exptl_crystal_size_min          0.054
_refine_diff_density_max         0.637
_refine_diff_density_min         -0.425
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     519
_refine_ls_number_reflns         9021
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0939
_refine_ls_R_factor_gt           0.0724
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1314P)^2^+0.2484P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1895
_refine_ls_wR_factor_ref         0.2057
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6818
_reflns_number_total             9021
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01568e2.cif
_cod_data_source_block           pnnnnligand
_cod_depositor_comments
'Adding full bibliography for 7719100--7719106.cif.'
_cod_database_code               7719101
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         RuNiCl5C50H50N5P5
_chemical_oxdiff_usercomment     'From DCM/HEX'
_shelx_estimated_absorpt_t_max   0.938
_shelx_estimated_absorpt_t_min   0.569
_olex2_refinement_description
;
1.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C38(H38A,H38B)
1.b Aromatic/amide H refined with riding coordinates:
 N2(H2), N6(H6), C34(H34), C31(H31), C35(H35), C13(H13), C26(H26), C5(H5),
 C8(H8), C28(H28), C11(H11), C4(H4), C3(H3), C12(H12), C36(H36), C27(H27)
1.c Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C1(H1A,H1B,H1C), C22(H22A,H22B,H22C), C41(H41A,H41B,
 H41C), C17(H17A,H17B,H17C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C46(H46A,
 H46B,H46C), C23(H23A,H23B,H23C), C18(H18A,H18B,H18C), C42(H42A,H42B,H42C),
 C21(H21A,H21B,H21C), C40(H40A,H40B,H40C), C19(H19A,H19B,H19C)
;
_shelx_res_checksum              2535
_shelx_hkl_checksum              14061
_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 3.352
_oxdiff_exptl_absorpt_empirical_full_min 0.324