Unlocking reactivity: synthetic, structural and catalytic exploration of ruthenium(II) complexes featuring pdc and NHC ligands
Awe, Babatunde; Swart, Glendin; Erasmus, Elizabeth; Landman, Marilé; Malan, Frederick Pieter; New Journal of Chemistry  (2026) –; doi:10.1039/D5NJ03988F

data_7064176
_publ_section_title
;
 Unlocking reactivity: synthetic, structural and catalytic exploration of
 ruthenium(II) complexes featuring pdc and NHC ligands
;
_journal_name_full               'New Journal of Chemistry'
_journal_paper_doi               10.1039/D5NJ03988F
_journal_year                    2026
_chemical_formula_moiety
'4(C32 H29 N5 O8 Ru), 2(C2 H5.10 Cl4.69 O1.10), 4(C H2 Cl2), H2 O'
_chemical_formula_sum            'C136 H136.2 Cl17.37 N20 O35.2 Ru4'
_chemical_formula_weight         3634.17
_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             2025-11-10
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2018.12.18 svn.r3554 for Rigaku Oxford Diffraction, GUI svn.r1)
;
_audit_update_record
;
2025-11-28 deposited with the CCDC.	2025-12-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.040(4)
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   9.9817(5)
_cell_length_b                   14.0691(8)
_cell_length_c                   26.5049(15)
_cell_measurement_reflns_used    7833
_cell_measurement_temperature    149.98(10)
_cell_measurement_theta_max      77.8040
_cell_measurement_theta_min      3.3410
_cell_volume                     3716.9(4)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.98(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.968
_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   2.00   0.50    3.50    --  -46.58 104.00-112.00   84
  2  \w     20.00  82.00   0.50    3.50    --   46.58-104.00 146.00  124
  3  \w   -173.00 -85.00   0.50   10.00    -- -102.00-104.00 146.00  176
  4  \w   -105.00 -70.00   0.50   10.00    -- -102.00 104.00-112.00   70
  5  \w    116.00 143.00   0.50   10.00    --  110.25 104.00-112.00   54
  6  \w     40.00 100.00   0.50   10.00    --  110.25-104.00 146.00  120
  7  \w     -4.00  29.00   0.50    3.50    --  -46.58  19.00 120.00   66
  8  \w     -3.00  26.00   0.50    3.50    --  -46.58  19.00-120.00   58
  9  \w     -5.00  20.00   0.50    3.50    --  -46.58  19.00 -30.00   50
 10  \w     -4.00  28.00   0.50    3.50    --  -46.58  19.00-150.00   64
 11  \w      0.00  27.00   0.50    3.50    --  -46.58  19.00 150.00   54
 12  \w    -29.00  26.00   0.50    3.50    --  -46.58  37.00   0.00  110
 13  \w    -28.00   9.00   0.50    3.50    --   46.58 -19.00 -30.00   74
 14  \w    -72.00 -47.00   0.50   10.00    -- -102.00  61.00  60.00   50
 15  \w   -121.00 -89.00   0.50   10.00    -- -102.00 -15.00  30.00   64
 16  \w   -163.00-135.00   0.50   10.00    -- -102.00 -15.00  30.00   56
 17  \w   -157.00-113.00   0.50   10.00    -- -102.00 -15.00 150.00   88
 18  \w    -72.00 -47.00   0.50   10.00    -- -102.00  61.00  30.00   50
 19  \w   -161.00-103.00   0.50   10.00    -- -102.00 -15.00-150.00  116
 20  \w     41.00  69.00   0.50   10.00    --  110.25-125.00 120.00   56
 21  \w     71.00 108.00   0.50   10.00    --  110.25-125.00-120.00   74
 22  \w     55.00  81.00   0.50   10.00    --  110.25 -94.00-120.00   52
 23  \w    147.00 175.00   0.50   10.00    --  110.25  15.00  60.00   56
 24  \w    106.00 140.00   0.50   10.00    --  110.25  15.00  60.00   68
 25  \w     39.00  74.00   0.50   10.00    --  110.25 -61.00 120.00   70
 26  \w     99.00 176.00   0.50   10.00    --  110.25  30.00 -30.00  154
 27  \w    147.00 173.00   0.50   10.00    --  110.25  61.00-120.00   52
 28  \w     54.00  81.00   0.50   10.00    --  110.25 -94.00-180.00   54
 29  \w     69.00 108.00   0.50   10.00    --  110.25-125.00-150.00   78
 30  \w     39.00 131.00   0.50   10.00    --  110.25 -77.00 -30.00  184
 31  \w     94.00 132.00   0.50   10.00    --  110.25  61.00-120.00   76
 32  \w     46.00  79.00   0.50   10.00    --  110.25 -61.00-180.00   66
 33  \w     72.00  97.00   0.50   10.00    --  110.25 -94.00-150.00   50
 34  \w     80.00 105.00   0.50   10.00    --  110.25-125.00 120.00   50
 35  \w     43.00  80.00   0.50   10.00    --  110.25 -61.00 150.00   74
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0001953000
_diffrn_orient_matrix_UB_12      -0.1005437000
_diffrn_orient_matrix_UB_13      0.0230507000
_diffrn_orient_matrix_UB_21      -0.1076621000
_diffrn_orient_matrix_UB_22      -0.0311424000
_diffrn_orient_matrix_UB_23      -0.0404055000
_diffrn_orient_matrix_UB_31      0.1107682000
_diffrn_orient_matrix_UB_32      -0.0301805000
_diffrn_orient_matrix_UB_33      -0.0350428000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0772
_diffrn_reflns_av_unetI/netI     0.0649
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            21596
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.118
_diffrn_reflns_theta_min         3.558
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.803
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54024
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.624
_exptl_crystal_description       blade
_exptl_crystal_F_000             1845
_exptl_crystal_size_max          0.284
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.762
_refine_diff_density_min         -1.543
_refine_diff_density_rms         0.166
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     512
_refine_ls_number_reflns         7101
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.1276
_refine_ls_R_factor_gt           0.1017
_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^)+(0.0891P)^2^+54.3866P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2606
_refine_ls_wR_factor_ref         0.2764
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5166
_reflns_number_total             7101
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj03988f2.cif
_cod_data_source_block           ba92_lt_auto
_cod_original_formula_sum        'C136 H136.20 Cl17.37 N20 O35.20 Ru4'
_cod_database_code               7064176
_shelxl_version_number           2013-3
_diffrn_oxdiff_digest_frames
;
01692ca3e618e9b80f277d3a1a5903e4a4000263ef3
;
_diffrn_oxdiff_digest_hkl
;
01ab8847cb283726ff51c1939814042a29d2d2
;
_reflns_odcompleteness_completeness 96.07
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 C35-Cl3 \\sim C35-Cl4 \\sim C35-Cl6
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O10) = Uanis(O9)
4. Others
 Sof(C34)=Sof(H34A)=Sof(H34B)=1-FVAR(1)
 Sof(Cl4)=Sof(Cl3)=Sof(Cl6)=Sof(O10)=Sof(H10A)=Sof(H10B)=Sof(C35)=Sof(H35)=
 FVAR(1)
 Fixed Sof: O9(0.25) H9A(0.25) H9B(0.25)
5.a Rotating group:
 O10(H10A,H10B), O9(H9A,H9B)
5.b Ternary CH refined with riding coordinates:
 C26(H26), C29(H29), C25(H25), C30(H30), C35(H35)
5.c Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C11(H11A,H11B), C27(H27A,H27B), C28(H28A,H28B), C32(H32A,
 H32B), C33(H33A,H33B), C31(H31A,H31B), C34(H34A,H34B)
5.d Aromatic/amide H refined with riding coordinates:
 C9(H9), C24(H24), C21(H21), C10(H10), C3(H3), C4(H4), C5(H5), C13(H13),
 C23(H23), C17(H17), C16(H16), C14(H14), C20(H20)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              53445
_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 1.767
_oxdiff_exptl_absorpt_empirical_full_min 0.578