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_7064171
_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         'C33 H32 N4 O6 Ru, 2(C H Cl3)'
_chemical_formula_sum            'C35 H34 Cl6 N4 O6 Ru'
_chemical_formula_weight         920.43
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2025-11-27
_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                81.329(2)
_cell_angle_beta                 75.973(2)
_cell_angle_gamma                72.202(2)
_cell_formula_units_Z            2
_cell_length_a                   9.9781(2)
_cell_length_b                   12.8763(2)
_cell_length_c                   15.9233(3)
_cell_measurement_reflns_used    33156
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      30.9120
_cell_measurement_theta_min      2.4230
_cell_volume                     1883.32(6)
_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      149.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.973
_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    -28.00  26.00   0.50    0.70    --    4.44  98.00-124.00  108
  2  \w     -5.00  80.00   0.50    0.70    --    4.44  19.00-180.00  170
  3  \w    -18.00  38.00   0.50    0.70    --    4.44 -99.00 -30.00  112
  4  \w    -22.00  37.00   0.50    0.70    --    4.44 -98.00 128.00  118
  5  \w    -67.00  27.00   0.50    0.70    --    4.44 -77.00  60.00  188
  6  \w     -5.00  69.00   0.50    0.70    --   -6.08  19.00 120.00  148
  7  \w    -39.00  26.00   0.50    0.70    --   -6.08  98.00-124.00  130
  8  \w     -5.00  69.00   0.50    0.70    --   -6.08  19.00-150.00  148
  9  \w    -22.00  27.00   0.50    0.70    --   -6.08 -98.00 128.00   98
 10  \w    -18.00  22.00   0.50    0.70    --   -6.08 -99.00   0.00   80
 11  \w    -18.00  27.00   0.50    0.70    --   -6.08 -99.00 -60.00   90
;
_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      0.0021680000
_diffrn_orient_matrix_UB_12      -0.0080559000
_diffrn_orient_matrix_UB_13      -0.0434583000
_diffrn_orient_matrix_UB_21      -0.0598905000
_diffrn_orient_matrix_UB_22      0.0468181000
_diffrn_orient_matrix_UB_23      -0.0013576000
_diffrn_orient_matrix_UB_31      0.0472844000
_diffrn_orient_matrix_UB_32      0.0333699000
_diffrn_orient_matrix_UB_33      -0.0152394000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0334
_diffrn_reflns_av_unetI/netI     0.0253
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            45900
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         2.646
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.893
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86097
_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    1.623
_exptl_crystal_description       block
_exptl_crystal_F_000             932
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.274
_exptl_crystal_size_min          0.244
_refine_diff_density_max         0.609
_refine_diff_density_min         -0.555
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     637
_refine_ls_number_reflns         9100
_refine_ls_number_restraints     438
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0334
_refine_ls_R_factor_gt           0.0287
_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^)+(0.0409P)^2^+0.9205P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0737
_refine_ls_wR_factor_ref         0.0758
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8177
_reflns_number_total             9100
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj03988f2.cif
_cod_data_source_block           ba66_lt2_auto
_cod_original_cell_volume        1883.32(7)
_cod_database_code               7064171
_shelxl_version_number           2013-3
_diffrn_oxdiff_digest_frames
;
012bd1403092c302bb9cd5ef730971a42200031b24b
;
_diffrn_oxdiff_digest_hkl
;
010aa2713e630a7adecc2c92ebc2d884e9626e
;
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C35-Cl4
 1.76 with sigma of 0.02
 C35-Cl5
 1.76 with sigma of 0.02
 C35-Cl6
 1.76 with sigma of 0.02
 C35A-Cl4A
 1.76 with sigma of 0.02
 C35A-Cl5A
 1.76 with sigma of 0.02
 C35A-Cl6A
 1.76 with sigma of 0.02
 C34-Cl1
 1.76 with sigma of 0.02
 C34-Cl2
 1.76 with sigma of 0.02
 C34-Cl3
 1.76 with sigma of 0.02
 C34A-Cl1A
 1.76 with sigma of 0.02
 C34A-Cl2A
 1.76 with sigma of 0.02
 C34A-Cl3A
 1.76 with sigma of 0.02
 Cl4-Cl5
 2.88 with sigma of 0.03
 Cl4-Cl6
 2.88 with sigma of 0.03
 Cl5-Cl6
 2.88 with sigma of 0.03
 Cl4A-Cl5A
 2.88 with sigma of 0.03
 Cl4A-Cl6A
 2.88 with sigma of 0.03
 Cl5A-Cl6A
 2.88 with sigma of 0.03
 Cl1-Cl2
 2.88 with sigma of 0.03
 Cl1-Cl3
 2.88 with sigma of 0.03
 Cl2-Cl3
 2.88 with sigma of 0.03
 Cl1A-Cl2A
 2.88 with sigma of 0.03
 Cl1A-Cl3A
 2.88 with sigma of 0.03
 Cl2A-Cl3A
 2.88 with sigma of 0.03
 C13-C14 \\sim C13-C14A
 with sigma of 0.02
 C13-C18 \\sim C13-C18A
 with sigma of 0.02
 C14-H14 \\sim C14A-H14A
 with sigma of 0.02
 C14-C15 \\sim C14A-C15A
 with sigma of 0.02
 C18-H18 \\sim C18A-H18A
 with sigma of 0.02
 C18-C17 \\sim C18A-C17A
 with sigma of 0.02
 C15-H15 \\sim C15A-H15A
 with sigma of 0.02
 C15-C16 \\sim C15A-C16A
 with sigma of 0.02
 C16-H16 \\sim C16A-H16A
 with sigma of 0.02
 C16-C17 \\sim C16A-C17A
 with sigma of 0.02
 C17-H17 \\sim C17A-H17A
 with sigma of 0.02
 C13-H14 \\sim C13-H14A
 with sigma of 0.04
 C13-H18 \\sim C13-H18A
 with sigma of 0.04
 C13-C15 \\sim C13-C15A
 with sigma of 0.04
 C13-C17 \\sim C13-C17A
 with sigma of 0.04
 C14-H15 \\sim C14A-H15A
 with sigma of 0.04
 C14-C16 \\sim C14A-C16A
 with sigma of 0.04
 H14-C15 \\sim H14A-C15A
 with sigma of 0.04
 C18-C16 \\sim C18A-C16A
 with sigma of 0.04
 C18-H17 \\sim C18A-H17A
 with sigma of 0.04
 H18-C17 \\sim H18A-C17A
 with sigma of 0.04
 C15-H16 \\sim C15A-H16A
 with sigma of 0.04
 C15-C17 \\sim C15A-C17A
 with sigma of 0.04
 H15-C16 \\sim H15A-C16A
 with sigma of 0.04
 C16-H17 \\sim C16A-H17A
 with sigma of 0.04
 H16-C17 \\sim H16A-C17A
 with sigma of 0.04
3. Rigid bond restraints
 C14, C15, C16, C17, C18
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C35A \\sim Cl6A \\sim Cl4A \\sim Cl5A: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
C34A \\sim Cl1A \\sim Cl2A \\sim Cl3A: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17 \\sim C18: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
O5 \\sim N4 \\sim O6 \\sim C35 \\sim H35 \\sim Cl6 \\sim Cl4 \\sim Cl5: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C35A \\sim H35A \\sim Cl6A \\sim Cl4A \\sim Cl5A \\sim N4A \\sim O5A \\sim O6A:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
O5 \\sim N4 \\sim O6 \\sim C14 \\sim H14 \\sim C18 \\sim H18 \\sim C15 \\sim
H15 \\sim C16 \\sim H16 \\sim C17 \\sim H17 \\sim C35 \\sim H35 \\sim Cl6 \\sim
Cl4 \\sim Cl5: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C35A \\sim H35A \\sim Cl6A \\sim Cl4A \\sim Cl5A \\sim N4A \\sim O5A \\sim O6A
\\sim C14A \\sim H14A \\sim H15A \\sim C15A \\sim C16A \\sim H16A \\sim H17A
\\sim C17A \\sim C18A \\sim H18A: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
Uanis(C16) \\sim Ueq, Uanis(C17) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
5. Rigid body (RIGU) restrains
 C35, Cl6, Cl5, Cl4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C35A, Cl6A, Cl5A, Cl4A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C34, Cl1, Cl3, Cl2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C34A, Cl1A, Cl2A, Cl3A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C13, C14, C15, C16, C17, C18
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O5, N4, O6, C35, H35, Cl6, Cl4, Cl5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C35A, H35A, Cl6A, Cl4A, Cl5A, N4A, O5A, O6A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O5, N4, O6, C14, H14, C18, H18, C15, H15, C16, H16, C17, H17, C35, H35, Cl6,
 Cl4, Cl5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C35A, H35A, Cl6A, Cl4A, Cl5A, N4A, O5A, O6A, C14A, H14A, H15A, C15A, C16A,
 H16A, H17A, C17A, C18A, H18A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C35A)=Sof(H35A)=Sof(Cl6A)=Sof(Cl4A)=Sof(Cl5A)=1-FVAR(1)
 Sof(C35)=Sof(H35)=Sof(Cl6)=Sof(Cl4)=Sof(Cl5)=FVAR(1)
 Sof(C34A)=Sof(H34A)=Sof(Cl1A)=Sof(Cl2A)=Sof(Cl3A)=1-FVAR(2)
 Sof(C34)=Sof(H34)=Sof(Cl1)=Sof(Cl2)=Sof(Cl3)=FVAR(2)
 Sof(N4A)=Sof(O5A)=Sof(O6A)=1-FVAR(3)
 Sof(O5)=Sof(N4)=Sof(O6)=FVAR(3)
 Sof(C14A)=Sof(H14A)=Sof(H15A)=Sof(C15A)=Sof(C16A)=Sof(H16A)=Sof(H17A)=
 Sof(C17A)=Sof(C18A)=Sof(H18A)=1-FVAR(4)
 Sof(C14)=Sof(H14)=Sof(C18)=Sof(H18)=Sof(C15)=Sof(H15)=Sof(C16)=Sof(H16)=
 Sof(C17)=Sof(H17)=FVAR(4)
7.a Ternary CH refined with riding coordinates:
 C27(H27), C26(H26), C30(H30), C31(H31), C35(H35), C35A(H35A), C34(H34),
 C34A(H34A)
7.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C19(H19A,H19B), C29(H29A,H29B), C33(H33A,H33B), C28(H28A,
 H28B), C12(H12A,H12B), C32(H32A,H32B)
7.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C3(H3), C9(H9), C25(H25), C4(H4), C10(H10), C24(H24), C14(H14),
 C18(H18), C21(H21), C15(H15), C16(H16), C17(H17), C22(H22)
;
_shelx_res_checksum              50969
_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 1.457
_oxdiff_exptl_absorpt_empirical_full_min 0.655