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_7064168
_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         'C20 H23 N3 O4 Ru, H2 O'
_chemical_formula_sum            'C20 H25 N3 O5 Ru'
_chemical_formula_weight         488.50
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2025-11-06
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.82300(10)
_cell_length_b                   15.2957(2)
_cell_length_c                   16.3651(2)
_cell_measurement_reflns_used    18614
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      78.1680
_cell_measurement_theta_min      2.6950
_cell_volume                     1958.22(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      149.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.975
_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     98.00 178.00   0.50    0.10    --  110.25  30.00   0.00  160
  2  \w     24.00 119.00   0.50    0.05    --   46.95  77.00-180.00  190
  3  \w     24.00 119.00   0.50    0.05    --   46.95  77.00 -60.00  190
  4  \w     24.00 119.00   0.50    0.05    --   46.95  77.00  60.00  190
  5  \w     32.00 118.00   0.50    0.05    --   46.95  57.00 150.00  172
  6  \w     38.00 105.00   0.50    0.10    --  110.25 -90.00   1.00  134
  7  \w     38.00  80.00   0.50    0.10    --  110.25 -61.00 -30.00   84
  8  \w     38.00 111.00   0.50    0.10    --  110.25-125.00 -90.00  146
  9  \w     38.00  80.00   0.50    0.10    --  110.25 -61.00-120.00   84
 10  \w     38.00  80.00   0.50    0.10    --  110.25 -61.00 -90.00   84
 11  \w     18.00  95.00   0.50    0.05    --   46.95-125.00   0.00  154
 12  \w     38.00  80.00   0.50    0.10    --  110.25 -61.00 150.00   84
 13  \w     38.00  80.00   0.50    0.10    --  110.25 -61.00 120.00   84
 14  \w     59.00 119.00   0.50    0.05    --   46.95 154.00  -8.00  120
 15  \w     82.00 178.00   0.50    0.10    --  110.25 120.00-165.00  192
 16  \w     -5.00  29.00   0.50    0.05    --  -46.95  19.00  90.00   68
 17  \w     -5.00  29.00   0.50    0.05    --  -46.95  19.00 120.00   68
 18  \w    -27.00  13.00   0.50    0.05    --   46.95 -19.00  90.00   80
 19  \w     -5.00  29.00   0.50    0.05    --  -46.95  19.00  30.00   68
 20  \w   -112.00 -29.00   0.50    0.10    -- -102.00 125.00   0.00  166
 21  \w   -167.00 -88.00   0.50    0.10    -- -102.00 -15.00-120.00  158
 22  \w   -175.00 -90.00   0.50    0.10    -- -102.00 -77.00 -30.00  170
 23  \w   -175.00 -85.00   0.50    0.10    -- -102.00 -61.00 150.00  180
 24  \w   -175.00 -88.00   0.50    0.10    -- -102.00 -33.00 177.00  174
 25  \w   -175.00 -79.00   0.50    0.10    -- -102.00 -77.00 120.00  192
 26  \w   -174.00 -89.00   0.50    0.10    -- -102.00 -45.00  60.00  170
 27  \w   -175.00 -80.00   0.50    0.10    -- -102.00 -90.00   1.00  190
 28  \w   -119.00 -74.00   0.50    0.05    --  -46.95-125.00 -90.00   90
 29  \w   -119.00 -74.00   0.50    0.05    --  -46.95-125.00   0.00   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      0.0926809000
_diffrn_orient_matrix_UB_12      -0.0101296000
_diffrn_orient_matrix_UB_13      -0.0824751000
_diffrn_orient_matrix_UB_21      0.1538594000
_diffrn_orient_matrix_UB_22      -0.0418016000
_diffrn_orient_matrix_UB_23      0.0439956000
_diffrn_orient_matrix_UB_31      -0.0807398000
_diffrn_orient_matrix_UB_32      -0.0910900000
_diffrn_orient_matrix_UB_33      -0.0110047000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_unetI/netI     0.0251
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            23077
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.052
_diffrn_reflns_theta_min         3.956
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.813
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55964
_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    1.657
_exptl_crystal_description       block
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.254
_exptl_crystal_size_min          0.190
_refine_diff_density_max         0.430
_refine_diff_density_min         -0.924
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.360(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         3988
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0258
_refine_ls_R_factor_gt           0.0253
_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^)+(0.0247P)^2^+2.3362P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0626
_refine_ls_wR_factor_ref         0.0628
_reflns_Friedel_coverage         0.747
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.971
_reflns_number_gt                3921
_reflns_number_total             3988
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj03988f2.cif
_cod_data_source_block           ba32_lt_auto
_cod_database_code               7064168
_shelxl_version_number           2013-3
_chemical_oxdiff_formula         'C20 H25 N3 O5 Ru'
_diffrn_oxdiff_digest_frames
;
01794819fad2674a669c8810fd6c1ac66a00055ab5b
;
_diffrn_oxdiff_digest_hkl
;
0198505244e0dd95ac48b66e53795f5e996609
;
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.640(11)
 0.360(11)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
3.a Free rotating group:
 O5(H5A,H5B)
3.b Ternary CH refined with riding coordinates:
 C13(H13), C17(H17), C18(H18), C14(H14)
3.c Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C15(H15A,H15B), C16(H16A,H16B), C19(H19A,H19B)
3.d Aromatic/amide H refined with riding coordinates:
 C4(H4), C3(H3), C5(H5), C10(H10), C9(H9)
3.e Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C)
;
_shelx_res_checksum              12957
_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 1.572
_oxdiff_exptl_absorpt_empirical_full_min 0.725