Ru(ii)–CNC pincer complexes with bis(protic-NHC): comparative analysis with bis(classical-NHC) and mixed protic- & classical-NHC analogues
Saha, Achena; Yadav, Ekta; Nath, Shambhu; Singh, Ashu; Singh, Amrendra K.; New Journal of Chemistry 49 (2025) 18191–18201; doi:10.1039/D5NJ03111G

data_7064015
_publ_section_title
;
 Ru(ii)--CNC pincer complexes with bis(protic-NHC): comparative analysis
 with bis(classical-NHC) and mixed protic- &amp; classical-NHC analogues
;
_journal_issue                   41
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              18191
_journal_page_last               18201
_journal_paper_doi               10.1039/D5NJ03111G
_journal_volume                  49
_journal_year                    2025
_chemical_formula_moiety         'C28 H22 I N8 Ru, F6 P, C H4 O'
_chemical_formula_sum            'C29 H26 F6 I N8 O P Ru'
_chemical_formula_weight         875.52
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-06-08
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-05-15 deposited with the CCDC.	2025-09-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.92860(10)
_cell_length_b                   13.8785(2)
_cell_length_c                   29.4112(4)
_cell_measurement_reflns_used    36151
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.9780
_cell_measurement_theta_min      2.1430
_cell_volume                     3236.32(8)
_computing_cell_refinement       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_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      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.974
_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     -8.00  83.00   0.50    5.00    --   10.96  20.00 -52.00  182
  2  \w     -4.00  77.00   0.50    5.00    --   10.96  37.00  90.00  162
  3  \w    -22.00  24.00   0.50    5.00    --  -11.35 -99.00  60.00   92
  4  \w      5.00  55.00   0.50    5.00    --   10.96-115.00  52.00  100
  5  \w     12.00  61.00   0.50    5.00    --   10.96-125.00 120.00   98
  6  \w      1.00  53.00   0.50    5.00    --   10.96-110.00 -42.00  104
  7  \w    -16.00  80.00   0.50    5.00    --   10.96  77.00-120.00  192
  8  \w    -45.00 -19.00   0.50    5.00    --   10.96 -19.00  90.00   52
  9  \w    -61.00   5.00   0.50    5.00    --   10.96 -19.00  60.00  132
 10  \w    -61.00   5.00   0.50    5.00    --   10.96 -19.00   0.00  132
 11  \w    -61.00   5.00   0.50    5.00    --   10.96 -19.00 -60.00  132
 12  \w     12.00  61.00   0.50    5.00    --   10.96-125.00 -90.00   98
 13  \w     30.00  61.00   0.50    5.00    --   10.96-125.00-150.00   62
 14  \w     12.00  61.00   0.50    5.00    --   10.96-125.00-180.00   98
 15  \w     12.00  61.00   0.50    5.00    --   10.96-125.00 -60.00   98
 16  \w    -83.00   7.00   0.50    5.00    --  -11.35 -20.00 140.00  180
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0169496000
_diffrn_orient_matrix_UB_12      -0.0065162000
_diffrn_orient_matrix_UB_13      0.0234769000
_diffrn_orient_matrix_UB_21      -0.0169500000
_diffrn_orient_matrix_UB_22      0.0499732000
_diffrn_orient_matrix_UB_23      0.0022005000
_diffrn_orient_matrix_UB_31      -0.0861773000
_diffrn_orient_matrix_UB_32      -0.0085249000
_diffrn_orient_matrix_UB_33      -0.0050669000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_unetI/netI     0.0257
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            52668
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.401
_diffrn_reflns_theta_min         2.018
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.561
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83029
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.797
_exptl_crystal_description       block
_exptl_crystal_F_000             1720
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.607
_refine_diff_density_min         -0.604
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details
;
 Flack x determined using 2503 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.020(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     427
_refine_ls_number_reflns         7087
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0410
_refine_ls_R_factor_gt           0.0340
_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^)+(0.0476P)^2^+1.7840P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0846
_refine_ls_wR_factor_ref         0.0888
_reflns_Friedel_coverage         0.749
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.947
_reflns_number_gt                6271
_reflns_number_total             7087
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj03111g2.cif
_cod_data_source_block           as1
_cod_depositor_comments          'Adding full bibliography for 7064015.cif.'
_cod_database_code               7064015
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N F P I Ru'
_shelx_estimated_absorpt_t_max   0.706
_shelx_estimated_absorpt_t_min   0.643
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N3(H3), N5(H5), C4(H4), C5(H5A), C6(H6), C7(H7), C11(H11), C12(H12), C13(H13),
  C14(H14), C16(H16), C17(H17), C18(H18), C21(H21), C22(H22), C24(H24),
 C25(H25), C26(H26), C27(H27)
2.b Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C1S(H1SA,H1SB,H1SC)
2.c Idealised tetrahedral OH refined as rotating group:
 O1S(H1S)
;
_shelx_res_checksum              28439
_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 1.311
_oxdiff_exptl_absorpt_empirical_full_min 0.836