Base-free synthesis of benchtop stable Ru(III)-NHC complexes from RuCl3·3H2O and their use as precursors for Ru(II)-NHC complexes
Shahid, Nida; Singh, Rahul Kumar; Srivastava, Navdeep; Singh, Amrendra Kumar; Dalton Transactions  (2023) –; doi:10.1039/D3DT00243H

data_7712348
_publ_section_title
;
 Base-free synthesis of benchtop stable Ru(III)-NHC complexes from
 RuCl3&#x00B7;3H2O and their use as precursors for Ru(II)-NHC complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00243H
_journal_year                    2023
_chemical_formula_moiety         'C22 H22 I N8 Ru, F6 P'
_chemical_formula_sum            'C22 H22 F6 I N8 P Ru'
_chemical_formula_weight         771.41
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-02-11
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-02-11 deposited with the CCDC.	2023-02-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.553(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.0771(5)
_cell_length_b                   10.9379(5)
_cell_length_c                   16.8084(6)
_cell_measurement_reflns_used    2712
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      67.8610
_cell_measurement_theta_min      4.8660
_cell_volume                     2682.97(19)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (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                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0309
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.937
_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    -29.00  11.00   1.00    8.00    --    0.00 108.00-156.00   40
  2  \w     10.00 101.00   1.00    8.00    --   54.00-108.00 107.00   91
  3  \w     54.00  96.00   1.00    8.00    --  108.00-108.00 107.00   42
  4  \w    109.00 152.00   1.00    8.00    --  108.00 108.00-156.00   43
  5  \w     34.00  59.00   1.00    8.00    --    0.00  57.00-180.00   25
  6  \w    -11.00  66.00   1.00    8.00    --    0.00  57.00 120.00   77
  7  \w     33.00 123.00   1.00    8.00    --   54.00  57.00-120.00   90
  8  \w     24.00  51.00   1.00    8.00    --   54.00 -38.00 120.00   27
  9  \w     71.00 112.00   1.00    8.00    --   54.00  77.00 -90.00   41
 10  \w     41.00 114.00   1.00    8.00    --   54.00  57.00 150.00   73
 11  \w     74.00 101.00   1.00    8.00    --  108.00-111.00-180.00   27
 12  \w    117.00 158.00   1.00    8.00    --  108.00  63.00  90.00   41
 13  \w     41.00 103.00   1.00    8.00    --  108.00-111.00 -60.00   62
 14  \w     41.00 132.00   1.00    8.00    --  108.00 -77.00 120.00   91
 15  \w     84.00 131.00   1.00    8.00    --  108.00  77.00 -30.00   47
 16  \w     80.00 172.00   1.00    8.00    --  108.00  77.00-120.00   92
 17  \w     41.00 141.00   1.00    8.00    --  108.00 -25.00  60.00  100
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0489994000
_diffrn_orient_matrix_UB_12      -0.1244019000
_diffrn_orient_matrix_UB_13      -0.0160514000
_diffrn_orient_matrix_UB_21      -0.0734511000
_diffrn_orient_matrix_UB_22      0.0563865000
_diffrn_orient_matrix_UB_23      -0.0713103000
_diffrn_orient_matrix_UB_31      0.0581192000
_diffrn_orient_matrix_UB_32      -0.0338586000
_diffrn_orient_matrix_UB_33      -0.0601806000
_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  0.1243
_diffrn_reflns_av_unetI/netI     0.1136
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.937
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10376
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.937
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.799
_diffrn_reflns_theta_min         4.872
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    14.975
_exptl_absorpt_correction_T_max  0.403
_exptl_absorpt_correction_T_min  0.071
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
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    1.910
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.721
_refine_diff_density_min         -1.234
_refine_diff_density_rms         0.192
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         4767
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1579
_refine_ls_R_factor_gt           0.1166
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3174
_refine_ls_wR_factor_ref         0.3690
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2459
_reflns_number_total             4767
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00243h2.cif
_cod_data_source_block           aks187a-3a
_cod_database_code               7712348
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N7 F6 P1 I1 Ru1'
_shelx_estimated_absorpt_t_max   0.380
_shelx_estimated_absorpt_t_min   0.112
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C16(H16), C18(H18), C15(H15), C8(H8), C6(H6), C12(H12), C11(H11),
 C2(H2), C19(H19), C14(H14), C5(H5), C7(H7)
2.b Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C9(H9A,H9B,H9C), C22(H22A,H22B,H22C)
;
_shelx_res_checksum              49959
_shelx_hkl_checksum              98266
_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
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 13.884
_oxdiff_exptl_absorpt_empirical_full_min 0.113