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_7712347
_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         'C11 H12 Cl3 N4 Ru, 0.75[CH3CN]'
_chemical_formula_sum            'C12.5 H14.25 Cl3 N4.75 Ru'
_chemical_formula_weight         438.46
_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   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                 104.622(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.1527(5)
_cell_length_b                   17.7460(14)
_cell_length_c                   12.1658(7)
_cell_measurement_reflns_used    8613
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.0750
_cell_measurement_theta_min      2.0680
_cell_volume                     1703.1(2)
_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                 '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 0.999
_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      9.00  77.00   0.50   21.79    --   10.55  37.00 -30.00  136
  2  \w     61.00  87.00   0.50   21.79    --   10.55   6.00  76.00   52
  3  \w     18.00  44.00   0.50   21.79    --  -11.09  37.00  60.00   52
  4  \w     12.00  67.00   0.50   21.79    --  -11.09   6.00  76.00  110
  5  \w    -17.00  23.00   0.50   21.79    --  -11.09 -99.00 -30.00   80
  6  \w     12.00  61.00   0.50   21.79    --   10.55-125.00 -60.00   98
  7  \w     21.00  61.00   0.50   21.79    --   10.55-125.00 -90.00   80
  8  \w     16.00  50.00   0.50   21.79    --   10.55-125.00-180.00   68
  9  \w    -10.00  20.00   0.50   21.79    --  -11.09 -99.00-180.00   60
 10  \w    -17.00  16.00   0.50   21.79    --  -11.09 -99.00-150.00   66
 11  \w    -23.00   2.00   0.50   21.79    --   10.55 -19.00 -90.00   50
 12  \w    -48.00   5.00   0.50   21.79    --  -11.09  -6.00 -99.00  106
 13  \w    -49.00 -24.00   0.50   21.79    --   10.55 -19.00 -90.00   50
 14  \w    -49.00  20.00   0.50   21.79    --   10.55 -37.00-150.00  138
 15  \w     13.00  53.00   0.50   21.79    --   10.55-125.00 -30.00   80
 16  \w     12.00  58.00   0.50   21.79    --   10.55-125.00  30.00   92
 17  \w    -25.00  14.00   0.50   21.79    --  -11.09  37.00  60.00   78
 18  \w    -63.00 -24.00   0.50   21.79    --   10.55  -6.00 -99.00   78
 19  \w    -62.00   3.00   0.50   21.79    --   10.55 -19.00 150.00  130
 20  \w    -87.00 -60.00   0.50   21.79    --  -11.09  -6.00 -99.00   54
;
_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      -0.0505090000
_diffrn_orient_matrix_UB_12      0.0187938000
_diffrn_orient_matrix_UB_13      0.0311084000
_diffrn_orient_matrix_UB_21      0.0742415000
_diffrn_orient_matrix_UB_22      0.0107414000
_diffrn_orient_matrix_UB_23      0.0415589000
_diffrn_orient_matrix_UB_31      0.0046421000
_diffrn_orient_matrix_UB_32      0.0336093000
_diffrn_orient_matrix_UB_33      -0.0305932000
_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  0.0867
_diffrn_reflns_av_unetI/netI     0.0829
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            22271
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.010
_diffrn_reflns_theta_min         2.076
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.390
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43343
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.710
_exptl_crystal_description       irregular
_exptl_crystal_F_000             870
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.537
_refine_diff_density_min         -0.557
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_reflns         3327
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0988
_refine_ls_R_factor_gt           0.0555
_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^)+(0.0748P)^2^+0.8725P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1346
_refine_ls_wR_factor_ref         0.1509
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2130
_reflns_number_total             3327
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00243h2.cif
_cod_data_source_block           aks-nsh-1a12-1a
_cod_original_formula_sum        'C12.50 H14.25 Cl3 N4.75 Ru'
_cod_database_code               7712347
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C4 H4 N4 Cl3 Ru '
_shelx_estimated_absorpt_t_max   0.808
_shelx_estimated_absorpt_t_min   0.689
_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), C8(H8), C2(H2), C7(H7), C5(H5), C6(H6)
2.b Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C11(H11A,H11B,H11C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              12089
_shelx_hkl_checksum              4138
_shelx_fab_checksum              45948
_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 2.954
_oxdiff_exptl_absorpt_empirical_full_min 0.538