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_7712346
_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         'C12 H17 Cl3 N3 O Ru, C H4 O'
_chemical_formula_sum            'C13 H21 Cl3 N3 O2 Ru'
_chemical_formula_weight         458.75
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2022-09-04
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-09-04 deposited with the CCDC.	2023-02-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.992(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9711(2)
_cell_length_b                   11.9322(2)
_cell_length_c                   14.5760(3)
_cell_measurement_reflns_used    16799
_cell_measurement_temperature    300
_cell_measurement_theta_max      27.1100
_cell_measurement_theta_min      1.9090
_cell_volume                     1884.68(6)
_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      300
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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     -2.00  53.00   0.50    8.55    --   10.55  30.00 -21.00  110
  2  \w     16.00  54.00   0.50    8.55    --  -11.09  30.00 -21.00   76
  3  \w     -5.00  29.00   0.50    8.55    --   10.55  37.00  90.00   68
  4  \w     43.00  74.00   0.50    8.55    --   10.55  37.00  90.00   62
  5  \w    -23.00   4.00   0.50    8.55    --   10.55 -99.00  60.00   54
  6  \w     10.00  44.00   0.50    8.55    --   10.55 -99.00  60.00   68
  7  \w     21.00  60.00   0.50    8.55    --   10.55-125.00  30.00   78
  8  \w     13.00  39.00   0.50    8.55    --   10.55-125.00 -60.00   52
  9  \w     12.00  61.00   0.50    8.55    --   10.55-125.00-150.00   98
 10  \w     14.00  58.00   0.50    8.55    --   10.55-125.00-180.00   88
 11  \w     -4.00  25.00   0.50    8.55    --   10.55 -57.00-180.00   58
 12  \w    -23.00  13.00   0.50    8.55    --  -11.09 -99.00-120.00   72
 13  \w    -17.00  13.00   0.50    8.55    --  -11.09 -99.00 -60.00   60
 14  \w    -18.00   8.00   0.50    8.55    --  -11.09 -99.00  60.00   52
 15  \w     12.00  48.00   0.50    8.55    --   10.55-125.00 120.00   72
 16  \w    -53.00 -22.00   0.50    8.55    --   10.55 -19.00 150.00   62
 17  \w    -58.00  14.00   0.50    8.55    --   10.55 -30.00 178.00  144
 18  \w    -23.00  24.00   0.50    8.55    --  -11.09 -99.00-180.00   94
 19  \w    -52.00 -14.00   0.50    8.55    --   10.55 -57.00-180.00   76
 20  \w    -59.00 -12.00   0.50    8.55    --   10.55 -19.00 -90.00   94
 21  \w    -62.00   4.00   0.50    8.55    --   10.55 -19.00 -60.00  132
 22  \w    -79.00  -1.00   0.50    8.55    --  -11.09 -30.00 178.00  156
;
_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      0.0619955000
_diffrn_orient_matrix_UB_12      -0.0139715000
_diffrn_orient_matrix_UB_13      -0.0033862000
_diffrn_orient_matrix_UB_21      -0.0195324000
_diffrn_orient_matrix_UB_22      -0.0531810000
_diffrn_orient_matrix_UB_23      -0.0184299000
_diffrn_orient_matrix_UB_31      -0.0077668000
_diffrn_orient_matrix_UB_32      0.0225757000
_diffrn_orient_matrix_UB_33      -0.0455639000
_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  0.0611
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            27015
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.021
_diffrn_reflns_theta_min         1.879
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.265
_exptl_absorpt_correction_T_max  0.846
_exptl_absorpt_correction_T_min  0.753
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.617
_exptl_crystal_description       irregular
_exptl_crystal_F_000             924
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.599
_refine_diff_density_min         -0.677
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         3713
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0309
_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^)+(0.0500P)^2^+0.3459P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0835
_refine_ls_wR_factor_ref         0.0868
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3258
_reflns_number_total             3713
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00243h2.cif
_cod_data_source_block           aks-nsh-1b1
_cod_database_code               7712346
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C64 H88 Cl12 N4 O4 Ru4 '
_shelx_estimated_absorpt_t_max   0.833
_shelx_estimated_absorpt_t_min   0.695
_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, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C9(H9)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C3(H3), C8(H8), C2(H2), C7(H7), C6(H6)
2.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C1S(H1SA,H1SB,H1SC), C10(H10A,H10B,
 H10C)
2.d Idealised tetrahedral OH refined as rotating group:
 O1(H1), O1S(H1S)
;
_shelx_res_checksum              92781
_shelx_hkl_checksum              20177
_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 1.784
_oxdiff_exptl_absorpt_empirical_full_min 0.497