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_7712349
_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         'C51 H44 Cl N4 P2 Ru, Cl, 2[CH3CN]'
_chemical_formula_sum            'C55 H50 Cl2 N6 P2 Ru'
_chemical_formula_weight         1028.92
_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                 100.884(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8605(4)
_cell_length_b                   23.0124(7)
_cell_length_c                   19.4293(6)
_cell_measurement_reflns_used    7066
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.7580
_cell_measurement_theta_min      3.1710
_cell_volume                     5207.6(3)
_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 0.996
_diffrn_measured_fraction_theta_max 0.979
_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     17.00  54.00   0.50    7.00    --   18.01-154.00 -40.00   74
  2  \w     -1.00  37.00   0.50    7.00    --   18.01-120.00 117.00   76
  3  \w    -73.00 -48.00   0.50    7.00    --  -19.26 120.00-158.00   50
  4  \w     -8.00  90.00   0.50    7.00    --   18.01  37.00 -30.00  196
  5  \w     35.00  60.00   0.50    7.00    --   18.01 178.00  90.00   50
  6  \w      8.00  46.00   0.50    7.00    --   18.01  37.00  90.00   76
  7  \w      9.00  35.00   0.50    7.00    --   18.01  57.00  60.00   52
  8  \w    -19.00  59.00   0.50    7.00    --   18.01 -99.00 150.00  156
  9  \w    -69.00 -42.00   0.50    7.00    --  -19.26 -37.00-120.00   54
;
_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      0.0130932000
_diffrn_orient_matrix_UB_12      0.0284727000
_diffrn_orient_matrix_UB_13      0.0130681000
_diffrn_orient_matrix_UB_21      0.0448104000
_diffrn_orient_matrix_UB_22      -0.0112838000
_diffrn_orient_matrix_UB_23      0.0259931000
_diffrn_orient_matrix_UB_31      0.0391155000
_diffrn_orient_matrix_UB_32      0.0033891000
_diffrn_orient_matrix_UB_33      -0.0231644000
_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  0.0858
_diffrn_reflns_av_unetI/netI     0.0971
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            39492
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.479
_diffrn_reflns_theta_min         3.057
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.507
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.34748
_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    1.312
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2120
_exptl_crystal_size_max          0.266
_exptl_crystal_size_mid          0.216
_exptl_crystal_size_min          0.175
_refine_diff_density_max         0.970
_refine_diff_density_min         -0.624
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     543
_refine_ls_number_reflns         11693
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.1083
_refine_ls_R_factor_gt           0.0625
_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^)+(0.0778P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1532
_refine_ls_wR_factor_ref         0.1844
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6710
_reflns_number_total             11693
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00243h2.cif
_cod_data_source_block           aks230a2-2c
_cod_database_code               7712349
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHNPRuCl
_shelx_estimated_absorpt_t_max   0.917
_shelx_estimated_absorpt_t_min   0.877
_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:
 C00C(H00C), C00J(H00J), C00K(H00K), C00L(H00L), C00M(H00M), C00O(H00O),
 C00P(H00P), C00Q(H00Q), C00R(H00R), C00S(H00S), C00T(H00T), C00U(H00U),
 C00V(H00V), C00W(H00W), C00X(H00X), C00Z(H00Z), C010(H010), C012(H012),
 C013(H013), C014(H014), C015(H015), C016(H016), C018(H018), C019(H019),
 C01A(H01D), C01B(H01E), C01C(H01F), C01D(H01G), C01E(H01H), C01F(H01I),
 C01G(H01J), C01H(H01K), C01I(H01L), C01J(H01M), C01K(H01N), C01L(H01O),
 C01M(H01P), C01N(H01Q)
2.b Idealised Me refined as rotating group:
 C011(H01A,H01B,H01C), C01O(H01R,H01S,H01T)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              86365
_shelx_hkl_checksum              97491
_shelx_fab_checksum              23542
_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 2.947
_oxdiff_exptl_absorpt_empirical_full_min 0.463