Protic- or anionic-NHCs with a classical-NHC in a single [Ru(CNC)(PPh<sub>3</sub>)<sub>2</sub>Cl]Cl pincer complex: direct comparison of structure & electronic properties and heterolytic H<sub>2</sub> splitting.
Srivastava, Navdeep; Singh, Amrendra K.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 6870–6874; doi:10.1039/d4dt00623b

data_7715670
_publ_section_title
;
 Protic- or anionic-NHCs with a classical-NHC in a single
 [Ru(CNC)(PPh<sub>3</sub>)<sub>2</sub>Cl]Cl pincer complex: direct
 comparison of structure &amp; electronic properties and heterolytic
 H<sub>2</sub> splitting.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6870
_journal_page_last               6874
_journal_paper_doi               10.1039/d4dt00623b
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C48 H41 Cl N5 P2 Ru, Cl, H2 O'
_chemical_formula_sum            'C48 H43 Cl2 N5 O P2 Ru'
_chemical_formula_weight         939.78
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-09-27
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-02-28 deposited with the CCDC.	2024-04-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.447(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.9308(2)
_cell_length_b                   17.8608(2)
_cell_length_c                   21.5668(5)
_cell_measurement_reflns_used    20901
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.3000
_cell_measurement_theta_min      1.8720
_cell_volume                     4450.42(14)
_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 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     -5.00  85.00   0.75   14.00    --   18.33  65.00 167.00  120
  2  \w    -49.00  41.00   0.75   14.00    --   18.33 -65.00  31.00  120
  3  \w    -43.00  47.00   0.75   14.00    --  -19.73  65.00 167.00  120
  4  \w    -87.00   3.00   0.75   14.00    --  -19.73 -65.00  31.00  120
  5  \w     34.00  94.00   0.75   14.00    --   18.33-178.00-180.00   80
  6  \w    -12.00  87.00   0.75   14.00    --   18.33  77.00   0.00  132
  7  \w    -54.00  43.50   0.75   14.00    --   18.33 -37.00-120.00  130
  8  \w    -75.00 -21.00   0.75   14.00    --  -19.73 121.00 -92.69   72
  9  \w    -90.00   9.00   0.75   14.00    --  -19.73 -77.00 150.00  132
 10  \w    -93.00  24.00   0.75   14.00    --  -19.73 -19.00 -60.00  156
 11  \w    -81.00 -27.00   0.75   14.00    --  -19.73 131.00-138.47   72
 12  \w     -3.00  87.00   0.75   14.00    --   18.33  57.00 -60.00  120
 13  \w    -20.00  42.25   0.75   14.00    --   18.33 -99.00   0.00   83
 14  \w    -82.00 -28.00   0.75   14.00    --  -19.73 132.00  83.95   72
;
_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      0.0584614000
_diffrn_orient_matrix_UB_12      0.0041887000
_diffrn_orient_matrix_UB_13      -0.0013432000
_diffrn_orient_matrix_UB_21      -0.0169237000
_diffrn_orient_matrix_UB_22      -0.0043548000
_diffrn_orient_matrix_UB_23      -0.0337628000
_diffrn_orient_matrix_UB_31      -0.0081338000
_diffrn_orient_matrix_UB_32      0.0392300000
_diffrn_orient_matrix_UB_33      -0.0035986000
_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  0.1053
_diffrn_reflns_av_unetI/netI     0.0507
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            81376
_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         25.349
_diffrn_reflns_theta_min         1.950
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.586
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_correction_T_min  0.968
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_description       block
_exptl_crystal_F_000             1928
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.963
_refine_diff_density_min         -0.671
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.165
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     536
_refine_ls_number_reflns         8144
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.165
_refine_ls_R_factor_all          0.1209
_refine_ls_R_factor_gt           0.0801
_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^)+(0.0049P)^2^+33.8824P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1513
_refine_ls_wR_factor_ref         0.1774
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5823
_reflns_number_total             8144
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00623b2.cif
_cod_data_source_block           red1a2
_cod_depositor_comments
'Adding full bibliography for 7715668--7715671.cif.'
_cod_database_code               7715670
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C48H41Cl2N5P2Ru
_shelx_estimated_absorpt_t_max   0.907
_shelx_estimated_absorpt_t_min   0.839
_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,H) groups
2.a Free rotating group:
 O1S(H1SA,H1SB)
2.b Aromatic/amide H refined with riding coordinates:
 N1(H1), C38(H38), C5(H5), C19(H19), C30(H30), C39(H39), C6(H6), C48(H48),
 C36(H36), C44(H44), C26(H26), C23(H23), C42(H42), C7(H7), C10(H10), C35(H35),
 C27(H27), C28(H28), C22(H22), C9(H9), C45(H45), C40(H40), C47(H47), C20(H20),
 C3(H3), C18(H18), C21(H21), C29(H29), C46(H46), C41(H41), C2(H2), C32(H32),
 C34(H34), C14(H14), C16(H16), C33(H33), C17(H17), C15(H15)
2.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C)
;
_shelx_res_checksum              57774
_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 1.902
_oxdiff_exptl_absorpt_empirical_full_min 0.580