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_7715671
_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         'C56 H45 Cl N5 P2 Ru, Cl, C2 H6 O S'
_chemical_formula_sum            'C58 H51 Cl2 N5 O P2 Ru S'
_chemical_formula_weight         1100.01
_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             2022-09-28
_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                 101.886(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.7331(3)
_cell_length_b                   23.3559(8)
_cell_length_c                   23.4710(8)
_cell_measurement_reflns_used    9410
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.5480
_cell_measurement_theta_min      3.1680
_cell_volume                     5221.2(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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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     11.00  85.00   1.00   20.00    --   18.01-140.00 137.00   74
  2  \w      6.00  79.00   1.00   20.00    --   18.01-130.00 -48.00   73
  3  \w    -80.00 -27.00   1.00   20.00    --  -19.26 130.00  23.00   53
  4  \w    -86.00 -32.00   1.00   20.00    --  -19.26 140.00-162.00   54
  5  \w     -8.00  90.00   1.00   20.00    --   18.01  37.00   0.00   98
  6  \w     35.00  94.00   1.00   20.00    --   18.01 178.00  90.00   59
  7  \w     35.00  94.00   1.00   20.00    --   18.01 178.00-120.00   59
  8  \w    -51.00  39.00   1.00   20.00    --   18.01 -57.00 -90.00   90
  9  \w    -55.00  62.00   1.00   20.00    --   18.01 -19.00 150.00  117
 10  \w     -3.00  87.00   1.00   20.00    --   18.01  57.00  90.00   90
 11  \w     -3.00  87.00   1.00   20.00    --   18.01  57.00 -90.00   90
 12  \w    -12.00  88.00   1.00   20.00    --   18.01  77.00 150.00  100
 13  \w    -12.00  25.00   1.00   20.00    --   18.01  77.00 -30.00   37
 14  \w     -3.00  87.00   1.00   20.00    --   18.01  57.00-150.00   90
;
_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      0.0175240000
_diffrn_orient_matrix_UB_12      0.0194650000
_diffrn_orient_matrix_UB_13      0.0235820000
_diffrn_orient_matrix_UB_21      0.0290538000
_diffrn_orient_matrix_UB_22      0.0190294000
_diffrn_orient_matrix_UB_23      -0.0179136000
_diffrn_orient_matrix_UB_31      -0.0662867000
_diffrn_orient_matrix_UB_32      0.0134738000
_diffrn_orient_matrix_UB_33      -0.0087600000
_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  0.2046
_diffrn_reflns_av_unetI/netI     0.1057
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            95237
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.026
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         3.031
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.550
_exptl_absorpt_correction_T_max  0.989
_exptl_absorpt_correction_T_min  0.967
_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    1.399
_exptl_crystal_description       prism
_exptl_crystal_F_000             2264
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.644
_refine_diff_density_min         -0.841
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     634
_refine_ls_number_reflns         9224
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.1229
_refine_ls_R_factor_gt           0.0683
_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^)+(0.0391P)^2^+12.0341P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1325
_refine_ls_wR_factor_ref         0.1551
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5757
_reflns_number_total             9224
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00623b2.cif
_cod_data_source_block           aks256ca14
_cod_depositor_comments
'Adding full bibliography for 7715668--7715671.cif.'
_cod_database_code               7715671
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N O Cl2 P2 S1 Ru1'
_shelx_estimated_absorpt_t_max   0.978
_shelx_estimated_absorpt_t_min   0.912
_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
2.a Aromatic/amide H refined with riding coordinates:
 N1(H1), C38(H38), C52(H52), C28(H28), C13(H13), C17(H17), C20(H20), C5(H5),
 C14(H14), C18(H18), C7(H7), C50(H50), C19(H19), C32(H32), C15(H15), C34(H34),
 C6(H6), C31(H31), C44(H44), C30(H30), C29(H29), C37(H37), C35(H35), C26(H26),
 C49(H49), C24(H24), C36(H36), C46(H46), C43(H43), C23(H23), C53(H53), C22(H22),
  C40(H40), C56(H56), C16(H16), C54(H54), C48(H48), C25(H25), C55(H55),
 C41(H41), C42(H42), C47(H47)
2.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C2S(H2SA,H2SB,H2SC), C1S(H1SA,H1SB,H1SC)
;
_shelx_res_checksum              97873
_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 2.241
_oxdiff_exptl_absorpt_empirical_full_min 0.460