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_7715669
_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 H44 Cl N5 P2 Ru, C H4 O, C4 H10 O'
_chemical_formula_sum            'C61 H58 Cl N5 O2 P2 Ru'
_chemical_formula_weight         1091.58
_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
_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                 93.432(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.1379(4)
_cell_length_b                   24.4204(6)
_cell_length_c                   17.1734(3)
_cell_measurement_reflns_used    20470
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.6710
_cell_measurement_theta_min      2.1770
_cell_volume                     5499.9(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                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0309
_diffrn_detector_type            Eos
_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    -45.00  49.00   0.50   28.00    --   18.09 -78.00-103.00  188
  2  \w    -45.00  11.00   0.50   28.00    --  -19.42 -78.00-103.00  112
  3  \w    -50.00  24.00   0.50   28.00    --  -19.42  78.00  21.00  148
  4  \w     35.00  94.00   0.50   28.00    --   18.09 178.00-150.00  118
  5  \w     -3.00  87.00   0.50   28.00    --   18.09  57.00-120.00  180
  6  \w    -63.00  54.00   0.50   28.00    --  -19.42  19.00-180.00  234
  7  \w    -49.00  41.00   0.50   28.00    --  -19.42  77.00 -90.00  180
;
_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      0.0344692000
_diffrn_orient_matrix_UB_12      -0.0182778000
_diffrn_orient_matrix_UB_13      -0.0168047000
_diffrn_orient_matrix_UB_21      -0.0009364000
_diffrn_orient_matrix_UB_22      0.0164344000
_diffrn_orient_matrix_UB_23      -0.0340609000
_diffrn_orient_matrix_UB_31      0.0417430000
_diffrn_orient_matrix_UB_32      0.0154548000
_diffrn_orient_matrix_UB_33      0.0163467000
_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  0.1022
_diffrn_reflns_av_unetI/netI     0.0635
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            56057
_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         26.021
_diffrn_reflns_theta_min         2.177
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.439
_exptl_absorpt_correction_T_max  0.934
_exptl_absorpt_correction_T_min  0.897
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2264
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.709
_refine_diff_density_min         -0.583
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     654
_refine_ls_number_reflns         10821
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0854
_refine_ls_R_factor_gt           0.0621
_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^)+(0.0683P)^2^+3.4231P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1546
_refine_ls_wR_factor_ref         0.1715
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7920
_reflns_number_total             10821
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00623b2.cif
_cod_data_source_block           aks258a1
_cod_depositor_comments
'Adding full bibliography for 7715668--7715671.cif.'
_cod_database_code               7715669
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C22 H15 N3 O2 P2 Cl2 Ru1'
_shelx_estimated_absorpt_t_max   0.917
_shelx_estimated_absorpt_t_min   0.869
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C4S(H4SA,H4SB), C3S(H3SA,H3SB)
2.b Aromatic/amide H refined with riding coordinates:
 C50(H50), C49(H49), C48(H48), C28(H28), C40(H40), C56(H56), C46(H46),
 C26(H26), C17(H17), C47(H47), C20(H20), C7(H7), C32(H32), C52(H52), C16(H16),
 C19(H19), C18(H18), C23(H23), C5(H5), C38(H38), C22(H22), C6(H6), C29(H29),
 C55(H55), C24(H24), C34(H34), C15(H15), C13(H13), C41(H41), C25(H25), C31(H31),
  C54(H54), C44(H44), C36(H36), C42(H42), C53(H53), C30(H30), C35(H35),
 C37(H37), C14(H14), C43(H43)
2.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C1S(H1SA,H1SB,H1SC), C2S(H2SA,H2SB,H2SC), C5S(H5SA,H5SB,
 H5SC)
2.d Idealised tetrahedral OH refined as rotating group:
 O1S(H1S)
;
_shelx_res_checksum              32520
_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
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 3.396
_oxdiff_exptl_absorpt_empirical_full_min 0.459