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_7715668
_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, [+ solvents]'
_chemical_formula_sum            'C56 H44 Cl N5 P2 Ru'
_chemical_formula_weight         985.42
_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             2022-09-28
_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                 114.968(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.6067(2)
_cell_length_b                   18.5906(2)
_cell_length_c                   19.4595(3)
_cell_measurement_reflns_used    31670
_cell_measurement_temperature    300
_cell_measurement_theta_max      29.0380
_cell_measurement_theta_min      2.3890
_cell_volume                     5446.24(15)
_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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      300
_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 0.926
_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    -25.00  25.10   0.30   17.00    --   18.09 -95.00 163.00  167
  2  \w    -47.00 -20.90   0.30   17.00    --  -19.42  95.00 -85.00   87
  3  \w      4.00  44.20   0.30   17.00    --   18.09  77.00 -30.00  134
  4  \w    -36.00  37.20   0.30   17.00    --   18.09 -57.00-150.00  244
  5  \w     34.00  91.00   0.30   17.00    --   18.09  37.00  30.00  190
  6  \w     43.00  91.00   0.30   17.00    --   18.09  37.00 -60.00  160
  7  \w     62.00  87.20   0.30   17.00    --   18.09  77.00 -30.00   84
  8  \w    -19.00  59.00   0.30   17.00    --   18.09 -99.00  90.00  260
  9  \w    -11.00  25.00   0.30   17.00    --   18.09  77.00-150.00  120
 10  \w     30.00  58.80   0.30   17.00    --   18.09 -99.00 -60.00   96
 11  \w    -29.00  -2.00   0.30   17.00    --  -19.42  37.00-180.00   90
 12  \w    -39.00  47.10   0.30   17.00    --  -19.42  57.00 -30.00  287
 13  \w     17.00  51.80   0.30   17.00    --  -19.42  37.00-180.00  116
;
_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      0.0304532000
_diffrn_orient_matrix_UB_12      -0.0280488000
_diffrn_orient_matrix_UB_13      0.0035699000
_diffrn_orient_matrix_UB_21      -0.0198054000
_diffrn_orient_matrix_UB_22      -0.0215468000
_diffrn_orient_matrix_UB_23      0.0187697000
_diffrn_orient_matrix_UB_31      -0.0299935000
_diffrn_orient_matrix_UB_32      -0.0142707000
_diffrn_orient_matrix_UB_33      -0.0353834000
_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  0.0468
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.926
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            67182
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.926
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.183
_diffrn_reflns_theta_min         1.741
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.434
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.495
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.202
_exptl_crystal_description       block
_exptl_crystal_F_000             2024
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.541
_refine_diff_density_min         -0.611
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     587
_refine_ls_number_reflns         13643
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0324
_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^)+(0.0355P)^2^+1.6195P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0804
_refine_ls_wR_factor_ref         0.0857
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11526
_reflns_number_total             13643
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00623b2.cif
_cod_data_source_block           aks259a1
_cod_depositor_comments
'Adding full bibliography for 7715668--7715671.cif.'
_cod_database_code               7715668
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N O'
_shelx_estimated_absorpt_t_max   0.930
_shelx_estimated_absorpt_t_min   0.835
_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:
 C7(H7), C44(H44), C32(H32), C5(H5), C22(H22), C34(H34), C6(H6), C16(H16),
 C43(H43), C52(H52), C38(H38), C28(H28), C17(H17), C50(H50), C13(H13), C26(H26),
  C46(H46), C35(H35), C23(H23), C40(H40), C56(H56), C15(H15), C42(H42),
 C14(H14), C31(H31), C36(H36), C24(H24), C49(H49), C20(H20), C18(H18), C55(H55),
  C25(H25), C29(H29), C30(H30), C41(H41), C37(H37), C19(H19), C48(H48),
 C54(H54), C47(H47), C53(H53)
2.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              2250
_shelx_fab_checksum              9087
_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 2.734
_oxdiff_exptl_absorpt_empirical_full_min 0.601