Cationic and neutral ruthenium(II) complexes bearing silyl-phosphines: synthesis, structures, and catalytic studies in selective hydroboration of carbonyl compounds.
Sahoo, Amiya Kumar; Dash, Rageshree; Agrawalla, Suraj Kumar; Purohit, Chandra Shekhar; Doddi, Adinarayana; Dalton transactions (Cambridge, England : 2003) 54 (2025) 4312–4323; doi:10.1039/d4dt03550j

data_7717886
_publ_section_title
;
 Cationic and neutral ruthenium(II) complexes bearing silyl-phosphines:
 synthesis, structures, and catalytic studies in selective hydroboration
 of carbonyl compounds.
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4312
_journal_page_last               4323
_journal_paper_doi               10.1039/d4dt03550j
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C30 H35 Cl2 P Ru Si'
_chemical_formula_sum            'C30 H35 Cl2 P Ru Si'
_chemical_formula_weight         626.61
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-09-24
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-09-27 deposited with the CCDC.	2025-01-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.7686(2)
_cell_length_b                   27.1132(6)
_cell_length_c                   12.3737(3)
_cell_measurement_reflns_used    6555
_cell_measurement_temperature    99.98
_cell_measurement_theta_max      75.1420
_cell_measurement_theta_min      4.7930
_cell_volume                     3277.27(13)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.98
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.9853
_diffrn_measured_fraction_theta_max 0.8344
_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    -54.00   3.00   0.50    4.00    --  -38.50  65.00 -49.00  114
  2  \w    -66.00 -23.00   0.50    4.00    --  -38.50 -65.00 174.00   86
  3  \w     73.00  98.00   0.50    4.00    --   49.06  65.00 -49.00   50
  4  \w     32.00  65.00   0.50    4.00    --   49.06 -65.00 174.00   66
  5  \w     68.00 121.00   0.50   16.00    --  106.83 -65.00 174.00  106
  6  \w    112.00 166.00   0.50   16.00    --  106.83  65.00 -49.00  108
  7  \w    -39.00  22.00   0.50    4.00    --  -38.50  37.00-150.00  122
  8  \w     46.00  95.00   0.50    4.00    --   49.06  37.00  30.00   98
  9  \w     29.00  91.00   0.50    4.00    --   49.06-125.00-180.00  124
 10  \w     49.00 109.00   0.50   16.00    --  106.83-125.00-150.00  120
 11  \w     82.00 109.00   0.50   16.00    --  106.83-125.00  90.00   54
 12  \w    108.00 169.00   0.50   16.00    --  106.83  45.00  30.00  122
 13  \w     44.00  78.00   0.50   16.00    --  106.83-125.00  90.00   68
 14  \w     47.00  72.00   0.50   16.00    --  106.83 -94.00  30.00   50
 15  \w     42.00 110.00   0.50   16.00    --  106.83 -45.00 -90.00  136
 16  \w    102.00 152.00   0.50   16.00    --  106.83  61.00-120.00  100
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Dual, Cu at home/near, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0197046000
_diffrn_orient_matrix_UB_12      0.0453441000
_diffrn_orient_matrix_UB_13      0.1111627000
_diffrn_orient_matrix_UB_21      -0.0420617000
_diffrn_orient_matrix_UB_22      0.0790336000
_diffrn_orient_matrix_UB_23      -0.0558764000
_diffrn_orient_matrix_UB_31      -0.0327212000
_diffrn_orient_matrix_UB_32      -0.1287136000
_diffrn_orient_matrix_UB_33      0.0049146000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0679
_diffrn_reflns_av_unetI/netI     0.0612
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14237
_diffrn_reflns_point_group_measured_fraction_full 0.890
_diffrn_reflns_point_group_measured_fraction_max 0.845
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.825
_diffrn_reflns_theta_min         4.812
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.292
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75081
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.270
_exptl_crystal_description       block
_exptl_crystal_F_000             1288
_exptl_crystal_preparation       'As per the reaction scheme'
_exptl_crystal_recrystallization_method 'Vapour diffusion method'
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.441
_refine_diff_density_min         -1.427
_refine_diff_density_rms         0.158
_refine_ls_abs_structure_details
;
 Flack x determined using 1896 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.077(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         5911
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0793
_refine_ls_R_factor_gt           0.0746
_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^)+(0.1057P)^2^+14.9026P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1957
_refine_ls_wR_factor_ref         0.1995
_reflns_Friedel_coverage         0.688
_reflns_Friedel_fraction_full    0.786
_reflns_Friedel_fraction_max     0.723
_reflns_number_gt                5419
_reflns_number_total             5911
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03550j3.cif
_cod_data_source_block           ska-ad-as-589
_cod_depositor_comments
'Adding full bibliography for 7717886--7717890.cif.'
_cod_database_code               7717886
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         'C H Si P Ru Cl'
_chemical_oxdiff_usercomment     'light red block'
_shelx_estimated_absorpt_t_max   0.338
_shelx_estimated_absorpt_t_min   0.292
_diffrn_oxdiff_ac3_digest_hkl    41dca9d871ac70f080771e58cbdf2df562ac03
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All Si(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C5) = Uanis(C4)
3.a Ternary CH refined with riding coordinates:
 Si1(H1), C7(H7)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C13(H13), C14(H14), C15(H15), C16(H16),
 C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C24(H24), C25(H25), C26(H26),
  C27(H27), C28(H28)
3.c Idealised Me refined as rotating group:
 C8(H8a,H8b,H8c), C9(H9a,H9b,H9c), C10(H10a,H10b,H10c), C29(H29a,H29b,H29c),
 C30(H30a,H30b,H30c)
;
_shelx_res_checksum              40432
_olex2_exptl_crystal_mounting_method 'Mounted on a nylon loop'
_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 2.597
_oxdiff_exptl_absorpt_empirical_full_min 0.665