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_7717890
_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 H34 Cl O P Ru Si, 0.75[C6H14]'
_chemical_formula_sum            'C34.5 H44.5 Cl O P Ru Si'
_chemical_formula_weight         670.78
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-06-13
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-07-04 deposited with the CCDC.	2025-01-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.4670(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.7334(2)
_cell_length_b                   8.79540(10)
_cell_length_c                   19.4148(2)
_cell_measurement_reflns_used    28398
_cell_measurement_temperature    100.03
_cell_measurement_theta_max      77.5270
_cell_measurement_theta_min      4.8080
_cell_volume                     3016.06(6)
_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      100.03
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.974
_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    -66.00  29.00   0.50    1.00    --  -38.50  85.00-109.00  190
  2  \w     40.00 135.00   0.50    3.00    --  106.83 -85.00 130.00  190
  3  \w    101.00 174.00   0.50    3.00    --  106.83  85.00-109.00  146
  4  \w   -101.00 -27.00   0.50    1.00    --  -38.50 -57.00 150.00  148
  5  \w   -105.00 -35.00   0.50    1.00    --  -38.50 -38.00 -60.00  140
  6  \w   -108.00 -33.00   0.50    1.00    --  -38.50 -19.00   0.00  150
  7  \w    -17.00  52.00   0.50    1.00    --   49.06 -38.00-180.00  138
  8  \w    -14.00  61.00   0.50    1.00    --   49.06 -57.00  30.00  150
  9  \w     38.00 112.00   0.50    1.00    --   49.06  57.00 -30.00  148
 10  \w    -14.00  61.00   0.50    1.00    --   49.06 -57.00 -90.00  150
 11  \w    -10.00  77.00   0.50    1.00    --   49.06 -85.00 130.00  174
 12  \w    103.00 171.00   0.50    3.00    --  106.83  77.00 -60.00  136
 13  \w     44.00 112.00   0.50    3.00    --  106.83-125.00 150.00  136
 14  \w     39.00 110.00   0.50    3.00    --  106.83 -30.00 150.00  142
 15  \w    103.00 171.00   0.50    3.00    --  106.83  77.00 120.00  136
 16  \w    102.00 171.00   0.50    3.00    --  106.83  45.00-180.00  138
 17  \w    104.00 175.00   0.50    3.00    --  106.83  30.00  60.00  142
 18  \w     44.00 112.00   0.50    3.00    --  106.83-125.00-120.00  136
 19  \w     44.00 120.00   0.50    3.00    --  106.83 -61.00 -30.00  152
 20  \w     39.00 106.00   0.50    3.00    --  106.83 -94.00   0.00  134
 21  \w     94.00 170.00   0.50    3.00    --  106.83  61.00 -90.00  152
 22  \w     39.00 106.00   0.50    3.00    --  106.83 -94.00  90.00  134
 23  \w    102.00 171.00   0.50    3.00    --  106.83  45.00   0.00  138
 24  \w     97.00 170.00   0.50    3.00    --  106.83 125.00 150.00  146
 25  \w     42.00 111.00   0.50    3.00    --  106.83 -45.00-150.00  138
 26  \w     44.00 112.00   0.50    3.00    --  106.83-125.00-150.00  136
 27  \w     39.00 106.00   0.50    3.00    --  106.83 -94.00 -60.00  134
 28  \w     44.00 112.00   0.50    3.00    --  106.83-125.00 -30.00  136
 29  \w     63.00 110.00   0.50    3.00    --  106.83 -30.00-120.00   94
;
_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      -0.0533849000
_diffrn_orient_matrix_UB_12      0.0618996000
_diffrn_orient_matrix_UB_13      -0.0733021000
_diffrn_orient_matrix_UB_21      0.0674946000
_diffrn_orient_matrix_UB_22      0.0795017000
_diffrn_orient_matrix_UB_23      -0.0133780000
_diffrn_orient_matrix_UB_31      0.0143711000
_diffrn_orient_matrix_UB_32      -0.1432656000
_diffrn_orient_matrix_UB_33      -0.0390992000
_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  0.0592
_diffrn_reflns_av_unetI/netI     0.0310
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            39265
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.025
_diffrn_reflns_theta_min         4.642
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.104
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55286
_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 orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.477
_exptl_crystal_description       needle
_exptl_crystal_F_000             1398
_exptl_crystal_preparation       'As per the reaction scheme'
_exptl_crystal_recrystallization_method 'slow vapour diffusion'
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.262
_refine_diff_density_min         -1.124
_refine_diff_density_rms         0.201
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     321
_refine_ls_number_reflns         6279
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0700
_refine_ls_R_factor_gt           0.0675
_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^)+(0.1316P)^2^+17.6843P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2071
_refine_ls_wR_factor_ref         0.2106
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5920
_reflns_number_total             6279
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03550j2.cif
_cod_data_source_block           ska-ad-as-527
_cod_depositor_comments
'Adding full bibliography for 7717886--7717890.cif.'
_cod_original_formula_sum        'C34.50 H44.50 Cl O P Ru Si'
_cod_database_code               7717890
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         'C H P O Si Ru Cl'
_chemical_oxdiff_usercomment     'light orange block'
_shelx_estimated_absorpt_t_max   0.406
_shelx_estimated_absorpt_t_min   0.253
_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 Ternary CH refined with riding coordinates:
 C8(H8)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C12(H12), C13(H13), C14(H14), C15(H15),
 C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C24(H24), C25(H25), C26(H26),
  C27(H27), C28(H28)
2.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C29(H29A,H29B,H29C),
 C30(H30A,H30B,H30C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              78325
_shelx_fab_checksum              60597
_olex2_exptl_crystal_mounting_method 'Mounted on the 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 2.648
_oxdiff_exptl_absorpt_empirical_full_min 0.435