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_7717887
_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         'C33 H40 Cl N P Ru Si, C3 H3, F6 P'
_chemical_formula_sum            'C36 H43 Cl F6 N P2 Ru Si'
_chemical_formula_weight         830.26
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-05-18
_audit_creation_method
;
Olex2 1.5
(compiled 2023.02.24 svn.rf166f9f3 for OlexSys, GUI svn.r6725)
;
_audit_update_record
;
2024-07-04 deposited with the CCDC.	2025-01-21 downloaded from the CCDC.
;
_cell_angle_alpha                92.9040(10)
_cell_angle_beta                 94.8830(10)
_cell_angle_gamma                102.109(2)
_cell_formula_units_Z            2
_cell_length_a                   9.6071(2)
_cell_length_b                   13.6074(2)
_cell_length_c                   15.4123(3)
_cell_measurement_reflns_used    28336
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      77.7500
_cell_measurement_theta_min      4.2080
_cell_volume                     1957.97(6)
_computing_cell_refinement       'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.9994
_diffrn_measured_fraction_theta_max 0.6944
_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    -15.00  73.00   0.50    0.20    --   49.31 -78.00  30.00  176
  2  \w     43.00 131.00   0.50    0.40    --  107.46 -78.00  30.00  176
  3  \w    103.00 172.00   0.50    0.40    --  107.46  78.00 155.00  138
  4  \w    -50.00  24.00   0.50    0.20    --  -38.50  57.00 120.00  148
  5  \w   -101.00 -23.00   0.50    0.20    --  -38.50 -65.00  17.29  156
  6  \w   -101.00 -26.00   0.50    0.20    --  -38.50 -59.00 -81.45  150
  7  \w    -62.00  26.00   0.50    0.20    --  -38.50  78.00 155.00  176
  8  \w    -42.00  28.00   0.50    0.20    --  -38.50  37.00-120.00  140
  9  \w    -13.00  61.00   0.50    0.20    --   49.31 -57.00-120.00  148
 10  \w     46.00 116.00   0.50    0.20    --   49.31  37.00-180.00  140
 11  \w    -13.00  61.00   0.50    0.20    --   49.31 -57.00  30.00  148
 12  \w    101.00 171.00   0.50    0.40    --  107.46  72.00 139.51  140
 13  \w     45.00 113.00   0.50    0.40    --  107.46-125.00-120.00  136
 14  \w     43.00 112.00   0.50    0.40    --  107.46 -45.00  90.00  138
 15  \w     43.00 112.00   0.50    0.40    --  107.46 -45.00   0.00  138
 16  \w     39.00 107.00   0.50    0.40    --  107.46 -94.00 120.00  136
 17  \w    103.00 172.00   0.50    0.40    --  107.46  77.00  60.00  138
 18  \w    103.00 172.00   0.50    0.40    --  107.46  77.00  90.00  138
 19  \w     45.00 113.00   0.50    0.40    --  107.46-125.00   0.00  136
 20  \w     39.00 116.00   0.50    0.40    --  107.46 -15.00 -30.00  154
 21  \w     39.00 107.00   0.50    0.40    --  107.46 -94.00  60.00  136
 22  \w     45.00 121.00   0.50    0.40    --  107.46 -61.00  90.00  152
 23  \w    104.00 176.00   0.50    0.40    --  107.46  30.00 -60.00  144
 24  \w    103.00 172.00   0.50    0.40    --  107.46  45.00 -90.00  138
 25  \w     39.00 137.00   0.50    0.40    --  107.46 -88.00-168.43  196
 26  \w    104.00 176.00   0.50    0.40    --  107.46  30.00   0.00  144
 27  \w    103.00 172.00   0.50    0.40    --  107.46  77.00 120.00  138
 28  \w     45.00 121.00   0.50    0.40    --  107.46 -61.00-180.00  152
 29  \w     45.00 113.00   0.50    0.40    --  107.46-125.00  30.00  136
 30  \w     39.00 107.00   0.50    0.40    --  107.46 -94.00 -90.00  136
 31  \w     39.00 107.00   0.50    0.40    --  107.46 -94.00   0.00  136
 32  \w     45.00 113.00   0.50    0.40    --  107.46-125.00 -60.00  136
 33  \w     39.00 110.00   0.50    0.40    --  107.46 -30.00 150.00  142
;
_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      -0.0276300000
_diffrn_orient_matrix_UB_12      -0.1153327000
_diffrn_orient_matrix_UB_13      0.0036617000
_diffrn_orient_matrix_UB_21      0.0724213000
_diffrn_orient_matrix_UB_22      -0.0080436000
_diffrn_orient_matrix_UB_23      -0.0847248000
_diffrn_orient_matrix_UB_31      0.1454319000
_diffrn_orient_matrix_UB_32      0.0103922000
_diffrn_orient_matrix_UB_33      0.0540603000
_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  0.0614
_diffrn_reflns_av_unetI/netI     0.0425
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            31178
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.375
_diffrn_reflns_theta_min         4.251
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.403
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43874
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.89a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_description       block
_exptl_crystal_F_000             850
_exptl_crystal_preparation       'As per the reaction scheme'
_exptl_crystal_recrystallization_method 'Slow vapour diffusion'
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.21
_refine_diff_density_max         2.426
_refine_diff_density_min         -2.103
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     440
_refine_ls_number_reflns         8210
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0467
_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^)+(0.0827P)^2^+3.3361P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1248
_refine_ls_wR_factor_ref         0.1252
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8153
_reflns_number_total             8210
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03550j2.cif
_cod_data_source_block           sjp-as-239_auto
_cod_depositor_comments
'Adding full bibliography for 7717886--7717890.cif.'
_cod_database_code               7717887
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         'C H Cl F P Ru Si'
_chemical_oxdiff_usercomment     'LIGHT YELLOW BLOCK'
_shelx_estimated_absorpt_t_max   0.397
_shelx_estimated_absorpt_t_min   0.303
_diffrn_oxdiff_ac3_digest_hkl    01d97422695f4cdaaddc0e867a318994ca3718
_diffrn_oxdiff_digest_frames
;
01e5cd394976855ab47bf1905c84c7422f00046fca3
;
_diffrn_oxdiff_digest_hkl
;
01f3d3ac189f75e1a2a452e4ddcc0e1d2572b9
;
_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:
 C29(H29)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C11(H11), C12(H12), C13(H13), C14(H14),
 C15(H15), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C24(H24), C25(H25),
  C27(H27), C28(H28), C34(H34), C35(H35), C36(H36)
2.c Idealised Me refined as rotating group:
 C7(H7a,H7b,H7c), C8(H8a,H8b,H8c), C9(H9a,H9b,H9c), C22(H22a,H22b,H22c),
 C30(H30a,H30b,H30c), C31(H31a,H31b,H31c), C33(H33a,H33b,H33c)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              1388
_shelx_fab_checksum              2907
_olex2_exptl_crystal_mounting_method 'Mounted on the 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 1.453
_oxdiff_exptl_absorpt_empirical_full_min 0.644