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_7717888
_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         'C20 H21 P Si'
_chemical_formula_sum            'C20 H21 P Si'
_chemical_formula_weight         320.43
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-05-31
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   7.49780(10)
_cell_length_b                   20.0084(2)
_cell_length_c                   24.0485(3)
_cell_measurement_reflns_used    23467
_cell_measurement_temperature    99.97
_cell_measurement_theta_max      77.2900
_cell_measurement_theta_min      4.2780
_cell_volume                     3607.73(8)
_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      99.97
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_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   -107.00 -35.00   0.50    1.00    --  -38.50 -29.00 -69.00  144
  2  \w    -19.00  53.00   0.50    1.00    --   49.06 -29.00 -69.00  144
  3  \w     46.00 117.00   0.50    1.00    --   49.06  29.00  91.00  142
  4  \w    104.00 175.00   0.50    4.00    --  106.83  29.00  91.00  142
  5  \w     39.00 110.00   0.50    4.00    --  106.83 -29.00 -69.00  142
  6  \w    -42.00  30.00   0.50    1.00    --  -38.50  29.00  91.00  144
  7  \w    -42.00  28.00   0.50    1.00    --  -38.50  38.00 150.00  140
  8  \w   -108.00 -33.00   0.50    1.00    --  -38.50 -19.00   0.00  150
  9  \w     28.00  98.00   0.50    1.00    --   49.06-125.00-150.00  140
 10  \w     28.00  98.00   0.50    1.00    --   49.06-125.00 -60.00  140
 11  \w     39.00 106.00   0.50    4.00    --  106.83 -94.00 150.00  134
 12  \w     44.00 112.00   0.50    4.00    --  106.83-125.00  30.00  136
 13  \w     44.00 112.00   0.50    4.00    --  106.83-125.00 -30.00  136
 14  \w    102.00 171.00   0.50    4.00    --  106.83  45.00 150.00  138
 15  \w    103.00 171.00   0.50    4.00    --  106.83  77.00  30.00  136
 16  \w     39.00 106.00   0.50    4.00    --  106.83 -94.00  60.00  134
 17  \w    108.00 134.00   0.50    4.00    --  106.83  77.00   0.00   52
 18  \w     77.00 106.00   0.50    4.00    --  106.83 -94.00-150.00   58
 19  \w     40.00 109.00   0.50    4.00    --  106.83 -30.00 150.00  138
 20  \w    105.00 157.00   0.50    4.00    --  106.83  30.00 120.00  104
 21  \w     78.00 112.00   0.50    4.00    --  106.83 -61.00 -60.00   68
 22  \w     51.00  84.00   0.50    4.00    --  106.83 -77.00 150.00   66
 23  \w     87.00 117.00   0.50    4.00    --  106.83 -77.00 150.00   60
 24  \w     53.00  88.00   0.50    4.00    --  106.83 -94.00 -90.00   70
 25  \w    137.00 168.00   0.50    4.00    --  106.83  77.00  90.00   62
 26  \w     43.00  82.00   0.50    4.00    --  106.83 -45.00 150.00   78
 27  \w     54.00 115.00   0.50    4.00    --  106.83 -61.00  30.00  122
 28  \w     97.00 129.00   0.50    4.00    --  106.83 125.00 -60.00   64
;
_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      0.0225848000
_diffrn_orient_matrix_UB_12      0.0709619000
_diffrn_orient_matrix_UB_13      -0.0237992000
_diffrn_orient_matrix_UB_21      -0.2041436000
_diffrn_orient_matrix_UB_22      0.0068101000
_diffrn_orient_matrix_UB_23      -0.0045543000
_diffrn_orient_matrix_UB_31      -0.0067975000
_diffrn_orient_matrix_UB_32      0.0290689000
_diffrn_orient_matrix_UB_33      0.0592980000
_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  0.0672
_diffrn_reflns_av_unetI/netI     0.0438
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            37246
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.822
_diffrn_reflns_theta_min         4.290
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.921
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57103
_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 white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.180
_exptl_crystal_description       block
_exptl_crystal_F_000             1360
_exptl_crystal_preparation       'As per reaction scheme'
_exptl_crystal_recrystallization_method 'vapour diffusion method'
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.370
_refine_diff_density_min         -0.451
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details
;
 Flack x determined using 2935 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.346(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         7507
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0391
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0459P)^2^+1.8005P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1002
_refine_ls_wR_factor_ref         0.1020
_reflns_Friedel_coverage         0.743
_reflns_Friedel_fraction_full    0.990
_reflns_Friedel_fraction_max     0.954
_reflns_number_gt                7167
_reflns_number_total             7507
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03550j2.cif
_cod_data_source_block           ska-ad-p-sih
_cod_depositor_comments
'Adding full bibliography for 7717886--7717890.cif.'
_cod_database_code               7717888
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         'C H P Si'
_chemical_oxdiff_usercomment     'white block'
_shelx_estimated_absorpt_t_max   0.656
_shelx_estimated_absorpt_t_min   0.545
_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.a Ternary CH refined with riding coordinates:
 Si1(H1), Si2(H2A)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12),
 C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C22(H22), C23(H23), C24(H24),
  C25(H25), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32), C34(H34),
 C35(H35), C36(H36), C37(H37), C38(H38)
2.c Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C39(H39A,H39B,H39C), C40(H40A,H40B,
 H40C)
;
_shelx_res_checksum              57451
_olex2_exptl_crystal_mounting_method 'mounted on a 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 1.694
_oxdiff_exptl_absorpt_empirical_full_min 0.677