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_7717889
_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 Cl O P Ru Si, C H2 Cl2, Cl'
_chemical_formula_sum            'C31 H37 Cl4 O P Ru Si'
_chemical_formula_weight         727.53
_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             2023-10-27
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-07-04 deposited with the CCDC.	2025-01-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.060(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6049(2)
_cell_length_b                   23.5234(4)
_cell_length_c                   13.4560(2)
_cell_measurement_reflns_used    21330
_cell_measurement_temperature    250(6)
_cell_measurement_theta_max      77.7420
_cell_measurement_theta_min      3.7670
_cell_volume                     3343.70(10)
_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      250(6)
_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 0.9809
_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   -101.00 -25.00   0.50    0.50    --  -38.50 -62.00 -66.00  152
  2  \w    -52.00  24.00   0.50    0.50    --  -38.50  62.00  70.00  152
  3  \w     36.00 112.00   0.50    0.50    --   49.56  62.00  70.00  152
  4  \w    -13.00  63.00   0.50    0.50    --   49.56 -62.00 -66.00  152
  5  \w     45.00 121.00   0.50    1.00    --  107.46 -62.00 -66.00  152
  6  \w     94.00 170.00   0.50    1.00    --  107.46  62.00  70.00  152
  7  \w   -101.00 -27.00   0.50    0.50    --  -38.50 -57.00-150.00  148
  8  \w     46.00 116.00   0.50    0.50    --   49.56  37.00-180.00  140
  9  \w    104.00 176.00   0.50    1.00    --  107.46  30.00   0.00  144
 10  \w     45.00 113.00   0.50    1.00    --  107.46-125.00   0.00  136
 11  \w    103.00 172.00   0.50    1.00    --  107.46  77.00  90.00  138
 12  \w     39.00 111.00   0.50    1.00    --  107.46 -30.00 -60.00  144
 13  \w    104.00 176.00   0.50    1.00    --  107.46  30.00 -30.00  144
 14  \w     97.00 170.00   0.50    1.00    --  107.46 125.00   0.00  146
 15  \w     39.00 111.00   0.50    1.00    --  107.46 -30.00 120.00  144
 16  \w     45.00  71.00   0.50    1.00    --  107.46 -45.00   0.00   52
 17  \w     85.00 111.00   0.50    1.00    --  107.46 -45.00   0.00   52
 18  \w     55.00 107.00   0.50    1.00    --  107.46 -94.00-150.00  104
 19  \w     39.00 104.00   0.50    1.00    --  107.46 -94.00 150.00  130
;
_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      -0.0064647000
_diffrn_orient_matrix_UB_12      0.0474381000
_diffrn_orient_matrix_UB_13      -0.0792285000
_diffrn_orient_matrix_UB_21      0.1456800000
_diffrn_orient_matrix_UB_22      0.0019019000
_diffrn_orient_matrix_UB_23      0.0062572000
_diffrn_orient_matrix_UB_31      -0.0005528000
_diffrn_orient_matrix_UB_32      -0.0451122000
_diffrn_orient_matrix_UB_33      -0.0830366000
_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  0.0541
_diffrn_reflns_av_unetI/netI     0.0343
_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       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            26806
_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         78.290
_diffrn_reflns_theta_min         3.796
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.707
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.27494
_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 orangish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.445
_exptl_crystal_description       block
_exptl_crystal_F_000             1488
_exptl_crystal_preparation       'As per the reaction scheme'
_exptl_crystal_recrystallization_method 'Slow vapour diffusion'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.612
_refine_diff_density_min         -1.938
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         7026
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0496
_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^)+(0.0860P)^2^+4.1191P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1293
_refine_ls_wR_factor_ref         0.1310
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6640
_reflns_number_total             7026
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03550j2.cif
_cod_data_source_block           sjp-as-385_auto
_cod_depositor_comments
'Adding full bibliography for 7717886--7717890.cif.'
_cod_database_code               7717889
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         'C H P Si Ru Cl '
_chemical_oxdiff_usercomment     'RED BLOCK'
_shelx_estimated_absorpt_t_max   0.239
_shelx_estimated_absorpt_t_min   0.206
_diffrn_oxdiff_digest_frames
;
01aa366fa75c17d5cdfe5c05897a7a0c2b00030fe0f
;
_diffrn_oxdiff_digest_hkl
;
010b2e07857e2120f867fba7199002ca5264f1
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C28(H28)
2.b Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C10(H10), C11(H11), C12(H12), C13(H13),
 C14(H14), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C22(H22), C23(H23),
  C25(H25), C26(H26)
2.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C),
 C30(H30A,H30B,H30C)
2.e Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_shelx_res_checksum              72924
_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 2.147
_oxdiff_exptl_absorpt_empirical_full_min 0.622