Hydrogenation and Silylation of a Double-Cyclometalated Ruthenium Complex: Structures and Dynamic Behavior of Hydrido and Hydridosilicate Ruthenium Complexes
Scherl, Peter; Wadepohl, Hubert; Gade, Lutz H.; Organometallics 32 (2013) 4409–; doi:10.1021/om400574a

data_4081181
_publ_section_title
;
 Hydrogenation and Silylation of a Double-Cyclometalated Ruthenium
 Complex: Structures and Dynamic Behavior of Hydrido and Hydridosilicate
 Ruthenium Complexes
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              4409
_journal_paper_doi               10.1021/om400574a
_journal_volume                  32
_journal_year                    2013
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C63 H64 N P3 Ru Si'
_chemical_formula_sum            'C63 H64 N P3 Ru Si'
_chemical_formula_weight         1057.22
_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'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_code                ga_ps24
_audit_creation_date
;
'Mon Jan 07 11:53:12 2013'
;
_audit_update_record             'Mon Jun 10 14:40:58 CEST 2013'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.90299(5)
_cell_length_b                   19.06264(8)
_cell_length_c                   22.67018(10)
_cell_measurement_reflns_used    250435
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      32.1510
_cell_measurement_theta_min      3.5190
_cell_volume                     5143.92(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
'encif (Wadepohl, 2009-13); encifer 1.4 (CCDC, 2011)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_diffrn_ambient_temperature      110(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9621
_diffrn_detector_type            'Agilent EOS'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
  1 omega   -1.00   96.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026   77.0000 -180.0000 194

  2 omega    6.00   97.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026   57.0000  -60.0000 182

  3 omega  -34.00   60.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026  -77.0000  -30.0000 188

  4 omega  -36.00   61.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026  -79.0000   65.0000 194

  5 omega   -2.00   96.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026   77.0000   90.0000 196

  6 omega   -4.00   45.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026   77.0000  -30.0000 98

  7 omega   48.00   74.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026   77.0000  -30.0000 52

  8 omega  -36.00   61.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026  -79.0000 -114.0000 194

  9 omega    1.00   78.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026   38.0000   60.0000 154

 10 omega  -40.00   57.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026  -77.0000 -180.0000 194

 11 omega  -99.00    4.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.0026  -77.0000  -60.0000 206

 12 omega  -60.00  -23.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.0026   77.0000 -180.0000 74

 13 omega  -41.00   50.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026  -57.0000   30.0000 182

 14 omega  -41.00   50.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026  -57.0000  -90.0000 182

 15 omega    1.00  101.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026   38.0000   90.0000 200

 16 omega  -41.00   50.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026  -57.0000  120.0000 182

 17 omega  -60.00  -34.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.0026   77.0000    0.0000 52

 18 omega  -35.00   -9.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.0026  -77.0000 -180.0000 52

 19 omega  -35.00   -9.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.0026  -79.0000   -9.0000 52

 20 omega  -31.00   -5.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.0026  -79.0000 -114.0000 52

 21 omega   16.00   42.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026   57.0000  -90.0000 52

 22 omega   12.00   38.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026   38.0000  -90.0000 52

 23 omega   33.00   59.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026  -77.0000   30.0000 52

 24 omega  -37.00  -11.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026  -77.0000   30.0000 52

 25 omega   35.00   61.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026  -79.0000  170.0000 52

 26 omega    5.00   55.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026   19.0000  -30.0000 100

 27 omega   33.00   59.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026  -77.0000  -60.0000 52

 28 omega    3.00   72.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026   38.0000 -150.0000 138

 29 phi    120.00  146.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
  28.0026   28.0026   40.0000     -     52

 30 omega   35.00   60.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026  -77.0000   90.0000 50

 31 omega -102.00   46.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.0026    0.0000  120.0000 296

 32 omega  -46.00    4.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.0026  -79.0000 -114.0000 100

 33 omega -102.00   46.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.0026    0.0000  240.0000 296

 34 omega -102.00   46.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.0026    0.0000    0.0000 296

 35 omega  -46.00    4.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.0026  -79.0000   -9.0000 100

 36 omega  -43.00   60.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026  -77.0000  -60.0000 206

 37 omega  -46.00  102.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026    0.0000  240.0000 296

 38 omega  -43.00   61.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026  -79.0000  170.0000 208

 39 omega  -46.00  102.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026    0.0000  120.0000 296

 40 omega  -46.00  102.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026    0.0000    0.0000 296

 41 omega  -21.00  102.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026   19.0000   60.0000 246

 42 omega   -4.00   99.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026   77.0000 -150.0000 206

 43 omega  -43.00   60.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026  -77.0000   90.0000 206

 44 omega  -21.00  102.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026   19.0000 -150.0000 246

 45 omega  -21.00  102.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026   19.0000 -180.0000 246

 46 omega  -43.00   60.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026  -77.0000    0.0000 206

 47 omega  -21.00  102.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026   19.0000 -120.0000 246

 48 omega  -21.00  102.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026   19.0000  -90.0000 246

 49 omega  -21.00  102.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026   19.0000  -60.0000 246

 50 omega  -21.00  102.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026   19.0000  -30.0000 246

 51 omega  -21.00  102.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026   19.0000    0.0000 246

 52 omega  -21.00  102.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026   19.0000   30.0000 246

 53 omega    6.00   97.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026   57.0000  -90.0000 182

 54 omega    1.00  101.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026   38.0000 -180.0000 200

 55 omega  -21.00  102.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026   19.0000  120.0000 246

 56 omega  -21.00  102.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026   19.0000  150.0000 246

 57 omega  -46.00   15.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026  -19.0000 -180.0000 122

 58 omega  -21.00   -3.50   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026   19.0000   90.0000 35

;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w and \p scans'
_diffrn_measurement_specimen_support 'polyimid foil'
_diffrn_orient_matrix_UB_11      -0.0058764000
_diffrn_orient_matrix_UB_12      -0.0316942000
_diffrn_orient_matrix_UB_13      -0.0160920000
_diffrn_orient_matrix_UB_21      -0.0333204000
_diffrn_orient_matrix_UB_22      0.0176782000
_diffrn_orient_matrix_UB_23      -0.0212593000
_diffrn_orient_matrix_UB_31      0.0490538000
_diffrn_orient_matrix_UB_32      0.0081922000
_diffrn_orient_matrix_UB_33      -0.0163782000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0960
_diffrn_reflns_av_unetI/netI     0.0283
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            614554
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.381
_diffrn_reflns_theta_min         3.193
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.464
_exptl_absorpt_correction_T_max  0.977
_exptl_absorpt_correction_T_min  0.906
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_description       needle
_exptl_crystal_F_000             2208
_exptl_crystal_size_max          0.2619
_exptl_crystal_size_mid          0.1085
_exptl_crystal_size_min          0.0553
_refine_diff_density_max         0.646
_refine_diff_density_min         -0.708
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details
;
 Flack x determined using 7512 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.020(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     630
_refine_ls_number_reflns         18157
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0274
_refine_ls_R_factor_gt           0.0243
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0332P)^2^+0.4446P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0547
_refine_ls_wR_factor_ref         0.0553
_reflns_Friedel_coverage         0.830
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.980
_reflns_number_gt                17253
_reflns_number_total             18157
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om400574a_si_002.cif
_cod_data_source_block           ga_ps24
_cod_database_code               4081181
_audit_block_refno               1673
_audit_block_usercomment         'PS409, needle, yellow'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Ternary CH refined with riding coordinates:
 C4(H4), C7(H7), C20(H20), C23(H23), C36(H36), C39(H39)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C5(H5A,H5B), C6(H6A,H6B), C21(H21A,
 H21B), C22(H22A,H22B), C37(H37A,H37B), C38(H38A,H38B)
2.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C12(H12), C13(H13), C15(H15), C16(H16), C17(H17),
 C18(H18), C19(H19), C25(H25), C26(H26), C27(H27), C28(H28), C29(H29), C31(H31),
  C32(H32), C33(H33), C34(H34), C35(H35), C41(H41), C42(H42), C43(H43),
 C44(H44), C45(H45), C48(H48), C49(H49), C50(H50), C51(H51), C53(H53), C54(H54),
  C55(H55), C56(H56), C57(H57), C59(H59), C60(H60), C61(H61), C62(H62), C63(H63)
;
_shelx_estimated_absorpt_t_max   0.955
_shelx_estimated_absorpt_t_min   0.955
_shelx_hkl_checksum              94561
_cell_oxdiff_length_a            11.90282(8)
_cell_oxdiff_length_b            19.06502(12)
_cell_oxdiff_length_c            22.66766(14)
_cell_oxdiff_angle_alpha         90.0010(5)
_cell_oxdiff_angle_beta          89.9852(5)
_cell_oxdiff_angle_gamma         89.9759(5)
_cell_oxdiff_volume              5143.92(6)
_cell_oxdiff_measurement_reflns_used 250417
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_theta     30.44
_reflns_odcompleteness_iscentric 1