Synthesis, Structure, and Reactivity of Trigonal Bipyramidal Ruthenium(IV) Trialkyl Complexes
Kwan Huang, Enrique; Cheung, Wai-Man; Chan, Sharon Lai-Fung; Sung, Herman H. Y.; Williams, Ian D.; Leung, Wa-Hung; Organometallics 32 (2013) 4483–; doi:10.1021/om400183n

data_4081220
_publ_section_title
;
 Synthesis, Structure, and Reactivity of Trigonal Bipyramidal
 Ruthenium(IV) Trialkyl Complexes
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              4483
_journal_paper_doi               10.1021/om400183n
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety      'C31 H48 N P Ru S Si3, 1/8(C4 H8 O), 1/8(C6 H14)'
_chemical_formula_sum            'C32.25 H50.75 N O0.125 P Ru S Si3'
_chemical_formula_weight         702.83
_chemical_name_systematic
;
 ? 
;
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-02-15
_audit_creation_method
;
  Olex2 1.2-beta
  (compiled Jan 17 2012 15:45:47, GUI svn.r4036)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 96.252(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.1717(8)
_cell_length_b                   19.8722(7)
_cell_length_c                   20.4513(7)
_cell_measurement_reflns_used    4355
_cell_measurement_temperature    173.00(14)
_cell_measurement_theta_max      71.7572
_cell_measurement_theta_min      3.1283
_cell_volume                     8149.3(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_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
;
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_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173.00(14)
_diffrn_detector_area_resol_mean 15.9578
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_details
;
  1 omega   44.00   72.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000   30.0000 28

  2 omega  -26.00   68.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   38.0000  -90.0000 94

  3 omega -122.00  -86.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -55.0000 -153.0000 -146.0000 36

  4 omega   92.00  122.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000  121.0000  -84.0000 30

  5 omega  -71.00    7.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000   38.0000  120.0000 78

  6 omega -136.00  -30.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000    0.0000   90.0000 106

  7 omega   38.00   71.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -38.0000  120.0000 33

  8 omega   40.00   79.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -50.0000  -90.0000 39

  9 omega   76.00  177.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   25.0000    0.0000 101

 10 omega   54.00   83.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -50.0000  -60.0000 29

 11 omega   37.00   72.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000   60.0000 35

 12 omega   41.00   71.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -38.0000   90.0000 30

 13 omega   38.00   70.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -38.0000  -30.0000 32

 14 omega   89.00  177.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   64.0000   60.0000 88
;
_diffrn_measurement_device       'kappa diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0319253000
_diffrn_orient_matrix_UB_12      -0.0506677000
_diffrn_orient_matrix_UB_13      -0.0440955000
_diffrn_orient_matrix_UB_21      -0.0415924000
_diffrn_orient_matrix_UB_22      0.0294585000
_diffrn_orient_matrix_UB_23      -0.0610045000
_diffrn_orient_matrix_UB_31      0.0562656000
_diffrn_orient_matrix_UB_32      0.0507046000
_diffrn_orient_matrix_UB_33      -0.0084941000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0811
_diffrn_reflns_av_unetI/netI     0.0941
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            26609
_diffrn_reflns_theta_full        66.50
_diffrn_reflns_theta_max         67.00
_diffrn_reflns_theta_min         4.66
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           35
_diffrn_source_power             1.75
_diffrn_source_target            Cu
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    4.948
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63224
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.141
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2932
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.908
_refine_diff_density_min         -0.971
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     739
_refine_ls_number_reflns         14314
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0917
_refine_ls_R_factor_gt           0.0607
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0640P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1409
_refine_ls_wR_factor_ref         0.1583
_reflns_number_gt                10046
_reflns_number_total             14314
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400183n_si_002.cif
_cod_data_source_block           erq36cult
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

2026-05-15
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_weight         1400.17
_cod_original_formula_moiety         '2(C31 H48 N P Ru S Si3), C2.5 O0.25'
_cod_original_formula_units_Z            4
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_original_formula_sum        'C64.50 H96 N2 O0.25 P2 Ru2 S2 Si6'
_cod_database_code               4081220
_reflns_odcompleteness_completeness 98.48
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13