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_4081219
_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 F3 O3 P Ru S Si3, C4 H10 O'
_chemical_formula_sum            'C35 H58 F3 O4 P Ru S Si3'
_chemical_formula_weight         848.18
_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             2011-05-17
_audit_creation_method
;
  Olex2 1.1-beta
  (compiled 2011.02.15 svn.r1672, GUI svn.r3494)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 93.0830(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.72890(10)
_cell_length_b                   18.1582(3)
_cell_length_c                   20.2285(3)
_cell_measurement_reflns_used    6323
_cell_measurement_temperature    173.0
_cell_measurement_theta_max      71.4910
_cell_measurement_theta_min      9.6870
_cell_volume                     4301.94(10)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_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  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
'A short history of SHELX (Sheldrick, 2007)/Bruker'
_diffrn_ambient_temperature      173.0
_diffrn_detector_area_resol_mean 15.9578
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_details
;
  1 omega   39.00   67.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000  150.0000 28

  2 omega   38.00  114.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000   68.0000 -174.0000 76

  3 omega   88.00  124.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000  125.0000 -120.0000 36

  4 omega   74.00  126.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000  125.0000 -180.0000 52

  5 omega   29.00  115.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000   38.0000  -60.0000 86

  6 omega   39.00   69.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000  -90.0000 30

  7 omega   40.00   72.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000 -120.0000 32

  8 omega   40.00   82.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -50.0000 -150.0000 42

  9 omega   40.00   71.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -50.0000   30.0000 31

 10 omega   48.00   77.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -50.0000   60.0000 29

 11 omega   44.00   83.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -50.0000  -30.0000 39

 12 omega   89.00  169.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   77.0000  -90.0000 80

 13 omega   92.00  167.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   58.0000  158.0000 75

 14 omega   89.00  171.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   50.0000 -120.0000 82
;
_diffrn_measurement_device       'kappa diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.1194583000
_diffrn_orient_matrix_UB_12      0.0017325000
_diffrn_orient_matrix_UB_13      -0.0280453000
_diffrn_orient_matrix_UB_21      -0.0379654000
_diffrn_orient_matrix_UB_22      -0.0587212000
_diffrn_orient_matrix_UB_23      -0.0515275000
_diffrn_orient_matrix_UB_31      -0.0397326000
_diffrn_orient_matrix_UB_32      0.0612418000
_diffrn_orient_matrix_UB_33      -0.0487484000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0756
_diffrn_reflns_av_unetI/netI     0.0668
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            14019
_diffrn_reflns_theta_full        66.50
_diffrn_reflns_theta_max         67.00
_diffrn_reflns_theta_min         9.69
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Cu
_exptl_absorpt_coefficient_mu    4.942
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73977
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         2.063
_refine_diff_density_min         -1.649
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     441
_refine_ls_number_reflns         7444
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0771
_refine_ls_R_factor_gt           0.0696
_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^)+(0.1485P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1879
_refine_ls_wR_factor_ref         0.1969
_reflns_number_gt                6364
_reflns_number_total             7444
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400183n_si_002.cif
_cod_data_source_block           erq24cult
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4081219
_reflns_odcompleteness_completeness 98.08
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13