Selective and Reversible Base-Induced Elimination of a Ruthenium Dithioether Yields a Vinyl Metallosulfonium Complex
Rajat Chauhan; Mark S. Mashuta; Craig A. Grapperhaus; Inorganic Chemistry 51 (2012) 7913–7920; doi:10.1021/ic300983x

data_4329765
_publ_contact_author_email       grapperhaus@louisville.edu
_publ_contact_author_fax         '(502)852-8149 '
_publ_contact_author_phone       '(502)852-5932 '
_publ_section_title
;
 Selective and Reversible Base-Induced Elimination of a Ruthenium
 Dithioether Yields a Vinyl Metallosulfonium Complex
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7913
_journal_page_last               7920
_journal_paper_doi               10.1021/ic300983x
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         '2(C56 H45 P3 Ru S3), 4(C7 H8), C7'
_chemical_formula_sum            'C73.5 H61 P3 Ru S3'
_chemical_formula_weight         1234.38
_chemical_name_common
;
bis(2-(diphenylphosphanyl)benzenethiolato)
[2-(ethenylsulfanyl)phenyl] diphenylphosphine ruthenium(II)
;
_chemical_name_systematic
; 
bis(2-(diphenylphosphanyl)benzenethiolato) 
[2-(ethenylsulfanyl)phenyl] diphenylphosphine ruthenium(II)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
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;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_audit_update_record
;
2011-05-20 # Formatted by publCIF
May_07_2012 text and data added by Mark S. Mashuta
;
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_cell_angle_beta                 98.154(4)
_cell_angle_gamma                105.209(3)
_cell_formula_units_Z            2
_cell_length_a                   11.2718(5)
_cell_length_b                   12.0524(3)
_cell_length_c                   23.6075(10)
_cell_measurement_reflns_used    20264
_cell_measurement_temperature    100.1
_cell_measurement_theta_max      29.55
_cell_measurement_theta_min      3.36
_cell_volume                     2965.0(2)
_computing_cell_refinement
'CrysAlisPro, Version 1.171.35.11 (Agilent Technologies., 2010)'
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'CrysAlisPro, Version 1.171.35.11 (Agilent Technologies., 2010)'
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'CrysAlisPro, Version 1.171.35.11 (Agilent Technologies., 2010)'
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'ORTEP-3 (Farrugia, 1997), PLATON (Spek, 2009) and publCIF (Westrip, 2010)'
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_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.1
_diffrn_detector_area_resol_mean 10.2836
_diffrn_measured_fraction_theta_full 0.924
_diffrn_measured_fraction_theta_max 0.924
_diffrn_measurement_details
;
  1 omega  -92.00  -66.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.9183  179.0000  150.0000 26

  2 omega   32.00   58.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       15.2308 -101.0000  -16.0000 26

  3 omega  -49.00   47.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       15.2308  -37.0000  -90.0000 96

  4 omega  -16.00   52.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       15.2308   77.0000 -180.0000 68

  5 omega  -47.00   40.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       15.2308  -77.0000   60.0000 87

  6 omega  -22.00   30.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.9183 -101.0000  -16.0000 52

  7 omega -108.00  -53.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.9183  179.0000 -120.0000 55

  8 omega -108.00  -53.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.9183  179.0000   90.0000 55

  9 omega -108.00  -53.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.9183  179.0000   30.0000 55

 10 omega  -18.00   96.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       15.2308   37.0000  -30.0000 114

 11 omega  -23.00   28.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       15.2308 -101.0000  -87.0000 51

 12 omega  -18.00   96.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       15.2308   37.0000 -180.0000 114

 13 omega  -18.00   96.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       15.2308   37.0000   60.0000 114
;
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) x-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0416
_diffrn_reflns_av_sigmaI/netI    0.0404
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            67874
_diffrn_reflns_theta_full        29.62
_diffrn_reflns_theta_max         29.62
_diffrn_reflns_theta_min         3.37
_exptl_absorpt_coefficient_mu    0.496
_exptl_absorpt_correction_T_max  0.952
_exptl_absorpt_correction_T_min  0.926
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Version 1.171.35.11 (Agilent Technologies., 2010)
empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_description       'cut block'
_exptl_crystal_F_000             1278
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.763
_refine_diff_density_min         -0.736
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     735
_refine_ls_number_reflns         15439
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0562
_refine_ls_R_factor_gt           0.0383
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0250P)^2^+2.7003P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0763
_refine_ls_wR_factor_ref         0.0849
_reflns_number_gt                12354
_reflns_number_total             15439
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic300983x_si_002.cif
_cod_data_source_block           1
_cod_original_cell_volume        2965.04(21)
_cod_original_formula_sum        'C73.50 H61 P3 Ru S3'
_cod_database_code               4329765
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_theta     27.04