Metal-Stabilized Thiyl Radicals as Scaffolds for Reversible Alkene Addition via C-S Bond Formation/Cleavage
Kagna Ouch; Mark S. Mashuta; Craig A. Grapperhaus; Inorganic Chemistry 50 (2011) 9904–9914; doi:10.1021/ic200416y

data_4326445
_publ_contact_author_email       grapperhaus@louisville.edu
_publ_contact_author_fax         '(502)852-8149 '
_publ_contact_author_phone       '(502)852-5932 '
_publ_section_title
;
 Metal-Stabilized Thiyl Radicals as Scaffolds for Reversible Alkene
 Addition via C-S Bond Formation/Cleavage
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9904
_journal_page_last               9914
_journal_paper_doi               10.1021/ic200416y
_journal_volume                  50
_journal_year                    2011
_chemical_absolute_configuration ad
_chemical_formula_moiety
;
2(C63 H52 P3 Ru S3), 2(F6 P), 3(C Cl2) 
;
_chemical_formula_sum            'C64.5 H52 Cl3 F6 P4 Ru S3'
_chemical_formula_weight         1368.54
_chemical_name_common
;
[(2-(diphenylphosphine)thiaphenolato)(m-methylphenylethane
-1,2-diylbis(thio-2,1-phenylene)diphenylphosphine)ruthenium(II)]
hexafluorophosphate
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
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_atom_sites_solution_primary     direct
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_audit_creation_method
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_cell_angle_alpha                90.00
_cell_angle_beta                 104.576(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.5855(4)
_cell_length_b                   16.8551(5)
_cell_length_c                   17.7704(4)
_cell_measurement_reflns_used    17101
_cell_measurement_temperature    100.1
_cell_measurement_theta_max      29.5987
_cell_measurement_theta_min      3.3797
_cell_volume                     3068.54(17)
_computing_cell_refinement
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CrysAlisPro, Oxford Diffraction Ltd.,
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_computing_data_collection
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
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_computing_data_reduction
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CrysAlisPro, Oxford Diffraction Ltd.,
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_computing_molecular_graphics    'SHELXTL 6.14 (Bruker, 2006)'
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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 0.945
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_details
;
  1 omega  -74.00  109.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       15.3871    0.0000 -180.0000 183

  2 omega   66.00   92.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       15.3871  179.0000 -120.0000 26

  3 omega  -95.00  -47.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.9965  154.0000  166.0000 48

  4 omega   19.00   67.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.9965 -159.0000  -70.0000 48

  5 omega  -36.00   22.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.9965  -77.0000    0.0000 58

  6 omega  -17.00   84.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       15.3871   37.0000  -90.0000 101

  7 omega   -7.00   96.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       15.3871   37.0000    0.0000 103

  8 omega   -4.00   71.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       15.3871 -118.0000   81.0000 75

  9 omega   59.00   85.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       15.3871  159.0000 -109.0000 26

;
_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     0.7107
_diffrn_reflns_av_R_equivalents  0.0498
_diffrn_reflns_av_sigmaI/netI    0.0584
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            50963
_diffrn_reflns_theta_full        29.65
_diffrn_reflns_theta_max         29.65
_diffrn_reflns_theta_min         3.38
_exptl_absorpt_coefficient_mu    0.651
_exptl_absorpt_correction_T_max  0.952
_exptl_absorpt_correction_T_min  0.926
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
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empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.481
_exptl_crystal_description       needle
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.372
_refine_diff_density_min         -0.564
_refine_diff_density_rms         0.098
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     778
_refine_ls_number_reflns         15701
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0563
_refine_ls_R_factor_gt           0.0438
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0630P)^2^+1.7472P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1042
_refine_ls_wR_factor_ref         0.1136
_reflns_number_gt                13750
_reflns_number_total             15701
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic200416y_si_002_1.cif
_cod_data_source_block           1
_cod_original_cell_volume        3068.53(18)
_cod_original_sg_symbol_H-M      'P 21'
_cod_original_formula_sum        'C64.50 H52 Cl3 F6 P4 Ru S3'
_cod_database_code               4326445