Oxidation of Thioether Ligands in Pseudotetrahedral Cyclopentadienylruthenium Complexes: Toward a New Stereoselective Synthesis of Chiral Sulfoxides1
Wolfdieter A. Schenk; Jürgen Frisch; Michael Dürr; Nicolai Burzlaff; Dietmar Stalke; Roland Fleischer; Waldemar Adam; Frank Prechtl; Alexander K. Smerz; Inorganic Chemistry 36 (1997) 2372–2378; doi:10.1021/ic961280f

data_4323447
_publ_contact_author
;
Prof. Dr. Wolfdieter A. Schenk
Institut f\"ur Anorganische Chemie
Universit\"at W\"urzburg
Am Hubland
D-97074 W\"urzburg
Germany
;
_publ_contact_author_email       wolfdieter@wacd48.chemie.uni-wuerzburg.de
_publ_contact_author_fax         '049 931 8884605'
_publ_contact_author_phone       '049 931 8885259'
_publ_section_title
;
 Oxidation of Thioether Ligands in Pseudotetrahedral
 Cyclopentadienylruthenium Complexes: Toward a New Stereoselective
 Synthesis of Chiral Sulfoxides1
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2372
_journal_page_last               2378
_journal_paper_doi               10.1021/ic961280f
_journal_volume                  36
_journal_year                    1997
_chemical_formula_moiety         'C37 H43 Cl1 F6 O P3 Ru S  x  0.93 CH2 Cl2'
_chemical_formula_sum            'C37.93 H44.86 Cl2.86 F6 O P3 Ru S'
_chemical_formula_weight         922.74
_chemical_name_systematic
;
[2(S),3(S)-Bis(diphenylphosphino)butane-(eta-5-cyclopentadienyl)-
(methyl-isopropyl-sulfoxide)-ruthenium]hexafluorophosphate
;
_chemical_temperature_decomposition 361
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.069(2)
_cell_length_b                   17.379(2)
_cell_length_c                   19.760(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      16
_cell_measurement_theta_min      10
_cell_volume                     4144.6(13)
_computing_cell_refinement       'SDP (ENRAF-NONIUS)'
_computing_data_collection       'ENRAF-NONIUS CAD4'
_computing_data_reduction        'SDP (ENRAF-NONIUS)'
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'ENRAF-NONIUS CAD4'
_diffrn_measurement_method       Omega-theta-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.70930
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0354
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5494
_diffrn_reflns_theta_max         27.89
_diffrn_reflns_theta_min         2.05
_diffrn_standards_decay_%        -17.4
_diffrn_standards_interval_time  3600
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.372
_exptl_absorpt_correction_T_max  0.9994
_exptl_absorpt_correction_T_min  0.9054
_exptl_absorpt_correction_type   psi-scans
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.479
_exptl_crystal_description       'clear prism'
_exptl_crystal_F_000             1884
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.5
_refine_diff_density_max         0.476
_refine_diff_density_min         -0.417
_refine_diff_density_rms         0.120
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.095
_refine_ls_goodness_of_fit_obs   0.991
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         5493
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_restrained_S_obs      0.991
_refine_ls_R_factor_all          0.0894
_refine_ls_R_factor_obs          0.0476
_refine_ls_shift/esd_max         0.138
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1040P)^2^+2.4881P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1802
_refine_ls_wR_factor_obs         0.1365
_reflns_number_observed          3973
_reflns_number_total             5494
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic961280f_3.cif
_cod_data_source_block           md3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1040P)^2^+2.4881P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1040P)^2^+2.4881P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        4144.7(14)
_cod_database_code               4323447