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_4323448
_publ_contact_author
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Prof. Dr. Wolfdieter A. Schenk
Institut f\"ur Anorganische Chemie
Universit\"at W\"urzburg
Am Hubland
D-97074 W\"urzburg
Germany
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_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_sum            'C37 H43 F6 P3 Ru S'
_chemical_formula_weight         827.75
_chemical_name_systematic
;
 ?
;
_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'
_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                 106.04(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.539(5)
_cell_length_b                   16.216(9)
_cell_length_c                   11.011(8)
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      25.76
_cell_measurement_theta_min      1.92
_cell_volume                     1808.5(19)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens SHELXTL-Plus'
_computing_publication_material  'Siemens SHELXTL-Plus'
_computing_structure_refinement  'SHELXL-96 (Sheldrick, 1996)'
_computing_structure_solution    'SHELXS-96 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measurement_device       Stoe-Huber-Siemens-CCD
_diffrn_measurement_method       Phi-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0223
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5950
_diffrn_reflns_theta_max         25.76
_diffrn_reflns_theta_min         1.92
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.682
_exptl_absorpt_correction_type   semiempirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_description       blocks
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.5
_refine_diff_density_max         .501
_refine_diff_density_min         -.610
_refine_diff_density_rms         .073
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.04(4)
_refine_ls_extinction_coef       0.0068(5)
_refine_ls_extinction_expression Fc^*^=3DkFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.101
_refine_ls_goodness_of_fit_obs   1.094
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     517
_refine_ls_number_reflns         5950
_refine_ls_number_restraints     225
_refine_ls_restrained_S_all      1.113
_refine_ls_restrained_S_obs      1.103
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_obs          0.0376
_refine_ls_shift/esd_max         0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0421P)^2^+4.3381P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0992
_refine_ls_wR_factor_obs         0.0983
_reflns_number_observed          5929
_reflns_number_total             5950
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic961280f_4.cif
_cod_data_source_block           duerr
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0421P)^2^+4.3381P] 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^)+(0.0421P)^2^+4.3381P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4323448