Transition Metal Complexes with Sulfur Ligands. 130.1 Synthesis, Structure, and Reactivity of the Sulfur-Rich Ruthenium Hydride Complexes [Ru(H)(PR~3~)('S~4~')]^-^ and the η2-H2 Complex [Ru(H~2~)(PCy~3~)('S~4~')] (R = Ph, ^i^Pr, Cy; 'S~4~'2- = 1,2-Bis((2-mercaptophenyl)thio)ethane(2-))
Dieter Sellmann; Torsten Gottschalk-Gaudig; Frank W. Heinemann; Inorganic Chemistry 37 (1998) 3982–3988; doi:10.1021/ic971068r

data_4322918
_publ_contact_author
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        Prof. Dr. D. Sellmann      
        Institut f\"ur Anorganische Chemie II                                   
        Universit\"at Erlangen-N\"urnberg                                       
        Egerlandstr. 1                                                          
        D-91058 Erlangen                                                        
        Bundesrepublik Deutschland                                              
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_publ_contact_author_email       SELLMANN@ANORGANIK.CHEMIE.UNI-ERLANGEN.DE
_publ_contact_author_fax         '049 9131 85-7367'
_publ_contact_author_phone       '049 9131 85-7360'
_publ_section_title
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 Transition Metal Complexes with Sulfur Ligands. 130.1 Synthesis,
 Structure, and Reactivity of the Sulfur-Rich Ruthenium Hydride Complexes
 [Ru(H)(PR~3~)('S~4~')]^-^ and the \h2-H2 Complex
 [Ru(H~2~)(PCy~3~)('S~4~')] (R = Ph, ^i^Pr, Cy; 'S~4~'2- =
 1,2-Bis((2-mercaptophenyl)thio)ethane(2-))
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3982
_journal_page_last               3988
_journal_paper_doi               10.1021/ic971068r
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C33 H57 Li O2.5 P Ru S4'
_chemical_formula_weight         761.01
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 95.040(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.016(2)
_cell_length_b                   10.452(3)
_cell_length_c                   25.906(4)
_cell_measurement_reflns_used    18
_cell_measurement_temperature    175(2)
_cell_measurement_theta_max      15.5
_cell_measurement_theta_min      14.0
_cell_volume                     3780.4(13)
_computing_cell_refinement       'P3 (Siemens Analytical X-Ray Instr., 1989)'
_computing_data_collection       'P3 (Siemens Analytical X-Ray Instr., 1989)'
_computing_data_reduction
'XDISK (Siemens Analytical X-Ray Instr. , 1989)'
_computing_molecular_graphics
'SHELXTL 5.03 (Siemens Analytical X-Ray Instr, 1995)'
_computing_publication_material
'SHELXTL 5.03 (Siemens Analytical X-Ray Instr, 1995)'
_computing_structure_refinement
'SHELXTL 5.03 (Siemens Analytical X-Ray Instr, 1995)'
_computing_structure_solution
'SHELXTL-PLUS (Siemens Analytical X-Ray Instr, 1990)'
_diffrn_ambient_temperature      175(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       'profile data from \w-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  0.0303
_diffrn_reflns_av_sigmaI/netI    0.0604
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            11814
_diffrn_reflns_theta_max         27.06
_diffrn_reflns_theta_min         2.10
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.706
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_description       block
_exptl_crystal_F_000             1604
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.778
_refine_diff_density_min         -0.574
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.925
_refine_ls_goodness_of_fit_obs   0.873
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     529
_refine_ls_number_reflns         8294
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.925
_refine_ls_restrained_S_obs      0.873
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_obs          0.0294
_refine_ls_shift/esd_max         -0.014
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0493P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0906
_refine_ls_wR_factor_obs         0.0713
_reflns_number_observed          5940
_reflns_number_total             8294
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic971068r_2.cif
_cod_data_source_block           tg37
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0493P)^2^+0.0000P] 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^)+(0.0493P)^2^+0.0000P] 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_original_formula_sum        'C33 H57 Li O2.50 P Ru S4'
_cod_database_code               4322918