New Class of Ruthenium Sulfide Clusters: Ru4S6(PPh3)4, Ru5S6(PPh3)5, and Ru6S8(PPh3)6
Amanda L. Eckermann; Markus Wunder; Dieter Fenske; Thomas B. Rauchfuss; Scott R. Wilson; Inorganic Chemistry 41 (2002) 2004–2006; doi:10.1021/ic0255104

data_4317903
_publ_contact_author
; 
Thomas B. Rauchfuss 
University of Illinois 
School of Chemical Sciences 
600 South Mathews Avenue Box 12-6 
Urbana, Illinois  61801 
USA 
;
_publ_contact_author_email       rauchfuz@uiuc.edu
_publ_contact_author_fax         '1  217 333 2685'
_publ_contact_author_phone       '1  217 333 7355'
_publ_section_title
;
 New Class of Ruthenium Sulfide Clusters: Ru4S6(PPh3)4, Ru5S6(PPh3)5, and
 Ru6S8(PPh3)6
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2004
_journal_page_last               2006
_journal_paper_doi               10.1021/ic0255104
_journal_volume                  41
_journal_year                    2002
_chemical_formula_moiety         'C90 H75 P5 Ru5 S6, C H2 Cl2, C4 H10 O'
_chemical_formula_sum            'C90 H75 Cl0 O0 P5 Ru5 S6'
_chemical_formula_weight         2009.06
_chemical_name_common            p90n
_chemical_name_systematic
; 
Pentaruthenium-hexakis(m-sulfido)-penta(triphenylphosphine) dichloromethane 
diethylether solvate 
;
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
; 
2002-01-17   text and data added, ALE 
;
_cell_angle_alpha                70.376(10)
_cell_angle_beta                 83.605(11)
_cell_angle_gamma                83.160(11)
_cell_formula_units_Z            2
_cell_length_a                   14.470(9)
_cell_length_b                   16.526(10)
_cell_length_c                   21.985(13)
_cell_measurement_reflns_used    1003
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.9
_cell_volume                     4902(5)
_computing_cell_refinement       'SAINT V5 (Bruker, 1998)'
_computing_data_collection       'SMART V5 (Bruker, 1998)'
_computing_data_reduction        'SAINT V5 (Bruker, 1998)'
_computing_molecular_graphics    'SHELXTL V5 (Bruker, 1998)'
_computing_publication_material  'CIFTAB (Sheldrick, 1998)'
_computing_structure_refinement  'SHELXTL V5 (Bruker, 1998)'
_computing_structure_solution    'SHELXTL V5 (Bruker, 1998)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device       'Siemens Platform/CCD'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'profile data from \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  p90na
_diffrn_reflns_av_R_equivalents  0.0823
_diffrn_reflns_av_sigmaI/netI    0.1129
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            35889
_diffrn_reflns_theta_full        25.07
_diffrn_reflns_theta_max         25.07
_diffrn_reflns_theta_min         1.67
_diffrn_standards_decay_%        1.7
_diffrn_standards_interval_time  546
_diffrn_standards_number         386
_exptl_absorpt_coefficient_mu    1.001
_exptl_absorpt_correction_T_max  0.9134
_exptl_absorpt_correction_T_min  0.7570
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(Bruker, 1998)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_description       tabular
_exptl_crystal_F_000             2012
_exptl_crystal_id                p90na
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Paratone-N, Exxon) to a thin 
glass fiber with the (1 0 0) scattering planes roughly normal to the 
spindle axis. 
;
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.643
_refine_diff_density_min         -1.252
_refine_diff_density_rms         0.165
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     955
_refine_ls_number_reflns         17209
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.1106
_refine_ls_R_factor_gt           0.0744
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0791P)^2^+36.7588P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1937
_refine_ls_wR_factor_ref         0.2050
_reflns_number_gt                11283
_reflns_number_total             17209
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0255104_s1_3.cif
_cod_data_source_block           p90nzs
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4317903