C-H Cleavage and Double Alkyl Additions to the Disulfido Ligand in Dicyanido-Bridged Ru2S2 Complexes
Sumito Ishizu; Hiroyasu Sugiyama; Brian K. Breedlove; Kazuko Matsumoto; Inorganic Chemistry 46 (2007) 3726–3735; doi:10.1021/ic062460k

data_4307986
_publ_section_title
;
C-H Cleavage and Double Alkyl Additions to the Disulfido Ligand in
Dicyanido-Bridged Ru2S2 Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3726
_journal_page_last               3735
_journal_paper_doi               10.1021/ic062460k
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C30 H56 Cl2 F6 N2 O18 P4 Ru2 S4'
_chemical_formula_weight         1371.93
_chemical_name_systematic
;
?
;
_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
_cell_angle_alpha                103.258(12)
_cell_angle_beta                 94.601(12)
_cell_angle_gamma                95.267(14)
_cell_formula_units_Z            2
_cell_length_a                   8.853(7)
_cell_length_b                   12.380(9)
_cell_length_c                   24.678(18)
_cell_measurement_reflns_used    'reflections from 45 data frames'
_cell_measurement_temperature    120(2)
_cell_volume                     2607(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.917
_diffrn_measured_fraction_theta_max 0.917
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0222
_diffrn_reflns_av_sigmaI/netI    0.0497
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            16055
_diffrn_reflns_theta_full        27.64
_diffrn_reflns_theta_max         27.64
_diffrn_reflns_theta_min         1.70
_diffrn_standards_number         '50 standard frames at start and end'
_exptl_absorpt_coefficient_mu    1.052
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing,R., Acta Cryst. (1995) A51 33-38.'
_exptl_crystal_density_diffrn    1.748
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1388
_refine_diff_density_max         4.066
_refine_diff_density_min         -1.681
_refine_diff_density_rms         0.172
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     547
_refine_ls_number_reflns         11153
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0842
_refine_ls_R_factor_gt           0.0626
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0776P)^2^+20.6845P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1570
_refine_ls_wR_factor_ref         0.1740
_reflns_number_gt                8657
_reflns_number_total             11153
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic062460ksi20070204_124206_08.cif
_cod_data_source_block           complex8
_cod_database_code               4307986