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_4307984
_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 H54 Br2 F6 N2 O18 P4 Ru2 S4'
_chemical_formula_weight         1458.83
_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                102.601(8)
_cell_angle_beta                 99.426(9)
_cell_angle_gamma                94.774(9)
_cell_formula_units_Z            2
_cell_length_a                   9.367(4)
_cell_length_b                   11.691(5)
_cell_length_c                   23.899(11)
_cell_measurement_reflns_used    'reflections from 45 data frames'
_cell_measurement_temperature    123(2)
_cell_volume                     2500.3(19)
_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      123(2)
_diffrn_measured_fraction_theta_full 0.909
_diffrn_measured_fraction_theta_max 0.909
_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  0.0346
_diffrn_reflns_av_sigmaI/netI    0.0751
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            14568
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         0.89
_diffrn_standards_number         '50 standard frames at start and end'
_exptl_absorpt_coefficient_mu    2.588
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing,R., Acta Cryst. (1995) A51 33-38.'
_exptl_crystal_density_diffrn    1.938
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1456
_refine_diff_density_max         3.338
_refine_diff_density_min         -2.305
_refine_diff_density_rms         0.249
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     547
_refine_ls_number_reflns         10468
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0994
_refine_ls_R_factor_gt           0.0754
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0210P)^2^+97.5199P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1897
_refine_ls_wR_factor_ref         0.2009
_reflns_number_gt                7900
_reflns_number_total             10468
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic062460ksi20070204_124206_06.cif
_cod_data_source_block           complex6Br
_cod_original_cell_volume        2500.4(19)
_cod_database_code               4307984