Syntheses of Ketonated Disulfide-Bridged Diruthenium Complexes via C-H Bond Activation and C-S Bond Formation
Hiroyasu Sugiyama; Md. Munkir Hossain; Yong-Shou Lin; Kazuko Matsumoto; Inorganic Chemistry 39 (2000) 3948–3956; doi:10.1021/ic0000855

data_4321298
_publ_section_title
;
 Syntheses of Ketonated Disulfide-Bridged Diruthenium Complexes via C-H
 Bond Activation and C-S Bond Formation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3948
_journal_page_last               3956
_journal_paper_doi               10.1021/ic0000855
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C34 H60 F9 N5 O23 P4 Ru2 S5'
_chemical_formula_weight         1564.19
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.8310(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.7178(7)
_cell_length_b                   24.4198(11)
_cell_length_c                   16.8492(8)
_cell_measurement_temperature    223(2)
_cell_volume                     6466.5(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.852
_diffrn_measured_fraction_theta_max 0.852
_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  0.0214
_diffrn_reflns_av_sigmaI/netI    0.0428
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            22192
_diffrn_reflns_theta_full        27.59
_diffrn_reflns_theta_max         27.59
_diffrn_reflns_theta_min         1.47
_exptl_absorpt_coefficient_mu    0.824
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.607
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             3168
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.009
_refine_diff_density_min         -0.929
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     763
_refine_ls_number_reflns         12765
_refine_ls_number_restraints     56
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0961
_refine_ls_R_factor_gt           0.0659
_refine_ls_shift/su_max          0.099
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1484P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1953
_refine_ls_wR_factor_ref         0.2191
_reflns_number_gt                8450
_reflns_number_total             12765
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0000855_3.cif
_cod_data_source_block           C34H60F9N5O23P4Ru2S5
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_database_code               4321298