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_4321297
_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_moiety         'C28 H61 F18 N5 O13 P4 S2 Ru2 Sb3 '
_chemical_formula_sum            'C28 H61 F18 N5 O13 P4 Ru2 S2 Sb3'
_chemical_formula_weight         1773.19
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90
_cell_angle_beta                 94.95(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.993(3)
_cell_length_b                   13.919(4)
_cell_length_c                   21.258(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298.2
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      14.5
_cell_volume                     6188(2)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan Ver. 1.10'
_computing_publication_material  'teXsan Ver. 1.10'
_computing_structure_refinement  SHELXL97
_computing_structure_solution    'DIRDIF94 (PATTY)'
_diffrn_measurement_device_type  'Rigaku AFC7R'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.068
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            12667
_diffrn_reflns_theta_max         27.47
_diffrn_standards_decay_%        5.93
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.044
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.887
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.903
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.77
_refine_diff_density_min         -0.63
_refine_ls_extinction_coef       0.0000
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.962
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     708
_refine_ls_number_reflns         5261
_refine_ls_R_factor_gt           0.0620
_refine_ls_shift/su_max          1.8680
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^) + (0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2014
_reflns_number_gt                5261
_reflns_number_total             10971
_reflns_threshold_expression     >2.0sigma(I)
_cod_data_source_file            ic0000855_2.cif
_cod_data_source_block           C28H61F18N5O13P4S2Ru2Sb3
_cod_original_cell_volume        6188(1)
_cod_original_formula_sum        'C28 H61 F18 N5 O13 P4 S2 Ru2 Sb3 '
_cod_database_code               4321297