Synthesis, Structural Characterization, and Ligand Replacement Reactions of gem-Dithiolato-Bridged Rhodium and Iridium Complexes
Angel B. Rivas; José M. Gascón; Fernando J. Lahoz; Ana I. Balana; Alvaro J. Pardey; Luis A. Oro; Jesús J. Pérez-Torrente; Inorganic Chemistry 47 (2008) 6090–6104; doi:10.1021/ic800464p

data_4305470
_publ_contact_author_address
;
  Dr. Fernando J. Lahoz
  Departamento de Qu\'imica Inorg\'anica - I.C.M.A.
  Facultad de Ciencias
  Universidad de Zaragoza - C.S.I.C.
  50009 Zaragoza, Spain
;
_publ_contact_author_email       lahoz@unizar.es
_publ_contact_author_fax         '+34 976 761187'
_publ_contact_author_name        'Dr. Fernando J. Lahoz'
_publ_contact_author_phone       '+34 976 761147'
_publ_section_title
;
Synthesis, Structural Characterization, and Ligand Replacement Reactions
of gem-Dithiolato-Bridged Rhodium and Iridium Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6090
_journal_page_last               6104
_journal_paper_doi               10.1021/ic800464p
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C21 H32 Rh2 S2'
_chemical_formula_sum            'C21 H32 Rh2 S2'
_chemical_formula_weight         554.41
_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                108.7250(10)
_cell_angle_beta                 92.1170(10)
_cell_angle_gamma                108.5870(10)
_cell_formula_units_Z            2
_cell_length_a                   7.5580(5)
_cell_length_b                   9.9802(6)
_cell_length_c                   15.1423(9)
_cell_measurement_reflns_used    9863
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.282
_cell_measurement_theta_min      2.243
_cell_volume                     1012.90(11)
_computing_cell_refinement       'SAINT+ v. 6.22 (Bruker AXS, 2001)'
_computing_data_collection       'SMART v. 5.625 (Bruker AXS, 2001)'
_computing_data_reduction        'SAINT+ v. 6.22 (Bruker AXS, 2001)'
_computing_molecular_graphics    'XP, SHELXTL v. 6.10 (Bruker, 2000)'
_computing_publication_material  'XCIF, SHELXTL v. 6.10 (Bruker, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_device_details
; 
 Full data completeness has been obtained considering the 2theta=50 
 degrees standard IUCr criterion. Addtional partial data, to a maximum
 2theta value of 56.57 degrees, has been measured to complete an overall
 0.939 fraction.
;
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       '\w rotations with narrow frames'
_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  0.0132
_diffrn_reflns_av_sigmaI/netI    0.0158
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            12332
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         2.24
_diffrn_standards_number         'no decay'
_exptl_absorpt_coefficient_mu    1.837
_exptl_absorpt_correction_T_max  0.5423
_exptl_absorpt_correction_T_min  0.5366
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; SADABS: Area-Detector Absorption Correction. Bruker-AXS 
  within SAINT+ package, v. 6.22 (2001).
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.818
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             560
_exptl_crystal_size_max          0.343
_exptl_crystal_size_mid          0.342
_exptl_crystal_size_min          0.336
_refine_diff_density_max         0.567
_refine_diff_density_min         -0.360
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     354
_refine_ls_number_reflns         4718
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0171
_refine_ls_R_factor_gt           0.0160
_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^)+(0.0186P)^2^+0.4895P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0393
_refine_ls_wR_factor_ref         0.0398
_reflns_number_gt                4539
_reflns_number_total             4718
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800464p-file002_3.cif
_cod_data_source_block           compound_6
_cod_database_code               4305470