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_4305471
_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         'C45 H42 O2 P2 Rh2 S2, C H2 Cl2'
_chemical_formula_sum            'C46 H44 Cl2 O2 P2 Rh2 S2'
_chemical_formula_weight         1031.59
_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                 107.7410(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.6034(12)
_cell_length_b                   10.6870(7)
_cell_length_c                   24.2161(17)
_cell_measurement_reflns_used    19904
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.294
_cell_measurement_theta_min      2.26
_cell_volume                     4339.1(5)
_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 0.999
_diffrn_measured_fraction_theta_max 0.968
_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  0.0286
_diffrn_reflns_av_sigmaI/netI    0.0237
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            51934
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         1.71
_diffrn_standards_number         'no decay'
_exptl_absorpt_coefficient_mu    1.092
_exptl_absorpt_correction_T_max  0.7921
_exptl_absorpt_correction_T_min  0.6850
_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    1.579
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             2088
_exptl_crystal_size_max          0.375
_exptl_crystal_size_mid          0.229
_exptl_crystal_size_min          0.224
_refine_diff_density_max         1.354
_refine_diff_density_min         -1.054
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     681
_refine_ls_number_reflns         10466
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0304
_refine_ls_R_factor_gt           0.0257
_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^)+(0.0255P)^2^+3.9875P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0587
_refine_ls_wR_factor_ref         0.0603
_reflns_number_gt                9397
_reflns_number_total             10466
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800464p-file002_4.cif
_cod_data_source_block           compound_16
_cod_database_code               4305471