Synthesis of Tetranuclear Rhodium and Iridium Complexes Directed by 6-Mercaptopyridin-2-ol: Electrochemical Behavior, Chemical Oxidation, and Coordination Chemistry
Pablo J. Alonso; Oscar Benedí; María J. Fabra; Fernando J. Lahoz; Luis A. Oro; Jesús J. Pérez-Torrente; Inorganic Chemistry 48 (2009) 7984–7993; doi:10.1021/ic9005289

data_4302919
_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 of Tetranuclear Rhodium and Iridium Complexes Directed by
6-Mercaptopyridin-2-ol: Electrochemical Behavior, Chemical Oxidation, and
Coordination Chemistry
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7984
_journal_page_last               7993
_journal_paper_doi               10.1021/ic9005289
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         ' C42 H54 N2 O2 Rh4 S2, 2(C H2 Cl2)'
_chemical_formula_sum            'C44 H58 Cl4 N2 O2 Rh4 S2'
_chemical_formula_weight         1264.48
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 98.994(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.3868(11)
_cell_length_b                   18.516(2)
_cell_length_c                   25.869(3)
_cell_measurement_reflns_used    7268
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.41
_cell_measurement_theta_min      2.2
_cell_volume                     4440.9(9)
_computing_cell_refinement       'SAINT+ v. 6.45 (Bruker AXS, 2003)'
_computing_data_collection       'SMART v. 5.611 (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT+ v. 6.45 (Bruker AXS, 2003)'
_computing_molecular_graphics    'XP program, SHELXTL v6.12, Bruker2000'
_computing_publication_material  'XCIF program, SHELXTLv6.12, BrukerAXS'
_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 0.982
_diffrn_measured_fraction_theta_max 0.918
_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  0.0253
_diffrn_reflns_av_sigmaI/netI    0.0340
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14434
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.57
_diffrn_reflns_theta_min         1.59
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    1.836
_exptl_absorpt_correction_T_max  0.8194
_exptl_absorpt_correction_T_min  0.6598
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS: Area-Detector Absorption Correction. (1996)  Bruker-AXS 
 within SAINT+ package, v. 6.45.                    
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.891
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             2528
_exptl_crystal_size_max          0.247
_exptl_crystal_size_mid          0.201
_exptl_crystal_size_min          0.113
_refine_diff_density_max         1.972
_refine_diff_density_min         -1.525
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         5191
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0351
_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^)+(0.0478P)^2^+23.5786P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0932
_refine_ls_wR_factor_ref         0.0955
_reflns_number_gt                4470
_reflns_number_total             5191
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9005289_si_001.cif
_cod_data_source_block           compound_1
_cod_original_cell_volume        4441.0(9)
_cod_database_code               4302919