Synthesis of Paramagnetic Tetranuclear Rhodium and Iridium Complexes with the 2,6-Pyridinedithiolate Ligand. Redox-Induced Degradation to Diamagnetic Triiridium Compounds
Miguel A. Casado; Jesús J. Pérez-Torrente; José A. López; Miguel A. Ciriano; Pablo J. Alonso; Fernando J. Lahoz; Luis A. Oro; Inorganic Chemistry 40 (2001) 4785–4792; doi:10.1021/ic001349q

data_4320157
_publ_contact_author
;
   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@posta.unizar.es
_publ_section_title
;
 Synthesis of Paramagnetic Tetranuclear Rhodium and Iridium Complexes with
 the 2,6-Pyridinedithiolate Ligand. Redox-Induced Degradation to
 Diamagnetic Triiridium Compounds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4785
_journal_page_last               4792
_journal_paper_doi               10.1021/ic001349q
_journal_volume                  40
_journal_year                    2001
_chemical_formula_moiety         '(C34 H42 Ir3 N2 S4 +), (B F4 -)'
_chemical_formula_sum            'C34 H42 B F4 Ir3 N2 S4'
_chemical_formula_weight         1270.35
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 96.395(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.9234(9)
_cell_length_b                   22.002(4)
_cell_length_c                   19.786(3)
_cell_measurement_reflns_used    46
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      16
_cell_measurement_theta_min      12.5
_cell_volume                     3427.8(9)
_computing_cell_refinement       'DIF4 (Stoe)'
_computing_data_collection       'DIF4 (Stoe)'
_computing_data_reduction        'REDU4 (Stoe)'
_computing_molecular_graphics    'XP, SHELXTL v.5 (Siemens)'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Giacovazzo, 1994)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Siemens-Stoe AED2'
_diffrn_measurement_method       '\w-2\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal focus Mo sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0379
_diffrn_reflns_av_sigmaI/netI    0.0354
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -3
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            6907
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.59
_diffrn_standards_decay_%        'no decay'
_diffrn_standards_interval_time  55
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    11.914
_exptl_absorpt_correction_T_max  0.09451
_exptl_absorpt_correction_T_min  0.04254
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
  Azimuthal psi-scans of 12 reflections at 10\% intervals.
  Data corrected with the program: XPREP, SHELXTL v. 5 (Siemens)
;
_exptl_crystal_colour            dark-purple
_exptl_crystal_density_diffrn    2.462
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             2384
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.834
_refine_diff_density_min         -1.405
_refine_diff_density_rms         0.203
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     436
_refine_ls_number_reflns         6026
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0354
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0410P)^2^+44.6149P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0861
_refine_ls_wR_factor_ref         0.0933
_reflns_number_gt                5057
_reflns_number_total             6026
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic001349q.cif
_cod_data_source_block           compound5b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4320157