Redox Chemistry, Acid Reactivity, and Hydrogenation Reactions of Two-Electron Mixed Valence Diiridium and Dirhodium Complexes
Thomas S. Teets; Timothy R. Cook; Brian D. McCarthy; Daniel G. Nocera; Inorganic Chemistry 50 (2011) 5223–5233; doi:10.1021/ic2005248

data_4325295
_publ_section_title
;
 Redox Chemistry, Acid Reactivity, and Hydrogenation Reactions of
 Two-Electron Mixed Valence Diiridium and Dirhodium Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5223
_journal_page_last               5233
_journal_paper_doi               10.1021/ic2005248
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         C35H48Cl2F24Ir2N4O11P4S,CH2Cl2
_chemical_formula_sum            'C36.25 H50.5 Cl4.5 F24 Ir2 N4 O11 P4 S'
_chemical_formula_weight         1874.17
_chemical_name_common            Ir2(tfepma)2(CNtBu)2(H)(OTs)
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        '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                 130.3560(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   29.043(3)
_cell_length_b                   29.565(3)
_cell_length_c                   19.9842(18)
_cell_measurement_reflns_used    9876
_cell_measurement_temperature    175(2)
_cell_measurement_theta_max      26.34
_cell_measurement_theta_min      2.30
_cell_volume                     13076(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      175(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0570
_diffrn_reflns_av_sigmaI/netI    0.0298
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            107930
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.15
_exptl_absorpt_coefficient_mu    4.499
_exptl_absorpt_correction_T_max  0.4664
_exptl_absorpt_correction_T_min  0.3455
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.904
_exptl_crystal_description       block
_exptl_crystal_F_000             7252
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.633
_refine_diff_density_min         -1.076
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     815
_refine_ls_number_reflns         11581
_refine_ls_number_restraints     76
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0639
_refine_ls_R_factor_gt           0.0426
_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^)+(0.0562P)^2^+141.0708P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1066
_refine_ls_wR_factor_ref         0.1263
_reflns_number_gt                9050
_reflns_number_total             11581
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2005248_si_002_08.cif
_cod_data_source_block           9
_cod_depositor_comments
;
 Updating space group information.

 Antanas Vaitkus,
 2018-06-10
;
_cod_original_formula_sum        'C36.25 H50.50 Cl4.50 F24 Ir2 N4 O11 P4 S'
_cod_database_code               4325295