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_4325288
_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         C28H40Cl2F24Ir2N4O8P4
_chemical_formula_sum            'C28 H40 Cl2 F24 Ir2 N4 O8 P4'
_chemical_formula_weight         1595.82
_chemical_name_common            Ir2(tfepma)2(CNtBu)2Cl2
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        '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                 103.753(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.7757(15)
_cell_length_b                   16.831(2)
_cell_length_c                   24.504(3)
_cell_measurement_temperature    100(2)
_cell_volume                     5118.0(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0614
_diffrn_reflns_av_sigmaI/netI    0.0358
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            113463
_diffrn_reflns_theta_full        29.57
_diffrn_reflns_theta_max         29.57
_diffrn_reflns_theta_min         1.48
_exptl_absorpt_coefficient_mu    5.558
_exptl_absorpt_correction_T_max  0.6064
_exptl_absorpt_correction_T_min  0.4028
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.071
_exptl_crystal_description       block
_exptl_crystal_F_000             3056
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.233
_refine_diff_density_min         -0.875
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     657
_refine_ls_number_reflns         14349
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0317
_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^)+(0.0306P)^2^+16.9095P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0712
_refine_ls_wR_factor_ref         0.0786
_reflns_number_gt                11833
_reflns_number_total             14349
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2005248_si_002_01.cif
_cod_data_source_block           2
_cod_depositor_comments
;
 Updating space group information.

 Antanas Vaitkus,
 2018-07-15
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_cod_original_cell_volume        5118.1(10)
_cod_database_code               4325288