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_4325293
_publ_section_title
;
 Redox Chemistry, Acid Reactivity, and Hydrogenation Reactions of
 Two-Electron Mixed Valence Diiridium and Dirhodium Complexes
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_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         C28H40Cl4f24Ir2N4O8P4
_chemical_formula_sum            'C28 H40 Cl4 F24 Ir2 N4 O8 P4'
_chemical_formula_weight         1666.72
_chemical_name_common            Ir2(tfepma)2(CNtBu)2cl4
_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                 95.925(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.810(2)
_cell_length_b                   13.7756(16)
_cell_length_c                   22.387(3)
_cell_measurement_reflns_used    9697
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      30.97
_cell_measurement_theta_min      2.35
_cell_volume                     5463.2(11)
_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, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(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  0.0532
_diffrn_reflns_av_sigmaI/netI    0.0306
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            115190
_diffrn_reflns_theta_full        28.70
_diffrn_reflns_theta_max         28.70
_diffrn_reflns_theta_min         1.39
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.306
_exptl_absorpt_correction_T_max  0.4167
_exptl_absorpt_correction_T_min  0.2989
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.026
_exptl_crystal_description       block
_exptl_crystal_F_000             3192
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.505
_refine_diff_density_min         -1.230
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     752
_refine_ls_number_reflns         14135
_refine_ls_number_restraints     289
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0338
_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^)+(0.0354P)^2^+16.2201P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0781
_refine_ls_wR_factor_ref         0.0896
_reflns_number_gt                10756
_reflns_number_total             14135
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2005248_si_002_06.cif
_cod_data_source_block           7
_cod_depositor_comments
;
 Updating space group information.

 Antanas Vaitkus,
 2018-07-15
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_cod_original_cell_volume        5463.1(11)
_cod_database_code               4325293