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_4325296
_publ_section_title
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 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         C40H57F24N5O11P4Rh2S
_chemical_formula_sum            'C40 H57 F24 N5 O11 P4 Rh2 S'
_chemical_formula_weight         1601.67
_chemical_name_common            '[Rh2(tfepma)2(CNtBu)3(mu-H)](OTs)'
_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                 93.474(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.9771(14)
_cell_length_b                   22.103(2)
_cell_length_c                   22.523(2)
_cell_measurement_reflns_used    9900
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.66
_cell_measurement_theta_min      2.42
_cell_volume                     6448.5(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, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(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  0.0733
_diffrn_reflns_av_sigmaI/netI    0.0384
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            94961
_diffrn_reflns_theta_full        24.11
_diffrn_reflns_theta_max         24.11
_diffrn_reflns_theta_min         1.29
_exptl_absorpt_coefficient_mu    0.765
_exptl_absorpt_correction_T_max  0.8620
_exptl_absorpt_correction_T_min  0.7008
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.650
_exptl_crystal_description       block
_exptl_crystal_F_000             3208
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.637
_refine_diff_density_min         -1.351
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.179
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     883
_refine_ls_number_reflns         10253
_refine_ls_number_restraints     647
_refine_ls_restrained_S_all      1.194
_refine_ls_R_factor_all          0.1133
_refine_ls_R_factor_gt           0.0963
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0288P)^2^+119.7426P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2099
_refine_ls_wR_factor_ref         0.2192
_reflns_number_gt                8421
_reflns_number_total             10253
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2005248_si_002_09.cif
_cod_data_source_block           10
_cod_depositor_comments
;
 Updating space group information.

 Antanas Vaitkus,
 2018-07-15
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_cod_original_cell_volume        6448.3(12)
_cod_database_code               4325296