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_4325289
_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         C33H49Cl2F24N5O8P4Rh2,CH2Cl2
_chemical_formula_sum            'C33.5 H50 Cl3 F24 N5 O8 P4 Rh2'
_chemical_formula_weight         1542.83
_chemical_name_common            '[Rh2(tfepma)2(CNtBu)3Cl]Cl'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        '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                 114.407(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   23.342(6)
_cell_length_b                   23.350(6)
_cell_length_c                   23.863(6)
_cell_measurement_temperature    100(2)
_cell_volume                     11844(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0741
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            27273
_diffrn_reflns_theta_full        27.86
_diffrn_reflns_theta_max         27.86
_diffrn_reflns_theta_min         0.96
_exptl_absorpt_coefficient_mu    0.923
_exptl_absorpt_correction_T_max  0.8369
_exptl_absorpt_correction_T_min  0.7692
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   twinabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.730
_exptl_crystal_description       block
_exptl_crystal_F_000             6136
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.879
_refine_diff_density_min         -0.840
_refine_diff_density_rms         0.171
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1548
_refine_ls_number_reflns         27526
_refine_ls_number_restraints     1572
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0963
_refine_ls_R_factor_gt           0.0614
_refine_ls_shift/su_max          0.082
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0419P)^2^+62.0428P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1341
_refine_ls_wR_factor_ref         0.1568
_reflns_number_gt                20955
_reflns_number_total             27273
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2005248_si_002_02.cif
_cod_data_source_block           3
_cod_depositor_comments
;
 Updating space group information.

 Antanas Vaitkus,
 2018-06-08
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_cod_original_formula_sum        'C33.50 H50 Cl3 F24 N5 O8 P4 Rh2'
_cod_database_code               4325289