Mechanistic Studies of O2 Reduction Effected by Group 9 Bimetallic Hydride Complexes
Thomas S. Teets; Daniel G. Nocera; Journal of the American Chemical Society 133 (2011) 17796–17806; doi:10.1021/ja2069196

data_4107049
_publ_section_title
;
 Mechanistic Studies of O2 Reduction Effected by Group 9 Bimetallic
 Hydride Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17796
_journal_page_last               17806
_journal_paper_doi               10.1021/ja2069196
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C28 H41 Cl3 F24 Ir2 N4 O10 P4'
_chemical_formula_weight         1664.28
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   '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                 91.086(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.003(2)
_cell_length_b                   10.798(2)
_cell_length_c                   18.699(4)
_cell_measurement_reflns_used    4919
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.93
_cell_measurement_theta_min      2.45
_cell_volume                     2625.0(8)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1016
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4479
_diffrn_reflns_theta_full        24.73
_diffrn_reflns_theta_max         24.73
_diffrn_reflns_theta_min         1.89
_exptl_absorpt_coefficient_mu    5.475
_exptl_absorpt_correction_T_max  0.7714
_exptl_absorpt_correction_T_min  0.2904
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.106
_exptl_crystal_description       plate
_exptl_crystal_F_000             1596
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.092
_refine_diff_density_min         -1.735
_refine_diff_density_rms         0.189
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         4479
_refine_ls_number_restraints     987
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0645
_refine_ls_R_factor_gt           0.0493
_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^)+(0.0351P)^2^+0.2789P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1175
_refine_ls_wR_factor_ref         0.1216
_reflns_number_gt                3409
_reflns_number_total             4479
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja2069196_si_002.cif
_cod_data_source_block           6
_cod_database_code               4107049