Cooperative Bimetallic Reactivity: Hydrogen Activation in Two-Electron Mixed-Valence Compounds
Thomas G. Gray; Adam S. Veige; Daniel G. Nocera; Journal of the American Chemical Society 126 (2004) 9760–9768; doi:10.1021/ja0491432

data_4112837
_publ_contact_author             'Daniel G. Nocera'
_publ_contact_author_email       nocera@mit.edu
_publ_section_title
;
 Cooperative Bimetallic Reactivity: Hydrogen Activation in Two-Electron
 Mixed-Valence Compounds
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9760
_journal_page_last               9768
_journal_paper_doi               10.1021/ja0491432
_journal_volume                  126
_journal_year                    2004
_chemical_formula_moiety         C27H33Cl2F36Ir2N3O12P6,3(C2H3N)
_chemical_formula_sum            'C33 H42 Cl2 F36 Ir2 N6 O12 P6'
_chemical_formula_weight         2039.85
_chemical_name_common            none
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   '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                 99.908(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.3635(15)
_cell_length_b                   23.491(3)
_cell_length_c                   23.867(3)
_cell_measurement_reflns_used    5822
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      46.646
_cell_measurement_theta_min      4.382
_cell_volume                     6828.3(15)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_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      193(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\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    0.0638
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            25493
_diffrn_reflns_theta_full        23.31
_diffrn_reflns_theta_max         23.31
_diffrn_reflns_theta_min         2.19
_exptl_absorpt_coefficient_mu    4.264
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.984
_exptl_crystal_description       block
_exptl_crystal_F_000             3920
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.28
_refine_diff_density_max         4.780
_refine_diff_density_min         -2.610
_refine_diff_density_rms         0.230
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.284
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     797
_refine_ls_number_reflns         9759
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.283
_refine_ls_R_factor_all          0.1008
_refine_ls_R_factor_gt           0.0919
_refine_ls_shift/su_max          0.050
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0619P)^2^+174.3487P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2049
_refine_ls_wR_factor_ref         0.2091
_reflns_number_gt                8883
_reflns_number_total             9759
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0491432si20040519_092930.cif
_cod_data_source_block           new
_cod_original_cell_volume        6828.3(14)
_cod_database_code               4112837