Redox-Switched Oxidation of Dihydrogen Using a Non-Innocent Ligand
Mark R. Ringenberg; Swarna Latha Kokatam; Zachariah M. Heiden; Thomas B. Rauchfuss; Journal of the American Chemical Society 130 (2008) 788–789; doi:10.1021/ja076801k

data_4107321
_publ_section_title
;
 Redox-Switched Oxidation of Dihydrogen Using a Non-Innocent Ligand
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              788
_journal_page_last               789
_journal_paper_doi               10.1021/ja076801k
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety
'C32 H12 B F24, C31 H39 F3 Ir N O, 2(C H2 Cl2)'
_chemical_formula_sum            'C65 H55 B Cl4 F27 Ir N O'
_chemical_formula_weight         1723.91
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
; 
?2007-10-17   text and data added, mrr 
;
_cell_angle_alpha                102.098(2)
_cell_angle_beta                 102.096(2)
_cell_angle_gamma                100.019(2)
_cell_formula_units_Z            2
_cell_length_a                   12.7251(3)
_cell_length_b                   16.5921(4)
_cell_length_c                   18.5918(5)
_cell_measurement_reflns_used    8715
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      18.93
_cell_measurement_theta_min      2.25
_cell_volume                     3654.24(17)
_computing_cell_refinement       'SAINT V7.23A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2.0-1 (Bruker, 2004)'
_computing_data_reduction
; 
SAINT V7.23A, XPREP V2005/2, SADABS V2007/4 (Bruker, 2005 & 2007) 
;
_computing_molecular_graphics    'SHELXTL V6.12 (Bruker, 2005)'
_computing_publication_material  'XCIF V6.12 (Bruker, 2005)'
_computing_structure_refinement  'SHELXTL V6.12 (Bruker, 2005)'
_computing_structure_solution    'SHELXTL V6.12 (Bruker, 2005)'
_diffrn_ambient_temperature      297(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device       'Bruker Kappa/ApexII CCD'
_diffrn_measurement_method       'profile data from \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_radiation_wavelength_id  ga93vas
_diffrn_reflns_av_R_equivalents  0.0516
_diffrn_reflns_av_sigmaI/netI    0.0689
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            45524
_diffrn_reflns_theta_full        25.76
_diffrn_reflns_theta_max         25.76
_diffrn_reflns_theta_min         1.50
_exptl_absorpt_coefficient_mu    2.082
_exptl_absorpt_correction_T_max  0.8193
_exptl_absorpt_correction_T_min  0.5720
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP V2005/2 (Bruker, 2005)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.567
_exptl_crystal_description       prism
_exptl_crystal_F_000             1706
_exptl_crystal_id                ga93vas
_exptl_crystal_preparation
; 
The data crystal was mounted using epoxy to a 0.3 mm cryo-loop 
(Hampton Research) with the (-1 2 2) scattering planes roughly normal 
to the spindle axis. 
;
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.11
_refine_diff_density_max         3.233
_refine_diff_density_min         -1.278
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1424
_refine_ls_number_reflns         13774
_refine_ls_number_restraints     3824
_refine_ls_restrained_S_all      0.968
_refine_ls_R_factor_all          0.1112
_refine_ls_R_factor_gt           0.0657
_refine_ls_shift/su_max          0.039
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0862P)^2^+8.3172P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1574
_refine_ls_wR_factor_ref         0.1819
_reflns_number_gt                8911
_reflns_number_total             13774
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja076801k-file003.cif
_cod_data_source_block           ga93vas
_cod_original_cell_volume        3654.24(16)
_cod_original_sg_symbol_Hall     '-P 1 '
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4107321