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_4107320
_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         'C31 H39 F3 Ir N O'
_chemical_formula_sum            'C31 H39 F3 Ir N O'
_chemical_formula_weight         690.83
_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
_audit_update_record
; 
2007-01-23   text and data added, mrr 
;
_cell_angle_alpha                90.00
_cell_angle_beta                 112.1540(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.9623(2)
_cell_length_b                   22.1940(5)
_cell_length_c                   12.8804(3)
_cell_measurement_reflns_used    5678
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      31.55
_cell_measurement_theta_min      2.51
_cell_volume                     2902.41(11)
_computing_cell_refinement       'SAINT V6.22 (Bruker, 2001)'
_computing_data_collection       'APEX2 V1.0-27 (Bruker, 2004)'
_computing_data_reduction        'SAINT V6.22 (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL V6.12 (Bruker, 2001)'
_computing_publication_material  'XCIF (Bruker, 2001)'
_computing_structure_refinement  'SHELXTL V6.12 (Bruker, 2001)'
_computing_structure_solution    'SHELXTL V6.12 (Bruker, 2001)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_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  ga34pas
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_sigmaI/netI    0.0400
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            39922
_diffrn_reflns_theta_full        32.11
_diffrn_reflns_theta_max         32.11
_diffrn_reflns_theta_min         1.84
_exptl_absorpt_coefficient_mu    4.643
_exptl_absorpt_correction_T_max  0.7585
_exptl_absorpt_correction_T_min  0.4005
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP (Bruker, 2001)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.581
_exptl_crystal_description       tabular
_exptl_crystal_F_000             1376
_exptl_crystal_id                ga34pas
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (4 0 -3) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.239
_refine_diff_density_min         -1.196
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         9761
_refine_ls_number_restraints     165
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0349
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0388P)^2^+7.7586P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0827
_refine_ls_wR_factor_ref         0.0925
_reflns_number_gt                7440
_reflns_number_total             9761
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja076801k-file002.cif
_cod_data_source_block           ga34pas
_cod_original_sg_symbol_Hall     '-P 2ybc '
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_database_code               4107320