Proton-Assisted Activation of Dihydrogen: Mechanistic Aspects of Proton-Catalyzed Addition of H2 to Ru and Ir Amido Complexes
Zachariah M. Heiden; Thomas B. Rauchfuss; Journal of the American Chemical Society 131 (2009) 3593–3600; doi:10.1021/ja807277s

data_4103995
_publ_contact_author
; 
Zachariah M. Heiden 
University of Illinois 
School of Chemical Sciences, Box 80-6 
600 South Goodwin Avenue 
Urbana, Illinois  61801 
USA 
;
_publ_contact_author_email       zheiden2@uiuc.edu
_publ_contact_author_phone       '1  217 333 2236'
_publ_section_title
;
 Proton-Assisted Activation of Dihydrogen: Mechanistic Aspects of
 Proton-Catalyzed Addition of H2 to Ru and Ir Amido Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3593
_journal_page_last               3600
_journal_paper_doi               10.1021/ja807277s
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         '2(C31 H36 Ir N2 O2 S), 2(C F3 O3 S), H2 O'
_chemical_formula_sum            'C64 H74 F6 Ir2 N4 O11 S4'
_chemical_formula_weight         1701.91
_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
; 
2008-08-06   text and data added, zmh 
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.074(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.181(8)
_cell_length_b                   17.048(6)
_cell_length_c                   14.967(5)
_cell_measurement_reflns_used    970
_cell_measurement_temperature    198(2)
_cell_measurement_theta_max      23.39
_cell_measurement_theta_min      2.39
_cell_volume                     6680(4)
_computing_cell_refinement       'SAINT V7.23A (Bruker, 2005)'
_computing_data_collection       'SMART V5.625 (Bruker, 2001)'
_computing_data_reduction
; 
SAINT V7.23A, XPREP V2005/2, SADABS V2007/4, TWINABS V2007/5 
(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      198(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'Siemens Platform/CCD'
_diffrn_measurement_method       'profile data from \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  b47aas
_diffrn_reflns_av_R_equivalents  0.0895
_diffrn_reflns_av_sigmaI/netI    0.0820
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            69266
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.57
_diffrn_standards_decay_%        3.2
_diffrn_standards_interval_time  205
_diffrn_standards_number         417
_exptl_absorpt_coefficient_mu    4.183
_exptl_absorpt_correction_T_max  0.5759
_exptl_absorpt_correction_T_min  0.3598
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP V2005/2 (Bruker, 2005)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.692
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3384
_exptl_crystal_id                b47aas
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (-1 1 0) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_refine_diff_density_max         4.839
_refine_diff_density_min         -3.003
_refine_diff_density_rms         0.198
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     871
_refine_ls_number_reflns         12328
_refine_ls_number_restraints     1049
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0977
_refine_ls_R_factor_gt           0.0624
_refine_ls_shift/su_max          0.039
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0928P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1537
_refine_ls_wR_factor_ref         0.1653
_reflns_number_gt                7768
_reflns_number_total             12328
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja807277s_si_002.cif
_cod_data_source_block           b47aas
_cod_original_sg_symbol_Hall     '-P 2ybc '
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_database_code               4103995