Intramolecular Trapping of an Intermediate in the Reduction of Imines by a Hydroxycyclopentadienyl Ruthenium Hydride: Support for a Concerted Outer Sphere Mechanism
Charles P. Casey; Timothy B. Clark; Ilia A. Guzei; Journal of the American Chemical Society 129 (2007) 11821–11827; doi:10.1021/ja073370x

data_4109953
_publ_contact_author_address
;
Department of Chemistry
University of Wisconsin-Madison
1101 University Ave
Madison, WI  53706
USA
;
_publ_contact_author_email       iguzei@chem.wisc.edu
_publ_contact_author_fax         608-262-0381
_publ_contact_author_name
;
Guzei, Ilia A. 
;
_publ_contact_author_phone       608-263-4694
_publ_section_title
;
 Intramolecular Trapping of an Intermediate in the Reduction of Imines by
 a Hydroxycyclopentadienyl Ruthenium Hydride: Support for a Concerted
 Outer Sphere Mechanism
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11821
_journal_page_last               11827
_journal_paper_doi               10.1021/ja073370x
_journal_volume                  129
_journal_year                    2007
_chemical_formula_moiety         'C86 H74 N2 O6 Ru2, 4(CH2 Cl2), 2(C7 H8)'
_chemical_formula_sum            'C104 H98 Cl8 N2 O6 Ru2'
_chemical_formula_weight         1957.58
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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
;
manual editing of the CIF file 
created by SHELXTL Ver. 6.10
and processed with modiCIfer-09152005. 
;
_audit_update_record
;
2007-03-05 # Formatted by publCIF
;
_cell_angle_alpha                80.245(3)
_cell_angle_beta                 87.922(4)
_cell_angle_gamma                81.829(3)
_cell_formula_units_Z            1
_cell_length_a                   9.898(2)
_cell_length_b                   10.507(2)
_cell_length_c                   21.638(4)
_cell_measurement_reflns_used    6267
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.1943
_cell_measurement_theta_min      2.2769
_cell_volume                     2195.1(7)
_computing_cell_refinement       'SAINT Ver. 6.22  (Bruker-AXS, 2003)'
_computing_data_collection       'SMART Ver. 5.622 (Bruker-AXS, 2003)'
_computing_data_reduction        'SAINT Ver. 6.22'
_computing_molecular_graphics    'SHELXTL Ver. 6.10'
_computing_publication_material  'SHELXTL Ver. 6.10'
_computing_structure_refinement  'SHELXTL Ver. 6.10'
_computing_structure_solution    'SHELXTL Ver. 6.10 (Bruker-AXS, 2003)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker CCD-1000 area detector'
_diffrn_measurement_method       '0.30\% \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_av_sigmaI/netI    0.0412
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            37090
_diffrn_reflns_theta_full        28.34
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_min         0.95
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.647
_exptl_absorpt_correction_T_max  0.9746
_exptl_absorpt_correction_T_min  0.7552
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS  (Bruker-AXS, 2003)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.481
_exptl_crystal_description       plate
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.04
_platon_squeeze_details
;
The volume occupied by solvent is 20.8 percent of the unit cell.
;
_refine_diff_density_max         1.144
_refine_diff_density_min         -0.338
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.840
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     453
_refine_ls_number_reflns         10795
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.840
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0353
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0570P)^2^+2.0914P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0844
_refine_ls_wR_factor_ref         0.0882
_reflns_number_gt                9029
_reflns_number_total             10795
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja073370xsi20070522_011239.cif
_cod_data_source_block           casey66
_cod_original_cell_volume        2195.1(8)
_cod_original_sg_symbol_Hall     '-P 1        '
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4109953