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_4109952
_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         'C53 H50 N2 O3 Ru, 0.5C8 H16'
_chemical_formula_sum            'C56.5 H58 N2 O3 Ru'
_chemical_formula_weight         914.12
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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
;
manual editing of the CIF file 
created by SHELXTL Ver. 6.10
and processed with modiCIfer-09152005. 
;
_audit_update_record
;
2007-03-12 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 98.959(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.0791(10)
_cell_length_b                   13.6712(12)
_cell_length_c                   28.205(2)
_cell_measurement_reflns_used    9207
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.9358
_cell_measurement_theta_min      2.2656
_cell_volume                     4600.8(6)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0727
_diffrn_reflns_av_sigmaI/netI    0.0629
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            60002
_diffrn_reflns_theta_full        28.34
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_min         1.46
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.388
_exptl_absorpt_correction_T_max  0.9441
_exptl_absorpt_correction_T_min  0.8666
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS  (Bruker-AXS, 2003)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_description       needle
_exptl_crystal_F_000             1916
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.791
_refine_diff_density_min         -0.766
_refine_diff_density_rms         0.173
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     581
_refine_ls_number_reflns         11461
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0887
_refine_ls_R_factor_gt           0.0486
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0719P)^2^+3.3481P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1112
_refine_ls_wR_factor_ref         0.1414
_reflns_number_gt                7958
_reflns_number_total             11461
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja073370xsi20070522_011221.cif
_cod_data_source_block           casey67
_cod_original_cell_volume        4600.9(7)
_cod_original_sg_symbol_Hall     '-P 2ybc     '
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        'C56.50 H58 N2 O3 Ru'
_cod_database_code               4109952