A Cyclometalated Ruthenium-NHC Precatalyst for the Asymmetric Hydrogenation of (Hetero)arenes and Its Activation Pathway
Paul, Daniel; Beiring, Bernhard; Plois, Markus; Ortega, Nuria; Kock, Slawomir; Schlüns, Danny; Neugebauer, Johannes; Wolf, Robert; Glorius, Frank; Organometallics 35 (2016) 3641–; doi:10.1021/acs.organomet.6b00702

data_4089103
_publ_section_title
;
 A Cyclometalated Ruthenium-NHC Precatalyst for the Asymmetric
 Hydrogenation of (Hetero)arenes and Its Activation Pathway
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              3641
_journal_paper_doi               10.1021/acs.organomet.6b00702
_journal_volume                  35
_journal_year                    2016
_chemical_formula_sum            'C38 H62 N4 Ru'
_chemical_formula_weight         675.99
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.9810(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.2090(4)
_cell_length_b                   18.2754(9)
_cell_length_c                   21.1889(9)
_cell_measurement_reflns_used    9152
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      29.67
_cell_measurement_theta_min      2.23
_cell_volume                     3500.8(3)
_computing_cell_refinement       'APEX2(Bruker AXS, 2007)'
_computing_data_collection       'APEX2(Bruker AXS, 2007)'
_computing_data_reduction        'SAINT,SADABS (Bruker AXS, 2007 )'
_computing_molecular_graphics
;
ORTEP3,L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565
;
_computing_structure_refinement
;
SHELXL-97, G. M. Sheldrick, Acta Cryst. (2008) A64, 112-122
;
_computing_structure_solution
;
SHELXS-97 , G. M. Sheldrick, Acta Cryst. (2008) A64, 112-122
;
_diffrn_ambient_temperature      153(1)
_diffrn_detector_area_resol_mean 80
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'Omega and Phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_av_sigmaI/netI    0.0250
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            19964
_diffrn_reflns_theta_full        29.72
_diffrn_reflns_theta_max         29.72
_diffrn_reflns_theta_min         1.96
_exptl_absorpt_coefficient_mu    0.479
_exptl_absorpt_correction_T_max  0.9649
_exptl_absorpt_correction_T_min  0.9145
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.283
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.498
_refine_diff_density_min         -0.257
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         4973
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0274
_refine_ls_R_factor_gt           0.0240
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0318P)^2^+1.6885P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0597
_refine_ls_wR_factor_ref         0.0613
_reflns_number_gt                4574
_reflns_number_total             4973
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om6b00702_si_003.cif
_cod_data_source_block           mp010411
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4089103