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_4089102
_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_absolute_configuration ad
_chemical_formula_sum            'C58 H58 N4 O Ru'
_chemical_formula_weight         928.15
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.10120(10)
_cell_length_b                   13.10640(10)
_cell_length_c                   31.3204(3)
_cell_measurement_reflns_used    7379
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      71.58
_cell_measurement_theta_min      2.82
_cell_volume                     4557.02(7)
_computing_cell_refinement       'SAINT (Bruker AXS, 2000)'
_computing_data_collection       'SMART (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT,SADABS (Bruker AXS, 2000)'
_computing_molecular_graphics
; 
 ? 
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(1)
_diffrn_detector_area_resol_mean 80
_diffrn_measured_fraction_theta_full 0.952
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  goebel-mirror
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0453
_diffrn_reflns_av_sigmaI/netI    0.0385
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            26867
_diffrn_reflns_theta_full        71.83
_diffrn_reflns_theta_max         71.83
_diffrn_reflns_theta_min         2.82
_exptl_absorpt_coefficient_mu    3.138
_exptl_absorpt_correction_T_max  0.7241
_exptl_absorpt_correction_T_min  0.3029
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1944
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.834
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.000(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     601
_refine_ls_number_reflns         8145
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0347
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0620P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0876
_refine_ls_wR_factor_ref         0.0887
_reflns_number_gt                7663
_reflns_number_total             8145
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om6b00702_si_004.cif
_cod_data_source_block           rw070311
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               4089102