Synthesis of NHC-Oxazoline Pincer Complexes of Rh and Ru and Their Catalytic Activity for Hydrogenation and Conjugate Reduction
Ito, Jun-ichi; Sugino, Kanae; Matsushima, Satoru; Sakaguchi, Hiroki; Iwata, Hiroshi; Ishihara, Takahiro; Nishiyama, Hisao; Organometallics 35 (2016) 1885–; doi:10.1021/acs.organomet.6b00239

data_4088613
_publ_section_title
;
 Synthesis of NHC-Oxazoline Pincer Complexes of Rh and Ru and Their
 Catalytic Activity for Hydrogenation and Conjugate Reduction
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              1885
_journal_paper_doi               10.1021/acs.organomet.6b00239
_journal_volume                  35
_journal_year                    2016
_chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk'
_chemical_formula_moiety         'C24 H31 N3 O4 Ru'
_chemical_formula_sum            'C24 H31 N3 O4 Ru'
_chemical_formula_weight         526.60
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-03-23
_audit_creation_method           'by CrystalStructure 4.0'
_cell_angle_alpha                90.0000
_cell_angle_beta                 105.106(5)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            2
_cell_length_a                   9.367(4)
_cell_length_b                   10.864(4)
_cell_length_c                   12.295(5)
_cell_measurement_reflns_used    5090
_cell_measurement_temperature    293
_cell_measurement_theta_max      31.02
_cell_measurement_theta_min      3.09
_cell_volume                     1207.9(8)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293
_diffrn_detector_area_resol_mean 7.111
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0212
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9584
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.683
_exptl_absorpt_correction_T_max  0.966
_exptl_absorpt_correction_T_min  0.901
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             544.00
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.840
_refine_diff_density_min         -0.320
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  2223 Friedel Pairs'
_refine_ls_abs_structure_Flack   -0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     289
_refine_ls_number_reflns         5106
_refine_ls_number_restraints     1
_refine_ls_R_factor_gt           0.0218
_refine_ls_shift/su_max          0.023
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0242P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0549
_reflns_number_gt                4580
_reflns_number_total             5108
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om6b00239_si_001.cif
_cod_data_source_block           9b
_cod_database_code               4088613