Ruthenium(II) Picolyl-NHC Complexes: Synthesis, Characterization, and Catalytic Activity in Amine N-alkylation and Transfer Hydrogenation Reactions
Fernández, Francys E.; Puerta, M. Carmen; Valerga, Pedro; Organometallics 31 (2012) 6868–; doi:10.1021/om300692a

data_4079342
_publ_section_title
;
 Ruthenium(II) Picolyl-NHC Complexes: Synthesis, Characterization, and
 Catalytic Activity in Amine N-alkylation and Transfer Hydrogenation
 Reactions
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              6868
_journal_paper_doi               10.1021/om300692a
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C20 H25 Cl N3 Ru, F6 P'
_chemical_formula_sum            'C20 H25 Cl F6 N3 P Ru'
_chemical_formula_weight         588.92
_chemical_name_systematic
;Chlorido-(\h^6^-p-cymene)-{\k^2^ <i>C</i>,<i>N</i>-3-methyl-1-
(pyrid-2-ylmethyl)-2,3-dihydro-imidazole-2-ylidene}-ruthenium(II)
hexafluorophosphate
;
_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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.98(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.321(3)
_cell_length_b                   10.964(2)
_cell_length_c                   17.109(3)
_cell_measurement_reflns_used    5371
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.579
_cell_measurement_theta_min      2.398
_cell_volume                     2294.1(8)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics    'ORTEP-3 vers. 1.08 (Farrugia, 2005)'
_computing_publication_material  'SHELXTL (Sheldrick, 2001)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2001)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2001)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.941
_diffrn_measured_fraction_theta_max 0.941
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '1700 omega scan frames, 0.3 deg, 10 sec'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0476
_diffrn_reflns_av_sigmaI/netI    0.0502
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11482
_diffrn_reflns_theta_full        24.63
_diffrn_reflns_theta_max         24.63
_diffrn_reflns_theta_min         1.67
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Bruker SMART APEX'
_diffrn_standards_decay_%        0.0009
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.931
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.877
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.705
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.494
_refine_diff_density_min         -0.584
_refine_diff_density_rms         0.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         3654
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0793
_refine_ls_R_factor_gt           0.0638
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1111P)^2^+10.2885P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1850
_refine_ls_wR_factor_ref         0.1961
_reflns_number_gt                2849
_reflns_number_total             3654
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300692a_si_002.cif
_cod_data_source_block           pv1207
_cod_original_cell_volume        2294.2(8)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4079342