Catalytic Allylic Alkylation and Allylic Phenolation Reactions with Ruthenium Complexes. Solid-State Structures of a Model Catalytic DMF Intermediate, [Ru(Cp*)(Cl)(η3-C3H5)(DMF)](PF6), and a New Tetranuclear Salt, [Ru(Cp){Ru(Cp)(η6-p-CH3C6H4CN)}3](PF6)4
Hermatschweiler, René; Fernández, Ignacio; Pregosin, Paul S.; Breher, Frank; Organometallics 25 (2006) 1440–1447; doi:10.1021/om051050l

data_4074953
_publ_section_title
;
 Catalytic Allylic Alkylation and Allylic Phenolation Reactions with
 Ruthenium Complexes. Solid-State Structures of a Model Catalytic DMF
 Intermediate, [Ru(Cp*)(Cl)(\h3-C3H5)(DMF)](PF6), and a New Tetranuclear
 Salt, [Ru(Cp){Ru(Cp)(\h6-p-CH3C6H4CN)}3](PF6)4
;
_journal_coden_ASTM              ORGND7
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1440
_journal_page_last               1447
_journal_paper_doi               10.1021/om051050l
_journal_volume                  25
_journal_year                    2006
_chemical_formula_moiety         'C44 H41 N3 Ru4, 4(F6 P)'
_chemical_formula_sum            'C44 H41 F24 N3 P4 Ru4'
_chemical_formula_weight         1595.96
_space_group_IT_number           161
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'R 3 -2"c'
_symmetry_space_group_name_H-M   'R 3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   17.5476(5)
_cell_length_b                   17.5476(5)
_cell_length_c                   30.2034(17)
_cell_measurement_temperature    200(2)
_cell_volume                     8054.2(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep32 for Windows'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.959
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'Bruker Apex with CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0756
_diffrn_reflns_av_sigmaI/netI    0.0861
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            17798
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         2.32
_exptl_absorpt_coefficient_mu    1.343
_exptl_absorpt_correction_T_max  0.9867
_exptl_absorpt_correction_T_min  0.9736
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.974
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular shaped crystal'
_exptl_crystal_F_000             4668
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.994
_refine_diff_density_min         -0.435
_refine_diff_density_rms         0.113
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.972
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         4187
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      0.982
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0458
_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^)+(0.0203P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0904
_refine_ls_wR_factor_ref         0.0939
_reflns_number_gt                3465
_reflns_number_total             4187
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om051050lsi20051208_101828.cif
_cod_data_source_block           '[Ru(Cp){Ru(Cp)(p-CH3C6H4CN)}3](PF6)4_14'
_cod_original_sg_symbol_Hall     R3-2"c
_cod_original_sg_symbol_H-M      R3c
_cod_database_code               4074953