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_4074952
_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         'C16 H27 Cl N O Ru, F6 P'
_chemical_formula_sum            'C16 H27 Cl F6 N O P Ru'
_chemical_formula_weight         530.88
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.5587(9)
_cell_length_b                   14.4403(15)
_cell_length_c                   16.9278(18)
_cell_measurement_temperature    200(2)
_cell_volume                     2092.1(4)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0805
_diffrn_reflns_av_sigmaI/netI    0.0711
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            18630
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    1.011
_exptl_absorpt_correction_T_max  0.9703
_exptl_absorpt_correction_T_min  0.5136
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.685
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.76
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.338
_refine_diff_density_min         -1.143
_refine_diff_density_rms         0.134
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.50(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.192
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         4263
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.192
_refine_ls_R_factor_all          0.0888
_refine_ls_R_factor_gt           0.0740
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0538P)^2^+2.8402P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1362
_refine_ls_wR_factor_ref         0.1415
_reflns_number_gt                3636
_reflns_number_total             4263
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om051050lsi20051208_101828.cif
_cod_data_source_block           '[Ru(Cp#Cl(C3H3)(DMF)](PF6)_12'
_cod_original_sg_symbol_Hall     P2ac2ab
_cod_original_sg_symbol_H-M      P212121
_cod_database_code               4074952