Regioselective Synthesis of η4-Dienylphosphane Ruthenium Complexes by Oxidative Coupling Reactions
Díez, J.; Gamasa, M. P.; Lastra, E.; Villar, A.; Pérez-Carreño, E.; Organometallics 26 (2007) 5315–; doi:10.1021/om700476f

data_4073573
_publ_section_title
;
 Regioselective Synthesis of \h4-Dienylphosphane Ruthenium Complexes by
 Oxidative Coupling Reactions
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              5315
_journal_paper_doi               10.1021/om700476f
_journal_volume                  26
_journal_year                    2007
_chemical_compound_source        synthesis
_chemical_formula_moiety         '2(C31 H32 O P Ru), C4 H10 O, 2(F6 P)'
_chemical_formula_sum            'C66 H74 F12 O3 P4 Ru2'
_chemical_formula_weight         1469.27
_chemical_name_systematic
;
 ?
;
_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                 105.379(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.1933(5)
_cell_length_b                   11.7672(5)
_cell_length_c                   21.0420(7)
_cell_measurement_temperature    100(2)
_cell_volume                     3149.8(2)
_computing_cell_refinement       'Bruker Smart'
_computing_data_collection       'Bruker Smart'
_computing_data_reduction        'Bruker Saint'
_computing_molecular_graphics    'Platon (Spek, 2006)'
_computing_publication_material  'Shelxl-97 (Sheldrick, 1997)'
_computing_structure_refinement  'Shelxl-97 (Sheldrick, 1997)'
_computing_structure_solution    'Dirdif-99 (Beurskens, 1999)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'ccd area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0724
_diffrn_reflns_av_sigmaI/netI    0.0681
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            18475
_diffrn_reflns_theta_full        69.49
_diffrn_reflns_theta_max         69.49
_diffrn_reflns_theta_min         3.47
_exptl_absorpt_coefficient_mu    5.549
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.643404
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Sadabs (Sheldrick,G.M.,1997-2001)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.549
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1500
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.826
_refine_diff_density_min         -0.518
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         5683
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0782
_refine_ls_R_factor_gt           0.0494
_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^)+(0.0626P)^2^+1.1655P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1103
_refine_ls_wR_factor_ref         0.1231
_reflns_number_gt                4128
_reflns_number_total             5683
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om700476f-file005.cif
_cod_data_source_block           9a
_cod_original_sg_symbol_Hall     '-p 2ybc'
_cod_original_sg_symbol_H-M      'p 21/c'
_cod_original_formula_sum        'C66 H74 F12 O3 P4 Ru2 '
_cod_database_code               4073573