Ruthenium-Mediated Cyclometalation Reactions of Allene and Allylphosphine C═C Bonds: Synthesis of κ(P),η4-(Hexa-2,5-dien-1-yl)diphenylphosphine‒Ruthenium(II) Complexes
Villar, Amparo; Díez, Josefina; Lastra, Elena; Gamasa, M. Pilar; Organometallics 30 (2011) 5803–; doi:10.1021/om200668h

data_4065267
_publ_section_title
;
 Ruthenium-Mediated Cyclometalation Reactions of Allene and Allylphosphine
 C&#x2550;C Bonds: Synthesis of
 \k(P),\h4-(Hexa-2,5-dien-1-yl)diphenylphosphine--Ruthenium(II) Complexes
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              5803
_journal_paper_doi               10.1021/om200668h
_journal_volume                  30
_journal_year                    2011
_chemical_compound_source        synthesis
_chemical_formula_moiety
'2(C32 H12 B F24), 2(C30 H38 P Ru), 0.5(C6 H14)'
_chemical_formula_sum            'C127 H107 B2 F48 P2 Ru2'
_chemical_formula_weight         2830.83
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                107.61(2)
_cell_angle_beta                 96.99(2)
_cell_angle_gamma                104.684(16)
_cell_formula_units_Z            2
_cell_length_a                   12.868(2)
_cell_length_b                   21.135(4)
_cell_length_c                   25.841(9)
_cell_measurement_reflns_used    39966
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      74.4812
_cell_measurement_theta_min      3.4038
_cell_volume                     6328(3)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET)
(compiled Aug 28 2006,13:05:05)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET)
(compiled Aug 28 2006,13:05:05)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET)
(compiled Aug 28 2006,13:05:05)
;
_computing_molecular_graphics    'PLATON (Spek, 2007)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXH-97 (Sheldrick, 1997)'
_computing_structure_solution    DIRDIF-1999
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.2640
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device
; 
165 mm Onyx CCD detector in \k-geometry diffractometer
;
_diffrn_measurement_device_type  'Xcalibur, Onyx, Nova'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Nova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_av_sigmaI/netI    0.0259
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            78915
_diffrn_reflns_theta_full        74.91
_diffrn_reflns_theta_max         74.91
_diffrn_reflns_theta_min         3.41
_exptl_absorpt_coefficient_mu    3.231
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.15991
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET)
(compiled Aug 28 2006,13:05:05)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.486
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2858
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.259
_refine_diff_density_min         -0.723
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1601
_refine_ls_number_reflns         25038
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.0949
_refine_ls_R_factor_gt           0.0779
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1635P)^2^+3.5661P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2381
_refine_ls_wR_factor_ref         0.2619
_reflns_number_gt                18227
_reflns_number_total             25038
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200668h_si_002.cif
_cod_data_source_block           6a
_cod_database_code               4065267