Allenylidene/Alkenylcarbyne Synthesis and Reactivity in Ruthenium Complexes with Monodentate Phosphine Ligands
Pino-Chamorro, Jose Angel; Bustelo, Emilio; Puerta, M. Carmen; Valerga, Pedro; Organometallics 28 (2009) 1546–; doi:10.1021/om801125f

data_4068842
_publ_section_title
;
 Allenylidene/Alkenylcarbyne Synthesis and Reactivity in Ruthenium
 Complexes with Monodentate Phosphine Ligands
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1546
_journal_paper_doi               10.1021/om801125f
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C37 H56 P2 Ru, 2(C32 H12 B F24), 2(C6 H5 F)'
_chemical_formula_sum            'C113 H90 B2 F50 P2 Ru'
_chemical_formula_weight         2582.48
_chemical_name_common
;
[(\h^5^-C~5~Me~5~)Ru{C-CH=CPh~2~}(PEt~3~)~2~]
[B(C~8~H~3~F~6~)~4~]~2~.2(FC~6~H~5~)
;
_chemical_name_systematic
;
(3,3-diphenylprop-2-en-1-ynyl)-(\h^5^-pentamethylcyclopentadienyl)-bis(triethyl 
phosphine)-ruthenium(II) tetrakis{3,5-bis(trifluoromethyl)phenyl}borate 
2 fluorobenzene solvate
;
_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                90.02(3)
_cell_angle_beta                 102.82(3)
_cell_angle_gamma                108.58(3)
_cell_formula_units_Z            2
_cell_length_a                   14.050(3)
_cell_length_b                   14.112(3)
_cell_length_c                   30.307(6)
_cell_measurement_reflns_used    5703
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.939
_cell_measurement_theta_min      2.290
_cell_volume                     5537(2)
_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 (Faruggia, 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 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0298
_diffrn_reflns_av_sigmaI/netI    0.0489
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            39406
_diffrn_reflns_theta_full        25.04
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         1.38
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Bruker SMART APEX'
_diffrn_standards_decay_%        -0.0066
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.304
_exptl_absorpt_correction_T_max  0.970
_exptl_absorpt_correction_T_min  0.873
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.549
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2604
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.969
_refine_diff_density_min         -0.567
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1547
_refine_ls_number_reflns         19314
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0702
_refine_ls_R_factor_gt           0.0638
_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^)+(0.0530P)^2^+16.8513P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1420
_refine_ls_wR_factor_ref         0.1462
_reflns_number_gt                17663
_reflns_number_total             19314
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om801125f_si_001.cif
_cod_data_source_block           CCDC708294
_cod_original_cell_volume        5538(2)
_cod_database_code               4068842