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_4068841
_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         'C30.92 H51 P2 Ru, B F4'
_chemical_formula_sum            'C30.92 H51 B F4 P2 Ru'
_chemical_formula_weight         672.58
_chemical_name_common
;          
[(\h^5^-C~5~Me~5~)Ru(=C=C=CHPh)(PEt~3~)~2~][BF~4~]
;
_chemical_name_systematic
;
(\h^5^-pentamethyl-cyclopentadienyl)-(3-phenylallenylidene)-
bis(triethylphosphine)-ruthenium (II) tetrafluoroborate
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.976(2)
_cell_length_b                   10.613(2)
_cell_length_c                   30.708(6)
_cell_measurement_reflns_used    5099
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.67
_cell_measurement_theta_min      2.33
_cell_volume                     3251.2(11)
_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 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.0432
_diffrn_reflns_av_sigmaI/netI    0.0406
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            20932
_diffrn_reflns_theta_full        24.15
_diffrn_reflns_theta_max         24.15
_diffrn_reflns_theta_min         2.03
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Bruker SMART APEX'
_diffrn_standards_decay_%        0.0065
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.623
_exptl_absorpt_correction_T_max  0.894
_exptl_absorpt_correction_T_min  0.801
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.374
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1406.1
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.974
_refine_diff_density_min         -0.490
_refine_diff_density_rms         0.105
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         5109
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_gt           0.0693
_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^)+(0.0908P)^2^+10.8320P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1715
_refine_ls_wR_factor_ref         0.1732
_reflns_number_gt                4947
_reflns_number_total             5109
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om801125f_si_001.cif
_cod_data_source_block           CCDC708293
_cod_database_code               4068841