First X-ray Characterization and Theoretical Study of π-Alkyne, Alkynyl-Hydride, and Vinylidene Isomers for the Same Transition Metal Fragment [Cp*Ru(PEt3)2]+
Emilio Bustelo; Jorge J. Carbó; Agustí Lledós; Kurt Mereiter; M. Carmen Puerta; Pedro Valerga; Journal of the American Chemical Society 125 (2003) 3311–3321; doi:10.1021/ja0291181

data_4113562
_publ_contact_author
;
Pedro S. Valerga Jimenez
Departamento de Ciencia de los Materiales e Ingenieria Metalurgica
y Quimica Inorganica. Facultad de Ciencias. Universidad de Cadiz. 
Apartado 40.  Puerto Real  11510. Spain. 
;
_publ_contact_author_email       pedro.valerga@uca.es
_publ_contact_author_fax         +34-956-016288
_publ_contact_author_phone       +34-956-016340
_publ_section_title
;
 First X-ray Characterization and Theoretical Study of \p-Alkyne,
 Alkynyl-Hydride, and Vinylidene Isomers for the Same Transition Metal
 Fragment [Cp*Ru(PEt3)2]+
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3311
_journal_page_last               3321
_journal_paper_doi               10.1021/ja0291181
_journal_volume                  125
_journal_year                    2003
_chemical_formula_moiety         'C24 H47 P2 Ru +, C24 H20 B -'
_chemical_formula_sum            'C48 H67 B P2 Ru'
_chemical_formula_weight         817.84
_chemical_name_common            '[Ru(Cp*)(PEt3)2(H)(kappa1-CCH)]BPh4'
_chemical_name_systematic
;  
(penta-hapto-pentamethylcyclopentadienyl)-bis(triethylphosphino)- 
alkynyl-hydride-ruthenium tetraphenylborate   
;
_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
_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                   13.604(2)
_cell_length_b                   16.518(3)
_cell_length_c                   19.219(3)
_cell_measurement_reflns_used    991
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      27.2
_cell_measurement_theta_min      2.5
_cell_volume                     4318.7(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT, SADABS, XPREP'
_computing_molecular_graphics    'ORTEP-3 vers. 1.07 (L.J. Faruggia, 1997)'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type
'BRUKER SMART 3-circle with CCD area detector'
_diffrn_measurement_method       '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  0.0486
_diffrn_reflns_av_sigmaI/netI    0.0232
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            95978
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.94
_exptl_absorpt_coefficient_mu    0.469
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.76
_exptl_absorpt_correction_type   'Semi-empirical from equivalents with SADABS'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.258
_exptl_crystal_description       prism
_exptl_crystal_F_000             1736
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.572
_refine_diff_density_min         -0.614
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.07(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     483
_refine_ls_number_reflns         9852
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_gt           0.0432
_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^)+(0.0465P)^2^+5.2034P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1046
_refine_ls_wR_factor_ref         0.1115
_reflns_number_gt                8869
_reflns_number_total             9852
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0291181si20030114_055415_2.cif
_cod_data_source_block           pvx661
_cod_database_code               4113562