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_4113561
_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(h2-CHCH)][BPh4]'
_chemical_name_systematic
;  
(penta-hapto-pentamethylcyclopentadienyl)-bis(triethylphosphino)- 
(di-hapto-alkyne)-ruthenium tetraphenylborate  
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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                 94.670(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.424(3)
_cell_length_b                   21.503(6)
_cell_length_c                   19.484(5)
_cell_measurement_reflns_used    999
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.4
_cell_volume                     4353(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT, SADABS and XPREP'
_computing_molecular_graphics    'ORTEP-3 vers. 1.07 (L.J. Faruggia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.0507
_diffrn_reflns_av_sigmaI/netI    0.0385
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            44447
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.10
_exptl_absorpt_coefficient_mu    0.465
_exptl_absorpt_correction_T_max  0.89
_exptl_absorpt_correction_T_min  0.80
_exptl_absorpt_correction_type   'Semi-empirical from equivalents with SADABS'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_description       block
_exptl_crystal_F_000             1736
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.990
_refine_diff_density_min         -0.633
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     475
_refine_ls_number_reflns         7556
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0635
_refine_ls_R_factor_gt           0.0477
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0632P)^2^+5.5672P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1211
_refine_ls_wR_factor_ref         0.1325
_reflns_number_gt                5942
_reflns_number_total             7556
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0291181si20030114_055415_1.cif
_cod_data_source_block           pvxy666
_cod_database_code               4113561