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_4113564
_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         'C26 H49 O2 P2 Ru +, C24 H20 B -'
_chemical_formula_sum            'C50 H69 B O2 P2 Ru'
_chemical_formula_weight         875.87
_chemical_name_common            '[Cp*Ru(PEt3)2(CCCOOMe)][BPh4]'
_chemical_name_systematic
;   
(penta-hapto-pentamethylcyclopentadienyl)-bis(triethylphosphino)- 
(carboxymethyl-vinylidene)-ruthenium tetraphenylborate 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 95.129(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.367(3)
_cell_length_b                   16.006(5)
_cell_length_c                   17.669(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15.5
_cell_measurement_theta_min      12.4
_cell_volume                     4610.2(18)
_computing_cell_refinement       'MSC-Rigaku teXsan'
_computing_data_collection       'MSC-Rigaku teXsan'
_computing_data_reduction        'MSC-Rigaku teXsan'
_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, 1990)'
_diffrn_ambient_temperature      17(2)
_diffrn_measured_fraction_theta_full 0.832
_diffrn_measured_fraction_theta_max 0.832
_diffrn_measurement_device_type  'MSC-Rigaku AFC6S 4-circle diffractometer'
_diffrn_measurement_method       'omega/2theta scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0650
_diffrn_reflns_av_sigmaI/netI    0.1079
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            6808
_diffrn_reflns_theta_full        25.06
_diffrn_reflns_theta_max         25.06
_diffrn_reflns_theta_min         2.54
_diffrn_standards_decay_%        0.80
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.447
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.710
_exptl_absorpt_correction_type   'psi-scan semi-empirical method'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.262
_exptl_crystal_description       prism
_exptl_crystal_F_000             1856
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.665
_refine_diff_density_min         -0.695
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         6808
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.1216
_refine_ls_R_factor_gt           0.0586
_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^)+(0.0695P)^2^+8.4169P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1529
_refine_ls_wR_factor_ref         0.1806
_reflns_number_gt                4004
_reflns_number_total             6808
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0291181si20030114_055415_4.cif
_cod_data_source_block           ebalquin
_cod_original_cell_volume        4610.3(18)
_cod_database_code               4113564