Monocyclopentadienylhydride Derivatives of Ruthenium: Stereoselective Proton Transfer and Proton-Hydride Exchange in an Extremely Short Dihydrogen Bond
Ester Cayuela; Félix A. Jalón; Blanca R. Manzano; Gustavo Espino; Walter Weissensteiner; Kurt Mereiter; Journal of the American Chemical Society 126 (2004) 7049–7062; doi:10.1021/ja031926k

data_4112622
_publ_contact_author
;
F\'elix A. Jal\'on
Facultad de Qu\'imicas
Universidad de Castilla-La Mancha
Avenida Camilo Jos\'e Cela, 10
13071 Ciudad Real, SPAIN
phone: ++34 926295300 (ext 3473)
fax: ++34 926295318
E-mail: Felix.Jalon@uclm.es
;
_publ_contact_author_email       Felix.Jalon@uclm.es
_publ_contact_author_fax         '+34 926 295318'
_publ_contact_author_phone       '+34 926 295300 (ext 3473)'
_publ_section_title
;
 Monocyclopentadienylhydride Derivatives of Ruthenium: Stereoselective
 Proton Transfer and Proton-Hydride Exchange in an Extremely Short
 Dihydrogen Bond
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7049
_journal_page_last               7062
_journal_paper_doi               10.1021/ja031926k
_journal_volume                  126
_journal_year                    2004
_chemical_formula_moiety         'C44 H37 F3 Fe O2 P2 Ru'
_chemical_formula_sum            'C44 H37 F3 Fe O2 P2 Ru'
_chemical_formula_weight         873.60
_chemical_name_common            CpRu(CF3CO2)(PP^Ph^PF)
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                82.07(2)
_cell_angle_beta                 88.66(2)
_cell_angle_gamma                62.05(2)
_cell_formula_units_Z            2
_cell_length_a                   11.350(5)
_cell_length_b                   11.543(5)
_cell_length_c                   16.084(7)
_cell_measurement_reflns_used    988
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      30.0
_cell_measurement_theta_min      2.4
_cell_volume                     1841.6(14)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT, SADABS, XPREP'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      297(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type
'BRUKER SMART 3-circle with CCD area detector'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0460
_diffrn_reflns_av_sigmaI/netI    0.0349
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            33751
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.02
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.945
_exptl_absorpt_correction_T_max  0.86
_exptl_absorpt_correction_T_min  0.58
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'program SADABS'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.575
_exptl_crystal_description       plate
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.64
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.645
_refine_diff_density_min         -0.571
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         10525
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0328
_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^)+(0.0473P)^2^+0.4512P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0830
_refine_ls_wR_factor_ref         0.0901
_reflns_number_gt                8557
_reflns_number_total             10525
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja031926ksi20031223_025429.cif
_cod_data_source_block           13
_cod_database_code               4112622