Proton-Transfer Reactions to Half-Sandwich Ruthenium Trihydride Complexes Bearing Hemilabile P,N Ligands: Experimental and Density Functional Theory Studies
Manuel Jiménez-Tenorio; M. Carmen Puerta; Pedro Valerga; Salvador Moncho; Gregori Ujaque; Agustí Lledós; Inorganic Chemistry 49 (2010) 6035–6057; doi:10.1021/ic100710d

data_4315949
_publ_contact_author_address
;
Departamento de CMIM y Qu\'imica Inorg\'anica
Universidad de C\'adiz
Facultad de Ciencias
Campus Universitario del R\'io San Pedro
11510. Puerto Real. SPAIN.
;
_publ_contact_author_email       pedro.valerga@uca.es
_publ_contact_author_fax         '34 (956) 016288'
_publ_contact_author_name        'Pedro Valerga'
_publ_contact_author_phone       '34 (956) 016340'
_publ_section_title
;
 Proton-Transfer Reactions to Half-Sandwich Ruthenium Trihydride Complexes
 Bearing Hemilabile P,N Ligands: Experimental and Density Functional
 Theory Studies
;
_journal_issue                   13
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6035
_journal_page_last               6057
_journal_paper_doi               10.1021/ic100710d
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C32 H12 B F24, C26 H37 N O2 P Ru'
_chemical_formula_sum            'C58 H49 B F24 N O2 P Ru'
_chemical_formula_weight         1390.83
_chemical_name_systematic
'{\k^2^ N,P-2-[(Diisopropylphosphanyl)-methyl]-quinoline}-(dioxygen)-(pentahapto-pentamethyl-cyclopentadienyl)-ruthenium (II) tetrakis{3,5-bis(trifluoromethyl)phenyl}borate'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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     vecmap
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.11(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.858(4)
_cell_length_b                   13.128(3)
_cell_length_c                   22.633(5)
_cell_measurement_reflns_used    9641
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.098
_cell_measurement_theta_min      2.325
_cell_volume                     5747(2)
_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 (Farrugia, 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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0272
_diffrn_reflns_av_sigmaI/netI    0.0252
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            38322
_diffrn_reflns_theta_full        25.12
_diffrn_reflns_theta_max         25.12
_diffrn_reflns_theta_min         1.05
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Bruker SMART APEX'
_diffrn_standards_decay_%        0.0061
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.423
_exptl_absorpt_correction_T_max  0.901
_exptl_absorpt_correction_T_min  0.756
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.607
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2800
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.27
_refine_diff_density_max         2.696
_refine_diff_density_min         -1.336
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     802
_refine_ls_number_reflns         10201
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0538
_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^)+(0.0531P)^2^+16.9260P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1235
_refine_ls_wR_factor_ref         0.1268
_reflns_number_gt                9461
_reflns_number_total             10201
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100710d_si_002_1.cif
_cod_data_source_block           pv0914
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4315949