Half-Sandwich Hydride Complexes of Ruthenium with Bidentate Phosphinoamine Ligands: Proton-Transfer Reactions to [(C5R5)RuH(L)] [R = H, Me; L = dippae, (R,R)-dippach]
Manuel Jiménez-Tenorio; M. Dolores Palacios Tejero; M.Carmen Puerta; Pedro Valerga; Inorganic Chemistry 46 (2007) 1001–1012; doi:10.1021/ic061745u

data_4307205
_publ_contact_author_address
;
Departamento de Ciencia de los Materiales e Ingenier\'ia Metal\'urgica y
Qu\'imica Inorg\'anica
Campus Universitario del R\'io San Pedro
Facultad de Ciencias
Apartado 40
Puerto Real 11510. 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
;
Half-Sandwich Hydride Complexes of Ruthenium with Bidentate Phosphinoamine
Ligands: Proton-Transfer Reactions to [(C5R5)RuH(L)] [R = H, Me; L =
dippae, (R,R)-dippach]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1001
_journal_page_last               1012
_journal_paper_doi               10.1021/ic061745u
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         'C24H51N2Ru 1+; C24H20B 1-'
_chemical_formula_sum            'C48 H71 B N2 P2 Ru'
_chemical_formula_weight         849.89
_chemical_name_common
'[Ru(Cp*)(H)~2~{\k^2^-P,P-(^i^Pr)~2~PNH(CH~2~)~2~NHP(^i^Pr)~2~}]BPh~4~'
_chemical_name_systematic
;
(Pentahapto-pentamethylcyclopentadienyl)-(dihydride)-
{bis(diisopropylphosphino-N,N')ethylenediamine-\k^2^-P,P'}-ruthenium
tetraphenylborate
;
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.6400(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.9028(6)
_cell_length_b                   20.1254(11)
_cell_length_c                   19.6180(11)
_cell_measurement_reflns_used    7557
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.591
_cell_measurement_theta_min      2.279
_cell_volume                     4657.7(4)
_computing_cell_refinement       'Bruker SAINT +'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT +, SADABS, XPREP'
_computing_molecular_graphics    'ORTEP-3 vers. 1.076 (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      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '1900 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  0.0401
_diffrn_reflns_av_sigmaI/netI    0.0368
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            34883
_diffrn_reflns_theta_full        25.07
_diffrn_reflns_theta_max         25.07
_diffrn_reflns_theta_min         1.46
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Bruker SMART APEX'
_diffrn_standards_decay_%        0.0016
_exptl_absorpt_coefficient_mu    0.438
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.876
_exptl_absorpt_correction_type   'semi-empirical from equiv.(prg.SADABS)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.212
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.868
_refine_diff_density_min         -0.407
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     508
_refine_ls_number_reflns         8191
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0667
_refine_ls_R_factor_gt           0.0537
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0536P)^2^+5.9715P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1176
_refine_ls_wR_factor_ref         0.1245
_reflns_number_gt                7145
_reflns_number_total             8191
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061745usi20060914_073736.cif
_cod_data_source_block           pv0408t
_cod_depositor_comments
;
 Replacing the "\K" substring with the "\k" substring in the
 values of the _chemical_name_common and _chemical_name_systematic
 data items.

 Antanas Vaitkus,
 2017-03-29
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4307205