Ruthenium Agostic (Phosphinoaryl)borane Complexes: Multinuclear Solid-State and Solution NMR, X-ray, and DFT Studies
Yann Gloaguen; Gilles Alcaraz; Alban Petit; Eric Clot; Yannick Coppel; Laure Vendier; Sylviane Sabo-Etienne; Journal of the American Chemical Society 133 (2011) 17232–17238; doi:10.1021/ja203828r

data_4107023
_publ_contact_author
;
Sylviane Sabo-Etienne
;
_publ_contact_author_address
;
Laboratoire de Chimie de Coordination
205 Route de Narbonne
31077 Toulouse Cedex 04
;
_publ_contact_author_email       Sylviane.Sabo@lcc-toulouse.fr
_publ_section_title
;
 Ruthenium Agostic (Phosphinoaryl)borane Complexes: Multinuclear
 Solid-State and Solution NMR, X-ray, and DFT Studies
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17232
_journal_page_last               17238
_journal_paper_doi               10.1021/ja203828r
_journal_volume                  133
_journal_year                    2011
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C60 H97 B N P3 Ru, 0.5 (C4 H9)'
_chemical_formula_sum            'C62 H101.5 B N P3 Ru'
_chemical_formula_weight         1065.73
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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
_cell_angle_alpha                99.330(2)
_cell_angle_beta                 96.380(2)
_cell_angle_gamma                108.261(2)
_cell_formula_units_Z            2
_cell_length_a                   12.0884(6)
_cell_length_b                   12.5779(6)
_cell_length_c                   20.5574(9)
_cell_measurement_reflns_used    9843
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      32.1
_cell_measurement_theta_min      2.1
_cell_measurement_wavelength     0.71073
_cell_volume                     2884.9(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      110
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measurement_device_type  'Bruker Kappa APEX II'
_diffrn_measurement_method       \w-\f
_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  0.0383
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            56265
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.8
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.393
_exptl_absorpt_correction_T_max  0.971
_exptl_absorpt_correction_T_min  0.902
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1149
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.125
_exptl_crystal_size_min          0.075
_refine_diff_density_max         0.938
_refine_diff_density_min         -0.46
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     639
_refine_ls_number_reflns         11676
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0345
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0404P)^2^+2.5204P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0812
_refine_ls_wR_factor_ref         0.0889
_reflns_number_gt                9706
_reflns_number_total             11676
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja203828r_si_002.cif
_cod_data_source_block           gao110509
_cod_original_formula_sum        'C62 H101.50 B N P3 Ru'
_cod_database_code               4107023