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_4107024
_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         'C24 H29 B1 N1 P1'
_chemical_formula_sum            'C24 H29 B N P'
_chemical_formula_weight         373.26
_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
_cell_angle_alpha                90
_cell_angle_beta                 92.541(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.3430(4)
_cell_length_b                   10.0641(7)
_cell_length_c                   14.1425(6)
_cell_measurement_reflns_used    9666
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      42.57
_cell_measurement_theta_min      2.48
_cell_measurement_wavelength     0.71073
_cell_volume                     2466.0(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, 2008)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      110
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0253
_diffrn_reflns_av_unetI/netI     0.0281
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            81157
_diffrn_reflns_theta_full        42.63
_diffrn_reflns_theta_max         42.63
_diffrn_reflns_theta_min         2.34
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.118
_exptl_absorpt_correction_T_max  0.991
_exptl_absorpt_correction_T_min  0.921
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.005
_exptl_crystal_description       block
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.605
_refine_diff_density_min         -0.214
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     252
_refine_ls_number_reflns         17698
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0609
_refine_ls_R_factor_gt           0.0435
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0764P)^2^+0.0769P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1262
_refine_ls_wR_factor_ref         0.135
_reflns_number_gt                13051
_reflns_number_total             17698
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja203828r_si_003.cif
_cod_data_source_block           yann151009
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4107024