B‒C Bond Cleavage and Ru‒C Bond Formation from a Phosphinoborane: Synthesis of a Bis-σ Borane Aryl-Ruthenium Complex
Cassen, Audrey; Vendier, Laure; Daran, Jean-Claude; Poblador-Bahamonde, Amalia I.; Clot, Eric; Alcaraz, Gilles; Sabo-Etienne, Sylviane; Organometallics 33 (2014) 7157–; doi:10.1021/om500972f

data_4084966
_publ_section_title
;
 B--C Bond Cleavage and Ru--C Bond Formation from a Phosphinoborane:
 Synthesis of a Bis-\s Borane Aryl-Ruthenium Complex
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              7157
_journal_paper_doi               10.1021/om500972f
_journal_volume                  33
_journal_year                    2014
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         '2(C43 H66 B N P2 Ru), C5 H12'
_chemical_formula_sum            'C91 H144 B2 N2 P4 Ru2'
_chemical_formula_weight         1613.72
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 104.723(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.1598(2)
_cell_length_b                   11.3665(5)
_cell_length_c                   28.1508(3)
_cell_measurement_reflns_used    9813
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      34.18
_cell_measurement_theta_min      2.82
_cell_measurement_wavelength     0.71073
_cell_volume                     8714.6(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_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      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.029
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            43169
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.01
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.464
_exptl_absorpt_correction_T_max  0.944
_exptl_absorpt_correction_T_min  0.832
_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    1.23
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3448
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.646
_refine_diff_density_min         -0.997
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     473
_refine_ls_number_reflns         8890
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_gt           0.0331
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0327P)^2^+25.3209P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0782
_refine_ls_wR_factor_ref         0.0825
_reflns_number_gt                7727
_reflns_number_total             8890
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om500972f_si_001.cif
_cod_data_source_block           aco260312
_cod_depositor_comments
'Adding full bibliography for 4084966--4084967.cif.'
_cod_database_code               4084966