Step-by-Step Introduction of Silazane Moieties at Ruthenium: Different Extents of Ru-H-Si Bond Activation
Katharine A. Smart; Mary Grellier; Laure Vendier; Sax A. Mason; Silvia C. Capelli; Alberto Albinati; Sylviane Sabo-Etienne; Inorganic Chemistry 52 (2013) 2654–2661; doi:10.1021/ic302682f

data_4334040
_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
;
 Step-by-Step Introduction of Silazane Moieties at Ruthenium: Different
 Extents of Ru-H-Si Bond Activation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2654
_journal_page_last               2661
_journal_paper_doi               10.1021/ic302682f
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C56 H53 B F24 N6 Ru Si3'
_chemical_formula_weight         1463.00
_chemical_name_common
;            
{RuH[(eta2-H-SiMe2)N(Me)kappa-N-(C5H4N)][kappa-Si,N-(SiMe2)N(Me)(C5H4N)]2}+
 {[3,5-(CF3)2C6H3]4B}-  
;
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.0112(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.9659(3)
_cell_length_b                   11.9966(4)
_cell_length_c                   18.2189(5)
_cell_measurement_reflns_used    4187
_cell_measurement_temperature    20(1)
_cell_measurement_theta_max      59.91
_cell_measurement_theta_min      3.35
_cell_volume                     3044.98(15)
_computing_cell_refinement       'ILL RAFD9'
_computing_data_collection       'ILL HKLGEN, MAD'
_computing_data_reduction        'ILL Retreat'
_computing_molecular_graphics
;     
 ORTEP for Windows v1.074 (L.J. Farrugia 1997)
 Mercury CSD 2.4.5 (Build RC3), CCDC, Cambridge (2011)
;
_computing_publication_material
'WinGX v1.64.05(L.J. Farrugia, J. Appl. Cryst.,1999,32, 837)'
_computing_structure_refinement  'SHELXL-97 (Acta Cryst.,2008,A64,112)'
_diffrn_ambient_temperature      20(1)
_diffrn_measured_fraction_theta_full 0.884
_diffrn_measured_fraction_theta_max 0.884
_diffrn_measurement_device_type
'D19 position-sensitive detector diffractometer'
_diffrn_measurement_method       'omega step-scans'
_diffrn_radiation_monochromator  'Cu (311)'
_diffrn_radiation_probe          neutron
_diffrn_radiation_source         'ILL High Flux Reactor'
_diffrn_radiation_type           neutron
_diffrn_radiation_wavelength     1.1708
_diffrn_reflns_av_R_equivalents  0.1253
_diffrn_reflns_av_sigmaI/netI    0.1198
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            27927
_diffrn_reflns_theta_full        61.29
_diffrn_reflns_theta_max         61.29
_diffrn_reflns_theta_min         4.82
_diffrn_standards_interval_time  420
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.183
_exptl_absorpt_correction_T_max  0.9129
_exptl_absorpt_correction_T_min  0.8042
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   'program D19abscan'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.596
_exptl_crystal_description       plate
_exptl_crystal_F_000             781
_exptl_crystal_size_max          1.24
_exptl_crystal_size_mid          1.24
_exptl_crystal_size_min          0.52
_refine_diff_density_max         1.298
_refine_diff_density_min         -1.301
_refine_diff_density_rms         0.270
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1297
_refine_ls_number_reflns         9494
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0882
_refine_ls_R_factor_gt           0.0617
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0460P)^2^+20.0133P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1197
_refine_ls_wR_factor_ref         0.1310
_reflns_number_gt                7647
_reflns_number_total             9494
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302682f_si_002_1.cif
_cod_data_source_block           ru8
_cod_database_code               4334040