Versatile Coordination of 2-Pyridinetetramethyldisilazane at Ruthenium: Ru(II) vs Ru(IV) As Evidenced by NMR, X-ray, Neutron, and DFT Studies
Mary Grellier; Tahra Ayed; Jean-Claude Barthelat; Alberto Albinati; Sax Mason; Laure Vendier; Yannick Coppel; Sylviane Sabo-Etienne; Journal of the American Chemical Society 131 (2009) 7633–7640; doi:10.1021/ja901140v

data_4104496
_publ_contact_author_address
;
 Laboratoire de Chimie de Coordination
 205 Route de Narbonne
 31077 Toulouse Cedex 04
;
_publ_contact_author_email       sabo@lcc-toulouse.fr
_publ_contact_author_name        'Sylviane Sabo-Etienne'
_publ_section_title
;
 Versatile Coordination of 2-Pyridinetetramethyldisilazane at Ruthenium:
 Ru(II) vs Ru(IV) As Evidenced by NMR, X-ray, Neutron, and DFT Studies
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7633
_journal_page_last               7640
_journal_paper_doi               10.1021/ja901140v
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C27 H52 N6 Ru Si6'
_chemical_formula_weight         730.33
_chemical_name_common            Ru(H)[(SiMe2)(N-[(C5H4N)(SiMe2H)]3(PCy3)2
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     'X-ray geometry'
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   18.5880(3)
_cell_length_b                   18.5880(3)
_cell_length_c                   18.8361(3)
_cell_measurement_reflns_used    2535
_cell_measurement_temperature    20(2)
_cell_measurement_theta_max      61.64
_cell_measurement_theta_min      2.74
_cell_volume                     5636.21(16)
_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)'
_computing_publication_material
'WinGX v1.64.05(L.J. Farrugia,J. Appl. Cryst.,1999,32, 837)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      20(2)
_diffrn_detector_area_resol_mean '1.5 mm vert. 2.5 mm hor.'
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type
'D19 position-sensitive detector diffractometer'
_diffrn_measurement_method       'omega step-scans'
_diffrn_radiation_monochromator  'Cu (331)'
_diffrn_radiation_probe          neutron
_diffrn_radiation_source         'ILL High Flux Reactor'
_diffrn_radiation_type           neutron
_diffrn_radiation_wavelength     1.16954(2)
_diffrn_reflns_av_R_equivalents  0.0971
_diffrn_reflns_av_sigmaI/netI    0.0854
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            13183
_diffrn_reflns_theta_full        61.71
_diffrn_reflns_theta_max         61.71
_diffrn_reflns_theta_min         2.74
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  '8 hours'
_diffrn_standards_number         10
_exptl_absorpt_coefficient_mu    0.201
_exptl_absorpt_correction_T_max  0.9675
_exptl_absorpt_correction_T_min  0.9066
_exptl_absorpt_correction_type   cylinder
_exptl_absorpt_process_details   'program D19abscan'
_exptl_crystal_colour            'dark yellow'
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             44
_exptl_crystal_size_max          2.1
_exptl_crystal_size_mid          2.0
_exptl_crystal_size_min          1.2
_refine_diff_density_max         1.362
_refine_diff_density_min         -1.217
_refine_diff_density_rms         0.291
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     278
_refine_ls_number_reflns         4285
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.1080
_refine_ls_R_factor_gt           0.0698
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+2.5085P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1306
_refine_ls_wR_factor_ref         0.1483
_reflns_number_gt                3216
_reflns_number_total             4285
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja901140v_si_003.cif
_cod_data_source_block           ruy21
_cod_original_cell_volume        5636.2(2)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4104496