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_4104495
_publ_contact_author
;
Sylviane Sabo-Etienne and Mary Grellier
;
_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 and grellier@lcc-toulouse.fr'
_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_compound_source        'synthesis as described'
_chemical_formula_moiety         'C27 H52 N6 Ru1 Si6'
_chemical_formula_sum            'C27 H52 N6 Ru Si6'
_chemical_formula_weight         730.36
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      148
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   18.645(2)
_cell_length_b                   18.645(2)
_cell_length_c                   19.061(2)
_cell_measurement_reflns_used    2200
_cell_measurement_temperature    110
_cell_measurement_theta_max      32.1176
_cell_measurement_theta_min      2.7335
_cell_measurement_wavelength     0.71073
_cell_volume                     5738.5(11)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Oxford-Diffraction XCALIBUR'
_diffrn_measurement_method       \w-\f
_diffrn_orient_matrix_UB_11      -0.003136264
_diffrn_orient_matrix_UB_12      0.0330220518
_diffrn_orient_matrix_UB_13      0.0153731951
_diffrn_orient_matrix_UB_21      0.0439013728
_diffrn_orient_matrix_UB_22      0.0239705201
_diffrn_orient_matrix_UB_23      0.0021206477
_diffrn_orient_matrix_UB_31      0.0013290748
_diffrn_orient_matrix_UB_32      0.0163693335
_diffrn_orient_matrix_UB_33      -0.0338219039
_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  0.0506
_diffrn_reflns_av_unetI/netI     0.0923
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            7095
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         3.31
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.623
_exptl_absorpt_correction_T_max  0.9884
_exptl_absorpt_correction_T_min  0.9768
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.268
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             2304
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.0875
_exptl_crystal_size_min          0.025
_refine_diff_density_max         0.435
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.894
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     129
_refine_ls_number_reflns         2409
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.894
_refine_ls_R_factor_all          0.0731
_refine_ls_R_factor_gt           0.0361
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0220P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0566
_refine_ls_wR_factor_ref         0.0632
_reflns_number_gt                1598
_reflns_number_total             2409
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja901140v_si_001.cif
_cod_data_source_block           mgo300306
_cod_original_cell_volume        5738.5(12)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4104495