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_4104497
_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         'C45 H86 N2 P2 Ru Si2'
_chemical_formula_sum            'C45 H86 N2 P2 Ru Si2'
_chemical_formula_weight         874.35
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      11
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 109.44(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.831(2)
_cell_length_b                   21.651(4)
_cell_length_c                   11.917(2)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      26.05
_cell_measurement_theta_min      1.65
_cell_measurement_wavelength     0.71073
_cell_volume                     2391.9(9)
_computing_cell_refinement       'Stoe IPDS software (Stoe, 1996)'
_computing_data_collection       'Stoe IPDS software (Stoe, 1996)'
_computing_data_reduction        'XRED (Stoe, 1.08, 1996)'
_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    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device       'Stoe IPDS'
_diffrn_measurement_method       \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  0.0464
_diffrn_reflns_av_unetI/netI     0.0266
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            34507
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.41
_diffrn_standards_decay_%        0.1
_diffrn_standards_interval_time  4
_diffrn_standards_number         200
_exptl_absorpt_coefficient_mu    0.476
_exptl_absorpt_correction_T_max  0.949
_exptl_absorpt_correction_T_min  0.912
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
        (See: Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.214
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.187
_refine_diff_density_min         -0.715
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         4805
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0466
_refine_ls_R_factor_gt           0.0403
_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^)+(0.0415P)^2^+2.7853P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0912
_refine_ls_wR_factor_ref         0.0953
_reflns_number_gt                4391
_reflns_number_total             4805
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja901140v_si_004.cif
_cod_data_source_block           mg1405
_cod_database_code               4104497