Exchange Processes in Complexes with Two Ruthenium (η2-Silane) Linkages: Role of the Secondary Interactions between Silicon and Hydrogen Atoms
Atheaux, Isabelle; Delpech, Fabien; Donnadieu, Bruno; Sabo-Etienne, Sylviane; Chaudret, Bruno; Hussein, Khansaa; Barthelat, Jean-Claude; Braun, Thomas; Duckett, Simon B.; Perutz, Robin N.; Organometallics 21 (2002) 5347–; doi:10.1021/om0206148

data_4077122
_publ_contact_author             'Dr S. Sabo-Etienne'
_publ_section_title
;
 Exchange Processes in Complexes with Two Ruthenium (\h2-Silane)
 Linkages:&#x00A0; Role of the Secondary Interactions between Silicon and
 Hydrogen Atoms
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              5347
_journal_paper_doi               10.1021/om0206148
_journal_volume                  21
_journal_year                    2002
_chemical_formula_sum            'C79 H72.5 O2.38 P3 Ru Si2'
_chemical_formula_weight         1310.03
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_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                89.99(2)
_cell_angle_beta                 91.03(2)
_cell_angle_gamma                90.02(2)
_cell_formula_units_Z            8
_cell_length_a                   40.246(3)
_cell_length_b                   19.777(3)
_cell_length_c                   17.734(4)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      22.0
_cell_measurement_theta_min      2.10
_cell_volume                     14113(4)
_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    'ORTEP3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1992)'
_diffrn_ambient_temperature      140(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_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  0.0733
_diffrn_reflns_av_sigmaI/netI    0.0687
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            38400
_diffrn_reflns_theta_full        22.72
_diffrn_reflns_theta_max         22.72
_diffrn_reflns_theta_min         2.06
_diffrn_standards_decay_%        <0.1
_diffrn_standards_interval_time  'every frame'
_diffrn_standards_number         200
_exptl_absorpt_coefficient_mu    0.370
_exptl_absorpt_correction_T_max  0.86
_exptl_absorpt_correction_T_min  0.54
_exptl_absorpt_correction_type   semi-empirical
_exptl_crystal_colour            'pale orange '
_exptl_crystal_density_diffrn    1.233
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             5460
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.063
_refine_diff_density_min         -0.403
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     902
_refine_ls_number_reflns         9282
_refine_ls_number_restraints     196
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.0782
_refine_ls_R_factor_gt           0.0485
_refine_ls_shift/su_max          0.036
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0749P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1119
_refine_ls_wR_factor_ref         0.1244
_reflns_number_gt                6730
_reflns_number_total             9282
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0206148.cif
_cod_data_source_block           global
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C79 H72.50 O2.38 P3 Ru Si2'
_cod_database_code               4077122
_computing_corr_abs              DIFABS