Trans Additions of Silanes to 1-Alkynes Catalyzed by Ruthenium Complexes: Role of in Situ Formed Polynuclear Aggregates
Martín, Marta; Sola, Eduardo; Lahoz, Fernando J.; Oro, Luis A.; Organometallics 21 (2002) 4027–; doi:10.1021/om0205243

data_4077063
_publ_section_title
;
 Trans Additions of Silanes to 1-Alkynes Catalyzed by Ruthenium
 Complexes:&#x00A0; Role of in Situ Formed Polynuclear Aggregates
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              4027
_journal_paper_doi               10.1021/om0205243
_journal_volume                  21
_journal_year                    2002
_chemical_formula_moiety         'C32 H73 Cl O2 P2 Ru2 Si2, 0.5(C6 H14)'
_chemical_formula_sum            'C35 H80 Cl O2 P2 Ru2 Si2'
_chemical_formula_weight         888.70
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                108.263(2)
_cell_angle_beta                 91.088(2)
_cell_angle_gamma                101.615(2)
_cell_formula_units_Z            2
_cell_length_a                   11.5346(11)
_cell_length_b                   11.7231(11)
_cell_length_c                   17.5248(17)
_cell_measurement_reflns_used    2997
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.54
_cell_measurement_theta_min      2.27
_cell_volume                     2195.7(4)
_computing_cell_refinement       'SAINT+ v. 6.01 (Bruker AXS, 2000)'
_computing_data_collection       'SMART v. 5.611 (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT+ v. 6.01 (Bruker AXS, 2000)'
_computing_molecular_graphics    'XP program, SHELXTL v6.10,Bruker2000'
_computing_publication_material  'XCIF program, SHELXTLv6.10,BrukerAXS'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       '\w rotations with narrow frames'
_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  0.0776
_diffrn_reflns_av_sigmaI/netI    0.1402
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22063
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.81
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    0.903
_exptl_absorpt_correction_T_max  0.9422
_exptl_absorpt_correction_T_min  0.7424
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; SADABS: Area-Detector Absorption Correction. (1996)  Bruker-AXS 
  within SAINT+ package, v. 6.01.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             938
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.685
_refine_diff_density_min         -1.104
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.908
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         7726
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.908
_refine_ls_R_factor_all          0.0926
_refine_ls_R_factor_gt           0.0537
_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^)+(0.0163P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0880
_refine_ls_wR_factor_ref         0.0970
_reflns_number_gt                5057
_reflns_number_total             7726
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0205243.cif
_cod_data_source_block           compound9
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4077063