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_4077064
_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         'C48 H106 Cl2 O4 P4 Ru4 Si2, 0.5 C6 H14'
_chemical_formula_sum            'C51 H113 Cl2 O4 P4 Ru4 Si2'
_chemical_formula_weight         1445.65
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 111.602(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.5670(18)
_cell_length_b                   12.8393(10)
_cell_length_c                   26.880(2)
_cell_measurement_reflns_used    2646
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      17.818
_cell_measurement_theta_min      2.169
_cell_volume                     7241.3(10)
_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      173(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.1656
_diffrn_reflns_av_sigmaI/netI    0.1727
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            72137
_diffrn_reflns_theta_full        25.06
_diffrn_reflns_theta_max         25.06
_diffrn_reflns_theta_min         1.63
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    1.048
_exptl_absorpt_correction_T_max  0.7924
_exptl_absorpt_correction_T_min  0.6329
_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            red
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2996
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.848
_refine_diff_density_min         -0.844
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.867
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     657
_refine_ls_number_reflns         12809
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      0.868
_refine_ls_R_factor_all          0.1126
_refine_ls_R_factor_gt           0.0572
_refine_ls_shift/su_max          0.062
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0347P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1191
_refine_ls_wR_factor_ref         0.1325
_reflns_number_gt                6972
_reflns_number_total             12809
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0205243.cif
_cod_data_source_block           compound10
_cod_original_cell_volume        7241.2(10)
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4077064