η5-1,2,3-Trisilacyclopentadienyl - A Ligand for Transition Metal Complexes: Rhodium Half-Sandwich and Ruthenium Sandwich
Hiroyuki Yasuda; Vladimir Ya. Lee; Akira Sekiguchi; Journal of the American Chemical Society 131 (2009) 9902–9903; doi:10.1021/ja9038664

data_4104726
_publ_section_title
;
 \h5-1,2,3-Trisilacyclopentadienyl - A Ligand for Transition Metal
 Complexes: Rhodium Half-Sandwich and Ruthenium Sandwich
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9902
_journal_page_last               9903
_journal_paper_doi               10.1021/ja9038664
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C35 H73 O2 Rh Si6'
_chemical_formula_weight         797.38
_chemical_name_systematic
; 
 (CO)2Rh(Si3C2) 
;
_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                98.802(2)
_cell_angle_beta                 98.343(2)
_cell_angle_gamma                99.888(3)
_cell_formula_units_Z            2
_cell_length_a                   9.2650(2)
_cell_length_b                   13.3550(6)
_cell_length_c                   18.8320(8)
_cell_measurement_reflns_used    23438
_cell_measurement_temperature    150.0(1)
_cell_measurement_theta_max      28.02
_cell_measurement_theta_min      2.22
_cell_volume                     2233.09(15)
_computing_cell_refinement       'HKL scalepack'
_computing_data_collection       'MacScience Xpress'
_computing_data_reduction        Denzo
_computing_molecular_graphics    ORTEP
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      150.0(1)
_diffrn_measured_fraction_theta_full 0.919
_diffrn_measured_fraction_theta_max 0.919
_diffrn_measurement_device       'MacScience DIP2030 Image plate'
_diffrn_measurement_method       char
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.027
_diffrn_reflns_av_sigmaI/netI    0.0457
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            23438
_diffrn_reflns_theta_full        28.02
_diffrn_reflns_theta_max         28.02
_diffrn_reflns_theta_min         2.22
_exptl_absorpt_coefficient_mu    0.570
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.186
_exptl_crystal_description       needle
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.725
_refine_diff_density_min         -0.930
_refine_diff_density_rms         0.083
_refine_ls_extinction_coef       0.0229(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         9942
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0362
_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^)+(0.0619P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0945
_refine_ls_wR_factor_ref         0.0979
_reflns_number_gt                8446
_reflns_number_total             9942
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9038664_si_001.cif
_cod_data_source_block           shelxl
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4104726