Structure and Reactivity of Bis(silyl) Dihydride Complexes (PMe3)3Ru(SiR3)2(H)2: Model Compounds and Real Intermediates in a Dehydrogenative C-Si Bond Forming Reaction
Vladimir K. Dioumaev; Bok R. Yoo; Leo J. Procopio; Patrick J. Carroll; Donald H. Berry; Journal of the American Chemical Society 125 (2003) 8936–8948; doi:10.1021/ja035916v

data_4113977
_publ_section_title
;
 Structure and Reactivity of Bis(silyl) Dihydride Complexes
 (PMe3)3Ru(SiR3)2(H)2: Model Compounds and Real Intermediates in a
 Dehydrogenative C-Si Bond Forming Reaction
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8936
_journal_page_last               8948
_journal_paper_doi               10.1021/ja035916v
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C15 H45 P3 Ru Si2'
_chemical_formula_weight         475.67
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_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
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 114.123(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   35.9187(5)
_cell_length_b                   9.3210(1)
_cell_length_c                   16.1099(1)
_cell_measurement_temperature    200(2)
_cell_volume                     4922.55(10)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SIR92 (Altomare, 1993)'
_diffrn_ambient_temperature      200(2)
_diffrn_measurement_device       'image plate area detector'
_diffrn_measurement_device_type  'Rigaku R-AXIS IIc'
_diffrn_measurement_method       'phi oscillations'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_av_sigmaI/netI    0.0236
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            23361
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.52
_exptl_absorpt_coefficient_mu    0.925
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.284
_exptl_crystal_F_000             2016
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.660
_refine_diff_density_min         -0.694
_refine_diff_density_rms         0.090
_refine_ls_extinction_coef       0.00146(11)
_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_all   1.103
_refine_ls_goodness_of_fit_obs   1.113
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         5604
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.103
_refine_ls_restrained_S_obs      1.113
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_obs          0.0445
_refine_ls_shift/esd_max         -0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0570P)^2^+11.1007P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1107
_refine_ls_wR_factor_obs         0.1065
_reflns_number_observed          5129
_reflns_number_total             5604
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja035916vsi20030501_113351.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0570P)^2^+11.1007P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0570P)^2^+11.1007P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        4922.55(9)
_cod_original_sg_symbol_H-M      'C 2/c '
_cod_database_code               4113977