Synthesis and Reactivity of Silyl Ruthenium Complexes: The Importance of Trans Effects in C-H Activation, Si-C Bond Formation, and Dehydrogenative Coupling of Silanes
Vladimir K. Dioumaev; Leo J. Procopio; Patrick J. Carroll; Donald H. Berry; Journal of the American Chemical Society 125 (2003) 8043–8058; doi:10.1021/ja035131p

data_4113865
_publ_section_title
;
 Synthesis and Reactivity of Silyl Ruthenium Complexes: The Importance of
 Trans Effects in C-H Activation, Si-C Bond Formation, and Dehydrogenative
 Coupling of Silanes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8043
_journal_page_last               8058
_journal_paper_doi               10.1021/ja035131p
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C16 H48 P4 Ru Si'
_chemical_formula_weight         493.58
_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                 103.982(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.2642(2)
_cell_length_b                   10.9388(1)
_cell_length_c                   31.0714(4)
_cell_measurement_reflns_used    18969
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      0.0
_cell_volume                     5034.34(11)
_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  0.0403
_diffrn_reflns_av_sigmaI/netI    0.0288
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            18969
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.51
_exptl_absorpt_coefficient_mu    0.922
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.302
_exptl_crystal_F_000             2096
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.504
_refine_diff_density_min         -0.583
_refine_diff_density_rms         0.084
_refine_ls_extinction_coef       0.00104(12)
_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   1.215
_refine_ls_goodness_of_fit_obs   1.238
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         4272
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.215
_refine_ls_restrained_S_obs      1.238
_refine_ls_R_factor_all          0.0653
_refine_ls_R_factor_obs          0.0554
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0520P)^2^+16.5345P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1295
_refine_ls_wR_factor_obs         0.1239
_reflns_number_observed          3787
_reflns_number_total             4272
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja035131psi20030313_065835.cif
_cod_data_source_block           7a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0520P)^2^+16.5345P] 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^)+(0.0520P)^2^+16.5345P] 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        5034.34(10)
_cod_original_sg_symbol_H-M      'C 2/c '
_cod_database_code               4113865