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_4113862
_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            'C18 H54 P4 Ru Si2'
_chemical_formula_weight         551.74
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 97.801(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.3876(1)
_cell_length_b                   23.6973(3)
_cell_length_c                   10.2102(1)
_cell_measurement_temperature    200(2)
_cell_volume                     2969.49(5)
_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     0.71070
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_sigmaI/netI    0.0242
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            28749
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.58
_exptl_absorpt_coefficient_mu    0.827
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.521
_refine_diff_density_min         -0.613
_refine_diff_density_rms         0.070
_refine_ls_extinction_coef       0.0080(4)
_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   1.182
_refine_ls_goodness_of_fit_obs   1.194
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         6757
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.182
_refine_ls_restrained_S_obs      1.194
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_obs          0.0448
_refine_ls_shift/esd_max         0.007
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0422P)^2^+2.8281P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1035
_refine_ls_wR_factor_obs         0.1004
_reflns_number_observed          6242
_reflns_number_total             6757
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja035131psi20030313_065710.cif
_cod_data_source_block           1b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0422P)^2^+2.8281P] 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^)+(0.0422P)^2^+2.8281P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_database_code               4113862