Interconversion of η(3)-H2SiRR' σ-Complexes and 16-Electron Silylene Complexes via Reversible H-H or C-H Elimination.
Lipke, Mark C.; Neumeyer, Felix; Tilley, T. Don; Journal of the American Chemical Society 136 (2014) 6092–6102; doi:10.1021/ja501803w

data_4121672
_publ_section_title
;
 Interconversion of \h(3)-H2SiRR' \s-Complexes and 16-Electron Silylene
 Complexes via Reversible H-H or C-H Elimination.
;
_journal_issue                   16
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6092
_journal_page_last               6102
_journal_paper_doi               10.1021/ja501803w
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety         'C72 H73 B N P3 Ru Si'
_chemical_formula_sum            'C72 H73 B N P3 Ru Si'
_chemical_formula_weight         1185.20
_chemical_name_systematic
; 
 ? 
;
_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                87.716(2)
_cell_angle_beta                 89.078(2)
_cell_angle_gamma                61.844(2)
_cell_formula_units_Z            2
_cell_length_a                   14.8682(10)
_cell_length_b                   15.3817(9)
_cell_length_c                   16.0142(11)
_cell_measurement_reflns_used    6240
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.344
_cell_measurement_theta_min      2.538
_cell_volume                     3226.4(4)
_computing_cell_refinement       'Bruker APEX2 v. 2009.1'
_computing_data_collection       'Bruker APEX2 v. 2009.1'
_computing_data_reduction        'Bruker APEX2 v. 2009.1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX I'
_diffrn_measurement_method       'w/ and f/ scans'
_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  0.0557
_diffrn_reflns_av_sigmaI/netI    0.1209
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22066
_diffrn_reflns_theta_full        25.43
_diffrn_reflns_theta_max         25.43
_diffrn_reflns_theta_min         1.27
_exptl_absorpt_coefficient_mu    0.375
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.9815
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.220
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1106
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_platon_squeeze_details
;
;
_refine_diff_density_max         0.568
_refine_diff_density_min         -0.566
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.929
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     723
_refine_ls_number_reflns         11828
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.929
_refine_ls_R_factor_all          0.0973
_refine_ls_R_factor_gt           0.0545
_refine_ls_shift/su_max          0.070
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0524P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1093
_refine_ls_wR_factor_ref         0.1217
_reflns_number_gt                7623
_reflns_number_total             11828
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja501803w_si_003.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
;Adding full bibliography for 4121672--4121674.cif.

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        3226.5(4)
_cod_database_code               4121672