Phosphine-Catalyzed Si−C Coupling of Bissilylmethanes: Preparation of Cyclic (Cl2SiCH2)2and Linear Cl2Si(CH2SiCl3)2via Silylene and Silene Intermediates
Hong, Soon Hyun; Hyun, Sang Il; Jung, Il Nam; Han, Won-Sik; Kim, Min-Hye; Yun, Hoseop; Nam, Suk-Woo; Kang, Sang Ook; Organometallics 29 (2010) 687–; doi:10.1021/om901071k

data_4067686
_publ_section_title
;
 Phosphine-Catalyzed Si&#x2212;C Coupling of Bissilylmethanes: Preparation
 of Cyclic (Cl2SiCH2)2and Linear Cl2Si(CH2SiCl3)2via Silylene and Silene
 Intermediates
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              687
_journal_paper_doi               10.1021/om901071k
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C3 H6 Cl6 Si3'
_chemical_formula_weight         339.05
_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                73.79
_cell_angle_beta                 81.34
_cell_angle_gamma                80.18
_cell_formula_units_Z            2
_cell_length_a                   6.269
_cell_length_b                   8.241
_cell_length_c                   12.869
_cell_measurement_temperature    293(2)
_cell_volume                     625.329
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0414
_diffrn_reflns_av_sigmaI/netI    0.0515
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6084
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         3.32
_exptl_absorpt_coefficient_mu    1.611
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.801
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             336
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.457
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     133
_refine_ls_number_reflns         2835
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0354
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0265P)^2^+0.7379P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0890
_refine_ls_wR_factor_ref         0.0929
_reflns_number_gt                2412
_reflns_number_total             2835
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om901071k_si_002.cif
_cod_data_source_block           l
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        625.3
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4067686