Unexpected Disproportionation of Tetramethylethylenediamine-Supported Perchlorodisilane Cl3SiSiCl3
Jan Tillmann; Frank Meyer-Wegner; Andor Nadj; Johanna Becker-Baldus; Tanja Sinke; Michael Bolte; Max C. Holthausen; Matthias Wagner; Hans-Wolfram Lerner; Inorganic Chemistry 51 (2012) 8599–8606; doi:10.1021/ic301283m

data_4329964
_publ_section_title
;
 Unexpected Disproportionation of Tetramethylethylenediamine-Supported
 Perchlorodisilane Cl3SiSiCl3
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8599
_journal_page_last               8606
_journal_paper_doi               10.1021/ic301283m
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C6 H16 Cl4 N2 Si'
_chemical_formula_sum            'C6 H16 Cl4 N2 Si'
_chemical_formula_weight         286.10
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.825(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   23.2626(13)
_cell_length_b                   14.4338(7)
_cell_length_c                   14.3613(8)
_cell_measurement_reflns_used    17456
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.0
_cell_measurement_theta_min      3.4
_cell_volume                     4816.2(4)
_computing_cell_refinement       'X-Area (Stoe & Cie, 2001)'
_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_data_reduction        'X-Area (Stoe & Cie, 2001)'
_computing_molecular_graphics    'XP in SHELXTL-Plus (Sheldrick, 1991)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008) '
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008) '
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'STOE IPDS II two-circle-diffractometer'
_diffrn_measurement_method       \w
_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  0.0984
_diffrn_reflns_av_sigmaI/netI    0.0944
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            21131
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.85
_diffrn_reflns_theta_min         3.25
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.043
_exptl_absorpt_correction_T_max  0.8030
_exptl_absorpt_correction_T_min  0.7588
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'MULABS (Spek, 2003; Blessing, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.578
_exptl_crystal_description       block
_exptl_crystal_F_000             2368
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.881
_refine_diff_density_min         -0.783
_refine_diff_density_rms         0.170
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.12(15)
_refine_ls_extinction_coef       0.0045(6)
_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_ref   1.988
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     471
_refine_ls_number_reflns         8158
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.987
_refine_ls_R_factor_all          0.0964
_refine_ls_R_factor_gt           0.0918
_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^)+(0.0682P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2194
_refine_ls_wR_factor_ref         0.2210
_reflns_number_gt                7637
_reflns_number_total             8158
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic301283m_si_001_4.cif
_cod_data_source_block           wa888
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               4329964