Sn[Si(SiMe3)3]3- and Sn3[Si(SiMe3)3]4: first insight into the mechanism of the disproportionation of a tin monohalide gives access to the shortest double bond of tin.
Schrenk, Claudio; Schnepf, Andreas; Chemical communications (Cambridge, England) 46 (2010) 6756–6758; doi:10.1039/c0cc02367a

data_7112853
_publ_section_title
;
 Sn[Si(SiMe3)3]3- and Sn3[Si(SiMe3)3]4: first insight into the mechanism
 of the disproportionation of a tin monohalide gives access to the
 shortest double bond of tin.
;
_journal_issue                   36
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              6756
_journal_page_last               6758
_journal_paper_doi               10.1039/c0cc02367a
_journal_volume                  46
_journal_year                    2010
_chemical_formula_sum            'C95 H282 Si40 Sn13'
_chemical_formula_weight         4091.78
_chemical_name_systematic
;
?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 103.44(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.351(3)
_cell_length_b                   43.305(9)
_cell_length_c                   15.351(3)
_cell_measurement_reflns_used    30885
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.09
_cell_measurement_theta_min      1.37
_cell_volume                     9925(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.730
_diffrn_measured_fraction_theta_max 0.730
_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  0.0501
_diffrn_reflns_av_sigmaI/netI    0.0487
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            30711
_diffrn_reflns_theta_full        23.67
_diffrn_reflns_theta_max         23.67
_diffrn_reflns_theta_min         1.36
_exptl_absorpt_coefficient_mu    1.876
_exptl_absorpt_correction_T_max  0.8936
_exptl_absorpt_correction_T_min  0.5180
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       diamond
_exptl_crystal_F_000             4124
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.271
_refine_diff_density_min         -1.295
_refine_diff_density_rms         0.150
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.52(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     859
_refine_ls_number_reflns         19643
_refine_ls_number_restraints     523
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.0725
_refine_ls_R_factor_gt           0.0634
_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^)+(0.0901P)^2^+67.5278P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1737
_refine_ls_wR_factor_ref         0.1817
_reflns_number_gt                17032
_reflns_number_total             19643
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0cc02367a.txt
_cod_data_source_block           cl27p21
_cod_original_cell_volume        9925(3)
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               7112853