Tin-Chalcogen Double-Bond Compounds, Stannanethione and Stannaneselone: Synthesis, Structure, and Reactivities
Masaichi Saito; Norihiro Tokitoh; Renji Okazaki; Journal of the American Chemical Society 126 (2004) 15572–15582; doi:10.1021/ja048453h

data_4113227
_publ_section_title
;
 Tin-Chalcogen Double-Bond Compounds, Stannanethione and Stannaneselone:
 Synthesis, Structure, and Reactivities
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15572
_journal_page_last               15582
_journal_paper_doi               10.1021/ja048453h
_journal_volume                  126
_journal_year                    2004
_chemical_formula_moiety         'C51 H84 Se Si6 Sn'
_chemical_formula_sum            'C51 H84 Se Si6 Sn'
_chemical_formula_weight         1063.37
_chemical_name_common            stannaneselone
_chemical_name_systematic        ?
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_date             1998-08-03
_audit_creation_method           SHELXL-97
_cell_angle_alpha                91.86(2)
_cell_angle_beta                 112.61(3)
_cell_angle_gamma                97.45(4)
_cell_formula_units_Z            2
_cell_length_a                   11.939(8)
_cell_length_b                   23.478(5)
_cell_length_c                   11.471(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      29.47
_cell_measurement_theta_min      23.78
_cell_volume                     2931(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Rigaku AFC5R'
_diffrn_measurement_method       '\q \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.1169
_diffrn_reflns_av_sigmaI/netI    0.3880
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            10794
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.49
_diffrn_standards_decay_%        16.4
_diffrn_standards_interval_time  4189
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.209
_exptl_absorpt_correction_T_max  0.7940
_exptl_absorpt_correction_T_min  0.5071
_exptl_absorpt_correction_type
;
\y scans(North,Phillips & Mathews,1968)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.205
_exptl_crystal_description       block
_exptl_crystal_F_000             1116
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.291
_refine_diff_density_min         -0.737
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     606
_refine_ls_number_reflns         10257
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.3159
_refine_ls_R_factor_gt           0.1037
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1113P)^2^+11.4268P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2125
_refine_ls_wR_factor_ref         0.3177
_reflns_number_gt                3427
_reflns_number_total             10257
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja048453hsi20040414_015340.cif
_cod_data_source_block           Stannaneselone
_cod_database_code               4113227