Cyclic and polycyclic tellurium-tin and tellurium-lead compounds ‒ synthesis, structures and thermal decomposition
Stephan Traut; Carsten von Hanisch; Alexander Peter Hahnel; Sven Stahl; Chem.Commun. 48 (2012) 6984–; doi:10.1039/c2cc32615a

data_7107949
_publ_section_title
;
 Cyclic and polycyclic tellurium-tin and tellurium-lead compounds --
 synthesis, structures and thermal decomposition
;
_journal_name_full               Chem.Commun.
_journal_page_first              6984
_journal_paper_doi               10.1039/c2cc32615a
_journal_volume                  48
_journal_year                    2012
_chemical_formula_sum            'C36 H108 Si16 Sn4 Te6'
_chemical_formula_weight         2231.02
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 91.70(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.5474(19)
_cell_length_b                   26.049(5)
_cell_length_c                   17.285(4)
_cell_measurement_reflns_used    2068
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      26.11
_cell_measurement_theta_min      2.40
_cell_volume                     4296.9(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  'STOE IPDS2'
_diffrn_measurement_method       'rotation method'
_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  0.0696
_diffrn_reflns_av_sigmaI/netI    0.0519
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19869
_diffrn_reflns_theta_full        25.62
_diffrn_reflns_theta_max         25.62
_diffrn_reflns_theta_min         2.41
_exptl_absorpt_coefficient_mu    3.390
_exptl_absorpt_correction_T_max  0.9040
_exptl_absorpt_correction_T_min  0.6503
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
(a) W. R. Busing and H. A. Levy, Acta Crystallogr. 1957, 10, 180-182.
(b) P. Coppens, L. Leiserowitz and D. Rabinovich, Acta Crystallogr. 1965, 18, 1035-1038.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.724
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             2120
_exptl_crystal_size_max          0.281
_exptl_crystal_size_mid          0.092
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.780
_refine_diff_density_min         -1.328
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         7752
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0540
_refine_ls_R_factor_gt           0.0411
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0549P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0939
_refine_ls_wR_factor_ref         0.0988
_reflns_number_gt                6339
_reflns_number_total             7752
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc32615a.txt
_cod_data_source_block           e:\traut\crystal\ah9\ah9abs\p21n
_cod_original_cell_volume        4297.0(15)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7107949