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_7107948
_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_moiety         'C48 H100 Pb2 Si8 Te2'
_chemical_formula_sum            'C48 H100 Pb2 Si8 Te2'
_chemical_formula_weight         1571.58
_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                 103.36(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.762(6)
_cell_length_b                   19.778(7)
_cell_length_c                   25.104(13)
_cell_measurement_reflns_used    20820
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      26.62
_cell_measurement_theta_min      1.32
_cell_volume                     6648(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'STOE IPDS 2'
_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  0.0931
_diffrn_reflns_av_sigmaI/netI    0.1173
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            41516
_diffrn_reflns_theta_full        26.79
_diffrn_reflns_theta_max         26.79
_diffrn_reflns_theta_min         1.32
_exptl_absorpt_coefficient_mu    6.090
_exptl_absorpt_correction_T_max  0.8502
_exptl_absorpt_correction_T_min  0.4408
_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    1.570
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3072
_exptl_crystal_size_max          0.1430
_exptl_crystal_size_mid          0.1230
_exptl_crystal_size_min          0.0350
_platon_squeeze_details
;
;
_refine_diff_density_max         2.439
_refine_diff_density_min         -2.438
_refine_diff_density_rms         0.214
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.953
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     573
_refine_ls_number_reflns         14056
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.953
_refine_ls_R_factor_all          0.1312
_refine_ls_R_factor_gt           0.0689
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0814P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1458
_refine_ls_wR_factor_ref         0.1732
_reflns_number_gt                7953
_reflns_number_total             14056
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc32615a.txt
_cod_data_source_block           shelxl
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7107948