# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2006 data_publication_text _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _ccdc_journal_manuscript_code B610833D _publ_contact_author_name 'Prof. Dr. S. Dehnen' _publ_contact_author_email dehnen@chemie.uni-marburg.de _publ_section_title ;Fine-Tuning of Optical Properties with Salts of Discrete or Polymeric, Heterobimetallic Telluride Anions [M4(\m4-Te)(SnTe4)4]10 (M = Mn, Zn, Cd, Hg) and {[Hg4(\m4-Te)(SnTe4)3]6} ; loop_ _publ_author_name 'Stefanie Dehnen' 'Andreas Fuchs' 'Eugen Ruzin' data_1 _database_code_depnum_ccdc_archive 'CCDC 616329' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H40 K10 Mn4 O20 Sn4 Te17' _chemical_formula_weight 3615.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.1399 0.1562 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.2704 0.4681 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -1.1587 0.9299 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Te Te -0.9710 1.0960 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M I-43m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' 'y, x, z' '-y, -x, z' 'y, -x, -z' '-y, x, -z' 'x, z, y' '-x, z, -y' '-x, -z, y' 'x, -z, -y' 'z, y, x' 'z, -y, -x' '-z, y, -x' '-z, -y, x' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'z+1/2, x+1/2, y+1/2' 'z+1/2, -x+1/2, -y+1/2' '-z+1/2, -x+1/2, y+1/2' '-z+1/2, x+1/2, -y+1/2' 'y+1/2, z+1/2, x+1/2' '-y+1/2, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x+1/2' '-y+1/2, -z+1/2, x+1/2' 'y+1/2, x+1/2, z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' 'x+1/2, z+1/2, y+1/2' '-x+1/2, z+1/2, -y+1/2' '-x+1/2, -z+1/2, y+1/2' 'x+1/2, -z+1/2, -y+1/2' 'z+1/2, y+1/2, x+1/2' 'z+1/2, -y+1/2, -x+1/2' '-z+1/2, y+1/2, -x+1/2' '-z+1/2, -y+1/2, x+1/2' _cell_length_a 16.0889(19) _cell_length_b 16.0889(19) _cell_length_c 16.0889(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4164.7(9) _cell_formula_units_Z 2 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'rhombic dodecahedron' _exptl_crystal_colour black _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.883 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3148 _exptl_absorpt_coefficient_mu 4.278 _exptl_absorpt_correction_type semi-empirical _exptl_absorpt_correction_T_min 0.23851 _exptl_absorpt_correction_T_max 0.28808 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.56087 _diffrn_radiation_type AgK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9978 _diffrn_reflns_av_R_equivalents 0.0759 _diffrn_reflns_av_sigmaI/netI 0.0242 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 20.98 _reflns_number_total 785 _reflns_number_gt 739 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0667P)^2^+50.9029P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_BASF 0.25(6) _refine_ls_number_reflns 785 _refine_ls_number_parameters 68 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0668 _refine_ls_R_factor_gt 0.0625 _refine_ls_wR_factor_ref 0.1638 _refine_ls_wR_factor_gt 0.1603 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Te1 Te 0.0000 0.0000 0.0000 0.0598(8) Uani 1 24 d S . . Te2 Te 0.19864(7) 0.19864(7) -0.00260(13) 0.1190(8) Uani 1 2 d S . . Te3 Te 0.25720(11) 0.25720(11) 0.25720(11) 0.180(2) Uani 1 6 d S . . Sn1 Sn 0.15940(8) 0.15940(8) 0.15940(8) 0.0942(9) Uani 1 6 d S . . Mn1 Mn 0.09776(17) 0.09776(17) -0.09776(17) 0.0717(12) Uani 1 6 d S . . K1A K 0.385(3) 0.318(3) 0.145(3) 0.085(11) Uiso 0.08 1 d P . . K1B K 0.334(4) 0.334(4) 0.104(7) 0.16(3) Uiso 0.11 2 d SP . . K1C K 0.317(5) 0.418(4) 0.074(5) 0.124(17) Uiso 0.09 1 d P . . K1D K 0.306(3) 0.489(2) 0.168(3) 0.090(10) Uiso 0.09 1 d P . . K2A K 0.0000 0.356(3) 0.0000 0.099(10) Uiso 0.20 4 d SP . . K2B K 0.005(5) 0.304(2) -0.005(5) 0.091(12) Uiso 0.13 2 d SP . . O1A O 0.267(2) 0.423(2) -0.062(2) 0.026(8) Uiso 0.11 1 d P . . O1B O 0.135(3) 0.392(3) -0.089(3) 0.045(9) Uiso 0.15 1 d P . . O1C O 0.038(5) 0.520(8) 0.038(5) 0.09(3) Uiso 0.12 2 d SP . . O2A O 0.174(2) 0.471(2) 0.029(2) 0.022(7) Uiso 0.11 1 d P . . O2B O 0.170(3) 0.384(4) 0.006(5) 0.049(12) Uiso 0.11 1 d P . . O2C O 0.4065(13) 0.4065(13) 0.070(2) 0.023(6) Uiso 0.19 2 d SP . . O3A O 0.197(3) 0.410(3) 0.117(4) 0.033(11) Uiso 0.09 1 d P . . O3B O 0.076(4) 0.374(3) 0.159(4) 0.038(11) Uiso 0.09 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Te1 0.0598(8) 0.0598(8) 0.0598(8) 0.000 0.000 0.000 Te2 0.1206(10) 0.1206(10) 0.1159(14) 0.0006(6) 0.0006(6) -0.0638(12) Te3 0.180(2) 0.180(2) 0.180(2) -0.0685(15) -0.0685(15) -0.0685(15) Sn1 0.0942(9) 0.0942(9) 0.0942(9) -0.0252(7) -0.0252(7) -0.0252(7) Mn1 0.0717(12) 0.0717(12) 0.0717(12) 0.0077(13) 0.0077(13) -0.0077(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Te1 Mn1 2.724(5) 2 ? Te1 Mn1 2.724(5) . ? Te1 Mn1 2.724(5) 4 ? Te1 Mn1 2.724(5) 3 ? Te2 K1D 2.16(4) 43_554 ? Te2 K1D 2.16(4) 31_554 ? Te2 Sn1 2.755(2) . ? Te2 Mn1 2.759(2) . ? Te2 K1A 3.11(5) 48_554 ? Te2 K1A 3.11(5) 36_554 ? Te2 K1B 3.53(11) . ? Te2 K2B 3.55(7) . ? Te2 K2B 3.55(7) 11 ? Te2 K2B 3.69(8) 9 ? Te2 K2B 3.69(8) 3 ? Te2 K1C 3.89(7) 31_554 ? Te3 Sn1 2.725(4) . ? Te3 K1A 2.91(5) 13 ? Te3 K1A 2.91(5) . ? Te3 K1A 2.91(5) 17 ? Te3 K1A 2.91(5) 5 ? Te3 K1A 2.91(5) 21 ? Te3 K1A 2.91(5) 9 ? Te3 K1B 3.02(10) 9 ? Te3 K1B 3.02(10) 5 ? Te3 K1B 3.02(10) . ? Te3 K1C 4.03(8) 13 ? Te3 K1C 4.03(8) . ? Sn1 Te2 2.755(2) 9 ? Sn1 Te2 2.755(2) 5 ? Mn1 Te2 2.759(2) 11 ? Mn1 Te2 2.759(2) 8 ? K1A O1B 1.04(6) 30 ? K1A K1B 1.08(8) . ? K1A K1C 1.26(9) 13 ? K1A K1A 1.51(10) 13 ? K1A O1B 1.64(6) 42 ? K1A K1D 1.73(6) 13 ? K1A O2C 1.89(6) . ? K1A O1A 1.95(6) 30 ? K1A O2B 2.02(9) 30 ? K1A O3A 2.05(7) 13 ? K1A K1C 2.25(9) . ? K1A O3B 2.80(8) 9 ? K1B K1A 1.08(8) 13 ? K1B O1B 1.33(10) 42 ? K1B O1B 1.33(10) 30 ? K1B K1C 1.45(9) . ? K1B K1C 1.45(9) 13 ? K1B O2C 1.73(10) . ? K1B O1A 2.37(4) 42 ? K1B O1A 2.37(4) 30 ? K1B O3A 2.53(6) 13 ? K1B O3A 2.53(6) . ? K1B K1D 2.73(8) . ? K1C O1B 0.95(7) 42 ? K1C K1A 1.26(9) 13 ? K1C O1A 1.39(9) 42 ? K1C O2C 1.45(8) . ? K1C O2B 1.59(9) 42 ? K1C O1B 1.82(9) 30 ? K1C O2A 1.87(8) 43_554 ? K1C K1D 1.90(8) . ? K1C O2A 1.94(8) 42 ? K1C O3A 2.06(9) . ? K1D O2B 0.96(6) 42 ? K1D O3B 1.65(7) 32 ? K1D K1A 1.73(6) 13 ? K1D O1B 1.84(6) 42 ? K1D O1A 2.04(6) 42 ? K1D Te2 2.16(4) 34 ? K1D O1A 2.29(6) 4_565 ? K1D O3A 2.32(7) . ? K1D O2A 2.35(6) 42 ? K1D O3A 2.40(7) 42 ? K1D O2C 2.61(4) . ? K2A K2B 0.83(5) 3 ? K2A K2B 0.83(5) . ? K2A O1C 2.18(14) 4_565 ? K2A O1C 2.18(14) 2_565 ? K2A O2C 2.44(4) 36_554 ? K2A O2C 2.44(4) 35_455 ? K2A O1B 2.67(5) 23 ? K2A O1B 2.67(5) 3 ? K2A O1B 2.67(5) . ? K2A O1B 2.67(5) 21 ? K2A O1C 2.78(13) . ? K2A O1C 2.78(13) 3 ? K2B K2B 0.2(2) 3 ? K2B O2C 2.85(9) 36_554 ? K2B O1B 2.87(11) 23 ? K2B O1B 2.87(11) . ? K2B O1C 2.93(14) 4_565 ? K2B O2B 2.96(10) . ? K2B O2B 2.96(10) 23 ? K2B O1C 2.99(13) 2_565 ? K2B O2C 3.01(10) 35_455 ? K2B O3B 3.02(7) 21 ? K2B O3B 3.02(7) 3 ? O1A O3A 0.98(7) 43_554 ? O1A O2A 1.33(5) 43_554 ? O1A K1C 1.39(9) 43_554 ? O1A O3B 1.57(7) 31_554 ? O1A O2B 1.75(8) 43_554 ? O1A K1A 1.95(6) 36_554 ? O1A K1D 2.04(6) 43_554 ? O1A K1D 2.29(6) 4_565 ? O1A K1B 2.37(4) 36_554 ? O1A K1C 2.69(8) 4_565 ? O1B O2C 0.91(5) 36_554 ? O1B K1C 0.95(7) 43_554 ? O1B K1A 1.04(6) 36_554 ? O1B O1B 1.06(8) 23 ? O1B K1B 1.33(10) 36_554 ? O1B K1A 1.64(6) 43_554 ? O1B O2B 1.64(8) . ? O1B K1C 1.82(9) 36_554 ? O1B K1D 1.84(6) 43_554 ? O1B K1D 2.79(5) 36_554 ? O1C O1C 1.38(17) 4_565 ? O1C O1C 1.38(17) 2_565 ? O1C O2C 1.50(11) 34 ? O1C O1C 1.7(2) 3 ? O1C K2A 2.18(14) 2_565 ? O1C K1C 2.59(12) 34 ? O1C K1C 2.59(12) 42 ? O1C K2B 2.93(14) 4_565 ? O1C K2B 2.99(13) 2_565 ? O1C K1B 3.21(15) 34 ? O1C K1A 3.31(12) 34 ? O2A O2A 1.32(8) 4_565 ? O2A O1A 1.33(5) 42 ? O2A O2B 1.45(7) . ? O2A O3B 1.76(6) 21 ? O2A O3A 1.76(6) . ? O2A K1C 1.87(8) 42 ? O2A K1C 1.94(8) 43_554 ? O2A K1D 2.35(6) 43_554 ? O2A K1A 2.98(6) 36_554 ? O2A K1B 3.07(9) 34 ? O2B K1D 0.96(6) 43_554 ? O2B O3B 1.15(10) 21 ? O2B K1C 1.59(9) 43_554 ? O2B O1A 1.75(8) 42 ? O2B K1A 2.02(9) 36_554 ? O2B K1B 2.78(10) 36_554 ? O2B K2B 3.09(9) 3 ? O2C O1B 0.91(5) 42 ? O2C O1B 0.91(5) 30 ? O2C K1C 1.45(8) 13 ? O2C O1C 1.50(11) 31_554 ? O2C K1A 1.89(6) 13 ? O2C K2A 2.44(4) 30 ? O2C K1D 2.61(4) 13 ? O2C K2B 2.85(9) 30 ? O3A O1A 0.98(7) 42 ? O3A O3B 1.07(8) 21 ? O3A K1A 2.05(7) 13 ? O3A K1D 2.40(7) 43_554 ? O3A K1C 2.71(9) 42 ? O3A K1C 3.22(9) 43_554 ? O3A K1B 3.27(11) 34 ? O3A K1D 3.33(7) 21 ? O3B O3A 1.07(9) 21 ? O3B O2B 1.15(10) 21 ? O3B O1A 1.57(7) 34 ? O3B K1D 1.65(7) 35_455 ? O3B O2A 1.76(6) 21 ? O3B K1C 2.64(10) 21 ? O3B K1C 2.71(9) 35_455 ? O3B K1A 2.80(8) 5 ? O3B K1B 2.92(8) 5 ? O3B K2B 3.02(7) 3 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Mn1 Te1 Mn1 109.5 2 . ? Mn1 Te1 Mn1 109.5 2 4 ? Mn1 Te1 Mn1 109.5 . 4 ? Mn1 Te1 Mn1 109.5 2 3 ? Mn1 Te1 Mn1 109.5 . 3 ? Mn1 Te1 Mn1 109.5 4 3 ? Sn1 Te2 Mn1 104.79(11) . . ? Te3 Sn1 Te2 106.35(6) . 9 ? Te3 Sn1 Te2 106.35(6) . 5 ? Te2 Sn1 Te2 112.40(5) 9 5 ? Te3 Sn1 Te2 106.35(6) . . ? Te2 Sn1 Te2 112.40(5) 9 . ? Te2 Sn1 Te2 112.40(5) 5 . ? Te1 Mn1 Te2 111.03(9) . . ? Te1 Mn1 Te2 111.03(9) . 11 ? Te2 Mn1 Te2 107.87(10) . 11 ? Te1 Mn1 Te2 111.03(9) . 8 ? Te2 Mn1 Te2 107.87(10) . 8 ? Te2 Mn1 Te2 107.87(10) 11 8 ? _diffrn_measured_fraction_theta_max 0.887 _diffrn_reflns_theta_full 20.98 _diffrn_measured_fraction_theta_full 0.887 _refine_diff_density_max 0.526 _refine_diff_density_min -0.653 _refine_diff_density_rms 0.119 # Attachment '2-rev2.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 616330' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H40 K10 O20 Sn4 Te17 Zn4' _chemical_formula_weight 3656.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.1399 0.1562 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.3242 0.9375 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -1.1587 0.9299 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Te Te -0.9710 1.0960 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M I-43m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' 'y, x, z' '-y, -x, z' 'y, -x, -z' '-y, x, -z' 'x, z, y' '-x, z, -y' '-x, -z, y' 'x, -z, -y' 'z, y, x' 'z, -y, -x' '-z, y, -x' '-z, -y, x' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'z+1/2, x+1/2, y+1/2' 'z+1/2, -x+1/2, -y+1/2' '-z+1/2, -x+1/2, y+1/2' '-z+1/2, x+1/2, -y+1/2' 'y+1/2, z+1/2, x+1/2' '-y+1/2, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x+1/2' '-y+1/2, -z+1/2, x+1/2' 'y+1/2, x+1/2, z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' 'x+1/2, z+1/2, y+1/2' '-x+1/2, z+1/2, -y+1/2' '-x+1/2, -z+1/2, y+1/2' 'x+1/2, -z+1/2, -y+1/2' 'z+1/2, y+1/2, x+1/2' 'z+1/2, -y+1/2, -x+1/2' '-z+1/2, y+1/2, -x+1/2' '-z+1/2, -y+1/2, x+1/2' _cell_length_a 15.9651(18) _cell_length_b 15.9651(18) _cell_length_c 15.9651(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4069.3(8) _cell_formula_units_Z 2 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'fragment of a rhombic dodecahedron' _exptl_crystal_colour black _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.984 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3188 _exptl_absorpt_coefficient_mu 4.677 _exptl_absorpt_correction_type semi-empirical _exptl_absorpt_correction_T_min 0.23851 _exptl_absorpt_correction_T_max 0.71571 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.56087 _diffrn_radiation_type AgK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6709 _diffrn_reflns_av_R_equivalents 0.1584 _diffrn_reflns_av_sigmaI/netI 0.0744 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.85 _diffrn_reflns_theta_max 19.97 _reflns_number_total 539 _reflns_number_gt 420 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_BASF 0.45(6) _refine_ls_number_reflns 539 _refine_ls_number_parameters 38 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1309 _refine_ls_R_factor_gt 0.0621 _refine_ls_wR_factor_ref 0.1977 _refine_ls_wR_factor_gt 0.1079 _refine_ls_goodness_of_fit_ref 0.880 _refine_ls_restrained_S_all 0.880 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Te1 Te 0.0000 0.0000 0.0000 0.052(3) Uani 1 24 d S . . Te2 Te 0.1953(2) 0.1953(2) -0.0067(5) 0.216(5) Uani 1 2 d S . . Te3 Te 0.2554(6) 0.2554(6) 0.2554(6) 0.366(14) Uani 1 6 d S . . Sn1 Sn 0.1574(3) 0.1574(3) 0.1574(3) 0.168(6) Uani 1 6 d S . . Zn1 Zn 0.0977(4) 0.0977(4) -0.0977(4) 0.129(5) Uani 1 6 d S . . K1 K 0.129(3) 0.409(5) 0.129(3) 0.13(2) Uiso 0.20 2 d SP . . K2A K 0.034(4) 0.343(8) 0.034(4) 0.17(3) Uiso 0.20 2 d SP . . K2B K 0.033(2) 0.297(3) 0.033(2) 0.112(11) Uiso 0.29 2 d SP . . K2C K 0.047(5) 0.341(9) -0.047(5) 0.15(3) Uiso 0.15 2 d SP . . O1A O 0.156(4) 0.565(5) 0.156(4) 0.09(2) Uiso 0.29 2 d SP . . O1B O 0.165(3) 0.580(3) 0.098(3) 0.070(11) Uiso 0.33 1 d P . . O2A O 0.140(4) 0.371(3) -0.084(4) 0.082(13) Uiso 0.33 1 d P . . O2B O 0.0000 0.5000 0.0000 0.16(8) Uiso 0.29 8 d SP . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Te1 0.052(3) 0.052(3) 0.052(3) 0.000 0.000 0.000 Te2 0.201(6) 0.201(6) 0.246(7) -0.004(3) -0.004(3) -0.091(4) Te3 0.366(14) 0.366(14) 0.366(14) -0.109(10) -0.109(10) -0.109(10) Sn1 0.168(6) 0.168(6) 0.168(6) -0.043(3) -0.043(3) -0.043(3) Zn1 0.129(5) 0.129(5) 0.129(5) 0.026(3) 0.026(3) -0.026(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Te1 Zn1 2.702(11) 2 ? Te1 Zn1 2.702(11) 4 ? Te1 Zn1 2.702(11) 3 ? Te1 Zn1 2.702(11) . ? Te2 Zn1 2.639(7) . ? Te2 Sn1 2.756(9) . ? Te2 K2B 3.13(3) 9 ? Te2 K2B 3.13(3) . ? Te2 K2C 3.38(11) . ? Te2 K2C 3.38(11) 11 ? Te2 K2A 3.55(9) 9 ? Te2 K2A 3.55(9) . ? Te2 K2B 4.01(4) 3 ? Te2 K2B 4.01(4) 11 ? Te3 Sn1 2.709(17) . ? Te3 K1 3.76(7) 9 ? Te3 K1 3.76(7) . ? Te3 K1 3.76(7) 5 ? Sn1 Te2 2.756(9) 9 ? Sn1 Te2 2.756(9) 5 ? Zn1 Te2 2.639(7) 11 ? Zn1 Te2 2.639(7) 8 ? K1 K2A 2.39(12) . ? K1 O1A 2.56(12) . ? K1 K2B 2.82(8) . ? K1 O1B 2.83(9) 21 ? K1 O1B 2.83(9) . ? K1 O2B 3.26(7) . ? K1 K2C 3.29(10) . ? K1 K2C 3.29(10) 3 ? K1 O1B 3.37(6) 43_554 ? K1 O1B 3.37(6) 35_455 ? K1 K2A 3.84(12) 3 ? K2A K2B 0.73(12) . ? K2A K2C 1.32(10) . ? K2A K2C 1.32(10) 3 ? K2A K2A 1.55(19) 3 ? K2A K2B 1.68(10) 3 ? K2A O2A 2.57(7) . ? K2A O2A 2.57(7) 21 ? K2A O2B 2.62(13) . ? K2A O2A 2.92(9) 23 ? K2A O2A 2.92(9) 3 ? K2A O1B 3.21(7) 24_565 ? K2B K2C 1.48(10) . ? K2B K2C 1.48(10) 3 ? K2B K2B 1.49(9) 3 ? K2B K2A 1.68(10) 3 ? K2B O2A 2.79(6) . ? K2B O2A 2.79(6) 21 ? K2B O2A 3.10(7) 23 ? K2B O2A 3.10(7) 3 ? K2B Te2 3.13(3) 5 ? K2C K2A 1.32(10) 3 ? K2C K2B 1.48(10) 3 ? K2C O2A 1.66(11) 23 ? K2C O2A 1.66(11) . ? K2C K2C 2.1(2) 3 ? K2C O1B 2.40(12) 22_565 ? K2C O1B 2.40(12) 4_565 ? K2C O2B 2.75(14) . ? K2C O1A 2.88(14) 4_565 ? O1A O1B 0.98(7) 21 ? O1A O1B 0.98(7) . ? O1A O2A 1.57(10) 24_565 ? O1A O2A 1.57(10) 4_565 ? O1A K2C 2.88(14) 4_565 ? O1B O2A 0.91(6) 4_565 ? O1B O1B 1.52(9) 21 ? O1B O2A 1.66(7) 24_565 ? O1B K2C 2.40(12) 4_565 ? O1B K2A 3.21(7) 4_565 ? O1B K1 3.37(6) 32 ? O2A O1B 0.91(6) 4_565 ? O2A O2A 1.26(10) 23 ? O2A O1A 1.57(10) 4_565 ? O2A O1B 1.66(7) 22_565 ? O2A K2A 2.92(9) 3 ? O2A K2B 3.10(7) 3 ? O2B K2A 2.62(13) 3 ? O2B K2A 2.62(13) 4_565 ? O2B K2A 2.62(13) 2_565 ? O2B K2C 2.75(14) 4_565 ? O2B K2C 2.75(14) 2_565 ? O2B K2C 2.75(14) 3 ? O2B K1 3.26(7) 3 ? O2B K1 3.26(7) 2_565 ? O2B K1 3.26(7) 4_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Zn1 Te1 Zn1 109.5 2 4 ? Zn1 Te1 Zn1 109.5 2 3 ? Zn1 Te1 Zn1 109.5 4 3 ? Zn1 Te1 Zn1 109.5 2 . ? Zn1 Te1 Zn1 109.5 4 . ? Zn1 Te1 Zn1 109.5 3 . ? Zn1 Te2 Sn1 105.3(3) . . ? Te3 Sn1 Te2 107.2(2) . 9 ? Te3 Sn1 Te2 107.2(2) . 5 ? Te2 Sn1 Te2 111.66(19) 9 5 ? Te3 Sn1 Te2 107.2(2) . . ? Te2 Sn1 Te2 111.66(19) 9 . ? Te2 Sn1 Te2 111.66(19) 5 . ? Te2 Zn1 Te2 107.6(3) . 11 ? Te2 Zn1 Te2 107.6(3) . 8 ? Te2 Zn1 Te2 107.6(3) 11 8 ? Te2 Zn1 Te1 111.3(3) . . ? Te2 Zn1 Te1 111.3(3) 11 . ? Te2 Zn1 Te1 111.3(3) 8 . ? _diffrn_measured_fraction_theta_max 0.806 _diffrn_reflns_theta_full 19.97 _diffrn_measured_fraction_theta_full 0.806 _refine_diff_density_max 0.032 _refine_diff_density_min -0.047 _refine_diff_density_rms 0.007 # Attachment '3a-rev2.cif' data_3a _database_code_depnum_ccdc_archive 'CCDC 616331' _ccdc_journal_manuscript_code B610833D _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H40 Cd4 K10 O20 Sn4 Te17' _chemical_formula_weight 3844.88 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.1399 0.1562 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -1.4396 0.7832 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -1.1587 0.9299 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Te Te -0.9710 1.0960 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M I-43m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' 'y, x, z' '-y, -x, z' 'y, -x, -z' '-y, x, -z' 'x, z, y' '-x, z, -y' '-x, -z, y' 'x, -z, -y' 'z, y, x' 'z, -y, -x' '-z, y, -x' '-z, -y, x' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'z+1/2, x+1/2, y+1/2' 'z+1/2, -x+1/2, -y+1/2' '-z+1/2, -x+1/2, y+1/2' '-z+1/2, x+1/2, -y+1/2' 'y+1/2, z+1/2, x+1/2' '-y+1/2, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x+1/2' '-y+1/2, -z+1/2, x+1/2' 'y+1/2, x+1/2, z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' 'x+1/2, z+1/2, y+1/2' '-x+1/2, z+1/2, -y+1/2' '-x+1/2, -z+1/2, y+1/2' 'x+1/2, -z+1/2, -y+1/2' 'z+1/2, y+1/2, x+1/2' 'z+1/2, -y+1/2, -x+1/2' '-z+1/2, y+1/2, -x+1/2' '-z+1/2, -y+1/2, x+1/2' _cell_length_a 16.1423(19) _cell_length_b 16.1423(19) _cell_length_c 16.1423(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4206.3(9) _cell_formula_units_Z 2 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'rhombic dodecahedron' _exptl_crystal_colour black _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.036 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3332 _exptl_absorpt_coefficient_mu 4.460 _exptl_absorpt_correction_type semi-empirical _exptl_absorpt_correction_T_min 0.23666 _exptl_absorpt_correction_T_max 0.32484 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.56087 _diffrn_radiation_type AgK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7857 _diffrn_reflns_av_R_equivalents 0.1450 _diffrn_reflns_av_sigmaI/netI 0.0648 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.44 _diffrn_reflns_theta_max 21.98 _reflns_number_total 940 _reflns_number_gt 727 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0557P)^2^+15.6472P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0046(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_BASF 0.07(4) _refine_ls_number_reflns 940 _refine_ls_number_parameters 52 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0707 _refine_ls_R_factor_gt 0.0530 _refine_ls_wR_factor_ref 0.1376 _refine_ls_wR_factor_gt 0.1275 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Te1 Te 0.0000 0.0000 0.0000 0.0560(7) Uani 1 24 d S . . Te2 Te 0.20081(5) 0.20081(5) 0.00022(9) 0.0935(5) Uani 1 2 d S . . Te3 Te 0.25813(7) 0.25813(7) 0.25813(7) 0.1080(10) Uani 1 6 d S . . Sn1 Sn 0.16047(7) 0.16047(7) 0.16047(7) 0.0744(6) Uani 1 6 d S . . Cd1 Cd 0.09970(7) 0.09970(7) -0.09970(7) 0.0666(5) Uani 1 6 d S . . K1A K 0.0000 0.3256(14) 0.0000 0.134(6) Uiso 0.50 4 d SP . . K1B K 0.086(4) 0.379(5) 0.086(4) 0.069(16) Uiso 0.05 2 d SP . . K2A K 0.091(4) 0.409(3) 0.292(4) 0.133(17) Uiso 0.09 1 d P . . K2B K 0.129(5) 0.375(3) 0.375(3) 0.137(19) Uiso 0.13 2 d SP . . K2C K 0.190(6) 0.353(4) 0.353(4) 0.13(2) Uiso 0.09 2 d SP . . K2D K 0.342(6) 0.369(5) 0.091(5) 0.13(2) Uiso 0.07 1 d P . . O1B O 0.187(3) 0.408(3) 0.093(3) 0.135(15) Uiso 0.34 1 d P . . O2A O 0.116(6) 0.398(7) 0.116(6) 0.20(4) Uiso 0.39 2 d SP . . O2B O 0.142(7) 0.416(10) 0.142(7) 0.23(6) Uiso 0.33 2 d SP . . O2C O 0.073(12) 0.487(11) 0.206(10) 0.19(6) Uiso 0.13 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Te1 0.0560(7) 0.0560(7) 0.0560(7) 0.000 0.000 0.000 Te2 0.1000(7) 0.1000(7) 0.0805(8) -0.0005(4) -0.0005(4) -0.0401(7) Te3 0.1080(10) 0.1080(10) 0.1080(10) -0.0306(7) -0.0306(7) -0.0306(7) Sn1 0.0744(6) 0.0744(6) 0.0744(6) -0.0118(5) -0.0118(5) -0.0118(5) Cd1 0.0666(5) 0.0666(5) 0.0666(5) 0.0040(5) 0.0040(5) -0.0040(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Te1 Cd1 2.7876(19) 2 ? Te1 Cd1 2.7876(19) 4 ? Te1 Cd1 2.7876(19) 3 ? Te1 Cd1 2.7876(19) . ? Te2 Sn1 2.7459(15) . ? Te2 Cd1 2.8159(14) . ? Te2 K2C 3.08(5) 31_554 ? Te2 K2C 3.08(5) 26_554 ? Te2 K1B 3.70(6) 9 ? Te2 K1B 3.70(6) . ? Te2 K2A 3.66(6) 43_554 ? Te2 K2A 3.66(6) 31_554 ? Te2 K2B 3.63(6) 31_554 ? Te2 K2B 3.63(6) 26_554 ? Te2 K2D 3.84(8) . ? Te2 K2D 3.84(8) 13 ? Te3 K2C 2.43(9) 5 ? Te3 K2C 2.43(9) . ? Te3 K2C 2.43(9) 9 ? Te3 Sn1 2.731(3) . ? Te3 K2B 3.39(7) . ? Te3 K2B 3.39(7) 9 ? Te3 K2B 3.39(7) 5 ? Te3 K2D 3.51(7) . ? Te3 K2D 3.51(7) 17 ? Te3 K2D 3.51(7) 5 ? Te3 K2D 3.51(7) 21 ? Te3 K2D 3.51(7) 9 ? Sn1 Te2 2.7459(15) 9 ? Sn1 Te2 2.7459(15) 5 ? Cd1 Te2 2.8159(14) 11 ? Cd1 Te2 2.8159(14) 8 ? K1A K1B 2.14(8) . ? K1A K1B 2.14(8) 3 ? K1A O2A 2.90(13) . ? K1A O2A 2.90(13) 3 ? K1A K2B 2.95(7) 30_455 ? K1A K2B 2.95(7) 31_554 ? K1A K2C 3.36(9) 30_455 ? K1A K2C 3.36(9) 31_554 ? K1A K2D 3.57(8) 35_455 ? K1A K2D 3.57(8) 44_455 ? K1A K2D 3.57(8) 36_554 ? K1A K2D 3.57(8) 43_554 ? K1B O2B 1.41(19) . ? K1B O1B 1.71(8) 21 ? K1B O1B 1.71(8) . ? K1B K1B 3.91(17) 3 ? K1B O2C 2.61(18) . ? K1B O2C 2.61(18) 21 ? K1B K2B 3.46(8) 30_455 ? K1B K2B 3.46(8) 31_554 ? K1B Te2 3.70(6) 5 ? K2A K2D 1.04(9) 21 ? K2A K2B 1.57(8) . ? K2A O1B 1.68(8) 21 ? K2A O2C 1.89(18) . ? K2A K2D 1.66(13) 5 ? K2A O2C 1.71(19) 39_455 ? K2A K2C 2.09(10) . ? K2A O2B 2.55(11) . ? K2A O2C 2.9(2) 40 ? K2A K2A 2.69(13) 17 ? K2A O2A 2.86(9) . ? K2A O1B 2.99(7) 34 ? K2B K2D 0.81(8) 5 ? K2B K2D 0.81(8) 21 ? K2B K2C 1.11(10) . ? K2B K2A 1.57(8) 17 ? K2B O2C 2.8(2) 39_455 ? K2B O2C 2.8(2) 35_455 ? K2B K1A 2.95(7) 34 ? K2B O1B 3.13(7) 5 ? K2B O1B 3.13(7) 21 ? K2B O2C 3.39(16) 17 ? K2B O2C 3.39(16) . ? K2C K2D 1.63(11) 5 ? K2C K2D 1.63(11) 21 ? K2C K2A 2.09(10) 17 ? K2C Te2 3.08(5) 34 ? K2C Te2 3.08(5) 26 ? K2C O1B 3.23(7) 5 ? K2C O1B 3.23(7) 21 ? K2C K1A 3.36(9) 34 ? K2D K2D 0.63(19) 13 ? K2D K2B 0.81(8) 9 ? K2D K2A 1.04(9) 21 ? K2D K2C 1.63(11) 9 ? K2D K2A 1.66(14) 9 ? K2D O2C 2.1(2) 31_554 ? K2D O1B 2.57(10) . ? K2D O2C 2.91(19) 21 ? K2D O2C 2.5(2) 43_554 ? K2D O2B 2.85(19) 31_554 ? K2D O1B 3.05(10) 43_554 ? K2D O1B 3.13(11) 13 ? O1B O2B 1.08(5) . ? O1B O2A 1.21(7) . ? O1B O2C 1.34(16) 21 ? O1B K2A 1.68(8) 21 ? O1B K2D 3.05(10) 42 ? O1B K2A 2.99(7) 31_554 ? O1B K2A 2.97(8) 32 ? O1B K2B 3.13(7) 9 ? O1B K2D 3.13(11) 13 ? O1B K2C 3.23(7) 9 ? O2A O2B 0.6(2) . ? O2A O1B 1.21(7) 21 ? O2A K2A 2.86(9) 21 ? O2A K2D 3.19(13) 34 ? O2A K2D 3.19(13) 42 ? O2B O1B 1.08(5) 21 ? O2B K2A 2.55(11) 21 ? O2B K2D 2.85(19) 42 ? O2B K2D 2.85(19) 34 ? O2B K2A 3.14(16) 40 ? O2B K2A 3.14(16) 32 ? O2B K2D 3.42(13) 21 ? O2C O1B 1.34(16) 21 ? O2C O2C 2.2(3) 39_455 ? O2C O2C 2.2(3) 40 ? O2C K2A 1.71(19) 40 ? O2C K2D 2.1(2) 34 ? O2C K2A 2.9(2) 39_455 ? O2C K2D 2.91(19) 21 ? O2C K2D 2.5(2) 42 ? O2C K2B 2.8(2) 32 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cd1 Te1 Cd1 109.5 2 4 ? Cd1 Te1 Cd1 109.5 2 3 ? Cd1 Te1 Cd1 109.5 4 3 ? Cd1 Te1 Cd1 109.5 2 . ? Cd1 Te1 Cd1 109.5 4 . ? Cd1 Te1 Cd1 109.5 3 . ? Sn1 Te2 Cd1 105.35(6) . . ? Te3 Sn1 Te2 105.67(4) . 9 ? Te3 Sn1 Te2 105.67(4) . 5 ? Te2 Sn1 Te2 112.99(4) 9 5 ? Te3 Sn1 Te2 105.67(4) . . ? Te2 Sn1 Te2 112.99(4) 9 . ? Te2 Sn1 Te2 112.99(4) 5 . ? Te1 Cd1 Te2 109.79(4) . . ? Te1 Cd1 Te2 109.79(4) . 11 ? Te2 Cd1 Te2 109.15(4) . 11 ? Te1 Cd1 Te2 109.79(4) . 8 ? Te2 Cd1 Te2 109.15(4) . 8 ? Te2 Cd1 Te2 109.15(4) 11 8 ? _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 21.98 _diffrn_measured_fraction_theta_full 0.952 _refine_diff_density_max 1.544 _refine_diff_density_min -0.828 _refine_diff_density_rms 0.149 # Attachment '3b-rev2.cif' data_3b _database_code_depnum_ccdc_archive 'CCDC 616332' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H40 Cd4 O20 Rb10 Sn4 Te17' _chemical_formula_weight 4308.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rb Rb -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M I-43m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' 'y, x, z' '-y, -x, z' 'y, -x, -z' '-y, x, -z' 'x, z, y' '-x, z, -y' '-x, -z, y' 'x, -z, -y' 'z, y, x' 'z, -y, -x' '-z, y, -x' '-z, -y, x' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'z+1/2, x+1/2, y+1/2' 'z+1/2, -x+1/2, -y+1/2' '-z+1/2, -x+1/2, y+1/2' '-z+1/2, x+1/2, -y+1/2' 'y+1/2, z+1/2, x+1/2' '-y+1/2, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x+1/2' '-y+1/2, -z+1/2, x+1/2' 'y+1/2, x+1/2, z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' 'x+1/2, z+1/2, y+1/2' '-x+1/2, z+1/2, -y+1/2' '-x+1/2, -z+1/2, y+1/2' 'x+1/2, -z+1/2, -y+1/2' 'z+1/2, y+1/2, x+1/2' 'z+1/2, -y+1/2, -x+1/2' '-z+1/2, y+1/2, -x+1/2' '-z+1/2, -y+1/2, x+1/2' _cell_length_a 16.1002(19) _cell_length_b 16.1002(19) _cell_length_c 16.1002(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4173.4(9) _cell_formula_units_Z 2 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'rhombic dodecahedron' _exptl_crystal_colour black _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.429 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3692 _exptl_absorpt_coefficient_mu 13.828 _exptl_absorpt_correction_type semi-empirical _exptl_absorpt_correction_T_min 0.44051 _exptl_absorpt_correction_T_max 0.54977 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17132 _diffrn_reflns_av_R_equivalents 0.1062 _diffrn_reflns_av_sigmaI/netI 0.0239 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 4.39 _diffrn_reflns_theta_max 24.98 _reflns_number_total 576 _reflns_number_gt 542 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0247P)^2^+30.8917P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00009(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_BASF 0.17(6) _refine_ls_number_reflns 576 _refine_ls_number_parameters 51 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0356 _refine_ls_R_factor_gt 0.0319 _refine_ls_wR_factor_ref 0.0652 _refine_ls_wR_factor_gt 0.0642 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.086 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Te1 Te 0.0000 0.0000 0.0000 0.0235(5) Uani 1 24 d S . . Te2 Te 0.20148(4) 0.20148(4) 0.00043(8) 0.0593(3) Uani 1 2 d S . . Te3 Te 0.25886(6) 0.25886(6) 0.25886(6) 0.1000(10) Uani 1 6 d S . . Sn1 Sn 0.16121(6) 0.16121(6) 0.16121(6) 0.0466(4) Uani 1 6 d S . . Cd1 Cd 0.10005(5) 0.10005(5) -0.10005(5) 0.0379(4) Uani 1 6 d S . . Rb1A Rb 0.0000 0.3250(4) 0.0000 0.1020(18) Uiso 0.71 4 d SP . . Rb1B Rb 0.0011(15) 0.329(2) 0.0443(19) 0.144(11) Uiso 0.09 1 d P . . Rb2A Rb 0.392(4) 0.293(4) 0.075(3) 0.173(17) Uiso 0.07 1 d P . . Rb2B Rb 0.413(2) 0.173(2) 0.092(2) 0.111(10) Uiso 0.05 1 d P . . Rb2C Rb 0.368(2) 0.368(2) 0.113(3) 0.107(12) Uiso 0.07 2 d SP . . O1A O 0.4289(12) 0.2623(12) -0.0673(13) 0.045(5) Uiso 0.40 1 d P . . O1B O 0.407(4) 0.252(4) -0.097(4) 0.051(13) Uiso 0.13 1 d P . . O2 O 0.016(2) 0.459(2) 0.178(2) 0.073(10) Uiso 0.23 1 d P . . O3 O 0.103(6) 0.465(8) 0.103(6) 0.10(4) Uiso 0.13 2 d SP . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Te1 0.0235(5) 0.0235(5) 0.0235(5) 0.000 0.000 0.000 Te2 0.0580(5) 0.0580(5) 0.0619(7) 0.0013(3) 0.0013(3) -0.0348(5) Te3 0.1000(10) 0.1000(10) 0.1000(10) -0.0440(7) -0.0440(7) -0.0440(7) Sn1 0.0466(4) 0.0466(4) 0.0466(4) -0.0141(4) -0.0141(4) -0.0141(4) Cd1 0.0379(4) 0.0379(4) 0.0379(4) 0.0051(4) 0.0051(4) -0.0051(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Te1 Cd1 2.7900(15) 2 ? Te1 Cd1 2.7900(15) . ? Te1 Cd1 2.7900(15) 4 ? Te1 Cd1 2.7900(15) 3 ? Te2 Sn1 2.7463(12) . ? Te2 Cd1 2.8197(12) . ? Te2 Rb1B 3.26(3) 21 ? Te2 Rb1B 3.26(3) 9 ? Te2 Rb2A 3.61(5) 13 ? Te2 Rb2A 3.61(5) . ? Te2 Rb2B 3.74(4) 13 ? Te2 Rb2B 3.74(4) . ? Te2 Rb1A 3.805(4) 9 ? Te2 Rb1A 3.805(4) . ? Te2 Rb2C 3.84(4) 36_554 ? Te2 Rb2C 3.84(4) 31_554 ? Te3 Sn1 2.723(2) . ? Te3 Rb2C 3.42(5) 9 ? Te3 Rb2C 3.42(5) 5 ? Te3 Rb2C 3.42(5) . ? Te3 Rb2A 3.69(6) . ? Te3 Rb2A 3.69(6) 5 ? Te3 Rb2A 3.69(6) 17 ? Te3 Rb2A 3.69(6) 9 ? Te3 Rb2A 3.69(6) 13 ? Te3 Rb2A 3.69(6) 21 ? Te3 Rb2B 3.91(4) 21 ? Te3 Rb2B 3.91(4) 9 ? Sn1 Te2 2.7463(12) 9 ? Sn1 Te2 2.7463(12) 5 ? Cd1 Te2 2.8197(12) 11 ? Cd1 Te2 2.8197(12) 8 ? Rb1A Rb1B 0.72(3) . ? Rb1A Rb1B 0.72(3) 21 ? Rb1A Rb1B 0.72(3) 23 ? Rb1A Rb1B 0.72(3) 3 ? Rb1A Rb2C 3.18(5) 36_554 ? Rb1A Rb2C 3.18(5) 35_455 ? Rb1A O3 3.25(14) . ? Rb1A O3 3.25(14) 3 ? Rb1A Rb2B 3.46(4) 13 ? Rb1A Rb2B 3.46(4) 5 ? Rb1A Rb2B 3.46(4) 16 ? Rb1A Rb2B 3.46(4) 8 ? Rb1B Rb1B 0.98(6) 21 ? Rb1B Rb1B 1.03(5) 23 ? Rb1B Rb1B 1.43(6) 3 ? Rb1B Rb2C 2.74(6) 35_455 ? Rb1B Rb2B 2.88(5) 5 ? Rb1B O3 2.89(14) . ? Rb1B O2 3.02(5) . ? Rb1B Rb2B 3.18(5) 13 ? Rb1B Te2 3.26(3) 5 ? Rb1B Rb2A 3.51(6) 44_455 ? Rb1B O2 3.57(5) 21 ? Rb2A O1B 0.81(8) 46 ? Rb2A O1A 1.11(6) 46 ? Rb2A Rb2C 1.40(6) . ? Rb2A Rb2B 1.98(7) . ? Rb2A O2 2.14(6) 44 ? Rb2A Rb2A 2.24(11) 13 ? Rb2A O2 2.35(7) 9 ? Rb2A O2 2.43(8) 43_554 ? Rb2A O1A 2.42(6) . ? Rb2A O3 2.44(14) 31_554 ? Rb2A Rb2B 2.68(7) 48_554 ? Rb2A O1B 2.86(8) . ? Rb2B O1A 1.14(4) 46 ? Rb2B O1B 1.21(7) 46 ? Rb2B O3 1.42(11) 9 ? Rb2B O2 1.43(5) 9 ? Rb2B Rb2B 1.84(8) 17 ? Rb2B Rb2A 2.68(7) 46 ? Rb2B O2 2.70(6) 10_655 ? Rb2B O1B 2.82(8) 30 ? Rb2B Rb1B 2.88(5) 9 ? Rb2B O1A 2.88(5) 30 ? Rb2B O1A 2.95(5) 3_655 ? Rb2C Rb2A 1.40(6) 13 ? Rb2C O1B 2.03(7) 46 ? Rb2C O1B 2.03(7) 34 ? Rb2C O1A 2.43(3) 46 ? Rb2C O1A 2.43(3) 34 ? Rb2C O3 2.47(15) 31_554 ? Rb2C Rb1B 2.74(6) 44 ? Rb2C Rb1B 2.74(6) 32 ? Rb2C O2 2.76(5) 44 ? Rb2C O2 2.76(5) 32 ? Rb2C O2 3.18(5) 43_554 ? O1A O1B 0.62(6) . ? O1A Rb2A 1.11(6) 48_554 ? O1A Rb2B 1.14(4) 48_554 ? O1A O2 1.37(4) 43_554 ? O1A Rb2C 2.43(3) 31_554 ? O1A Rb2B 2.88(5) 36_554 ? O1A Rb2A 2.93(6) 3_655 ? O1A Rb2B 2.95(5) 3_655 ? O1A Rb2A 3.35(6) 31_554 ? O1B Rb2A 0.81(8) 48_554 ? O1B Rb2B 1.21(7) 48_554 ? O1B Rb2C 2.03(7) 31_554 ? O1B Rb2B 2.82(8) 36_554 ? O1B Rb2A 2.93(10) 31_554 ? O1B Rb2B 3.17(8) 3_655 ? O1B Rb2A 3.33(9) 3_655 ? O2 O1A 1.37(4) 42 ? O2 O2 1.41(8) 2_565 ? O2 Rb2B 1.43(5) 5 ? O2 Rb2A 2.14(6) 44_455 ? O2 Rb2A 2.35(7) 5 ? O2 Rb2A 2.43(8) 42 ? O2 Rb2B 2.70(6) 7_565 ? O2 Rb2C 2.76(5) 35_455 ? O2 Rb2B 2.97(6) 13 ? O2 Rb2B 3.03(6) 44_455 ? O2 Rb2C 3.18(5) 34 ? O3 Rb2B 1.42(11) 13 ? O3 Rb2B 1.42(11) 5 ? O3 Rb2A 2.44(14) 42 ? O3 Rb2A 2.44(14) 34 ? O3 Rb2C 2.47(15) 34 ? O3 Rb1B 2.89(14) 21 ? O3 Rb2A 3.31(10) 5 ? O3 Rb2A 3.31(10) 13 ? O3 Rb1B 3.63(14) 23 ? O3 Rb1B 3.63(14) 3 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cd1 Te1 Cd1 109.5 2 . ? Cd1 Te1 Cd1 109.5 2 4 ? Cd1 Te1 Cd1 109.5 . 4 ? Cd1 Te1 Cd1 109.5 2 3 ? Cd1 Te1 Cd1 109.5 . 3 ? Cd1 Te1 Cd1 109.5 4 3 ? Sn1 Te2 Cd1 105.51(5) . . ? Te3 Sn1 Te2 105.76(3) . 9 ? Te3 Sn1 Te2 105.76(3) . 5 ? Te2 Sn1 Te2 112.91(3) 9 5 ? Te3 Sn1 Te2 105.76(3) . . ? Te2 Sn1 Te2 112.91(3) 9 . ? Te2 Sn1 Te2 112.91(3) 5 . ? Te1 Cd1 Te2 109.73(3) . . ? Te1 Cd1 Te2 109.73(3) . 11 ? Te2 Cd1 Te2 109.21(3) . 11 ? Te1 Cd1 Te2 109.73(3) . 8 ? Te2 Cd1 Te2 109.21(3) . 8 ? Te2 Cd1 Te2 109.21(3) 11 8 ? _diffrn_measured_fraction_theta_max 0.824 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.824 _refine_diff_density_max 0.473 _refine_diff_density_min -0.552 _refine_diff_density_rms 0.098 # Attachment '4-rev2.cif' data_4 _database_code_depnum_ccdc_archive 'CCDC 616333' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H40 Hg4 K10 O20 Sn4 Te17' _chemical_formula_weight 4197.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M I-43m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' 'y, x, z' '-y, -x, z' 'y, -x, -z' '-y, x, -z' 'x, z, y' '-x, z, -y' '-x, -z, y' 'x, -z, -y' 'z, y, x' 'z, -y, -x' '-z, y, -x' '-z, -y, x' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'z+1/2, x+1/2, y+1/2' 'z+1/2, -x+1/2, -y+1/2' '-z+1/2, -x+1/2, y+1/2' '-z+1/2, x+1/2, -y+1/2' 'y+1/2, z+1/2, x+1/2' '-y+1/2, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x+1/2' '-y+1/2, -z+1/2, x+1/2' 'y+1/2, x+1/2, z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' 'x+1/2, z+1/2, y+1/2' '-x+1/2, z+1/2, -y+1/2' '-x+1/2, -z+1/2, y+1/2' 'x+1/2, -z+1/2, -y+1/2' 'z+1/2, y+1/2, x+1/2' 'z+1/2, -y+1/2, -x+1/2' '-z+1/2, y+1/2, -x+1/2' '-z+1/2, -y+1/2, x+1/2' _cell_length_a 16.0760(19) _cell_length_b 16.0760(19) _cell_length_c 16.0760(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4154.6(9) _cell_formula_units_Z 2 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'rhombic dodecahedron' _exptl_crystal_colour black _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.355 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3588 _exptl_absorpt_coefficient_mu 14.930 _exptl_absorpt_correction_type semi-empirical _exptl_absorpt_correction_T_min 0.21109 _exptl_absorpt_correction_T_max 0.28773 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3873 _diffrn_reflns_av_R_equivalents 0.1384 _diffrn_reflns_av_sigmaI/netI 0.0535 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 23.98 _reflns_number_total 463 _reflns_number_gt 400 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+185.8749P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00059(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_BASF 0.17(3) _refine_ls_number_reflns 463 _refine_ls_number_parameters 50 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0778 _refine_ls_R_factor_gt 0.0635 _refine_ls_wR_factor_ref 0.1236 _refine_ls_wR_factor_gt 0.1146 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_restrained_S_all 1.095 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Te1 Te 0.0000 0.0000 0.0000 0.0381(17) Uani 1 24 d S . . Te2 Te 0.20172(12) 0.20172(12) 0.0003(3) 0.0942(13) Uani 1 2 d S . . Te3 Te 0.2579(2) 0.2579(2) 0.2579(2) 0.147(3) Uani 1 6 d S . . Sn1 Sn 0.16139(15) 0.16139(15) 0.16139(15) 0.0781(17) Uani 1 6 d S . . Hg1 Hg 0.09922(7) 0.09922(7) -0.09922(7) 0.0545(9) Uani 1 6 d S . . K1 K 0.5000 0.5000 -0.181(3) 0.140(14) Uiso 0.56 4 d SP . . K2 K 0.222(3) 0.410(3) -0.005(4) 0.100(13) Uiso 0.18 1 d P . . K3 K 0.376(3) 0.376(3) 0.208(5) 0.08(2) Uiso 0.13 2 d SP . . K3B K 0.337(6) 0.365(5) 0.170(6) 0.01(2) Uiso 0.03 1 d P . . O1A O 0.421(4) 0.309(4) 0.067(4) 0.031(15) Uiso 0.18 1 d P . . O1B O 0.390(3) 0.390(3) 0.038(4) 0.066(18) Uiso 0.38 2 d SP . . O2A O 0.347(4) 0.410(4) -0.102(3) 0.022(11) Uiso 0.20 1 d P . . O2B O 0.378(4) 0.453(4) -0.072(4) 0.030(15) Uiso 0.20 1 d P . . O2C O 0.412(13) 0.412(13) -0.093(18) 0.10(6) Uiso 0.13 2 d SP . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Te1 0.0381(17) 0.0381(17) 0.0381(17) 0.000 0.000 0.000 Te2 0.0884(16) 0.0884(16) 0.106(3) 0.0003(11) 0.0003(11) -0.0473(19) Te3 0.147(3) 0.147(3) 0.147(3) -0.056(2) -0.056(2) -0.056(2) Sn1 0.0781(17) 0.0781(17) 0.0781(17) -0.0291(12) -0.0291(12) -0.0291(12) Hg1 0.0545(9) 0.0545(9) 0.0545(9) 0.0117(7) 0.0117(7) -0.0117(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Te1 Hg1 2.763(2) 2 ? Te1 Hg1 2.763(2) 4 ? Te1 Hg1 2.763(2) 3 ? Te1 Hg1 2.763(2) . ? Te2 Sn1 2.748(4) . ? Te2 Hg1 2.826(3) . ? Te2 K3B 3.06(8) 43_554 ? Te2 K3B 3.06(8) 31_554 ? Te2 K2 3.36(5) . ? Te2 K2 3.36(6) 13 ? Te2 K3B 3.51(10) 48_554 ? Te2 K3B 3.51(10) 36_554 ? Te2 K1 3.75(2) 29_544 ? Te2 K1 3.75(2) 33_454 ? Te3 Sn1 2.688(7) . ? Sn1 Te2 2.748(4) 9 ? Sn1 Te2 2.748(4) 5 ? Hg1 Te2 2.826(3) 11 ? Hg1 Te2 2.826(3) 8 ? K1 O2C 2.5(3) 2_665 ? K1 O2C 2.5(3) . ? K1 O2B 2.74(7) 14_665 ? K1 O2B 2.74(7) 2_665 ? K1 O2B 2.74(7) . ? K1 O2B 2.74(7) 13 ? K1 K3 2.86(8) 4_565 ? K1 K3 2.86(8) 3_655 ? K1 O2A 3.13(6) 14_665 ? K1 O2A 3.13(6) 2_665 ? K1 O2A 3.13(6) 13 ? K1 O2A 3.13(6) . ? K2 O1A 1.34(9) 36_554 ? K2 O1A 1.82(9) 13 ? K2 O2B 1.83(7) 42 ? K2 O2A 1.90(9) 42 ? K2 K2 2.24(8) 42 ? K2 K2 2.24(8) 43_554 ? K2 O2A 2.54(7) . ? K2 O1B 2.62(6) 36_554 ? K2 O2C 2.62(8) 34 ? K2 K3B 2.63(10) 43_554 ? K2 O1B 2.80(6) . ? K2 O2B 2.81(7) . ? K3 K3B 0.90(9) . ? K3 K3B 0.90(9) 13 ? K3 O1A 2.61(10) . ? K3 O1A 2.61(10) 13 ? K3 O1B 2.76(11) . ? K3 Te2 2.76(5) 34 ? K3 Te2 2.76(5) 30 ? K3 K1 2.86(8) 3_655 ? K3 K2 3.13(8) 42 ? K3 K2 3.13(8) 30 ? K3B K3B 0.65(15) 13 ? K3B O1A 1.93(11) 13 ? K3B O1A 2.32(10) . ? K3B O1B 2.33(10) . ? K3B K2 2.63(10) 42 ? K3B Te2 3.06(8) 34 ? K3B K2 3.18(10) 30 ? K3B O2A 3.26(11) 42 ? K3B O2B 3.38(10) 4_565 ? K3B K1 3.41(9) 3_655 ? O1A K2 1.34(9) 30 ? O1A O1B 1.48(7) . ? O1A K2 1.82(9) 13 ? O1A K3B 1.93(11) 13 ? O1A K2 2.91(8) 31_554 ? O1A K2 3.22(8) 16_655 ? O1B O1A 1.48(7) 13 ? O1B K3B 2.33(10) 13 ? O1B K2 2.62(6) 42 ? O1B K2 2.62(6) 30 ? O1B K2 2.80(6) 13 ? O1B K2 3.30(7) 31_554 ? O1B K2 3.30(7) 43_554 ? O1B K1 3.40(7) 3_655 ? O2A O2B 0.98(7) . ? O2A O2C 1.1(2) . ? O2A O2A 1.43(13) 13 ? O2A K2 1.90(9) 43_554 ? O2A K3B 3.26(11) 43_554 ? O2A K2 3.31(8) 31_554 ? O2B O2C 0.92(10) . ? O2B O2B 1.71(12) 13 ? O2B K2 1.83(7) 43_554 ? O2B K2 3.14(8) 42 ? O2B K3B 3.38(10) 4_565 ? O2C O2B 0.92(10) 13 ? O2C O2A 1.1(2) 13 ? O2C K2 2.62(8) 31_554 ? O2C K2 2.62(8) 43_554 ? O2C K2 3.4(2) 13 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Hg1 Te1 Hg1 109.5 2 4 ? Hg1 Te1 Hg1 109.5 2 3 ? Hg1 Te1 Hg1 109.5 4 3 ? Hg1 Te1 Hg1 109.5 2 . ? Hg1 Te1 Hg1 109.5 4 . ? Hg1 Te1 Hg1 109.5 3 . ? Sn1 Te2 Hg1 104.96(13) . . ? Te3 Sn1 Te2 105.77(9) . 9 ? Te3 Sn1 Te2 105.77(9) . 5 ? Te2 Sn1 Te2 112.91(8) 9 5 ? Te3 Sn1 Te2 105.77(9) . . ? Te2 Sn1 Te2 112.91(8) 9 . ? Te2 Sn1 Te2 112.91(8) 5 . ? Te1 Hg1 Te2 110.27(9) . . ? Te1 Hg1 Te2 110.27(9) . 11 ? Te2 Hg1 Te2 108.66(9) . 11 ? Te1 Hg1 Te2 110.27(9) . 8 ? Te2 Hg1 Te2 108.66(9) . 8 ? Te2 Hg1 Te2 108.66(9) 11 8 ? _diffrn_measured_fraction_theta_max 0.781 _diffrn_reflns_theta_full 23.98 _diffrn_measured_fraction_theta_full 0.781 _refine_diff_density_max 0.449 _refine_diff_density_min -0.516 _refine_diff_density_rms 0.104 # Attachment '5-rev3.cif' data_5 _database_code_depnum_ccdc_archive 'CCDC 616334' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H8 Cs6 Hg4 O4 Sn3 Te13' _chemical_formula_weight 3686.75 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M R3m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-y, -x, z' '-x+y, y, z' 'x, x-y, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' '-y+2/3, -x+1/3, z+1/3' '-x+y+2/3, y+1/3, z+1/3' 'x+2/3, x-y+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-y+1/3, -x+2/3, z+2/3' '-x+y+1/3, y+2/3, z+2/3' 'x+1/3, x-y+2/3, z+2/3' _cell_length_a 15.880(2) _cell_length_b 15.880(2) _cell_length_c 17.367(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3793.0(11) _cell_formula_units_Z 3 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description cuboid _exptl_crystal_colour black _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 4.842 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4548 _exptl_absorpt_coefficient_mu 25.170 _exptl_absorpt_correction_type semi-empirical _exptl_absorpt_correction_T_min 0.21489 _exptl_absorpt_correction_T_max 0.39132 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2415 _diffrn_reflns_av_R_equivalents 0.0840 _diffrn_reflns_av_sigmaI/netI 0.0833 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 24.97 _reflns_number_total 1173 _reflns_number_gt 963 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0563P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_BASF 0.483(19) _refine_ls_number_reflns 1173 _refine_ls_number_parameters 67 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0573 _refine_ls_R_factor_gt 0.0474 _refine_ls_wR_factor_ref 0.1050 _refine_ls_wR_factor_gt 0.1025 _refine_ls_goodness_of_fit_ref 0.950 _refine_ls_restrained_S_all 0.950 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Hg1 Hg 0.0000 0.0000 0.32132(17) 0.0258(7) Uani 1 6 d S . . Hg2 Hg 0.09705(6) 0.19410(11) 0.11562(10) 0.0275(4) Uani 1 2 d S . . Sn1 Sn 0.30505(18) 0.15252(9) 0.24789(17) 0.0207(6) Uani 1 2 d S . . Te1 Te 0.0000 0.0000 0.1633(4) 0.0186(9) Uani 1 6 d S . . Te2 Te 0.19230(17) 0.09615(9) 0.37828(16) 0.0242(6) Uani 1 2 d S . . Te3 Te 0.08481(8) 0.16962(17) -0.04603(18) 0.0236(6) Uani 1 2 d S . . Te4 Te 0.00118(14) 0.29156(12) 0.16429(14) 0.0241(4) Uani 1 1 d . . . Cs1 Cs -0.16059(10) 0.16059(10) -0.0181(2) 0.0396(8) Uani 1 2 d S . . Cs2 Cs 0.16113(10) 0.3223(2) 0.3490(2) 0.0401(7) Uani 1 2 d S . . O1A O -0.252(4) 0.252(4) -0.125(9) 0.02(3) Uiso 0.20 2 d SP . . O1B O -0.360(4) 0.185(4) -0.072(4) 0.006(13) Uiso 0.23 1 d P . . O2A O -0.377(5) 0.195(5) 0.117(5) 0.012(19) Uiso 0.20 1 d P . . O2B O -0.092(5) 0.092(5) -0.195(9) 0.05(4) Uiso 0.27 2 d SP . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Hg1 0.0260(8) 0.0260(8) 0.025(2) 0.000 0.000 0.0130(4) Hg2 0.0281(6) 0.0310(8) 0.0244(10) 0.0015(8) 0.0008(4) 0.0155(4) Sn1 0.0206(12) 0.0210(9) 0.0202(16) -0.0014(5) -0.0027(11) 0.0103(6) Te1 0.0207(11) 0.0207(11) 0.014(2) 0.000 0.000 0.0104(6) Te2 0.0197(11) 0.0285(10) 0.0215(18) -0.0017(6) -0.0034(11) 0.0098(6) Te3 0.0292(10) 0.0186(12) 0.0195(17) 0.0036(10) 0.0018(5) 0.0093(6) Te4 0.0242(8) 0.0231(8) 0.0258(10) 0.0007(9) 0.0036(7) 0.0123(7) Cs1 0.0385(11) 0.0385(11) 0.039(2) 0.0027(7) -0.0027(7) 0.0171(12) Cs2 0.0382(11) 0.0430(17) 0.041(2) -0.0052(14) -0.0026(7) 0.0215(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Hg1 Te1 2.744(7) . ? Hg1 Te2 2.824(3) . ? Hg1 Te2 2.824(3) 2 ? Hg1 Te2 2.824(3) 3 ? Hg2 Te4 2.790(2) 5 ? Hg2 Te4 2.790(2) . ? Hg2 Te1 2.795(2) . ? Hg2 Te3 2.827(4) . ? Sn1 Te3 2.728(3) 8 ? Sn1 Te2 2.745(4) . ? Sn1 Te4 2.748(3) 5 ? Sn1 Te4 2.748(3) 3 ? Te1 Hg2 2.795(2) 2 ? Te1 Hg2 2.795(2) 3 ? Te2 Cs2 3.895(2) 3 ? Te2 Cs2 3.895(2) . ? Te3 Sn1 2.728(3) 15_554 ? Te3 Cs1 3.858(3) . ? Te3 Cs1 3.858(3) 3 ? Te4 Sn1 2.748(3) 2 ? Te4 Cs1 3.951(4) . ? Te4 Cs2 3.968(4) . ? Te4 Cs2 4.207(3) 14_554 ? Te4 Cs1 4.234(3) 9_455 ? Cs1 O1A 3.14(13) . ? Cs1 O1B 3.51(6) 4 ? Cs1 O1B 3.51(6) . ? Cs1 O2B 3.60(16) . ? Cs1 Te3 3.858(3) 2 ? Cs1 Te4 3.951(4) 4 ? Cs1 Te4 4.234(3) 17_444 ? Cs1 Te4 4.234(3) 14_554 ? Cs1 Hg2 4.499(3) 2 ? Cs2 O2B 3.07(14) 14 ? Cs2 O1B 3.19(6) 7 ? Cs2 O1B 3.19(6) 11_455 ? Cs2 O2A 3.36(8) 7 ? Cs2 O2A 3.36(8) 11_455 ? Cs2 Te2 3.895(2) 2 ? Cs2 Te4 3.968(4) 5 ? Cs2 Te4 4.207(3) 10 ? Cs2 Te4 4.207(3) 9_455 ? O1A O1B 1.76(10) 4 ? O1A O1B 1.76(10) . ? O1B O1B 1.50(11) 5_455 ? O1B Cs2 3.19(6) 13_444 ? O2A O2A 0.80(12) 5_455 ? O2A O2B 0.83(12) 8_455 ? O2A Cs2 3.36(8) 13_444 ? O2B O2A 0.83(12) 15_444 ? O2B O2A 0.83(12) 18_554 ? O2B Cs2 3.07(14) 9_454 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Te1 Hg1 Te2 110.51(8) . . ? Te1 Hg1 Te2 110.51(8) . 2 ? Te2 Hg1 Te2 108.42(8) . 2 ? Te1 Hg1 Te2 110.51(8) . 3 ? Te2 Hg1 Te2 108.42(8) . 3 ? Te2 Hg1 Te2 108.42(8) 2 3 ? Te4 Hg2 Te4 110.78(10) 5 . ? Te4 Hg2 Te1 111.66(8) 5 . ? Te4 Hg2 Te1 111.66(8) . . ? Te4 Hg2 Te3 110.98(6) 5 . ? Te4 Hg2 Te3 110.98(6) . . ? Te1 Hg2 Te3 100.40(14) . . ? Te3 Sn1 Te2 109.86(13) 8 . ? Te3 Sn1 Te4 101.75(7) 8 5 ? Te2 Sn1 Te4 113.24(8) . 5 ? Te3 Sn1 Te4 101.75(7) 8 3 ? Te2 Sn1 Te4 113.24(8) . 3 ? Te4 Sn1 Te4 115.52(15) 5 3 ? Hg1 Te1 Hg2 107.24(12) . 2 ? Hg1 Te1 Hg2 107.24(12) . 3 ? Hg2 Te1 Hg2 111.61(11) 2 3 ? Hg1 Te1 Hg2 107.24(12) . . ? Hg2 Te1 Hg2 111.61(11) 2 . ? Hg2 Te1 Hg2 111.61(11) 3 . ? Sn1 Te2 Hg1 103.89(12) . . ? Sn1 Te3 Hg2 97.70(11) 15_554 . ? Sn1 Te4 Hg2 103.07(8) 2 . ? _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 2.049 _refine_diff_density_min -2.538 _refine_diff_density_rms 0.396