# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 ############################################### # Powder data for Sb2Te, SbTe, Sb4Te3, Sb8Te9 # # Rad: Cu(Ka1); ? = 1.540598 Å # ############################################### data_Sb2Te Symmetry : Trigonal_H P Spacegroup : P -3 m 1 Cell_A : 4.2720(1) Å Cell_C : 17.6330(3) Å d (Å) 2Theta I/Io h k l 8.8073 10.04 0.18 0 0 2 4.4052 20.14 2.59 0 0 4 3.6185 24.58 0.26 0 1 1 3.5244 25.25 2.2 0 0 5 3.4093 26.12 1.1 0 1 2 3.1294 28.50 100 0 1 3 2.832 31.56 0.13 1 0 4 2.5518 35.14 0.2 0 1 5 2.3008 39.12 34.34 0 1 6 2.1358 42.28 31.27 1 1 0 2.0819 43.43 2.72 0 1 7 1.9591 46.31 5.7 0 0 9 1.9220 47.25 1.34 1 1 4 1.8934 48.01 2.47 0 1 8 1.8270 49.87 1.72 1 1 5 1.7643 51.77 16.73 0 2 3 1.5916 57.89 2.06 0 1 10 1.5656 58.95 9.96 0 2 6 #=============================================END data_SbTe Symmetry : Trigonal_H P Spacegroup : P -3 m 1 Cell_A : 4.260(1) Å Cell_C : 23.90(3) Å d(Å) 2Theta I/Io h k l 11.9374 7.40 1.13 0 0 2 4.7769 18.56 2.59 0 0 5 3.4123 26.09 1.65 0 0 7 3.3460 26.62 1.1 1 0 3 3.1376 28.42 100 0 1 4 2.7057 33.08 1.32 0 1 6 2.3212 38.76 35.94 0 1 8 2.1548 41.89 2.69 0 1 9 2.1296 42.41 32.17 1 1 0 2.0057 45.17 1.34 0 1 10 1.9914 45.51 5.98 0 0 12 1.9455 46.65 1.15 1 1 5 1.8721 48.59 1.77 0 1 11 1.8070 50.47 1.37 1 1 7 1.7624 51.83 16.88 0 2 4 1.6453 55.83 2.2 0 1 13 1.5696 58.78 9.78 0 2 8 #=============================================END data_Sb4Te3 Symmetry : Trigonal_H R Spacegroup : R -3 m Cell_A : 4.2754(6) Å Cell_C : 83.564(2) Å d (Å) 2Theta I/Io h k l 27.8547 3.17 0.41 0 0 3 5.5709 15.90 1.88 0 0 15 4.6425 19.10 2.47 0 0 18 3.9792 22.32 0.2 0 0 21 3.6990 24.04 0.79 1 0 1 3.6882 24.11 0.35 0 1 2 3.6458 24.40 0.26 1 0 4 3.6150 24.61 0.22 0 1 5 3.4818 25.56 1.77 0 0 24 3.3852 26.31 0.89 1 0 10 3.1464 28.34 100 0 1 14 3.0206 29.55 0.32 1 0 16 2.8325 31.56 0.29 1 0 19 2.7711 32.28 0.38 0 1 20 2.6514 33.78 0.23 1 0 22 2.5933 34.56 0.25 0 1 23 2.3236 38.72 31.82 1 0 28 2.2740 39.60 0.85 0 1 29 2.1377 42.24 30.93 1 1 0 2.1340 42.32 1.95 0 1 32 2.0477 44.19 0.58 1 0 34 2.0066 45.15 0.21 0 1 35 1.9958 45.41 0.56 1 1 15 1.9896 45.56 4.37 0 0 42 1.9417 46.75 1.06 1 1 18 1.9281 47.10 0.31 1 0 37 1.8907 48.08 1.52 0 1 38 1.8218 50.03 1.28 1 1 24 1.7682 51.65 14.1 2 0 14 1.7409 52.52 0.24 0 0 48 1.7207 53.187 0.43 1 0 43 1.6309 56.37 1.06 1 0 46 1.5732 58.63 7.09 0 2 28 #=============================================END data_Sb8Te9 Symmetry : Trigonal_H R Spacegroup : R-3m Cell_A : 4.2738(5) Å Cell_C : 102.6900(9) Å d (Å) 2Theta I/Io h k l 34.2341 2.58 1.16 0 0 3 17.0939 5.16 0.26 0 0 6 11.3990 7.74 0.64 0 0 9 8.5575 10.33 0.75 0 0 12 6.8419 12.92 0.68 0 0 15 5.7011 15.52 1.23 0 0 18 4.8866 18.13 2.06 0 0 21 3.6988 24.04 0.77 1 0 1 3.69164 24.09 0.27 0 1 2 3.5563 25.02 0.33 0 1 8 3.4230 26.01 2.03 0 0 30 3.3516 26.58 1.61 1 0 13 3.2063 27.80 0.32 1 0 16 3.1559 28.26 100 0 1 17 2.7496 32.54 0.62 1 0 25 2.7007 33.14 1.18 0 1 26 2.5587 35.04 0.49 0 1 29 2.4246 37.05 0.25 0 1 32 2.3400 38.44 34.99 1 0 34 2.2992 39.15 0.46 0 1 35 2.1825 41.33 2.27 0 1 38 2.1369 42.26 33.19 1 1 0 2.0135 44.99 5.3 0 0 51 2.0067 45.15 1.63 1 0 43 2.0011 45.28 0.4 1 1 18 1.9581 46.33 0.89 1 1 21 1.9116 47.53 0.45 1 0 46 1.8815 48.34 1.8 0 1 47 1.8127 50.30 1.86 1 1 30 1.8018 50.62 0.27 0 2 13 1.7694 51.61 16.48 2 0 17 1.7423 52.48 0.21 1 0 52 1.7115 53.50 0.67 0 0 60 1.6758 54.73 0.25 2 0 26 1.6670 55.04 1.65 1 0 55 1.6090 57.21 0.27 1 1 42 1.5780 58.44 9.07 0 2 34 #=============================================END data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Kanatzidis, Mercouri' 'Poudeu Poudeu, Pierre Ferdinand' _publ_contact_author_name 'Prof. Mercouri Kanatzidis' _publ_contact_author_address ; Prof. Mercouri Kanatzidis Department of Chemistry Michigan State University Department of Chemistry East Lansing MI 48824 UNITED STATES OF AMERICA ; _publ_contact_author_email KANATZID@CHEMISTRY.MSU.EDU _publ_section_title ; Design in solid state chemistry based on phase homologies. Sb4Te3 and Sb8Te9 as new members of the series (Sb~2~Te~3~)~m~\.(Sb~2~)~n~ ; data_Sb4Te3 _database_code_depnum_ccdc_archive 'CCDC 261145' _audit_creation_method SHELXL-97 _chemical_name_systematic ; antimony telluride (4/3) ; _chemical_name_common 'Sb4 Te3' _chemical_melting_point '540\% C' _chemical_formula_moiety ? _chemical_formula_sum 'Sb4 Te3' _chemical_formula_weight 869.8 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Sb Sb -0.5866 1.5461 '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 Trigonal _symmetry_space_group_name_H-M R-3m 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' '-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 4.2754(6) _cell_length_b 4.2754(6) _cell_length_c 83.564(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1322.8(4) _cell_formula_units_Z 6 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4015 _cell_measurement_theta_min 1.15 _cell_measurement_theta_max 26 _exptl_crystal_description prismatic _exptl_crystal_colour silver-like _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.120 _exptl_crystal_size_min 0.076 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 6.551 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2160 _exptl_absorpt_coefficient_mu 21.753 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.0536 _exptl_absorpt_correction_T_max 0.1937 _exptl_absorpt_process_details ; crystal description with a video camera using FacietVideo (STOE & Cie GmbH, 2002) and optimized with X-SHAPE (STOE & Cie GmbH, 1999) using a set of equivalent reflections ; _exptl_special_details ; collection of intensity data: Two set of data were collected; phi = 0 \% with omega scanning from 0\% to 180\% and phi = 90\% with omega scanning from 0\% to 90\% at a step of 0.7\%, The crystal to detector distance was 100.0 mm with 2 min exposure time per frame.lattice parameters determined using STOE IPDS-II diffraction ; _diffrn_ambient_temperature 293(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 'IPDS-II (STOE)' _diffrn_measurement_method 'incremental omega oscillation 0.7\%' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count 0.7\% _diffrn_standards_interval_time '2 min' _diffrn_standards_decay_% ? _diffrn_reflns_number 4015 _diffrn_reflns_av_R_equivalents 0.0949 _diffrn_reflns_av_sigmaI/netI 0.0277 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -102 _diffrn_reflns_limit_l_max 102 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 25.90 _reflns_number_total 407 _reflns_number_gt 253 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'WinXpose (STOE & Cie GmbH, 2003)' _computing_cell_refinement 'Cell (STOE & Cie GmbH, 2003)' _computing_data_reduction 'Integrate (STOE & Cie GmbH, 2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond (Brandenburg, 1995)' _computing_publication_material 'Shelxl-97 and Diamond' _refine_special_details ; Assignments of Te positions using bond valence sum (BVS) calculation and the analogy with the structure of Sb~2~Te~3~. The BVS were 2.028, 2.046 and 1.989 for Te1, Te2 and Te3. 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^)+(0.0639P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 407 _refine_ls_number_parameters 22 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0663 _refine_ls_R_factor_gt 0.0410 _refine_ls_wR_factor_ref 0.1064 _refine_ls_wR_factor_gt 0.0964 _refine_ls_goodness_of_fit_ref 0.905 _refine_ls_restrained_S_all 0.905 _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 Sb1 Sb -0.3333 0.3333 0.014193(19) 0.0391(5) Uani 1 6 d S . . Sb2 Sb 0.0000 0.0000 0.03261(2) 0.0415(5) Uani 1 6 d S . . Sb3 Sb -0.3333 0.3333 0.082448(18) 0.0458(6) Uani 1 6 d S . . Sb4 Sb 0.3333 -0.3333 0.13041(2) 0.0450(6) Uani 1 6 d S . . Te1 Te -0.6667 0.6667 0.06148(2) 0.0383(5) Uani 1 6 d S . . Te2 Te 0.0000 0.0000 0.10581(2) 0.0368(5) Uani 1 6 d S . . Te3 Te 0.6667 -0.6667 0.15048(2) 0.0405(5) Uani 1 6 d S . . 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 Sb1 0.0347(8) 0.0347(8) 0.0478(8) 0.000 0.000 0.0174(4) Sb2 0.0335(8) 0.0335(8) 0.0575(10) 0.000 0.000 0.0168(4) Sb3 0.0367(8) 0.0367(8) 0.0642(12) 0.000 0.000 0.0183(4) Sb4 0.0350(8) 0.0350(8) 0.0649(10) 0.000 0.000 0.0175(4) Te1 0.0355(6) 0.0355(6) 0.0440(7) 0.000 0.000 0.0177(3) Te2 0.0335(6) 0.0335(6) 0.0434(7) 0.000 0.000 0.0167(3) Te3 0.0354(7) 0.0354(7) 0.0508(8) 0.000 0.000 0.0177(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 Sb1 Sb2 2.9087(14) 1_565 yes Sb1 Sb2 2.9087(14) . yes Sb1 Sb2 2.9087(14) 1_455 yes Sb1 Sb1 3.423(2) 19_455 no Sb1 Sb1 3.423(2) 19_565 no Sb1 Sb1 3.423(2) 19_465 no Sb2 Sb1 2.9087(14) 1_545 yes Sb2 Sb1 2.9087(14) 1_655 yes Sb2 Te1 3.4518(19) 1_655 no Sb2 Te1 3.4518(19) 1_645 no Sb2 Te1 3.4518(19) 1_545 no Sb3 Te1 3.0271(14) 1_545 yes Sb3 Te1 3.0271(14) 1_655 yes Sb3 Te1 3.0271(14) . yes Sb3 Te2 3.1470(15) . yes Sb3 Te2 3.1470(15) 1_565 yes Sb3 Te2 3.1470(15) 1_455 yes Sb4 Te3 2.9843(16) 1_565 yes Sb4 Te3 2.9843(16) 1_455 yes Sb4 Te3 2.9843(16) . yes Sb4 Te2 3.2125(15) 1_545 yes Sb4 Te2 3.2125(15) . yes Sb4 Te2 3.2125(15) 1_655 yes Te1 Sb3 3.0271(14) 1_565 yes Te1 Sb3 3.0271(14) 1_455 yes Te1 Sb2 3.4518(19) 1_455 no Te1 Sb2 3.4518(19) 1_465 no Te1 Sb2 3.4518(19) 1_565 no Te2 Sb3 3.1470(15) 1_545 yes Te2 Sb3 3.1470(15) 1_655 yes Te2 Sb4 3.2126(15) 1_565 yes Te2 Sb4 3.2126(15) 1_455 yes Te3 Sb4 2.9843(16) 1_545 yes Te3 Sb4 2.9843(16) 1_655 yes Te3 Te3 3.662(3) 25_635 no Te3 Te3 3.662(3) 25_645 no Te3 Te3 3.662(3) 25_535 no 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 Sb2 Sb1 Sb2 94.60(6) 1_565 . yes Sb2 Sb1 Sb2 94.60(6) 1_565 1_455 yes Sb2 Sb1 Sb2 94.60(6) . 1_455 yes Sb2 Sb1 Sb1 168.08(7) 1_565 19_455 yes Sb2 Sb1 Sb1 93.47(3) . 19_455 yes Sb2 Sb1 Sb1 93.47(3) 1_455 19_455 yes Sb2 Sb1 Sb1 93.47(3) 1_565 19_565 yes Sb2 Sb1 Sb1 93.47(3) . 19_565 yes Sb2 Sb1 Sb1 168.08(7) 1_455 19_565 yes Sb1 Sb1 Sb1 77.28(6) 19_455 19_565 yes Sb2 Sb1 Sb1 93.47(3) 1_565 19_465 yes Sb2 Sb1 Sb1 168.08(7) . 19_465 yes Sb2 Sb1 Sb1 93.47(3) 1_455 19_465 yes Sb1 Sb1 Sb1 77.28(6) 19_455 19_465 yes Sb1 Sb1 Sb1 77.28(6) 19_565 19_465 yes Sb1 Sb2 Sb1 94.60(6) 1_545 . yes Sb1 Sb2 Sb1 94.60(6) 1_545 1_655 yes Sb1 Sb2 Sb1 94.60(6) . 1_655 yes Sb1 Sb2 Te1 167.59(6) 1_545 1_655 yes Sb1 Sb2 Te1 93.80(3) . 1_655 yes Sb1 Sb2 Te1 93.80(3) 1_655 1_655 yes Sb1 Sb2 Te1 93.80(3) 1_545 1_645 yes Sb1 Sb2 Te1 167.59(6) . 1_645 yes Sb1 Sb2 Te1 93.80(3) 1_655 1_645 yes Te1 Sb2 Te1 76.53(5) 1_655 1_645 yes Sb1 Sb2 Te1 93.80(3) 1_545 1_545 yes Sb1 Sb2 Te1 93.80(3) . 1_545 yes Sb1 Sb2 Te1 167.59(6) 1_655 1_545 yes Te1 Sb2 Te1 76.53(5) 1_655 1_545 yes Te1 Sb2 Te1 76.53(5) 1_645 1_545 yes Te1 Sb3 Te1 89.85(5) 1_545 1_655 yes Te1 Sb3 Te1 89.85(5) 1_545 . yes Te1 Sb3 Te1 89.85(5) 1_655 . yes Te1 Sb3 Te2 92.25(3) 1_545 . yes Te1 Sb3 Te2 92.25(3) 1_655 . yes Te1 Sb3 Te2 177.03(6) . . yes Te1 Sb3 Te2 177.03(6) 1_545 1_565 yes Te1 Sb3 Te2 92.25(3) 1_655 1_565 yes Te1 Sb3 Te2 92.25(3) . 1_565 yes Te2 Sb3 Te2 85.58(5) . 1_565 yes Te1 Sb3 Te2 92.25(3) 1_545 1_455 yes Te1 Sb3 Te2 177.03(6) 1_655 1_455 yes Te1 Sb3 Te2 92.25(3) . 1_455 yes Te2 Sb3 Te2 85.58(5) . 1_455 yes Te2 Sb3 Te2 85.58(5) 1_565 1_455 yes Te3 Sb4 Te3 91.50(6) 1_565 1_455 yes Te3 Sb4 Te3 91.50(6) 1_565 . yes Te3 Sb4 Te3 91.50(6) 1_455 . yes Te3 Sb4 Te2 174.40(6) 1_565 1_545 yes Te3 Sb4 Te2 92.40(3) 1_455 1_545 yes Te3 Sb4 Te2 92.40(3) . 1_545 yes Te3 Sb4 Te2 92.40(3) 1_565 . yes Te3 Sb4 Te2 92.40(3) 1_455 . yes Te3 Sb4 Te2 174.40(6) . . yes Te2 Sb4 Te2 83.43(5) 1_545 . yes Te3 Sb4 Te2 92.40(3) 1_565 1_655 yes Te3 Sb4 Te2 174.40(6) 1_455 1_655 yes Te3 Sb4 Te2 92.40(3) . 1_655 yes Te2 Sb4 Te2 83.43(5) 1_545 1_655 yes Te2 Sb4 Te2 83.43(5) . 1_655 yes Sb3 Te1 Sb3 89.85(5) 1_565 1_455 yes Sb3 Te1 Sb3 89.85(5) 1_565 . yes Sb3 Te1 Sb3 89.85(5) 1_455 . yes Sb3 Te1 Sb2 171.02(6) 1_565 1_455 yes Sb3 Te1 Sb2 96.49(3) 1_455 1_455 yes Sb3 Te1 Sb2 96.49(3) . 1_455 yes Sb3 Te1 Sb2 96.49(3) 1_565 1_465 yes Sb3 Te1 Sb2 96.49(3) 1_455 1_465 yes Sb3 Te1 Sb2 171.02(6) . 1_465 yes Sb2 Te1 Sb2 76.53(5) 1_455 1_465 yes Sb3 Te1 Sb2 96.49(3) 1_565 1_565 yes Sb3 Te1 Sb2 171.02(6) 1_455 1_565 yes Sb3 Te1 Sb2 96.49(3) . 1_565 yes Sb2 Te1 Sb2 76.53(5) 1_455 1_565 yes Sb2 Te1 Sb2 76.53(5) 1_465 1_565 yes Sb3 Te2 Sb3 85.58(5) 1_545 . yes Sb3 Te2 Sb3 85.58(5) 1_545 1_655 yes Sb3 Te2 Sb3 85.58(5) . 1_655 yes Sb3 Te2 Sb4 95.49(3) 1_545 . yes Sb3 Te2 Sb4 178.54(6) . . yes Sb3 Te2 Sb4 95.49(3) 1_655 . yes Sb3 Te2 Sb4 178.54(6) 1_545 1_565 yes Sb3 Te2 Sb4 95.49(3) . 1_565 yes Sb3 Te2 Sb4 95.49(3) 1_655 1_565 yes Sb4 Te2 Sb4 83.43(5) . 1_565 yes Sb3 Te2 Sb4 95.49(3) 1_545 1_455 yes Sb3 Te2 Sb4 95.49(3) . 1_455 yes Sb3 Te2 Sb4 178.54(6) 1_655 1_455 yes Sb4 Te2 Sb4 83.43(5) . 1_455 yes Sb4 Te2 Sb4 83.43(5) 1_565 1_455 yes Sb4 Te3 Sb4 91.50(6) 1_545 1_655 yes Sb4 Te3 Sb4 91.50(6) 1_545 . yes Sb4 Te3 Sb4 91.50(6) 1_655 . yes Sb4 Te3 Te3 97.84(2) 1_545 25_635 yes Sb4 Te3 Te3 97.84(3) 1_655 25_635 yes Sb4 Te3 Te3 166.58(7) . 25_635 yes Sb4 Te3 Te3 166.58(7) 1_545 25_645 yes Sb4 Te3 Te3 97.84(3) 1_655 25_645 yes Sb4 Te3 Te3 97.84(3) . 25_645 yes Te3 Te3 Te3 71.44(6) 25_635 25_645 yes Sb4 Te3 Te3 97.84(2) 1_545 25_535 yes Sb4 Te3 Te3 166.58(7) 1_655 25_535 yes Sb4 Te3 Te3 97.84(2) . 25_535 yes Te3 Te3 Te3 71.44(6) 25_635 25_535 yes Te3 Te3 Te3 71.44(6) 25_645 25_535 yes _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 25.90 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 1.916 _refine_diff_density_min -1.526 _refine_diff_density_rms 0.309 #===========================================================END data_Sb8Te9 _database_code_depnum_ccdc_archive 'CCDC 261146' _audit_creation_method SHELXL-97 _chemical_name_systematic ; antimony telluride (8/9) ; _chemical_name_common 'Sb8 Te9' _chemical_melting_point 540\% _chemical_formula_moiety ? _chemical_formula_sum 'Sb8 Te9' _chemical_formula_weight 2122.4 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Sb Sb -0.5866 1.5461 '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 Trigonal _symmetry_space_group_name_H-M R-3m 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' '-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 4.2738(5) _cell_length_b 4.2738(5) _cell_length_c 102.69(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1624.4(5) _cell_formula_units_Z 3 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6155 _cell_measurement_theta_min 0.59 _cell_measurement_theta_max 28.52 _exptl_crystal_description prismatic _exptl_crystal_colour silver-like _exptl_crystal_size_max none _exptl_crystal_size_mid none _exptl_crystal_size_min none _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 6.509 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2628 _exptl_absorpt_coefficient_mu 21.682 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.331 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ; The absorption correction was based on 903 unique reflections using the SADABS program. Sheldric, G. M. (1996). SADABS. Bruker Area Detector Absorption Correction Software. University of Gottingen, Germany. ; _exptl_special_details ; The data collection nominally covered a full sphere of reciprocal space, by a combination of four sets of exposures; each set had a different \f angle for the crystal and each exposure covered 0.3\% in \w. The crystal-to-detector distance was 5 cm. Coverage of the unique set is 96% complete to at 28\% in \q. Crystal decay was monitored by repeating the initial frames at the end of data collection and analyzing the duplicate reflections. ; _diffrn_ambient_temperature 293(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6155 _diffrn_reflns_av_R_equivalents 0.0474 _diffrn_reflns_av_sigmaI/netI 0.0205 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -131 _diffrn_reflns_limit_l_max 131 _diffrn_reflns_theta_min 0.59 _diffrn_reflns_theta_max 28.52 _reflns_number_total 623 _reflns_number_gt 528 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond (Brandenburg, 1995)' _computing_publication_material 'SHELXL-97 and Diamond' _refine_special_details ; Assignments of Te positions using bond valence sum (BVS) calculation and the analogy with the structure of Sb~2~Te~3~. The BVS were 2.046, 2.052, 1.908, 2.076 and 1.935 for Te1, Te2 Te3, Te4 and Te5. 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^)+(0.0168P)^2^+63.2276P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment none _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00043(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 623 _refine_ls_number_parameters 28 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0347 _refine_ls_R_factor_gt 0.0292 _refine_ls_wR_factor_ref 0.0778 _refine_ls_wR_factor_gt 0.0748 _refine_ls_goodness_of_fit_ref 1.196 _refine_ls_restrained_S_all 1.196 _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 Sb1 Sb 0.0000 0.0000 0.118145(10) 0.0247(3) Uani 1 6 d S . . Sb2 Sb 0.6667 0.3333 0.159135(9) 0.0174(3) Uani 1 6 d S . . Sb3 Sb -0.6667 0.6667 0.079169(11) 0.0249(3) Uani 1 6 d S . . Sb4 Sb 0.3333 0.6667 0.019419(10) 0.0217(3) Uani 1 6 d S . . Te1 Te 0.3333 0.6667 0.134887(9) 0.0166(3) Uani 1 6 d S . . Te2 Te -0.3333 0.3333 0.098920(8) 0.0148(3) Uani 1 6 d S . . Te3 Te 0.6667 0.3333 0.036000(8) 0.0167(3) Uani 1 6 d S . . Te4 Te 0.0000 0.0000 0.0000 0.0142(3) Uani 1 12 d S . . Te5 Te 0.0000 0.0000 0.062689(9) 0.0176(3) Uani 1 6 d S . . 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 Sb1 0.0193(4) 0.0193(4) 0.0357(6) 0.000 0.000 0.00964(18) Sb2 0.0142(3) 0.0142(3) 0.0240(5) 0.000 0.000 0.00708(17) Sb3 0.0198(4) 0.0198(4) 0.0352(6) 0.000 0.000 0.00989(19) Sb4 0.0184(4) 0.0184(4) 0.0282(5) 0.000 0.000 0.00920(18) Te1 0.0146(3) 0.0146(3) 0.0204(5) 0.000 0.000 0.00731(17) Te2 0.0139(3) 0.0139(3) 0.0165(5) 0.000 0.000 0.00694(17) Te3 0.0160(3) 0.0160(3) 0.0181(5) 0.000 0.000 0.00801(17) Te4 0.0133(4) 0.0133(4) 0.0160(6) 0.000 0.000 0.0066(2) Te5 0.0158(3) 0.0158(3) 0.0213(5) 0.000 0.000 0.00792(17) _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 Sb1 Te1 3.0073(9) 1_545 yes Sb1 Te1 3.0073(9) . yes Sb1 Te1 3.0073(9) 1_445 yes Sb1 Te2 3.1600(9) . yes Sb1 Te2 3.1600(9) 1_545 yes Sb1 Te2 3.1600(9) 1_655 yes Sb2 Sb2 2.9123(11) 25_655 yes Sb2 Sb2 2.9124(11) 25_665 yes Sb2 Sb2 2.9124(11) 25 yes Sb2 Te1 3.5055(10) 1_545 no Sb2 Te1 3.5055(10) 1_655 no Sb2 Te1 3.5055(10) . no Sb3 Te5 2.9921(8) 1_455 yes Sb3 Te5 2.9921(8) 1_465 yes Sb3 Te5 2.9921(8) 1_565 yes Sb3 Te2 3.1941(9) 1_565 yes Sb3 Te2 3.1941(9) 1_455 yes Sb3 Te2 3.1941(9) . yes Sb4 Te3 2.9979(8) 1_565 yes Sb4 Te3 2.9979(8) 1_455 yes Sb4 Te3 2.9979(8) . yes Sb4 Te4 3.1725(7) . yes Sb4 Te4 3.1725(7) 1_565 yes Sb4 Te4 3.1725(7) 1_665 yes Te1 Sb1 3.0073(9) 1_565 yes Te1 Sb1 3.0073(9) 1_665 yes Te1 Sb2 3.5055(10) 1_565 no Te1 Sb2 3.5055(10) 1_455 no Te2 Sb1 3.1600(9) 1_565 yes Te2 Sb1 3.1600(9) 1_455 yes Te2 Sb3 3.1941(9) 1_545 yes Te2 Sb3 3.1941(9) 1_655 yes Te3 Sb4 2.9979(8) 1_545 yes Te3 Sb4 2.9979(8) 1_655 yes Te3 Te5 3.6878(11) 1_665 no Te3 Te5 3.6878(11) 1_655 no Te3 Te5 3.6878(11) . no Te4 Sb4 3.1725(7) 19 yes Te4 Sb4 3.1725(7) 19_565 yes Te4 Sb4 3.1725(7) 1_545 yes Te4 Sb4 3.1725(7) 19_665 yes Te4 Sb4 3.1725(7) 1_445 yes Te5 Sb3 2.9921(8) 1_655 yes Te5 Sb3 2.9921(8) 1_645 yes Te5 Sb3 2.9921(8) 1_545 yes Te5 Te3 3.6878(11) 1_445 no Te5 Te3 3.6878(11) 1_455 no 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 Sb1 Te1 90.56(3) 1_545 . yes Te1 Sb1 Te1 90.56(3) 1_545 1_445 yes Te1 Sb1 Te1 90.56(3) . 1_445 yes Te1 Sb1 Te2 176.20(4) 1_545 . yes Te1 Sb1 Te2 92.109(17) . . yes Te1 Sb1 Te2 92.109(17) 1_445 . yes Te1 Sb1 Te2 92.109(16) 1_545 1_545 yes Te1 Sb1 Te2 176.20(4) . 1_545 yes Te1 Sb1 Te2 92.109(16) 1_445 1_545 yes Te2 Sb1 Te2 85.10(3) . 1_545 yes Te1 Sb1 Te2 92.109(17) 1_545 1_655 yes Te1 Sb1 Te2 92.109(17) . 1_655 yes Te1 Sb1 Te2 176.20(4) 1_445 1_655 yes Te2 Sb1 Te2 85.10(3) . 1_655 yes Te2 Sb1 Te2 85.10(3) 1_545 1_655 yes Sb2 Sb2 Sb2 94.40(4) 25_655 25_665 yes Sb2 Sb2 Sb2 94.40(4) 25_655 25 yes Sb2 Sb2 Sb2 94.40(4) 25_665 25 yes Sb2 Sb2 Te1 94.54(2) 25_655 1_545 yes Sb2 Sb2 Te1 166.83(4) 25_665 1_545 yes Sb2 Sb2 Te1 94.54(2) 25 1_545 yes Sb2 Sb2 Te1 94.54(2) 25_655 1_655 yes Sb2 Sb2 Te1 94.54(2) 25_665 1_655 yes Sb2 Sb2 Te1 166.83(4) 25 1_655 yes Te1 Sb2 Te1 75.12(3) 1_545 1_655 yes Sb2 Sb2 Te1 166.83(4) 25_655 . yes Sb2 Sb2 Te1 94.54(2) 25_665 . yes Sb2 Sb2 Te1 94.54(2) 25 . yes Te1 Sb2 Te1 75.12(3) 1_545 . yes Te1 Sb2 Te1 75.12(3) 1_655 . yes Te5 Sb3 Te5 91.15(3) 1_455 1_465 yes Te5 Sb3 Te5 91.15(3) 1_455 1_565 yes Te5 Sb3 Te5 91.15(3) 1_465 1_565 yes Te5 Sb3 Te2 175.03(3) 1_455 1_565 yes Te5 Sb3 Te2 92.329(16) 1_465 1_565 yes Te5 Sb3 Te2 92.329(16) 1_565 1_565 yes Te5 Sb3 Te2 92.329(16) 1_455 1_455 yes Te5 Sb3 Te2 92.329(16) 1_465 1_455 yes Te5 Sb3 Te2 175.03(3) 1_565 1_455 yes Te2 Sb3 Te2 83.98(3) 1_565 1_455 yes Te5 Sb3 Te2 92.329(16) 1_455 . yes Te5 Sb3 Te2 175.03(3) 1_465 . yes Te5 Sb3 Te2 92.329(16) 1_565 . yes Te2 Sb3 Te2 83.98(3) 1_565 . yes Te2 Sb3 Te2 83.98(3) 1_455 . yes Te3 Sb4 Te3 90.93(3) 1_565 1_455 yes Te3 Sb4 Te3 90.93(3) 1_565 . yes Te3 Sb4 Te3 90.93(3) 1_455 . yes Te3 Sb4 Te4 175.66(3) 1_565 . yes Te3 Sb4 Te4 92.115(14) 1_455 . yes Te3 Sb4 Te4 92.115(14) . . yes Te3 Sb4 Te4 92.115(14) 1_565 1_565 yes Te3 Sb4 Te4 92.115(14) 1_455 1_565 yes Te3 Sb4 Te4 175.66(3) . 1_565 yes Te4 Sb4 Te4 84.69(2) . 1_565 yes Te3 Sb4 Te4 92.115(14) 1_565 1_665 yes Te3 Sb4 Te4 175.66(3) 1_455 1_665 yes Te3 Sb4 Te4 92.115(14) . 1_665 yes Te4 Sb4 Te4 84.69(2) . 1_665 yes Te4 Sb4 Te4 84.69(2) 1_565 1_665 yes Sb1 Te1 Sb1 90.56(3) . 1_565 no Sb1 Te1 Sb1 90.56(3) . 1_665 no Sb1 Te1 Sb1 90.56(3) 1_565 1_665 no Sb1 Te1 Sb2 169.61(3) . 1_565 no Sb1 Te1 Sb2 96.737(19) 1_565 1_565 no Sb1 Te1 Sb2 96.737(19) 1_665 1_565 no Sb1 Te1 Sb2 96.737(19) . 1_455 no Sb1 Te1 Sb2 96.737(19) 1_565 1_455 no Sb1 Te1 Sb2 169.61(3) 1_665 1_455 no Sb2 Te1 Sb2 75.12(3) 1_565 1_455 no Sb1 Te1 Sb2 96.737(19) . . no Sb1 Te1 Sb2 169.61(3) 1_565 . no Sb1 Te1 Sb2 96.737(19) 1_665 . no Sb2 Te1 Sb2 75.12(3) 1_565 . no Sb2 Te1 Sb2 75.12(3) 1_455 . no Sb1 Te2 Sb1 85.10(3) 1_565 . no Sb1 Te2 Sb1 85.10(3) 1_565 1_455 no Sb1 Te2 Sb1 85.10(3) . 1_455 no Sb1 Te2 Sb3 179.24(3) 1_565 1_545 no Sb1 Te2 Sb3 95.46(2) . 1_545 no Sb1 Te2 Sb3 95.456(19) 1_455 1_545 no Sb1 Te2 Sb3 95.46(2) 1_565 1_655 no Sb1 Te2 Sb3 95.46(2) . 1_655 no Sb1 Te2 Sb3 179.24(3) 1_455 1_655 no Sb3 Te2 Sb3 83.98(3) 1_545 1_655 no Sb1 Te2 Sb3 95.456(19) 1_565 . no Sb1 Te2 Sb3 179.24(3) . . no Sb1 Te2 Sb3 95.46(2) 1_455 . no Sb3 Te2 Sb3 83.98(3) 1_545 . no Sb3 Te2 Sb3 83.98(3) 1_655 . no Sb4 Te3 Sb4 90.93(3) 1_545 1_655 no Sb4 Te3 Sb4 90.93(3) 1_545 . no Sb4 Te3 Sb4 90.93(3) 1_655 . no Sb4 Te3 Te5 166.60(3) 1_545 1_665 no Sb4 Te3 Te5 98.437(19) 1_655 1_665 no Sb4 Te3 Te5 98.437(19) . 1_665 no Sb4 Te3 Te5 98.437(19) 1_545 1_655 no Sb4 Te3 Te5 98.437(19) 1_655 1_655 no Sb4 Te3 Te5 166.60(3) . 1_655 no Te5 Te3 Te5 70.82(3) 1_665 1_655 no Sb4 Te3 Te5 98.437(19) 1_545 . no Sb4 Te3 Te5 166.60(3) 1_655 . no Sb4 Te3 Te5 98.437(19) . . no Te5 Te3 Te5 70.82(3) 1_665 . no Te5 Te3 Te5 70.82(3) 1_655 . no Sb4 Te4 Sb4 84.69(2) 19 19_565 no Sb4 Te4 Sb4 95.31(2) 19 1_545 no Sb4 Te4 Sb4 180.00(3) 19_565 1_545 no Sb4 Te4 Sb4 180.00(3) 19 . no Sb4 Te4 Sb4 95.31(2) 19_565 . no Sb4 Te4 Sb4 84.69(2) 1_545 . no Sb4 Te4 Sb4 84.69(2) 19 19_665 no Sb4 Te4 Sb4 84.69(2) 19_565 19_665 no Sb4 Te4 Sb4 95.31(2) 1_545 19_665 no Sb4 Te4 Sb4 95.31(2) . 19_665 no Sb4 Te4 Sb4 95.31(2) 19 1_445 no Sb4 Te4 Sb4 95.31(2) 19_565 1_445 no Sb4 Te4 Sb4 84.69(2) 1_545 1_445 no Sb4 Te4 Sb4 84.69(2) . 1_445 no Sb4 Te4 Sb4 180.00(3) 19_665 1_445 no Sb3 Te5 Sb3 91.15(3) 1_655 1_645 no Sb3 Te5 Sb3 91.15(3) 1_655 1_545 no Sb3 Te5 Sb3 91.15(3) 1_645 1_545 no Sb3 Te5 Te3 166.44(3) 1_655 1_445 no Sb3 Te5 Te3 98.307(19) 1_645 1_445 no Sb3 Te5 Te3 98.307(19) 1_545 1_445 no Sb3 Te5 Te3 98.307(19) 1_655 1_455 no Sb3 Te5 Te3 166.44(3) 1_645 1_455 no Sb3 Te5 Te3 98.307(19) 1_545 1_455 no Te3 Te5 Te3 70.82(3) 1_445 1_455 no Sb3 Te5 Te3 98.307(19) 1_655 . no Sb3 Te5 Te3 98.307(19) 1_645 . no Sb3 Te5 Te3 166.44(3) 1_545 . no Te3 Te5 Te3 70.82(3) 1_445 . no Te3 Te5 Te3 70.82(3) 1_455 . no _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 28.52 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 1.417 _refine_diff_density_min -1.963 _refine_diff_density_rms 0.235