# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 # SUBMISSION DETAILS _publ_contact_author_name ; Dr. Oliver Oeckler ; _publ_contact_author_address ; Department Chemie und Biochemie Ludwig-Maximilians-Universit\"at Butenandtstr. 5-13 (Haus D) 81377 Muenchen, Germany ; _publ_contact_author_email oliver.oeckler@gmx.de _publ_contact_author_fax ; +49/89/2180-77440 ; _publ_contact_author_phone ; +49/89/2180-77421 ; _publ_requested_journal 'Dalton Trans.' _publ_requested_coeditor_name ? _publ_contact_letter ; Please consider this CIF submission as supplementary material for Dalton Trans. ; #============================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; A new series of long-range ordered metastable phases (MTe)n(Sb2Te3)m(Sb2)k (m, n, k > 0; M = Ge, Ag) ; loop_ _publ_author_name _publ_author_address 'Matthias N. Schneider' ; Department Chemie und Biochemie Ludwig-Maximilians-Universit\"at Butenandtstr. 5-13 (Haus D) 81377 M\"unchen Germany ; 'Markus Seibald' ; Department Chemie und Biochemie Ludwig-Maximilians-Universit\"at Butenandtstr. 5-13 (Haus D) 81377 M\"unchen Germany ; 'Oliver Oeckler' ; Department Chemie und Biochemie Ludwig-Maximilians-Universit\"at Butenandtstr. 5-13 (Haus D) 81377 M\"unchen Germany ; #============================================================================== # CRYSTAL DATA data_p-3m1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Silver antimony telluride ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Ag0.24 Sb10.76 Te4' _chemical_formula_weight 1846.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 'P-3m1' 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, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z' '-x+y, y, z' 'x, x-y, z' _cell_length_a 4.2820(10) _cell_length_b 4.2820(10) _cell_length_c 28.636(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 454.71(17) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1675 _cell_measurement_theta_min 5 _cell_measurement_theta_max 30 _exptl_crystal_description platelet _exptl_crystal_colour metallic_dark_grey _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 6.742 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 768 _exptl_absorpt_coefficient_mu 22.215 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.028 _exptl_absorpt_correction_T_max 0.641 _exptl_absorpt_process_details 'from equivalents, scaled' _exptl_special_details ; ? ; _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 4373 _diffrn_reflns_av_R_equivalents 0.1040 _diffrn_reflns_av_sigmaI/netI 0.0462 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 2.85 _diffrn_reflns_theta_max 29.90 _reflns_number_total 601 _reflns_number_gt 333 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS software package (Stoe, 2002)' _computing_cell_refinement 'IPDS software package (Stoe, 2002)' _computing_data_reduction 'X-Area (Stoe, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 3.1' _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^)+(0.0514P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary none _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0027(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 601 _refine_ls_number_parameters 26 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0839 _refine_ls_R_factor_gt 0.0538 _refine_ls_wR_factor_ref 0.1207 _refine_ls_wR_factor_gt 0.1023 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _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 0.3333 0.6667 0.06246(5) 0.0175(3) Uani 1 6 d S . . Te2 Te 0.0000 0.0000 0.19164(5) 0.0180(4) Uani 1 6 d S . . Sb1 Sb 0.0000 0.0000 0.0000 0.0262(5) Uani 1 12 d S . . Sb2 Sb 0.6667 0.3333 0.13472(6) 0.0310(7) Uani 0.88(9) 6 d SP . . Ag2 Ag 0.6667 0.3333 0.13472(6) 0.0310(7) Uani 0.12(9) 6 d SP . . Sb3 Sb 0.3333 0.6667 0.27267(5) 0.0174(4) Uani 1 6 d S . . Sb4 Sb 0.6667 0.3333 0.32588(5) 0.0186(4) Uani 1 6 d S . . Sb5 Sb 0.0000 0.0000 0.40724(4) 0.0170(4) Uani 1 6 d S . . Sb6 Sb 0.3333 0.6667 0.46023(4) 0.0129(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 Te1 0.0155(4) 0.0155(4) 0.0215(5) 0.000 0.000 0.0077(2) Te2 0.0156(5) 0.0156(5) 0.0227(6) 0.000 0.000 0.0078(2) Sb1 0.0259(7) 0.0259(7) 0.0267(9) 0.000 0.000 0.0130(3) Sb2 0.0213(7) 0.0213(7) 0.0502(12) 0.000 0.000 0.0107(4) Ag2 0.0213(7) 0.0213(7) 0.0502(12) 0.000 0.000 0.0107(4) Sb3 0.0137(4) 0.0137(4) 0.0247(6) 0.000 0.000 0.0068(2) Sb4 0.0141(5) 0.0141(5) 0.0278(7) 0.000 0.000 0.0070(2) Sb5 0.0155(4) 0.0155(4) 0.0200(6) 0.000 0.000 0.0077(2) Sb6 0.0113(4) 0.0113(4) 0.0160(6) 0.000 0.000 0.0056(2) _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 Sb1 3.0514(10) . ? Te1 Sb1 3.0514(10) 1_565 ? Te1 Sb1 3.0514(10) 1_665 ? Te1 Ag2 3.2238(15) 1_565 ? Te1 Sb2 3.2238(15) 1_565 ? Te1 Ag2 3.2238(15) 1_455 ? Te1 Sb2 3.2238(15) 1_455 ? Te1 Sb2 3.2238(15) . ? Te2 Ag2 2.9612(13) 1_455 ? Te2 Ag2 2.9612(13) 1_445 ? Te2 Sb2 2.9612(13) 1_455 ? Te2 Sb2 2.9612(13) 1_445 ? Te2 Sb2 2.9612(13) . ? Sb1 Te1 3.0514(10) 7 ? Sb1 Te1 3.0514(10) 7_565 ? Sb1 Te1 3.0514(10) 1_545 ? Sb1 Te1 3.0514(10) 7_665 ? Sb1 Te1 3.0514(10) 1_445 ? Sb2 Te2 2.9612(13) 1_665 ? Sb2 Te2 2.9612(13) 1_655 ? Sb2 Te1 3.2238(15) 1_545 ? Sb2 Te1 3.2238(15) 1_655 ? Sb3 Sb4 2.9041(11) 1_565 ? Sb3 Sb4 2.9041(11) 1_455 ? Sb3 Sb4 2.9041(11) . ? Sb4 Sb3 2.9041(11) 1_545 ? Sb4 Sb3 2.9041(11) 1_655 ? Sb5 Sb6 2.9007(9) 1_545 ? Sb5 Sb6 2.9007(9) . ? Sb5 Sb6 2.9007(9) 1_445 ? Sb6 Sb5 2.9007(9) 1_565 ? Sb6 Sb5 2.9007(9) 1_665 ? 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 Sb1 Te1 Sb1 89.12(3) . 1_565 ? Sb1 Te1 Sb1 89.12(3) . 1_665 ? Sb1 Te1 Sb1 89.12(3) 1_565 1_665 ? Sb1 Te1 Ag2 175.96(5) . 1_565 ? Sb1 Te1 Ag2 93.76(2) 1_565 1_565 ? Sb1 Te1 Ag2 93.76(2) 1_665 1_565 ? Sb1 Te1 Sb2 175.96(5) . 1_565 ? Sb1 Te1 Sb2 93.76(2) 1_565 1_565 ? Sb1 Te1 Sb2 93.76(2) 1_665 1_565 ? Sb1 Te1 Ag2 93.76(2) . 1_455 ? Sb1 Te1 Ag2 93.76(2) 1_565 1_455 ? Sb1 Te1 Ag2 175.96(5) 1_665 1_455 ? Ag2 Te1 Ag2 83.23(5) 1_565 1_455 ? Sb2 Te1 Ag2 83.23(5) 1_565 1_455 ? Sb1 Te1 Sb2 93.76(2) . 1_455 ? Sb1 Te1 Sb2 93.76(2) 1_565 1_455 ? Sb1 Te1 Sb2 175.96(5) 1_665 1_455 ? Ag2 Te1 Sb2 83.23(5) 1_565 1_455 ? Sb2 Te1 Sb2 83.23(5) 1_565 1_455 ? Sb1 Te1 Sb2 93.76(2) . . ? Sb1 Te1 Sb2 175.96(5) 1_565 . ? Sb1 Te1 Sb2 93.76(2) 1_665 . ? Ag2 Te1 Sb2 83.23(5) 1_565 . ? Sb2 Te1 Sb2 83.23(5) 1_565 . ? Ag2 Te1 Sb2 83.23(5) 1_455 . ? Sb2 Te1 Sb2 83.23(5) 1_455 . ? Ag2 Te2 Ag2 92.61(5) 1_455 1_445 ? Ag2 Te2 Sb2 92.61(5) 1_445 1_455 ? Ag2 Te2 Sb2 92.61(5) 1_455 1_445 ? Sb2 Te2 Sb2 92.61(5) 1_455 1_445 ? Ag2 Te2 Sb2 92.61(5) 1_455 . ? Ag2 Te2 Sb2 92.61(5) 1_445 . ? Sb2 Te2 Sb2 92.61(5) 1_455 . ? Sb2 Te2 Sb2 92.61(5) 1_445 . ? Te1 Sb1 Te1 180.00(4) 7 . ? Te1 Sb1 Te1 89.12(3) 7 7_565 ? Te1 Sb1 Te1 90.88(3) . 7_565 ? Te1 Sb1 Te1 90.88(3) 7 1_545 ? Te1 Sb1 Te1 89.12(3) . 1_545 ? Te1 Sb1 Te1 180.00(4) 7_565 1_545 ? Te1 Sb1 Te1 89.12(3) 7 7_665 ? Te1 Sb1 Te1 90.88(3) . 7_665 ? Te1 Sb1 Te1 89.12(3) 7_565 7_665 ? Te1 Sb1 Te1 90.88(3) 1_545 7_665 ? Te1 Sb1 Te1 90.88(3) 7 1_445 ? Te1 Sb1 Te1 89.12(3) . 1_445 ? Te1 Sb1 Te1 90.88(3) 7_565 1_445 ? Te1 Sb1 Te1 89.12(3) 1_545 1_445 ? Te1 Sb1 Te1 180.00(4) 7_665 1_445 ? Te2 Sb2 Te2 92.61(5) 1_665 1_655 ? Te2 Sb2 Te2 92.61(5) 1_665 . ? Te2 Sb2 Te2 92.61(5) 1_655 . ? Te2 Sb2 Te1 173.47(6) 1_665 1_545 ? Te2 Sb2 Te1 91.90(2) 1_655 1_545 ? Te2 Sb2 Te1 91.90(2) . 1_545 ? Te2 Sb2 Te1 91.90(2) 1_665 1_655 ? Te2 Sb2 Te1 91.90(2) 1_655 1_655 ? Te2 Sb2 Te1 173.47(6) . 1_655 ? Te1 Sb2 Te1 83.23(5) 1_545 1_655 ? Te2 Sb2 Te1 91.90(2) 1_665 . ? Te2 Sb2 Te1 173.47(6) 1_655 . ? Te2 Sb2 Te1 91.90(2) . . ? Te1 Sb2 Te1 83.23(5) 1_545 . ? Te1 Sb2 Te1 83.23(5) 1_655 . ? Sb4 Sb3 Sb4 94.99(5) 1_565 1_455 ? Sb4 Sb3 Sb4 94.99(5) 1_565 . ? Sb4 Sb3 Sb4 94.99(5) 1_455 . ? Sb3 Sb4 Sb3 94.99(5) 1_545 1_655 ? Sb3 Sb4 Sb3 94.99(5) 1_545 . ? Sb3 Sb4 Sb3 94.99(5) 1_655 . ? Sb6 Sb5 Sb6 95.14(4) 1_545 . ? Sb6 Sb5 Sb6 95.14(4) 1_545 1_445 ? Sb6 Sb5 Sb6 95.14(4) . 1_445 ? Sb5 Sb6 Sb5 95.14(4) 1_565 . ? Sb5 Sb6 Sb5 95.14(4) 1_565 1_665 ? Sb5 Sb6 Sb5 95.14(4) . 1_665 ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 29.90 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.094 _refine_diff_density_min -1.465 _refine_diff_density_rms 0.325 # CRYSTAL DATA data_018_m _audit_creation_method SHELXL-97 _chemical_name_systematic ; germanium antimony telluride ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Ge4.71 Sb31.29 Te15' _chemical_formula_weight 6065.95 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Ge' 'Ge' 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 4.2580(10) _cell_length_b 4.2580(10) _cell_length_c 97.23(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1526.7(6) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 758 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 27.0 _exptl_crystal_description block _exptl_crystal_colour metallic_dark_grey _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 6.598 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2526.5 _exptl_absorpt_coefficient_mu 22.880 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.118 _exptl_absorpt_correction_T_max 0.319 _exptl_absorpt_process_details 'from equivalents, scaled' _exptl_special_details ; ? ; _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 3700 _diffrn_reflns_av_R_equivalents 0.0690 _diffrn_reflns_av_sigmaI/netI 0.0288 _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 -120 _diffrn_reflns_limit_l_max 120 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 26.76 _reflns_number_total 513 _reflns_number_gt 385 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS software package (Stoe, 2002)' _computing_cell_refinement 'IPDS software package (Stoe, 2002)' _computing_data_reduction 'X-Area (Stoe, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 3.1' _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^)+(0.0469P)^2^+17.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 513 _refine_ls_number_parameters 29 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0570 _refine_ls_R_factor_gt 0.0438 _refine_ls_wR_factor_ref 0.1100 _refine_ls_wR_factor_gt 0.1037 _refine_ls_goodness_of_fit_ref 1.286 _refine_ls_restrained_S_all 1.286 _refine_ls_shift/su_max 0.002 _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 0.0144(4) Uani 1 12 d S . . Sb1 Sb 0.0000 0.0000 0.351797(17) 0.0263(7) Uani 0.443(19) 6 d SP . . Ge1 Ge 0.0000 0.0000 0.351797(17) 0.0263(7) Uani 0.557(19) 6 d SP . . Te2 Te 0.0000 0.0000 0.702715(13) 0.0179(4) Uani 1 6 d S . . Sb2 Sb 0.0000 0.0000 0.058591(17) 0.0264(6) Uani 0.772(19) 6 d SP . . Ge2 Ge 0.0000 0.0000 0.058591(17) 0.0264(6) Uani 0.228(19) 6 d SP . . Te3 Te 0.0000 0.0000 0.407901(16) 0.0227(4) Uani 1 6 d S . . Sb3 Sb 0.0000 0.0000 0.765985(12) 0.0184(4) Uani 1 6 d S . . Sb4 Sb 0.0000 0.0000 0.115051(13) 0.0184(4) Uani 1 6 d S . . Sb5 Sb 0.0000 0.0000 0.472209(10) 0.0147(4) Uani 1 6 d S . . Sb6 Sb 0.0000 0.0000 0.821361(10) 0.0121(4) 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 Te1 0.0153(6) 0.0153(6) 0.0126(7) 0.000 0.000 0.0076(3) Sb1 0.0254(8) 0.0254(8) 0.0282(10) 0.000 0.000 0.0127(4) Ge1 0.0254(8) 0.0254(8) 0.0282(10) 0.000 0.000 0.0127(4) Te2 0.0165(5) 0.0165(5) 0.0206(6) 0.000 0.000 0.0083(2) Sb2 0.0184(7) 0.0184(7) 0.0423(11) 0.000 0.000 0.0092(4) Ge2 0.0184(7) 0.0184(7) 0.0423(11) 0.000 0.000 0.0092(4) Te3 0.0153(5) 0.0153(5) 0.0375(8) 0.000 0.000 0.0077(2) Sb3 0.0143(5) 0.0143(5) 0.0265(7) 0.000 0.000 0.0072(2) Sb4 0.0152(5) 0.0152(5) 0.0249(7) 0.000 0.000 0.0076(2) Sb5 0.0138(5) 0.0138(5) 0.0166(7) 0.000 0.000 0.0069(2) Sb6 0.0110(5) 0.0110(5) 0.0144(6) 0.000 0.000 0.0055(2) _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 Ge1 3.0439(11) 25_445 ? Te1 Ge1 3.0439(11) 13_554 ? Te1 Sb1 3.0439(11) 25_445 ? Te1 Sb1 3.0439(11) 13_554 ? Te1 Ge1 3.0439(11) 25 ? Te1 Sb1 3.0439(11) 13_444 ? Te1 Sb1 3.0439(11) 25 ? Te1 Ge1 3.0439(11) 13_444 ? Te1 Sb1 3.0439(11) 25_455 ? Te1 Sb1 3.0439(11) 13_544 ? Te1 Ge1 3.0439(11) 13_544 ? Te1 Ge1 3.0439(11) 25_455 ? Sb1 Te2 2.9943(14) 13_554 ? Sb1 Te2 2.9943(14) 13_444 ? Sb1 Te2 2.9943(14) 13_544 ? Sb1 Te1 3.0439(11) 7_445 ? Sb1 Te1 3.0439(11) 7 ? Sb1 Te1 3.0439(11) 7_455 ? Te2 Ge1 2.9943(14) 7_445 ? Te2 Sb1 2.9943(14) 7_445 ? Te2 Ge1 2.9943(14) 7 ? Te2 Sb1 2.9943(14) 7 ? Te2 Sb1 2.9943(14) 7_455 ? Te2 Ge1 2.9943(14) 7_455 ? Sb2 Te3 2.9079(13) 13_554 ? Sb2 Te3 2.9079(13) 13_444 ? Sb2 Te3 2.9079(13) 13_544 ? Te3 Ge2 2.9079(13) 7_445 ? Te3 Sb2 2.9079(13) 7_445 ? Te3 Ge2 2.9079(13) 7 ? Te3 Sb2 2.9079(13) 7 ? Te3 Sb2 2.9079(13) 7_455 ? Te3 Ge2 2.9079(13) 7_455 ? Sb3 Sb4 2.8953(11) 13 ? Sb3 Sb4 2.8953(11) 13_445 ? Sb3 Sb4 2.8953(11) 13_545 ? Sb4 Sb3 2.8953(11) 7_444 ? Sb4 Sb3 2.8953(11) 7_554 ? Sb4 Sb3 2.8953(11) 7_454 ? Sb5 Sb6 2.8997(10) 13_554 ? Sb5 Sb6 2.8997(10) 13_444 ? Sb5 Sb6 2.8997(10) 13_544 ? Sb6 Sb5 2.8997(10) 7_445 ? Sb6 Sb5 2.8997(10) 7 ? Sb6 Sb5 2.8997(10) 7_455 ? 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 Ge1 Te1 Ge1 180.00(5) 25_445 13_554 ? Ge1 Te1 Sb1 180.00(5) 13_554 25_445 ? Ge1 Te1 Sb1 180.00(5) 25_445 13_554 ? Sb1 Te1 Sb1 180.00(5) 25_445 13_554 ? Ge1 Te1 Ge1 88.76(4) 25_445 25 ? Ge1 Te1 Ge1 91.24(4) 13_554 25 ? Sb1 Te1 Ge1 88.76(4) 25_445 25 ? Sb1 Te1 Ge1 91.24(4) 13_554 25 ? Ge1 Te1 Sb1 91.24(4) 25_445 13_444 ? Ge1 Te1 Sb1 88.76(4) 13_554 13_444 ? Sb1 Te1 Sb1 91.24(4) 25_445 13_444 ? Sb1 Te1 Sb1 88.76(4) 13_554 13_444 ? Ge1 Te1 Sb1 180.00(5) 25 13_444 ? Ge1 Te1 Sb1 88.76(4) 25_445 25 ? Ge1 Te1 Sb1 91.24(4) 13_554 25 ? Sb1 Te1 Sb1 88.76(4) 25_445 25 ? Sb1 Te1 Sb1 91.24(4) 13_554 25 ? Sb1 Te1 Sb1 180.00(5) 13_444 25 ? Ge1 Te1 Ge1 91.24(4) 25_445 13_444 ? Ge1 Te1 Ge1 88.76(4) 13_554 13_444 ? Sb1 Te1 Ge1 91.24(4) 25_445 13_444 ? Sb1 Te1 Ge1 88.76(4) 13_554 13_444 ? Ge1 Te1 Ge1 180.00(5) 25 13_444 ? Sb1 Te1 Ge1 180.00(5) 25 13_444 ? Ge1 Te1 Sb1 88.76(4) 25_445 25_455 ? Ge1 Te1 Sb1 91.24(4) 13_554 25_455 ? Sb1 Te1 Sb1 88.76(4) 25_445 25_455 ? Sb1 Te1 Sb1 91.24(4) 13_554 25_455 ? Ge1 Te1 Sb1 88.76(4) 25 25_455 ? Sb1 Te1 Sb1 91.24(4) 13_444 25_455 ? Sb1 Te1 Sb1 88.76(4) 25 25_455 ? Ge1 Te1 Sb1 91.24(4) 13_444 25_455 ? Ge1 Te1 Sb1 91.24(4) 25_445 13_544 ? Ge1 Te1 Sb1 88.76(4) 13_554 13_544 ? Sb1 Te1 Sb1 91.24(4) 25_445 13_544 ? Sb1 Te1 Sb1 88.76(4) 13_554 13_544 ? Ge1 Te1 Sb1 91.24(4) 25 13_544 ? Sb1 Te1 Sb1 88.76(4) 13_444 13_544 ? Sb1 Te1 Sb1 91.24(4) 25 13_544 ? Ge1 Te1 Sb1 88.76(4) 13_444 13_544 ? Sb1 Te1 Sb1 180.00(5) 25_455 13_544 ? Ge1 Te1 Ge1 91.24(4) 25_445 13_544 ? Ge1 Te1 Ge1 88.76(4) 13_554 13_544 ? Sb1 Te1 Ge1 91.24(4) 25_445 13_544 ? Sb1 Te1 Ge1 88.76(4) 13_554 13_544 ? Ge1 Te1 Ge1 91.24(4) 25 13_544 ? Sb1 Te1 Ge1 88.76(4) 13_444 13_544 ? Sb1 Te1 Ge1 91.24(4) 25 13_544 ? Ge1 Te1 Ge1 88.76(4) 13_444 13_544 ? Sb1 Te1 Ge1 180.00(5) 25_455 13_544 ? Ge1 Te1 Ge1 88.76(4) 25_445 25_455 ? Ge1 Te1 Ge1 91.24(4) 13_554 25_455 ? Sb1 Te1 Ge1 88.76(4) 25_445 25_455 ? Sb1 Te1 Ge1 91.24(4) 13_554 25_455 ? Ge1 Te1 Ge1 88.76(4) 25 25_455 ? Sb1 Te1 Ge1 91.24(4) 13_444 25_455 ? Sb1 Te1 Ge1 88.76(4) 25 25_455 ? Ge1 Te1 Ge1 91.24(4) 13_444 25_455 ? Sb1 Te1 Ge1 180.00(5) 13_544 25_455 ? Ge1 Te1 Ge1 180.00(5) 13_544 25_455 ? Te2 Sb1 Te2 90.64(5) 13_554 13_444 ? Te2 Sb1 Te2 90.63(5) 13_554 13_544 ? Te2 Sb1 Te2 90.63(5) 13_444 13_544 ? Te2 Sb1 Te1 178.68(6) 13_554 7_445 ? Te2 Sb1 Te1 90.31(1) 13_444 7_445 ? Te2 Sb1 Te1 90.31(1) 13_544 7_445 ? Te2 Sb1 Te1 90.31(1) 13_554 7 ? Te2 Sb1 Te1 178.68(6) 13_444 7 ? Te2 Sb1 Te1 90.31(1) 13_544 7 ? Te1 Sb1 Te1 88.76(4) 7_445 7 ? Te2 Sb1 Te1 90.31(1) 13_554 7_455 ? Te2 Sb1 Te1 90.31(1) 13_444 7_455 ? Te2 Sb1 Te1 178.68(6) 13_544 7_455 ? Te1 Sb1 Te1 88.76(4) 7_445 7_455 ? Te1 Sb1 Te1 88.76(4) 7 7_455 ? Ge1 Te2 Ge1 90.64(5) 7_445 7 ? Sb1 Te2 Ge1 90.64(5) 7_445 7 ? Ge1 Te2 Sb1 90.64(5) 7_445 7 ? Sb1 Te2 Sb1 90.64(5) 7_445 7 ? Ge1 Te2 Sb1 90.63(5) 7_445 7_455 ? Sb1 Te2 Sb1 90.63(5) 7_445 7_455 ? Ge1 Te2 Sb1 90.63(5) 7 7_455 ? Sb1 Te2 Sb1 90.63(5) 7 7_455 ? Ge1 Te2 Ge1 90.63(5) 7_445 7_455 ? Sb1 Te2 Ge1 90.63(5) 7_445 7_455 ? Ge1 Te2 Ge1 90.63(5) 7 7_455 ? Sb1 Te2 Ge1 90.63(5) 7 7_455 ? Te3 Sb2 Te3 94.13(5) 13_554 13_444 ? Te3 Sb2 Te3 94.13(5) 13_554 13_544 ? Te3 Sb2 Te3 94.13(5) 13_444 13_544 ? Ge2 Te3 Ge2 94.13(5) 7_445 7 ? Sb2 Te3 Ge2 94.13(5) 7_445 7 ? Ge2 Te3 Sb2 94.13(5) 7_445 7 ? Sb2 Te3 Sb2 94.13(5) 7_445 7 ? Ge2 Te3 Sb2 94.13(5) 7_445 7_455 ? Sb2 Te3 Sb2 94.13(5) 7_445 7_455 ? Ge2 Te3 Sb2 94.13(5) 7 7_455 ? Sb2 Te3 Sb2 94.13(5) 7 7_455 ? Ge2 Te3 Ge2 94.13(5) 7_445 7_455 ? Sb2 Te3 Ge2 94.13(5) 7_445 7_455 ? Ge2 Te3 Ge2 94.13(5) 7 7_455 ? Sb2 Te3 Ge2 94.13(5) 7 7_455 ? Sb4 Sb3 Sb4 94.67(4) 13 13_445 ? Sb4 Sb3 Sb4 94.67(4) 13 13_545 ? Sb4 Sb3 Sb4 94.67(4) 13_445 13_545 ? Sb3 Sb4 Sb3 94.67(4) 7_444 7_554 ? Sb3 Sb4 Sb3 94.67(4) 7_444 7_454 ? Sb3 Sb4 Sb3 94.67(4) 7_554 7_454 ? Sb6 Sb5 Sb6 94.48(4) 13_554 13_444 ? Sb6 Sb5 Sb6 94.48(4) 13_554 13_544 ? Sb6 Sb5 Sb6 94.48(4) 13_444 13_544 ? Sb5 Sb6 Sb5 94.48(4) 7_445 7 ? Sb5 Sb6 Sb5 94.48(4) 7_445 7_455 ? Sb5 Sb6 Sb5 94.48(4) 7 7_455 ? _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 26.76 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 2.764 _refine_diff_density_min -2.681 _refine_diff_density_rms 0.322