Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Kanatzidis, Mercouri' 'Hogan, Tim' 'Hsu, Kuei-Fang' 'Lal, Sangeeta' _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@CEM.MSU.EDU' _publ_section_title ; CsPb3Bi3Te8 and CsPb4Bi3Te9: Low-Dimensional Compounds and the Homologous Series CsPbmBi3Te5+m ; data_CsPb3Bi3Te8 _database_code_CSD 180732 _audit_creation_method SHELXL-97 _chemical_name_systematic ; cesium lead bismuth telluride (0.93/2.93/3.07/8) ; _chemical_formula_moiety 'Cs0.93 Pb2.93 Bi3.07 Te8' _chemical_formula_sum 'Bi3.07 Cs0.93 Pb2.93 Te8' _chemical_formula_weight 2393.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source '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' 'Pb' 'Pb' -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Bi' 'Bi' -4.1077 10.2566 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Cmcm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-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' '-x, -y, -z' 'x, y, -z-1/2' 'x, -y, z-1/2' '-x, y, z' '-x+1/2, -y+1/2, -z' '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' _cell_length_a 6.3736(8) _cell_length_b 37.731(5) _cell_length_c 4.4416(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1068.1(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 975 _cell_measurement_theta_min 3.24 _cell_measurement_theta_max 27.75 _exptl_crystal_description needle _exptl_crystal_colour black _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 15.765 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4084 _exptl_absorpt_coefficient_mu 124.459 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.2597 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ; The absorption correction was based on 1538 symmetry-equivalent 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 hemisphere of reciprocal space, by a combination of three 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 94.5% complete to at 28.15\% 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 ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3069 _diffrn_reflns_av_R_equivalents 0.0588 _diffrn_reflns_av_sigmaI/netI 0.0417 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -48 _diffrn_reflns_limit_k_max 45 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 28.15 _reflns_number_total 757 _reflns_number_gt 563 _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 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1000P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00021(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 757 _refine_ls_number_parameters 34 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0782 _refine_ls_R_factor_gt 0.0597 _refine_ls_wR_factor_ref 0.1696 _refine_ls_wR_factor_gt 0.1583 _refine_ls_goodness_of_fit_ref 1.131 _refine_ls_restrained_S_all 1.131 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.001 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 Bi1 Bi 0.5000 0.41005(3) 0.2500 0.0249(5) Uani 1 4 d S . . Bi2 Bi 0.0000 0.34622(4) 0.7500 0.0283(5) Uani 1 4 d S . . Bi3 Bi 0.5000 0.28139(3) 0.2500 0.0245(4) Uani 1 4 d S . . Te1 Te 0.5000 0.46260(7) -0.2500 0.0564(11) Uani 1 4 d S . . Te2 Te 0.0000 0.40296(7) 0.2500 0.0277(6) Uani 1 4 d S . . Te3 Te 0.5000 0.34168(5) 0.7500 0.0178(5) Uani 1 4 d S . . Te4 Te 0.0000 0.28040(5) 0.2500 0.0181(6) Uani 1 4 d S . . Cs1 Cs 0.0000 0.49777(14) -0.2500 0.0459(15) Uani 0.47 4 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 Bi1 0.0229(8) 0.0270(8) 0.0248(7) 0.000 0.000 0.000 Bi2 0.0152(7) 0.0429(9) 0.0269(8) 0.000 0.000 0.000 Bi3 0.0161(8) 0.0314(8) 0.0260(8) 0.000 0.000 0.000 Te1 0.124(3) 0.0219(12) 0.0234(14) 0.000 0.000 0.000 Te2 0.0106(12) 0.0466(15) 0.0259(13) 0.000 0.000 0.000 Te3 0.0108(11) 0.0208(11) 0.0217(11) 0.000 0.000 0.000 Te4 0.0094(12) 0.0224(11) 0.0225(12) 0.000 0.000 0.000 Cs1 0.024(3) 0.031(3) 0.082(4) 0.000 0.000 0.000 _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 Bi1 Te1 2.977(2) 1_556 yes Bi1 Te1 2.977(2) . yes Bi1 Te2 3.1980(5) . yes Bi1 Te2 3.1980(5) 1_655 yes Bi1 Te3 3.4038(18) . yes Bi1 Te3 3.4038(18) 1_554 yes Bi1 Cs1 4.717(4) 9_665 no Bi1 Cs1 4.717(4) 9_565 no Bi2 Te2 3.084(2) 1_556 yes Bi2 Te2 3.084(2) . yes Bi2 Te3 3.1914(4) 1_455 yes Bi2 Te3 3.1914(4) . yes Bi2 Te4 3.3318(17) . yes Bi2 Te4 3.3318(17) 1_556 yes Bi3 Te3 3.1790(15) 1_554 yes Bi3 Te3 3.1790(15) . yes Bi3 Te4 3.1870(4) 1_655 yes Bi3 Te4 3.1870(4) . yes Bi3 Te4 3.2199(16) 13 yes Bi3 Te4 3.2199(16) 13_556 yes Te1 Bi1 2.977(2) 1_554 no Te1 Cs1 3.452(2) 1_655 yes Te1 Cs1 3.452(2) . yes Te1 Cs1 4.162(2) 9_665 yes Te1 Cs1 4.162(2) 9_564 yes Te1 Cs1 4.162(2) 9_664 yes Te1 Cs1 4.162(2) 9_565 yes Te2 Bi2 3.084(2) 1_554 no Te2 Bi1 3.1980(5) 1_455 no Te2 Cs1 3.746(6) 9_565 yes Te2 Cs1 4.211(5) 1_556 yes Te2 Cs1 4.211(5) . yes Te3 Bi3 3.1790(15) 1_556 no Te3 Bi2 3.1914(4) 1_655 no Te3 Bi1 3.4038(18) 1_556 no Te4 Bi3 3.1870(4) 1_455 no Te4 Bi3 3.2199(16) 13 no Te4 Bi3 3.2199(16) 13_556 no Te4 Bi2 3.3318(17) 1_554 no Cs1 Cs1 2.2272(9) 9_565 no Cs1 Cs1 2.2272(9) 9_564 no Cs1 Te1 3.452(2) 1_455 no Cs1 Te2 3.746(6) 9_565 no Cs1 Te1 4.162(2) 9_665 no Cs1 Te1 4.162(2) 9_564 no Cs1 Te1 4.162(2) 9_664 no Cs1 Te1 4.162(2) 9_565 no Cs1 Te2 4.211(5) 1_554 no Cs1 Cs1 4.4416(6) 1_556 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 Bi1 Te1 96.48(9) 1_556 . yes Te1 Bi1 Te2 93.19(4) 1_556 . yes Te1 Bi1 Te2 93.19(4) . . yes Te1 Bi1 Te2 93.19(4) 1_556 1_655 yes Te1 Bi1 Te2 93.19(4) . 1_655 yes Te2 Bi1 Te2 170.40(11) . 1_655 yes Te1 Bi1 Te3 91.03(4) 1_556 . yes Te1 Bi1 Te3 172.49(6) . . yes Te2 Bi1 Te3 86.36(4) . . yes Te2 Bi1 Te3 86.36(4) 1_655 . yes Te1 Bi1 Te3 172.49(6) 1_556 1_554 yes Te1 Bi1 Te3 91.03(4) . 1_554 yes Te2 Bi1 Te3 86.36(4) . 1_554 yes Te2 Bi1 Te3 86.36(4) 1_655 1_554 yes Te3 Bi1 Te3 81.45(5) . 1_554 yes Te2 Bi2 Te2 92.11(8) 1_556 . yes Te2 Bi2 Te3 92.14(3) 1_556 1_455 yes Te2 Bi2 Te3 92.14(3) . 1_455 yes Te2 Bi2 Te3 92.14(3) 1_556 . yes Te2 Bi2 Te3 92.14(3) . . yes Te3 Bi2 Te3 173.84(9) 1_455 . yes Te2 Bi2 Te4 175.75(5) 1_556 . yes Te2 Bi2 Te4 92.14(4) . . yes Te3 Bi2 Te4 87.71(3) 1_455 . yes Te3 Bi2 Te4 87.71(3) . . yes Te2 Bi2 Te4 92.14(4) 1_556 1_556 yes Te2 Bi2 Te4 175.75(5) . 1_556 ? Te3 Bi2 Te4 87.71(3) 1_455 1_556 yes Te3 Bi2 Te4 87.71(3) . 1_556 yes Te4 Bi2 Te4 83.60(5) . 1_556 yes Te3 Bi3 Te3 88.63(5) 1_554 . yes Te3 Bi3 Te4 90.48(3) 1_554 1_655 yes Te3 Bi3 Te4 90.48(3) . 1_655 yes Te3 Bi3 Te4 90.48(3) 1_554 . yes Te3 Bi3 Te4 90.48(3) . . yes Te4 Bi3 Te4 178.65(8) 1_655 . yes Te3 Bi3 Te4 92.08(4) 1_554 13 yes Te3 Bi3 Te4 179.29(4) . 13 yes Te4 Bi3 Te4 89.51(3) 1_655 13 yes Te4 Bi3 Te4 89.51(3) . 13 yes Te3 Bi3 Te4 179.29(4) 1_554 13_556 yes Te3 Bi3 Te4 92.08(4) . 13_556 yes Te4 Bi3 Te4 89.51(3) 1_655 13_556 yes Te4 Bi3 Te4 89.51(3) . 13_556 yes Te4 Bi3 Te4 87.22(5) 13 13_556 yes Te1 Cs1 Te1 134.78(18) 1_455 . no Te1 Cs1 Te2 112.61(9) 1_455 9_565 no Te1 Cs1 Te2 112.61(9) . 9_565 no Te1 Cs1 Te1 147.665(12) 1_455 9_665 no Te1 Cs1 Te1 55.34(6) . 9_665 no Te2 Cs1 Te1 68.95(8) 9_565 9_665 no Te1 Cs1 Te1 55.34(6) 1_455 9_564 no Te1 Cs1 Te1 147.665(12) . 9_564 no Te2 Cs1 Te1 68.95(8) 9_565 9_564 no Te1 Cs1 Te1 137.89(16) 9_665 9_564 no Te1 Cs1 Te1 147.665(12) 1_455 9_664 no Te1 Cs1 Te1 55.34(6) . 9_664 no Te2 Cs1 Te1 68.95(8) 9_565 9_664 no Te1 Cs1 Te1 64.49(4) 9_665 9_664 no Te1 Cs1 Te1 99.93(7) 9_564 9_664 no Te1 Cs1 Te1 55.34(6) 1_455 9_565 no Te1 Cs1 Te1 147.665(12) . 9_565 no Te2 Cs1 Te1 68.95(8) 9_565 9_565 no Te1 Cs1 Te1 99.93(7) 9_665 9_565 no Te1 Cs1 Te1 64.49(4) 9_564 9_565 no Te1 Cs1 Te1 137.89(16) 9_664 9_565 no Te1 Cs1 Te2 70.94(8) 1_455 1_554 no Te1 Cs1 Te2 70.94(8) . 1_554 no Te2 Cs1 Te2 148.17(4) 9_565 1_554 no Te1 Cs1 Te2 125.92(8) 9_665 1_554 no Te1 Cs1 Te2 91.36(5) 9_564 1_554 no Te1 Cs1 Te2 91.36(5) 9_664 1_554 no Te1 Cs1 Te2 125.92(8) 9_565 1_554 no Te1 Cs1 Te2 70.94(8) 1_455 . no Te1 Cs1 Te2 70.94(8) . . no Te2 Cs1 Te2 148.17(4) 9_565 . no Te1 Cs1 Te2 91.36(5) 9_665 . no Te1 Cs1 Te2 125.92(8) 9_564 . no Te1 Cs1 Te2 125.92(8) 9_664 . no Te1 Cs1 Te2 91.36(5) 9_565 . no Te2 Cs1 Te2 63.66(9) 1_554 . no _diffrn_measured_fraction_theta_max 0.945 _diffrn_reflns_theta_full 28.15 _diffrn_measured_fraction_theta_full 0.945 _refine_diff_density_max 4.528 _refine_diff_density_min -6.556 _refine_diff_density_rms 0.904 #===========================================================END data_CsPb4Bi3Te9 _database_code_CSD 180733 _audit_creation_method SHELXL-97 _chemical_name_systematic ; cesium lead bismuth telluride (0.96/3.96/3.04/9) ; _chemical_name_common 'Cs0.96 Pb3.96 Bi3.04 Te9' _chemical_formula_moiety 'Bi3.04 Cs0.96 Pb3.96 Te9' _chemical_formula_sum ? _chemical_formula_weight 2731.80 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source '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' 'Pb' 'Pb' -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Bi' 'Bi' -4.1077 10.2566 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Cmcm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-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' '-x, -y, -z' 'x, y, -z-1/2' 'x, -y, z-1/2' '-x, y, z' '-x+1/2, -y+1/2, -z' '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' _cell_length_a 4.4524(6) _cell_length_b 42.133(6) _cell_length_c 12.7419(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2390.3(6) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 689 _cell_measurement_theta_min 3.20 _cell_measurement_theta_max 28.61 _exptl_crystal_description needle _exptl_crystal_colour black _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 15.231 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8816 _exptl_absorpt_coefficient_mu 125.916 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.3069 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ; The absorption correction was based on 2556 symmetry-equivalent 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 hemisphere of reciprocal space, by a combination of three 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 92.8% complete to at 29.01\% 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 ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7600 _diffrn_reflns_av_R_equivalents 0.0750 _diffrn_reflns_av_sigmaI/netI 0.0496 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -46 _diffrn_reflns_limit_k_max 54 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 29.01 _reflns_number_total 1727 _reflns_number_gt 1059 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0625P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.000018(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1727 _refine_ls_number_parameters 62 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0925 _refine_ls_R_factor_gt 0.0489 _refine_ls_wR_factor_ref 0.1250 _refine_ls_wR_factor_gt 0.1069 _refine_ls_goodness_of_fit_ref 0.945 _refine_ls_restrained_S_all 0.945 _refine_ls_shift/su_max 0.001 _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 Bi1 Bi 0.0000 0.32990(2) 0.50316(6) 0.0244(2) Uani 1 2 d S . . Bi2 Bi 0.5000 0.38399(3) 0.2500 0.0253(3) Uani 1 4 d S . . Bi3 Bi 0.5000 0.38956(3) 0.7500 0.0259(3) Uani 1 4 d S . . Bi4 Bi 0.0000 0.443910(19) 0.49958(6) 0.0250(2) Uani 1 2 d S . . Bi5 Bi 0.5000 0.49795(3) 0.2500 0.0253(3) Uani 1 4 d S . . Cs1 Cs 0.5000 0.25208(5) 0.2500 0.0333(5) Uani 0.96 4 d SP . . Te1 Te 0.5000 0.28342(3) 0.52226(11) 0.0229(3) Uani 1 2 d S . . Te2 Te 0.0000 0.33245(5) 0.2500 0.0234(5) Uani 1 4 d S . . Te3 Te 0.0000 0.33996(5) 0.7500 0.0216(4) Uani 1 4 d S . . Te4 Te 0.5000 0.39086(3) 0.50085(9) 0.0176(3) Uani 1 2 d S . . Te5 Te 0.0000 0.44384(4) 0.2500 0.0176(4) Uani 1 4 d S . . Te6 Te 0.0000 0.44732(4) 0.7500 0.0174(4) Uani 1 4 d S . . Te7 Te 0.5000 0.5000 0.5000 0.0174(4) Uani 1 4 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 Bi1 0.0208(5) 0.0199(5) 0.0324(5) -0.0001(3) 0.000 0.000 Bi2 0.0237(7) 0.0285(7) 0.0238(6) 0.000 0.000 0.000 Bi3 0.0258(7) 0.0271(7) 0.0249(6) 0.000 0.000 0.000 Bi4 0.0256(5) 0.0243(5) 0.0249(5) 0.0009(3) 0.000 0.000 Bi5 0.0265(7) 0.0250(7) 0.0245(6) 0.000 0.000 0.000 Cs1 0.0442(13) 0.0300(13) 0.0258(11) 0.000 0.000 0.000 Te1 0.0197(7) 0.0171(7) 0.0317(7) 0.0001(5) 0.000 0.000 Te2 0.0229(12) 0.0233(12) 0.0239(10) 0.000 0.000 0.000 Te3 0.0248(12) 0.0188(10) 0.0212(10) 0.000 0.000 0.000 Te4 0.0185(7) 0.0155(7) 0.0190(7) 0.0002(5) 0.000 0.000 Te5 0.0189(11) 0.0163(10) 0.0177(9) 0.000 0.000 0.000 Te6 0.0195(11) 0.0143(9) 0.0184(9) 0.000 0.000 0.000 Te7 0.0188(10) 0.0159(10) 0.0175(10) 0.0002(7) 0.000 0.000 _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 Bi1 Te1 2.9750(12) 1_455 yes Bi1 Te1 2.9750(12) . yes Bi1 Te3 3.1737(9) . yes Bi1 Te2 3.2275(9) . yes Bi1 Te4 3.3992(12) . yes Bi1 Te4 3.3992(12) 1_455 yes Bi1 Cs1 4.6716(18) 13_556 no Bi2 Te2 3.1099(16) . yes Bi2 Te2 3.1099(16) 1_655 yes Bi2 Te4 3.2095(12) . yes Bi2 Te4 3.2095(12) 10_556 yes Bi2 Te5 3.3639(16) . yes Bi2 Te5 3.3639(16) 1_655 yes Bi3 Te3 3.0534(16) . yes Bi3 Te3 3.0534(16) 1_655 yes Bi3 Te4 3.1751(12) 10_557 yes Bi3 Te4 3.1751(12) . yes Bi3 Te6 3.2981(16) . yes Bi3 Te6 3.2981(16) 1_655 yes Bi4 Te4 3.1546(11) 1_455 yes Bi4 Te4 3.1546(11) . yes Bi4 Te5 3.1801(8) . yes Bi4 Te6 3.1941(8) . yes Bi4 Te7 3.2467(7) . yes Bi4 Te7 3.2467(7) 1_455 yes Bi5 Te5 3.1864(15) 1_655 yes Bi5 Te5 3.1864(15) . yes Bi5 Te7 3.1866(5) . yes Bi5 Te7 3.1866(5) 2_664 yes Bi5 Te6 3.2053(16) 9_666 yes Bi5 Te6 3.2053(16) 9_566 yes Cs1 Te1 3.7118(17) . yes Cs1 Te1 3.7118(17) 10_556 yes Cs1 Te3 3.878(3) 13_556 yes Cs1 Te1 3.9515(15) 6_554 yes Cs1 Te1 3.9515(15) 13_656 yes Cs1 Te1 3.9515(15) 6_654 yes Cs1 Te1 3.9515(15) 13_556 yes Cs1 Te2 4.052(3) 1_655 yes Cs1 Te2 4.052(3) . yes 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 Bi1 Te1 96.89(5) 1_455 . yes Te1 Bi1 Te3 90.39(4) 1_455 . yes Te1 Bi1 Te3 90.39(4) . . yes Te1 Bi1 Te2 95.95(4) 1_455 . yes Te1 Bi1 Te2 95.95(4) . . yes Te3 Bi1 Te2 170.42(6) . . yes Te1 Bi1 Te4 171.20(4) 1_455 . yes Te1 Bi1 Te4 90.46(3) . . yes Te3 Bi1 Te4 84.70(4) . . yes Te2 Bi1 Te4 88.07(4) . . yes Te1 Bi1 Te4 90.46(3) 1_455 1_455 yes Te1 Bi1 Te4 171.20(4) . 1_455 yes Te3 Bi1 Te4 84.70(4) . 1_455 yes Te2 Bi1 Te4 88.07(4) . 1_455 yes Te4 Bi1 Te4 81.83(4) . 1_455 yes Te2 Bi2 Te2 91.42(6) . 1_655 yes Te2 Bi2 Te4 93.61(2) . . yes Te2 Bi2 Te4 93.61(2) 1_655 . yes Te2 Bi2 Te4 93.61(2) . 10_556 yes Te2 Bi2 Te4 93.61(2) 1_655 10_556 yes Te4 Bi2 Te4 169.64(6) . 10_556 yes Te2 Bi2 Te5 92.85(3) . . yes Te2 Bi2 Te5 175.72(4) 1_655 . yes Te4 Bi2 Te5 86.12(2) . . yes Te4 Bi2 Te5 86.12(2) 10_556 . yes Te2 Bi2 Te5 175.72(4) . 1_655 yes Te2 Bi2 Te5 92.85(3) 1_655 1_655 yes Te4 Bi2 Te5 86.12(2) . 1_655 yes Te4 Bi2 Te5 86.12(2) 10_556 1_655 yes Te5 Bi2 Te5 82.87(5) . 1_655 yes Te3 Bi3 Te3 93.62(7) . 1_655 yes Te3 Bi3 Te4 90.68(2) . 10_557 yes Te3 Bi3 Te4 90.68(2) 1_655 10_557 yes Te3 Bi3 Te4 90.68(2) . . yes Te3 Bi3 Te4 90.68(2) 1_655 . yes Te4 Bi3 Te4 178.02(6) 10_557 . yes Te3 Bi3 Te6 90.74(3) . . yes Te3 Bi3 Te6 175.64(5) 1_655 . yes Te4 Bi3 Te6 89.27(2) 10_557 . yes Te4 Bi3 Te6 89.27(2) . . yes Te3 Bi3 Te6 175.64(5) . 1_655 yes Te3 Bi3 Te6 90.74(3) 1_655 1_655 yes Te4 Bi3 Te6 89.27(2) 10_557 1_655 yes Te4 Bi3 Te6 89.27(2) . 1_655 yes Te6 Bi3 Te6 84.91(5) . 1_655 yes Te4 Bi4 Te4 89.77(4) 1_455 . yes Te4 Bi4 Te5 90.26(3) 1_455 . yes Te4 Bi4 Te5 90.26(3) . . yes Te4 Bi4 Te6 91.53(4) 1_455 . yes Te4 Bi4 Te6 91.53(4) . . yes Te5 Bi4 Te6 177.48(5) . . yes Te4 Bi4 Te7 178.36(3) 1_455 . yes Te4 Bi4 Te7 91.82(2) . . yes Te5 Bi4 Te7 90.13(3) . . yes Te6 Bi4 Te7 88.03(3) . . yes Te4 Bi4 Te7 91.82(2) 1_455 1_455 yes Te4 Bi4 Te7 178.36(3) . 1_455 yes Te5 Bi4 Te7 90.13(3) . 1_455 yes Te6 Bi4 Te7 88.03(3) . 1_455 yes Te7 Bi4 Te7 86.58(2) . 1_455 yes Te5 Bi5 Te5 88.64(5) 1_655 . yes Te5 Bi5 Te7 91.111(15) 1_655 . yes Te5 Bi5 Te7 91.111(15) . . yes Te5 Bi5 Te7 91.111(15) 1_655 2_664 yes Te5 Bi5 Te7 91.111(15) . 2_664 yes Te7 Bi5 Te7 176.89(4) . 2_664 yes Te5 Bi5 Te6 91.69(3) 1_655 9_666 yes Te5 Bi5 Te6 179.67(4) . 9_666 yes Te7 Bi5 Te6 88.883(15) . 9_666 yes Te7 Bi5 Te6 88.883(15) 2_664 9_666 yes Te5 Bi5 Te6 179.67(4) 1_655 9_566 yes Te5 Bi5 Te6 91.69(3) . 9_566 yes Te7 Bi5 Te6 88.883(15) . 9_566 yes Te7 Bi5 Te6 88.883(15) 2_664 9_566 yes Te6 Bi5 Te6 87.98(6) 9_666 9_566 yes Te1 Cs1 Te1 138.33(7) . 10_556 no Te1 Cs1 Te3 110.84(4) . 13_556 no Te1 Cs1 Te3 110.84(4) 10_556 13_556 no Te1 Cs1 Te1 145.184(15) . 6_554 no Te1 Cs1 Te1 56.52(3) 10_556 6_554 no Te3 Cs1 Te1 67.76(4) 13_556 6_554 no Te1 Cs1 Te1 56.52(3) . 13_656 no Te1 Cs1 Te1 145.184(15) 10_556 13_656 no Te3 Cs1 Te1 67.76(4) 13_556 13_656 no Te1 Cs1 Te1 135.51(7) 6_554 13_656 no Te1 Cs1 Te1 145.184(15) . 6_654 no Te1 Cs1 Te1 56.52(3) 10_556 6_654 no Te3 Cs1 Te1 67.76(4) 13_556 6_654 no Te1 Cs1 Te1 68.58(3) 6_554 6_654 no Te1 Cs1 Te1 94.51(4) 13_656 6_654 no Te1 Cs1 Te1 56.52(3) . 13_556 no Te1 Cs1 Te1 145.184(15) 10_556 13_556 no Te3 Cs1 Te1 67.76(4) 13_556 13_556 no Te1 Cs1 Te1 94.51(4) 6_554 13_556 no Te1 Cs1 Te1 68.58(3) 13_656 13_556 no Te1 Cs1 Te1 135.51(7) 6_654 13_556 no Te1 Cs1 Te2 72.71(3) . 1_655 no Te1 Cs1 Te2 72.71(3) 10_556 1_655 no Te3 Cs1 Te2 146.68(2) 13_556 1_655 no Te1 Cs1 Te2 128.74(4) 6_554 1_655 no Te1 Cs1 Te2 90.39(3) 13_656 1_655 no Te1 Cs1 Te2 90.39(3) 6_654 1_655 no Te1 Cs1 Te2 128.74(4) 13_556 1_655 no Te1 Cs1 Te2 72.71(3) . . no Te1 Cs1 Te2 72.71(3) 10_556 . no Te3 Cs1 Te2 146.68(2) 13_556 . no Te1 Cs1 Te2 90.39(3) 6_554 . no Te1 Cs1 Te2 128.74(4) 13_656 . no Te1 Cs1 Te2 128.74(4) 6_654 . no Te1 Cs1 Te2 90.39(3) 13_556 . no Te2 Cs1 Te2 66.65(5) 1_655 . no _diffrn_measured_fraction_theta_max 0.928 _diffrn_reflns_theta_full 29.01 _diffrn_measured_fraction_theta_full 0.928 _refine_diff_density_max 3.514 _refine_diff_density_min -2.757 _refine_diff_density_rms 0.803