# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Mercouri Kanatzidis' _publ_contact_author_address ; Department of Chemistry Michigan State University 320 Chemistry Building East Lansing MI 48824 UNITED STATES OF AMERICA ; _publ_contact_author_email KANATZID@CEM.MSU.EDU _publ_section_title ; A New Homologous Series A2[M5+nSe9+n] (A = Rb, Cs; M = Bi, Ag, Cd) and its members ?-CsBi3Se5, Rb2CdBi6Se11, CsAg0.5Bi3.5Se6, CsCdBi3Se6, Rb2Ag1.5Bi7.5Se13, and Cs2Ag1.5Bi7.5Se13 ; loop_ _publ_author_name 'Mercouri Kanatzidis' 'Duck-Young Chung' 'Jun-Ho Kim' # Attachment 'CsBi3Se5.CIF' data_62a _database_code_depnum_ccdc_archive 'CCDC 291021' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common CsBi3Se5 _chemical_melting_point ? _chemical_formula_moiety CsBi3Se5 _chemical_formula_sum 'Bi3 Cs Se5' _chemical_formula_weight 1154.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Se Se -0.0929 2.2259 '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' 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 Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 22.740(13) _cell_length_b 4.171(2) _cell_length_c 12.472(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1183.0(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8168 _cell_measurement_theta_min 1.71 _cell_measurement_theta_max 27.98 _exptl_crystal_description needle _exptl_crystal_colour black _exptl_crystal_size_max 0.488 _exptl_crystal_size_mid 0.082 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 6.483 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1896 _exptl_absorpt_coefficient_mu 62.867 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.733003 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ; An analytical absorption correction was performed using face indexing and the program XPREP, followed by a semiempirical absorption correction based on symmetrically equivalent reflections with the program SADABS. ; _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 '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 8168 _diffrn_reflns_av_R_equivalents 0.0688 _diffrn_reflns_av_sigmaI/netI 0.0434 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 27.98 _reflns_number_total 1542 _reflns_number_gt 1206 _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^)+(0.0784P)^2^+187.3588P] 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_number_reflns 1542 _refine_ls_number_parameters 55 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0922 _refine_ls_R_factor_gt 0.0670 _refine_ls_wR_factor_ref 0.1965 _refine_ls_wR_factor_gt 0.1688 _refine_ls_goodness_of_fit_ref 1.188 _refine_ls_restrained_S_all 1.188 _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 Bi1 Bi 0.47624(7) 0.2500 0.86339(10) 0.0192(4) Uani 1 2 d S . . Bi2 Bi 0.42555(7) -0.2500 0.59380(10) 0.0183(4) Uani 1 2 d S . . Bi3 Bi 0.37630(7) -0.7500 0.30625(11) 0.0196(4) Uani 1 2 d S . . Cs1 Cs 0.28796(13) -1.7500 -0.0115(2) 0.0314(7) Uani 1 2 d S . . Se1 Se 0.34386(17) -0.7500 0.5286(3) 0.0178(8) Uani 1 2 d S . . Se2 Se 0.3011(2) -1.2500 0.2474(3) 0.0254(9) Uani 1 2 d S . . Se3 Se 0.38800(18) -0.2500 0.8058(3) 0.0199(8) Uani 1 2 d S . . Se4 Se 0.43671(17) 0.2500 1.0846(3) 0.0178(8) Uani 1 2 d S . . Se5 Se 0.51924(17) 0.2500 0.6390(3) 0.0153(8) Uani 1 2 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 0.0313(9) 0.0151(7) 0.0112(6) 0.000 0.0004(6) 0.000 Bi2 0.0286(8) 0.0129(7) 0.0133(6) 0.000 -0.0014(5) 0.000 Bi3 0.0261(8) 0.0173(7) 0.0155(7) 0.000 -0.0004(6) 0.000 Cs1 0.0287(15) 0.0309(15) 0.0346(14) 0.000 -0.0047(12) 0.000 Se1 0.023(2) 0.0154(18) 0.0149(16) 0.000 -0.0007(14) 0.000 Se2 0.029(2) 0.024(2) 0.0237(19) 0.000 -0.0023(17) 0.000 Se3 0.024(2) 0.0194(19) 0.0163(17) 0.000 0.0045(15) 0.000 Se4 0.024(2) 0.0171(19) 0.0122(16) 0.000 0.0017(14) 0.000 Se5 0.025(2) 0.0122(17) 0.0086(15) 0.000 -0.0009(13) 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 Se4 2.902(4) . ? Bi1 Se4 2.948(3) 5_667 ? Bi1 Se4 2.948(3) 5_657 ? Bi1 Se5 2.965(4) . ? Bi1 Se3 2.982(3) . ? Bi1 Se3 2.982(3) 1_565 ? Bi1 Cs1 4.557(4) 1_576 ? Bi2 Se3 2.779(4) . ? Bi2 Se1 2.909(3) . ? Bi2 Se1 2.909(3) 1_565 ? Bi2 Se5 3.034(3) . ? Bi2 Se5 3.034(3) 1_545 ? Bi2 Se5 3.163(4) 5_656 ? Bi3 Se2 2.795(3) . ? Bi3 Se2 2.795(3) 1_565 ? Bi3 Se1 2.870(4) . ? Bi3 Se4 3.087(4) 1_544 ? Bi3 Se5 3.234(3) 5_656 ? Bi3 Se5 3.234(3) 5_646 ? Bi3 Cs1 4.443(4) 1_565 ? Cs1 Se4 3.588(5) 1_534 ? Cs1 Se2 3.627(5) 2_524 ? Cs1 Se1 3.686(4) 2_524 ? Cs1 Se1 3.686(4) 2_534 ? Cs1 Se3 3.836(4) 1_544 ? Cs1 Se3 3.836(4) 1_534 ? Cs1 Se2 3.855(5) . ? Cs1 Se2 3.855(5) 1_545 ? Cs1 Cs1 4.171(2) 1_545 ? Cs1 Cs1 4.171(2) 1_565 ? Cs1 Bi3 4.443(4) 1_545 ? Cs1 Bi1 4.557(4) 1_534 ? Se1 Bi2 2.909(3) 1_545 ? Se1 Cs1 3.686(4) 2_525 ? Se1 Cs1 3.686(4) 2_535 ? Se2 Bi3 2.795(3) 1_545 ? Se2 Cs1 3.627(5) 2_525 ? Se2 Cs1 3.855(5) 1_565 ? Se3 Bi1 2.982(3) 1_545 ? Se3 Cs1 3.836(4) 1_576 ? Se3 Cs1 3.836(4) 1_566 ? Se4 Bi1 2.948(3) 5_667 ? Se4 Bi1 2.948(3) 5_657 ? Se4 Bi3 3.087(4) 1_566 ? Se4 Cs1 3.588(5) 1_576 ? Se5 Bi2 3.034(3) 1_565 ? Se5 Bi2 3.163(4) 5_656 ? Se5 Bi3 3.234(3) 5_656 ? Se5 Bi3 3.234(3) 5_646 ? 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 Se4 Bi1 Se4 89.93(10) . 5_667 ? Se4 Bi1 Se4 89.93(10) . 5_657 ? Se4 Bi1 Se4 90.07(12) 5_667 5_657 ? Se4 Bi1 Se5 178.79(12) . . ? Se4 Bi1 Se5 89.21(9) 5_667 . ? Se4 Bi1 Se5 89.21(9) 5_657 . ? Se4 Bi1 Se3 91.17(10) . . ? Se4 Bi1 Se3 178.73(10) 5_667 . ? Se4 Bi1 Se3 90.58(9) 5_657 . ? Se5 Bi1 Se3 89.69(9) . . ? Se4 Bi1 Se3 91.17(10) . 1_565 ? Se4 Bi1 Se3 90.58(9) 5_667 1_565 ? Se4 Bi1 Se3 178.73(10) 5_657 1_565 ? Se5 Bi1 Se3 89.69(9) . 1_565 ? Se3 Bi1 Se3 88.76(12) . 1_565 ? Se4 Bi1 Cs1 51.93(9) . 1_576 ? Se4 Bi1 Cs1 123.75(8) 5_667 1_576 ? Se4 Bi1 Cs1 123.75(8) 5_657 1_576 ? Se5 Bi1 Cs1 129.29(9) . 1_576 ? Se3 Bi1 Cs1 56.65(8) . 1_576 ? Se3 Bi1 Cs1 56.65(8) 1_565 1_576 ? Se3 Bi2 Se1 94.01(10) . . ? Se3 Bi2 Se1 94.01(10) . 1_565 ? Se1 Bi2 Se1 91.61(13) . 1_565 ? Se3 Bi2 Se5 92.23(10) . . ? Se1 Bi2 Se5 173.28(11) . . ? Se1 Bi2 Se5 90.43(8) 1_565 . ? Se3 Bi2 Se5 92.23(10) . 1_545 ? Se1 Bi2 Se5 90.43(8) . 1_545 ? Se1 Bi2 Se5 173.28(11) 1_565 1_545 ? Se5 Bi2 Se5 86.84(11) . 1_545 ? Se3 Bi2 Se5 174.51(13) . 5_656 ? Se1 Bi2 Se5 89.82(9) . 5_656 ? Se1 Bi2 Se5 89.82(9) 1_565 5_656 ? Se5 Bi2 Se5 83.79(9) . 5_656 ? Se5 Bi2 Se5 83.79(9) 1_545 5_656 ? Se2 Bi3 Se2 96.54(15) . 1_565 ? Se2 Bi3 Se1 95.55(11) . . ? Se2 Bi3 Se1 95.55(11) 1_565 . ? Se2 Bi3 Se4 92.11(11) . 1_544 ? Se2 Bi3 Se4 92.11(11) 1_565 1_544 ? Se1 Bi3 Se4 168.48(12) . 1_544 ? Se2 Bi3 Se5 170.39(10) . 5_656 ? Se2 Bi3 Se5 91.34(9) 1_565 5_656 ? Se1 Bi3 Se5 89.13(9) . 5_656 ? Se4 Bi3 Se5 82.08(9) 1_544 5_656 ? Se2 Bi3 Se5 91.34(9) . 5_646 ? Se2 Bi3 Se5 170.39(10) 1_565 5_646 ? Se1 Bi3 Se5 89.13(9) . 5_646 ? Se4 Bi3 Se5 82.08(9) 1_544 5_646 ? Se5 Bi3 Se5 80.32(10) 5_656 5_646 ? Se2 Bi3 Cs1 59.27(9) . 1_565 ? Se2 Bi3 Cs1 59.27(9) 1_565 1_565 ? Se1 Bi3 Cs1 138.22(10) . 1_565 ? Se4 Bi3 Cs1 53.30(9) 1_544 1_565 ? Se5 Bi3 Cs1 121.36(7) 5_656 1_565 ? Se5 Bi3 Cs1 121.36(7) 5_646 1_565 ? Se4 Cs1 Se2 143.47(13) 1_534 2_524 ? Se4 Cs1 Se1 136.17(8) 1_534 2_524 ? Se2 Cs1 Se1 70.01(9) 2_524 2_524 ? Se4 Cs1 Se1 136.17(8) 1_534 2_534 ? Se2 Cs1 Se1 70.01(9) 2_524 2_534 ? Se1 Cs1 Se1 68.92(9) 2_524 2_534 ? Se4 Cs1 Se3 68.86(9) 1_534 1_544 ? Se2 Cs1 Se3 80.72(11) 2_524 1_544 ? Se1 Cs1 Se3 150.51(12) 2_524 1_544 ? Se1 Cs1 Se3 104.78(7) 2_534 1_544 ? Se4 Cs1 Se3 68.86(9) 1_534 1_534 ? Se2 Cs1 Se3 80.72(11) 2_524 1_534 ? Se1 Cs1 Se3 104.78(7) 2_524 1_534 ? Se1 Cs1 Se3 150.51(12) 2_534 1_534 ? Se3 Cs1 Se3 65.86(9) 1_544 1_534 ? Se4 Cs1 Se2 69.34(9) 1_534 . ? Se2 Cs1 Se2 137.56(6) 2_524 . ? Se1 Cs1 Se2 104.82(11) 2_524 . ? Se1 Cs1 Se2 69.12(9) 2_534 . ? Se3 Cs1 Se2 99.04(8) 1_544 . ? Se3 Cs1 Se2 138.19(12) 1_534 . ? Se4 Cs1 Se2 69.34(9) 1_534 1_545 ? Se2 Cs1 Se2 137.56(6) 2_524 1_545 ? Se1 Cs1 Se2 69.12(9) 2_524 1_545 ? Se1 Cs1 Se2 104.82(11) 2_534 1_545 ? Se3 Cs1 Se2 138.19(12) 1_544 1_545 ? Se3 Cs1 Se2 99.04(8) 1_534 1_545 ? Se2 Cs1 Se2 65.50(9) . 1_545 ? Se4 Cs1 Cs1 90.0 1_534 1_545 ? Se2 Cs1 Cs1 90.0 2_524 1_545 ? Se1 Cs1 Cs1 55.54(5) 2_524 1_545 ? Se1 Cs1 Cs1 124.46(5) 2_534 1_545 ? Se3 Cs1 Cs1 122.93(4) 1_544 1_545 ? Se3 Cs1 Cs1 57.07(4) 1_534 1_545 ? Se2 Cs1 Cs1 122.75(5) . 1_545 ? Se2 Cs1 Cs1 57.25(5) 1_545 1_545 ? Se4 Cs1 Cs1 90.0 1_534 1_565 ? Se2 Cs1 Cs1 90.0 2_524 1_565 ? Se1 Cs1 Cs1 124.46(5) 2_524 1_565 ? Se1 Cs1 Cs1 55.54(5) 2_534 1_565 ? Se3 Cs1 Cs1 57.07(4) 1_544 1_565 ? Se3 Cs1 Cs1 122.93(4) 1_534 1_565 ? Se2 Cs1 Cs1 57.25(5) . 1_565 ? Se2 Cs1 Cs1 122.75(5) 1_545 1_565 ? Cs1 Cs1 Cs1 180.00(16) 1_545 1_565 ? Se4 Cs1 Bi3 43.61(7) 1_534 1_545 ? Se2 Cs1 Bi3 172.92(11) 2_524 1_545 ? Se1 Cs1 Bi3 104.29(9) 2_524 1_545 ? Se1 Cs1 Bi3 104.29(9) 2_534 1_545 ? Se3 Cs1 Bi3 105.17(9) 1_544 1_545 ? Se3 Cs1 Bi3 105.17(9) 1_534 1_545 ? Se2 Cs1 Bi3 38.55(6) . 1_545 ? Se2 Cs1 Bi3 38.55(6) 1_545 1_545 ? Cs1 Cs1 Bi3 90.0 1_545 1_545 ? Cs1 Cs1 Bi3 90.0 1_565 1_545 ? Se4 Cs1 Bi1 39.53(7) 1_534 1_534 ? Se2 Cs1 Bi1 103.94(11) 2_524 1_534 ? Se1 Cs1 Bi1 144.15(5) 2_524 1_534 ? Se1 Cs1 Bi1 144.15(5) 2_534 1_534 ? Se3 Cs1 Bi1 40.49(6) 1_544 1_534 ? Se3 Cs1 Bi1 40.49(6) 1_534 1_534 ? Se2 Cs1 Bi1 102.34(9) . 1_534 ? Se2 Cs1 Bi1 102.34(9) 1_545 1_534 ? Cs1 Cs1 Bi1 90.0 1_545 1_534 ? Cs1 Cs1 Bi1 90.0 1_565 1_534 ? Bi3 Cs1 Bi1 83.15(6) 1_545 1_534 ? Bi3 Se1 Bi2 96.09(10) . . ? Bi3 Se1 Bi2 96.09(10) . 1_545 ? Bi2 Se1 Bi2 91.61(13) . 1_545 ? Bi3 Se1 Cs1 94.48(10) . 2_525 ? Bi2 Se1 Cs1 164.35(12) . 2_525 ? Bi2 Se1 Cs1 98.72(6) 1_545 2_525 ? Bi3 Se1 Cs1 94.48(10) . 2_535 ? Bi2 Se1 Cs1 98.72(6) . 2_535 ? Bi2 Se1 Cs1 164.35(12) 1_545 2_535 ? Cs1 Se1 Cs1 68.92(9) 2_525 2_535 ? Bi3 Se2 Bi3 96.54(15) . 1_545 ? Bi3 Se2 Cs1 97.11(11) . 2_525 ? Bi3 Se2 Cs1 97.11(11) 1_545 2_525 ? Bi3 Se2 Cs1 132.17(15) . . ? Bi3 Se2 Cs1 82.18(8) 1_545 . ? Cs1 Se2 Cs1 130.62(10) 2_525 . ? Bi3 Se2 Cs1 82.18(8) . 1_565 ? Bi3 Se2 Cs1 132.17(15) 1_545 1_565 ? Cs1 Se2 Cs1 130.62(10) 2_525 1_565 ? Cs1 Se2 Cs1 65.50(9) . 1_565 ? Bi2 Se3 Bi1 91.28(10) . . ? Bi2 Se3 Bi1 91.28(10) . 1_545 ? Bi1 Se3 Bi1 88.76(12) . 1_545 ? Bi2 Se3 Cs1 138.37(9) . 1_576 ? Bi1 Se3 Cs1 82.87(7) . 1_576 ? Bi1 Se3 Cs1 129.52(12) 1_545 1_576 ? Bi2 Se3 Cs1 138.37(9) . 1_566 ? Bi1 Se3 Cs1 129.52(12) . 1_566 ? Bi1 Se3 Cs1 82.87(7) 1_545 1_566 ? Cs1 Se3 Cs1 65.86(9) 1_576 1_566 ? Bi1 Se4 Bi1 90.07(10) . 5_667 ? Bi1 Se4 Bi1 90.07(10) . 5_657 ? Bi1 Se4 Bi1 90.07(12) 5_667 5_657 ? Bi1 Se4 Bi3 171.63(16) . 1_566 ? Bi1 Se4 Bi3 95.84(9) 5_667 1_566 ? Bi1 Se4 Bi3 95.84(9) 5_657 1_566 ? Bi1 Se4 Cs1 88.54(11) . 1_576 ? Bi1 Se4 Cs1 134.95(6) 5_667 1_576 ? Bi1 Se4 Cs1 134.95(6) 5_657 1_576 ? Bi3 Se4 Cs1 83.08(11) 1_566 1_576 ? Bi1 Se5 Bi2 86.78(9) . . ? Bi1 Se5 Bi2 86.78(9) . 1_565 ? Bi2 Se5 Bi2 86.84(11) . 1_565 ? Bi1 Se5 Bi2 175.88(14) . 5_656 ? Bi2 Se5 Bi2 96.21(9) . 5_656 ? Bi2 Se5 Bi2 96.21(9) 1_565 5_656 ? Bi1 Se5 Bi3 92.46(9) . 5_656 ? Bi2 Se5 Bi3 176.62(10) . 5_656 ? Bi2 Se5 Bi3 96.42(5) 1_565 5_656 ? Bi2 Se5 Bi3 84.39(9) 5_656 5_656 ? Bi1 Se5 Bi3 92.46(9) . 5_646 ? Bi2 Se5 Bi3 96.42(5) . 5_646 ? Bi2 Se5 Bi3 176.62(10) 1_565 5_646 ? Bi2 Se5 Bi3 84.39(9) 5_656 5_646 ? Bi3 Se5 Bi3 80.32(10) 5_656 5_646 ? _diffrn_measured_fraction_theta_max 0.948 _diffrn_reflns_theta_full 27.98 _diffrn_measured_fraction_theta_full 0.948 _refine_diff_density_max 4.173 _refine_diff_density_min -4.842 _refine_diff_density_rms 0.934 # Attachment 'Rb2Ag1.5Bi7.5Se13.CIF' data_new_b _database_code_depnum_ccdc_archive 'CCDC 291022' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Rb2Ag1.5Bi7.5Se13 _chemical_melting_point ? _chemical_formula_moiety Rb2Ag1.5Bi7.5Se13 _chemical_formula_sum 'Ag1.50 Bi7.50 Rb2 Se13' _chemical_formula_weight 2927.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Se Se -0.0929 2.2259 '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' Ag Ag -0.8971 1.1015 '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 Pnnm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z' '-x-1/2, y-1/2, z-1/2' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.386(2) _cell_length_b 27.642(5) _cell_length_c 4.1107(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1407.4(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 11237 _cell_measurement_theta_min 1.47 _cell_measurement_theta_max 28.29 _exptl_crystal_description needle _exptl_crystal_colour black _exptl_crystal_size_max 0.264 _exptl_crystal_size_mid 0.046 _exptl_crystal_size_min 0.026 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 6.906 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2418 _exptl_absorpt_coefficient_mu 67.966 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.448201 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ; An analytical absorption correction was performed using face indexing and the program XPREP, followed by a semiempirical absorption correction based on symmetrically equivalent reflections with the program SADABS. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 11237 _diffrn_reflns_av_R_equivalents 0.0922 _diffrn_reflns_av_sigmaI/netI 0.1157 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 4 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 28.29 _reflns_number_total 1956 _reflns_number_gt 911 _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^)+(0.0387P)^2^+0.0000P] 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 0.00037(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1956 _refine_ls_number_parameters 86 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1021 _refine_ls_R_factor_gt 0.0389 _refine_ls_wR_factor_ref 0.0923 _refine_ls_wR_factor_gt 0.0831 _refine_ls_goodness_of_fit_ref 0.799 _refine_ls_restrained_S_all 0.799 _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 Bi1 Bi 0.5000 0.5000 1.0000 0.0154(4) Uani 0.67 4 d SP . . Ag1 Ag 0.5000 0.5000 1.0000 0.0154(4) Uani 0.33 4 d SP . . Bi2 Bi 0.2208(8) 0.4603(2) 0.5000 0.0154(8) Uani 0.72 2 d SP . . Ag2 Ag 0.225(4) 0.4677(13) 0.5000 0.0154(8) Uani 0.28 2 d SP . . Bi3 Bi -0.05675(17) 0.42189(4) 0.0000 0.0156(4) Uani 0.93 2 d SP . . Ag3 Ag -0.057(5) 0.4068(14) 0.0000 0.0156(4) Uani 0.07 2 d SP . . Bi4 Bi 0.6690(2) 0.38634(8) 0.5000 0.0162(5) Uani 0.77 2 d SP . . Ag4 Ag 0.682(2) 0.3750(7) 0.5000 0.0162(5) Uani 0.23 2 d SP . . Bi5 Bi 0.38976(8) 0.34455(4) 0.0000 0.0144(3) Uani 1 2 d S . . Rb1 Rb 0.0779(2) 0.27957(9) -1.0000 0.0227(6) Uani 1 2 d S . . Se1 Se 0.6099(2) 0.31985(9) 0.0000 0.0135(5) Uani 1 2 d S . . Se2 Se 0.3313(2) 0.28251(10) -0.5000 0.0168(6) Uani 1 2 d S . . Se3 Se 0.16756(19) 0.39650(10) 0.0000 0.0147(6) Uani 1 2 d S . . Se4 Se -0.1061(2) 0.35434(9) -0.5000 0.0149(6) Uani 1 2 d S . . Se5 Se 0.4468(2) 0.42986(9) 0.5000 0.0129(6) Uani 1 2 d S . . Se6 Se 0.2792(2) 0.53768(10) 1.0000 0.0151(6) Uani 1 2 d S . . Se7 Se 0.0000 0.5000 0.5000 0.0123(8) 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 0.0127(9) 0.0197(10) 0.0138(10) 0.000 0.000 -0.0015(7) Ag1 0.0127(9) 0.0197(10) 0.0138(10) 0.000 0.000 -0.0015(7) Bi2 0.0125(11) 0.018(2) 0.0155(6) 0.000 0.000 -0.0007(18) Ag2 0.0125(11) 0.018(2) 0.0155(6) 0.000 0.000 -0.0007(18) Bi3 0.0115(6) 0.0205(9) 0.0149(6) 0.000 0.000 0.0003(8) Ag3 0.0115(6) 0.0205(9) 0.0149(6) 0.000 0.000 0.0003(8) Bi4 0.0127(11) 0.0209(15) 0.0148(7) 0.000 0.000 -0.0008(9) Ag4 0.0127(11) 0.0209(15) 0.0148(7) 0.000 0.000 -0.0008(9) Bi5 0.0112(5) 0.0198(5) 0.0121(5) 0.000 0.000 -0.0014(4) Rb1 0.0279(16) 0.0192(14) 0.0210(15) 0.000 0.000 -0.0070(12) Se1 0.0101(12) 0.0178(14) 0.0125(13) 0.000 0.000 -0.0002(11) Se2 0.0143(14) 0.0208(15) 0.0153(15) 0.000 0.000 -0.0044(11) Se3 0.0087(13) 0.0216(15) 0.0139(15) 0.000 0.000 0.0006(11) Se4 0.0135(13) 0.0199(14) 0.0114(14) 0.000 0.000 0.0019(12) Se5 0.0105(14) 0.0161(14) 0.0122(15) 0.000 0.000 0.0016(11) Se6 0.0088(12) 0.0217(14) 0.0147(14) 0.000 0.000 0.0019(11) Se7 0.0092(19) 0.018(2) 0.010(2) 0.000 0.000 0.0006(15) _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 Se5 2.9013(18) 5_667 ? Bi1 Se5 2.9013(18) . ? Bi1 Se5 2.9013(18) 5_666 ? Bi1 Se5 2.9013(18) 1_556 ? Bi1 Se6 2.927(3) . ? Bi1 Se6 2.927(3) 5_667 ? Bi2 Se3 2.787(4) . ? Bi2 Se3 2.787(4) 1_556 ? Bi2 Se5 2.923(11) . ? Bi2 Se7 2.947(10) . ? Bi2 Se6 3.054(4) . ? Bi2 Se6 3.054(4) 1_554 ? Ag2 Se6 2.90(2) . ? Ag2 Se6 2.90(2) 1_554 ? Ag2 Se7 2.93(6) . ? Ag2 Se3 2.93(2) . ? Ag2 Se3 2.93(2) 1_556 ? Ag2 Se5 2.94(6) . ? Bi3 Se4 2.843(2) . ? Bi3 Se4 2.843(2) 1_556 ? Bi3 Se3 2.866(3) . ? Bi3 Se6 2.973(3) 5_566 ? Bi3 Se7 3.0627(10) . ? Bi3 Se7 3.0627(10) 1_554 ? Bi3 Rb1 4.273(3) 1_556 ? Ag3 Se4 2.59(3) . ? Ag3 Se4 2.59(3) 1_556 ? Ag3 Se3 2.80(6) . ? Ag3 Rb1 3.89(4) 1_556 ? Bi4 Se1 2.853(3) . ? Bi4 Se1 2.853(3) 1_556 ? Bi4 Se4 2.923(4) 1_656 ? Bi4 Se5 3.003(4) . ? Bi4 Se6 3.008(3) 5_667 ? Bi4 Se6 3.008(3) 5_666 ? Ag4 Se4 2.68(2) 1_656 ? Ag4 Se1 2.711(16) . ? Ag4 Se1 2.711(16) 1_556 ? Bi5 Se2 2.7732(19) . ? Bi5 Se2 2.7732(19) 1_556 ? Bi5 Se1 2.811(3) . ? Bi5 Se3 3.104(3) . ? Bi5 Se5 3.207(2) . ? Bi5 Se5 3.207(2) 1_554 ? Bi5 Rb1 4.260(3) 1_556 ? Rb1 Se3 3.418(4) 1_554 ? Rb1 Se1 3.455(3) 3_453 ? Rb1 Se1 3.455(3) 3_454 ? Rb1 Se2 3.503(4) 3_453 ? Rb1 Se4 3.699(3) 1_554 ? Rb1 Se4 3.699(3) . ? Rb1 Se2 3.753(3) . ? Rb1 Se2 3.753(3) 1_554 ? Rb1 Ag3 3.89(4) 1_554 ? Rb1 Rb1 4.1107(8) 1_556 ? Rb1 Rb1 4.1107(8) 1_554 ? Rb1 Bi5 4.260(3) 1_554 ? Se1 Ag4 2.711(16) 1_554 ? Se1 Bi4 2.853(3) 1_554 ? Se1 Rb1 3.455(3) 3_553 ? Se1 Rb1 3.455(3) 3_554 ? Se2 Bi5 2.7732(19) 1_554 ? Se2 Rb1 3.503(4) 3_553 ? Se2 Rb1 3.753(3) 1_556 ? Se3 Bi2 2.787(4) 1_554 ? Se3 Ag2 2.93(2) 1_554 ? Se3 Rb1 3.418(4) 1_556 ? Se4 Ag3 2.59(3) 1_554 ? Se4 Ag4 2.68(2) 1_454 ? Se4 Bi3 2.843(2) 1_554 ? Se4 Bi4 2.923(4) 1_454 ? Se4 Rb1 3.699(3) 1_556 ? Se5 Ag1 2.9013(18) 1_554 ? Se5 Bi1 2.9013(18) 1_554 ? Se5 Bi5 3.207(2) 1_556 ? Se6 Ag2 2.90(2) 1_556 ? Se6 Bi3 2.973(3) 5_566 ? Se6 Bi4 3.008(3) 5_667 ? Se6 Bi4 3.008(3) 5_666 ? Se6 Bi2 3.054(4) 1_556 ? Se7 Ag2 2.93(6) 5_566 ? Se7 Bi2 2.947(10) 5_566 ? Se7 Bi3 3.0627(10) 5_566 ? Se7 Bi3 3.0627(10) 5_565 ? Se7 Bi3 3.0627(10) 1_556 ? 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 Se5 Bi1 Se5 180.00(7) 5_667 . ? Se5 Bi1 Se5 90.21(7) 5_667 5_666 ? Se5 Bi1 Se5 89.79(7) . 5_666 ? Se5 Bi1 Se5 89.79(7) 5_667 1_556 ? Se5 Bi1 Se5 90.21(7) . 1_556 ? Se5 Bi1 Se5 180.00(7) 5_666 1_556 ? Se5 Bi1 Se6 88.54(6) 5_667 . ? Se5 Bi1 Se6 91.46(6) . . ? Se5 Bi1 Se6 88.54(6) 5_666 . ? Se5 Bi1 Se6 91.46(6) 1_556 . ? Se5 Bi1 Se6 91.46(6) 5_667 5_667 ? Se5 Bi1 Se6 88.54(6) . 5_667 ? Se5 Bi1 Se6 91.46(6) 5_666 5_667 ? Se5 Bi1 Se6 88.54(6) 1_556 5_667 ? Se6 Bi1 Se6 180.0 . 5_667 ? Se3 Bi2 Se3 95.06(19) . 1_556 ? Se3 Bi2 Se5 92.6(2) . . ? Se3 Bi2 Se5 92.6(2) 1_556 . ? Se3 Bi2 Se7 90.9(2) . . ? Se3 Bi2 Se7 90.9(2) 1_556 . ? Se5 Bi2 Se7 174.8(2) . . ? Se3 Bi2 Se6 174.61(18) . . ? Se3 Bi2 Se6 90.16(6) 1_556 . ? Se5 Bi2 Se6 88.5(2) . . ? Se7 Bi2 Se6 87.6(2) . . ? Se3 Bi2 Se6 90.16(6) . 1_554 ? Se3 Bi2 Se6 174.61(18) 1_556 1_554 ? Se5 Bi2 Se6 88.5(2) . 1_554 ? Se7 Bi2 Se6 87.6(2) . 1_554 ? Se6 Bi2 Se6 84.60(15) . 1_554 ? Se6 Ag2 Se6 90.2(10) . 1_554 ? Se6 Ag2 Se7 90.9(12) . . ? Se6 Ag2 Se7 90.9(12) 1_554 . ? Se6 Ag2 Se3 179.2(17) . . ? Se6 Ag2 Se3 90.40(6) 1_554 . ? Se7 Ag2 Se3 88.5(12) . . ? Se6 Ag2 Se3 90.40(6) . 1_556 ? Se6 Ag2 Se3 179.2(17) 1_554 1_556 ? Se7 Ag2 Se3 88.5(12) . 1_556 ? Se3 Ag2 Se3 89.0(9) . 1_556 ? Se6 Ag2 Se5 91.2(12) . . ? Se6 Ag2 Se5 91.2(12) 1_554 . ? Se7 Ag2 Se5 176.9(13) . . ? Se3 Ag2 Se5 89.3(11) . . ? Se3 Ag2 Se5 89.3(11) 1_556 . ? Se4 Bi3 Se4 92.59(8) . 1_556 ? Se4 Bi3 Se3 92.72(7) . . ? Se4 Bi3 Se3 92.72(7) 1_556 . ? Se4 Bi3 Se6 92.74(8) . 5_566 ? Se4 Bi3 Se6 92.74(8) 1_556 5_566 ? Se3 Bi3 Se6 172.10(9) . 5_566 ? Se4 Bi3 Se7 175.86(5) . . ? Se4 Bi3 Se7 91.55(4) 1_556 . ? Se3 Bi3 Se7 87.14(6) . . ? Se6 Bi3 Se7 87.00(5) 5_566 . ? Se4 Bi3 Se7 91.55(4) . 1_554 ? Se4 Bi3 Se7 175.86(5) 1_556 1_554 ? Se3 Bi3 Se7 87.14(6) . 1_554 ? Se6 Bi3 Se7 87.00(5) 5_566 1_554 ? Se7 Bi3 Se7 84.30(3) . 1_554 ? Se4 Bi3 Rb1 58.61(5) . 1_556 ? Se4 Bi3 Rb1 58.61(5) 1_556 1_556 ? Se3 Bi3 Rb1 52.85(6) . 1_556 ? Se6 Bi3 Rb1 135.05(8) 5_566 1_556 ? Se7 Bi3 Rb1 124.02(5) . 1_556 ? Se7 Bi3 Rb1 124.02(5) 1_554 1_556 ? Se4 Ag3 Se4 105.1(15) . 1_556 ? Se4 Ag3 Se3 100.1(14) . . ? Se4 Ag3 Se3 100.1(14) 1_556 . ? Se4 Ag3 Rb1 66.1(8) . 1_556 ? Se4 Ag3 Rb1 66.1(8) 1_556 1_556 ? Se3 Ag3 Rb1 58.7(9) . 1_556 ? Se1 Bi4 Se1 92.20(11) . 1_556 ? Se1 Bi4 Se4 92.84(8) . 1_656 ? Se1 Bi4 Se4 92.84(8) 1_556 1_656 ? Se1 Bi4 Se5 91.32(10) . . ? Se1 Bi4 Se5 91.32(10) 1_556 . ? Se4 Bi4 Se5 173.99(13) 1_656 . ? Se1 Bi4 Se6 175.51(9) . 5_667 ? Se1 Bi4 Se6 90.70(5) 1_556 5_667 ? Se4 Bi4 Se6 90.44(10) 1_656 5_667 ? Se5 Bi4 Se6 85.18(7) . 5_667 ? Se1 Bi4 Se6 90.70(5) . 5_666 ? Se1 Bi4 Se6 175.51(9) 1_556 5_666 ? Se4 Bi4 Se6 90.44(10) 1_656 5_666 ? Se5 Bi4 Se6 85.18(7) . 5_666 ? Se6 Bi4 Se6 86.20(10) 5_667 5_666 ? Se4 Ag4 Se1 101.7(5) 1_656 . ? Se4 Ag4 Se1 101.7(5) 1_656 1_556 ? Se1 Ag4 Se1 98.6(8) . 1_556 ? Se2 Bi5 Se2 95.66(9) . 1_556 ? Se2 Bi5 Se1 95.92(7) . . ? Se2 Bi5 Se1 95.92(7) 1_556 . ? Se2 Bi5 Se3 93.12(7) . . ? Se2 Bi5 Se3 93.12(7) 1_556 . ? Se1 Bi5 Se3 166.50(8) . . ? Se2 Bi5 Se5 170.86(6) . . ? Se2 Bi5 Se5 92.14(5) 1_556 . ? Se1 Bi5 Se5 87.99(6) . . ? Se3 Bi5 Se5 81.67(6) . . ? Se2 Bi5 Se5 92.14(5) . 1_554 ? Se2 Bi5 Se5 170.86(6) 1_556 1_554 ? Se1 Bi5 Se5 87.99(6) . 1_554 ? Se3 Bi5 Se5 81.67(6) . 1_554 ? Se5 Bi5 Se5 79.72(6) . 1_554 ? Se2 Bi5 Rb1 60.16(5) . 1_556 ? Se2 Bi5 Rb1 60.16(5) 1_556 1_556 ? Se1 Bi5 Rb1 141.01(7) . 1_556 ? Se3 Bi5 Rb1 52.49(6) . 1_556 ? Se5 Bi5 Rb1 120.65(5) . 1_556 ? Se5 Bi5 Rb1 120.65(5) 1_554 1_556 ? Se3 Rb1 Se1 135.64(6) 1_554 3_453 ? Se3 Rb1 Se1 135.64(6) 1_554 3_454 ? Se1 Rb1 Se1 73.02(7) 3_453 3_454 ? Se3 Rb1 Se2 138.30(10) 1_554 3_453 ? Se1 Rb1 Se2 73.17(7) 3_453 3_453 ? Se1 Rb1 Se2 73.17(7) 3_454 3_453 ? Se3 Rb1 Se4 70.84(7) 1_554 1_554 ? Se1 Rb1 Se4 100.64(5) 3_453 1_554 ? Se1 Rb1 Se4 147.75(10) 3_454 1_554 ? Se2 Rb1 Se4 74.74(7) 3_453 1_554 ? Se3 Rb1 Se4 70.84(7) 1_554 . ? Se1 Rb1 Se4 147.75(10) 3_453 . ? Se1 Rb1 Se4 100.64(5) 3_454 . ? Se2 Rb1 Se4 74.74(7) 3_453 . ? Se4 Rb1 Se4 67.50(6) 1_554 . ? Se3 Rb1 Se2 73.00(7) 1_554 . ? Se1 Rb1 Se2 104.30(9) 3_453 . ? Se1 Rb1 Se2 66.13(7) 3_454 . ? Se2 Rb1 Se2 137.71(5) 3_453 . ? Se4 Rb1 Se2 143.83(9) 1_554 . ? Se4 Rb1 Se2 101.46(5) . . ? Se3 Rb1 Se2 73.00(7) 1_554 1_554 ? Se1 Rb1 Se2 66.13(7) 3_453 1_554 ? Se1 Rb1 Se2 104.30(9) 3_454 1_554 ? Se2 Rb1 Se2 137.71(5) 3_453 1_554 ? Se4 Rb1 Se2 101.46(5) 1_554 1_554 ? Se4 Rb1 Se2 143.83(9) . 1_554 ? Se2 Rb1 Se2 66.42(6) . 1_554 ? Se3 Rb1 Ag3 44.4(8) 1_554 1_554 ? Se1 Rb1 Ag3 140.2(3) 3_453 1_554 ? Se1 Rb1 Ag3 140.2(3) 3_454 1_554 ? Se2 Rb1 Ag3 93.9(8) 3_453 1_554 ? Se4 Rb1 Ag3 39.7(4) 1_554 1_554 ? Se4 Rb1 Ag3 39.7(4) . 1_554 ? Se2 Rb1 Ag3 109.8(7) . 1_554 ? Se2 Rb1 Ag3 109.8(7) 1_554 1_554 ? Se3 Rb1 Rb1 90.0 1_554 1_556 ? Se1 Rb1 Rb1 126.51(4) 3_453 1_556 ? Se1 Rb1 Rb1 53.49(4) 3_454 1_556 ? Se2 Rb1 Rb1 90.0 3_453 1_556 ? Se4 Rb1 Rb1 123.75(3) 1_554 1_556 ? Se4 Rb1 Rb1 56.25(3) . 1_556 ? Se2 Rb1 Rb1 56.79(3) . 1_556 ? Se2 Rb1 Rb1 123.21(3) 1_554 1_556 ? Ag3 Rb1 Rb1 90.0 1_554 1_556 ? Se3 Rb1 Rb1 90.0 1_554 1_554 ? Se1 Rb1 Rb1 53.49(4) 3_453 1_554 ? Se1 Rb1 Rb1 126.51(4) 3_454 1_554 ? Se2 Rb1 Rb1 90.0 3_453 1_554 ? Se4 Rb1 Rb1 56.25(3) 1_554 1_554 ? Se4 Rb1 Rb1 123.75(3) . 1_554 ? Se2 Rb1 Rb1 123.21(3) . 1_554 ? Se2 Rb1 Rb1 56.79(3) 1_554 1_554 ? Ag3 Rb1 Rb1 90.0 1_554 1_554 ? Rb1 Rb1 Rb1 180.00(15) 1_556 1_554 ? Se3 Rb1 Bi5 46.10(5) 1_554 1_554 ? Se1 Rb1 Bi5 103.37(7) 3_453 1_554 ? Se1 Rb1 Bi5 103.37(7) 3_454 1_554 ? Se2 Rb1 Bi5 175.61(9) 3_453 1_554 ? Se4 Rb1 Bi5 108.84(7) 1_554 1_554 ? Se4 Rb1 Bi5 108.83(7) . 1_554 ? Se2 Rb1 Bi5 39.87(4) . 1_554 ? Se2 Rb1 Bi5 39.87(4) 1_554 1_554 ? Ag3 Rb1 Bi5 90.5(8) 1_554 1_554 ? Rb1 Rb1 Bi5 90.0 1_556 1_554 ? Rb1 Rb1 Bi5 90.0 1_554 1_554 ? Ag4 Se1 Ag4 98.6(8) . 1_554 ? Ag4 Se1 Bi5 100.6(5) . . ? Ag4 Se1 Bi5 100.6(5) 1_554 . ? Ag4 Se1 Bi4 6.7(4) . . ? Ag4 Se1 Bi4 95.7(3) 1_554 . ? Bi5 Se1 Bi4 95.30(8) . . ? Ag4 Se1 Bi4 95.7(3) . 1_554 ? Ag4 Se1 Bi4 6.7(4) 1_554 1_554 ? Bi5 Se1 Bi4 95.30(8) . 1_554 ? Bi4 Se1 Bi4 92.20(11) . 1_554 ? Ag4 Se1 Rb1 159.4(4) . 3_553 ? Ag4 Se1 Rb1 91.9(3) 1_554 3_553 ? Bi5 Se1 Rb1 94.69(8) . 3_553 ? Bi4 Se1 Rb1 166.08(9) . 3_553 ? Bi4 Se1 Rb1 96.51(5) 1_554 3_553 ? Ag4 Se1 Rb1 91.9(3) . 3_554 ? Ag4 Se1 Rb1 159.4(4) 1_554 3_554 ? Bi5 Se1 Rb1 94.69(8) . 3_554 ? Bi4 Se1 Rb1 96.51(5) . 3_554 ? Bi4 Se1 Rb1 166.08(9) 1_554 3_554 ? Rb1 Se1 Rb1 73.02(7) 3_553 3_554 ? Bi5 Se2 Bi5 95.66(9) . 1_554 ? Bi5 Se2 Rb1 94.31(7) . 3_553 ? Bi5 Se2 Rb1 94.31(7) 1_554 3_553 ? Bi5 Se2 Rb1 129.63(10) . . ? Bi5 Se2 Rb1 79.97(5) 1_554 . ? Rb1 Se2 Rb1 135.94(5) 3_553 . ? Bi5 Se2 Rb1 79.97(5) . 1_556 ? Bi5 Se2 Rb1 129.63(10) 1_554 1_556 ? Rb1 Se2 Rb1 135.94(5) 3_553 1_556 ? Rb1 Se2 Rb1 66.42(6) . 1_556 ? Bi2 Se3 Bi2 95.06(19) . 1_554 ? Bi2 Se3 Ag3 99.8(6) . . ? Bi2 Se3 Ag3 99.8(6) 1_554 . ? Bi2 Se3 Bi3 94.3(2) . . ? Bi2 Se3 Bi3 94.3(2) 1_554 . ? Ag3 Se3 Bi3 8.3(8) . . ? Bi2 Se3 Ag2 3.1(6) . . ? Bi2 Se3 Ag2 92.0(4) 1_554 . ? Ag3 Se3 Ag2 100.0(12) . . ? Bi3 Se3 Ag2 94.1(11) . . ? Bi2 Se3 Ag2 92.0(4) . 1_554 ? Bi2 Se3 Ag2 3.1(6) 1_554 1_554 ? Ag3 Se3 Ag2 100.0(12) . 1_554 ? Bi3 Se3 Ag2 94.1(11) . 1_554 ? Ag2 Se3 Ag2 89.0(9) . 1_554 ? Bi2 Se3 Bi5 94.8(2) . . ? Bi2 Se3 Bi5 94.8(2) 1_554 . ? Ag3 Se3 Bi5 158.3(8) . . ? Bi3 Se3 Bi5 166.62(10) . . ? Ag2 Se3 Bi5 95.5(11) . . ? Ag2 Se3 Bi5 95.5(11) 1_554 . ? Bi2 Se3 Rb1 132.45(9) . 1_556 ? Bi2 Se3 Rb1 132.45(9) 1_554 1_556 ? Ag3 Se3 Rb1 76.9(8) . 1_556 ? Bi3 Se3 Rb1 85.21(8) . 1_556 ? Ag2 Se3 Rb1 135.5(5) . 1_556 ? Ag2 Se3 Rb1 135.5(5) 1_554 1_556 ? Bi5 Se3 Rb1 81.41(8) . 1_556 ? Ag3 Se4 Ag3 105.1(15) . 1_554 ? Ag3 Se4 Ag4 96.3(13) . 1_454 ? Ag3 Se4 Ag4 96.3(13) 1_554 1_454 ? Ag3 Se4 Bi3 7.0(7) . . ? Ag3 Se4 Bi3 98.9(7) 1_554 . ? Ag4 Se4 Bi3 94.0(3) 1_454 . ? Ag3 Se4 Bi3 98.9(7) . 1_554 ? Ag3 Se4 Bi3 7.0(7) 1_554 1_554 ? Ag4 Se4 Bi3 94.0(3) 1_454 1_554 ? Bi3 Se4 Bi3 92.59(8) . 1_554 ? Ag3 Se4 Bi4 93.1(13) . 1_454 ? Ag3 Se4 Bi4 93.1(13) 1_554 1_454 ? Ag4 Se4 Bi4 5.3(5) 1_454 1_454 ? Bi3 Se4 Bi4 90.35(8) . 1_454 ? Bi3 Se4 Bi4 90.35(8) 1_554 1_454 ? Ag3 Se4 Rb1 127.6(13) . . ? Ag3 Se4 Rb1 74.2(10) 1_554 . ? Ag4 Se4 Rb1 136.1(3) 1_454 . ? Bi3 Se4 Rb1 129.51(10) . . ? Bi3 Se4 Rb1 80.39(6) 1_554 . ? Bi4 Se4 Rb1 139.11(7) 1_454 . ? Ag3 Se4 Rb1 74.2(10) . 1_556 ? Ag3 Se4 Rb1 127.6(13) 1_554 1_556 ? Ag4 Se4 Rb1 136.1(3) 1_454 1_556 ? Bi3 Se4 Rb1 80.39(6) . 1_556 ? Bi3 Se4 Rb1 129.51(10) 1_554 1_556 ? Bi4 Se4 Rb1 139.11(7) 1_454 1_556 ? Rb1 Se4 Rb1 67.50(6) . 1_556 ? Bi1 Se5 Ag1 90.21(7) . 1_554 ? Bi1 Se5 Bi1 90.21(7) . 1_554 ? Ag1 Se5 Bi1 0.0 1_554 1_554 ? Bi1 Se5 Bi2 91.46(10) . . ? Ag1 Se5 Bi2 91.46(10) 1_554 . ? Bi1 Se5 Bi2 91.46(10) 1_554 . ? Bi1 Se5 Ag2 88.5(5) . . ? Ag1 Se5 Ag2 88.5(5) 1_554 . ? Bi1 Se5 Ag2 88.5(5) 1_554 . ? Bi2 Se5 Ag2 4.1(8) . . ? Bi1 Se5 Bi4 93.42(7) . . ? Ag1 Se5 Bi4 93.42(7) 1_554 . ? Bi1 Se5 Bi4 93.42(7) 1_554 . ? Bi2 Se5 Bi4 173.09(15) . . ? Ag2 Se5 Bi4 177.2(7) . . ? Bi1 Se5 Bi5 174.53(7) . . ? Ag1 Se5 Bi5 95.01(2) 1_554 . ? Bi1 Se5 Bi5 95.01(2) 1_554 . ? Bi2 Se5 Bi5 90.02(10) . . ? Ag2 Se5 Bi5 93.2(5) . . ? Bi4 Se5 Bi5 84.68(7) . . ? Bi1 Se5 Bi5 95.01(2) . 1_556 ? Ag1 Se5 Bi5 174.53(7) 1_554 1_556 ? Bi1 Se5 Bi5 174.53(7) 1_554 1_556 ? Bi2 Se5 Bi5 90.02(10) . 1_556 ? Ag2 Se5 Bi5 93.2(5) . 1_556 ? Bi4 Se5 Bi5 84.68(7) . 1_556 ? Bi5 Se5 Bi5 79.72(6) . 1_556 ? Ag2 Se6 Ag2 90.2(10) . 1_556 ? Ag2 Se6 Bi1 88.8(11) . . ? Ag2 Se6 Bi1 88.8(11) 1_556 . ? Ag2 Se6 Bi3 92.1(11) . 5_566 ? Ag2 Se6 Bi3 92.1(11) 1_556 5_566 ? Bi1 Se6 Bi3 178.77(11) . 5_566 ? Ag2 Se6 Bi4 177.5(8) . 5_667 ? Ag2 Se6 Bi4 91.8(5) 1_556 5_667 ? Bi1 Se6 Bi4 92.80(8) . 5_667 ? Bi3 Se6 Bi4 86.30(8) 5_566 5_667 ? Ag2 Se6 Bi4 91.8(5) . 5_666 ? Ag2 Se6 Bi4 177.5(8) 1_556 5_666 ? Bi1 Se6 Bi4 92.80(8) . 5_666 ? Bi3 Se6 Bi4 86.30(8) 5_566 5_666 ? Bi4 Se6 Bi4 86.20(10) 5_667 5_666 ? Ag2 Se6 Bi2 2.8(6) . . ? Ag2 Se6 Bi2 87.4(4) 1_556 . ? Bi1 Se6 Bi2 88.4(2) . . ? Bi3 Se6 Bi2 92.5(2) 5_566 . ? Bi4 Se6 Bi2 178.5(2) 5_667 . ? Bi4 Se6 Bi2 94.59(8) 5_666 . ? Ag2 Se6 Bi2 87.4(4) . 1_556 ? Ag2 Se6 Bi2 2.8(6) 1_556 1_556 ? Bi1 Se6 Bi2 88.4(2) . 1_556 ? Bi3 Se6 Bi2 92.5(2) 5_566 1_556 ? Bi4 Se6 Bi2 94.59(8) 5_667 1_556 ? Bi4 Se6 Bi2 178.5(2) 5_666 1_556 ? Bi2 Se6 Bi2 84.60(15) . 1_556 ? Ag2 Se7 Ag2 180.000(3) . 5_566 ? Ag2 Se7 Bi2 4.1(8) . . ? Ag2 Se7 Bi2 175.9(8) 5_566 . ? Ag2 Se7 Bi2 175.9(8) . 5_566 ? Ag2 Se7 Bi2 4.1(8) 5_566 5_566 ? Bi2 Se7 Bi2 180.000(1) . 5_566 ? Ag2 Se7 Bi3 89.8(5) . 5_566 ? Ag2 Se7 Bi3 90.2(5) 5_566 5_566 ? Bi2 Se7 Bi3 92.85(9) . 5_566 ? Bi2 Se7 Bi3 87.15(9) 5_566 5_566 ? Ag2 Se7 Bi3 90.2(5) . . ? Ag2 Se7 Bi3 89.8(5) 5_566 . ? Bi2 Se7 Bi3 87.15(9) . . ? Bi2 Se7 Bi3 92.85(9) 5_566 . ? Bi3 Se7 Bi3 180.00(3) 5_566 . ? Ag2 Se7 Bi3 89.8(5) . 5_565 ? Ag2 Se7 Bi3 90.2(5) 5_566 5_565 ? Bi2 Se7 Bi3 92.85(9) . 5_565 ? Bi2 Se7 Bi3 87.15(9) 5_566 5_565 ? Bi3 Se7 Bi3 84.30(3) 5_566 5_565 ? Bi3 Se7 Bi3 95.70(3) . 5_565 ? Ag2 Se7 Bi3 90.2(5) . 1_556 ? Ag2 Se7 Bi3 89.8(5) 5_566 1_556 ? Bi2 Se7 Bi3 87.15(9) . 1_556 ? Bi2 Se7 Bi3 92.85(9) 5_566 1_556 ? Bi3 Se7 Bi3 95.70(3) 5_566 1_556 ? Bi3 Se7 Bi3 84.30(3) . 1_556 ? Bi3 Se7 Bi3 180.00(3) 5_565 1_556 ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 3.907 _refine_diff_density_min -2.548 _refine_diff_density_rms 0.567 # Attachment 'Rb2Cd6Se11.CIF' data_58s _database_code_depnum_ccdc_archive 'CCDC 291023' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Rb2CdBi6Se11 _chemical_melting_point ? _chemical_formula_moiety Rb2CdBi6Se11 _chemical_formula_sum 'Bi6 Cd Rb2 Se11' _chemical_formula_weight 2407.22 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Se Se -0.0929 2.2259 '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' 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 Pnnm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z' 'x-1/2, -y-1/2, z-1/2' '-x-1/2, y-1/2, z-1/2' _cell_length_a 12.385(3) _cell_length_b 23.839(6) _cell_length_c 4.1124(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1214.1(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 10010 _cell_measurement_theta_min 1.71 _cell_measurement_theta_max 27.98 _exptl_crystal_description needle _exptl_crystal_colour black _exptl_crystal_size_max 0.238 _exptl_crystal_size_mid 0.028 _exptl_crystal_size_min 0.028 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 6.581 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1988 _exptl_absorpt_coefficient_mu 64.636 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.469545 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ; An analytical absorption correction was performed using face indexing and the program XPREP, followed by a semiempirical absorption correction based on symmetrically equivalent reflections with the program SADABS. ; _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 '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 10010 _diffrn_reflns_av_R_equivalents 0.1763 _diffrn_reflns_av_sigmaI/netI 0.1603 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 28.29 _reflns_number_total 1681 _reflns_number_gt 790 _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^)+(0.0807P)^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_number_reflns 1681 _refine_ls_number_parameters 65 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1565 _refine_ls_R_factor_gt 0.0640 _refine_ls_wR_factor_ref 0.1751 _refine_ls_wR_factor_gt 0.1497 _refine_ls_goodness_of_fit_ref 0.929 _refine_ls_restrained_S_all 0.929 _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 0.5000 0.5000 0.0000 0.0091(9) Uani 0.733(9) 4 d SP . . Cd1 Cd 0.5000 0.5000 0.0000 0.0091(9) Uani 0.27 4 d SP . . Bi2 Bi 0.22478(13) 0.54771(8) -0.5000 0.0122(4) Uani 1 2 d S . . Bi3 Bi 0.95032(15) 0.59096(9) -1.0000 0.0123(7) Uani 0.645(7) 2 d SP . . Cd3 Cd 0.95032(15) 0.59096(9) -1.0000 0.0123(7) Uani 0.35 2 d SP . . Bi4 Bi 0.66749(13) 0.64035(7) -0.5000 0.0117(4) Uani 1 2 d S . . Se1 Se 0.8904(4) 0.66589(19) -0.5000 0.0143(10) Uani 1 2 d S . . Se2 Se 0.4432(3) 0.5812(2) -0.5000 0.0144(10) Uani 1 2 d S . . Se3 Se 0.1674(4) 0.62715(19) -1.0000 0.0159(10) Uani 1 2 d S . . Se4 Se 0.6142(4) 0.7141(2) -1.0000 0.0176(10) Uani 1 2 d S . . Se5 Se 0.2760(3) 0.4579(2) 0.0000 0.0105(9) Uani 1 2 d S . . Se6 Se 0.0000 0.5000 -0.5000 0.0163(15) Uani 1 4 d S . . Rb1 Rb 0.8586(4) 0.7841(2) -1.0000 0.0376(14) Uani 1 2 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 0.0048(13) 0.0171(18) 0.0053(13) 0.000 0.000 -0.0023(11) Cd1 0.0048(13) 0.0171(18) 0.0053(13) 0.000 0.000 -0.0023(11) Bi2 0.0078(8) 0.0217(10) 0.0072(7) 0.000 0.000 -0.0017(7) Bi3 0.0085(10) 0.0232(14) 0.0050(10) 0.000 0.000 0.0017(9) Cd3 0.0085(10) 0.0232(14) 0.0050(10) 0.000 0.000 0.0017(9) Bi4 0.0100(8) 0.0212(10) 0.0038(7) 0.000 0.000 0.0027(7) Se1 0.009(2) 0.020(3) 0.014(2) 0.000 0.000 -0.0037(19) Se2 0.007(2) 0.018(3) 0.017(2) 0.000 0.000 -0.0039(19) Se3 0.014(2) 0.021(3) 0.013(2) 0.000 0.000 0.000(2) Se4 0.025(2) 0.016(3) 0.011(2) 0.000 0.000 0.008(2) Se5 0.0061(18) 0.021(2) 0.0050(17) 0.000 0.000 -0.0009(18) Se6 0.007(3) 0.031(4) 0.011(3) 0.000 0.000 -0.002(3) Rb1 0.037(3) 0.029(3) 0.047(3) 0.000 0.000 -0.009(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 Bi1 Se2 2.910(3) 5_664 ? Bi1 Se2 2.910(3) 5_665 ? Bi1 Se2 2.910(3) . ? Bi1 Se2 2.910(3) 1_556 ? Bi1 Se5 2.951(4) . ? Bi1 Se5 2.951(4) 5_665 ? Bi2 Se2 2.821(4) . ? Bi2 Se3 2.884(4) 1_556 ? Bi2 Se3 2.884(4) . ? Bi2 Se6 3.0072(18) . ? Bi2 Se5 3.036(4) 1_554 ? Bi2 Se5 3.036(4) . ? Bi2 Rb1 4.338(6) 7_576 ? Bi3 Se1 2.823(4) . ? Bi3 Se1 2.823(4) 1_554 ? Bi3 Se3 2.823(5) 1_655 ? Bi3 Se5 3.035(5) 5_664 ? Bi3 Se6 3.0510(17) 1_654 ? Bi3 Se6 3.0510(17) 1_655 ? Bi4 Se4 2.785(3) . ? Bi4 Se4 2.785(3) 1_556 ? Bi4 Se1 2.827(5) . ? Bi4 Se2 3.115(4) . ? Bi4 Se5 3.194(4) 5_664 ? Bi4 Se5 3.194(4) 5_665 ? Bi4 Rb1 4.228(6) 7_576 ? Se1 Cd3 2.823(4) 1_556 ? Se1 Bi3 2.823(4) 1_556 ? Se1 Rb1 3.511(6) 1_556 ? Se1 Rb1 3.511(6) . ? Se2 Cd1 2.910(3) 1_554 ? Se2 Bi1 2.910(3) 1_554 ? Se2 Rb1 3.377(7) 7_576 ? Se3 Cd3 2.823(5) 1_455 ? Se3 Bi3 2.823(5) 1_455 ? Se3 Bi2 2.884(4) 1_554 ? Se3 Rb1 3.783(6) 7_576 ? Se3 Rb1 3.783(6) 7_575 ? Se4 Bi4 2.785(3) 1_554 ? Se4 Rb1 3.457(7) . ? Se4 Rb1 3.775(6) 7_575 ? Se4 Rb1 3.775(6) 7_576 ? Se5 Cd3 3.035(5) 5_664 ? Se5 Bi3 3.035(5) 5_664 ? Se5 Bi2 3.036(4) 1_556 ? Se5 Bi4 3.194(4) 5_664 ? Se5 Bi4 3.194(4) 5_665 ? Se6 Bi2 3.0072(18) 5_564 ? Se6 Cd3 3.0510(17) 5_663 ? Se6 Bi3 3.0510(17) 5_663 ? Se6 Cd3 3.0510(17) 5_664 ? Se6 Bi3 3.0510(17) 5_664 ? Se6 Bi3 3.0510(17) 1_456 ? Se6 Cd3 3.0510(17) 1_456 ? Se6 Cd3 3.0510(17) 1_455 ? Se6 Bi3 3.0510(17) 1_455 ? Rb1 Se2 3.377(7) 7_675 ? Rb1 Se1 3.511(6) 1_554 ? Rb1 Se4 3.775(6) 7_676 ? Rb1 Se4 3.775(6) 7_675 ? Rb1 Se3 3.783(6) 7_675 ? Rb1 Se3 3.783(6) 7_676 ? Rb1 Rb1 4.1124(10) 1_556 ? Rb1 Rb1 4.1124(10) 1_554 ? Rb1 Bi4 4.228(6) 7_675 ? Rb1 Bi2 4.338(6) 7_675 ? 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 Se2 Bi1 Se2 89.91(13) 5_664 5_665 ? Se2 Bi1 Se2 90.09(13) 5_664 . ? Se2 Bi1 Se2 180.0 5_665 . ? Se2 Bi1 Se2 180.0 5_664 1_556 ? Se2 Bi1 Se2 90.09(13) 5_665 1_556 ? Se2 Bi1 Se2 89.91(13) . 1_556 ? Se2 Bi1 Se5 90.05(10) 5_664 . ? Se2 Bi1 Se5 90.05(10) 5_665 . ? Se2 Bi1 Se5 89.95(10) . . ? Se2 Bi1 Se5 89.95(10) 1_556 . ? Se2 Bi1 Se5 89.95(10) 5_664 5_665 ? Se2 Bi1 Se5 89.95(10) 5_665 5_665 ? Se2 Bi1 Se5 90.05(10) . 5_665 ? Se2 Bi1 Se5 90.05(10) 1_556 5_665 ? Se5 Bi1 Se5 180.00(18) . 5_665 ? Se2 Bi2 Se3 92.90(12) . 1_556 ? Se2 Bi2 Se3 92.90(12) . . ? Se3 Bi2 Se3 90.94(14) 1_556 . ? Se2 Bi2 Se6 174.22(12) . . ? Se3 Bi2 Se6 91.16(10) 1_556 . ? Se3 Bi2 Se6 91.16(10) . . ? Se2 Bi2 Se5 89.96(12) . 1_554 ? Se3 Bi2 Se5 175.92(12) 1_556 1_554 ? Se3 Bi2 Se5 91.82(9) . 1_554 ? Se6 Bi2 Se5 85.79(9) . 1_554 ? Se2 Bi2 Se5 89.96(12) . . ? Se3 Bi2 Se5 91.82(9) 1_556 . ? Se3 Bi2 Se5 175.92(12) . . ? Se6 Bi2 Se5 85.79(9) . . ? Se5 Bi2 Se5 85.27(13) 1_554 . ? Se2 Bi2 Rb1 51.10(12) . 7_576 ? Se3 Bi2 Rb1 59.17(10) 1_556 7_576 ? Se3 Bi2 Rb1 59.17(10) . 7_576 ? Se6 Bi2 Rb1 134.69(9) . 7_576 ? Se5 Bi2 Rb1 124.90(9) 1_554 7_576 ? Se5 Bi2 Rb1 124.90(9) . 7_576 ? Se1 Bi3 Se1 93.50(15) . 1_554 ? Se1 Bi3 Se3 93.26(12) . 1_655 ? Se1 Bi3 Se3 93.26(12) 1_554 1_655 ? Se1 Bi3 Se5 90.01(12) . 5_664 ? Se1 Bi3 Se5 90.01(12) 1_554 5_664 ? Se3 Bi3 Se5 175.23(15) 1_655 5_664 ? Se1 Bi3 Se6 173.52(11) . 1_654 ? Se1 Bi3 Se6 90.68(7) 1_554 1_654 ? Se3 Bi3 Se6 91.44(8) 1_655 1_654 ? Se5 Bi3 Se6 85.04(8) 5_664 1_654 ? Se1 Bi3 Se6 90.68(7) . 1_655 ? Se1 Bi3 Se6 173.52(11) 1_554 1_655 ? Se3 Bi3 Se6 91.44(8) 1_655 1_655 ? Se5 Bi3 Se6 85.04(8) 5_664 1_655 ? Se6 Bi3 Se6 84.75(6) 1_654 1_655 ? Se4 Bi4 Se4 95.19(16) . 1_556 ? Se4 Bi4 Se1 95.48(13) . . ? Se4 Bi4 Se1 95.48(13) 1_556 . ? Se4 Bi4 Se2 94.27(13) . . ? Se4 Bi4 Se2 94.27(13) 1_556 . ? Se1 Bi4 Se2 165.53(14) . . ? Se4 Bi4 Se5 92.26(9) . 5_664 ? Se4 Bi4 Se5 171.96(11) 1_556 5_664 ? Se1 Bi4 Se5 86.78(11) . 5_664 ? Se2 Bi4 Se5 82.16(11) . 5_664 ? Se4 Bi4 Se5 171.96(11) . 5_665 ? Se4 Bi4 Se5 92.26(9) 1_556 5_665 ? Se1 Bi4 Se5 86.78(11) . 5_665 ? Se2 Bi4 Se5 82.16(11) . 5_665 ? Se5 Bi4 Se5 80.14(12) 5_664 5_665 ? Se4 Bi4 Rb1 61.10(10) . 7_576 ? Se4 Bi4 Rb1 61.10(10) 1_556 7_576 ? Se1 Bi4 Rb1 142.36(13) . 7_576 ? Se2 Bi4 Rb1 52.12(12) . 7_576 ? Se5 Bi4 Rb1 120.70(9) 5_664 7_576 ? Se5 Bi4 Rb1 120.70(9) 5_665 7_576 ? Cd3 Se1 Bi3 0.00(7) 1_556 1_556 ? Cd3 Se1 Bi3 93.50(15) 1_556 . ? Bi3 Se1 Bi3 93.50(15) 1_556 . ? Cd3 Se1 Bi4 96.91(12) 1_556 . ? Bi3 Se1 Bi4 96.91(12) 1_556 . ? Bi3 Se1 Bi4 96.91(12) . . ? Cd3 Se1 Rb1 96.37(8) 1_556 1_556 ? Bi3 Se1 Rb1 96.37(8) 1_556 1_556 ? Bi3 Se1 Rb1 164.59(16) . 1_556 ? Bi4 Se1 Rb1 93.63(14) . 1_556 ? Cd3 Se1 Rb1 164.59(16) 1_556 . ? Bi3 Se1 Rb1 164.59(16) 1_556 . ? Bi3 Se1 Rb1 96.37(8) . . ? Bi4 Se1 Rb1 93.63(14) . . ? Rb1 Se1 Rb1 71.70(14) 1_556 . ? Bi2 Se2 Cd1 92.49(11) . 1_554 ? Bi2 Se2 Bi1 92.49(11) . 1_554 ? Cd1 Se2 Bi1 0.0 1_554 1_554 ? Bi2 Se2 Bi1 92.49(11) . . ? Cd1 Se2 Bi1 89.91(13) 1_554 . ? Bi1 Se2 Bi1 89.91(13) 1_554 . ? Bi2 Se2 Bi4 169.53(19) . . ? Cd1 Se2 Bi4 94.91(10) 1_554 . ? Bi1 Se2 Bi4 94.91(10) 1_554 . ? Bi1 Se2 Bi4 94.91(10) . . ? Bi2 Se2 Rb1 88.36(15) . 7_576 ? Cd1 Se2 Rb1 135.02(7) 1_554 7_576 ? Bi1 Se2 Rb1 135.02(7) 1_554 7_576 ? Bi1 Se2 Rb1 135.02(7) . 7_576 ? Bi4 Se2 Rb1 81.17(15) . 7_576 ? Cd3 Se3 Bi3 0.00(2) 1_455 1_455 ? Cd3 Se3 Bi2 91.95(12) 1_455 1_554 ? Bi3 Se3 Bi2 91.95(12) 1_455 1_554 ? Cd3 Se3 Bi2 91.95(12) 1_455 . ? Bi3 Se3 Bi2 91.95(12) 1_455 . ? Bi2 Se3 Bi2 90.94(14) 1_554 . ? Cd3 Se3 Rb1 140.08(11) 1_455 7_576 ? Bi3 Se3 Rb1 140.08(11) 1_455 7_576 ? Bi2 Se3 Rb1 126.89(16) 1_554 7_576 ? Bi2 Se3 Rb1 79.94(10) . 7_576 ? Cd3 Se3 Rb1 140.08(11) 1_455 7_575 ? Bi3 Se3 Rb1 140.08(11) 1_455 7_575 ? Bi2 Se3 Rb1 79.94(10) 1_554 7_575 ? Bi2 Se3 Rb1 126.89(16) . 7_575 ? Rb1 Se3 Rb1 65.85(12) 7_576 7_575 ? Bi4 Se4 Bi4 95.19(15) 1_554 . ? Bi4 Se4 Rb1 95.59(14) 1_554 . ? Bi4 Se4 Rb1 95.59(14) . . ? Bi4 Se4 Rb1 78.68(10) 1_554 7_575 ? Bi4 Se4 Rb1 127.45(18) . 7_575 ? Rb1 Se4 Rb1 136.79(10) . 7_575 ? Bi4 Se4 Rb1 127.45(18) 1_554 7_576 ? Bi4 Se4 Rb1 78.68(10) . 7_576 ? Rb1 Se4 Rb1 136.79(10) . 7_576 ? Rb1 Se4 Rb1 66.00(12) 7_575 7_576 ? Bi1 Se5 Cd3 177.33(19) . 5_664 ? Bi1 Se5 Bi3 177.33(19) . 5_664 ? Cd3 Se5 Bi3 0.00(8) 5_664 5_664 ? Bi1 Se5 Bi2 87.50(11) . 1_556 ? Cd3 Se5 Bi2 94.46(11) 5_664 1_556 ? Bi3 Se5 Bi2 94.46(11) 5_664 1_556 ? Bi1 Se5 Bi2 87.50(11) . . ? Cd3 Se5 Bi2 94.46(11) 5_664 . ? Bi3 Se5 Bi2 94.46(11) 5_664 . ? Bi2 Se5 Bi2 85.27(13) 1_556 . ? Bi1 Se5 Bi4 92.48(11) . 5_664 ? Cd3 Se5 Bi4 85.48(11) 5_664 5_664 ? Bi3 Se5 Bi4 85.48(11) 5_664 5_664 ? Bi2 Se5 Bi4 177.43(12) 1_556 5_664 ? Bi2 Se5 Bi4 97.29(4) . 5_664 ? Bi1 Se5 Bi4 92.48(11) . 5_665 ? Cd3 Se5 Bi4 85.48(11) 5_664 5_665 ? Bi3 Se5 Bi4 85.48(11) 5_664 5_665 ? Bi2 Se5 Bi4 97.29(4) 1_556 5_665 ? Bi2 Se5 Bi4 177.43(12) . 5_665 ? Bi4 Se5 Bi4 80.14(12) 5_664 5_665 ? Bi2 Se6 Bi2 180.00(7) 5_564 . ? Bi2 Se6 Cd3 85.29(5) 5_564 5_663 ? Bi2 Se6 Cd3 94.71(5) . 5_663 ? Bi2 Se6 Bi3 85.29(5) 5_564 5_663 ? Bi2 Se6 Bi3 94.71(5) . 5_663 ? Cd3 Se6 Bi3 0.00(6) 5_663 5_663 ? Bi2 Se6 Cd3 85.29(5) 5_564 5_664 ? Bi2 Se6 Cd3 94.71(5) . 5_664 ? Cd3 Se6 Cd3 84.75(6) 5_663 5_664 ? Bi3 Se6 Cd3 84.75(6) 5_663 5_664 ? Bi2 Se6 Bi3 85.29(5) 5_564 5_664 ? Bi2 Se6 Bi3 94.71(5) . 5_664 ? Cd3 Se6 Bi3 84.75(6) 5_663 5_664 ? Bi3 Se6 Bi3 84.75(6) 5_663 5_664 ? Cd3 Se6 Bi3 0.00(6) 5_664 5_664 ? Bi2 Se6 Bi3 94.71(5) 5_564 1_456 ? Bi2 Se6 Bi3 85.29(5) . 1_456 ? Cd3 Se6 Bi3 180.00(6) 5_663 1_456 ? Bi3 Se6 Bi3 180.00(6) 5_663 1_456 ? Cd3 Se6 Bi3 95.25(6) 5_664 1_456 ? Bi3 Se6 Bi3 95.25(6) 5_664 1_456 ? Bi2 Se6 Cd3 94.71(5) 5_564 1_456 ? Bi2 Se6 Cd3 85.29(5) . 1_456 ? Cd3 Se6 Cd3 180.00(6) 5_663 1_456 ? Bi3 Se6 Cd3 180.00(6) 5_663 1_456 ? Cd3 Se6 Cd3 95.25(6) 5_664 1_456 ? Bi3 Se6 Cd3 95.25(6) 5_664 1_456 ? Bi3 Se6 Cd3 0.00(9) 1_456 1_456 ? Bi2 Se6 Cd3 94.71(5) 5_564 1_455 ? Bi2 Se6 Cd3 85.29(5) . 1_455 ? Cd3 Se6 Cd3 95.25(6) 5_663 1_455 ? Bi3 Se6 Cd3 95.25(6) 5_663 1_455 ? Cd3 Se6 Cd3 180.00(6) 5_664 1_455 ? Bi3 Se6 Cd3 180.00(6) 5_664 1_455 ? Bi3 Se6 Cd3 84.75(6) 1_456 1_455 ? Cd3 Se6 Cd3 84.75(6) 1_456 1_455 ? Bi2 Se6 Bi3 94.71(5) 5_564 1_455 ? Bi2 Se6 Bi3 85.29(5) . 1_455 ? Cd3 Se6 Bi3 95.25(6) 5_663 1_455 ? Bi3 Se6 Bi3 95.25(6) 5_663 1_455 ? Cd3 Se6 Bi3 180.00(6) 5_664 1_455 ? Bi3 Se6 Bi3 180.00(6) 5_664 1_455 ? Bi3 Se6 Bi3 84.75(6) 1_456 1_455 ? Cd3 Se6 Bi3 84.75(6) 1_456 1_455 ? Cd3 Se6 Bi3 0.00(9) 1_455 1_455 ? Se2 Rb1 Se4 137.0(2) 7_675 . ? Se2 Rb1 Se1 136.74(12) 7_675 1_554 ? Se4 Rb1 Se1 73.18(13) . 1_554 ? Se2 Rb1 Se1 136.74(12) 7_675 . ? Se4 Rb1 Se1 73.18(13) . . ? Se1 Rb1 Se1 71.70(14) 1_554 . ? Se2 Rb1 Se4 74.28(13) 7_675 7_676 ? Se4 Rb1 Se4 137.71(11) . 7_676 ? Se1 Rb1 Se4 103.53(17) 1_554 7_676 ? Se1 Rb1 Se4 66.17(12) . 7_676 ? Se2 Rb1 Se4 74.28(13) 7_675 7_675 ? Se4 Rb1 Se4 137.71(11) . 7_675 ? Se1 Rb1 Se4 66.17(12) 1_554 7_675 ? Se1 Rb1 Se4 103.53(17) . 7_675 ? Se4 Rb1 Se4 66.00(12) 7_676 7_675 ? Se2 Rb1 Se3 70.29(13) 7_675 7_675 ? Se4 Rb1 Se3 73.85(13) . 7_675 ? Se1 Rb1 Se3 101.58(10) 1_554 7_675 ? Se1 Rb1 Se3 146.87(19) . 7_675 ? Se4 Rb1 Se3 144.56(19) 7_676 7_675 ? Se4 Rb1 Se3 102.86(10) 7_675 7_675 ? Se2 Rb1 Se3 70.29(13) 7_675 7_676 ? Se4 Rb1 Se3 73.85(13) . 7_676 ? Se1 Rb1 Se3 146.87(19) 1_554 7_676 ? Se1 Rb1 Se3 101.58(10) . 7_676 ? Se4 Rb1 Se3 102.86(10) 7_676 7_676 ? Se4 Rb1 Se3 144.56(19) 7_675 7_676 ? Se3 Rb1 Se3 65.85(12) 7_675 7_676 ? Se2 Rb1 Rb1 90.0 7_675 1_556 ? Se4 Rb1 Rb1 90.0 . 1_556 ? Se1 Rb1 Rb1 125.85(7) 1_554 1_556 ? Se1 Rb1 Rb1 54.15(7) . 1_556 ? Se4 Rb1 Rb1 57.00(6) 7_676 1_556 ? Se4 Rb1 Rb1 123.00(6) 7_675 1_556 ? Se3 Rb1 Rb1 122.93(6) 7_675 1_556 ? Se3 Rb1 Rb1 57.07(6) 7_676 1_556 ? Se2 Rb1 Rb1 90.0 7_675 1_554 ? Se4 Rb1 Rb1 90.0 . 1_554 ? Se1 Rb1 Rb1 54.15(7) 1_554 1_554 ? Se1 Rb1 Rb1 125.85(7) . 1_554 ? Se4 Rb1 Rb1 123.00(6) 7_676 1_554 ? Se4 Rb1 Rb1 57.00(6) 7_675 1_554 ? Se3 Rb1 Rb1 57.07(6) 7_675 1_554 ? Se3 Rb1 Rb1 122.93(6) 7_676 1_554 ? Rb1 Rb1 Rb1 180.0(3) 1_556 1_554 ? Se2 Rb1 Bi4 46.71(10) 7_675 7_675 ? Se4 Rb1 Bi4 176.33(18) . 7_675 ? Se1 Rb1 Bi4 103.91(14) 1_554 7_675 ? Se1 Rb1 Bi4 103.91(14) . 7_675 ? Se4 Rb1 Bi4 40.22(8) 7_676 7_675 ? Se4 Rb1 Bi4 40.22(8) 7_675 7_675 ? Se3 Rb1 Bi4 109.17(13) 7_675 7_675 ? Se3 Rb1 Bi4 109.17(13) 7_676 7_675 ? Rb1 Rb1 Bi4 90.0 1_556 7_675 ? Rb1 Rb1 Bi4 90.0 1_554 7_675 ? Se2 Rb1 Bi2 40.54(10) 7_675 7_675 ? Se4 Rb1 Bi2 96.42(14) . 7_675 ? Se1 Rb1 Bi2 141.70(9) 1_554 7_675 ? Se1 Rb1 Bi2 141.70(9) . 7_675 ? Se4 Rb1 Bi2 108.06(14) 7_676 7_675 ? Se4 Rb1 Bi2 108.06(14) 7_675 7_675 ? Se3 Rb1 Bi2 40.89(8) 7_675 7_675 ? Se3 Rb1 Bi2 40.89(8) 7_676 7_675 ? Rb1 Rb1 Bi2 90.0 1_556 7_675 ? Rb1 Rb1 Bi2 90.0 1_554 7_675 ? Bi4 Rb1 Bi2 87.26(10) 7_675 7_675 ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 3.868 _refine_diff_density_min -6.326 _refine_diff_density_rms 0.906 # Attachment 'CsCdBi3Se6.CIF' data_new _database_code_depnum_ccdc_archive 'CCDC 291024' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common CsCdBi3Se6 _chemical_melting_point ? _chemical_formula_moiety CsCdBi3Se6 _chemical_formula_sum 'Bi3 Cd Cs Se6' _chemical_formula_weight 1347.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Se Se -0.0929 2.2259 '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' Cs Cs -0.3680 2.1192 '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 Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 26.512(8) _cell_length_b 4.1192(13) _cell_length_c 12.396(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1353.7(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 10826 _cell_measurement_theta_min 1.54 _cell_measurement_theta_max 28.24 _exptl_crystal_description needle _exptl_crystal_colour black _exptl_crystal_size_max 0.278 _exptl_crystal_size_mid 0.034 _exptl_crystal_size_min 0.016 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 6.604 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2224 _exptl_absorpt_coefficient_mu 59.161 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.727570 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ; An analytical absorption correction was performed using face indexing and the program XPREP, followed by a semiempirical absorption correction based on symmetrically equivalent reflections with the program SADABS. ; _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 '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 10826 _diffrn_reflns_av_R_equivalents 0.0621 _diffrn_reflns_av_sigmaI/netI 0.0467 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 28.24 _reflns_number_total 1819 _reflns_number_gt 1223 _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^)+(0.0799P)^2^+26.0284P] 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_number_reflns 1819 _refine_ls_number_parameters 70 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0856 _refine_ls_R_factor_gt 0.0503 _refine_ls_wR_factor_ref 0.1568 _refine_ls_wR_factor_gt 0.1269 _refine_ls_goodness_of_fit_ref 1.116 _refine_ls_restrained_S_all 1.116 _refine_ls_shift/su_max 0.003 _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 0.02102(5) -0.2500 0.86147(9) 0.0173(4) Uani 0.605(5) 2 d SP . . Cd1 Cd 0.02102(5) -0.2500 0.86147(9) 0.0173(4) Uani 0.40 2 d SP . . Bi2 Bi 0.06187(4) -0.7500 0.58396(9) 0.0208(4) Uani 0.811(5) 2 d SP . . Cd2 Cd 0.06187(4) -0.7500 0.58396(9) 0.0208(4) Uani 0.19 2 d SP . . Bi3 Bi -0.10088(5) 0.2500 0.68911(10) 0.0219(5) Uani 0.595(5) 2 d SP . . Cd3 Cd -0.10088(5) 0.2500 0.68911(10) 0.0219(5) Uani 0.40 2 d SP . . Bi4 Bi -0.14382(4) -0.2500 0.96928(8) 0.0175(3) Uani 1 2 d S . . Cs1 Cs -0.21829(8) -0.2500 1.28440(16) 0.0358(5) Uani 1 2 d S . . Se1 Se -0.16766(10) 0.7500 0.7476(2) 0.0188(6) Uani 1 2 d S . . Se2 Se 0.08935(10) -0.7500 0.8049(2) 0.0194(6) Uani 1 2 d S . . Se3 Se 0.13008(11) -0.2500 0.5302(2) 0.0210(6) Uani 1 2 d S . . Se4 Se 0.05505(10) -0.2500 1.0844(2) 0.0188(6) Uani 1 2 d S . . Se5 Se -0.20884(11) 0.2500 1.0275(2) 0.0241(6) Uani 1 2 d S . . Se6 Se -0.02108(10) -0.2500 0.6400(2) 0.0225(6) Uani 1 2 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 0.0227(7) 0.0175(7) 0.0116(7) 0.000 -0.0005(5) 0.000 Cd1 0.0227(7) 0.0175(7) 0.0116(7) 0.000 -0.0005(5) 0.000 Bi2 0.0291(8) 0.0190(7) 0.0143(6) 0.000 -0.0015(5) 0.000 Cd2 0.0291(8) 0.0190(7) 0.0143(6) 0.000 -0.0015(5) 0.000 Bi3 0.0295(8) 0.0186(7) 0.0177(8) 0.000 0.0037(5) 0.000 Cd3 0.0295(8) 0.0186(7) 0.0177(8) 0.000 0.0037(5) 0.000 Bi4 0.0228(6) 0.0156(5) 0.0141(5) 0.000 0.0004(4) 0.000 Cs1 0.0292(11) 0.0432(12) 0.0350(11) 0.000 0.0070(9) 0.000 Se1 0.0242(15) 0.0182(12) 0.0141(12) 0.000 -0.0006(11) 0.000 Se2 0.0224(14) 0.0236(14) 0.0122(12) 0.000 -0.0017(10) 0.000 Se3 0.0279(16) 0.0171(13) 0.0180(14) 0.000 -0.0021(11) 0.000 Se4 0.0230(15) 0.0196(14) 0.0138(13) 0.000 -0.0001(11) 0.000 Se5 0.0269(16) 0.0228(14) 0.0226(14) 0.000 0.0029(12) 0.000 Se6 0.0263(15) 0.0260(15) 0.0152(14) 0.000 -0.0038(11) 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 Se2 2.831(2) 1_565 ? Bi1 Se2 2.831(2) . ? Bi1 Se4 2.906(3) . ? Bi1 Se4 2.960(2) 5_547 ? Bi1 Se4 2.960(2) 5_557 ? Bi1 Se6 2.964(3) . ? Bi2 Se3 2.821(2) . ? Bi2 Se3 2.821(2) 1_545 ? Bi2 Se2 2.834(3) . ? Bi2 Se6 2.979(3) 5_546 ? Bi2 Se6 3.092(2) 1_545 ? Bi2 Se6 3.092(2) . ? Bi2 Cs1 4.456(3) 5_547 ? Bi3 Se1 2.811(2) 1_545 ? Bi3 Se1 2.811(2) . ? Bi3 Se3 2.827(3) 5_556 ? Bi3 Se6 3.015(2) . ? Bi3 Se6 3.015(2) 1_565 ? Bi3 Se4 3.060(3) 5_557 ? Bi4 Se5 2.781(2) 1_545 ? Bi4 Se5 2.781(2) . ? Bi4 Se1 2.820(3) 1_545 ? Bi4 Se2 3.150(3) 5_547 ? Bi4 Se4 3.197(2) 5_557 ? Bi4 Se4 3.197(2) 5_547 ? Bi4 Cs1 4.377(2) . ? Cs1 Se5 3.579(4) 2_455 ? Cs1 Se2 3.593(4) 5_547 ? Cs1 Se1 3.687(3) 2_455 ? Cs1 Se1 3.687(3) 2_465 ? Cs1 Se5 3.801(3) 1_545 ? Cs1 Se5 3.801(3) . ? Cs1 Se3 3.872(3) 5_557 ? Cs1 Se3 3.872(3) 5_547 ? Cs1 Cs1 4.1192(13) 1_545 ? Cs1 Cs1 4.1192(13) 1_565 ? Cs1 Bi2 4.456(3) 5_547 ? Se1 Cd3 2.811(2) 1_565 ? Se1 Bi3 2.811(2) 1_565 ? Se1 Bi4 2.820(3) 1_565 ? Se1 Cs1 3.687(3) 2_454 ? Se1 Cs1 3.687(3) 2_464 ? Se2 Cd1 2.831(2) 1_545 ? Se2 Bi1 2.831(2) 1_545 ? Se2 Bi4 3.150(3) 5_547 ? Se2 Cs1 3.593(4) 5_547 ? Se3 Cd2 2.821(2) 1_565 ? Se3 Bi2 2.821(2) 1_565 ? Se3 Cd3 2.827(3) 5_556 ? Se3 Bi3 2.827(3) 5_556 ? Se3 Cs1 3.872(3) 5_557 ? Se3 Cs1 3.872(3) 5_547 ? Se4 Cd1 2.960(2) 5_547 ? Se4 Bi1 2.960(2) 5_547 ? Se4 Cd1 2.960(2) 5_557 ? Se4 Bi1 2.960(2) 5_557 ? Se4 Cd3 3.060(3) 5_557 ? Se4 Bi3 3.060(3) 5_557 ? Se4 Bi4 3.197(2) 5_557 ? Se4 Bi4 3.197(2) 5_547 ? Se5 Bi4 2.781(2) 1_565 ? Se5 Cs1 3.579(4) 2_454 ? Se5 Cs1 3.801(3) 1_565 ? Se6 Cd2 2.979(3) 5_546 ? Se6 Bi2 2.979(3) 5_546 ? Se6 Cd3 3.015(2) 1_545 ? Se6 Bi3 3.015(2) 1_545 ? Se6 Bi2 3.092(2) 1_565 ? Se6 Cd2 3.092(2) 1_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 Se2 Bi1 Se2 93.35(9) 1_565 . ? Se2 Bi1 Se4 92.12(7) 1_565 . ? Se2 Bi1 Se4 92.12(7) . . ? Se2 Bi1 Se4 176.77(7) 1_565 5_547 ? Se2 Bi1 Se4 89.20(6) . 5_547 ? Se4 Bi1 Se4 89.76(7) . 5_547 ? Se2 Bi1 Se4 89.20(6) 1_565 5_557 ? Se2 Bi1 Se4 176.77(7) . 5_557 ? Se4 Bi1 Se4 89.76(7) . 5_557 ? Se4 Bi1 Se4 88.19(8) 5_547 5_557 ? Se2 Bi1 Se6 90.65(7) 1_565 . ? Se2 Bi1 Se6 90.65(7) . . ? Se4 Bi1 Se6 175.96(9) . . ? Se4 Bi1 Se6 87.34(7) 5_547 . ? Se4 Bi1 Se6 87.34(7) 5_557 . ? Se3 Bi2 Se3 93.80(9) . 1_545 ? Se3 Bi2 Se2 93.64(7) . . ? Se3 Bi2 Se2 93.64(7) 1_545 . ? Se3 Bi2 Se6 90.72(7) . 5_546 ? Se3 Bi2 Se6 90.72(7) 1_545 5_546 ? Se2 Bi2 Se6 173.61(9) . 5_546 ? Se3 Bi2 Se6 174.52(6) . 1_545 ? Se3 Bi2 Se6 91.30(6) 1_545 1_545 ? Se2 Bi2 Se6 88.04(7) . 1_545 ? Se6 Bi2 Se6 87.20(7) 5_546 1_545 ? Se3 Bi2 Se6 91.30(6) . . ? Se3 Bi2 Se6 174.52(6) 1_545 . ? Se2 Bi2 Se6 88.04(7) . . ? Se6 Bi2 Se6 87.20(7) 5_546 . ? Se6 Bi2 Se6 83.53(8) 1_545 . ? Se3 Bi2 Cs1 59.33(6) . 5_547 ? Se3 Bi2 Cs1 59.33(6) 1_545 5_547 ? Se2 Bi2 Cs1 53.62(6) . 5_547 ? Se6 Bi2 Cs1 132.76(7) 5_546 5_547 ? Se6 Bi2 Cs1 125.42(5) 1_545 5_547 ? Se6 Bi2 Cs1 125.42(5) . 5_547 ? Se1 Bi3 Se1 94.22(9) 1_545 . ? Se1 Bi3 Se3 94.33(7) 1_545 5_556 ? Se1 Bi3 Se3 94.33(7) . 5_556 ? Se1 Bi3 Se6 89.63(6) 1_545 . ? Se1 Bi3 Se6 174.06(8) . . ? Se3 Bi3 Se6 89.89(7) 5_556 . ? Se1 Bi3 Se6 174.06(8) 1_545 1_565 ? Se1 Bi3 Se6 89.63(6) . 1_565 ? Se3 Bi3 Se6 89.89(7) 5_556 1_565 ? Se6 Bi3 Se6 86.19(8) . 1_565 ? Se1 Bi3 Se4 90.77(7) 1_545 5_557 ? Se1 Bi3 Se4 90.77(7) . 5_557 ? Se3 Bi3 Se4 172.50(9) 5_556 5_557 ? Se6 Bi3 Se4 84.65(7) . 5_557 ? Se6 Bi3 Se4 84.65(7) 1_565 5_557 ? Se5 Bi4 Se5 95.57(10) 1_545 . ? Se5 Bi4 Se1 96.53(8) 1_545 1_545 ? Se5 Bi4 Se1 96.53(8) . 1_545 ? Se5 Bi4 Se2 93.08(7) 1_545 5_547 ? Se5 Bi4 Se2 93.08(7) . 5_547 ? Se1 Bi4 Se2 165.67(8) 1_545 5_547 ? Se5 Bi4 Se4 170.85(7) 1_545 5_557 ? Se5 Bi4 Se4 91.90(6) . 5_557 ? Se1 Bi4 Se4 87.84(7) 1_545 5_557 ? Se2 Bi4 Se4 81.22(6) 5_547 5_557 ? Se5 Bi4 Se4 91.90(6) 1_545 5_547 ? Se5 Bi4 Se4 170.85(7) . 5_547 ? Se1 Bi4 Se4 87.84(7) 1_545 5_547 ? Se2 Bi4 Se4 81.22(6) 5_547 5_547 ? Se4 Bi4 Se4 80.21(7) 5_557 5_547 ? Se5 Bi4 Cs1 59.26(6) 1_545 . ? Se5 Bi4 Cs1 59.26(6) . . ? Se1 Bi4 Cs1 140.23(7) 1_545 . ? Se2 Bi4 Cs1 54.10(6) 5_547 . ? Se4 Bi4 Cs1 121.18(5) 5_557 . ? Se4 Bi4 Cs1 121.18(5) 5_547 . ? Se5 Cs1 Se2 140.60(9) 2_455 5_547 ? Se5 Cs1 Se1 70.21(6) 2_455 2_455 ? Se2 Cs1 Se1 137.91(5) 5_547 2_455 ? Se5 Cs1 Se1 70.21(6) 2_455 2_465 ? Se2 Cs1 Se1 137.91(5) 5_547 2_465 ? Se1 Cs1 Se1 67.93(6) 2_455 2_465 ? Se5 Cs1 Se5 137.81(4) 2_455 1_545 ? Se2 Cs1 Se5 71.29(6) 5_547 1_545 ? Se1 Cs1 Se5 69.37(6) 2_455 1_545 ? Se1 Cs1 Se5 104.66(7) 2_465 1_545 ? Se5 Cs1 Se5 137.81(4) 2_455 . ? Se2 Cs1 Se5 71.29(6) 5_547 . ? Se1 Cs1 Se5 104.66(7) 2_455 . ? Se1 Cs1 Se5 69.37(6) 2_465 . ? Se5 Cs1 Se5 65.62(6) 1_545 . ? Se5 Cs1 Se3 80.00(7) 2_455 5_557 ? Se2 Cs1 Se3 66.93(6) 5_547 5_557 ? Se1 Cs1 Se3 149.99(8) 2_455 5_557 ? Se1 Cs1 Se3 105.76(5) 2_465 5_557 ? Se5 Cs1 Se3 138.22(9) 1_545 5_557 ? Se5 Cs1 Se3 99.75(6) . 5_557 ? Se5 Cs1 Se3 80.00(7) 2_455 5_547 ? Se2 Cs1 Se3 66.93(6) 5_547 5_547 ? Se1 Cs1 Se3 105.76(5) 2_455 5_547 ? Se1 Cs1 Se3 149.99(8) 2_465 5_547 ? Se5 Cs1 Se3 99.75(6) 1_545 5_547 ? Se5 Cs1 Se3 138.22(9) . 5_547 ? Se3 Cs1 Se3 64.27(6) 5_557 5_547 ? Se5 Cs1 Cs1 90.0 2_455 1_545 ? Se2 Cs1 Cs1 90.0 5_547 1_545 ? Se1 Cs1 Cs1 56.04(3) 2_455 1_545 ? Se1 Cs1 Cs1 123.96(3) 2_465 1_545 ? Se5 Cs1 Cs1 57.19(3) 1_545 1_545 ? Se5 Cs1 Cs1 122.81(3) . 1_545 ? Se3 Cs1 Cs1 122.13(3) 5_557 1_545 ? Se3 Cs1 Cs1 57.87(3) 5_547 1_545 ? Se5 Cs1 Cs1 90.0 2_455 1_565 ? Se2 Cs1 Cs1 90.0 5_547 1_565 ? Se1 Cs1 Cs1 123.96(3) 2_455 1_565 ? Se1 Cs1 Cs1 56.04(3) 2_465 1_565 ? Se5 Cs1 Cs1 122.81(3) 1_545 1_565 ? Se5 Cs1 Cs1 57.19(3) . 1_565 ? Se3 Cs1 Cs1 57.87(3) 5_557 1_565 ? Se3 Cs1 Cs1 122.13(3) 5_547 1_565 ? Cs1 Cs1 Cs1 180.00(11) 1_545 1_565 ? Se5 Cs1 Bi4 174.15(8) 2_455 . ? Se2 Cs1 Bi4 45.25(5) 5_547 . ? Se1 Cs1 Bi4 105.04(6) 2_455 . ? Se1 Cs1 Bi4 105.04(6) 2_465 . ? Se5 Cs1 Bi4 38.96(4) 1_545 . ? Se5 Cs1 Bi4 38.96(4) . . ? Se3 Cs1 Bi4 104.91(6) 5_557 . ? Se3 Cs1 Bi4 104.91(6) 5_547 . ? Cs1 Cs1 Bi4 90.0 1_545 . ? Cs1 Cs1 Bi4 90.0 1_565 . ? Se5 Cs1 Bi2 101.19(7) 2_455 5_547 ? Se2 Cs1 Bi2 39.41(5) 5_547 5_547 ? Se1 Cs1 Bi2 143.95(4) 2_455 5_547 ? Se1 Cs1 Bi2 143.95(4) 2_465 5_547 ? Se5 Cs1 Bi2 104.21(6) 1_545 5_547 ? Se5 Cs1 Bi2 104.21(6) . 5_547 ? Se3 Cs1 Bi2 38.80(4) 5_557 5_547 ? Se3 Cs1 Bi2 38.80(4) 5_547 5_547 ? Cs1 Cs1 Bi2 90.0 1_545 5_547 ? Cs1 Cs1 Bi2 90.0 1_565 5_547 ? Bi4 Cs1 Bi2 84.66(4) . 5_547 ? Cd3 Se1 Bi3 0.00(6) 1_565 1_565 ? Cd3 Se1 Bi3 94.22(9) 1_565 . ? Bi3 Se1 Bi3 94.22(9) 1_565 . ? Cd3 Se1 Bi4 96.32(8) 1_565 1_565 ? Bi3 Se1 Bi4 96.32(8) 1_565 1_565 ? Bi3 Se1 Bi4 96.32(8) . 1_565 ? Cd3 Se1 Cs1 163.29(8) 1_565 2_454 ? Bi3 Se1 Cs1 163.29(8) 1_565 2_454 ? Bi3 Se1 Cs1 98.00(4) . 2_454 ? Bi4 Se1 Cs1 93.63(7) 1_565 2_454 ? Cd3 Se1 Cs1 98.00(4) 1_565 2_464 ? Bi3 Se1 Cs1 98.00(4) 1_565 2_464 ? Bi3 Se1 Cs1 163.29(8) . 2_464 ? Bi4 Se1 Cs1 93.63(7) 1_565 2_464 ? Cs1 Se1 Cs1 67.93(6) 2_454 2_464 ? Cd1 Se2 Bi1 0.00(4) 1_545 1_545 ? Cd1 Se2 Bi1 93.35(9) 1_545 . ? Bi1 Se2 Bi1 93.35(9) 1_545 . ? Cd1 Se2 Bi2 94.30(7) 1_545 . ? Bi1 Se2 Bi2 94.30(7) 1_545 . ? Bi1 Se2 Bi2 94.30(7) . . ? Cd1 Se2 Bi4 94.19(7) 1_545 5_547 ? Bi1 Se2 Bi4 94.19(7) 1_545 5_547 ? Bi1 Se2 Bi4 94.19(7) . 5_547 ? Bi2 Se2 Bi4 167.61(11) . 5_547 ? Cd1 Se2 Cs1 133.24(5) 1_545 5_547 ? Bi1 Se2 Cs1 133.24(5) 1_545 5_547 ? Bi1 Se2 Cs1 133.24(5) . 5_547 ? Bi2 Se2 Cs1 86.96(8) . 5_547 ? Bi4 Se2 Cs1 80.65(7) 5_547 5_547 ? Cd2 Se3 Bi2 0.00(6) 1_565 1_565 ? Cd2 Se3 Bi2 93.80(9) 1_565 . ? Bi2 Se3 Bi2 93.80(9) 1_565 . ? Cd2 Se3 Cd3 92.96(7) 1_565 5_556 ? Bi2 Se3 Cd3 92.96(7) 1_565 5_556 ? Bi2 Se3 Cd3 92.96(7) . 5_556 ? Cd2 Se3 Bi3 92.96(7) 1_565 5_556 ? Bi2 Se3 Bi3 92.96(7) 1_565 5_556 ? Bi2 Se3 Bi3 92.96(7) . 5_556 ? Cd3 Se3 Bi3 0.00(5) 5_556 5_556 ? Cd2 Se3 Cs1 81.87(5) 1_565 5_557 ? Bi2 Se3 Cs1 81.87(5) 1_565 5_557 ? Bi2 Se3 Cs1 129.44(9) . 5_557 ? Cd3 Se3 Cs1 137.42(7) 5_556 5_557 ? Bi3 Se3 Cs1 137.42(7) 5_556 5_557 ? Cd2 Se3 Cs1 129.44(9) 1_565 5_547 ? Bi2 Se3 Cs1 129.44(9) 1_565 5_547 ? Bi2 Se3 Cs1 81.87(5) . 5_547 ? Cd3 Se3 Cs1 137.42(7) 5_556 5_547 ? Bi3 Se3 Cs1 137.42(7) 5_556 5_547 ? Cs1 Se3 Cs1 64.27(6) 5_557 5_547 ? Bi1 Se4 Cd1 90.24(7) . 5_547 ? Bi1 Se4 Bi1 90.24(7) . 5_547 ? Cd1 Se4 Bi1 0.00(3) 5_547 5_547 ? Bi1 Se4 Cd1 90.24(7) . 5_557 ? Cd1 Se4 Cd1 88.19(8) 5_547 5_557 ? Bi1 Se4 Cd1 88.19(8) 5_547 5_557 ? Bi1 Se4 Bi1 90.24(7) . 5_557 ? Cd1 Se4 Bi1 88.19(8) 5_547 5_557 ? Bi1 Se4 Bi1 88.19(8) 5_547 5_557 ? Cd1 Se4 Bi1 0.00(5) 5_557 5_557 ? Bi1 Se4 Cd3 174.69(11) . 5_557 ? Cd1 Se4 Cd3 93.57(7) 5_547 5_557 ? Bi1 Se4 Cd3 93.57(7) 5_547 5_557 ? Cd1 Se4 Cd3 93.57(7) 5_557 5_557 ? Bi1 Se4 Cd3 93.57(7) 5_557 5_557 ? Bi1 Se4 Bi3 174.69(11) . 5_557 ? Cd1 Se4 Bi3 93.57(7) 5_547 5_557 ? Bi1 Se4 Bi3 93.57(7) 5_547 5_557 ? Cd1 Se4 Bi3 93.57(7) 5_557 5_557 ? Bi1 Se4 Bi3 93.57(7) 5_557 5_557 ? Cd3 Se4 Bi3 0.000(19) 5_557 5_557 ? Bi1 Se4 Bi4 91.76(7) . 5_557 ? Cd1 Se4 Bi4 175.56(8) 5_547 5_557 ? Bi1 Se4 Bi4 175.56(8) 5_547 5_557 ? Cd1 Se4 Bi4 95.77(3) 5_557 5_557 ? Bi1 Se4 Bi4 95.77(3) 5_557 5_557 ? Cd3 Se4 Bi4 84.18(6) 5_557 5_557 ? Bi3 Se4 Bi4 84.18(6) 5_557 5_557 ? Bi1 Se4 Bi4 91.76(7) . 5_547 ? Cd1 Se4 Bi4 95.77(3) 5_547 5_547 ? Bi1 Se4 Bi4 95.77(3) 5_547 5_547 ? Cd1 Se4 Bi4 175.56(8) 5_557 5_547 ? Bi1 Se4 Bi4 175.56(8) 5_557 5_547 ? Cd3 Se4 Bi4 84.18(6) 5_557 5_547 ? Bi3 Se4 Bi4 84.18(6) 5_557 5_547 ? Bi4 Se4 Bi4 80.21(7) 5_557 5_547 ? Bi4 Se5 Bi4 95.57(10) 1_565 . ? Bi4 Se5 Cs1 96.68(8) 1_565 2_454 ? Bi4 Se5 Cs1 96.68(8) . 2_454 ? Bi4 Se5 Cs1 81.77(5) 1_565 1_565 ? Bi4 Se5 Cs1 131.26(10) . 1_565 ? Cs1 Se5 Cs1 132.05(6) 2_454 1_565 ? Bi4 Se5 Cs1 131.26(10) 1_565 . ? Bi4 Se5 Cs1 81.77(5) . . ? Cs1 Se5 Cs1 132.05(6) 2_454 . ? Cs1 Se5 Cs1 65.62(6) 1_565 . ? Bi1 Se6 Cd2 179.16(11) . 5_546 ? Bi1 Se6 Bi2 179.16(11) . 5_546 ? Cd2 Se6 Bi2 0.00(4) 5_546 5_546 ? Bi1 Se6 Cd3 94.43(7) . 1_545 ? Cd2 Se6 Cd3 86.18(7) 5_546 1_545 ? Bi2 Se6 Cd3 86.18(7) 5_546 1_545 ? Bi1 Se6 Bi3 94.43(7) . 1_545 ? Cd2 Se6 Bi3 86.18(7) 5_546 1_545 ? Bi2 Se6 Bi3 86.18(7) 5_546 1_545 ? Cd3 Se6 Bi3 0.00(4) 1_545 1_545 ? Bi1 Se6 Bi3 94.43(7) . . ? Cd2 Se6 Bi3 86.18(7) 5_546 . ? Bi2 Se6 Bi3 86.18(7) 5_546 . ? Cd3 Se6 Bi3 86.19(8) 1_545 . ? Bi3 Se6 Bi3 86.19(8) 1_545 . ? Bi1 Se6 Bi2 86.57(7) . 1_565 ? Cd2 Se6 Bi2 92.80(7) 5_546 1_565 ? Bi2 Se6 Bi2 92.80(7) 5_546 1_565 ? Cd3 Se6 Bi2 178.28(9) 1_545 1_565 ? Bi3 Se6 Bi2 178.28(9) 1_545 1_565 ? Bi3 Se6 Bi2 95.13(3) . 1_565 ? Bi1 Se6 Cd2 86.57(7) . 1_565 ? Cd2 Se6 Cd2 92.80(7) 5_546 1_565 ? Bi2 Se6 Cd2 92.80(7) 5_546 1_565 ? Cd3 Se6 Cd2 178.28(9) 1_545 1_565 ? Bi3 Se6 Cd2 178.28(9) 1_545 1_565 ? Bi3 Se6 Cd2 95.13(3) . 1_565 ? Bi2 Se6 Cd2 0.00(5) 1_565 1_565 ? Bi1 Se6 Bi2 86.57(7) . . ? Cd2 Se6 Bi2 92.80(7) 5_546 . ? Bi2 Se6 Bi2 92.80(7) 5_546 . ? Cd3 Se6 Bi2 95.13(3) 1_545 . ? Bi3 Se6 Bi2 95.13(3) 1_545 . ? Bi3 Se6 Bi2 178.28(9) . . ? Bi2 Se6 Bi2 83.53(8) 1_565 . ? Cd2 Se6 Bi2 83.53(8) 1_565 . ? _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 28.24 _diffrn_measured_fraction_theta_full 0.952 _refine_diff_density_max 2.827 _refine_diff_density_min -3.671 _refine_diff_density_rms 0.705