# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Susan Latturner' _publ_contact_author_email LATTURNE@CHEM.FSU.EDU _publ_section_title ; Zintl phase as dopant source in the flux synthesis of Ba1-xKxFe2As2 superconductors ; loop_ _publ_author_name 'Susan Latturner' 'Josiah L Mathieu' # Attachment 'Ba34K66Fe2As22r.cif' data_data_0m _database_code_depnum_ccdc_archive 'CCDC 734670' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'As2 Ba0.34 Fe2 K0.66' _chemical_formula_weight 334.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M I4/mmm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' '-x, y, -z' 'x, -y, -z' 'y, x, -z' '-y, -x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'y+1/2, x+1/2, -z+1/2' '-y+1/2, -x+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z' 'y, -x, -z' '-y, x, -z' 'x, -y, z' '-x, y, z' '-y, -x, z' 'y, x, z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' 'x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, x+1/2, z+1/2' _cell_length_a 3.8822(4) _cell_length_b 3.8822(4) _cell_length_c 13.5396(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 204.06(4) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 46 _cell_measurement_theta_min 3.01 _cell_measurement_theta_max 20.95 _exptl_crystal_description plate _exptl_crystal_colour silver _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.005 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 5.439 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 302 _exptl_absorpt_coefficient_mu 27.008 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.730 _exptl_absorpt_correction_T_max 0.874 _exptl_absorpt_process_details 'via SADABS (Bruker, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'Bruker APEX CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 265 _diffrn_reflns_av_R_equivalents 0.0256 _diffrn_reflns_av_sigmaI/netI 0.0245 _diffrn_reflns_limit_h_min -3 _diffrn_reflns_limit_h_max 3 _diffrn_reflns_limit_k_min -3 _diffrn_reflns_limit_k_max 3 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 20.95 _reflns_number_total 46 _reflns_number_gt 45 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker APEX2' _computing_data_reduction 'Bruker APEX2' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0705P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 46 _refine_ls_number_parameters 9 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0394 _refine_ls_R_factor_gt 0.0391 _refine_ls_wR_factor_ref 0.1103 _refine_ls_wR_factor_gt 0.1102 _refine_ls_goodness_of_fit_ref 1.467 _refine_ls_restrained_S_all 1.467 _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 Ba1 Ba 0.0000 0.0000 0.0000 0.016(3) Uani 0.341(14) 16 d SP . . K1 K 0.0000 0.0000 0.0000 0.016(3) Uani 0.659(14) 16 d SP . . As2 As 0.0000 0.0000 0.3537(2) 0.0126(19) Uani 1 8 d S . . Fe3 Fe 0.0000 0.5000 0.2500 0.011(2) Uani 1 8 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 Ba1 0.012(3) 0.012(3) 0.026(4) 0.000 0.000 0.000 K1 0.012(3) 0.012(3) 0.026(4) 0.000 0.000 0.000 As2 0.006(2) 0.006(2) 0.025(3) 0.000 0.000 0.000 Fe3 0.005(2) 0.005(2) 0.023(3) 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 Ba1 As2 3.3849(18) 25 ? Ba1 As2 3.3849(18) 9_444 ? Ba1 As2 3.3849(18) 25_455 ? Ba1 As2 3.3849(18) 25_545 ? Ba1 As2 3.3849(18) 25_445 ? Ba1 As2 3.3849(18) 9_554 ? Ba1 As2 3.3849(18) 9_454 ? Ba1 As2 3.3849(18) 9_544 ? Ba1 Ba1 3.8822(4) 1_455 ? Ba1 K1 3.8822(4) 1_565 ? Ba1 Ba1 3.8822(4) 1_545 ? Ba1 K1 3.8822(4) 1_655 ? As2 Fe3 2.3960(18) 25_455 ? As2 Fe3 2.3960(18) 1_545 ? As2 Fe3 2.3960(18) 25 ? As2 Fe3 2.3960(18) . ? As2 K1 3.3849(18) 9 ? As2 Ba1 3.3849(18) 9 ? As2 Ba1 3.3849(18) 9_545 ? As2 K1 3.3849(18) 9_545 ? As2 K1 3.3849(18) 9_455 ? As2 Ba1 3.3849(18) 9_455 ? As2 K1 3.3849(18) 9_445 ? As2 Ba1 3.3849(18) 9_445 ? Fe3 As2 2.3960(18) 25_455 ? Fe3 As2 2.3960(18) 1_565 ? Fe3 As2 2.3960(18) 25 ? Fe3 Fe3 2.7451(3) 25_565 ? Fe3 Fe3 2.7451(3) 25_455 ? Fe3 Fe3 2.7451(3) 25_465 ? Fe3 Fe3 2.7451(3) 25 ? Fe3 Ba1 3.9020(3) 9 ? Fe3 K1 3.9020(3) 9 ? 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 As2 Ba1 As2 180.00(8) 25 9_444 ? As2 Ba1 As2 69.98(4) 25 25_455 ? As2 Ba1 As2 110.02(4) 9_444 25_455 ? As2 Ba1 As2 69.98(4) 25 25_545 ? As2 Ba1 As2 110.02(4) 9_444 25_545 ? As2 Ba1 As2 108.39(8) 25_455 25_545 ? As2 Ba1 As2 108.39(8) 25 25_445 ? As2 Ba1 As2 71.61(8) 9_444 25_445 ? As2 Ba1 As2 69.98(4) 25_455 25_445 ? As2 Ba1 As2 69.98(4) 25_545 25_445 ? As2 Ba1 As2 71.61(8) 25 9_554 ? As2 Ba1 As2 108.39(8) 9_444 9_554 ? As2 Ba1 As2 110.02(4) 25_455 9_554 ? As2 Ba1 As2 110.02(4) 25_545 9_554 ? As2 Ba1 As2 180.00(8) 25_445 9_554 ? As2 Ba1 As2 110.02(4) 25 9_454 ? As2 Ba1 As2 69.98(4) 9_444 9_454 ? As2 Ba1 As2 71.61(8) 25_455 9_454 ? As2 Ba1 As2 180.00(8) 25_545 9_454 ? As2 Ba1 As2 110.02(4) 25_445 9_454 ? As2 Ba1 As2 69.98(4) 9_554 9_454 ? As2 Ba1 As2 110.02(4) 25 9_544 ? As2 Ba1 As2 69.98(4) 9_444 9_544 ? As2 Ba1 As2 180.00(8) 25_455 9_544 ? As2 Ba1 As2 71.61(8) 25_545 9_544 ? As2 Ba1 As2 110.02(4) 25_445 9_544 ? As2 Ba1 As2 69.98(4) 9_554 9_544 ? As2 Ba1 As2 108.39(8) 9_454 9_544 ? As2 Ba1 Ba1 124.99(2) 25 1_455 ? As2 Ba1 Ba1 55.01(2) 9_444 1_455 ? As2 Ba1 Ba1 55.01(2) 25_455 1_455 ? As2 Ba1 Ba1 124.99(2) 25_545 1_455 ? As2 Ba1 Ba1 55.01(2) 25_445 1_455 ? As2 Ba1 Ba1 124.99(2) 9_554 1_455 ? As2 Ba1 Ba1 55.01(2) 9_454 1_455 ? As2 Ba1 Ba1 124.99(2) 9_544 1_455 ? As2 Ba1 K1 55.01(2) 25 1_565 ? As2 Ba1 K1 124.99(2) 9_444 1_565 ? As2 Ba1 K1 55.01(2) 25_455 1_565 ? As2 Ba1 K1 124.99(2) 25_545 1_565 ? As2 Ba1 K1 124.99(2) 25_445 1_565 ? As2 Ba1 K1 55.01(2) 9_554 1_565 ? As2 Ba1 K1 55.01(2) 9_454 1_565 ? As2 Ba1 K1 124.99(2) 9_544 1_565 ? Ba1 Ba1 K1 90.0 1_455 1_565 ? As2 Ba1 Ba1 124.99(2) 25 1_545 ? As2 Ba1 Ba1 55.01(2) 9_444 1_545 ? As2 Ba1 Ba1 124.99(2) 25_455 1_545 ? As2 Ba1 Ba1 55.01(2) 25_545 1_545 ? As2 Ba1 Ba1 55.01(2) 25_445 1_545 ? As2 Ba1 Ba1 124.99(2) 9_554 1_545 ? As2 Ba1 Ba1 124.99(2) 9_454 1_545 ? As2 Ba1 Ba1 55.01(2) 9_544 1_545 ? Ba1 Ba1 Ba1 90.0 1_455 1_545 ? K1 Ba1 Ba1 180.0 1_565 1_545 ? As2 Ba1 K1 55.01(2) 25 1_655 ? As2 Ba1 K1 124.99(2) 9_444 1_655 ? As2 Ba1 K1 124.99(2) 25_455 1_655 ? As2 Ba1 K1 55.01(2) 25_545 1_655 ? As2 Ba1 K1 124.99(2) 25_445 1_655 ? As2 Ba1 K1 55.01(2) 9_554 1_655 ? As2 Ba1 K1 124.99(2) 9_454 1_655 ? As2 Ba1 K1 55.01(2) 9_544 1_655 ? Ba1 Ba1 K1 180.0 1_455 1_655 ? K1 Ba1 K1 90.0 1_565 1_655 ? Ba1 Ba1 K1 90.0 1_545 1_655 ? Fe3 As2 Fe3 69.90(6) 25_455 1_545 ? Fe3 As2 Fe3 108.22(12) 25_455 25 ? Fe3 As2 Fe3 69.90(6) 1_545 25 ? Fe3 As2 Fe3 69.90(6) 25_455 . ? Fe3 As2 Fe3 108.22(12) 1_545 . ? Fe3 As2 Fe3 69.90(6) 25 . ? Fe3 As2 K1 143.858(5) 25_455 9 ? Fe3 As2 K1 143.858(5) 1_545 9 ? Fe3 As2 K1 83.014(16) 25 9 ? Fe3 As2 K1 83.014(16) . 9 ? Fe3 As2 Ba1 143.858(5) 25_455 9 ? Fe3 As2 Ba1 143.858(5) 1_545 9 ? Fe3 As2 Ba1 83.014(16) 25 9 ? Fe3 As2 Ba1 83.014(16) . 9 ? K1 As2 Ba1 0.0 9 9 ? Fe3 As2 Ba1 143.858(5) 25_455 9_545 ? Fe3 As2 Ba1 83.014(16) 1_545 9_545 ? Fe3 As2 Ba1 83.014(16) 25 9_545 ? Fe3 As2 Ba1 143.858(4) . 9_545 ? K1 As2 Ba1 69.98(4) 9 9_545 ? Ba1 As2 Ba1 69.98(4) 9 9_545 ? Fe3 As2 K1 143.858(5) 25_455 9_545 ? Fe3 As2 K1 83.014(16) 1_545 9_545 ? Fe3 As2 K1 83.014(16) 25 9_545 ? Fe3 As2 K1 143.858(4) . 9_545 ? K1 As2 K1 69.98(4) 9 9_545 ? Ba1 As2 K1 69.98(4) 9 9_545 ? Ba1 As2 K1 0.0 9_545 9_545 ? Fe3 As2 K1 83.014(16) 25_455 9_455 ? Fe3 As2 K1 143.858(5) 1_545 9_455 ? Fe3 As2 K1 143.858(4) 25 9_455 ? Fe3 As2 K1 83.014(16) . 9_455 ? K1 As2 K1 69.98(4) 9 9_455 ? Ba1 As2 K1 69.98(4) 9 9_455 ? Ba1 As2 K1 108.39(8) 9_545 9_455 ? K1 As2 K1 108.39(8) 9_545 9_455 ? Fe3 As2 Ba1 83.014(16) 25_455 9_455 ? Fe3 As2 Ba1 143.858(5) 1_545 9_455 ? Fe3 As2 Ba1 143.858(4) 25 9_455 ? Fe3 As2 Ba1 83.014(16) . 9_455 ? K1 As2 Ba1 69.98(4) 9 9_455 ? Ba1 As2 Ba1 69.98(4) 9 9_455 ? Ba1 As2 Ba1 108.39(8) 9_545 9_455 ? K1 As2 Ba1 108.39(8) 9_545 9_455 ? K1 As2 Ba1 0.0 9_455 9_455 ? Fe3 As2 K1 83.014(16) 25_455 9_445 ? Fe3 As2 K1 83.014(16) 1_545 9_445 ? Fe3 As2 K1 143.858(5) 25 9_445 ? Fe3 As2 K1 143.858(5) . 9_445 ? K1 As2 K1 108.39(8) 9 9_445 ? Ba1 As2 K1 108.39(8) 9 9_445 ? Ba1 As2 K1 69.98(4) 9_545 9_445 ? K1 As2 K1 69.98(4) 9_545 9_445 ? K1 As2 K1 69.98(4) 9_455 9_445 ? Ba1 As2 K1 69.98(4) 9_455 9_445 ? Fe3 As2 Ba1 83.014(16) 25_455 9_445 ? Fe3 As2 Ba1 83.014(16) 1_545 9_445 ? Fe3 As2 Ba1 143.858(5) 25 9_445 ? Fe3 As2 Ba1 143.858(5) . 9_445 ? K1 As2 Ba1 108.39(8) 9 9_445 ? Ba1 As2 Ba1 108.39(8) 9 9_445 ? Ba1 As2 Ba1 69.98(4) 9_545 9_445 ? K1 As2 Ba1 69.98(4) 9_545 9_445 ? K1 As2 Ba1 69.98(4) 9_455 9_445 ? Ba1 As2 Ba1 69.98(4) 9_455 9_445 ? K1 As2 Ba1 0.0 9_445 9_445 ? As2 Fe3 As2 110.10(6) . 25_455 ? As2 Fe3 As2 108.22(12) . 1_565 ? As2 Fe3 As2 110.10(6) 25_455 1_565 ? As2 Fe3 As2 110.10(6) . 25 ? As2 Fe3 As2 108.22(12) 25_455 25 ? As2 Fe3 As2 110.10(6) 1_565 25 ? As2 Fe3 Fe3 124.95(3) . 25_565 ? As2 Fe3 Fe3 124.95(3) 25_455 25_565 ? As2 Fe3 Fe3 55.05(3) 1_565 25_565 ? As2 Fe3 Fe3 55.05(3) 25 25_565 ? As2 Fe3 Fe3 55.05(3) . 25_455 ? As2 Fe3 Fe3 55.05(3) 25_455 25_455 ? As2 Fe3 Fe3 124.95(3) 1_565 25_455 ? As2 Fe3 Fe3 124.95(3) 25 25_455 ? Fe3 Fe3 Fe3 180.0 25_565 25_455 ? As2 Fe3 Fe3 124.95(3) . 25_465 ? As2 Fe3 Fe3 55.05(3) 25_455 25_465 ? As2 Fe3 Fe3 55.05(3) 1_565 25_465 ? As2 Fe3 Fe3 124.95(3) 25 25_465 ? Fe3 Fe3 Fe3 90.0 25_565 25_465 ? Fe3 Fe3 Fe3 90.0 25_455 25_465 ? As2 Fe3 Fe3 55.05(3) . 25 ? As2 Fe3 Fe3 124.95(3) 25_455 25 ? As2 Fe3 Fe3 124.95(3) 1_565 25 ? As2 Fe3 Fe3 55.05(3) 25 25 ? Fe3 Fe3 Fe3 90.0 25_565 25 ? Fe3 Fe3 Fe3 90.0 25_455 25 ? Fe3 Fe3 Fe3 180.0 25_465 25 ? As2 Fe3 Ba1 59.43(5) . 9 ? As2 Fe3 Ba1 155.72(6) 25_455 9 ? As2 Fe3 Ba1 59.43(5) 1_565 9 ? As2 Fe3 Ba1 96.06(6) 25 9 ? Fe3 Fe3 Ba1 69.405(2) 25_565 9 ? Fe3 Fe3 Ba1 110.595(2) 25_455 9 ? Fe3 Fe3 Ba1 110.595(2) 25_465 9 ? Fe3 Fe3 Ba1 69.405(3) 25 9 ? As2 Fe3 K1 59.43(5) . 9 ? As2 Fe3 K1 155.72(6) 25_455 9 ? As2 Fe3 K1 59.43(5) 1_565 9 ? As2 Fe3 K1 96.06(6) 25 9 ? Fe3 Fe3 K1 69.405(2) 25_565 9 ? Fe3 Fe3 K1 110.595(2) 25_455 9 ? Fe3 Fe3 K1 110.595(2) 25_465 9 ? Fe3 Fe3 K1 69.405(3) 25 9 ? Ba1 Fe3 K1 0.0 9 9 ? As2 Fe3 Ba1 96.06(6) . . ? As2 Fe3 Ba1 59.43(5) 25_455 . ? As2 Fe3 Ba1 155.72(6) 1_565 . ? As2 Fe3 Ba1 59.43(5) 25 . ? Fe3 Fe3 Ba1 110.595(2) 25_565 . ? Fe3 Fe3 Ba1 69.405(2) 25_455 . ? Fe3 Fe3 Ba1 110.595(2) 25_465 . ? Fe3 Fe3 Ba1 69.405(3) 25 . ? Ba1 Fe3 Ba1 138.810(5) 9 . ? K1 Fe3 Ba1 138.810(5) 9 . ? _diffrn_measured_fraction_theta_max 0.939 _diffrn_reflns_theta_full 20.95 _diffrn_measured_fraction_theta_full 0.939 _refine_diff_density_max 0.721 _refine_diff_density_min -0.975 _refine_diff_density_rms 0.265 # Attachment 'Ba54K43Sn03Fe2As2r.cif' data_data_0m2 _database_code_depnum_ccdc_archive 'CCDC 734671' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'As2 Ba0.50 Fe2 K0.40 Sn0.10' _chemical_formula_weight 357.72 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M I4/mmm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' '-x, y, -z' 'x, -y, -z' 'y, x, -z' '-y, -x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'y+1/2, x+1/2, -z+1/2' '-y+1/2, -x+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z' 'y, -x, -z' '-y, x, -z' 'x, -y, z' '-x, y, z' '-y, -x, z' 'y, x, z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' 'x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, x+1/2, z+1/2' _cell_length_a 3.9021(5) _cell_length_b 3.9021(5) _cell_length_c 13.3538(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 203.33(5) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 99 _cell_measurement_theta_min 3.05 _cell_measurement_theta_max 28.49 _exptl_crystal_description plate _exptl_crystal_colour silver _exptl_crystal_size_max 0.02 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.005 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 5.821 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 317 _exptl_absorpt_coefficient_mu 28.797 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.715 _exptl_absorpt_correction_T_max 0.866 _exptl_absorpt_process_details 'via SADABS (Bruker, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'Bruker APEX CCD area detector ' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 547 _diffrn_reflns_av_R_equivalents 0.0426 _diffrn_reflns_av_sigmaI/netI 0.0347 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -4 _diffrn_reflns_limit_k_max 3 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 28.49 _reflns_number_total 99 _reflns_number_gt 96 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX CCD area detector' _computing_cell_refinement 'Bruker APEX CCD area detector' _computing_data_reduction 'Bruker APEX CCD area detector' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0664P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 99 _refine_ls_number_parameters 12 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0380 _refine_ls_R_factor_gt 0.0378 _refine_ls_wR_factor_ref 0.0910 _refine_ls_wR_factor_gt 0.0908 _refine_ls_goodness_of_fit_ref 1.130 _refine_ls_restrained_S_all 1.124 _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 Ba1 Ba 0.0000 0.0000 0.0000 0.0148(7) Uani 0.546(8) 16 d SP . . K1 K 0.0000 0.0000 0.0000 0.0148(7) Uani 0.425(9) 16 d SP . . As2 As 0.0000 0.0000 0.35419(10) 0.0117(6) Uani 1 8 d S . . Fe3 Fe 0.0000 0.5000 0.2500 0.0106(6) Uani 1 8 d S . . Sn1 Sn 0.0000 0.0000 0.097(5) 0.0148(7) Uani 0.014(3) 8 d SP . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ba1 0.0153(8) 0.0153(8) 0.0140(11) 0.000 0.000 0.000 K1 0.0153(8) 0.0153(8) 0.0140(11) 0.000 0.000 0.000 As2 0.0100(6) 0.0100(6) 0.0151(9) 0.000 0.000 0.000 Fe3 0.0082(7) 0.0082(7) 0.0153(11) 0.000 0.000 0.000 Sn1 0.0153(8) 0.0153(8) 0.0140(11) 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 Ba1 Sn1 1.29(6) 17 ? Ba1 Sn1 1.29(6) . ? Ba1 As2 3.3771(9) 25 ? Ba1 As2 3.3771(9) 9_444 ? Ba1 As2 3.3771(9) 25_455 ? Ba1 As2 3.3771(9) 25_545 ? Ba1 As2 3.3771(9) 25_445 ? Ba1 As2 3.3771(9) 9_554 ? Ba1 As2 3.3771(9) 9_454 ? Ba1 As2 3.3771(9) 9_544 ? Ba1 Fe3 3.8668(4) . ? Ba1 Fe3 3.8668(4) 25 ? As2 Fe3 2.3963(8) 25_455 ? As2 Fe3 2.3963(8) 1_545 ? As2 Fe3 2.3963(8) 25 ? As2 Fe3 2.3963(8) . ? As2 Sn1 2.837(15) 25 ? As2 Sn1 2.837(15) 25_445 ? As2 Sn1 2.837(15) 25_455 ? As2 Sn1 2.837(15) 25_545 ? As2 Ba1 3.3771(9) 9 ? As2 K1 3.3771(9) 9 ? As2 Ba1 3.3771(9) 9_445 ? As2 Ba1 3.3771(9) 9_455 ? Fe3 As2 2.3963(8) 25_455 ? Fe3 As2 2.3963(8) 1_565 ? Fe3 As2 2.3963(8) 25 ? Fe3 Fe3 2.7592(4) 25_565 ? Fe3 Fe3 2.7592(4) 25_455 ? Fe3 Fe3 2.7592(4) 25_465 ? Fe3 Fe3 2.7592(4) 25 ? Fe3 Sn1 2.83(5) . ? Fe3 Sn1 2.83(5) 25 ? Fe3 Sn1 2.83(5) 25_455 ? Fe3 Sn1 2.83(5) 1_565 ? Sn1 Sn1 2.58(13) 17 ? Sn1 Fe3 2.83(5) 25 ? Sn1 Fe3 2.83(5) 25_455 ? Sn1 Fe3 2.83(5) 1_545 ? Sn1 As2 2.837(15) 25 ? Sn1 As2 2.837(15) 25_445 ? Sn1 As2 2.837(15) 25_545 ? Sn1 As2 2.837(15) 25_455 ? Sn1 K1 4.11(2) 1_545 ? 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 Sn1 Ba1 Sn1 180.000(1) 17 . ? Sn1 Ba1 As2 125.21(2) 17 25 ? Sn1 Ba1 As2 54.79(2) . 25 ? Sn1 Ba1 As2 54.79(2) 17 9_444 ? Sn1 Ba1 As2 125.21(2) . 9_444 ? As2 Ba1 As2 180.00(4) 25 9_444 ? Sn1 Ba1 As2 125.21(2) 17 25_455 ? Sn1 Ba1 As2 54.79(2) . 25_455 ? As2 Ba1 As2 70.58(2) 25 25_455 ? As2 Ba1 As2 109.42(2) 9_444 25_455 ? Sn1 Ba1 As2 125.21(2) 17 25_545 ? Sn1 Ba1 As2 54.79(2) . 25_545 ? As2 Ba1 As2 70.58(2) 25 25_545 ? As2 Ba1 As2 109.42(2) 9_444 25_545 ? As2 Ba1 As2 109.58(4) 25_455 25_545 ? Sn1 Ba1 As2 125.21(2) 17 25_445 ? Sn1 Ba1 As2 54.79(2) . 25_445 ? As2 Ba1 As2 109.58(4) 25 25_445 ? As2 Ba1 As2 70.42(4) 9_444 25_445 ? As2 Ba1 As2 70.58(2) 25_455 25_445 ? As2 Ba1 As2 70.58(2) 25_545 25_445 ? Sn1 Ba1 As2 54.79(2) 17 9_554 ? Sn1 Ba1 As2 125.21(2) . 9_554 ? As2 Ba1 As2 70.42(4) 25 9_554 ? As2 Ba1 As2 109.58(4) 9_444 9_554 ? As2 Ba1 As2 109.42(2) 25_455 9_554 ? As2 Ba1 As2 109.42(2) 25_545 9_554 ? As2 Ba1 As2 180.0 25_445 9_554 ? Sn1 Ba1 As2 54.79(2) 17 9_454 ? Sn1 Ba1 As2 125.21(2) . 9_454 ? As2 Ba1 As2 109.42(2) 25 9_454 ? As2 Ba1 As2 70.58(2) 9_444 9_454 ? As2 Ba1 As2 70.42(4) 25_455 9_454 ? As2 Ba1 As2 180.0 25_545 9_454 ? As2 Ba1 As2 109.42(2) 25_445 9_454 ? As2 Ba1 As2 70.58(2) 9_554 9_454 ? Sn1 Ba1 As2 54.79(2) 17 9_544 ? Sn1 Ba1 As2 125.21(2) . 9_544 ? As2 Ba1 As2 109.42(2) 25 9_544 ? As2 Ba1 As2 70.58(2) 9_444 9_544 ? As2 Ba1 As2 180.0 25_455 9_544 ? As2 Ba1 As2 70.42(4) 25_545 9_544 ? As2 Ba1 As2 109.42(2) 25_445 9_544 ? As2 Ba1 As2 70.58(2) 9_554 9_544 ? As2 Ba1 As2 109.58(4) 9_454 9_544 ? Sn1 Ba1 Fe3 149.697(5) 17 . ? Sn1 Ba1 Fe3 30.303(5) . . ? As2 Ba1 Fe3 37.879(16) 25 . ? As2 Ba1 Fe3 142.121(16) 9_444 . ? As2 Ba1 Fe3 37.879(16) 25_455 . ? As2 Ba1 Fe3 78.095(19) 25_545 . ? As2 Ba1 Fe3 78.09(2) 25_445 . ? As2 Ba1 Fe3 101.91(2) 9_554 . ? As2 Ba1 Fe3 101.905(19) 9_454 . ? As2 Ba1 Fe3 142.121(16) 9_544 . ? Sn1 Ba1 Fe3 149.697(5) 17 25 ? Sn1 Ba1 Fe3 30.303(5) . 25 ? As2 Ba1 Fe3 37.879(16) 25 25 ? As2 Ba1 Fe3 142.121(16) 9_444 25 ? As2 Ba1 Fe3 78.095(19) 25_455 25 ? As2 Ba1 Fe3 37.879(16) 25_545 25 ? As2 Ba1 Fe3 78.09(2) 25_445 25 ? As2 Ba1 Fe3 101.91(2) 9_554 25 ? As2 Ba1 Fe3 142.121(16) 9_454 25 ? As2 Ba1 Fe3 101.905(19) 9_544 25 ? Fe3 Ba1 Fe3 41.806(6) . 25 ? Fe3 As2 Fe3 70.30(3) 25_455 1_545 ? Fe3 As2 Fe3 109.01(5) 25_455 25 ? Fe3 As2 Fe3 70.30(3) 1_545 25 ? Fe3 As2 Fe3 70.30(3) 25_455 . ? Fe3 As2 Fe3 109.01(5) 1_545 . ? Fe3 As2 Fe3 70.30(3) 25 . ? Fe3 As2 Sn1 134.0(8) 25_455 25 ? Fe3 As2 Sn1 134.0(8) 1_545 25 ? Fe3 As2 Sn1 64.8(10) 25 25 ? Fe3 As2 Sn1 64.8(10) . 25 ? Fe3 As2 Sn1 64.8(10) 25_455 25_445 ? Fe3 As2 Sn1 64.8(10) 1_545 25_445 ? Fe3 As2 Sn1 134.0(8) 25 25_445 ? Fe3 As2 Sn1 134.0(8) . 25_445 ? Sn1 As2 Sn1 153(3) 25 25_445 ? Fe3 As2 Sn1 64.8(10) 25_455 25_455 ? Fe3 As2 Sn1 134.0(8) 1_545 25_455 ? Fe3 As2 Sn1 134.0(8) 25 25_455 ? Fe3 As2 Sn1 64.8(10) . 25_455 ? Sn1 As2 Sn1 86.9(6) 25 25_455 ? Sn1 As2 Sn1 86.9(6) 25_445 25_455 ? Fe3 As2 Sn1 134.0(8) 25_455 25_545 ? Fe3 As2 Sn1 64.8(10) 1_545 25_545 ? Fe3 As2 Sn1 64.8(10) 25 25_545 ? Fe3 As2 Sn1 134.0(8) . 25_545 ? Sn1 As2 Sn1 86.9(6) 25 25_545 ? Sn1 As2 Sn1 86.9(6) 25_445 25_545 ? Sn1 As2 Sn1 153(3) 25_455 25_545 ? Fe3 As2 Ba1 143.625(3) 25_455 9 ? Fe3 As2 Ba1 143.625(3) 1_545 9 ? Fe3 As2 Ba1 82.205(10) 25 9 ? Fe3 As2 Ba1 82.205(10) . 9 ? Sn1 As2 Ba1 21.8(13) 25 9 ? Sn1 As2 Ba1 131.4(13) 25_445 9 ? Sn1 As2 Ba1 82.3(7) 25_455 9 ? Sn1 As2 Ba1 82.3(7) 25_545 9 ? Fe3 As2 K1 143.625(3) 25_455 9 ? Fe3 As2 K1 143.625(3) 1_545 9 ? Fe3 As2 K1 82.205(10) 25 9 ? Fe3 As2 K1 82.205(10) . 9 ? Sn1 As2 K1 21.8(13) 25 9 ? Sn1 As2 K1 131.4(13) 25_445 9 ? Sn1 As2 K1 82.3(7) 25_455 9 ? Sn1 As2 K1 82.3(7) 25_545 9 ? Ba1 As2 K1 0.0 9 9 ? Fe3 As2 Ba1 82.205(10) 25_455 9_445 ? Fe3 As2 Ba1 82.205(10) 1_545 9_445 ? Fe3 As2 Ba1 143.625(3) 25 9_445 ? Fe3 As2 Ba1 143.625(3) . 9_445 ? Sn1 As2 Ba1 131.4(13) 25 9_445 ? Sn1 As2 Ba1 21.8(13) 25_445 9_445 ? Sn1 As2 Ba1 82.3(7) 25_455 9_445 ? Sn1 As2 Ba1 82.3(7) 25_545 9_445 ? Ba1 As2 Ba1 109.58(4) 9 9_445 ? K1 As2 Ba1 109.58(4) 9 9_445 ? Fe3 As2 Ba1 82.205(10) 25_455 9_455 ? Fe3 As2 Ba1 143.625(3) 1_545 9_455 ? Fe3 As2 Ba1 143.625(3) 25 9_455 ? Fe3 As2 Ba1 82.205(10) . 9_455 ? Sn1 As2 Ba1 82.3(7) 25 9_455 ? Sn1 As2 Ba1 82.3(7) 25_445 9_455 ? Sn1 As2 Ba1 21.8(13) 25_455 9_455 ? Sn1 As2 Ba1 131.4(13) 25_545 9_455 ? Ba1 As2 Ba1 70.58(2) 9 9_455 ? K1 As2 Ba1 70.58(2) 9 9_455 ? Ba1 As2 Ba1 70.58(2) 9_445 9_455 ? As2 Fe3 As2 109.70(3) 25_455 1_565 ? As2 Fe3 As2 109.01(5) 25_455 25 ? As2 Fe3 As2 109.70(3) 1_565 25 ? As2 Fe3 As2 109.70(3) 25_455 . ? As2 Fe3 As2 109.01(5) 1_565 . ? As2 Fe3 As2 109.70(3) 25 . ? As2 Fe3 Fe3 125.150(14) 25_455 25_565 ? As2 Fe3 Fe3 54.850(14) 1_565 25_565 ? As2 Fe3 Fe3 54.850(14) 25 25_565 ? As2 Fe3 Fe3 125.150(14) . 25_565 ? As2 Fe3 Fe3 54.850(14) 25_455 25_455 ? As2 Fe3 Fe3 125.150(14) 1_565 25_455 ? As2 Fe3 Fe3 125.150(14) 25 25_455 ? As2 Fe3 Fe3 54.850(14) . 25_455 ? Fe3 Fe3 Fe3 180.0 25_565 25_455 ? As2 Fe3 Fe3 54.850(14) 25_455 25_465 ? As2 Fe3 Fe3 54.850(14) 1_565 25_465 ? As2 Fe3 Fe3 125.150(14) 25 25_465 ? As2 Fe3 Fe3 125.150(14) . 25_465 ? Fe3 Fe3 Fe3 90.0 25_565 25_465 ? Fe3 Fe3 Fe3 90.0 25_455 25_465 ? As2 Fe3 Fe3 125.150(14) 25_455 25 ? As2 Fe3 Fe3 125.150(14) 1_565 25 ? As2 Fe3 Fe3 54.850(14) 25 25 ? As2 Fe3 Fe3 54.850(14) . 25 ? Fe3 Fe3 Fe3 90.0 25_565 25 ? Fe3 Fe3 Fe3 90.0 25_455 25 ? Fe3 Fe3 Fe3 180.0 25_465 25 ? As2 Fe3 Sn1 65.1(4) 25_455 . ? As2 Fe3 Sn1 169.1(9) 1_565 . ? As2 Fe3 Sn1 65.1(4) 25 . ? As2 Fe3 Sn1 81.9(9) . . ? Fe3 Fe3 Sn1 119.2(5) 25_565 . ? Fe3 Fe3 Sn1 60.8(5) 25_455 . ? Fe3 Fe3 Sn1 119.2(5) 25_465 . ? Fe3 Fe3 Sn1 60.8(5) 25 . ? As2 Fe3 Sn1 169.1(9) 25_455 25 ? As2 Fe3 Sn1 65.1(4) 1_565 25 ? As2 Fe3 Sn1 81.9(9) 25 25 ? As2 Fe3 Sn1 65.1(4) . 25 ? Fe3 Fe3 Sn1 60.8(5) 25_565 25 ? Fe3 Fe3 Sn1 119.2(5) 25_455 25 ? Fe3 Fe3 Sn1 119.2(5) 25_465 25 ? Fe3 Fe3 Sn1 60.8(5) 25 25 ? Sn1 Fe3 Sn1 121.6(10) . 25 ? As2 Fe3 Sn1 81.9(9) 25_455 25_455 ? As2 Fe3 Sn1 65.1(4) 1_565 25_455 ? As2 Fe3 Sn1 169.1(9) 25 25_455 ? As2 Fe3 Sn1 65.1(4) . 25_455 ? Fe3 Fe3 Sn1 119.2(5) 25_565 25_455 ? Fe3 Fe3 Sn1 60.8(5) 25_455 25_455 ? Fe3 Fe3 Sn1 60.8(5) 25_465 25_455 ? Fe3 Fe3 Sn1 119.2(5) 25 25_455 ? Sn1 Fe3 Sn1 121.6(11) . 25_455 ? Sn1 Fe3 Sn1 87.2(18) 25 25_455 ? As2 Fe3 Sn1 65.1(4) 25_455 1_565 ? As2 Fe3 Sn1 81.9(9) 1_565 1_565 ? As2 Fe3 Sn1 65.1(4) 25 1_565 ? As2 Fe3 Sn1 169.1(9) . 1_565 ? Fe3 Fe3 Sn1 60.8(5) 25_565 1_565 ? Fe3 Fe3 Sn1 119.2(5) 25_455 1_565 ? Fe3 Fe3 Sn1 60.8(5) 25_465 1_565 ? Fe3 Fe3 Sn1 119.2(5) 25 1_565 ? Sn1 Fe3 Sn1 87.2(18) . 1_565 ? Sn1 Fe3 Sn1 121.6(11) 25 1_565 ? Sn1 Fe3 Sn1 121.6(10) 25_455 1_565 ? Ba1 Sn1 Sn1 0.000(1) . 17 ? Ba1 Sn1 Fe3 136.4(9) . . ? Sn1 Sn1 Fe3 136.4(9) 17 . ? Ba1 Sn1 Fe3 136.4(9) . 25 ? Sn1 Sn1 Fe3 136.4(9) 17 25 ? Fe3 Sn1 Fe3 58.4(10) . 25 ? Ba1 Sn1 Fe3 136.4(9) . 25_455 ? Sn1 Sn1 Fe3 136.4(9) 17 25_455 ? Fe3 Sn1 Fe3 58.4(10) . 25_455 ? Fe3 Sn1 Fe3 87.2(18) 25 25_455 ? Ba1 Sn1 Fe3 136.4(9) . 1_545 ? Sn1 Sn1 Fe3 136.4(9) 17 1_545 ? Fe3 Sn1 Fe3 87.2(18) . 1_545 ? Fe3 Sn1 Fe3 58.4(10) 25 1_545 ? Fe3 Sn1 Fe3 58.4(10) 25_455 1_545 ? Ba1 Sn1 As2 103.4(13) . 25 ? Sn1 Sn1 As2 103.4(13) 17 25 ? Fe3 Sn1 As2 50.0(6) . 25 ? Fe3 Sn1 As2 50.0(6) 25 25 ? Fe3 Sn1 As2 107.8(17) 25_455 25 ? Fe3 Sn1 As2 107.8(17) 1_545 25 ? Ba1 Sn1 As2 103.4(13) . 25_445 ? Sn1 Sn1 As2 103.4(13) 17 25_445 ? Fe3 Sn1 As2 107.8(17) . 25_445 ? Fe3 Sn1 As2 107.8(17) 25 25_445 ? Fe3 Sn1 As2 50.0(6) 25_455 25_445 ? Fe3 Sn1 As2 50.0(6) 1_545 25_445 ? As2 Sn1 As2 153(3) 25 25_445 ? Ba1 Sn1 As2 103.4(13) . 25_545 ? Sn1 Sn1 As2 103.4(13) 17 25_545 ? Fe3 Sn1 As2 107.8(17) . 25_545 ? Fe3 Sn1 As2 50.0(6) 25 25_545 ? Fe3 Sn1 As2 107.8(17) 25_455 25_545 ? Fe3 Sn1 As2 50.0(6) 1_545 25_545 ? As2 Sn1 As2 86.9(6) 25 25_545 ? As2 Sn1 As2 86.9(6) 25_445 25_545 ? Ba1 Sn1 As2 103.4(13) . 25_455 ? Sn1 Sn1 As2 103.4(13) 17 25_455 ? Fe3 Sn1 As2 50.0(6) . 25_455 ? Fe3 Sn1 As2 107.8(17) 25 25_455 ? Fe3 Sn1 As2 50.0(6) 25_455 25_455 ? Fe3 Sn1 As2 107.8(17) 1_545 25_455 ? As2 Sn1 As2 86.9(6) 25 25_455 ? As2 Sn1 As2 86.9(6) 25_445 25_455 ? As2 Sn1 As2 153(3) 25_545 25_455 ? Ba1 Sn1 K1 71.7(8) . 1_545 ? Sn1 Sn1 K1 71.7(8) 17 1_545 ? Fe3 Sn1 K1 151.9(17) . 1_545 ? Fe3 Sn1 K1 103.1(4) 25 1_545 ? Fe3 Sn1 K1 103.1(4) 25_455 1_545 ? Fe3 Sn1 K1 64.69(5) 1_545 1_545 ? As2 Sn1 K1 136.5(3) 25 1_545 ? As2 Sn1 K1 54.5(3) 25_445 1_545 ? As2 Sn1 K1 54.5(3) 25_545 1_545 ? As2 Sn1 K1 136.5(3) 25_455 1_545 ? _diffrn_measured_fraction_theta_max 0.943 _diffrn_reflns_theta_full 28.49 _diffrn_measured_fraction_theta_full 0.943 _refine_diff_density_max 1.865 _refine_diff_density_min -1.745 _refine_diff_density_rms 0.375 # Attachment 'Ba61K35Sn4Fe2As21r.cif' data_jm2102a_0m _database_code_depnum_ccdc_archive 'CCDC 734672' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'As2 Ba0.61 Fe2 K0.35 Sn0.04' _chemical_formula_weight 363.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M I4/mmm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' '-x, y, -z' 'x, -y, -z' 'y, x, -z' '-y, -x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'y+1/2, x+1/2, -z+1/2' '-y+1/2, -x+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z' 'y, -x, -z' '-y, x, -z' 'x, -y, z' '-x, y, z' '-y, -x, z' 'y, x, z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' 'x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, x+1/2, z+1/2' _cell_length_a 3.9063(11) _cell_length_b 3.9063(11) _cell_length_c 13.352(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 203.75(10) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 108 _cell_measurement_theta_min 3.05 _cell_measurement_theta_max 29.38 _exptl_crystal_description plate _exptl_crystal_colour silver _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.005 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 5.927 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 314 _exptl_absorpt_coefficient_mu 28.316 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.512 _exptl_absorpt_correction_T_max 0.868 _exptl_absorpt_process_details 'via SADABS (Bruker, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'Bruker APEX CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 581 _diffrn_reflns_av_R_equivalents 0.0283 _diffrn_reflns_av_sigmaI/netI 0.0235 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -4 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 29.38 _reflns_number_total 108 _reflns_number_gt 101 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker APEX2' _computing_data_reduction 'Bruker APEX2' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0399P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0036(19) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 108 _refine_ls_number_parameters 13 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0271 _refine_ls_R_factor_gt 0.0260 _refine_ls_wR_factor_ref 0.0626 _refine_ls_wR_factor_gt 0.0621 _refine_ls_goodness_of_fit_ref 1.201 _refine_ls_restrained_S_all 1.195 _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 Ba1 Ba 0.0000 0.0000 0.0000 0.0153(5) Uani 0.606(9) 16 d SP . . K1 K 0.0000 0.0000 0.0000 0.0153(5) Uani 0.349(11) 16 d SP . . As2 As 0.0000 0.0000 0.35427(8) 0.0104(4) Uani 1 8 d S . . Fe3 Fe 0.0000 0.5000 0.2500 0.0101(4) Uani 1 8 d S . . Sn1 Sn 0.0000 0.0000 0.094(2) 0.0153(5) Uani 0.022(2) 8 d SP . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ba1 0.0166(6) 0.0166(6) 0.0128(8) 0.000 0.000 0.000 K1 0.0166(6) 0.0166(6) 0.0128(8) 0.000 0.000 0.000 As2 0.0102(5) 0.0102(5) 0.0108(6) 0.000 0.000 0.000 Fe3 0.0091(5) 0.0091(5) 0.0121(7) 0.000 0.000 0.000 Sn1 0.0166(6) 0.0166(6) 0.0128(8) 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 Ba1 Sn1 1.26(3) . ? Ba1 Sn1 1.26(3) 17 ? Ba1 As2 3.3787(9) 25 ? Ba1 As2 3.3787(9) 9_444 ? Ba1 As2 3.3787(9) 25_445 ? Ba1 As2 3.3787(9) 9_554 ? Ba1 As2 3.3787(9) 25_455 ? Ba1 As2 3.3787(9) 25_545 ? Ba1 As2 3.3787(9) 9_454 ? Ba1 As2 3.3787(9) 9_544 ? Ba1 Fe3 3.8675(8) . ? Ba1 Fe3 3.8675(8) 25 ? As2 Fe3 2.3986(8) 25_455 ? As2 Fe3 2.3986(8) 1_545 ? As2 Fe3 2.3986(8) 25 ? As2 Fe3 2.3986(8) . ? As2 Sn1 2.846(8) 25 ? As2 Sn1 2.846(8) 25_445 ? As2 Sn1 2.846(8) 25_455 ? As2 Sn1 2.846(8) 25_545 ? As2 Ba1 3.3787(9) 9 ? As2 K1 3.3787(9) 9 ? As2 Ba1 3.3787(9) 9_445 ? As2 Ba1 3.3787(9) 9_455 ? Fe3 As2 2.3986(8) 25_455 ? Fe3 As2 2.3986(8) 1_565 ? Fe3 As2 2.3986(8) 25 ? Fe3 Fe3 2.7622(8) 25_565 ? Fe3 Fe3 2.7622(8) 25_455 ? Fe3 Fe3 2.7622(8) 25_465 ? Fe3 Fe3 2.7622(8) 25 ? Fe3 Sn1 2.85(2) 25 ? Fe3 Sn1 2.85(2) 25_455 ? Fe3 Sn1 2.85(2) 1_565 ? Fe3 Sn1 2.85(2) . ? Sn1 Sn1 2.52(6) 17 ? Sn1 As2 2.846(8) 25 ? Sn1 As2 2.846(8) 25_445 ? Sn1 As2 2.846(8) 25_455 ? Sn1 As2 2.846(8) 25_545 ? Sn1 Fe3 2.85(2) 25 ? Sn1 Fe3 2.85(2) 25_455 ? Sn1 Fe3 2.85(2) 1_545 ? Sn1 K1 4.104(10) 1_455 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Sn1 Ba1 Sn1 180.000(1) . 17 ? Sn1 Ba1 As2 54.837(18) . 25 ? Sn1 Ba1 As2 125.163(18) 17 25 ? Sn1 Ba1 As2 125.163(18) . 9_444 ? Sn1 Ba1 As2 54.837(18) 17 9_444 ? As2 Ba1 As2 180.00(3) 25 9_444 ? Sn1 Ba1 As2 54.837(18) . 25_445 ? Sn1 Ba1 As2 125.163(18) 17 25_445 ? As2 Ba1 As2 109.67(4) 25 25_445 ? As2 Ba1 As2 70.33(4) 9_444 25_445 ? Sn1 Ba1 As2 125.163(18) . 9_554 ? Sn1 Ba1 As2 54.837(18) 17 9_554 ? As2 Ba1 As2 70.33(4) 25 9_554 ? As2 Ba1 As2 109.67(4) 9_444 9_554 ? As2 Ba1 As2 180.0 25_445 9_554 ? Sn1 Ba1 As2 54.837(18) . 25_455 ? Sn1 Ba1 As2 125.163(18) 17 25_455 ? As2 Ba1 As2 70.630(18) 25 25_455 ? As2 Ba1 As2 109.370(18) 9_444 25_455 ? As2 Ba1 As2 70.630(18) 25_445 25_455 ? As2 Ba1 As2 109.370(18) 9_554 25_455 ? Sn1 Ba1 As2 54.837(18) . 25_545 ? Sn1 Ba1 As2 125.163(18) 17 25_545 ? As2 Ba1 As2 70.630(18) 25 25_545 ? As2 Ba1 As2 109.370(18) 9_444 25_545 ? As2 Ba1 As2 70.630(18) 25_445 25_545 ? As2 Ba1 As2 109.370(18) 9_554 25_545 ? As2 Ba1 As2 109.67(4) 25_455 25_545 ? Sn1 Ba1 As2 125.163(18) . 9_454 ? Sn1 Ba1 As2 54.837(18) 17 9_454 ? As2 Ba1 As2 109.370(18) 25 9_454 ? As2 Ba1 As2 70.630(18) 9_444 9_454 ? As2 Ba1 As2 109.370(18) 25_445 9_454 ? As2 Ba1 As2 70.630(18) 9_554 9_454 ? As2 Ba1 As2 70.33(4) 25_455 9_454 ? As2 Ba1 As2 180.0 25_545 9_454 ? Sn1 Ba1 As2 125.163(18) . 9_544 ? Sn1 Ba1 As2 54.837(18) 17 9_544 ? As2 Ba1 As2 109.370(18) 25 9_544 ? As2 Ba1 As2 70.630(18) 9_444 9_544 ? As2 Ba1 As2 109.370(18) 25_445 9_544 ? As2 Ba1 As2 70.630(18) 9_554 9_544 ? As2 Ba1 As2 180.0 25_455 9_544 ? As2 Ba1 As2 70.33(4) 25_545 9_544 ? As2 Ba1 As2 109.67(4) 9_454 9_544 ? Sn1 Ba1 Fe3 30.332(10) . . ? Sn1 Ba1 Fe3 149.668(10) 17 . ? As2 Ba1 Fe3 37.907(13) 25 . ? As2 Ba1 Fe3 142.093(13) 9_444 . ? As2 Ba1 Fe3 78.16(2) 25_445 . ? As2 Ba1 Fe3 101.84(2) 9_554 . ? As2 Ba1 Fe3 37.907(13) 25_455 . ? As2 Ba1 Fe3 78.16(2) 25_545 . ? As2 Ba1 Fe3 101.84(2) 9_454 . ? As2 Ba1 Fe3 142.093(13) 9_544 . ? Sn1 Ba1 Fe3 30.332(10) . 25 ? Sn1 Ba1 Fe3 149.668(10) 17 25 ? As2 Ba1 Fe3 37.907(13) 25 25 ? As2 Ba1 Fe3 142.093(13) 9_444 25 ? As2 Ba1 Fe3 78.16(2) 25_445 25 ? As2 Ba1 Fe3 101.84(2) 9_554 25 ? As2 Ba1 Fe3 78.16(2) 25_455 25 ? As2 Ba1 Fe3 37.907(13) 25_545 25 ? As2 Ba1 Fe3 142.093(13) 9_454 25 ? As2 Ba1 Fe3 101.84(2) 9_544 25 ? Fe3 Ba1 Fe3 41.844(13) . 25 ? Fe3 As2 Fe3 70.31(2) 25_455 1_545 ? Fe3 As2 Fe3 109.03(5) 25_455 25 ? Fe3 As2 Fe3 70.31(2) 1_545 25 ? Fe3 As2 Fe3 70.31(2) 25_455 . ? Fe3 As2 Fe3 109.03(5) 1_545 . ? Fe3 As2 Fe3 70.31(2) 25 . ? Fe3 As2 Sn1 134.3(4) 25_455 25 ? Fe3 As2 Sn1 134.3(4) 1_545 25 ? Fe3 As2 Sn1 65.2(5) 25 25 ? Fe3 As2 Sn1 65.2(5) . 25 ? Fe3 As2 Sn1 65.2(5) 25_455 25_445 ? Fe3 As2 Sn1 65.2(5) 1_545 25_445 ? Fe3 As2 Sn1 134.3(4) 25 25_445 ? Fe3 As2 Sn1 134.3(4) . 25_445 ? Sn1 As2 Sn1 152.1(12) 25 25_445 ? Fe3 As2 Sn1 65.2(5) 25_455 25_455 ? Fe3 As2 Sn1 134.3(4) 1_545 25_455 ? Fe3 As2 Sn1 134.3(4) 25 25_455 ? Fe3 As2 Sn1 65.2(5) . 25_455 ? Sn1 As2 Sn1 86.7(3) 25 25_455 ? Sn1 As2 Sn1 86.7(3) 25_445 25_455 ? Fe3 As2 Sn1 134.3(4) 25_455 25_545 ? Fe3 As2 Sn1 65.2(5) 1_545 25_545 ? Fe3 As2 Sn1 65.2(5) 25 25_545 ? Fe3 As2 Sn1 134.3(4) . 25_545 ? Sn1 As2 Sn1 86.7(3) 25 25_545 ? Sn1 As2 Sn1 86.7(3) 25_445 25_545 ? Sn1 As2 Sn1 152.1(12) 25_455 25_545 ? Fe3 As2 Ba1 143.611(5) 25_455 9 ? Fe3 As2 Ba1 143.611(5) 1_545 9 ? Fe3 As2 Ba1 82.159(18) 25 9 ? Fe3 As2 Ba1 82.159(18) . 9 ? Sn1 As2 Ba1 21.2(6) 25 9 ? Sn1 As2 Ba1 130.9(6) 25_445 9 ? Sn1 As2 Ba1 82.0(4) 25_455 9 ? Sn1 As2 Ba1 82.0(4) 25_545 9 ? Fe3 As2 K1 143.611(5) 25_455 9 ? Fe3 As2 K1 143.611(5) 1_545 9 ? Fe3 As2 K1 82.159(18) 25 9 ? Fe3 As2 K1 82.159(18) . 9 ? Sn1 As2 K1 21.2(6) 25 9 ? Sn1 As2 K1 130.9(6) 25_445 9 ? Sn1 As2 K1 82.0(4) 25_455 9 ? Sn1 As2 K1 82.0(4) 25_545 9 ? Ba1 As2 K1 0.0 9 9 ? Fe3 As2 Ba1 82.159(18) 25_455 9_445 ? Fe3 As2 Ba1 82.159(18) 1_545 9_445 ? Fe3 As2 Ba1 143.611(5) 25 9_445 ? Fe3 As2 Ba1 143.611(5) . 9_445 ? Sn1 As2 Ba1 130.9(6) 25 9_445 ? Sn1 As2 Ba1 21.2(6) 25_445 9_445 ? Sn1 As2 Ba1 82.0(4) 25_455 9_445 ? Sn1 As2 Ba1 82.0(4) 25_545 9_445 ? Ba1 As2 Ba1 109.67(4) 9 9_445 ? K1 As2 Ba1 109.67(4) 9 9_445 ? Fe3 As2 Ba1 82.159(18) 25_455 9_455 ? Fe3 As2 Ba1 143.611(5) 1_545 9_455 ? Fe3 As2 Ba1 143.611(5) 25 9_455 ? Fe3 As2 Ba1 82.159(18) . 9_455 ? Sn1 As2 Ba1 82.0(4) 25 9_455 ? Sn1 As2 Ba1 82.0(4) 25_445 9_455 ? Sn1 As2 Ba1 21.2(6) 25_455 9_455 ? Sn1 As2 Ba1 130.9(6) 25_545 9_455 ? Ba1 As2 Ba1 70.630(18) 9 9_455 ? K1 As2 Ba1 70.630(18) 9 9_455 ? Ba1 As2 Ba1 70.630(18) 9_445 9_455 ? As2 Fe3 As2 109.69(2) 25_455 1_565 ? As2 Fe3 As2 109.04(5) 25_455 25 ? As2 Fe3 As2 109.69(2) 1_565 25 ? As2 Fe3 As2 109.69(2) 25_455 . ? As2 Fe3 As2 109.03(5) 1_565 . ? As2 Fe3 As2 109.69(2) 25 . ? As2 Fe3 Fe3 125.155(11) 25_455 25_565 ? As2 Fe3 Fe3 54.845(12) 1_565 25_565 ? As2 Fe3 Fe3 54.845(12) 25 25_565 ? As2 Fe3 Fe3 125.155(11) . 25_565 ? As2 Fe3 Fe3 54.845(12) 25_455 25_455 ? As2 Fe3 Fe3 125.155(11) 1_565 25_455 ? As2 Fe3 Fe3 125.155(11) 25 25_455 ? As2 Fe3 Fe3 54.845(11) . 25_455 ? Fe3 Fe3 Fe3 180.0 25_565 25_455 ? As2 Fe3 Fe3 54.845(12) 25_455 25_465 ? As2 Fe3 Fe3 54.845(12) 1_565 25_465 ? As2 Fe3 Fe3 125.155(11) 25 25_465 ? As2 Fe3 Fe3 125.155(11) . 25_465 ? Fe3 Fe3 Fe3 90.0 25_565 25_465 ? Fe3 Fe3 Fe3 90.0 25_455 25_465 ? As2 Fe3 Fe3 125.155(11) 25_455 25 ? As2 Fe3 Fe3 125.155(11) 1_565 25 ? As2 Fe3 Fe3 54.845(11) 25 25 ? As2 Fe3 Fe3 54.845(12) . 25 ? Fe3 Fe3 Fe3 90.0 25_565 25 ? Fe3 Fe3 Fe3 90.0 25_455 25 ? Fe3 Fe3 Fe3 180.0 25_465 25 ? As2 Fe3 Sn1 168.7(4) 25_455 25 ? As2 Fe3 Sn1 65.0(2) 1_565 25 ? As2 Fe3 Sn1 82.3(4) 25 25 ? As2 Fe3 Sn1 64.97(19) . 25 ? Fe3 Fe3 Sn1 61.0(3) 25_565 25 ? Fe3 Fe3 Sn1 119.0(3) 25_455 25 ? Fe3 Fe3 Sn1 119.0(3) 25_465 25 ? Fe3 Fe3 Sn1 61.0(3) 25 25 ? As2 Fe3 Sn1 82.3(4) 25_455 25_455 ? As2 Fe3 Sn1 65.0(2) 1_565 25_455 ? As2 Fe3 Sn1 168.7(4) 25 25_455 ? As2 Fe3 Sn1 65.0(2) . 25_455 ? Fe3 Fe3 Sn1 119.0(3) 25_565 25_455 ? Fe3 Fe3 Sn1 61.0(3) 25_455 25_455 ? Fe3 Fe3 Sn1 61.0(3) 25_465 25_455 ? Fe3 Fe3 Sn1 119.0(3) 25 25_455 ? Sn1 Fe3 Sn1 86.4(9) 25 25_455 ? As2 Fe3 Sn1 64.97(19) 25_455 1_565 ? As2 Fe3 Sn1 82.3(4) 1_565 1_565 ? As2 Fe3 Sn1 64.97(19) 25 1_565 ? As2 Fe3 Sn1 168.7(4) . 1_565 ? Fe3 Fe3 Sn1 61.0(3) 25_565 1_565 ? Fe3 Fe3 Sn1 119.0(3) 25_455 1_565 ? Fe3 Fe3 Sn1 61.0(3) 25_465 1_565 ? Fe3 Fe3 Sn1 119.0(3) 25 1_565 ? Sn1 Fe3 Sn1 122.1(5) 25 1_565 ? Sn1 Fe3 Sn1 122.1(5) 25_455 1_565 ? As2 Fe3 Sn1 65.0(2) 25_455 . ? As2 Fe3 Sn1 168.7(4) 1_565 . ? As2 Fe3 Sn1 64.97(19) 25 . ? As2 Fe3 Sn1 82.3(4) . . ? Fe3 Fe3 Sn1 119.0(3) 25_565 . ? Fe3 Fe3 Sn1 61.0(3) 25_455 . ? Fe3 Fe3 Sn1 119.0(3) 25_465 . ? Fe3 Fe3 Sn1 61.0(3) 25 . ? Sn1 Fe3 Sn1 122.1(5) 25 . ? Sn1 Fe3 Sn1 122.1(5) 25_455 . ? Sn1 Fe3 Sn1 86.4(9) 1_565 . ? Ba1 Sn1 Sn1 0.0 . 17 ? Ba1 Sn1 As2 104.0(6) . 25 ? Sn1 Sn1 As2 104.0(6) 17 25 ? Ba1 Sn1 As2 104.0(6) . 25_445 ? Sn1 Sn1 As2 104.0(6) 17 25_445 ? As2 Sn1 As2 152.1(12) 25 25_445 ? Ba1 Sn1 As2 104.0(6) . 25_455 ? Sn1 Sn1 As2 104.0(6) 17 25_455 ? As2 Sn1 As2 86.7(3) 25 25_455 ? As2 Sn1 As2 86.7(3) 25_445 25_455 ? Ba1 Sn1 As2 104.0(6) . 25_545 ? Sn1 Sn1 As2 104.0(6) 17 25_545 ? As2 Sn1 As2 86.7(3) 25 25_545 ? As2 Sn1 As2 86.7(3) 25_445 25_545 ? As2 Sn1 As2 152.1(12) 25_455 25_545 ? Ba1 Sn1 Fe3 136.8(4) . . ? Sn1 Sn1 Fe3 136.8(4) 17 . ? As2 Sn1 Fe3 49.8(3) 25 . ? As2 Sn1 Fe3 107.1(8) 25_445 . ? As2 Sn1 Fe3 49.8(3) 25_455 . ? As2 Sn1 Fe3 107.1(8) 25_545 . ? Ba1 Sn1 Fe3 136.8(4) . 25 ? Sn1 Sn1 Fe3 136.8(4) 17 25 ? As2 Sn1 Fe3 49.8(3) 25 25 ? As2 Sn1 Fe3 107.1(8) 25_445 25 ? As2 Sn1 Fe3 107.1(8) 25_455 25 ? As2 Sn1 Fe3 49.8(3) 25_545 25 ? Fe3 Sn1 Fe3 57.9(5) . 25 ? Ba1 Sn1 Fe3 136.8(4) . 25_455 ? Sn1 Sn1 Fe3 136.8(4) 17 25_455 ? As2 Sn1 Fe3 107.1(8) 25 25_455 ? As2 Sn1 Fe3 49.8(3) 25_445 25_455 ? As2 Sn1 Fe3 49.8(3) 25_455 25_455 ? As2 Sn1 Fe3 107.1(8) 25_545 25_455 ? Fe3 Sn1 Fe3 57.9(5) . 25_455 ? Fe3 Sn1 Fe3 86.4(9) 25 25_455 ? Ba1 Sn1 Fe3 136.8(4) . 1_545 ? Sn1 Sn1 Fe3 136.8(4) 17 1_545 ? As2 Sn1 Fe3 107.1(8) 25 1_545 ? As2 Sn1 Fe3 49.8(3) 25_445 1_545 ? As2 Sn1 Fe3 107.1(8) 25_455 1_545 ? As2 Sn1 Fe3 49.8(3) 25_545 1_545 ? Fe3 Sn1 Fe3 86.4(9) . 1_545 ? Fe3 Sn1 Fe3 57.9(5) 25 1_545 ? Fe3 Sn1 Fe3 57.9(5) 25_455 1_545 ? Ba1 Sn1 K1 72.1(4) . 1_455 ? Sn1 Sn1 K1 72.1(4) 17 1_455 ? As2 Sn1 K1 136.65(11) 25 1_455 ? As2 Sn1 K1 54.61(12) 25_445 1_455 ? As2 Sn1 K1 54.61(12) 25_455 1_455 ? As2 Sn1 K1 136.65(11) 25_545 1_455 ? Fe3 Sn1 K1 102.9(2) . 1_455 ? Fe3 Sn1 K1 151.1(9) 25 1_455 ? Fe3 Sn1 K1 64.65(2) 25_455 1_455 ? Fe3 Sn1 K1 102.9(2) 1_545 1_455 ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 29.38 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 1.093 _refine_diff_density_min -1.121 _refine_diff_density_rms 0.284 # Attachment 'Ba68K24Sn7Fe2As2r.cif' data_data_0m3 _database_code_depnum_ccdc_archive 'CCDC 734673' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'As2 Ba0.68 Fe2 K0.24 Sn0.07' _chemical_formula_weight 372.59 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M I4/mmm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' '-x, y, -z' 'x, -y, -z' 'y, x, -z' '-y, -x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'y+1/2, x+1/2, -z+1/2' '-y+1/2, -x+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z' 'y, -x, -z' '-y, x, -z' 'x, -y, z' '-x, y, z' '-y, -x, z' 'y, x, z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' 'x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, x+1/2, z+1/2' _cell_length_a 3.946(2) _cell_length_b 3.946(2) _cell_length_c 13.431(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 209.1(2) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 125 _cell_measurement_theta_min 3.03 _cell_measurement_theta_max 32.39 _exptl_crystal_description plate _exptl_crystal_colour silver _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 5.935 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 310 _exptl_absorpt_coefficient_mu 29.173 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.501 _exptl_absorpt_correction_T_max 0.747 _exptl_absorpt_process_details 'via SADABS (Bruker, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'Bruker APEX CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 609 _diffrn_reflns_av_R_equivalents 0.0261 _diffrn_reflns_av_sigmaI/netI 0.0220 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 32.39 _reflns_number_total 125 _reflns_number_gt 117 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker APEX2' _computing_data_reduction 'Bruker APEX2' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0224P)^2^+1.2844P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0054(15) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 125 _refine_ls_number_parameters 13 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0245 _refine_ls_R_factor_gt 0.0232 _refine_ls_wR_factor_ref 0.0563 _refine_ls_wR_factor_gt 0.0558 _refine_ls_goodness_of_fit_ref 1.294 _refine_ls_restrained_S_all 1.288 _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 Ba1 Ba 0.0000 0.0000 0.0000 0.0167(4) Uani 0.683(8) 16 d SP . . K1 K 0.0000 0.0000 0.0000 0.0167(4) Uani 0.244(10) 16 d SP . . As2 As 0.0000 0.0000 0.35435(8) 0.0112(4) Uani 1 8 d S . . Fe3 Fe 0.0000 0.5000 0.2500 0.0109(4) Uani 1 8 d S . . Sn1 Sn 0.0000 0.0000 0.0903(16) 0.0167(4) Uani 0.037(2) 8 d SP . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ba1 0.0186(5) 0.0186(5) 0.0129(8) 0.000 0.000 0.000 K1 0.0186(5) 0.0186(5) 0.0129(8) 0.000 0.000 0.000 As2 0.0120(4) 0.0120(4) 0.0095(7) 0.000 0.000 0.000 Fe3 0.0102(4) 0.0102(4) 0.0124(8) 0.000 0.000 0.000 Sn1 0.0186(5) 0.0186(5) 0.0129(8) 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 Ba1 Sn1 1.21(2) 17 ? Ba1 Sn1 1.21(2) . ? Ba1 As2 3.4077(17) 25 ? Ba1 As2 3.4077(17) 9_444 ? Ba1 As2 3.4077(17) 25_455 ? Ba1 As2 3.4077(17) 25_545 ? Ba1 As2 3.4077(17) 9_454 ? Ba1 As2 3.4077(17) 9_544 ? Ba1 As2 3.4077(17) 25_445 ? Ba1 As2 3.4077(17) 9_554 ? Ba1 Fe3 3.895(2) . ? Ba1 Fe3 3.895(2) 25 ? As2 Fe3 2.4202(13) 25_455 ? As2 Fe3 2.4202(13) 1_545 ? As2 Fe3 2.4202(13) 25 ? As2 Fe3 2.4202(13) . ? As2 Sn1 2.888(6) 25 ? As2 Sn1 2.888(6) 25_445 ? As2 Sn1 2.888(6) 25_455 ? As2 Sn1 2.888(6) 25_545 ? As2 Ba1 3.4077(17) 9 ? As2 K1 3.4077(17) 9 ? As2 K1 3.4077(17) 9_545 ? As2 Ba1 3.4077(17) 9_455 ? Fe3 As2 2.4202(13) 25_455 ? Fe3 As2 2.4202(13) 1_565 ? Fe3 As2 2.4202(13) 25 ? Fe3 Fe3 2.7903(17) 25_565 ? Fe3 Fe3 2.7903(17) 25_455 ? Fe3 Fe3 2.7903(17) 25_465 ? Fe3 Fe3 2.7903(17) 25 ? Fe3 Sn1 2.914(16) . ? Fe3 Sn1 2.914(16) 25 ? Fe3 Sn1 2.914(16) 25_455 ? Fe3 Sn1 2.914(16) 1_565 ? Sn1 Sn1 2.43(4) 17 ? Sn1 As2 2.888(6) 25 ? Sn1 As2 2.888(6) 25_445 ? Sn1 As2 2.888(6) 25_455 ? Sn1 As2 2.888(6) 25_545 ? Sn1 Fe3 2.914(16) 25 ? Sn1 Fe3 2.914(16) 25_455 ? Sn1 Fe3 2.914(16) 1_545 ? Sn1 K1 4.128(7) 1_455 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Sn1 Ba1 Sn1 180.0 17 . ? Sn1 Ba1 As2 125.03(3) 17 25 ? Sn1 Ba1 As2 54.97(3) . 25 ? Sn1 Ba1 As2 54.97(3) 17 9_444 ? Sn1 Ba1 As2 125.03(3) . 9_444 ? As2 Ba1 As2 180.00(3) 25 9_444 ? Sn1 Ba1 As2 125.03(3) 17 25_455 ? Sn1 Ba1 As2 54.97(3) . 25_455 ? As2 Ba1 As2 70.76(3) 25 25_455 ? As2 Ba1 As2 109.24(3) 9_444 25_455 ? Sn1 Ba1 As2 125.03(3) 17 25_545 ? Sn1 Ba1 As2 54.97(3) . 25_545 ? As2 Ba1 As2 70.76(3) 25 25_545 ? As2 Ba1 As2 109.24(3) 9_444 25_545 ? As2 Ba1 As2 109.93(6) 25_455 25_545 ? Sn1 Ba1 As2 54.97(3) 17 9_454 ? Sn1 Ba1 As2 125.03(3) . 9_454 ? As2 Ba1 As2 109.24(3) 25 9_454 ? As2 Ba1 As2 70.76(3) 9_444 9_454 ? As2 Ba1 As2 70.07(6) 25_455 9_454 ? As2 Ba1 As2 180.00(3) 25_545 9_454 ? Sn1 Ba1 As2 54.97(3) 17 9_544 ? Sn1 Ba1 As2 125.03(3) . 9_544 ? As2 Ba1 As2 109.24(3) 25 9_544 ? As2 Ba1 As2 70.76(3) 9_444 9_544 ? As2 Ba1 As2 180.00(3) 25_455 9_544 ? As2 Ba1 As2 70.07(6) 25_545 9_544 ? As2 Ba1 As2 109.93(6) 9_454 9_544 ? Sn1 Ba1 As2 125.03(3) 17 25_445 ? Sn1 Ba1 As2 54.97(3) . 25_445 ? As2 Ba1 As2 109.93(6) 25 25_445 ? As2 Ba1 As2 70.07(6) 9_444 25_445 ? As2 Ba1 As2 70.76(3) 25_455 25_445 ? As2 Ba1 As2 70.76(3) 25_545 25_445 ? As2 Ba1 As2 109.24(3) 9_454 25_445 ? As2 Ba1 As2 109.24(3) 9_544 25_445 ? Sn1 Ba1 As2 54.97(3) 17 9_554 ? Sn1 Ba1 As2 125.03(3) . 9_554 ? As2 Ba1 As2 70.07(6) 25 9_554 ? As2 Ba1 As2 109.93(6) 9_444 9_554 ? As2 Ba1 As2 109.24(3) 25_455 9_554 ? As2 Ba1 As2 109.24(3) 25_545 9_554 ? As2 Ba1 As2 70.76(3) 9_454 9_554 ? As2 Ba1 As2 70.76(3) 9_544 9_554 ? As2 Ba1 As2 180.00(3) 25_445 9_554 ? Sn1 Ba1 Fe3 149.56(2) 17 . ? Sn1 Ba1 Fe3 30.44(2) . . ? As2 Ba1 Fe3 37.977(17) 25 . ? As2 Ba1 Fe3 142.023(17) 9_444 . ? As2 Ba1 Fe3 37.977(17) 25_455 . ? As2 Ba1 Fe3 78.37(4) 25_545 . ? As2 Ba1 Fe3 101.63(4) 9_454 . ? As2 Ba1 Fe3 142.023(17) 9_544 . ? As2 Ba1 Fe3 78.37(4) 25_445 . ? As2 Ba1 Fe3 101.63(4) 9_554 . ? Sn1 Ba1 Fe3 149.56(2) 17 25 ? Sn1 Ba1 Fe3 30.44(2) . 25 ? As2 Ba1 Fe3 37.977(17) 25 25 ? As2 Ba1 Fe3 142.023(17) 9_444 25 ? As2 Ba1 Fe3 78.37(4) 25_455 25 ? As2 Ba1 Fe3 37.977(17) 25_545 25 ? As2 Ba1 Fe3 142.023(17) 9_454 25 ? As2 Ba1 Fe3 101.63(4) 9_544 25 ? As2 Ba1 Fe3 78.37(4) 25_445 25 ? As2 Ba1 Fe3 101.63(4) 9_554 25 ? Fe3 Ba1 Fe3 41.98(3) . 25 ? Fe3 As2 Fe3 70.41(3) 25_455 1_545 ? Fe3 As2 Fe3 109.22(6) 25_455 25 ? Fe3 As2 Fe3 70.41(3) 1_545 25 ? Fe3 As2 Fe3 70.41(3) 25_455 . ? Fe3 As2 Fe3 109.22(6) 1_545 . ? Fe3 As2 Fe3 70.41(3) 25 . ? Fe3 As2 Sn1 134.9(2) 25_455 25 ? Fe3 As2 Sn1 134.9(2) 1_545 25 ? Fe3 As2 Sn1 65.9(3) 25 25 ? Fe3 As2 Sn1 65.9(3) . 25 ? Fe3 As2 Sn1 65.9(3) 25_455 25_445 ? Fe3 As2 Sn1 65.9(3) 1_545 25_445 ? Fe3 As2 Sn1 134.9(2) 25 25_445 ? Fe3 As2 Sn1 134.9(2) . 25_445 ? Sn1 As2 Sn1 150.2(8) 25 25_445 ? Fe3 As2 Sn1 65.9(3) 25_455 25_455 ? Fe3 As2 Sn1 134.9(2) 1_545 25_455 ? Fe3 As2 Sn1 134.9(2) 25 25_455 ? Fe3 As2 Sn1 65.9(3) . 25_455 ? Sn1 As2 Sn1 86.2(2) 25 25_455 ? Sn1 As2 Sn1 86.2(2) 25_445 25_455 ? Fe3 As2 Sn1 134.9(2) 25_455 25_545 ? Fe3 As2 Sn1 65.9(3) 1_545 25_545 ? Fe3 As2 Sn1 65.9(3) 25 25_545 ? Fe3 As2 Sn1 134.9(2) . 25_545 ? Sn1 As2 Sn1 86.2(2) 25 25_545 ? Sn1 As2 Sn1 86.2(2) 25_445 25_545 ? Sn1 As2 Sn1 150.2(8) 25_455 25_545 ? Fe3 As2 Ba1 143.558(11) 25_455 9 ? Fe3 As2 Ba1 143.558(11) 1_545 9 ? Fe3 As2 Ba1 81.98(4) 25 9 ? Fe3 As2 Ba1 81.98(4) . 9 ? Sn1 As2 Ba1 20.1(4) 25 9 ? Sn1 As2 Ba1 130.0(4) 25_445 9 ? Sn1 As2 Ba1 81.5(2) 25_455 9 ? Sn1 As2 Ba1 81.5(2) 25_545 9 ? Fe3 As2 K1 143.558(11) 25_455 9 ? Fe3 As2 K1 143.558(11) 1_545 9 ? Fe3 As2 K1 81.98(4) 25 9 ? Fe3 As2 K1 81.98(4) . 9 ? Sn1 As2 K1 20.1(4) 25 9 ? Sn1 As2 K1 130.0(4) 25_445 9 ? Sn1 As2 K1 81.5(2) 25_455 9 ? Sn1 As2 K1 81.5(2) 25_545 9 ? Ba1 As2 K1 0.0 9 9 ? Fe3 As2 K1 143.558(11) 25_455 9_545 ? Fe3 As2 K1 81.98(4) 1_545 9_545 ? Fe3 As2 K1 81.98(4) 25 9_545 ? Fe3 As2 K1 143.558(11) . 9_545 ? Sn1 As2 K1 81.5(2) 25 9_545 ? Sn1 As2 K1 81.5(2) 25_445 9_545 ? Sn1 As2 K1 130.0(4) 25_455 9_545 ? Sn1 As2 K1 20.1(4) 25_545 9_545 ? Ba1 As2 K1 70.76(3) 9 9_545 ? K1 As2 K1 70.76(3) 9 9_545 ? Fe3 As2 Ba1 81.98(4) 25_455 9_455 ? Fe3 As2 Ba1 143.558(11) 1_545 9_455 ? Fe3 As2 Ba1 143.558(11) 25 9_455 ? Fe3 As2 Ba1 81.98(4) . 9_455 ? Sn1 As2 Ba1 81.5(2) 25 9_455 ? Sn1 As2 Ba1 81.5(2) 25_445 9_455 ? Sn1 As2 Ba1 20.1(4) 25_455 9_455 ? Sn1 As2 Ba1 130.0(4) 25_545 9_455 ? Ba1 As2 Ba1 70.76(3) 9 9_455 ? K1 As2 Ba1 70.76(3) 9 9_455 ? K1 As2 Ba1 109.93(6) 9_545 9_455 ? As2 Fe3 As2 109.60(3) . 25_455 ? As2 Fe3 As2 109.22(6) . 1_565 ? As2 Fe3 As2 109.60(3) 25_455 1_565 ? As2 Fe3 As2 109.60(3) . 25 ? As2 Fe3 As2 109.22(6) 25_455 25 ? As2 Fe3 As2 109.60(3) 1_565 25 ? As2 Fe3 Fe3 125.203(16) . 25_565 ? As2 Fe3 Fe3 125.202(16) 25_455 25_565 ? As2 Fe3 Fe3 54.798(16) 1_565 25_565 ? As2 Fe3 Fe3 54.798(16) 25 25_565 ? As2 Fe3 Fe3 54.797(16) . 25_455 ? As2 Fe3 Fe3 54.798(16) 25_455 25_455 ? As2 Fe3 Fe3 125.202(16) 1_565 25_455 ? As2 Fe3 Fe3 125.202(16) 25 25_455 ? Fe3 Fe3 Fe3 180.0 25_565 25_455 ? As2 Fe3 Fe3 125.203(16) . 25_465 ? As2 Fe3 Fe3 54.798(16) 25_455 25_465 ? As2 Fe3 Fe3 54.798(16) 1_565 25_465 ? As2 Fe3 Fe3 125.202(16) 25 25_465 ? Fe3 Fe3 Fe3 90.0 25_565 25_465 ? Fe3 Fe3 Fe3 90.0 25_455 25_465 ? As2 Fe3 Fe3 54.797(16) . 25 ? As2 Fe3 Fe3 125.202(16) 25_455 25 ? As2 Fe3 Fe3 125.202(16) 1_565 25 ? As2 Fe3 Fe3 54.798(16) 25 25 ? Fe3 Fe3 Fe3 90.0 25_565 25 ? Fe3 Fe3 Fe3 90.0 25_455 25 ? Fe3 Fe3 Fe3 180.0 25_465 25 ? As2 Fe3 Sn1 82.8(3) . . ? As2 Fe3 Sn1 64.77(13) 25_455 . ? As2 Fe3 Sn1 168.0(3) 1_565 . ? As2 Fe3 Sn1 64.77(13) 25 . ? Fe3 Fe3 Sn1 118.60(17) 25_565 . ? Fe3 Fe3 Sn1 61.40(17) 25_455 . ? Fe3 Fe3 Sn1 118.60(17) 25_465 . ? Fe3 Fe3 Sn1 61.40(17) 25 . ? As2 Fe3 Sn1 64.77(13) . 25 ? As2 Fe3 Sn1 168.0(3) 25_455 25 ? As2 Fe3 Sn1 64.77(13) 1_565 25 ? As2 Fe3 Sn1 82.8(3) 25 25 ? Fe3 Fe3 Sn1 61.40(17) 25_565 25 ? Fe3 Fe3 Sn1 118.60(17) 25_455 25 ? Fe3 Fe3 Sn1 118.60(17) 25_465 25 ? Fe3 Fe3 Sn1 61.40(17) 25 25 ? Sn1 Fe3 Sn1 122.8(3) . 25 ? As2 Fe3 Sn1 64.77(13) . 25_455 ? As2 Fe3 Sn1 82.8(3) 25_455 25_455 ? As2 Fe3 Sn1 64.77(13) 1_565 25_455 ? As2 Fe3 Sn1 168.0(3) 25 25_455 ? Fe3 Fe3 Sn1 118.60(17) 25_565 25_455 ? Fe3 Fe3 Sn1 61.40(17) 25_455 25_455 ? Fe3 Fe3 Sn1 61.40(17) 25_465 25_455 ? Fe3 Fe3 Sn1 118.60(17) 25 25_455 ? Sn1 Fe3 Sn1 122.8(3) . 25_455 ? Sn1 Fe3 Sn1 85.2(6) 25 25_455 ? As2 Fe3 Sn1 168.0(3) . 1_565 ? As2 Fe3 Sn1 64.77(13) 25_455 1_565 ? As2 Fe3 Sn1 82.8(3) 1_565 1_565 ? As2 Fe3 Sn1 64.77(13) 25 1_565 ? Fe3 Fe3 Sn1 61.40(17) 25_565 1_565 ? Fe3 Fe3 Sn1 118.60(17) 25_455 1_565 ? Fe3 Fe3 Sn1 61.40(17) 25_465 1_565 ? Fe3 Fe3 Sn1 118.60(17) 25 1_565 ? Sn1 Fe3 Sn1 85.2(6) . 1_565 ? Sn1 Fe3 Sn1 122.8(3) 25 1_565 ? Sn1 Fe3 Sn1 122.8(3) 25_455 1_565 ? Ba1 Sn1 Sn1 0.0 . 17 ? Ba1 Sn1 As2 104.9(4) . 25 ? Sn1 Sn1 As2 104.9(4) 17 25 ? Ba1 Sn1 As2 104.9(4) . 25_445 ? Sn1 Sn1 As2 104.9(4) 17 25_445 ? As2 Sn1 As2 150.2(8) 25 25_445 ? Ba1 Sn1 As2 104.9(4) . 25_455 ? Sn1 Sn1 As2 104.9(4) 17 25_455 ? As2 Sn1 As2 86.2(2) 25 25_455 ? As2 Sn1 As2 86.2(2) 25_445 25_455 ? Ba1 Sn1 As2 104.9(4) . 25_545 ? Sn1 Sn1 As2 104.9(4) 17 25_545 ? As2 Sn1 As2 86.2(2) 25 25_545 ? As2 Sn1 As2 86.2(2) 25_445 25_545 ? As2 Sn1 As2 150.2(8) 25_455 25_545 ? Ba1 Sn1 Fe3 137.4(3) . . ? Sn1 Sn1 Fe3 137.4(3) 17 . ? As2 Sn1 Fe3 49.3(2) 25 . ? As2 Sn1 Fe3 105.9(6) 25_445 . ? As2 Sn1 Fe3 49.3(2) 25_455 . ? As2 Sn1 Fe3 105.9(6) 25_545 . ? Ba1 Sn1 Fe3 137.4(3) . 25 ? Sn1 Sn1 Fe3 137.4(3) 17 25 ? As2 Sn1 Fe3 49.3(2) 25 25 ? As2 Sn1 Fe3 105.9(6) 25_445 25 ? As2 Sn1 Fe3 105.9(6) 25_455 25 ? As2 Sn1 Fe3 49.3(2) 25_545 25 ? Fe3 Sn1 Fe3 57.2(3) . 25 ? Ba1 Sn1 Fe3 137.4(3) . 25_455 ? Sn1 Sn1 Fe3 137.4(3) 17 25_455 ? As2 Sn1 Fe3 105.9(6) 25 25_455 ? As2 Sn1 Fe3 49.3(2) 25_445 25_455 ? As2 Sn1 Fe3 49.3(2) 25_455 25_455 ? As2 Sn1 Fe3 105.9(6) 25_545 25_455 ? Fe3 Sn1 Fe3 57.2(3) . 25_455 ? Fe3 Sn1 Fe3 85.2(6) 25 25_455 ? Ba1 Sn1 Fe3 137.4(3) . 1_545 ? Sn1 Sn1 Fe3 137.4(3) 17 1_545 ? As2 Sn1 Fe3 105.9(6) 25 1_545 ? As2 Sn1 Fe3 49.3(2) 25_445 1_545 ? As2 Sn1 Fe3 105.9(6) 25_455 1_545 ? As2 Sn1 Fe3 49.3(2) 25_545 1_545 ? Fe3 Sn1 Fe3 85.2(6) . 1_545 ? Fe3 Sn1 Fe3 57.2(3) 25 1_545 ? Fe3 Sn1 Fe3 57.2(3) 25_455 1_545 ? Ba1 Sn1 K1 72.9(3) . 1_455 ? Sn1 Sn1 K1 72.9(3) 17 1_455 ? As2 Sn1 K1 136.78(5) 25 1_455 ? As2 Sn1 K1 54.72(8) 25_445 1_455 ? As2 Sn1 K1 54.72(8) 25_455 1_455 ? As2 Sn1 K1 136.78(5) 25_545 1_455 ? Fe3 Sn1 K1 102.49(15) . 1_455 ? Fe3 Sn1 K1 149.7(6) 25 1_455 ? Fe3 Sn1 K1 64.48(4) 25_455 1_455 ? Fe3 Sn1 K1 102.49(15) 1_545 1_455 ? _diffrn_measured_fraction_theta_max 0.887 _diffrn_reflns_theta_full 32.39 _diffrn_measured_fraction_theta_full 0.887 _refine_diff_density_max 2.118 _refine_diff_density_min -1.681 _refine_diff_density_rms 0.235 # Attachment 'Ba78K13Sn10Fe2As2r.cif' data_data_0m4 _database_code_depnum_ccdc_archive 'CCDC 734674' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'As2 Ba0.78 Fe2 K0.12 Sn0.10' _chemical_formula_weight 384.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M I4/mmm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' '-x, y, -z' 'x, -y, -z' 'y, x, -z' '-y, -x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'y+1/2, x+1/2, -z+1/2' '-y+1/2, -x+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z' 'y, -x, -z' '-y, x, -z' 'x, -y, z' '-x, y, z' '-y, -x, z' 'y, x, z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' 'x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, x+1/2, z+1/2' _cell_length_a 3.922(2) _cell_length_b 3.922(2) _cell_length_c 13.285(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 204.38(19) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 87 _cell_measurement_theta_min 3.07 _cell_measurement_theta_max 27.39 _exptl_crystal_description plate _exptl_crystal_colour silver _exptl_crystal_size_max 0.02 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.005 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 6.250 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 325 _exptl_absorpt_coefficient_mu 29.490 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.709 _exptl_absorpt_correction_T_max 0.863 _exptl_absorpt_process_details 'via SADABS (Bruker, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'Bruker APEX CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 439 _diffrn_reflns_av_R_equivalents 0.0264 _diffrn_reflns_av_sigmaI/netI 0.0225 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 4 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 27.39 _reflns_number_total 87 _reflns_number_gt 78 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker APEX2' _computing_data_reduction 'Bruker APEX2' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0367P)^2^+0.9011P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0039(18) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 87 _refine_ls_number_parameters 13 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0270 _refine_ls_R_factor_gt 0.0226 _refine_ls_wR_factor_ref 0.0614 _refine_ls_wR_factor_gt 0.0596 _refine_ls_goodness_of_fit_ref 1.175 _refine_ls_restrained_S_all 1.167 _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 Ba1 Ba 0.0000 0.0000 0.0000 0.0190(7) Uani 0.777(10) 16 d SP . . K1 K 0.0000 0.0000 0.0000 0.0190(7) Uani 0.126(13) 16 d SP . . As2 As 0.0000 0.0000 0.35461(12) 0.0119(6) Uani 1 8 d S . . Fe3 Fe 0.0000 0.5000 0.2500 0.0112(6) Uani 1 8 d S . . Sn1 Sn 0.0000 0.0000 0.0961(19) 0.0190(7) Uani 0.048(3) 8 d SP . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ba1 0.0195(8) 0.0195(8) 0.0179(12) 0.000 0.000 0.000 K1 0.0195(8) 0.0195(8) 0.0179(12) 0.000 0.000 0.000 As2 0.0123(6) 0.0123(6) 0.0113(10) 0.000 0.000 0.000 Fe3 0.0098(7) 0.0098(7) 0.0141(13) 0.000 0.000 0.000 Sn1 0.0195(8) 0.0195(8) 0.0179(12) 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 Ba1 Sn1 1.28(2) 17 ? Ba1 Sn1 1.28(2) . ? Ba1 As2 3.3798(16) 25 ? Ba1 As2 3.3798(16) 9_444 ? Ba1 As2 3.3798(16) 25_445 ? Ba1 As2 3.3798(16) 9_554 ? Ba1 As2 3.3798(16) 25_455 ? Ba1 As2 3.3798(16) 25_545 ? Ba1 As2 3.3798(16) 9_454 ? Ba1 As2 3.3798(16) 9_544 ? Ba1 Fe3 3.8570(16) . ? Ba1 Fe3 3.8570(16) 25 ? As2 Fe3 2.4037(13) 25_455 ? As2 Fe3 2.4037(13) 1_545 ? As2 Fe3 2.4037(13) 25 ? As2 Fe3 2.4037(13) . ? As2 Sn1 2.850(6) 25 ? As2 Sn1 2.850(6) 25_445 ? As2 Sn1 2.850(6) 25_455 ? As2 Sn1 2.850(6) 25_545 ? As2 Ba1 3.3798(16) 9 ? As2 K1 3.3798(16) 9 ? As2 Ba1 3.3798(16) 9_445 ? As2 K1 3.3798(16) 9_445 ? Fe3 As2 2.4037(13) 25_455 ? Fe3 As2 2.4037(13) 1_565 ? Fe3 As2 2.4037(13) 25 ? Fe3 Fe3 2.7735(15) 25_565 ? Fe3 Fe3 2.7735(15) 25_455 ? Fe3 Fe3 2.7735(15) 25_465 ? Fe3 Fe3 2.7735(15) 25 ? Fe3 Sn1 2.833(18) . ? Fe3 Sn1 2.833(18) 25 ? Fe3 Sn1 2.833(18) 25_455 ? Fe3 Sn1 2.833(18) 1_565 ? Sn1 Sn1 2.55(5) 17 ? Sn1 Fe3 2.833(18) 25 ? Sn1 Fe3 2.833(18) 25_455 ? Sn1 Fe3 2.833(18) 1_545 ? Sn1 As2 2.850(6) 25 ? Sn1 As2 2.850(6) 25_445 ? Sn1 As2 2.850(6) 25_545 ? Sn1 As2 2.850(6) 25_455 ? Sn1 K1 4.125(8) 1_545 ? 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 Sn1 Ba1 Sn1 180.0 17 . ? Sn1 Ba1 As2 124.85(3) 17 25 ? Sn1 Ba1 As2 55.15(3) . 25 ? Sn1 Ba1 As2 55.15(3) 17 9_444 ? Sn1 Ba1 As2 124.85(3) . 9_444 ? As2 Ba1 As2 180.00(4) 25 9_444 ? Sn1 Ba1 As2 124.85(3) 17 25_445 ? Sn1 Ba1 As2 55.15(3) . 25_445 ? As2 Ba1 As2 110.29(6) 25 25_445 ? As2 Ba1 As2 69.71(6) 9_444 25_445 ? Sn1 Ba1 As2 55.15(3) 17 9_554 ? Sn1 Ba1 As2 124.85(3) . 9_554 ? As2 Ba1 As2 69.71(6) 25 9_554 ? As2 Ba1 As2 110.29(6) 9_444 9_554 ? As2 Ba1 As2 180.00(4) 25_445 9_554 ? Sn1 Ba1 As2 124.85(3) 17 25_455 ? Sn1 Ba1 As2 55.15(3) . 25_455 ? As2 Ba1 As2 70.94(3) 25 25_455 ? As2 Ba1 As2 109.06(3) 9_444 25_455 ? As2 Ba1 As2 70.94(3) 25_445 25_455 ? As2 Ba1 As2 109.06(3) 9_554 25_455 ? Sn1 Ba1 As2 124.85(3) 17 25_545 ? Sn1 Ba1 As2 55.15(3) . 25_545 ? As2 Ba1 As2 70.94(3) 25 25_545 ? As2 Ba1 As2 109.06(3) 9_444 25_545 ? As2 Ba1 As2 70.94(3) 25_445 25_545 ? As2 Ba1 As2 109.06(3) 9_554 25_545 ? As2 Ba1 As2 110.29(6) 25_455 25_545 ? Sn1 Ba1 As2 55.15(3) 17 9_454 ? Sn1 Ba1 As2 124.85(3) . 9_454 ? As2 Ba1 As2 109.06(3) 25 9_454 ? As2 Ba1 As2 70.94(3) 9_444 9_454 ? As2 Ba1 As2 109.06(3) 25_445 9_454 ? As2 Ba1 As2 70.94(3) 9_554 9_454 ? As2 Ba1 As2 69.71(6) 25_455 9_454 ? As2 Ba1 As2 180.00(4) 25_545 9_454 ? Sn1 Ba1 As2 55.15(3) 17 9_544 ? Sn1 Ba1 As2 124.85(3) . 9_544 ? As2 Ba1 As2 109.06(3) 25 9_544 ? As2 Ba1 As2 70.94(3) 9_444 9_544 ? As2 Ba1 As2 109.06(3) 25_445 9_544 ? As2 Ba1 As2 70.94(3) 9_554 9_544 ? As2 Ba1 As2 180.00(4) 25_455 9_544 ? As2 Ba1 As2 69.71(6) 25_545 9_544 ? As2 Ba1 As2 110.29(6) 9_454 9_544 ? Sn1 Ba1 Fe3 149.439(19) 17 . ? Sn1 Ba1 Fe3 30.561(19) . . ? As2 Ba1 Fe3 38.08(2) 25 . ? As2 Ba1 Fe3 141.92(2) 9_444 . ? As2 Ba1 Fe3 78.64(4) 25_445 . ? As2 Ba1 Fe3 101.36(4) 9_554 . ? As2 Ba1 Fe3 38.08(2) 25_455 . ? As2 Ba1 Fe3 78.64(4) 25_545 . ? As2 Ba1 Fe3 101.36(4) 9_454 . ? As2 Ba1 Fe3 141.92(2) 9_544 . ? Sn1 Ba1 Fe3 149.439(19) 17 25 ? Sn1 Ba1 Fe3 30.561(19) . 25 ? As2 Ba1 Fe3 38.08(2) 25 25 ? As2 Ba1 Fe3 141.92(2) 9_444 25 ? As2 Ba1 Fe3 78.64(4) 25_445 25 ? As2 Ba1 Fe3 101.36(4) 9_554 25 ? As2 Ba1 Fe3 78.64(4) 25_455 25 ? As2 Ba1 Fe3 38.08(2) 25_545 25 ? As2 Ba1 Fe3 141.92(2) 9_454 25 ? As2 Ba1 Fe3 101.36(4) 9_544 25 ? Fe3 Ba1 Fe3 42.14(3) . 25 ? Fe3 As2 Fe3 70.47(4) 25_455 1_545 ? Fe3 As2 Fe3 109.35(7) 25_455 25 ? Fe3 As2 Fe3 70.47(4) 1_545 25 ? Fe3 As2 Fe3 70.47(4) 25_455 . ? Fe3 As2 Fe3 109.35(7) 1_545 . ? Fe3 As2 Fe3 70.47(4) 25 . ? Fe3 As2 Sn1 134.0(3) 25_455 25 ? Fe3 As2 Sn1 134.0(3) 1_545 25 ? Fe3 As2 Sn1 64.6(4) 25 25 ? Fe3 As2 Sn1 64.6(4) . 25 ? Fe3 As2 Sn1 64.6(4) 25_455 25_445 ? Fe3 As2 Sn1 64.6(4) 1_545 25_445 ? Fe3 As2 Sn1 134.0(3) 25 25_445 ? Fe3 As2 Sn1 134.0(3) . 25_445 ? Sn1 As2 Sn1 153.4(10) 25 25_445 ? Fe3 As2 Sn1 64.6(4) 25_455 25_455 ? Fe3 As2 Sn1 134.0(3) 1_545 25_455 ? Fe3 As2 Sn1 134.0(3) 25 25_455 ? Fe3 As2 Sn1 64.6(4) . 25_455 ? Sn1 As2 Sn1 87.0(2) 25 25_455 ? Sn1 As2 Sn1 87.0(2) 25_445 25_455 ? Fe3 As2 Sn1 134.0(3) 25_455 25_545 ? Fe3 As2 Sn1 64.6(4) 1_545 25_545 ? Fe3 As2 Sn1 64.6(4) 25 25_545 ? Fe3 As2 Sn1 134.0(3) . 25_545 ? Sn1 As2 Sn1 87.0(2) 25 25_545 ? Sn1 As2 Sn1 87.0(2) 25_445 25_545 ? Sn1 As2 Sn1 153.4(10) 25_455 25_545 ? Fe3 As2 Ba1 143.501(9) 25_455 9 ? Fe3 As2 Ba1 143.501(9) 1_545 9 ? Fe3 As2 Ba1 81.78(3) 25 9 ? Fe3 As2 Ba1 81.78(3) . 9 ? Sn1 As2 Ba1 21.6(5) 25 9 ? Sn1 As2 Ba1 131.9(5) 25_445 9 ? Sn1 As2 Ba1 82.5(3) 25_455 9 ? Sn1 As2 Ba1 82.5(3) 25_545 9 ? Fe3 As2 K1 143.501(9) 25_455 9 ? Fe3 As2 K1 143.501(9) 1_545 9 ? Fe3 As2 K1 81.78(3) 25 9 ? Fe3 As2 K1 81.78(3) . 9 ? Sn1 As2 K1 21.6(5) 25 9 ? Sn1 As2 K1 131.9(5) 25_445 9 ? Sn1 As2 K1 82.5(3) 25_455 9 ? Sn1 As2 K1 82.5(3) 25_545 9 ? Ba1 As2 K1 0.0 9 9 ? Fe3 As2 Ba1 81.78(3) 25_455 9_445 ? Fe3 As2 Ba1 81.78(3) 1_545 9_445 ? Fe3 As2 Ba1 143.501(10) 25 9_445 ? Fe3 As2 Ba1 143.501(10) . 9_445 ? Sn1 As2 Ba1 131.9(5) 25 9_445 ? Sn1 As2 Ba1 21.6(5) 25_445 9_445 ? Sn1 As2 Ba1 82.5(3) 25_455 9_445 ? Sn1 As2 Ba1 82.5(3) 25_545 9_445 ? Ba1 As2 Ba1 110.29(6) 9 9_445 ? K1 As2 Ba1 110.29(6) 9 9_445 ? Fe3 As2 K1 81.78(3) 25_455 9_445 ? Fe3 As2 K1 81.78(3) 1_545 9_445 ? Fe3 As2 K1 143.501(10) 25 9_445 ? Fe3 As2 K1 143.501(10) . 9_445 ? Sn1 As2 K1 131.9(5) 25 9_445 ? Sn1 As2 K1 21.6(5) 25_445 9_445 ? Sn1 As2 K1 82.5(3) 25_455 9_445 ? Sn1 As2 K1 82.5(3) 25_545 9_445 ? Ba1 As2 K1 110.29(6) 9 9_445 ? K1 As2 K1 110.29(6) 9 9_445 ? Ba1 As2 K1 0.0 9_445 9_445 ? As2 Fe3 As2 109.53(4) . 25_455 ? As2 Fe3 As2 109.35(7) . 1_565 ? As2 Fe3 As2 109.53(4) 25_455 1_565 ? As2 Fe3 As2 109.53(4) . 25 ? As2 Fe3 As2 109.35(7) 25_455 25 ? As2 Fe3 As2 109.53(4) 1_565 25 ? As2 Fe3 Fe3 125.235(19) . 25_565 ? As2 Fe3 Fe3 125.235(19) 25_455 25_565 ? As2 Fe3 Fe3 54.765(19) 1_565 25_565 ? As2 Fe3 Fe3 54.765(19) 25 25_565 ? As2 Fe3 Fe3 54.765(19) . 25_455 ? As2 Fe3 Fe3 54.765(19) 25_455 25_455 ? As2 Fe3 Fe3 125.235(19) 1_565 25_455 ? As2 Fe3 Fe3 125.235(19) 25 25_455 ? Fe3 Fe3 Fe3 180.0 25_565 25_455 ? As2 Fe3 Fe3 125.235(19) . 25_465 ? As2 Fe3 Fe3 54.765(19) 25_455 25_465 ? As2 Fe3 Fe3 54.765(19) 1_565 25_465 ? As2 Fe3 Fe3 125.235(19) 25 25_465 ? Fe3 Fe3 Fe3 90.0 25_565 25_465 ? Fe3 Fe3 Fe3 90.0 25_455 25_465 ? As2 Fe3 Fe3 54.765(19) . 25 ? As2 Fe3 Fe3 125.235(19) 25_455 25 ? As2 Fe3 Fe3 125.235(19) 1_565 25 ? As2 Fe3 Fe3 54.765(19) 25 25 ? Fe3 Fe3 Fe3 90.0 25_565 25 ? Fe3 Fe3 Fe3 90.0 25_455 25 ? Fe3 Fe3 Fe3 180.0 25_465 25 ? As2 Fe3 Sn1 81.5(4) . . ? As2 Fe3 Sn1 65.34(16) 25_455 . ? As2 Fe3 Sn1 169.1(4) 1_565 . ? As2 Fe3 Sn1 65.34(16) 25 . ? Fe3 Fe3 Sn1 119.3(2) 25_565 . ? Fe3 Fe3 Sn1 60.7(2) 25_455 . ? Fe3 Fe3 Sn1 119.3(2) 25_465 . ? Fe3 Fe3 Sn1 60.7(2) 25 . ? As2 Fe3 Sn1 65.34(16) . 25 ? As2 Fe3 Sn1 169.1(4) 25_455 25 ? As2 Fe3 Sn1 65.34(16) 1_565 25 ? As2 Fe3 Sn1 81.5(4) 25 25 ? Fe3 Fe3 Sn1 60.7(2) 25_565 25 ? Fe3 Fe3 Sn1 119.3(2) 25_455 25 ? Fe3 Fe3 Sn1 119.3(2) 25_465 25 ? Fe3 Fe3 Sn1 60.7(2) 25 25 ? Sn1 Fe3 Sn1 121.4(4) . 25 ? As2 Fe3 Sn1 65.34(16) . 25_455 ? As2 Fe3 Sn1 81.5(4) 25_455 25_455 ? As2 Fe3 Sn1 65.34(16) 1_565 25_455 ? As2 Fe3 Sn1 169.1(4) 25 25_455 ? Fe3 Fe3 Sn1 119.3(2) 25_565 25_455 ? Fe3 Fe3 Sn1 60.7(2) 25_455 25_455 ? Fe3 Fe3 Sn1 60.7(2) 25_465 25_455 ? Fe3 Fe3 Sn1 119.3(2) 25 25_455 ? Sn1 Fe3 Sn1 121.4(4) . 25_455 ? Sn1 Fe3 Sn1 87.6(7) 25 25_455 ? As2 Fe3 Sn1 169.1(4) . 1_565 ? As2 Fe3 Sn1 65.34(16) 25_455 1_565 ? As2 Fe3 Sn1 81.5(4) 1_565 1_565 ? As2 Fe3 Sn1 65.34(16) 25 1_565 ? Fe3 Fe3 Sn1 60.7(2) 25_565 1_565 ? Fe3 Fe3 Sn1 119.3(2) 25_455 1_565 ? Fe3 Fe3 Sn1 60.7(2) 25_465 1_565 ? Fe3 Fe3 Sn1 119.3(2) 25 1_565 ? Sn1 Fe3 Sn1 87.6(7) . 1_565 ? Sn1 Fe3 Sn1 121.4(4) 25 1_565 ? Sn1 Fe3 Sn1 121.4(4) 25_455 1_565 ? Ba1 Sn1 Sn1 0.0 . 17 ? Ba1 Sn1 Fe3 136.2(4) . . ? Sn1 Sn1 Fe3 136.2(4) 17 . ? Ba1 Sn1 Fe3 136.2(4) . 25 ? Sn1 Sn1 Fe3 136.2(4) 17 25 ? Fe3 Sn1 Fe3 58.6(4) . 25 ? Ba1 Sn1 Fe3 136.2(4) . 25_455 ? Sn1 Sn1 Fe3 136.2(4) 17 25_455 ? Fe3 Sn1 Fe3 58.6(4) . 25_455 ? Fe3 Sn1 Fe3 87.6(7) 25 25_455 ? Ba1 Sn1 Fe3 136.2(4) . 1_545 ? Sn1 Sn1 Fe3 136.2(4) 17 1_545 ? Fe3 Sn1 Fe3 87.6(7) . 1_545 ? Fe3 Sn1 Fe3 58.6(4) 25 1_545 ? Fe3 Sn1 Fe3 58.6(4) 25_455 1_545 ? Ba1 Sn1 As2 103.3(5) . 25 ? Sn1 Sn1 As2 103.3(5) 17 25 ? Fe3 Sn1 As2 50.0(2) . 25 ? Fe3 Sn1 As2 50.0(2) 25 25 ? Fe3 Sn1 As2 108.1(7) 25_455 25 ? Fe3 Sn1 As2 108.1(7) 1_545 25 ? Ba1 Sn1 As2 103.3(5) . 25_445 ? Sn1 Sn1 As2 103.3(5) 17 25_445 ? Fe3 Sn1 As2 108.1(7) . 25_445 ? Fe3 Sn1 As2 108.1(7) 25 25_445 ? Fe3 Sn1 As2 50.0(2) 25_455 25_445 ? Fe3 Sn1 As2 50.0(2) 1_545 25_445 ? As2 Sn1 As2 153.4(10) 25 25_445 ? Ba1 Sn1 As2 103.3(5) . 25_545 ? Sn1 Sn1 As2 103.3(5) 17 25_545 ? Fe3 Sn1 As2 108.1(7) . 25_545 ? Fe3 Sn1 As2 50.0(2) 25 25_545 ? Fe3 Sn1 As2 108.1(7) 25_455 25_545 ? Fe3 Sn1 As2 50.0(2) 1_545 25_545 ? As2 Sn1 As2 87.0(2) 25 25_545 ? As2 Sn1 As2 87.0(2) 25_445 25_545 ? Ba1 Sn1 As2 103.3(5) . 25_455 ? Sn1 Sn1 As2 103.3(5) 17 25_455 ? Fe3 Sn1 As2 50.0(2) . 25_455 ? Fe3 Sn1 As2 108.1(7) 25 25_455 ? Fe3 Sn1 As2 50.0(2) 25_455 25_455 ? Fe3 Sn1 As2 108.1(7) 1_545 25_455 ? As2 Sn1 As2 87.0(2) 25 25_455 ? As2 Sn1 As2 87.0(2) 25_445 25_455 ? As2 Sn1 As2 153.4(10) 25_545 25_455 ? Ba1 Sn1 K1 72.0(3) . 1_545 ? Sn1 Sn1 K1 72.0(3) 17 1_545 ? Fe3 Sn1 K1 151.8(7) . 1_545 ? Fe3 Sn1 K1 102.91(16) 25 1_545 ? Fe3 Sn1 K1 102.91(16) 25_455 1_545 ? Fe3 Sn1 K1 64.22(4) 1_545 1_545 ? As2 Sn1 K1 136.51(10) 25 1_545 ? As2 Sn1 K1 54.32(10) 25_445 1_545 ? As2 Sn1 K1 54.32(10) 25_545 1_545 ? As2 Sn1 K1 136.51(10) 25_455 1_545 ? _diffrn_measured_fraction_theta_max 0.926 _diffrn_reflns_theta_full 27.39 _diffrn_measured_fraction_theta_full 0.926 _refine_diff_density_max 0.957 _refine_diff_density_min -1.061 _refine_diff_density_rms 0.244 # Attachment 'Ba89Sn11Fe2As21r.cif' data_data_0m5 _database_code_depnum_ccdc_archive 'CCDC 734675' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'As2 Ba0.90 Fe2 Sn0.10' _chemical_formula_weight 397.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M I4/mmm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' '-x, y, -z' 'x, -y, -z' 'y, x, -z' '-y, -x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'y+1/2, x+1/2, -z+1/2' '-y+1/2, -x+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z' 'y, -x, -z' '-y, x, -z' 'x, -y, z' '-x, y, z' '-y, -x, z' 'y, x, z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' 'x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, x+1/2, z+1/2' _cell_length_a 3.9297(8) _cell_length_b 3.9297(8) _cell_length_c 13.158(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 203.20(7) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 137 _cell_measurement_theta_min 3.10 _cell_measurement_theta_max 32.75 _exptl_crystal_description plate _exptl_crystal_colour silver _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.005 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 6.489 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 347 _exptl_absorpt_coefficient_mu 32.201 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.686 _exptl_absorpt_correction_T_max 0.851 _exptl_absorpt_process_details 'via SADABS (Bruker, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'Bruker APEX CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 1298 _diffrn_reflns_av_R_equivalents 0.0246 _diffrn_reflns_av_sigmaI/netI 0.0141 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 32.75 _reflns_number_total 137 _reflns_number_gt 130 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker APEX2' _computing_data_reduction 'Bruker APEX2' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0406P)^2^+3.0655P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.009(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 137 _refine_ls_number_parameters 11 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0295 _refine_ls_R_factor_gt 0.0287 _refine_ls_wR_factor_ref 0.0729 _refine_ls_wR_factor_gt 0.0725 _refine_ls_goodness_of_fit_ref 1.198 _refine_ls_restrained_S_all 1.198 _refine_ls_shift/su_max 0.068 _refine_ls_shift/su_mean 0.012 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 Ba1 Ba 0.0000 0.0000 0.0000 0.0145(4) Uani 0.899(4) 16 d SP . . Sn1 Sn 0.0000 0.0000 0.0872(11) 0.0145(4) Uani 0.051(2) 8 d SP . . As2 As 0.0000 0.0000 0.35474(8) 0.0109(4) Uani 1 8 d S . . Fe3 Fe 0.0000 0.5000 0.2500 0.0107(4) Uani 1 8 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 Ba1 0.0161(4) 0.0161(4) 0.0113(5) 0.000 0.000 0.000 Sn1 0.0161(4) 0.0161(4) 0.0113(5) 0.000 0.000 0.000 As2 0.0112(4) 0.0112(4) 0.0102(5) 0.000 0.000 0.000 Fe3 0.0094(5) 0.0094(5) 0.0133(6) 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 Ba1 Sn1 1.148(15) . ? Ba1 Sn1 1.148(15) 17 ? Ba1 As2 3.3726(8) 25 ? Ba1 As2 3.3726(8) 9_444 ? Ba1 As2 3.3726(8) 25_455 ? Ba1 As2 3.3726(8) 25_545 ? Ba1 As2 3.3726(8) 25_445 ? Ba1 As2 3.3726(8) 9_554 ? Ba1 As2 3.3726(8) 9_454 ? Ba1 As2 3.3726(8) 9_544 ? Ba1 Fe3 3.8317(6) 25 ? Ba1 Fe3 3.8317(6) 17 ? Sn1 Sn1 2.30(3) 17 ? Sn1 As2 2.882(4) 25 ? Sn1 As2 2.882(4) 25_445 ? Sn1 As2 2.882(4) 25_455 ? Sn1 As2 2.882(4) 25_545 ? Sn1 Fe3 2.907(11) 25 ? Sn1 Fe3 2.907(11) . ? Sn1 Fe3 2.907(11) 1_545 ? Sn1 Fe3 2.907(11) 25_455 ? As2 Fe3 2.4000(7) 25_455 ? As2 Fe3 2.4000(7) 1_545 ? As2 Fe3 2.4000(7) 25 ? As2 Fe3 2.4000(7) . ? As2 Sn1 2.882(4) 25 ? As2 Sn1 2.882(4) 25_445 ? As2 Sn1 2.882(4) 25_455 ? As2 Sn1 2.882(4) 25_545 ? As2 Ba1 3.3726(8) 9 ? As2 Ba1 3.3726(8) 9_545 ? As2 Ba1 3.3726(8) 9_445 ? As2 Ba1 3.3726(8) 9_455 ? Fe3 As2 2.4001(7) 25_455 ? Fe3 As2 2.4001(7) 1_565 ? Fe3 As2 2.4001(7) 25 ? Fe3 Fe3 2.7787(6) 25_565 ? Fe3 Fe3 2.7787(6) 25_455 ? Fe3 Fe3 2.7787(6) 25_465 ? Fe3 Fe3 2.7787(6) 25 ? Fe3 Sn1 2.907(11) 25 ? Fe3 Sn1 2.907(11) 1_565 ? Fe3 Sn1 2.907(11) 25_455 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Sn1 Ba1 Sn1 180.0 . 17 ? Sn1 Ba1 As2 55.478(17) . 25 ? Sn1 Ba1 As2 124.522(17) 17 25 ? Sn1 Ba1 As2 124.522(17) . 9_444 ? Sn1 Ba1 As2 55.478(17) 17 9_444 ? As2 Ba1 As2 180.00(3) 25 9_444 ? Sn1 Ba1 As2 55.478(17) . 25_455 ? Sn1 Ba1 As2 124.522(17) 17 25_455 ? As2 Ba1 As2 71.266(17) 25 25_455 ? As2 Ba1 As2 108.734(17) 9_444 25_455 ? Sn1 Ba1 As2 55.478(17) . 25_545 ? Sn1 Ba1 As2 124.522(17) 17 25_545 ? As2 Ba1 As2 71.266(17) 25 25_545 ? As2 Ba1 As2 108.734(17) 9_444 25_545 ? As2 Ba1 As2 110.96(3) 25_455 25_545 ? Sn1 Ba1 As2 55.478(17) . 25_445 ? Sn1 Ba1 As2 124.522(17) 17 25_445 ? As2 Ba1 As2 110.96(3) 25 25_445 ? As2 Ba1 As2 69.04(3) 9_444 25_445 ? As2 Ba1 As2 71.266(17) 25_455 25_445 ? As2 Ba1 As2 71.266(17) 25_545 25_445 ? Sn1 Ba1 As2 124.522(17) . 9_554 ? Sn1 Ba1 As2 55.478(17) 17 9_554 ? As2 Ba1 As2 69.04(3) 25 9_554 ? As2 Ba1 As2 110.96(3) 9_444 9_554 ? As2 Ba1 As2 108.734(17) 25_455 9_554 ? As2 Ba1 As2 108.734(17) 25_545 9_554 ? As2 Ba1 As2 180.00(3) 25_445 9_554 ? Sn1 Ba1 As2 124.522(17) . 9_454 ? Sn1 Ba1 As2 55.478(17) 17 9_454 ? As2 Ba1 As2 108.734(17) 25 9_454 ? As2 Ba1 As2 71.266(17) 9_444 9_454 ? As2 Ba1 As2 69.04(3) 25_455 9_454 ? As2 Ba1 As2 180.00(3) 25_545 9_454 ? As2 Ba1 As2 108.734(17) 25_445 9_454 ? As2 Ba1 As2 71.266(17) 9_554 9_454 ? Sn1 Ba1 As2 124.522(17) . 9_544 ? Sn1 Ba1 As2 55.478(17) 17 9_544 ? As2 Ba1 As2 108.734(17) 25 9_544 ? As2 Ba1 As2 71.266(17) 9_444 9_544 ? As2 Ba1 As2 180.00(3) 25_455 9_544 ? As2 Ba1 As2 69.04(3) 25_545 9_544 ? As2 Ba1 As2 108.734(17) 25_445 9_544 ? As2 Ba1 As2 71.266(17) 9_554 9_544 ? As2 Ba1 As2 110.96(3) 9_454 9_544 ? Sn1 Ba1 Fe3 30.850(7) . 25 ? Sn1 Ba1 Fe3 149.150(7) 17 25 ? As2 Ba1 Fe3 38.253(13) 25 25 ? As2 Ba1 Fe3 141.747(13) 9_444 25 ? As2 Ba1 Fe3 79.176(19) 25_455 25 ? As2 Ba1 Fe3 38.253(13) 25_545 25 ? As2 Ba1 Fe3 79.176(19) 25_445 25 ? As2 Ba1 Fe3 100.824(19) 9_554 25 ? As2 Ba1 Fe3 141.747(13) 9_454 25 ? As2 Ba1 Fe3 100.824(19) 9_544 25 ? Sn1 Ba1 Fe3 149.150(7) . 17 ? Sn1 Ba1 Fe3 30.850(7) 17 17 ? As2 Ba1 Fe3 141.747(13) 25 17 ? As2 Ba1 Fe3 38.253(13) 9_444 17 ? As2 Ba1 Fe3 141.747(13) 25_455 17 ? As2 Ba1 Fe3 100.824(19) 25_545 17 ? As2 Ba1 Fe3 100.824(19) 25_445 17 ? As2 Ba1 Fe3 79.176(19) 9_554 17 ? As2 Ba1 Fe3 79.176(19) 9_454 17 ? As2 Ba1 Fe3 38.253(13) 9_544 17 ? Fe3 Ba1 Fe3 137.481(10) 25 17 ? Ba1 Sn1 Sn1 0.0 . 17 ? Ba1 Sn1 As2 105.4(3) . 25 ? Sn1 Sn1 As2 105.4(3) 17 25 ? Ba1 Sn1 As2 105.4(3) . 25_445 ? Sn1 Sn1 As2 105.4(3) 17 25_445 ? As2 Sn1 As2 149.3(6) 25 25_445 ? Ba1 Sn1 As2 105.4(3) . 25_455 ? Sn1 Sn1 As2 105.4(3) 17 25_455 ? As2 Sn1 As2 85.97(15) 25 25_455 ? As2 Sn1 As2 85.97(15) 25_445 25_455 ? Ba1 Sn1 As2 105.4(3) . 25_545 ? Sn1 Sn1 As2 105.4(3) 17 25_545 ? As2 Sn1 As2 85.97(15) 25 25_545 ? As2 Sn1 As2 85.97(15) 25_445 25_545 ? As2 Sn1 As2 149.3(6) 25_455 25_545 ? Ba1 Sn1 Fe3 137.5(2) . 25 ? Sn1 Sn1 Fe3 137.5(2) 17 25 ? As2 Sn1 Fe3 48.99(14) 25 25 ? As2 Sn1 Fe3 105.4(4) 25_445 25 ? As2 Sn1 Fe3 105.4(4) 25_455 25 ? As2 Sn1 Fe3 48.99(14) 25_545 25 ? Ba1 Sn1 Fe3 137.5(2) . . ? Sn1 Sn1 Fe3 137.5(2) 17 . ? As2 Sn1 Fe3 48.99(14) 25 . ? As2 Sn1 Fe3 105.4(4) 25_445 . ? As2 Sn1 Fe3 48.99(14) 25_455 . ? As2 Sn1 Fe3 105.4(4) 25_545 . ? Fe3 Sn1 Fe3 57.1(2) 25 . ? Ba1 Sn1 Fe3 137.5(2) . 1_545 ? Sn1 Sn1 Fe3 137.5(2) 17 1_545 ? As2 Sn1 Fe3 105.4(4) 25 1_545 ? As2 Sn1 Fe3 48.99(14) 25_445 1_545 ? As2 Sn1 Fe3 105.4(4) 25_455 1_545 ? As2 Sn1 Fe3 48.99(14) 25_545 1_545 ? Fe3 Sn1 Fe3 57.1(2) 25 1_545 ? Fe3 Sn1 Fe3 85.1(4) . 1_545 ? Ba1 Sn1 Fe3 137.5(2) . 25_455 ? Sn1 Sn1 Fe3 137.5(2) 17 25_455 ? As2 Sn1 Fe3 105.4(4) 25 25_455 ? As2 Sn1 Fe3 48.99(14) 25_445 25_455 ? As2 Sn1 Fe3 48.99(14) 25_455 25_455 ? As2 Sn1 Fe3 105.4(4) 25_545 25_455 ? Fe3 Sn1 Fe3 85.1(4) 25 25_455 ? Fe3 Sn1 Fe3 57.1(2) . 25_455 ? Fe3 Sn1 Fe3 57.1(2) 1_545 25_455 ? Fe3 As2 Fe3 70.74(2) 25_455 1_545 ? Fe3 As2 Fe3 109.90(5) 25_455 25 ? Fe3 As2 Fe3 70.74(2) 1_545 25 ? Fe3 As2 Fe3 70.74(2) 25_455 . ? Fe3 As2 Fe3 109.90(5) 1_545 . ? Fe3 As2 Fe3 70.74(2) 25 . ? Fe3 As2 Sn1 135.27(16) 25_455 25 ? Fe3 As2 Sn1 135.27(16) 1_545 25 ? Fe3 As2 Sn1 66.0(2) 25 25 ? Fe3 As2 Sn1 66.0(2) . 25 ? Fe3 As2 Sn1 66.0(2) 25_455 25_445 ? Fe3 As2 Sn1 66.0(2) 1_545 25_445 ? Fe3 As2 Sn1 135.27(16) 25 25_445 ? Fe3 As2 Sn1 135.27(16) . 25_445 ? Sn1 As2 Sn1 149.3(6) 25 25_445 ? Fe3 As2 Sn1 66.0(2) 25_455 25_455 ? Fe3 As2 Sn1 135.27(16) 1_545 25_455 ? Fe3 As2 Sn1 135.27(16) 25 25_455 ? Fe3 As2 Sn1 66.0(2) . 25_455 ? Sn1 As2 Sn1 85.97(15) 25 25_455 ? Sn1 As2 Sn1 85.97(15) 25_445 25_455 ? Fe3 As2 Sn1 135.27(16) 25_455 25_545 ? Fe3 As2 Sn1 66.0(2) 1_545 25_545 ? Fe3 As2 Sn1 66.0(2) 25 25_545 ? Fe3 As2 Sn1 135.27(16) . 25_545 ? Sn1 As2 Sn1 85.97(15) 25 25_545 ? Sn1 As2 Sn1 85.97(15) 25_445 25_545 ? Sn1 As2 Sn1 149.3(6) 25_455 25_545 ? Fe3 As2 Ba1 143.360(4) 25_455 9 ? Fe3 As2 Ba1 143.360(4) 1_545 9 ? Fe3 As2 Ba1 81.286(14) 25 9 ? Fe3 As2 Ba1 81.286(14) . 9 ? Sn1 As2 Ba1 19.2(3) 25 9 ? Sn1 As2 Ba1 130.1(3) 25_445 9 ? Sn1 As2 Ba1 81.36(16) 25_455 9 ? Sn1 As2 Ba1 81.36(16) 25_545 9 ? Fe3 As2 Ba1 143.360(4) 25_455 9_545 ? Fe3 As2 Ba1 81.286(14) 1_545 9_545 ? Fe3 As2 Ba1 81.286(14) 25 9_545 ? Fe3 As2 Ba1 143.360(4) . 9_545 ? Sn1 As2 Ba1 81.36(16) 25 9_545 ? Sn1 As2 Ba1 81.36(16) 25_445 9_545 ? Sn1 As2 Ba1 130.1(3) 25_455 9_545 ? Sn1 As2 Ba1 19.2(3) 25_545 9_545 ? Ba1 As2 Ba1 71.266(17) 9 9_545 ? Fe3 As2 Ba1 81.286(14) 25_455 9_445 ? Fe3 As2 Ba1 81.286(14) 1_545 9_445 ? Fe3 As2 Ba1 143.360(4) 25 9_445 ? Fe3 As2 Ba1 143.360(4) . 9_445 ? Sn1 As2 Ba1 130.1(3) 25 9_445 ? Sn1 As2 Ba1 19.2(3) 25_445 9_445 ? Sn1 As2 Ba1 81.36(16) 25_455 9_445 ? Sn1 As2 Ba1 81.36(16) 25_545 9_445 ? Ba1 As2 Ba1 110.96(3) 9 9_445 ? Ba1 As2 Ba1 71.266(17) 9_545 9_445 ? Fe3 As2 Ba1 81.286(14) 25_455 9_455 ? Fe3 As2 Ba1 143.360(4) 1_545 9_455 ? Fe3 As2 Ba1 143.360(4) 25 9_455 ? Fe3 As2 Ba1 81.286(14) . 9_455 ? Sn1 As2 Ba1 81.36(16) 25 9_455 ? Sn1 As2 Ba1 81.36(16) 25_445 9_455 ? Sn1 As2 Ba1 19.2(3) 25_455 9_455 ? Sn1 As2 Ba1 130.1(3) 25_545 9_455 ? Ba1 As2 Ba1 71.266(17) 9 9_455 ? Ba1 As2 Ba1 110.96(3) 9_545 9_455 ? Ba1 As2 Ba1 71.266(17) 9_445 9_455 ? As2 Fe3 As2 109.26(2) . 25_455 ? As2 Fe3 As2 109.90(5) . 1_565 ? As2 Fe3 As2 109.26(2) 25_455 1_565 ? As2 Fe3 As2 109.26(2) . 25 ? As2 Fe3 As2 109.90(5) 25_455 25 ? As2 Fe3 As2 109.26(2) 1_565 25 ? As2 Fe3 Fe3 125.372(11) . 25_565 ? As2 Fe3 Fe3 125.372(11) 25_455 25_565 ? As2 Fe3 Fe3 54.628(11) 1_565 25_565 ? As2 Fe3 Fe3 54.628(11) 25 25_565 ? As2 Fe3 Fe3 54.628(11) . 25_455 ? As2 Fe3 Fe3 54.628(11) 25_455 25_455 ? As2 Fe3 Fe3 125.372(11) 1_565 25_455 ? As2 Fe3 Fe3 125.372(11) 25 25_455 ? Fe3 Fe3 Fe3 180.0 25_565 25_455 ? As2 Fe3 Fe3 125.372(11) . 25_465 ? As2 Fe3 Fe3 54.628(11) 25_455 25_465 ? As2 Fe3 Fe3 54.628(11) 1_565 25_465 ? As2 Fe3 Fe3 125.372(11) 25 25_465 ? Fe3 Fe3 Fe3 90.0 25_565 25_465 ? Fe3 Fe3 Fe3 90.0 25_455 25_465 ? As2 Fe3 Fe3 54.628(11) . 25 ? As2 Fe3 Fe3 125.372(11) 25_455 25 ? As2 Fe3 Fe3 125.372(11) 1_565 25 ? As2 Fe3 Fe3 54.628(11) 25 25 ? Fe3 Fe3 Fe3 90.0 25_565 25 ? Fe3 Fe3 Fe3 90.0 25_455 25 ? Fe3 Fe3 Fe3 180.0 25_465 25 ? As2 Fe3 Sn1 64.96(9) . 25 ? As2 Fe3 Sn1 167.6(2) 25_455 25 ? As2 Fe3 Sn1 64.96(9) 1_565 25 ? As2 Fe3 Sn1 82.5(2) 25 25 ? Fe3 Fe3 Sn1 61.45(12) 25_565 25 ? Fe3 Fe3 Sn1 118.55(12) 25_455 25 ? Fe3 Fe3 Sn1 118.55(12) 25_465 25 ? Fe3 Fe3 Sn1 61.45(12) 25 25 ? As2 Fe3 Sn1 167.6(2) . 1_565 ? As2 Fe3 Sn1 64.96(9) 25_455 1_565 ? As2 Fe3 Sn1 82.5(2) 1_565 1_565 ? As2 Fe3 Sn1 64.96(9) 25 1_565 ? Fe3 Fe3 Sn1 61.45(12) 25_565 1_565 ? Fe3 Fe3 Sn1 118.55(12) 25_455 1_565 ? Fe3 Fe3 Sn1 61.45(12) 25_465 1_565 ? Fe3 Fe3 Sn1 118.55(12) 25 1_565 ? Sn1 Fe3 Sn1 122.9(2) 25 1_565 ? As2 Fe3 Sn1 64.96(9) . 25_455 ? As2 Fe3 Sn1 82.5(2) 25_455 25_455 ? As2 Fe3 Sn1 64.96(9) 1_565 25_455 ? As2 Fe3 Sn1 167.6(2) 25 25_455 ? Fe3 Fe3 Sn1 118.55(12) 25_565 25_455 ? Fe3 Fe3 Sn1 61.45(12) 25_455 25_455 ? Fe3 Fe3 Sn1 61.45(12) 25_465 25_455 ? Fe3 Fe3 Sn1 118.55(12) 25 25_455 ? Sn1 Fe3 Sn1 85.1(4) 25 25_455 ? Sn1 Fe3 Sn1 122.9(2) 1_565 25_455 ? As2 Fe3 Sn1 82.5(2) . . ? As2 Fe3 Sn1 64.96(9) 25_455 . ? As2 Fe3 Sn1 167.6(2) 1_565 . ? As2 Fe3 Sn1 64.96(9) 25 . ? Fe3 Fe3 Sn1 118.55(12) 25_565 . ? Fe3 Fe3 Sn1 61.45(12) 25_455 . ? Fe3 Fe3 Sn1 118.55(12) 25_465 . ? Fe3 Fe3 Sn1 61.45(12) 25 . ? Sn1 Fe3 Sn1 122.9(2) 25 . ? Sn1 Fe3 Sn1 85.1(4) 1_565 . ? Sn1 Fe3 Sn1 122.9(2) 25_455 . ? _diffrn_measured_fraction_theta_max 0.958 _diffrn_reflns_theta_full 32.75 _diffrn_measured_fraction_theta_full 0.958 _refine_diff_density_max 3.068 _refine_diff_density_min -2.606 _refine_diff_density_rms 0.491