# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Phelan, W.' 'Nguyen, Giang' 'Young, David' 'Chan, Julia' 'Karki, Amar' _publ_contact_author_name 'Chan, Julia' _publ_contact_author_email jchan@lsu.edu _publ_section_title ; Synthesis, Structure, Magnetic and Transport Properties of LnFeSb3 (Ln = Pr, Nd, Sm, Gd, and Tb) Tuning of Anisotropic Long-range Magnetic Order as a Function of Ln ; # Attachment '- GdFeSb3.cif' data_GdFeSb3 _database_code_depnum_ccdc_archive 'CCDC 768388' #TrackingRef '- GdFeSb3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Gd Fe Sb3' _chemical_formula_sum 'Fe Gd Sb3' _chemical_formula_weight 578.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Gd Gd -0.1653 3.9035 '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' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P b c m ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z-1/2' '-x, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 12.4700(2) _cell_length_b 6.1350(4) _cell_length_c 12.0640(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 922.94(7) _cell_formula_units_Z 8 _cell_measurement_temperature 298(5) _cell_measurement_reflns_used 1519 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 8.324 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1944 _exptl_absorpt_coefficient_mu 34.369 _exptl_absorpt_correction_type sphere _exptl_absorpt_correction_T_min 0.1304 _exptl_absorpt_correction_T_max 0.1825 _exptl_absorpt_process_details 'HKL Scalepack (Otwinowski & Minor 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(5) _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 'Nonius KappaCCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2531 _diffrn_reflns_av_R_equivalents 0.0365 _diffrn_reflns_av_sigmaI/netI 0.0432 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 30.04 _reflns_number_total 1409 _reflns_number_gt 1260 _reflns_threshold_expression I>2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0139P)^2^+14.1908P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens ? _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00132(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1409 _refine_ls_number_parameters 53 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0343 _refine_ls_R_factor_gt 0.0288 _refine_ls_wR_factor_ref 0.0706 _refine_ls_wR_factor_gt 0.0651 _refine_ls_goodness_of_fit_ref 1.156 _refine_ls_restrained_S_all 1.156 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd1 Gd 0.69917(4) 0.2500 0.0000 0.00822(13) Uani 1 2 d S . . Gd2 Gd 0.30761(4) 0.27811(9) 0.7500 0.00822(13) Uani 1 2 d S . . Fe1 Fe 0.10361(9) 0.03721(18) 0.86072(9) 0.0115(2) Uani 1 1 d . . . Sb1 Sb 0.97146(5) 0.2500 0.0000 0.00932(17) Uani 1 2 d S . . Sb2 Sb 0.77617(6) 0.26331(11) 0.7500 0.00852(16) Uani 1 2 d S . . Sb3 Sb 0.50319(4) 0.51259(8) 0.87641(4) 0.00842(14) Uani 1 1 d . . . Sb4 Sb 0.22661(6) 0.2500 0.0000 0.00832(16) Uani 1 2 d S . . Sb5 Sb 0.93905(5) 0.89508(11) 0.7500 0.00939(17) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.0051(3) 0.0106(3) 0.0090(3) -0.00044(17) 0.000 0.000 Gd2 0.0042(2) 0.0112(2) 0.0092(3) 0.000 0.000 0.00017(17) Fe1 0.0082(5) 0.0139(5) 0.0123(5) -0.0010(4) 0.0005(4) -0.0006(4) Sb1 0.0059(3) 0.0104(3) 0.0117(3) 0.0006(2) 0.000 0.000 Sb2 0.0060(3) 0.0102(3) 0.0093(3) 0.000 0.000 -0.0012(2) Sb3 0.0051(3) 0.0111(2) 0.0090(3) -0.00015(16) -0.00020(17) -0.00026(16) Sb4 0.0062(3) 0.0104(3) 0.0084(3) -0.0009(2) 0.000 0.000 Sb5 0.0052(3) 0.0109(3) 0.0121(3) 0.000 0.000 -0.0012(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 Sb2 3.1662(3) 3_556 ? Gd1 Sb2 3.1662(3) 1_554 ? Gd1 Sb4 3.2041(3) 5_655 ? Gd1 Sb4 3.2041(3) 5_665 ? Gd1 Sb3 3.2729(6) 5_666 ? Gd1 Sb3 3.2729(6) 7_654 ? Gd1 Sb3 3.2849(6) 1_554 ? Gd1 Sb3 3.2849(6) 3_556 ? Gd1 Sb1 3.3955(8) . ? Gd1 Fe1 3.4606(12) 5_656 ? Gd1 Fe1 3.4606(12) 7_664 ? Gd2 Sb2 3.1548(9) 7_665 ? Gd2 Sb5 3.1586(8) 7_655 ? Gd2 Sb4 3.1853(3) 6_556 ? Gd2 Sb4 3.1853(3) 1_556 ? Gd2 Sb3 3.2160(6) . ? Gd2 Sb3 3.2160(6) 6_557 ? Gd2 Fe1 3.2311(12) . ? Gd2 Fe1 3.2311(12) 6_557 ? Gd2 Sb3 3.2474(7) 7_655 ? Gd2 Sb3 3.2474(7) 4_646 ? Gd2 Sb2 3.3266(9) 7_655 ? Fe1 Sb5 2.5991(12) 1_445 ? Fe1 Sb1 2.6085(11) 5_656 ? Fe1 Sb2 2.6182(12) 7_655 ? Fe1 Sb4 2.6230(12) 1_556 ? Fe1 Sb5 2.6245(13) 7_655 ? Fe1 Fe1 2.672(2) 6_557 ? Fe1 Sb1 2.6914(12) 1_456 ? Fe1 Gd1 3.4607(12) 5_656 ? Sb1 Fe1 2.6085(11) 5_656 ? Sb1 Fe1 2.6085(11) 7_664 ? Sb1 Fe1 2.6913(12) 1_654 ? Sb1 Fe1 2.6913(12) 3_656 ? Sb1 Sb1 3.1490(4) 5_755 ? Sb1 Sb1 3.1490(4) 5_765 ? Sb1 Sb4 3.1817(10) 1_655 ? Sb2 Fe1 2.6182(12) 7_665 ? Sb2 Fe1 2.6182(12) 4_656 ? Sb2 Sb5 3.0379(10) 1_545 ? Sb2 Gd2 3.1547(9) 7_655 ? Sb2 Gd1 3.1662(3) 6_556 ? Sb2 Gd1 3.1662(3) 1_556 ? Sb2 Gd2 3.3266(9) 7_665 ? Sb3 Sb3 2.9870(9) 5_667 ? Sb3 Sb3 3.0501(9) 6_557 ? Sb3 Sb3 3.0685(2) 7_665 ? Sb3 Sb3 3.0685(2) 7_655 ? Sb3 Gd2 3.2474(7) 7_665 ? Sb3 Gd1 3.2729(6) 5_666 ? Sb3 Gd1 3.2849(6) 1_556 ? Sb4 Fe1 2.6230(12) 1_554 ? Sb4 Fe1 2.6230(12) 3_556 ? Sb4 Sb1 3.1817(10) 1_455 ? Sb4 Gd2 3.1853(3) 3_556 ? Sb4 Gd2 3.1853(3) 1_554 ? Sb4 Gd1 3.2041(3) 5_655 ? Sb4 Gd1 3.2041(3) 5_665 ? Sb5 Fe1 2.5992(12) 1_665 ? Sb5 Fe1 2.5992(12) 6_667 ? Sb5 Fe1 2.6245(13) 4_656 ? Sb5 Fe1 2.6245(13) 7_665 ? Sb5 Sb2 3.0379(10) 1_565 ? Sb5 Gd2 3.1585(8) 7_665 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Sb2 Gd1 Sb2 144.69(3) 3_556 1_554 ? Sb2 Gd1 Sb4 83.552(14) 3_556 5_655 ? Sb2 Gd1 Sb4 86.392(14) 1_554 5_655 ? Sb2 Gd1 Sb4 86.393(14) 3_556 5_665 ? Sb2 Gd1 Sb4 83.552(14) 1_554 5_665 ? Sb4 Gd1 Sb4 146.42(3) 5_655 5_665 ? Sb2 Gd1 Sb3 79.128(15) 3_556 5_666 ? Sb2 Gd1 Sb3 131.017(17) 1_554 5_666 ? Sb4 Gd1 Sb3 130.448(16) 5_655 5_666 ? Sb4 Gd1 Sb3 78.268(14) 5_665 5_666 ? Sb2 Gd1 Sb3 131.017(17) 3_556 7_654 ? Sb2 Gd1 Sb3 79.127(15) 1_554 7_654 ? Sb4 Gd1 Sb3 78.267(14) 5_655 7_654 ? Sb4 Gd1 Sb3 130.449(16) 5_665 7_654 ? Sb3 Gd1 Sb3 79.11(2) 5_666 7_654 ? Sb2 Gd1 Sb3 132.116(17) 3_556 1_554 ? Sb2 Gd1 Sb3 77.328(15) 1_554 1_554 ? Sb4 Gd1 Sb3 133.190(16) 5_655 1_554 ? Sb4 Gd1 Sb3 75.250(15) 5_665 1_554 ? Sb3 Gd1 Sb3 54.192(15) 5_666 1_554 ? Sb3 Gd1 Sb3 55.798(9) 7_654 1_554 ? Sb2 Gd1 Sb3 77.328(15) 3_556 3_556 ? Sb2 Gd1 Sb3 132.115(17) 1_554 3_556 ? Sb4 Gd1 Sb3 75.249(15) 5_655 3_556 ? Sb4 Gd1 Sb3 133.190(16) 5_665 3_556 ? Sb3 Gd1 Sb3 55.798(9) 5_666 3_556 ? Sb3 Gd1 Sb3 54.192(15) 7_654 3_556 ? Sb3 Gd1 Sb3 83.86(2) 1_554 3_556 ? Sb2 Gd1 Sb1 72.345(15) 3_556 . ? Sb2 Gd1 Sb1 72.345(15) 1_554 . ? Sb4 Gd1 Sb1 73.210(15) 5_655 . ? Sb4 Gd1 Sb1 73.210(15) 5_665 . ? Sb3 Gd1 Sb1 140.443(10) 5_666 . ? Sb3 Gd1 Sb1 140.443(10) 7_654 . ? Sb3 Gd1 Sb1 138.070(10) 1_554 . ? Sb3 Gd1 Sb1 138.070(10) 3_556 . ? Sb2 Gd1 Fe1 46.28(2) 3_556 5_656 ? Sb2 Gd1 Fe1 105.08(2) 1_554 5_656 ? Sb4 Gd1 Fe1 46.15(2) 5_655 5_656 ? Sb4 Gd1 Fe1 106.39(2) 5_665 5_656 ? Sb3 Gd1 Fe1 123.59(2) 5_666 5_656 ? Sb3 Gd1 Fe1 122.85(2) 7_654 5_656 ? Sb3 Gd1 Fe1 177.16(2) 1_554 5_656 ? Sb3 Gd1 Fe1 93.36(2) 3_556 5_656 ? Sb1 Gd1 Fe1 44.712(19) . 5_656 ? Sb2 Gd1 Fe1 105.08(2) 3_556 7_664 ? Sb2 Gd1 Fe1 46.28(2) 1_554 7_664 ? Sb4 Gd1 Fe1 106.39(2) 5_655 7_664 ? Sb4 Gd1 Fe1 46.15(2) 5_665 7_664 ? Sb3 Gd1 Fe1 122.85(2) 5_666 7_664 ? Sb3 Gd1 Fe1 123.59(2) 7_654 7_664 ? Sb3 Gd1 Fe1 93.36(2) 1_554 7_664 ? Sb3 Gd1 Fe1 177.16(2) 3_556 7_664 ? Sb1 Gd1 Fe1 44.712(19) . 7_664 ? Fe1 Gd1 Fe1 89.42(4) 5_656 7_664 ? Sb2 Gd2 Sb5 57.53(2) 7_665 7_655 ? Sb2 Gd2 Sb4 86.907(12) 7_665 6_556 ? Sb5 Gd2 Sb4 72.751(15) 7_655 6_556 ? Sb2 Gd2 Sb4 86.907(12) 7_665 1_556 ? Sb5 Gd2 Sb4 72.751(15) 7_655 1_556 ? Sb4 Gd2 Sb4 142.47(3) 6_556 1_556 ? Sb2 Gd2 Sb3 80.160(18) 7_665 . ? Sb5 Gd2 Sb3 129.558(19) 7_655 . ? Sb4 Gd2 Sb3 135.535(18) 6_556 . ? Sb4 Gd2 Sb3 79.380(14) 1_556 . ? Sb2 Gd2 Sb3 80.160(18) 7_665 6_557 ? Sb5 Gd2 Sb3 129.558(19) 7_655 6_557 ? Sb4 Gd2 Sb3 79.380(14) 6_556 6_557 ? Sb4 Gd2 Sb3 135.535(18) 1_556 6_557 ? Sb3 Gd2 Sb3 56.614(18) . 6_557 ? Sb2 Gd2 Fe1 99.84(3) 7_665 . ? Sb5 Gd2 Fe1 48.49(2) 7_655 . ? Sb4 Gd2 Fe1 96.72(3) 6_556 . ? Sb4 Gd2 Fe1 48.25(2) 1_556 . ? Sb3 Gd2 Fe1 127.27(2) . . ? Sb3 Gd2 Fe1 176.10(2) 6_557 . ? Sb2 Gd2 Fe1 99.84(3) 7_665 6_557 ? Sb5 Gd2 Fe1 48.49(2) 7_655 6_557 ? Sb4 Gd2 Fe1 48.25(2) 6_556 6_557 ? Sb4 Gd2 Fe1 96.72(3) 1_556 6_557 ? Sb3 Gd2 Fe1 176.10(2) . 6_557 ? Sb3 Gd2 Fe1 127.27(2) 6_557 6_557 ? Fe1 Gd2 Fe1 48.84(4) . 6_557 ? Sb2 Gd2 Sb3 135.556(18) 7_665 7_655 ? Sb5 Gd2 Sb3 145.234(16) 7_655 7_655 ? Sb4 Gd2 Sb3 130.383(18) 6_556 7_655 ? Sb4 Gd2 Sb3 76.029(14) 1_556 7_655 ? Sb3 Gd2 Sb3 56.684(9) . 7_655 ? Sb3 Gd2 Sb3 84.038(15) 6_557 7_655 ? Fe1 Gd2 Sb3 98.53(2) . 7_655 ? Fe1 Gd2 Sb3 122.46(3) 6_557 7_655 ? Sb2 Gd2 Sb3 135.556(18) 7_665 4_646 ? Sb5 Gd2 Sb3 145.234(16) 7_655 4_646 ? Sb4 Gd2 Sb3 76.029(14) 6_556 4_646 ? Sb4 Gd2 Sb3 130.383(18) 1_556 4_646 ? Sb3 Gd2 Sb3 84.038(15) . 4_646 ? Sb3 Gd2 Sb3 56.684(9) 6_557 4_646 ? Fe1 Gd2 Sb3 122.46(3) . 4_646 ? Fe1 Gd2 Sb3 98.53(2) 6_557 4_646 ? Sb3 Gd2 Sb3 56.020(18) 7_655 4_646 ? Sb2 Gd2 Sb2 142.35(3) 7_665 7_655 ? Sb5 Gd2 Sb2 84.83(2) 7_655 7_655 ? Sb4 Gd2 Sb2 81.316(11) 6_556 7_655 ? Sb4 Gd2 Sb2 81.316(11) 1_556 7_655 ? Sb3 Gd2 Sb2 131.517(18) . 7_655 ? Sb3 Gd2 Sb2 131.517(18) 6_557 7_655 ? Fe1 Gd2 Sb2 47.04(2) . 7_655 ? Fe1 Gd2 Sb2 47.04(2) 6_557 7_655 ? Sb3 Gd2 Sb2 75.638(17) 7_655 7_655 ? Sb3 Gd2 Sb2 75.638(17) 4_646 7_655 ? Sb5 Fe1 Sb1 79.69(3) 1_445 5_656 ? Sb5 Fe1 Sb2 88.54(4) 1_445 7_655 ? Sb1 Fe1 Sb2 95.77(4) 5_656 7_655 ? Sb5 Fe1 Sb4 163.31(5) 1_445 1_556 ? Sb1 Fe1 Sb4 97.67(4) 5_656 1_556 ? Sb2 Fe1 Sb4 108.15(4) 7_655 1_556 ? Sb5 Fe1 Sb5 81.90(3) 1_445 7_655 ? Sb1 Fe1 Sb5 145.10(5) 5_656 7_655 ? Sb2 Fe1 Sb5 113.16(4) 7_655 7_655 ? Sb4 Fe1 Sb5 91.62(4) 1_556 7_655 ? Sb5 Fe1 Fe1 59.07(3) 1_445 6_557 ? Sb1 Fe1 Fe1 130.10(2) 5_656 6_557 ? Sb2 Fe1 Fe1 59.32(3) 7_655 6_557 ? Sb4 Fe1 Fe1 129.84(2) 1_556 6_557 ? Sb5 Fe1 Fe1 59.41(2) 7_655 6_557 ? Sb5 Fe1 Sb1 90.01(4) 1_445 1_456 ? Sb1 Fe1 Sb1 72.89(3) 5_656 1_456 ? Sb2 Fe1 Sb1 168.64(5) 7_655 1_456 ? Sb4 Fe1 Sb1 73.54(3) 1_556 1_456 ? Sb5 Fe1 Sb1 77.75(3) 7_655 1_456 ? Fe1 Fe1 Sb1 128.63(3) 6_557 1_456 ? Sb5 Fe1 Gd2 124.24(4) 1_445 . ? Sb1 Fe1 Gd2 149.07(4) 5_656 . ? Sb2 Fe1 Gd2 68.40(3) 7_655 . ? Sb4 Fe1 Gd2 64.96(3) 1_556 . ? Sb5 Fe1 Gd2 64.31(3) 7_655 . ? Fe1 Fe1 Gd2 65.58(2) 6_557 . ? Sb1 Fe1 Gd2 121.22(4) 1_456 . ? Sb5 Fe1 Gd1 129.78(4) 1_445 5_656 ? Sb1 Fe1 Gd1 66.32(3) 5_656 5_656 ? Sb2 Fe1 Gd1 60.93(2) 7_655 5_656 ? Sb4 Fe1 Gd1 61.76(2) 1_556 5_656 ? Sb5 Fe1 Gd1 144.80(4) 7_655 5_656 ? Fe1 Fe1 Gd1 119.047(18) 6_557 5_656 ? Sb1 Fe1 Gd1 112.27(4) 1_456 5_656 ? Gd2 Fe1 Gd1 82.77(3) . 5_656 ? Fe1 Sb1 Fe1 137.93(6) 5_656 7_664 ? Fe1 Sb1 Fe1 107.11(3) 5_656 1_654 ? Fe1 Sb1 Fe1 98.35(4) 7_664 1_654 ? Fe1 Sb1 Fe1 98.35(4) 5_656 3_656 ? Fe1 Sb1 Fe1 107.11(3) 7_664 3_656 ? Fe1 Sb1 Fe1 104.49(5) 1_654 3_656 ? Fe1 Sb1 Sb1 54.77(2) 5_656 5_755 ? Fe1 Sb1 Sb1 137.66(3) 7_664 5_755 ? Fe1 Sb1 Sb1 52.34(3) 1_654 5_755 ? Fe1 Sb1 Sb1 109.52(3) 3_656 5_755 ? Fe1 Sb1 Sb1 137.66(3) 5_656 5_765 ? Fe1 Sb1 Sb1 54.77(2) 7_664 5_765 ? Fe1 Sb1 Sb1 109.52(3) 1_654 5_765 ? Fe1 Sb1 Sb1 52.34(3) 3_656 5_765 ? Sb1 Sb1 Sb1 153.87(5) 5_755 5_765 ? Fe1 Sb1 Sb4 111.03(3) 5_656 1_655 ? Fe1 Sb1 Sb4 111.03(3) 7_664 1_655 ? Fe1 Sb1 Sb4 52.24(3) 1_654 1_655 ? Fe1 Sb1 Sb4 52.24(3) 3_656 1_655 ? Sb1 Sb1 Sb4 76.94(2) 5_755 1_655 ? Sb1 Sb1 Sb4 76.94(2) 5_765 1_655 ? Fe1 Sb1 Gd1 68.97(3) 5_656 . ? Fe1 Sb1 Gd1 68.97(3) 7_664 . ? Fe1 Sb1 Gd1 127.76(3) 1_654 . ? Fe1 Sb1 Gd1 127.76(3) 3_656 . ? Sb1 Sb1 Gd1 103.06(2) 5_755 . ? Sb1 Sb1 Gd1 103.06(2) 5_765 . ? Sb4 Sb1 Gd1 180.0 1_655 . ? Fe1 Sb2 Fe1 61.35(5) 7_665 4_656 ? Fe1 Sb2 Sb5 95.42(3) 7_665 1_545 ? Fe1 Sb2 Sb5 95.42(3) 4_656 1_545 ? Fe1 Sb2 Gd2 142.67(3) 7_665 7_655 ? Fe1 Sb2 Gd2 142.67(3) 4_656 7_655 ? Sb5 Sb2 Gd2 61.30(2) 1_545 7_655 ? Fe1 Sb2 Gd1 132.55(3) 7_665 6_556 ? Fe1 Sb2 Gd1 72.80(3) 4_656 6_556 ? Sb5 Sb2 Gd1 100.580(14) 1_545 6_556 ? Gd2 Sb2 Gd1 82.832(13) 7_655 6_556 ? Fe1 Sb2 Gd1 72.80(3) 7_665 1_556 ? Fe1 Sb2 Gd1 132.55(3) 4_656 1_556 ? Sb5 Sb2 Gd1 100.580(14) 1_545 1_556 ? Gd2 Sb2 Gd1 82.832(13) 7_655 1_556 ? Gd1 Sb2 Gd1 144.56(3) 6_556 1_556 ? Fe1 Sb2 Gd2 64.56(3) 7_665 7_665 ? Fe1 Sb2 Gd2 64.56(3) 4_656 7_665 ? Sb5 Sb2 Gd2 156.35(3) 1_545 7_665 ? Gd2 Sb2 Gd2 142.35(3) 7_655 7_665 ? Gd1 Sb2 Gd2 85.942(14) 6_556 7_665 ? Gd1 Sb2 Gd2 85.942(14) 1_556 7_665 ? Sb3 Sb3 Sb3 176.665(18) 5_667 6_557 ? Sb3 Sb3 Sb3 92.924(18) 5_667 7_665 ? Sb3 Sb3 Sb3 90.0 6_557 7_665 ? Sb3 Sb3 Sb3 86.997(18) 5_667 7_655 ? Sb3 Sb3 Sb3 90.0 6_557 7_655 ? Sb3 Sb3 Sb3 177.03(3) 7_665 7_655 ? Sb3 Sb3 Gd2 115.47(2) 5_667 . ? Sb3 Sb3 Gd2 61.693(9) 6_557 . ? Sb3 Sb3 Gd2 115.31(2) 7_665 . ? Sb3 Sb3 Gd2 62.172(17) 7_655 . ? Sb3 Sb3 Gd2 120.94(2) 5_667 7_665 ? Sb3 Sb3 Gd2 61.991(9) 6_557 7_665 ? Sb3 Sb3 Gd2 61.143(16) 7_665 7_665 ? Sb3 Sb3 Gd2 121.35(2) 7_655 7_665 ? Gd2 Sb3 Gd2 123.547(15) . 7_665 ? Sb3 Sb3 Gd1 63.109(16) 5_667 5_666 ? Sb3 Sb3 Gd1 117.101(9) 6_557 5_666 ? Sb3 Sb3 Gd1 62.298(15) 7_665 5_666 ? Sb3 Sb3 Gd1 115.14(2) 7_655 5_666 ? Gd2 Sb3 Gd1 80.237(15) . 5_666 ? Gd2 Sb3 Gd1 123.424(17) 7_665 5_666 ? Sb3 Sb3 Gd1 62.699(16) 5_667 1_556 ? Sb3 Sb3 Gd1 116.993(8) 6_557 1_556 ? Sb3 Sb3 Gd1 120.63(2) 7_665 1_556 ? Sb3 Sb3 Gd1 61.903(14) 7_655 1_556 ? Gd2 Sb3 Gd1 124.058(18) . 1_556 ? Gd2 Sb3 Gd1 85.335(16) 7_665 1_556 ? Gd1 Sb3 Gd1 125.807(15) 5_666 1_556 ? Fe1 Sb4 Fe1 108.43(5) 1_554 3_556 ? Fe1 Sb4 Sb1 54.22(3) 1_554 1_455 ? Fe1 Sb4 Sb1 54.21(3) 3_556 1_455 ? Fe1 Sb4 Gd2 139.91(3) 1_554 3_556 ? Fe1 Sb4 Gd2 66.79(3) 3_556 3_556 ? Sb1 Sb4 Gd2 108.488(15) 1_455 3_556 ? Fe1 Sb4 Gd2 66.79(3) 1_554 1_554 ? Fe1 Sb4 Gd2 139.91(3) 3_556 1_554 ? Sb1 Sb4 Gd2 108.488(15) 1_455 1_554 ? Gd2 Sb4 Gd2 143.02(3) 3_556 1_554 ? Fe1 Sb4 Gd1 72.09(3) 1_554 5_655 ? Fe1 Sb4 Gd1 130.20(3) 3_556 5_655 ? Sb1 Sb4 Gd1 106.791(15) 1_455 5_655 ? Gd2 Sb4 Gd1 81.754(12) 3_556 5_655 ? Gd2 Sb4 Gd1 87.721(13) 1_554 5_655 ? Fe1 Sb4 Gd1 130.20(3) 1_554 5_665 ? Fe1 Sb4 Gd1 72.09(3) 3_556 5_665 ? Sb1 Sb4 Gd1 106.791(15) 1_455 5_665 ? Gd2 Sb4 Gd1 87.720(13) 3_556 5_665 ? Gd2 Sb4 Gd1 81.753(12) 1_554 5_665 ? Gd1 Sb4 Gd1 146.42(3) 5_655 5_665 ? Fe1 Sb5 Fe1 61.85(5) 1_665 6_667 ? Fe1 Sb5 Fe1 134.61(4) 1_665 4_656 ? Fe1 Sb5 Fe1 100.32(4) 6_667 4_656 ? Fe1 Sb5 Fe1 100.32(4) 1_665 7_665 ? Fe1 Sb5 Fe1 134.61(4) 6_667 7_665 ? Fe1 Sb5 Fe1 61.19(5) 4_656 7_665 ? Fe1 Sb5 Sb2 106.17(3) 1_665 1_565 ? Fe1 Sb5 Sb2 106.17(3) 6_667 1_565 ? Fe1 Sb5 Sb2 119.11(3) 4_656 1_565 ? Fe1 Sb5 Sb2 119.11(3) 7_665 1_565 ? Fe1 Sb5 Gd2 147.68(3) 1_665 7_665 ? Fe1 Sb5 Gd2 147.68(3) 6_667 7_665 ? Fe1 Sb5 Gd2 67.20(3) 4_656 7_665 ? Fe1 Sb5 Gd2 67.20(3) 7_665 7_665 ? Sb2 Sb5 Gd2 61.17(2) 1_565 7_665 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 30.04 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.821 _refine_diff_density_min -2.841 _refine_diff_density_rms 0.496 # Attachment '- NdFeSb3.cif' data_NdFeSb3 _database_code_depnum_ccdc_archive 'CCDC 768389' #TrackingRef '- NdFeSb3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Fe Nd Sb3' _chemical_formula_sum 'Fe Nd Sb3' _chemical_formula_weight 565.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Nd Nd -0.1943 3.0179 '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' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P b c m ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z-1/2' '-x, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 12.6790(2) _cell_length_b 6.1630(3) _cell_length_c 12.1370(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 948.39(5) _cell_formula_units_Z 8 _cell_measurement_temperature 298(5) _cell_measurement_reflns_used 2352 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 34.972 _exptl_crystal_description plate _exptl_crystal_colour silver _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 7.919 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1912 _exptl_absorpt_coefficient_mu 30.409 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2088 _exptl_absorpt_correction_T_max 0.5169 _exptl_absorpt_process_details 'HKL Scalepack (Otwinowski & Minor 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(5) _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 'Nonius KappaCCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3918 _diffrn_reflns_av_R_equivalents 0.0347 _diffrn_reflns_av_sigmaI/netI 0.0454 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 34.97 _reflns_number_total 2157 _reflns_number_gt 1970 _reflns_threshold_expression I>2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0581P)^2^+11.7017P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens ? _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0040(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2157 _refine_ls_number_parameters 53 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0419 _refine_ls_R_factor_gt 0.0379 _refine_ls_wR_factor_ref 0.1125 _refine_ls_wR_factor_gt 0.1033 _refine_ls_goodness_of_fit_ref 1.120 _refine_ls_restrained_S_all 1.120 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nd1 Nd 0.69957(4) 0.2500 0.0000 0.00772(12) Uani 1 2 d S . . Nd2 Nd 0.30703(4) 0.27582(8) 0.7500 0.00757(12) Uani 1 2 d S . . Fe1 Fe 0.10107(7) 0.03803(15) 0.86044(7) 0.00936(17) Uani 1 1 d . . . Sb1 Sb 0.97164(5) 0.2500 0.0000 0.00897(14) Uani 1 2 d S . . Sb2 Sb 0.78036(5) 0.26467(9) 0.7500 0.00830(13) Uani 1 2 d S . . Sb3 Sb 0.50275(3) 0.51211(7) 0.87662(3) 0.00848(12) Uani 1 1 d . . . Sb4 Sb 0.22219(5) 0.2500 0.0000 0.00809(13) Uani 1 2 d S . . Sb5 Sb 0.93923(4) 0.89557(9) 0.7500 0.00888(13) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd1 0.0062(2) 0.0082(2) 0.0087(2) -0.00035(12) 0.000 0.000 Nd2 0.0055(2) 0.0089(2) 0.0084(2) 0.000 0.000 0.00012(13) Fe1 0.0083(4) 0.0095(3) 0.0103(4) -0.0007(3) 0.0002(3) 0.0004(3) Sb1 0.0076(2) 0.0085(2) 0.0108(3) 0.00069(15) 0.000 0.000 Sb2 0.0076(3) 0.0085(2) 0.0088(3) 0.000 0.000 -0.00102(15) Sb3 0.0066(2) 0.0097(2) 0.0091(2) -0.00018(11) -0.00012(11) -0.00018(10) Sb4 0.0081(3) 0.0081(2) 0.0081(3) -0.00087(15) 0.000 0.000 Sb5 0.0057(2) 0.0089(2) 0.0120(2) 0.000 0.000 -0.00118(16) _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 Nd1 Sb2 3.2038(3) 3_556 ? Nd1 Sb2 3.2038(3) 1_554 ? Nd1 Sb4 3.2372(3) 5_655 ? Nd1 Sb4 3.2372(3) 5_665 ? Nd1 Sb3 3.3125(5) 5_666 ? Nd1 Sb3 3.3125(5) 7_654 ? Nd1 Sb3 3.3285(5) 1_554 ? Nd1 Sb3 3.3286(5) 3_556 ? Nd1 Sb1 3.4496(7) . ? Nd1 Fe1 3.5227(10) 5_656 ? Nd1 Fe1 3.5227(10) 7_664 ? Nd2 Sb5 3.2084(7) 7_655 ? Nd2 Sb2 3.2101(7) 7_665 ? Nd2 Sb4 3.2232(3) 6_556 ? Nd2 Sb4 3.2232(3) 1_556 ? Nd2 Sb3 3.2620(5) 6_557 ? Nd2 Sb3 3.2620(5) . ? Nd2 Fe1 3.2808(10) . ? Nd2 Fe1 3.2808(10) 6_557 ? Nd2 Sb3 3.2893(6) 7_655 ? Nd2 Sb3 3.2893(6) 4_646 ? Nd2 Sb2 3.3394(7) 7_655 ? Fe1 Sb5 2.6034(10) 1_445 ? Fe1 Sb1 2.6211(10) 5_656 ? Fe1 Sb2 2.6259(10) 7_655 ? Fe1 Sb5 2.6293(11) 7_655 ? Fe1 Sb4 2.6333(9) 1_556 ? Fe1 Fe1 2.6809(18) 6_557 ? Fe1 Sb1 2.6960(9) 1_456 ? Fe1 Nd1 3.5227(10) 5_656 ? Sb1 Fe1 2.6211(10) 5_656 ? Sb1 Fe1 2.6211(9) 7_664 ? Sb1 Fe1 2.6960(9) 1_654 ? Sb1 Fe1 2.6960(9) 3_656 ? Sb1 Sb1 3.1643(3) 5_755 ? Sb1 Sb1 3.1643(3) 5_765 ? Sb1 Sb4 3.1767(8) 1_655 ? Sb2 Fe1 2.6259(10) 7_665 ? Sb2 Fe1 2.6259(10) 4_656 ? Sb2 Sb5 3.0384(8) 1_545 ? Sb2 Nd1 3.2038(3) 6_556 ? Sb2 Nd1 3.2038(3) 1_556 ? Sb2 Nd2 3.2100(7) 7_655 ? Sb2 Nd2 3.3394(7) 7_665 ? Sb3 Sb3 2.9995(7) 5_667 ? Sb3 Sb3 3.0735(7) 6_557 ? Sb3 Sb3 3.08227(15) 7_665 ? Sb3 Sb3 3.08231(15) 7_655 ? Sb3 Nd2 3.2893(6) 7_665 ? Sb3 Nd1 3.3125(5) 5_666 ? Sb3 Nd1 3.3285(5) 1_556 ? Sb4 Fe1 2.6332(9) 1_554 ? Sb4 Fe1 2.6332(9) 3_556 ? Sb4 Sb1 3.1767(8) 1_455 ? Sb4 Nd2 3.2232(3) 3_556 ? Sb4 Nd2 3.2232(3) 1_554 ? Sb4 Nd1 3.2372(3) 5_655 ? Sb4 Nd1 3.2372(3) 5_665 ? Sb5 Fe1 2.6034(10) 1_665 ? Sb5 Fe1 2.6034(10) 6_667 ? Sb5 Fe1 2.6293(11) 4_656 ? Sb5 Fe1 2.6293(11) 7_665 ? Sb5 Sb2 3.0384(8) 1_565 ? Sb5 Nd2 3.2084(7) 7_665 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Sb2 Nd1 Sb2 142.71(3) 3_556 1_554 ? Sb2 Nd1 Sb4 82.828(11) 3_556 5_655 ? Sb2 Nd1 Sb4 85.922(12) 1_554 5_655 ? Sb2 Nd1 Sb4 85.922(12) 3_556 5_665 ? Sb2 Nd1 Sb4 82.828(11) 1_554 5_665 ? Sb4 Nd1 Sb4 144.31(3) 5_655 5_665 ? Sb2 Nd1 Sb3 80.326(12) 3_556 5_666 ? Sb2 Nd1 Sb3 131.550(15) 1_554 5_666 ? Sb4 Nd1 Sb3 131.194(14) 5_655 5_666 ? Sb4 Nd1 Sb3 79.397(12) 5_665 5_666 ? Sb2 Nd1 Sb3 131.550(15) 3_556 7_654 ? Sb2 Nd1 Sb3 80.326(12) 1_554 7_654 ? Sb4 Nd1 Sb3 79.397(12) 5_655 7_654 ? Sb4 Nd1 Sb3 131.195(14) 5_665 7_654 ? Sb3 Nd1 Sb3 78.494(17) 5_666 7_654 ? Sb2 Nd1 Sb3 132.805(14) 3_556 1_554 ? Sb2 Nd1 Sb3 78.459(12) 1_554 1_554 ? Sb4 Nd1 Sb3 133.765(13) 5_655 1_554 ? Sb4 Nd1 Sb3 76.572(12) 5_665 1_554 ? Sb3 Nd1 Sb3 53.700(13) 5_666 1_554 ? Sb3 Nd1 Sb3 55.307(8) 7_654 1_554 ? Sb2 Nd1 Sb3 78.459(12) 3_556 3_556 ? Sb2 Nd1 Sb3 132.804(14) 1_554 3_556 ? Sb4 Nd1 Sb3 76.571(12) 5_655 3_556 ? Sb4 Nd1 Sb3 133.765(13) 5_665 3_556 ? Sb3 Nd1 Sb3 55.307(8) 5_666 3_556 ? Sb3 Nd1 Sb3 53.700(13) 7_654 3_556 ? Sb3 Nd1 Sb3 82.869(17) 1_554 3_556 ? Sb2 Nd1 Sb1 71.353(13) 3_556 . ? Sb2 Nd1 Sb1 71.353(13) 1_554 . ? Sb4 Nd1 Sb1 72.156(13) 5_655 . ? Sb4 Nd1 Sb1 72.156(13) 5_665 . ? Sb3 Nd1 Sb1 140.753(9) 5_666 . ? Sb3 Nd1 Sb1 140.753(9) 7_654 . ? Sb3 Nd1 Sb1 138.565(9) 1_554 . ? Sb3 Nd1 Sb1 138.565(9) 3_556 . ? Sb2 Nd1 Fe1 45.650(18) 3_556 5_656 ? Sb2 Nd1 Fe1 103.90(2) 1_554 5_656 ? Sb4 Nd1 Fe1 45.609(17) 5_655 5_656 ? Sb4 Nd1 Fe1 105.06(2) 5_665 5_656 ? Sb3 Nd1 Fe1 124.149(15) 5_666 5_656 ? Sb3 Nd1 Fe1 123.368(16) 7_654 5_656 ? Sb3 Nd1 Fe1 177.230(19) 1_554 5_656 ? Sb3 Nd1 Fe1 94.420(17) 3_556 5_656 ? Sb1 Nd1 Fe1 44.147(16) . 5_656 ? Sb2 Nd1 Fe1 103.90(2) 3_556 7_664 ? Sb2 Nd1 Fe1 45.650(18) 1_554 7_664 ? Sb4 Nd1 Fe1 105.06(2) 5_655 7_664 ? Sb4 Nd1 Fe1 45.609(17) 5_665 7_664 ? Sb3 Nd1 Fe1 123.369(16) 5_666 7_664 ? Sb3 Nd1 Fe1 124.149(15) 7_654 7_664 ? Sb3 Nd1 Fe1 94.421(16) 1_554 7_664 ? Sb3 Nd1 Fe1 177.230(19) 3_556 7_664 ? Sb1 Nd1 Fe1 44.148(16) . 7_664 ? Fe1 Nd1 Fe1 88.30(3) 5_656 7_664 ? Sb5 Nd2 Sb2 56.509(16) 7_655 7_665 ? Sb5 Nd2 Sb4 71.734(13) 7_655 6_556 ? Sb2 Nd2 Sb4 86.052(10) 7_665 6_556 ? Sb5 Nd2 Sb4 71.734(13) 7_655 1_556 ? Sb2 Nd2 Sb4 86.052(11) 7_665 1_556 ? Sb4 Nd2 Sb4 140.57(3) 6_556 1_556 ? Sb5 Nd2 Sb3 129.618(16) 7_655 6_557 ? Sb2 Nd2 Sb3 81.002(15) 7_665 6_557 ? Sb4 Nd2 Sb3 80.354(12) 6_556 6_557 ? Sb4 Nd2 Sb3 136.007(15) 1_556 6_557 ? Sb5 Nd2 Sb3 129.617(16) 7_655 . ? Sb2 Nd2 Sb3 81.001(15) 7_665 . ? Sb4 Nd2 Sb3 136.007(15) 6_556 . ? Sb4 Nd2 Sb3 80.354(12) 1_556 . ? Sb3 Nd2 Sb3 56.213(15) 6_557 . ? Sb5 Nd2 Fe1 47.79(2) 7_655 . ? Sb2 Nd2 Fe1 98.31(2) 7_665 . ? Sb4 Nd2 Fe1 95.56(2) 6_556 . ? Sb4 Nd2 Fe1 47.755(18) 1_556 . ? Sb3 Nd2 Fe1 175.887(18) 6_557 . ? Sb3 Nd2 Fe1 127.768(17) . . ? Sb5 Nd2 Fe1 47.789(19) 7_655 6_557 ? Sb2 Nd2 Fe1 98.31(2) 7_665 6_557 ? Sb4 Nd2 Fe1 47.755(18) 6_556 6_557 ? Sb4 Nd2 Fe1 95.56(2) 1_556 6_557 ? Sb3 Nd2 Fe1 127.768(17) 6_557 6_557 ? Sb3 Nd2 Fe1 175.887(18) . 6_557 ? Fe1 Nd2 Fe1 48.23(3) . 6_557 ? Sb5 Nd2 Sb3 145.813(13) 7_655 7_655 ? Sb2 Nd2 Sb3 135.792(15) 7_665 7_655 ? Sb4 Nd2 Sb3 131.308(16) 6_556 7_655 ? Sb4 Nd2 Sb3 77.320(12) 1_556 7_655 ? Sb3 Nd2 Sb3 83.275(13) 6_557 7_655 ? Sb3 Nd2 Sb3 56.130(7) . 7_655 ? Fe1 Nd2 Sb3 99.905(19) . 7_655 ? Fe1 Nd2 Sb3 123.63(2) 6_557 7_655 ? Sb5 Nd2 Sb3 145.813(13) 7_655 4_646 ? Sb2 Nd2 Sb3 135.792(15) 7_665 4_646 ? Sb4 Nd2 Sb3 77.320(12) 6_556 4_646 ? Sb4 Nd2 Sb3 131.308(15) 1_556 4_646 ? Sb3 Nd2 Sb3 56.130(7) 6_557 4_646 ? Sb3 Nd2 Sb3 83.275(13) . 4_646 ? Fe1 Nd2 Sb3 123.63(2) . 4_646 ? Fe1 Nd2 Sb3 99.905(19) 6_557 4_646 ? Sb3 Nd2 Sb3 55.705(15) 7_655 4_646 ? Sb5 Nd2 Sb2 83.922(18) 7_655 7_655 ? Sb2 Nd2 Sb2 140.43(2) 7_665 7_655 ? Sb4 Nd2 Sb2 80.950(10) 6_556 7_655 ? Sb4 Nd2 Sb2 80.950(10) 1_556 7_655 ? Sb3 Nd2 Sb2 132.342(15) 6_557 7_655 ? Sb3 Nd2 Sb2 132.342(15) . 7_655 ? Fe1 Nd2 Sb2 46.727(19) . 7_655 ? Fe1 Nd2 Sb2 46.727(19) 6_557 7_655 ? Sb3 Nd2 Sb2 77.124(14) 7_655 7_655 ? Sb3 Nd2 Sb2 77.124(14) 4_646 7_655 ? Sb5 Fe1 Sb1 80.05(3) 1_445 5_656 ? Sb5 Fe1 Sb2 88.40(3) 1_445 7_655 ? Sb1 Fe1 Sb2 95.55(3) 5_656 7_655 ? Sb5 Fe1 Sb5 82.36(3) 1_445 7_655 ? Sb1 Fe1 Sb5 145.96(4) 5_656 7_655 ? Sb2 Fe1 Sb5 112.87(3) 7_655 7_655 ? Sb5 Fe1 Sb4 163.36(4) 1_445 1_556 ? Sb1 Fe1 Sb4 97.21(3) 5_656 1_556 ? Sb2 Fe1 Sb4 108.22(4) 7_655 1_556 ? Sb5 Fe1 Sb4 91.46(3) 7_655 1_556 ? Sb5 Fe1 Fe1 59.01(2) 1_445 6_557 ? Sb1 Fe1 Fe1 130.258(19) 5_656 6_557 ? Sb2 Fe1 Fe1 59.31(2) 7_655 6_557 ? Sb5 Fe1 Fe1 59.35(2) 7_655 6_557 ? Sb4 Fe1 Fe1 130.03(2) 1_556 6_557 ? Sb5 Fe1 Sb1 90.41(3) 1_445 1_456 ? Sb1 Fe1 Sb1 73.03(2) 5_656 1_456 ? Sb2 Fe1 Sb1 168.54(4) 7_655 1_456 ? Sb5 Fe1 Sb1 78.22(3) 7_655 1_456 ? Sb4 Fe1 Sb1 73.17(3) 1_556 1_456 ? Fe1 Fe1 Sb1 128.92(2) 6_557 1_456 ? Sb5 Fe1 Nd2 124.58(3) 1_445 . ? Sb1 Fe1 Nd2 147.83(4) 5_656 . ? Sb2 Fe1 Nd2 67.81(2) 7_655 . ? Sb5 Fe1 Nd2 64.66(2) 7_655 . ? Sb4 Fe1 Nd2 64.98(2) 1_556 . ? Fe1 Fe1 Nd2 65.885(16) 6_557 . ? Sb1 Fe1 Nd2 121.65(3) 1_456 . ? Sb5 Fe1 Nd1 130.03(3) 1_445 5_656 ? Sb1 Fe1 Nd1 66.45(2) 5_656 5_656 ? Sb2 Fe1 Nd1 60.746(19) 7_655 5_656 ? Sb5 Fe1 Nd1 143.79(3) 7_655 5_656 ? Sb4 Fe1 Nd1 61.460(19) 1_556 5_656 ? Fe1 Fe1 Nd1 118.739(14) 6_557 5_656 ? Sb1 Fe1 Nd1 112.26(3) 1_456 5_656 ? Nd2 Fe1 Nd1 81.40(2) . 5_656 ? Fe1 Sb1 Fe1 138.81(5) 5_656 7_664 ? Fe1 Sb1 Fe1 106.97(2) 5_656 1_654 ? Fe1 Sb1 Fe1 97.83(3) 7_664 1_654 ? Fe1 Sb1 Fe1 97.83(3) 5_656 3_656 ? Fe1 Sb1 Fe1 106.97(2) 7_664 3_656 ? Fe1 Sb1 Fe1 105.01(4) 1_654 3_656 ? Fe1 Sb1 Sb1 54.58(2) 5_656 5_755 ? Fe1 Sb1 Sb1 137.69(2) 7_664 5_755 ? Fe1 Sb1 Sb1 52.40(2) 1_654 5_755 ? Fe1 Sb1 Sb1 109.49(3) 3_656 5_755 ? Fe1 Sb1 Sb1 137.69(2) 5_656 5_765 ? Fe1 Sb1 Sb1 54.58(2) 7_664 5_765 ? Fe1 Sb1 Sb1 109.49(3) 1_654 5_765 ? Fe1 Sb1 Sb1 52.40(2) 3_656 5_765 ? Sb1 Sb1 Sb1 153.73(4) 5_755 5_765 ? Fe1 Sb1 Sb4 110.59(2) 5_656 1_655 ? Fe1 Sb1 Sb4 110.59(2) 7_664 1_655 ? Fe1 Sb1 Sb4 52.51(2) 1_654 1_655 ? Fe1 Sb1 Sb4 52.51(2) 3_656 1_655 ? Sb1 Sb1 Sb4 76.86(2) 5_755 1_655 ? Sb1 Sb1 Sb4 76.86(2) 5_765 1_655 ? Fe1 Sb1 Nd1 69.41(2) 5_656 . ? Fe1 Sb1 Nd1 69.41(2) 7_664 . ? Fe1 Sb1 Nd1 127.49(2) 1_654 . ? Fe1 Sb1 Nd1 127.49(2) 3_656 . ? Sb1 Sb1 Nd1 103.14(2) 5_755 . ? Sb1 Sb1 Nd1 103.14(2) 5_765 . ? Sb4 Sb1 Nd1 180.0 1_655 . ? Fe1 Sb2 Fe1 61.39(4) 7_665 4_656 ? Fe1 Sb2 Sb5 95.78(3) 7_665 1_545 ? Fe1 Sb2 Sb5 95.78(3) 4_656 1_545 ? Fe1 Sb2 Nd1 133.21(3) 7_665 6_556 ? Fe1 Sb2 Nd1 73.60(2) 4_656 6_556 ? Sb5 Sb2 Nd1 101.002(12) 1_545 6_556 ? Fe1 Sb2 Nd1 73.60(2) 7_665 1_556 ? Fe1 Sb2 Nd1 133.21(3) 4_656 1_556 ? Sb5 Sb2 Nd1 101.002(12) 1_545 1_556 ? Nd1 Sb2 Nd1 142.56(3) 6_556 1_556 ? Fe1 Sb2 Nd2 143.11(2) 7_665 7_655 ? Fe1 Sb2 Nd2 143.11(2) 4_656 7_655 ? Sb5 Sb2 Nd2 61.719(16) 1_545 7_655 ? Nd1 Sb2 Nd2 82.134(11) 6_556 7_655 ? Nd1 Sb2 Nd2 82.134(11) 1_556 7_655 ? Fe1 Sb2 Nd2 65.46(2) 7_665 7_665 ? Fe1 Sb2 Nd2 65.46(2) 4_656 7_665 ? Sb5 Sb2 Nd2 157.85(2) 1_545 7_665 ? Nd1 Sb2 Nd2 85.442(11) 6_556 7_665 ? Nd1 Sb2 Nd2 85.442(11) 1_556 7_665 ? Nd2 Sb2 Nd2 140.43(2) 7_655 7_665 ? Sb3 Sb3 Sb3 176.850(16) 5_667 6_557 ? Sb3 Sb3 Sb3 92.822(16) 5_667 7_665 ? Sb3 Sb3 Sb3 90.0 6_557 7_665 ? Sb3 Sb3 Sb3 87.117(16) 5_667 7_655 ? Sb3 Sb3 Sb3 90.0 6_557 7_655 ? Sb3 Sb3 Sb3 177.40(3) 7_665 7_655 ? Sb3 Sb3 Nd2 115.497(19) 5_667 . ? Sb3 Sb3 Nd2 61.893(7) 6_557 . ? Sb3 Sb3 Nd2 115.409(17) 7_665 . ? Sb3 Sb3 Nd2 62.383(14) 7_655 . ? Sb3 Sb3 Nd2 120.54(2) 5_667 7_665 ? Sb3 Sb3 Nd2 62.148(7) 6_557 7_665 ? Sb3 Sb3 Nd2 61.486(13) 7_665 7_665 ? Sb3 Sb3 Nd2 120.703(17) 7_655 7_665 ? Nd2 Sb3 Nd2 123.936(13) . 7_665 ? Sb3 Sb3 Nd1 63.424(13) 5_667 5_666 ? Sb3 Sb3 Nd1 116.877(7) 6_557 5_666 ? Sb3 Sb3 Nd1 62.611(12) 7_665 5_666 ? Sb3 Sb3 Nd1 115.147(17) 7_655 5_666 ? Nd2 Sb3 Nd1 79.713(13) . 5_666 ? Nd2 Sb3 Nd1 124.078(15) 7_665 5_666 ? Sb3 Sb3 Nd1 62.876(13) 5_667 1_556 ? Sb3 Sb3 Nd1 116.736(7) 6_557 1_556 ? Sb3 Sb3 Nd1 120.144(16) 7_665 1_556 ? Sb3 Sb3 Nd1 62.082(12) 7_655 1_556 ? Nd2 Sb3 Nd1 124.446(15) . 1_556 ? Nd2 Sb3 Nd1 84.278(13) 7_665 1_556 ? Nd1 Sb3 Nd1 126.300(13) 5_666 1_556 ? Fe1 Sb4 Fe1 108.65(4) 1_554 3_556 ? Fe1 Sb4 Sb1 54.32(2) 1_554 1_455 ? Fe1 Sb4 Sb1 54.32(2) 3_556 1_455 ? Fe1 Sb4 Nd2 140.87(2) 1_554 3_556 ? Fe1 Sb4 Nd2 67.27(2) 3_556 3_556 ? Sb1 Sb4 Nd2 109.495(13) 1_455 3_556 ? Fe1 Sb4 Nd2 67.27(2) 1_554 1_554 ? Fe1 Sb4 Nd2 140.87(2) 3_556 1_554 ? Sb1 Sb4 Nd2 109.495(13) 1_455 1_554 ? Nd2 Sb4 Nd2 141.01(3) 3_556 1_554 ? Fe1 Sb4 Nd1 72.93(2) 1_554 5_655 ? Fe1 Sb4 Nd1 130.61(2) 3_556 5_655 ? Sb1 Sb4 Nd1 107.845(13) 1_455 5_655 ? Nd2 Sb4 Nd1 81.415(10) 3_556 5_655 ? Nd2 Sb4 Nd1 86.832(11) 1_554 5_655 ? Fe1 Sb4 Nd1 130.61(2) 1_554 5_665 ? Fe1 Sb4 Nd1 72.93(2) 3_556 5_665 ? Sb1 Sb4 Nd1 107.845(13) 1_455 5_665 ? Nd2 Sb4 Nd1 86.832(11) 3_556 5_665 ? Nd2 Sb4 Nd1 81.415(10) 1_554 5_665 ? Nd1 Sb4 Nd1 144.31(3) 5_655 5_665 ? Fe1 Sb5 Fe1 61.98(4) 1_665 6_667 ? Fe1 Sb5 Fe1 134.29(3) 1_665 4_656 ? Fe1 Sb5 Fe1 99.98(3) 6_667 4_656 ? Fe1 Sb5 Fe1 99.98(3) 1_665 7_665 ? Fe1 Sb5 Fe1 134.29(3) 6_667 7_665 ? Fe1 Sb5 Fe1 61.30(4) 4_656 7_665 ? Fe1 Sb5 Sb2 105.67(3) 1_665 1_565 ? Fe1 Sb5 Sb2 105.67(3) 6_667 1_565 ? Fe1 Sb5 Sb2 119.91(3) 4_656 1_565 ? Fe1 Sb5 Sb2 119.91(3) 7_665 1_565 ? Fe1 Sb5 Nd2 147.63(2) 1_665 7_665 ? Fe1 Sb5 Nd2 147.63(2) 6_667 7_665 ? Fe1 Sb5 Nd2 67.55(2) 4_656 7_665 ? Fe1 Sb5 Nd2 67.55(2) 7_665 7_665 ? Sb2 Sb5 Nd2 61.773(17) 1_565 7_665 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 34.97 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 3.922 _refine_diff_density_min -3.653 _refine_diff_density_rms 0.710 # Attachment '- PrFeSb3.cif' data_PrFeSb3 _database_code_depnum_ccdc_archive 'CCDC 768390' #TrackingRef '- PrFeSb3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Pr Fe Sb3' _chemical_formula_sum 'Fe Pr Sb3' _chemical_formula_weight 562.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Pr Pr -0.2180 2.8214 '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' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P b c m ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z-1/2' '-x, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 12.7490(2) _cell_length_b 6.1730(4) _cell_length_c 12.1590(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 956.91(7) _cell_formula_units_Z 8 _cell_measurement_temperature 298(5) _cell_measurement_reflns_used 1402 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 7.802 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1904 _exptl_absorpt_coefficient_mu 29.470 _exptl_absorpt_correction_type sphere _exptl_absorpt_correction_T_min 0.1566 _exptl_absorpt_correction_T_max 0.5262 _exptl_absorpt_process_details 'HKL Scalepack (Otwinowski & Minor 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(5) _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 'Nonius KappaCCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2532 _diffrn_reflns_av_R_equivalents 0.0254 _diffrn_reflns_av_sigmaI/netI 0.0388 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 30.02 _reflns_number_total 1433 _reflns_number_gt 1383 _reflns_threshold_expression I>2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0458P)^2^+16.7696P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens ? _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0051(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1433 _refine_ls_number_parameters 53 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0365 _refine_ls_R_factor_gt 0.0348 _refine_ls_wR_factor_ref 0.1043 _refine_ls_wR_factor_gt 0.0952 _refine_ls_goodness_of_fit_ref 1.248 _refine_ls_restrained_S_all 1.248 _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 Pr1 Pr 0.69967(5) 0.2500 0.0000 0.00728(18) Uani 1 2 d S . . Pr2 Pr 0.30688(5) 0.27533(10) 0.7500 0.00710(18) Uani 1 2 d S . . Fe1 Fe 0.10037(9) 0.03820(19) 0.86031(9) 0.0092(3) Uani 1 1 d . . . Sb1 Sb 0.97171(6) 0.2500 0.0000 0.0085(2) Uani 1 2 d S . . Sb2 Sb 0.78166(6) 0.26514(11) 0.7500 0.0079(2) Uani 1 2 d S . . Sb3 Sb 0.50269(4) 0.51195(8) 0.87671(4) 0.00806(18) Uani 1 1 d . . . Sb4 Sb 0.22097(6) 0.2500 0.0000 0.0077(2) Uani 1 2 d S . . Sb5 Sb 0.93925(5) 0.89587(11) 0.7500 0.0085(2) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pr1 0.0064(3) 0.0075(3) 0.0079(3) -0.00036(17) 0.000 0.000 Pr2 0.0052(3) 0.0081(3) 0.0080(3) 0.000 0.000 0.00008(19) Fe1 0.0089(5) 0.0093(5) 0.0093(5) -0.0007(4) 0.0004(4) -0.0002(4) Sb1 0.0079(4) 0.0076(3) 0.0101(3) 0.0008(2) 0.000 0.000 Sb2 0.0081(4) 0.0075(4) 0.0080(3) 0.000 0.000 -0.0012(2) Sb3 0.0072(3) 0.0086(3) 0.0085(3) -0.00015(15) -0.00004(14) -0.00042(15) Sb4 0.0078(4) 0.0076(4) 0.0077(3) -0.0009(2) 0.000 0.000 Sb5 0.0065(3) 0.0082(3) 0.0108(3) 0.000 0.000 -0.0012(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pr1 Sb2 3.2158(3) 3_556 ? Pr1 Sb2 3.2158(3) 1_554 ? Pr1 Sb4 3.2481(4) 5_665 ? Pr1 Sb4 3.2481(4) 5_655 ? Pr1 Sb3 3.3259(7) 5_666 ? Pr1 Sb3 3.3259(7) 7_654 ? Pr1 Sb3 3.3420(7) 1_554 ? Pr1 Sb3 3.3420(7) 3_556 ? Pr1 Sb1 3.4683(9) . ? Pr1 Fe1 3.5425(12) 7_664 ? Pr1 Fe1 3.5425(12) 5_656 ? Pr2 Sb5 3.2249(9) 7_655 ? Pr2 Sb2 3.2274(9) 7_665 ? Pr2 Sb4 3.2348(4) 6_556 ? Pr2 Sb4 3.2348(4) 1_556 ? Pr2 Sb3 3.2771(7) . ? Pr2 Sb3 3.2771(7) 6_557 ? Pr2 Fe1 3.2975(12) . ? Pr2 Fe1 3.2975(12) 6_557 ? Pr2 Sb3 3.3033(7) 7_655 ? Pr2 Sb3 3.3033(7) 4_646 ? Pr2 Sb2 3.3456(9) 7_655 ? Fe1 Sb5 2.6058(12) 1_445 ? Fe1 Sb1 2.6257(12) 5_656 ? Fe1 Sb2 2.6272(13) 7_655 ? Fe1 Sb5 2.6323(13) 7_655 ? Fe1 Sb4 2.6379(12) 1_556 ? Fe1 Fe1 2.683(2) 6_557 ? Fe1 Sb1 2.6990(12) 1_456 ? Fe1 Pr1 3.5425(12) 5_656 ? Sb1 Fe1 2.6257(12) 7_664 ? Sb1 Fe1 2.6257(12) 5_656 ? Sb1 Fe1 2.6989(12) 3_656 ? Sb1 Fe1 2.6990(12) 1_654 ? Sb1 Sb1 3.1696(4) 5_765 ? Sb1 Sb1 3.1696(4) 5_755 ? Sb1 Sb4 3.1778(11) 1_655 ? Sb2 Fe1 2.6273(13) 7_665 ? Sb2 Fe1 2.6273(13) 4_656 ? Sb2 Sb5 3.0385(10) 1_545 ? Sb2 Pr1 3.2158(3) 6_556 ? Sb2 Pr1 3.2158(3) 1_556 ? Sb2 Pr2 3.2274(9) 7_655 ? Sb2 Pr2 3.3456(9) 7_665 ? Sb3 Sb3 3.0024(9) 5_667 ? Sb3 Sb3 3.0815(9) 6_557 ? Sb3 Sb3 3.0873(2) 7_655 ? Sb3 Sb3 3.0873(2) 7_665 ? Sb3 Pr2 3.3033(7) 7_665 ? Sb3 Pr1 3.3259(7) 5_666 ? Sb3 Pr1 3.3420(7) 1_556 ? Sb4 Fe1 2.6379(12) 3_556 ? Sb4 Fe1 2.6379(12) 1_554 ? Sb4 Sb1 3.1778(11) 1_455 ? Sb4 Pr2 3.2348(4) 3_556 ? Sb4 Pr2 3.2348(4) 1_554 ? Sb4 Pr1 3.2481(4) 5_665 ? Sb4 Pr1 3.2481(4) 5_655 ? Sb5 Fe1 2.6058(12) 1_665 ? Sb5 Fe1 2.6058(12) 6_667 ? Sb5 Fe1 2.6323(13) 4_656 ? Sb5 Fe1 2.6323(13) 7_665 ? Sb5 Sb2 3.0385(10) 1_565 ? Sb5 Pr2 3.2248(9) 7_665 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Sb2 Pr1 Sb2 142.06(3) 3_556 1_554 ? Sb2 Pr1 Sb4 85.777(15) 3_556 5_665 ? Sb2 Pr1 Sb4 82.596(14) 1_554 5_665 ? Sb2 Pr1 Sb4 82.596(14) 3_556 5_655 ? Sb2 Pr1 Sb4 85.777(16) 1_554 5_655 ? Sb4 Pr1 Sb4 143.70(3) 5_665 5_655 ? Sb2 Pr1 Sb3 80.732(15) 3_556 5_666 ? Sb2 Pr1 Sb3 131.707(19) 1_554 5_666 ? Sb4 Pr1 Sb3 79.734(15) 5_665 5_666 ? Sb4 Pr1 Sb3 131.410(18) 5_655 5_666 ? Sb2 Pr1 Sb3 131.707(19) 3_556 7_654 ? Sb2 Pr1 Sb3 80.732(15) 1_554 7_654 ? Sb4 Pr1 Sb3 131.411(18) 5_665 7_654 ? Sb4 Pr1 Sb3 79.734(15) 5_655 7_654 ? Sb3 Pr1 Sb3 78.27(2) 5_666 7_654 ? Sb2 Pr1 Sb3 133.025(18) 3_556 1_554 ? Sb2 Pr1 Sb3 78.827(16) 1_554 1_554 ? Sb4 Pr1 Sb3 76.955(16) 5_665 1_554 ? Sb4 Pr1 Sb3 133.937(17) 5_655 1_554 ? Sb3 Pr1 Sb3 53.523(16) 5_666 1_554 ? Sb3 Pr1 Sb3 55.162(10) 7_654 1_554 ? Sb2 Pr1 Sb3 78.827(16) 3_556 3_556 ? Sb2 Pr1 Sb3 133.024(18) 1_554 3_556 ? Sb4 Pr1 Sb3 133.937(17) 5_665 3_556 ? Sb4 Pr1 Sb3 76.955(16) 5_655 3_556 ? Sb3 Pr1 Sb3 55.162(10) 5_666 3_556 ? Sb3 Pr1 Sb3 53.523(16) 7_654 3_556 ? Sb3 Pr1 Sb3 82.57(2) 1_554 3_556 ? Sb2 Pr1 Sb1 71.031(17) 3_556 . ? Sb2 Pr1 Sb1 71.031(17) 1_554 . ? Sb4 Pr1 Sb1 71.851(17) 5_665 . ? Sb4 Pr1 Sb1 71.851(17) 5_655 . ? Sb3 Pr1 Sb1 140.866(11) 5_666 . ? Sb3 Pr1 Sb1 140.866(11) 7_654 . ? Sb3 Pr1 Sb1 138.717(11) 1_554 . ? Sb3 Pr1 Sb1 138.716(11) 3_556 . ? Sb2 Pr1 Fe1 103.52(3) 3_556 7_664 ? Sb2 Pr1 Fe1 45.43(2) 1_554 7_664 ? Sb4 Pr1 Fe1 45.46(2) 5_665 7_664 ? Sb4 Pr1 Fe1 104.66(3) 5_655 7_664 ? Sb3 Pr1 Fe1 123.53(2) 5_666 7_664 ? Sb3 Pr1 Fe1 124.334(19) 7_654 7_664 ? Sb3 Pr1 Fe1 94.75(2) 1_554 7_664 ? Sb3 Pr1 Fe1 177.25(2) 3_556 7_664 ? Sb1 Pr1 Fe1 43.973(19) . 7_664 ? Sb2 Pr1 Fe1 45.43(2) 3_556 5_656 ? Sb2 Pr1 Fe1 103.52(3) 1_554 5_656 ? Sb4 Pr1 Fe1 104.66(3) 5_665 5_656 ? Sb4 Pr1 Fe1 45.46(2) 5_655 5_656 ? Sb3 Pr1 Fe1 124.334(19) 5_666 5_656 ? Sb3 Pr1 Fe1 123.53(2) 7_654 5_656 ? Sb3 Pr1 Fe1 177.25(2) 1_554 5_656 ? Sb3 Pr1 Fe1 94.75(2) 3_556 5_656 ? Sb1 Pr1 Fe1 43.974(19) . 5_656 ? Fe1 Pr1 Fe1 87.95(4) 7_664 5_656 ? Sb5 Pr2 Sb2 56.19(2) 7_655 7_665 ? Sb5 Pr2 Sb4 71.441(16) 7_655 6_556 ? Sb2 Pr2 Sb4 85.807(14) 7_665 6_556 ? Sb5 Pr2 Sb4 71.441(16) 7_655 1_556 ? Sb2 Pr2 Sb4 85.807(14) 7_665 1_556 ? Sb4 Pr2 Sb4 140.00(3) 6_556 1_556 ? Sb5 Pr2 Sb3 129.67(2) 7_655 . ? Sb2 Pr2 Sb3 81.307(19) 7_665 . ? Sb4 Pr2 Sb3 136.16(2) 6_556 . ? Sb4 Pr2 Sb3 80.657(15) 1_556 . ? Sb5 Pr2 Sb3 129.67(2) 7_655 6_557 ? Sb2 Pr2 Sb3 81.307(19) 7_665 6_557 ? Sb4 Pr2 Sb3 80.657(15) 6_556 6_557 ? Sb4 Pr2 Sb3 136.16(2) 1_556 6_557 ? Sb3 Pr2 Sb3 56.089(18) . 6_557 ? Sb5 Pr2 Fe1 47.59(2) 7_655 . ? Sb2 Pr2 Fe1 97.85(3) 7_665 . ? Sb4 Pr2 Fe1 95.19(3) 6_556 . ? Sb4 Pr2 Fe1 47.62(2) 1_556 . ? Sb3 Pr2 Fe1 127.94(2) . . ? Sb3 Pr2 Fe1 175.80(2) 6_557 . ? Sb5 Pr2 Fe1 47.59(2) 7_655 6_557 ? Sb2 Pr2 Fe1 97.85(3) 7_665 6_557 ? Sb4 Pr2 Fe1 47.62(2) 6_556 6_557 ? Sb4 Pr2 Fe1 95.19(3) 1_556 6_557 ? Sb3 Pr2 Fe1 175.80(2) . 6_557 ? Sb3 Pr2 Fe1 127.94(2) 6_557 6_557 ? Fe1 Pr2 Fe1 48.00(4) . 6_557 ? Sb5 Pr2 Sb3 145.967(16) 7_655 7_655 ? Sb2 Pr2 Sb3 135.90(2) 7_665 7_655 ? Sb4 Pr2 Sb3 131.56(2) 6_556 7_655 ? Sb4 Pr2 Sb3 77.687(16) 1_556 7_655 ? Sb3 Pr2 Sb3 55.958(10) . 7_655 ? Sb3 Pr2 Sb3 83.038(17) 6_557 7_655 ? Fe1 Pr2 Sb3 100.29(2) . 7_655 ? Fe1 Pr2 Sb3 123.92(3) 6_557 7_655 ? Sb5 Pr2 Sb3 145.967(16) 7_655 4_646 ? Sb2 Pr2 Sb3 135.90(2) 7_665 4_646 ? Sb4 Pr2 Sb3 77.687(16) 6_556 4_646 ? Sb4 Pr2 Sb3 131.56(2) 1_556 4_646 ? Sb3 Pr2 Sb3 83.038(16) . 4_646 ? Sb3 Pr2 Sb3 55.958(10) 6_557 4_646 ? Fe1 Pr2 Sb3 123.92(3) . 4_646 ? Fe1 Pr2 Sb3 100.29(2) 6_557 4_646 ? Sb3 Pr2 Sb3 55.605(19) 7_655 4_646 ? Sb5 Pr2 Sb2 83.62(2) 7_655 7_655 ? Sb2 Pr2 Sb2 139.81(3) 7_665 7_655 ? Sb4 Pr2 Sb2 80.808(13) 6_556 7_655 ? Sb4 Pr2 Sb2 80.808(13) 1_556 7_655 ? Sb3 Pr2 Sb2 132.58(2) . 7_655 ? Sb3 Pr2 Sb2 132.58(2) 6_557 7_655 ? Fe1 Pr2 Sb2 46.59(2) . 7_655 ? Fe1 Pr2 Sb2 46.59(2) 6_557 7_655 ? Sb3 Pr2 Sb2 77.564(19) 7_655 7_655 ? Sb3 Pr2 Sb2 77.564(18) 4_646 7_655 ? Sb5 Fe1 Sb1 80.13(4) 1_445 5_656 ? Sb5 Fe1 Sb2 88.41(4) 1_445 7_655 ? Sb1 Fe1 Sb2 95.50(4) 5_656 7_655 ? Sb5 Fe1 Sb5 82.49(3) 1_445 7_655 ? Sb1 Fe1 Sb5 146.18(5) 5_656 7_655 ? Sb2 Fe1 Sb5 112.82(4) 7_655 7_655 ? Sb5 Fe1 Sb4 163.34(5) 1_445 1_556 ? Sb1 Fe1 Sb4 97.08(4) 5_656 1_556 ? Sb2 Fe1 Sb4 108.24(5) 7_655 1_556 ? Sb5 Fe1 Sb4 91.39(4) 7_655 1_556 ? Sb5 Fe1 Fe1 59.02(3) 1_445 6_557 ? Sb1 Fe1 Fe1 130.31(2) 5_656 6_557 ? Sb2 Fe1 Fe1 59.30(3) 7_655 6_557 ? Sb5 Fe1 Fe1 59.37(2) 7_655 6_557 ? Sb4 Fe1 Fe1 130.08(3) 1_556 6_557 ? Sb5 Fe1 Sb1 90.47(4) 1_445 1_456 ? Sb1 Fe1 Sb1 73.05(3) 5_656 1_456 ? Sb2 Fe1 Sb1 168.51(5) 7_655 1_456 ? Sb5 Fe1 Sb1 78.33(3) 7_655 1_456 ? Sb4 Fe1 Sb1 73.08(3) 1_556 1_456 ? Fe1 Fe1 Sb1 129.00(3) 6_557 1_456 ? Sb5 Fe1 Pr2 124.73(4) 1_445 . ? Sb1 Fe1 Pr2 147.49(5) 5_656 . ? Sb2 Fe1 Pr2 67.67(3) 7_655 . ? Sb5 Fe1 Pr2 64.76(3) 7_655 . ? Sb4 Fe1 Pr2 64.94(3) 1_556 . ? Fe1 Fe1 Pr2 65.999(19) 6_557 . ? Sb1 Fe1 Pr2 121.75(4) 1_456 . ? Sb5 Fe1 Pr1 130.15(4) 1_445 5_656 ? Sb1 Fe1 Pr1 66.51(3) 5_656 5_656 ? Sb2 Fe1 Pr1 60.70(2) 7_655 5_656 ? Sb5 Fe1 Pr1 143.48(4) 7_655 5_656 ? Sb4 Fe1 Pr1 61.36(2) 1_556 5_656 ? Fe1 Fe1 Pr1 118.650(18) 6_557 5_656 ? Sb1 Fe1 Pr1 112.27(4) 1_456 5_656 ? Pr2 Fe1 Pr1 80.99(3) . 5_656 ? Fe1 Sb1 Fe1 139.03(6) 7_664 5_656 ? Fe1 Sb1 Fe1 106.95(3) 7_664 3_656 ? Fe1 Sb1 Fe1 97.69(4) 5_656 3_656 ? Fe1 Sb1 Fe1 97.69(4) 7_664 1_654 ? Fe1 Sb1 Fe1 106.95(3) 5_656 1_654 ? Fe1 Sb1 Fe1 105.15(5) 3_656 1_654 ? Fe1 Sb1 Sb1 54.54(3) 7_664 5_765 ? Fe1 Sb1 Sb1 137.68(3) 5_656 5_765 ? Fe1 Sb1 Sb1 52.41(3) 3_656 5_765 ? Fe1 Sb1 Sb1 109.48(4) 1_654 5_765 ? Fe1 Sb1 Sb1 137.68(3) 7_664 5_755 ? Fe1 Sb1 Sb1 54.54(3) 5_656 5_755 ? Fe1 Sb1 Sb1 109.48(4) 3_656 5_755 ? Fe1 Sb1 Sb1 52.41(3) 1_654 5_755 ? Sb1 Sb1 Sb1 153.70(5) 5_765 5_755 ? Fe1 Sb1 Sb4 110.49(3) 7_664 1_655 ? Fe1 Sb1 Sb4 110.49(3) 5_656 1_655 ? Fe1 Sb1 Sb4 52.58(3) 3_656 1_655 ? Fe1 Sb1 Sb4 52.58(3) 1_654 1_655 ? Sb1 Sb1 Sb4 76.85(3) 5_765 1_655 ? Sb1 Sb1 Sb4 76.85(3) 5_755 1_655 ? Fe1 Sb1 Pr1 69.51(3) 7_664 . ? Fe1 Sb1 Pr1 69.51(3) 5_656 . ? Fe1 Sb1 Pr1 127.42(3) 3_656 . ? Fe1 Sb1 Pr1 127.42(3) 1_654 . ? Sb1 Sb1 Pr1 103.15(3) 5_765 . ? Sb1 Sb1 Pr1 103.15(3) 5_755 . ? Sb4 Sb1 Pr1 180.0 1_655 . ? Fe1 Sb2 Fe1 61.40(5) 7_665 4_656 ? Fe1 Sb2 Sb5 95.90(3) 7_665 1_545 ? Fe1 Sb2 Sb5 95.90(3) 4_656 1_545 ? Fe1 Sb2 Pr1 133.42(3) 7_665 6_556 ? Fe1 Sb2 Pr1 73.87(3) 4_656 6_556 ? Sb5 Sb2 Pr1 101.135(15) 1_545 6_556 ? Fe1 Sb2 Pr1 73.87(3) 7_665 1_556 ? Fe1 Sb2 Pr1 133.42(3) 4_656 1_556 ? Sb5 Sb2 Pr1 101.135(15) 1_545 1_556 ? Pr1 Sb2 Pr1 141.91(3) 6_556 1_556 ? Fe1 Sb2 Pr2 143.25(3) 7_665 7_655 ? Fe1 Sb2 Pr2 143.25(3) 4_656 7_655 ? Sb5 Sb2 Pr2 61.86(2) 1_545 7_655 ? Pr1 Sb2 Pr2 81.899(14) 6_556 7_655 ? Pr1 Sb2 Pr2 81.899(14) 1_556 7_655 ? Fe1 Sb2 Pr2 65.74(3) 7_665 7_665 ? Fe1 Sb2 Pr2 65.74(3) 4_656 7_665 ? Sb5 Sb2 Pr2 158.33(3) 1_545 7_665 ? Pr1 Sb2 Pr2 85.279(15) 6_556 7_665 ? Pr1 Sb2 Pr2 85.279(15) 1_556 7_665 ? Pr2 Sb2 Pr2 139.81(3) 7_655 7_665 ? Sb3 Sb3 Sb3 176.89(2) 5_667 6_557 ? Sb3 Sb3 Sb3 87.15(2) 5_667 7_655 ? Sb3 Sb3 Sb3 90.0 6_557 7_655 ? Sb3 Sb3 Sb3 92.79(2) 5_667 7_665 ? Sb3 Sb3 Sb3 90.0 6_557 7_665 ? Sb3 Sb3 Sb3 177.46(4) 7_655 7_665 ? Sb3 Sb3 Pr2 115.48(2) 5_667 . ? Sb3 Sb3 Pr2 61.956(9) 6_557 . ? Sb3 Sb3 Pr2 62.451(17) 7_655 . ? Sb3 Sb3 Pr2 115.39(2) 7_665 . ? Sb3 Sb3 Pr2 120.44(2) 5_667 7_665 ? Sb3 Sb3 Pr2 62.198(9) 6_557 7_665 ? Sb3 Sb3 Pr2 120.56(2) 7_655 7_665 ? Sb3 Sb3 Pr2 61.591(17) 7_665 7_665 ? Pr2 Sb3 Pr2 124.054(16) . 7_665 ? Sb3 Sb3 Pr1 63.511(17) 5_667 5_666 ? Sb3 Sb3 Pr1 116.789(9) 6_557 5_666 ? Sb3 Sb3 Pr1 115.12(2) 7_655 5_666 ? Sb3 Sb3 Pr1 62.683(15) 7_665 5_666 ? Pr2 Sb3 Pr1 79.511(17) . 5_666 ? Pr2 Sb3 Pr1 124.255(18) 7_665 5_666 ? Sb3 Sb3 Pr1 62.965(17) 5_667 1_556 ? Sb3 Sb3 Pr1 116.651(9) 6_557 1_556 ? Sb3 Sb3 Pr1 62.155(15) 7_655 1_556 ? Sb3 Sb3 Pr1 120.03(2) 7_665 1_556 ? Pr2 Sb3 Pr1 124.586(19) . 1_556 ? Pr2 Sb3 Pr1 83.976(17) 7_665 1_556 ? Pr1 Sb3 Pr1 126.476(16) 5_666 1_556 ? Fe1 Sb4 Fe1 108.69(5) 3_556 1_554 ? Fe1 Sb4 Sb1 54.35(3) 3_556 1_455 ? Fe1 Sb4 Sb1 54.35(3) 1_554 1_455 ? Fe1 Sb4 Pr2 67.44(3) 3_556 3_556 ? Fe1 Sb4 Pr2 141.12(3) 1_554 3_556 ? Sb1 Sb4 Pr2 109.790(17) 1_455 3_556 ? Fe1 Sb4 Pr2 141.12(3) 3_556 1_554 ? Fe1 Sb4 Pr2 67.44(3) 1_554 1_554 ? Sb1 Sb4 Pr2 109.790(17) 1_455 1_554 ? Pr2 Sb4 Pr2 140.42(3) 3_556 1_554 ? Fe1 Sb4 Pr1 73.18(3) 3_556 5_665 ? Fe1 Sb4 Pr1 130.73(3) 1_554 5_665 ? Sb1 Sb4 Pr1 108.150(17) 1_455 5_665 ? Pr2 Sb4 Pr1 86.587(15) 3_556 5_665 ? Pr2 Sb4 Pr1 81.292(13) 1_554 5_665 ? Fe1 Sb4 Pr1 130.73(3) 3_556 5_655 ? Fe1 Sb4 Pr1 73.18(3) 1_554 5_655 ? Sb1 Sb4 Pr1 108.149(17) 1_455 5_655 ? Pr2 Sb4 Pr1 81.292(13) 3_556 5_655 ? Pr2 Sb4 Pr1 86.587(15) 1_554 5_655 ? Pr1 Sb4 Pr1 143.70(3) 5_665 5_655 ? Fe1 Sb5 Fe1 61.96(5) 1_665 6_667 ? Fe1 Sb5 Fe1 134.13(4) 1_665 4_656 ? Fe1 Sb5 Fe1 99.89(4) 6_667 4_656 ? Fe1 Sb5 Fe1 99.89(4) 1_665 7_665 ? Fe1 Sb5 Fe1 134.13(4) 6_667 7_665 ? Fe1 Sb5 Fe1 61.27(5) 4_656 7_665 ? Fe1 Sb5 Sb2 105.56(3) 1_665 1_565 ? Fe1 Sb5 Sb2 105.56(3) 6_667 1_565 ? Fe1 Sb5 Sb2 120.16(3) 4_656 1_565 ? Fe1 Sb5 Sb2 120.16(3) 7_665 1_565 ? Fe1 Sb5 Pr2 147.65(3) 1_665 7_665 ? Fe1 Sb5 Pr2 147.65(3) 6_667 7_665 ? Fe1 Sb5 Pr2 67.65(3) 4_656 7_665 ? Fe1 Sb5 Pr2 67.65(3) 7_665 7_665 ? Sb2 Sb5 Pr2 61.95(2) 1_565 7_665 ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 30.02 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 2.219 _refine_diff_density_min -2.824 _refine_diff_density_rms 0.651 # Attachment '- SmFeSb3.cif' data_SmFeSb3 _database_code_depnum_ccdc_archive 'CCDC 768391' #TrackingRef '- SmFeSb3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Fe Sb3 Sm' _chemical_formula_sum 'Fe Sb3 Sm' _chemical_formula_weight 571.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Sm Sm -0.1638 3.4418 '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' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P b c m ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z-1/2' '-x, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 12.54900(10) _cell_length_b 6.1440(4) _cell_length_c 12.0910(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 932.23(7) _cell_formula_units_Z 8 _cell_measurement_temperature 298(5) _cell_measurement_reflns_used 1554 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description plate _exptl_crystal_colour silver _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 8.143 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1928 _exptl_absorpt_coefficient_mu 32.395 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2942 _exptl_absorpt_correction_T_max 0.4981 _exptl_absorpt_process_details 'HKL Scalepack (Otwinowski & Minor 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(5) _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 'Nonius KappaCCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2511 _diffrn_reflns_av_R_equivalents 0.0194 _diffrn_reflns_av_sigmaI/netI 0.0297 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 30.00 _reflns_number_total 1417 _reflns_number_gt 1333 _reflns_threshold_expression I>2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0359P)^2^+16.5472P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens ? _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00361(15) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1417 _refine_ls_number_parameters 53 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0327 _refine_ls_R_factor_gt 0.0301 _refine_ls_wR_factor_ref 0.0819 _refine_ls_wR_factor_gt 0.0760 _refine_ls_goodness_of_fit_ref 1.189 _refine_ls_restrained_S_all 1.189 _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 Sm1 Sm 0.69930(4) 0.2500 0.0000 0.00576(14) Uani 1 2 d S . . Sm2 Sm 0.30726(4) 0.27661(9) 0.7500 0.00569(14) Uani 1 2 d S . . Fe1 Fe 0.10261(8) 0.03777(17) 0.86050(9) 0.0085(2) Uani 1 1 d . . . Sb1 Sb 0.97152(5) 0.2500 0.0000 0.00695(17) Uani 1 2 d S . . Sb2 Sb 0.77789(5) 0.26395(10) 0.7500 0.00601(16) Uani 1 2 d S . . Sb3 Sb 0.50292(3) 0.51195(7) 0.87647(3) 0.00609(15) Uani 1 1 d . . . Sb4 Sb 0.22480(5) 0.2500 0.0000 0.00588(16) Uani 1 2 d S . . Sb5 Sb 0.93895(5) 0.89540(10) 0.7500 0.00688(17) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sm1 0.0060(2) 0.0042(2) 0.0071(3) -0.00048(15) 0.000 0.000 Sm2 0.0047(2) 0.0051(2) 0.0072(3) 0.000 0.000 0.00019(15) Fe1 0.0095(5) 0.0063(4) 0.0098(5) -0.0010(4) 0.0000(4) -0.0004(4) Sb1 0.0067(3) 0.0044(3) 0.0098(3) 0.0010(2) 0.000 0.000 Sb2 0.0072(3) 0.0040(3) 0.0069(3) 0.000 0.000 -0.0010(2) Sb3 0.0058(3) 0.0050(2) 0.0074(3) -0.00018(14) -0.00014(15) -0.00012(13) Sb4 0.0072(3) 0.0038(3) 0.0067(3) -0.0009(2) 0.000 0.000 Sb5 0.0054(3) 0.0049(3) 0.0104(3) 0.000 0.000 -0.0009(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sm1 Sb2 3.1807(3) 3_556 ? Sm1 Sb2 3.1807(3) 1_554 ? Sm1 Sb4 3.2163(3) 5_655 ? Sm1 Sb4 3.2163(3) 5_665 ? Sm1 Sb3 3.2878(6) 5_666 ? Sm1 Sb3 3.2878(6) 7_654 ? Sm1 Sb3 3.3007(6) 1_554 ? Sm1 Sb3 3.3007(6) 3_556 ? Sm1 Sb1 3.4161(8) . ? Sm1 Fe1 3.4857(11) 5_656 ? Sm1 Fe1 3.4858(11) 7_664 ? Sm2 Sb5 3.1747(8) 7_655 ? Sm2 Sb2 3.1792(8) 7_665 ? Sm2 Sb4 3.1992(3) 6_556 ? Sm2 Sb4 3.1992(3) 1_556 ? Sm2 Sb3 3.2338(6) 6_557 ? Sm2 Sb3 3.2338(6) . ? Sm2 Fe1 3.2456(11) 6_557 ? Sm2 Fe1 3.2456(11) . ? Sm2 Sb3 3.2644(6) 7_655 ? Sm2 Sb3 3.2644(6) 4_646 ? Sm2 Sb2 3.3261(8) 7_655 ? Fe1 Sb5 2.6016(12) 1_445 ? Fe1 Sb1 2.6146(11) 5_656 ? Fe1 Sb2 2.6199(12) 7_655 ? Fe1 Sb5 2.6239(12) 7_655 ? Fe1 Sb4 2.6261(11) 1_556 ? Fe1 Fe1 2.672(2) 6_557 ? Fe1 Sb1 2.6928(11) 1_456 ? Fe1 Sm1 3.4857(11) 5_656 ? Sb1 Fe1 2.6146(11) 5_656 ? Sb1 Fe1 2.6146(11) 7_664 ? Sb1 Fe1 2.6928(11) 1_654 ? Sb1 Fe1 2.6929(11) 3_656 ? Sb1 Sb1 3.1540(4) 5_755 ? Sb1 Sb1 3.1540(4) 5_765 ? Sb1 Sb4 3.1783(9) 1_655 ? Sb2 Fe1 2.6199(12) 7_665 ? Sb2 Fe1 2.6199(12) 4_656 ? Sb2 Sb5 3.0352(9) 1_545 ? Sb2 Sm2 3.1792(8) 7_655 ? Sb2 Sm1 3.1807(3) 6_556 ? Sb2 Sm1 3.1807(3) 1_556 ? Sb2 Sm2 3.3261(8) 7_665 ? Sb3 Sb3 2.9917(8) 5_667 ? Sb3 Sb3 3.0583(8) 6_557 ? Sb3 Sb3 3.0729(2) 7_665 ? Sb3 Sb3 3.0729(2) 7_655 ? Sb3 Sm2 3.2644(6) 7_665 ? Sb3 Sm1 3.2878(6) 5_666 ? Sb3 Sm1 3.3007(6) 1_556 ? Sb4 Fe1 2.6261(11) 1_554 ? Sb4 Fe1 2.6261(11) 3_556 ? Sb4 Sb1 3.1784(9) 1_455 ? Sb4 Sm2 3.1992(3) 3_556 ? Sb4 Sm2 3.1992(3) 1_554 ? Sb4 Sm1 3.2163(3) 5_655 ? Sb4 Sm1 3.2163(3) 5_665 ? Sb5 Fe1 2.6015(12) 1_665 ? Sb5 Fe1 2.6015(12) 6_667 ? Sb5 Fe1 2.6239(12) 4_656 ? Sb5 Fe1 2.6239(12) 7_665 ? Sb5 Sb2 3.0352(9) 1_565 ? Sb5 Sm2 3.1748(8) 7_665 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Sb2 Sm1 Sb2 143.87(3) 3_556 1_554 ? Sb2 Sm1 Sb4 83.248(13) 3_556 5_655 ? Sb2 Sm1 Sb4 86.211(14) 1_554 5_655 ? Sb2 Sm1 Sb4 86.211(14) 3_556 5_665 ? Sb2 Sm1 Sb4 83.248(13) 1_554 5_665 ? Sb4 Sm1 Sb4 145.55(3) 5_655 5_665 ? Sb2 Sm1 Sb3 79.607(14) 3_556 5_666 ? Sb2 Sm1 Sb3 131.227(17) 1_554 5_666 ? Sb4 Sm1 Sb3 130.803(16) 5_655 5_666 ? Sb4 Sm1 Sb3 78.678(14) 5_665 5_666 ? Sb2 Sm1 Sb3 131.227(17) 3_556 7_654 ? Sb2 Sm1 Sb3 79.607(14) 1_554 7_654 ? Sb4 Sm1 Sb3 78.678(13) 5_655 7_654 ? Sb4 Sm1 Sb3 130.804(16) 5_665 7_654 ? Sb3 Sm1 Sb3 78.96(2) 5_666 7_654 ? Sb2 Sm1 Sb3 132.429(16) 3_556 1_554 ? Sb2 Sm1 Sb3 77.780(14) 1_554 1_554 ? Sb4 Sm1 Sb3 133.380(15) 5_655 1_554 ? Sb4 Sm1 Sb3 75.841(14) 5_665 1_554 ? Sb3 Sm1 Sb3 54.010(15) 5_666 1_554 ? Sb3 Sm1 Sb3 55.601(8) 7_654 1_554 ? Sb2 Sm1 Sb3 77.781(14) 3_556 3_556 ? Sb2 Sm1 Sb3 132.429(16) 1_554 3_556 ? Sb4 Sm1 Sb3 75.840(14) 5_655 3_556 ? Sb4 Sm1 Sb3 133.381(15) 5_665 3_556 ? Sb3 Sm1 Sb3 55.601(8) 5_666 3_556 ? Sb3 Sm1 Sb3 54.010(15) 7_654 3_556 ? Sb3 Sm1 Sb3 83.398(19) 1_554 3_556 ? Sb2 Sm1 Sb1 71.937(15) 3_556 . ? Sb2 Sm1 Sb1 71.937(15) 1_554 . ? Sb4 Sm1 Sb1 72.774(15) 5_655 . ? Sb4 Sm1 Sb1 72.774(15) 5_665 . ? Sb3 Sm1 Sb1 140.520(10) 5_666 . ? Sb3 Sm1 Sb1 140.520(10) 7_654 . ? Sb3 Sm1 Sb1 138.301(9) 1_554 . ? Sb3 Sm1 Sb1 138.301(10) 3_556 . ? Sb2 Sm1 Fe1 46.00(2) 3_556 5_656 ? Sb2 Sm1 Fe1 104.62(2) 1_554 5_656 ? Sb4 Sm1 Fe1 45.921(19) 5_655 5_656 ? Sb4 Sm1 Fe1 105.86(2) 5_665 5_656 ? Sb3 Sm1 Fe1 123.797(19) 5_666 5_656 ? Sb3 Sm1 Fe1 122.999(19) 7_654 5_656 ? Sb3 Sm1 Fe1 177.14(2) 1_554 5_656 ? Sb3 Sm1 Fe1 93.795(19) 3_556 5_656 ? Sb1 Sm1 Fe1 44.508(18) . 5_656 ? Sb2 Sm1 Fe1 104.62(2) 3_556 7_664 ? Sb2 Sm1 Fe1 46.00(2) 1_554 7_664 ? Sb4 Sm1 Fe1 105.86(2) 5_655 7_664 ? Sb4 Sm1 Fe1 45.921(19) 5_665 7_664 ? Sb3 Sm1 Fe1 122.999(19) 5_666 7_664 ? Sb3 Sm1 Fe1 123.797(19) 7_654 7_664 ? Sb3 Sm1 Fe1 93.795(19) 1_554 7_664 ? Sb3 Sm1 Fe1 177.14(2) 3_556 7_664 ? Sb1 Sm1 Fe1 44.509(18) . 7_664 ? Fe1 Sm1 Fe1 89.02(4) 5_656 7_664 ? Sb5 Sm2 Sb2 57.069(19) 7_655 7_665 ? Sb5 Sm2 Sb4 72.358(15) 7_655 6_556 ? Sb2 Sm2 Sb4 86.526(12) 7_665 6_556 ? Sb5 Sm2 Sb4 72.358(15) 7_655 1_556 ? Sb2 Sm2 Sb4 86.526(12) 7_665 1_556 ? Sb4 Sm2 Sb4 141.77(3) 6_556 1_556 ? Sb5 Sm2 Sb3 129.504(18) 7_655 6_557 ? Sb2 Sm2 Sb3 80.449(17) 7_665 6_557 ? Sb4 Sm2 Sb3 79.727(13) 6_556 6_557 ? Sb4 Sm2 Sb3 135.664(18) 1_556 6_557 ? Sb5 Sm2 Sb3 129.504(18) 7_655 . ? Sb2 Sm2 Sb3 80.449(17) 7_665 . ? Sb4 Sm2 Sb3 135.663(18) 6_556 . ? Sb4 Sm2 Sb3 79.727(14) 1_556 . ? Sb3 Sm2 Sb3 56.442(17) 6_557 . ? Sb5 Sm2 Fe1 48.23(2) 7_655 6_557 ? Sb2 Sm2 Fe1 99.20(3) 7_665 6_557 ? Sb4 Sm2 Fe1 48.09(2) 6_556 6_557 ? Sb4 Sm2 Fe1 96.31(2) 1_556 6_557 ? Sb3 Sm2 Fe1 127.47(2) 6_557 6_557 ? Sb3 Sm2 Fe1 176.03(2) . 6_557 ? Sb5 Sm2 Fe1 48.23(2) 7_655 . ? Sb2 Sm2 Fe1 99.20(3) 7_665 . ? Sb4 Sm2 Fe1 96.31(2) 6_556 . ? Sb4 Sm2 Fe1 48.09(2) 1_556 . ? Sb3 Sm2 Fe1 176.03(2) 6_557 . ? Sb3 Sm2 Fe1 127.47(2) . . ? Fe1 Sm2 Fe1 48.62(4) 6_557 . ? Sb5 Sm2 Sb3 145.554(15) 7_655 7_655 ? Sb2 Sm2 Sb3 135.594(17) 7_665 7_655 ? Sb4 Sm2 Sb3 130.783(18) 6_556 7_655 ? Sb4 Sm2 Sb3 76.584(14) 1_556 7_655 ? Sb3 Sm2 Sb3 83.697(14) 6_557 7_655 ? Sb3 Sm2 Sb3 56.440(8) . 7_655 ? Fe1 Sm2 Sb3 123.02(3) 6_557 7_655 ? Fe1 Sm2 Sb3 99.17(2) . 7_655 ? Sb5 Sm2 Sb3 145.554(15) 7_655 4_646 ? Sb2 Sm2 Sb3 135.594(17) 7_665 4_646 ? Sb4 Sm2 Sb3 76.584(14) 6_556 4_646 ? Sb4 Sm2 Sb3 130.783(18) 1_556 4_646 ? Sb3 Sm2 Sb3 56.440(8) 6_557 4_646 ? Sb3 Sm2 Sb3 83.697(14) . 4_646 ? Fe1 Sm2 Sb3 99.17(2) 6_557 4_646 ? Fe1 Sm2 Sb3 123.02(3) . 4_646 ? Sb3 Sm2 Sb3 55.866(17) 7_655 4_646 ? Sb5 Sm2 Sb2 84.55(2) 7_655 7_655 ? Sb2 Sm2 Sb2 141.62(3) 7_665 7_655 ? Sb4 Sm2 Sb2 81.239(11) 6_556 7_655 ? Sb4 Sm2 Sb2 81.239(11) 1_556 7_655 ? Sb3 Sm2 Sb2 131.863(18) 6_557 7_655 ? Sb3 Sm2 Sb2 131.863(18) . 7_655 ? Fe1 Sm2 Sb2 46.97(2) 6_557 7_655 ? Fe1 Sm2 Sb2 46.97(2) . 7_655 ? Sb3 Sm2 Sb2 76.274(17) 7_655 7_655 ? Sb3 Sm2 Sb2 76.274(17) 4_646 7_655 ? Sb5 Fe1 Sb1 79.81(3) 1_445 5_656 ? Sb5 Fe1 Sb2 88.51(4) 1_445 7_655 ? Sb1 Fe1 Sb2 95.65(4) 5_656 7_655 ? Sb5 Fe1 Sb5 82.14(3) 1_445 7_655 ? Sb1 Fe1 Sb5 145.49(5) 5_656 7_655 ? Sb2 Fe1 Sb5 113.07(4) 7_655 7_655 ? Sb5 Fe1 Sb4 163.28(5) 1_445 1_556 ? Sb1 Fe1 Sb4 97.42(4) 5_656 1_556 ? Sb2 Fe1 Sb4 108.19(4) 7_655 1_556 ? Sb5 Fe1 Sb4 91.56(3) 7_655 1_556 ? Sb5 Fe1 Fe1 59.10(2) 1_445 6_557 ? Sb1 Fe1 Fe1 130.17(2) 5_656 6_557 ? Sb2 Fe1 Fe1 59.34(2) 7_655 6_557 ? Sb5 Fe1 Fe1 59.39(2) 7_655 6_557 ? Sb4 Fe1 Fe1 129.96(2) 1_556 6_557 ? Sb5 Fe1 Sb1 90.13(4) 1_445 1_456 ? Sb1 Fe1 Sb1 72.90(3) 5_656 1_456 ? Sb2 Fe1 Sb1 168.53(5) 7_655 1_456 ? Sb5 Fe1 Sb1 78.00(3) 7_655 1_456 ? Sb4 Fe1 Sb1 73.38(3) 1_556 1_456 ? Fe1 Fe1 Sb1 128.78(2) 6_557 1_456 ? Sb5 Fe1 Sm2 124.42(4) 1_445 . ? Sb1 Fe1 Sm2 148.52(4) 5_656 . ? Sb2 Fe1 Sm2 68.13(3) 7_655 . ? Sb5 Fe1 Sm2 64.47(3) 7_655 . ? Sb4 Fe1 Sm2 65.03(2) 1_556 . ? Fe1 Fe1 Sm2 65.692(19) 6_557 . ? Sb1 Fe1 Sm2 121.49(4) 1_456 . ? Sb5 Fe1 Sm1 129.86(4) 1_445 5_656 ? Sb1 Fe1 Sm1 66.33(3) 5_656 5_656 ? Sb2 Fe1 Sm1 60.85(2) 7_655 5_656 ? Sb5 Fe1 Sm1 144.38(4) 7_655 5_656 ? Sb4 Fe1 Sm1 61.62(2) 1_556 5_656 ? Fe1 Fe1 Sm1 118.940(17) 6_557 5_656 ? Sb1 Fe1 Sm1 112.22(3) 1_456 5_656 ? Sm2 Fe1 Sm1 82.20(3) . 5_656 ? Fe1 Sb1 Fe1 138.32(5) 5_656 7_664 ? Fe1 Sb1 Fe1 107.10(3) 5_656 1_654 ? Fe1 Sb1 Fe1 98.09(4) 7_664 1_654 ? Fe1 Sb1 Fe1 98.09(4) 5_656 3_656 ? Fe1 Sb1 Fe1 107.10(3) 7_664 3_656 ? Fe1 Sb1 Fe1 104.69(5) 1_654 3_656 ? Fe1 Sb1 Sb1 54.69(2) 5_656 5_755 ? Fe1 Sb1 Sb1 137.67(2) 7_664 5_755 ? Fe1 Sb1 Sb1 52.41(3) 1_654 5_755 ? Fe1 Sb1 Sb1 109.46(3) 3_656 5_755 ? Fe1 Sb1 Sb1 137.67(2) 5_656 5_765 ? Fe1 Sb1 Sb1 54.69(2) 7_664 5_765 ? Fe1 Sb1 Sb1 109.46(3) 1_654 5_765 ? Fe1 Sb1 Sb1 52.41(3) 3_656 5_765 ? Sb1 Sb1 Sb1 153.81(5) 5_755 5_765 ? Fe1 Sb1 Sb4 110.84(3) 5_656 1_655 ? Fe1 Sb1 Sb4 110.84(3) 7_664 1_655 ? Fe1 Sb1 Sb4 52.35(2) 1_654 1_655 ? Fe1 Sb1 Sb4 52.35(2) 3_656 1_655 ? Sb1 Sb1 Sb4 76.90(2) 5_755 1_655 ? Sb1 Sb1 Sb4 76.90(2) 5_765 1_655 ? Fe1 Sb1 Sm1 69.16(3) 5_656 . ? Fe1 Sb1 Sm1 69.16(3) 7_664 . ? Fe1 Sb1 Sm1 127.65(2) 1_654 . ? Fe1 Sb1 Sm1 127.65(2) 3_656 . ? Sb1 Sb1 Sm1 103.10(2) 5_755 . ? Sb1 Sb1 Sm1 103.10(2) 5_765 . ? Sb4 Sb1 Sm1 180.0 1_655 . ? Fe1 Sb2 Fe1 61.32(5) 7_665 4_656 ? Fe1 Sb2 Sb5 95.62(3) 7_665 1_545 ? Fe1 Sb2 Sb5 95.62(3) 4_656 1_545 ? Fe1 Sb2 Sm2 142.86(3) 7_665 7_655 ? Fe1 Sb2 Sm2 142.86(3) 4_656 7_655 ? Sb5 Sb2 Sm2 61.392(19) 1_545 7_655 ? Fe1 Sb2 Sm1 132.80(3) 7_665 6_556 ? Fe1 Sb2 Sm1 73.15(2) 4_656 6_556 ? Sb5 Sb2 Sm1 100.740(14) 1_545 6_556 ? Sm2 Sb2 Sm1 82.553(13) 7_655 6_556 ? Fe1 Sb2 Sm1 73.15(2) 7_665 1_556 ? Fe1 Sb2 Sm1 132.80(3) 4_656 1_556 ? Sb5 Sb2 Sm1 100.740(14) 1_545 1_556 ? Sm2 Sb2 Sm1 82.553(13) 7_655 1_556 ? Sm1 Sb2 Sm1 143.73(3) 6_556 1_556 ? Fe1 Sb2 Sm2 64.90(3) 7_665 7_665 ? Fe1 Sb2 Sm2 64.90(3) 4_656 7_665 ? Sb5 Sb2 Sm2 156.99(3) 1_545 7_665 ? Sm2 Sb2 Sm2 141.62(3) 7_655 7_665 ? Sm1 Sb2 Sm2 85.751(13) 6_556 7_665 ? Sm1 Sb2 Sm2 85.751(13) 1_556 7_665 ? Sb3 Sb3 Sb3 176.855(17) 5_667 6_557 ? Sb3 Sb3 Sb3 92.779(17) 5_667 7_665 ? Sb3 Sb3 Sb3 90.0 6_557 7_665 ? Sb3 Sb3 Sb3 87.153(17) 5_667 7_655 ? Sb3 Sb3 Sb3 90.0 6_557 7_655 ? Sb3 Sb3 Sb3 177.27(3) 7_665 7_655 ? Sb3 Sb3 Sm2 115.57(2) 5_667 . ? Sb3 Sb3 Sm2 61.779(9) 6_557 . ? Sb3 Sb3 Sm2 115.40(2) 7_665 . ? Sb3 Sb3 Sm2 62.283(16) 7_655 . ? Sb3 Sb3 Sm2 120.67(2) 5_667 7_665 ? Sb3 Sb3 Sm2 62.068(9) 6_557 7_665 ? Sb3 Sb3 Sm2 61.277(15) 7_665 7_665 ? Sb3 Sb3 Sm2 121.02(2) 7_655 7_665 ? Sm2 Sb3 Sm2 123.727(15) . 7_665 ? Sb3 Sb3 Sm1 63.214(15) 5_667 5_666 ? Sb3 Sb3 Sm1 117.018(8) 6_557 5_666 ? Sb3 Sb3 Sm1 62.411(14) 7_665 5_666 ? Sb3 Sb3 Sm1 115.234(19) 7_655 5_666 ? Sm2 Sb3 Sm1 80.079(15) . 5_666 ? Sm2 Sb3 Sm1 123.670(16) 7_665 5_666 ? Sb3 Sb3 Sm1 62.775(15) 5_667 1_556 ? Sb3 Sb3 Sm1 116.905(8) 6_557 1_556 ? Sb3 Sb3 Sm1 120.349(19) 7_665 1_556 ? Sb3 Sb3 Sm1 61.988(13) 7_655 1_556 ? Sm2 Sb3 Sm1 124.253(17) . 1_556 ? Sm2 Sb3 Sm1 84.838(15) 7_665 1_556 ? Sm1 Sb3 Sm1 125.989(15) 5_666 1_556 ? Fe1 Sb4 Fe1 108.55(5) 1_554 3_556 ? Fe1 Sb4 Sb1 54.28(3) 1_554 1_455 ? Fe1 Sb4 Sb1 54.28(3) 3_556 1_455 ? Fe1 Sb4 Sm2 140.39(3) 1_554 3_556 ? Fe1 Sb4 Sm2 66.88(2) 3_556 3_556 ? Sb1 Sb4 Sm2 108.873(15) 1_455 3_556 ? Fe1 Sb4 Sm2 66.88(2) 1_554 1_554 ? Fe1 Sb4 Sm2 140.39(3) 3_556 1_554 ? Sb1 Sb4 Sm2 108.873(15) 1_455 1_554 ? Sm2 Sb4 Sm2 142.25(3) 3_556 1_554 ? Fe1 Sb4 Sm1 72.46(2) 1_554 5_655 ? Fe1 Sb4 Sm1 130.33(3) 3_556 5_655 ? Sb1 Sb4 Sm1 107.227(15) 1_455 5_655 ? Sm2 Sb4 Sm1 81.685(12) 3_556 5_655 ? Sm2 Sb4 Sm1 87.307(13) 1_554 5_655 ? Fe1 Sb4 Sm1 130.33(3) 1_554 5_665 ? Fe1 Sb4 Sm1 72.46(2) 3_556 5_665 ? Sb1 Sb4 Sm1 107.227(15) 1_455 5_665 ? Sm2 Sb4 Sm1 87.307(13) 3_556 5_665 ? Sm2 Sb4 Sm1 81.685(12) 1_554 5_665 ? Sm1 Sb4 Sm1 145.55(3) 5_655 5_665 ? Fe1 Sb5 Fe1 61.80(5) 1_665 6_667 ? Fe1 Sb5 Fe1 134.42(4) 1_665 4_656 ? Fe1 Sb5 Fe1 100.19(4) 6_667 4_656 ? Fe1 Sb5 Fe1 100.19(4) 1_665 7_665 ? Fe1 Sb5 Fe1 134.42(4) 6_667 7_665 ? Fe1 Sb5 Fe1 61.22(5) 4_656 7_665 ? Fe1 Sb5 Sb2 105.95(3) 1_665 1_565 ? Fe1 Sb5 Sb2 105.95(3) 6_667 1_565 ? Fe1 Sb5 Sb2 119.50(3) 4_656 1_565 ? Fe1 Sb5 Sb2 119.50(3) 7_665 1_565 ? Fe1 Sb5 Sm2 147.74(3) 1_665 7_665 ? Fe1 Sb5 Sm2 147.74(3) 6_667 7_665 ? Fe1 Sb5 Sm2 67.30(3) 4_656 7_665 ? Fe1 Sb5 Sm2 67.30(3) 7_665 7_665 ? Sb2 Sb5 Sm2 61.539(19) 1_565 7_665 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 3.595 _refine_diff_density_min -3.493 _refine_diff_density_rms 0.620 # Attachment '- TbFeSb3.cif' data_TbFeSb3 _database_code_depnum_ccdc_archive 'CCDC 768392' #TrackingRef '- TbFeSb3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Tb Fe Sb3' _chemical_formula_sum 'Fe Sb3 Tb' _chemical_formula_weight 580.02 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Tb Tb -0.1723 4.1537 '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' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P b c m ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z-1/2' '-x, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 12.3920(2) _cell_length_b 6.1220(4) _cell_length_c 12.0230(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 912.11(7) _cell_formula_units_Z 8 _cell_measurement_temperature 298(5) _cell_measurement_reflns_used 1528 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 8.448 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1952 _exptl_absorpt_coefficient_mu 35.741 _exptl_absorpt_correction_type sphere _exptl_absorpt_correction_T_min 0.1244 _exptl_absorpt_correction_T_max 0.2681 _exptl_absorpt_process_details 'HKL Scalepack (Otwinowski & Minor 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(5) _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 'Nonius KappaCCD' _diffrn_measurement_method '\w and \scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2496 _diffrn_reflns_av_R_equivalents 0.0370 _diffrn_reflns_av_sigmaI/netI 0.0417 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 30.04 _reflns_number_total 1400 _reflns_number_gt 1297 _reflns_threshold_expression I>2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1069P)^2^+23.9559P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens ? _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0035(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1400 _refine_ls_number_parameters 53 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0612 _refine_ls_R_factor_gt 0.0582 _refine_ls_wR_factor_ref 0.1630 _refine_ls_wR_factor_gt 0.1585 _refine_ls_goodness_of_fit_ref 1.129 _refine_ls_restrained_S_all 1.129 _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 Tb1 Tb 0.69903(7) 0.2500 0.0000 0.0081(3) Uani 1 2 d S . . Tb2 Tb 0.30763(7) 0.27854(14) 0.7500 0.0083(3) Uani 1 2 d S . . Fe1 Fe 0.10468(14) 0.0375(3) 0.86064(14) 0.0113(4) Uani 1 1 d . . . Sb1 Sb 0.97121(9) 0.2500 0.0000 0.0095(3) Uani 1 2 d S . . Sb2 Sb 0.77482(10) 0.26277(17) 0.7500 0.0087(3) Uani 1 2 d S . . Sb3 Sb 0.50330(6) 0.51265(13) 0.87632(6) 0.0086(3) Uani 1 1 d . . . Sb4 Sb 0.22806(10) 0.2500 0.0000 0.0088(3) Uani 1 2 d S . . Sb5 Sb 0.93865(8) 0.89501(18) 0.7500 0.0094(3) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tb1 0.0047(5) 0.0098(4) 0.0099(5) -0.0003(2) 0.000 0.000 Tb2 0.0040(4) 0.0109(4) 0.0099(4) 0.000 0.000 0.0001(2) Fe1 0.0085(8) 0.0122(8) 0.0131(8) -0.0010(6) -0.0004(6) -0.0011(6) Sb1 0.0064(6) 0.0102(5) 0.0118(5) 0.0005(3) 0.000 0.000 Sb2 0.0071(6) 0.0096(5) 0.0093(6) 0.000 0.000 -0.0010(3) Sb3 0.0055(5) 0.0106(4) 0.0097(5) -0.0003(2) 0.0000(2) 0.0001(2) Sb4 0.0077(6) 0.0096(5) 0.0090(6) -0.0008(3) 0.000 0.000 Sb5 0.0041(5) 0.0104(5) 0.0136(5) 0.000 0.000 -0.0012(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tb1 Sb2 3.1500(5) 3_556 ? Tb1 Sb2 3.1500(5) 1_554 ? Tb1 Sb4 3.1916(5) 5_665 ? Tb1 Sb4 3.1916(5) 5_655 ? Tb1 Sb3 3.2571(10) 7_654 ? Tb1 Sb3 3.2571(10) 5_666 ? Tb1 Sb3 3.2680(9) 1_554 ? Tb1 Sb3 3.2680(9) 3_556 ? Tb1 Sb1 3.3728(13) . ? Tb1 Fe1 3.4384(18) 7_664 ? Tb1 Fe1 3.4384(18) 5_656 ? Tb2 Sb5 3.1342(13) 7_655 ? Tb2 Sb2 3.1356(13) 7_665 ? Tb2 Sb4 3.1682(5) 6_556 ? Tb2 Sb4 3.1682(5) 1_556 ? Tb2 Sb3 3.1999(10) 6_557 ? Tb2 Sb3 3.2000(10) . ? Tb2 Fe1 3.2049(19) . ? Tb2 Fe1 3.2049(19) 6_557 ? Tb2 Sb3 3.2320(10) 7_655 ? Tb2 Sb3 3.2320(10) 4_646 ? Tb2 Sb2 3.3188(13) 7_655 ? Fe1 Sb5 2.6008(19) 1_445 ? Fe1 Sb1 2.6059(19) 5_656 ? Fe1 Sb2 2.613(2) 7_655 ? Fe1 Sb4 2.6147(18) 1_556 ? Fe1 Sb5 2.617(2) 7_655 ? Fe1 Fe1 2.660(3) 6_557 ? Fe1 Sb1 2.6898(18) 1_456 ? Fe1 Tb1 3.4384(18) 5_656 ? Sb1 Fe1 2.6059(19) 7_664 ? Sb1 Fe1 2.6059(19) 5_656 ? Sb1 Fe1 2.6898(18) 3_656 ? Sb1 Fe1 2.6898(18) 1_654 ? Sb1 Sb1 3.1431(5) 5_765 ? Sb1 Sb1 3.1431(5) 5_755 ? Sb1 Sb4 3.1829(16) 1_655 ? Sb2 Fe1 2.613(2) 7_665 ? Sb2 Fe1 2.613(2) 4_656 ? Sb2 Sb5 3.0316(15) 1_545 ? Sb2 Tb2 3.1356(13) 7_655 ? Sb2 Tb1 3.1500(5) 6_556 ? Sb2 Tb1 3.1500(5) 1_556 ? Sb2 Tb2 3.3187(13) 7_665 ? Sb3 Sb3 2.9791(13) 5_667 ? Sb3 Sb3 3.0375(13) 6_557 ? Sb3 Sb3 3.0621(2) 7_665 ? Sb3 Sb3 3.0621(2) 7_655 ? Sb3 Tb2 3.2320(10) 7_665 ? Sb3 Tb1 3.2571(10) 5_666 ? Sb3 Tb1 3.2680(9) 1_556 ? Sb4 Fe1 2.6147(18) 3_556 ? Sb4 Fe1 2.6147(18) 1_554 ? Sb4 Tb2 3.1682(5) 3_556 ? Sb4 Tb2 3.1682(5) 1_554 ? Sb4 Sb1 3.1829(16) 1_455 ? Sb4 Tb1 3.1916(5) 5_665 ? Sb4 Tb1 3.1916(5) 5_655 ? Sb5 Fe1 2.6007(19) 1_665 ? Sb5 Fe1 2.6007(19) 6_667 ? Sb5 Fe1 2.617(2) 4_656 ? Sb5 Fe1 2.617(2) 7_665 ? Sb5 Sb2 3.0316(16) 1_565 ? Sb5 Tb2 3.1342(13) 7_665 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Sb2 Tb1 Sb2 145.31(5) 3_556 1_554 ? Sb2 Tb1 Sb4 86.53(2) 3_556 5_665 ? Sb2 Tb1 Sb4 83.79(2) 1_554 5_665 ? Sb2 Tb1 Sb4 83.79(2) 3_556 5_655 ? Sb2 Tb1 Sb4 86.53(2) 1_554 5_655 ? Sb4 Tb1 Sb4 147.11(6) 5_665 5_655 ? Sb2 Tb1 Sb3 130.85(3) 3_556 7_654 ? Sb2 Tb1 Sb3 78.75(3) 1_554 7_654 ? Sb4 Tb1 Sb3 130.23(3) 5_665 7_654 ? Sb4 Tb1 Sb3 77.88(2) 5_655 7_654 ? Sb2 Tb1 Sb3 78.75(3) 3_556 5_666 ? Sb2 Tb1 Sb3 130.85(3) 1_554 5_666 ? Sb4 Tb1 Sb3 77.88(2) 5_665 5_666 ? Sb4 Tb1 Sb3 130.23(3) 5_655 5_666 ? Sb3 Tb1 Sb3 79.33(3) 7_654 5_666 ? Sb2 Tb1 Sb3 131.89(3) 3_556 1_554 ? Sb2 Tb1 Sb3 76.99(3) 1_554 1_554 ? Sb4 Tb1 Sb3 74.82(3) 5_665 1_554 ? Sb4 Tb1 Sb3 133.00(3) 5_655 1_554 ? Sb3 Tb1 Sb3 55.975(14) 7_654 1_554 ? Sb3 Tb1 Sb3 54.33(2) 5_666 1_554 ? Sb2 Tb1 Sb3 76.99(3) 3_556 3_556 ? Sb2 Tb1 Sb3 131.89(3) 1_554 3_556 ? Sb4 Tb1 Sb3 133.00(3) 5_665 3_556 ? Sb4 Tb1 Sb3 74.82(3) 5_655 3_556 ? Sb3 Tb1 Sb3 54.33(2) 7_654 3_556 ? Sb3 Tb1 Sb3 55.975(14) 5_666 3_556 ? Sb3 Tb1 Sb3 84.16(3) 1_554 3_556 ? Sb2 Tb1 Sb1 72.65(3) 3_556 . ? Sb2 Tb1 Sb1 72.65(3) 1_554 . ? Sb4 Tb1 Sb1 73.55(3) 5_665 . ? Sb4 Tb1 Sb1 73.55(3) 5_655 . ? Sb3 Tb1 Sb1 140.333(17) 7_654 . ? Sb3 Tb1 Sb1 140.333(17) 5_666 . ? Sb3 Tb1 Sb1 137.920(16) 1_554 . ? Sb3 Tb1 Sb1 137.920(16) 3_556 . ? Sb2 Tb1 Fe1 105.47(4) 3_556 7_664 ? Sb2 Tb1 Fe1 46.48(4) 1_554 7_664 ? Sb4 Tb1 Fe1 46.27(3) 5_665 7_664 ? Sb4 Tb1 Fe1 106.90(4) 5_655 7_664 ? Sb3 Tb1 Fe1 123.40(3) 7_654 7_664 ? Sb3 Tb1 Fe1 122.59(3) 5_666 7_664 ? Sb3 Tb1 Fe1 92.95(3) 1_554 7_664 ? Sb3 Tb1 Fe1 177.05(4) 3_556 7_664 ? Sb1 Tb1 Fe1 44.97(3) . 7_664 ? Sb2 Tb1 Fe1 46.48(4) 3_556 5_656 ? Sb2 Tb1 Fe1 105.47(4) 1_554 5_656 ? Sb4 Tb1 Fe1 106.90(4) 5_665 5_656 ? Sb4 Tb1 Fe1 46.27(3) 5_655 5_656 ? Sb3 Tb1 Fe1 122.59(3) 7_654 5_656 ? Sb3 Tb1 Fe1 123.40(3) 5_666 5_656 ? Sb3 Tb1 Fe1 177.05(4) 1_554 5_656 ? Sb3 Tb1 Fe1 92.95(3) 3_556 5_656 ? Sb1 Tb1 Fe1 44.97(3) . 5_656 ? Fe1 Tb1 Fe1 89.95(6) 7_664 5_656 ? Sb5 Tb2 Sb2 57.83(3) 7_655 7_665 ? Sb5 Tb2 Sb4 73.11(3) 7_655 6_556 ? Sb2 Tb2 Sb4 87.18(2) 7_665 6_556 ? Sb5 Tb2 Sb4 73.11(3) 7_655 1_556 ? Sb2 Tb2 Sb4 87.18(2) 7_665 1_556 ? Sb4 Tb2 Sb4 143.15(5) 6_556 1_556 ? Sb5 Tb2 Sb3 129.49(3) 7_655 6_557 ? Sb2 Tb2 Sb3 79.83(3) 7_665 6_557 ? Sb4 Tb2 Sb3 79.06(2) 6_556 6_557 ? Sb4 Tb2 Sb3 135.30(3) 1_556 6_557 ? Sb5 Tb2 Sb3 129.49(3) 7_655 . ? Sb2 Tb2 Sb3 79.83(3) 7_665 . ? Sb4 Tb2 Sb3 135.30(3) 6_556 . ? Sb4 Tb2 Sb3 79.06(2) 1_556 . ? Sb3 Tb2 Sb3 56.67(3) 6_557 . ? Sb5 Tb2 Fe1 48.74(4) 7_655 . ? Sb2 Tb2 Fe1 100.34(5) 7_665 . ? Sb4 Tb2 Fe1 97.13(4) 6_556 . ? Sb4 Tb2 Fe1 48.44(4) 1_556 . ? Sb3 Tb2 Fe1 176.18(3) 6_557 . ? Sb3 Tb2 Fe1 127.14(3) . . ? Sb5 Tb2 Fe1 48.74(4) 7_655 6_557 ? Sb2 Tb2 Fe1 100.34(5) 7_665 6_557 ? Sb4 Tb2 Fe1 48.44(4) 6_556 6_557 ? Sb4 Tb2 Fe1 97.13(4) 1_556 6_557 ? Sb3 Tb2 Fe1 127.14(3) 6_557 6_557 ? Sb3 Tb2 Fe1 176.18(3) . 6_557 ? Fe1 Tb2 Fe1 49.05(6) . 6_557 ? Sb5 Tb2 Sb3 145.13(2) 7_655 7_655 ? Sb2 Tb2 Sb3 135.43(3) 7_665 7_655 ? Sb4 Tb2 Sb3 130.07(3) 6_556 7_655 ? Sb4 Tb2 Sb3 75.64(3) 1_556 7_655 ? Sb3 Tb2 Sb3 84.22(2) 6_557 7_655 ? Sb3 Tb2 Sb3 56.856(13) . 7_655 ? Fe1 Tb2 Sb3 98.16(4) . 7_655 ? Fe1 Tb2 Sb3 122.14(4) 6_557 7_655 ? Sb5 Tb2 Sb3 145.13(2) 7_655 4_646 ? Sb2 Tb2 Sb3 135.43(3) 7_665 4_646 ? Sb4 Tb2 Sb3 75.64(3) 6_556 4_646 ? Sb4 Tb2 Sb3 130.07(3) 1_556 4_646 ? Sb3 Tb2 Sb3 56.856(14) 6_557 4_646 ? Sb3 Tb2 Sb3 84.22(2) . 4_646 ? Fe1 Tb2 Sb3 122.14(4) . 4_646 ? Fe1 Tb2 Sb3 98.16(4) 6_557 4_646 ? Sb3 Tb2 Sb3 56.06(3) 7_655 4_646 ? Sb5 Tb2 Sb2 85.22(4) 7_655 7_655 ? Sb2 Tb2 Sb2 143.05(5) 7_665 7_655 ? Sb4 Tb2 Sb2 81.471(19) 6_556 7_655 ? Sb4 Tb2 Sb2 81.471(19) 1_556 7_655 ? Sb3 Tb2 Sb2 131.25(3) 6_557 7_655 ? Sb3 Tb2 Sb2 131.25(3) . 7_655 ? Fe1 Tb2 Sb2 47.19(4) . 7_655 ? Fe1 Tb2 Sb2 47.19(4) 6_557 7_655 ? Sb3 Tb2 Sb2 75.17(3) 7_655 7_655 ? Sb3 Tb2 Sb2 75.17(3) 4_646 7_655 ? Sb5 Fe1 Sb1 79.44(6) 1_445 5_656 ? Sb5 Fe1 Sb2 88.61(6) 1_445 7_655 ? Sb1 Fe1 Sb2 95.66(7) 5_656 7_655 ? Sb5 Fe1 Sb4 163.18(8) 1_445 1_556 ? Sb1 Fe1 Sb4 97.76(6) 5_656 1_556 ? Sb2 Fe1 Sb4 108.20(7) 7_655 1_556 ? Sb5 Fe1 Sb5 81.85(5) 1_445 7_655 ? Sb1 Fe1 Sb5 144.86(8) 5_656 7_655 ? Sb2 Fe1 Sb5 113.38(7) 7_655 7_655 ? Sb4 Fe1 Sb5 91.70(6) 1_556 7_655 ? Sb5 Fe1 Fe1 59.24(4) 1_445 6_557 ? Sb1 Fe1 Fe1 130.01(4) 5_656 6_557 ? Sb2 Fe1 Fe1 59.40(4) 7_655 6_557 ? Sb4 Fe1 Fe1 129.85(4) 1_556 6_557 ? Sb5 Fe1 Fe1 59.45(4) 7_655 6_557 ? Sb5 Fe1 Sb1 89.68(6) 1_445 1_456 ? Sb1 Fe1 Sb1 72.79(5) 5_656 1_456 ? Sb2 Fe1 Sb1 168.45(8) 7_655 1_456 ? Sb4 Fe1 Sb1 73.73(5) 1_556 1_456 ? Sb5 Fe1 Sb1 77.65(5) 7_655 1_456 ? Fe1 Fe1 Sb1 128.53(4) 6_557 1_456 ? Sb5 Fe1 Tb2 124.26(6) 1_445 . ? Sb1 Fe1 Tb2 149.43(7) 5_656 . ? Sb2 Fe1 Tb2 68.69(5) 7_655 . ? Sb4 Fe1 Tb2 65.05(4) 1_556 . ? Sb5 Fe1 Tb2 64.22(5) 7_655 . ? Fe1 Fe1 Tb2 65.48(3) 6_557 . ? Sb1 Fe1 Tb2 121.23(6) 1_456 . ? Sb5 Fe1 Tb1 129.58(7) 1_445 5_656 ? Sb1 Fe1 Tb1 66.18(5) 5_656 5_656 ? Sb2 Fe1 Tb1 60.94(4) 7_655 5_656 ? Sb4 Fe1 Tb1 61.88(4) 1_556 5_656 ? Sb5 Fe1 Tb1 145.19(7) 7_655 5_656 ? Fe1 Fe1 Tb1 119.16(3) 6_557 5_656 ? Sb1 Fe1 Tb1 112.27(6) 1_456 5_656 ? Tb2 Fe1 Tb1 83.27(4) . 5_656 ? Fe1 Sb1 Fe1 137.69(9) 7_664 5_656 ? Fe1 Sb1 Fe1 107.20(5) 7_664 3_656 ? Fe1 Sb1 Fe1 98.51(6) 5_656 3_656 ? Fe1 Sb1 Fe1 98.51(6) 7_664 1_654 ? Fe1 Sb1 Fe1 107.20(5) 5_656 1_654 ? Fe1 Sb1 Fe1 104.11(8) 3_656 1_654 ? Fe1 Sb1 Sb1 54.83(4) 7_664 5_765 ? Fe1 Sb1 Sb1 137.72(4) 5_656 5_765 ? Fe1 Sb1 Sb1 52.37(4) 3_656 5_765 ? Fe1 Sb1 Sb1 109.35(6) 1_654 5_765 ? Fe1 Sb1 Sb1 137.72(4) 7_664 5_755 ? Fe1 Sb1 Sb1 54.83(4) 5_656 5_755 ? Fe1 Sb1 Sb1 109.35(6) 3_656 5_755 ? Fe1 Sb1 Sb1 52.37(4) 1_654 5_755 ? Sb1 Sb1 Sb1 153.75(8) 5_765 5_755 ? Fe1 Sb1 Sb4 111.15(4) 7_664 1_655 ? Fe1 Sb1 Sb4 111.15(4) 5_656 1_655 ? Fe1 Sb1 Sb4 52.05(4) 3_656 1_655 ? Fe1 Sb1 Sb4 52.05(4) 1_654 1_655 ? Sb1 Sb1 Sb4 76.88(4) 5_765 1_655 ? Sb1 Sb1 Sb4 76.88(4) 5_755 1_655 ? Fe1 Sb1 Tb1 68.85(4) 7_664 . ? Fe1 Sb1 Tb1 68.85(4) 5_656 . ? Fe1 Sb1 Tb1 127.95(4) 3_656 . ? Fe1 Sb1 Tb1 127.95(4) 1_654 . ? Sb1 Sb1 Tb1 103.12(4) 5_765 . ? Sb1 Sb1 Tb1 103.12(4) 5_755 . ? Sb4 Sb1 Tb1 180.0 1_655 . ? Fe1 Sb2 Fe1 61.20(8) 7_665 4_656 ? Fe1 Sb2 Sb5 95.47(5) 7_665 1_545 ? Fe1 Sb2 Sb5 95.47(5) 4_656 1_545 ? Fe1 Sb2 Tb2 142.63(5) 7_665 7_655 ? Fe1 Sb2 Tb2 142.63(5) 4_656 7_655 ? Sb5 Sb2 Tb2 61.06(3) 1_545 7_655 ? Fe1 Sb2 Tb1 132.23(5) 7_665 6_556 ? Fe1 Sb2 Tb1 72.58(4) 4_656 6_556 ? Sb5 Sb2 Tb1 100.44(2) 1_545 6_556 ? Tb2 Sb2 Tb1 83.07(2) 7_655 6_556 ? Fe1 Sb2 Tb1 72.58(4) 7_665 1_556 ? Fe1 Sb2 Tb1 132.23(5) 4_656 1_556 ? Sb5 Sb2 Tb1 100.44(2) 1_545 1_556 ? Tb2 Sb2 Tb1 83.07(2) 7_655 1_556 ? Tb1 Sb2 Tb1 145.18(5) 6_556 1_556 ? Fe1 Sb2 Tb2 64.12(5) 7_665 7_665 ? Fe1 Sb2 Tb2 64.12(5) 4_656 7_665 ? Sb5 Sb2 Tb2 155.89(5) 1_545 7_665 ? Tb2 Sb2 Tb2 143.05(5) 7_655 7_665 ? Tb1 Sb2 Tb2 86.09(2) 6_556 7_665 ? Tb1 Sb2 Tb2 86.09(2) 1_556 7_665 ? Sb3 Sb3 Sb3 176.63(3) 5_667 6_557 ? Sb3 Sb3 Sb3 92.94(3) 5_667 7_665 ? Sb3 Sb3 Sb3 90.0 6_557 7_665 ? Sb3 Sb3 Sb3 86.98(3) 5_667 7_655 ? Sb3 Sb3 Sb3 90.0 6_557 7_655 ? Sb3 Sb3 Sb3 176.94(5) 7_665 7_655 ? Sb3 Sb3 Tb2 115.45(4) 5_667 . ? Sb3 Sb3 Tb2 61.665(14) 6_557 . ? Sb3 Sb3 Tb2 115.31(3) 7_665 . ? Sb3 Sb3 Tb2 62.10(3) 7_655 . ? Sb3 Sb3 Tb2 121.01(4) 5_667 7_665 ? Sb3 Sb3 Tb2 61.971(14) 6_557 7_665 ? Sb3 Sb3 Tb2 61.04(2) 7_665 7_665 ? Sb3 Sb3 Tb2 121.52(3) 7_655 7_665 ? Tb2 Sb3 Tb2 123.49(2) . 7_665 ? Sb3 Sb3 Tb1 63.02(2) 5_667 5_666 ? Sb3 Sb3 Tb1 117.164(13) 6_557 5_666 ? Sb3 Sb3 Tb1 62.19(2) 7_665 5_666 ? Sb3 Sb3 Tb1 115.18(3) 7_655 5_666 ? Tb2 Sb3 Tb1 80.40(2) . 5_666 ? Tb2 Sb3 Tb1 123.22(3) 7_665 5_666 ? Sb3 Sb3 Tb1 62.65(3) 5_667 1_556 ? Sb3 Sb3 Tb1 117.066(13) 6_557 1_556 ? Sb3 Sb3 Tb1 120.77(3) 7_665 1_556 ? Sb3 Sb3 Tb1 61.83(2) 7_655 1_556 ? Tb2 Sb3 Tb1 123.92(3) . 1_556 ? Tb2 Sb3 Tb1 85.62(2) 7_665 1_556 ? Tb1 Sb3 Tb1 125.67(2) 5_666 1_556 ? Fe1 Sb4 Fe1 108.43(9) 3_556 1_554 ? Fe1 Sb4 Tb2 66.51(4) 3_556 3_556 ? Fe1 Sb4 Tb2 139.69(5) 1_554 3_556 ? Fe1 Sb4 Tb2 139.69(5) 3_556 1_554 ? Fe1 Sb4 Tb2 66.51(4) 1_554 1_554 ? Tb2 Sb4 Tb2 143.73(6) 3_556 1_554 ? Fe1 Sb4 Sb1 54.22(4) 3_556 1_455 ? Fe1 Sb4 Sb1 54.22(4) 1_554 1_455 ? Tb2 Sb4 Sb1 108.13(3) 3_556 1_455 ? Tb2 Sb4 Sb1 108.13(3) 1_554 1_455 ? Fe1 Sb4 Tb1 71.85(4) 3_556 5_665 ? Fe1 Sb4 Tb1 129.99(5) 1_554 5_665 ? Tb2 Sb4 Tb1 87.98(2) 3_556 5_665 ? Tb2 Sb4 Tb1 81.89(2) 1_554 5_665 ? Sb1 Sb4 Tb1 106.45(3) 1_455 5_665 ? Fe1 Sb4 Tb1 129.99(5) 3_556 5_655 ? Fe1 Sb4 Tb1 71.85(4) 1_554 5_655 ? Tb2 Sb4 Tb1 81.89(2) 3_556 5_655 ? Tb2 Sb4 Tb1 87.98(2) 1_554 5_655 ? Sb1 Sb4 Tb1 106.44(3) 1_455 5_655 ? Tb1 Sb4 Tb1 147.11(6) 5_665 5_655 ? Fe1 Sb5 Fe1 61.53(8) 1_665 6_667 ? Fe1 Sb5 Fe1 134.67(7) 1_665 4_656 ? Fe1 Sb5 Fe1 100.54(7) 6_667 4_656 ? Fe1 Sb5 Fe1 100.54(7) 1_665 7_665 ? Fe1 Sb5 Fe1 134.67(7) 6_667 7_665 ? Fe1 Sb5 Fe1 61.11(8) 4_656 7_665 ? Fe1 Sb5 Sb2 106.30(5) 1_665 1_565 ? Fe1 Sb5 Sb2 106.30(6) 6_667 1_565 ? Fe1 Sb5 Sb2 118.92(5) 4_656 1_565 ? Fe1 Sb5 Sb2 118.92(5) 7_665 1_565 ? Fe1 Sb5 Tb2 147.85(4) 1_665 7_665 ? Fe1 Sb5 Tb2 147.85(4) 6_667 7_665 ? Fe1 Sb5 Tb2 67.04(5) 4_656 7_665 ? Fe1 Sb5 Tb2 67.04(5) 7_665 7_665 ? Sb2 Sb5 Tb2 61.11(3) 1_565 7_665 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 30.04 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 4.899 _refine_diff_density_min -8.530 _refine_diff_density_rms 1.509