# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email cwd@fjirsm.ac.cn _publ_contact_author_name 'Cheng, Wen-Dan' loop_ _publ_author_name 'Ye-Yu Li' 'Wen-Dan Cheng' 'Hao Zhang' 'Chensheng Lin' 'Wei-Long Zhang' 'Lei Geng' 'Guoliang Chai' 'Zhong-Zhen Luo' 'Zhang-Zhen He' data_a1 _database_code_depnum_ccdc_archive 'CCDC 818403' #TrackingRef '- CeBiW2O9.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Bi Ce O9 W2' _chemical_formula_sum 'Bi Ce O9 W2' _chemical_formula_weight 860.80 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Bi Bi -4.1077 10.2566 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 10.2140(11) _cell_length_b 9.9229(10) _cell_length_c 13.7281(16) _cell_angle_alpha 90.00 _cell_angle_beta 102.701(5) _cell_angle_gamma 90.00 _cell_volume 1357.3(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2051 _cell_measurement_theta_min 2.8967 _cell_measurement_theta_max 27.4797 _exptl_crystal_description block _exptl_crystal_colour Reddish-brown _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 8.425 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2888 _exptl_absorpt_coefficient_mu 66.243 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.0388 _exptl_absorpt_correction_T_max 0.0579 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Mercury2 _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 13.6612 _diffrn_standards_number 1652 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 5156 _diffrn_reflns_av_R_equivalents 0.0626 _diffrn_reflns_av_sigmaI/netI 0.0639 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 27.49 _reflns_number_total 1559 _reflns_number_gt 1381 _reflns_threshold_expression >2sigma(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^)+(0.0563P)^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 0.00345(12) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1559 _refine_ls_number_parameters 120 _refine_ls_number_restraints 66 _refine_ls_R_factor_all 0.0408 _refine_ls_R_factor_gt 0.0377 _refine_ls_wR_factor_ref 0.0991 _refine_ls_wR_factor_gt 0.0973 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.032 _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 Ce1 Ce 0.64969(9) 0.52109(8) 0.61715(6) 0.0081(2) Uani 1 1 d U . . Bi1 Bi 1.06202(6) 0.41016(6) 0.63987(5) 0.0137(2) Uani 1 1 d . . . W1 W 0.79434(5) 0.20352(5) 0.61818(4) 0.0026(2) Uani 1 1 d . . . W2 W 0.92568(6) 0.76331(6) 0.63509(4) 0.0038(2) Uani 1 1 d . . . O1 O 0.6338(10) 0.2804(10) 0.6304(8) 0.008(2) Uani 1 1 d U . . O2 O 1.0000 0.6384(14) 0.7500 0.005(3) Uani 1 2 d SU . . O3 O 0.7529(12) 0.7555(11) 0.6424(9) 0.011(2) Uani 1 1 d U . . O4 O 0.8638(11) 0.3804(10) 0.6935(8) 0.008(2) Uani 1 1 d U . . O5 O 0.7904(10) 0.0687(11) 0.7021(8) 0.007(2) Uani 1 1 d U . . O6 O 1.0000 0.8860(14) 0.7500 0.005(3) Uani 1 2 d SU . . O7 O 0.9790(11) 0.2019(11) 0.6165(9) 0.008(2) Uani 1 1 d U . . O8 O 0.7291(10) 0.1217(10) 0.5001(8) 0.006(2) Uani 1 1 d U . . O9 O 0.9223(11) 0.9122(10) 0.5539(8) 0.009(2) Uani 1 1 d U . . O10 O 0.9214(12) 0.6214(11) 0.5536(9) 0.014(2) Uani 1 1 d U . . 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 Ce1 0.0125(5) 0.0039(4) 0.0057(4) -0.0028(3) -0.0032(3) 0.0031(3) Bi1 0.0124(4) 0.0122(4) 0.0144(4) 0.0004(3) -0.0018(3) -0.0023(2) W1 0.0037(3) 0.0004(3) 0.0029(3) -0.0002(2) -0.0007(2) 0.00001(19) W2 0.0046(3) 0.0027(3) 0.0033(3) 0.0001(2) -0.0011(2) 0.00020(19) O1 0.008(3) 0.008(3) 0.007(3) -0.0005(19) 0.0013(19) -0.0004(19) O2 0.005(3) 0.004(3) 0.005(3) 0.000 0.000(2) 0.000 O3 0.012(3) 0.010(3) 0.010(3) 0.0000(19) 0.0018(19) -0.0011(19) O4 0.009(3) 0.007(3) 0.008(3) -0.0026(19) 0.0008(19) -0.0008(19) O5 0.008(3) 0.006(3) 0.007(3) 0.0004(19) 0.0020(19) -0.0005(19) O6 0.005(3) 0.004(3) 0.004(3) 0.000 0.001(2) 0.000 O7 0.008(3) 0.009(3) 0.009(3) -0.0003(19) 0.0028(19) 0.0002(19) O8 0.007(3) 0.006(3) 0.006(3) 0.0015(19) 0.0016(19) -0.0003(18) O9 0.010(3) 0.008(3) 0.009(3) 0.0002(19) 0.0014(19) -0.0004(19) O10 0.015(3) 0.012(3) 0.015(3) -0.0001(19) 0.0015(19) -0.0002(19) _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 Ce1 O9 2.395(11) 7_666 ? Ce1 O1 2.404(10) . ? Ce1 O5 2.467(11) 4_656 ? Ce1 O7 2.500(11) 3_455 ? Ce1 O9 2.536(11) 3_445 ? Ce1 O3 2.546(11) . ? Ce1 O4 2.612(11) . ? Ce1 O8 2.647(11) 7_656 ? Ce1 O6 2.948(6) 3_445 ? Ce1 W2 3.4767(11) 3_445 ? Ce1 W1 3.4791(10) . ? Ce1 W2 3.6713(11) . ? Bi1 O7 2.230(11) . ? Bi1 O4 2.265(11) 2_756 ? Bi1 O4 2.320(11) . ? Bi1 O3 2.475(11) 3_545 ? Bi1 O10 2.667(11) . ? Bi1 O10 2.716(12) 5_766 ? Bi1 W1 3.3780(9) . ? Bi1 Bi1 3.5262(14) 2_756 ? W1 O5 1.772(11) . ? W1 O8 1.805(10) . ? W1 O1 1.849(10) . ? W1 O7 1.892(11) . ? W1 O4 2.081(10) . ? W1 O8 2.352(10) 7_656 ? W2 O3 1.791(12) . ? W2 O10 1.793(11) . ? W2 O9 1.846(11) . ? W2 O6 2.005(8) . ? W2 O2 2.019(9) . ? W2 O1 2.147(10) 3 ? W2 W2 3.1864(12) 2_756 ? W2 Ce1 3.4767(11) 3 ? O1 W2 2.147(10) 3_445 ? O2 W2 2.019(9) 2_756 ? O3 Bi1 2.475(11) 3_455 ? O4 Bi1 2.265(11) 2_756 ? O5 Ce1 2.467(11) 4_646 ? O6 W2 2.005(8) 2_756 ? O6 Ce1 2.948(6) 4_656 ? O6 Ce1 2.948(6) 3 ? O7 Ce1 2.500(11) 3_545 ? O8 W1 2.352(10) 7_656 ? O8 Ce1 2.647(11) 7_656 ? O9 Ce1 2.395(11) 7_666 ? O9 Ce1 2.536(11) 3 ? O10 Bi1 2.716(12) 5_766 ? 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 O9 Ce1 O1 109.8(3) 7_666 . ? O9 Ce1 O5 152.6(4) 7_666 4_656 ? O1 Ce1 O5 96.9(3) . 4_656 ? O9 Ce1 O7 74.6(4) 7_666 3_455 ? O1 Ce1 O7 130.9(4) . 3_455 ? O5 Ce1 O7 83.4(4) 4_656 3_455 ? O9 Ce1 O9 73.8(4) 7_666 3_445 ? O1 Ce1 O9 62.0(3) . 3_445 ? O5 Ce1 O9 115.6(4) 4_656 3_445 ? O7 Ce1 O9 73.7(3) 3_455 3_445 ? O9 Ce1 O3 84.8(4) 7_666 . ? O1 Ce1 O3 158.5(4) . . ? O5 Ce1 O3 71.6(4) 4_656 . ? O7 Ce1 O3 67.2(4) 3_455 . ? O9 Ce1 O3 139.2(4) 3_445 . ? O9 Ce1 O4 126.2(4) 7_666 . ? O1 Ce1 O4 60.2(3) . . ? O5 Ce1 O4 72.4(3) 4_656 . ? O7 Ce1 O4 155.0(4) 3_455 . ? O9 Ce1 O4 122.2(3) 3_445 . ? O3 Ce1 O4 98.5(3) . . ? O9 Ce1 O8 68.6(3) 7_666 7_656 ? O1 Ce1 O8 64.1(3) . 7_656 ? O5 Ce1 O8 131.9(3) 4_656 7_656 ? O7 Ce1 O8 143.2(3) 3_455 7_656 ? O9 Ce1 O8 94.6(3) 3_445 7_656 ? O3 Ce1 O8 109.7(3) . 7_656 ? O4 Ce1 O8 59.7(3) . 7_656 ? O9 Ce1 O6 130.1(3) 7_666 3_445 ? O1 Ce1 O6 56.5(3) . 3_445 ? O5 Ce1 O6 60.8(3) 4_656 3_445 ? O7 Ce1 O6 82.7(3) 3_455 3_445 ? O9 Ce1 O6 57.1(3) 3_445 3_445 ? O3 Ce1 O6 125.9(3) . 3_445 ? O4 Ce1 O6 90.6(3) . 3_445 ? O8 Ce1 O6 120.6(3) 7_656 3_445 ? O9 Ce1 W2 102.0(3) 7_666 3_445 ? O1 Ce1 W2 37.5(2) . 3_445 ? O5 Ce1 W2 95.2(3) 4_656 3_445 ? O7 Ce1 W2 93.4(3) 3_455 3_445 ? O9 Ce1 W2 31.0(2) 3_445 3_445 ? O3 Ce1 W2 157.2(3) . 3_445 ? O4 Ce1 W2 94.8(2) . 3_445 ? O8 Ce1 W2 93.0(2) 7_656 3_445 ? O6 Ce1 W2 35.16(17) 3_445 3_445 ? O9 Ce1 W1 107.0(3) 7_666 . ? O1 Ce1 W1 30.2(2) . . ? O5 Ce1 W1 99.1(2) 4_656 . ? O7 Ce1 W1 160.9(3) 3_455 . ? O9 Ce1 W1 88.4(2) 3_445 . ? O3 Ce1 W1 131.6(3) . . ? O4 Ce1 W1 36.6(2) . . ? O8 Ce1 W1 42.5(2) 7_656 . ? O6 Ce1 W1 82.1(2) 3_445 . ? W2 Ce1 W1 67.59(2) 3_445 . ? O9 Ce1 W2 87.2(3) 7_666 . ? O1 Ce1 W2 135.2(2) . . ? O5 Ce1 W2 77.9(2) 4_656 . ? O7 Ce1 W2 93.2(3) 3_455 . ? O9 Ce1 W2 159.1(2) 3_445 . ? O3 Ce1 W2 26.3(3) . . ? O4 Ce1 W2 76.1(2) . . ? O8 Ce1 W2 86.4(2) 7_656 . ? O6 Ce1 W2 138.71(13) 3_445 . ? W2 Ce1 W2 169.90(3) 3_445 . ? W1 Ce1 W2 105.88(3) . . ? O7 Bi1 O4 93.3(4) . 2_756 ? O7 Bi1 O4 66.2(4) . . ? O4 Bi1 O4 77.5(4) 2_756 . ? O7 Bi1 O3 72.6(4) . 3_545 ? O4 Bi1 O3 79.5(4) 2_756 3_545 ? O4 Bi1 O3 131.0(4) . 3_545 ? O7 Bi1 O10 120.9(4) . . ? O4 Bi1 O10 125.4(4) 2_756 . ? O4 Bi1 O10 79.6(4) . . ? O3 Bi1 O10 147.0(4) 3_545 . ? O7 Bi1 O10 81.7(4) . 5_766 ? O4 Bi1 O10 153.3(4) 2_756 5_766 ? O4 Bi1 O10 122.8(4) . 5_766 ? O3 Bi1 O10 74.0(4) 3_545 5_766 ? O10 Bi1 O10 78.5(4) . 5_766 ? O7 Bi1 W1 31.8(3) . . ? O4 Bi1 W1 95.4(3) 2_756 . ? O4 Bi1 W1 37.3(3) . . ? O3 Bi1 W1 104.2(3) 3_545 . ? O10 Bi1 W1 95.2(2) . . ? O10 Bi1 W1 93.9(2) 5_766 . ? O7 Bi1 Bi1 85.8(3) . 2_756 ? O4 Bi1 Bi1 40.3(3) 2_756 2_756 ? O4 Bi1 Bi1 39.2(3) . 2_756 ? O3 Bi1 Bi1 114.7(3) 3_545 2_756 ? O10 Bi1 Bi1 96.9(3) . 2_756 ? O10 Bi1 Bi1 161.8(2) 5_766 2_756 ? W1 Bi1 Bi1 68.84(2) . 2_756 ? O5 W1 O8 100.8(5) . . ? O5 W1 O1 96.0(5) . . ? O8 W1 O1 96.2(5) . . ? O5 W1 O7 99.6(5) . . ? O8 W1 O7 99.0(5) . . ? O1 W1 O7 155.7(5) . . ? O5 W1 O4 111.6(5) . . ? O8 W1 O4 147.6(4) . . ? O1 W1 O4 79.6(4) . . ? O7 W1 O4 77.4(4) . . ? O5 W1 O8 172.9(4) . 7_656 ? O8 W1 O8 75.5(5) . 7_656 ? O1 W1 O8 78.5(4) . 7_656 ? O7 W1 O8 87.0(4) . 7_656 ? O4 W1 O8 72.1(4) . 7_656 ? O5 W1 Bi1 122.3(3) . . ? O8 W1 Bi1 119.0(3) . . ? O1 W1 Bi1 117.3(3) . . ? O7 W1 Bi1 38.4(3) . . ? O4 W1 Bi1 42.5(3) . . ? O8 W1 Bi1 64.6(2) 7_656 . ? O5 W1 Ce1 128.1(3) . . ? O8 W1 Ce1 109.3(3) . . ? O1 W1 Ce1 40.8(3) . . ? O7 W1 Ce1 115.6(3) . . ? O4 W1 Ce1 48.4(3) . . ? O8 W1 Ce1 49.5(3) 7_656 . ? Bi1 W1 Ce1 77.60(2) . . ? O3 W2 O10 96.4(5) . . ? O3 W2 O9 100.4(5) . . ? O10 W2 O9 104.9(5) . . ? O3 W2 O6 100.9(4) . . ? O10 W2 O6 157.1(4) . . ? O9 W2 O6 86.7(4) . . ? O3 W2 O2 97.8(4) . . ? O10 W2 O2 87.7(5) . . ? O9 W2 O2 156.5(4) . . ? O6 W2 O2 75.3(4) . . ? O3 W2 O1 177.5(5) . 3 ? O10 W2 O1 86.1(5) . 3 ? O9 W2 O1 78.8(4) . 3 ? O6 W2 O1 76.7(3) . 3 ? O2 W2 O1 82.4(3) . 3 ? O3 W2 W2 101.9(4) . 2_756 ? O10 W2 W2 124.0(4) . 2_756 ? O9 W2 W2 122.6(3) . 2_756 ? O6 W2 W2 37.4(3) . 2_756 ? O2 W2 W2 37.9(3) . 2_756 ? O1 W2 W2 76.7(3) 3 2_756 ? O3 W2 Ce1 135.0(3) . 3 ? O10 W2 Ce1 117.4(4) . 3 ? O9 W2 Ce1 45.1(3) . 3 ? O6 W2 Ce1 57.85(19) . 3 ? O2 W2 Ce1 111.5(2) . 3 ? O1 W2 Ce1 43.0(3) 3 3 ? W2 W2 Ce1 83.82(2) 2_756 3 ? O3 W2 Ce1 39.1(3) . . ? O10 W2 Ce1 62.0(4) . . ? O9 W2 Ce1 124.8(3) . . ? O6 W2 Ce1 127.05(15) . . ? O2 W2 Ce1 78.6(2) . . ? O1 W2 Ce1 143.2(3) 3 . ? W2 W2 Ce1 104.96(2) 2_756 . ? Ce1 W2 Ce1 169.90(3) 3 . ? W1 O1 W2 150.9(6) . 3_445 ? W1 O1 Ce1 109.1(5) . . ? W2 O1 Ce1 99.5(4) 3_445 . ? W2 O2 W2 104.2(6) 2_756 . ? W2 O3 Bi1 139.0(6) . 3_455 ? W2 O3 Ce1 114.5(5) . . ? Bi1 O3 Ce1 105.3(4) 3_455 . ? W1 O4 Bi1 127.8(5) . 2_756 ? W1 O4 Bi1 100.1(4) . . ? Bi1 O4 Bi1 100.5(4) 2_756 . ? W1 O4 Ce1 95.0(4) . . ? Bi1 O4 Ce1 113.6(4) 2_756 . ? Bi1 O4 Ce1 121.1(5) . . ? W1 O5 Ce1 139.7(6) . 4_646 ? W2 O6 W2 105.2(6) . 2_756 ? W2 O6 Ce1 127.22(7) . 4_656 ? W2 O6 Ce1 86.99(3) 2_756 4_656 ? W2 O6 Ce1 86.99(3) . 3 ? W2 O6 Ce1 127.22(7) 2_756 3 ? Ce1 O6 Ce1 125.9(5) 4_656 3 ? W1 O7 Bi1 109.8(5) . . ? W1 O7 Ce1 134.6(5) . 3_545 ? Bi1 O7 Ce1 114.9(4) . 3_545 ? W1 O8 W1 104.5(5) . 7_656 ? W1 O8 Ce1 131.1(5) . 7_656 ? W1 O8 Ce1 88.0(3) 7_656 7_656 ? W2 O9 Ce1 140.7(6) . 7_666 ? W2 O9 Ce1 103.9(5) . 3 ? Ce1 O9 Ce1 106.2(4) 7_666 3 ? W2 O10 Bi1 113.8(5) . . ? W2 O10 Bi1 134.6(6) . 5_766 ? Bi1 O10 Bi1 101.5(4) . 5_766 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 3.559 _refine_diff_density_min -4.211 _refine_diff_density_rms 0.787 # Attachment '- ErBiW2O9.CIF' data_a2 _database_code_depnum_ccdc_archive 'CCDC 818404' #TrackingRef '- ErBiW2O9.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Bi Er O9 W2' _chemical_formula_sum 'Bi Er O9 W2' _chemical_formula_weight 887.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Bi Bi -4.1077 10.2566 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 32.112(2) _cell_length_b 5.6402(2) _cell_length_c 3.9579(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 716.85(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1824 _cell_measurement_theta_min 2.5370 _cell_measurement_theta_max 27.4603 _exptl_crystal_description strip _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 8.227 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1484 _exptl_absorpt_coefficient_mu 68.072 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.0450 _exptl_absorpt_correction_T_max 0.2346 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Mercury2 _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 13.6612 _diffrn_standards_number 1038 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5104 _diffrn_reflns_av_R_equivalents 0.0754 _diffrn_reflns_av_sigmaI/netI 0.0520 _diffrn_reflns_limit_h_min -41 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 27.46 _reflns_number_total 896 _reflns_number_gt 851 _reflns_threshold_expression >2sigma(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^)+(0.0419P)^2^+11.1456P] 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 0.00092(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 896 _refine_ls_number_parameters 71 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0383 _refine_ls_R_factor_gt 0.0354 _refine_ls_wR_factor_ref 0.0900 _refine_ls_wR_factor_gt 0.0879 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.055 _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 Er1 Er 0.16670(2) -0.2500 0.73853(16) 0.0048(2) Uani 1 2 d S . . Bi1 Bi -0.027803(19) 0.2500 0.71176(16) 0.0081(2) Uani 1 2 d S . . W1 W 0.29397(2) -0.2500 0.79683(16) 0.0043(2) Uani 1 2 d S . . W2 W 0.07864(2) 0.2500 0.79528(17) 0.0049(2) Uani 1 2 d S . . O1 O -0.2591(4) -0.2500 -0.227(3) 0.013(3) Uani 1 2 d SU . . O2 O 0.0280(3) 0.0214(15) 0.7400(17) 0.0084(19) Uani 1 1 d U . . O3 O -0.0733(4) -0.2500 0.749(3) 0.015(3) Uani 1 2 d SU . . O4 O -0.2005(4) -0.2500 0.259(3) 0.020(3) Uani 1 2 d SU . . O5 O -0.1119(3) -0.0020(14) 0.265(2) 0.020(2) Uani 1 1 d U . . O6 O -0.3214(3) -0.0232(15) -0.7315(19) 0.014(2) Uani 1 1 d U . . 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 Er1 0.0028(4) 0.0064(4) 0.0052(4) 0.000 -0.0004(2) 0.000 Bi1 0.0057(4) 0.0064(3) 0.0120(4) 0.000 0.0011(2) 0.000 W1 0.0060(4) 0.0015(3) 0.0053(4) 0.000 0.0001(2) 0.000 W2 0.0040(4) 0.0045(3) 0.0063(4) 0.000 -0.0001(2) 0.000 O1 0.012(3) 0.013(3) 0.013(3) 0.000 -0.0016(19) 0.000 O2 0.008(2) 0.008(2) 0.009(2) -0.0003(16) 0.0000(17) 0.0009(17) O3 0.014(3) 0.016(3) 0.014(3) 0.000 0.0006(19) 0.000 O4 0.020(4) 0.022(4) 0.019(4) 0.000 -0.0004(19) 0.000 O5 0.019(3) 0.021(3) 0.021(3) 0.0004(18) -0.0005(17) 0.0024(18) O6 0.014(3) 0.013(2) 0.014(3) 0.0002(17) 0.0007(17) -0.0001(18) _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 Er1 O5 2.262(10) 4_546 ? Er1 O5 2.262(10) 5_556 ? Er1 O6 2.364(8) 6_656 ? Er1 O6 2.364(8) 3_545 ? Er1 O1 2.384(14) 6_656 ? Er1 O6 2.411(8) 3_544 ? Er1 O6 2.411(8) 6_655 ? Er1 W1 3.5502(6) 2_544 ? Er1 W1 3.5502(6) 2_554 ? Er1 Er1 3.95790(19) 1_554 ? Er1 Er1 3.9579(2) 1_556 ? Bi1 O2 2.210(8) 8_565 ? Bi1 O2 2.210(8) . ? Bi1 O2 2.354(7) 5_556 ? Bi1 O2 2.354(7) 4_556 ? Bi1 O2 2.655(7) 4_557 ? Bi1 O2 2.655(7) 5_557 ? Bi1 W2 3.4341(10) . ? W1 O1 1.725(14) 6_656 ? W1 O4 1.766(12) 6_657 ? W1 O6 1.793(9) 5 ? W1 O6 1.793(9) 4_545 ? W1 O4 2.208(12) 6_656 ? W1 Er1 3.5502(6) 2 ? W1 Er1 3.5502(6) 2_545 ? W2 O5 1.776(9) 4_556 ? W2 O5 1.776(9) 5_556 ? W2 O3 1.811(12) 5_557 ? W2 O2 2.087(8) . ? W2 O2 2.087(8) 8_565 ? W2 O3 2.161(12) 5_556 ? O1 W1 1.725(14) 6_556 ? O1 Er1 2.384(14) 6_556 ? O2 Bi1 2.354(7) 5_556 ? O2 Bi1 2.655(7) 5_557 ? O3 W2 1.811(12) 5_557 ? O3 W2 2.161(12) 5_556 ? O4 W1 1.766(12) 6_557 ? O4 W1 2.208(12) 6_556 ? O5 W2 1.776(9) 5_556 ? O5 Er1 2.262(10) 5_556 ? O6 W1 1.793(9) 5 ? O6 Er1 2.364(8) 6_556 ? O6 Er1 2.411(8) 6 ? 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 O5 Er1 O5 77.9(5) 4_546 5_556 ? O5 Er1 O6 118.1(3) 4_546 6_656 ? O5 Er1 O6 77.9(3) 5_556 6_656 ? O5 Er1 O6 77.9(3) 4_546 3_545 ? O5 Er1 O6 118.1(3) 5_556 3_545 ? O6 Er1 O6 65.5(4) 6_656 3_545 ? O5 Er1 O1 141.0(2) 4_546 6_656 ? O5 Er1 O1 141.0(2) 5_556 6_656 ? O6 Er1 O1 81.6(3) 6_656 6_656 ? O6 Er1 O1 81.6(3) 3_545 6_656 ? O5 Er1 O6 77.6(3) 4_546 3_544 ? O5 Er1 O6 116.9(3) 5_556 3_544 ? O6 Er1 O6 161.5(4) 6_656 3_544 ? O6 Er1 O6 112.0(3) 3_545 3_544 ? O1 Er1 O6 79.9(3) 6_656 3_544 ? O5 Er1 O6 116.9(3) 4_546 6_655 ? O5 Er1 O6 77.6(3) 5_556 6_655 ? O6 Er1 O6 112.0(4) 6_656 6_655 ? O6 Er1 O6 161.5(4) 3_545 6_655 ? O1 Er1 O6 79.9(3) 6_656 6_655 ? O6 Er1 O6 64.1(4) 3_544 6_655 ? O5 Er1 W1 77.0(2) 4_546 2_544 ? O5 Er1 W1 140.6(2) 5_556 2_544 ? O6 Er1 W1 141.1(2) 6_656 2_544 ? O6 Er1 W1 85.3(2) 3_545 2_544 ? O1 Er1 W1 68.58(14) 6_656 2_544 ? O6 Er1 W1 27.4(2) 3_544 2_544 ? O6 Er1 W1 87.4(2) 6_655 2_544 ? O5 Er1 W1 140.6(2) 4_546 2_554 ? O5 Er1 W1 77.0(2) 5_556 2_554 ? O6 Er1 W1 85.3(2) 6_656 2_554 ? O6 Er1 W1 141.1(2) 3_545 2_554 ? O1 Er1 W1 68.58(14) 6_656 2_554 ? O6 Er1 W1 87.4(2) 3_544 2_554 ? O6 Er1 W1 27.4(2) 6_655 2_554 ? W1 Er1 W1 105.19(3) 2_544 2_554 ? O5 Er1 Er1 89.6(2) 4_546 1_554 ? O5 Er1 Er1 89.6(2) 5_556 1_554 ? O6 Er1 Er1 145.6(2) 6_656 1_554 ? O6 Er1 Er1 145.6(2) 3_545 1_554 ? O1 Er1 Er1 88.9(3) 6_656 1_554 ? O6 Er1 Er1 33.6(2) 3_544 1_554 ? O6 Er1 Er1 33.6(2) 6_655 1_554 ? W1 Er1 Er1 60.500(14) 2_544 1_554 ? W1 Er1 Er1 60.500(14) 2_554 1_554 ? O5 Er1 Er1 90.4(2) 4_546 1_556 ? O5 Er1 Er1 90.4(2) 5_556 1_556 ? O6 Er1 Er1 34.4(2) 6_656 1_556 ? O6 Er1 Er1 34.4(2) 3_545 1_556 ? O1 Er1 Er1 91.1(3) 6_656 1_556 ? O6 Er1 Er1 146.4(2) 3_544 1_556 ? O6 Er1 Er1 146.4(2) 6_655 1_556 ? W1 Er1 Er1 119.500(14) 2_544 1_556 ? W1 Er1 Er1 119.500(14) 2_554 1_556 ? Er1 Er1 Er1 180.0 1_554 1_556 ? O2 Bi1 O2 71.4(4) 8_565 . ? O2 Bi1 O2 114.83(14) 8_565 5_556 ? O2 Bi1 O2 70.2(3) . 5_556 ? O2 Bi1 O2 70.2(3) 8_565 4_556 ? O2 Bi1 O2 114.83(14) . 4_556 ? O2 Bi1 O2 81.1(4) 5_556 4_556 ? O2 Bi1 O2 67.9(3) 8_565 4_557 ? O2 Bi1 O2 107.26(15) . 4_557 ? O2 Bi1 O2 174.6(2) 5_556 4_557 ? O2 Bi1 O2 104.2(3) 4_556 4_557 ? O2 Bi1 O2 107.26(15) 8_565 5_557 ? O2 Bi1 O2 67.9(3) . 5_557 ? O2 Bi1 O2 104.2(3) 5_556 5_557 ? O2 Bi1 O2 174.6(2) 4_556 5_557 ? O2 Bi1 O2 70.4(3) 4_557 5_557 ? O2 Bi1 W2 35.7(2) 8_565 . ? O2 Bi1 W2 35.7(2) . . ? O2 Bi1 W2 94.3(2) 5_556 . ? O2 Bi1 W2 94.3(2) 4_556 . ? O2 Bi1 W2 85.62(18) 4_557 . ? O2 Bi1 W2 85.62(18) 5_557 . ? O1 W1 O4 105.0(6) 6_656 6_657 ? O1 W1 O6 117.4(3) 6_656 5 ? O4 W1 O6 95.4(3) 6_657 5 ? O1 W1 O6 117.4(3) 6_656 4_545 ? O4 W1 O6 95.4(3) 6_657 4_545 ? O6 W1 O6 118.5(6) 5 4_545 ? O1 W1 O4 85.4(5) 6_656 6_656 ? O4 W1 O4 169.7(8) 6_657 6_656 ? O6 W1 O4 79.5(3) 5 6_656 ? O6 W1 O4 79.5(3) 4_545 6_656 ? O1 W1 Er1 115.48(17) 6_656 2 ? O4 W1 Er1 58.29(16) 6_657 2 ? O6 W1 Er1 38.2(2) 5 2 ? O6 W1 Er1 125.4(3) 4_545 2 ? O4 W1 Er1 117.54(16) 6_656 2 ? O1 W1 Er1 115.48(17) 6_656 2_545 ? O4 W1 Er1 58.29(16) 6_657 2_545 ? O6 W1 Er1 125.4(3) 5 2_545 ? O6 W1 Er1 38.2(2) 4_545 2_545 ? O4 W1 Er1 117.54(16) 6_656 2_545 ? Er1 W1 Er1 105.19(3) 2 2_545 ? O5 W2 O5 103.9(7) 4_556 5_556 ? O5 W2 O3 101.0(4) 4_556 5_557 ? O5 W2 O3 101.0(4) 5_556 5_557 ? O5 W2 O2 160.3(4) 4_556 . ? O5 W2 O2 88.2(4) 5_556 . ? O3 W2 O2 91.8(4) 5_557 . ? O5 W2 O2 88.2(4) 4_556 8_565 ? O5 W2 O2 160.3(4) 5_556 8_565 ? O3 W2 O2 91.8(4) 5_557 8_565 ? O2 W2 O2 76.3(5) . 8_565 ? O5 W2 O3 85.0(4) 4_556 5_556 ? O5 W2 O3 85.0(4) 5_556 5_556 ? O3 W2 O3 170.1(8) 5_557 5_556 ? O2 W2 O3 80.5(3) . 5_556 ? O2 W2 O3 80.5(3) 8_565 5_556 ? O5 W2 Bi1 125.9(3) 4_556 . ? O5 W2 Bi1 125.9(3) 5_556 . ? O3 W2 Bi1 90.1(4) 5_557 . ? O2 W2 Bi1 38.2(2) . . ? O2 W2 Bi1 38.2(2) 8_565 . ? O3 W2 Bi1 80.0(3) 5_556 . ? W1 O1 Er1 169.6(6) 6_556 6_556 ? W2 O2 Bi1 106.1(3) . . ? W2 O2 Bi1 118.9(3) . 5_556 ? Bi1 O2 Bi1 109.8(3) . 5_556 ? W2 O2 Bi1 105.8(3) . 5_557 ? Bi1 O2 Bi1 112.1(3) . 5_557 ? Bi1 O2 Bi1 104.2(3) 5_556 5_557 ? W2 O3 W2 170.1(8) 5_557 5_556 ? W1 O4 W1 169.7(8) 6_557 6_556 ? W2 O5 Er1 164.1(6) 5_556 5_556 ? W1 O6 Er1 131.6(4) 5 6_556 ? W1 O6 Er1 114.5(4) 5 6 ? Er1 O6 Er1 112.0(3) 6_556 6 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Bi1 W2 O5 -11.0(5) 8_565 . . 4_556 ? O2 Bi1 W2 O5 163.6(5) . . . 4_556 ? O2 Bi1 W2 O5 117.0(4) 5_556 . . 4_556 ? O2 Bi1 W2 O5 35.6(4) 4_556 . . 4_556 ? O2 Bi1 W2 O5 -68.4(4) 4_557 . . 4_556 ? O2 Bi1 W2 O5 -139.0(4) 5_557 . . 4_556 ? O2 Bi1 W2 O5 -163.6(5) 8_565 . . 5_556 ? O2 Bi1 W2 O5 11.0(5) . . . 5_556 ? O2 Bi1 W2 O5 -35.6(4) 5_556 . . 5_556 ? O2 Bi1 W2 O5 -117.0(4) 4_556 . . 5_556 ? O2 Bi1 W2 O5 139.0(4) 4_557 . . 5_556 ? O2 Bi1 W2 O5 68.4(4) 5_557 . . 5_556 ? O2 Bi1 W2 O3 92.7(3) 8_565 . . 5_557 ? O2 Bi1 W2 O3 -92.7(3) . . . 5_557 ? O2 Bi1 W2 O3 -139.30(19) 5_556 . . 5_557 ? O2 Bi1 W2 O3 139.30(19) 4_556 . . 5_557 ? O2 Bi1 W2 O3 35.32(17) 4_557 . . 5_557 ? O2 Bi1 W2 O3 -35.32(17) 5_557 . . 5_557 ? O2 Bi1 W2 O2 -174.6(6) 8_565 . . . ? O2 Bi1 W2 O2 -46.6(4) 5_556 . . . ? O2 Bi1 W2 O2 -128.0(2) 4_556 . . . ? O2 Bi1 W2 O2 128.0(3) 4_557 . . . ? O2 Bi1 W2 O2 57.4(4) 5_557 . . . ? O2 Bi1 W2 O2 174.6(6) . . . 8_565 ? O2 Bi1 W2 O2 128.0(2) 5_556 . . 8_565 ? O2 Bi1 W2 O2 46.6(4) 4_556 . . 8_565 ? O2 Bi1 W2 O2 -57.4(4) 4_557 . . 8_565 ? O2 Bi1 W2 O2 -128.0(3) 5_557 . . 8_565 ? O2 Bi1 W2 O3 -87.3(3) 8_565 . . 5_556 ? O2 Bi1 W2 O3 87.3(3) . . . 5_556 ? O2 Bi1 W2 O3 40.70(19) 5_556 . . 5_556 ? O2 Bi1 W2 O3 -40.70(19) 4_556 . . 5_556 ? O2 Bi1 W2 O3 -144.68(17) 4_557 . . 5_556 ? O2 Bi1 W2 O3 144.68(17) 5_557 . . 5_556 ? O5 W2 O2 Bi1 -42.6(12) 4_556 . . . ? O5 W2 O2 Bi1 -171.1(4) 5_556 . . . ? O3 W2 O2 Bi1 88.0(4) 5_557 . . . ? O2 W2 O2 Bi1 -3.4(4) 8_565 . . . ? O3 W2 O2 Bi1 -85.9(3) 5_556 . . . ? O5 W2 O2 Bi1 81.6(11) 4_556 . . 5_556 ? O5 W2 O2 Bi1 -47.0(4) 5_556 . . 5_556 ? O3 W2 O2 Bi1 -147.9(4) 5_557 . . 5_556 ? O2 W2 O2 Bi1 120.7(3) 8_565 . . 5_556 ? O3 W2 O2 Bi1 38.3(4) 5_556 . . 5_556 ? Bi1 W2 O2 Bi1 124.2(5) . . . 5_556 ? O5 W2 O2 Bi1 -161.8(9) 4_556 . . 5_557 ? O5 W2 O2 Bi1 69.7(4) 5_556 . . 5_557 ? O3 W2 O2 Bi1 -31.3(4) 5_557 . . 5_557 ? O2 W2 O2 Bi1 -122.7(2) 8_565 . . 5_557 ? O3 W2 O2 Bi1 154.9(4) 5_556 . . 5_557 ? Bi1 W2 O2 Bi1 -119.2(4) . . . 5_557 ? O2 Bi1 O2 W2 3.3(4) 8_565 . . . ? O2 Bi1 O2 W2 129.7(5) 5_556 . . . ? O2 Bi1 O2 W2 60.0(3) 4_556 . . . ? O2 Bi1 O2 W2 -55.3(3) 4_557 . . . ? O2 Bi1 O2 W2 -115.0(4) 5_557 . . . ? O2 Bi1 O2 Bi1 -126.3(2) 8_565 . . 5_556 ? O2 Bi1 O2 Bi1 0.0 5_556 . . 5_556 ? O2 Bi1 O2 Bi1 -69.7(5) 4_556 . . 5_556 ? O2 Bi1 O2 Bi1 175.0(3) 4_557 . . 5_556 ? O2 Bi1 O2 Bi1 115.4(5) 5_557 . . 5_556 ? W2 Bi1 O2 Bi1 -129.7(5) . . . 5_556 ? O2 Bi1 O2 Bi1 118.3(2) 8_565 . . 5_557 ? O2 Bi1 O2 Bi1 -115.4(5) 5_556 . . 5_557 ? O2 Bi1 O2 Bi1 175.0(3) 4_556 . . 5_557 ? O2 Bi1 O2 Bi1 59.7(4) 4_557 . . 5_557 ? O2 Bi1 O2 Bi1 0.0 5_557 . . 5_557 ? W2 Bi1 O2 Bi1 115.0(4) . . . 5_557 ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 2.592 _refine_diff_density_min -3.037 _refine_diff_density_rms 0.758 # Attachment '- EuBiW2O9.CIF' data_a3 _database_code_depnum_ccdc_archive 'CCDC 818405' #TrackingRef '- EuBiW2O9.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Bi Eu O9 W2' _chemical_formula_sum 'Bi Eu O9 W2' _chemical_formula_weight 872.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Bi Bi -4.1077 10.2566 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 32.295(3) _cell_length_b 5.6524(7) _cell_length_c 3.9845(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 727.35(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 762 _cell_measurement_theta_min 2.5226 _cell_measurement_theta_max 27.4449 _exptl_crystal_description strip _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 7.969 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1464 _exptl_absorpt_coefficient_mu 64.174 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.0346 _exptl_absorpt_correction_T_max 0.2491 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Mercury2 _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 13.6612 _diffrn_standards_number 1869 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4857 _diffrn_reflns_av_R_equivalents 0.0840 _diffrn_reflns_av_sigmaI/netI 0.0543 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 41 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 27.47 _reflns_number_total 897 _reflns_number_gt 830 _reflns_threshold_expression >2sigma(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^)+(0.0363P)^2^+0.7235P] 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 0.0052(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 897 _refine_ls_number_parameters 71 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0343 _refine_ls_R_factor_gt 0.0318 _refine_ls_wR_factor_ref 0.0740 _refine_ls_wR_factor_gt 0.0721 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _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 Eu1 Eu 0.16666(2) 0.2500 0.26358(16) 0.0092(2) Uani 1 2 d S . . Bi1 Bi -0.027596(17) 0.7500 0.29398(14) 0.0104(2) Uani 1 2 d S . . W1 W 0.293973(17) 0.2500 0.19983(14) 0.0055(2) Uani 1 2 d S . . W2 W 0.077955(17) 0.7500 0.20243(14) 0.0069(2) Uani 1 2 d S . . O1 O 0.2414(3) 0.2500 0.274(2) 0.016(2) Uani 1 2 d S . . O2 O 0.0731(4) 0.7500 0.757(2) 0.018(2) Uani 1 2 d S . . O3 O 0.2984(4) 0.2500 0.758(2) 0.024(3) Uani 1 2 d S . . O4 O 0.0281(2) 0.5237(15) 0.2643(16) 0.0161(18) Uani 1 1 d . . . O5 O 0.3212(3) 0.5254(13) 0.2706(16) 0.0153(17) Uani 1 1 d . . . O6 O 0.1114(3) 0.5047(13) 0.2671(18) 0.022(2) Uani 1 1 d . . . 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 Eu1 0.0043(4) 0.0155(4) 0.0077(4) 0.000 0.0000(2) 0.000 Bi1 0.0062(3) 0.0097(3) 0.0153(3) 0.000 -0.0017(2) 0.000 W1 0.0046(3) 0.0040(3) 0.0080(3) 0.000 0.00026(19) 0.000 W2 0.0039(3) 0.0086(3) 0.0083(3) 0.000 0.00015(19) 0.000 O1 0.004(5) 0.022(6) 0.023(6) 0.000 -0.007(4) 0.000 O2 0.017(6) 0.028(7) 0.010(5) 0.000 0.001(4) 0.000 O3 0.012(6) 0.054(9) 0.006(5) 0.000 -0.002(4) 0.000 O4 0.004(4) 0.023(5) 0.022(4) 0.006(3) 0.003(3) 0.001(3) O5 0.021(4) 0.009(4) 0.016(4) -0.002(3) -0.001(3) 0.001(3) O6 0.012(4) 0.026(5) 0.029(5) 0.006(3) -0.005(3) 0.009(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu1 O6 2.294(8) 8_565 ? Eu1 O6 2.294(8) . ? Eu1 O5 2.371(7) 7_655 ? Eu1 O5 2.371(7) 2_564 ? Eu1 O1 2.413(11) . ? Eu1 O5 2.418(7) 2_565 ? Eu1 O5 2.418(7) 7_656 ? Eu1 O3 3.043(4) 2_564 ? Eu1 O3 3.043(4) 2_554 ? Eu1 W1 3.5532(6) 2_565 ? Eu1 W1 3.5532(6) 2 ? Eu1 W1 3.8275(6) 2_554 ? Bi1 O4 2.211(8) 8_575 ? Bi1 O4 2.211(8) . ? Bi1 O4 2.343(7) 4_556 ? Bi1 O4 2.343(7) 5_566 ? Bi1 O4 2.710(7) 5_565 ? Bi1 O4 2.710(7) 4 ? Bi1 W2 3.4283(9) . ? W1 O1 1.725(11) . ? W1 O3 1.767(10) 1_554 ? W1 O5 1.811(8) . ? W1 O5 1.811(8) 8_565 ? W1 O3 2.228(10) . ? W1 Eu1 3.5532(6) 2_554 ? W1 Eu1 3.5532(6) 2_564 ? W1 Eu1 3.8275(6) 2_565 ? W1 Eu1 3.8275(6) 2 ? W2 O6 1.776(8) 8_575 ? W2 O6 1.776(8) . ? W2 O2 1.781(9) 1_554 ? W2 O4 2.070(8) . ? W2 O4 2.070(8) 8_575 ? W2 O2 2.216(9) . ? O2 W2 1.781(9) 1_556 ? O3 W1 1.767(10) 1_556 ? O3 Eu1 3.043(4) 2_565 ? O3 Eu1 3.043(4) 2 ? O4 Bi1 2.343(7) 5_566 ? O4 Bi1 2.710(7) 5_565 ? O5 Eu1 2.371(7) 2_565 ? O5 Eu1 2.418(7) 2_564 ? 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 O6 Eu1 O6 77.8(4) 8_565 . ? O6 Eu1 O5 78.3(3) 8_565 7_655 ? O6 Eu1 O5 118.0(3) . 7_655 ? O6 Eu1 O5 118.0(3) 8_565 2_564 ? O6 Eu1 O5 78.3(3) . 2_564 ? O5 Eu1 O5 64.7(3) 7_655 2_564 ? O6 Eu1 O1 141.1(2) 8_565 . ? O6 Eu1 O1 141.1(2) . . ? O5 Eu1 O1 81.3(3) 7_655 . ? O5 Eu1 O1 81.3(3) 2_564 . ? O6 Eu1 O5 116.8(3) 8_565 2_565 ? O6 Eu1 O5 77.9(3) . 2_565 ? O5 Eu1 O5 161.2(4) 7_655 2_565 ? O5 Eu1 O5 112.6(3) 2_564 2_565 ? O1 Eu1 O5 79.9(3) . 2_565 ? O6 Eu1 O5 77.9(3) 8_565 7_656 ? O6 Eu1 O5 116.8(3) . 7_656 ? O5 Eu1 O5 112.6(3) 7_655 7_656 ? O5 Eu1 O5 161.2(4) 2_564 7_656 ? O1 Eu1 O5 79.9(3) . 7_656 ? O5 Eu1 O5 63.3(3) 2_565 7_656 ? O6 Eu1 O3 150.6(3) 8_565 2_564 ? O6 Eu1 O3 72.9(3) . 2_564 ? O5 Eu1 O3 115.5(2) 7_655 2_564 ? O5 Eu1 O3 55.6(3) 2_564 2_564 ? O1 Eu1 O3 68.3(2) . 2_564 ? O5 Eu1 O3 57.2(3) 2_565 2_564 ? O5 Eu1 O3 115.7(3) 7_656 2_564 ? O6 Eu1 O3 72.9(3) 8_565 2_554 ? O6 Eu1 O3 150.6(3) . 2_554 ? O5 Eu1 O3 55.6(3) 7_655 2_554 ? O5 Eu1 O3 115.5(2) 2_564 2_554 ? O1 Eu1 O3 68.3(2) . 2_554 ? O5 Eu1 O3 115.7(2) 2_565 2_554 ? O5 Eu1 O3 57.2(3) 7_656 2_554 ? O3 Eu1 O3 136.5(4) 2_564 2_554 ? O6 Eu1 W1 140.78(19) 8_565 2_565 ? O6 Eu1 W1 77.1(2) . 2_565 ? O5 Eu1 W1 140.54(18) 7_655 2_565 ? O5 Eu1 W1 85.44(18) 2_564 2_565 ? O1 Eu1 W1 68.53(12) . 2_565 ? O5 Eu1 W1 27.85(18) 2_565 2_565 ? O5 Eu1 W1 87.19(17) 7_656 2_565 ? O3 Eu1 W1 29.81(18) 2_564 2_565 ? O3 Eu1 W1 127.6(2) 2_554 2_565 ? O6 Eu1 W1 77.1(2) 8_565 2 ? O6 Eu1 W1 140.78(19) . 2 ? O5 Eu1 W1 85.44(18) 7_655 2 ? O5 Eu1 W1 140.54(18) 2_564 2 ? O1 Eu1 W1 68.53(12) . 2 ? O5 Eu1 W1 87.19(16) 2_565 2 ? O5 Eu1 W1 27.85(18) 7_656 2 ? O3 Eu1 W1 127.6(2) 2_564 2 ? O3 Eu1 W1 29.81(18) 2_554 2 ? W1 Eu1 W1 105.39(2) 2_565 2 ? O6 Eu1 W1 78.4(2) 8_565 2_554 ? O6 Eu1 W1 136.52(19) . 2_554 ? O5 Eu1 W1 20.58(19) 7_655 2_554 ? O5 Eu1 W1 81.62(17) 2_564 2_554 ? O1 Eu1 W1 71.20(14) . 2_554 ? O5 Eu1 W1 145.52(18) 2_565 2_554 ? O5 Eu1 W1 92.81(17) 7_656 2_554 ? O3 Eu1 W1 123.93(19) 2_564 2_554 ? O3 Eu1 W1 35.58(18) 2_554 2_554 ? W1 Eu1 W1 139.08(2) 2_565 2_554 ? W1 Eu1 W1 65.224(10) 2 2_554 ? O4 Bi1 O4 70.7(4) 8_575 . ? O4 Bi1 O4 70.4(3) 8_575 4_556 ? O4 Bi1 O4 115.35(13) . 4_556 ? O4 Bi1 O4 115.35(13) 8_575 5_566 ? O4 Bi1 O4 70.4(3) . 5_566 ? O4 Bi1 O4 82.6(4) 4_556 5_566 ? O4 Bi1 O4 106.95(14) 8_575 5_565 ? O4 Bi1 O4 68.4(3) . 5_565 ? O4 Bi1 O4 173.45(18) 4_556 5_565 ? O4 Bi1 O4 103.9(3) 5_566 5_565 ? O4 Bi1 O4 68.4(3) 8_575 4 ? O4 Bi1 O4 106.95(14) . 4 ? O4 Bi1 O4 103.9(3) 4_556 4 ? O4 Bi1 O4 173.45(18) 5_566 4 ? O4 Bi1 O4 69.6(3) 5_565 4 ? O4 Bi1 W2 35.4(2) 8_575 . ? O4 Bi1 W2 35.4(2) . . ? O4 Bi1 W2 95.01(18) 4_556 . ? O4 Bi1 W2 95.01(18) 5_566 . ? O4 Bi1 W2 85.36(15) 5_565 . ? O4 Bi1 W2 85.36(15) 4 . ? O1 W1 O3 104.5(5) . 1_554 ? O1 W1 O5 116.9(3) . . ? O3 W1 O5 96.7(3) 1_554 . ? O1 W1 O5 116.9(3) . 8_565 ? O3 W1 O5 96.7(3) 1_554 8_565 ? O5 W1 O5 118.6(5) . 8_565 ? O1 W1 O3 83.9(4) . . ? O3 W1 O3 171.7(7) 1_554 . ? O5 W1 O3 79.2(3) . . ? O5 W1 O3 79.2(3) 8_565 . ? O1 W1 Eu1 115.85(15) . 2_554 ? O3 W1 Eu1 58.90(14) 1_554 2_554 ? O5 W1 Eu1 125.9(2) . 2_554 ? O5 W1 Eu1 38.6(2) 8_565 2_554 ? O3 W1 Eu1 117.72(13) . 2_554 ? O1 W1 Eu1 115.85(15) . 2_564 ? O3 W1 Eu1 58.90(14) 1_554 2_564 ? O5 W1 Eu1 38.6(2) . 2_564 ? O5 W1 Eu1 125.9(2) 8_565 2_564 ? O3 W1 Eu1 117.72(13) . 2_564 ? Eu1 W1 Eu1 105.39(2) 2_554 2_564 ? O1 W1 Eu1 103.1(2) . 2_565 ? O3 W1 Eu1 123.92(17) 1_554 2_565 ? O5 W1 Eu1 27.4(2) . 2_565 ? O5 W1 Eu1 112.5(2) 8_565 2_565 ? O3 W1 Eu1 52.63(11) . 2_565 ? Eu1 W1 Eu1 139.08(2) 2_554 2_565 ? Eu1 W1 Eu1 65.224(10) 2_564 2_565 ? O1 W1 Eu1 103.1(2) . 2 ? O3 W1 Eu1 123.92(17) 1_554 2 ? O5 W1 Eu1 112.5(2) . 2 ? O5 W1 Eu1 27.4(2) 8_565 2 ? O3 W1 Eu1 52.63(11) . 2 ? Eu1 W1 Eu1 65.224(10) 2_554 2 ? Eu1 W1 Eu1 139.08(2) 2_564 2 ? Eu1 W1 Eu1 95.19(2) 2_565 2 ? O6 W2 O6 102.7(6) 8_575 . ? O6 W2 O2 101.4(3) 8_575 1_554 ? O6 W2 O2 101.4(3) . 1_554 ? O6 W2 O4 159.6(3) 8_575 . ? O6 W2 O4 88.4(4) . . ? O2 W2 O4 92.9(3) 1_554 . ? O6 W2 O4 88.4(4) 8_575 8_575 ? O6 W2 O4 159.6(3) . 8_575 ? O2 W2 O4 92.9(3) 1_554 8_575 ? O4 W2 O4 76.3(4) . 8_575 ? O6 W2 O2 84.2(3) 8_575 . ? O6 W2 O2 84.2(3) . . ? O2 W2 O2 170.9(7) 1_554 . ? O4 W2 O2 80.0(3) . . ? O4 W2 O2 80.0(3) 8_575 . ? O6 W2 Bi1 126.1(3) 8_575 . ? O6 W2 Bi1 126.1(3) . . ? O2 W2 Bi1 91.1(4) 1_554 . ? O4 W2 Bi1 38.2(2) . . ? O4 W2 Bi1 38.2(2) 8_575 . ? O2 W2 Bi1 79.8(3) . . ? W1 O1 Eu1 169.2(5) . . ? W2 O2 W2 170.9(7) 1_556 . ? W1 O3 W1 171.7(7) 1_556 . ? W1 O3 Eu1 91.3(2) 1_556 2_565 ? W1 O3 Eu1 91.8(2) . 2_565 ? W1 O3 Eu1 91.3(2) 1_556 2 ? W1 O3 Eu1 91.8(2) . 2 ? Eu1 O3 Eu1 136.5(4) 2_565 2 ? W2 O4 Bi1 106.4(4) . . ? W2 O4 Bi1 120.2(3) . 5_566 ? Bi1 O4 Bi1 109.6(3) . 5_566 ? W2 O4 Bi1 105.1(3) . 5_565 ? Bi1 O4 Bi1 111.6(3) . 5_565 ? Bi1 O4 Bi1 103.9(3) 5_566 5_565 ? W1 O5 Eu1 132.0(4) . 2_565 ? W1 O5 Eu1 113.6(3) . 2_564 ? Eu1 O5 Eu1 112.6(3) 2_565 2_564 ? W2 O6 Eu1 164.2(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 Bi1 W2 O6 11.7(4) 8_575 . . 8_575 ? O4 Bi1 W2 O6 -161.7(4) . . . 8_575 ? O4 Bi1 W2 O6 -33.5(3) 4_556 . . 8_575 ? O4 Bi1 W2 O6 -116.5(4) 5_566 . . 8_575 ? O4 Bi1 W2 O6 139.9(3) 5_565 . . 8_575 ? O4 Bi1 W2 O6 70.0(3) 4 . . 8_575 ? O4 Bi1 W2 O6 161.7(4) 8_575 . . . ? O4 Bi1 W2 O6 -11.7(4) . . . . ? O4 Bi1 W2 O6 116.5(4) 4_556 . . . ? O4 Bi1 W2 O6 33.5(3) 5_566 . . . ? O4 Bi1 W2 O6 -70.0(3) 5_565 . . . ? O4 Bi1 W2 O6 -139.9(3) 4 . . . ? O4 Bi1 W2 O2 -93.3(3) 8_575 . . 1_554 ? O4 Bi1 W2 O2 93.3(3) . . . 1_554 ? O4 Bi1 W2 O2 -138.49(19) 4_556 . . 1_554 ? O4 Bi1 W2 O2 138.49(19) 5_566 . . 1_554 ? O4 Bi1 W2 O2 34.95(16) 5_565 . . 1_554 ? O4 Bi1 W2 O2 -34.95(16) 4 . . 1_554 ? O4 Bi1 W2 O4 173.4(6) 8_575 . . . ? O4 Bi1 W2 O4 128.2(2) 4_556 . . . ? O4 Bi1 W2 O4 45.2(4) 5_566 . . . ? O4 Bi1 W2 O4 -58.4(4) 5_565 . . . ? O4 Bi1 W2 O4 -128.3(3) 4 . . . ? O4 Bi1 W2 O4 -173.4(6) . . . 8_575 ? O4 Bi1 W2 O4 -45.2(4) 4_556 . . 8_575 ? O4 Bi1 W2 O4 -128.2(2) 5_566 . . 8_575 ? O4 Bi1 W2 O4 128.3(3) 5_565 . . 8_575 ? O4 Bi1 W2 O4 58.4(4) 4 . . 8_575 ? O4 Bi1 W2 O2 86.7(3) 8_575 . . . ? O4 Bi1 W2 O2 -86.7(3) . . . . ? O4 Bi1 W2 O2 41.51(19) 4_556 . . . ? O4 Bi1 W2 O2 -41.51(19) 5_566 . . . ? O4 Bi1 W2 O2 -145.05(16) 5_565 . . . ? O4 Bi1 W2 O2 145.05(16) 4 . . . ? O3 W1 O1 Eu1 0.000(2) 1_554 . . . ? O5 W1 O1 Eu1 105.4(3) . . . . ? O5 W1 O1 Eu1 -105.4(3) 8_565 . . . ? O3 W1 O1 Eu1 180.000(2) . . . . ? Eu1 W1 O1 Eu1 -62.11(14) 2_554 . . . ? Eu1 W1 O1 Eu1 62.11(14) 2_564 . . . ? Eu1 W1 O1 Eu1 130.69(6) 2_565 . . . ? Eu1 W1 O1 Eu1 -130.69(6) 2 . . . ? O6 Eu1 O1 W1 91.8(4) 8_565 . . . ? O6 Eu1 O1 W1 -91.8(4) . . . . ? O5 Eu1 O1 W1 32.79(17) 7_655 . . . ? O5 Eu1 O1 W1 -32.79(17) 2_564 . . . ? O5 Eu1 O1 W1 -147.77(17) 2_565 . . . ? O5 Eu1 O1 W1 147.77(17) 7_656 . . . ? O3 Eu1 O1 W1 -89.2(2) 2_564 . . . ? O3 Eu1 O1 W1 89.2(2) 2_554 . . . ? W1 Eu1 O1 W1 -121.28(8) 2_565 . . . ? W1 Eu1 O1 W1 121.28(8) 2 . . . ? W1 Eu1 O1 W1 51.26(6) 2_554 . . . ? O6 W2 O2 W2 -51.7(3) 8_575 . . 1_556 ? O6 W2 O2 W2 51.7(3) . . . 1_556 ? O2 W2 O2 W2 180.000(4) 1_554 . . 1_556 ? O4 W2 O2 W2 141.1(2) . . . 1_556 ? O4 W2 O2 W2 -141.1(2) 8_575 . . 1_556 ? Bi1 W2 O2 W2 180.000(2) . . . 1_556 ? O1 W1 O3 W1 0.000(1) . . . 1_556 ? O3 W1 O3 W1 180.000(3) 1_554 . . 1_556 ? O5 W1 O3 W1 118.9(3) . . . 1_556 ? O5 W1 O3 W1 -118.9(3) 8_565 . . 1_556 ? Eu1 W1 O3 W1 -116.03(14) 2_554 . . 1_556 ? Eu1 W1 O3 W1 116.03(14) 2_564 . . 1_556 ? Eu1 W1 O3 W1 111.7(2) 2_565 . . 1_556 ? Eu1 W1 O3 W1 -111.7(2) 2 . . 1_556 ? O1 W1 O3 Eu1 -111.7(2) . . . 2_565 ? O3 W1 O3 Eu1 68.3(2) 1_554 . . 2_565 ? O5 W1 O3 Eu1 7.2(3) . . . 2_565 ? O5 W1 O3 Eu1 129.4(4) 8_565 . . 2_565 ? Eu1 W1 O3 Eu1 132.27(8) 2_554 . . 2_565 ? Eu1 W1 O3 Eu1 4.3(3) 2_564 . . 2_565 ? Eu1 W1 O3 Eu1 136.6(4) 2 . . 2_565 ? O1 W1 O3 Eu1 111.7(2) . . . 2 ? O3 W1 O3 Eu1 -68.3(2) 1_554 . . 2 ? O5 W1 O3 Eu1 -129.4(4) . . . 2 ? O5 W1 O3 Eu1 -7.2(3) 8_565 . . 2 ? Eu1 W1 O3 Eu1 -4.3(3) 2_554 . . 2 ? Eu1 W1 O3 Eu1 -132.27(8) 2_564 . . 2 ? Eu1 W1 O3 Eu1 -136.6(4) 2_565 . . 2 ? O6 W2 O4 Bi1 46.8(10) 8_575 . . . ? O6 W2 O4 Bi1 170.6(3) . . . . ? O2 W2 O4 Bi1 -88.1(3) 1_554 . . . ? O4 W2 O4 Bi1 4.2(4) 8_575 . . . ? O2 W2 O4 Bi1 86.2(3) . . . . ? O6 W2 O4 Bi1 -78.4(10) 8_575 . . 5_566 ? O6 W2 O4 Bi1 45.4(4) . . . 5_566 ? O2 W2 O4 Bi1 146.8(4) 1_554 . . 5_566 ? O4 W2 O4 Bi1 -120.9(3) 8_575 . . 5_566 ? O2 W2 O4 Bi1 -38.9(4) . . . 5_566 ? Bi1 W2 O4 Bi1 -125.1(5) . . . 5_566 ? O6 W2 O4 Bi1 165.3(8) 8_575 . . 5_565 ? O6 W2 O4 Bi1 -70.9(3) . . . 5_565 ? O2 W2 O4 Bi1 30.5(3) 1_554 . . 5_565 ? O4 W2 O4 Bi1 122.7(2) 8_575 . . 5_565 ? O2 W2 O4 Bi1 -155.3(3) . . . 5_565 ? Bi1 W2 O4 Bi1 118.5(4) . . . 5_565 ? O4 Bi1 O4 W2 -4.1(3) 8_575 . . . ? O4 Bi1 O4 W2 -60.0(3) 4_556 . . . ? O4 Bi1 O4 W2 -131.4(5) 5_566 . . . ? O4 Bi1 O4 W2 114.1(4) 5_565 . . . ? O4 Bi1 O4 W2 54.9(3) 4 . . . ? O4 Bi1 O4 Bi1 127.3(2) 8_575 . . 5_566 ? O4 Bi1 O4 Bi1 71.4(5) 4_556 . . 5_566 ? O4 Bi1 O4 Bi1 0.0 5_566 . . 5_566 ? O4 Bi1 O4 Bi1 -114.5(5) 5_565 . . 5_566 ? O4 Bi1 O4 Bi1 -173.7(3) 4 . . 5_566 ? W2 Bi1 O4 Bi1 131.4(5) . . . 5_566 ? O4 Bi1 O4 Bi1 -118.1(2) 8_575 . . 5_565 ? O4 Bi1 O4 Bi1 -174.1(2) 4_556 . . 5_565 ? O4 Bi1 O4 Bi1 114.5(5) 5_566 . . 5_565 ? O4 Bi1 O4 Bi1 0.0 5_565 . . 5_565 ? O4 Bi1 O4 Bi1 -59.2(4) 4 . . 5_565 ? W2 Bi1 O4 Bi1 -114.1(4) . . . 5_565 ? O1 W1 O5 Eu1 64.8(6) . . . 2_565 ? O3 W1 O5 Eu1 174.8(5) 1_554 . . 2_565 ? O5 W1 O5 Eu1 -83.9(6) 8_565 . . 2_565 ? O3 W1 O5 Eu1 -12.6(5) . . . 2_565 ? Eu1 W1 O5 Eu1 -129.1(4) 2_554 . . 2_565 ? Eu1 W1 O5 Eu1 163.3(8) 2_564 . . 2_565 ? Eu1 W1 O5 Eu1 -54.2(5) 2 . . 2_565 ? O1 W1 O5 Eu1 -98.5(5) . . . 2_564 ? O3 W1 O5 Eu1 11.5(5) 1_554 . . 2_564 ? O5 W1 O5 Eu1 112.8(4) 8_565 . . 2_564 ? O3 W1 O5 Eu1 -175.9(4) . . . 2_564 ? Eu1 W1 O5 Eu1 67.6(4) 2_554 . . 2_564 ? Eu1 W1 O5 Eu1 -163.3(8) 2_565 . . 2_564 ? Eu1 W1 O5 Eu1 142.5(2) 2 . . 2_564 ? O6 W2 O6 Eu1 -43.4(18) 8_575 . . . ? O2 W2 O6 Eu1 61.3(16) 1_554 . . . ? O4 W2 O6 Eu1 153.9(16) . . . . ? O4 W2 O6 Eu1 -165.0(11) 8_575 . . . ? O2 W2 O6 Eu1 -126.0(16) . . . . ? Bi1 W2 O6 Eu1 161.1(14) . . . . ? O6 Eu1 O6 W2 -146.6(15) 8_565 . . . ? O5 Eu1 O6 W2 -77.1(16) 7_655 . . . ? O5 Eu1 O6 W2 -24.2(16) 2_564 . . . ? O1 Eu1 O6 W2 35.7(18) . . . . ? O5 Eu1 O6 W2 92.3(16) 2_565 . . . ? O5 Eu1 O6 W2 143.9(15) 7_656 . . . ? O3 Eu1 O6 W2 33.2(16) 2_564 . . . ? O3 Eu1 O6 W2 -146.0(14) 2_554 . . . ? W1 Eu1 O6 W2 63.8(16) 2_565 . . . ? W1 Eu1 O6 W2 162.3(14) 2 . . . ? W1 Eu1 O6 W2 -88.4(16) 2_554 . . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 2.704 _refine_diff_density_min -2.751 _refine_diff_density_rms 0.560 # Attachment '- SmBiW2O9.CIF' data_a4 _database_code_depnum_ccdc_archive 'CCDC 818406' #TrackingRef '- SmBiW2O9.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Bi O9 Sm W2' _chemical_formula_sum 'Bi O9 Sm W2' _chemical_formula_weight 871.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Bi Bi -4.1077 10.2566 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 32.38(2) _cell_length_b 5.664(4) _cell_length_c 3.996(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 732.9(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 787 _cell_measurement_theta_min 3.8121 _cell_measurement_theta_max 27.4487 _exptl_crystal_description strip _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 7.894 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1460 _exptl_absorpt_coefficient_mu 63.145 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.0492 _exptl_absorpt_correction_T_max 0.1444 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Mercury2 _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 13.6612 _diffrn_standards_number 1062 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 5127 _diffrn_reflns_av_R_equivalents 0.0973 _diffrn_reflns_av_sigmaI/netI 0.0571 _diffrn_reflns_limit_h_min -42 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 4 _diffrn_reflns_theta_min 3.78 _diffrn_reflns_theta_max 27.45 _reflns_number_total 905 _reflns_number_gt 844 _reflns_threshold_expression >2sigma(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^)+(0.0672P)^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 0.00181(16) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 905 _refine_ls_number_parameters 71 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0450 _refine_ls_R_factor_gt 0.0424 _refine_ls_wR_factor_ref 0.1032 _refine_ls_wR_factor_gt 0.1013 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _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 0.16654(3) 0.7500 1.2360(2) 0.0088(3) Uani 1 2 d S . . Bi1 Bi -0.02755(2) 0.2500 1.20442(17) 0.0105(3) Uani 1 2 d S . . W1 W 0.20602(2) 1.2500 0.80007(16) 0.0056(3) Uani 1 2 d S . . W2 W 0.07769(2) 0.2500 1.29818(17) 0.0071(3) Uani 1 2 d S . . O1 O 0.0280(3) 0.4797(16) 1.2371(19) 0.018(2) Uani 1 1 d . . . O2 O 0.1110(4) 0.4961(14) 1.240(2) 0.027(3) Uani 1 1 d . . . O3 O 0.1787(4) 0.9760(15) 0.733(2) 0.018(2) Uani 1 1 d . . . O4 O 0.0719(5) 0.2500 0.738(3) 0.018(3) Uani 1 2 d S . . O5 O 0.2410(5) 0.7500 1.225(3) 0.016(3) Uani 1 2 d S . . O6 O 0.2019(5) 0.2500 1.240(3) 0.023(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 Sm1 0.0073(5) 0.0118(5) 0.0074(4) 0.000 -0.0004(3) 0.000 Bi1 0.0088(4) 0.0078(4) 0.0149(4) 0.000 0.0015(2) 0.000 W1 0.0072(4) 0.0017(3) 0.0079(4) 0.000 0.0003(2) 0.000 W2 0.0068(4) 0.0060(4) 0.0085(4) 0.000 -0.0003(2) 0.000 O1 0.024(7) 0.013(4) 0.017(5) 0.001(3) 0.008(3) -0.006(4) O2 0.023(7) 0.013(5) 0.045(7) -0.008(4) 0.004(4) -0.007(4) O3 0.025(6) 0.009(4) 0.019(5) -0.001(3) -0.005(4) 0.003(4) O4 0.023(8) 0.020(6) 0.010(6) 0.000 0.012(5) 0.000 O5 0.021(8) 0.015(6) 0.011(6) 0.000 -0.003(5) 0.000 O6 0.012(8) 0.044(9) 0.013(6) 0.000 0.005(5) 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 Sm1 O2 2.303(11) 8_575 ? Sm1 O2 2.303(11) . ? Sm1 O3 2.395(8) 1_556 ? Sm1 O3 2.395(8) 8_576 ? Sm1 O5 2.412(16) . ? Sm1 O3 2.416(9) 8_575 ? Sm1 O3 2.416(9) . ? Sm1 W1 3.5622(19) 1_545 ? Sm1 W1 3.5622(19) . ? Sm1 Sm1 3.996(3) 1_554 ? Sm1 Sm1 3.996(3) 1_556 ? Bi1 O1 2.224(10) . ? Bi1 O1 2.224(10) 8_565 ? Bi1 O1 2.336(8) 4_547 ? Bi1 O1 2.336(8) 5_567 ? Bi1 O1 2.706(8) 5_568 ? Bi1 O1 2.706(8) 4_548 ? Bi1 W2 3.428(2) . ? W1 O5 1.741(16) 2_574 ? W1 O6 1.763(12) 1_565 ? W1 O3 1.806(10) . ? W1 O3 1.806(10) 8_585 ? W1 O6 2.242(12) 1_564 ? W1 Sm1 3.5622(19) 1_565 ? W2 O4 1.767(11) 1_556 ? W2 O2 1.778(10) . ? W2 O2 1.778(10) 8_565 ? W2 O1 2.083(11) 8_565 ? W2 O1 2.083(11) . ? W2 O4 2.247(12) . ? O1 Bi1 2.336(8) 5_567 ? O1 Bi1 2.706(8) 5_568 ? O3 Sm1 2.395(8) 1_554 ? O4 W2 1.767(11) 1_554 ? O5 W1 1.741(16) 2_575 ? O6 W1 1.763(12) 1_545 ? O6 W1 2.242(12) 1_546 ? 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 O2 Sm1 O2 77.3(5) 8_575 . ? O2 Sm1 O3 77.9(4) 8_575 1_556 ? O2 Sm1 O3 117.2(4) . 1_556 ? O2 Sm1 O3 117.2(4) 8_575 8_576 ? O2 Sm1 O3 77.9(4) . 8_576 ? O3 Sm1 O3 64.6(4) 1_556 8_576 ? O2 Sm1 O5 141.3(3) 8_575 . ? O2 Sm1 O5 141.3(3) . . ? O3 Sm1 O5 81.4(4) 1_556 . ? O3 Sm1 O5 81.4(4) 8_576 . ? O2 Sm1 O3 117.6(4) 8_575 8_575 ? O2 Sm1 O3 78.6(4) . 8_575 ? O3 Sm1 O3 161.1(6) 1_556 8_575 ? O3 Sm1 O3 112.3(4) 8_576 8_575 ? O5 Sm1 O3 79.7(4) . 8_575 ? O2 Sm1 O3 78.6(4) 8_575 . ? O2 Sm1 O3 117.6(4) . . ? O3 Sm1 O3 112.3(4) 1_556 . ? O3 Sm1 O3 161.1(6) 8_576 . ? O5 Sm1 O3 79.7(4) . . ? O3 Sm1 O3 64.0(4) 8_575 . ? O2 Sm1 W1 141.2(3) 8_575 1_545 ? O2 Sm1 W1 77.7(3) . 1_545 ? O3 Sm1 W1 140.5(2) 1_556 1_545 ? O3 Sm1 W1 85.5(2) 8_576 1_545 ? O5 Sm1 W1 68.44(14) . 1_545 ? O3 Sm1 W1 27.5(2) 8_575 1_545 ? O3 Sm1 W1 87.5(2) . 1_545 ? O2 Sm1 W1 77.7(3) 8_575 . ? O2 Sm1 W1 141.2(3) . . ? O3 Sm1 W1 85.5(2) 1_556 . ? O3 Sm1 W1 140.5(2) 8_576 . ? O5 Sm1 W1 68.44(14) . . ? O3 Sm1 W1 87.5(2) 8_575 . ? O3 Sm1 W1 27.5(2) . . ? W1 Sm1 W1 105.31(6) 1_545 . ? O2 Sm1 Sm1 90.4(2) 8_575 1_554 ? O2 Sm1 Sm1 90.4(3) . 1_554 ? O3 Sm1 Sm1 146.0(2) 1_556 1_554 ? O3 Sm1 Sm1 146.0(2) 8_576 1_554 ? O5 Sm1 Sm1 89.0(3) . 1_554 ? O3 Sm1 Sm1 33.7(2) 8_575 1_554 ? O3 Sm1 Sm1 33.7(2) . 1_554 ? W1 Sm1 Sm1 60.72(3) 1_545 1_554 ? W1 Sm1 Sm1 60.72(3) . 1_554 ? O2 Sm1 Sm1 89.6(2) 8_575 1_556 ? O2 Sm1 Sm1 89.6(3) . 1_556 ? O3 Sm1 Sm1 34.0(2) 1_556 1_556 ? O3 Sm1 Sm1 34.0(2) 8_576 1_556 ? O5 Sm1 Sm1 91.0(3) . 1_556 ? O3 Sm1 Sm1 146.3(2) 8_575 1_556 ? O3 Sm1 Sm1 146.3(2) . 1_556 ? W1 Sm1 Sm1 119.28(3) 1_545 1_556 ? W1 Sm1 Sm1 119.28(3) . 1_556 ? Sm1 Sm1 Sm1 180.0 1_554 1_556 ? O1 Bi1 O1 71.6(5) . 8_565 ? O1 Bi1 O1 115.65(18) . 4_547 ? O1 Bi1 O1 70.5(4) 8_565 4_547 ? O1 Bi1 O1 70.5(4) . 5_567 ? O1 Bi1 O1 115.65(18) 8_565 5_567 ? O1 Bi1 O1 81.9(4) 4_547 5_567 ? O1 Bi1 O1 68.0(4) . 5_568 ? O1 Bi1 O1 106.67(17) 8_565 5_568 ? O1 Bi1 O1 173.5(2) 4_547 5_568 ? O1 Bi1 O1 104.6(3) 5_567 5_568 ? O1 Bi1 O1 106.67(17) . 4_548 ? O1 Bi1 O1 68.0(4) 8_565 4_548 ? O1 Bi1 O1 104.6(3) 4_547 4_548 ? O1 Bi1 O1 173.5(2) 5_567 4_548 ? O1 Bi1 O1 68.9(4) 5_568 4_548 ? O1 Bi1 W2 35.9(3) . . ? O1 Bi1 W2 35.9(3) 8_565 . ? O1 Bi1 W2 95.1(3) 4_547 . ? O1 Bi1 W2 95.1(3) 5_567 . ? O1 Bi1 W2 85.1(2) 5_568 . ? O1 Bi1 W2 85.1(2) 4_548 . ? O5 W1 O6 104.2(6) 2_574 1_565 ? O5 W1 O3 117.2(4) 2_574 . ? O6 W1 O3 96.4(4) 1_565 . ? O5 W1 O3 117.2(4) 2_574 8_585 ? O6 W1 O3 96.4(4) 1_565 8_585 ? O3 W1 O3 118.5(7) . 8_585 ? O5 W1 O6 83.5(6) 2_574 1_564 ? O6 W1 O6 172.3(9) 1_565 1_564 ? O3 W1 O6 79.8(3) . 1_564 ? O3 W1 O6 79.8(3) 8_585 1_564 ? O5 W1 Sm1 115.95(18) 2_574 1_565 ? O6 W1 Sm1 59.0(2) 1_565 1_565 ? O3 W1 Sm1 125.5(3) . 1_565 ? O3 W1 Sm1 38.2(3) 8_585 1_565 ? O6 W1 Sm1 117.84(18) 1_564 1_565 ? O5 W1 Sm1 115.95(18) 2_574 . ? O6 W1 Sm1 59.0(2) 1_565 . ? O3 W1 Sm1 38.2(3) . . ? O3 W1 Sm1 125.5(3) 8_585 . ? O6 W1 Sm1 117.84(18) 1_564 . ? Sm1 W1 Sm1 105.31(6) 1_565 . ? O4 W2 O2 101.3(4) 1_556 . ? O4 W2 O2 101.3(4) 1_556 8_565 ? O2 W2 O2 103.3(8) . 8_565 ? O4 W2 O1 92.0(5) 1_556 8_565 ? O2 W2 O1 160.5(4) . 8_565 ? O2 W2 O1 87.9(5) 8_565 8_565 ? O4 W2 O1 92.0(5) 1_556 . ? O2 W2 O1 87.9(5) . . ? O2 W2 O1 160.5(4) 8_565 . ? O1 W2 O1 77.3(5) 8_565 . ? O4 W2 O4 169.1(9) 1_556 . ? O2 W2 O4 85.4(4) . . ? O2 W2 O4 85.4(4) 8_565 . ? O1 W2 O4 79.5(4) 8_565 . ? O1 W2 O4 79.5(4) . . ? O4 W2 Bi1 90.2(5) 1_556 . ? O2 W2 Bi1 126.1(4) . . ? O2 W2 Bi1 126.1(4) 8_565 . ? O1 W2 Bi1 38.7(3) 8_565 . ? O1 W2 Bi1 38.7(3) . . ? O4 W2 Bi1 78.9(4) . . ? W2 O1 Bi1 105.4(4) . . ? W2 O1 Bi1 120.2(4) . 5_567 ? Bi1 O1 Bi1 109.5(4) . 5_567 ? W2 O1 Bi1 105.1(4) . 5_568 ? Bi1 O1 Bi1 112.0(4) . 5_568 ? Bi1 O1 Bi1 104.6(3) 5_567 5_568 ? W2 O2 Sm1 164.6(7) . . ? W1 O3 Sm1 131.5(5) . 1_554 ? W1 O3 Sm1 114.3(4) . . ? Sm1 O3 Sm1 112.3(4) 1_554 . ? W2 O4 W2 169.1(9) 1_554 . ? W1 O5 Sm1 169.1(7) 2_575 . ? W1 O6 W1 172.3(9) 1_545 1_546 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Sm1 W1 O5 169.5(5) 8_575 . . 2_574 ? O2 Sm1 W1 O5 -139.7(5) . . . 2_574 ? O3 Sm1 W1 O5 90.9(5) 1_556 . . 2_574 ? O3 Sm1 W1 O5 51.4(5) 8_576 . . 2_574 ? O5 Sm1 W1 O5 8.43(16) . . . 2_574 ? O3 Sm1 W1 O5 -71.5(5) 8_575 . . 2_574 ? O3 Sm1 W1 O5 -101.7(7) . . . 2_574 ? W1 Sm1 W1 O5 -50.4(4) 1_545 . . 2_574 ? Sm1 Sm1 W1 O5 -93.1(4) 1_554 . . 2_574 ? Sm1 Sm1 W1 O5 86.9(4) 1_556 . . 2_574 ? O2 Sm1 W1 O6 78.0(6) 8_575 . . 1_565 ? O2 Sm1 W1 O6 128.8(7) . . . 1_565 ? O3 Sm1 W1 O6 -0.6(6) 1_556 . . 1_565 ? O3 Sm1 W1 O6 -40.1(7) 8_576 . . 1_565 ? O5 Sm1 W1 O6 -83.1(6) . . . 1_565 ? O3 Sm1 W1 O6 -163.0(6) 8_575 . . 1_565 ? O3 Sm1 W1 O6 166.8(8) . . . 1_565 ? W1 Sm1 W1 O6 -141.9(6) 1_545 . . 1_565 ? Sm1 Sm1 W1 O6 175.4(6) 1_554 . . 1_565 ? Sm1 Sm1 W1 O6 -4.6(6) 1_556 . . 1_565 ? O2 Sm1 W1 O3 -88.9(6) 8_575 . . . ? O2 Sm1 W1 O3 -38.0(7) . . . . ? O3 Sm1 W1 O3 -167.4(8) 1_556 . . . ? O3 Sm1 W1 O3 153.0(9) 8_576 . . . ? O5 Sm1 W1 O3 110.1(6) . . . . ? O3 Sm1 W1 O3 30.1(4) 8_575 . . . ? W1 Sm1 W1 O3 51.3(6) 1_545 . . . ? Sm1 Sm1 W1 O3 8.6(6) 1_554 . . . ? Sm1 Sm1 W1 O3 -171.4(6) 1_556 . . . ? O2 Sm1 W1 O3 3.5(4) 8_575 . . 8_585 ? O2 Sm1 W1 O3 54.4(5) . . . 8_585 ? O3 Sm1 W1 O3 -75.0(3) 1_556 . . 8_585 ? O3 Sm1 W1 O3 -114.6(5) 8_576 . . 8_585 ? O5 Sm1 W1 O3 -157.5(4) . . . 8_585 ? O3 Sm1 W1 O3 122.5(5) 8_575 . . 8_585 ? O3 Sm1 W1 O3 92.4(8) . . . 8_585 ? W1 Sm1 W1 O3 143.7(3) 1_545 . . 8_585 ? Sm1 Sm1 W1 O3 101.0(3) 1_554 . . 8_585 ? Sm1 Sm1 W1 O3 -79.0(3) 1_556 . . 8_585 ? O2 Sm1 W1 O6 -93.9(5) 8_575 . . 1_564 ? O2 Sm1 W1 O6 -43.1(6) . . . 1_564 ? O3 Sm1 W1 O6 -172.5(5) 1_556 . . 1_564 ? O3 Sm1 W1 O6 148.0(6) 8_576 . . 1_564 ? O5 Sm1 W1 O6 105.0(5) . . . 1_564 ? O3 Sm1 W1 O6 25.0(5) 8_575 . . 1_564 ? O3 Sm1 W1 O6 -5.1(7) . . . 1_564 ? W1 Sm1 W1 O6 46.2(4) 1_545 . . 1_564 ? Sm1 Sm1 W1 O6 3.5(4) 1_554 . . 1_564 ? Sm1 Sm1 W1 O6 -176.5(4) 1_556 . . 1_564 ? O2 Sm1 W1 Sm1 39.8(3) 8_575 . . 1_565 ? O2 Sm1 W1 Sm1 90.7(4) . . . 1_565 ? O3 Sm1 W1 Sm1 -38.7(3) 1_556 . . 1_565 ? O3 Sm1 W1 Sm1 -78.3(4) 8_576 . . 1_565 ? O5 Sm1 W1 Sm1 -121.2(3) . . . 1_565 ? O3 Sm1 W1 Sm1 158.8(3) 8_575 . . 1_565 ? O3 Sm1 W1 Sm1 128.7(6) . . . 1_565 ? W1 Sm1 W1 Sm1 180.0 1_545 . . 1_565 ? Sm1 Sm1 W1 Sm1 137.30(4) 1_554 . . 1_565 ? Sm1 Sm1 W1 Sm1 -42.70(4) 1_556 . . 1_565 ? O1 Bi1 W2 O4 92.9(3) . . . 1_556 ? O1 Bi1 W2 O4 -92.9(3) 8_565 . . 1_556 ? O1 Bi1 W2 O4 -138.9(2) 4_547 . . 1_556 ? O1 Bi1 W2 O4 138.9(2) 5_567 . . 1_556 ? O1 Bi1 W2 O4 34.59(18) 5_568 . . 1_556 ? O1 Bi1 W2 O4 -34.59(18) 4_548 . . 1_556 ? O1 Bi1 W2 O2 -11.2(5) . . . . ? O1 Bi1 W2 O2 162.9(5) 8_565 . . . ? O1 Bi1 W2 O2 117.0(5) 4_547 . . . ? O1 Bi1 W2 O2 34.7(4) 5_567 . . . ? O1 Bi1 W2 O2 -69.5(4) 5_568 . . . ? O1 Bi1 W2 O2 -138.7(4) 4_548 . . . ? O1 Bi1 W2 O2 -162.9(5) . . . 8_565 ? O1 Bi1 W2 O2 11.2(5) 8_565 . . 8_565 ? O1 Bi1 W2 O2 -34.7(4) 4_547 . . 8_565 ? O1 Bi1 W2 O2 -117.0(5) 5_567 . . 8_565 ? O1 Bi1 W2 O2 138.7(4) 5_568 . . 8_565 ? O1 Bi1 W2 O2 69.5(4) 4_548 . . 8_565 ? O1 Bi1 W2 O1 -174.1(7) . . . 8_565 ? O1 Bi1 W2 O1 -45.9(5) 4_547 . . 8_565 ? O1 Bi1 W2 O1 -128.2(3) 5_567 . . 8_565 ? O1 Bi1 W2 O1 127.5(3) 5_568 . . 8_565 ? O1 Bi1 W2 O1 58.3(4) 4_548 . . 8_565 ? O1 Bi1 W2 O1 174.1(7) 8_565 . . . ? O1 Bi1 W2 O1 128.2(3) 4_547 . . . ? O1 Bi1 W2 O1 45.9(5) 5_567 . . . ? O1 Bi1 W2 O1 -58.3(4) 5_568 . . . ? O1 Bi1 W2 O1 -127.5(3) 4_548 . . . ? O1 Bi1 W2 O4 -87.1(3) . . . . ? O1 Bi1 W2 O4 87.1(3) 8_565 . . . ? O1 Bi1 W2 O4 41.1(2) 4_547 . . . ? O1 Bi1 W2 O4 -41.1(2) 5_567 . . . ? O1 Bi1 W2 O4 -145.41(18) 5_568 . . . ? O1 Bi1 W2 O4 145.41(18) 4_548 . . . ? O4 W2 O1 Bi1 -87.8(4) 1_556 . . . ? O2 W2 O1 Bi1 171.0(4) . . . . ? O2 W2 O1 Bi1 45.3(12) 8_565 . . . ? O1 W2 O1 Bi1 3.8(4) 8_565 . . . ? O4 W2 O1 Bi1 85.3(4) . . . . ? O4 W2 O1 Bi1 148.1(5) 1_556 . . 5_567 ? O2 W2 O1 Bi1 46.8(5) . . . 5_567 ? O2 W2 O1 Bi1 -78.9(13) 8_565 . . 5_567 ? O1 W2 O1 Bi1 -120.4(4) 8_565 . . 5_567 ? O4 W2 O1 Bi1 -38.9(4) . . . 5_567 ? Bi1 W2 O1 Bi1 -124.1(6) . . . 5_567 ? O4 W2 O1 Bi1 30.7(4) 1_556 . . 5_568 ? O2 W2 O1 Bi1 -70.5(4) . . . 5_568 ? O2 W2 O1 Bi1 163.8(10) 8_565 . . 5_568 ? O1 W2 O1 Bi1 122.3(2) 8_565 . . 5_568 ? O4 W2 O1 Bi1 -156.2(4) . . . 5_568 ? Bi1 W2 O1 Bi1 118.5(4) . . . 5_568 ? O1 Bi1 O1 W2 -3.6(4) 8_565 . . . ? O1 Bi1 O1 W2 -60.3(3) 4_547 . . . ? O1 Bi1 O1 W2 -130.6(5) 5_567 . . . ? O1 Bi1 O1 W2 113.8(5) 5_568 . . . ? O1 Bi1 O1 W2 55.6(3) 4_548 . . . ? O1 Bi1 O1 Bi1 127.0(3) 8_565 . . 5_567 ? O1 Bi1 O1 Bi1 70.4(5) 4_547 . . 5_567 ? O1 Bi1 O1 Bi1 0.0 5_567 . . 5_567 ? O1 Bi1 O1 Bi1 -115.6(6) 5_568 . . 5_567 ? O1 Bi1 O1 Bi1 -173.8(3) 4_548 . . 5_567 ? W2 Bi1 O1 Bi1 130.6(5) . . . 5_567 ? O1 Bi1 O1 Bi1 -117.4(3) 8_565 . . 5_568 ? O1 Bi1 O1 Bi1 -174.1(3) 4_547 . . 5_568 ? O1 Bi1 O1 Bi1 115.6(6) 5_567 . . 5_568 ? O1 Bi1 O1 Bi1 0.0 5_568 . . 5_568 ? O1 Bi1 O1 Bi1 -58.2(5) 4_548 . . 5_568 ? W2 Bi1 O1 Bi1 -113.8(5) . . . 5_568 ? O4 W2 O2 Sm1 68(2) 1_556 . . . ? O2 W2 O2 Sm1 -37(2) 8_565 . . . ? O1 W2 O2 Sm1 -160.6(15) 8_565 . . . ? O1 W2 O2 Sm1 159(2) . . . . ? O4 W2 O2 Sm1 -121(2) . . . . ? Bi1 W2 O2 Sm1 166.1(18) . . . . ? O2 Sm1 O2 W2 -151.4(19) 8_575 . . . ? O3 Sm1 O2 W2 -82(2) 1_556 . . . ? O3 Sm1 O2 W2 -30(2) 8_576 . . . ? O5 Sm1 O2 W2 30(2) . . . . ? O3 Sm1 O2 W2 87(2) 8_575 . . . ? O3 Sm1 O2 W2 139(2) . . . . ? W1 Sm1 O2 W2 58(2) 1_545 . . . ? W1 Sm1 O2 W2 157.7(18) . . . . ? Sm1 Sm1 O2 W2 118(2) 1_554 . . . ? Sm1 Sm1 O2 W2 -62(2) 1_556 . . . ? O5 W1 O3 Sm1 -64.9(8) 2_574 . . 1_554 ? O6 W1 O3 Sm1 -174.5(7) 1_565 . . 1_554 ? O3 W1 O3 Sm1 84.7(9) 8_585 . . 1_554 ? O6 W1 O3 Sm1 12.3(7) 1_564 . . 1_554 ? Sm1 W1 O3 Sm1 129.3(5) 1_565 . . 1_554 ? Sm1 W1 O3 Sm1 -163.1(11) . . . 1_554 ? O5 W1 O3 Sm1 98.2(6) 2_574 . . . ? O6 W1 O3 Sm1 -11.3(7) 1_565 . . . ? O3 W1 O3 Sm1 -112.2(4) 8_585 . . . ? O6 W1 O3 Sm1 175.4(6) 1_564 . . . ? Sm1 W1 O3 Sm1 -67.6(5) 1_565 . . . ? O2 Sm1 O3 W1 85.2(5) 8_575 . . . ? O2 Sm1 O3 W1 154.2(5) . . . . ? O3 Sm1 O3 W1 13.6(9) 1_556 . . . ? O3 Sm1 O3 W1 -63.0(8) 8_576 . . . ? O5 Sm1 O3 W1 -62.6(5) . . . . ? O3 Sm1 O3 W1 -146.1(3) 8_575 . . . ? W1 Sm1 O3 W1 -131.1(5) 1_545 . . . ? Sm1 Sm1 O3 W1 -166.4(9) 1_554 . . . ? Sm1 Sm1 O3 W1 13.6(9) 1_556 . . . ? O2 Sm1 O3 Sm1 -108.3(6) 8_575 . . 1_554 ? O2 Sm1 O3 Sm1 -39.4(5) . . . 1_554 ? O3 Sm1 O3 Sm1 180.0 1_556 . . 1_554 ? O3 Sm1 O3 Sm1 103.4(7) 8_576 . . 1_554 ? O5 Sm1 O3 Sm1 103.8(4) . . . 1_554 ? O3 Sm1 O3 Sm1 20.3(6) 8_575 . . 1_554 ? W1 Sm1 O3 Sm1 35.3(4) 1_545 . . 1_554 ? W1 Sm1 O3 Sm1 166.4(9) . . . 1_554 ? Sm1 Sm1 O3 Sm1 180.000(1) 1_556 . . 1_554 ? O4 W2 O4 W2 180.000(3) 1_556 . . 1_554 ? O2 W2 O4 W2 51.9(4) . . . 1_554 ? O2 W2 O4 W2 -51.9(4) 8_565 . . 1_554 ? O1 W2 O4 W2 -140.6(3) 8_565 . . 1_554 ? O1 W2 O4 W2 140.6(3) . . . 1_554 ? Bi1 W2 O4 W2 180.000(7) . . . 1_554 ? O2 Sm1 O5 W1 90.7(5) 8_575 . . 2_575 ? O2 Sm1 O5 W1 -90.7(5) . . . 2_575 ? O3 Sm1 O5 W1 32.7(2) 1_556 . . 2_575 ? O3 Sm1 O5 W1 -32.7(2) 8_576 . . 2_575 ? O3 Sm1 O5 W1 -147.4(2) 8_575 . . 2_575 ? O3 Sm1 O5 W1 147.4(2) . . . 2_575 ? W1 Sm1 O5 W1 -121.26(10) 1_545 . . 2_575 ? W1 Sm1 O5 W1 121.26(10) . . . 2_575 ? Sm1 Sm1 O5 W1 180.000(6) 1_554 . . 2_575 ? Sm1 Sm1 O5 W1 0.000(6) 1_556 . . 2_575 ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 3.322 _refine_diff_density_min -5.668 _refine_diff_density_rms 0.839