# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 1145/152 data_Bi2W2O9 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'Bi2 O9 W2' _chemical_formula_weight 929.66 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' '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 ? _symmetry_space_group_name_H-M ? 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' _cell_length_a 5.4400(10) _cell_length_b 5.4130(10) _cell_length_c 23.740(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 699.1(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 8.833 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1544 _exptl_absorpt_coefficient_mu 83.021 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1320 _diffrn_reflns_av_R_equivalents 0.0502 _diffrn_reflns_av_sigmaI/netI 0.0579 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 1 _diffrn_reflns_theta_min 3.86 _diffrn_reflns_theta_max 29.99 _reflns_number_total 983 _reflns_number_gt 686 _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 w=1/[\s^2^(Fo^2^)+(0.0408P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00080(9) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.12(8) _refine_ls_number_reflns 983 _refine_ls_number_parameters 74 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0696 _refine_ls_R_factor_gt 0.0458 _refine_ls_wR_factor_ref 0.1002 _refine_ls_wR_factor_gt 0.0925 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.151 _refine_ls_shift/su_mean 0.006 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Bi1 Bi 0.1441(6) 0.4777(7) 0.28992(7) 0.0145(6) Uani 1 d . . . Bi2 Bi 0.1444(6) 0.9812(5) 0.39841(10) 0.0155(6) Uani 1 d . . . W1 W 0.1630(5) -0.0032(6) 0.17083(7) 0.0061(5) Uani 1 d . . . W2 W 0.8321(6) 0.5083(7) 0.01727(8) 0.0073(5) Uani 1 d . . . O1 O 0.910(6) 0.760(6) 0.3391(15) 0.008(7) Uiso 1 d . . . O2 O 0.937(5) 0.227(5) 0.3396(13) 0.010(6) Uiso 1 d . . . O3 O 0.765(7) 0.554(3) 0.0950(18) 0.012(4) Uiso 1 d . . . O4 O 0.900(7) 0.196(7) 0.1622(18) 0.014(8) Uiso 1 d . . . O5 O 0.066(6) 0.298(6) 0.0285(14) 0.008(7) Uiso 1 d . . . O6 O 0.770(8) 0.409(8) 0.9372(19) 0.026(9) Uiso 1 d . . . O7 O 0.989(6) 0.721(6) 0.1842(14) 0.006(6) Uiso 1 d . . . O8 O 0.998(6) 0.800(6) 0.0098(16) 0.010(7) Uiso 1 d . . . O9 O 0.215(5) 0.052(5) 0.2445(12) 0.010(6) Uiso 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 Bi1 0.0163(10) 0.0223(16) 0.0048(9) -0.0036(14) 0.0053(13) 0.0052(12) Bi2 0.0164(12) 0.0052(10) 0.0250(14) -0.0068(13) -0.0001(14) -0.0042(10) W1 0.0022(8) 0.0093(11) 0.0067(9) 0.0019(11) -0.0003(10) -0.0017(12) W2 0.0123(11) 0.0032(11) 0.0064(9) -0.0022(11) 0.0002(11) 0.0017(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Bi1 O2 2.12(3) 1_455 ? Bi1 O2 2.27(3) 3_455 ? Bi1 O1 2.31(3) 1_455 ? Bi1 O1 2.34(4) 3_465 ? Bi1 O9 2.58(3) 3_455 ? Bi1 O9 2.57(3) . ? Bi1 Bi1 3.671(5) 3_455 ? Bi1 Bi1 3.671(5) 3 ? Bi2 O2 2.24(3) 1_465 ? Bi2 O1 2.25(3) 1_455 ? Bi2 O6 2.35(4) 2_664 ? Bi2 O1 2.40(3) 3_465 ? Bi2 O6 2.47(5) 4_554 ? Bi2 O2 2.64(3) 3_465 ? Bi2 Bi2 3.696(3) 3_465 ? Bi2 Bi2 3.696(3) 3_565 ? W1 O9 1.80(3) . ? W1 O7 1.80(3) 1_445 ? W1 O4 1.80(4) 1_455 ? W1 O3 1.90(4) 3_455 ? W1 O4 2.11(4) 3_455 ? W1 O7 2.15(3) 3_455 ? W2 O5 1.73(3) 1_655 ? W2 O8 1.83(4) . ? W2 O3 1.90(4) . ? W2 O6 2.00(4) 1_554 ? W2 O8 2.10(3) 3_465 ? W2 O5 2.22(3) 3 ? O1 Bi2 2.25(3) 1_655 ? O1 Bi1 2.31(3) 1_655 ? O1 Bi1 2.34(4) 3_565 ? O1 Bi2 2.40(3) 3_565 ? O2 Bi1 2.12(3) 1_655 ? O2 Bi2 2.24(3) 1_645 ? O2 Bi1 2.27(3) 3 ? O2 Bi2 2.64(3) 3_565 ? O3 W1 1.90(4) 3 ? O4 W1 1.80(4) 1_655 ? O4 W1 2.11(4) 3 ? O5 W2 1.73(3) 1_455 ? O5 W2 2.22(3) 3_455 ? O6 W2 2.00(4) 1_556 ? O6 Bi2 2.35(4) 2_665 ? O6 Bi2 2.47(4) 4_545 ? O7 W1 1.80(3) 1_665 ? O7 W1 2.15(3) 3 ? O8 W2 2.10(3) 3_565 ? O9 Bi1 2.58(3) 3 ? 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 Bi1 O2 76.8(7) 1_455 3_455 ? O2 Bi1 O1 81.3(12) 1_455 1_455 ? O2 Bi1 O1 116.6(13) 3_455 1_455 ? O2 Bi1 O1 116.1(13) 1_455 3_465 ? O2 Bi1 O1 66.7(12) 3_455 3_465 ? O1 Bi1 O1 71.7(6) 1_455 3_465 ? O2 Bi1 O9 73.2(10) 1_455 3_455 ? O2 Bi1 O9 145.4(10) 3_455 3_455 ? O1 Bi1 O9 75.7(11) 1_455 3_455 ? O1 Bi1 O9 143.7(10) 3_465 3_455 ? O2 Bi1 O9 74.9(11) 1_455 . ? O2 Bi1 O9 71.0(9) 3_455 . ? O1 Bi1 O9 152.6(10) 1_455 . ? O1 Bi1 O9 131.3(10) 3_465 . ? O9 Bi1 O9 84.5(9) 3_455 . ? O2 Bi1 Bi1 34.6(8) 1_455 3_455 ? O2 Bi1 Bi1 101.1(8) 3_455 3_455 ? O1 Bi1 Bi1 92.0(8) 1_455 3_455 ? O1 Bi1 Bi1 150.0(8) 3_465 3_455 ? O9 Bi1 Bi1 44.5(7) 3_455 3_455 ? O9 Bi1 Bi1 60.7(7) . 3_455 ? O2 Bi1 Bi1 87.9(8) 1_455 3 ? O2 Bi1 Bi1 32.1(8) 3_455 3 ? O1 Bi1 Bi1 148.7(9) 1_455 3 ? O1 Bi1 Bi1 87.2(8) 3_465 3 ? O9 Bi1 Bi1 129.0(7) 3_455 3 ? O9 Bi1 Bi1 44.5(6) . 3 ? Bi1 Bi1 Bi1 95.62(18) 3_455 3 ? O2 Bi2 O1 68.8(12) 1_465 1_455 ? O2 Bi2 O6 151.6(13) 1_465 2_664 ? O1 Bi2 O6 83.0(14) 1_455 2_664 ? O2 Bi2 O1 105.1(13) 1_465 3_465 ? O1 Bi2 O1 71.6(8) 1_455 3_465 ? O6 Bi2 O1 67.9(13) 2_664 3_465 ? O2 Bi2 O6 82.3(13) 1_465 4_554 ? O1 Bi2 O6 68.2(13) 1_455 4_554 ? O6 Bi2 O6 83.8(14) 2_664 4_554 ? O1 Bi2 O6 133.0(13) 3_465 4_554 ? O2 Bi2 O2 67.5(6) 1_465 3_465 ? O1 Bi2 O2 109.3(12) 1_455 3_465 ? O6 Bi2 O2 128.8(12) 2_664 3_465 ? O1 Bi2 O2 69.7(11) 3_465 3_465 ? O6 Bi2 O2 147.4(12) 4_554 3_465 ? O2 Bi2 Bi2 91.8(7) 1_465 3_465 ? O1 Bi2 Bi2 38.8(8) 1_455 3_465 ? O6 Bi2 Bi2 62.4(11) 2_664 3_465 ? O1 Bi2 Bi2 94.3(8) 3_465 3_465 ? O6 Bi2 Bi2 38.7(10) 4_554 3_465 ? O2 Bi2 Bi2 148.0(6) 3_465 3_465 ? O2 Bi2 Bi2 140.8(9) 1_465 3_565 ? O1 Bi2 Bi2 93.2(9) 1_455 3_565 ? O6 Bi2 Bi2 41.1(11) 2_664 3_565 ? O1 Bi2 Bi2 35.9(8) 3_465 3_565 ? O6 Bi2 Bi2 124.4(10) 4_554 3_565 ? O2 Bi2 Bi2 87.8(6) 3_465 3_565 ? Bi2 Bi2 Bi2 94.76(12) 3_465 3_565 ? O9 W1 O7 92.8(14) . 1_445 ? O9 W1 O4 97.9(16) . 1_455 ? O7 W1 O4 95.6(17) 1_445 1_455 ? O9 W1 O3 154.0(15) . 3_455 ? O7 W1 O3 101.5(13) 1_445 3_455 ? O4 W1 O3 102.1(16) 1_455 3_455 ? O9 W1 O4 82.4(14) . 3_455 ? O7 W1 O4 172.9(17) 1_445 3_455 ? O4 W1 O4 90.1(5) 1_455 3_455 ? O3 W1 O4 81.1(14) 3_455 3_455 ? O9 W1 O7 79.4(13) . 3_455 ? O7 W1 O7 87.3(5) 1_445 3_455 ? O4 W1 O7 176.1(17) 1_455 3_455 ? O3 W1 O7 79.7(13) 3_455 3_455 ? O4 W1 O7 86.7(14) 3_455 3_455 ? O5 W2 O8 102.7(16) 1_655 . ? O5 W2 O3 94.5(15) 1_655 . ? O8 W2 O3 94.4(14) . . ? O5 W2 O6 95.3(17) 1_655 1_554 ? O8 W2 O6 102.9(18) . 1_554 ? O3 W2 O6 157.7(17) . 1_554 ? O5 W2 O8 167.3(14) 1_655 3_465 ? O8 W2 O8 89.6(6) . 3_465 ? O3 W2 O8 81.4(15) . 3_465 ? O6 W2 O8 84.7(17) 1_554 3_465 ? O5 W2 O5 88.3(4) 1_655 3 ? O8 W2 O5 168.6(14) . 3 ? O3 W2 O5 81.7(12) . 3 ? O6 W2 O5 78.7(15) 1_554 3 ? O8 W2 O5 79.3(13) 3_465 3 ? Bi2 O1 Bi1 110.9(14) 1_655 1_655 ? Bi2 O1 Bi1 109.8(13) 1_655 3_565 ? Bi1 O1 Bi1 119.4(15) 1_655 3_565 ? Bi2 O1 Bi2 105.3(14) 1_655 3_565 ? Bi1 O1 Bi2 105.7(13) 1_655 3_565 ? Bi1 O1 Bi2 104.6(13) 3_565 3_565 ? Bi1 O2 Bi2 117.3(13) 1_655 1_645 ? Bi1 O2 Bi1 113.4(13) 1_655 3 ? Bi2 O2 Bi1 112.9(11) 1_645 3 ? Bi1 O2 Bi2 103.3(11) 1_655 3_565 ? Bi2 O2 Bi2 109.2(13) 1_645 3_565 ? Bi1 O2 Bi2 98.3(10) 3 3_565 ? W2 O3 W1 163.1(12) . 3 ? W1 O4 W1 161(2) 1_655 3 ? W2 O5 W2 163(2) 1_455 3_455 ? W2 O6 Bi2 125(2) 1_556 2_665 ? W2 O6 Bi2 118(2) 1_556 4_545 ? Bi2 O6 Bi2 100.2(16) 2_665 4_545 ? W1 O7 W1 150(2) 1_665 3 ? W2 O8 W2 148(2) . 3_565 ? W1 O9 Bi1 122.8(14) . 3 ? W1 O9 Bi1 122.2(13) . . ? Bi1 O9 Bi1 90.9(9) 3 . ? _diffrn_measured_fraction_theta_max 0.905 _diffrn_reflns_theta_full 29.99 _diffrn_measured_fraction_theta_full 0.905 _refine_diff_density_max 3.337 _refine_diff_density_min -3.246 _refine_diff_density_rms 0.724