# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full Chem.Commun. #============================================================================ # 1. SUBMISSION DETAILS _journal_coden_Cambridge 0182 _publ_contact_author_name 'Louis Messerle' _publ_contact_author_address # Name and address of author for correspondence ; Dr. Louis Messerle Department of Chemistry The University of Iowa Iowa City, IA. 52242 United States of America ; _publ_contact_author_phone '319 335 1372' _publ_contact_author_fax '319 335 1270' _publ_contact_author_email lou-messerle@uiowa.edu _publ_requested_coeditor_name ? loop_ _publ_author_name _publ_author_address J.H.Thurston ; Department of Chemistry The University of Iowa Corner of Market and Madison Streets Iowa City, IA. 52242 United States of America ; D.C.Swenson ; Department of Chemistry The University of Iowa Corner of Market and Madison Streets Iowa City, IA. 52242 United States of America ; L.Messerle ; Department of Chemistry The University of Iowa Corner of Market and Madison Streets Iowa City, IA. 52242 United States of America ; #============================================================================ data_1 _database_code_depnum_ccdc_archive 'CCDC 268349' #data_Bi9(O)8(OH)6(ClO4)5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H12 Bi9 Cl5 O37' _chemical_formula_weight 2662.17 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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 Im loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z' 'x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 9.983(2) _cell_length_b 16.774(3) _cell_length_c 10.608(2) _cell_angle_alpha 90.00 _cell_angle_beta 92.85(3) _cell_angle_gamma 90.00 _cell_volume 1774.2(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 4.983 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2280 _exptl_absorpt_coefficient_mu 44.956 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1335 _exptl_absorpt_correction_T_max 0.2480 _exptl_absorpt_process_details 'HKL Scalepack (Otwinowski & Minor, 1997)' _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 'Nonius, kappa, CCD' _diffrn_measurement_method 'phi-omega CCD scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7405 _diffrn_reflns_av_R_equivalents 0.0331 _diffrn_reflns_av_sigmaI/netI 0.0582 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.66 _diffrn_reflns_theta_max 27.51 _reflns_number_total 4119 _reflns_number_gt 3743 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SHELXTL v. 6.1 (Bruker AXs, 2001)' _computing_cell_refinement 'SHELXTL v. 6.1 (Bruker AXs, 2001)' _computing_data_reduction 'SHELXTL v. 6.1 (Bruker AXs, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL v. 6.1 (Bruker AXs, 2001)' _computing_publication_material 'SHELXTL v. 6.1 (Bruker AXs, 2001)' _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^)+(0.0221P)^2^+5.6351P] 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 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.015(12) _refine_ls_number_reflns 4119 _refine_ls_number_parameters 221 _refine_ls_number_restraints 122 _refine_ls_R_factor_all 0.0380 _refine_ls_R_factor_gt 0.0309 _refine_ls_wR_factor_ref 0.0674 _refine_ls_wR_factor_gt 0.0647 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Bi1 Bi -1.10933(6) 0.5000 0.81771(6) 0.01514(14) Uani 1 2 d SU . . Bi2 Bi -1.09062(7) 0.5000 1.15633(6) 0.01717(15) Uani 1 2 d SU . . Bi4 Bi -0.78613(4) 0.61005(3) 0.81975(4) 0.01568(11) Uani 1 1 d U . . Bi5 Bi -0.76734(4) 0.61280(3) 1.15794(4) 0.01691(12) Uani 1 1 d U . . Bi3\ Bi -1.07218(5) 0.69244(3) 0.98419(5) 0.01958(11) Uani 1 1 d U . . Bi6 Bi -0.51199(7) 0.5000 0.98936(6) 0.01565(15) Uani 1 2 d SU . . Cl1 Cl -1.4043(3) 0.6766(2) 0.7638(3) 0.0248(7) Uani 1 1 d U . . O11 O -1.3037(10) 0.7314(6) 0.8107(11) 0.039(2) Uani 1 1 d U . . O12 O -1.4122(13) 0.6785(7) 0.6286(11) 0.050(3) Uani 1 1 d U . . O13 O -1.5348(11) 0.6996(7) 0.8122(13) 0.047(3) Uani 1 1 d U . . O14 O -1.3688(10) 0.5969(6) 0.8058(11) 0.035(2) Uani 1 1 d U . . Cl2 Cl -0.3593(4) 0.6575(2) 1.2607(4) 0.0321(8) Uiso 0.44(2) 1 d PU A 1 O21 O -0.317(3) 0.5792(18) 1.296(3) 0.052(9) Uiso 0.44(2) 1 d PU A 1 O22 O -0.380(3) 0.650(2) 1.135(3) 0.065(10) Uiso 0.44(2) 1 d PU A 1 O23 O -0.273(2) 0.7132(14) 1.309(2) 0.032(7) Uiso 0.44(2) 1 d PU A 1 O24 O -0.4886(12) 0.6701(7) 1.3090(10) 0.040(3) Uiso 0.44(2) 1 d PU A 1 Cl2' Cl -0.3593(4) 0.6575(2) 1.2607(4) 0.0321(8) Uiso 0.56(2) 1 d PU A 2 O21' O -0.3429(19) 0.5912(11) 1.1793(17) 0.029(5) Uiso 0.56(2) 1 d PU A 2 O22' O -0.314(2) 0.7306(14) 1.196(2) 0.057(7) Uiso 0.56(2) 1 d PU A 2 O23' O -0.259(3) 0.6582(19) 1.355(3) 0.084(10) Uiso 0.56(2) 1 d PU A 2 O24' O -0.4886(12) 0.6701(7) 1.3090(10) 0.040(3) Uiso 0.56(2) 1 d PU A 2 Cl3 Cl -0.8747(9) 0.5000 1.4674(7) 0.082(3) Uani 1 2 d SU . . O31 O -0.7940(17) 0.5733(11) 1.4273(16) 0.087 Uiso 1 1 d U . . O32 O -0.999(2) 0.5000 1.414(2) 0.075 Uiso 1 2 d SU . . O33 O -0.875(2) 0.5000 1.599(2) 0.082 Uiso 1 2 d SU . . O1 O -1.0307(9) 0.6425(5) 0.7912(8) 0.0186(3) Uani 1 1 d U . . H10A H -1.0623 0.6722 0.7159 0.022 Uiso 1 1 calc R . . O2 O -0.8923(11) 0.5000 0.8531(11) 0.0120(4) Uani 1 2 d SU . . O3 O -1.0136(9) 0.6398(5) 1.1852(8) 0.0207(4) Uani 1 1 d U . . H10B H -1.0396 0.6691 1.2600 0.025 Uiso 1 1 calc R . . O4 O -0.8775(11) 0.5000 1.1355(10) 0.0136(5) Uani 1 2 d SU . . O5 O -0.8670(8) 0.6628(5) 0.9891(8) 0.0164(3) Uani 1 1 d U . . O6 O -1.1302(8) 0.5730(5) 0.9860(8) 0.0153(4) Uani 1 1 d U . . O7 O -0.6262(12) 0.5000 0.7918(11) 0.0168(4) Uani 1 2 d SU . . H10C H -0.5735 0.5000 0.7163 0.020 Uiso 1 2 calc SR . . O8 O -0.6001(12) 0.5000 1.1862(11) 0.0171(6) Uani 1 2 d SU . . H10D H -0.5384 0.5000 1.2610 0.020 Uiso 1 2 calc SR . . O9 O -0.6571(8) 0.4102(5) 0.9894(8) 0.0159(13) Uani 1 1 d U . . O101 O -0.6220(11) 0.7658(6) 0.0778(10) 0.039(3) Uani 1 1 d . . . O102 O -0.517(2) 0.5000 -0.4480(19) 0.068(6) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Bi1 0.0116(3) 0.0185(3) 0.0150(3) 0.000 -0.0023(3) 0.000 Bi2 0.0121(3) 0.0246(3) 0.0150(3) 0.000 0.0028(3) 0.000 Bi4 0.0145(2) 0.0147(2) 0.0179(2) 0.00470(18) 0.00130(19) -0.00105(18) Bi5 0.0150(2) 0.0180(2) 0.0175(2) -0.00576(19) -0.00089(19) 0.00022(18) Bi3\ 0.0152(2) 0.0139(2) 0.0295(3) -0.00241(19) -0.00102(19) 0.00418(19) Bi6 0.0092(3) 0.0164(3) 0.0214(4) 0.000 0.0015(2) 0.000 Cl1 0.0138(15) 0.0230(16) 0.0375(18) 0.0165(14) -0.0005(13) -0.0027(12) O11 0.021(4) 0.026(4) 0.069(6) 0.003(5) -0.009(4) -0.001(3) O12 0.076(9) 0.035(6) 0.037(2) 0.012(4) -0.003(4) -0.001(6) O13 0.021(3) 0.039(6) 0.083(7) 0.023(6) 0.016(4) 0.005(3) O14 0.020(5) 0.025(3) 0.061(6) 0.022(4) -0.004(5) -0.001(3) Cl3 0.068(5) 0.144(8) 0.033(4) 0.000 0.006(3) 0.000 O1 0.0167(9) 0.0173(8) 0.0216(6) 0.0055(7) -0.0020(7) 0.0031(8) O2 0.0108(7) 0.0128(8) 0.0124(11) 0.000 0.0005(8) 0.000 O3 0.0171(11) 0.0238(10) 0.0213(6) -0.0087(8) 0.0015(7) 0.0036(9) O4 0.0116(9) 0.0174(11) 0.0117(11) 0.000 0.0005(10) 0.000 O5 0.0140(7) 0.0113(10) 0.0238(7) -0.0013(6) -0.0005(6) 0.0010(6) O6 0.0114(10) 0.0153(9) 0.0192(8) -0.0011(5) 0.0005(7) 0.0024(9) O7 0.0130(11) 0.0211(16) 0.0167(8) 0.000 0.0053(8) 0.000 O8 0.0128(12) 0.021(2) 0.0168(7) 0.000 -0.0033(9) 0.000 O9 0.016(4) 0.011(2) 0.0207(18) 0.0004(12) -0.001(3) -0.0003(16) O101 0.039(6) 0.035(6) 0.042(6) -0.017(5) -0.016(5) 0.005(5) O102 0.096(16) 0.046(11) 0.062(12) 0.000 0.016(11) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Bi1 O2 2.180(11) . ? Bi1 O6 2.183(9) . ? Bi1 O6 2.183(9) 2_565 ? Bi1 O1 2.536(9) 2_565 ? Bi1 O1 2.536(9) . ? Bi1 Bi2 3.5877(11) . ? Bi1 Bi3\ 3.6894(8) . ? Bi1 Bi3\ 3.6894(8) 2_565 ? Bi2 O4 2.150(12) . ? Bi2 O6 2.203(9) 2_565 ? Bi2 O6 2.203(9) . ? Bi2 O3 2.482(9) 2_565 ? Bi2 O3 2.482(9) . ? Bi4 O2 2.167(6) . ? Bi4 O9 2.186(8) 2_565 ? Bi4 O5 2.192(9) . ? Bi4 O7 2.468(8) . ? Bi4 O1 2.505(8) . ? Bi4 Bi5 3.5835(9) . ? Bi4 Bi3\ 3.6883(11) . ? Bi4 Bi4 3.6921(12) 2_565 ? Bi4 Bi6 3.6938(11) . ? Bi5 O5 2.174(8) . ? Bi5 O9 2.180(9) 2_565 ? Bi5 O4 2.195(6) . ? Bi5 O3 2.530(9) . ? Bi5 O8 2.531(8) . ? Bi3\ O6 2.085(9) . ? Bi3\ O5 2.106(8) . ? Bi3\ O1 2.269(9) . ? Bi3\ O3 2.355(9) . ? Bi6 O9 2.090(8) . ? Bi6 O9 2.090(8) 2_565 ? Bi6 O8 2.306(12) . ? Bi6 O7 2.335(12) . ? Bi6 Bi4 3.6938(11) 2_565 ? Cl1 O11 1.432(10) . ? Cl1 O12 1.433(12) . ? Cl1 O14 1.448(10) . ? Cl1 O13 1.476(12) . ? Cl2 O22 1.34(3) . ? Cl2 O23 1.35(2) . ? Cl2 O21 1.43(3) . ? Cl2 O24 1.428(12) . ? Cl3 O32 1.34(2) . ? Cl3 O33 1.39(2) . ? Cl3 O31 1.541(18) 2_565 ? Cl3 O31 1.541(18) . ? O2 Bi4 2.167(6) 2_565 ? O4 Bi5 2.195(6) 2_565 ? O7 Bi4 2.468(8) 2_565 ? O8 Bi5 2.531(8) 2_565 ? O9 Bi5 2.180(9) 2_565 ? O9 Bi4 2.186(8) 2_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Bi1 O6 89.6(3) . . ? O2 Bi1 O6 89.6(3) . 2_565 ? O6 Bi1 O6 68.3(5) . 2_565 ? O2 Bi1 O1 73.1(2) . 2_565 ? O6 Bi1 O1 131.5(3) . 2_565 ? O6 Bi1 O1 66.7(3) 2_565 2_565 ? O2 Bi1 O1 73.1(2) . . ? O6 Bi1 O1 66.7(3) . . ? O6 Bi1 O1 131.5(3) 2_565 . ? O1 Bi1 O1 141.0(4) 2_565 . ? O2 Bi1 Bi2 80.0(3) . . ? O6 Bi1 Bi2 35.3(2) . . ? O6 Bi1 Bi2 35.3(2) 2_565 . ? O1 Bi1 Bi2 96.3(2) 2_565 . ? O1 Bi1 Bi2 96.3(2) . . ? O2 Bi1 Bi3\ 80.92(14) . . ? O6 Bi1 Bi3\ 29.4(2) . . ? O6 Bi1 Bi3\ 96.4(2) 2_565 . ? O1 Bi1 Bi3\ 148.60(19) 2_565 . ? O1 Bi1 Bi3\ 37.3(2) . . ? Bi2 Bi1 Bi3\ 61.427(14) . . ? O2 Bi1 Bi3\ 80.92(14) . 2_565 ? O6 Bi1 Bi3\ 96.4(2) . 2_565 ? O6 Bi1 Bi3\ 29.4(2) 2_565 2_565 ? O1 Bi1 Bi3\ 37.3(2) 2_565 2_565 ? O1 Bi1 Bi3\ 148.60(19) . 2_565 ? Bi2 Bi1 Bi3\ 61.427(14) . 2_565 ? Bi3\ Bi1 Bi3\ 122.08(3) . 2_565 ? O4 Bi2 O6 93.1(3) . 2_565 ? O4 Bi2 O6 93.1(3) . . ? O6 Bi2 O6 67.6(4) 2_565 . ? O4 Bi2 O3 73.2(2) . 2_565 ? O6 Bi2 O3 67.5(3) 2_565 2_565 ? O6 Bi2 O3 132.0(3) . 2_565 ? O4 Bi2 O3 73.2(2) . . ? O6 Bi2 O3 132.0(3) 2_565 . ? O6 Bi2 O3 67.5(3) . . ? O3 Bi2 O3 141.7(4) 2_565 . ? O4 Bi2 Bi1 84.2(3) . . ? O6 Bi2 Bi1 34.9(2) 2_565 . ? O6 Bi2 Bi1 34.9(2) . . ? O3 Bi2 Bi1 97.1(2) 2_565 . ? O3 Bi2 Bi1 97.1(2) . . ? O2 Bi4 O9 90.4(4) . 2_565 ? O2 Bi4 O5 90.4(4) . . ? O9 Bi4 O5 67.3(3) 2_565 . ? O2 Bi4 O7 73.0(3) . . ? O9 Bi4 O7 68.0(3) 2_565 . ? O5 Bi4 O7 131.8(3) . . ? O2 Bi4 O1 73.9(3) . . ? O9 Bi4 O1 131.6(3) 2_565 . ? O5 Bi4 O1 67.4(3) . . ? O7 Bi4 O1 141.3(3) . . ? O2 Bi4 Bi5 81.3(3) . . ? O9 Bi4 Bi5 34.8(2) 2_565 . ? O5 Bi4 Bi5 34.7(2) . . ? O7 Bi4 Bi5 97.3(3) . . ? O1 Bi4 Bi5 96.9(2) . . ? O2 Bi4 Bi3\ 81.1(3) . . ? O9 Bi4 Bi3\ 96.1(2) 2_565 . ? O5 Bi4 Bi3\ 30.2(2) . . ? O7 Bi4 Bi3\ 149.1(2) . . ? O1 Bi4 Bi3\ 37.2(2) . . ? Bi5 Bi4 Bi3\ 61.63(3) . . ? O2 Bi4 Bi4 31.6(3) . 2_565 ? O9 Bi4 Bi4 81.1(2) 2_565 2_565 ? O5 Bi4 Bi4 113.8(2) . 2_565 ? O7 Bi4 Bi4 41.6(2) . 2_565 ? O1 Bi4 Bi4 102.6(2) . 2_565 ? Bi5 Bi4 Bi4 90.736(12) . 2_565 ? Bi3\ Bi4 Bi4 112.005(13) . 2_565 ? O2 Bi4 Bi6 81.4(3) . . ? O9 Bi4 Bi6 29.5(2) 2_565 . ? O5 Bi4 Bi6 95.5(2) . . ? O7 Bi4 Bi6 38.4(3) . . ? O1 Bi4 Bi6 149.5(2) . . ? Bi5 Bi4 Bi6 61.20(2) . . ? Bi3\ Bi4 Bi6 121.95(2) . . ? Bi4 Bi4 Bi6 60.015(13) 2_565 . ? O5 Bi5 O9 67.7(3) . 2_565 ? O5 Bi5 O4 92.1(3) . . ? O9 Bi5 O4 91.7(4) 2_565 . ? O5 Bi5 O3 67.5(3) . . ? O9 Bi5 O3 131.2(3) 2_565 . ? O4 Bi5 O3 71.5(3) . . ? O5 Bi5 O8 131.2(3) . . ? O9 Bi5 O8 66.9(3) 2_565 . ? O4 Bi5 O8 72.1(3) . . ? O3 Bi5 O8 139.4(3) . . ? O5 Bi5 Bi4 35.0(2) . . ? O9 Bi5 Bi4 34.9(2) 2_565 . ? O4 Bi5 Bi4 83.1(3) . . ? O3 Bi5 Bi4 96.5(2) . . ? O8 Bi5 Bi4 96.3(3) . . ? O6 Bi3\ O5 92.5(3) . . ? O6 Bi3\ O1 73.6(3) . . ? O5 Bi3\ O1 73.4(3) . . ? O6 Bi3\ O3 71.8(3) . . ? O5 Bi3\ O3 72.0(3) . . ? O1 Bi3\ O3 129.1(3) . . ? O6 Bi3\ Bi4 82.3(2) . . ? O5 Bi3\ Bi4 31.6(2) . . ? O1 Bi3\ Bi4 41.8(2) . . ? O3 Bi3\ Bi4 97.2(2) . . ? O6 Bi3\ Bi1 31.0(2) . . ? O5 Bi3\ Bi1 83.1(2) . . ? O1 Bi3\ Bi1 42.6(2) . . ? O3 Bi3\ Bi1 96.9(2) . . ? Bi4 Bi3\ Bi1 60.493(18) . . ? O9 Bi6 O9 92.3(4) . 2_565 ? O9 Bi6 O8 72.8(3) . . ? O9 Bi6 O8 72.8(3) 2_565 . ? O9 Bi6 O7 72.1(3) . . ? O9 Bi6 O7 72.1(3) 2_565 . ? O8 Bi6 O7 128.4(4) . . ? O9 Bi6 Bi4 31.0(2) . 2_565 ? O9 Bi6 Bi4 82.2(2) 2_565 2_565 ? O8 Bi6 Bi4 97.7(2) . 2_565 ? O7 Bi6 Bi4 41.1(2) . 2_565 ? O9 Bi6 Bi4 82.2(2) . . ? O9 Bi6 Bi4 31.0(2) 2_565 . ? O8 Bi6 Bi4 97.7(2) . . ? O7 Bi6 Bi4 41.07(19) . . ? Bi4 Bi6 Bi4 59.97(3) 2_565 . ? O11 Cl1 O12 109.7(7) . . ? O11 Cl1 O14 109.2(6) . . ? O12 Cl1 O14 109.2(7) . . ? O11 Cl1 O13 109.1(7) . . ? O12 Cl1 O13 109.7(7) . . ? O14 Cl1 O13 109.9(7) . . ? O22 Cl2 O23 120.2(18) . . ? O22 Cl2 O21 102(2) . . ? O23 Cl2 O21 111.2(15) . . ? O22 Cl2 O24 105.6(15) . . ? O23 Cl2 O24 109.3(11) . . ? O21 Cl2 O24 107.7(13) . . ? O32 Cl3 O33 112.1(15) . . ? O32 Cl3 O31 111.6(9) . 2_565 ? O33 Cl3 O31 107.7(9) . 2_565 ? O32 Cl3 O31 111.6(9) . . ? O33 Cl3 O31 107.7(9) . . ? O31 Cl3 O31 105.8(14) 2_565 . ? Bi3\ O1 Bi4 101.0(3) . . ? Bi3\ O1 Bi1 100.1(3) . . ? Bi4 O1 Bi1 95.0(3) . . ? Bi4 O2 Bi4 116.9(5) 2_565 . ? Bi4 O2 Bi1 117.5(3) 2_565 . ? Bi4 O2 Bi1 117.5(3) . . ? Bi3\ O3 Bi2 100.4(3) . . ? Bi3\ O3 Bi5 99.4(3) . . ? Bi2 O3 Bi5 96.5(3) . . ? Bi2 O4 Bi5 118.8(3) . 2_565 ? Bi2 O4 Bi5 118.8(3) . . ? Bi5 O4 Bi5 119.1(5) 2_565 . ? Bi3\ O5 Bi5 121.1(4) . . ? Bi3\ O5 Bi4 118.2(4) . . ? Bi5 O5 Bi4 110.3(3) . . ? Bi3\ O6 Bi1 119.6(4) . . ? Bi3\ O6 Bi2 120.2(4) . . ? Bi1 O6 Bi2 109.8(4) . . ? Bi6 O7 Bi4 100.5(4) . 2_565 ? Bi6 O7 Bi4 100.5(3) . . ? Bi4 O7 Bi4 96.8(4) 2_565 . ? Bi6 O8 Bi5 99.9(3) . 2_565 ? Bi6 O8 Bi5 99.9(3) . . ? Bi5 O8 Bi5 96.8(4) 2_565 . ? Bi6 O9 Bi5 120.4(4) . 2_565 ? Bi6 O9 Bi4 119.4(4) . 2_565 ? Bi5 O9 Bi4 110.3(3) 2_565 2_565 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.493 _refine_diff_density_min -2.013 _refine_diff_density_rms 0.347 #====END data_2 _database_code_depnum_ccdc_archive 'CCDC 268350' #data_Bi9(O)8(OEt)6(HOEt)4(ClO4)5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H78 Bi9 Cl5 O42' _chemical_formula_weight 3144.97 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 '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' Cl Cl 0.1484 0.1585 '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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.434(3) _cell_length_b 26.027(5) _cell_length_c 20.985(4) _cell_angle_alpha 90.00 _cell_angle_beta 106.87(3) _cell_angle_gamma 90.00 _cell_volume 7022(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 trapezoid _exptl_crystal_colour colorless _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.085 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.975 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5656 _exptl_absorpt_coefficient_mu 22.748 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.0690 _exptl_absorpt_correction_T_max 0.2944 _exptl_absorpt_process_details 'HKL Scalepack (Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius, kappa, CCD' _diffrn_measurement_method 'phi-omega CCD scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25308 _diffrn_reflns_av_R_equivalents 0.0831 _diffrn_reflns_av_sigmaI/netI 0.0607 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.28 _diffrn_reflns_theta_max 20.81 _reflns_number_total 7352 _reflns_number_gt 5741 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SHELXTL 6.10 (Bruker AXS, 2001)' _computing_cell_refinement 'SHELXTL 6.10 (Bruker AXS, 2001)' _computing_data_reduction 'SHELXTL 6.10 (Bruker AXS, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL 6.10 (Bruker AXS, 2001)' _computing_publication_material 'SHELXTL 6.10 (Bruker AXS, 2001)' _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^)+(0.0650P)^2^+73.9884P] 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 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7352 _refine_ls_number_parameters 590 _refine_ls_number_restraints 259 _refine_ls_R_factor_all 0.0702 _refine_ls_R_factor_gt 0.0465 _refine_ls_wR_factor_ref 0.1377 _refine_ls_wR_factor_gt 0.1169 _refine_ls_goodness_of_fit_ref 1.188 _refine_ls_restrained_S_all 1.168 _refine_ls_shift/su_max 0.146 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Bi1 Bi 1.89601(6) -0.70951(3) -0.34202(5) 0.0318(3) Uani 1 1 d U . . Bi2 Bi 1.87317(7) -0.56514(3) -0.35817(5) 0.0333(3) Uani 1 1 d U . . Bi3 Bi 2.13348(6) -0.63021(3) -0.31409(5) 0.0311(3) Uani 1 1 d U . . Bi4 Bi 1.91513(7) -0.70069(3) -0.16907(5) 0.0320(3) Uani 1 1 d U . . Bi5 Bi 1.88452(7) -0.55742(3) -0.18699(5) 0.0324(3) Uani 1 1 d U . . Bi6 Bi 2.15080(6) -0.61755(3) -0.14095(5) 0.0312(3) Uani 1 1 d U . . Bi7 Bi 1.68307(7) -0.64229(3) -0.29587(5) 0.0362(3) Uani 1 1 d U . . Bi8 Bi 2.10080(7) -0.50068(3) -0.24283(5) 0.0348(3) Uani 1 1 d U . . Bi9 Bi 2.14267(6) -0.74909(3) -0.21597(5) 0.0331(3) Uani 1 1 d U . . Cl2 Cl 1.0447(5) -0.3573(3) 0.5000(3) 0.0496(18) Uani 1 1 d . . . Cl3 Cl 1.0013(5) -0.3779(2) 0.0053(3) 0.0420(15) Uani 1 1 d U . . Cl4 Cl 0.9392(5) -0.1101(2) 0.2235(4) 0.059(2) Uani 1 1 d . . . Cl5 Cl 1.3837(7) -0.4805(3) -0.1841(5) 0.082(3) Uani 1 1 d . . . Cl6 Cl 1.3979(5) 0.1525(2) 0.1981(4) 0.0514(19) Uani 1 1 d . . . O1 O 1.9833(10) -0.6273(5) -0.1770(7) 0.032(2) Uani 1 1 d U . . O2X O 1.7498(14) -0.4799(7) -0.3780(10) 0.078(6) Uiso 1 1 d D . . H2XZ H 1.702(5) -0.492(3) -0.408(2) 0.117 Uiso 1 1 d D . . O2 O 1.9674(10) -0.6337(5) -0.3262(7) 0.029(2) Uani 1 1 d U . . O3 O 2.0844(10) -0.7245(5) -0.3298(7) 0.0344(8) Uani 1 1 d U . . O4 O 2.0587(11) -0.5376(5) -0.3481(7) 0.0360(8) Uani 1 1 d U . . O5 O 1.7449(11) -0.6446(5) -0.3889(7) 0.0366(8) Uani 1 1 d U . . O5X O 1.7373(17) -0.4874(8) -0.2180(12) 0.095(7) Uiso 1 1 d D . . H5XZ H 1.738(9) -0.4566(9) -0.226(3) 0.143 Uiso 1 1 d D . . O6 O 1.7638(11) -0.6299(5) -0.1818(8) 0.0358(8) Uani 1 1 d U . . O7 O 2.1090(11) -0.7186(5) -0.1224(7) 0.0348(8) Uani 1 1 d U . . O7X O 1.6161(13) -0.7383(7) -0.3434(9) 0.065(5) Uiso 1 1 d D . . H7XZ H 1.610(5) -0.727(4) -0.3810(19) 0.098 Uiso 1 1 d D . . O8 O 2.0853(11) -0.5293(5) -0.1430(7) 0.0354(8) Uani 1 1 d U . . O9X O 2.3453(13) -0.7296(7) -0.1487(9) 0.065(5) Uiso 1 1 d D . . H9XZ H 2.368(13) -0.734(8) -0.1085(13) 0.098 Uiso 1 1 d D . . O9 O 2.1699(10) -0.6713(5) -0.2194(7) 0.0294(18) Uani 1 1 d U . . O10 O 2.1551(10) -0.5760(5) -0.2293(7) 0.032(2) Uani 1 1 d U . . O11 O 1.9488(10) -0.5274(5) -0.2639(7) 0.0352(19) Uani 1 1 d U . . O12 O 1.7894(10) -0.5813(5) -0.2853(7) 0.033(2) Uani 1 1 d U . . O13 O 1.8082(10) -0.6928(5) -0.2705(7) 0.033(2) Uani 1 1 d U . . O14 O 1.9827(10) -0.7330(5) -0.2414(7) 0.0313(18) Uani 1 1 d U . . O21 O 0.9401(13) -0.3631(7) 0.4562(9) 0.061(5) Uani 1 1 d . . . O22 O 1.0416(14) -0.3577(7) 0.5671(9) 0.065(5) Uani 1 1 d . . . O23 O 1.1054(14) -0.4006(7) 0.4906(10) 0.084(7) Uani 1 1 d . . . O24 O 1.0900(15) -0.3110(7) 0.4835(10) 0.070(6) Uani 1 1 d . . . O31 O 1.0581(12) -0.4200(6) 0.0441(8) 0.053(4) Uani 1 1 d U . . O32 O 0.8974(12) -0.3776(6) 0.0141(9) 0.054(4) Uani 1 1 d U . . O33 O 0.9945(14) -0.3823(6) -0.0639(8) 0.058(5) Uani 1 1 d U . . O34 O 1.0523(12) -0.3308(6) 0.0348(9) 0.054(4) Uani 1 1 d U . . O41 O 0.9818(14) -0.1603(6) 0.2301(14) 0.109(10) Uani 1 1 d . . . O42 O 0.9762(15) -0.0803(8) 0.1759(10) 0.081(6) Uani 1 1 d . . . O43 O 0.9744(14) -0.0838(6) 0.2876(10) 0.063(5) Uani 1 1 d . . . O44 O 0.8271(13) -0.1144(6) 0.2001(10) 0.066(6) Uani 1 1 d . . . O51 O 1.3155(17) -0.4897(10) -0.1507(13) 0.109(8) Uani 1 1 d . . . O52 O 1.4562(15) -0.5232(8) -0.1746(11) 0.082(6) Uani 1 1 d . . . O53 O 1.4304(19) -0.4378(9) -0.1700(18) 0.157(14) Uani 1 1 d . . . O54 O 1.3171(19) -0.4802(10) -0.2549(14) 0.119(9) Uani 1 1 d . . . O61 O 1.4862(14) 0.1677(7) 0.2531(11) 0.079(6) Uani 1 1 d . . . O62 O 1.3558(13) 0.1066(7) 0.2155(11) 0.078(7) Uani 1 1 d . . . O63 O 1.3209(13) 0.1919(7) 0.1849(11) 0.073(6) Uani 1 1 d . . . O64 O 1.4297(13) 0.1431(7) 0.1389(10) 0.064(5) Uani 1 1 d . . . C2X C 1.758(3) -0.4476(16) -0.4398(18) 0.144(17) Uiso 1 1 d D . . H2XA H 1.8094 -0.4210 -0.4234 0.173 Uiso 1 1 calc R . . H2XB H 1.7846 -0.4701 -0.4678 0.173 Uiso 1 1 calc R . . C2Y C 1.674(3) -0.4254(19) -0.478(2) 0.19(2) Uiso 1 1 d D . . H2YA H 1.6907 -0.4079 -0.5137 0.278 Uiso 1 1 calc R . . H2YB H 1.6483 -0.4011 -0.4521 0.278 Uiso 1 1 calc R . . H2YC H 1.6218 -0.4509 -0.4957 0.278 Uiso 1 1 calc R . . C3A C 2.1111(17) -0.7525(8) -0.3827(12) 0.039(6) Uiso 1 1 d . . . H3AA H 2.1452 -0.7292 -0.4057 0.046 Uiso 1 1 calc R . . H3AB H 2.0474 -0.7643 -0.4146 0.046 Uiso 1 1 calc R . . C3B C 2.1809(18) -0.7981(9) -0.3588(13) 0.055(7) Uiso 1 1 d . . . H3BA H 2.1953 -0.8145 -0.3961 0.082 Uiso 1 1 calc R . . H3BB H 2.1471 -0.8219 -0.3370 0.082 Uiso 1 1 calc R . . H3BC H 2.2449 -0.7867 -0.3280 0.082 Uiso 1 1 calc R . . C4A C 2.0732(19) -0.5079(10) -0.4048(14) 0.057(8) Uiso 1 1 d . . . H4AA H 2.0552 -0.4722 -0.4007 0.069 Uiso 1 1 calc R . . H4AB H 2.0276 -0.5213 -0.4461 0.069 Uiso 1 1 calc R . . C4B C 2.187(2) -0.5117(13) -0.4058(18) 0.102(12) Uiso 1 1 d . . . H4BA H 2.1954 -0.4926 -0.4429 0.153 Uiso 1 1 calc R . . H4BB H 2.2042 -0.5471 -0.4099 0.153 Uiso 1 1 calc R . . H4BC H 2.2315 -0.4979 -0.3652 0.153 Uiso 1 1 calc R . . C5A C 1.673(2) -0.6550(12) -0.4594(17) 0.087(10) Uiso 1 1 d . . . H5AA H 1.7156 -0.6587 -0.4896 0.105 Uiso 1 1 calc R . . H5AB H 1.6367 -0.6871 -0.4595 0.105 Uiso 1 1 calc R . . C5B C 1.601(3) -0.6155(17) -0.482(2) 0.154(18) Uiso 1 1 d . . . H5BA H 1.5580 -0.6236 -0.5264 0.231 Uiso 1 1 calc R . . H5BB H 1.6369 -0.5838 -0.4834 0.231 Uiso 1 1 calc R . . H5BC H 1.5582 -0.6121 -0.4530 0.231 Uiso 1 1 calc R . . C5X C 1.727(4) -0.4630(18) -0.1511(18) 0.17(2) Uiso 1 1 d D . . H5XA H 1.6835 -0.4843 -0.1324 0.206 Uiso 1 1 calc R . . H5XB H 1.7951 -0.4600 -0.1188 0.206 Uiso 1 1 calc R . . C5Y C 1.685(5) -0.418(2) -0.166(3) 0.26(3) Uiso 1 1 d D . . H5YA H 1.6817 -0.4007 -0.1260 0.396 Uiso 1 1 calc R . . H5YB H 1.6167 -0.4211 -0.1960 0.396 Uiso 1 1 calc R . . H5YC H 1.7273 -0.3975 -0.1867 0.396 Uiso 1 1 calc R . . C6A C 1.7033(18) -0.6235(9) -0.1341(13) 0.046(7) Uiso 1 1 d . . . H6AA H 1.7434 -0.6038 -0.0960 0.055 Uiso 1 1 calc R . . H6AB H 1.6399 -0.6047 -0.1550 0.055 Uiso 1 1 calc R . . C6B C 1.678(2) -0.6738(9) -0.1120(14) 0.059(8) Uiso 1 1 d . . . H6BA H 1.6378 -0.6693 -0.0811 0.089 Uiso 1 1 calc R . . H6BB H 1.7405 -0.6921 -0.0907 0.089 Uiso 1 1 calc R . . H6BC H 1.6374 -0.6930 -0.1498 0.089 Uiso 1 1 calc R . . C7A C 2.1554(18) -0.7415(9) -0.0570(12) 0.047(7) Uiso 1 1 d . . . H7AA H 2.2112 -0.7191 -0.0328 0.056 Uiso 1 1 calc R . . H7AB H 2.1030 -0.7412 -0.0335 0.056 Uiso 1 1 calc R . . C7B C 2.194(3) -0.7897(15) -0.053(2) 0.136(16) Uiso 1 1 d . . . H7BA H 2.2210 -0.7995 -0.0071 0.204 Uiso 1 1 calc R . . H7BB H 2.2493 -0.7908 -0.0737 0.204 Uiso 1 1 calc R . . H7BC H 2.1401 -0.8131 -0.0754 0.204 Uiso 1 1 calc R . . C7X C 1.510(2) -0.7634(13) -0.3838(17) 0.114(13) Uiso 1 1 d D . . H7XA H 1.4555 -0.7377 -0.3925 0.136 Uiso 1 1 calc R . . H7XB H 1.5157 -0.7756 -0.4262 0.136 Uiso 1 1 calc R . . C7Y C 1.485(3) -0.8019(12) -0.3511(18) 0.107(12) Uiso 1 1 d D . . H7YA H 1.4206 -0.8168 -0.3774 0.160 Uiso 1 1 calc R . . H7YB H 1.4765 -0.7896 -0.3098 0.160 Uiso 1 1 calc R . . H7YC H 1.5387 -0.8274 -0.3423 0.160 Uiso 1 1 calc R . . C8A C 2.1010(18) -0.4937(9) -0.0870(13) 0.051(7) Uiso 1 1 d . . . H8AA H 2.0436 -0.4971 -0.0680 0.062 Uiso 1 1 calc R . . H8AB H 2.1003 -0.4588 -0.1034 0.062 Uiso 1 1 calc R . . C8B C 2.204(2) -0.5028(11) -0.0317(16) 0.083(10) Uiso 1 1 d . . . H8BA H 2.2102 -0.4786 0.0037 0.125 Uiso 1 1 calc R . . H8BB H 2.2617 -0.4984 -0.0498 0.125 Uiso 1 1 calc R . . H8BC H 2.2052 -0.5371 -0.0147 0.125 Uiso 1 1 calc R . . C9X C 2.436(2) -0.7681(10) -0.1456(18) 0.091(11) Uiso 1 1 d D . . H9XA H 2.4746 -0.7561 -0.1755 0.109 Uiso 1 1 calc R . . H9XB H 2.4837 -0.7678 -0.1008 0.109 Uiso 1 1 calc R . . C9Y C 2.406(3) -0.8156(12) -0.1615(19) 0.117(13) Uiso 1 1 d D . . H9YA H 2.4661 -0.8366 -0.1590 0.176 Uiso 1 1 calc R . . H9YB H 2.3602 -0.8165 -0.2060 0.176 Uiso 1 1 calc R . . H9YC H 2.3710 -0.8284 -0.1310 0.176 Uiso 1 1 calc R . . O91A O 2.3718(14) -0.6185(7) -0.1241(10) 0.074(6) Uiso 1 1 d . . . H91E H 2.3735 -0.6500 -0.1218 0.111 Uiso 1 1 calc R . . C91A C 2.428(4) -0.6178(18) -0.005(3) 0.17(2) Uiso 1 1 d . . . H91F H 2.4702 -0.6024 0.0353 0.251 Uiso 1 1 calc R . . H91G H 2.4461 -0.6534 -0.0061 0.251 Uiso 1 1 calc R . . H91H H 2.3558 -0.6151 -0.0064 0.251 Uiso 1 1 calc R . . C92A C 2.442(3) -0.5947(14) -0.0549(19) 0.109(13) Uiso 1 1 d . . . H92E H 2.5150 -0.5973 -0.0531 0.131 Uiso 1 1 calc R . . H92F H 2.4256 -0.5586 -0.0529 0.131 Uiso 1 1 calc R . . O92A O 1.8351(12) -0.8041(6) -0.1866(9) 0.054(5) Uiso 1 1 d . . . H92A H 1.8201 -0.8029 -0.2273 0.080 Uiso 1 1 calc R . . C93A C 1.700(3) -0.8625(12) -0.1740(19) 0.105(12) Uiso 1 1 d . . . H93F H 1.6391 -0.8631 -0.1593 0.157 Uiso 1 1 calc R . . H93G H 1.7512 -0.8857 -0.1474 0.157 Uiso 1 1 calc R . . H93H H 1.6829 -0.8728 -0.2198 0.157 Uiso 1 1 calc R . . C94A C 1.743(2) -0.8109(11) -0.1671(17) 0.082(10) Uiso 1 1 d . . . H94E H 1.6901 -0.7878 -0.1934 0.098 Uiso 1 1 calc R . . H94F H 1.7574 -0.8006 -0.1209 0.098 Uiso 1 1 calc R . . O93B O 1.7902(11) 1.1995(5) -0.3253(8) 0.042(4) Uiso 1 1 d . . . H93E H 1.7321 1.2125 -0.3379 0.063 Uiso 1 1 calc R . . C95B C 1.748(3) 1.1542(13) -0.4294(17) 0.097(11) Uiso 1 1 d . . . H95A H 1.7524 1.1215 -0.4497 0.146 Uiso 1 1 calc R . . H95B H 1.7852 1.1795 -0.4467 0.146 Uiso 1 1 calc R . . H95C H 1.6765 1.1642 -0.4390 0.146 Uiso 1 1 calc R . . C96B C 1.791(2) 1.1504(10) -0.3621(15) 0.069(9) Uiso 1 1 d . . . H96A H 1.8623 1.1387 -0.3531 0.083 Uiso 1 1 calc R . . H96B H 1.7532 1.1245 -0.3452 0.083 Uiso 1 1 calc R . . O94A O 1.5567(14) -0.5412(7) 0.7186(10) 0.070(6) Uiso 1 1 d . . . H94A H 1.6094 -0.5245 0.7360 0.105 Uiso 1 1 calc R . . C97A C 1.492(2) -0.4657(11) 0.6513(17) 0.092(11) Uiso 1 1 d . . . H97D H 1.4602 -0.4561 0.6058 0.138 Uiso 1 1 calc R . . H97E H 1.5572 -0.4482 0.6679 0.138 Uiso 1 1 calc R . . H97F H 1.4469 -0.4565 0.6775 0.138 Uiso 1 1 calc R . . C98A C 1.510(2) -0.5226(10) 0.6555(15) 0.068(8) Uiso 1 1 d . . . H98C H 1.4438 -0.5398 0.6378 0.082 Uiso 1 1 calc R . . H98D H 1.5533 -0.5315 0.6273 0.082 Uiso 1 1 calc R . . 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 0.0351(5) 0.0293(5) 0.0303(5) -0.0035(4) 0.0082(4) -0.0016(4) Bi2 0.0368(5) 0.0312(5) 0.0315(5) 0.0042(4) 0.0094(4) 0.0057(4) Bi3 0.0321(5) 0.0326(5) 0.0301(5) -0.0001(4) 0.0114(4) 0.0012(4) Bi4 0.0384(5) 0.0281(5) 0.0315(5) -0.0010(4) 0.0133(4) -0.0021(4) Bi5 0.0381(5) 0.0269(5) 0.0336(6) -0.0025(4) 0.0126(4) 0.0040(4) Bi6 0.0338(5) 0.0303(5) 0.0277(5) -0.0015(4) 0.0061(4) 0.0011(4) Bi7 0.0302(5) 0.0376(5) 0.0407(7) -0.0010(5) 0.0099(4) 0.0008(4) Bi8 0.0383(6) 0.0232(5) 0.0434(7) 0.0003(4) 0.0126(5) -0.0006(4) Bi9 0.0370(5) 0.0247(5) 0.0365(6) -0.0012(4) 0.0090(4) 0.0051(4) Cl2 0.058(4) 0.061(5) 0.029(4) 0.003(3) 0.011(3) 0.007(4) Cl3 0.058(4) 0.042(3) 0.028(3) -0.002(3) 0.016(3) 0.003(3) Cl4 0.063(5) 0.031(4) 0.089(6) -0.007(4) 0.030(4) -0.002(3) Cl5 0.077(6) 0.068(6) 0.113(9) -0.001(5) 0.046(6) -0.009(5) Cl6 0.034(4) 0.048(4) 0.072(6) 0.009(4) 0.015(4) 0.003(3) O1 0.0334(12) 0.0241(17) 0.037(6) -0.002(4) 0.009(4) 0.0011(14) O2 0.0310(18) 0.0279(14) 0.027(6) 0.007(4) 0.008(4) 0.0002(12) O3 0.037(2) 0.033(2) 0.035(2) -0.002(4) 0.012(4) 0.000(4) O4 0.045(3) 0.030(3) 0.034(3) 0.009(3) 0.013(5) -0.005(4) O5 0.032(5) 0.043(5) 0.031(4) -0.003(4) 0.002(4) 0.0015(14) O6 0.036(5) 0.038(5) 0.038(2) -0.004(5) 0.019(4) 0.0000(15) O7 0.042(2) 0.030(3) 0.032(4) 0.005(4) 0.011(4) 0.006(4) O8 0.044(3) 0.025(3) 0.036(4) -0.009(4) 0.010(4) -0.005(4) O9 0.030(6) 0.0260(17) 0.032(3) 0.000(2) 0.009(5) 0.003(4) O10 0.039(6) 0.024(3) 0.034(3) 0.0004(12) 0.010(5) 0.000(4) O11 0.038(3) 0.031(6) 0.035(3) 0.004(3) 0.008(3) -0.002(4) O12 0.029(6) 0.035(5) 0.036(2) -0.002(5) 0.010(3) 0.003(3) O13 0.028(5) 0.033(6) 0.037(2) -0.004(5) 0.0091(17) -0.002(3) O14 0.037(2) 0.025(6) 0.033(2) 0.001(4) 0.011(3) 0.004(4) O21 0.055(12) 0.071(12) 0.050(13) 0.008(10) 0.006(10) -0.002(9) O22 0.085(14) 0.094(14) 0.024(12) -0.003(10) 0.026(10) 0.000(11) O23 0.081(14) 0.064(13) 0.094(18) 0.017(12) 0.008(12) 0.047(11) O24 0.090(14) 0.054(12) 0.065(15) 0.012(11) 0.021(11) -0.001(11) O31 0.068(10) 0.054(8) 0.036(10) 0.000(7) 0.013(9) 0.017(7) O32 0.053(6) 0.056(10) 0.055(12) -0.013(9) 0.015(8) -0.002(7) O33 0.097(13) 0.052(10) 0.030(5) 0.005(7) 0.026(8) 0.010(9) O34 0.063(10) 0.051(7) 0.059(12) -0.016(7) 0.032(10) -0.007(7) O41 0.052(12) 0.020(11) 0.24(3) -0.008(13) 0.021(15) 0.003(9) O42 0.101(16) 0.088(15) 0.061(15) -0.032(13) 0.035(13) -0.024(13) O43 0.084(13) 0.049(11) 0.068(15) 0.009(11) 0.040(11) -0.016(10) O44 0.042(11) 0.063(12) 0.088(16) -0.009(11) 0.011(10) 0.004(9) O51 0.069(15) 0.15(2) 0.10(2) -0.035(17) 0.014(15) -0.016(15) O52 0.084(15) 0.083(14) 0.096(18) 0.001(13) 0.051(13) 0.016(12) O53 0.106(19) 0.078(17) 0.28(4) -0.06(2) 0.04(2) -0.044(16) O54 0.108(19) 0.14(2) 0.11(2) 0.011(19) 0.036(18) 0.017(17) O61 0.052(12) 0.091(15) 0.094(17) -0.004(13) 0.022(12) 0.008(11) O62 0.056(12) 0.047(11) 0.13(2) 0.030(12) 0.023(12) -0.003(10) O63 0.056(12) 0.059(12) 0.116(19) 0.042(12) 0.043(12) 0.004(10) O64 0.048(11) 0.076(13) 0.070(15) 0.002(11) 0.019(11) 0.006(9) _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 2.176(13) . ? Bi1 O14 2.183(14) . ? Bi1 O13 2.206(14) . ? Bi1 O3 2.500(13) . ? Bi1 O5 2.604(14) . ? Bi1 Bi4 3.5706(15) . ? Bi2 O11 2.179(14) . ? Bi2 O2 2.179(13) . ? Bi2 O12 2.186(15) . ? Bi2 O4 2.543(14) . ? Bi2 O5 2.649(14) . ? Bi2 O2X 2.727(19) . ? Bi2 Bi5 3.5568(15) . ? Bi3 O2 2.173(13) . ? Bi3 O9 2.184(14) . ? Bi3 O10 2.223(14) . ? Bi3 O3 2.537(13) . ? Bi3 O4 2.628(13) . ? Bi3 Bi6 3.5877(15) . ? Bi3 Bi9 3.6988(13) . ? Bi4 O1 2.146(13) . ? Bi4 O14 2.153(14) . ? Bi4 O13 2.204(14) . ? Bi4 O7 2.545(13) . ? Bi4 O6 2.700(14) . ? Bi4 Bi9 3.6941(14) . ? Bi5 O12 2.178(14) . ? Bi5 O11 2.183(15) . ? Bi5 O1 2.225(13) . ? Bi5 O6 2.511(14) . ? Bi5 O5X 2.63(2) . ? Bi5 O8 2.686(14) . ? Bi6 O10 2.161(14) . ? Bi6 O1 2.171(13) . ? Bi6 O9 2.230(14) . ? Bi6 O8 2.456(13) . ? Bi6 O7 2.741(13) . ? Bi6 Bi8 3.6661(13) . ? Bi7 O13 2.078(13) . ? Bi7 O12 2.104(13) . ? Bi7 O5 2.333(16) . ? Bi7 O6 2.346(15) . ? Bi7 O7X 2.742(17) . ? Bi8 O11 2.080(13) . ? Bi8 O10 2.082(13) . ? Bi8 O8 2.290(15) . ? Bi8 O4 2.324(15) . ? Bi9 O9 2.063(13) . ? Bi9 O14 2.100(13) . ? Bi9 O7 2.283(15) . ? Bi9 O3 2.375(15) . ? Bi9 O9X 2.726(18) . ? Cl2 O22 1.419(18) . ? Cl2 O24 1.437(18) . ? Cl2 O23 1.438(18) . ? Cl2 O21 1.446(17) . ? Cl3 O33 1.433(17) . ? Cl3 O31 1.445(16) . ? Cl3 O34 1.452(16) . ? Cl3 O32 1.460(17) . ? Cl4 O41 1.416(17) . ? Cl4 O44 1.446(17) . ? Cl4 O42 1.46(2) . ? Cl4 O43 1.462(19) . ? Cl5 O53 1.27(2) . ? Cl5 O51 1.33(3) . ? Cl5 O52 1.45(2) . ? Cl5 O54 1.50(3) . ? Cl6 O62 1.417(18) . ? Cl6 O63 1.426(17) . ? Cl6 O64 1.45(2) . ? Cl6 O61 1.45(2) . ? O2X C2X 1.57(2) . ? O3 C3A 1.46(2) . ? O4 C4A 1.48(3) . ? O5 C5A 1.54(3) . ? O5X C5X 1.58(2) . ? O6 C6A 1.47(3) . ? O7 C7A 1.46(3) . ? O7X C7X 1.57(2) . ? O8 C8A 1.46(3) . ? O9X C9X 1.57(2) . ? C2X C2Y 1.31(2) . ? C3A C3B 1.50(3) . ? C4A C4B 1.53(4) . ? C5A C5B 1.40(5) . ? C5X C5Y 1.31(2) . ? C6A C6B 1.46(3) . ? C7A C7B 1.35(4) . ? C7X C7Y 1.31(2) . ? C8A C8B 1.55(3) . ? C9X C9Y 1.31(2) . ? O91A C92A 1.61(4) . ? C91A C92A 1.27(5) . ? O92A C94A 1.42(3) . ? C93A C94A 1.45(4) . ? O93B C96B 1.50(3) . ? C95B C96B 1.36(4) . ? O94A C98A 1.38(3) . ? C97A C98A 1.50(4) . ? 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 O14 91.1(5) . . ? O2 Bi1 O13 91.0(5) . . ? O14 Bi1 O13 68.7(5) . . ? O2 Bi1 O3 74.7(5) . . ? O14 Bi1 O3 67.4(5) . . ? O13 Bi1 O3 133.4(5) . . ? O2 Bi1 O5 74.4(4) . . ? O14 Bi1 O5 133.3(5) . . ? O13 Bi1 O5 67.5(5) . . ? O3 Bi1 O5 142.7(5) . . ? O2 Bi1 Bi4 83.6(4) . . ? O14 Bi1 Bi4 34.3(4) . . ? O13 Bi1 Bi4 35.9(3) . . ? O3 Bi1 Bi4 97.7(3) . . ? O5 Bi1 Bi4 99.2(3) . . ? O11 Bi2 O2 90.8(5) . . ? O11 Bi2 O12 69.5(5) . . ? O2 Bi2 O12 89.9(5) . . ? O11 Bi2 O4 67.0(5) . . ? O2 Bi2 O4 74.7(5) . . ? O12 Bi2 O4 133.4(5) . . ? O11 Bi2 O5 132.2(5) . . ? O2 Bi2 O5 73.4(4) . . ? O12 Bi2 O5 65.7(5) . . ? O4 Bi2 O5 142.5(4) . . ? O11 Bi2 O2X 82.8(5) . . ? O2 Bi2 O2X 170.6(6) . . ? O12 Bi2 O2X 81.4(5) . . ? O4 Bi2 O2X 108.7(5) . . ? O5 Bi2 O2X 105.9(5) . . ? O11 Bi2 Bi5 35.4(4) . . ? O2 Bi2 Bi5 83.4(4) . . ? O12 Bi2 Bi5 35.3(4) . . ? O4 Bi2 Bi5 98.4(3) . . ? O5 Bi2 Bi5 97.1(3) . . ? O2X Bi2 Bi5 87.4(4) . . ? O2 Bi3 O9 92.1(5) . . ? O2 Bi3 O10 90.7(5) . . ? O9 Bi3 O10 68.9(5) . . ? O2 Bi3 O3 74.0(5) . . ? O9 Bi3 O3 68.0(5) . . ? O10 Bi3 O3 133.3(5) . . ? O2 Bi3 O4 73.1(4) . . ? O9 Bi3 O4 131.5(5) . . ? O10 Bi3 O4 65.6(5) . . ? O3 Bi3 O4 141.9(4) . . ? O2 Bi3 Bi6 83.4(4) . . ? O9 Bi3 Bi6 36.1(3) . . ? O10 Bi3 Bi6 34.5(4) . . ? O3 Bi3 Bi6 99.1(3) . . ? O4 Bi3 Bi6 95.6(3) . . ? O2 Bi3 Bi9 84.1(3) . . ? O9 Bi3 Bi9 28.5(3) . . ? O10 Bi3 Bi9 96.3(4) . . ? O3 Bi3 Bi9 39.5(3) . . ? O4 Bi3 Bi9 150.1(3) . . ? Bi6 Bi3 Bi9 62.05(3) . . ? O1 Bi4 O14 90.9(5) . . ? O1 Bi4 O13 90.9(5) . . ? O14 Bi4 O13 69.3(5) . . ? O1 Bi4 O7 77.3(5) . . ? O14 Bi4 O7 66.8(5) . . ? O13 Bi4 O7 134.1(5) . . ? O1 Bi4 O6 73.2(5) . . ? O14 Bi4 O6 131.1(5) . . ? O13 Bi4 O6 65.2(5) . . ? O7 Bi4 O6 145.1(4) . . ? O1 Bi4 Bi1 83.4(4) . . ? O14 Bi4 Bi1 34.8(4) . . ? O13 Bi4 Bi1 36.0(4) . . ? O7 Bi4 Bi1 98.3(3) . . ? O6 Bi4 Bi1 96.5(3) . . ? O1 Bi4 Bi9 83.0(4) . . ? O14 Bi4 Bi9 29.3(4) . . ? O13 Bi4 Bi9 97.6(4) . . ? O7 Bi4 Bi9 37.5(3) . . ? O6 Bi4 Bi9 149.8(3) . . ? Bi1 Bi4 Bi9 61.86(4) . . ? O12 Bi5 O11 69.6(5) . . ? O12 Bi5 O1 91.5(5) . . ? O11 Bi5 O1 90.5(5) . . ? O12 Bi5 O6 67.5(5) . . ? O11 Bi5 O6 134.4(5) . . ? O1 Bi5 O6 76.0(5) . . ? O12 Bi5 O5X 76.8(6) . . ? O11 Bi5 O5X 90.0(6) . . ? O1 Bi5 O5X 167.2(6) . . ? O6 Bi5 O5X 94.7(6) . . ? O12 Bi5 O8 131.1(5) . . ? O11 Bi5 O8 65.4(5) . . ? O1 Bi5 O8 71.3(4) . . ? O6 Bi5 O8 141.9(4) . . ? O5X Bi5 O8 120.3(5) . . ? O12 Bi5 Bi2 35.5(4) . . ? O11 Bi5 Bi2 35.3(4) . . ? O1 Bi5 Bi2 84.2(4) . . ? O6 Bi5 Bi2 99.4(3) . . ? O5X Bi5 Bi2 88.9(5) . . ? O8 Bi5 Bi2 96.2(3) . . ? O10 Bi6 O1 92.4(5) . . ? O10 Bi6 O9 69.1(5) . . ? O1 Bi6 O9 89.9(5) . . ? O10 Bi6 O8 67.4(5) . . ? O1 Bi6 O8 76.9(5) . . ? O9 Bi6 O8 133.7(5) . . ? O10 Bi6 O7 131.3(5) . . ? O1 Bi6 O7 72.7(4) . . ? O9 Bi6 O7 64.9(5) . . ? O8 Bi6 O7 144.3(4) . . ? O10 Bi6 Bi3 35.7(4) . . ? O1 Bi6 Bi3 83.1(4) . . ? O9 Bi6 Bi3 35.2(3) . . ? O8 Bi6 Bi3 98.7(3) . . ? O7 Bi6 Bi3 95.8(3) . . ? O10 Bi6 Bi8 29.6(4) . . ? O1 Bi6 Bi8 84.1(4) . . ? O9 Bi6 Bi8 97.5(3) . . ? O8 Bi6 Bi8 37.8(4) . . ? O7 Bi6 Bi8 150.3(3) . . ? Bi3 Bi6 Bi8 62.52(3) . . ? O13 Bi7 O12 88.7(5) . . ? O13 Bi7 O5 75.0(5) . . ? O12 Bi7 O5 73.3(5) . . ? O13 Bi7 O6 74.1(5) . . ? O12 Bi7 O6 71.9(5) . . ? O5 Bi7 O6 133.3(5) . . ? O13 Bi7 O7X 70.9(5) . . ? O12 Bi7 O7X 150.1(5) . . ? O5 Bi7 O7X 80.3(5) . . ? O6 Bi7 O7X 120.1(5) . . ? O11 Bi8 O10 89.8(5) . . ? O11 Bi8 O8 75.0(5) . . ? O10 Bi8 O8 72.0(5) . . ? O11 Bi8 O4 72.9(5) . . ? O10 Bi8 O4 73.7(5) . . ? O8 Bi8 O4 132.4(5) . . ? O11 Bi8 Bi6 81.3(4) . . ? O10 Bi8 Bi6 30.9(4) . . ? O8 Bi8 Bi6 41.1(3) . . ? O4 Bi8 Bi6 99.4(3) . . ? O9 Bi9 O14 88.6(5) . . ? O9 Bi9 O7 76.7(5) . . ? O14 Bi9 O7 72.9(5) . . ? O9 Bi9 O3 73.2(5) . . ? O14 Bi9 O3 71.1(5) . . ? O7 Bi9 O3 133.0(5) . . ? O9 Bi9 O9X 71.0(5) . . ? O14 Bi9 O9X 152.7(5) . . ? O7 Bi9 O9X 84.7(5) . . ? O3 Bi9 O9X 117.3(5) . . ? O9 Bi9 Bi4 81.0(4) . . ? O14 Bi9 Bi4 30.1(4) . . ? O7 Bi9 Bi4 42.8(3) . . ? O3 Bi9 Bi4 96.8(3) . . ? O9X Bi9 Bi4 125.3(4) . . ? O9 Bi9 Bi3 30.4(4) . . ? O14 Bi9 Bi3 80.0(4) . . ? O7 Bi9 Bi3 101.8(3) . . ? O3 Bi9 Bi3 42.8(3) . . ? O9X Bi9 Bi3 90.0(4) . . ? Bi4 Bi9 Bi3 88.08(3) . . ? O22 Cl2 O24 112.5(12) . . ? O22 Cl2 O23 108.1(12) . . ? O24 Cl2 O23 109.0(12) . . ? O22 Cl2 O21 109.1(11) . . ? O24 Cl2 O21 109.6(11) . . ? O23 Cl2 O21 108.4(12) . . ? O33 Cl3 O31 112.3(10) . . ? O33 Cl3 O34 112.5(10) . . ? O31 Cl3 O34 107.1(10) . . ? O33 Cl3 O32 110.3(11) . . ? O31 Cl3 O32 107.4(10) . . ? O34 Cl3 O32 107.0(9) . . ? O41 Cl4 O44 108.3(11) . . ? O41 Cl4 O42 110.4(15) . . ? O44 Cl4 O42 109.6(13) . . ? O41 Cl4 O43 109.2(14) . . ? O44 Cl4 O43 112.0(11) . . ? O42 Cl4 O43 107.3(10) . . ? O53 Cl5 O51 114(2) . . ? O53 Cl5 O52 111.9(16) . . ? O51 Cl5 O52 109.2(15) . . ? O53 Cl5 O54 110(2) . . ? O51 Cl5 O54 102.7(15) . . ? O52 Cl5 O54 109.0(15) . . ? O62 Cl6 O63 109.6(10) . . ? O62 Cl6 O64 108.5(13) . . ? O63 Cl6 O64 109.6(12) . . ? O62 Cl6 O61 108.7(13) . . ? O63 Cl6 O61 109.8(12) . . ? O64 Cl6 O61 110.6(11) . . ? Bi4 O1 Bi6 120.0(6) . . ? Bi4 O1 Bi5 118.6(6) . . ? Bi6 O1 Bi5 117.8(6) . . ? C2X O2X Bi2 112.2(19) . . ? Bi3 O2 Bi1 116.7(6) . . ? Bi3 O2 Bi2 119.1(6) . . ? Bi1 O2 Bi2 120.3(6) . . ? C3A O3 Bi9 123.3(11) . . ? C3A O3 Bi1 117.7(11) . . ? Bi9 O3 Bi1 100.0(5) . . ? C3A O3 Bi3 118.1(12) . . ? Bi9 O3 Bi3 97.7(5) . . ? Bi1 O3 Bi3 94.6(4) . . ? C4A O4 Bi8 119.7(13) . . ? C4A O4 Bi2 115.8(12) . . ? Bi8 O4 Bi2 99.1(5) . . ? C4A O4 Bi3 124.7(13) . . ? Bi8 O4 Bi3 98.8(5) . . ? Bi2 O4 Bi3 93.0(4) . . ? C5A O5 Bi7 122.4(15) . . ? C5A O5 Bi1 116.8(14) . . ? Bi7 O5 Bi1 97.4(5) . . ? C5A O5 Bi2 123.5(15) . . ? Bi7 O5 Bi2 98.1(5) . . ? Bi1 O5 Bi2 91.9(4) . . ? C5X O5X Bi5 108(2) . . ? C6A O6 Bi7 121.8(13) . . ? C6A O6 Bi5 115.9(12) . . ? Bi7 O6 Bi5 99.9(5) . . ? C6A O6 Bi4 124.0(12) . . ? Bi7 O6 Bi4 96.8(5) . . ? Bi5 O6 Bi4 92.3(4) . . ? C7A O7 Bi9 121.9(12) . . ? C7A O7 Bi4 123.2(13) . . ? Bi9 O7 Bi4 99.7(5) . . ? C7A O7 Bi6 118.5(12) . . ? Bi9 O7 Bi6 96.4(5) . . ? Bi4 O7 Bi6 89.9(4) . . ? C7X O7X Bi7 136.4(16) . . ? C8A O8 Bi8 119.9(13) . . ? C8A O8 Bi6 127.7(13) . . ? Bi8 O8 Bi6 101.1(5) . . ? C8A O8 Bi5 110.2(12) . . ? Bi8 O8 Bi5 97.1(5) . . ? Bi6 O8 Bi5 94.0(4) . . ? C9X O9X Bi9 123.5(15) . . ? Bi9 O9 Bi3 121.1(6) . . ? Bi9 O9 Bi6 122.0(7) . . ? Bi3 O9 Bi6 108.7(5) . . ? Bi8 O10 Bi6 119.5(7) . . ? Bi8 O10 Bi3 121.9(7) . . ? Bi6 O10 Bi3 109.8(6) . . ? Bi8 O11 Bi2 120.9(7) . . ? Bi8 O11 Bi5 122.5(7) . . ? Bi2 O11 Bi5 109.3(6) . . ? Bi7 O12 Bi5 120.6(7) . . ? Bi7 O12 Bi2 122.9(7) . . ? Bi5 O12 Bi2 109.2(6) . . ? Bi7 O13 Bi4 124.0(7) . . ? Bi7 O13 Bi1 120.2(7) . . ? Bi4 O13 Bi1 108.1(5) . . ? Bi9 O14 Bi4 120.6(7) . . ? Bi9 O14 Bi1 121.4(7) . . ? Bi4 O14 Bi1 110.9(6) . . ? C2Y C2X O2X 119(4) . . ? O3 C3A C3B 114.1(19) . . ? O4 C4A C4B 110(2) . . ? C5B C5A O5 112(3) . . ? C5Y C5X O5X 107(4) . . ? C6B C6A O6 110.0(19) . . ? C7B C7A O7 119(3) . . ? C7Y C7X O7X 112(3) . . ? O8 C8A C8B 113(2) . . ? C9Y C9X O9X 114(3) . . ? C91A C92A O91A 112(4) . . ? O92A C94A C93A 116(3) . . ? C95B C96B O93B 114(3) . . ? O94A C98A C97A 115(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 20.81 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.003 _refine_diff_density_min -3.077 _refine_diff_density_rms 0.713 #====END # End of Crystallographic Information File