# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Prof Nicolas Mercier' _publ_contact_author_email NICOLAS.MERCIER@UNIV-ANGERS.FR _publ_section_title ; Reversible Dynamic Isomerism Change in Solid State, from Bi4I16 Cluster to BiI4 1D Chain in L-cystin Based Hybrids: Templating Effect of Cations in Iodobismuthate Network Formation ; loop_ _publ_author_name 'Nicolas Mercier' 'Wenhua Bi.' # Attachment 'revisedCif_CC_Mercier.cif' data_1 #(BI4)2-L-Cystin _database_code_depnum_ccdc_archive 'CCDC 695943' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Bi2 I8, C6 H14 N2 O4 S2' _chemical_formula_sum 'C6 H14 Bi2 I8 N2 O4 S2' _chemical_formula_weight 1675.47 _chemical_absolute_configuration syn 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' N N 0.0061 0.0033 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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 'p 21' _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 12.317(3) _cell_length_b 7.763(2) _cell_length_c 15.223(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.07(3) _cell_angle_gamma 90.00 _cell_volume 1453.6(6) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 18746 _cell_measurement_theta_min 3.5 _cell_measurement_theta_max 29.2 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.828 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1436 _exptl_absorpt_coefficient_mu 20.743 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.136 _exptl_absorpt_correction_T_max 0.296 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker KappaCCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 48600 _diffrn_reflns_av_R_equivalents 0.044 _diffrn_reflns_av_sigmaI/netI 0.049 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.1 _diffrn_reflns_theta_max 30.5 _reflns_number_total 8773 _reflns_number_gt 6611 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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^)+(0.0220P)^2^+15.5808P] 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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00026(3) _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 -0.022(5) _refine_ls_number_reflns 8773 _refine_ls_number_parameters 222 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.077 _refine_ls_R_factor_gt 0.044 _refine_ls_wR_factor_ref 0.082 _refine_ls_wR_factor_gt 0.072 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.067 _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 0.78921(3) 0.17886(6) 0.65628(2) 0.02968(10) Uani 1 1 d . . . Bi2 Bi 0.74677(3) 0.68262(6) 0.81631(2) 0.02941(10) Uani 1 1 d . . . I1 I 0.61233(6) 0.01118(10) 0.79309(5) 0.03432(17) Uani 1 1 d . . . I2 I 0.65787(8) 0.03354(13) 0.50150(5) 0.0488(2) Uani 1 1 d . . . I3 I 0.91521(7) -0.15416(11) 0.68428(6) 0.0428(2) Uani 1 1 d . . . I4 I 0.94995(7) 0.34208(14) 0.55719(6) 0.0509(2) Uani 1 1 d . . . I5 I 0.62552(7) 0.49347(11) 0.64396(5) 0.0417(2) Uani 1 1 d . . . I6 I 0.88130(6) 0.34155(10) 0.83804(4) 0.03137(16) Uani 1 1 d . . . I7 I 0.57958(8) 0.56269(15) 0.93413(7) 0.0636(3) Uani 1 1 d . . . I8 I 0.88745(7) 0.80956(12) 0.96296(5) 0.0446(2) Uani 1 1 d . . . S1 S 0.3214(3) 0.9383(4) 0.8325(2) 0.0427(8) Uani 1 1 d . . . S2 S 0.3269(3) 0.8010(4) 0.7186(2) 0.0439(8) Uani 1 1 d . . . O1 O 0.1319(7) 0.5340(12) 0.8010(6) 0.044(2) Uani 1 1 d . . . H1 H 0.1286 0.4341 0.7835 0.053 Uiso 1 1 calc R . . O2 O 0.2992(7) 0.4724(11) 0.8567(5) 0.040(2) Uani 1 1 d . . . O3 O 0.3556(7) 1.2979(11) 0.7170(6) 0.040(2) Uani 1 1 d . . . H3 H 0.3426 1.3543 0.7607 0.049 Uiso 1 1 calc R . . O4 O 0.1751(8) 1.2585(14) 0.7061(7) 0.064(3) Uani 1 1 d . . . N1 N 0.2896(8) 0.6804(16) 0.9892(6) 0.041(2) Uani 1 1 d . . . H1A H 0.3523 0.7027 0.9650 0.062 Uiso 1 1 calc R . . H1B H 0.2911 0.5741 1.0111 0.062 Uiso 1 1 calc R . . H1C H 0.2796 0.7556 1.0321 0.062 Uiso 1 1 calc R . . N2 N 0.3987(10) 1.0886(16) 0.5926(7) 0.055(3) Uani 1 1 d . . . H2A H 0.4264 1.1943 0.5910 0.082 Uiso 1 1 calc R . . H2B H 0.4042 1.0381 0.5406 0.082 Uiso 1 1 calc R . . H2C H 0.4350 1.0273 0.6339 0.082 Uiso 1 1 calc R . . C1 C 0.2139(9) 0.5512(14) 0.8557(7) 0.028(2) Uani 1 1 d . . . C2 C 0.1988(9) 0.6952(17) 0.9210(7) 0.034(2) Uani 1 1 d . . . H2 H 0.1302 0.6758 0.9493 0.041 Uiso 1 1 calc R . . C3 C 0.1946(11) 0.8728(18) 0.8790(8) 0.045(3) Uani 1 1 d . . . H3A H 0.1759 0.9565 0.9230 0.054 Uiso 1 1 calc R . . H3B H 0.1372 0.8741 0.8328 0.054 Uiso 1 1 calc R . . C4 C 0.2407(11) 0.9195(18) 0.6400(8) 0.045(3) Uani 1 1 d . . . H4A H 0.2301 0.8501 0.5873 0.054 Uiso 1 1 calc R . . H4B H 0.1701 0.9342 0.6644 0.054 Uiso 1 1 calc R . . C5 C 0.2826(11) 1.0988(18) 0.6133(7) 0.043(3) Uani 1 1 d . . . H5 H 0.2405 1.1363 0.5602 0.051 Uiso 1 1 calc R . . C6 C 0.2668(11) 1.2282(15) 0.6848(8) 0.037(3) 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 Bi1 0.0312(2) 0.0339(2) 0.02373(18) 0.0019(2) -0.00091(15) -0.0037(2) Bi2 0.0302(2) 0.0314(2) 0.02658(19) 0.0006(2) 0.00089(15) -0.0017(2) I1 0.0270(4) 0.0365(4) 0.0396(4) 0.0043(3) 0.0031(3) 0.0007(3) I2 0.0520(6) 0.0615(6) 0.0320(4) -0.0107(4) -0.0054(4) -0.0153(4) I3 0.0383(5) 0.0410(5) 0.0507(5) 0.0102(4) 0.0188(4) 0.0072(4) I4 0.0381(5) 0.0740(6) 0.0408(4) 0.0186(5) 0.0040(4) -0.0114(5) I5 0.0402(5) 0.0447(5) 0.0388(4) 0.0004(3) -0.0115(4) 0.0059(4) I6 0.0306(4) 0.0351(4) 0.0279(3) -0.0012(3) -0.0033(3) -0.0014(3) I7 0.0362(5) 0.0809(7) 0.0760(7) 0.0429(6) 0.0237(5) 0.0160(5) I8 0.0406(5) 0.0510(5) 0.0411(4) -0.0188(4) -0.0081(4) 0.0068(4) S1 0.054(2) 0.0443(18) 0.0303(15) 0.0015(13) 0.0035(14) -0.0186(15) S2 0.049(2) 0.0440(19) 0.0388(16) -0.0005(13) 0.0057(14) -0.0055(15) O1 0.026(5) 0.044(5) 0.062(6) -0.012(4) 0.000(4) -0.006(4) O2 0.033(5) 0.050(5) 0.037(4) -0.009(4) 0.001(4) 0.001(4) O3 0.038(5) 0.043(5) 0.041(5) -0.002(4) 0.010(4) -0.008(4) O4 0.039(6) 0.076(7) 0.075(7) -0.023(5) -0.006(5) 0.008(5) N1 0.048(6) 0.043(5) 0.032(5) 0.001(5) 0.007(4) -0.001(6) N2 0.068(9) 0.070(8) 0.028(5) 0.001(5) 0.022(5) -0.004(7) C1 0.021(6) 0.031(6) 0.032(6) -0.001(4) 0.004(4) -0.004(4) C2 0.025(6) 0.044(6) 0.035(5) -0.005(6) 0.010(4) -0.004(6) C3 0.045(8) 0.058(9) 0.032(6) 0.005(6) 0.005(5) 0.013(6) C4 0.042(8) 0.062(9) 0.029(6) -0.013(6) -0.007(5) 0.000(6) C5 0.049(8) 0.065(9) 0.015(5) 0.001(5) 0.004(5) 0.009(6) C6 0.039(7) 0.036(7) 0.037(6) -0.001(5) 0.007(5) 0.001(5) _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 I4 2.8497(11) . ? Bi1 I2 3.0055(12) . ? Bi1 I3 3.0338(11) . ? Bi1 I5 3.1663(11) . ? Bi1 I6 3.1940(10) . ? Bi1 I1 3.3564(12) . ? Bi2 I8 2.9229(12) . ? Bi2 I7 2.9531(13) . ? Bi2 I1 3.0514(10) 1_565 ? Bi2 I6 3.1318(10) . ? Bi2 I3 3.2243(12) 1_565 ? Bi2 I5 3.2940(12) . ? I1 Bi2 3.0514(10) 1_545 ? I3 Bi2 3.2243(12) 1_545 ? S1 C3 1.822(14) . ? S1 S2 2.039(5) . ? S2 C4 1.808(14) . ? O1 C1 1.281(13) . ? O1 H1 0.8200 . ? O2 C1 1.216(13) . ? O3 C6 1.293(15) . ? O3 H3 0.8200 . ? O4 C6 1.215(15) . ? N1 C2 1.489(14) . ? N1 H1A 0.8900 . ? N1 H1B 0.8900 . ? N1 H1C 0.8900 . ? N2 C5 1.482(17) . ? N2 H2A 0.8900 . ? N2 H2B 0.8900 . ? N2 H2C 0.8900 . ? C1 C2 1.514(16) . ? C2 C3 1.519(18) . ? C2 H2 0.9800 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.55(2) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.502(17) . ? C5 H5 0.9800 . ? 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 I4 Bi1 I2 96.43(3) . . ? I4 Bi1 I3 95.09(3) . . ? I2 Bi1 I3 92.29(3) . . ? I4 Bi1 I5 94.81(3) . . ? I2 Bi1 I5 85.92(3) . . ? I3 Bi1 I5 170.08(3) . . ? I4 Bi1 I6 93.34(3) . . ? I2 Bi1 I6 168.19(3) . . ? I3 Bi1 I6 93.44(3) . . ? I5 Bi1 I6 86.66(3) . . ? I4 Bi1 I1 173.42(3) . . ? I2 Bi1 I1 90.05(3) . . ? I3 Bi1 I1 85.78(3) . . ? I5 Bi1 I1 84.46(3) . . ? I6 Bi1 I1 80.09(3) . . ? I8 Bi2 I7 92.67(4) . . ? I8 Bi2 I1 95.88(3) . 1_565 ? I7 Bi2 I1 86.69(3) . 1_565 ? I8 Bi2 I6 85.17(3) . . ? I7 Bi2 I6 92.95(3) . . ? I1 Bi2 I6 178.91(3) 1_565 . ? I8 Bi2 I3 88.21(3) . 1_565 ? I7 Bi2 I3 174.53(3) . 1_565 ? I1 Bi2 I3 87.85(3) 1_565 1_565 ? I6 Bi2 I3 92.51(3) . 1_565 ? I8 Bi2 I5 169.61(3) . . ? I7 Bi2 I5 92.41(4) . . ? I1 Bi2 I5 93.46(3) 1_565 . ? I6 Bi2 I5 85.52(3) . . ? I3 Bi2 I5 87.60(3) 1_565 . ? Bi2 I1 Bi1 91.71(3) 1_545 . ? Bi1 I3 Bi2 94.66(3) . 1_545 ? Bi1 I5 Bi2 92.10(3) . . ? Bi2 I6 Bi1 94.68(3) . . ? C3 S1 S2 104.6(5) . . ? C4 S2 S1 104.6(5) . . ? C1 O1 H1 109.5 . . ? C6 O3 H3 109.5 . . ? C2 N1 H1A 109.5 . . ? C2 N1 H1B 109.5 . . ? H1A N1 H1B 109.5 . . ? C2 N1 H1C 109.5 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? C5 N2 H2A 109.5 . . ? C5 N2 H2B 109.5 . . ? H2A N2 H2B 109.5 . . ? C5 N2 H2C 109.5 . . ? H2A N2 H2C 109.5 . . ? H2B N2 H2C 109.5 . . ? O2 C1 O1 127.3(11) . . ? O2 C1 C2 120.0(10) . . ? O1 C1 C2 112.6(10) . . ? N1 C2 C1 106.7(10) . . ? N1 C2 C3 111.8(11) . . ? C1 C2 C3 113.4(9) . . ? N1 C2 H2 108.3 . . ? C1 C2 H2 108.3 . . ? C3 C2 H2 108.3 . . ? C2 C3 S1 114.0(9) . . ? C2 C3 H3A 108.8 . . ? S1 C3 H3A 108.8 . . ? C2 C3 H3B 108.8 . . ? S1 C3 H3B 108.8 . . ? H3A C3 H3B 107.7 . . ? C5 C4 S2 116.1(9) . . ? C5 C4 H4A 108.3 . . ? S2 C4 H4A 108.3 . . ? C5 C4 H4B 108.3 . . ? S2 C4 H4B 108.3 . . ? H4A C4 H4B 107.4 . . ? N2 C5 C6 110.7(11) . . ? N2 C5 C4 110.3(11) . . ? C6 C5 C4 110.7(10) . . ? N2 C5 H5 108.3 . . ? C6 C5 H5 108.3 . . ? C4 C5 H5 108.3 . . ? O4 C6 O3 126.7(12) . . ? O4 C6 C5 118.8(12) . . ? O3 C6 C5 114.5(12) . . ? 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 I2 Bi1 I1 Bi2 92.46(3) . . . 1_545 ? I3 Bi1 I1 Bi2 0.16(3) . . . 1_545 ? I5 Bi1 I1 Bi2 178.36(2) . . . 1_545 ? I6 Bi1 I1 Bi2 -94.08(3) . . . 1_545 ? I4 Bi1 I3 Bi2 173.30(3) . . . 1_545 ? I2 Bi1 I3 Bi2 -90.04(3) . . . 1_545 ? I6 Bi1 I3 Bi2 79.64(3) . . . 1_545 ? I1 Bi1 I3 Bi2 -0.15(3) . . . 1_545 ? I4 Bi1 I5 Bi2 -85.51(3) . . . . ? I2 Bi1 I5 Bi2 178.36(3) . . . . ? I6 Bi1 I5 Bi2 7.56(2) . . . . ? I1 Bi1 I5 Bi2 87.92(3) . . . . ? I8 Bi2 I5 Bi1 18.70(17) . . . . ? I7 Bi2 I5 Bi1 -100.49(3) . . . . ? I1 Bi2 I5 Bi1 172.69(2) 1_565 . . . ? I6 Bi2 I5 Bi1 -7.72(2) . . . . ? I3 Bi2 I5 Bi1 84.98(3) 1_565 . . . ? I8 Bi2 I6 Bi1 -167.71(3) . . . . ? I7 Bi2 I6 Bi1 99.86(4) . . . . ? I3 Bi2 I6 Bi1 -79.72(3) 1_565 . . . ? I5 Bi2 I6 Bi1 7.67(2) . . . . ? I4 Bi1 I6 Bi2 86.66(3) . . . . ? I2 Bi1 I6 Bi2 -59.12(15) . . . . ? I3 Bi1 I6 Bi2 -178.03(2) . . . . ? I5 Bi1 I6 Bi2 -7.97(2) . . . . ? I1 Bi1 I6 Bi2 -92.93(3) . . . . ? C3 S1 S2 C4 80.8(7) . . . . ? O2 C1 C2 N1 -13.3(15) . . . . ? O1 C1 C2 N1 170.2(9) . . . . ? O2 C1 C2 C3 110.1(13) . . . . ? O1 C1 C2 C3 -66.4(13) . . . . ? N1 C2 C3 S1 55.1(12) . . . . ? C1 C2 C3 S1 -65.5(12) . . . . ? S2 S1 C3 C2 75.5(9) . . . . ? S1 S2 C4 C5 67.7(10) . . . . ? S2 C4 C5 N2 46.7(12) . . . . ? S2 C4 C5 C6 -76.2(13) . . . . ? N2 C5 C6 O4 176.1(12) . . . . ? C4 C5 C6 O4 -61.2(16) . . . . ? N2 C5 C6 O3 -3.2(15) . . . . ? C4 C5 C6 O3 119.4(12) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 O4 0.82 1.91 2.651(14) 149.7 1_545 O3 H3 O2 0.82 1.83 2.645(12) 174.1 1_565 N1 H1A S1 0.89 2.73 3.155(11) 110.2 . N1 H1A I7 0.89 3.06 3.823(10) 144.6 . N1 H1B I8 0.89 3.05 3.707(11) 132.2 2_647 N1 H1B I1 0.89 3.19 3.707(9) 119.5 2_657 N1 H1C I6 0.89 2.95 3.675(10) 139.9 2_657 N1 H1C I7 0.89 2.98 3.545(12) 123.3 2_657 N2 H2A I2 0.89 3.14 3.790(13) 132.0 2_666 N2 H2B I5 0.89 2.83 3.673(11) 157.5 2_656 N2 H2C S2 0.89 2.59 3.103(12) 117.5 . N2 H2C I1 0.89 3.18 3.967(12) 149.3 1_565 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 30.5 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.46 _refine_diff_density_min -1.33 _refine_diff_density_rms 0.258 #===END data_2 #Bi4I16(L-Cystin)2-6H2O _database_code_depnum_ccdc_archive 'CCDC 695944' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C6 H14 N2 O4 S2), Bi4 I16, 6(H2 O)' _chemical_formula_sum 'C12 H40 Bi4 I16 N4 O14 S4' _chemical_formula_weight 3459.08 _chemical_absolute_configuration syn 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' N N 0.0061 0.0033 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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 'P 21' _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.280(2) _cell_length_b 20.396(4) _cell_length_c 14.375(3) _cell_angle_alpha 90.00 _cell_angle_beta 101.79(3) _cell_angle_gamma 90.00 _cell_volume 3237.4(11) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 32732 _cell_measurement_theta_min 3.7 _cell_measurement_theta_max 27.6 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.549 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2992 _exptl_absorpt_coefficient_mu 18.639 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.182 _exptl_absorpt_correction_T_max 0.689 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker KappaCCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 93175 _diffrn_reflns_av_R_equivalents 0.0547 _diffrn_reflns_av_sigmaI/netI 0.0525 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.90 _diffrn_reflns_theta_max 28.28 _reflns_number_total 15908 _reflns_number_gt 11952 _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. The H atoms on water molecules cannot be located in the difference map. ; _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^)+(0.0068P)^2^+14.9406P] 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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.000303(7) _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 -0.026(3) _refine_ls_number_reflns 15908 _refine_ls_number_parameters 496 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0716 _refine_ls_R_factor_gt 0.038 _refine_ls_wR_factor_ref 0.054 _refine_ls_wR_factor_gt 0.046 _refine_ls_goodness_of_fit_ref 1.059 _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 0.76843(3) 0.37173(2) 0.94524(3) 0.03152(10) Uani 1 1 d . . . Bi2 Bi 0.39837(3) 0.37432(2) 0.72612(3) 0.02839(10) Uani 1 1 d . . . Bi3 Bi 0.61827(3) 0.17021(2) 0.78279(3) 0.02844(10) Uani 1 1 d . . . Bi4 Bi 0.25556(3) 0.17358(2) 0.55740(3) 0.03027(10) Uani 1 1 d . . . I1 I 0.99501(7) 0.43658(5) 0.92797(7) 0.0562(3) Uani 1 1 d . . . I2 I 0.68074(7) 0.47505(5) 1.04733(6) 0.0515(2) Uani 1 1 d . . . I3 I 0.89222(8) 0.30128(5) 1.11933(7) 0.0582(2) Uani 1 1 d . . . I4 I 0.85743(6) 0.24945(4) 0.81148(6) 0.0433(2) Uani 1 1 d . . . I5 I 0.65043(6) 0.43850(5) 0.74513(6) 0.0432(2) Uani 1 1 d . . . I6 I 0.52068(6) 0.28052(4) 0.91799(6) 0.03707(19) Uani 1 1 d . . . I7 I 0.71254(8) 0.08410(5) 0.94154(6) 0.0517(2) Uani 1 1 d . . . I8 I 0.31355(7) 0.46200(4) 0.85651(6) 0.0425(2) Uani 1 1 d . . . I9 I 0.30792(8) 0.45901(5) 0.56511(6) 0.0550(2) Uani 1 1 d . . . I10 I 0.16330(6) 0.29245(4) 0.69772(6) 0.0435(2) Uani 1 1 d . . . I11 I 0.70297(7) 0.08555(4) 0.64587(6) 0.0427(2) Uani 1 1 d . . . I12 I 0.37113(6) 0.10285(4) 0.76003(6) 0.0429(2) Uani 1 1 d . . . I13 I 0.50016(6) 0.26299(4) 0.59437(5) 0.03380(18) Uani 1 1 d . . . I14 I 0.14859(8) 0.24793(5) 0.38716(6) 0.0539(2) Uani 1 1 d . . . I15 I 0.35231(7) 0.07520(4) 0.45280(6) 0.0467(2) Uani 1 1 d . . . I16 I 0.02775(6) 0.10454(5) 0.56927(7) 0.0510(2) Uani 1 1 d . . . S1 S 0.6386(3) 0.39042(17) 0.4344(3) 0.0582(9) Uani 1 1 d . . . S2 S 0.5565(3) 0.35498(15) 0.3057(3) 0.0678(10) Uani 1 1 d . . . S3 S 0.6369(2) 0.68428(16) 0.8933(2) 0.0527(8) Uani 1 1 d . . . S4 S 0.5346(2) 0.60197(14) 0.86583(19) 0.0439(6) Uani 1 1 d . . . O1 O 1.0634(7) 0.4172(5) 0.3646(7) 0.055(3) Uani 1 1 d . . . O2 O 0.9031(8) 0.4586(6) 0.2652(6) 0.065(3) Uani 1 1 d . . . H2 H 0.9498 0.4643 0.2290 0.078 Uiso 1 1 calc R . . O3 O 0.3214(10) 0.3721(6) 0.0830(7) 0.083(3) Uani 1 1 d . . . H3 H 0.2866 0.3443 0.0461 0.100 Uiso 1 1 calc R . . O4 O 0.2268(9) 0.3241(6) 0.1834(7) 0.077(3) Uani 1 1 d . . . O5 O 1.0564(7) 0.6257(5) 0.8635(7) 0.058(3) Uani 1 1 d . . . O6 O 0.9118(7) 0.5763(5) 0.7571(7) 0.058(3) Uani 1 1 d . . . H6 H 0.9672 0.5675 0.7300 0.070 Uiso 1 1 calc R . . O7 O 0.3427(8) 0.7009(5) 0.5954(6) 0.068(3) Uani 1 1 d . . . H7 H 0.3222 0.7318 0.5592 0.081 Uiso 1 1 calc R . . O8 O 0.1868(8) 0.7254(6) 0.6549(7) 0.084(4) Uani 1 1 d . . . O9 O 0.8134(8) 0.7845(5) 0.0430(6) 0.070(3) Uani 1 1 d . . . O10 O 0.8949(9) 0.0690(6) 0.3265(7) 0.076(3) Uani 1 1 d . . . O11 O 0.8237(7) 0.2473(5) 0.5552(6) 0.052(2) Uani 1 1 d . . . O12 O 0.9388(13) 0.4286(8) 0.6409(10) 0.129(5) Uani 1 1 d . . . O13 O 0.0734(17) 0.1078(11) 0.8425(10) 0.193(10) Uani 1 1 d . . . O14 O -0.0705(10) -0.0115(9) 0.8318(9) 0.135(6) Uani 1 1 d . . . N1 N 0.9276(8) 0.3550(5) 0.4662(8) 0.057(3) Uani 1 1 d . . . H1A H 0.9924 0.3348 0.4534 0.086 Uiso 1 1 calc R . . H1B H 0.8784 0.3256 0.4840 0.086 Uiso 1 1 calc R . . H1C H 0.9509 0.3838 0.5130 0.086 Uiso 1 1 calc R . . N2 N 0.2981(8) 0.4077(5) 0.3209(7) 0.054(3) Uani 1 1 d . . . H2A H 0.2192 0.4163 0.3116 0.082 Uiso 1 1 calc R . . H2B H 0.3381 0.4338 0.3663 0.082 Uiso 1 1 calc R . . H2C H 0.3111 0.3660 0.3384 0.082 Uiso 1 1 calc R . . N3 N 0.9174(9) 0.6605(7) 0.9784(8) 0.084(4) Uani 1 1 d . . . H3A H 0.8821 0.6994 0.9800 0.126 Uiso 1 1 calc R . . H3B H 0.9955 0.6662 0.9777 0.126 Uiso 1 1 calc R . . H3C H 0.9104 0.6374 1.0296 0.126 Uiso 1 1 calc R . . N4 N 0.2718(8) 0.6609(6) 0.8179(7) 0.059(3) Uani 1 1 d . . . H4A H 0.2150 0.6344 0.7860 0.089 Uiso 1 1 calc R . . H4B H 0.2373 0.6969 0.8350 0.089 Uiso 1 1 calc R . . H4C H 0.3118 0.6404 0.8695 0.089 Uiso 1 1 calc R . . C1 C 0.9563(11) 0.4237(6) 0.3376(9) 0.042(3) Uani 1 1 d . . . C2 C 0.8643(9) 0.3891(5) 0.3819(8) 0.038(3) Uani 1 1 d . . . H2D H 0.8246 0.3560 0.3367 0.046 Uiso 1 1 calc R . . C3 C 0.7664(9) 0.4336(5) 0.4054(9) 0.049(3) Uani 1 1 d . . . H3D H 0.7374 0.4620 0.3515 0.059 Uiso 1 1 calc R . . H3E H 0.8020 0.4612 0.4588 0.059 Uiso 1 1 calc R . . C4 C 0.4779(10) 0.4253(7) 0.2494(10) 0.056(4) Uani 1 1 d . . . H4D H 0.5028 0.4636 0.2887 0.067 Uiso 1 1 calc R . . H4E H 0.5013 0.4323 0.1889 0.067 Uiso 1 1 calc R . . C5 C 0.3406(9) 0.4192(5) 0.2325(7) 0.041(3) Uani 1 1 d . . . H5 H 0.3061 0.4609 0.2062 0.050 Uiso 1 1 calc R . . C6 C 0.2895(10) 0.3664(6) 0.1635(8) 0.042(3) Uani 1 1 d . . . C7 C 0.9547(10) 0.6076(7) 0.8354(10) 0.046(3) Uani 1 1 d . . . C8 C 0.8571(9) 0.6241(6) 0.8904(8) 0.046(3) Uani 1 1 d . . . H8 H 0.8208 0.5835 0.9084 0.056 Uiso 1 1 calc R . . C9 C 0.7597(8) 0.6674(5) 0.8342(8) 0.045(3) Uani 1 1 d . . . H9A H 0.7273 0.6464 0.7737 0.054 Uiso 1 1 calc R . . H9B H 0.7960 0.7086 0.8210 0.054 Uiso 1 1 calc R . . C10 C 0.4428(9) 0.6223(6) 0.7494(8) 0.037(3) Uani 1 1 d . . . H10A H 0.4956 0.6335 0.7063 0.045 Uiso 1 1 calc R . . H10B H 0.3955 0.5843 0.7238 0.045 Uiso 1 1 calc R . . C11 C 0.3585(8) 0.6792(5) 0.7557(7) 0.039(2) Uani 1 1 d . . . H11 H 0.4076 0.7161 0.7856 0.047 Uiso 1 1 calc R . . C12 C 0.2847(9) 0.7026(6) 0.6607(8) 0.037(3) 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 Bi1 0.0314(2) 0.0290(3) 0.0336(2) -0.0004(2) 0.00537(16) -0.00220(18) Bi2 0.02965(19) 0.0265(2) 0.0292(2) -0.0013(2) 0.00651(15) 0.00087(18) Bi3 0.03030(19) 0.0252(2) 0.0296(2) 0.0000(2) 0.00572(15) 0.00126(18) Bi4 0.0331(2) 0.0266(2) 0.0315(2) -0.0003(2) 0.00765(16) -0.00072(18) I1 0.0362(4) 0.0530(6) 0.0793(7) 0.0152(5) 0.0117(4) -0.0099(4) I2 0.0642(5) 0.0480(6) 0.0404(5) -0.0077(4) 0.0060(4) 0.0173(4) I3 0.0740(6) 0.0460(6) 0.0481(5) 0.0119(4) -0.0025(4) 0.0055(4) I4 0.0324(4) 0.0496(6) 0.0493(5) -0.0136(4) 0.0115(3) -0.0077(3) I5 0.0377(4) 0.0490(6) 0.0414(5) 0.0131(4) 0.0049(3) -0.0086(3) I6 0.0376(4) 0.0349(5) 0.0426(5) -0.0021(4) 0.0174(3) -0.0030(3) I7 0.0737(5) 0.0510(6) 0.0288(4) 0.0084(4) 0.0067(4) 0.0177(4) I8 0.0560(5) 0.0363(5) 0.0411(5) -0.0078(4) 0.0235(4) -0.0004(4) I9 0.0780(6) 0.0560(7) 0.0288(4) 0.0082(4) 0.0059(4) 0.0190(5) I10 0.0341(4) 0.0479(6) 0.0505(5) -0.0148(4) 0.0136(3) -0.0078(3) I11 0.0585(5) 0.0327(5) 0.0417(5) -0.0047(4) 0.0219(4) 0.0029(4) I12 0.0387(4) 0.0415(5) 0.0469(5) 0.0135(4) 0.0052(3) -0.0089(3) I13 0.0356(4) 0.0300(5) 0.0392(4) -0.0014(3) 0.0159(3) -0.0016(3) I14 0.0793(6) 0.0439(6) 0.0399(5) 0.0123(4) 0.0152(4) 0.0214(4) I15 0.0576(5) 0.0378(5) 0.0487(5) -0.0059(4) 0.0201(4) 0.0074(4) I16 0.0365(4) 0.0521(6) 0.0645(6) 0.0084(5) 0.0106(4) -0.0099(4) S1 0.0400(16) 0.056(2) 0.081(2) 0.0094(18) 0.0196(16) 0.0023(14) S2 0.0382(16) 0.0387(18) 0.120(3) -0.0182(18) 0.0005(18) 0.0018(13) S3 0.0376(15) 0.056(2) 0.064(2) -0.0146(16) 0.0102(14) 0.0002(13) S4 0.0388(15) 0.0416(16) 0.0509(16) 0.0125(13) 0.0085(12) 0.0053(12) O1 0.033(5) 0.062(7) 0.067(6) 0.008(5) 0.001(4) 0.000(4) O2 0.060(5) 0.086(8) 0.044(6) 0.006(5) 0.000(4) 0.006(5) O3 0.123(8) 0.084(9) 0.047(6) -0.005(5) 0.028(6) -0.045(7) O4 0.100(7) 0.080(8) 0.056(6) -0.010(5) 0.026(5) -0.037(6) O5 0.029(4) 0.073(8) 0.070(7) -0.003(6) 0.006(4) 0.000(4) O6 0.043(5) 0.072(7) 0.059(6) -0.011(5) 0.007(4) 0.008(5) O7 0.069(6) 0.087(8) 0.055(6) 0.032(5) 0.028(5) 0.027(5) O8 0.057(6) 0.142(11) 0.058(6) 0.029(6) 0.024(5) 0.036(6) O9 0.073(6) 0.081(8) 0.047(6) -0.007(5) -0.010(4) 0.000(5) O10 0.096(7) 0.071(7) 0.062(6) 0.016(5) 0.019(5) -0.019(6) O11 0.060(5) 0.049(6) 0.045(5) 0.004(4) 0.004(4) -0.013(4) O12 0.162(12) 0.145(13) 0.097(9) 0.011(9) 0.061(9) 0.060(10) O13 0.266(19) 0.25(2) 0.080(10) 0.025(12) 0.068(11) 0.153(17) O14 0.099(8) 0.220(18) 0.086(9) -0.016(10) 0.019(7) 0.055(10) N1 0.033(5) 0.054(7) 0.085(8) 0.010(6) 0.014(5) 0.008(4) N2 0.049(6) 0.064(8) 0.056(7) -0.011(6) 0.023(5) -0.008(5) N3 0.053(6) 0.137(14) 0.058(7) -0.012(8) 0.004(5) 0.013(7) N4 0.047(6) 0.085(9) 0.050(6) 0.018(6) 0.020(5) 0.014(6) C1 0.052(7) 0.029(7) 0.047(8) -0.012(6) 0.009(6) -0.001(5) C2 0.038(6) 0.029(7) 0.044(6) -0.005(5) -0.002(5) -0.001(5) C3 0.045(6) 0.023(6) 0.077(8) 0.000(6) 0.009(6) 0.007(5) C4 0.044(7) 0.041(8) 0.082(10) 0.001(7) 0.013(7) -0.013(6) C5 0.050(7) 0.040(7) 0.034(6) -0.006(5) 0.008(5) -0.006(5) C6 0.054(7) 0.029(7) 0.046(7) 0.012(6) 0.016(5) -0.004(5) C7 0.034(6) 0.049(8) 0.051(8) 0.011(7) -0.003(6) 0.009(5) C8 0.038(6) 0.051(8) 0.048(7) 0.008(6) 0.004(5) 0.004(5) C9 0.033(5) 0.044(7) 0.059(7) 0.014(6) 0.010(5) 0.003(5) C10 0.034(6) 0.029(7) 0.048(7) -0.006(5) 0.008(5) -0.003(5) C11 0.040(6) 0.039(7) 0.041(6) 0.002(5) 0.017(5) -0.002(5) C12 0.028(6) 0.038(7) 0.048(7) -0.001(5) 0.012(5) 0.011(5) _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 I2 2.8577(11) . ? Bi1 I1 2.9330(10) . ? Bi1 I3 2.9745(12) . ? Bi1 I5 3.2149(12) . ? Bi1 I6 3.3131(10) . ? Bi1 I4 3.4226(11) . ? Bi2 I8 2.8914(10) . ? Bi2 I9 2.9011(11) . ? Bi2 I10 3.0891(10) . ? Bi2 I5 3.0910(10) . ? Bi2 I13 3.3091(10) . ? Bi2 I6 3.4080(12) . ? Bi3 I7 2.9036(11) . ? Bi3 I11 2.9218(10) . ? Bi3 I12 3.0648(10) . ? Bi3 I4 3.0991(10) . ? Bi3 I6 3.3054(10) . ? Bi3 I13 3.3492(11) . ? Bi4 I15 2.8547(10) . ? Bi4 I14 2.9219(11) . ? Bi4 I16 2.9654(10) . ? Bi4 I13 3.2590(10) . ? Bi4 I12 3.2729(12) . ? Bi4 I10 3.4480(10) . ? S1 C3 1.809(11) . ? S1 S2 2.025(5) . ? S2 C4 1.791(13) . ? S3 C9 1.801(10) . ? S3 S4 2.029(4) . ? S4 C10 1.827(11) . ? O1 C1 1.198(13) . ? O2 C1 1.302(15) . ? O2 H2 0.8200 . ? O3 C6 1.285(14) . ? O3 H3 0.8200 . ? O4 C6 1.187(13) . ? O5 C7 1.194(13) . ? O6 C7 1.298(15) . ? O6 H6 0.8200 . ? O7 C12 1.249(13) . ? O7 H7 0.8200 . ? O8 C12 1.185(12) . ? N1 C2 1.452(14) . ? N1 H1A 0.8900 . ? N1 H1B 0.8900 . ? N1 H1C 0.8900 . ? N2 C5 1.465(13) . ? N2 H2A 0.8900 . ? N2 H2B 0.8900 . ? N2 H2C 0.8900 . ? N3 C8 1.504(15) . ? N3 H3A 0.8900 . ? N3 H3B 0.8900 . ? N3 H3C 0.8900 . ? N4 C11 1.500(12) . ? N4 H4A 0.8900 . ? N4 H4B 0.8900 . ? N4 H4C 0.8900 . ? C1 C2 1.500(16) . ? C2 C3 1.520(14) . ? C2 H2D 0.9800 . ? C3 H3D 0.9700 . ? C3 H3E 0.9700 . ? C4 C5 1.523(14) . ? C4 H4D 0.9700 . ? C4 H4E 0.9700 . ? C5 C6 1.498(15) . ? C5 H5 0.9800 . ? C7 C8 1.519(17) . ? C8 C9 1.509(14) . ? C8 H8 0.9800 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.515(14) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.524(14) . ? C11 H11 0.9800 . ? 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 I2 Bi1 I1 96.31(4) . . ? I2 Bi1 I3 94.38(3) . . ? I1 Bi1 I3 91.25(4) . . ? I2 Bi1 I5 91.35(3) . . ? I1 Bi1 I5 86.66(4) . . ? I3 Bi1 I5 174.08(3) . . ? I2 Bi1 I6 95.90(3) . . ? I1 Bi1 I6 166.35(3) . . ? I3 Bi1 I6 93.89(4) . . ? I5 Bi1 I6 86.97(3) . . ? I2 Bi1 I4 176.31(3) . . ? I1 Bi1 I4 85.43(3) . . ? I3 Bi1 I4 88.83(3) . . ? I5 Bi1 I4 85.49(3) . . ? I6 Bi1 I4 82.04(3) . . ? I8 Bi2 I9 92.28(3) . . ? I8 Bi2 I10 91.79(3) . . ? I9 Bi2 I10 93.67(4) . . ? I8 Bi2 I5 95.79(3) . . ? I9 Bi2 I5 89.17(4) . . ? I10 Bi2 I5 171.79(3) . . ? I8 Bi2 I13 174.24(3) . . ? I9 Bi2 I13 93.36(3) . . ? I10 Bi2 I13 86.69(3) . . ? I5 Bi2 I13 85.45(3) . . ? I8 Bi2 I6 87.45(3) . . ? I9 Bi2 I6 176.44(3) . . ? I10 Bi2 I6 89.89(3) . . ? I5 Bi2 I6 87.32(3) . . ? I13 Bi2 I6 86.99(3) . . ? I7 Bi3 I11 93.11(3) . . ? I7 Bi3 I12 89.53(4) . . ? I11 Bi3 I12 94.52(3) . . ? I7 Bi3 I4 92.40(4) . . ? I11 Bi3 I4 90.13(3) . . ? I12 Bi3 I4 174.87(3) . . ? I7 Bi3 I6 93.56(3) . . ? I11 Bi3 I6 172.93(3) . . ? I12 Bi3 I6 87.88(3) . . ? I4 Bi3 I6 87.26(3) . . ? I7 Bi3 I13 176.96(3) . . ? I11 Bi3 I13 85.41(3) . . ? I12 Bi3 I13 87.95(3) . . ? I4 Bi3 I13 90.26(3) . . ? I6 Bi3 I13 88.03(3) . . ? I15 Bi4 I14 93.47(3) . . ? I15 Bi4 I16 97.21(3) . . ? I14 Bi4 I16 94.61(4) . . ? I15 Bi4 I13 94.43(3) . . ? I14 Bi4 I13 92.12(4) . . ? I16 Bi4 I13 166.16(3) . . ? I15 Bi4 I12 91.91(3) . . ? I14 Bi4 I12 174.44(3) . . ? I16 Bi4 I12 86.08(3) . . ? I13 Bi4 I12 86.08(3) . . ? Bi3 I4 Bi1 96.17(3) . . ? Bi2 I5 Bi1 96.02(4) . . ? Bi3 I6 Bi1 94.45(3) . . ? Bi3 I6 Bi2 91.99(3) . . ? Bi1 I6 Bi2 88.43(3) . . ? Bi3 I12 Bi4 94.91(3) . . ? Bi4 I13 Bi2 95.51(3) . . ? Bi4 I13 Bi3 89.96(3) . . ? Bi2 I13 Bi3 92.99(3) . . ? C3 S1 S2 101.6(4) . . ? C4 S2 S1 102.6(5) . . ? C9 S3 S4 102.2(4) . . ? C10 S4 S3 100.6(4) . . ? C1 O2 H2 109.5 . . ? C6 O3 H3 109.5 . . ? C7 O6 H6 109.5 . . ? C12 O7 H7 109.5 . . ? C2 N1 H1A 109.5 . . ? C2 N1 H1B 109.5 . . ? H1A N1 H1B 109.5 . . ? C2 N1 H1C 109.5 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? C5 N2 H2A 109.5 . . ? C5 N2 H2B 109.5 . . ? H2A N2 H2B 109.5 . . ? C5 N2 H2C 109.5 . . ? H2A N2 H2C 109.5 . . ? H2B N2 H2C 109.5 . . ? C8 N3 H3A 109.5 . . ? C8 N3 H3B 109.5 . . ? H3A N3 H3B 109.5 . . ? C8 N3 H3C 109.5 . . ? H3A N3 H3C 109.5 . . ? H3B N3 H3C 109.5 . . ? C11 N4 H4A 109.5 . . ? C11 N4 H4B 109.5 . . ? H4A N4 H4B 109.5 . . ? C11 N4 H4C 109.5 . . ? H4A N4 H4C 109.5 . . ? H4B N4 H4C 109.5 . . ? O1 C1 O2 126.1(13) . . ? O1 C1 C2 123.3(12) . . ? O2 C1 C2 110.6(10) . . ? N1 C2 C1 108.4(9) . . ? N1 C2 C3 110.8(9) . . ? C1 C2 C3 114.2(9) . . ? N1 C2 H2D 107.7 . . ? C1 C2 H2D 107.7 . . ? C3 C2 H2D 107.7 . . ? C2 C3 S1 114.2(7) . . ? C2 C3 H3D 108.7 . . ? S1 C3 H3D 108.7 . . ? C2 C3 H3E 108.7 . . ? S1 C3 H3E 108.7 . . ? H3D C3 H3E 107.6 . . ? C5 C4 S2 113.5(8) . . ? C5 C4 H4D 108.9 . . ? S2 C4 H4D 108.9 . . ? C5 C4 H4E 108.9 . . ? S2 C4 H4E 108.9 . . ? H4D C4 H4E 107.7 . . ? N2 C5 C6 108.0(9) . . ? N2 C5 C4 112.2(9) . . ? C6 C5 C4 114.0(9) . . ? N2 C5 H5 107.5 . . ? C6 C5 H5 107.5 . . ? C4 C5 H5 107.5 . . ? O4 C6 O3 125.0(12) . . ? O4 C6 C5 122.1(11) . . ? O3 C6 C5 113.0(10) . . ? O5 C7 O6 127.4(13) . . ? O5 C7 C8 120.2(13) . . ? O6 C7 C8 112.2(10) . . ? N3 C8 C9 108.5(10) . . ? N3 C8 C7 107.2(9) . . ? C9 C8 C7 112.1(9) . . ? N3 C8 H8 109.7 . . ? C9 C8 H8 109.7 . . ? C7 C8 H8 109.7 . . ? C8 C9 S3 113.9(7) . . ? C8 C9 H9A 108.8 . . ? S3 C9 H9A 108.8 . . ? C8 C9 H9B 108.8 . . ? S3 C9 H9B 108.8 . . ? H9A C9 H9B 107.7 . . ? C11 C10 S4 111.4(8) . . ? C11 C10 H10A 109.4 . . ? S4 C10 H10A 109.4 . . ? C11 C10 H10B 109.4 . . ? S4 C10 H10B 109.4 . . ? H10A C10 H10B 108.0 . . ? N4 C11 C10 109.7(9) . . ? N4 C11 C12 108.0(8) . . ? C10 C11 C12 114.9(9) . . ? N4 C11 H11 108.0 . . ? C10 C11 H11 108.0 . . ? C12 C11 H11 108.0 . . ? O8 C12 O7 125.5(11) . . ? O8 C12 C11 121.1(10) . . ? O7 C12 C11 113.0(9) . . ? 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 I7 Bi3 I4 Bi1 -95.61(3) . . . . ? I11 Bi3 I4 Bi1 171.27(3) . . . . ? I12 Bi3 I4 Bi1 16.4(3) . . . . ? I6 Bi3 I4 Bi1 -2.15(2) . . . . ? I13 Bi3 I4 Bi1 85.86(3) . . . . ? I2 Bi1 I4 Bi3 -54.1(5) . . . . ? I1 Bi1 I4 Bi3 -172.40(3) . . . . ? I3 Bi1 I4 Bi3 96.26(4) . . . . ? I5 Bi1 I4 Bi3 -85.39(3) . . . . ? I6 Bi1 I4 Bi3 2.17(2) . . . . ? I8 Bi2 I5 Bi1 78.50(3) . . . . ? I9 Bi2 I5 Bi1 170.71(3) . . . . ? I10 Bi2 I5 Bi1 -78.93(19) . . . . ? I13 Bi2 I5 Bi1 -95.85(3) . . . . ? I6 Bi2 I5 Bi1 -8.66(3) . . . . ? I2 Bi1 I5 Bi2 -86.92(3) . . . . ? I1 Bi1 I5 Bi2 176.83(3) . . . . ? I3 Bi1 I5 Bi2 107.4(3) . . . . ? I6 Bi1 I5 Bi2 8.91(3) . . . . ? I4 Bi1 I5 Bi2 91.16(3) . . . . ? I7 Bi3 I6 Bi1 94.46(4) . . . . ? I11 Bi3 I6 Bi1 -66.2(2) . . . . ? I12 Bi3 I6 Bi1 -176.15(2) . . . . ? I4 Bi3 I6 Bi1 2.22(2) . . . . ? I13 Bi3 I6 Bi1 -88.13(3) . . . . ? I7 Bi3 I6 Bi2 -176.96(2) . . . . ? I11 Bi3 I6 Bi2 22.4(2) . . . . ? I12 Bi3 I6 Bi2 -87.57(3) . . . . ? I4 Bi3 I6 Bi2 90.80(3) . . . . ? I13 Bi3 I6 Bi2 0.45(2) . . . . ? I2 Bi1 I6 Bi3 174.89(3) . . . . ? I1 Bi1 I6 Bi3 21.56(13) . . . . ? I3 Bi1 I6 Bi3 -90.29(3) . . . . ? I5 Bi1 I6 Bi3 83.84(3) . . . . ? I4 Bi1 I6 Bi3 -2.03(2) . . . . ? I2 Bi1 I6 Bi2 83.01(3) . . . . ? I1 Bi1 I6 Bi2 -70.32(12) . . . . ? I3 Bi1 I6 Bi2 177.83(3) . . . . ? I5 Bi1 I6 Bi2 -8.04(2) . . . . ? I4 Bi1 I6 Bi2 -93.90(3) . . . . ? I8 Bi2 I6 Bi3 178.03(2) . . . . ? I9 Bi2 I6 Bi3 -96.2(4) . . . . ? I10 Bi2 I6 Bi3 86.24(3) . . . . ? I5 Bi2 I6 Bi3 -86.04(3) . . . . ? I13 Bi2 I6 Bi3 -0.46(2) . . . . ? I8 Bi2 I6 Bi1 -87.57(3) . . . . ? I9 Bi2 I6 Bi1 -1.8(5) . . . . ? I10 Bi2 I6 Bi1 -179.36(2) . . . . ? I5 Bi2 I6 Bi1 8.36(2) . . . . ? I13 Bi2 I6 Bi1 93.94(3) . . . . ? I7 Bi3 I12 Bi4 -170.28(3) . . . . ? I11 Bi3 I12 Bi4 -77.19(3) . . . . ? I4 Bi3 I12 Bi4 77.6(3) . . . . ? I6 Bi3 I12 Bi4 96.14(3) . . . . ? I13 Bi3 I12 Bi4 8.03(2) . . . . ? I15 Bi4 I12 Bi3 86.04(3) . . . . ? I14 Bi4 I12 Bi3 -79.5(3) . . . . ? I16 Bi4 I12 Bi3 -176.86(3) . . . . ? I13 Bi4 I12 Bi3 -8.27(2) . . . . ? I15 Bi4 I13 Bi2 -177.08(3) . . . . ? I14 Bi4 I13 Bi2 89.28(3) . . . . ? I16 Bi4 I13 Bi2 -29.83(12) . . . . ? I12 Bi4 I13 Bi2 -85.46(3) . . . . ? I15 Bi4 I13 Bi3 -84.08(3) . . . . ? I14 Bi4 I13 Bi3 -177.73(2) . . . . ? I16 Bi4 I13 Bi3 63.17(12) . . . . ? I12 Bi4 I13 Bi3 7.54(2) . . . . ? I8 Bi2 I13 Bi4 75.5(2) . . . . ? I9 Bi2 I13 Bi4 -92.86(4) . . . . ? I10 Bi2 I13 Bi4 0.63(2) . . . . ? I5 Bi2 I13 Bi4 178.24(2) . . . . ? I6 Bi2 I13 Bi4 90.69(3) . . . . ? I8 Bi2 I13 Bi3 -14.8(2) . . . . ? I9 Bi2 I13 Bi3 176.90(2) . . . . ? I10 Bi2 I13 Bi3 -89.61(3) . . . . ? I5 Bi2 I13 Bi3 88.00(3) . . . . ? I6 Bi2 I13 Bi3 0.45(2) . . . . ? I7 Bi3 I13 Bi4 25.7(5) . . . . ? I11 Bi3 I13 Bi4 86.66(3) . . . . ? I12 Bi3 I13 Bi4 -8.04(2) . . . . ? I4 Bi3 I13 Bi4 176.77(2) . . . . ? I6 Bi3 I13 Bi4 -95.98(3) . . . . ? I7 Bi3 I13 Bi2 121.2(5) . . . . ? I11 Bi3 I13 Bi2 -177.82(2) . . . . ? I12 Bi3 I13 Bi2 87.48(3) . . . . ? I4 Bi3 I13 Bi2 -87.71(3) . . . . ? I6 Bi3 I13 Bi2 -0.46(2) . . . . ? C3 S1 S2 C4 -78.3(5) . . . . ? C9 S3 S4 C10 -85.2(5) . . . . ? O1 C1 C2 N1 6.8(16) . . . . ? O2 C1 C2 N1 -175.7(10) . . . . ? O1 C1 C2 C3 130.9(13) . . . . ? O2 C1 C2 C3 -51.6(14) . . . . ? N1 C2 C3 S1 -70.0(11) . . . . ? C1 C2 C3 S1 167.3(8) . . . . ? S2 S1 C3 C2 -71.7(8) . . . . ? S1 S2 C4 C5 -112.9(8) . . . . ? S2 C4 C5 N2 57.9(12) . . . . ? S2 C4 C5 C6 -65.3(12) . . . . ? N2 C5 C6 O4 -0.6(16) . . . . ? C4 C5 C6 O4 124.8(13) . . . . ? N2 C5 C6 O3 179.9(11) . . . . ? C4 C5 C6 O3 -54.7(14) . . . . ? O5 C7 C8 N3 -2.6(16) . . . . ? O6 C7 C8 N3 -179.5(11) . . . . ? O5 C7 C8 C9 116.3(13) . . . . ? O6 C7 C8 C9 -60.6(15) . . . . ? N3 C8 C9 S3 -65.4(11) . . . . ? C7 C8 C9 S3 176.4(9) . . . . ? S4 S3 C9 C8 -80.8(8) . . . . ? S3 S4 C10 C11 -65.9(8) . . . . ? S4 C10 C11 N4 -62.2(10) . . . . ? S4 C10 C11 C12 175.9(7) . . . . ? N4 C11 C12 O8 26.2(16) . . . . ? C10 C11 C12 O8 149.0(12) . . . . ? N4 C11 C12 O7 -160.4(11) . . . . ? C10 C11 C12 O7 -37.5(14) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.317 _refine_diff_density_min -1.210 _refine_diff_density_rms 0.222 #===END