# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Guo-Cong Guo' _publ_contact_author_address ; Fuzhou Fujian China 350002 ; _publ_contact_author_email gcguo@fjirsm.ac.cn loop_ _publ_author_name 'Gang Xu' 'Guo-Cong Guo' 'Jin-Shuang Guo' 'Sheng-Ping Guo' ; Xiao-Ming Jiang ; 'Chen Yang' 'Ming-Sheng Wang' 'Zhang-Jing Zhang' #=================================================== #black1 data_2_black_1 _database_code_depnum_ccdc_archive 'CCDC 756322' #TrackingRef '- compounds CIF CIFCheck.txt' #TrackingRef '- compounds CIF CIFCheck.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; '(mv)4BI6CL26 2H2O' ; _chemical_name_common "'(mv)4BI6CL26 2H2O'" _chemical_melting_point 'not measured' _chemical_formula_moiety '(mv)4BI6CL26 2H2O' _chemical_formula_sum 'C48 H60 Bi6 Cl26 N8 O2' _chemical_formula_weight 2956.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Bi Bi -4.1077 10.2566 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.3233(12) _cell_length_b 12.5298(18) _cell_length_c 19.723(2) _cell_angle_alpha 99.90(4) _cell_angle_beta 103.02(3) _cell_angle_gamma 107.72(2) _cell_volume 2065.2(5) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3821 _cell_measurement_theta_min 3.0910 _cell_measurement_theta_max 27.4835 _exptl_crystal_description Prism _exptl_crystal_colour black _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.377 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1360 _exptl_absorpt_coefficient_mu 13.618 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.3727 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Sphere (Rigaku CrystalClear)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating-anode generator' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury CCD ' _diffrn_measurement_method '\w ' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7489 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0778 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 25.35 _reflns_number_total 7489 _reflns_number_gt 5190 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2002)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2002)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2002)' _computing_structure_solution 'Siemens SHELXTL^TM^ 5' _computing_structure_refinement 'Siemens SHELXTL^TM^ 5' _computing_molecular_graphics ? _computing_publication_material 'Siemens SHELXTL^TM^ 5' _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^)+(0.0502P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7489 _refine_ls_number_parameters 415 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0712 _refine_ls_R_factor_gt 0.0456 _refine_ls_wR_factor_ref 0.1149 _refine_ls_wR_factor_gt 0.1006 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _refine_ls_shift/su_max 0.006 _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 0.108505(13) -0.436138(9) 0.281142(7) 0.01975(4) Uani 1 1 d . . . Bi2 Bi 0.167331(13) -0.164862(9) 0.174718(7) 0.02018(4) Uani 1 1 d . . . Bi3 Bi 0.525691(12) 0.134431(9) 0.448049(6) 0.01597(3) Uani 1 1 d . . . Cl1 Cl -0.09558(9) -0.52670(7) 0.34022(5) 0.0331(3) Uani 1 1 d . . . Cl2 Cl -0.05639(10) -0.58742(8) 0.16230(5) 0.0377(3) Uani 1 1 d . . . Cl3 Cl 0.26302(9) -0.56681(7) 0.30999(5) 0.0331(3) Uani 1 1 d . . . Cl4 Cl 0.32424(8) -0.31564(6) 0.20930(5) 0.0264(2) Uani 1 1 d . . . Cl5 Cl -0.05405(8) -0.28431(6) 0.23496(4) 0.0253(2) Uani 1 1 d . . . Cl6 Cl 0.38373(10) -0.05682(7) 0.11844(5) 0.0348(3) Uani 1 1 d . . . Cl7 Cl 0.00703(10) -0.30851(8) 0.05028(5) 0.0381(3) Uani 1 1 d . . . Cl8 Cl 0.00427(10) -0.03157(7) 0.14617(6) 0.0427(3) Uani 1 1 d . . . Cl9 Cl 0.34351(9) -0.01236(7) 0.31295(5) 0.0311(3) Uani 1 1 d . . . Cl10 Cl 0.73119(9) 0.23147(6) 0.38933(5) 0.0279(2) Uani 1 1 d . . . Cl11 Cl 0.37509(9) 0.27076(6) 0.42357(5) 0.0289(3) Uani 1 1 d . . . Cl12 Cl 0.68860(8) -0.01869(6) 0.48341(4) 0.0230(2) Uani 1 1 d . . . Cl13 Cl 0.69993(9) 0.28081(7) 0.57516(5) 0.0327(3) Uani 1 1 d . . . C1 C 0.4960(6) -0.1632(4) -0.0332(3) 0.0798(18) Uani 1 1 d . . . H1A H 0.6045 -0.1186 -0.0261 0.120 Uiso 1 1 calc R . . H1B H 0.4442 -0.1129 -0.0167 0.120 Uiso 1 1 calc R . . H1C H 0.4451 -0.2007 -0.0834 0.120 Uiso 1 1 calc R . . C2 C 0.6148(4) -0.2649(4) 0.0472(2) 0.0576(16) Uani 1 1 d . . . H2A H 0.7135 -0.2156 0.0488 0.069 Uiso 1 1 calc R . . C3 C 0.6034(4) -0.3480(4) 0.0844(2) 0.0526(15) Uani 1 1 d . . . H3A H 0.6943 -0.3523 0.1131 0.063 Uiso 1 1 calc R . . C4 C 0.4571(4) -0.4263(3) 0.0794(2) 0.0333(11) Uani 1 1 d . . . C5 C 0.3266(4) -0.4128(3) 0.0381(2) 0.0398(14) Uani 1 1 d . . . H5A H 0.2262 -0.4619 0.0345 0.048 Uiso 1 1 calc R . . C6 C 0.3438(4) -0.3277(3) 0.0023(2) 0.0422(13) Uani 1 1 d . . . H6A H 0.2552 -0.3212 -0.0271 0.051 Uiso 1 1 calc R . . C7 C 0.4432(3) -0.5187(3) 0.11952(18) 0.0267(10) Uani 1 1 d . . . C8 C 0.2988(4) -0.5968(3) 0.1135(2) 0.0477(14) Uani 1 1 d . . . H8A H 0.2083 -0.5933 0.0838 0.057 Uiso 1 1 calc R . . C9 C 0.2867(4) -0.6812(3) 0.1514(2) 0.0443(13) Uani 1 1 d . . . H9A H 0.1878 -0.7332 0.1474 0.053 Uiso 1 1 calc R . . C10 C 0.4009(4) -0.7778(3) 0.2338(2) 0.0466(14) Uani 1 1 d . . . H10A H 0.5039 -0.7712 0.2611 0.070 Uiso 1 1 calc R . . H10B H 0.3493 -0.8533 0.2007 0.070 Uiso 1 1 calc R . . H10C H 0.3400 -0.7672 0.2660 0.070 Uiso 1 1 calc R . . C11 C 0.5532(4) -0.6135(3) 0.1997(2) 0.0563(15) Uani 1 1 d . . . H11A H 0.6425 -0.6192 0.2290 0.068 Uiso 1 1 calc R . . C12 C 0.5718(4) -0.5281(3) 0.1658(3) 0.073(2) Uani 1 1 d . . . H12A H 0.6721 -0.4748 0.1734 0.087 Uiso 1 1 calc R . . C13 C 0.2357(4) 0.4729(3) 0.5076(2) 0.0333(12) Uani 1 1 d . . . H13A H 0.3444 0.5228 0.5224 0.050 Uiso 1 1 calc R . . H13B H 0.1731 0.5165 0.5208 0.050 Uiso 1 1 calc R . . H13C H 0.2008 0.4413 0.4563 0.050 Uiso 1 1 calc R . . C14 C 0.3444(4) 0.3753(3) 0.5911(2) 0.0380(13) Uani 1 1 d . . . H14A H 0.4418 0.4331 0.5999 0.046 Uiso 1 1 calc R . . C15 C 0.3342(3) 0.2907(3) 0.62740(19) 0.0348(12) Uani 1 1 d . . . H15A H 0.4229 0.2910 0.6605 0.042 Uiso 1 1 calc R . . C16 C 0.1878(3) 0.2043(2) 0.6135(2) 0.0270(11) Uani 1 1 d . . . C17 C 0.0652(4) 0.2128(3) 0.5678(2) 0.0484(15) Uani 1 1 d . . . H17A H -0.0347 0.1590 0.5603 0.058 Uiso 1 1 calc R . . C18 C 0.0806(4) 0.2992(3) 0.5307(3) 0.0522(16) Uani 1 1 d . . . H18A H -0.0067 0.3004 0.4974 0.063 Uiso 1 1 calc R . . C19 C 0.1710(3) 0.1087(3) 0.65126(17) 0.0224(10) Uani 1 1 d . . . C20 C 0.2975(4) 0.0977(3) 0.6942(2) 0.0492(15) Uani 1 1 d . . . H20A H 0.3981 0.1496 0.7006 0.059 Uiso 1 1 calc R . . C21 C 0.2781(4) 0.0089(3) 0.7289(2) 0.0408(12) Uani 1 1 d U . . H21A H 0.3660 0.0046 0.7601 0.049 Uiso 1 1 calc R . . C22 C 0.1207(4) -0.1649(3) 0.7541(2) 0.0443(14) Uani 1 1 d . . . H22A H 0.2229 -0.1578 0.7826 0.066 Uiso 1 1 calc R . . H22B H 0.0743 -0.2380 0.7183 0.066 Uiso 1 1 calc R . . H22C H 0.0546 -0.1610 0.7847 0.066 Uiso 1 1 calc R . . C23 C 0.0133(4) -0.0595(3) 0.6759(2) 0.0480(14) Uani 1 1 d . . . H23A H -0.0859 -0.1142 0.6685 0.058 Uiso 1 1 calc R . . C24 C 0.0240(4) 0.0286(3) 0.6416(2) 0.0450(13) Uani 1 1 d . . . H24A H -0.0659 0.0339 0.6126 0.054 Uiso 1 1 calc R . . N1 N 0.4866(3) -0.2542(2) 0.00920(16) 0.0376(10) Uani 1 1 d . . . N2 N 0.4157(3) -0.6886(2) 0.19354(17) 0.0368(10) Uani 1 1 d . . . N3 N 0.2185(3) 0.3777(2) 0.54332(17) 0.0309(10) Uani 1 1 d . . . N4 N 0.1363(3) -0.0703(2) 0.71856(16) 0.0306(9) Uani 1 1 d . . . O1W O 0.8554(7) -0.0980(5) -0.0326(4) 0.075(3) Uani 0.50 1 d P . . O2W O -0.1196(9) -0.8702(5) 0.0544(4) 0.104(3) Uani 0.50 1 d P . . 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 0.01763(5) 0.01328(5) 0.02180(6) 0.00088(4) 0.00104(4) 0.00201(4) Bi2 0.01928(5) 0.01205(5) 0.02155(6) -0.00102(4) 0.00054(5) 0.00196(4) Bi3 0.01371(4) 0.00776(4) 0.02042(5) -0.00012(4) 0.00116(4) 0.00044(4) Cl1 0.0263(4) 0.0249(4) 0.0416(5) 0.0058(3) 0.0133(3) -0.0008(3) Cl2 0.0329(4) 0.0319(4) 0.0300(5) -0.0092(4) -0.0033(4) 0.0050(3) Cl3 0.0331(4) 0.0257(3) 0.0383(5) 0.0018(3) 0.0025(4) 0.0167(3) Cl4 0.0230(3) 0.0206(3) 0.0306(4) -0.0002(3) 0.0078(3) 0.0046(3) Cl5 0.0224(3) 0.0211(3) 0.0297(4) 0.0033(3) 0.0056(3) 0.0072(3) Cl6 0.0359(4) 0.0290(4) 0.0336(4) 0.0057(3) 0.0130(3) 0.0029(3) Cl7 0.0311(4) 0.0324(4) 0.0317(5) -0.0097(4) -0.0019(4) 0.0028(3) Cl8 0.0457(4) 0.0381(4) 0.0489(6) 0.0073(4) 0.0102(4) 0.0263(3) Cl9 0.0291(4) 0.0232(4) 0.0277(5) -0.0046(3) 0.0000(4) 0.0032(3) Cl10 0.0247(3) 0.0191(3) 0.0376(4) 0.0074(3) 0.0126(3) 0.0023(3) Cl11 0.0299(3) 0.0219(3) 0.0340(4) 0.0034(3) 0.0036(3) 0.0145(3) Cl12 0.0197(3) 0.0168(3) 0.0311(4) 0.0048(3) 0.0067(3) 0.0060(3) Cl13 0.0265(4) 0.0239(4) 0.0309(5) -0.0070(4) -0.0004(4) -0.0001(3) C1 0.136(3) 0.062(2) 0.080(3) 0.034(2) 0.075(2) 0.048(2) C2 0.0257(18) 0.084(3) 0.057(2) 0.034(2) 0.0124(17) 0.0032(19) C3 0.0074(14) 0.079(3) 0.061(3) 0.024(2) 0.0012(17) 0.0040(16) C4 0.0426(16) 0.0258(15) 0.0275(19) -0.0095(14) 0.0052(14) 0.0194(12) C5 0.0241(16) 0.0157(15) 0.061(3) -0.0023(16) -0.0012(18) -0.0014(13) C6 0.0378(17) 0.0371(18) 0.050(2) 0.0069(16) 0.0052(17) 0.0188(14) C7 0.0238(14) 0.0247(15) 0.0186(17) -0.0145(13) -0.0008(13) 0.0070(12) C8 0.0315(17) 0.064(2) 0.048(2) 0.0265(16) 0.0025(17) 0.0184(15) C9 0.0142(15) 0.064(2) 0.046(2) 0.0285(16) 0.0049(15) -0.0028(16) C10 0.078(2) 0.0268(16) 0.037(2) 0.0043(15) 0.0140(19) 0.0260(15) C11 0.0348(18) 0.0263(16) 0.077(3) 0.0039(17) -0.035(2) 0.0104(14) C12 0.0152(17) 0.0213(17) 0.154(5) 0.020(2) -0.017(2) -0.0002(14) C13 0.0225(16) 0.0277(17) 0.028(2) -0.0068(15) -0.0079(15) -0.0025(14) C14 0.0156(14) 0.058(2) 0.0292(19) 0.0070(16) 0.0031(14) 0.0023(15) C15 0.0068(13) 0.0531(19) 0.0390(19) 0.0220(14) 0.0021(13) 0.0009(13) C16 0.0204(13) 0.0109(13) 0.048(2) 0.0008(13) 0.0097(14) 0.0079(10) C17 0.0246(17) 0.0135(15) 0.091(3) 0.0170(17) 0.001(2) -0.0058(14) C18 0.0251(18) 0.0235(17) 0.083(3) 0.0137(18) -0.011(2) -0.0070(15) C19 0.0096(12) 0.0365(15) 0.0184(16) 0.0020(12) 0.0009(11) 0.0097(11) C20 0.0210(17) 0.0326(19) 0.075(3) 0.0137(18) -0.0024(19) -0.0047(15) C21 0.0186(14) 0.0345(16) 0.057(2) 0.0117(15) -0.0006(15) 0.0019(12) C22 0.0490(18) 0.0122(15) 0.070(3) 0.0048(16) 0.0222(18) 0.0085(14) C23 0.0228(18) 0.047(2) 0.054(2) 0.0211(17) 0.0014(17) -0.0126(17) C24 0.0122(15) 0.062(2) 0.045(2) 0.0263(16) -0.0069(16) -0.0039(15) N1 0.0491(15) 0.0343(14) 0.0257(16) -0.0033(12) 0.0080(13) 0.0179(12) N2 0.0419(14) 0.0280(13) 0.0371(18) -0.0031(12) 0.0066(13) 0.0181(11) N3 0.0185(12) 0.0113(12) 0.0499(19) -0.0021(12) 0.0019(13) -0.0010(10) N4 0.0385(13) 0.0229(13) 0.0299(15) 0.0043(11) 0.0118(12) 0.0107(11) O1W 0.097(4) 0.057(3) 0.080(4) 0.033(3) 0.043(3) 0.017(3) O2W 0.184(6) 0.082(4) 0.038(4) 0.003(3) -0.008(4) 0.072(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Bi1 Cl1 2.5308(12) . ? Bi1 Cl3 2.5430(11) . ? Bi1 Cl2 2.5545(16) . ? Bi1 Cl5 2.9111(11) . ? Bi1 Cl4 2.9161(12) . ? Bi1 Cl13 2.9525(17) 2_656 ? Bi2 Cl7 2.5861(16) . ? Bi2 Cl8 2.6269(12) . ? Bi2 Cl6 2.6454(12) . ? Bi2 Cl5 2.7835(11) . ? Bi2 Cl4 2.8019(11) . ? Bi2 Cl9 2.8395(17) . ? Bi3 Cl10 2.5604(11) . ? Bi3 Cl11 2.5614(10) . ? Bi3 Cl13 2.6567(16) . ? Bi3 Cl9 2.7824(16) . ? Bi3 Cl12 2.8371(11) 2_656 ? Bi3 Cl12 2.8689(10) . ? Cl12 Bi3 2.8371(11) 2_656 ? Cl13 Bi1 2.9525(17) 2_656 ? C1 N1 1.518(6) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 N1 1.318(5) . ? C2 C3 1.364(7) . ? C2 H2A 0.9300 . ? C3 C4 1.388(5) . ? C3 H3A 0.9300 . ? C4 C5 1.377(5) . ? C4 C7 1.501(5) . ? C5 C6 1.367(6) . ? C5 H5A 0.9300 . ? C6 N1 1.329(4) . ? C6 H6A 0.9300 . ? C7 C8 1.367(5) . ? C7 C12 1.383(5) . ? C8 C9 1.389(6) . ? C8 H8A 0.9300 . ? C9 N2 1.338(5) . ? C9 H9A 0.9300 . ? C10 N2 1.471(5) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 N2 1.304(4) . ? C11 C12 1.345(7) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? C13 N3 1.472(5) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 N3 1.342(4) . ? C14 C15 1.369(6) . ? C14 H14A 0.9300 . ? C15 C16 1.394(4) . ? C15 H15A 0.9300 . ? C16 C17 1.331(5) . ? C16 C19 1.503(5) . ? C17 C18 1.399(6) . ? C17 H17A 0.9300 . ? C18 N3 1.297(4) . ? C18 H18A 0.9300 . ? C19 C20 1.348(5) . ? C19 C24 1.378(4) . ? C20 C21 1.391(6) . ? C20 H20A 0.9300 . ? C21 N4 1.336(4) . ? C21 H21A 0.9300 . ? C22 N4 1.464(5) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 N4 1.319(5) . ? C23 C24 1.381(6) . ? C23 H23A 0.9300 . ? C24 H24A 0.9300 . ? 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 Cl1 Bi1 Cl3 93.26(4) . . ? Cl1 Bi1 Cl2 89.67(4) . . ? Cl3 Bi1 Cl2 89.09(4) . . ? Cl1 Bi1 Cl5 92.41(3) . . ? Cl3 Bi1 Cl5 173.72(3) . . ? Cl2 Bi1 Cl5 88.24(4) . . ? Cl1 Bi1 Cl4 173.76(3) . . ? Cl3 Bi1 Cl4 92.97(3) . . ? Cl2 Bi1 Cl4 90.37(3) . . ? Cl5 Bi1 Cl4 81.36(3) . . ? Cl1 Bi1 Cl13 87.33(3) . 2_656 ? Cl3 Bi1 Cl13 86.23(4) . 2_656 ? Cl2 Bi1 Cl13 174.28(3) . 2_656 ? Cl5 Bi1 Cl13 96.75(3) . 2_656 ? Cl4 Bi1 Cl13 93.15(3) . 2_656 ? Cl7 Bi2 Cl8 89.37(4) . . ? Cl7 Bi2 Cl6 90.31(4) . . ? Cl8 Bi2 Cl6 92.10(4) . . ? Cl7 Bi2 Cl5 89.64(4) . . ? Cl8 Bi2 Cl5 90.11(3) . . ? Cl6 Bi2 Cl5 177.78(3) . . ? Cl7 Bi2 Cl4 90.52(4) . . ? Cl8 Bi2 Cl4 175.81(3) . . ? Cl6 Bi2 Cl4 92.08(3) . . ? Cl5 Bi2 Cl4 85.70(3) . . ? Cl7 Bi2 Cl9 178.43(3) . . ? Cl8 Bi2 Cl9 91.90(4) . . ? Cl6 Bi2 Cl9 90.57(3) . . ? Cl5 Bi2 Cl9 89.44(3) . . ? Cl4 Bi2 Cl9 88.15(4) . . ? Cl10 Bi3 Cl11 92.16(3) . . ? Cl10 Bi3 Cl13 90.41(3) . . ? Cl11 Bi3 Cl13 90.28(4) . . ? Cl10 Bi3 Cl9 88.44(3) . . ? Cl11 Bi3 Cl9 88.16(4) . . ? Cl13 Bi3 Cl9 178.03(3) . . ? Cl10 Bi3 Cl12 176.10(3) . 2_656 ? Cl11 Bi3 Cl12 91.68(3) . 2_656 ? Cl13 Bi3 Cl12 88.87(3) . 2_656 ? Cl9 Bi3 Cl12 92.38(3) . 2_656 ? Cl10 Bi3 Cl12 90.83(3) . . ? Cl11 Bi3 Cl12 176.46(3) . . ? Cl13 Bi3 Cl12 87.81(4) . . ? Cl9 Bi3 Cl12 93.81(4) . . ? Cl12 Bi3 Cl12 85.31(3) 2_656 . ? Bi2 Cl4 Bi1 96.12(3) . . ? Bi2 Cl5 Bi1 96.64(3) . . ? Bi3 Cl9 Bi2 177.84(4) . . ? Bi3 Cl12 Bi3 94.69(3) 2_656 . ? Bi3 Cl13 Bi1 177.87(4) . 2_656 ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 120.4(3) . . ? N1 C2 H2A 119.8 . . ? C3 C2 H2A 119.8 . . ? C2 C3 C4 120.4(4) . . ? C2 C3 H3A 119.8 . . ? C4 C3 H3A 119.8 . . ? C5 C4 C3 117.0(4) . . ? C5 C4 C7 122.1(3) . . ? C3 C4 C7 120.9(3) . . ? C6 C5 C4 120.4(3) . . ? C6 C5 H5A 119.8 . . ? C4 C5 H5A 119.8 . . ? N1 C6 C5 120.3(3) . . ? N1 C6 H6A 119.9 . . ? C5 C6 H6A 119.9 . . ? C8 C7 C12 116.3(4) . . ? C8 C7 C4 120.6(3) . . ? C12 C7 C4 123.0(3) . . ? C7 C8 C9 120.3(3) . . ? C7 C8 H8A 119.8 . . ? C9 C8 H8A 119.8 . . ? N2 C9 C8 120.7(3) . . ? N2 C9 H9A 119.6 . . ? C8 C9 H9A 119.6 . . ? N2 C10 H10A 109.5 . . ? N2 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N2 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N2 C11 C12 123.0(4) . . ? N2 C11 H11A 118.5 . . ? C12 C11 H11A 118.5 . . ? C11 C12 C7 120.7(3) . . ? C11 C12 H12A 119.7 . . ? C7 C12 H12A 119.7 . . ? N3 C13 H13A 109.5 . . ? N3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N3 C14 C15 122.2(3) . . ? N3 C14 H14A 118.9 . . ? C15 C14 H14A 118.9 . . ? C14 C15 C16 118.4(3) . . ? C14 C15 H15A 120.8 . . ? C16 C15 H15A 120.8 . . ? C17 C16 C15 117.2(3) . . ? C17 C16 C19 122.3(3) . . ? C15 C16 C19 120.4(3) . . ? C16 C17 C18 122.7(3) . . ? C16 C17 H17A 118.7 . . ? C18 C17 H17A 118.7 . . ? N3 C18 C17 119.1(4) . . ? N3 C18 H18A 120.4 . . ? C17 C18 H18A 120.4 . . ? C20 C19 C24 118.4(4) . . ? C20 C19 C16 121.5(3) . . ? C24 C19 C16 120.1(3) . . ? C19 C20 C21 120.2(3) . . ? C19 C20 H20A 119.9 . . ? C21 C20 H20A 119.9 . . ? N4 C21 C20 121.6(3) . . ? N4 C21 H21A 119.2 . . ? C20 C21 H21A 119.2 . . ? N4 C22 H22A 109.5 . . ? N4 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N4 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N4 C23 C24 123.5(3) . . ? N4 C23 H23A 118.3 . . ? C24 C23 H23A 118.3 . . ? C19 C24 C23 118.5(3) . . ? C19 C24 H24A 120.7 . . ? C23 C24 H24A 120.7 . . ? C2 N1 C6 121.3(4) . . ? C2 N1 C1 121.4(3) . . ? C6 N1 C1 117.1(3) . . ? C11 N2 C9 118.9(4) . . ? C11 N2 C10 121.0(3) . . ? C9 N2 C10 120.1(3) . . ? C18 N3 C14 120.3(4) . . ? C18 N3 C13 119.9(3) . . ? C14 N3 C13 119.8(3) . . ? C23 N4 C21 117.7(3) . . ? C23 N4 C22 122.1(3) . . ? C21 N4 C22 120.2(3) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.844 _refine_diff_density_min -1.759 _refine_diff_density_rms 0.251 #============================================================ data_2_colorless_1 _database_code_depnum_ccdc_archive 'CCDC 756323' #TrackingRef '- compounds CIF CIFCheck.txt' #TrackingRef '- compounds CIF CIFCheck.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; '(mv)4BI6CL26 2H2O' ; _chemical_name_common "'(mv)4BI6CL26 2H2O'" _chemical_melting_point 'not measured' _chemical_formula_moiety '(mv)4BI6CL26 2H2O' _chemical_formula_sum 'C48 H60 Bi6 Cl26 N8 O2' _chemical_formula_weight 2956.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Bi Bi -4.1077 10.2566 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.3132(16) _cell_length_b 12.499(3) _cell_length_c 19.727(4) _cell_angle_alpha 99.926(11) _cell_angle_beta 103.057(8) _cell_angle_gamma 107.672(7) _cell_volume 2058.3(7) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5494 _cell_measurement_theta_min 3.0957 _cell_measurement_theta_max 27.4835 _exptl_crystal_description Prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.385 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1360 _exptl_absorpt_coefficient_mu 13.663 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.1210 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Sphere (Rigaku CrystalClear)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating-anode generator' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury CCD ' _diffrn_measurement_method '\w ' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7364 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1230 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 25.34 _reflns_number_total 7364 _reflns_number_gt 4830 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2002)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2002)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2002)' _computing_structure_solution 'Siemens SHELXTL^TM^ 5' _computing_structure_refinement 'Siemens SHELXTL^TM^ 5' _computing_molecular_graphics ? _computing_publication_material 'Siemens SHELXTL^TM^ 5' _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^)+(0.0001P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7364 _refine_ls_number_parameters 415 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0617 _refine_ls_R_factor_gt 0.0500 _refine_ls_wR_factor_ref 0.1005 _refine_ls_wR_factor_gt 0.0983 _refine_ls_goodness_of_fit_ref 0.937 _refine_ls_restrained_S_all 0.937 _refine_ls_shift/su_max 0.002 _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 0.108303(12) -0.436229(9) 0.281233(7) 0.03358(4) Uani 1 1 d . . . Bi2 Bi 0.166979(12) -0.165266(9) 0.174510(7) 0.03364(4) Uani 1 1 d . . . Bi3 Bi 0.525498(12) 0.134223(9) 0.447893(7) 0.03022(3) Uani 1 1 d . . . Cl1 Cl -0.09596(9) -0.52682(7) 0.34070(5) 0.0445(3) Uani 1 1 d . . . Cl2 Cl -0.05733(9) -0.58821(7) 0.16230(5) 0.0488(3) Uani 1 1 d . . . Cl3 Cl 0.26361(9) -0.56661(7) 0.31068(5) 0.0451(3) Uani 1 1 d . . . Cl4 Cl 0.32463(8) -0.31646(6) 0.20963(5) 0.0376(2) Uani 1 1 d . . . Cl5 Cl -0.05548(8) -0.28474(6) 0.23495(5) 0.0378(2) Uani 1 1 d . . . Cl6 Cl 0.38339(9) -0.05698(7) 0.11813(5) 0.0468(3) Uani 1 1 d . . . Cl7 Cl 0.00502(9) -0.30996(7) 0.04993(5) 0.0495(3) Uani 1 1 d . . . Cl8 Cl 0.00392(9) -0.03170(7) 0.14624(5) 0.0500(3) Uani 1 1 d . . . Cl9 Cl 0.34271(9) -0.01324(6) 0.31263(5) 0.0428(3) Uani 1 1 d . . . Cl10 Cl 0.73129(8) 0.23158(6) 0.38812(5) 0.0409(3) Uani 1 1 d . . . Cl11 Cl 0.37552(8) 0.27112(6) 0.42364(5) 0.0404(3) Uani 1 1 d . . . Cl12 Cl 0.68878(8) -0.01932(6) 0.48340(4) 0.0351(2) Uani 1 1 d . . . Cl13 Cl 0.70117(9) 0.28106(6) 0.57562(5) 0.0433(3) Uani 1 1 d . . . C1 C 0.5009(5) -0.1636(3) -0.0288(3) 0.0913(18) Uani 1 1 d . . . H1A H 0.6105 -0.1205 -0.0207 0.137 Uiso 1 1 calc R . . H1B H 0.4518 -0.1125 -0.0103 0.137 Uiso 1 1 calc R . . H1C H 0.4501 -0.1967 -0.0796 0.137 Uiso 1 1 calc R . . C2 C 0.6160(4) -0.2678(4) 0.0479(2) 0.0693(17) Uani 1 1 d . . . H2A H 0.7155 -0.2172 0.0512 0.083 Uiso 1 1 calc R . . C3 C 0.6038(4) -0.3513(3) 0.0829(2) 0.0597(14) Uani 1 1 d . . . H3A H 0.6954 -0.3574 0.1099 0.072 Uiso 1 1 calc R . . C4 C 0.4597(3) -0.4284(3) 0.08028(19) 0.0407(10) Uani 1 1 d . . . C5 C 0.3276(4) -0.4157(3) 0.0378(2) 0.0570(14) Uani 1 1 d . . . H5A H 0.2281 -0.4677 0.0330 0.068 Uiso 1 1 calc R . . C6 C 0.3392(4) -0.3312(3) 0.0036(2) 0.0534(13) Uani 1 1 d . . . H6A H 0.2484 -0.3234 -0.0229 0.064 Uiso 1 1 calc R . . C7 C 0.4423(3) -0.5190(3) 0.11892(18) 0.0387(10) Uani 1 1 d . . . C8 C 0.2935(4) -0.6005(3) 0.1146(2) 0.0533(13) Uani 1 1 d . . . H8A H 0.2014 -0.5961 0.0868 0.064 Uiso 1 1 calc R . . C9 C 0.2850(4) -0.6813(3) 0.1492(2) 0.0657(15) Uani 1 1 d . . . H9A H 0.1867 -0.7364 0.1431 0.079 Uiso 1 1 calc R . . C10 C 0.4001(4) -0.7794(3) 0.2341(2) 0.0564(14) Uani 1 1 d . . . H10A H 0.5029 -0.7731 0.2615 0.085 Uiso 1 1 calc R . . H10B H 0.3487 -0.8547 0.2005 0.085 Uiso 1 1 calc R . . H10C H 0.3385 -0.7695 0.2661 0.085 Uiso 1 1 calc R . . C11 C 0.5534(4) -0.6140(3) 0.1997(3) 0.0710(17) Uani 1 1 d . . . H11A H 0.6423 -0.6184 0.2303 0.085 Uiso 1 1 calc R . . C12 C 0.5731(4) -0.5297(3) 0.1624(3) 0.0728(19) Uani 1 1 d . . . H12A H 0.6738 -0.4803 0.1665 0.087 Uiso 1 1 calc R . . C13 C 0.2376(4) 0.4745(3) 0.5066(2) 0.0500(13) Uani 1 1 d . . . H13A H 0.3462 0.5249 0.5212 0.075 Uiso 1 1 calc R . . H13B H 0.1746 0.5181 0.5197 0.075 Uiso 1 1 calc R . . H13C H 0.2024 0.4424 0.4553 0.075 Uiso 1 1 calc R . . C14 C 0.3468(4) 0.3783(3) 0.5924(2) 0.0538(13) Uani 1 1 d . . . H14A H 0.4445 0.4368 0.6028 0.065 Uiso 1 1 calc R . . C15 C 0.3349(4) 0.2939(3) 0.62781(18) 0.0465(12) Uani 1 1 d . . . H15A H 0.4239 0.2947 0.6610 0.056 Uiso 1 1 calc R . . C16 C 0.1900(3) 0.2058(3) 0.61482(19) 0.0380(10) Uani 1 1 d . . . C17 C 0.0615(4) 0.2126(3) 0.5653(3) 0.0622(16) Uani 1 1 d . . . H17A H -0.0383 0.1571 0.5556 0.075 Uiso 1 1 calc R . . C18 C 0.0805(4) 0.2990(3) 0.5311(3) 0.0589(15) Uani 1 1 d . . . H18A H -0.0076 0.3015 0.4989 0.071 Uiso 1 1 calc R . . C19 C 0.1706(3) 0.1100(3) 0.65011(19) 0.0383(10) Uani 1 1 d . . . C20 C 0.2988(4) 0.0983(3) 0.6960(3) 0.0674(17) Uani 1 1 d . . . H20A H 0.3995 0.1513 0.7039 0.081 Uiso 1 1 calc R . . C21 C 0.2798(4) 0.0098(3) 0.7300(2) 0.0557(14) Uani 1 1 d . . . H21A H 0.3677 0.0050 0.7611 0.067 Uiso 1 1 calc R . . C22 C 0.1176(4) -0.1658(3) 0.7538(2) 0.0559(14) Uani 1 1 d . . . H22A H 0.2188 -0.1603 0.7826 0.084 Uiso 1 1 calc R . . H22B H 0.0706 -0.2385 0.7175 0.084 Uiso 1 1 calc R . . H22C H 0.0506 -0.1617 0.7839 0.084 Uiso 1 1 calc R . . C23 C 0.0109(4) -0.0583(3) 0.6767(2) 0.0598(14) Uani 1 1 d . . . H23A H -0.0894 -0.1096 0.6716 0.072 Uiso 1 1 calc R . . C24 C 0.0264(4) 0.0278(3) 0.6406(2) 0.0551(13) Uani 1 1 d . . . H24A H -0.0629 0.0300 0.6091 0.066 Uiso 1 1 calc R . . N1 N 0.4859(3) -0.2557(3) 0.00759(17) 0.0533(11) Uani 1 1 d . . . N2 N 0.4157(3) -0.6876(2) 0.19394(15) 0.0429(9) Uani 1 1 d . . . N3 N 0.2220(3) 0.3813(2) 0.54216(16) 0.0411(9) Uani 1 1 d . . . N4 N 0.1372(3) -0.0696(2) 0.71916(16) 0.0415(9) Uani 1 1 d . . . O1W O 0.8581(7) -0.1031(5) -0.0382(4) 0.084(3) Uani 0.50 1 d P . . O2W O -0.1174(8) -0.8670(5) 0.0535(4) 0.109(3) Uani 0.50 1 d P . . 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 0.02054(5) 0.02312(5) 0.04694(6) -0.00871(5) -0.00309(5) 0.01310(4) Bi2 0.02235(5) 0.02107(5) 0.04674(6) -0.01092(5) -0.00282(5) 0.01327(4) Bi3 0.01799(4) 0.01787(4) 0.04561(6) -0.00959(4) -0.00260(4) 0.01229(4) Cl1 0.0332(4) 0.0320(4) 0.0607(5) -0.0017(4) 0.0079(3) 0.0132(3) Cl2 0.0311(4) 0.0393(4) 0.0559(5) -0.0171(4) -0.0067(4) 0.0155(3) Cl3 0.0320(3) 0.0333(3) 0.0592(5) -0.0094(4) -0.0063(4) 0.0229(3) Cl4 0.0231(3) 0.0289(3) 0.0497(4) -0.0101(3) -0.0010(3) 0.0137(3) Cl5 0.0238(3) 0.0273(3) 0.0546(4) -0.0059(3) 0.0021(3) 0.0144(3) Cl6 0.0383(4) 0.0338(4) 0.0598(5) -0.0034(4) 0.0097(3) 0.0132(3) Cl7 0.0331(4) 0.0356(4) 0.0582(5) -0.0195(4) -0.0051(4) 0.0134(3) Cl8 0.0430(4) 0.0375(4) 0.0654(5) -0.0063(4) 0.0039(4) 0.0283(3) Cl9 0.0304(4) 0.0303(4) 0.0493(5) -0.0154(4) -0.0098(4) 0.0154(3) Cl10 0.0312(3) 0.0267(3) 0.0600(4) -0.0025(3) 0.0092(3) 0.0146(3) Cl11 0.0298(3) 0.0266(3) 0.0598(5) -0.0050(3) 0.0001(3) 0.0216(3) Cl12 0.0228(3) 0.0238(3) 0.0527(4) -0.0059(3) 0.0026(3) 0.0149(3) Cl13 0.0280(4) 0.0289(4) 0.0532(5) -0.0141(4) -0.0090(4) 0.0115(3) C1 0.106(2) 0.076(2) 0.126(3) 0.021(2) 0.061(2) 0.0646(19) C2 0.0288(17) 0.081(3) 0.082(3) 0.003(2) 0.0075(19) 0.0139(18) C3 0.0355(16) 0.086(2) 0.064(2) 0.0249(18) 0.0112(15) 0.0290(16) C4 0.0239(13) 0.0448(16) 0.0435(17) -0.0161(14) -0.0030(12) 0.0230(12) C5 0.0226(14) 0.0387(17) 0.088(3) -0.0164(19) -0.0160(17) 0.0225(12) C6 0.0417(16) 0.0221(15) 0.092(3) -0.0026(17) 0.0187(17) 0.0162(13) C7 0.0243(13) 0.0365(15) 0.0436(17) -0.0148(14) -0.0031(12) 0.0183(12) C8 0.0308(14) 0.060(2) 0.075(2) 0.0198(17) 0.0206(14) 0.0190(15) C9 0.0269(16) 0.082(2) 0.093(3) 0.034(2) 0.0090(18) 0.0268(16) C10 0.0437(16) 0.0360(16) 0.082(3) -0.0096(18) 0.0010(18) 0.0298(13) C11 0.0293(17) 0.0419(18) 0.118(4) 0.009(2) -0.017(2) 0.0146(15) C12 0.0297(17) 0.0265(16) 0.139(4) 0.005(2) -0.011(2) 0.0134(14) C13 0.0399(16) 0.0247(15) 0.075(2) -0.0090(16) 0.0045(16) 0.0192(13) C14 0.0200(14) 0.070(2) 0.064(2) 0.0056(19) -0.0003(15) 0.0210(14) C15 0.0355(15) 0.0615(19) 0.0389(16) 0.0034(15) 0.0010(13) 0.0250(14) C16 0.0216(12) 0.0309(15) 0.0530(18) -0.0129(14) 0.0022(12) 0.0173(11) C17 0.0294(17) 0.0249(15) 0.112(3) 0.0031(19) -0.011(2) 0.0122(13) C18 0.0216(16) 0.0305(16) 0.102(3) 0.0073(18) -0.0138(19) 0.0072(13) C19 0.0177(12) 0.0297(15) 0.0540(18) -0.0161(14) 0.0008(12) 0.0118(11) C20 0.0236(16) 0.0290(16) 0.126(4) -0.002(2) -0.013(2) 0.0140(13) C21 0.0232(15) 0.0357(16) 0.091(3) -0.0004(18) -0.0094(18) 0.0152(13) C22 0.0404(16) 0.0398(17) 0.086(3) 0.0018(18) 0.0154(17) 0.0227(14) C23 0.0214(15) 0.071(2) 0.081(2) 0.0285(18) 0.0051(17) 0.0102(16) C24 0.0201(14) 0.084(2) 0.0490(19) 0.0095(18) -0.0057(15) 0.0182(16) N1 0.0526(15) 0.0498(16) 0.0470(16) -0.0078(14) 0.0062(13) 0.0213(13) N2 0.0411(13) 0.0419(13) 0.0375(14) -0.0136(12) -0.0052(11) 0.0288(10) N3 0.0326(12) 0.0249(12) 0.0557(16) -0.0137(12) -0.0006(12) 0.0194(10) N4 0.0303(11) 0.0305(12) 0.0533(15) -0.0181(12) 0.0048(11) 0.0181(10) O1W 0.069(3) 0.050(3) 0.124(5) 0.014(3) 0.022(3) 0.017(3) O2W 0.177(5) 0.114(3) 0.073(4) 0.038(3) 0.023(4) 0.104(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Bi1 Cl1 2.5369(10) . ? Bi1 Cl3 2.5422(10) . ? Bi1 Cl2 2.5577(10) . ? Bi1 Cl5 2.9096(10) . ? Bi1 Cl4 2.9120(10) . ? Bi1 Cl13 2.9398(10) 2_656 ? Bi2 Cl7 2.5927(10) . ? Bi2 Cl8 2.6234(11) . ? Bi2 Cl6 2.6471(10) . ? Bi2 Cl5 2.7920(10) . ? Bi2 Cl4 2.8077(10) . ? Bi2 Cl9 2.8329(10) . ? Bi3 Cl11 2.5571(10) . ? Bi3 Cl10 2.5777(10) . ? Bi3 Cl13 2.6672(9) . ? Bi3 Cl9 2.7861(9) . ? Bi3 Cl12 2.8347(9) 2_656 ? Bi3 Cl12 2.8706(10) . ? Cl12 Bi3 2.8347(9) 2_656 ? Cl13 Bi1 2.9398(10) 2_656 ? C1 N1 1.446(6) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.338(7) . ? C2 N1 1.357(5) . ? C2 H2A 0.9300 . ? C3 C4 1.378(5) . ? C3 H3A 0.9300 . ? C4 C5 1.392(5) . ? C4 C7 1.460(5) . ? C5 C6 1.339(6) . ? C5 H5A 0.9300 . ? C6 N1 1.381(4) . ? C6 H6A 0.9300 . ? C7 C12 1.380(5) . ? C7 C8 1.422(4) . ? C8 C9 1.306(6) . ? C8 H8A 0.9300 . ? C9 N2 1.365(5) . ? C9 H9A 0.9300 . ? C10 N2 1.493(5) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 N2 1.298(4) . ? C11 C12 1.377(7) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? C13 N3 1.448(5) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 C15 1.353(6) . ? C14 N3 1.361(4) . ? C14 H14A 0.9300 . ? C15 C16 1.394(4) . ? C15 H15A 0.9300 . ? C16 C17 1.399(5) . ? C16 C19 1.471(5) . ? C17 C18 1.356(6) . ? C17 H17A 0.9300 . ? C18 N3 1.346(4) . ? C18 H18A 0.9300 . ? C19 C24 1.369(4) . ? C19 C20 1.389(5) . ? C20 C21 1.377(6) . ? C20 H20A 0.9300 . ? C21 N4 1.339(4) . ? C21 H21A 0.9300 . ? C22 N4 1.467(5) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 N4 1.342(5) . ? C23 C24 1.380(6) . ? C23 H23A 0.9300 . ? C24 H24A 0.9300 . ? 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 Cl1 Bi1 Cl3 93.20(3) . . ? Cl1 Bi1 Cl2 89.71(3) . . ? Cl3 Bi1 Cl2 89.36(3) . . ? Cl1 Bi1 Cl5 92.28(3) . . ? Cl3 Bi1 Cl5 173.96(3) . . ? Cl2 Bi1 Cl5 88.11(3) . . ? Cl1 Bi1 Cl4 174.04(3) . . ? Cl3 Bi1 Cl4 92.76(3) . . ? Cl2 Bi1 Cl4 90.43(3) . . ? Cl5 Bi1 Cl4 81.78(3) . . ? Cl1 Bi1 Cl13 87.13(3) . 2_656 ? Cl3 Bi1 Cl13 86.04(3) . 2_656 ? Cl2 Bi1 Cl13 174.27(3) . 2_656 ? Cl5 Bi1 Cl13 96.79(3) . 2_656 ? Cl4 Bi1 Cl13 93.20(3) . 2_656 ? Cl7 Bi2 Cl8 89.39(3) . . ? Cl7 Bi2 Cl6 90.51(3) . . ? Cl8 Bi2 Cl6 92.11(3) . . ? Cl7 Bi2 Cl5 89.45(3) . . ? Cl8 Bi2 Cl5 89.91(3) . . ? Cl6 Bi2 Cl5 177.98(3) . . ? Cl7 Bi2 Cl4 90.72(3) . . ? Cl8 Bi2 Cl4 175.68(3) . . ? Cl6 Bi2 Cl4 92.21(3) . . ? Cl5 Bi2 Cl4 85.77(3) . . ? Cl7 Bi2 Cl9 178.17(3) . . ? Cl8 Bi2 Cl9 91.90(3) . . ? Cl6 Bi2 Cl9 90.73(3) . . ? Cl5 Bi2 Cl9 89.26(3) . . ? Cl4 Bi2 Cl9 87.89(3) . . ? Cl11 Bi3 Cl10 91.97(3) . . ? Cl11 Bi3 Cl13 90.35(3) . . ? Cl10 Bi3 Cl13 90.71(3) . . ? Cl11 Bi3 Cl9 88.29(3) . . ? Cl10 Bi3 Cl9 88.17(3) . . ? Cl13 Bi3 Cl9 178.21(3) . . ? Cl11 Bi3 Cl12 91.56(3) . 2_656 ? Cl10 Bi3 Cl12 176.43(3) . 2_656 ? Cl13 Bi3 Cl12 88.71(3) . 2_656 ? Cl9 Bi3 Cl12 92.49(3) . 2_656 ? Cl11 Bi3 Cl12 176.41(3) . . ? Cl10 Bi3 Cl12 90.98(3) . . ? Cl13 Bi3 Cl12 87.58(3) . . ? Cl9 Bi3 Cl12 93.84(3) . . ? Cl12 Bi3 Cl12 85.47(3) 2_656 . ? Bi2 Cl4 Bi1 95.94(3) . . ? Bi2 Cl5 Bi1 96.34(3) . . ? Bi3 Cl9 Bi2 177.82(4) . . ? Bi3 Cl12 Bi3 94.53(3) 2_656 . ? Bi3 Cl13 Bi1 178.01(4) . 2_656 ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 N1 121.2(3) . . ? C3 C2 H2A 119.4 . . ? N1 C2 H2A 119.4 . . ? C2 C3 C4 122.1(4) . . ? C2 C3 H3A 119.0 . . ? C4 C3 H3A 119.0 . . ? C3 C4 C5 115.9(4) . . ? C3 C4 C7 123.4(3) . . ? C5 C4 C7 120.7(3) . . ? C6 C5 C4 122.2(3) . . ? C6 C5 H5A 118.9 . . ? C4 C5 H5A 118.9 . . ? C5 C6 N1 120.0(3) . . ? C5 C6 H6A 120.0 . . ? N1 C6 H6A 120.0 . . ? C12 C7 C8 116.1(4) . . ? C12 C7 C4 120.6(3) . . ? C8 C7 C4 123.3(3) . . ? C9 C8 C7 120.7(3) . . ? C9 C8 H8A 119.7 . . ? C7 C8 H8A 119.7 . . ? C8 C9 N2 122.1(3) . . ? C8 C9 H9A 119.0 . . ? N2 C9 H9A 119.0 . . ? N2 C10 H10A 109.5 . . ? N2 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N2 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N2 C11 C12 122.6(4) . . ? N2 C11 H11A 118.7 . . ? C12 C11 H11A 118.7 . . ? C11 C12 C7 119.6(3) . . ? C11 C12 H12A 120.2 . . ? C7 C12 H12A 120.2 . . ? N3 C13 H13A 109.5 . . ? N3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 N3 122.9(3) . . ? C15 C14 H14A 118.6 . . ? N3 C14 H14A 118.6 . . ? C14 C15 C16 120.4(3) . . ? C14 C15 H15A 119.8 . . ? C16 C15 H15A 119.8 . . ? C15 C16 C17 116.1(3) . . ? C15 C16 C19 122.9(3) . . ? C17 C16 C19 121.0(3) . . ? C18 C17 C16 120.9(3) . . ? C18 C17 H17A 119.5 . . ? C16 C17 H17A 119.5 . . ? N3 C18 C17 122.5(3) . . ? N3 C18 H18A 118.7 . . ? C17 C18 H18A 118.7 . . ? C24 C19 C20 115.9(4) . . ? C24 C19 C16 122.6(3) . . ? C20 C19 C16 121.5(3) . . ? C21 C20 C19 121.4(3) . . ? C21 C20 H20A 119.3 . . ? C19 C20 H20A 119.3 . . ? N4 C21 C20 121.2(3) . . ? N4 C21 H21A 119.4 . . ? C20 C21 H21A 119.4 . . ? N4 C22 H22A 109.5 . . ? N4 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N4 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N4 C23 C24 121.5(3) . . ? N4 C23 H23A 119.2 . . ? C24 C23 H23A 119.2 . . ? C19 C24 C23 121.3(3) . . ? C19 C24 H24A 119.3 . . ? C23 C24 H24A 119.3 . . ? C2 N1 C6 118.6(4) . . ? C2 N1 C1 120.6(3) . . ? C6 N1 C1 120.8(3) . . ? C11 N2 C9 118.8(4) . . ? C11 N2 C10 120.8(3) . . ? C9 N2 C10 120.3(3) . . ? C18 N3 C14 117.0(3) . . ? C18 N3 C13 121.2(3) . . ? C14 N3 C13 121.5(3) . . ? C21 N4 C23 118.5(3) . . ? C21 N4 C22 121.2(3) . . ? C23 N4 C22 120.3(3) . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 25.34 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 2.324 _refine_diff_density_min -2.868 _refine_diff_density_rms 0.253 #================================================== #yellowish1 data_x_yellowish_1 _database_code_depnum_ccdc_archive 'CCDC 756324' #TrackingRef '- compounds CIF CIFCheck.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; '(mv)4BI6CL26 2H2O' ; _chemical_name_common "'(mv)4BI6CL26 2H2O'" _chemical_melting_point 'not measured' _chemical_formula_moiety '(mv)4BI6CL26 2H2O' _chemical_formula_sum 'C48 H60 Bi6 Cl26 N8 O2' _chemical_formula_weight 2956.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Bi Bi -4.1077 10.2566 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.327(2) _cell_length_b 12.528(3) _cell_length_c 19.738(6) _cell_angle_alpha 99.887(12) _cell_angle_beta 102.928(9) _cell_angle_gamma 107.801(9) _cell_volume 2067.4(10) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4937 _cell_measurement_theta_min 2.4340 _cell_measurement_theta_max 27.4835 _exptl_crystal_description Prism _exptl_crystal_colour yellowish _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.27 _exptl_crystal_density_diffrn 2.375 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1360 _exptl_absorpt_coefficient_mu 13.603 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5410 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Sphere (Rigaku CrystalClear)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating-anode generator' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury CCD ' _diffrn_measurement_method '\w ' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14435 _diffrn_reflns_av_R_equivalents 0.0358 _diffrn_reflns_av_sigmaI/netI 0.0464 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.76 _diffrn_reflns_theta_max 25.35 _reflns_number_total 7180 _reflns_number_gt 5762 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2002)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2002)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2002)' _computing_structure_solution 'Siemens SHELXTL^TM^ 5' _computing_structure_refinement 'Siemens SHELXTL^TM^ 5' _computing_molecular_graphics ? _computing_publication_material 'Siemens SHELXTL^TM^ 5' _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^)+(0.0323P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7180 _refine_ls_number_parameters 415 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0446 _refine_ls_R_factor_gt 0.0321 _refine_ls_wR_factor_ref 0.0748 _refine_ls_wR_factor_gt 0.0704 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _refine_ls_shift/su_max 0.008 _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 0.108793(8) -0.435973(7) 0.281297(4) 0.01716(2) Uani 1 1 d . . . Bi2 Bi 0.167726(8) -0.164905(7) 0.174714(4) 0.01764(2) Uani 1 1 d . . . Bi3 Bi 0.525657(8) 0.134308(6) 0.447942(4) 0.01376(2) Uani 1 1 d . . . Cl1 Cl -0.09546(6) -0.52696(5) 0.34022(3) 0.03072(18) Uani 1 1 d . . . Cl2 Cl -0.05577(7) -0.58731(6) 0.16262(3) 0.03522(19) Uani 1 1 d . . . Cl3 Cl 0.26375(6) -0.56625(5) 0.31067(3) 0.03117(18) Uani 1 1 d . . . Cl4 Cl 0.32457(6) -0.31614(5) 0.20921(3) 0.02325(16) Uani 1 1 d . . . Cl5 Cl -0.05453(6) -0.28450(5) 0.23480(3) 0.02423(16) Uani 1 1 d . . . Cl6 Cl 0.38459(7) -0.05644(5) 0.11872(3) 0.03261(19) Uani 1 1 d . . . Cl7 Cl 0.00622(7) -0.30919(6) 0.05033(3) 0.0358(2) Uani 1 1 d . . . Cl8 Cl 0.00529(7) -0.03140(5) 0.14636(4) 0.03720(19) Uani 1 1 d . . . Cl9 Cl 0.34343(6) -0.01269(5) 0.31282(3) 0.03048(19) Uani 1 1 d . . . Cl10 Cl 0.73142(6) 0.23158(5) 0.38896(3) 0.02591(16) Uani 1 1 d . . . Cl11 Cl 0.37527(6) 0.27100(5) 0.42362(3) 0.02613(16) Uani 1 1 d . . . Cl12 Cl 0.68840(5) -0.01887(4) 0.48325(3) 0.02009(15) Uani 1 1 d . . . Cl13 Cl 0.70001(6) 0.28078(5) 0.57505(3) 0.03008(19) Uani 1 1 d . . . C1 C 0.5015(4) -0.1589(3) -0.03028(17) 0.0663(12) Uani 1 1 d . . . H1A H 0.6109 -0.1156 -0.0223 0.099 Uiso 1 1 calc R . . H1B H 0.4522 -0.1081 -0.0119 0.099 Uiso 1 1 calc R . . H1C H 0.4509 -0.1922 -0.0809 0.099 Uiso 1 1 calc R . . C2 C 0.6159(3) -0.2643(3) 0.04854(16) 0.0563(11) Uani 1 1 d . . . H2A H 0.7146 -0.2115 0.0528 0.068 Uiso 1 1 calc R . . C3 C 0.6049(3) -0.3501(3) 0.08344(15) 0.0485(10) Uani 1 1 d . . . H3A H 0.6958 -0.3573 0.1099 0.058 Uiso 1 1 calc R . . C4 C 0.4599(3) -0.4257(2) 0.07945(12) 0.0264(7) Uani 1 1 d . . . C5 C 0.3282(3) -0.4137(2) 0.03834(14) 0.0381(9) Uani 1 1 d . . . H5A H 0.2286 -0.4645 0.0346 0.046 Uiso 1 1 calc R . . C6 C 0.3425(3) -0.3272(2) 0.00258(14) 0.0335(8) Uani 1 1 d . . . H6A H 0.2533 -0.3192 -0.0250 0.040 Uiso 1 1 calc R . . C7 C 0.4431(2) -0.51832(19) 0.11935(12) 0.0244(7) Uani 1 1 d . . . C8 C 0.2977(3) -0.5958(2) 0.11439(13) 0.0404(9) Uani 1 1 d . . . H8A H 0.2066 -0.5916 0.0859 0.048 Uiso 1 1 calc R . . C9 C 0.2878(3) -0.6793(3) 0.15173(14) 0.0446(9) Uani 1 1 d . . . H9A H 0.1890 -0.7312 0.1480 0.053 Uiso 1 1 calc R . . C10 C 0.4022(3) -0.7762(2) 0.23453(15) 0.0473(9) Uani 1 1 d . . . H10A H 0.5054 -0.7691 0.2617 0.071 Uiso 1 1 calc R . . H10B H 0.3503 -0.8521 0.2020 0.071 Uiso 1 1 calc R . . H10C H 0.3419 -0.7647 0.2668 0.071 Uiso 1 1 calc R . . C11 C 0.5561(3) -0.6131(2) 0.19982(18) 0.0539(10) Uani 1 1 d . . . H11A H 0.6452 -0.6169 0.2303 0.065 Uiso 1 1 calc R . . C12 C 0.5735(3) -0.5302(2) 0.16299(18) 0.0508(10) Uani 1 1 d . . . H12A H 0.6741 -0.4807 0.1670 0.061 Uiso 1 1 calc R . . C13 C 0.2366(3) 0.4725(2) 0.50641(14) 0.0365(8) Uani 1 1 d . . . H13A H 0.3450 0.5230 0.5209 0.055 Uiso 1 1 calc R . . H13B H 0.1732 0.5162 0.5184 0.055 Uiso 1 1 calc R . . H13C H 0.2023 0.4388 0.4554 0.055 Uiso 1 1 calc R . . C14 C 0.3460(3) 0.3767(2) 0.59066(14) 0.0373(9) Uani 1 1 d . . . H14A H 0.4440 0.4339 0.5993 0.045 Uiso 1 1 calc R . . C15 C 0.3332(3) 0.2905(2) 0.62619(14) 0.0368(8) Uani 1 1 d . . . H15A H 0.4223 0.2893 0.6582 0.044 Uiso 1 1 calc R . . C16 C 0.1877(2) 0.20527(19) 0.61431(13) 0.0258(7) Uani 1 1 d . . . C17 C 0.0609(3) 0.2118(2) 0.56581(17) 0.0486(10) Uani 1 1 d . . . H17A H -0.0385 0.1556 0.5558 0.058 Uiso 1 1 calc R . . C18 C 0.0794(3) 0.2997(2) 0.53219(17) 0.0477(10) Uani 1 1 d . . . H18A H -0.0081 0.3035 0.5005 0.057 Uiso 1 1 calc R . . C19 C 0.1700(2) 0.10922(19) 0.65118(12) 0.0241(7) Uani 1 1 d . . . C20 C 0.2985(3) 0.0967(2) 0.69531(17) 0.0454(10) Uani 1 1 d . . . H20A H 0.3989 0.1495 0.7025 0.054 Uiso 1 1 calc R . . C21 C 0.2811(3) 0.0083(2) 0.72863(17) 0.0469(10) Uani 1 1 d . . . H21A H 0.3691 0.0018 0.7582 0.056 Uiso 1 1 calc R . . C22 C 0.1204(3) -0.1650(2) 0.75369(15) 0.0390(9) Uani 1 1 d . . . H22A H 0.2222 -0.1582 0.7822 0.059 Uiso 1 1 calc R . . H22B H 0.0742 -0.2377 0.7176 0.059 Uiso 1 1 calc R . . H22C H 0.0538 -0.1616 0.7841 0.059 Uiso 1 1 calc R . . C23 C 0.0107(3) -0.0602(3) 0.67505(15) 0.0459(10) Uani 1 1 d . . . H23A H -0.0886 -0.1147 0.6678 0.055 Uiso 1 1 calc R . . C24 C 0.0248(3) 0.0274(2) 0.64099(14) 0.0394(9) Uani 1 1 d . . . H24A H -0.0645 0.0314 0.6108 0.047 Uiso 1 1 calc R . . N1 N 0.4864(2) -0.25488(19) 0.00816(11) 0.0386(7) Uani 1 1 d . . . N2 N 0.4161(2) -0.68842(17) 0.19349(10) 0.0315(6) Uani 1 1 d . . . N3 N 0.2203(2) 0.37967(15) 0.54406(10) 0.0253(6) Uani 1 1 d . . . N4 N 0.13712(19) -0.06896(16) 0.71860(10) 0.0254(6) Uani 1 1 d . . . O1W O 0.8602(5) -0.0987(4) -0.0334(2) 0.0658(16) Uani 0.50 1 d P . . O2W O -0.1164(6) -0.8671(4) 0.0541(2) 0.0878(19) Uani 0.50 1 d P . . 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 0.01457(3) 0.01480(3) 0.01749(4) 0.00093(3) 0.00163(3) 0.00292(3) Bi2 0.01673(3) 0.01355(3) 0.01714(4) -0.00086(3) 0.00160(3) 0.00293(3) Bi3 0.01198(3) 0.00969(3) 0.01612(3) 0.00030(3) 0.00213(3) 0.00218(2) Cl1 0.0263(2) 0.0286(3) 0.0340(3) 0.0081(2) 0.0142(2) 0.0015(2) Cl2 0.0300(3) 0.0356(3) 0.0244(3) -0.0085(3) -0.0034(2) 0.0074(2) Cl3 0.0305(2) 0.0280(3) 0.0335(3) 0.0034(2) 0.0015(2) 0.0167(2) Cl4 0.0194(2) 0.0223(2) 0.0248(3) 0.0016(2) 0.00689(19) 0.00518(19) Cl5 0.0181(2) 0.0219(2) 0.0311(3) 0.0051(2) 0.0060(2) 0.00692(18) Cl6 0.0340(3) 0.0311(3) 0.0287(3) 0.0058(2) 0.0139(2) 0.0040(2) Cl7 0.0275(3) 0.0345(3) 0.0280(3) -0.0111(3) -0.0013(2) 0.0046(2) Cl8 0.0400(3) 0.0342(3) 0.0406(3) 0.0047(3) 0.0095(2) 0.0220(2) Cl9 0.0291(3) 0.0250(3) 0.0266(3) -0.0039(3) 0.0026(2) 0.0046(2) Cl10 0.0213(2) 0.0243(3) 0.0323(3) 0.0085(2) 0.0126(2) 0.0044(2) Cl11 0.0271(2) 0.0226(2) 0.0306(3) 0.0050(2) 0.0046(2) 0.01526(18) Cl12 0.0160(2) 0.0170(2) 0.0272(3) 0.0046(2) 0.00719(19) 0.00577(17) Cl13 0.0256(3) 0.0249(3) 0.0266(3) -0.0039(2) 0.0000(2) 0.0023(2) C1 0.105(2) 0.0492(17) 0.0568(17) 0.0202(14) 0.0460(15) 0.0255(16) C2 0.0359(13) 0.083(2) 0.0468(16) 0.0260(15) 0.0146(12) 0.0096(14) C3 0.0198(11) 0.0739(19) 0.0425(15) 0.0169(14) 0.0034(11) 0.0073(12) C4 0.0271(10) 0.0259(11) 0.0176(11) -0.0065(9) -0.0009(9) 0.0096(8) C5 0.0332(12) 0.0273(12) 0.0449(15) 0.0014(11) -0.0012(11) 0.0121(9) C6 0.0333(11) 0.0252(11) 0.0399(14) 0.0025(11) 0.0107(10) 0.0107(9) C7 0.0168(9) 0.0241(11) 0.0237(11) -0.0079(9) 0.0025(8) 0.0060(8) C8 0.0195(10) 0.0713(17) 0.0317(12) 0.0244(12) 0.0080(9) 0.0118(11) C9 0.0229(12) 0.0623(17) 0.0407(14) 0.0205(13) 0.0055(11) 0.0034(12) C10 0.0647(15) 0.0386(13) 0.0387(15) 0.0030(12) 0.0077(13) 0.0280(11) C11 0.0192(11) 0.0351(13) 0.083(2) 0.0075(14) -0.0243(13) 0.0084(10) C12 0.0164(11) 0.0261(13) 0.089(2) 0.0108(14) -0.0129(13) 0.0018(10) C13 0.0323(12) 0.0266(12) 0.0391(14) -0.0011(11) 0.0004(11) 0.0073(10) C14 0.0236(11) 0.0448(14) 0.0376(13) 0.0126(11) 0.0071(10) 0.0045(10) C15 0.0169(10) 0.0531(15) 0.0337(13) 0.0160(11) 0.0039(10) 0.0031(10) C16 0.0192(9) 0.0238(11) 0.0268(12) -0.0078(10) 0.0024(9) 0.0082(8) C17 0.0166(11) 0.0254(13) 0.083(2) 0.0111(13) -0.0089(13) -0.0022(10) C18 0.0199(11) 0.0237(12) 0.079(2) 0.0112(13) -0.0147(13) 0.0025(10) C19 0.0187(9) 0.0220(10) 0.0270(12) -0.0037(9) 0.0037(9) 0.0084(8) C20 0.0177(11) 0.0251(12) 0.0728(19) 0.0053(13) -0.0118(12) 0.0013(10) C21 0.0303(12) 0.0286(12) 0.0732(19) 0.0175(12) -0.0057(13) 0.0113(10) C22 0.0418(12) 0.0279(13) 0.0465(15) 0.0037(11) 0.0200(11) 0.0095(10) C23 0.0197(12) 0.0641(17) 0.0414(14) 0.0223(13) 0.0004(11) -0.0008(12) C24 0.0156(10) 0.0588(16) 0.0382(13) 0.0219(12) 0.0037(10) 0.0036(11) N1 0.0494(10) 0.0454(12) 0.0251(10) 0.0058(9) 0.0196(8) 0.0181(9) N2 0.0359(9) 0.0304(10) 0.0230(10) -0.0037(8) 0.0013(8) 0.0157(7) N3 0.0229(8) 0.0194(9) 0.0286(10) -0.0032(8) 0.0015(7) 0.0101(7) N4 0.0237(8) 0.0208(9) 0.0305(10) -0.0013(8) 0.0136(7) 0.0067(7) O1W 0.071(2) 0.068(2) 0.066(2) 0.0425(19) 0.0314(19) 0.013(2) O2W 0.146(3) 0.082(2) 0.045(2) 0.028(2) 0.001(2) 0.066(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Bi1 Cl1 2.5299(8) . ? Bi1 Cl3 2.5458(8) . ? Bi1 Cl2 2.5542(9) . ? Bi1 Cl4 2.9148(8) . ? Bi1 Cl5 2.9161(8) . ? Bi1 Cl13 2.9537(10) 2_656 ? Bi2 Cl7 2.5923(9) . ? Bi2 Cl8 2.6263(9) . ? Bi2 Cl6 2.6448(8) . ? Bi2 Cl5 2.7857(8) . ? Bi2 Cl4 2.8081(8) . ? Bi2 Cl9 2.8386(9) . ? Bi3 Cl11 2.5651(8) . ? Bi3 Cl10 2.5653(8) . ? Bi3 Cl13 2.6599(9) . ? Bi3 Cl9 2.7866(9) . ? Bi3 Cl12 2.8364(8) 2_656 ? Bi3 Cl12 2.8704(8) . ? Cl12 Bi3 2.8364(8) 2_656 ? Cl13 Bi1 2.9537(10) 2_656 ? C1 N1 1.516(4) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 N1 1.340(4) . ? C2 C3 1.363(5) . ? C2 H2A 0.9300 . ? C3 C4 1.370(3) . ? C3 H3A 0.9300 . ? C4 C5 1.378(4) . ? C4 C7 1.500(4) . ? C5 C6 1.381(4) . ? C5 H5A 0.9300 . ? C6 N1 1.338(3) . ? C6 H6A 0.9300 . ? C7 C8 1.377(3) . ? C7 C12 1.389(4) . ? C8 C9 1.372(4) . ? C8 H8A 0.9300 . ? C9 N2 1.341(3) . ? C9 H9A 0.9300 . ? C10 N2 1.465(4) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 N2 1.321(3) . ? C11 C12 1.357(5) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? C13 N3 1.472(4) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 N3 1.334(3) . ? C14 C15 1.376(4) . ? C14 H14A 0.9300 . ? C15 C16 1.386(3) . ? C15 H15A 0.9300 . ? C16 C17 1.379(4) . ? C16 C19 1.496(4) . ? C17 C18 1.367(4) . ? C17 H17A 0.9300 . ? C18 N3 1.328(3) . ? C18 H18A 0.9300 . ? C19 C24 1.373(3) . ? C19 C20 1.384(4) . ? C20 C21 1.369(4) . ? C20 H20A 0.9300 . ? C21 N4 1.341(3) . ? C21 H21A 0.9300 . ? C22 N4 1.473(4) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 N4 1.341(3) . ? C23 C24 1.370(4) . ? C23 H23A 0.9300 . ? C24 H24A 0.9300 . ? 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 Cl1 Bi1 Cl3 93.16(3) . . ? Cl1 Bi1 Cl2 89.62(3) . . ? Cl3 Bi1 Cl2 89.31(3) . . ? Cl1 Bi1 Cl4 173.94(2) . . ? Cl3 Bi1 Cl4 92.89(3) . . ? Cl2 Bi1 Cl4 90.19(3) . . ? Cl1 Bi1 Cl5 92.39(3) . . ? Cl3 Bi1 Cl5 173.85(2) . . ? Cl2 Bi1 Cl5 88.09(3) . . ? Cl4 Bi1 Cl5 81.55(2) . . ? Cl1 Bi1 Cl13 87.32(3) . 2_656 ? Cl3 Bi1 Cl13 85.94(2) . 2_656 ? Cl2 Bi1 Cl13 174.20(2) . 2_656 ? Cl4 Bi1 Cl13 93.37(3) . 2_656 ? Cl5 Bi1 Cl13 96.96(2) . 2_656 ? Cl7 Bi2 Cl8 89.36(3) . . ? Cl7 Bi2 Cl6 90.65(3) . . ? Cl8 Bi2 Cl6 92.08(3) . . ? Cl7 Bi2 Cl5 89.35(3) . . ? Cl8 Bi2 Cl5 90.04(3) . . ? Cl6 Bi2 Cl5 177.88(2) . . ? Cl7 Bi2 Cl4 90.54(3) . . ? Cl8 Bi2 Cl4 175.848(19) . . ? Cl6 Bi2 Cl4 92.07(3) . . ? Cl5 Bi2 Cl4 85.81(3) . . ? Cl7 Bi2 Cl9 178.26(2) . . ? Cl8 Bi2 Cl9 91.88(3) . . ? Cl6 Bi2 Cl9 90.53(3) . . ? Cl5 Bi2 Cl9 89.42(3) . . ? Cl4 Bi2 Cl9 88.14(2) . . ? Cl11 Bi3 Cl10 92.14(3) . . ? Cl11 Bi3 Cl13 90.27(3) . . ? Cl10 Bi3 Cl13 90.49(3) . . ? Cl11 Bi3 Cl9 88.21(2) . . ? Cl10 Bi3 Cl9 88.36(3) . . ? Cl13 Bi3 Cl9 178.05(2) . . ? Cl11 Bi3 Cl12 91.65(3) . 2_656 ? Cl10 Bi3 Cl12 176.137(19) . 2_656 ? Cl13 Bi3 Cl12 88.73(3) . 2_656 ? Cl9 Bi3 Cl12 92.53(3) . 2_656 ? Cl11 Bi3 Cl12 176.432(19) . . ? Cl10 Bi3 Cl12 90.85(3) . . ? Cl13 Bi3 Cl12 87.75(2) . . ? Cl9 Bi3 Cl12 93.83(2) . . ? Cl12 Bi3 Cl12 85.34(2) 2_656 . ? Bi2 Cl4 Bi1 95.99(2) . . ? Bi2 Cl5 Bi1 96.45(3) . . ? Bi3 Cl9 Bi2 177.82(3) . . ? Bi3 Cl12 Bi3 94.66(2) 2_656 . ? Bi3 Cl13 Bi1 177.83(3) . 2_656 ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 120.9(2) . . ? N1 C2 H2A 119.6 . . ? C3 C2 H2A 119.6 . . ? C2 C3 C4 119.9(3) . . ? C2 C3 H3A 120.0 . . ? C4 C3 H3A 120.0 . . ? C3 C4 C5 118.2(3) . . ? C3 C4 C7 121.4(2) . . ? C5 C4 C7 120.4(2) . . ? C4 C5 C6 120.8(2) . . ? C4 C5 H5A 119.6 . . ? C6 C5 H5A 119.6 . . ? N1 C6 C5 119.1(2) . . ? N1 C6 H6A 120.5 . . ? C5 C6 H6A 120.5 . . ? C8 C7 C12 116.8(3) . . ? C8 C7 C4 121.6(2) . . ? C12 C7 C4 121.6(2) . . ? C9 C8 C7 119.6(2) . . ? C9 C8 H8A 120.2 . . ? C7 C8 H8A 120.2 . . ? N2 C9 C8 122.2(2) . . ? N2 C9 H9A 118.9 . . ? C8 C9 H9A 118.9 . . ? N2 C10 H10A 109.5 . . ? N2 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N2 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N2 C11 C12 121.7(2) . . ? N2 C11 H11A 119.1 . . ? C12 C11 H11A 119.1 . . ? C11 C12 C7 120.9(2) . . ? C11 C12 H12A 119.6 . . ? C7 C12 H12A 119.6 . . ? N3 C13 H13A 109.5 . . ? N3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N3 C14 C15 121.1(2) . . ? N3 C14 H14A 119.5 . . ? C15 C14 H14A 119.5 . . ? C14 C15 C16 120.1(2) . . ? C14 C15 H15A 120.0 . . ? C16 C15 H15A 120.0 . . ? C17 C16 C15 116.9(3) . . ? C17 C16 C19 121.60(19) . . ? C15 C16 C19 121.5(2) . . ? C18 C17 C16 120.8(2) . . ? C18 C17 H17A 119.6 . . ? C16 C17 H17A 119.6 . . ? N3 C18 C17 121.0(2) . . ? N3 C18 H18A 119.5 . . ? C17 C18 H18A 119.5 . . ? C24 C19 C20 117.0(3) . . ? C24 C19 C16 121.1(2) . . ? C20 C19 C16 121.9(2) . . ? C21 C20 C19 121.5(2) . . ? C21 C20 H20A 119.3 . . ? C19 C20 H20A 119.3 . . ? N4 C21 C20 120.0(2) . . ? N4 C21 H21A 120.0 . . ? C20 C21 H21A 120.0 . . ? N4 C22 H22A 109.5 . . ? N4 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N4 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N4 C23 C24 121.4(2) . . ? N4 C23 H23A 119.3 . . ? C24 C23 H23A 119.3 . . ? C23 C24 C19 120.3(2) . . ? C23 C24 H24A 119.8 . . ? C19 C24 H24A 119.8 . . ? C6 N1 C2 121.1(3) . . ? C6 N1 C1 118.9(2) . . ? C2 N1 C1 120.0(2) . . ? C11 N2 C9 118.8(3) . . ? C11 N2 C10 120.1(2) . . ? C9 N2 C10 121.1(2) . . ? C18 N3 C14 120.0(2) . . ? C18 N3 C13 119.7(2) . . ? C14 N3 C13 120.22(19) . . ? C21 N4 C23 119.8(2) . . ? C21 N4 C22 119.5(2) . . ? C23 N4 C22 120.7(2) . . ? _diffrn_measured_fraction_theta_max 0.950 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.950 _refine_diff_density_max 1.847 _refine_diff_density_min -1.212 _refine_diff_density_rms 0.149