# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Xiao, Xin' _publ_contact_author_email gyhxxiaoxin@163.com _publ_section_title ; Coordination Polymers Constructed from Alkali Metal Ions and (HO)10cucurbit[5]uril ; _publ_author_name 'Xin Xiao' # Attachment '- complex1-3.cif' data_complex1 _database_code_depnum_ccdc_archive 'CCDC 806941' #TrackingRef '- complex1-3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H50 Cl K2 N21 O33' _chemical_formula_weight 1346.56 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.8265(8) _cell_length_b 14.2642(8) _cell_length_c 25.1428(14) _cell_angle_alpha 90.00 _cell_angle_beta 92.711(2) _cell_angle_gamma 90.00 _cell_volume 4953.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6731 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 26.89 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.806 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2784 _exptl_absorpt_coefficient_mu 0.375 _exptl_absorpt_correction_type 'multi scan' _exptl_absorpt_correction_T_min 0.8708 _exptl_absorpt_correction_T_max 0.9188 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 Smart Apex CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 29070 _diffrn_reflns_av_R_equivalents 0.0200 _diffrn_reflns_av_sigmaI/netI 0.0212 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 26.00 _reflns_number_total 9640 _reflns_number_gt 8258 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1221P)^2^+19.8015P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9640 _refine_ls_number_parameters 784 _refine_ls_number_restraints 288 _refine_ls_R_factor_all 0.0852 _refine_ls_R_factor_gt 0.0764 _refine_ls_wR_factor_ref 0.2276 _refine_ls_wR_factor_gt 0.2185 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.244 _refine_ls_shift/su_max 0.064 _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 K1 K 0.49419(8) -0.04274(7) 0.84872(4) 0.0247(3) Uani 1 1 d . . . K2 K 0.01350(8) 0.11739(7) 0.81917(4) 0.0237(3) Uani 1 1 d . . . Cl1 Cl 0.11142(11) 0.13986(11) 0.54259(7) 0.0443(4) Uani 1 1 d . . . C1 C 0.4159(3) 0.1465(3) 0.93394(18) 0.0186(9) Uani 1 1 d . . . C2 C 0.3141(3) 0.2782(3) 0.93644(18) 0.0189(9) Uani 1 1 d . . . C3 C 0.2824(3) 0.2030(3) 0.97824(17) 0.0175(9) Uani 1 1 d . . . C4 C 0.1507(3) 0.2392(3) 0.91914(18) 0.0185(9) Uani 1 1 d . . . C5 C 0.3548(3) 0.0453(3) 1.00560(18) 0.0188(9) Uani 1 1 d . . . H5A H 0.3346 0.0612 1.0418 0.023 Uiso 1 1 calc R . . H5B H 0.4223 0.0222 1.0090 0.023 Uiso 1 1 calc R . . C6 C 0.1191(3) 0.1216(3) 0.98816(18) 0.0188(9) Uani 1 1 d . . . H6A H 0.0519 0.1440 0.9812 0.023 Uiso 1 1 calc R . . H6B H 0.1349 0.1283 1.0268 0.023 Uiso 1 1 calc R . . C7 C 0.1939(3) -0.0428(3) 0.99697(17) 0.0180(9) Uani 1 1 d . . . C8 C 0.3289(3) -0.1021(3) 0.95511(17) 0.0179(9) Uani 1 1 d . . . C9 C 0.0618(3) -0.0176(3) 0.93684(17) 0.0187(9) Uani 1 1 d . . . C10 C 0.1657(3) -0.1377(3) 0.96788(18) 0.0189(9) Uani 1 1 d . . . C11 C 0.2640(3) -0.2464(3) 0.91091(18) 0.0206(9) Uani 1 1 d . . . H11A H 0.3317 -0.2691 0.9145 0.025 Uiso 1 1 calc R . . H11B H 0.2218 -0.2966 0.9240 0.025 Uiso 1 1 calc R . . C12 C 0.0316(3) -0.1740(3) 0.89667(18) 0.0203(9) Uani 1 1 d . . . H12A H -0.0363 -0.1518 0.8932 0.024 Uiso 1 1 calc R . . H12B H 0.0313 -0.2363 0.9140 0.024 Uiso 1 1 calc R . . C13 C 0.1447(3) -0.2485(3) 0.83047(18) 0.0185(9) Uani 1 1 d . . . C14 C 0.3078(3) -0.2098(3) 0.81915(18) 0.0191(9) Uani 1 1 d . . . C15 C 0.0389(3) -0.1283(3) 0.80175(18) 0.0182(9) Uani 1 1 d . . . C16 C 0.1600(3) -0.2255(3) 0.77000(18) 0.0178(9) Uani 1 1 d . . . C17 C 0.3124(3) -0.1846(3) 0.72185(18) 0.0204(9) Uani 1 1 d . . . H17A H 0.2846 -0.2258 0.6934 0.024 Uiso 1 1 calc R . . H17B H 0.3810 -0.2027 0.7286 0.024 Uiso 1 1 calc R . . C18 C 0.0733(3) -0.1094(3) 0.70661(18) 0.0183(9) Uani 1 1 d . . . H18A H 0.0064 -0.0843 0.7047 0.022 Uiso 1 1 calc R . . H18B H 0.0767 -0.1598 0.6797 0.022 Uiso 1 1 calc R . . C19 C 0.2315(3) -0.0493(3) 0.66937(18) 0.0185(9) Uani 1 1 d . . . C20 C 0.3816(3) -0.0256(3) 0.71417(17) 0.0182(9) Uani 1 1 d . . . C21 C 0.1153(3) 0.0572(3) 0.69671(17) 0.0173(9) Uani 1 1 d . . . C22 C 0.2679(3) 0.0546(3) 0.66012(18) 0.0184(9) Uani 1 1 d . . . C23 C 0.4234(3) 0.1390(3) 0.69356(18) 0.0196(9) Uani 1 1 d . . . H23A H 0.4910 0.1162 0.6977 0.024 Uiso 1 1 calc R . . H23B H 0.4166 0.1733 0.6594 0.024 Uiso 1 1 calc R . . C24 C 0.1886(3) 0.2122(3) 0.68053(18) 0.0183(9) Uani 1 1 d . . . H24A H 0.2209 0.2359 0.6489 0.022 Uiso 1 1 calc R . . H24B H 0.1205 0.2338 0.6778 0.022 Uiso 1 1 calc R . . C25 C 0.3365(3) 0.2794(3) 0.73281(18) 0.0178(9) Uani 1 1 d . . . C26 C 0.4524(3) 0.1969(3) 0.78545(18) 0.0193(9) Uani 1 1 d . . . C27 C 0.1856(3) 0.2755(3) 0.77225(18) 0.0187(9) Uani 1 1 d . . . C28 C 0.3458(3) 0.3242(3) 0.79062(18) 0.0192(9) Uani 1 1 d . . . C29 C 0.4516(3) 0.2770(3) 0.87266(18) 0.0208(9) Uani 1 1 d . . . H29A H 0.4541 0.3445 0.8819 0.025 Uiso 1 1 calc R . . H29B H 0.5181 0.2516 0.8779 0.025 Uiso 1 1 calc R . . C30 C 0.2186(3) 0.3562(3) 0.85827(19) 0.0210(9) Uani 1 1 d . . . H30A H 0.1505 0.3766 0.8523 0.025 Uiso 1 1 calc R . . H30B H 0.2582 0.4129 0.8656 0.025 Uiso 1 1 calc R . . N1 N 0.3890(3) 0.2294(3) 0.90898(15) 0.0199(8) Uani 1 1 d . . . N2 N 0.2253(3) 0.2957(3) 0.90501(15) 0.0200(8) Uani 1 1 d . . . N3 N 0.3523(3) 0.1298(3) 0.97346(15) 0.0189(8) Uani 1 1 d . . . N4 N 0.1838(3) 0.1803(3) 0.95938(15) 0.0192(8) Uani 1 1 d . . . N5 N 0.2933(3) -0.0293(3) 0.98437(15) 0.0193(8) Uani 1 1 d . . . N6 N 0.1241(3) 0.0229(3) 0.97387(15) 0.0184(8) Uani 1 1 d . . . N7 N 0.2545(3) -0.1640(3) 0.94418(15) 0.0198(8) Uani 1 1 d . . . N8 N 0.0866(3) -0.1098(3) 0.93067(15) 0.0192(8) Uani 1 1 d . . . N9 N 0.2390(3) -0.2297(3) 0.85524(16) 0.0196(8) Uani 1 1 d . . . N10 N 0.0683(3) -0.1843(3) 0.84363(15) 0.0197(8) Uani 1 1 d . . . N11 N 0.2609(3) -0.2001(3) 0.76986(16) 0.0202(8) Uani 1 1 d . . . N12 N 0.0933(3) -0.1493(3) 0.75905(15) 0.0174(8) Uani 1 1 d . . . N13 N 0.3083(3) -0.0879(3) 0.70336(16) 0.0200(8) Uani 1 1 d . . . N14 N 0.1395(3) -0.0350(3) 0.69332(15) 0.0183(8) Uani 1 1 d . . . N15 N 0.3584(3) 0.0584(3) 0.69137(15) 0.0177(8) Uani 1 1 d . . . N16 N 0.1898(3) 0.1103(3) 0.67949(15) 0.0187(8) Uani 1 1 d . . . N17 N 0.4054(3) 0.2031(3) 0.73657(15) 0.0190(8) Uani 1 1 d . . . N18 N 0.2357(3) 0.2528(3) 0.72790(15) 0.0181(8) Uani 1 1 d . . . N19 N 0.4207(3) 0.2674(3) 0.81691(15) 0.0206(8) Uani 1 1 d . . . N20 N 0.2498(3) 0.3132(3) 0.81022(16) 0.0211(8) Uani 1 1 d . . . O1 O 0.4847(2) 0.0983(2) 0.92343(13) 0.0242(7) Uani 1 1 d U . . O2 O 0.4123(2) -0.1112(2) 0.94269(13) 0.0226(7) Uani 1 1 d U . . O3 O 0.3943(2) -0.2029(2) 0.82891(14) 0.0265(7) Uani 1 1 d U . . O4 O 0.4571(2) -0.0440(2) 0.73965(13) 0.0238(7) Uani 1 1 d U . . O5 O 0.5160(3) 0.1403(2) 0.79799(14) 0.0267(7) Uani 1 1 d U . . O6 O 0.0677(2) 0.2415(2) 0.90015(13) 0.0233(7) Uani 1 1 d U . . O7 O -0.0077(2) 0.0214(2) 0.91388(13) 0.0213(7) Uani 1 1 d U . . O8 O -0.0261(2) -0.0705(2) 0.80150(13) 0.0233(7) Uani 1 1 d U . . O9 O 0.0381(2) 0.0874(2) 0.71202(13) 0.0206(7) Uani 1 1 d U . . O10 O 0.0992(2) 0.2667(2) 0.77668(13) 0.0221(7) Uani 1 1 d U . . O11 O 0.3534(3) 0.3585(3) 0.95947(16) 0.0331(8) Uani 1 1 d U . . H11 H 0.3989 0.3438 0.9812 0.050 Uiso 1 1 calc R . . O12 O 0.2837(2) 0.2330(2) 1.03077(13) 0.0244(7) Uani 1 1 d U . . H12 H 0.3391 0.2533 1.0398 0.037 Uiso 1 1 calc R . . O13 O 0.1898(2) -0.0458(2) 1.05215(13) 0.0239(7) Uani 1 1 d U . . H13 H 0.1322 -0.0537 1.0604 0.036 Uiso 1 1 calc R . . O14 O 0.1311(3) -0.2067(2) 1.00025(14) 0.0264(7) Uani 1 1 d U . . H14 H 0.1723 -0.2180 1.0250 0.040 Uiso 1 1 calc R . . O15 O 0.1217(3) -0.3409(2) 0.84113(14) 0.0250(7) Uani 1 1 d U . . H15 H 0.0669 -0.3535 0.8271 0.037 Uiso 1 1 calc R . . O16 O 0.1381(3) -0.2990(2) 0.73534(13) 0.0250(7) Uani 1 1 d U . . O17 O 0.2211(3) -0.1045(3) 0.62415(14) 0.0302(8) Uani 1 1 d U . . H17 H 0.1767 -0.0827 0.6038 0.045 Uiso 1 1 calc R . . O18 O 0.2866(3) 0.0770(3) 0.60805(13) 0.0256(7) Uani 1 1 d U . . H18 H 0.2349 0.0751 0.5892 0.038 Uiso 1 1 calc R . . O19 O 0.3605(2) 0.3390(2) 0.69173(13) 0.0227(7) Uani 1 1 d U . . O20 O 0.3677(2) 0.4188(2) 0.79226(14) 0.0246(7) Uani 1 1 d U . . H20 H 0.4233 0.4273 0.7811 0.037 Uiso 1 1 calc R . . O1W O 0.2918(3) -0.2466(3) 0.56326(18) 0.0446(10) Uani 1 1 d U . . H1WA H 0.3139 -0.2915 0.5824 0.054 Uiso 1 1 d R . . H1WB H 0.3388 -0.2187 0.5495 0.054 Uiso 1 1 d R . . O2W O 0.6718(3) 0.0859(4) 0.86400(18) 0.0496(12) Uani 1 1 d U . . O3W O 0.4755(3) 0.2818(3) 1.06566(19) 0.0495(11) Uani 1 1 d U . . H3WA H 0.5028 0.2284 1.0668 0.059 Uiso 1 1 d R . . H3WB H 0.5036 0.3154 1.0432 0.059 Uiso 1 1 d R . . O4W O 0.2060(4) 0.4252(4) 0.6507(2) 0.0635(15) Uani 1 1 d U . . O5W O 0.4162(4) -0.1327(4) 0.5092(2) 0.0632(13) Uani 1 1 d U . . O6W O 0.0547(4) -0.1082(4) 0.5710(2) 0.0616(13) Uani 1 1 d U . . O7W O 0.2851(7) 0.5248(4) 0.9504(4) 0.106(3) Uani 1 1 d U . . O8W O 0.4730(5) -0.0014(4) 0.5855(2) 0.0691(14) Uani 1 1 d U . . O9W O 0.0999(5) -0.0433(5) 0.4680(3) 0.094(2) Uani 1 1 d U . . O10W O 0.2830(6) -0.4172(5) 0.7488(3) 0.105(2) Uani 1 1 d U . . H10A H 0.3081 -0.4665 0.7624 0.126 Uiso 1 1 d R . . H10B H 0.2955 -0.4156 0.7160 0.126 Uiso 1 1 d R . . N21 N 0.2454(3) 0.0403(3) 0.83295(14) 0.0291(7) Uani 1 1 d . . . O23 O 0.3183(5) 0.0050(6) 0.8462(3) 0.0682(16) Uani 1 1 d U . . O22 O 0.2339(6) 0.0834(6) 0.7947(3) 0.0761(17) Uani 1 1 d U . . O21 O 0.1742(6) 0.0211(6) 0.8553(3) 0.0718(19) Uani 1 1 d U . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 K1 0.0235(5) 0.0272(5) 0.0236(5) -0.0022(4) 0.0028(4) -0.0007(4) K2 0.0298(6) 0.0209(5) 0.0202(5) 0.0029(4) -0.0009(4) -0.0017(4) Cl1 0.0379(8) 0.0450(8) 0.0496(9) 0.0077(7) -0.0034(6) -0.0021(6) C1 0.016(2) 0.022(2) 0.017(2) -0.0036(17) -0.0002(16) -0.0029(17) C2 0.018(2) 0.020(2) 0.019(2) -0.0021(17) 0.0011(17) -0.0019(17) C3 0.017(2) 0.020(2) 0.016(2) -0.0040(16) 0.0020(16) -0.0012(17) C4 0.020(2) 0.018(2) 0.017(2) -0.0027(16) 0.0042(17) -0.0002(17) C5 0.018(2) 0.022(2) 0.016(2) -0.0006(17) -0.0018(16) -0.0015(17) C6 0.017(2) 0.020(2) 0.019(2) -0.0003(17) 0.0037(17) 0.0001(17) C7 0.017(2) 0.021(2) 0.017(2) 0.0018(16) 0.0011(16) -0.0015(17) C8 0.020(2) 0.019(2) 0.014(2) 0.0032(16) -0.0022(16) -0.0008(17) C9 0.015(2) 0.027(2) 0.014(2) 0.0011(17) 0.0046(16) -0.0037(18) C10 0.018(2) 0.021(2) 0.017(2) 0.0023(17) -0.0009(17) -0.0019(17) C11 0.023(2) 0.017(2) 0.021(2) 0.0018(17) -0.0040(18) 0.0003(17) C12 0.017(2) 0.026(2) 0.018(2) -0.0020(18) 0.0027(17) -0.0066(18) C13 0.018(2) 0.017(2) 0.021(2) -0.0009(17) -0.0029(17) -0.0014(17) C14 0.020(2) 0.0138(19) 0.023(2) -0.0015(17) 0.0006(17) 0.0016(17) C15 0.015(2) 0.018(2) 0.021(2) -0.0023(17) -0.0026(17) -0.0038(17) C16 0.017(2) 0.014(2) 0.022(2) -0.0016(16) 0.0002(17) -0.0005(16) C17 0.021(2) 0.017(2) 0.023(2) 0.0008(17) 0.0052(18) 0.0030(17) C18 0.017(2) 0.016(2) 0.022(2) 0.0000(17) -0.0001(17) -0.0026(16) C19 0.016(2) 0.021(2) 0.019(2) -0.0008(17) 0.0020(16) 0.0016(17) C20 0.017(2) 0.021(2) 0.017(2) 0.0011(17) 0.0044(17) 0.0034(17) C21 0.017(2) 0.019(2) 0.016(2) 0.0010(16) -0.0018(16) 0.0005(17) C22 0.016(2) 0.022(2) 0.017(2) 0.0027(17) 0.0001(16) 0.0009(17) C23 0.015(2) 0.021(2) 0.022(2) 0.0008(17) 0.0026(17) -0.0016(17) C24 0.019(2) 0.016(2) 0.020(2) 0.0033(16) -0.0016(17) 0.0002(17) C25 0.017(2) 0.017(2) 0.019(2) 0.0025(16) 0.0022(16) -0.0037(17) C26 0.014(2) 0.023(2) 0.021(2) 0.0025(17) 0.0010(17) -0.0052(17) C27 0.018(2) 0.014(2) 0.023(2) 0.0038(17) 0.0005(17) 0.0006(16) C28 0.016(2) 0.021(2) 0.021(2) 0.0022(17) 0.0027(17) -0.0027(17) C29 0.018(2) 0.027(2) 0.018(2) -0.0003(18) 0.0009(17) -0.0057(18) C30 0.020(2) 0.019(2) 0.023(2) 0.0033(18) 0.0021(18) 0.0011(17) N1 0.0168(19) 0.0228(19) 0.0203(19) 0.0023(15) 0.0028(15) -0.0001(15) N2 0.0169(19) 0.0223(19) 0.0207(19) 0.0027(15) 0.0026(15) 0.0016(15) N3 0.0176(19) 0.0204(19) 0.0188(19) -0.0007(15) 0.0019(14) -0.0006(15) N4 0.0151(18) 0.0233(19) 0.0194(19) 0.0001(15) 0.0006(14) -0.0017(15) N5 0.0155(19) 0.0214(19) 0.0211(19) -0.0022(15) 0.0008(14) -0.0017(15) N6 0.0182(19) 0.0201(19) 0.0168(18) 0.0006(14) -0.0011(14) -0.0019(15) N7 0.0199(19) 0.0191(18) 0.0203(19) 0.0008(15) -0.0004(15) -0.0012(15) N8 0.0165(19) 0.0214(19) 0.0195(19) 0.0005(15) -0.0020(15) -0.0019(15) N9 0.0158(19) 0.0213(19) 0.021(2) -0.0005(15) -0.0019(15) -0.0023(15) N10 0.0165(19) 0.0220(19) 0.0207(19) -0.0004(15) 0.0009(15) -0.0002(15) N11 0.0164(19) 0.0217(19) 0.023(2) 0.0006(15) 0.0025(15) -0.0001(15) N12 0.0163(18) 0.0182(18) 0.0176(18) 0.0023(14) 0.0006(14) 0.0020(14) N13 0.0165(19) 0.0184(18) 0.025(2) 0.0024(15) 0.0005(15) 0.0028(14) N14 0.0168(19) 0.0174(18) 0.0211(19) 0.0005(14) 0.0029(14) -0.0007(14) N15 0.0128(18) 0.0191(18) 0.0211(19) 0.0019(15) 0.0000(14) 0.0001(14) N16 0.0158(19) 0.0170(18) 0.0233(19) 0.0025(15) 0.0015(15) 0.0004(14) N17 0.0156(18) 0.0209(19) 0.0204(19) 0.0020(15) 0.0007(14) 0.0008(15) N18 0.0147(18) 0.0205(18) 0.0190(19) 0.0026(15) 0.0012(14) -0.0018(14) N19 0.0196(19) 0.025(2) 0.0175(19) 0.0025(15) 0.0000(15) -0.0024(15) N20 0.0173(19) 0.025(2) 0.021(2) 0.0000(15) 0.0031(15) -0.0041(15) O1 0.0203(16) 0.0282(17) 0.0243(17) -0.0001(13) 0.0035(13) 0.0036(13) O2 0.0171(16) 0.0250(16) 0.0259(17) -0.0021(13) 0.0016(13) 0.0000(13) O3 0.0163(16) 0.0280(17) 0.0352(19) 0.0014(14) -0.0001(13) 0.0014(13) O4 0.0180(16) 0.0293(17) 0.0242(16) 0.0013(13) 0.0009(13) 0.0051(13) O5 0.0241(17) 0.0294(17) 0.0260(17) 0.0023(14) -0.0048(13) 0.0044(14) O6 0.0173(16) 0.0292(17) 0.0231(16) 0.0012(13) 0.0003(13) 0.0008(13) O7 0.0161(15) 0.0286(17) 0.0192(15) 0.0031(13) 0.0014(12) 0.0016(13) O8 0.0193(16) 0.0249(16) 0.0258(17) -0.0022(13) 0.0023(13) 0.0014(13) O9 0.0161(15) 0.0208(15) 0.0250(16) 0.0007(13) 0.0018(12) 0.0019(12) O10 0.0163(16) 0.0234(16) 0.0268(17) 0.0032(13) 0.0012(12) 0.0011(12) O11 0.036(2) 0.0280(19) 0.035(2) -0.0066(15) -0.0023(16) -0.0095(16) O12 0.0234(17) 0.0309(18) 0.0188(16) -0.0053(13) 0.0008(13) -0.0023(14) O13 0.0209(17) 0.0344(19) 0.0165(16) 0.0014(13) 0.0000(12) -0.0006(14) O14 0.0276(18) 0.0263(17) 0.0252(18) 0.0077(14) 0.0008(14) -0.0071(14) O15 0.0269(18) 0.0189(16) 0.0284(18) 0.0034(13) -0.0049(14) -0.0065(13) O16 0.0329(19) 0.0185(16) 0.0234(17) -0.0040(13) 0.0009(14) -0.0024(14) O17 0.033(2) 0.0310(19) 0.0269(18) -0.0076(15) 0.0014(15) 0.0002(15) O18 0.0252(18) 0.0342(19) 0.0174(16) 0.0053(14) 0.0008(13) -0.0011(14) O19 0.0207(16) 0.0241(16) 0.0234(17) 0.0083(13) 0.0040(13) -0.0032(13) O20 0.0198(16) 0.0218(16) 0.0325(19) -0.0008(14) 0.0046(14) -0.0047(13) O1W 0.043(2) 0.045(2) 0.045(2) -0.0086(19) -0.0051(19) 0.0059(19) O2W 0.041(2) 0.062(3) 0.045(2) -0.012(2) -0.0109(19) 0.022(2) O3W 0.044(3) 0.052(3) 0.053(3) -0.001(2) -0.004(2) 0.011(2) O4W 0.042(3) 0.061(3) 0.090(4) 0.049(3) 0.023(2) 0.021(2) O5W 0.061(3) 0.060(3) 0.068(3) -0.001(3) -0.007(3) -0.002(2) O6W 0.049(3) 0.064(3) 0.071(3) 0.014(3) -0.015(2) -0.014(2) O7W 0.146(7) 0.040(3) 0.126(6) -0.010(3) -0.057(5) 0.006(4) O8W 0.085(4) 0.063(3) 0.061(3) -0.002(3) 0.019(3) 0.020(3) O9W 0.082(4) 0.088(5) 0.112(5) 0.004(4) 0.008(4) -0.001(4) O10W 0.122(5) 0.073(4) 0.123(5) 0.038(4) 0.054(4) 0.052(4) N21 0.0252(18) 0.0227(18) 0.0272(18) 0.0068(14) 0.0032(14) 0.0035(14) O23 0.054(3) 0.070(3) 0.075(4) 0.010(3) -0.006(3) 0.015(3) O22 0.095(4) 0.072(3) 0.062(3) 0.018(3) 0.001(3) 0.002(3) O21 0.076(4) 0.062(4) 0.071(4) 0.016(4) 0.021(3) -0.003(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 K1 O23 2.524(7) . ? K1 O3 2.703(4) . ? K1 O1 2.760(4) . ? K1 O4 2.766(4) . ? K1 O2 2.841(4) . ? K1 O19 2.847(3) 2_646 ? K1 O5 2.927(4) . ? K1 O2W 3.075(5) . ? K2 O10 2.684(3) . ? K2 O16 2.724(4) 2_556 ? K2 O21 2.730(9) . ? K2 O9 2.765(3) . ? K2 O8 2.766(4) . ? K2 O7 2.774(3) . ? K2 O6 2.774(4) . ? K2 O22 3.175(9) . ? K2 N21 3.392(4) . ? K2 C27 3.522(5) . ? K2 C4 3.533(5) . ? C1 O1 1.213(6) . ? C1 N3 1.378(6) . ? C1 N1 1.381(6) . ? C2 O11 1.383(6) . ? C2 N1 1.450(6) . ? C2 N2 1.451(6) . ? C2 C3 1.579(6) . ? C3 O12 1.388(5) . ? C3 N3 1.432(6) . ? C3 N4 1.458(6) . ? C4 O6 1.223(6) . ? C4 N2 1.368(6) . ? C4 N4 1.377(6) . ? C5 N3 1.450(6) . ? C5 N5 1.449(6) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 N4 1.444(6) . ? C6 N6 1.456(6) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 O13 1.392(5) . ? C7 N5 1.439(6) . ? C7 N6 1.447(6) . ? C7 C10 1.579(6) . ? C8 O2 1.217(6) . ? C8 N7 1.373(6) . ? C8 N5 1.376(6) . ? C9 O7 1.231(6) . ? C9 N6 1.366(6) . ? C9 N8 1.370(6) . ? C10 O14 1.378(6) . ? C10 N7 1.439(6) . ? C10 N8 1.461(6) . ? C11 N9 1.446(6) . ? C11 N7 1.453(6) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 N8 1.444(6) . ? C12 N10 1.457(6) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 O15 1.385(5) . ? C13 N9 1.443(6) . ? C13 N10 1.448(6) . ? C13 C16 1.579(6) . ? C14 O3 1.214(6) . ? C14 N9 1.375(6) . ? C14 N11 1.379(6) . ? C15 O8 1.220(6) . ? C15 N10 1.369(6) . ? C15 N12 1.373(6) . ? C16 O16 1.388(5) . ? C16 N11 1.440(6) . ? C16 N12 1.444(6) . ? C17 N11 1.447(6) . ? C17 N13 1.457(6) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 N12 1.451(6) . ? C18 N14 1.451(6) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 O17 1.385(6) . ? C19 N13 1.440(6) . ? C19 N14 1.447(6) . ? C19 C22 1.586(6) . ? C20 O4 1.227(6) . ? C20 N15 1.361(6) . ? C20 N13 1.365(6) . ? C21 O9 1.229(6) . ? C21 N14 1.362(6) . ? C21 N16 1.365(6) . ? C22 O18 1.384(5) . ? C22 N16 1.443(6) . ? C22 N15 1.447(6) . ? C23 N17 1.447(6) . ? C23 N15 1.458(6) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 N18 1.451(6) . ? C24 N16 1.454(6) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 O19 1.391(5) . ? C25 N18 1.443(6) . ? C25 N17 1.447(6) . ? C25 C28 1.588(6) . ? C26 O5 1.225(6) . ? C26 N19 1.364(6) . ? C26 N17 1.365(6) . ? C27 O10 1.211(6) . ? C27 N20 1.382(6) . ? C27 N18 1.379(6) . ? C28 O20 1.382(6) . ? C28 N20 1.447(6) . ? C28 N19 1.449(6) . ? C29 N19 1.453(6) . ? C29 N1 1.456(6) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 N20 1.439(6) . ? C30 N2 1.457(6) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? O11 H11 0.8400 . ? O12 H12 0.8400 . ? O13 H13 0.8400 . ? O14 H14 0.8400 . ? O15 H15 0.8400 . ? O16 K2 2.724(4) 2_546 ? O17 H17 0.8400 . ? O18 H18 0.8400 . ? O19 K1 2.847(3) 2_656 ? O20 H20 0.8400 . ? O1W H1WA 0.8500 . ? O1W H1WB 0.8500 . ? O3W H3WA 0.8500 . ? O3W H3WB 0.8499 . ? O10W H10A 0.8500 . ? O10W H10B 0.8501 . ? N21 O22 1.147(8) . ? N21 O23 1.160(7) . ? N21 O21 1.188(8) . ? 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 O23 K1 O3 74.9(2) . . ? O23 K1 O1 75.1(2) . . ? O3 K1 O1 134.51(11) . . ? O23 K1 O4 81.0(2) . . ? O3 K1 O4 75.10(11) . . ? O1 K1 O4 131.82(11) . . ? O23 K1 O2 72.1(2) . . ? O3 K1 O2 69.06(10) . . ? O1 K1 O2 69.56(10) . . ? O4 K1 O2 139.46(11) . . ? O23 K1 O19 147.8(2) . 2_646 ? O3 K1 O19 78.26(10) . 2_646 ? O1 K1 O19 137.06(10) . 2_646 ? O4 K1 O19 75.11(10) . 2_646 ? O2 K1 O19 114.14(10) . 2_646 ? O23 K1 O5 82.4(2) . . ? O3 K1 O5 137.35(11) . . ? O1 K1 O5 69.86(10) . . ? O4 K1 O5 65.90(10) . . ? O2 K1 O5 136.24(10) . . ? O19 K1 O5 106.48(10) 2_646 . ? O23 K1 O2W 127.3(2) . . ? O3 K1 O2W 157.69(11) . . ? O1 K1 O2W 62.85(11) . . ? O4 K1 O2W 103.72(12) . . ? O2 K1 O2W 116.64(12) . . ? O19 K1 O2W 79.93(11) 2_646 . ? O5 K1 O2W 54.85(11) . . ? O10 K2 O16 78.24(10) . 2_556 ? O10 K2 O21 99.42(19) . . ? O16 K2 O21 169.1(2) 2_556 . ? O10 K2 O9 70.00(10) . . ? O16 K2 O9 72.84(10) 2_556 . ? O21 K2 O9 96.32(19) . . ? O10 K2 O8 142.42(11) . . ? O16 K2 O8 101.61(10) 2_556 . ? O21 K2 O8 73.6(2) . . ? O9 K2 O8 74.10(10) . . ? O10 K2 O7 143.12(11) . . ? O16 K2 O7 122.53(10) 2_556 . ? O21 K2 O7 65.41(17) . . ? O9 K2 O7 141.51(10) . . ? O8 K2 O7 68.39(10) . . ? O10 K2 O6 71.14(10) . . ? O16 K2 O6 105.34(10) 2_556 . ? O21 K2 O6 83.7(2) . . ? O9 K2 O6 140.59(11) . . ? O8 K2 O6 141.30(11) . . ? O7 K2 O6 73.79(10) . . ? O10 K2 O22 66.30(16) . . ? O16 K2 O22 133.80(16) 2_556 . ? O21 K2 O22 38.2(2) . . ? O9 K2 O22 67.89(16) . . ? O8 K2 O22 90.30(16) . . ? O7 K2 O22 103.43(15) . . ? O6 K2 O22 90.67(17) . . ? O10 K2 N21 82.23(10) . . ? O16 K2 N21 153.43(10) 2_556 . ? O21 K2 N21 18.65(17) . . ? O9 K2 N21 83.67(9) . . ? O8 K2 N21 83.18(10) . . ? O7 K2 N21 83.68(9) . . ? O6 K2 N21 84.89(10) . . ? O22 K2 N21 19.75(14) . . ? O10 K2 C27 16.33(10) . . ? O16 K2 C27 93.85(11) 2_556 . ? O21 K2 C27 83.19(18) . . ? O9 K2 C27 69.91(10) . . ? O8 K2 C27 134.28(11) . . ? O7 K2 C27 134.75(11) . . ? O6 K2 C27 70.97(11) . . ? O22 K2 C27 50.44(16) . . ? N21 K2 C27 65.90(10) . . ? O10 K2 C4 70.15(11) . . ? O16 K2 C4 121.13(11) 2_556 . ? O21 K2 C4 67.0(2) . . ? O9 K2 C4 133.04(10) . . ? O8 K2 C4 133.33(11) . . ? O7 K2 C4 72.97(10) . . ? O6 K2 C4 17.61(10) . . ? O22 K2 C4 74.05(17) . . ? N21 K2 C4 67.28(10) . . ? C27 K2 C4 64.84(11) . . ? O1 C1 N3 126.3(4) . . ? O1 C1 N1 125.7(4) . . ? N3 C1 N1 108.0(4) . . ? O11 C2 N1 108.8(4) . . ? O11 C2 N2 113.0(4) . . ? N1 C2 N2 115.4(4) . . ? O11 C2 C3 113.6(4) . . ? N1 C2 C3 102.6(3) . . ? N2 C2 C3 103.0(3) . . ? O12 C3 N3 109.1(4) . . ? O12 C3 N4 110.4(4) . . ? N3 C3 N4 115.8(4) . . ? O12 C3 C2 115.6(4) . . ? N3 C3 C2 103.3(3) . . ? N4 C3 C2 102.7(3) . . ? O6 C4 N2 126.0(4) . . ? O6 C4 N4 125.2(4) . . ? N2 C4 N4 108.8(4) . . ? O6 C4 K2 43.3(2) . . ? N2 C4 K2 119.4(3) . . ? N4 C4 K2 111.8(3) . . ? N3 C5 N5 114.1(4) . . ? N3 C5 H5A 108.7 . . ? N5 C5 H5A 108.7 . . ? N3 C5 H5B 108.7 . . ? N5 C5 H5B 108.7 . . ? H5A C5 H5B 107.6 . . ? N4 C6 N6 113.5(4) . . ? N4 C6 H6A 108.9 . . ? N6 C6 H6A 108.9 . . ? N4 C6 H6B 108.9 . . ? N6 C6 H6B 108.9 . . ? H6A C6 H6B 107.7 . . ? O13 C7 N5 107.9(4) . . ? O13 C7 N6 111.3(4) . . ? N5 C7 N6 116.9(4) . . ? O13 C7 C10 114.5(4) . . ? N5 C7 C10 103.2(4) . . ? N6 C7 C10 103.0(3) . . ? O2 C8 N7 126.2(4) . . ? O2 C8 N5 125.8(4) . . ? N7 C8 N5 108.0(4) . . ? O7 C9 N6 125.6(4) . . ? O7 C9 N8 125.1(4) . . ? N6 C9 N8 109.3(4) . . ? O14 C10 N7 112.6(4) . . ? O14 C10 N8 107.6(4) . . ? N7 C10 N8 115.7(4) . . ? O14 C10 C7 115.1(4) . . ? N7 C10 C7 102.7(3) . . ? N8 C10 C7 103.0(3) . . ? N9 C11 N7 113.6(4) . . ? N9 C11 H11A 108.8 . . ? N7 C11 H11A 108.8 . . ? N9 C11 H11B 108.8 . . ? N7 C11 H11B 108.8 . . ? H11A C11 H11B 107.7 . . ? N8 C12 N10 114.2(4) . . ? N8 C12 H12A 108.7 . . ? N10 C12 H12A 108.7 . . ? N8 C12 H12B 108.7 . . ? N10 C12 H12B 108.7 . . ? H12A C12 H12B 107.6 . . ? O15 C13 N9 107.7(4) . . ? O15 C13 N10 112.3(4) . . ? N9 C13 N10 116.0(4) . . ? O15 C13 C16 115.2(4) . . ? N9 C13 C16 102.6(4) . . ? N10 C13 C16 102.8(3) . . ? O3 C14 N9 126.1(4) . . ? O3 C14 N11 126.3(4) . . ? N9 C14 N11 107.6(4) . . ? O8 C15 N10 126.2(4) . . ? O8 C15 N12 125.1(4) . . ? N10 C15 N12 108.7(4) . . ? O16 C16 N11 111.8(4) . . ? O16 C16 N12 109.3(4) . . ? N11 C16 N12 114.8(4) . . ? O16 C16 C13 114.4(4) . . ? N11 C16 C13 103.2(3) . . ? N12 C16 C13 103.1(3) . . ? N11 C17 N13 113.4(4) . . ? N11 C17 H17A 108.9 . . ? N13 C17 H17A 108.9 . . ? N11 C17 H17B 108.9 . . ? N13 C17 H17B 108.9 . . ? H17A C17 H17B 107.7 . . ? N12 C18 N14 113.6(4) . . ? N12 C18 H18A 108.8 . . ? N14 C18 H18A 108.8 . . ? N12 C18 H18B 108.8 . . ? N14 C18 H18B 108.8 . . ? H18A C18 H18B 107.7 . . ? O17 C19 N13 108.3(4) . . ? O17 C19 N14 111.2(4) . . ? N13 C19 N14 116.4(4) . . ? O17 C19 C22 115.6(4) . . ? N13 C19 C22 102.4(3) . . ? N14 C19 C22 102.8(3) . . ? O4 C20 N15 125.8(4) . . ? O4 C20 N13 124.8(4) . . ? N15 C20 N13 109.4(4) . . ? O9 C21 N14 125.2(4) . . ? O9 C21 N16 125.8(4) . . ? N14 C21 N16 109.0(4) . . ? O18 C22 N16 111.6(4) . . ? O18 C22 N15 108.0(4) . . ? N16 C22 N15 115.9(4) . . ? O18 C22 C19 115.4(4) . . ? N16 C22 C19 102.6(3) . . ? N15 C22 C19 103.2(3) . . ? N17 C23 N15 113.5(4) . . ? N17 C23 H23A 108.9 . . ? N15 C23 H23A 108.9 . . ? N17 C23 H23B 108.9 . . ? N15 C23 H23B 108.9 . . ? H23A C23 H23B 107.7 . . ? N18 C24 N16 114.1(4) . . ? N18 C24 H24A 108.7 . . ? N16 C24 H24A 108.7 . . ? N18 C24 H24B 108.7 . . ? N16 C24 H24B 108.7 . . ? H24A C24 H24B 107.6 . . ? O19 C25 N18 111.2(4) . . ? O19 C25 N17 109.2(4) . . ? N18 C25 N17 116.0(4) . . ? O19 C25 C28 114.9(4) . . ? N18 C25 C28 102.8(3) . . ? N17 C25 C28 102.6(3) . . ? O5 C26 N19 125.7(4) . . ? O5 C26 N17 125.4(4) . . ? N19 C26 N17 108.8(4) . . ? O10 C27 N20 125.6(4) . . ? O10 C27 N18 125.8(4) . . ? N20 C27 N18 108.6(4) . . ? O10 C27 K2 38.6(2) . . ? N20 C27 K2 116.1(3) . . ? N18 C27 K2 119.6(3) . . ? O20 C28 N20 107.4(4) . . ? O20 C28 N19 112.4(4) . . ? N20 C28 N19 115.5(4) . . ? O20 C28 C25 115.4(4) . . ? N20 C28 C25 103.4(3) . . ? N19 C28 C25 102.6(4) . . ? N19 C29 N1 113.9(4) . . ? N19 C29 H29A 108.8 . . ? N1 C29 H29A 108.8 . . ? N19 C29 H29B 108.8 . . ? N1 C29 H29B 108.8 . . ? H29A C29 H29B 107.7 . . ? N20 C30 N2 114.5(4) . . ? N20 C30 H30A 108.6 . . ? N2 C30 H30A 108.6 . . ? N20 C30 H30B 108.6 . . ? N2 C30 H30B 108.6 . . ? H30A C30 H30B 107.6 . . ? C1 N1 C2 112.2(4) . . ? C1 N1 C29 122.0(4) . . ? C2 N1 C29 122.3(4) . . ? C4 N2 C2 112.7(4) . . ? C4 N2 C30 122.5(4) . . ? C2 N2 C30 124.1(4) . . ? C1 N3 C3 113.0(4) . . ? C1 N3 C5 123.1(4) . . ? C3 N3 C5 123.8(4) . . ? C4 N4 C6 122.0(4) . . ? C4 N4 C3 112.1(4) . . ? C6 N4 C3 123.9(4) . . ? C8 N5 C7 112.7(4) . . ? C8 N5 C5 122.2(4) . . ? C7 N5 C5 124.5(4) . . ? C9 N6 C7 112.7(4) . . ? C9 N6 C6 122.8(4) . . ? C7 N6 C6 124.5(4) . . ? C8 N7 C10 113.2(4) . . ? C8 N7 C11 123.3(4) . . ? C10 N7 C11 123.5(4) . . ? C9 N8 C12 123.2(4) . . ? C9 N8 C10 111.8(4) . . ? C12 N8 C10 124.4(4) . . ? C14 N9 C13 113.1(4) . . ? C14 N9 C11 122.1(4) . . ? C13 N9 C11 123.9(4) . . ? C15 N10 C13 112.7(4) . . ? C15 N10 C12 122.8(4) . . ? C13 N10 C12 124.3(4) . . ? C14 N11 C16 112.8(4) . . ? C14 N11 C17 122.4(4) . . ? C16 N11 C17 123.7(4) . . ? C15 N12 C16 112.6(4) . . ? C15 N12 C18 122.5(4) . . ? C16 N12 C18 124.2(4) . . ? C20 N13 C19 112.9(4) . . ? C20 N13 C17 122.4(4) . . ? C19 N13 C17 124.6(4) . . ? C21 N14 C19 112.6(4) . . ? C21 N14 C18 122.2(4) . . ? C19 N14 C18 124.8(4) . . ? C20 N15 C22 112.1(4) . . ? C20 N15 C23 123.1(4) . . ? C22 N15 C23 124.5(4) . . ? C21 N16 C22 112.9(4) . . ? C21 N16 C24 122.6(4) . . ? C22 N16 C24 124.5(4) . . ? C26 N17 C25 113.0(4) . . ? C26 N17 C23 122.7(4) . . ? C25 N17 C23 124.3(4) . . ? C27 N18 C25 112.9(4) . . ? C27 N18 C24 122.3(4) . . ? C25 N18 C24 124.7(4) . . ? C26 N19 C28 112.9(4) . . ? C26 N19 C29 122.8(4) . . ? C28 N19 C29 124.0(4) . . ? C27 N20 C30 122.5(4) . . ? C27 N20 C28 112.2(4) . . ? C30 N20 C28 123.8(4) . . ? C1 O1 K1 128.7(3) . . ? C8 O2 K1 126.6(3) . . ? C14 O3 K1 126.6(3) . . ? C20 O4 K1 129.0(3) . . ? C26 O5 K1 127.8(3) . . ? C4 O6 K2 119.1(3) . . ? C9 O7 K2 120.9(3) . . ? C15 O8 K2 120.9(3) . . ? C21 O9 K2 120.5(3) . . ? C27 O10 K2 125.1(3) . . ? C2 O11 H11 109.5 . . ? C3 O12 H12 109.5 . . ? C7 O13 H13 109.5 . . ? C10 O14 H14 109.5 . . ? C13 O15 H15 109.5 . . ? C16 O16 K2 141.9(3) . 2_546 ? C19 O17 H17 109.5 . . ? C22 O18 H18 109.5 . . ? C25 O19 K1 145.6(3) . 2_656 ? C28 O20 H20 109.5 . . ? H1WA O1W H1WB 108.8 . . ? H3WA O3W H3WB 108.1 . . ? H10A O10W H10B 108.4 . . ? O22 N21 O23 123.9(7) . . ? O22 N21 O21 115.7(7) . . ? O23 N21 O21 119.5(7) . . ? O22 N21 K2 69.4(5) . . ? O23 N21 K2 166.7(5) . . ? O21 N21 K2 47.3(4) . . ? N21 O23 K1 161.2(6) . . ? N21 O22 K2 90.9(5) . . ? N21 O21 K2 114.0(5) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 2.173 _refine_diff_density_min -1.927 _refine_diff_density_rms 0.130 #===END data_complex2 _database_code_depnum_ccdc_archive 'CCDC 806942' #TrackingRef '- complex1-3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H52 Cl N20 O35 Rb3 S' _chemical_formula_weight 1576.84 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rb Rb -0.9393 2.9676 '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' _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 11.4458(6) _cell_length_b 12.4198(7) _cell_length_c 19.5596(11) _cell_angle_alpha 77.185(2) _cell_angle_beta 81.055(2) _cell_angle_gamma 77.905(2) _cell_volume 2633.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8683 _cell_measurement_theta_min 0.00 _cell_measurement_theta_max 0.00 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.988 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1592 _exptl_absorpt_coefficient_mu 2.993 _exptl_absorpt_correction_type 'multi scan' _exptl_absorpt_correction_T_min 0.4293 _exptl_absorpt_correction_T_max 0.5859 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 Smart Apex CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 29587 _diffrn_reflns_av_R_equivalents 0.0539 _diffrn_reflns_av_sigmaI/netI 0.0584 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.07 _diffrn_reflns_theta_max 26.00 _reflns_number_total 10040 _reflns_number_gt 7987 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1913P)^2^+31.0582P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10040 _refine_ls_number_parameters 820 _refine_ls_number_restraints 325 _refine_ls_R_factor_all 0.1108 _refine_ls_R_factor_gt 0.0937 _refine_ls_wR_factor_ref 0.3013 _refine_ls_wR_factor_gt 0.2821 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.065 _refine_ls_shift/su_mean 0.003 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 Rb1 Rb 0.76711(8) 0.03061(7) 0.19470(4) 0.0340(2) Uani 1 1 d . . . Rb2 Rb 0.44172(7) 0.32247(7) 0.17110(5) 0.0334(2) Uani 1 1 d . . . Rb3 Rb 0.54412(11) 0.44345(11) 0.32864(7) 0.0601(3) Uani 1 1 d . . . S1 S 0.12518(14) 0.23953(13) 0.16521(8) 0.0116(3) Uani 1 1 d . . . O1 O 0.5107(4) 0.0737(4) 0.1984(3) 0.0160(9) Uani 1 1 d U . . N1 N 0.4107(5) -0.0482(4) 0.1666(3) 0.0106(11) Uani 1 1 d . . . C1 C 0.2851(5) -0.0849(5) 0.2732(3) 0.0102(12) Uani 1 1 d . . . O2 O 0.6341(4) 0.0262(4) 0.3421(3) 0.0188(10) Uani 1 1 d U . . N2 N 0.6308(5) -0.1240(4) 0.4351(3) 0.0117(11) Uani 1 1 d . . . C2 C 0.5441(6) -0.1873(5) 0.4781(3) 0.0115(13) Uani 1 1 d . . . O3 O 0.8885(4) -0.0990(4) 0.3120(2) 0.0152(10) Uani 1 1 d U . . N3 N 0.9402(5) -0.5033(4) 0.2491(3) 0.0099(11) Uani 1 1 d . . . C3 C 0.8656(6) -0.3393(5) 0.4435(3) 0.0100(12) Uani 1 1 d . . . O4 O 0.7162(4) -0.0391(4) 0.0738(2) 0.0139(9) Uani 1 1 d U . . N4 N 0.9068(5) -0.4730(4) 0.3699(3) 0.0103(11) Uani 1 1 d . . . C4 C 0.4240(6) -0.1348(5) 0.4417(3) 0.0119(13) Uani 1 1 d . . . O5 O 0.9463(4) -0.1389(4) 0.1423(2) 0.0139(9) Uani 1 1 d U . . N5 N 0.8461(4) -0.4679(4) 0.1523(3) 0.0086(10) Uani 1 1 d . . . C5 C 0.8726(5) -0.2405(5) 0.0415(3) 0.0093(12) Uani 1 1 d . . . H5A H 0.8987 -0.2860 0.0044 0.011 Uiso 1 1 calc R . . H5B H 0.8998 -0.1677 0.0236 0.011 Uiso 1 1 calc R . . O6 O 0.7352(4) -0.5503(4) 0.4085(3) 0.0159(9) Uani 1 1 d U . . C6 C 0.3833(6) 0.0258(5) 0.3372(4) 0.0134(13) Uani 1 1 d . . . H6A H 0.3041 0.0416 0.3652 0.016 Uiso 1 1 calc R . . H6B H 0.4146 0.0969 0.3222 0.016 Uiso 1 1 calc R . . O7 O 0.4751(4) -0.4171(4) 0.4255(2) 0.0138(9) Uani 1 1 d U . . N7 N 0.9306(5) -0.2976(4) 0.1034(3) 0.0086(10) Uani 1 1 d . . . C7 C 0.6659(5) -0.2931(5) 0.0437(3) 0.0084(12) Uani 1 1 d . . . O8 O 0.7781(4) -0.5883(4) 0.2511(2) 0.0153(9) Uani 1 1 d U . . N8 N 0.5554(5) -0.1275(4) 0.0799(3) 0.0098(11) Uani 1 1 d . . . C8 C 0.7686(5) -0.4854(5) 0.1054(3) 0.0089(12) Uani 1 1 d . . . H8A H 0.8159 -0.4916 0.0590 0.011 Uiso 1 1 calc R . . H8B H 0.7404 -0.5573 0.1250 0.011 Uiso 1 1 calc R . . O9 O 0.3418(4) -0.3782(4) 0.2912(2) 0.0135(9) Uani 1 1 d U . . N9 N 0.3137(5) -0.1988(4) 0.3126(3) 0.0102(11) Uani 1 1 d . . . C9 C 0.5818(6) -0.0445(5) 0.3822(3) 0.0116(13) Uani 1 1 d . . . O10 O 0.5306(4) -0.4824(4) 0.1785(2) 0.0121(9) Uani 1 1 d U . . N10 N 0.3668(5) -0.0120(4) 0.2749(3) 0.0113(11) Uani 1 1 d . . . C10 C 0.7539(6) -0.1377(5) 0.4497(3) 0.0114(13) Uani 1 1 d . . . H10A H 0.7565 -0.1603 0.5013 0.014 Uiso 1 1 calc R . . H10B H 0.7805 -0.0643 0.4341 0.014 Uiso 1 1 calc R . . N11 N 0.3932(5) -0.2313(4) 0.4248(3) 0.0110(11) Uani 1 1 d . . . O11 O 0.5358(5) -0.1750(5) 0.5476(3) 0.0242(12) Uani 1 1 d U . . C11 C 0.2911(5) -0.2288(5) 0.3893(3) 0.0121(13) Uani 1 1 d . . . H11A H 0.2226 -0.1740 0.4061 0.015 Uiso 1 1 calc R . . H11B H 0.2677 -0.3037 0.4024 0.015 Uiso 1 1 calc R . . O12 O 1.0765(4) -0.4260(4) 0.4019(3) 0.0168(10) Uani 1 1 d U . . H12A H 1.0795 -0.4894 0.4286 0.025 Uiso 1 1 calc R . . N12 N 0.4649(5) -0.0544(4) 0.3818(3) 0.0112(11) Uani 1 1 d . . . C12 C 1.0100(5) -0.4307(5) 0.1982(3) 0.0082(12) Uani 1 1 d . . . O13 O 0.4697(4) -0.1876(4) 0.0013(2) 0.0153(10) Uani 1 1 d U . . H13A H 0.4464 -0.2415 -0.0088 0.023 Uiso 1 1 calc R . . N13 N 0.4781(5) -0.3029(4) 0.1135(3) 0.0085(10) Uani 1 1 d . . . C13 C 0.9602(5) -0.3858(5) 0.3840(3) 0.0088(12) Uani 1 1 d . . . O14 O 0.3317(5) -0.0784(4) 0.4818(3) 0.0206(11) Uani 1 1 d U . . H14A H 0.3115 -0.1226 0.5188 0.031 Uiso 1 1 calc R . . N14 N 0.9624(5) -0.2889(4) 0.3285(3) 0.0095(11) Uani 1 1 d . . . C14 C 0.9559(5) -0.2412(5) 0.1507(3) 0.0084(12) Uani 1 1 d . . . O15 O 0.1668(4) -0.0422(4) 0.2955(3) 0.0185(11) Uani 1 1 d U . . H15A H 0.1468 0.0228 0.2720 0.028 Uiso 1 1 calc R . . N15 N 0.7697(5) -0.3998(4) 0.4483(3) 0.0117(11) Uani 1 1 d . . . C15 C 0.9529(5) -0.4173(5) 0.1280(3) 0.0086(12) Uani 1 1 d . . . O16 O 1.0269(4) -0.4670(4) 0.0761(2) 0.0127(9) Uani 1 1 d U . . H16A H 1.0319 -0.5370 0.0872 0.019 Uiso 1 1 calc R . . N16 N 0.3322(5) -0.2220(4) 0.2015(3) 0.0093(11) Uani 1 1 d . . . C16 C 0.3090(5) -0.1025(5) 0.1943(3) 0.0090(12) Uani 1 1 d U . . N17 N 0.9940(5) -0.3176(4) 0.2083(3) 0.0092(10) Uani 1 1 d . . . C17 C 0.4617(6) -0.0349(5) 0.0935(3) 0.0103(12) Uani 1 1 d . . . H17A H 0.3971 -0.0277 0.0636 0.012 Uiso 1 1 calc R . . H17B H 0.4948 0.0353 0.0801 0.012 Uiso 1 1 calc R . . O18 O 0.9068(4) -0.3641(4) 0.5094(2) 0.0169(10) Uani 1 1 d U . . H18A H 0.9329 -0.3089 0.5156 0.025 Uiso 1 1 calc R . . N18 N 0.7411(4) -0.2199(4) 0.0539(3) 0.0074(10) Uani 1 1 d . . . C18 C 0.5340(5) -0.2262(5) 0.0583(3) 0.0082(12) Uani 1 1 d U . . O19 O 0.6921(4) -0.3194(4) -0.0230(2) 0.0156(10) Uani 1 1 d U . . N19 N 0.6658(5) -0.3966(4) 0.0950(3) 0.0095(11) Uani 1 1 d . . . C19 C 0.9625(6) -0.5476(5) 0.3213(3) 0.0103(12) Uani 1 1 d U . . H19A H 1.0505 -0.5643 0.3235 0.012 Uiso 1 1 calc R . . H19B H 0.9325 -0.6193 0.3373 0.012 Uiso 1 1 calc R . . O20 O 1.1324(4) -0.4750(4) 0.1952(2) 0.0130(9) Uani 1 1 d U . . H20C H 1.1436 -0.5430 0.1923 0.019 Uiso 1 1 calc R . . N20 N 0.8386(5) -0.2207(4) 0.4153(3) 0.0106(11) Uani 1 1 d . . . C20 C 0.3529(5) -0.2817(5) 0.1442(3) 0.0101(12) Uani 1 1 d . . . H20A H 0.3032 -0.2379 0.1067 0.012 Uiso 1 1 calc R . . H20B H 0.3255 -0.3545 0.1615 0.012 Uiso 1 1 calc R . . O17 O 0.2127(4) -0.0581(4) 0.1549(3) 0.0161(10) Uani 1 1 d U . . H17C H 0.2076 0.0118 0.1428 0.024 Uiso 1 1 calc R . . N6 N 0.5632(5) -0.3032(4) 0.4721(3) 0.0124(11) Uani 1 1 d . . . C21 C 0.7970(6) -0.4809(5) 0.4082(3) 0.0105(12) Uani 1 1 d . . . C22 C 0.4780(6) -0.3266(5) 0.4388(3) 0.0098(12) Uani 1 1 d U . . C23 C 0.8952(5) -0.1929(5) 0.3487(3) 0.0091(12) Uani 1 1 d . . . C24 C 0.5551(5) -0.4019(5) 0.1342(3) 0.0087(12) Uani 1 1 d . . . C25 C 0.4370(5) 0.0099(5) 0.2122(3) 0.0105(12) Uani 1 1 d . . . C26 C 0.3307(5) -0.2771(5) 0.2714(3) 0.0098(12) Uani 1 1 d U . . C27 C 0.6615(6) -0.3900(5) 0.4984(3) 0.0125(13) Uani 1 1 d . . . H27A H 0.6339 -0.4631 0.5111 0.015 Uiso 1 1 calc R . . H27B H 0.6818 -0.3737 0.5420 0.015 Uiso 1 1 calc R . . C28 C 1.0429(5) -0.2857(5) 0.2640(3) 0.0097(12) Uani 1 1 d . . . H28A H 1.1197 -0.3372 0.2737 0.012 Uiso 1 1 calc R . . H28B H 1.0604 -0.2088 0.2473 0.012 Uiso 1 1 calc R . . C29 C 0.8471(5) -0.5263(5) 0.2208(3) 0.0092(12) Uani 1 1 d U . . C30 C 0.6746(5) -0.1205(5) 0.0695(3) 0.0077(12) Uani 1 1 d . . . O21 O 0.0779(5) 0.1676(5) 0.2287(3) 0.0290(13) Uani 1 1 d U . . O22 O 0.0271(4) 0.3098(4) 0.1256(3) 0.0182(10) Uani 1 1 d U . . O23 O 0.2077(4) 0.1685(4) 0.1197(3) 0.0181(10) Uani 1 1 d U . . O24 O 0.1941(5) 0.3132(4) 0.1858(3) 0.0261(11) Uani 1 1 d U . . Cl1 Cl 0.9597(4) 0.2074(3) 0.47007(18) 0.0715(9) Uani 1 1 d D . . O11W O 0.9900(15) 0.0189(8) 0.5802(6) 0.145(6) Uani 1 1 d D . . H11D H 0.9811 0.0742 0.5458 0.174 Uiso 1 1 d R . . H11C H 1.0034 -0.0414 0.5643 0.174 Uiso 1 1 d R . . O10W O 0.6199(5) 0.3301(5) 0.0476(3) 0.0266(12) Uani 1 1 d U . . H10C H 0.6910 0.3106 0.0591 0.032 Uiso 1 1 d R . . H10D H 0.6123 0.3952 0.0215 0.032 Uiso 1 1 d R . . O9W O 0.3111(5) 0.5149(5) 0.0662(3) 0.0277(12) Uani 1 1 d U . . O8W O 0.8589(5) 0.1332(5) 0.3037(3) 0.0317(13) Uani 1 1 d U . . O7W O 0.1700(5) 0.2293(5) 0.3499(3) 0.0308(12) Uani 1 1 d U . . H7WA H 0.1142 0.2242 0.3840 0.037 Uiso 1 1 d R . . H7WB H 0.1473 0.2125 0.3149 0.037 Uiso 1 1 d R . . O6W O 0.6261(5) 0.2468(5) 0.2542(3) 0.0314(12) Uani 1 1 d U . . O5W O 0.8407(5) 0.2190(6) 0.0917(4) 0.0386(15) Uani 1 1 d U . . H5WA H 0.8685 0.1987 0.0527 0.046 Uiso 1 1 d R . . H5WB H 0.8954 0.2421 0.1062 0.046 Uiso 1 1 d R . . O4W O 0.3272(6) 0.3830(5) 0.3123(4) 0.0400(14) Uani 1 1 d U . . O3W O 0.7123(9) 0.2339(6) 0.4053(4) 0.061(2) Uani 1 1 d U . . O2W O 0.8718(7) 0.1069(7) -0.0155(4) 0.0549(18) Uani 1 1 d U . . H2WA H 0.8369 0.0510 0.0007 0.066 Uiso 1 1 d R . . H2WB H 0.9194 0.0948 -0.0521 0.066 Uiso 1 1 d R . . O1W O 0.6597(10) -0.2486(13) 0.2581(6) 0.088(4) Uani 0.80 1 d PU . . O1W' O 0.605(2) -0.382(2) 0.2806(14) 0.022(2) Uani 0.20 1 d PU . . 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 Rb1 0.0305(4) 0.0397(5) 0.0295(4) -0.0099(3) -0.0071(3) 0.0048(3) Rb2 0.0299(4) 0.0286(4) 0.0412(5) -0.0019(3) -0.0076(3) -0.0066(3) Rb3 0.0467(6) 0.0771(8) 0.0604(7) -0.0309(6) -0.0086(5) 0.0005(5) S1 0.0098(7) 0.0096(7) 0.0118(7) -0.0003(6) 0.0006(6) 0.0027(6) O1 0.013(2) 0.014(2) 0.022(2) -0.0028(17) -0.0016(18) -0.0053(17) N1 0.009(2) 0.008(2) 0.013(3) 0.002(2) -0.003(2) -0.0029(19) C1 0.007(3) 0.008(3) 0.014(3) 0.000(2) -0.001(2) 0.001(2) O2 0.017(2) 0.014(2) 0.023(2) 0.0036(18) -0.0015(18) -0.0052(17) N2 0.011(3) 0.009(2) 0.014(3) 0.002(2) -0.002(2) -0.004(2) C2 0.013(3) 0.013(3) 0.010(3) -0.003(2) 0.002(2) -0.007(2) O3 0.019(2) 0.008(2) 0.017(2) 0.0010(17) -0.0008(18) -0.0022(17) N3 0.010(2) 0.007(2) 0.012(3) 0.0007(19) -0.002(2) -0.0038(19) C3 0.014(3) 0.008(3) 0.008(3) 0.000(2) -0.006(2) -0.001(2) O4 0.013(2) 0.012(2) 0.018(2) -0.0027(17) -0.0017(17) -0.0052(16) N4 0.013(3) 0.006(2) 0.011(3) 0.001(2) -0.002(2) -0.002(2) C4 0.014(3) 0.008(3) 0.013(3) -0.005(2) 0.003(2) -0.001(2) O5 0.018(2) 0.007(2) 0.017(2) -0.0013(17) -0.0040(18) -0.0023(16) N5 0.004(2) 0.012(2) 0.010(2) 0.001(2) -0.0013(19) -0.0036(19) C5 0.009(3) 0.012(3) 0.006(3) -0.001(2) 0.000(2) -0.001(2) O6 0.015(2) 0.012(2) 0.023(2) -0.0074(17) -0.0003(18) -0.0056(17) C6 0.010(3) 0.008(3) 0.020(3) -0.005(2) 0.000(2) 0.003(2) O7 0.016(2) 0.0096(19) 0.017(2) -0.0038(17) 0.0005(17) -0.0045(16) N7 0.008(2) 0.004(2) 0.012(3) 0.0036(19) -0.002(2) -0.0005(18) C7 0.007(3) 0.008(3) 0.010(3) 0.001(2) 0.000(2) -0.004(2) O8 0.015(2) 0.014(2) 0.017(2) 0.0032(17) -0.0005(17) -0.0088(17) N8 0.009(2) 0.005(2) 0.017(3) -0.005(2) -0.002(2) -0.0014(19) C8 0.006(3) 0.006(3) 0.014(3) -0.002(2) -0.002(2) 0.001(2) O9 0.014(2) 0.0072(19) 0.018(2) 0.0015(16) -0.0025(17) -0.0018(16) N9 0.009(2) 0.004(2) 0.015(3) 0.002(2) -0.002(2) -0.0007(19) C9 0.016(3) 0.008(3) 0.011(3) -0.003(2) 0.000(2) -0.004(2) O10 0.012(2) 0.0085(19) 0.014(2) 0.0043(16) -0.0017(16) -0.0047(16) N10 0.009(2) 0.010(2) 0.015(3) -0.004(2) 0.001(2) -0.004(2) C10 0.012(3) 0.009(3) 0.016(3) -0.006(2) -0.001(2) -0.004(2) N11 0.011(3) 0.005(2) 0.017(3) -0.002(2) -0.001(2) -0.0024(19) O11 0.030(3) 0.034(3) 0.011(2) -0.007(2) 0.000(2) -0.010(2) C11 0.005(3) 0.016(3) 0.013(3) -0.001(2) 0.003(2) -0.002(2) O12 0.011(2) 0.016(2) 0.022(2) 0.0061(19) -0.0120(19) -0.0002(18) N12 0.011(3) 0.007(2) 0.012(3) 0.004(2) 0.000(2) -0.001(2) C12 0.004(3) 0.008(3) 0.010(3) 0.001(2) -0.001(2) 0.002(2) O13 0.019(2) 0.014(2) 0.014(2) 0.0045(18) -0.0110(18) -0.0053(18) N13 0.008(2) 0.005(2) 0.010(2) 0.0041(19) -0.0025(19) -0.0016(19) C13 0.005(3) 0.010(3) 0.012(3) 0.000(2) -0.005(2) 0.000(2) O14 0.022(3) 0.016(2) 0.019(2) -0.0053(19) 0.011(2) -0.002(2) N14 0.012(2) 0.005(2) 0.009(2) 0.0038(19) -0.002(2) -0.0007(19) C14 0.004(3) 0.011(3) 0.009(3) 0.000(2) 0.001(2) -0.003(2) O15 0.008(2) 0.015(2) 0.026(3) 0.0024(19) 0.0010(19) 0.0035(17) N15 0.013(3) 0.010(2) 0.014(3) -0.003(2) 0.000(2) -0.006(2) C15 0.005(3) 0.007(3) 0.012(3) -0.002(2) 0.000(2) 0.001(2) O16 0.012(2) 0.008(2) 0.015(2) -0.0036(17) 0.0062(17) 0.0001(17) N16 0.009(2) 0.003(2) 0.014(3) 0.0024(19) -0.003(2) 0.0022(18) C16 0.005(2) 0.006(2) 0.014(3) 0.002(2) -0.002(2) 0.0006(19) N17 0.008(2) 0.008(2) 0.010(2) 0.0015(19) -0.0025(19) -0.0007(19) C17 0.009(3) 0.005(3) 0.013(3) 0.004(2) 0.000(2) 0.001(2) O18 0.022(2) 0.016(2) 0.013(2) 0.0023(18) -0.0086(19) -0.0056(19) N18 0.005(2) 0.008(2) 0.010(2) -0.0020(19) -0.0002(19) -0.0029(18) C18 0.010(2) 0.005(2) 0.010(2) 0.002(2) -0.003(2) -0.005(2) O19 0.022(2) 0.015(2) 0.011(2) -0.0057(18) 0.0006(18) -0.0051(18) N19 0.007(2) 0.006(2) 0.012(3) 0.003(2) -0.001(2) -0.0002(19) C19 0.011(3) 0.005(2) 0.012(3) 0.003(2) -0.004(2) 0.002(2) O20 0.0049(18) 0.0100(19) 0.022(2) -0.0021(16) -0.0005(16) 0.0021(15) N20 0.013(3) 0.007(2) 0.010(3) -0.001(2) -0.002(2) 0.000(2) C20 0.004(3) 0.013(3) 0.014(3) -0.003(2) -0.001(2) -0.003(2) O17 0.012(2) 0.013(2) 0.024(2) -0.0016(18) -0.0111(18) 0.0010(17) N6 0.014(3) 0.006(2) 0.017(3) -0.001(2) -0.002(2) -0.003(2) C21 0.012(3) 0.007(3) 0.010(3) 0.003(2) -0.005(2) 0.000(2) C22 0.010(2) 0.011(2) 0.006(2) 0.001(2) 0.005(2) -0.003(2) C23 0.009(3) 0.007(3) 0.011(3) 0.002(2) -0.006(2) -0.002(2) C24 0.007(3) 0.007(3) 0.012(3) -0.003(2) -0.002(2) -0.001(2) C25 0.006(3) 0.006(3) 0.017(3) 0.001(2) -0.003(2) 0.001(2) C26 0.003(2) 0.012(3) 0.014(3) 0.000(2) -0.002(2) -0.0021(19) C27 0.012(3) 0.012(3) 0.010(3) 0.004(2) -0.004(2) 0.001(2) C28 0.006(3) 0.009(3) 0.015(3) -0.001(2) -0.002(2) -0.004(2) C29 0.006(2) 0.008(2) 0.012(3) -0.002(2) -0.003(2) 0.004(2) C30 0.008(3) 0.006(3) 0.009(3) 0.000(2) -0.001(2) -0.004(2) O21 0.025(3) 0.021(3) 0.025(3) 0.011(2) 0.008(2) 0.007(2) O22 0.013(2) 0.012(2) 0.027(3) 0.0011(19) -0.0112(19) 0.0057(18) O23 0.019(2) 0.013(2) 0.016(2) -0.0030(18) 0.0040(19) 0.0065(18) O24 0.023(2) 0.019(2) 0.040(3) -0.012(2) -0.014(2) 0.0023(19) Cl1 0.085(2) 0.071(2) 0.0627(19) -0.0182(16) -0.0124(17) -0.0148(17) O11W 0.132(13) 0.128(12) 0.184(16) -0.059(12) -0.008(12) -0.016(10) O10W 0.028(3) 0.025(3) 0.030(3) -0.003(2) -0.009(2) -0.010(2) O9W 0.031(3) 0.026(3) 0.028(3) -0.007(2) 0.001(2) -0.009(2) O8W 0.029(3) 0.023(3) 0.041(3) -0.007(2) 0.005(2) -0.006(2) O7W 0.028(3) 0.030(3) 0.032(3) -0.009(2) -0.008(2) 0.006(2) O6W 0.030(3) 0.021(2) 0.043(3) 0.000(2) -0.014(2) -0.001(2) O5W 0.027(3) 0.052(4) 0.044(3) -0.019(3) -0.004(3) -0.013(3) O4W 0.034(3) 0.034(3) 0.053(3) -0.008(3) -0.011(3) -0.003(2) O3W 0.116(6) 0.029(3) 0.033(3) -0.009(3) 0.021(4) -0.026(4) O2W 0.065(4) 0.067(4) 0.045(4) -0.021(3) 0.017(3) -0.046(3) O1W 0.054(6) 0.134(10) 0.067(7) -0.037(7) -0.017(5) 0.031(7) O1W' 0.021(3) 0.022(3) 0.023(3) -0.004(3) -0.002(3) -0.002(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 Rb1 O5 2.860(5) . ? Rb1 O1 2.864(5) . ? Rb1 O3 2.864(5) . ? Rb1 O4 2.869(5) . ? Rb1 O5W 2.907(7) . ? Rb1 O2 3.039(5) . ? Rb1 O8W 3.121(6) . ? Rb1 O6W 3.187(6) . ? Rb1 Rb2 4.6215(12) . ? Rb1 H5WA 3.2957 . ? Rb1 H5WB 3.2958 . ? Rb2 O6W 2.745(6) . ? Rb2 O24 2.828(5) . ? Rb2 O10 2.858(4) 1_565 ? Rb2 O10W 2.907(6) . ? Rb2 O1 2.972(5) . ? Rb2 O4W 3.049(7) . ? Rb2 O9W 3.072(6) . ? Rb2 O19 3.492(5) 2_655 ? Rb2 S1 3.9934(18) . ? Rb2 Rb3 4.1282(15) . ? Rb3 O1W' 2.36(3) 1_565 ? Rb3 O7 2.762(5) 1_565 ? Rb3 O4W 2.822(7) . ? Rb3 O8 2.861(5) 1_565 ? Rb3 O10 2.895(5) 1_565 ? Rb3 O6 2.902(5) 1_565 ? Rb3 O9 2.909(5) 1_565 ? Rb3 O6W 3.026(6) . ? Rb3 O3W 3.129(9) . ? S1 O21 1.460(5) . ? S1 O22 1.477(5) . ? S1 O24 1.478(5) . ? S1 O23 1.483(5) . ? O1 C25 1.235(8) . ? N1 C25 1.366(9) . ? N1 C16 1.439(8) . ? N1 C17 1.445(8) . ? C1 O15 1.387(7) . ? C1 N10 1.440(8) . ? C1 N9 1.450(8) . ? C1 C16 1.579(9) . ? O2 C9 1.230(8) . ? N2 C9 1.362(8) . ? N2 C2 1.443(8) . ? N2 C10 1.449(8) . ? C2 O11 1.387(8) . ? C2 N6 1.438(8) . ? C2 C4 1.595(9) . ? O3 C23 1.221(8) . ? N3 C29 1.380(8) . ? N3 C19 1.440(8) . ? N3 C12 1.448(8) . ? C3 O18 1.389(8) . ? C3 N15 1.437(8) . ? C3 N20 1.439(8) . ? C3 C13 1.583(8) . ? O4 C30 1.228(8) . ? N4 C21 1.369(8) . ? N4 C13 1.444(8) . ? N4 C19 1.457(8) . ? C4 O14 1.377(8) . ? C4 N11 1.436(8) . ? C4 N12 1.447(8) . ? O5 C14 1.228(8) . ? N5 C29 1.375(8) . ? N5 C8 1.449(8) . ? N5 C15 1.458(8) . ? C5 N7 1.441(8) . ? C5 N18 1.464(8) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? O6 C21 1.223(8) . ? O6 Rb3 2.902(5) 1_545 ? C6 N10 1.450(9) . ? C6 N12 1.450(8) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? O7 C22 1.216(8) . ? O7 Rb3 2.762(5) 1_545 ? N7 C14 1.374(8) . ? N7 C15 1.438(8) . ? C7 O19 1.387(8) . ? C7 N18 1.439(8) . ? C7 N19 1.444(8) . ? C7 C18 1.580(8) . ? O8 C29 1.215(8) . ? O8 Rb3 2.861(5) 1_545 ? N8 C30 1.365(8) . ? N8 C17 1.441(8) . ? N8 C18 1.459(7) . ? C8 N19 1.440(8) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? O9 C26 1.214(8) . ? O9 Rb3 2.909(5) 1_545 ? N9 C26 1.362(8) . ? N9 C11 1.460(8) . ? C9 N12 1.370(9) . ? O10 C24 1.218(8) . ? O10 Rb2 2.858(4) 1_545 ? O10 Rb3 2.895(5) 1_545 ? N10 C25 1.364(8) . ? C10 N20 1.462(8) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? N11 C22 1.370(8) . ? N11 C11 1.440(9) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? O12 C13 1.391(7) . ? O12 H12A 0.8400 . ? C12 O20 1.390(7) . ? C12 N17 1.432(8) . ? C12 C15 1.573(9) . ? O13 C18 1.373(8) . ? O13 H13A 0.8400 . ? N13 C24 1.374(8) . ? N13 C18 1.438(8) . ? N13 C20 1.459(8) . ? C13 N14 1.432(8) . ? O14 H14A 0.8400 . ? N14 C23 1.379(8) . ? N14 C28 1.441(8) . ? C14 N17 1.365(8) . ? O15 H15A 0.8400 . ? N15 C21 1.366(8) . ? N15 C27 1.457(8) . ? C15 O16 1.386(7) . ? O16 H16A 0.8400 . ? N16 C26 1.387(8) . ? N16 C16 1.431(8) . ? N16 C20 1.440(8) . ? C16 O17 1.391(8) . ? N17 C28 1.459(8) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? O18 H18A 0.8400 . ? N18 C30 1.377(8) . ? O19 Rb2 3.492(5) 2_655 ? N19 C24 1.382(8) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? O20 H20C 0.8400 . ? N20 C23 1.367(8) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? O17 H17C 0.8400 . ? N6 C22 1.364(9) . ? N6 C27 1.456(8) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? O11W H11D 0.8499 . ? O11W H11C 0.8499 . ? O10W H10C 0.8500 . ? O10W H10D 0.8500 . ? O7W H7WA 0.8500 . ? O7W H7WB 0.8500 . ? O5W H5WA 0.8500 . ? O5W H5WB 0.8499 . ? O2W H2WA 0.8500 . ? O2W H2WB 0.8500 . ? O1W O1W' 1.83(3) . ? O1W' Rb3 2.36(3) 1_545 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Rb1 O1 130.87(14) . . ? O5 Rb1 O3 73.07(13) . . ? O1 Rb1 O3 122.55(14) . . ? O5 Rb1 O4 64.17(13) . . ? O1 Rb1 O4 73.58(13) . . ? O3 Rb1 O4 129.38(13) . . ? O5 Rb1 O5W 95.97(16) . . ? O1 Rb1 O5W 103.79(16) . . ? O3 Rb1 O5W 127.31(16) . . ? O4 Rb1 O5W 84.21(16) . . ? O5 Rb1 O2 129.14(13) . . ? O1 Rb1 O2 66.15(14) . . ? O3 Rb1 O2 61.83(13) . . ? O4 Rb1 O2 131.96(13) . . ? O5W Rb1 O2 129.34(16) . . ? O5 Rb1 O8W 112.41(14) . . ? O1 Rb1 O8W 113.77(15) . . ? O3 Rb1 O8W 55.67(14) . . ? O4 Rb1 O8W 168.17(14) . . ? O5W Rb1 O8W 84.96(17) . . ? O2 Rb1 O8W 59.46(14) . . ? O5 Rb1 O6W 165.24(15) . . ? O1 Rb1 O6W 63.60(14) . . ? O3 Rb1 O6W 102.30(14) . . ? O4 Rb1 O6W 125.54(14) . . ? O5W Rb1 O6W 75.47(17) . . ? O2 Rb1 O6W 55.17(14) . . ? O8W Rb1 O6W 55.58(15) . . ? O5 Rb1 Rb2 152.79(10) . . ? O1 Rb1 Rb2 38.46(9) . . ? O3 Rb1 Rb2 133.89(10) . . ? O4 Rb1 Rb2 90.19(9) . . ? O5W Rb1 Rb2 71.18(13) . . ? O2 Rb1 Rb2 74.34(9) . . ? O8W Rb1 Rb2 90.80(11) . . ? O6W Rb1 Rb2 35.50(11) . . ? O5 Rb1 H5WA 84.1 . . ? O1 Rb1 H5WA 106.4 . . ? O3 Rb1 H5WA 129.8 . . ? O4 Rb1 H5WA 72.3 . . ? O5W Rb1 H5WA 14.0 . . ? O2 Rb1 H5WA 143.2 . . ? O8W Rb1 H5WA 96.4 . . ? O6W Rb1 H5WA 88.7 . . ? Rb2 Rb1 H5WA 79.2 . . ? O5 Rb1 H5WB 95.1 . . ? O1 Rb1 H5WB 114.0 . . ? O3 Rb1 H5WB 113.6 . . ? O4 Rb1 H5WB 96.4 . . ? O5W Rb1 H5WB 14.0 . . ? O2 Rb1 H5WB 123.0 . . ? O8W Rb1 H5WB 72.3 . . ? O6W Rb1 H5WB 73.6 . . ? Rb2 Rb1 H5WB 78.1 . . ? H5WA Rb1 H5WB 24.2 . . ? O6W Rb2 O24 136.42(18) . . ? O6W Rb2 O10 74.28(15) . 1_565 ? O24 Rb2 O10 123.44(14) . 1_565 ? O6W Rb2 O10W 88.63(17) . . ? O24 Rb2 O10W 130.76(16) . . ? O10 Rb2 O10W 80.43(14) 1_565 . ? O6W Rb2 O1 67.95(15) . . ? O24 Rb2 O1 92.20(14) . . ? O10 Rb2 O1 140.76(13) 1_565 . ? O10W Rb2 O1 88.27(14) . . ? O6W Rb2 O4W 77.05(18) . . ? O24 Rb2 O4W 71.68(17) . . ? O10 Rb2 O4W 74.71(15) 1_565 . ? O10W Rb2 O4W 153.85(16) . . ? O1 Rb2 O4W 105.90(16) . . ? O6W Rb2 O9W 147.92(16) . . ? O24 Rb2 O9W 69.57(16) . . ? O10 Rb2 O9W 74.54(14) 1_565 . ? O10W Rb2 O9W 78.95(15) . . ? O1 Rb2 O9W 139.90(14) . . ? O4W Rb2 O9W 101.73(16) . . ? O6W Rb2 O19 150.80(15) . 2_655 ? O24 Rb2 O19 60.56(14) . 2_655 ? O10 Rb2 O19 119.46(12) 1_565 2_655 ? O10W Rb2 O19 70.20(14) . 2_655 ? O1 Rb2 O19 90.85(12) . 2_655 ? O4W Rb2 O19 129.88(15) . 2_655 ? O9W Rb2 O19 49.05(13) . 2_655 ? O6W Rb2 S1 136.18(13) . . ? O24 Rb2 S1 15.56(11) . . ? O10 Rb2 S1 137.81(9) 1_565 . ? O10W Rb2 S1 120.24(11) . . ? O1 Rb2 S1 79.91(9) . . ? O4W Rb2 S1 84.41(13) . . ? O9W Rb2 S1 74.44(11) . . ? O19 Rb2 S1 51.89(8) 2_655 . ? O6W Rb2 Rb3 47.13(13) . . ? O24 Rb2 Rb3 114.38(12) . . ? O10 Rb2 Rb3 44.50(9) 1_565 . ? O10W Rb2 Rb3 111.76(11) . . ? O1 Rb2 Rb3 109.23(10) . . ? O4W Rb2 Rb3 43.13(13) . . ? O9W Rb2 Rb3 110.82(11) . . ? O19 Rb2 Rb3 159.75(8) 2_655 . ? S1 Rb2 Rb3 127.53(4) . . ? O6W Rb2 Rb1 42.39(13) . . ? O24 Rb2 Rb1 128.99(11) . . ? O10 Rb2 Rb1 105.47(9) 1_565 . ? O10W Rb2 Rb1 66.48(11) . . ? O1 Rb2 Rb1 36.82(9) . . ? O4W Rb2 Rb1 112.48(12) . . ? O9W Rb2 Rb1 144.65(11) . . ? O19 Rb2 Rb1 108.92(8) 2_655 . ? S1 Rb2 Rb1 116.39(3) . . ? Rb3 Rb2 Rb1 89.50(3) . . ? O1W' Rb3 O7 70.4(6) 1_565 1_565 ? O1W' Rb3 O4W 126.5(6) 1_565 . ? O7 Rb3 O4W 103.72(17) 1_565 . ? O1W' Rb3 O8 69.3(6) 1_565 1_565 ? O7 Rb3 O8 123.92(14) 1_565 1_565 ? O4W Rb3 O8 131.50(18) . 1_565 ? O1W' Rb3 O10 65.7(6) 1_565 1_565 ? O7 Rb3 O10 124.06(14) 1_565 1_565 ? O4W Rb3 O10 77.72(17) . 1_565 ? O8 Rb3 O10 69.00(13) 1_565 1_565 ? O1W' Rb3 O6 74.7(6) 1_565 1_565 ? O7 Rb3 O6 66.22(14) 1_565 1_565 ? O4W Rb3 O6 153.83(18) . 1_565 ? O8 Rb3 O6 66.65(14) 1_565 1_565 ? O10 Rb3 O6 128.27(14) 1_565 1_565 ? O1W' Rb3 O9 67.9(6) 1_565 1_565 ? O7 Rb3 O9 67.06(14) 1_565 1_565 ? O4W Rb3 O9 61.69(16) . 1_565 ? O8 Rb3 O9 126.67(14) 1_565 1_565 ? O10 Rb3 O9 65.36(13) 1_565 1_565 ? O6 Rb3 O9 127.29(13) 1_565 1_565 ? O1W' Rb3 O6W 121.0(6) 1_565 . ? O7 Rb3 O6W 166.17(16) 1_565 . ? O4W Rb3 O6W 76.30(18) . . ? O8 Rb3 O6W 59.76(15) 1_565 . ? O10 Rb3 O6W 69.67(14) 1_565 . ? O6 Rb3 O6W 107.61(15) 1_565 . ? O9 Rb3 O6W 123.02(15) 1_565 . ? O1W' Rb3 O3W 123.3(7) 1_565 . ? O7 Rb3 O3W 104.71(17) 1_565 . ? O4W Rb3 O3W 109.8(2) . . ? O8 Rb3 O3W 69.04(17) 1_565 . ? O10 Rb3 O3W 127.83(16) 1_565 . ? O6 Rb3 O3W 54.35(18) 1_565 . ? O9 Rb3 O3W 164.28(18) 1_565 . ? O6W Rb3 O3W 63.06(18) . . ? O1W' Rb3 Rb2 109.5(6) 1_565 . ? O7 Rb3 Rb2 146.16(11) 1_565 . ? O4W Rb3 Rb2 47.61(15) . . ? O8 Rb3 Rb2 84.40(10) 1_565 . ? O10 Rb3 Rb2 43.79(9) 1_565 . ? O6 Rb3 Rb2 147.56(10) 1_565 . ? O9 Rb3 Rb2 81.39(10) 1_565 . ? O6W Rb3 Rb2 41.66(11) . . ? O3W Rb3 Rb2 102.75(14) . . ? O21 S1 O22 111.2(3) . . ? O21 S1 O24 109.1(4) . . ? O22 S1 O24 109.1(3) . . ? O21 S1 O23 109.2(3) . . ? O22 S1 O23 109.7(3) . . ? O24 S1 O23 108.5(3) . . ? O21 S1 Rb2 116.3(3) . . ? O22 S1 Rb2 125.8(2) . . ? O24 S1 Rb2 30.9(2) . . ? O23 S1 Rb2 78.0(2) . . ? C25 O1 Rb1 131.6(4) . . ? C25 O1 Rb2 123.5(4) . . ? Rb1 O1 Rb2 104.72(14) . . ? C25 N1 C16 112.5(5) . . ? C25 N1 C17 122.6(5) . . ? C16 N1 C17 123.5(5) . . ? O15 C1 N10 112.9(5) . . ? O15 C1 N9 107.6(5) . . ? N10 C1 N9 115.7(5) . . ? O15 C1 C16 115.0(5) . . ? N10 C1 C16 103.1(5) . . ? N9 C1 C16 102.3(5) . . ? C9 O2 Rb1 131.6(4) . . ? C9 N2 C2 112.5(5) . . ? C9 N2 C10 123.6(5) . . ? C2 N2 C10 123.8(5) . . ? O11 C2 N6 112.2(5) . . ? O11 C2 N2 109.6(5) . . ? N6 C2 N2 115.0(5) . . ? O11 C2 C4 114.0(5) . . ? N6 C2 C4 102.6(5) . . ? N2 C2 C4 103.0(5) . . ? C23 O3 Rb1 138.0(4) . . ? C29 N3 C19 122.5(5) . . ? C29 N3 C12 112.3(5) . . ? C19 N3 C12 125.2(5) . . ? O18 C3 N15 107.6(5) . . ? O18 C3 N20 113.2(5) . . ? N15 C3 N20 115.7(5) . . ? O18 C3 C13 114.0(5) . . ? N15 C3 C13 102.8(5) . . ? N20 C3 C13 103.2(5) . . ? C30 O4 Rb1 130.6(4) . . ? C21 N4 C13 113.1(5) . . ? C21 N4 C19 122.2(5) . . ? C13 N4 C19 124.7(5) . . ? O14 C4 N11 112.6(5) . . ? O14 C4 N12 108.3(5) . . ? N11 C4 N12 115.2(5) . . ? O14 C4 C2 115.9(5) . . ? N11 C4 C2 102.3(5) . . ? N12 C4 C2 102.3(5) . . ? C14 O5 Rb1 132.7(4) . . ? C29 N5 C8 121.9(5) . . ? C29 N5 C15 111.9(5) . . ? C8 N5 C15 123.6(5) . . ? N7 C5 N18 114.0(5) . . ? N7 C5 H5A 108.8 . . ? N18 C5 H5A 108.8 . . ? N7 C5 H5B 108.8 . . ? N18 C5 H5B 108.8 . . ? H5A C5 H5B 107.7 . . ? C21 O6 Rb3 134.3(4) . 1_545 ? N10 C6 N12 113.8(5) . . ? N10 C6 H6A 108.8 . . ? N12 C6 H6A 108.8 . . ? N10 C6 H6B 108.8 . . ? N12 C6 H6B 108.8 . . ? H6A C6 H6B 107.7 . . ? C22 O7 Rb3 146.1(4) . 1_545 ? C14 N7 C15 112.2(5) . . ? C14 N7 C5 122.4(5) . . ? C15 N7 C5 124.8(5) . . ? O19 C7 N18 111.9(5) . . ? O19 C7 N19 108.2(5) . . ? N18 C7 N19 116.3(5) . . ? O19 C7 C18 113.7(5) . . ? N18 C7 C18 103.7(5) . . ? N19 C7 C18 102.8(5) . . ? C29 O8 Rb3 134.5(4) . 1_545 ? C30 N8 C17 122.8(5) . . ? C30 N8 C18 112.0(5) . . ? C17 N8 C18 123.5(5) . . ? N19 C8 N5 113.1(5) . . ? N19 C8 H8A 109.0 . . ? N5 C8 H8A 109.0 . . ? N19 C8 H8B 109.0 . . ? N5 C8 H8B 109.0 . . ? H8A C8 H8B 107.8 . . ? C26 O9 Rb3 133.9(4) . 1_545 ? C26 N9 C1 112.7(5) . . ? C26 N9 C11 121.5(5) . . ? C1 N9 C11 123.3(5) . . ? O2 C9 N2 125.0(6) . . ? O2 C9 N12 125.7(6) . . ? N2 C9 N12 109.3(5) . . ? C24 O10 Rb2 133.0(4) . 1_545 ? C24 O10 Rb3 135.3(4) . 1_545 ? Rb2 O10 Rb3 91.71(13) 1_545 1_545 ? C25 N10 C1 112.3(5) . . ? C25 N10 C6 122.5(5) . . ? C1 N10 C6 124.9(5) . . ? N2 C10 N20 114.1(5) . . ? N2 C10 H10A 108.7 . . ? N20 C10 H10A 108.7 . . ? N2 C10 H10B 108.7 . . ? N20 C10 H10B 108.7 . . ? H10A C10 H10B 107.6 . . ? C22 N11 C4 113.3(5) . . ? C22 N11 C11 121.6(5) . . ? C4 N11 C11 124.7(5) . . ? N11 C11 N9 113.5(5) . . ? N11 C11 H11A 108.9 . . ? N9 C11 H11A 108.9 . . ? N11 C11 H11B 108.9 . . ? N9 C11 H11B 108.9 . . ? H11A C11 H11B 107.7 . . ? C13 O12 H12A 109.5 . . ? C9 N12 C4 112.4(5) . . ? C9 N12 C6 123.0(5) . . ? C4 N12 C6 122.8(5) . . ? O20 C12 N17 107.7(5) . . ? O20 C12 N3 111.6(5) . . ? N17 C12 N3 115.9(5) . . ? O20 C12 C15 115.2(5) . . ? N17 C12 C15 103.3(5) . . ? N3 C12 C15 103.1(5) . . ? C18 O13 H13A 109.5 . . ? C24 N13 C18 112.7(5) . . ? C24 N13 C20 122.4(5) . . ? C18 N13 C20 124.9(5) . . ? O12 C13 N14 108.3(5) . . ? O12 C13 N4 112.0(5) . . ? N14 C13 N4 115.5(5) . . ? O12 C13 C3 115.5(5) . . ? N14 C13 C3 102.9(5) . . ? N4 C13 C3 102.4(5) . . ? C4 O14 H14A 109.5 . . ? C23 N14 C13 112.3(5) . . ? C23 N14 C28 122.2(5) . . ? C13 N14 C28 124.4(5) . . ? O5 C14 N17 125.7(6) . . ? O5 C14 N7 125.5(6) . . ? N17 C14 N7 108.8(5) . . ? C1 O15 H15A 109.5 . . ? C21 N15 C3 113.1(5) . . ? C21 N15 C27 121.9(5) . . ? C3 N15 C27 124.3(5) . . ? O16 C15 N7 108.7(5) . . ? O16 C15 N5 111.8(5) . . ? N7 C15 N5 115.5(5) . . ? O16 C15 C12 115.1(5) . . ? N7 C15 C12 102.7(5) . . ? N5 C15 C12 102.8(5) . . ? C15 O16 H16A 109.5 . . ? C26 N16 C16 112.4(5) . . ? C26 N16 C20 122.1(5) . . ? C16 N16 C20 125.5(5) . . ? O17 C16 N16 108.4(5) . . ? O17 C16 N1 111.8(5) . . ? N16 C16 N1 115.6(5) . . ? O17 C16 C1 115.0(5) . . ? N16 C16 C1 103.5(5) . . ? N1 C16 C1 102.4(5) . . ? C14 N17 C12 112.1(5) . . ? C14 N17 C28 122.2(5) . . ? C12 N17 C28 123.7(5) . . ? N8 C17 N1 112.8(5) . . ? N8 C17 H17A 109.0 . . ? N1 C17 H17A 109.0 . . ? N8 C17 H17B 109.0 . . ? N1 C17 H17B 109.0 . . ? H17A C17 H17B 107.8 . . ? C3 O18 H18A 109.5 . . ? C30 N18 C7 111.9(5) . . ? C30 N18 C5 122.7(5) . . ? C7 N18 C5 125.0(5) . . ? O13 C18 N13 113.0(5) . . ? O13 C18 N8 106.8(5) . . ? N13 C18 N8 114.7(5) . . ? O13 C18 C7 116.4(5) . . ? N13 C18 C7 103.4(5) . . ? N8 C18 C7 102.3(5) . . ? C7 O19 Rb2 142.2(4) . 2_655 ? C24 N19 C8 122.7(5) . . ? C24 N19 C7 112.6(5) . . ? C8 N19 C7 124.7(5) . . ? N3 C19 N4 114.4(5) . . ? N3 C19 H19A 108.7 . . ? N4 C19 H19A 108.7 . . ? N3 C19 H19B 108.7 . . ? N4 C19 H19B 108.7 . . ? H19A C19 H19B 107.6 . . ? C12 O20 H20C 109.5 . . ? C23 N20 C3 112.2(5) . . ? C23 N20 C10 122.0(5) . . ? C3 N20 C10 125.6(5) . . ? N16 C20 N13 114.3(5) . . ? N16 C20 H20A 108.7 . . ? N13 C20 H20A 108.7 . . ? N16 C20 H20B 108.7 . . ? N13 C20 H20B 108.7 . . ? H20A C20 H20B 107.6 . . ? C16 O17 H17C 109.5 . . ? C22 N6 C2 113.3(5) . . ? C22 N6 C27 121.4(5) . . ? C2 N6 C27 125.3(5) . . ? O6 C21 N15 125.4(6) . . ? O6 C21 N4 126.4(6) . . ? N15 C21 N4 108.2(5) . . ? O7 C22 N6 126.4(6) . . ? O7 C22 N11 125.4(6) . . ? N6 C22 N11 108.2(5) . . ? O3 C23 N20 126.5(6) . . ? O3 C23 N14 124.4(6) . . ? N20 C23 N14 109.0(5) . . ? O10 C24 N13 126.5(6) . . ? O10 C24 N19 125.1(6) . . ? N13 C24 N19 108.4(5) . . ? O1 C25 N10 125.5(6) . . ? O1 C25 N1 125.5(6) . . ? N10 C25 N1 109.0(5) . . ? O9 C26 N9 126.9(6) . . ? O9 C26 N16 124.8(6) . . ? N9 C26 N16 108.3(5) . . ? N6 C27 N15 113.9(5) . . ? N6 C27 H27A 108.8 . . ? N15 C27 H27A 108.8 . . ? N6 C27 H27B 108.8 . . ? N15 C27 H27B 108.8 . . ? H27A C27 H27B 107.7 . . ? N14 C28 N17 112.9(5) . . ? N14 C28 H28A 109.0 . . ? N17 C28 H28A 109.0 . . ? N14 C28 H28B 109.0 . . ? N17 C28 H28B 109.0 . . ? H28A C28 H28B 107.8 . . ? O8 C29 N5 125.7(6) . . ? O8 C29 N3 125.8(6) . . ? N5 C29 N3 108.5(5) . . ? O4 C30 N8 125.6(6) . . ? O4 C30 N18 125.3(6) . . ? N8 C30 N18 109.1(5) . . ? S1 O24 Rb2 133.6(3) . . ? H11D O11W H11C 108.5 . . ? Rb2 O10W H10C 111.5 . . ? Rb2 O10W H10D 111.4 . . ? H10C O10W H10D 109.4 . . ? H7WA O7W H7WB 108.3 . . ? Rb2 O6W Rb3 91.21(16) . . ? Rb2 O6W Rb1 102.10(19) . . ? Rb3 O6W Rb1 166.4(2) . . ? Rb1 O5W H5WA 110.0 . . ? Rb1 O5W H5WB 110.0 . . ? H5WA O5W H5WB 108.4 . . ? Rb3 O4W Rb2 89.26(19) . . ? H2WA O2W H2WB 108.9 . . ? O1W O1W' Rb3 170.4(15) . 1_545 ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 2.888 _refine_diff_density_min -4.357 _refine_diff_density_rms 0.239 #===END data_complex3 _database_code_depnum_ccdc_archive 'CCDC 806943' #TrackingRef '- complex1-3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H40 Cs2 N20 O29 S' _chemical_formula_weight 1442.70 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' Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 15.618(4) _cell_length_b 14.081(4) _cell_length_c 21.400(6) _cell_angle_alpha 90.00 _cell_angle_beta 100.475(3) _cell_angle_gamma 90.00 _cell_volume 4628(2) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 5419 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 25.82 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.31 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.071 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2872 _exptl_absorpt_coefficient_mu 1.746 _exptl_absorpt_correction_type 'multi scan' _exptl_absorpt_correction_T_min 0.5347 _exptl_absorpt_correction_T_max 0.6137 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 Smart Apex CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 14655 _diffrn_reflns_av_R_equivalents 0.0538 _diffrn_reflns_av_sigmaI/netI 0.0513 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 25.97 _reflns_number_total 4286 _reflns_number_gt 4014 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0537P)^2^+321.6475P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4286 _refine_ls_number_parameters 390 _refine_ls_number_restraints 54 _refine_ls_R_factor_all 0.1012 _refine_ls_R_factor_gt 0.0982 _refine_ls_wR_factor_ref 0.2497 _refine_ls_wR_factor_gt 0.2481 _refine_ls_goodness_of_fit_ref 1.248 _refine_ls_restrained_S_all 1.245 _refine_ls_shift/su_max 0.089 _refine_ls_shift/su_mean 0.012 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 Cs1 Cs 0.25604(5) 0.07411(6) 0.17644(4) 0.0292(3) Uani 1 1 d . . . O6 O 0.1459(7) 0.3315(7) 0.4459(4) 0.032(2) Uani 1 1 d . . . H6C H 0.1110 0.3620 0.4630 0.048 Uiso 1 1 calc R . . N1 N -0.0263(7) 0.2365(7) 0.0962(5) 0.023(2) Uani 1 1 d . . . C1 C 0.0195(8) -0.1654(8) 0.1139(5) 0.018(2) Uani 1 1 d U . . H1A H -0.0129 -0.2192 0.0922 0.021 Uiso 1 1 calc R . . H1B H 0.0760 -0.1627 0.1001 0.021 Uiso 1 1 calc R . . S1 S 0.0000 0.5000 0.5000 0.0467(15) Uani 1 2 d S . . O1W O 0.0000 0.071(3) 0.2500 0.188(18) Uani 1 2 d S . . O7 O -0.1494(6) -0.1410(6) 0.0295(4) 0.0246(19) Uani 1 1 d U . . H7A H -0.1380 -0.1951 0.0440 0.037 Uiso 1 1 calc R . . N2 N 0.1634(7) 0.2331(7) 0.3639(5) 0.020(2) Uani 1 1 d . . . C2 C 0.1019(7) 0.2879(8) 0.3920(5) 0.017(2) Uani 1 1 d U . . O2W O 0.0867(7) -0.3918(8) 0.1505(5) 0.041(3) Uani 1 1 d . . . H2WA H 0.1373 -0.4139 0.1643 0.050 Uiso 1 1 d R . . H2WB H 0.0606 -0.4300 0.1226 0.050 Uiso 1 1 d R . . O5 O -0.2565(6) 0.0111(6) 0.1813(4) 0.0247(19) Uani 1 1 d . . . N3 N -0.1893(7) 0.0697(7) 0.1009(5) 0.025(2) Uani 1 1 d . . . C3 C -0.0607(7) 0.3553(8) 0.1643(5) 0.016(2) Uani 1 1 d U . . O3W O -0.3164(10) -0.1474(11) -0.0143(11) 0.127(9) Uani 1 1 d . . . H3WA H -0.2623 -0.1432 0.0007 0.152 Uiso 1 1 d R . . H3WB H -0.3410 -0.0964 -0.0058 0.152 Uiso 1 1 d R . . O4 O 0.1227(6) 0.2399(7) 0.1268(4) 0.028(2) Uani 1 1 d . . . N4 N -0.1688(7) -0.0809(7) 0.1288(4) 0.022(2) Uani 1 1 d . . . C4 C -0.1742(7) -0.1690(8) 0.1649(5) 0.012(2) Uani 1 1 d U . . H4A H -0.2294 -0.1693 0.1806 0.015 Uiso 1 1 calc R . . H4B H -0.1750 -0.2232 0.1360 0.015 Uiso 1 1 calc R . . O3 O 0.1686(6) -0.1113(6) 0.2041(4) 0.0247(19) Uani 1 1 d . . . N5 N 0.1061(7) 0.3265(7) 0.2843(5) 0.024(2) Uani 1 1 d . . . C5 C 0.0100(8) 0.0046(8) 0.0824(5) 0.019(2) Uani 1 1 d U . . O8 O -0.0767(6) 0.4522(5) 0.1532(4) 0.0233(19) Uani 1 1 d . . . N6 N -0.1041(7) -0.1818(7) 0.2179(5) 0.019(2) Uani 1 1 d . . . C6 C 0.0943(8) 0.3750(8) 0.2235(5) 0.019(2) Uani 1 1 d . . . H6A H 0.0774 0.4409 0.2296 0.023 Uiso 1 1 calc R . . H6B H 0.1503 0.3764 0.2090 0.023 Uiso 1 1 calc R . . O2 O 0.0893(6) 0.0169(6) 0.0882(4) 0.0246(19) Uani 1 1 d . . . N7 N 0.0342(7) -0.1821(7) 0.1819(4) 0.020(2) Uani 1 1 d . . . C7 C 0.0504(8) 0.2659(8) 0.1310(5) 0.020(2) Uani 1 1 d . . . O1 O 0.2120(6) 0.2208(6) 0.2695(4) 0.0253(19) Uani 1 1 d . . . N8 N 0.0299(7) 0.3328(7) 0.1741(5) 0.023(2) Uani 1 1 d . . . C8 C 0.1100(7) -0.1532(8) 0.2212(5) 0.015(2) Uani 1 1 d . . . O9 O -0.0483(6) -0.3204(6) 0.1888(4) 0.0203(18) Uani 1 1 d . . . N9 N -0.0510(7) 0.0719(8) 0.0629(5) 0.026(2) Uani 1 1 d . . . C9 C -0.2232(8) 0.1648(8) 0.0991(6) 0.019(2) Uani 1 1 d . . . H9A H -0.2778 0.1641 0.1156 0.023 Uiso 1 1 calc R . . H9B H -0.2366 0.1860 0.0548 0.023 Uiso 1 1 calc R . . O10 O -0.1869(6) 0.0469(7) -0.0042(4) 0.031(2) Uani 1 1 d . . . H10A H -0.1581 0.0282 -0.0308 0.047 Uiso 1 1 calc R . . N10 N -0.0284(7) -0.0778(8) 0.0941(5) 0.025(2) Uani 1 1 d . . . C10 C 0.1652(8) 0.2568(8) 0.3023(6) 0.020(2) Uani 1 1 d . . . C11 C -0.2089(7) 0.0003(8) 0.1405(5) 0.016(2) Uani 1 1 d . . . O11 O -0.0109(18) 0.6099(14) 0.4926(12) 0.053(6) Uani 0.50 1 d P . . C12 C -0.0287(9) 0.1673(9) 0.0458(6) 0.026(3) Uani 1 1 d . . . H12A H 0.0285 0.1657 0.0331 0.031 Uiso 1 1 calc R . . H12B H -0.0712 0.1881 0.0089 0.031 Uiso 1 1 calc R . . O12 O 0.0393(15) 0.5315(15) 0.4531(9) 0.040(5) Uani 0.50 1 d P . . C13 C -0.1383(8) 0.0334(8) 0.0576(5) 0.018(2) Uani 1 1 d U . . O13 O -0.0295(16) 0.4700(18) 0.4335(12) 0.055(6) Uani 0.50 1 d PU . . C14 C -0.1215(8) -0.0730(8) 0.0774(5) 0.020(2) Uani 1 1 d . . . O14 O -0.0998(18) 0.512(2) 0.4901(13) 0.065(7) Uani 0.50 1 d P . . C15 C -0.0251(7) -0.2320(8) 0.2137(5) 0.015(2) Uani 1 1 d U . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cs1 0.0330(5) 0.0211(4) 0.0347(5) 0.0016(4) 0.0095(3) -0.0008(3) O6 0.056(6) 0.028(5) 0.008(4) -0.008(4) -0.007(4) 0.009(4) N1 0.035(6) 0.023(5) 0.013(5) -0.009(4) 0.010(4) 0.000(5) C1 0.024(4) 0.017(4) 0.014(4) -0.004(3) 0.006(3) 0.003(3) S1 0.064(4) 0.052(4) 0.022(3) -0.013(2) 0.003(2) 0.027(3) O1W 0.22(5) 0.14(3) 0.18(4) 0.000 -0.01(3) 0.000 O7 0.037(4) 0.023(3) 0.013(3) -0.001(3) 0.000(3) -0.001(3) N2 0.027(5) 0.015(5) 0.020(5) -0.005(4) 0.011(4) 0.001(4) C2 0.021(4) 0.017(4) 0.011(4) -0.002(3) -0.001(3) -0.001(3) O2W 0.040(6) 0.048(6) 0.037(6) -0.009(5) 0.009(5) 0.010(5) O5 0.038(5) 0.018(4) 0.020(4) 0.006(4) 0.010(4) 0.009(4) N3 0.042(6) 0.018(5) 0.016(5) 0.001(4) 0.006(4) 0.001(5) C3 0.021(4) 0.014(4) 0.013(4) 0.007(3) 0.006(3) 0.003(3) O3W 0.060(9) 0.050(9) 0.24(3) -0.043(12) -0.057(12) 0.014(7) O4 0.031(5) 0.034(5) 0.022(5) -0.007(4) 0.014(4) 0.000(4) N4 0.032(6) 0.020(5) 0.013(5) 0.008(4) 0.007(4) 0.003(4) C4 0.018(4) 0.013(4) 0.006(4) 0.000(3) 0.003(3) -0.004(3) O3 0.032(5) 0.025(5) 0.019(4) 0.008(4) 0.007(4) -0.008(4) N5 0.034(6) 0.023(5) 0.020(5) 0.000(4) 0.016(5) 0.004(5) C5 0.025(4) 0.021(4) 0.012(4) -0.001(3) 0.005(3) -0.002(4) O8 0.045(5) 0.008(4) 0.018(4) 0.001(3) 0.009(4) 0.002(4) N6 0.027(5) 0.021(5) 0.010(5) -0.001(4) 0.000(4) 0.006(4) C6 0.029(6) 0.017(6) 0.016(6) -0.007(5) 0.015(5) -0.001(5) O2 0.034(5) 0.030(5) 0.011(4) -0.001(4) 0.006(4) -0.006(4) N7 0.026(5) 0.024(5) 0.009(5) 0.001(4) 0.003(4) -0.003(4) C7 0.035(7) 0.015(6) 0.012(5) 0.007(4) 0.009(5) 0.006(5) O1 0.036(5) 0.020(4) 0.020(4) -0.002(4) 0.006(4) 0.005(4) N8 0.028(6) 0.018(5) 0.025(6) -0.005(4) 0.011(4) 0.004(4) C8 0.025(6) 0.011(5) 0.009(5) -0.002(4) 0.003(4) 0.002(4) O9 0.033(5) 0.016(4) 0.012(4) -0.001(3) 0.004(3) -0.004(3) N9 0.036(6) 0.020(5) 0.021(5) 0.002(4) 0.004(4) -0.006(5) C9 0.024(6) 0.014(6) 0.018(6) 0.006(5) 0.003(5) 0.001(5) O10 0.047(6) 0.035(5) 0.010(4) 0.003(4) 0.005(4) 0.002(4) N10 0.031(6) 0.024(5) 0.025(5) 0.001(5) 0.012(4) 0.003(5) C10 0.032(6) 0.014(5) 0.017(6) 0.002(5) 0.015(5) -0.002(5) C11 0.027(6) 0.017(6) 0.003(5) 0.000(4) 0.000(4) -0.005(5) O11 0.091(19) 0.021(10) 0.055(15) -0.012(10) 0.037(14) 0.002(11) C12 0.042(8) 0.017(6) 0.020(6) -0.006(5) 0.009(6) -0.006(5) O12 0.071(15) 0.039(12) 0.012(9) -0.008(8) 0.013(9) -0.004(10) C13 0.023(4) 0.020(4) 0.011(4) -0.002(3) 0.002(3) 0.001(3) O13 0.057(7) 0.057(7) 0.053(7) -0.005(5) 0.014(5) -0.001(5) C14 0.037(7) 0.013(5) 0.011(5) -0.004(5) 0.008(5) -0.001(5) O14 0.076(18) 0.062(17) 0.060(17) 0.000(14) 0.017(14) 0.025(14) C15 0.020(4) 0.015(4) 0.011(4) 0.003(3) 0.005(3) -0.001(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 Cs1 O1 3.034(8) . ? Cs1 O2 3.035(8) . ? Cs1 O3 3.054(8) . ? Cs1 O5 3.169(9) 2 ? Cs1 O4 3.180(9) . ? Cs1 O8 3.239(9) 3_545 ? Cs1 O9 3.365(8) 3 ? Cs1 C4 3.798(10) 3 ? O6 C2 1.374(14) . ? O6 H6C 0.8300 . ? N1 C7 1.356(16) . ? N1 C2 1.445(15) 2 ? N1 C12 1.449(15) . ? C1 N7 1.452(14) . ? C1 N10 1.464(15) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? S1 O12 1.34(2) . ? S1 O12 1.34(2) 5_566 ? S1 O13 1.47(3) . ? S1 O13 1.47(3) 5_566 ? S1 O14 1.54(3) 5_566 ? S1 O14 1.54(3) . ? S1 O11 1.56(2) . ? S1 O11 1.56(2) 5_566 ? O7 C14 1.413(13) . ? O7 H7A 0.8300 . ? N2 C10 1.367(15) . ? N2 C2 1.446(15) . ? N2 C9 1.468(15) 2 ? C2 N1 1.445(15) 2 ? C2 C3 1.576(16) 2 ? O2W H2WA 0.8500 . ? O2W H2WB 0.8500 . ? O5 C11 1.255(14) . ? O5 Cs1 3.169(9) 2 ? N3 C11 1.365(15) . ? N3 C13 1.422(15) . ? N3 C9 1.437(15) . ? C3 O8 1.400(13) . ? C3 N8 1.427(15) . ? C3 N5 1.469(14) 2 ? C3 C2 1.576(16) 2 ? O3W H3WA 0.8500 . ? O3W H3WB 0.8500 . ? O4 C7 1.206(15) . ? N4 C11 1.348(15) . ? N4 C14 1.438(15) . ? N4 C4 1.472(14) . ? C4 N6 1.439(14) . ? C4 Cs1 3.798(10) 3_445 ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? O3 C8 1.200(14) . ? N5 C10 1.355(16) . ? N5 C6 1.452(15) . ? N5 C3 1.469(14) 2 ? C5 O2 1.233(14) . ? C5 N10 1.351(16) . ? C5 N9 1.354(16) . ? O8 Cs1 3.239(9) 3_455 ? N6 C8 1.382(14) 2 ? N6 C15 1.438(15) . ? C6 N8 1.448(16) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? N7 C8 1.383(15) . ? N7 C15 1.430(14) . ? C7 N8 1.395(15) . ? O1 C10 1.212(14) . ? C8 N6 1.382(14) 2 ? O9 C15 1.377(13) . ? O9 Cs1 3.365(8) 3_445 ? N9 C13 1.453(16) . ? N9 C12 1.452(16) . ? C9 N2 1.468(15) 2 ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? O10 C13 1.412(14) . ? O10 H10A 0.8300 . ? N10 C14 1.434(16) . ? O11 O12 1.67(3) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? O12 O13 1.38(3) . ? O12 O14 1.53(3) 5_566 ? C13 C14 1.566(16) . ? O14 O12 1.53(3) 5_566 ? C15 C15 1.61(2) 2 ? 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 O1 Cs1 O2 108.5(2) . . ? O1 Cs1 O3 107.0(2) . . ? O2 Cs1 O3 62.0(2) . . ? O1 Cs1 O5 61.4(2) . 2 ? O2 Cs1 O5 112.0(2) . 2 ? O3 Cs1 O5 59.8(2) . 2 ? O1 Cs1 O4 60.4(2) . . ? O2 Cs1 O4 63.4(2) . . ? O3 Cs1 O4 113.8(2) . . ? O5 Cs1 O4 114.4(2) 2 . ? O1 Cs1 O8 138.3(2) . 3_545 ? O2 Cs1 O8 112.9(2) . 3_545 ? O3 Cs1 O8 88.8(2) . 3_545 ? O5 Cs1 O8 97.9(2) 2 3_545 ? O4 Cs1 O8 146.6(2) . 3_545 ? O1 Cs1 O9 87.6(2) . 3 ? O2 Cs1 O9 146.2(2) . 3 ? O3 Cs1 O9 142.6(2) . 3 ? O5 Cs1 O9 101.8(2) 2 3 ? O4 Cs1 O9 103.4(2) . 3 ? O8 Cs1 O9 60.0(2) 3_545 3 ? O1 Cs1 C4 59.7(2) . 3 ? O2 Cs1 C4 115.9(2) . 3 ? O3 Cs1 C4 166.0(2) . 3 ? O5 Cs1 C4 112.2(2) 2 3 ? O4 Cs1 C4 57.1(2) . 3 ? O8 Cs1 C4 104.2(2) 3_545 3 ? O9 Cs1 C4 47.0(2) 3 3 ? C2 O6 H6C 109.5 . . ? C7 N1 C2 114.8(9) . 2 ? C7 N1 C12 121.0(11) . . ? C2 N1 C12 123.7(10) 2 . ? N7 C1 N10 114.0(9) . . ? N7 C1 H1A 108.8 . . ? N10 C1 H1A 108.8 . . ? N7 C1 H1B 108.8 . . ? N10 C1 H1B 108.8 . . ? H1A C1 H1B 107.7 . . ? O12 S1 O12 180.000(7) . 5_566 ? O12 S1 O13 58.6(12) . . ? O12 S1 O13 121.4(13) 5_566 . ? O12 S1 O13 121.4(13) . 5_566 ? O12 S1 O13 58.6(12) 5_566 5_566 ? O13 S1 O13 180.000(7) . 5_566 ? O12 S1 O14 63.5(14) . 5_566 ? O12 S1 O14 116.5(14) 5_566 5_566 ? O13 S1 O14 103.4(14) . 5_566 ? O13 S1 O14 76.6(14) 5_566 5_566 ? O12 S1 O14 116.5(14) . . ? O12 S1 O14 63.5(14) 5_566 . ? O13 S1 O14 76.6(14) . . ? O13 S1 O14 103.4(14) 5_566 . ? O14 S1 O14 180.000(5) 5_566 . ? O12 S1 O11 69.7(12) . . ? O12 S1 O11 110.3(12) 5_566 . ? O13 S1 O11 100.2(14) . . ? O13 S1 O11 79.8(14) 5_566 . ? O14 S1 O11 102.3(15) 5_566 . ? O14 S1 O11 77.7(15) . . ? O12 S1 O11 110.3(12) . 5_566 ? O12 S1 O11 69.7(12) 5_566 5_566 ? O13 S1 O11 79.8(14) . 5_566 ? O13 S1 O11 100.2(14) 5_566 5_566 ? O14 S1 O11 77.7(15) 5_566 5_566 ? O14 S1 O11 102.3(15) . 5_566 ? O11 S1 O11 180.000(5) . 5_566 ? C14 O7 H7A 109.5 . . ? C10 N2 C2 113.8(10) . . ? C10 N2 C9 123.8(10) . 2 ? C2 N2 C9 122.2(9) . 2 ? O6 C2 N1 112.2(10) . 2 ? O6 C2 N2 108.5(9) . . ? N1 C2 N2 115.5(10) 2 . ? O6 C2 C3 116.4(9) . 2 ? N1 C2 C3 101.7(9) 2 2 ? N2 C2 C3 102.3(9) . 2 ? H2WA O2W H2WB 108.0 . . ? C11 O5 Cs1 143.6(8) . 2 ? C11 N3 C13 111.3(10) . . ? C11 N3 C9 124.1(10) . . ? C13 N3 C9 124.4(10) . . ? O8 C3 N8 112.5(10) . . ? O8 C3 N5 107.5(9) . 2 ? N8 C3 N5 115.4(9) . 2 ? O8 C3 C2 114.9(9) . 2 ? N8 C3 C2 103.5(9) . 2 ? N5 C3 C2 102.8(9) 2 2 ? H3WA O3W H3WB 108.5 . . ? C7 O4 Cs1 139.7(8) . . ? C11 N4 C14 113.4(9) . . ? C11 N4 C4 123.0(9) . . ? C14 N4 C4 123.6(10) . . ? N6 C4 N4 114.3(9) . . ? N6 C4 Cs1 90.9(6) . 3_445 ? N4 C4 Cs1 151.8(7) . 3_445 ? N6 C4 H4A 108.7 . . ? N4 C4 H4A 108.7 . . ? Cs1 C4 H4A 72.2 3_445 . ? N6 C4 H4B 108.7 . . ? N4 C4 H4B 108.7 . . ? Cs1 C4 H4B 47.9 3_445 . ? H4A C4 H4B 107.6 . . ? C8 O3 Cs1 150.7(8) . . ? C10 N5 C6 124.3(10) . . ? C10 N5 C3 112.6(10) . 2 ? C6 N5 C3 122.8(10) . 2 ? O2 C5 N10 125.0(11) . . ? O2 C5 N9 124.8(11) . . ? N10 C5 N9 110.2(10) . . ? C3 O8 Cs1 127.9(7) . 3_455 ? C8 N6 C15 114.0(9) 2 . ? C8 N6 C4 122.4(10) 2 . ? C15 N6 C4 123.4(9) . . ? N8 C6 N5 114.8(10) . . ? N8 C6 H6A 108.6 . . ? N5 C6 H6A 108.6 . . ? N8 C6 H6B 108.6 . . ? N5 C6 H6B 108.6 . . ? H6A C6 H6B 107.6 . . ? C5 O2 Cs1 146.3(7) . . ? C8 N7 C15 114.3(9) . . ? C8 N7 C1 121.6(10) . . ? C15 N7 C1 124.1(9) . . ? O4 C7 N1 127.8(11) . . ? O4 C7 N8 125.8(12) . . ? N1 C7 N8 106.4(10) . . ? C10 O1 Cs1 153.8(8) . . ? C7 N8 C3 113.2(10) . . ? C7 N8 C6 123.2(10) . . ? C3 N8 C6 123.7(10) . . ? O3 C8 N6 128.0(11) . 2 ? O3 C8 N7 125.1(10) . . ? N6 C8 N7 106.9(10) 2 . ? C15 O9 Cs1 126.9(6) . 3_445 ? C5 N9 C13 111.2(10) . . ? C5 N9 C12 122.5(11) . . ? C13 N9 C12 126.2(11) . . ? N3 C9 N2 113.6(10) . 2 ? N3 C9 H9A 108.8 . . ? N2 C9 H9A 108.9 2 . ? N3 C9 H9B 108.8 . . ? N2 C9 H9B 108.8 2 . ? H9A C9 H9B 107.7 . . ? C13 O10 H10A 109.5 . . ? C5 N10 C14 112.2(10) . . ? C5 N10 C1 123.8(10) . . ? C14 N10 C1 123.7(10) . . ? O1 C10 N5 126.2(11) . . ? O1 C10 N2 125.3(11) . . ? N5 C10 N2 108.5(10) . . ? O5 C11 N4 125.8(10) . . ? O5 C11 N3 125.0(11) . . ? N4 C11 N3 109.2(10) . . ? S1 O11 O12 49.0(9) . . ? N1 C12 N9 114.1(10) . . ? N1 C12 H12A 108.7 . . ? N9 C12 H12A 108.7 . . ? N1 C12 H12B 108.7 . . ? N9 C12 H12B 108.7 . . ? H12A C12 H12B 107.6 . . ? S1 O12 O13 65.5(15) . . ? S1 O12 O14 64.7(14) . 5_566 ? O13 O12 O14 109(2) . 5_566 ? S1 O12 O11 61.3(11) . . ? O13 O12 O11 99.0(19) . . ? O14 O12 O11 98.2(16) 5_566 . ? O10 C13 N3 107.1(9) . . ? O10 C13 N9 111.2(10) . . ? N3 C13 N9 116.3(10) . . ? O10 C13 C14 114.6(9) . . ? N3 C13 C14 104.7(9) . . ? N9 C13 C14 103.0(9) . . ? O12 O13 S1 56.0(12) . . ? O7 C14 N10 108.3(9) . . ? O7 C14 N4 111.6(10) . . ? N10 C14 N4 116.4(10) . . ? O7 C14 C13 115.9(9) . . ? N10 C14 C13 103.1(9) . . ? N4 C14 C13 101.3(9) . . ? O12 O14 S1 51.9(12) 5_566 . ? O9 C15 N7 114.0(9) . . ? O9 C15 N6 107.5(9) . . ? N7 C15 N6 115.2(9) . . ? O9 C15 C15 114.9(6) . 2 ? N7 C15 C15 102.4(9) . 2 ? N6 C15 C15 102.3(9) . 2 ? _diffrn_measured_fraction_theta_max 0.945 _diffrn_reflns_theta_full 25.97 _diffrn_measured_fraction_theta_full 0.945 _refine_diff_density_max 1.883 _refine_diff_density_min -1.694 _refine_diff_density_rms 0.220 #===END