# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_A _database_code_depnum_ccdc_archive 'CCDC 742107' #TrackingRef 'web_deposit_cif_file_0_Xin-longNi_1352613104.A.submit.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H56 I2 K2 N20 O17' _chemical_formula_weight 1541.15 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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' _cell_length_a 11.997(14) _cell_length_b 15.364(17) _cell_length_c 16.000(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2949(6) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.735 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1552 _exptl_absorpt_coefficient_mu 1.296 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19598 _diffrn_reflns_av_R_equivalents 0.0966 _diffrn_reflns_av_sigmaI/netI 0.1133 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.27 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5313 _reflns_number_gt 2852 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0722P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0051(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00 _refine_ls_number_reflns 5313 _refine_ls_number_parameters 423 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1331 _refine_ls_R_factor_gt 0.0580 _refine_ls_wR_factor_ref 0.1550 _refine_ls_wR_factor_gt 0.1325 _refine_ls_goodness_of_fit_ref 0.932 _refine_ls_restrained_S_all 0.932 _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 O1W O 0.0000 0.0000 0.2584(6) 0.116(4) Uani 1 2 d S . . O2W O -0.0153(6) 0.1050(5) 0.0658(5) 0.110(3) Uani 1 1 d . . . O3W O 0.0000 0.0000 -0.0903(8) 0.146(5) Uani 1 2 d S . . O4W O -0.5000 0.0000 0.1728(15) 0.330(16) Uani 1 2 d S . . K1 K -0.19101(17) 0.07589(14) 0.16869(13) 0.0709(7) Uani 1 1 d . . . I1 I 0.78212(13) 0.9977(2) 0.76147(10) 0.0628(10) Uani 0.718(17) 1 d P A 1 I1' I 0.7502(19) 1.0269(12) 0.7320(16) 0.149(7) Uani 0.282(17) 1 d P A 2 C16 C 0.6286(10) 0.1724(9) 0.6043(9) 0.100(4) Uani 1 1 d . . . C17 C 0.5464(12) 0.1452(12) 0.6659(9) 0.128(5) Uani 1 1 d . . . H17 H 0.5530 0.0951 0.6982 0.153 Uiso 1 1 calc R . . C18 C 0.4529(11) 0.2048(13) 0.6715(9) 0.129(6) Uani 1 1 d . . . H18 H 0.3970 0.1903 0.7093 0.155 Uiso 1 1 calc R . . C19 C 0.4372(11) 0.2838(10) 0.6249(8) 0.111(4) Uani 1 1 d . . . H19 H 0.3745 0.3185 0.6325 0.134 Uiso 1 1 calc R . . C20 C 0.5229(7) 0.3066(8) 0.5661(6) 0.074(3) Uani 1 1 d . . . C21 C 0.5063(12) 0.3777(7) 0.5164(6) 0.086(3) Uani 1 1 d . . . H21 H 0.4420 0.4110 0.5212 0.104 Uiso 1 1 calc R . . C22 C 0.5863(10) 0.3983(8) 0.4599(8) 0.097(4) Uani 1 1 d . . . H22 H 0.5783 0.4481 0.4274 0.116 Uiso 1 1 calc R . . C23 C 0.6794(10) 0.3466(8) 0.4497(6) 0.083(3) Uani 1 1 d . . . H23 H 0.7315 0.3622 0.4094 0.100 Uiso 1 1 calc R . . C24 C 0.6982(8) 0.2737(7) 0.4963(6) 0.073(3) Uani 1 1 d . . . H24 H 0.7627 0.2410 0.4894 0.088 Uiso 1 1 calc R . . C25 C 0.6169(9) 0.2500(7) 0.5548(6) 0.070(3) Uani 1 1 d . . . O6 O 0.7275(7) 0.1254(6) 0.5912(5) 0.108(3) Uani 1 1 d . . . H6 H 0.7283 0.0826 0.6218 0.162 Uiso 1 1 calc R . . C1 C -0.3915(8) 0.1490(6) 0.3295(6) 0.055(2) Uani 1 1 d . . . C2 C -0.5761(7) 0.1965(7) 0.3581(5) 0.060(3) Uani 1 1 d . . . H2 H -0.5921 0.2491 0.3905 0.072 Uiso 1 1 calc R . . C3 C -0.5459(6) 0.1185(7) 0.4166(6) 0.060(3) Uani 1 1 d . . . H3 H -0.5513 0.1338 0.4759 0.072 Uiso 1 1 calc R . . C4 C -0.2968(7) -0.0823(6) 0.3377(5) 0.053(2) Uani 1 1 d . . . C5 C -0.3611(7) 0.0331(6) 0.4307(6) 0.064(3) Uani 1 1 d . . . H5A H -0.3798 0.0294 0.4895 0.076 Uiso 1 1 calc R . . H5B H -0.2838 0.0512 0.4263 0.076 Uiso 1 1 calc R . . C6 C -0.2665(7) -0.2161(7) 0.2527(6) 0.072(3) Uani 1 1 d . . . H6A H -0.2658 -0.2766 0.2701 0.086 Uiso 1 1 calc R . . H6B H -0.1898 -0.1962 0.2513 0.086 Uiso 1 1 calc R . . C7 C -0.4602(7) 0.2800(6) 0.2515(6) 0.066(3) Uani 1 1 d . . . H7A H -0.3821 0.2963 0.2514 0.080 Uiso 1 1 calc R . . H7B H -0.5028 0.3294 0.2717 0.080 Uiso 1 1 calc R . . C8 C -0.2740(7) -0.1512(6) 0.1120(6) 0.054(2) Uani 1 1 d . . . C9 C -0.6070(6) 0.2700(6) 0.1322(6) 0.052(2) Uani 1 1 d . . . H9 H -0.6318 0.3307 0.1353 0.063 Uiso 1 1 calc R . . C10 C -0.4026(6) -0.2382(6) 0.0416(6) 0.056(2) Uani 1 1 d . . . H10 H -0.3841 -0.2845 0.0019 0.067 Uiso 1 1 calc R . . C11 C -0.4221(8) 0.2269(6) 0.1059(6) 0.053(2) Uani 1 1 d . . . C12 C -0.3024(6) -0.1174(5) -0.0372(5) 0.051(2) Uani 1 1 d . . . H12A H -0.3086 -0.1551 -0.0856 0.061 Uiso 1 1 calc R . . H12B H -0.2268 -0.0952 -0.0352 0.061 Uiso 1 1 calc R . . C13 C -0.4271(7) 0.1873(6) -0.0435(5) 0.054(2) Uani 1 1 d . . . H13A H -0.4636 0.2176 -0.0891 0.065 Uiso 1 1 calc R . . H13B H -0.3500 0.2063 -0.0422 0.065 Uiso 1 1 calc R . . C14 C -0.3460(7) 0.0406(7) -0.0324(6) 0.054(2) Uani 1 1 d . . . C15 C -0.4785(6) -0.0488(5) -0.0968(5) 0.046(2) Uani 1 1 d . . . H15 H -0.4621 -0.0692 -0.1536 0.056 Uiso 1 1 calc R . . N1 N -0.4763(5) 0.2075(5) 0.3070(4) 0.0560(19) Uani 1 1 d . . . N2 N -0.4307(6) 0.0967(5) 0.3914(5) 0.055(2) Uani 1 1 d . . . N3 N -0.3260(6) -0.1661(5) 0.3148(5) 0.059(2) Uani 1 1 d . . . N4 N -0.3741(6) -0.0514(6) 0.3927(5) 0.064(2) Uani 1 1 d . . . N5 N -0.3124(5) -0.2111(5) 0.1678(4) 0.0551(18) Uani 1 1 d . . . N6 N -0.3237(5) -0.1667(4) 0.0362(4) 0.0489(17) Uani 1 1 d . . . N7 N -0.4957(6) 0.2592(4) 0.1642(4) 0.0575(17) Uani 1 1 d . . . N8 N -0.4805(5) 0.2127(4) 0.0349(4) 0.0510(17) Uani 1 1 d . . . N9 N -0.3793(5) -0.0451(5) -0.0463(5) 0.0485(18) Uani 1 1 d . . . N10 N -0.4296(5) 0.0961(5) -0.0604(4) 0.0509(18) Uani 1 1 d . . . O1 O -0.2987(5) 0.1497(4) 0.3002(4) 0.0665(18) Uani 1 1 d . . . O2 O -0.2154(5) -0.0429(4) 0.3105(4) 0.0690(17) Uani 1 1 d . . . O3 O -0.2020(5) -0.0949(4) 0.1252(3) 0.0620(17) Uani 1 1 d . . . O4 O -0.2567(4) 0.0640(4) 0.0019(4) 0.0577(16) Uani 1 1 d . . . O5 O -0.3202(4) 0.2174(4) 0.1146(4) 0.0581(16) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1W 0.061(5) 0.161(11) 0.124(8) 0.000 0.000 -0.015(7) O2W 0.074(5) 0.095(6) 0.162(7) 0.042(5) -0.027(5) -0.009(5) O3W 0.118(9) 0.177(13) 0.143(10) 0.000 0.000 0.017(11) O4W 0.49(5) 0.24(3) 0.26(3) 0.000 0.000 0.14(3) K1 0.0666(13) 0.0655(15) 0.0806(14) 0.0011(12) 0.0023(12) -0.0023(11) I1 0.0770(12) 0.0559(11) 0.0556(11) 0.0008(6) 0.0002(5) 0.0061(7) I1' 0.185(8) 0.094(6) 0.168(10) -0.038(7) 0.053(9) -0.033(7) C16 0.078(8) 0.093(10) 0.129(11) -0.023(9) -0.033(8) -0.005(8) C17 0.092(9) 0.182(16) 0.109(10) 0.011(11) -0.005(8) -0.029(11) C18 0.065(8) 0.202(19) 0.120(12) 0.017(13) 0.012(8) -0.028(10) C19 0.093(9) 0.138(14) 0.103(10) -0.002(10) -0.021(8) -0.014(9) C20 0.043(6) 0.103(9) 0.076(6) -0.020(6) 0.001(5) -0.008(6) C21 0.099(8) 0.084(8) 0.076(6) 0.004(6) -0.006(9) -0.003(9) C22 0.095(9) 0.082(9) 0.114(10) -0.009(8) -0.003(8) 0.008(8) C23 0.105(9) 0.081(8) 0.064(6) 0.002(6) 0.006(6) -0.021(7) C24 0.071(6) 0.094(9) 0.055(5) -0.019(6) -0.005(5) -0.020(6) C25 0.076(7) 0.064(8) 0.069(7) -0.007(6) -0.024(6) -0.017(6) O6 0.111(6) 0.112(7) 0.102(5) 0.005(5) -0.019(5) 0.017(6) C1 0.052(5) 0.052(6) 0.062(6) -0.011(5) -0.011(5) 0.001(5) C2 0.055(6) 0.073(8) 0.053(6) -0.017(5) 0.000(4) -0.008(5) C3 0.037(4) 0.081(8) 0.063(6) -0.014(6) 0.005(4) -0.009(5) C4 0.045(5) 0.055(6) 0.059(5) 0.005(5) -0.013(5) 0.000(5) C5 0.054(5) 0.080(8) 0.058(6) -0.012(5) -0.007(4) -0.007(5) C6 0.047(5) 0.076(7) 0.092(7) 0.029(6) -0.001(5) 0.011(5) C7 0.057(5) 0.055(6) 0.087(7) -0.004(6) -0.004(5) -0.010(4) C8 0.046(5) 0.034(5) 0.080(6) 0.010(5) 0.004(5) 0.012(5) C9 0.041(5) 0.041(5) 0.076(6) 0.000(5) 0.007(4) 0.000(4) C10 0.041(5) 0.044(6) 0.083(7) -0.011(5) 0.006(4) 0.002(4) C11 0.064(6) 0.039(6) 0.057(6) -0.001(5) -0.001(5) -0.007(5) C12 0.038(4) 0.053(6) 0.061(5) 0.004(4) 0.012(4) 0.011(4) C13 0.051(5) 0.052(7) 0.059(6) 0.013(5) 0.000(4) 0.001(4) C14 0.042(5) 0.062(7) 0.058(6) -0.009(5) 0.012(4) 0.018(5) C15 0.035(5) 0.048(5) 0.055(4) 0.001(4) 0.008(4) -0.002(4) N1 0.054(5) 0.056(5) 0.057(4) -0.001(4) 0.001(4) -0.014(4) N2 0.048(4) 0.053(5) 0.064(5) -0.001(4) -0.004(4) -0.014(4) N3 0.048(4) 0.062(6) 0.066(5) 0.009(4) 0.007(4) 0.007(4) N4 0.042(4) 0.069(6) 0.079(6) -0.003(5) 0.007(4) -0.014(4) N5 0.048(4) 0.058(5) 0.059(4) 0.017(4) -0.007(4) 0.004(4) N6 0.041(4) 0.052(5) 0.054(4) -0.004(4) -0.003(3) 0.007(3) N7 0.050(4) 0.051(4) 0.071(4) -0.012(3) 0.009(5) -0.007(4) N8 0.043(4) 0.047(4) 0.063(4) -0.003(3) 0.006(4) 0.009(3) N9 0.034(4) 0.043(5) 0.068(5) 0.000(4) 0.001(3) 0.010(4) N10 0.049(4) 0.042(5) 0.062(5) 0.005(4) 0.004(3) 0.003(4) O1 0.038(3) 0.092(5) 0.069(4) -0.008(3) 0.000(3) -0.012(3) O2 0.042(3) 0.082(4) 0.083(4) 0.002(3) 0.006(3) -0.012(3) O3 0.045(3) 0.066(4) 0.075(4) 0.021(3) -0.005(3) -0.006(3) O4 0.031(3) 0.061(4) 0.081(4) 0.007(3) -0.005(3) 0.000(3) O5 0.037(3) 0.068(4) 0.069(4) 0.003(3) -0.001(3) -0.012(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 O1W K1 2.944(6) . ? O1W K1 2.944(6) 2 ? O2W K1 2.711(9) . ? K1 O1 2.717(7) . ? K1 O3 2.717(7) . ? K1 O4 2.788(7) . ? K1 O5 2.807(7) . ? K1 O2 2.927(7) . ? C16 O6 1.405(13) . ? C16 C25 1.438(16) . ? C16 C17 1.455(18) . ? C17 C18 1.45(2) . ? C18 C19 1.436(19) . ? C19 C20 1.437(15) . ? C20 C21 1.365(14) . ? C20 C25 1.437(14) . ? C21 C22 1.356(15) . ? C22 C23 1.380(14) . ? C23 C24 1.363(14) . ? C24 C25 1.400(13) . ? C1 O1 1.209(10) . ? C1 N2 1.359(11) . ? C1 N1 1.405(11) . ? C2 N3 1.442(11) 2_455 ? C2 N1 1.459(10) . ? C2 C3 1.564(13) . ? C3 N4 1.460(11) 2_455 ? C3 N2 1.478(10) . ? C4 O2 1.229(10) . ? C4 N4 1.363(10) . ? C4 N3 1.384(11) . ? C5 N2 1.431(11) . ? C5 N4 1.442(11) . ? C6 N3 1.444(11) . ? C6 N5 1.469(10) . ? C7 N1 1.439(11) . ? C7 N7 1.494(10) . ? C8 O3 1.241(9) . ? C8 N5 1.363(10) . ? C8 N6 1.372(10) . ? C9 N7 1.440(11) . ? C9 N5 1.441(10) 2_455 ? C9 C10 1.535(13) 2_455 ? C10 N6 1.452(10) . ? C10 N8 1.461(10) 2_455 ? C10 C9 1.535(13) 2_455 ? C11 O5 1.239(10) . ? C11 N8 1.353(11) . ? C11 N7 1.377(11) . ? C12 N6 1.421(10) . ? C12 N9 1.451(10) . ? C13 N10 1.427(10) . ? C13 N8 1.461(10) . ? C14 O4 1.257(10) . ? C14 N10 1.390(10) . ? C14 N9 1.394(11) . ? C15 N9 1.441(10) . ? C15 N10 1.444(9) 2_455 ? C15 C15 1.586(16) 2_455 ? N3 C2 1.442(11) 2_455 ? N4 C3 1.460(11) 2_455 ? N5 C9 1.441(10) 2_455 ? N8 C10 1.461(10) 2_455 ? N10 C15 1.444(9) 2_455 ? 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 K1 O1W K1 121.7(4) . 2 ? O2W K1 O1 140.4(2) . . ? O2W K1 O3 92.4(2) . . ? O1 K1 O3 125.34(19) . . ? O2W K1 O4 69.5(2) . . ? O1 K1 O4 129.36(19) . . ? O3 K1 O4 71.18(18) . . ? O2W K1 O5 96.6(2) . . ? O1 K1 O5 69.69(19) . . ? O3 K1 O5 129.94(19) . . ? O4 K1 O5 66.42(18) . . ? O2W K1 O2 130.6(2) . . ? O1 K1 O2 67.20(19) . . ? O3 K1 O2 65.92(18) . . ? O4 K1 O2 132.28(19) . . ? O5 K1 O2 131.83(18) . . ? O2W K1 O1W 75.9(2) . . ? O1 K1 O1W 99.1(2) . . ? O3 K1 O1W 77.32(15) . . ? O4 K1 O1W 131.3(2) . . ? O5 K1 O1W 152.46(15) . . ? O2 K1 O1W 56.84(17) . . ? O6 C16 C25 115.2(12) . . ? O6 C16 C17 121.8(14) . . ? C25 C16 C17 123.0(13) . . ? C18 C17 C16 112.6(15) . . ? C19 C18 C17 127.1(13) . . ? C18 C19 C20 116.9(13) . . ? C21 C20 C25 121.7(11) . . ? C21 C20 C19 118.2(12) . . ? C25 C20 C19 119.8(12) . . ? C22 C21 C20 118.2(13) . . ? C21 C22 C23 121.1(12) . . ? C24 C23 C22 122.8(11) . . ? C23 C24 C25 117.7(11) . . ? C24 C25 C20 118.2(10) . . ? C24 C25 C16 121.1(11) . . ? C20 C25 C16 120.6(11) . . ? O1 C1 N2 127.4(9) . . ? O1 C1 N1 124.2(9) . . ? N2 C1 N1 108.3(8) . . ? N3 C2 N1 115.9(7) 2_455 . ? N3 C2 C3 103.2(8) 2_455 . ? N1 C2 C3 103.5(7) . . ? N4 C3 N2 112.6(8) 2_455 . ? N4 C3 C2 103.4(7) 2_455 . ? N2 C3 C2 103.1(8) . . ? O2 C4 N4 126.7(9) . . ? O2 C4 N3 124.4(8) . . ? N4 C4 N3 108.8(8) . . ? N2 C5 N4 111.5(7) . . ? N3 C6 N5 115.1(7) . . ? N1 C7 N7 111.9(7) . . ? O3 C8 N5 126.6(8) . . ? O3 C8 N6 125.0(8) . . ? N5 C8 N6 108.3(8) . . ? N7 C9 N5 114.2(7) . 2_455 ? N7 C9 C10 103.3(7) . 2_455 ? N5 C9 C10 102.9(7) 2_455 2_455 ? N6 C10 N8 114.8(7) . 2_455 ? N6 C10 C9 104.4(7) . 2_455 ? N8 C10 C9 103.1(7) 2_455 2_455 ? O5 C11 N8 125.9(9) . . ? O5 C11 N7 126.8(8) . . ? N8 C11 N7 107.2(8) . . ? N6 C12 N9 112.1(6) . . ? N10 C13 N8 114.5(7) . . ? O4 C14 N10 125.5(9) . . ? O4 C14 N9 125.7(8) . . ? N10 C14 N9 108.8(8) . . ? N9 C15 N10 115.1(7) . 2_455 ? N9 C15 C15 103.4(7) . 2_455 ? N10 C15 C15 103.2(6) 2_455 2_455 ? C1 N1 C7 123.9(7) . . ? C1 N1 C2 112.1(8) . . ? C7 N1 C2 123.1(7) . . ? C1 N2 C5 121.4(7) . . ? C1 N2 C3 112.9(8) . . ? C5 N2 C3 125.5(8) . . ? C4 N3 C2 112.3(8) . 2_455 ? C4 N3 C6 123.5(8) . . ? C2 N3 C6 124.1(8) 2_455 . ? C4 N4 C5 120.7(7) . . ? C4 N4 C3 111.8(8) . 2_455 ? C5 N4 C3 126.6(8) . 2_455 ? C8 N5 C9 113.1(7) . 2_455 ? C8 N5 C6 120.9(7) . . ? C9 N5 C6 125.8(7) 2_455 . ? C8 N6 C12 124.1(7) . . ? C8 N6 C10 111.2(7) . . ? C12 N6 C10 124.7(7) . . ? C11 N7 C9 113.3(7) . . ? C11 N7 C7 121.9(7) . . ? C9 N7 C7 124.9(7) . . ? C11 N8 C10 113.1(8) . 2_455 ? C11 N8 C13 122.5(7) . . ? C10 N8 C13 123.8(7) 2_455 . ? C14 N9 C15 111.3(7) . . ? C14 N9 C12 121.7(7) . . ? C15 N9 C12 123.5(7) . . ? C14 N10 C13 121.8(8) . . ? C14 N10 C15 111.8(7) . 2_455 ? C13 N10 C15 125.9(7) . 2_455 ? C1 O1 K1 137.3(6) . . ? C4 O2 K1 131.4(5) . . ? C8 O3 K1 138.7(5) . . ? C14 O4 K1 132.7(5) . . ? C11 O5 K1 132.1(5) . . ? _diffrn_measured_fraction_theta_max 0.943 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.943 _refine_diff_density_max 0.509 _refine_diff_density_min -0.395 _refine_diff_density_rms 0.086 data_C _database_code_depnum_ccdc_archive 'CCDC 742108' #TrackingRef 'web_deposit_cif_file_2_Xin-longNi_1352613104.C.submit.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H56 N22 O23 Tl2' _chemical_formula_weight 1741.91 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' Tl Tl -2.8358 9.6688 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z' _cell_length_a 15.839(7) _cell_length_b 12.035(5) _cell_length_c 15.133(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2885(2) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.005 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1712 _exptl_absorpt_coefficient_mu 5.684 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17503 _diffrn_reflns_av_R_equivalents 0.0446 _diffrn_reflns_av_sigmaI/netI 0.0608 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5303 _reflns_number_gt 4738 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0445P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.005(8) _refine_ls_number_reflns 5303 _refine_ls_number_parameters 443 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0437 _refine_ls_R_factor_gt 0.0366 _refine_ls_wR_factor_ref 0.0910 _refine_ls_wR_factor_gt 0.0882 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1W O 0.3941(3) 0.4900(4) 0.5350(4) 0.0399(14) Uani 1 1 d . . . H1WA H 0.4254 0.4974 0.4811 0.048 Uiso 1 1 d R . . H1WB H 0.4146 0.5430 0.5591 0.048 Uiso 1 1 d R . . O2W O 0.0000 0.0000 0.2468(6) 0.049(2) Uani 1 2 d S . . H2W H -0.0326 -0.0138 0.2028 0.059 Uiso 1 1 d R . . O3W O 0.5000 0.5000 0.3828(6) 0.086(4) Uani 1 2 d S . . H3WA H 0.5108 0.5611 0.3444 0.103 Uiso 1 1 d R . . O4W O -0.0089(17) 0.4682(16) 0.3404(11) 0.103(6) Uani 0.50 1 d P . . C1 C 0.0805(4) 0.2942(5) 0.1598(4) 0.0224(13) Uani 1 1 d . . . C2 C 0.1145(4) 0.4527(6) 0.0781(4) 0.0222(15) Uani 1 1 d . . . H2 H 0.1291 0.4470 0.0153 0.027 Uiso 1 1 calc R . . C3 C 0.1912(4) 0.4230(5) 0.1376(4) 0.0184(15) Uani 1 1 d . . . H3 H 0.2421 0.4075 0.1029 0.022 Uiso 1 1 calc R . . C4 C 0.1487(4) 0.6065(5) 0.1673(4) 0.0210(14) Uani 1 1 d . . . C5 C 0.2079(4) 0.2643(5) 0.2495(5) 0.0247(16) Uani 1 1 d . . . H5A H 0.2667 0.2637 0.2318 0.030 Uiso 1 1 calc R . . H5B H 0.1886 0.1878 0.2508 0.030 Uiso 1 1 calc R . . C6 C 0.2701(4) 0.5382(6) 0.2545(4) 0.0232(15) Uani 1 1 d . . . H6A H 0.3190 0.4972 0.2338 0.028 Uiso 1 1 calc R . . H6B H 0.2849 0.6164 0.2552 0.028 Uiso 1 1 calc R . . C7 C 0.1449(4) 0.2693(5) 0.3992(5) 0.0211(15) Uani 1 1 d . . . C8 C 0.2597(4) 0.3904(5) 0.3768(4) 0.0211(15) Uani 1 1 d . . . H8 H 0.3184 0.3649 0.3741 0.025 Uiso 1 1 calc R . . C9 C 0.2279(4) 0.4002(5) 0.4735(5) 0.0201(14) Uani 1 1 d . . . H9 H 0.2723 0.3804 0.5157 0.024 Uiso 1 1 calc R . . C10 C 0.2236(4) 0.5760(5) 0.4064(4) 0.0188(14) Uani 1 1 d . . . C11 C 0.1088(4) 0.3004(6) 0.5542(4) 0.0207(15) Uani 1 1 d . . . H11A H 0.1455 0.3028 0.6055 0.025 Uiso 1 1 calc R . . H11B H 0.0856 0.2260 0.5503 0.025 Uiso 1 1 calc R . . C12 C 0.1837(4) 0.5684(6) 0.5661(5) 0.0252(16) Uani 1 1 d . . . H12A H 0.2044 0.6442 0.5649 0.030 Uiso 1 1 calc R . . H12B H 0.2130 0.5296 0.6133 0.030 Uiso 1 1 calc R . . C13 C -0.0424(4) 0.3470(5) 0.5545(4) 0.0181(14) Uani 1 1 d . . . C14 C 0.0452(4) 0.4782(5) 0.6222(4) 0.0191(14) Uani 1 1 d . . . H14 H 0.0640 0.4602 0.6822 0.023 Uiso 1 1 calc R . . C15 C -0.0326(4) 0.3629(6) 0.0622(5) 0.0248(15) Uani 1 1 d . . . H15A H -0.0286 0.3818 0.0001 0.030 Uiso 1 1 calc R . . H15B H -0.0506 0.2860 0.0662 0.030 Uiso 1 1 calc R . . C16 C 0.3063(5) 0.1265(8) 0.1003(5) 0.0377(19) Uani 1 1 d . . . C17 C 0.3279(5) 0.0474(8) 0.1601(6) 0.046(2) Uani 1 1 d . . . H17 H 0.3769 0.0549 0.1933 0.056 Uiso 1 1 calc R . . C18 C 0.2756(7) -0.0457(8) 0.1715(6) 0.054(3) Uani 1 1 d . . . H18 H 0.2902 -0.0991 0.2133 0.064 Uiso 1 1 calc R . . C19 C 0.2010(7) -0.0603(7) 0.1207(6) 0.051(2) Uani 1 1 d . . . H19 H 0.1657 -0.1211 0.1295 0.062 Uiso 1 1 calc R . . C20 C 0.1823(5) 0.0216(7) 0.0559(5) 0.0316(17) Uani 1 1 d . . . C21 C 0.2348(4) 0.1173(6) 0.0459(5) 0.0282(16) Uani 1 1 d . . . C22 C 0.2137(5) 0.1956(7) -0.0172(5) 0.0347(18) Uani 1 1 d . . . H22 H 0.2468 0.2588 -0.0238 0.042 Uiso 1 1 calc R . . C23 C 0.1445(5) 0.1807(8) -0.0699(5) 0.0379(18) Uani 1 1 d . . . H23 H 0.1316 0.2337 -0.1126 0.046 Uiso 1 1 calc R . . C24 C 0.0938(5) 0.0892(7) -0.0609(5) 0.042(2) Uani 1 1 d . . . H24 H 0.0465 0.0813 -0.0968 0.051 Uiso 1 1 calc R . . C25 C 0.1125(5) 0.0086(7) 0.0009(5) 0.040(2) Uani 1 1 d . . . H25 H 0.0786 -0.0542 0.0059 0.048 Uiso 1 1 calc R . . N1 N 0.0513(3) 0.3728(5) 0.1020(4) 0.0211(13) Uani 1 1 d . . . N2 N 0.1602(3) 0.3235(5) 0.1842(3) 0.0211(12) Uani 1 1 d . . . N3 N 0.0963(3) 0.5674(4) 0.1030(4) 0.0211(13) Uani 1 1 d . . . N4 N 0.2009(3) 0.5213(4) 0.1931(3) 0.0196(12) Uani 1 1 d . . . N5 N 0.2019(3) 0.3101(4) 0.3379(4) 0.0213(11) Uani 1 1 d . . . N6 N 0.1587(3) 0.3215(5) 0.4763(3) 0.0214(11) Uani 1 1 d . . . N7 N 0.2506(3) 0.5032(4) 0.3440(4) 0.0192(11) Uani 1 1 d . . . N8 N 0.2034(3) 0.5153(5) 0.4827(4) 0.0186(12) Uani 1 1 d . . . N9 N 0.0400(3) 0.3784(4) 0.5674(3) 0.0166(12) Uani 1 1 d . . . N10 N 0.0937(3) 0.5696(4) 0.5855(3) 0.0209(13) Uani 1 1 d . . . N11 N 0.4967(5) 0.2790(7) 0.2439(5) 0.0440(18) Uani 1 1 d . . . O1 O 0.0428(3) 0.2126(4) 0.1852(3) 0.0256(11) Uani 1 1 d . . . O2 O 0.0933(3) 0.1976(4) 0.3842(3) 0.0241(10) Uani 1 1 d . . . O3 O -0.0654(3) 0.2602(3) 0.5204(3) 0.0224(10) Uani 1 1 d . . . O4 O 0.1492(3) 0.7002(4) 0.1973(3) 0.0229(10) Uani 1 1 d . . . O5 O 0.2186(2) 0.6765(4) 0.3998(3) 0.0232(10) Uani 1 1 d . . . O6 O 0.5557(4) 0.3146(7) 0.2837(4) 0.0626(18) Uani 1 1 d . . . O7 O 0.5005(6) 0.1844(8) 0.2064(5) 0.088(2) Uani 1 1 d . . . O8 O 0.4298(4) 0.3275(7) 0.2375(5) 0.086(2) Uani 1 1 d . . . O9 O 0.3520(4) 0.2231(5) 0.0891(4) 0.0502(16) Uani 1 1 d . . . H9A H 0.3919 0.2236 0.1236 0.075 Uiso 1 1 calc R . . Tl1 Tl -0.077980(18) 0.18183(3) 0.34229(2) 0.03712(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1W 0.030(3) 0.020(3) 0.070(4) -0.015(3) -0.010(3) -0.002(2) O2W 0.076(6) 0.019(4) 0.054(6) 0.000 0.000 -0.002(4) O3W 0.158(12) 0.065(7) 0.034(5) 0.000 0.000 0.014(7) O4W 0.109(15) 0.091(19) 0.110(11) 0.006(12) -0.027(14) -0.046(14) C1 0.026(3) 0.016(3) 0.024(3) -0.007(3) 0.009(4) 0.004(3) C2 0.022(3) 0.023(4) 0.021(4) 0.004(3) 0.004(3) -0.002(3) C3 0.021(3) 0.017(3) 0.018(4) -0.001(3) 0.006(3) -0.006(3) C4 0.026(3) 0.023(4) 0.014(3) 0.010(3) 0.007(3) -0.006(3) C5 0.028(4) 0.011(3) 0.036(4) -0.001(3) 0.013(3) 0.007(3) C6 0.012(3) 0.027(4) 0.030(4) -0.002(3) 0.002(3) -0.006(3) C7 0.018(3) 0.013(3) 0.032(4) 0.003(3) 0.001(3) 0.005(3) C8 0.019(3) 0.015(3) 0.030(4) 0.000(3) -0.002(3) 0.003(3) C9 0.012(3) 0.020(3) 0.028(4) 0.004(3) -0.006(3) 0.001(3) C10 0.009(3) 0.022(4) 0.025(4) 0.003(3) -0.003(3) 0.002(3) C11 0.030(3) 0.014(4) 0.018(3) 0.008(3) -0.005(2) 0.001(3) C12 0.019(3) 0.028(4) 0.029(4) -0.009(3) -0.006(3) -0.004(3) C13 0.022(3) 0.018(4) 0.015(3) 0.011(3) 0.004(2) 0.001(3) C14 0.031(4) 0.020(4) 0.006(3) 0.001(3) -0.007(2) -0.009(3) C15 0.037(4) 0.015(3) 0.023(4) -0.007(3) -0.001(3) -0.002(3) C16 0.039(5) 0.043(5) 0.031(4) -0.009(4) 0.010(4) 0.007(4) C17 0.056(5) 0.052(5) 0.030(4) -0.002(5) 0.008(4) 0.009(4) C18 0.088(7) 0.041(5) 0.032(5) 0.000(4) -0.005(5) 0.035(5) C19 0.081(7) 0.025(5) 0.048(6) 0.000(4) 0.001(5) 0.005(5) C20 0.040(4) 0.036(5) 0.019(4) 0.003(3) 0.007(3) 0.008(3) C21 0.032(4) 0.023(4) 0.030(4) -0.008(3) 0.012(3) 0.006(3) C22 0.047(4) 0.030(4) 0.027(4) -0.003(4) 0.018(3) 0.001(4) C23 0.047(4) 0.038(4) 0.029(4) 0.005(4) 0.004(3) 0.001(5) C24 0.044(5) 0.048(5) 0.035(4) 0.000(4) -0.004(4) -0.005(4) C25 0.042(4) 0.035(5) 0.043(5) 0.000(4) 0.001(4) -0.008(4) N1 0.022(3) 0.019(3) 0.022(3) 0.003(3) 0.004(2) -0.005(2) N2 0.021(3) 0.018(3) 0.024(3) -0.001(3) 0.007(2) 0.004(3) N3 0.024(3) 0.017(3) 0.022(3) 0.000(2) 0.001(2) -0.003(2) N4 0.024(3) 0.011(3) 0.023(3) 0.000(2) 0.005(2) 0.001(2) N5 0.022(2) 0.018(3) 0.024(3) 0.002(3) 0.007(2) -0.001(2) N6 0.022(3) 0.020(3) 0.021(3) 0.006(3) -0.001(2) 0.000(3) N7 0.022(3) 0.017(3) 0.019(3) 0.002(3) -0.001(2) -0.002(2) N8 0.019(3) 0.017(3) 0.020(3) 0.004(3) -0.002(2) -0.002(2) N9 0.022(3) 0.012(3) 0.016(3) 0.002(2) -0.008(2) -0.001(2) N10 0.030(3) 0.015(3) 0.018(3) -0.005(2) -0.005(2) -0.006(2) N11 0.054(5) 0.044(5) 0.034(4) 0.011(4) 0.014(4) -0.003(4) O1 0.029(2) 0.015(3) 0.033(3) 0.0008(19) 0.0026(19) -0.0045(19) O2 0.032(3) 0.013(2) 0.028(2) -0.0015(19) 0.0030(19) -0.004(2) O3 0.025(2) 0.012(2) 0.030(3) -0.001(2) -0.001(2) -0.0040(19) O4 0.032(3) 0.014(3) 0.022(2) 0.003(2) 0.0010(19) 0.001(2) O5 0.019(2) 0.013(2) 0.038(3) -0.001(2) -0.0025(18) -0.007(2) O6 0.053(4) 0.094(5) 0.041(4) 0.010(4) -0.014(3) -0.013(4) O7 0.101(6) 0.089(7) 0.076(5) 0.000(5) 0.009(5) -0.031(6) O8 0.037(4) 0.115(7) 0.104(6) 0.023(5) -0.005(4) 0.010(5) O9 0.046(3) 0.071(5) 0.034(3) -0.007(3) 0.006(3) -0.012(3) Tl1 0.03431(15) 0.03573(16) 0.04132(17) 0.00118(16) 0.00105(14) 0.00264(15) _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 O4W O4W 0.82(3) 2_565 ? C1 O1 1.212(7) . ? C1 N2 1.361(8) . ? C1 N1 1.370(8) . ? C2 N1 1.435(8) . ? C2 N3 1.460(9) . ? C2 C3 1.554(9) . ? C3 N4 1.459(8) . ? C3 N2 1.475(8) . ? C4 O4 1.215(8) . ? C4 N3 1.364(9) . ? C4 N4 1.374(8) . ? C5 N2 1.433(9) . ? C5 N5 1.451(9) . ? C6 N7 1.452(8) . ? C6 N4 1.452(8) . ? C7 O2 1.210(8) . ? C7 N6 1.343(9) . ? C7 N5 1.383(8) . ? C8 N7 1.453(8) . ? C8 N5 1.456(8) . ? C8 C9 1.551(9) . ? C9 N8 1.444(8) . ? C9 N6 1.449(8) . ? C10 O5 1.216(8) . ? C10 N7 1.357(8) . ? C10 N8 1.403(8) . ? C11 N6 1.443(8) . ? C11 N9 1.451(8) . ? C12 N8 1.450(8) . ? C12 N10 1.456(8) . ? C13 O3 1.220(8) . ? C13 N9 1.373(8) . ? C13 N10 1.374(8) 2_565 ? C14 N10 1.452(8) . ? C14 N9 1.463(8) . ? C14 C14 1.525(13) 2_565 ? C15 N3 1.450(8) 2_565 ? C15 N1 1.463(8) . ? C16 C17 1.356(12) . ? C16 O9 1.380(11) . ? C16 C21 1.404(11) . ? C17 C18 1.405(13) . ? C18 C19 1.421(14) . ? C19 C20 1.422(11) . ? C20 C25 1.393(11) . ? C20 C21 1.428(11) . ? C21 C22 1.382(10) . ? C22 C23 1.367(11) . ? C23 C24 1.370(11) . ? C24 C25 1.380(11) . ? N3 C15 1.450(8) 2_565 ? N10 C13 1.374(8) 2_565 ? N11 O6 1.190(9) . ? N11 O8 1.214(9) . ? N11 O7 1.274(11) . ? O2 Tl1 2.793(5) . ? 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 C1 N2 125.5(6) . . ? O1 C1 N1 126.5(6) . . ? N2 C1 N1 107.9(5) . . ? N1 C2 N3 115.5(5) . . ? N1 C2 C3 104.3(5) . . ? N3 C2 C3 102.9(5) . . ? N4 C3 N2 114.7(5) . . ? N4 C3 C2 103.3(5) . . ? N2 C3 C2 101.7(5) . . ? O4 C4 N3 126.2(6) . . ? O4 C4 N4 125.6(6) . . ? N3 C4 N4 108.2(6) . . ? N2 C5 N5 114.3(5) . . ? N7 C6 N4 113.3(5) . . ? O2 C7 N6 127.3(6) . . ? O2 C7 N5 124.6(6) . . ? N6 C7 N5 108.1(6) . . ? N7 C8 N5 114.8(5) . . ? N7 C8 C9 102.6(5) . . ? N5 C8 C9 103.2(5) . . ? N8 C9 N6 114.9(5) . . ? N8 C9 C8 104.6(5) . . ? N6 C9 C8 102.9(5) . . ? O5 C10 N7 127.2(6) . . ? O5 C10 N8 124.8(6) . . ? N7 C10 N8 108.0(5) . . ? N6 C11 N9 114.2(5) . . ? N8 C12 N10 113.0(5) . . ? O3 C13 N9 125.4(6) . . ? O3 C13 N10 126.4(6) . 2_565 ? N9 C13 N10 108.2(6) . 2_565 ? N10 C14 N9 115.8(5) . . ? N10 C14 C14 103.7(6) . 2_565 ? N9 C14 C14 103.3(5) . 2_565 ? N3 C15 N1 114.2(5) 2_565 . ? C17 C16 O9 122.7(8) . . ? C17 C16 C21 122.6(8) . . ? O9 C16 C21 114.7(8) . . ? C16 C17 C18 119.6(9) . . ? C17 C18 C19 121.5(9) . . ? C18 C19 C20 117.4(9) . . ? C25 C20 C19 120.0(8) . . ? C25 C20 C21 119.3(7) . . ? C19 C20 C21 120.8(7) . . ? C22 C21 C16 123.1(7) . . ? C22 C21 C20 118.8(7) . . ? C16 C21 C20 118.1(7) . . ? C23 C22 C21 120.5(8) . . ? C22 C23 C24 121.1(8) . . ? C23 C24 C25 120.5(8) . . ? C24 C25 C20 119.8(8) . . ? C1 N1 C2 112.8(5) . . ? C1 N1 C15 120.9(5) . . ? C2 N1 C15 125.9(6) . . ? C1 N2 C5 123.1(6) . . ? C1 N2 C3 113.0(5) . . ? C5 N2 C3 123.9(5) . . ? C4 N3 C15 121.8(5) . 2_565 ? C4 N3 C2 112.9(5) . . ? C15 N3 C2 125.2(5) 2_565 . ? C4 N4 C6 122.1(6) . . ? C4 N4 C3 112.2(5) . . ? C6 N4 C3 124.2(5) . . ? C7 N5 C5 121.8(5) . . ? C7 N5 C8 112.0(5) . . ? C5 N5 C8 125.7(5) . . ? C7 N6 C11 122.6(6) . . ? C7 N6 C9 113.8(5) . . ? C11 N6 C9 123.6(6) . . ? C10 N7 C6 121.9(5) . . ? C10 N7 C8 113.4(5) . . ? C6 N7 C8 124.7(5) . . ? C10 N8 C9 111.0(5) . . ? C10 N8 C12 122.4(5) . . ? C9 N8 C12 124.4(5) . . ? C13 N9 C11 121.1(5) . . ? C13 N9 C14 111.1(5) . . ? C11 N9 C14 124.5(5) . . ? C13 N10 C14 111.8(5) 2_565 . ? C13 N10 C12 121.2(6) 2_565 . ? C14 N10 C12 126.0(5) . . ? O6 N11 O8 123.5(9) . . ? O6 N11 O7 120.7(9) . . ? O8 N11 O7 115.8(9) . . ? C7 O2 Tl1 138.3(4) . . ? _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 1.220 _refine_diff_density_min -0.591 _refine_diff_density_rms 0.127 data_B _database_code_depnum_ccdc_archive 'CCDC 742109' #TrackingRef 'web_deposit_cif_file_1_Xin-longNi_1352613104.B.submit.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H64 I2 K2 N20 O24' _chemical_formula_weight 1541.11 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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 11.9430(6) _cell_length_b 15.8512(8) _cell_length_c 30.5821(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5789.5(5) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.768 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3120 _exptl_absorpt_coefficient_mu 1.329 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 50878 _diffrn_reflns_av_R_equivalents 0.0417 _diffrn_reflns_av_sigmaI/netI 0.0386 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 26.00 _reflns_number_total 11225 _reflns_number_gt 9544 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0589P)^2^+2.7094P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.029(14) _refine_ls_number_reflns 11225 _refine_ls_number_parameters 812 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0522 _refine_ls_R_factor_gt 0.0410 _refine_ls_wR_factor_ref 0.1088 _refine_ls_wR_factor_gt 0.1035 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _refine_ls_shift/su_max 0.004 _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 O1W O -0.2409(3) 0.5796(2) 0.73686(12) 0.0422(8) Uani 1 1 d . . . O2W O 0.7336(3) 0.3781(2) 0.72319(15) 0.0563(11) Uani 1 1 d . . . O3W O -0.2548(3) 0.5147(4) 0.62158(17) 0.0841(17) Uani 1 1 d . . . O4W O -0.1825(7) 0.6995(4) 0.64455(16) 0.127(3) Uani 1 1 d . . . O5W O -0.2475(3) 0.4699(4) 0.81076(16) 0.0759(15) Uani 1 1 d . . . O6W O 0.2433(5) 0.5225(5) 0.43922(18) 0.116(3) Uani 1 1 d . . . O7W O 0.2592(11) 0.4826(6) 0.6731(3) 0.229(7) Uani 1 1 d . . . O8W O 0.042(2) 0.8290(8) 0.5262(5) 0.323(12) Uani 1 1 d . A 1 O12W O -0.0770(19) 0.750(2) 0.5286(9) 0.55(3) Uani 1 1 d . B 2 O13W O 0.179(3) 0.8769(8) 0.5209(8) 0.52(2) Uani 1 1 d . C 3 O9W O 0.263(3) 0.7386(8) 0.4541(5) 0.415(19) Uani 1 1 d . . . O10W O 0.067(2) 0.7272(12) 0.4836(3) 0.322(12) Uani 1 1 d . D 1 O11W O -0.169(4) 0.6562(17) 0.5033(10) 0.57(3) Uani 1 1 d . E 2 K1 K 0.55889(10) 0.41462(7) 0.66820(4) 0.0410(3) Uani 1 1 d . . . K2 K -0.06333(9) 0.55764(7) 0.68146(4) 0.0408(3) Uani 1 1 d . . . I1 I 0.9774(3) 0.5158(2) 0.89185(11) 0.0557(6) Uani 0.607(19) 1 d P F 1 I1' I 0.9599(6) 0.5216(3) 0.88964(15) 0.0617(10) Uani 0.393(19) 1 d P F 2 I2 I 0.5167(3) 0.4454(3) 0.88338(14) 0.0497(7) Uani 0.607(19) 1 d P F 1 I2' I 0.5167(5) 0.4558(5) 0.8808(2) 0.0534(11) Uani 0.393(19) 1 d P F 2 C1 C 0.4840(3) 0.6336(2) 0.69522(13) 0.0243(9) Uani 1 1 d . . . C2 C 0.3595(4) 0.7460(3) 0.68445(15) 0.0280(9) Uani 1 1 d . . . H2 H 0.3862 0.8040 0.6811 0.034 Uiso 1 1 calc R . . C3 C 0.3570(3) 0.7191(3) 0.73335(15) 0.0277(9) Uani 1 1 d . . . H3 H 0.3753 0.7663 0.7527 0.033 Uiso 1 1 calc R . . C4 C 0.1761(4) 0.7080(3) 0.70390(15) 0.0274(9) Uani 1 1 d . . . C5 C 0.4624(3) 0.6047(3) 0.77492(13) 0.0250(9) Uani 1 1 d . . . H5A H 0.5380 0.5826 0.7736 0.030 Uiso 1 1 calc R . . H5B H 0.4575 0.6416 0.8001 0.030 Uiso 1 1 calc R . . C6 C 0.1938(4) 0.6730(3) 0.78209(15) 0.0280(10) Uani 1 1 d . . . H6A H 0.1173 0.6935 0.7825 0.034 Uiso 1 1 calc R . . H6B H 0.2354 0.7041 0.8040 0.034 Uiso 1 1 calc R . . C7 C 0.4162(3) 0.4530(3) 0.77183(13) 0.0232(9) Uani 1 1 d . . . C8 C 0.2896(3) 0.5392(3) 0.81027(14) 0.0266(9) Uani 1 1 d . . . H8 H 0.3118 0.5595 0.8393 0.032 Uiso 1 1 calc R . . C9 C 0.2494(3) 0.4469(3) 0.81188(14) 0.0283(9) Uani 1 1 d . . . H9 H 0.2437 0.4263 0.8420 0.034 Uiso 1 1 calc R . . C10 C 0.1074(4) 0.5313(3) 0.78145(15) 0.0300(10) Uani 1 1 d . . . C11 C 0.3410(4) 0.3111(3) 0.78253(15) 0.0295(10) Uani 1 1 d . . . H11A H 0.3114 0.2848 0.8087 0.035 Uiso 1 1 calc R . . H11B H 0.4192 0.2952 0.7800 0.035 Uiso 1 1 calc R . . C12 C 0.0662(4) 0.3789(3) 0.78628(15) 0.0323(10) Uani 1 1 d . . . H12A H -0.0107 0.3986 0.7855 0.039 Uiso 1 1 calc R . . H12B H 0.0745 0.3430 0.8118 0.039 Uiso 1 1 calc R . . C13 C 0.3313(4) 0.2626(2) 0.70572(15) 0.0271(10) Uani 1 1 d . . . C14 C 0.1623(4) 0.2575(3) 0.74531(15) 0.0299(10) Uani 1 1 d . . . H14 H 0.1446 0.2158 0.7679 0.036 Uiso 1 1 calc R . . C15 C 0.1430(3) 0.2217(3) 0.69821(15) 0.0270(9) Uani 1 1 d . . . H15 H 0.1171 0.1630 0.6988 0.032 Uiso 1 1 calc R . . C16 C 0.0278(4) 0.3397(3) 0.71009(15) 0.0312(10) Uani 1 1 d . . . C17 C 0.2778(4) 0.2067(3) 0.63357(15) 0.0290(10) Uani 1 1 d . . . H17A H 0.2329 0.1581 0.6256 0.035 Uiso 1 1 calc R . . H17B H 0.3559 0.1902 0.6318 0.035 Uiso 1 1 calc R . . C18 C 0.0064(4) 0.2700(3) 0.63808(15) 0.0328(10) Uani 1 1 d . . . H18A H 0.0051 0.2108 0.6301 0.039 Uiso 1 1 calc R . . H18B H -0.0706 0.2889 0.6404 0.039 Uiso 1 1 calc R . . C19 C 0.3387(4) 0.3299(3) 0.58889(13) 0.0249(9) Uani 1 1 d . . . C20 C 0.1530(3) 0.2858(3) 0.57799(15) 0.0278(10) Uani 1 1 d . . . H20 H 0.1327 0.2349 0.5617 0.033 Uiso 1 1 calc R . . C21 C 0.1794(4) 0.3611(3) 0.54668(15) 0.0295(10) Uani 1 1 d . . . H21 H 0.1714 0.3446 0.5159 0.035 Uiso 1 1 calc R . . C22 C 0.0271(4) 0.3965(3) 0.59181(14) 0.0309(10) Uani 1 1 d . . . C23 C 0.3624(4) 0.4423(3) 0.53368(14) 0.0285(9) Uani 1 1 d . . . H23A H 0.3374 0.4442 0.5035 0.034 Uiso 1 1 calc R . . H23B H 0.4395 0.4230 0.5337 0.034 Uiso 1 1 calc R . . C24 C 0.0876(4) 0.5067(3) 0.53958(15) 0.0327(10) Uani 1 1 d . . . H24A H 0.1033 0.5027 0.5085 0.039 Uiso 1 1 calc R . . H24B H 0.0110 0.5259 0.5429 0.039 Uiso 1 1 calc R . . C25 C 0.4405(4) 0.5573(3) 0.57927(14) 0.0302(9) Uani 1 1 d . . . C26 C 0.2730(4) 0.5887(3) 0.54166(15) 0.0304(10) Uani 1 1 d . . . H26 H 0.2708 0.6018 0.5104 0.037 Uiso 1 1 calc R . . C27 C 0.3097(4) 0.6666(3) 0.56925(14) 0.0310(10) Uani 1 1 d . . . H27 H 0.3231 0.7160 0.5507 0.037 Uiso 1 1 calc R . . C28 C 0.1280(4) 0.6249(3) 0.59022(15) 0.0309(10) Uani 1 1 d . . . C29 C 0.4764(4) 0.6894(3) 0.62031(14) 0.0307(9) Uani 1 1 d . . . H29A H 0.5535 0.6704 0.6196 0.037 Uiso 1 1 calc R . . H29B H 0.4751 0.7476 0.6105 0.037 Uiso 1 1 calc R . . C30 C 0.2017(4) 0.7524(3) 0.62722(15) 0.0331(11) Uani 1 1 d . . . H30A H 0.2415 0.7999 0.6146 0.040 Uiso 1 1 calc R . . H30B H 0.1230 0.7674 0.6288 0.040 Uiso 1 1 calc R . . N1 N 0.4366(3) 0.6861(2) 0.66486(12) 0.0275(8) Uani 1 1 d . . . N2 N 0.4405(3) 0.6535(2) 0.73562(11) 0.0252(8) Uani 1 1 d . . . N3 N 0.2431(3) 0.7380(2) 0.67117(13) 0.0296(8) Uani 1 1 d . . . N4 N 0.2418(3) 0.6907(2) 0.73954(12) 0.0269(8) Uani 1 1 d . . . N5 N 0.3851(3) 0.5354(2) 0.78057(11) 0.0239(8) Uani 1 1 d . . . N6 N 0.3339(3) 0.4010(2) 0.78713(12) 0.0264(8) Uani 1 1 d . . . N7 N 0.1937(3) 0.5843(2) 0.79389(12) 0.0261(8) Uani 1 1 d . . . N8 N 0.1397(3) 0.4503(2) 0.79057(12) 0.0301(8) Uani 1 1 d . . . N9 N 0.2807(3) 0.2789(2) 0.74489(12) 0.0287(8) Uani 1 1 d . . . N10 N 0.2527(3) 0.2295(2) 0.67790(12) 0.0282(8) Uani 1 1 d . . . N11 N 0.0882(3) 0.3293(2) 0.74710(12) 0.0314(9) Uani 1 1 d . . . N12 N 0.0591(3) 0.2781(2) 0.68047(13) 0.0329(9) Uani 1 1 d . . . N13 N 0.2572(3) 0.2747(2) 0.60173(12) 0.0263(8) Uani 1 1 d . . . N14 N 0.2948(3) 0.3824(2) 0.55715(12) 0.0282(8) Uani 1 1 d . . . N15 N 0.0607(3) 0.3168(2) 0.60352(13) 0.0324(9) Uani 1 1 d . . . N16 N 0.0979(3) 0.4237(2) 0.55888(12) 0.0312(8) Uani 1 1 d . . . N17 N 0.3584(3) 0.5268(2) 0.55166(12) 0.0279(8) Uani 1 1 d . . . N18 N 0.4109(3) 0.6384(2) 0.59004(12) 0.0319(9) Uani 1 1 d . . . N19 N 0.1617(3) 0.5687(2) 0.55871(12) 0.0298(8) Uani 1 1 d . . . N20 N 0.2143(3) 0.6799(2) 0.59852(13) 0.0330(9) Uani 1 1 d . . . O1 O 0.5565(2) 0.58078(19) 0.68789(10) 0.0314(7) Uani 1 1 d . . . O2 O 0.5019(2) 0.43094(19) 0.75331(10) 0.0312(7) Uani 1 1 d . . . O3 O 0.4305(2) 0.27427(18) 0.69695(10) 0.0288(7) Uani 1 1 d . . . O4 O 0.4347(2) 0.33249(19) 0.60252(10) 0.0302(7) Uani 1 1 d . . . O5 O 0.5240(3) 0.51887(19) 0.59056(10) 0.0344(7) Uani 1 1 d . . . O6 O 0.0741(2) 0.6999(2) 0.70210(11) 0.0338(7) Uani 1 1 d . . . O7 O 0.0191(2) 0.55290(19) 0.76591(10) 0.0345(7) Uani 1 1 d . . . O8 O -0.0436(2) 0.3933(2) 0.70340(11) 0.0380(8) Uani 1 1 d . . . O9 O -0.0514(2) 0.4356(2) 0.60649(11) 0.0388(8) Uani 1 1 d . . . O10 O 0.0365(3) 0.6255(2) 0.60781(11) 0.0414(8) Uani 1 1 d . . . C31 C 0.6864(4) 0.2455(3) 0.58937(15) 0.0314(10) Uani 1 1 d . . . C32 C 0.7792(4) 0.1900(3) 0.58482(16) 0.0357(11) Uani 1 1 d . . . H32 H 0.7861 0.1440 0.6035 0.043 Uiso 1 1 calc R . . C33 C 0.8572(4) 0.2033(3) 0.55374(15) 0.0336(11) Uani 1 1 d . . . H33 H 0.9172 0.1661 0.5513 0.040 Uiso 1 1 calc R . . C34 C 0.8499(4) 0.2728(3) 0.52467(15) 0.0306(10) Uani 1 1 d . . . C35 C 0.9310(4) 0.2894(3) 0.49206(16) 0.0385(11) Uani 1 1 d . . . H35 H 0.9924 0.2537 0.4891 0.046 Uiso 1 1 calc R . . C36 C 0.9199(5) 0.3583(4) 0.46448(17) 0.0454(13) Uani 1 1 d . . . H36 H 0.9744 0.3694 0.4435 0.054 Uiso 1 1 calc R . . C37 C 0.8269(5) 0.4111(4) 0.46824(18) 0.0486(14) Uani 1 1 d . . . H37 H 0.8194 0.4566 0.4492 0.058 Uiso 1 1 calc R . . C38 C 0.7471(5) 0.3975(3) 0.49907(18) 0.0453(13) Uani 1 1 d . . . H38 H 0.6859 0.4336 0.5010 0.054 Uiso 1 1 calc R . . C39 C 0.7566(4) 0.3284(3) 0.52845(16) 0.0330(10) Uani 1 1 d . . . C40 C 0.6758(4) 0.3136(3) 0.56253(16) 0.0338(10) Uani 1 1 d . . . H40 H 0.6162 0.3507 0.5662 0.041 Uiso 1 1 calc R . . O11 O 0.6127(3) 0.2285(2) 0.62322(12) 0.0484(9) Uani 1 1 d . . . H11C H 0.5371 0.2278 0.6273 0.058 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1W 0.0262(16) 0.049(2) 0.051(2) -0.0046(17) -0.0024(15) -0.0003(15) O2W 0.037(2) 0.0353(19) 0.096(3) 0.006(2) 0.013(2) 0.0003(17) O3W 0.034(2) 0.139(5) 0.079(3) -0.049(3) -0.011(2) 0.023(2) O4W 0.204(7) 0.128(5) 0.051(3) -0.009(3) -0.002(4) 0.112(5) O5W 0.066(3) 0.099(4) 0.063(3) 0.019(3) -0.004(2) -0.010(3) O6W 0.126(5) 0.163(6) 0.060(3) -0.048(4) -0.037(3) 0.058(5) O7W 0.43(2) 0.155(8) 0.108(7) 0.019(6) -0.040(8) -0.082(11) O8W 0.57(3) 0.150(9) 0.244(14) -0.003(9) -0.263(19) -0.058(15) O12W 0.38(2) 0.77(5) 0.49(3) 0.58(4) -0.21(2) -0.23(3) O13W 1.00(6) 0.102(8) 0.47(3) 0.041(13) -0.55(4) -0.01(2) O9W 0.86(5) 0.117(8) 0.267(18) 0.097(10) -0.27(3) -0.042(18) O10W 0.51(2) 0.349(19) 0.107(7) -0.025(9) -0.121(11) 0.33(2) O11W 0.87(7) 0.32(3) 0.52(4) 0.28(3) -0.39(5) -0.11(4) K1 0.0503(6) 0.0344(5) 0.0384(6) -0.0061(4) 0.0065(5) 0.0011(5) K2 0.0345(5) 0.0371(5) 0.0510(6) -0.0072(5) 0.0072(5) 0.0047(5) I1 0.0375(11) 0.0585(13) 0.0711(14) -0.0199(9) 0.0078(7) -0.0052(6) I1' 0.099(3) 0.0321(11) 0.0541(14) 0.0009(9) -0.0251(17) 0.0142(14) I2 0.0535(10) 0.0476(10) 0.0480(14) -0.0158(9) -0.0102(8) 0.0159(9) I2' 0.074(2) 0.0553(19) 0.0313(13) 0.0013(11) -0.0206(11) -0.0103(15) C1 0.0181(19) 0.027(2) 0.028(2) -0.0030(16) 0.0017(18) -0.0099(19) C2 0.026(2) 0.022(2) 0.036(3) -0.0009(18) 0.0003(19) -0.0038(17) C3 0.025(2) 0.025(2) 0.033(3) -0.0047(18) 0.0005(19) -0.0017(17) C4 0.029(2) 0.020(2) 0.034(3) -0.0027(18) -0.001(2) 0.0020(18) C5 0.018(2) 0.030(2) 0.027(2) -0.0013(17) -0.0047(17) -0.0018(17) C6 0.027(2) 0.025(2) 0.032(2) -0.0071(19) 0.0076(19) 0.0040(18) C7 0.021(2) 0.028(2) 0.020(2) -0.0004(17) -0.0079(16) 0.0027(18) C8 0.022(2) 0.034(2) 0.024(2) -0.0065(18) 0.0010(17) 0.0024(18) C9 0.029(2) 0.035(2) 0.021(2) 0.0039(19) 0.0057(17) 0.0028(19) C10 0.022(2) 0.031(3) 0.036(3) -0.0028(19) 0.0110(19) -0.0016(18) C11 0.033(2) 0.027(2) 0.028(2) 0.0011(18) 0.0027(19) 0.0043(19) C12 0.031(2) 0.030(2) 0.035(3) -0.0013(19) 0.016(2) -0.001(2) C13 0.037(3) 0.0131(19) 0.031(2) 0.0032(17) 0.000(2) 0.0021(18) C14 0.034(2) 0.023(2) 0.033(3) 0.0045(18) 0.008(2) -0.0042(18) C15 0.026(2) 0.019(2) 0.036(3) -0.0026(18) 0.0062(19) -0.0012(17) C16 0.024(2) 0.023(2) 0.046(3) -0.0083(18) 0.010(2) -0.009(2) C17 0.032(2) 0.018(2) 0.038(3) -0.0057(18) 0.005(2) 0.0034(18) C18 0.022(2) 0.030(2) 0.047(3) -0.0084(19) 0.002(2) -0.0063(18) C19 0.030(2) 0.027(2) 0.018(2) -0.0080(17) 0.0037(17) 0.0058(18) C20 0.023(2) 0.026(2) 0.034(3) -0.0087(19) -0.0024(19) -0.0017(18) C21 0.028(2) 0.033(2) 0.028(2) -0.0073(19) -0.0054(19) 0.0006(19) C22 0.029(2) 0.031(2) 0.033(2) -0.0066(18) -0.007(2) 0.001(2) C23 0.026(2) 0.034(2) 0.025(2) 0.0003(19) 0.0014(17) 0.004(2) C24 0.026(2) 0.038(3) 0.033(3) -0.004(2) -0.0091(19) 0.004(2) C25 0.028(2) 0.035(2) 0.028(2) 0.0018(19) 0.0070(18) -0.003(2) C26 0.035(2) 0.028(2) 0.028(2) 0.0057(18) -0.004(2) 0.001(2) C27 0.043(3) 0.023(2) 0.026(2) 0.0050(18) -0.001(2) -0.006(2) C28 0.027(2) 0.034(2) 0.032(3) 0.0011(19) -0.008(2) 0.010(2) C29 0.032(2) 0.031(2) 0.029(2) 0.0006(17) 0.001(2) -0.0093(19) C30 0.043(3) 0.023(2) 0.033(3) 0.0015(19) -0.008(2) 0.0083(19) N1 0.0283(18) 0.0267(18) 0.0276(19) 0.0005(15) 0.0020(16) -0.0020(15) N2 0.0246(17) 0.0273(18) 0.0237(19) -0.0013(14) 0.0015(15) -0.0003(15) N3 0.030(2) 0.0231(18) 0.036(2) 0.0016(16) 0.0002(17) -0.0008(15) N4 0.0227(18) 0.0260(18) 0.032(2) -0.0040(15) 0.0003(16) -0.0013(14) N5 0.0206(16) 0.0245(19) 0.0265(19) -0.0043(14) 0.0043(14) -0.0011(14) N6 0.0242(18) 0.0255(18) 0.029(2) -0.0040(15) 0.0010(15) 0.0041(15) N7 0.0207(17) 0.0241(18) 0.034(2) 0.0009(15) 0.0082(15) 0.0026(14) N8 0.0184(16) 0.0299(19) 0.042(2) 0.0000(17) 0.0085(15) 0.0030(16) N9 0.0291(18) 0.0257(19) 0.031(2) -0.0030(16) 0.0092(17) -0.0043(16) N10 0.0254(18) 0.0270(18) 0.032(2) -0.0001(15) 0.0021(16) -0.0016(15) N11 0.038(2) 0.0246(18) 0.032(2) 0.0004(16) 0.0105(17) 0.0017(16) N12 0.0278(19) 0.0246(18) 0.046(2) -0.0105(16) 0.0011(18) -0.0023(15) N13 0.0213(17) 0.0276(18) 0.030(2) 0.0008(15) -0.0009(15) 0.0000(15) N14 0.0267(19) 0.030(2) 0.028(2) -0.0034(16) -0.0065(16) 0.0027(16) N15 0.0234(17) 0.032(2) 0.041(2) -0.0074(17) 0.0051(17) 0.0036(16) N16 0.0263(19) 0.034(2) 0.033(2) -0.0053(16) -0.0030(17) 0.0062(16) N17 0.0288(19) 0.0278(19) 0.0272(19) -0.0014(15) -0.0039(15) -0.0037(15) N18 0.032(2) 0.033(2) 0.031(2) -0.0033(16) -0.0037(17) -0.0035(16) N19 0.0262(18) 0.031(2) 0.032(2) -0.0063(16) -0.0052(16) 0.0064(16) N20 0.033(2) 0.029(2) 0.037(2) -0.0030(17) 0.0001(18) 0.0030(17) O1 0.0257(15) 0.0377(17) 0.0309(17) -0.0031(13) 0.0015(13) 0.0041(14) O2 0.0219(15) 0.0386(17) 0.0331(16) -0.0087(13) 0.0022(12) 0.0051(13) O3 0.0232(15) 0.0310(16) 0.0322(17) 0.0016(13) 0.0028(13) 0.0020(13) O4 0.0199(14) 0.0384(16) 0.0324(17) 0.0014(13) -0.0026(13) -0.0008(13) O5 0.0265(15) 0.0369(16) 0.0397(18) -0.0051(13) 0.0004(15) -0.0021(16) O6 0.0239(15) 0.0359(17) 0.0416(19) -0.0030(14) -0.0045(14) 0.0056(14) O7 0.0173(14) 0.0355(16) 0.0509(19) -0.0026(14) 0.0003(14) 0.0055(14) O8 0.0242(17) 0.0347(17) 0.055(2) -0.0103(15) 0.0024(15) 0.0038(14) O9 0.0229(15) 0.0451(18) 0.048(2) -0.0092(16) -0.0006(14) 0.0097(14) O10 0.0339(19) 0.0445(18) 0.046(2) -0.0113(15) -0.0023(17) 0.0053(15) C31 0.025(2) 0.039(3) 0.030(2) -0.001(2) -0.0052(19) -0.0027(19) C32 0.035(2) 0.038(3) 0.033(3) -0.001(2) -0.007(2) 0.002(2) C33 0.030(2) 0.042(3) 0.030(3) -0.006(2) -0.007(2) 0.001(2) C34 0.030(2) 0.036(2) 0.026(2) -0.0108(19) -0.0028(19) -0.005(2) C35 0.030(2) 0.051(3) 0.034(3) -0.012(2) -0.001(2) -0.007(2) C36 0.042(3) 0.057(3) 0.038(3) -0.002(2) 0.004(2) -0.016(3) C37 0.055(3) 0.047(3) 0.044(3) 0.010(3) 0.008(3) -0.009(3) C38 0.044(3) 0.045(3) 0.047(3) 0.009(2) 0.000(3) -0.001(2) C39 0.028(2) 0.039(3) 0.032(2) -0.004(2) -0.0053(19) -0.009(2) C40 0.027(2) 0.038(3) 0.037(3) -0.002(2) -0.001(2) 0.000(2) O11 0.0333(17) 0.058(2) 0.054(2) 0.0102(18) 0.0070(17) 0.0021(17) _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 O1W K2 2.737(3) . ? O2W K1 2.742(4) . ? O3W K2 3.008(4) . ? O3W K1 3.082(6) 1_455 ? O4W K2 2.890(5) . ? K1 O1 2.702(3) . ? K1 O2 2.703(3) . ? K1 O4 2.816(3) . ? K1 O3 2.841(3) . ? K1 O5 2.923(3) . ? K1 O3W 3.082(6) 1_655 ? K1 O11 3.318(4) . ? K2 O8 2.700(3) . ? K2 O7 2.765(3) . ? K2 O10 2.766(4) . ? K2 O6 2.859(3) . ? K2 O9 3.003(3) . ? C1 O1 1.224(5) . ? C1 N1 1.370(5) . ? C1 N2 1.377(5) . ? C2 N1 1.452(6) . ? C2 N3 1.453(6) . ? C2 C3 1.555(6) . ? C3 N2 1.442(5) . ? C3 N4 1.459(5) . ? C4 O6 1.226(5) . ? C4 N3 1.367(6) . ? C4 N4 1.371(6) . ? C5 N5 1.445(5) . ? C5 N2 1.453(5) . ? C6 N4 1.449(6) . ? C6 N7 1.451(6) . ? C7 O2 1.221(5) . ? C7 N6 1.366(5) . ? C7 N5 1.385(5) . ? C8 N7 1.440(6) . ? C8 N5 1.459(5) . ? C8 C9 1.541(7) . ? C9 N6 1.458(5) . ? C9 N8 1.463(5) . ? C10 O7 1.206(5) . ? C10 N8 1.370(6) . ? C10 N7 1.383(6) . ? C11 N6 1.434(6) . ? C11 N9 1.451(6) . ? C12 N8 1.439(6) . ? C12 N11 1.457(6) . ? C13 O3 1.229(5) . ? C13 N9 1.366(6) . ? C13 N10 1.371(6) . ? C14 N11 1.442(6) . ? C14 N9 1.454(5) . ? C14 C15 1.565(6) . ? C15 N12 1.450(6) . ? C15 N10 1.454(5) . ? C16 O8 1.222(5) . ? C16 N11 1.352(6) . ? C16 N12 1.382(6) . ? C17 N10 1.434(6) . ? C17 N13 1.473(6) . ? C18 N15 1.445(6) . ? C18 N12 1.446(6) . ? C19 O4 1.220(5) . ? C19 N13 1.367(6) . ? C19 N14 1.381(6) . ? C20 N15 1.437(5) . ? C20 N13 1.451(5) . ? C20 C21 1.561(6) . ? C21 N16 1.440(6) . ? C21 N14 1.455(6) . ? C22 O9 1.210(5) . ? C22 N15 1.374(6) . ? C22 N16 1.384(6) . ? C23 N14 1.438(6) . ? C23 N17 1.448(6) . ? C24 N19 1.446(6) . ? C24 N16 1.447(6) . ? C25 O5 1.218(5) . ? C25 N18 1.375(6) . ? C25 N17 1.381(6) . ? C26 N17 1.448(6) . ? C26 N19 1.463(6) . ? C26 C27 1.557(6) . ? C27 N18 1.437(6) . ? C27 N20 1.464(6) . ? C28 O10 1.218(5) . ? C28 N19 1.373(6) . ? C28 N20 1.374(6) . ? C29 N1 1.444(6) . ? C29 N18 1.457(6) . ? C30 N3 1.451(6) . ? C30 N20 1.455(6) . ? C31 C40 1.362(7) . ? C31 O11 1.385(6) . ? C31 C32 1.422(7) . ? C32 C33 1.348(7) . ? C33 C34 1.419(7) . ? C34 C35 1.415(7) . ? C34 C39 1.425(7) . ? C35 C36 1.386(8) . ? C36 C37 1.396(8) . ? C37 C38 1.358(8) . ? C38 C39 1.421(7) . ? C39 C40 1.440(7) . ? 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 K2 O3W K1 112.56(18) . 1_455 ? O1 K1 O2 71.90(9) . . ? O1 K1 O2W 94.43(11) . . ? O2 K1 O2W 67.73(11) . . ? O1 K1 O4 127.15(10) . . ? O2 K1 O4 126.77(10) . . ? O2W K1 O4 137.80(11) . . ? O1 K1 O3 133.52(9) . . ? O2 K1 O3 68.97(9) . . ? O2W K1 O3 93.18(10) . . ? O4 K1 O3 64.82(9) . . ? O1 K1 O5 68.18(9) . . ? O2 K1 O5 133.81(9) . . ? O2W K1 O5 136.58(11) . . ? O4 K1 O5 66.84(9) . . ? O3 K1 O5 128.10(9) . . ? O1 K1 O3W 66.99(11) . 1_655 ? O2 K1 O3W 125.30(11) . 1_655 ? O2W K1 O3W 80.97(12) . 1_655 ? O4 K1 O3W 106.75(11) . 1_655 ? O3 K1 O3W 159.34(11) . 1_655 ? O5 K1 O3W 55.68(11) . 1_655 ? O1 K1 O11 163.98(10) . . ? O2 K1 O11 122.22(10) . . ? O2W K1 O11 85.36(11) . . ? O4 K1 O11 52.79(9) . . ? O3 K1 O11 62.40(9) . . ? O5 K1 O11 101.16(9) . . ? O3W K1 O11 97.24(11) 1_655 . ? O8 K2 O1W 92.10(11) . . ? O8 K2 O7 73.18(10) . . ? O1W K2 O7 72.62(10) . . ? O8 K2 O10 122.67(10) . . ? O1W K2 O10 142.06(11) . . ? O7 K2 O10 128.15(10) . . ? O8 K2 O6 130.97(10) . . ? O1W K2 O6 102.00(10) . . ? O7 K2 O6 67.09(10) . . ? O10 K2 O6 68.03(10) . . ? O8 K2 O4W 152.9(2) . . ? O1W K2 O4W 76.18(16) . . ? O7 K2 O4W 124.15(13) . . ? O10 K2 O4W 65.91(16) . . ? O6 K2 O4W 75.85(19) . . ? O8 K2 O9 64.17(10) . . ? O1W K2 O9 126.26(10) . . ? O7 K2 O9 132.74(9) . . ? O10 K2 O9 66.92(10) . . ? O6 K2 O9 130.47(10) . . ? O4W K2 O9 103.07(13) . . ? O8 K2 O3W 89.96(14) . . ? O1W K2 O3W 79.43(11) . . ? O7 K2 O3W 146.45(13) . . ? O10 K2 O3W 85.40(13) . . ? O6 K2 O3W 138.53(14) . . ? O4W K2 O3W 64.1(2) . . ? O9 K2 O3W 54.94(10) . . ? O1 C1 N1 125.7(4) . . ? O1 C1 N2 126.0(4) . . ? N1 C1 N2 108.2(3) . . ? N1 C2 N3 115.7(4) . . ? N1 C2 C3 103.3(3) . . ? N3 C2 C3 103.1(3) . . ? N2 C3 N4 115.1(4) . . ? N2 C3 C2 103.3(3) . . ? N4 C3 C2 103.1(3) . . ? O6 C4 N3 125.9(4) . . ? O6 C4 N4 125.7(4) . . ? N3 C4 N4 108.4(4) . . ? N5 C5 N2 112.9(3) . . ? N4 C6 N7 114.3(3) . . ? O2 C7 N6 126.1(4) . . ? O2 C7 N5 125.8(4) . . ? N6 C7 N5 108.1(3) . . ? N7 C8 N5 115.2(3) . . ? N7 C8 C9 103.5(3) . . ? N5 C8 C9 103.0(3) . . ? N6 C9 N8 114.0(4) . . ? N6 C9 C8 104.0(3) . . ? N8 C9 C8 103.3(4) . . ? O7 C10 N8 126.3(4) . . ? O7 C10 N7 126.0(4) . . ? N8 C10 N7 107.7(4) . . ? N6 C11 N9 113.5(4) . . ? N8 C12 N11 112.9(3) . . ? O3 C13 N9 126.1(4) . . ? O3 C13 N10 125.6(4) . . ? N9 C13 N10 108.3(4) . . ? N11 C14 N9 114.4(4) . . ? N11 C14 C15 103.4(4) . . ? N9 C14 C15 102.6(3) . . ? N12 C15 N10 114.2(4) . . ? N12 C15 C14 102.8(3) . . ? N10 C15 C14 103.3(3) . . ? O8 C16 N11 126.7(4) . . ? O8 C16 N12 124.7(4) . . ? N11 C16 N12 108.6(4) . . ? N10 C17 N13 113.9(3) . . ? N15 C18 N12 114.5(3) . . ? O4 C19 N13 126.3(4) . . ? O4 C19 N14 125.2(4) . . ? N13 C19 N14 108.5(4) . . ? N15 C20 N13 115.3(4) . . ? N15 C20 C21 103.1(4) . . ? N13 C20 C21 103.1(3) . . ? N16 C21 N14 115.0(4) . . ? N16 C21 C20 103.4(4) . . ? N14 C21 C20 103.5(3) . . ? O9 C22 N15 127.0(4) . . ? O9 C22 N16 125.7(4) . . ? N15 C22 N16 107.3(4) . . ? N14 C23 N17 113.7(3) . . ? N19 C24 N16 113.6(3) . . ? O5 C25 N18 127.6(4) . . ? O5 C25 N17 125.4(4) . . ? N18 C25 N17 106.9(4) . . ? N17 C26 N19 114.7(4) . . ? N17 C26 C27 103.0(4) . . ? N19 C26 C27 103.6(4) . . ? N18 C27 N20 115.4(4) . . ? N18 C27 C26 103.3(4) . . ? N20 C27 C26 103.1(4) . . ? O10 C28 N19 125.3(4) . . ? O10 C28 N20 125.9(4) . . ? N19 C28 N20 108.7(4) . . ? N1 C29 N18 113.7(4) . . ? N3 C30 N20 113.5(4) . . ? C1 N1 C29 121.7(4) . . ? C1 N1 C2 112.3(3) . . ? C29 N1 C2 125.0(4) . . ? C1 N2 C3 112.5(3) . . ? C1 N2 C5 123.5(3) . . ? C3 N2 C5 123.2(3) . . ? C4 N3 C30 122.2(4) . . ? C4 N3 C2 112.7(4) . . ? C30 N3 C2 124.9(4) . . ? C4 N4 C6 121.7(4) . . ? C4 N4 C3 112.1(4) . . ? C6 N4 C3 123.3(4) . . ? C7 N5 C5 121.5(3) . . ? C7 N5 C8 111.7(3) . . ? C5 N5 C8 122.8(3) . . ? C7 N6 C11 121.6(4) . . ? C7 N6 C9 112.0(3) . . ? C11 N6 C9 126.1(4) . . ? C10 N7 C8 112.8(3) . . ? C10 N7 C6 121.4(4) . . ? C8 N7 C6 124.5(4) . . ? C10 N8 C12 123.2(4) . . ? C10 N8 C9 112.1(4) . . ? C12 N8 C9 123.9(4) . . ? C13 N9 C11 122.8(4) . . ? C13 N9 C14 113.2(4) . . ? C11 N9 C14 123.9(4) . . ? C13 N10 C17 122.6(4) . . ? C13 N10 C15 112.6(4) . . ? C17 N10 C15 124.8(4) . . ? C16 N11 C14 113.1(4) . . ? C16 N11 C12 121.8(4) . . ? C14 N11 C12 124.6(4) . . ? C16 N12 C18 122.2(4) . . ? C16 N12 C15 112.2(4) . . ? C18 N12 C15 125.5(4) . . ? C19 N13 C20 112.9(4) . . ? C19 N13 C17 122.6(3) . . ? C20 N13 C17 124.2(4) . . ? C19 N14 C23 122.4(4) . . ? C19 N14 C21 112.0(4) . . ? C23 N14 C21 125.1(4) . . ? C22 N15 C20 113.4(4) . . ? C22 N15 C18 122.1(4) . . ? C20 N15 C18 124.5(4) . . ? C22 N16 C21 112.8(4) . . ? C22 N16 C24 121.9(4) . . ? C21 N16 C24 125.4(4) . . ? C25 N17 C23 122.2(4) . . ? C25 N17 C26 113.1(4) . . ? C23 N17 C26 124.7(4) . . ? C25 N18 C27 113.6(4) . . ? C25 N18 C29 122.3(4) . . ? C27 N18 C29 124.1(4) . . ? C28 N19 C24 123.0(4) . . ? C28 N19 C26 112.1(4) . . ? C24 N19 C26 124.0(4) . . ? C28 N20 C30 122.4(4) . . ? C28 N20 C27 112.3(4) . . ? C30 N20 C27 124.3(4) . . ? C1 O1 K1 135.6(3) . . ? C7 O2 K1 133.2(3) . . ? C13 O3 K1 134.9(3) . . ? C19 O4 K1 138.9(3) . . ? C25 O5 K1 129.0(3) . . ? C4 O6 K2 131.5(3) . . ? C10 O7 K2 133.4(3) . . ? C16 O8 K2 140.7(3) . . ? C22 O9 K2 130.6(3) . . ? C28 O10 K2 138.0(3) . . ? C40 C31 O11 123.1(4) . . ? C40 C31 C32 120.3(4) . . ? O11 C31 C32 116.6(4) . . ? C33 C32 C31 120.7(5) . . ? C32 C33 C34 121.4(5) . . ? C35 C34 C33 122.9(5) . . ? C35 C34 C39 118.5(5) . . ? C33 C34 C39 118.5(4) . . ? C36 C35 C34 120.6(5) . . ? C35 C36 C37 119.9(5) . . ? C38 C37 C36 121.3(5) . . ? C37 C38 C39 120.4(5) . . ? C38 C39 C34 119.2(5) . . ? C38 C39 C40 122.0(5) . . ? C34 C39 C40 118.8(4) . . ? C31 C40 C39 120.2(4) . . ? C31 O11 K1 105.1(3) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.677 _refine_diff_density_min -0.809 _refine_diff_density_rms 0.082 data_D _database_code_depnum_ccdc_archive 'CCDC 742110' #TrackingRef 'web_deposit_cif_file_3_Xin-longNi_1352613104.D.submit.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H52 N22 O24 Tl2' _chemical_formula_weight 1633.78 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' Tl Tl -2.8358 9.6688 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 12.059(2) _cell_length_b 16.142(3) _cell_length_c 29.452(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5733.1(18) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.893 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3200 _exptl_absorpt_coefficient_mu 5.714 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39590 _diffrn_reflns_av_R_equivalents 0.0722 _diffrn_reflns_av_sigmaI/netI 0.0857 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 25.99 _reflns_number_total 10665 _reflns_number_gt 7922 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1056P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.027(10) _refine_ls_number_reflns 10665 _refine_ls_number_parameters 793 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0861 _refine_ls_R_factor_gt 0.0587 _refine_ls_wR_factor_ref 0.1806 _refine_ls_wR_factor_gt 0.1685 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1W O -0.2606(7) -0.0813(6) 0.7590(3) 0.044(2) Uani 1 1 d . . . O2W O -0.2366(8) 0.1226(6) 0.7580(4) 0.049(3) Uani 1 1 d . . . O3W O -0.2503(9) 0.0109(9) 0.6801(5) 0.082(4) Uani 1 1 d . . . O4W O -0.2481(9) -0.0178(12) 0.8797(7) 0.128(8) Uani 1 1 d . . . O5W O -0.3284(19) -0.2057(17) 0.8652(7) 0.207(15) Uani 1 1 d . . . O6W O 0.2706(17) -0.0089(14) 1.0590(7) 0.149(9) Uani 1 1 d . . . O7W O 0.528(4) 0.187(2) 0.5322(9) 0.46(4) Uani 1 1 d . . . N21 N 0.4831(12) 0.4768(11) 0.8933(6) 0.062(4) Uani 1 1 d . . . N22 N 0.0202(12) -0.4430(13) 0.8841(5) 0.068(5) Uani 1 1 d . . . O12 O 0.5594(13) 0.0427(8) 0.6236(5) 0.088(4) Uani 1 1 d . . . O13 O 0.4330(15) 0.4175(9) 0.8970(7) 0.124(7) Uani 1 1 d . . . O14 O 0.570(2) 0.4804(15) 0.9078(10) 0.192(12) Uani 1 1 d . . . O15 O -0.0421(14) -0.0082(8) 0.6315(4) 0.080(4) Uani 1 1 d . . . O16 O 0.0923(16) -0.3897(9) 0.8841(7) 0.123(7) Uani 1 1 d . . . O17 O 0.0690(16) 0.083(3) 0.6028(9) 0.37(3) Uani 1 1 d . . . Tl1 Tl -0.07444(5) 0.08849(3) 0.823578(19) 0.04305(17) Uani 1 1 d . . . Tl2 Tl 0.55661(5) -0.05455(3) 0.81400(2) 0.0512(2) Uani 1 1 d . . . C1 C 0.0866(9) 0.0512(7) 0.7194(4) 0.026(3) Uani 1 1 d . . . C2 C 0.2524(9) 0.0562(8) 0.6785(4) 0.031(3) Uani 1 1 d . . . H2 H 0.2592 0.0755 0.6471 0.037 Uiso 1 1 calc R . . C3 C 0.2112(9) -0.0329(6) 0.6809(4) 0.024(2) Uani 1 1 d . . . H3 H 0.1887 -0.0528 0.6509 0.029 Uiso 1 1 calc R . . C4 C 0.3939(10) -0.0297(7) 0.7112(4) 0.027(3) Uani 1 1 d . . . C5 C 0.0410(9) -0.0960(7) 0.7182(4) 0.026(3) Uani 1 1 d . . . H5A H -0.0335 -0.0735 0.7197 0.031 Uiso 1 1 calc R . . H5B H 0.0443 -0.1325 0.6921 0.031 Uiso 1 1 calc R . . C6 C 0.3035(9) -0.1666(7) 0.7108(4) 0.026(3) Uani 1 1 d . . . H6A H 0.2629 -0.1971 0.6878 0.031 Uiso 1 1 calc R . . H6B H 0.3790 -0.1872 0.7108 0.031 Uiso 1 1 calc R . . C7 C 0.0154(9) -0.1275(7) 0.7974(5) 0.032(3) Uani 1 1 d . . . C8 C 0.1423(9) -0.2101(7) 0.7595(4) 0.019(2) Uani 1 1 d . . . H8 H 0.1223 -0.2554 0.7389 0.023 Uiso 1 1 calc R . . C9 C 0.1377(9) -0.2372(7) 0.8088(4) 0.029(3) Uani 1 1 d . . . H9 H 0.1122 -0.2947 0.8114 0.035 Uiso 1 1 calc R . . C10 C 0.3216(11) -0.2042(7) 0.7906(4) 0.030(3) Uani 1 1 d . . . C11 C 0.0176(11) -0.1838(8) 0.8764(5) 0.036(3) Uani 1 1 d . . . H11A H 0.0164 -0.2410 0.8866 0.043 Uiso 1 1 calc R . . H11B H -0.0579 -0.1632 0.8769 0.043 Uiso 1 1 calc R . . C12 C 0.2945(11) -0.2464(7) 0.8690(4) 0.030(3) Uani 1 1 d . . . H12A H 0.3723 -0.2612 0.8669 0.036 Uiso 1 1 calc R . . H12B H 0.2549 -0.2939 0.8810 0.036 Uiso 1 1 calc R . . C13 C 0.0565(10) -0.0543(7) 0.9208(4) 0.026(3) Uani 1 1 d . . . C14 C 0.1884(10) -0.1643(8) 0.9310(4) 0.030(3) Uani 1 1 d . . . H14 H 0.1744 -0.2128 0.9501 0.035 Uiso 1 1 calc R . . C15 C 0.2239(11) -0.0859(8) 0.9597(5) 0.037(3) Uani 1 1 d . . . H15 H 0.2245 -0.0980 0.9923 0.044 Uiso 1 1 calc R . . C16 C 0.3669(10) -0.1255(8) 0.9108(4) 0.029(3) Uani 1 1 d . . . C17 C 0.1378(10) 0.0583(8) 0.9688(5) 0.033(3) Uani 1 1 d . . . H17A H 0.0619 0.0782 0.9702 0.039 Uiso 1 1 calc R . . H17B H 0.1655 0.0549 0.9996 0.039 Uiso 1 1 calc R . . C18 C 0.4082(11) -0.0061(8) 0.9631(4) 0.034(3) Uani 1 1 d . . . H18A H 0.3941 -0.0025 0.9954 0.041 Uiso 1 1 calc R . . H18B H 0.4841 -0.0248 0.9590 0.041 Uiso 1 1 calc R . . C19 C 0.1602(10) 0.1688(7) 0.9128(4) 0.028(3) Uani 1 1 d . . . C20 C 0.3174(9) 0.1375(8) 0.9552(4) 0.028(3) Uani 1 1 d . . . H20 H 0.3244 0.1539 0.9871 0.034 Uiso 1 1 calc R . . C21 C 0.3432(10) 0.2082(8) 0.9244(4) 0.027(3) Uani 1 1 d . . . H21 H 0.3649 0.2573 0.9418 0.033 Uiso 1 1 calc R . . C22 C 0.4690(10) 0.0999(8) 0.9090(5) 0.031(3) Uani 1 1 d . . . C23 C 0.2236(10) 0.2865(8) 0.8648(5) 0.038(3) Uani 1 1 d . . . H23A H 0.1458 0.3017 0.8656 0.045 Uiso 1 1 calc R . . H23B H 0.2662 0.3354 0.8728 0.045 Uiso 1 1 calc R . . C24 C 0.4947(9) 0.2243(7) 0.8613(4) 0.026(3) Uani 1 1 d . . . H24A H 0.4993 0.2821 0.8702 0.031 Uiso 1 1 calc R . . H24B H 0.5698 0.2029 0.8596 0.031 Uiso 1 1 calc R . . C25 C 0.1739(11) 0.2361(7) 0.7905(5) 0.032(3) Uani 1 1 d . . . C26 C 0.3565(9) 0.2736(7) 0.7989(4) 0.019(2) Uani 1 1 d . . . H26 H 0.3792 0.3319 0.7986 0.023 Uiso 1 1 calc R . . C27 C 0.3386(9) 0.2400(7) 0.7509(4) 0.027(3) Uani 1 1 d . . . H27 H 0.3576 0.2819 0.7282 0.032 Uiso 1 1 calc R . . C28 C 0.4776(9) 0.1607(7) 0.7868(4) 0.025(3) Uani 1 1 d . . . C29 C 0.1652(10) 0.1909(7) 0.7085(4) 0.029(3) Uani 1 1 d . . . H29A H 0.0883 0.2084 0.7098 0.035 Uiso 1 1 calc R . . H29B H 0.1987 0.2164 0.6821 0.035 Uiso 1 1 calc R . . C30 C 0.4350(11) 0.1220(7) 0.7053(4) 0.031(3) Uani 1 1 d . . . H30A H 0.4247 0.1585 0.6795 0.037 Uiso 1 1 calc R . . H30B H 0.5112 0.1028 0.7051 0.037 Uiso 1 1 calc R . . N1 N 0.1692(7) 0.1024(6) 0.7035(4) 0.029(2) Uani 1 1 d . . . N2 N 0.1170(7) -0.0296(6) 0.7115(3) 0.019(2) Uani 1 1 d . . . N3 N 0.3605(8) 0.0513(6) 0.7013(4) 0.028(2) Uani 1 1 d . . . N4 N 0.3053(8) -0.0793(6) 0.6978(3) 0.027(2) Uani 1 1 d . . . N5 N 0.0612(8) -0.1432(6) 0.7580(3) 0.024(2) Uani 1 1 d . . . N6 N 0.0597(9) -0.1803(6) 0.8307(4) 0.033(2) Uani 1 1 d . . . N7 N 0.2566(7) -0.1830(6) 0.7526(3) 0.021(2) Uani 1 1 d . . . N8 N 0.2544(8) -0.2287(6) 0.8251(4) 0.029(2) Uani 1 1 d . . . N9 N 0.0855(9) -0.1348(7) 0.9074(4) 0.037(3) Uani 1 1 d . . . N10 N 0.1386(8) -0.0262(6) 0.9482(3) 0.027(2) Uani 1 1 d . . . N11 N 0.2823(9) -0.1765(7) 0.9007(4) 0.038(3) Uani 1 1 d . . . N12 N 0.3330(9) -0.0677(6) 0.9432(4) 0.033(3) Uani 1 1 d . . . N13 N 0.2028(8) 0.1161(6) 0.9442(3) 0.028(2) Uani 1 1 d . . . N14 N 0.2430(7) 0.2234(6) 0.8992(4) 0.026(2) Uani 1 1 d . . . N15 N 0.3969(8) 0.0733(6) 0.9438(4) 0.031(2) Uani 1 1 d . . . N16 N 0.4348(8) 0.1789(6) 0.8964(3) 0.026(2) Uani 1 1 d . . . N17 N 0.2519(7) 0.2629(6) 0.8188(3) 0.023(2) Uani 1 1 d . . . N18 N 0.2218(8) 0.2194(6) 0.7487(3) 0.026(2) Uani 1 1 d . . . N19 N 0.4445(8) 0.2192(6) 0.8168(4) 0.029(2) Uani 1 1 d . . . N20 N 0.4138(9) 0.1685(6) 0.7478(4) 0.033(3) Uani 1 1 d . . . O1 O 0.0018(6) 0.0760(5) 0.7384(3) 0.028(2) Uani 1 1 d . . . O2 O -0.0604(7) -0.0795(5) 0.8071(3) 0.0323(18) Uani 1 1 d . . . O3 O -0.0260(7) -0.0187(5) 0.9091(3) 0.038(2) Uani 1 1 d . . . O4 O 0.0648(7) 0.1710(5) 0.8982(3) 0.0303(18) Uani 1 1 d . . . O5 O 0.0721(7) 0.2283(5) 0.7967(3) 0.0333(19) Uani 1 1 d . . . O6 O 0.4812(6) -0.0507(5) 0.7240(3) 0.0291(19) Uani 1 1 d . . . O7 O 0.4221(7) -0.1996(5) 0.7928(3) 0.0303(19) Uani 1 1 d . . . O8 O 0.4613(7) -0.1262(6) 0.8924(3) 0.040(2) Uani 1 1 d . . . O9 O 0.5480(6) 0.0628(5) 0.8945(3) 0.0310(19) Uani 1 1 d . . . O10 O 0.5546(7) 0.1116(5) 0.7912(3) 0.033(2) Uani 1 1 d . . . C31 C -0.2863(12) 0.3036(9) 0.9225(5) 0.046(4) Uani 1 1 d . . . H31 H -0.2934 0.3517 0.9053 0.055 Uiso 1 1 calc R . . C32 C -0.3599(10) 0.2857(8) 0.9513(4) 0.031(3) Uani 1 1 d . . . H32 H -0.4210 0.3204 0.9539 0.037 Uiso 1 1 calc R . . C33 C -0.3538(10) 0.2184(8) 0.9784(4) 0.032(3) Uani 1 1 d . . . C34 C -0.4381(12) 0.1942(11) 1.0128(4) 0.047(4) Uani 1 1 d . . . H34 H -0.5018 0.2262 1.0158 0.057 Uiso 1 1 calc R . . C35 C -0.4250(15) 0.1272(11) 1.0397(5) 0.059(5) Uani 1 1 d . . . H35 H -0.4804 0.1127 1.0601 0.071 Uiso 1 1 calc R . . C36 C -0.3249(14) 0.0779(10) 1.0367(5) 0.057(4) Uani 1 1 d . . . H36 H -0.3139 0.0355 1.0576 0.069 Uiso 1 1 calc R . . C37 C -0.2491(13) 0.0913(12) 1.0054(5) 0.060(4) Uani 1 1 d . . . H37 H -0.1889 0.0556 1.0027 0.072 Uiso 1 1 calc R . . C38 C -0.2597(10) 0.1636(8) 0.9744(5) 0.036(3) Uani 1 1 d . . . C39 C -0.1809(11) 0.1803(8) 0.9411(4) 0.033(3) Uani 1 1 d . . . H39 H -0.1224 0.1437 0.9365 0.040 Uiso 1 1 calc R . . C40 C -0.1888(10) 0.2495(7) 0.9155(5) 0.030(3) Uani 1 1 d . . . O11 O -0.1115(7) 0.2711(6) 0.8813(3) 0.040(2) Uani 1 1 d . . . H11 H -0.1325 0.2527 0.8568 0.060 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1W 0.038(5) 0.036(5) 0.057(6) -0.004(5) -0.006(5) -0.003(4) O2W 0.029(5) 0.032(5) 0.087(8) -0.005(5) 0.009(5) -0.001(4) O3W 0.071(9) 0.122(12) 0.054(8) -0.001(8) 0.001(6) -0.007(8) O4W 0.037(8) 0.19(2) 0.156(17) -0.099(15) -0.017(8) 0.025(10) O5W 0.18(2) 0.27(3) 0.17(2) -0.14(2) -0.082(17) 0.15(2) O6W 0.146(18) 0.19(2) 0.112(16) -0.049(14) -0.003(12) 0.044(16) O7W 0.83(10) 0.40(5) 0.16(2) -0.05(3) -0.22(4) -0.38(6) N21 0.042(8) 0.073(11) 0.070(10) -0.002(8) -0.001(8) -0.002(8) N22 0.042(8) 0.114(15) 0.048(9) -0.019(9) -0.018(7) -0.004(9) O12 0.096(10) 0.071(8) 0.098(10) -0.029(8) 0.005(9) -0.024(9) O13 0.105(12) 0.058(9) 0.21(2) -0.008(10) 0.018(13) -0.031(10) O14 0.15(2) 0.136(18) 0.29(3) 0.03(2) -0.12(2) 0.002(17) O15 0.135(13) 0.048(7) 0.056(7) -0.007(6) -0.039(9) 0.025(8) O16 0.126(14) 0.061(9) 0.182(18) 0.009(10) -0.019(13) -0.037(10) O17 0.058(12) 0.88(10) 0.17(2) 0.23(4) -0.057(14) 0.06(3) Tl1 0.0485(3) 0.0300(3) 0.0506(3) -0.0079(2) 0.0047(3) 0.0025(2) Tl2 0.0529(4) 0.0405(3) 0.0600(4) -0.0059(3) 0.0030(3) 0.0003(3) C1 0.022(6) 0.030(6) 0.026(6) 0.011(5) -0.006(5) -0.007(5) C2 0.025(6) 0.043(7) 0.025(7) -0.001(6) 0.008(5) 0.011(5) C3 0.016(5) 0.024(6) 0.032(7) -0.007(5) -0.001(6) 0.004(4) C4 0.021(6) 0.026(6) 0.034(7) -0.002(5) 0.012(6) -0.002(5) C5 0.021(6) 0.028(6) 0.030(6) -0.008(5) -0.009(5) 0.000(5) C6 0.014(6) 0.026(6) 0.036(7) 0.000(5) 0.000(5) 0.008(5) C7 0.016(6) 0.021(6) 0.059(9) -0.003(6) -0.002(6) -0.005(5) C8 0.016(6) 0.014(5) 0.028(7) 0.003(5) -0.008(5) -0.002(4) C9 0.029(6) 0.013(5) 0.046(8) -0.009(5) -0.003(6) -0.009(5) C10 0.044(8) 0.006(5) 0.042(8) -0.016(5) 0.003(7) 0.002(5) C11 0.032(7) 0.036(7) 0.038(8) -0.006(6) 0.008(6) -0.002(6) C12 0.031(7) 0.025(7) 0.033(7) 0.001(5) -0.005(6) 0.004(5) C13 0.019(6) 0.029(6) 0.030(6) -0.002(5) 0.010(5) -0.005(6) C14 0.029(7) 0.029(7) 0.031(7) -0.009(5) 0.006(6) -0.004(6) C15 0.043(8) 0.026(6) 0.041(8) -0.001(6) 0.001(6) 0.000(6) C16 0.029(7) 0.028(6) 0.029(7) 0.003(6) -0.013(6) 0.002(5) C17 0.031(7) 0.025(6) 0.043(8) -0.009(6) 0.004(6) 0.005(5) C18 0.030(7) 0.035(7) 0.037(7) 0.007(6) -0.013(6) 0.000(6) C19 0.022(7) 0.026(6) 0.036(7) -0.013(6) 0.008(6) 0.002(5) C20 0.017(6) 0.041(7) 0.027(7) -0.007(6) 0.003(5) 0.004(5) C21 0.021(6) 0.025(6) 0.036(8) -0.012(6) -0.001(5) -0.003(5) C22 0.020(6) 0.034(7) 0.039(8) -0.008(6) -0.010(6) -0.004(5) C23 0.016(6) 0.027(7) 0.070(11) 0.005(7) 0.000(6) 0.006(5) C24 0.018(6) 0.023(6) 0.038(8) -0.015(5) 0.002(5) -0.007(5) C25 0.044(8) 0.006(5) 0.047(8) 0.005(5) 0.008(7) 0.003(5) C26 0.021(6) 0.018(5) 0.018(6) 0.004(4) -0.002(5) 0.002(4) C27 0.018(6) 0.017(6) 0.047(8) 0.009(5) -0.001(6) -0.004(5) C28 0.024(6) 0.028(6) 0.023(6) -0.001(5) -0.007(5) -0.015(5) C29 0.026(6) 0.022(6) 0.039(8) 0.003(5) -0.018(6) 0.004(5) C30 0.027(6) 0.023(6) 0.043(7) -0.008(5) -0.003(6) -0.005(6) N1 0.011(4) 0.025(6) 0.049(7) 0.000(5) 0.000(4) 0.003(4) N2 0.013(4) 0.018(5) 0.027(5) -0.007(4) -0.003(4) 0.001(4) N3 0.018(5) 0.018(5) 0.049(7) 0.002(5) -0.004(5) -0.002(4) N4 0.025(5) 0.023(5) 0.033(6) -0.001(4) 0.008(4) -0.001(4) N5 0.019(5) 0.030(5) 0.023(5) -0.008(4) 0.003(5) 0.008(4) N6 0.028(5) 0.023(5) 0.047(7) 0.007(4) 0.006(5) -0.002(4) N7 0.012(5) 0.021(5) 0.029(6) -0.002(4) -0.006(4) 0.004(4) N8 0.023(5) 0.020(5) 0.043(7) 0.001(5) 0.006(5) 0.001(4) N9 0.025(6) 0.047(7) 0.038(6) -0.009(5) -0.007(5) -0.012(5) N10 0.024(5) 0.026(5) 0.030(6) -0.003(5) 0.001(5) -0.001(4) N11 0.036(6) 0.030(6) 0.047(7) 0.008(5) -0.011(6) -0.011(5) N12 0.032(6) 0.028(6) 0.038(6) 0.000(5) 0.004(5) 0.009(5) N13 0.018(5) 0.030(6) 0.035(6) -0.007(5) -0.006(5) -0.003(4) N14 0.016(5) 0.022(5) 0.041(6) -0.002(5) 0.000(5) 0.001(4) N15 0.020(5) 0.027(6) 0.046(6) 0.005(5) 0.004(5) 0.008(4) N16 0.016(5) 0.028(5) 0.033(6) -0.005(4) 0.004(5) 0.000(5) N17 0.027(5) 0.026(5) 0.015(5) -0.003(4) -0.007(4) -0.007(4) N18 0.022(5) 0.023(5) 0.033(6) 0.000(4) 0.002(5) -0.002(4) N19 0.025(5) 0.024(5) 0.040(6) -0.004(4) 0.008(5) 0.000(4) N20 0.034(6) 0.024(5) 0.042(7) -0.002(5) 0.010(5) 0.004(5) O1 0.011(4) 0.037(5) 0.037(5) -0.010(4) -0.003(3) 0.007(3) O2 0.024(4) 0.033(4) 0.040(5) -0.001(4) -0.002(4) 0.001(4) O3 0.022(5) 0.029(5) 0.062(6) -0.011(4) -0.003(4) -0.003(4) O4 0.017(4) 0.037(5) 0.036(5) 0.000(4) 0.000(4) 0.006(4) O5 0.020(4) 0.029(4) 0.051(5) 0.000(4) 0.003(4) 0.007(4) O6 0.013(4) 0.034(5) 0.040(5) 0.000(4) -0.001(4) 0.004(4) O7 0.013(4) 0.031(4) 0.047(5) -0.005(4) -0.003(4) 0.006(4) O8 0.030(5) 0.042(5) 0.046(6) -0.008(4) 0.002(5) 0.004(4) O9 0.016(4) 0.035(5) 0.042(5) -0.011(4) -0.002(4) 0.006(4) O10 0.027(4) 0.026(4) 0.047(5) -0.009(4) -0.010(4) 0.006(4) C31 0.030(8) 0.047(8) 0.060(10) -0.016(8) -0.025(8) 0.005(7) C32 0.019(6) 0.040(8) 0.035(7) -0.011(6) 0.016(6) -0.002(5) C33 0.027(7) 0.043(8) 0.026(7) -0.010(6) 0.000(5) -0.007(6) C34 0.031(7) 0.094(12) 0.016(6) -0.010(7) 0.006(6) -0.006(8) C35 0.064(11) 0.091(12) 0.023(7) -0.011(8) 0.003(8) -0.034(11) C36 0.074(11) 0.047(9) 0.051(10) 0.004(8) 0.020(9) -0.005(9) C37 0.046(9) 0.076(12) 0.057(10) 0.026(9) 0.008(8) -0.001(9) C38 0.027(7) 0.036(7) 0.045(9) 0.002(6) 0.000(6) -0.001(6) C39 0.031(7) 0.027(7) 0.042(9) 0.013(6) 0.006(6) 0.000(5) C40 0.022(6) 0.028(7) 0.041(8) 0.000(6) -0.001(6) -0.002(5) O11 0.032(5) 0.042(5) 0.046(6) -0.006(5) 0.002(4) -0.002(4) _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 O1W Tl2 2.770(10) 1_455 ? N21 O14 1.13(2) . ? N21 O13 1.136(19) . ? N21 O12 1.282(19) 4_656 ? N22 O15 1.18(2) 4_546 ? N22 O17 1.22(3) 4_546 ? N22 O16 1.22(2) . ? O12 N21 1.282(19) 4_646 ? O15 N22 1.18(2) 4_556 ? O17 N22 1.22(3) 4_556 ? Tl1 O1 2.680(8) . ? Tl1 O2 2.759(8) . ? Tl2 O10 2.765(8) . ? Tl2 O1W 2.770(10) 1_655 ? C1 O1 1.233(14) . ? C1 N2 1.373(16) . ? C1 N1 1.376(15) . ? C2 N1 1.451(15) . ? C2 N3 1.469(15) . ? C2 C3 1.523(18) . ? C3 N4 1.449(14) . ? C3 N2 1.450(14) . ? C4 O6 1.168(14) . ? C4 N4 1.391(15) . ? C4 N3 1.400(16) . ? C5 N5 1.420(15) . ? C5 N2 1.424(15) . ? C6 N7 1.380(15) . ? C6 N4 1.459(15) . ? C7 O2 1.233(14) . ? C7 N5 1.310(16) . ? C7 N6 1.404(16) . ? C8 N5 1.458(14) . ? C8 N7 1.460(14) . ? C8 C9 1.518(17) . ? C9 N6 1.464(15) . ? C9 N8 1.493(15) . ? C10 O7 1.216(15) . ? C10 N8 1.358(16) . ? C10 N7 1.409(16) . ? C11 N6 1.441(17) . ? C11 N9 1.460(17) . ? C12 N8 1.410(16) . ? C12 N11 1.472(16) . ? C13 O3 1.198(14) . ? C13 N10 1.356(15) . ? C13 N9 1.402(16) . ? C14 N11 1.454(17) . ? C14 N9 1.498(17) . ? C14 C15 1.582(18) . ? C15 N12 1.433(17) . ? C15 N10 1.449(16) . ? C16 O8 1.261(15) . ? C16 N11 1.344(16) . ? C16 N12 1.395(16) . ? C17 N13 1.418(16) . ? C17 N10 1.493(16) . ? C18 N15 1.408(16) . ? C18 N12 1.468(16) . ? C19 O4 1.229(15) . ? C19 N13 1.357(16) . ? C19 N14 1.390(15) . ? C20 N15 1.452(15) . ? C20 N13 1.460(16) . ? C20 C21 1.491(18) . ? C21 N14 1.439(15) . ? C21 N16 1.457(15) . ? C22 O9 1.204(14) . ? C22 N16 1.390(16) . ? C22 N15 1.411(17) . ? C23 N17 1.448(17) . ? C23 N14 1.457(16) . ? C24 N19 1.445(15) . ? C24 N16 1.458(15) . ? C25 O5 1.247(16) . ? C25 N17 1.330(16) . ? C25 N18 1.385(16) . ? C26 N17 1.401(14) . ? C26 N19 1.475(14) . ? C26 C27 1.529(17) . ? C27 N18 1.448(15) . ? C27 N20 1.471(15) . ? C28 O10 1.228(14) . ? C28 N19 1.354(15) . ? C28 N20 1.389(16) . ? C29 N1 1.437(15) . ? C29 N18 1.443(16) . ? C30 N3 1.456(15) . ? C30 N20 1.480(15) . ? C31 C32 1.26(2) . ? C31 C40 1.478(19) . ? C32 C33 1.350(19) . ? C33 C38 1.444(18) . ? C33 C34 1.487(18) . ? C34 C35 1.35(2) . ? C35 C36 1.45(3) . ? C36 C37 1.32(2) . ? C37 C38 1.49(2) . ? C38 C39 1.392(18) . ? C39 C40 1.351(17) . ? C40 O11 1.416(16) . ? 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 O14 N21 O13 120(2) . . ? O14 N21 O12 118(2) . 4_656 ? O13 N21 O12 121.6(18) . 4_656 ? O15 N22 O17 129(3) 4_546 4_546 ? O15 N22 O16 117.9(17) 4_546 . ? O17 N22 O16 113(3) 4_546 . ? O1 Tl1 O2 74.9(3) . . ? O10 Tl2 O1W 90.9(3) . 1_655 ? O1 C1 N2 127.4(10) . . ? O1 C1 N1 124.0(11) . . ? N2 C1 N1 108.6(10) . . ? N1 C2 N3 114.1(10) . . ? N1 C2 C3 103.6(9) . . ? N3 C2 C3 102.6(10) . . ? N4 C3 N2 114.8(10) . . ? N4 C3 C2 104.4(9) . . ? N2 C3 C2 104.5(9) . . ? O6 C4 N4 128.0(12) . . ? O6 C4 N3 126.6(11) . . ? N4 C4 N3 105.0(10) . . ? N5 C5 N2 114.1(9) . . ? N7 C6 N4 115.2(10) . . ? O2 C7 N5 129.7(12) . . ? O2 C7 N6 120.2(12) . . ? N5 C7 N6 109.9(10) . . ? N5 C8 N7 114.1(9) . . ? N5 C8 C9 102.6(9) . . ? N7 C8 C9 104.8(9) . . ? N6 C9 N8 114.0(9) . . ? N6 C9 C8 105.3(9) . . ? N8 C9 C8 104.2(9) . . ? O7 C10 N8 124.9(13) . . ? O7 C10 N7 125.6(12) . . ? N8 C10 N7 109.4(11) . . ? N6 C11 N9 111.4(10) . . ? N8 C12 N11 113.1(10) . . ? O3 C13 N10 128.0(11) . . ? O3 C13 N9 124.9(11) . . ? N10 C13 N9 107.1(10) . . ? N11 C14 N9 113.8(10) . . ? N11 C14 C15 103.0(10) . . ? N9 C14 C15 102.5(10) . . ? N12 C15 N10 115.9(11) . . ? N12 C15 C14 103.3(10) . . ? N10 C15 C14 102.4(10) . . ? O8 C16 N11 125.8(12) . . ? O8 C16 N12 124.3(11) . . ? N11 C16 N12 109.8(11) . . ? N13 C17 N10 113.0(10) . . ? N15 C18 N12 113.3(10) . . ? O4 C19 N13 127.7(11) . . ? O4 C19 N14 123.5(12) . . ? N13 C19 N14 108.8(10) . . ? N15 C20 N13 113.9(10) . . ? N15 C20 C21 105.5(9) . . ? N13 C20 C21 104.1(10) . . ? N14 C21 N16 113.5(10) . . ? N14 C21 C20 105.6(10) . . ? N16 C21 C20 104.8(9) . . ? O9 C22 N16 126.7(12) . . ? O9 C22 N15 126.3(12) . . ? N16 C22 N15 106.9(10) . . ? N17 C23 N14 115.4(10) . . ? N19 C24 N16 114.0(9) . . ? O5 C25 N17 129.6(12) . . ? O5 C25 N18 121.4(12) . . ? N17 C25 N18 108.9(11) . . ? N17 C26 N19 115.1(9) . . ? N17 C26 C27 102.4(9) . . ? N19 C26 C27 102.8(9) . . ? N18 C27 N20 114.6(10) . . ? N18 C27 C26 105.1(10) . . ? N20 C27 C26 104.5(9) . . ? O10 C28 N19 127.1(11) . . ? O10 C28 N20 124.4(11) . . ? N19 C28 N20 108.4(10) . . ? N1 C29 N18 112.6(10) . . ? N3 C30 N20 111.1(10) . . ? C1 N1 C29 122.5(10) . . ? C1 N1 C2 111.4(10) . . ? C29 N1 C2 125.9(10) . . ? C1 N2 C5 121.3(9) . . ? C1 N2 C3 110.4(9) . . ? C5 N2 C3 124.2(9) . . ? C4 N3 C30 122.6(10) . . ? C4 N3 C2 113.6(10) . . ? C30 N3 C2 122.9(10) . . ? C4 N4 C3 113.6(9) . . ? C4 N4 C6 119.5(10) . . ? C3 N4 C6 125.2(9) . . ? C7 N5 C5 123.7(10) . . ? C7 N5 C8 113.5(10) . . ? C5 N5 C8 122.6(9) . . ? C7 N6 C11 122.9(10) . . ? C7 N6 C9 108.5(10) . . ? C11 N6 C9 127.8(10) . . ? C6 N7 C10 121.9(10) . . ? C6 N7 C8 124.7(9) . . ? C10 N7 C8 109.9(9) . . ? C10 N8 C12 122.7(10) . . ? C10 N8 C9 110.5(11) . . ? C12 N8 C9 126.8(10) . . ? C13 N9 C11 122.5(11) . . ? C13 N9 C14 111.8(10) . . ? C11 N9 C14 125.6(11) . . ? C13 N10 C15 115.8(10) . . ? C13 N10 C17 122.8(10) . . ? C15 N10 C17 121.2(10) . . ? C16 N11 C14 111.9(11) . . ? C16 N11 C12 122.3(12) . . ? C14 N11 C12 124.8(10) . . ? C16 N12 C15 111.4(11) . . ? C16 N12 C18 123.0(11) . . ? C15 N12 C18 124.8(11) . . ? C19 N13 C17 123.4(10) . . ? C19 N13 C20 111.2(10) . . ? C17 N13 C20 124.4(10) . . ? C19 N14 C21 110.3(10) . . ? C19 N14 C23 121.9(10) . . ? C21 N14 C23 127.8(10) . . ? C18 N15 C22 120.7(10) . . ? C18 N15 C20 128.4(11) . . ? C22 N15 C20 110.9(10) . . ? C22 N16 C21 111.8(10) . . ? C22 N16 C24 120.2(10) . . ? C21 N16 C24 127.9(10) . . ? C25 N17 C26 114.6(10) . . ? C25 N17 C23 120.3(10) . . ? C26 N17 C23 124.8(9) . . ? C25 N18 C29 126.4(11) . . ? C25 N18 C27 108.8(10) . . ? C29 N18 C27 124.7(10) . . ? C28 N19 C24 120.6(10) . . ? C28 N19 C26 113.1(10) . . ? C24 N19 C26 126.3(9) . . ? C28 N20 C27 111.1(10) . . ? C28 N20 C30 123.9(11) . . ? C27 N20 C30 123.9(11) . . ? C1 O1 Tl1 137.2(7) . . ? C7 O2 Tl1 134.8(7) . . ? C28 O10 Tl2 131.2(7) . . ? C32 C31 C40 121.2(14) . . ? C31 C32 C33 123.0(13) . . ? C32 C33 C38 119.2(12) . . ? C32 C33 C34 125.3(13) . . ? C38 C33 C34 115.5(13) . . ? C35 C34 C33 122.1(15) . . ? C34 C35 C36 120.2(15) . . ? C37 C36 C35 122.0(16) . . ? C36 C37 C38 119.9(16) . . ? C39 C38 C33 118.4(12) . . ? C39 C38 C37 121.7(12) . . ? C33 C38 C37 119.9(12) . . ? C40 C39 C38 120.3(12) . . ? C39 C40 O11 123.7(11) . . ? C39 C40 C31 117.8(13) . . ? O11 C40 C31 118.5(12) . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 1.764 _refine_diff_density_min -1.841 _refine_diff_density_rms 0.228