# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Guo-Bi Li' _publ_contact_author_email lgbgo2004@yahoo.com.cn loop_ _publ_author_name 'Guobi Li' 'Jianrong He' 'Junmin Liu' 'Cheng-Yong Su' data_0 _database_code_depnum_ccdc_archive 'CCDC 803603' #TrackingRef '0.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H44 Cd2 N12 O28.40' _chemical_formula_weight 1468.15 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' Cd Cd -0.8075 1.2024 '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 7.687(5) _cell_length_b 13.508(5) _cell_length_c 16.022(5) _cell_angle_alpha 74.365(5) _cell_angle_beta 79.218(5) _cell_angle_gamma 84.054(5) _cell_volume 1571.3(13) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2988 _cell_measurement_theta_min 3.0399 _cell_measurement_theta_max 29.9764 _exptl_crystal_description block _exptl_crystal_colour white _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.552 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 739 _exptl_absorpt_coefficient_mu 0.770 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.95965 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Gemini S Ultra' _diffrn_measurement_method '\w and \p scan' _diffrn_detector_area_resol_mean 16.0855 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 9293 _diffrn_reflns_av_R_equivalents 0.0421 _diffrn_reflns_av_sigmaI/netI 0.1304 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6152 _reflns_number_gt 3823 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker FRAMBO' _computing_cell_refinement 'Bruker FRAMBO' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.1824P)^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 geom _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6152 _refine_ls_number_parameters 386 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.1345 _refine_ls_R_factor_gt 0.0959 _refine_ls_wR_factor_ref 0.2843 _refine_ls_wR_factor_gt 0.2598 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.000 _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 Cd1 Cd 1.46200(10) 0.16874(6) 0.13237(5) 0.0252(3) Uani 1 1 d . . . O3 O 1.2086(10) -0.5266(6) 0.7685(5) 0.0313(17) Uani 1 1 d . . . O2 O 1.0930(9) -0.2851(5) 0.2977(4) 0.0259(16) Uani 1 1 d . . . O6 O 1.5707(10) 0.1665(6) -0.0207(5) 0.0331(17) Uani 1 1 d . . . O1 O 1.6142(9) -0.3476(6) 0.4064(4) 0.0280(16) Uani 1 1 d . . . O4 O 0.6893(9) -0.4581(6) 0.6596(5) 0.0317(17) Uani 1 1 d . . . N2 N 1.3733(10) -0.2999(6) 0.3319(5) 0.0199(17) Uani 1 1 d . . . O11 O 1.2252(11) 0.0952(6) 0.1021(5) 0.0388(14) Uani 1 1 d DU . . H11 H 1.1379 0.0721 0.1503 0.047 Uiso 1 1 calc R . . N4 N 0.6531(12) -0.3323(7) 0.9172(6) 0.028(2) Uani 1 1 d . . . N3 N 0.9261(11) -0.4976(6) 0.7357(5) 0.0200(17) Uani 1 1 d . . . O7 O 1.8368(10) 0.1991(6) -0.0903(5) 0.038(2) Uani 1 1 d . . . O5 O 1.7637(11) 0.2085(6) 0.0452(5) 0.0387(19) Uani 1 1 d . . . O8 O 1.2326(13) 0.1567(7) 0.2623(5) 0.052(2) Uani 1 1 d . . . O12 O 1.6018(10) 0.2337(6) 0.2239(5) 0.0388(14) Uani 1 1 d U . . H12 H 1.6128 0.1915 0.2793 0.047 Uiso 1 1 calc R . . C10 C 1.1915(12) -0.3059(7) 0.3511(6) 0.0183(19) Uani 1 1 d . . . N5 N 1.7289(13) 0.1917(7) -0.0241(6) 0.031(2) Uani 1 1 d . . . C13 C 0.9936(12) -0.4188(7) 0.5889(6) 0.0167(19) Uani 1 1 d . . . C4 C 1.5770(12) -0.1755(7) 0.2241(6) 0.019(2) Uani 1 1 d . . . C12 C 1.1494(12) -0.4383(7) 0.6215(6) 0.0178(19) Uani 1 1 d . . . C17 C 0.831(2) -0.5534(11) 0.8196(9) 0.056(2) Uani 1 1 d . . . H17A H 0.9055 -0.6130 0.8437 0.067 Uiso 1 1 calc R . . H17B H 0.7252 -0.5783 0.8096 0.067 Uiso 1 1 calc R . . C6 C 1.4740(12) -0.2698(7) 0.2412(6) 0.0179(19) Uani 1 1 d . . . H6A H 1.3918 -0.2570 0.1998 0.021 Uiso 1 1 calc R . . H6B H 1.5556 -0.3267 0.2308 0.021 Uiso 1 1 calc R . . O10 O 0.9914(12) 0.1993(9) 0.2005(8) 0.073(4) Uani 1 1 d . . . O9 O 1.0120(18) 0.2419(9) 0.3194(8) 0.082(4) Uani 1 1 d . . . N1 N 1.5818(11) 0.0066(6) 0.1845(5) 0.0256(19) Uani 1 1 d . . . C15 C 1.1104(13) -0.4919(7) 0.7169(6) 0.021(2) Uani 1 1 d . . . C18 C 0.7789(13) -0.4914(7) 0.8868(7) 0.024(2) Uani 1 1 d . . . C14 C 0.9877(13) -0.3733(7) 0.5005(6) 0.020(2) Uani 1 1 d . . . H14A H 0.8817 -0.3602 0.4785 0.024 Uiso 1 1 calc R . . C19 C 0.7036(14) -0.3907(7) 0.8624(6) 0.025(2) Uani 1 1 d . . . H19A H 0.6887 -0.3639 0.8042 0.030 Uiso 1 1 calc R . . C16 C 0.8474(13) -0.4564(7) 0.6620(6) 0.021(2) Uani 1 1 d . . . C9 C 1.1486(12) -0.3491(7) 0.4477(6) 0.0183(19) Uani 1 1 d . . . C8 C 1.3078(12) -0.3699(7) 0.4813(6) 0.0184(19) Uani 1 1 d . . . C22 C 0.7924(15) -0.5322(9) 0.9746(7) 0.033(3) Uani 1 1 d . . . H22A H 0.8416 -0.5987 0.9931 0.040 Uiso 1 1 calc R . . C3 C 1.7554(13) -0.1846(8) 0.2305(7) 0.027(2) Uani 1 1 d . . . H3A H 1.8135 -0.2493 0.2449 0.032 Uiso 1 1 calc R . . C11 C 1.3154(12) -0.4140(7) 0.5691(6) 0.019(2) Uani 1 1 d . . . H11A H 1.4210 -0.4265 0.5916 0.023 Uiso 1 1 calc R . . C5 C 1.4966(12) -0.0774(7) 0.2000(6) 0.021(2) Uani 1 1 d . . . H5A H 1.3772 -0.0710 0.1947 0.025 Uiso 1 1 calc R . . C7 C 1.4551(12) -0.3384(7) 0.4050(6) 0.021(2) Uani 1 1 d . . . N6 N 1.0729(17) 0.1990(9) 0.2624(7) 0.052(3) Uani 1 1 d . . . C20 C 0.6710(14) -0.3728(9) 1.0018(7) 0.034(3) Uani 1 1 d . . . H20A H 0.6406 -0.3316 1.0410 0.041 Uiso 1 1 calc R . . C2 C 1.8476(13) -0.0955(9) 0.2152(7) 0.034(3) Uani 1 1 d . . . H2A H 1.9676 -0.0995 0.2188 0.041 Uiso 1 1 calc R . . C21 C 0.7345(19) -0.4760(11) 1.0333(8) 0.050(4) Uani 1 1 d . . . H21A H 0.7362 -0.5042 1.0929 0.060 Uiso 1 1 calc R . . C1 C 1.7545(13) -0.0018(9) 0.1944(7) 0.030(2) Uani 1 1 d . . . H1A H 1.8123 0.0579 0.1870 0.036 Uiso 1 1 calc R . . C23 C 1.194(2) 0.0802(12) 0.0218(8) 0.056(2) Uani 1 1 d D . . H23A H 1.0838 0.0475 0.0319 0.084 Uiso 1 1 calc R . . H23B H 1.2888 0.0373 -0.0003 0.084 Uiso 1 1 calc R . . H23C H 1.1870 0.1456 -0.0204 0.084 Uiso 1 1 calc R . . O2W O 1.206(2) -0.1079(14) 0.3874(11) 0.099(5) Uiso 0.80 1 d P . . C24 C 1.668(2) 0.3296(11) 0.2007(10) 0.056(2) Uani 1 1 d . . . H24A H 1.7197 0.3388 0.2480 0.084 Uiso 1 1 calc R . . H24B H 1.5737 0.3811 0.1888 0.084 Uiso 1 1 calc R . . H24C H 1.7569 0.3360 0.1490 0.084 Uiso 1 1 calc R . . O4W O 1.069(2) -0.0306(15) 0.4981(12) 0.033(4) Uiso 0.40 1 d P . 1 O3W O 1.113(5) 0.030(3) 0.544(2) 0.102(11) Uiso 0.40 1 d P A 2 O1W O 1.603(3) 0.1583(19) 0.3900(15) 0.101(7) Uiso 0.60 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0328(5) 0.0199(4) 0.0245(4) -0.0099(3) -0.0008(3) -0.0047(3) O3 0.040(4) 0.033(4) 0.021(4) -0.005(3) -0.019(3) 0.012(3) O2 0.024(4) 0.035(4) 0.016(3) -0.002(3) -0.005(3) 0.003(3) O6 0.033(4) 0.037(4) 0.031(4) -0.018(3) -0.003(3) 0.005(3) O1 0.023(4) 0.038(4) 0.021(4) -0.003(3) -0.004(3) -0.007(3) O4 0.026(4) 0.039(4) 0.026(4) -0.005(3) -0.002(3) -0.003(3) N2 0.023(4) 0.018(4) 0.020(4) -0.005(3) -0.004(3) -0.004(3) O11 0.046(3) 0.041(3) 0.036(3) -0.020(3) -0.004(3) -0.009(3) N4 0.034(5) 0.023(5) 0.029(5) -0.007(4) -0.006(4) -0.005(4) N3 0.028(4) 0.017(4) 0.016(4) -0.008(3) -0.001(3) -0.003(3) O7 0.039(4) 0.046(5) 0.020(4) -0.001(3) 0.009(3) -0.003(4) O5 0.053(5) 0.036(5) 0.027(4) -0.004(4) -0.006(4) -0.016(4) O8 0.068(7) 0.059(6) 0.027(4) -0.017(4) 0.019(4) -0.029(5) O12 0.046(3) 0.041(3) 0.036(3) -0.020(3) -0.004(3) -0.009(3) C10 0.025(5) 0.012(4) 0.018(5) -0.003(4) -0.009(4) 0.004(4) N5 0.043(6) 0.022(5) 0.029(5) -0.009(4) -0.002(4) -0.004(4) C13 0.019(5) 0.016(5) 0.017(5) -0.008(4) -0.002(4) -0.003(4) C4 0.023(5) 0.021(5) 0.018(5) -0.006(4) -0.009(4) -0.003(4) C12 0.025(5) 0.016(5) 0.016(4) -0.006(4) -0.009(4) 0.005(4) C17 0.059(5) 0.058(5) 0.053(5) -0.021(4) -0.003(4) -0.009(4) C6 0.026(5) 0.015(5) 0.011(4) -0.001(4) -0.004(4) 0.003(4) O10 0.036(5) 0.102(9) 0.109(9) -0.088(8) 0.011(6) -0.017(5) O9 0.121(10) 0.067(7) 0.069(7) -0.050(6) 0.002(7) 0.011(7) N1 0.032(5) 0.025(5) 0.021(4) -0.011(4) 0.003(4) -0.009(4) C15 0.029(5) 0.014(5) 0.023(5) -0.009(4) -0.004(4) 0.003(4) C18 0.027(5) 0.019(5) 0.027(5) -0.006(4) -0.005(4) -0.009(4) C14 0.026(5) 0.019(5) 0.019(5) -0.004(4) -0.011(4) -0.006(4) C19 0.039(6) 0.020(5) 0.016(5) -0.005(4) 0.003(4) -0.008(4) C16 0.024(5) 0.019(5) 0.024(5) -0.014(4) -0.001(4) 0.006(4) C9 0.021(5) 0.020(5) 0.017(5) -0.008(4) -0.007(4) 0.002(4) C8 0.020(5) 0.017(5) 0.021(5) -0.007(4) -0.004(4) -0.004(4) C22 0.037(6) 0.028(6) 0.036(6) -0.010(5) -0.012(5) 0.011(5) C3 0.023(5) 0.029(6) 0.022(5) 0.004(4) -0.004(4) -0.001(4) C11 0.017(4) 0.020(5) 0.022(5) -0.006(4) -0.009(4) 0.004(4) C5 0.020(5) 0.024(5) 0.019(5) -0.008(4) 0.000(4) -0.005(4) C7 0.020(5) 0.025(5) 0.020(5) -0.007(4) -0.004(4) 0.000(4) N6 0.060(8) 0.047(7) 0.042(6) -0.025(5) 0.032(6) -0.019(6) C20 0.033(6) 0.051(7) 0.023(5) -0.021(5) -0.003(5) 0.002(5) C2 0.018(5) 0.044(7) 0.033(6) 0.008(5) -0.009(4) -0.009(5) C21 0.069(9) 0.064(9) 0.023(6) -0.020(6) -0.024(6) 0.026(7) C1 0.025(5) 0.038(6) 0.024(5) 0.001(5) -0.008(4) -0.014(5) C23 0.059(5) 0.058(5) 0.053(5) -0.021(4) -0.003(4) -0.009(4) C24 0.059(5) 0.058(5) 0.053(5) -0.021(4) -0.003(4) -0.009(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 Cd1 N4 2.282(9) 2_756 ? Cd1 N1 2.286(9) . ? Cd1 O11 2.346(8) . ? Cd1 O12 2.356(8) . ? Cd1 O6 2.445(7) . ? Cd1 O8 2.444(8) . ? Cd1 O5 2.502(8) . ? O3 C15 1.193(12) . ? O2 C10 1.206(11) . ? O6 N5 1.284(12) . ? O1 C7 1.221(11) . ? O4 C16 1.226(12) . ? N2 C10 1.379(12) . ? N2 C7 1.384(12) . ? N2 C6 1.485(11) . ? O11 C23 1.422(13) . ? O11 H11 0.9300 . ? N4 C19 1.314(13) . ? N4 C20 1.345(14) . ? N4 Cd1 2.282(9) 2_756 ? N3 C16 1.383(13) . ? N3 C15 1.398(13) . ? N3 C17 1.452(16) . ? O7 N5 1.206(11) . ? O5 N5 1.270(11) . ? O8 N6 1.300(15) . ? O12 C24 1.372(16) . ? O12 H12 0.9300 . ? C10 C9 1.485(13) . ? C13 C12 1.367(13) . ? C13 C14 1.391(13) . ? C13 C16 1.482(13) . ? C4 C3 1.385(14) . ? C4 C5 1.390(13) . ? C4 C6 1.505(13) . ? C12 C11 1.407(13) . ? C12 C15 1.493(13) . ? C17 C18 1.510(17) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? O10 N6 1.266(16) . ? O9 N6 1.207(13) . ? N1 C5 1.310(12) . ? N1 C1 1.357(13) . ? C18 C22 1.384(15) . ? C18 C19 1.404(14) . ? C14 C9 1.377(14) . ? C14 H14A 0.9300 . ? C19 H19A 0.9300 . ? C9 C8 1.400(13) . ? C8 C11 1.382(13) . ? C8 C7 1.503(13) . ? C22 C21 1.349(16) . ? C22 H22A 0.9300 . ? C3 C2 1.401(15) . ? C3 H3A 0.9300 . ? C11 H11A 0.9300 . ? C5 H5A 0.9300 . ? C20 C21 1.417(17) . ? C20 H20A 0.9300 . ? C2 C1 1.378(16) . ? C2 H2A 0.9300 . ? C21 H21A 0.9300 . ? C1 H1A 0.9300 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? O4W O4W 1.27(4) 2_756 ? 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 N4 Cd1 N1 178.4(3) 2_756 . ? N4 Cd1 O11 92.7(3) 2_756 . ? N1 Cd1 O11 88.8(3) . . ? N4 Cd1 O12 87.1(3) 2_756 . ? N1 Cd1 O12 91.2(3) . . ? O11 Cd1 O12 152.9(3) . . ? N4 Cd1 O6 88.3(3) 2_756 . ? N1 Cd1 O6 92.6(3) . . ? O11 Cd1 O6 79.6(3) . . ? O12 Cd1 O6 127.5(3) . . ? N4 Cd1 O8 86.4(3) 2_756 . ? N1 Cd1 O8 93.4(3) . . ? O11 Cd1 O8 75.0(3) . . ? O12 Cd1 O8 78.0(3) . . ? O6 Cd1 O8 153.7(3) . . ? N4 Cd1 O5 93.3(3) 2_756 . ? N1 Cd1 O5 86.1(3) . . ? O11 Cd1 O5 131.0(3) . . ? O12 Cd1 O5 76.0(3) . . ? O6 Cd1 O5 52.1(3) . . ? O8 Cd1 O5 154.0(3) . . ? N5 O6 Cd1 96.9(6) . . ? C10 N2 C7 113.0(8) . . ? C10 N2 C6 123.7(8) . . ? C7 N2 C6 122.7(8) . . ? C23 O11 Cd1 130.4(8) . . ? C23 O11 H11 114.8 . . ? Cd1 O11 H11 114.8 . . ? C19 N4 C20 117.7(9) . . ? C19 N4 Cd1 119.9(7) . 2_756 ? C20 N4 Cd1 122.4(7) . 2_756 ? C16 N3 C15 112.2(8) . . ? C16 N3 C17 123.6(9) . . ? C15 N3 C17 123.6(9) . . ? N5 O5 Cd1 94.5(6) . . ? N6 O8 Cd1 125.2(7) . . ? C24 O12 Cd1 124.2(8) . . ? C24 O12 H12 117.9 . . ? Cd1 O12 H12 117.9 . . ? O2 C10 N2 125.3(9) . . ? O2 C10 C9 128.6(9) . . ? N2 C10 C9 106.0(8) . . ? O7 N5 O5 122.6(10) . . ? O7 N5 O6 120.9(9) . . ? O5 N5 O6 116.5(8) . . ? C12 C13 C14 122.2(9) . . ? C12 C13 C16 108.3(8) . . ? C14 C13 C16 129.5(9) . . ? C3 C4 C5 118.4(9) . . ? C3 C4 C6 120.6(9) . . ? C5 C4 C6 121.0(8) . . ? C13 C12 C11 123.2(8) . . ? C13 C12 C15 108.6(8) . . ? C11 C12 C15 128.2(8) . . ? N3 C17 C18 114.7(11) . . ? N3 C17 H17A 108.6 . . ? C18 C17 H17A 108.6 . . ? N3 C17 H17B 108.6 . . ? C18 C17 H17B 108.6 . . ? H17A C17 H17B 107.6 . . ? N2 C6 C4 113.2(8) . . ? N2 C6 H6A 108.9 . . ? C4 C6 H6A 108.9 . . ? N2 C6 H6B 108.9 . . ? C4 C6 H6B 108.9 . . ? H6A C6 H6B 107.8 . . ? C5 N1 C1 119.1(9) . . ? C5 N1 Cd1 123.8(7) . . ? C1 N1 Cd1 117.0(7) . . ? O3 C15 N3 124.9(9) . . ? O3 C15 C12 130.2(9) . . ? N3 C15 C12 104.9(8) . . ? C22 C18 C19 117.5(9) . . ? C22 C18 C17 122.2(10) . . ? C19 C18 C17 120.2(10) . . ? C9 C14 C13 115.9(8) . . ? C9 C14 H14A 122.1 . . ? C13 C14 H14A 122.1 . . ? N4 C19 C18 123.7(9) . . ? N4 C19 H19A 118.1 . . ? C18 C19 H19A 118.1 . . ? O4 C16 N3 125.1(9) . . ? O4 C16 C13 128.8(9) . . ? N3 C16 C13 106.0(8) . . ? C14 C9 C8 121.7(8) . . ? C14 C9 C10 130.0(8) . . ? C8 C9 C10 108.2(8) . . ? C11 C8 C9 123.0(8) . . ? C11 C8 C7 129.9(8) . . ? C9 C8 C7 107.0(8) . . ? C21 C22 C18 120.3(10) . . ? C21 C22 H22A 119.9 . . ? C18 C22 H22A 119.9 . . ? C4 C3 C2 119.4(9) . . ? C4 C3 H3A 120.3 . . ? C2 C3 H3A 120.3 . . ? C8 C11 C12 114.0(8) . . ? C8 C11 H11A 123.0 . . ? C12 C11 H11A 123.0 . . ? N1 C5 C4 122.8(9) . . ? N1 C5 H5A 118.6 . . ? C4 C5 H5A 118.6 . . ? O1 C7 N2 126.9(9) . . ? O1 C7 C8 127.3(9) . . ? N2 C7 C8 105.7(8) . . ? O9 N6 O10 122.5(13) . . ? O9 N6 O8 117.9(14) . . ? O10 N6 O8 119.4(10) . . ? N4 C20 C21 122.3(10) . . ? N4 C20 H20A 118.8 . . ? C21 C20 H20A 118.8 . . ? C1 C2 C3 117.7(9) . . ? C1 C2 H2A 121.1 . . ? C3 C2 H2A 121.1 . . ? C22 C21 C20 118.2(10) . . ? C22 C21 H21A 120.9 . . ? C20 C21 H21A 120.9 . . ? N1 C1 C2 122.5(10) . . ? N1 C1 H1A 118.8 . . ? C2 C1 H1A 118.8 . . ? O11 C23 H23A 109.5 . . ? O11 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? O11 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O12 C24 H24A 109.5 . . ? O12 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? O12 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 Cd1 O6 N5 96.4(6) 2_756 . . . ? N1 Cd1 O6 N5 -82.3(6) . . . . ? O11 Cd1 O6 N5 -170.6(6) . . . . ? O12 Cd1 O6 N5 11.3(7) . . . . ? O8 Cd1 O6 N5 174.7(6) . . . . ? O5 Cd1 O6 N5 0.8(5) . . . . ? N4 Cd1 O11 C23 81.2(10) 2_756 . . . ? N1 Cd1 O11 C23 -99.4(10) . . . . ? O12 Cd1 O11 C23 170.1(9) . . . . ? O6 Cd1 O11 C23 -6.5(10) . . . . ? O8 Cd1 O11 C23 166.8(11) . . . . ? O5 Cd1 O11 C23 -15.5(11) . . . . ? N4 Cd1 O5 N5 -86.0(6) 2_756 . . . ? N1 Cd1 O5 N5 95.5(6) . . . . ? O11 Cd1 O5 N5 10.5(7) . . . . ? O12 Cd1 O5 N5 -172.2(6) . . . . ? O6 Cd1 O5 N5 -0.8(5) . . . . ? O8 Cd1 O5 N5 -174.7(7) . . . . ? N4 Cd1 O8 N6 35.5(9) 2_756 . . . ? N1 Cd1 O8 N6 -146.1(9) . . . . ? O11 Cd1 O8 N6 -58.3(9) . . . . ? O12 Cd1 O8 N6 123.3(9) . . . . ? O6 Cd1 O8 N6 -43.3(13) . . . . ? O5 Cd1 O8 N6 125.8(9) . . . . ? N4 Cd1 O12 C24 -35.5(9) 2_756 . . . ? N1 Cd1 O12 C24 144.4(9) . . . . ? O11 Cd1 O12 C24 -125.8(10) . . . . ? O6 Cd1 O12 C24 50.1(10) . . . . ? O8 Cd1 O12 C24 -122.5(10) . . . . ? O5 Cd1 O12 C24 58.7(9) . . . . ? C7 N2 C10 O2 -173.8(9) . . . . ? C6 N2 C10 O2 -2.2(14) . . . . ? C7 N2 C10 C9 2.5(10) . . . . ? C6 N2 C10 C9 174.1(8) . . . . ? Cd1 O5 N5 O7 -179.1(8) . . . . ? Cd1 O5 N5 O6 1.3(9) . . . . ? Cd1 O6 N5 O7 179.0(8) . . . . ? Cd1 O6 N5 O5 -1.4(9) . . . . ? C14 C13 C12 C11 0.3(14) . . . . ? C16 C13 C12 C11 178.8(8) . . . . ? C14 C13 C12 C15 -177.1(8) . . . . ? C16 C13 C12 C15 1.4(10) . . . . ? C16 N3 C17 C18 -100.6(13) . . . . ? C15 N3 C17 C18 88.6(13) . . . . ? C10 N2 C6 C4 120.3(9) . . . . ? C7 N2 C6 C4 -68.8(11) . . . . ? C3 C4 C6 N2 97.1(10) . . . . ? C5 C4 C6 N2 -84.2(11) . . . . ? N4 Cd1 N1 C5 145(10) 2_756 . . . ? O11 Cd1 N1 C5 -11.7(7) . . . . ? O12 Cd1 N1 C5 141.2(7) . . . . ? O6 Cd1 N1 C5 -91.1(7) . . . . ? O8 Cd1 N1 C5 63.2(8) . . . . ? O5 Cd1 N1 C5 -142.8(8) . . . . ? N4 Cd1 N1 C1 -39(11) 2_756 . . . ? O11 Cd1 N1 C1 164.3(7) . . . . ? O12 Cd1 N1 C1 -42.8(7) . . . . ? O6 Cd1 N1 C1 84.8(7) . . . . ? O8 Cd1 N1 C1 -120.8(7) . . . . ? O5 Cd1 N1 C1 33.1(7) . . . . ? C16 N3 C15 O3 -176.3(9) . . . . ? C17 N3 C15 O3 -4.5(15) . . . . ? C16 N3 C15 C12 1.8(10) . . . . ? C17 N3 C15 C12 173.6(9) . . . . ? C13 C12 C15 O3 176.0(10) . . . . ? C11 C12 C15 O3 -1.3(17) . . . . ? C13 C12 C15 N3 -1.9(10) . . . . ? C11 C12 C15 N3 -179.2(9) . . . . ? N3 C17 C18 C22 -139.0(11) . . . . ? N3 C17 C18 C19 44.9(16) . . . . ? C12 C13 C14 C9 -0.1(13) . . . . ? C16 C13 C14 C9 -178.2(9) . . . . ? C20 N4 C19 C18 -1.7(16) . . . . ? Cd1 N4 C19 C18 178.7(8) 2_756 . . . ? C22 C18 C19 N4 3.1(16) . . . . ? C17 C18 C19 N4 179.4(10) . . . . ? C15 N3 C16 O4 174.9(9) . . . . ? C17 N3 C16 O4 3.1(15) . . . . ? C15 N3 C16 C13 -1.0(10) . . . . ? C17 N3 C16 C13 -172.8(9) . . . . ? C12 C13 C16 O4 -176.0(10) . . . . ? C14 C13 C16 O4 2.3(17) . . . . ? C12 C13 C16 N3 -0.3(10) . . . . ? C14 C13 C16 N3 178.0(9) . . . . ? C13 C14 C9 C8 0.5(13) . . . . ? C13 C14 C9 C10 176.3(9) . . . . ? O2 C10 C9 C14 -2.0(17) . . . . ? N2 C10 C9 C14 -178.0(9) . . . . ? O2 C10 C9 C8 174.2(9) . . . . ? N2 C10 C9 C8 -1.8(10) . . . . ? C14 C9 C8 C11 -1.2(14) . . . . ? C10 C9 C8 C11 -177.8(9) . . . . ? C14 C9 C8 C7 177.2(9) . . . . ? C10 C9 C8 C7 0.6(10) . . . . ? C19 C18 C22 C21 0.0(17) . . . . ? C17 C18 C22 C21 -176.2(13) . . . . ? C5 C4 C3 C2 1.9(14) . . . . ? C6 C4 C3 C2 -179.4(9) . . . . ? C9 C8 C11 C12 1.3(13) . . . . ? C7 C8 C11 C12 -176.7(9) . . . . ? C13 C12 C11 C8 -0.9(13) . . . . ? C15 C12 C11 C8 176.0(9) . . . . ? C1 N1 C5 C4 -1.8(14) . . . . ? Cd1 N1 C5 C4 174.1(7) . . . . ? C3 C4 C5 N1 -1.1(14) . . . . ? C6 C4 C5 N1 -179.8(8) . . . . ? C10 N2 C7 O1 175.9(9) . . . . ? C6 N2 C7 O1 4.1(15) . . . . ? C10 N2 C7 C8 -2.1(10) . . . . ? C6 N2 C7 C8 -173.8(8) . . . . ? C11 C8 C7 O1 1.1(17) . . . . ? C9 C8 C7 O1 -177.1(10) . . . . ? C11 C8 C7 N2 179.1(9) . . . . ? C9 C8 C7 N2 0.8(10) . . . . ? Cd1 O8 N6 O9 -136.3(10) . . . . ? Cd1 O8 N6 O10 39.6(15) . . . . ? C19 N4 C20 C21 -2.7(17) . . . . ? Cd1 N4 C20 C21 176.9(9) 2_756 . . . ? C4 C3 C2 C1 0.2(16) . . . . ? C18 C22 C21 C20 -4(2) . . . . ? N4 C20 C21 C22 6(2) . . . . ? C5 N1 C1 C2 4.1(15) . . . . ? Cd1 N1 C1 C2 -172.1(8) . . . . ? C3 C2 C1 N1 -3.2(16) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 3.684 _refine_diff_density_min -2.895 _refine_diff_density_rms 0.246 # Attachment '1.CIF' data_1 _database_code_depnum_ccdc_archive 'CCDC 803604' #TrackingRef '1.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C94 H72 Cd3 Cl12 N22 O38' _chemical_formula_weight 2880.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd 0.1185 4.6533 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 '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 11.6915(4) _cell_length_b 14.5628(7) _cell_length_c 17.3643(8) _cell_angle_alpha 104.113(4) _cell_angle_beta 104.147(4) _cell_angle_gamma 95.717(4) _cell_volume 2740.1(2) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8325 _cell_measurement_theta_min 2.7316 _cell_measurement_theta_max 62.6046 _exptl_crystal_description block _exptl_crystal_colour white _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.746 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1442 _exptl_absorpt_coefficient_mu 8.147 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.22699 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Gemini S Ultra' _diffrn_measurement_method '\w and \p scan' _diffrn_detector_area_resol_mean 16.0855 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 15995 _diffrn_reflns_av_R_equivalents 0.0499 _diffrn_reflns_av_sigmaI/netI 0.0503 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.73 _diffrn_reflns_theta_max 60.00 _reflns_number_total 8107 _reflns_number_gt 6788 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker FRAMBO' _computing_cell_refinement 'Bruker FRAMBO' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.1584P)^2^+16.3551P] 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 geom _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8107 _refine_ls_number_parameters 729 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0937 _refine_ls_R_factor_gt 0.0829 _refine_ls_wR_factor_ref 0.2561 _refine_ls_wR_factor_gt 0.2361 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.095 _refine_ls_shift/su_max 0.000 _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 Cl6 Cl 0.9378(3) 0.24660(18) 0.61747(16) 0.0569(7) Uani 1 1 d . . . Cl5 Cl 0.8689(3) 0.4223(2) 0.58872(17) 0.0599(7) Uani 1 1 d . . . Cl4 Cl 0.7677(2) 0.3343(2) 0.69527(16) 0.0567(7) Uani 1 1 d . . . Cl3 Cl 0.3933(3) 0.2005(2) 0.36281(18) 0.0641(7) Uani 1 1 d . . . Cl2 Cl 0.5592(4) 0.3535(4) 0.4937(3) 0.1083(15) Uani 1 1 d . . . Cl1 Cl 0.3778(9) 0.2362(3) 0.5288(3) 0.194(4) Uani 1 1 d . . . C8 C 1.0806(7) -0.0415(6) 0.3137(5) 0.0294(17) Uani 1 1 d . . . C18 C 1.5779(8) -0.2285(6) 0.2574(5) 0.0298(17) Uani 1 1 d . . . C5 C 0.8834(8) 0.3202(6) 0.3720(5) 0.0343(19) Uani 1 1 d . . . H5A H 0.9423 0.3684 0.3725 0.041 Uiso 1 1 calc R . . C35 C 0.1196(7) 0.4998(6) 0.0149(5) 0.0279(17) Uani 1 1 d . . . C44 C 0.2945(8) 0.2129(6) -0.0931(6) 0.036(2) Uani 1 1 d . . . H44A H 0.2180 0.2071 -0.1277 0.043 Uiso 1 1 calc R . . C7 C 0.9582(8) -0.0198(6) 0.3105(5) 0.0301(18) Uani 1 1 d . . . C37 C 0.1101(8) 0.3865(6) -0.1062(5) 0.0296(18) Uani 1 1 d . . . C38 C 0.0394(8) 0.4398(6) -0.0559(5) 0.0294(18) Uani 1 1 d . . . C39 C 0.3302(8) 0.3856(6) -0.0905(5) 0.0326(18) Uani 1 1 d . . . H39A H 0.3971 0.4385 -0.0695 0.039 Uiso 1 1 calc R . . H39B H 0.3081 0.3696 -0.1504 0.039 Uiso 1 1 calc R . . C30 C 0.0402(8) 0.0947(7) 0.0153(6) 0.038(2) Uani 1 1 d . . . C19 C 1.5036(7) -0.3158(6) 0.2251(5) 0.0301(17) Uani 1 1 d . . . H19A H 1.4270 -0.3203 0.1912 0.036 Uiso 1 1 calc R . . C3 C 0.8339(7) 0.1658(6) 0.3914(5) 0.0308(18) Uani 1 1 d . . . C16 C 1.4434(8) -0.0579(6) 0.3481(5) 0.0322(18) Uani 1 1 d . . . C13 C 1.3184(8) -0.0475(6) 0.3498(5) 0.0312(18) Uani 1 1 d . . . C9 C 1.1547(8) 0.0081(6) 0.3913(5) 0.0302(18) Uani 1 1 d . . . C14 C 1.2769(8) 0.0046(6) 0.4129(5) 0.0356(19) Uani 1 1 d . . . H14A H 1.3270 0.0349 0.4656 0.043 Uiso 1 1 calc R . . C20 C 1.5421(8) -0.3969(6) 0.2428(5) 0.0316(18) Uani 1 1 d . . . H20A H 1.4898 -0.4552 0.2202 0.038 Uiso 1 1 calc R . . C23 C 0.4605(8) 0.3323(6) 0.2143(6) 0.043(2) Uani 1 1 d . . . H23A H 0.5114 0.3043 0.1854 0.051 Uiso 1 1 calc R . . C4 C 0.9183(8) 0.2377(6) 0.3893(6) 0.037(2) Uani 1 1 d . . . H4A H 0.9984 0.2307 0.3995 0.044 Uiso 1 1 calc R . . C47 C 0.8958(8) 0.3560(7) 0.6607(6) 0.040(2) Uani 1 1 d . . . H05E H 0.9618 0.3932 0.7084 0.048 Uiso 1 1 calc R . . C34 C 0.0822(8) 0.5638(6) 0.0743(5) 0.0332(19) Uani 1 1 d . . . H34 H 0.1351 0.6051 0.1221 0.040 Uiso 1 1 calc R . . C12 C 1.2414(8) -0.0974(6) 0.2723(5) 0.0310(18) Uani 1 1 d . . . C26 C 0.3131(9) 0.4135(7) 0.2975(6) 0.042(2) Uani 1 1 d . . . H26A H 0.2637 0.4429 0.3270 0.050 Uiso 1 1 calc R . . C33 C 0.0217(8) 0.0389(7) -0.0645(6) 0.042(2) Uani 1 1 d . . . H33A H 0.0356 0.0644 -0.1062 0.051 Uiso 1 1 calc R . . C27 C 0.4349(8) 0.4418(6) 0.3262(6) 0.040(2) Uani 1 1 d . . . H27A H 0.4671 0.4900 0.3755 0.048 Uiso 1 1 calc R . . C36 C 0.2428(8) 0.4855(6) 0.0133(5) 0.0316(18) Uani 1 1 d . . . C22 C 1.6917(8) -0.2260(7) 0.3062(6) 0.040(2) Uani 1 1 d . . . H22A H 1.7456 -0.1685 0.3279 0.048 Uiso 1 1 calc R . . C2 C 0.7180(8) 0.1794(7) 0.3737(7) 0.046(2) Uani 1 1 d . . . H2A H 0.6579 0.1323 0.3735 0.055 Uiso 1 1 calc R . . C24 C 0.3411(8) 0.3008(7) 0.1825(6) 0.044(2) Uani 1 1 d . . . H24A H 0.3108 0.2527 0.1329 0.053 Uiso 1 1 calc R . . C43 C 0.3320(8) 0.1343(6) -0.0708(6) 0.036(2) Uani 1 1 d . . . H43A H 0.2783 0.0767 -0.0896 0.043 Uiso 1 1 calc R . . C42 C 0.5126(9) 0.2248(7) 0.0059(6) 0.050(3) Uani 1 1 d . . . H42A H 0.5880 0.2306 0.0418 0.059 Uiso 1 1 calc R . . C17 C 1.5363(8) -0.1391(6) 0.2385(5) 0.0356(19) Uani 1 1 d . . . H17A H 1.6014 -0.0851 0.2642 0.043 Uiso 1 1 calc R . . H17B H 1.5156 -0.1482 0.1793 0.043 Uiso 1 1 calc R . . C25 C 0.2647(8) 0.3422(6) 0.2258(6) 0.040(2) Uani 1 1 d . . . C40 C 0.3697(7) 0.3006(6) -0.0643(5) 0.0281(17) Uani 1 1 d . . . C21 C 1.7245(8) -0.3077(7) 0.3224(6) 0.044(2) Uani 1 1 d . . . H21A H 1.8008 -0.3035 0.3566 0.052 Uiso 1 1 calc R . . C15 C 1.3149(8) -0.1429(6) 0.2204(5) 0.0339(19) Uani 1 1 d . . . C11 C 1.1211(8) -0.0973(6) 0.2525(5) 0.0305(18) Uani 1 1 d . . . H11A H 1.0699 -0.1323 0.2014 0.037 Uiso 1 1 calc R . . C29 C 0.0826(8) 0.2010(7) 0.0521(6) 0.045(2) Uani 1 1 d . . . C10 C 1.0833(8) 0.0578(6) 0.4406(5) 0.0329(19) Uani 1 1 d . . . C41 C 0.4813(9) 0.3055(6) -0.0134(6) 0.042(2) Uani 1 1 d . . . H41A H 0.5348 0.3631 0.0076 0.051 Uiso 1 1 calc R . . C46 C 0.4172(13) 0.2828(10) 0.4566(8) 0.075(4) Uani 1 1 d . . . H07D H 0.3619 0.3276 0.4464 0.090 Uiso 1 1 calc R . . C31 C 0.0189(7) 0.0576(7) 0.0781(5) 0.039(2) Uani 1 1 d . . . C6 C 0.8653(8) 0.0762(6) 0.4137(5) 0.0311(18) Uani 1 1 d . . . H6A H 0.8824 0.0884 0.4732 0.037 Uiso 1 1 calc R . . H6B H 0.7959 0.0257 0.3886 0.037 Uiso 1 1 calc R . . C28 C 0.1300(9) 0.3141(8) 0.1941(7) 0.052(3) Uani 1 1 d . . . H28A H 0.0978 0.3157 0.2408 0.063 Uiso 1 1 calc R . . H28B H 0.0981 0.3615 0.1680 0.063 Uiso 1 1 calc R . . C1 C 0.6902(9) 0.2625(7) 0.3563(8) 0.054(3) Uani 1 1 d . . . H1A H 0.6102 0.2698 0.3448 0.064 Uiso 1 1 calc R . . C32 C 0.0527(8) 0.1372(7) 0.1570(6) 0.044(2) Uani 1 1 d . . . C45 C 0.7304(14) 0.1358(9) 0.1675(7) 0.086(5) Uani 1 1 d . . . H45A H 0.8127 0.1637 0.1782 0.129 Uiso 1 1 calc R . . H45B H 0.7252 0.0917 0.2000 0.129 Uiso 1 1 calc R . . H45C H 0.6852 0.1857 0.1819 0.129 Uiso 1 1 calc R . . O1 O 0.8670(5) -0.0484(4) 0.2548(4) 0.0396(14) Uani 1 1 d . . . O9 O 0.8677(6) 0.4802(5) 0.2595(5) 0.0554(18) Uani 1 1 d . . . O4 O 1.5371(6) -0.0238(5) 0.4001(4) 0.0425(15) Uani 1 1 d . . . O5 O 0.1055(6) 0.2607(5) 0.0174(4) 0.0510(17) Uani 1 1 d . . . O3 O 1.2829(6) -0.1952(5) 0.1494(4) 0.0456(16) Uani 1 1 d . . . O2 O 1.1103(6) 0.1048(4) 0.5131(4) 0.0394(14) Uani 1 1 d . . . O8 O 0.0757(6) 0.3262(5) -0.1741(4) 0.0411(15) Uani 1 1 d . . . O12 O 0.8601(6) 0.5712(6) 0.4455(5) 0.0550(18) Uani 1 1 d . . . O13 O 0.6839(6) 0.5358(5) 0.4617(4) 0.0530(18) Uani 1 1 d . . . O14 O 0.8252(7) 0.6331(6) 0.5629(5) 0.066(2) Uani 1 1 d . . . O6 O 0.0460(6) 0.1339(5) 0.2238(4) 0.0514(17) Uani 1 1 d . . . O18 O 0.6852(8) 0.0881(5) 0.0857(5) 0.065(2) Uani 1 1 d . . . H18 H 0.7420 0.0913 0.0567 0.078 Uiso 1 1 calc R . . O11 O 0.8656(8) 0.4064(6) 0.1329(5) 0.067(2) Uani 1 1 d . . . O10 O 0.7060(6) 0.3967(6) 0.1754(4) 0.0543(18) Uani 1 1 d . . . O7 O 0.3364(5) 0.5232(5) 0.0635(4) 0.0441(16) Uani 1 1 d . . . OW1 O 0.8161(9) 0.2087(7) 0.0230(6) 0.079(2) Uiso 1 1 d . . . HW1A H 0.8695 0.1651 0.0380 0.095 Uiso 1 1 calc R . . HW1B H 0.8482 0.2740 0.0569 0.095 Uiso 1 1 calc R . . N9 N 0.7904(7) 0.5818(6) 0.4915(5) 0.046(2) Uani 1 1 d . . . N5 N 0.5085(6) 0.4014(5) 0.2848(5) 0.0352(16) Uani 1 1 d . . . N3 N 1.6530(6) -0.3954(5) 0.2917(4) 0.0304(15) Uani 1 1 d . . . N2 N 0.9670(6) 0.0412(5) 0.3885(4) 0.0310(15) Uani 1 1 d . . . N8 N 0.2294(6) 0.4170(5) -0.0620(4) 0.0292(15) Uani 1 1 d . . . N1 N 0.7700(6) 0.3342(5) 0.3545(5) 0.0341(16) Uani 1 1 d . . . N7 N 0.4435(6) 0.1365(5) -0.0226(5) 0.0337(16) Uani 1 1 d . . . N4 N 1.4330(6) -0.1169(5) 0.2682(4) 0.0304(15) Uani 1 1 d . . . N6 N 0.0889(7) 0.2189(6) 0.1348(5) 0.0423(18) Uani 1 1 d . . . N10 N 0.8104(8) 0.4272(6) 0.1877(6) 0.051(2) Uani 1 1 d . . . Cd2 Cd 0.5000 0.0000 0.0000 0.0356(2) Uani 1 2 d S . . Cd1 Cd 0.71109(5) 0.46920(4) 0.32596(4) 0.0356(2) Uani 1 1 d . . . N11 N 0.3677(17) 0.0367(13) 0.1333(11) 0.122(2) Uiso 1 1 d . . . O15 O 0.4723(11) 0.0311(11) 0.1422(8) 0.122(2) Uiso 1 1 d D . . O16 O 0.3191(12) 0.0508(10) 0.1916(8) 0.122(2) Uiso 1 1 d D . . O17 O 0.3053(12) 0.0207(10) 0.0634(8) 0.122(2) Uiso 1 1 d 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 Cl6 0.0750(18) 0.0429(13) 0.0494(13) 0.0114(11) 0.0103(12) 0.0156(12) Cl5 0.0655(17) 0.0673(16) 0.0680(16) 0.0429(14) 0.0266(13) 0.0275(13) Cl4 0.0508(14) 0.0724(17) 0.0531(14) 0.0269(13) 0.0174(11) 0.0067(12) Cl3 0.0694(18) 0.0588(16) 0.0644(16) 0.0188(13) 0.0206(14) 0.0038(13) Cl2 0.084(3) 0.127(4) 0.081(2) -0.016(2) 0.014(2) -0.003(2) Cl1 0.424(12) 0.067(3) 0.119(4) 0.011(2) 0.163(6) -0.012(4) C8 0.033(4) 0.022(4) 0.035(4) 0.013(3) 0.005(4) 0.009(3) C18 0.035(4) 0.031(4) 0.025(4) 0.009(3) 0.008(3) 0.010(4) C5 0.033(5) 0.026(4) 0.043(5) 0.016(4) 0.004(4) -0.002(3) C35 0.028(4) 0.025(4) 0.027(4) 0.004(3) 0.006(3) 0.004(3) C44 0.023(4) 0.034(5) 0.046(5) 0.011(4) 0.002(4) 0.011(4) C7 0.036(5) 0.022(4) 0.030(4) 0.008(3) 0.004(4) 0.006(3) C37 0.036(5) 0.029(4) 0.026(4) 0.007(4) 0.009(3) 0.012(4) C38 0.032(5) 0.024(4) 0.031(4) 0.008(3) 0.007(4) 0.006(3) C39 0.033(5) 0.031(4) 0.037(4) 0.012(4) 0.012(4) 0.007(4) C30 0.029(4) 0.043(5) 0.044(5) 0.022(4) 0.005(4) 0.001(4) C19 0.026(4) 0.030(4) 0.034(4) 0.012(3) 0.002(3) 0.012(3) C3 0.031(4) 0.027(4) 0.029(4) 0.008(3) 0.000(3) 0.002(3) C16 0.032(5) 0.028(4) 0.033(4) 0.009(4) 0.002(4) 0.007(4) C13 0.037(5) 0.025(4) 0.029(4) 0.007(3) 0.005(4) 0.009(3) C9 0.035(5) 0.023(4) 0.031(4) 0.008(3) 0.006(4) 0.005(3) C14 0.036(5) 0.038(5) 0.028(4) 0.007(4) 0.000(4) 0.006(4) C20 0.032(4) 0.023(4) 0.039(5) 0.008(3) 0.009(4) 0.008(3) C23 0.032(5) 0.033(5) 0.057(6) 0.001(4) 0.013(4) 0.000(4) C4 0.029(4) 0.034(5) 0.048(5) 0.017(4) 0.006(4) 0.003(4) C47 0.034(5) 0.041(5) 0.039(5) 0.011(4) 0.002(4) 0.003(4) C34 0.028(4) 0.029(4) 0.033(4) 0.002(3) -0.001(3) 0.002(3) C12 0.037(5) 0.027(4) 0.032(4) 0.012(3) 0.008(4) 0.011(4) C26 0.044(5) 0.038(5) 0.047(5) 0.012(4) 0.017(4) 0.010(4) C33 0.035(5) 0.051(6) 0.040(5) 0.022(4) 0.003(4) 0.001(4) C27 0.037(5) 0.035(5) 0.048(5) 0.012(4) 0.011(4) 0.013(4) C36 0.032(5) 0.026(4) 0.035(4) 0.007(4) 0.006(4) 0.005(4) C22 0.036(5) 0.033(5) 0.041(5) 0.012(4) -0.006(4) -0.005(4) C2 0.032(5) 0.033(5) 0.079(7) 0.026(5) 0.015(5) 0.007(4) C24 0.034(5) 0.040(5) 0.048(5) -0.003(4) 0.005(4) 0.007(4) C43 0.027(4) 0.025(4) 0.058(6) 0.013(4) 0.011(4) 0.007(3) C42 0.043(6) 0.033(5) 0.056(6) 0.016(4) -0.016(5) -0.004(4) C17 0.042(5) 0.032(4) 0.038(5) 0.017(4) 0.014(4) 0.008(4) C25 0.029(5) 0.036(5) 0.051(5) 0.013(4) 0.004(4) -0.001(4) C40 0.030(4) 0.030(4) 0.026(4) 0.008(3) 0.009(3) 0.006(3) C21 0.031(5) 0.034(5) 0.057(6) 0.024(4) -0.013(4) -0.002(4) C15 0.042(5) 0.027(4) 0.029(5) 0.008(4) 0.003(4) 0.012(4) C11 0.034(5) 0.023(4) 0.026(4) 0.005(3) -0.004(3) 0.003(3) C29 0.035(5) 0.047(6) 0.057(6) 0.023(5) 0.011(4) 0.000(4) C10 0.034(5) 0.030(4) 0.030(5) 0.010(4) 0.002(4) 0.003(4) C41 0.041(5) 0.027(5) 0.048(5) 0.012(4) -0.005(4) -0.003(4) C46 0.077(9) 0.073(8) 0.075(8) 0.023(7) 0.025(7) 0.004(7) C31 0.020(4) 0.057(6) 0.039(5) 0.019(4) 0.002(3) 0.003(4) C6 0.031(4) 0.026(4) 0.038(4) 0.013(4) 0.009(4) 0.004(3) C28 0.032(5) 0.052(6) 0.063(6) 0.000(5) 0.013(5) -0.003(4) C1 0.031(5) 0.036(5) 0.098(8) 0.036(6) 0.010(5) 0.004(4) C32 0.026(5) 0.058(6) 0.047(6) 0.019(5) 0.009(4) 0.001(4) C45 0.100(11) 0.059(7) 0.054(7) -0.011(6) -0.038(7) 0.026(7) O1 0.029(3) 0.037(3) 0.042(3) 0.005(3) -0.002(3) 0.001(3) O9 0.038(4) 0.055(4) 0.072(5) 0.025(4) 0.011(4) -0.004(3) O4 0.035(4) 0.043(4) 0.041(3) 0.008(3) -0.001(3) 0.007(3) O5 0.045(4) 0.047(4) 0.064(4) 0.027(3) 0.012(3) 0.004(3) O3 0.051(4) 0.049(4) 0.029(3) 0.001(3) 0.004(3) 0.015(3) O2 0.038(3) 0.042(3) 0.032(3) 0.002(3) 0.002(3) 0.015(3) O8 0.040(3) 0.045(4) 0.031(3) -0.003(3) 0.006(3) 0.017(3) O12 0.040(4) 0.060(4) 0.057(4) 0.020(4) 0.000(3) -0.004(3) O13 0.043(4) 0.052(4) 0.048(4) 0.008(3) -0.001(3) -0.014(3) O14 0.055(5) 0.078(5) 0.048(4) 0.010(4) 0.003(4) -0.022(4) O6 0.042(4) 0.066(5) 0.044(4) 0.015(3) 0.009(3) 0.008(3) O18 0.068(5) 0.047(4) 0.059(5) 0.007(4) -0.015(4) 0.014(4) O11 0.065(5) 0.079(6) 0.072(5) 0.031(4) 0.033(4) 0.015(4) O10 0.039(4) 0.071(5) 0.050(4) 0.013(4) 0.013(3) 0.005(4) O7 0.026(3) 0.042(4) 0.050(4) -0.006(3) 0.003(3) 0.005(3) N9 0.040(5) 0.042(4) 0.045(5) 0.017(4) -0.009(4) -0.008(4) N5 0.022(3) 0.032(4) 0.050(4) 0.016(3) 0.003(3) 0.005(3) N3 0.026(4) 0.021(3) 0.039(4) 0.003(3) 0.004(3) 0.010(3) N2 0.029(4) 0.027(3) 0.039(4) 0.012(3) 0.006(3) 0.010(3) N8 0.023(3) 0.028(3) 0.037(4) 0.008(3) 0.007(3) 0.009(3) N1 0.022(4) 0.030(4) 0.048(4) 0.007(3) 0.008(3) 0.006(3) N7 0.024(4) 0.032(4) 0.045(4) 0.010(3) 0.007(3) 0.009(3) N4 0.028(4) 0.033(4) 0.031(4) 0.010(3) 0.004(3) 0.015(3) N6 0.029(4) 0.046(4) 0.046(4) 0.011(4) 0.004(3) 0.000(3) N10 0.048(5) 0.048(5) 0.057(5) 0.022(4) 0.012(4) 0.000(4) Cd2 0.0302(4) 0.0263(3) 0.0481(4) 0.0157(2) 0.0018(2) 0.0048(2) Cd1 0.0302(4) 0.0263(3) 0.0481(4) 0.0157(2) 0.0018(2) 0.0048(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl6 C47 1.759(10) . ? Cl5 C47 1.747(9) . ? Cl4 C47 1.772(9) . ? Cl3 C46 1.711(14) . ? Cl2 C46 1.745(14) . ? Cl1 C46 1.697(14) . ? C8 C11 1.384(12) . ? C8 C9 1.385(12) . ? C8 C7 1.487(12) . ? C18 C19 1.371(12) . ? C18 C22 1.384(13) . ? C18 C17 1.515(12) . ? C5 N1 1.335(12) . ? C5 C4 1.383(13) . ? C5 H5A 0.9300 . ? C35 C38 1.379(12) . ? C35 C34 1.400(12) . ? C35 C36 1.481(12) . ? C44 C43 1.374(13) . ? C44 C40 1.379(12) . ? C44 H44A 0.9300 . ? C7 O1 1.208(10) . ? C7 N2 1.400(11) . ? C37 O8 1.231(10) . ? C37 N8 1.386(11) . ? C37 C38 1.482(11) . ? C38 C34 1.372(12) 2_565 ? C39 N8 1.459(11) . ? C39 C40 1.496(12) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C30 C33 1.377(13) . ? C30 C31 1.392(12) . ? C30 C29 1.504(14) . ? C19 C20 1.382(12) . ? C19 H19A 0.9300 . ? C3 C2 1.359(13) . ? C3 C4 1.378(12) . ? C3 C6 1.504(12) . ? C16 O4 1.204(11) . ? C16 N4 1.413(11) . ? C16 C13 1.491(12) . ? C13 C14 1.393(12) . ? C13 C12 1.396(12) . ? C9 C14 1.395(13) . ? C9 C10 1.456(12) . ? C14 H14A 0.9300 . ? C20 N3 1.360(11) . ? C20 H20A 0.9300 . ? C23 N5 1.334(12) . ? C23 C24 1.355(13) . ? C23 H23A 0.9300 . ? C4 H4A 0.9300 . ? C47 H05E 0.9800 . ? C34 C38 1.372(12) 2_565 ? C34 H34 0.9300 . ? C12 C11 1.363(12) . ? C12 C15 1.481(12) . ? C26 C25 1.363(13) . ? C26 C27 1.372(14) . ? C26 H26A 0.9300 . ? C33 C31 1.381(14) 2 ? C33 H33A 0.9300 . ? C27 N5 1.343(12) . ? C27 H27A 0.9300 . ? C36 O7 1.200(11) . ? C36 N8 1.400(11) . ? C22 C21 1.357(13) . ? C22 H22A 0.9300 . ? C2 C1 1.368(14) . ? C2 H2A 0.9300 . ? C24 C25 1.393(14) . ? C24 H24A 0.9300 . ? C43 N7 1.359(12) . ? C43 H43A 0.9300 . ? C42 C41 1.358(14) . ? C42 N7 1.356(12) . ? C42 H42A 0.9300 . ? C17 N4 1.459(11) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C25 C28 1.513(13) . ? C40 C41 1.370(13) . ? C21 N3 1.360(11) . ? C21 H21A 0.9300 . ? C15 O3 1.224(10) . ? C15 N4 1.385(11) . ? C11 H11A 0.9300 . ? C29 O5 1.214(12) . ? C29 N6 1.378(13) . ? C10 O2 1.222(10) . ? C10 N2 1.398(11) . ? C41 H41A 0.9300 . ? C46 H07D 0.9800 . ? C31 C33 1.381(14) 2 ? C31 C32 1.498(14) . ? C6 N2 1.459(11) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C28 N6 1.464(13) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C1 N1 1.341(12) . ? C1 H1A 0.9300 . ? C32 O6 1.193(11) . ? C32 N6 1.395(13) . ? C45 O18 1.363(13) . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? O9 N10 1.271(11) . ? O9 Cd1 2.403(7) . ? O12 N9 1.269(12) . ? O12 Cd1 2.401(7) . ? O13 N9 1.271(10) . ? O13 Cd1 2.430(7) . ? O14 N9 1.226(11) . ? O18 Cd2 2.343(8) . ? O18 H18 0.9300 . ? O11 N10 1.271(12) . ? O10 N10 1.205(11) . ? O10 Cd1 2.553(7) . ? OW1 HW1A 0.9700 . ? OW1 HW1B 0.9700 . ? N5 Cd1 2.336(7) . ? N3 Cd1 2.312(7) 1_645 ? N1 Cd1 2.272(7) . ? N7 Cd2 2.248(7) . ? Cd2 N7 2.248(7) 2_655 ? Cd2 O18 2.343(8) 2_655 ? Cd2 O15 2.507(13) . ? Cd2 O15 2.507(13) 2_655 ? Cd1 N3 2.312(7) 1_465 ? N11 O15 1.21(2) . ? N11 O17 1.206(19) . ? N11 O16 1.261(19) . ? 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 C11 C8 C9 123.2(8) . . ? C11 C8 C7 129.2(8) . . ? C9 C8 C7 107.5(7) . . ? C19 C18 C22 117.5(8) . . ? C19 C18 C17 120.6(8) . . ? C22 C18 C17 121.9(8) . . ? N1 C5 C4 123.6(8) . . ? N1 C5 H5A 118.2 . . ? C4 C5 H5A 118.2 . . ? C38 C35 C34 121.9(8) . . ? C38 C35 C36 109.2(7) . . ? C34 C35 C36 128.9(7) . . ? C43 C44 C40 120.3(8) . . ? C43 C44 H44A 119.8 . . ? C40 C44 H44A 119.8 . . ? O1 C7 N2 124.9(8) . . ? O1 C7 C8 129.3(8) . . ? N2 C7 C8 105.7(7) . . ? O8 C37 N8 123.7(7) . . ? O8 C37 C38 129.6(8) . . ? N8 C37 C38 106.7(7) . . ? C34 C38 C35 124.0(8) 2_565 . ? C34 C38 C37 128.7(8) 2_565 . ? C35 C38 C37 107.2(7) . . ? N8 C39 C40 113.7(7) . . ? N8 C39 H39A 108.8 . . ? C40 C39 H39A 108.8 . . ? N8 C39 H39B 108.8 . . ? C40 C39 H39B 108.8 . . ? H39A C39 H39B 107.7 . . ? C33 C30 C31 123.1(9) . . ? C33 C30 C29 129.8(8) . . ? C31 C30 C29 107.1(8) . . ? C18 C19 C20 120.3(8) . . ? C18 C19 H19A 119.9 . . ? C20 C19 H19A 119.9 . . ? C2 C3 C4 117.2(8) . . ? C2 C3 C6 119.8(8) . . ? C4 C3 C6 123.0(8) . . ? O4 C16 N4 124.2(8) . . ? O4 C16 C13 130.5(8) . . ? N4 C16 C13 105.2(7) . . ? C14 C13 C12 122.0(8) . . ? C14 C13 C16 129.6(8) . . ? C12 C13 C16 108.4(7) . . ? C8 C9 C14 121.4(8) . . ? C8 C9 C10 109.0(8) . . ? C14 C9 C10 129.6(8) . . ? C13 C14 C9 115.2(8) . . ? C13 C14 H14A 122.4 . . ? C9 C14 H14A 122.4 . . ? N3 C20 C19 122.9(8) . . ? N3 C20 H20A 118.5 . . ? C19 C20 H20A 118.5 . . ? N5 C23 C24 123.2(9) . . ? N5 C23 H23A 118.4 . . ? C24 C23 H23A 118.4 . . ? C3 C4 C5 119.8(8) . . ? C3 C4 H4A 120.1 . . ? C5 C4 H4A 120.1 . . ? Cl5 C47 Cl6 110.3(5) . . ? Cl5 C47 Cl4 110.8(5) . . ? Cl6 C47 Cl4 110.2(5) . . ? Cl5 C47 H05E 108.5 . . ? Cl6 C47 H05E 108.5 . . ? Cl4 C47 H05E 108.5 . . ? C38 C34 C35 114.1(8) 2_565 . ? C38 C34 H34 122.9 2_565 . ? C35 C34 H34 122.9 . . ? C11 C12 C13 122.6(8) . . ? C11 C12 C15 129.6(8) . . ? C13 C12 C15 107.7(8) . . ? C25 C26 C27 119.8(9) . . ? C25 C26 H26A 120.1 . . ? C27 C26 H26A 120.1 . . ? C30 C33 C31 115.1(8) . 2 ? C30 C33 H33A 122.4 . . ? C31 C33 H33A 122.4 2 . ? N5 C27 C26 121.5(9) . . ? N5 C27 H27A 119.2 . . ? C26 C27 H27A 119.2 . . ? O7 C36 N8 125.3(8) . . ? O7 C36 C35 129.5(8) . . ? N8 C36 C35 105.2(7) . . ? C21 C22 C18 119.8(8) . . ? C21 C22 H22A 120.1 . . ? C18 C22 H22A 120.1 . . ? C3 C2 C1 119.7(9) . . ? C3 C2 H2A 120.1 . . ? C1 C2 H2A 120.1 . . ? C23 C24 C25 118.5(9) . . ? C23 C24 H24A 120.7 . . ? C25 C24 H24A 120.7 . . ? N7 C43 C44 123.3(8) . . ? N7 C43 H43A 118.4 . . ? C44 C43 H43A 118.4 . . ? C41 C42 N7 125.8(9) . . ? C41 C42 H42A 117.1 . . ? N7 C42 H42A 117.1 . . ? N4 C17 C18 112.4(7) . . ? N4 C17 H17A 109.1 . . ? C18 C17 H17A 109.1 . . ? N4 C17 H17B 109.1 . . ? C18 C17 H17B 109.1 . . ? H17A C17 H17B 107.9 . . ? C26 C25 C24 118.6(8) . . ? C26 C25 C28 118.9(9) . . ? C24 C25 C28 122.4(9) . . ? C41 C40 C44 117.6(8) . . ? C41 C40 C39 122.1(8) . . ? C44 C40 C39 120.3(8) . . ? C22 C21 N3 124.3(8) . . ? C22 C21 H21A 117.9 . . ? N3 C21 H21A 117.9 . . ? O3 C15 N4 124.0(8) . . ? O3 C15 C12 129.1(8) . . ? N4 C15 C12 106.8(7) . . ? C12 C11 C8 115.4(7) . . ? C12 C11 H11A 122.3 . . ? C8 C11 H11A 122.3 . . ? O5 C29 N6 125.9(9) . . ? O5 C29 C30 128.3(9) . . ? N6 C29 C30 105.8(8) . . ? O2 C10 N2 122.6(8) . . ? O2 C10 C9 131.1(8) . . ? N2 C10 C9 106.4(7) . . ? C42 C41 C40 119.0(8) . . ? C42 C41 H41A 120.5 . . ? C40 C41 H41A 120.5 . . ? Cl1 C46 Cl3 113.8(8) . . ? Cl1 C46 Cl2 112.7(9) . . ? Cl3 C46 Cl2 114.1(8) . . ? Cl1 C46 H07D 105.0 . . ? Cl3 C46 H07D 105.0 . . ? Cl2 C46 H07D 105.0 . . ? C33 C31 C30 121.8(9) 2 . ? C33 C31 C32 129.3(8) 2 . ? C30 C31 C32 108.8(8) . . ? N2 C6 C3 115.4(7) . . ? N2 C6 H6A 108.4 . . ? C3 C6 H6A 108.4 . . ? N2 C6 H6B 108.4 . . ? C3 C6 H6B 108.4 . . ? H6A C6 H6B 107.5 . . ? N6 C28 C25 114.1(8) . . ? N6 C28 H28A 108.7 . . ? C25 C28 H28A 108.7 . . ? N6 C28 H28B 108.7 . . ? C25 C28 H28B 108.7 . . ? H28A C28 H28B 107.6 . . ? N1 C1 C2 124.7(9) . . ? N1 C1 H1A 117.6 . . ? C2 C1 H1A 117.6 . . ? O6 C32 N6 126.7(10) . . ? O6 C32 C31 128.6(9) . . ? N6 C32 C31 104.6(8) . . ? O18 C45 H45A 109.5 . . ? O18 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? O18 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? N10 O9 Cd1 98.3(5) . . ? N9 O12 Cd1 95.0(5) . . ? N9 O13 Cd1 93.6(6) . . ? C45 O18 Cd2 135.8(10) . . ? C45 O18 H18 112.1 . . ? Cd2 O18 H18 112.1 . . ? N10 O10 Cd1 92.8(6) . . ? HW1A OW1 HW1B 110.8 . . ? O14 N9 O12 121.1(8) . . ? O14 N9 O13 121.1(9) . . ? O12 N9 O13 117.8(8) . . ? C23 N5 C27 118.3(8) . . ? C23 N5 Cd1 121.5(6) . . ? C27 N5 Cd1 119.4(6) . . ? C20 N3 C21 115.2(7) . . ? C20 N3 Cd1 122.1(5) . 1_645 ? C21 N3 Cd1 122.6(5) . 1_645 ? C10 N2 C7 111.2(7) . . ? C10 N2 C6 124.6(7) . . ? C7 N2 C6 123.9(7) . . ? C37 N8 C36 111.7(7) . . ? C37 N8 C39 125.0(7) . . ? C36 N8 C39 123.3(7) . . ? C5 N1 C1 115.0(8) . . ? C5 N1 Cd1 124.1(5) . . ? C1 N1 Cd1 120.9(6) . . ? C42 N7 C43 114.0(8) . . ? C42 N7 Cd2 126.0(6) . . ? C43 N7 Cd2 119.9(6) . . ? C15 N4 C16 111.9(7) . . ? C15 N4 C17 124.9(7) . . ? C16 N4 C17 123.0(7) . . ? C29 N6 C32 113.5(8) . . ? C29 N6 C28 123.5(8) . . ? C32 N6 C28 123.0(9) . . ? O10 N10 O9 118.1(9) . . ? O10 N10 O11 122.7(9) . . ? O9 N10 O11 119.2(9) . . ? N7 Cd2 N7 180.0(6) 2_655 . ? N7 Cd2 O18 90.4(3) 2_655 . ? N7 Cd2 O18 89.6(3) . . ? N7 Cd2 O18 89.6(3) 2_655 2_655 ? N7 Cd2 O18 90.4(3) . 2_655 ? O18 Cd2 O18 180.0(7) . 2_655 ? N7 Cd2 O15 84.4(4) 2_655 . ? N7 Cd2 O15 95.6(4) . . ? O18 Cd2 O15 76.5(4) . . ? O18 Cd2 O15 103.5(4) 2_655 . ? N7 Cd2 O15 95.6(4) 2_655 2_655 ? N7 Cd2 O15 84.4(4) . 2_655 ? O18 Cd2 O15 103.5(4) . 2_655 ? O18 Cd2 O15 76.5(4) 2_655 2_655 ? O15 Cd2 O15 180.0(5) . 2_655 ? N1 Cd1 N3 177.6(2) . 1_465 ? N1 Cd1 N5 92.7(2) . . ? N3 Cd1 N5 87.7(2) 1_465 . ? N1 Cd1 O12 92.1(3) . . ? N3 Cd1 O12 89.1(3) 1_465 . ? N5 Cd1 O12 139.9(3) . . ? N1 Cd1 O9 88.7(3) . . ? N3 Cd1 O9 89.4(3) 1_465 . ? N5 Cd1 O9 136.2(3) . . ? O12 Cd1 O9 83.7(3) . . ? N1 Cd1 O13 94.5(3) . . ? N3 Cd1 O13 87.9(2) 1_465 . ? N5 Cd1 O13 86.4(2) . . ? O12 Cd1 O13 53.5(2) . . ? O9 Cd1 O13 137.1(2) . . ? N1 Cd1 O10 88.8(3) . . ? N3 Cd1 O10 88.9(3) 1_465 . ? N5 Cd1 O10 85.6(2) . . ? O12 Cd1 O10 134.3(2) . . ? O9 Cd1 O10 50.6(2) . . ? O13 Cd1 O10 171.5(2) . . ? O15 N11 O17 117.1(18) . . ? O15 N11 O16 124.0(18) . . ? O17 N11 O16 118.7(18) . . ? N11 O15 Cd2 105.3(12) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C11 C8 C7 O1 2.5(15) . . . . ? C9 C8 C7 O1 -179.6(8) . . . . ? C11 C8 C7 N2 -179.0(8) . . . . ? C9 C8 C7 N2 -1.0(9) . . . . ? C34 C35 C38 C34 -0.7(15) . . . 2_565 ? C36 C35 C38 C34 -179.0(8) . . . 2_565 ? C34 C35 C38 C37 177.0(8) . . . . ? C36 C35 C38 C37 -1.3(9) . . . . ? O8 C37 C38 C34 -1.9(15) . . . 2_565 ? N8 C37 C38 C34 178.2(8) . . . 2_565 ? O8 C37 C38 C35 -179.4(9) . . . . ? N8 C37 C38 C35 0.7(9) . . . . ? C22 C18 C19 C20 1.2(12) . . . . ? C17 C18 C19 C20 -179.8(7) . . . . ? O4 C16 C13 C14 -0.3(15) . . . . ? N4 C16 C13 C14 -178.6(8) . . . . ? O4 C16 C13 C12 176.8(9) . . . . ? N4 C16 C13 C12 -1.4(9) . . . . ? C11 C8 C9 C14 -0.1(12) . . . . ? C7 C8 C9 C14 -178.2(7) . . . . ? C11 C8 C9 C10 -179.0(7) . . . . ? C7 C8 C9 C10 2.9(9) . . . . ? C12 C13 C14 C9 -3.8(12) . . . . ? C16 C13 C14 C9 173.0(8) . . . . ? C8 C9 C14 C13 3.2(12) . . . . ? C10 C9 C14 C13 -178.1(8) . . . . ? C18 C19 C20 N3 -0.1(13) . . . . ? C2 C3 C4 C5 1.7(13) . . . . ? C6 C3 C4 C5 -177.0(8) . . . . ? N1 C5 C4 C3 -1.9(14) . . . . ? C38 C35 C34 C38 0.6(13) . . . 2_565 ? C36 C35 C34 C38 178.5(8) . . . 2_565 ? C14 C13 C12 C11 1.1(13) . . . . ? C16 C13 C12 C11 -176.3(8) . . . . ? C14 C13 C12 C15 179.0(8) . . . . ? C16 C13 C12 C15 1.6(9) . . . . ? C31 C30 C33 C31 -0.6(14) . . . 2 ? C29 C30 C33 C31 -179.5(9) . . . 2 ? C25 C26 C27 N5 0.6(14) . . . . ? C38 C35 C36 O7 -179.1(9) . . . . ? C34 C35 C36 O7 2.7(16) . . . . ? C38 C35 C36 N8 1.4(9) . . . . ? C34 C35 C36 N8 -176.7(8) . . . . ? C19 C18 C22 C21 -1.9(13) . . . . ? C17 C18 C22 C21 179.1(9) . . . . ? C4 C3 C2 C1 -1.0(15) . . . . ? C6 C3 C2 C1 177.7(10) . . . . ? N5 C23 C24 C25 -0.4(16) . . . . ? C40 C44 C43 N7 -2.2(14) . . . . ? C19 C18 C17 N4 61.5(10) . . . . ? C22 C18 C17 N4 -119.5(9) . . . . ? C27 C26 C25 C24 -1.2(14) . . . . ? C27 C26 C25 C28 -178.3(9) . . . . ? C23 C24 C25 C26 1.0(15) . . . . ? C23 C24 C25 C28 178.0(10) . . . . ? C43 C44 C40 C41 0.0(13) . . . . ? C43 C44 C40 C39 178.2(8) . . . . ? N8 C39 C40 C41 -117.0(9) . . . . ? N8 C39 C40 C44 64.9(10) . . . . ? C18 C22 C21 N3 1.7(16) . . . . ? C11 C12 C15 O3 -4.7(15) . . . . ? C13 C12 C15 O3 177.6(9) . . . . ? C11 C12 C15 N4 176.5(8) . . . . ? C13 C12 C15 N4 -1.3(9) . . . . ? C13 C12 C11 C8 2.1(12) . . . . ? C15 C12 C11 C8 -175.3(8) . . . . ? C9 C8 C11 C12 -2.7(12) . . . . ? C7 C8 C11 C12 175.0(8) . . . . ? C33 C30 C29 O5 2.9(17) . . . . ? C31 C30 C29 O5 -176.2(10) . . . . ? C33 C30 C29 N6 -178.2(9) . . . . ? C31 C30 C29 N6 2.8(10) . . . . ? C8 C9 C10 O2 175.3(9) . . . . ? C14 C9 C10 O2 -3.5(15) . . . . ? C8 C9 C10 N2 -3.7(9) . . . . ? C14 C9 C10 N2 177.5(8) . . . . ? N7 C42 C41 C40 1.8(17) . . . . ? C44 C40 C41 C42 0.2(14) . . . . ? C39 C40 C41 C42 -178.0(9) . . . . ? C33 C30 C31 C33 0.6(15) . . . 2 ? C29 C30 C31 C33 179.8(8) . . . 2 ? C33 C30 C31 C32 177.9(8) . . . . ? C29 C30 C31 C32 -2.9(10) . . . . ? C2 C3 C6 N2 148.0(9) . . . . ? C4 C3 C6 N2 -33.3(12) . . . . ? C26 C25 C28 N6 -160.4(9) . . . . ? C24 C25 C28 N6 22.6(15) . . . . ? C3 C2 C1 N1 0.4(18) . . . . ? C33 C31 C32 O6 -3.9(16) 2 . . . ? C30 C31 C32 O6 179.0(10) . . . . ? C33 C31 C32 N6 179.1(9) 2 . . . ? C30 C31 C32 N6 2.0(10) . . . . ? Cd1 O12 N9 O14 -178.0(8) . . . . ? Cd1 O12 N9 O13 3.4(9) . . . . ? Cd1 O13 N9 O14 178.0(8) . . . . ? Cd1 O13 N9 O12 -3.3(8) . . . . ? C24 C23 N5 C27 -0.1(14) . . . . ? C24 C23 N5 Cd1 -170.3(8) . . . . ? C26 C27 N5 C23 0.0(13) . . . . ? C26 C27 N5 Cd1 170.4(7) . . . . ? C19 C20 N3 C21 -0.2(12) . . . . ? C19 C20 N3 Cd1 176.6(6) . . . 1_645 ? C22 C21 N3 C20 -0.6(14) . . . . ? C22 C21 N3 Cd1 -177.4(8) . . . 1_645 ? O2 C10 N2 C7 -176.0(8) . . . . ? C9 C10 N2 C7 3.1(9) . . . . ? O2 C10 N2 C6 -0.8(13) . . . . ? C9 C10 N2 C6 178.3(7) . . . . ? O1 C7 N2 C10 177.3(8) . . . . ? C8 C7 N2 C10 -1.4(9) . . . . ? O1 C7 N2 C6 2.0(13) . . . . ? C8 C7 N2 C6 -176.6(7) . . . . ? C3 C6 N2 C10 99.1(9) . . . . ? C3 C6 N2 C7 -86.3(9) . . . . ? O8 C37 N8 C36 -179.7(8) . . . . ? C38 C37 N8 C36 0.2(9) . . . . ? O8 C37 N8 C39 2.8(13) . . . . ? C38 C37 N8 C39 -177.4(7) . . . . ? O7 C36 N8 C37 179.5(9) . . . . ? C35 C36 N8 C37 -0.9(9) . . . . ? O7 C36 N8 C39 -2.9(13) . . . . ? C35 C36 N8 C39 176.6(7) . . . . ? C40 C39 N8 C37 -92.2(10) . . . . ? C40 C39 N8 C36 90.5(9) . . . . ? C4 C5 N1 C1 1.2(14) . . . . ? C4 C5 N1 Cd1 179.9(7) . . . . ? C2 C1 N1 C5 -0.4(16) . . . . ? C2 C1 N1 Cd1 -179.3(9) . . . . ? C41 C42 N7 C43 -3.8(16) . . . . ? C41 C42 N7 Cd2 174.3(9) . . . . ? C44 C43 N7 C42 3.9(13) . . . . ? C44 C43 N7 Cd2 -174.3(7) . . . . ? O3 C15 N4 C16 -178.6(8) . . . . ? C12 C15 N4 C16 0.3(9) . . . . ? O3 C15 N4 C17 6.9(13) . . . . ? C12 C15 N4 C17 -174.2(7) . . . . ? O4 C16 N4 C15 -177.8(8) . . . . ? C13 C16 N4 C15 0.6(9) . . . . ? O4 C16 N4 C17 -3.1(13) . . . . ? C13 C16 N4 C17 175.3(7) . . . . ? C18 C17 N4 C15 -96.4(9) . . . . ? C18 C17 N4 C16 89.7(9) . . . . ? O5 C29 N6 C32 177.5(9) . . . . ? C30 C29 N6 C32 -1.5(10) . . . . ? O5 C29 N6 C28 -2.8(15) . . . . ? C30 C29 N6 C28 178.2(8) . . . . ? O6 C32 N6 C29 -177.3(9) . . . . ? C31 C32 N6 C29 -0.2(10) . . . . ? O6 C32 N6 C28 3.0(15) . . . . ? C31 C32 N6 C28 -179.9(8) . . . . ? C25 C28 N6 C29 -81.2(12) . . . . ? C25 C28 N6 C32 98.4(11) . . . . ? Cd1 O10 N10 O9 -3.9(9) . . . . ? Cd1 O10 N10 O11 174.1(9) . . . . ? Cd1 O9 N10 O10 4.2(10) . . . . ? Cd1 O9 N10 O11 -173.9(8) . . . . ? C42 N7 Cd2 N7 -43(78) . . . 2_655 ? C43 N7 Cd2 N7 135(78) . . . 2_655 ? C42 N7 Cd2 O18 3.8(8) . . . . ? C43 N7 Cd2 O18 -178.2(7) . . . . ? C42 N7 Cd2 O18 -176.2(8) . . . 2_655 ? C43 N7 Cd2 O18 1.8(7) . . . 2_655 ? C42 N7 Cd2 O15 80.2(9) . . . . ? C43 N7 Cd2 O15 -101.8(7) . . . . ? C42 N7 Cd2 O15 -99.8(9) . . . 2_655 ? C43 N7 Cd2 O15 78.2(7) . . . 2_655 ? C45 O18 Cd2 N7 -91.6(10) . . . 2_655 ? C45 O18 Cd2 N7 88.4(10) . . . . ? C45 O18 Cd2 O18 -80.2(11) . . . 2_655 ? C45 O18 Cd2 O15 -7.4(11) . . . . ? C45 O18 Cd2 O15 172.6(11) . . . 2_655 ? C5 N1 Cd1 N3 71(6) . . . 1_465 ? C1 N1 Cd1 N3 -110(6) . . . 1_465 ? C5 N1 Cd1 N5 170.6(7) . . . . ? C1 N1 Cd1 N5 -10.7(8) . . . . ? C5 N1 Cd1 O12 -49.2(7) . . . . ? C1 N1 Cd1 O12 129.5(8) . . . . ? C5 N1 Cd1 O9 34.4(7) . . . . ? C1 N1 Cd1 O9 -146.8(8) . . . . ? C5 N1 Cd1 O13 -102.8(7) . . . . ? C1 N1 Cd1 O13 76.0(8) . . . . ? C5 N1 Cd1 O10 85.1(7) . . . . ? C1 N1 Cd1 O10 -96.2(8) . . . . ? C23 N5 Cd1 N1 -71.3(7) . . . . ? C27 N5 Cd1 N1 118.7(7) . . . . ? C23 N5 Cd1 N3 106.4(7) . . . 1_465 ? C27 N5 Cd1 N3 -63.7(6) . . . 1_465 ? C23 N5 Cd1 O12 -167.8(6) . . . . ? C27 N5 Cd1 O12 22.2(8) . . . . ? C23 N5 Cd1 O9 19.7(8) . . . . ? C27 N5 Cd1 O9 -150.3(6) . . . . ? C23 N5 Cd1 O13 -165.6(7) . . . . ? C27 N5 Cd1 O13 24.4(6) . . . . ? C23 N5 Cd1 O10 17.3(7) . . . . ? C27 N5 Cd1 O10 -152.7(7) . . . . ? N9 O12 Cd1 N1 -96.0(6) . . . . ? N9 O12 Cd1 N3 86.1(5) . . . 1_465 ? N9 O12 Cd1 N5 0.8(7) . . . . ? N9 O12 Cd1 O9 175.5(6) . . . . ? N9 O12 Cd1 O13 -1.9(5) . . . . ? N9 O12 Cd1 O10 173.7(5) . . . . ? N10 O9 Cd1 N1 87.2(6) . . . . ? N10 O9 Cd1 N3 -91.4(6) . . . 1_465 ? N10 O9 Cd1 N5 -5.4(7) . . . . ? N10 O9 Cd1 O12 179.5(6) . . . . ? N10 O9 Cd1 O13 -177.5(5) . . . . ? N10 O9 Cd1 O10 -2.3(5) . . . . ? N9 O13 Cd1 N1 91.2(5) . . . . ? N9 O13 Cd1 N3 -88.5(5) . . . 1_465 ? N9 O13 Cd1 N5 -176.3(6) . . . . ? N9 O13 Cd1 O12 1.9(5) . . . . ? N9 O13 Cd1 O9 -1.8(7) . . . . ? N9 O13 Cd1 O10 -156.2(15) . . . . ? N10 O10 Cd1 N1 -87.0(6) . . . . ? N10 O10 Cd1 N3 92.5(6) . . . 1_465 ? N10 O10 Cd1 N5 -179.8(6) . . . . ? N10 O10 Cd1 O12 4.8(8) . . . . ? N10 O10 Cd1 O9 2.4(5) . . . . ? N10 O10 Cd1 O13 160.1(15) . . . . ? O17 N11 O15 Cd2 5(2) . . . . ? O16 N11 O15 Cd2 178.9(16) . . . . ? N7 Cd2 O15 N11 -119.7(13) 2_655 . . . ? N7 Cd2 O15 N11 60.3(13) . . . . ? O18 Cd2 O15 N11 148.5(14) . . . . ? O18 Cd2 O15 N11 -31.5(14) 2_655 . . . ? O15 Cd2 O15 N11 47(100) 2_655 . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 60.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.507 _refine_diff_density_min -1.751 _refine_diff_density_rms 0.180 # Attachment 'ok.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 803605' #TrackingRef 'ok.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C216 H136 Cd4 Cl24 N40 O56' _chemical_formula_weight 5488.05 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4(3) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y, x, z+3/4' 'y, -x, z+1/4' _cell_length_a 17.2841(5) _cell_length_b 17.2841(5) _cell_length_c 20.9702(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6264.6(6) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4843 _cell_measurement_theta_min 2.5490 _cell_measurement_theta_max 29.6852 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.455 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2760 _exptl_absorpt_coefficient_mu 0.673 _exptl_absorpt_correction_T_min 0.89453 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 16.0855 _diffrn_measurement_device_type Oxford _diffrn_measurement_method '\w and \p scan' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26471 _diffrn_reflns_av_R_equivalents 0.0690 _diffrn_reflns_av_sigmaI/netI 0.2046 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 26.50 _reflns_number_total 11760 _reflns_number_gt 5132 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0810P)^2^+20.0000P] 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 geom _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 0.28(4) _refine_ls_number_reflns 11760 _refine_ls_number_parameters 894 _refine_ls_number_restraints 1322 _refine_ls_R_factor_all 0.1953 _refine_ls_R_factor_gt 0.0984 _refine_ls_wR_factor_ref 0.2464 _refine_ls_wR_factor_gt 0.2102 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.001 _refine_ls_shift/su_max 0.073 _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 Cd1 Cd 1.19721(4) 0.75560(3) 0.00234(5) 0.06604(17) Uani 1 1 d . A 1 N2 N 0.7912(4) 0.6318(5) -0.0563(4) 0.085(2) Uani 1 1 d U A 1 N3 N 0.6555(5) 0.3098(5) -0.2258(5) 0.099(3) Uani 1 1 d U A 1 N6 N 1.1372(4) 1.1701(3) 0.0854(3) 0.0581(18) Uani 1 1 d U A 1 N7 N 0.8300(4) 1.3816(4) 0.2188(3) 0.067(2) Uani 1 1 d U A 1 O1 O 0.8017(4) 0.6982(4) -0.1505(4) 0.107(2) Uani 1 1 d U A 1 O2 O 0.7973(5) 0.5587(5) 0.0308(4) 0.117(3) Uani 1 1 d U A 1 O3 O 0.6603(4) 0.2377(4) -0.1352(4) 0.109(2) Uani 1 1 d U A 1 O4 O 0.6443(5) 0.3820(5) -0.3145(4) 0.130(3) Uani 1 1 d U A 1 O5 O 1.0733(4) 1.1588(4) -0.0059(3) 0.097(2) Uani 1 1 d U A 1 O6 O 1.2010(3) 1.1772(3) 0.1795(3) 0.0744(18) Uani 1 1 d U A 1 O7 O 0.7587(4) 1.3664(4) 0.1279(4) 0.096(2) Uani 1 1 d U A 1 O8 O 0.9023(4) 1.4042(3) 0.3049(3) 0.0806(19) Uani 1 1 d U A 1 C3 C 0.9056(6) 0.7073(5) -0.0173(5) 0.098(3) Uani 1 1 d DU A 1 C4 C 0.9419(7) 0.7610(6) 0.0269(5) 0.116(4) Uani 1 1 d DU A 1 H4A H 0.9101 0.7864 0.0559 0.140 Uiso 1 1 calc R A 1 C5 C 1.0169(6) 0.7762(7) 0.0288(6) 0.109(3) Uani 1 1 d DU A 1 H5A H 1.0359 0.8148 0.0555 0.130 Uiso 1 1 calc R A 1 N1 N 1.0654(4) 0.7350(4) -0.0085(4) 0.074(2) Uani 1 1 d DU A 1 C1 C 1.0394(7) 0.6849(6) -0.0429(6) 0.112(3) Uani 1 1 d DU A 1 H1A H 1.0755 0.6551 -0.0647 0.135 Uiso 1 1 calc R A 1 C2 C 0.9570(6) 0.6658(5) -0.0540(5) 0.116(3) Uani 1 1 d DU A 1 H2 H 0.9412 0.6288 -0.0835 0.140 Uiso 1 1 calc R A 1 C6 C 0.8179(5) 0.6993(6) -0.0213(5) 0.091(3) Uani 1 1 d U A 1 H6A H 0.7972 0.6971 0.0216 0.109 Uiso 1 1 calc R A 1 H6B H 0.7972 0.7453 -0.0416 0.109 Uiso 1 1 calc R A 1 C7 C 0.7853(3) 0.6387(5) -0.1221(5) 0.085(3) Uani 1 1 d DU A 1 C8 C 0.7566(2) 0.5697(5) -0.1585(4) 0.076(3) Uani 1 1 d DU A 1 C9 C 0.7433(4) 0.5722(6) -0.2248(5) 0.093(3) Uani 1 1 d DU A 1 H9A H 0.7530 0.6180 -0.2466 0.112 Uiso 1 1 calc R A 1 C10 C 0.7172(5) 0.5113(6) -0.2576(5) 0.080(3) Uani 1 1 d DU A 1 H10A H 0.7103 0.5142 -0.3015 0.096 Uiso 1 1 calc R A 1 C11 C 0.7005(5) 0.4433(6) -0.2244(4) 0.076(3) Uani 1 1 d DU A 1 C12 C 0.6647(6) 0.3758(7) -0.2587(6) 0.099(3) Uani 1 1 d DU A 1 C13 C 0.6717(6) 0.2998(6) -0.1645(6) 0.096(3) Uani 1 1 d DU A 1 C14 C 0.7013(5) 0.3692(5) -0.1276(5) 0.068(2) Uani 1 1 d DU A 1 C15 C 0.7195(5) 0.3638(5) -0.0665(5) 0.081(3) Uani 1 1 d DU A 1 H15A H 0.7150 0.3157 -0.0470 0.097 Uiso 1 1 calc R A 1 C16 C 0.7445(6) 0.4249(6) -0.0303(5) 0.083(3) Uani 1 1 d DU A 1 H16A H 0.7542 0.4190 0.0131 0.100 Uiso 1 1 calc R A 1 C17 C 0.7550(5) 0.4954(5) -0.0597(4) 0.073(2) Uani 1 1 d DU A 1 C18 C 0.7826(6) 0.5664(7) -0.0266(5) 0.088(3) Uani 1 1 d DU A 1 C19 C 0.7401(4) 0.5025(5) -0.1249(4) 0.062(2) Uani 1 1 d DU A 1 C20 C 0.7137(5) 0.4341(5) -0.1596(4) 0.065(2) Uani 1 1 d DU A 1 C21 C 0.6269(6) 0.2444(7) -0.2614(6) 0.106(3) Uani 1 1 d DU A 1 H21A H 0.6506 0.1974 -0.2453 0.128 Uiso 1 1 calc R A 1 H21B H 0.6416 0.2500 -0.3059 0.128 Uiso 1 1 calc R A 1 C22 C 0.5385(5) 0.2374(5) -0.2567(5) 0.084(2) Uani 1 1 d DU A 1 C23 C 0.5021(7) 0.1981(6) -0.2989(6) 0.088(3) Uani 0.60 1 d PDU A 1 H23A H 0.5318 0.1739 -0.3301 0.106 Uiso 1 1 calc R A 1 C24 C 0.4240(7) 0.1884(8) -0.3023(7) 0.081(3) Uani 0.60 1 d PDU A 1 H24A H 0.4029 0.1609 -0.3362 0.098 Uiso 1 1 calc R A 1 N4 N 0.3775(4) 0.2177(4) -0.2581(4) 0.079(2) Uani 1 1 d DU A 1 C25 C 0.4057(7) 0.2645(8) -0.2114(6) 0.080(3) Uani 0.60 1 d PDU A 1 H25 H 0.3758 0.2880 -0.1800 0.096 Uiso 1 1 calc R A 1 C26 C 0.4879(7) 0.2726(9) -0.2172(7) 0.085(3) Uani 0.60 1 d PDU A 1 H26A H 0.5099 0.3080 -0.1892 0.102 Uiso 1 1 calc R A 1 C29 C 1.2006(4) 1.0473(5) 0.0439(4) 0.059(2) Uani 1 1 d DU A 1 C30 C 1.2241(5) 1.0175(5) -0.0089(5) 0.077(3) Uani 1 1 d DU A 1 H30A H 1.2412 1.0495 -0.0417 0.092 Uiso 1 1 calc R A 1 C31 C 1.2239(6) 0.9378(6) -0.0174(5) 0.086(3) Uani 1 1 d DU A 1 H31A H 1.2460 0.9174 -0.0542 0.103 Uiso 1 1 calc R A 1 N5 N 1.1920(4) 0.8874(4) 0.0270(3) 0.0593(19) Uani 1 1 d DU A 1 C27 C 1.1703(4) 0.9214(5) 0.0785(4) 0.060(2) Uani 1 1 d DU A 1 H27A H 1.1515 0.8905 0.1114 0.072 Uiso 1 1 calc R A 1 C28 C 1.1725(4) 1.0006(5) 0.0889(4) 0.064(2) Uani 1 1 d DU A 1 H28A H 1.1545 1.0211 0.1271 0.077 Uiso 1 1 calc R A 1 C32 C 1.2033(5) 1.1360(4) 0.0534(4) 0.062(2) Uani 1 1 d U A 1 H32A H 1.2494 1.1486 0.0777 0.075 Uiso 1 1 calc R A 1 H32B H 1.2086 1.1602 0.0118 0.075 Uiso 1 1 calc R A 1 C33 C 1.0732(6) 1.1834(5) 0.0486(4) 0.070(2) Uani 1 1 d U A 1 C34 C 1.0066(6) 1.2278(5) 0.0751(4) 0.069(2) Uani 1 1 d U A 1 C35 C 0.9408(5) 1.2374(5) 0.0380(5) 0.076(3) Uani 1 1 d U A 1 H35A H 0.9360 1.2166 -0.0027 0.091 Uiso 1 1 calc R A 1 C36 C 0.8804(6) 1.2823(5) 0.0678(5) 0.079(3) Uani 1 1 d U A 1 H36A H 0.8362 1.2934 0.0442 0.095 Uiso 1 1 calc R A 1 C37 C 0.8848(5) 1.3087(5) 0.1274(4) 0.060(2) Uani 1 1 d U A 1 C38 C 0.8209(6) 1.3561(5) 0.1580(5) 0.073(2) Uani 1 1 d U A 1 C39 C 0.8960(5) 1.3720(5) 0.2528(5) 0.065(2) Uani 1 1 d U A 1 C40 C 0.9596(5) 1.3263(5) 0.2254(4) 0.058(2) Uani 1 1 d U A 1 C41 C 1.0257(5) 1.3113(5) 0.2631(4) 0.068(2) Uani 1 1 d U A 1 H41A H 1.0286 1.3302 0.3046 0.082 Uiso 1 1 calc R A 1 C42 C 1.0865(5) 1.2681(4) 0.2378(4) 0.065(2) Uani 1 1 d U A 1 H42A H 1.1305 1.2580 0.2620 0.078 Uiso 1 1 calc R A 1 C43 C 1.0801(4) 1.2406(4) 0.1762(4) 0.052(2) Uani 1 1 d U A 1 C44 C 1.1443(5) 1.1922(5) 0.1486(4) 0.060(2) Uani 1 1 d U A 1 C45 C 1.0153(5) 1.2542(4) 0.1395(4) 0.055(2) Uani 1 1 d U A 1 C46 C 0.9521(4) 1.2980(4) 0.1643(4) 0.052(2) Uani 1 1 d U A 1 C47 C 0.7647(5) 1.4184(5) 0.2496(5) 0.075(2) Uani 1 1 d U A 1 H47A H 0.7646 1.4047 0.2944 0.090 Uiso 1 1 calc R A 1 H47B H 0.7172 1.3989 0.2308 0.090 Uiso 1 1 calc R A 1 C48 C 0.7661(4) 1.5085(5) 0.2432(4) 0.069(2) Uani 1 1 d DU A 1 C49 C 0.7874(6) 1.5472(6) 0.1953(6) 0.070(3) Uani 0.60 1 d PDU A 1 H49A H 0.8043 1.5231 0.1582 0.084 Uiso 1 1 calc R A 1 C50 C 0.7847(7) 1.6224(6) 0.2001(6) 0.061(3) Uani 0.60 1 d PDU A 1 H50 H 0.7986 1.6487 0.1632 0.074 Uiso 1 1 calc R A 1 N8 N 0.7669(4) 1.6646(4) 0.2451(4) 0.0765(19) Uani 1 1 d DU A 1 C51 C 0.7324(8) 1.6284(7) 0.2967(6) 0.079(3) Uani 0.60 1 d PDU A 1 C52 C 0.7321(9) 1.5479(7) 0.2931(7) 0.084(3) Uani 0.60 1 d PDU A 1 H52A H 0.7081 1.5199 0.3253 0.101 Uiso 1 1 calc R A 1 N9 N 1.1860(5) 0.7618(5) -0.1474(4) 0.093(2) Uani 1 1 d U A 1 O9 O 1.2318(5) 0.7094(5) -0.1436(4) 0.121(3) Uani 1 1 d U A 1 O10 O 1.1483(4) 0.7729(4) -0.1975(3) 0.092(2) Uani 1 1 d U A 1 O11 O 1.1770(5) 0.8028(5) -0.1021(4) 0.119(3) Uani 1 1 d U A 1 N10 N 1.1836(6) 0.7082(7) 0.1456(5) 0.121(3) Uani 1 1 d U B 1 O12 O 1.1297(6) 0.7046(6) 0.1106(4) 0.147(3) Uani 1 1 d U B 1 O13 O 1.1888(4) 0.6784(5) 0.1978(4) 0.107(2) Uani 1 1 d U B 1 O14 O 1.2388(7) 0.7517(5) 0.1247(6) 0.162(3) Uani 1 1 d U B 1 C53 C 1.0133(6) 0.9054(7) -0.1546(4) 0.088(4) Uani 0.50 1 d PDU C 1 H53A H 1.0510 0.8630 -0.1555 0.106 Uiso 0.50 1 calc PR C 1 Cl1 Cl 1.0551(3) 0.9705(2) -0.1040(2) 0.0785(15) Uani 0.50 1 d PDU C 1 Cl2 Cl 0.9317(3) 0.8616(3) -0.1288(2) 0.0757(14) Uani 0.50 1 d PDU C 1 Cl3 Cl 1.0100(3) 0.9340(4) -0.2307(2) 0.112(2) Uani 0.50 1 d PDU C 1 C54 C 0.9406(6) 0.4547(9) -0.3213(5) 0.121(9) Uani 0.40 1 d PDU D 1 H54A H 0.9121 0.4097 -0.3373 0.146 Uiso 0.40 1 calc PR D 1 Cl4 Cl 0.9441(7) 0.4537(7) -0.2383(5) 0.227(5) Uani 0.40 1 d PDU D 1 Cl5 Cl 1.0359(5) 0.4529(5) -0.3480(5) 0.177(4) Uani 0.40 1 d PDU D 1 Cl6 Cl 0.8985(3) 0.5400(3) -0.3480(3) 0.084(2) Uani 0.40 1 d PDU D 1 C23' C 0.4980(9) 0.2844(9) -0.2905(7) 0.080(3) Uani 0.40 1 d PDU E 2 C24' C 0.4209(10) 0.2848(8) -0.2983(7) 0.077(3) Uani 0.40 1 d PDU E 2 C25' C 0.4353(9) 0.1740(12) -0.2285(10) 0.077(3) Uani 0.40 1 d PDU F 2 C26' C 0.5187(10) 0.1839(13) -0.2306(11) 0.086(3) Uani 0.40 1 d PDU F 2 C49' C 0.7465(7) 1.5505(8) 0.1955(8) 0.062(3) Uani 0.40 1 d PDU G 2 C50' C 0.7478(9) 1.6262(9) 0.1907(9) 0.064(3) Uani 0.40 1 d PDU G 2 C51' C 0.7973(14) 1.6347(9) 0.2895(10) 0.078(3) Uani 0.40 1 d PDU H 2 C52' C 0.7991(13) 1.5537(10) 0.2949(10) 0.077(3) Uani 0.40 1 d PDU H 2 C55 C 0.4347(9) 0.5001(6) -0.4321(5) 0.076(7) Uiso 0.40 1 d PD I 3 H55A H 0.4890 0.4868 -0.4242 0.114 Uiso 0.40 1 calc PR I 3 Cl9 Cl 0.3798(5) 0.4212(5) -0.4274(5) 0.143(3) Uiso 0.40 1 d PD I 3 Cl8 Cl 0.4252(12) 0.5410(9) -0.5045(6) 0.300 Uiso 0.40 1 d PD I 3 Cl7 Cl 0.4042(10) 0.5630(8) -0.3782(6) 0.254(7) Uiso 0.40 1 d PD I 3 C56 C 0.4897(6) 0.4704(7) -0.3775(6) 0.169(15) Uiso 0.40 1 d PD J 4 H56A H 0.5149 0.4352 -0.3473 0.203 Uiso 0.40 1 calc PR J 4 Cl10 Cl 0.5540(4) 0.4889(4) -0.4345(3) 0.101(2) Uiso 0.40 1 d PD J 4 Cl11 Cl 0.4107(8) 0.4231(8) -0.4058(8) 0.300 Uiso 0.40 1 d PD J 4 Cl12 Cl 0.4594(6) 0.5464(5) -0.3350(5) 0.144(3) Uiso 0.40 1 d PD J 4 C57 C 0.9831(12) 0.4099(7) -0.0568(5) 0.20(3) Uiso 0.30 1 d PD K 6 H57A H 0.9337 0.3854 -0.0677 0.242 Uiso 0.30 1 calc PR K 6 Cl15 Cl 1.0515(6) 0.3393(4) -0.0783(4) 0.114(3) Uani 0.30 1 d PD K 6 Cl14 Cl 0.9828(11) 0.4946(6) -0.1035(6) 0.226(8) Uiso 0.30 1 d PD K 6 Cl13 Cl 0.9739(18) 0.4281(12) 0.0252(7) 0.160(15) Uiso 0.10 1 d PD K 6 Cl16 Cl 1.0547(10) 0.3612(10) -0.1216(8) 0.111(5) Uiso 0.20 1 d P L 7 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 Cd1 0.0610(3) 0.0503(3) 0.0867(4) -0.0057(4) 0.0170(4) -0.0065(3) N2 0.073(4) 0.085(4) 0.098(5) 0.002(4) 0.006(4) -0.025(4) N3 0.070(4) 0.093(5) 0.134(6) 0.000(4) -0.026(4) 0.012(4) N6 0.059(3) 0.038(3) 0.078(4) -0.009(3) -0.003(3) 0.003(3) N7 0.084(4) 0.045(3) 0.073(4) 0.003(3) 0.013(4) 0.011(3) O1 0.085(4) 0.083(4) 0.153(5) 0.034(4) 0.038(4) 0.003(4) O2 0.126(5) 0.123(5) 0.102(5) -0.006(4) 0.004(4) -0.043(4) O3 0.090(4) 0.091(4) 0.148(5) 0.017(4) -0.019(4) -0.010(4) O4 0.127(5) 0.144(5) 0.119(5) -0.013(5) -0.060(4) 0.028(4) O5 0.114(4) 0.104(4) 0.073(4) -0.013(4) -0.002(4) 0.027(4) O6 0.065(3) 0.061(3) 0.098(4) 0.007(3) -0.002(3) 0.004(3) O7 0.089(4) 0.080(4) 0.118(4) 0.018(4) -0.016(4) 0.023(3) O8 0.089(4) 0.068(3) 0.085(4) -0.003(3) 0.011(3) 0.000(3) C3 0.086(5) 0.090(5) 0.118(6) -0.007(5) 0.028(5) -0.023(5) C4 0.101(6) 0.114(6) 0.134(7) -0.020(6) 0.011(6) -0.002(6) C5 0.086(6) 0.107(6) 0.133(7) -0.021(6) 0.019(6) 0.001(5) N1 0.068(4) 0.049(3) 0.106(5) -0.009(4) 0.015(4) -0.010(3) C1 0.087(6) 0.103(6) 0.147(7) -0.018(6) 0.016(6) -0.008(5) C2 0.079(6) 0.118(6) 0.153(7) -0.024(6) 0.012(6) -0.013(6) C6 0.076(5) 0.085(5) 0.111(6) -0.010(5) 0.016(5) -0.015(5) C7 0.068(4) 0.070(5) 0.116(5) 0.023(5) 0.028(5) 0.001(4) C8 0.069(5) 0.078(5) 0.080(5) 0.018(4) 0.000(4) 0.004(4) C9 0.088(5) 0.106(6) 0.087(6) 0.031(5) 0.003(5) 0.011(5) C10 0.087(5) 0.092(5) 0.062(5) 0.001(5) -0.016(5) 0.005(5) C11 0.074(5) 0.089(5) 0.067(5) -0.006(4) -0.004(4) 0.016(4) C12 0.077(5) 0.119(5) 0.099(5) -0.007(5) -0.033(5) 0.026(5) C13 0.080(5) 0.078(5) 0.132(6) 0.010(5) -0.006(5) -0.006(5) C14 0.053(4) 0.061(4) 0.088(5) 0.026(4) -0.009(4) -0.009(4) C15 0.071(5) 0.067(5) 0.104(6) 0.017(5) 0.010(5) -0.016(4) C16 0.094(5) 0.079(5) 0.076(5) 0.014(5) 0.015(5) -0.023(5) C17 0.084(5) 0.070(5) 0.065(5) -0.003(4) 0.018(4) -0.006(4) C18 0.097(5) 0.097(5) 0.069(5) 0.000(5) 0.003(5) -0.030(5) C19 0.054(4) 0.067(4) 0.064(5) 0.017(4) 0.008(4) -0.003(4) C20 0.050(4) 0.078(5) 0.067(5) 0.015(4) -0.004(4) -0.005(4) C21 0.075(5) 0.111(6) 0.133(7) -0.008(6) -0.018(5) 0.018(5) C22 0.059(4) 0.090(4) 0.102(5) -0.004(4) -0.002(4) 0.001(4) C23 0.072(5) 0.101(5) 0.092(5) -0.004(5) 0.006(5) 0.006(5) C24 0.072(5) 0.094(5) 0.078(5) -0.006(5) -0.015(5) -0.002(5) N4 0.076(4) 0.073(4) 0.090(4) 0.010(4) -0.013(4) 0.001(3) C25 0.073(6) 0.077(6) 0.088(6) -0.005(6) -0.008(6) -0.005(5) C26 0.070(5) 0.087(5) 0.099(5) -0.006(5) -0.008(5) -0.006(5) C29 0.064(4) 0.045(4) 0.069(5) -0.003(4) 0.011(4) -0.005(4) C30 0.098(5) 0.052(4) 0.081(5) 0.003(4) 0.016(5) -0.025(4) C31 0.105(6) 0.082(5) 0.072(6) 0.000(5) 0.015(5) -0.010(5) N5 0.082(4) 0.051(3) 0.045(4) 0.006(3) 0.015(3) -0.014(3) C27 0.080(5) 0.053(4) 0.047(4) 0.012(4) 0.016(4) 0.006(4) C28 0.082(5) 0.048(4) 0.063(5) -0.006(4) 0.016(4) -0.005(4) C32 0.055(4) 0.043(4) 0.088(5) -0.010(4) 0.014(4) -0.005(4) C33 0.082(5) 0.068(4) 0.060(5) -0.005(4) 0.004(4) 0.004(4) C34 0.090(5) 0.052(4) 0.066(5) 0.007(4) 0.014(4) -0.004(4) C35 0.080(5) 0.077(5) 0.070(5) 0.004(4) -0.018(4) 0.021(5) C36 0.083(5) 0.078(5) 0.076(5) 0.004(5) -0.023(5) 0.008(5) C37 0.060(4) 0.054(4) 0.066(5) -0.004(4) -0.002(4) 0.005(4) C38 0.077(4) 0.048(4) 0.094(5) 0.021(4) -0.008(4) 0.012(4) C39 0.071(4) 0.058(4) 0.065(4) -0.007(4) 0.007(4) 0.011(4) C40 0.059(4) 0.062(4) 0.052(4) -0.002(4) 0.007(4) -0.002(4) C41 0.066(4) 0.083(5) 0.055(5) -0.004(4) -0.001(4) 0.000(4) C42 0.071(4) 0.054(4) 0.069(5) 0.008(4) 0.004(4) 0.002(4) C43 0.052(4) 0.040(4) 0.063(4) 0.002(4) 0.008(4) -0.006(3) C44 0.064(4) 0.050(4) 0.067(4) 0.013(4) -0.003(4) -0.004(4) C45 0.068(4) 0.046(4) 0.050(4) 0.002(4) 0.007(4) -0.011(4) C46 0.051(4) 0.039(4) 0.066(4) -0.003(4) 0.003(4) 0.000(3) C47 0.074(4) 0.070(5) 0.081(5) 0.005(5) 0.026(5) 0.001(4) C48 0.066(4) 0.071(4) 0.070(4) 0.006(4) 0.017(4) 0.016(3) C49 0.080(5) 0.066(5) 0.065(5) 0.003(5) 0.016(5) 0.017(5) C50 0.078(5) 0.049(5) 0.057(5) -0.004(5) 0.006(5) 0.014(5) N8 0.079(4) 0.064(3) 0.087(4) -0.007(4) -0.011(4) 0.019(3) C51 0.081(6) 0.071(6) 0.086(6) 0.005(5) 0.003(6) 0.023(5) C52 0.082(6) 0.083(6) 0.088(6) 0.007(6) 0.010(6) 0.018(6) N9 0.118(5) 0.071(4) 0.089(4) -0.018(4) -0.005(4) -0.024(4) O9 0.140(5) 0.092(4) 0.130(5) -0.006(4) -0.042(4) 0.000(4) O10 0.112(4) 0.073(4) 0.093(4) -0.007(4) -0.007(4) -0.017(4) O11 0.163(6) 0.118(5) 0.075(4) -0.016(4) 0.014(4) -0.046(5) N10 0.108(5) 0.126(5) 0.128(5) 0.009(5) 0.014(5) 0.025(4) O12 0.138(6) 0.178(6) 0.124(6) 0.001(5) -0.027(5) 0.023(5) O13 0.105(4) 0.117(5) 0.099(5) 0.021(4) 0.019(4) 0.025(4) O14 0.174(6) 0.126(5) 0.187(6) 0.029(5) 0.015(6) 0.026(5) C53 0.089(6) 0.094(6) 0.081(6) 0.000(6) -0.003(6) -0.025(6) Cl1 0.080(3) 0.052(2) 0.104(4) 0.002(3) -0.003(3) -0.017(2) Cl2 0.077(3) 0.074(3) 0.076(3) 0.008(2) 0.013(2) -0.026(2) Cl3 0.109(4) 0.134(4) 0.095(4) 0.020(3) -0.001(3) -0.039(3) C54 0.110(14) 0.126(14) 0.128(14) -0.013(12) -0.044(12) -0.001(12) Cl4 0.246(9) 0.201(8) 0.233(9) -0.051(8) -0.109(8) 0.047(7) Cl5 0.099(5) 0.117(6) 0.315(10) -0.022(7) 0.013(6) 0.030(5) Cl6 0.055(3) 0.058(3) 0.138(5) -0.036(3) -0.004(3) -0.003(3) C23' 0.068(5) 0.080(5) 0.092(5) 0.001(5) -0.003(5) 0.001(5) C24' 0.070(5) 0.079(6) 0.081(6) 0.003(5) -0.012(5) -0.008(5) C25' 0.066(5) 0.081(5) 0.085(5) 0.006(5) -0.011(5) 0.006(5) C26' 0.068(5) 0.094(5) 0.097(5) -0.002(5) -0.004(5) 0.001(5) C49' 0.065(5) 0.059(5) 0.063(5) 0.006(5) 0.005(5) 0.014(5) C50' 0.072(5) 0.056(5) 0.063(5) -0.005(5) 0.005(5) 0.011(5) C51' 0.081(6) 0.068(5) 0.084(6) 0.001(5) -0.004(5) 0.019(5) C52' 0.073(6) 0.074(6) 0.084(6) 0.001(5) 0.004(5) 0.012(5) Cl15 0.190(9) 0.062(4) 0.091(6) -0.038(4) 0.060(6) -0.062(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N1 2.317(7) . ? Cd1 N5 2.337(6) . ? Cd1 N4 2.338(7) 4_665 ? Cd1 O11 2.364(8) . ? Cd1 N8 2.402(7) 3_854 ? N2 C18 1.298(13) . ? N2 C7 1.388(13) . ? N2 C6 1.454(12) . ? N3 C13 1.326(15) . ? N3 C12 1.344(14) . ? N3 C21 1.443(14) . ? N6 C33 1.367(11) . ? N6 C44 1.385(11) . ? N6 C32 1.451(10) . ? N7 C39 1.355(11) . ? N7 C38 1.359(12) . ? N7 C47 1.447(11) . ? O1 C7 1.222(11) . ? O2 C18 1.237(12) . ? O3 C13 1.253(13) . ? O4 C12 1.226(13) . ? O5 C33 1.218(11) . ? O6 C44 1.203(10) . ? O7 C38 1.258(11) . ? O8 C39 1.232(11) . ? C3 C2 1.377(14) . ? C3 C4 1.454(12) . ? C3 C6 1.524(13) . ? C4 C5 1.324(15) . ? C4 H4A 0.9300 . ? C5 N1 1.351(13) . ? C5 H5A 0.9300 . ? N1 C1 1.211(13) . ? C1 C2 1.481(15) . ? C1 H1A 0.9300 . ? C2 H2 0.9300 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.500(12) . ? C8 C19 1.389(12) . ? C8 C9 1.411(13) . ? C9 C10 1.334(13) . ? C9 H9A 0.9300 . ? C10 C11 1.396(13) . ? C10 H10A 0.9300 . ? C11 C20 1.387(12) . ? C11 C12 1.503(14) . ? C13 C14 1.516(14) . ? C14 C15 1.322(13) . ? C14 C20 1.326(12) . ? C15 C16 1.372(13) . ? C15 H15A 0.9300 . ? C16 C17 1.377(13) . ? C16 H16A 0.9300 . ? C17 C19 1.395(12) . ? C17 C18 1.489(14) . ? C19 C20 1.461(12) . ? C21 C22 1.536(13) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.280(15) . ? C22 C26 1.350(16) . ? C23 C24 1.363(16) . ? C23 H23A 0.9300 . ? C24 N4 1.327(15) . ? C24 H24A 0.9300 . ? N4 C25 1.360(12) . ? N4 Cd1 2.338(7) 3_644 ? C25 C26 1.431(16) . ? C25 H25 0.9300 . ? C26 H26A 0.9300 . ? C29 C30 1.287(12) . ? C29 C28 1.333(11) . ? C29 C32 1.548(11) . ? C30 C31 1.389(13) . ? C30 H30A 0.9300 . ? C31 N5 1.390(11) . ? C31 H31A 0.9300 . ? N5 C27 1.286(10) . ? C27 C28 1.387(11) . ? C27 H27A 0.9300 . ? C28 H28A 0.9300 . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.491(13) . ? C34 C35 1.389(13) . ? C34 C45 1.434(12) . ? C35 C36 1.444(13) . ? C35 H35A 0.9300 . ? C36 C37 1.334(12) . ? C36 H36A 0.9300 . ? C37 C46 1.410(11) . ? C37 C38 1.517(12) . ? C39 C40 1.470(11) . ? C40 C46 1.379(11) . ? C40 C41 1.414(11) . ? C41 C42 1.394(11) . ? C41 H41A 0.9300 . ? C42 C43 1.381(11) . ? C42 H42A 0.9300 . ? C43 C45 1.379(11) . ? C43 C44 1.507(11) . ? C45 C46 1.427(11) . ? C47 C48 1.564(12) . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C48 C49 1.261(15) . ? C48 C52 1.380(16) . ? C49 C50 1.305(14) . ? C49 H49A 0.9300 . ? C50 N8 1.232(14) . ? C50 H50 0.9300 . ? N8 C51 1.384(12) . ? N8 Cd1 2.402(7) 4_585 ? C51 C52 1.393(15) . ? C52 H52A 0.9300 . ? N9 O11 1.195(11) . ? N9 O9 1.207(11) . ? N9 O10 1.249(11) . ? N10 O12 1.189(13) . ? N10 O13 1.213(12) . ? N10 O14 1.291(14) . ? C53 Cl3 1.673(9) . ? C53 Cl2 1.690(9) . ? C53 Cl1 1.705(10) . ? C53 H53A 0.9800 . ? C54 Cl6 1.738(13) . ? C54 Cl5 1.739(12) . ? C54 Cl4 1.741(12) . ? C54 H54A 0.9800 . ? C23' C24' 1.343(19) . ? C25' C26' 1.452(19) . ? C49' C50' 1.312(17) . ? C51' C52' 1.405(19) . ? C55 Cl7 1.653(12) . ? C55 Cl9 1.665(11) . ? C55 Cl8 1.683(12) . ? C55 H55A 0.9800 . ? C56 Cl10 1.664(11) . ? C56 Cl12 1.671(11) . ? C56 Cl11 1.698(12) . ? C56 H56A 0.9800 . ? C57 Cl13 1.756(14) . ? C57 Cl15 1.757(14) . ? C57 Cl14 1.761(13) . ? C57 H57A 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cd1 N5 97.7(2) . . ? N1 Cd1 N4 89.3(2) . 4_665 ? N5 Cd1 N4 170.2(3) . 4_665 ? N1 Cd1 O11 79.4(3) . . ? N5 Cd1 O11 82.1(2) . . ? N4 Cd1 O11 106.0(3) 4_665 . ? N1 Cd1 N8 169.8(3) . 3_854 ? N5 Cd1 N8 88.5(3) . 3_854 ? N4 Cd1 N8 85.6(3) 4_665 3_854 ? O11 Cd1 N8 93.5(3) . 3_854 ? C18 N2 C7 122.9(9) . . ? C18 N2 C6 119.6(9) . . ? C7 N2 C6 117.1(8) . . ? C13 N3 C12 125.8(10) . . ? C13 N3 C21 118.2(10) . . ? C12 N3 C21 116.1(10) . . ? C33 N6 C44 124.5(7) . . ? C33 N6 C32 116.4(7) . . ? C44 N6 C32 119.0(7) . . ? C39 N7 C38 123.4(8) . . ? C39 N7 C47 118.5(8) . . ? C38 N7 C47 118.1(8) . . ? C2 C3 C4 114.3(9) . . ? C2 C3 C6 124.3(9) . . ? C4 C3 C6 121.4(9) . . ? C5 C4 C3 124.6(11) . . ? C5 C4 H4A 117.7 . . ? C3 C4 H4A 117.7 . . ? C4 C5 N1 119.0(11) . . ? C4 C5 H5A 120.5 . . ? N1 C5 H5A 120.5 . . ? C1 N1 C5 119.4(9) . . ? C1 N1 Cd1 122.2(7) . . ? C5 N1 Cd1 118.2(6) . . ? N1 C1 C2 127.5(11) . . ? N1 C1 H1A 116.2 . . ? C2 C1 H1A 116.2 . . ? C3 C2 C1 114.6(9) . . ? C3 C2 H2 122.7 . . ? C1 C2 H2 122.7 . . ? N2 C6 C3 114.6(8) . . ? N2 C6 H6A 108.6 . . ? C3 C6 H6A 108.6 . . ? N2 C6 H6B 108.6 . . ? C3 C6 H6B 108.6 . . ? H6A C6 H6B 107.6 . . ? O1 C7 N2 122.7(9) . . ? O1 C7 C8 119.8(10) . . ? N2 C7 C8 117.4(8) . . ? C19 C8 C9 119.5(8) . . ? C19 C8 C7 118.4(8) . . ? C9 C8 C7 122.1(9) . . ? C10 C9 C8 122.6(9) . . ? C10 C9 H9A 118.7 . . ? C8 C9 H9A 118.7 . . ? C9 C10 C11 118.6(9) . . ? C9 C10 H10A 120.7 . . ? C11 C10 H10A 120.7 . . ? C20 C11 C10 123.4(9) . . ? C20 C11 C12 116.6(9) . . ? C10 C11 C12 120.0(9) . . ? O4 C12 N3 122.1(11) . . ? O4 C12 C11 120.5(11) . . ? N3 C12 C11 117.5(10) . . ? O3 C13 N3 123.7(11) . . ? O3 C13 C14 118.7(11) . . ? N3 C13 C14 117.5(10) . . ? C15 C14 C20 120.8(9) . . ? C15 C14 C13 121.3(9) . . ? C20 C14 C13 117.7(9) . . ? C14 C15 C16 123.9(9) . . ? C14 C15 H15A 118.1 . . ? C16 C15 H15A 118.1 . . ? C15 C16 C17 118.3(9) . . ? C15 C16 H16A 120.8 . . ? C17 C16 H16A 120.8 . . ? C16 C17 C19 119.5(9) . . ? C16 C17 C18 124.2(9) . . ? C19 C17 C18 116.3(8) . . ? O2 C18 N2 122.4(11) . . ? O2 C18 C17 115.5(10) . . ? N2 C18 C17 122.1(9) . . ? C8 C19 C17 122.1(8) . . ? C8 C19 C20 119.2(8) . . ? C17 C19 C20 118.4(8) . . ? C14 C20 C11 124.6(9) . . ? C14 C20 C19 118.8(8) . . ? C11 C20 C19 116.6(8) . . ? N3 C21 C22 111.6(9) . . ? N3 C21 H21A 109.3 . . ? C22 C21 H21A 109.3 . . ? N3 C21 H21B 109.3 . . ? C22 C21 H21B 109.3 . . ? H21A C21 H21B 108.0 . . ? C23 C22 C26 110.1(10) . . ? C23 C22 C21 119.0(10) . . ? C26 C22 C21 130.5(10) . . ? C22 C23 C24 126.0(13) . . ? C22 C23 H23A 117.0 . . ? C24 C23 H23A 117.0 . . ? N4 C24 C23 121.1(13) . . ? N4 C24 H24A 119.5 . . ? C23 C24 H24A 119.5 . . ? C24 N4 C25 120.8(9) . . ? C24 N4 Cd1 127.1(7) . 3_644 ? C25 N4 Cd1 112.1(7) . 3_644 ? N4 C25 C26 110.6(11) . . ? N4 C25 H25 124.7 . . ? C26 C25 H25 124.7 . . ? C22 C26 C25 130.7(13) . . ? C22 C26 H26A 114.7 . . ? C25 C26 H26A 114.7 . . ? C30 C29 C28 118.9(8) . . ? C30 C29 C32 119.9(8) . . ? C28 C29 C32 121.3(8) . . ? C29 C30 C31 120.4(9) . . ? C29 C30 H30A 119.8 . . ? C31 C30 H30A 119.8 . . ? C30 C31 N5 122.4(9) . . ? C30 C31 H31A 118.8 . . ? N5 C31 H31A 118.8 . . ? C27 N5 C31 113.1(7) . . ? C27 N5 Cd1 130.0(5) . . ? C31 N5 Cd1 116.6(5) . . ? N5 C27 C28 125.2(8) . . ? N5 C27 H27A 117.4 . . ? C28 C27 H27A 117.4 . . ? C29 C28 C27 119.7(8) . . ? C29 C28 H28A 120.1 . . ? C27 C28 H28A 120.1 . . ? N6 C32 C29 116.0(6) . . ? N6 C32 H32A 108.3 . . ? C29 C32 H32A 108.3 . . ? N6 C32 H32B 108.3 . . ? C29 C32 H32B 108.3 . . ? H32A C32 H32B 107.4 . . ? O5 C33 N6 118.0(9) . . ? O5 C33 C34 122.0(9) . . ? N6 C33 C34 120.0(8) . . ? C35 C34 C45 125.2(9) . . ? C35 C34 C33 119.0(8) . . ? C45 C34 C33 115.7(8) . . ? C34 C35 C36 114.5(9) . . ? C34 C35 H35A 122.8 . . ? C36 C35 H35A 122.8 . . ? C37 C36 C35 123.3(9) . . ? C37 C36 H36A 118.3 . . ? C35 C36 H36A 118.3 . . ? C36 C37 C46 121.0(8) . . ? C36 C37 C38 122.7(8) . . ? C46 C37 C38 116.1(8) . . ? O7 C38 N7 121.6(9) . . ? O7 C38 C37 119.0(9) . . ? N7 C38 C37 119.2(8) . . ? O8 C39 N7 119.1(8) . . ? O8 C39 C40 121.5(8) . . ? N7 C39 C40 119.4(8) . . ? C46 C40 C41 122.0(8) . . ? C46 C40 C39 118.9(8) . . ? C41 C40 C39 119.0(7) . . ? C42 C41 C40 119.7(8) . . ? C42 C41 H41A 120.2 . . ? C40 C41 H41A 120.2 . . ? C43 C42 C41 118.7(8) . . ? C43 C42 H42A 120.7 . . ? C41 C42 H42A 120.7 . . ? C45 C43 C42 121.9(7) . . ? C45 C43 C44 118.5(7) . . ? C42 C43 C44 119.5(7) . . ? O6 C44 N6 121.9(8) . . ? O6 C44 C43 120.8(8) . . ? N6 C44 C43 117.1(7) . . ? C43 C45 C46 120.6(7) . . ? C43 C45 C34 123.8(8) . . ? C46 C45 C34 115.6(8) . . ? C40 C46 C37 122.7(7) . . ? C40 C46 C45 117.1(7) . . ? C37 C46 C45 120.2(8) . . ? N7 C47 C48 112.8(7) . . ? N7 C47 H47A 109.0 . . ? C48 C47 H47A 109.0 . . ? N7 C47 H47B 109.0 . . ? C48 C47 H47B 109.0 . . ? H47A C47 H47B 107.8 . . ? C49 C48 C52 117.8(10) . . ? C49 C48 C47 126.9(9) . . ? C52 C48 C47 114.8(9) . . ? C48 C49 C50 117.2(12) . . ? C48 C49 H49A 121.4 . . ? C50 C49 H49A 121.4 . . ? N8 C50 C49 131.1(13) . . ? N8 C50 H50 114.5 . . ? C49 C50 H50 114.5 . . ? C50 N8 C51 116.1(9) . . ? C50 N8 Cd1 131.1(8) . 4_585 ? C51 N8 Cd1 111.4(6) . 4_585 ? N8 C51 C52 114.2(11) . . ? C48 C52 C51 122.2(13) . . ? C48 C52 H52A 118.9 . . ? C51 C52 H52A 118.9 . . ? O11 N9 O9 118.5(10) . . ? O11 N9 O10 120.6(9) . . ? O9 N9 O10 120.9(9) . . ? N9 O11 Cd1 120.9(7) . . ? O12 N10 O13 126.4(12) . . ? O12 N10 O14 113.5(12) . . ? O13 N10 O14 120.0(11) . . ? Cl3 C53 Cl2 114.1(6) . . ? Cl3 C53 Cl1 114.4(7) . . ? Cl2 C53 Cl1 116.8(6) . . ? Cl3 C53 H53A 103.0 . . ? Cl2 C53 H53A 103.0 . . ? Cl1 C53 H53A 103.0 . . ? Cl6 C54 Cl5 107.9(8) . . ? Cl6 C54 Cl4 110.2(9) . . ? Cl5 C54 Cl4 106.8(8) . . ? Cl6 C54 H54A 110.6 . . ? Cl5 C54 H54A 110.6 . . ? Cl4 C54 H54A 110.6 . . ? Cl7 C55 Cl9 108.5(9) . . ? Cl7 C55 Cl8 108.0(10) . . ? Cl9 C55 Cl8 109.9(10) . . ? Cl7 C55 H55A 110.1 . . ? Cl9 C55 H55A 110.1 . . ? Cl8 C55 H55A 110.1 . . ? Cl10 C56 Cl12 116.2(8) . . ? Cl10 C56 Cl11 112.2(9) . . ? Cl12 C56 Cl11 108.2(9) . . ? Cl10 C56 H56A 106.6 . . ? Cl12 C56 H56A 106.5 . . ? Cl11 C56 H56A 106.5 . . ? Cl13 C57 Cl15 115.9(10) . . ? Cl13 C57 Cl14 113.3(9) . . ? Cl15 C57 Cl14 115.9(9) . . ? Cl13 C57 H57A 103.1 . . ? Cl15 C57 H57A 103.1 . . ? Cl14 C57 H57A 103.1 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.821 _refine_diff_density_min -0.520 _refine_diff_density_rms 0.110