# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name 'Shengqun Su' 'Chao Qin' 'Zhiyong Guo' 'Huadong Guo' 'Shuyan Song' ; Ruiping Deng ; 'Feng Cao' 'Song Wang' 'Guanghua Li' 'Hongjie Zhang' _publ_contact_author_name 'Dr Hongjie Zhang' _publ_contact_author_email hongjie@ciac.jl.cn data_1 _database_code_depnum_ccdc_archive 'CCDC 803528' #TrackingRef '- 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C28 H28 Cd N4 O4' _chemical_formula_sum 'C28 H28 Cd N4 O4' _chemical_formula_weight 596.94 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 Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.4485(7) _cell_length_b 12.3314(6) _cell_length_c 17.4418(9) _cell_angle_alpha 90.00 _cell_angle_beta 94.3890(10) _cell_angle_gamma 90.00 _cell_volume 2669.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 185(2) _cell_measurement_reflns_used 5249 _cell_measurement_theta_min 1.94 _cell_measurement_theta_max 26.04 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.485 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1216 _exptl_absorpt_coefficient_mu 0.858 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7828 _exptl_absorpt_correction_T_max 0.9191 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 185(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 9.00cm _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 14580 _diffrn_reflns_av_R_equivalents 0.0364 _diffrn_reflns_av_sigmaI/netI 0.0439 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 26.04 _reflns_number_total 5249 _reflns_number_gt 3831 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXP-97 _computing_publication_material 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^)+(0.0595P)^2^+3.1468P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5249 _refine_ls_number_parameters 342 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0670 _refine_ls_R_factor_gt 0.0462 _refine_ls_wR_factor_ref 0.1266 _refine_ls_wR_factor_gt 0.1140 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _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 Cd1 Cd 0.10865(3) 0.84465(2) 0.051757(19) 0.04109(13) Uani 1 1 d . . . C1 C 0.2821(4) 1.0945(3) -0.1259(2) 0.0390(10) Uani 1 1 d . . . H1A H 0.2064 1.1047 -0.1262 0.047 Uiso 1 1 calc R . . C2 C 0.3313(4) 1.0042(3) -0.0893(2) 0.0403(10) Uani 1 1 d . . . C3 C 0.4414(4) 0.9889(4) -0.0911(3) 0.0429(11) Uani 1 1 d . . . H3A H 0.4737 0.9259 -0.0681 0.052 Uiso 1 1 calc R . . C4 C 0.5050(4) 1.0631(3) -0.1257(3) 0.0411(10) Uani 1 1 d . . . H4A H 0.5806 1.0527 -0.1255 0.049 Uiso 1 1 calc R . . C5 C 0.6080(4) 1.2678(3) -0.2128(2) 0.0392(10) Uani 1 1 d . . . H5A H 0.6647 1.2218 -0.1930 0.047 Uiso 1 1 calc R . . C6 C 0.6293(4) 1.3605(3) -0.2550(2) 0.0397(10) Uani 1 1 d . . . H6A H 0.7017 1.3778 -0.2640 0.048 Uiso 1 1 calc R . . C7 C 0.5469(4) 1.4276(3) -0.2837(2) 0.0394(10) Uani 1 1 d . . . C8 C 0.4408(4) 1.4044(4) -0.2704(3) 0.0436(11) Uani 1 1 d . . . H8A H 0.3842 1.4507 -0.2899 0.052 Uiso 1 1 calc R . . C9 C 0.3104(4) 1.2722(4) -0.2041(3) 0.0453(11) Uani 1 1 d . . . C10 C 0.3449(4) 1.1682(3) -0.1614(2) 0.0382(10) Uani 1 1 d . . . C11 C 0.4561(3) 1.1531(3) -0.1607(2) 0.0365(9) Uani 1 1 d . . . C12 C 0.5024(4) 1.2451(3) -0.2008(2) 0.0360(10) Uani 1 1 d . . . C13 C 0.4183(4) 1.3129(3) -0.2281(3) 0.0394(10) Uani 1 1 d . . . C14 C 0.2292(4) 1.2486(5) -0.2726(3) 0.0674(16) Uani 1 1 d . . . H14A H 0.2608 1.1973 -0.3074 0.101 Uiso 1 1 calc R . . H14B H 0.2112 1.3163 -0.3001 0.101 Uiso 1 1 calc R . . H14C H 0.1637 1.2172 -0.2540 0.101 Uiso 1 1 calc R . . C15 C 0.2628(5) 1.3529(4) -0.1488(4) 0.0667(16) Uani 1 1 d . . . H15A H 0.3155 1.3669 -0.1053 0.100 Uiso 1 1 calc R . . H15B H 0.1971 1.3223 -0.1299 0.100 Uiso 1 1 calc R . . H15C H 0.2454 1.4210 -0.1759 0.100 Uiso 1 1 calc R . . C16 C 0.2657(4) 0.9278(4) -0.0444(3) 0.0466(12) Uani 1 1 d . . . C17 C 0.5734(4) 1.5217(4) -0.3339(3) 0.0457(11) Uani 1 1 d . . . C18 C 0.0510(4) 0.6237(4) 0.1770(3) 0.0547(13) Uani 1 1 d . . . H18A H 0.0250 0.6982 0.1698 0.082 Uiso 1 1 calc R . . H18B H 0.0744 0.6120 0.2313 0.082 Uiso 1 1 calc R . . H18C H -0.0072 0.5729 0.1614 0.082 Uiso 1 1 calc R . . C19 C 0.1428(3) 0.6053(3) 0.1296(3) 0.0381(10) Uani 1 1 d . . . C20 C 0.2059(3) 0.5127(3) 0.1209(3) 0.0382(10) Uani 1 1 d . . . C21 C 0.2840(4) 0.5455(4) 0.0736(3) 0.0455(11) Uani 1 1 d . . . C22 C 0.3806(4) 0.4878(5) 0.0493(4) 0.0709(17) Uani 1 1 d . . . H22A H 0.4193 0.5349 0.0155 0.106 Uiso 1 1 calc R . . H22B H 0.3581 0.4215 0.0216 0.106 Uiso 1 1 calc R . . H22C H 0.4280 0.4690 0.0948 0.106 Uiso 1 1 calc R . . C23 C 0.1938(4) 0.4035(4) 0.1556(3) 0.0420(11) Uani 1 1 d . . . C24 C -0.0513(4) 0.3752(4) 0.0845(3) 0.0507(12) Uani 1 1 d . . . H24A H -0.1154 0.3476 0.0547 0.076 Uiso 1 1 calc R . . H24B H -0.0376 0.4500 0.0691 0.076 Uiso 1 1 calc R . . H24C H -0.0630 0.3732 0.1394 0.076 Uiso 1 1 calc R . . C25 C 0.0430(4) 0.3066(3) 0.0698(2) 0.0390(10) Uani 1 1 d . . . C26 C 0.1501(4) 0.3175(3) 0.1003(3) 0.0394(10) Uani 1 1 d . . . C27 C 0.2037(4) 0.2300(4) 0.0715(3) 0.0442(11) Uani 1 1 d . . . C28 C 0.3179(4) 0.1916(4) 0.0846(4) 0.0629(15) Uani 1 1 d . . . H28A H 0.3276 0.1260 0.0541 0.094 Uiso 1 1 calc R . . H28B H 0.3338 0.1751 0.1393 0.094 Uiso 1 1 calc R . . H28C H 0.3667 0.2484 0.0690 0.094 Uiso 1 1 calc R . . N1 N 0.1800(3) 0.6877(3) 0.0891(2) 0.0394(9) Uani 1 1 d . . . N2 N 0.2656(3) 0.6484(3) 0.0557(2) 0.0460(9) Uani 1 1 d . . . H2A H 0.3048 0.6866 0.0256 0.055 Uiso 1 1 calc R . . N3 N 0.0330(3) 0.2195(3) 0.0244(2) 0.0406(9) Uani 1 1 d . . . N4 N 0.1319(3) 0.1751(3) 0.0255(2) 0.0421(9) Uani 1 1 d . . . H4B H 0.1475 0.1171 -0.0008 0.050 Uiso 1 1 calc R . . O1 O 0.1758(3) 0.9635(3) -0.02570(19) 0.0512(8) Uani 1 1 d . . . O2 O 0.3021(3) 0.8373(3) -0.0258(2) 0.0594(10) Uani 1 1 d . . . O3 O 0.6700(3) 1.5391(3) -0.34632(19) 0.0521(8) Uani 1 1 d . . . O4 O 0.4983(3) 1.5780(3) -0.3645(2) 0.0579(9) Uani 1 1 d . . . H23B H 0.266(4) 0.381(4) 0.173(3) 0.048(13) Uiso 1 1 d . . . H23A H 0.146(4) 0.412(4) 0.196(3) 0.056(15) Uiso 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 Cd1 0.0534(2) 0.02893(18) 0.0408(2) -0.00221(14) 0.00312(15) -0.00370(15) C1 0.043(2) 0.040(2) 0.034(2) 0.0007(19) 0.0024(19) -0.001(2) C2 0.059(3) 0.029(2) 0.032(2) -0.0016(17) -0.002(2) -0.005(2) C3 0.051(3) 0.035(2) 0.042(3) 0.0054(19) -0.002(2) 0.005(2) C4 0.041(2) 0.038(2) 0.043(3) 0.005(2) -0.004(2) 0.007(2) C5 0.046(3) 0.038(2) 0.033(2) -0.0012(19) -0.0043(19) 0.000(2) C6 0.041(2) 0.044(3) 0.033(2) -0.0071(19) -0.0037(19) -0.008(2) C7 0.050(3) 0.037(2) 0.032(2) 0.0011(18) 0.002(2) -0.005(2) C8 0.049(3) 0.039(3) 0.042(3) 0.009(2) 0.002(2) 0.006(2) C9 0.042(3) 0.041(2) 0.054(3) 0.014(2) 0.007(2) 0.003(2) C10 0.048(3) 0.034(2) 0.032(2) 0.0030(18) 0.0006(19) 0.004(2) C11 0.041(2) 0.037(2) 0.031(2) 0.0014(18) 0.0011(18) -0.0011(19) C12 0.044(2) 0.033(2) 0.030(2) -0.0002(17) -0.0040(19) 0.0012(19) C13 0.045(3) 0.035(2) 0.038(2) 0.0055(19) 0.002(2) 0.0040(19) C14 0.046(3) 0.086(4) 0.068(4) 0.034(3) -0.012(3) -0.002(3) C15 0.069(4) 0.044(3) 0.091(4) 0.017(3) 0.034(3) 0.015(3) C16 0.065(3) 0.041(3) 0.033(2) -0.004(2) -0.002(2) -0.010(2) C17 0.056(3) 0.041(3) 0.040(3) -0.002(2) 0.004(2) -0.003(2) C18 0.050(3) 0.045(3) 0.072(4) -0.003(2) 0.020(3) 0.003(2) C19 0.037(2) 0.035(2) 0.042(2) -0.0051(19) -0.0034(19) -0.0016(19) C20 0.041(2) 0.034(2) 0.038(2) -0.0049(18) -0.0045(19) -0.0009(19) C21 0.041(3) 0.043(3) 0.052(3) -0.014(2) 0.005(2) -0.001(2) C22 0.058(3) 0.063(4) 0.094(5) -0.011(3) 0.023(3) 0.006(3) C23 0.046(3) 0.034(2) 0.044(3) -0.001(2) -0.007(2) 0.002(2) C24 0.052(3) 0.054(3) 0.046(3) -0.010(2) -0.001(2) 0.003(2) C25 0.048(3) 0.032(2) 0.036(2) 0.0029(18) 0.002(2) -0.0002(19) C26 0.053(3) 0.027(2) 0.038(2) 0.0040(18) -0.004(2) 0.0045(19) C27 0.053(3) 0.033(2) 0.046(3) 0.005(2) -0.001(2) 0.005(2) C28 0.059(3) 0.045(3) 0.083(4) -0.004(3) -0.009(3) 0.018(3) N1 0.044(2) 0.0337(19) 0.041(2) -0.0040(16) 0.0039(17) -0.0024(16) N2 0.047(2) 0.044(2) 0.048(2) -0.0052(18) 0.0108(18) -0.0067(18) N3 0.049(2) 0.034(2) 0.039(2) -0.0007(16) 0.0012(17) -0.0036(17) N4 0.056(2) 0.0282(19) 0.042(2) -0.0030(16) 0.0053(18) 0.0028(17) O1 0.068(2) 0.0365(17) 0.051(2) 0.0008(15) 0.0156(17) -0.0067(17) O2 0.077(3) 0.0361(19) 0.064(2) 0.0157(16) 0.002(2) -0.0031(17) O3 0.058(2) 0.0468(19) 0.051(2) 0.0122(16) 0.0008(16) -0.0070(17) O4 0.059(2) 0.052(2) 0.063(2) 0.0241(18) 0.0062(18) 0.0061(18) _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 O1 2.201(3) . ? Cd1 N1 2.207(4) . ? Cd1 N3 2.267(4) 3_565 ? Cd1 O4 2.289(3) 4_586 ? Cd1 O3 2.365(3) 4_586 ? Cd1 C17 2.649(5) 4_586 ? C1 C10 1.376(6) . ? C1 C2 1.402(6) . ? C1 H1A 0.9500 . ? C2 C3 1.386(6) . ? C2 C16 1.505(6) . ? C3 C4 1.379(6) . ? C3 H3A 0.9500 . ? C4 C11 1.385(6) . ? C4 H4A 0.9500 . ? C5 C12 1.377(6) . ? C5 C6 1.396(6) . ? C5 H5A 0.9500 . ? C6 C7 1.382(6) . ? C6 H6A 0.9500 . ? C7 C8 1.389(6) . ? C7 C17 1.505(6) . ? C8 C13 1.389(6) . ? C8 H8A 0.9500 . ? C9 C13 1.523(6) . ? C9 C10 1.528(6) . ? C9 C14 1.531(7) . ? C9 C15 1.537(7) . ? C10 C11 1.397(6) . ? C11 C12 1.472(6) . ? C12 C13 1.394(6) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 O2 1.238(6) . ? C16 O1 1.268(6) . ? C17 O4 1.251(6) . ? C17 O3 1.256(6) . ? C17 Cd1 2.649(5) 4_685 ? C18 C19 1.478(6) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 N1 1.339(6) . ? C19 C20 1.401(6) . ? C20 C21 1.383(6) . ? C20 C23 1.488(6) . ? C21 N2 1.323(6) . ? C21 C22 1.486(7) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C26 1.507(6) . ? C23 H23B 0.96(5) . ? C23 H23A 0.97(5) . ? C24 C25 1.485(6) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 N3 1.335(5) . ? C25 C26 1.403(6) . ? C26 C27 1.384(6) . ? C27 N4 1.337(6) . ? C27 C28 1.499(7) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? N1 N2 1.344(5) . ? N2 H2A 0.8800 . ? N3 N4 1.346(5) . ? N3 Cd1 2.267(4) 3_565 ? N4 H4B 0.8800 . ? O3 Cd1 2.365(3) 4_685 ? O4 Cd1 2.289(3) 4_685 ? 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 Cd1 N1 127.00(13) . . ? O1 Cd1 N3 100.81(13) . 3_565 ? N1 Cd1 N3 98.31(13) . 3_565 ? O1 Cd1 O4 112.89(13) . 4_586 ? N1 Cd1 O4 115.14(13) . 4_586 ? N3 Cd1 O4 92.38(13) 3_565 4_586 ? O1 Cd1 O3 86.65(12) . 4_586 ? N1 Cd1 O3 102.14(12) . 4_586 ? N3 Cd1 O3 147.56(13) 3_565 4_586 ? O4 Cd1 O3 56.12(12) 4_586 4_586 ? O1 Cd1 C17 98.07(14) . 4_586 ? N1 Cd1 C17 114.16(14) . 4_586 ? N3 Cd1 C17 119.46(15) 3_565 4_586 ? O4 Cd1 C17 28.14(13) 4_586 4_586 ? O3 Cd1 C17 28.30(13) 4_586 4_586 ? C10 C1 C2 119.1(4) . . ? C10 C1 H1A 120.4 . . ? C2 C1 H1A 120.4 . . ? C3 C2 C1 119.7(4) . . ? C3 C2 C16 120.2(4) . . ? C1 C2 C16 120.0(4) . . ? C4 C3 C2 121.4(4) . . ? C4 C3 H3A 119.3 . . ? C2 C3 H3A 119.3 . . ? C3 C4 C11 118.5(4) . . ? C3 C4 H4A 120.7 . . ? C11 C4 H4A 120.7 . . ? C12 C5 C6 118.0(4) . . ? C12 C5 H5A 121.0 . . ? C6 C5 H5A 121.0 . . ? C7 C6 C5 121.0(4) . . ? C7 C6 H6A 119.5 . . ? C5 C6 H6A 119.5 . . ? C6 C7 C8 120.4(4) . . ? C6 C7 C17 118.9(4) . . ? C8 C7 C17 120.7(4) . . ? C7 C8 C13 119.3(4) . . ? C7 C8 H8A 120.4 . . ? C13 C8 H8A 120.4 . . ? C13 C9 C10 100.9(4) . . ? C13 C9 C14 113.1(4) . . ? C10 C9 C14 111.5(4) . . ? C13 C9 C15 110.4(4) . . ? C10 C9 C15 110.1(4) . . ? C14 C9 C15 110.5(4) . . ? C1 C10 C11 120.4(4) . . ? C1 C10 C9 128.7(4) . . ? C11 C10 C9 110.9(4) . . ? C4 C11 C10 120.8(4) . . ? C4 C11 C12 130.7(4) . . ? C10 C11 C12 108.5(4) . . ? C5 C12 C13 121.8(4) . . ? C5 C12 C11 129.9(4) . . ? C13 C12 C11 108.3(4) . . ? C8 C13 C12 119.5(4) . . ? C8 C13 C9 129.2(4) . . ? C12 C13 C9 111.3(4) . . ? C9 C14 H14A 109.5 . . ? C9 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C9 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C9 C15 H15A 109.5 . . ? C9 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C9 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O2 C16 O1 123.9(5) . . ? O2 C16 C2 119.9(5) . . ? O1 C16 C2 116.1(4) . . ? O4 C17 O3 121.7(4) . . ? O4 C17 C7 119.1(4) . . ? O3 C17 C7 119.1(4) . . ? O4 C17 Cd1 59.7(2) . 4_685 ? O3 C17 Cd1 63.2(2) . 4_685 ? C7 C17 Cd1 166.8(3) . 4_685 ? C19 C18 H18A 109.5 . . ? C19 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C19 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N1 C19 C20 110.0(4) . . ? N1 C19 C18 119.4(4) . . ? C20 C19 C18 130.5(4) . . ? C21 C20 C19 104.6(4) . . ? C21 C20 C23 127.2(4) . . ? C19 C20 C23 128.2(4) . . ? N2 C21 C20 107.7(4) . . ? N2 C21 C22 121.5(5) . . ? C20 C21 C22 130.6(5) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20 C23 C26 114.7(4) . . ? C20 C23 H23B 106(3) . . ? C26 C23 H23B 106(3) . . ? C20 C23 H23A 107(3) . . ? C26 C23 H23A 109(3) . . ? H23B C23 H23A 114(4) . . ? C25 C24 H24A 109.5 . . ? C25 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C25 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N3 C25 C26 110.2(4) . . ? N3 C25 C24 121.5(4) . . ? C26 C25 C24 128.3(4) . . ? C27 C26 C25 104.9(4) . . ? C27 C26 C23 128.4(4) . . ? C25 C26 C23 126.6(4) . . ? N4 C27 C26 107.1(4) . . ? N4 C27 C28 120.9(4) . . ? C26 C27 C28 132.0(5) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C19 N1 N2 105.8(4) . . ? C19 N1 Cd1 132.3(3) . . ? N2 N1 Cd1 120.2(3) . . ? C21 N2 N1 111.9(4) . . ? C21 N2 H2A 124.1 . . ? N1 N2 H2A 124.1 . . ? C25 N3 N4 105.9(4) . . ? C25 N3 Cd1 131.4(3) . 3_565 ? N4 N3 Cd1 122.4(3) . 3_565 ? C27 N4 N3 111.8(4) . . ? C27 N4 H4B 124.1 . . ? N3 N4 H4B 124.1 . . ? C16 O1 Cd1 108.1(3) . . ? C17 O3 Cd1 88.5(3) . 4_685 ? C17 O4 Cd1 92.2(3) . 4_685 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.04 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.298 _refine_diff_density_min -1.032 _refine_diff_density_rms 0.090 # Attachment '- 2.cif' data_m2 _database_code_depnum_ccdc_archive 'CCDC 803529' #TrackingRef '- 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C30 H32 Cd N4 O4' _chemical_formula_sum 'C30 H32 Cd N4 O4' _chemical_formula_weight 625.00 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 Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.5219(7) _cell_length_b 12.2292(7) _cell_length_c 17.7853(10) _cell_angle_alpha 90.00 _cell_angle_beta 96.4210(10) _cell_angle_gamma 90.00 _cell_volume 2706.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 185(2) _cell_measurement_reflns_used 5374 _cell_measurement_theta_min 1.89 _cell_measurement_theta_max 26.10 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.534 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1280 _exptl_absorpt_coefficient_mu 0.850 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8416 _exptl_absorpt_correction_T_max 0.9123 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 185(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 9.00cm _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 17980 _diffrn_reflns_av_R_equivalents 0.0627 _diffrn_reflns_av_sigmaI/netI 0.0668 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 26.10 _reflns_number_total 5374 _reflns_number_gt 3661 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXP-97 _computing_publication_material 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^)+(0.0574P)^2^+1.0407P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5374 _refine_ls_number_parameters 360 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0830 _refine_ls_R_factor_gt 0.0485 _refine_ls_wR_factor_ref 0.1239 _refine_ls_wR_factor_gt 0.1086 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _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 0.11001(3) 0.35216(3) 0.05144(2) 0.03381(14) Uani 1 1 d . . . C1 C 0.2802(4) 0.5891(4) -0.1323(3) 0.0307(11) Uani 1 1 d . . . H1A H 0.2051 0.6008 -0.1330 0.037 Uiso 1 1 calc R . . C2 C 0.3306(4) 0.5026(4) -0.0902(3) 0.0314(11) Uani 1 1 d . . . C3 C 0.4409(4) 0.4852(4) -0.0908(3) 0.0381(12) Uani 1 1 d . . . H3A H 0.4740 0.4239 -0.0650 0.046 Uiso 1 1 calc R . . C4 C 0.5018(4) 0.5556(4) -0.1283(3) 0.0357(11) Uani 1 1 d . . . H4A H 0.5771 0.5447 -0.1269 0.043 Uiso 1 1 calc R . . C5 C 0.6044(4) 0.7543(4) -0.2168(3) 0.0309(11) Uani 1 1 d . . . H5A H 0.6609 0.7092 -0.1941 0.037 Uiso 1 1 calc R . . C6 C 0.6266(4) 0.8455(4) -0.2586(3) 0.0306(10) Uani 1 1 d . . . H6A H 0.6992 0.8622 -0.2647 0.037 Uiso 1 1 calc R . . C7 C 0.5460(4) 0.9128(4) -0.2916(3) 0.0310(11) Uani 1 1 d . . . C8 C 0.4390(4) 0.8881(4) -0.2841(3) 0.0340(11) Uani 1 1 d . . . H8A H 0.3827 0.9324 -0.3078 0.041 Uiso 1 1 calc R . . C9 C 0.3058(3) 0.7530(4) -0.2246(3) 0.0311(11) Uani 1 1 d . . . C10 C 0.3403(4) 0.6564(4) -0.1724(3) 0.0287(10) Uani 1 1 d . . . C11 C 0.4526(4) 0.6423(4) -0.1680(2) 0.0289(10) Uani 1 1 d . . . C12 C 0.4991(4) 0.7304(4) -0.2089(2) 0.0271(10) Uani 1 1 d . . . C13 C 0.4156(4) 0.7970(4) -0.2411(3) 0.0311(11) Uani 1 1 d . . . C14 C 0.2435(4) 0.7134(4) -0.3003(3) 0.0404(13) Uani 1 1 d . . . H14A H 0.2435 0.7737 -0.3374 0.048 Uiso 1 1 calc R . . H14B H 0.2843 0.6520 -0.3195 0.048 Uiso 1 1 calc R . . C15 C 0.1289(4) 0.6763(5) -0.2987(3) 0.0589(17) Uani 1 1 d . . . H15A H 0.0992 0.6528 -0.3495 0.088 Uiso 1 1 calc R . . H15B H 0.0859 0.7369 -0.2822 0.088 Uiso 1 1 calc R . . H15C H 0.1270 0.6150 -0.2634 0.088 Uiso 1 1 calc R . . C16 C 0.2396(4) 0.8377(4) -0.1873(3) 0.0413(13) Uani 1 1 d . . . H16A H 0.2200 0.8971 -0.2241 0.050 Uiso 1 1 calc R . . H16B H 0.1721 0.8029 -0.1755 0.050 Uiso 1 1 calc R . . C17 C 0.2942(5) 0.8868(5) -0.1168(3) 0.0543(15) Uani 1 1 d . . . H17A H 0.2465 0.9404 -0.0969 0.082 Uiso 1 1 calc R . . H17B H 0.3604 0.9231 -0.1279 0.082 Uiso 1 1 calc R . . H17C H 0.3117 0.8292 -0.0792 0.082 Uiso 1 1 calc R . . C18 C 0.2705(5) 0.4299(4) -0.0417(3) 0.0371(12) Uani 1 1 d . . . C19 C 0.5738(4) 1.0079(4) -0.3391(3) 0.0362(12) Uani 1 1 d . . . C20 C 0.0523(4) 0.1264(4) 0.1683(3) 0.0492(15) Uani 1 1 d . . . H20A H 0.0256 0.2014 0.1606 0.074 Uiso 1 1 calc R . . H20B H 0.0728 0.1137 0.2224 0.074 Uiso 1 1 calc R . . H20C H -0.0043 0.0747 0.1495 0.074 Uiso 1 1 calc R . . C21 C 0.1468(4) 0.1105(4) 0.1267(3) 0.0322(11) Uani 1 1 d . . . C22 C 0.2116(3) 0.0179(4) 0.1202(3) 0.0279(10) Uani 1 1 d . . . C23 C 0.2924(4) 0.0528(4) 0.0790(3) 0.0318(11) Uani 1 1 d . . . C24 C 0.3924(4) -0.0026(4) 0.0615(3) 0.0471(14) Uani 1 1 d . . . H24A H 0.4320 0.0458 0.0306 0.071 Uiso 1 1 calc R . . H24B H 0.3738 -0.0703 0.0336 0.071 Uiso 1 1 calc R . . H24C H 0.4373 -0.0198 0.1087 0.071 Uiso 1 1 calc R . . C25 C 0.1995(5) -0.0945(4) 0.1516(3) 0.0359(12) Uani 1 1 d . . . C26 C -0.0466(4) -0.1191(4) 0.0760(3) 0.0392(12) Uani 1 1 d . . . H26A H -0.1110 -0.1466 0.0455 0.059 Uiso 1 1 calc R . . H26B H -0.0327 -0.0437 0.0610 0.059 Uiso 1 1 calc R . . H26C H -0.0577 -0.1208 0.1296 0.059 Uiso 1 1 calc R . . C27 C 0.0471(4) -0.1892(4) 0.0634(3) 0.0320(11) Uani 1 1 d . . . C28 C 0.1550(4) -0.1787(4) 0.0955(3) 0.0312(11) Uani 1 1 d . . . C29 C 0.2071(4) -0.2668(4) 0.0670(3) 0.0360(12) Uani 1 1 d . . . C30 C 0.3204(4) -0.3065(4) 0.0829(4) 0.0509(15) Uani 1 1 d . . . H30A H 0.3299 -0.3721 0.0527 0.076 Uiso 1 1 calc R . . H30B H 0.3358 -0.3240 0.1368 0.076 Uiso 1 1 calc R . . H30C H 0.3698 -0.2493 0.0695 0.076 Uiso 1 1 calc R . . N1 N 0.1846(3) 0.1952(3) 0.0899(2) 0.0308(9) Uani 1 1 d . . . N2 N 0.2730(3) 0.1569(3) 0.0613(2) 0.0335(9) Uani 1 1 d . . . H2A H 0.3131 0.1965 0.0342 0.040 Uiso 1 1 calc R . . N3 N 0.0357(3) -0.2766(3) 0.0179(2) 0.0321(9) Uani 1 1 d . . . N4 N 0.1346(3) -0.3216(3) 0.0208(2) 0.0358(10) Uani 1 1 d . . . H4B H 0.1495 -0.3802 -0.0048 0.043 Uiso 1 1 calc R . . O1 O 0.1790(3) 0.4642(3) -0.0270(2) 0.0479(9) Uani 1 1 d . . . O2 O 0.3094(3) 0.3425(3) -0.0178(2) 0.0560(11) Uani 1 1 d . . . O3 O 0.6700(3) 1.0245(3) -0.3483(2) 0.0462(9) Uani 1 1 d . . . O4 O 0.4998(3) 1.0650(3) -0.3717(2) 0.0557(11) Uani 1 1 d . . . H25A H 0.156(4) -0.093(4) 0.188(3) 0.043(16) Uiso 1 1 d . . . H25B H 0.278(4) -0.114(4) 0.172(3) 0.038(14) Uiso 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 Cd1 0.0363(2) 0.02461(19) 0.0422(2) -0.00358(17) 0.01187(16) -0.00112(17) C1 0.034(3) 0.031(3) 0.028(3) -0.002(2) 0.006(2) -0.001(2) C2 0.045(3) 0.021(2) 0.029(3) -0.002(2) 0.005(2) -0.008(2) C3 0.054(3) 0.026(2) 0.033(3) 0.005(2) -0.001(2) 0.007(2) C4 0.036(3) 0.032(3) 0.039(3) 0.003(2) 0.006(2) 0.004(2) C5 0.032(3) 0.030(3) 0.031(3) 0.000(2) 0.003(2) 0.003(2) C6 0.027(2) 0.033(3) 0.033(3) -0.008(2) 0.008(2) -0.006(2) C7 0.037(3) 0.027(2) 0.030(3) -0.004(2) 0.011(2) -0.003(2) C8 0.034(3) 0.030(2) 0.039(3) 0.006(2) 0.005(2) 0.003(2) C9 0.025(2) 0.031(2) 0.040(3) 0.009(2) 0.011(2) 0.002(2) C10 0.036(3) 0.025(2) 0.025(2) -0.003(2) 0.005(2) 0.000(2) C11 0.036(3) 0.026(2) 0.026(2) 0.003(2) 0.006(2) 0.000(2) C12 0.032(3) 0.028(2) 0.022(2) -0.0029(19) 0.0020(19) 0.000(2) C13 0.033(3) 0.026(2) 0.035(3) 0.001(2) 0.006(2) 0.000(2) C14 0.037(3) 0.048(3) 0.036(3) 0.012(2) 0.001(2) 0.000(2) C15 0.049(4) 0.071(4) 0.055(4) 0.002(3) -0.001(3) -0.009(3) C16 0.035(3) 0.037(3) 0.052(3) 0.009(3) 0.011(3) 0.002(2) C17 0.052(4) 0.054(3) 0.060(4) -0.002(3) 0.017(3) 0.003(3) C18 0.057(3) 0.027(3) 0.026(3) -0.007(2) 0.002(2) -0.010(2) C19 0.038(3) 0.035(3) 0.037(3) -0.003(2) 0.011(2) -0.005(2) C20 0.043(3) 0.039(3) 0.071(4) -0.001(3) 0.029(3) 0.003(3) C21 0.031(3) 0.032(2) 0.034(3) -0.001(2) 0.003(2) -0.004(2) C22 0.027(2) 0.028(2) 0.028(3) -0.005(2) 0.001(2) -0.001(2) C23 0.028(3) 0.027(2) 0.041(3) -0.008(2) 0.006(2) -0.001(2) C24 0.037(3) 0.046(3) 0.061(4) -0.004(3) 0.017(3) 0.005(3) C25 0.037(3) 0.033(3) 0.037(3) 0.004(2) 0.003(3) -0.004(2) C26 0.032(3) 0.045(3) 0.042(3) -0.010(2) 0.008(2) 0.002(2) C27 0.040(3) 0.030(2) 0.028(3) 0.002(2) 0.010(2) -0.003(2) C28 0.039(3) 0.024(2) 0.032(3) 0.007(2) 0.008(2) -0.002(2) C29 0.034(3) 0.030(3) 0.045(3) 0.007(2) 0.008(2) 0.001(2) C30 0.047(3) 0.033(3) 0.072(4) 0.001(3) 0.005(3) 0.014(3) N1 0.031(2) 0.028(2) 0.035(2) -0.0014(18) 0.0094(18) -0.0015(18) N2 0.031(2) 0.037(2) 0.034(2) -0.0021(19) 0.0123(18) -0.0058(19) N3 0.035(2) 0.028(2) 0.035(2) -0.0023(18) 0.0084(18) 0.0026(18) N4 0.037(2) 0.026(2) 0.046(3) -0.0006(19) 0.014(2) 0.0052(18) O1 0.069(3) 0.0315(19) 0.047(2) 0.0033(17) 0.022(2) -0.0103(19) O2 0.081(3) 0.031(2) 0.056(3) 0.0147(18) 0.005(2) -0.006(2) O3 0.044(2) 0.045(2) 0.050(2) 0.0114(18) 0.0107(18) -0.0039(18) O4 0.040(2) 0.054(2) 0.074(3) 0.036(2) 0.017(2) 0.0045(19) _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 O1 2.200(3) . ? Cd1 N1 2.209(4) . ? Cd1 N3 2.280(4) 3 ? Cd1 O4 2.285(3) 4_576 ? Cd1 O3 2.391(3) 4_576 ? Cd1 C19 2.668(5) 4_576 ? C1 C10 1.368(6) . ? C1 C2 1.404(6) . ? C1 H1A 0.9500 . ? C2 C3 1.399(7) . ? C2 C18 1.499(7) . ? C3 C4 1.370(7) . ? C3 H3A 0.9500 . ? C4 C11 1.380(6) . ? C4 H4A 0.9500 . ? C5 C12 1.373(6) . ? C5 C6 1.386(6) . ? C5 H5A 0.9500 . ? C6 C7 1.382(6) . ? C6 H6A 0.9500 . ? C7 C8 1.394(6) . ? C7 C19 1.502(7) . ? C8 C13 1.400(6) . ? C8 H8A 0.9500 . ? C9 C16 1.524(6) . ? C9 C10 1.534(6) . ? C9 C13 1.535(6) . ? C9 C14 1.556(7) . ? C10 C11 1.410(6) . ? C11 C12 1.458(6) . ? C12 C13 1.397(6) . ? C14 C15 1.509(7) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.486(8) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 O2 1.231(6) . ? C18 O1 1.275(6) . ? C19 O3 1.250(6) . ? C19 O4 1.250(6) . ? C19 Cd1 2.668(5) 4_675 ? C20 C21 1.478(7) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 N1 1.339(6) . ? C21 C22 1.406(6) . ? C22 C23 1.381(6) . ? C22 C25 1.497(6) . ? C23 N2 1.327(6) . ? C23 C24 1.488(6) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C28 1.497(7) . ? C25 H25A 0.88(5) . ? C25 H25B 1.03(5) . ? C26 C27 1.490(6) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 N3 1.339(6) . ? C27 C28 1.412(7) . ? C28 C29 1.385(6) . ? C29 N4 1.335(6) . ? C29 C30 1.496(7) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? N1 N2 1.352(5) . ? N2 H2A 0.8800 . ? N3 N4 1.351(5) . ? N3 Cd1 2.280(4) 3 ? N4 H4B 0.8800 . ? O3 Cd1 2.391(3) 4_675 ? O4 Cd1 2.285(3) 4_675 ? 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 Cd1 N1 123.73(14) . . ? O1 Cd1 N3 104.90(14) . 3 ? N1 Cd1 N3 95.74(14) . 3 ? O1 Cd1 O4 114.15(15) . 4_576 ? N1 Cd1 O4 117.56(15) . 4_576 ? N3 Cd1 O4 90.17(13) 3 4_576 ? O1 Cd1 O3 88.11(13) . 4_576 ? N1 Cd1 O3 103.33(13) . 4_576 ? N3 Cd1 O3 145.52(12) 3 4_576 ? O4 Cd1 O3 55.56(12) 4_576 4_576 ? O1 Cd1 C19 99.98(14) . 4_576 ? N1 Cd1 C19 115.60(14) . 4_576 ? N3 Cd1 C19 117.61(15) 3 4_576 ? O4 Cd1 C19 27.88(13) 4_576 4_576 ? O3 Cd1 C19 27.91(13) 4_576 4_576 ? C10 C1 C2 119.3(4) . . ? C10 C1 H1A 120.4 . . ? C2 C1 H1A 120.4 . . ? C3 C2 C1 119.8(4) . . ? C3 C2 C18 118.3(4) . . ? C1 C2 C18 121.9(4) . . ? C4 C3 C2 120.8(4) . . ? C4 C3 H3A 119.6 . . ? C2 C3 H3A 119.6 . . ? C3 C4 C11 119.4(4) . . ? C3 C4 H4A 120.3 . . ? C11 C4 H4A 120.3 . . ? C12 C5 C6 118.6(4) . . ? C12 C5 H5A 120.7 . . ? C6 C5 H5A 120.7 . . ? C7 C6 C5 121.8(4) . . ? C7 C6 H6A 119.1 . . ? C5 C6 H6A 119.1 . . ? C6 C7 C8 119.6(4) . . ? C6 C7 C19 119.7(4) . . ? C8 C7 C19 120.5(4) . . ? C7 C8 C13 119.1(4) . . ? C7 C8 H8A 120.4 . . ? C13 C8 H8A 120.4 . . ? C16 C9 C10 113.0(4) . . ? C16 C9 C13 112.8(4) . . ? C10 C9 C13 100.8(4) . . ? C16 C9 C14 110.1(4) . . ? C10 C9 C14 111.3(4) . . ? C13 C9 C14 108.5(4) . . ? C1 C10 C11 120.1(4) . . ? C1 C10 C9 130.1(4) . . ? C11 C10 C9 109.9(4) . . ? C4 C11 C10 120.5(4) . . ? C4 C11 C12 130.1(4) . . ? C10 C11 C12 109.4(4) . . ? C5 C12 C13 121.2(4) . . ? C5 C12 C11 130.5(4) . . ? C13 C12 C11 108.2(4) . . ? C12 C13 C8 119.6(4) . . ? C12 C13 C9 111.3(4) . . ? C8 C13 C9 129.0(4) . . ? C15 C14 C9 117.6(4) . . ? C15 C14 H14A 107.9 . . ? C9 C14 H14A 107.9 . . ? C15 C14 H14B 107.9 . . ? C9 C14 H14B 107.9 . . ? H14A C14 H14B 107.2 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C9 114.8(4) . . ? C17 C16 H16A 108.6 . . ? C9 C16 H16A 108.6 . . ? C17 C16 H16B 108.6 . . ? C9 C16 H16B 108.6 . . ? H16A C16 H16B 107.5 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O2 C18 O1 123.0(5) . . ? O2 C18 C2 120.6(5) . . ? O1 C18 C2 116.3(4) . . ? O3 C19 O4 121.6(5) . . ? O3 C19 C7 119.2(5) . . ? O4 C19 C7 119.1(4) . . ? O3 C19 Cd1 63.6(3) . 4_675 ? O4 C19 Cd1 58.7(2) . 4_675 ? C7 C19 Cd1 167.6(3) . 4_675 ? C21 C20 H20A 109.5 . . ? C21 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C21 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N1 C21 C22 110.2(4) . . ? N1 C21 C20 119.3(4) . . ? C22 C21 C20 130.5(4) . . ? C23 C22 C21 104.9(4) . . ? C23 C22 C25 126.3(4) . . ? C21 C22 C25 128.8(4) . . ? N2 C23 C22 107.3(4) . . ? N2 C23 C24 121.5(4) . . ? C22 C23 C24 130.8(5) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C28 C25 C22 115.4(4) . . ? C28 C25 H25A 107(3) . . ? C22 C25 H25A 110(3) . . ? C28 C25 H25B 110(3) . . ? C22 C25 H25B 102(3) . . ? H25A C25 H25B 113(4) . . ? C27 C26 H26A 109.5 . . ? C27 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C27 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N3 C27 C28 110.5(4) . . ? N3 C27 C26 121.1(4) . . ? C28 C27 C26 128.4(4) . . ? C29 C28 C27 104.5(4) . . ? C29 C28 C25 128.5(5) . . ? C27 C28 C25 126.9(4) . . ? N4 C29 C28 107.4(4) . . ? N4 C29 C30 121.3(4) . . ? C28 C29 C30 131.2(5) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C21 N1 N2 105.3(4) . . ? C21 N1 Cd1 131.5(3) . . ? N2 N1 Cd1 121.3(3) . . ? C23 N2 N1 112.2(4) . . ? C23 N2 H2A 123.9 . . ? N1 N2 H2A 123.9 . . ? C27 N3 N4 105.5(4) . . ? C27 N3 Cd1 132.5(3) . 3 ? N4 N3 Cd1 122.0(3) . 3 ? C29 N4 N3 112.1(4) . . ? C29 N4 H4B 123.9 . . ? N3 N4 H4B 123.9 . . ? C18 O1 Cd1 110.5(3) . . ? C19 O3 Cd1 88.5(3) . 4_675 ? C19 O4 Cd1 93.4(3) . 4_675 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.10 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.086 _refine_diff_density_min -0.787 _refine_diff_density_rms 0.100 # Attachment '- 3.cif' data_m3 _database_code_depnum_ccdc_archive 'CCDC 803530' #TrackingRef '- 3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C49 H43 N5 O10 Zn2' _chemical_formula_sum 'C49 H43 N5 O10 Zn2' _chemical_formula_weight 992.62 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.7713(8) _cell_length_b 18.1647(16) _cell_length_c 15.8994(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.0041 _cell_angle_gamma 90.00 _cell_volume 2533.2(4) _cell_formula_units_Z 2 _cell_measurement_temperature 185(2) _cell_measurement_reflns_used 4990 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 26.05 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.301 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1024 _exptl_absorpt_coefficient_mu 1.005 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8091 _exptl_absorpt_correction_T_max 0.8975 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 185(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 9.00cm _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 13791 _diffrn_reflns_av_R_equivalents 0.0419 _diffrn_reflns_av_sigmaI/netI 0.0461 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 26.05 _reflns_number_total 4990 _reflns_number_gt 3875 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXP-97 _computing_publication_material 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^)+(0.0858P)^2^+3.2664P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4990 _refine_ls_number_parameters 301 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0693 _refine_ls_R_factor_gt 0.0528 _refine_ls_wR_factor_ref 0.1609 _refine_ls_wR_factor_gt 0.1480 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.097 _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 Zn1 Zn 0.38676(4) 0.51923(2) 0.43292(2) 0.01753(16) Uani 1 1 d . . . C1 C 0.8550(4) 0.3236(2) 0.3668(2) 0.0262(8) Uani 1 1 d . . . H1A H 0.9017 0.3338 0.4195 0.031 Uiso 1 1 calc R . . C2 C 0.7117(4) 0.3518(2) 0.3489(2) 0.0287(9) Uani 1 1 d . . . C3 C 0.6426(5) 0.3356(3) 0.2724(3) 0.0535(15) Uani 1 1 d . . . H3A H 0.5451 0.3555 0.2597 0.064 Uiso 1 1 calc R . . C4 C 0.7151(6) 0.2907(4) 0.2148(3) 0.0651(18) Uani 1 1 d U . . H4A H 0.6660 0.2783 0.1634 0.078 Uiso 1 1 calc R . . C5 C 0.9407(5) 0.1852(3) 0.1030(3) 0.0459(13) Uani 1 1 d . . . H5A H 0.8484 0.1916 0.0726 0.055 Uiso 1 1 calc R . . C6 C 1.0585(5) 0.1439(3) 0.0707(3) 0.0369(10) Uani 1 1 d . . . H6A H 1.0458 0.1207 0.0175 0.044 Uiso 1 1 calc R . . C7 C 1.1954(4) 0.1350(2) 0.1134(2) 0.0254(8) Uani 1 1 d . . . C8 C 1.2141(4) 0.1662(2) 0.1935(2) 0.0263(8) Uani 1 1 d . . . H8A H 1.3062 0.1594 0.2239 0.032 Uiso 1 1 calc R . . C9 C 1.0877(4) 0.2456(2) 0.3125(2) 0.0281(9) Uani 1 1 d . . . C10 C 0.9305(4) 0.2803(2) 0.3080(2) 0.0275(9) Uani 1 1 d . . . C11 C 0.8586(5) 0.2640(3) 0.2319(3) 0.0386(11) Uani 1 1 d . . . C12 C 0.9615(5) 0.2174(3) 0.1824(3) 0.0335(10) Uani 1 1 d . . . C13 C 1.0966(4) 0.2069(2) 0.2272(2) 0.0260(8) Uani 1 1 d . . . C14 C 1.0947(6) 0.1902(3) 0.3844(3) 0.0462(13) Uani 1 1 d . . . H14A H 1.0131 0.1538 0.3777 0.069 Uiso 1 1 calc R . . H14B H 1.0818 0.2159 0.4381 0.069 Uiso 1 1 calc R . . H14C H 1.1937 0.1652 0.3837 0.069 Uiso 1 1 calc R . . C15 C 1.2138(5) 0.3035(3) 0.3206(3) 0.0458(13) Uani 1 1 d . . . H15A H 1.2066 0.3384 0.2737 0.069 Uiso 1 1 calc R . . H15B H 1.3135 0.2792 0.3194 0.069 Uiso 1 1 calc R . . H15C H 1.2019 0.3301 0.3739 0.069 Uiso 1 1 calc R . . C16 C 0.6331(4) 0.4005(2) 0.4106(2) 0.0247(8) Uani 1 1 d . . . C17 C 1.3184(4) 0.0903(2) 0.0738(2) 0.0243(8) Uani 1 1 d . . . C18 C 0.0991(5) 0.4972(2) 0.3325(3) 0.0300(9) Uani 1 1 d . . . H18A H 0.0539 0.4861 0.3853 0.036 Uiso 1 1 calc R . . C19 C 0.0112(5) 0.4893(3) 0.2602(3) 0.0344(10) Uani 1 1 d . . . H19A H -0.0920 0.4737 0.2639 0.041 Uiso 1 1 calc R . . C20 C 0.0764(5) 0.5043(2) 0.1830(2) 0.0302(9) Uani 1 1 d . . . C21 C 0.2258(6) 0.5281(3) 0.1816(3) 0.0535(16) Uani 1 1 d . . . H21A H 0.2737 0.5397 0.1296 0.064 Uiso 1 1 calc R . . C22 C 0.3046(5) 0.5350(3) 0.2557(3) 0.0477(14) Uani 1 1 d . . . H22A H 0.4073 0.5514 0.2536 0.057 Uiso 1 1 calc R . . C23 C -0.0114(5) 0.4944(3) 0.1048(3) 0.0359(10) Uani 1 1 d . . . H23A H -0.1149 0.4792 0.1076 0.043 Uiso 1 1 calc R . . N1 N 0.2435(4) 0.51954(17) 0.33107(19) 0.0225(7) Uani 1 1 d . . . N2 N 0.0502(4) 0.5060(2) 0.0338(2) 0.0430(10) Uani 1 1 d . . . O1 O 0.6881(3) 0.40445(16) 0.48401(16) 0.0349(7) Uani 1 1 d . . . O2 O 0.5189(3) 0.43578(17) 0.38475(18) 0.0351(7) Uani 1 1 d . . . O3 O 1.2830(3) 0.05666(17) 0.00713(17) 0.0370(7) Uani 1 1 d . . . O4 O 1.4467(3) 0.08817(16) 0.10856(18) 0.0331(7) Uani 1 1 d . . . C24 C 0.5123(14) 0.2807(9) -0.0183(8) 0.0794(16) Uani 0.50 1 d P . . H24A H 0.5694 0.2925 -0.0695 0.119 Uiso 0.50 1 calc PR . . H24B H 0.4370 0.2424 -0.0307 0.119 Uiso 0.50 1 calc PR . . H24C H 0.5828 0.2630 0.0250 0.119 Uiso 0.50 1 calc PR . . C25 C 0.3464(14) 0.3372(9) 0.0860(7) 0.0794(16) Uani 0.50 1 d P . . H25A H 0.3018 0.3845 0.1023 0.119 Uiso 0.50 1 calc PR . . H25B H 0.4119 0.3191 0.1315 0.119 Uiso 0.50 1 calc PR . . H25C H 0.2648 0.3015 0.0755 0.119 Uiso 0.50 1 calc PR . . C26 C 0.4173(14) 0.4110(10) -0.0293(8) 0.0794(16) Uani 0.50 1 d P . . H26A H 0.3590 0.4479 -0.0018 0.095 Uiso 0.50 1 calc PR . . N3 N 0.4346(12) 0.3464(8) 0.0118(6) 0.0794(16) Uani 0.50 1 d P . . O5 O 0.4669(9) 0.4259(6) -0.0953(5) 0.0794(16) Uani 0.50 1 d P . . O1W O -0.3537(17) 0.4828(11) 0.2013(12) 0.053(5) Uani 0.20 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 Zn1 0.0173(2) 0.0225(3) 0.0128(2) 0.00060(16) -0.00180(15) 0.00000(16) C1 0.0273(19) 0.031(2) 0.0197(18) -0.0043(16) -0.0018(15) 0.0029(17) C2 0.026(2) 0.036(2) 0.024(2) -0.0068(17) 0.0007(16) 0.0063(17) C3 0.033(2) 0.092(4) 0.036(3) -0.027(3) -0.010(2) 0.032(3) C4 0.043(3) 0.113(5) 0.039(3) -0.042(3) -0.023(2) 0.039(3) C5 0.038(2) 0.072(4) 0.028(2) -0.018(2) -0.0133(19) 0.026(2) C6 0.037(2) 0.051(3) 0.023(2) -0.0119(19) -0.0054(17) 0.013(2) C7 0.0279(19) 0.027(2) 0.0215(19) -0.0003(16) 0.0023(15) 0.0043(16) C8 0.0239(19) 0.030(2) 0.024(2) -0.0031(16) -0.0037(15) 0.0051(16) C9 0.0253(19) 0.035(2) 0.024(2) -0.0113(17) -0.0059(15) 0.0107(17) C10 0.026(2) 0.033(2) 0.0231(19) -0.0048(17) -0.0016(15) 0.0025(17) C11 0.032(2) 0.055(3) 0.029(2) -0.019(2) -0.0076(18) 0.015(2) C12 0.027(2) 0.047(3) 0.026(2) -0.0149(19) -0.0049(16) 0.0140(19) C13 0.0242(19) 0.029(2) 0.025(2) -0.0079(16) -0.0020(15) 0.0043(16) C14 0.058(3) 0.052(3) 0.029(2) -0.008(2) -0.007(2) 0.028(2) C15 0.026(2) 0.054(3) 0.057(3) -0.029(3) -0.006(2) 0.004(2) C16 0.0242(19) 0.028(2) 0.0223(19) -0.0019(16) 0.0027(15) 0.0014(16) C17 0.0278(19) 0.025(2) 0.0204(18) 0.0015(16) 0.0028(15) 0.0052(16) C18 0.028(2) 0.041(2) 0.022(2) 0.0051(17) -0.0045(16) -0.0029(18) C19 0.025(2) 0.049(3) 0.029(2) 0.000(2) -0.0046(17) -0.0081(19) C20 0.033(2) 0.039(2) 0.0185(19) 0.0006(17) -0.0068(16) 0.0001(18) C21 0.040(3) 0.104(5) 0.016(2) 0.006(2) -0.0023(18) -0.027(3) C22 0.032(2) 0.091(4) 0.020(2) 0.006(2) -0.0029(18) -0.024(2) C23 0.032(2) 0.050(3) 0.026(2) 0.0012(19) -0.0095(18) -0.005(2) N1 0.0227(16) 0.0288(18) 0.0159(15) 0.0009(13) -0.0038(12) 0.0003(13) N2 0.038(2) 0.069(3) 0.0216(19) -0.0031(18) -0.0113(16) -0.0038(19) O1 0.0437(17) 0.0403(17) 0.0207(14) -0.0081(13) -0.0008(12) 0.0166(14) O2 0.0318(15) 0.0391(17) 0.0345(16) -0.0113(14) -0.0064(12) 0.0162(13) O3 0.0385(17) 0.0442(18) 0.0283(15) -0.0134(14) -0.0019(12) 0.0178(14) O4 0.0266(14) 0.0388(17) 0.0339(15) -0.0105(13) -0.0015(12) 0.0098(13) C24 0.053(3) 0.131(5) 0.054(3) -0.010(3) 0.002(2) -0.013(3) C25 0.053(3) 0.131(5) 0.054(3) -0.010(3) 0.002(2) -0.013(3) C26 0.053(3) 0.131(5) 0.054(3) -0.010(3) 0.002(2) -0.013(3) N3 0.053(3) 0.131(5) 0.054(3) -0.010(3) 0.002(2) -0.013(3) O5 0.053(3) 0.131(5) 0.054(3) -0.010(3) 0.002(2) -0.013(3) O1W 0.021(8) 0.083(14) 0.055(11) 0.003(9) 0.018(7) 0.003(8) _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 Zn1 O1 2.024(3) 3_666 ? Zn1 O3 2.030(3) 4_466 ? Zn1 O4 2.034(3) 2_755 ? Zn1 N1 2.050(3) . ? Zn1 O2 2.056(3) . ? Zn1 Zn1 2.9974(8) 3_666 ? C1 C2 1.388(5) . ? C1 C10 1.389(5) . ? C1 H1A 0.9500 . ? C2 C3 1.390(6) . ? C2 C16 1.490(5) . ? C3 C4 1.382(6) . ? C3 H3A 0.9500 . ? C4 C11 1.377(6) . ? C4 H4A 0.9500 . ? C5 C6 1.377(6) . ? C5 C12 1.403(6) . ? C5 H5A 0.9500 . ? C6 C7 1.389(6) . ? C6 H6A 0.9500 . ? C7 C8 1.403(5) . ? C7 C17 1.490(5) . ? C8 C13 1.377(5) . ? C8 H8A 0.9500 . ? C9 C10 1.519(5) . ? C9 C14 1.525(6) . ? C9 C13 1.529(5) . ? C9 C15 1.533(6) . ? C10 C11 1.396(5) . ? C11 C12 1.466(5) . ? C12 C13 1.396(5) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 O2 1.259(5) . ? C16 O1 1.264(4) . ? C17 O4 1.254(5) . ? C17 O3 1.263(5) . ? C18 N1 1.330(5) . ? C18 C19 1.392(6) . ? C18 H18A 0.9500 . ? C19 C20 1.381(6) . ? C19 H19A 0.9500 . ? C20 C21 1.380(6) . ? C20 C23 1.473(6) . ? C21 C22 1.372(6) . ? C21 H21A 0.9500 . ? C22 N1 1.342(5) . ? C22 H22A 0.9500 . ? C23 N2 1.270(6) . ? C23 H23A 0.9500 . ? N2 N2 1.405(7) 3_565 ? O1 Zn1 2.024(3) 3_666 ? O3 Zn1 2.030(3) 4_665 ? O4 Zn1 2.034(3) 2_745 ? C24 N3 1.455(18) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 N3 1.421(15) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 O5 1.168(14) . ? C26 N3 1.351(19) . ? C26 H26A 0.9500 . ? 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 Zn1 O3 86.59(13) 3_666 4_466 ? O1 Zn1 O4 91.30(13) 3_666 2_755 ? O3 Zn1 O4 158.21(12) 4_466 2_755 ? O1 Zn1 N1 108.36(12) 3_666 . ? O3 Zn1 N1 100.73(12) 4_466 . ? O4 Zn1 N1 100.51(12) 2_755 . ? O1 Zn1 O2 158.56(11) 3_666 . ? O3 Zn1 O2 88.21(13) 4_466 . ? O4 Zn1 O2 85.89(13) 2_755 . ? N1 Zn1 O2 93.05(12) . . ? O1 Zn1 Zn1 84.84(8) 3_666 3_666 ? O3 Zn1 Zn1 74.06(8) 4_466 3_666 ? O4 Zn1 Zn1 84.15(8) 2_755 3_666 ? N1 Zn1 Zn1 165.74(9) . 3_666 ? O2 Zn1 Zn1 73.73(8) . 3_666 ? C2 C1 C10 120.2(3) . . ? C2 C1 H1A 119.9 . . ? C10 C1 H1A 119.9 . . ? C1 C2 C3 119.8(4) . . ? C1 C2 C16 120.2(3) . . ? C3 C2 C16 120.0(4) . . ? C4 C3 C2 120.3(4) . . ? C4 C3 H3A 119.8 . . ? C2 C3 H3A 119.8 . . ? C11 C4 C3 119.8(4) . . ? C11 C4 H4A 120.1 . . ? C3 C4 H4A 120.1 . . ? C6 C5 C12 117.8(4) . . ? C6 C5 H5A 121.1 . . ? C12 C5 H5A 121.1 . . ? C5 C6 C7 121.9(4) . . ? C5 C6 H6A 119.0 . . ? C7 C6 H6A 119.0 . . ? C6 C7 C8 119.9(4) . . ? C6 C7 C17 118.8(3) . . ? C8 C7 C17 121.3(3) . . ? C13 C8 C7 118.9(4) . . ? C13 C8 H8A 120.6 . . ? C7 C8 H8A 120.6 . . ? C10 C9 C14 110.3(3) . . ? C10 C9 C13 101.3(3) . . ? C14 C9 C13 111.1(3) . . ? C10 C9 C15 112.0(3) . . ? C14 C9 C15 111.2(4) . . ? C13 C9 C15 110.7(3) . . ? C1 C10 C11 119.3(4) . . ? C1 C10 C9 129.5(3) . . ? C11 C10 C9 111.2(3) . . ? C4 C11 C10 120.6(4) . . ? C4 C11 C12 131.3(4) . . ? C10 C11 C12 108.1(3) . . ? C13 C12 C5 120.9(4) . . ? C13 C12 C11 109.1(3) . . ? C5 C12 C11 130.1(4) . . ? C8 C13 C12 120.6(3) . . ? C8 C13 C9 129.1(3) . . ? C12 C13 C9 110.3(3) . . ? C9 C14 H14A 109.5 . . ? C9 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C9 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C9 C15 H15A 109.5 . . ? C9 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C9 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O2 C16 O1 125.2(3) . . ? O2 C16 C2 117.1(3) . . ? O1 C16 C2 117.7(3) . . ? O4 C17 O3 125.2(4) . . ? O4 C17 C7 118.7(3) . . ? O3 C17 C7 116.1(3) . . ? N1 C18 C19 123.0(4) . . ? N1 C18 H18A 118.5 . . ? C19 C18 H18A 118.5 . . ? C20 C19 C18 119.0(4) . . ? C20 C19 H19A 120.5 . . ? C18 C19 H19A 120.5 . . ? C21 C20 C19 118.0(4) . . ? C21 C20 C23 121.4(4) . . ? C19 C20 C23 120.6(4) . . ? C22 C21 C20 119.5(4) . . ? C22 C21 H21A 120.2 . . ? C20 C21 H21A 120.2 . . ? N1 C22 C21 123.2(4) . . ? N1 C22 H22A 118.4 . . ? C21 C22 H22A 118.4 . . ? N2 C23 C20 120.5(4) . . ? N2 C23 H23A 119.7 . . ? C20 C23 H23A 119.7 . . ? C18 N1 C22 117.3(3) . . ? C18 N1 Zn1 124.7(3) . . ? C22 N1 Zn1 117.5(3) . . ? C23 N2 N2 112.8(5) . 3_565 ? C16 O1 Zn1 121.2(2) . 3_666 ? C16 O2 Zn1 134.6(3) . . ? C17 O3 Zn1 134.9(3) . 4_665 ? C17 O4 Zn1 121.4(3) . 2_745 ? N3 C24 H24A 109.5 . . ? N3 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N3 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N3 C25 H25A 109.5 . . ? N3 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N3 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? O5 C26 N3 126.4(16) . . ? O5 C26 H26A 116.8 . . ? N3 C26 H26A 116.8 . . ? C26 N3 C25 116.3(13) . . ? C26 N3 C24 127.2(12) . . ? C25 N3 C24 115.6(13) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.05 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.302 _refine_diff_density_min -0.928 _refine_diff_density_rms 0.116 # Attachment '- 4.cif' data_m4 _database_code_depnum_ccdc_archive 'CCDC 803531' #TrackingRef '- 4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C50.75 H43.75 N4.25 O8.25 Zn2' _chemical_formula_sum 'C50.75 H43.75 N4.25 O8.25 Zn2' _chemical_formula_weight 975.89 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/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' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 15.3836(7) _cell_length_b 21.5307(10) _cell_length_c 15.7987(7) _cell_angle_alpha 90.00 _cell_angle_beta 96.4010(10) _cell_angle_gamma 90.00 _cell_volume 5200.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 185(2) _cell_measurement_reflns_used 5304 _cell_measurement_theta_min 1.89 _cell_measurement_theta_max 26.11 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.246 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2016 _exptl_absorpt_coefficient_mu 0.976 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8288 _exptl_absorpt_correction_T_max 0.8675 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 185(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 9.00cm _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 14572 _diffrn_reflns_av_R_equivalents 0.0292 _diffrn_reflns_av_sigmaI/netI 0.0352 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 26.11 _reflns_number_total 5304 _reflns_number_gt 4229 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXP-97 _computing_publication_material 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^)+(0.0975P)^2^+21.7045P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5304 _refine_ls_number_parameters 319 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0643 _refine_ls_R_factor_gt 0.0511 _refine_ls_wR_factor_ref 0.1861 _refine_ls_wR_factor_gt 0.1763 _refine_ls_goodness_of_fit_ref 1.138 _refine_ls_restrained_S_all 1.151 _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 Zn1 Zn 0.94966(4) 0.0000 0.57430(4) 0.01658(19) Uani 1 2 d S . . Zn2 Zn 0.07497(4) 0.0000 0.95126(4) 0.01692(19) Uani 1 2 d S . . C1 C 1.1416(4) 0.1610(2) 0.6990(3) 0.0461(14) Uani 1 1 d . . . H1A H 1.1001 0.1443 0.7331 0.055 Uiso 1 1 calc R . . C2 C 1.1476(3) 0.1376(2) 0.6180(3) 0.0343(10) Uani 1 1 d . . . C3 C 1.2083(4) 0.1619(3) 0.5692(3) 0.0485(14) Uani 1 1 d . . . H3A H 1.2122 0.1457 0.5138 0.058 Uiso 1 1 calc R . . C4 C 1.2634(4) 0.2093(3) 0.5996(3) 0.0556(17) Uani 1 1 d . . . H4A H 1.3048 0.2260 0.5654 0.067 Uiso 1 1 calc R . . C5 C 1.3764(3) 0.3171(2) 0.7071(3) 0.0433(13) Uani 1 1 d . . . H5A H 1.3974 0.3127 0.6530 0.052 Uiso 1 1 calc R . . C6 C 1.4138(3) 0.3594(2) 0.7654(3) 0.0360(11) Uani 1 1 d . . . H6A H 1.4618 0.3839 0.7519 0.043 Uiso 1 1 calc R . . C7 C 1.3821(3) 0.36661(19) 0.8438(3) 0.0273(9) Uani 1 1 d . . . C8 C 1.3115(3) 0.3314(2) 0.8641(3) 0.0367(11) Uani 1 1 d . . . H8A H 1.2884 0.3372 0.9169 0.044 Uiso 1 1 calc R . . C9 C 1.2028(4) 0.2416(3) 0.8153(3) 0.067(2) Uani 1 1 d D . . C10 C 1.1964(4) 0.2090(2) 0.7299(3) 0.0434(13) Uani 1 1 d . . . C11 C 1.2577(3) 0.2324(2) 0.6807(3) 0.0369(11) Uani 1 1 d . . . C12 C 1.3077(3) 0.2810(2) 0.7284(3) 0.0339(10) Uani 1 1 d . A . C13 C 1.2753(3) 0.2879(2) 0.8065(3) 0.0363(11) Uani 1 1 d . A . C18 C 1.0894(3) 0.0855(2) 0.5830(3) 0.0296(9) Uani 1 1 d . . . C19 C 1.4230(3) 0.41502(18) 0.9042(3) 0.0270(9) Uani 1 1 d . . . C20 C 0.8497(4) 0.0000 0.7259(4) 0.0272(13) Uani 1 2 d S . . H20A H 0.9060 0.0000 0.7574 0.033 Uiso 1 2 calc SR . . C21 C 0.7770(4) 0.0000 0.7696(4) 0.0330(14) Uani 1 2 d S . . H21A H 0.7833 0.0000 0.8302 0.040 Uiso 1 2 calc SR . . C22 C 0.6956(4) 0.0000 0.7248(4) 0.0361(15) Uani 1 2 d S . . C23 C 0.6890(5) 0.0000 0.6355(5) 0.058(2) Uani 1 2 d S . . H23A H 0.6335 0.0000 0.6023 0.069 Uiso 1 2 calc SR . . C24 C 0.7646(4) 0.0000 0.5977(4) 0.049(2) Uani 1 2 d S . . H24A H 0.7605 0.0000 0.5373 0.059 Uiso 1 2 calc SR . . C25 C 0.6164(5) 0.0000 0.7707(5) 0.0472(19) Uani 1 2 d S . . H25A H 0.6223 0.0000 0.8312 0.057 Uiso 1 2 calc SR . . C26 C 0.4000(5) 0.0000 0.7442(5) 0.0477(19) Uani 1 2 d S . . H26A H 0.3932 0.0000 0.6837 0.057 Uiso 1 2 calc SR . . C27 C 0.3223(4) 0.0000 0.7909(4) 0.0374(15) Uani 1 2 d S . . C28 C 0.3318(4) 0.0000 0.8795(5) 0.0402(16) Uani 1 2 d S . . H28A H 0.3882 0.0000 0.9108 0.048 Uiso 1 2 calc SR . . C29 C 0.2575(4) 0.0000 0.9213(4) 0.0353(15) Uani 1 2 d S . . H29A H 0.2640 0.0000 0.9818 0.042 Uiso 1 2 calc SR . . C30 C 0.1690(4) 0.0000 0.7959(4) 0.0377(16) Uani 1 2 d S . . H30A H 0.1118 0.0000 0.7662 0.045 Uiso 1 2 calc SR . . C31 C 0.2399(5) 0.0000 0.7488(5) 0.0456(18) Uani 1 2 d S . . H31A H 0.2312 0.0000 0.6883 0.055 Uiso 1 2 calc SR . . N1 N 0.8443(3) 0.0000 0.6414(3) 0.0229(10) Uani 1 2 d S . . N2 N 0.5408(4) 0.0000 0.7288(4) 0.058(2) Uani 1 2 d S . . N3 N 0.4751(4) 0.0000 0.7842(4) 0.0576(19) Uani 1 2 d S . . N4 N 0.1772(3) 0.0000 0.8800(3) 0.0240(10) Uani 1 2 d S . . O1 O 1.0329(2) 0.06569(14) 0.62809(19) 0.0337(7) Uani 1 1 d . . . O2 O 1.1011(2) 0.06562(16) 0.5107(2) 0.0404(8) Uani 1 1 d . . . O3 O 1.4968(2) 0.43515(15) 0.8898(2) 0.0386(8) Uani 1 1 d . . . O4 O 1.3806(2) 0.43332(14) 0.9629(2) 0.0347(7) Uani 1 1 d . . . C14 C 1.0837(8) 0.3230(5) 0.7479(7) 0.0703(18) Uani 0.60 1 d PD A 1 H14A H 1.0284 0.3430 0.7575 0.105 Uiso 0.60 1 calc PR A 1 H14B H 1.0759 0.2997 0.6944 0.105 Uiso 0.60 1 calc PR A 1 H14C H 1.1289 0.3548 0.7448 0.105 Uiso 0.60 1 calc PR A 1 C15 C 1.1120(8) 0.2783(6) 0.8222(8) 0.0703(18) Uani 0.60 1 d PD A 1 H15A H 1.0649 0.2473 0.8256 0.084 Uiso 0.60 1 calc PR A 1 H15B H 1.1177 0.3023 0.8759 0.084 Uiso 0.60 1 calc PR A 1 C16 C 1.2882(9) 0.1700(6) 0.8956(8) 0.0703(18) Uani 0.60 1 d PD A 1 H16A H 1.2938 0.1432 0.9460 0.105 Uiso 0.60 1 calc PR A 1 H16B H 1.3364 0.2001 0.9001 0.105 Uiso 0.60 1 calc PR A 1 H16C H 1.2903 0.1446 0.8444 0.105 Uiso 0.60 1 calc PR A 1 C17 C 1.2033(8) 0.2039(6) 0.8900(7) 0.0703(18) Uani 0.60 1 d PD A 1 H17A H 1.1536 0.1744 0.8843 0.084 Uiso 0.60 1 calc PR A 1 H17B H 1.1998 0.2299 0.9411 0.084 Uiso 0.60 1 calc PR A 1 C14' C 1.0878(14) 0.2996(8) 0.7947(12) 0.0703(18) Uani 0.40 1 d PD A 2 H14D H 1.0328 0.3144 0.8135 0.105 Uiso 0.40 1 calc PR A 2 H14E H 1.0758 0.2795 0.7390 0.105 Uiso 0.40 1 calc PR A 2 H14F H 1.1273 0.3349 0.7902 0.105 Uiso 0.40 1 calc PR A 2 C15' C 1.1303(11) 0.2532(8) 0.8591(11) 0.0703(18) Uani 0.40 1 d PD A 2 H15C H 1.1466 0.2718 0.9159 0.084 Uiso 0.40 1 calc PR A 2 H15D H 1.0939 0.2157 0.8642 0.084 Uiso 0.40 1 calc PR A 2 C16' C 1.3385(11) 0.1643(8) 0.8760(11) 0.0703(18) Uani 0.40 1 d PD A 2 H16D H 1.3561 0.1349 0.9222 0.105 Uiso 0.40 1 calc PR A 2 H16E H 1.3808 0.1984 0.8779 0.105 Uiso 0.40 1 calc PR A 2 H16F H 1.3368 0.1429 0.8211 0.105 Uiso 0.40 1 calc PR A 2 C17' C 1.2452(11) 0.1910(8) 0.8869(11) 0.0703(18) Uani 0.40 1 d PD A 2 H17C H 1.2480 0.2109 0.9436 0.084 Uiso 0.40 1 calc PR A 2 H17D H 1.2042 0.1555 0.8871 0.084 Uiso 0.40 1 calc PR A 2 C32 C 0.5538(15) -0.1042(10) 0.4553(14) 0.048(3) Uiso 0.25 1 d P . . C33 C 0.5000 -0.2068(15) 0.5000 0.048(3) Uiso 0.25 2 d SP . . N5 N 0.5000 -0.1341(12) 0.5000 0.048(3) Uiso 0.25 2 d SP . . O5 O 0.5960(19) -0.0580(14) 0.4535(19) 0.048(3) Uiso 0.13 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 Zn1 0.0147(3) 0.0191(3) 0.0158(3) 0.000 0.0013(2) 0.000 Zn2 0.0141(3) 0.0189(3) 0.0176(3) 0.000 0.0011(2) 0.000 C1 0.054(3) 0.050(3) 0.039(3) -0.019(2) 0.022(2) -0.032(3) C2 0.039(3) 0.036(2) 0.029(2) -0.0138(19) 0.0067(19) -0.017(2) C3 0.058(3) 0.059(3) 0.031(3) -0.021(2) 0.017(2) -0.030(3) C4 0.066(4) 0.066(4) 0.039(3) -0.024(3) 0.026(3) -0.045(3) C5 0.050(3) 0.048(3) 0.035(3) -0.016(2) 0.016(2) -0.024(2) C6 0.031(2) 0.038(2) 0.040(3) -0.010(2) 0.010(2) -0.014(2) C7 0.031(2) 0.024(2) 0.026(2) -0.0035(17) -0.0003(17) -0.0063(17) C8 0.049(3) 0.036(2) 0.027(2) -0.0098(19) 0.009(2) -0.019(2) C9 0.093(5) 0.074(4) 0.043(3) -0.038(3) 0.040(3) -0.065(4) C10 0.055(3) 0.049(3) 0.029(2) -0.017(2) 0.016(2) -0.029(2) C11 0.044(3) 0.039(2) 0.028(2) -0.0111(19) 0.007(2) -0.020(2) C12 0.039(3) 0.036(2) 0.027(2) -0.0091(19) 0.0083(19) -0.016(2) C13 0.046(3) 0.038(2) 0.027(2) -0.0088(19) 0.008(2) -0.023(2) C18 0.027(2) 0.028(2) 0.033(2) -0.0105(18) 0.0017(18) -0.0064(17) C19 0.031(2) 0.0213(19) 0.026(2) 0.0009(16) -0.0070(17) -0.0046(17) C20 0.023(3) 0.040(3) 0.018(3) 0.000 0.003(2) 0.000 C21 0.027(3) 0.051(4) 0.022(3) 0.000 0.005(2) 0.000 C22 0.026(3) 0.053(4) 0.031(3) 0.000 0.012(3) 0.000 C23 0.020(3) 0.118(8) 0.035(4) 0.000 0.002(3) 0.000 C24 0.022(3) 0.102(7) 0.022(3) 0.000 0.003(3) 0.000 C25 0.032(4) 0.071(5) 0.042(4) 0.000 0.018(3) 0.000 C26 0.030(4) 0.077(5) 0.038(4) 0.000 0.015(3) 0.000 C27 0.026(3) 0.050(4) 0.038(4) 0.000 0.013(3) 0.000 C28 0.019(3) 0.062(5) 0.039(4) 0.000 0.003(3) 0.000 C29 0.024(3) 0.053(4) 0.029(3) 0.000 0.004(3) 0.000 C30 0.021(3) 0.068(5) 0.024(3) 0.000 0.005(3) 0.000 C31 0.035(4) 0.076(5) 0.027(4) 0.000 0.009(3) 0.000 N1 0.016(2) 0.031(2) 0.021(2) 0.000 0.0006(18) 0.000 N2 0.024(3) 0.106(6) 0.048(4) 0.000 0.016(3) 0.000 N3 0.028(3) 0.098(6) 0.051(4) 0.000 0.020(3) 0.000 N4 0.019(2) 0.029(2) 0.025(3) 0.000 0.0046(19) 0.000 O1 0.0354(17) 0.0337(16) 0.0319(17) -0.0093(13) 0.0032(14) -0.0158(14) O2 0.0342(18) 0.0488(19) 0.0389(19) -0.0257(16) 0.0070(14) -0.0158(15) O3 0.0342(17) 0.0410(18) 0.0394(18) -0.0110(15) -0.0012(14) -0.0164(15) O4 0.0396(18) 0.0330(16) 0.0307(17) -0.0124(13) 0.0006(14) -0.0116(14) C14 0.092(5) 0.069(4) 0.054(3) -0.016(2) 0.025(3) -0.037(4) C15 0.092(5) 0.069(4) 0.054(3) -0.016(2) 0.025(3) -0.037(4) C16 0.092(5) 0.069(4) 0.054(3) -0.016(2) 0.025(3) -0.037(4) C17 0.092(5) 0.069(4) 0.054(3) -0.016(2) 0.025(3) -0.037(4) C14' 0.092(5) 0.069(4) 0.054(3) -0.016(2) 0.025(3) -0.037(4) C15' 0.092(5) 0.069(4) 0.054(3) -0.016(2) 0.025(3) -0.037(4) C16' 0.092(5) 0.069(4) 0.054(3) -0.016(2) 0.025(3) -0.037(4) C17' 0.092(5) 0.069(4) 0.054(3) -0.016(2) 0.025(3) -0.037(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 Zn1 O1 2.029(3) . ? Zn1 O1 2.029(3) 6 ? Zn1 N1 2.033(5) . ? Zn1 O2 2.044(3) 5_756 ? Zn1 O2 2.044(3) 2_756 ? Zn1 Zn1 2.9533(11) 5_756 ? Zn2 O3 2.019(3) 3_345 ? Zn2 O3 2.019(3) 8_355 ? Zn2 N4 2.034(5) . ? Zn2 O4 2.040(3) 7_657 ? Zn2 O4 2.040(3) 4_647 ? Zn2 Zn2 2.9127(11) 5_557 ? C1 C10 1.388(6) . ? C1 C2 1.388(6) . ? C1 H1A 0.9500 . ? C2 C3 1.379(6) . ? C2 C18 1.501(6) . ? C3 C4 1.380(7) . ? C3 H3A 0.9500 . ? C4 C11 1.384(6) . ? C4 H4A 0.9500 . ? C5 C6 1.375(6) . ? C5 C12 1.384(6) . ? C5 H5A 0.9500 . ? C6 C7 1.391(6) . ? C6 H6A 0.9500 . ? C7 C8 1.392(6) . ? C7 C19 1.503(6) . ? C8 C13 1.378(6) . ? C8 H8A 0.9500 . ? C9 C15' 1.398(14) . ? C9 C17 1.432(12) . ? C9 C13 1.514(6) . ? C9 C10 1.515(6) . ? C9 C15 1.619(13) . ? C9 C17' 1.652(15) . ? C10 C11 1.382(6) . ? C11 C12 1.459(6) . ? C12 C13 1.389(6) . ? C18 O2 1.252(5) . ? C18 O1 1.258(5) . ? C19 O4 1.255(5) . ? C19 O3 1.259(5) . ? C20 N1 1.328(7) . ? C20 C21 1.379(8) . ? C20 H20A 0.9500 . ? C21 C22 1.368(9) . ? C21 H21A 0.9500 . ? C22 C23 1.403(10) . ? C22 C25 1.486(9) . ? C23 C24 1.366(9) . ? C23 H23A 0.9500 . ? C24 N1 1.338(8) . ? C24 H24A 0.9500 . ? C25 N2 1.273(10) . ? C25 H25A 0.9500 . ? C26 N3 1.253(10) . ? C26 C27 1.472(9) . ? C26 H26A 0.9500 . ? C27 C31 1.365(10) . ? C27 C28 1.392(10) . ? C28 C29 1.381(9) . ? C28 H28A 0.9500 . ? C29 N4 1.331(8) . ? C29 H29A 0.9500 . ? C30 N4 1.322(8) . ? C30 C31 1.386(9) . ? C30 H30A 0.9500 . ? C31 H31A 0.9500 . ? N2 N3 1.408(9) . ? O2 Zn1 2.044(3) 5_756 ? O3 Zn2 2.019(3) 3_655 ? O4 Zn2 2.040(3) 7_657 ? C14 C15 1.542(13) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.490(13) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C14' C15' 1.522(16) . ? C14' H14D 0.9800 . ? C14' H14E 0.9800 . ? C14' H14F 0.9800 . ? C15' H15C 0.9900 . ? C15' H15D 0.9900 . ? C16' C17' 1.574(16) . ? C16' H16D 0.9800 . ? C16' H16E 0.9800 . ? C16' H16F 0.9800 . ? C17' H17C 0.9900 . ? C17' H17D 0.9900 . ? C32 O5 1.19(3) . ? C32 N5 1.31(2) . ? C33 N5 1.57(4) . ? N5 C32 1.31(2) 2_656 ? 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 Zn1 O1 88.37(19) . 6 ? O1 Zn1 N1 106.49(13) . . ? O1 Zn1 N1 106.49(13) 6 . ? O1 Zn1 O2 159.09(13) . 5_756 ? O1 Zn1 O2 88.31(14) 6 5_756 ? N1 Zn1 O2 94.24(13) . 5_756 ? O1 Zn1 O2 88.31(14) . 2_756 ? O1 Zn1 O2 159.09(13) 6 2_756 ? N1 Zn1 O2 94.24(13) . 2_756 ? O2 Zn1 O2 87.5(2) 5_756 2_756 ? O1 Zn1 Zn1 88.32(9) . 5_756 ? O1 Zn1 Zn1 88.32(9) 6 5_756 ? N1 Zn1 Zn1 159.02(14) . 5_756 ? O2 Zn1 Zn1 70.95(9) 5_756 5_756 ? O2 Zn1 Zn1 70.95(9) 2_756 5_756 ? O3 Zn2 O3 87.5(2) 3_345 8_355 ? O3 Zn2 N4 100.96(14) 3_345 . ? O3 Zn2 N4 100.96(14) 8_355 . ? O3 Zn2 O4 160.67(14) 3_345 7_657 ? O3 Zn2 O4 88.30(14) 8_355 7_657 ? N4 Zn2 O4 98.37(13) . 7_657 ? O3 Zn2 O4 88.30(14) 3_345 4_647 ? O3 Zn2 O4 160.67(14) 8_355 4_647 ? N4 Zn2 O4 98.37(13) . 4_647 ? O4 Zn2 O4 89.47(19) 7_657 4_647 ? O3 Zn2 Zn2 77.87(10) 3_345 5_557 ? O3 Zn2 Zn2 77.87(10) 8_355 5_557 ? N4 Zn2 Zn2 178.34(15) . 5_557 ? O4 Zn2 Zn2 82.80(9) 7_657 5_557 ? O4 Zn2 Zn2 82.80(9) 4_647 5_557 ? C10 C1 C2 119.7(4) . . ? C10 C1 H1A 120.2 . . ? C2 C1 H1A 120.2 . . ? C3 C2 C1 119.7(4) . . ? C3 C2 C18 119.4(4) . . ? C1 C2 C18 120.9(4) . . ? C2 C3 C4 121.0(4) . . ? C2 C3 H3A 119.5 . . ? C4 C3 H3A 119.5 . . ? C3 C4 C11 119.2(4) . . ? C3 C4 H4A 120.4 . . ? C11 C4 H4A 120.4 . . ? C6 C5 C12 118.9(4) . . ? C6 C5 H5A 120.6 . . ? C12 C5 H5A 120.6 . . ? C5 C6 C7 120.6(4) . . ? C5 C6 H6A 119.7 . . ? C7 C6 H6A 119.7 . . ? C6 C7 C8 120.3(4) . . ? C6 C7 C19 118.6(4) . . ? C8 C7 C19 121.0(4) . . ? C13 C8 C7 119.1(4) . . ? C13 C8 H8A 120.4 . . ? C7 C8 H8A 120.4 . . ? C15' C9 C17 67.9(9) . . ? C15' C9 C13 124.4(8) . . ? C17 C9 C13 120.8(7) . . ? C15' C9 C10 123.2(8) . . ? C17 C9 C10 117.7(6) . . ? C13 C9 C10 101.4(4) . . ? C15' C9 C15 30.5(7) . . ? C17 C9 C15 98.5(7) . . ? C13 C9 C15 109.6(6) . . ? C10 C9 C15 108.4(6) . . ? C15' C9 C17' 93.1(10) . . ? C17 C9 C17' 25.3(6) . . ? C13 C9 C17' 105.0(8) . . ? C10 C9 C17' 106.6(8) . . ? C15 C9 C17' 123.6(8) . . ? C11 C10 C1 119.9(4) . . ? C11 C10 C9 110.6(4) . . ? C1 C10 C9 129.4(4) . . ? C10 C11 C4 120.5(4) . . ? C10 C11 C12 108.9(4) . . ? C4 C11 C12 130.6(4) . . ? C5 C12 C13 121.0(4) . . ? C5 C12 C11 130.5(4) . . ? C13 C12 C11 108.4(4) . . ? C8 C13 C12 120.1(4) . . ? C8 C13 C9 129.3(4) . . ? C12 C13 C9 110.6(4) . . ? O2 C18 O1 125.5(4) . . ? O2 C18 C2 116.7(4) . . ? O1 C18 C2 117.8(4) . . ? O4 C19 O3 125.3(4) . . ? O4 C19 C7 118.1(4) . . ? O3 C19 C7 116.5(4) . . ? N1 C20 C21 122.8(6) . . ? N1 C20 H20A 118.6 . . ? C21 C20 H20A 118.6 . . ? C22 C21 C20 119.1(6) . . ? C22 C21 H21A 120.4 . . ? C20 C21 H21A 120.4 . . ? C21 C22 C23 118.7(6) . . ? C21 C22 C25 119.9(6) . . ? C23 C22 C25 121.3(6) . . ? C24 C23 C22 118.0(7) . . ? C24 C23 H23A 121.0 . . ? C22 C23 H23A 121.0 . . ? N1 C24 C23 123.5(6) . . ? N1 C24 H24A 118.3 . . ? C23 C24 H24A 118.3 . . ? N2 C25 C22 119.8(7) . . ? N2 C25 H25A 120.1 . . ? C22 C25 H25A 120.1 . . ? N3 C26 C27 120.1(7) . . ? N3 C26 H26A 119.9 . . ? C27 C26 H26A 119.9 . . ? C31 C27 C28 118.5(6) . . ? C31 C27 C26 121.2(7) . . ? C28 C27 C26 120.3(6) . . ? C29 C28 C27 118.8(6) . . ? C29 C28 H28A 120.6 . . ? C27 C28 H28A 120.6 . . ? N4 C29 C28 122.6(6) . . ? N4 C29 H29A 118.7 . . ? C28 C29 H29A 118.7 . . ? N4 C30 C31 123.1(6) . . ? N4 C30 H30A 118.4 . . ? C31 C30 H30A 118.4 . . ? C27 C31 C30 118.9(6) . . ? C27 C31 H31A 120.6 . . ? C30 C31 H31A 120.6 . . ? C20 N1 C24 118.0(5) . . ? C20 N1 Zn1 124.1(4) . . ? C24 N1 Zn1 118.0(4) . . ? C25 N2 N3 110.8(7) . . ? C26 N3 N2 111.9(7) . . ? C30 N4 C29 118.2(5) . . ? C30 N4 Zn2 124.3(4) . . ? C29 N4 Zn2 117.5(4) . . ? C18 O1 Zn1 116.3(3) . . ? C18 O2 Zn1 138.8(3) . 5_756 ? C19 O3 Zn2 130.7(3) . 3_655 ? C19 O4 Zn2 123.3(3) . 7_657 ? C15 C14 H14A 109.5 . . ? C15 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C15 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C14 C15 C9 115.2(9) . . ? C14 C15 H15A 108.5 . . ? C9 C15 H15A 108.5 . . ? C14 C15 H15B 108.5 . . ? C9 C15 H15B 108.5 . . ? H15A C15 H15B 107.5 . . ? C17 C16 H16A 109.5 . . ? C17 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C17 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C9 C17 C16 104.5(9) . . ? C9 C17 H17A 110.8 . . ? C16 C17 H17A 110.8 . . ? C9 C17 H17B 110.8 . . ? C16 C17 H17B 110.8 . . ? H17A C17 H17B 108.9 . . ? C15' C14' H14D 109.5 . . ? C15' C14' H14E 109.5 . . ? H14D C14' H14E 109.5 . . ? C15' C14' H14F 109.5 . . ? H14D C14' H14F 109.5 . . ? H14E C14' H14F 109.5 . . ? C9 C15' C14' 95.4(13) . . ? C9 C15' H15C 112.7 . . ? C14' C15' H15C 112.7 . . ? C9 C15' H15D 112.7 . . ? C14' C15' H15D 112.7 . . ? H15C C15' H15D 110.2 . . ? C17' C16' H16D 109.5 . . ? C17' C16' H16E 109.5 . . ? H16D C16' H16E 109.5 . . ? C17' C16' H16F 109.5 . . ? H16D C16' H16F 109.5 . . ? H16E C16' H16F 109.5 . . ? C16' C17' C9 117.4(12) . . ? C16' C17' H17C 107.9 . . ? C9 C17' H17C 107.9 . . ? C16' C17' H17D 107.9 . . ? C9 C17' H17D 107.9 . . ? H17C C17' H17D 107.2 . . ? O5 C32 N5 143(3) . . ? C32 N5 C32 121(3) . 2_656 ? C32 N5 C33 119.3(14) . . ? C32 N5 C33 119.3(14) 2_656 . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.11 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.286 _refine_diff_density_min -0.607 _refine_diff_density_rms 0.130 # Attachment '- 5.cif' data_m5 _database_code_depnum_ccdc_archive 'CCDC 806385' #TrackingRef '- 5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C61 H53 Cd2 N9 O10' _chemical_formula_sum 'C61 H53 Cd2 N9 O10' _chemical_formula_weight 1296.92 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 Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.9388(11) _cell_length_b 28.520(2) _cell_length_c 16.1837(11) _cell_angle_alpha 90.00 _cell_angle_beta 105.7140(10) _cell_angle_gamma 90.00 _cell_volume 7081.7(8) _cell_formula_units_Z 4 _cell_measurement_temperature 185(2) _cell_measurement_reflns_used 12469 _cell_measurement_theta_min 1.43 _cell_measurement_theta_max 25.05 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.216 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2632 _exptl_absorpt_coefficient_mu 0.655 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8693 _exptl_absorpt_correction_T_max 0.9374 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 185(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 9.00cm _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 35610 _diffrn_reflns_av_R_equivalents 0.0962 _diffrn_reflns_av_sigmaI/netI 0.1213 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 25.05 _reflns_number_total 12469 _reflns_number_gt 6286 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXP-97 _computing_publication_material 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^)+(0.1289P)^2^+55.0817P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12469 _refine_ls_number_parameters 741 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1599 _refine_ls_R_factor_gt 0.0812 _refine_ls_wR_factor_ref 0.3021 _refine_ls_wR_factor_gt 0.2564 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.019 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.38001(6) 0.03381(3) 0.86392(5) 0.0301(3) Uani 1 1 d . . . Cd2 Cd 0.33799(5) -0.03398(3) 0.64984(5) 0.0280(3) Uani 1 1 d . . . C1 C 0.3177(8) 0.1329(4) 0.5423(7) 0.031(3) Uani 1 1 d . . . H1A H 0.3104 0.1130 0.4938 0.038 Uiso 1 1 calc R . . C2 C 0.3222(8) 0.1139(4) 0.6239(7) 0.029(3) Uani 1 1 d . . . C3 C 0.3315(8) 0.1431(4) 0.6925(8) 0.037(3) Uani 1 1 d . . . H3A H 0.3328 0.1298 0.7467 0.044 Uiso 1 1 calc R . . C4 C 0.3391(9) 0.1909(4) 0.6869(7) 0.038(3) Uani 1 1 d . . . H4A H 0.3450 0.2104 0.7357 0.046 Uiso 1 1 calc R . . C5 C 0.3613(9) 0.2992(4) 0.6314(8) 0.040(3) Uani 1 1 d . . . H5A H 0.3650 0.2987 0.6910 0.048 Uiso 1 1 calc R . . C6 C 0.3702(9) 0.3407(4) 0.5905(7) 0.040(3) Uani 1 1 d . . . H6A H 0.3823 0.3687 0.6234 0.048 Uiso 1 1 calc R . . C7 C 0.3621(8) 0.3430(4) 0.5018(7) 0.034(3) Uani 1 1 d . . . C8 C 0.3468(9) 0.3009(4) 0.4533(8) 0.038(3) Uani 1 1 d . . . H8A H 0.3421 0.3015 0.3935 0.045 Uiso 1 1 calc R . . C9 C 0.3385(9) 0.2589(4) 0.4940(7) 0.034(3) Uani 1 1 d . . . C10 C 0.3466(9) 0.2582(4) 0.5829(7) 0.034(3) Uani 1 1 d . . . C11 C 0.3379(8) 0.2095(4) 0.6081(7) 0.034(3) Uani 1 1 d . . . C12 C 0.3240(8) 0.1809(3) 0.5342(7) 0.029(3) Uani 1 1 d . . . C13 C 0.3237(8) 0.2099(4) 0.4555(7) 0.033(3) Uani 1 1 d . . . C14 C 0.3963(11) 0.1951(4) 0.4172(9) 0.058(4) Uani 1 1 d . . . H14A H 0.4523 0.1972 0.4610 0.087 Uiso 1 1 calc R . . H14B H 0.3970 0.2157 0.3691 0.087 Uiso 1 1 calc R . . H14C H 0.3865 0.1626 0.3967 0.087 Uiso 1 1 calc R . . C15 C 0.2375(10) 0.2059(5) 0.3869(8) 0.057(4) Uani 1 1 d . . . H15A H 0.1898 0.2151 0.4112 0.086 Uiso 1 1 calc R . . H15B H 0.2287 0.1735 0.3665 0.086 Uiso 1 1 calc R . . H15C H 0.2381 0.2267 0.3388 0.086 Uiso 1 1 calc R . . C16 C 0.3193(8) 0.0613(4) 0.6344(8) 0.030(3) Uani 1 1 d . . . C17 C 0.3722(8) 0.3882(3) 0.4592(8) 0.031(3) Uani 1 1 d . . . C18 C 0.3903(8) -0.1332(4) 0.9674(7) 0.031(3) Uani 1 1 d . . . H18A H 0.3881 -0.1131 1.0136 0.037 Uiso 1 1 calc R . . C19 C 0.3988(8) -0.1148(4) 0.8890(8) 0.034(3) Uani 1 1 d . . . C20 C 0.4055(8) -0.1449(4) 0.8227(7) 0.033(3) Uani 1 1 d . . . H20A H 0.4114 -0.1319 0.7705 0.040 Uiso 1 1 calc R . . C21 C 0.4038(9) -0.1930(4) 0.8316(7) 0.036(3) Uani 1 1 d . . . H21A H 0.4096 -0.2133 0.7869 0.043 Uiso 1 1 calc R . . C22 C 0.3813(10) -0.3013(4) 0.8899(8) 0.047(4) Uani 1 1 d . . . H22A H 0.3900 -0.3015 0.8341 0.056 Uiso 1 1 calc R . . C23 C 0.3677(9) -0.3425(4) 0.9288(8) 0.041(3) Uani 1 1 d . . . H23A H 0.3664 -0.3714 0.8994 0.049 Uiso 1 1 calc R . . C24 C 0.3560(9) -0.3420(4) 1.0106(7) 0.038(3) Uani 1 1 d . . . C25 C 0.3565(8) -0.3003(4) 1.0548(7) 0.031(3) Uani 1 1 d . . . H25A H 0.3481 -0.3001 1.1107 0.037 Uiso 1 1 calc R . . C26 C 0.3695(9) -0.2586(4) 1.0152(8) 0.036(3) Uani 1 1 d . . . C27 C 0.3820(9) -0.2595(4) 0.9341(8) 0.040(3) Uani 1 1 d . . . C28 C 0.3932(9) -0.2108(4) 0.9091(7) 0.039(3) Uani 1 1 d . . . C29 C 0.3855(8) -0.1813(4) 0.9745(7) 0.032(3) Uani 1 1 d . . . C30 C 0.3717(9) -0.2096(4) 1.0487(8) 0.039(3) Uani 1 1 d . . . C31 C 0.4501(9) -0.2040(4) 1.1292(7) 0.045(4) Uani 1 1 d . . . H31A H 0.5040 -0.2127 1.1149 0.068 Uiso 1 1 calc R . . H31B H 0.4419 -0.2244 1.1751 0.068 Uiso 1 1 calc R . . H31C H 0.4539 -0.1713 1.1485 0.068 Uiso 1 1 calc R . . C32 C 0.2894(9) -0.1957(4) 1.0726(9) 0.050(4) Uani 1 1 d . . . H32A H 0.2391 -0.1989 1.0223 0.075 Uiso 1 1 calc R . . H32B H 0.2942 -0.1630 1.0922 0.075 Uiso 1 1 calc R . . H32C H 0.2817 -0.2161 1.1187 0.075 Uiso 1 1 calc R . . C33 C 0.3991(7) -0.0624(4) 0.8754(8) 0.028(3) Uani 1 1 d . . . C34 C 0.3410(8) -0.3881(4) 1.0530(8) 0.034(3) Uani 1 1 d . . . C35 C 0.1277(9) -0.0196(5) 0.6102(10) 0.051(4) Uani 1 1 d . . . H35A H 0.1378 0.0038 0.5724 0.061 Uiso 1 1 calc R . . C36 C 0.0463(10) -0.0257(6) 0.6154(11) 0.065(5) Uani 1 1 d . . . H36A H 0.0005 -0.0067 0.5822 0.078 Uiso 1 1 calc R . . C37 C 0.0294(10) -0.0585(5) 0.6675(11) 0.058(4) Uani 1 1 d . . . C38 C 0.0955(10) -0.0832(5) 0.7170(11) 0.070(5) Uani 1 1 d . . . H38A H 0.0858 -0.1049 0.7580 0.083 Uiso 1 1 calc R . . C39 C 0.1795(10) -0.0762(5) 0.7071(12) 0.071(5) Uani 1 1 d . . . H39A H 0.2259 -0.0952 0.7394 0.086 Uiso 1 1 calc R . . C40 C -0.0603(11) -0.0664(6) 0.6786(11) 0.065(4) Uani 1 1 d . . . H40A H -0.0694 -0.0898 0.7169 0.077 Uiso 1 1 calc R . . C41 C -0.2596(9) -0.0240(5) 0.6247(8) 0.043(3) Uani 1 1 d . . . H41A H -0.2457 0.0010 0.5917 0.052 Uiso 1 1 calc R . . C42 C -0.3458(9) -0.0268(4) 0.6359(8) 0.039(3) Uani 1 1 d . . . C43 C -0.3734(9) -0.0625(5) 0.6827(9) 0.049(4) Uani 1 1 d . . . H43A H -0.3343 -0.0868 0.7085 0.059 Uiso 1 1 calc R . . C44 C -0.4580(8) -0.0621(4) 0.6912(9) 0.045(3) Uani 1 1 d . . . H44A H -0.4757 -0.0863 0.7231 0.054 Uiso 1 1 calc R . . C45 C -0.4882(9) 0.0054(4) 0.6121(8) 0.044(3) Uani 1 1 d . . . H45A H -0.5279 0.0297 0.5875 0.052 Uiso 1 1 calc R . . C46 C -0.4058(9) 0.0067(5) 0.6016(9) 0.050(4) Uani 1 1 d . . . H46A H -0.3903 0.0315 0.5695 0.060 Uiso 1 1 calc R . . C47 C 0.5784(9) 0.0103(4) 0.8771(7) 0.037(3) Uani 1 1 d . . . H47A H 0.5638 -0.0155 0.9078 0.045 Uiso 1 1 calc R . . C48 C 0.6633(8) 0.0133(4) 0.8686(8) 0.038(3) Uani 1 1 d . . . H48A H 0.7055 -0.0099 0.8931 0.045 Uiso 1 1 calc R . . C49 C 0.6841(8) 0.0502(4) 0.8244(8) 0.036(3) Uani 1 1 d . . . C50 C 0.6206(9) 0.0826(4) 0.7896(8) 0.046(4) Uani 1 1 d . . . H50A H 0.6334 0.1085 0.7582 0.056 Uiso 1 1 calc R . . C51 C 0.5383(8) 0.0775(4) 0.8005(8) 0.035(3) Uani 1 1 d . . . H51A H 0.4948 0.1001 0.7763 0.042 Uiso 1 1 calc R . . C52 C 0.7711(9) 0.0557(5) 0.8131(9) 0.050(4) Uani 1 1 d . . . H52A H 0.7827 0.0806 0.7787 0.060 Uiso 1 1 calc R . . C53 C 0.9745(9) 0.0089(6) 0.8741(11) 0.060(4) Uani 1 1 d . . . H53A H 0.9629 -0.0144 0.9113 0.072 Uiso 1 1 calc R . . C54 C 1.0611(10) 0.0142(5) 0.8637(9) 0.052(4) Uani 1 1 d . . . C55 C 1.1252(10) -0.0130(5) 0.9149(10) 0.061(4) Uani 1 1 d . . . H55A H 1.1122 -0.0351 0.9536 0.074 Uiso 1 1 calc R . . C56 C 1.2116(8) -0.0070(5) 0.9086(9) 0.046(3) Uani 1 1 d . . . H56A H 1.2565 -0.0248 0.9462 0.055 Uiso 1 1 calc R . . C57 C 1.1707(10) 0.0456(5) 0.8025(10) 0.056(4) Uani 1 1 d . . . H57A H 1.1847 0.0652 0.7607 0.068 Uiso 1 1 calc R . . C58 C 1.0828(10) 0.0442(6) 0.8057(10) 0.062(4) Uani 1 1 d . . . H58A H 1.0398 0.0635 0.7689 0.074 Uiso 1 1 calc R . . N1 N 0.1963(7) -0.0446(3) 0.6552(7) 0.037(3) Uani 1 1 d . . . N2 N -0.1228(9) -0.0420(5) 0.6373(9) 0.067(4) Uani 1 1 d . . . N3 N -0.2030(8) -0.0534(5) 0.6571(8) 0.056(3) Uani 1 1 d . . . N4 N -0.5148(6) -0.0288(3) 0.6561(6) 0.033(2) Uani 1 1 d . . . N5 N 0.5182(7) 0.0414(3) 0.8445(6) 0.033(2) Uani 1 1 d . . . N6 N 0.8320(8) 0.0272(5) 0.8493(9) 0.066(4) Uani 1 1 d . . . N7 N 0.9113(9) 0.0369(5) 0.8314(9) 0.069(4) Uani 1 1 d . . . N8 N 1.2338(7) 0.0216(3) 0.8538(7) 0.040(3) Uani 1 1 d . . . O1 O 0.3098(6) 0.0358(2) 0.5706(5) 0.037(2) Uani 1 1 d . . . O2 O 0.3307(5) 0.0451(2) 0.7088(5) 0.0333(19) Uani 1 1 d . . . O3 O 0.3742(7) 0.3870(3) 0.3836(5) 0.049(2) Uani 1 1 d . . . O4 O 0.3748(6) 0.4251(3) 0.5014(5) 0.045(2) Uani 1 1 d . . . O5 O 0.4072(6) -0.0364(2) 0.9387(5) 0.036(2) Uani 1 1 d . . . O6 O 0.3874(5) -0.0469(2) 0.7998(5) 0.035(2) Uani 1 1 d . . . O7 O 0.3271(6) -0.4252(3) 1.0107(5) 0.040(2) Uani 1 1 d . . . O8 O 0.3454(6) -0.3861(3) 1.1319(5) 0.041(2) Uani 1 1 d . . . C59 C 0.101(3) 0.2272(13) 0.588(2) 0.086(11) Uiso 0.50 1 d P . . C60 C 0.108(2) 0.1806(12) 0.715(2) 0.076(10) Uiso 0.50 1 d P . . C61 C 0.100(2) 0.1456(11) 0.5876(19) 0.058(8) Uiso 0.50 1 d P . . N9 N 0.1045(15) 0.1808(8) 0.6300(14) 0.052(6) Uiso 0.50 1 d P . . O9 O 0.0995(13) 0.1037(7) 0.6175(12) 0.064(6) Uiso 0.50 1 d P . . C62 C 0.178(2) -0.2267(12) 0.705(2) 0.074(10) Uiso 0.50 1 d P . . C63 C 0.157(2) -0.1952(11) 0.8317(19) 0.059(8) Uiso 0.50 1 d P . . C64 C 0.030(3) -0.2050(13) 0.718(2) 0.082(11) Uiso 0.50 1 d P . . N10 N 0.1147(16) -0.2090(8) 0.7451(15) 0.056(6) Uiso 0.50 1 d P . . O10 O 0.001(2) -0.2149(12) 0.641(2) 0.134(11) Uiso 0.50 1 d P . . O1W O 0.1247(17) -0.3596(9) 0.9085(16) 0.033(6) Uiso 0.30 1 d P . . O2W O -0.0053(19) -0.1163(10) 0.8912(18) 0.048(8) Uiso 0.30 1 d P . . O3W O 0.118(2) -0.4078(11) 0.895(2) 0.022(8) Uiso 0.20 1 d P . . O4W O -0.085(3) -0.1306(14) 0.967(3) 0.042(11) Uiso 0.20 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 0.0416(6) 0.0139(4) 0.0413(5) -0.0011(4) 0.0222(4) 0.0002(4) Cd2 0.0353(5) 0.0143(4) 0.0394(5) -0.0014(4) 0.0187(4) 0.0001(4) C1 0.038(7) 0.031(6) 0.028(6) -0.005(5) 0.014(6) -0.001(6) C2 0.035(7) 0.023(6) 0.032(6) 0.001(5) 0.014(5) -0.005(5) C3 0.051(9) 0.025(6) 0.035(7) -0.001(5) 0.012(6) 0.001(6) C4 0.065(9) 0.023(6) 0.031(7) 0.008(5) 0.021(6) 0.001(6) C5 0.069(10) 0.029(6) 0.027(6) 0.005(5) 0.019(6) -0.001(6) C6 0.070(10) 0.019(6) 0.029(6) 0.000(5) 0.012(6) -0.002(6) C7 0.052(8) 0.018(6) 0.039(7) 0.001(5) 0.024(6) 0.000(6) C8 0.058(9) 0.022(6) 0.037(7) 0.006(5) 0.021(7) -0.006(6) C9 0.059(9) 0.014(5) 0.036(7) 0.002(5) 0.025(6) 0.002(6) C10 0.056(9) 0.021(6) 0.022(6) 0.003(5) 0.007(6) -0.008(6) C11 0.050(8) 0.015(5) 0.037(7) 0.000(5) 0.014(6) -0.009(5) C12 0.040(7) 0.012(5) 0.038(7) -0.006(5) 0.014(6) 0.002(5) C13 0.050(8) 0.015(5) 0.036(7) -0.001(5) 0.013(6) -0.002(5) C14 0.106(13) 0.021(6) 0.059(9) 0.005(6) 0.045(9) 0.000(8) C15 0.080(12) 0.033(7) 0.047(8) 0.007(6) -0.001(8) -0.008(8) C16 0.032(7) 0.016(6) 0.046(8) 0.000(5) 0.016(6) -0.003(5) C17 0.041(8) 0.011(5) 0.044(7) 0.002(5) 0.016(6) -0.003(5) C18 0.043(8) 0.018(6) 0.035(7) 0.004(5) 0.015(6) -0.007(5) C19 0.042(8) 0.018(6) 0.044(7) -0.002(5) 0.018(6) 0.001(5) C20 0.052(8) 0.021(6) 0.032(6) 0.005(5) 0.022(6) 0.001(6) C21 0.066(9) 0.014(5) 0.032(6) -0.003(5) 0.019(6) -0.002(6) C22 0.080(11) 0.022(6) 0.041(7) 0.002(5) 0.020(7) -0.002(7) C23 0.068(10) 0.016(6) 0.044(7) -0.008(5) 0.025(7) -0.010(6) C24 0.059(9) 0.017(6) 0.035(7) 0.003(5) 0.005(6) -0.002(6) C25 0.043(8) 0.019(6) 0.032(6) 0.007(5) 0.013(6) 0.008(5) C26 0.052(9) 0.023(6) 0.038(7) 0.005(5) 0.017(6) 0.000(6) C27 0.073(10) 0.015(6) 0.034(7) 0.007(5) 0.018(7) 0.005(6) C28 0.065(9) 0.020(6) 0.035(7) 0.009(5) 0.020(7) 0.003(6) C29 0.052(8) 0.021(6) 0.025(6) -0.008(5) 0.013(6) -0.006(6) C30 0.064(9) 0.017(6) 0.044(7) -0.007(5) 0.029(7) -0.005(6) C31 0.079(11) 0.024(6) 0.027(6) 0.003(5) 0.004(7) -0.006(7) C32 0.070(10) 0.029(7) 0.060(9) 0.003(6) 0.035(8) -0.007(7) C33 0.031(7) 0.016(5) 0.046(7) 0.004(5) 0.022(6) 0.000(5) C34 0.041(8) 0.022(6) 0.041(7) 0.007(5) 0.016(6) -0.002(6) C35 0.030(8) 0.054(9) 0.074(10) 0.022(7) 0.023(7) 0.004(7) C36 0.035(9) 0.080(12) 0.084(12) 0.029(9) 0.022(8) -0.003(8) C37 0.045(10) 0.056(9) 0.078(11) 0.007(8) 0.026(8) -0.003(8) C38 0.042(10) 0.070(11) 0.106(14) 0.049(10) 0.035(9) 0.002(8) C39 0.047(10) 0.059(10) 0.112(14) 0.033(10) 0.028(10) 0.017(8) C40 0.058(11) 0.063(10) 0.082(12) 0.017(9) 0.034(10) -0.010(9) C41 0.041(9) 0.055(9) 0.035(7) -0.010(6) 0.013(7) -0.010(7) C42 0.039(8) 0.041(7) 0.042(7) -0.006(6) 0.021(6) 0.004(7) C43 0.030(8) 0.043(8) 0.074(10) 0.008(7) 0.013(7) 0.003(6) C44 0.028(8) 0.042(8) 0.068(9) 0.015(7) 0.017(7) -0.002(6) C45 0.051(9) 0.029(7) 0.057(8) 0.008(6) 0.024(7) 0.001(6) C46 0.051(10) 0.050(9) 0.056(9) -0.002(7) 0.026(8) -0.023(8) C47 0.051(9) 0.025(6) 0.035(7) -0.004(5) 0.011(6) 0.003(6) C48 0.031(8) 0.032(7) 0.049(8) 0.006(6) 0.009(6) 0.011(6) C49 0.026(7) 0.040(7) 0.045(7) -0.008(6) 0.015(6) -0.002(6) C50 0.060(10) 0.035(7) 0.048(8) -0.002(6) 0.022(7) -0.011(7) C51 0.031(7) 0.025(6) 0.048(8) 0.002(5) 0.011(6) -0.006(5) C52 0.045(9) 0.046(8) 0.068(10) 0.002(7) 0.028(8) -0.001(7) C53 0.034(9) 0.063(10) 0.087(12) 0.021(9) 0.024(9) 0.007(8) C54 0.049(10) 0.062(9) 0.050(9) -0.005(7) 0.023(8) -0.002(8) C55 0.060(11) 0.064(10) 0.078(11) 0.026(8) 0.049(9) 0.013(8) C56 0.024(7) 0.057(9) 0.059(9) 0.023(7) 0.014(7) 0.006(6) C57 0.055(10) 0.061(10) 0.065(10) 0.010(8) 0.037(8) 0.008(8) C58 0.042(9) 0.089(12) 0.060(10) 0.017(9) 0.022(8) 0.008(9) N1 0.034(6) 0.022(5) 0.059(7) 0.001(5) 0.021(5) -0.008(5) N2 0.042(8) 0.082(10) 0.077(9) 0.017(8) 0.015(7) -0.004(7) N3 0.035(7) 0.081(9) 0.058(8) 0.006(7) 0.022(6) -0.008(7) N4 0.026(6) 0.027(5) 0.047(6) -0.002(5) 0.014(5) 0.002(5) N5 0.038(6) 0.026(5) 0.039(6) 0.001(4) 0.017(5) 0.004(5) N6 0.046(8) 0.076(9) 0.090(10) 0.016(8) 0.038(7) 0.003(7) N7 0.066(10) 0.074(9) 0.073(9) -0.005(7) 0.030(8) -0.026(8) N8 0.038(7) 0.032(6) 0.053(7) 0.001(5) 0.017(6) 0.003(5) O1 0.058(6) 0.016(4) 0.039(5) 0.000(4) 0.016(4) -0.004(4) O2 0.048(5) 0.016(4) 0.036(5) 0.005(3) 0.013(4) -0.001(4) O3 0.093(8) 0.019(4) 0.043(5) 0.002(4) 0.037(5) 0.000(5) O4 0.075(7) 0.016(4) 0.047(5) -0.003(4) 0.021(5) -0.006(4) O5 0.059(6) 0.016(4) 0.042(5) -0.002(4) 0.026(4) 0.003(4) O6 0.052(6) 0.019(4) 0.037(5) 0.007(3) 0.020(4) 0.000(4) O7 0.064(6) 0.016(4) 0.042(5) 0.004(4) 0.017(5) -0.004(4) O8 0.064(6) 0.024(4) 0.037(5) 0.002(4) 0.017(4) -0.004(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 O3 2.285(7) 4_566 ? Cd1 N5 2.317(10) . ? Cd1 N8 2.317(11) 1_455 ? Cd1 O5 2.318(7) . ? Cd1 O2 2.440(8) . ? Cd1 O4 2.536(8) 4_566 ? Cd1 O6 2.541(7) . ? Cd1 C17 2.729(11) 4_566 ? Cd2 N1 2.304(10) . ? Cd2 O8 2.304(7) 4 ? Cd2 N4 2.326(9) 1_655 ? Cd2 O1 2.343(7) . ? Cd2 O6 2.370(8) . ? Cd2 O2 2.462(7) . ? Cd2 O7 2.499(8) 4 ? Cd2 C34 2.728(11) 4 ? Cd2 C16 2.738(10) . ? C1 C12 1.381(14) . ? C1 C2 1.411(15) . ? C2 C3 1.364(15) . ? C2 C16 1.510(14) . ? C3 C4 1.375(15) . ? C4 C11 1.376(15) . ? C5 C6 1.382(15) . ? C5 C10 1.393(15) . ? C6 C7 1.407(15) . ? C7 C8 1.419(15) . ? C7 C17 1.490(14) . ? C8 C9 1.391(14) . ? C9 C10 1.411(15) . ? C9 C13 1.523(14) . ? C10 C11 1.463(14) . ? C11 C12 1.416(15) . ? C12 C13 1.517(15) . ? C13 C14 1.512(18) . ? C13 C15 1.520(18) . ? C16 O1 1.239(13) . ? C16 O2 1.257(13) . ? C17 O3 1.234(13) . ? C17 O4 1.249(13) . ? C17 Cd1 2.729(10) 4_565 ? C18 C29 1.381(14) . ? C18 C19 1.411(15) . ? C19 C20 1.401(15) . ? C19 C33 1.512(14) . ? C20 C21 1.380(14) . ? C21 C28 1.406(15) . ? C22 C23 1.379(15) . ? C22 C27 1.389(16) . ? C23 C24 1.386(16) . ? C24 C25 1.388(15) . ? C24 C34 1.530(15) . ? C25 C26 1.391(15) . ? C26 C27 1.381(16) . ? C26 C30 1.497(15) . ? C27 C28 1.470(15) . ? C28 C29 1.384(15) . ? C29 C30 1.511(16) . ? C30 C32 1.518(18) . ? C30 C31 1.550(18) . ? C33 O5 1.244(13) . ? C33 O6 1.265(13) . ? C34 O7 1.247(13) . ? C34 O8 1.262(13) . ? C34 Cd2 2.728(11) 4_556 ? C35 C36 1.334(18) . ? C35 N1 1.342(16) . ? C36 C37 1.335(19) . ? C37 C38 1.34(2) . ? C37 C40 1.50(2) . ? C38 C39 1.41(2) . ? C39 N1 1.308(17) . ? C40 N2 1.249(19) . ? C41 N3 1.241(17) . ? C41 C42 1.436(18) . ? C42 C46 1.360(18) . ? C42 C43 1.408(18) . ? C43 C44 1.392(18) . ? C44 N4 1.329(15) . ? C45 N4 1.342(14) . ? C45 C46 1.369(18) . ? C47 N5 1.309(14) . ? C47 C48 1.400(17) . ? C48 C49 1.363(17) . ? C49 C50 1.374(17) . ? C49 C52 1.456(17) . ? C50 C51 1.379(17) . ? C51 N5 1.338(14) . ? C52 N6 1.281(17) . ? C53 N7 1.324(18) . ? C53 C54 1.443(19) . ? C54 C55 1.37(2) . ? C54 C58 1.380(19) . ? C55 C56 1.420(18) . ? C56 N8 1.322(15) . ? C57 N8 1.311(17) . ? C57 C58 1.417(19) . ? N2 N3 1.437(16) . ? N4 Cd2 2.326(9) 1_455 ? N6 N7 1.400(17) . ? N8 Cd1 2.317(11) 1_655 ? O3 Cd1 2.285(7) 4_565 ? O4 Cd1 2.536(8) 4_565 ? O7 Cd2 2.499(8) 4_556 ? O8 Cd2 2.304(7) 4_556 ? C59 N9 1.48(4) . ? C60 N9 1.37(4) . ? C61 N9 1.21(3) . ? C61 O9 1.29(3) . ? C62 N10 1.43(4) . ? C63 N10 1.43(4) . ? C64 O10 1.24(4) . ? C64 N10 1.31(4) . ? O1W O3W 1.39(4) . ? 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 O3 Cd1 N5 90.1(3) 4_566 . ? O3 Cd1 N8 94.6(3) 4_566 1_455 ? N5 Cd1 N8 168.1(4) . 1_455 ? O3 Cd1 O5 142.1(3) 4_566 . ? N5 Cd1 O5 95.8(3) . . ? N8 Cd1 O5 87.1(3) 1_455 . ? O3 Cd1 O2 90.0(3) 4_566 . ? N5 Cd1 O2 84.3(3) . . ? N8 Cd1 O2 84.8(3) 1_455 . ? O5 Cd1 O2 127.8(2) . . ? O3 Cd1 O4 53.8(3) 4_566 4_566 ? N5 Cd1 O4 109.5(3) . 4_566 ? N8 Cd1 O4 82.0(3) 1_455 4_566 ? O5 Cd1 O4 89.2(3) . 4_566 ? O2 Cd1 O4 139.8(3) . 4_566 ? O3 Cd1 O6 163.8(3) 4_566 . ? N5 Cd1 O6 83.0(3) . . ? N8 Cd1 O6 89.5(3) 1_455 . ? O5 Cd1 O6 53.7(3) . . ? O2 Cd1 O6 74.7(2) . . ? O4 Cd1 O6 142.5(2) 4_566 . ? O3 Cd1 C17 26.7(3) 4_566 4_566 ? N5 Cd1 C17 101.0(3) . 4_566 ? N8 Cd1 C17 87.9(4) 1_455 4_566 ? O5 Cd1 C17 116.1(3) . 4_566 ? O2 Cd1 C17 115.0(3) . 4_566 ? O4 Cd1 C17 27.1(3) 4_566 4_566 ? O6 Cd1 C17 169.6(3) . 4_566 ? N1 Cd2 O8 87.6(3) . 4 ? N1 Cd2 N4 174.0(3) . 1_655 ? O8 Cd2 N4 89.0(3) 4 1_655 ? N1 Cd2 O1 95.0(3) . . ? O8 Cd2 O1 141.2(3) 4 . ? N4 Cd2 O1 90.7(3) 1_655 . ? N1 Cd2 O6 89.9(3) . . ? O8 Cd2 O6 87.7(3) 4 . ? N4 Cd2 O6 85.1(3) 1_655 . ? O1 Cd2 O6 130.9(3) . . ? N1 Cd2 O2 87.5(3) . . ? O8 Cd2 O2 164.4(3) 4 . ? N4 Cd2 O2 94.5(3) 1_655 . ? O1 Cd2 O2 54.1(3) . . ? O6 Cd2 O2 77.5(2) . . ? N1 Cd2 O7 98.2(3) . 4 ? O8 Cd2 O7 54.5(3) 4 4 ? N4 Cd2 O7 83.8(3) 1_655 4 ? O1 Cd2 O7 86.9(3) . 4 ? O6 Cd2 O7 140.6(3) . 4 ? O2 Cd2 O7 141.0(2) . 4 ? N1 Cd2 C34 94.8(4) . 4 ? O8 Cd2 C34 27.4(3) 4 4 ? N4 Cd2 C34 84.4(3) 1_655 4 ? O1 Cd2 C34 114.1(3) . 4 ? O6 Cd2 C34 114.1(3) . 4 ? O2 Cd2 C34 168.1(3) . 4 ? O7 Cd2 C34 27.1(3) 4 4 ? N1 Cd2 C16 92.9(3) . . ? O8 Cd2 C16 168.0(3) 4 . ? N4 Cd2 C16 91.4(3) 1_655 . ? O1 Cd2 C16 26.8(3) . . ? O6 Cd2 C16 104.2(3) . . ? O2 Cd2 C16 27.3(3) . . ? O7 Cd2 C16 113.7(3) 4 . ? C34 Cd2 C16 140.8(4) 4 . ? C12 C1 C2 118.9(10) . . ? C3 C2 C1 119.6(10) . . ? C3 C2 C16 121.0(10) . . ? C1 C2 C16 119.4(10) . . ? C2 C3 C4 122.9(11) . . ? C3 C4 C11 117.8(11) . . ? C6 C5 C10 118.2(10) . . ? C5 C6 C7 122.5(11) . . ? C6 C7 C8 118.6(10) . . ? C6 C7 C17 121.4(10) . . ? C8 C7 C17 120.0(10) . . ? C9 C8 C7 119.5(11) . . ? C8 C9 C10 120.1(10) . . ? C8 C9 C13 128.5(10) . . ? C10 C9 C13 111.4(9) . . ? C5 C10 C9 121.2(10) . . ? C5 C10 C11 130.8(10) . . ? C9 C10 C11 108.0(9) . . ? C4 C11 C12 121.3(10) . . ? C4 C11 C10 130.2(10) . . ? C12 C11 C10 108.5(10) . . ? C1 C12 C11 119.4(10) . . ? C1 C12 C13 129.5(10) . . ? C11 C12 C13 111.0(9) . . ? C14 C13 C12 111.3(10) . . ? C14 C13 C15 108.7(11) . . ? C12 C13 C15 111.7(10) . . ? C14 C13 C9 111.9(10) . . ? C12 C13 C9 101.1(9) . . ? C15 C13 C9 112.0(10) . . ? O1 C16 O2 122.3(10) . . ? O1 C16 C2 119.4(10) . . ? O2 C16 C2 118.2(10) . . ? O1 C16 Cd2 58.5(5) . . ? O2 C16 Cd2 64.0(5) . . ? C2 C16 Cd2 171.6(8) . . ? O3 C17 O4 124.0(10) . . ? O3 C17 C7 118.1(10) . . ? O4 C17 C7 117.9(10) . . ? O3 C17 Cd1 56.2(5) . 4_565 ? O4 C17 Cd1 67.8(6) . 4_565 ? C7 C17 Cd1 173.4(9) . 4_565 ? C29 C18 C19 117.7(10) . . ? C20 C19 C18 120.5(10) . . ? C20 C19 C33 119.3(10) . . ? C18 C19 C33 120.2(10) . . ? C21 C20 C19 121.3(10) . . ? C20 C21 C28 117.6(10) . . ? C23 C22 C27 118.5(12) . . ? C22 C23 C24 120.5(11) . . ? C23 C24 C25 121.1(10) . . ? C23 C24 C34 119.9(10) . . ? C25 C24 C34 119.0(10) . . ? C24 C25 C26 118.4(11) . . ? C27 C26 C25 120.1(10) . . ? C27 C26 C30 111.4(10) . . ? C25 C26 C30 128.6(11) . . ? C26 C27 C22 121.4(10) . . ? C26 C27 C28 107.7(10) . . ? C22 C27 C28 130.8(11) . . ? C29 C28 C21 121.3(10) . . ? C29 C28 C27 108.8(10) . . ? C21 C28 C27 129.8(11) . . ? C18 C29 C28 121.4(11) . . ? C18 C29 C30 128.4(10) . . ? C28 C29 C30 110.2(9) . . ? C26 C30 C29 101.9(9) . . ? C26 C30 C32 113.5(11) . . ? C29 C30 C32 112.6(11) . . ? C26 C30 C31 109.7(10) . . ? C29 C30 C31 110.8(10) . . ? C32 C30 C31 108.3(11) . . ? O5 C33 O6 122.9(10) . . ? O5 C33 C19 118.3(10) . . ? O6 C33 C19 118.7(10) . . ? O7 C34 O8 123.1(10) . . ? O7 C34 C24 120.5(10) . . ? O8 C34 C24 116.4(10) . . ? O7 C34 Cd2 66.1(6) . 4_556 ? O8 C34 Cd2 57.2(5) . 4_556 ? C24 C34 Cd2 170.4(9) . 4_556 ? C36 C35 N1 124.0(13) . . ? C35 C36 C37 119.8(15) . . ? C36 C37 C38 119.1(14) . . ? C36 C37 C40 122.7(15) . . ? C38 C37 C40 118.0(14) . . ? C37 C38 C39 118.5(14) . . ? N1 C39 C38 122.5(14) . . ? N2 C40 C37 119.9(14) . . ? N3 C41 C42 121.3(13) . . ? C46 C42 C43 116.1(12) . . ? C46 C42 C41 120.0(12) . . ? C43 C42 C41 123.9(13) . . ? C44 C43 C42 119.9(12) . . ? N4 C44 C43 122.0(12) . . ? N4 C45 C46 122.4(13) . . ? C42 C46 C45 121.5(13) . . ? N5 C47 C48 122.8(11) . . ? C49 C48 C47 118.6(11) . . ? C48 C49 C50 118.6(11) . . ? C48 C49 C52 121.6(12) . . ? C50 C49 C52 119.8(12) . . ? C49 C50 C51 119.8(12) . . ? N5 C51 C50 121.6(12) . . ? N6 C52 C49 120.2(13) . . ? N7 C53 C54 119.5(14) . . ? C55 C54 C58 118.7(14) . . ? C55 C54 C53 116.7(14) . . ? C58 C54 C53 124.5(14) . . ? C54 C55 C56 117.9(13) . . ? N8 C56 C55 124.3(12) . . ? N8 C57 C58 124.1(13) . . ? C54 C58 C57 118.2(14) . . ? C39 N1 C35 115.9(12) . . ? C39 N1 Cd2 119.2(10) . . ? C35 N1 Cd2 124.9(8) . . ? C40 N2 N3 112.5(13) . . ? C41 N3 N2 109.9(12) . . ? C44 N4 C45 118.1(11) . . ? C44 N4 Cd2 122.4(8) . 1_455 ? C45 N4 Cd2 118.9(8) . 1_455 ? C47 N5 C51 118.8(11) . . ? C47 N5 Cd1 120.1(8) . . ? C51 N5 Cd1 121.1(8) . . ? C52 N6 N7 113.2(13) . . ? C53 N7 N6 111.9(13) . . ? C57 N8 C56 116.6(12) . . ? C57 N8 Cd1 123.4(9) . 1_655 ? C56 N8 Cd1 119.5(9) . 1_655 ? C16 O1 Cd2 94.6(7) . . ? C16 O2 Cd1 163.1(7) . . ? C16 O2 Cd2 88.6(6) . . ? Cd1 O2 Cd2 104.0(3) . . ? C17 O3 Cd1 97.2(6) . 4_565 ? C17 O4 Cd1 85.1(7) . 4_565 ? C33 O5 Cd1 97.0(7) . . ? C33 O6 Cd2 164.9(7) . . ? C33 O6 Cd1 86.1(6) . . ? Cd2 O6 Cd1 103.7(3) . . ? C34 O7 Cd2 86.7(7) . 4_556 ? C34 O8 Cd2 95.4(6) . 4_556 ? N9 C61 O9 124(3) . . ? C61 N9 C60 123(3) . . ? C61 N9 C59 120(3) . . ? C60 N9 C59 117(3) . . ? O10 C64 N10 113(4) . . ? C64 N10 C62 132(3) . . ? C64 N10 C63 118(3) . . ? C62 N10 C63 110(3) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.788 _refine_diff_density_min -0.769 _refine_diff_density_rms 0.220