# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Wang, Yao-Yu' _publ_contact_author_email wyaoyu@nwu.edu.cn _publ_section_title ; Synthesis, structural diversity and fluorescent characterisation of a series of d10 metal-organic frameworks (MOFs): reaction condition, second ligand and metal effects ; loop_ _publ_author_name W.-H.Zhang Z.Dong Y.-Y.Wang L.Hou J.-C.Jin W.-H.Huang Q.Shi data_1 _database_code_depnum_ccdc_archive 'CCDC 761111' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H58 O19 Zn3' _chemical_formula_sum 'C42 H58 O19 Zn3' _chemical_formula_weight 1062.99 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' 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/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.844(5) _cell_length_b 20.201(5) _cell_length_c 11.540(3) _cell_angle_alpha 90.00 _cell_angle_beta 114.492(5) _cell_angle_gamma 90.00 _cell_volume 4422.1(18) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 2080 _cell_measurement_theta_min 2.798 _cell_measurement_theta_max 22.817 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.597 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2208 _exptl_absorpt_coefficient_mu 1.693 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6219 _exptl_absorpt_correction_T_max 0.6486 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10860 _diffrn_reflns_av_R_equivalents 0.0826 _diffrn_reflns_av_sigmaI/netI 0.0827 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 25.15 _reflns_number_total 3956 _reflns_number_gt 2733 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1040P)^2^+1.6126P] 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 3956 _refine_ls_number_parameters 283 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0841 _refine_ls_R_factor_gt 0.0557 _refine_ls_wR_factor_ref 0.1761 _refine_ls_wR_factor_gt 0.1535 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _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 0.29669(3) 0.19302(3) 0.50975(6) 0.0298(2) Uani 1 1 d . . . Zn2 Zn 0.5000 0.10477(4) 0.7500 0.0389(3) Uani 1 2 d S . . O1 O 0.37224(18) 0.12753(16) 0.5570(3) 0.0384(9) Uani 1 1 d . . . O2 O 0.44393(19) 0.04387(18) 0.6139(4) 0.0503(11) Uani 1 1 d . . . O3 O 0.24067(19) -0.15936(17) 0.1058(3) 0.0375(9) Uani 1 1 d . . . O4 O 0.16787(19) -0.24339(17) 0.0885(4) 0.0430(10) Uani 1 1 d . . . O5 O 0.35615(17) 0.24682(17) 0.6723(3) 0.0374(9) Uani 1 1 d . . . O6 O 0.28451(18) 0.33154(18) 0.6564(3) 0.0380(9) Uani 1 1 d . . . O7 O 0.45547(19) 0.16260(19) 0.8306(4) 0.0457(10) Uani 1 1 d . . . O8 O 0.5000 0.274(2) 0.2500 0.59(2) Uiso 1 2 d S . . O9 O 0.5351(2) 0.2164(3) 0.0621(5) 0.099(2) Uani 1 1 d . . . O10 O 0.545(2) 0.935(2) 0.660(3) 0.72(2) Uiso 1 1 d . . . C1 C 0.3866(3) 0.0689(2) 0.5374(5) 0.0312(12) Uani 1 1 d . . . C2 C 0.3398(3) 0.0312(2) 0.4247(5) 0.0371(13) Uani 1 1 d . . . H2A H 0.3658 0.0208 0.3739 0.044 Uiso 1 1 calc R . . H2B H 0.3007 0.0594 0.3736 0.044 Uiso 1 1 calc R . . C3 C 0.3098(2) -0.0337(2) 0.4517(5) 0.0283(11) Uani 1 1 d . . . C4 C 0.2564(3) -0.0614(2) 0.3253(5) 0.0317(12) Uani 1 1 d . . . H4A H 0.2798 -0.0694 0.2694 0.038 Uiso 1 1 calc R . . H4B H 0.2197 -0.0287 0.2848 0.038 Uiso 1 1 calc R . . C5 C 0.2226(3) -0.1259(2) 0.3426(5) 0.0347(12) Uani 1 1 d . . . C6 C 0.1864(4) -0.1114(3) 0.4306(6) 0.061(2) Uani 1 1 d . . . H6A H 0.1663 -0.1520 0.4461 0.073 Uiso 1 1 calc R . . H6B H 0.1483 -0.0803 0.3896 0.073 Uiso 1 1 calc R . . C7 C 0.2385(4) -0.0825(4) 0.5582(7) 0.065(2) Uani 1 1 d . . . H7A H 0.2139 -0.0735 0.6127 0.078 Uiso 1 1 calc R . . C8 C 0.2714(3) -0.0203(3) 0.5385(6) 0.0432(15) Uani 1 1 d . . . H8A H 0.3048 -0.0035 0.6200 0.052 Uiso 1 1 calc R . . H8B H 0.2353 0.0131 0.4998 0.052 Uiso 1 1 calc R . . C9 C 0.2960(5) -0.1349(3) 0.6213(6) 0.071(2) Uani 1 1 d . . . H9A H 0.3299 -0.1188 0.7030 0.085 Uiso 1 1 calc R . . H9B H 0.2750 -0.1752 0.6356 0.085 Uiso 1 1 calc R . . C10 C 0.3327(4) -0.1491(3) 0.5352(6) 0.0497(16) Uani 1 1 d . . . H10 H 0.3696 -0.1823 0.5754 0.060 Uiso 1 1 calc R . . C11 C 0.3663(3) -0.0855(3) 0.5148(5) 0.0409(14) Uani 1 1 d . . . H11A H 0.4002 -0.0690 0.5961 0.049 Uiso 1 1 calc R . . H11B H 0.3910 -0.0946 0.4615 0.049 Uiso 1 1 calc R . . C12 C 0.2803(3) -0.1751(3) 0.4072(5) 0.0446(15) Uani 1 1 d . . . H12A H 0.3046 -0.1842 0.3533 0.054 Uiso 1 1 calc R . . H12B H 0.2600 -0.2162 0.4198 0.054 Uiso 1 1 calc R . . C13 C 0.1667(3) -0.1515(3) 0.2158(6) 0.0442(15) Uani 1 1 d . . . H13A H 0.1359 -0.1817 0.2338 0.053 Uiso 1 1 calc R . . H13B H 0.1383 -0.1143 0.1692 0.053 Uiso 1 1 calc R . . C14 C 0.1950(3) -0.1864(3) 0.1308(5) 0.0384(13) Uani 1 1 d . . . C15 C 0.3419(3) 0.3014(3) 0.7078(5) 0.0337(13) Uani 1 1 d . . . C16 C 0.3996(3) 0.3367(3) 0.8211(5) 0.0339(12) Uani 1 1 d . . . H16A H 0.3775 0.3655 0.8611 0.041 Uiso 1 1 calc R . . H16B H 0.4268 0.3038 0.8834 0.041 Uiso 1 1 calc R . . C17 C 0.4489(3) 0.3771(2) 0.7834(5) 0.0325(12) Uani 1 1 d . . . C18 C 0.4072(3) 0.4225(3) 0.6697(6) 0.0416(14) Uani 1 1 d . . . H18A H 0.3783 0.3958 0.5968 0.050 Uiso 1 1 calc R . . H18B H 0.3762 0.4510 0.6911 0.050 Uiso 1 1 calc R . . C19 C 0.4574(3) 0.4644(3) 0.6363(6) 0.0510(16) Uani 1 1 d . . . H19 H 0.4299 0.4922 0.5628 0.061 Uiso 1 1 calc R . . C20 C 0.5000 0.5093(4) 0.7500 0.060(3) Uani 1 2 d S . . H20A H 0.4685 0.5373 0.7708 0.072 Uiso 0.50 1 calc PR . . H20B H 0.5315 0.5373 0.7292 0.072 Uiso 0.50 1 calc PR . . C21 C 0.4932(3) 0.4222(3) 0.8964(6) 0.0461(15) Uani 1 1 d . . . H21A H 0.4621 0.4503 0.9181 0.055 Uiso 1 1 calc R . . H21B H 0.5201 0.3951 0.9700 0.055 Uiso 1 1 calc R . . C22 C 0.5000 0.3346(3) 0.7500 0.0322(17) Uani 1 2 d S . . H22A H 0.5268 0.3063 0.8218 0.039 Uiso 0.50 1 calc PR . . H22B H 0.4732 0.3063 0.6782 0.039 Uiso 0.50 1 calc PR . . H7WA H 0.4843 0.1735 0.9013 0.048 Uiso 1 1 d R . . H7WB H 0.4330 0.1950 0.7872 0.048 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0234(3) 0.0248(4) 0.0397(4) 0.0044(3) 0.0117(3) 0.0050(2) Zn2 0.0302(5) 0.0252(5) 0.0499(6) 0.000 0.0053(4) 0.000 O1 0.0318(19) 0.024(2) 0.053(2) -0.0022(18) 0.0112(18) 0.0080(15) O2 0.036(2) 0.022(2) 0.066(3) -0.0074(19) -0.006(2) 0.0082(16) O3 0.040(2) 0.033(2) 0.044(2) -0.0086(17) 0.0224(19) -0.0035(17) O4 0.044(2) 0.029(2) 0.058(3) -0.0176(19) 0.023(2) -0.0047(17) O5 0.034(2) 0.028(2) 0.046(2) -0.0060(17) 0.0119(18) 0.0015(16) O6 0.0269(19) 0.042(2) 0.040(2) 0.0013(18) 0.0090(17) 0.0030(16) O7 0.039(2) 0.045(2) 0.041(2) 0.0038(19) 0.0052(18) 0.0131(18) O9 0.036(3) 0.130(5) 0.119(4) -0.073(4) 0.022(3) -0.018(3) C1 0.029(3) 0.020(3) 0.043(3) 0.002(2) 0.014(2) -0.002(2) C2 0.041(3) 0.026(3) 0.038(3) -0.002(2) 0.010(3) -0.004(2) C3 0.031(3) 0.019(3) 0.035(3) -0.001(2) 0.014(2) 0.000(2) C4 0.030(3) 0.021(3) 0.040(3) -0.003(2) 0.011(2) 0.000(2) C5 0.039(3) 0.022(3) 0.046(3) -0.010(2) 0.021(3) -0.009(2) C6 0.073(5) 0.059(4) 0.075(5) -0.034(4) 0.056(4) -0.034(4) C7 0.088(5) 0.067(5) 0.063(5) -0.034(4) 0.053(4) -0.039(4) C8 0.052(4) 0.034(3) 0.048(4) -0.017(3) 0.025(3) -0.008(3) C9 0.138(7) 0.028(4) 0.052(4) -0.006(3) 0.045(5) -0.028(4) C10 0.080(5) 0.015(3) 0.048(4) 0.003(3) 0.021(3) 0.002(3) C11 0.043(3) 0.032(3) 0.038(3) 0.001(3) 0.007(3) 0.008(2) C12 0.064(4) 0.027(3) 0.047(4) -0.006(3) 0.027(3) -0.008(3) C13 0.040(3) 0.034(3) 0.067(4) -0.017(3) 0.030(3) -0.012(3) C14 0.032(3) 0.043(4) 0.031(3) -0.003(3) 0.004(3) 0.007(3) C15 0.023(3) 0.048(4) 0.031(3) 0.007(3) 0.012(2) -0.005(2) C16 0.031(3) 0.030(3) 0.042(3) -0.007(2) 0.016(2) 0.003(2) C17 0.028(3) 0.025(3) 0.047(3) -0.003(2) 0.017(3) 0.002(2) C18 0.026(3) 0.036(3) 0.057(4) 0.000(3) 0.011(3) 0.006(2) C19 0.042(3) 0.032(3) 0.072(5) 0.020(3) 0.017(3) 0.008(3) C20 0.052(5) 0.031(5) 0.104(8) 0.000 0.040(6) 0.000 C21 0.034(3) 0.052(4) 0.050(4) -0.021(3) 0.015(3) -0.002(3) C22 0.029(4) 0.026(4) 0.042(5) 0.000 0.016(3) 0.000 _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 1.953(3) . ? Zn1 O6 2.024(4) 7_556 ? Zn1 O3 2.031(3) 6_556 ? Zn1 O4 2.044(3) 4 ? Zn1 O5 2.076(3) . ? Zn1 Zn1 2.9624(12) 7_556 ? Zn2 O7 1.951(4) 2_656 ? Zn2 O7 1.951(4) . ? Zn2 O2 1.955(4) . ? Zn2 O2 1.955(4) 2_656 ? O1 C1 1.265(6) . ? O2 C1 1.260(6) . ? O3 C14 1.231(6) . ? O3 Zn1 2.031(3) 6 ? O4 C14 1.285(6) . ? O4 Zn1 2.044(3) 4_545 ? O5 C15 1.255(6) . ? O6 C15 1.251(6) . ? O6 Zn1 2.024(4) 7_556 ? O7 H7WA 0.8181 . ? O7 H7WB 0.8388 . ? C1 C2 1.474(7) . ? C2 C3 1.540(7) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C11 1.517(7) . ? C3 C4 1.527(7) . ? C3 C8 1.542(7) . ? C4 C5 1.534(7) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C12 1.498(7) . ? C5 C6 1.524(7) . ? C5 C13 1.534(7) . ? C6 C7 1.537(9) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.495(8) . ? C7 C9 1.538(10) . ? C7 H7A 0.9800 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.511(9) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C12 1.521(8) . ? C10 C11 1.526(8) . ? C10 H10 0.9800 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.513(7) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C15 C16 1.535(7) . ? C16 C17 1.512(7) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C22 1.537(6) . ? C17 C18 1.540(7) . ? C17 C21 1.544(7) . ? C18 C19 1.515(8) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C21 1.500(8) 2_656 ? C19 C20 1.538(8) . ? C19 H19 0.9800 . ? C20 C19 1.538(8) 2_656 ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C19 1.500(8) 2_656 ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C17 1.537(6) 2_656 ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? 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 O6 111.06(15) . 7_556 ? O1 Zn1 O3 101.55(15) . 6_556 ? O6 Zn1 O3 89.47(15) 7_556 6_556 ? O1 Zn1 O4 98.37(15) . 4 ? O6 Zn1 O4 88.91(15) 7_556 4 ? O3 Zn1 O4 159.20(15) 6_556 4 ? O1 Zn1 O5 89.55(14) . . ? O6 Zn1 O5 159.39(14) 7_556 . ? O3 Zn1 O5 86.84(14) 6_556 . ? O4 Zn1 O5 87.41(15) 4 . ? O1 Zn1 Zn1 167.37(11) . 7_556 ? O6 Zn1 Zn1 81.57(10) 7_556 7_556 ? O3 Zn1 Zn1 78.07(10) 6_556 7_556 ? O4 Zn1 Zn1 81.18(10) 4 7_556 ? O5 Zn1 Zn1 77.82(10) . 7_556 ? O7 Zn2 O7 106.4(2) 2_656 . ? O7 Zn2 O2 103.77(17) 2_656 . ? O7 Zn2 O2 121.02(16) . . ? O7 Zn2 O2 121.02(16) 2_656 2_656 ? O7 Zn2 O2 103.77(17) . 2_656 ? O2 Zn2 O2 102.0(2) . 2_656 ? C1 O1 Zn1 143.9(3) . . ? C1 O2 Zn2 112.8(3) . . ? C14 O3 Zn1 130.8(4) . 6 ? C14 O4 Zn1 124.7(3) . 4_545 ? C15 O5 Zn1 128.5(3) . . ? C15 O6 Zn1 126.2(4) . 7_556 ? Zn2 O7 H7WA 109.8 . . ? Zn2 O7 H7WB 116.1 . . ? H7WA O7 H7WB 112.5 . . ? O2 C1 O1 118.4(5) . . ? O2 C1 C2 119.9(5) . . ? O1 C1 C2 121.5(5) . . ? C1 C2 C3 116.0(4) . . ? C1 C2 H2A 108.3 . . ? C3 C2 H2A 108.3 . . ? C1 C2 H2B 108.3 . . ? C3 C2 H2B 108.3 . . ? H2A C2 H2B 107.4 . . ? C11 C3 C4 108.7(4) . . ? C11 C3 C2 112.6(4) . . ? C4 C3 C2 108.3(4) . . ? C11 C3 C8 108.5(4) . . ? C4 C3 C8 108.5(4) . . ? C2 C3 C8 110.2(4) . . ? C3 C4 C5 112.2(4) . . ? C3 C4 H4A 109.2 . . ? C5 C4 H4A 109.2 . . ? C3 C4 H4B 109.2 . . ? C5 C4 H4B 109.2 . . ? H4A C4 H4B 107.9 . . ? C12 C5 C6 108.2(5) . . ? C12 C5 C4 108.2(4) . . ? C6 C5 C4 107.7(4) . . ? C12 C5 C13 112.8(4) . . ? C6 C5 C13 108.0(4) . . ? C4 C5 C13 111.7(5) . . ? C5 C6 C7 111.3(5) . . ? C5 C6 H6A 109.4 . . ? C7 C6 H6A 109.4 . . ? C5 C6 H6B 109.4 . . ? C7 C6 H6B 109.4 . . ? H6A C6 H6B 108.0 . . ? C8 C7 C6 111.2(6) . . ? C8 C7 C9 109.5(6) . . ? C6 C7 C9 107.2(6) . . ? C8 C7 H7A 109.7 . . ? C6 C7 H7A 109.7 . . ? C9 C7 H7A 109.7 . . ? C7 C8 C3 110.1(4) . . ? C7 C8 H8A 109.6 . . ? C3 C8 H8A 109.6 . . ? C7 C8 H8B 109.6 . . ? C3 C8 H8B 109.6 . . ? H8A C8 H8B 108.1 . . ? C10 C9 C7 109.0(5) . . ? C10 C9 H9A 109.9 . . ? C7 C9 H9A 109.9 . . ? C10 C9 H9B 109.9 . . ? C7 C9 H9B 109.9 . . ? H9A C9 H9B 108.3 . . ? C9 C10 C12 110.4(6) . . ? C9 C10 C11 109.4(5) . . ? C12 C10 C11 109.4(5) . . ? C9 C10 H10 109.2 . . ? C12 C10 H10 109.2 . . ? C11 C10 H10 109.2 . . ? C3 C11 C10 109.8(5) . . ? C3 C11 H11A 109.7 . . ? C10 C11 H11A 109.7 . . ? C3 C11 H11B 109.7 . . ? C10 C11 H11B 109.7 . . ? H11A C11 H11B 108.2 . . ? C5 C12 C10 111.0(4) . . ? C5 C12 H12A 109.4 . . ? C10 C12 H12A 109.4 . . ? C5 C12 H12B 109.4 . . ? C10 C12 H12B 109.4 . . ? H12A C12 H12B 108.0 . . ? C14 C13 C5 115.4(4) . . ? C14 C13 H13A 108.4 . . ? C5 C13 H13A 108.4 . . ? C14 C13 H13B 108.4 . . ? C5 C13 H13B 108.4 . . ? H13A C13 H13B 107.5 . . ? O3 C14 O4 124.8(5) . . ? O3 C14 C13 119.4(5) . . ? O4 C14 C13 115.8(5) . . ? O6 C15 O5 125.6(5) . . ? O6 C15 C16 115.9(5) . . ? O5 C15 C16 118.5(4) . . ? C17 C16 C15 113.1(4) . . ? C17 C16 H16A 109.0 . . ? C15 C16 H16A 109.0 . . ? C17 C16 H16B 109.0 . . ? C15 C16 H16B 109.0 . . ? H16A C16 H16B 107.8 . . ? C16 C17 C22 113.2(4) . . ? C16 C17 C18 110.8(4) . . ? C22 C17 C18 109.0(4) . . ? C16 C17 C21 108.4(4) . . ? C22 C17 C21 107.9(4) . . ? C18 C17 C21 107.3(4) . . ? C19 C18 C17 110.1(4) . . ? C19 C18 H18A 109.6 . . ? C17 C18 H18A 109.6 . . ? C19 C18 H18B 109.6 . . ? C17 C18 H18B 109.6 . . ? H18A C18 H18B 108.2 . . ? C21 C19 C18 111.4(5) 2_656 . ? C21 C19 C20 109.6(5) 2_656 . ? C18 C19 C20 109.1(5) . . ? C21 C19 H19 108.9 2_656 . ? C18 C19 H19 108.9 . . ? C20 C19 H19 108.9 . . ? C19 C20 C19 107.8(7) . 2_656 ? C19 C20 H20A 110.1 . . ? C19 C20 H20A 110.1 2_656 . ? C19 C20 H20B 110.1 . . ? C19 C20 H20B 110.1 2_656 . ? H20A C20 H20B 108.5 . . ? C19 C21 C17 110.8(5) 2_656 . ? C19 C21 H21A 109.5 2_656 . ? C17 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 2_656 . ? C17 C21 H21B 109.5 . . ? H21A C21 H21B 108.1 . . ? C17 C22 C17 111.9(6) 2_656 . ? C17 C22 H22A 109.2 2_656 . ? C17 C22 H22A 109.2 . . ? C17 C22 H22B 109.2 2_656 . ? C17 C22 H22B 109.2 . . ? H22A C22 H22B 107.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O6 Zn1 O1 C1 -18.5(6) 7_556 . . . ? O3 Zn1 O1 C1 75.5(6) 6_556 . . . ? O4 Zn1 O1 C1 -110.5(6) 4 . . . ? O5 Zn1 O1 C1 162.2(6) . . . . ? Zn1 Zn1 O1 C1 162.5(4) 7_556 . . . ? O7 Zn2 O2 C1 -79.3(4) 2_656 . . . ? O7 Zn2 O2 C1 39.9(4) . . . . ? O2 Zn2 O2 C1 154.2(4) 2_656 . . . ? O1 Zn1 O5 C15 177.0(4) . . . . ? O6 Zn1 O5 C15 -1.3(7) 7_556 . . . ? O3 Zn1 O5 C15 -81.4(4) 6_556 . . . ? O4 Zn1 O5 C15 78.6(4) 4 . . . ? Zn1 Zn1 O5 C15 -2.9(4) 7_556 . . . ? Zn2 O2 C1 O1 -0.6(6) . . . . ? Zn2 O2 C1 C2 176.3(4) . . . . ? Zn1 O1 C1 O2 -166.0(4) . . . . ? Zn1 O1 C1 C2 17.1(9) . . . . ? O2 C1 C2 C3 62.9(7) . . . . ? O1 C1 C2 C3 -120.2(5) . . . . ? C1 C2 C3 C11 -66.3(6) . . . . ? C1 C2 C3 C4 173.5(4) . . . . ? C1 C2 C3 C8 55.0(6) . . . . ? C11 C3 C4 C5 58.2(5) . . . . ? C2 C3 C4 C5 -179.3(4) . . . . ? C8 C3 C4 C5 -59.7(5) . . . . ? C3 C4 C5 C12 -57.9(5) . . . . ? C3 C4 C5 C6 58.9(6) . . . . ? C3 C4 C5 C13 177.4(4) . . . . ? C12 C5 C6 C7 60.2(7) . . . . ? C4 C5 C6 C7 -56.6(7) . . . . ? C13 C5 C6 C7 -177.4(5) . . . . ? C5 C6 C7 C8 58.3(8) . . . . ? C5 C6 C7 C9 -61.3(7) . . . . ? C6 C7 C8 C3 -58.1(7) . . . . ? C9 C7 C8 C3 60.1(6) . . . . ? C11 C3 C8 C7 -59.8(6) . . . . ? C4 C3 C8 C7 58.1(6) . . . . ? C2 C3 C8 C7 176.6(5) . . . . ? C8 C7 C9 C10 -60.5(7) . . . . ? C6 C7 C9 C10 60.2(6) . . . . ? C7 C9 C10 C12 -60.2(6) . . . . ? C7 C9 C10 C11 60.2(7) . . . . ? C4 C3 C11 C10 -58.3(6) . . . . ? C2 C3 C11 C10 -178.3(4) . . . . ? C8 C3 C11 C10 59.4(6) . . . . ? C9 C10 C11 C3 -60.9(7) . . . . ? C12 C10 C11 C3 60.1(6) . . . . ? C6 C5 C12 C10 -57.9(6) . . . . ? C4 C5 C12 C10 58.5(6) . . . . ? C13 C5 C12 C10 -177.4(4) . . . . ? C9 C10 C12 C5 59.5(6) . . . . ? C11 C10 C12 C5 -60.8(6) . . . . ? C12 C5 C13 C14 -43.8(7) . . . . ? C6 C5 C13 C14 -163.3(5) . . . . ? C4 C5 C13 C14 78.3(6) . . . . ? Zn1 O3 C14 O4 -6.7(8) 6 . . . ? Zn1 O3 C14 C13 174.1(4) 6 . . . ? Zn1 O4 C14 O3 8.6(8) 4_545 . . . ? Zn1 O4 C14 C13 -172.2(3) 4_545 . . . ? C5 C13 C14 O3 -51.3(7) . . . . ? C5 C13 C14 O4 129.5(5) . . . . ? Zn1 O6 C15 O5 -8.1(7) 7_556 . . . ? Zn1 O6 C15 C16 169.7(3) 7_556 . . . ? Zn1 O5 C15 O6 7.4(7) . . . . ? Zn1 O5 C15 C16 -170.4(3) . . . . ? O6 C15 C16 C17 -94.1(5) . . . . ? O5 C15 C16 C17 83.8(6) . . . . ? C15 C16 C17 C22 -73.0(5) . . . . ? C15 C16 C17 C18 49.8(6) . . . . ? C15 C16 C17 C21 167.3(4) . . . . ? C16 C17 C18 C19 178.0(5) . . . . ? C22 C17 C18 C19 -56.8(6) . . . . ? C21 C17 C18 C19 59.8(6) . . . . ? C17 C18 C19 C21 58.8(7) . . . 2_656 ? C17 C18 C19 C20 -62.4(6) . . . . ? C21 C19 C20 C19 -60.9(4) 2_656 . . 2_656 ? C18 C19 C20 C19 61.4(3) . . . 2_656 ? C16 C17 C21 C19 -179.2(4) . . . 2_656 ? C22 C17 C21 C19 57.9(6) . . . 2_656 ? C18 C17 C21 C19 -59.4(6) . . . 2_656 ? C16 C17 C22 C17 -178.0(5) . . . 2_656 ? C18 C17 C22 C17 58.2(3) . . . 2_656 ? C21 C17 C22 C17 -58.0(3) . . . 2_656 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.15 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.944 _refine_diff_density_min -0.775 _refine_diff_density_rms 0.130 data_2 _database_code_depnum_ccdc_archive 'CCDC 761112' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H22 N O4 Zn' _chemical_formula_sum 'C19 H22 N O4 Zn' _chemical_formula_weight 393.75 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' 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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.602(5) _cell_length_b 14.062(3) _cell_length_c 11.233(2) _cell_angle_alpha 90.00 _cell_angle_beta 113.450(3) _cell_angle_gamma 90.00 _cell_volume 3275.3(12) _cell_formula_units_Z 8 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 1237 _cell_measurement_theta_min 2.328 _cell_measurement_theta_max 22.766 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.597 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1640 _exptl_absorpt_coefficient_mu 1.525 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7502 _exptl_absorpt_correction_T_max 0.7816 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8099 _diffrn_reflns_av_R_equivalents 0.0488 _diffrn_reflns_av_sigmaI/netI 0.0606 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 25.10 _reflns_number_total 2904 _reflns_number_gt 2026 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0446P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2904 _refine_ls_number_parameters 229 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0556 _refine_ls_R_factor_gt 0.0366 _refine_ls_wR_factor_ref 0.0919 _refine_ls_wR_factor_gt 0.0868 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _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 0.0000 0.30424(3) -0.2500 0.02250(16) Uani 1 2 d S . . Zn2 Zn 0.0000 0.09764(3) -0.2500 0.02081(17) Uani 1 2 d S . . N1 N 0.0000 0.4515(2) -0.2500 0.0234(9) Uani 1 2 d S . . N2 N 0.0000 0.9529(2) -0.2500 0.0194(8) Uani 1 2 d S . . O1 O 0.07115(11) 0.29063(14) -0.0716(2) 0.0287(5) Uani 1 1 d . . . O2 O 0.08225(11) 0.13443(15) -0.0898(2) 0.0324(6) Uani 1 1 d . . . O3 O 0.43215(11) 0.22890(15) 0.3306(2) 0.0301(6) Uani 1 1 d . . . O4 O 0.44809(11) 0.38511(15) 0.3567(2) 0.0299(6) Uani 1 1 d . . . C1 C 0.10277(16) 0.2134(2) -0.0370(3) 0.0247(8) Uani 1 1 d . . . C2 C 0.16876(16) 0.2121(2) 0.0697(3) 0.0285(8) Uani 1 1 d . . . H2A H 0.1983 0.1939 0.0303 0.034 Uiso 1 1 calc R . . H2B H 0.1691 0.1607 0.1275 0.034 Uiso 1 1 calc R . . C3 C 0.19896(16) 0.2990(2) 0.1563(3) 0.0220(7) Uani 1 1 d . . . C4 C 0.16309(16) 0.3240(2) 0.2430(3) 0.0272(8) Uani 1 1 d . . . H4A H 0.1192 0.3427 0.1894 0.033 Uiso 1 1 calc R . . H4B H 0.1614 0.2686 0.2931 0.033 Uiso 1 1 calc R . . C5 C 0.19758(16) 0.4053(2) 0.3346(3) 0.0335(9) Uani 1 1 d . . . H5 H 0.1744 0.4203 0.3898 0.040 Uiso 1 1 calc R . . C6 C 0.19883(17) 0.4927(2) 0.2566(3) 0.0368(9) Uani 1 1 d . . . H6A H 0.2197 0.5450 0.3146 0.044 Uiso 1 1 calc R . . H6B H 0.1551 0.5118 0.2020 0.044 Uiso 1 1 calc R . . C7 C 0.23597(16) 0.4689(2) 0.1725(3) 0.0307(8) Uani 1 1 d . . . H7 H 0.2370 0.5253 0.1220 0.037 Uiso 1 1 calc R . . C8 C 0.20151(17) 0.3882(2) 0.0790(3) 0.0289(8) Uani 1 1 d . . . H8A H 0.2243 0.3737 0.0241 0.035 Uiso 1 1 calc R . . H8B H 0.1581 0.4078 0.0237 0.035 Uiso 1 1 calc R . . C9 C 0.26830(15) 0.2712(2) 0.2444(3) 0.0236(8) Uani 1 1 d . . . H9A H 0.2673 0.2154 0.2945 0.028 Uiso 1 1 calc R . . H9B H 0.2915 0.2544 0.1909 0.028 Uiso 1 1 calc R . . C10 C 0.26679(16) 0.3766(2) 0.4204(3) 0.0310(9) Uani 1 1 d . . . H10A H 0.2662 0.3223 0.4732 0.037 Uiso 1 1 calc R . . H10B H 0.2881 0.4287 0.4781 0.037 Uiso 1 1 calc R . . C11 C 0.30462(15) 0.3509(2) 0.3376(3) 0.0217(7) Uani 1 1 d . . . C12 C 0.37257(16) 0.3183(2) 0.4283(3) 0.0259(8) Uani 1 1 d . . . H12A H 0.3895 0.3631 0.4996 0.031 Uiso 1 1 calc R . . H12B H 0.3689 0.2571 0.4647 0.031 Uiso 1 1 calc R . . C13 C 0.42092(15) 0.3090(2) 0.3665(3) 0.0231(7) Uani 1 1 d . . . C14 C 0.02224(16) 0.5007(2) -0.1391(3) 0.0282(8) Uani 1 1 d . . . H14 H 0.0386 0.4674 -0.0612 0.034 Uiso 1 1 calc R . . C15 C 0.02216(16) 0.5980(2) -0.1347(3) 0.0266(8) Uani 1 1 d . . . H15 H 0.0368 0.6293 -0.0553 0.032 Uiso 1 1 calc R . . C16 C 0.0000 0.6497(3) -0.2500 0.0207(10) Uani 1 2 d S . . C17 C 0.0000 0.7547(3) -0.2500 0.0186(10) Uani 1 2 d S . . C18 C 0.01998(15) 0.8057(2) -0.3328(3) 0.0216(7) Uani 1 1 d . . . H18 H 0.0331 0.7741 -0.3909 0.026 Uiso 1 1 calc R . . C19 C 0.02030(15) 0.9031(2) -0.3285(3) 0.0233(7) Uani 1 1 d . . . H19 H 0.0353 0.9363 -0.3825 0.028 Uiso 1 1 calc R . . C26 C 0.30524(16) 0.4394(2) 0.2572(3) 0.0273(8) Uani 1 1 d . . . H26A H 0.3273 0.4912 0.3148 0.033 Uiso 1 1 calc R . . H26B H 0.3283 0.4253 0.2027 0.033 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0240(3) 0.0133(3) 0.0249(3) 0.000 0.0041(2) 0.000 Zn2 0.0221(3) 0.0137(3) 0.0262(3) 0.000 0.0092(3) 0.000 N1 0.023(2) 0.025(2) 0.022(2) 0.000 0.0080(19) 0.000 N2 0.021(2) 0.0151(19) 0.021(2) 0.000 0.0067(18) 0.000 O1 0.0236(14) 0.0286(13) 0.0245(13) -0.0003(10) -0.0004(11) 0.0042(10) O2 0.0245(14) 0.0302(14) 0.0320(14) -0.0062(10) 0.0000(12) -0.0024(10) O3 0.0303(15) 0.0253(12) 0.0366(15) -0.0020(10) 0.0155(12) 0.0009(10) O4 0.0306(14) 0.0271(13) 0.0368(15) -0.0014(10) 0.0186(12) -0.0059(11) C1 0.027(2) 0.0268(19) 0.0209(18) 0.0000(14) 0.0105(16) 0.0019(15) C2 0.024(2) 0.0278(19) 0.0249(19) -0.0069(14) -0.0001(16) 0.0008(15) C3 0.0231(19) 0.0183(15) 0.0232(18) -0.0007(14) 0.0078(15) 0.0016(14) C4 0.018(2) 0.0329(19) 0.027(2) -0.0016(14) 0.0050(16) -0.0063(14) C5 0.029(2) 0.043(2) 0.035(2) -0.0130(17) 0.0200(19) -0.0020(17) C6 0.028(2) 0.0268(19) 0.050(3) -0.0103(17) 0.0097(19) 0.0018(16) C7 0.029(2) 0.0195(17) 0.040(2) 0.0069(15) 0.0101(18) -0.0029(14) C8 0.027(2) 0.035(2) 0.025(2) 0.0040(15) 0.0106(17) 0.0046(16) C9 0.027(2) 0.0218(17) 0.0223(19) 0.0023(13) 0.0103(16) 0.0019(14) C10 0.031(2) 0.037(2) 0.025(2) -0.0092(15) 0.0114(17) -0.0057(16) C11 0.0206(19) 0.0246(17) 0.0206(18) -0.0013(14) 0.0090(15) -0.0048(14) C12 0.026(2) 0.0260(18) 0.0241(19) -0.0012(14) 0.0088(16) -0.0047(14) C13 0.0185(19) 0.0296(19) 0.0170(17) 0.0011(14) 0.0028(15) 0.0015(15) C14 0.039(2) 0.0223(17) 0.022(2) 0.0065(14) 0.0110(17) 0.0060(16) C15 0.038(2) 0.0177(16) 0.0218(18) -0.0013(13) 0.0090(17) 0.0005(15) C16 0.021(3) 0.012(2) 0.030(3) 0.000 0.010(2) 0.000 C17 0.017(3) 0.012(2) 0.021(3) 0.000 0.001(2) 0.000 C18 0.026(2) 0.0192(16) 0.0233(18) -0.0015(13) 0.0135(15) 0.0030(14) C19 0.026(2) 0.0191(16) 0.0263(19) 0.0022(14) 0.0118(16) 0.0014(14) C26 0.025(2) 0.0246(17) 0.032(2) 0.0019(15) 0.0115(17) -0.0024(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O1 2.018(2) . ? Zn1 O1 2.018(2) 2_554 ? Zn1 N1 2.070(4) . ? Zn1 O3 2.120(2) 8_455 ? Zn1 O3 2.120(2) 7 ? Zn1 Zn2 2.9053(9) . ? Zn2 O4 1.998(2) 7 ? Zn2 O4 1.998(2) 8_455 ? Zn2 N2 2.035(3) 1_545 ? Zn2 O2 2.074(2) . ? Zn2 O2 2.074(2) 2_554 ? N1 C14 1.336(4) . ? N1 C14 1.336(4) 2_554 ? N2 C19 1.342(3) . ? N2 C19 1.342(3) 2_554 ? N2 Zn2 2.035(3) 1_565 ? O1 C1 1.273(4) . ? O2 C1 1.257(3) . ? O3 C13 1.256(3) . ? O3 Zn1 2.120(2) 7 ? O4 C13 1.260(3) . ? O4 Zn2 1.998(2) 7 ? C1 C2 1.496(4) . ? C2 C3 1.541(4) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C9 1.534(4) . ? C3 C4 1.535(4) . ? C3 C8 1.540(4) . ? C4 C5 1.529(4) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.517(5) . ? C5 C10 1.529(5) . ? C5 H5 0.9800 . ? C6 C7 1.530(4) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C26 1.531(4) . ? C7 C8 1.533(4) . ? C7 H7 0.9800 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C11 1.531(4) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.536(4) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.537(4) . ? C11 C26 1.541(4) . ? C12 C13 1.515(4) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C14 C15 1.368(4) . ? C14 H14 0.9300 . ? C15 C16 1.393(4) . ? C15 H15 0.9300 . ? C16 C15 1.393(4) 2_554 ? C16 C17 1.476(6) . ? C17 C18 1.385(4) 2_554 ? C17 C18 1.385(4) . ? C18 C19 1.370(4) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? 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 169.11(12) . 2_554 ? O1 Zn1 N1 95.44(6) . . ? O1 Zn1 N1 95.44(6) 2_554 . ? O1 Zn1 O3 88.93(9) . 8_455 ? O1 Zn1 O3 88.68(9) 2_554 8_455 ? N1 Zn1 O3 102.70(6) . 8_455 ? O1 Zn1 O3 88.68(9) . 7 ? O1 Zn1 O3 88.93(9) 2_554 7 ? N1 Zn1 O3 102.70(6) . 7 ? O3 Zn1 O3 154.60(12) 8_455 7 ? O1 Zn1 Zn2 84.56(6) . . ? O1 Zn1 Zn2 84.56(6) 2_554 . ? N1 Zn1 Zn2 180.0 . . ? O3 Zn1 Zn2 77.30(6) 8_455 . ? O3 Zn1 Zn2 77.30(6) 7 . ? O4 Zn2 O4 166.05(12) 7 8_455 ? O4 Zn2 N2 96.97(6) 7 1_545 ? O4 Zn2 N2 96.97(6) 8_455 1_545 ? O4 Zn2 O2 87.30(9) 7 . ? O4 Zn2 O2 89.23(9) 8_455 . ? N2 Zn2 O2 104.45(6) 1_545 . ? O4 Zn2 O2 89.23(9) 7 2_554 ? O4 Zn2 O2 87.30(9) 8_455 2_554 ? N2 Zn2 O2 104.45(6) 1_545 2_554 ? O2 Zn2 O2 151.10(12) . 2_554 ? O4 Zn2 Zn1 83.03(6) 7 . ? O4 Zn2 Zn1 83.03(6) 8_455 . ? N2 Zn2 Zn1 180.0 1_545 . ? O2 Zn2 Zn1 75.55(6) . . ? O2 Zn2 Zn1 75.55(6) 2_554 . ? C14 N1 C14 117.5(4) . 2_554 ? C14 N1 Zn1 121.23(19) . . ? C14 N1 Zn1 121.23(19) 2_554 . ? C19 N2 C19 117.1(4) . 2_554 ? C19 N2 Zn2 121.47(18) . 1_565 ? C19 N2 Zn2 121.47(18) 2_554 1_565 ? C1 O1 Zn1 120.9(2) . . ? C1 O2 Zn2 131.7(2) . . ? C13 O3 Zn1 127.4(2) . 7 ? C13 O4 Zn2 125.3(2) . 7 ? O2 C1 O1 123.5(3) . . ? O2 C1 C2 115.5(3) . . ? O1 C1 C2 120.9(3) . . ? C1 C2 C3 123.1(3) . . ? C1 C2 H2A 106.6 . . ? C3 C2 H2A 106.6 . . ? C1 C2 H2B 106.6 . . ? C3 C2 H2B 106.6 . . ? H2A C2 H2B 106.5 . . ? C9 C3 C4 108.1(3) . . ? C9 C3 C8 108.3(3) . . ? C4 C3 C8 108.6(2) . . ? C9 C3 C2 106.7(2) . . ? C4 C3 C2 111.6(3) . . ? C8 C3 C2 113.3(3) . . ? C5 C4 C3 110.0(2) . . ? C5 C4 H4A 109.7 . . ? C3 C4 H4A 109.7 . . ? C5 C4 H4B 109.7 . . ? C3 C4 H4B 109.7 . . ? H4A C4 H4B 108.2 . . ? C6 C5 C4 109.8(3) . . ? C6 C5 C10 109.2(3) . . ? C4 C5 C10 110.2(3) . . ? C6 C5 H5 109.2 . . ? C4 C5 H5 109.2 . . ? C10 C5 H5 109.2 . . ? C5 C6 C7 108.7(3) . . ? C5 C6 H6A 109.9 . . ? C7 C6 H6A 109.9 . . ? C5 C6 H6B 109.9 . . ? C7 C6 H6B 109.9 . . ? H6A C6 H6B 108.3 . . ? C6 C7 C26 110.6(3) . . ? C6 C7 C8 109.3(3) . . ? C26 C7 C8 109.9(3) . . ? C6 C7 H7 109.0 . . ? C26 C7 H7 109.0 . . ? C8 C7 H7 109.0 . . ? C7 C8 C3 109.9(3) . . ? C7 C8 H8A 109.7 . . ? C3 C8 H8A 109.7 . . ? C7 C8 H8B 109.7 . . ? C3 C8 H8B 109.7 . . ? H8A C8 H8B 108.2 . . ? C11 C9 C3 112.7(2) . . ? C11 C9 H9A 109.0 . . ? C3 C9 H9A 109.0 . . ? C11 C9 H9B 109.0 . . ? C3 C9 H9B 109.0 . . ? H9A C9 H9B 107.8 . . ? C5 C10 C11 110.9(3) . . ? C5 C10 H10A 109.5 . . ? C11 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? C11 C10 H10B 109.5 . . ? H10A C10 H10B 108.0 . . ? C9 C11 C10 108.0(2) . . ? C9 C11 C12 110.9(3) . . ? C10 C11 C12 108.6(3) . . ? C9 C11 C26 108.6(3) . . ? C10 C11 C26 107.6(3) . . ? C12 C11 C26 113.0(3) . . ? C13 C12 C11 115.8(3) . . ? C13 C12 H12A 108.3 . . ? C11 C12 H12A 108.3 . . ? C13 C12 H12B 108.3 . . ? C11 C12 H12B 108.3 . . ? H12A C12 H12B 107.4 . . ? O3 C13 O4 124.5(3) . . ? O3 C13 C12 120.0(3) . . ? O4 C13 C12 115.6(3) . . ? N1 C14 C15 123.1(3) . . ? N1 C14 H14 118.4 . . ? C15 C14 H14 118.4 . . ? C14 C15 C16 119.6(3) . . ? C14 C15 H15 120.2 . . ? C16 C15 H15 120.2 . . ? C15 C16 C15 117.1(4) 2_554 . ? C15 C16 C17 121.47(19) 2_554 . ? C15 C16 C17 121.47(19) . . ? C18 C17 C18 117.6(4) 2_554 . ? C18 C17 C16 121.22(18) 2_554 . ? C18 C17 C16 121.22(18) . . ? C19 C18 C17 119.5(3) . . ? C19 C18 H18 120.2 . . ? C17 C18 H18 120.2 . . ? N2 C19 C18 123.1(3) . . ? N2 C19 H19 118.4 . . ? C18 C19 H19 118.4 . . ? C7 C26 C11 109.7(3) . . ? C7 C26 H26A 109.7 . . ? C11 C26 H26A 109.7 . . ? C7 C26 H26B 109.7 . . ? C11 C26 H26B 109.7 . . ? H26A C26 H26B 108.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Zn1 Zn2 O4 -99.88(9) . . . 7 ? O1 Zn1 Zn2 O4 80.12(9) 2_554 . . 7 ? N1 Zn1 Zn2 O4 146(100) . . . 7 ? O3 Zn1 Zn2 O4 169.99(9) 8_455 . . 7 ? O3 Zn1 Zn2 O4 -10.01(9) 7 . . 7 ? O1 Zn1 Zn2 O4 80.12(9) . . . 8_455 ? O1 Zn1 Zn2 O4 -99.88(9) 2_554 . . 8_455 ? N1 Zn1 Zn2 O4 -34(100) . . . 8_455 ? O3 Zn1 Zn2 O4 -10.01(9) 8_455 . . 8_455 ? O3 Zn1 Zn2 O4 169.99(9) 7 . . 8_455 ? O1 Zn1 Zn2 N2 -119(100) . . . 1_545 ? O1 Zn1 Zn2 N2 61(100) 2_554 . . 1_545 ? N1 Zn1 Zn2 N2 0.0 . . . 1_545 ? O3 Zn1 Zn2 N2 151(100) 8_455 . . 1_545 ? O3 Zn1 Zn2 N2 -29(100) 7 . . 1_545 ? O1 Zn1 Zn2 O2 -10.88(9) . . . . ? O1 Zn1 Zn2 O2 169.12(9) 2_554 . . . ? N1 Zn1 Zn2 O2 -125(100) . . . . ? O3 Zn1 Zn2 O2 -101.01(9) 8_455 . . . ? O3 Zn1 Zn2 O2 78.99(9) 7 . . . ? O1 Zn1 Zn2 O2 169.12(9) . . . 2_554 ? O1 Zn1 Zn2 O2 -10.88(9) 2_554 . . 2_554 ? N1 Zn1 Zn2 O2 55(100) . . . 2_554 ? O3 Zn1 Zn2 O2 78.99(9) 8_455 . . 2_554 ? O3 Zn1 Zn2 O2 -101.01(9) 7 . . 2_554 ? O1 Zn1 N1 C14 -23.45(18) . . . . ? O1 Zn1 N1 C14 156.55(18) 2_554 . . . ? O3 Zn1 N1 C14 66.68(18) 8_455 . . . ? O3 Zn1 N1 C14 -113.32(18) 7 . . . ? Zn2 Zn1 N1 C14 90(100) . . . . ? O1 Zn1 N1 C14 156.55(18) . . . 2_554 ? O1 Zn1 N1 C14 -23.45(18) 2_554 . . 2_554 ? O3 Zn1 N1 C14 -113.32(18) 8_455 . . 2_554 ? O3 Zn1 N1 C14 66.68(18) 7 . . 2_554 ? Zn2 Zn1 N1 C14 -90(100) . . . 2_554 ? O1 Zn1 O1 C1 19.7(2) 2_554 . . . ? N1 Zn1 O1 C1 -160.3(2) . . . . ? O3 Zn1 O1 C1 97.0(2) 8_455 . . . ? O3 Zn1 O1 C1 -57.7(2) 7 . . . ? Zn2 Zn1 O1 C1 19.7(2) . . . . ? O4 Zn2 O2 C1 91.0(3) 7 . . . ? O4 Zn2 O2 C1 -75.5(3) 8_455 . . . ? N2 Zn2 O2 C1 -172.5(3) 1_545 . . . ? O2 Zn2 O2 C1 7.5(3) 2_554 . . . ? Zn1 Zn2 O2 C1 7.5(3) . . . . ? Zn2 O2 C1 O1 5.3(5) . . . . ? Zn2 O2 C1 C2 -173.4(2) . . . . ? Zn1 O1 C1 O2 -21.3(4) . . . . ? Zn1 O1 C1 C2 157.3(2) . . . . ? O2 C1 C2 C3 -172.7(3) . . . . ? O1 C1 C2 C3 8.6(5) . . . . ? C1 C2 C3 C9 -175.2(3) . . . . ? C1 C2 C3 C4 66.9(4) . . . . ? C1 C2 C3 C8 -56.1(4) . . . . ? C9 C3 C4 C5 58.5(3) . . . . ? C8 C3 C4 C5 -58.7(3) . . . . ? C2 C3 C4 C5 175.6(3) . . . . ? C3 C4 C5 C6 60.7(3) . . . . ? C3 C4 C5 C10 -59.7(3) . . . . ? C4 C5 C6 C7 -61.1(3) . . . . ? C10 C5 C6 C7 59.8(3) . . . . ? C5 C6 C7 C26 -60.1(3) . . . . ? C5 C6 C7 C8 61.1(3) . . . . ? C6 C7 C8 C3 -60.6(3) . . . . ? C26 C7 C8 C3 61.0(3) . . . . ? C9 C3 C8 C7 -58.2(3) . . . . ? C4 C3 C8 C7 58.9(3) . . . . ? C2 C3 C8 C7 -176.4(3) . . . . ? C4 C3 C9 C11 -59.4(3) . . . . ? C8 C3 C9 C11 58.1(3) . . . . ? C2 C3 C9 C11 -179.6(2) . . . . ? C6 C5 C10 C11 -61.6(3) . . . . ? C4 C5 C10 C11 59.2(3) . . . . ? C3 C9 C11 C10 58.3(3) . . . . ? C3 C9 C11 C12 177.2(2) . . . . ? C3 C9 C11 C26 -58.1(3) . . . . ? C5 C10 C11 C9 -57.1(3) . . . . ? C5 C10 C11 C12 -177.4(3) . . . . ? C5 C10 C11 C26 60.0(3) . . . . ? C9 C11 C12 C13 73.2(3) . . . . ? C10 C11 C12 C13 -168.2(2) . . . . ? C26 C11 C12 C13 -48.9(4) . . . . ? Zn1 O3 C13 O4 2.0(5) 7 . . . ? Zn1 O3 C13 C12 -177.03(19) 7 . . . ? Zn2 O4 C13 O3 13.9(4) 7 . . . ? Zn2 O4 C13 C12 -167.07(19) 7 . . . ? C11 C12 C13 O3 -98.4(3) . . . . ? C11 C12 C13 O4 82.5(3) . . . . ? C14 N1 C14 C15 1.1(2) 2_554 . . . ? Zn1 N1 C14 C15 -178.9(2) . . . . ? N1 C14 C15 C16 -2.2(5) . . . . ? C14 C15 C16 C15 1.0(2) . . . 2_554 ? C14 C15 C16 C17 -179.0(2) . . . . ? C15 C16 C17 C18 136.8(2) 2_554 . . 2_554 ? C15 C16 C17 C18 -43.2(2) . . . 2_554 ? C15 C16 C17 C18 -43.2(2) 2_554 . . . ? C15 C16 C17 C18 136.8(2) . . . . ? C18 C17 C18 C19 1.1(2) 2_554 . . . ? C16 C17 C18 C19 -178.9(2) . . . . ? C19 N2 C19 C18 1.2(2) 2_554 . . . ? Zn2 N2 C19 C18 -178.8(2) 1_565 . . . ? C17 C18 C19 N2 -2.3(4) . . . . ? C6 C7 C26 C11 60.1(3) . . . . ? C8 C7 C26 C11 -60.8(3) . . . . ? C9 C11 C26 C7 58.1(3) . . . . ? C10 C11 C26 C7 -58.6(3) . . . . ? C12 C11 C26 C7 -178.4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.555 _refine_diff_density_min -0.502 _refine_diff_density_rms 0.082 data_3 _database_code_depnum_ccdc_archive 'CCDC 761113' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H48 N2 O8 Zn2' _chemical_formula_sum 'C40 H48 N2 O8 Zn2' _chemical_formula_weight 815.54 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 Pc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' _cell_length_a 11.617(4) _cell_length_b 10.670(4) _cell_length_c 15.830(6) _cell_angle_alpha 90.00 _cell_angle_beta 108.996(6) _cell_angle_gamma 90.00 _cell_volume 1855.3(11) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 2050 _cell_measurement_theta_min 2.342 _cell_measurement_theta_max 22.191 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.460 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 852 _exptl_absorpt_coefficient_mu 1.348 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7649 _exptl_absorpt_correction_T_max 0.8132 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9029 _diffrn_reflns_av_R_equivalents 0.0662 _diffrn_reflns_av_sigmaI/netI 0.0975 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 25.09 _reflns_number_total 4528 _reflns_number_gt 3208 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1012P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.09(2) _refine_ls_number_reflns 4528 _refine_ls_number_parameters 469 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0769 _refine_ls_R_factor_gt 0.0519 _refine_ls_wR_factor_ref 0.1579 _refine_ls_wR_factor_gt 0.1266 _refine_ls_goodness_of_fit_ref 0.966 _refine_ls_restrained_S_all 0.966 _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 1.04237(8) 0.37888(10) 0.22676(6) 0.0384(3) Uani 1 1 d . . . Zn2 Zn 0.85755(9) 0.46213(10) 0.03921(7) 0.0385(3) Uani 1 1 d . . . N1 N 0.1596(7) 0.3808(7) -0.6469(5) 0.0360(19) Uani 1 1 d . . . N2 N 0.7450(8) 0.4008(8) -0.0881(5) 0.046(2) Uani 1 1 d . . . O1 O 0.9163(6) 0.2600(7) 0.2267(4) 0.0485(18) Uani 1 1 d . . . O2 O 0.7896(6) 0.3257(6) 0.0980(4) 0.056(2) Uani 1 1 d . . . O3 O 0.7245(6) 0.3909(6) 0.5364(4) 0.0485(17) Uani 1 1 d . . . O4 O 0.8801(6) 0.3566(6) 0.4925(4) 0.0493(17) Uani 1 1 d . . . O5 O 0.9608(7) 0.5405(6) 0.1884(4) 0.0486(18) Uani 1 1 d . . . O6 O 1.1478(7) 0.5970(7) 0.2003(4) 0.0524(18) Uani 1 1 d . . . O7 O 1.0088(6) 0.6151(6) 0.5268(4) 0.0421(16) Uani 1 1 d . . . O8 O 1.1275(7) 0.6944(7) 0.6554(4) 0.0500(17) Uani 1 1 d . . . C1 C 0.8206(8) 0.2480(9) 0.1607(5) 0.038(2) Uani 1 1 d . . . C2 C 0.7381(9) 0.1374(8) 0.1601(6) 0.045(2) Uani 1 1 d . . . H2A H 0.6822 0.1271 0.0998 0.054 Uiso 1 1 calc R . . H2B H 0.7879 0.0624 0.1748 0.054 Uiso 1 1 calc R . . C3 C 0.6662(8) 0.1464(8) 0.2218(6) 0.037(2) Uani 1 1 d . . . C4 C 0.5956(10) 0.0195(9) 0.2163(6) 0.044(2) Uani 1 1 d . . . H4A H 0.5453 0.0045 0.1549 0.052 Uiso 1 1 calc R . . H4B H 0.6536 -0.0487 0.2345 0.052 Uiso 1 1 calc R . . C5 C 0.5167(8) 0.0215(9) 0.2749(6) 0.038(2) Uani 1 1 d . . . H5 H 0.4739 -0.0586 0.2704 0.045 Uiso 1 1 calc R . . C6 C 0.5985(9) 0.0429(8) 0.3712(6) 0.039(2) Uani 1 1 d . . . H6A H 0.5502 0.0385 0.4108 0.047 Uiso 1 1 calc R . . H6B H 0.6598 -0.0224 0.3884 0.047 Uiso 1 1 calc R . . C7 C 0.6590(8) 0.1676(8) 0.3802(6) 0.035(2) Uani 1 1 d . . . C8 C 0.7419(9) 0.1695(8) 0.3203(6) 0.037(2) Uani 1 1 d . . . H8A H 0.7824 0.2501 0.3259 0.044 Uiso 1 1 calc R . . H8B H 0.8039 0.1053 0.3402 0.044 Uiso 1 1 calc R . . C9 C 0.5648(8) 0.2712(9) 0.3503(6) 0.042(2) Uani 1 1 d . . . H9A H 0.6053 0.3518 0.3561 0.051 Uiso 1 1 calc R . . H9B H 0.5133 0.2718 0.3878 0.051 Uiso 1 1 calc R . . C10 C 0.4867(9) 0.2495(9) 0.2524(6) 0.043(2) Uani 1 1 d . . . H10 H 0.4256 0.3160 0.2332 0.052 Uiso 1 1 calc R . . C11 C 0.4254(10) 0.1268(10) 0.2445(7) 0.054(3) Uani 1 1 d . . . H11A H 0.3760 0.1129 0.1828 0.065 Uiso 1 1 calc R . . H11B H 0.3719 0.1269 0.2805 0.065 Uiso 1 1 calc R . . C12 C 0.5702(8) 0.2515(9) 0.1936(6) 0.037(2) Uani 1 1 d . . . H12A H 0.5213 0.2405 0.1315 0.044 Uiso 1 1 calc R . . H12B H 0.6107 0.3321 0.1995 0.044 Uiso 1 1 calc R . . C13 C 0.7400(9) 0.1872(9) 0.4796(6) 0.045(2) Uani 1 1 d . . . H13A H 0.6931 0.1631 0.5177 0.054 Uiso 1 1 calc R . . H13B H 0.8091 0.1308 0.4924 0.054 Uiso 1 1 calc R . . C14 C 0.7871(9) 0.3177(9) 0.5043(5) 0.038(2) Uani 1 1 d . . . C15 C 1.0409(12) 0.6250(10) 0.1952(5) 0.052(3) Uani 1 1 d . . . C16 C 1.0019(9) 0.7564(10) 0.2029(6) 0.047(3) Uani 1 1 d . . . H16A H 0.9171 0.7562 0.1996 0.056 Uiso 1 1 calc R . . H16B H 1.0083 0.8044 0.1526 0.056 Uiso 1 1 calc R . . C17 C 1.0780(8) 0.8216(8) 0.2904(6) 0.037(2) Uani 1 1 d . . . C18 C 1.0056(10) 0.9368(9) 0.3092(7) 0.053(3) Uani 1 1 d . . . H18A H 0.9874 0.9951 0.2596 0.063 Uiso 1 1 calc R . . H18B H 0.9291 0.9084 0.3149 0.063 Uiso 1 1 calc R . . C19 C 1.0807(11) 1.0026(9) 0.3951(8) 0.054(3) Uani 1 1 d . . . H19 H 1.0370 1.0766 0.4053 0.065 Uiso 1 1 calc R . . C20 C 1.2058(10) 1.0423(9) 0.3869(8) 0.059(3) Uani 1 1 d . . . H20A H 1.1929 1.1008 0.3378 0.071 Uiso 1 1 calc R . . H20B H 1.2542 1.0839 0.4414 0.071 Uiso 1 1 calc R . . C21 C 1.2707(10) 0.9317(9) 0.3714(7) 0.045(3) Uani 1 1 d . . . H21 H 1.3492 0.9591 0.3671 0.054 Uiso 1 1 calc R . . C22 C 1.2008(9) 0.8672(9) 0.2853(6) 0.043(2) Uani 1 1 d . . . H22A H 1.2473 0.7966 0.2753 0.051 Uiso 1 1 calc R . . H22B H 1.1875 0.9251 0.2358 0.051 Uiso 1 1 calc R . . C23 C 1.1005(8) 0.7322(8) 0.3702(5) 0.033(2) Uani 1 1 d . . . H23A H 1.0229 0.7035 0.3735 0.040 Uiso 1 1 calc R . . H23B H 1.1450 0.6594 0.3608 0.040 Uiso 1 1 calc R . . C24 C 1.1720(8) 0.7941(8) 0.4581(6) 0.037(2) Uani 1 1 d . . . C25 C 1.2954(9) 0.8406(9) 0.4498(6) 0.039(2) Uani 1 1 d . . . H25A H 1.3426 0.8822 0.5047 0.046 Uiso 1 1 calc R . . H25B H 1.3420 0.7697 0.4405 0.046 Uiso 1 1 calc R . . C26 C 1.0999(11) 0.9085(9) 0.4727(7) 0.053(3) Uani 1 1 d . . . H26A H 1.1441 0.9487 0.5289 0.063 Uiso 1 1 calc R . . H26B H 1.0216 0.8815 0.4758 0.063 Uiso 1 1 calc R . . C27 C 1.2043(8) 0.7016(9) 0.5350(6) 0.038(2) Uani 1 1 d . . . H27A H 1.2320 0.6249 0.5151 0.045 Uiso 1 1 calc R . . H27B H 1.2724 0.7356 0.5828 0.045 Uiso 1 1 calc R . . C28 C 1.1049(9) 0.6680(8) 0.5737(6) 0.038(2) Uani 1 1 d . . . C29 C 0.1177(9) 0.3536(9) -0.5779(6) 0.037(2) Uani 1 1 d . . . H29 H 0.0367 0.3309 -0.5895 0.045 Uiso 1 1 calc R . . C30 C 0.1954(10) 0.3598(9) -0.4908(6) 0.047(3) Uani 1 1 d . . . H30 H 0.1669 0.3409 -0.4437 0.057 Uiso 1 1 calc R . . C31 C 0.3184(9) 0.3949(10) -0.4734(6) 0.046(3) Uani 1 1 d . . . C32 C 0.3564(10) 0.4200(11) -0.5457(7) 0.053(3) Uani 1 1 d . . . H32 H 0.4368 0.4429 -0.5368 0.063 Uiso 1 1 calc R . . C33 C 0.2746(9) 0.4110(10) -0.6315(6) 0.046(3) Uani 1 1 d . . . H33 H 0.3016 0.4267 -0.6797 0.055 Uiso 1 1 calc R . . C34 C 0.4033(12) 0.4127(14) -0.3799(8) 0.074(4) Uani 1 1 d . . . H34A H 0.4408 0.4948 -0.3754 0.089 Uiso 1 1 calc R . . H34B H 0.3563 0.4111 -0.3392 0.089 Uiso 1 1 calc R . . C35 C 0.4992(12) 0.3178(12) -0.3517(7) 0.081(5) Uani 1 1 d . . . H35A H 0.5440 0.3158 -0.3938 0.097 Uiso 1 1 calc R . . H35B H 0.4626 0.2360 -0.3520 0.097 Uiso 1 1 calc R . . C36 C 0.5872(12) 0.3456(11) -0.2580(7) 0.059(3) Uani 1 1 d . . . C37 C 0.5543(10) 0.3286(11) -0.1829(7) 0.051(3) Uani 1 1 d . . . H37 H 0.4773 0.2979 -0.1883 0.061 Uiso 1 1 calc R . . C38 C 0.6347(10) 0.3566(10) -0.0998(6) 0.049(3) Uani 1 1 d . . . H38 H 0.6104 0.3440 -0.0499 0.058 Uiso 1 1 calc R . . C39 C 0.7781(10) 0.4200(10) -0.1611(6) 0.045(2) Uani 1 1 d . . . H39 H 0.8548 0.4531 -0.1539 0.054 Uiso 1 1 calc R . . C40 C 0.7022(10) 0.3922(10) -0.2464(6) 0.052(3) Uani 1 1 d . . . H40 H 0.7284 0.4048 -0.2954 0.062 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0376(6) 0.0574(7) 0.0172(5) 0.0019(5) 0.0048(4) 0.0002(6) Zn2 0.0383(6) 0.0498(6) 0.0240(5) 0.0067(5) 0.0056(4) 0.0042(5) N1 0.039(5) 0.049(5) 0.021(4) 0.000(3) 0.010(3) 0.005(4) N2 0.040(5) 0.062(6) 0.027(4) 0.009(4) 0.000(4) -0.011(4) O1 0.038(4) 0.073(5) 0.027(3) 0.010(3) -0.001(3) -0.003(3) O2 0.060(5) 0.066(5) 0.026(3) 0.014(3) -0.005(3) -0.019(4) O3 0.055(4) 0.058(4) 0.033(4) -0.002(3) 0.015(3) -0.002(3) O4 0.046(4) 0.068(5) 0.034(3) 0.003(3) 0.014(3) -0.017(4) O5 0.056(4) 0.045(4) 0.033(3) 0.008(3) -0.002(3) -0.008(4) O6 0.044(4) 0.079(5) 0.034(4) -0.006(3) 0.012(3) -0.008(4) O7 0.040(4) 0.061(4) 0.026(3) -0.004(3) 0.011(3) -0.012(3) O8 0.065(5) 0.065(4) 0.027(3) -0.006(3) 0.024(3) -0.013(4) C1 0.042(5) 0.051(6) 0.022(4) -0.007(4) 0.014(4) -0.008(4) C2 0.052(6) 0.049(6) 0.030(5) -0.003(4) 0.009(4) 0.003(5) C3 0.043(6) 0.042(5) 0.024(4) 0.000(4) 0.006(4) -0.008(4) C4 0.053(6) 0.039(5) 0.033(5) 0.000(4) 0.006(4) -0.008(5) C5 0.032(5) 0.046(5) 0.036(5) -0.002(4) 0.011(4) -0.017(4) C6 0.038(5) 0.044(5) 0.032(5) -0.002(4) 0.007(4) -0.001(4) C7 0.035(5) 0.041(5) 0.033(5) 0.000(4) 0.015(4) -0.006(4) C8 0.042(5) 0.036(5) 0.028(5) 0.006(4) 0.005(4) 0.002(4) C9 0.043(5) 0.053(6) 0.035(5) 0.004(4) 0.018(4) -0.007(5) C10 0.034(5) 0.053(6) 0.036(5) 0.009(4) 0.003(4) 0.003(5) C11 0.044(6) 0.080(8) 0.031(5) 0.010(5) 0.004(4) -0.020(6) C12 0.032(5) 0.041(5) 0.031(5) 0.001(4) 0.002(4) 0.004(4) C13 0.051(6) 0.056(6) 0.027(5) 0.002(4) 0.012(4) 0.004(5) C14 0.039(6) 0.058(6) 0.014(4) 0.001(4) 0.003(4) 0.004(5) C15 0.083(9) 0.053(7) 0.012(4) 0.004(4) 0.006(5) -0.018(7) C16 0.039(6) 0.069(7) 0.026(5) 0.002(4) 0.003(4) -0.008(5) C17 0.038(5) 0.042(5) 0.032(5) 0.009(4) 0.011(4) -0.003(4) C18 0.047(6) 0.053(6) 0.052(6) 0.011(5) 0.007(5) 0.010(5) C19 0.059(7) 0.035(5) 0.071(8) -0.003(5) 0.027(6) 0.006(5) C20 0.070(8) 0.043(6) 0.063(7) 0.009(5) 0.018(6) -0.018(6) C21 0.049(7) 0.043(6) 0.049(6) 0.006(5) 0.025(5) -0.015(5) C22 0.044(6) 0.049(6) 0.038(5) 0.007(4) 0.017(4) -0.012(5) C23 0.040(5) 0.033(5) 0.022(4) -0.001(3) 0.004(4) -0.009(4) C24 0.035(5) 0.040(5) 0.031(5) -0.001(4) 0.006(4) -0.008(4) C25 0.038(5) 0.050(6) 0.029(5) 0.000(4) 0.012(4) -0.007(4) C26 0.066(7) 0.052(6) 0.041(5) -0.012(5) 0.018(5) -0.001(5) C27 0.032(5) 0.053(6) 0.029(4) 0.004(4) 0.012(4) -0.008(4) C28 0.045(6) 0.046(5) 0.022(4) 0.001(4) 0.011(4) 0.003(4) C29 0.039(6) 0.046(5) 0.031(5) 0.000(4) 0.016(4) 0.000(5) C30 0.061(7) 0.072(7) 0.012(4) 0.006(4) 0.016(4) 0.013(5) C31 0.038(6) 0.069(7) 0.028(5) 0.001(5) 0.008(4) 0.008(5) C32 0.032(6) 0.076(7) 0.043(6) -0.013(5) 0.003(5) 0.014(5) C33 0.034(6) 0.075(7) 0.026(5) -0.004(5) 0.008(4) 0.011(5) C34 0.067(9) 0.110(11) 0.031(6) -0.013(7) -0.003(6) 0.022(8) C35 0.095(10) 0.083(9) 0.030(6) -0.009(6) -0.027(6) 0.009(8) C36 0.075(9) 0.065(7) 0.021(5) 0.004(4) -0.006(5) 0.004(6) C37 0.039(6) 0.068(7) 0.044(6) -0.005(5) 0.011(5) -0.004(5) C38 0.050(7) 0.075(7) 0.022(5) -0.002(4) 0.014(4) 0.003(6) C39 0.036(6) 0.067(6) 0.035(5) 0.005(5) 0.017(4) 0.020(5) C40 0.051(7) 0.075(7) 0.027(5) 0.004(5) 0.008(4) 0.015(6) _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 O8 1.896(7) 2_564 ? Zn1 O1 1.937(7) . ? Zn1 O5 1.966(6) . ? Zn1 N1 2.020(7) 1_656 ? Zn2 O7 2.007(7) 2_564 ? Zn2 O2 2.021(7) . ? Zn2 O4 2.118(7) 2_564 ? Zn2 N2 2.118(8) . ? Zn2 O3 2.191(7) 2_564 ? Zn2 O5 2.423(6) . ? Zn2 C14 2.490(10) 2_564 ? N1 C33 1.318(13) . ? N1 C29 1.364(13) . ? N1 Zn1 2.020(7) 1_454 ? N2 C38 1.321(14) . ? N2 C39 1.347(13) . ? O1 C1 1.260(10) . ? O2 C1 1.253(10) . ? O3 C14 1.279(11) . ? O3 Zn2 2.191(7) 2_565 ? O4 C14 1.227(11) . ? O4 Zn2 2.118(7) 2_565 ? O5 C15 1.274(12) . ? O6 C15 1.254(14) . ? O7 C28 1.255(11) . ? O7 Zn2 2.007(7) 2_565 ? O8 C28 1.265(10) . ? O8 Zn1 1.896(7) 2_565 ? C1 C2 1.518(13) . ? C2 C3 1.481(14) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C12 1.542(12) . ? C3 C8 1.541(12) . ? C3 C4 1.571(12) . ? C4 C5 1.502(14) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C11 1.511(14) . ? C5 C6 1.529(12) . ? C5 H5 0.9800 . ? C6 C7 1.489(12) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C9 1.519(13) . ? C7 C8 1.557(13) . ? C7 C13 1.563(12) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.537(12) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.477(13) . ? C10 C12 1.547(13) . ? C10 H10 0.9800 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.501(14) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 Zn2 2.490(10) 2_565 ? C15 C16 1.490(14) . ? C16 C17 1.545(12) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C23 1.535(11) . ? C17 C22 1.534(13) . ? C17 C18 1.572(14) . ? C18 C19 1.526(15) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C26 1.546(15) . ? C19 C20 1.559(16) . ? C19 H19 0.9800 . ? C20 C21 1.464(15) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.506(14) . ? C21 C25 1.529(13) . ? C21 H21 0.9800 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.520(11) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C27 1.517(12) . ? C24 C26 1.541(14) . ? C24 C25 1.562(13) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.515(13) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C29 C30 1.382(13) . ? C29 H29 0.9300 . ? C30 C31 1.415(15) . ? C30 H30 0.9300 . ? C31 C32 1.381(15) . ? C31 C34 1.500(14) . ? C32 C33 1.385(13) . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? C34 C35 1.464(17) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.532(13) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 C40 1.382(17) . ? C36 C37 1.373(17) . ? C37 C38 1.376(14) . ? C37 H37 0.9300 . ? C38 H38 0.9300 . ? C39 C40 1.383(14) . ? C39 H39 0.9300 . ? C40 H40 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O8 Zn1 O1 105.7(3) 2_564 . ? O8 Zn1 O5 118.0(3) 2_564 . ? O1 Zn1 O5 106.6(3) . . ? O8 Zn1 N1 106.3(3) 2_564 1_656 ? O1 Zn1 N1 105.8(3) . 1_656 ? O5 Zn1 N1 113.5(3) . 1_656 ? O7 Zn2 O2 103.6(3) 2_564 . ? O7 Zn2 O4 97.4(3) 2_564 2_564 ? O2 Zn2 O4 158.4(3) . 2_564 ? O7 Zn2 N2 93.9(3) 2_564 . ? O2 Zn2 N2 90.2(3) . . ? O4 Zn2 N2 93.3(3) 2_564 . ? O7 Zn2 O3 157.7(3) 2_564 2_564 ? O2 Zn2 O3 98.4(3) . 2_564 ? O4 Zn2 O3 60.4(3) 2_564 2_564 ? N2 Zn2 O3 89.4(3) . 2_564 ? O7 Zn2 O5 93.8(3) 2_564 . ? O2 Zn2 O5 86.8(2) . . ? O4 Zn2 O5 87.0(2) 2_564 . ? N2 Zn2 O5 172.2(3) . . ? O3 Zn2 O5 84.0(2) 2_564 . ? O7 Zn2 C14 126.9(3) 2_564 2_564 ? O2 Zn2 C14 129.2(3) . 2_564 ? O4 Zn2 C14 29.5(3) 2_564 2_564 ? N2 Zn2 C14 91.4(3) . 2_564 ? O3 Zn2 C14 30.9(3) 2_564 2_564 ? O5 Zn2 C14 85.0(2) . 2_564 ? C33 N1 C29 120.6(8) . . ? C33 N1 Zn1 120.1(6) . 1_454 ? C29 N1 Zn1 119.3(7) . 1_454 ? C38 N2 C39 118.0(9) . . ? C38 N2 Zn2 120.9(7) . . ? C39 N2 Zn2 120.6(7) . . ? C1 O1 Zn1 122.0(6) . . ? C1 O2 Zn2 141.8(6) . . ? C14 O3 Zn2 87.5(6) . 2_565 ? C14 O4 Zn2 92.3(6) . 2_565 ? C15 O5 Zn1 109.2(7) . . ? C15 O5 Zn2 116.3(6) . . ? Zn1 O5 Zn2 92.0(3) . . ? C28 O7 Zn2 139.9(6) . 2_565 ? C28 O8 Zn1 122.9(6) . 2_565 ? O2 C1 O1 122.6(8) . . ? O2 C1 C2 119.4(8) . . ? O1 C1 C2 118.0(8) . . ? C3 C2 C1 115.8(8) . . ? C3 C2 H2A 108.3 . . ? C1 C2 H2A 108.3 . . ? C3 C2 H2B 108.3 . . ? C1 C2 H2B 108.3 . . ? H2A C2 H2B 107.4 . . ? C2 C3 C12 111.6(8) . . ? C2 C3 C8 114.8(8) . . ? C12 C3 C8 107.3(8) . . ? C2 C3 C4 107.7(8) . . ? C12 C3 C4 107.2(8) . . ? C8 C3 C4 108.0(7) . . ? C5 C4 C3 111.5(8) . . ? C5 C4 H4A 109.3 . . ? C3 C4 H4A 109.3 . . ? C5 C4 H4B 109.3 . . ? C3 C4 H4B 109.3 . . ? H4A C4 H4B 108.0 . . ? C4 C5 C11 108.7(8) . . ? C4 C5 C6 108.1(7) . . ? C11 C5 C6 110.5(8) . . ? C4 C5 H5 109.8 . . ? C11 C5 H5 109.8 . . ? C6 C5 H5 109.8 . . ? C7 C6 C5 110.5(7) . . ? C7 C6 H6A 109.6 . . ? C5 C6 H6A 109.6 . . ? C7 C6 H6B 109.6 . . ? C5 C6 H6B 109.6 . . ? H6A C6 H6B 108.1 . . ? C6 C7 C9 110.6(8) . . ? C6 C7 C8 108.6(8) . . ? C9 C7 C8 109.0(7) . . ? C6 C7 C13 109.1(7) . . ? C9 C7 C13 110.7(7) . . ? C8 C7 C13 108.8(7) . . ? C3 C8 C7 110.6(7) . . ? C3 C8 H8A 109.5 . . ? C7 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 108.1 . . ? C7 C9 C10 109.4(8) . . ? C7 C9 H9A 109.8 . . ? C10 C9 H9A 109.8 . . ? C7 C9 H9B 109.8 . . ? C10 C9 H9B 109.8 . . ? H9A C9 H9B 108.2 . . ? C11 C10 C9 109.3(8) . . ? C11 C10 C12 109.9(9) . . ? C9 C10 C12 109.0(7) . . ? C11 C10 H10 109.6 . . ? C9 C10 H10 109.6 . . ? C12 C10 H10 109.6 . . ? C10 C11 C5 111.3(8) . . ? C10 C11 H11A 109.4 . . ? C5 C11 H11A 109.4 . . ? C10 C11 H11B 109.4 . . ? C5 C11 H11B 109.4 . . ? H11A C11 H11B 108.0 . . ? C3 C12 C10 110.6(8) . . ? C3 C12 H12A 109.5 . . ? C10 C12 H12A 109.5 . . ? C3 C12 H12B 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 108.1 . . ? C14 C13 C7 115.9(7) . . ? C14 C13 H13A 108.3 . . ? C7 C13 H13A 108.3 . . ? C14 C13 H13B 108.3 . . ? C7 C13 H13B 108.3 . . ? H13A C13 H13B 107.4 . . ? O4 C14 O3 119.8(9) . . ? O4 C14 C13 122.5(9) . . ? O3 C14 C13 117.7(9) . . ? O4 C14 Zn2 58.2(5) . 2_565 ? O3 C14 Zn2 61.6(5) . 2_565 ? C13 C14 Zn2 177.3(6) . 2_565 ? O6 C15 O5 121.2(10) . . ? O6 C15 C16 122.6(10) . . ? O5 C15 C16 116.1(12) . . ? C15 C16 C17 113.4(7) . . ? C15 C16 H16A 108.9 . . ? C17 C16 H16A 108.9 . . ? C15 C16 H16B 108.9 . . ? C17 C16 H16B 108.9 . . ? H16A C16 H16B 107.7 . . ? C23 C17 C22 109.2(7) . . ? C23 C17 C16 110.6(7) . . ? C22 C17 C16 111.5(8) . . ? C23 C17 C18 106.8(8) . . ? C22 C17 C18 109.0(8) . . ? C16 C17 C18 109.7(7) . . ? C19 C18 C17 110.0(8) . . ? C19 C18 H18A 109.7 . . ? C17 C18 H18A 109.7 . . ? C19 C18 H18B 109.7 . . ? C17 C18 H18B 109.7 . . ? H18A C18 H18B 108.2 . . ? C18 C19 C26 107.6(8) . . ? C18 C19 C20 109.2(10) . . ? C26 C19 C20 110.2(9) . . ? C18 C19 H19 109.9 . . ? C26 C19 H19 109.9 . . ? C20 C19 H19 109.9 . . ? C21 C20 C19 109.9(8) . . ? C21 C20 H20A 109.7 . . ? C19 C20 H20A 109.7 . . ? C21 C20 H20B 109.7 . . ? C19 C20 H20B 109.7 . . ? H20A C20 H20B 108.2 . . ? C20 C21 C22 111.4(9) . . ? C20 C21 C25 110.2(9) . . ? C22 C21 C25 110.4(8) . . ? C20 C21 H21 108.2 . . ? C22 C21 H21 108.2 . . ? C25 C21 H21 108.2 . . ? C21 C22 C17 109.5(8) . . ? C21 C22 H22A 109.8 . . ? C17 C22 H22A 109.8 . . ? C21 C22 H22B 109.8 . . ? C17 C22 H22B 109.8 . . ? H22A C22 H22B 108.2 . . ? C24 C23 C17 112.3(7) . . ? C24 C23 H23A 109.2 . . ? C17 C23 H23A 109.2 . . ? C24 C23 H23B 109.2 . . ? C17 C23 H23B 109.2 . . ? H23A C23 H23B 107.9 . . ? C27 C24 C23 111.8(7) . . ? C27 C24 C26 113.5(8) . . ? C23 C24 C26 108.7(7) . . ? C27 C24 C25 106.3(7) . . ? C23 C24 C25 107.7(8) . . ? C26 C24 C25 108.6(8) . . ? C21 C25 C24 109.6(8) . . ? C21 C25 H25A 109.7 . . ? C24 C25 H25A 109.7 . . ? C21 C25 H25B 109.7 . . ? C24 C25 H25B 109.7 . . ? H25A C25 H25B 108.2 . . ? C24 C26 C19 109.8(9) . . ? C24 C26 H26A 109.7 . . ? C19 C26 H26A 109.7 . . ? C24 C26 H26B 109.7 . . ? C19 C26 H26B 109.7 . . ? H26A C26 H26B 108.2 . . ? C28 C27 C24 117.2(7) . . ? C28 C27 H27A 108.0 . . ? C24 C27 H27A 108.0 . . ? C28 C27 H27B 108.0 . . ? C24 C27 H27B 108.0 . . ? H27A C27 H27B 107.2 . . ? O7 C28 O8 123.6(9) . . ? O7 C28 C27 121.0(8) . . ? O8 C28 C27 115.3(8) . . ? N1 C29 C30 120.1(9) . . ? N1 C29 H29 119.9 . . ? C30 C29 H29 119.9 . . ? C29 C30 C31 119.8(9) . . ? C29 C30 H30 120.1 . . ? C31 C30 H30 120.1 . . ? C32 C31 C30 117.8(9) . . ? C32 C31 C34 120.6(11) . . ? C30 C31 C34 121.5(10) . . ? C31 C32 C33 119.8(11) . . ? C31 C32 H32 120.1 . . ? C33 C32 H32 120.1 . . ? N1 C33 C32 122.0(10) . . ? N1 C33 H33 119.0 . . ? C32 C33 H33 119.0 . . ? C35 C34 C31 113.8(10) . . ? C35 C34 H34A 108.8 . . ? C31 C34 H34A 108.8 . . ? C35 C34 H34B 108.8 . . ? C31 C34 H34B 108.8 . . ? H34A C34 H34B 107.7 . . ? C34 C35 C36 111.3(10) . . ? C34 C35 H35A 109.4 . . ? C36 C35 H35A 109.4 . . ? C34 C35 H35B 109.4 . . ? C36 C35 H35B 109.4 . . ? H35A C35 H35B 108.0 . . ? C40 C36 C37 117.5(9) . . ? C40 C36 C35 120.6(12) . . ? C37 C36 C35 121.8(12) . . ? C38 C37 C36 120.4(11) . . ? C38 C37 H37 119.8 . . ? C36 C37 H37 119.8 . . ? N2 C38 C37 122.4(10) . . ? N2 C38 H38 118.8 . . ? C37 C38 H38 118.8 . . ? N2 C39 C40 122.4(11) . . ? N2 C39 H39 118.8 . . ? C40 C39 H39 118.8 . . ? C36 C40 C39 119.2(10) . . ? C36 C40 H40 120.4 . . ? C39 C40 H40 120.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O7 Zn2 N2 C38 138.9(8) 2_564 . . . ? O2 Zn2 N2 C38 35.2(9) . . . . ? O4 Zn2 N2 C38 -123.4(8) 2_564 . . . ? O3 Zn2 N2 C38 -63.2(8) 2_564 . . . ? O5 Zn2 N2 C38 -32(3) . . . . ? C14 Zn2 N2 C38 -94.0(9) 2_564 . . . ? O7 Zn2 N2 C39 -49.3(8) 2_564 . . . ? O2 Zn2 N2 C39 -152.9(8) . . . . ? O4 Zn2 N2 C39 48.4(8) 2_564 . . . ? O3 Zn2 N2 C39 108.7(8) 2_564 . . . ? O5 Zn2 N2 C39 140.1(18) . . . . ? C14 Zn2 N2 C39 77.9(8) 2_564 . . . ? O8 Zn1 O1 C1 -76.6(8) 2_564 . . . ? O5 Zn1 O1 C1 49.7(8) . . . . ? N1 Zn1 O1 C1 170.9(7) 1_656 . . . ? O7 Zn2 O2 C1 46.4(11) 2_564 . . . ? O4 Zn2 O2 C1 -120.0(11) 2_564 . . . ? N2 Zn2 O2 C1 140.5(11) . . . . ? O3 Zn2 O2 C1 -130.1(11) 2_564 . . . ? O5 Zn2 O2 C1 -46.7(11) . . . . ? C14 Zn2 O2 C1 -127.6(10) 2_564 . . . ? O8 Zn1 O5 C15 -67.4(7) 2_564 . . . ? O1 Zn1 O5 C15 174.0(6) . . . . ? N1 Zn1 O5 C15 57.9(7) 1_656 . . . ? O8 Zn1 O5 Zn2 51.4(4) 2_564 . . . ? O1 Zn1 O5 Zn2 -67.2(3) . . . . ? N1 Zn1 O5 Zn2 176.7(3) 1_656 . . . ? O7 Zn2 O5 C15 65.7(8) 2_564 . . . ? O2 Zn2 O5 C15 169.1(8) . . . . ? O4 Zn2 O5 C15 -31.6(8) 2_564 . . . ? N2 Zn2 O5 C15 -124(2) . . . . ? O3 Zn2 O5 C15 -92.1(8) 2_564 . . . ? C14 Zn2 O5 C15 -61.1(8) 2_564 . . . ? O7 Zn2 O5 Zn1 -46.9(3) 2_564 . . . ? O2 Zn2 O5 Zn1 56.5(3) . . . . ? O4 Zn2 O5 Zn1 -144.2(3) 2_564 . . . ? N2 Zn2 O5 Zn1 124(2) . . . . ? O3 Zn2 O5 Zn1 155.3(3) 2_564 . . . ? C14 Zn2 O5 Zn1 -173.7(3) 2_564 . . . ? Zn2 O2 C1 O1 20.8(17) . . . . ? Zn2 O2 C1 C2 -161.7(8) . . . . ? Zn1 O1 C1 O2 -13.2(13) . . . . ? Zn1 O1 C1 C2 169.3(6) . . . . ? O2 C1 C2 C3 -103.8(10) . . . . ? O1 C1 C2 C3 73.7(11) . . . . ? C1 C2 C3 C12 67.0(10) . . . . ? C1 C2 C3 C8 -55.3(11) . . . . ? C1 C2 C3 C4 -175.7(7) . . . . ? C2 C3 C4 C5 -178.2(7) . . . . ? C12 C3 C4 C5 -58.1(9) . . . . ? C8 C3 C4 C5 57.2(10) . . . . ? C3 C4 C5 C11 60.0(9) . . . . ? C3 C4 C5 C6 -60.0(10) . . . . ? C4 C5 C6 C7 63.3(10) . . . . ? C11 C5 C6 C7 -55.6(11) . . . . ? C5 C6 C7 C9 57.1(11) . . . . ? C5 C6 C7 C8 -62.5(10) . . . . ? C5 C6 C7 C13 179.0(8) . . . . ? C2 C3 C8 C7 -175.8(7) . . . . ? C12 C3 C8 C7 59.6(10) . . . . ? C4 C3 C8 C7 -55.6(10) . . . . ? C6 C7 C8 C3 59.6(9) . . . . ? C9 C7 C8 C3 -61.0(9) . . . . ? C13 C7 C8 C3 178.3(7) . . . . ? C6 C7 C9 C10 -59.1(10) . . . . ? C8 C7 C9 C10 60.3(9) . . . . ? C13 C7 C9 C10 179.9(8) . . . . ? C7 C9 C10 C11 59.6(11) . . . . ? C7 C9 C10 C12 -60.5(10) . . . . ? C9 C10 C11 C5 -59.2(11) . . . . ? C12 C10 C11 C5 60.4(10) . . . . ? C4 C5 C11 C10 -61.2(11) . . . . ? C6 C5 C11 C10 57.3(11) . . . . ? C2 C3 C12 C10 173.6(7) . . . . ? C8 C3 C12 C10 -59.9(10) . . . . ? C4 C3 C12 C10 55.9(9) . . . . ? C11 C10 C12 C3 -58.7(9) . . . . ? C9 C10 C12 C3 61.0(10) . . . . ? C6 C7 C13 C14 -168.0(9) . . . . ? C9 C7 C13 C14 -46.1(11) . . . . ? C8 C7 C13 C14 73.7(10) . . . . ? Zn2 O4 C14 O3 -0.8(8) 2_565 . . . ? Zn2 O4 C14 C13 177.0(7) 2_565 . . . ? Zn2 O3 C14 O4 0.8(7) 2_565 . . . ? Zn2 O3 C14 C13 -177.1(6) 2_565 . . . ? C7 C13 C14 O4 -84.6(11) . . . . ? C7 C13 C14 O3 93.2(10) . . . . ? C7 C13 C14 Zn2 20(17) . . . 2_565 ? Zn1 O5 C15 O6 18.5(10) . . . . ? Zn2 O5 C15 O6 -83.8(9) . . . . ? Zn1 O5 C15 C16 -157.5(6) . . . . ? Zn2 O5 C15 C16 100.2(8) . . . . ? O6 C15 C16 C17 -56.2(12) . . . . ? O5 C15 C16 C17 119.8(9) . . . . ? C15 C16 C17 C23 -42.7(12) . . . . ? C15 C16 C17 C22 79.0(11) . . . . ? C15 C16 C17 C18 -160.1(9) . . . . ? C23 C17 C18 C19 60.7(11) . . . . ? C22 C17 C18 C19 -57.1(11) . . . . ? C16 C17 C18 C19 -179.4(9) . . . . ? C17 C18 C19 C26 -62.9(12) . . . . ? C17 C18 C19 C20 56.7(11) . . . . ? C18 C19 C20 C21 -59.1(11) . . . . ? C26 C19 C20 C21 58.9(11) . . . . ? C19 C20 C21 C22 61.6(11) . . . . ? C19 C20 C21 C25 -61.2(11) . . . . ? C20 C21 C22 C17 -61.9(11) . . . . ? C25 C21 C22 C17 60.9(11) . . . . ? C23 C17 C22 C21 -58.4(10) . . . . ? C16 C17 C22 C21 179.2(8) . . . . ? C18 C17 C22 C21 57.9(10) . . . . ? C22 C17 C23 C24 58.7(10) . . . . ? C16 C17 C23 C24 -178.3(8) . . . . ? C18 C17 C23 C24 -59.0(10) . . . . ? C17 C23 C24 C27 -174.5(8) . . . . ? C17 C23 C24 C26 59.5(10) . . . . ? C17 C23 C24 C25 -58.1(10) . . . . ? C20 C21 C25 C24 62.3(10) . . . . ? C22 C21 C25 C24 -61.2(11) . . . . ? C27 C24 C25 C21 178.2(8) . . . . ? C23 C24 C25 C21 58.3(9) . . . . ? C26 C24 C25 C21 -59.3(10) . . . . ? C27 C24 C26 C19 175.2(8) . . . . ? C23 C24 C26 C19 -59.7(10) . . . . ? C25 C24 C26 C19 57.2(10) . . . . ? C18 C19 C26 C24 62.0(11) . . . . ? C20 C19 C26 C24 -56.9(11) . . . . ? C23 C24 C27 C28 -78.6(11) . . . . ? C26 C24 C27 C28 44.9(11) . . . . ? C25 C24 C27 C28 164.2(8) . . . . ? Zn2 O7 C28 O8 -4.7(16) 2_565 . . . ? Zn2 O7 C28 C27 173.7(6) 2_565 . . . ? Zn1 O8 C28 O7 16.9(13) 2_565 . . . ? Zn1 O8 C28 C27 -161.5(6) 2_565 . . . ? C24 C27 C28 O7 62.0(12) . . . . ? C24 C27 C28 O8 -119.5(9) . . . . ? C33 N1 C29 C30 1.2(14) . . . . ? Zn1 N1 C29 C30 -177.2(7) 1_454 . . . ? N1 C29 C30 C31 0.3(15) . . . . ? C29 C30 C31 C32 -1.0(15) . . . . ? C29 C30 C31 C34 175.1(10) . . . . ? C30 C31 C32 C33 0.4(16) . . . . ? C34 C31 C32 C33 -175.7(11) . . . . ? C29 N1 C33 C32 -1.9(15) . . . . ? Zn1 N1 C33 C32 176.5(8) 1_454 . . . ? C31 C32 C33 N1 1.1(17) . . . . ? C32 C31 C34 C35 -72.6(17) . . . . ? C30 C31 C34 C35 111.5(13) . . . . ? C31 C34 C35 C36 176.6(13) . . . . ? C34 C35 C36 C40 -105.5(15) . . . . ? C34 C35 C36 C37 72.8(16) . . . . ? C40 C36 C37 C38 -0.5(17) . . . . ? C35 C36 C37 C38 -178.8(11) . . . . ? C39 N2 C38 C37 0.8(16) . . . . ? Zn2 N2 C38 C37 172.9(8) . . . . ? C36 C37 C38 N2 0.2(17) . . . . ? C38 N2 C39 C40 -1.6(16) . . . . ? Zn2 N2 C39 C40 -173.7(8) . . . . ? C37 C36 C40 C39 -0.3(16) . . . . ? C35 C36 C40 C39 178.0(10) . . . . ? N2 C39 C40 C36 1.4(16) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.09 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.775 _refine_diff_density_min -0.890 _refine_diff_density_rms 0.102 data_4 _database_code_depnum_ccdc_archive 'CCDC 761114' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H48 N2 O8 Zn2' _chemical_formula_sum 'C40 H48 N2 O8 Zn2' _chemical_formula_weight 815.54 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' 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' N N 0.0061 0.0033 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.751(7) _cell_length_b 12.311(7) _cell_length_c 14.001(14) _cell_angle_alpha 103.871(14) _cell_angle_beta 104.149(15) _cell_angle_gamma 103.195(10) _cell_volume 1816(2) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 544 _cell_measurement_theta_min 2.162 _cell_measurement_theta_max 16.056 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.491 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 852 _exptl_absorpt_coefficient_mu 1.378 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8097 _exptl_absorpt_correction_T_max 0.8305 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9134 _diffrn_reflns_av_R_equivalents 0.0729 _diffrn_reflns_av_sigmaI/netI 0.2967 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 25.10 _reflns_number_total 6299 _reflns_number_gt 2241 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0303P)^2^+0.2542P] 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 SHELXL _refine_ls_extinction_coef 0.0027(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6299 _refine_ls_number_parameters 470 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1850 _refine_ls_R_factor_gt 0.0810 _refine_ls_wR_factor_ref 0.1506 _refine_ls_wR_factor_gt 0.1290 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.010 _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 N1 N 0.2282(6) 1.5780(6) 0.9459(5) 0.029(2) Uani 1 1 d . . . C34 C 0.3255(7) 1.5508(9) 0.9331(7) 0.037(3) Uani 1 1 d . . . H34 H 0.4022 1.5962 0.9805 0.045 Uiso 1 1 calc R . . C30 C 0.1249(9) 1.5140(8) 0.8772(7) 0.046(3) Uani 1 1 d 0 . . H30 H 0.0558 1.5337 0.8868 0.056 Uiso 1 1 calc R . . C33 C 0.3199(9) 1.4547(9) 0.8497(7) 0.048(3) Uani 1 1 d . . . H33 H 0.3915 1.4379 0.8433 0.058 Uiso 1 1 calc R . . C31 C 0.1038(8) 1.4248(8) 0.7955(7) 0.042(2) Uani 1 1 d 0 . . H31 H 0.0247 1.3865 0.7493 0.050 Uiso 1 1 calc R . . C32 C 0.2083(9) 1.3880(8) 0.7797(7) 0.036(2) Uani 1 1 d 0 . . C35 C 0.1911(9) 1.2857(9) 0.6924(8) 0.067(4) Uani 1 1 d . . . H35A H 0.1038 1.2517 0.6544 0.081 Uiso 1 1 calc R . . H35B H 0.2183 1.2272 0.7195 0.081 Uiso 1 1 calc R . . C36 C 0.2585(9) 1.3119(8) 0.6187(8) 0.054(3) Uani 1 1 d . . . H36A H 0.3433 1.3580 0.6582 0.065 Uiso 1 1 calc R . . H36B H 0.2215 1.3595 0.5824 0.065 Uiso 1 1 calc R . . O7 O 0.6597(6) 1.2212(5) 0.5847(5) 0.049(2) Uani 1 1 d . . . O8 O 0.8575(6) 1.2600(6) 0.6117(5) 0.053(2) Uani 1 1 d . . . C28 C 0.7565(10) 1.2652(8) 0.5641(7) 0.040(3) Uani 1 1 d . . . C27 C 0.7441(8) 1.3192(8) 0.4770(7) 0.056(4) Uani 1 1 d . . . H27A H 0.8093 1.3932 0.4996 0.067 Uiso 1 1 calc R . . H27B H 0.6660 1.3360 0.4625 0.067 Uiso 1 1 calc R . . Zn1 Zn 0.24269(9) 0.71167(10) 0.07075(8) 0.0392(4) Uani 1 1 d . . . Zn2 Zn 0.26086(9) 0.83923(10) 0.30284(8) 0.0418(4) Uani 1 1 d . . . O2 O 0.4143(6) 0.6232(6) 0.1899(5) 0.057(2) Uani 1 1 d . . . O1 O 0.2318(5) 0.6475(5) 0.1839(4) 0.0402(18) Uani 1 1 d . . . O3 O -0.0922(5) 0.2486(6) -0.0298(5) 0.045(2) Uani 1 1 d . . . O4 O -0.1106(5) 0.1613(6) -0.1975(5) 0.052(2) Uani 1 1 d . . . O5 O 0.3955(5) 0.8349(6) 0.1041(5) 0.050(2) Uani 1 1 d . . . O6 O 0.4154(5) 0.9038(6) 0.2732(5) 0.0434(19) Uani 1 1 d . . . N2 N 0.2615(6) 1.0008(7) 0.4003(5) 0.030(2) Uani 1 1 d . . . C18 C 0.6682(8) 1.1156(8) 0.3504(6) 0.037(3) Uani 1 1 d . . . H18A H 0.5842 1.1167 0.3429 0.044 Uiso 1 1 calc R . . H18B H 0.6943 1.0849 0.4070 0.044 Uiso 1 1 calc R . . C1 C 0.3166(9) 0.6025(9) 0.2132(7) 0.044(3) Uani 1 1 d . . . C39 C 0.3612(9) 1.0830(8) 0.4572(7) 0.039(3) Uani 1 1 d . . . H39 H 0.4348 1.0728 0.4494 0.047 Uiso 1 1 calc R . . C14 C -0.0528(9) 0.2012(9) -0.0983(9) 0.048(3) Uani 1 1 d . . . C11 C 0.1134(7) 0.1413(7) 0.0979(6) 0.045(3) Uani 1 1 d . . . H11A H 0.0341 0.1483 0.1024 0.053 Uiso 1 1 calc R . . H11B H 0.1020 0.0600 0.0616 0.053 Uiso 1 1 calc R . . C13 C 0.0751(6) 0.1841(8) -0.0754(6) 0.035(2) Uani 1 1 d . . . H13A H 0.1192 0.2260 -0.1123 0.041 Uiso 1 1 calc R . . H13B H 0.0632 0.1013 -0.1064 0.041 Uiso 1 1 calc R . . C19 C 0.7505(8) 1.2389(9) 0.3759(8) 0.043(3) Uani 1 1 d . . . C12 C 0.1807(7) 0.3497(7) 0.0988(6) 0.035(2) Uani 1 1 d . . . H12A H 0.2083 0.4011 0.0609 0.042 Uiso 1 1 calc R . . H12B H 0.1029 0.3580 0.1062 0.042 Uiso 1 1 calc R . . C26 C 0.7070(8) 1.2896(8) 0.2890(7) 0.042(3) Uani 1 1 d . . . H26A H 0.6235 1.2921 0.2819 0.051 Uiso 1 1 calc R . . H26B H 0.7599 1.3690 0.3054 0.051 Uiso 1 1 calc R . . C23 C 0.6292(7) 1.0831(8) 0.1602(7) 0.044(3) Uani 1 1 d . . . H23A H 0.5439 1.0810 0.1498 0.052 Uiso 1 1 calc R . . H23B H 0.6346 1.0354 0.0964 0.052 Uiso 1 1 calc R . . C4 C 0.2227(7) 0.3035(8) 0.2654(6) 0.038(3) Uani 1 1 d . . . H4A H 0.2796 0.3251 0.3348 0.046 Uiso 1 1 calc R . . H4B H 0.1447 0.3130 0.2711 0.046 Uiso 1 1 calc R . . C17 C 0.6724(8) 1.0340(8) 0.2484(7) 0.030(2) Uani 1 1 d . . . C10 C 0.1615(8) 0.2204(8) 0.0368(7) 0.030(2) Uani 1 1 d . . . C3 C 0.2754(8) 0.3860(8) 0.2058(7) 0.032(2) Uani 1 1 d . . . C7 C 0.3768(7) 0.2386(8) 0.1386(7) 0.038(3) Uani 1 1 d . . . H7 H 0.4555 0.2290 0.1325 0.045 Uiso 1 1 calc R . . C40 C 0.1557(8) 1.0165(9) 0.4105(7) 0.042(3) Uani 1 1 d . . . H40 H 0.0818 0.9587 0.3702 0.050 Uiso 1 1 calc R . . C6 C 0.3271(7) 0.1584(8) 0.1973(7) 0.038(3) Uani 1 1 d . . . H6A H 0.3861 0.1777 0.2655 0.046 Uiso 1 1 calc R . . H6B H 0.3138 0.0770 0.1597 0.046 Uiso 1 1 calc R . . C2 C 0.2914(8) 0.5134(8) 0.2707(6) 0.038(3) Uani 1 1 d . . . H2A H 0.2172 0.5149 0.2891 0.046 Uiso 1 1 calc R . . H2B H 0.3591 0.5363 0.3346 0.046 Uiso 1 1 calc R . . C20 C 0.8827(8) 1.2401(8) 0.3858(7) 0.042(3) Uani 1 1 d . . . H20A H 0.9142 1.2125 0.4432 0.051 Uiso 1 1 calc R . . H20B H 0.9337 1.3200 0.4007 0.051 Uiso 1 1 calc R . . C15 C 0.4601(9) 0.8811(9) 0.2004(9) 0.049(3) Uani 1 1 d . . . C16 C 0.5988(7) 0.9050(8) 0.2232(6) 0.040(3) Uani 1 1 d . . . H16A H 0.6135 0.8587 0.1635 0.047 Uiso 1 1 calc R . . H16B H 0.6298 0.8783 0.2813 0.047 Uiso 1 1 calc R . . C41 C 0.1538(9) 1.1156(10) 0.4786(7) 0.053(3) Uani 1 1 d . . . H41 H 0.0782 1.1229 0.4834 0.063 Uiso 1 1 calc R . . C38 C 0.3685(9) 1.1850(10) 0.5287(8) 0.062(4) Uani 1 1 d . . . H38 H 0.4445 1.2398 0.5687 0.074 Uiso 1 1 calc R . . C5 C 0.2044(8) 0.1766(8) 0.2076(7) 0.038(3) Uani 1 1 d . . . H5 H 0.1716 0.1260 0.2452 0.046 Uiso 1 1 calc R . . C8 C 0.3968(7) 0.3685(8) 0.1987(7) 0.039(3) Uani 1 1 d . . . H8A H 0.4541 0.3893 0.2679 0.047 Uiso 1 1 calc R . . H8B H 0.4320 0.4195 0.1633 0.047 Uiso 1 1 calc R . . C9 C 0.2849(7) 0.2062(8) 0.0301(6) 0.035(2) Uani 1 1 d . . . H9A H 0.3175 0.2564 -0.0069 0.043 Uiso 1 1 calc R . . H9B H 0.2733 0.1255 -0.0083 0.043 Uiso 1 1 calc R . . C21 C 0.8911(8) 1.1616(9) 0.2857(8) 0.052(3) Uani 1 1 d . . . H21 H 0.9763 1.1615 0.2937 0.062 Uiso 1 1 calc R . . C25 C 0.8442(8) 1.2114(9) 0.1971(7) 0.055(3) Uani 1 1 d . . . H25A H 0.8967 1.2907 0.2120 0.066 Uiso 1 1 calc R . . H25B H 0.8467 1.1632 0.1322 0.066 Uiso 1 1 calc R . . C24 C 0.7115(8) 1.2121(8) 0.1878(7) 0.041(3) Uani 1 1 d . . . H24 H 0.6819 1.2435 0.1317 0.049 Uiso 1 1 calc R . . C22 C 0.8069(7) 1.0374(8) 0.2607(7) 0.042(3) Uani 1 1 d . . . H22A H 0.8360 1.0057 0.3159 0.050 Uiso 1 1 calc R . . H22B H 0.8109 0.9879 0.1970 0.050 Uiso 1 1 calc R . . C37 C 0.2582(11) 1.2043(9) 0.5399(7) 0.044(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.023(4) 0.036(6) 0.027(5) 0.004(4) 0.019(4) 0.001(4) C34 0.013(5) 0.056(8) 0.044(7) 0.024(6) 0.006(5) 0.006(5) C30 0.050(6) 0.025(6) 0.039(6) -0.008(4) -0.006(5) 0.003(5) C33 0.070(8) 0.043(8) 0.028(7) -0.008(5) 0.025(6) 0.018(6) C31 0.038(5) 0.031(5) 0.037(5) 0.002(4) -0.007(4) 0.003(4) C32 0.050(6) 0.025(6) 0.024(5) -0.003(4) 0.015(5) -0.001(5) C35 0.079(8) 0.044(8) 0.045(8) 0.008(7) -0.005(7) -0.012(7) C36 0.085(8) 0.029(8) 0.049(8) -0.002(6) 0.035(6) 0.021(6) O7 0.050(4) 0.038(5) 0.045(5) 0.011(4) 0.007(4) -0.001(4) O8 0.055(4) 0.052(5) 0.036(5) 0.005(4) 0.005(4) 0.009(4) C28 0.060(8) 0.017(6) 0.023(6) -0.001(5) -0.008(6) 0.005(6) C27 0.056(7) 0.037(8) 0.045(8) 0.023(7) -0.016(6) -0.018(6) Zn1 0.0395(7) 0.0400(9) 0.0285(8) 0.0057(6) 0.0044(6) 0.0064(6) Zn2 0.0371(7) 0.0511(10) 0.0302(8) 0.0106(7) 0.0039(6) 0.0100(6) O2 0.054(5) 0.050(5) 0.053(5) 0.014(4) 0.014(4) -0.003(4) O1 0.034(4) 0.051(5) 0.037(4) 0.022(4) 0.007(3) 0.014(3) O3 0.038(4) 0.051(5) 0.033(5) 0.001(4) -0.002(3) 0.012(4) O4 0.049(4) 0.062(5) 0.038(5) 0.015(4) -0.004(4) 0.023(4) O5 0.036(4) 0.063(5) 0.032(4) 0.015(4) 0.000(3) -0.009(4) O6 0.038(4) 0.054(5) 0.046(5) 0.016(4) 0.023(3) 0.018(3) N2 0.021(4) 0.047(6) 0.018(5) 0.001(4) 0.011(3) 0.007(4) C18 0.044(6) 0.035(7) 0.026(6) 0.005(5) 0.013(5) 0.003(5) C1 0.046(7) 0.026(7) 0.030(7) 0.001(5) -0.019(6) -0.002(6) C39 0.043(7) 0.033(7) 0.021(6) -0.004(5) 0.005(5) -0.005(6) C14 0.051(7) 0.036(8) 0.043(8) 0.024(7) -0.003(6) -0.004(6) C11 0.043(6) 0.037(7) 0.036(6) 0.014(5) -0.005(5) -0.006(5) C13 0.023(5) 0.038(7) 0.038(6) 0.000(5) 0.010(4) 0.013(5) C19 0.032(6) 0.043(8) 0.047(7) 0.022(6) -0.001(5) 0.004(6) C12 0.035(5) 0.032(7) 0.036(6) 0.006(5) 0.010(5) 0.011(5) C26 0.038(6) 0.035(7) 0.042(7) 0.014(6) 0.004(5) -0.004(5) C23 0.034(6) 0.054(8) 0.036(6) 0.017(6) 0.004(5) 0.004(5) C4 0.022(5) 0.064(8) 0.036(6) 0.029(6) 0.011(4) 0.014(5) C17 0.040(6) 0.026(7) 0.031(6) 0.016(5) 0.020(5) 0.011(5) C10 0.036(6) 0.024(6) 0.028(6) 0.006(5) 0.010(5) 0.009(5) C3 0.037(6) 0.016(6) 0.031(6) 0.002(5) 0.001(5) 0.002(5) C7 0.025(5) 0.044(7) 0.042(7) 0.012(6) 0.009(5) 0.010(5) C40 0.021(6) 0.050(9) 0.039(7) 0.012(6) -0.003(5) -0.001(5) C6 0.023(5) 0.040(7) 0.048(7) 0.011(6) -0.002(5) 0.020(5) C2 0.050(6) 0.039(7) 0.034(6) 0.009(5) 0.020(5) 0.025(5) C20 0.038(6) 0.032(7) 0.046(7) 0.012(6) 0.000(5) 0.005(5) C15 0.055(7) 0.033(7) 0.050(8) 0.028(7) 0.004(6) -0.003(6) C16 0.028(5) 0.061(8) 0.034(6) 0.012(6) 0.019(5) 0.015(5) C41 0.058(8) 0.052(9) 0.033(7) 0.004(6) 0.006(6) 0.006(7) C38 0.035(7) 0.060(10) 0.061(9) 0.025(7) -0.002(6) -0.027(7) C5 0.048(6) 0.031(7) 0.044(7) 0.021(6) 0.012(5) 0.019(5) C8 0.028(5) 0.044(8) 0.039(7) 0.009(6) 0.002(5) 0.012(5) C9 0.033(5) 0.033(7) 0.034(6) 0.002(5) 0.003(5) 0.015(5) C21 0.031(6) 0.072(9) 0.055(8) 0.030(7) 0.013(5) 0.012(6) C25 0.039(6) 0.073(9) 0.063(8) 0.028(7) 0.034(6) 0.011(6) C24 0.057(7) 0.041(8) 0.038(7) 0.027(6) 0.018(5) 0.020(6) C22 0.038(6) 0.041(7) 0.039(7) 0.014(5) 0.002(5) 0.008(5) C37 0.072(8) 0.027(7) 0.028(7) 0.005(5) 0.017(6) 0.007(7) _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 N1 C30 1.284(9) . ? N1 C34 1.303(10) . ? N1 Zn1 2.035(7) 1_566 ? C34 C33 1.425(12) . ? C34 H34 0.9300 . ? C30 C31 1.307(12) . ? C30 H30 0.9300 . ? C33 C32 1.360(11) . ? C33 H33 0.9300 . ? C31 C32 1.449(12) . ? C31 H31 0.9300 . ? C32 C35 1.465(13) . ? C35 C36 1.497(11) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 C37 1.505(12) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? O7 C28 1.274(10) . ? O7 Zn2 2.016(6) 2_676 ? O8 C28 1.234(9) . ? O8 Zn2 2.366(6) 2_676 ? C28 C27 1.516(11) . ? C28 Zn2 2.525(10) 2_676 ? C27 C19 1.550(13) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? Zn1 O3 1.931(6) 2_565 ? Zn1 O5 1.936(5) . ? Zn1 O1 1.950(6) . ? Zn1 N1 2.035(7) 1_544 ? Zn2 O6 1.992(6) . ? Zn2 O4 2.003(6) 2_565 ? Zn2 O7 2.016(6) 2_676 ? Zn2 N2 2.123(8) . ? Zn2 O8 2.366(6) 2_676 ? Zn2 O1 2.436(7) . ? Zn2 C28 2.525(10) 2_676 ? O2 C1 1.257(11) . ? O1 C1 1.275(10) . ? O3 C14 1.244(12) . ? O3 Zn1 1.931(6) 2_565 ? O4 C14 1.300(10) . ? O4 Zn2 2.003(6) 2_565 ? O5 C15 1.286(10) . ? O6 C15 1.260(11) . ? N2 C39 1.284(9) . ? N2 C40 1.336(10) . ? C18 C19 1.506(11) . ? C18 C17 1.557(11) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C1 C2 1.527(11) . ? C39 C38 1.375(14) . ? C39 H39 0.9300 . ? C14 C13 1.533(12) . ? C11 C5 1.534(10) . ? C11 C10 1.544(10) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C13 C10 1.540(10) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C19 C20 1.522(11) . ? C19 C26 1.529(11) . ? C12 C3 1.523(10) . ? C12 C10 1.554(11) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C26 C24 1.527(12) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C23 C17 1.529(10) . ? C23 C24 1.558(11) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C4 C5 1.516(11) . ? C4 C3 1.575(10) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C17 C16 1.533(11) . ? C17 C22 1.538(10) . ? C10 C9 1.521(10) . ? C3 C8 1.513(11) . ? C3 C2 1.555(11) . ? C7 C9 1.532(10) . ? C7 C6 1.532(10) . ? C7 C8 1.552(11) . ? C7 H7 0.9800 . ? C40 C41 1.364(13) . ? C40 H40 0.9300 . ? C6 C5 1.545(11) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C20 C21 1.539(12) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C15 C16 1.525(11) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C41 C37 1.364(12) . ? C41 H41 0.9300 . ? C38 C37 1.409(13) . ? C38 H38 0.9300 . ? C5 H5 0.9800 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C21 C22 1.525(11) . ? C21 C25 1.550(11) . ? C21 H21 0.9800 . ? C25 C24 1.535(11) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C24 H24 0.9800 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? 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 C30 N1 C34 116.0(9) . . ? C30 N1 Zn1 123.2(7) . 1_566 ? C34 N1 Zn1 120.8(7) . 1_566 ? N1 C34 C33 123.1(9) . . ? N1 C34 H34 118.5 . . ? C33 C34 H34 118.5 . . ? N1 C30 C31 128.7(11) . . ? N1 C30 H30 115.6 . . ? C31 C30 H30 115.6 . . ? C32 C33 C34 118.9(10) . . ? C32 C33 H33 120.5 . . ? C34 C33 H33 120.5 . . ? C30 C31 C32 117.5(9) . . ? C30 C31 H31 121.2 . . ? C32 C31 H31 121.2 . . ? C33 C32 C31 115.7(9) . . ? C33 C32 C35 123.7(10) . . ? C31 C32 C35 120.6(9) . . ? C32 C35 C36 114.4(8) . . ? C32 C35 H35A 108.7 . . ? C36 C35 H35A 108.7 . . ? C32 C35 H35B 108.7 . . ? C36 C35 H35B 108.7 . . ? H35A C35 H35B 107.6 . . ? C35 C36 C37 114.0(9) . . ? C35 C36 H36A 108.7 . . ? C37 C36 H36A 108.7 . . ? C35 C36 H36B 108.7 . . ? C37 C36 H36B 108.7 . . ? H36A C36 H36B 107.6 . . ? C28 O7 Zn2 97.7(6) . 2_676 ? C28 O8 Zn2 82.7(6) . 2_676 ? O8 C28 O7 120.6(9) . . ? O8 C28 C27 120.8(10) . . ? O7 C28 C27 118.6(9) . . ? O8 C28 Zn2 68.3(5) . 2_676 ? O7 C28 Zn2 52.3(4) . 2_676 ? C27 C28 Zn2 170.6(7) . 2_676 ? C28 C27 C19 113.1(9) . . ? C28 C27 H27A 109.0 . . ? C19 C27 H27A 109.0 . . ? C28 C27 H27B 109.0 . . ? C19 C27 H27B 109.0 . . ? H27A C27 H27B 107.8 . . ? O3 Zn1 O5 116.7(3) 2_565 . ? O3 Zn1 O1 105.4(3) 2_565 . ? O5 Zn1 O1 113.2(2) . . ? O3 Zn1 N1 103.9(3) 2_565 1_544 ? O5 Zn1 N1 108.9(3) . 1_544 ? O1 Zn1 N1 107.9(3) . 1_544 ? O6 Zn2 O4 112.4(2) . 2_565 ? O6 Zn2 O7 95.6(3) . 2_676 ? O4 Zn2 O7 150.3(2) 2_565 2_676 ? O6 Zn2 N2 96.3(3) . . ? O4 Zn2 N2 89.2(3) 2_565 . ? O7 Zn2 N2 97.6(3) 2_676 . ? O6 Zn2 O8 154.6(2) . 2_676 ? O4 Zn2 O8 92.5(2) 2_565 2_676 ? O7 Zn2 O8 59.0(2) 2_676 2_676 ? N2 Zn2 O8 88.7(2) . 2_676 ? O6 Zn2 O1 89.7(2) . . ? O4 Zn2 O1 84.8(2) 2_565 . ? O7 Zn2 O1 85.7(2) 2_676 . ? N2 Zn2 O1 172.7(2) . . ? O8 Zn2 O1 87.6(2) 2_676 . ? O6 Zn2 C28 125.6(3) . 2_676 ? O4 Zn2 C28 121.2(3) 2_565 2_676 ? O7 Zn2 C28 30.0(3) 2_676 2_676 ? N2 Zn2 C28 93.5(3) . 2_676 ? O8 Zn2 C28 29.0(2) 2_676 2_676 ? O1 Zn2 C28 86.2(3) . 2_676 ? C1 O1 Zn1 114.7(6) . . ? C1 O1 Zn2 113.3(6) . . ? Zn1 O1 Zn2 92.4(2) . . ? C14 O3 Zn1 118.8(7) . 2_565 ? C14 O4 Zn2 141.3(7) . 2_565 ? C15 O5 Zn1 116.9(6) . . ? C15 O6 Zn2 137.4(6) . . ? C39 N2 C40 117.1(9) . . ? C39 N2 Zn2 122.7(7) . . ? C40 N2 Zn2 120.0(7) . . ? C19 C18 C17 111.1(7) . . ? C19 C18 H18A 109.4 . . ? C17 C18 H18A 109.4 . . ? C19 C18 H18B 109.4 . . ? C17 C18 H18B 109.4 . . ? H18A C18 H18B 108.0 . . ? O2 C1 O1 122.1(9) . . ? O2 C1 C2 120.1(9) . . ? O1 C1 C2 117.7(9) . . ? N2 C39 C38 125.6(10) . . ? N2 C39 H39 117.2 . . ? C38 C39 H39 117.2 . . ? O3 C14 O4 126.3(10) . . ? O3 C14 C13 123.3(9) . . ? O4 C14 C13 110.4(10) . . ? C5 C11 C10 110.7(6) . . ? C5 C11 H11A 109.5 . . ? C10 C11 H11A 109.5 . . ? C5 C11 H11B 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 108.1 . . ? C14 C13 C10 121.1(8) . . ? C14 C13 H13A 107.0 . . ? C10 C13 H13A 107.0 . . ? C14 C13 H13B 107.0 . . ? C10 C13 H13B 107.0 . . ? H13A C13 H13B 106.8 . . ? C18 C19 C20 110.8(9) . . ? C18 C19 C26 109.8(7) . . ? C20 C19 C26 107.8(8) . . ? C18 C19 C27 110.4(8) . . ? C20 C19 C27 110.6(8) . . ? C26 C19 C27 107.4(9) . . ? C3 C12 C10 111.1(7) . . ? C3 C12 H12A 109.4 . . ? C10 C12 H12A 109.4 . . ? C3 C12 H12B 109.4 . . ? C10 C12 H12B 109.4 . . ? H12A C12 H12B 108.0 . . ? C24 C26 C19 108.9(9) . . ? C24 C26 H26A 109.9 . . ? C19 C26 H26A 109.9 . . ? C24 C26 H26B 109.9 . . ? C19 C26 H26B 109.9 . . ? H26A C26 H26B 108.3 . . ? C17 C23 C24 109.6(7) . . ? C17 C23 H23A 109.8 . . ? C24 C23 H23A 109.8 . . ? C17 C23 H23B 109.8 . . ? C24 C23 H23B 109.8 . . ? H23A C23 H23B 108.2 . . ? C5 C4 C3 109.9(7) . . ? C5 C4 H4A 109.7 . . ? C3 C4 H4A 109.7 . . ? C5 C4 H4B 109.7 . . ? C3 C4 H4B 109.7 . . ? H4A C4 H4B 108.2 . . ? C23 C17 C16 111.9(7) . . ? C23 C17 C22 107.8(7) . . ? C16 C17 C22 106.6(7) . . ? C23 C17 C18 108.5(8) . . ? C16 C17 C18 113.4(7) . . ? C22 C17 C18 108.4(7) . . ? C9 C10 C13 106.9(7) . . ? C9 C10 C11 108.2(7) . . ? C13 C10 C11 112.2(7) . . ? C9 C10 C12 109.3(7) . . ? C13 C10 C12 112.5(7) . . ? C11 C10 C12 107.7(7) . . ? C8 C3 C12 111.5(8) . . ? C8 C3 C2 112.2(7) . . ? C12 C3 C2 111.8(7) . . ? C8 C3 C4 107.9(7) . . ? C12 C3 C4 107.0(6) . . ? C2 C3 C4 106.1(7) . . ? C9 C7 C6 110.0(7) . . ? C9 C7 C8 109.2(7) . . ? C6 C7 C8 109.7(7) . . ? C9 C7 H7 109.3 . . ? C6 C7 H7 109.3 . . ? C8 C7 H7 109.3 . . ? N2 C40 C41 121.5(9) . . ? N2 C40 H40 119.3 . . ? C41 C40 H40 119.3 . . ? C7 C6 C5 108.3(7) . . ? C7 C6 H6A 110.0 . . ? C5 C6 H6A 110.0 . . ? C7 C6 H6B 110.0 . . ? C5 C6 H6B 110.0 . . ? H6A C6 H6B 108.4 . . ? C1 C2 C3 113.0(7) . . ? C1 C2 H2A 109.0 . . ? C3 C2 H2A 109.0 . . ? C1 C2 H2B 109.0 . . ? C3 C2 H2B 109.0 . . ? H2A C2 H2B 107.8 . . ? C19 C20 C21 111.3(8) . . ? C19 C20 H20A 109.4 . . ? C21 C20 H20A 109.4 . . ? C19 C20 H20B 109.4 . . ? C21 C20 H20B 109.4 . . ? H20A C20 H20B 108.0 . . ? O6 C15 O5 124.1(10) . . ? O6 C15 C16 120.6(9) . . ? O5 C15 C16 115.3(10) . . ? C15 C16 C17 115.0(8) . . ? C15 C16 H16A 108.5 . . ? C17 C16 H16A 108.5 . . ? C15 C16 H16B 108.5 . . ? C17 C16 H16B 108.5 . . ? H16A C16 H16B 107.5 . . ? C37 C41 C40 122.7(11) . . ? C37 C41 H41 118.6 . . ? C40 C41 H41 118.6 . . ? C39 C38 C37 118.4(9) . . ? C39 C38 H38 120.8 . . ? C37 C38 H38 120.8 . . ? C4 C5 C11 110.1(7) . . ? C4 C5 C6 111.0(7) . . ? C11 C5 C6 107.9(8) . . ? C4 C5 H5 109.3 . . ? C11 C5 H5 109.3 . . ? C6 C5 H5 109.3 . . ? C3 C8 C7 110.1(7) . . ? C3 C8 H8A 109.6 . . ? C7 C8 H8A 109.6 . . ? C3 C8 H8B 109.6 . . ? C7 C8 H8B 109.6 . . ? H8A C8 H8B 108.2 . . ? C10 C9 C7 110.7(7) . . ? C10 C9 H9A 109.5 . . ? C7 C9 H9A 109.5 . . ? C10 C9 H9B 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 108.1 . . ? C22 C21 C20 108.9(7) . . ? C22 C21 C25 108.9(7) . . ? C20 C21 C25 107.5(9) . . ? C22 C21 H21 110.5 . . ? C20 C21 H21 110.5 . . ? C25 C21 H21 110.5 . . ? C24 C25 C21 109.1(7) . . ? C24 C25 H25A 109.9 . . ? C21 C25 H25A 109.9 . . ? C24 C25 H25B 109.9 . . ? C21 C25 H25B 109.9 . . ? H25A C25 H25B 108.3 . . ? C26 C24 C25 110.2(8) . . ? C26 C24 C23 111.2(7) . . ? C25 C24 C23 108.4(8) . . ? C26 C24 H24 109.0 . . ? C25 C24 H24 109.0 . . ? C23 C24 H24 109.0 . . ? C21 C22 C17 112.1(8) . . ? C21 C22 H22A 109.2 . . ? C17 C22 H22A 109.2 . . ? C21 C22 H22B 109.2 . . ? C17 C22 H22B 109.2 . . ? H22A C22 H22B 107.9 . . ? C41 C37 C38 114.7(10) . . ? C41 C37 C36 123.5(11) . . ? C38 C37 C36 121.6(11) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C30 N1 C34 C33 -1.3(13) . . . . ? Zn1 N1 C34 C33 177.0(7) 1_566 . . . ? C34 N1 C30 C31 -0.1(15) . . . . ? Zn1 N1 C30 C31 -178.4(8) 1_566 . . . ? N1 C34 C33 C32 0.2(14) . . . . ? N1 C30 C31 C32 2.4(16) . . . . ? C34 C33 C32 C31 2.0(13) . . . . ? C34 C33 C32 C35 -178.6(9) . . . . ? C30 C31 C32 C33 -3.2(13) . . . . ? C30 C31 C32 C35 177.4(9) . . . . ? C33 C32 C35 C36 -59.5(14) . . . . ? C31 C32 C35 C36 119.9(10) . . . . ? C32 C35 C36 C37 170.2(10) . . . . ? Zn2 O8 C28 O7 0.2(9) 2_676 . . . ? Zn2 O8 C28 C27 -177.2(9) 2_676 . . . ? Zn2 O7 C28 O8 -0.2(11) 2_676 . . . ? Zn2 O7 C28 C27 177.2(8) 2_676 . . . ? O8 C28 C27 C19 74.8(11) . . . . ? O7 C28 C27 C19 -102.6(11) . . . . ? Zn2 C28 C27 C19 -89(5) 2_676 . . . ? O3 Zn1 O1 C1 171.8(6) 2_565 . . . ? O5 Zn1 O1 C1 -59.5(7) . . . . ? N1 Zn1 O1 C1 61.2(7) 1_544 . . . ? O3 Zn1 O1 Zn2 -71.2(3) 2_565 . . . ? O5 Zn1 O1 Zn2 57.6(3) . . . . ? N1 Zn1 O1 Zn2 178.2(2) 1_544 . . . ? O6 Zn2 O1 C1 63.9(7) . . . . ? O4 Zn2 O1 C1 176.4(7) 2_565 . . . ? O7 Zn2 O1 C1 -31.7(7) 2_676 . . . ? N2 Zn2 O1 C1 -149.6(16) . . . . ? O8 Zn2 O1 C1 -90.8(7) 2_676 . . . ? C28 Zn2 O1 C1 -61.8(7) 2_676 . . . ? O6 Zn2 O1 Zn1 -54.4(2) . . . . ? O4 Zn2 O1 Zn1 58.2(2) 2_565 . . . ? O7 Zn2 O1 Zn1 -150.0(3) 2_676 . . . ? N2 Zn2 O1 Zn1 92.1(17) . . . . ? O8 Zn2 O1 Zn1 151.0(2) 2_676 . . . ? C28 Zn2 O1 Zn1 180.0(3) 2_676 . . . ? O3 Zn1 O5 C15 107.0(8) 2_565 . . . ? O1 Zn1 O5 C15 -15.7(8) . . . . ? N1 Zn1 O5 C15 -135.7(7) 1_544 . . . ? O4 Zn2 O6 C15 -58.6(10) 2_565 . . . ? O7 Zn2 O6 C15 111.4(10) 2_676 . . . ? N2 Zn2 O6 C15 -150.3(10) . . . . ? O8 Zn2 O6 C15 109.4(10) 2_676 . . . ? O1 Zn2 O6 C15 25.7(10) . . . . ? C28 Zn2 O6 C15 110.8(10) 2_676 . . . ? O6 Zn2 N2 C39 -30.9(7) . . . . ? O4 Zn2 N2 C39 -143.3(7) 2_565 . . . ? O7 Zn2 N2 C39 65.6(7) 2_676 . . . ? O8 Zn2 N2 C39 124.1(7) 2_676 . . . ? O1 Zn2 N2 C39 -177.1(14) . . . . ? C28 Zn2 N2 C39 95.5(7) 2_676 . . . ? O6 Zn2 N2 C40 154.4(6) . . . . ? O4 Zn2 N2 C40 42.0(6) 2_565 . . . ? O7 Zn2 N2 C40 -109.1(6) 2_676 . . . ? O8 Zn2 N2 C40 -50.6(6) 2_676 . . . ? O1 Zn2 N2 C40 8(2) . . . . ? C28 Zn2 N2 C40 -79.2(7) 2_676 . . . ? Zn1 O1 C1 O2 16.6(12) . . . . ? Zn2 O1 C1 O2 -87.7(10) . . . . ? Zn1 O1 C1 C2 -158.3(6) . . . . ? Zn2 O1 C1 C2 97.4(8) . . . . ? C40 N2 C39 C38 1.0(14) . . . . ? Zn2 N2 C39 C38 -173.8(7) . . . . ? Zn1 O3 C14 O4 -9.1(14) 2_565 . . . ? Zn1 O3 C14 C13 169.7(6) 2_565 . . . ? Zn2 O4 C14 O3 9.8(17) 2_565 . . . ? Zn2 O4 C14 C13 -169.1(6) 2_565 . . . ? O3 C14 C13 C10 2.9(14) . . . . ? O4 C14 C13 C10 -178.1(7) . . . . ? C17 C18 C19 C20 -57.8(10) . . . . ? C17 C18 C19 C26 61.2(11) . . . . ? C17 C18 C19 C27 179.3(7) . . . . ? C28 C27 C19 C18 47.3(11) . . . . ? C28 C27 C19 C20 -75.7(10) . . . . ? C28 C27 C19 C26 166.9(7) . . . . ? C18 C19 C26 C24 -59.7(10) . . . . ? C20 C19 C26 C24 61.1(10) . . . . ? C27 C19 C26 C24 -179.7(7) . . . . ? C24 C23 C17 C16 -177.1(7) . . . . ? C24 C23 C17 C22 -60.3(10) . . . . ? C24 C23 C17 C18 56.9(9) . . . . ? C19 C18 C17 C23 -59.8(9) . . . . ? C19 C18 C17 C16 175.2(7) . . . . ? C19 C18 C17 C22 57.0(9) . . . . ? C14 C13 C10 C9 -172.7(8) . . . . ? C14 C13 C10 C11 68.9(11) . . . . ? C14 C13 C10 C12 -52.8(10) . . . . ? C5 C11 C10 C9 59.9(10) . . . . ? C5 C11 C10 C13 177.6(7) . . . . ? C5 C11 C10 C12 -58.1(9) . . . . ? C3 C12 C10 C9 -56.2(9) . . . . ? C3 C12 C10 C13 -174.8(7) . . . . ? C3 C12 C10 C11 61.0(9) . . . . ? C10 C12 C3 C8 56.1(9) . . . . ? C10 C12 C3 C2 -177.5(7) . . . . ? C10 C12 C3 C4 -61.7(9) . . . . ? C5 C4 C3 C8 -59.4(9) . . . . ? C5 C4 C3 C12 60.7(9) . . . . ? C5 C4 C3 C2 -179.8(7) . . . . ? C39 N2 C40 C41 -0.2(13) . . . . ? Zn2 N2 C40 C41 174.8(7) . . . . ? C9 C7 C6 C5 -61.0(10) . . . . ? C8 C7 C6 C5 59.2(9) . . . . ? O2 C1 C2 C3 -65.0(11) . . . . ? O1 C1 C2 C3 110.1(10) . . . . ? C8 C3 C2 C1 74.2(9) . . . . ? C12 C3 C2 C1 -51.9(10) . . . . ? C4 C3 C2 C1 -168.2(7) . . . . ? C18 C19 C20 C21 57.8(10) . . . . ? C26 C19 C20 C21 -62.3(11) . . . . ? C27 C19 C20 C21 -179.4(8) . . . . ? Zn2 O6 C15 O5 30.5(16) . . . . ? Zn2 O6 C15 C16 -147.8(7) . . . . ? Zn1 O5 C15 O6 -39.7(13) . . . . ? Zn1 O5 C15 C16 138.8(6) . . . . ? O6 C15 C16 C17 -77.9(11) . . . . ? O5 C15 C16 C17 103.6(10) . . . . ? C23 C17 C16 C15 -58.4(10) . . . . ? C22 C17 C16 C15 -176.0(7) . . . . ? C18 C17 C16 C15 64.8(10) . . . . ? N2 C40 C41 C37 0.2(15) . . . . ? N2 C39 C38 C37 -1.9(15) . . . . ? C3 C4 C5 C11 -60.0(9) . . . . ? C3 C4 C5 C6 59.5(9) . . . . ? C10 C11 C5 C4 59.3(10) . . . . ? C10 C11 C5 C6 -62.0(10) . . . . ? C7 C6 C5 C4 -59.3(9) . . . . ? C7 C6 C5 C11 61.5(9) . . . . ? C12 C3 C8 C7 -57.0(9) . . . . ? C2 C3 C8 C7 176.8(6) . . . . ? C4 C3 C8 C7 60.3(9) . . . . ? C9 C7 C8 C3 58.5(9) . . . . ? C6 C7 C8 C3 -62.1(9) . . . . ? C13 C10 C9 C7 -179.1(7) . . . . ? C11 C10 C9 C7 -58.1(9) . . . . ? C12 C10 C9 C7 58.9(9) . . . . ? C6 C7 C9 C10 60.1(10) . . . . ? C8 C7 C9 C10 -60.3(9) . . . . ? C19 C20 C21 C22 -56.9(10) . . . . ? C19 C20 C21 C25 60.9(9) . . . . ? C22 C21 C25 C24 59.3(11) . . . . ? C20 C21 C25 C24 -58.5(10) . . . . ? C19 C26 C24 C25 -61.7(9) . . . . ? C19 C26 C24 C23 58.6(9) . . . . ? C21 C25 C24 C26 60.5(10) . . . . ? C21 C25 C24 C23 -61.4(10) . . . . ? C17 C23 C24 C26 -58.4(10) . . . . ? C17 C23 C24 C25 62.9(10) . . . . ? C20 C21 C22 C17 58.0(10) . . . . ? C25 C21 C22 C17 -58.9(10) . . . . ? C23 C17 C22 C21 59.4(10) . . . . ? C16 C17 C22 C21 179.7(7) . . . . ? C18 C17 C22 C21 -57.8(9) . . . . ? C40 C41 C37 C38 -1.0(14) . . . . ? C40 C41 C37 C36 -177.3(9) . . . . ? C39 C38 C37 C41 1.7(14) . . . . ? C39 C38 C37 C36 178.1(9) . . . . ? C35 C36 C37 C41 52.0(14) . . . . ? C35 C36 C37 C38 -124.1(10) . . . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.822 _refine_diff_density_min -1.033 _refine_diff_density_rms 0.129 data_5 _database_code_depnum_ccdc_archive 'CCDC 761115' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C41 H50 N2 O8 Zn2' _chemical_formula_sum 'C41 H50 N2 O8 Zn2' _chemical_formula_weight 829.57 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.7872(15) _cell_length_b 12.1029(15) _cell_length_c 14.0397(17) _cell_angle_alpha 101.690(2) _cell_angle_beta 105.584(2) _cell_angle_gamma 103.652(2) _cell_volume 1797.4(4) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 846 _cell_measurement_theta_min 2.815 _cell_measurement_theta_max 17.614 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.533 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 868 _exptl_absorpt_coefficient_mu 1.393 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8732 _exptl_absorpt_correction_T_max 0.9336 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15833 _diffrn_reflns_av_R_equivalents 0.0471 _diffrn_reflns_av_sigmaI/netI 0.0738 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 26.34 _reflns_number_total 7282 _reflns_number_gt 5009 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0375P)^2^+1.1409P] 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 7282 _refine_ls_number_parameters 478 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0769 _refine_ls_R_factor_gt 0.0426 _refine_ls_wR_factor_ref 0.0976 _refine_ls_wR_factor_gt 0.0858 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.020 _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 0.74125(4) 0.68706(3) 0.18827(3) 0.01503(11) Uani 1 1 d U . . Zn2 Zn 0.75525(4) 0.78529(3) 0.41799(3) 0.01504(11) Uani 1 1 d . . . N1 N 0.7340(3) 1.5228(2) 1.0956(2) 0.0154(6) Uani 1 1 d . . . N2 N 0.7708(3) 0.9149(2) 0.5405(2) 0.0166(6) Uani 1 1 d . . . O1 O 0.7670(2) 0.8572(2) 0.30506(17) 0.0164(5) Uani 1 1 d . . . O2 O 0.5890(2) 0.8864(2) 0.31096(19) 0.0200(6) Uani 1 1 d . . . O5 O 0.6644(2) 0.7516(2) 0.07128(18) 0.0192(6) Uani 1 1 d . . . O6 O 0.8632(2) 0.7805(2) 0.10285(18) 0.0226(5) Uani 1 1 d U . . O8 O 0.4001(2) 0.3377(2) -0.37827(18) 0.0189(5) Uani 1 1 d . . . O7 O 0.4208(2) 0.3851(2) -0.21024(18) 0.0193(6) Uani 1 1 d . . . O3 O 1.0930(2) 1.2561(2) 0.53733(18) 0.0191(6) Uani 1 1 d . . . O4 O 1.1112(2) 1.3237(2) 0.70229(18) 0.0210(6) Uani 1 1 d . . . C1 C 0.6808(3) 0.9096(3) 0.2845(3) 0.0171(8) Uani 1 1 d . . . C2 C 0.7049(3) 1.0041(3) 0.2308(3) 0.0169(8) Uani 1 1 d . . . H2A H 0.6343 0.9843 0.1664 0.020 Uiso 1 1 calc R . . H2B H 0.7798 1.0045 0.2115 0.020 Uiso 1 1 calc R . . C15 C 0.7618(3) 0.7862(3) 0.0494(3) 0.0169(8) Uani 1 1 d . . . C16 C 0.7519(3) 0.8303(3) -0.0447(3) 0.0167(8) Uani 1 1 d . . . H16A H 0.8199 0.9050 -0.0266 0.020 Uiso 1 1 calc R . . H16B H 0.6726 0.8482 -0.0656 0.020 Uiso 1 1 calc R . . C28 C 0.4641(3) 0.3728(3) -0.2831(3) 0.0169(8) Uani 1 1 d . . . C27 C 0.6023(3) 0.3986(3) -0.2565(3) 0.0164(8) Uani 1 1 d . . . H27A H 0.6179 0.3435 -0.3105 0.020 Uiso 1 1 calc R . . H27B H 0.6342 0.3800 -0.1908 0.020 Uiso 1 1 calc R . . C14 C 1.0531(3) 1.2974(3) 0.6079(3) 0.0163(8) Uani 1 1 d . . . C13 C 0.9270(3) 1.3156(3) 0.5811(3) 0.0159(7) Uani 1 1 d . . . H13A H 0.9406 1.4006 0.6128 0.019 Uiso 1 1 calc R . . H13B H 0.8804 1.2708 0.6175 0.019 Uiso 1 1 calc R . . C40 C 0.8393(3) 1.5048(3) 1.0875(3) 0.0178(8) Uani 1 1 d . . . H40 H 0.9127 1.5705 1.1129 0.021 Uiso 1 1 calc R . . C41 C 0.8447(4) 1.3943(3) 1.0434(3) 0.0212(8) Uani 1 1 d . . . H41 H 0.9206 1.3852 1.0375 0.025 Uiso 1 1 calc R . . C37 C 0.7400(4) 1.2969(3) 1.0080(3) 0.0192(8) Uani 1 1 d . . . C38 C 0.6300(4) 1.3172(3) 1.0112(3) 0.0205(8) Uani 1 1 d . . . H38 H 0.5545 1.2539 0.9830 0.025 Uiso 1 1 calc R . . C39 C 0.6311(3) 1.4304(3) 1.0557(3) 0.0180(8) Uani 1 1 d . . . H39 H 0.5552 1.4429 1.0580 0.022 Uiso 1 1 calc R . . C3 C 0.7233(3) 1.1294(3) 0.2979(3) 0.0144(7) Uani 1 1 d . . . C4 C 0.7710(3) 1.2191(3) 0.2428(3) 0.0173(8) Uani 1 1 d . . . H4A H 0.8497 1.2115 0.2342 0.021 Uiso 1 1 calc R . . H4B H 0.7099 1.2018 0.1734 0.021 Uiso 1 1 calc R . . C5 C 0.7917(3) 1.3457(3) 0.3054(3) 0.0176(8) Uani 1 1 d . . . H5 H 0.8238 1.4030 0.2694 0.021 Uiso 1 1 calc R . . C12 C 0.6687(3) 1.3577(3) 0.3154(3) 0.0195(8) Uani 1 1 d . . . H12A H 0.6810 1.4396 0.3554 0.023 Uiso 1 1 calc R . . H12B H 0.6076 1.3413 0.2462 0.023 Uiso 1 1 calc R . . C10 C 0.6206(3) 1.2695(3) 0.3704(3) 0.0189(8) Uani 1 1 d . . . H10 H 0.5403 1.2768 0.3776 0.023 Uiso 1 1 calc R . . C9 C 0.6011(3) 1.1432(3) 0.3084(3) 0.0165(8) Uani 1 1 d . . . H9A H 0.5397 1.1251 0.2391 0.020 Uiso 1 1 calc R . . H9B H 0.5683 1.0863 0.3435 0.020 Uiso 1 1 calc R . . C7 C 0.8397(3) 1.2845(3) 0.4697(3) 0.0142(7) Uani 1 1 d . . . C11 C 0.7152(3) 1.2956(3) 0.4771(3) 0.0165(8) Uani 1 1 d . . . H11A H 0.6831 1.2394 0.5131 0.020 Uiso 1 1 calc R . . H11B H 0.7274 1.3769 0.5183 0.020 Uiso 1 1 calc R . . C8 C 0.8183(3) 1.1583(3) 0.4056(2) 0.0133(7) Uani 1 1 d . . . H8A H 0.7884 1.1011 0.4415 0.016 Uiso 1 1 calc R . . H8B H 0.8977 1.1502 0.3989 0.016 Uiso 1 1 calc R . . C6 C 0.8853(3) 1.3722(3) 0.4124(3) 0.0167(8) Uani 1 1 d . . . H6A H 0.8985 1.4541 0.4528 0.020 Uiso 1 1 calc R . . H6B H 0.9655 1.3666 0.4060 0.020 Uiso 1 1 calc R . . C17 C 0.7582(3) 0.7407(3) -0.1370(3) 0.0156(7) Uani 1 1 d . . . C18 C 0.7111(3) 0.7776(3) -0.2353(3) 0.0161(8) Uani 1 1 d . . . H18A H 0.6257 0.7809 -0.2451 0.019 Uiso 1 1 calc R . . H18B H 0.7642 0.8577 -0.2277 0.019 Uiso 1 1 calc R . . C19 C 0.7123(3) 0.6891(3) -0.3303(3) 0.0169(8) Uani 1 1 d . . . H19 H 0.6805 0.7139 -0.3935 0.020 Uiso 1 1 calc R . . C20 C 0.8451(3) 0.6874(3) -0.3153(3) 0.0220(8) Uani 1 1 d . . . H20A H 0.8983 0.7671 -0.3089 0.026 Uiso 1 1 calc R . . H20B H 0.8474 0.6305 -0.3759 0.026 Uiso 1 1 calc R . . C21 C 0.8937(3) 0.6508(3) -0.2176(3) 0.0175(8) Uani 1 1 d . . . H21 H 0.9805 0.6495 -0.2077 0.021 Uiso 1 1 calc R . . C25 C 0.8122(3) 0.5283(3) -0.2283(3) 0.0183(8) Uani 1 1 d . . . H25A H 0.8437 0.5049 -0.1651 0.022 Uiso 1 1 calc R . . H25B H 0.8161 0.4702 -0.2872 0.022 Uiso 1 1 calc R . . C26 C 0.6783(3) 0.5256(3) -0.2454(3) 0.0133(7) Uani 1 1 d . . . C23 C 0.6756(3) 0.6154(3) -0.1517(3) 0.0139(7) Uani 1 1 d . . . H23A H 0.5894 0.6163 -0.1617 0.017 Uiso 1 1 calc R . . H23B H 0.7044 0.5904 -0.0889 0.017 Uiso 1 1 calc R . . C24 C 0.6302(3) 0.5645(3) -0.3421(3) 0.0166(8) Uani 1 1 d . . . H24A H 0.5439 0.5650 -0.3524 0.020 Uiso 1 1 calc R . . H24B H 0.6307 0.5076 -0.4034 0.020 Uiso 1 1 calc R . . C22 C 0.8908(3) 0.7392(3) -0.1234(3) 0.0186(8) Uani 1 1 d . . . H22A H 0.9238 0.7160 -0.0603 0.022 Uiso 1 1 calc R . . H22B H 0.9439 0.8195 -0.1153 0.022 Uiso 1 1 calc R . . C33 C 0.8807(3) 0.9763(3) 0.6120(3) 0.0172(8) Uani 1 1 d . . . H33 H 0.9520 0.9580 0.6034 0.021 Uiso 1 1 calc R . . C32 C 0.8959(3) 1.0648(3) 0.6977(3) 0.0177(8) Uani 1 1 d . . . H32 H 0.9760 1.1065 0.7465 0.021 Uiso 1 1 calc R . . C31 C 0.7926(3) 1.0922(3) 0.7117(3) 0.0177(8) Uani 1 1 d . . . C30 C 0.6789(3) 1.0323(3) 0.6352(3) 0.0192(8) Uani 1 1 d . . . H30 H 0.6070 1.0522 0.6401 0.023 Uiso 1 1 calc R . . C29 C 0.6709(3) 0.9441(3) 0.5524(3) 0.0180(8) Uani 1 1 d . . . H29 H 0.5921 0.9023 0.5017 0.022 Uiso 1 1 calc R . . C34 C 0.8028(4) 1.1786(3) 0.8097(3) 0.0223(8) Uani 1 1 d . . . H34A H 0.7864 1.2508 0.7946 0.027 Uiso 1 1 calc R . . H34B H 0.8878 1.2020 0.8594 0.027 Uiso 1 1 calc R . . C35 C 0.7088(4) 1.1212(3) 0.8574(3) 0.0247(9) Uani 1 1 d . . . H35A H 0.6277 1.1307 0.8240 0.030 Uiso 1 1 calc R . . H35B H 0.6983 1.0351 0.8418 0.030 Uiso 1 1 calc R . . C36 C 0.7452(4) 1.1723(3) 0.9729(3) 0.0255(9) Uani 1 1 d . . . H36A H 0.6898 1.1198 0.9984 0.031 Uiso 1 1 calc R . . H36B H 0.8305 1.1715 1.0054 0.031 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0186(2) 0.0155(2) 0.0139(2) 0.00437(17) 0.00567(18) 0.00989(18) Zn2 0.0181(2) 0.0146(2) 0.0145(2) 0.00375(17) 0.00539(17) 0.00913(18) N1 0.0208(16) 0.0153(15) 0.0144(15) 0.0066(12) 0.0065(13) 0.0106(13) N2 0.0208(17) 0.0149(15) 0.0156(15) 0.0042(13) 0.0063(13) 0.0083(13) O1 0.0195(14) 0.0164(12) 0.0161(13) 0.0060(10) 0.0057(11) 0.0100(11) O2 0.0220(14) 0.0149(13) 0.0276(14) 0.0075(11) 0.0103(12) 0.0101(11) O5 0.0277(15) 0.0164(13) 0.0183(13) 0.0077(11) 0.0093(11) 0.0116(12) O6 0.0256(15) 0.0231(14) 0.0175(13) 0.0075(11) 0.0042(10) 0.0064(12) O8 0.0208(14) 0.0187(13) 0.0167(13) 0.0063(11) 0.0036(11) 0.0074(11) O7 0.0209(14) 0.0160(13) 0.0219(14) 0.0010(11) 0.0112(11) 0.0064(11) O3 0.0201(14) 0.0232(13) 0.0170(13) 0.0055(11) 0.0061(11) 0.0122(11) O4 0.0270(15) 0.0231(14) 0.0145(13) 0.0042(11) 0.0035(11) 0.0156(12) C1 0.023(2) 0.0118(17) 0.0141(18) -0.0005(14) 0.0021(16) 0.0101(16) C2 0.023(2) 0.0152(18) 0.0133(18) 0.0029(15) 0.0052(15) 0.0089(16) C15 0.027(2) 0.0119(17) 0.0090(17) -0.0009(14) 0.0028(16) 0.0081(16) C16 0.022(2) 0.0119(17) 0.0171(18) 0.0038(15) 0.0055(15) 0.0082(15) C28 0.026(2) 0.0057(16) 0.022(2) 0.0032(15) 0.0089(17) 0.0088(15) C27 0.023(2) 0.0139(17) 0.0166(18) 0.0045(15) 0.0085(16) 0.0107(16) C14 0.023(2) 0.0104(17) 0.0161(19) 0.0044(14) 0.0068(16) 0.0056(15) C13 0.0142(18) 0.0164(18) 0.0154(18) 0.0015(15) 0.0022(15) 0.0077(15) C40 0.021(2) 0.0172(18) 0.0177(19) 0.0079(15) 0.0061(16) 0.0089(16) C41 0.025(2) 0.025(2) 0.021(2) 0.0088(17) 0.0116(17) 0.0154(18) C37 0.036(2) 0.0160(18) 0.0137(18) 0.0064(15) 0.0127(17) 0.0165(18) C38 0.029(2) 0.0164(18) 0.0156(19) 0.0027(15) 0.0087(16) 0.0067(17) C39 0.0189(19) 0.0198(19) 0.0178(19) 0.0061(16) 0.0067(16) 0.0090(16) C3 0.0179(19) 0.0123(17) 0.0163(18) 0.0052(15) 0.0070(15) 0.0081(15) C4 0.0194(19) 0.0197(19) 0.0176(19) 0.0082(15) 0.0072(15) 0.0110(16) C5 0.023(2) 0.0126(17) 0.0180(19) 0.0075(15) 0.0041(16) 0.0072(15) C12 0.025(2) 0.0139(18) 0.022(2) 0.0065(15) 0.0049(16) 0.0108(16) C10 0.0168(19) 0.0178(18) 0.024(2) 0.0053(16) 0.0060(16) 0.0113(16) C9 0.0203(19) 0.0133(17) 0.0175(18) 0.0055(15) 0.0056(15) 0.0076(15) C7 0.0150(18) 0.0135(17) 0.0137(17) 0.0038(14) 0.0020(14) 0.0067(15) C11 0.021(2) 0.0135(17) 0.0188(19) 0.0053(15) 0.0075(16) 0.0106(16) C8 0.0163(18) 0.0121(17) 0.0142(17) 0.0051(14) 0.0056(14) 0.0072(15) C6 0.0176(19) 0.0137(17) 0.0182(19) 0.0039(15) 0.0038(15) 0.0067(15) C17 0.0162(18) 0.0181(18) 0.0151(18) 0.0073(15) 0.0059(15) 0.0072(15) C18 0.0171(19) 0.0131(17) 0.0219(19) 0.0096(15) 0.0067(15) 0.0074(15) C19 0.022(2) 0.0162(18) 0.0172(18) 0.0091(15) 0.0091(15) 0.0084(16) C20 0.024(2) 0.024(2) 0.026(2) 0.0111(17) 0.0145(17) 0.0114(17) C21 0.0132(18) 0.0198(19) 0.023(2) 0.0096(16) 0.0076(15) 0.0072(16) C25 0.022(2) 0.0205(19) 0.0175(19) 0.0076(16) 0.0079(16) 0.0127(16) C26 0.0130(18) 0.0129(17) 0.0156(18) 0.0050(14) 0.0049(14) 0.0060(14) C23 0.0162(19) 0.0123(17) 0.0150(18) 0.0034(14) 0.0052(15) 0.0082(15) C24 0.0217(19) 0.0189(19) 0.0144(18) 0.0083(15) 0.0068(15) 0.0120(16) C22 0.0178(19) 0.0192(19) 0.0198(19) 0.0095(16) 0.0040(16) 0.0067(16) C33 0.019(2) 0.0176(18) 0.0196(19) 0.0082(16) 0.0059(16) 0.0112(16) C32 0.0189(19) 0.0158(18) 0.0181(19) 0.0064(15) 0.0042(15) 0.0056(16) C31 0.026(2) 0.0131(17) 0.0188(19) 0.0087(15) 0.0106(16) 0.0069(16) C30 0.022(2) 0.025(2) 0.0196(19) 0.0100(16) 0.0118(16) 0.0143(17) C29 0.019(2) 0.0208(19) 0.0152(18) 0.0075(16) 0.0050(15) 0.0074(16) C34 0.029(2) 0.0180(19) 0.020(2) 0.0002(16) 0.0088(17) 0.0103(17) C35 0.035(2) 0.0166(19) 0.026(2) 0.0065(17) 0.0137(18) 0.0098(18) C36 0.041(3) 0.021(2) 0.023(2) 0.0101(17) 0.0138(19) 0.0198(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 Zn1 O7 2.036(2) 2_665 ? Zn1 O4 2.038(2) 2_776 ? Zn1 O5 2.045(2) . ? Zn1 N1 2.113(3) 1_544 ? Zn1 O1 2.256(2) . ? Zn1 O6 2.343(3) . ? Zn2 O8 1.926(2) 2_665 ? Zn2 O3 1.947(2) 2_776 ? Zn2 O1 1.978(2) . ? Zn2 N2 2.014(3) . ? N1 C39 1.333(4) . ? N1 C40 1.339(4) . ? N1 Zn1 2.113(3) 1_566 ? N2 C33 1.335(4) . ? N2 C29 1.349(4) . ? O1 C1 1.318(4) . ? O2 C1 1.226(4) . ? O5 C15 1.266(4) . ? O6 C15 1.255(4) . ? O8 C28 1.270(4) . ? O8 Zn2 1.926(2) 2_665 ? O7 C28 1.258(4) . ? O7 Zn1 2.036(2) 2_665 ? O3 C14 1.270(4) . ? O3 Zn2 1.947(2) 2_776 ? O4 C14 1.250(4) . ? O4 Zn1 2.038(2) 2_776 ? C1 C2 1.507(5) . ? C2 C3 1.547(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C15 C16 1.510(5) . ? C16 C17 1.543(5) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C28 C27 1.508(5) . ? C27 C26 1.539(5) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C14 C13 1.513(5) . ? C13 C7 1.536(4) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C40 C41 1.379(5) . ? C40 H40 0.9500 . ? C41 C37 1.380(5) . ? C41 H41 0.9500 . ? C37 C38 1.386(5) . ? C37 C36 1.510(5) . ? C38 C39 1.381(5) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C3 C9 1.530(5) . ? C3 C8 1.535(5) . ? C3 C4 1.543(5) . ? C4 C5 1.530(5) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.525(5) . ? C5 C12 1.531(5) . ? C5 H5 1.0000 . ? C12 C10 1.530(5) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C10 C11 1.527(5) . ? C10 C9 1.528(4) . ? C10 H10 1.0000 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C7 C8 1.532(4) . ? C7 C11 1.534(5) . ? C7 C6 1.539(5) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C17 C22 1.528(5) . ? C17 C23 1.536(5) . ? C17 C18 1.539(5) . ? C18 C19 1.538(5) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.529(5) . ? C19 C24 1.536(5) . ? C19 H19 1.0000 . ? C20 C21 1.533(5) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C25 1.518(5) . ? C21 C22 1.537(5) . ? C21 H21 1.0000 . ? C25 C26 1.523(5) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C24 1.535(4) . ? C26 C23 1.540(4) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C33 C32 1.378(5) . ? C33 H33 0.9500 . ? C32 C31 1.386(5) . ? C32 H32 0.9500 . ? C31 C30 1.388(5) . ? C31 C34 1.507(5) . ? C30 C29 1.375(5) . ? C30 H30 0.9500 . ? C29 H29 0.9500 . ? C34 C35 1.543(5) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.514(5) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? 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 O7 Zn1 O4 111.35(10) 2_665 2_776 ? O7 Zn1 O5 95.50(10) 2_665 . ? O4 Zn1 O5 152.41(10) 2_776 . ? O7 Zn1 N1 92.42(10) 2_665 1_544 ? O4 Zn1 N1 87.98(10) 2_776 1_544 ? O5 Zn1 N1 97.43(10) . 1_544 ? O7 Zn1 O1 88.80(9) 2_665 . ? O4 Zn1 O1 84.32(9) 2_776 . ? O5 Zn1 O1 90.21(9) . . ? N1 Zn1 O1 172.11(10) 1_544 . ? O7 Zn1 O6 154.73(9) 2_665 . ? O4 Zn1 O6 93.92(9) 2_776 . ? O5 Zn1 O6 59.46(9) . . ? N1 Zn1 O6 87.97(10) 1_544 . ? O1 Zn1 O6 94.25(8) . . ? O8 Zn2 O3 117.97(10) 2_665 2_776 ? O8 Zn2 O1 111.24(10) 2_665 . ? O3 Zn2 O1 106.08(10) 2_776 . ? O8 Zn2 N2 109.87(11) 2_665 . ? O3 Zn2 N2 103.29(11) 2_776 . ? O1 Zn2 N2 107.71(11) . . ? C39 N1 C40 117.8(3) . . ? C39 N1 Zn1 122.4(2) . 1_566 ? C40 N1 Zn1 119.2(2) . 1_566 ? C33 N2 C29 117.6(3) . . ? C33 N2 Zn2 121.2(2) . . ? C29 N2 Zn2 121.2(2) . . ? C1 O1 Zn2 109.9(2) . . ? C1 O1 Zn1 117.06(19) . . ? Zn2 O1 Zn1 95.85(9) . . ? C15 O5 Zn1 96.4(2) . . ? C15 O6 Zn1 83.1(2) . . ? C28 O8 Zn2 116.4(2) . 2_665 ? C28 O7 Zn1 136.6(2) . 2_665 ? C14 O3 Zn2 116.3(2) . 2_776 ? C14 O4 Zn1 145.9(2) . 2_776 ? O2 C1 O1 122.3(3) . . ? O2 C1 C2 121.8(3) . . ? O1 C1 C2 115.8(3) . . ? C1 C2 C3 113.0(3) . . ? C1 C2 H2A 109.0 . . ? C3 C2 H2A 109.0 . . ? C1 C2 H2B 109.0 . . ? C3 C2 H2B 109.0 . . ? H2A C2 H2B 107.8 . . ? O6 C15 O5 120.8(3) . . ? O6 C15 C16 120.8(3) . . ? O5 C15 C16 118.3(3) . . ? C15 C16 C17 113.3(3) . . ? C15 C16 H16A 108.9 . . ? C17 C16 H16A 108.9 . . ? C15 C16 H16B 108.9 . . ? C17 C16 H16B 108.9 . . ? H16A C16 H16B 107.7 . . ? O7 C28 O8 125.0(3) . . ? O7 C28 C27 118.2(3) . . ? O8 C28 C27 116.8(3) . . ? C28 C27 C26 117.0(3) . . ? C28 C27 H27A 108.0 . . ? C26 C27 H27A 108.0 . . ? C28 C27 H27B 108.0 . . ? C26 C27 H27B 108.0 . . ? H27A C27 H27B 107.3 . . ? O4 C14 O3 124.2(3) . . ? O4 C14 C13 115.3(3) . . ? O3 C14 C13 120.6(3) . . ? C14 C13 C7 123.1(3) . . ? C14 C13 H13A 106.5 . . ? C7 C13 H13A 106.5 . . ? C14 C13 H13B 106.5 . . ? C7 C13 H13B 106.5 . . ? H13A C13 H13B 106.5 . . ? N1 C40 C41 122.2(3) . . ? N1 C40 H40 118.9 . . ? C41 C40 H40 118.9 . . ? C40 C41 C37 120.1(3) . . ? C40 C41 H41 119.9 . . ? C37 C41 H41 119.9 . . ? C41 C37 C38 117.2(3) . . ? C41 C37 C36 121.9(3) . . ? C38 C37 C36 120.8(4) . . ? C39 C38 C37 119.4(4) . . ? C39 C38 H38 120.3 . . ? C37 C38 H38 120.3 . . ? N1 C39 C38 122.9(3) . . ? N1 C39 H39 118.6 . . ? C38 C39 H39 118.6 . . ? C9 C3 C8 109.3(3) . . ? C9 C3 C4 107.9(3) . . ? C8 C3 C4 108.9(3) . . ? C9 C3 C2 111.5(3) . . ? C8 C3 C2 111.7(3) . . ? C4 C3 C2 107.5(3) . . ? C5 C4 C3 110.3(3) . . ? C5 C4 H4A 109.6 . . ? C3 C4 H4A 109.6 . . ? C5 C4 H4B 109.6 . . ? C3 C4 H4B 109.6 . . ? H4A C4 H4B 108.1 . . ? C6 C5 C4 109.6(3) . . ? C6 C5 C12 109.5(3) . . ? C4 C5 C12 109.3(3) . . ? C6 C5 H5 109.5 . . ? C4 C5 H5 109.5 . . ? C12 C5 H5 109.5 . . ? C10 C12 C5 108.9(3) . . ? C10 C12 H12A 109.9 . . ? C5 C12 H12A 109.9 . . ? C10 C12 H12B 109.9 . . ? C5 C12 H12B 109.9 . . ? H12A C12 H12B 108.3 . . ? C11 C10 C9 108.8(3) . . ? C11 C10 C12 109.5(3) . . ? C9 C10 C12 109.8(3) . . ? C11 C10 H10 109.6 . . ? C9 C10 H10 109.6 . . ? C12 C10 H10 109.6 . . ? C10 C9 C3 110.5(3) . . ? C10 C9 H9A 109.6 . . ? C3 C9 H9A 109.6 . . ? C10 C9 H9B 109.6 . . ? C3 C9 H9B 109.6 . . ? H9A C9 H9B 108.1 . . ? C8 C7 C11 108.4(3) . . ? C8 C7 C13 113.6(3) . . ? C11 C7 C13 106.3(3) . . ? C8 C7 C6 108.7(3) . . ? C11 C7 C6 107.6(3) . . ? C13 C7 C6 112.1(3) . . ? C10 C11 C7 111.3(3) . . ? C10 C11 H11A 109.4 . . ? C7 C11 H11A 109.4 . . ? C10 C11 H11B 109.4 . . ? C7 C11 H11B 109.4 . . ? H11A C11 H11B 108.0 . . ? C7 C8 C3 111.2(3) . . ? C7 C8 H8A 109.4 . . ? C3 C8 H8A 109.4 . . ? C7 C8 H8B 109.4 . . ? C3 C8 H8B 109.4 . . ? H8A C8 H8B 108.0 . . ? C5 C6 C7 111.0(3) . . ? C5 C6 H6A 109.4 . . ? C7 C6 H6A 109.4 . . ? C5 C6 H6B 109.4 . . ? C7 C6 H6B 109.4 . . ? H6A C6 H6B 108.0 . . ? C22 C17 C23 109.5(3) . . ? C22 C17 C18 107.9(3) . . ? C23 C17 C18 108.3(3) . . ? C22 C17 C16 111.6(3) . . ? C23 C17 C16 110.7(3) . . ? C18 C17 C16 108.7(3) . . ? C19 C18 C17 110.8(3) . . ? C19 C18 H18A 109.5 . . ? C17 C18 H18A 109.5 . . ? C19 C18 H18B 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 108.1 . . ? C20 C19 C24 109.3(3) . . ? C20 C19 C18 108.9(3) . . ? C24 C19 C18 109.6(3) . . ? C20 C19 H19 109.7 . . ? C24 C19 H19 109.7 . . ? C18 C19 H19 109.7 . . ? C19 C20 C21 109.3(3) . . ? C19 C20 H20A 109.8 . . ? C21 C20 H20A 109.8 . . ? C19 C20 H20B 109.8 . . ? C21 C20 H20B 109.8 . . ? H20A C20 H20B 108.3 . . ? C25 C21 C20 109.5(3) . . ? C25 C21 C22 108.8(3) . . ? C20 C21 C22 110.0(3) . . ? C25 C21 H21 109.5 . . ? C20 C21 H21 109.5 . . ? C22 C21 H21 109.5 . . ? C21 C25 C26 111.3(3) . . ? C21 C25 H25A 109.4 . . ? C26 C25 H25A 109.4 . . ? C21 C25 H25B 109.4 . . ? C26 C25 H25B 109.4 . . ? H25A C25 H25B 108.0 . . ? C25 C26 C24 109.5(3) . . ? C25 C26 C27 107.9(3) . . ? C24 C26 C27 111.6(3) . . ? C25 C26 C23 107.9(3) . . ? C24 C26 C23 108.4(3) . . ? C27 C26 C23 111.5(3) . . ? C17 C23 C26 111.2(3) . . ? C17 C23 H23A 109.4 . . ? C26 C23 H23A 109.4 . . ? C17 C23 H23B 109.4 . . ? C26 C23 H23B 109.4 . . ? H23A C23 H23B 108.0 . . ? C26 C24 C19 110.0(3) . . ? C26 C24 H24A 109.7 . . ? C19 C24 H24A 109.7 . . ? C26 C24 H24B 109.7 . . ? C19 C24 H24B 109.7 . . ? H24A C24 H24B 108.2 . . ? C17 C22 C21 110.0(3) . . ? C17 C22 H22A 109.7 . . ? C21 C22 H22A 109.7 . . ? C17 C22 H22B 109.7 . . ? C21 C22 H22B 109.7 . . ? H22A C22 H22B 108.2 . . ? N2 C33 C32 123.4(3) . . ? N2 C33 H33 118.3 . . ? C32 C33 H33 118.3 . . ? C33 C32 C31 119.0(3) . . ? C33 C32 H32 120.5 . . ? C31 C32 H32 120.5 . . ? C32 C31 C30 117.8(3) . . ? C32 C31 C34 120.8(3) . . ? C30 C31 C34 121.3(3) . . ? C29 C30 C31 119.7(3) . . ? C29 C30 H30 120.1 . . ? C31 C30 H30 120.1 . . ? N2 C29 C30 122.4(3) . . ? N2 C29 H29 118.8 . . ? C30 C29 H29 118.8 . . ? C31 C34 C35 110.0(3) . . ? C31 C34 H34A 109.7 . . ? C35 C34 H34A 109.7 . . ? C31 C34 H34B 109.7 . . ? C35 C34 H34B 109.7 . . ? H34A C34 H34B 108.2 . . ? C36 C35 C34 114.4(3) . . ? C36 C35 H35A 108.7 . . ? C34 C35 H35A 108.7 . . ? C36 C35 H35B 108.7 . . ? C34 C35 H35B 108.7 . . ? H35A C35 H35B 107.6 . . ? C37 C36 C35 115.3(3) . . ? C37 C36 H36A 108.5 . . ? C35 C36 H36A 108.5 . . ? C37 C36 H36B 108.5 . . ? C35 C36 H36B 108.5 . . ? H36A C36 H36B 107.5 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.34 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.645 _refine_diff_density_min -0.848 _refine_diff_density_rms 0.095 data_6 _database_code_depnum_ccdc_archive 'CCDC 761116' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H46 Cd N2 O8' _chemical_formula_sum 'C38 H46 Cd N2 O8' _chemical_formula_weight 771.17 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' Cd Cd -0.8075 1.2024 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 32.433(2) _cell_length_b 6.9550(4) _cell_length_c 16.9017(11) _cell_angle_alpha 90.00 _cell_angle_beta 116.5320(10) _cell_angle_gamma 90.00 _cell_volume 3411.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 4585 _cell_measurement_theta_min 2.418 _cell_measurement_theta_max 27.632 _exptl_crystal_description colorless _exptl_crystal_colour block _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.502 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1600 _exptl_absorpt_coefficient_mu 0.697 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8966 _exptl_absorpt_correction_T_max 0.9210 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8190 _diffrn_reflns_av_R_equivalents 0.0165 _diffrn_reflns_av_sigmaI/netI 0.0195 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 25.10 _reflns_number_total 3031 _reflns_number_gt 2776 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0416P)^2^+3.7891P] 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 3031 _refine_ls_number_parameters 222 _refine_ls_number_restraints 27 _refine_ls_R_factor_all 0.0453 _refine_ls_R_factor_gt 0.0420 _refine_ls_wR_factor_ref 0.1122 _refine_ls_wR_factor_gt 0.1104 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.041 _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 0.0000 0.41999(5) 0.2500 0.03481(16) Uani 1 2 d S . . N1 N -0.00337(11) 0.6471(5) 0.1485(2) 0.0389(7) Uani 1 1 d . . . O1 O 0.05402(11) 0.1994(5) 0.3396(2) 0.0675(8) Uani 1 1 d U . . O2 O 0.07463(13) 0.3770(6) 0.2630(3) 0.0781(9) Uani 1 1 d U . . O3 O 0.09856(13) 0.3791(7) 0.6131(2) 0.0753(11) Uani 1 1 d U . . O4 O 0.14180(16) 0.4184(8) 0.7543(3) 0.1094(19) Uani 1 1 d U . . H4 H 0.1180 0.4649 0.7516 0.131 Uiso 1 1 d R . . C1 C 0.08418(16) 0.2500(8) 0.3194(3) 0.0604(9) Uani 1 1 d U . . C2 C 0.13077(14) 0.1566(7) 0.3531(3) 0.0450(9) Uani 1 1 d . . . H2A H 0.1521 0.2516 0.3506 0.054 Uiso 1 1 calc R . . H2B H 0.1286 0.0546 0.3122 0.054 Uiso 1 1 calc R . . C3 C 0.15227(13) 0.0709(5) 0.4469(3) 0.0353(8) Uani 1 1 d . . . C4 C 0.20223(13) 0.0160(6) 0.4701(3) 0.0428(9) Uani 1 1 d . . . H4A H 0.2025 -0.0788 0.4282 0.051 Uiso 1 1 calc R . . H4B H 0.2188 0.1287 0.4659 0.051 Uiso 1 1 calc R . . C5 C 0.22632(14) -0.0664(6) 0.5639(3) 0.0463(10) Uani 1 1 d . . . H5 H 0.2583 -0.0990 0.5782 0.056 Uiso 1 1 calc R . . C6 C 0.20086(16) -0.2473(6) 0.5688(3) 0.0542(11) Uani 1 1 d . . . H6A H 0.2160 -0.3017 0.6278 0.065 Uiso 1 1 calc R . . H6B H 0.2013 -0.3424 0.5272 0.065 Uiso 1 1 calc R . . C7 C 0.15095(15) -0.1952(6) 0.5464(3) 0.0477(10) Uani 1 1 d . . . H7 H 0.1346 -0.3111 0.5496 0.057 Uiso 1 1 calc R . . C8 C 0.12684(14) -0.1115(6) 0.4527(3) 0.0422(9) Uani 1 1 d . . . H8A H 0.0951 -0.0802 0.4383 0.051 Uiso 1 1 calc R . . H8B H 0.1267 -0.2059 0.4103 0.051 Uiso 1 1 calc R . . C9 C 0.22567(14) 0.0816(6) 0.6297(3) 0.0459(10) Uani 1 1 d . . . H9A H 0.2423 0.1956 0.6273 0.055 Uiso 1 1 calc R . . H9B H 0.2411 0.0294 0.6891 0.055 Uiso 1 1 calc R . . C10 C 0.17586(13) 0.1370(6) 0.6090(3) 0.0387(9) Uani 1 1 d . . . C11 C 0.15032(15) -0.0466(6) 0.6127(3) 0.0457(10) Uani 1 1 d . . . H11A H 0.1650 -0.1000 0.6719 0.055 Uiso 1 1 calc R . . H11B H 0.1187 -0.0153 0.5990 0.055 Uiso 1 1 calc R . . C12 C 0.15220(13) 0.2183(5) 0.5143(2) 0.0360(8) Uani 1 1 d . . . H12A H 0.1207 0.2532 0.4999 0.043 Uiso 1 1 calc R . . H12B H 0.1682 0.3336 0.5110 0.043 Uiso 1 1 calc R . . C13 C 0.17860(15) 0.2834(7) 0.6786(3) 0.0496(10) Uani 1 1 d . . . H13A H 0.1958 0.2243 0.7361 0.060 Uiso 1 1 calc R . . H13B H 0.1968 0.3911 0.6754 0.060 Uiso 1 1 calc R . . C14 C 0.13502(16) 0.3638(7) 0.6759(3) 0.0502(10) Uani 1 1 d U . . C15 C -0.02685(14) 0.6240(6) 0.0609(3) 0.0400(9) Uani 1 1 d . . . H15 H -0.0445 0.5135 0.0393 0.048 Uiso 1 1 calc R . . C16 C -0.02603(13) 0.7568(6) 0.0013(2) 0.0396(9) Uani 1 1 d . . . H16 H -0.0426 0.7337 -0.0591 0.048 Uiso 1 1 calc R . . C17 C -0.00067(13) 0.9252(5) 0.0306(2) 0.0332(8) Uani 1 1 d . . . C18 C 0.02365(15) 0.9468(6) 0.1219(3) 0.0439(10) Uani 1 1 d . . . H18 H 0.0413 1.0566 0.1454 0.053 Uiso 1 1 calc R . . C19 C 0.02172(15) 0.8077(6) 0.1769(3) 0.0476(10) Uani 1 1 d . . . H19 H 0.0388 0.8253 0.2376 0.057 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0336(2) 0.0353(2) 0.0324(2) 0.000 0.01195(17) 0.000 N1 0.0389(17) 0.0424(18) 0.0334(17) 0.0025(14) 0.0142(14) 0.0010(15) O1 0.0425(15) 0.077(2) 0.0839(19) 0.0384(16) 0.0289(14) 0.0143(14) O2 0.0556(17) 0.091(2) 0.090(2) 0.0529(16) 0.0348(16) 0.0213(15) O3 0.055(2) 0.115(3) 0.056(2) 0.009(2) 0.0249(18) 0.027(2) O4 0.072(3) 0.167(5) 0.076(3) -0.060(3) 0.021(2) 0.018(3) C1 0.0447(16) 0.0732(19) 0.0711(19) 0.0362(15) 0.0329(14) 0.0199(15) C2 0.042(2) 0.054(2) 0.040(2) 0.0072(19) 0.0189(18) 0.006(2) C3 0.0311(19) 0.0325(19) 0.041(2) 0.0020(16) 0.0145(16) 0.0018(15) C4 0.035(2) 0.043(2) 0.052(2) 0.0017(19) 0.0208(19) 0.0044(18) C5 0.031(2) 0.049(2) 0.054(3) 0.0045(19) 0.0148(19) 0.0104(18) C6 0.056(3) 0.037(2) 0.065(3) 0.010(2) 0.023(2) 0.012(2) C7 0.048(2) 0.033(2) 0.059(3) 0.0073(19) 0.022(2) -0.0036(18) C8 0.037(2) 0.036(2) 0.050(2) -0.0052(17) 0.0171(18) -0.0052(17) C9 0.033(2) 0.051(3) 0.043(2) 0.0048(18) 0.0075(17) 0.0038(18) C10 0.0320(19) 0.040(2) 0.039(2) 0.0006(17) 0.0111(16) 0.0024(16) C11 0.043(2) 0.051(3) 0.044(2) 0.0124(19) 0.0197(19) 0.0025(19) C12 0.0309(18) 0.0313(19) 0.043(2) 0.0005(16) 0.0147(16) -0.0004(15) C13 0.044(2) 0.057(3) 0.042(2) -0.005(2) 0.0129(18) 0.002(2) C14 0.050(2) 0.055(2) 0.047(2) -0.006(2) 0.023(2) -0.001(2) C15 0.040(2) 0.037(2) 0.038(2) -0.0002(16) 0.0124(17) 0.0008(17) C16 0.042(2) 0.040(2) 0.0304(19) -0.0013(16) 0.0104(16) 0.0005(17) C17 0.0320(18) 0.035(2) 0.0323(18) -0.0005(14) 0.0146(16) 0.0060(15) C18 0.051(2) 0.045(2) 0.032(2) -0.0055(17) 0.0156(18) -0.0113(19) C19 0.052(2) 0.053(3) 0.031(2) -0.0001(18) 0.0135(18) -0.008(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N1 2.298(3) 2 ? Cd1 N1 2.298(3) . ? Cd1 O1 2.312(3) 2 ? Cd1 O1 2.312(3) . ? Cd1 O2 2.350(4) . ? Cd1 O2 2.350(4) 2 ? Cd1 C1 2.714(4) 2 ? N1 C19 1.339(5) . ? N1 C15 1.339(5) . ? O1 C1 1.223(5) . ? O2 C1 1.233(5) . ? O3 C14 1.189(6) . ? O4 C14 1.300(6) . ? O4 H4 0.8200 . ? C1 C2 1.503(6) . ? C2 C3 1.540(5) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C12 1.533(5) . ? C3 C4 1.536(5) . ? C3 C8 1.539(5) . ? C4 C5 1.533(6) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C9 1.522(6) . ? C5 C6 1.527(6) . ? C5 H5 0.9800 . ? C6 C7 1.532(6) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C11 1.531(6) . ? C7 C8 1.534(6) . ? C7 H7 0.9800 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.541(5) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C13 1.529(6) . ? C10 C11 1.538(6) . ? C10 C12 1.540(5) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.502(6) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C15 C16 1.376(6) . ? C15 H15 0.9300 . ? C16 C17 1.389(5) . ? C16 H16 0.9300 . ? C17 C18 1.392(5) . ? C17 C17 1.482(7) 5_575 ? C18 C19 1.363(6) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cd1 N1 93.17(17) 2 . ? N1 Cd1 O1 135.59(11) 2 2 ? N1 Cd1 O1 101.41(13) . 2 ? N1 Cd1 O1 101.41(13) 2 . ? N1 Cd1 O1 135.59(11) . . ? O1 Cd1 O1 96.9(2) 2 . ? N1 Cd1 O2 108.31(15) 2 . ? N1 Cd1 O2 81.99(12) . . ? O1 Cd1 O2 115.10(14) 2 . ? O1 Cd1 O2 53.62(11) . . ? N1 Cd1 O2 81.99(12) 2 2 ? N1 Cd1 O2 108.31(14) . 2 ? O1 Cd1 O2 53.62(11) 2 2 ? O1 Cd1 O2 115.10(14) . 2 ? O2 Cd1 O2 165.4(2) . 2 ? N1 Cd1 C1 108.97(12) 2 2 ? N1 Cd1 C1 105.89(15) . 2 ? O1 Cd1 C1 26.67(12) 2 2 ? O1 Cd1 C1 108.38(15) . 2 ? O2 Cd1 C1 141.29(15) . 2 ? O2 Cd1 C1 26.97(12) 2 2 ? C19 N1 C15 116.8(3) . . ? C19 N1 Cd1 119.1(3) . . ? C15 N1 Cd1 123.9(3) . . ? C1 O1 Cd1 95.3(3) . . ? C1 O2 Cd1 93.2(3) . . ? C14 O4 H4 109.4 . . ? O1 C1 O2 117.8(4) . . ? O1 C1 C2 124.3(4) . . ? O2 C1 C2 117.7(4) . . ? C1 C2 C3 118.3(3) . . ? C1 C2 H2A 107.7 . . ? C3 C2 H2A 107.7 . . ? C1 C2 H2B 107.7 . . ? C3 C2 H2B 107.7 . . ? H2A C2 H2B 107.1 . . ? C12 C3 C4 109.2(3) . . ? C12 C3 C8 109.0(3) . . ? C4 C3 C8 108.3(3) . . ? C12 C3 C2 110.9(3) . . ? C4 C3 C2 107.4(3) . . ? C8 C3 C2 112.1(3) . . ? C5 C4 C3 110.4(3) . . ? C5 C4 H4A 109.6 . . ? C3 C4 H4A 109.6 . . ? C5 C4 H4B 109.6 . . ? C3 C4 H4B 109.6 . . ? H4A C4 H4B 108.1 . . ? C9 C5 C6 109.5(4) . . ? C9 C5 C4 109.6(3) . . ? C6 C5 C4 109.0(4) . . ? C9 C5 H5 109.6 . . ? C6 C5 H5 109.6 . . ? C4 C5 H5 109.6 . . ? C5 C6 C7 109.2(3) . . ? C5 C6 H6A 109.8 . . ? C7 C6 H6A 109.8 . . ? C5 C6 H6B 109.8 . . ? C7 C6 H6B 109.8 . . ? H6A C6 H6B 108.3 . . ? C11 C7 C6 109.7(4) . . ? C11 C7 C8 109.4(3) . . ? C6 C7 C8 109.8(4) . . ? C11 C7 H7 109.3 . . ? C6 C7 H7 109.3 . . ? C8 C7 H7 109.3 . . ? C7 C8 C3 109.7(3) . . ? C7 C8 H8A 109.7 . . ? C3 C8 H8A 109.7 . . ? C7 C8 H8B 109.7 . . ? C3 C8 H8B 109.7 . . ? H8A C8 H8B 108.2 . . ? C5 C9 C10 111.0(3) . . ? C5 C9 H9A 109.4 . . ? C10 C9 H9A 109.4 . . ? C5 C9 H9B 109.4 . . ? C10 C9 H9B 109.4 . . ? H9A C9 H9B 108.0 . . ? C13 C10 C11 111.6(4) . . ? C13 C10 C12 112.7(3) . . ? C11 C10 C12 108.6(3) . . ? C13 C10 C9 107.3(3) . . ? C11 C10 C9 108.2(3) . . ? C12 C10 C9 108.3(3) . . ? C7 C11 C10 110.3(3) . . ? C7 C11 H11A 109.6 . . ? C10 C11 H11A 109.6 . . ? C7 C11 H11B 109.6 . . ? C10 C11 H11B 109.6 . . ? H11A C11 H11B 108.1 . . ? C3 C12 C10 111.1(3) . . ? C3 C12 H12A 109.4 . . ? C10 C12 H12A 109.4 . . ? C3 C12 H12B 109.4 . . ? C10 C12 H12B 109.4 . . ? H12A C12 H12B 108.0 . . ? C14 C13 C10 119.6(4) . . ? C14 C13 H13A 107.4 . . ? C10 C13 H13A 107.4 . . ? C14 C13 H13B 107.4 . . ? C10 C13 H13B 107.4 . . ? H13A C13 H13B 106.9 . . ? O3 C14 O4 122.1(5) . . ? O3 C14 C13 127.4(4) . . ? O4 C14 C13 110.5(4) . . ? N1 C15 C16 122.8(4) . . ? N1 C15 H15 118.6 . . ? C16 C15 H15 118.6 . . ? C15 C16 C17 120.4(4) . . ? C15 C16 H16 119.8 . . ? C17 C16 H16 119.8 . . ? C16 C17 C18 116.0(3) . . ? C16 C17 C17 122.7(4) . 5_575 ? C18 C17 C17 121.3(4) . 5_575 ? C19 C18 C17 120.3(4) . . ? C19 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? N1 C19 C18 123.6(4) . . ? N1 C19 H19 118.2 . . ? C18 C19 H19 118.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Cd1 N1 C19 38.0(3) 2 . . . ? O1 Cd1 N1 C19 175.8(3) 2 . . . ? O1 Cd1 N1 C19 -71.8(4) . . . . ? O2 Cd1 N1 C19 -70.0(3) . . . . ? O2 Cd1 N1 C19 120.6(3) 2 . . . ? C1 Cd1 N1 C19 148.8(3) 2 . . . ? N1 Cd1 N1 C15 -146.5(4) 2 . . . ? O1 Cd1 N1 C15 -8.7(3) 2 . . . ? O1 Cd1 N1 C15 103.7(3) . . . . ? O2 Cd1 N1 C15 105.4(3) . . . . ? O2 Cd1 N1 C15 -63.9(3) 2 . . . ? C1 Cd1 N1 C15 -35.7(3) 2 . . . ? N1 Cd1 O1 C1 -102.8(4) 2 . . . ? N1 Cd1 O1 C1 3.9(4) . . . . ? O1 Cd1 O1 C1 117.9(4) 2 . . . ? O2 Cd1 O1 C1 1.7(3) . . . . ? O2 Cd1 O1 C1 170.8(3) 2 . . . ? C1 Cd1 O1 C1 142.6(3) 2 . . . ? N1 Cd1 O2 C1 89.2(4) 2 . . . ? N1 Cd1 O2 C1 179.9(4) . . . . ? O1 Cd1 O2 C1 -81.2(4) 2 . . . ? O1 Cd1 O2 C1 -1.7(3) . . . . ? O2 Cd1 O2 C1 -44.2(4) 2 . . . ? C1 Cd1 O2 C1 -74.6(6) 2 . . . ? Cd1 O1 C1 O2 -2.9(6) . . . . ? Cd1 O1 C1 C2 -177.7(5) . . . . ? Cd1 O2 C1 O1 2.9(6) . . . . ? Cd1 O2 C1 C2 178.0(4) . . . . ? O1 C1 C2 C3 -32.1(8) . . . . ? O2 C1 C2 C3 153.1(5) . . . . ? C1 C2 C3 C12 -51.7(5) . . . . ? C1 C2 C3 C4 -170.9(4) . . . . ? C1 C2 C3 C8 70.4(5) . . . . ? C12 C3 C4 C5 58.4(4) . . . . ? C8 C3 C4 C5 -60.2(4) . . . . ? C2 C3 C4 C5 178.6(3) . . . . ? C3 C4 C5 C9 -58.9(5) . . . . ? C3 C4 C5 C6 61.0(4) . . . . ? C9 C5 C6 C7 59.8(5) . . . . ? C4 C5 C6 C7 -60.1(5) . . . . ? C5 C6 C7 C11 -60.1(5) . . . . ? C5 C6 C7 C8 60.2(5) . . . . ? C11 C7 C8 C3 60.3(4) . . . . ? C6 C7 C8 C3 -60.1(4) . . . . ? C12 C3 C8 C7 -59.3(4) . . . . ? C4 C3 C8 C7 59.3(4) . . . . ? C2 C3 C8 C7 177.6(3) . . . . ? C6 C5 C9 C10 -60.1(4) . . . . ? C4 C5 C9 C10 59.5(5) . . . . ? C5 C9 C10 C13 179.3(4) . . . . ? C5 C9 C10 C11 58.8(4) . . . . ? C5 C9 C10 C12 -58.8(4) . . . . ? C6 C7 C11 C10 60.1(4) . . . . ? C8 C7 C11 C10 -60.4(4) . . . . ? C13 C10 C11 C7 -176.3(3) . . . . ? C12 C10 C11 C7 58.8(4) . . . . ? C9 C10 C11 C7 -58.5(4) . . . . ? C4 C3 C12 C10 -59.0(4) . . . . ? C8 C3 C12 C10 59.1(4) . . . . ? C2 C3 C12 C10 -177.1(3) . . . . ? C13 C10 C12 C3 177.2(3) . . . . ? C11 C10 C12 C3 -58.6(4) . . . . ? C9 C10 C12 C3 58.7(4) . . . . ? C11 C10 C13 C14 -61.2(5) . . . . ? C12 C10 C13 C14 61.4(5) . . . . ? C9 C10 C13 C14 -179.6(4) . . . . ? C10 C13 C14 O3 -26.0(8) . . . . ? C10 C13 C14 O4 154.0(5) . . . . ? C19 N1 C15 C16 -0.2(6) . . . . ? Cd1 N1 C15 C16 -175.8(3) . . . . ? N1 C15 C16 C17 -0.9(6) . . . . ? C15 C16 C17 C18 1.0(6) . . . . ? C15 C16 C17 C17 -178.7(4) . . . 5_575 ? C16 C17 C18 C19 -0.1(6) . . . . ? C17 C17 C18 C19 179.7(4) 5_575 . . . ? C15 N1 C19 C18 1.2(6) . . . . ? Cd1 N1 C19 C18 177.0(4) . . . . ? C17 C18 C19 N1 -1.1(7) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O4 H4 O2 0.82 1.86 2.661(6) 164.5 6_566 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.810 _refine_diff_density_min -0.782 _refine_diff_density_rms 0.092 data_7 _database_code_depnum_ccdc_archive 'CCDC 761117' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C67 H84 Cd3 N4 O14' _chemical_formula_sum 'C67 H84 Cd3 N4 O14' _chemical_formula_weight 1506.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.0525(7) _cell_length_b 13.6256(8) _cell_length_c 22.0015(13) _cell_angle_alpha 94.6770(10) _cell_angle_beta 103.5900(10) _cell_angle_gamma 114.4180(10) _cell_volume 3132.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 3100 _cell_measurement_theta_min 2.278 _cell_measurement_theta_max 22.490 _exptl_crystal_description colorless _exptl_crystal_colour block _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.598 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1540 _exptl_absorpt_coefficient_mu 1.079 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8378 _exptl_absorpt_correction_T_max 0.8636 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15883 _diffrn_reflns_av_R_equivalents 0.0240 _diffrn_reflns_av_sigmaI/netI 0.0603 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 25.10 _reflns_number_total 10969 _reflns_number_gt 7679 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0549P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10969 _refine_ls_number_parameters 794 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0621 _refine_ls_R_factor_gt 0.0408 _refine_ls_wR_factor_ref 0.1070 _refine_ls_wR_factor_gt 0.1010 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.027 _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 0.83860(3) 0.58644(3) 0.552759(16) 0.03006(10) Uani 1 1 d . . . Cd2 Cd 0.98124(3) 0.68314(3) 0.778678(16) 0.03087(10) Uani 1 1 d . . . Cd3 Cd 0.18067(4) 0.77122(3) 1.002988(18) 0.04486(12) Uani 1 1 d . . . N1 N 0.6848(3) 0.4253(3) 0.57098(18) 0.0350(9) Uani 1 1 d . . . N2 N -0.0079(4) -0.2459(3) 0.5390(2) 0.0435(10) Uani 1 1 d . . . N3 N 0.7975(4) 0.5268(3) 0.78159(18) 0.0357(9) Uani 1 1 d . . . N4 N 0.1624(4) -0.1609(3) 0.77679(18) 0.0344(9) Uani 1 1 d . . . O1 O 0.9900(3) 0.5372(3) 0.59962(15) 0.0546(10) Uani 1 1 d . . . H1WA H 1.0364 0.5260 0.5824 0.066 Uiso 1 1 d R . . H1WB H 1.0137 0.5476 0.6377 0.066 Uiso 1 1 d R . . O2 O 0.7476(3) 0.6884(3) 0.58797(15) 0.0363(8) Uani 1 1 d . . . O3 O 0.8784(3) 0.6761(2) 0.67174(14) 0.0337(7) Uani 1 1 d . . . O4 O 0.3086(3) 0.4609(3) 0.55195(15) 0.0436(8) Uani 1 1 d . . . O5 O 0.1471(3) 0.4992(3) 0.54231(14) 0.0395(8) Uani 1 1 d . . . O6 O 0.9260(3) 0.7933(3) 0.83224(16) 0.0472(9) Uani 1 1 d . . . O7 O 1.0357(4) 0.7616(3) 0.91452(17) 0.0587(11) Uani 1 1 d . . . O8 O 0.3533(4) 0.8506(3) 0.97090(19) 0.0592(10) Uani 1 1 d . . . O9 O 0.3982(4) 0.7782(4) 1.05348(18) 0.0649(11) Uani 1 1 d . . . O10 O 0.1115(4) 0.5927(3) 0.95221(16) 0.0564(10) Uani 1 1 d . . . H10 H 0.1102 0.5973 0.9160 0.068 Uiso 1 1 d R . . O11 O 0.1112(4) 0.7115(3) 1.08786(17) 0.0585(10) Uani 1 1 d U . . O12 O 0.2050(4) 0.8878(3) 1.0946(2) 0.0755(12) Uani 1 1 d U . . O13 O -0.1068(3) 0.3921(3) 1.16887(14) 0.0383(8) Uani 1 1 d . . . O14 O -0.0711(3) 0.4277(3) 1.27125(15) 0.0447(9) Uani 1 1 d . . . C1 C 0.8018(4) 0.7133(3) 0.6474(2) 0.0306(11) Uani 1 1 d . . . C2 C 0.7824(4) 0.7929(4) 0.6897(2) 0.0375(12) Uani 1 1 d . . . H2A H 0.8459 0.8663 0.6908 0.045 Uiso 1 1 calc R . . H2B H 0.8010 0.7792 0.7326 0.045 Uiso 1 1 calc R . . C3 C 0.6527(4) 0.7942(3) 0.6739(2) 0.0299(10) Uani 1 1 d . . . C4 C 0.5425(4) 0.6792(4) 0.6633(2) 0.0319(11) Uani 1 1 d . . . H4A H 0.5579 0.6469 0.7002 0.038 Uiso 1 1 calc R . . H4B H 0.5390 0.6327 0.6264 0.038 Uiso 1 1 calc R . . C5 C 0.4138(4) 0.6833(4) 0.6528(2) 0.0319(11) Uani 1 1 d . . . C6 C 0.4221(5) 0.7581(4) 0.7124(2) 0.0438(13) Uani 1 1 d . . . H6A H 0.3416 0.7615 0.7069 0.053 Uiso 1 1 calc R . . H6B H 0.4379 0.7270 0.7498 0.053 Uiso 1 1 calc R . . C7 C 0.5287(5) 0.8733(4) 0.7224(2) 0.0434(13) Uani 1 1 d . . . H7 H 0.5329 0.9196 0.7602 0.052 Uiso 1 1 calc R . . C8 C 0.6557(4) 0.8676(4) 0.7318(2) 0.0376(12) Uani 1 1 d . . . H8A H 0.6737 0.8386 0.7698 0.045 Uiso 1 1 calc R . . H8B H 0.7237 0.9412 0.7381 0.045 Uiso 1 1 calc R . . C9 C 0.6254(4) 0.8449(4) 0.6145(2) 0.0358(11) Uani 1 1 d . . . H9A H 0.6940 0.9181 0.6204 0.043 Uiso 1 1 calc R . . H9B H 0.6213 0.7999 0.5768 0.043 Uiso 1 1 calc R . . C10 C 0.5040(5) 0.9237(4) 0.6628(3) 0.0507(14) Uani 1 1 d . . . H10A H 0.4238 0.9281 0.6560 0.061 Uiso 1 1 calc R . . H10B H 0.5717 0.9974 0.6693 0.061 Uiso 1 1 calc R . . C11 C 0.4992(4) 0.8514(4) 0.6053(2) 0.0392(12) Uani 1 1 d . . . H11 H 0.4827 0.8825 0.5675 0.047 Uiso 1 1 calc R . . C12 C 0.3916(4) 0.7361(4) 0.5952(2) 0.0375(11) Uani 1 1 d . . . H12A H 0.3863 0.6907 0.5573 0.045 Uiso 1 1 calc R . . H12B H 0.3112 0.7401 0.5886 0.045 Uiso 1 1 calc R . . C13 C 0.3060(4) 0.5670(4) 0.6439(2) 0.0378(12) Uani 1 1 d . . . H13A H 0.3387 0.5260 0.6706 0.045 Uiso 1 1 calc R . . H13B H 0.2384 0.5729 0.6584 0.045 Uiso 1 1 calc R . . C14 C 0.2498(4) 0.5031(4) 0.5752(2) 0.0324(11) Uani 1 1 d . . . C15 C 0.9648(4) 0.8020(4) 0.8909(2) 0.0358(11) Uani 1 1 d . . . C16 C 0.9185(4) 0.8611(4) 0.9332(2) 0.0418(12) Uani 1 1 d . . . H16A H 0.9147 0.9230 0.9155 0.050 Uiso 1 1 calc R . . H16B H 0.9806 0.8903 0.9752 0.050 Uiso 1 1 calc R . . C17 C 0.7864(4) 0.7883(4) 0.9407(2) 0.0343(11) Uani 1 1 d . . . C18 C 0.7945(5) 0.7078(5) 0.9846(3) 0.0522(14) Uani 1 1 d . . . H18A H 0.8234 0.6590 0.9662 0.063 Uiso 1 1 calc R . . H18B H 0.8555 0.7484 1.0259 0.063 Uiso 1 1 calc R . . C19 C 0.6625(6) 0.6401(5) 0.9927(3) 0.0676(19) Uani 1 1 d . . . H19 H 0.6694 0.5895 1.0209 0.081 Uiso 1 1 calc R . . C20 C 0.5690(7) 0.5746(5) 0.9305(4) 0.083(2) Uani 1 1 d . . . H20A H 0.4866 0.5308 0.9363 0.100 Uiso 1 1 calc R . . H20B H 0.5968 0.5252 0.9118 0.100 Uiso 1 1 calc R . . C21 C 0.5577(5) 0.6522(5) 0.8865(3) 0.0603(17) Uani 1 1 d . . . H21 H 0.4960 0.6093 0.8451 0.072 Uiso 1 1 calc R . . C22 C 0.6879(4) 0.7215(4) 0.8770(2) 0.0475(13) Uani 1 1 d . . . H22A H 0.7160 0.6734 0.8572 0.057 Uiso 1 1 calc R . . H22B H 0.6798 0.7708 0.8487 0.057 Uiso 1 1 calc R . . C23 C 0.7392(4) 0.8620(4) 0.9711(2) 0.0408(12) Uani 1 1 d . . . H23A H 0.7348 0.9143 0.9444 0.049 Uiso 1 1 calc R . . H23B H 0.8001 0.9033 1.0124 0.049 Uiso 1 1 calc R . . C24 C 0.5124(5) 0.7302(4) 0.9154(2) 0.0460(13) Uani 1 1 d . . . H24A H 0.5055 0.7796 0.8870 0.055 Uiso 1 1 calc R . . H24B H 0.4288 0.6878 0.9204 0.055 Uiso 1 1 calc R . . C25 C 0.6068(4) 0.7967(4) 0.9802(2) 0.0364(11) Uani 1 1 d . . . C26 C 0.6182(5) 0.7165(5) 1.0236(3) 0.0539(15) Uani 1 1 d . . . H26A H 0.6790 0.7573 1.0650 0.065 Uiso 1 1 calc R . . H26B H 0.5361 0.6733 1.0300 0.065 Uiso 1 1 calc R . . C27 C 0.5680(5) 0.8785(4) 1.0091(3) 0.0531(15) Uani 1 1 d . . . H27A H 0.5805 0.9358 0.9843 0.064 Uiso 1 1 calc R . . H27B H 0.6253 0.9128 1.0520 0.064 Uiso 1 1 calc R . . C28 C 0.4306(5) 0.8314(4) 1.0126(3) 0.0467(13) Uani 1 1 d . . . C29 C 0.1628(6) 0.8075(5) 1.1195(3) 0.0519(12) Uani 1 1 d U . . C30 C 0.1849(5) 0.8269(4) 1.1919(2) 0.0464(13) Uani 1 1 d . . . H30A H 0.2352 0.7904 1.2099 0.056 Uiso 1 1 calc R . . H30B H 0.2362 0.9052 1.2088 0.056 Uiso 1 1 calc R . . C31 C 0.0684(4) 0.7892(4) 1.2159(2) 0.0389(12) Uani 1 1 d . . . C32 C -0.0088(4) 0.6632(4) 1.1994(2) 0.0370(11) Uani 1 1 d . . . H32A H -0.0406 0.6388 1.1534 0.044 Uiso 1 1 calc R . . H32B H 0.0468 0.6304 1.2159 0.044 Uiso 1 1 calc R . . C33 C -0.1209(4) 0.6237(4) 1.2271(2) 0.0330(11) Uani 1 1 d . . . C34 C -0.0716(5) 0.6633(4) 1.2994(2) 0.0441(13) Uani 1 1 d . . . H34A H -0.0162 0.6313 1.3177 0.053 Uiso 1 1 calc R . . H34B H -0.1428 0.6391 1.3170 0.053 Uiso 1 1 calc R . . C35 C 0.0021(5) 0.7887(4) 1.3169(2) 0.0503(14) Uani 1 1 d . . . H35 H 0.0338 0.8130 1.3635 0.060 Uiso 1 1 calc R . . C36 C 0.1153(5) 0.8244(4) 1.2888(2) 0.0448(13) Uani 1 1 d . . . H36A H 0.1651 0.9037 1.3007 0.054 Uiso 1 1 calc R . . H36B H 0.1701 0.7914 1.3063 0.054 Uiso 1 1 calc R . . C37 C -0.0846(6) 0.8398(4) 1.2886(3) 0.0573(16) Uani 1 1 d . . . H37A H -0.1566 0.8171 1.3057 0.069 Uiso 1 1 calc R . . H37B H -0.0378 0.9194 1.3001 0.069 Uiso 1 1 calc R . . C38 C -0.1314(5) 0.8038(4) 1.2174(3) 0.0475(13) Uani 1 1 d . . . H38 H -0.1875 0.8365 1.1997 0.057 Uiso 1 1 calc R . . C39 C -0.2071(5) 0.6779(4) 1.1993(3) 0.0457(13) Uani 1 1 d . . . H39A H -0.2387 0.6546 1.1532 0.055 Uiso 1 1 calc R . . H39B H -0.2798 0.6543 1.2159 0.055 Uiso 1 1 calc R . . C40 C -0.0200(5) 0.8407(4) 1.1893(2) 0.0443(13) Uani 1 1 d . . . H40A H 0.0273 0.9203 1.2000 0.053 Uiso 1 1 calc R . . H40B H -0.0519 0.8182 1.1431 0.053 Uiso 1 1 calc R . . C41 C -0.1999(4) 0.4985(3) 1.2073(2) 0.0329(11) Uani 1 1 d . . . H41A H -0.2605 0.4750 1.2317 0.040 Uiso 1 1 calc R . . H41B H -0.2482 0.4801 1.1626 0.040 Uiso 1 1 calc R . . C42 C -0.1220(4) 0.4350(4) 1.2170(2) 0.0327(11) Uani 1 1 d . . . C43 C 0.7063(5) 0.3412(4) 0.5887(2) 0.0454(13) Uani 1 1 d . . . H43 H 0.7891 0.3485 0.5980 0.055 Uiso 1 1 calc R . . C44 C 0.6120(5) 0.2455(4) 0.5935(3) 0.0532(15) Uani 1 1 d . . . H44 H 0.6317 0.1896 0.6060 0.064 Uiso 1 1 calc R . . C45 C 0.4873(4) 0.2304(4) 0.5802(2) 0.0408(12) Uani 1 1 d . . . C46 C 0.4655(4) 0.3184(4) 0.5621(2) 0.0433(13) Uani 1 1 d . . . H46 H 0.3836 0.3131 0.5528 0.052 Uiso 1 1 calc R . . C47 C 0.5640(4) 0.4119(4) 0.5581(2) 0.0376(12) Uani 1 1 d . . . H47 H 0.5470 0.4692 0.5459 0.045 Uiso 1 1 calc R . . C48 C 0.3809(5) 0.1263(4) 0.5855(3) 0.0572(16) Uani 1 1 d . . . H48A H 0.4177 0.0845 0.6092 0.069 Uiso 1 1 calc R . . H48B H 0.3326 0.1456 0.6097 0.069 Uiso 1 1 calc R . . C49 C 0.2917(6) 0.0550(5) 0.5225(3) 0.0709(19) Uani 1 1 d . . . H49A H 0.3403 0.0368 0.4980 0.085 Uiso 1 1 calc R . . H49B H 0.2540 0.0964 0.4991 0.085 Uiso 1 1 calc R . . C50 C 0.1862(5) -0.0503(5) 0.5276(3) 0.0510(15) Uani 1 1 d . . . C51 C 0.1819(5) -0.1507(5) 0.5092(3) 0.0571(15) Uani 1 1 d . . . H51 H 0.2439 -0.1551 0.4923 0.069 Uiso 1 1 calc R . . C52 C 0.0863(5) -0.2439(4) 0.5157(3) 0.0512(14) Uani 1 1 d . . . H52 H 0.0864 -0.3107 0.5031 0.061 Uiso 1 1 calc R . . C53 C -0.0040(5) -0.1495(4) 0.5561(3) 0.0523(14) Uani 1 1 d . . . H53 H -0.0678 -0.1468 0.5721 0.063 Uiso 1 1 calc R . . C54 C 0.0924(6) -0.0505(5) 0.5512(3) 0.0621(17) Uani 1 1 d . . . H54 H 0.0917 0.0158 0.5644 0.075 Uiso 1 1 calc R . . C55 C 0.8010(5) 0.4778(4) 0.8323(2) 0.0421(12) Uani 1 1 d . . . H55 H 0.8773 0.5059 0.8651 0.051 Uiso 1 1 calc R . . C56 C 0.6991(5) 0.3894(4) 0.8381(2) 0.0408(12) Uani 1 1 d . . . H56 H 0.7076 0.3590 0.8742 0.049 Uiso 1 1 calc R . . C57 C 0.5829(4) 0.3442(4) 0.7911(2) 0.0339(11) Uani 1 1 d . . . C58 C 0.5778(5) 0.3956(4) 0.7398(2) 0.0468(13) Uani 1 1 d . . . H58 H 0.5016 0.3702 0.7071 0.056 Uiso 1 1 calc R . . C59 C 0.6857(5) 0.4852(4) 0.7365(2) 0.0475(13) Uani 1 1 d . . . H59 H 0.6794 0.5177 0.7011 0.057 Uiso 1 1 calc R . . C60 C 0.4715(4) 0.2432(4) 0.7949(3) 0.0418(12) Uani 1 1 d . . . H60A H 0.3949 0.2344 0.7635 0.050 Uiso 1 1 calc R . . H60B H 0.4599 0.2525 0.8368 0.050 Uiso 1 1 calc R . . C61 C 0.4898(4) 0.1397(4) 0.7833(3) 0.0430(13) Uani 1 1 d . . . H61A H 0.5085 0.1342 0.7430 0.052 Uiso 1 1 calc R . . H61B H 0.5629 0.1467 0.8167 0.052 Uiso 1 1 calc R . . C62 C 0.3750(4) 0.0350(4) 0.7818(2) 0.0362(11) Uani 1 1 d . . . C63 C 0.3752(5) -0.0250(4) 0.8293(2) 0.0438(13) Uani 1 1 d . . . H63 H 0.4478 -0.0009 0.8641 0.053 Uiso 1 1 calc R . . C64 C 0.2686(5) -0.1203(4) 0.8255(2) 0.0454(13) Uani 1 1 d . . . H64 H 0.2711 -0.1581 0.8587 0.054 Uiso 1 1 calc R . . C65 C 0.1628(5) -0.1049(4) 0.7302(3) 0.0460(13) Uani 1 1 d . . . H65 H 0.0900 -0.1323 0.6953 0.055 Uiso 1 1 calc R . . C66 C 0.2639(5) -0.0094(4) 0.7304(2) 0.0465(14) Uani 1 1 d . . . H66 H 0.2586 0.0260 0.6962 0.056 Uiso 1 1 calc R . . C67 C 0.1548(7) 0.5235(5) 0.9788(3) 0.074(2) Uani 1 1 d . . . H67A H 0.2455 0.5543 0.9867 0.111 Uiso 1 1 calc R . . H67B H 0.1146 0.4535 0.9500 0.111 Uiso 1 1 calc R . . H67C H 0.1348 0.5141 1.0183 0.111 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.02450(18) 0.02538(19) 0.0381(2) 0.00485(15) 0.01350(14) 0.00711(15) Cd2 0.02735(19) 0.02422(18) 0.0415(2) 0.00972(15) 0.01566(15) 0.00847(15) Cd3 0.0443(2) 0.0548(3) 0.0443(2) 0.01496(19) 0.02092(18) 0.0253(2) N1 0.029(2) 0.031(2) 0.041(2) 0.0076(18) 0.0125(18) 0.0097(19) N2 0.036(2) 0.031(2) 0.057(3) 0.012(2) 0.017(2) 0.007(2) N3 0.030(2) 0.030(2) 0.044(2) 0.0095(19) 0.0159(19) 0.0075(19) N4 0.033(2) 0.026(2) 0.041(2) 0.0075(18) 0.0158(19) 0.0072(18) O1 0.052(2) 0.100(3) 0.0323(19) 0.0101(19) 0.0142(17) 0.053(2) O2 0.0350(19) 0.0411(19) 0.0344(19) 0.0023(15) 0.0096(15) 0.0197(16) O3 0.0315(18) 0.0315(18) 0.0390(19) 0.0065(14) 0.0113(14) 0.0145(16) O4 0.042(2) 0.045(2) 0.048(2) 0.0022(17) 0.0155(17) 0.0229(18) O5 0.0296(19) 0.050(2) 0.0334(18) -0.0019(16) 0.0062(15) 0.0166(17) O6 0.045(2) 0.065(2) 0.039(2) 0.0063(18) 0.0148(17) 0.031(2) O7 0.064(3) 0.083(3) 0.052(2) 0.016(2) 0.020(2) 0.053(2) O8 0.050(2) 0.069(3) 0.078(3) 0.032(2) 0.034(2) 0.033(2) O9 0.055(3) 0.096(3) 0.059(3) 0.033(2) 0.031(2) 0.037(2) O10 0.075(3) 0.062(3) 0.040(2) 0.0162(19) 0.0179(19) 0.036(2) O11 0.067(2) 0.052(2) 0.052(2) 0.0091(17) 0.0310(19) 0.0157(19) O12 0.109(3) 0.053(2) 0.075(3) 0.021(2) 0.055(2) 0.030(2) O13 0.049(2) 0.0388(19) 0.0351(19) 0.0059(15) 0.0163(16) 0.0253(17) O14 0.059(2) 0.053(2) 0.033(2) 0.0097(16) 0.0120(17) 0.036(2) C1 0.015(2) 0.023(2) 0.045(3) 0.008(2) 0.011(2) 0.000(2) C2 0.030(3) 0.039(3) 0.041(3) 0.000(2) 0.005(2) 0.018(2) C3 0.031(3) 0.029(2) 0.030(3) 0.004(2) 0.009(2) 0.014(2) C4 0.031(3) 0.034(3) 0.032(3) 0.005(2) 0.009(2) 0.017(2) C5 0.029(3) 0.036(3) 0.035(3) 0.006(2) 0.011(2) 0.016(2) C6 0.049(3) 0.045(3) 0.046(3) 0.010(2) 0.023(3) 0.023(3) C7 0.048(3) 0.037(3) 0.049(3) 0.001(2) 0.022(3) 0.020(3) C8 0.041(3) 0.032(3) 0.034(3) -0.002(2) 0.014(2) 0.012(2) C9 0.036(3) 0.030(3) 0.036(3) 0.006(2) 0.009(2) 0.011(2) C10 0.050(3) 0.036(3) 0.073(4) 0.011(3) 0.016(3) 0.026(3) C11 0.040(3) 0.043(3) 0.040(3) 0.015(2) 0.009(2) 0.024(3) C12 0.029(3) 0.044(3) 0.042(3) 0.013(2) 0.011(2) 0.017(2) C13 0.028(3) 0.047(3) 0.038(3) 0.010(2) 0.013(2) 0.014(2) C14 0.027(3) 0.027(3) 0.039(3) 0.009(2) 0.016(2) 0.004(2) C15 0.028(3) 0.034(3) 0.046(3) 0.009(2) 0.016(2) 0.012(2) C16 0.030(3) 0.038(3) 0.051(3) -0.001(2) 0.016(2) 0.010(2) C17 0.032(3) 0.037(3) 0.034(3) 0.002(2) 0.014(2) 0.013(2) C18 0.054(4) 0.070(4) 0.058(4) 0.031(3) 0.030(3) 0.041(3) C19 0.083(5) 0.071(4) 0.102(5) 0.059(4) 0.060(4) 0.060(4) C20 0.089(5) 0.037(4) 0.141(7) 0.024(4) 0.085(5) 0.017(4) C21 0.036(3) 0.062(4) 0.056(4) -0.023(3) 0.012(3) 0.005(3) C22 0.038(3) 0.058(4) 0.039(3) -0.001(3) 0.015(2) 0.014(3) C23 0.034(3) 0.035(3) 0.051(3) 0.006(2) 0.018(2) 0.012(2) C24 0.033(3) 0.057(3) 0.041(3) 0.008(3) 0.013(2) 0.014(3) C25 0.033(3) 0.035(3) 0.043(3) 0.008(2) 0.016(2) 0.014(2) C26 0.059(4) 0.071(4) 0.056(4) 0.033(3) 0.038(3) 0.038(3) C27 0.042(3) 0.042(3) 0.076(4) 0.003(3) 0.032(3) 0.013(3) C28 0.040(3) 0.046(3) 0.056(4) 0.002(3) 0.022(3) 0.019(3) C29 0.065(3) 0.048(2) 0.060(3) 0.017(2) 0.041(2) 0.029(2) C30 0.039(3) 0.041(3) 0.053(3) 0.001(3) 0.021(3) 0.009(3) C31 0.036(3) 0.038(3) 0.041(3) 0.007(2) 0.017(2) 0.012(2) C32 0.038(3) 0.035(3) 0.037(3) 0.007(2) 0.010(2) 0.016(2) C33 0.033(3) 0.031(3) 0.036(3) 0.004(2) 0.012(2) 0.015(2) C34 0.054(3) 0.040(3) 0.043(3) 0.010(2) 0.024(3) 0.019(3) C35 0.063(4) 0.041(3) 0.039(3) 0.001(2) 0.019(3) 0.015(3) C36 0.035(3) 0.035(3) 0.048(3) -0.003(2) 0.004(2) 0.007(2) C37 0.066(4) 0.044(3) 0.070(4) 0.005(3) 0.041(3) 0.022(3) C38 0.048(3) 0.045(3) 0.067(4) 0.026(3) 0.026(3) 0.029(3) C39 0.041(3) 0.043(3) 0.062(4) 0.016(3) 0.020(3) 0.023(3) C40 0.046(3) 0.035(3) 0.050(3) 0.009(2) 0.016(3) 0.015(3) C41 0.025(2) 0.036(3) 0.038(3) 0.008(2) 0.012(2) 0.013(2) C42 0.029(3) 0.027(3) 0.043(3) 0.010(2) 0.015(2) 0.010(2) C43 0.029(3) 0.040(3) 0.066(4) 0.020(3) 0.012(2) 0.013(3) C44 0.044(3) 0.039(3) 0.075(4) 0.023(3) 0.012(3) 0.018(3) C45 0.031(3) 0.035(3) 0.042(3) 0.017(2) 0.008(2) 0.002(2) C46 0.024(3) 0.045(3) 0.054(3) 0.015(3) 0.011(2) 0.008(2) C47 0.029(3) 0.032(3) 0.048(3) 0.015(2) 0.008(2) 0.011(2) C48 0.049(3) 0.044(3) 0.061(4) 0.022(3) 0.011(3) 0.005(3) C49 0.061(4) 0.058(4) 0.066(4) 0.019(3) 0.022(3) -0.001(3) C50 0.037(3) 0.049(4) 0.047(3) 0.017(3) 0.011(3) -0.001(3) C51 0.042(3) 0.053(4) 0.070(4) 0.019(3) 0.027(3) 0.008(3) C52 0.040(3) 0.039(3) 0.072(4) 0.012(3) 0.027(3) 0.009(3) C53 0.044(3) 0.043(3) 0.069(4) 0.020(3) 0.026(3) 0.013(3) C54 0.067(4) 0.038(3) 0.069(4) 0.015(3) 0.016(3) 0.014(3) C55 0.038(3) 0.038(3) 0.046(3) 0.013(2) 0.014(2) 0.011(2) C56 0.038(3) 0.035(3) 0.043(3) 0.011(2) 0.010(2) 0.010(2) C57 0.034(3) 0.026(3) 0.041(3) 0.006(2) 0.015(2) 0.011(2) C58 0.033(3) 0.044(3) 0.048(3) 0.011(3) 0.007(2) 0.006(3) C59 0.042(3) 0.044(3) 0.048(3) 0.016(3) 0.013(3) 0.010(3) C60 0.032(3) 0.030(3) 0.060(3) 0.011(2) 0.020(2) 0.008(2) C61 0.030(3) 0.036(3) 0.062(3) 0.008(3) 0.019(2) 0.011(2) C62 0.029(3) 0.031(3) 0.049(3) 0.005(2) 0.019(2) 0.011(2) C63 0.035(3) 0.040(3) 0.042(3) 0.004(2) 0.007(2) 0.007(2) C64 0.048(3) 0.042(3) 0.039(3) 0.011(2) 0.015(3) 0.010(3) C65 0.025(3) 0.044(3) 0.057(3) 0.020(3) 0.007(2) 0.005(2) C66 0.034(3) 0.049(3) 0.056(3) 0.032(3) 0.016(3) 0.013(3) C67 0.098(5) 0.063(4) 0.056(4) 0.008(3) 0.001(4) 0.042(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 O1 2.255(3) . ? Cd1 O2 2.283(3) . ? Cd1 N1 2.354(4) . ? Cd1 N2 2.369(4) 1_665 ? Cd1 O5 2.388(3) 2_666 ? Cd1 O4 2.400(3) 2_666 ? Cd1 O3 2.642(3) . ? Cd1 C14 2.739(5) 2_666 ? Cd2 O6 2.234(3) . ? Cd2 O13 2.309(3) 2_667 ? Cd2 N4 2.347(4) 1_665 ? Cd2 O3 2.362(3) . ? Cd2 N3 2.373(4) . ? Cd2 O14 2.510(3) 2_667 ? Cd3 O8 2.225(4) . ? Cd3 O7 2.242(4) 1_455 ? Cd3 O11 2.295(4) . ? Cd3 O10 2.302(4) . ? Cd3 O12 2.342(4) . ? Cd3 O9 2.554(4) . ? N1 C43 1.343(6) . ? N1 C47 1.345(5) . ? N2 C53 1.316(6) . ? N2 C52 1.343(6) . ? N2 Cd1 2.369(4) 1_445 ? N3 C59 1.330(6) . ? N3 C55 1.348(6) . ? N4 C65 1.327(6) . ? N4 C64 1.329(6) . ? N4 Cd2 2.347(4) 1_445 ? O1 H1WA 0.8000 . ? O1 H1WB 0.7999 . ? O2 C1 1.264(5) . ? O3 C1 1.262(5) . ? O4 C14 1.247(5) . ? O4 Cd1 2.400(3) 2_666 ? O5 C14 1.255(5) . ? O5 Cd1 2.388(3) 2_666 ? O6 C15 1.242(5) . ? O7 C15 1.238(5) . ? O7 Cd3 2.242(4) 1_655 ? O8 C28 1.271(6) . ? O9 C28 1.234(6) . ? O10 C67 1.363(6) . ? O10 H10 0.8000 . ? O11 C29 1.248(6) . ? O12 C29 1.236(6) . ? O13 C42 1.255(5) . ? O13 Cd2 2.309(3) 2_667 ? O14 C42 1.240(5) . ? O14 Cd2 2.510(3) 2_667 ? C1 C2 1.498(6) . ? C2 C3 1.527(6) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.533(6) . ? C3 C8 1.537(6) . ? C3 C9 1.558(6) . ? C4 C5 1.539(6) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C12 1.531(6) . ? C5 C13 1.537(6) . ? C5 C6 1.550(6) . ? C6 C7 1.518(7) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.531(6) . ? C7 C10 1.553(7) . ? C7 H7 0.9800 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C11 1.527(6) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.513(7) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.524(6) . ? C11 H11 0.9800 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.524(6) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 Cd1 2.739(5) 2_666 ? C15 C16 1.523(6) . ? C16 C17 1.546(6) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C23 1.523(6) . ? C17 C22 1.524(6) . ? C17 C18 1.537(7) . ? C18 C19 1.536(8) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.479(9) . ? C19 C26 1.532(8) . ? C19 H19 0.9800 . ? C20 C21 1.515(9) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.536(7) . ? C21 C24 1.537(7) . ? C21 H21 0.9800 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C25 1.543(6) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.524(6) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C27 1.522(7) . ? C25 C26 1.536(7) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.534(7) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C29 C30 1.532(7) . ? C30 C31 1.521(6) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C36 1.530(6) . ? C31 C32 1.537(6) . ? C31 C40 1.538(7) . ? C32 C33 1.526(6) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.524(6) . ? C33 C41 1.532(6) . ? C33 C39 1.551(6) . ? C34 C35 1.528(7) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C37 1.527(7) . ? C35 C36 1.543(7) . ? C35 H35 0.9800 . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 C38 1.498(7) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 C40 1.523(7) . ? C38 C39 1.535(7) . ? C38 H38 0.9800 . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 C42 1.511(6) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C43 C44 1.363(7) . ? C43 H43 0.9300 . ? C44 C45 1.384(7) . ? C44 H44 0.9300 . ? C45 C46 1.397(7) . ? C45 C48 1.505(7) . ? C46 C47 1.363(6) . ? C46 H46 0.9300 . ? C47 H47 0.9300 . ? C48 C49 1.497(7) . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C49 C50 1.507(7) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 C54 1.350(8) . ? C50 C51 1.371(8) . ? C51 C52 1.363(7) . ? C51 H51 0.9300 . ? C52 H52 0.9300 . ? C53 C54 1.402(7) . ? C53 H53 0.9300 . ? C54 H54 0.9300 . ? C55 C56 1.361(7) . ? C55 H55 0.9300 . ? C56 C57 1.383(6) . ? C56 H56 0.9300 . ? C57 C58 1.379(6) . ? C57 C60 1.500(6) . ? C58 C59 1.390(7) . ? C58 H58 0.9300 . ? C59 H59 0.9300 . ? C60 C61 1.524(6) . ? C60 H60A 0.9700 . ? C60 H60B 0.9700 . ? C61 C62 1.513(6) . ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? C62 C63 1.379(7) . ? C62 C66 1.394(7) . ? C63 C64 1.377(7) . ? C63 H63 0.9300 . ? C64 H64 0.9300 . ? C65 C66 1.364(6) . ? C65 H65 0.9300 . ? C66 H66 0.9300 . ? C67 H67A 0.9600 . ? C67 H67B 0.9600 . ? C67 H67C 0.9600 . ? 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 O2 134.78(11) . . ? O1 Cd1 N1 88.61(13) . . ? O2 Cd1 N1 91.09(12) . . ? O1 Cd1 N2 92.20(14) . 1_665 ? O2 Cd1 N2 86.21(13) . 1_665 ? N1 Cd1 N2 176.90(14) . 1_665 ? O1 Cd1 O5 82.45(11) . 2_666 ? O2 Cd1 O5 142.34(11) . 2_666 ? N1 Cd1 O5 96.10(12) . 2_666 ? N2 Cd1 O5 86.98(13) 1_665 2_666 ? O1 Cd1 O4 135.20(11) . 2_666 ? O2 Cd1 O4 89.76(11) . 2_666 ? N1 Cd1 O4 85.45(12) . 2_666 ? N2 Cd1 O4 96.06(13) 1_665 2_666 ? O5 Cd1 O4 54.27(10) 2_666 2_666 ? O1 Cd1 O3 82.61(10) . . ? O2 Cd1 O3 52.26(10) . . ? N1 Cd1 O3 86.56(11) . . ? N2 Cd1 O3 90.57(12) 1_665 . ? O5 Cd1 O3 164.76(10) 2_666 . ? O4 Cd1 O3 140.97(10) 2_666 . ? O1 Cd1 C14 108.80(13) . 2_666 ? O2 Cd1 C14 116.42(13) . 2_666 ? N1 Cd1 C14 89.71(13) . 2_666 ? N2 Cd1 C14 92.86(14) 1_665 2_666 ? O5 Cd1 C14 27.26(11) 2_666 2_666 ? O4 Cd1 C14 27.06(12) 2_666 2_666 ? O3 Cd1 C14 167.93(12) . 2_666 ? O6 Cd2 O13 121.43(12) . 2_667 ? O6 Cd2 N4 88.83(13) . 1_665 ? O13 Cd2 N4 91.13(12) 2_667 1_665 ? O6 Cd2 O3 101.75(11) . . ? O13 Cd2 O3 136.81(10) 2_667 . ? N4 Cd2 O3 90.36(12) 1_665 . ? O6 Cd2 N3 90.41(13) . . ? O13 Cd2 N3 89.14(13) 2_667 . ? N4 Cd2 N3 179.23(13) 1_665 . ? O3 Cd2 N3 89.94(12) . . ? O6 Cd2 O14 172.66(12) . 2_667 ? O13 Cd2 O14 53.20(10) 2_667 2_667 ? N4 Cd2 O14 86.37(12) 1_665 2_667 ? O3 Cd2 O14 83.85(10) . 2_667 ? N3 Cd2 O14 94.36(12) . 2_667 ? O8 Cd3 O7 97.88(14) . 1_455 ? O8 Cd3 O11 143.94(14) . . ? O7 Cd3 O11 118.09(14) 1_455 . ? O8 Cd3 O10 98.36(14) . . ? O7 Cd3 O10 79.82(13) 1_455 . ? O11 Cd3 O10 90.96(13) . . ? O8 Cd3 O12 108.05(15) . . ? O7 Cd3 O12 115.32(15) 1_455 . ? O11 Cd3 O12 55.67(13) . . ? O10 Cd3 O12 146.59(14) . . ? O8 Cd3 O9 54.26(13) . . ? O7 Cd3 O9 148.08(13) 1_455 . ? O11 Cd3 O9 91.53(13) . . ? O10 Cd3 O9 88.60(13) . . ? O12 Cd3 O9 90.49(15) . . ? C43 N1 C47 116.9(4) . . ? C43 N1 Cd1 124.7(3) . . ? C47 N1 Cd1 118.2(3) . . ? C53 N2 C52 115.5(4) . . ? C53 N2 Cd1 123.7(4) . 1_445 ? C52 N2 Cd1 120.7(3) . 1_445 ? C59 N3 C55 116.0(4) . . ? C59 N3 Cd2 123.9(3) . . ? C55 N3 Cd2 120.1(3) . . ? C65 N4 C64 116.6(4) . . ? C65 N4 Cd2 122.8(3) . 1_445 ? C64 N4 Cd2 120.5(3) . 1_445 ? Cd1 O1 H1WA 124.5 . . ? Cd1 O1 H1WB 118.7 . . ? H1WA O1 H1WB 114.5 . . ? C1 O2 Cd1 102.0(3) . . ? C1 O3 Cd2 132.2(3) . . ? C1 O3 Cd1 85.1(3) . . ? Cd2 O3 Cd1 142.38(13) . . ? C14 O4 Cd1 91.8(3) . 2_666 ? C14 O5 Cd1 92.1(3) . 2_666 ? C15 O6 Cd2 111.8(3) . . ? C15 O7 Cd3 144.6(3) . 1_655 ? C28 O8 Cd3 98.7(3) . . ? C28 O9 Cd3 84.3(3) . . ? C67 O10 Cd3 122.5(3) . . ? C67 O10 H10 118.2 . . ? Cd3 O10 H10 104.0 . . ? C29 O11 Cd3 91.8(3) . . ? C29 O12 Cd3 89.9(3) . . ? C42 O13 Cd2 97.7(3) . 2_667 ? C42 O14 Cd2 88.6(3) . 2_667 ? O3 C1 O2 120.5(4) . . ? O3 C1 C2 118.8(4) . . ? O2 C1 C2 120.5(4) . . ? C1 C2 C3 119.2(4) . . ? C1 C2 H2A 107.5 . . ? C3 C2 H2A 107.5 . . ? C1 C2 H2B 107.5 . . ? C3 C2 H2B 107.5 . . ? H2A C2 H2B 107.0 . . ? C2 C3 C4 112.3(4) . . ? C2 C3 C8 106.4(3) . . ? C4 C3 C8 108.8(4) . . ? C2 C3 C9 113.4(4) . . ? C4 C3 C9 108.4(3) . . ? C8 C3 C9 107.3(4) . . ? C3 C4 C5 111.6(4) . . ? C3 C4 H4A 109.3 . . ? C5 C4 H4A 109.3 . . ? C3 C4 H4B 109.3 . . ? C5 C4 H4B 109.3 . . ? H4A C4 H4B 108.0 . . ? C12 C5 C13 112.1(4) . . ? C12 C5 C4 108.8(4) . . ? C13 C5 C4 110.2(4) . . ? C12 C5 C6 107.9(4) . . ? C13 C5 C6 109.6(4) . . ? C4 C5 C6 108.2(4) . . ? C7 C6 C5 110.5(4) . . ? C7 C6 H6A 109.5 . . ? C5 C6 H6A 109.5 . . ? C7 C6 H6B 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 108.1 . . ? C6 C7 C8 109.4(4) . . ? C6 C7 C10 109.9(4) . . ? C8 C7 C10 108.5(4) . . ? C6 C7 H7 109.7 . . ? C8 C7 H7 109.7 . . ? C10 C7 H7 109.7 . . ? C7 C8 C3 111.4(4) . . ? C7 C8 H8A 109.3 . . ? C3 C8 H8A 109.3 . . ? C7 C8 H8B 109.3 . . ? C3 C8 H8B 109.3 . . ? H8A C8 H8B 108.0 . . ? C11 C9 C3 109.9(4) . . ? C11 C9 H9A 109.7 . . ? C3 C9 H9A 109.7 . . ? C11 C9 H9B 109.7 . . ? C3 C9 H9B 109.7 . . ? H9A C9 H9B 108.2 . . ? C11 C10 C7 108.7(4) . . ? C11 C10 H10A 109.9 . . ? C7 C10 H10A 109.9 . . ? C11 C10 H10B 109.9 . . ? C7 C10 H10B 109.9 . . ? H10A C10 H10B 108.3 . . ? C10 C11 C12 109.5(4) . . ? C10 C11 C9 110.9(4) . . ? C12 C11 C9 109.4(4) . . ? C10 C11 H11 109.0 . . ? C12 C11 H11 109.0 . . ? C9 C11 H11 109.0 . . ? C11 C12 C5 111.1(4) . . ? C11 C12 H12A 109.4 . . ? C5 C12 H12A 109.4 . . ? C11 C12 H12B 109.4 . . ? C5 C12 H12B 109.4 . . ? H12A C12 H12B 108.0 . . ? C14 C13 C5 113.7(4) . . ? C14 C13 H13A 108.8 . . ? C5 C13 H13A 108.8 . . ? C14 C13 H13B 108.8 . . ? C5 C13 H13B 108.8 . . ? H13A C13 H13B 107.7 . . ? O4 C14 O5 121.6(4) . . ? O4 C14 C13 120.1(4) . . ? O5 C14 C13 118.2(4) . . ? O4 C14 Cd1 61.2(2) . 2_666 ? O5 C14 Cd1 60.6(2) . 2_666 ? C13 C14 Cd1 172.7(3) . 2_666 ? O7 C15 O6 121.7(4) . . ? O7 C15 C16 120.6(5) . . ? O6 C15 C16 117.7(4) . . ? C15 C16 C17 114.6(4) . . ? C15 C16 H16A 108.6 . . ? C17 C16 H16A 108.6 . . ? C15 C16 H16B 108.6 . . ? C17 C16 H16B 108.6 . . ? H16A C16 H16B 107.6 . . ? C23 C17 C22 108.4(4) . . ? C23 C17 C18 107.8(4) . . ? C22 C17 C18 108.0(4) . . ? C23 C17 C16 108.9(4) . . ? C22 C17 C16 112.3(4) . . ? C18 C17 C16 111.3(4) . . ? C19 C18 C17 109.6(4) . . ? C19 C18 H18A 109.8 . . ? C17 C18 H18A 109.8 . . ? C19 C18 H18B 109.8 . . ? C17 C18 H18B 109.8 . . ? H18A C18 H18B 108.2 . . ? C20 C19 C26 110.6(5) . . ? C20 C19 C18 110.7(5) . . ? C26 C19 C18 110.0(5) . . ? C20 C19 H19 108.5 . . ? C26 C19 H19 108.5 . . ? C18 C19 H19 108.5 . . ? C19 C20 C21 108.9(5) . . ? C19 C20 H20A 109.9 . . ? C21 C20 H20A 109.9 . . ? C19 C20 H20B 109.9 . . ? C21 C20 H20B 109.9 . . ? H20A C20 H20B 108.3 . . ? C20 C21 C22 110.0(5) . . ? C20 C21 C24 110.2(5) . . ? C22 C21 C24 108.7(4) . . ? C20 C21 H21 109.3 . . ? C22 C21 H21 109.3 . . ? C24 C21 H21 109.3 . . ? C17 C22 C21 110.6(4) . . ? C17 C22 H22A 109.5 . . ? C21 C22 H22A 109.5 . . ? C17 C22 H22B 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 108.1 . . ? C17 C23 C25 112.8(4) . . ? C17 C23 H23A 109.0 . . ? C25 C23 H23A 109.0 . . ? C17 C23 H23B 109.0 . . ? C25 C23 H23B 109.0 . . ? H23A C23 H23B 107.8 . . ? C25 C24 C21 109.9(4) . . ? C25 C24 H24A 109.7 . . ? C21 C24 H24A 109.7 . . ? C25 C24 H24B 109.7 . . ? C21 C24 H24B 109.7 . . ? H24A C24 H24B 108.2 . . ? C27 C25 C24 111.4(4) . . ? C27 C25 C26 112.5(4) . . ? C24 C25 C26 108.6(4) . . ? C27 C25 C23 108.2(4) . . ? C24 C25 C23 108.6(4) . . ? C26 C25 C23 107.5(4) . . ? C19 C26 C25 109.4(4) . . ? C19 C26 H26A 109.8 . . ? C25 C26 H26A 109.8 . . ? C19 C26 H26B 109.8 . . ? C25 C26 H26B 109.8 . . ? H26A C26 H26B 108.2 . . ? C25 C27 C28 116.2(4) . . ? C25 C27 H27A 108.2 . . ? C28 C27 H27A 108.2 . . ? C25 C27 H27B 108.2 . . ? C28 C27 H27B 108.2 . . ? H27A C27 H27B 107.4 . . ? O9 C28 O8 122.7(5) . . ? O9 C28 C27 121.5(5) . . ? O8 C28 C27 115.7(5) . . ? O12 C29 O11 121.3(5) . . ? O12 C29 C30 118.7(5) . . ? O11 C29 C30 119.7(5) . . ? C31 C30 C29 117.9(4) . . ? C31 C30 H30A 107.8 . . ? C29 C30 H30A 107.8 . . ? C31 C30 H30B 107.8 . . ? C29 C30 H30B 107.8 . . ? H30A C30 H30B 107.2 . . ? C30 C31 C36 107.8(4) . . ? C30 C31 C32 111.5(4) . . ? C36 C31 C32 107.6(4) . . ? C30 C31 C40 112.4(4) . . ? C36 C31 C40 108.6(4) . . ? C32 C31 C40 108.9(4) . . ? C33 C32 C31 112.1(4) . . ? C33 C32 H32A 109.2 . . ? C31 C32 H32A 109.2 . . ? C33 C32 H32B 109.2 . . ? C31 C32 H32B 109.2 . . ? H32A C32 H32B 107.9 . . ? C34 C33 C32 109.4(4) . . ? C34 C33 C41 112.4(4) . . ? C32 C33 C41 111.0(4) . . ? C34 C33 C39 108.2(4) . . ? C32 C33 C39 107.3(4) . . ? C41 C33 C39 108.4(4) . . ? C33 C34 C35 110.7(4) . . ? C33 C34 H34A 109.5 . . ? C35 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? C35 C34 H34B 109.5 . . ? H34A C34 H34B 108.1 . . ? C37 C35 C34 109.9(5) . . ? C37 C35 C36 109.3(4) . . ? C34 C35 C36 108.2(4) . . ? C37 C35 H35 109.8 . . ? C34 C35 H35 109.8 . . ? C36 C35 H35 109.8 . . ? C31 C36 C35 110.9(4) . . ? C31 C36 H36A 109.5 . . ? C35 C36 H36A 109.5 . . ? C31 C36 H36B 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 108.0 . . ? C38 C37 C35 109.7(4) . . ? C38 C37 H37A 109.7 . . ? C35 C37 H37A 109.7 . . ? C38 C37 H37B 109.7 . . ? C35 C37 H37B 109.7 . . ? H37A C37 H37B 108.2 . . ? C37 C38 C40 110.7(5) . . ? C37 C38 C39 109.6(4) . . ? C40 C38 C39 109.4(4) . . ? C37 C38 H38 109.0 . . ? C40 C38 H38 109.0 . . ? C39 C38 H38 109.0 . . ? C38 C39 C33 110.3(4) . . ? C38 C39 H39A 109.6 . . ? C33 C39 H39A 109.6 . . ? C38 C39 H39B 109.6 . . ? C33 C39 H39B 109.6 . . ? H39A C39 H39B 108.1 . . ? C38 C40 C31 109.8(4) . . ? C38 C40 H40A 109.7 . . ? C31 C40 H40A 109.7 . . ? C38 C40 H40B 109.7 . . ? C31 C40 H40B 109.7 . . ? H40A C40 H40B 108.2 . . ? C42 C41 C33 114.3(4) . . ? C42 C41 H41A 108.7 . . ? C33 C41 H41A 108.7 . . ? C42 C41 H41B 108.7 . . ? C33 C41 H41B 108.7 . . ? H41A C41 H41B 107.6 . . ? O14 C42 O13 120.4(4) . . ? O14 C42 C41 121.1(4) . . ? O13 C42 C41 118.5(4) . . ? N1 C43 C44 122.8(5) . . ? N1 C43 H43 118.6 . . ? C44 C43 H43 118.6 . . ? C43 C44 C45 120.9(5) . . ? C43 C44 H44 119.5 . . ? C45 C44 H44 119.5 . . ? C44 C45 C46 116.1(4) . . ? C44 C45 C48 122.3(5) . . ? C46 C45 C48 121.5(5) . . ? C47 C46 C45 120.1(5) . . ? C47 C46 H46 119.9 . . ? C45 C46 H46 119.9 . . ? N1 C47 C46 123.2(4) . . ? N1 C47 H47 118.4 . . ? C46 C47 H47 118.4 . . ? C49 C48 C45 113.8(5) . . ? C49 C48 H48A 108.8 . . ? C45 C48 H48A 108.8 . . ? C49 C48 H48B 108.8 . . ? C45 C48 H48B 108.8 . . ? H48A C48 H48B 107.7 . . ? C48 C49 C50 114.0(5) . . ? C48 C49 H49A 108.7 . . ? C50 C49 H49A 108.7 . . ? C48 C49 H49B 108.7 . . ? C50 C49 H49B 108.7 . . ? H49A C49 H49B 107.6 . . ? C54 C50 C51 116.7(5) . . ? C54 C50 C49 121.9(6) . . ? C51 C50 C49 121.4(6) . . ? C52 C51 C50 119.7(5) . . ? C52 C51 H51 120.1 . . ? C50 C51 H51 120.1 . . ? N2 C52 C51 124.5(5) . . ? N2 C52 H52 117.7 . . ? C51 C52 H52 117.7 . . ? N2 C53 C54 122.8(5) . . ? N2 C53 H53 118.6 . . ? C54 C53 H53 118.6 . . ? C50 C54 C53 120.7(6) . . ? C50 C54 H54 119.6 . . ? C53 C54 H54 119.6 . . ? N3 C55 C56 123.5(5) . . ? N3 C55 H55 118.2 . . ? C56 C55 H55 118.2 . . ? C55 C56 C57 121.0(5) . . ? C55 C56 H56 119.5 . . ? C57 C56 H56 119.5 . . ? C58 C57 C56 115.8(4) . . ? C58 C57 C60 122.4(4) . . ? C56 C57 C60 121.8(4) . . ? C57 C58 C59 120.4(5) . . ? C57 C58 H58 119.8 . . ? C59 C58 H58 119.8 . . ? N3 C59 C58 123.3(5) . . ? N3 C59 H59 118.4 . . ? C58 C59 H59 118.4 . . ? C57 C60 C61 112.2(4) . . ? C57 C60 H60A 109.2 . . ? C61 C60 H60A 109.2 . . ? C57 C60 H60B 109.2 . . ? C61 C60 H60B 109.2 . . ? H60A C60 H60B 107.9 . . ? C62 C61 C60 113.6(4) . . ? C62 C61 H61A 108.8 . . ? C60 C61 H61A 108.8 . . ? C62 C61 H61B 108.8 . . ? C60 C61 H61B 108.8 . . ? H61A C61 H61B 107.7 . . ? C63 C62 C66 115.8(4) . . ? C63 C62 C61 122.5(4) . . ? C66 C62 C61 121.7(4) . . ? C64 C63 C62 120.3(5) . . ? C64 C63 H63 119.8 . . ? C62 C63 H63 119.8 . . ? N4 C64 C63 123.3(5) . . ? N4 C64 H64 118.3 . . ? C63 C64 H64 118.3 . . ? N4 C65 C66 123.9(5) . . ? N4 C65 H65 118.0 . . ? C66 C65 H65 118.1 . . ? C65 C66 C62 120.1(5) . . ? C65 C66 H66 120.0 . . ? C62 C66 H66 120.0 . . ? O10 C67 H67A 109.5 . . ? O10 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? O10 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Cd1 N1 C43 -12.9(4) . . . . ? O2 Cd1 N1 C43 -147.6(4) . . . . ? N2 Cd1 N1 C43 -118(2) 1_665 . . . ? O5 Cd1 N1 C43 69.4(4) 2_666 . . . ? O4 Cd1 N1 C43 122.7(4) 2_666 . . . ? O3 Cd1 N1 C43 -95.5(4) . . . . ? C14 Cd1 N1 C43 96.0(4) 2_666 . . . ? O1 Cd1 N1 C47 172.6(3) . . . . ? O2 Cd1 N1 C47 37.8(3) . . . . ? N2 Cd1 N1 C47 67(3) 1_665 . . . ? O5 Cd1 N1 C47 -105.1(3) 2_666 . . . ? O4 Cd1 N1 C47 -51.8(3) 2_666 . . . ? O3 Cd1 N1 C47 89.9(3) . . . . ? C14 Cd1 N1 C47 -78.6(3) 2_666 . . . ? O6 Cd2 N3 C59 90.8(4) . . . . ? O13 Cd2 N3 C59 -147.7(4) 2_667 . . . ? N4 Cd2 N3 C59 102(11) 1_665 . . . ? O3 Cd2 N3 C59 -10.9(4) . . . . ? O14 Cd2 N3 C59 -94.7(4) 2_667 . . . ? O6 Cd2 N3 C55 -86.2(4) . . . . ? O13 Cd2 N3 C55 35.3(4) 2_667 . . . ? N4 Cd2 N3 C55 -75(11) 1_665 . . . ? O3 Cd2 N3 C55 172.1(4) . . . . ? O14 Cd2 N3 C55 88.2(4) 2_667 . . . ? O1 Cd1 O2 C1 -2.4(3) . . . . ? N1 Cd1 O2 C1 86.8(3) . . . . ? N2 Cd1 O2 C1 -91.7(3) 1_665 . . . ? O5 Cd1 O2 C1 -171.8(2) 2_666 . . . ? O4 Cd1 O2 C1 172.2(3) 2_666 . . . ? O3 Cd1 O2 C1 2.0(2) . . . . ? C14 Cd1 O2 C1 177.0(3) 2_666 . . . ? O6 Cd2 O3 C1 -6.1(4) . . . . ? O13 Cd2 O3 C1 173.0(3) 2_667 . . . ? N4 Cd2 O3 C1 -95.0(4) 1_665 . . . ? N3 Cd2 O3 C1 84.3(4) . . . . ? O14 Cd2 O3 C1 178.7(4) 2_667 . . . ? O6 Cd2 O3 Cd1 -178.2(2) . . . . ? O13 Cd2 O3 Cd1 0.9(3) 2_667 . . . ? N4 Cd2 O3 Cd1 92.9(2) 1_665 . . . ? N3 Cd2 O3 Cd1 -87.8(2) . . . . ? O14 Cd2 O3 Cd1 6.6(2) 2_667 . . . ? O1 Cd1 O3 C1 175.0(3) . . . . ? O2 Cd1 O3 C1 -1.9(2) . . . . ? N1 Cd1 O3 C1 -96.0(2) . . . . ? N2 Cd1 O3 C1 82.8(3) 1_665 . . . ? O5 Cd1 O3 C1 163.4(4) 2_666 . . . ? O4 Cd1 O3 C1 -17.5(3) 2_666 . . . ? C14 Cd1 O3 C1 -23.7(6) 2_666 . . . ? O1 Cd1 O3 Cd2 -10.9(2) . . . . ? O2 Cd1 O3 Cd2 172.2(3) . . . . ? N1 Cd1 O3 Cd2 78.1(2) . . . . ? N2 Cd1 O3 Cd2 -103.0(2) 1_665 . . . ? O5 Cd1 O3 Cd2 -22.5(5) 2_666 . . . ? O4 Cd1 O3 Cd2 156.58(18) 2_666 . . . ? C14 Cd1 O3 Cd2 150.4(5) 2_666 . . . ? O13 Cd2 O6 C15 -3.6(4) 2_667 . . . ? N4 Cd2 O6 C15 -94.2(3) 1_665 . . . ? O3 Cd2 O6 C15 175.7(3) . . . . ? N3 Cd2 O6 C15 85.6(3) . . . . ? O14 Cd2 O6 C15 -45.0(11) 2_667 . . . ? O7 Cd3 O8 C28 -164.3(3) 1_455 . . . ? O11 Cd3 O8 C28 19.9(4) . . . . ? O10 Cd3 O8 C28 -83.5(3) . . . . ? O12 Cd3 O8 C28 75.8(3) . . . . ? O9 Cd3 O8 C28 -1.3(3) . . . . ? O8 Cd3 O9 C28 1.3(3) . . . . ? O7 Cd3 O9 C28 34.6(5) 1_455 . . . ? O11 Cd3 O9 C28 -166.4(3) . . . . ? O10 Cd3 O9 C28 102.7(3) . . . . ? O12 Cd3 O9 C28 -110.7(3) . . . . ? O8 Cd3 O10 C67 86.3(5) . . . . ? O7 Cd3 O10 C67 -177.2(5) 1_455 . . . ? O11 Cd3 O10 C67 -58.8(5) . . . . ? O12 Cd3 O10 C67 -56.1(6) . . . . ? O9 Cd3 O10 C67 32.7(5) . . . . ? O8 Cd3 O11 C29 66.2(4) . . . . ? O7 Cd3 O11 C29 -109.2(3) 1_455 . . . ? O10 Cd3 O11 C29 171.9(3) . . . . ? O12 Cd3 O11 C29 -6.3(3) . . . . ? O9 Cd3 O11 C29 83.2(3) . . . . ? O8 Cd3 O12 C29 -137.4(4) . . . . ? O7 Cd3 O12 C29 114.3(4) 1_455 . . . ? O11 Cd3 O12 C29 6.4(3) . . . . ? O10 Cd3 O12 C29 3.1(5) . . . . ? O9 Cd3 O12 C29 -85.1(4) . . . . ? Cd2 O3 C1 O2 -172.0(3) . . . . ? Cd1 O3 C1 O2 3.2(4) . . . . ? Cd2 O3 C1 C2 11.8(6) . . . . ? Cd1 O3 C1 C2 -173.1(4) . . . . ? Cd1 O2 C1 O3 -3.8(5) . . . . ? Cd1 O2 C1 C2 172.4(3) . . . . ? O3 C1 C2 C3 -148.8(4) . . . . ? O2 C1 C2 C3 34.9(6) . . . . ? C1 C2 C3 C4 50.9(6) . . . . ? C1 C2 C3 C8 169.8(4) . . . . ? C1 C2 C3 C9 -72.5(5) . . . . ? C2 C3 C4 C5 175.4(4) . . . . ? C8 C3 C4 C5 57.9(5) . . . . ? C9 C3 C4 C5 -58.5(5) . . . . ? C3 C4 C5 C12 58.1(5) . . . . ? C3 C4 C5 C13 -178.7(4) . . . . ? C3 C4 C5 C6 -58.9(5) . . . . ? C12 C5 C6 C7 -58.1(5) . . . . ? C13 C5 C6 C7 179.6(4) . . . . ? C4 C5 C6 C7 59.5(5) . . . . ? C5 C6 C7 C8 -59.7(5) . . . . ? C5 C6 C7 C10 59.3(5) . . . . ? C6 C7 C8 C3 58.9(5) . . . . ? C10 C7 C8 C3 -61.0(5) . . . . ? C2 C3 C8 C7 -178.6(4) . . . . ? C4 C3 C8 C7 -57.4(5) . . . . ? C9 C3 C8 C7 59.7(5) . . . . ? C2 C3 C9 C11 -175.5(4) . . . . ? C4 C3 C9 C11 59.0(5) . . . . ? C8 C3 C9 C11 -58.3(5) . . . . ? C6 C7 C10 C11 -60.0(5) . . . . ? C8 C7 C10 C11 59.6(5) . . . . ? C7 C10 C11 C12 60.2(5) . . . . ? C7 C10 C11 C9 -60.6(5) . . . . ? C3 C9 C11 C10 60.8(5) . . . . ? C3 C9 C11 C12 -60.1(5) . . . . ? C10 C11 C12 C5 -61.5(5) . . . . ? C9 C11 C12 C5 60.2(5) . . . . ? C13 C5 C12 C11 179.7(4) . . . . ? C4 C5 C12 C11 -58.2(5) . . . . ? C6 C5 C12 C11 58.9(5) . . . . ? C12 C5 C13 C14 34.5(5) . . . . ? C4 C5 C13 C14 -86.7(5) . . . . ? C6 C5 C13 C14 154.3(4) . . . . ? Cd1 O4 C14 O5 4.6(5) 2_666 . . . ? Cd1 O4 C14 C13 -171.7(4) 2_666 . . . ? Cd1 O5 C14 O4 -4.6(5) 2_666 . . . ? Cd1 O5 C14 C13 171.8(3) 2_666 . . . ? C5 C13 C14 O4 77.1(5) . . . . ? C5 C13 C14 O5 -99.4(5) . . . . ? C5 C13 C14 Cd1 -21(3) . . . 2_666 ? Cd3 O7 C15 O6 157.1(4) 1_655 . . . ? Cd3 O7 C15 C16 -25.1(9) 1_655 . . . ? Cd2 O6 C15 O7 6.4(6) . . . . ? Cd2 O6 C15 C16 -171.4(3) . . . . ? O7 C15 C16 C17 -94.7(6) . . . . ? O6 C15 C16 C17 83.2(6) . . . . ? C15 C16 C17 C23 -167.5(4) . . . . ? C15 C16 C17 C22 -47.4(6) . . . . ? C15 C16 C17 C18 73.8(5) . . . . ? C23 C17 C18 C19 58.7(6) . . . . ? C22 C17 C18 C19 -58.3(6) . . . . ? C16 C17 C18 C19 178.0(4) . . . . ? C17 C18 C19 C20 61.3(6) . . . . ? C17 C18 C19 C26 -61.2(6) . . . . ? C26 C19 C20 C21 61.1(6) . . . . ? C18 C19 C20 C21 -61.0(6) . . . . ? C19 C20 C21 C22 59.7(6) . . . . ? C19 C20 C21 C24 -60.1(6) . . . . ? C23 C17 C22 C21 -58.5(6) . . . . ? C18 C17 C22 C21 58.0(6) . . . . ? C16 C17 C22 C21 -178.9(4) . . . . ? C20 C21 C22 C17 -59.3(6) . . . . ? C24 C21 C22 C17 61.4(6) . . . . ? C22 C17 C23 C25 57.0(5) . . . . ? C18 C17 C23 C25 -59.7(5) . . . . ? C16 C17 C23 C25 179.5(4) . . . . ? C20 C21 C24 C25 59.3(6) . . . . ? C22 C21 C24 C25 -61.3(6) . . . . ? C21 C24 C25 C27 177.6(4) . . . . ? C21 C24 C25 C26 -58.0(5) . . . . ? C21 C24 C25 C23 58.5(5) . . . . ? C17 C23 C25 C27 -178.5(4) . . . . ? C17 C23 C25 C24 -57.5(5) . . . . ? C17 C23 C25 C26 59.8(5) . . . . ? C20 C19 C26 C25 -61.2(6) . . . . ? C18 C19 C26 C25 61.4(6) . . . . ? C27 C25 C26 C19 -177.8(5) . . . . ? C24 C25 C26 C19 58.5(6) . . . . ? C23 C25 C26 C19 -58.7(6) . . . . ? C24 C25 C27 C28 51.9(7) . . . . ? C26 C25 C27 C28 -70.3(6) . . . . ? C23 C25 C27 C28 171.1(5) . . . . ? Cd3 O9 C28 O8 -2.3(5) . . . . ? Cd3 O9 C28 C27 177.9(5) . . . . ? Cd3 O8 C28 O9 2.6(6) . . . . ? Cd3 O8 C28 C27 -177.6(4) . . . . ? C25 C27 C28 O9 76.5(7) . . . . ? C25 C27 C28 O8 -103.3(6) . . . . ? Cd3 O12 C29 O11 -11.4(6) . . . . ? Cd3 O12 C29 C30 163.4(4) . . . . ? Cd3 O11 C29 O12 11.6(6) . . . . ? Cd3 O11 C29 C30 -163.1(4) . . . . ? O12 C29 C30 C31 119.4(6) . . . . ? O11 C29 C30 C31 -65.7(7) . . . . ? C29 C30 C31 C36 -176.3(4) . . . . ? C29 C30 C31 C32 65.8(6) . . . . ? C29 C30 C31 C40 -56.8(6) . . . . ? C30 C31 C32 C33 176.2(4) . . . . ? C36 C31 C32 C33 58.2(5) . . . . ? C40 C31 C32 C33 -59.3(5) . . . . ? C31 C32 C33 C34 -58.1(5) . . . . ? C31 C32 C33 C41 177.3(4) . . . . ? C31 C32 C33 C39 59.1(5) . . . . ? C32 C33 C34 C35 58.4(5) . . . . ? C41 C33 C34 C35 -177.8(4) . . . . ? C39 C33 C34 C35 -58.2(5) . . . . ? C33 C34 C35 C37 59.5(5) . . . . ? C33 C34 C35 C36 -59.8(5) . . . . ? C30 C31 C36 C35 -179.9(4) . . . . ? C32 C31 C36 C35 -59.6(5) . . . . ? C40 C31 C36 C35 58.1(5) . . . . ? C37 C35 C36 C31 -58.5(5) . . . . ? C34 C35 C36 C31 61.1(5) . . . . ? C34 C35 C37 C38 -59.9(6) . . . . ? C36 C35 C37 C38 58.7(6) . . . . ? C35 C37 C38 C40 -60.5(6) . . . . ? C35 C37 C38 C39 60.2(6) . . . . ? C37 C38 C39 C33 -60.3(6) . . . . ? C40 C38 C39 C33 61.3(5) . . . . ? C34 C33 C39 C38 58.5(5) . . . . ? C32 C33 C39 C38 -59.4(5) . . . . ? C41 C33 C39 C38 -179.4(4) . . . . ? C37 C38 C40 C31 60.6(5) . . . . ? C39 C38 C40 C31 -60.2(5) . . . . ? C30 C31 C40 C38 -177.5(4) . . . . ? C36 C31 C40 C38 -58.4(5) . . . . ? C32 C31 C40 C38 58.5(5) . . . . ? C34 C33 C41 C42 -74.5(5) . . . . ? C32 C33 C41 C42 48.4(5) . . . . ? C39 C33 C41 C42 166.0(4) . . . . ? Cd2 O14 C42 O13 -1.0(4) 2_667 . . . ? Cd2 O14 C42 C41 -179.0(4) 2_667 . . . ? Cd2 O13 C42 O14 1.1(5) 2_667 . . . ? Cd2 O13 C42 C41 179.2(3) 2_667 . . . ? C33 C41 C42 O14 72.3(6) . . . . ? C33 C41 C42 O13 -105.8(5) . . . . ? C47 N1 C43 C44 0.3(8) . . . . ? Cd1 N1 C43 C44 -174.3(4) . . . . ? N1 C43 C44 C45 0.0(9) . . . . ? C43 C44 C45 C46 -0.3(8) . . . . ? C43 C44 C45 C48 -179.5(5) . . . . ? C44 C45 C46 C47 0.4(8) . . . . ? C48 C45 C46 C47 179.5(5) . . . . ? C43 N1 C47 C46 -0.2(7) . . . . ? Cd1 N1 C47 C46 174.7(4) . . . . ? C45 C46 C47 N1 -0.1(8) . . . . ? C44 C45 C48 C49 -107.1(6) . . . . ? C46 C45 C48 C49 73.8(7) . . . . ? C45 C48 C49 C50 179.1(5) . . . . ? C48 C49 C50 C54 68.0(8) . . . . ? C48 C49 C50 C51 -111.2(7) . . . . ? C54 C50 C51 C52 -0.5(9) . . . . ? C49 C50 C51 C52 178.7(5) . . . . ? C53 N2 C52 C51 0.0(8) . . . . ? Cd1 N2 C52 C51 -176.7(4) 1_445 . . . ? C50 C51 C52 N2 0.6(9) . . . . ? C52 N2 C53 C54 -0.7(8) . . . . ? Cd1 N2 C53 C54 175.9(4) 1_445 . . . ? C51 C50 C54 C53 -0.2(9) . . . . ? C49 C50 C54 C53 -179.3(5) . . . . ? N2 C53 C54 C50 0.8(9) . . . . ? C59 N3 C55 C56 1.3(7) . . . . ? Cd2 N3 C55 C56 178.6(4) . . . . ? N3 C55 C56 C57 -0.3(8) . . . . ? C55 C56 C57 C58 -1.3(7) . . . . ? C55 C56 C57 C60 176.6(4) . . . . ? C56 C57 C58 C59 1.7(7) . . . . ? C60 C57 C58 C59 -176.2(5) . . . . ? C55 N3 C59 C58 -0.9(8) . . . . ? Cd2 N3 C59 C58 -178.0(4) . . . . ? C57 C58 C59 N3 -0.6(8) . . . . ? C58 C57 C60 C61 105.8(6) . . . . ? C56 C57 C60 C61 -71.9(6) . . . . ? C57 C60 C61 C62 -175.5(4) . . . . ? C60 C61 C62 C63 -110.1(6) . . . . ? C60 C61 C62 C66 72.9(6) . . . . ? C66 C62 C63 C64 -2.3(7) . . . . ? C61 C62 C63 C64 -179.5(5) . . . . ? C65 N4 C64 C63 0.3(7) . . . . ? Cd2 N4 C64 C63 -175.5(4) 1_445 . . . ? C62 C63 C64 N4 1.3(8) . . . . ? C64 N4 C65 C66 -0.9(8) . . . . ? Cd2 N4 C65 C66 174.9(4) 1_445 . . . ? N4 C65 C66 C62 -0.3(9) . . . . ? C63 C62 C66 C65 1.8(8) . . . . ? C61 C62 C66 C65 179.0(5) . . . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.834 _refine_diff_density_min -1.068 _refine_diff_density_rms 0.097 data_8 _database_code_depnum_ccdc_archive 'CCDC 761118' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H78 Cd2 N4 O15' _chemical_formula_sum 'C54 H78 Cd2 N4 O15' _chemical_formula_weight 1248.00 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 Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 13.1885(11) _cell_length_b 18.1129(15) _cell_length_c 24.841(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5934.0(9) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 4150 _cell_measurement_theta_min 2.252 _cell_measurement_theta_max 18.865 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.397 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2584 _exptl_absorpt_coefficient_mu 0.782 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8531 _exptl_absorpt_correction_T_max 0.8657 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29847 _diffrn_reflns_av_R_equivalents 0.0606 _diffrn_reflns_av_sigmaI/netI 0.0805 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 25.05 _reflns_number_total 10497 _reflns_number_gt 6921 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1107P)^2^+0.2841P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(4) _refine_ls_number_reflns 10497 _refine_ls_number_parameters 676 _refine_ls_number_restraints 89 _refine_ls_R_factor_all 0.1039 _refine_ls_R_factor_gt 0.0680 _refine_ls_wR_factor_ref 0.2027 _refine_ls_wR_factor_gt 0.1757 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.079 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _chemical_absolute_configuration ad 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 0.16726(5) 0.02061(4) 0.67544(3) 0.0559(2) Uani 1 1 d . . . N1 N 0.1088(6) -0.0559(5) 0.7445(4) 0.062(2) Uani 1 1 d . . . N2 N 0.1759(7) 0.0960(5) 0.5994(3) 0.066(2) Uani 1 1 d . . . N3 N 0.0647(8) 0.0268(5) 1.0782(3) 0.070(2) Uani 1 1 d . . . N4 N 0.0846(7) 0.1732(5) 0.2297(3) 0.059(2) Uani 1 1 d . . . O1 O 0.1588(6) 0.1335(4) 0.7245(3) 0.072(2) Uani 1 1 d . . . O2 O 0.0133(5) 0.0900(4) 0.6954(3) 0.071(2) Uani 1 1 d . . . O3 O -0.1001(8) 0.4287(5) 0.8824(3) 0.088(2) Uani 1 1 d . . . O4 O -0.2423(6) 0.3775(8) 0.8631(4) 0.128(4) Uani 1 1 d . . . O5 O 0.3352(5) 0.0021(4) 0.6950(3) 0.0643(18) Uani 1 1 d . . . O6 O 0.4993(6) -0.0038(4) 0.7035(3) 0.0680(19) Uani 1 1 d . . . O7 O 0.4225(7) 0.3464(4) 0.8677(3) 0.078(2) Uani 1 1 d . . . O8 O 0.5557(6) 0.2962(5) 0.9035(3) 0.080(2) Uani 1 1 d . . . O9 O 0.3514(19) 0.3727(11) 0.5543(8) 0.259(10) Uani 1 1 d . . . O10 O 0.2853(8) 0.4025(7) 0.6592(5) 0.146(4) Uani 1 1 d . . . O11 O 0.7421(7) 0.1419(6) 0.1832(4) 0.115(3) Uani 1 1 d . . . O12 O 0.6130(9) 0.0651(8) 0.1112(6) 0.163(5) Uani 1 1 d . . . O13 O 0.3196(7) 0.4141(8) 0.3402(5) 0.143(4) Uani 1 1 d . . . O14 O 0.7956(7) 0.0065(7) 0.2300(5) 0.127(4) Uani 1 1 d . . . O15 O 0.2482(8) 0.7251(5) 0.2206(4) 0.113(3) Uani 1 1 d . . . C1 C 0.0650(9) 0.1361(6) 0.7221(4) 0.058(3) Uani 1 1 d . . . C2 C 0.0103(9) 0.1971(6) 0.7498(4) 0.070(3) Uani 1 1 d . . . H2A H -0.0480 0.2103 0.7280 0.084 Uiso 1 1 calc R . . H2B H 0.0547 0.2397 0.7508 0.084 Uiso 1 1 calc R . . C3 C -0.0275(9) 0.1819(7) 0.8085(5) 0.075(3) Uani 1 1 d U . . C4 C -0.0576(8) 0.2526(6) 0.8339(4) 0.067(3) Uani 1 1 d U . . H4A H -0.1083 0.2767 0.8117 0.080 Uiso 1 1 calc R . . H4B H 0.0010 0.2849 0.8360 0.080 Uiso 1 1 calc R . . C5 C -0.1009(9) 0.2405(7) 0.8913(4) 0.075(3) Uani 1 1 d U . . C6 C -0.0184(14) 0.1992(10) 0.9227(7) 0.127(6) Uani 1 1 d U . . H6A H 0.0425 0.2293 0.9227 0.153 Uiso 1 1 calc R . . H6B H -0.0405 0.1945 0.9598 0.153 Uiso 1 1 calc R . . C7 C 0.0091(14) 0.1223(10) 0.9017(7) 0.115(4) Uani 1 1 d U . . H7 H 0.0579 0.0963 0.9246 0.138 Uiso 1 1 calc R . . C8 C 0.0540(12) 0.1429(9) 0.8429(6) 0.111(3) Uani 1 1 d U . . H8A H 0.1123 0.1750 0.8469 0.133 Uiso 1 1 calc R . . H8B H 0.0760 0.0982 0.8248 0.133 Uiso 1 1 calc R . . C9 C -0.1183(13) 0.1311(8) 0.8055(6) 0.117(6) Uani 1 1 d . . . H9A H -0.0972 0.0839 0.7908 0.140 Uiso 1 1 calc R . . H9B H -0.1682 0.1522 0.7812 0.140 Uiso 1 1 calc R . . C10 C -0.0769(17) 0.0842(10) 0.8937(7) 0.140(8) Uani 1 1 d . . . H10A H -0.1038 0.0716 0.9288 0.168 Uiso 1 1 calc R . . H10B H -0.0585 0.0382 0.8763 0.168 Uiso 1 1 calc R . . C11 C -0.1664(15) 0.1190(9) 0.8601(7) 0.127(6) Uani 1 1 d . . . H11 H -0.2261 0.0869 0.8585 0.153 Uiso 1 1 calc R . . C12 C -0.1873(14) 0.1919(8) 0.8892(6) 0.120(6) Uani 1 1 d . . . H12A H -0.2426 0.2171 0.8711 0.144 Uiso 1 1 calc R . . H12B H -0.2092 0.1812 0.9256 0.144 Uiso 1 1 calc R . . C13 C -0.1297(11) 0.3147(7) 0.9169(5) 0.090(3) Uani 1 1 d U . . H13A H -0.1809 0.3040 0.9438 0.108 Uiso 1 1 calc R . . H13B H -0.0702 0.3316 0.9363 0.108 Uiso 1 1 calc R . . C14 C -0.1673(11) 0.3790(7) 0.8857(4) 0.069(3) Uani 1 1 d U . . C15 C 0.4151(8) 0.0300(5) 0.7122(3) 0.052(2) Uani 1 1 d . . . C16 C 0.4120(8) 0.1003(5) 0.7446(4) 0.056(2) Uani 1 1 d . . . H16A H 0.3480 0.1250 0.7377 0.067 Uiso 1 1 calc R . . H16B H 0.4658 0.1326 0.7321 0.067 Uiso 1 1 calc R . . C17 C 0.5268(9) 0.0583(7) 0.8219(4) 0.073(3) Uani 1 1 d . . . H17A H 0.5359 0.0097 0.8062 0.088 Uiso 1 1 calc R . . H17B H 0.5806 0.0901 0.8088 0.088 Uiso 1 1 calc R . . C18 C 0.4235(7) 0.0896(5) 0.8053(4) 0.053(2) Uani 1 1 d . . . C19 C 0.4077(8) 0.1658(5) 0.8319(4) 0.061(2) Uani 1 1 d . . . H19A H 0.3416 0.1848 0.8219 0.074 Uiso 1 1 calc R . . H19B H 0.4586 0.1999 0.8187 0.074 Uiso 1 1 calc R . . C20 C 0.4150(8) 0.1610(6) 0.8941(4) 0.060(2) Uani 1 1 d . . . C21 C 0.5220(10) 0.1291(7) 0.9086(5) 0.081(4) Uani 1 1 d . . . H21A H 0.5747 0.1614 0.8951 0.097 Uiso 1 1 calc R . . H21B H 0.5292 0.1254 0.9474 0.097 Uiso 1 1 calc R . . C22 C 0.5317(12) 0.0532(8) 0.8832(5) 0.095(4) Uani 1 1 d . . . H22 H 0.5986 0.0336 0.8928 0.114 Uiso 1 1 calc R . . C23 C 0.4563(15) 0.0018(7) 0.9030(6) 0.113(6) Uani 1 1 d . . . H23A H 0.4623 -0.0030 0.9418 0.136 Uiso 1 1 calc R . . H23B H 0.4671 -0.0464 0.8871 0.136 Uiso 1 1 calc R . . C24 C 0.3329(10) 0.1072(7) 0.9121(5) 0.085(3) Uani 1 1 d . . . H24A H 0.2671 0.1255 0.9008 0.102 Uiso 1 1 calc R . . H24B H 0.3328 0.1041 0.9511 0.102 Uiso 1 1 calc R . . C25 C 0.3498(11) 0.0301(7) 0.8885(5) 0.088(4) Uani 1 1 d . . . H25 H 0.2981 -0.0041 0.9020 0.105 Uiso 1 1 calc R . . C26 C 0.3431(8) 0.0361(6) 0.8279(4) 0.067(3) Uani 1 1 d . . . H26A H 0.2761 0.0533 0.8179 0.081 Uiso 1 1 calc R . . H26B H 0.3528 -0.0124 0.8121 0.081 Uiso 1 1 calc R . . C27 C 0.3948(9) 0.2352(6) 0.9196(4) 0.072(3) Uani 1 1 d . . . H27A H 0.4045 0.2315 0.9582 0.087 Uiso 1 1 calc R . . H27B H 0.3249 0.2492 0.9131 0.087 Uiso 1 1 calc R . . C28 C 0.4665(11) 0.2958(6) 0.8966(4) 0.065(3) Uani 1 1 d . . . C29 C 0.0132(9) -0.0627(6) 0.7547(5) 0.070(3) Uani 1 1 d . . . H29 H -0.0332 -0.0357 0.7346 0.083 Uiso 1 1 calc R . . C30 C -0.0230(10) -0.1106(7) 0.7960(5) 0.081(4) Uani 1 1 d . . . H30 H -0.0921 -0.1141 0.8031 0.097 Uiso 1 1 calc R . . C31 C 0.0445(13) -0.1509(6) 0.8249(4) 0.079(4) Uani 1 1 d . . . C32 C 0.1441(9) -0.1433(6) 0.8133(5) 0.070(3) Uani 1 1 d . . . H32 H 0.1921 -0.1701 0.8326 0.085 Uiso 1 1 calc R . . C33 C 0.1743(8) -0.0970(6) 0.7736(4) 0.066(3) Uani 1 1 d . . . H33 H 0.2432 -0.0933 0.7661 0.079 Uiso 1 1 calc R . . C34 C 0.0040(14) -0.1988(8) 0.8716(4) 0.122(7) Uani 1 1 d D . . H34A H -0.0695 -0.1992 0.8705 0.146 Uiso 1 1 calc R . . H34B H 0.0274 -0.2491 0.8670 0.146 Uiso 1 1 calc R . . C35 C 0.1610(15) 0.2372(11) 0.4597(7) 0.162(5) Uani 1 1 d DU . . H35A H 0.1856 0.2857 0.4699 0.194 Uiso 1 1 calc R . . H35B H 0.2117 0.2157 0.4362 0.194 Uiso 1 1 calc R . . C36 C 0.1583(12) 0.1911(8) 0.5099(6) 0.113(5) Uani 1 1 d . . . C37 C 0.2334(11) 0.1999(8) 0.5493(6) 0.097(4) Uani 1 1 d . . . H37 H 0.2807 0.2378 0.5468 0.116 Uiso 1 1 calc R . . C38 C 0.2359(10) 0.1509(8) 0.5922(5) 0.090(4) Uani 1 1 d . . . H38 H 0.2856 0.1585 0.6181 0.107 Uiso 1 1 calc R . . C39 C 0.0991(11) 0.0884(8) 0.5605(5) 0.095(4) Uani 1 1 d . . . H39 H 0.0524 0.0502 0.5637 0.114 Uiso 1 1 calc R . . C40 C 0.0922(13) 0.1360(9) 0.5185(6) 0.122(6) Uani 1 1 d . . . H40 H 0.0389 0.1301 0.4943 0.147 Uiso 1 1 calc R . . C41 C 0.1366(11) 0.0124(7) 1.0402(5) 0.084(3) Uani 1 1 d . . . H41 H 0.2007 0.0331 1.0440 0.101 Uiso 1 1 calc R . . C42 C 0.1175(15) -0.0309(8) 0.9972(5) 0.108(5) Uani 1 1 d . . . H42 H 0.1705 -0.0420 0.9739 0.130 Uiso 1 1 calc R . . C43 C 0.0205(18) -0.0603(7) 0.9861(5) 0.112(6) Uani 1 1 d DU . . C44 C -0.0478(12) -0.0449(7) 1.0248(5) 0.093(4) Uani 1 1 d . . . H44 H -0.1130 -0.0639 1.0212 0.112 Uiso 1 1 calc R . . C45 C -0.0271(11) -0.0036(7) 1.0682(5) 0.088(4) Uani 1 1 d . . . H45 H -0.0788 0.0046 1.0930 0.105 Uiso 1 1 calc R . . C46 C -0.0139(15) -0.1013(8) 0.9369(5) 0.137(7) Uani 1 1 d DU . . H46A H -0.0857 -0.1116 0.9406 0.164 Uiso 1 1 calc R . . H46B H -0.0059 -0.0689 0.9060 0.164 Uiso 1 1 calc R . . C47 C 0.0381(14) -0.1708(8) 0.9251(5) 0.129(6) Uani 1 1 d D . . H47A H 0.0227 -0.2069 0.9527 0.155 Uiso 1 1 calc R . . H47B H 0.1109 -0.1630 0.9246 0.155 Uiso 1 1 calc R . . C48 C 0.0695(15) 0.2482(11) 0.4276(7) 0.158(5) Uani 1 1 d DU . . H48A H 0.0420 0.2001 0.4187 0.190 Uiso 1 1 calc R . . H48B H 0.0198 0.2733 0.4499 0.190 Uiso 1 1 calc R . . C49 C 0.0815(17) 0.2897(10) 0.3782(6) 0.138(5) Uani 1 1 d U . . H49A H 0.1438 0.3179 0.3813 0.165 Uiso 1 1 calc R . . H49B H 0.0264 0.3251 0.3765 0.165 Uiso 1 1 calc R . . C50 C 0.0845(9) 0.2507(5) 0.3261(4) 0.065(3) Uani 1 1 d . . . C51 C 0.1494(9) 0.2671(6) 0.2880(5) 0.071(3) Uani 1 1 d . . . H51 H 0.1962 0.3048 0.2934 0.085 Uiso 1 1 calc R . . C52 C 0.1489(8) 0.2281(7) 0.2388(5) 0.074(3) Uani 1 1 d . . . H52 H 0.1950 0.2411 0.2121 0.089 Uiso 1 1 calc R . . C53 C 0.0164(9) 0.1606(6) 0.2690(5) 0.071(3) Uani 1 1 d . . . H53 H -0.0319 0.1240 0.2634 0.086 Uiso 1 1 calc R . . C54 C 0.0137(10) 0.1991(7) 0.3181(5) 0.081(3) Uani 1 1 d . . . H54 H -0.0354 0.1891 0.3439 0.097 Uiso 1 1 calc R . . Cd2 Cd 0.41330(6) -0.10217(4) 0.65164(3) 0.0586(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0592(4) 0.0502(4) 0.0582(4) 0.0003(3) 0.0040(3) 0.0008(4) N1 0.054(5) 0.058(5) 0.075(6) 0.000(4) 0.013(4) -0.010(4) N2 0.077(5) 0.062(6) 0.060(5) -0.003(4) 0.007(5) -0.007(5) N3 0.088(7) 0.062(6) 0.059(5) 0.002(4) -0.002(5) 0.016(5) N4 0.060(5) 0.062(5) 0.055(5) -0.012(4) -0.001(4) 0.009(5) O1 0.072(5) 0.067(5) 0.076(5) -0.005(4) 0.006(4) 0.006(4) O2 0.057(4) 0.070(5) 0.085(5) -0.007(4) 0.003(4) -0.003(4) O3 0.115(7) 0.076(5) 0.073(5) -0.008(4) -0.014(5) -0.007(6) O4 0.057(5) 0.243(14) 0.085(6) -0.018(7) -0.010(5) 0.014(7) O5 0.058(4) 0.067(5) 0.068(4) -0.006(3) 0.002(3) 0.007(4) O6 0.071(5) 0.063(5) 0.070(4) -0.011(4) 0.005(4) 0.003(4) O7 0.096(5) 0.054(4) 0.086(5) 0.006(4) 0.002(5) -0.027(4) O8 0.069(5) 0.073(6) 0.097(6) 0.010(4) -0.005(4) -0.016(4) O9 0.35(2) 0.186(17) 0.244(19) -0.041(14) 0.086(19) -0.118(18) O10 0.130(8) 0.152(11) 0.155(10) 0.038(9) 0.003(8) -0.004(8) O11 0.092(6) 0.105(7) 0.146(9) 0.017(7) 0.017(6) -0.001(5) O12 0.117(8) 0.170(12) 0.202(13) -0.015(10) 0.029(9) -0.010(9) O13 0.076(5) 0.186(12) 0.166(10) -0.012(9) 0.021(6) 0.009(7) O14 0.081(6) 0.153(10) 0.148(9) 0.045(8) -0.017(6) -0.002(6) O15 0.104(6) 0.082(6) 0.153(9) -0.022(6) 0.000(6) -0.016(6) C1 0.078(8) 0.044(6) 0.051(6) 0.010(4) 0.008(5) 0.015(5) C2 0.083(7) 0.050(6) 0.077(7) 0.015(5) 0.011(6) 0.024(6) C3 0.074(4) 0.077(4) 0.073(4) 0.006(4) 0.004(4) 0.013(4) C4 0.083(4) 0.057(4) 0.059(4) 0.000(3) 0.003(4) 0.016(4) C5 0.085(4) 0.073(4) 0.069(4) 0.003(4) 0.005(4) 0.010(4) C6 0.136(7) 0.124(7) 0.122(7) 0.002(5) -0.005(5) 0.013(5) C7 0.118(5) 0.114(5) 0.113(5) 0.000(4) 0.004(4) 0.014(4) C8 0.113(5) 0.112(5) 0.108(5) 0.007(4) 0.001(4) 0.017(4) C9 0.183(16) 0.074(9) 0.093(10) -0.017(7) 0.067(10) -0.016(10) C10 0.188(18) 0.112(13) 0.121(13) 0.041(10) 0.069(13) 0.084(14) C11 0.139(13) 0.102(12) 0.140(14) 0.034(11) 0.044(12) -0.026(11) C12 0.166(16) 0.088(11) 0.105(11) -0.018(9) 0.063(11) 0.012(11) C13 0.105(4) 0.081(4) 0.084(4) 0.002(3) 0.005(4) 0.010(4) C14 0.078(4) 0.066(4) 0.064(4) 0.003(3) 0.004(4) 0.009(4) C15 0.050(5) 0.054(6) 0.051(5) 0.005(4) 0.002(5) -0.006(5) C16 0.074(6) 0.038(5) 0.056(5) 0.002(4) 0.006(5) 0.002(6) C17 0.090(8) 0.066(7) 0.063(7) 0.004(6) -0.001(6) 0.021(6) C18 0.056(5) 0.040(5) 0.063(6) 0.003(4) 0.013(5) 0.002(5) C19 0.067(6) 0.051(6) 0.066(6) 0.000(5) 0.013(5) -0.009(5) C20 0.071(6) 0.061(6) 0.050(6) 0.004(5) 0.010(5) -0.007(6) C21 0.099(9) 0.075(9) 0.068(7) -0.003(6) -0.034(6) 0.008(7) C22 0.129(11) 0.080(10) 0.077(9) 0.027(7) -0.019(8) 0.011(9) C23 0.214(19) 0.055(9) 0.072(9) 0.011(6) -0.003(10) 0.000(10) C24 0.099(8) 0.089(9) 0.069(7) -0.004(6) 0.025(7) -0.021(8) C25 0.128(11) 0.052(7) 0.083(8) -0.003(6) 0.049(8) -0.028(8) C26 0.079(7) 0.050(6) 0.072(7) -0.006(5) 0.019(6) -0.006(5) C27 0.093(8) 0.069(7) 0.055(6) -0.008(5) 0.020(6) -0.019(7) C28 0.108(10) 0.048(7) 0.038(6) -0.007(5) 0.017(6) -0.002(6) C29 0.071(7) 0.055(7) 0.083(8) -0.014(6) -0.003(6) -0.004(6) C30 0.083(8) 0.075(9) 0.085(9) -0.032(7) 0.038(7) -0.020(7) C31 0.149(12) 0.044(6) 0.045(6) -0.007(5) 0.007(7) -0.026(7) C32 0.076(8) 0.064(7) 0.072(8) 0.001(6) 0.000(6) 0.000(6) C33 0.056(6) 0.069(7) 0.073(7) -0.007(6) 0.006(5) 0.000(6) C34 0.237(19) 0.088(10) 0.041(6) -0.019(6) 0.038(9) -0.086(12) C35 0.200(13) 0.141(10) 0.145(10) 0.081(9) -0.016(10) -0.051(11) C36 0.113(10) 0.099(11) 0.126(12) 0.072(10) -0.037(10) -0.034(10) C37 0.095(9) 0.092(10) 0.104(10) 0.027(8) 0.011(8) -0.015(8) C38 0.087(9) 0.088(9) 0.093(9) 0.030(8) -0.004(7) -0.034(8) C39 0.119(10) 0.097(10) 0.068(8) 0.017(7) -0.015(8) -0.008(9) C40 0.121(12) 0.131(14) 0.114(12) 0.071(11) -0.018(10) 0.002(12) C41 0.102(9) 0.076(8) 0.075(8) -0.015(7) 0.001(7) -0.002(7) C42 0.192(16) 0.087(10) 0.046(7) -0.012(7) 0.028(8) 0.013(11) C43 0.22(2) 0.055(8) 0.063(9) 0.010(6) -0.018(11) -0.004(11) C44 0.130(11) 0.075(9) 0.074(8) -0.027(7) 0.000(8) -0.030(8) C45 0.098(9) 0.088(10) 0.076(8) -0.005(7) 0.005(7) -0.008(8) C46 0.26(2) 0.093(11) 0.053(7) 0.010(7) 0.011(10) 0.023(14) C47 0.195(18) 0.125(15) 0.068(9) 0.012(9) 0.020(10) -0.001(14) C48 0.210(12) 0.145(10) 0.118(9) 0.056(8) -0.019(9) -0.052(10) C49 0.200(13) 0.131(10) 0.082(8) 0.046(7) -0.026(9) -0.046(11) C50 0.095(7) 0.045(6) 0.054(6) -0.005(5) -0.016(7) -0.005(6) C51 0.076(7) 0.061(7) 0.077(8) -0.014(6) -0.004(6) -0.009(6) C52 0.060(7) 0.075(8) 0.087(8) -0.003(7) 0.008(6) -0.005(6) C53 0.088(8) 0.044(6) 0.083(8) -0.007(6) 0.010(7) -0.011(6) C54 0.101(9) 0.076(8) 0.066(7) 0.007(7) 0.023(7) -0.007(7) Cd2 0.0660(4) 0.0528(4) 0.0571(4) 0.0035(3) 0.0045(4) 0.0042(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 O5 2.292(7) . ? Cd1 N2 2.334(9) . ? Cd1 N1 2.336(9) . ? Cd1 O3 2.372(9) 3_546 ? Cd1 O1 2.382(7) . ? Cd1 O2 2.439(7) . ? N1 C29 1.292(14) . ? N1 C33 1.351(13) . ? N2 C38 1.282(14) . ? N2 C39 1.406(15) . ? N3 C45 1.353(16) . ? N3 C41 1.363(15) . ? N3 Cd2 2.297(9) 2 ? N4 C52 1.326(13) . ? N4 C53 1.348(14) . ? N4 Cd2 2.327(8) 2_554 ? O1 C1 1.239(13) . ? O2 C1 1.266(12) . ? O3 C14 1.265(15) . ? O3 Cd1 2.372(9) 3_556 ? O4 C14 1.137(14) . ? O4 Cd2 2.315(8) 3_556 ? O5 C15 1.245(11) . ? O5 Cd2 2.405(7) . ? O6 C15 1.286(12) . ? O6 Cd2 2.474(7) . ? O7 C28 1.300(13) . ? O7 Cd2 2.406(8) 3_656 ? O8 C28 1.190(14) . ? O8 Cd2 2.331(8) 3_656 ? C1 C2 1.488(14) . ? C2 C3 1.565(15) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.482(15) . ? C3 C9 1.512(19) . ? C3 C8 1.545(18) . ? C4 C5 1.550(15) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C12 1.441(19) . ? C5 C6 1.534(19) . ? C5 C13 1.535(17) . ? C6 C7 1.53(2) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C10 1.34(2) . ? C7 C8 1.62(2) . ? C7 H7 0.9800 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C11 1.515(18) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.58(2) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.53(2) . ? C11 H11 0.9800 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.483(16) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C15 C16 1.507(13) . ? C16 C18 1.528(13) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C22 1.527(16) . ? C17 C18 1.532(14) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C26 1.544(13) . ? C18 C19 1.544(13) . ? C19 C20 1.549(14) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C27 1.509(14) . ? C20 C24 1.524(15) . ? C20 C21 1.567(16) . ? C21 C22 1.518(18) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.45(2) . ? C22 H22 0.9800 . ? C23 C25 1.54(2) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.530(17) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.512(16) . ? C25 H25 0.9800 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.558(15) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 Cd2 2.714(11) 3_656 ? C29 C30 1.425(17) . ? C29 H29 0.9300 . ? C30 C31 1.358(17) . ? C30 H30 0.9300 . ? C31 C32 1.352(17) . ? C31 C34 1.543(15) . ? C32 C33 1.355(15) . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? C34 C47 1.490(9) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C48 1.459(10) . ? C35 C36 1.501(18) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 C40 1.342(19) . ? C36 C37 1.402(18) . ? C37 C38 1.386(17) . ? C37 H37 0.9300 . ? C38 H38 0.9300 . ? C39 C40 1.357(17) . ? C39 H39 0.9300 . ? C40 H40 0.9300 . ? C41 C42 1.349(18) . ? C41 H41 0.9300 . ? C42 C43 1.41(2) . ? C42 H42 0.9300 . ? C43 C44 1.35(2) . ? C43 C46 1.502(9) . ? C44 C45 1.340(17) . ? C44 H44 0.9300 . ? C45 H45 0.9300 . ? C46 C47 1.464(9) . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C48 C49 1.449(19) . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C49 C50 1.476(18) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 C51 1.309(15) . ? C50 C54 1.337(15) . ? C51 C52 1.412(16) . ? C51 H51 0.9300 . ? C52 H52 0.9300 . ? C53 C54 1.403(16) . ? C53 H53 0.9300 . ? C54 H54 0.9300 . ? Cd2 N3 2.297(9) 2_554 ? Cd2 O4 2.315(8) 3_546 ? Cd2 N4 2.327(8) 2 ? Cd2 O8 2.331(8) 3_646 ? Cd2 O7 2.406(8) 3_646 ? Cd2 C28 2.714(11) 3_646 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Cd1 N2 102.1(3) . . ? O5 Cd1 N1 94.4(3) . . ? N2 Cd1 N1 163.3(3) . . ? O5 Cd1 O3 112.7(3) . 3_546 ? N2 Cd1 O3 86.5(3) . 3_546 ? N1 Cd1 O3 84.6(3) . 3_546 ? O5 Cd1 O1 93.6(3) . . ? N2 Cd1 O1 85.0(3) . . ? N1 Cd1 O1 96.8(3) . . ? O3 Cd1 O1 153.5(3) 3_546 . ? O5 Cd1 O2 146.8(3) . . ? N2 Cd1 O2 84.5(3) . . ? N1 Cd1 O2 83.2(3) . . ? O3 Cd1 O2 100.0(3) 3_546 . ? O1 Cd1 O2 54.2(3) . . ? C29 N1 C33 117.7(10) . . ? C29 N1 Cd1 121.6(8) . . ? C33 N1 Cd1 120.6(7) . . ? C38 N2 C39 115.1(10) . . ? C38 N2 Cd1 126.6(8) . . ? C39 N2 Cd1 117.6(8) . . ? C45 N3 C41 114.7(10) . . ? C45 N3 Cd2 120.0(8) . 2 ? C41 N3 Cd2 125.1(8) . 2 ? C52 N4 C53 115.5(9) . . ? C52 N4 Cd2 123.3(7) . 2_554 ? C53 N4 Cd2 121.2(7) . 2_554 ? C1 O1 Cd1 93.2(7) . . ? C1 O2 Cd1 89.9(6) . . ? C14 O3 Cd1 106.1(7) . 3_556 ? C14 O4 Cd2 157.2(9) . 3_556 ? C15 O5 Cd1 146.3(7) . . ? C15 O5 Cd2 96.3(6) . . ? Cd1 O5 Cd2 115.7(3) . . ? C15 O6 Cd2 92.0(6) . . ? C28 O7 Cd2 88.9(7) . 3_656 ? C28 O8 Cd2 95.3(7) . 3_656 ? O1 C1 O2 122.5(9) . . ? O1 C1 C2 119.4(11) . . ? O2 C1 C2 118.1(10) . . ? C1 C2 C3 117.1(9) . . ? C1 C2 H2A 108.0 . . ? C3 C2 H2A 108.0 . . ? C1 C2 H2B 108.0 . . ? C3 C2 H2B 108.0 . . ? H2A C2 H2B 107.3 . . ? C4 C3 C9 109.6(10) . . ? C4 C3 C8 110.3(11) . . ? C9 C3 C8 107.4(12) . . ? C4 C3 C2 109.3(9) . . ? C9 C3 C2 108.2(10) . . ? C8 C3 C2 112.0(10) . . ? C3 C4 C5 111.6(9) . . ? C3 C4 H4A 109.3 . . ? C5 C4 H4A 109.3 . . ? C3 C4 H4B 109.3 . . ? C5 C4 H4B 109.3 . . ? H4A C4 H4B 108.0 . . ? C12 C5 C6 106.3(13) . . ? C12 C5 C13 110.8(11) . . ? C6 C5 C13 113.0(11) . . ? C12 C5 C4 110.2(10) . . ? C6 C5 C4 106.0(11) . . ? C13 C5 C4 110.4(10) . . ? C7 C6 C5 116.0(14) . . ? C7 C6 H6A 108.3 . . ? C5 C6 H6A 108.3 . . ? C7 C6 H6B 108.3 . . ? C5 C6 H6B 108.3 . . ? H6A C6 H6B 107.4 . . ? C10 C7 C6 108.6(15) . . ? C10 C7 C8 107.1(15) . . ? C6 C7 C8 100.7(14) . . ? C10 C7 H7 113.2 . . ? C6 C7 H7 113.2 . . ? C8 C7 H7 113.2 . . ? C3 C8 C7 110.5(12) . . ? C3 C8 H8A 109.6 . . ? C7 C8 H8A 109.6 . . ? C3 C8 H8B 109.6 . . ? C7 C8 H8B 109.6 . . ? H8A C8 H8B 108.1 . . ? C3 C9 C11 112.0(12) . . ? C3 C9 H9A 109.2 . . ? C11 C9 H9A 109.2 . . ? C3 C9 H9B 109.2 . . ? C11 C9 H9B 109.2 . . ? H9A C9 H9B 107.9 . . ? C7 C10 C11 120.3(15) . . ? C7 C10 H10A 107.2 . . ? C11 C10 H10A 107.2 . . ? C7 C10 H10B 107.2 . . ? C11 C10 H10B 107.2 . . ? H10A C10 H10B 106.9 . . ? C9 C11 C12 112.0(12) . . ? C9 C11 C10 102.6(14) . . ? C12 C11 C10 103.4(15) . . ? C9 C11 H11 112.7 . . ? C12 C11 H11 112.7 . . ? C10 C11 H11 112.7 . . ? C5 C12 C11 113.7(13) . . ? C5 C12 H12A 108.8 . . ? C11 C12 H12A 108.8 . . ? C5 C12 H12B 108.8 . . ? C11 C12 H12B 108.8 . . ? H12A C12 H12B 107.7 . . ? C14 C13 C5 123.6(11) . . ? C14 C13 H13A 106.4 . . ? C5 C13 H13A 106.4 . . ? C14 C13 H13B 106.4 . . ? C5 C13 H13B 106.4 . . ? H13A C13 H13B 106.5 . . ? O4 C14 O3 126.4(13) . . ? O4 C14 C13 122.0(14) . . ? O3 C14 C13 111.0(12) . . ? O5 C15 O6 118.7(9) . . ? O5 C15 C16 120.2(9) . . ? O6 C15 C16 121.0(9) . . ? C15 C16 C18 114.6(7) . . ? C15 C16 H16A 108.6 . . ? C18 C16 H16A 108.6 . . ? C15 C16 H16B 108.6 . . ? C18 C16 H16B 108.6 . . ? H16A C16 H16B 107.6 . . ? C22 C17 C18 109.2(10) . . ? C22 C17 H17A 109.8 . . ? C18 C17 H17A 109.8 . . ? C22 C17 H17B 109.8 . . ? C18 C17 H17B 109.8 . . ? H17A C17 H17B 108.3 . . ? C16 C18 C17 113.7(8) . . ? C16 C18 C26 111.8(8) . . ? C17 C18 C26 106.2(8) . . ? C16 C18 C19 107.3(7) . . ? C17 C18 C19 109.6(9) . . ? C26 C18 C19 108.2(8) . . ? C18 C19 C20 111.7(8) . . ? C18 C19 H19A 109.3 . . ? C20 C19 H19A 109.3 . . ? C18 C19 H19B 109.3 . . ? C20 C19 H19B 109.3 . . ? H19A C19 H19B 107.9 . . ? C27 C20 C24 108.7(9) . . ? C27 C20 C19 111.0(8) . . ? C24 C20 C19 106.5(9) . . ? C27 C20 C21 113.0(9) . . ? C24 C20 C21 109.6(10) . . ? C19 C20 C21 107.8(9) . . ? C22 C21 C20 108.4(10) . . ? C22 C21 H21A 110.0 . . ? C20 C21 H21A 110.0 . . ? C22 C21 H21B 110.0 . . ? C20 C21 H21B 110.0 . . ? H21A C21 H21B 108.4 . . ? C23 C22 C21 112.5(13) . . ? C23 C22 C17 110.4(13) . . ? C21 C22 C17 110.9(10) . . ? C23 C22 H22 107.6 . . ? C21 C22 H22 107.6 . . ? C17 C22 H22 107.6 . . ? C22 C23 C25 109.4(11) . . ? C22 C23 H23A 109.8 . . ? C25 C23 H23A 109.8 . . ? C22 C23 H23B 109.8 . . ? C25 C23 H23B 109.8 . . ? H23A C23 H23B 108.2 . . ? C20 C24 C25 111.5(10) . . ? C20 C24 H24A 109.3 . . ? C25 C24 H24A 109.3 . . ? C20 C24 H24B 109.3 . . ? C25 C24 H24B 109.3 . . ? H24A C24 H24B 108.0 . . ? C26 C25 C24 107.9(10) . . ? C26 C25 C23 108.1(10) . . ? C24 C25 C23 110.3(12) . . ? C26 C25 H25 110.1 . . ? C24 C25 H25 110.1 . . ? C23 C25 H25 110.1 . . ? C25 C26 C18 111.6(9) . . ? C25 C26 H26A 109.3 . . ? C18 C26 H26A 109.3 . . ? C25 C26 H26B 109.3 . . ? C18 C26 H26B 109.3 . . ? H26A C26 H26B 108.0 . . ? C20 C27 C28 111.5(8) . . ? C20 C27 H27A 109.3 . . ? C28 C27 H27A 109.3 . . ? C20 C27 H27B 109.3 . . ? C28 C27 H27B 109.3 . . ? H27A C27 H27B 108.0 . . ? O8 C28 O7 121.2(11) . . ? O8 C28 C27 123.5(11) . . ? O7 C28 C27 115.3(11) . . ? O8 C28 Cd2 58.8(6) . 3_656 ? O7 C28 Cd2 62.5(6) . 3_656 ? C27 C28 Cd2 175.3(7) . 3_656 ? N1 C29 C30 121.8(12) . . ? N1 C29 H29 119.1 . . ? C30 C29 H29 119.1 . . ? C31 C30 C29 119.3(11) . . ? C31 C30 H30 120.4 . . ? C29 C30 H30 120.4 . . ? C32 C31 C30 118.0(11) . . ? C32 C31 C34 123.6(14) . . ? C30 C31 C34 118.3(14) . . ? C31 C32 C33 120.3(12) . . ? C31 C32 H32 119.9 . . ? C33 C32 H32 119.9 . . ? N1 C33 C32 122.9(10) . . ? N1 C33 H33 118.5 . . ? C32 C33 H33 118.5 . . ? C47 C34 C31 112.0(10) . . ? C47 C34 H34A 109.2 . . ? C31 C34 H34A 109.2 . . ? C47 C34 H34B 109.2 . . ? C31 C34 H34B 109.2 . . ? H34A C34 H34B 107.9 . . ? C48 C35 C36 120.7(14) . . ? C48 C35 H35A 107.1 . . ? C36 C35 H35A 107.1 . . ? C48 C35 H35B 107.2 . . ? C36 C35 H35B 107.2 . . ? H35A C35 H35B 106.8 . . ? C40 C36 C37 115.6(12) . . ? C40 C36 C35 124.1(14) . . ? C37 C36 C35 120.0(13) . . ? C38 C37 C36 118.7(13) . . ? C38 C37 H37 120.7 . . ? C36 C37 H37 120.7 . . ? N2 C38 C37 126.1(13) . . ? N2 C38 H38 117.0 . . ? C37 C38 H38 117.0 . . ? C40 C39 N2 121.0(14) . . ? C40 C39 H39 119.5 . . ? N2 C39 H39 119.5 . . ? C36 C40 C39 123.4(15) . . ? C36 C40 H40 118.3 . . ? C39 C40 H40 118.3 . . ? C42 C41 N3 121.9(14) . . ? C42 C41 H41 119.0 . . ? N3 C41 H41 119.0 . . ? C41 C42 C43 122.9(14) . . ? C41 C42 H42 118.6 . . ? C43 C42 H42 118.6 . . ? C44 C43 C42 112.9(11) . . ? C44 C43 C46 118.8(18) . . ? C42 C43 C46 128.2(18) . . ? C45 C44 C43 123.6(14) . . ? C45 C44 H44 118.2 . . ? C43 C44 H44 118.2 . . ? C44 C45 N3 123.8(13) . . ? C44 C45 H45 118.1 . . ? N3 C45 H45 118.1 . . ? C47 C46 C43 116.6(13) . . ? C47 C46 H46A 108.2 . . ? C43 C46 H46A 108.1 . . ? C47 C46 H46B 108.1 . . ? C43 C46 H46B 108.2 . . ? H46A C46 H46B 107.3 . . ? C46 C47 C34 109.2(12) . . ? C46 C47 H47A 109.8 . . ? C34 C47 H47A 109.8 . . ? C46 C47 H47B 109.8 . . ? C34 C47 H47B 109.8 . . ? H47A C47 H47B 108.3 . . ? C49 C48 C35 116.3(16) . . ? C49 C48 H48A 108.2 . . ? C35 C48 H48A 108.2 . . ? C49 C48 H48B 108.2 . . ? C35 C48 H48B 108.2 . . ? H48A C48 H48B 107.3 . . ? C48 C49 C50 119.9(15) . . ? C48 C49 H49A 107.4 . . ? C50 C49 H49A 107.4 . . ? C48 C49 H49B 107.3 . . ? C50 C49 H49B 107.4 . . ? H49A C49 H49B 106.9 . . ? C51 C50 C54 120.5(10) . . ? C51 C50 C49 122.9(12) . . ? C54 C50 C49 116.6(13) . . ? C50 C51 C52 120.6(11) . . ? C50 C51 H51 119.7 . . ? C52 C51 H51 119.7 . . ? N4 C52 C51 121.7(10) . . ? N4 C52 H52 119.1 . . ? C51 C52 H52 119.1 . . ? N4 C53 C54 124.2(10) . . ? N4 C53 H53 117.9 . . ? C54 C53 H53 117.9 . . ? C50 C54 C53 117.4(11) . . ? C50 C54 H54 121.3 . . ? C53 C54 H54 121.3 . . ? N3 Cd2 O4 95.3(4) 2_554 3_546 ? N3 Cd2 N4 171.4(4) 2_554 2 ? O4 Cd2 N4 93.2(3) 3_546 2 ? N3 Cd2 O8 88.9(3) 2_554 3_646 ? O4 Cd2 O8 87.2(4) 3_546 3_646 ? N4 Cd2 O8 92.9(3) 2 3_646 ? N3 Cd2 O5 86.8(3) 2_554 . ? O4 Cd2 O5 77.2(4) 3_546 . ? N4 Cd2 O5 93.8(3) 2 . ? O8 Cd2 O5 163.4(3) 3_646 . ? N3 Cd2 O7 87.6(3) 2_554 3_646 ? O4 Cd2 O7 141.6(4) 3_546 3_646 ? N4 Cd2 O7 86.7(3) 2 3_646 ? O8 Cd2 O7 54.5(3) 3_646 3_646 ? O5 Cd2 O7 141.2(3) . 3_646 ? N3 Cd2 O6 85.9(3) 2_554 . ? O4 Cd2 O6 130.1(4) 3_546 . ? N4 Cd2 O6 87.6(3) 2 . ? O8 Cd2 O6 142.6(3) 3_646 . ? O5 Cd2 O6 53.0(2) . . ? O7 Cd2 O6 88.3(3) 3_646 . ? N3 Cd2 C28 88.8(3) 2_554 3_646 ? O4 Cd2 C28 113.0(4) 3_546 3_646 ? N4 Cd2 C28 89.1(3) 2 3_646 ? O8 Cd2 C28 25.9(3) 3_646 3_646 ? O5 Cd2 C28 169.2(3) . 3_646 ? O7 Cd2 C28 28.6(3) 3_646 3_646 ? O6 Cd2 C28 116.9(3) . 3_646 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O5 Cd1 N1 C29 175.6(8) . . . . ? N2 Cd1 N1 C29 -13.8(16) . . . . ? O3 Cd1 N1 C29 -71.9(9) 3_546 . . . ? O1 Cd1 N1 C29 81.5(9) . . . . ? O2 Cd1 N1 C29 28.9(8) . . . . ? O5 Cd1 N1 C33 -7.3(8) . . . . ? N2 Cd1 N1 C33 163.3(9) . . . . ? O3 Cd1 N1 C33 105.2(8) 3_546 . . . ? O1 Cd1 N1 C33 -101.4(8) . . . . ? O2 Cd1 N1 C33 -154.0(8) . . . . ? O5 Cd1 N2 C38 -42.5(11) . . . . ? N1 Cd1 N2 C38 147.1(12) . . . . ? O3 Cd1 N2 C38 -155.0(11) 3_546 . . . ? O1 Cd1 N2 C38 50.1(11) . . . . ? O2 Cd1 N2 C38 104.5(11) . . . . ? O5 Cd1 N2 C39 147.3(9) . . . . ? N1 Cd1 N2 C39 -23.0(16) . . . . ? O3 Cd1 N2 C39 34.8(9) 3_546 . . . ? O1 Cd1 N2 C39 -120.0(9) . . . . ? O2 Cd1 N2 C39 -65.6(9) . . . . ? O5 Cd1 O1 C1 -168.5(6) . . . . ? N2 Cd1 O1 C1 89.6(6) . . . . ? N1 Cd1 O1 C1 -73.7(6) . . . . ? O3 Cd1 O1 C1 17.8(10) 3_546 . . . ? O2 Cd1 O1 C1 2.8(6) . . . . ? O5 Cd1 O2 C1 13.2(8) . . . . ? N2 Cd1 O2 C1 -90.6(6) . . . . ? N1 Cd1 O2 C1 100.7(6) . . . . ? O3 Cd1 O2 C1 -176.0(6) 3_546 . . . ? O1 Cd1 O2 C1 -2.8(5) . . . . ? N2 Cd1 O5 C15 71.1(11) . . . . ? N1 Cd1 O5 C15 -111.6(11) . . . . ? O3 Cd1 O5 C15 162.4(10) 3_546 . . . ? O1 Cd1 O5 C15 -14.6(11) . . . . ? O2 Cd1 O5 C15 -27.4(13) . . . . ? N2 Cd1 O5 Cd2 -89.0(3) . . . . ? N1 Cd1 O5 Cd2 88.2(3) . . . . ? O3 Cd1 O5 Cd2 2.2(4) 3_546 . . . ? O1 Cd1 O5 Cd2 -174.7(3) . . . . ? O2 Cd1 O5 Cd2 172.4(3) . . . . ? Cd1 O1 C1 O2 -5.2(10) . . . . ? Cd1 O1 C1 C2 177.1(8) . . . . ? Cd1 O2 C1 O1 5.1(10) . . . . ? Cd1 O2 C1 C2 -177.2(8) . . . . ? O1 C1 C2 C3 -93.2(13) . . . . ? O2 C1 C2 C3 89.0(13) . . . . ? C1 C2 C3 C4 166.7(11) . . . . ? C1 C2 C3 C9 -74.0(14) . . . . ? C1 C2 C3 C8 44.2(16) . . . . ? C9 C3 C4 C5 58.6(13) . . . . ? C8 C3 C4 C5 -59.4(13) . . . . ? C2 C3 C4 C5 177.1(9) . . . . ? C3 C4 C5 C12 -58.3(13) . . . . ? C3 C4 C5 C6 56.4(14) . . . . ? C3 C4 C5 C13 179.0(10) . . . . ? C12 C5 C6 C7 54.2(18) . . . . ? C13 C5 C6 C7 176.0(14) . . . . ? C4 C5 C6 C7 -63.0(17) . . . . ? C5 C6 C7 C10 -49(2) . . . . ? C5 C6 C7 C8 63.6(18) . . . . ? C4 C3 C8 C7 62.6(16) . . . . ? C9 C3 C8 C7 -56.8(15) . . . . ? C2 C3 C8 C7 -175.5(12) . . . . ? C10 C7 C8 C3 53.2(18) . . . . ? C6 C7 C8 C3 -60.2(17) . . . . ? C4 C3 C9 C11 -55.5(16) . . . . ? C8 C3 C9 C11 64.3(15) . . . . ? C2 C3 C9 C11 -174.6(12) . . . . ? C6 C7 C10 C11 50(2) . . . . ? C8 C7 C10 C11 -58(2) . . . . ? C3 C9 C11 C12 51(2) . . . . ? C3 C9 C11 C10 -59.6(17) . . . . ? C7 C10 C11 C9 61(2) . . . . ? C7 C10 C11 C12 -55.3(19) . . . . ? C6 C5 C12 C11 -61.3(17) . . . . ? C13 C5 C12 C11 175.5(12) . . . . ? C4 C5 C12 C11 53.1(17) . . . . ? C9 C11 C12 C5 -51(2) . . . . ? C10 C11 C12 C5 59.0(16) . . . . ? C12 C5 C13 C14 -90.0(16) . . . . ? C6 C5 C13 C14 150.8(14) . . . . ? C4 C5 C13 C14 32.3(18) . . . . ? Cd2 O4 C14 O3 -92(3) 3_556 . . . ? Cd2 O4 C14 C13 98(3) 3_556 . . . ? Cd1 O3 C14 O4 3.5(15) 3_556 . . . ? Cd1 O3 C14 C13 174.5(7) 3_556 . . . ? C5 C13 C14 O4 64.6(18) . . . . ? C5 C13 C14 O3 -106.9(14) . . . . ? Cd1 O5 C15 O6 -164.3(8) . . . . ? Cd2 O5 C15 O6 -2.2(9) . . . . ? Cd1 O5 C15 C16 18.2(16) . . . . ? Cd2 O5 C15 C16 -179.7(7) . . . . ? Cd2 O6 C15 O5 2.1(8) . . . . ? Cd2 O6 C15 C16 179.6(7) . . . . ? O5 C15 C16 C18 102.0(11) . . . . ? O6 C15 C16 C18 -75.5(11) . . . . ? C15 C16 C18 C17 64.3(12) . . . . ? C15 C16 C18 C26 -55.9(11) . . . . ? C15 C16 C18 C19 -174.4(8) . . . . ? C22 C17 C18 C16 177.5(10) . . . . ? C22 C17 C18 C26 -59.2(12) . . . . ? C22 C17 C18 C19 57.5(12) . . . . ? C16 C18 C19 C20 178.5(9) . . . . ? C17 C18 C19 C20 -57.6(11) . . . . ? C26 C18 C19 C20 57.8(11) . . . . ? C18 C19 C20 C27 -177.5(8) . . . . ? C18 C19 C20 C24 -59.4(12) . . . . ? C18 C19 C20 C21 58.2(11) . . . . ? C27 C20 C21 C22 177.2(9) . . . . ? C24 C20 C21 C22 55.8(12) . . . . ? C19 C20 C21 C22 -59.7(12) . . . . ? C20 C21 C22 C23 -61.2(13) . . . . ? C20 C21 C22 C17 63.0(15) . . . . ? C18 C17 C22 C23 63.5(15) . . . . ? C18 C17 C22 C21 -61.9(15) . . . . ? C21 C22 C23 C25 62.0(14) . . . . ? C17 C22 C23 C25 -62.4(15) . . . . ? C27 C20 C24 C25 -178.9(11) . . . . ? C19 C20 C24 C25 61.4(13) . . . . ? C21 C20 C24 C25 -54.9(13) . . . . ? C20 C24 C25 C26 -62.4(15) . . . . ? C20 C24 C25 C23 55.5(14) . . . . ? C22 C23 C25 C26 60.0(14) . . . . ? C22 C23 C25 C24 -57.8(14) . . . . ? C24 C25 C26 C18 59.7(13) . . . . ? C23 C25 C26 C18 -59.7(12) . . . . ? C16 C18 C26 C25 -175.7(9) . . . . ? C17 C18 C26 C25 59.8(11) . . . . ? C19 C18 C26 C25 -57.9(12) . . . . ? C24 C20 C27 C28 -171.8(10) . . . . ? C19 C20 C27 C28 -55.0(13) . . . . ? C21 C20 C27 C28 66.3(12) . . . . ? Cd2 O8 C28 O7 -3.3(11) 3_656 . . . ? Cd2 O8 C28 C27 175.1(8) 3_656 . . . ? Cd2 O7 C28 O8 3.2(11) 3_656 . . . ? Cd2 O7 C28 C27 -175.4(7) 3_656 . . . ? C20 C27 C28 O8 -66.3(14) . . . . ? C20 C27 C28 O7 112.2(11) . . . . ? C20 C27 C28 Cd2 51(11) . . . 3_656 ? C33 N1 C29 C30 1.4(16) . . . . ? Cd1 N1 C29 C30 178.6(7) . . . . ? N1 C29 C30 C31 -1.0(17) . . . . ? C29 C30 C31 C32 0.5(17) . . . . ? C29 C30 C31 C34 176.4(9) . . . . ? C30 C31 C32 C33 -0.4(18) . . . . ? C34 C31 C32 C33 -176.1(10) . . . . ? C29 N1 C33 C32 -1.3(16) . . . . ? Cd1 N1 C33 C32 -178.5(8) . . . . ? C31 C32 C33 N1 0.9(18) . . . . ? C32 C31 C34 C47 63.5(18) . . . . ? C30 C31 C34 C47 -112.3(15) . . . . ? C48 C35 C36 C40 27(3) . . . . ? C48 C35 C36 C37 -158.9(19) . . . . ? C40 C36 C37 C38 2(2) . . . . ? C35 C36 C37 C38 -172.6(17) . . . . ? C39 N2 C38 C37 -3(2) . . . . ? Cd1 N2 C38 C37 -173.0(11) . . . . ? C36 C37 C38 N2 1(3) . . . . ? C38 N2 C39 C40 1(2) . . . . ? Cd1 N2 C39 C40 172.2(12) . . . . ? C37 C36 C40 C39 -4(3) . . . . ? C35 C36 C40 C39 170.7(18) . . . . ? N2 C39 C40 C36 2(3) . . . . ? C45 N3 C41 C42 -2.2(18) . . . . ? Cd2 N3 C41 C42 -178.2(10) 2 . . . ? N3 C41 C42 C43 5(2) . . . . ? C41 C42 C43 C44 -5(2) . . . . ? C41 C42 C43 C46 172.0(13) . . . . ? C42 C43 C44 C45 2(2) . . . . ? C46 C43 C44 C45 -174.5(13) . . . . ? C43 C44 C45 N3 0(2) . . . . ? C41 N3 C45 C44 0.0(19) . . . . ? Cd2 N3 C45 C44 176.3(11) 2 . . . ? C44 C43 C46 C47 -122.4(18) . . . . ? C42 C43 C46 C47 61(2) . . . . ? C43 C46 C47 C34 -172.8(14) . . . . ? C31 C34 C47 C46 70.4(19) . . . . ? C36 C35 C48 C49 -176.3(19) . . . . ? C35 C48 C49 C50 103(2) . . . . ? C48 C49 C50 C51 -136.8(17) . . . . ? C48 C49 C50 C54 46(2) . . . . ? C54 C50 C51 C52 -3.2(17) . . . . ? C49 C50 C51 C52 -179.9(13) . . . . ? C53 N4 C52 C51 3.8(16) . . . . ? Cd2 N4 C52 C51 -176.1(8) 2_554 . . . ? C50 C51 C52 N4 -1.0(18) . . . . ? C52 N4 C53 C54 -2.9(17) . . . . ? Cd2 N4 C53 C54 177.1(9) 2_554 . . . ? C51 C50 C54 C53 4.0(17) . . . . ? C49 C50 C54 C53 -179.0(13) . . . . ? N4 C53 C54 C50 -1.0(18) . . . . ? C15 O5 Cd2 N3 -86.0(6) . . . 2_554 ? Cd1 O5 Cd2 N3 83.0(4) . . . 2_554 ? C15 O5 Cd2 O4 177.8(6) . . . 3_546 ? Cd1 O5 Cd2 O4 -13.1(3) . . . 3_546 ? C15 O5 Cd2 N4 85.4(6) . . . 2 ? Cd1 O5 Cd2 N4 -105.5(4) . . . 2 ? C15 O5 Cd2 O8 -161.0(9) . . . 3_646 ? Cd1 O5 Cd2 O8 8.0(11) . . . 3_646 ? C15 O5 Cd2 O7 -4.0(7) . . . 3_646 ? Cd1 O5 Cd2 O7 165.1(3) . . . 3_646 ? C15 O5 Cd2 O6 1.2(5) . . . . ? Cd1 O5 Cd2 O6 170.3(5) . . . . ? C15 O5 Cd2 C28 -20.0(17) . . . 3_646 ? Cd1 O5 Cd2 C28 149.1(13) . . . 3_646 ? C15 O6 Cd2 N3 87.8(6) . . . 2_554 ? C15 O6 Cd2 O4 -5.5(7) . . . 3_546 ? C15 O6 Cd2 N4 -97.7(6) . . . 2 ? C15 O6 Cd2 O8 170.6(5) . . . 3_646 ? C15 O6 Cd2 O5 -1.2(5) . . . . ? C15 O6 Cd2 O7 175.5(5) . . . 3_646 ? C15 O6 Cd2 C28 174.5(5) . . . 3_646 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.845 _refine_diff_density_min -0.623 _refine_diff_density_rms 0.128