# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Zhong-Min Su' _publ_contact_author_email ZMSU@NENU.EDU.CN _publ_section_title ; d10 Metal coordination polymers based on analogue di(pyridyl)imidazole derivatives and 4,4'-oxydibenzoic acid: influence of flexible and angular characters of neutral ligands on structural diversity ; loop_ _publ_author_name 'Zhong-Min Su' 'Qiang Fu' 'Yao-Mei Fu' 'Ya-Qian Lan' 'Shun-Li Li' 'Lu Li' ; Yan-Hong Xu ; # Attachment '1-8-revised.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 687548' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H15 N3 O5 Zn' _chemical_formula_weight 466.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.6100(5) _cell_length_b 18.8880(10) _cell_length_c 14.7840(13) _cell_angle_alpha 90.00 _cell_angle_beta 98.8060(10) _cell_angle_gamma 90.00 _cell_volume 2100.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.76 _cell_measurement_theta_max 28.28 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.476 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 952 _exptl_absorpt_coefficient_mu 1.208 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.686 _exptl_absorpt_correction_T_max 0.722 _exptl_absorpt_process_details 'SADABS(Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12692 _diffrn_reflns_av_R_equivalents 0.0227 _diffrn_reflns_av_sigmaI/netI 0.0285 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 28.28 _reflns_number_total 5007 _reflns_number_gt 3072 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SMART (Bruker, 1997)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97(Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material SHELXL-97 _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. The disordered 2-(2-pyridyl)imidazole group were refined using C and N atoms split over two equivalent sites, with a total occupancy of 1. ; _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^)+(0.0720P)^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 5007 _refine_ls_number_parameters 342 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0761 _refine_ls_R_factor_gt 0.0420 _refine_ls_wR_factor_ref 0.1316 _refine_ls_wR_factor_gt 0.1141 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C16 C 0.4210(4) 0.19958(15) 0.33886(18) 0.0633(6) Uani 1 1 d . A . C17 C 0.5578(3) 0.25692(12) 0.34927(16) 0.0538(5) Uani 1 1 d . . . C18 C 0.5078(3) 0.32595(14) 0.36026(19) 0.0646(7) Uani 1 1 d . . . H18 H 0.3880 0.3372 0.3570 0.077 Uiso 1 1 calc R . . C19 C 0.6343(4) 0.37849(14) 0.37614(19) 0.0648(6) Uani 1 1 d . . . H19 H 0.5997 0.4251 0.3838 0.078 Uiso 1 1 calc R . . C20 C 0.8096(3) 0.36244(12) 0.38062(16) 0.0563(6) Uani 1 1 d . . . C21 C 0.8639(4) 0.29420(14) 0.3662(2) 0.0733(8) Uani 1 1 d . . . H21 H 0.9836 0.2838 0.3671 0.088 Uiso 1 1 calc R . . C22 C 0.7356(3) 0.24134(14) 0.3503(2) 0.0694(7) Uani 1 1 d . . . H22 H 0.7698 0.1951 0.3403 0.083 Uiso 1 1 calc R . . O1 O 0.4716(3) 0.13573(10) 0.33778(16) 0.0817(6) Uani 1 1 d . A . O2 O 0.2598(3) 0.21413(11) 0.33355(17) 0.0856(6) Uani 1 1 d . A . Zn1 Zn 0.21858(4) 0.093649(18) 0.33457(2) 0.07401(16) Uani 1 1 d . . . O3 O 0.9351(3) 0.41704(9) 0.39440(13) 0.0712(5) Uani 1 1 d . . . C11 C 1.2293(3) 0.43600(12) 0.46583(16) 0.0561(6) Uani 1 1 d . . . H11 H 1.2561 0.4522 0.4101 0.067 Uiso 1 1 calc R . . C10 C 1.0605(3) 0.41367(11) 0.47321(16) 0.0539(6) Uani 1 1 d . . . C12 C 1.0163(4) 0.39308(15) 0.5570(2) 0.0708(7) Uani 1 1 d . . . H12 H 0.9009 0.3792 0.5618 0.085 Uiso 1 1 calc R . . C14 C 1.3200(3) 0.41329(11) 0.62599(17) 0.0520(6) Uani 1 1 d . . . C13 C 1.3589(3) 0.43418(12) 0.54208(16) 0.0541(5) Uani 1 1 d . . . H13 H 1.4746 0.4473 0.5367 0.065 Uiso 1 1 calc R . . C15 C 1.1471(4) 0.39363(14) 0.63325(19) 0.0693(7) Uani 1 1 d . . . H15 H 1.1187 0.3807 0.6900 0.083 Uiso 1 1 calc R . . C4 C 1.4655(4) 0.41353(12) 0.70696(19) 0.0621(7) Uani 1 1 d . . . O4 O 1.6225(3) 0.42395(11) 0.69529(14) 0.0777(5) Uani 1 1 d . . . O5 O 1.4288(3) 0.40358(12) 0.78580(14) 0.0906(7) Uani 1 1 d . . . C2 C 0.206(2) 0.0360(7) 0.5208(8) 0.068(3) Uani 0.446(8) 1 d PG A 1 N1 N 0.1778(16) 0.0384(5) 0.6063(6) 0.093(3) Uani 0.446(8) 1 d PG A 1 H1B H 0.1897 0.0037 0.6445 0.112 Uiso 0.446(8) 1 calc PR A 1 C3 C 0.1278(17) 0.1032(5) 0.6232(7) 0.098(4) Uani 0.446(8) 1 d PG A 1 H3A H 0.0991 0.1195 0.6784 0.117 Uiso 0.446(8) 1 calc PR A 1 C1 C 0.125(2) 0.1408(7) 0.5481(8) 0.087(4) Uani 0.446(8) 1 d PG A 1 H1A H 0.0948 0.1884 0.5409 0.105 Uiso 0.446(8) 1 calc PR A 1 N2 N 0.174(2) 0.0993(8) 0.4848(8) 0.071(3) Uani 0.446(8) 1 d PG A 1 C5 C 0.2509(17) -0.0228(7) 0.4671(8) 0.076(3) Uani 0.446(8) 1 d PG A 1 N3 N 0.2634(19) -0.0067(7) 0.3749(10) 0.066(3) Uani 0.446(8) 1 d PG A 1 C9 C 0.3110(17) -0.0601(7) 0.3162(9) 0.085(3) Uani 0.446(8) 1 d PG A 1 H9A H 0.3193 -0.0495 0.2555 0.102 Uiso 0.446(8) 1 calc PR A 1 C8 C 0.3461(14) -0.1296(6) 0.3496(6) 0.112(4) Uani 0.446(8) 1 d PG A 1 H8A H 0.3774 -0.1647 0.3109 0.135 Uiso 0.446(8) 1 calc PR A 1 C7 C 0.3335(12) -0.1457(5) 0.4417(6) 0.105(4) Uani 0.40 1 d PG A 1 H7A H 0.3566 -0.1915 0.4637 0.127 Uiso 0.40 1 calc PR A 1 C6 C 0.2859(12) -0.0924(6) 0.5005(6) 0.089(3) Uani 0.446(8) 1 d PG A 1 H6A H 0.2777 -0.1030 0.5611 0.106 Uiso 0.446(8) 1 calc PR A 1 C5' C 0.2420(17) 0.0222(6) 0.5071(7) 0.069(3) Uani 0.554(8) 1 d PG A 2 C6' C 0.2280(15) 0.0115(4) 0.5981(7) 0.091(3) Uani 0.554(8) 1 d PG A 2 H6'A H 0.2529 -0.0328 0.6245 0.110 Uiso 0.554(8) 1 calc PR A 2 C7' C 0.1770(12) 0.0664(4) 0.6499(5) 0.111(3) Uani 0.60 1 d PG A 2 H7'A H 0.1676 0.0592 0.7112 0.133 Uiso 0.60 1 calc PR A 2 C8' C 0.1401(14) 0.1322(5) 0.6107(7) 0.117(5) Uani 0.554(8) 1 d PG A 2 H8'A H 0.1058 0.1692 0.6456 0.141 Uiso 0.554(8) 1 calc PR A 2 C9' C 0.1541(14) 0.1429(6) 0.5197(8) 0.101(4) Uani 0.554(8) 1 d PG A 2 H9'A H 0.1293 0.1872 0.4933 0.121 Uiso 0.554(8) 1 calc PR A 2 N3' N 0.2051(15) 0.0879(7) 0.4679(7) 0.066(2) Uani 0.554(8) 1 d PG A 2 C2' C 0.2975(12) -0.0280(5) 0.4511(6) 0.062(2) Uani 0.554(8) 1 d PG A 2 N2' N 0.3014(15) -0.0170(6) 0.3621(7) 0.066(2) Uani 0.554(8) 1 d PG A 2 C1' C 0.3590(13) -0.0763(6) 0.3270(7) 0.087(3) Uani 0.554(8) 1 d PG A 2 H1'A H 0.3744 -0.0832 0.2665 0.105 Uiso 0.554(8) 1 calc PR A 2 C3' C 0.3907(11) -0.1240(4) 0.3944(5) 0.108(3) Uani 0.554(8) 1 d PG A 2 H3'A H 0.4319 -0.1699 0.3888 0.129 Uiso 0.554(8) 1 calc PR A 2 N1' N 0.3527(8) -0.0942(3) 0.4710(5) 0.084(2) Uani 0.554(8) 1 d PG A 2 H1'B H 0.3621 -0.1140 0.5239 0.101 Uiso 0.554(8) 1 calc PR A 2 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 C16 0.0538(16) 0.0758(18) 0.0600(15) -0.0036(12) 0.0076(12) -0.0075(13) C17 0.0462(13) 0.0620(14) 0.0524(13) -0.0047(10) 0.0050(10) 0.0015(11) C18 0.0470(14) 0.0704(16) 0.0771(18) -0.0019(13) 0.0118(12) 0.0101(12) C19 0.0621(16) 0.0572(14) 0.0758(17) -0.0074(13) 0.0126(13) 0.0073(13) C20 0.0570(15) 0.0583(14) 0.0494(13) 0.0017(10) -0.0049(10) -0.0074(11) C21 0.0413(14) 0.0728(17) 0.103(2) 0.0049(15) 0.0025(14) 0.0041(12) C22 0.0506(15) 0.0571(14) 0.101(2) -0.0069(13) 0.0126(14) 0.0057(11) O1 0.0674(12) 0.0677(12) 0.1123(16) -0.0155(11) 0.0212(11) -0.0122(9) O2 0.0473(11) 0.0936(14) 0.1141(18) -0.0017(11) 0.0070(10) -0.0056(10) Zn1 0.0618(2) 0.0931(3) 0.0608(2) 0.01101(15) -0.01077(15) -0.02148(16) O3 0.0731(13) 0.0726(11) 0.0596(11) 0.0151(8) -0.0165(9) -0.0192(9) C11 0.0633(15) 0.0607(13) 0.0452(12) 0.0008(10) 0.0108(11) -0.0068(12) C10 0.0569(14) 0.0537(12) 0.0478(12) 0.0039(10) -0.0032(10) -0.0054(10) C12 0.0517(15) 0.0923(19) 0.0660(16) 0.0180(14) 0.0008(12) -0.0186(13) C14 0.0527(14) 0.0520(12) 0.0490(13) 0.0043(9) -0.0002(10) -0.0055(10) C13 0.0481(13) 0.0604(13) 0.0543(13) -0.0018(11) 0.0090(10) -0.0063(10) C15 0.0628(17) 0.0927(19) 0.0506(14) 0.0178(13) 0.0029(12) -0.0196(14) C4 0.0628(17) 0.0582(14) 0.0602(16) 0.0064(11) -0.0067(12) -0.0088(11) O4 0.0534(12) 0.1032(14) 0.0712(12) -0.0029(10) -0.0070(9) -0.0083(10) O5 0.0793(15) 0.1318(19) 0.0537(11) 0.0284(11) -0.0121(10) -0.0323(12) C2 0.064(7) 0.101(8) 0.037(5) 0.000(4) 0.004(4) -0.018(5) N1 0.101(7) 0.148(8) 0.033(4) -0.014(6) 0.015(4) -0.019(6) C3 0.114(9) 0.116(11) 0.059(6) 0.011(7) 0.000(5) -0.012(7) C1 0.092(8) 0.125(8) 0.047(8) -0.015(5) 0.019(5) -0.008(6) N2 0.058(6) 0.125(9) 0.033(4) -0.013(6) 0.018(3) -0.009(5) C5 0.045(6) 0.117(9) 0.061(7) 0.017(6) -0.010(4) -0.022(5) N3 0.055(6) 0.078(5) 0.064(6) -0.007(4) 0.004(4) -0.009(4) C9 0.074(8) 0.111(9) 0.061(5) 0.003(5) -0.013(5) 0.004(6) C8 0.094(8) 0.102(8) 0.130(11) 0.000(8) -0.017(7) 0.002(7) C7 0.089(7) 0.115(8) 0.104(9) 0.043(7) -0.013(6) -0.022(6) C6 0.066(6) 0.127(8) 0.069(6) 0.041(6) -0.003(4) -0.003(5) C5' 0.067(6) 0.098(6) 0.041(4) -0.006(4) 0.005(3) -0.018(4) C6' 0.115(8) 0.111(6) 0.051(4) -0.011(4) 0.022(4) -0.043(5) C7' 0.126(7) 0.145(9) 0.065(5) 0.004(5) 0.028(5) -0.021(6) C8' 0.112(7) 0.131(10) 0.115(11) -0.034(8) 0.037(7) 0.002(7) C9' 0.074(5) 0.171(9) 0.061(8) -0.039(6) 0.023(5) 0.002(5) N3' 0.043(4) 0.109(5) 0.046(4) -0.027(3) 0.008(3) -0.012(3) C2' 0.049(5) 0.091(5) 0.043(4) 0.006(3) -0.005(3) -0.012(3) N2' 0.052(4) 0.090(5) 0.049(4) 0.003(4) -0.010(3) -0.006(3) C1' 0.069(6) 0.100(7) 0.083(6) -0.010(5) -0.018(4) 0.000(5) C3' 0.078(6) 0.095(6) 0.134(9) -0.014(6) -0.033(6) 0.010(4) N1' 0.074(5) 0.098(4) 0.073(4) 0.025(4) -0.011(3) -0.017(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C16 O2 1.248(3) . ? C16 O1 1.267(3) . ? C16 C17 1.494(3) . ? C16 Zn1 2.520(3) . ? C17 C18 1.375(3) . ? C17 C22 1.383(3) . ? C18 C19 1.377(4) . ? C18 H18 0.9300 . ? C19 C20 1.360(4) . ? C19 H19 0.9300 . ? C20 C21 1.380(4) . ? C20 O3 1.399(3) . ? C21 C22 1.391(4) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? O1 Zn1 2.0769(19) . ? O2 Zn1 2.297(2) . ? Zn1 N3' 1.993(10) . ? Zn1 N3 2.001(14) . ? Zn1 O4 2.103(2) 4_465 ? Zn1 N2' 2.202(10) . ? Zn1 O5 2.213(2) 4_465 ? Zn1 N2 2.299(9) . ? Zn1 C4 2.485(3) 4_465 ? O3 C10 1.390(3) . ? C11 C10 1.372(3) . ? C11 C13 1.380(3) . ? C11 H11 0.9300 . ? C10 C12 1.388(4) . ? C12 C15 1.385(4) . ? C12 H12 0.9300 . ? C14 C13 1.377(3) . ? C14 C15 1.387(4) . ? C14 C4 1.501(4) . ? C13 H13 0.9300 . ? C15 H15 0.9300 . ? C4 O4 1.248(3) . ? C4 O5 1.254(4) . ? C4 Zn1 2.485(3) 4_766 ? O4 Zn1 2.103(2) 4_766 ? O5 Zn1 2.213(2) 4_766 ? C2 N2 1.316(8) . ? C2 N1 1.316(8) . ? C2 C5 1.436(14) . ? N1 C3 1.316(8) . ? N1 H1B 0.8600 . ? C3 C1 1.317(8) . ? C3 H3A 0.9300 . ? C1 N2 1.316(8) . ? C1 H1A 0.9300 . ? C5 N3 1.414(8) . ? C5 C6 1.414(8) . ? N3 C9 1.414(8) . ? C9 C8 1.414(8) . ? C9 H9A 0.9300 . ? C8 C7 1.414(8) . ? C8 H8A 0.9300 . ? C7 C6 1.414(8) . ? C7 H7A 0.9300 . ? C6 H6A 0.9300 . ? C5' C2' 1.367(11) . ? C5' N3' 1.381(6) . ? C5' C6' 1.381(6) . ? C6' C7' 1.381(6) . ? C6' H6'A 0.9300 . ? C7' C8' 1.381(6) . ? C7' H7'A 0.9300 . ? C8' C9' 1.381(6) . ? C8' H8'A 0.9300 . ? C9' N3' 1.381(6) . ? C9' H9'A 0.9300 . ? C2' N1' 1.337(7) . ? C2' N2' 1.337(7) . ? N2' C1' 1.337(7) . ? C1' C3' 1.337(7) . ? C1' H1'A 0.9300 . ? C3' N1' 1.337(7) . ? C3' H3'A 0.9300 . ? N1' H1'B 0.8600 . ? 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 O2 C16 O1 120.4(2) . . ? O2 C16 C17 120.7(3) . . ? O1 C16 C17 118.9(2) . . ? O2 C16 Zn1 65.28(15) . . ? O1 C16 Zn1 55.22(13) . . ? C17 C16 Zn1 172.7(2) . . ? C18 C17 C22 119.2(2) . . ? C18 C17 C16 119.9(2) . . ? C22 C17 C16 120.8(2) . . ? C17 C18 C19 120.3(2) . . ? C17 C18 H18 119.8 . . ? C19 C18 H18 119.8 . . ? C20 C19 C18 120.2(2) . . ? C20 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? C19 C20 C21 121.0(2) . . ? C19 C20 O3 119.0(2) . . ? C21 C20 O3 119.8(2) . . ? C20 C21 C22 118.6(2) . . ? C20 C21 H21 120.7 . . ? C22 C21 H21 120.7 . . ? C17 C22 C21 120.6(2) . . ? C17 C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? C16 O1 Zn1 94.71(16) . . ? C16 O2 Zn1 85.15(17) . . ? N3' Zn1 N3 71.7(5) . . ? N3' Zn1 O1 100.7(3) . . ? N3 Zn1 O1 103.9(4) . . ? N3' Zn1 O4 153.8(3) . 4_465 ? N3 Zn1 O4 99.2(5) . 4_465 ? O1 Zn1 O4 105.36(9) . 4_465 ? N3' Zn1 N2' 79.8(4) . . ? N3 Zn1 N2' 10.0(6) . . ? O1 Zn1 N2' 96.9(3) . . ? O4 Zn1 N2' 94.5(3) 4_465 . ? N3' Zn1 O5 97.1(3) . 4_465 ? N3 Zn1 O5 103.6(4) . 4_465 ? O1 Zn1 O5 150.74(9) . 4_465 ? O4 Zn1 O5 60.34(8) 4_465 4_465 ? N2' Zn1 O5 109.0(3) . 4_465 ? N3' Zn1 O2 95.0(4) . . ? N3 Zn1 O2 157.4(5) . . ? O1 Zn1 O2 59.62(7) . . ? O4 Zn1 O2 100.22(8) 4_465 . ? N2' Zn1 O2 154.9(3) . . ? O5 Zn1 O2 96.00(8) 4_465 . ? N3' Zn1 N2 7.9(7) . . ? N3 Zn1 N2 78.4(5) . . ? O1 Zn1 N2 103.5(4) . . ? O4 Zn1 N2 150.7(4) 4_465 . ? N2' Zn1 N2 86.9(5) . . ? O5 Zn1 N2 91.5(4) 4_465 . ? O2 Zn1 N2 90.0(4) . . ? N3' Zn1 C4 126.7(3) . 4_465 ? N3 Zn1 C4 104.6(5) . 4_465 ? O1 Zn1 C4 130.26(10) . 4_465 ? O4 Zn1 C4 30.14(9) 4_465 4_465 ? N2' Zn1 C4 104.8(3) . 4_465 ? O5 Zn1 C4 30.26(9) 4_465 4_465 ? O2 Zn1 C4 98.03(8) . 4_465 ? N2 Zn1 C4 121.6(4) . 4_465 ? N3' Zn1 C16 98.2(4) . . ? N3 Zn1 C16 132.0(5) . . ? O1 Zn1 C16 30.07(8) . . ? O4 Zn1 C16 105.65(9) 4_465 . ? N2' Zn1 C16 126.3(3) . . ? O5 Zn1 C16 124.34(9) 4_465 . ? O2 Zn1 C16 29.57(8) . . ? N2 Zn1 C16 96.8(4) . . ? C4 Zn1 C16 117.52(9) 4_465 . ? C10 O3 C20 116.99(18) . . ? C10 C11 C13 119.2(2) . . ? C10 C11 H11 120.4 . . ? C13 C11 H11 120.4 . . ? C11 C10 C12 121.0(2) . . ? C11 C10 O3 116.7(2) . . ? C12 C10 O3 122.1(2) . . ? C15 C12 C10 118.8(3) . . ? C15 C12 H12 120.6 . . ? C10 C12 H12 120.6 . . ? C13 C14 C15 119.0(2) . . ? C13 C14 C4 118.9(2) . . ? C15 C14 C4 122.1(2) . . ? C14 C13 C11 121.2(2) . . ? C14 C13 H13 119.4 . . ? C11 C13 H13 119.4 . . ? C12 C15 C14 120.7(2) . . ? C12 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? O4 C4 O5 120.4(3) . . ? O4 C4 C14 119.7(2) . . ? O5 C4 C14 119.9(3) . . ? O4 C4 Zn1 57.77(14) . 4_766 ? O5 C4 Zn1 62.81(15) . 4_766 ? C14 C4 Zn1 175.4(2) . 4_766 ? C4 O4 Zn1 92.09(17) . 4_766 ? C4 O5 Zn1 86.93(17) . 4_766 ? N2 C2 N1 108.0 . . ? N2 C2 C5 121.6(10) . . ? N1 C2 C5 130.2(10) . . ? C3 N1 C2 108.0 . . ? C3 N1 H1B 126.0 . . ? C2 N1 H1B 126.0 . . ? N1 C3 C1 108.0 . . ? N1 C3 H3A 126.0 . . ? C1 C3 H3A 126.0 . . ? N2 C1 C3 108.0 . . ? N2 C1 H1A 126.0 . . ? C3 C1 H1A 126.0 . . ? C2 N2 C1 108.0 . . ? C2 N2 Zn1 107.6(7) . . ? C1 N2 Zn1 144.4(7) . . ? N3 C5 C6 120.0 . . ? N3 C5 C2 115.0(10) . . ? C6 C5 C2 125.0(10) . . ? C5 N3 C9 120.0 . . ? C5 N3 Zn1 117.3(7) . . ? C9 N3 Zn1 122.7(7) . . ? N3 C9 C8 120.0 . . ? N3 C9 H9A 120.0 . . ? C8 C9 H9A 120.0 . . ? C7 C8 C9 120.0 . . ? C7 C8 H8A 120.0 . . ? C9 C8 H8A 120.0 . . ? C6 C7 C8 120.0 . . ? C6 C7 H7A 120.0 . . ? C8 C7 H7A 120.0 . . ? C7 C6 C5 120.0 . . ? C7 C6 H6A 120.0 . . ? C5 C6 H6A 120.0 . . ? C2' C5' N3' 115.6(9) . . ? C2' C5' C6' 124.4(9) . . ? N3' C5' C6' 120.0 . . ? C5' C6' C7' 120.0 . . ? C5' C6' H6'A 120.0 . . ? C7' C6' H6'A 120.0 . . ? C8' C7' C6' 120.0 . . ? C8' C7' H7'A 120.0 . . ? C6' C7' H7'A 120.0 . . ? C7' C8' C9' 120.0 . . ? C7' C8' H8'A 120.0 . . ? C9' C8' H8'A 120.0 . . ? N3' C9' C8' 120.0 . . ? N3' C9' H9'A 120.0 . . ? C8' C9' H9'A 120.0 . . ? C5' N3' C9' 120.0 . . ? C5' N3' Zn1 115.2(7) . . ? C9' N3' Zn1 124.7(7) . . ? N1' C2' N2' 108.0 . . ? N1' C2' C5' 129.1(8) . . ? N2' C2' C5' 122.9(8) . . ? C1' N2' C2' 108.0 . . ? C1' N2' Zn1 145.6(5) . . ? C2' N2' Zn1 106.3(5) . . ? C3' C1' N2' 108.0 . . ? C3' C1' H1'A 126.0 . . ? N2' C1' H1'A 126.0 . . ? N1' C3' C1' 108.0 . . ? N1' C3' H3'A 126.0 . . ? C1' C3' H3'A 126.0 . . ? C3' N1' C2' 108.0 . . ? C3' N1' H1'B 126.0 . . ? C2' N1' H1'B 126.0 . . ? 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 O2 C16 C17 C18 5.1(4) . . . . ? O1 C16 C17 C18 -173.2(2) . . . . ? O2 C16 C17 C22 -176.6(3) . . . . ? O1 C16 C17 C22 5.2(4) . . . . ? C22 C17 C18 C19 -2.8(4) . . . . ? C16 C17 C18 C19 175.6(2) . . . . ? C17 C18 C19 C20 0.3(4) . . . . ? C18 C19 C20 C21 2.3(4) . . . . ? C18 C19 C20 O3 178.3(2) . . . . ? C19 C20 C21 C22 -2.4(4) . . . . ? O3 C20 C21 C22 -178.3(3) . . . . ? C18 C17 C22 C21 2.8(4) . . . . ? C16 C17 C22 C21 -175.6(3) . . . . ? C20 C21 C22 C17 -0.2(5) . . . . ? O2 C16 O1 Zn1 -3.3(3) . . . . ? C17 C16 O1 Zn1 175.0(2) . . . . ? O1 C16 O2 Zn1 3.0(3) . . . . ? C17 C16 O2 Zn1 -175.2(2) . . . . ? C16 O1 Zn1 N3' -87.8(4) . . . . ? C16 O1 Zn1 N3 -161.4(5) . . . . ? C16 O1 Zn1 O4 94.79(17) . . . 4_465 ? C16 O1 Zn1 N2' -168.6(3) . . . . ? C16 O1 Zn1 O5 38.8(3) . . . 4_465 ? C16 O1 Zn1 O2 1.80(16) . . . . ? C16 O1 Zn1 N2 -80.2(4) . . . . ? C16 O1 Zn1 C4 75.28(19) . . . 4_465 ? C16 O2 Zn1 N3' 97.7(4) . . . . ? C16 O2 Zn1 N3 45.1(9) . . . . ? C16 O2 Zn1 O1 -1.83(16) . . . . ? C16 O2 Zn1 O4 -103.74(17) . . . 4_465 ? C16 O2 Zn1 N2' 21.1(7) . . . . ? C16 O2 Zn1 O5 -164.62(17) . . . 4_465 ? C16 O2 Zn1 N2 103.8(4) . . . . ? C16 O2 Zn1 C4 -134.19(17) . . . 4_465 ? O2 C16 Zn1 N3' -85.8(4) . . . . ? O1 C16 Zn1 N3' 97.3(4) . . . . ? O2 C16 Zn1 N3 -158.5(5) . . . . ? O1 C16 Zn1 N3 24.6(6) . . . . ? O2 C16 Zn1 O1 176.9(3) . . . . ? O2 C16 Zn1 O4 83.10(17) . . . 4_465 ? O1 C16 Zn1 O4 -93.75(17) . . . 4_465 ? O2 C16 Zn1 N2' -169.1(4) . . . . ? O1 C16 Zn1 N2' 14.1(4) . . . . ? O2 C16 Zn1 O5 18.6(2) . . . 4_465 ? O1 C16 Zn1 O5 -158.22(16) . . . 4_465 ? O1 C16 Zn1 O2 -176.9(3) . . . . ? O2 C16 Zn1 N2 -77.9(4) . . . . ? O1 C16 Zn1 N2 105.2(4) . . . . ? O2 C16 Zn1 C4 53.19(19) . . . 4_465 ? O1 C16 Zn1 C4 -123.67(17) . . . 4_465 ? C19 C20 O3 C10 118.6(3) . . . . ? C21 C20 O3 C10 -65.3(3) . . . . ? C13 C11 C10 C12 3.6(4) . . . . ? C13 C11 C10 O3 179.6(2) . . . . ? C20 O3 C10 C11 143.2(2) . . . . ? C20 O3 C10 C12 -40.8(3) . . . . ? C11 C10 C12 C15 -1.7(4) . . . . ? O3 C10 C12 C15 -177.5(2) . . . . ? C15 C14 C13 C11 0.2(4) . . . . ? C4 C14 C13 C11 -179.0(2) . . . . ? C10 C11 C13 C14 -2.8(4) . . . . ? C10 C12 C15 C14 -1.0(4) . . . . ? C13 C14 C15 C12 1.8(4) . . . . ? C4 C14 C15 C12 -179.1(2) . . . . ? C13 C14 C4 O4 -8.9(3) . . . . ? C15 C14 C4 O4 172.0(3) . . . . ? C13 C14 C4 O5 170.8(2) . . . . ? C15 C14 C4 O5 -8.3(4) . . . . ? O5 C4 O4 Zn1 4.8(3) . . . 4_766 ? C14 C4 O4 Zn1 -175.47(19) . . . 4_766 ? O4 C4 O5 Zn1 -4.6(3) . . . 4_766 ? C14 C4 O5 Zn1 175.7(2) . . . 4_766 ? N2 C2 N1 C3 0.0 . . . . ? C5 C2 N1 C3 -175.2(19) . . . . ? C2 N1 C3 C1 0.0 . . . . ? N1 C3 C1 N2 0.0 . . . . ? N1 C2 N2 C1 0.0 . . . . ? C5 C2 N2 C1 175.7(17) . . . . ? N1 C2 N2 Zn1 -178.8(10) . . . . ? C5 C2 N2 Zn1 -3.1(13) . . . . ? C3 C1 N2 C2 0.0 . . . . ? C3 C1 N2 Zn1 178.0(16) . . . . ? N3' Zn1 N2 C2 -29(5) . . . . ? N3 Zn1 N2 C2 2.3(8) . . . . ? O1 Zn1 N2 C2 -99.5(7) . . . . ? O4 Zn1 N2 C2 90.5(8) 4_465 . . . ? N2' Zn1 N2 C2 -3.1(7) . . . . ? O5 Zn1 N2 C2 105.9(6) 4_465 . . . ? O2 Zn1 N2 C2 -158.1(6) . . . . ? C4 Zn1 N2 C2 102.4(6) 4_465 . . . ? C16 Zn1 N2 C2 -129.3(6) . . . . ? N3' Zn1 N2 C1 153(7) . . . . ? N3 Zn1 N2 C1 -175.7(16) . . . . ? O1 Zn1 N2 C1 82.6(15) . . . . ? O4 Zn1 N2 C1 -87.5(17) 4_465 . . . ? N2' Zn1 N2 C1 179.0(16) . . . . ? O5 Zn1 N2 C1 -72.1(15) 4_465 . . . ? O2 Zn1 N2 C1 23.9(15) . . . . ? C4 Zn1 N2 C1 -75.6(16) 4_465 . . . ? C16 Zn1 N2 C1 52.8(15) . . . . ? N2 C2 C5 N3 2.3(14) . . . . ? N1 C2 C5 N3 176.9(10) . . . . ? N2 C2 C5 C6 -179.5(8) . . . . ? N1 C2 C5 C6 -5(2) . . . . ? C6 C5 N3 C9 0.0 . . . . ? C2 C5 N3 C9 178.3(12) . . . . ? C6 C5 N3 Zn1 -178.2(9) . . . . ? C2 C5 N3 Zn1 0.1(10) . . . . ? N3' Zn1 N3 C5 3.1(5) . . . . ? O1 Zn1 N3 C5 100.0(5) . . . . ? O4 Zn1 N3 C5 -151.6(5) 4_465 . . . ? N2' Zn1 N3 C5 146(5) . . . . ? O5 Zn1 N3 C5 -90.0(6) 4_465 . . . ? O2 Zn1 N3 C5 59.5(11) . . . . ? N2 Zn1 N3 C5 -1.2(6) . . . . ? C4 Zn1 N3 C5 -121.2(5) 4_465 . . . ? C16 Zn1 N3 C5 87.6(6) . . . . ? N3' Zn1 N3 C9 -175.1(8) . . . . ? O1 Zn1 N3 C9 -78.2(7) . . . . ? O4 Zn1 N3 C9 30.3(7) 4_465 . . . ? N2' Zn1 N3 C9 -32(4) . . . . ? O5 Zn1 N3 C9 91.8(6) 4_465 . . . ? O2 Zn1 N3 C9 -118.7(9) . . . . ? N2 Zn1 N3 C9 -179.4(8) . . . . ? C4 Zn1 N3 C9 60.6(7) 4_465 . . . ? C16 Zn1 N3 C9 -90.6(8) . . . . ? C5 N3 C9 C8 0.0 . . . . ? Zn1 N3 C9 C8 178.1(10) . . . . ? N3 C9 C8 C7 0.0 . . . . ? C9 C8 C7 C6 0.0 . . . . ? C8 C7 C6 C5 0.0 . . . . ? N3 C5 C6 C7 0.0 . . . . ? C2 C5 C6 C7 -178.1(14) . . . . ? C2' C5' C6' C7' 177.5(13) . . . . ? N3' C5' C6' C7' 0.0 . . . . ? C5' C6' C7' C8' 0.0 . . . . ? C6' C7' C8' C9' 0.0 . . . . ? C7' C8' C9' N3' 0.0 . . . . ? C2' C5' N3' C9' -177.7(12) . . . . ? C6' C5' N3' C9' 0.0 . . . . ? C2' C5' N3' Zn1 5.5(9) . . . . ? C6' C5' N3' Zn1 -176.8(7) . . . . ? C8' C9' N3' C5' 0.0 . . . . ? C8' C9' N3' Zn1 176.5(8) . . . . ? N3 Zn1 N3' C5' 3.1(6) . . . . ? O1 Zn1 N3' C5' -98.2(5) . . . . ? O4 Zn1 N3' C5' 76.2(8) 4_465 . . . ? N2' Zn1 N3' C5' -3.0(6) . . . . ? O5 Zn1 N3' C5' 105.1(5) 4_465 . . . ? O2 Zn1 N3' C5' -158.2(5) . . . . ? N2 Zn1 N3' C5' 151(6) . . . . ? C4 Zn1 N3' C5' 97.9(5) 4_465 . . . ? C16 Zn1 N3' C5' -128.6(5) . . . . ? N3 Zn1 N3' C9' -173.6(9) . . . . ? O1 Zn1 N3' C9' 85.2(7) . . . . ? O4 Zn1 N3' C9' -100.5(9) 4_465 . . . ? N2' Zn1 N3' C9' -179.7(8) . . . . ? O5 Zn1 N3' C9' -71.5(7) 4_465 . . . ? O2 Zn1 N3' C9' 25.2(7) . . . . ? N2 Zn1 N3' C9' -26(5) . . . . ? C4 Zn1 N3' C9' -78.7(7) 4_465 . . . ? C16 Zn1 N3' C9' 54.8(7) . . . . ? N3' C5' C2' N1' 175.5(7) . . . . ? C6' C5' C2' N1' -2.2(15) . . . . ? N3' C5' C2' N2' -5.7(11) . . . . ? C6' C5' C2' N2' 176.7(5) . . . . ? N1' C2' N2' C1' 0.0 . . . . ? C5' C2' N2' C1' -179.0(11) . . . . ? N1' C2' N2' Zn1 -178.1(7) . . . . ? C5' C2' N2' Zn1 2.9(9) . . . . ? N3' Zn1 N2' C1' -176.5(11) . . . . ? N3 Zn1 N2' C1' 148(5) . . . . ? O1 Zn1 N2' C1' -76.8(10) . . . . ? O4 Zn1 N2' C1' 29.2(10) 4_465 . . . ? O5 Zn1 N2' C1' 89.4(10) 4_465 . . . ? O2 Zn1 N2' C1' -96.6(12) . . . . ? N2 Zn1 N2' C1' 179.9(11) . . . . ? C4 Zn1 N2' C1' 58.0(10) 4_465 . . . ? C16 Zn1 N2' C1' -83.9(11) . . . . ? N3' Zn1 N2' C2' 0.2(5) . . . . ? N3 Zn1 N2' C2' -35(4) . . . . ? O1 Zn1 N2' C2' 99.9(4) . . . . ? O4 Zn1 N2' C2' -154.0(4) 4_465 . . . ? O5 Zn1 N2' C2' -93.9(4) 4_465 . . . ? O2 Zn1 N2' C2' 80.1(8) . . . . ? N2 Zn1 N2' C2' -3.3(6) . . . . ? C4 Zn1 N2' C2' -125.2(4) 4_465 . . . ? C16 Zn1 N2' C2' 92.8(4) . . . . ? C2' N2' C1' C3' 0.0 . . . . ? Zn1 N2' C1' C3' 176.7(12) . . . . ? N2' C1' C3' N1' 0.0 . . . . ? C1' C3' N1' C2' 0.0 . . . . ? N2' C2' N1' C3' 0.0 . . . . ? C5' C2' N1' C3' 179.0(12) . . . . ? 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 N1 H1B O5 0.86 2.40 3.175(11) 151.0 2_646 _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.391 _refine_diff_density_min -0.588 _refine_diff_density_rms 0.047 data_2 _database_code_depnum_ccdc_archive 'CCDC 687549' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H15 Cd N3 O5' _chemical_formula_weight 513.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.7140(4) _cell_length_b 16.0590(4) _cell_length_c 11.2640(5) _cell_angle_alpha 90.00 _cell_angle_beta 96.4820(10) _cell_angle_gamma 90.00 _cell_volume 2105.38(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.75 _cell_measurement_theta_max 28.29 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.621 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1024 _exptl_absorpt_coefficient_mu 1.076 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.678 _exptl_absorpt_correction_T_max 0.756 _exptl_absorpt_process_details 'SADABS(Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12844 _diffrn_reflns_av_R_equivalents 0.0202 _diffrn_reflns_av_sigmaI/netI 0.0250 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 28.29 _reflns_number_total 5054 _reflns_number_gt 4229 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SMART (Bruker, 1997)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97(Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material SHELXL-97 _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^)+(0.0317P)^2^+0.2721P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5054 _refine_ls_number_parameters 284 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0334 _refine_ls_R_factor_gt 0.0250 _refine_ls_wR_factor_ref 0.0639 _refine_ls_wR_factor_gt 0.0603 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.511767(12) 0.454350(9) 0.152860(12) 0.03386(6) Uani 1 1 d . . . O1 O -0.37762(11) 0.01642(9) 0.50686(12) 0.0374(3) Uani 1 1 d . . . O5 O 0.39117(12) 0.34834(9) 0.11499(12) 0.0417(3) Uani 1 1 d . . . O2 O -0.32414(13) 0.14154(10) 0.57113(15) 0.0522(4) Uani 1 1 d . . . N2 N 0.52546(16) 0.62997(12) 0.44486(17) 0.0436(4) Uani 1 1 d . . . O4 O 0.42395(15) 0.35688(11) 0.30993(14) 0.0570(4) Uani 1 1 d . . . O3 O 0.07801(14) 0.05046(9) 0.25710(17) 0.0574(5) Uani 1 1 d . . . N1 N 0.48869(15) 0.56792(11) 0.27063(16) 0.0389(4) Uani 1 1 d . . . N3 N 0.65737(16) 0.44904(11) 0.32030(17) 0.0421(4) Uani 1 1 d . . . C10 C 0.29860(15) 0.24994(12) 0.22789(17) 0.0330(4) Uani 1 1 d . . . C19 C -0.20419(16) 0.07101(13) 0.44741(18) 0.0340(4) Uani 1 1 d . . . C4 C 0.64325(17) 0.50448(14) 0.40683(18) 0.0392(5) Uani 1 1 d . . . C3 C 0.55251(18) 0.56575(13) 0.37555(18) 0.0370(5) Uani 1 1 d . . . C9 C 0.37698(16) 0.32252(12) 0.21765(18) 0.0340(4) Uani 1 1 d . . . C17 C -0.08121(18) -0.00843(14) 0.33293(19) 0.0414(5) Uani 1 1 d . . . H17 H -0.0628 -0.0586 0.2985 0.050 Uiso 1 1 calc R . . C2 C 0.4417(2) 0.67503(15) 0.3809(2) 0.0487(5) Uani 1 1 d . . . H2 H 0.4064 0.7228 0.4059 0.058 Uiso 1 1 calc R . . C15 C 0.30879(17) 0.20142(13) 0.32968(18) 0.0394(5) Uani 1 1 d . . . H15 H 0.3651 0.2138 0.3922 0.047 Uiso 1 1 calc R . . C18 C -0.17723(17) -0.00280(13) 0.39263(18) 0.0369(4) Uani 1 1 d . . . H18 H -0.2246 -0.0490 0.3963 0.044 Uiso 1 1 calc R . . C1 C 0.41964(19) 0.63680(14) 0.2740(2) 0.0473(5) Uani 1 1 d . . . H1 H 0.3658 0.6544 0.2121 0.057 Uiso 1 1 calc R . . C14 C 0.23629(19) 0.13477(14) 0.3395(2) 0.0448(5) Uani 1 1 d . . . H14 H 0.2448 0.1014 0.4074 0.054 Uiso 1 1 calc R . . C21 C -0.13234(18) 0.13898(14) 0.4407(2) 0.0479(5) Uani 1 1 d . . . H21 H -0.1481 0.1883 0.4790 0.057 Uiso 1 1 calc R . . C20 C -0.30862(17) 0.07823(14) 0.51232(18) 0.0362(4) Uani 1 1 d . . . C16 C -0.01210(17) 0.06092(14) 0.3243(2) 0.0400(5) Uani 1 1 d . . . C22 C -0.03749(19) 0.13482(15) 0.3780(2) 0.0510(6) Uani 1 1 d . . . H22 H 0.0087 0.1814 0.3721 0.061 Uiso 1 1 calc R . . C12 C 0.1407(2) 0.16450(17) 0.1456(2) 0.0555(6) Uani 1 1 d . . . H12 H 0.0841 0.1518 0.0836 0.067 Uiso 1 1 calc R . . C13 C 0.15157(18) 0.11819(14) 0.2484(2) 0.0438(5) Uani 1 1 d . . . C8 C 0.7409(2) 0.39273(17) 0.3414(2) 0.0588(7) Uani 1 1 d . . . H8 H 0.7511 0.3541 0.2820 0.071 Uiso 1 1 calc R . . C11 C 0.21511(19) 0.23059(16) 0.1351(2) 0.0493(6) Uani 1 1 d . . . H11 H 0.2088 0.2621 0.0654 0.059 Uiso 1 1 calc R . . C6 C 0.7968(3) 0.4447(2) 0.5343(3) 0.0805(10) Uani 1 1 d . . . H6 H 0.8438 0.4428 0.6065 0.097 Uiso 1 1 calc R . . C7 C 0.8120(3) 0.3890(2) 0.4457(3) 0.0763(9) Uani 1 1 d . . . H7 H 0.8700 0.3492 0.4565 0.092 Uiso 1 1 calc R . . C5 C 0.7110(2) 0.50357(18) 0.5157(2) 0.0601(7) Uani 1 1 d . . . H5 H 0.6989 0.5418 0.5750 0.072 Uiso 1 1 calc R . . H1N H 0.554(3) 0.6376(19) 0.519(3) 0.088(10) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.03444(9) 0.03569(9) 0.03298(9) -0.00440(6) 0.01056(6) -0.00499(6) O1 0.0298(7) 0.0472(8) 0.0370(8) 0.0001(6) 0.0112(6) -0.0057(6) O5 0.0454(8) 0.0432(9) 0.0374(8) 0.0068(6) 0.0081(6) -0.0109(7) O2 0.0531(9) 0.0429(9) 0.0653(11) -0.0055(8) 0.0265(8) -0.0003(7) N2 0.0513(11) 0.0425(11) 0.0376(10) -0.0099(8) 0.0083(8) -0.0088(9) O4 0.0706(11) 0.0594(11) 0.0417(9) -0.0093(8) 0.0095(8) -0.0262(9) O3 0.0513(10) 0.0475(10) 0.0809(13) -0.0121(8) 0.0406(9) -0.0182(7) N1 0.0412(10) 0.0378(10) 0.0378(10) -0.0064(7) 0.0053(8) -0.0031(7) N3 0.0425(10) 0.0418(11) 0.0420(10) -0.0014(8) 0.0048(8) 0.0001(8) C10 0.0296(9) 0.0374(11) 0.0335(10) 0.0022(8) 0.0107(7) -0.0028(8) C19 0.0301(9) 0.0359(10) 0.0372(11) 0.0045(8) 0.0093(8) -0.0023(8) C4 0.0423(11) 0.0404(12) 0.0356(11) 0.0008(9) 0.0075(9) -0.0091(9) C3 0.0416(11) 0.0364(11) 0.0348(11) -0.0049(8) 0.0118(9) -0.0082(9) C9 0.0306(9) 0.0340(10) 0.0383(11) -0.0012(8) 0.0078(8) -0.0006(8) C17 0.0408(11) 0.0391(12) 0.0470(12) -0.0046(10) 0.0168(9) -0.0064(9) C2 0.0523(13) 0.0400(12) 0.0551(14) -0.0113(10) 0.0113(11) -0.0012(10) C15 0.0372(11) 0.0464(12) 0.0351(11) 0.0037(9) 0.0059(8) -0.0033(9) C18 0.0356(10) 0.0367(12) 0.0399(11) 0.0022(9) 0.0112(8) -0.0093(8) C1 0.0477(13) 0.0406(12) 0.0527(14) -0.0081(10) 0.0020(10) 0.0049(10) C14 0.0493(12) 0.0447(13) 0.0429(12) 0.0105(10) 0.0159(10) -0.0010(10) C21 0.0436(12) 0.0367(12) 0.0669(15) -0.0061(11) 0.0214(11) -0.0064(9) C20 0.0331(10) 0.0415(11) 0.0349(10) 0.0059(9) 0.0084(8) 0.0038(9) C16 0.0333(11) 0.0448(13) 0.0444(12) 0.0003(9) 0.0148(9) -0.0065(8) C22 0.0433(12) 0.0378(12) 0.0760(17) -0.0052(11) 0.0251(12) -0.0132(10) C12 0.0425(12) 0.0716(18) 0.0513(14) 0.0009(12) 0.0010(10) -0.0207(12) C13 0.0386(11) 0.0410(12) 0.0563(14) -0.0034(10) 0.0254(10) -0.0100(9) C8 0.0578(15) 0.0567(16) 0.0603(16) -0.0061(12) -0.0001(12) 0.0113(12) C11 0.0474(12) 0.0623(16) 0.0371(12) 0.0128(11) -0.0004(9) -0.0147(11) C6 0.085(2) 0.082(2) 0.066(2) -0.0035(16) -0.0284(17) 0.0171(17) C7 0.0724(19) 0.074(2) 0.076(2) -0.0038(16) -0.0180(16) 0.0269(16) C5 0.0699(17) 0.0617(17) 0.0460(14) -0.0049(12) -0.0055(12) 0.0016(14) _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 2.2225(14) . ? Cd1 O1 2.2550(13) 4_665 ? Cd1 N1 2.2892(17) . ? Cd1 N3 2.3973(18) . ? Cd1 O1 2.4620(14) 2 ? O1 C20 1.277(2) . ? O1 Cd1 2.2550(13) 4_466 ? O1 Cd1 2.4620(14) 2_545 ? O5 C9 1.257(2) . ? O2 C20 1.238(3) . ? N2 C3 1.353(3) . ? N2 C2 1.358(3) . ? N2 H1N 0.87(3) . ? O4 C9 1.248(2) . ? O3 C16 1.377(2) . ? O3 C13 1.398(2) . ? N1 C3 1.326(3) . ? N1 C1 1.373(3) . ? N3 C8 1.334(3) . ? N3 C4 1.344(3) . ? C10 C15 1.380(3) . ? C10 C11 1.384(3) . ? C10 C9 1.496(3) . ? C19 C21 1.386(3) . ? C19 C18 1.389(3) . ? C19 C20 1.499(3) . ? C4 C5 1.384(3) . ? C4 C3 1.462(3) . ? C17 C18 1.377(3) . ? C17 C16 1.387(3) . ? C17 H17 0.9300 . ? C2 C1 1.350(3) . ? C2 H2 0.9300 . ? C15 C14 1.379(3) . ? C15 H15 0.9300 . ? C18 H18 0.9300 . ? C1 H1 0.9300 . ? C14 C13 1.371(3) . ? C14 H14 0.9300 . ? C21 C22 1.384(3) . ? C21 H21 0.9300 . ? C16 C22 1.379(3) . ? C22 H22 0.9300 . ? C12 C13 1.370(3) . ? C12 C11 1.387(3) . ? C12 H12 0.9300 . ? C8 C7 1.363(4) . ? C8 H8 0.9300 . ? C11 H11 0.9300 . ? C6 C7 1.367(4) . ? C6 C5 1.379(4) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C5 H5 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 O5 Cd1 O1 115.12(5) . 4_665 ? O5 Cd1 N1 127.40(6) . . ? O1 Cd1 N1 111.84(6) 4_665 . ? O5 Cd1 N3 120.27(6) . . ? O1 Cd1 N3 99.49(6) 4_665 . ? N1 Cd1 N3 72.09(6) . . ? O5 Cd1 O1 80.24(5) . 2 ? O1 Cd1 O1 75.80(5) 4_665 2 ? N1 Cd1 O1 89.63(6) . 2 ? N3 Cd1 O1 158.13(5) . 2 ? C20 O1 Cd1 102.46(12) . 4_466 ? C20 O1 Cd1 134.28(12) . 2_545 ? Cd1 O1 Cd1 104.20(5) 4_466 2_545 ? C9 O5 Cd1 102.91(12) . . ? C3 N2 C2 107.60(19) . . ? C3 N2 H1N 125(2) . . ? C2 N2 H1N 127(2) . . ? C16 O3 C13 117.42(17) . . ? C3 N1 C1 105.73(17) . . ? C3 N1 Cd1 113.83(14) . . ? C1 N1 Cd1 140.02(14) . . ? C8 N3 C4 117.9(2) . . ? C8 N3 Cd1 127.36(16) . . ? C4 N3 Cd1 114.34(14) . . ? C15 C10 C11 119.22(19) . . ? C15 C10 C9 120.50(18) . . ? C11 C10 C9 120.29(18) . . ? C21 C19 C18 118.56(18) . . ? C21 C19 C20 119.99(19) . . ? C18 C19 C20 121.45(18) . . ? N3 C4 C5 122.1(2) . . ? N3 C4 C3 114.63(18) . . ? C5 C4 C3 123.3(2) . . ? N1 C3 N2 110.44(19) . . ? N1 C3 C4 123.65(18) . . ? N2 C3 C4 125.8(2) . . ? O4 C9 O5 121.90(18) . . ? O4 C9 C10 119.78(18) . . ? O5 C9 C10 118.29(17) . . ? C18 C17 C16 119.8(2) . . ? C18 C17 H17 120.1 . . ? C16 C17 H17 120.1 . . ? C1 C2 N2 106.5(2) . . ? C1 C2 H2 126.7 . . ? N2 C2 H2 126.7 . . ? C14 C15 C10 120.59(19) . . ? C14 C15 H15 119.7 . . ? C10 C15 H15 119.7 . . ? C17 C18 C19 120.81(19) . . ? C17 C18 H18 119.6 . . ? C19 C18 H18 119.6 . . ? C2 C1 N1 109.7(2) . . ? C2 C1 H1 125.2 . . ? N1 C1 H1 125.2 . . ? C13 C14 C15 119.4(2) . . ? C13 C14 H14 120.3 . . ? C15 C14 H14 120.3 . . ? C22 C21 C19 121.2(2) . . ? C22 C21 H21 119.4 . . ? C19 C21 H21 119.4 . . ? O2 C20 O1 122.26(18) . . ? O2 C20 C19 120.12(19) . . ? O1 C20 C19 117.60(19) . . ? O3 C16 C22 124.23(19) . . ? O3 C16 C17 115.50(19) . . ? C22 C16 C17 120.24(19) . . ? C16 C22 C21 119.4(2) . . ? C16 C22 H22 120.3 . . ? C21 C22 H22 120.3 . . ? C13 C12 C11 119.2(2) . . ? C13 C12 H12 120.4 . . ? C11 C12 H12 120.4 . . ? C12 C13 C14 121.2(2) . . ? C12 C13 O3 118.9(2) . . ? C14 C13 O3 119.9(2) . . ? N3 C8 C7 123.3(2) . . ? N3 C8 H8 118.4 . . ? C7 C8 H8 118.4 . . ? C10 C11 C12 120.3(2) . . ? C10 C11 H11 119.8 . . ? C12 C11 H11 119.8 . . ? C7 C6 C5 119.4(3) . . ? C7 C6 H6 120.3 . . ? C5 C6 H6 120.3 . . ? C8 C7 C6 118.9(3) . . ? C8 C7 H7 120.6 . . ? C6 C7 H7 120.6 . . ? C6 C5 C4 118.5(3) . . ? C6 C5 H5 120.8 . . ? C4 C5 H5 120.8 . . ? 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 O5 C9 153.72(12) 4_665 . . . ? N1 Cd1 O5 C9 -55.15(15) . . . . ? N3 Cd1 O5 C9 34.74(15) . . . . ? O1 Cd1 O5 C9 -137.12(13) 2 . . . ? O5 Cd1 N1 C3 104.98(14) . . . . ? O1 Cd1 N1 C3 -103.12(14) 4_665 . . . ? N3 Cd1 N1 C3 -9.85(13) . . . . ? O1 Cd1 N1 C3 -177.64(14) 2 . . . ? O5 Cd1 N1 C1 -66.1(2) . . . . ? O1 Cd1 N1 C1 85.8(2) 4_665 . . . ? N3 Cd1 N1 C1 179.1(2) . . . . ? O1 Cd1 N1 C1 11.3(2) 2 . . . ? O5 Cd1 N3 C8 59.0(2) . . . . ? O1 Cd1 N3 C8 -67.6(2) 4_665 . . . ? N1 Cd1 N3 C8 -177.6(2) . . . . ? O1 Cd1 N3 C8 -143.00(19) 2 . . . ? O5 Cd1 N3 C4 -113.30(14) . . . . ? O1 Cd1 N3 C4 120.12(15) 4_665 . . . ? N1 Cd1 N3 C4 10.10(14) . . . . ? O1 Cd1 N3 C4 44.7(2) 2 . . . ? C8 N3 C4 C5 -1.0(3) . . . . ? Cd1 N3 C4 C5 172.11(18) . . . . ? C8 N3 C4 C3 178.1(2) . . . . ? Cd1 N3 C4 C3 -8.8(2) . . . . ? C1 N1 C3 N2 0.6(2) . . . . ? Cd1 N1 C3 N2 -173.48(14) . . . . ? C1 N1 C3 C4 -176.2(2) . . . . ? Cd1 N1 C3 C4 9.7(2) . . . . ? C2 N2 C3 N1 -0.5(2) . . . . ? C2 N2 C3 C4 176.3(2) . . . . ? N3 C4 C3 N1 -0.4(3) . . . . ? C5 C4 C3 N1 178.7(2) . . . . ? N3 C4 C3 N2 -176.69(19) . . . . ? C5 C4 C3 N2 2.4(3) . . . . ? Cd1 O5 C9 O4 1.5(2) . . . . ? Cd1 O5 C9 C10 179.71(14) . . . . ? C15 C10 C9 O4 -24.1(3) . . . . ? C11 C10 C9 O4 156.1(2) . . . . ? C15 C10 C9 O5 157.67(19) . . . . ? C11 C10 C9 O5 -22.2(3) . . . . ? C3 N2 C2 C1 0.1(3) . . . . ? C11 C10 C15 C14 -0.5(3) . . . . ? C9 C10 C15 C14 179.68(19) . . . . ? C16 C17 C18 C19 -1.8(3) . . . . ? C21 C19 C18 C17 0.0(3) . . . . ? C20 C19 C18 C17 179.76(19) . . . . ? N2 C2 C1 N1 0.2(3) . . . . ? C3 N1 C1 C2 -0.5(2) . . . . ? Cd1 N1 C1 C2 171.03(17) . . . . ? C10 C15 C14 C13 -1.7(3) . . . . ? C18 C19 C21 C22 1.9(3) . . . . ? C20 C19 C21 C22 -177.8(2) . . . . ? Cd1 O1 C20 O2 -12.1(2) 4_466 . . . ? Cd1 O1 C20 O2 112.4(2) 2_545 . . . ? Cd1 O1 C20 C19 166.03(14) 4_466 . . . ? Cd1 O1 C20 C19 -69.5(2) 2_545 . . . ? C21 C19 C20 O2 -8.0(3) . . . . ? C18 C19 C20 O2 172.2(2) . . . . ? C21 C19 C20 O1 173.80(19) . . . . ? C18 C19 C20 O1 -5.9(3) . . . . ? C13 O3 C16 C22 3.5(3) . . . . ? C13 O3 C16 C17 -178.5(2) . . . . ? C18 C17 C16 O3 -176.4(2) . . . . ? C18 C17 C16 C22 1.7(3) . . . . ? O3 C16 C22 C21 178.1(2) . . . . ? C17 C16 C22 C21 0.2(4) . . . . ? C19 C21 C22 C16 -2.0(4) . . . . ? C11 C12 C13 C14 -1.6(4) . . . . ? C11 C12 C13 O3 -178.5(2) . . . . ? C15 C14 C13 C12 2.8(3) . . . . ? C15 C14 C13 O3 179.61(19) . . . . ? C16 O3 C13 C12 -102.8(3) . . . . ? C16 O3 C13 C14 80.3(3) . . . . ? C4 N3 C8 C7 -0.1(4) . . . . ? Cd1 N3 C8 C7 -172.2(2) . . . . ? C15 C10 C11 C12 1.6(3) . . . . ? C9 C10 C11 C12 -178.5(2) . . . . ? C13 C12 C11 C10 -0.6(4) . . . . ? N3 C8 C7 C6 0.9(5) . . . . ? C5 C6 C7 C8 -0.6(5) . . . . ? C7 C6 C5 C4 -0.4(5) . . . . ? N3 C4 C5 C6 1.2(4) . . . . ? C3 C4 C5 C6 -177.8(3) . . . . ? 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 N2 H1N O4 0.87(3) 1.92(3) 2.767(2) 164(3) 3_666 _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.377 _refine_diff_density_min -0.426 _refine_diff_density_rms 0.070 data_3 _database_code_depnum_ccdc_archive 'CCDC 687550' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H52 N6 O18 Zn2' _chemical_formula_weight 1131.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 17.309(3) _cell_length_b 16.441(2) _cell_length_c 18.128(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.439(3) _cell_angle_gamma 90.00 _cell_volume 5154.1(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.59 _cell_measurement_theta_max 26.43 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.458 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2344 _exptl_absorpt_coefficient_mu 1.009 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.754 _exptl_absorpt_correction_T_max 0.769 _exptl_absorpt_process_details 'SADABS(Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27392 _diffrn_reflns_av_R_equivalents 0.0454 _diffrn_reflns_av_sigmaI/netI 0.0578 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 26.43 _reflns_number_total 10240 _reflns_number_gt 6957 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SMART (Bruker, 1997)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97(Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material SHELXL-97 _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^)+(0.0718P)^2^+4.5564P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10240 _refine_ls_number_parameters 715 _refine_ls_number_restraints 26 _refine_ls_R_factor_all 0.0868 _refine_ls_R_factor_gt 0.0584 _refine_ls_wR_factor_ref 0.1572 _refine_ls_wR_factor_gt 0.1421 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.015 _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 0.27597(3) 0.50093(3) 0.77244(3) 0.04213(14) Uani 1 1 d . . . Zn2 Zn 0.29169(3) -0.00625(3) 0.20914(2) 0.03965(14) Uani 1 1 d . . . O10 O -0.18637(17) -0.51630(18) 0.59543(16) 0.0520(7) Uani 1 1 d . . . N6 N 0.25581(17) 0.20018(18) 0.32783(16) 0.0349(7) Uani 1 1 d . . . O8 O -0.00044(19) -0.36644(19) 0.33179(15) 0.0596(9) Uani 1 1 d . . . N3 N 0.25233(18) 0.28462(19) 0.66326(16) 0.0371(7) Uani 1 1 d . . . O9 O -0.13614(18) -0.40861(18) 0.65063(16) 0.0535(7) Uani 1 1 d . . . O7 O 0.18965(18) -0.07397(17) 0.20646(16) 0.0520(7) Uani 1 1 d . . . N5 N 0.38405(18) 0.03364(19) 0.27827(17) 0.0376(7) Uani 1 1 d . . . O5 O 0.49025(19) 0.61755(19) 1.16962(16) 0.0604(9) Uani 1 1 d . . . C17 C 0.2843(2) 0.3551(2) 0.68756(19) 0.0335(8) Uani 1 1 d . . . O6 O 0.26470(19) -0.0991(2) 0.30263(19) 0.0640(9) Uani 1 1 d . . . O2 O 0.2819(2) 0.4728(2) 0.90109(19) 0.0730(10) Uani 1 1 d . . . C48 C -0.1439(2) -0.4530(2) 0.5944(2) 0.0425(9) Uani 1 1 d . . . C25 C 0.2641(3) 0.2100(2) 0.4649(2) 0.0447(10) Uani 1 1 d . . . H25A H 0.3064 0.1725 0.4753 0.054 Uiso 1 1 calc R . . H25B H 0.2165 0.1788 0.4614 0.054 Uiso 1 1 calc R . . C26 C 0.2759(2) 0.2523(2) 0.39199(19) 0.0381(8) Uani 1 1 d . . . H26A H 0.2443 0.3011 0.3893 0.046 Uiso 1 1 calc R . . H26B H 0.3296 0.2688 0.3900 0.046 Uiso 1 1 calc R . . N2 N 0.36715(19) 0.4663(2) 0.70513(19) 0.0443(8) Uani 1 1 d . . . O1 O 0.34829(19) 0.5650(2) 0.84456(17) 0.0636(9) Uani 1 1 d . . . N1 N 0.24076(18) 0.3883(2) 0.73853(16) 0.0385(7) Uani 1 1 d . . . C29 C 0.2922(2) 0.1345(2) 0.30074(18) 0.0320(8) Uani 1 1 d . . . C16 C 0.1860(2) 0.2724(3) 0.7008(2) 0.0442(9) Uani 1 1 d . . . H16 H 0.1523 0.2285 0.6958 0.053 Uiso 1 1 calc R . . N4 N 0.24824(18) 0.10131(19) 0.24682(17) 0.0372(7) Uani 1 1 d . . . C23 C 0.2743(2) 0.2311(2) 0.60221(18) 0.0365(8) Uani 1 1 d . . . H23A H 0.2448 0.1810 0.6039 0.044 Uiso 1 1 calc R . . H23B H 0.3287 0.2173 0.6086 0.044 Uiso 1 1 calc R . . C30 C 0.3692(2) 0.1008(2) 0.31898(19) 0.0351(8) Uani 1 1 d . . . C35 C 0.2042(2) -0.1125(2) 0.2657(2) 0.0441(10) Uani 1 1 d . . . C36 C 0.1487(2) -0.1759(2) 0.2895(2) 0.0392(9) Uani 1 1 d . . . C11 C 0.6369(2) 0.8150(2) 1.2048(2) 0.0449(10) Uani 1 1 d . . . C5 C 0.4551(2) 0.5973(3) 1.1020(2) 0.0469(10) Uani 1 1 d . . . C1 C 0.3326(3) 0.5264(3) 0.9027(3) 0.0515(11) Uani 1 1 d . . . C39 C 0.0488(2) -0.3000(2) 0.3242(2) 0.0457(10) Uani 1 1 d . . . C42 C -0.0306(2) -0.3859(2) 0.3988(2) 0.0449(10) Uani 1 1 d . . . C31 C 0.4242(2) 0.1311(3) 0.3690(2) 0.0455(10) Uani 1 1 d . . . H31 H 0.4135 0.1764 0.3975 0.055 Uiso 1 1 calc R . . C38 C 0.0265(2) -0.2448(3) 0.2700(2) 0.0495(10) Uani 1 1 d . . . H38 H -0.0218 -0.2487 0.2458 0.059 Uiso 1 1 calc R . . C44 C -0.1134(3) -0.4760(3) 0.4617(2) 0.0522(11) Uani 1 1 d . . . H44 H -0.1450 -0.5219 0.4611 0.063 Uiso 1 1 calc R . . C24 C 0.2600(2) 0.2709(2) 0.52759(19) 0.0421(9) Uani 1 1 d . . . H24A H 0.2983 0.3132 0.5212 0.051 Uiso 1 1 calc R . . H24B H 0.2094 0.2963 0.5258 0.051 Uiso 1 1 calc R . . C8 C 0.5389(2) 0.6848(3) 1.1766(2) 0.0468(10) Uani 1 1 d . . . C18 C 0.3570(2) 0.3950(2) 0.66881(19) 0.0362(8) Uani 1 1 d . . . C28 C 0.1823(2) 0.1468(3) 0.2391(2) 0.0498(10) Uani 1 1 d . . . H28 H 0.1413 0.1369 0.2055 0.060 Uiso 1 1 calc R . . C2 C 0.3759(2) 0.5493(2) 0.9727(2) 0.0425(9) Uani 1 1 d . . . C37 C 0.0769(2) -0.1839(3) 0.2525(2) 0.0480(10) Uani 1 1 d . . . H37 H 0.0628 -0.1474 0.2151 0.058 Uiso 1 1 calc R . . C43 C -0.0773(3) -0.4537(3) 0.3979(3) 0.0581(12) Uani 1 1 d . . . H43 H -0.0845 -0.4843 0.3550 0.070 Uiso 1 1 calc R . . C12 C 0.5705(2) 0.8054(3) 1.2435(2) 0.0492(10) Uani 1 1 d . . . H12 H 0.5590 0.8432 1.2796 0.059 Uiso 1 1 calc R . . C13 C 0.5208(2) 0.7413(3) 1.2298(2) 0.0515(11) Uani 1 1 d . . . H13 H 0.4759 0.7360 1.2559 0.062 Uiso 1 1 calc R . . C4 C 0.4657(3) 0.6382(3) 1.0378(2) 0.0566(12) Uani 1 1 d . . . H4 H 0.4989 0.6826 1.0373 0.068 Uiso 1 1 calc R . . C46 C -0.0191(3) -0.3415(3) 0.4626(2) 0.0542(12) Uani 1 1 d . . . H46 H 0.0131 -0.2962 0.4635 0.065 Uiso 1 1 calc R . . C33 C 0.5106(3) 0.0274(3) 0.3339(3) 0.0553(11) Uani 1 1 d . . . H33 H 0.5585 0.0017 0.3380 0.066 Uiso 1 1 calc R . . C19 C 0.4125(2) 0.3655(3) 0.6239(2) 0.0492(10) Uani 1 1 d . . . H19 H 0.4050 0.3164 0.5991 0.059 Uiso 1 1 calc R . . C47 C -0.1034(2) -0.4314(2) 0.5261(2) 0.0403(9) Uani 1 1 d . . . C41 C 0.1686(2) -0.2311(3) 0.3451(2) 0.0480(10) Uani 1 1 d . . . H41 H 0.2159 -0.2259 0.3710 0.058 Uiso 1 1 calc R . . C10 C 0.6535(2) 0.7577(3) 1.1514(2) 0.0525(11) Uani 1 1 d . . . H10 H 0.6977 0.7638 1.1244 0.063 Uiso 1 1 calc R . . C34 C 0.4532(2) -0.0009(3) 0.2848(3) 0.0487(10) Uani 1 1 d . . . H34 H 0.4636 -0.0456 0.2554 0.058 Uiso 1 1 calc R . . C27 C 0.1865(2) 0.2090(3) 0.2886(2) 0.0453(10) Uani 1 1 d . . . H27 H 0.1498 0.2494 0.2947 0.054 Uiso 1 1 calc R . . C40 C 0.1189(3) -0.2938(3) 0.3625(2) 0.0515(11) Uani 1 1 d . . . H40 H 0.1327 -0.3310 0.3993 0.062 Uiso 1 1 calc R . . C20 C 0.4797(3) 0.4096(3) 0.6160(3) 0.0617(13) Uani 1 1 d . . . H20 H 0.5175 0.3910 0.5852 0.074 Uiso 1 1 calc R . . C9 C 0.6055(3) 0.6916(3) 1.1377(3) 0.0536(11) Uani 1 1 d . . . H9 H 0.6178 0.6525 1.1030 0.064 Uiso 1 1 calc R . . C6 C 0.4040(3) 0.5328(3) 1.1029(3) 0.0614(13) Uani 1 1 d . . . H6 H 0.3960 0.5055 1.1469 0.074 Uiso 1 1 calc R . . C45 C -0.0560(3) -0.3649(3) 0.5257(2) 0.0507(10) Uani 1 1 d . . . H45 H -0.0484 -0.3347 0.5688 0.061 Uiso 1 1 calc R . . C32 C 0.4954(3) 0.0935(3) 0.3761(2) 0.0546(11) Uani 1 1 d . . . H32 H 0.5330 0.1133 0.4097 0.066 Uiso 1 1 calc R . . C15 C 0.1793(2) 0.3376(3) 0.7469(2) 0.0480(10) Uani 1 1 d . . . H15 H 0.1394 0.3460 0.7788 0.058 Uiso 1 1 calc R . . C3 C 0.4269(3) 0.6133(3) 0.9729(2) 0.0568(12) Uani 1 1 d . . . H3 H 0.4356 0.6404 0.9290 0.068 Uiso 1 1 calc R . . C22 C 0.4325(3) 0.5068(3) 0.6984(3) 0.0630(13) Uani 1 1 d . . . H22 H 0.4398 0.5548 0.7250 0.076 Uiso 1 1 calc R . . C21 C 0.4897(3) 0.4812(3) 0.6542(3) 0.0708(15) Uani 1 1 d . . . H21 H 0.5346 0.5117 0.6500 0.085 Uiso 1 1 calc R . . C7 C 0.3651(3) 0.5091(3) 1.0388(3) 0.0604(13) Uani 1 1 d . . . H7 H 0.3310 0.4654 1.0398 0.072 Uiso 1 1 calc R . . C14 C 0.6913(3) 0.8838(3) 1.2229(3) 0.0527(11) Uani 1 1 d . . . O3 O 0.67600(18) 0.93173(18) 1.2741(2) 0.0626(9) Uani 1 1 d . . . O1W O 0.1219(2) -0.0836(2) 0.0604(2) 0.0711(9) Uani 1 1 d D . . O4 O 0.7510(2) 0.8930(2) 1.1879(2) 0.0758(10) Uani 1 1 d . . . O2W O 0.4894(2) 0.2949(2) 0.4588(2) 0.0803(11) Uani 1 1 d D . . O6W O 0.6421(3) 0.3137(3) 0.4040(4) 0.1219(19) Uani 1 1 d D . . O3W O 0.3664(3) -0.0988(3) 0.4297(2) 0.0946(13) Uani 1 1 d D . . O4W O 0.1331(3) 0.5397(3) 0.9716(3) 0.0915(13) Uani 1 1 d D . . O5W O 0.5190(3) 0.8350(3) 1.4351(2) 0.0868(12) Uani 1 1 d D . . O7W O 0.2016(4) 0.3319(3) 0.9499(3) 0.1261(19) Uani 1 1 d D . . O8W O 0.1689(3) 0.0732(5) 0.0289(5) 0.187(4) Uani 1 1 d D . . H2B H 0.528(4) 0.305(7) 0.437(6) 0.281 Uiso 1 1 d D . . H1B H 0.154(6) -0.084(7) 0.093(5) 0.281 Uiso 1 1 d D . . H1A H 0.112(6) -0.041(4) 0.040(6) 0.281 Uiso 1 1 d D . . H8A H 0.181(7) 0.068(6) -0.013(2) 0.281 Uiso 1 1 d D . . H3A H 0.394(6) -0.137(5) 0.421(7) 0.281 Uiso 1 1 d D . . H3B H 0.327(4) -0.094(7) 0.406(6) 0.281 Uiso 1 1 d D . . H8B H 0.204(5) 0.078(9) 0.060(4) 0.281 Uiso 1 1 d D . . H5B H 0.549(6) 0.870(5) 1.448(7) 0.281 Uiso 1 1 d D . . H4A H 0.125(8) 0.506(6) 1.003(6) 0.281 Uiso 1 1 d D . . H4B H 0.165(6) 0.530(8) 0.942(6) 0.281 Uiso 1 1 d D . . H5A H 0.514(7) 0.797(5) 1.462(6) 0.281 Uiso 1 1 d D . . H7B H 0.227(7) 0.367(5) 0.932(6) 0.281 Uiso 1 1 d D . . H7A H 0.182(7) 0.341(7) 0.988(4) 0.281 Uiso 1 1 d D . . H2A H 0.453(4) 0.325(6) 0.454(7) 0.281 Uiso 1 1 d D . . H6A H 0.658(4) 0.268(3) 0.412(7) 0.281 Uiso 1 1 d D . . H6B H 0.665(6) 0.341(5) 0.375(6) 0.281 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0420(3) 0.0390(3) 0.0452(3) -0.01022(19) 0.00062(19) 0.0035(2) Zn2 0.0439(3) 0.0384(3) 0.0374(2) -0.00985(18) 0.01040(19) -0.0073(2) O10 0.0555(18) 0.0526(18) 0.0491(18) 0.0142(13) 0.0155(14) -0.0048(14) N6 0.0368(17) 0.0356(17) 0.0322(16) -0.0078(12) 0.0022(13) 0.0019(13) O8 0.081(2) 0.0576(19) 0.0421(16) -0.0054(14) 0.0281(15) -0.0302(16) N3 0.0438(18) 0.0383(17) 0.0297(16) -0.0049(13) 0.0068(13) -0.0034(14) O9 0.066(2) 0.0533(18) 0.0429(17) 0.0075(14) 0.0178(14) 0.0038(15) O7 0.068(2) 0.0449(17) 0.0445(17) 0.0046(13) 0.0146(14) -0.0152(14) N5 0.0384(18) 0.0361(17) 0.0389(18) 0.0001(13) 0.0080(13) -0.0012(14) O5 0.072(2) 0.060(2) 0.0479(17) 0.0097(14) -0.0153(15) -0.0294(16) C17 0.0330(19) 0.036(2) 0.0309(18) -0.0042(15) 0.0005(14) 0.0010(15) O6 0.053(2) 0.065(2) 0.074(2) 0.0090(17) -0.0011(16) -0.0192(16) O2 0.092(3) 0.051(2) 0.074(2) -0.0160(17) -0.0270(19) -0.0119(19) C48 0.041(2) 0.042(2) 0.046(2) 0.0153(18) 0.0116(17) 0.0103(18) C25 0.062(3) 0.039(2) 0.033(2) -0.0068(16) 0.0055(18) -0.0032(19) C26 0.050(2) 0.0319(19) 0.0324(19) -0.0063(15) 0.0030(16) -0.0025(17) N2 0.0387(19) 0.0397(18) 0.055(2) -0.0057(16) 0.0080(15) -0.0047(15) O1 0.061(2) 0.084(2) 0.0452(18) -0.0097(17) -0.0051(15) 0.0101(17) N1 0.0359(17) 0.0467(19) 0.0330(17) -0.0116(14) 0.0038(13) -0.0014(14) C29 0.037(2) 0.0321(19) 0.0269(17) -0.0031(14) 0.0043(14) -0.0020(15) C16 0.040(2) 0.050(2) 0.044(2) -0.0041(18) 0.0094(17) -0.0109(18) N4 0.0364(17) 0.0399(18) 0.0354(17) -0.0084(13) 0.0034(13) -0.0023(14) C23 0.049(2) 0.0312(19) 0.0298(18) -0.0027(14) 0.0056(16) -0.0005(16) C30 0.038(2) 0.037(2) 0.0308(18) -0.0010(15) 0.0057(15) -0.0047(16) C35 0.043(2) 0.036(2) 0.055(3) -0.0091(19) 0.0185(19) -0.0023(18) C36 0.039(2) 0.039(2) 0.041(2) -0.0003(16) 0.0142(16) -0.0015(17) C11 0.036(2) 0.040(2) 0.057(3) 0.0029(18) -0.0109(18) -0.0021(17) C5 0.048(2) 0.048(2) 0.043(2) 0.0018(18) -0.0108(18) -0.0080(19) C1 0.058(3) 0.045(2) 0.051(3) -0.015(2) -0.008(2) 0.020(2) C39 0.052(3) 0.043(2) 0.044(2) -0.0074(18) 0.0239(19) -0.0093(19) C42 0.050(2) 0.046(2) 0.040(2) 0.0008(17) 0.0169(18) -0.0052(19) C31 0.043(2) 0.050(2) 0.042(2) -0.0096(18) -0.0035(17) 0.0012(19) C38 0.040(2) 0.058(3) 0.052(2) 0.003(2) 0.0130(18) -0.008(2) C44 0.064(3) 0.045(2) 0.049(3) 0.0036(19) 0.015(2) -0.018(2) C24 0.055(2) 0.038(2) 0.033(2) -0.0030(16) 0.0028(17) 0.0053(18) C8 0.041(2) 0.048(2) 0.050(2) 0.0100(19) -0.0145(19) -0.0087(19) C18 0.037(2) 0.039(2) 0.0337(19) 0.0000(15) 0.0025(15) -0.0019(16) C28 0.040(2) 0.064(3) 0.045(2) -0.012(2) -0.0055(18) 0.005(2) C2 0.045(2) 0.039(2) 0.043(2) -0.0086(17) -0.0042(17) 0.0063(18) C37 0.045(2) 0.045(2) 0.054(3) 0.0065(19) 0.0093(19) 0.0017(19) C43 0.071(3) 0.054(3) 0.050(3) -0.004(2) 0.016(2) -0.026(2) C12 0.041(2) 0.050(3) 0.056(3) -0.008(2) -0.0044(19) 0.0019(19) C13 0.040(2) 0.065(3) 0.049(3) 0.003(2) -0.0054(19) -0.007(2) C4 0.060(3) 0.060(3) 0.049(3) 0.011(2) -0.013(2) -0.020(2) C46 0.070(3) 0.043(2) 0.051(3) -0.007(2) 0.025(2) -0.018(2) C33 0.043(2) 0.065(3) 0.059(3) 0.001(2) 0.004(2) 0.011(2) C19 0.042(2) 0.060(3) 0.047(2) -0.015(2) 0.0094(18) -0.009(2) C47 0.044(2) 0.037(2) 0.041(2) 0.0088(16) 0.0116(17) 0.0061(17) C41 0.043(2) 0.056(3) 0.046(2) 0.0019(19) 0.0078(18) -0.0057(19) C10 0.036(2) 0.058(3) 0.065(3) -0.008(2) 0.0052(19) -0.0060(19) C34 0.050(2) 0.046(2) 0.051(2) 0.0024(18) 0.0091(19) 0.014(2) C27 0.043(2) 0.051(2) 0.042(2) -0.0073(18) -0.0020(17) 0.0106(19) C40 0.063(3) 0.051(3) 0.041(2) 0.0107(19) 0.012(2) 0.001(2) C20 0.046(3) 0.081(4) 0.059(3) -0.017(3) 0.019(2) -0.012(2) C9 0.048(3) 0.047(3) 0.065(3) -0.010(2) -0.004(2) 0.000(2) C6 0.080(3) 0.055(3) 0.048(3) 0.007(2) -0.008(2) -0.025(3) C45 0.063(3) 0.049(3) 0.041(2) -0.0016(19) 0.013(2) -0.005(2) C32 0.043(2) 0.074(3) 0.047(2) -0.006(2) -0.0058(19) 0.003(2) C15 0.040(2) 0.061(3) 0.044(2) -0.011(2) 0.0130(18) -0.0071(19) C3 0.063(3) 0.065(3) 0.042(2) 0.007(2) -0.009(2) -0.012(2) C22 0.063(3) 0.050(3) 0.077(3) -0.016(2) 0.015(2) -0.019(2) C21 0.061(3) 0.071(3) 0.082(4) -0.011(3) 0.028(3) -0.029(3) C7 0.076(3) 0.045(3) 0.059(3) 0.000(2) -0.012(2) -0.020(2) C14 0.050(3) 0.040(2) 0.067(3) 0.009(2) -0.012(2) -0.002(2) O3 0.055(2) 0.0404(18) 0.091(3) -0.0127(17) -0.0063(17) -0.0033(14) O1W 0.066(2) 0.072(2) 0.075(2) -0.0145(18) -0.0002(18) 0.0066(18) O4 0.060(2) 0.072(2) 0.095(3) -0.008(2) 0.011(2) -0.0230(18) O2W 0.081(3) 0.074(3) 0.085(3) -0.011(2) -0.003(2) 0.002(2) O6W 0.112(4) 0.107(4) 0.151(5) 0.042(3) 0.065(3) 0.039(3) O3W 0.081(3) 0.127(4) 0.075(3) 0.033(2) 0.003(2) 0.002(3) O4W 0.077(3) 0.090(3) 0.108(4) -0.033(3) -0.001(2) 0.001(2) O5W 0.087(3) 0.098(3) 0.076(3) -0.005(2) 0.012(2) 0.001(2) O7W 0.149(5) 0.095(4) 0.141(5) -0.040(3) 0.076(4) -0.041(3) O8W 0.112(5) 0.187(7) 0.257(8) 0.129(7) -0.051(5) -0.035(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N1 2.036(3) . ? Zn1 O3 2.056(3) 4_575 ? Zn1 O1 2.061(3) . ? Zn1 N2 2.114(3) . ? Zn1 O4 2.350(4) 4_575 ? Zn1 O2 2.375(4) . ? Zn1 C14 2.537(4) 4_575 ? Zn1 C1 2.553(4) . ? Zn2 N4 2.050(3) . ? Zn2 O7 2.087(3) . ? Zn2 N5 2.094(3) . ? Zn2 O10 2.144(3) 4_655 ? Zn2 O9 2.181(3) 4_655 ? Zn2 O6 2.343(3) . ? Zn2 C48 2.493(4) 4_655 ? Zn2 C35 2.554(4) . ? O10 C48 1.276(5) . ? O10 Zn2 2.144(3) 4_556 ? N6 C29 1.353(4) . ? N6 C27 1.376(5) . ? N6 C26 1.474(4) . ? O8 C42 1.380(4) . ? O8 C39 1.396(5) . ? N3 C17 1.350(5) . ? N3 C16 1.375(5) . ? N3 C23 1.476(4) . ? O9 C48 1.255(5) . ? O9 Zn2 2.181(3) 4_556 ? O7 C35 1.262(5) . ? N5 C34 1.326(5) . ? N5 C30 1.359(5) . ? O5 C5 1.386(5) . ? O5 C8 1.392(5) . ? C17 N1 1.334(4) . ? C17 C18 1.471(5) . ? O6 C35 1.238(5) . ? O2 C1 1.243(6) . ? C48 C47 1.493(5) . ? C48 Zn2 2.493(4) 4_556 ? C25 C26 1.515(5) . ? C25 C24 1.519(5) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? N2 C22 1.322(5) . ? N2 C18 1.352(5) . ? O1 C1 1.271(6) . ? N1 C15 1.365(5) . ? C29 N4 1.330(5) . ? C29 C30 1.469(5) . ? C16 C15 1.367(6) . ? C16 H16 0.9300 . ? N4 C28 1.367(5) . ? C23 C24 1.514(5) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C30 C31 1.379(5) . ? C35 C36 1.494(5) . ? C36 C41 1.387(6) . ? C36 C37 1.395(6) . ? C11 C12 1.381(6) . ? C11 C10 1.390(6) . ? C11 C14 1.498(6) . ? C5 C4 1.363(6) . ? C5 C6 1.381(6) . ? C1 C2 1.493(6) . ? C39 C40 1.375(6) . ? C39 C38 1.381(6) . ? C42 C46 1.376(6) . ? C42 C43 1.377(6) . ? C31 C32 1.380(6) . ? C31 H31 0.9300 . ? C38 C37 1.373(6) . ? C38 H38 0.9300 . ? C44 C47 1.384(6) . ? C44 C43 1.387(6) . ? C44 H44 0.9300 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C8 C9 1.381(6) . ? C8 C13 1.385(6) . ? C18 C19 1.374(5) . ? C28 C27 1.359(6) . ? C28 H28 0.9300 . ? C2 C3 1.374(6) . ? C2 C7 1.389(6) . ? C37 H37 0.9300 . ? C43 H43 0.9300 . ? C12 C13 1.375(6) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C4 C3 1.391(6) . ? C4 H4 0.9300 . ? C46 C45 1.389(6) . ? C46 H46 0.9300 . ? C33 C32 1.361(6) . ? C33 C34 1.385(6) . ? C33 H33 0.9300 . ? C19 C20 1.383(6) . ? C19 H19 0.9300 . ? C47 C45 1.366(6) . ? C41 C40 1.389(6) . ? C41 H41 0.9300 . ? C10 C9 1.384(6) . ? C10 H10 0.9300 . ? C34 H34 0.9300 . ? C27 H27 0.9300 . ? C40 H40 0.9300 . ? C20 C21 1.374(7) . ? C20 H20 0.9300 . ? C9 H9 0.9300 . ? C6 C7 1.375(6) . ? C6 H6 0.9300 . ? C45 H45 0.9300 . ? C32 H32 0.9300 . ? C15 H15 0.9300 . ? C3 H3 0.9300 . ? C22 C21 1.367(7) . ? C22 H22 0.9300 . ? C21 H21 0.9300 . ? C7 H7 0.9300 . ? C14 O4 1.244(6) . ? C14 O3 1.256(6) . ? C14 Zn1 2.537(4) 4_676 ? O3 Zn1 2.056(3) 4_676 ? O1W H1B 0.79(10) . ? O1W H1A 0.81(7) . ? O4 Zn1 2.350(4) 4_676 ? O2W H2B 0.81(8) . ? O2W H2A 0.80(8) . ? O6W H6A 0.81(6) . ? O6W H6B 0.81(10) . ? O3W H3A 0.81(9) . ? O3W H3B 0.79(8) . ? O4W H4A 0.81(10) . ? O4W H4B 0.80(10) . ? O5W H5B 0.80(10) . ? O5W H5A 0.80(9) . ? O7W H7B 0.80(10) . ? O7W H7A 0.80(9) . ? O8W H8A 0.80(6) . ? O8W H8B 0.82(9) . ? 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 Zn1 O3 104.65(13) . 4_575 ? N1 Zn1 O1 145.33(13) . . ? O3 Zn1 O1 101.77(13) 4_575 . ? N1 Zn1 N2 78.58(12) . . ? O3 Zn1 N2 143.46(14) 4_575 . ? O1 Zn1 N2 93.20(13) . . ? N1 Zn1 O4 115.70(13) . 4_575 ? O3 Zn1 O4 58.56(13) 4_575 4_575 ? O1 Zn1 O4 97.13(14) . 4_575 ? N2 Zn1 O4 86.82(13) . 4_575 ? N1 Zn1 O2 96.84(12) . . ? O3 Zn1 O2 95.24(14) 4_575 . ? O1 Zn1 O2 58.47(13) . . ? N2 Zn1 O2 120.81(14) . . ? O4 Zn1 O2 141.62(13) 4_575 . ? N1 Zn1 C14 114.31(13) . 4_575 ? O3 Zn1 C14 29.42(14) 4_575 4_575 ? O1 Zn1 C14 99.71(14) . 4_575 ? N2 Zn1 C14 115.53(15) . 4_575 ? O4 Zn1 C14 29.18(13) 4_575 4_575 ? O2 Zn1 C14 119.56(15) . 4_575 ? N1 Zn1 C1 121.76(14) . . ? O3 Zn1 C1 100.86(14) 4_575 . ? O1 Zn1 C1 29.59(15) . . ? N2 Zn1 C1 108.15(14) . . ? O4 Zn1 C1 122.32(15) 4_575 . ? O2 Zn1 C1 28.92(14) . . ? C14 Zn1 C1 113.49(14) 4_575 . ? N4 Zn2 O7 98.39(12) . . ? N4 Zn2 N5 79.16(12) . . ? O7 Zn2 N5 143.60(12) . . ? N4 Zn2 O10 104.70(12) . 4_655 ? O7 Zn2 O10 104.73(11) . 4_655 ? N5 Zn2 O10 111.05(12) . 4_655 ? N4 Zn2 O9 160.28(12) . 4_655 ? O7 Zn2 O9 98.51(12) . 4_655 ? N5 Zn2 O9 93.07(12) . 4_655 ? O10 Zn2 O9 60.98(11) 4_655 4_655 ? N4 Zn2 O6 103.53(12) . . ? O7 Zn2 O6 58.30(11) . . ? N5 Zn2 O6 86.67(12) . . ? O10 Zn2 O6 148.98(12) 4_655 . ? O9 Zn2 O6 93.98(12) 4_655 . ? N4 Zn2 C48 133.91(13) . 4_655 ? O7 Zn2 C48 104.19(12) . 4_655 ? N5 Zn2 C48 103.07(12) . 4_655 ? O9 Zn2 C48 30.22(12) 4_655 4_655 ? O6 Zn2 C48 122.55(13) . 4_655 ? N4 Zn2 C35 102.96(12) . . ? O7 Zn2 C35 29.42(13) . . ? N5 Zn2 C35 115.12(13) . . ? O10 Zn2 C35 129.50(13) 4_655 . ? O9 Zn2 C35 96.75(12) 4_655 . ? O6 Zn2 C35 28.88(12) . . ? C48 Zn2 C35 116.38(13) 4_655 . ? C48 O10 Zn2 89.9(2) . 4_556 ? C29 N6 C27 107.8(3) . . ? C29 N6 C26 130.7(3) . . ? C27 N6 C26 121.2(3) . . ? C42 O8 C39 121.6(3) . . ? C17 N3 C16 107.7(3) . . ? C17 N3 C23 129.9(3) . . ? C16 N3 C23 122.1(3) . . ? C48 O9 Zn2 88.8(2) . 4_556 ? C35 O7 Zn2 96.3(3) . . ? C34 N5 C30 119.3(3) . . ? C34 N5 Zn2 125.7(3) . . ? C30 N5 Zn2 115.0(2) . . ? C5 O5 C8 120.8(3) . . ? N1 C17 N3 110.0(3) . . ? N1 C17 C18 119.4(3) . . ? N3 C17 C18 130.5(3) . . ? C35 O6 Zn2 85.1(3) . . ? C1 O2 Zn1 83.5(3) . . ? O9 C48 O10 120.3(4) . . ? O9 C48 C47 119.9(4) . . ? O10 C48 C47 119.8(4) . . ? O9 C48 Zn2 61.0(2) . 4_556 ? O10 C48 Zn2 59.33(19) . 4_556 ? C47 C48 Zn2 177.8(3) . 4_556 ? C26 C25 C24 111.2(3) . . ? C26 C25 H25A 109.4 . . ? C24 C25 H25A 109.4 . . ? C26 C25 H25B 109.4 . . ? C24 C25 H25B 109.4 . . ? H25A C25 H25B 108.0 . . ? N6 C26 C25 112.6(3) . . ? N6 C26 H26A 109.1 . . ? C25 C26 H26A 109.1 . . ? N6 C26 H26B 109.1 . . ? C25 C26 H26B 109.1 . . ? H26A C26 H26B 107.8 . . ? C22 N2 C18 119.1(4) . . ? C22 N2 Zn1 125.4(3) . . ? C18 N2 Zn1 115.5(2) . . ? C1 O1 Zn1 97.2(3) . . ? C17 N1 C15 107.0(3) . . ? C17 N1 Zn1 114.2(2) . . ? C15 N1 Zn1 138.3(3) . . ? N4 C29 N6 109.5(3) . . ? N4 C29 C30 119.8(3) . . ? N6 C29 C30 130.7(3) . . ? C15 C16 N3 106.4(3) . . ? C15 C16 H16 126.8 . . ? N3 C16 H16 126.8 . . ? C29 N4 C28 107.4(3) . . ? C29 N4 Zn2 113.1(2) . . ? C28 N4 Zn2 139.0(3) . . ? N3 C23 C24 112.0(3) . . ? N3 C23 H23A 109.2 . . ? C24 C23 H23A 109.2 . . ? N3 C23 H23B 109.2 . . ? C24 C23 H23B 109.2 . . ? H23A C23 H23B 107.9 . . ? N5 C30 C31 120.6(4) . . ? N5 C30 C29 112.0(3) . . ? C31 C30 C29 127.3(3) . . ? O6 C35 O7 120.3(4) . . ? O6 C35 C36 120.4(4) . . ? O7 C35 C36 119.2(4) . . ? O6 C35 Zn2 66.0(2) . . ? O7 C35 Zn2 54.3(2) . . ? C36 C35 Zn2 173.1(3) . . ? C41 C36 C37 118.4(4) . . ? C41 C36 C35 121.6(4) . . ? C37 C36 C35 119.9(4) . . ? C12 C11 C10 118.5(4) . . ? C12 C11 C14 120.3(4) . . ? C10 C11 C14 121.1(4) . . ? C4 C5 C6 119.9(4) . . ? C4 C5 O5 124.5(4) . . ? C6 C5 O5 115.5(4) . . ? O2 C1 O1 120.7(4) . . ? O2 C1 C2 121.8(4) . . ? O1 C1 C2 117.5(4) . . ? O2 C1 Zn1 67.6(2) . . ? O1 C1 Zn1 53.2(2) . . ? C2 C1 Zn1 170.4(4) . . ? C40 C39 C38 121.6(4) . . ? C40 C39 O8 122.5(4) . . ? C38 C39 O8 115.6(4) . . ? C46 C42 C43 120.3(4) . . ? C46 C42 O8 124.8(4) . . ? C43 C42 O8 114.9(4) . . ? C30 C31 C32 119.2(4) . . ? C30 C31 H31 120.4 . . ? C32 C31 H31 120.4 . . ? C37 C38 C39 118.9(4) . . ? C37 C38 H38 120.5 . . ? C39 C38 H38 120.5 . . ? C47 C44 C43 121.2(4) . . ? C47 C44 H44 119.4 . . ? C43 C44 H44 119.4 . . ? C23 C24 C25 111.9(3) . . ? C23 C24 H24A 109.2 . . ? C25 C24 H24A 109.2 . . ? C23 C24 H24B 109.2 . . ? C25 C24 H24B 109.2 . . ? H24A C24 H24B 107.9 . . ? C9 C8 C13 121.3(4) . . ? C9 C8 O5 122.2(4) . . ? C13 C8 O5 116.3(4) . . ? N2 C18 C19 121.0(3) . . ? N2 C18 C17 111.6(3) . . ? C19 C18 C17 127.3(3) . . ? C27 C28 N4 108.8(3) . . ? C27 C28 H28 125.6 . . ? N4 C28 H28 125.6 . . ? C3 C2 C7 118.2(4) . . ? C3 C2 C1 119.7(4) . . ? C7 C2 C1 122.1(4) . . ? C38 C37 C36 121.3(4) . . ? C38 C37 H37 119.4 . . ? C36 C37 H37 119.4 . . ? C42 C43 C44 119.3(4) . . ? C42 C43 H43 120.3 . . ? C44 C43 H43 120.3 . . ? C13 C12 C11 121.6(4) . . ? C13 C12 H12 119.2 . . ? C11 C12 H12 119.2 . . ? C12 C13 C8 118.8(4) . . ? C12 C13 H13 120.6 . . ? C8 C13 H13 120.6 . . ? C5 C4 C3 119.9(4) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C42 C46 C45 119.4(4) . . ? C42 C46 H46 120.3 . . ? C45 C46 H46 120.3 . . ? C32 C33 C34 118.6(4) . . ? C32 C33 H33 120.7 . . ? C34 C33 H33 120.7 . . ? C18 C19 C20 119.2(4) . . ? C18 C19 H19 120.4 . . ? C20 C19 H19 120.4 . . ? C45 C47 C44 118.3(4) . . ? C45 C47 C48 119.8(4) . . ? C44 C47 C48 121.9(4) . . ? C36 C41 C40 120.9(4) . . ? C36 C41 H41 119.6 . . ? C40 C41 H41 119.6 . . ? C9 C10 C11 121.1(4) . . ? C9 C10 H10 119.5 . . ? C11 C10 H10 119.5 . . ? N5 C34 C33 122.3(4) . . ? N5 C34 H34 118.9 . . ? C33 C34 H34 118.9 . . ? C28 C27 N6 106.5(3) . . ? C28 C27 H27 126.8 . . ? N6 C27 H27 126.8 . . ? C39 C40 C41 118.9(4) . . ? C39 C40 H40 120.6 . . ? C41 C40 H40 120.6 . . ? C21 C20 C19 119.1(4) . . ? C21 C20 H20 120.5 . . ? C19 C20 H20 120.5 . . ? C8 C9 C10 118.7(4) . . ? C8 C9 H9 120.6 . . ? C10 C9 H9 120.6 . . ? C7 C6 C5 119.9(4) . . ? C7 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? C47 C45 C46 121.5(4) . . ? C47 C45 H45 119.2 . . ? C46 C45 H45 119.2 . . ? C33 C32 C31 119.9(4) . . ? C33 C32 H32 120.1 . . ? C31 C32 H32 120.1 . . ? N1 C15 C16 109.0(3) . . ? N1 C15 H15 125.5 . . ? C16 C15 H15 125.5 . . ? C2 C3 C4 121.0(4) . . ? C2 C3 H3 119.5 . . ? C4 C3 H3 119.5 . . ? N2 C22 C21 122.9(4) . . ? N2 C22 H22 118.6 . . ? C21 C22 H22 118.6 . . ? C22 C21 C20 118.7(4) . . ? C22 C21 H21 120.6 . . ? C20 C21 H21 120.6 . . ? C6 C7 C2 121.0(4) . . ? C6 C7 H7 119.5 . . ? C2 C7 H7 119.5 . . ? O4 C14 O3 120.5(4) . . ? O4 C14 C11 120.5(4) . . ? O3 C14 C11 119.0(4) . . ? O4 C14 Zn1 67.1(3) . 4_676 ? O3 C14 Zn1 53.5(2) . 4_676 ? C11 C14 Zn1 171.5(4) . 4_676 ? C14 O3 Zn1 97.0(3) . 4_676 ? H1B O1W H1A 119(11) . . ? C14 O4 Zn1 83.7(3) . 4_676 ? H2B O2W H2A 119(10) . . ? H6A O6W H6B 117(9) . . ? H3A O3W H3B 118(11) . . ? H4A O4W H4B 119(13) . . ? H5B O5W H5A 118(11) . . ? H7B O7W H7A 119(11) . . ? H8A O8W H8B 117(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 Zn2 O7 C35 -101.5(2) . . . . ? N5 Zn2 O7 C35 -18.4(3) . . . . ? O10 Zn2 O7 C35 150.8(2) 4_655 . . . ? O9 Zn2 O7 C35 88.7(2) 4_655 . . . ? O6 Zn2 O7 C35 -0.8(2) . . . . ? C48 Zn2 O7 C35 119.0(2) 4_655 . . . ? N4 Zn2 N5 C34 -172.8(3) . . . . ? O7 Zn2 N5 C34 97.7(4) . . . . ? O10 Zn2 N5 C34 -71.1(3) 4_655 . . . ? O9 Zn2 N5 C34 -11.1(3) 4_655 . . . ? O6 Zn2 N5 C34 82.7(3) . . . . ? C48 Zn2 N5 C34 -39.9(3) 4_655 . . . ? C35 Zn2 N5 C34 87.8(3) . . . . ? N4 Zn2 N5 C30 7.2(3) . . . . ? O7 Zn2 N5 C30 -82.2(3) . . . . ? O10 Zn2 N5 C30 109.0(3) 4_655 . . . ? O9 Zn2 N5 C30 169.0(3) 4_655 . . . ? O6 Zn2 N5 C30 -97.2(3) . . . . ? C48 Zn2 N5 C30 140.1(3) 4_655 . . . ? C35 Zn2 N5 C30 -92.1(3) . . . . ? C16 N3 C17 N1 -0.4(4) . . . . ? C23 N3 C17 N1 172.7(3) . . . . ? C16 N3 C17 C18 176.8(4) . . . . ? C23 N3 C17 C18 -10.0(6) . . . . ? N4 Zn2 O6 C35 92.4(3) . . . . ? O7 Zn2 O6 C35 0.8(2) . . . . ? N5 Zn2 O6 C35 170.4(3) . . . . ? O10 Zn2 O6 C35 -62.7(4) 4_655 . . . ? O9 Zn2 O6 C35 -96.8(3) 4_655 . . . ? C48 Zn2 O6 C35 -86.2(3) 4_655 . . . ? N1 Zn1 O2 C1 151.5(3) . . . . ? O3 Zn1 O2 C1 -103.0(3) 4_575 . . . ? O1 Zn1 O2 C1 -2.4(3) . . . . ? N2 Zn1 O2 C1 70.8(3) . . . . ? O4 Zn1 O2 C1 -59.7(4) 4_575 . . . ? C14 Zn1 O2 C1 -85.5(3) 4_575 . . . ? Zn2 O9 C48 O10 2.5(4) 4_556 . . . ? Zn2 O9 C48 C47 -177.7(3) 4_556 . . . ? Zn2 O10 C48 O9 -2.5(4) 4_556 . . . ? Zn2 O10 C48 C47 177.6(3) 4_556 . . . ? C29 N6 C26 C25 -71.8(5) . . . . ? C27 N6 C26 C25 101.1(4) . . . . ? C24 C25 C26 N6 -161.9(3) . . . . ? N1 Zn1 N2 C22 -172.1(4) . . . . ? O3 Zn1 N2 C22 88.6(4) 4_575 . . . ? O1 Zn1 N2 C22 -26.1(4) . . . . ? O4 Zn1 N2 C22 70.8(4) 4_575 . . . ? O2 Zn1 N2 C22 -80.9(4) . . . . ? C14 Zn1 N2 C22 76.2(4) 4_575 . . . ? C1 Zn1 N2 C22 -52.2(4) . . . . ? N1 Zn1 N2 C18 5.3(3) . . . . ? O3 Zn1 N2 C18 -93.9(3) 4_575 . . . ? O1 Zn1 N2 C18 151.3(3) . . . . ? O4 Zn1 N2 C18 -111.7(3) 4_575 . . . ? O2 Zn1 N2 C18 96.5(3) . . . . ? C14 Zn1 N2 C18 -106.3(3) 4_575 . . . ? C1 Zn1 N2 C18 125.3(3) . . . . ? N1 Zn1 O1 C1 -47.8(4) . . . . ? O3 Zn1 O1 C1 91.3(3) 4_575 . . . ? N2 Zn1 O1 C1 -122.2(3) . . . . ? O4 Zn1 O1 C1 150.6(3) 4_575 . . . ? O2 Zn1 O1 C1 2.3(2) . . . . ? C14 Zn1 O1 C1 121.2(3) 4_575 . . . ? N3 C17 N1 C15 0.0(4) . . . . ? C18 C17 N1 C15 -177.6(3) . . . . ? N3 C17 N1 Zn1 -173.9(2) . . . . ? C18 C17 N1 Zn1 8.5(4) . . . . ? O3 Zn1 N1 C17 135.4(3) 4_575 . . . ? O1 Zn1 N1 C17 -86.2(3) . . . . ? N2 Zn1 N1 C17 -7.2(3) . . . . ? O4 Zn1 N1 C17 73.6(3) 4_575 . . . ? O2 Zn1 N1 C17 -127.4(3) . . . . ? C14 Zn1 N1 C17 105.8(3) 4_575 . . . ? C1 Zn1 N1 C17 -111.6(3) . . . . ? O3 Zn1 N1 C15 -35.8(4) 4_575 . . . ? O1 Zn1 N1 C15 102.7(4) . . . . ? N2 Zn1 N1 C15 -178.4(4) . . . . ? O4 Zn1 N1 C15 -97.6(4) 4_575 . . . ? O2 Zn1 N1 C15 61.4(4) . . . . ? C14 Zn1 N1 C15 -65.4(4) 4_575 . . . ? C1 Zn1 N1 C15 77.2(4) . . . . ? C27 N6 C29 N4 -0.7(4) . . . . ? C26 N6 C29 N4 172.9(3) . . . . ? C27 N6 C29 C30 175.8(4) . . . . ? C26 N6 C29 C30 -10.6(6) . . . . ? C17 N3 C16 C15 0.7(4) . . . . ? C23 N3 C16 C15 -173.1(3) . . . . ? N6 C29 N4 C28 0.1(4) . . . . ? C30 C29 N4 C28 -176.8(3) . . . . ? N6 C29 N4 Zn2 -173.5(2) . . . . ? C30 C29 N4 Zn2 9.5(4) . . . . ? O7 Zn2 N4 C29 134.4(3) . . . . ? N5 Zn2 N4 C29 -8.8(2) . . . . ? O10 Zn2 N4 C29 -117.9(3) 4_655 . . . ? O9 Zn2 N4 C29 -76.9(5) 4_655 . . . ? O6 Zn2 N4 C29 75.1(3) . . . . ? C48 Zn2 N4 C29 -106.6(3) 4_655 . . . ? C35 Zn2 N4 C29 104.8(3) . . . . ? O7 Zn2 N4 C28 -36.4(4) . . . . ? N5 Zn2 N4 C28 -179.5(4) . . . . ? O10 Zn2 N4 C28 71.3(4) 4_655 . . . ? O9 Zn2 N4 C28 112.4(5) 4_655 . . . ? O6 Zn2 N4 C28 -95.7(4) . . . . ? C48 Zn2 N4 C28 82.7(5) 4_655 . . . ? C35 Zn2 N4 C28 -66.0(4) . . . . ? C17 N3 C23 C24 -67.7(5) . . . . ? C16 N3 C23 C24 104.6(4) . . . . ? C34 N5 C30 C31 -2.7(5) . . . . ? Zn2 N5 C30 C31 177.2(3) . . . . ? C34 N5 C30 C29 175.6(3) . . . . ? Zn2 N5 C30 C29 -4.4(4) . . . . ? N4 C29 C30 N5 -3.4(5) . . . . ? N6 C29 C30 N5 -179.6(3) . . . . ? N4 C29 C30 C31 174.8(4) . . . . ? N6 C29 C30 C31 -1.4(6) . . . . ? Zn2 O6 C35 O7 -1.3(4) . . . . ? Zn2 O6 C35 C36 177.1(3) . . . . ? Zn2 O7 C35 O6 1.4(4) . . . . ? Zn2 O7 C35 C36 -177.0(3) . . . . ? N4 Zn2 C35 O6 -94.6(3) . . . . ? O7 Zn2 C35 O6 -178.7(4) . . . . ? N5 Zn2 C35 O6 -10.6(3) . . . . ? O10 Zn2 C35 O6 143.6(2) 4_655 . . . ? O9 Zn2 C35 O6 86.0(3) 4_655 . . . ? C48 Zn2 C35 O6 110.1(3) 4_655 . . . ? N4 Zn2 C35 O7 84.1(2) . . . . ? N5 Zn2 C35 O7 168.0(2) . . . . ? O10 Zn2 C35 O7 -37.7(3) 4_655 . . . ? O9 Zn2 C35 O7 -95.3(2) 4_655 . . . ? O6 Zn2 C35 O7 178.7(4) . . . . ? C48 Zn2 C35 O7 -71.2(3) 4_655 . . . ? O6 C35 C36 C41 -11.7(6) . . . . ? O7 C35 C36 C41 166.7(4) . . . . ? O6 C35 C36 C37 172.5(4) . . . . ? O7 C35 C36 C37 -9.1(6) . . . . ? C8 O5 C5 C4 1.8(7) . . . . ? C8 O5 C5 C6 -175.7(4) . . . . ? Zn1 O2 C1 O1 3.8(4) . . . . ? Zn1 O2 C1 C2 -177.7(4) . . . . ? Zn1 O1 C1 O2 -4.4(5) . . . . ? Zn1 O1 C1 C2 177.0(3) . . . . ? N1 Zn1 C1 O2 -33.8(3) . . . . ? O3 Zn1 C1 O2 81.1(3) 4_575 . . . ? O1 Zn1 C1 O2 175.9(4) . . . . ? N2 Zn1 C1 O2 -121.4(3) . . . . ? O4 Zn1 C1 O2 140.6(3) 4_575 . . . ? C14 Zn1 C1 O2 109.0(3) 4_575 . . . ? N1 Zn1 C1 O1 150.3(2) . . . . ? O3 Zn1 C1 O1 -94.8(3) 4_575 . . . ? N2 Zn1 C1 O1 62.7(3) . . . . ? O4 Zn1 C1 O1 -35.2(3) 4_575 . . . ? O2 Zn1 C1 O1 -175.9(4) . . . . ? C14 Zn1 C1 O1 -66.9(3) 4_575 . . . ? C42 O8 C39 C40 60.9(6) . . . . ? C42 O8 C39 C38 -125.7(4) . . . . ? C39 O8 C42 C46 3.2(7) . . . . ? C39 O8 C42 C43 -179.0(4) . . . . ? N5 C30 C31 C32 1.5(6) . . . . ? C29 C30 C31 C32 -176.6(4) . . . . ? C40 C39 C38 C37 2.2(6) . . . . ? O8 C39 C38 C37 -171.3(4) . . . . ? N3 C23 C24 C25 -166.3(3) . . . . ? C26 C25 C24 C23 -161.4(3) . . . . ? C5 O5 C8 C9 -60.3(6) . . . . ? C5 O5 C8 C13 125.5(4) . . . . ? C22 N2 C18 C19 -1.7(6) . . . . ? Zn1 N2 C18 C19 -179.3(3) . . . . ? C22 N2 C18 C17 175.1(4) . . . . ? Zn1 N2 C18 C17 -2.5(4) . . . . ? N1 C17 C18 N2 -3.9(5) . . . . ? N3 C17 C18 N2 179.1(4) . . . . ? N1 C17 C18 C19 172.6(4) . . . . ? N3 C17 C18 C19 -4.3(7) . . . . ? C29 N4 C28 C27 0.5(5) . . . . ? Zn2 N4 C28 C27 171.6(3) . . . . ? O2 C1 C2 C3 -174.7(4) . . . . ? O1 C1 C2 C3 3.8(6) . . . . ? O2 C1 C2 C7 3.7(7) . . . . ? O1 C1 C2 C7 -177.8(4) . . . . ? C39 C38 C37 C36 -1.7(6) . . . . ? C41 C36 C37 C38 0.0(6) . . . . ? C35 C36 C37 C38 175.9(4) . . . . ? C46 C42 C43 C44 1.0(7) . . . . ? O8 C42 C43 C44 -176.9(4) . . . . ? C47 C44 C43 C42 0.0(8) . . . . ? C10 C11 C12 C13 -0.5(6) . . . . ? C14 C11 C12 C13 -177.8(4) . . . . ? C11 C12 C13 C8 0.8(6) . . . . ? C9 C8 C13 C12 0.4(6) . . . . ? O5 C8 C13 C12 174.5(4) . . . . ? C6 C5 C4 C3 -1.9(8) . . . . ? O5 C5 C4 C3 -179.3(4) . . . . ? C43 C42 C46 C45 -1.1(7) . . . . ? O8 C42 C46 C45 176.5(4) . . . . ? N2 C18 C19 C20 0.0(6) . . . . ? C17 C18 C19 C20 -176.2(4) . . . . ? C43 C44 C47 C45 -0.8(7) . . . . ? C43 C44 C47 C48 177.9(4) . . . . ? O9 C48 C47 C45 2.1(6) . . . . ? O10 C48 C47 C45 -178.0(4) . . . . ? O9 C48 C47 C44 -176.6(4) . . . . ? O10 C48 C47 C44 3.3(6) . . . . ? C37 C36 C41 C40 1.2(6) . . . . ? C35 C36 C41 C40 -174.6(4) . . . . ? C12 C11 C10 C9 -1.0(7) . . . . ? C14 C11 C10 C9 176.3(4) . . . . ? C30 N5 C34 C33 2.4(6) . . . . ? Zn2 N5 C34 C33 -177.5(3) . . . . ? C32 C33 C34 N5 -0.9(7) . . . . ? N4 C28 C27 N6 -0.9(5) . . . . ? C29 N6 C27 C28 1.0(5) . . . . ? C26 N6 C27 C28 -173.4(3) . . . . ? C38 C39 C40 C41 -1.0(6) . . . . ? O8 C39 C40 C41 172.1(4) . . . . ? C36 C41 C40 C39 -0.7(6) . . . . ? C18 C19 C20 C21 1.1(7) . . . . ? C13 C8 C9 C10 -1.8(7) . . . . ? O5 C8 C9 C10 -175.6(4) . . . . ? C11 C10 C9 C8 2.1(7) . . . . ? C4 C5 C6 C7 1.2(8) . . . . ? O5 C5 C6 C7 178.7(5) . . . . ? C44 C47 C45 C46 0.6(7) . . . . ? C48 C47 C45 C46 -178.1(4) . . . . ? C42 C46 C45 C47 0.3(7) . . . . ? C34 C33 C32 C31 -0.4(7) . . . . ? C30 C31 C32 C33 0.1(7) . . . . ? C17 N1 C15 C16 0.5(5) . . . . ? Zn1 N1 C15 C16 172.1(3) . . . . ? N3 C16 C15 N1 -0.7(5) . . . . ? C7 C2 C3 C4 -1.0(7) . . . . ? C1 C2 C3 C4 177.4(4) . . . . ? C5 C4 C3 C2 1.9(8) . . . . ? C18 N2 C22 C21 2.3(8) . . . . ? Zn1 N2 C22 C21 179.7(4) . . . . ? N2 C22 C21 C20 -1.2(9) . . . . ? C19 C20 C21 C22 -0.5(8) . . . . ? C5 C6 C7 C2 -0.3(8) . . . . ? C3 C2 C7 C6 0.3(7) . . . . ? C1 C2 C7 C6 -178.1(5) . . . . ? C12 C11 C14 O4 -179.5(4) . . . . ? C10 C11 C14 O4 3.3(6) . . . . ? C12 C11 C14 O3 0.8(6) . . . . ? C10 C11 C14 O3 -176.3(4) . . . . ? O4 C14 O3 Zn1 -4.3(5) . . . 4_676 ? C11 C14 O3 Zn1 175.3(3) . . . 4_676 ? O3 C14 O4 Zn1 3.8(4) . . . 4_676 ? C11 C14 O4 Zn1 -175.9(4) . . . 4_676 ? 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 O2W H2A O1W 0.80(8) 2.00(9) 2.787(5) 169(12) 2 O1W H1A O8W 0.81(7) 2.13(8) 2.770(8) 136(10) . O1W H1B O7 0.79(10) 2.12(7) 2.854(5) 152(13) . O2W H2B O6W 0.81(8) 2.09(7) 2.878(6) 165(11) . O3W H3A O5W 0.81(9) 2.22(8) 2.854(6) 136(11) 1_544 O3W H3B O6 0.79(8) 2.12(7) 2.840(5) 150(12) . O4W H4A O3W 0.81(10) 2.11(10) 2.895(7) 163(12) 2_556 O4W H4B O2 0.80(10) 2.38(6) 3.124(6) 155(13) . O5W H5A O2W 0.80(9) 2.09(10) 2.882(6) 172(12) 3_667 O5W H5B O4W 0.80(10) 2.11(9) 2.910(6) 175(13) 4_676 O6W H6A O7W 0.81(6) 1.93(3) 2.722(6) 168(15) 4_665 O6W H6B O4 0.81(10) 2.07(10) 2.857(6) 164(10) 2_646 O7W H7A O3W 0.80(9) 2.00(10) 2.769(6) 162(13) 2_556 O7W H7B O2 0.80(10) 2.07(9) 2.861(6) 168(12) . O8W H8B O10 0.82(9) 2.22(10) 2.889(7) 130(13) 4_655 _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 1.019 _refine_diff_density_min -0.482 _refine_diff_density_rms 0.075 data_4 _database_code_depnum_ccdc_archive 'CCDC 687551' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H40 Cd2 N6 O12' _chemical_formula_weight 1117.66 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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.0580(4) _cell_length_b 10.6750(4) _cell_length_c 12.0480(5) _cell_angle_alpha 85.8410(10) _cell_angle_beta 68.7740(10) _cell_angle_gamma 66.1710(10) _cell_volume 1098.90(8) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.09 _cell_measurement_theta_max 28.26 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.689 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 562 _exptl_absorpt_coefficient_mu 1.041 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.739 _exptl_absorpt_correction_T_max 0.771 _exptl_absorpt_process_details 'SADABS(Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6902 _diffrn_reflns_av_R_equivalents 0.0161 _diffrn_reflns_av_sigmaI/netI 0.0407 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 28.26 _reflns_number_total 5038 _reflns_number_gt 4249 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SMART (Bruker, 1997)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97(Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material SHELXL-97 _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^)+(0.0319P)^2^+0.3905P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5038 _refine_ls_number_parameters 314 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0437 _refine_ls_R_factor_gt 0.0345 _refine_ls_wR_factor_ref 0.0777 _refine_ls_wR_factor_gt 0.0728 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.42887(2) 0.40157(2) 0.926495(19) 0.03529(8) Uani 1 1 d . . . O1 O 1.5563(2) 0.3855(2) 0.05890(18) 0.0414(5) Uani 1 1 d . . . O5 O 1.3325(2) -0.0203(2) 0.41412(19) 0.0447(5) Uani 1 1 d . . . N1 N 0.2997(3) 0.3072(3) 0.8637(2) 0.0391(6) Uani 1 1 d . . . O3 O 0.6482(2) 0.3394(2) 0.7678(2) 0.0491(6) Uani 1 1 d . . . N3 N 0.2039(3) 0.4099(3) 1.0888(2) 0.0378(6) Uani 1 1 d . . . C16 C 1.1360(3) -0.0410(3) 0.5853(3) 0.0376(7) Uani 1 1 d . . . H16 H 1.2004 -0.1333 0.5823 0.045 Uiso 1 1 calc R . . N2 N 0.1209(3) 0.2269(3) 0.8925(2) 0.0392(6) Uani 1 1 d . . . C8 C 0.1605(4) 0.4678(3) 1.1981(3) 0.0478(8) Uani 1 1 d . . . H8 H 0.2190 0.5104 1.2106 0.057 Uiso 1 1 calc R . . O4 O 0.6873(3) 0.1461(2) 0.85726(19) 0.0504(6) Uani 1 1 d . . . C19 C 1.3990(3) 0.0667(3) 0.3479(3) 0.0375(7) Uani 1 1 d . . . C1 C 0.3218(4) 0.2513(3) 0.7567(3) 0.0441(7) Uani 1 1 d . . . H1 H 0.3999 0.2474 0.6841 0.053 Uiso 1 1 calc R . . C3 C 0.1786(3) 0.2910(3) 0.9453(3) 0.0335(6) Uani 1 1 d . . . C24 C 1.5839(3) 0.3444(3) 0.1528(3) 0.0339(6) Uani 1 1 d . . . C15 C 1.1866(3) 0.0418(3) 0.5015(2) 0.0338(6) Uani 1 1 d . . . C4 C 0.1209(3) 0.3463(3) 1.0702(3) 0.0348(6) Uani 1 1 d . . . C12 C 0.8910(3) 0.1519(3) 0.6797(2) 0.0339(6) Uani 1 1 d . . . C10 C 0.0630(4) 0.0280(3) 0.9751(3) 0.0442(8) Uani 1 1 d . . . H10A H 0.1089 0.0246 1.0341 0.053 Uiso 1 1 calc R . . H10B H 0.1448 -0.0298 0.9045 0.053 Uiso 1 1 calc R . . C22 C 1.5294(3) 0.2389(3) 0.2174(3) 0.0320(6) Uani 1 1 d . . . C9 C -0.0020(4) 0.1748(3) 0.9429(3) 0.0440(8) Uani 1 1 d . . . H9A H -0.0500 0.1787 0.8851 0.053 Uiso 1 1 calc R . . H9B H -0.0822 0.2332 1.0138 0.053 Uiso 1 1 calc R . . C18 C 1.4444(4) 0.1430(3) 0.4032(3) 0.0438(7) Uani 1 1 d . . . H18 H 1.4315 0.1362 0.4835 0.053 Uiso 1 1 calc R . . C21 C 1.4887(3) 0.1574(3) 0.1630(3) 0.0373(7) Uani 1 1 d . . . H21 H 1.5058 0.1607 0.0818 0.045 Uiso 1 1 calc R . . C20 C 1.4227(3) 0.0709(3) 0.2282(3) 0.0375(7) Uani 1 1 d . . . H20 H 1.3949 0.0166 0.1916 0.045 Uiso 1 1 calc R . . C17 C 0.9887(3) 0.0150(3) 0.6735(2) 0.0361(7) Uani 1 1 d . . . H17 H 0.9549 -0.0407 0.7297 0.043 Uiso 1 1 calc R . . C13 C 0.9434(3) 0.2331(3) 0.5944(3) 0.0374(7) Uani 1 1 d . . . H13 H 0.8785 0.3252 0.5971 0.045 Uiso 1 1 calc R . . C23 C 1.5091(4) 0.2296(3) 0.3374(3) 0.0401(7) Uani 1 1 d . . . H23 H 1.5393 0.2818 0.3739 0.048 Uiso 1 1 calc R . . C11 C 0.7311(3) 0.2143(3) 0.7759(3) 0.0388(7) Uani 1 1 d . . . C6 C -0.0505(4) 0.4010(4) 1.2747(3) 0.0594(10) Uani 1 1 d . . . H6 H -0.1368 0.3982 1.3371 0.071 Uiso 1 1 calc R . . C5 C -0.0051(4) 0.3388(4) 1.1626(3) 0.0553(9) Uani 1 1 d . . . H5 H -0.0594 0.2921 1.1497 0.066 Uiso 1 1 calc R . . C7 C 0.0329(4) 0.4670(4) 1.2929(3) 0.0526(9) Uani 1 1 d . . . H7 H 0.0040 0.5100 1.3674 0.063 Uiso 1 1 calc R . . C14 C 1.0904(4) 0.1796(3) 0.5053(3) 0.0388(7) Uani 1 1 d . . . H14 H 1.1240 0.2351 0.4489 0.047 Uiso 1 1 calc R . . C2 C 0.2116(4) 0.2023(3) 0.7736(3) 0.0474(8) Uani 1 1 d . . . H2 H 0.1999 0.1598 0.7152 0.057 Uiso 1 1 calc R . . O2 O 1.6497(3) 0.3950(2) 0.1949(2) 0.0480(6) Uani 1 1 d . . . O1W O 0.5856(6) 0.3962(5) 0.5550(4) 0.1366(17) Uani 1 1 d D . . H1A H 0.491(3) 0.453(7) 0.584(5) 0.205 Uiso 1 1 d D . . H1B H 0.619(6) 0.376(6) 0.612(4) 0.15(3) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.03294(12) 0.03893(13) 0.03847(13) -0.00110(9) -0.00643(9) -0.02396(10) O1 0.0514(13) 0.0439(12) 0.0388(12) 0.0087(9) -0.0166(10) -0.0297(11) O5 0.0388(12) 0.0338(11) 0.0467(12) 0.0013(9) 0.0039(10) -0.0173(10) N1 0.0391(14) 0.0436(14) 0.0409(14) 0.0024(11) -0.0110(12) -0.0259(12) O3 0.0343(12) 0.0510(14) 0.0491(13) -0.0061(11) -0.0043(10) -0.0127(11) N3 0.0330(13) 0.0409(14) 0.0430(14) -0.0020(11) -0.0088(11) -0.0217(11) C16 0.0391(16) 0.0316(15) 0.0425(17) 0.0052(12) -0.0116(14) -0.0178(13) N2 0.0377(14) 0.0425(14) 0.0490(15) 0.0062(12) -0.0196(12) -0.0246(12) C8 0.0461(19) 0.053(2) 0.049(2) -0.0070(15) -0.0105(16) -0.0287(17) O4 0.0508(14) 0.0654(15) 0.0381(12) -0.0005(11) -0.0035(10) -0.0368(13) C19 0.0304(15) 0.0297(15) 0.0446(17) 0.0013(12) -0.0034(13) -0.0135(13) C1 0.0438(18) 0.0486(18) 0.0395(17) -0.0029(14) -0.0087(14) -0.0230(16) C3 0.0327(15) 0.0338(15) 0.0418(16) 0.0029(12) -0.0163(13) -0.0186(13) C24 0.0264(14) 0.0320(15) 0.0406(16) -0.0002(12) -0.0069(12) -0.0134(12) C15 0.0343(15) 0.0347(15) 0.0336(15) 0.0006(12) -0.0081(12) -0.0185(13) C4 0.0312(15) 0.0336(15) 0.0448(17) 0.0054(12) -0.0150(13) -0.0174(13) C12 0.0314(15) 0.0404(16) 0.0346(15) -0.0023(12) -0.0099(12) -0.0201(13) C10 0.0358(16) 0.053(2) 0.0524(19) 0.0036(15) -0.0147(15) -0.0270(15) C22 0.0272(14) 0.0305(14) 0.0379(15) 0.0017(12) -0.0081(12) -0.0143(12) C9 0.0382(17) 0.0508(19) 0.056(2) -0.0020(15) -0.0167(15) -0.0300(15) C18 0.054(2) 0.0495(19) 0.0304(16) 0.0051(13) -0.0125(14) -0.0266(16) C21 0.0417(17) 0.0368(16) 0.0345(16) 0.0018(12) -0.0102(13) -0.0200(14) C20 0.0402(16) 0.0360(16) 0.0397(17) -0.0008(13) -0.0109(14) -0.0213(14) C17 0.0423(17) 0.0420(16) 0.0316(15) 0.0082(12) -0.0117(13) -0.0270(14) C13 0.0374(16) 0.0323(15) 0.0435(17) 0.0005(13) -0.0129(14) -0.0161(13) C23 0.0438(17) 0.0432(17) 0.0426(17) 0.0034(13) -0.0176(14) -0.0251(15) C11 0.0342(16) 0.0530(19) 0.0365(16) -0.0098(14) -0.0093(13) -0.0255(15) C6 0.047(2) 0.085(3) 0.047(2) 0.0016(19) -0.0047(16) -0.038(2) C5 0.048(2) 0.081(3) 0.052(2) 0.0032(18) -0.0128(17) -0.045(2) C7 0.052(2) 0.061(2) 0.0442(19) -0.0060(16) -0.0086(16) -0.0278(18) C14 0.0399(17) 0.0385(16) 0.0365(16) 0.0046(13) -0.0088(13) -0.0191(14) C2 0.050(2) 0.055(2) 0.0448(19) -0.0048(15) -0.0161(16) -0.0279(17) O2 0.0508(13) 0.0540(14) 0.0602(14) 0.0136(11) -0.0276(11) -0.0363(12) O1W 0.190(5) 0.118(4) 0.118(3) 0.024(3) -0.109(4) -0.035(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O3 2.216(2) . ? Cd1 N1 2.270(2) . ? Cd1 O1 2.341(2) 1_456 ? Cd1 O1 2.3600(19) 2_766 ? Cd1 N3 2.369(2) . ? Cd1 O2 2.544(2) 2_766 ? O1 C24 1.267(3) . ? O1 Cd1 2.341(2) 1_654 ? O1 Cd1 2.3600(19) 2_766 ? O5 C15 1.378(3) . ? O5 C19 1.398(3) . ? N1 C3 1.327(3) . ? N1 C1 1.365(4) . ? O3 C11 1.276(4) . ? N3 C8 1.338(4) . ? N3 C4 1.351(3) . ? C16 C17 1.385(4) . ? C16 C15 1.386(4) . ? C16 H16 0.9300 . ? N2 C3 1.365(3) . ? N2 C2 1.366(4) . ? N2 C9 1.473(3) . ? C8 C7 1.378(4) . ? C8 H8 0.9300 . ? O4 C11 1.237(4) . ? C19 C20 1.375(4) . ? C19 C18 1.383(4) . ? C1 C2 1.354(4) . ? C1 H1 0.9300 . ? C3 C4 1.472(4) . ? C24 O2 1.249(3) . ? C24 C22 1.495(4) . ? C15 C14 1.389(4) . ? C4 C5 1.379(4) . ? C12 C17 1.382(4) . ? C12 C13 1.390(4) . ? C12 C11 1.506(4) . ? C10 C9 1.517(4) . ? C10 C10 1.528(5) 2_557 ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C22 C21 1.386(4) . ? C22 C23 1.388(4) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C18 C23 1.382(4) . ? C18 H18 0.9300 . ? C21 C20 1.387(4) . ? C21 H21 0.9300 . ? C20 H20 0.9300 . ? C17 H17 0.9300 . ? C13 C14 1.386(4) . ? C13 H13 0.9300 . ? C23 H23 0.9300 . ? C6 C7 1.371(5) . ? C6 C5 1.382(5) . ? C6 H6 0.9300 . ? C5 H5 0.9300 . ? C7 H7 0.9300 . ? C14 H14 0.9300 . ? C2 H2 0.9300 . ? O2 Cd1 2.544(2) 2_766 ? O1W H1A 0.85(6) . ? O1W H1B 0.85(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Cd1 N1 99.50(9) . . ? O3 Cd1 O1 92.97(8) . 1_456 ? N1 Cd1 O1 144.74(8) . 1_456 ? O3 Cd1 O1 87.98(8) . 2_766 ? N1 Cd1 O1 140.43(8) . 2_766 ? O1 Cd1 O1 72.33(8) 1_456 2_766 ? O3 Cd1 N3 165.55(8) . . ? N1 Cd1 N3 70.49(8) . . ? O1 Cd1 N3 90.07(8) 1_456 . ? O1 Cd1 N3 106.39(8) 2_766 . ? O3 Cd1 O2 80.75(8) . 2_766 ? N1 Cd1 O2 89.79(8) . 2_766 ? O1 Cd1 O2 124.88(7) 1_456 2_766 ? O1 Cd1 O2 52.88(7) 2_766 2_766 ? N3 Cd1 O2 108.93(8) . 2_766 ? C24 O1 Cd1 151.55(18) . 1_654 ? C24 O1 Cd1 95.19(16) . 2_766 ? Cd1 O1 Cd1 107.67(8) 1_654 2_766 ? C15 O5 C19 116.7(2) . . ? C3 N1 C1 107.2(2) . . ? C3 N1 Cd1 117.88(19) . . ? C1 N1 Cd1 134.8(2) . . ? C11 O3 Cd1 106.60(19) . . ? C8 N3 C4 119.0(3) . . ? C8 N3 Cd1 123.4(2) . . ? C4 N3 Cd1 117.45(19) . . ? C17 C16 C15 119.5(3) . . ? C17 C16 H16 120.3 . . ? C15 C16 H16 120.3 . . ? C3 N2 C2 107.0(2) . . ? C3 N2 C9 131.6(3) . . ? C2 N2 C9 121.1(3) . . ? N3 C8 C7 122.7(3) . . ? N3 C8 H8 118.6 . . ? C7 C8 H8 118.6 . . ? C20 C19 C18 121.5(3) . . ? C20 C19 O5 119.1(3) . . ? C18 C19 O5 119.4(3) . . ? C2 C1 N1 108.9(3) . . ? C2 C1 H1 125.6 . . ? N1 C1 H1 125.6 . . ? N1 C3 N2 109.7(3) . . ? N1 C3 C4 120.4(2) . . ? N2 C3 C4 129.9(3) . . ? O2 C24 O1 120.9(3) . . ? O2 C24 C22 119.6(3) . . ? O1 C24 C22 119.4(2) . . ? O5 C15 C16 116.9(3) . . ? O5 C15 C14 122.7(2) . . ? C16 C15 C14 120.4(3) . . ? N3 C4 C5 120.7(3) . . ? N3 C4 C3 113.3(2) . . ? C5 C4 C3 126.1(3) . . ? C17 C12 C13 118.4(3) . . ? C17 C12 C11 121.8(3) . . ? C13 C12 C11 119.8(3) . . ? C9 C10 C10 111.9(3) . 2_557 ? C9 C10 H10A 109.2 . . ? C10 C10 H10A 109.2 2_557 . ? C9 C10 H10B 109.2 . . ? C10 C10 H10B 109.2 2_557 . ? H10A C10 H10B 107.9 . . ? C21 C22 C23 119.3(3) . . ? C21 C22 C24 121.8(3) . . ? C23 C22 C24 118.7(2) . . ? N2 C9 C10 111.5(2) . . ? N2 C9 H9A 109.3 . . ? C10 C9 H9A 109.3 . . ? N2 C9 H9B 109.3 . . ? C10 C9 H9B 109.3 . . ? H9A C9 H9B 108.0 . . ? C23 C18 C19 119.1(3) . . ? C23 C18 H18 120.4 . . ? C19 C18 H18 120.4 . . ? C22 C21 C20 120.7(3) . . ? C22 C21 H21 119.6 . . ? C20 C21 H21 119.6 . . ? C19 C20 C21 118.9(3) . . ? C19 C20 H20 120.6 . . ? C21 C20 H20 120.6 . . ? C12 C17 C16 121.3(3) . . ? C12 C17 H17 119.4 . . ? C16 C17 H17 119.4 . . ? C14 C13 C12 121.4(3) . . ? C14 C13 H13 119.3 . . ? C12 C13 H13 119.3 . . ? C18 C23 C22 120.4(3) . . ? C18 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? O4 C11 O3 123.6(3) . . ? O4 C11 C12 120.5(3) . . ? O3 C11 C12 115.9(3) . . ? C7 C6 C5 119.4(3) . . ? C7 C6 H6 120.3 . . ? C5 C6 H6 120.3 . . ? C4 C5 C6 119.8(3) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? C6 C7 C8 118.4(3) . . ? C6 C7 H7 120.8 . . ? C8 C7 H7 120.8 . . ? C13 C14 C15 119.0(3) . . ? C13 C14 H14 120.5 . . ? C15 C14 H14 120.5 . . ? C1 C2 N2 107.2(3) . . ? C1 C2 H2 126.4 . . ? N2 C2 H2 126.4 . . ? C24 O2 Cd1 87.16(17) . 2_766 ? H1A O1W H1B 107(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 O3 Cd1 N1 C3 162.9(2) . . . . ? O1 Cd1 N1 C3 53.7(3) 1_456 . . . ? O1 Cd1 N1 C3 -98.7(2) 2_766 . . . ? N3 Cd1 N1 C3 -6.4(2) . . . . ? O2 Cd1 N1 C3 -116.6(2) 2_766 . . . ? O3 Cd1 N1 C1 -12.0(3) . . . . ? O1 Cd1 N1 C1 -121.1(3) 1_456 . . . ? O1 Cd1 N1 C1 86.4(3) 2_766 . . . ? N3 Cd1 N1 C1 178.8(3) . . . . ? O2 Cd1 N1 C1 68.6(3) 2_766 . . . ? N1 Cd1 O3 C11 -79.89(19) . . . . ? O1 Cd1 O3 C11 67.01(19) 1_456 . . . ? O1 Cd1 O3 C11 139.20(19) 2_766 . . . ? N3 Cd1 O3 C11 -34.9(4) . . . . ? O2 Cd1 O3 C11 -168.11(19) 2_766 . . . ? O3 Cd1 N3 C8 134.9(3) . . . . ? N1 Cd1 N3 C8 -177.4(3) . . . . ? O1 Cd1 N3 C8 32.6(3) 1_456 . . . ? O1 Cd1 N3 C8 -39.0(3) 2_766 . . . ? O2 Cd1 N3 C8 -94.6(3) 2_766 . . . ? O3 Cd1 N3 C4 -41.6(5) . . . . ? N1 Cd1 N3 C4 6.1(2) . . . . ? O1 Cd1 N3 C4 -143.9(2) 1_456 . . . ? O1 Cd1 N3 C4 144.6(2) 2_766 . . . ? O2 Cd1 N3 C4 88.9(2) 2_766 . . . ? C4 N3 C8 C7 -0.9(5) . . . . ? Cd1 N3 C8 C7 -177.3(3) . . . . ? C15 O5 C19 C20 -113.8(3) . . . . ? C15 O5 C19 C18 68.4(4) . . . . ? C3 N1 C1 C2 0.8(4) . . . . ? Cd1 N1 C1 C2 176.0(2) . . . . ? C1 N1 C3 N2 -0.7(3) . . . . ? Cd1 N1 C3 N2 -176.91(18) . . . . ? C1 N1 C3 C4 -177.4(3) . . . . ? Cd1 N1 C3 C4 6.4(4) . . . . ? C2 N2 C3 N1 0.4(3) . . . . ? C9 N2 C3 N1 174.2(3) . . . . ? C2 N2 C3 C4 176.7(3) . . . . ? C9 N2 C3 C4 -9.6(5) . . . . ? Cd1 O1 C24 O2 -164.7(3) 1_654 . . . ? Cd1 O1 C24 O2 -20.8(3) 2_766 . . . ? Cd1 O1 C24 C22 12.1(6) 1_654 . . . ? Cd1 O1 C24 C22 156.0(2) 2_766 . . . ? C19 O5 C15 C16 -165.1(3) . . . . ? C19 O5 C15 C14 17.0(4) . . . . ? C17 C16 C15 O5 -178.4(3) . . . . ? C17 C16 C15 C14 -0.4(4) . . . . ? C8 N3 C4 C5 -1.1(5) . . . . ? Cd1 N3 C4 C5 175.5(2) . . . . ? C8 N3 C4 C3 178.3(3) . . . . ? Cd1 N3 C4 C3 -5.1(3) . . . . ? N1 C3 C4 N3 -0.7(4) . . . . ? N2 C3 C4 N3 -176.6(3) . . . . ? N1 C3 C4 C5 178.6(3) . . . . ? N2 C3 C4 C5 2.7(5) . . . . ? O2 C24 C22 C21 -165.1(3) . . . . ? O1 C24 C22 C21 18.1(4) . . . . ? O2 C24 C22 C23 19.4(4) . . . . ? O1 C24 C22 C23 -157.5(3) . . . . ? C3 N2 C9 C10 -88.0(4) . . . . ? C2 N2 C9 C10 85.1(4) . . . . ? C10 C10 C9 N2 -178.7(3) 2_557 . . . ? C20 C19 C18 C23 2.7(5) . . . . ? O5 C19 C18 C23 -179.6(3) . . . . ? C23 C22 C21 C20 2.5(4) . . . . ? C24 C22 C21 C20 -173.0(3) . . . . ? C18 C19 C20 C21 -2.3(5) . . . . ? O5 C19 C20 C21 180.0(3) . . . . ? C22 C21 C20 C19 -0.4(4) . . . . ? C13 C12 C17 C16 0.4(4) . . . . ? C11 C12 C17 C16 -179.4(3) . . . . ? C15 C16 C17 C12 0.0(4) . . . . ? C17 C12 C13 C14 -0.5(4) . . . . ? C11 C12 C13 C14 179.4(3) . . . . ? C19 C18 C23 C22 -0.5(5) . . . . ? C21 C22 C23 C18 -2.1(4) . . . . ? C24 C22 C23 C18 173.6(3) . . . . ? Cd1 O3 C11 O4 2.1(3) . . . . ? Cd1 O3 C11 C12 -176.93(18) . . . . ? C17 C12 C11 O4 5.1(4) . . . . ? C13 C12 C11 O4 -174.8(3) . . . . ? C17 C12 C11 O3 -175.9(3) . . . . ? C13 C12 C11 O3 4.3(4) . . . . ? N3 C4 C5 C6 2.2(5) . . . . ? C3 C4 C5 C6 -177.1(3) . . . . ? C7 C6 C5 C4 -1.4(6) . . . . ? C5 C6 C7 C8 -0.4(6) . . . . ? N3 C8 C7 C6 1.6(6) . . . . ? C12 C13 C14 C15 0.1(5) . . . . ? O5 C15 C14 C13 178.2(3) . . . . ? C16 C15 C14 C13 0.3(4) . . . . ? N1 C1 C2 N2 -0.5(4) . . . . ? C3 N2 C2 C1 0.1(4) . . . . ? C9 N2 C2 C1 -174.5(3) . . . . ? O1 C24 O2 Cd1 19.2(3) . . . 2_766 ? C22 C24 O2 Cd1 -157.6(2) . . . 2_766 ? 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 O1W H1B O3 0.85(6) 1.99(5) 2.825(5) 167(6) . _diffrn_measured_fraction_theta_max 0.926 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.449 _refine_diff_density_min -0.409 _refine_diff_density_rms 0.076 data_5 _database_code_depnum_ccdc_archive 'CCDC 687552' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C66 H44 N6 O15 Zn3' _chemical_formula_weight 1357.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' 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 14.3040(4) _cell_length_b 17.4700(4) _cell_length_c 25.6360(10) _cell_angle_alpha 90.00 _cell_angle_beta 94.0690(10) _cell_angle_gamma 90.00 _cell_volume 6390.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.84 _cell_measurement_theta_max 28.32 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.31 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.411 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2768 _exptl_absorpt_coefficient_mu 1.188 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.674 _exptl_absorpt_correction_T_max 0.692 _exptl_absorpt_process_details 'SADABS(Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19563 _diffrn_reflns_av_R_equivalents 0.0288 _diffrn_reflns_av_sigmaI/netI 0.0348 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 28.32 _reflns_number_total 7664 _reflns_number_gt 6163 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SMART (Bruker, 1997)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97(Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material SHELXL-97 _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^)+(0.0652P)^2^+10.3681P] 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 7664 _refine_ls_number_parameters 408 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0522 _refine_ls_R_factor_gt 0.0399 _refine_ls_wR_factor_ref 0.1272 _refine_ls_wR_factor_gt 0.1202 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.003 _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 Zn2 Zn 0.2500 0.2500 0.5000 0.01746(10) Uani 1 2 d S . . Zn1 Zn 0.48607(2) 0.331929(19) 0.505698(12) 0.03196(10) Uani 1 1 d . . . O4 O 0.34561(16) 0.18157(14) 0.45558(9) 0.0491(6) Uani 1 1 d . . . O8 O 0.5000 0.04649(18) 0.2500 0.0446(7) Uani 1 2 d S . . O5 O 0.27099(17) 0.34997(14) 0.44487(10) 0.0539(6) Uani 1 1 d . . . O7 O 0.2380(2) 0.62324(16) 0.28161(9) 0.0645(8) Uani 1 1 d . . . N1 N 0.59620(19) 0.27199(16) 0.56363(10) 0.0434(6) Uani 1 1 d . . . N3 N 0.76515(17) 0.40243(16) 0.51190(11) 0.0435(6) Uani 1 1 d . . . O3 O 0.48310(17) 0.24315(13) 0.45540(9) 0.0484(5) Uani 1 1 d . . . C19 C 0.3523(2) 0.64768(18) 0.13840(11) 0.0389(6) Uani 1 1 d . . . C2 C 0.4431(2) 0.15742(18) 0.38732(11) 0.0370(6) Uani 1 1 d . . . C16 C 0.2808(2) 0.6290(2) 0.23505(12) 0.0453(7) Uani 1 1 d . . . C10 C 0.3087(2) 0.45485(18) 0.39177(11) 0.0369(6) Uani 1 1 d . . . C15 C 0.3674(2) 0.5161(2) 0.38577(12) 0.0454(7) Uani 1 1 d . . . H15 H 0.4224 0.5203 0.4072 0.055 Uiso 1 1 calc R . . C33 C 1.0046(2) 0.5748(2) 0.51505(14) 0.0515(8) Uani 1 1 d . . . H33 H 1.0075 0.6257 0.5256 0.062 Uiso 1 1 calc R . . C25 C 0.6856(2) 0.29269(18) 0.55720(12) 0.0407(7) Uani 1 1 d . . . C9 C 0.3325(2) 0.39641(18) 0.43375(11) 0.0377(6) Uani 1 1 d . . . C6 C 0.4198(2) 0.05309(19) 0.32692(11) 0.0431(7) Uani 1 1 d . . . H6 H 0.3914 0.0067 0.3176 0.052 Uiso 1 1 calc R . . O6 O 0.41445(16) 0.40037(14) 0.45461(9) 0.0508(6) Uani 1 1 d . . . N2 N 0.61438(17) 0.38067(16) 0.49331(10) 0.0408(6) Uani 1 1 d . . . C7 C 0.4008(2) 0.08863(19) 0.37315(12) 0.0452(7) Uani 1 1 d . . . H7 H 0.3593 0.0661 0.3949 0.054 Uiso 1 1 calc R . . C24 C 0.69121(19) 0.35654(18) 0.52090(11) 0.0368(6) Uani 1 1 d . . . C5 C 0.4811(2) 0.08661(18) 0.29468(10) 0.0378(6) Uani 1 1 d . . . C32 C 0.9350(2) 0.5282(2) 0.53182(14) 0.0530(8) Uani 1 1 d . . . H32 H 0.8912 0.5481 0.5533 0.064 Uiso 1 1 calc R . . C14 C 0.3457(3) 0.5717(2) 0.34817(13) 0.0519(8) Uani 1 1 d . . . H14 H 0.3853 0.6133 0.3446 0.062 Uiso 1 1 calc R . . C29 C 0.5806(3) 0.2184(2) 0.59912(15) 0.0580(9) Uani 1 1 d . . . H29 H 0.5190 0.2055 0.6045 0.070 Uiso 1 1 calc R . . C18 C 0.2946(2) 0.70334(19) 0.15797(11) 0.0419(7) Uani 1 1 d . . . H18 H 0.2798 0.7470 0.1383 0.050 Uiso 1 1 calc R . . C23 C 0.7324(2) 0.4580(2) 0.47735(14) 0.0528(9) Uani 1 1 d . . . H23 H 0.7669 0.4979 0.4643 0.063 Uiso 1 1 calc R . . C13 C 0.2649(2) 0.5646(2) 0.31638(12) 0.0476(8) Uani 1 1 d . . . C21 C 0.3380(3) 0.5735(2) 0.21662(13) 0.0547(9) Uani 1 1 d . . . H21 H 0.3525 0.5299 0.2364 0.066 Uiso 1 1 calc R . . C11 C 0.2280(2) 0.4485(2) 0.35875(13) 0.0478(8) Uani 1 1 d . . . H11 H 0.1880 0.4071 0.3622 0.057 Uiso 1 1 calc R . . C3 C 0.5052(2) 0.1901(2) 0.35476(12) 0.0428(7) Uani 1 1 d . . . H3 H 0.5339 0.2363 0.3642 0.051 Uiso 1 1 calc R . . C20 C 0.3735(3) 0.5833(2) 0.16844(13) 0.0515(8) Uani 1 1 d . . . H20 H 0.4125 0.5460 0.1559 0.062 Uiso 1 1 calc R . . C4 C 0.5252(2) 0.1553(2) 0.30851(12) 0.0433(7) Uani 1 1 d . . . H4 H 0.5673 0.1775 0.2870 0.052 Uiso 1 1 calc R . . C26 C 0.7598(3) 0.2560(2) 0.58393(18) 0.0657(11) Uani 1 1 d . . . H26 H 0.8212 0.2694 0.5782 0.079 Uiso 1 1 calc R . . C12 C 0.2064(3) 0.5031(2) 0.32084(13) 0.0541(9) Uani 1 1 d . . . H12 H 0.1526 0.4982 0.2985 0.065 Uiso 1 1 calc R . . C17 C 0.2592(2) 0.6943(2) 0.20611(12) 0.0469(8) Uani 1 1 d . . . H17 H 0.2210 0.7318 0.2191 0.056 Uiso 1 1 calc R . . C1 C 0.4214(2) 0.19740(19) 0.43678(11) 0.0402(7) Uani 1 1 d . . . C30 C 0.8603(2) 0.3981(2) 0.53853(16) 0.0605(10) Uani 1 1 d . . . H30A H 0.8837 0.3464 0.5354 0.073 Uiso 1 1 calc R . . H30B H 0.8560 0.4087 0.5754 0.073 Uiso 1 1 calc R . . C31 C 0.9299(2) 0.4530(2) 0.51711(13) 0.0452(7) Uani 1 1 d . . . C22 C 0.6398(2) 0.4434(2) 0.46595(14) 0.0499(8) Uani 1 1 d . . . H22 H 0.6000 0.4717 0.4431 0.060 Uiso 1 1 calc R . . C28 C 0.6510(3) 0.1818(3) 0.6279(2) 0.0827(15) Uani 1 1 d . . . H28 H 0.6377 0.1457 0.6530 0.099 Uiso 1 1 calc R . . C27 C 0.7419(3) 0.1997(3) 0.6188(2) 0.0892(17) Uani 1 1 d . . . H27 H 0.7913 0.1736 0.6365 0.107 Uiso 1 1 calc R . . C8 C 0.3925(2) 0.65681(19) 0.08701(11) 0.0382(6) Uani 1 1 d . . . O2 O 0.37338(14) 0.71470(14) 0.05869(8) 0.0434(5) Uani 1 1 d . . . O1 O 0.44897(16) 0.60725(14) 0.07298(8) 0.0490(5) 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 Zn2 0.01431(17) 0.02301(19) 0.01539(16) -0.00099(13) 0.00334(12) -0.00278(14) Zn1 0.02747(17) 0.03989(19) 0.02837(16) 0.00047(12) 0.00087(12) -0.00095(13) O4 0.0477(13) 0.0587(14) 0.0423(12) -0.0078(10) 0.0122(10) 0.0046(11) O8 0.060(2) 0.0467(17) 0.0280(14) 0.000 0.0085(13) 0.000 O5 0.0501(14) 0.0552(14) 0.0563(14) 0.0220(12) 0.0022(11) -0.0060(11) O7 0.0762(18) 0.0775(18) 0.0430(13) 0.0282(12) 0.0252(12) 0.0340(15) N1 0.0432(14) 0.0429(14) 0.0444(14) 0.0005(12) 0.0046(11) -0.0041(12) N3 0.0301(12) 0.0505(16) 0.0498(15) 0.0116(12) 0.0025(11) -0.0014(11) O3 0.0492(13) 0.0528(14) 0.0428(12) -0.0112(10) 0.0004(10) 0.0021(11) C19 0.0380(15) 0.0484(17) 0.0303(13) 0.0068(12) 0.0029(11) 0.0039(13) C2 0.0360(15) 0.0443(16) 0.0307(13) -0.0007(12) 0.0014(11) 0.0056(12) C16 0.0452(17) 0.057(2) 0.0341(14) 0.0136(14) 0.0089(13) 0.0092(15) C10 0.0360(15) 0.0439(16) 0.0308(13) 0.0048(12) 0.0014(11) 0.0020(12) C15 0.0434(17) 0.0518(19) 0.0405(16) 0.0071(14) -0.0020(13) -0.0060(15) C33 0.0487(18) 0.0448(18) 0.060(2) 0.0011(16) -0.0004(16) -0.0020(15) C25 0.0362(15) 0.0411(17) 0.0441(16) 0.0035(13) -0.0012(12) -0.0030(13) C9 0.0384(15) 0.0416(16) 0.0331(14) 0.0029(12) 0.0023(12) 0.0026(12) C6 0.0527(18) 0.0409(16) 0.0363(15) -0.0006(13) 0.0070(13) -0.0048(14) O6 0.0445(12) 0.0542(14) 0.0516(13) 0.0137(11) -0.0110(10) 0.0022(11) N2 0.0331(12) 0.0485(15) 0.0406(13) 0.0075(11) 0.0019(10) 0.0005(11) C7 0.0513(18) 0.0494(18) 0.0362(15) 0.0027(14) 0.0121(13) -0.0022(15) C24 0.0288(13) 0.0423(16) 0.0390(15) 0.0030(12) 0.0009(11) -0.0005(12) C5 0.0403(15) 0.0468(17) 0.0262(12) -0.0001(12) 0.0010(11) 0.0028(13) C32 0.0441(18) 0.055(2) 0.061(2) 0.0056(17) 0.0138(16) 0.0021(16) C14 0.056(2) 0.051(2) 0.0501(18) 0.0140(15) 0.0108(16) -0.0032(16) C29 0.054(2) 0.054(2) 0.067(2) 0.0149(18) 0.0073(18) -0.0095(17) C18 0.0460(17) 0.0455(17) 0.0345(14) 0.0110(13) 0.0045(12) 0.0077(14) C23 0.0378(17) 0.061(2) 0.060(2) 0.0251(18) 0.0031(15) -0.0031(15) C13 0.0508(19) 0.058(2) 0.0350(15) 0.0159(14) 0.0126(14) 0.0159(16) C21 0.065(2) 0.056(2) 0.0445(17) 0.0223(16) 0.0137(16) 0.0238(18) C11 0.0394(17) 0.056(2) 0.0475(17) 0.0072(15) -0.0023(14) -0.0041(15) C3 0.0409(16) 0.0479(18) 0.0394(15) -0.0048(13) 0.0025(13) -0.0056(14) C20 0.059(2) 0.054(2) 0.0421(17) 0.0100(15) 0.0120(15) 0.0198(17) C4 0.0391(16) 0.057(2) 0.0341(14) -0.0002(13) 0.0071(12) -0.0064(14) C26 0.0428(19) 0.065(2) 0.087(3) 0.032(2) -0.0110(19) -0.0048(17) C12 0.0474(19) 0.074(3) 0.0390(16) 0.0097(16) -0.0075(14) 0.0070(17) C17 0.0470(18) 0.0549(19) 0.0393(16) 0.0089(14) 0.0072(14) 0.0145(15) C1 0.0435(16) 0.0428(16) 0.0339(14) -0.0004(12) -0.0002(13) 0.0094(14) C30 0.0315(16) 0.072(3) 0.077(2) 0.030(2) -0.0062(16) -0.0082(16) C31 0.0255(14) 0.0534(19) 0.0560(19) 0.0146(15) -0.0019(13) -0.0032(13) C22 0.0394(17) 0.058(2) 0.0514(18) 0.0187(16) 0.0005(14) 0.0027(15) C28 0.075(3) 0.079(3) 0.092(3) 0.049(3) -0.009(3) -0.013(2) C27 0.063(3) 0.088(3) 0.113(4) 0.055(3) -0.018(3) -0.006(2) C8 0.0324(14) 0.0515(18) 0.0304(13) 0.0035(12) 0.0002(11) -0.0021(13) O2 0.0374(11) 0.0575(14) 0.0347(10) 0.0140(10) -0.0011(9) 0.0002(10) O1 0.0482(13) 0.0587(14) 0.0411(12) 0.0018(10) 0.0101(10) 0.0085(11) _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 Zn2 O4 2.195(2) . ? Zn2 O4 2.195(2) 7_556 ? Zn2 O5 2.280(2) 7_556 ? Zn2 O5 2.280(2) . ? Zn2 O2 2.320(2) 4_545 ? Zn2 O2 2.320(2) 6_566 ? Zn1 O6 2.001(2) . ? Zn1 O3 2.015(2) . ? Zn1 N2 2.068(3) . ? Zn1 O1 2.125(2) 6_566 ? Zn1 O2 2.328(2) 6_566 ? Zn1 N1 2.335(3) . ? Zn1 C8 2.564(3) 6_566 ? O4 C1 1.248(4) . ? O8 C5 1.386(3) 2_655 ? O8 C5 1.386(3) . ? O5 C9 1.244(4) . ? O7 C16 1.383(4) . ? O7 C13 1.394(4) . ? N1 C29 1.335(4) . ? N1 C25 1.350(4) . ? N3 C24 1.360(4) . ? N3 C23 1.373(4) . ? N3 C30 1.480(4) . ? O3 C1 1.259(4) . ? C19 C20 1.385(4) . ? C19 C18 1.391(4) . ? C19 C8 1.483(4) . ? C2 C7 1.382(5) . ? C2 C3 1.384(4) . ? C2 C1 1.499(4) . ? C16 C21 1.374(5) . ? C16 C17 1.383(4) . ? C10 C15 1.375(4) . ? C10 C11 1.387(4) . ? C10 C9 1.505(4) . ? C15 C14 1.389(4) . ? C15 H15 0.9300 . ? C33 C31 1.379(5) 5_766 ? C33 C32 1.377(5) . ? C33 H33 0.9300 . ? C25 C26 1.380(5) . ? C25 C24 1.459(4) . ? C9 O6 1.256(4) . ? C6 C5 1.377(4) . ? C6 C7 1.382(4) . ? C6 H6 0.9300 . ? N2 C24 1.332(4) . ? N2 C22 1.364(4) . ? C7 H7 0.9300 . ? C5 C4 1.390(4) . ? C32 C31 1.367(5) . ? C32 H32 0.9300 . ? C14 C13 1.372(5) . ? C14 H14 0.9300 . ? C29 C28 1.365(6) . ? C29 H29 0.9300 . ? C18 C17 1.376(4) . ? C18 H18 0.9300 . ? C23 C22 1.360(5) . ? C23 H23 0.9300 . ? C13 C12 1.371(5) . ? C21 C20 1.380(5) . ? C21 H21 0.9300 . ? C11 C12 1.381(5) . ? C11 H11 0.9300 . ? C3 C4 1.380(4) . ? C3 H3 0.9300 . ? C20 H20 0.9300 . ? C4 H4 0.9300 . ? C26 C27 1.366(6) . ? C26 H26 0.9300 . ? C12 H12 0.9300 . ? C17 H17 0.9300 . ? C30 C31 1.513(4) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C33 1.379(5) 5_766 ? C22 H22 0.9300 . ? C28 C27 1.374(7) . ? C28 H28 0.9300 . ? C27 H27 0.9300 . ? C8 O1 1.254(4) . ? C8 O2 1.263(4) . ? C8 Zn1 2.564(3) 6_565 ? O2 Zn2 2.320(2) 4 ? O2 Zn1 2.328(2) 6_565 ? O1 Zn1 2.125(2) 6_565 ? 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 O4 Zn2 O4 180.00(10) . 7_556 ? O4 Zn2 O5 91.07(9) . 7_556 ? O4 Zn2 O5 88.93(9) 7_556 7_556 ? O4 Zn2 O5 88.93(9) . . ? O4 Zn2 O5 91.07(9) 7_556 . ? O5 Zn2 O5 180.0 7_556 . ? O4 Zn2 O2 89.55(8) . 4_545 ? O4 Zn2 O2 90.45(8) 7_556 4_545 ? O5 Zn2 O2 94.06(9) 7_556 4_545 ? O5 Zn2 O2 85.94(9) . 4_545 ? O4 Zn2 O2 90.45(8) . 6_566 ? O4 Zn2 O2 89.55(8) 7_556 6_566 ? O5 Zn2 O2 85.94(9) 7_556 6_566 ? O5 Zn2 O2 94.06(9) . 6_566 ? O2 Zn2 O2 180.00(8) 4_545 6_566 ? O6 Zn1 O3 93.12(10) . . ? O6 Zn1 N2 94.14(10) . . ? O3 Zn1 N2 101.37(10) . . ? O6 Zn1 O1 94.97(10) . 6_566 ? O3 Zn1 O1 155.36(10) . 6_566 ? N2 Zn1 O1 101.20(10) . 6_566 ? O6 Zn1 O2 104.33(9) . 6_566 ? O3 Zn1 O2 96.89(9) . 6_566 ? N2 Zn1 O2 153.20(9) . 6_566 ? O1 Zn1 O2 58.54(8) 6_566 6_566 ? O6 Zn1 N1 167.23(10) . . ? O3 Zn1 N1 92.55(10) . . ? N2 Zn1 N1 73.52(9) . . ? O1 Zn1 N1 84.49(9) 6_566 . ? O2 Zn1 N1 86.31(8) 6_566 . ? O6 Zn1 C8 102.34(10) . 6_566 ? O3 Zn1 C8 126.21(10) . 6_566 ? N2 Zn1 C8 127.85(10) . 6_566 ? O1 Zn1 C8 29.16(9) 6_566 6_566 ? O2 Zn1 C8 29.44(9) 6_566 6_566 ? N1 Zn1 C8 83.39(9) . 6_566 ? C1 O4 Zn2 132.1(2) . . ? C5 O8 C5 119.2(3) 2_655 . ? C9 O5 Zn2 140.2(2) . . ? C16 O7 C13 119.1(3) . . ? C29 N1 C25 118.4(3) . . ? C29 N1 Zn1 127.6(2) . . ? C25 N1 Zn1 113.8(2) . . ? C24 N3 C23 107.0(3) . . ? C24 N3 C30 126.3(3) . . ? C23 N3 C30 126.4(3) . . ? C1 O3 Zn1 135.5(2) . . ? C20 C19 C18 118.7(3) . . ? C20 C19 C8 119.8(3) . . ? C18 C19 C8 121.5(3) . . ? C7 C2 C3 119.2(3) . . ? C7 C2 C1 120.9(3) . . ? C3 C2 C1 119.9(3) . . ? C21 C16 O7 123.8(3) . . ? C21 C16 C17 120.9(3) . . ? O7 C16 C17 115.3(3) . . ? C15 C10 C11 118.8(3) . . ? C15 C10 C9 120.0(3) . . ? C11 C10 C9 121.2(3) . . ? C10 C15 C14 120.9(3) . . ? C10 C15 H15 119.5 . . ? C14 C15 H15 119.5 . . ? C31 C33 C32 121.0(3) 5_766 . ? C31 C33 H33 119.5 5_766 . ? C32 C33 H33 119.5 . . ? N1 C25 C26 121.1(3) . . ? N1 C25 C24 112.2(3) . . ? C26 C25 C24 126.6(3) . . ? O5 C9 O6 126.3(3) . . ? O5 C9 C10 118.6(3) . . ? O6 C9 C10 115.1(3) . . ? C5 C6 C7 119.7(3) . . ? C5 C6 H6 120.1 . . ? C7 C6 H6 120.1 . . ? C9 O6 Zn1 131.7(2) . . ? C24 N2 C22 106.7(3) . . ? C24 N2 Zn1 119.7(2) . . ? C22 N2 Zn1 133.0(2) . . ? C6 C7 C2 120.5(3) . . ? C6 C7 H7 119.8 . . ? C2 C7 H7 119.8 . . ? N2 C24 N3 110.2(3) . . ? N2 C24 C25 120.0(3) . . ? N3 C24 C25 129.6(3) . . ? C6 C5 O8 116.8(3) . . ? C6 C5 C4 120.7(3) . . ? O8 C5 C4 122.4(3) . . ? C31 C32 C33 120.4(3) . . ? C31 C32 H32 119.8 . . ? C33 C32 H32 119.8 . . ? C13 C14 C15 119.1(3) . . ? C13 C14 H14 120.4 . . ? C15 C14 H14 120.4 . . ? N1 C29 C28 123.0(4) . . ? N1 C29 H29 118.5 . . ? C28 C29 H29 118.5 . . ? C17 C18 C19 120.6(3) . . ? C17 C18 H18 119.7 . . ? C19 C18 H18 119.7 . . ? C22 C23 N3 106.8(3) . . ? C22 C23 H23 126.6 . . ? N3 C23 H23 126.6 . . ? C12 C13 C14 121.0(3) . . ? C12 C13 O7 119.2(3) . . ? C14 C13 O7 119.7(3) . . ? C16 C21 C20 119.1(3) . . ? C16 C21 H21 120.4 . . ? C20 C21 H21 120.4 . . ? C12 C11 C10 120.6(3) . . ? C12 C11 H11 119.7 . . ? C10 C11 H11 119.7 . . ? C4 C3 C2 121.2(3) . . ? C4 C3 H3 119.4 . . ? C2 C3 H3 119.4 . . ? C21 C20 C19 121.2(3) . . ? C21 C20 H20 119.4 . . ? C19 C20 H20 119.4 . . ? C3 C4 C5 118.8(3) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? C27 C26 C25 119.1(4) . . ? C27 C26 H26 120.4 . . ? C25 C26 H26 120.4 . . ? C13 C12 C11 119.5(3) . . ? C13 C12 H12 120.2 . . ? C11 C12 H12 120.2 . . ? C18 C17 C16 119.6(3) . . ? C18 C17 H17 120.2 . . ? C16 C17 H17 120.2 . . ? O4 C1 O3 126.8(3) . . ? O4 C1 C2 117.5(3) . . ? O3 C1 C2 115.8(3) . . ? N3 C30 C31 114.0(3) . . ? N3 C30 H30A 108.7 . . ? C31 C30 H30A 108.7 . . ? N3 C30 H30B 108.7 . . ? C31 C30 H30B 108.7 . . ? H30A C30 H30B 107.6 . . ? C32 C31 C33 118.5(3) . 5_766 ? C32 C31 C30 122.2(3) . . ? C33 C31 C30 119.1(3) 5_766 . ? C23 C22 N2 109.4(3) . . ? C23 C22 H22 125.3 . . ? N2 C22 H22 125.3 . . ? C29 C28 C27 118.2(4) . . ? C29 C28 H28 120.9 . . ? C27 C28 H28 120.9 . . ? C26 C27 C28 119.9(4) . . ? C26 C27 H27 120.1 . . ? C28 C27 H27 120.1 . . ? O1 C8 O2 120.3(3) . . ? O1 C8 C19 118.6(3) . . ? O2 C8 C19 121.0(3) . . ? O1 C8 Zn1 55.64(15) . 6_565 ? O2 C8 Zn1 64.88(15) . 6_565 ? C19 C8 Zn1 171.3(2) . 6_565 ? C8 O2 Zn2 135.1(2) . 4 ? C8 O2 Zn1 85.69(18) . 6_565 ? Zn2 O2 Zn1 103.95(8) 4 6_565 ? C8 O1 Zn1 95.20(19) . 6_565 ? 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 Zn2 O4 C1 -138.1(3) 7_556 . . . ? O5 Zn2 O4 C1 41.9(3) . . . . ? O2 Zn2 O4 C1 127.8(3) 4_545 . . . ? O2 Zn2 O4 C1 -52.2(3) 6_566 . . . ? O4 Zn2 O5 C9 -69.3(4) . . . . ? O4 Zn2 O5 C9 110.7(4) 7_556 . . . ? O2 Zn2 O5 C9 -159.0(4) 4_545 . . . ? O2 Zn2 O5 C9 21.0(4) 6_566 . . . ? O6 Zn1 N1 C29 162.9(4) . . . . ? O3 Zn1 N1 C29 -80.7(3) . . . . ? N2 Zn1 N1 C29 178.2(3) . . . . ? O1 Zn1 N1 C29 74.7(3) 6_566 . . . ? O2 Zn1 N1 C29 16.0(3) 6_566 . . . ? C8 Zn1 N1 C29 45.4(3) 6_566 . . . ? O6 Zn1 N1 C25 -20.8(6) . . . . ? O3 Zn1 N1 C25 95.5(2) . . . . ? N2 Zn1 N1 C25 -5.6(2) . . . . ? O1 Zn1 N1 C25 -109.0(2) 6_566 . . . ? O2 Zn1 N1 C25 -167.8(2) 6_566 . . . ? C8 Zn1 N1 C25 -138.4(2) 6_566 . . . ? O6 Zn1 O3 C1 -71.7(3) . . . . ? N2 Zn1 O3 C1 -166.5(3) . . . . ? O1 Zn1 O3 C1 37.4(4) 6_566 . . . ? O2 Zn1 O3 C1 33.2(3) 6_566 . . . ? N1 Zn1 O3 C1 119.8(3) . . . . ? C8 Zn1 O3 C1 36.1(3) 6_566 . . . ? C13 O7 C16 C21 10.8(6) . . . . ? C13 O7 C16 C17 -171.8(3) . . . . ? C11 C10 C15 C14 1.4(5) . . . . ? C9 C10 C15 C14 -178.3(3) . . . . ? C29 N1 C25 C26 4.4(5) . . . . ? Zn1 N1 C25 C26 -172.2(3) . . . . ? C29 N1 C25 C24 -174.5(3) . . . . ? Zn1 N1 C25 C24 8.9(3) . . . . ? Zn2 O5 C9 O6 -0.3(6) . . . . ? Zn2 O5 C9 C10 -179.7(2) . . . . ? C15 C10 C9 O5 166.8(3) . . . . ? C11 C10 C9 O5 -12.9(5) . . . . ? C15 C10 C9 O6 -12.6(4) . . . . ? C11 C10 C9 O6 167.6(3) . . . . ? O5 C9 O6 Zn1 7.9(5) . . . . ? C10 C9 O6 Zn1 -172.6(2) . . . . ? O3 Zn1 O6 C9 63.9(3) . . . . ? N2 Zn1 O6 C9 165.6(3) . . . . ? O1 Zn1 O6 C9 -92.8(3) 6_566 . . . ? O2 Zn1 O6 C9 -34.0(3) 6_566 . . . ? C8 Zn1 O6 C9 -64.2(3) 6_566 . . . ? O6 Zn1 N2 C24 177.5(2) . . . . ? O3 Zn1 N2 C24 -88.5(2) . . . . ? O1 Zn1 N2 C24 81.6(2) 6_566 . . . ? O2 Zn1 N2 C24 43.6(4) 6_566 . . . ? N1 Zn1 N2 C24 0.8(2) . . . . ? C8 Zn1 N2 C24 68.4(3) 6_566 . . . ? O6 Zn1 N2 C22 7.9(3) . . . . ? O3 Zn1 N2 C22 102.0(3) . . . . ? O1 Zn1 N2 C22 -88.0(3) 6_566 . . . ? O2 Zn1 N2 C22 -126.0(3) 6_566 . . . ? N1 Zn1 N2 C22 -168.7(3) . . . . ? C8 Zn1 N2 C22 -101.2(3) 6_566 . . . ? C5 C6 C7 C2 -0.2(5) . . . . ? C3 C2 C7 C6 -0.4(5) . . . . ? C1 C2 C7 C6 178.6(3) . . . . ? C22 N2 C24 N3 0.1(4) . . . . ? Zn1 N2 C24 N3 -171.9(2) . . . . ? C22 N2 C24 C25 176.0(3) . . . . ? Zn1 N2 C24 C25 4.0(4) . . . . ? C23 N3 C24 N2 0.4(4) . . . . ? C30 N3 C24 N2 174.6(3) . . . . ? C23 N3 C24 C25 -174.9(3) . . . . ? C30 N3 C24 C25 -0.7(6) . . . . ? N1 C25 C24 N2 -8.8(4) . . . . ? C26 C25 C24 N2 172.3(4) . . . . ? N1 C25 C24 N3 166.1(3) . . . . ? C26 C25 C24 N3 -12.8(6) . . . . ? C7 C6 C5 O8 177.5(3) . . . . ? C7 C6 C5 C4 0.9(5) . . . . ? C5 O8 C5 C6 148.0(3) 2_655 . . . ? C5 O8 C5 C4 -35.6(2) 2_655 . . . ? C31 C33 C32 C31 0.4(6) 5_766 . . . ? C10 C15 C14 C13 -0.7(5) . . . . ? C25 N1 C29 C28 -2.3(6) . . . . ? Zn1 N1 C29 C28 173.8(4) . . . . ? C20 C19 C18 C17 -0.3(5) . . . . ? C8 C19 C18 C17 -179.0(3) . . . . ? C24 N3 C23 C22 -0.8(4) . . . . ? C30 N3 C23 C22 -175.0(4) . . . . ? C15 C14 C13 C12 -0.8(5) . . . . ? C15 C14 C13 O7 174.4(3) . . . . ? C16 O7 C13 C12 -105.4(4) . . . . ? C16 O7 C13 C14 79.3(4) . . . . ? O7 C16 C21 C20 176.8(4) . . . . ? C17 C16 C21 C20 -0.4(6) . . . . ? C15 C10 C11 C12 -0.6(5) . . . . ? C9 C10 C11 C12 179.1(3) . . . . ? C7 C2 C3 C4 0.2(5) . . . . ? C1 C2 C3 C4 -178.8(3) . . . . ? C16 C21 C20 C19 -0.3(6) . . . . ? C18 C19 C20 C21 0.6(6) . . . . ? C8 C19 C20 C21 179.3(3) . . . . ? C2 C3 C4 C5 0.5(5) . . . . ? C6 C5 C4 C3 -1.1(5) . . . . ? O8 C5 C4 C3 -177.4(3) . . . . ? N1 C25 C26 C27 -2.4(7) . . . . ? C24 C25 C26 C27 176.3(4) . . . . ? C14 C13 C12 C11 1.6(5) . . . . ? O7 C13 C12 C11 -173.7(3) . . . . ? C10 C11 C12 C13 -0.8(5) . . . . ? C19 C18 C17 C16 -0.4(5) . . . . ? C21 C16 C17 C18 0.7(6) . . . . ? O7 C16 C17 C18 -176.7(3) . . . . ? Zn2 O4 C1 O3 33.2(5) . . . . ? Zn2 O4 C1 C2 -147.8(2) . . . . ? Zn1 O3 C1 O4 -21.0(5) . . . . ? Zn1 O3 C1 C2 160.1(2) . . . . ? C7 C2 C1 O4 -22.3(4) . . . . ? C3 C2 C1 O4 156.6(3) . . . . ? C7 C2 C1 O3 156.8(3) . . . . ? C3 C2 C1 O3 -24.3(4) . . . . ? C24 N3 C30 C31 175.5(3) . . . . ? C23 N3 C30 C31 -11.5(6) . . . . ? C33 C32 C31 C33 -0.4(6) . . . 5_766 ? C33 C32 C31 C30 174.3(3) . . . . ? N3 C30 C31 C32 81.9(5) . . . . ? N3 C30 C31 C33 -103.4(4) . . . 5_766 ? N3 C23 C22 N2 0.9(4) . . . . ? C24 N2 C22 C23 -0.6(4) . . . . ? Zn1 N2 C22 C23 169.9(3) . . . . ? N1 C29 C28 C27 -1.7(8) . . . . ? C25 C26 C27 C28 -1.7(8) . . . . ? C29 C28 C27 C26 3.7(9) . . . . ? C20 C19 C8 O1 -3.4(5) . . . . ? C18 C19 C8 O1 175.3(3) . . . . ? C20 C19 C8 O2 179.3(3) . . . . ? C18 C19 C8 O2 -2.0(5) . . . . ? O1 C8 O2 Zn2 100.9(3) . . . 4 ? C19 C8 O2 Zn2 -81.9(4) . . . 4 ? Zn1 C8 O2 Zn2 105.5(2) 6_565 . . 4 ? O1 C8 O2 Zn1 -4.6(3) . . . 6_565 ? C19 C8 O2 Zn1 172.7(3) . . . 6_565 ? O2 C8 O1 Zn1 5.0(3) . . . 6_565 ? C19 C8 O1 Zn1 -172.3(2) . . . 6_565 ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.517 _refine_diff_density_min -0.630 _refine_diff_density_rms 0.081 data_6 _database_code_depnum_ccdc_archive 'CCDC 687553' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C76 H56 Cd2 N12 O10' _chemical_formula_weight 1522.13 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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.6950(11) _cell_length_b 12.4600(13) _cell_length_c 15.1400(16) _cell_angle_alpha 111.061(2) _cell_angle_beta 96.603(2) _cell_angle_gamma 101.133(2) _cell_volume 1640.3(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.83 _cell_measurement_theta_max 28.63 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.541 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 772 _exptl_absorpt_coefficient_mu 0.721 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.777 _exptl_absorpt_correction_T_max 0.794 _exptl_absorpt_process_details 'SADABS(Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10241 _diffrn_reflns_av_R_equivalents 0.0436 _diffrn_reflns_av_sigmaI/netI 0.1133 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 28.63 _reflns_number_total 7502 _reflns_number_gt 4367 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SMART (Bruker, 1997)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97(Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0589P)^2^+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 7502 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1178 _refine_ls_R_factor_gt 0.0606 _refine_ls_wR_factor_ref 0.1473 _refine_ls_wR_factor_gt 0.1214 _refine_ls_goodness_of_fit_ref 0.957 _refine_ls_restrained_S_all 0.957 _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 0.53968(4) 0.14232(3) 0.48075(3) 0.04523(15) Uani 1 1 d . . . O4 O 0.5745(4) 0.0717(3) -0.4023(2) 0.0523(9) Uani 1 1 d . . . O1 O 0.7169(4) 0.0980(4) 0.3861(3) 0.0662(11) Uani 1 1 d . . . O2 O 0.5678(5) 0.1924(4) 0.3477(3) 0.0684(11) Uani 1 1 d . . . N3 N 0.1682(5) 0.2795(4) 0.5611(3) 0.0530(11) Uani 1 1 d . . . O5 O 0.7756(4) 0.2077(3) -0.3778(3) 0.0554(9) Uani 1 1 d . . . O3 O 0.8984(4) 0.1016(4) -0.0012(3) 0.0809(14) Uani 1 1 d . . . C13 C 0.6677(6) 0.1435(5) 0.3321(4) 0.0496(13) Uani 1 1 d . . . N2 N 0.3109(5) 0.1688(4) 0.4941(4) 0.0555(12) Uani 1 1 d . . . N1 N 0.5532(4) 0.3478(4) 0.5667(3) 0.0441(10) Uani 1 1 d . . . C10 C 0.0538(5) 0.4410(4) 0.5537(4) 0.0470(13) Uani 1 1 d . . . C14 C 0.7280(6) 0.1371(4) 0.2436(4) 0.0466(12) Uani 1 1 d . . . C9 C 0.1064(6) 0.3771(5) 0.6145(4) 0.0532(14) Uani 1 1 d . . . H9A H 0.1785 0.4343 0.6697 0.064 Uiso 1 1 calc R . . H9B H 0.0268 0.3452 0.6387 0.064 Uiso 1 1 calc R . . C4 C 0.4303(5) 0.3814(4) 0.5776(4) 0.0423(12) Uani 1 1 d . . . N4 N 0.2649(7) 0.4191(5) 0.1434(4) 0.0796(16) Uani 1 1 d . . . C15 C 0.6718(6) 0.1798(5) 0.1788(4) 0.0503(13) Uani 1 1 d . . . H15 H 0.5970 0.2161 0.1915 0.060 Uiso 1 1 calc R . . C16 C 0.7236(6) 0.1700(5) 0.0956(4) 0.0562(14) Uani 1 1 d . . . H16 H 0.6851 0.2000 0.0531 0.067 Uiso 1 1 calc R . . C3 C 0.3034(5) 0.2801(4) 0.5464(4) 0.0450(12) Uani 1 1 d . . . C26 C 0.9362(6) 0.1635(5) -0.1261(4) 0.0610(15) Uani 1 1 d . . . H26 H 1.0327 0.1915 -0.0962 0.073 Uiso 1 1 calc R . . C5 C 0.4287(6) 0.5011(5) 0.6134(4) 0.0519(14) Uani 1 1 d . . . H5 H 0.3425 0.5228 0.6185 0.062 Uiso 1 1 calc R . . C7 C 0.6827(6) 0.5524(5) 0.6306(4) 0.0584(15) Uani 1 1 d . . . H7 H 0.7703 0.6086 0.6488 0.070 Uiso 1 1 calc R . . C24 C 0.6993(6) 0.1371(5) -0.3520(4) 0.0461(13) Uani 1 1 d . . . C20 C 0.8373(7) 0.1121(5) -0.0848(4) 0.0582(15) Uani 1 1 d . . . C12 C -0.0638(5) 0.4396(5) 0.4051(4) 0.0513(13) Uani 1 1 d . . . H12 H -0.1066 0.3978 0.3402 0.062 Uiso 1 1 calc R . . C17 C 0.8325(6) 0.1153(5) 0.0770(4) 0.0565(15) Uani 1 1 d . . . C18 C 0.8928(6) 0.0736(5) 0.1417(4) 0.0626(16) Uani 1 1 d . . . H18 H 0.9681 0.0378 0.1290 0.075 Uiso 1 1 calc R . . C23 C 0.7484(6) 0.1266(4) -0.2587(4) 0.0462(12) Uani 1 1 d . . . C6 C 0.5559(6) 0.5865(5) 0.6409(4) 0.0550(14) Uani 1 1 d . . . H6 H 0.5569 0.6667 0.6662 0.066 Uiso 1 1 calc R . . C30 C 0.5099(7) 0.5470(6) 0.1571(4) 0.0640(16) Uani 1 1 d . . . C29 C 0.4061(7) 0.4351(6) 0.1325(5) 0.0707(18) Uani 1 1 d . . . C11 C -0.0125(6) 0.3796(5) 0.4565(4) 0.0508(13) Uani 1 1 d . . . H11 H -0.0219 0.2983 0.4267 0.061 Uiso 1 1 calc R . . C19 C 0.8411(6) 0.0850(5) 0.2244(4) 0.0555(14) Uani 1 1 d . . . H19 H 0.8824 0.0576 0.2679 0.067 Uiso 1 1 calc R . . N6 N 0.4881(7) 0.6485(6) 0.2174(4) 0.0811(16) Uani 1 1 d . . . C25 C 0.8904(6) 0.1730(5) -0.2124(4) 0.0590(15) Uani 1 1 d . . . H25 H 0.9554 0.2107 -0.2392 0.071 Uiso 1 1 calc R . . C1 C 0.1762(7) 0.0980(5) 0.4778(5) 0.0719(18) Uani 1 1 d . . . H1 H 0.1502 0.0159 0.4445 0.086 Uiso 1 1 calc R . . C35 C 0.1775(8) 0.5065(7) 0.1709(5) 0.082(2) Uani 1 1 d . . . H35A H 0.2403 0.5856 0.2058 0.098 Uiso 1 1 calc R . . H35B H 0.1174 0.4888 0.2134 0.098 Uiso 1 1 calc R . . C21 C 0.6973(7) 0.0663(6) -0.1290(4) 0.0709(18) Uani 1 1 d . . . H21 H 0.6321 0.0310 -0.1008 0.085 Uiso 1 1 calc R . . C2 C 0.0868(6) 0.1631(5) 0.5165(6) 0.0734(19) Uani 1 1 d . . . H2 H -0.0105 0.1356 0.5139 0.088 Uiso 1 1 calc R . . C22 C 0.6528(7) 0.0729(5) -0.2163(4) 0.0627(16) Uani 1 1 d . . . H22 H 0.5570 0.0407 -0.2474 0.075 Uiso 1 1 calc R . . C37 C 0.1400(7) 0.5687(6) 0.0322(5) 0.0766(19) Uani 1 1 d . . . H37 H 0.2339 0.6154 0.0528 0.092 Uiso 1 1 calc R . . C36 C 0.0851(7) 0.5037(6) 0.0837(5) 0.0659(16) Uani 1 1 d . . . C38 C 0.0542(8) 0.5639(7) -0.0501(5) 0.082(2) Uani 1 1 d . . . H38 H 0.0926 0.6082 -0.0836 0.098 Uiso 1 1 calc R . . C8 C 0.6748(6) 0.4314(5) 0.5921(4) 0.0540(14) Uani 1 1 d . . . H8 H 0.7594 0.4079 0.5837 0.065 Uiso 1 1 calc R . . C32 C 0.5895(9) 0.7474(7) 0.2404(6) 0.089(2) Uani 1 1 d . . . H32 H 0.5762 0.8176 0.2840 0.107 Uiso 1 1 calc R . . N5 N 0.4373(7) 0.3309(6) 0.0979(5) 0.103(2) Uani 1 1 d . . . C31 C 0.6308(9) 0.5445(8) 0.1218(7) 0.113(3) Uani 1 1 d . . . H31 H 0.6445 0.4725 0.0815 0.135 Uiso 1 1 calc R . . C28 C 0.2111(10) 0.2999(8) 0.1120(6) 0.105(3) Uani 1 1 d . . . H28 H 0.1171 0.2618 0.1089 0.126 Uiso 1 1 calc R . . C27 C 0.3148(11) 0.2466(8) 0.0863(7) 0.116(3) Uani 1 1 d . . . H27 H 0.3059 0.1652 0.0641 0.139 Uiso 1 1 calc R . . C34 C 0.7341(11) 0.6483(9) 0.1452(8) 0.135(4) Uani 1 1 d . . . H34 H 0.8181 0.6472 0.1212 0.162 Uiso 1 1 calc R . . C33 C 0.7118(9) 0.7533(7) 0.2044(7) 0.100(3) Uani 1 1 d . . . H33 H 0.7774 0.8255 0.2194 0.120 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 0.0500(3) 0.0521(3) 0.0492(2) 0.02761(19) 0.02299(17) 0.02495(18) O4 0.060(2) 0.051(2) 0.044(2) 0.0174(18) 0.0051(18) 0.0166(19) O1 0.071(3) 0.089(3) 0.058(2) 0.041(2) 0.029(2) 0.029(2) O2 0.079(3) 0.077(3) 0.076(3) 0.040(2) 0.047(2) 0.039(2) N3 0.048(3) 0.051(3) 0.075(3) 0.031(3) 0.028(2) 0.023(2) O5 0.058(2) 0.067(3) 0.053(2) 0.035(2) 0.0152(19) 0.0175(19) O3 0.068(3) 0.158(4) 0.057(3) 0.065(3) 0.037(2) 0.060(3) C13 0.053(3) 0.048(3) 0.045(3) 0.016(3) 0.015(3) 0.006(3) N2 0.049(3) 0.044(3) 0.080(3) 0.026(3) 0.021(2) 0.019(2) N1 0.038(2) 0.051(3) 0.050(3) 0.023(2) 0.016(2) 0.017(2) C10 0.033(3) 0.041(3) 0.071(4) 0.020(3) 0.024(3) 0.015(2) C14 0.054(3) 0.044(3) 0.043(3) 0.017(3) 0.017(2) 0.009(2) C9 0.045(3) 0.054(3) 0.072(4) 0.027(3) 0.030(3) 0.023(3) C4 0.042(3) 0.048(3) 0.046(3) 0.022(3) 0.013(2) 0.020(2) N4 0.081(4) 0.079(4) 0.082(4) 0.042(3) 0.000(3) 0.016(3) C15 0.052(3) 0.056(4) 0.049(3) 0.025(3) 0.014(3) 0.017(3) C16 0.059(4) 0.076(4) 0.047(3) 0.036(3) 0.010(3) 0.023(3) C3 0.039(3) 0.047(3) 0.060(3) 0.028(3) 0.019(2) 0.017(2) C26 0.044(3) 0.093(5) 0.058(4) 0.038(3) 0.018(3) 0.022(3) C5 0.042(3) 0.061(4) 0.063(4) 0.030(3) 0.016(3) 0.022(3) C7 0.052(4) 0.057(4) 0.063(4) 0.026(3) 0.008(3) 0.005(3) C24 0.054(4) 0.053(3) 0.036(3) 0.015(3) 0.014(3) 0.026(3) C20 0.062(4) 0.089(5) 0.044(3) 0.038(3) 0.021(3) 0.036(3) C12 0.041(3) 0.049(3) 0.059(3) 0.014(3) 0.010(3) 0.016(3) C17 0.051(3) 0.090(4) 0.042(3) 0.033(3) 0.019(3) 0.028(3) C18 0.069(4) 0.096(5) 0.050(3) 0.041(3) 0.030(3) 0.048(3) C23 0.045(3) 0.054(3) 0.047(3) 0.022(3) 0.016(2) 0.018(3) C6 0.054(4) 0.054(4) 0.062(4) 0.025(3) 0.017(3) 0.018(3) C30 0.067(4) 0.071(5) 0.058(4) 0.023(3) 0.014(3) 0.031(4) C29 0.061(4) 0.077(5) 0.082(5) 0.042(4) 0.004(4) 0.021(4) C11 0.044(3) 0.037(3) 0.068(4) 0.016(3) 0.013(3) 0.012(2) C19 0.071(4) 0.062(4) 0.046(3) 0.028(3) 0.018(3) 0.028(3) N6 0.089(4) 0.077(4) 0.089(4) 0.035(4) 0.040(3) 0.030(4) C25 0.052(4) 0.086(4) 0.059(4) 0.045(3) 0.023(3) 0.023(3) C1 0.056(4) 0.045(4) 0.113(5) 0.022(4) 0.037(4) 0.014(3) C35 0.084(5) 0.106(6) 0.073(5) 0.045(4) 0.021(4) 0.039(4) C21 0.068(5) 0.094(5) 0.058(4) 0.042(4) 0.018(3) 0.013(4) C2 0.041(3) 0.059(4) 0.133(6) 0.043(4) 0.041(4) 0.018(3) C22 0.061(4) 0.074(4) 0.047(3) 0.024(3) 0.012(3) 0.002(3) C37 0.060(4) 0.091(5) 0.083(5) 0.039(4) 0.012(4) 0.020(4) C36 0.065(4) 0.067(4) 0.069(4) 0.025(4) 0.012(3) 0.027(3) C38 0.075(5) 0.106(6) 0.078(5) 0.051(4) 0.019(4) 0.025(4) C8 0.040(3) 0.070(4) 0.062(4) 0.029(3) 0.018(3) 0.023(3) C32 0.101(6) 0.074(5) 0.102(6) 0.034(5) 0.042(5) 0.038(5) N5 0.098(5) 0.068(4) 0.139(6) 0.039(4) -0.005(4) 0.033(4) C31 0.084(6) 0.086(6) 0.152(8) 0.017(6) 0.057(6) 0.023(5) C28 0.105(7) 0.086(6) 0.120(7) 0.056(6) -0.022(5) 0.006(5) C27 0.107(7) 0.066(6) 0.159(9) 0.043(6) -0.028(6) 0.018(5) C34 0.101(7) 0.101(7) 0.189(11) 0.025(7) 0.071(7) 0.031(6) C33 0.092(6) 0.076(6) 0.133(7) 0.035(5) 0.048(5) 0.019(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 O4 2.263(3) 1_556 ? Cd1 N2 2.326(4) . ? Cd1 O2 2.342(4) . ? Cd1 O1 2.382(4) . ? Cd1 N1 2.388(4) . ? Cd1 O4 2.455(4) 2_655 ? Cd1 C13 2.695(5) . ? O4 C24 1.292(6) . ? O4 Cd1 2.263(3) 1_554 ? O4 Cd1 2.455(4) 2_655 ? O1 C13 1.250(6) . ? O2 C13 1.241(6) . ? N3 C3 1.353(6) . ? N3 C2 1.383(7) . ? N3 C9 1.475(6) . ? O5 C24 1.240(6) . ? O3 C17 1.382(6) . ? O3 C20 1.396(6) . ? C13 C14 1.505(7) . ? N2 C3 1.348(6) . ? N2 C1 1.367(7) . ? N1 C8 1.325(6) . ? N1 C4 1.346(6) . ? C10 C12 1.370(7) 2_566 ? C10 C11 1.395(7) . ? C10 C9 1.522(7) . ? C14 C15 1.380(7) . ? C14 C19 1.387(7) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C4 C5 1.396(7) . ? C4 C3 1.473(7) . ? N4 C28 1.356(8) . ? N4 C29 1.382(8) . ? N4 C35 1.480(8) . ? C15 C16 1.384(7) . ? C15 H15 0.9300 . ? C16 C17 1.366(7) . ? C16 H16 0.9300 . ? C26 C20 1.381(7) . ? C26 C25 1.384(7) . ? C26 H26 0.9300 . ? C5 C6 1.372(7) . ? C5 H5 0.9300 . ? C7 C6 1.383(7) . ? C7 C8 1.390(7) . ? C7 H7 0.9300 . ? C24 C23 1.498(7) . ? C20 C21 1.354(8) . ? C12 C10 1.370(7) 2_566 ? C12 C11 1.374(7) . ? C12 H12 0.9300 . ? C17 C18 1.386(7) . ? C18 C19 1.372(7) . ? C18 H18 0.9300 . ? C23 C25 1.378(7) . ? C23 C22 1.386(7) . ? C6 H6 0.9300 . ? C30 N6 1.339(8) . ? C30 C31 1.345(9) . ? C30 C29 1.446(9) . ? C29 N5 1.324(8) . ? C11 H11 0.9300 . ? C19 H19 0.9300 . ? N6 C32 1.323(9) . ? C25 H25 0.9300 . ? C1 C2 1.342(8) . ? C1 H1 0.9300 . ? C35 C36 1.493(8) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C21 C22 1.379(8) . ? C21 H21 0.9300 . ? C2 H2 0.9300 . ? C22 H22 0.9300 . ? C37 C36 1.388(9) . ? C37 C38 1.392(9) . ? C37 H37 0.9300 . ? C36 C38 1.374(9) 2_565 ? C38 C36 1.374(9) 2_565 ? C38 H38 0.9300 . ? C8 H8 0.9300 . ? C32 C33 1.361(10) . ? C32 H32 0.9300 . ? N5 C27 1.372(10) . ? C31 C34 1.376(11) . ? C31 H31 0.9300 . ? C28 C27 1.329(12) . ? C28 H28 0.9300 . ? C27 H27 0.9300 . ? C34 C33 1.368(11) . ? C34 H34 0.9300 . ? C33 H33 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 O4 Cd1 N2 98.53(15) 1_556 . ? O4 Cd1 O2 161.63(14) 1_556 . ? N2 Cd1 O2 99.33(15) . . ? O4 Cd1 O1 106.62(13) 1_556 . ? N2 Cd1 O1 150.56(16) . . ? O2 Cd1 O1 55.02(13) . . ? O4 Cd1 N1 104.40(13) 1_556 . ? N2 Cd1 N1 70.05(15) . . ? O2 Cd1 N1 85.77(14) . . ? O1 Cd1 N1 116.60(14) . . ? O4 Cd1 O4 74.89(14) 1_556 2_655 ? N2 Cd1 O4 86.78(14) . 2_655 ? O2 Cd1 O4 101.86(13) . 2_655 ? O1 Cd1 O4 85.27(13) . 2_655 ? N1 Cd1 O4 156.58(13) . 2_655 ? O4 Cd1 C13 134.25(16) 1_556 . ? N2 Cd1 C13 125.20(17) . . ? O2 Cd1 C13 27.41(14) . . ? O1 Cd1 C13 27.64(14) . . ? N1 Cd1 C13 102.84(15) . . ? O4 Cd1 C13 93.16(14) 2_655 . ? C24 O4 Cd1 102.6(3) . 1_554 ? C24 O4 Cd1 136.0(3) . 2_655 ? Cd1 O4 Cd1 105.11(14) 1_554 2_655 ? C13 O1 Cd1 90.2(3) . . ? C13 O2 Cd1 92.3(3) . . ? C3 N3 C2 107.4(4) . . ? C3 N3 C9 130.8(5) . . ? C2 N3 C9 121.8(4) . . ? C17 O3 C20 123.1(4) . . ? O2 C13 O1 122.3(5) . . ? O2 C13 C14 118.1(5) . . ? O1 C13 C14 119.6(5) . . ? O2 C13 Cd1 60.3(3) . . ? O1 C13 Cd1 62.1(3) . . ? C14 C13 Cd1 175.3(4) . . ? C3 N2 C1 105.6(4) . . ? C3 N2 Cd1 116.3(3) . . ? C1 N2 Cd1 136.9(4) . . ? C8 N1 C4 118.4(4) . . ? C8 N1 Cd1 122.3(3) . . ? C4 N1 Cd1 118.6(3) . . ? C12 C10 C11 118.1(5) 2_566 . ? C12 C10 C9 120.3(5) 2_566 . ? C11 C10 C9 121.5(5) . . ? C15 C14 C19 118.2(5) . . ? C15 C14 C13 121.8(5) . . ? C19 C14 C13 120.0(5) . . ? N3 C9 C10 113.5(4) . . ? N3 C9 H9A 108.9 . . ? C10 C9 H9A 108.9 . . ? N3 C9 H9B 108.9 . . ? C10 C9 H9B 108.9 . . ? H9A C9 H9B 107.7 . . ? N1 C4 C5 121.5(5) . . ? N1 C4 C3 112.9(4) . . ? C5 C4 C3 125.5(4) . . ? C28 N4 C29 105.8(6) . . ? C28 N4 C35 123.9(7) . . ? C29 N4 C35 129.9(6) . . ? C14 C15 C16 121.9(5) . . ? C14 C15 H15 119.0 . . ? C16 C15 H15 119.0 . . ? C17 C16 C15 118.6(5) . . ? C17 C16 H16 120.7 . . ? C15 C16 H16 120.7 . . ? N2 C3 N3 110.1(4) . . ? N2 C3 C4 120.9(4) . . ? N3 C3 C4 129.0(5) . . ? C20 C26 C25 119.4(5) . . ? C20 C26 H26 120.3 . . ? C25 C26 H26 120.3 . . ? C6 C5 C4 119.2(5) . . ? C6 C5 H5 120.4 . . ? C4 C5 H5 120.4 . . ? C6 C7 C8 117.8(5) . . ? C6 C7 H7 121.1 . . ? C8 C7 H7 121.1 . . ? O5 C24 O4 122.3(5) . . ? O5 C24 C23 120.5(5) . . ? O4 C24 C23 117.2(5) . . ? C21 C20 C26 121.4(5) . . ? C21 C20 O3 124.6(5) . . ? C26 C20 O3 113.7(5) . . ? C10 C12 C11 122.1(5) 2_566 . ? C10 C12 H12 118.9 2_566 . ? C11 C12 H12 118.9 . . ? C16 C17 O3 125.6(5) . . ? C16 C17 C18 120.7(5) . . ? O3 C17 C18 113.6(5) . . ? C19 C18 C17 119.9(5) . . ? C19 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? C25 C23 C22 118.9(5) . . ? C25 C23 C24 119.9(5) . . ? C22 C23 C24 121.2(5) . . ? C5 C6 C7 119.5(5) . . ? C5 C6 H6 120.3 . . ? C7 C6 H6 120.3 . . ? N6 C30 C31 121.7(7) . . ? N6 C30 C29 120.4(6) . . ? C31 C30 C29 117.9(6) . . ? N5 C29 N4 109.9(6) . . ? N5 C29 C30 123.1(7) . . ? N4 C29 C30 127.0(6) . . ? C12 C11 C10 119.8(5) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? C18 C19 C14 120.6(5) . . ? C18 C19 H19 119.7 . . ? C14 C19 H19 119.7 . . ? C32 N6 C30 117.6(6) . . ? C23 C25 C26 120.1(5) . . ? C23 C25 H25 120.0 . . ? C26 C25 H25 120.0 . . ? C2 C1 N2 110.7(5) . . ? C2 C1 H1 124.6 . . ? N2 C1 H1 124.6 . . ? N4 C35 C36 110.9(5) . . ? N4 C35 H35A 109.5 . . ? C36 C35 H35A 109.5 . . ? N4 C35 H35B 109.5 . . ? C36 C35 H35B 109.5 . . ? H35A C35 H35B 108.0 . . ? C20 C21 C22 119.0(6) . . ? C20 C21 H21 120.5 . . ? C22 C21 H21 120.5 . . ? C1 C2 N3 106.3(5) . . ? C1 C2 H2 126.9 . . ? N3 C2 H2 126.9 . . ? C21 C22 C23 121.1(6) . . ? C21 C22 H22 119.4 . . ? C23 C22 H22 119.4 . . ? C36 C37 C38 119.9(6) . . ? C36 C37 H37 120.0 . . ? C38 C37 H37 120.0 . . ? C38 C36 C37 117.7(6) 2_565 . ? C38 C36 C35 122.1(6) 2_565 . ? C37 C36 C35 120.2(6) . . ? C36 C38 C37 122.4(6) 2_565 . ? C36 C38 H38 118.8 2_565 . ? C37 C38 H38 118.8 . . ? N1 C8 C7 123.6(5) . . ? N1 C8 H8 118.2 . . ? C7 C8 H8 118.2 . . ? N6 C32 C33 124.3(7) . . ? N6 C32 H32 117.8 . . ? C33 C32 H32 117.8 . . ? C29 N5 C27 106.5(7) . . ? C30 C31 C34 120.0(8) . . ? C30 C31 H31 120.0 . . ? C34 C31 H31 120.0 . . ? C27 C28 N4 108.7(8) . . ? C27 C28 H28 125.6 . . ? N4 C28 H28 125.6 . . ? C28 C27 N5 109.1(8) . . ? C28 C27 H27 125.4 . . ? N5 C27 H27 125.4 . . ? C33 C34 C31 119.2(9) . . ? C33 C34 H34 120.4 . . ? C31 C34 H34 120.4 . . ? C32 C33 C34 117.1(8) . . ? C32 C33 H33 121.4 . . ? C34 C33 H33 121.4 . . ? 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 O4 Cd1 O1 C13 178.8(3) 1_556 . . . ? N2 Cd1 O1 C13 31.2(5) . . . . ? O2 Cd1 O1 C13 -1.9(3) . . . . ? N1 Cd1 O1 C13 -65.1(3) . . . . ? O4 Cd1 O1 C13 106.1(3) 2_655 . . . ? O4 Cd1 O2 C13 4.2(7) 1_556 . . . ? N2 Cd1 O2 C13 -162.2(3) . . . . ? O1 Cd1 O2 C13 2.0(3) . . . . ? N1 Cd1 O2 C13 128.8(4) . . . . ? O4 Cd1 O2 C13 -73.6(4) 2_655 . . . ? Cd1 O2 C13 O1 -3.6(6) . . . . ? Cd1 O2 C13 C14 174.9(4) . . . . ? Cd1 O1 C13 O2 3.5(6) . . . . ? Cd1 O1 C13 C14 -175.0(4) . . . . ? O4 Cd1 C13 O2 -178.2(3) 1_556 . . . ? N2 Cd1 C13 O2 21.6(4) . . . . ? O1 Cd1 C13 O2 -176.6(5) . . . . ? N1 Cd1 C13 O2 -52.9(4) . . . . ? O4 Cd1 C13 O2 109.9(3) 2_655 . . . ? O4 Cd1 C13 O1 -1.6(4) 1_556 . . . ? N2 Cd1 C13 O1 -161.8(3) . . . . ? O2 Cd1 C13 O1 176.6(5) . . . . ? N1 Cd1 C13 O1 123.7(3) . . . . ? O4 Cd1 C13 O1 -73.5(3) 2_655 . . . ? O4 Cd1 N2 C3 98.3(4) 1_556 . . . ? O2 Cd1 N2 C3 -86.0(4) . . . . ? O1 Cd1 N2 C3 -113.0(4) . . . . ? N1 Cd1 N2 C3 -4.0(3) . . . . ? O4 Cd1 N2 C3 172.5(4) 2_655 . . . ? C13 Cd1 N2 C3 -95.9(4) . . . . ? O4 Cd1 N2 C1 -66.6(6) 1_556 . . . ? O2 Cd1 N2 C1 109.1(6) . . . . ? O1 Cd1 N2 C1 82.0(7) . . . . ? N1 Cd1 N2 C1 -168.9(6) . . . . ? O4 Cd1 N2 C1 7.6(6) 2_655 . . . ? C13 Cd1 N2 C1 99.2(6) . . . . ? O4 Cd1 N1 C8 92.4(4) 1_556 . . . ? N2 Cd1 N1 C8 -173.6(4) . . . . ? O2 Cd1 N1 C8 -72.0(4) . . . . ? O1 Cd1 N1 C8 -24.9(4) . . . . ? O4 Cd1 N1 C8 177.6(3) 2_655 . . . ? C13 Cd1 N1 C8 -50.4(4) . . . . ? O4 Cd1 N1 C4 -97.2(3) 1_556 . . . ? N2 Cd1 N1 C4 -3.2(3) . . . . ? O2 Cd1 N1 C4 98.3(3) . . . . ? O1 Cd1 N1 C4 145.5(3) . . . . ? O4 Cd1 N1 C4 -12.0(5) 2_655 . . . ? C13 Cd1 N1 C4 119.9(3) . . . . ? O2 C13 C14 C15 -2.4(8) . . . . ? O1 C13 C14 C15 176.2(5) . . . . ? O2 C13 C14 C19 178.9(5) . . . . ? O1 C13 C14 C19 -2.5(8) . . . . ? C3 N3 C9 C10 87.3(7) . . . . ? C2 N3 C9 C10 -94.2(6) . . . . ? C12 C10 C9 N3 -146.1(5) 2_566 . . . ? C11 C10 C9 N3 37.4(7) . . . . ? C8 N1 C4 C5 0.9(7) . . . . ? Cd1 N1 C4 C5 -169.8(4) . . . . ? C8 N1 C4 C3 179.8(4) . . . . ? Cd1 N1 C4 C3 9.1(5) . . . . ? C19 C14 C15 C16 1.1(8) . . . . ? C13 C14 C15 C16 -177.6(5) . . . . ? C14 C15 C16 C17 0.7(8) . . . . ? C1 N2 C3 N3 -1.0(6) . . . . ? Cd1 N2 C3 N3 -170.4(3) . . . . ? C1 N2 C3 C4 -179.9(5) . . . . ? Cd1 N2 C3 C4 10.7(6) . . . . ? C2 N3 C3 N2 0.2(6) . . . . ? C9 N3 C3 N2 178.9(5) . . . . ? C2 N3 C3 C4 179.0(5) . . . . ? C9 N3 C3 C4 -2.4(9) . . . . ? N1 C4 C3 N2 -13.2(7) . . . . ? C5 C4 C3 N2 165.6(5) . . . . ? N1 C4 C3 N3 168.2(5) . . . . ? C5 C4 C3 N3 -13.0(8) . . . . ? N1 C4 C5 C6 -2.1(8) . . . . ? C3 C4 C5 C6 179.2(5) . . . . ? Cd1 O4 C24 O5 -7.4(6) 1_554 . . . ? Cd1 O4 C24 O5 120.6(5) 2_655 . . . ? Cd1 O4 C24 C23 171.3(3) 1_554 . . . ? Cd1 O4 C24 C23 -60.7(6) 2_655 . . . ? C25 C26 C20 C21 2.7(9) . . . . ? C25 C26 C20 O3 176.4(5) . . . . ? C17 O3 C20 C21 -42.4(9) . . . . ? C17 O3 C20 C26 144.2(6) . . . . ? C15 C16 C17 O3 -178.0(5) . . . . ? C15 C16 C17 C18 -1.9(9) . . . . ? C20 O3 C17 C16 -18.4(10) . . . . ? C20 O3 C17 C18 165.2(5) . . . . ? C16 C17 C18 C19 1.2(9) . . . . ? O3 C17 C18 C19 177.8(5) . . . . ? O5 C24 C23 C25 -15.4(8) . . . . ? O4 C24 C23 C25 165.8(5) . . . . ? O5 C24 C23 C22 163.2(5) . . . . ? O4 C24 C23 C22 -15.5(7) . . . . ? C4 C5 C6 C7 1.5(8) . . . . ? C8 C7 C6 C5 0.1(8) . . . . ? C28 N4 C29 N5 -1.1(8) . . . . ? C35 N4 C29 N5 -173.9(6) . . . . ? C28 N4 C29 C30 -179.1(6) . . . . ? C35 N4 C29 C30 8.1(11) . . . . ? N6 C30 C29 N5 -159.8(7) . . . . ? C31 C30 C29 N5 16.9(10) . . . . ? N6 C30 C29 N4 18.0(10) . . . . ? C31 C30 C29 N4 -165.4(7) . . . . ? C10 C12 C11 C10 -0.8(8) 2_566 . . . ? C12 C10 C11 C12 0.8(8) 2_566 . . . ? C9 C10 C11 C12 177.4(5) . . . . ? C17 C18 C19 C14 0.6(9) . . . . ? C15 C14 C19 C18 -1.7(8) . . . . ? C13 C14 C19 C18 176.9(5) . . . . ? C31 C30 N6 C32 0.8(10) . . . . ? C29 C30 N6 C32 177.3(6) . . . . ? C22 C23 C25 C26 1.3(8) . . . . ? C24 C23 C25 C26 180.0(5) . . . . ? C20 C26 C25 C23 -2.9(9) . . . . ? C3 N2 C1 C2 1.5(8) . . . . ? Cd1 N2 C1 C2 167.5(5) . . . . ? C28 N4 C35 C36 -73.3(8) . . . . ? C29 N4 C35 C36 98.3(8) . . . . ? C26 C20 C21 C22 -0.9(10) . . . . ? O3 C20 C21 C22 -173.9(5) . . . . ? N2 C1 C2 N3 -1.4(8) . . . . ? C3 N3 C2 C1 0.7(7) . . . . ? C9 N3 C2 C1 -178.1(5) . . . . ? C20 C21 C22 C23 -0.8(10) . . . . ? C25 C23 C22 C21 0.6(9) . . . . ? C24 C23 C22 C21 -178.1(5) . . . . ? C38 C37 C36 C38 0.1(11) . . . 2_565 ? C38 C37 C36 C35 178.8(6) . . . . ? N4 C35 C36 C38 94.1(8) . . . 2_565 ? N4 C35 C36 C37 -84.5(8) . . . . ? C36 C37 C38 C36 -0.1(12) . . . 2_565 ? C4 N1 C8 C7 0.8(8) . . . . ? Cd1 N1 C8 C7 171.2(4) . . . . ? C6 C7 C8 N1 -1.3(8) . . . . ? C30 N6 C32 C33 2.3(11) . . . . ? N4 C29 N5 C27 0.0(8) . . . . ? C30 C29 N5 C27 178.1(7) . . . . ? N6 C30 C31 C34 -1.8(13) . . . . ? C29 C30 C31 C34 -178.4(8) . . . . ? C29 N4 C28 C27 1.9(9) . . . . ? C35 N4 C28 C27 175.2(7) . . . . ? N4 C28 C27 N5 -2.0(11) . . . . ? C29 N5 C27 C28 1.2(10) . . . . ? C30 C31 C34 C33 -0.1(16) . . . . ? N6 C32 C33 C34 -4.1(13) . . . . ? C31 C34 C33 C32 2.9(15) . . . . ? _diffrn_measured_fraction_theta_max 0.891 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.864 _refine_diff_density_min -0.841 _refine_diff_density_rms 0.097 data_7 _database_code_depnum_ccdc_archive 'CCDC 687554' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H30 Cd N6 O6' _chemical_formula_weight 779.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.4090(3) _cell_length_b 20.5790(4) _cell_length_c 14.6440(6) _cell_angle_alpha 90.00 _cell_angle_beta 114.6370(10) _cell_angle_gamma 90.00 _cell_volume 3399.14(17) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.98 _cell_measurement_theta_max 28.29 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.522 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1584 _exptl_absorpt_coefficient_mu 0.700 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.834 _exptl_absorpt_correction_T_max 0.845 _exptl_absorpt_process_details 'SADABS(Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20887 _diffrn_reflns_av_R_equivalents 0.0192 _diffrn_reflns_av_sigmaI/netI 0.0244 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 28.29 _reflns_number_total 8188 _reflns_number_gt 6541 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SMART (Bruker, 1997)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97(Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material SHELXL-97 _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^)+(0.0332P)^2^+1.0535P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8188 _refine_ls_number_parameters 466 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0438 _refine_ls_R_factor_gt 0.0308 _refine_ls_wR_factor_ref 0.0755 _refine_ls_wR_factor_gt 0.0695 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.003 _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 0.222551(13) 0.524275(7) 0.807168(11) 0.04145(6) Uani 1 1 d . . . O4 O 0.62178(15) 0.87457(7) 0.30295(13) 0.0563(4) Uani 1 1 d . . . O5 O 0.79566(15) 0.89301(7) 0.42832(13) 0.0588(4) Uani 1 1 d . . . N3 N 0.07025(17) 0.48643(9) 0.87909(14) 0.0489(4) Uani 1 1 d . . . O2 O 0.30221(15) 0.57864(9) 0.70968(12) 0.0627(4) Uani 1 1 d . . . N1 N 0.30501(16) 0.38816(8) 1.05562(13) 0.0453(4) Uani 1 1 d . . . O3 O 0.69752(18) 0.60827(8) 0.54240(17) 0.0805(6) Uani 1 1 d . . . O1 O 0.40642(15) 0.49015(9) 0.77096(13) 0.0630(5) Uani 1 1 d . . . N2 N 0.29899(15) 0.44688(8) 0.92788(13) 0.0437(4) Uani 1 1 d . . . C4 C 0.10598(18) 0.43178(10) 0.93340(15) 0.0419(4) Uani 1 1 d . . . C16 C 0.30633(19) 0.24818(10) 1.07040(15) 0.0450(5) Uani 1 1 d . . . H16 H 0.3321 0.2687 1.0265 0.054 Uiso 1 1 calc R . . C38 C 0.7063(2) 0.85756(10) 0.38229(18) 0.0483(5) Uani 1 1 d . . . C3 C 0.23473(18) 0.42170(9) 0.97176(15) 0.0397(4) Uani 1 1 d . . . C9 C 0.2739(2) 0.35887(11) 1.13239(17) 0.0512(5) Uani 1 1 d . . . H9A H 0.1984 0.3765 1.1256 0.061 Uiso 1 1 calc R . . H9B H 0.3330 0.3714 1.1981 0.061 Uiso 1 1 calc R . . C26 C 0.46384(19) 0.55792(10) 0.66763(15) 0.0434(5) Uani 1 1 d . . . C14 C 0.31026(19) 0.18095(10) 1.07679(16) 0.0472(5) Uani 1 1 d . . . C10 C 0.26509(18) 0.28551(10) 1.12770(16) 0.0445(5) Uani 1 1 d . . . C37 C 0.7036(2) 0.79165(10) 0.42559(17) 0.0471(5) Uani 1 1 d . . . C2 C 0.4191(2) 0.39266(11) 1.06266(18) 0.0525(5) Uani 1 1 d . . . H2 H 0.4867 0.3744 1.1122 0.063 Uiso 1 1 calc R . . C32 C 0.6969(2) 0.67015(12) 0.5027(2) 0.0613(7) Uani 1 1 d . . . C28 C 0.5378(2) 0.63950(11) 0.58932(19) 0.0550(6) Uani 1 1 d . . . H28 H 0.5363 0.6820 0.5670 0.066 Uiso 1 1 calc R . . C31 C 0.6157(2) 0.59480(11) 0.58111(19) 0.0532(6) Uani 1 1 d . . . O1W O 0.6109(3) 0.40835(17) 0.8540(2) 0.1117(10) Uani 1 1 d . . . C5 C 0.0278(2) 0.38980(12) 0.94848(18) 0.0560(6) Uani 1 1 d . . . H5 H 0.0541 0.3508 0.9826 0.067 Uiso 1 1 calc R . . C15 C 0.3659(2) 0.14386(11) 1.01875(16) 0.0523(5) Uani 1 1 d . . . H15A H 0.3041 0.1310 0.9546 0.063 Uiso 1 1 calc R . . H15B H 0.4196 0.1726 1.0053 0.063 Uiso 1 1 calc R . . C1 C 0.4137(2) 0.42847(10) 0.98417(18) 0.0501(5) Uani 1 1 d . . . H1 H 0.4782 0.4391 0.9702 0.060 Uiso 1 1 calc R . . C8 C -0.0447(2) 0.50133(13) 0.84294(19) 0.0599(6) Uani 1 1 d . . . H8 H -0.0704 0.5390 0.8048 0.072 Uiso 1 1 calc R . . C30 C 0.6181(2) 0.53195(11) 0.6143(2) 0.0604(6) Uani 1 1 d . . . H30 H 0.6699 0.5017 0.6074 0.073 Uiso 1 1 calc R . . C33 C 0.6000(2) 0.69247(13) 0.4219(2) 0.0692(7) Uani 1 1 d . . . H33 H 0.5326 0.6667 0.3927 0.083 Uiso 1 1 calc R . . C29 C 0.5427(2) 0.51416(11) 0.65801(19) 0.0550(6) Uani 1 1 d . . . H29 H 0.5454 0.4719 0.6813 0.066 Uiso 1 1 calc R . . C27 C 0.4615(2) 0.62019(11) 0.63134(17) 0.0505(5) Uani 1 1 d . . . H27 H 0.4072 0.6499 0.6353 0.061 Uiso 1 1 calc R . . C36 C 0.8017(2) 0.76719(12) 0.50556(19) 0.0587(6) Uani 1 1 d . . . H36 H 0.8706 0.7919 0.5335 0.070 Uiso 1 1 calc R . . C35 C 0.7982(3) 0.70595(12) 0.5445(2) 0.0641(7) Uani 1 1 d . . . H35 H 0.8640 0.6897 0.5984 0.077 Uiso 1 1 calc R . . C6 C -0.0908(2) 0.40743(15) 0.9114(2) 0.0668(7) Uani 1 1 d . . . H6 H -0.1452 0.3809 0.9222 0.080 Uiso 1 1 calc R . . C11 C 0.2238(2) 0.25438(12) 1.19134(18) 0.0553(6) Uani 1 1 d . . . H11 H 0.1957 0.2787 1.2304 0.066 Uiso 1 1 calc R . . C12 C 0.2244(2) 0.18762(13) 1.1965(2) 0.0648(7) Uani 1 1 d . . . H12 H 0.1954 0.1669 1.2381 0.078 Uiso 1 1 calc R . . C13 C 0.2681(2) 0.15110(12) 1.13984(19) 0.0593(6) Uani 1 1 d . . . H13 H 0.2690 0.1060 1.1443 0.071 Uiso 1 1 calc R . . C25 C 0.3855(2) 0.54056(12) 0.71931(16) 0.0493(5) Uani 1 1 d . . . C34 C 0.6032(2) 0.75367(12) 0.3838(2) 0.0589(6) Uani 1 1 d . . . H34 H 0.5370 0.7693 0.3296 0.071 Uiso 1 1 calc R . . C7 C -0.1269(2) 0.46429(14) 0.8588(2) 0.0655(7) Uani 1 1 d . . . H7 H -0.2056 0.4775 0.8344 0.079 Uiso 1 1 calc R . . N4 N 0.43157(17) 0.08554(8) 1.07043(13) 0.0490(4) Uani 1 1 d . . . C18 C 0.54379(19) 0.08211(10) 1.14353(15) 0.0441(5) Uani 1 1 d . . . C19 C 0.6219(2) 0.13795(10) 1.18993(16) 0.0466(5) Uani 1 1 d . . . C17 C 0.3886(2) 0.02320(11) 1.05035(18) 0.0547(6) Uani 1 1 d . . . H17 H 0.3139 0.0105 1.0039 0.066 Uiso 1 1 calc R . . N6 N 0.5690(2) 0.19379(11) 1.19318(19) 0.0798(7) Uani 1 1 d . . . N5 N 0.57322(17) 0.02032(8) 1.16939(14) 0.0474(4) Uani 1 1 d . . . C24 C 0.4759(2) -0.01577(11) 1.11111(18) 0.0544(6) Uani 1 1 d . . . H24 H 0.4710 -0.0608 1.1133 0.065 Uiso 1 1 calc R . . C20 C 0.7427(2) 0.13305(12) 1.2283(2) 0.0639(7) Uani 1 1 d . . . H20 H 0.7785 0.0947 1.2217 0.077 Uiso 1 1 calc R . . C23 C 0.8109(3) 0.18643(15) 1.2772(2) 0.0777(9) Uani 1 1 d . . . H23 H 0.8932 0.1837 1.3061 0.093 Uiso 1 1 calc R . . C22 C 0.7568(3) 0.24239(15) 1.2824(2) 0.0813(9) Uani 1 1 d . . . H22 H 0.8005 0.2784 1.3161 0.098 Uiso 1 1 calc R . . C21 C 0.6389(3) 0.24426(15) 1.2380(3) 0.0939(11) Uani 1 1 d . . . H21 H 0.6024 0.2837 1.2380 0.113 Uiso 1 1 calc R . . H1A H 0.560(4) 0.433(2) 0.833(3) 0.141 Uiso 1 1 d . . . H1B H 0.635(4) 0.406(2) 0.912(3) 0.141 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.04681(9) 0.03460(8) 0.04682(9) 0.00110(6) 0.02336(7) -0.00084(6) O4 0.0591(10) 0.0449(9) 0.0638(10) 0.0116(8) 0.0243(9) 0.0016(7) O5 0.0681(11) 0.0429(9) 0.0642(10) 0.0007(7) 0.0265(9) -0.0088(8) N3 0.0506(11) 0.0495(11) 0.0483(10) 0.0031(8) 0.0224(9) 0.0059(8) O2 0.0558(10) 0.0792(12) 0.0630(11) 0.0129(9) 0.0346(9) 0.0015(9) N1 0.0501(10) 0.0387(9) 0.0469(10) 0.0030(8) 0.0201(8) 0.0015(8) O3 0.0894(14) 0.0585(11) 0.1315(17) 0.0437(11) 0.0837(14) 0.0245(10) O1 0.0622(11) 0.0660(11) 0.0652(11) 0.0193(9) 0.0308(9) -0.0113(8) N2 0.0454(10) 0.0371(9) 0.0524(10) 0.0015(8) 0.0241(8) -0.0002(7) C4 0.0483(12) 0.0420(11) 0.0393(11) -0.0030(9) 0.0222(9) 0.0003(9) C16 0.0487(12) 0.0428(11) 0.0410(11) 0.0093(9) 0.0163(9) 0.0024(9) C38 0.0592(14) 0.0396(11) 0.0581(14) 0.0016(10) 0.0362(12) 0.0010(10) C3 0.0450(11) 0.0318(10) 0.0430(11) -0.0026(8) 0.0189(9) -0.0002(8) C9 0.0615(14) 0.0485(13) 0.0445(12) 0.0047(10) 0.0230(11) 0.0038(10) C26 0.0446(11) 0.0462(12) 0.0396(11) 0.0033(9) 0.0176(9) -0.0074(9) C14 0.0463(12) 0.0451(12) 0.0416(11) 0.0053(9) 0.0098(9) 0.0014(9) C10 0.0408(11) 0.0461(12) 0.0420(11) 0.0083(9) 0.0127(9) 0.0039(9) C37 0.0575(13) 0.0415(11) 0.0535(13) 0.0044(9) 0.0343(11) 0.0013(10) C2 0.0448(12) 0.0437(12) 0.0613(14) 0.0008(11) 0.0147(11) 0.0008(10) C32 0.0725(17) 0.0505(13) 0.0854(18) 0.0243(13) 0.0572(15) 0.0120(12) C28 0.0630(15) 0.0416(12) 0.0706(15) 0.0201(11) 0.0382(13) 0.0066(10) C31 0.0565(14) 0.0464(12) 0.0689(15) 0.0171(11) 0.0384(12) 0.0034(10) O1W 0.103(2) 0.167(3) 0.0839(17) 0.0481(18) 0.0578(16) 0.0638(17) C5 0.0539(14) 0.0585(14) 0.0604(14) 0.0038(11) 0.0285(12) -0.0053(11) C15 0.0633(14) 0.0439(12) 0.0411(12) 0.0047(9) 0.0133(11) 0.0071(10) C1 0.0456(12) 0.0408(11) 0.0654(14) -0.0015(10) 0.0246(11) -0.0035(9) C8 0.0566(15) 0.0675(15) 0.0574(15) 0.0069(12) 0.0254(12) 0.0150(13) C30 0.0759(17) 0.0454(13) 0.0781(17) 0.0175(11) 0.0501(15) 0.0118(12) C33 0.0613(16) 0.0618(16) 0.090(2) 0.0183(14) 0.0368(15) -0.0128(13) C29 0.0726(16) 0.0397(12) 0.0626(15) 0.0111(10) 0.0380(13) -0.0025(11) C27 0.0510(13) 0.0495(12) 0.0579(14) 0.0118(10) 0.0295(11) 0.0082(10) C36 0.0610(15) 0.0511(14) 0.0643(15) 0.0060(12) 0.0263(12) -0.0008(11) C35 0.0700(17) 0.0592(15) 0.0684(17) 0.0199(12) 0.0340(14) 0.0143(13) C6 0.0521(15) 0.089(2) 0.0656(16) -0.0040(14) 0.0312(13) -0.0147(14) C11 0.0520(13) 0.0586(14) 0.0616(15) 0.0088(11) 0.0298(12) 0.0051(11) C12 0.0688(17) 0.0620(16) 0.0736(17) 0.0156(13) 0.0395(14) -0.0038(13) C13 0.0656(16) 0.0435(12) 0.0674(16) 0.0122(11) 0.0265(13) -0.0024(11) C25 0.0478(13) 0.0600(14) 0.0377(11) 0.0015(10) 0.0153(10) -0.0158(11) C34 0.0553(14) 0.0575(14) 0.0669(15) 0.0188(12) 0.0286(12) -0.0022(11) C7 0.0460(13) 0.096(2) 0.0554(15) -0.0025(14) 0.0220(12) 0.0115(13) N4 0.0597(11) 0.0393(9) 0.0419(10) 0.0003(8) 0.0151(9) 0.0043(8) C18 0.0554(13) 0.0399(11) 0.0398(11) 0.0017(9) 0.0226(10) 0.0070(9) C19 0.0582(14) 0.0401(11) 0.0401(11) 0.0025(9) 0.0189(10) 0.0047(10) C17 0.0642(15) 0.0480(13) 0.0486(13) -0.0059(10) 0.0202(11) -0.0066(11) N6 0.0740(15) 0.0590(14) 0.0873(17) -0.0277(12) 0.0146(13) 0.0104(11) N5 0.0590(11) 0.0383(9) 0.0453(10) 0.0031(8) 0.0222(9) 0.0040(8) C24 0.0714(16) 0.0395(12) 0.0543(14) 0.0013(10) 0.0282(12) 0.0009(11) C20 0.0652(16) 0.0486(14) 0.0813(18) 0.0146(13) 0.0340(14) 0.0042(12) C23 0.0647(18) 0.078(2) 0.0764(19) 0.0201(16) 0.0159(15) -0.0183(15) C22 0.106(3) 0.0617(18) 0.0562(16) -0.0074(14) 0.0135(17) -0.0185(17) C21 0.107(3) 0.0579(18) 0.094(2) -0.0311(17) 0.019(2) 0.0037(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N2 2.2723(17) . ? Cd1 N5 2.2869(18) 4_565 ? Cd1 O2 2.3332(16) . ? Cd1 O5 2.3507(16) 4_576 ? Cd1 O4 2.4158(15) 4_576 ? Cd1 N3 2.6357(19) . ? Cd1 O1 2.6436(18) . ? Cd1 C38 2.711(2) 4_576 ? O4 C38 1.248(3) . ? O4 Cd1 2.4158(15) 4_675 ? O5 C38 1.262(3) . ? O5 Cd1 2.3507(16) 4_675 ? N3 C8 1.334(3) . ? N3 C4 1.342(3) . ? O2 C25 1.257(3) . ? N1 C3 1.361(3) . ? N1 C2 1.379(3) . ? N1 C9 1.462(3) . ? O3 C31 1.382(3) . ? O3 C32 1.399(3) . ? O1 C25 1.246(3) . ? N2 C3 1.321(3) . ? N2 C1 1.368(3) . ? C4 C5 1.383(3) . ? C4 C3 1.471(3) . ? C16 C10 1.384(3) . ? C16 C14 1.386(3) . ? C16 H16 0.9300 . ? C38 C37 1.504(3) . ? C38 Cd1 2.711(2) 4_675 ? C9 C10 1.513(3) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C26 C29 1.380(3) . ? C26 C27 1.383(3) . ? C26 C25 1.503(3) . ? C14 C13 1.381(3) . ? C14 C15 1.507(3) . ? C10 C11 1.393(3) . ? C37 C34 1.380(3) . ? C37 C36 1.385(3) . ? C2 C1 1.343(3) . ? C2 H2 0.9300 . ? C32 C35 1.362(4) . ? C32 C33 1.368(4) . ? C28 C31 1.376(3) . ? C28 C27 1.385(3) . ? C28 H28 0.9300 . ? C31 C30 1.378(3) . ? O1W H1A 0.77(4) . ? O1W H1B 0.77(4) . ? C5 C6 1.389(3) . ? C5 H5 0.9300 . ? C15 N4 1.471(3) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C1 H1 0.9300 . ? C8 C7 1.369(4) . ? C8 H8 0.9300 . ? C30 C29 1.384(3) . ? C30 H30 0.9300 . ? C33 C34 1.384(3) . ? C33 H33 0.9300 . ? C29 H29 0.9300 . ? C27 H27 0.9300 . ? C36 C35 1.392(3) . ? C36 H36 0.9300 . ? C35 H35 0.9300 . ? C6 C7 1.369(4) . ? C6 H6 0.9300 . ? C11 C12 1.376(3) . ? C11 H11 0.9300 . ? C12 C13 1.386(4) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C34 H34 0.9300 . ? C7 H7 0.9300 . ? N4 C18 1.359(3) . ? N4 C17 1.373(3) . ? C18 N5 1.334(3) . ? C18 C19 1.474(3) . ? C19 N6 1.334(3) . ? C19 C20 1.368(3) . ? C17 C24 1.343(3) . ? C17 H17 0.9300 . ? N6 C21 1.337(4) . ? N5 C24 1.371(3) . ? N5 Cd1 2.2869(18) 4_666 ? C24 H24 0.9300 . ? C20 C23 1.390(4) . ? C20 H20 0.9300 . ? C23 C22 1.351(4) . ? C23 H23 0.9300 . ? C22 C21 1.330(4) . ? C22 H22 0.9300 . ? C21 H21 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 N2 Cd1 N5 109.09(6) . 4_565 ? N2 Cd1 O2 131.78(6) . . ? N5 Cd1 O2 92.68(6) 4_565 . ? N2 Cd1 O5 90.90(6) . 4_576 ? N5 Cd1 O5 150.72(6) 4_565 4_576 ? O2 Cd1 O5 89.19(6) . 4_576 ? N2 Cd1 O4 131.88(6) . 4_576 ? N5 Cd1 O4 95.90(6) 4_565 4_576 ? O2 Cd1 O4 85.30(6) . 4_576 ? O5 Cd1 O4 55.12(6) 4_576 4_576 ? N2 Cd1 N3 67.56(6) . . ? N5 Cd1 N3 77.39(6) 4_565 . ? O2 Cd1 N3 160.64(6) . . ? O5 Cd1 N3 91.59(6) 4_576 . ? O4 Cd1 N3 79.34(6) 4_576 . ? N2 Cd1 O1 81.64(6) . . ? N5 Cd1 O1 99.56(6) 4_565 . ? O2 Cd1 O1 51.93(6) . . ? O5 Cd1 O1 104.47(6) 4_576 . ? O4 Cd1 O1 134.80(5) 4_576 . ? N3 Cd1 O1 145.51(5) . . ? N2 Cd1 C38 112.99(7) . 4_576 ? N5 Cd1 C38 123.23(7) 4_565 4_576 ? O2 Cd1 C38 86.57(7) . 4_576 ? O5 Cd1 C38 27.72(6) 4_576 4_576 ? O4 Cd1 C38 27.41(6) 4_576 4_576 ? N3 Cd1 C38 85.18(6) . 4_576 ? O1 Cd1 C38 122.41(6) . 4_576 ? C38 O4 Cd1 89.58(13) . 4_675 ? C38 O5 Cd1 92.23(14) . 4_675 ? C8 N3 C4 117.5(2) . . ? C8 N3 Cd1 126.85(16) . . ? C4 N3 Cd1 111.70(13) . . ? C25 O2 Cd1 99.82(14) . . ? C3 N1 C2 106.56(18) . . ? C3 N1 C9 128.87(19) . . ? C2 N1 C9 124.21(19) . . ? C31 O3 C32 118.41(18) . . ? C25 O1 Cd1 85.51(15) . . ? C3 N2 C1 106.62(18) . . ? C3 N2 Cd1 120.84(14) . . ? C1 N2 Cd1 130.91(14) . . ? N3 C4 C5 122.5(2) . . ? N3 C4 C3 112.49(18) . . ? C5 C4 C3 125.0(2) . . ? C10 C16 C14 121.7(2) . . ? C10 C16 H16 119.2 . . ? C14 C16 H16 119.2 . . ? O4 C38 O5 123.1(2) . . ? O4 C38 C37 119.2(2) . . ? O5 C38 C37 117.7(2) . . ? O4 C38 Cd1 63.02(11) . 4_675 ? O5 C38 Cd1 60.05(11) . 4_675 ? C37 C38 Cd1 177.25(16) . 4_675 ? N2 C3 N1 110.38(18) . . ? N2 C3 C4 122.61(18) . . ? N1 C3 C4 126.98(19) . . ? N1 C9 C10 114.43(18) . . ? N1 C9 H9A 108.7 . . ? C10 C9 H9A 108.7 . . ? N1 C9 H9B 108.7 . . ? C10 C9 H9B 108.7 . . ? H9A C9 H9B 107.6 . . ? C29 C26 C27 117.9(2) . . ? C29 C26 C25 122.1(2) . . ? C27 C26 C25 120.0(2) . . ? C13 C14 C16 118.5(2) . . ? C13 C14 C15 122.8(2) . . ? C16 C14 C15 118.6(2) . . ? C16 C10 C11 118.9(2) . . ? C16 C10 C9 122.93(19) . . ? C11 C10 C9 117.9(2) . . ? C34 C37 C36 118.8(2) . . ? C34 C37 C38 119.9(2) . . ? C36 C37 C38 121.2(2) . . ? C1 C2 N1 106.9(2) . . ? C1 C2 H2 126.6 . . ? N1 C2 H2 126.6 . . ? C35 C32 C33 121.4(2) . . ? C35 C32 O3 117.5(2) . . ? C33 C32 O3 121.1(3) . . ? C31 C28 C27 118.8(2) . . ? C31 C28 H28 120.6 . . ? C27 C28 H28 120.6 . . ? C28 C31 C30 120.6(2) . . ? C28 C31 O3 124.42(19) . . ? C30 C31 O3 115.0(2) . . ? H1A O1W H1B 111(5) . . ? C4 C5 C6 118.3(2) . . ? C4 C5 H5 120.8 . . ? C6 C5 H5 120.8 . . ? N4 C15 C14 114.14(18) . . ? N4 C15 H15A 108.7 . . ? C14 C15 H15A 108.7 . . ? N4 C15 H15B 108.7 . . ? C14 C15 H15B 108.7 . . ? H15A C15 H15B 107.6 . . ? C2 C1 N2 109.6(2) . . ? C2 C1 H1 125.2 . . ? N2 C1 H1 125.2 . . ? N3 C8 C7 123.6(2) . . ? N3 C8 H8 118.2 . . ? C7 C8 H8 118.2 . . ? C31 C30 C29 119.5(2) . . ? C31 C30 H30 120.3 . . ? C29 C30 H30 120.3 . . ? C32 C33 C34 119.5(2) . . ? C32 C33 H33 120.3 . . ? C34 C33 H33 120.3 . . ? C26 C29 C30 121.3(2) . . ? C26 C29 H29 119.4 . . ? C30 C29 H29 119.4 . . ? C26 C27 C28 121.9(2) . . ? C26 C27 H27 119.1 . . ? C28 C27 H27 119.1 . . ? C37 C36 C35 120.6(2) . . ? C37 C36 H36 119.7 . . ? C35 C36 H36 119.7 . . ? C32 C35 C36 119.1(2) . . ? C32 C35 H35 120.5 . . ? C36 C35 H35 120.5 . . ? C7 C6 C5 119.2(2) . . ? C7 C6 H6 120.4 . . ? C5 C6 H6 120.4 . . ? C12 C11 C10 120.1(2) . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C11 C12 C13 120.2(2) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? C14 C13 C12 120.7(2) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? O1 C25 O2 122.7(2) . . ? O1 C25 C26 119.3(2) . . ? O2 C25 C26 118.0(2) . . ? C37 C34 C33 120.6(2) . . ? C37 C34 H34 119.7 . . ? C33 C34 H34 119.7 . . ? C8 C7 C6 118.7(2) . . ? C8 C7 H7 120.7 . . ? C6 C7 H7 120.7 . . ? C18 N4 C17 107.41(18) . . ? C18 N4 C15 127.85(18) . . ? C17 N4 C15 124.7(2) . . ? N5 C18 N4 110.03(19) . . ? N5 C18 C19 124.3(2) . . ? N4 C18 C19 125.69(18) . . ? N6 C19 C20 121.3(2) . . ? N6 C19 C18 116.7(2) . . ? C20 C19 C18 121.9(2) . . ? C24 C17 N4 106.4(2) . . ? C24 C17 H17 126.8 . . ? N4 C17 H17 126.8 . . ? C19 N6 C21 117.3(3) . . ? C18 N5 C24 105.90(19) . . ? C18 N5 Cd1 131.18(15) . 4_666 ? C24 N5 Cd1 120.76(14) . 4_666 ? C17 C24 N5 110.3(2) . . ? C17 C24 H24 124.9 . . ? N5 C24 H24 124.9 . . ? C19 C20 C23 118.7(3) . . ? C19 C20 H20 120.6 . . ? C23 C20 H20 120.6 . . ? C22 C23 C20 119.5(3) . . ? C22 C23 H23 120.2 . . ? C20 C23 H23 120.2 . . ? C21 C22 C23 117.9(3) . . ? C21 C22 H22 121.1 . . ? C23 C22 H22 121.1 . . ? C22 C21 N6 125.0(3) . . ? C22 C21 H21 117.5 . . ? N6 C21 H21 117.5 . . ? 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 N2 Cd1 N3 C8 -170.4(2) . . . . ? N5 Cd1 N3 C8 -53.3(2) 4_565 . . . ? O2 Cd1 N3 C8 7.2(3) . . . . ? O5 Cd1 N3 C8 99.3(2) 4_576 . . . ? O4 Cd1 N3 C8 45.2(2) 4_576 . . . ? O1 Cd1 N3 C8 -141.91(18) . . . . ? C38 Cd1 N3 C8 72.3(2) 4_576 . . . ? N2 Cd1 N3 C4 -13.46(14) . . . . ? N5 Cd1 N3 C4 103.60(15) 4_565 . . . ? O2 Cd1 N3 C4 164.13(17) . . . . ? O5 Cd1 N3 C4 -103.78(14) 4_576 . . . ? O4 Cd1 N3 C4 -157.81(15) 4_576 . . . ? O1 Cd1 N3 C4 15.0(2) . . . . ? C38 Cd1 N3 C4 -130.77(15) 4_576 . . . ? N2 Cd1 O2 C25 18.99(18) . . . . ? N5 Cd1 O2 C25 -99.75(15) 4_565 . . . ? O5 Cd1 O2 C25 109.48(14) 4_576 . . . ? O4 Cd1 O2 C25 164.55(15) 4_576 . . . ? N3 Cd1 O2 C25 -158.01(17) . . . . ? O1 Cd1 O2 C25 0.30(13) . . . . ? C38 Cd1 O2 C25 137.10(15) 4_576 . . . ? N2 Cd1 O1 C25 -166.33(14) . . . . ? N5 Cd1 O1 C25 85.59(14) 4_565 . . . ? O2 Cd1 O1 C25 -0.30(13) . . . . ? O5 Cd1 O1 C25 -77.56(14) 4_576 . . . ? O4 Cd1 O1 C25 -22.72(17) 4_576 . . . ? N3 Cd1 O1 C25 167.21(12) . . . . ? C38 Cd1 O1 C25 -54.35(15) 4_576 . . . ? N5 Cd1 N2 C3 -66.21(16) 4_565 . . . ? O2 Cd1 N2 C3 -178.27(14) . . . . ? O5 Cd1 N2 C3 92.01(16) 4_576 . . . ? O4 Cd1 N2 C3 50.94(18) 4_576 . . . ? N3 Cd1 N2 C3 0.66(14) . . . . ? O1 Cd1 N2 C3 -163.50(16) . . . . ? C38 Cd1 N2 C3 74.76(16) 4_576 . . . ? N5 Cd1 N2 C1 130.45(19) 4_565 . . . ? O2 Cd1 N2 C1 18.4(2) . . . . ? O5 Cd1 N2 C1 -71.34(19) 4_576 . . . ? O4 Cd1 N2 C1 -112.40(18) 4_576 . . . ? N3 Cd1 N2 C1 -162.7(2) . . . . ? O1 Cd1 N2 C1 33.16(19) . . . . ? C38 Cd1 N2 C1 -88.58(19) 4_576 . . . ? C8 N3 C4 C5 3.1(3) . . . . ? Cd1 N3 C4 C5 -156.16(17) . . . . ? C8 N3 C4 C3 -178.15(19) . . . . ? Cd1 N3 C4 C3 22.5(2) . . . . ? Cd1 O4 C38 O5 1.2(2) 4_675 . . . ? Cd1 O4 C38 C37 -178.17(17) 4_675 . . . ? Cd1 O5 C38 O4 -1.3(2) 4_675 . . . ? Cd1 O5 C38 C37 178.14(16) 4_675 . . . ? C1 N2 C3 N1 0.7(2) . . . . ? Cd1 N2 C3 N1 -166.19(13) . . . . ? C1 N2 C3 C4 179.15(18) . . . . ? Cd1 N2 C3 C4 12.2(3) . . . . ? C2 N1 C3 N2 -0.6(2) . . . . ? C9 N1 C3 N2 172.56(19) . . . . ? C2 N1 C3 C4 -178.94(19) . . . . ? C9 N1 C3 C4 -5.8(3) . . . . ? N3 C4 C3 N2 -24.9(3) . . . . ? C5 C4 C3 N2 153.8(2) . . . . ? N3 C4 C3 N1 153.2(2) . . . . ? C5 C4 C3 N1 -28.1(3) . . . . ? C3 N1 C9 C10 106.3(2) . . . . ? C2 N1 C9 C10 -81.6(3) . . . . ? C10 C16 C14 C13 2.1(3) . . . . ? C10 C16 C14 C15 -174.8(2) . . . . ? C14 C16 C10 C11 -1.7(3) . . . . ? C14 C16 C10 C9 172.1(2) . . . . ? N1 C9 C10 C16 12.8(3) . . . . ? N1 C9 C10 C11 -173.39(19) . . . . ? O4 C38 C37 C34 -6.9(3) . . . . ? O5 C38 C37 C34 173.7(2) . . . . ? O4 C38 C37 C36 171.3(2) . . . . ? O5 C38 C37 C36 -8.1(3) . . . . ? C3 N1 C2 C1 0.2(2) . . . . ? C9 N1 C2 C1 -173.34(19) . . . . ? C31 O3 C32 C35 121.0(3) . . . . ? C31 O3 C32 C33 -61.9(4) . . . . ? C27 C28 C31 C30 -0.1(4) . . . . ? C27 C28 C31 O3 -178.8(2) . . . . ? C32 O3 C31 C28 -4.3(4) . . . . ? C32 O3 C31 C30 177.0(3) . . . . ? N3 C4 C5 C6 -4.4(3) . . . . ? C3 C4 C5 C6 177.1(2) . . . . ? C13 C14 C15 N4 -32.6(3) . . . . ? C16 C14 C15 N4 144.2(2) . . . . ? N1 C2 C1 N2 0.2(3) . . . . ? C3 N2 C1 C2 -0.6(2) . . . . ? Cd1 N2 C1 C2 164.54(15) . . . . ? C4 N3 C8 C7 0.4(4) . . . . ? Cd1 N3 C8 C7 156.2(2) . . . . ? C28 C31 C30 C29 -1.2(4) . . . . ? O3 C31 C30 C29 177.5(2) . . . . ? C35 C32 C33 C34 -2.3(4) . . . . ? O3 C32 C33 C34 -179.2(2) . . . . ? C27 C26 C29 C30 0.6(4) . . . . ? C25 C26 C29 C30 -177.0(2) . . . . ? C31 C30 C29 C26 1.0(4) . . . . ? C29 C26 C27 C28 -2.0(4) . . . . ? C25 C26 C27 C28 175.6(2) . . . . ? C31 C28 C27 C26 1.8(4) . . . . ? C34 C37 C36 C35 -1.4(4) . . . . ? C38 C37 C36 C35 -179.7(2) . . . . ? C33 C32 C35 C36 1.6(4) . . . . ? O3 C32 C35 C36 178.6(2) . . . . ? C37 C36 C35 C32 0.3(4) . . . . ? C4 C5 C6 C7 2.1(4) . . . . ? C16 C10 C11 C12 0.0(3) . . . . ? C9 C10 C11 C12 -174.1(2) . . . . ? C10 C11 C12 C13 1.2(4) . . . . ? C16 C14 C13 C12 -0.9(4) . . . . ? C15 C14 C13 C12 175.9(2) . . . . ? C11 C12 C13 C14 -0.7(4) . . . . ? Cd1 O1 C25 O2 0.5(2) . . . . ? Cd1 O1 C25 C26 179.22(18) . . . . ? Cd1 O2 C25 O1 -0.6(3) . . . . ? Cd1 O2 C25 C26 -179.32(16) . . . . ? C29 C26 C25 O1 13.5(3) . . . . ? C27 C26 C25 O1 -164.0(2) . . . . ? C29 C26 C25 O2 -167.7(2) . . . . ? C27 C26 C25 O2 14.8(3) . . . . ? C36 C37 C34 C33 0.7(4) . . . . ? C38 C37 C34 C33 179.0(2) . . . . ? C32 C33 C34 C37 1.1(4) . . . . ? N3 C8 C7 C6 -2.6(4) . . . . ? C5 C6 C7 C8 1.2(4) . . . . ? C14 C15 N4 C18 -81.3(3) . . . . ? C14 C15 N4 C17 100.2(3) . . . . ? C17 N4 C18 N5 0.5(2) . . . . ? C15 N4 C18 N5 -178.2(2) . . . . ? C17 N4 C18 C19 -178.2(2) . . . . ? C15 N4 C18 C19 3.1(3) . . . . ? N5 C18 C19 N6 -149.9(2) . . . . ? N4 C18 C19 N6 28.6(3) . . . . ? N5 C18 C19 C20 29.9(3) . . . . ? N4 C18 C19 C20 -151.6(2) . . . . ? C18 N4 C17 C24 -0.4(3) . . . . ? C15 N4 C17 C24 178.4(2) . . . . ? C20 C19 N6 C21 -1.9(4) . . . . ? C18 C19 N6 C21 177.9(3) . . . . ? N4 C18 N5 C24 -0.5(2) . . . . ? C19 C18 N5 C24 178.2(2) . . . . ? N4 C18 N5 Cd1 -163.38(15) . . . 4_666 ? C19 C18 N5 Cd1 15.4(3) . . . 4_666 ? N4 C17 C24 N5 0.1(3) . . . . ? C18 N5 C24 C17 0.3(3) . . . . ? Cd1 N5 C24 C17 165.32(16) 4_666 . . . ? N6 C19 C20 C23 4.2(4) . . . . ? C18 C19 C20 C23 -175.5(2) . . . . ? C19 C20 C23 C22 -2.5(4) . . . . ? C20 C23 C22 C21 -1.5(5) . . . . ? C23 C22 C21 N6 4.1(6) . . . . ? C19 N6 C21 C22 -2.5(5) . . . . ? 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 O1W H1A O1 0.77(4) 2.09(4) 2.859(3) 173(5) . O1W H1B O5 0.77(4) 2.15(4) 2.920(3) 176(5) 2_646 _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.591 _refine_diff_density_min -0.539 _refine_diff_density_rms 0.049 data_8 _database_code_depnum_ccdc_archive 'CCDC 687555' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H34 Cd N6 O8' _chemical_formula_weight 815.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.4920(4) _cell_length_b 11.7810(4) _cell_length_c 14.6520(5) _cell_angle_alpha 71.9450(10) _cell_angle_beta 73.4360(10) _cell_angle_gamma 80.0840(10) _cell_volume 1800.08(11) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.83 _cell_measurement_theta_max 28.32 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.504 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 832 _exptl_absorpt_coefficient_mu 0.668 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.812 _exptl_absorpt_correction_T_max 0.841 _exptl_absorpt_process_details 'SADABS(Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11223 _diffrn_reflns_av_R_equivalents 0.0137 _diffrn_reflns_av_sigmaI/netI 0.0290 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 28.32 _reflns_number_total 8218 _reflns_number_gt 7267 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SMART (Bruker, 1997)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97(Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material SHELXL-97 _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^)+(0.0470P)^2^+0.7787P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8218 _refine_ls_number_parameters 490 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0405 _refine_ls_R_factor_gt 0.0341 _refine_ls_wR_factor_ref 0.0907 _refine_ls_wR_factor_gt 0.0855 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.146753(14) 0.060121(15) 0.497420(11) 0.03732(7) Uani 1 1 d . . . O2 O 0.03962(18) 0.19811(19) 0.57891(14) 0.0550(5) Uani 1 1 d . . . O1 O 0.17972(16) 0.08200(17) 0.64880(13) 0.0490(4) Uani 1 1 d . . . N3 N 0.35181(18) 0.11643(19) 0.43330(15) 0.0429(4) Uani 1 1 d . . . O3 O -0.0915(2) 0.35911(18) 0.97248(13) 0.0568(5) Uani 1 1 d . . . N2 N 0.27263(18) -0.09162(19) 0.44844(16) 0.0446(5) Uani 1 1 d . . . N1 N 0.44624(19) -0.16749(19) 0.36824(17) 0.0464(5) Uani 1 1 d . . . N4 N 0.4751(2) -0.2574(2) 0.0666(2) 0.0602(6) Uani 1 1 d . . . C25 C 0.0926(2) 0.1620(2) 0.64879(17) 0.0417(5) Uani 1 1 d . . . C4 C 0.4367(2) 0.0408(2) 0.39213(17) 0.0385(5) Uani 1 1 d . . . C5 C 0.5566(2) 0.0692(3) 0.3513(2) 0.0527(6) Uani 1 1 d . . . H5 H 0.6154 0.0168 0.3231 0.063 Uiso 1 1 calc R . . C28 C -0.0818(2) 0.3620(2) 0.81071(18) 0.0424(5) Uani 1 1 d . . . H28 H -0.1391 0.4284 0.8078 0.051 Uiso 1 1 calc R . . C29 C -0.0390(2) 0.3100(2) 0.89440(17) 0.0411(5) Uani 1 1 d . . . C26 C 0.0484(2) 0.2158(2) 0.73403(17) 0.0389(5) Uani 1 1 d . . . C1 C 0.3638(3) -0.2519(3) 0.3988(2) 0.0557(7) Uani 1 1 d . . . H1 H 0.3782 -0.3276 0.3883 0.067 Uiso 1 1 calc R . . C3 C 0.3879(2) -0.0708(2) 0.40031(18) 0.0402(5) Uani 1 1 d . . . C23 C 0.7854(3) 0.0523(3) -0.1054(4) 0.0877(13) Uani 1 1 d . . . H23 H 0.8381 0.1109 -0.1208 0.105 Uiso 1 1 calc R . . C7 C 0.5000(3) 0.2535(3) 0.3948(2) 0.0560(7) Uani 1 1 d . . . H7 H 0.5190 0.3264 0.3963 0.067 Uiso 1 1 calc R . . C2 C 0.2578(3) -0.2033(3) 0.4470(2) 0.0548(7) Uani 1 1 d . . . H2 H 0.1858 -0.2405 0.4749 0.066 Uiso 1 1 calc R . . C15 C 0.5746(3) -0.3230(2) 0.2071(2) 0.0521(6) Uani 1 1 d . . . C30 C 0.0496(3) 0.2130(3) 0.89884(19) 0.0497(6) Uani 1 1 d . . . H30 H 0.0791 0.1794 0.9552 0.060 Uiso 1 1 calc R . . N6 N 0.6442(2) -0.0780(2) 0.0177(2) 0.0644(7) Uani 1 1 d . . . C27 C -0.0385(2) 0.3139(2) 0.73085(17) 0.0428(5) Uani 1 1 d . . . H27 H -0.0679 0.3476 0.6744 0.051 Uiso 1 1 calc R . . C20 C 0.6292(3) -0.1171(2) -0.0538(2) 0.0523(6) Uani 1 1 d . . . C31 C 0.0927(2) 0.1676(2) 0.81775(19) 0.0452(6) Uani 1 1 d . . . H31 H 0.1527 0.1035 0.8195 0.054 Uiso 1 1 calc R . . C16 C 0.4753(3) -0.2439(3) 0.1618(2) 0.0609(7) Uani 1 1 d . . . H16A H 0.3969 -0.2623 0.2075 0.073 Uiso 1 1 calc R . . H16B H 0.4850 -0.1609 0.1536 0.073 Uiso 1 1 calc R . . C8 C 0.3836(3) 0.2193(2) 0.4342(2) 0.0519(6) Uani 1 1 d . . . H8 H 0.3240 0.2707 0.4630 0.062 Uiso 1 1 calc R . . C19 C 0.5423(3) -0.2070(3) -0.0264(2) 0.0570(7) Uani 1 1 d . . . C9 C 0.5732(2) -0.1795(3) 0.3064(2) 0.0561(7) Uani 1 1 d . . . H9A H 0.6290 -0.1689 0.3412 0.067 Uiso 1 1 calc R . . H9B H 0.5814 -0.1154 0.2451 0.067 Uiso 1 1 calc R . . C10 C 0.6108(2) -0.2972(3) 0.2814(2) 0.0534(7) Uani 1 1 d . . . C6 C 0.5869(3) 0.1770(3) 0.3534(2) 0.0591(7) Uani 1 1 d . . . H6 H 0.6668 0.1973 0.3265 0.071 Uiso 1 1 calc R . . C11 C 0.6940(3) -0.3773(3) 0.3278(3) 0.0670(8) Uani 1 1 d . . . H11 H 0.7158 -0.3615 0.3788 0.080 Uiso 1 1 calc R . . C22 C 0.7216(3) 0.0065(3) -0.0090(3) 0.0777(10) Uani 1 1 d . . . H22 H 0.7327 0.0356 0.0399 0.093 Uiso 1 1 calc R . . N5 N 0.5164(3) -0.2485(3) -0.0921(2) 0.0818(9) Uani 1 1 d . . . C14 C 0.6270(3) -0.4270(3) 0.1798(3) 0.0664(8) Uani 1 1 d . . . H14 H 0.6045 -0.4450 0.1300 0.080 Uiso 1 1 calc R . . C21 C 0.6906(3) -0.0747(3) -0.1528(3) 0.0711(9) Uani 1 1 d . . . H21 H 0.6778 -0.1038 -0.2011 0.085 Uiso 1 1 calc R . . C17 C 0.4037(3) -0.3331(4) 0.0573(4) 0.0854(12) Uani 1 1 d . . . H17 H 0.3481 -0.3801 0.1081 0.102 Uiso 1 1 calc R . . C24 C 0.7703(4) 0.0107(3) -0.1779(3) 0.0865(12) Uani 1 1 d . . . H24 H 0.8134 0.0396 -0.2433 0.104 Uiso 1 1 calc R . . C12 C 0.7449(3) -0.4801(3) 0.2998(3) 0.0778(10) Uani 1 1 d . . . H12 H 0.8011 -0.5325 0.3312 0.093 Uiso 1 1 calc R . . C13 C 0.7122(3) -0.5042(3) 0.2256(3) 0.0777(10) Uani 1 1 d . . . H13 H 0.7472 -0.5727 0.2056 0.093 Uiso 1 1 calc R . . C18 C 0.4296(4) -0.3264(4) -0.0387(4) 0.0956(13) Uani 1 1 d . . . H18 H 0.3936 -0.3687 -0.0657 0.115 Uiso 1 1 calc R . . C33 C -0.0546(2) 0.3081(2) 1.06053(17) 0.0443(6) Uani 1 1 d . . . C32 C -0.1156(3) 0.2182(2) 1.1322(2) 0.0519(6) Uani 1 1 d . . . H32 H -0.1783 0.1877 1.1211 0.062 Uiso 1 1 calc R . . C34 C 0.0380(3) 0.3542(3) 1.0748(2) 0.0582(7) Uani 1 1 d . . . H34 H 0.0798 0.4143 1.0246 0.070 Uiso 1 1 calc R . . C36 C 0.0085(2) 0.2192(2) 1.23923(16) 0.0387(5) Uani 1 1 d . . . C35 C -0.0831(2) 0.1728(2) 1.22175(19) 0.0472(6) Uani 1 1 d . . . H35 H -0.1234 0.1106 1.2705 0.057 Uiso 1 1 calc R . . C37 C 0.0688(3) 0.3102(3) 1.1651(2) 0.0553(7) Uani 1 1 d . . . H37 H 0.1306 0.3421 1.1760 0.066 Uiso 1 1 calc R . . O5 O -0.00154(17) 0.08082(17) 1.39964(13) 0.0517(4) Uani 1 1 d . . . O4 O 0.13298(19) 0.21069(19) 1.34557(14) 0.0594(5) Uani 1 1 d . . . C38 C 0.0476(2) 0.1680(2) 1.33408(17) 0.0399(5) Uani 1 1 d . . . O3W O 0.0778(8) 0.4218(4) 0.4528(5) 0.312(6) Uani 1 1 d . . . O2W O 0.3151(4) 0.5205(3) 0.3475(4) 0.1287(13) Uani 1 1 d D . . O1W O 0.3122(3) 0.3752(2) 0.2287(2) 0.0839(7) Uani 1 1 d D . . H2B H 0.257(4) 0.505(5) 0.395(3) 0.126 Uiso 1 1 d D . . H1B H 0.259(3) 0.337(3) 0.270(3) 0.126 Uiso 1 1 d D . . H2A H 0.327(4) 0.477(4) 0.311(3) 0.126 Uiso 1 1 d D . . H1A H 0.373(3) 0.337(3) 0.206(4) 0.126 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.03516(9) 0.04620(11) 0.03120(9) -0.01427(7) -0.00638(6) -0.00177(7) O2 0.0614(12) 0.0683(12) 0.0416(10) -0.0268(9) -0.0184(9) 0.0087(10) O1 0.0448(9) 0.0570(11) 0.0467(10) -0.0250(8) -0.0052(8) 0.0010(8) N3 0.0401(10) 0.0459(11) 0.0432(11) -0.0155(9) -0.0078(9) -0.0039(9) O3 0.0782(13) 0.0577(11) 0.0386(9) -0.0232(8) -0.0273(9) 0.0236(10) N2 0.0371(10) 0.0470(12) 0.0496(12) -0.0203(10) -0.0014(9) -0.0064(9) N1 0.0383(10) 0.0470(12) 0.0542(13) -0.0240(10) -0.0006(9) -0.0043(9) N4 0.0515(13) 0.0621(15) 0.0694(16) -0.0252(13) -0.0064(12) -0.0132(11) C25 0.0423(12) 0.0487(14) 0.0340(12) -0.0148(10) -0.0021(10) -0.0095(10) C4 0.0377(11) 0.0433(12) 0.0359(11) -0.0135(10) -0.0102(9) -0.0010(9) C5 0.0373(12) 0.0532(15) 0.0681(18) -0.0243(14) -0.0048(12) -0.0056(11) C28 0.0488(13) 0.0408(12) 0.0373(12) -0.0114(10) -0.0140(10) 0.0036(10) C29 0.0480(13) 0.0435(13) 0.0345(11) -0.0149(10) -0.0131(10) 0.0013(10) C26 0.0390(11) 0.0450(13) 0.0325(11) -0.0131(10) -0.0056(9) -0.0046(10) C1 0.0534(15) 0.0493(15) 0.0654(18) -0.0269(13) 0.0004(13) -0.0125(12) C3 0.0356(11) 0.0459(13) 0.0408(12) -0.0173(10) -0.0067(9) -0.0030(9) C23 0.060(2) 0.058(2) 0.131(4) -0.011(2) -0.014(2) -0.0141(16) C7 0.0581(16) 0.0507(15) 0.0658(18) -0.0202(14) -0.0168(14) -0.0121(13) C2 0.0455(14) 0.0558(16) 0.0616(17) -0.0237(13) 0.0034(12) -0.0149(12) C15 0.0479(14) 0.0455(14) 0.0556(16) -0.0183(12) 0.0035(12) -0.0047(11) C30 0.0573(15) 0.0563(15) 0.0385(13) -0.0173(11) -0.0214(12) 0.0109(12) N6 0.0675(16) 0.0603(15) 0.0715(17) -0.0117(13) -0.0282(14) -0.0151(13) C27 0.0502(13) 0.0473(13) 0.0313(11) -0.0093(10) -0.0141(10) -0.0016(11) C20 0.0477(14) 0.0477(15) 0.0616(17) -0.0155(13) -0.0150(13) -0.0016(11) C31 0.0455(13) 0.0496(14) 0.0411(13) -0.0168(11) -0.0139(11) 0.0078(11) C16 0.0543(16) 0.0584(17) 0.0627(18) -0.0226(14) -0.0006(14) 0.0015(13) C8 0.0514(15) 0.0473(14) 0.0589(16) -0.0227(13) -0.0090(13) -0.0023(12) C19 0.0522(15) 0.0618(17) 0.0623(18) -0.0237(14) -0.0157(14) -0.0041(13) C9 0.0392(13) 0.0566(16) 0.0750(19) -0.0353(15) 0.0013(13) -0.0048(11) C10 0.0408(13) 0.0515(15) 0.0642(17) -0.0265(13) 0.0039(12) -0.0044(11) C6 0.0447(14) 0.0599(17) 0.074(2) -0.0208(15) -0.0083(14) -0.0148(13) C11 0.0528(17) 0.069(2) 0.080(2) -0.0299(17) -0.0115(16) 0.0004(15) C22 0.075(2) 0.061(2) 0.108(3) -0.014(2) -0.044(2) -0.0161(17) N5 0.086(2) 0.096(2) 0.081(2) -0.0401(18) -0.0259(17) -0.0168(18) C14 0.070(2) 0.0537(17) 0.076(2) -0.0332(16) -0.0032(16) -0.0014(15) C21 0.076(2) 0.0593(19) 0.067(2) -0.0191(16) -0.0036(17) 0.0002(16) C17 0.063(2) 0.082(2) 0.117(3) -0.036(2) -0.009(2) -0.0288(19) C24 0.078(2) 0.056(2) 0.094(3) -0.0100(19) 0.015(2) -0.0040(18) C12 0.065(2) 0.061(2) 0.100(3) -0.0247(19) -0.0174(19) 0.0142(16) C13 0.074(2) 0.0513(18) 0.101(3) -0.0353(19) -0.005(2) 0.0102(16) C18 0.085(3) 0.110(3) 0.121(4) -0.057(3) -0.031(3) -0.028(2) C33 0.0558(14) 0.0464(13) 0.0332(12) -0.0176(10) -0.0164(11) 0.0103(11) C32 0.0619(16) 0.0496(15) 0.0552(16) -0.0170(12) -0.0290(13) -0.0045(12) C34 0.0664(18) 0.0602(17) 0.0405(14) 0.0035(12) -0.0168(13) -0.0126(14) C36 0.0424(12) 0.0424(12) 0.0309(11) -0.0120(9) -0.0088(9) 0.0003(10) C35 0.0487(14) 0.0489(14) 0.0424(13) -0.0057(11) -0.0136(11) -0.0089(11) C37 0.0631(17) 0.0557(16) 0.0498(15) -0.0019(12) -0.0249(13) -0.0177(13) O5 0.0556(11) 0.0599(11) 0.0347(9) -0.0022(8) -0.0109(8) -0.0130(9) O4 0.0658(12) 0.0738(13) 0.0433(10) -0.0049(9) -0.0235(9) -0.0232(11) C38 0.0438(12) 0.0455(13) 0.0302(11) -0.0131(10) -0.0076(9) -0.0009(10) O3W 0.383(10) 0.098(3) 0.239(7) 0.027(4) 0.136(7) 0.048(5) O2W 0.128(3) 0.086(2) 0.190(5) -0.061(3) -0.043(3) -0.010(2) O1W 0.0888(19) 0.0873(18) 0.0790(18) -0.0149(14) -0.0235(15) -0.0278(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 Cd1 N2 2.262(2) . ? Cd1 O2 2.2934(18) . ? Cd1 N3 2.401(2) . ? Cd1 O4 2.4040(19) 1_554 ? Cd1 O5 2.4049(18) 2_557 ? Cd1 O1 2.4489(18) . ? Cd1 O5 2.4594(19) 1_554 ? Cd1 C25 2.712(2) . ? O2 C25 1.264(3) . ? O1 C25 1.251(3) . ? N3 C8 1.329(3) . ? N3 C4 1.344(3) . ? O3 C29 1.380(3) . ? O3 C33 1.396(3) . ? N2 C3 1.335(3) . ? N2 C2 1.363(3) . ? N1 C3 1.362(3) . ? N1 C1 1.377(3) . ? N1 C9 1.492(3) . ? N4 C19 1.365(4) . ? N4 C17 1.371(4) . ? N4 C16 1.452(4) . ? C25 C26 1.496(3) . ? C4 C5 1.390(3) . ? C4 C3 1.476(3) . ? C5 C6 1.384(4) . ? C5 H5 0.9300 . ? C28 C29 1.377(3) . ? C28 C27 1.386(3) . ? C28 H28 0.9300 . ? C29 C30 1.392(3) . ? C26 C31 1.382(3) . ? C26 C27 1.389(3) . ? C1 C2 1.353(4) . ? C1 H1 0.9300 . ? C23 C24 1.362(6) . ? C23 C22 1.376(6) . ? C23 H23 0.9300 . ? C7 C6 1.364(4) . ? C7 C8 1.374(4) . ? C7 H7 0.9300 . ? C2 H2 0.9300 . ? C15 C14 1.391(4) . ? C15 C10 1.398(4) . ? C15 C16 1.514(4) . ? C30 C31 1.382(3) . ? C30 H30 0.9300 . ? N6 C20 1.330(4) . ? N6 C22 1.343(4) . ? C27 H27 0.9300 . ? C20 C21 1.393(4) . ? C20 C19 1.467(4) . ? C31 H31 0.9300 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C8 H8 0.9300 . ? C19 N5 1.327(4) . ? C9 C10 1.504(4) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.390(5) . ? C6 H6 0.9300 . ? C11 C12 1.380(5) . ? C11 H11 0.9300 . ? C22 H22 0.9300 . ? N5 C18 1.369(5) . ? C14 C13 1.389(5) . ? C14 H14 0.9300 . ? C21 C24 1.373(5) . ? C21 H21 0.9300 . ? C17 C18 1.331(6) . ? C17 H17 0.9300 . ? C24 H24 0.9300 . ? C12 C13 1.366(6) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C18 H18 0.9300 . ? C33 C32 1.365(4) . ? C33 C34 1.366(4) . ? C32 C35 1.387(4) . ? C32 H32 0.9300 . ? C34 C37 1.387(4) . ? C34 H34 0.9300 . ? C36 C35 1.382(3) . ? C36 C37 1.384(4) . ? C36 C38 1.497(3) . ? C35 H35 0.9300 . ? C37 H37 0.9300 . ? O5 C38 1.256(3) . ? O5 Cd1 2.4049(18) 2_557 ? O5 Cd1 2.4594(19) 1_556 ? O4 C38 1.249(3) . ? O4 Cd1 2.4040(19) 1_556 ? O2W H2B 0.81(4) . ? O2W H2A 0.82(4) . ? O1W H1B 0.81(4) . ? O1W H1A 0.81(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Cd1 O2 166.26(7) . . ? N2 Cd1 N3 70.19(7) . . ? O2 Cd1 N3 106.04(7) . . ? N2 Cd1 O4 104.48(8) . 1_554 ? O2 Cd1 O4 87.25(7) . 1_554 ? N3 Cd1 O4 78.31(7) . 1_554 ? N2 Cd1 O5 89.27(7) . 2_557 ? O2 Cd1 O5 89.08(7) . 2_557 ? N3 Cd1 O5 151.23(7) . 2_557 ? O4 Cd1 O5 127.72(6) 1_554 2_557 ? N2 Cd1 O1 111.23(7) . . ? O2 Cd1 O1 55.07(6) . . ? N3 Cd1 O1 81.22(7) . . ? O4 Cd1 O1 129.28(7) 1_554 . ? O5 Cd1 O1 88.16(6) 2_557 . ? N2 Cd1 O5 98.17(7) . 1_554 ? O2 Cd1 O5 94.61(7) . 1_554 ? N3 Cd1 O5 126.05(6) . 1_554 ? O4 Cd1 O5 53.07(6) 1_554 1_554 ? O5 Cd1 O5 75.35(6) 2_557 1_554 ? O1 Cd1 O5 146.11(6) . 1_554 ? N2 Cd1 C25 138.60(8) . . ? O2 Cd1 C25 27.66(7) . . ? N3 Cd1 C25 95.06(7) . . ? O4 Cd1 C25 110.13(8) 1_554 . ? O5 Cd1 C25 87.18(7) 2_557 . ? O1 Cd1 C25 27.46(7) . . ? O5 Cd1 C25 120.57(7) 1_554 . ? C25 O2 Cd1 94.91(15) . . ? C25 O1 Cd1 88.04(14) . . ? C8 N3 C4 119.2(2) . . ? C8 N3 Cd1 123.18(17) . . ? C4 N3 Cd1 117.55(15) . . ? C29 O3 C33 118.23(19) . . ? C3 N2 C2 106.9(2) . . ? C3 N2 Cd1 117.88(16) . . ? C2 N2 Cd1 134.91(17) . . ? C3 N1 C1 107.3(2) . . ? C3 N1 C9 127.4(2) . . ? C1 N1 C9 125.2(2) . . ? C19 N4 C17 106.7(3) . . ? C19 N4 C16 130.5(3) . . ? C17 N4 C16 122.7(3) . . ? O1 C25 O2 121.7(2) . . ? O1 C25 C26 119.5(2) . . ? O2 C25 C26 118.7(2) . . ? O1 C25 Cd1 64.50(13) . . ? O2 C25 Cd1 57.43(12) . . ? C26 C25 Cd1 173.65(17) . . ? N3 C4 C5 120.6(2) . . ? N3 C4 C3 112.5(2) . . ? C5 C4 C3 126.8(2) . . ? C6 C5 C4 118.9(3) . . ? C6 C5 H5 120.6 . . ? C4 C5 H5 120.6 . . ? C29 C28 C27 119.0(2) . . ? C29 C28 H28 120.5 . . ? C27 C28 H28 120.5 . . ? C28 C29 O3 115.4(2) . . ? C28 C29 C30 121.3(2) . . ? O3 C29 C30 123.3(2) . . ? C31 C26 C27 119.0(2) . . ? C31 C26 C25 120.3(2) . . ? C27 C26 C25 120.7(2) . . ? C2 C1 N1 106.6(2) . . ? C2 C1 H1 126.7 . . ? N1 C1 H1 126.7 . . ? N2 C3 N1 109.6(2) . . ? N2 C3 C4 121.1(2) . . ? N1 C3 C4 129.2(2) . . ? C24 C23 C22 119.2(3) . . ? C24 C23 H23 120.4 . . ? C22 C23 H23 120.4 . . ? C6 C7 C8 117.8(3) . . ? C6 C7 H7 121.1 . . ? C8 C7 H7 121.1 . . ? C1 C2 N2 109.7(2) . . ? C1 C2 H2 125.2 . . ? N2 C2 H2 125.2 . . ? C14 C15 C10 118.5(3) . . ? C14 C15 C16 120.6(3) . . ? C10 C15 C16 120.9(2) . . ? C31 C30 C29 118.6(2) . . ? C31 C30 H30 120.7 . . ? C29 C30 H30 120.7 . . ? C20 N6 C22 117.2(3) . . ? C28 C27 C26 120.8(2) . . ? C28 C27 H27 119.6 . . ? C26 C27 H27 119.6 . . ? N6 C20 C21 122.8(3) . . ? N6 C20 C19 117.9(3) . . ? C21 C20 C19 119.3(3) . . ? C30 C31 C26 121.2(2) . . ? C30 C31 H31 119.4 . . ? C26 C31 H31 119.4 . . ? N4 C16 C15 114.0(2) . . ? N4 C16 H16A 108.7 . . ? C15 C16 H16A 108.7 . . ? N4 C16 H16B 108.7 . . ? C15 C16 H16B 108.7 . . ? H16A C16 H16B 107.6 . . ? N3 C8 C7 123.3(3) . . ? N3 C8 H8 118.3 . . ? C7 C8 H8 118.3 . . ? N5 C19 N4 110.3(3) . . ? N5 C19 C20 123.0(3) . . ? N4 C19 C20 126.6(3) . . ? N1 C9 C10 114.8(2) . . ? N1 C9 H9A 108.6 . . ? C10 C9 H9A 108.6 . . ? N1 C9 H9B 108.6 . . ? C10 C9 H9B 108.6 . . ? H9A C9 H9B 107.5 . . ? C11 C10 C15 119.4(3) . . ? C11 C10 C9 117.8(3) . . ? C15 C10 C9 122.5(3) . . ? C7 C6 C5 120.2(3) . . ? C7 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C12 C11 C10 121.3(3) . . ? C12 C11 H11 119.4 . . ? C10 C11 H11 119.4 . . ? N6 C22 C23 123.1(4) . . ? N6 C22 H22 118.5 . . ? C23 C22 H22 118.5 . . ? C19 N5 C18 105.5(3) . . ? C13 C14 C15 121.0(3) . . ? C13 C14 H14 119.5 . . ? C15 C14 H14 119.5 . . ? C24 C21 C20 118.7(4) . . ? C24 C21 H21 120.6 . . ? C20 C21 H21 120.6 . . ? C18 C17 N4 106.7(3) . . ? C18 C17 H17 126.7 . . ? N4 C17 H17 126.7 . . ? C23 C24 C21 118.9(4) . . ? C23 C24 H24 120.5 . . ? C21 C24 H24 120.5 . . ? C13 C12 C11 119.5(3) . . ? C13 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? C12 C13 C14 120.3(3) . . ? C12 C13 H13 119.9 . . ? C14 C13 H13 119.9 . . ? C17 C18 N5 110.7(3) . . ? C17 C18 H18 124.6 . . ? N5 C18 H18 124.6 . . ? C32 C33 C34 121.6(2) . . ? C32 C33 O3 119.5(2) . . ? C34 C33 O3 118.8(2) . . ? C33 C32 C35 119.1(3) . . ? C33 C32 H32 120.4 . . ? C35 C32 H32 120.4 . . ? C33 C34 C37 119.1(3) . . ? C33 C34 H34 120.5 . . ? C37 C34 H34 120.5 . . ? C35 C36 C37 118.9(2) . . ? C35 C36 C38 121.2(2) . . ? C37 C36 C38 119.8(2) . . ? C36 C35 C32 120.6(2) . . ? C36 C35 H35 119.7 . . ? C32 C35 H35 119.7 . . ? C36 C37 C34 120.6(3) . . ? C36 C37 H37 119.7 . . ? C34 C37 H37 119.7 . . ? C38 O5 Cd1 162.53(17) . 2_557 ? C38 O5 Cd1 91.72(15) . 1_556 ? Cd1 O5 Cd1 104.65(6) 2_557 1_556 ? C38 O4 Cd1 94.52(15) . 1_556 ? O4 C38 O5 120.4(2) . . ? O4 C38 C36 119.0(2) . . ? O5 C38 C36 120.5(2) . . ? H2B O2W H2A 114(5) . . ? H1B O1W H1A 116(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 N2 Cd1 O2 C25 2.5(4) . . . . ? N3 Cd1 O2 C25 -69.48(17) . . . . ? O4 Cd1 O2 C25 -146.48(16) 1_554 . . . ? O5 Cd1 O2 C25 85.69(16) 2_557 . . . ? O1 Cd1 O2 C25 -2.71(14) . . . . ? O5 Cd1 O2 C25 160.91(16) 1_554 . . . ? N2 Cd1 O1 C25 -175.94(14) . . . . ? O2 Cd1 O1 C25 2.73(14) . . . . ? N3 Cd1 O1 C25 119.40(15) . . . . ? O4 Cd1 O1 C25 52.43(17) 1_554 . . . ? O5 Cd1 O1 C25 -87.43(15) 2_557 . . . ? O5 Cd1 O1 C25 -27.5(2) 1_554 . . . ? N2 Cd1 N3 C8 -175.8(2) . . . . ? O2 Cd1 N3 C8 -9.7(2) . . . . ? O4 Cd1 N3 C8 73.9(2) 1_554 . . . ? O5 Cd1 N3 C8 -129.0(2) 2_557 . . . ? O1 Cd1 N3 C8 -59.4(2) . . . . ? O5 Cd1 N3 C8 98.5(2) 1_554 . . . ? C25 Cd1 N3 C8 -35.6(2) . . . . ? N2 Cd1 N3 C4 6.18(17) . . . . ? O2 Cd1 N3 C4 172.28(17) . . . . ? O4 Cd1 N3 C4 -104.06(18) 1_554 . . . ? O5 Cd1 N3 C4 53.0(2) 2_557 . . . ? O1 Cd1 N3 C4 122.61(18) . . . . ? O5 Cd1 N3 C4 -79.49(19) 1_554 . . . ? C25 Cd1 N3 C4 146.40(18) . . . . ? O2 Cd1 N2 C3 -83.9(4) . . . . ? N3 Cd1 N2 C3 -7.56(18) . . . . ? O4 Cd1 N2 C3 64.1(2) 1_554 . . . ? O5 Cd1 N2 C3 -167.00(19) 2_557 . . . ? O1 Cd1 N2 C3 -79.26(19) . . . . ? O5 Cd1 N2 C3 117.91(19) 1_554 . . . ? C25 Cd1 N2 C3 -82.1(2) . . . . ? O2 Cd1 N2 C2 104.1(4) . . . . ? N3 Cd1 N2 C2 -179.6(3) . . . . ? O4 Cd1 N2 C2 -108.0(3) 1_554 . . . ? O5 Cd1 N2 C2 21.0(3) 2_557 . . . ? O1 Cd1 N2 C2 108.7(3) . . . . ? O5 Cd1 N2 C2 -54.1(3) 1_554 . . . ? C25 Cd1 N2 C2 105.9(3) . . . . ? Cd1 O1 C25 O2 -4.8(2) . . . . ? Cd1 O1 C25 C26 174.5(2) . . . . ? Cd1 O2 C25 O1 5.1(3) . . . . ? Cd1 O2 C25 C26 -174.13(19) . . . . ? N2 Cd1 C25 O1 5.7(2) . . . . ? O2 Cd1 C25 O1 -175.2(2) . . . . ? N3 Cd1 C25 O1 -59.81(15) . . . . ? O4 Cd1 C25 O1 -139.20(14) 1_554 . . . ? O5 Cd1 C25 O1 91.43(14) 2_557 . . . ? O5 Cd1 C25 O1 162.58(13) 1_554 . . . ? N2 Cd1 C25 O2 -179.09(14) . . . . ? N3 Cd1 C25 O2 115.37(16) . . . . ? O4 Cd1 C25 O2 35.98(17) 1_554 . . . ? O5 Cd1 C25 O2 -93.39(16) 2_557 . . . ? O1 Cd1 C25 O2 175.2(2) . . . . ? O5 Cd1 C25 O2 -22.24(18) 1_554 . . . ? C8 N3 C4 C5 0.3(4) . . . . ? Cd1 N3 C4 C5 178.4(2) . . . . ? C8 N3 C4 C3 177.9(2) . . . . ? Cd1 N3 C4 C3 -4.0(3) . . . . ? N3 C4 C5 C6 -0.3(4) . . . . ? C3 C4 C5 C6 -177.6(3) . . . . ? C27 C28 C29 O3 -176.6(2) . . . . ? C27 C28 C29 C30 2.1(4) . . . . ? C33 O3 C29 C28 178.1(2) . . . . ? C33 O3 C29 C30 -0.6(4) . . . . ? O1 C25 C26 C31 -8.1(4) . . . . ? O2 C25 C26 C31 171.2(2) . . . . ? O1 C25 C26 C27 172.6(2) . . . . ? O2 C25 C26 C27 -8.2(4) . . . . ? C3 N1 C1 C2 0.9(3) . . . . ? C9 N1 C1 C2 -175.9(3) . . . . ? C2 N2 C3 N1 0.1(3) . . . . ? Cd1 N2 C3 N1 -174.00(16) . . . . ? C2 N2 C3 C4 -177.1(2) . . . . ? Cd1 N2 C3 C4 8.8(3) . . . . ? C1 N1 C3 N2 -0.6(3) . . . . ? C9 N1 C3 N2 176.0(3) . . . . ? C1 N1 C3 C4 176.2(3) . . . . ? C9 N1 C3 C4 -7.1(4) . . . . ? N3 C4 C3 N2 -3.0(3) . . . . ? C5 C4 C3 N2 174.5(3) . . . . ? N3 C4 C3 N1 -179.5(2) . . . . ? C5 C4 C3 N1 -2.1(4) . . . . ? N1 C1 C2 N2 -0.8(4) . . . . ? C3 N2 C2 C1 0.5(3) . . . . ? Cd1 N2 C2 C1 173.1(2) . . . . ? C28 C29 C30 C31 -1.2(4) . . . . ? O3 C29 C30 C31 177.4(3) . . . . ? C29 C28 C27 C26 -1.0(4) . . . . ? C31 C26 C27 C28 -1.0(4) . . . . ? C25 C26 C27 C28 178.4(2) . . . . ? C22 N6 C20 C21 0.5(5) . . . . ? C22 N6 C20 C19 -178.3(3) . . . . ? C29 C30 C31 C26 -0.9(4) . . . . ? C27 C26 C31 C30 1.9(4) . . . . ? C25 C26 C31 C30 -177.4(2) . . . . ? C19 N4 C16 C15 -82.7(4) . . . . ? C17 N4 C16 C15 94.6(4) . . . . ? C14 C15 C16 N4 -22.8(4) . . . . ? C10 C15 C16 N4 160.9(3) . . . . ? C4 N3 C8 C7 0.1(4) . . . . ? Cd1 N3 C8 C7 -177.9(2) . . . . ? C6 C7 C8 N3 -0.4(5) . . . . ? C17 N4 C19 N5 -0.4(4) . . . . ? C16 N4 C19 N5 177.2(3) . . . . ? C17 N4 C19 C20 177.9(3) . . . . ? C16 N4 C19 C20 -4.4(5) . . . . ? N6 C20 C19 N5 177.1(3) . . . . ? C21 C20 C19 N5 -1.8(5) . . . . ? N6 C20 C19 N4 -1.1(5) . . . . ? C21 C20 C19 N4 -180.0(3) . . . . ? C3 N1 C9 C10 -178.8(3) . . . . ? C1 N1 C9 C10 -2.8(4) . . . . ? C14 C15 C10 C11 -2.2(4) . . . . ? C16 C15 C10 C11 174.1(3) . . . . ? C14 C15 C10 C9 171.3(3) . . . . ? C16 C15 C10 C9 -12.4(4) . . . . ? N1 C9 C10 C11 -108.1(3) . . . . ? N1 C9 C10 C15 78.3(4) . . . . ? C8 C7 C6 C5 0.4(5) . . . . ? C4 C5 C6 C7 -0.1(5) . . . . ? C15 C10 C11 C12 2.2(5) . . . . ? C9 C10 C11 C12 -171.5(3) . . . . ? C20 N6 C22 C23 -0.6(5) . . . . ? C24 C23 C22 N6 -0.1(6) . . . . ? N4 C19 N5 C18 0.6(4) . . . . ? C20 C19 N5 C18 -177.9(3) . . . . ? C10 C15 C14 C13 0.6(5) . . . . ? C16 C15 C14 C13 -175.7(3) . . . . ? N6 C20 C21 C24 0.2(5) . . . . ? C19 C20 C21 C24 179.1(3) . . . . ? C19 N4 C17 C18 0.1(4) . . . . ? C16 N4 C17 C18 -177.8(3) . . . . ? C22 C23 C24 C21 0.9(6) . . . . ? C20 C21 C24 C23 -0.9(6) . . . . ? C10 C11 C12 C13 -0.6(6) . . . . ? C11 C12 C13 C14 -1.0(6) . . . . ? C15 C14 C13 C12 1.0(6) . . . . ? N4 C17 C18 N5 0.3(5) . . . . ? C19 N5 C18 C17 -0.5(5) . . . . ? C29 O3 C33 C32 -90.6(3) . . . . ? C29 O3 C33 C34 92.9(3) . . . . ? C34 C33 C32 C35 0.2(4) . . . . ? O3 C33 C32 C35 -176.2(2) . . . . ? C32 C33 C34 C37 -1.4(4) . . . . ? O3 C33 C34 C37 175.1(3) . . . . ? C37 C36 C35 C32 -1.2(4) . . . . ? C38 C36 C35 C32 -177.7(2) . . . . ? C33 C32 C35 C36 1.1(4) . . . . ? C35 C36 C37 C34 0.0(4) . . . . ? C38 C36 C37 C34 176.6(3) . . . . ? C33 C34 C37 C36 1.3(5) . . . . ? Cd1 O4 C38 O5 5.4(3) 1_556 . . . ? Cd1 O4 C38 C36 -172.12(18) 1_556 . . . ? Cd1 O5 C38 O4 154.5(5) 2_557 . . . ? Cd1 O5 C38 O4 -5.2(2) 1_556 . . . ? Cd1 O5 C38 C36 -28.1(7) 2_557 . . . ? Cd1 O5 C38 C36 172.21(19) 1_556 . . . ? C35 C36 C38 O4 178.1(2) . . . . ? C37 C36 C38 O4 1.6(4) . . . . ? C35 C36 C38 O5 0.6(4) . . . . ? C37 C36 C38 O5 -175.8(2) . . . . ? 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 O1W H1A N5 0.81(4) 2.22(3) 2.950(5) 151(5) 2_655 O1W H1B O4 0.81(4) 2.08(4) 2.870(3) 163(5) 1_554 O2W H2A O1W 0.82(4) 2.00(5) 2.804(5) 167(5) . O2W H2B O3W 0.81(4) 2.26(3) 2.958(9) 144(4) . _diffrn_measured_fraction_theta_max 0.915 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.963 _refine_diff_density_min -0.555 _refine_diff_density_rms 0.062