# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Arjan Kleij' _publ_contact_author_email AKLEIJ@ICIQ.ES _publ_section_title ; Self-assembly of Zn(salphen) complexes: Steric regulation, stability studies and crystallographic analysis revealing an unexpected dimeric 3,3'-t-Bu-substituted Zn(salphen) complex ; loop_ _publ_author_name 'Arjan Kleij' 'Daniele Anselmo' 'Jordi Benet-Buchholz' 'Eduardo C. Escudero-Adan' 'Robert M. Haak' ; M.M.Belmonte ; 'Sander J. Wezenberg' # Attachment 'DA111_0mX1.cif' data_da111_0m _database_code_depnum_ccdc_archive 'CCDC 755295' #TrackingRef 'DA111_0mX1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H63 N5 O4 Zn2' _chemical_formula_weight 1024.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.5175(7) _cell_length_b 13.5978(9) _cell_length_c 16.0896(11) _cell_angle_alpha 94.283(2) _cell_angle_beta 91.422(2) _cell_angle_gamma 97.6590(10) _cell_volume 2488.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6909 _cell_measurement_theta_min 3.03 _cell_measurement_theta_max 36.50 _exptl_crystal_description Block _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.368 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1076 _exptl_absorpt_coefficient_mu 1.017 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9152 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_process_details ; SADABS Version 2008/1 Bruker-Nonius Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_special_details ; It should be noted that the esd's of the cell dimensions are probably too low; they should be multiplied by a factor of 2 to 10 ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_specimen_suppport 'magnetic support whith 10 micron nylon fiber cryoloop' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'rotating anode X-ray tube' _diffrn_source_type 'Bruker-Nonius FR 591' _diffrn_source_power 50 _diffrn_source_current 70 _diffrn_source_size '3 mm x 0.3 mm fine focus' _diffrn_radiation_monochromator 'Multilayer Montel 200 mirrors' _diffrn_detector_type '4K CCD area detector APEX II' _diffrn_measurement_device_type 'Kappa 4-axis goniometer bruker-nonius' _diffrn_measurement_method ; Fullsphere data collection, phi and omega scans ; _diffrn_detector_area_resol_mean 512 _diffrn_reflns_number 54401 _diffrn_reflns_av_R_equivalents 0.0346 _diffrn_reflns_av_sigmaI/netI 0.0437 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.88 _diffrn_reflns_theta_max 36.62 _reflns_number_total 23200 _reflns_number_gt 18247 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v2009.1-0' _computing_cell_refinement 'Bruker APEX2 v2009.1-0' _computing_data_reduction 'Bruker SAINT V7.60A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXS-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0673P)^2^+0.2658P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 23200 _refine_ls_number_parameters 648 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0549 _refine_ls_R_factor_gt 0.0400 _refine_ls_wR_factor_ref 0.1167 _refine_ls_wR_factor_gt 0.1086 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _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 C1A C 0.11800(9) 0.64999(8) 0.01860(7) 0.01813(17) Uani 1 1 d . A . C2A C 0.09658(10) 0.70872(9) -0.04989(8) 0.02026(19) Uani 1 1 d . . . C3A C 0.09858(11) 0.66587(10) -0.13083(8) 0.0244(2) Uani 1 1 d . . . H3A H 0.0872 0.7057 -0.1756 0.029 Uiso 1 1 calc R . . C4A C 0.11655(11) 0.56685(10) -0.15001(8) 0.0249(2) Uani 1 1 d . . . H4A H 0.1168 0.5403 -0.2063 0.030 Uiso 1 1 calc R . . C5A C 0.13378(10) 0.50898(9) -0.08535(8) 0.0220(2) Uani 1 1 d . . . H5A H 0.1434 0.4411 -0.0973 0.026 Uiso 1 1 calc R . . C6A C 0.13731(9) 0.54880(8) -0.00178(7) 0.01846(18) Uani 1 1 d . . . C7A C 0.15625(9) 0.48076(8) 0.06004(7) 0.01842(18) Uani 1 1 d . A . H7A H 0.1504 0.4122 0.0416 0.022 Uiso 1 1 calc R . . C8A C 0.06995(12) 0.81608(9) -0.03269(9) 0.0252(2) Uani 1 1 d . . . C9A C 0.16902(13) 0.87993(10) 0.02070(10) 0.0312(3) Uani 1 1 d . . . H9A1 H 0.1527 0.9490 0.0271 0.047 Uiso 1 1 calc R . . H9A2 H 0.2437 0.8775 -0.0068 0.047 Uiso 1 1 calc R . . H9A3 H 0.1737 0.8540 0.0757 0.047 Uiso 1 1 calc R . . C10A C -0.04852(12) 0.81299(10) 0.01056(10) 0.0284(2) Uani 1 1 d . . . H10A H -0.0465 0.7750 0.0599 0.043 Uiso 1 1 calc R . . H10B H -0.1116 0.7810 -0.0283 0.043 Uiso 1 1 calc R . . H10C H -0.0626 0.8810 0.0275 0.043 Uiso 1 1 calc R . . C11A C 0.05667(17) 0.86719(11) -0.11385(11) 0.0375(3) Uani 1 1 d . . . H11A H 0.0393 0.9351 -0.1005 0.056 Uiso 1 1 calc R . . H11B H -0.0075 0.8295 -0.1488 0.056 Uiso 1 1 calc R . . H11C H 0.1298 0.8695 -0.1440 0.056 Uiso 1 1 calc R . . C12A C 0.19223(9) 0.43164(8) 0.19467(7) 0.01757(17) Uani 1 1 d . A . C13A C 0.23475(10) 0.34190(8) 0.17430(8) 0.0216(2) Uani 1 1 d . . . H13A H 0.2549 0.3251 0.1186 0.026 Uiso 1 1 calc R . . C14A C 0.24765(11) 0.27695(9) 0.23573(9) 0.0250(2) Uani 1 1 d . . . H14A H 0.2757 0.2155 0.2216 0.030 Uiso 1 1 calc R . . C15A C 0.21978(12) 0.30122(9) 0.31756(9) 0.0271(2) Uani 1 1 d . . . H15A H 0.2292 0.2565 0.3591 0.032 Uiso 1 1 calc R . . C16A C 0.17803(11) 0.39089(9) 0.33882(8) 0.0238(2) Uani 1 1 d . . . H16A H 0.1596 0.4077 0.3949 0.029 Uiso 1 1 calc R . . C17A C 0.16320(9) 0.45637(8) 0.27736(7) 0.01792(17) Uani 1 1 d . A . C18A C 0.07389(9) 0.57566(8) 0.35855(8) 0.01925(18) Uani 1 1 d . A . H18A H 0.0510 0.5241 0.3939 0.023 Uiso 1 1 calc R . . C19A C 0.04202(10) 0.67334(8) 0.38274(7) 0.01963(19) Uani 1 1 d . . . C20A C -0.02399(15) 0.68043(14) 0.45476(11) 0.0216(4) Uani 0.829(10) 1 d PD A 1 H20A H -0.0439 0.6230 0.4844 0.026 Uiso 0.829(10) 1 calc PR A 1 C21A C -0.06032(17) 0.76903(18) 0.48325(14) 0.0230(4) Uani 0.829(10) 1 d PD A 1 H21A H -0.0986 0.7748 0.5347 0.028 Uiso 0.829(10) 1 calc PR A 1 C22A C -0.03959(17) 0.85018(16) 0.43485(14) 0.0209(4) Uani 0.829(10) 1 d PD A 1 H22A H -0.0687 0.9101 0.4528 0.025 Uiso 0.829(10) 1 calc PR A 1 C20' C -0.04301(17) 0.66329(16) 0.44845(14) 0.047(3) Uani 0.171(10) 1 d PRD A 2 H20' H -0.0642 0.6026 0.4734 0.057 Uiso 0.171(10) 1 calc PR A 2 C21' C -0.0901(19) 0.7491(11) 0.4714(12) 0.047(3) Uani 0.171(10) 1 d PD A 2 H21' H -0.1382 0.7512 0.5185 0.057 Uiso 0.171(10) 1 calc PR A 2 C22' C -0.0682(19) 0.8308(12) 0.4273(12) 0.047(3) Uani 0.171(10) 1 d PD A 2 H22' H -0.1144 0.8827 0.4390 0.057 Uiso 0.171(10) 1 calc PR A 2 C23A C 0.02156(10) 0.84707(9) 0.36180(8) 0.02040(19) Uani 1 1 d . . . C24A C 0.07529(9) 0.75996(8) 0.33999(7) 0.01761(17) Uani 1 1 d . A . C25A C 0.02442(10) 0.93218(9) 0.30435(8) 0.0216(2) Uani 1 1 d . A . C26A C -0.05275(14) 1.01043(11) 0.33504(10) 0.0324(3) Uani 1 1 d . . . H26A H -0.1325 0.9778 0.3427 0.049 Uiso 1 1 calc R A . H26B H -0.0548 1.0597 0.2938 0.049 Uiso 1 1 calc R . . H26C H -0.0202 1.0438 0.3883 0.049 Uiso 1 1 calc R . . C27A C -0.02553(13) 0.88707(10) 0.21805(9) 0.0294(3) Uani 1 1 d . . . H27A H 0.0228 0.8376 0.1962 0.044 Uiso 1 1 calc R A . H27B H -0.0250 0.9399 0.1798 0.044 Uiso 1 1 calc R . . H27C H -0.1061 0.8550 0.2233 0.044 Uiso 1 1 calc R . . C28A C 0.14787(13) 0.98717(11) 0.29436(12) 0.0351(3) Uani 1 1 d . . . H28A H 0.1816 1.0140 0.3492 0.053 Uiso 1 1 calc R A . H28B H 0.1434 1.0419 0.2586 0.053 Uiso 1 1 calc R . . H28C H 0.1975 0.9408 0.2689 0.053 Uiso 1 1 calc R . . C1B C 0.43262(9) 0.62386(8) 0.22565(8) 0.01814(18) Uani 1 1 d . A . C2B C 0.50355(10) 0.60845(9) 0.15540(8) 0.0211(2) Uani 1 1 d . . . C3B C 0.56705(11) 0.52759(9) 0.15408(10) 0.0265(2) Uani 1 1 d . . . H3B H 0.6125 0.5152 0.1069 0.032 Uiso 1 1 calc R . . C4B C 0.56719(11) 0.46418(9) 0.21839(10) 0.0286(3) Uani 1 1 d . . . H4B H 0.6082 0.4080 0.2134 0.034 Uiso 1 1 calc R . . C5B C 0.50712(10) 0.48426(9) 0.28909(10) 0.0255(2) Uani 1 1 d . . . H5B H 0.5097 0.4436 0.3344 0.031 Uiso 1 1 calc R . . C6B C 0.44161(9) 0.56499(8) 0.29457(8) 0.02034(19) Uani 1 1 d . . . C7B C 0.39282(10) 0.58440(9) 0.37545(8) 0.0211(2) Uani 1 1 d . . . H7B H 0.3971 0.5361 0.4147 0.025 Uiso 1 1 calc R . . C8B C 0.51744(10) 0.68140(9) 0.08673(8) 0.0229(2) Uani 1 1 d . . . C9B C 0.56567(13) 0.78559(10) 0.12722(10) 0.0301(3) Uani 1 1 d . . . H9B1 H 0.5677 0.8342 0.0851 0.045 Uiso 1 1 calc R . . H9B2 H 0.6451 0.7848 0.1502 0.045 Uiso 1 1 calc R . . H9B3 H 0.5148 0.8040 0.1721 0.045 Uiso 1 1 calc R . . C10B C 0.40174(12) 0.68478(12) 0.03990(9) 0.0316(3) Uani 1 1 d . . . H10D H 0.3700 0.6176 0.0167 0.047 Uiso 1 1 calc R . . H10E H 0.4148 0.7288 -0.0054 0.047 Uiso 1 1 calc R . . H10F H 0.3459 0.7101 0.0783 0.047 Uiso 1 1 calc R . . C11B C 0.60527(13) 0.65336(12) 0.02162(10) 0.0335(3) Uani 1 1 d . . . H11D H 0.5782 0.5867 -0.0048 0.050 Uiso 1 1 calc R . . H11E H 0.6823 0.6538 0.0491 0.050 Uiso 1 1 calc R . . H11F H 0.6113 0.7016 -0.0209 0.050 Uiso 1 1 calc R . . C12B C 0.29692(10) 0.67318(9) 0.47894(8) 0.0219(2) Uani 1 1 d . . . C13B C 0.26630(12) 0.59563(11) 0.52995(9) 0.0279(2) Uani 1 1 d . . . H13B H 0.2813 0.5302 0.5132 0.034 Uiso 1 1 calc R . . C14B C 0.21375(14) 0.61453(13) 0.60538(10) 0.0351(3) Uani 1 1 d . . . H14B H 0.1941 0.5619 0.6403 0.042 Uiso 1 1 calc R . . C15B C 0.18988(14) 0.70923(14) 0.63011(10) 0.0368(3) Uani 1 1 d . . . H15B H 0.1530 0.7211 0.6814 0.044 Uiso 1 1 calc R . . C16B C 0.21992(13) 0.78716(12) 0.57993(9) 0.0303(3) Uani 1 1 d . . . H16B H 0.2027 0.8520 0.5967 0.036 Uiso 1 1 calc R . . C17B C 0.27540(10) 0.77005(10) 0.50493(8) 0.0231(2) Uani 1 1 d . . . C18B C 0.34363(11) 0.93493(9) 0.47729(9) 0.0246(2) Uani 1 1 d . . . H18B H 0.3373 0.9517 0.5352 0.030 Uiso 1 1 calc R . . C19B C 0.38957(11) 1.01341(9) 0.42702(9) 0.0252(2) Uani 1 1 d . . . C20B C 0.39799(12) 1.11060(10) 0.46693(11) 0.0307(3) Uani 1 1 d . . . H20B H 0.3729 1.1198 0.5225 0.037 Uiso 1 1 calc R . . C21B C 0.44228(13) 1.19198(10) 0.42578(12) 0.0341(3) Uani 1 1 d . . . H21B H 0.4459 1.2574 0.4519 0.041 Uiso 1 1 calc R . . C22B C 0.48178(12) 1.17688(10) 0.34519(11) 0.0315(3) Uani 1 1 d . . . H22B H 0.5124 1.2336 0.3176 0.038 Uiso 1 1 calc R . . C23B C 0.47884(11) 1.08343(9) 0.30286(10) 0.0260(2) Uani 1 1 d . . . C24B C 0.42974(10) 0.99754(9) 0.34418(9) 0.0226(2) Uani 1 1 d . A . C25B C 0.52855(12) 1.07236(10) 0.21592(10) 0.0284(3) Uani 1 1 d . . . C26B C 0.57218(16) 1.17347(11) 0.18260(13) 0.0404(4) Uani 1 1 d . . . H26D H 0.5065 1.2119 0.1779 0.061 Uiso 1 1 calc R . . H26E H 0.6051 1.1626 0.1276 0.061 Uiso 1 1 calc R . . H26F H 0.6328 1.2103 0.2211 0.061 Uiso 1 1 calc R . . C27B C 0.63552(12) 1.01536(11) 0.22135(11) 0.0309(3) Uani 1 1 d . . . H27D H 0.6966 1.0543 0.2583 0.046 Uiso 1 1 calc R . . H27E H 0.6662 1.0047 0.1656 0.046 Uiso 1 1 calc R . . H27F H 0.6117 0.9509 0.2437 0.046 Uiso 1 1 calc R . . C28B C 0.43425(13) 1.01844(11) 0.15260(10) 0.0317(3) Uani 1 1 d . . . H28D H 0.4056 0.9526 0.1707 0.048 Uiso 1 1 calc R . . H28E H 0.4683 1.0109 0.0976 0.048 Uiso 1 1 calc R . . H28F H 0.3689 1.0575 0.1492 0.048 Uiso 1 1 calc R . . C1S C 0.68361(14) 0.66165(12) 0.40201(12) 0.0375(3) Uani 1 1 d . . . C2S C 0.7140(2) 0.70758(19) 0.32514(15) 0.0602(6) Uani 1 1 d . . . H2S1 H 0.6967 0.6579 0.2776 0.090 Uiso 1 1 calc R . . H2S2 H 0.7978 0.7333 0.3273 0.090 Uiso 1 1 calc R . . H2S3 H 0.6681 0.7624 0.3187 0.090 Uiso 1 1 calc R . . N1 N 0.13057(8) 0.55280(7) 0.29322(6) 0.01767(16) Uani 1 1 d . . . N2 N 0.18048(8) 0.50473(7) 0.13835(6) 0.01787(16) Uani 1 1 d . . . N1B N 0.34390(8) 0.66186(7) 0.39876(7) 0.01974(17) Uani 1 1 d . . . N2B N 0.31020(9) 0.84319(8) 0.44973(7) 0.02178(17) Uani 1 1 d . . . N1S N 0.65926(13) 0.62532(11) 0.46146(11) 0.0392(3) Uani 1 1 d . . . O3 O 0.11621(8) 0.68909(6) 0.09497(5) 0.01987(14) Uani 1 1 d . . . O6 O 0.15616(7) 0.76084(6) 0.28168(5) 0.01697(13) Uani 1 1 d . . . O1B O 0.35848(7) 0.69251(6) 0.22686(6) 0.01766(14) Uani 1 1 d . . . O2B O 0.42548(8) 0.90881(6) 0.30562(6) 0.02338(16) Uani 1 1 d . . . Zn1 Zn 0.181714(11) 0.645848(9) 0.196448(8) 0.01564(3) Uani 1 1 d . A . Zn2 Zn 0.329744(11) 0.785631(9) 0.328706(9) 0.01708(3) Uani 1 1 d . A . 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 C1A 0.0185(4) 0.0198(4) 0.0171(4) 0.0042(3) 0.0025(3) 0.0042(3) C2A 0.0211(4) 0.0222(5) 0.0183(5) 0.0066(4) 0.0013(4) 0.0030(4) C3A 0.0247(5) 0.0316(6) 0.0181(5) 0.0073(4) 0.0030(4) 0.0051(4) C4A 0.0252(5) 0.0344(6) 0.0163(5) 0.0016(4) 0.0037(4) 0.0079(4) C5A 0.0202(4) 0.0289(5) 0.0179(5) -0.0001(4) 0.0036(4) 0.0078(4) C6A 0.0186(4) 0.0205(4) 0.0173(5) 0.0025(3) 0.0033(3) 0.0054(3) C7A 0.0195(4) 0.0180(4) 0.0188(5) 0.0012(3) 0.0036(4) 0.0061(3) C8A 0.0317(6) 0.0202(5) 0.0244(6) 0.0076(4) -0.0026(4) 0.0034(4) C9A 0.0371(7) 0.0229(5) 0.0320(7) 0.0059(5) -0.0042(5) -0.0027(5) C10A 0.0328(6) 0.0219(5) 0.0322(7) 0.0013(4) -0.0023(5) 0.0109(4) C11A 0.0565(9) 0.0276(6) 0.0290(7) 0.0128(5) -0.0064(6) 0.0042(6) C12A 0.0187(4) 0.0160(4) 0.0189(5) 0.0035(3) 0.0035(3) 0.0041(3) C13A 0.0246(5) 0.0192(4) 0.0226(5) 0.0034(4) 0.0049(4) 0.0074(4) C14A 0.0293(5) 0.0195(5) 0.0290(6) 0.0071(4) 0.0071(5) 0.0091(4) C15A 0.0329(6) 0.0232(5) 0.0292(6) 0.0118(4) 0.0098(5) 0.0115(4) C16A 0.0296(5) 0.0227(5) 0.0222(5) 0.0094(4) 0.0089(4) 0.0089(4) C17A 0.0190(4) 0.0165(4) 0.0195(5) 0.0047(3) 0.0045(3) 0.0044(3) C18A 0.0183(4) 0.0213(4) 0.0198(5) 0.0062(4) 0.0052(4) 0.0053(3) C19A 0.0195(4) 0.0231(5) 0.0186(5) 0.0047(4) 0.0065(4) 0.0085(4) C20A 0.0204(7) 0.0259(7) 0.0197(7) 0.0053(5) 0.0068(5) 0.0045(5) C21A 0.0209(7) 0.0298(8) 0.0187(7) -0.0002(6) 0.0067(6) 0.0050(6) C22A 0.0196(7) 0.0235(8) 0.0203(7) -0.0022(5) 0.0035(6) 0.0068(5) C20' 0.067(6) 0.037(4) 0.051(6) 0.024(3) 0.050(5) 0.037(4) C21' 0.067(6) 0.037(4) 0.051(6) 0.024(3) 0.050(5) 0.037(4) C22' 0.067(6) 0.037(4) 0.051(6) 0.024(3) 0.050(5) 0.037(4) C23A 0.0213(4) 0.0230(5) 0.0190(5) 0.0011(4) 0.0027(4) 0.0107(4) C24A 0.0184(4) 0.0205(4) 0.0157(4) 0.0026(3) 0.0041(3) 0.0081(3) C25A 0.0231(5) 0.0205(5) 0.0234(5) 0.0020(4) 0.0007(4) 0.0106(4) C26A 0.0381(7) 0.0301(6) 0.0327(7) -0.0002(5) 0.0010(6) 0.0198(5) C27A 0.0397(7) 0.0260(6) 0.0243(6) 0.0028(4) -0.0032(5) 0.0121(5) C28A 0.0288(6) 0.0251(6) 0.0532(10) 0.0086(6) 0.0001(6) 0.0076(5) C1B 0.0154(4) 0.0169(4) 0.0228(5) 0.0014(3) 0.0043(3) 0.0041(3) C2B 0.0182(4) 0.0206(5) 0.0251(5) -0.0009(4) 0.0066(4) 0.0046(3) C3B 0.0211(5) 0.0231(5) 0.0359(7) -0.0033(5) 0.0079(5) 0.0068(4) C4B 0.0256(5) 0.0195(5) 0.0425(8) -0.0002(5) 0.0056(5) 0.0098(4) C5B 0.0216(5) 0.0184(5) 0.0381(7) 0.0047(4) 0.0028(5) 0.0071(4) C6B 0.0174(4) 0.0175(4) 0.0276(6) 0.0047(4) 0.0039(4) 0.0056(3) C7B 0.0186(4) 0.0207(4) 0.0254(5) 0.0068(4) 0.0019(4) 0.0054(3) C8B 0.0191(4) 0.0264(5) 0.0239(5) 0.0013(4) 0.0084(4) 0.0045(4) C9B 0.0316(6) 0.0262(6) 0.0325(7) 0.0043(5) 0.0107(5) 0.0013(5) C10B 0.0251(5) 0.0478(8) 0.0235(6) 0.0077(5) 0.0067(5) 0.0071(5) C11B 0.0286(6) 0.0421(8) 0.0310(7) 0.0017(6) 0.0150(5) 0.0077(5) C12B 0.0205(4) 0.0276(5) 0.0184(5) 0.0056(4) 0.0017(4) 0.0039(4) C13B 0.0290(5) 0.0337(6) 0.0220(6) 0.0096(5) 0.0022(4) 0.0036(5) C14B 0.0383(7) 0.0452(8) 0.0219(6) 0.0111(6) 0.0051(5) 0.0007(6) C15B 0.0378(7) 0.0526(9) 0.0198(6) 0.0031(6) 0.0083(5) 0.0040(6) C16B 0.0317(6) 0.0392(7) 0.0194(6) -0.0021(5) 0.0040(5) 0.0048(5) C17B 0.0224(5) 0.0290(5) 0.0180(5) 0.0017(4) 0.0012(4) 0.0043(4) C18B 0.0242(5) 0.0263(5) 0.0236(6) -0.0030(4) -0.0007(4) 0.0070(4) C19B 0.0239(5) 0.0215(5) 0.0300(6) -0.0021(4) -0.0026(4) 0.0058(4) C20B 0.0291(6) 0.0261(6) 0.0362(7) -0.0074(5) -0.0062(5) 0.0081(4) C21B 0.0338(6) 0.0197(5) 0.0478(9) -0.0061(5) -0.0098(6) 0.0067(5) C22B 0.0294(6) 0.0192(5) 0.0456(9) 0.0019(5) -0.0068(6) 0.0039(4) C23B 0.0227(5) 0.0190(5) 0.0361(7) 0.0038(4) -0.0042(5) 0.0027(4) C24B 0.0201(4) 0.0195(4) 0.0281(6) 0.0015(4) -0.0029(4) 0.0031(4) C25B 0.0276(5) 0.0215(5) 0.0364(7) 0.0080(5) -0.0006(5) 0.0012(4) C26B 0.0453(8) 0.0248(6) 0.0515(11) 0.0135(6) 0.0033(7) -0.0001(6) C27B 0.0254(5) 0.0280(6) 0.0398(8) 0.0073(5) 0.0029(5) 0.0024(4) C28B 0.0325(6) 0.0303(6) 0.0327(7) 0.0075(5) -0.0016(5) 0.0027(5) C1S 0.0363(7) 0.0346(7) 0.0397(9) 0.0011(6) -0.0048(6) 0.0004(6) C2S 0.0654(13) 0.0655(13) 0.0410(11) 0.0155(9) -0.0153(9) -0.0263(10) N1 0.0188(4) 0.0176(4) 0.0180(4) 0.0042(3) 0.0046(3) 0.0054(3) N2 0.0200(4) 0.0173(4) 0.0176(4) 0.0036(3) 0.0038(3) 0.0054(3) N1B 0.0195(4) 0.0213(4) 0.0198(4) 0.0052(3) 0.0035(3) 0.0052(3) N2B 0.0217(4) 0.0239(4) 0.0202(5) 0.0004(3) 0.0014(3) 0.0053(3) N1S 0.0413(7) 0.0337(6) 0.0433(8) 0.0020(6) 0.0015(6) 0.0083(5) O3 0.0258(4) 0.0193(3) 0.0160(4) 0.0032(3) 0.0021(3) 0.0076(3) O6 0.0166(3) 0.0186(3) 0.0168(3) 0.0021(3) 0.0044(3) 0.0055(2) O1B 0.0163(3) 0.0174(3) 0.0208(4) 0.0028(3) 0.0045(3) 0.0067(2) O2B 0.0252(4) 0.0182(3) 0.0265(4) 0.0017(3) 0.0040(3) 0.0017(3) Zn1 0.01794(5) 0.01535(5) 0.01486(6) 0.00309(4) 0.00401(4) 0.00502(4) Zn2 0.01781(6) 0.01661(6) 0.01775(6) 0.00224(4) 0.00292(4) 0.00480(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 C1A O3 1.3037(15) . ? C1A C6A 1.4380(15) . ? C1A C2A 1.4435(16) . ? C2A C3A 1.3885(18) . ? C2A C8A 1.5378(17) . ? C3A C4A 1.4023(19) . ? C4A C5A 1.3765(18) . ? C5A C6A 1.4090(17) . ? C6A C7A 1.4399(16) . ? C7A N2 1.2917(15) . ? C8A C11A 1.5380(19) . ? C8A C9A 1.539(2) . ? C8A C10A 1.544(2) . ? C12A C13A 1.3942(15) . ? C12A C17A 1.4072(16) . ? C12A N2 1.4112(14) . ? C13A C14A 1.3919(17) . ? C14A C15A 1.3891(19) . ? C15A C16A 1.3919(17) . ? C16A C17A 1.4013(16) . ? C17A N1 1.4184(14) . ? C18A N1 1.2911(14) . ? C18A C19A 1.4526(15) . ? C19A C20A 1.4060(19) . ? C19A C24A 1.4216(15) . ? C19A C20' 1.460(3) . ? C20A C21A 1.378(2) . ? C21A C22A 1.396(2) . ? C22A C23A 1.386(3) . ? C20' C21' 1.381(10) . ? C21' C22' 1.362(12) . ? C22' C23A 1.502(12) . ? C23A C24A 1.4330(14) . ? C23A C25A 1.5317(17) . ? C24A O6 1.3379(13) . ? C25A C28A 1.5338(19) . ? C25A C26A 1.5367(17) . ? C25A C27A 1.541(2) . ? C1B O1B 1.3459(12) . ? C1B C6B 1.4248(17) . ? C1B C2B 1.4300(16) . ? C2B C3B 1.3985(16) . ? C2B C8B 1.5364(18) . ? C3B C4B 1.396(2) . ? C4B C5B 1.375(2) . ? C5B C6B 1.4112(15) . ? C6B C7B 1.4504(18) . ? C7B N1B 1.2951(15) . ? C8B C10B 1.5223(19) . ? C8B C11B 1.5368(17) . ? C8B C9B 1.5409(19) . ? C12B C13B 1.3981(18) . ? C12B C17B 1.4076(18) . ? C12B N1B 1.4169(16) . ? C13B C14B 1.392(2) . ? C14B C15B 1.384(2) . ? C15B C16B 1.392(2) . ? C16B C17B 1.3980(18) . ? C17B N2B 1.4078(17) . ? C18B N2B 1.2970(16) . ? C18B C19B 1.440(2) . ? C19B C20B 1.4158(18) . ? C19B C24B 1.432(2) . ? C20B C21B 1.378(2) . ? C21B C22B 1.395(3) . ? C22B C23B 1.3920(19) . ? C23B C24B 1.4438(18) . ? C23B C25B 1.529(2) . ? C24B O2B 1.3092(15) . ? C25B C26B 1.5393(19) . ? C25B C28B 1.542(2) . ? C25B C27B 1.5446(19) . ? C1S N1S 1.133(2) . ? C1S C2S 1.456(3) . ? N1 Zn1 2.1244(9) . ? N2 Zn1 2.0689(10) . ? N1B Zn2 2.1159(10) . ? N2B Zn2 2.0726(11) . ? O3 Zn1 1.9446(9) . ? O6 Zn1 2.0578(8) . ? O6 Zn2 2.0953(8) . ? O1B Zn2 2.0560(9) . ? O1B Zn1 2.0849(8) . ? O2B Zn2 1.9443(9) . ? Zn1 Zn2 3.0659(2) . ? 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 C1A C6A 123.19(10) . . ? O3 C1A C2A 119.51(10) . . ? C6A C1A C2A 117.27(11) . . ? C3A C2A C1A 118.77(11) . . ? C3A C2A C8A 121.08(10) . . ? C1A C2A C8A 120.13(11) . . ? C2A C3A C4A 123.47(11) . . ? C5A C4A C3A 118.46(12) . . ? C4A C5A C6A 121.04(11) . . ? C5A C6A C1A 120.92(10) . . ? C5A C6A C7A 115.68(10) . . ? C1A C6A C7A 123.36(10) . . ? N2 C7A C6A 125.75(10) . . ? C2A C8A C11A 111.78(12) . . ? C2A C8A C9A 111.19(10) . . ? C11A C8A C9A 107.21(11) . . ? C2A C8A C10A 108.49(10) . . ? C11A C8A C10A 106.78(12) . . ? C9A C8A C10A 111.33(12) . . ? C13A C12A C17A 119.83(10) . . ? C13A C12A N2 124.60(11) . . ? C17A C12A N2 115.50(9) . . ? C14A C13A C12A 119.86(11) . . ? C15A C14A C13A 120.57(11) . . ? C14A C15A C16A 120.13(11) . . ? C15A C16A C17A 119.87(12) . . ? C16A C17A C12A 119.73(10) . . ? C16A C17A N1 124.49(11) . . ? C12A C17A N1 115.50(9) . . ? N1 C18A C19A 125.72(10) . . ? C20A C19A C24A 119.40(11) . . ? C20A C19A C18A 116.07(11) . . ? C24A C19A C18A 124.51(10) . . ? C20A C19A C20' 12.11(9) . . ? C24A C19A C20' 126.31(12) . . ? C18A C19A C20' 108.53(12) . . ? C21A C20A C19A 121.29(14) . . ? C20A C21A C22A 118.50(16) . . ? C23A C22A C21A 122.85(15) . . ? C21' C20' C19A 114.6(6) . . ? C22' C21' C20' 120.6(9) . . ? C21' C22' C23A 126.6(8) . . ? C22A C23A C24A 118.00(13) . . ? C22A C23A C22' 15.4(10) . . ? C24A C23A C22' 112.7(5) . . ? C22A C23A C25A 120.20(12) . . ? C24A C23A C25A 121.70(10) . . ? C22' C23A C25A 122.4(5) . . ? O6 C24A C19A 120.93(9) . . ? O6 C24A C23A 120.65(10) . . ? C19A C24A C23A 118.41(10) . . ? C23A C25A C28A 113.49(10) . . ? C23A C25A C26A 112.17(11) . . ? C28A C25A C26A 107.18(11) . . ? C23A C25A C27A 107.55(10) . . ? C28A C25A C27A 108.84(12) . . ? C26A C25A C27A 107.41(10) . . ? O1B C1B C6B 120.42(10) . . ? O1B C1B C2B 120.81(10) . . ? C6B C1B C2B 118.78(10) . . ? C3B C2B C1B 117.38(11) . . ? C3B C2B C8B 120.56(10) . . ? C1B C2B C8B 121.92(10) . . ? C4B C3B C2B 123.48(12) . . ? C5B C4B C3B 119.01(11) . . ? C4B C5B C6B 120.29(12) . . ? C5B C6B C1B 120.48(11) . . ? C5B C6B C7B 114.67(11) . . ? C1B C6B C7B 124.75(9) . . ? N1B C7B C6B 125.66(11) . . ? C10B C8B C2B 111.74(10) . . ? C10B C8B C11B 107.00(12) . . ? C2B C8B C11B 112.23(11) . . ? C10B C8B C9B 110.16(11) . . ? C2B C8B C9B 108.52(11) . . ? C11B C8B C9B 107.09(11) . . ? C13B C12B C17B 119.54(12) . . ? C13B C12B N1B 124.88(12) . . ? C17B C12B N1B 115.49(10) . . ? C14B C13B C12B 119.85(14) . . ? C15B C14B C13B 120.70(14) . . ? C14B C15B C16B 120.05(14) . . ? C15B C16B C17B 120.02(14) . . ? C16B C17B C12B 119.78(12) . . ? C16B C17B N2B 124.85(12) . . ? C12B C17B N2B 115.34(11) . . ? N2B C18B C19B 125.16(13) . . ? C20B C19B C24B 120.77(13) . . ? C20B C19B C18B 114.87(13) . . ? C24B C19B C18B 124.30(11) . . ? C21B C20B C19B 120.43(15) . . ? C20B C21B C22B 118.99(13) . . ? C23B C22B C21B 123.73(14) . . ? C22B C23B C24B 118.01(14) . . ? C22B C23B C25B 120.77(12) . . ? C24B C23B C25B 121.20(11) . . ? O2B C24B C19B 122.70(11) . . ? O2B C24B C23B 119.26(12) . . ? C19B C24B C23B 118.03(11) . . ? C23B C25B C26B 112.44(13) . . ? C23B C25B C28B 110.79(11) . . ? C26B C25B C28B 106.80(13) . . ? C23B C25B C27B 108.39(12) . . ? C26B C25B C27B 106.92(12) . . ? C28B C25B C27B 111.46(12) . . ? N1S C1S C2S 179.4(2) . . ? C18A N1 C17A 121.47(9) . . ? C18A N1 Zn1 126.88(7) . . ? C17A N1 Zn1 111.63(7) . . ? C7A N2 C12A 121.32(10) . . ? C7A N2 Zn1 124.80(7) . . ? C12A N2 Zn1 113.30(8) . . ? C7B N1B C12B 121.39(10) . . ? C7B N1B Zn2 126.20(9) . . ? C12B N1B Zn2 112.37(7) . . ? C18B N2B C17B 120.88(12) . . ? C18B N2B Zn2 124.62(9) . . ? C17B N2B Zn2 113.65(8) . . ? C1A O3 Zn1 128.84(7) . . ? C24A O6 Zn1 127.23(7) . . ? C24A O6 Zn2 114.52(7) . . ? Zn1 O6 Zn2 95.16(3) . . ? C1B O1B Zn2 125.34(8) . . ? C1B O1B Zn1 118.60(7) . . ? Zn2 O1B Zn1 95.53(3) . . ? C24B O2B Zn2 128.82(8) . . ? O3 Zn1 O6 101.14(3) . . ? O3 Zn1 N2 89.92(4) . . ? O6 Zn1 N2 162.10(4) . . ? O3 Zn1 O1B 118.11(4) . . ? O6 Zn1 O1B 83.62(3) . . ? N2 Zn1 O1B 103.68(3) . . ? O3 Zn1 N1 139.48(4) . . ? O6 Zn1 N1 84.98(3) . . ? N2 Zn1 N1 77.53(4) . . ? O1B Zn1 N1 102.33(4) . . ? O3 Zn1 Zn2 124.05(3) . . ? O6 Zn1 Zn2 42.89(2) . . ? N2 Zn1 Zn2 138.40(3) . . ? O1B Zn1 Zn2 41.87(2) . . ? N1 Zn1 Zn2 87.48(3) . . ? O2B Zn2 O1B 101.80(4) . . ? O2B Zn2 N2B 90.04(4) . . ? O1B Zn2 N2B 162.96(4) . . ? O2B Zn2 O6 117.87(4) . . ? O1B Zn2 O6 83.41(3) . . ? N2B Zn2 O6 102.00(4) . . ? O2B Zn2 N1B 138.14(4) . . ? O1B Zn2 N1B 85.55(4) . . ? N2B Zn2 N1B 77.48(4) . . ? O6 Zn2 N1B 103.84(4) . . ? O2B Zn2 Zn1 124.28(3) . . ? O1B Zn2 Zn1 42.60(2) . . ? N2B Zn2 Zn1 137.10(3) . . ? O6 Zn2 Zn1 41.95(2) . . ? N1B Zn2 Zn1 88.85(3) . . ? 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 C1A C2A C3A -179.87(10) . . . . ? C6A C1A C2A C3A -1.56(16) . . . . ? O3 C1A C2A C8A -0.95(16) . . . . ? C6A C1A C2A C8A 177.37(10) . . . . ? C1A C2A C3A C4A 2.20(18) . . . . ? C8A C2A C3A C4A -176.71(11) . . . . ? C2A C3A C4A C5A -0.36(19) . . . . ? C3A C4A C5A C6A -2.11(18) . . . . ? C4A C5A C6A C1A 2.69(17) . . . . ? C4A C5A C6A C7A -179.81(11) . . . . ? O3 C1A C6A C5A 177.46(10) . . . . ? C2A C1A C6A C5A -0.79(16) . . . . ? O3 C1A C6A C7A 0.15(17) . . . . ? C2A C1A C6A C7A -178.09(10) . . . . ? C5A C6A C7A N2 168.60(11) . . . . ? C1A C6A C7A N2 -13.96(17) . . . . ? C3A C2A C8A C11A -4.26(17) . . . . ? C1A C2A C8A C11A 176.84(12) . . . . ? C3A C2A C8A C9A -124.04(13) . . . . ? C1A C2A C8A C9A 57.06(15) . . . . ? C3A C2A C8A C10A 113.22(13) . . . . ? C1A C2A C8A C10A -65.69(14) . . . . ? C17A C12A C13A C14A 0.36(17) . . . . ? N2 C12A C13A C14A 177.12(11) . . . . ? C12A C13A C14A C15A -0.75(19) . . . . ? C13A C14A C15A C16A 0.3(2) . . . . ? C14A C15A C16A C17A 0.5(2) . . . . ? C15A C16A C17A C12A -0.91(19) . . . . ? C15A C16A C17A N1 -174.60(12) . . . . ? C13A C12A C17A C16A 0.46(17) . . . . ? N2 C12A C17A C16A -176.59(11) . . . . ? C13A C12A C17A N1 174.70(10) . . . . ? N2 C12A C17A N1 -2.35(14) . . . . ? N1 C18A C19A C20A 177.52(13) . . . . ? N1 C18A C19A C24A -4.01(19) . . . . ? N1 C18A C19A C20' 167.26(13) . . . . ? C24A C19A C20A C21A 2.1(2) . . . . ? C18A C19A C20A C21A -179.33(14) . . . . ? C20' C19A C20A C21A -125.7(5) . . . . ? C19A C20A C21A C22A 5.8(2) . . . . ? C20A C21A C22A C23A -3.7(2) . . . . ? C20A C19A C20' C21' 56.0(12) . . . . ? C24A C19A C20' C21' -2.6(12) . . . . ? C18A C19A C20' C21' -173.7(12) . . . . ? C19A C20' C21' C22' 8(2) . . . . ? C20' C21' C22' C23A -12(3) . . . . ? C21A C22A C23A C24A -6.3(2) . . . . ? C21A C22A C23A C22' 67(2) . . . . ? C21A C22A C23A C25A 170.11(13) . . . . ? C21' C22' C23A C22A -105(3) . . . . ? C21' C22' C23A C24A 8(2) . . . . ? C21' C22' C23A C25A 168.4(14) . . . . ? C20A C19A C24A O6 166.87(13) . . . . ? C18A C19A C24A O6 -11.55(18) . . . . ? C20' C19A C24A O6 178.74(13) . . . . ? C20A C19A C24A C23A -12.08(18) . . . . ? C18A C19A C24A C23A 169.49(11) . . . . ? C20' C19A C24A C23A -0.2(2) . . . . ? C22A C23A C24A O6 -164.94(13) . . . . ? C22' C23A C24A O6 179.0(11) . . . . ? C25A C23A C24A O6 18.67(17) . . . . ? C22A C23A C24A C19A 14.01(18) . . . . ? C22' C23A C24A C19A -2.0(11) . . . . ? C25A C23A C24A C19A -162.37(11) . . . . ? C22A C23A C25A C28A 117.56(15) . . . . ? C24A C23A C25A C28A -66.14(16) . . . . ? C22' C23A C25A C28A 135.4(12) . . . . ? C22A C23A C25A C26A -4.10(18) . . . . ? C24A C23A C25A C26A 172.20(11) . . . . ? C22' C23A C25A C26A 13.8(12) . . . . ? C22A C23A C25A C27A -122.00(14) . . . . ? C24A C23A C25A C27A 54.31(15) . . . . ? C22' C23A C25A C27A -104.1(12) . . . . ? O1B C1B C2B C3B -172.05(11) . . . . ? C6B C1B C2B C3B 7.84(17) . . . . ? O1B C1B C2B C8B 12.30(17) . . . . ? C6B C1B C2B C8B -167.81(11) . . . . ? C1B C2B C3B C4B -2.05(19) . . . . ? C8B C2B C3B C4B 173.66(13) . . . . ? C2B C3B C4B C5B -3.5(2) . . . . ? C3B C4B C5B C6B 3.1(2) . . . . ? C4B C5B C6B C1B 2.82(19) . . . . ? C4B C5B C6B C7B -173.77(12) . . . . ? O1B C1B C6B C5B 171.51(11) . . . . ? C2B C1B C6B C5B -8.38(17) . . . . ? O1B C1B C6B C7B -12.26(18) . . . . ? C2B C1B C6B C7B 167.84(11) . . . . ? C5B C6B C7B N1B 169.92(12) . . . . ? C1B C6B C7B N1B -6.5(2) . . . . ? C3B C2B C8B C10B 120.21(13) . . . . ? C1B C2B C8B C10B -64.28(16) . . . . ? C3B C2B C8B C11B 0.02(17) . . . . ? C1B C2B C8B C11B 175.53(12) . . . . ? C3B C2B C8B C9B -118.13(13) . . . . ? C1B C2B C8B C9B 57.38(14) . . . . ? C17B C12B C13B C14B 0.7(2) . . . . ? N1B C12B C13B C14B -175.83(13) . . . . ? C12B C13B C14B C15B 0.9(2) . . . . ? C13B C14B C15B C16B -0.9(3) . . . . ? C14B C15B C16B C17B -0.7(2) . . . . ? C15B C16B C17B C12B 2.3(2) . . . . ? C15B C16B C17B N2B -179.63(13) . . . . ? C13B C12B C17B C16B -2.28(19) . . . . ? N1B C12B C17B C16B 174.57(12) . . . . ? C13B C12B C17B N2B 179.46(11) . . . . ? N1B C12B C17B N2B -3.69(16) . . . . ? N2B C18B C19B C20B 167.84(12) . . . . ? N2B C18B C19B C24B -14.9(2) . . . . ? C24B C19B C20B C21B 1.7(2) . . . . ? C18B C19B C20B C21B 179.03(12) . . . . ? C19B C20B C21B C22B -1.8(2) . . . . ? C20B C21B C22B C23B 0.3(2) . . . . ? C21B C22B C23B C24B 1.4(2) . . . . ? C21B C22B C23B C25B -177.38(13) . . . . ? C20B C19B C24B O2B 178.75(12) . . . . ? C18B C19B C24B O2B 1.69(19) . . . . ? C20B C19B C24B C23B -0.01(18) . . . . ? C18B C19B C24B C23B -177.07(11) . . . . ? C22B C23B C24B O2B 179.73(11) . . . . ? C25B C23B C24B O2B -1.50(18) . . . . ? C22B C23B C24B C19B -1.47(17) . . . . ? C25B C23B C24B C19B 177.30(11) . . . . ? C22B C23B C25B C26B -3.31(18) . . . . ? C24B C23B C25B C26B 177.95(12) . . . . ? C22B C23B C25B C28B -122.74(13) . . . . ? C24B C23B C25B C28B 58.52(15) . . . . ? C22B C23B C25B C27B 114.66(13) . . . . ? C24B C23B C25B C27B -64.07(15) . . . . ? C19A C18A N1 C17A 176.49(11) . . . . ? C19A C18A N1 Zn1 -5.57(17) . . . . ? C16A C17A N1 C18A -24.22(17) . . . . ? C12A C17A N1 C18A 161.85(11) . . . . ? C16A C17A N1 Zn1 157.55(10) . . . . ? C12A C17A N1 Zn1 -16.38(12) . . . . ? C6A C7A N2 C12A 177.07(10) . . . . ? C6A C7A N2 Zn1 6.45(16) . . . . ? C13A C12A N2 C7A 32.18(17) . . . . ? C17A C12A N2 C7A -150.93(10) . . . . ? C13A C12A N2 Zn1 -156.20(9) . . . . ? C17A C12A N2 Zn1 20.69(12) . . . . ? C6B C7B N1B C12B 178.90(11) . . . . ? C6B C7B N1B Zn2 -3.75(18) . . . . ? C13B C12B N1B C7B -19.76(19) . . . . ? C17B C12B N1B C7B 163.57(11) . . . . ? C13B C12B N1B Zn2 162.56(10) . . . . ? C17B C12B N1B Zn2 -14.11(13) . . . . ? C19B C18B N2B C17B 174.76(11) . . . . ? C19B C18B N2B Zn2 6.01(17) . . . . ? C16B C17B N2B C18B 32.19(19) . . . . ? C12B C17B N2B C18B -149.65(12) . . . . ? C16B C17B N2B Zn2 -157.90(11) . . . . ? C12B C17B N2B Zn2 20.26(13) . . . . ? C6A C1A O3 Zn1 20.45(16) . . . . ? C2A C1A O3 Zn1 -161.34(8) . . . . ? C19A C24A O6 Zn1 36.64(15) . . . . ? C23A C24A O6 Zn1 -144.43(9) . . . . ? C19A C24A O6 Zn2 -81.44(12) . . . . ? C23A C24A O6 Zn2 97.49(11) . . . . ? C6B C1B O1B Zn2 40.28(14) . . . . ? C2B C1B O1B Zn2 -139.83(9) . . . . ? C6B C1B O1B Zn1 -81.13(12) . . . . ? C2B C1B O1B Zn1 98.76(11) . . . . ? C19B C24B O2B Zn2 19.91(17) . . . . ? C23B C24B O2B Zn2 -161.35(9) . . . . ? C1A O3 Zn1 O6 172.88(9) . . . . ? C1A O3 Zn1 N2 -21.30(10) . . . . ? C1A O3 Zn1 O1B 84.21(10) . . . . ? C1A O3 Zn1 N1 -91.78(10) . . . . ? C1A O3 Zn1 Zn2 133.06(9) . . . . ? C24A O6 Zn1 O3 104.91(9) . . . . ? Zn2 O6 Zn1 O3 -128.79(3) . . . . ? C24A O6 Zn1 N2 -22.29(17) . . . . ? Zn2 O6 Zn1 N2 104.00(11) . . . . ? C24A O6 Zn1 O1B -137.63(9) . . . . ? Zn2 O6 Zn1 O1B -11.33(3) . . . . ? C24A O6 Zn1 N1 -34.59(9) . . . . ? Zn2 O6 Zn1 N1 91.70(4) . . . . ? C24A O6 Zn1 Zn2 -126.30(10) . . . . ? C7A N2 Zn1 O3 7.77(9) . . . . ? C12A N2 Zn1 O3 -163.51(7) . . . . ? C7A N2 Zn1 O6 136.38(11) . . . . ? C12A N2 Zn1 O6 -34.90(16) . . . . ? C7A N2 Zn1 O1B -111.21(9) . . . . ? C12A N2 Zn1 O1B 77.51(7) . . . . ? C7A N2 Zn1 N1 148.93(10) . . . . ? C12A N2 Zn1 N1 -22.35(7) . . . . ? C7A N2 Zn1 Zn2 -139.55(8) . . . . ? C12A N2 Zn1 Zn2 49.17(9) . . . . ? C1B O1B Zn1 O3 -113.58(8) . . . . ? Zn2 O1B Zn1 O3 110.81(4) . . . . ? C1B O1B Zn1 O6 147.18(8) . . . . ? Zn2 O1B Zn1 O6 11.56(3) . . . . ? C1B O1B Zn1 N2 -16.20(9) . . . . ? Zn2 O1B Zn1 N2 -151.82(3) . . . . ? C1B O1B Zn1 N1 63.76(8) . . . . ? Zn2 O1B Zn1 N1 -71.86(4) . . . . ? C1B O1B Zn1 Zn2 135.62(9) . . . . ? C18A N1 Zn1 O3 -82.44(12) . . . . ? C17A N1 Zn1 O3 95.67(8) . . . . ? C18A N1 Zn1 O6 18.85(10) . . . . ? C17A N1 Zn1 O6 -163.04(8) . . . . ? C18A N1 Zn1 N2 -157.31(11) . . . . ? C17A N1 Zn1 N2 20.80(7) . . . . ? C18A N1 Zn1 O1B 101.18(10) . . . . ? C17A N1 Zn1 O1B -80.71(8) . . . . ? C18A N1 Zn1 Zn2 61.77(10) . . . . ? C17A N1 Zn1 Zn2 -120.12(7) . . . . ? C24B O2B Zn2 O1B 170.54(10) . . . . ? C24B O2B Zn2 N2B -21.81(11) . . . . ? C24B O2B Zn2 O6 81.81(11) . . . . ? C24B O2B Zn2 N1B -92.90(11) . . . . ? C24B O2B Zn2 Zn1 130.69(10) . . . . ? C1B O1B Zn2 O2B 100.31(8) . . . . ? Zn1 O1B Zn2 O2B -128.53(4) . . . . ? C1B O1B Zn2 N2B -32.82(17) . . . . ? Zn1 O1B Zn2 N2B 98.35(12) . . . . ? C1B O1B Zn2 O6 -142.52(8) . . . . ? Zn1 O1B Zn2 O6 -11.36(3) . . . . ? C1B O1B Zn2 N1B -38.02(8) . . . . ? Zn1 O1B Zn2 N1B 93.15(4) . . . . ? C1B O1B Zn2 Zn1 -131.17(9) . . . . ? C18B N2B Zn2 O2B 8.67(10) . . . . ? C17B N2B Zn2 O2B -160.80(8) . . . . ? C18B N2B Zn2 O1B 143.07(12) . . . . ? C17B N2B Zn2 O1B -26.40(17) . . . . ? C18B N2B Zn2 O6 -109.89(10) . . . . ? C17B N2B Zn2 O6 80.63(8) . . . . ? C18B N2B Zn2 N1B 148.38(11) . . . . ? C17B N2B Zn2 N1B -21.09(8) . . . . ? C18B N2B Zn2 Zn1 -137.24(9) . . . . ? C17B N2B Zn2 Zn1 53.29(9) . . . . ? C24A O6 Zn2 O2B -113.47(7) . . . . ? Zn1 O6 Zn2 O2B 111.39(4) . . . . ? C24A O6 Zn2 O1B 146.64(7) . . . . ? Zn1 O6 Zn2 O1B 11.50(3) . . . . ? C24A O6 Zn2 N2B -16.97(8) . . . . ? Zn1 O6 Zn2 N2B -152.11(4) . . . . ? C24A O6 Zn2 N1B 62.90(8) . . . . ? Zn1 O6 Zn2 N1B -72.24(4) . . . . ? C24A O6 Zn2 Zn1 135.14(8) . . . . ? C7B N1B Zn2 O2B -82.96(12) . . . . ? C12B N1B Zn2 O2B 94.59(9) . . . . ? C7B N1B Zn2 O1B 19.77(10) . . . . ? C12B N1B Zn2 O1B -162.68(8) . . . . ? C7B N1B Zn2 N2B -158.67(11) . . . . ? C12B N1B Zn2 N2B 18.88(8) . . . . ? C7B N1B Zn2 O6 101.86(10) . . . . ? C12B N1B Zn2 O6 -80.59(8) . . . . ? C7B N1B Zn2 Zn1 62.30(10) . . . . ? C12B N1B Zn2 Zn1 -120.15(8) . . . . ? O3 Zn1 Zn2 O2B -27.69(4) . . . . ? O6 Zn1 Zn2 O2B -95.05(5) . . . . ? N2 Zn1 Zn2 O2B 111.64(5) . . . . ? O1B Zn1 Zn2 O2B 67.93(5) . . . . ? N1 Zn1 Zn2 O2B 179.61(4) . . . . ? O3 Zn1 Zn2 O1B -95.62(5) . . . . ? O6 Zn1 Zn2 O1B -162.99(5) . . . . ? N2 Zn1 Zn2 O1B 43.71(5) . . . . ? N1 Zn1 Zn2 O1B 111.68(4) . . . . ? O3 Zn1 Zn2 N2B 109.60(5) . . . . ? O6 Zn1 Zn2 N2B 42.23(5) . . . . ? N2 Zn1 Zn2 N2B -111.07(6) . . . . ? O1B Zn1 Zn2 N2B -154.78(5) . . . . ? N1 Zn1 Zn2 N2B -43.10(5) . . . . ? O3 Zn1 Zn2 O6 67.37(4) . . . . ? N2 Zn1 Zn2 O6 -153.30(5) . . . . ? O1B Zn1 Zn2 O6 162.99(5) . . . . ? N1 Zn1 Zn2 O6 -85.33(4) . . . . ? O3 Zn1 Zn2 N1B 179.71(4) . . . . ? O6 Zn1 Zn2 N1B 112.34(4) . . . . ? N2 Zn1 Zn2 N1B -40.96(5) . . . . ? O1B Zn1 Zn2 N1B -84.67(4) . . . . ? N1 Zn1 Zn2 N1B 27.01(4) . . . . ? _diffrn_measured_fraction_theta_max 0.941 _diffrn_reflns_theta_full 36.62 _diffrn_measured_fraction_theta_full 0.941 _refine_diff_density_max 1.435 _refine_diff_density_min -1.130 _refine_diff_density_rms 0.080 # Attachment 'AWK319Pca21X1.cif' data_awk319pca21 _database_code_depnum_ccdc_archive 'CCDC 755296' #TrackingRef 'AWK319Pca21X1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C69.33 H58.67 N5.33 O5.33 Zn2.67' _chemical_formula_weight 1226.20 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 Orthorhombic _symmetry_space_group_name_H-M Pca2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 14.6644(5) _cell_length_b 12.6647(4) _cell_length_c 22.4167(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4163.2(2) _cell_formula_units_Z 3 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5471 _cell_measurement_theta_min 3.22 _cell_measurement_theta_max 37.92 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.467 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1904 _exptl_absorpt_coefficient_mu 1.206 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.66 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_process_details ; SADABS Version 2008/1 Bruker-Nonius Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_special_details ; It should be noted that the esd's of the cell dimensions are probably too low; they should be multiplied by a factor of 2 to 10 ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_specimen_suppport 'magnetic support whith 10 micron nylon fiber cryoloop' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'rotating anode X-ray tube' _diffrn_source_type 'Bruker-Nonius FR 591' _diffrn_source_power 50 _diffrn_source_current 70 _diffrn_source_size '3 mm x 0.3 mm fine focus' _diffrn_radiation_monochromator 'Multilayer Montel 200 mirrors' _diffrn_detector_type '4K CCD area detector APEX II' _diffrn_measurement_device_type 'Kappa 4-axis goniometer bruker-nonius' _diffrn_measurement_method ; Fullsphere data collection, phi and omega scans ; _diffrn_detector_area_resol_mean 512 _diffrn_reflns_number 33023 _diffrn_reflns_av_R_equivalents 0.0289 _diffrn_reflns_av_sigmaI/netI 0.0605 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.80 _diffrn_reflns_theta_max 39.31 _reflns_number_total 17366 _reflns_number_gt 15142 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v2009.1-0' _computing_cell_refinement 'Bruker APEX2 v2009.1-0' _computing_data_reduction 'Bruker SAINT V7.60A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXS-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0300P)^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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.002(4) _refine_ls_number_reflns 17366 _refine_ls_number_parameters 559 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0403 _refine_ls_R_factor_gt 0.0322 _refine_ls_wR_factor_ref 0.0748 _refine_ls_wR_factor_gt 0.0723 _refine_ls_goodness_of_fit_ref 0.982 _refine_ls_restrained_S_all 0.982 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1A C 0.39457(8) 0.97536(9) 0.82630(6) 0.01158(18) Uani 1 1 d . . . C2A C 0.39016(9) 1.06038(11) 0.86737(6) 0.0137(2) Uani 1 1 d . . . C3A C 0.35368(11) 1.15587(11) 0.84853(6) 0.0173(2) Uani 1 1 d . . . H3A H 0.3507 1.2129 0.8760 0.021 Uiso 1 1 calc R . . C4A C 0.32121(12) 1.17078(12) 0.79047(6) 0.0198(3) Uani 1 1 d . . . H4A H 0.2980 1.2375 0.7785 0.024 Uiso 1 1 calc R . . C5A C 0.32336(10) 1.08750(11) 0.75088(6) 0.0170(2) Uani 1 1 d . . . H5A H 0.3009 1.0969 0.7115 0.020 Uiso 1 1 calc R . . C6A C 0.35858(9) 0.98847(10) 0.76817(6) 0.0134(2) Uani 1 1 d . . . C7A C 0.35207(10) 0.90412(11) 0.72485(6) 0.0147(2) Uani 1 1 d . . . H7A H 0.3331 0.9221 0.6856 0.018 Uiso 1 1 calc R . . C8A C 0.36377(10) 0.72814(11) 0.69073(6) 0.0142(2) Uani 1 1 d . . . C9A C 0.37918(11) 0.74709(13) 0.63017(6) 0.0184(3) Uani 1 1 d . . . H9A H 0.3906 0.8167 0.6163 0.022 Uiso 1 1 calc R . . C10A C 0.37752(12) 0.66267(14) 0.59036(6) 0.0228(3) Uani 1 1 d . . . H10A H 0.3866 0.6750 0.5490 0.027 Uiso 1 1 calc R . . C11A C 0.36266(12) 0.56069(13) 0.61079(6) 0.0234(3) Uani 1 1 d . . . H11A H 0.3624 0.5036 0.5833 0.028 Uiso 1 1 calc R . . C12A C 0.34826(11) 0.54123(13) 0.67087(6) 0.0198(3) Uani 1 1 d . . . H12A H 0.3388 0.4711 0.6846 0.024 Uiso 1 1 calc R . . C13A C 0.34770(10) 0.62546(11) 0.71124(6) 0.0146(2) Uani 1 1 d . . . C14A C 0.29384(10) 0.53474(11) 0.79656(6) 0.0152(2) Uani 1 1 d . . . H14A H 0.2663 0.4857 0.7700 0.018 Uiso 1 1 calc R . . C15A C 0.28432(10) 0.51569(11) 0.85932(6) 0.0151(2) Uani 1 1 d . . . C16A C 0.24746(10) 0.41665(12) 0.87579(7) 0.0180(2) Uani 1 1 d . . . H16A H 0.2278 0.3696 0.8454 0.022 Uiso 1 1 calc R . . C17A C 0.23927(11) 0.38659(12) 0.93422(7) 0.0210(3) Uani 1 1 d . . . H17A H 0.2145 0.3197 0.9445 0.025 Uiso 1 1 calc R . . C18A C 0.26847(11) 0.45719(12) 0.97849(7) 0.0198(3) Uani 1 1 d . . . H18A H 0.2641 0.4363 1.0191 0.024 Uiso 1 1 calc R . . C19A C 0.30335(10) 0.55593(11) 0.96539(6) 0.0170(2) Uani 1 1 d . . . C20A C 0.31112(9) 0.58940(11) 0.90447(6) 0.0145(2) Uani 1 1 d . . . C21A C 0.42623(10) 1.04216(12) 0.92952(6) 0.0165(2) Uani 1 1 d . . . H21C H 0.4043 0.9726 0.9437 0.020 Uiso 1 1 calc R . . H21D H 0.4936 1.0390 0.9277 0.020 Uiso 1 1 calc R . . C22A C 0.39929(11) 1.12451(13) 0.97441(6) 0.0194(3) Uani 1 1 d . . . H22A H 0.3364 1.1415 0.9780 0.023 Uiso 1 1 calc R . . C23A C 0.45765(14) 1.17476(15) 1.00917(7) 0.0280(3) Uani 1 1 d . . . H23A H 0.5210 1.1595 1.0066 0.034 Uiso 1 1 calc R . . H23B H 0.4363 1.2261 1.0367 0.034 Uiso 1 1 calc R . . C24A C 0.34082(13) 0.62617(13) 1.01342(7) 0.0238(3) Uani 1 1 d . . . H24C H 0.3093 0.6103 1.0515 0.029 Uiso 1 1 calc R . . H24D H 0.3280 0.7007 1.0031 0.029 Uiso 1 1 calc R . . C25A C 0.44242(16) 0.6123(2) 1.02193(8) 0.0381(5) Uani 1 1 d . . . H25A H 0.4713 0.6584 1.0495 0.046 Uiso 1 1 calc R . . C26A C 0.49421(15) 0.5436(2) 0.99525(8) 0.0470(6) Uani 1 1 d . . . H26C H 0.4686 0.4957 0.9673 0.056 Uiso 1 1 calc R . . H26D H 0.5576 0.5413 1.0038 0.056 Uiso 1 1 calc R . . C1B C 0.56101(9) 0.64460(10) 0.77193(6) 0.0125(2) Uani 1 1 d . . . C2B C 0.55587(9) 0.53440(11) 0.78198(6) 0.0141(2) Uani 1 1 d . . . C3B C 0.57632(11) 0.46546(12) 0.73601(6) 0.0185(3) Uani 1 1 d . . . H3B H 0.5721 0.3916 0.7430 0.022 Uiso 1 1 calc R . . C4B C 0.60316(12) 0.50114(13) 0.67938(7) 0.0223(3) Uani 1 1 d . . . H4B H 0.6154 0.4523 0.6482 0.027 Uiso 1 1 calc R . . C5B C 0.61138(11) 0.60739(12) 0.66988(6) 0.0188(3) Uani 1 1 d . . . H5B H 0.6309 0.6321 0.6320 0.023 Uiso 1 1 calc R . . C6B C 0.59136(9) 0.68138(11) 0.71548(6) 0.0141(2) Uani 1 1 d . . . C7B C 0.60214(10) 0.79141(12) 0.69998(6) 0.0150(2) Uani 1 1 d . . . H7B H 0.6204 0.8070 0.6603 0.018 Uiso 1 1 calc R . . C8B C 0.60063(10) 0.97516(11) 0.71409(6) 0.0144(2) Uani 1 1 d . . . C9B C 0.59092(11) 1.00529(12) 0.65428(6) 0.0183(3) Uani 1 1 d . . . H9B H 0.5761 0.9541 0.6249 0.022 Uiso 1 1 calc R . . C10B C 0.60307(12) 1.11009(13) 0.63806(6) 0.0208(3) Uani 1 1 d . . . H10B H 0.5978 1.1303 0.5974 0.025 Uiso 1 1 calc R . . C11B C 0.62299(12) 1.18570(13) 0.68112(7) 0.0210(3) Uani 1 1 d . . . H11B H 0.6313 1.2573 0.6696 0.025 Uiso 1 1 calc R . . C12B C 0.63085(11) 1.15746(12) 0.74070(7) 0.0186(2) Uani 1 1 d . . . H12B H 0.6432 1.2099 0.7699 0.022 Uiso 1 1 calc R . . C13B C 0.62063(10) 1.05189(11) 0.75778(6) 0.0140(2) Uani 1 1 d . . . C14B C 0.67359(10) 1.06401(11) 0.85695(6) 0.0138(2) Uani 1 1 d . . . H14B H 0.7051 1.1258 0.8446 0.017 Uiso 1 1 calc R . . C15B C 0.68150(9) 1.03397(11) 0.91852(6) 0.0138(2) Uani 1 1 d . . . C16B C 0.72061(10) 1.10991(11) 0.95702(6) 0.0164(2) Uani 1 1 d . . . H16B H 0.7433 1.1740 0.9408 0.020 Uiso 1 1 calc R . . C17B C 0.72635(11) 1.09269(12) 1.01744(6) 0.0191(3) Uani 1 1 d . . . H17B H 0.7529 1.1441 1.0429 0.023 Uiso 1 1 calc R . . C18B C 0.69225(11) 0.99765(12) 1.04086(6) 0.0187(3) Uani 1 1 d . . . H18B H 0.6949 0.9862 1.0827 0.022 Uiso 1 1 calc R . . C19B C 0.65513(10) 0.92057(11) 1.00492(6) 0.0151(2) Uani 1 1 d . . . C20B C 0.65070(9) 0.93430(11) 0.94178(5) 0.0132(2) Uani 1 1 d . . . C21B C 0.52901(10) 0.49659(11) 0.84364(6) 0.0160(2) Uani 1 1 d . . . H21A H 0.5780 0.5160 0.8720 0.019 Uiso 1 1 calc R . . H21B H 0.4731 0.5344 0.8560 0.019 Uiso 1 1 calc R . . C22B C 0.51203(12) 0.38024(12) 0.84846(7) 0.0212(3) Uani 1 1 d . . . H22B H 0.4633 0.3512 0.8259 0.025 Uiso 1 1 calc R . . C23B C 0.56070(14) 0.31510(15) 0.88224(9) 0.0297(4) Uani 1 1 d . . . H23C H 0.6099 0.3416 0.9054 0.036 Uiso 1 1 calc R . . H23D H 0.5463 0.2420 0.8833 0.036 Uiso 1 1 calc R . . C24B C 0.61639(11) 0.81995(12) 1.03203(6) 0.0193(3) Uani 1 1 d . . . H24A H 0.5587 0.8371 1.0528 0.023 Uiso 1 1 calc R . . H24B H 0.6020 0.7697 0.9995 0.023 Uiso 1 1 calc R . . C25B C 0.67965(13) 0.76760(12) 1.07517(7) 0.0228(3) Uani 1 1 d . . . H25B H 0.7396 0.7518 1.0617 0.027 Uiso 1 1 calc R . . C26B C 0.65842(15) 0.74144(13) 1.13088(7) 0.0273(3) Uani 1 1 d . . . H26A H 0.5992 0.7559 1.1459 0.033 Uiso 1 1 calc R . . H26B H 0.7025 0.7083 1.1556 0.033 Uiso 1 1 calc R . . N1A N 0.37012(8) 0.80649(9) 0.73566(5) 0.01333(19) Uani 1 1 d . . . N2A N 0.33741(8) 0.61412(9) 0.77321(5) 0.01445(19) Uani 1 1 d . . . N1B N 0.58919(9) 0.87047(9) 0.73539(5) 0.0136(2) Uani 1 1 d . . . N2B N 0.62718(8) 1.01393(8) 0.81685(5) 0.01346(17) Uani 1 1 d . . . O1A O 0.43331(7) 0.88533(8) 0.84419(4) 0.01259(16) Uani 1 1 d . . . O2A O 0.34207(8) 0.68417(8) 0.89394(4) 0.01675(18) Uani 1 1 d . . . O1B O 0.53502(6) 0.71020(7) 0.81536(4) 0.01229(15) Uani 1 1 d . . . O2B O 0.62044(8) 0.85725(8) 0.90928(4) 0.01592(18) Uani 1 1 d . . . Zn1A Zn 0.396475(10) 0.736879(11) 0.820988(6) 0.01142(3) Uani 1 1 d . . . Zn1B Zn 0.570471(10) 0.864835(11) 0.829345(6) 0.01163(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1A 0.0126(4) 0.0088(4) 0.0134(4) 0.0006(4) 0.0020(4) -0.0007(3) C2A 0.0136(5) 0.0109(5) 0.0168(5) -0.0004(4) 0.0011(4) -0.0009(4) C3A 0.0200(6) 0.0103(5) 0.0217(5) -0.0033(4) 0.0003(5) 0.0024(5) C4A 0.0267(7) 0.0107(6) 0.0221(6) 0.0022(5) -0.0021(5) 0.0042(5) C5A 0.0191(6) 0.0132(6) 0.0187(5) 0.0026(5) -0.0017(4) 0.0011(5) C6A 0.0150(5) 0.0110(5) 0.0142(4) -0.0003(4) -0.0003(4) 0.0003(4) C7A 0.0161(5) 0.0147(6) 0.0133(4) 0.0005(4) -0.0004(4) 0.0005(5) C8A 0.0159(5) 0.0144(6) 0.0124(4) -0.0023(4) -0.0025(4) 0.0006(4) C9A 0.0218(6) 0.0207(7) 0.0127(5) 0.0010(5) -0.0005(4) -0.0003(5) C10A 0.0260(7) 0.0276(8) 0.0147(5) -0.0043(5) 0.0004(5) -0.0014(6) C11A 0.0277(8) 0.0238(8) 0.0185(6) -0.0074(5) -0.0012(5) -0.0012(6) C12A 0.0219(7) 0.0180(7) 0.0196(5) -0.0061(5) 0.0001(5) -0.0021(5) C13A 0.0139(5) 0.0153(6) 0.0146(5) -0.0027(4) -0.0013(4) -0.0020(4) C14A 0.0135(5) 0.0126(6) 0.0195(5) -0.0018(4) -0.0014(4) -0.0007(4) C15A 0.0126(5) 0.0138(6) 0.0188(5) 0.0011(4) 0.0011(4) -0.0008(4) C16A 0.0143(5) 0.0141(6) 0.0256(6) 0.0006(5) 0.0019(5) -0.0018(5) C17A 0.0206(6) 0.0143(6) 0.0279(7) 0.0051(5) 0.0042(5) -0.0021(5) C18A 0.0201(6) 0.0182(6) 0.0212(6) 0.0046(5) 0.0054(5) 0.0004(5) C19A 0.0176(6) 0.0158(6) 0.0177(5) 0.0033(4) 0.0041(4) 0.0023(5) C20A 0.0134(5) 0.0130(6) 0.0171(5) 0.0013(4) 0.0026(4) 0.0008(4) C21A 0.0194(6) 0.0142(6) 0.0159(5) -0.0031(4) -0.0010(4) 0.0010(5) C22A 0.0184(6) 0.0213(7) 0.0184(5) -0.0035(5) 0.0028(5) 0.0006(5) C23A 0.0312(9) 0.0295(9) 0.0232(6) -0.0093(6) 0.0009(6) -0.0039(7) C24A 0.0352(9) 0.0201(7) 0.0161(5) 0.0019(5) 0.0018(5) -0.0026(6) C25A 0.0342(10) 0.0593(14) 0.0208(7) 0.0030(8) -0.0013(6) -0.0218(10) C26A 0.0216(8) 0.095(2) 0.0249(8) 0.0135(9) -0.0034(7) 0.0014(11) C1B 0.0118(5) 0.0111(5) 0.0146(4) -0.0021(4) -0.0006(4) 0.0013(4) C2B 0.0131(5) 0.0110(5) 0.0181(5) -0.0009(4) 0.0005(4) 0.0007(4) C3B 0.0220(6) 0.0118(6) 0.0218(6) -0.0029(5) 0.0020(5) 0.0011(5) C4B 0.0287(8) 0.0169(7) 0.0212(6) -0.0065(5) 0.0033(6) 0.0027(6) C5B 0.0230(7) 0.0171(6) 0.0164(5) -0.0033(5) 0.0033(5) 0.0023(5) C6B 0.0160(5) 0.0121(6) 0.0143(5) -0.0021(4) 0.0003(4) 0.0008(4) C7B 0.0162(5) 0.0153(6) 0.0137(5) -0.0006(4) 0.0008(4) 0.0003(5) C8B 0.0148(5) 0.0132(6) 0.0151(5) 0.0018(4) -0.0003(4) 0.0004(4) C9B 0.0227(7) 0.0180(7) 0.0142(5) 0.0014(5) -0.0009(4) 0.0011(5) C10B 0.0250(7) 0.0203(7) 0.0170(5) 0.0046(5) 0.0005(5) 0.0032(6) C11B 0.0274(7) 0.0146(6) 0.0211(6) 0.0054(5) 0.0015(5) 0.0028(5) C12B 0.0233(7) 0.0130(6) 0.0194(5) 0.0006(5) 0.0003(5) 0.0013(5) C13B 0.0148(5) 0.0125(6) 0.0147(5) 0.0011(4) -0.0003(4) 0.0009(4) C14B 0.0142(5) 0.0116(5) 0.0157(5) 0.0000(4) -0.0002(4) -0.0007(4) C15B 0.0134(5) 0.0127(5) 0.0153(5) -0.0020(4) -0.0009(4) -0.0002(4) C16B 0.0164(6) 0.0142(6) 0.0186(5) -0.0035(5) -0.0011(4) -0.0022(5) C17B 0.0226(7) 0.0179(6) 0.0168(5) -0.0055(5) -0.0026(5) -0.0015(5) C18B 0.0229(7) 0.0187(6) 0.0145(5) -0.0036(5) -0.0005(5) -0.0002(5) C19B 0.0168(5) 0.0146(6) 0.0139(4) -0.0017(4) 0.0000(4) 0.0010(4) C20B 0.0121(5) 0.0136(6) 0.0141(4) -0.0013(4) -0.0013(4) 0.0017(4) C21B 0.0157(5) 0.0122(5) 0.0201(5) 0.0010(4) 0.0015(4) 0.0013(4) C22B 0.0217(7) 0.0138(6) 0.0282(7) 0.0000(5) 0.0054(5) -0.0016(5) C23B 0.0304(9) 0.0185(8) 0.0402(9) 0.0092(7) 0.0083(7) 0.0044(6) C24B 0.0250(7) 0.0171(7) 0.0160(5) 0.0007(5) 0.0019(5) -0.0024(5) C25B 0.0290(8) 0.0170(6) 0.0225(6) 0.0004(5) 0.0014(6) 0.0012(6) C26B 0.0407(10) 0.0203(7) 0.0209(6) 0.0037(5) -0.0031(6) -0.0052(7) N1A 0.0146(5) 0.0123(5) 0.0131(4) -0.0013(4) -0.0007(3) 0.0003(4) N2A 0.0150(5) 0.0134(5) 0.0150(4) -0.0009(4) -0.0005(4) -0.0014(4) N1B 0.0151(5) 0.0119(5) 0.0139(4) 0.0000(4) -0.0010(3) -0.0009(4) N2B 0.0147(4) 0.0109(4) 0.0147(4) -0.0006(4) -0.0008(4) -0.0002(3) O1A 0.0136(4) 0.0092(4) 0.0150(3) -0.0001(3) -0.0006(3) 0.0011(3) O2A 0.0223(5) 0.0111(4) 0.0169(4) 0.0009(3) 0.0033(3) -0.0031(4) O1B 0.0131(3) 0.0105(4) 0.0132(3) -0.0019(3) -0.0001(3) 0.0002(3) O2B 0.0202(5) 0.0122(4) 0.0154(4) -0.0003(3) -0.0045(3) -0.0021(4) Zn1A 0.01232(5) 0.00932(6) 0.01263(5) -0.00026(5) -0.00002(5) -0.00060(4) Zn1B 0.01254(5) 0.00989(6) 0.01247(5) -0.00073(5) -0.00109(5) -0.00088(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 C1A O1A 1.3355(15) . ? C1A C6A 1.4156(18) . ? C1A C2A 1.4181(18) . ? C2A C3A 1.388(2) . ? C2A C21A 1.5082(19) . ? C3A C4A 1.399(2) . ? C4A C5A 1.379(2) . ? C5A C6A 1.4106(19) . ? C6A C7A 1.4469(18) . ? C7A N1A 1.2874(18) . ? C8A C9A 1.3969(19) . ? C8A C13A 1.399(2) . ? C8A N1A 1.4169(17) . ? C9A C10A 1.393(2) . ? C10A C11A 1.388(2) . ? C11A C12A 1.386(2) . ? C12A C13A 1.3989(19) . ? C13A N2A 1.4048(17) . ? C14A N2A 1.3011(18) . ? C14A C15A 1.4343(18) . ? C15A C16A 1.415(2) . ? C15A C20A 1.4319(19) . ? C16A C17A 1.369(2) . ? C17A C18A 1.403(2) . ? C18A C19A 1.383(2) . ? C19A C20A 1.4343(18) . ? C19A C24A 1.501(2) . ? C20A O2A 1.3047(18) . ? C21A C22A 1.502(2) . ? C22A C23A 1.321(2) . ? C24A C25A 1.512(3) . ? C25A C26A 1.301(4) . ? C1B O1B 1.3354(15) . ? C1B C2B 1.4158(19) . ? C1B C6B 1.4199(18) . ? C2B C3B 1.3836(19) . ? C2B C21B 1.5148(19) . ? C3B C4B 1.404(2) . ? C4B C5B 1.368(2) . ? C5B C6B 1.4175(19) . ? C6B C7B 1.445(2) . ? C7B N1B 1.2917(18) . ? C8B C9B 1.4011(19) . ? C8B C13B 1.4105(19) . ? C8B N1B 1.4192(18) . ? C9B C10B 1.388(2) . ? C10B C11B 1.391(2) . ? C11B C12B 1.387(2) . ? C12B C13B 1.399(2) . ? C13B N2B 1.4120(17) . ? C14B N2B 1.2937(17) . ? C14B C15B 1.4363(18) . ? C15B C16B 1.4138(19) . ? C15B C20B 1.439(2) . ? C16B C17B 1.3744(19) . ? C17B C18B 1.405(2) . ? C18B C19B 1.3777(19) . ? C19B C20B 1.4275(17) . ? C19B C24B 1.522(2) . ? C20B O2B 1.2961(16) . ? C21B C22B 1.498(2) . ? C22B C23B 1.328(3) . ? C24B C25B 1.495(2) . ? C25B C26B 1.329(2) . ? N1A Zn1A 2.1414(11) . ? N2A Zn1A 2.0770(11) . ? N1B Zn1B 2.1252(11) . ? N2B Zn1B 2.0822(11) . ? O1A Zn1A 2.0241(10) . ? O1A Zn1B 2.0551(10) . ? O2A Zn1A 1.9381(10) . ? O1B Zn1B 2.0504(9) . ? O1B Zn1A 2.0634(10) . ? O2B Zn1B 1.9384(10) . ? Zn1A Zn1B 3.0285(2) . ? 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 O1A C1A C6A 122.35(11) . . ? O1A C1A C2A 118.21(12) . . ? C6A C1A C2A 119.44(11) . . ? C3A C2A C1A 118.79(12) . . ? C3A C2A C21A 123.33(12) . . ? C1A C2A C21A 117.88(12) . . ? C2A C3A C4A 122.14(13) . . ? C5A C4A C3A 119.20(13) . . ? C4A C5A C6A 120.77(13) . . ? C5A C6A C1A 119.59(11) . . ? C5A C6A C7A 116.60(12) . . ? C1A C6A C7A 123.77(12) . . ? N1A C7A C6A 124.69(12) . . ? C9A C8A C13A 120.41(12) . . ? C9A C8A N1A 124.04(13) . . ? C13A C8A N1A 115.37(11) . . ? C10A C9A C8A 119.21(14) . . ? C11A C10A C9A 120.38(13) . . ? C12A C11A C10A 120.68(14) . . ? C11A C12A C13A 119.61(15) . . ? C12A C13A C8A 119.68(13) . . ? C12A C13A N2A 124.22(13) . . ? C8A C13A N2A 115.98(11) . . ? N2A C14A C15A 124.91(12) . . ? C16A C15A C20A 119.89(13) . . ? C16A C15A C14A 116.24(13) . . ? C20A C15A C14A 123.85(13) . . ? C17A C16A C15A 121.98(14) . . ? C16A C17A C18A 118.21(14) . . ? C19A C18A C17A 122.62(13) . . ? C18A C19A C20A 119.94(13) . . ? C18A C19A C24A 121.27(12) . . ? C20A C19A C24A 118.60(13) . . ? O2A C20A C15A 124.56(12) . . ? O2A C20A C19A 118.16(12) . . ? C15A C20A C19A 117.28(13) . . ? C22A C21A C2A 114.86(13) . . ? C23A C22A C21A 124.01(15) . . ? C19A C24A C25A 112.49(15) . . ? C26A C25A C24A 126.50(19) . . ? O1B C1B C2B 118.82(11) . . ? O1B C1B C6B 122.35(12) . . ? C2B C1B C6B 118.81(12) . . ? C3B C2B C1B 119.47(13) . . ? C3B C2B C21B 122.45(12) . . ? C1B C2B C21B 118.08(12) . . ? C2B C3B C4B 122.08(14) . . ? C5B C4B C3B 118.84(13) . . ? C4B C5B C6B 121.31(13) . . ? C5B C6B C1B 119.39(13) . . ? C5B C6B C7B 116.20(12) . . ? C1B C6B C7B 124.40(12) . . ? N1B C7B C6B 125.72(12) . . ? C9B C8B C13B 119.86(13) . . ? C9B C8B N1B 124.36(13) . . ? C13B C8B N1B 115.76(11) . . ? C10B C9B C8B 119.88(14) . . ? C9B C10B C11B 120.24(13) . . ? C12B C11B C10B 120.54(14) . . ? C11B C12B C13B 120.06(14) . . ? C12B C13B C8B 119.39(12) . . ? C12B C13B N2B 125.09(12) . . ? C8B C13B N2B 115.51(12) . . ? N2B C14B C15B 125.48(13) . . ? C16B C15B C14B 116.05(12) . . ? C16B C15B C20B 120.20(12) . . ? C14B C15B C20B 123.74(12) . . ? C17B C16B C15B 121.23(13) . . ? C16B C17B C18B 118.84(13) . . ? C19B C18B C17B 121.94(13) . . ? C18B C19B C20B 120.76(13) . . ? C18B C19B C24B 120.49(12) . . ? C20B C19B C24B 118.74(12) . . ? O2B C20B C19B 118.77(12) . . ? O2B C20B C15B 124.36(11) . . ? C19B C20B C15B 116.87(11) . . ? C22B C21B C2B 114.83(12) . . ? C23B C22B C21B 124.25(17) . . ? C25B C24B C19B 113.45(13) . . ? C26B C25B C24B 124.97(18) . . ? C7A N1A C8A 121.69(11) . . ? C7A N1A Zn1A 126.91(9) . . ? C8A N1A Zn1A 111.00(9) . . ? C14A N2A C13A 121.97(12) . . ? C14A N2A Zn1A 125.15(9) . . ? C13A N2A Zn1A 112.87(9) . . ? C7B N1B C8B 120.01(12) . . ? C7B N1B Zn1B 127.01(10) . . ? C8B N1B Zn1B 112.34(8) . . ? C14B N2B C13B 121.37(11) . . ? C14B N2B Zn1B 124.14(9) . . ? C13B N2B Zn1B 114.07(8) . . ? C1A O1A Zn1A 127.04(8) . . ? C1A O1A Zn1B 118.39(8) . . ? Zn1A O1A Zn1B 95.87(4) . . ? C20A O2A Zn1A 127.79(9) . . ? C1B O1B Zn1B 129.29(8) . . ? C1B O1B Zn1A 115.31(8) . . ? Zn1B O1B Zn1A 94.81(4) . . ? C20B O2B Zn1B 127.72(9) . . ? O2A Zn1A O1A 102.30(4) . . ? O2A Zn1A O1B 113.61(4) . . ? O1A Zn1A O1B 84.55(4) . . ? O2A Zn1A N2A 90.32(4) . . ? O1A Zn1A N2A 159.89(4) . . ? O1B Zn1A N2A 104.86(4) . . ? O2A Zn1A N1A 145.21(5) . . ? O1A Zn1A N1A 83.99(4) . . ? O1B Zn1A N1A 100.98(4) . . ? N2A Zn1A N1A 76.84(4) . . ? O2A Zn1A Zn1B 118.61(3) . . ? O1A Zn1A Zn1B 42.46(3) . . ? O1B Zn1A Zn1B 42.43(3) . . ? N2A Zn1A Zn1B 141.61(3) . . ? N1A Zn1A Zn1B 89.25(3) . . ? O2B Zn1B O1B 100.95(4) . . ? O2B Zn1B O1A 103.10(4) . . ? O1B Zn1B O1A 84.10(4) . . ? O2B Zn1B N2B 91.05(4) . . ? O1B Zn1B N2B 161.24(4) . . ? O1A Zn1B N2B 107.34(4) . . ? O2B Zn1B N1B 150.35(5) . . ? O1B Zn1B N1B 85.02(4) . . ? O1A Zn1B N1B 106.42(4) . . ? N2B Zn1B N1B 77.56(5) . . ? O2B Zn1B Zn1A 110.44(3) . . ? O1B Zn1B Zn1A 42.76(3) . . ? O1A Zn1B Zn1A 41.67(3) . . ? N2B Zn1B Zn1A 144.43(3) . . ? N1B Zn1B Zn1A 93.75(3) . . ? 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 O1A C1A C2A C3A 177.22(12) . . . . ? C6A C1A C2A C3A -2.51(19) . . . . ? O1A C1A C2A C21A -2.38(18) . . . . ? C6A C1A C2A C21A 177.90(12) . . . . ? C1A C2A C3A C4A 0.0(2) . . . . ? C21A C2A C3A C4A 179.60(15) . . . . ? C2A C3A C4A C5A 1.6(2) . . . . ? C3A C4A C5A C6A -0.6(2) . . . . ? C4A C5A C6A C1A -1.9(2) . . . . ? C4A C5A C6A C7A 175.82(14) . . . . ? O1A C1A C6A C5A -176.29(12) . . . . ? C2A C1A C6A C5A 3.42(19) . . . . ? O1A C1A C6A C7A 6.2(2) . . . . ? C2A C1A C6A C7A -174.10(13) . . . . ? C5A C6A C7A N1A -170.92(14) . . . . ? C1A C6A C7A N1A 6.7(2) . . . . ? C13A C8A C9A C10A 0.6(2) . . . . ? N1A C8A C9A C10A 175.41(15) . . . . ? C8A C9A C10A C11A -1.4(2) . . . . ? C9A C10A C11A C12A 0.7(3) . . . . ? C10A C11A C12A C13A 0.7(3) . . . . ? C11A C12A C13A C8A -1.5(2) . . . . ? C11A C12A C13A N2A -177.33(15) . . . . ? C9A C8A C13A C12A 0.8(2) . . . . ? N1A C8A C13A C12A -174.43(13) . . . . ? C9A C8A C13A N2A 177.01(13) . . . . ? N1A C8A C13A N2A 1.76(18) . . . . ? N2A C14A C15A C16A -170.08(14) . . . . ? N2A C14A C15A C20A 8.8(3) . . . . ? C20A C15A C16A C17A -2.4(2) . . . . ? C14A C15A C16A C17A 176.55(14) . . . . ? C15A C16A C17A C18A 0.1(2) . . . . ? C16A C17A C18A C19A 1.2(2) . . . . ? C17A C18A C19A C20A -0.3(2) . . . . ? C17A C18A C19A C24A -175.11(15) . . . . ? C16A C15A C20A O2A -176.94(14) . . . . ? C14A C15A C20A O2A 4.2(2) . . . . ? C16A C15A C20A C19A 3.2(2) . . . . ? C14A C15A C20A C19A -175.64(14) . . . . ? C18A C19A C20A O2A 178.20(14) . . . . ? C24A C19A C20A O2A -6.8(2) . . . . ? C18A C19A C20A C15A -1.9(2) . . . . ? C24A C19A C20A C15A 173.04(14) . . . . ? C3A C2A C21A C22A 14.6(2) . . . . ? C1A C2A C21A C22A -165.79(12) . . . . ? C2A C21A C22A C23A -128.04(17) . . . . ? C18A C19A C24A C25A 92.49(18) . . . . ? C20A C19A C24A C25A -82.41(18) . . . . ? C19A C24A C25A C26A -4.8(3) . . . . ? O1B C1B C2B C3B 175.39(13) . . . . ? C6B C1B C2B C3B -3.0(2) . . . . ? O1B C1B C2B C21B -5.36(19) . . . . ? C6B C1B C2B C21B 176.27(12) . . . . ? C1B C2B C3B C4B 0.7(2) . . . . ? C21B C2B C3B C4B -178.53(15) . . . . ? C2B C3B C4B C5B 1.6(3) . . . . ? C3B C4B C5B C6B -1.5(3) . . . . ? C4B C5B C6B C1B -0.8(2) . . . . ? C4B C5B C6B C7B -179.68(15) . . . . ? O1B C1B C6B C5B -175.25(13) . . . . ? C2B C1B C6B C5B 3.1(2) . . . . ? O1B C1B C6B C7B 3.5(2) . . . . ? C2B C1B C6B C7B -178.20(13) . . . . ? C5B C6B C7B N1B -178.51(15) . . . . ? C1B C6B C7B N1B 2.7(2) . . . . ? C13B C8B C9B C10B 1.5(2) . . . . ? N1B C8B C9B C10B 179.63(14) . . . . ? C8B C9B C10B C11B -1.3(2) . . . . ? C9B C10B C11B C12B -0.1(3) . . . . ? C10B C11B C12B C13B 1.3(3) . . . . ? C11B C12B C13B C8B -1.2(2) . . . . ? C11B C12B C13B N2B 179.98(14) . . . . ? C9B C8B C13B C12B -0.2(2) . . . . ? N1B C8B C13B C12B -178.53(13) . . . . ? C9B C8B C13B N2B 178.73(13) . . . . ? N1B C8B C13B N2B 0.40(18) . . . . ? N2B C14B C15B C16B -168.23(14) . . . . ? N2B C14B C15B C20B 10.5(2) . . . . ? C14B C15B C16B C17B 175.82(14) . . . . ? C20B C15B C16B C17B -3.0(2) . . . . ? C15B C16B C17B C18B -0.2(2) . . . . ? C16B C17B C18B C19B 1.4(2) . . . . ? C17B C18B C19B C20B 0.6(2) . . . . ? C17B C18B C19B C24B -178.24(15) . . . . ? C18B C19B C20B O2B 175.80(14) . . . . ? C24B C19B C20B O2B -5.4(2) . . . . ? C18B C19B C20B C15B -3.6(2) . . . . ? C24B C19B C20B C15B 175.24(13) . . . . ? C16B C15B C20B O2B -174.59(13) . . . . ? C14B C15B C20B O2B 6.7(2) . . . . ? C16B C15B C20B C19B 4.8(2) . . . . ? C14B C15B C20B C19B -173.94(13) . . . . ? C3B C2B C21B C22B -9.2(2) . . . . ? C1B C2B C21B C22B 171.62(13) . . . . ? C2B C21B C22B C23B 117.00(18) . . . . ? C18B C19B C24B C25B -49.7(2) . . . . ? C20B C19B C24B C25B 131.43(14) . . . . ? C19B C24B C25B C26B 126.13(17) . . . . ? C6A C7A N1A C8A -178.89(13) . . . . ? C6A C7A N1A Zn1A 9.0(2) . . . . ? C9A C8A N1A C7A 30.3(2) . . . . ? C13A C8A N1A C7A -154.61(13) . . . . ? C9A C8A N1A Zn1A -156.41(12) . . . . ? C13A C8A N1A Zn1A 18.65(15) . . . . ? C15A C14A N2A C13A 177.01(14) . . . . ? C15A C14A N2A Zn1A -4.0(2) . . . . ? C12A C13A N2A C14A -27.2(2) . . . . ? C8A C13A N2A C14A 156.82(14) . . . . ? C12A C13A N2A Zn1A 153.75(12) . . . . ? C8A C13A N2A Zn1A -22.24(15) . . . . ? C6B C7B N1B C8B -178.86(13) . . . . ? C6B C7B N1B Zn1B 11.1(2) . . . . ? C9B C8B N1B C7B 25.7(2) . . . . ? C13B C8B N1B C7B -156.04(14) . . . . ? C9B C8B N1B Zn1B -162.89(12) . . . . ? C13B C8B N1B Zn1B 15.35(15) . . . . ? C15B C14B N2B C13B 177.55(13) . . . . ? C15B C14B N2B Zn1B -10.4(2) . . . . ? C12B C13B N2B C14B -24.9(2) . . . . ? C8B C13B N2B C14B 156.28(13) . . . . ? C12B C13B N2B Zn1B 162.35(12) . . . . ? C8B C13B N2B Zn1B -16.51(15) . . . . ? C6A C1A O1A Zn1A -35.44(16) . . . . ? C2A C1A O1A Zn1A 144.84(9) . . . . ? C6A C1A O1A Zn1B 88.17(13) . . . . ? C2A C1A O1A Zn1B -91.54(12) . . . . ? C15A C20A O2A Zn1A -21.3(2) . . . . ? C19A C20A O2A Zn1A 158.58(10) . . . . ? C2B C1B O1B Zn1B 157.29(10) . . . . ? C6B C1B O1B Zn1B -24.40(18) . . . . ? C2B C1B O1B Zn1A -82.25(13) . . . . ? C6B C1B O1B Zn1A 96.06(13) . . . . ? C19B C20B O2B Zn1B 158.57(10) . . . . ? C15B C20B O2B Zn1B -22.1(2) . . . . ? C20A O2A Zn1A O1A -176.02(12) . . . . ? C20A O2A Zn1A O1B -86.64(12) . . . . ? C20A O2A Zn1A N2A 19.76(12) . . . . ? C20A O2A Zn1A N1A 86.75(14) . . . . ? C20A O2A Zn1A Zn1B -133.86(11) . . . . ? C1A O1A Zn1A O2A -108.23(10) . . . . ? Zn1B O1A Zn1A O2A 119.20(4) . . . . ? C1A O1A Zn1A O1B 138.75(10) . . . . ? Zn1B O1A Zn1A O1B 6.18(4) . . . . ? C1A O1A Zn1A N2A 19.49(19) . . . . ? Zn1B O1A Zn1A N2A -113.08(12) . . . . ? C1A O1A Zn1A N1A 37.07(10) . . . . ? Zn1B O1A Zn1A N1A -95.49(4) . . . . ? C1A O1A Zn1A Zn1B 132.57(12) . . . . ? C1B O1B Zn1A O2A 114.78(9) . . . . ? Zn1B O1B Zn1A O2A -107.25(4) . . . . ? C1B O1B Zn1A O1A -144.16(9) . . . . ? Zn1B O1B Zn1A O1A -6.19(4) . . . . ? C1B O1B Zn1A N2A 17.75(9) . . . . ? Zn1B O1B Zn1A N2A 155.73(4) . . . . ? C1B O1B Zn1A N1A -61.39(9) . . . . ? Zn1B O1B Zn1A N1A 76.59(4) . . . . ? C1B O1B Zn1A Zn1B -137.98(10) . . . . ? C14A N2A Zn1A O2A -7.36(13) . . . . ? C13A N2A Zn1A O2A 171.68(10) . . . . ? C14A N2A Zn1A O1A -136.75(13) . . . . ? C13A N2A Zn1A O1A 42.28(18) . . . . ? C14A N2A Zn1A O1B 107.22(12) . . . . ? C13A N2A Zn1A O1B -73.75(10) . . . . ? C14A N2A Zn1A N1A -154.72(13) . . . . ? C13A N2A Zn1A N1A 24.31(9) . . . . ? C14A N2A Zn1A Zn1B 133.74(11) . . . . ? C13A N2A Zn1A Zn1B -47.23(12) . . . . ? C7A N1A Zn1A O2A 78.84(15) . . . . ? C8A N1A Zn1A O2A -93.99(11) . . . . ? C7A N1A Zn1A O1A -24.09(12) . . . . ? C8A N1A Zn1A O1A 163.08(10) . . . . ? C7A N1A Zn1A O1B -107.33(12) . . . . ? C8A N1A Zn1A O1B 79.84(10) . . . . ? C7A N1A Zn1A N2A 149.78(13) . . . . ? C8A N1A Zn1A N2A -23.05(9) . . . . ? C7A N1A Zn1A Zn1B -66.31(12) . . . . ? C8A N1A Zn1A Zn1B 120.85(9) . . . . ? C20B O2B Zn1B O1B -177.19(12) . . . . ? C20B O2B Zn1B O1A -90.77(12) . . . . ? C20B O2B Zn1B N2B 17.31(12) . . . . ? C20B O2B Zn1B N1B 83.54(15) . . . . ? C20B O2B Zn1B Zn1A -133.74(11) . . . . ? C1B O1B Zn1B O2B -123.10(11) . . . . ? Zn1A O1B Zn1B O2B 108.34(5) . . . . ? C1B O1B Zn1B O1A 134.66(11) . . . . ? Zn1A O1B Zn1B O1A 6.10(4) . . . . ? C1B O1B Zn1B N2B 5.77(19) . . . . ? Zn1A O1B Zn1B N2B -122.79(12) . . . . ? C1B O1B Zn1B N1B 27.55(11) . . . . ? Zn1A O1B Zn1B N1B -101.01(4) . . . . ? C1B O1B Zn1B Zn1A 128.56(12) . . . . ? C1A O1A Zn1B O2B 115.80(9) . . . . ? Zn1A O1A Zn1B O2B -106.13(4) . . . . ? C1A O1A Zn1B O1B -144.30(9) . . . . ? Zn1A O1A Zn1B O1B -6.23(4) . . . . ? C1A O1A Zn1B N2B 20.50(10) . . . . ? Zn1A O1A Zn1B N2B 158.57(4) . . . . ? C1A O1A Zn1B N1B -61.27(10) . . . . ? Zn1A O1A Zn1B N1B 76.80(5) . . . . ? C1A O1A Zn1B Zn1A -138.07(11) . . . . ? C14B N2B Zn1B O2B -1.41(12) . . . . ? C13B N2B Zn1B O2B 171.15(9) . . . . ? C14B N2B Zn1B O1B -131.55(13) . . . . ? C13B N2B Zn1B O1B 41.01(18) . . . . ? C14B N2B Zn1B O1A 102.66(11) . . . . ? C13B N2B Zn1B O1A -84.78(9) . . . . ? C14B N2B Zn1B N1B -153.79(12) . . . . ? C13B N2B Zn1B N1B 18.77(9) . . . . ? C14B N2B Zn1B Zn1A 127.35(10) . . . . ? C13B N2B Zn1B Zn1A -60.09(11) . . . . ? C7B N1B Zn1B O2B 82.87(15) . . . . ? C8B N1B Zn1B O2B -87.79(13) . . . . ? C7B N1B Zn1B O1B -20.57(13) . . . . ? C8B N1B Zn1B O1B 168.77(10) . . . . ? C7B N1B Zn1B O1A -102.91(13) . . . . ? C8B N1B Zn1B O1A 86.43(10) . . . . ? C7B N1B Zn1B N2B 152.42(13) . . . . ? C8B N1B Zn1B N2B -18.24(9) . . . . ? C7B N1B Zn1B Zn1A -62.47(13) . . . . ? C8B N1B Zn1B Zn1A 126.87(9) . . . . ? O2A Zn1A Zn1B O2B 10.55(5) . . . . ? O1A Zn1A Zn1B O2B 86.85(5) . . . . ? O1B Zn1A Zn1B O2B -84.00(5) . . . . ? N2A Zn1A Zn1B O2B -123.77(6) . . . . ? N1A Zn1A Zn1B O2B 168.74(5) . . . . ? O2A Zn1A Zn1B O1B 94.55(5) . . . . ? O1A Zn1A Zn1B O1B 170.85(6) . . . . ? N2A Zn1A Zn1B O1B -39.77(7) . . . . ? N1A Zn1A Zn1B O1B -107.25(5) . . . . ? O2A Zn1A Zn1B O1A -76.30(5) . . . . ? O1B Zn1A Zn1B O1A -170.85(6) . . . . ? N2A Zn1A Zn1B O1A 149.38(7) . . . . ? N1A Zn1A Zn1B O1A 81.90(5) . . . . ? O2A Zn1A Zn1B N2B -113.15(7) . . . . ? O1A Zn1A Zn1B N2B -36.84(7) . . . . ? O1B Zn1A Zn1B N2B 152.30(7) . . . . ? N2A Zn1A Zn1B N2B 112.53(8) . . . . ? N1A Zn1A Zn1B N2B 45.05(6) . . . . ? O2A Zn1A Zn1B N1B 173.07(5) . . . . ? O1A Zn1A Zn1B N1B -110.63(5) . . . . ? O1B Zn1A Zn1B N1B 78.52(5) . . . . ? N2A Zn1A Zn1B N1B 38.75(6) . . . . ? N1A Zn1A Zn1B N1B -28.73(5) . . . . ? _diffrn_measured_fraction_theta_max 0.937 _diffrn_reflns_theta_full 39.31 _diffrn_measured_fraction_theta_full 0.937 _refine_diff_density_max 0.788 _refine_diff_density_min -0.427 _refine_diff_density_rms 0.078 # Attachment 'AWK539_01_P-1X1.cif' data_awk539_01_p-1 _database_code_depnum_ccdc_archive 'CCDC 755297' #TrackingRef 'AWK539_01_P-1X1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H66 N6 O4 Zn2' _chemical_formula_weight 1065.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2145(13) _cell_length_b 12.2716(7) _cell_length_c 12.7552(8) _cell_angle_alpha 114.879(2) _cell_angle_beta 97.484(3) _cell_angle_gamma 105.221(2) _cell_volume 1345.6(2) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9908 _cell_measurement_theta_min 2.76 _cell_measurement_theta_max 35.01 _exptl_crystal_description BLOCK _exptl_crystal_colour yellow _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.315 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 560 _exptl_absorpt_coefficient_mu 0.944 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7860 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_process_details ; SADABS Version 2008/1 Bruker-Nonius Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_special_details ; It should be noted that the esd's of the cell dimensions are probably too low; they should be multiplied by a factor of 2 to 10 ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_specimen_suppport 'magnetic support whith 10 micron nylon fiber cryoloop' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'rotating anode X-ray tube' _diffrn_source_type 'Bruker-Nonius FR 591' _diffrn_source_power 50 _diffrn_source_current 70 _diffrn_source_size '3 mm x 0.3 mm fine focus' _diffrn_radiation_monochromator 'Multilayer Montel 200 mirrors' _diffrn_detector_type '4K CCD area detector APEX II' _diffrn_measurement_device_type 'Kappa 4-axis goniometer bruker-nonius' _diffrn_measurement_method ; Fullsphere data collection, phi and omega scans ; _diffrn_detector_area_resol_mean 512 _diffrn_reflns_number 25611 _diffrn_reflns_av_R_equivalents 0.0204 _diffrn_reflns_av_sigmaI/netI 0.0242 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.75 _diffrn_reflns_theta_max 34.98 _reflns_number_total 10750 _reflns_number_gt 9839 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v2009.1-0' _computing_cell_refinement 'Bruker APEX2 v2009.1-0' _computing_data_reduction 'Bruker SAINT V7.60A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXS-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0407P)^2^+0.3841P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10750 _refine_ls_number_parameters 332 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0305 _refine_ls_R_factor_gt 0.0267 _refine_ls_wR_factor_ref 0.0752 _refine_ls_wR_factor_gt 0.0728 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.64135(9) 0.09939(7) 0.84594(7) 0.01367(13) Uani 1 1 d . . . C2 C 0.64156(9) 0.20616(7) 0.95319(7) 0.01513(14) Uani 1 1 d . . . C3 C 0.58069(11) 0.30435(8) 0.94350(7) 0.01827(16) Uani 1 1 d . . . C4 C 0.58590(16) 0.40621(11) 1.06763(9) 0.0332(3) Uani 1 1 d . . . H4A H 0.5445 0.4663 1.0584 0.050 Uiso 1 1 calc R . . H4B H 0.6842 0.4531 1.1166 0.050 Uiso 1 1 calc R . . H4C H 0.5324 0.3644 1.1072 0.050 Uiso 1 1 calc R . . C5 C 0.66815(13) 0.37187(10) 0.88450(10) 0.0270(2) Uani 1 1 d . . . H5A H 0.6636 0.3082 0.8040 0.041 Uiso 1 1 calc R . . H5B H 0.7665 0.4155 0.9336 0.041 Uiso 1 1 calc R . . H5C H 0.6301 0.4350 0.8783 0.041 Uiso 1 1 calc R . . C6 C 0.42449(12) 0.23915(10) 0.86942(10) 0.0262(2) Uani 1 1 d . . . H6A H 0.3694 0.1973 0.9083 0.039 Uiso 1 1 calc R . . H6B H 0.4166 0.1748 0.7882 0.039 Uiso 1 1 calc R . . H6C H 0.3883 0.3039 0.8648 0.039 Uiso 1 1 calc R . . C7 C 0.70091(10) 0.21950(8) 1.06397(7) 0.01583(14) Uani 1 1 d . . . H7 H 0.6990 0.2897 1.1337 0.019 Uiso 1 1 calc R . . C8 C 0.76409(9) 0.13629(8) 1.08087(7) 0.01402(13) Uani 1 1 d . . . C9 C 0.82166(9) 0.16083(8) 1.20915(7) 0.01510(13) Uani 1 1 d . . . C10 C 0.90683(10) 0.07499(9) 1.21141(8) 0.01978(16) Uani 1 1 d . . . H10A H 0.9460 0.0962 1.2948 0.030 Uiso 1 1 calc R . . H10B H 0.9839 0.0894 1.1748 0.030 Uiso 1 1 calc R . . H10C H 0.8448 -0.0153 1.1661 0.030 Uiso 1 1 calc R . . C11 C 0.69734(11) 0.13201(10) 1.26084(9) 0.02281(17) Uani 1 1 d . . . H11A H 0.6448 0.1890 1.2634 0.034 Uiso 1 1 calc R . . H11B H 0.7330 0.1461 1.3424 0.034 Uiso 1 1 calc R . . H11C H 0.6347 0.0425 1.2098 0.034 Uiso 1 1 calc R . . C12 C 0.91809(10) 0.30228(8) 1.29051(8) 0.01968(16) Uani 1 1 d . . . H12A H 0.8637 0.3582 1.2945 0.030 Uiso 1 1 calc R . . H12B H 0.9966 0.3229 1.2573 0.030 Uiso 1 1 calc R . . H12C H 0.9552 0.3156 1.3715 0.030 Uiso 1 1 calc R . . C13 C 0.76186(9) 0.03308(8) 0.97836(7) 0.01472(13) Uani 1 1 d . . . H13 H 0.8018 -0.0258 0.9860 0.018 Uiso 1 1 calc R . . C14 C 0.70141(9) 0.01201(7) 0.86121(7) 0.01392(13) Uani 1 1 d . . . C15 C 0.69779(9) -0.10429(7) 0.76314(7) 0.01444(13) Uani 1 1 d . . . H15 H 0.7357 -0.1583 0.7830 0.017 Uiso 1 1 calc R . . C16 C 0.63934(9) -0.26415(7) 0.56167(7) 0.01425(13) Uani 1 1 d . . . C17 C 0.73714(10) -0.32261(8) 0.57013(8) 0.01753(15) Uani 1 1 d . . . H17 H 0.8173 -0.2796 0.6380 0.021 Uiso 1 1 calc R . . C18 C 0.71741(11) -0.44415(9) 0.47903(8) 0.01969(16) Uani 1 1 d . . . H18 H 0.7840 -0.4841 0.4850 0.024 Uiso 1 1 calc R . . C19 C 0.60001(11) -0.50749(8) 0.37880(8) 0.02052(16) Uani 1 1 d . . . H19 H 0.5862 -0.5911 0.3177 0.025 Uiso 1 1 calc R . . C20 C 0.50328(11) -0.44890(8) 0.36792(8) 0.01893(15) Uani 1 1 d . . . H20 H 0.4248 -0.4914 0.2987 0.023 Uiso 1 1 calc R . . C21 C 0.52216(9) -0.32711(7) 0.45927(7) 0.01506(13) Uani 1 1 d . . . C22 C 0.29826(10) -0.31651(8) 0.40504(8) 0.01726(15) Uani 1 1 d . . . H22 H 0.2641 -0.4077 0.3668 0.021 Uiso 1 1 calc R . . C23 C 0.87780(10) 0.07633(9) 0.57944(9) 0.02016(16) Uani 1 1 d . . . H23 H 0.8559 -0.0123 0.5559 0.024 Uiso 1 1 calc R . . C24 C 1.01685(10) 0.15878(10) 0.63270(10) 0.02464(18) Uani 1 1 d . . . H24 H 1.0887 0.1258 0.6445 0.030 Uiso 1 1 calc R . . C25 C 1.05284(11) 0.28998(11) 0.66932(10) 0.02608(19) Uani 1 1 d . . . H25 H 1.1486 0.3458 0.7031 0.031 Uiso 1 1 calc R . . C26 C 0.94629(10) 0.33667(9) 0.65542(9) 0.02299(18) Uani 1 1 d . . . H26 H 0.9698 0.4261 0.6827 0.028 Uiso 1 1 calc R . . C27 C 0.80320(9) 0.25513(8) 0.60176(8) 0.01661(14) Uani 1 1 d . . . C28 C 0.76814(9) 0.12088(8) 0.55945(7) 0.01492(13) Uani 1 1 d . . . N1 N 0.64721(8) -0.14258(6) 0.64922(6) 0.01423(12) Uani 1 1 d . . . N2 N 0.43161(8) -0.25752(7) 0.45888(6) 0.01500(12) Uani 1 1 d . . . O1 O 0.58622(7) 0.08572(6) 0.74139(5) 0.01658(11) Uani 1 1 d . . . O2 O 0.63733(7) 0.03678(6) 0.50240(5) 0.01425(10) Uani 1 1 d . . . Zn1 Zn 0.532628(10) -0.059270(8) 0.580420(8) 0.01255(3) Uani 1 1 d . . . C1N C 0.12474(13) 0.29269(11) 0.04839(10) 0.0278(2) Uani 1 1 d . . . N1N N 0.20370(14) 0.30378(13) 0.12674(12) 0.0422(3) Uani 1 1 d . . . C2N C 0.02321(16) 0.27669(16) -0.05292(14) 0.0448(4) Uani 1 1 d . . . H2N1 H -0.0073 0.1883 -0.1180 0.067 Uiso 1 1 calc R . . H2N2 H 0.0672 0.3362 -0.0814 0.067 Uiso 1 1 calc R . . H2N3 H -0.0587 0.2948 -0.0277 0.067 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 C1 0.0166(3) 0.0120(3) 0.0110(3) 0.0046(2) 0.0022(2) 0.0051(2) C2 0.0210(4) 0.0128(3) 0.0109(3) 0.0045(2) 0.0027(3) 0.0078(3) C3 0.0289(4) 0.0147(3) 0.0115(3) 0.0047(3) 0.0027(3) 0.0120(3) C4 0.0615(8) 0.0271(5) 0.0142(4) 0.0051(3) 0.0047(4) 0.0312(5) C5 0.0378(6) 0.0187(4) 0.0274(5) 0.0138(3) 0.0070(4) 0.0103(4) C6 0.0276(5) 0.0233(4) 0.0270(5) 0.0089(4) 0.0032(4) 0.0152(4) C7 0.0219(4) 0.0145(3) 0.0107(3) 0.0045(2) 0.0032(3) 0.0089(3) C8 0.0167(3) 0.0141(3) 0.0108(3) 0.0053(2) 0.0026(2) 0.0064(2) C9 0.0176(3) 0.0154(3) 0.0109(3) 0.0056(2) 0.0018(2) 0.0059(3) C10 0.0227(4) 0.0195(3) 0.0163(3) 0.0081(3) 0.0004(3) 0.0093(3) C11 0.0231(4) 0.0304(4) 0.0198(4) 0.0153(3) 0.0083(3) 0.0097(3) C12 0.0215(4) 0.0168(3) 0.0148(3) 0.0040(3) 0.0000(3) 0.0062(3) C13 0.0176(3) 0.0138(3) 0.0118(3) 0.0052(2) 0.0020(2) 0.0068(2) C14 0.0171(3) 0.0126(3) 0.0106(3) 0.0041(2) 0.0022(2) 0.0062(2) C15 0.0167(3) 0.0133(3) 0.0118(3) 0.0044(2) 0.0025(2) 0.0065(2) C16 0.0178(3) 0.0123(3) 0.0110(3) 0.0042(2) 0.0037(2) 0.0053(2) C17 0.0208(4) 0.0160(3) 0.0146(3) 0.0050(3) 0.0047(3) 0.0085(3) C18 0.0273(4) 0.0172(3) 0.0164(3) 0.0063(3) 0.0080(3) 0.0122(3) C19 0.0312(5) 0.0147(3) 0.0139(3) 0.0039(3) 0.0066(3) 0.0101(3) C20 0.0263(4) 0.0138(3) 0.0120(3) 0.0029(3) 0.0029(3) 0.0067(3) C21 0.0197(3) 0.0123(3) 0.0112(3) 0.0044(2) 0.0031(3) 0.0050(3) C22 0.0191(4) 0.0139(3) 0.0141(3) 0.0055(3) 0.0009(3) 0.0024(3) C23 0.0164(4) 0.0218(4) 0.0201(4) 0.0082(3) 0.0039(3) 0.0071(3) C24 0.0159(4) 0.0295(4) 0.0248(4) 0.0107(4) 0.0034(3) 0.0073(3) C25 0.0156(4) 0.0283(4) 0.0270(4) 0.0118(4) 0.0008(3) 0.0013(3) C26 0.0181(4) 0.0206(4) 0.0229(4) 0.0098(3) -0.0004(3) -0.0005(3) C27 0.0156(3) 0.0157(3) 0.0145(3) 0.0067(3) 0.0010(3) 0.0018(3) C28 0.0148(3) 0.0163(3) 0.0115(3) 0.0060(2) 0.0030(2) 0.0035(2) N1 0.0168(3) 0.0118(2) 0.0110(3) 0.0030(2) 0.0023(2) 0.0052(2) N2 0.0179(3) 0.0131(3) 0.0115(3) 0.0048(2) 0.0017(2) 0.0045(2) O1 0.0244(3) 0.0143(2) 0.0094(2) 0.00435(19) 0.0014(2) 0.0081(2) O2 0.0142(2) 0.0137(2) 0.0121(2) 0.00546(19) 0.00149(19) 0.00291(19) Zn1 0.01531(5) 0.01072(4) 0.00924(4) 0.00383(3) 0.00131(3) 0.00359(3) C1N 0.0283(5) 0.0275(4) 0.0272(5) 0.0150(4) 0.0079(4) 0.0059(4) N1N 0.0406(6) 0.0439(6) 0.0414(6) 0.0260(5) 0.0018(5) 0.0086(5) C2N 0.0343(6) 0.0555(8) 0.0403(7) 0.0319(7) -0.0032(5) 0.0005(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.3001(9) . ? C1 C14 1.4333(11) . ? C1 C2 1.4415(11) . ? C2 C7 1.3861(11) . ? C2 C3 1.5338(11) . ? C3 C4 1.5330(13) . ? C3 C5 1.5370(15) . ? C3 C6 1.5425(14) . ? C7 C8 1.4144(11) . ? C8 C13 1.3777(11) . ? C8 C9 1.5347(11) . ? C9 C11 1.5333(14) . ? C9 C10 1.5387(12) . ? C9 C12 1.5429(12) . ? C13 C14 1.4253(11) . ? C14 C15 1.4357(11) . ? C15 N1 1.3044(10) . ? C16 C17 1.3920(12) . ? C16 N1 1.4111(11) . ? C16 C21 1.4120(11) . ? C17 C18 1.3922(12) . ? C18 C19 1.3971(13) . ? C19 C20 1.3907(13) . ? C20 C21 1.3977(12) . ? C21 N2 1.4148(11) . ? C22 N2 1.2928(11) . ? C22 C27 1.4458(13) 2_656 ? C23 C24 1.3851(13) . ? C23 C28 1.4082(12) . ? C24 C25 1.3989(16) . ? C25 C26 1.3809(15) . ? C26 C27 1.4147(12) . ? C27 C28 1.4231(12) . ? C27 C22 1.4459(13) 2_656 ? C28 O2 1.3307(10) . ? N1 Zn1 2.0738(7) . ? N2 Zn1 2.1162(7) . ? O1 Zn1 1.9501(6) . ? O2 Zn1 2.0311(7) . ? O2 Zn1 2.0555(6) 2_656 ? Zn1 O2 2.0555(6) 2_656 ? Zn1 Zn1 3.0714(2) 2_656 ? C1N N1N 1.1339(16) . ? C1N C2N 1.4541(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 C14 123.33(7) . . ? O1 C1 C2 119.37(7) . . ? C14 C1 C2 117.29(7) . . ? C7 C2 C1 118.67(7) . . ? C7 C2 C3 121.26(7) . . ? C1 C2 C3 120.05(7) . . ? C4 C3 C2 111.35(7) . . ? C4 C3 C5 108.51(9) . . ? C2 C3 C5 108.98(8) . . ? C4 C3 C6 106.73(9) . . ? C2 C3 C6 111.16(7) . . ? C5 C3 C6 110.06(8) . . ? C2 C7 C8 124.84(8) . . ? C13 C8 C7 116.48(7) . . ? C13 C8 C9 124.40(7) . . ? C7 C8 C9 119.01(7) . . ? C11 C9 C8 108.86(7) . . ? C11 C9 C10 108.72(8) . . ? C8 C9 C10 111.60(7) . . ? C11 C9 C12 108.49(8) . . ? C8 C9 C12 110.73(7) . . ? C10 C9 C12 108.37(7) . . ? C8 C13 C14 122.00(7) . . ? C13 C14 C1 120.69(7) . . ? C13 C14 C15 115.66(7) . . ? C1 C14 C15 123.54(7) . . ? N1 C15 C14 125.91(7) . . ? C17 C16 N1 124.86(7) . . ? C17 C16 C21 119.83(7) . . ? N1 C16 C21 115.31(7) . . ? C16 C17 C18 119.95(8) . . ? C17 C18 C19 120.21(8) . . ? C20 C19 C18 120.40(8) . . ? C19 C20 C21 119.66(8) . . ? C20 C21 C16 119.91(8) . . ? C20 C21 N2 125.09(7) . . ? C16 C21 N2 114.99(7) . . ? N2 C22 C27 125.35(8) . 2_656 ? C24 C23 C28 121.49(9) . . ? C23 C24 C25 120.81(9) . . ? C26 C25 C24 118.66(9) . . ? C25 C26 C27 121.90(9) . . ? C26 C27 C28 119.09(8) . . ? C26 C27 C22 116.37(8) . 2_656 ? C28 C27 C22 124.53(8) . 2_656 ? O2 C28 C23 119.13(8) . . ? O2 C28 C27 122.95(8) . . ? C23 C28 C27 117.92(8) . . ? C15 N1 C16 120.34(7) . . ? C15 N1 Zn1 125.34(6) . . ? C16 N1 Zn1 112.88(5) . . ? C22 N2 C21 120.79(7) . . ? C22 N2 Zn1 126.38(6) . . ? C21 N2 Zn1 111.77(5) . . ? C1 O1 Zn1 131.16(5) . . ? C28 O2 Zn1 120.24(5) . . ? C28 O2 Zn1 128.62(5) . 2_656 ? Zn1 O2 Zn1 97.45(3) . 2_656 ? O1 Zn1 O2 97.51(3) . . ? O1 Zn1 O2 101.00(3) . 2_656 ? O2 Zn1 O2 82.55(3) . 2_656 ? O1 Zn1 N1 88.95(3) . . ? O2 Zn1 N1 114.33(3) . . ? O2 Zn1 N1 159.34(3) 2_656 . ? O1 Zn1 N2 150.63(3) . . ? O2 Zn1 N2 111.76(3) . . ? O2 Zn1 N2 85.65(3) 2_656 . ? N1 Zn1 N2 77.16(3) . . ? O1 Zn1 Zn1 102.366(19) . 2_656 ? O2 Zn1 Zn1 41.575(18) . 2_656 ? O2 Zn1 Zn1 40.976(18) 2_656 2_656 ? N1 Zn1 Zn1 153.98(2) . 2_656 ? N2 Zn1 Zn1 101.21(2) . 2_656 ? N1N C1N C2N 179.24(15) . . ? 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 C1 C2 C7 -179.91(8) . . . . ? C14 C1 C2 C7 0.92(13) . . . . ? O1 C1 C2 C3 -1.61(13) . . . . ? C14 C1 C2 C3 179.21(8) . . . . ? C7 C2 C3 C4 -4.12(14) . . . . ? C1 C2 C3 C4 177.63(10) . . . . ? C7 C2 C3 C5 115.55(10) . . . . ? C1 C2 C3 C5 -62.71(11) . . . . ? C7 C2 C3 C6 -122.99(10) . . . . ? C1 C2 C3 C6 58.76(12) . . . . ? C1 C2 C7 C8 0.84(14) . . . . ? C3 C2 C7 C8 -177.44(9) . . . . ? C2 C7 C8 C13 -1.84(14) . . . . ? C2 C7 C8 C9 -178.19(9) . . . . ? C13 C8 C9 C11 -106.97(10) . . . . ? C7 C8 C9 C11 69.07(10) . . . . ? C13 C8 C9 C10 13.02(12) . . . . ? C7 C8 C9 C10 -170.94(8) . . . . ? C13 C8 C9 C12 133.84(9) . . . . ? C7 C8 C9 C12 -50.12(11) . . . . ? C7 C8 C13 C14 1.06(13) . . . . ? C9 C8 C13 C14 177.19(8) . . . . ? C8 C13 C14 C1 0.63(13) . . . . ? C8 C13 C14 C15 -175.74(8) . . . . ? O1 C1 C14 C13 179.24(8) . . . . ? C2 C1 C14 C13 -1.62(13) . . . . ? O1 C1 C14 C15 -4.69(14) . . . . ? C2 C1 C14 C15 174.45(8) . . . . ? C13 C14 C15 N1 179.87(9) . . . . ? C1 C14 C15 N1 3.62(15) . . . . ? N1 C16 C17 C18 178.86(9) . . . . ? C21 C16 C17 C18 -1.52(14) . . . . ? C16 C17 C18 C19 0.28(15) . . . . ? C17 C18 C19 C20 1.23(16) . . . . ? C18 C19 C20 C21 -1.47(15) . . . . ? C19 C20 C21 C16 0.23(14) . . . . ? C19 C20 C21 N2 179.96(9) . . . . ? C17 C16 C21 C20 1.26(13) . . . . ? N1 C16 C21 C20 -179.07(8) . . . . ? C17 C16 C21 N2 -178.49(8) . . . . ? N1 C16 C21 N2 1.17(11) . . . . ? C28 C23 C24 C25 0.46(17) . . . . ? C23 C24 C25 C26 2.37(17) . . . . ? C24 C25 C26 C27 -2.16(17) . . . . ? C25 C26 C27 C28 -0.83(15) . . . . ? C25 C26 C27 C22 178.72(10) . . . 2_656 ? C24 C23 C28 O2 176.57(9) . . . . ? C24 C23 C28 C27 -3.42(14) . . . . ? C26 C27 C28 O2 -176.43(9) . . . . ? C22 C27 C28 O2 4.06(14) 2_656 . . . ? C26 C27 C28 C23 3.57(13) . . . . ? C22 C27 C28 C23 -175.95(9) 2_656 . . . ? C14 C15 N1 C16 -174.78(8) . . . . ? C14 C15 N1 Zn1 -9.47(13) . . . . ? C17 C16 N1 C15 -34.86(13) . . . . ? C21 C16 N1 C15 145.49(9) . . . . ? C17 C16 N1 Zn1 158.11(7) . . . . ? C21 C16 N1 Zn1 -21.53(10) . . . . ? C27 C22 N2 C21 -179.45(8) 2_656 . . . ? C27 C22 N2 Zn1 13.32(13) 2_656 . . . ? C20 C21 N2 C22 30.46(14) . . . . ? C16 C21 N2 C22 -149.80(9) . . . . ? C20 C21 N2 Zn1 -160.59(8) . . . . ? C16 C21 N2 Zn1 19.15(9) . . . . ? C14 C1 O1 Zn1 12.99(13) . . . . ? C2 C1 O1 Zn1 -166.14(7) . . . . ? C23 C28 O2 Zn1 67.09(10) . . . . ? C27 C28 O2 Zn1 -112.91(8) . . . . ? C23 C28 O2 Zn1 -161.78(7) . . . 2_656 ? C27 C28 O2 Zn1 18.22(12) . . . 2_656 ? C1 O1 Zn1 O2 -128.44(8) . . . . ? C1 O1 Zn1 O2 147.74(8) . . . 2_656 ? C1 O1 Zn1 N1 -14.03(8) . . . . ? C1 O1 Zn1 N2 46.90(11) . . . . ? C1 O1 Zn1 Zn1 -170.40(8) . . . 2_656 ? C28 O2 Zn1 O1 43.41(7) . . . . ? Zn1 O2 Zn1 O1 -100.19(3) 2_656 . . . ? C28 O2 Zn1 O2 143.60(7) . . . 2_656 ? Zn1 O2 Zn1 O2 0.0 2_656 . . 2_656 ? C28 O2 Zn1 N1 -48.84(7) . . . . ? Zn1 O2 Zn1 N1 167.56(2) 2_656 . . . ? C28 O2 Zn1 N2 -134.13(6) . . . . ? Zn1 O2 Zn1 N2 82.27(3) 2_656 . . . ? C28 O2 Zn1 Zn1 143.59(7) . . . 2_656 ? C15 N1 Zn1 O1 11.79(8) . . . . ? C16 N1 Zn1 O1 178.05(6) . . . . ? C15 N1 Zn1 O2 109.56(8) . . . . ? C16 N1 Zn1 O2 -84.18(6) . . . . ? C15 N1 Zn1 O2 -107.70(9) . . . 2_656 ? C16 N1 Zn1 O2 58.56(11) . . . 2_656 ? C15 N1 Zn1 N2 -142.12(8) . . . . ? C16 N1 Zn1 N2 24.14(6) . . . . ? C15 N1 Zn1 Zn1 128.58(7) . . . 2_656 ? C16 N1 Zn1 Zn1 -65.16(8) . . . 2_656 ? C22 N2 Zn1 O1 81.20(9) . . . . ? C21 N2 Zn1 O1 -87.00(8) . . . . ? C22 N2 Zn1 O2 -103.78(8) . . . . ? C21 N2 Zn1 O2 88.02(6) . . . . ? C22 N2 Zn1 O2 -23.59(8) . . . 2_656 ? C21 N2 Zn1 O2 168.21(6) . . . 2_656 ? C22 N2 Zn1 N1 144.87(8) . . . . ? C21 N2 Zn1 N1 -23.33(6) . . . . ? C22 N2 Zn1 Zn1 -61.69(8) . . . 2_656 ? C21 N2 Zn1 Zn1 130.11(5) . . . 2_656 ? _diffrn_measured_fraction_theta_max 0.909 _diffrn_reflns_theta_full 34.98 _diffrn_measured_fraction_theta_full 0.909 _refine_diff_density_max 0.536 _refine_diff_density_min -0.435 _refine_diff_density_rms 0.062 # Attachment 'AWK546t51.cif' data_awk546t5 _database_code_depnum_ccdc_archive 'CCDC 755298' #TrackingRef 'AWK546t51.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H70 N6 O4 Zn2' _chemical_formula_weight 1166.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.030(4) _cell_length_b 10.664(4) _cell_length_c 15.255(7) _cell_angle_alpha 79.508(8) _cell_angle_beta 75.796(9) _cell_angle_gamma 75.139(14) _cell_volume 1516.6(11) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 315 _cell_measurement_theta_min 2.57 _cell_measurement_theta_max 24.22 _exptl_crystal_description neddle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.277 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 612 _exptl_absorpt_coefficient_mu 0.844 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9512 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ; TWINABS Version 2008/4 Bruker AXS Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_special_details ; It should be noted that the esd's of the cell dimensions are probably too low; they should be multiplied by a factor of 2 to 10 ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_specimen_suppport 'magnetic support whith 10 micron nylon fiber cryoloop' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'rotating anode X-ray tube' _diffrn_source_type 'Bruker-Nonius FR 591' _diffrn_source_power 50 _diffrn_source_current 70 _diffrn_source_size '3 mm x 0.3 mm fine focus' _diffrn_radiation_monochromator 'Multilayer Montel 200 mirrors' _diffrn_detector_type '4K CCD area detector APEX II' _diffrn_measurement_device_type 'Kappa 4-axis goniometer bruker-nonius' _diffrn_measurement_method ; Fullsphere data collection, phi and omega scans ; _diffrn_detector_area_resol_mean 512 _diffrn_reflns_number 6766 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0731 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 28.65 _reflns_number_total 6766 _reflns_number_gt 5401 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v2009.1-0' _computing_cell_refinement 'Bruker APEX2 v2009.1-0' _computing_data_reduction 'Bruker SAINT V7.60A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXS-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0754P)^2^+1.0920P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6766 _refine_ls_number_parameters 369 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0820 _refine_ls_R_factor_gt 0.0570 _refine_ls_wR_factor_ref 0.1414 _refine_ls_wR_factor_gt 0.1291 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _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 0.49391(5) 0.01366(5) 0.39836(3) 0.01556(12) Uani 1 1 d . . . O1 O 0.6198(3) -0.1458(3) 0.35089(18) 0.0198(6) Uani 1 1 d . . . N1 N 0.5317(3) 0.1152(3) 0.2676(2) 0.0188(7) Uani 1 1 d . . . C1 C 0.6637(4) -0.1741(4) 0.2664(3) 0.0189(8) Uani 1 1 d . . . N2 N 0.3226(3) 0.1795(3) 0.4042(2) 0.0162(6) Uani 1 1 d . . . C2 C 0.7291(4) -0.3072(4) 0.2489(3) 0.0204(9) Uani 1 1 d . . . O2 O 0.3828(3) -0.0512(3) 0.52288(18) 0.0163(6) Uani 1 1 d . . . C3 C 0.7646(4) -0.3346(4) 0.1587(3) 0.0200(8) Uani 1 1 d . . . H3A H 0.8068 -0.4226 0.1482 0.024 Uiso 1 1 calc R . . C4 C 0.7424(5) -0.2412(4) 0.0818(3) 0.0214(9) Uani 1 1 d . . . C5 C 0.6852(5) -0.1132(4) 0.0979(3) 0.0222(9) Uani 1 1 d . . . H5A H 0.6704 -0.0477 0.0478 0.027 Uiso 1 1 calc R . . C6 C 0.6475(4) -0.0764(4) 0.1881(3) 0.0201(8) Uani 1 1 d . . . C7 C 0.5864(4) 0.0601(4) 0.1930(3) 0.0199(9) Uani 1 1 d . . . H7A H 0.5856 0.1157 0.1368 0.024 Uiso 1 1 calc R . . C8 C 0.4686(4) 0.2506(4) 0.2622(3) 0.0191(8) Uani 1 1 d . . . C9 C 0.5112(5) 0.3472(4) 0.1930(3) 0.0243(9) Uani 1 1 d . . . H9A H 0.5894 0.3241 0.1447 0.029 Uiso 1 1 calc R . . C10 C 0.4384(5) 0.4772(5) 0.1954(3) 0.0283(10) Uani 1 1 d . . . H10A H 0.4663 0.5427 0.1482 0.034 Uiso 1 1 calc R . . C11 C 0.3235(5) 0.5116(5) 0.2677(3) 0.0283(10) Uani 1 1 d . . . H11A H 0.2733 0.6001 0.2688 0.034 Uiso 1 1 calc R . . C12 C 0.2833(5) 0.4159(4) 0.3377(3) 0.0223(9) Uani 1 1 d . . . H12A H 0.2075 0.4403 0.3871 0.027 Uiso 1 1 calc R . . C13 C 0.3533(4) 0.2846(4) 0.3359(3) 0.0183(8) Uani 1 1 d . . . C14 C 0.1937(4) 0.1839(4) 0.4518(2) 0.0154(8) Uani 1 1 d . . . H14A H 0.1230 0.2574 0.4363 0.019 Uiso 1 1 calc R . . C15 C 0.1489(4) 0.0882(4) 0.5254(2) 0.0150(7) Uani 1 1 d . . . C16 C -0.0004(4) 0.1108(4) 0.5713(3) 0.0175(8) Uani 1 1 d . . . C17 C -0.1042(4) 0.2219(4) 0.5453(3) 0.0209(9) Uani 1 1 d . . . H17A H -0.0770 0.2841 0.4953 0.025 Uiso 1 1 calc R . . C18 C -0.2449(4) 0.2408(5) 0.5919(3) 0.0273(9) Uani 1 1 d . . . H18A H -0.3114 0.3161 0.5736 0.033 Uiso 1 1 calc R . . C19 C -0.2896(5) 0.1499(5) 0.6657(3) 0.0265(9) Uani 1 1 d . . . H19A H -0.3854 0.1638 0.6972 0.032 Uiso 1 1 calc R . . C20 C -0.1933(4) 0.0413(5) 0.6917(3) 0.0235(9) Uani 1 1 d . . . H20A H -0.2238 -0.0204 0.7411 0.028 Uiso 1 1 calc R . . C21 C -0.0478(4) 0.0185(4) 0.6460(3) 0.0182(8) Uani 1 1 d . . . C22 C 0.0513(5) -0.0931(4) 0.6747(3) 0.0229(9) Uani 1 1 d . . . H22A H 0.0201 -0.1547 0.7239 0.027 Uiso 1 1 calc R . . C23 C 0.1922(4) -0.1140(4) 0.6323(3) 0.0198(8) Uani 1 1 d . . . H23A H 0.2562 -0.1895 0.6531 0.024 Uiso 1 1 calc R . . C24 C 0.2437(4) -0.0237(4) 0.5575(2) 0.0159(8) Uani 1 1 d . . . C25 C 0.7608(5) -0.4148(4) 0.3279(3) 0.0198(9) Uani 1 1 d . . . C26 C 0.6220(5) -0.4337(5) 0.3962(3) 0.0288(10) Uani 1 1 d . . . H26A H 0.5746 -0.3523 0.4223 0.043 Uiso 1 1 calc R . . H26B H 0.6442 -0.5040 0.4451 0.043 Uiso 1 1 calc R . . H26C H 0.5599 -0.4568 0.3641 0.043 Uiso 1 1 calc R . . C27 C 0.8602(5) -0.3799(5) 0.3786(3) 0.0266(10) Uani 1 1 d . . . H27A H 0.8125 -0.3003 0.4069 0.040 Uiso 1 1 calc R . . H27B H 0.9463 -0.3653 0.3351 0.040 Uiso 1 1 calc R . . H27C H 0.8848 -0.4521 0.4258 0.040 Uiso 1 1 calc R . . C28 C 0.8370(5) -0.5482(5) 0.2942(3) 0.0301(11) Uani 1 1 d . . . H28A H 0.9277 -0.5407 0.2537 0.045 Uiso 1 1 calc R . . H28B H 0.7785 -0.5743 0.2610 0.045 Uiso 1 1 calc R . . H28C H 0.8530 -0.6142 0.3466 0.045 Uiso 1 1 calc R . . C29 C 0.7843(5) -0.2827(5) -0.0154(3) 0.0255(10) Uani 1 1 d . . . C30 C 0.9471(6) -0.3139(6) -0.0433(3) 0.0384(13) Uani 1 1 d . . . H30A H 0.9866 -0.3808 0.0024 0.058 Uiso 1 1 calc R . . H30B H 0.9812 -0.2343 -0.0472 0.058 Uiso 1 1 calc R . . H30C H 0.9769 -0.3464 -0.1027 0.058 Uiso 1 1 calc R . . C31 C 0.7287(6) -0.4038(6) -0.0164(3) 0.0377(12) Uani 1 1 d . . . H31A H 0.7649 -0.4748 0.0282 0.057 Uiso 1 1 calc R . . H31B H 0.7604 -0.4315 -0.0773 0.057 Uiso 1 1 calc R . . H31C H 0.6254 -0.3822 -0.0006 0.057 Uiso 1 1 calc R . . C32 C 0.7246(8) -0.1744(6) -0.0853(3) 0.0477(16) Uani 1 1 d . . . H32A H 0.6217 -0.1503 -0.0663 0.072 Uiso 1 1 calc R . . H32B H 0.7501 -0.2059 -0.1450 0.072 Uiso 1 1 calc R . . H32C H 0.7638 -0.0978 -0.0894 0.072 Uiso 1 1 calc R . . C1S C 1.1831(7) -0.1967(7) 0.0826(4) 0.0498(15) Uani 1 1 d . . . N1S N 1.2864(7) -0.2191(7) 0.0320(4) 0.072(2) Uani 1 1 d . . . C2S C 1.0496(7) -0.1684(10) 0.1507(5) 0.077(3) Uani 1 1 d . . . H2S1 H 1.0704 -0.1789 0.2115 0.115 Uiso 1 1 calc R . . H2S2 H 0.9914 -0.2291 0.1499 0.115 Uiso 1 1 calc R . . H2S3 H 0.9986 -0.0784 0.1358 0.115 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0134(2) 0.0157(2) 0.01480(19) -0.0046(2) 0.00050(18) 0.00031(15) O1 0.0178(14) 0.0221(15) 0.0170(13) -0.0056(12) 0.0002(11) -0.0013(12) N1 0.0141(16) 0.0185(17) 0.0208(15) -0.0026(14) 0.0010(12) -0.0026(14) C1 0.0126(18) 0.025(2) 0.0192(18) -0.0075(17) -0.0025(14) -0.0022(17) N2 0.0135(15) 0.0178(15) 0.0157(14) -0.0011(14) -0.0020(13) -0.0023(12) C2 0.0161(19) 0.022(2) 0.0234(19) -0.0031(17) -0.0037(15) -0.0053(17) O2 0.0116(13) 0.0156(13) 0.0189(13) -0.0044(11) 0.0006(11) -0.0005(11) C3 0.018(2) 0.018(2) 0.0233(19) -0.0064(16) -0.0015(16) -0.0021(16) C4 0.021(2) 0.023(2) 0.0200(19) -0.0074(17) -0.0009(15) -0.0038(17) C5 0.023(2) 0.022(2) 0.0188(18) -0.0044(17) -0.0023(16) 0.0000(18) C6 0.0185(19) 0.020(2) 0.0180(18) -0.0003(16) 0.0001(15) -0.0033(16) C7 0.023(2) 0.020(2) 0.0155(17) -0.0041(16) -0.0031(14) -0.0022(18) C8 0.019(2) 0.018(2) 0.0201(18) -0.0038(16) -0.0024(15) -0.0040(17) C9 0.026(2) 0.024(2) 0.0208(19) -0.0035(17) 0.0015(16) -0.0081(18) C10 0.035(3) 0.022(2) 0.026(2) 0.0003(19) -0.0008(19) -0.010(2) C11 0.034(3) 0.018(2) 0.031(2) -0.0023(18) -0.0042(19) -0.0035(19) C12 0.023(2) 0.019(2) 0.0236(19) -0.0019(17) -0.0017(16) -0.0061(18) C13 0.0169(19) 0.023(2) 0.0159(17) -0.0015(16) -0.0019(14) -0.0075(17) C14 0.0145(18) 0.0148(18) 0.0146(16) -0.0032(14) -0.0024(14) 0.0014(15) C15 0.0170(18) 0.0159(18) 0.0140(16) -0.0036(14) -0.0013(14) -0.0074(15) C16 0.0141(19) 0.021(2) 0.0177(17) -0.0066(15) -0.0019(14) -0.0031(16) C17 0.017(2) 0.023(2) 0.0219(19) -0.0053(17) -0.0006(15) -0.0047(17) C18 0.0146(19) 0.032(2) 0.033(2) -0.010(2) -0.0041(18) 0.0007(17) C19 0.015(2) 0.037(3) 0.028(2) -0.014(2) 0.0014(16) -0.0064(19) C20 0.019(2) 0.031(2) 0.0222(19) -0.0074(18) 0.0037(16) -0.0131(18) C21 0.0150(19) 0.025(2) 0.0179(18) -0.0092(16) -0.0003(14) -0.0090(16) C22 0.027(2) 0.022(2) 0.0189(19) 0.0006(17) 0.0005(16) -0.0116(19) C23 0.020(2) 0.0167(19) 0.0197(18) -0.0014(15) -0.0033(15) -0.0012(17) C24 0.0136(18) 0.0194(19) 0.0148(17) -0.0078(15) 0.0000(14) -0.0030(15) C25 0.025(2) 0.0138(19) 0.0183(18) -0.0039(15) 0.0000(16) -0.0036(17) C26 0.025(2) 0.028(2) 0.029(2) 0.004(2) -0.004(2) -0.0064(18) C27 0.026(2) 0.026(2) 0.029(2) -0.0033(18) -0.0137(18) -0.0006(19) C28 0.043(3) 0.019(2) 0.025(2) -0.0043(18) -0.008(2) 0.000(2) C29 0.033(2) 0.023(2) 0.0180(18) -0.0071(17) -0.0030(17) -0.0015(19) C30 0.038(3) 0.041(3) 0.029(2) -0.016(2) 0.010(2) -0.007(2) C31 0.050(3) 0.035(3) 0.028(2) -0.014(2) -0.005(2) -0.008(3) C32 0.073(4) 0.039(3) 0.024(2) -0.012(2) -0.010(3) 0.004(3) C1S 0.052(4) 0.050(4) 0.045(3) 0.000(3) 0.002(3) -0.024(3) N1S 0.073(4) 0.066(4) 0.055(3) 0.004(3) 0.019(3) -0.014(3) C2S 0.053(4) 0.137(8) 0.058(4) -0.047(5) 0.015(3) -0.055(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 O1 1.977(3) . ? Zn1 O2 2.051(3) . ? Zn1 O2 2.072(3) 2_656 ? Zn1 N1 2.085(3) . ? Zn1 N2 2.124(3) . ? Zn1 Zn1 3.0911(17) 2_656 ? O1 C1 1.320(5) . ? N1 C7 1.309(5) . ? N1 C8 1.417(5) . ? C1 C2 1.446(6) . ? C1 C6 1.447(6) . ? N2 C14 1.312(5) . ? N2 C13 1.425(5) . ? C2 C3 1.400(6) . ? C2 C25 1.538(6) . ? O2 C24 1.340(5) . ? O2 Zn1 2.072(3) 2_656 ? C3 C4 1.416(6) . ? C4 C5 1.380(6) . ? C4 C29 1.552(6) . ? C5 C6 1.433(6) . ? C6 C7 1.435(6) . ? C8 C9 1.402(6) . ? C8 C13 1.424(5) . ? C9 C10 1.394(6) . ? C10 C11 1.410(6) . ? C11 C12 1.395(6) . ? C12 C13 1.399(6) . ? C14 C15 1.440(5) . ? C15 C24 1.415(6) . ? C15 C16 1.467(5) . ? C16 C17 1.430(6) . ? C16 C21 1.435(6) . ? C17 C18 1.397(6) . ? C18 C19 1.409(7) . ? C19 C20 1.370(7) . ? C20 C21 1.434(5) . ? C21 C22 1.418(6) . ? C22 C23 1.381(6) . ? C23 C24 1.436(6) . ? C25 C28 1.546(6) . ? C25 C27 1.550(7) . ? C25 C26 1.555(6) . ? C29 C32 1.530(7) . ? C29 C31 1.535(8) . ? C29 C30 1.547(7) . ? C1S N1S 1.128(8) . ? C1S C2S 1.479(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 O1 Zn1 O2 105.07(11) . . ? O1 Zn1 O2 99.44(12) . 2_656 ? O2 Zn1 O2 82.86(13) . 2_656 ? O1 Zn1 N1 89.21(12) . . ? O2 Zn1 N1 158.87(12) . . ? O2 Zn1 N1 110.52(13) 2_656 . ? O1 Zn1 N2 156.35(13) . . ? O2 Zn1 N2 84.28(12) . . ? O2 Zn1 N2 103.30(13) 2_656 . ? N1 Zn1 N2 76.87(13) . . ? O1 Zn1 Zn1 106.41(9) . 2_656 ? O2 Zn1 Zn1 41.68(9) . 2_656 ? O2 Zn1 Zn1 41.18(7) 2_656 2_656 ? N1 Zn1 Zn1 148.64(12) . 2_656 ? N2 Zn1 Zn1 95.05(9) . 2_656 ? C1 O1 Zn1 129.9(3) . . ? C7 N1 C8 120.0(4) . . ? C7 N1 Zn1 124.7(3) . . ? C8 N1 Zn1 114.3(3) . . ? O1 C1 C2 120.3(4) . . ? O1 C1 C6 122.6(4) . . ? C2 C1 C6 117.2(4) . . ? C14 N2 C13 120.4(3) . . ? C14 N2 Zn1 126.6(3) . . ? C13 N2 Zn1 112.0(2) . . ? C3 C2 C1 118.4(4) . . ? C3 C2 C25 121.3(4) . . ? C1 C2 C25 120.4(4) . . ? C24 O2 Zn1 129.8(2) . . ? C24 O2 Zn1 115.0(2) . 2_656 ? Zn1 O2 Zn1 97.14(13) . 2_656 ? C2 C3 C4 125.0(4) . . ? C5 C4 C3 116.8(4) . . ? C5 C4 C29 122.5(4) . . ? C3 C4 C29 120.7(4) . . ? C4 C5 C6 121.8(4) . . ? C5 C6 C7 114.7(4) . . ? C5 C6 C1 120.7(4) . . ? C7 C6 C1 124.5(4) . . ? N1 C7 C6 126.1(4) . . ? C9 C8 N1 125.6(4) . . ? C9 C8 C13 120.6(4) . . ? N1 C8 C13 113.8(4) . . ? C10 C9 C8 119.7(4) . . ? C9 C10 C11 120.1(4) . . ? C12 C11 C10 120.2(4) . . ? C11 C12 C13 120.7(4) . . ? C12 C13 C8 118.7(4) . . ? C12 C13 N2 125.4(4) . . ? C8 C13 N2 115.8(4) . . ? N2 C14 C15 126.3(3) . . ? C24 C15 C14 122.8(3) . . ? C24 C15 C16 118.7(3) . . ? C14 C15 C16 118.4(3) . . ? C17 C16 C21 117.1(4) . . ? C17 C16 C15 123.2(4) . . ? C21 C16 C15 119.8(3) . . ? C18 C17 C16 121.3(4) . . ? C17 C18 C19 121.0(4) . . ? C20 C19 C18 119.3(4) . . ? C19 C20 C21 121.5(4) . . ? C22 C21 C20 121.0(4) . . ? C22 C21 C16 119.2(4) . . ? C20 C21 C16 119.8(4) . . ? C23 C22 C21 121.2(4) . . ? C22 C23 C24 121.2(4) . . ? O2 C24 C15 123.7(4) . . ? O2 C24 C23 116.5(3) . . ? C15 C24 C23 119.8(3) . . ? C2 C25 C28 112.2(3) . . ? C2 C25 C27 110.5(4) . . ? C28 C25 C27 106.3(4) . . ? C2 C25 C26 110.7(3) . . ? C28 C25 C26 107.5(4) . . ? C27 C25 C26 109.6(4) . . ? C32 C29 C31 107.6(5) . . ? C32 C29 C30 108.8(4) . . ? C31 C29 C30 110.1(4) . . ? C32 C29 C4 112.1(4) . . ? C31 C29 C4 110.5(4) . . ? C30 C29 C4 107.7(4) . . ? N1S C1S C2S 178.6(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 O2 Zn1 O1 C1 145.6(4) . . . . ? O2 Zn1 O1 C1 -129.3(4) 2_656 . . . ? N1 Zn1 O1 C1 -18.6(4) . . . . ? N2 Zn1 O1 C1 34.7(6) . . . . ? Zn1 Zn1 O1 C1 -171.0(3) 2_656 . . . ? O1 Zn1 N1 C7 16.0(4) . . . . ? O2 Zn1 N1 C7 -117.3(4) . . . . ? O2 Zn1 N1 C7 115.8(3) 2_656 . . . ? N2 Zn1 N1 C7 -144.7(4) . . . . ? Zn1 Zn1 N1 C7 137.4(3) 2_656 . . . ? O1 Zn1 N1 C8 -175.6(3) . . . . ? O2 Zn1 N1 C8 51.1(6) . . . . ? O2 Zn1 N1 C8 -75.9(3) 2_656 . . . ? N2 Zn1 N1 C8 23.6(3) . . . . ? Zn1 Zn1 N1 C8 -54.3(4) 2_656 . . . ? Zn1 O1 C1 C2 -165.8(3) . . . . ? Zn1 O1 C1 C6 13.3(6) . . . . ? O1 Zn1 N2 C14 91.3(4) . . . . ? O2 Zn1 N2 C14 -23.7(3) . . . . ? O2 Zn1 N2 C14 -105.0(3) 2_656 . . . ? N1 Zn1 N2 C14 146.7(4) . . . . ? Zn1 Zn1 N2 C14 -64.0(3) 2_656 . . . ? O1 Zn1 N2 C13 -77.3(4) . . . . ? O2 Zn1 N2 C13 167.7(3) . . . . ? O2 Zn1 N2 C13 86.4(3) 2_656 . . . ? N1 Zn1 N2 C13 -21.9(3) . . . . ? Zn1 Zn1 N2 C13 127.4(3) 2_656 . . . ? O1 C1 C2 C3 175.4(4) . . . . ? C6 C1 C2 C3 -3.8(6) . . . . ? O1 C1 C2 C25 -5.7(6) . . . . ? C6 C1 C2 C25 175.2(4) . . . . ? O1 Zn1 O2 C24 -131.0(3) . . . . ? O2 Zn1 O2 C24 131.1(4) 2_656 . . . ? N1 Zn1 O2 C24 0.1(6) . . . . ? N2 Zn1 O2 C24 26.9(3) . . . . ? Zn1 Zn1 O2 C24 131.1(4) 2_656 . . . ? O1 Zn1 O2 Zn1 97.90(13) . . . 2_656 ? O2 Zn1 O2 Zn1 0.0 2_656 . . 2_656 ? N1 Zn1 O2 Zn1 -131.0(4) . . . 2_656 ? N2 Zn1 O2 Zn1 -104.21(14) . . . 2_656 ? C1 C2 C3 C4 0.5(7) . . . . ? C25 C2 C3 C4 -178.4(4) . . . . ? C2 C3 C4 C5 2.0(7) . . . . ? C2 C3 C4 C29 -179.3(4) . . . . ? C3 C4 C5 C6 -1.1(7) . . . . ? C29 C4 C5 C6 -179.8(4) . . . . ? C4 C5 C6 C7 -178.7(4) . . . . ? C4 C5 C6 C1 -2.3(7) . . . . ? O1 C1 C6 C5 -174.5(4) . . . . ? C2 C1 C6 C5 4.7(6) . . . . ? O1 C1 C6 C7 1.6(7) . . . . ? C2 C1 C6 C7 -179.3(4) . . . . ? C8 N1 C7 C6 -176.9(4) . . . . ? Zn1 N1 C7 C6 -9.2(6) . . . . ? C5 C6 C7 N1 173.2(4) . . . . ? C1 C6 C7 N1 -3.0(7) . . . . ? C7 N1 C8 C9 -32.8(7) . . . . ? Zn1 N1 C8 C9 158.2(4) . . . . ? C7 N1 C8 C13 147.6(4) . . . . ? Zn1 N1 C8 C13 -21.4(5) . . . . ? N1 C8 C9 C10 179.2(5) . . . . ? C13 C8 C9 C10 -1.3(7) . . . . ? C8 C9 C10 C11 0.8(8) . . . . ? C9 C10 C11 C12 0.8(8) . . . . ? C10 C11 C12 C13 -1.9(8) . . . . ? C11 C12 C13 C8 1.3(7) . . . . ? C11 C12 C13 N2 179.0(4) . . . . ? C9 C8 C13 C12 0.2(7) . . . . ? N1 C8 C13 C12 179.8(4) . . . . ? C9 C8 C13 N2 -177.7(4) . . . . ? N1 C8 C13 N2 1.9(6) . . . . ? C14 N2 C13 C12 30.5(7) . . . . ? Zn1 N2 C13 C12 -160.1(4) . . . . ? C14 N2 C13 C8 -151.7(4) . . . . ? Zn1 N2 C13 C8 17.7(5) . . . . ? C13 N2 C14 C15 -176.9(4) . . . . ? Zn1 N2 C14 C15 15.4(6) . . . . ? N2 C14 C15 C24 2.1(7) . . . . ? N2 C14 C15 C16 179.4(4) . . . . ? C24 C15 C16 C17 178.9(4) . . . . ? C14 C15 C16 C17 1.4(6) . . . . ? C24 C15 C16 C21 -1.4(6) . . . . ? C14 C15 C16 C21 -178.8(4) . . . . ? C21 C16 C17 C18 1.4(6) . . . . ? C15 C16 C17 C18 -178.9(4) . . . . ? C16 C17 C18 C19 -0.8(7) . . . . ? C17 C18 C19 C20 -0.2(7) . . . . ? C18 C19 C20 C21 0.6(7) . . . . ? C19 C20 C21 C22 178.8(4) . . . . ? C19 C20 C21 C16 0.0(7) . . . . ? C17 C16 C21 C22 -179.8(4) . . . . ? C15 C16 C21 C22 0.5(6) . . . . ? C17 C16 C21 C20 -1.0(6) . . . . ? C15 C16 C21 C20 179.3(4) . . . . ? C20 C21 C22 C23 -178.4(4) . . . . ? C16 C21 C22 C23 0.3(6) . . . . ? C21 C22 C23 C24 -0.2(7) . . . . ? Zn1 O2 C24 C15 -20.8(6) . . . . ? Zn1 O2 C24 C15 103.7(4) 2_656 . . . ? Zn1 O2 C24 C23 160.3(3) . . . . ? Zn1 O2 C24 C23 -75.3(4) 2_656 . . . ? C14 C15 C24 O2 -0.1(6) . . . . ? C16 C15 C24 O2 -177.4(4) . . . . ? C14 C15 C24 C23 178.8(4) . . . . ? C16 C15 C24 C23 1.5(6) . . . . ? C22 C23 C24 O2 178.3(4) . . . . ? C22 C23 C24 C15 -0.7(6) . . . . ? C3 C2 C25 C28 1.6(6) . . . . ? C1 C2 C25 C28 -177.3(4) . . . . ? C3 C2 C25 C27 120.0(4) . . . . ? C1 C2 C25 C27 -59.0(5) . . . . ? C3 C2 C25 C26 -118.4(5) . . . . ? C1 C2 C25 C26 62.7(5) . . . . ? C5 C4 C29 C32 -13.1(7) . . . . ? C3 C4 C29 C32 168.3(5) . . . . ? C5 C4 C29 C31 -133.2(5) . . . . ? C3 C4 C29 C31 48.2(6) . . . . ? C5 C4 C29 C30 106.6(5) . . . . ? C3 C4 C29 C30 -72.1(6) . . . . ? _diffrn_measured_fraction_theta_max 0.867 _diffrn_reflns_theta_full 28.65 _diffrn_measured_fraction_theta_full 0.867 _refine_diff_density_max 1.101 _refine_diff_density_min -0.945 _refine_diff_density_rms 0.110 # Attachment 'AWK80b_0mX1.cif' data_awk80b_0m _database_code_depnum_ccdc_archive 'CCDC 756455' #TrackingRef 'AWK80b_0mX1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C63 H65 N9 O12 Zn2' _chemical_formula_weight 1270.98 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 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 9.9018(5) _cell_length_b 22.1253(11) _cell_length_c 27.9995(14) _cell_angle_alpha 90.00 _cell_angle_beta 98.874(3) _cell_angle_gamma 90.00 _cell_volume 6060.7(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7541 _cell_measurement_theta_min 3.46 _cell_measurement_theta_max 39.60 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.393 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2648 _exptl_absorpt_coefficient_mu 0.861 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8512 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ; SADABS Version 2008/1 Bruker-Nonius Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_special_details ; It should be noted that the esd's of the cell dimensions are probably too low; they should be multiplied by a factor of 2 to 10 ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_specimen_suppport 'magnetic support whith 10 micron nylon fiber cryoloop' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'rotating anode X-ray tube' _diffrn_source_type 'Bruker-Nonius FR 591' _diffrn_source_power 50 _diffrn_source_current 70 _diffrn_source_size '3 mm x 0.3 mm fine focus' _diffrn_radiation_monochromator 'Multilayer Montel 200 mirrors' _diffrn_detector_type '4K CCD area detector APEX II' _diffrn_measurement_device_type 'Kappa 4-axis goniometer bruker-nonius' _diffrn_measurement_method ; Fullsphere data collection, phi and omega scans ; _diffrn_detector_area_resol_mean 512 _diffrn_reflns_number 70784 _diffrn_reflns_av_R_equivalents 0.0383 _diffrn_reflns_av_sigmaI/netI 0.0308 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 48 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 40.04 _reflns_number_total 17502 _reflns_number_gt 14918 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v2009.1-0' _computing_cell_refinement 'Bruker APEX2 v2009.1-0' _computing_data_reduction 'Bruker SAINT V7.60A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXS-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0785P)^2^+7.3853P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17502 _refine_ls_number_parameters 406 _refine_ls_number_restraints 72 _refine_ls_R_factor_all 0.0565 _refine_ls_R_factor_gt 0.0476 _refine_ls_wR_factor_ref 0.1435 _refine_ls_wR_factor_gt 0.1355 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.119 _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 C1 C 0.68492(12) 0.29355(6) 0.32504(5) 0.01889(19) Uani 1 1 d . . . C2 C 0.74457(14) 0.25997(8) 0.36625(5) 0.0254(2) Uani 1 1 d . . . C3 C 0.81463(18) 0.29236(10) 0.40513(6) 0.0332(3) Uani 1 1 d . . . H2 H 0.8522 0.2703 0.4331 0.040 Uiso 1 1 calc R . . C4 C 0.83345(17) 0.35458(10) 0.40583(6) 0.0335(3) Uani 1 1 d . . . C5 C 0.78628(15) 0.38571(8) 0.36341(6) 0.0279(3) Uani 1 1 d . . . H5 H 0.8020 0.4280 0.3619 0.034 Uiso 1 1 calc R . . C6 C 0.71570(12) 0.35591(6) 0.32270(5) 0.0199(2) Uani 1 1 d . . . C7 C 0.73790(18) 0.19074(9) 0.36774(6) 0.0321(3) Uani 1 1 d . . . C8 C 0.7959(3) 0.16417(10) 0.32427(8) 0.0455(5) Uani 1 1 d . . . H8A H 0.7844 0.1202 0.3238 0.068 Uiso 1 1 calc R . . H8B H 0.8932 0.1741 0.3271 0.068 Uiso 1 1 calc R . . H8C H 0.7468 0.1814 0.2943 0.068 Uiso 1 1 calc R . . C9 C 0.5918(2) 0.16879(9) 0.36668(8) 0.0386(4) Uani 1 1 d . . . H9A H 0.5911 0.1246 0.3693 0.058 Uiso 1 1 calc R . . H9B H 0.5361 0.1811 0.3362 0.058 Uiso 1 1 calc R . . H9C H 0.5539 0.1865 0.3939 0.058 Uiso 1 1 calc R . . C10 C 0.8242(2) 0.16394(13) 0.41322(8) 0.0466(5) Uani 1 1 d . . . H10A H 0.7848 0.1758 0.4418 0.070 Uiso 1 1 calc R . . H10B H 0.9180 0.1792 0.4161 0.070 Uiso 1 1 calc R . . H10C H 0.8247 0.1198 0.4107 0.070 Uiso 1 1 calc R . . C11 C 0.9024(2) 0.38868(13) 0.45074(8) 0.0463(5) Uani 1 1 d . . . C12 C 1.0187(3) 0.42646(17) 0.43841(12) 0.0680(8) Uani 1 1 d U . . H12A H 0.9823 0.4594 0.4167 0.102 Uiso 1 1 calc R . . H12B H 1.0794 0.4012 0.4224 0.102 Uiso 1 1 calc R . . H12C H 1.0701 0.4434 0.4681 0.102 Uiso 1 1 calc R . . C13 C 0.7947(3) 0.42550(14) 0.47074(11) 0.0569(6) Uani 1 1 d U . . H13A H 0.8355 0.4447 0.5011 0.085 Uiso 1 1 calc R . . H13B H 0.7199 0.3989 0.4767 0.085 Uiso 1 1 calc R . . H13C H 0.7589 0.4567 0.4473 0.085 Uiso 1 1 calc R . . C14 C 0.9647(3) 0.34442(14) 0.49128(10) 0.0560(6) Uani 1 1 d U . . H14A H 1.0335 0.3190 0.4795 0.084 Uiso 1 1 calc R . . H14B H 0.8922 0.3188 0.5005 0.084 Uiso 1 1 calc R . . H14C H 1.0076 0.3675 0.5194 0.084 Uiso 1 1 calc R . . C15 C 0.68748(12) 0.39249(6) 0.27943(5) 0.01810(18) Uani 1 1 d . . . H15 H 0.7042 0.4347 0.2827 0.022 Uiso 1 1 calc R . . C16 C 0.61695(11) 0.41143(5) 0.19642(4) 0.01508(16) Uani 1 1 d . . . C17 C 0.59392(13) 0.47355(5) 0.19871(5) 0.0197(2) Uani 1 1 d . . . H17 H 0.5989 0.4931 0.2291 0.024 Uiso 1 1 calc R . . C18 C 0.56366(15) 0.50662(5) 0.15622(6) 0.0236(2) Uani 1 1 d . . . H18 H 0.5477 0.5489 0.1579 0.028 Uiso 1 1 calc R . . C19 C 0.55642(16) 0.47882(6) 0.11125(6) 0.0236(2) Uani 1 1 d . . . H19 H 0.5351 0.5020 0.0825 0.028 Uiso 1 1 calc R . . C20 C 0.58042(14) 0.41705(5) 0.10854(5) 0.0201(2) Uani 1 1 d . . . H20 H 0.5759 0.3978 0.0780 0.024 Uiso 1 1 calc R . . C21 C 0.61122(12) 0.38359(5) 0.15101(4) 0.01538(16) Uani 1 1 d . . . C22 C 0.69675(13) 0.29604(5) 0.11970(4) 0.01758(18) Uani 1 1 d . . . H22 H 0.7179 0.3210 0.0942 0.021 Uiso 1 1 calc R . . C23 C 0.73346(12) 0.23264(5) 0.11900(4) 0.01573(17) Uani 1 1 d . . . C24 C 0.73505(12) 0.19302(5) 0.16000(4) 0.01605(17) Uani 1 1 d . . . C25 C 0.77423(15) 0.13193(5) 0.15157(5) 0.0204(2) Uani 1 1 d . . . C26 C 0.80173(14) 0.11045(5) 0.10803(5) 0.0201(2) Uani 1 1 d . . . H26 H 0.8194 0.0688 0.1037 0.024 Uiso 1 1 calc R . . C27 C 0.80293(13) 0.15139(5) 0.07057(4) 0.01784(18) Uani 1 1 d . . . C28 C 0.77065(14) 0.21165(5) 0.07600(5) 0.01853(19) Uani 1 1 d . . . H28 H 0.7739 0.2390 0.0501 0.022 Uiso 1 1 calc R . . N1 N 0.64141(10) 0.37236(4) 0.23668(4) 0.01502(15) Uani 1 1 d . . . N2 N 0.63756(11) 0.32072(4) 0.15242(4) 0.01527(15) Uani 1 1 d . . . N3 N 0.78390(19) 0.08806(6) 0.19107(6) 0.0346(3) Uani 1 1 d . . . N4 N 0.84155(14) 0.13079(5) 0.02566(4) 0.0232(2) Uani 1 1 d . . . O1 O 0.60088(9) 0.26655(4) 0.28893(3) 0.01598(13) Uani 1 1 d . . . O2 O 0.70303(11) 0.20864(4) 0.20056(4) 0.01952(16) Uani 1 1 d . . . O3 O 0.8444(2) 0.10269(8) 0.23035(6) 0.0562(5) Uani 1 1 d U . . O4 O 0.7367(2) 0.03782(6) 0.18160(7) 0.0519(5) Uani 1 1 d . . . O5 O 0.86823(16) 0.07711(5) 0.02136(5) 0.0331(3) Uani 1 1 d . . . O6 O 0.84676(17) 0.16845(6) -0.00644(4) 0.0352(3) Uani 1 1 d . . . Zn1 Zn 0.603812(14) 0.281686(6) 0.217438(5) 0.01394(4) Uani 1 1 d . . . N1P N 0.9603(3) 0.39423(15) 0.20639(11) 0.0480(9) Uani 0.50 1 d PGU A -1 C2P C 0.9691(4) 0.45550(14) 0.21742(11) 0.0493(10) Uani 0.50 1 d PGU A -1 C3P C 1.0139(5) 0.47412(15) 0.26462(12) 0.0658(10) Uani 0.50 1 d PGU A -1 H3PA H 1.0199 0.5160 0.2722 0.079 Uiso 0.50 1 calc PR A -1 C4P C 1.0499(5) 0.4315(2) 0.30080(11) 0.0658(10) Uani 0.50 1 d PGU A -1 H4PA H 1.0805 0.4442 0.3331 0.079 Uiso 0.50 1 calc PR A -1 C5P C 1.0411(5) 0.37020(18) 0.28977(13) 0.0658(10) Uani 0.50 1 d PGU A -1 H5PA H 1.0657 0.3410 0.3145 0.079 Uiso 0.50 1 calc PR A -1 C6P C 0.9963(6) 0.35158(14) 0.24257(14) 0.0571(12) Uani 0.50 1 d PGU A -1 C7P C 0.9281(8) 0.4942(4) 0.1788(3) 0.0687(16) Uani 0.50 1 d PU A -1 H7PA H 0.9005 0.4704 0.1494 0.103 Uiso 0.50 1 calc PR A -1 H7PB H 1.0042 0.5208 0.1742 0.103 Uiso 0.50 1 calc PR A -1 H7PC H 0.8508 0.5187 0.1855 0.103 Uiso 0.50 1 calc PR A -1 C8P C 0.9933(10) 0.2862(3) 0.2304(3) 0.077(2) Uani 0.50 1 d PU A -1 H8PA H 1.0212 0.2626 0.2599 0.115 Uiso 0.50 1 calc PR A -1 H8PB H 1.0562 0.2782 0.2074 0.115 Uiso 0.50 1 calc PR A -1 H8PC H 0.9003 0.2746 0.2160 0.115 Uiso 0.50 1 calc PR A -1 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 C1 0.0164(4) 0.0273(5) 0.0126(5) 0.0003(4) 0.0012(3) 0.0029(4) C2 0.0218(5) 0.0385(7) 0.0151(5) 0.0045(5) 0.0004(4) 0.0054(5) C3 0.0282(6) 0.0540(10) 0.0150(6) 0.0022(6) -0.0040(5) 0.0048(6) C4 0.0260(6) 0.0543(10) 0.0176(7) -0.0083(6) -0.0043(5) -0.0010(6) C5 0.0235(5) 0.0400(8) 0.0189(6) -0.0090(5) -0.0013(4) -0.0048(5) C6 0.0172(4) 0.0279(5) 0.0141(5) -0.0044(4) 0.0005(3) -0.0019(4) C7 0.0331(7) 0.0393(8) 0.0231(7) 0.0127(6) 0.0019(5) 0.0139(6) C8 0.0599(12) 0.0433(10) 0.0358(10) 0.0127(8) 0.0151(9) 0.0310(9) C9 0.0381(8) 0.0381(8) 0.0388(10) 0.0181(7) 0.0030(7) 0.0079(7) C10 0.0391(9) 0.0632(13) 0.0355(10) 0.0239(9) -0.0001(7) 0.0189(9) C11 0.0408(9) 0.0691(15) 0.0238(9) -0.0160(9) -0.0117(7) 0.0010(9) C12 0.0634(13) 0.0728(15) 0.0596(14) -0.0145(12) -0.0162(11) -0.0182(12) C13 0.0595(10) 0.0580(9) 0.0496(9) -0.0159(8) -0.0033(8) 0.0072(8) C14 0.0544(11) 0.0696(14) 0.0367(11) -0.0094(10) -0.0156(9) 0.0111(10) C15 0.0167(4) 0.0209(4) 0.0167(5) -0.0049(3) 0.0028(3) -0.0033(3) C16 0.0173(4) 0.0127(3) 0.0159(5) -0.0017(3) 0.0045(3) -0.0009(3) C17 0.0245(5) 0.0133(4) 0.0225(6) -0.0033(3) 0.0080(4) -0.0013(3) C18 0.0312(6) 0.0124(4) 0.0287(7) 0.0002(4) 0.0096(5) 0.0013(4) C19 0.0329(6) 0.0147(4) 0.0240(6) 0.0043(4) 0.0070(5) 0.0047(4) C20 0.0299(5) 0.0149(4) 0.0163(5) 0.0022(3) 0.0058(4) 0.0041(4) C21 0.0209(4) 0.0117(3) 0.0141(4) -0.0001(3) 0.0048(3) 0.0016(3) C22 0.0281(5) 0.0133(4) 0.0125(5) 0.0012(3) 0.0067(4) 0.0038(3) C23 0.0237(4) 0.0129(3) 0.0112(4) 0.0004(3) 0.0048(3) 0.0031(3) C24 0.0220(4) 0.0136(4) 0.0132(4) 0.0014(3) 0.0050(3) 0.0037(3) C25 0.0312(5) 0.0142(4) 0.0172(5) 0.0030(3) 0.0078(4) 0.0064(4) C26 0.0289(5) 0.0143(4) 0.0179(5) -0.0002(3) 0.0061(4) 0.0052(4) C27 0.0250(5) 0.0162(4) 0.0123(5) -0.0012(3) 0.0030(4) 0.0056(3) C28 0.0283(5) 0.0155(4) 0.0124(5) 0.0003(3) 0.0049(4) 0.0056(3) N1 0.0161(3) 0.0160(3) 0.0134(4) -0.0017(3) 0.0036(3) -0.0012(3) N2 0.0219(4) 0.0115(3) 0.0129(4) 0.0003(3) 0.0043(3) 0.0023(3) N3 0.0624(10) 0.0209(5) 0.0256(6) 0.0097(4) 0.0226(6) 0.0186(6) N4 0.0357(6) 0.0210(4) 0.0130(4) -0.0022(3) 0.0033(4) 0.0108(4) O1 0.0180(3) 0.0192(3) 0.0107(3) 0.0006(3) 0.0020(3) 0.0025(3) O2 0.0304(4) 0.0162(3) 0.0136(4) 0.0024(3) 0.0086(3) 0.0066(3) O3 0.1065(13) 0.0372(7) 0.0234(6) 0.0100(5) 0.0052(7) 0.0277(8) O4 0.0843(13) 0.0220(5) 0.0570(10) 0.0145(6) 0.0351(9) 0.0037(6) O5 0.0565(8) 0.0214(4) 0.0223(5) -0.0044(4) 0.0088(5) 0.0156(5) O6 0.0647(9) 0.0285(5) 0.0146(5) 0.0039(4) 0.0133(5) 0.0188(5) Zn1 0.01820(6) 0.01308(6) 0.01109(7) 0.00019(4) 0.00395(4) 0.00078(4) N1P 0.0287(12) 0.0566(17) 0.0608(18) 0.0057(15) 0.0140(12) -0.0014(12) C2P 0.0317(13) 0.0601(19) 0.059(2) -0.0046(16) 0.0174(14) -0.0030(13) C3P 0.0561(12) 0.0754(14) 0.0682(14) -0.0030(11) 0.0172(11) 0.0014(11) C4P 0.0561(12) 0.0754(14) 0.0682(14) -0.0030(11) 0.0172(11) 0.0014(11) C5P 0.0561(12) 0.0754(14) 0.0682(14) -0.0030(11) 0.0172(11) 0.0014(11) C6P 0.0383(14) 0.075(2) 0.058(2) 0.0116(17) 0.0067(17) 0.0003(18) C7P 0.063(2) 0.072(2) 0.072(2) 0.0040(18) 0.0118(18) -0.0012(18) C8P 0.068(3) 0.081(3) 0.081(3) 0.0013(19) 0.012(2) -0.0073(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.3461(16) . ? C1 C6 1.417(2) . ? C1 C2 1.4218(19) . ? C2 C3 1.395(2) . ? C2 C7 1.534(3) . ? C3 C4 1.389(3) . ? C4 C5 1.390(3) . ? C4 C11 1.534(2) . ? C5 C6 1.4062(19) . ? C6 C15 1.4479(19) . ? C7 C9 1.522(3) . ? C7 C10 1.538(2) . ? C7 C8 1.540(3) . ? C11 C12 1.505(4) . ? C11 C13 1.517(4) . ? C11 C14 1.553(4) . ? C15 N1 1.2925(16) . ? C16 C17 1.3964(16) . ? C16 C21 1.4059(16) . ? C16 N1 1.4114(16) . ? C17 C18 1.390(2) . ? C18 C19 1.393(2) . ? C19 C20 1.3913(17) . ? C20 C21 1.3940(17) . ? C21 N2 1.4148(14) . ? C22 N2 1.2832(15) . ? C22 C23 1.4500(15) . ? C23 C28 1.3918(17) . ? C23 C24 1.4425(16) . ? C24 O2 1.2730(15) . ? C24 C25 1.4359(16) . ? C25 C26 1.3743(18) . ? C25 N3 1.4634(18) . ? C26 C27 1.3872(18) . ? C27 C28 1.3849(16) . ? C27 N4 1.4435(17) . ? N1 Zn1 2.0957(10) . ? N2 Zn1 2.0880(10) . ? N3 O3 1.212(3) . ? N3 O4 1.219(2) . ? N4 O5 1.2266(15) . ? N4 O6 1.2326(17) . ? O1 Zn1 2.0342(9) . ? O1 Zn1 2.0348(9) 2_655 ? O2 Zn1 1.9860(9) . ? Zn1 O1 2.0348(9) 2_655 ? Zn1 Zn1 2.9510(3) 2_655 ? N1P C2P 1.3900 . ? N1P C6P 1.3900 . ? C2P C3P 1.3900 . ? C2P C7P 1.391(8) . ? C3P C4P 1.3900 . ? C4P C5P 1.3900 . ? C5P C6P 1.3900 . ? C6P C8P 1.485(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 C6 120.65(11) . . ? O1 C1 C2 120.60(13) . . ? C6 C1 C2 118.75(13) . . ? C3 C2 C1 117.33(16) . . ? C3 C2 C7 120.66(14) . . ? C1 C2 C7 121.98(14) . . ? C4 C3 C2 124.72(16) . . ? C3 C4 C5 116.90(15) . . ? C3 C4 C11 122.76(18) . . ? C5 C4 C11 120.3(2) . . ? C4 C5 C6 121.32(16) . . ? C5 C6 C1 120.18(14) . . ? C5 C6 C15 115.08(13) . . ? C1 C6 C15 124.62(11) . . ? C9 C7 C2 111.27(13) . . ? C9 C7 C10 107.34(16) . . ? C2 C7 C10 112.75(18) . . ? C9 C7 C8 109.4(2) . . ? C2 C7 C8 109.67(15) . . ? C10 C7 C8 106.26(16) . . ? C12 C11 C13 113.1(3) . . ? C12 C11 C4 110.2(2) . . ? C13 C11 C4 108.50(18) . . ? C12 C11 C14 106.6(2) . . ? C13 C11 C14 106.9(2) . . ? C4 C11 C14 111.4(2) . . ? N1 C15 C6 125.26(11) . . ? C17 C16 C21 119.25(11) . . ? C17 C16 N1 125.11(11) . . ? C21 C16 N1 115.60(9) . . ? C18 C17 C16 119.61(12) . . ? C17 C18 C19 121.04(11) . . ? C20 C19 C18 119.83(13) . . ? C19 C20 C21 119.47(12) . . ? C20 C21 C16 120.78(10) . . ? C20 C21 N2 124.12(10) . . ? C16 C21 N2 115.09(10) . . ? N2 C22 C23 124.36(11) . . ? C28 C23 C24 120.91(10) . . ? C28 C23 C22 115.78(10) . . ? C24 C23 C22 123.30(10) . . ? O2 C24 C25 120.85(10) . . ? O2 C24 C23 124.85(10) . . ? C25 C24 C23 114.29(10) . . ? C26 C25 C24 124.53(11) . . ? C26 C25 N3 116.24(11) . . ? C24 C25 N3 119.22(11) . . ? C25 C26 C27 118.10(11) . . ? C28 C27 C26 121.10(11) . . ? C28 C27 N4 119.75(11) . . ? C26 C27 N4 119.13(10) . . ? C27 C28 C23 120.83(11) . . ? C15 N1 C16 121.41(10) . . ? C15 N1 Zn1 126.24(9) . . ? C16 N1 Zn1 112.28(7) . . ? C22 N2 C21 120.08(10) . . ? C22 N2 Zn1 126.77(8) . . ? C21 N2 Zn1 112.17(7) . . ? O3 N3 O4 124.06(16) . . ? O3 N3 C25 118.29(16) . . ? O4 N3 C25 117.53(17) . . ? O5 N4 O6 123.30(12) . . ? O5 N4 C27 118.77(12) . . ? O6 N4 C27 117.92(11) . . ? C1 O1 Zn1 124.41(8) . . ? C1 O1 Zn1 119.00(7) . 2_655 ? Zn1 O1 Zn1 92.98(4) . 2_655 ? C24 O2 Zn1 129.32(8) . . ? O2 Zn1 O1 100.54(4) . . ? O2 Zn1 O1 111.58(4) . 2_655 ? O1 Zn1 O1 83.91(4) . 2_655 ? O2 Zn1 N2 88.71(4) . . ? O1 Zn1 N2 162.67(4) . . ? O1 Zn1 N2 106.43(4) 2_655 . ? O2 Zn1 N1 139.95(4) . . ? O1 Zn1 N1 86.19(4) . . ? O1 Zn1 N1 108.37(4) 2_655 . ? N2 Zn1 N1 77.42(4) . . ? O2 Zn1 Zn1 124.36(3) . 2_655 ? O1 Zn1 Zn1 43.52(2) . 2_655 ? O1 Zn1 Zn1 43.51(3) 2_655 2_655 ? N2 Zn1 Zn1 139.40(3) . 2_655 ? N1 Zn1 Zn1 87.38(3) . 2_655 ? C2P N1P C6P 120.0 . . ? C3P C2P N1P 120.0 . . ? C3P C2P C7P 124.7(4) . . ? N1P C2P C7P 115.3(4) . . ? C2P C3P C4P 120.0 . . ? C5P C4P C3P 120.0 . . ? C4P C5P C6P 120.0 . . ? C5P C6P N1P 120.0 . . ? C5P C6P C8P 119.9(4) . . ? N1P C6P C8P 120.0(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 O1 C1 C2 C3 -171.15(13) . . . . ? C6 C1 C2 C3 8.9(2) . . . . ? O1 C1 C2 C7 11.2(2) . . . . ? C6 C1 C2 C7 -168.78(13) . . . . ? C1 C2 C3 C4 -2.0(3) . . . . ? C7 C2 C3 C4 175.75(16) . . . . ? C2 C3 C4 C5 -4.4(3) . . . . ? C2 C3 C4 C11 175.53(18) . . . . ? C3 C4 C5 C6 3.6(2) . . . . ? C11 C4 C5 C6 -176.26(16) . . . . ? C4 C5 C6 C1 3.3(2) . . . . ? C4 C5 C6 C15 -172.81(14) . . . . ? O1 C1 C6 C5 170.35(12) . . . . ? C2 C1 C6 C5 -9.71(19) . . . . ? O1 C1 C6 C15 -13.92(18) . . . . ? C2 C1 C6 C15 166.02(12) . . . . ? C3 C2 C7 C9 115.95(18) . . . . ? C1 C2 C7 C9 -66.44(19) . . . . ? C3 C2 C7 C10 -4.7(2) . . . . ? C1 C2 C7 C10 172.90(15) . . . . ? C3 C2 C7 C8 -122.90(18) . . . . ? C1 C2 C7 C8 54.7(2) . . . . ? C3 C4 C11 C12 126.2(3) . . . . ? C5 C4 C11 C12 -53.9(3) . . . . ? C3 C4 C11 C13 -109.4(3) . . . . ? C5 C4 C11 C13 70.4(3) . . . . ? C3 C4 C11 C14 8.0(3) . . . . ? C5 C4 C11 C14 -172.1(2) . . . . ? C5 C6 C15 N1 169.85(12) . . . . ? C1 C6 C15 N1 -6.08(19) . . . . ? C21 C16 C17 C18 1.01(18) . . . . ? N1 C16 C17 C18 -176.51(12) . . . . ? C16 C17 C18 C19 -0.3(2) . . . . ? C17 C18 C19 C20 -0.3(2) . . . . ? C18 C19 C20 C21 0.1(2) . . . . ? C19 C20 C21 C16 0.63(19) . . . . ? C19 C20 C21 N2 -179.89(12) . . . . ? C17 C16 C21 C20 -1.21(17) . . . . ? N1 C16 C21 C20 176.55(11) . . . . ? C17 C16 C21 N2 179.27(10) . . . . ? N1 C16 C21 N2 -2.98(14) . . . . ? N2 C22 C23 C28 167.23(13) . . . . ? N2 C22 C23 C24 -14.0(2) . . . . ? C28 C23 C24 O2 179.77(13) . . . . ? C22 C23 C24 O2 1.1(2) . . . . ? C28 C23 C24 C25 -1.38(18) . . . . ? C22 C23 C24 C25 179.92(12) . . . . ? O2 C24 C25 C26 175.64(14) . . . . ? C23 C24 C25 C26 -3.3(2) . . . . ? O2 C24 C25 N3 -3.1(2) . . . . ? C23 C24 C25 N3 178.00(14) . . . . ? C24 C25 C26 C27 5.6(2) . . . . ? N3 C25 C26 C27 -175.66(14) . . . . ? C25 C26 C27 C28 -3.2(2) . . . . ? C25 C26 C27 N4 175.40(13) . . . . ? C26 C27 C28 C23 -1.2(2) . . . . ? N4 C27 C28 C23 -179.83(13) . . . . ? C24 C23 C28 C27 3.6(2) . . . . ? C22 C23 C28 C27 -177.64(12) . . . . ? C6 C15 N1 C16 -179.92(11) . . . . ? C6 C15 N1 Zn1 -3.13(17) . . . . ? C17 C16 N1 C15 -22.58(17) . . . . ? C21 C16 N1 C15 159.81(11) . . . . ? C17 C16 N1 Zn1 160.21(10) . . . . ? C21 C16 N1 Zn1 -17.40(12) . . . . ? C23 C22 N2 C21 177.28(12) . . . . ? C23 C22 N2 Zn1 9.56(19) . . . . ? C20 C21 N2 C22 33.08(18) . . . . ? C16 C21 N2 C22 -147.42(12) . . . . ? C20 C21 N2 Zn1 -157.52(10) . . . . ? C16 C21 N2 Zn1 21.98(12) . . . . ? C26 C25 N3 O3 134.10(18) . . . . ? C24 C25 N3 O3 -47.1(2) . . . . ? C26 C25 N3 O4 -42.0(2) . . . . ? C24 C25 N3 O4 136.80(17) . . . . ? C28 C27 N4 O5 -179.17(14) . . . . ? C26 C27 N4 O5 2.2(2) . . . . ? C28 C27 N4 O6 1.3(2) . . . . ? C26 C27 N4 O6 -177.35(15) . . . . ? C6 C1 O1 Zn1 41.71(15) . . . . ? C2 C1 O1 Zn1 -138.23(10) . . . . ? C6 C1 O1 Zn1 -75.14(13) . . . 2_655 ? C2 C1 O1 Zn1 104.92(12) . . . 2_655 ? C25 C24 O2 Zn1 -163.39(10) . . . . ? C23 C24 O2 Zn1 15.39(19) . . . . ? C24 O2 Zn1 O1 179.62(11) . . . . ? C24 O2 Zn1 O1 92.05(12) . . . 2_655 ? C24 O2 Zn1 N2 -15.13(12) . . . . ? C24 O2 Zn1 N1 -83.70(13) . . . . ? C24 O2 Zn1 Zn1 139.65(10) . . . 2_655 ? C1 O1 Zn1 O2 101.76(9) . . . . ? Zn1 O1 Zn1 O2 -129.63(4) 2_655 . . . ? C1 O1 Zn1 O1 -147.36(8) . . . 2_655 ? Zn1 O1 Zn1 O1 -18.75(5) 2_655 . . 2_655 ? C1 O1 Zn1 N2 -19.54(18) . . . . ? Zn1 O1 Zn1 N2 109.07(12) 2_655 . . . ? C1 O1 Zn1 N1 -38.41(9) . . . . ? Zn1 O1 Zn1 N1 90.20(4) 2_655 . . . ? C1 O1 Zn1 Zn1 -128.61(10) . . . 2_655 ? C22 N2 Zn1 O2 2.64(11) . . . . ? C21 N2 Zn1 O2 -165.89(8) . . . . ? C22 N2 Zn1 O1 125.47(13) . . . . ? C21 N2 Zn1 O1 -43.06(17) . . . . ? C22 N2 Zn1 O1 -109.50(11) . . . 2_655 ? C21 N2 Zn1 O1 81.96(8) . . . 2_655 ? C22 N2 Zn1 N1 144.79(12) . . . . ? C21 N2 Zn1 N1 -23.75(8) . . . . ? C22 N2 Zn1 Zn1 -144.63(9) . . . 2_655 ? C21 N2 Zn1 Zn1 46.84(10) . . . 2_655 ? C15 N1 Zn1 O2 -82.39(11) . . . . ? C16 N1 Zn1 O2 94.65(9) . . . . ? C15 N1 Zn1 O1 19.48(10) . . . . ? C16 N1 Zn1 O1 -163.48(7) . . . . ? C15 N1 Zn1 O1 101.77(10) . . . 2_655 ? C16 N1 Zn1 O1 -81.19(8) . . . 2_655 ? C15 N1 Zn1 N2 -154.86(10) . . . . ? C16 N1 Zn1 N2 22.19(7) . . . . ? C15 N1 Zn1 Zn1 63.05(9) . . . 2_655 ? C16 N1 Zn1 Zn1 -119.90(7) . . . 2_655 ? C6P N1P C2P C3P 0.0 . . . . ? C6P N1P C2P C7P -178.8(4) . . . . ? N1P C2P C3P C4P 0.0 . . . . ? C7P C2P C3P C4P 178.7(5) . . . . ? C2P C3P C4P C5P 0.0 . . . . ? C3P C4P C5P C6P 0.0 . . . . ? C4P C5P C6P N1P 0.0 . . . . ? C4P C5P C6P C8P 177.1(6) . . . . ? C2P N1P C6P C5P 0.0 . . . . ? C2P N1P C6P C8P -177.1(6) . . . . ? _diffrn_measured_fraction_theta_max 0.930 _diffrn_reflns_theta_full 40.04 _diffrn_measured_fraction_theta_full 0.930 _refine_diff_density_max 3.376 _refine_diff_density_min -1.081 _refine_diff_density_rms 0.105 # Attachment 'AWK292_0m1.cif' data_awk292_0m _database_code_depnum_ccdc_archive 'CCDC 756456' #TrackingRef 'AWK292_0m1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H77 N7 O4 Zn2' _chemical_formula_weight 1187.11 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' 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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.3096(6) _cell_length_b 13.0108(5) _cell_length_c 29.4617(11) _cell_angle_alpha 90.00 _cell_angle_beta 102.979(2) _cell_angle_gamma 90.00 _cell_volume 6092.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9885 _cell_measurement_theta_min 3.00 _cell_measurement_theta_max 33.21 _exptl_crystal_description neddle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.294 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2504 _exptl_absorpt_coefficient_mu 0.842 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7982 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ; SADABS Version 2008/1 Bruker-Nonius Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_special_details ; It should be noted that the esd's of the cell dimensions are probably too low; they should be multiplied by a factor of 2 to 10 ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_specimen_suppport 'magnetic support whith 10 micron nylon fiber cryoloop' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'rotating anode X-ray tube' _diffrn_source_type 'Bruker-Nonius FR 591' _diffrn_source_power 50 _diffrn_source_current 70 _diffrn_source_size '3 mm x 0.3 mm fine focus' _diffrn_radiation_monochromator 'Multilayer Montel 200 mirrors' _diffrn_detector_type '4K CCD area detector APEX II' _diffrn_measurement_device_type 'Kappa 4-axis goniometer bruker-nonius' _diffrn_measurement_method ; Fullsphere data collection, phi and omega scans ; _diffrn_detector_area_resol_mean 512 _diffrn_reflns_number 113286 _diffrn_reflns_av_R_equivalents 0.0591 _diffrn_reflns_av_sigmaI/netI 0.0507 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_theta_min 2.63 _diffrn_reflns_theta_max 33.90 _reflns_number_total 23903 _reflns_number_gt 19315 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v2009.1-0' _computing_cell_refinement 'Bruker APEX2 v2009.1-0' _computing_data_reduction 'Bruker SAINT V7.60A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXS-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0859P)^2^+18.1568P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 23903 _refine_ls_number_parameters 749 _refine_ls_number_restraints 140 _refine_ls_R_factor_all 0.1004 _refine_ls_R_factor_gt 0.0828 _refine_ls_wR_factor_ref 0.2173 _refine_ls_wR_factor_gt 0.2053 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.100 _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 C1A C -0.0238(6) 0.1455(6) -0.0289(3) 0.088(2) Uani 1 1 d U . . H1A1 H -0.0653 0.1322 -0.0565 0.106 Uiso 1 1 calc R . . H1A2 H -0.0263 0.1112 -0.0008 0.106 Uiso 1 1 calc R . . C2A C 0.0369(5) 0.2111(5) -0.0296(2) 0.0720(16) Uani 1 1 d U . . H2A H 0.0765 0.2213 -0.0010 0.086 Uiso 1 1 calc R . . C3A C 0.0505(4) 0.2702(4) -0.06918(17) 0.0536(11) Uani 1 1 d U . . H3AA H 0.0126 0.2439 -0.0979 0.064 Uiso 1 1 calc R . . H3AB H 0.1092 0.2597 -0.0722 0.064 Uiso 1 1 calc R . . C4A C 0.0962(2) 0.4416(3) -0.03460(11) 0.0323(6) Uani 1 1 d U . . C5A C 0.0354(3) 0.3815(4) -0.06512(13) 0.0416(8) Uani 1 1 d U . . C6A C -0.0397(3) 0.4330(4) -0.08962(13) 0.0453(9) Uani 1 1 d U . . H6A H -0.0821 0.3928 -0.1091 0.054 Uiso 1 1 calc R . . C7A C -0.0531(3) 0.5310(4) -0.08675(14) 0.0479(9) Uani 1 1 d U . . H7A H -0.1026 0.5612 -0.1051 0.057 Uiso 1 1 calc R . . C8A C 0.0045(3) 0.5909(4) -0.05702(13) 0.0431(8) Uani 1 1 d U . . H8A H -0.0057 0.6623 -0.0543 0.052 Uiso 1 1 calc R . . C9A C 0.0794(2) 0.5458(4) -0.03025(10) 0.0396(9) Uani 1 1 d . . . C10A C 0.1337(2) 0.6159(3) 0.00023(11) 0.0319(7) Uani 1 1 d . . . H10A H 0.1197 0.6868 -0.0022 0.038 Uiso 1 1 calc R . . C11A C 0.25152(19) 0.6641(2) 0.05820(10) 0.0235(5) Uani 1 1 d . . . C12A C 0.2583(3) 0.7661(3) 0.04470(14) 0.0384(8) Uani 1 1 d . . . H12A H 0.2250 0.7905 0.0161 0.046 Uiso 1 1 calc R . . C13A C 0.3145(3) 0.8320(3) 0.07365(18) 0.0472(10) Uani 1 1 d . . . H13A H 0.3199 0.9012 0.0644 0.057 Uiso 1 1 calc R . . C14A C 0.3622(3) 0.7974(3) 0.11544(18) 0.0435(9) Uani 1 1 d . . . H14A H 0.3995 0.8433 0.1350 0.052 Uiso 1 1 calc R . . C15A C 0.3564(2) 0.6962(2) 0.12922(13) 0.0293(6) Uani 1 1 d . . . H15A H 0.3900 0.6728 0.1580 0.035 Uiso 1 1 calc R . . C16A C 0.30077(18) 0.6288(2) 0.10064(10) 0.0200(4) Uani 1 1 d . . . C17A C 0.31241(16) 0.4876(2) 0.15193(8) 0.0182(4) Uani 1 1 d . . . H17A H 0.3367 0.5340 0.1761 0.022 Uiso 1 1 calc R . . C18A C 0.30245(19) 0.3822(2) 0.16478(9) 0.0218(5) Uani 1 1 d . . . C19A C 0.3392(2) 0.3561(3) 0.21160(10) 0.0308(7) Uani 1 1 d . . . H19A H 0.3676 0.4076 0.2321 0.037 Uiso 1 1 calc R . . C20A C 0.3347(3) 0.2575(3) 0.22821(12) 0.0421(10) Uani 1 1 d . A . C21A C 0.2915(3) 0.1847(3) 0.19701(15) 0.0460(11) Uani 1 1 d . . . H21A H 0.2882 0.1167 0.2082 0.055 Uiso 1 1 calc R . . C22A C 0.2537(3) 0.2039(3) 0.15153(14) 0.0415(9) Uani 1 1 d . . . C23A C 0.2578(2) 0.3064(2) 0.13375(10) 0.0268(6) Uani 1 1 d . . . C24A C 0.3729(3) 0.2267(3) 0.27843(13) 0.0425(8) Uani 1 1 d DU . . C25A C 0.4402(7) 0.1462(8) 0.2804(3) 0.0619(15) Uani 0.671(12) 1 d PU A 1 H25A H 0.4816 0.1707 0.2634 0.093 Uiso 0.671(12) 1 calc PR A 1 H25B H 0.4146 0.0825 0.2662 0.093 Uiso 0.671(12) 1 calc PR A 1 H25C H 0.4683 0.1333 0.3130 0.093 Uiso 0.671(12) 1 calc PR A 1 C26A C 0.3122(6) 0.2304(7) 0.3081(3) 0.0619(15) Uani 0.671(12) 1 d PU A 1 H26A H 0.3419 0.2240 0.3408 0.093 Uiso 0.671(12) 1 calc PR A 1 H26B H 0.2721 0.1736 0.2999 0.093 Uiso 0.671(12) 1 calc PR A 1 H26C H 0.2819 0.2959 0.3034 0.093 Uiso 0.671(12) 1 calc PR A 1 C27A C 0.4241(6) 0.3184(6) 0.3052(3) 0.0619(15) Uani 0.671(12) 1 d PDU A 1 H27A H 0.3894 0.3806 0.3006 0.093 Uiso 0.671(12) 1 calc PR A 1 H27B H 0.4749 0.3299 0.2933 0.093 Uiso 0.671(12) 1 calc PR A 1 H27C H 0.4403 0.3022 0.3385 0.093 Uiso 0.671(12) 1 calc PR A 1 C25' C 0.3086(8) 0.1589(11) 0.2961(5) 0.049(2) Uani 0.329(12) 1 d PDU A 2 H25G H 0.2857 0.1071 0.2725 0.073 Uiso 0.329(12) 1 calc PR A 2 H25H H 0.2628 0.2020 0.3019 0.073 Uiso 0.329(12) 1 calc PR A 2 H25I H 0.3366 0.1246 0.3250 0.073 Uiso 0.329(12) 1 calc PR A 2 C26' C 0.4575(11) 0.1840(13) 0.2898(6) 0.049(2) Uani 0.329(12) 1 d PU A 2 H26G H 0.4565 0.1140 0.2774 0.073 Uiso 0.329(12) 1 calc PR A 2 H26H H 0.4782 0.1824 0.3237 0.073 Uiso 0.329(12) 1 calc PR A 2 H26I H 0.4948 0.2268 0.2759 0.073 Uiso 0.329(12) 1 calc PR A 2 C27' C 0.3787(11) 0.3063(12) 0.3096(5) 0.049(2) Uani 0.329(12) 1 d PU A 2 H27G H 0.3292 0.3061 0.3233 0.073 Uiso 0.329(12) 1 calc PR A 2 H27H H 0.3814 0.3717 0.2935 0.073 Uiso 0.329(12) 1 calc PR A 2 H27I H 0.4297 0.2980 0.3343 0.073 Uiso 0.329(12) 1 calc PR A 2 C28A C 0.2050(4) 0.1195(3) 0.11861(17) 0.0500(10) Uani 1 1 d U . . C29A C 0.2102(5) 0.0141(5) 0.1426(2) 0.0690(15) Uani 1 1 d U . . H29A H 0.1734 0.0136 0.1647 0.104 Uiso 1 1 calc R . . H29B H 0.2684 0.0010 0.1592 0.104 Uiso 1 1 calc R . . H29C H 0.1922 -0.0394 0.1191 0.104 Uiso 1 1 calc R . . C30A C 0.1140(4) 0.1463(4) 0.1036(2) 0.0593(12) Uani 1 1 d U . . H30A H 0.0847 0.0926 0.0828 0.089 Uiso 1 1 calc R . . H30B H 0.1080 0.2122 0.0870 0.089 Uiso 1 1 calc R . . H30C H 0.0896 0.1517 0.1310 0.089 Uiso 1 1 calc R . . C31A C 0.2457(4) 0.1059(4) 0.07615(19) 0.0572(12) Uani 1 1 d U . . H31A H 0.2179 0.0494 0.0566 0.086 Uiso 1 1 calc R . . H31B H 0.3056 0.0903 0.0871 0.086 Uiso 1 1 calc R . . H31C H 0.2392 0.1695 0.0579 0.086 Uiso 1 1 calc R . . C1B C 0.5209(3) 0.2256(3) 0.16612(13) 0.0436(9) Uani 1 1 d . . . H1B1 H 0.4671 0.2183 0.1730 0.052 Uiso 1 1 calc R . . H1B2 H 0.5695 0.2001 0.1872 0.052 Uiso 1 1 calc R . . C2B C 0.5283(2) 0.2716(3) 0.12707(12) 0.0323(6) Uani 1 1 d . . . H2B H 0.5830 0.2778 0.1211 0.039 Uiso 1 1 calc R . . C3B C 0.4557(2) 0.3142(2) 0.09179(10) 0.0265(5) Uani 1 1 d . . . H3B1 H 0.4051 0.3120 0.1051 0.032 Uiso 1 1 calc R . . H3B2 H 0.4449 0.2685 0.0642 0.032 Uiso 1 1 calc R . . C4B C 0.40434(17) 0.4591(2) 0.03707(9) 0.0188(4) Uani 1 1 d . . . C5B C 0.46579(18) 0.4228(2) 0.07549(9) 0.0216(5) Uani 1 1 d . . . C6B C 0.53185(19) 0.4873(3) 0.09585(10) 0.0258(5) Uani 1 1 d . . . H6B H 0.5720 0.4640 0.1224 0.031 Uiso 1 1 calc R . . C7B C 0.5406(2) 0.5854(3) 0.07827(11) 0.0279(6) Uani 1 1 d . . . H7B H 0.5854 0.6288 0.0931 0.033 Uiso 1 1 calc R . . C8B C 0.4835(2) 0.6186(2) 0.03918(11) 0.0250(5) Uani 1 1 d . . . H8B H 0.4905 0.6843 0.0265 0.030 Uiso 1 1 calc R . . C9B C 0.41483(18) 0.5568(2) 0.01766(9) 0.0201(4) Uani 1 1 d . . . C10B C 0.35847(18) 0.5985(2) -0.02313(10) 0.0214(5) Uani 1 1 d . . . H10B H 0.3686 0.6669 -0.0318 0.026 Uiso 1 1 calc R . . C11B C 0.24003(18) 0.5992(2) -0.08656(10) 0.0226(5) Uani 1 1 d . . . C12B C 0.2285(2) 0.7056(3) -0.09047(13) 0.0318(6) Uani 1 1 d . . . H12B H 0.2605 0.7503 -0.0677 0.038 Uiso 1 1 calc R . . C13B C 0.1696(3) 0.7452(3) -0.12809(16) 0.0437(9) Uani 1 1 d . . . H13B H 0.1630 0.8175 -0.1315 0.052 Uiso 1 1 calc R . . C14B C 0.1207(3) 0.6810(3) -0.16053(15) 0.0416(9) Uani 1 1 d . . . H14B H 0.0804 0.7096 -0.1858 0.050 Uiso 1 1 calc R . . C15B C 0.1298(2) 0.5757(3) -0.15658(11) 0.0316(6) Uani 1 1 d . . . H15B H 0.0949 0.5318 -0.1785 0.038 Uiso 1 1 calc R . . C16B C 0.19086(19) 0.5337(2) -0.12010(10) 0.0233(5) Uani 1 1 d . . . C17B C 0.19337(18) 0.3633(2) -0.14748(9) 0.0228(5) Uani 1 1 d . . . H17B H 0.1646 0.3887 -0.1770 0.027 Uiso 1 1 calc R . . C18B C 0.21661(18) 0.2563(2) -0.14490(9) 0.0224(5) Uani 1 1 d . . . C19B C 0.19247(19) 0.2000(3) -0.18690(10) 0.0263(6) Uani 1 1 d . . . H19B H 0.1576 0.2324 -0.2132 0.032 Uiso 1 1 calc R . . C20B C 0.2175(2) 0.1001(3) -0.19121(10) 0.0274(6) Uani 1 1 d . . . C21B C 0.2697(2) 0.0556(2) -0.15131(10) 0.0261(5) Uani 1 1 d . . . H21B H 0.2878 -0.0132 -0.1536 0.031 Uiso 1 1 calc R . . C22B C 0.29634(19) 0.1057(2) -0.10896(10) 0.0232(5) Uani 1 1 d . . . C23B C 0.26831(18) 0.2093(2) -0.10443(9) 0.0217(5) Uani 1 1 d . . . C24B C 0.1913(2) 0.0423(3) -0.23787(12) 0.0343(7) Uani 1 1 d . . . C25B C 0.0953(3) 0.0303(4) -0.25146(15) 0.0477(11) Uani 1 1 d . . . H25D H 0.0792 -0.0044 -0.2817 0.071 Uiso 1 1 calc R . . H25E H 0.0689 0.0983 -0.2536 0.071 Uiso 1 1 calc R . . H25F H 0.0765 -0.0107 -0.2278 0.071 Uiso 1 1 calc R . . C26B C 0.2192(3) 0.1053(4) -0.27607(12) 0.0440(10) Uani 1 1 d . . . H26D H 0.2045 0.0680 -0.3057 0.066 Uiso 1 1 calc R . . H26E H 0.2802 0.1158 -0.2674 0.066 Uiso 1 1 calc R . . H26F H 0.1907 0.1721 -0.2794 0.066 Uiso 1 1 calc R . . C27B C 0.2332(3) -0.0638(4) -0.23598(16) 0.0515(11) Uani 1 1 d . . . H27D H 0.2157 -0.1061 -0.2123 0.077 Uiso 1 1 calc R . . H27E H 0.2945 -0.0556 -0.2280 0.077 Uiso 1 1 calc R . . H27F H 0.2161 -0.0972 -0.2664 0.077 Uiso 1 1 calc R . . C28B C 0.3564(2) 0.0524(2) -0.06791(11) 0.0280(6) Uani 1 1 d . . . C29B C 0.4385(3) 0.1136(3) -0.05434(17) 0.0480(10) Uani 1 1 d U . . H29D H 0.4774 0.0783 -0.0290 0.072 Uiso 1 1 calc R . . H29E H 0.4265 0.1825 -0.0440 0.072 Uiso 1 1 calc R . . H29F H 0.4640 0.1193 -0.0813 0.072 Uiso 1 1 calc R . . C30B C 0.3164(4) 0.0437(4) -0.02589(15) 0.0558(13) Uani 1 1 d . . . H30D H 0.2633 0.0057 -0.0348 0.084 Uiso 1 1 calc R . . H30E H 0.3054 0.1127 -0.0152 0.084 Uiso 1 1 calc R . . H30F H 0.3548 0.0072 -0.0007 0.084 Uiso 1 1 calc R . . C31B C 0.3798(3) -0.0558(3) -0.07999(15) 0.0447(10) Uani 1 1 d . . . H31D H 0.4182 -0.0863 -0.0530 0.067 Uiso 1 1 calc R . . H31E H 0.4074 -0.0530 -0.1063 0.067 Uiso 1 1 calc R . . H31F H 0.3288 -0.0979 -0.0885 0.067 Uiso 1 1 calc R . . C1R C 0.5976(6) 0.5502(7) 0.4192(3) 0.095(2) Uani 1 1 d U . . C2R C 0.5636(6) 0.4871(7) 0.3802(3) 0.093(2) Uani 1 1 d U . . H2R1 H 0.5297 0.5292 0.3553 0.140 Uiso 1 1 calc R . . H2R2 H 0.5282 0.4337 0.3894 0.140 Uiso 1 1 calc R . . H2R3 H 0.6095 0.4548 0.3689 0.140 Uiso 1 1 calc R . . C1S C 0.5515(3) 0.8615(3) 0.20642(13) 0.0374(7) Uani 1 1 d . . . C2S C 0.5800(3) 0.7681(3) 0.18794(16) 0.0418(8) Uani 1 1 d . . . H2S1 H 0.6395 0.7750 0.1872 0.063 Uiso 1 1 calc R . . H2S2 H 0.5467 0.7563 0.1563 0.063 Uiso 1 1 calc R . . H2S3 H 0.5729 0.7098 0.2078 0.063 Uiso 1 1 calc R . . C1T C 0.4098(3) 0.7365(4) 0.26961(16) 0.0458(10) Uani 1 1 d . . . C2T C 0.3881(3) 0.8355(4) 0.28626(18) 0.0495(11) Uani 1 1 d . . . H2T1 H 0.4035 0.8901 0.2668 0.074 Uiso 1 1 calc R . . H2T2 H 0.4189 0.8452 0.3186 0.074 Uiso 1 1 calc R . . H2T3 H 0.3275 0.8381 0.2846 0.074 Uiso 1 1 calc R . . N1A N 0.20006(16) 0.5892(2) 0.03056(8) 0.0233(4) Uani 1 1 d . . . N2A N 0.29089(14) 0.52398(16) 0.11015(7) 0.0164(4) Uani 1 1 d . . . N1B N 0.29540(16) 0.55059(18) -0.04880(8) 0.0200(4) Uani 1 1 d . . . N2B N 0.20817(16) 0.4279(2) -0.11318(8) 0.0216(4) Uani 1 1 d . . . N1R N 0.6244(8) 0.6025(8) 0.4523(4) 0.171(5) Uani 1 1 d . . . N1S N 0.5290(3) 0.9347(4) 0.22139(15) 0.0563(10) Uani 1 1 d . . . N1T N 0.4269(3) 0.6601(4) 0.25598(17) 0.0598(11) Uani 1 1 d U . . O1A O 0.16812(15) 0.3954(2) -0.01196(7) 0.0296(5) Uani 1 1 d . . . O2A O 0.22013(19) 0.32555(18) 0.09106(8) 0.0326(5) Uani 1 1 d . . . O1B O 0.33686(13) 0.40073(15) 0.02146(6) 0.0194(3) Uani 1 1 d . . . O2B O 0.29204(18) 0.25657(17) -0.06472(7) 0.0308(5) Uani 1 1 d . . . Zn1A Zn 0.23715(2) 0.43819(2) 0.051455(10) 0.01831(8) Uani 1 1 d . . . Zn1B Zn 0.26692(2) 0.39269(2) -0.044678(10) 0.01962(8) 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 C1A 0.088(3) 0.088(3) 0.090(3) -0.0043(19) 0.0223(19) -0.0077(19) C2A 0.072(2) 0.074(2) 0.071(2) -0.0004(17) 0.0178(17) -0.0085(18) C3A 0.0524(18) 0.0628(18) 0.0447(16) -0.0075(14) 0.0090(14) -0.0171(15) C4A 0.0246(12) 0.0532(15) 0.0201(10) -0.0019(10) 0.0072(9) -0.0098(11) C5A 0.0359(15) 0.0604(17) 0.0293(12) -0.0057(12) 0.0091(11) -0.0129(13) C6A 0.0341(15) 0.0729(19) 0.0279(13) -0.0009(13) 0.0046(11) -0.0136(14) C7A 0.0329(15) 0.0784(19) 0.0332(14) 0.0053(14) 0.0091(12) 0.0018(14) C8A 0.0339(15) 0.0648(18) 0.0319(13) 0.0078(13) 0.0104(11) 0.0073(13) C9A 0.0146(13) 0.088(3) 0.0170(11) 0.0116(14) 0.0046(9) 0.0057(15) C10A 0.0190(14) 0.055(2) 0.0243(13) 0.0155(13) 0.0089(10) 0.0142(13) C11A 0.0222(13) 0.0221(11) 0.0292(12) 0.0064(9) 0.0119(10) 0.0082(9) C12A 0.045(2) 0.0278(15) 0.050(2) 0.0180(14) 0.0261(17) 0.0129(14) C13A 0.054(3) 0.0176(13) 0.077(3) 0.0078(16) 0.030(2) 0.0012(14) C14A 0.040(2) 0.0213(14) 0.073(3) -0.0074(15) 0.0221(19) -0.0069(13) C15A 0.0251(15) 0.0227(12) 0.0416(16) -0.0082(11) 0.0106(12) -0.0047(10) C16A 0.0194(12) 0.0162(10) 0.0269(12) -0.0008(8) 0.0109(9) 0.0004(8) C17A 0.0140(11) 0.0250(11) 0.0152(9) -0.0016(8) 0.0021(7) 0.0010(8) C18A 0.0231(13) 0.0270(12) 0.0166(10) 0.0052(9) 0.0069(9) 0.0052(10) C19A 0.0246(15) 0.0504(19) 0.0183(11) 0.0109(11) 0.0070(10) 0.0157(13) C20A 0.040(2) 0.061(2) 0.0312(15) 0.0293(16) 0.0220(14) 0.0318(18) C21A 0.066(3) 0.0360(18) 0.048(2) 0.0238(16) 0.037(2) 0.0211(18) C22A 0.070(3) 0.0228(14) 0.0430(19) 0.0101(13) 0.0359(19) 0.0041(15) C23A 0.0389(17) 0.0215(12) 0.0237(12) 0.0040(9) 0.0150(11) 0.0004(11) C24A 0.0399(15) 0.0545(16) 0.0355(13) 0.0173(12) 0.0138(12) 0.0161(13) C25A 0.0616(18) 0.0664(18) 0.0577(17) 0.0072(11) 0.0136(11) 0.0061(11) C26A 0.0616(18) 0.0664(18) 0.0577(17) 0.0072(11) 0.0136(11) 0.0061(11) C27A 0.0616(18) 0.0664(18) 0.0577(17) 0.0072(11) 0.0136(11) 0.0061(11) C25' 0.048(3) 0.050(3) 0.047(3) 0.0022(11) 0.0100(12) 0.0004(12) C26' 0.048(3) 0.050(3) 0.047(3) 0.0022(11) 0.0100(12) 0.0004(12) C27' 0.048(3) 0.050(3) 0.047(3) 0.0022(11) 0.0100(12) 0.0004(12) C28A 0.0652(19) 0.0377(15) 0.0519(17) 0.0033(13) 0.0233(15) -0.0089(14) C29A 0.081(2) 0.059(2) 0.070(2) 0.0055(17) 0.0239(17) -0.0084(17) C30A 0.066(2) 0.0541(18) 0.0608(19) -0.0032(15) 0.0202(16) -0.0184(16) C31A 0.071(2) 0.0484(17) 0.0576(18) -0.0035(15) 0.0252(16) -0.0066(15) C1B 0.047(2) 0.049(2) 0.0329(17) 0.0087(15) 0.0056(15) 0.0189(18) C2B 0.0300(16) 0.0371(16) 0.0295(14) 0.0019(12) 0.0063(11) 0.0121(13) C3B 0.0264(14) 0.0286(13) 0.0234(12) 0.0007(10) 0.0029(10) 0.0055(11) C4B 0.0179(11) 0.0205(10) 0.0190(10) -0.0053(8) 0.0062(8) 0.0012(8) C5B 0.0180(12) 0.0280(12) 0.0190(10) -0.0038(9) 0.0044(8) 0.0047(9) C6B 0.0177(12) 0.0359(15) 0.0235(12) -0.0073(10) 0.0043(9) 0.0014(10) C7B 0.0208(13) 0.0340(14) 0.0293(13) -0.0125(11) 0.0067(10) -0.0038(11) C8B 0.0209(13) 0.0251(12) 0.0312(13) -0.0085(10) 0.0103(10) -0.0034(10) C9B 0.0182(12) 0.0207(11) 0.0227(11) -0.0041(8) 0.0071(8) -0.0002(8) C10B 0.0193(12) 0.0206(11) 0.0270(12) -0.0005(9) 0.0109(9) -0.0005(9) C11B 0.0176(12) 0.0260(12) 0.0261(12) 0.0061(9) 0.0089(9) 0.0027(9) C12B 0.0312(17) 0.0261(13) 0.0387(16) 0.0113(12) 0.0087(12) 0.0022(11) C13B 0.039(2) 0.0343(17) 0.055(2) 0.0203(16) 0.0051(17) 0.0076(15) C14B 0.0295(18) 0.048(2) 0.045(2) 0.0223(16) 0.0035(14) 0.0109(15) C15B 0.0221(14) 0.0440(18) 0.0280(14) 0.0105(12) 0.0045(10) 0.0066(12) C16B 0.0188(12) 0.0300(13) 0.0225(11) 0.0057(10) 0.0077(9) 0.0033(10) C17B 0.0145(11) 0.0369(14) 0.0173(10) 0.0007(9) 0.0042(8) 0.0035(10) C18B 0.0162(12) 0.0339(13) 0.0175(10) -0.0040(9) 0.0044(8) -0.0008(10) C19B 0.0172(12) 0.0433(16) 0.0184(11) -0.0079(10) 0.0039(9) -0.0040(11) C20B 0.0205(13) 0.0391(16) 0.0233(12) -0.0126(11) 0.0068(9) -0.0072(11) C21B 0.0245(14) 0.0293(13) 0.0260(12) -0.0111(10) 0.0088(10) -0.0084(10) C22B 0.0235(13) 0.0232(12) 0.0231(11) -0.0072(9) 0.0060(9) -0.0058(10) C23B 0.0198(12) 0.0260(12) 0.0187(10) -0.0060(9) 0.0031(8) -0.0027(9) C24B 0.0272(16) 0.0490(19) 0.0278(14) -0.0194(13) 0.0082(11) -0.0102(13) C25B 0.0267(18) 0.075(3) 0.0416(19) -0.027(2) 0.0091(14) -0.0204(18) C26B 0.038(2) 0.070(3) 0.0253(15) -0.0178(16) 0.0111(13) -0.0091(18) C27B 0.057(3) 0.055(3) 0.041(2) -0.0294(19) 0.0085(18) -0.003(2) C28B 0.0309(16) 0.0206(12) 0.0304(14) -0.0048(10) 0.0023(11) -0.0021(10) C29B 0.0417(16) 0.0374(14) 0.0568(17) 0.0044(13) -0.0060(13) -0.0029(13) C30B 0.074(4) 0.063(3) 0.0340(19) 0.0146(19) 0.021(2) 0.025(3) C31B 0.063(3) 0.0216(14) 0.044(2) -0.0059(13) 0.0011(18) 0.0042(15) C1R 0.094(3) 0.095(3) 0.096(3) 0.0010(10) 0.0206(11) -0.0013(10) C2R 0.093(2) 0.093(2) 0.094(2) -0.0009(10) 0.0221(11) 0.0000(10) C1S 0.0329(18) 0.048(2) 0.0328(16) 0.0030(14) 0.0094(13) -0.0003(15) C2S 0.0327(19) 0.0419(19) 0.054(2) 0.0007(17) 0.0163(16) -0.0014(15) C1T 0.032(2) 0.060(3) 0.048(2) -0.0207(19) 0.0156(16) -0.0082(17) C2T 0.038(2) 0.053(2) 0.066(3) -0.022(2) 0.028(2) -0.0130(18) N1A 0.0176(11) 0.0342(12) 0.0191(9) 0.0083(8) 0.0063(8) 0.0077(9) N2A 0.0153(9) 0.0173(8) 0.0166(8) -0.0003(7) 0.0033(7) 0.0008(7) N1B 0.0191(11) 0.0209(9) 0.0216(10) 0.0020(7) 0.0080(8) 0.0019(8) N2B 0.0186(11) 0.0284(11) 0.0188(9) 0.0016(8) 0.0063(7) 0.0029(8) N1R 0.198(13) 0.142(8) 0.134(8) -0.002(7) -0.043(8) -0.072(8) N1S 0.061(3) 0.059(2) 0.051(2) -0.0078(18) 0.0167(19) 0.006(2) N1T 0.0591(14) 0.0605(13) 0.0602(13) -0.0063(9) 0.0141(9) 0.0017(9) O1A 0.0246(11) 0.0472(13) 0.0170(8) -0.0061(8) 0.0048(7) -0.0166(9) O2A 0.0529(16) 0.0247(10) 0.0218(9) -0.0012(8) 0.0120(9) -0.0174(10) O1B 0.0213(9) 0.0189(8) 0.0173(8) -0.0020(6) 0.0031(6) -0.0008(7) O2B 0.0445(14) 0.0249(10) 0.0185(9) -0.0059(7) -0.0028(8) 0.0057(9) Zn1A 0.01852(15) 0.02320(14) 0.01276(12) -0.00069(9) 0.00255(9) -0.00569(11) Zn1B 0.02437(16) 0.01992(14) 0.01434(13) -0.00155(9) 0.00390(10) 0.00026(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 C1A C2A 1.311(10) . ? C2A C3A 1.455(8) . ? C3A C5A 1.479(7) . ? C4A O1A 1.353(5) . ? C4A C9A 1.395(6) . ? C4A C5A 1.415(5) . ? C5A C6A 1.439(7) . ? C6A C7A 1.300(7) . ? C7A C8A 1.374(7) . ? C8A C9A 1.424(5) . ? C9A C10A 1.438(6) . ? C10A N1A 1.286(4) . ? C11A C12A 1.397(4) . ? C11A C16A 1.403(4) . ? C11A N1A 1.418(4) . ? C12A C13A 1.397(7) . ? C13A C14A 1.376(7) . ? C14A C15A 1.387(5) . ? C15A C16A 1.399(4) . ? C16A N2A 1.409(3) . ? C17A N2A 1.292(3) . ? C17A C18A 1.442(4) . ? C18A C19A 1.416(4) . ? C18A C23A 1.428(4) . ? C19A C20A 1.381(5) . ? C20A C21A 1.396(7) . ? C20A C24A 1.525(5) . ? C21A C22A 1.367(6) . ? C22A C23A 1.440(4) . ? C22A C28A 1.559(7) . ? C23A O2A 1.294(4) . ? C24A C27' 1.375(16) . ? C24A C26' 1.455(17) . ? C24A C26A 1.460(10) . ? C24A C25A 1.508(10) . ? C24A C25' 1.547(5) . ? C24A C27A 1.566(5) . ? C28A C30A 1.492(8) . ? C28A C29A 1.536(7) . ? C28A C31A 1.552(7) . ? C1B C2B 1.325(5) . ? C2B C3B 1.496(4) . ? C3B C5B 1.512(4) . ? C4B O1B 1.331(3) . ? C4B C5B 1.414(4) . ? C4B C9B 1.420(4) . ? C5B C6B 1.391(4) . ? C6B C7B 1.396(5) . ? C7B C8B 1.378(5) . ? C8B C9B 1.408(4) . ? C9B C10B 1.445(4) . ? C10B N1B 1.292(4) . ? C11B C12B 1.398(4) . ? C11B C16B 1.410(4) . ? C11B N1B 1.415(4) . ? C12B C13B 1.393(5) . ? C13B C14B 1.380(7) . ? C14B C15B 1.381(5) . ? C15B C16B 1.401(4) . ? C16B N2B 1.412(4) . ? C17B N2B 1.295(4) . ? C17B C18B 1.440(4) . ? C18B C19B 1.416(4) . ? C18B C23B 1.433(4) . ? C19B C20B 1.377(5) . ? C20B C21B 1.411(5) . ? C20B C24B 1.541(4) . ? C21B C22B 1.388(4) . ? C22B C23B 1.439(4) . ? C22B C28B 1.539(4) . ? C23B O2B 1.301(3) . ? C24B C25B 1.534(5) . ? C24B C27B 1.536(6) . ? C24B C26B 1.541(6) . ? C28B C31B 1.522(5) . ? C28B C30B 1.527(6) . ? C28B C29B 1.532(5) . ? C1R N1R 1.188(12) . ? C1R C2R 1.420(12) . ? C1S N1S 1.144(6) . ? C1S C2S 1.450(6) . ? C1T N1T 1.131(6) . ? C1T C2T 1.449(6) . ? N1A Zn1A 2.106(3) . ? N2A Zn1A 2.079(2) . ? N1B Zn1B 2.116(2) . ? N2B Zn1B 2.081(2) . ? O1A Zn1A 2.031(2) . ? O1A Zn1B 2.055(2) . ? O2A Zn1A 1.932(2) . ? O1B Zn1B 2.0274(19) . ? O1B Zn1A 2.076(2) . ? O2B Zn1B 1.940(2) . ? Zn1A Zn1B 3.0373(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 C1A C2A C3A 127.5(7) . . ? C2A C3A C5A 113.2(5) . . ? O1A C4A C9A 123.6(3) . . ? O1A C4A C5A 118.3(4) . . ? C9A C4A C5A 118.1(4) . . ? C4A C5A C6A 117.2(4) . . ? C4A C5A C3A 119.1(4) . . ? C6A C5A C3A 123.6(4) . . ? C7A C6A C5A 124.1(4) . . ? C6A C7A C8A 119.8(4) . . ? C7A C8A C9A 119.9(5) . . ? C4A C9A C8A 120.8(4) . . ? C4A C9A C10A 124.6(3) . . ? C8A C9A C10A 114.6(4) . . ? N1A C10A C9A 124.5(4) . . ? C12A C11A C16A 119.9(3) . . ? C12A C11A N1A 124.3(3) . . ? C16A C11A N1A 115.7(2) . . ? C11A C12A C13A 119.5(4) . . ? C14A C13A C12A 120.4(3) . . ? C13A C14A C15A 120.7(4) . . ? C14A C15A C16A 119.8(4) . . ? C15A C16A C11A 119.7(3) . . ? C15A C16A N2A 125.1(3) . . ? C11A C16A N2A 115.2(2) . . ? N2A C17A C18A 125.2(2) . . ? C19A C18A C23A 120.1(3) . . ? C19A C18A C17A 115.8(3) . . ? C23A C18A C17A 124.1(2) . . ? C20A C19A C18A 121.6(4) . . ? C19A C20A C21A 117.2(3) . . ? C19A C20A C24A 123.1(4) . . ? C21A C20A C24A 119.7(4) . . ? C22A C21A C20A 124.8(3) . . ? C21A C22A C23A 118.6(4) . . ? C21A C22A C28A 122.4(3) . . ? C23A C22A C28A 119.0(4) . . ? O2A C23A C18A 123.5(3) . . ? O2A C23A C22A 118.7(3) . . ? C18A C23A C22A 117.7(3) . . ? C27' C24A C26' 102.4(10) . . ? C27' C24A C26A 61.9(8) . . ? C26' C24A C26A 127.6(8) . . ? C27' C24A C25A 123.8(8) . . ? C26' C24A C25A 23.3(6) . . ? C26A C24A C25A 125.8(6) . . ? C27' C24A C20A 113.7(7) . . ? C26' C24A C20A 118.9(7) . . ? C26A C24A C20A 112.8(5) . . ? C25A C24A C20A 110.9(5) . . ? C27' C24A C25' 98.9(9) . . ? C26' C24A C25' 112.6(9) . . ? C26A C24A C25' 38.4(6) . . ? C25A C24A C25' 97.7(7) . . ? C20A C24A C25' 108.4(6) . . ? C27' C24A C27A 30.5(7) . . ? C26' C24A C27A 78.7(8) . . ? C26A C24A C27A 91.7(6) . . ? C25A C24A C27A 102.0(6) . . ? C20A C24A C27A 110.1(4) . . ? C25' C24A C27A 126.2(7) . . ? C30A C28A C29A 107.1(5) . . ? C30A C28A C31A 111.3(5) . . ? C29A C28A C31A 106.2(4) . . ? C30A C28A C22A 110.8(4) . . ? C29A C28A C22A 112.0(4) . . ? C31A C28A C22A 109.3(4) . . ? C1B C2B C3B 123.9(4) . . ? C2B C3B C5B 116.2(3) . . ? O1B C4B C5B 117.9(2) . . ? O1B C4B C9B 122.4(2) . . ? C5B C4B C9B 119.6(3) . . ? C6B C5B C4B 119.0(3) . . ? C6B C5B C3B 123.8(3) . . ? C4B C5B C3B 117.2(3) . . ? C5B C6B C7B 121.7(3) . . ? C8B C7B C6B 119.4(3) . . ? C7B C8B C9B 121.1(3) . . ? C8B C9B C4B 119.0(3) . . ? C8B C9B C10B 116.9(3) . . ? C4B C9B C10B 124.0(2) . . ? N1B C10B C9B 125.4(3) . . ? C12B C11B C16B 119.7(3) . . ? C12B C11B N1B 123.9(3) . . ? C16B C11B N1B 116.3(2) . . ? C13B C12B C11B 119.2(4) . . ? C14B C13B C12B 121.1(3) . . ? C13B C14B C15B 120.5(3) . . ? C14B C15B C16B 119.7(3) . . ? C15B C16B C11B 119.8(3) . . ? C15B C16B N2B 125.1(3) . . ? C11B C16B N2B 115.1(2) . . ? N2B C17B C18B 125.8(3) . . ? C19B C18B C23B 120.2(3) . . ? C19B C18B C17B 115.8(3) . . ? C23B C18B C17B 123.7(2) . . ? C20B C19B C18B 122.6(3) . . ? C19B C20B C21B 116.5(3) . . ? C19B C20B C24B 120.9(3) . . ? C21B C20B C24B 122.5(3) . . ? C22B C21B C20B 124.4(3) . . ? C21B C22B C23B 118.8(3) . . ? C21B C22B C28B 120.7(3) . . ? C23B C22B C28B 120.6(2) . . ? O2B C23B C18B 123.2(3) . . ? O2B C23B C22B 119.3(3) . . ? C18B C23B C22B 117.5(2) . . ? C25B C24B C27B 109.7(4) . . ? C25B C24B C20B 110.2(3) . . ? C27B C24B C20B 112.0(3) . . ? C25B C24B C26B 108.4(4) . . ? C27B C24B C26B 107.6(3) . . ? C20B C24B C26B 108.9(3) . . ? C31B C28B C30B 107.2(3) . . ? C31B C28B C29B 107.0(3) . . ? C30B C28B C29B 109.5(4) . . ? C31B C28B C22B 112.4(3) . . ? C30B C28B C22B 111.0(3) . . ? C29B C28B C22B 109.6(3) . . ? N1R C1R C2R 178.4(12) . . ? N1S C1S C2S 179.4(5) . . ? N1T C1T C2T 178.8(6) . . ? C10A N1A C11A 120.7(3) . . ? C10A N1A Zn1A 126.6(3) . . ? C11A N1A Zn1A 112.28(17) . . ? C17A N2A C16A 121.7(2) . . ? C17A N2A Zn1A 124.70(18) . . ? C16A N2A Zn1A 113.57(17) . . ? C10B N1B C11B 121.9(2) . . ? C10B N1B Zn1B 126.2(2) . . ? C11B N1B Zn1B 111.69(19) . . ? C17B N2B C16B 121.6(2) . . ? C17B N2B Zn1B 125.4(2) . . ? C16B N2B Zn1B 112.85(18) . . ? C4A O1A Zn1A 124.9(2) . . ? C4A O1A Zn1B 117.42(19) . . ? Zn1A O1A Zn1B 96.03(10) . . ? C23A O2A Zn1A 129.2(2) . . ? C4B O1B Zn1B 127.21(17) . . ? C4B O1B Zn1A 112.64(15) . . ? Zn1B O1B Zn1A 95.50(9) . . ? C23B O2B Zn1B 131.7(2) . . ? O2A Zn1A O1A 102.85(10) . . ? O2A Zn1A O1B 108.16(10) . . ? O1A Zn1A O1B 82.49(9) . . ? O2A Zn1A N2A 89.76(9) . . ? O1A Zn1A N2A 162.83(10) . . ? O1B Zn1A N2A 104.83(8) . . ? O2A Zn1A N1A 144.42(11) . . ? O1A Zn1A N1A 85.61(11) . . ? O1B Zn1A N1A 107.19(9) . . ? N2A Zn1A N1A 77.42(9) . . ? O2A Zn1A Zn1B 119.34(7) . . ? O1A Zn1A Zn1B 42.29(7) . . ? O1B Zn1A Zn1B 41.64(5) . . ? N2A Zn1A Zn1B 138.97(6) . . ? N1A Zn1A Zn1B 90.28(7) . . ? O2B Zn1B O1B 103.18(9) . . ? O2B Zn1B O1A 113.57(11) . . ? O1B Zn1B O1A 83.08(9) . . ? O2B Zn1B N2B 89.33(9) . . ? O1B Zn1B N2B 163.27(9) . . ? O1A Zn1B N2B 102.26(9) . . ? O2B Zn1B N1B 143.61(11) . . ? O1B Zn1B N1B 85.51(9) . . ? O1A Zn1B N1B 102.46(10) . . ? N2B Zn1B N1B 77.88(10) . . ? O2B Zn1B Zn1A 123.43(7) . . ? O1B Zn1B Zn1A 42.86(6) . . ? O1A Zn1B Zn1A 41.67(6) . . ? N2B Zn1B Zn1A 136.56(7) . . ? N1B Zn1B Zn1A 86.98(6) . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 33.90 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 2.081 _refine_diff_density_min -1.122 _refine_diff_density_rms 0.123 # Attachment 'AWK540_0m1.cif' data_awk540_0m _database_code_depnum_ccdc_archive 'CCDC 756457' #TrackingRef 'AWK540_0m1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C70 H85 N7 O4 Zn2' _chemical_formula_weight 1219.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.4320(5) _cell_length_b 15.3730(5) _cell_length_c 17.8265(6) _cell_angle_alpha 108.669(2) _cell_angle_beta 91.977(2) _cell_angle_gamma 101.818(2) _cell_volume 3393.5(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9818 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 34.83 _exptl_crystal_description BLOCK _exptl_crystal_colour yellow _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.193 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1292 _exptl_absorpt_coefficient_mu 0.757 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6049 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ; SADABS Version 2008/1 Bruker-Nonius Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_special_details ; It should be noted that the esd's of the cell dimensions are probably too low; they should be multiplied by a factor of 2 to 10 ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_specimen_suppport 'magnetic support whith 10 micron nylon fiber cryoloop' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'rotating anode X-ray tube' _diffrn_source_type 'Bruker-Nonius FR 591' _diffrn_source_power 50 _diffrn_source_current 70 _diffrn_source_size '3 mm x 0.3 mm fine focus' _diffrn_radiation_monochromator 'Multilayer Montel 200 mirrors' _diffrn_detector_type '4K CCD area detector APEX II' _diffrn_measurement_device_type 'Kappa 4-axis goniometer bruker-nonius' _diffrn_measurement_method ; Fullsphere data collection, phi and omega scans ; _diffrn_detector_area_resol_mean 512 _diffrn_reflns_number 64628 _diffrn_reflns_av_R_equivalents 0.0255 _diffrn_reflns_av_sigmaI/netI 0.0346 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.21 _diffrn_reflns_theta_max 34.94 _reflns_number_total 27120 _reflns_number_gt 21585 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v2009.1-0' _computing_cell_refinement 'Bruker APEX2 v2009.1-0' _computing_data_reduction 'Bruker SAINT V7.60A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXS-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0668P)^2^+1.8460P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 27120 _refine_ls_number_parameters 829 _refine_ls_number_restraints 98 _refine_ls_R_factor_all 0.0603 _refine_ls_R_factor_gt 0.0442 _refine_ls_wR_factor_ref 0.1292 _refine_ls_wR_factor_gt 0.1185 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.073 _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 C1A C 0.14067(10) 0.29723(10) 0.48797(9) 0.0184(2) Uani 1 1 d . A . C2A C 0.24627(10) 0.29438(10) 0.47943(10) 0.0187(2) Uani 1 1 d . . . C3A C 0.30945(11) 0.35447(10) 0.43591(10) 0.0207(3) Uani 1 1 d . . . C4A C 0.26425(13) 0.32161(14) 0.34839(11) 0.0290(3) Uani 1 1 d . . . H4A1 H 0.3071 0.3575 0.3201 0.043 Uiso 1 1 calc R . . H4A2 H 0.1948 0.3320 0.3458 0.043 Uiso 1 1 calc R . . H4A3 H 0.2620 0.2543 0.3235 0.043 Uiso 1 1 calc R . . C5A C 0.31123(13) 0.45988(11) 0.47565(13) 0.0285(3) Uani 1 1 d . . . H5A1 H 0.3434 0.4815 0.5306 0.043 Uiso 1 1 calc R . . H5A2 H 0.2410 0.4688 0.4756 0.043 Uiso 1 1 calc R . . H5A3 H 0.3504 0.4963 0.4459 0.043 Uiso 1 1 calc R . . C6A C 0.42117(12) 0.34572(13) 0.43667(13) 0.0299(4) Uani 1 1 d . . . H6A1 H 0.4522 0.3663 0.4919 0.045 Uiso 1 1 calc R . . H6A2 H 0.4590 0.3854 0.4089 0.045 Uiso 1 1 calc R . . H6A3 H 0.4237 0.2799 0.4098 0.045 Uiso 1 1 calc R . . C7A C 0.28734(11) 0.23638(11) 0.51110(11) 0.0227(3) Uani 1 1 d . . . H7A H 0.3574 0.2357 0.5062 0.027 Uiso 1 1 calc R . . C8A C 0.23226(12) 0.17830(12) 0.55010(12) 0.0267(3) Uani 1 1 d . A . C9A C 0.28428(16) 0.11590(17) 0.58237(16) 0.0421(5) Uani 1 1 d D . . C10A C 0.3722(2) 0.1831(2) 0.6480(2) 0.0513(4) Uani 0.80 1 d PU A 1 H10A H 0.3429 0.2244 0.6911 0.077 Uiso 0.80 1 calc PR A 1 H10B H 0.4203 0.2215 0.6246 0.077 Uiso 0.80 1 calc PR A 1 H10C H 0.4084 0.1453 0.6693 0.077 Uiso 0.80 1 calc PR A 1 C11A C 0.3364(3) 0.0569(3) 0.5157(2) 0.0513(4) Uani 0.80 1 d PU A 1 H11A H 0.3725 0.0188 0.5365 0.077 Uiso 0.80 1 calc PR A 1 H11B H 0.3854 0.0990 0.4960 0.077 Uiso 0.80 1 calc PR A 1 H11C H 0.2846 0.0154 0.4721 0.077 Uiso 0.80 1 calc PR A 1 C12A C 0.2131(2) 0.0550(3) 0.6160(2) 0.0513(4) Uani 0.80 1 d PU A 1 H12A H 0.1568 0.0155 0.5753 0.077 Uiso 0.80 1 calc PR A 1 H12B H 0.1857 0.0945 0.6616 0.077 Uiso 0.80 1 calc PR A 1 H12C H 0.2497 0.0147 0.6335 0.077 Uiso 0.80 1 calc PR A 1 C10C C 0.2707(10) 0.1359(10) 0.6735(9) 0.0513(4) Uani 0.20 1 d PU A 2 H10D H 0.2983 0.0912 0.6921 0.077 Uiso 0.20 1 calc PR A 2 H10E H 0.1978 0.1284 0.6809 0.077 Uiso 0.20 1 calc PR A 2 H10F H 0.3074 0.2004 0.7042 0.077 Uiso 0.20 1 calc PR A 2 C11C C 0.3867(7) 0.0973(10) 0.5573(9) 0.0513(4) Uani 0.20 1 d PDU A 2 H11D H 0.4409 0.1534 0.5846 0.077 Uiso 0.20 1 calc PR A 2 H11E H 0.3859 0.0829 0.4995 0.077 Uiso 0.20 1 calc PR A 2 H11F H 0.3994 0.0438 0.5715 0.077 Uiso 0.20 1 calc PR A 2 C12C C 0.2102(7) 0.0162(5) 0.5598(9) 0.0513(4) Uani 0.20 1 d PDU A 2 H12D H 0.2017 -0.0143 0.5018 0.077 Uiso 0.20 1 calc PR A 2 H12E H 0.1435 0.0231 0.5784 0.077 Uiso 0.20 1 calc PR A 2 H12F H 0.2390 -0.0225 0.5850 0.077 Uiso 0.20 1 calc PR A 2 C13A C 0.13130(12) 0.18151(12) 0.55839(12) 0.0267(3) Uani 1 1 d . . . H13A H 0.0923 0.1434 0.5846 0.032 Uiso 1 1 calc R A . C14A C 0.08444(11) 0.24013(11) 0.52877(10) 0.0212(3) Uani 1 1 d . A . C15A C -0.02340(11) 0.23041(11) 0.53652(10) 0.0214(3) Uani 1 1 d . . . H15A H -0.0567 0.1815 0.5548 0.026 Uiso 1 1 calc R A . C16A C -0.18561(10) 0.26403(10) 0.51813(9) 0.0169(2) Uani 1 1 d . . . C17A C -0.24300(11) 0.21400(10) 0.56074(10) 0.0203(3) Uani 1 1 d . A . H17A H -0.2099 0.1915 0.5962 0.024 Uiso 1 1 calc R . . C18A C -0.34914(12) 0.19716(11) 0.55107(11) 0.0239(3) Uani 1 1 d . . . H18A H -0.3887 0.1622 0.5795 0.029 Uiso 1 1 calc R A . C19A C -0.39763(11) 0.23120(12) 0.50002(11) 0.0241(3) Uani 1 1 d . A . H19A H -0.4702 0.2192 0.4938 0.029 Uiso 1 1 calc R . . C20A C -0.34136(11) 0.28248(11) 0.45802(10) 0.0214(3) Uani 1 1 d . . . H20A H -0.3751 0.3063 0.4239 0.026 Uiso 1 1 calc R A . C21A C -0.23501(10) 0.29878(10) 0.46630(9) 0.0173(2) Uani 1 1 d . A . C22A C -0.19666(11) 0.35014(10) 0.35675(10) 0.0201(3) Uani 1 1 d . A . H22A H -0.2618 0.3127 0.3311 0.024 Uiso 1 1 calc R . . C23A C -0.13358(11) 0.40165(10) 0.31357(10) 0.0201(3) Uani 1 1 d . A . C24A C -0.16700(13) 0.38149(11) 0.23280(10) 0.0239(3) Uani 1 1 d . . . H24A H -0.2279 0.3346 0.2100 0.029 Uiso 1 1 calc R . . C25A C -0.11491(14) 0.42715(12) 0.18502(11) 0.0266(3) Uani 1 1 d . B . C26A C -0.15256(17) 0.40476(14) 0.09778(12) 0.0363(4) Uani 1 1 d D . . C27A C -0.1588(4) 0.4940(3) 0.0824(3) 0.0379(9) Uani 0.50 1 d P B 1 H27A H -0.0924 0.5390 0.0994 0.057 Uiso 0.50 1 calc PR B 1 H27B H -0.2112 0.5213 0.1124 0.057 Uiso 0.50 1 calc PR B 1 H27C H -0.1769 0.4800 0.0254 0.057 Uiso 0.50 1 calc PR B 1 C28A C -0.2491(3) 0.3296(3) 0.0684(3) 0.0415(10) Uani 0.50 1 d PD B 1 H28A H -0.2664 0.3173 0.0116 0.062 Uiso 0.50 1 calc PR B 1 H28B H -0.3048 0.3507 0.0980 0.062 Uiso 0.50 1 calc PR B 1 H28C H -0.2392 0.2717 0.0765 0.062 Uiso 0.50 1 calc PR B 1 C29A C -0.0665(4) 0.3655(4) 0.0467(3) 0.0487(12) Uani 0.50 1 d PD B 1 H29A H -0.0866 0.3524 -0.0099 0.073 Uiso 0.50 1 calc PR B 1 H29B H -0.0583 0.3073 0.0551 0.073 Uiso 0.50 1 calc PR B 1 H29C H -0.0016 0.4127 0.0634 0.073 Uiso 0.50 1 calc PR B 1 C27C C -0.1784(5) 0.2990(3) 0.0562(3) 0.0440(11) Uani 0.50 1 d P B 2 H27D H -0.2145 0.2841 0.0033 0.066 Uiso 0.50 1 calc PR B 2 H27E H -0.2221 0.2684 0.0877 0.066 Uiso 0.50 1 calc PR B 2 H27F H -0.1151 0.2761 0.0506 0.066 Uiso 0.50 1 calc PR B 2 C28C C -0.2612(4) 0.4315(4) 0.0953(3) 0.0560(14) Uani 0.50 1 d PDU B 2 H28D H -0.2525 0.4996 0.1209 0.084 Uiso 0.50 1 calc PR B 2 H28E H -0.3073 0.3982 0.1238 0.084 Uiso 0.50 1 calc PR B 2 H28F H -0.2903 0.4130 0.0399 0.084 Uiso 0.50 1 calc PR B 2 C29C C -0.0867(5) 0.4580(4) 0.0534(3) 0.0560(14) Uani 0.50 1 d PDU B 2 H29D H -0.1194 0.4411 -0.0009 0.084 Uiso 0.50 1 calc PR B 2 H29E H -0.0197 0.4420 0.0513 0.084 Uiso 0.50 1 calc PR B 2 H29F H -0.0779 0.5259 0.0807 0.084 Uiso 0.50 1 calc PR B 2 C30A C -0.02633(15) 0.49708(12) 0.22162(11) 0.0282(3) Uani 1 1 d . . . H30A H 0.0103 0.5309 0.1911 0.034 Uiso 1 1 calc R B . C31A C 0.00928(13) 0.51837(12) 0.30045(11) 0.0246(3) Uani 1 1 d . B . H31A H 0.0695 0.5663 0.3228 0.029 Uiso 1 1 calc R . . C35A C -0.04180(11) 0.47048(10) 0.34831(9) 0.0195(2) Uani 1 1 d . . . N1A N -0.07808(9) 0.28357(9) 0.52029(8) 0.0175(2) Uani 1 1 d . A . N2A N -0.17066(9) 0.35146(9) 0.42763(8) 0.0179(2) Uani 1 1 d . . . O1A O 0.10068(8) 0.34898(8) 0.45581(8) 0.0218(2) Uani 1 1 d . . . O2A O -0.00271(8) 0.48944(8) 0.42265(7) 0.01975(19) Uani 1 1 d . . . Zn1A Zn -0.021459(12) 0.394263(11) 0.481718(11) 0.01674(4) Uani 1 1 d . . . C1B C 0.16980(11) 0.26916(10) 0.06234(10) 0.0210(3) Uani 1 1 d . . . C2B C 0.25029(12) 0.31524(11) 0.02743(11) 0.0230(3) Uani 1 1 d . . . C3B C 0.27451(15) 0.26450(13) -0.05670(12) 0.0318(4) Uani 1 1 d . . . C4B C 0.30491(19) 0.17220(15) -0.06040(16) 0.0429(5) Uani 1 1 d . . . H4B1 H 0.3669 0.1865 -0.0240 0.064 Uiso 1 1 calc R . . H4B2 H 0.3179 0.1396 -0.1149 0.064 Uiso 1 1 calc R . . H4B3 H 0.2492 0.1317 -0.0447 0.064 Uiso 1 1 calc R . . C5B C 0.36388(19) 0.32404(17) -0.08272(16) 0.0449(5) Uani 1 1 d . . . H5B1 H 0.3484 0.3847 -0.0794 0.067 Uiso 1 1 calc R . . H5B2 H 0.3740 0.2905 -0.1377 0.067 Uiso 1 1 calc R . . H5B3 H 0.4263 0.3350 -0.0477 0.067 Uiso 1 1 calc R . . C6B C 0.1812(2) 0.2427(2) -0.11770(15) 0.0485(6) Uani 1 1 d . . . H6B1 H 0.1249 0.1981 -0.1069 0.073 Uiso 1 1 calc R . . H6B2 H 0.1994 0.2149 -0.1715 0.073 Uiso 1 1 calc R . . H6B3 H 0.1597 0.3011 -0.1135 0.073 Uiso 1 1 calc R . . C7B C 0.30447(12) 0.40502(11) 0.07143(12) 0.0259(3) Uani 1 1 d . . . H7B H 0.3574 0.4347 0.0477 0.031 Uiso 1 1 calc R . . C8B C 0.28678(12) 0.45568(11) 0.14899(12) 0.0268(3) Uani 1 1 d . C . C9B C 0.34989(15) 0.55595(13) 0.19300(15) 0.0387(5) Uani 1 1 d D . . C10B C 0.4637(2) 0.5524(2) 0.1986(3) 0.0447(8) Uani 0.70 1 d P C 1 H10X H 0.5058 0.6165 0.2231 0.067 Uiso 0.70 1 calc PR C 1 H10Y H 0.4828 0.5245 0.1450 0.067 Uiso 0.70 1 calc PR C 1 H10Z H 0.4748 0.5139 0.2312 0.067 Uiso 0.70 1 calc PR C 1 C11B C 0.3161(3) 0.6034(2) 0.2678(2) 0.0525(9) Uani 0.70 1 d PU C 1 H11X H 0.2431 0.6015 0.2600 0.079 Uiso 0.70 1 calc PR C 1 H11Y H 0.3548 0.6691 0.2883 0.079 Uiso 0.70 1 calc PR C 1 H11Z H 0.3276 0.5718 0.3061 0.079 Uiso 0.70 1 calc PR C 1 C12B C 0.3438(3) 0.61826(19) 0.1365(2) 0.0405(7) Uani 0.70 1 d P C 1 H12X H 0.2723 0.6191 0.1247 0.061 Uiso 0.70 1 calc PR C 1 H12Y H 0.3721 0.5908 0.0866 0.061 Uiso 0.70 1 calc PR C 1 H12Z H 0.3834 0.6828 0.1636 0.061 Uiso 0.70 1 calc PR C 1 C10D C 0.2764(8) 0.6220(6) 0.2026(6) 0.054(2) Uani 0.30 1 d PU C 2 H10G H 0.3128 0.6865 0.2337 0.081 Uiso 0.30 1 calc PR C 2 H10H H 0.2192 0.6016 0.2303 0.081 Uiso 0.30 1 calc PR C 2 H10I H 0.2503 0.6201 0.1500 0.081 Uiso 0.30 1 calc PR C 2 C11D C 0.4567(6) 0.5808(9) 0.1712(8) 0.069(3) Uani 0.30 1 d PDU C 2 H11G H 0.4535 0.5841 0.1172 0.104 Uiso 0.30 1 calc PR C 2 H11H H 0.4932 0.5324 0.1733 0.104 Uiso 0.30 1 calc PR C 2 H11I H 0.4930 0.6420 0.2089 0.104 Uiso 0.30 1 calc PR C 2 C12D C 0.3706(6) 0.5655(5) 0.2837(3) 0.0449(19) Uani 0.30 1 d PD C 2 H12G H 0.4154 0.5242 0.2884 0.067 Uiso 0.30 1 calc PR C 2 H12H H 0.3056 0.5472 0.3041 0.067 Uiso 0.30 1 calc PR C 2 H12I H 0.4037 0.6310 0.3147 0.067 Uiso 0.30 1 calc PR C 2 C13B C 0.21148(12) 0.41056(11) 0.18266(11) 0.0259(3) Uani 1 1 d . . . H13B H 0.1978 0.4425 0.2351 0.031 Uiso 1 1 calc R C . C14B C 0.15355(11) 0.31800(10) 0.14178(10) 0.0210(3) Uani 1 1 d . C . C15B C 0.07605(11) 0.28171(10) 0.18498(10) 0.0204(3) Uani 1 1 d . . . H15B H 0.0668 0.3229 0.2355 0.024 Uiso 1 1 calc R C . C16B C -0.06074(10) 0.16870(9) 0.20321(9) 0.0169(2) Uani 1 1 d . . . C17B C -0.05216(12) 0.18681(11) 0.28481(10) 0.0217(3) Uani 1 1 d . C . H17B H 0.0097 0.2231 0.3169 0.026 Uiso 1 1 calc R . . C18B C -0.13536(13) 0.15116(12) 0.31905(10) 0.0240(3) Uani 1 1 d . . . H18B H -0.1292 0.1612 0.3746 0.029 Uiso 1 1 calc R C . C19B C -0.22743(12) 0.10102(12) 0.27301(10) 0.0241(3) Uani 1 1 d . C . H19B H -0.2849 0.0804 0.2977 0.029 Uiso 1 1 calc R . . C20B C -0.23565(11) 0.08101(11) 0.19123(10) 0.0219(3) Uani 1 1 d . . . H20B H -0.2983 0.0460 0.1597 0.026 Uiso 1 1 calc R C . C21B C -0.15155(10) 0.11249(10) 0.15561(9) 0.0174(2) Uani 1 1 d . . . C22B C 0.22615(11) -0.06803(10) -0.02293(9) 0.0192(2) Uani 1 1 d . . . H22B H 0.2893 -0.0756 -0.0435 0.023 Uiso 1 1 calc R . . C23B C 0.22470(10) -0.03591(10) 0.06266(9) 0.0183(2) Uani 1 1 d . . . C24B C 0.31249(11) -0.03658(11) 0.10819(10) 0.0201(3) Uani 1 1 d . . . H24B H 0.3675 -0.0574 0.0813 0.024 Uiso 1 1 calc R . . C25B C 0.32141(12) -0.00810(11) 0.19037(10) 0.0213(3) Uani 1 1 d . . . C26B C 0.41293(12) -0.01478(12) 0.24044(11) 0.0251(3) Uani 1 1 d . . . C27B C 0.49232(13) -0.05459(15) 0.18830(12) 0.0324(4) Uani 1 1 d . . . H27X H 0.4608 -0.1183 0.1521 0.049 Uiso 1 1 calc R . . H27Y H 0.5499 -0.0571 0.2222 0.049 Uiso 1 1 calc R . . H27Z H 0.5171 -0.0139 0.1572 0.049 Uiso 1 1 calc R . . C28B C 0.37486(15) -0.08056(17) 0.28758(14) 0.0373(4) Uani 1 1 d . . . H28X H 0.3247 -0.0557 0.3220 0.056 Uiso 1 1 calc R . . H28Y H 0.4328 -0.0844 0.3204 0.056 Uiso 1 1 calc R . . H28Z H 0.3427 -0.1436 0.2505 0.056 Uiso 1 1 calc R . . C29B C 0.46492(17) 0.08293(15) 0.29855(14) 0.0402(5) Uani 1 1 d . . . H29X H 0.4944 0.1236 0.2686 0.060 Uiso 1 1 calc R . . H29Y H 0.5193 0.0772 0.3335 0.060 Uiso 1 1 calc R . . H29Z H 0.4143 0.1105 0.3308 0.060 Uiso 1 1 calc R . . C30B C 0.24004(13) 0.02634(12) 0.22796(10) 0.0245(3) Uani 1 1 d . . . H30B H 0.2449 0.0489 0.2845 0.029 Uiso 1 1 calc R . . C31B C 0.15305(12) 0.02833(11) 0.18487(10) 0.0232(3) Uani 1 1 d . . . H31B H 0.1002 0.0528 0.2125 0.028 Uiso 1 1 calc R . . C32B C 0.14156(11) -0.00504(10) 0.10137(9) 0.0179(2) Uani 1 1 d . . . N1B N 0.01818(9) 0.19743(8) 0.16023(8) 0.0178(2) Uani 1 1 d . C . N2B N 0.14647(9) -0.08689(9) -0.07270(8) 0.0179(2) Uani 1 1 d . . . O1B O 0.11534(10) 0.18611(8) 0.01974(8) 0.0266(2) Uani 1 1 d . C . O2B O 0.05423(8) -0.00803(7) 0.06211(7) 0.01826(19) Uani 1 1 d . . . Zn1B Zn 0.006976(12) 0.102371(11) 0.047406(10) 0.01574(4) Uani 1 1 d . . . C1N C 0.6512(2) 0.4870(2) 0.29839(16) 0.0475(6) Uani 1 1 d . . . C2N C 0.7234(2) 0.57520(18) 0.30419(17) 0.0508(6) Uani 1 1 d . . . H2N1 H 0.7286 0.6204 0.3582 0.076 Uiso 1 1 calc R . . H2N2 H 0.6990 0.6016 0.2657 0.076 Uiso 1 1 calc R . . H2N3 H 0.7908 0.5625 0.2926 0.076 Uiso 1 1 calc R . . N1N N 0.59557(19) 0.4180(2) 0.29449(17) 0.0602(6) Uani 1 1 d . . . C1T C 0.4882(2) 0.1901(2) 0.1254(2) 0.0531(7) Uani 1 1 d . . . C2T C 0.40735(18) 0.23194(17) 0.16287(16) 0.0426(5) Uani 1 1 d . . . H2T1 H 0.3500 0.1821 0.1650 0.064 Uiso 1 1 calc R . . H2T2 H 0.3840 0.2678 0.1319 0.064 Uiso 1 1 calc R . . H2T3 H 0.4334 0.2743 0.2171 0.064 Uiso 1 1 calc R . . N1T N 0.5504(2) 0.1554(2) 0.0956(2) 0.0766(8) Uani 1 1 d U . . C1L C 0.0980(3) 0.7822(2) 0.1599(2) 0.0662(8) Uani 1 1 d U . . H1L1 H 0.0412 0.7892 0.1280 0.099 Uiso 1 1 calc R . . H1L2 H 0.0989 0.7152 0.1455 0.099 Uiso 1 1 calc R . . H1L3 H 0.1627 0.8170 0.1497 0.099 Uiso 1 1 calc R . . C2L C 0.0849(3) 0.8190(3) 0.2435(2) 0.0661(8) Uani 1 1 d U . . N1L N 0.0785(3) 0.8561(3) 0.3128(3) 0.0993(11) Uani 1 1 d U . . 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 C1A 0.0148(5) 0.0217(6) 0.0219(7) 0.0100(5) 0.0037(5) 0.0069(4) C2A 0.0134(5) 0.0206(5) 0.0239(7) 0.0085(5) 0.0034(5) 0.0060(4) C3A 0.0140(5) 0.0219(6) 0.0283(8) 0.0102(5) 0.0056(5) 0.0053(4) C4A 0.0252(7) 0.0371(8) 0.0260(9) 0.0132(7) 0.0081(6) 0.0050(6) C5A 0.0245(7) 0.0215(6) 0.0400(10) 0.0110(6) 0.0070(6) 0.0046(5) C6A 0.0157(6) 0.0325(8) 0.0477(11) 0.0193(8) 0.0095(6) 0.0081(5) C7A 0.0156(6) 0.0263(6) 0.0309(8) 0.0127(6) 0.0045(5) 0.0097(5) C8A 0.0205(6) 0.0327(7) 0.0376(10) 0.0213(7) 0.0072(6) 0.0136(6) C9A 0.0333(9) 0.0549(12) 0.0629(15) 0.0409(12) 0.0133(9) 0.0285(9) C10A 0.0456(8) 0.0613(9) 0.0705(11) 0.0421(9) 0.0123(8) 0.0302(7) C11A 0.0456(8) 0.0613(9) 0.0705(11) 0.0421(9) 0.0123(8) 0.0302(7) C12A 0.0456(8) 0.0613(9) 0.0705(11) 0.0421(9) 0.0123(8) 0.0302(7) C10C 0.0456(8) 0.0613(9) 0.0705(11) 0.0421(9) 0.0123(8) 0.0302(7) C11C 0.0456(8) 0.0613(9) 0.0705(11) 0.0421(9) 0.0123(8) 0.0302(7) C12C 0.0456(8) 0.0613(9) 0.0705(11) 0.0421(9) 0.0123(8) 0.0302(7) C13A 0.0203(6) 0.0340(8) 0.0382(10) 0.0246(7) 0.0087(6) 0.0128(6) C14A 0.0158(5) 0.0279(6) 0.0281(8) 0.0172(6) 0.0066(5) 0.0099(5) C15A 0.0174(6) 0.0278(6) 0.0277(8) 0.0178(6) 0.0071(5) 0.0095(5) C16A 0.0141(5) 0.0198(5) 0.0202(7) 0.0097(5) 0.0049(4) 0.0062(4) C17A 0.0178(6) 0.0235(6) 0.0252(7) 0.0135(5) 0.0069(5) 0.0076(5) C18A 0.0186(6) 0.0273(7) 0.0319(9) 0.0165(6) 0.0101(5) 0.0068(5) C19A 0.0149(6) 0.0289(7) 0.0329(9) 0.0153(6) 0.0064(5) 0.0060(5) C20A 0.0148(5) 0.0262(6) 0.0278(8) 0.0135(6) 0.0044(5) 0.0075(5) C21A 0.0141(5) 0.0201(5) 0.0211(7) 0.0099(5) 0.0046(4) 0.0059(4) C22A 0.0180(6) 0.0234(6) 0.0229(7) 0.0122(5) 0.0021(5) 0.0062(5) C23A 0.0209(6) 0.0224(6) 0.0208(7) 0.0116(5) 0.0028(5) 0.0065(5) C24A 0.0285(7) 0.0252(6) 0.0206(7) 0.0110(6) 0.0006(6) 0.0069(5) C25A 0.0361(8) 0.0271(7) 0.0205(8) 0.0122(6) 0.0036(6) 0.0089(6) C26A 0.0591(13) 0.0326(8) 0.0211(9) 0.0134(7) 0.0003(8) 0.0121(8) C27A 0.051(2) 0.0376(18) 0.032(2) 0.0220(17) -0.0038(17) 0.0102(17) C28A 0.056(3) 0.0392(19) 0.028(2) 0.0156(16) -0.0108(18) 0.0025(18) C29A 0.066(3) 0.070(3) 0.0178(19) 0.0123(19) 0.0081(18) 0.035(3) C27C 0.072(3) 0.0349(19) 0.024(2) 0.0091(15) 0.0015(19) 0.012(2) C28C 0.074(3) 0.065(3) 0.039(2) 0.022(2) -0.004(2) 0.033(2) C29C 0.084(3) 0.053(2) 0.030(2) 0.023(2) 0.004(2) 0.001(2) C30A 0.0364(9) 0.0293(7) 0.0245(8) 0.0158(6) 0.0086(6) 0.0075(6) C31A 0.0276(7) 0.0259(7) 0.0234(8) 0.0133(6) 0.0066(6) 0.0045(5) C35A 0.0212(6) 0.0219(6) 0.0198(7) 0.0106(5) 0.0050(5) 0.0082(5) N1A 0.0141(5) 0.0219(5) 0.0205(6) 0.0106(4) 0.0043(4) 0.0068(4) N2A 0.0149(5) 0.0216(5) 0.0219(6) 0.0121(5) 0.0044(4) 0.0064(4) O1A 0.0159(4) 0.0287(5) 0.0299(6) 0.0186(5) 0.0074(4) 0.0101(4) O2A 0.0205(5) 0.0216(4) 0.0203(5) 0.0107(4) 0.0028(4) 0.0057(4) Zn1A 0.01329(7) 0.01933(7) 0.02146(9) 0.01090(6) 0.00305(5) 0.00545(5) C1B 0.0180(6) 0.0207(6) 0.0245(8) 0.0079(5) 0.0057(5) 0.0038(5) C2B 0.0200(6) 0.0235(6) 0.0277(8) 0.0112(6) 0.0074(5) 0.0046(5) C3B 0.0323(8) 0.0321(8) 0.0304(10) 0.0120(7) 0.0137(7) 0.0016(7) C4B 0.0498(12) 0.0316(9) 0.0479(14) 0.0096(9) 0.0302(10) 0.0122(8) C5B 0.0476(12) 0.0414(10) 0.0419(13) 0.0138(9) 0.0253(10) -0.0011(9) C6B 0.0503(13) 0.0593(14) 0.0317(12) 0.0196(11) 0.0039(10) -0.0036(11) C7B 0.0195(6) 0.0237(6) 0.0361(9) 0.0128(6) 0.0070(6) 0.0034(5) C8B 0.0196(6) 0.0219(6) 0.0350(9) 0.0064(6) 0.0046(6) 0.0011(5) C9B 0.0299(9) 0.0264(8) 0.0496(13) 0.0056(8) 0.0009(8) -0.0040(6) C10B 0.0266(12) 0.0405(15) 0.062(2) 0.0222(16) -0.0105(13) -0.0101(11) C11B 0.0569(18) 0.0380(14) 0.0421(18) -0.0009(12) 0.0165(14) -0.0129(13) C12B 0.0463(16) 0.0216(10) 0.0498(19) 0.0104(11) -0.0010(14) 0.0027(10) C10D 0.061(4) 0.034(3) 0.066(4) 0.019(3) -0.006(3) 0.005(3) C11D 0.069(4) 0.066(4) 0.066(4) 0.023(3) 0.014(3) 0.000(3) C12D 0.036(3) 0.025(3) 0.057(5) 0.001(3) 0.013(3) -0.012(2) C13B 0.0203(6) 0.0222(6) 0.0293(9) 0.0028(6) 0.0040(6) 0.0009(5) C14B 0.0168(6) 0.0192(6) 0.0245(8) 0.0049(5) 0.0050(5) 0.0020(4) C15B 0.0174(6) 0.0200(6) 0.0211(7) 0.0036(5) 0.0034(5) 0.0036(5) C16B 0.0157(5) 0.0174(5) 0.0172(6) 0.0047(5) 0.0033(4) 0.0042(4) C17B 0.0216(6) 0.0242(6) 0.0172(7) 0.0042(5) 0.0028(5) 0.0050(5) C18B 0.0260(7) 0.0281(7) 0.0169(7) 0.0065(6) 0.0056(5) 0.0055(5) C19B 0.0239(7) 0.0277(7) 0.0214(8) 0.0094(6) 0.0085(5) 0.0044(5) C20B 0.0173(6) 0.0268(6) 0.0206(7) 0.0081(5) 0.0049(5) 0.0024(5) C21B 0.0153(5) 0.0206(5) 0.0170(6) 0.0064(5) 0.0034(4) 0.0047(4) C22B 0.0146(5) 0.0244(6) 0.0193(7) 0.0078(5) 0.0026(4) 0.0050(4) C23B 0.0150(5) 0.0232(6) 0.0171(6) 0.0069(5) 0.0013(4) 0.0051(4) C24B 0.0157(5) 0.0244(6) 0.0207(7) 0.0077(5) 0.0004(5) 0.0057(5) C25B 0.0200(6) 0.0246(6) 0.0199(7) 0.0075(5) -0.0018(5) 0.0072(5) C26B 0.0207(6) 0.0323(7) 0.0240(8) 0.0105(6) -0.0029(5) 0.0091(6) C27B 0.0213(7) 0.0480(10) 0.0311(10) 0.0138(8) 0.0000(6) 0.0146(7) C28B 0.0287(8) 0.0559(12) 0.0417(12) 0.0316(10) 0.0040(7) 0.0168(8) C29B 0.0357(10) 0.0397(10) 0.0360(11) 0.0026(8) -0.0154(8) 0.0079(8) C30B 0.0261(7) 0.0303(7) 0.0166(7) 0.0039(6) -0.0016(5) 0.0125(6) C31B 0.0230(6) 0.0295(7) 0.0181(7) 0.0047(5) 0.0007(5) 0.0134(5) C32B 0.0168(5) 0.0205(5) 0.0170(6) 0.0056(5) 0.0005(4) 0.0066(4) N1B 0.0148(5) 0.0195(5) 0.0182(6) 0.0054(4) 0.0034(4) 0.0034(4) N2B 0.0146(5) 0.0220(5) 0.0166(6) 0.0061(4) 0.0023(4) 0.0038(4) O1B 0.0274(5) 0.0224(5) 0.0235(6) 0.0029(4) 0.0098(4) -0.0019(4) O2B 0.0156(4) 0.0207(4) 0.0182(5) 0.0044(4) -0.0002(3) 0.0074(3) Zn1B 0.01301(7) 0.01757(7) 0.01597(8) 0.00436(6) 0.00243(5) 0.00393(5) C1N 0.0419(12) 0.0639(15) 0.0389(13) 0.0106(11) 0.0035(9) 0.0275(11) C2N 0.0562(14) 0.0505(13) 0.0428(14) 0.0042(10) -0.0010(11) 0.0251(11) N1N 0.0426(11) 0.0794(17) 0.0580(16) 0.0183(13) 0.0069(10) 0.0194(12) C1T 0.0472(13) 0.0642(15) 0.0694(19) 0.0388(14) 0.0248(12) 0.0304(12) C2T 0.0392(10) 0.0486(11) 0.0500(14) 0.0212(10) 0.0133(9) 0.0229(9) N1T 0.0685(14) 0.0863(15) 0.0918(17) 0.0369(13) 0.0329(12) 0.0392(12) C1L 0.0571(13) 0.0590(13) 0.0799(17) 0.0207(12) 0.0091(12) 0.0115(11) C2L 0.0563(13) 0.0823(16) 0.0776(17) 0.0488(14) 0.0105(12) 0.0187(12) N1L 0.0968(18) 0.133(2) 0.0937(18) 0.0694(16) 0.0189(14) 0.0295(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 C1A O1A 1.3023(17) . ? C1A C14A 1.430(2) . ? C1A C2A 1.4398(19) . ? C2A C7A 1.386(2) . ? C2A C3A 1.536(2) . ? C3A C6A 1.534(2) . ? C3A C4A 1.537(2) . ? C3A C5A 1.542(2) . ? C7A C8A 1.411(2) . ? C8A C13A 1.378(2) . ? C8A C9A 1.530(2) . ? C9A C12A 1.477(4) . ? C9A C11C 1.515(5) . ? C9A C11A 1.533(4) . ? C9A C12C 1.567(5) . ? C9A C10A 1.569(5) . ? C9A C10C 1.579(15) . ? C13A C14A 1.415(2) . ? C14A C15A 1.441(2) . ? C15A N1A 1.2936(17) . ? C16A C17A 1.391(2) . ? C16A N1A 1.4103(18) . ? C16A C21A 1.4135(19) . ? C17A C18A 1.390(2) . ? C18A C19A 1.389(2) . ? C19A C20A 1.388(2) . ? C20A C21A 1.3930(19) . ? C21A N2A 1.4106(19) . ? C22A N2A 1.2920(19) . ? C22A C23A 1.448(2) . ? C23A C24A 1.408(2) . ? C23A C35A 1.420(2) . ? C24A C25A 1.389(2) . ? C25A C30A 1.404(3) . ? C25A C26A 1.525(3) . ? C26A C28A 1.497(4) . ? C26A C29C 1.498(4) . ? C26A C27A 1.500(4) . ? C26A C27C 1.514(5) . ? C26A C29A 1.592(4) . ? C26A C28C 1.597(4) . ? C30A C31A 1.381(2) . ? C31A C35A 1.406(2) . ? C35A O2A 1.3263(19) . ? N1A Zn1A 2.0499(12) . ? N2A Zn1A 2.0735(12) . ? O1A Zn1A 1.9246(11) . ? O2A Zn1A 1.9952(12) 2_566 ? O2A Zn1A 2.0412(11) . ? Zn1A O2A 1.9953(12) 2_566 ? Zn1A Zn1A 3.0292(3) 2_566 ? C1B O1B 1.3039(18) . ? C1B C14B 1.423(2) . ? C1B C2B 1.440(2) . ? C2B C7B 1.381(2) . ? C2B C3B 1.534(3) . ? C3B C5B 1.534(3) . ? C3B C4B 1.537(3) . ? C3B C6B 1.539(3) . ? C7B C8B 1.408(3) . ? C8B C13B 1.373(2) . ? C8B C9B 1.535(2) . ? C9B C11B 1.439(4) . ? C9B C11D 1.505(5) . ? C9B C10D 1.531(10) . ? C9B C10B 1.542(4) . ? C9B C12D 1.585(5) . ? C9B C12B 1.608(4) . ? C13B C14B 1.416(2) . ? C14B C15B 1.442(2) . ? C15B N1B 1.2943(18) . ? C16B C17B 1.387(2) . ? C16B C21B 1.4078(19) . ? C16B N1B 1.4096(19) . ? C17B C18B 1.390(2) . ? C18B C19B 1.390(2) . ? C19B C20B 1.386(2) . ? C20B C21B 1.391(2) . ? C21B N2B 1.411(2) 2 ? C22B N2B 1.2882(18) . ? C22B C23B 1.448(2) . ? C23B C24B 1.4118(19) . ? C23B C32B 1.417(2) . ? C24B C25B 1.381(2) . ? C25B C30B 1.409(2) . ? C25B C26B 1.534(2) . ? C26B C29B 1.530(3) . ? C26B C27B 1.532(3) . ? C26B C28B 1.534(3) . ? C30B C31B 1.387(2) . ? C31B C32B 1.402(2) . ? C32B O2B 1.3299(16) . ? N1B Zn1B 2.0520(13) . ? N2B C21B 1.411(2) 2 ? N2B Zn1B 2.1071(12) 2 ? O1B Zn1B 1.9255(12) . ? O2B Zn1B 2.0166(10) . ? O2B Zn1B 2.0442(11) 2 ? Zn1B O2B 2.0442(11) 2 ? Zn1B N2B 2.1071(12) 2 ? Zn1B Zn1B 3.0215(3) 2 ? C1N N1N 1.147(4) . ? C1N C2N 1.467(4) . ? C1T N1T 1.139(4) . ? C1T C2T 1.449(3) . ? C1L C2L 1.445(5) . ? C2L N1L 1.198(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1A C1A C14A 123.61(13) . . ? O1A C1A C2A 118.31(13) . . ? C14A C1A C2A 118.03(12) . . ? C7A C2A C1A 118.08(14) . . ? C7A C2A C3A 122.17(13) . . ? C1A C2A C3A 119.75(12) . . ? C6A C3A C2A 111.95(13) . . ? C6A C3A C4A 107.52(15) . . ? C2A C3A C4A 109.72(12) . . ? C6A C3A C5A 106.79(13) . . ? C2A C3A C5A 111.15(14) . . ? C4A C3A C5A 109.59(14) . . ? C2A C7A C8A 124.50(14) . . ? C13A C8A C7A 117.20(14) . . ? C13A C8A C9A 122.21(16) . . ? C7A C8A C9A 120.58(15) . . ? C12A C9A C11C 123.4(5) . . ? C12A C9A C8A 112.97(18) . . ? C11C C9A C8A 120.8(5) . . ? C12A C9A C11A 111.0(2) . . ? C11C C9A C11A 36.0(6) . . ? C8A C9A C11A 108.9(2) . . ? C12A C9A C12C 37.6(6) . . ? C11C C9A C12C 105.4(8) . . ? C8A C9A C12C 108.4(4) . . ? C11A C9A C12C 78.6(6) . . ? C12A C9A C10A 110.2(3) . . ? C11C C9A C10A 70.3(7) . . ? C8A C9A C10A 107.19(19) . . ? C11A C9A C10A 106.3(2) . . ? C12C C9A C10A 140.0(5) . . ? C12A C9A C10C 53.9(6) . . ? C11C C9A C10C 116.1(7) . . ? C8A C9A C10C 110.4(4) . . ? C11A C9A C10C 140.7(4) . . ? C12C C9A C10C 91.1(8) . . ? C10A C9A C10C 59.5(6) . . ? C8A C13A C14A 121.58(15) . . ? C13A C14A C1A 120.58(13) . . ? C13A C14A C15A 115.06(14) . . ? C1A C14A C15A 124.11(12) . . ? N1A C15A C14A 124.67(13) . . ? C17A C16A N1A 125.55(12) . . ? C17A C16A C21A 120.10(12) . . ? N1A C16A C21A 114.34(12) . . ? C18A C17A C16A 119.60(14) . . ? C19A C18A C17A 120.26(14) . . ? C20A C19A C18A 120.82(14) . . ? C19A C20A C21A 119.54(14) . . ? C20A C21A N2A 124.08(13) . . ? C20A C21A C16A 119.67(13) . . ? N2A C21A C16A 116.21(12) . . ? N2A C22A C23A 124.64(13) . . ? C24A C23A C35A 119.26(14) . . ? C24A C23A C22A 117.06(14) . . ? C35A C23A C22A 123.68(14) . . ? C25A C24A C23A 122.95(15) . . ? C24A C25A C30A 116.56(16) . . ? C24A C25A C26A 122.22(16) . . ? C30A C25A C26A 121.20(16) . . ? C28A C26A C29C 129.5(3) . . ? C28A C26A C27A 112.9(3) . . ? C29C C26A C27A 49.6(3) . . ? C28A C26A C27C 44.5(3) . . ? C29C C26A C27C 113.4(3) . . ? C27A C26A C27C 140.4(3) . . ? C28A C26A C25A 114.4(2) . . ? C29C C26A C25A 116.0(3) . . ? C27A C26A C25A 109.8(2) . . ? C27C C26A C25A 109.6(2) . . ? C28A C26A C29A 106.3(3) . . ? C29C C26A C29A 56.7(3) . . ? C27A C26A C29A 105.9(3) . . ? C27C C26A C29A 65.5(3) . . ? C25A C26A C29A 106.9(2) . . ? C28A C26A C28C 59.1(3) . . ? C29C C26A C28C 106.3(4) . . ? C27A C26A C28C 61.2(3) . . ? C27C C26A C28C 103.1(3) . . ? C25A C26A C28C 107.3(2) . . ? C29A C26A C28C 145.8(3) . . ? C31A C30A C25A 122.19(16) . . ? C30A C31A C35A 121.32(15) . . ? O2A C35A C31A 119.73(14) . . ? O2A C35A C23A 122.60(13) . . ? C31A C35A C23A 117.66(14) . . ? C15A N1A C16A 122.86(12) . . ? C15A N1A Zn1A 124.12(10) . . ? C16A N1A Zn1A 112.60(9) . . ? C22A N2A C21A 122.04(13) . . ? C22A N2A Zn1A 124.18(10) . . ? C21A N2A Zn1A 111.36(9) . . ? C1A O1A Zn1A 126.77(11) . . ? C35A O2A Zn1A 132.15(9) . 2_566 ? C35A O2A Zn1A 124.26(9) . . ? Zn1A O2A Zn1A 97.25(5) 2_566 . ? O1A Zn1A O2A 113.01(5) . 2_566 ? O1A Zn1A O2A 97.75(5) . . ? O2A Zn1A O2A 82.75(5) 2_566 . ? O1A Zn1A N1A 90.97(5) . . ? O2A Zn1A N1A 106.38(5) 2_566 . ? O2A Zn1A N1A 163.84(5) . . ? O1A Zn1A N2A 133.34(5) . . ? O2A Zn1A N2A 113.56(5) 2_566 . ? O2A Zn1A N2A 85.29(5) . . ? N1A Zn1A N2A 78.85(5) . . ? O1A Zn1A Zn1A 110.38(3) . 2_566 ? O2A Zn1A Zn1A 41.95(3) 2_566 2_566 ? O2A Zn1A Zn1A 40.80(3) . 2_566 ? N1A Zn1A Zn1A 146.40(4) . 2_566 ? N2A Zn1A Zn1A 102.00(3) . 2_566 ? O1B C1B C14B 123.64(14) . . ? O1B C1B C2B 118.76(15) . . ? C14B C1B C2B 117.59(14) . . ? C7B C2B C1B 118.50(16) . . ? C7B C2B C3B 121.45(15) . . ? C1B C2B C3B 120.05(14) . . ? C2B C3B C5B 112.33(16) . . ? C2B C3B C4B 110.42(16) . . ? C5B C3B C4B 106.96(18) . . ? C2B C3B C6B 110.36(18) . . ? C5B C3B C6B 107.16(19) . . ? C4B C3B C6B 109.49(19) . . ? C2B C7B C8B 124.56(15) . . ? C13B C8B C7B 116.67(15) . . ? C13B C8B C9B 122.37(18) . . ? C7B C8B C9B 120.96(16) . . ? C11B C9B C11D 124.1(6) . . ? C11B C9B C10D 56.0(5) . . ? C11D C9B C10D 122.3(7) . . ? C11B C9B C8B 115.0(2) . . ? C11D C9B C8B 117.0(5) . . ? C10D C9B C8B 106.8(4) . . ? C11B C9B C10B 114.0(3) . . ? C11D C9B C10B 29.1(5) . . ? C10D C9B C10B 144.0(4) . . ? C8B C9B C10B 108.1(2) . . ? C11B C9B C12D 42.5(3) . . ? C11D C9B C12D 101.9(6) . . ? C10D C9B C12D 98.4(5) . . ? C8B C9B C12D 107.4(3) . . ? C10B C9B C12D 78.8(3) . . ? C11B C9B C12B 107.4(3) . . ? C11D C9B C12B 74.3(6) . . ? C10D C9B C12B 57.2(4) . . ? C8B C9B C12B 108.05(19) . . ? C10B C9B C12B 103.4(2) . . ? C12D C9B C12B 141.6(3) . . ? C8B C13B C14B 122.11(17) . . ? C13B C14B C1B 120.48(15) . . ? C13B C14B C15B 115.07(15) . . ? C1B C14B C15B 124.36(13) . . ? N1B C15B C14B 125.07(15) . . ? C17B C16B C21B 120.24(14) . . ? C17B C16B N1B 125.24(13) . . ? C21B C16B N1B 114.40(13) . . ? C16B C17B C18B 119.10(14) . . ? C19B C18B C17B 120.81(16) . . ? C20B C19B C18B 120.21(15) . . ? C19B C20B C21B 119.58(14) . . ? C20B C21B C16B 119.83(14) . . ? C20B C21B N2B 124.71(13) . 2 ? C16B C21B N2B 115.31(13) . 2 ? N2B C22B C23B 123.58(14) . . ? C24B C23B C32B 119.87(14) . . ? C24B C23B C22B 116.32(13) . . ? C32B C23B C22B 123.82(12) . . ? C25B C24B C23B 122.52(14) . . ? C24B C25B C30B 116.81(13) . . ? C24B C25B C26B 123.18(15) . . ? C30B C25B C26B 119.99(15) . . ? C29B C26B C27B 108.51(16) . . ? C29B C26B C28B 109.26(17) . . ? C27B C26B C28B 108.21(15) . . ? C29B C26B C25B 110.05(14) . . ? C27B C26B C25B 111.77(14) . . ? C28B C26B C25B 108.99(14) . . ? C31B C30B C25B 121.95(15) . . ? C30B C31B C32B 121.31(15) . . ? O2B C32B C31B 119.60(13) . . ? O2B C32B C23B 122.98(13) . . ? C31B C32B C23B 117.41(12) . . ? C15B N1B C16B 121.99(13) . . ? C15B N1B Zn1B 125.13(11) . . ? C16B N1B Zn1B 111.55(9) . . ? C22B N2B C21B 122.22(13) . 2 ? C22B N2B Zn1B 126.86(11) . 2 ? C21B N2B Zn1B 110.44(9) 2 2 ? C1B O1B Zn1B 130.28(11) . . ? C32B O2B Zn1B 126.68(9) . . ? C32B O2B Zn1B 125.76(9) . 2 ? Zn1B O2B Zn1B 96.15(4) . 2 ? O1B Zn1B O2B 111.61(5) . . ? O1B Zn1B O2B 101.61(5) . 2 ? O2B Zn1B O2B 83.85(4) . 2 ? O1B Zn1B N1B 90.92(5) . . ? O2B Zn1B N1B 104.99(5) . . ? O2B Zn1B N1B 160.94(5) 2 . ? O1B Zn1B N2B 141.96(5) . 2 ? O2B Zn1B N2B 106.37(5) . 2 ? O2B Zn1B N2B 84.12(5) 2 2 ? N1B Zn1B N2B 77.22(5) . 2 ? O1B Zn1B Zn1B 112.45(4) . 2 ? O2B Zn1B Zn1B 42.27(3) . 2 ? O2B Zn1B Zn1B 41.57(3) 2 2 ? N1B Zn1B Zn1B 144.30(4) . 2 ? N2B Zn1B Zn1B 96.82(3) 2 2 ? N1N C1N C2N 179.2(3) . . ? N1T C1T C2T 178.7(3) . . ? N1L C2L C1L 174.9(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 O1A C1A C2A C7A -177.55(15) . . . . ? C14A C1A C2A C7A 0.1(2) . . . . ? O1A C1A C2A C3A 2.2(2) . . . . ? C14A C1A C2A C3A 179.90(14) . . . . ? C7A C2A C3A C6A -3.1(2) . . . . ? C1A C2A C3A C6A 177.10(15) . . . . ? C7A C2A C3A C4A 116.18(17) . . . . ? C1A C2A C3A C4A -63.60(18) . . . . ? C7A C2A C3A C5A -122.44(17) . . . . ? C1A C2A C3A C5A 57.77(19) . . . . ? C1A C2A C7A C8A 1.2(3) . . . . ? C3A C2A C7A C8A -178.60(16) . . . . ? C2A C7A C8A C13A -1.4(3) . . . . ? C2A C7A C8A C9A 179.38(19) . . . . ? C13A C8A C9A C12A 5.0(4) . . . . ? C7A C8A C9A C12A -175.8(2) . . . . ? C13A C8A C9A C11C 166.6(8) . . . . ? C7A C8A C9A C11C -14.3(8) . . . . ? C13A C8A C9A C11A 128.8(2) . . . . ? C7A C8A C9A C11A -52.0(3) . . . . ? C13A C8A C9A C12C 44.9(7) . . . . ? C7A C8A C9A C12C -135.9(7) . . . . ? C13A C8A C9A C10A -116.5(2) . . . . ? C7A C8A C9A C10A 62.6(3) . . . . ? C13A C8A C9A C10C -53.4(6) . . . . ? C7A C8A C9A C10C 125.8(6) . . . . ? C7A C8A C13A C14A 0.3(3) . . . . ? C9A C8A C13A C14A 179.5(2) . . . . ? C8A C13A C14A C1A 0.9(3) . . . . ? C8A C13A C14A C15A 175.44(18) . . . . ? O1A C1A C14A C13A 176.40(17) . . . . ? C2A C1A C14A C13A -1.1(2) . . . . ? O1A C1A C14A C15A 2.4(3) . . . . ? C2A C1A C14A C15A -175.12(16) . . . . ? C13A C14A C15A N1A 173.05(17) . . . . ? C1A C14A C15A N1A -12.7(3) . . . . ? N1A C16A C17A C18A -177.93(15) . . . . ? C21A C16A C17A C18A 1.0(2) . . . . ? C16A C17A C18A C19A -0.9(3) . . . . ? C17A C18A C19A C20A -0.1(3) . . . . ? C18A C19A C20A C21A 1.0(3) . . . . ? C19A C20A C21A N2A -178.71(15) . . . . ? C19A C20A C21A C16A -0.8(2) . . . . ? C17A C16A C21A C20A -0.1(2) . . . . ? N1A C16A C21A C20A 178.91(14) . . . . ? C17A C16A C21A N2A 177.89(14) . . . . ? N1A C16A C21A N2A -3.06(19) . . . . ? N2A C22A C23A C24A 170.87(15) . . . . ? N2A C22A C23A C35A -9.5(2) . . . . ? C35A C23A C24A C25A -1.0(2) . . . . ? C22A C23A C24A C25A 178.62(15) . . . . ? C23A C24A C25A C30A -1.1(3) . . . . ? C23A C24A C25A C26A -179.67(16) . . . . ? C24A C25A C26A C28A -0.4(3) . . . . ? C30A C25A C26A C28A -178.9(3) . . . . ? C24A C25A C26A C29C -178.4(3) . . . . ? C30A C25A C26A C29C 3.0(4) . . . . ? C24A C25A C26A C27A 127.8(3) . . . . ? C30A C25A C26A C27A -50.8(3) . . . . ? C24A C25A C26A C27C -48.4(3) . . . . ? C30A C25A C26A C27C 133.1(3) . . . . ? C24A C25A C26A C29A -117.8(3) . . . . ? C30A C25A C26A C29A 63.6(3) . . . . ? C24A C25A C26A C28C 62.9(3) . . . . ? C30A C25A C26A C28C -115.6(3) . . . . ? C24A C25A C30A C31A 1.5(3) . . . . ? C26A C25A C30A C31A -179.84(17) . . . . ? C25A C30A C31A C35A 0.1(3) . . . . ? C30A C31A C35A O2A 176.65(15) . . . . ? C30A C31A C35A C23A -2.2(2) . . . . ? C24A C23A C35A O2A -176.21(14) . . . . ? C22A C23A C35A O2A 4.2(2) . . . . ? C24A C23A C35A C31A 2.7(2) . . . . ? C22A C23A C35A C31A -176.98(14) . . . . ? C14A C15A N1A C16A 171.04(16) . . . . ? C14A C15A N1A Zn1A -1.0(2) . . . . ? C17A C16A N1A C15A 27.1(2) . . . . ? C21A C16A N1A C15A -151.92(15) . . . . ? C17A C16A N1A Zn1A -160.07(13) . . . . ? C21A C16A N1A Zn1A 20.94(16) . . . . ? C23A C22A N2A C21A -179.20(14) . . . . ? C23A C22A N2A Zn1A -18.4(2) . . . . ? C20A C21A N2A C22A -35.0(2) . . . . ? C16A C21A N2A C22A 147.07(15) . . . . ? C20A C21A N2A Zn1A 162.01(13) . . . . ? C16A C21A N2A Zn1A -15.93(16) . . . . ? C14A C1A O1A Zn1A 21.4(2) . . . . ? C2A C1A O1A Zn1A -161.11(11) . . . . ? C31A C35A O2A Zn1A 64.63(19) . . . 2_566 ? C23A C35A O2A Zn1A -116.53(14) . . . 2_566 ? C31A C35A O2A Zn1A -150.01(12) . . . . ? C23A C35A O2A Zn1A 28.83(19) . . . . ? C1A O1A Zn1A O2A 82.15(13) . . . 2_566 ? C1A O1A Zn1A O2A 167.52(13) . . . . ? C1A O1A Zn1A N1A -26.13(13) . . . . ? C1A O1A Zn1A N2A -101.65(14) . . . . ? C1A O1A Zn1A Zn1A 127.38(12) . . . 2_566 ? C35A O2A Zn1A O1A 92.78(12) . . . . ? Zn1A O2A Zn1A O1A -112.35(5) 2_566 . . . ? C35A O2A Zn1A O2A -154.86(14) . . . 2_566 ? Zn1A O2A Zn1A O2A 0.0 2_566 . . 2_566 ? C35A O2A Zn1A N1A -29.3(2) . . . . ? Zn1A O2A Zn1A N1A 125.60(17) 2_566 . . . ? C35A O2A Zn1A N2A -40.36(12) . . . . ? Zn1A O2A Zn1A N2A 114.51(5) 2_566 . . . ? C35A O2A Zn1A Zn1A -154.86(14) . . . 2_566 ? C15A N1A Zn1A O1A 15.89(14) . . . . ? C16A N1A Zn1A O1A -156.87(11) . . . . ? C15A N1A Zn1A O2A -98.47(13) . . . 2_566 ? C16A N1A Zn1A O2A 88.77(11) . . . 2_566 ? C15A N1A Zn1A O2A 138.75(17) . . . . ? C16A N1A Zn1A O2A -34.0(2) . . . . ? C15A N1A Zn1A N2A 150.02(14) . . . . ? C16A N1A Zn1A N2A -22.74(10) . . . . ? C15A N1A Zn1A Zn1A -115.03(13) . . . 2_566 ? C16A N1A Zn1A Zn1A 72.21(12) . . . 2_566 ? C22A N2A Zn1A O1A -61.16(14) . . . . ? C21A N2A Zn1A O1A 101.41(11) . . . . ? C22A N2A Zn1A O2A 115.03(12) . . . 2_566 ? C21A N2A Zn1A O2A -82.41(10) . . . 2_566 ? C22A N2A Zn1A O2A 35.06(12) . . . . ? C21A N2A Zn1A O2A -162.38(10) . . . . ? C22A N2A Zn1A N1A -141.82(13) . . . . ? C21A N2A Zn1A N1A 20.75(10) . . . . ? C22A N2A Zn1A Zn1A 72.49(12) . . . 2_566 ? C21A N2A Zn1A Zn1A -124.95(9) . . . 2_566 ? O1B C1B C2B C7B 176.94(15) . . . . ? C14B C1B C2B C7B -2.3(2) . . . . ? O1B C1B C2B C3B -3.3(2) . . . . ? C14B C1B C2B C3B 177.42(15) . . . . ? C7B C2B C3B C5B 0.9(3) . . . . ? C1B C2B C3B C5B -178.80(18) . . . . ? C7B C2B C3B C4B 120.24(19) . . . . ? C1B C2B C3B C4B -59.5(2) . . . . ? C7B C2B C3B C6B -118.57(19) . . . . ? C1B C2B C3B C6B 61.7(2) . . . . ? C1B C2B C7B C8B 0.0(3) . . . . ? C3B C2B C7B C8B -179.73(17) . . . . ? C2B C7B C8B C13B 1.4(3) . . . . ? C2B C7B C8B C9B -179.08(17) . . . . ? C13B C8B C9B C11B -7.3(4) . . . . ? C7B C8B C9B C11B 173.2(3) . . . . ? C13B C8B C9B C11D 151.5(6) . . . . ? C7B C8B C9B C11D -28.0(7) . . . . ? C13B C8B C9B C10D -67.1(5) . . . . ? C7B C8B C9B C10D 113.5(5) . . . . ? C13B C8B C9B C10B 121.4(2) . . . . ? C7B C8B C9B C10B -58.1(3) . . . . ? C13B C8B C9B C12D 37.7(4) . . . . ? C7B C8B C9B C12D -141.7(4) . . . . ? C13B C8B C9B C12B -127.3(2) . . . . ? C7B C8B C9B C12B 53.2(3) . . . . ? C7B C8B C13B C14B -0.4(3) . . . . ? C9B C8B C13B C14B -179.95(17) . . . . ? C8B C13B C14B C1B -1.9(3) . . . . ? C8B C13B C14B C15B -178.75(16) . . . . ? O1B C1B C14B C13B -175.98(15) . . . . ? C2B C1B C14B C13B 3.3(2) . . . . ? O1B C1B C14B C15B 0.6(2) . . . . ? C2B C1B C14B C15B 179.79(14) . . . . ? C13B C14B C15B N1B -176.51(15) . . . . ? C1B C14B C15B N1B 6.8(3) . . . . ? C21B C16B C17B C18B -1.9(2) . . . . ? N1B C16B C17B C18B -177.66(14) . . . . ? C16B C17B C18B C19B -2.4(2) . . . . ? C17B C18B C19B C20B 3.9(3) . . . . ? C18B C19B C20B C21B -0.8(2) . . . . ? C19B C20B C21B C16B -3.5(2) . . . . ? C19B C20B C21B N2B 171.75(14) . . . 2 ? C17B C16B C21B C20B 4.9(2) . . . . ? N1B C16B C21B C20B -178.93(13) . . . . ? C17B C16B C21B N2B -170.76(13) . . . 2 ? N1B C16B C21B N2B 5.40(18) . . . 2 ? N2B C22B C23B C24B 167.67(14) . . . . ? N2B C22B C23B C32B -12.2(2) . . . . ? C32B C23B C24B C25B 0.1(2) . . . . ? C22B C23B C24B C25B -179.80(14) . . . . ? C23B C24B C25B C30B -2.9(2) . . . . ? C23B C24B C25B C26B 175.64(14) . . . . ? C24B C25B C26B C29B 121.72(19) . . . . ? C30B C25B C26B C29B -59.8(2) . . . . ? C24B C25B C26B C27B 1.1(2) . . . . ? C30B C25B C26B C27B 179.54(16) . . . . ? C24B C25B C26B C28B -118.47(19) . . . . ? C30B C25B C26B C28B 60.0(2) . . . . ? C24B C25B C30B C31B 2.5(2) . . . . ? C26B C25B C30B C31B -176.07(16) . . . . ? C25B C30B C31B C32B 0.7(3) . . . . ? C30B C31B C32B O2B 175.39(15) . . . . ? C30B C31B C32B C23B -3.5(2) . . . . ? C24B C23B C32B O2B -175.75(13) . . . . ? C22B C23B C32B O2B 4.1(2) . . . . ? C24B C23B C32B C31B 3.1(2) . . . . ? C22B C23B C32B C31B -177.03(14) . . . . ? C14B C15B N1B C16B -175.66(14) . . . . ? C14B C15B N1B Zn1B -10.0(2) . . . . ? C17B C16B N1B C15B -44.8(2) . . . . ? C21B C16B N1B C15B 139.28(14) . . . . ? C17B C16B N1B Zn1B 147.77(12) . . . . ? C21B C16B N1B Zn1B -28.16(14) . . . . ? C23B C22B N2B C21B 176.02(13) . . . 2 ? C23B C22B N2B Zn1B -12.7(2) . . . 2 ? C14B C1B O1B Zn1B -3.6(2) . . . . ? C2B C1B O1B Zn1B 177.19(11) . . . . ? C31B C32B O2B Zn1B 75.37(17) . . . . ? C23B C32B O2B Zn1B -105.81(15) . . . . ? C31B C32B O2B Zn1B -150.11(12) . . . 2 ? C23B C32B O2B Zn1B 28.71(19) . . . 2 ? C1B O1B Zn1B O2B -105.77(14) . . . . ? C1B O1B Zn1B O2B 166.31(14) . . . 2 ? C1B O1B Zn1B N1B 0.77(15) . . . . ? C1B O1B Zn1B N2B 70.99(18) . . . 2 ? C1B O1B Zn1B Zn1B -151.54(13) . . . 2 ? C32B O2B Zn1B O1B 44.34(14) . . . . ? Zn1B O2B Zn1B O1B -100.07(5) 2 . . . ? C32B O2B Zn1B O2B 144.41(15) . . . 2 ? Zn1B O2B Zn1B O2B 0.0 2 . . 2 ? C32B O2B Zn1B N1B -52.79(13) . . . . ? Zn1B O2B Zn1B N1B 162.80(5) 2 . . . ? C32B O2B Zn1B N2B -133.58(12) . . . 2 ? Zn1B O2B Zn1B N2B 82.00(5) 2 . . 2 ? C32B O2B Zn1B Zn1B 144.41(14) . . . 2 ? C15B N1B Zn1B O1B 5.86(13) . . . . ? C16B N1B Zn1B O1B 172.83(10) . . . . ? C15B N1B Zn1B O2B 118.54(12) . . . . ? C16B N1B Zn1B O2B -74.49(10) . . . . ? C15B N1B Zn1B O2B -125.65(15) . . . 2 ? C16B N1B Zn1B O2B 41.32(19) . . . 2 ? C15B N1B Zn1B N2B -137.66(13) . . . 2 ? C16B N1B Zn1B N2B 29.31(9) . . . 2 ? C15B N1B Zn1B Zn1B 138.47(10) . . . 2 ? C16B N1B Zn1B Zn1B -54.56(12) . . . 2 ? _diffrn_measured_fraction_theta_max 0.911 _diffrn_reflns_theta_full 34.94 _diffrn_measured_fraction_theta_full 0.911 _refine_diff_density_max 1.157 _refine_diff_density_min -0.859 _refine_diff_density_rms 0.124