# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 440/125 data_compound-1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C44 H28 N4 Zn).(H2 O).(C20 H24 O6)' _chemical_formula_sum 'C64 H54 N4 O7 Zn' _chemical_formula_weight 1056.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 '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 'P1bar' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2070(10) _cell_length_b 14.4500(10) _cell_length_c 17.8270(10) _cell_angle_alpha 81.9790(10) _cell_angle_beta 85.9670(10) _cell_angle_gamma 88.8730(10) _cell_volume 2597.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 9425 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 26.3 _exptl_crystal_description 'prisms' _exptl_crystal_colour 'deep red' _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.351 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1104 _exptl_absorpt_coefficient_mu 0.534 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. Phi & Omega scans' _diffrn_detector_area_resol_mean '56 microns' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9425 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1195 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 26.37 _reflns_number_total 9425 _reflns_number_gt 4379 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement 'Denzo & Scalepack' _computing_data_reduction 'Denzo' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0721P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9425 _refine_ls_number_parameters 697 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1705 _refine_ls_R_factor_gt 0.0632 _refine_ls_wR_factor_ref 0.1472 _refine_ls_wR_factor_gt 0.1185 _refine_ls_goodness_of_fit_ref 0.881 _refine_ls_restrained_S_all 0.881 _refine_ls_shift/su_max 0.309 _refine_ls_shift/su_mean 0.017 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.4679(3) 0.2095(2) 0.17428(18) 0.0476(9) Uani 1 1 d . . . N2 N 0.3006(3) 0.3693(2) 0.13685(18) 0.0469(9) Uani 1 1 d . . . N3 N 0.2724(3) 0.3962(2) 0.29416(18) 0.0444(8) Uani 1 1 d . . . N4 N 0.4412(3) 0.2387(2) 0.33149(18) 0.0441(8) Uani 1 1 d . . . C5 C 0.5172(4) 0.1596(3) 0.3383(2) 0.0458(10) Uani 1 1 d . . . C6 C 0.5688(4) 0.1130(3) 0.2791(2) 0.0461(11) Uani 1 1 d . . . C7 C 0.5494(4) 0.1389(3) 0.2019(2) 0.0468(11) Uani 1 1 d . . . C8 C 0.6163(4) 0.0989(3) 0.1408(3) 0.0572(12) Uani 1 1 d . . . H8 H 0.6760 0.0492 0.1450 0.069 Uiso 1 1 calc R . . C9 C 0.5769(4) 0.1463(3) 0.0765(3) 0.0597(12) Uani 1 1 d . . . H9 H 0.6056 0.1367 0.0275 0.072 Uiso 1 1 calc R . . C10 C 0.4822(4) 0.2149(3) 0.0968(3) 0.0501(11) Uani 1 1 d . . . C11 C 0.4160(4) 0.2776(3) 0.0458(2) 0.0503(11) Uani 1 1 d . . . C12 C 0.3286(4) 0.3488(3) 0.0647(2) 0.0485(11) Uani 1 1 d . . . C13 C 0.2539(4) 0.4076(3) 0.0129(2) 0.0564(12) Uani 1 1 d . . . H13 H 0.2547 0.4067 -0.0392 0.068 Uiso 1 1 calc R . . C14 C 0.1822(4) 0.4644(3) 0.0528(2) 0.0577(12) Uani 1 1 d . . . H14 H 0.1234 0.5102 0.0338 0.069 Uiso 1 1 calc R . . C15 C 0.2127(4) 0.4417(3) 0.1307(2) 0.0493(11) Uani 1 1 d . . . C16 C 0.1620(4) 0.4878(3) 0.1901(2) 0.0444(10) Uani 1 1 d . . . C17 C 0.1930(4) 0.4672(3) 0.2658(2) 0.0429(10) Uani 1 1 d . . . C18 C 0.1498(4) 0.5203(3) 0.3245(2) 0.0525(11) Uani 1 1 d . . . H18 H 0.0928 0.5715 0.3198 0.063 Uiso 1 1 calc R . . C19 C 0.2059(4) 0.4833(3) 0.3876(2) 0.0546(11) Uani 1 1 d . . . H19 H 0.1968 0.5050 0.4345 0.065 Uiso 1 1 calc R . . C20 C 0.2829(4) 0.4038(3) 0.3695(2) 0.0448(10) Uani 1 1 d . . . C21 C 0.3534(4) 0.3440(3) 0.4204(2) 0.0438(10) Uani 1 1 d . . . C22 C 0.4256(4) 0.2655(3) 0.4025(2) 0.0446(10) Uani 1 1 d . . . C23 C 0.4910(4) 0.2000(3) 0.4552(2) 0.0534(11) Uani 1 1 d . . . H23 H 0.4940 0.2020 0.5070 0.064 Uiso 1 1 calc R . . C24 C 0.5471(4) 0.1352(3) 0.4164(2) 0.0550(12) Uani 1 1 d . . . H24 H 0.5964 0.0838 0.4361 0.066 Uiso 1 1 calc R . . C25 C 0.6571(4) 0.0310(3) 0.2980(2) 0.0457(10) Uani 1 1 d . . . C26 C 0.6075(4) -0.0562(3) 0.3208(3) 0.0643(13) Uani 1 1 d . . . H26 H 0.5170 -0.0643 0.3261 0.077 Uiso 1 1 calc R . . C27 C 0.6891(5) -0.1323(3) 0.3361(3) 0.0763(15) Uani 1 1 d . . . H27 H 0.6537 -0.1913 0.3513 0.092 Uiso 1 1 calc R . . C28 C 0.8217(6) -0.1213(4) 0.3290(3) 0.0798(15) Uani 1 1 d . . . H28 H 0.8776 -0.1724 0.3388 0.096 Uiso 1 1 calc R . . C29 C 0.8706(5) -0.0348(5) 0.3074(3) 0.0967(19) Uani 1 1 d . . . H29 H 0.9611 -0.0266 0.3029 0.116 Uiso 1 1 calc R . . C30 C 0.7893(4) 0.0413(4) 0.2919(3) 0.0843(17) Uani 1 1 d . . . H30 H 0.8251 0.1003 0.2770 0.101 Uiso 1 1 calc R . . C31 C 0.3516(4) 0.3650(3) 0.5004(2) 0.0479(11) Uani 1 1 d . . . C32 C 0.2363(4) 0.3652(3) 0.5453(3) 0.0585(12) Uani 1 1 d . . . H32 H 0.1583 0.3506 0.5260 0.070 Uiso 1 1 calc R . . C33 C 0.2341(5) 0.3865(3) 0.6174(3) 0.0693(13) Uani 1 1 d . . . H33 H 0.1549 0.3856 0.6467 0.083 Uiso 1 1 calc R . . C34 C 0.3469(6) 0.4090(3) 0.6474(3) 0.0720(14) Uani 1 1 d . . . H34 H 0.3444 0.4244 0.6964 0.086 Uiso 1 1 calc R . . C35 C 0.4639(5) 0.4087(3) 0.6045(3) 0.0674(13) Uani 1 1 d . . . H35 H 0.5415 0.4233 0.6244 0.081 Uiso 1 1 calc R . . C36 C 0.4654(4) 0.3866(3) 0.5315(3) 0.0591(12) Uani 1 1 d . . . H36 H 0.5449 0.3863 0.5027 0.071 Uiso 1 1 calc R . . C37 C 0.0765(4) 0.5712(3) 0.1709(2) 0.0447(10) Uani 1 1 d . . . C38 C 0.1292(4) 0.6535(3) 0.1329(3) 0.0641(13) Uani 1 1 d . . . H38 H 0.2183 0.6558 0.1178 0.077 Uiso 1 1 calc R . . C39 C 0.0534(5) 0.7313(3) 0.1172(3) 0.0763(15) Uani 1 1 d . . . H39 H 0.0911 0.7862 0.0922 0.092 Uiso 1 1 calc R . . C40 C -0.0775(6) 0.7291(4) 0.1379(3) 0.0797(15) Uani 1 1 d . . . H40 H -0.1289 0.7827 0.1284 0.096 Uiso 1 1 calc R . . C41 C -0.1325(5) 0.6480(4) 0.1724(3) 0.0749(15) Uani 1 1 d . . . H41 H -0.2225 0.6458 0.1848 0.090 Uiso 1 1 calc R . . C42 C -0.0574(4) 0.5698(3) 0.1890(2) 0.0617(13) Uani 1 1 d . . . H42 H -0.0966 0.5148 0.2127 0.074 Uiso 1 1 calc R . . C43 C 0.4402(4) 0.2703(3) -0.0372(2) 0.0561(12) Uani 1 1 d . . . C44 C 0.4062(4) 0.1909(4) -0.0667(3) 0.0673(13) Uani 1 1 d . . . H44 H 0.3691 0.1407 -0.0344 0.081 Uiso 1 1 calc R . . C45 C 0.4268(5) 0.1856(4) -0.1432(3) 0.0763(15) Uani 1 1 d . . . H45 H 0.4034 0.1320 -0.1623 0.092 Uiso 1 1 calc R . . C46 C 0.4812(5) 0.2588(5) -0.1910(3) 0.0820(17) Uani 1 1 d . . . H46 H 0.4937 0.2556 -0.2427 0.098 Uiso 1 1 calc R . . C47 C 0.5173(4) 0.3368(4) -0.1629(3) 0.0741(15) Uani 1 1 d . . . H47 H 0.5561 0.3859 -0.1957 0.089 Uiso 1 1 calc R . . C48 C 0.4972(4) 0.3440(3) -0.0866(3) 0.0622(13) Uani 1 1 d . . . H48 H 0.5216 0.3979 -0.0682 0.075 Uiso 1 1 calc R . . Zn49 Zn 0.34967(4) 0.29141(3) 0.23645(3) 0.04723(19) Uani 1 1 d . . . O50 O 0.1805(3) 0.2038(3) 0.2564(2) 0.0600(8) Uani 1 1 d D . . H50A H 0.172(5) 0.154(2) 0.281(3) 0.11(2) Uiso 1 1 d D . . H50B H 0.110(3) 0.223(4) 0.243(3) 0.14(3) Uiso 1 1 d D . . O51 O 0.0138(3) 0.1606(2) 0.42086(17) 0.0674(9) Uani 1 1 d . . . C52 C 0.1360(5) 0.1383(4) 0.4522(3) 0.0789(15) Uani 1 1 d . . . H52A H 0.1318 0.1520 0.5041 0.095 Uiso 1 1 calc R . . H52B H 0.2041 0.1765 0.4233 0.095 Uiso 1 1 calc R . . C53 C 0.1691(5) 0.0391(4) 0.4512(3) 0.0803(15) Uani 1 1 d . . . H53A H 0.2442 0.0221 0.4809 0.096 Uiso 1 1 calc R . . H53B H 0.0956 0.0007 0.4733 0.096 Uiso 1 1 calc R . . O54 O 0.1992(3) 0.0240(2) 0.37409(18) 0.0692(9) Uani 1 1 d . . . C55 C 0.2157(4) -0.0648(4) 0.3603(3) 0.0637(13) Uani 1 1 d . . . C56 C 0.2176(5) -0.1424(5) 0.4150(3) 0.0954(18) Uani 1 1 d . . . H56 H 0.2095 -0.1355 0.4662 0.114 Uiso 1 1 calc R . . C57 C 0.2315(6) -0.2300(5) 0.3933(5) 0.127(3) Uani 1 1 d . . . H57 H 0.2330 -0.2825 0.4299 0.152 Uiso 1 1 calc R . . C58 C 0.2430(6) -0.2397(5) 0.3180(6) 0.124(3) Uani 1 1 d . . . H58 H 0.2518 -0.2991 0.3036 0.149 Uiso 1 1 calc R . . C59 C 0.2417(5) -0.1632(5) 0.2636(4) 0.0955(18) Uani 1 1 d . . . H59 H 0.2495 -0.1708 0.2126 0.115 Uiso 1 1 calc R . . C60 C 0.2290(4) -0.0768(4) 0.2837(3) 0.0668(14) Uani 1 1 d . . . O61 O 0.2288(3) 0.0044(2) 0.2354(2) 0.0843(10) Uani 1 1 d . . . C62 C 0.2495(7) 0.0057(6) 0.1552(4) 0.132(3) Uani 1 1 d . . . H62A H 0.3048 0.0585 0.1353 0.158 Uiso 1 1 calc R . . H62B H 0.2980 -0.0505 0.1461 0.158 Uiso 1 1 calc R . . C63 C 0.1472(9) 0.0107(6) 0.1171(4) 0.163(3) Uani 1 1 d . . . H63A H 0.1024 -0.0485 0.1301 0.195 Uiso 1 1 calc R . . H63B H 0.1775 0.0153 0.0639 0.195 Uiso 1 1 calc R . . O64 O 0.0516(4) 0.0819(3) 0.1234(2) 0.0967(11) Uani 1 1 d . . . C65 C 0.0833(5) 0.1680(4) 0.0827(3) 0.0830(16) Uani 1 1 d . . . H65A H 0.1090 0.1606 0.0304 0.100 Uiso 1 1 calc R . . H65B H 0.1570 0.1937 0.1040 0.100 Uiso 1 1 calc R . . C66 C -0.0302(5) 0.2328(3) 0.0849(3) 0.0713(14) Uani 1 1 d . . . H66A H -0.0124 0.2892 0.0496 0.086 Uiso 1 1 calc R . . H66B H -0.1075 0.2038 0.0702 0.086 Uiso 1 1 calc R . . O67 O -0.0530(3) 0.2556(2) 0.16021(17) 0.0688(9) Uani 1 1 d . . . C68 C -0.1600(4) 0.3097(3) 0.1741(3) 0.0598(12) Uani 1 1 d . . . C69 C -0.2388(5) 0.3522(3) 0.1197(3) 0.0739(14) Uani 1 1 d . . . H69 H -0.2198 0.3456 0.0689 0.089 Uiso 1 1 calc R . . C70 C -0.3469(5) 0.4049(4) 0.1409(4) 0.0803(16) Uani 1 1 d . . . H70 H -0.3996 0.4347 0.1042 0.096 Uiso 1 1 calc R . . C71 C -0.3753(5) 0.4129(3) 0.2150(4) 0.0795(16) Uani 1 1 d . . . H71 H -0.4489 0.4472 0.2288 0.095 Uiso 1 1 calc R . . C72 C -0.2969(5) 0.3710(3) 0.2703(3) 0.0710(14) Uani 1 1 d . . . H72 H -0.3172 0.3774 0.3210 0.085 Uiso 1 1 calc R . . C73 C -0.1882(5) 0.3194(3) 0.2497(3) 0.0587(12) Uani 1 1 d . . . O74 O -0.1022(3) 0.2776(2) 0.29907(18) 0.0674(9) Uani 1 1 d . . . C75 C -0.1277(5) 0.2856(4) 0.3777(3) 0.0742(14) Uani 1 1 d . . . H75A H -0.2008 0.2461 0.3988 0.080(15) Uiso 1 1 calc R . . H75B H -0.1508 0.3497 0.3837 0.083(17) Uiso 1 1 calc R . . C76 C -0.0104(5) 0.2570(4) 0.4174(3) 0.0737(14) Uani 1 1 d . . . H76A H 0.0647 0.2908 0.3914 0.078(15) Uiso 1 1 calc R . . H76B H -0.0210 0.2731 0.4685 0.074(15) 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 N1 0.052(2) 0.052(2) 0.038(2) -0.0031(18) -0.0021(16) 0.0130(18) N2 0.055(2) 0.047(2) 0.037(2) -0.0033(17) -0.0017(16) 0.0163(18) N3 0.047(2) 0.045(2) 0.040(2) -0.0017(17) -0.0047(16) 0.0116(17) N4 0.047(2) 0.043(2) 0.042(2) -0.0049(18) -0.0055(16) 0.0119(17) C5 0.049(2) 0.046(3) 0.041(3) 0.002(2) -0.006(2) 0.008(2) C6 0.045(2) 0.042(3) 0.049(3) 0.001(2) -0.003(2) 0.006(2) C7 0.048(2) 0.044(3) 0.046(3) 0.001(2) -0.004(2) 0.011(2) C8 0.063(3) 0.055(3) 0.053(3) -0.006(3) -0.003(2) 0.020(2) C9 0.067(3) 0.065(3) 0.046(3) -0.007(3) 0.003(2) 0.021(2) C10 0.055(3) 0.050(3) 0.045(3) -0.006(2) -0.002(2) 0.015(2) C11 0.056(3) 0.056(3) 0.038(3) -0.005(2) -0.005(2) 0.013(2) C12 0.050(2) 0.051(3) 0.042(3) -0.001(2) -0.004(2) 0.013(2) C13 0.064(3) 0.064(3) 0.040(3) -0.002(2) -0.007(2) 0.023(2) C14 0.066(3) 0.061(3) 0.044(3) 0.003(2) -0.011(2) 0.022(2) C15 0.054(3) 0.049(3) 0.044(3) -0.001(2) -0.006(2) 0.008(2) C16 0.047(2) 0.043(3) 0.042(3) -0.002(2) -0.003(2) 0.007(2) C17 0.049(2) 0.039(3) 0.040(3) -0.004(2) -0.002(2) 0.008(2) C18 0.060(3) 0.050(3) 0.048(3) -0.009(2) -0.006(2) 0.016(2) C19 0.073(3) 0.049(3) 0.043(3) -0.009(2) -0.005(2) 0.014(2) C20 0.048(2) 0.045(3) 0.041(3) -0.002(2) -0.005(2) 0.004(2) C21 0.048(2) 0.041(3) 0.041(3) -0.001(2) -0.007(2) 0.005(2) C22 0.047(2) 0.044(3) 0.041(3) 0.001(2) -0.005(2) 0.003(2) C23 0.062(3) 0.055(3) 0.042(3) -0.001(2) -0.014(2) 0.016(2) C24 0.062(3) 0.048(3) 0.053(3) 0.003(2) -0.013(2) 0.019(2) C25 0.049(3) 0.043(3) 0.044(3) -0.004(2) -0.005(2) 0.008(2) C26 0.053(3) 0.059(3) 0.077(4) 0.006(3) -0.014(2) 0.007(3) C27 0.093(4) 0.054(3) 0.081(4) 0.001(3) -0.020(3) 0.015(3) C28 0.088(4) 0.068(4) 0.081(4) -0.002(3) -0.015(3) 0.040(3) C29 0.056(3) 0.099(5) 0.128(5) 0.009(4) -0.008(3) 0.026(4) C30 0.054(3) 0.066(4) 0.127(5) 0.010(3) -0.014(3) 0.008(3) C31 0.055(3) 0.044(3) 0.044(3) -0.001(2) -0.012(2) 0.005(2) C32 0.061(3) 0.067(3) 0.048(3) -0.009(2) -0.008(2) 0.011(2) C33 0.082(4) 0.078(4) 0.048(3) -0.011(3) -0.002(3) 0.016(3) C34 0.107(4) 0.064(4) 0.046(3) -0.011(3) -0.011(3) 0.011(3) C35 0.088(4) 0.057(3) 0.060(4) -0.009(3) -0.024(3) -0.010(3) C36 0.071(3) 0.058(3) 0.047(3) -0.001(2) -0.004(2) -0.002(2) C37 0.048(3) 0.046(3) 0.041(3) -0.005(2) -0.0087(19) 0.011(2) C38 0.055(3) 0.054(3) 0.080(4) 0.005(3) -0.011(2) 0.002(3) C39 0.093(4) 0.048(3) 0.089(4) -0.001(3) -0.026(3) 0.012(3) C40 0.094(4) 0.075(4) 0.069(4) -0.008(3) -0.018(3) 0.041(3) C41 0.058(3) 0.102(5) 0.060(3) 0.001(3) -0.002(2) 0.035(3) C42 0.052(3) 0.070(3) 0.059(3) 0.006(3) -0.002(2) 0.006(3) C43 0.058(3) 0.068(3) 0.041(3) -0.004(3) -0.010(2) 0.027(2) C44 0.082(3) 0.073(4) 0.049(3) -0.017(3) -0.002(3) 0.014(3) C45 0.081(4) 0.092(4) 0.060(4) -0.028(3) -0.012(3) 0.028(3) C46 0.082(4) 0.124(5) 0.040(3) -0.015(4) -0.006(3) 0.041(4) C47 0.062(3) 0.105(5) 0.049(4) 0.006(3) -0.002(3) 0.026(3) C48 0.057(3) 0.078(4) 0.050(3) -0.005(3) -0.002(2) 0.025(3) Zn49 0.0540(3) 0.0461(3) 0.0402(3) -0.0024(2) -0.0048(2) 0.0125(2) O50 0.058(2) 0.057(2) 0.062(2) 0.0034(19) -0.0078(17) -0.0008(19) O51 0.068(2) 0.068(2) 0.064(2) -0.0019(18) -0.0063(16) -0.0003(18) C52 0.086(4) 0.097(5) 0.055(3) -0.012(3) -0.010(3) 0.003(3) C53 0.081(4) 0.099(5) 0.058(4) 0.003(3) -0.013(3) 0.007(3) O54 0.081(2) 0.066(2) 0.057(2) 0.0029(19) -0.0026(16) 0.0024(18) C55 0.049(3) 0.053(4) 0.085(4) 0.002(3) -0.003(3) 0.014(2) C56 0.094(4) 0.080(5) 0.098(5) 0.024(4) 0.013(3) 0.024(3) C57 0.114(5) 0.069(5) 0.173(8) 0.033(5) 0.046(5) 0.032(4) C58 0.105(5) 0.064(5) 0.197(9) -0.022(6) 0.045(5) 0.006(4) C59 0.088(4) 0.074(5) 0.125(6) -0.023(4) 0.002(4) 0.020(3) C60 0.054(3) 0.060(4) 0.083(4) -0.003(3) -0.002(3) 0.014(3) O61 0.112(3) 0.080(3) 0.058(2) -0.002(2) -0.0069(19) 0.036(2) C62 0.121(5) 0.198(8) 0.083(6) -0.050(5) -0.020(4) 0.081(5) C63 0.202(9) 0.185(8) 0.113(6) -0.063(6) -0.042(6) 0.112(7) O64 0.123(3) 0.084(3) 0.083(3) -0.011(2) -0.018(2) 0.031(3) C65 0.083(4) 0.108(5) 0.061(4) -0.026(4) 0.002(3) 0.012(4) C66 0.085(4) 0.074(4) 0.052(3) -0.001(3) -0.002(3) 0.006(3) O67 0.075(2) 0.073(2) 0.057(2) -0.0059(18) -0.0072(17) 0.0216(18) C68 0.059(3) 0.053(3) 0.065(4) 0.004(3) -0.006(3) 0.001(3) C69 0.078(3) 0.066(4) 0.076(4) -0.001(3) -0.015(3) 0.004(3) C70 0.079(4) 0.059(4) 0.101(5) 0.004(3) -0.024(3) 0.009(3) C71 0.059(3) 0.056(4) 0.121(5) -0.005(4) -0.002(4) 0.008(3) C72 0.073(3) 0.054(3) 0.083(4) -0.003(3) 0.003(3) 0.001(3) C73 0.061(3) 0.045(3) 0.068(4) 0.000(3) 0.002(3) -0.005(2) O74 0.077(2) 0.070(2) 0.054(2) -0.0054(18) -0.0059(18) 0.0129(18) C75 0.086(4) 0.075(4) 0.061(4) -0.013(3) 0.008(3) 0.004(3) C76 0.084(4) 0.079(4) 0.060(4) -0.015(3) -0.006(3) -0.002(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C7 1.363(5) . ? N1 C10 1.370(5) . ? N1 Zn49 2.051(3) . ? N2 C15 1.363(5) . ? N2 C12 1.369(5) . ? N2 Zn49 2.053(3) . ? N3 C17 1.357(5) . ? N3 C20 1.375(5) . ? N3 Zn49 2.061(3) . ? N4 C5 1.365(5) . ? N4 C22 1.372(5) . ? N4 Zn49 2.039(3) . ? C5 C6 1.397(5) . ? C5 C24 1.440(5) . ? C6 C7 1.402(5) . ? C6 C25 1.490(5) . ? C7 C8 1.430(5) . ? C8 C9 1.334(5) . ? C9 C10 1.435(5) . ? C10 C11 1.392(5) . ? C11 C12 1.410(5) . ? C11 C43 1.500(6) . ? C12 C13 1.418(5) . ? C13 C14 1.335(5) . ? C14 C15 1.435(5) . ? C15 C16 1.394(5) . ? C16 C17 1.398(5) . ? C16 C37 1.489(5) . ? C17 C18 1.422(5) . ? C18 C19 1.339(5) . ? C19 C20 1.441(5) . ? C20 C21 1.391(5) . ? C21 C22 1.401(5) . ? C21 C31 1.498(5) . ? C22 C23 1.430(5) . ? C23 C24 1.337(5) . ? C25 C30 1.355(5) . ? C25 C26 1.365(5) . ? C26 C27 1.374(6) . ? C27 C28 1.361(6) . ? C28 C29 1.350(7) . ? C29 C30 1.373(6) . ? C31 C32 1.376(5) . ? C31 C36 1.381(5) . ? C32 C33 1.362(5) . ? C33 C34 1.366(6) . ? C34 C35 1.372(6) . ? C35 C36 1.381(6) . ? C37 C38 1.383(5) . ? C37 C42 1.382(5) . ? C38 C39 1.360(6) . ? C39 C40 1.360(6) . ? C40 C41 1.357(6) . ? C41 C42 1.363(6) . ? C43 C44 1.386(6) . ? C43 C48 1.393(6) . ? C44 C45 1.379(6) . ? C45 C46 1.363(7) . ? C46 C47 1.362(7) . ? C47 C48 1.380(6) . ? Zn49 O50 2.141(3) . ? O51 C52 1.416(5) . ? O51 C76 1.403(5) . ? C52 C53 1.468(6) . ? C53 O54 1.433(5) . ? O54 C55 1.345(5) . ? C55 C56 1.380(6) . ? C55 C60 1.397(6) . ? C56 C57 1.376(8) . ? C57 C58 1.366(9) . ? C58 C59 1.365(8) . ? C59 C60 1.348(7) . ? C60 O61 1.355(5) . ? O61 C62 1.427(6) . ? C62 C63 1.281(8) . ? C63 O64 1.414(7) . ? O64 C65 1.381(6) . ? C65 C66 1.477(6) . ? C66 O67 1.428(5) . ? O67 C68 1.360(5) . ? C68 C69 1.374(6) . ? C68 C73 1.384(6) . ? C69 C70 1.389(6) . ? C70 C71 1.353(7) . ? C71 C72 1.380(6) . ? C72 C73 1.382(6) . ? C73 O74 1.359(5) . ? O74 C75 1.427(5) . ? C75 C76 1.458(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C7 N1 C10 106.0(3) . . ? C7 N1 Zn49 126.8(3) . . ? C10 N1 Zn49 127.2(3) . . ? C15 N2 C12 106.1(3) . . ? C15 N2 Zn49 125.7(3) . . ? C12 N2 Zn49 127.2(3) . . ? C17 N3 C20 107.1(3) . . ? C17 N3 Zn49 125.9(3) . . ? C20 N3 Zn49 126.8(3) . . ? C5 N4 C22 106.5(3) . . ? C5 N4 Zn49 124.7(3) . . ? C22 N4 Zn49 128.2(3) . . ? N4 C5 C6 126.4(4) . . ? N4 C5 C24 109.3(4) . . ? C6 C5 C24 124.1(4) . . ? C5 C6 C7 125.6(4) . . ? C5 C6 C25 118.2(4) . . ? C7 C6 C25 116.1(4) . . ? N1 C7 C6 124.4(4) . . ? N1 C7 C8 110.2(4) . . ? C6 C7 C8 125.3(4) . . ? C9 C8 C7 106.9(4) . . ? C8 C9 C10 107.6(4) . . ? N1 C10 C11 125.3(4) . . ? N1 C10 C9 109.3(4) . . ? C11 C10 C9 125.4(4) . . ? C10 C11 C12 125.9(4) . . ? C10 C11 C43 117.7(4) . . ? C12 C11 C43 116.4(4) . . ? N2 C12 C11 124.5(4) . . ? N2 C12 C13 110.0(4) . . ? C11 C12 C13 125.4(4) . . ? C14 C13 C12 107.2(4) . . ? C13 C14 C15 107.4(4) . . ? N2 C15 C16 125.5(4) . . ? N2 C15 C14 109.3(4) . . ? C16 C15 C14 125.2(4) . . ? C15 C16 C17 125.5(4) . . ? C15 C16 C37 117.6(4) . . ? C17 C16 C37 116.7(4) . . ? N3 C17 C16 125.7(4) . . ? N3 C17 C18 109.6(4) . . ? C16 C17 C18 124.7(4) . . ? C19 C18 C17 107.7(4) . . ? C18 C19 C20 107.2(4) . . ? N3 C20 C21 126.1(4) . . ? N3 C20 C19 108.4(4) . . ? C21 C20 C19 125.5(4) . . ? C20 C21 C22 125.0(4) . . ? C20 C21 C31 117.4(4) . . ? C22 C21 C31 117.7(4) . . ? N4 C22 C21 124.9(4) . . ? N4 C22 C23 109.6(4) . . ? C21 C22 C23 125.5(4) . . ? C24 C23 C22 107.3(4) . . ? C23 C24 C5 107.3(4) . . ? C30 C25 C26 118.4(4) . . ? C30 C25 C6 120.5(4) . . ? C26 C25 C6 121.1(4) . . ? C25 C26 C27 121.1(4) . . ? C28 C27 C26 119.9(5) . . ? C29 C28 C27 118.9(5) . . ? C28 C29 C30 121.3(5) . . ? C25 C30 C29 120.4(5) . . ? C32 C31 C36 117.4(4) . . ? C32 C31 C21 121.4(4) . . ? C36 C31 C21 121.2(4) . . ? C33 C32 C31 121.5(4) . . ? C34 C33 C32 120.8(4) . . ? C33 C34 C35 119.4(5) . . ? C34 C35 C36 119.5(4) . . ? C35 C36 C31 121.5(4) . . ? C38 C37 C42 117.3(4) . . ? C38 C37 C16 120.6(4) . . ? C42 C37 C16 122.1(4) . . ? C39 C38 C37 121.3(4) . . ? C40 C39 C38 120.2(5) . . ? C41 C40 C39 119.6(5) . . ? C40 C41 C42 120.8(4) . . ? C41 C42 C37 120.7(4) . . ? C44 C43 C48 118.5(4) . . ? C44 C43 C11 121.2(4) . . ? C48 C43 C11 120.3(4) . . ? C45 C44 C43 120.8(5) . . ? C46 C45 C44 120.1(5) . . ? C47 C46 C45 120.0(5) . . ? C46 C47 C48 121.1(5) . . ? C47 C48 C43 119.6(5) . . ? N4 Zn49 N1 89.73(13) . . ? N4 Zn49 N2 164.12(12) . . ? N1 Zn49 N2 88.96(13) . . ? N4 Zn49 N3 88.43(13) . . ? N1 Zn49 N3 165.10(11) . . ? N2 Zn49 N3 88.79(13) . . ? N4 Zn49 O50 97.42(13) . . ? N1 Zn49 O50 98.74(13) . . ? N2 Zn49 O50 98.42(14) . . ? N3 Zn49 O50 96.16(12) . . ? C52 O51 C76 109.4(4) . . ? O51 C52 C53 110.8(4) . . ? O54 C53 C52 108.7(4) . . ? C55 O54 C53 117.6(4) . . ? O54 C55 C56 125.3(6) . . ? O54 C55 C60 115.5(5) . . ? C56 C55 C60 119.2(5) . . ? C55 C56 C57 119.6(6) . . ? C58 C57 C56 120.0(7) . . ? C59 C58 C57 120.7(7) . . ? C60 C59 C58 120.3(6) . . ? C59 C60 O61 125.9(6) . . ? C59 C60 C55 120.2(6) . . ? O61 C60 C55 113.9(5) . . ? C60 O61 C62 121.4(5) . . ? C63 C62 O61 117.0(6) . . ? C62 C63 O64 121.2(7) . . ? C65 O64 C63 115.3(5) . . ? O64 C65 C66 110.4(4) . . ? O67 C66 C65 109.0(4) . . ? C68 O67 C66 117.1(4) . . ? O67 C68 C69 124.9(5) . . ? O67 C68 C73 114.9(4) . . ? C69 C68 C73 120.2(5) . . ? C68 C69 C70 119.7(5) . . ? C71 C70 C69 119.9(5) . . ? C70 C71 C72 121.2(5) . . ? C71 C72 C73 119.4(5) . . ? O74 C73 C72 124.4(5) . . ? O74 C73 C68 116.0(4) . . ? C72 C73 C68 119.6(5) . . ? C73 O74 C75 117.8(4) . . ? O74 C75 C76 108.8(4) . . ? O51 C76 C75 111.7(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 C22 N4 C5 C6 -173.3(4) . . . . ? Zn49 N4 C5 C6 14.8(5) . . . . ? C22 N4 C5 C24 1.4(4) . . . . ? Zn49 N4 C5 C24 -170.4(2) . . . . ? N4 C5 C6 C7 -1.1(6) . . . . ? C24 C5 C6 C7 -175.1(4) . . . . ? N4 C5 C6 C25 176.0(3) . . . . ? C24 C5 C6 C25 2.0(6) . . . . ? C10 N1 C7 C6 177.0(3) . . . . ? Zn49 N1 C7 C6 -2.4(5) . . . . ? C10 N1 C7 C8 -0.1(4) . . . . ? Zn49 N1 C7 C8 -179.5(3) . . . . ? C5 C6 C7 N1 -5.6(6) . . . . ? C25 C6 C7 N1 177.2(3) . . . . ? C5 C6 C7 C8 171.0(4) . . . . ? C25 C6 C7 C8 -6.1(6) . . . . ? N1 C7 C8 C9 1.0(5) . . . . ? C6 C7 C8 C9 -176.0(4) . . . . ? C7 C8 C9 C10 -1.5(5) . . . . ? C7 N1 C10 C11 179.5(4) . . . . ? Zn49 N1 C10 C11 -1.0(6) . . . . ? C7 N1 C10 C9 -0.9(4) . . . . ? Zn49 N1 C10 C9 178.6(3) . . . . ? C8 C9 C10 N1 1.5(5) . . . . ? C8 C9 C10 C11 -178.9(4) . . . . ? N1 C10 C11 C12 3.5(7) . . . . ? C9 C10 C11 C12 -176.0(4) . . . . ? N1 C10 C11 C43 -177.4(4) . . . . ? C9 C10 C11 C43 3.1(6) . . . . ? C15 N2 C12 C11 -179.9(4) . . . . ? Zn49 N2 C12 C11 -11.2(5) . . . . ? C15 N2 C12 C13 -1.8(4) . . . . ? Zn49 N2 C12 C13 166.9(2) . . . . ? C10 C11 C12 N2 3.0(6) . . . . ? C43 C11 C12 N2 -176.1(4) . . . . ? C10 C11 C12 C13 -174.8(4) . . . . ? C43 C11 C12 C13 6.1(6) . . . . ? N2 C12 C13 C14 0.9(5) . . . . ? C11 C12 C13 C14 179.0(4) . . . . ? C12 C13 C14 C15 0.4(5) . . . . ? C12 N2 C15 C16 -176.9(4) . . . . ? Zn49 N2 C15 C16 14.2(5) . . . . ? C12 N2 C15 C14 2.1(4) . . . . ? Zn49 N2 C15 C14 -166.8(2) . . . . ? C13 C14 C15 N2 -1.6(5) . . . . ? C13 C14 C15 C16 177.4(4) . . . . ? N2 C15 C16 C17 0.0(6) . . . . ? C14 C15 C16 C17 -178.8(4) . . . . ? N2 C15 C16 C37 174.4(4) . . . . ? C14 C15 C16 C37 -4.4(6) . . . . ? C20 N3 C17 C16 176.6(3) . . . . ? Zn49 N3 C17 C16 -7.9(5) . . . . ? C20 N3 C17 C18 -1.1(4) . . . . ? Zn49 N3 C17 C18 174.5(2) . . . . ? C15 C16 C17 N3 -3.4(6) . . . . ? C37 C16 C17 N3 -177.9(3) . . . . ? C15 C16 C17 C18 173.9(4) . . . . ? C37 C16 C17 C18 -0.6(5) . . . . ? N3 C17 C18 C19 1.8(4) . . . . ? C16 C17 C18 C19 -175.9(4) . . . . ? C17 C18 C19 C20 -1.7(4) . . . . ? C17 N3 C20 C21 178.8(3) . . . . ? Zn49 N3 C20 C21 3.2(5) . . . . ? C17 N3 C20 C19 0.0(4) . . . . ? Zn49 N3 C20 C19 -175.5(2) . . . . ? C18 C19 C20 N3 1.1(4) . . . . ? C18 C19 C20 C21 -177.7(4) . . . . ? N3 C20 C21 C22 -0.1(6) . . . . ? C19 C20 C21 C22 178.4(4) . . . . ? N3 C20 C21 C31 -179.9(3) . . . . ? C19 C20 C21 C31 -1.4(5) . . . . ? C5 N4 C22 C21 -179.9(3) . . . . ? Zn49 N4 C22 C21 -8.4(5) . . . . ? C5 N4 C22 C23 -1.5(4) . . . . ? Zn49 N4 C22 C23 170.0(2) . . . . ? C20 C21 C22 N4 2.7(6) . . . . ? C31 C21 C22 N4 -177.5(3) . . . . ? C20 C21 C22 C23 -175.5(4) . . . . ? C31 C21 C22 C23 4.3(5) . . . . ? N4 C22 C23 C24 0.9(4) . . . . ? C21 C22 C23 C24 179.4(4) . . . . ? C22 C23 C24 C5 0.0(4) . . . . ? N4 C5 C24 C23 -0.9(4) . . . . ? C6 C5 C24 C23 174.0(4) . . . . ? C5 C6 C25 C30 -95.6(5) . . . . ? C7 C6 C25 C30 81.8(5) . . . . ? C5 C6 C25 C26 85.3(5) . . . . ? C7 C6 C25 C26 -97.4(5) . . . . ? C30 C25 C26 C27 -1.0(7) . . . . ? C6 C25 C26 C27 178.1(4) . . . . ? C25 C26 C27 C28 0.4(8) . . . . ? C26 C27 C28 C29 0.5(8) . . . . ? C27 C28 C29 C30 -0.7(9) . . . . ? C26 C25 C30 C29 0.8(8) . . . . ? C6 C25 C30 C29 -178.3(5) . . . . ? C28 C29 C30 C25 0.0(9) . . . . ? C20 C21 C31 C32 61.5(5) . . . . ? C22 C21 C31 C32 -118.3(4) . . . . ? C20 C21 C31 C36 -117.4(4) . . . . ? C22 C21 C31 C36 62.8(5) . . . . ? C36 C31 C32 C33 0.4(6) . . . . ? C21 C31 C32 C33 -178.5(4) . . . . ? C31 C32 C33 C34 0.5(7) . . . . ? C32 C33 C34 C35 -1.0(7) . . . . ? C33 C34 C35 C36 0.7(7) . . . . ? C34 C35 C36 C31 0.3(7) . . . . ? C32 C31 C36 C35 -0.8(6) . . . . ? C21 C31 C36 C35 178.1(4) . . . . ? C15 C16 C37 C38 -70.7(5) . . . . ? C17 C16 C37 C38 104.2(4) . . . . ? C15 C16 C37 C42 108.4(5) . . . . ? C17 C16 C37 C42 -76.7(5) . . . . ? C42 C37 C38 C39 3.1(7) . . . . ? C16 C37 C38 C39 -177.7(4) . . . . ? C37 C38 C39 C40 -0.9(7) . . . . ? C38 C39 C40 C41 -1.9(8) . . . . ? C39 C40 C41 C42 2.4(8) . . . . ? C40 C41 C42 C37 -0.1(8) . . . . ? C38 C37 C42 C41 -2.6(7) . . . . ? C16 C37 C42 C41 178.3(4) . . . . ? C10 C11 C43 C44 63.4(5) . . . . ? C12 C11 C43 C44 -117.5(5) . . . . ? C10 C11 C43 C48 -117.0(4) . . . . ? C12 C11 C43 C48 62.2(5) . . . . ? C48 C43 C44 C45 -0.8(7) . . . . ? C11 C43 C44 C45 178.8(4) . . . . ? C43 C44 C45 C46 0.1(7) . . . . ? C44 C45 C46 C47 1.0(8) . . . . ? C45 C46 C47 C48 -1.4(7) . . . . ? C46 C47 C48 C43 0.6(7) . . . . ? C44 C43 C48 C47 0.5(6) . . . . ? C11 C43 C48 C47 -179.2(4) . . . . ? C5 N4 Zn49 N1 -16.3(3) . . . . ? C22 N4 Zn49 N1 173.7(3) . . . . ? C5 N4 Zn49 N2 -101.6(6) . . . . ? C22 N4 Zn49 N2 88.4(6) . . . . ? C5 N4 Zn49 N3 178.5(3) . . . . ? C22 N4 Zn49 N3 8.4(3) . . . . ? C5 N4 Zn49 O50 82.5(3) . . . . ? C22 N4 Zn49 O50 -87.6(3) . . . . ? C7 N1 Zn49 N4 10.8(3) . . . . ? C10 N1 Zn49 N4 -168.6(3) . . . . ? C7 N1 Zn49 N2 175.0(3) . . . . ? C10 N1 Zn49 N2 -4.4(3) . . . . ? C7 N1 Zn49 N3 93.6(6) . . . . ? C10 N1 Zn49 N3 -85.7(6) . . . . ? C7 N1 Zn49 O50 -86.7(3) . . . . ? C10 N1 Zn49 O50 93.9(3) . . . . ? C15 N2 Zn49 N4 -97.8(5) . . . . ? C12 N2 Zn49 N4 95.6(6) . . . . ? C15 N2 Zn49 N1 176.8(3) . . . . ? C12 N2 Zn49 N1 10.2(3) . . . . ? C15 N2 Zn49 N3 -17.9(3) . . . . ? C12 N2 Zn49 N3 175.5(3) . . . . ? C15 N2 Zn49 O50 78.1(3) . . . . ? C12 N2 Zn49 O50 -88.5(3) . . . . ? C17 N3 Zn49 N4 179.3(3) . . . . ? C20 N3 Zn49 N4 -5.9(3) . . . . ? C17 N3 Zn49 N1 96.3(6) . . . . ? C20 N3 Zn49 N1 -88.9(6) . . . . ? C17 N3 Zn49 N2 15.0(3) . . . . ? C20 N3 Zn49 N2 -170.3(3) . . . . ? C17 N3 Zn49 O50 -83.4(3) . . . . ? C20 N3 Zn49 O50 91.4(3) . . . . ? C76 O51 C52 C53 -175.6(4) . . . . ? O51 C52 C53 O54 69.9(5) . . . . ? C52 C53 O54 C55 -171.7(4) . . . . ? C53 O54 C55 C56 -6.0(7) . . . . ? C53 O54 C55 C60 172.6(4) . . . . ? O54 C55 C56 C57 178.1(5) . . . . ? C60 C55 C56 C57 -0.5(8) . . . . ? C55 C56 C57 C58 -0.2(9) . . . . ? C56 C57 C58 C59 0.4(11) . . . . ? C57 C58 C59 C60 0.0(10) . . . . ? C58 C59 C60 O61 178.7(5) . . . . ? C58 C59 C60 C55 -0.7(8) . . . . ? O54 C55 C60 C59 -177.8(4) . . . . ? C56 C55 C60 C59 0.9(7) . . . . ? O54 C55 C60 O61 2.7(6) . . . . ? C56 C55 C60 O61 -178.6(4) . . . . ? C59 C60 O61 C62 -3.4(8) . . . . ? C55 C60 O61 C62 176.1(4) . . . . ? C60 O61 C62 C63 97.9(8) . . . . ? O61 C62 C63 O64 53.2(12) . . . . ? C62 C63 O64 C65 79.2(10) . . . . ? C63 O64 C65 C66 172.3(5) . . . . ? O64 C65 C66 O67 69.0(5) . . . . ? C65 C66 O67 C68 -175.5(4) . . . . ? C66 O67 C68 C69 -7.5(6) . . . . ? C66 O67 C68 C73 171.6(4) . . . . ? O67 C68 C69 C70 179.1(4) . . . . ? C73 C68 C69 C70 0.0(7) . . . . ? C68 C69 C70 C71 -1.1(7) . . . . ? C69 C70 C71 C72 1.4(8) . . . . ? C70 C71 C72 C73 -0.5(7) . . . . ? C71 C72 C73 O74 177.9(4) . . . . ? C71 C72 C73 C68 -0.6(7) . . . . ? O67 C68 C73 O74 3.0(6) . . . . ? C69 C68 C73 O74 -177.8(4) . . . . ? O67 C68 C73 C72 -178.3(4) . . . . ? C69 C68 C73 C72 0.8(7) . . . . ? C72 C73 O74 C75 1.6(6) . . . . ? C68 C73 O74 C75 -179.9(4) . . . . ? C73 O74 C75 C76 -166.1(4) . . . . ? C52 O51 C76 C75 173.5(4) . . . . ? O74 C75 C76 O51 -69.4(5) . . . . ? _diffrn_measured_fraction_theta_max 0.888 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.888 _refine_diff_density_max 0.396 _refine_diff_density_min -0.292 _refine_diff_density_rms 0.049 #=====END================== data_compound-2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C44 H28 N4 Zn).(H2 O).1/2(C12 H24 O6).(C9 H10 O2)' _chemical_formula_sum 'C59 H52 N4 O6 Zn' _chemical_formula_weight 978.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'triclinic' _symmetry_space_group_name_H-M 'P1bar' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.1820(10) _cell_length_b 12.4310(10) _cell_length_c 17.0770(10) _cell_angle_alpha 70.6520(10) _cell_angle_beta 82.9990(10) _cell_angle_gamma 87.5520(10) _cell_volume 2421.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 120 _cell_measurement_reflns_used 9878 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 26.3 _exptl_crystal_description 'prisms' _exptl_crystal_colour 'deep red' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.342 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1024 _exptl_absorpt_coefficient_mu 0.565 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120 _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '1 degree Phi & Omega scans' _diffrn_detector_area_resol_mean '56 microns' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9878 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1644 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 26.37 _reflns_number_total 9878 _reflns_number_gt 4371 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement 'Denzo & Scalepack' _computing_data_reduction 'Denzo' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0624P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9878 _refine_ls_number_parameters 638 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.2001 _refine_ls_R_factor_gt 0.0764 _refine_ls_wR_factor_ref 0.1603 _refine_ls_wR_factor_gt 0.1360 _refine_ls_goodness_of_fit_ref 0.885 _refine_ls_restrained_S_all 0.885 _refine_ls_shift/su_max 0.369 _refine_ls_shift/su_mean 0.070 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.7484(3) 0.1947(3) 0.2934(2) 0.0200(10) Uani 1 1 d . . . N2 N 0.6407(3) 0.0407(3) 0.2325(2) 0.0197(10) Uani 1 1 d . . . N3 N 0.4429(3) 0.1794(4) 0.2221(2) 0.0208(10) Uani 1 1 d . . . N4 N 0.5476(3) 0.3292(3) 0.2891(2) 0.0211(10) Uani 1 1 d . . . C5 C 0.6103(4) 0.3908(4) 0.3204(3) 0.0226(12) Uani 1 1 d . . . C6 C 0.7212(4) 0.3679(4) 0.3348(3) 0.0200(12) Uani 1 1 d . . . C7 C 0.7856(4) 0.2785(4) 0.3189(3) 0.0231(12) Uani 1 1 d . . . C8 C 0.9031(4) 0.2617(4) 0.3283(3) 0.0262(13) Uani 1 1 d . . . H8 H 0.9495 0.3087 0.3440 0.031 Uiso 1 1 calc R . . C9 C 0.9327(4) 0.1661(4) 0.3104(3) 0.0237(12) Uani 1 1 d . . . H9 H 1.0046 0.1333 0.3111 0.028 Uiso 1 1 calc R . . C10 C 0.8363(4) 0.1220(4) 0.2898(3) 0.0209(12) Uani 1 1 d . . . C11 C 0.8323(4) 0.0242(4) 0.2676(3) 0.0217(12) Uani 1 1 d . . . C12 C 0.7423(4) -0.0138(4) 0.2397(3) 0.0197(12) Uani 1 1 d . . . C13 C 0.7422(4) -0.1100(4) 0.2114(3) 0.0239(12) Uani 1 1 d . . . H13 H 0.8017 -0.1618 0.2108 0.029 Uiso 1 1 calc R . . C14 C 0.6418(4) -0.1141(4) 0.1854(3) 0.0242(12) Uani 1 1 d . . . H14 H 0.6184 -0.1682 0.1626 0.029 Uiso 1 1 calc R . . C15 C 0.5777(4) -0.0208(4) 0.1993(3) 0.0204(12) Uani 1 1 d . . . C16 C 0.4692(4) 0.0059(4) 0.1797(3) 0.0224(12) Uani 1 1 d . . . C17 C 0.4053(4) 0.0980(4) 0.1925(3) 0.0225(12) Uani 1 1 d . . . C18 C 0.2910(4) 0.1213(4) 0.1774(3) 0.0266(13) Uani 1 1 d . . . H18 H 0.2459 0.0778 0.1575 0.032 Uiso 1 1 calc R . . C19 C 0.2606(4) 0.2146(4) 0.1964(3) 0.0257(13) Uani 1 1 d . . . H19 H 0.1896 0.2495 0.1930 0.031 Uiso 1 1 calc R . . C20 C 0.3561(4) 0.2535(4) 0.2233(3) 0.0232(12) Uani 1 1 d . . . C21 C 0.3576(4) 0.3498(4) 0.2477(3) 0.0215(12) Uani 1 1 d . . . C22 C 0.4454(4) 0.3850(4) 0.2801(3) 0.0207(12) Uani 1 1 d . . . C23 C 0.4472(4) 0.4831(5) 0.3070(3) 0.0280(13) Uani 1 1 d . . . H23 H 0.3886 0.5363 0.3064 0.034 Uiso 1 1 calc R . . C24 C 0.5469(4) 0.4862(4) 0.3331(3) 0.0269(13) Uani 1 1 d . . . H24 H 0.5709 0.5405 0.3555 0.032 Uiso 1 1 calc R . . C25 C 0.7745(4) 0.4419(5) 0.3734(3) 0.0234(12) Uani 1 1 d . . . C26 C 0.7962(4) 0.5562(4) 0.3315(3) 0.0262(13) Uani 1 1 d . . . H26 H 0.7776 0.5896 0.2761 0.031 Uiso 1 1 calc R . . C27 C 0.8447(4) 0.6230(5) 0.3688(3) 0.0268(13) Uani 1 1 d . . . H27 H 0.8611 0.7009 0.3388 0.032 Uiso 1 1 calc R . . C28 C 0.8690(4) 0.5742(5) 0.4510(3) 0.0254(13) Uani 1 1 d . . . H28 H 0.9011 0.6192 0.4776 0.030 Uiso 1 1 calc R . . C29 C 0.8464(4) 0.4607(5) 0.4937(3) 0.0313(14) Uani 1 1 d . . . H29 H 0.8630 0.4278 0.5496 0.038 Uiso 1 1 calc R . . C30 C 0.7997(4) 0.3946(5) 0.4557(3) 0.0286(13) Uani 1 1 d . . . H30 H 0.7846 0.3164 0.4857 0.034 Uiso 1 1 calc R . . C31 C 0.2550(4) 0.4262(4) 0.2378(3) 0.0215(12) Uani 1 1 d . . . C32 C 0.2243(4) 0.4784(4) 0.1575(3) 0.0239(12) Uani 1 1 d . . . H32 H 0.2674 0.4663 0.1109 0.029 Uiso 1 1 calc R . . C33 C 0.1314(4) 0.5477(4) 0.1456(3) 0.0277(13) Uani 1 1 d . . . H33 H 0.1115 0.5837 0.0908 0.033 Uiso 1 1 calc R . . C34 C 0.0680(4) 0.5644(4) 0.2130(3) 0.0257(13) Uani 1 1 d . . . H34 H 0.0042 0.6118 0.2051 0.031 Uiso 1 1 calc R . . C35 C 0.0978(4) 0.5123(5) 0.2915(3) 0.0295(13) Uani 1 1 d . . . H35 H 0.0531 0.5229 0.3380 0.035 Uiso 1 1 calc R . . C36 C 0.1915(4) 0.4443(4) 0.3049(3) 0.0245(13) Uani 1 1 d . . . H36 H 0.2117 0.4105 0.3598 0.029 Uiso 1 1 calc R . . C37 C 0.4165(4) -0.0677(5) 0.1410(3) 0.0230(12) Uani 1 1 d . . . C38 C 0.4025(4) -0.1852(5) 0.1800(3) 0.0255(13) Uani 1 1 d . . . H38 H 0.4259 -0.2200 0.2338 0.031 Uiso 1 1 calc R . . C39 C 0.3562(4) -0.2514(5) 0.1432(3) 0.0308(13) Uani 1 1 d . . . H39 H 0.3485 -0.3312 0.1710 0.037 Uiso 1 1 calc R . . C40 C 0.3204(4) -0.2020(5) 0.0650(3) 0.0294(14) Uani 1 1 d . . . H40 H 0.2870 -0.2480 0.0398 0.035 Uiso 1 1 calc R . . C41 C 0.3329(4) -0.0877(5) 0.0241(3) 0.0260(13) Uani 1 1 d . . . H41 H 0.3100 -0.0547 -0.0300 0.031 Uiso 1 1 calc R . . C42 C 0.3790(4) -0.0197(5) 0.0617(3) 0.0250(13) Uani 1 1 d . . . H42 H 0.3853 0.0601 0.0336 0.030 Uiso 1 1 calc R . . C43 C 0.9336(4) -0.0500(4) 0.2759(3) 0.0203(12) Uani 1 1 d . . . C44 C 0.9639(4) -0.1087(4) 0.3559(3) 0.0269(13) Uani 1 1 d . . . H44 H 0.9212 -0.0994 0.4037 0.032 Uiso 1 1 calc R . . C45 C 1.0552(4) -0.1798(4) 0.3658(3) 0.0293(13) Uani 1 1 d . . . H45 H 1.0750 -0.2185 0.4203 0.035 Uiso 1 1 calc R . . C46 C 1.1185(4) -0.1955(5) 0.2966(3) 0.0338(14) Uani 1 1 d . . . H46 H 1.1805 -0.2454 0.3038 0.041 Uiso 1 1 calc R . . C47 C 1.0902(4) -0.1375(5) 0.2176(3) 0.0312(14) Uani 1 1 d . . . H47 H 1.1334 -0.1466 0.1700 0.037 Uiso 1 1 calc R . . C48 C 0.9990(4) -0.0662(4) 0.2079(3) 0.0295(13) Uani 1 1 d . . . H48 H 0.9803 -0.0272 0.1532 0.035 Uiso 1 1 calc R . . Zn49 Zn 0.58695(5) 0.17143(6) 0.27700(3) 0.02114(18) Uani 1 1 d . . . O50 O 0.5410(3) 0.0761(4) 0.4050(2) 0.0272(9) Uani 1 1 d D . . H50A H 0.582(4) 0.027(4) 0.428(3) 0.08(2) Uiso 1 1 d D . . H50B H 0.531(5) 0.110(5) 0.438(3) 0.07(2) Uiso 1 1 d D . . O51 O 0.3260(4) -0.1222(4) 0.4588(3) 0.0678(15) Uani 1 1 d . . . C52 C 0.4054(6) -0.1611(7) 0.3958(4) 0.072(2) Uani 1 1 d . . . H52A H 0.3628 -0.1963 0.3648 0.086 Uiso 1 1 calc R . . H52B H 0.4456 -0.0945 0.3550 0.086 Uiso 1 1 calc R . . C53 C 0.4833(8) -0.2428(9) 0.4399(5) 0.106(3) Uani 1 1 d . . . H53A H 0.4436 -0.3074 0.4834 0.128 Uiso 1 1 calc R . . H53B H 0.5309 -0.2730 0.4007 0.128 Uiso 1 1 calc R . . O54 O 0.5445(5) -0.1889(5) 0.4750(3) 0.0809(17) Uani 1 1 d . . . C55 C 0.6559(7) -0.2400(7) 0.4845(6) 0.110(4) Uani 1 1 d . . . H55A H 0.6969 -0.2305 0.4289 0.132 Uiso 1 1 calc R . . H55B H 0.6498 -0.3225 0.5162 0.132 Uiso 1 1 calc R . . C56 C 0.7160(8) -0.1818(9) 0.5302(5) 0.131(5) Uani 1 1 d . . . H56A H 0.6722 -0.1854 0.5838 0.157 Uiso 1 1 calc R . . H56B H 0.7883 -0.2192 0.5422 0.157 Uiso 1 1 calc R . . O57 O 0.7302(3) -0.0782(4) 0.4834(2) 0.0598(15) Uani 1 1 d . . . C58 C 0.2003(5) 0.0065(8) 0.4790(4) 0.080(3) Uani 1 1 d . . . H58A H 0.1675 -0.0602 0.5247 0.096 Uiso 1 1 calc R . . H58B H 0.1390 0.0541 0.4524 0.096 Uiso 1 1 calc R . . C59 C 0.2686(8) -0.0325(8) 0.4175(6) 0.125(4) Uani 1 1 d . . . H59A H 0.2214 -0.0540 0.3817 0.150 Uiso 1 1 calc R . . H59B H 0.3193 0.0289 0.3814 0.150 Uiso 1 1 calc R . . C60 C 0.9589(4) 0.6579(5) -0.0433(3) 0.0340(14) Uani 1 1 d . . . H60 H 0.9255 0.5985 -0.0555 0.041 Uiso 1 1 calc R . . C61 C 1.0608(5) 0.7011(6) -0.0854(3) 0.0444(17) Uani 1 1 d . . . H61 H 1.0978 0.6700 -0.1253 0.053 Uiso 1 1 calc R . . C62 C 1.1085(5) 0.7899(5) -0.0690(3) 0.0440(17) Uani 1 1 d . . . H62 H 1.1771 0.8209 -0.0989 0.053 Uiso 1 1 calc R . . C63 C 1.0562(5) 0.8333(5) -0.0092(3) 0.0434(16) Uani 1 1 d . . . H63 H 1.0902 0.8920 0.0035 0.052 Uiso 1 1 calc R . . C64 C 0.9545(5) 0.7909(5) 0.0319(3) 0.0409(16) Uani 1 1 d . . . H64 H 0.9174 0.8234 0.0710 0.049 Uiso 1 1 calc R . . C65 C 0.9051(4) 0.7017(5) 0.0173(3) 0.0323(14) Uani 1 1 d . . . C66 C 0.7998(5) 0.6545(5) 0.0663(3) 0.0380(15) Uani 1 1 d . . . O67 O 0.7556(3) 0.6867(4) 0.1226(2) 0.0517(12) Uani 1 1 d . . . O68 O 0.7582(3) 0.5720(3) 0.0446(2) 0.0425(11) Uani 1 1 d . . . C69 C 0.6472(5) 0.5219(6) 0.0893(3) 0.0537(18) Uani 1 1 d . . . C70A C 0.5639(7) 0.6028(8) 0.0484(5) 0.019(2) Uiso 0.50 1 d P . . H70A H 0.5731 0.6761 0.0566 0.028 Uiso 0.50 1 calc PR . . H70B H 0.4899 0.5728 0.0728 0.028 Uiso 0.50 1 calc PR . . H70C H 0.5731 0.6135 -0.0115 0.028 Uiso 0.50 1 calc PR . . C70B C 0.6405(7) 0.4136(8) 0.0802(5) 0.016(2) Uiso 0.50 1 d P . . H70D H 0.6984 0.3638 0.1083 0.025 Uiso 0.50 1 calc PR . . H70E H 0.6504 0.4216 0.0207 0.025 Uiso 0.50 1 calc PR . . H70F H 0.5678 0.3801 0.1053 0.025 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.018(2) 0.021(3) 0.021(2) -0.0071(19) -0.0038(18) 0.002(2) N2 0.017(2) 0.020(3) 0.022(2) -0.0068(19) -0.0026(18) 0.002(2) N3 0.017(2) 0.021(3) 0.024(2) -0.0088(19) 0.0001(18) 0.004(2) N4 0.018(2) 0.018(3) 0.027(2) -0.0078(19) -0.0047(18) 0.0000(19) C5 0.021(3) 0.021(3) 0.025(3) -0.006(2) -0.006(2) 0.002(2) C6 0.023(3) 0.012(3) 0.024(3) -0.003(2) -0.004(2) -0.006(2) C7 0.020(3) 0.022(3) 0.028(3) -0.009(2) -0.006(2) 0.005(2) C8 0.022(3) 0.026(3) 0.034(3) -0.014(3) -0.006(2) 0.004(3) C9 0.019(3) 0.020(3) 0.030(3) -0.005(2) -0.007(2) 0.006(2) C10 0.020(3) 0.025(3) 0.018(2) -0.007(2) -0.002(2) 0.000(2) C11 0.019(3) 0.028(3) 0.021(3) -0.013(2) 0.002(2) -0.004(2) C12 0.018(3) 0.021(3) 0.019(3) -0.006(2) -0.001(2) 0.003(2) C13 0.023(3) 0.017(3) 0.029(3) -0.005(2) -0.005(2) 0.004(2) C14 0.024(3) 0.024(3) 0.026(3) -0.009(2) -0.006(2) 0.001(2) C15 0.022(3) 0.021(3) 0.017(2) -0.006(2) 0.000(2) 0.000(2) C16 0.023(3) 0.024(3) 0.017(2) -0.002(2) -0.004(2) 0.003(2) C17 0.019(3) 0.020(3) 0.021(3) 0.001(2) 0.000(2) -0.002(2) C18 0.024(3) 0.024(3) 0.033(3) -0.009(3) -0.009(2) -0.002(3) C19 0.023(3) 0.022(3) 0.031(3) -0.007(2) -0.008(2) 0.002(3) C20 0.026(3) 0.022(3) 0.024(3) -0.010(2) -0.006(2) 0.008(3) C21 0.023(3) 0.022(3) 0.018(2) -0.004(2) -0.002(2) 0.001(2) C22 0.021(3) 0.023(3) 0.018(3) -0.006(2) -0.003(2) 0.001(2) C23 0.025(3) 0.028(4) 0.033(3) -0.014(3) -0.004(2) 0.003(3) C24 0.030(3) 0.025(3) 0.032(3) -0.016(3) -0.007(2) 0.001(3) C25 0.014(3) 0.025(3) 0.033(3) -0.012(3) -0.003(2) 0.002(2) C26 0.025(3) 0.022(3) 0.034(3) -0.012(3) -0.007(2) 0.004(3) C27 0.025(3) 0.019(3) 0.038(3) -0.011(2) -0.004(2) -0.001(2) C28 0.019(3) 0.030(4) 0.034(3) -0.017(3) -0.008(2) 0.001(3) C29 0.031(3) 0.033(4) 0.029(3) -0.008(3) -0.009(2) 0.007(3) C30 0.029(3) 0.029(3) 0.031(3) -0.012(3) -0.009(2) 0.000(3) C31 0.022(3) 0.019(3) 0.027(3) -0.008(2) -0.011(2) 0.000(2) C32 0.025(3) 0.023(3) 0.025(3) -0.010(2) -0.001(2) -0.002(2) C33 0.024(3) 0.028(3) 0.031(3) -0.006(2) -0.012(2) 0.000(3) C34 0.025(3) 0.023(3) 0.035(3) -0.015(2) -0.013(2) 0.011(3) C35 0.026(3) 0.033(4) 0.032(3) -0.013(3) -0.003(2) 0.004(3) C36 0.023(3) 0.026(3) 0.022(3) -0.005(2) -0.004(2) 0.003(3) C37 0.018(3) 0.025(3) 0.030(3) -0.015(2) 0.001(2) 0.000(2) C38 0.027(3) 0.026(3) 0.025(3) -0.010(2) -0.004(2) 0.003(3) C39 0.037(3) 0.024(3) 0.034(3) -0.013(3) -0.004(3) -0.002(3) C40 0.029(3) 0.035(4) 0.027(3) -0.013(3) -0.005(2) -0.006(3) C41 0.021(3) 0.037(4) 0.020(3) -0.008(3) -0.005(2) -0.006(3) C42 0.022(3) 0.025(3) 0.028(3) -0.009(2) -0.006(2) 0.000(2) C43 0.022(3) 0.014(3) 0.028(3) -0.012(2) -0.002(2) 0.000(2) C44 0.024(3) 0.026(3) 0.031(3) -0.009(2) -0.003(2) 0.001(3) C45 0.026(3) 0.019(3) 0.041(3) -0.006(3) -0.010(3) -0.001(3) C46 0.025(3) 0.028(4) 0.052(4) -0.018(3) -0.006(3) 0.005(3) C47 0.027(3) 0.033(4) 0.038(3) -0.018(3) -0.003(2) 0.000(3) C48 0.036(3) 0.021(3) 0.034(3) -0.011(3) -0.010(3) 0.005(3) Zn49 0.0198(3) 0.0201(4) 0.0245(3) -0.0085(3) -0.0036(2) 0.0013(3) O50 0.029(2) 0.028(2) 0.025(2) -0.0087(19) -0.0030(17) 0.0035(19) O51 0.089(4) 0.046(3) 0.062(3) 0.004(3) -0.037(3) -0.021(3) C52 0.087(6) 0.107(7) 0.029(4) -0.031(4) 0.011(4) -0.057(5) C53 0.111(8) 0.136(10) 0.085(7) -0.066(7) 0.018(6) 0.004(7) O54 0.094(4) 0.071(4) 0.097(4) -0.063(3) 0.024(3) -0.031(3) C55 0.097(8) 0.024(5) 0.162(10) -0.008(5) 0.090(7) 0.015(5) C56 0.116(9) 0.113(10) 0.080(7) 0.050(6) 0.050(6) 0.083(8) O57 0.054(3) 0.086(4) 0.034(2) -0.014(3) -0.013(2) 0.037(3) C58 0.032(4) 0.176(10) 0.044(4) -0.054(5) -0.014(3) 0.040(5) C59 0.155(9) 0.085(7) 0.126(8) 0.014(6) -0.101(8) -0.058(7) C60 0.043(4) 0.030(4) 0.032(3) -0.013(3) -0.009(3) 0.003(3) C61 0.037(4) 0.060(5) 0.033(3) -0.012(3) -0.007(3) 0.010(4) C62 0.051(4) 0.043(5) 0.030(3) 0.003(3) -0.013(3) -0.008(3) C63 0.051(4) 0.037(4) 0.041(4) -0.006(3) -0.016(3) -0.005(3) C64 0.052(4) 0.035(4) 0.042(3) -0.017(3) -0.022(3) 0.008(3) C65 0.037(3) 0.027(4) 0.027(3) 0.000(3) -0.012(3) 0.004(3) C66 0.051(4) 0.038(4) 0.027(3) -0.012(3) -0.009(3) 0.005(3) O67 0.062(3) 0.055(3) 0.045(2) -0.029(2) 0.007(2) -0.006(2) O68 0.055(3) 0.042(3) 0.035(2) -0.020(2) -0.002(2) -0.006(2) C69 0.059(4) 0.056(5) 0.042(4) -0.017(3) 0.023(3) -0.032(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 Zn49 N2 2.063(4) . ? Zn49 N1 2.066(4) . ? Zn49 N4 2.070(4) . ? Zn49 N3 2.072(4) . ? Zn49 O50 2.130(4) . ? N1 C7 1.367(6) . ? N1 C10 1.380(5) . ? N2 C12 1.385(5) . ? N2 C15 1.392(6) . ? N3 C20 1.375(5) . ? N3 C17 1.387(6) . ? N4 C5 1.371(6) . ? N4 C22 1.399(5) . ? C5 C6 1.402(6) . ? C5 C24 1.449(6) . ? C6 C7 1.414(6) . ? C6 C25 1.503(7) . ? C7 C8 1.457(6) . ? C8 C9 1.347(6) . ? C9 C10 1.444(7) . ? C10 C11 1.392(7) . ? C11 C12 1.405(6) . ? C11 C43 1.500(6) . ? C12 C13 1.432(7) . ? C13 C14 1.359(6) . ? C14 C15 1.439(6) . ? C15 C16 1.401(6) . ? C16 C17 1.419(6) . ? C16 C37 1.497(7) . ? C17 C18 1.447(6) . ? C18 C19 1.331(6) . ? C19 C20 1.458(7) . ? C20 C21 1.394(7) . ? C21 C22 1.409(6) . ? C21 C31 1.529(6) . ? C22 C23 1.440(7) . ? C23 C24 1.351(6) . ? C25 C26 1.383(7) . ? C25 C30 1.400(6) . ? C26 C27 1.389(7) . ? C27 C28 1.395(6) . ? C28 C29 1.379(7) . ? C29 C30 1.379(7) . ? C31 C36 1.379(6) . ? C31 C32 1.398(6) . ? C32 C33 1.386(6) . ? C33 C34 1.376(6) . ? C34 C35 1.367(6) . ? C35 C36 1.387(6) . ? C37 C38 1.398(7) . ? C37 C42 1.412(6) . ? C38 C39 1.364(7) . ? C39 C40 1.387(6) . ? C40 C41 1.366(7) . ? C41 C42 1.389(7) . ? C43 C48 1.394(6) . ? C43 C44 1.405(6) . ? C44 C45 1.382(6) . ? C45 C46 1.396(7) . ? C46 C47 1.380(6) . ? C47 C48 1.382(6) . ? O51 C59 1.328(9) . ? O51 C52 1.541(7) . ? C52 C53 1.444(10) . ? C53 O54 1.335(10) . ? O54 C55 1.477(9) . ? C55 C56 1.492(13) . ? C56 O57 1.276(10) . ? O57 C58 1.581(9) 2_656 ? C58 C59 1.456(11) . ? C58 O57 1.581(9) 2_656 ? C60 C61 1.389(8) . ? C60 C65 1.405(7) . ? C61 C62 1.391(8) . ? C62 C63 1.384(8) . ? C63 C64 1.380(8) . ? C64 C65 1.390(8) . ? C65 C66 1.472(8) . ? C66 O67 1.219(6) . ? C66 O68 1.337(7) . ? O68 C69 1.517(7) . ? C69 C70B 1.413(11) . ? C69 C70A 1.466(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 N2 Zn49 N1 88.79(15) . . ? N2 Zn49 N4 164.55(14) . . ? N1 Zn49 N4 88.96(15) . . ? N2 Zn49 N3 88.72(15) . . ? N1 Zn49 N3 161.74(14) . . ? N4 Zn49 N3 88.64(15) . . ? N2 Zn49 O50 99.79(15) . . ? N1 Zn49 O50 94.33(14) . . ? N4 Zn49 O50 95.62(15) . . ? N3 Zn49 O50 103.92(14) . . ? C7 N1 C10 107.0(4) . . ? C7 N1 Zn49 126.2(3) . . ? C10 N1 Zn49 126.5(3) . . ? C12 N2 C15 105.7(4) . . ? C12 N2 Zn49 126.8(3) . . ? C15 N2 Zn49 127.0(3) . . ? C20 N3 C17 106.1(4) . . ? C20 N3 Zn49 126.3(3) . . ? C17 N3 Zn49 126.5(3) . . ? C5 N4 C22 106.1(4) . . ? C5 N4 Zn49 126.4(3) . . ? C22 N4 Zn49 126.8(3) . . ? N4 C5 C6 125.0(4) . . ? N4 C5 C24 110.1(4) . . ? C6 C5 C24 124.9(5) . . ? C5 C6 C7 125.5(5) . . ? C5 C6 C25 117.2(4) . . ? C7 C6 C25 117.3(4) . . ? N1 C7 C6 125.9(4) . . ? N1 C7 C8 109.7(4) . . ? C6 C7 C8 124.4(5) . . ? C9 C8 C7 106.3(5) . . ? C8 C9 C10 108.3(4) . . ? N1 C10 C11 125.2(4) . . ? N1 C10 C9 108.7(4) . . ? C11 C10 C9 126.1(4) . . ? C10 C11 C12 126.7(4) . . ? C10 C11 C43 117.0(4) . . ? C12 C11 C43 116.3(4) . . ? N2 C12 C11 124.1(5) . . ? N2 C12 C13 109.8(4) . . ? C11 C12 C13 126.0(4) . . ? C14 C13 C12 107.8(4) . . ? C13 C14 C15 106.8(5) . . ? N2 C15 C16 125.3(4) . . ? N2 C15 C14 109.8(4) . . ? C16 C15 C14 124.8(5) . . ? C15 C16 C17 125.4(5) . . ? C15 C16 C37 117.5(4) . . ? C17 C16 C37 117.0(4) . . ? N3 C17 C16 125.1(4) . . ? N3 C17 C18 109.4(4) . . ? C16 C17 C18 125.5(5) . . ? C19 C18 C17 107.6(5) . . ? C18 C19 C20 107.5(4) . . ? N3 C20 C21 125.8(4) . . ? N3 C20 C19 109.4(4) . . ? C21 C20 C19 124.8(4) . . ? C20 C21 C22 126.4(4) . . ? C20 C21 C31 117.4(4) . . ? C22 C21 C31 116.3(4) . . ? N4 C22 C21 124.0(5) . . ? N4 C22 C23 109.1(4) . . ? C21 C22 C23 126.9(4) . . ? C24 C23 C22 107.8(4) . . ? C23 C24 C5 106.9(5) . . ? C26 C25 C30 118.7(5) . . ? C26 C25 C6 122.4(4) . . ? C30 C25 C6 118.9(5) . . ? C25 C26 C27 121.3(5) . . ? C26 C27 C28 119.1(5) . . ? C29 C28 C27 120.0(5) . . ? C28 C29 C30 120.5(5) . . ? C29 C30 C25 120.4(5) . . ? C36 C31 C32 119.2(4) . . ? C36 C31 C21 122.5(4) . . ? C32 C31 C21 118.4(4) . . ? C33 C32 C31 120.4(5) . . ? C34 C33 C32 120.0(4) . . ? C35 C34 C33 119.4(4) . . ? C34 C35 C36 121.7(5) . . ? C31 C36 C35 119.4(4) . . ? C38 C37 C42 116.9(5) . . ? C38 C37 C16 122.8(4) . . ? C42 C37 C16 120.3(5) . . ? C39 C38 C37 122.0(4) . . ? C38 C39 C40 119.8(5) . . ? C41 C40 C39 120.4(5) . . ? C40 C41 C42 120.0(4) . . ? C41 C42 C37 120.8(5) . . ? C48 C43 C44 117.5(4) . . ? C48 C43 C11 123.3(4) . . ? C44 C43 C11 119.3(4) . . ? C45 C44 C43 120.7(5) . . ? C44 C45 C46 120.6(4) . . ? C47 C46 C45 119.3(4) . . ? C46 C47 C48 120.0(5) . . ? C47 C48 C43 122.0(4) . . ? C59 O51 C52 109.2(6) . . ? C53 C52 O51 109.5(5) . . ? O54 C53 C52 107.4(8) . . ? C53 O54 C55 111.6(7) . . ? O54 C55 C56 108.6(7) . . ? O57 C56 C55 107.3(8) . . ? C56 O57 C58 113.5(7) . 2_656 ? C59 C58 O57 111.5(6) . 2_656 ? O51 C59 C58 107.6(7) . . ? C61 C60 C65 120.2(6) . . ? C60 C61 C62 119.9(6) . . ? C63 C62 C61 120.2(6) . . ? C64 C63 C62 119.7(6) . . ? C63 C64 C65 121.3(6) . . ? C64 C65 C60 118.5(6) . . ? C64 C65 C66 119.5(5) . . ? C60 C65 C66 122.0(6) . . ? O67 C66 O68 123.1(6) . . ? O67 C66 C65 122.7(6) . . ? O68 C66 C65 114.2(5) . . ? C66 O68 C69 117.8(4) . . ? C70B C69 C70A 113.4(7) . . ? C70B C69 O68 106.8(6) . . ? C70A C69 O68 105.7(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Zn49 N1 C7 175.6(4) . . . . ? N4 Zn49 N1 C7 10.9(4) . . . . ? N3 Zn49 N1 C7 93.4(6) . . . . ? O50 Zn49 N1 C7 -84.6(4) . . . . ? N2 Zn49 N1 C10 -12.0(4) . . . . ? N4 Zn49 N1 C10 -176.8(4) . . . . ? N3 Zn49 N1 C10 -94.3(6) . . . . ? O50 Zn49 N1 C10 87.7(4) . . . . ? N1 Zn49 N2 C12 14.5(4) . . . . ? N4 Zn49 N2 C12 96.2(6) . . . . ? N3 Zn49 N2 C12 176.4(4) . . . . ? O50 Zn49 N2 C12 -79.7(4) . . . . ? N1 Zn49 N2 C15 -174.8(4) . . . . ? N4 Zn49 N2 C15 -93.1(7) . . . . ? N3 Zn49 N2 C15 -12.9(4) . . . . ? O50 Zn49 N2 C15 91.0(4) . . . . ? N2 Zn49 N3 C20 -179.5(4) . . . . ? N1 Zn49 N3 C20 -97.2(6) . . . . ? N4 Zn49 N3 C20 -14.7(4) . . . . ? O50 Zn49 N3 C20 80.8(4) . . . . ? N2 Zn49 N3 C17 14.7(4) . . . . ? N1 Zn49 N3 C17 96.9(6) . . . . ? N4 Zn49 N3 C17 179.5(4) . . . . ? O50 Zn49 N3 C17 -85.1(4) . . . . ? N2 Zn49 N4 C5 -97.2(6) . . . . ? N1 Zn49 N4 C5 -15.6(4) . . . . ? N3 Zn49 N4 C5 -177.5(4) . . . . ? O50 Zn49 N4 C5 78.7(4) . . . . ? N2 Zn49 N4 C22 94.1(7) . . . . ? N1 Zn49 N4 C22 175.8(4) . . . . ? N3 Zn49 N4 C22 13.9(4) . . . . ? O50 Zn49 N4 C22 -89.9(4) . . . . ? C22 N4 C5 C6 -176.5(4) . . . . ? Zn49 N4 C5 C6 13.0(7) . . . . ? C22 N4 C5 C24 1.0(5) . . . . ? Zn49 N4 C5 C24 -169.5(3) . . . . ? N4 C5 C6 C7 0.4(8) . . . . ? C24 C5 C6 C7 -176.8(5) . . . . ? N4 C5 C6 C25 -177.2(4) . . . . ? C24 C5 C6 C25 5.7(7) . . . . ? C10 N1 C7 C6 -176.8(4) . . . . ? Zn49 N1 C7 C6 -3.3(7) . . . . ? C10 N1 C7 C8 2.6(5) . . . . ? Zn49 N1 C7 C8 176.2(3) . . . . ? C5 C6 C7 N1 -5.6(8) . . . . ? C25 C6 C7 N1 172.0(4) . . . . ? C5 C6 C7 C8 175.0(5) . . . . ? C25 C6 C7 C8 -7.4(7) . . . . ? N1 C7 C8 C9 -1.6(5) . . . . ? C6 C7 C8 C9 177.8(4) . . . . ? C7 C8 C9 C10 0.0(5) . . . . ? C7 N1 C10 C11 179.0(4) . . . . ? Zn49 N1 C10 C11 5.5(6) . . . . ? C7 N1 C10 C9 -2.6(5) . . . . ? Zn49 N1 C10 C9 -176.1(3) . . . . ? C8 C9 C10 N1 1.6(5) . . . . ? C8 C9 C10 C11 180.0(4) . . . . ? N1 C10 C11 C12 4.7(8) . . . . ? C9 C10 C11 C12 -173.4(5) . . . . ? N1 C10 C11 C43 -173.9(4) . . . . ? C9 C10 C11 C43 8.0(7) . . . . ? C15 N2 C12 C11 177.2(4) . . . . ? Zn49 N2 C12 C11 -10.6(6) . . . . ? C15 N2 C12 C13 -0.4(5) . . . . ? Zn49 N2 C12 C13 171.9(3) . . . . ? C10 C11 C12 N2 -2.0(8) . . . . ? C43 C11 C12 N2 176.6(4) . . . . ? C10 C11 C12 C13 175.2(5) . . . . ? C43 C11 C12 C13 -6.3(7) . . . . ? N2 C12 C13 C14 1.0(5) . . . . ? C11 C12 C13 C14 -176.5(5) . . . . ? C12 C13 C14 C15 -1.1(5) . . . . ? C12 N2 C15 C16 -178.5(4) . . . . ? Zn49 N2 C15 C16 9.2(7) . . . . ? C12 N2 C15 C14 -0.3(5) . . . . ? Zn49 N2 C15 C14 -172.6(3) . . . . ? C13 C14 C15 N2 0.9(5) . . . . ? C13 C14 C15 C16 179.1(4) . . . . ? N2 C15 C16 C17 -1.6(8) . . . . ? C14 C15 C16 C17 -179.6(5) . . . . ? N2 C15 C16 C37 177.5(4) . . . . ? C14 C15 C16 C37 -0.4(7) . . . . ? C20 N3 C17 C16 178.8(4) . . . . ? Zn49 N3 C17 C16 -13.1(6) . . . . ? C20 N3 C17 C18 -1.7(5) . . . . ? Zn49 N3 C17 C18 166.4(3) . . . . ? C15 C16 C17 N3 3.7(8) . . . . ? C37 C16 C17 N3 -175.4(4) . . . . ? C15 C16 C17 C18 -175.7(4) . . . . ? C37 C16 C17 C18 5.2(7) . . . . ? N3 C17 C18 C19 0.7(5) . . . . ? C16 C17 C18 C19 -179.8(4) . . . . ? C17 C18 C19 C20 0.6(5) . . . . ? C17 N3 C20 C21 -179.1(4) . . . . ? Zn49 N3 C20 C21 12.7(7) . . . . ? C17 N3 C20 C19 2.1(5) . . . . ? Zn49 N3 C20 C19 -166.1(3) . . . . ? C18 C19 C20 N3 -1.7(6) . . . . ? C18 C19 C20 C21 179.4(5) . . . . ? N3 C20 C21 C22 -3.9(8) . . . . ? C19 C20 C21 C22 174.8(5) . . . . ? N3 C20 C21 C31 175.3(4) . . . . ? C19 C20 C21 C31 -6.1(7) . . . . ? C5 N4 C22 C21 178.6(4) . . . . ? Zn49 N4 C22 C21 -10.9(6) . . . . ? C5 N4 C22 C23 0.0(5) . . . . ? Zn49 N4 C22 C23 170.5(3) . . . . ? C20 C21 C22 N4 2.9(7) . . . . ? C31 C21 C22 N4 -176.3(4) . . . . ? C20 C21 C22 C23 -178.8(5) . . . . ? C31 C21 C22 C23 2.0(7) . . . . ? N4 C22 C23 C24 -1.1(5) . . . . ? C21 C22 C23 C24 -179.6(5) . . . . ? C22 C23 C24 C5 1.6(5) . . . . ? N4 C5 C24 C23 -1.7(6) . . . . ? C6 C5 C24 C23 175.8(5) . . . . ? C5 C6 C25 C26 -68.0(6) . . . . ? C7 C6 C25 C26 114.3(5) . . . . ? C5 C6 C25 C30 109.8(5) . . . . ? C7 C6 C25 C30 -68.0(6) . . . . ? C30 C25 C26 C27 1.7(7) . . . . ? C6 C25 C26 C27 179.4(4) . . . . ? C25 C26 C27 C28 -1.8(7) . . . . ? C26 C27 C28 C29 1.0(7) . . . . ? C27 C28 C29 C30 0.0(7) . . . . ? C28 C29 C30 C25 -0.1(7) . . . . ? C26 C25 C30 C29 -0.7(7) . . . . ? C6 C25 C30 C29 -178.5(4) . . . . ? C20 C21 C31 C36 117.7(5) . . . . ? C22 C21 C31 C36 -63.0(7) . . . . ? C20 C21 C31 C32 -61.7(6) . . . . ? C22 C21 C31 C32 117.6(5) . . . . ? C36 C31 C32 C33 0.2(8) . . . . ? C21 C31 C32 C33 179.6(5) . . . . ? C31 C32 C33 C34 -0.8(8) . . . . ? C32 C33 C34 C35 0.1(8) . . . . ? C33 C34 C35 C36 1.1(9) . . . . ? C32 C31 C36 C35 1.0(8) . . . . ? C21 C31 C36 C35 -178.3(5) . . . . ? C34 C35 C36 C31 -1.7(8) . . . . ? C15 C16 C37 C38 58.8(6) . . . . ? C17 C16 C37 C38 -122.0(5) . . . . ? C15 C16 C37 C42 -120.8(5) . . . . ? C17 C16 C37 C42 58.4(6) . . . . ? C42 C37 C38 C39 0.9(7) . . . . ? C16 C37 C38 C39 -178.7(5) . . . . ? C37 C38 C39 C40 -0.7(8) . . . . ? C38 C39 C40 C41 1.1(8) . . . . ? C39 C40 C41 C42 -1.7(7) . . . . ? C40 C41 C42 C37 1.9(7) . . . . ? C38 C37 C42 C41 -1.5(7) . . . . ? C16 C37 C42 C41 178.1(4) . . . . ? C10 C11 C43 C48 -114.0(6) . . . . ? C12 C11 C43 C48 67.3(7) . . . . ? C10 C11 C43 C44 67.5(6) . . . . ? C12 C11 C43 C44 -111.2(5) . . . . ? C48 C43 C44 C45 -0.1(8) . . . . ? C11 C43 C44 C45 178.5(5) . . . . ? C43 C44 C45 C46 -0.5(8) . . . . ? C44 C45 C46 C47 1.1(8) . . . . ? C45 C46 C47 C48 -0.9(8) . . . . ? C46 C47 C48 C43 0.3(9) . . . . ? C44 C43 C48 C47 0.3(8) . . . . ? C11 C43 C48 C47 -178.3(5) . . . . ? C59 O51 C52 C53 168.5(7) . . . . ? O51 C52 C53 O54 -64.3(8) . . . . ? C52 C53 O54 C55 -151.7(6) . . . . ? C53 O54 C55 C56 -175.4(8) . . . . ? O54 C55 C56 O57 -65.3(9) . . . . ? C55 C56 O57 C58 -176.4(6) . . . 2_656 ? C52 O51 C59 C58 -176.2(6) . . . . ? O57 C58 C59 O51 78.6(8) 2_656 . . . ? C65 C60 C61 C62 -1.6(7) . . . . ? C60 C61 C62 C63 1.8(8) . . . . ? C61 C62 C63 C64 -2.4(8) . . . . ? C62 C63 C64 C65 2.9(8) . . . . ? C63 C64 C65 C60 -2.6(7) . . . . ? C63 C64 C65 C66 176.2(4) . . . . ? C61 C60 C65 C64 2.0(7) . . . . ? C61 C60 C65 C66 -176.9(4) . . . . ? C64 C65 C66 O67 -3.5(7) . . . . ? C60 C65 C66 O67 175.3(5) . . . . ? C64 C65 C66 O68 177.6(4) . . . . ? C60 C65 C66 O68 -3.5(7) . . . . ? O67 C66 O68 C69 3.8(7) . . . . ? C65 C66 O68 C69 -177.4(4) . . . . ? C66 O68 C69 C70B -158.6(5) . . . . ? C66 O68 C69 C70A 80.3(6) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.796 _refine_diff_density_min -0.636 _refine_diff_density_rms 0.091 #====END=============================================== data_compound-3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C48 H27 N4 O8 Zn)-.(C12 H24 O6 Na)+.4(C H4 O)' _chemical_formula_sum 'C64 H67 N4 Na O18 Zn' _chemical_formula_weight 1268.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 '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' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Na' 'Na' 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'triclinic' _symmetry_space_group_name_H-M 'P1bar' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.0190(10) _cell_length_b 10.7470(10) _cell_length_c 16.2060(10) _cell_angle_alpha 83.0670(10) _cell_angle_beta 80.6480(10) _cell_angle_gamma 77.5660(10) _cell_volume 1507.6(2) _cell_formula_units_Z 1 _cell_measurement_temperature 120 _cell_measurement_reflns_used 6247 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 27.8 _exptl_crystal_description 'needles' _exptl_crystal_colour 'deep red-purple' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.397 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 664 _exptl_absorpt_coefficient_mu 0.492 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120 _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. Phi & Omega scans' _diffrn_detector_area_resol_mean '56 microns' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6247 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0768 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 27.82 _reflns_number_total 6247 _reflns_number_gt 4423 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement 'Denzo & Scalepack' _computing_data_reduction 'Denzo' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0823P)^2^+1.0725P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6247 _refine_ls_number_parameters 436 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0966 _refine_ls_R_factor_gt 0.0613 _refine_ls_wR_factor_ref 0.1671 _refine_ls_wR_factor_gt 0.1517 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.196 _refine_ls_shift/su_mean 0.080 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N -0.1216(3) 0.0997(2) 0.09684(15) 0.0192(5) Uani 1 1 d . . . N2 N 0.1628(3) 0.1121(2) -0.01374(15) 0.0172(5) Uani 1 1 d . . . C3 C -0.2908(3) -0.1054(3) 0.07270(18) 0.0182(6) Uani 1 1 d . . . C4 C -0.3381(3) -0.0154(3) 0.13252(18) 0.0191(6) Uani 1 1 d . . . C5 C -0.2598(3) 0.0814(3) 0.14173(18) 0.0206(6) Uani 1 1 d . . . C6 C -0.3156(4) 0.1785(3) 0.1994(2) 0.0270(7) Uani 1 1 d . . . H6 H -0.4070 0.1880 0.2363 0.032 Uiso 1 1 calc . . . C7 C -0.2100(4) 0.2535(3) 0.1900(2) 0.0255(7) Uani 1 1 d . . . H7 H -0.2148 0.3236 0.2196 0.031 Uiso 1 1 calc . . . C8 C -0.0888(3) 0.2044(3) 0.12572(18) 0.0198(6) Uani 1 1 d . . . C9 C 0.0414(3) 0.2580(3) 0.09603(18) 0.0179(6) Uani 1 1 d . . . C10 C 0.1578(3) 0.2145(3) 0.03083(17) 0.0165(6) Uani 1 1 d . . . C11 C 0.2874(3) 0.2732(3) -0.00124(18) 0.0204(6) Uani 1 1 d . . . H11 H 0.3104 0.3439 0.0182 0.025 Uiso 1 1 calc . . . C12 C 0.3695(3) 0.2064(3) -0.06491(18) 0.0212(6) Uani 1 1 d . . . H12 H 0.4594 0.2224 -0.0975 0.025 Uiso 1 1 calc . . . C13 C -0.4814(3) -0.0223(3) 0.19260(18) 0.0188(6) Uani 1 1 d . . . C14 C -0.4754(3) -0.0482(3) 0.27861(18) 0.0214(6) Uani 1 1 d . . . H14 H -0.3810 -0.0655 0.2982 0.026 Uiso 1 1 calc . . . C15 C -0.6087(3) -0.0483(3) 0.33539(18) 0.0230(6) Uani 1 1 d . . . H15 H -0.6028 -0.0645 0.3926 0.028 Uiso 1 1 calc . . . C16 C -0.7515(3) -0.0242(3) 0.30736(18) 0.0192(6) Uani 1 1 d . . . C17 C -0.7580(3) -0.0028(3) 0.22075(19) 0.0213(6) Uani 1 1 d . . . H17 H -0.8520 0.0102 0.2011 0.026 Uiso 1 1 calc . . . C18 C -0.6248(3) -0.0009(3) 0.16402(18) 0.0216(6) Uani 1 1 d . . . H18 H -0.6305 0.0146 0.1068 0.026 Uiso 1 1 calc . . . C19 C -0.8953(3) -0.0198(3) 0.3689(2) 0.0235(7) Uani 1 1 d . . . O20 O -0.8881(2) 0.0095(2) 0.44211(13) 0.0259(5) Uani 1 1 d . . . O21 O -1.0152(2) -0.0412(2) 0.34817(14) 0.0281(5) Uani 1 1 d . . . C22 C 0.0561(3) 0.3721(3) 0.13718(18) 0.0202(6) Uani 1 1 d . . . C23 C 0.1661(3) 0.3616(3) 0.1899(2) 0.0251(7) Uani 1 1 d . . . H23 H 0.2334 0.2840 0.1983 0.030 Uiso 1 1 calc . . . C24 C 0.1769(4) 0.4657(3) 0.2303(2) 0.0274(7) Uani 1 1 d . . . H24 H 0.2504 0.4575 0.2658 0.033 Uiso 1 1 calc . . . C25 C 0.0766(3) 0.5827(3) 0.2172(2) 0.0254(7) Uani 1 1 d . . . C26 C -0.0314(3) 0.5940(3) 0.1636(2) 0.0259(7) Uani 1 1 d . . . H26 H -0.0975 0.6721 0.1543 0.031 Uiso 1 1 calc . . . C27 C -0.0417(3) 0.4895(3) 0.12358(19) 0.0239(7) Uani 1 1 d . . . H27 H -0.1143 0.4981 0.0875 0.029 Uiso 1 1 calc . . . C28 C 0.0834(4) 0.6917(3) 0.2649(2) 0.0275(7) Uani 1 1 d . . . O29 O 0.1619(3) 0.6794(2) 0.32140(19) 0.0471(7) Uani 1 1 d . . . O30 O -0.0048(3) 0.8003(2) 0.24250(15) 0.0336(6) Uani 1 1 d . . . H30 H -0.010(5) 0.873(4) 0.278(3) 0.056 Uiso 1 1 d . . . Zn31 Zn 0.0172(4) -0.0160(3) 0.0041(3) 0.0151(4) Uani 0.50 1 d P . . O32 O 0.7930(3) 0.5517(3) 0.46339(18) 0.0493(7) Uani 1 1 d . . . C33 C 0.8997(4) 0.4716(5) 0.4091(3) 0.0535(11) Uani 1 1 d . . . H33A H 1.0033 0.4773 0.4150 0.064 Uiso 1 1 calc . . . H33B H 0.8841 0.4984 0.3513 0.064 Uiso 1 1 calc . . . C34 C 0.8781(5) 0.3398(4) 0.4309(3) 0.0510(11) Uani 1 1 d . . . H34A H 0.9542 0.2823 0.3964 0.061 Uiso 1 1 calc . . . H34B H 0.8898 0.3140 0.4893 0.061 Uiso 1 1 calc . . . O35 O 0.7269(3) 0.3340(2) 0.41678(16) 0.0421(6) Uani 1 1 d . . . C36 C 0.7072(5) 0.2050(4) 0.4230(2) 0.0452(10) Uani 1 1 d . . . H36A H 0.7364 0.1607 0.4755 0.054 Uiso 1 1 calc . . . H36B H 0.7721 0.1609 0.3773 0.054 Uiso 1 1 calc . . . C37 C 0.5443(5) 0.2047(4) 0.4192(3) 0.0487(10) Uani 1 1 d . . . H37A H 0.5121 0.2571 0.3697 0.058 Uiso 1 1 calc . . . H37B H 0.5321 0.1181 0.4154 0.058 Uiso 1 1 calc . . . O38 O 0.4532(3) 0.2530(2) 0.49171(15) 0.0396(6) Uani 1 1 d . . . C39 C 0.2980(5) 0.2414(4) 0.4935(3) 0.0531(11) Uani 1 1 d . . . H39A H 0.2894 0.1524 0.5051 0.064 Uiso 1 1 calc . . . H39B H 0.2644 0.2729 0.4396 0.064 Uiso 1 1 calc . . . C40 C 0.2024(5) 0.3170(5) 0.5597(3) 0.0518(11) Uani 1 1 d . . . H40A H 0.0977 0.3046 0.5660 0.062 Uiso 1 1 calc . . . H40B H 0.2410 0.2898 0.6128 0.062 Uiso 1 1 calc . . . Na41 Na 0.5000 0.5000 0.5000 0.0363(5) Uani 1 2 d S . . O42 O -0.1486(5) 0.1533(4) -0.0849(2) 0.0216(9) Uani 0.50 1 d P . . H42 H -0.095(8) 0.169(7) -0.144(5) 0.038 Uiso 0.50 1 d P . . C43 C -0.2545(8) 0.2661(7) -0.0553(4) 0.0343(16) Uani 0.50 1 d PG . . H43A H -0.3245 0.2309 -0.0125 0.020(16) Uiso 0.50 1 d PG . . H43B H -0.3109 0.3226 -0.0951 0.04(2) Uiso 0.50 1 d PG . . H43C H -0.1967 0.3129 -0.0302 0.04(2) Uiso 0.50 1 d PG . . O44 O 0.4367(3) 0.5477(3) 0.36440(15) 0.0408(6) Uani 1 1 d . . . H44 H 0.349(6) 0.596(5) 0.358(3) 0.064 Uiso 1 1 d . . . C45 C 0.5325(4) 0.5826(4) 0.2905(2) 0.0403(9) Uani 1 1 d . . . H45A H 0.4761 0.5976 0.2436 0.060 Uiso 1 1 calc R . . H45B H 0.6200 0.5147 0.2803 0.060 Uiso 1 1 calc R . . H45C H 0.5661 0.6591 0.2975 0.060 Uiso 1 1 calc R . . O46 O -0.4453(10) 0.4400(9) 0.0554(5) 0.057(2) Uani 0.50 1 d P . . C47 C -0.3470(12) 0.3801(10) -0.0191(6) 0.065(3) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.0172(12) 0.0180(14) 0.0241(13) -0.0003(10) -0.0026(10) -0.0082(10) N2 0.0144(12) 0.0152(13) 0.0223(12) -0.0008(9) -0.0024(10) -0.0044(9) C3 0.0140(14) 0.0201(16) 0.0214(15) -0.0002(11) -0.0030(11) -0.0061(11) C4 0.0164(14) 0.0208(16) 0.0193(14) 0.0001(11) -0.0003(11) -0.0046(11) C5 0.0189(15) 0.0206(17) 0.0209(15) -0.0017(11) 0.0018(12) -0.0044(11) C6 0.0231(16) 0.0253(18) 0.0315(17) -0.0071(13) 0.0081(13) -0.0091(13) C7 0.0244(16) 0.0180(17) 0.0344(18) -0.0093(12) 0.0031(13) -0.0069(12) C8 0.0198(15) 0.0157(16) 0.0237(15) -0.0033(11) -0.0011(12) -0.0039(11) C9 0.0194(15) 0.0123(15) 0.0227(15) -0.0031(11) -0.0038(11) -0.0032(11) C10 0.0169(14) 0.0126(15) 0.0203(14) -0.0009(10) -0.0050(11) -0.0024(10) C11 0.0226(15) 0.0151(16) 0.0263(15) -0.0024(11) -0.0059(12) -0.0076(11) C12 0.0185(15) 0.0206(17) 0.0254(15) 0.0014(11) -0.0018(12) -0.0087(12) C13 0.0169(14) 0.0138(16) 0.0259(15) -0.0017(11) -0.0006(11) -0.0056(11) C14 0.0161(14) 0.0239(17) 0.0248(16) -0.0020(12) -0.0027(12) -0.0058(11) C15 0.0226(16) 0.0261(18) 0.0211(15) -0.0019(12) -0.0005(12) -0.0089(12) C16 0.0168(14) 0.0155(16) 0.0256(15) -0.0026(11) 0.0013(12) -0.0064(11) C17 0.0159(14) 0.0164(16) 0.0304(16) 0.0022(11) -0.0036(12) -0.0025(11) C18 0.0226(15) 0.0182(16) 0.0236(15) 0.0013(11) -0.0032(12) -0.0048(12) C19 0.0227(16) 0.0154(17) 0.0314(17) -0.0070(12) 0.0027(13) -0.0040(12) O20 0.0246(11) 0.0325(13) 0.0235(11) -0.0062(9) -0.0011(9) -0.0114(9) O21 0.0166(11) 0.0333(14) 0.0380(13) -0.0204(10) 0.0036(9) -0.0089(9) C22 0.0163(14) 0.0173(16) 0.0278(16) -0.0048(11) 0.0007(12) -0.0067(11) C23 0.0227(16) 0.0125(17) 0.0409(19) -0.0064(13) -0.0070(14) -0.0011(11) C24 0.0224(16) 0.0220(18) 0.0402(19) -0.0065(13) -0.0105(14) -0.0031(12) C25 0.0192(15) 0.0198(18) 0.0385(18) -0.0064(13) 0.0013(13) -0.0082(12) C26 0.0229(16) 0.0147(17) 0.0400(19) -0.0039(13) -0.0031(14) -0.0037(12) C27 0.0209(16) 0.0214(18) 0.0306(17) -0.0007(12) -0.0052(13) -0.0070(12) C28 0.0224(16) 0.0187(19) 0.0418(19) -0.0100(13) 0.0030(14) -0.0068(13) O29 0.0325(14) 0.0333(16) 0.084(2) -0.0336(14) -0.0211(14) 0.0006(11) O30 0.0445(15) 0.0132(13) 0.0390(14) -0.0064(9) 0.0061(11) -0.0033(10) Zn31 0.0159(13) 0.0162(15) 0.0143(7) -0.0041(9) 0.0017(8) -0.0067(8) O32 0.0423(16) 0.0476(18) 0.0545(18) 0.0031(13) 0.0001(13) -0.0104(13) C33 0.027(2) 0.067(3) 0.057(3) 0.006(2) 0.0032(18) -0.0018(19) C34 0.034(2) 0.052(3) 0.059(3) 0.004(2) -0.0077(19) 0.0046(18) O35 0.0339(14) 0.0398(16) 0.0449(15) 0.0061(11) -0.0049(12) 0.0034(11) C36 0.045(2) 0.041(3) 0.039(2) -0.0002(17) -0.0010(17) 0.0069(17) C37 0.065(3) 0.036(2) 0.045(2) -0.0141(17) -0.011(2) -0.0008(19) O38 0.0384(15) 0.0452(16) 0.0378(14) -0.0061(11) -0.0045(11) -0.0132(12) C39 0.054(3) 0.057(3) 0.057(3) -0.012(2) -0.007(2) -0.028(2) C40 0.040(2) 0.066(3) 0.054(3) -0.001(2) -0.0064(19) -0.024(2) Na41 0.0368(11) 0.0476(12) 0.0242(10) -0.0012(8) -0.0100(8) -0.0042(9) O42 0.028(2) 0.023(2) 0.014(2) 0.0007(16) -0.0023(17) -0.0070(17) C43 0.025(4) 0.040(4) 0.034(4) 0.012(3) -0.006(3) -0.007(3) O44 0.0344(15) 0.0574(18) 0.0272(13) -0.0005(11) -0.0091(11) 0.0001(12) C45 0.041(2) 0.044(2) 0.036(2) -0.0018(16) -0.0051(16) -0.0092(17) O46 0.057(5) 0.077(6) 0.045(5) -0.001(4) -0.001(4) -0.038(5) C47 0.075(6) 0.071(7) 0.057(6) -0.011(5) 0.009(5) -0.040(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 N1 C8 1.374(4) . ? N1 C5 1.378(4) . ? N1 Zn31 1.965(5) 2 ? N1 Zn31 2.131(5) . ? N2 C3 1.369(4) 2 ? N2 C10 1.377(3) . ? N2 Zn31 2.064(5) . ? N2 Zn31 2.080(5) 2 ? C3 N2 1.369(4) 2 ? C3 C4 1.404(4) . ? C3 C12 1.446(4) 2 ? C4 C5 1.411(4) . ? C4 C13 1.496(4) . ? C5 C6 1.440(4) . ? C6 C7 1.354(4) . ? C7 C8 1.440(4) . ? C8 C9 1.408(4) . ? C9 C10 1.409(4) . ? C9 C22 1.503(4) . ? C10 C11 1.441(4) . ? C11 C12 1.353(4) . ? C12 C3 1.446(4) 2 ? C13 C14 1.396(4) . ? C13 C18 1.407(4) . ? C14 C15 1.391(4) . ? C15 C16 1.397(4) . ? C16 C17 1.403(4) . ? C16 C19 1.498(4) . ? C17 C18 1.392(4) . ? C19 O21 1.257(4) . ? C19 O20 1.279(4) . ? C22 C23 1.390(4) . ? C22 C27 1.391(4) . ? C23 C24 1.389(4) . ? C24 C25 1.398(4) . ? C25 C26 1.384(4) . ? C25 C28 1.496(4) . ? C26 C27 1.390(4) . ? C28 O29 1.225(4) . ? C28 O30 1.311(4) . ? Zn31 Zn31 0.433(4) 2 ? Zn31 N1 1.965(5) 2 ? Zn31 N2 2.080(5) 2 ? Zn31 O42 2.141(5) 2 ? O32 C33 1.411(5) . ? O32 C40 1.423(5) 2_666 ? O32 Na41 2.773(3) . ? C33 C34 1.465(6) . ? C34 O35 1.434(5) . ? O35 C36 1.425(5) . ? O35 Na41 2.702(3) . ? C36 C37 1.481(6) . ? C37 O38 1.405(5) . ? O38 C39 1.427(5) . ? O38 Na41 2.798(2) . ? C39 C40 1.471(6) . ? C40 O32 1.423(5) 2_666 ? Na41 O44 2.330(2) . ? Na41 O44 2.330(2) 2_666 ? Na41 O35 2.702(3) 2_666 ? Na41 O32 2.773(3) 2_666 ? Na41 O38 2.798(3) 2_666 ? O42 C43 1.451(8) . ? O42 Zn31 2.141(5) 2 ? C43 C47 1.455(11) . ? O44 C45 1.420(4) . ? O46 C47 1.501(13) . ? 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 C8 N1 C5 106.5(2) . . ? C8 N1 Zn31 126.6(2) . 2 ? C5 N1 Zn31 125.8(2) . 2 ? C8 N1 Zn31 126.9(2) . . ? C5 N1 Zn31 126.6(2) . . ? Zn31 N1 Zn31 11.22(14) 2 . ? C3 N2 C10 106.6(2) 2 . ? C3 N2 Zn31 124.5(2) 2 . ? C10 N2 Zn31 128.8(2) . . ? C3 N2 Zn31 128.8(2) 2 2 ? C10 N2 Zn31 123.6(2) . 2 ? Zn31 N2 Zn31 12.00(11) . 2 ? N2 C3 C4 125.4(2) 2 . ? N2 C3 C12 109.7(2) 2 2 ? C4 C3 C12 124.9(3) . 2 ? C3 C4 C5 125.2(3) . . ? C3 C4 C13 118.2(2) . . ? C5 C4 C13 116.6(2) . . ? N1 C5 C4 126.1(3) . . ? N1 C5 C6 109.5(2) . . ? C4 C5 C6 124.4(3) . . ? C7 C6 C5 107.2(3) . . ? C6 C7 C8 107.2(3) . . ? N1 C8 C9 125.6(3) . . ? N1 C8 C7 109.7(2) . . ? C9 C8 C7 124.8(3) . . ? C8 C9 C10 125.5(3) . . ? C8 C9 C22 116.9(2) . . ? C10 C9 C22 117.5(2) . . ? N2 C10 C9 125.4(2) . . ? N2 C10 C11 109.6(2) . . ? C9 C10 C11 125.0(3) . . ? C12 C11 C10 107.2(2) . . ? C11 C12 C3 107.0(2) . 2 ? C14 C13 C18 118.7(3) . . ? C14 C13 C4 120.3(3) . . ? C18 C13 C4 121.0(3) . . ? C15 C14 C13 120.8(3) . . ? C14 C15 C16 120.6(3) . . ? C15 C16 C17 118.9(3) . . ? C15 C16 C19 120.4(3) . . ? C17 C16 C19 120.7(3) . . ? C18 C17 C16 120.4(3) . . ? C17 C18 C13 120.5(3) . . ? O21 C19 O20 123.0(3) . . ? O21 C19 C16 121.2(3) . . ? O20 C19 C16 115.7(3) . . ? C23 C22 C27 119.0(3) . . ? C23 C22 C9 120.7(3) . . ? C27 C22 C9 120.3(3) . . ? C24 C23 C22 120.9(3) . . ? C23 C24 C25 119.6(3) . . ? C26 C25 C24 119.7(3) . . ? C26 C25 C28 121.3(3) . . ? C24 C25 C28 119.0(3) . . ? C25 C26 C27 120.4(3) . . ? C26 C27 C22 120.4(3) . . ? O29 C28 O30 123.0(3) . . ? O29 C28 C25 122.7(3) . . ? O30 C28 C25 114.3(3) . . ? Zn31 Zn31 N1 106.8(12) 2 2 ? Zn31 Zn31 N2 86.1(12) 2 . ? N1 Zn31 N2 91.95(19) 2 . ? Zn31 Zn31 N2 81.9(12) 2 2 ? N1 Zn31 N2 91.5(2) 2 2 ? N2 Zn31 N2 168.00(11) . 2 ? Zn31 Zn31 N1 61.9(11) 2 . ? N1 Zn31 N1 168.77(14) 2 . ? N2 Zn31 N1 87.40(19) . . ? N2 Zn31 N1 86.96(17) 2 . ? Zn31 Zn31 O42 160.4(13) 2 2 ? N1 Zn31 O42 92.62(16) 2 2 ? N2 Zn31 O42 95.51(19) . 2 ? N2 Zn31 O42 95.8(2) 2 2 ? N1 Zn31 O42 98.6(2) . 2 ? C33 O32 C40 111.5(3) . 2_666 ? C33 O32 Na41 116.5(2) . . ? C40 O32 Na41 114.4(2) 2_666 . ? O32 C33 C34 108.6(3) . . ? O35 C34 C33 108.2(3) . . ? C36 O35 C34 111.1(3) . . ? C36 O35 Na41 116.3(2) . . ? C34 O35 Na41 114.3(2) . . ? O35 C36 C37 109.0(3) . . ? O38 C37 C36 109.5(3) . . ? C37 O38 C39 110.4(3) . . ? C37 O38 Na41 108.0(2) . . ? C39 O38 Na41 116.0(2) . . ? O38 C39 C40 108.1(3) . . ? O32 C40 C39 108.4(3) 2_666 . ? O44 Na41 O44 180.00(3) . 2_666 ? O44 Na41 O35 79.85(9) . . ? O44 Na41 O35 100.15(9) 2_666 . ? O44 Na41 O35 100.15(9) . 2_666 ? O44 Na41 O35 79.85(9) 2_666 2_666 ? O35 Na41 O35 180.0 . 2_666 ? O44 Na41 O32 96.84(9) . . ? O44 Na41 O32 83.16(9) 2_666 . ? O35 Na41 O32 60.33(8) . . ? O35 Na41 O32 119.67(8) 2_666 . ? O44 Na41 O32 83.16(9) . 2_666 ? O44 Na41 O32 96.84(9) 2_666 2_666 ? O35 Na41 O32 119.67(8) . 2_666 ? O35 Na41 O32 60.33(8) 2_666 2_666 ? O32 Na41 O32 180.00(3) . 2_666 ? O44 Na41 O38 87.24(9) . . ? O44 Na41 O38 92.76(9) 2_666 . ? O35 Na41 O38 61.97(8) . . ? O35 Na41 O38 118.03(8) 2_666 . ? O32 Na41 O38 120.25(8) . . ? O32 Na41 O38 59.75(8) 2_666 . ? O44 Na41 O38 92.76(9) . 2_666 ? O44 Na41 O38 87.24(9) 2_666 2_666 ? O35 Na41 O38 118.03(8) . 2_666 ? O35 Na41 O38 61.97(8) 2_666 2_666 ? O32 Na41 O38 59.75(8) . 2_666 ? O32 Na41 O38 120.25(8) 2_666 2_666 ? O38 Na41 O38 180.0 . 2_666 ? C43 O42 Zn31 122.9(4) . 2 ? O42 C43 C47 173.0(6) . . ? C45 O44 Na41 127.4(2) . . ? C43 C47 O46 148.6(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 O32 C33 C34 O35 62.9(4) . . . . ? C33 C34 O35 C36 170.1(3) . . . . ? C34 O35 C36 C37 172.6(3) . . . . ? O35 C36 C37 O38 -67.4(4) . . . . ? C36 C37 O38 C39 -174.1(3) . . . . ? C37 O38 C39 C40 -168.1(3) . . . . ? O38 C39 C40 O32 65.0(4) . . . 2_666 ? C39 C40 O32 C33 171.3(3) . . 2_666 2_666 ? C40 O32 C33 C34 174.2(3) . 2_666 2_666 2_666 ? _diffrn_measured_fraction_theta_max 0.875 _diffrn_reflns_theta_full 27.82 _diffrn_measured_fraction_theta_full 0.875 _refine_diff_density_max 0.946 _refine_diff_density_min -0.623 _refine_diff_density_rms 0.097 #====END========================================= data_compound-4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C48 H27 N4 O8 Zn)-.(C12 H24 O6 K)+.4(C H4 O)' _chemical_formula_sum 'C64 H67 K N4 O18 Zn' _chemical_formula_weight 1284.69 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' 'K' 'K' 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'triclinic' _symmetry_space_group_name_H-M 'P1bar' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.4480(10) _cell_length_b 15.4120(10) _cell_length_c 16.3070(10) _cell_angle_alpha 100.549(10) _cell_angle_beta 90.827(10) _cell_angle_gamma 100.268(10) _cell_volume 3022.8(4) _cell_formula_units_Z 2 _cell_measurement_temperature 120 _cell_measurement_reflns_used 14874 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 28.7 _exptl_crystal_description 'needles' _exptl_crystal_colour 'dark red-purple' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.411 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1344 _exptl_absorpt_coefficient_mu 0.553 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120 _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. Phi & Omega scans' _diffrn_detector_area_resol_mean '56 microns' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14874 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1297 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 28.74 _reflns_number_total 14874 _reflns_number_gt 8122 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement 'Denzo & Scalepack' _computing_data_reduction 'Denzo' _computing_structure_solution 'SIR-92' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1219P)^2^+0.1263P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14874 _refine_ls_number_parameters 821 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1671 _refine_ls_R_factor_gt 0.0820 _refine_ls_wR_factor_ref 0.2395 _refine_ls_wR_factor_gt 0.1969 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.534 _refine_ls_shift/su_mean 0.119 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.2219(2) 0.1121(2) 0.98170(19) 0.0148(7) Uani 1 1 d . . . N2 N 0.3587(2) 0.2609(2) 1.0911(2) 0.0163(7) Uani 1 1 d . . . N3 N 0.2729(2) 0.3868(2) 1.0094(2) 0.0151(7) Uani 1 1 d . . . N4 N 0.1371(2) 0.2383(2) 0.89794(19) 0.0150(7) Uani 1 1 d . . . C5 C 0.0782(3) 0.1600(3) 0.8528(2) 0.0176(9) Uani 1 1 d . . . C6 C 0.0859(3) 0.0727(3) 0.8631(2) 0.0152(8) Uani 1 1 d . . . C7 C 0.1542(3) 0.0508(3) 0.9231(2) 0.0148(8) Uani 1 1 d . . . H8 H 0.1273 -0.0932 0.8962 0.030(13) Uiso 1 1 d R . . C8 C 0.1648(3) -0.0386(3) 0.9306(3) 0.0186(9) Uani 1 1 d . . . H9 H 0.2626 -0.0789 1.0149 0.028(12) Uiso 1 1 d R . . C9 C 0.2386(3) -0.0307(3) 0.9940(3) 0.0187(9) Uani 1 1 d . . . C10 C 0.2754(3) 0.0628(3) 1.0257(2) 0.0155(9) Uani 1 1 d . . . C11 C 0.3561(3) 0.0995(3) 1.0897(2) 0.0165(9) Uani 1 1 d . . . C12 C 0.3954(3) 0.1915(3) 1.1189(2) 0.0184(9) Uani 1 1 d . . . H13 H 0.5180 0.1937 1.2140 0.031(13) Uiso 1 1 d R . . C13 C 0.4804(3) 0.2279(3) 1.1828(3) 0.0219(10) Uani 1 1 d . . . H14 H 0.5509 0.3612 1.2288 0.046(15) Uiso 1 1 d R . . C14 C 0.4960(3) 0.3188(3) 1.1922(3) 0.0230(10) Uani 1 1 d . . . C15 C 0.4186(3) 0.3394(3) 1.1357(3) 0.0184(9) Uani 1 1 d . . . C16 C 0.4097(3) 0.4271(3) 1.1272(2) 0.0161(9) Uani 1 1 d . . . C17 C 0.3404(3) 0.4486(3) 1.0676(2) 0.0154(8) Uani 1 1 d . . . H18 H 0.3671 0.5933 1.0940 0.034(13) Uiso 1 1 d R . . C18 C 0.3287(3) 0.5378(3) 1.0602(3) 0.0194(9) Uani 1 1 d . . . H19 H 0.2297 0.5782 0.9779 0.023(12) Uiso 1 1 d R . . C19 C 0.2549(3) 0.5301(3) 0.9970(2) 0.0177(9) Uani 1 1 d . . . C20 C 0.2186(3) 0.4357(3) 0.9647(2) 0.0161(9) Uani 1 1 d . . . C21 C 0.1393(3) 0.3991(3) 0.8997(2) 0.0147(8) Uani 1 1 d . . . C22 C 0.1014(3) 0.3076(3) 0.8699(2) 0.0177(9) Uani 1 1 d . . . H23 H -0.0204 0.3053 0.7729 0.019(11) Uiso 1 1 d R . . C23 C 0.0172(3) 0.2707(3) 0.8049(3) 0.0222(10) Uani 1 1 d . . . H24 H -0.0501 0.1377 0.7565 0.034(13) Uiso 1 1 d R . . C24 C 0.0027(3) 0.1805(3) 0.7952(3) 0.0243(10) Uani 1 1 d . . . C25 C 0.0184(3) -0.0029(3) 0.8025(2) 0.0167(9) Uani 1 1 d . . . H26 H 0.0956 0.0265 0.6978 0.011(10) Uiso 1 1 d R . . C26 C 0.0366(3) -0.0140(3) 0.7173(3) 0.0195(9) Uani 1 1 d . . . H27 H -0.0153 -0.0877 0.6014 0.038(14) Uiso 1 1 d R . . C27 C -0.0287(3) -0.0805(3) 0.6606(3) 0.0207(9) Uani 1 1 d . . . C28 C -0.1128(3) -0.1395(3) 0.6872(2) 0.0165(9) Uani 1 1 d . . . H29 H -0.1851 -0.1736 0.7912 0.004(9) Uiso 1 1 d R . . C29 C -0.1296(3) -0.1311(3) 0.7724(3) 0.0175(9) Uani 1 1 d . . . H30 H -0.0809 -0.0562 0.8894 0.014(10) Uiso 1 1 d R . . C30 C -0.0661(3) -0.0636(3) 0.8298(2) 0.0179(9) Uani 1 1 d . . . C31 C -0.1859(3) -0.2100(3) 0.6243(3) 0.0183(9) Uani 1 1 d . . . O32 O -0.2009(2) -0.19209(19) 0.55321(17) 0.0215(7) Uani 1 1 d . . . O33 O -0.2320(2) -0.28275(19) 0.64514(17) 0.0204(6) Uani 1 1 d . . . C34 C 0.4069(3) 0.0346(3) 1.1294(2) 0.0190(9) Uani 1 1 d . . . H35 H 0.5581 0.0622 1.0792 0.034(13) Uiso 1 1 d R . . C35 C 0.5155(3) 0.0268(3) 1.1162(3) 0.0201(9) Uani 1 1 d . . . H36 H 0.6377 -0.0366 1.1450 0.018(10) Uiso 1 1 d R . . C36 C 0.5627(3) -0.0308(3) 1.1544(3) 0.0205(9) Uani 1 1 d . . . C37 C 0.5044(3) -0.0804(3) 1.2062(3) 0.0200(9) Uani 1 1 d . . . H38 H 0.3542 -0.1106 1.2539 0.007(10) Uiso 1 1 d R . . C38 C 0.3958(3) -0.0747(3) 1.2186(3) 0.0240(10) Uani 1 1 d . . . H39 H 0.2703 -0.0136 1.1902 0.017(11) Uiso 1 1 d R . . C39 C 0.3473(3) -0.0171(3) 1.1805(3) 0.0227(10) Uani 1 1 d . . . C40 C 0.5572(3) -0.1389(3) 1.2532(3) 0.0227(10) Uani 1 1 d . . . O41 O 0.6603(2) -0.1402(2) 1.23570(19) 0.0273(7) Uani 1 1 d . . . H41 H 0.6846 -0.1733 1.2623 0.041 Uiso 1 1 calc R . . O42 O 0.5112(2) -0.1786(2) 1.3037(2) 0.0365(9) Uani 1 1 d . . . C43 C 0.4774(3) 0.5027(3) 1.1869(2) 0.0167(9) Uani 1 1 d . . . H44 H 0.5708 0.5584 1.0979 0.012(10) Uiso 1 1 d R . . C44 C 0.5599(3) 0.5637(3) 1.1584(3) 0.0186(9) Uani 1 1 d . . . H45 H 0.6792 0.6759 1.1978 0.013(10) Uiso 1 1 d R . . C45 C 0.6254(3) 0.6312(3) 1.2159(3) 0.0182(9) Uani 1 1 d . . . C46 C 0.6123(3) 0.6373(3) 1.3013(2) 0.0168(9) Uani 1 1 d . . . H47 H 0.5187 0.5851 1.3880 0.040(14) Uiso 1 1 d R . . C47 C 0.5295(3) 0.5789(3) 1.3288(2) 0.0204(9) Uani 1 1 d . . . H48 H 0.4065 0.4710 1.2937 0.016(11) Uiso 1 1 d R . . C48 C 0.4622(3) 0.5122(3) 1.2734(3) 0.0192(9) Uani 1 1 d . . . C49 C 0.6883(3) 0.7084(3) 1.3614(3) 0.0185(9) Uani 1 1 d . . . O50 O 0.6940(2) 0.6885(2) 1.43622(18) 0.0248(7) Uani 1 1 d . . . H50 H 0.7352 0.7291 1.4672 0.037 Uiso 1 1 calc R . . O51 O 0.7406(2) 0.7757(2) 1.34184(18) 0.0224(7) Uani 1 1 d . . . C52 C 0.0918(3) 0.4639(3) 0.8585(2) 0.0165(9) Uani 1 1 d . . . H53 H -0.0604 0.4413 0.9084 0.039(14) Uiso 1 1 d R . . C53 C -0.0161(3) 0.4751(3) 0.8707(3) 0.0192(9) Uani 1 1 d . . . H54 H -0.1359 0.5394 0.8392 0.022(11) Uiso 1 1 d R . . C54 C -0.0616(3) 0.5315(3) 0.8301(3) 0.0206(9) Uani 1 1 d . . . C55 C -0.0014(3) 0.5785(3) 0.7762(2) 0.0194(9) Uani 1 1 d . . . H56 H 0.1497 0.6010 0.7260 0.027(12) Uiso 1 1 d R . . C56 C 0.1073(3) 0.5690(3) 0.7641(3) 0.0212(9) Uani 1 1 d . . . H57 H 0.2290 0.5074 0.7977 0.041(14) Uiso 1 1 d R . . C57 C 0.1522(3) 0.5125(3) 0.8057(3) 0.0222(10) Uani 1 1 d . . . C58 C -0.0509(3) 0.6371(3) 0.7276(3) 0.0183(9) Uani 1 1 d . . . O59 O -0.1461(2) 0.6531(2) 0.75232(17) 0.0224(7) Uani 1 1 d . . . H59 H -0.1737 0.6769 0.7184 0.034 Uiso 1 1 calc R . . O60 O -0.0056(2) 0.6655(2) 0.66910(19) 0.0270(7) Uani 1 1 d . . . Zn61 Zn 0.23409(4) 0.24953(3) 1.00365(3) 0.01629(16) Uani 1 1 d . . . K62 K 0.25723(9) -0.24780(8) 0.50112(7) 0.0477(3) Uani 1 1 d . . . O63 O 0.0563(2) -0.2797(2) 0.41795(19) 0.0312(8) Uani 1 1 d . . . C64 C -0.0143(4) -0.3568(4) 0.4347(3) 0.0369(12) Uani 1 1 d . . . H64A H -0.0821 -0.3674 0.4013 0.044 Uiso 1 1 calc . . . H64B H -0.0314 -0.3476 0.4932 0.044 Uiso 1 1 calc . . . C65 C 0.0409(4) -0.4355(4) 0.4141(3) 0.0397(13) Uani 1 1 d . . . H65A H -0.0085 -0.4896 0.4212 0.048 Uiso 1 1 calc . . . H65B H 0.0614 -0.4428 0.3564 0.048 Uiso 1 1 calc . . . O66 O 0.1357(3) -0.4214(2) 0.4681(2) 0.0373(8) Uani 1 1 d . . . C67 C 0.1993(4) -0.4895(3) 0.4456(3) 0.0382(12) Uani 1 1 d . . . H67A H 0.2323 -0.4843 0.3928 0.046 Uiso 1 1 calc . . . H67B H 0.1534 -0.5484 0.4397 0.046 Uiso 1 1 calc . . . C68 C 0.2845(5) -0.4782(4) 0.5116(3) 0.0439(14) Uani 1 1 d . . . H68A H 0.2516 -0.4781 0.5651 0.053 Uiso 1 1 calc . . . H68B H 0.3239 -0.5278 0.5010 0.053 Uiso 1 1 calc . . . O69 O 0.3578(3) -0.3960(2) 0.5135(2) 0.0335(8) Uani 1 1 d . . . C70 C 0.4272(4) -0.3727(4) 0.5873(3) 0.0467(15) Uani 1 1 d . . . H70A H 0.4650 -0.4215 0.5921 0.056 Uiso 1 1 calc . . . H70B H 0.3840 -0.3623 0.6359 0.056 Uiso 1 1 calc . . . C71 C 0.5072(4) -0.2909(4) 0.5834(3) 0.0407(14) Uani 1 1 d . . . H71A H 0.5625 -0.2806 0.6284 0.049 Uiso 1 1 calc . . . H71B H 0.5431 -0.2986 0.5308 0.049 Uiso 1 1 calc . . . O72 O 0.4537(2) -0.2156(2) 0.5904(2) 0.0367(9) Uani 1 1 d . . . C73 C 0.5255(4) -0.1368(4) 0.5788(4) 0.0495(15) Uani 1 1 d . . . H73A H 0.5471 -0.1433 0.5214 0.059 Uiso 1 1 calc . . . H73B H 0.5908 -0.1267 0.6150 0.059 Uiso 1 1 calc . . . C74 C 0.4678(4) -0.0597(4) 0.5990(4) 0.0465(14) Uani 1 1 d . . . H74A H 0.4422 -0.0555 0.6553 0.056 Uiso 1 1 calc . . . H74B H 0.5173 -0.0043 0.5960 0.056 Uiso 1 1 calc . . . O75 O 0.3769(3) -0.0729(2) 0.5403(2) 0.0398(9) Uani 1 1 d . . . C76 C 0.3119(4) -0.0055(4) 0.5617(3) 0.0428(13) Uani 1 1 d . . . H76A H 0.3574 0.0536 0.5683 0.051 Uiso 1 1 calc . . . H76B H 0.2779 -0.0111 0.6140 0.051 Uiso 1 1 calc . . . C77 C 0.2271(5) -0.0170(4) 0.4941(3) 0.0447(14) Uani 1 1 d . . . H77A H 0.1867 0.0320 0.5043 0.054 Uiso 1 1 calc . . . H77B H 0.2608 -0.0168 0.4408 0.054 Uiso 1 1 calc . . . O78 O 0.1554(3) -0.1001(2) 0.4923(2) 0.0325(8) Uani 1 1 d . . . C79 C 0.0847(4) -0.1227(4) 0.4196(3) 0.0387(13) Uani 1 1 d . . . H79A H 0.1266 -0.1341 0.3704 0.046 Uiso 1 1 calc . . . H79B H 0.0479 -0.0732 0.4151 0.046 Uiso 1 1 calc . . . C80 C 0.0033(4) -0.2038(4) 0.4251(3) 0.0354(12) Uani 1 1 d . . . H80A H -0.0313 -0.1951 0.4782 0.043 Uiso 1 1 calc . . . H80B H -0.0528 -0.2141 0.3807 0.043 Uiso 1 1 calc . . . O81 O 0.0991(2) 0.2523(2) 1.08471(18) 0.0277(7) Uani 1 1 d . . . H81 H 0.1176 0.2864 1.1446 0.040 Uiso 1 1 d . . . C82 C -0.0088(4) 0.2576(4) 1.0551(3) 0.0563(16) Uani 1 1 d . . . H82A H -0.0065 0.3132 1.0360 0.084 Uiso 1 1 calc R . . H82B H -0.0580 0.2548 1.0997 0.084 Uiso 1 1 calc R . . H82C H -0.0338 0.2083 1.0099 0.084 Uiso 1 1 calc R . . O83 O 0.2016(3) -0.2571(3) 0.6454(3) 0.0505(10) Uani 1 1 d . . . H83 H 0.1329 -0.2783 0.6496 0.073 Uiso 1 1 d . . . C84 C 0.2263(5) -0.1925(4) 0.7184(4) 0.0522(16) Uani 1 1 d . . . H84A H 0.2320 -0.2216 0.7651 0.078 Uiso 1 1 calc . . . H84B H 0.1693 -0.1576 0.7268 0.078 Uiso 1 1 calc . . . H84C H 0.2945 -0.1537 0.7135 0.078 Uiso 1 1 calc . . . O85 O 0.3084(3) -0.2438(3) 0.3549(3) 0.0579(11) Uani 1 1 d . . . H85 H 0.3799 -0.2215 0.3480 0.084 Uiso 1 1 d . . . C86 C 0.2697(5) -0.3104(4) 0.2845(4) 0.0545(16) Uani 1 1 d . . . H86A H 0.2626 -0.2826 0.2371 0.081 Uiso 1 1 calc . . . H86B H 0.1997 -0.3431 0.2951 0.081 Uiso 1 1 calc . . . H86C H 0.3203 -0.3508 0.2734 0.081 Uiso 1 1 calc . . . O87 O 0.6902(5) 0.2527(4) 1.0556(4) 0.0386(17) Uani 1 1 d . . . C88 C 0.6152(8) 0.2359(6) 0.9835(5) 0.032(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.0195(17) 0.0130(19) 0.0124(17) 0.0013(14) -0.0050(13) 0.0058(14) N2 0.0157(16) 0.0149(19) 0.0192(18) 0.0031(15) -0.0087(14) 0.0058(14) N3 0.0181(17) 0.0111(19) 0.0162(17) 0.0021(14) -0.0019(13) 0.0040(14) N4 0.0159(16) 0.0142(19) 0.0148(17) 0.0029(15) -0.0071(13) 0.0029(14) C5 0.019(2) 0.018(2) 0.013(2) -0.0026(17) -0.0036(16) 0.0027(17) C6 0.0136(19) 0.014(2) 0.016(2) -0.0014(17) -0.0025(15) 0.0012(16) C7 0.0166(19) 0.012(2) 0.016(2) 0.0019(17) 0.0010(16) 0.0029(16) C8 0.022(2) 0.008(2) 0.025(2) -0.0006(18) -0.0018(17) 0.0031(17) C9 0.022(2) 0.012(2) 0.022(2) 0.0020(18) -0.0032(17) 0.0043(17) C10 0.0170(19) 0.014(2) 0.018(2) 0.0056(18) -0.0018(16) 0.0050(16) C11 0.019(2) 0.015(2) 0.017(2) 0.0057(18) 0.0007(16) 0.0048(17) C12 0.023(2) 0.014(2) 0.019(2) 0.0022(18) -0.0035(17) 0.0054(17) C13 0.021(2) 0.018(2) 0.026(2) 0.0014(19) -0.0117(18) 0.0057(18) C14 0.026(2) 0.016(2) 0.025(2) 0.0011(19) -0.0102(18) 0.0023(18) C15 0.021(2) 0.012(2) 0.020(2) -0.0016(18) -0.0049(17) 0.0035(17) C16 0.0159(19) 0.012(2) 0.016(2) -0.0062(17) -0.0035(16) 0.0009(16) C17 0.0171(19) 0.010(2) 0.017(2) -0.0015(17) -0.0025(16) 0.0031(16) C18 0.021(2) 0.012(2) 0.023(2) -0.0012(18) -0.0031(17) 0.0029(17) C19 0.021(2) 0.012(2) 0.020(2) 0.0019(18) -0.0020(17) 0.0049(17) C20 0.018(2) 0.016(2) 0.015(2) 0.0033(18) -0.0054(16) 0.0055(16) C21 0.0174(19) 0.012(2) 0.015(2) 0.0035(17) -0.0007(16) 0.0039(16) C22 0.020(2) 0.018(2) 0.014(2) 0.0001(18) -0.0012(16) 0.0051(17) C23 0.023(2) 0.022(3) 0.021(2) 0.0006(19) -0.0112(18) 0.0070(18) C24 0.029(2) 0.019(3) 0.021(2) -0.0023(19) -0.0082(19) 0.0035(19) C25 0.018(2) 0.011(2) 0.019(2) -0.0027(17) -0.0075(16) 0.0026(16) C26 0.020(2) 0.018(2) 0.018(2) 0.0001(18) -0.0038(17) -0.0008(17) C27 0.027(2) 0.017(2) 0.017(2) 0.0021(18) -0.0044(17) 0.0025(18) C28 0.0152(19) 0.014(2) 0.020(2) -0.0008(18) -0.0098(16) 0.0060(16) C29 0.0147(19) 0.016(2) 0.022(2) 0.0034(18) -0.0026(16) 0.0039(16) C30 0.021(2) 0.017(2) 0.016(2) 0.0015(18) 0.0000(16) 0.0063(17) C31 0.018(2) 0.016(2) 0.019(2) -0.0039(18) -0.0072(17) 0.0071(17) O32 0.0256(15) 0.0174(17) 0.0180(16) 0.0011(13) -0.0100(12) -0.0021(12) O33 0.0188(14) 0.0147(17) 0.0245(16) 0.0024(13) -0.0104(12) -0.0030(12) C34 0.023(2) 0.014(2) 0.019(2) 0.0001(18) -0.0083(17) 0.0034(17) C35 0.022(2) 0.017(2) 0.022(2) 0.0067(19) 0.0007(17) 0.0047(17) C36 0.018(2) 0.020(2) 0.024(2) 0.0036(19) -0.0055(17) 0.0065(17) C37 0.022(2) 0.014(2) 0.023(2) 0.0041(19) -0.0074(17) 0.0008(17) C38 0.021(2) 0.022(3) 0.028(3) 0.009(2) -0.0023(18) 0.0004(18) C39 0.016(2) 0.026(3) 0.029(2) 0.010(2) -0.0052(17) 0.0057(18) C40 0.022(2) 0.018(3) 0.028(2) 0.004(2) -0.0085(18) 0.0048(18) O41 0.0223(16) 0.029(2) 0.0357(19) 0.0139(15) -0.0045(13) 0.0101(13) O42 0.0276(17) 0.038(2) 0.052(2) 0.0275(19) 0.0021(16) 0.0080(15) C43 0.0163(19) 0.012(2) 0.021(2) -0.0002(18) -0.0059(16) 0.0037(16) C44 0.020(2) 0.014(2) 0.020(2) -0.0003(18) -0.0049(17) 0.0025(17) C45 0.017(2) 0.013(2) 0.023(2) 0.0007(18) -0.0032(17) 0.0013(16) C46 0.0166(19) 0.013(2) 0.020(2) -0.0023(18) -0.0066(16) 0.0066(16) C47 0.028(2) 0.020(2) 0.012(2) 0.0008(18) -0.0024(17) 0.0029(18) C48 0.022(2) 0.015(2) 0.018(2) 0.0016(18) -0.0029(17) -0.0020(17) C49 0.017(2) 0.017(2) 0.022(2) 0.0016(19) -0.0069(17) 0.0061(17) O50 0.0302(17) 0.0184(18) 0.0199(16) -0.0001(14) -0.0105(13) -0.0063(13) O51 0.0203(15) 0.0179(17) 0.0271(17) 0.0042(14) -0.0105(12) -0.0004(12) C52 0.025(2) 0.007(2) 0.015(2) -0.0011(17) -0.0065(17) 0.0003(16) C53 0.022(2) 0.017(2) 0.020(2) 0.0038(18) 0.0026(17) 0.0062(17) C54 0.020(2) 0.022(3) 0.021(2) 0.0027(19) -0.0037(17) 0.0088(18) C55 0.023(2) 0.017(2) 0.018(2) 0.0006(18) -0.0037(17) 0.0043(17) C56 0.023(2) 0.018(2) 0.023(2) 0.0049(19) -0.0022(18) 0.0031(18) C57 0.018(2) 0.021(3) 0.028(2) 0.006(2) -0.0045(18) 0.0049(18) C58 0.017(2) 0.014(2) 0.022(2) 0.0026(19) -0.0027(17) 0.0020(17) O59 0.0274(16) 0.0247(18) 0.0186(16) 0.0055(14) -0.0037(12) 0.0127(13) O60 0.0227(16) 0.031(2) 0.0304(18) 0.0152(16) 0.0012(13) 0.0048(14) Zn61 0.0218(3) 0.0110(3) 0.0148(3) 0.00015(19) -0.00787(18) 0.00290(19) K62 0.0460(7) 0.0531(9) 0.0421(7) 0.0085(6) -0.0032(6) 0.0047(6) O63 0.0199(15) 0.035(2) 0.0338(19) -0.0008(16) -0.0012(13) 0.0006(14) C64 0.026(2) 0.042(3) 0.035(3) 0.000(3) -0.001(2) -0.006(2) C65 0.035(3) 0.034(3) 0.038(3) -0.005(2) -0.006(2) -0.013(2) O66 0.0333(18) 0.033(2) 0.040(2) -0.0013(17) -0.0030(15) -0.0007(15) C67 0.047(3) 0.024(3) 0.038(3) -0.003(2) 0.004(2) 0.002(2) C68 0.056(3) 0.035(4) 0.045(3) 0.017(3) 0.003(3) 0.012(3) O69 0.0331(18) 0.033(2) 0.035(2) 0.0109(16) -0.0045(15) 0.0026(15) C70 0.043(3) 0.061(4) 0.044(3) 0.018(3) -0.009(3) 0.024(3) C71 0.021(2) 0.064(4) 0.035(3) 0.002(3) -0.007(2) 0.010(2) O72 0.0223(16) 0.046(2) 0.042(2) 0.0080(18) 0.0009(15) 0.0047(16) C73 0.022(3) 0.057(4) 0.064(4) 0.008(3) -0.003(2) -0.004(3) C74 0.038(3) 0.042(4) 0.049(4) -0.002(3) -0.006(3) -0.010(2) O75 0.0362(19) 0.037(2) 0.040(2) -0.0001(17) -0.0048(16) -0.0026(16) C76 0.056(3) 0.025(3) 0.043(3) 0.004(3) -0.005(3) -0.002(3) C77 0.054(3) 0.034(3) 0.046(3) 0.011(3) -0.010(3) 0.003(3) O78 0.0376(18) 0.028(2) 0.0308(19) 0.0085(16) -0.0067(14) 0.0018(15) C79 0.040(3) 0.048(4) 0.031(3) 0.009(3) -0.006(2) 0.017(3) C80 0.025(2) 0.048(4) 0.031(3) -0.002(2) -0.006(2) 0.010(2) O81 0.0279(16) 0.033(2) 0.0230(17) 0.0034(15) -0.0015(13) 0.0099(14) C82 0.050(3) 0.064(4) 0.043(3) -0.006(3) 0.002(3) -0.005(3) O83 0.0289(19) 0.050(3) 0.067(3) 0.007(2) 0.0105(18) -0.0044(17) C84 0.043(3) 0.039(4) 0.072(4) 0.012(3) -0.003(3) -0.001(3) O85 0.032(2) 0.050(3) 0.084(3) 0.005(2) 0.015(2) -0.0055(18) C86 0.046(3) 0.043(4) 0.073(5) 0.011(3) 0.006(3) 0.002(3) O87 0.051(4) 0.029(4) 0.036(4) 0.002(3) 0.003(3) 0.010(3) C88 0.066(7) 0.008(5) 0.017(5) 0.001(4) 0.001(4) -0.004(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C7 1.370(5) . ? N1 C10 1.379(4) . ? N1 Zn61 2.059(3) . ? N2 C15 1.375(5) . ? N2 C12 1.380(5) . ? N2 Zn61 2.054(3) . ? N3 C17 1.369(5) . ? N3 C20 1.387(5) . ? N3 Zn61 2.068(3) . ? N4 C22 1.375(5) . ? N4 C5 1.371(5) . ? N4 Zn61 2.053(3) . ? C5 C6 1.405(6) . ? C5 C24 1.433(5) . ? C6 C7 1.412(5) . ? C6 C25 1.499(5) . ? C7 C8 1.435(5) . ? C8 C9 1.347(5) . ? C9 C10 1.428(6) . ? C10 C11 1.403(5) . ? C11 C12 1.405(6) . ? C11 C34 1.508(5) . ? C12 C13 1.436(5) . ? C13 C14 1.359(6) . ? C14 C15 1.438(5) . ? C15 C16 1.407(6) . ? C16 C17 1.412(5) . ? C16 C43 1.493(5) . ? C17 C18 1.435(5) . ? C18 C19 1.344(5) . ? C19 C20 1.442(6) . ? C20 C21 1.403(5) . ? C21 C22 1.397(6) . ? C21 C52 1.498(5) . ? C22 C23 1.442(5) . ? C23 C24 1.349(6) . ? C25 C26 1.396(6) . ? C25 C30 1.411(6) . ? C26 C27 1.378(6) . ? C27 C28 1.388(6) . ? C28 C29 1.394(6) . ? C28 C31 1.508(5) . ? C29 C30 1.382(6) . ? C31 O32 1.259(5) . ? C31 O33 1.272(5) . ? C34 C35 1.395(5) . ? C34 C39 1.389(6) . ? C35 C36 1.378(5) . ? C36 C37 1.371(6) . ? C37 C38 1.386(6) . ? C37 C40 1.511(5) . ? C38 C39 1.386(5) . ? C40 O42 1.205(5) . ? C40 O41 1.321(5) . ? C43 C44 1.409(6) . ? C43 C48 1.410(6) . ? C44 C45 1.395(6) . ? C45 C46 1.391(6) . ? C46 C47 1.381(6) . ? C46 C49 1.504(6) . ? C47 C48 1.379(6) . ? C49 O51 1.221(5) . ? C49 O50 1.316(5) . ? C52 C57 1.386(6) . ? C52 C53 1.397(5) . ? C53 C54 1.375(5) . ? C54 C55 1.384(6) . ? C55 C56 1.399(5) . ? C55 C58 1.508(5) . ? C56 C57 1.382(5) . ? C58 O60 1.225(5) . ? C58 O59 1.307(5) . ? Zn61 O81 2.155(3) . ? K62 O83 2.484(4) . ? K62 O85 2.485(4) . ? K62 O72 2.748(3) . ? K62 O63 2.749(3) . ? K62 O66 2.783(4) . ? K62 O75 2.794(4) . ? K62 O78 2.820(3) . ? K62 O69 2.829(3) . ? K62 C86 3.500(7) . ? K62 C79 3.526(5) . ? K62 C84 3.532(7) . ? O63 C64 1.419(6) . ? O63 C80 1.430(6) . ? C64 C65 1.487(7) . ? C65 O66 1.422(6) . ? O66 C67 1.424(6) . ? C67 C68 1.465(7) . ? C68 O69 1.418(6) . ? O69 C70 1.422(6) . ? C70 C71 1.472(8) . ? C71 O72 1.425(6) . ? O72 C73 1.419(6) . ? C73 C74 1.484(8) . ? C74 O75 1.433(6) . ? O75 C76 1.424(6) . ? C76 C77 1.480(7) . ? C77 O78 1.420(6) . ? O78 C79 1.418(5) . ? C79 C80 1.480(7) . ? O81 C82 1.441(6) . ? O83 C84 1.396(7) . ? O85 C86 1.406(7) . ? O87 C88 1.448(11) . ? 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 C7 N1 C10 106.0(3) . . ? C7 N1 Zn61 126.8(2) . . ? C10 N1 Zn61 127.1(3) . . ? C15 N2 C12 106.8(3) . . ? C15 N2 Zn61 126.5(3) . . ? C12 N2 Zn61 126.7(3) . . ? C17 N3 C20 106.1(3) . . ? C17 N3 Zn61 127.4(3) . . ? C20 N3 Zn61 125.4(3) . . ? C22 N4 C5 106.9(3) . . ? C22 N4 Zn61 126.0(3) . . ? C5 N4 Zn61 125.8(3) . . ? N4 C5 C6 126.0(3) . . ? N4 C5 C24 109.4(4) . . ? C6 C5 C24 124.5(4) . . ? C5 C6 C7 125.7(4) . . ? C5 C6 C25 116.4(3) . . ? C7 C6 C25 117.9(3) . . ? N1 C7 C6 124.9(4) . . ? N1 C7 C8 110.0(3) . . ? C6 C7 C8 125.1(4) . . ? C9 C8 C7 106.7(4) . . ? C8 C9 C10 107.8(3) . . ? N1 C10 C11 124.9(4) . . ? N1 C10 C9 109.4(3) . . ? C11 C10 C9 125.6(3) . . ? C10 C11 C12 125.8(3) . . ? C10 C11 C34 117.1(4) . . ? C12 C11 C34 117.1(3) . . ? N2 C12 C11 125.7(3) . . ? N2 C12 C13 109.3(4) . . ? C11 C12 C13 125.1(3) . . ? C14 C13 C12 107.3(3) . . ? C13 C14 C15 107.2(4) . . ? N2 C15 C16 126.4(3) . . ? N2 C15 C14 109.4(3) . . ? C16 C15 C14 124.1(4) . . ? C15 C16 C17 125.0(4) . . ? C15 C16 C43 117.1(3) . . ? C17 C16 C43 117.9(3) . . ? N3 C17 C16 124.6(4) . . ? N3 C17 C18 110.1(3) . . ? C16 C17 C18 125.2(4) . . ? C19 C18 C17 107.3(4) . . ? C18 C19 C20 107.5(3) . . ? N3 C20 C21 125.5(4) . . ? N3 C20 C19 109.1(3) . . ? C21 C20 C19 125.4(3) . . ? C22 C21 C20 125.7(3) . . ? C22 C21 C52 117.3(3) . . ? C20 C21 C52 117.0(4) . . ? N4 C22 C21 125.8(3) . . ? N4 C22 C23 109.0(4) . . ? C21 C22 C23 125.2(4) . . ? C24 C23 C22 107.2(3) . . ? C23 C24 C5 107.5(4) . . ? C26 C25 C30 118.4(4) . . ? C26 C25 C6 120.5(4) . . ? C30 C25 C6 121.1(4) . . ? C27 C26 C25 121.0(4) . . ? C26 C27 C28 120.7(4) . . ? C27 C28 C29 119.0(4) . . ? C27 C28 C31 120.1(4) . . ? C29 C28 C31 120.9(4) . . ? C30 C29 C28 120.9(4) . . ? C29 C30 C25 120.1(4) . . ? O32 C31 O33 122.8(4) . . ? O32 C31 C28 117.3(4) . . ? O33 C31 C28 119.8(4) . . ? C35 C34 C39 119.1(3) . . ? C35 C34 C11 120.0(4) . . ? C39 C34 C11 120.8(3) . . ? C36 C35 C34 119.9(4) . . ? C37 C36 C35 120.8(4) . . ? C36 C37 C38 119.9(4) . . ? C36 C37 C40 121.4(4) . . ? C38 C37 C40 118.7(4) . . ? C39 C38 C37 119.9(4) . . ? C38 C39 C34 120.3(4) . . ? O42 C40 O41 122.9(4) . . ? O42 C40 C37 123.6(4) . . ? O41 C40 C37 113.5(4) . . ? C44 C43 C48 118.9(4) . . ? C44 C43 C16 120.8(4) . . ? C48 C43 C16 120.3(4) . . ? C45 C44 C43 119.6(4) . . ? C46 C45 C44 120.8(4) . . ? C47 C46 C45 119.3(4) . . ? C47 C46 C49 121.6(4) . . ? C45 C46 C49 119.0(4) . . ? C48 C47 C46 121.3(4) . . ? C47 C48 C43 120.0(4) . . ? O51 C49 O50 124.0(4) . . ? O51 C49 C46 123.4(4) . . ? O50 C49 C46 112.5(4) . . ? C57 C52 C53 118.2(3) . . ? C57 C52 C21 121.2(3) . . ? C53 C52 C21 120.6(4) . . ? C54 C53 C52 120.8(4) . . ? C53 C54 C55 120.7(4) . . ? C54 C55 C56 119.4(3) . . ? C54 C55 C58 121.8(3) . . ? C56 C55 C58 118.8(4) . . ? C57 C56 C55 119.4(4) . . ? C56 C57 C52 121.6(4) . . ? O60 C58 O59 123.6(4) . . ? O60 C58 C55 122.1(3) . . ? O59 C58 C55 114.3(4) . . ? N4 Zn61 N2 167.19(12) . . ? N4 Zn61 N1 89.76(12) . . ? N2 Zn61 N1 89.37(12) . . ? N4 Zn61 N3 89.44(13) . . ? N2 Zn61 N3 88.80(13) . . ? N1 Zn61 N3 168.15(12) . . ? N4 Zn61 O81 93.42(12) . . ? N2 Zn61 O81 99.38(12) . . ? N1 Zn61 O81 95.57(12) . . ? N3 Zn61 O81 96.28(12) . . ? O83 K62 O85 177.90(13) . . ? O83 K62 O72 76.93(11) . . ? O85 K62 O72 104.40(12) . . ? O83 K62 O63 100.69(11) . . ? O85 K62 O63 77.99(11) . . ? O72 K62 O63 177.60(10) . . ? O83 K62 O66 81.85(12) . . ? O85 K62 O66 96.07(12) . . ? O72 K62 O66 118.92(11) . . ? O63 K62 O66 60.70(10) . . ? O83 K62 O75 96.07(12) . . ? O85 K62 O75 86.01(12) . . ? O72 K62 O75 60.57(10) . . ? O63 K62 O75 119.71(11) . . ? O66 K62 O75 177.91(10) . . ? O83 K62 O78 93.93(12) . . ? O85 K62 O78 86.88(12) . . ? O72 K62 O78 117.88(11) . . ? O63 K62 O78 61.72(10) . . ? O66 K62 O78 120.17(10) . . ? O75 K62 O78 59.65(10) . . ? O83 K62 O69 84.81(12) . . ? O85 K62 O69 94.38(12) . . ? O72 K62 O69 61.86(10) . . ? O63 K62 O69 118.47(11) . . ? O66 K62 O69 59.67(10) . . ? O75 K62 O69 120.46(10) . . ? O78 K62 O69 178.74(9) . . ? O83 K62 C86 158.91(14) . . ? O85 K62 C86 19.00(13) . . ? O72 K62 C86 115.49(12) . . ? O63 K62 C86 66.87(12) . . ? O66 K62 C86 77.19(13) . . ? O75 K62 C86 104.89(13) . . ? O78 K62 C86 94.56(12) . . ? O69 K62 C86 86.63(12) . . ? O83 K62 C79 106.86(13) . . ? O85 K62 C79 73.29(13) . . ? O72 K62 C79 137.87(13) . . ? O63 K62 C79 42.32(11) . . ? O66 K62 C79 102.99(12) . . ? O75 K62 C79 77.39(12) . . ? O78 K62 C79 22.49(11) . . ? O69 K62 C79 158.22(12) . . ? C86 K62 C79 76.00(13) . . ? O83 K62 C84 17.91(13) . . ? O85 K62 C84 164.16(14) . . ? O72 K62 C84 67.99(12) . . ? O63 K62 C84 109.64(12) . . ? O66 K62 C84 99.76(12) . . ? O75 K62 C84 78.15(12) . . ? O78 K62 C84 84.92(12) . . ? O69 K62 C84 93.87(12) . . ? C86 K62 C84 176.15(12) . . ? C79 K62 C84 102.61(13) . . ? C64 O63 C80 112.1(4) . . ? C64 O63 K62 113.1(3) . . ? C80 O63 K62 115.2(3) . . ? O63 C64 C65 108.9(4) . . ? O66 C65 C64 108.9(4) . . ? C65 O66 C67 111.9(4) . . ? C65 O66 K62 116.0(3) . . ? C67 O66 K62 114.1(3) . . ? O66 C67 C68 108.2(4) . . ? O69 C68 C67 109.3(4) . . ? C68 O69 C70 111.2(4) . . ? C68 O69 K62 115.0(3) . . ? C70 O69 K62 108.0(3) . . ? O69 C70 C71 109.2(4) . . ? O72 C71 C70 110.1(4) . . ? C73 O72 C71 112.2(4) . . ? C73 O72 K62 114.0(3) . . ? C71 O72 K62 114.8(3) . . ? O72 C73 C74 108.5(4) . . ? O75 C74 C73 108.8(4) . . ? C76 O75 C74 111.3(4) . . ? C76 O75 K62 114.3(3) . . ? C74 O75 K62 115.4(3) . . ? O75 C76 C77 108.5(4) . . ? O78 C77 C76 108.2(4) . . ? C79 O78 C77 110.7(4) . . ? C79 O78 K62 108.0(3) . . ? C77 O78 K62 115.6(3) . . ? O78 C79 C80 108.9(4) . . ? O78 C79 K62 49.5(2) . . ? C80 C79 K62 80.8(3) . . ? O63 C80 C79 109.6(4) . . ? C82 O81 Zn61 122.2(3) . . ? C84 O83 K62 128.9(3) . . ? O83 C84 K62 33.2(2) . . ? C86 O85 K62 125.9(3) . . ? O85 C86 K62 35.1(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O63 C64 C65 O66 63.9(5) . . . . ? C64 C65 O66 C67 -173.4(4) . . . . ? C65 O66 C67 C68 -171.0(4) . . . . ? O66 C67 C68 O69 -65.9(5) . . . . ? C67 C68 O69 C70 167.2(4) . . . . ? C68 O69 C70 C71 175.6(4) . . . . ? O69 C70 C71 O72 69.2(5) . . . . ? C70 C71 O72 C73 -174.2(4) . . . . ? C71 O72 C73 C74 -172.1(4) . . . . ? O72 C73 C74 O75 -64.4(6) . . . . ? C73 C74 O75 C76 174.1(4) . . . . ? C74 O75 C76 C77 173.9(4) . . . . ? O75 C76 C77 O78 65.8(5) . . . . ? C76 C77 O78 C79 -169.2(4) . . . . ? C77 O78 C79 C80 -173.5(4) . . . . ? O78 C79 C80 O63 -69.0(5) . . . . ? C79 C80 O63 C64 171.5(4) . . . . ? C80 O63 C64 C65 171.9(4) . . . . ? _diffrn_measured_fraction_theta_max 0.949 _diffrn_reflns_theta_full 28.74 _diffrn_measured_fraction_theta_full 0.949 _refine_diff_density_max 1.308 _refine_diff_density_min -1.390 _refine_diff_density_rms 0.115 #====END----------------------------------------------