# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email jurekl@wchuwr.pl _publ_contact_author_name 'Jerzy Lisowski' loop_ _publ_author_name 'Aleksandra Sarnicka' 'Przemyslaw Starynowicz' 'Jerzy Lisowski' data_scczn _database_code_depnum_ccdc_archive 'CCDC 851728' #TrackingRef '- complex3.CIF' _vrf_PLAT761_I ; PROBLEM: CIF Contains no X-H Bonds ...................... ? RESPONSE: The data contain only C-bonded H atoms, calculated from geometry and set at standard distances... ; _vrf_PLAT762_I ; PROBLEM: CIF Contains no X-Y-H or H-Y-H Angles .......... ? RESPONSE: ...and angles ; _vrf_PLAT780_I ; PROBLEM: Coordinates do not Form a Properly Connected Set ? RESPONSE: The complecs seems to be connected properly. The problem may result from the presence of lattice solvent molecules ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H68 N4 O12 Zn2' _chemical_formula_weight 975.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 8.886(3) _cell_length_b 11.478(3) _cell_length_c 12.337(3) _cell_angle_alpha 91.92(2) _cell_angle_beta 98.96(2) _cell_angle_gamma 103.52(2) _cell_volume 1205.3(6) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 13059 _cell_measurement_theta_min 4.6806 _cell_measurement_theta_max 38.5148 _exptl_crystal_description irregular _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4250 _exptl_crystal_size_mid 0.3537 _exptl_crystal_size_min 0.1914 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.344 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 516 _exptl_absorpt_coefficient_mu 1.057 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.730 _exptl_absorpt_correction_T_max 0.868 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET) (compiled May 29 2009,17:40:42) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Kuma KM4 with a CCD counter' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 8.1956 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26681 _diffrn_reflns_av_R_equivalents 0.0212 _diffrn_reflns_av_sigmaI/netI 0.0645 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 4.69 _diffrn_reflns_theta_max 38.58 _reflns_number_total 17647 _reflns_number_gt 12712 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET) (compiled May 29 2009,17:40:42) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET) (compiled May 29 2009,17:40:42) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET) (compiled May 29 2009,17:40:42) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.013(7) _refine_ls_number_reflns 17647 _refine_ls_number_parameters 570 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0568 _refine_ls_R_factor_gt 0.0367 _refine_ls_wR_factor_ref 0.0852 _refine_ls_wR_factor_gt 0.0816 _refine_ls_goodness_of_fit_ref 0.964 _refine_ls_restrained_S_all 0.964 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.00969(2) 0.352167(18) 0.676474(16) 0.01498(7) Uani 1 1 d . . . Zn2 Zn 0.11556(2) 0.403909(18) 0.443728(17) 0.01476(7) Uani 1 1 d . . . O1 O -0.0393(3) 0.2899(2) 0.51724(18) 0.0243(5) Uani 1 1 d . . . O2 O 0.1619(3) 0.4686(2) 0.60351(17) 0.0201(5) Uani 1 1 d . . . O41 O -0.0193(3) 0.5058(2) 0.37926(18) 0.0236(5) Uani 1 1 d . . . O42 O 0.1046(3) 0.5165(3) 0.2365(2) 0.0409(8) Uani 1 1 d . . . O43 O 0.1418(3) 0.2458(2) 0.73884(19) 0.0250(5) Uani 1 1 d . . . O44 O 0.0186(3) 0.2331(3) 0.8808(2) 0.0380(7) Uani 1 1 d . . . O51 O 0.1960(3) 0.6142(2) 0.05588(19) 0.0292(6) Uani 1 1 d . . . O52 O -0.0642(3) 0.1395(2) 1.0637(2) 0.0323(6) Uani 1 1 d . . . O53 O -0.1564(3) 0.6128(2) 0.5287(2) 0.0342(6) Uani 1 1 d . . . O54 O 0.2797(3) 0.1256(2) 0.5972(2) 0.0322(6) Uani 1 1 d . . . OW1 O -0.0012(2) -0.06622(16) 1.15043(15) 0.0358(4) Uani 1 1 d . . . OW2 O 0.0756(6) 0.8834(5) 0.0739(4) 0.0834(9) Uani 1 1 d . . . N1 N -0.2301(3) 0.3099(2) 0.66724(19) 0.0139(5) Uani 1 1 d . . . N2 N 0.1417(3) 0.2515(2) 0.36426(18) 0.0148(4) Uani 1 1 d . . . N3 N 0.3513(3) 0.4583(2) 0.44934(19) 0.0147(5) Uani 1 1 d . . . N4 N 0.0012(3) 0.4950(2) 0.77479(19) 0.0162(4) Uani 1 1 d . . . C1 C -0.1389(2) 0.46028(18) 0.82698(16) 0.0141(3) Uani 1 1 d . . . H1 H -0.1193 0.4003 0.8786 0.017 Uiso 1 1 calc R . . C2 C -0.1814(3) 0.5594(3) 0.8927(2) 0.0142(5) Uani 1 1 d . . . H2A H -0.0923 0.5989 0.9480 0.017 Uiso 1 1 calc R . . H2B H -0.2079 0.6189 0.8441 0.017 Uiso 1 1 calc R . . C3 C -0.3217(3) 0.5046(2) 0.94830(18) 0.0189(4) Uani 1 1 d . . . H3A H -0.3516 0.5680 0.9874 0.023 Uiso 1 1 calc R . . H3B H -0.2915 0.4504 1.0015 0.023 Uiso 1 1 calc R . . C4 C -0.4616(3) 0.4361(2) 0.8643(2) 0.0196(5) Uani 1 1 d . . . H4A H -0.5004 0.4926 0.8174 0.024 Uiso 1 1 calc R . . H4B H -0.5451 0.3975 0.9027 0.024 Uiso 1 1 calc R . . C5 C -0.4195(4) 0.3407(3) 0.7927(3) 0.0223(6) Uani 1 1 d . . . H5A H -0.3948 0.2779 0.8378 0.027 Uiso 1 1 calc R . . H5B H -0.5091 0.3046 0.7364 0.027 Uiso 1 1 calc R . . C6 C -0.2788(3) 0.3961(2) 0.73803(18) 0.0148(4) Uani 1 1 d . . . H6 H -0.3084 0.4573 0.6915 0.018 Uiso 1 1 calc R . . C7 C -0.3275(4) 0.2297(3) 0.6018(2) 0.0163(6) Uani 1 1 d . . . H7 H -0.4332 0.2166 0.6072 0.020 Uiso 1 1 calc R . . C8 C -0.2828(4) 0.1551(3) 0.5165(2) 0.0138(5) Uani 1 1 d . . . C9 C -0.3960(4) 0.0510(3) 0.4671(2) 0.0149(5) Uani 1 1 d . . . H9 H -0.4924 0.0295 0.4909 0.018 Uiso 1 1 calc R . . C10 C -0.3645(3) -0.0199(3) 0.3829(2) 0.0152(5) Uani 1 1 d . . . C11 C -0.4862(4) -0.1318(3) 0.3245(3) 0.0182(6) Uani 1 1 d . . . C12 C -0.6395(4) -0.1571(3) 0.3712(3) 0.0353(9) Uani 1 1 d . . . H12A H -0.7090 -0.2294 0.3349 0.053 Uiso 1 1 calc R . . H12B H -0.6882 -0.0912 0.3594 0.053 Uiso 1 1 calc R . . H12C H -0.6174 -0.1665 0.4487 0.053 Uiso 1 1 calc R . . C13 C -0.4155(4) -0.2410(3) 0.3387(3) 0.0293(7) Uani 1 1 d . . . H13A H -0.3228 -0.2288 0.3054 0.044 Uiso 1 1 calc R . . H13B H -0.4908 -0.3116 0.3040 0.044 Uiso 1 1 calc R . . H13C H -0.3885 -0.2511 0.4157 0.044 Uiso 1 1 calc R . . C14 C -0.5212(4) -0.1136(3) 0.2015(3) 0.0313(8) Uani 1 1 d . . . H14A H -0.4267 -0.1048 0.1707 0.047 Uiso 1 1 calc R . . H14B H -0.5599 -0.0426 0.1918 0.047 Uiso 1 1 calc R . . H14C H -0.5989 -0.1820 0.1649 0.047 Uiso 1 1 calc R . . C15 C -0.2178(3) 0.0158(3) 0.3489(2) 0.0143(5) Uani 1 1 d . . . H15 H -0.1934 -0.0327 0.2957 0.017 Uiso 1 1 calc R . . C16 C -0.1085(3) 0.1200(3) 0.3914(2) 0.0147(5) Uani 1 1 d . . . C17 C -0.1405(4) 0.1923(3) 0.4760(2) 0.0152(6) Uani 1 1 d . . . C18 C 0.0450(3) 0.1466(2) 0.3547(2) 0.0170(5) Uani 1 1 d . . . H18 H 0.0748 0.0832 0.3221 0.020 Uiso 1 1 calc R . . C19 C 0.3057(2) 0.26395(18) 0.34443(17) 0.0150(4) Uani 1 1 d . . . H19 H 0.3602 0.2247 0.4022 0.018 Uiso 1 1 calc R . . C20 C 0.3199(4) 0.2090(3) 0.2333(3) 0.0197(6) Uani 1 1 d . . . H20A H 0.2686 0.1240 0.2268 0.024 Uiso 1 1 calc R . . H20B H 0.2664 0.2467 0.1751 0.024 Uiso 1 1 calc R . . C21 C 0.4885(3) 0.2246(2) 0.21926(19) 0.0197(4) Uani 1 1 d . . . H21A H 0.4922 0.1939 0.1457 0.024 Uiso 1 1 calc R . . H21B H 0.5384 0.1779 0.2713 0.024 Uiso 1 1 calc R . . C22 C 0.5797(3) 0.3562(2) 0.2372(2) 0.0184(5) Uani 1 1 d . . . H22A H 0.6898 0.3614 0.2356 0.022 Uiso 1 1 calc R . . H22B H 0.5411 0.4005 0.1777 0.022 Uiso 1 1 calc R . . C23 C 0.5629(3) 0.4127(3) 0.3462(2) 0.0153(5) Uani 1 1 d . . . H23A H 0.6120 0.3745 0.4061 0.018 Uiso 1 1 calc R . . H23B H 0.6159 0.4974 0.3529 0.018 Uiso 1 1 calc R . . C24 C 0.3913(3) 0.3988(2) 0.35373(18) 0.0147(4) Uani 1 1 d . . . H24 H 0.3456 0.4330 0.2885 0.018 Uiso 1 1 calc R . . C25 C 0.4511(3) 0.5359(3) 0.5181(2) 0.0123(5) Uani 1 1 d . . . H25 H 0.5554 0.5525 0.5082 0.015 Uiso 1 1 calc R . . C26 C 0.4146(3) 0.6004(3) 0.6108(2) 0.0132(5) Uani 1 1 d . . . C27 C 0.5250(3) 0.6996(3) 0.6640(2) 0.0146(5) Uani 1 1 d . . . H27 H 0.6206 0.7217 0.6391 0.017 Uiso 1 1 calc R . . C28 C 0.5024(3) 0.7684(3) 0.7521(2) 0.0144(5) Uani 1 1 d . . . C29 C 0.6227(4) 0.8797(3) 0.8091(3) 0.0188(6) Uani 1 1 d . . . C30 C 0.7745(4) 0.9043(3) 0.7614(3) 0.0287(7) Uani 1 1 d . . . H30A H 0.8193 0.8359 0.7685 0.043 Uiso 1 1 calc R . . H30B H 0.8473 0.9736 0.8006 0.043 Uiso 1 1 calc R . . H30C H 0.7523 0.9188 0.6850 0.043 Uiso 1 1 calc R . . C31 C 0.6640(4) 0.8615(3) 0.9320(3) 0.0275(7) Uani 1 1 d . . . H31A H 0.5697 0.8431 0.9635 0.041 Uiso 1 1 calc R . . H31B H 0.7333 0.9337 0.9689 0.041 Uiso 1 1 calc R . . H31C H 0.7148 0.7964 0.9404 0.041 Uiso 1 1 calc R . . C32 C 0.5533(4) 0.9900(3) 0.7958(3) 0.0325(8) Uani 1 1 d . . . H32A H 0.5266 1.0009 0.7190 0.049 Uiso 1 1 calc R . . H32B H 0.6292 1.0600 0.8311 0.049 Uiso 1 1 calc R . . H32C H 0.4606 0.9780 0.8291 0.049 Uiso 1 1 calc R . . C33 C 0.3603(3) 0.7308(3) 0.7892(2) 0.0157(5) Uani 1 1 d . . . H33 H 0.3413 0.7758 0.8474 0.019 Uiso 1 1 calc R . . C34 C 0.2441(3) 0.6288(3) 0.7436(2) 0.0136(5) Uani 1 1 d . . . C35 C 0.2695(4) 0.5624(3) 0.6501(2) 0.0140(6) Uani 1 1 d . . . C36 C 0.1013(3) 0.5951(2) 0.79329(19) 0.0160(5) Uani 1 1 d . . . H36 H 0.0832 0.6518 0.8421 0.019 Uiso 1 1 calc R . . C40 C 0.0070(4) 0.5451(3) 0.2865(3) 0.0208(7) Uani 1 1 d . . . C41 C -0.0867(4) 0.6315(3) 0.2398(3) 0.0300(8) Uani 1 1 d . . . H41A H -0.0400 0.7106 0.2746 0.045 Uiso 1 1 calc R . . H41B H -0.1926 0.6059 0.2532 0.045 Uiso 1 1 calc R . . H41C H -0.0871 0.6330 0.1620 0.045 Uiso 1 1 calc R . . C42 C 0.1202(4) 0.2089(3) 0.8333(3) 0.0215(7) Uani 1 1 d . . . C43 C 0.2241(4) 0.1331(4) 0.8846(3) 0.0309(8) Uani 1 1 d . . . H43A H 0.2541 0.1559 0.9620 0.046 Uiso 1 1 calc R . . H43B H 0.3164 0.1448 0.8509 0.046 Uiso 1 1 calc R . . H43C H 0.1685 0.0500 0.8739 0.046 Uiso 1 1 calc R . . C51 C 0.3043(5) 0.5470(4) 0.0369(3) 0.0380(9) Uani 1 1 d . . . H51A H 0.3353 0.5633 -0.0333 0.046 Uiso 1 1 calc R . . H51B H 0.2564 0.4629 0.0373 0.046 Uiso 1 1 calc R . . H51C H 0.3950 0.5690 0.0937 0.046 Uiso 1 1 calc R . . C52 C -0.1580(5) 0.2114(4) 1.0985(3) 0.0410(10) Uani 1 1 d . . . H52A H -0.2201 0.1696 1.1488 0.049 Uiso 1 1 calc R . . H52B H -0.2260 0.2287 1.0359 0.049 Uiso 1 1 calc R . . H52C H -0.0920 0.2853 1.1347 0.049 Uiso 1 1 calc R . . C53 C -0.0512(4) 0.7269(3) 0.5473(3) 0.0324(8) Uani 1 1 d . . . H53A H -0.0499 0.7596 0.6202 0.039 Uiso 1 1 calc R . . H53B H -0.0842 0.7792 0.4944 0.039 Uiso 1 1 calc R . . H53C H 0.0523 0.7196 0.5400 0.039 Uiso 1 1 calc R . . C54 C 0.1769(5) 0.0056(4) 0.5897(3) 0.0391(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.01312(15) 0.01639(16) 0.01505(14) -0.00284(12) 0.00652(12) 0.00065(13) Zn2 0.01176(15) 0.01716(16) 0.01427(14) -0.00309(12) 0.00554(12) -0.00030(12) O1 0.0237(12) 0.0244(12) 0.0205(11) -0.0086(9) 0.0159(10) -0.0093(10) O2 0.0164(11) 0.0211(11) 0.0156(10) -0.0080(9) 0.0044(9) -0.0094(9) O41 0.0202(12) 0.0324(13) 0.0229(11) 0.0036(10) 0.0087(10) 0.0122(10) O42 0.0417(17) 0.066(2) 0.0335(14) 0.0174(14) 0.0247(13) 0.0365(16) O43 0.0246(13) 0.0278(13) 0.0283(12) 0.0065(10) 0.0137(10) 0.0109(11) O44 0.0507(18) 0.0440(16) 0.0369(15) 0.0166(13) 0.0279(14) 0.0310(14) O51 0.0334(14) 0.0396(15) 0.0236(11) 0.0074(11) 0.0119(11) 0.0215(12) O52 0.0329(14) 0.0305(14) 0.0404(14) 0.0053(12) 0.0118(12) 0.0176(12) O53 0.0184(11) 0.0415(14) 0.0393(14) -0.0100(11) 0.0062(10) 0.0015(10) O54 0.0243(12) 0.0336(12) 0.0429(14) -0.0032(10) 0.0177(11) 0.0080(10) OW1 0.0481(11) 0.0312(9) 0.0293(9) -0.0010(8) 0.0061(8) 0.0127(9) OW2 0.081(2) 0.0772(17) 0.099(3) 0.0010(17) 0.0249(18) 0.0274(16) N1 0.0141(11) 0.0142(10) 0.0128(10) -0.0033(8) 0.0055(9) 0.0010(8) N2 0.0121(9) 0.0178(10) 0.0146(9) -0.0014(7) 0.0075(7) 0.0007(7) N3 0.0137(11) 0.0168(11) 0.0138(10) 0.0006(8) 0.0051(9) 0.0025(9) N4 0.0135(9) 0.0182(10) 0.0161(9) -0.0005(8) 0.0051(8) 0.0007(8) C1 0.0132(8) 0.0167(9) 0.0135(8) -0.0003(7) 0.0062(7) 0.0036(7) C2 0.0106(10) 0.0185(12) 0.0129(10) -0.0046(9) 0.0057(8) 0.0006(9) C3 0.0198(10) 0.0222(11) 0.0165(9) -0.0026(8) 0.0074(8) 0.0062(8) C4 0.0145(10) 0.0243(13) 0.0222(11) -0.0024(9) 0.0098(9) 0.0051(9) C5 0.0172(13) 0.0209(13) 0.0276(14) -0.0042(11) 0.0089(11) -0.0004(10) C6 0.0150(9) 0.0149(10) 0.0150(9) -0.0024(7) 0.0061(8) 0.0026(8) C7 0.0163(14) 0.0183(13) 0.0168(12) 0.0028(11) 0.0087(11) 0.0051(11) C8 0.0129(13) 0.0141(13) 0.0116(11) -0.0039(10) 0.0013(10) -0.0009(10) C9 0.0139(13) 0.0134(12) 0.0159(11) -0.0010(9) 0.0029(10) 0.0000(10) C10 0.0143(11) 0.0130(11) 0.0165(11) 0.0010(9) 0.0025(9) -0.0004(9) C11 0.0143(12) 0.0162(12) 0.0214(12) -0.0039(10) 0.0044(10) -0.0014(10) C12 0.0195(15) 0.0303(17) 0.049(2) -0.0205(15) 0.0119(15) -0.0096(13) C13 0.0314(17) 0.0131(13) 0.0417(17) -0.0005(12) 0.0058(14) 0.0023(12) C14 0.0318(16) 0.0224(15) 0.0292(15) -0.0017(12) -0.0095(13) -0.0042(12) C15 0.0135(10) 0.0156(11) 0.0143(10) -0.0006(8) 0.0048(8) 0.0030(9) C16 0.0113(11) 0.0185(12) 0.0128(10) -0.0003(9) 0.0045(9) -0.0004(9) C17 0.0136(14) 0.0190(14) 0.0124(11) -0.0004(11) 0.0063(10) 0.0002(11) C18 0.0170(11) 0.0172(11) 0.0161(11) -0.0020(8) 0.0075(9) 0.0000(8) C19 0.0117(8) 0.0159(9) 0.0165(9) -0.0013(7) 0.0041(7) 0.0010(7) C20 0.0190(13) 0.0163(12) 0.0217(13) -0.0060(10) 0.0050(10) -0.0001(10) C21 0.0169(10) 0.0227(11) 0.0200(10) -0.0050(9) 0.0084(8) 0.0034(8) C22 0.0160(10) 0.0201(12) 0.0209(11) 0.0010(9) 0.0096(8) 0.0041(9) C23 0.0123(11) 0.0143(11) 0.0198(11) -0.0004(9) 0.0080(9) 0.0013(9) C24 0.0156(9) 0.0144(10) 0.0143(9) -0.0003(7) 0.0070(8) 0.0010(8) C25 0.0097(12) 0.0117(11) 0.0134(11) -0.0014(9) 0.0014(10) -0.0011(9) C26 0.0123(12) 0.0161(13) 0.0129(11) 0.0034(10) 0.0052(10) 0.0049(11) C27 0.0107(12) 0.0171(13) 0.0164(11) 0.0032(10) 0.0052(9) 0.0022(10) C28 0.0135(11) 0.0136(11) 0.0147(10) -0.0013(9) 0.0005(9) 0.0019(9) C29 0.0168(13) 0.0133(12) 0.0240(13) -0.0051(10) 0.0039(10) -0.0005(10) C30 0.0223(15) 0.0236(15) 0.0343(16) -0.0060(13) 0.0068(13) -0.0062(12) C31 0.0243(14) 0.0313(16) 0.0222(13) -0.0088(12) 0.0015(11) 0.0005(12) C32 0.0247(15) 0.0173(14) 0.050(2) -0.0017(14) -0.0047(14) 0.0013(12) C33 0.0146(11) 0.0156(11) 0.0154(11) -0.0044(9) 0.0001(9) 0.0029(9) C34 0.0142(11) 0.0122(11) 0.0138(10) 0.0000(9) 0.0041(9) 0.0014(9) C35 0.0149(14) 0.0102(12) 0.0142(12) -0.0001(10) 0.0010(11) -0.0010(10) C36 0.0178(11) 0.0183(11) 0.0122(10) -0.0021(8) 0.0037(8) 0.0046(8) C40 0.0179(15) 0.0224(17) 0.0219(15) 0.0036(13) 0.0030(13) 0.0044(13) C41 0.0253(16) 0.0313(18) 0.0380(19) 0.0093(15) 0.0106(14) 0.0115(14) C42 0.0207(16) 0.0187(16) 0.0275(16) -0.0012(13) 0.0109(13) 0.0053(13) C43 0.0271(17) 0.038(2) 0.0348(18) 0.0112(15) 0.0138(14) 0.0143(15) C51 0.048(2) 0.054(2) 0.0279(15) 0.0144(15) 0.0198(15) 0.0324(18) C52 0.048(2) 0.059(3) 0.0311(17) 0.0123(17) 0.0190(15) 0.034(2) C53 0.0239(14) 0.0393(18) 0.0350(16) -0.0069(13) 0.0051(12) 0.0105(13) C54 0.0328(17) 0.0310(16) 0.0456(19) -0.0049(14) -0.0021(14) -0.0015(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O43 1.978(2) . yes Zn1 O1 2.013(2) . yes Zn1 O2 2.010(2) . yes Zn1 N4 2.030(3) . yes Zn1 N1 2.056(3) . yes Zn2 O41 1.964(2) . yes Zn2 O1 2.013(2) . yes Zn2 N3 2.031(3) . yes Zn2 O2 2.028(2) . yes Zn2 N2 2.055(2) . yes O1 C17 1.293(4) . no O2 C35 1.307(4) . no O41 C40 1.280(4) . no O42 C40 1.235(4) . no O43 C42 1.280(4) . no O44 C42 1.227(4) . no O51 C51 1.408(4) . no O52 C52 1.404(5) . no O53 C53 1.408(4) . no O54 C54 1.455(5) . no OW1 OW2 1.428(5) 1_546 no OW2 OW1 1.428(5) 1_564 no N1 C7 1.268(4) . no N1 C6 1.479(3) . no N2 C18 1.295(4) . no N2 C19 1.490(3) . no N3 C25 1.283(4) . no N3 C24 1.475(3) . no N4 C36 1.267(4) . no N4 C1 1.469(3) . no C1 C2 1.526(3) . no C1 C6 1.544(3) . no C2 C3 1.532(4) . no C3 C4 1.524(3) . no C4 C5 1.533(4) . no C5 C6 1.530(4) . no C7 C8 1.492(4) . no C8 C17 1.411(4) . no C8 C9 1.418(4) . no C9 C10 1.399(4) . no C10 C15 1.406(4) . no C10 C11 1.544(4) . no C11 C13 1.531(4) . no C11 C14 1.533(4) . no C11 C12 1.530(5) . no C15 C16 1.380(4) . no C16 C17 1.415(4) . no C16 C18 1.471(4) . no C19 C20 1.525(4) . no C19 C24 1.548(3) . no C20 C21 1.505(4) . no C21 C22 1.529(3) . no C22 C23 1.517(4) . no C23 C24 1.513(3) . no C25 C26 1.460(4) . no C26 C27 1.385(4) . no C26 C35 1.426(5) . no C27 C28 1.389(4) . no C28 C33 1.388(4) . no C28 C29 1.529(4) . no C29 C30 1.525(5) . no C29 C31 1.537(4) . no C29 C32 1.535(4) . no C33 C34 1.401(4) . no C34 C35 1.437(4) . no C34 C36 1.471(4) . no C40 C41 1.511(5) . no C42 C43 1.497(5) . no 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 O43 Zn1 O1 100.56(10) . . no O43 Zn1 O2 101.39(10) . . no O1 Zn1 O2 75.60(8) . . no O43 Zn1 N4 117.19(10) . . no O1 Zn1 N4 140.89(10) . . no O2 Zn1 N4 86.76(10) . . no O43 Zn1 N1 122.54(10) . . no O1 Zn1 N1 84.47(10) . . no O2 Zn1 N1 134.45(9) . . no N4 Zn1 N1 83.63(10) . . no O41 Zn2 O1 99.67(10) . . no O41 Zn2 N3 119.22(10) . . no O1 Zn2 N3 139.14(10) . . no O41 Zn2 O2 100.66(9) . . no O1 Zn2 O2 75.20(8) . . no N3 Zn2 O2 85.14(10) . . no O41 Zn2 N2 124.08(10) . . no O1 Zn2 N2 85.08(10) . . no N3 Zn2 N2 83.23(10) . . no O2 Zn2 N2 133.63(9) . . no C17 O1 Zn1 126.06(19) . . no C17 O1 Zn2 128.93(19) . . no Zn1 O1 Zn2 104.79(11) . . no C35 O2 Zn1 127.37(19) . . no C35 O2 Zn2 128.21(19) . . no Zn1 O2 Zn2 104.39(10) . . no C40 O41 Zn2 115.8(2) . . no C42 O43 Zn1 116.2(2) . . no C7 N1 C6 122.9(2) . . no C7 N1 Zn1 125.8(2) . . no C6 N1 Zn1 110.90(16) . . no C18 N2 C19 120.3(2) . . no C18 N2 Zn2 125.9(2) . . no C19 N2 Zn2 111.83(16) . . no C25 N3 C24 124.0(3) . . no C25 N3 Zn2 127.9(2) . . no C24 N3 Zn2 108.02(17) . . no C36 N4 C1 125.0(2) . . no C36 N4 Zn1 127.0(2) . . no C1 N4 Zn1 107.87(16) . . no N4 C1 C2 117.0(2) . . no N4 C1 C6 108.43(17) . . no C2 C1 C6 110.85(19) . . no C3 C2 C1 109.4(2) . . no C2 C3 C4 111.3(2) . . no C3 C4 C5 112.4(2) . . no C6 C5 C4 110.9(2) . . no N1 C6 C5 114.4(2) . . no N1 C6 C1 110.08(18) . . no C5 C6 C1 109.6(2) . . no N1 C7 C8 124.0(3) . . no C17 C8 C9 119.8(3) . . no C17 C8 C7 121.9(3) . . no C9 C8 C7 117.8(3) . . no C10 C9 C8 120.8(3) . . no C9 C10 C15 117.9(3) . . no C9 C10 C11 122.5(3) . . no C15 C10 C11 119.6(3) . . no C13 C11 C14 108.7(3) . . no C13 C11 C12 108.5(3) . . no C14 C11 C12 109.4(3) . . no C13 C11 C10 108.6(3) . . no C14 C11 C10 109.0(2) . . no C12 C11 C10 112.6(3) . . no C16 C15 C10 122.6(3) . . no C15 C16 C17 119.6(3) . . no C15 C16 C18 118.6(3) . . no C17 C16 C18 121.6(3) . . no O1 C17 C16 120.5(3) . . no O1 C17 C8 120.4(3) . . no C16 C17 C8 119.1(3) . . no N2 C18 C16 125.1(3) . . no N2 C19 C20 114.90(19) . . no N2 C19 C24 109.34(17) . . no C20 C19 C24 108.20(19) . . no C21 C20 C19 111.9(2) . . no C20 C21 C22 111.9(2) . . no C23 C22 C21 111.5(2) . . no C24 C23 C22 110.4(2) . . no N3 C24 C23 118.4(2) . . no N3 C24 C19 108.71(18) . . no C23 C24 C19 110.09(19) . . no N3 C25 C26 125.5(3) . . no C27 C26 C35 118.9(3) . . no C27 C26 C25 119.3(3) . . no C35 C26 C25 121.8(3) . . no C26 C27 C28 124.2(3) . . no C33 C28 C27 116.3(3) . . no C33 C28 C29 119.4(3) . . no C27 C28 C29 124.3(3) . . no C28 C29 C30 112.3(3) . . no C28 C29 C31 109.4(3) . . no C30 C29 C31 107.8(3) . . no C28 C29 C32 109.5(3) . . no C30 C29 C32 108.3(3) . . no C31 C29 C32 109.5(3) . . no C28 C33 C34 123.5(3) . . no C33 C34 C35 118.5(3) . . no C33 C34 C36 118.4(3) . . no C35 C34 C36 123.1(3) . . no O2 C35 C26 121.3(3) . . no O2 C35 C34 120.2(3) . . no C26 C35 C34 118.5(3) . . no N4 C36 C34 125.1(3) . . no O42 C40 O41 123.0(3) . . no O42 C40 C41 120.5(3) . . no O41 C40 C41 116.5(3) . . no O44 C42 O43 122.3(3) . . no O44 C42 C43 120.5(3) . . no O43 C42 C43 117.2(3) . . no _diffrn_measured_fraction_theta_max 0.953 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.912 _refine_diff_density_min -0.922 _refine_diff_density_rms 0.078 # Attachment '- complex4a.CIF' data_shcczn2 _database_code_depnum_ccdc_archive 'CCDC 851729' #TrackingRef '- complex4a.CIF' _vrf_PLAT306_I ; PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... OW1 RESPONSE: A water molecule. No O-bonded hydrogen atoms have been localized ; _vrf_PLAT430_I ; PROBLEM: Short Inter D...A Contact OW6 .. OW91 .. 1.73 Ang. RESPONSE: They are disordered water molecules ; _vrf_PLAT601_I ; PROBLEM: Structure Contains Solvent Accessible VOIDS of . 1334 A**3 RESPONSE: Probably occupied by unlocalized disordered solvent molecules ; _vrf_PLAT761_I ; PROBLEM: CIF Contains no X-H Bonds ...................... ? RESPONSE: The data contain only C-bonded H atoms, calculated from geometry and set at standard distances... ; _vrf_PLAT762_I ; PROBLEM: CIF Contains no X-Y-H or H-Y-H Angles .......... ? RESPONSE: ...and angles ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C116 H192 N12 O25 Zn3' _chemical_formula_weight 2350.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 19.17(3) _cell_length_b 24.42(2) _cell_length_c 18.37(3) _cell_angle_alpha 90.00 _cell_angle_beta 113.31(17) _cell_angle_gamma 90.00 _cell_volume 7897(17) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8210 _cell_measurement_theta_min 2.81 _cell_measurement_theta_max 36.85 _exptl_crystal_description irregular _exptl_crystal_colour colourless _exptl_crystal_size_max 0.5032 _exptl_crystal_size_mid 0.4254 _exptl_crystal_size_min 0.3510 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.989 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2524 _exptl_absorpt_coefficient_mu 0.509 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.847 _exptl_absorpt_correction_T_max 0.893 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET) (compiled May 29 2009,17:40:42) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Kuma KM4 with a CCD counter' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 8.3359 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48122 _diffrn_reflns_av_R_equivalents 0.1088 _diffrn_reflns_av_sigmaI/netI 0.3248 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -39 _diffrn_reflns_limit_k_max 41 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.82 _diffrn_reflns_theta_max 36.83 _reflns_number_total 26139 _reflns_number_gt 7720 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET) (compiled May 29 2009,17:40:42) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET) (compiled May 29 2009,17:40:42) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET) (compiled May 29 2009,17:40:42) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.05(2) _refine_ls_number_reflns 26139 _refine_ls_number_parameters 671 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.3311 _refine_ls_R_factor_gt 0.1315 _refine_ls_wR_factor_ref 0.4127 _refine_ls_wR_factor_gt 0.3130 _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_restrained_S_all 0.996 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.0000 0.84223(6) 0.0000 0.0415(4) Uani 1 2 d S . . Zn2 Zn -0.18754(6) 0.61461(4) -0.07704(6) 0.0368(3) Uani 1 1 d . . . O1 O -0.0894(4) 0.8240(3) 0.0222(4) 0.0535(19) Uani 1 1 d . . . O2 O -0.1016(4) 0.5851(3) 0.0125(4) 0.0368(14) Uani 1 1 d . . . O3 O 0.1833(4) 0.6806(3) 0.1308(4) 0.0437(16) Uani 1 1 d . . . N1 N -0.2746(5) 0.7414(3) 0.0118(5) 0.0353(18) Uani 1 1 d . . . N2 N -0.2522(4) 0.6275(3) -0.0161(4) 0.0314(16) Uani 1 1 d . . . N3 N 0.0744(5) 0.4939(3) 0.1460(5) 0.0375(18) Uani 1 1 d . . . N4 N 0.2037(4) 0.5652(3) 0.1694(5) 0.0337(17) Uani 1 1 d . . . N5 N 0.1963(5) 0.8359(3) 0.2087(5) 0.0442(19) Uani 1 1 d . . . N6 N 0.0509(5) 0.8806(3) 0.1113(5) 0.041(2) Uani 1 1 d . . . C1 C -0.0930(6) 0.8194(4) 0.0897(6) 0.040(2) Uani 1 1 d . . . C2 C -0.0427(5) 0.8408(4) 0.1578(7) 0.041(2) Uani 1 1 d . . . C3 C -0.0515(6) 0.8353(4) 0.2323(7) 0.048(3) Uani 1 1 d . . . H3 H -0.0162 0.8516 0.2777 0.057 Uiso 1 1 calc R . . C4 C -0.1135(6) 0.8052(4) 0.2370(6) 0.046(2) Uani 1 1 d . . . C5 C -0.1218(9) 0.7956(6) 0.3131(8) 0.070(4) Uani 1 1 d . . . C6 C -0.2040(10) 0.8166(11) 0.3039(10) 0.125(8) Uani 1 1 d . . . H6A H -0.2101 0.8542 0.2876 0.150 Uiso 1 1 calc R . . H6B H -0.2088 0.8132 0.3538 0.150 Uiso 1 1 calc R . . H6C H -0.2424 0.7949 0.2647 0.150 Uiso 1 1 calc R . . C7 C -0.0626(10) 0.8256(7) 0.3840(8) 0.091(5) Uani 1 1 d . . . H7A H -0.0128 0.8120 0.3931 0.110 Uiso 1 1 calc R . . H7B H -0.0730 0.8194 0.4304 0.110 Uiso 1 1 calc R . . H7C H -0.0648 0.8641 0.3730 0.110 Uiso 1 1 calc R . . C8 C -0.1219(11) 0.7346(7) 0.3321(8) 0.093(5) Uani 1 1 d . . . H8A H -0.1531 0.7152 0.2851 0.112 Uiso 1 1 calc R . . H8B H -0.1416 0.7297 0.3722 0.112 Uiso 1 1 calc R . . H8C H -0.0709 0.7208 0.3510 0.112 Uiso 1 1 calc R . . C9 C -0.1632(6) 0.7837(4) 0.1657(7) 0.047(3) Uani 1 1 d . . . H9 H -0.2047 0.7645 0.1667 0.056 Uiso 1 1 calc R . . C10 C -0.1579(6) 0.7878(4) 0.0943(6) 0.038(2) Uani 1 1 d . . . C11 C -0.2107(6) 0.7632(4) 0.0206(6) 0.038(2) Uani 1 1 d . . . H11 H -0.1973 0.7634 -0.0228 0.045 Uiso 1 1 calc R . . C12 C -0.3170(5) 0.7171(4) -0.0650(5) 0.0312(19) Uani 1 1 d . . . H12 H -0.2888 0.7216 -0.0989 0.037 Uiso 1 1 calc R . . C13 C -0.3941(7) 0.7449(4) -0.1033(7) 0.056(3) Uani 1 1 d . . . H13A H -0.3873 0.7839 -0.1078 0.067 Uiso 1 1 calc R . . H13B H -0.4228 0.7395 -0.0707 0.067 Uiso 1 1 calc R . . C14 C -0.4378(7) 0.7200(5) -0.1868(8) 0.063(3) Uani 1 1 d . . . H14A H -0.4087 0.7244 -0.2192 0.075 Uiso 1 1 calc R . . H14B H -0.4863 0.7384 -0.2129 0.075 Uiso 1 1 calc R . . C15 C -0.4507(7) 0.6580(5) -0.1759(8) 0.060(3) Uani 1 1 d . . . H15A H -0.4767 0.6411 -0.2275 0.072 Uiso 1 1 calc R . . H15B H -0.4824 0.6540 -0.1463 0.072 Uiso 1 1 calc R . . C16 C -0.3729(6) 0.6282(4) -0.1308(5) 0.040(2) Uani 1 1 d . . . H16A H -0.3824 0.5904 -0.1215 0.048 Uiso 1 1 calc R . . H16B H -0.3438 0.6285 -0.1636 0.048 Uiso 1 1 calc R . . C17 C -0.3280(5) 0.6550(4) -0.0537(5) 0.033(2) Uani 1 1 d . . . H17 H -0.3551 0.6509 -0.0187 0.040 Uiso 1 1 calc R . . C18 C -0.2290(4) 0.6165(4) 0.0582(6) 0.036(2) Uani 1 1 d . . . H18 H -0.2617 0.6258 0.0825 0.043 Uiso 1 1 calc R . . C19 C -0.1579(5) 0.5913(3) 0.1083(6) 0.033(2) Uani 1 1 d . . . C20 C -0.1479(6) 0.5819(4) 0.1875(6) 0.038(2) Uani 1 1 d . . . H20 H -0.1863 0.5928 0.2032 0.046 Uiso 1 1 calc R . . C21 C -0.0835(6) 0.5571(4) 0.2434(6) 0.043(2) Uani 1 1 d . . . C22 C -0.0716(7) 0.5486(5) 0.3289(7) 0.056(3) Uani 1 1 d . . . C23 C 0.0012(9) 0.5791(6) 0.3839(8) 0.077(4) Uani 1 1 d . . . H23A H 0.0409 0.5734 0.3653 0.093 Uiso 1 1 calc R . . H23B H 0.0171 0.5652 0.4370 0.093 Uiso 1 1 calc R . . H23C H -0.0093 0.6176 0.3836 0.093 Uiso 1 1 calc R . . C24 C -0.0551(9) 0.4861(5) 0.3513(8) 0.074(4) Uani 1 1 d . . . H24A H -0.0943 0.4641 0.3136 0.089 Uiso 1 1 calc R . . H24B H -0.0541 0.4800 0.4034 0.089 Uiso 1 1 calc R . . H24C H -0.0069 0.4763 0.3507 0.089 Uiso 1 1 calc R . . C25 C -0.1408(9) 0.5679(9) 0.3472(9) 0.097(6) Uani 1 1 d . . . H25A H -0.1384 0.6069 0.3549 0.116 Uiso 1 1 calc R . . H25B H -0.1393 0.5502 0.3945 0.116 Uiso 1 1 calc R . . H25C H -0.1872 0.5585 0.3036 0.116 Uiso 1 1 calc R . . C26 C -0.0275(6) 0.5408(4) 0.2171(6) 0.039(2) Uani 1 1 d . . . H26 H 0.0158 0.5233 0.2524 0.047 Uiso 1 1 calc R . . C27 C -0.0347(6) 0.5500(4) 0.1396(6) 0.042(2) Uani 1 1 d . . . C28 C -0.0987(5) 0.5767(3) 0.0830(5) 0.0301(19) Uani 1 1 d . . . C29 C 0.0243(6) 0.5320(3) 0.1110(6) 0.037(2) Uani 1 1 d . . . H29 H 0.0256 0.5486 0.0660 0.044 Uiso 1 1 calc R . . C30 C 0.1266(5) 0.4812(3) 0.1106(5) 0.0322(19) Uani 1 1 d . . . H30 H 0.1083 0.4978 0.0577 0.039 Uiso 1 1 calc R . . C31 C 0.1325(6) 0.4191(4) 0.1024(7) 0.044(2) Uani 1 1 d . . . H31A H 0.1475 0.4023 0.1542 0.052 Uiso 1 1 calc R . . H31B H 0.0829 0.4048 0.0689 0.052 Uiso 1 1 calc R . . C32 C 0.1900(6) 0.4031(4) 0.0667(7) 0.050(3) Uani 1 1 d . . . H32A H 0.1726 0.4166 0.0127 0.060 Uiso 1 1 calc R . . H32B H 0.1938 0.3636 0.0654 0.060 Uiso 1 1 calc R . . C33 C 0.2690(6) 0.4277(4) 0.1165(7) 0.045(2) Uani 1 1 d . . . H33A H 0.3038 0.4191 0.0915 0.054 Uiso 1 1 calc R . . H33B H 0.2888 0.4113 0.1689 0.054 Uiso 1 1 calc R . . C34 C 0.2642(6) 0.4918(4) 0.1243(6) 0.045(2) Uiso 1 1 d . . . H34A H 0.3139 0.5063 0.1569 0.054 Uiso 1 1 calc R . . H34B H 0.2474 0.5086 0.0724 0.054 Uiso 1 1 calc R . . C35 C 0.2080(6) 0.5050(3) 0.1622(6) 0.037(2) Uani 1 1 d . . . H35 H 0.2263 0.4886 0.2152 0.044 Uiso 1 1 calc R . . C36 C 0.2011(6) 0.5828(4) 0.2326(7) 0.046(3) Uani 1 1 d . . . H36 H 0.2011 0.5564 0.2691 0.055 Uiso 1 1 calc R . . C37 C 0.1981(6) 0.6395(4) 0.2555(6) 0.043(2) Uani 1 1 d . . . C38 C 0.2004(7) 0.6475(4) 0.3325(7) 0.056(3) Uani 1 1 d . . . H38 H 0.2046 0.6172 0.3646 0.067 Uiso 1 1 calc R . . C39 C 0.1965(8) 0.7007(5) 0.3626(7) 0.067(3) Uani 1 1 d . . . C40 C 0.1934(12) 0.7078(7) 0.4447(8) 0.095(5) Uani 1 1 d . . . C41 C 0.2016(13) 0.6587(8) 0.4871(9) 0.113(7) Uani 1 1 d . . . H41A H 0.2120 0.6667 0.5415 0.136 Uiso 1 1 calc R . . H41B H 0.2430 0.6379 0.4841 0.136 Uiso 1 1 calc R . . H41C H 0.1556 0.6377 0.4646 0.136 Uiso 1 1 calc R . . C42 C 0.1251(16) 0.7389(9) 0.4368(12) 0.154(11) Uani 1 1 d . . . H42A H 0.0854 0.7315 0.3860 0.184 Uiso 1 1 calc R . . H42B H 0.1365 0.7773 0.4415 0.184 Uiso 1 1 calc R . . H42C H 0.1089 0.7280 0.4779 0.184 Uiso 1 1 calc R . . C43 C 0.2548(17) 0.7507(14) 0.4858(17) 0.183(11) Uiso 1 1 d . . . H43A H 0.2322 0.7818 0.4998 0.219 Uiso 1 1 calc R . . H43B H 0.2779 0.7619 0.4504 0.219 Uiso 1 1 calc R . . H43C H 0.2927 0.7351 0.5328 0.219 Uiso 1 1 calc R . . C44 C 0.1921(7) 0.7435(4) 0.3127(7) 0.056(3) Uani 1 1 d . . . H44 H 0.1914 0.7787 0.3318 0.067 Uiso 1 1 calc R . . C45 C 0.1885(6) 0.7387(4) 0.2372(6) 0.041(2) Uani 1 1 d . . . C46 C 0.1909(6) 0.6852(4) 0.2049(6) 0.039(2) Uani 1 1 d . . . C47 C 0.1849(6) 0.7852(4) 0.1848(6) 0.042(2) Uani 1 1 d . . . H47 H 0.1738 0.7779 0.1316 0.051 Uiso 1 1 calc R . . C48 C 0.1878(5) 0.8749(4) 0.1460(5) 0.036(2) Uani 1 1 d . . . H48 H 0.1799 0.8554 0.0967 0.043 Uiso 1 1 calc R . . C49 C 0.2616(6) 0.9114(4) 0.1715(7) 0.052(3) Uani 1 1 d . . . H49A H 0.2698 0.9304 0.2206 0.063 Uiso 1 1 calc R . . H49B H 0.3056 0.8886 0.1801 0.063 Uiso 1 1 calc R . . C50 C 0.2510(7) 0.9528(4) 0.1054(8) 0.060(3) Uani 1 1 d . . . H50A H 0.2967 0.9748 0.1194 0.072 Uiso 1 1 calc R . . H50B H 0.2432 0.9334 0.0567 0.072 Uiso 1 1 calc R . . C51 C 0.1859(7) 0.9889(4) 0.0925(9) 0.064(3) Uani 1 1 d . . . H51A H 0.1812 1.0160 0.0523 0.076 Uiso 1 1 calc R . . H51B H 0.1922 1.0078 0.1412 0.076 Uiso 1 1 calc R . . C52 C 0.1085(6) 0.9487(5) 0.0628(7) 0.057(3) Uani 1 1 d . . . H52A H 0.0627 0.9706 0.0483 0.069 Uiso 1 1 calc R . . H52B H 0.1050 0.9266 0.0176 0.069 Uiso 1 1 calc R . . C53 C 0.1195(5) 0.9134(4) 0.1332(6) 0.039(2) Uani 1 1 d . . . H53 H 0.1280 0.9356 0.1805 0.047 Uiso 1 1 calc R . . C54 C 0.0251(6) 0.8725(4) 0.1649(7) 0.039(2) Uani 1 1 d . . . H54 H 0.0523 0.8884 0.2140 0.047 Uiso 1 1 calc R . . O10 O -0.5406(8) 0.9110(6) -0.2276(8) 0.115(4) Uiso 1 1 d . . . C60 C -0.4708(11) 0.8904(8) -0.1741(11) 0.100(5) Uiso 1 1 d . . . O11 O 0.1510(6) 0.2273(4) 0.1105(6) 0.088(3) Uani 1 1 d . . . C61 C 0.0983(8) 0.2696(6) 0.1050(9) 0.079(4) Uani 1 1 d . . . O12 O 0.0884(15) 0.9151(11) 0.3805(16) 0.218(9) Uiso 1 1 d . . . C62 C 0.1119(15) 0.9094(11) 0.4617(16) 0.140(8) Uiso 1 1 d . . . O13 O -0.3979(17) 0.6679(13) -0.3648(17) 0.130(9) Uiso 0.50 1 d P . . C63 C -0.468(3) 0.691(2) -0.405(3) 0.124(13) Uiso 0.50 1 d P . . O14 O -0.0066(18) 0.6913(15) 0.1463(19) 0.141(10) Uiso 0.50 1 d P . . C64 C -0.0497(19) 0.6958(12) 0.0639(17) 0.070(7) Uiso 0.50 1 d P . . OW1 O 0.2157(12) 0.8824(5) 0.3509(8) 0.153(7) Uani 1 1 d . . . OW2 O 0.1877(13) 0.1484(9) 0.2132(14) 0.085(6) Uiso 0.50 1 d P . . OW22 O 0.1767(15) 0.1543(11) 0.2723(16) 0.115(8) Uiso 0.50 1 d P . . OW3 O 0.196(3) 0.486(2) 0.399(3) 0.203(16) Uiso 0.50 1 d P . . OW4 O -0.511(2) 0.5131(17) -0.218(2) 0.163(12) Uiso 0.50 1 d P . . OW5 O -0.0023(19) 0.7024(14) 0.0772(18) 0.132(10) Uiso 0.50 1 d P . . OW6 O -0.5309(16) 0.6017(14) -0.0274(17) 0.136(11) Uiso 0.50 1 d P . . OW7 O -0.474(2) 0.5760(16) -0.034(2) 0.144(11) Uiso 0.50 1 d P . . OW8 O -0.116(2) 0.9959(19) 0.355(2) 0.182(14) Uiso 0.50 1 d P . . OW9 O 0.148(2) 0.1266(15) 0.168(2) 0.067(9) Uiso 0.25 1 d P . . OW91 O -0.616(3) 0.610(2) -0.108(3) 0.100(13) Uiso 0.25 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0403(10) 0.0328(8) 0.0619(11) 0.000 0.0315(9) 0.000 Zn2 0.0430(6) 0.0261(5) 0.0492(6) 0.0025(5) 0.0267(5) 0.0019(5) O1 0.054(5) 0.053(4) 0.064(5) 0.002(4) 0.035(4) -0.020(4) O2 0.037(4) 0.035(3) 0.040(4) 0.002(3) 0.018(3) 0.008(3) O3 0.054(4) 0.028(3) 0.059(4) -0.003(3) 0.033(4) 0.004(3) N1 0.042(5) 0.027(4) 0.047(5) 0.006(3) 0.028(4) 0.008(3) N2 0.037(4) 0.018(3) 0.044(4) -0.004(3) 0.021(4) -0.006(3) N3 0.045(5) 0.024(3) 0.057(5) 0.007(3) 0.035(4) 0.006(3) N4 0.034(5) 0.025(4) 0.040(4) 0.010(3) 0.012(4) 0.006(3) N5 0.048(5) 0.031(4) 0.062(5) -0.007(4) 0.031(4) -0.005(4) N6 0.050(5) 0.019(3) 0.069(6) 0.003(4) 0.038(5) 0.001(3) C1 0.046(6) 0.025(4) 0.056(6) 0.001(4) 0.028(5) -0.003(4) C2 0.028(5) 0.026(4) 0.073(7) 0.001(5) 0.023(5) 0.005(4) C3 0.041(6) 0.039(5) 0.069(7) -0.019(5) 0.028(5) -0.009(5) C4 0.058(7) 0.037(5) 0.052(6) 0.008(5) 0.032(6) 0.005(5) C5 0.094(10) 0.060(8) 0.066(8) -0.008(6) 0.041(8) -0.021(7) C6 0.096(13) 0.22(3) 0.073(10) -0.029(12) 0.051(10) -0.006(14) C7 0.122(14) 0.088(11) 0.071(9) -0.029(8) 0.047(9) -0.036(10) C8 0.146(15) 0.093(11) 0.049(7) -0.006(7) 0.048(9) -0.044(10) C9 0.055(7) 0.026(4) 0.073(7) 0.006(5) 0.041(6) -0.004(4) C10 0.038(6) 0.035(5) 0.047(6) 0.003(4) 0.025(5) -0.003(4) C11 0.058(7) 0.033(4) 0.039(5) 0.011(4) 0.038(5) 0.010(4) C12 0.030(5) 0.034(4) 0.034(5) 0.008(4) 0.017(4) 0.010(4) C13 0.079(9) 0.038(5) 0.057(7) 0.014(5) 0.033(6) 0.029(6) C14 0.053(8) 0.061(8) 0.072(8) 0.016(6) 0.022(6) 0.027(6) C15 0.047(7) 0.053(7) 0.073(8) -0.003(6) 0.017(6) -0.007(5) C16 0.046(6) 0.039(5) 0.034(5) 0.000(4) 0.014(4) -0.003(4) C17 0.029(5) 0.033(4) 0.040(5) 0.008(4) 0.018(4) -0.001(4) C18 0.023(4) 0.017(3) 0.078(6) 0.002(5) 0.031(4) 0.001(4) C19 0.036(5) 0.016(3) 0.060(6) 0.002(4) 0.032(5) -0.001(3) C20 0.046(6) 0.034(5) 0.045(6) 0.001(4) 0.028(5) -0.002(4) C21 0.049(6) 0.036(5) 0.056(6) 0.004(5) 0.033(5) 0.004(4) C22 0.061(8) 0.055(6) 0.071(8) -0.004(6) 0.046(7) 0.005(6) C23 0.098(11) 0.082(10) 0.064(8) -0.017(7) 0.045(8) -0.007(8) C24 0.105(11) 0.060(8) 0.072(8) 0.019(7) 0.050(8) 0.008(7) C25 0.092(12) 0.151(16) 0.072(9) 0.012(10) 0.059(9) 0.018(11) C26 0.036(6) 0.031(5) 0.054(6) 0.001(4) 0.023(5) 0.001(4) C27 0.038(6) 0.031(4) 0.065(7) -0.008(4) 0.031(5) -0.001(4) C28 0.030(5) 0.020(3) 0.046(5) 0.000(4) 0.020(4) 0.005(3) C29 0.042(6) 0.026(4) 0.049(6) -0.001(4) 0.026(5) 0.002(4) C30 0.038(5) 0.026(4) 0.033(5) 0.003(3) 0.015(4) 0.002(4) C31 0.048(6) 0.027(4) 0.066(7) 0.009(4) 0.034(5) 0.009(4) C32 0.044(6) 0.023(4) 0.094(8) 0.006(5) 0.038(6) 0.011(4) C33 0.043(6) 0.037(5) 0.061(7) 0.001(5) 0.026(5) 0.000(4) C35 0.048(6) 0.022(4) 0.041(5) 0.009(4) 0.020(5) 0.014(4) C36 0.049(7) 0.027(5) 0.067(7) 0.005(5) 0.028(6) -0.001(4) C37 0.041(6) 0.038(5) 0.045(6) 0.002(4) 0.012(5) 0.006(4) C38 0.079(9) 0.038(6) 0.059(7) 0.010(5) 0.037(7) 0.010(5) C39 0.089(10) 0.062(8) 0.058(7) -0.003(6) 0.040(7) -0.001(7) C40 0.173(18) 0.065(9) 0.064(9) -0.015(7) 0.066(11) -0.004(10) C41 0.19(2) 0.102(14) 0.056(9) -0.021(9) 0.064(12) -0.036(13) C42 0.28(3) 0.124(17) 0.105(14) 0.029(12) 0.131(19) 0.074(19) C44 0.084(9) 0.034(5) 0.061(7) -0.001(5) 0.040(7) 0.002(5) C45 0.049(6) 0.026(4) 0.054(6) -0.001(4) 0.026(5) 0.000(4) C46 0.047(6) 0.029(4) 0.051(6) 0.008(4) 0.030(5) 0.006(4) C47 0.068(7) 0.039(5) 0.035(5) 0.002(4) 0.036(5) 0.009(5) C48 0.045(6) 0.028(4) 0.042(5) -0.009(4) 0.025(5) -0.008(4) C49 0.047(7) 0.044(6) 0.075(8) -0.026(5) 0.034(6) -0.009(5) C50 0.067(8) 0.035(5) 0.106(10) -0.020(6) 0.065(8) -0.012(5) C51 0.068(8) 0.026(5) 0.109(10) 0.001(6) 0.049(8) -0.015(5) C52 0.036(6) 0.090(8) 0.061(7) 0.062(6) 0.035(5) 0.038(6) C53 0.035(5) 0.025(4) 0.061(6) -0.002(4) 0.022(5) -0.003(4) C54 0.042(6) 0.025(4) 0.056(6) -0.011(4) 0.025(5) 0.002(4) O11 0.087(7) 0.098(8) 0.114(8) 0.027(6) 0.075(7) 0.020(6) C61 0.083(10) 0.070(9) 0.114(11) 0.015(8) 0.070(9) 0.025(7) OW1 0.31(2) 0.085(8) 0.111(9) -0.036(7) 0.134(12) -0.062(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O1 1.963(7) . ? Zn1 O1 1.963(7) 2 ? Zn1 N6 2.105(9) . ? Zn1 N6 2.105(9) 2 ? Zn2 O3 1.907(6) 2 ? Zn2 O2 1.947(8) . ? Zn2 N2 1.997(7) . ? Zn2 N4 2.004(7) 2 ? O1 C1 1.273(11) . ? O2 C28 1.291(10) . ? O3 C46 1.315(11) . ? O3 Zn2 1.907(6) 2 ? N1 C11 1.285(12) . ? N1 C12 1.448(12) . ? N2 C18 1.284(12) . ? N2 C17 1.498(12) . ? N3 C29 1.309(12) . ? N3 C30 1.426(11) . ? N4 C36 1.257(13) . ? N4 C35 1.481(11) . ? N4 Zn2 2.004(7) 2 ? N5 C47 1.303(12) . ? N5 C48 1.452(12) . ? N6 C54 1.279(12) . ? N6 C53 1.454(12) . ? C1 C2 1.347(15) . ? C1 C10 1.496(13) . ? C2 C3 1.450(15) . ? C2 C54 1.474(14) . ? C3 C4 1.429(14) . ? C4 C9 1.383(15) . ? C4 C5 1.488(15) . ? C5 C8 1.53(2) . ? C5 C7 1.53(2) . ? C5 C6 1.60(2) . ? C9 C10 1.358(13) . ? C10 C11 1.460(15) . ? C12 C13 1.523(14) . ? C12 C17 1.555(12) . ? C13 C14 1.552(18) . ? C14 C15 1.559(17) . ? C15 C16 1.568(16) . ? C16 C17 1.486(13) . ? C18 C19 1.447(14) . ? C19 C20 1.408(13) . ? C19 C28 1.430(11) . ? C20 C21 1.393(15) . ? C21 C26 1.399(13) . ? C21 C22 1.509(15) . ? C22 C23 1.553(19) . ? C22 C25 1.565(17) . ? C22 C24 1.581(17) . ? C26 C27 1.394(14) . ? C27 C28 1.415(14) . ? C27 C29 1.489(12) . ? C30 C31 1.532(12) . ? C30 C35 1.582(14) . ? C31 C32 1.539(13) . ? C32 C33 1.547(16) . ? C33 C34 1.578(14) . ? C34 C35 1.531(13) . ? C36 C37 1.454(14) . ? C37 C46 1.424(14) . ? C37 C38 1.412(15) . ? C38 C39 1.425(17) . ? C39 C44 1.370(16) . ? C39 C40 1.543(17) . ? C40 C41 1.41(2) . ? C40 C42 1.47(3) . ? C40 C43 1.53(3) . ? C44 C45 1.365(14) . ? C45 C46 1.445(13) . ? C45 C47 1.472(13) . ? C48 C53 1.553(13) . ? C48 C49 1.580(14) . ? C49 C50 1.531(17) . ? C50 C51 1.470(17) . ? C51 C52 1.679(17) . ? C52 C53 1.497(13) . ? O10 C60 1.40(2) . ? O11 C61 1.419(15) . ? O12 C62 1.38(3) . ? O13 C63 1.37(5) . ? O14 OW5 1.33(4) . ? O14 C64 1.41(4) . ? C64 OW5 0.86(4) . ? OW2 OW9 1.03(4) . ? OW2 OW22 1.19(3) . ? OW6 OW6 1.21(5) 2_455 ? OW6 OW7 1.26(4) 2_455 ? OW6 OW7 1.30(4) . ? OW6 OW91 1.73(6) . ? OW7 OW6 1.26(4) 2_455 ? OW9 OW91 1.10(5) 4_445 ? OW91 OW9 1.10(5) 4_455 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn1 O1 153.8(5) . 2 ? O1 Zn1 N6 90.4(3) . . ? O1 Zn1 N6 101.2(3) 2 . ? O1 Zn1 N6 101.2(3) . 2 ? O1 Zn1 N6 90.4(3) 2 2 ? N6 Zn1 N6 127.2(4) . 2 ? O3 Zn2 O2 123.6(3) 2 . ? O3 Zn2 N2 108.6(3) 2 . ? O2 Zn2 N2 95.2(3) . . ? O3 Zn2 N4 95.4(3) 2 2 ? O2 Zn2 N4 106.7(3) . 2 ? N2 Zn2 N4 130.3(3) . 2 ? C1 O1 Zn1 127.6(7) . . ? C28 O2 Zn2 126.3(5) . . ? C46 O3 Zn2 126.7(6) . 2 ? C11 N1 C12 115.7(7) . . ? C18 N2 C17 116.6(7) . . ? C18 N2 Zn2 122.1(6) . . ? C17 N2 Zn2 121.1(5) . . ? C29 N3 C30 116.2(7) . . ? C36 N4 C35 116.5(7) . . ? C36 N4 Zn2 121.8(7) . 2 ? C35 N4 Zn2 121.2(6) . 2 ? C47 N5 C48 113.9(8) . . ? C54 N6 C53 117.1(9) . . ? C54 N6 Zn1 120.4(7) . . ? C53 N6 Zn1 122.3(6) . . ? O1 C1 C2 125.1(9) . . ? O1 C1 C10 117.9(9) . . ? C2 C1 C10 117.0(9) . . ? C1 C2 C3 122.2(9) . . ? C1 C2 C54 124.6(9) . . ? C3 C2 C54 113.2(9) . . ? C4 C3 C2 121.0(10) . . ? C9 C4 C3 114.6(9) . . ? C9 C4 C5 122.6(10) . . ? C3 C4 C5 122.7(11) . . ? C4 C5 C8 112.3(10) . . ? C4 C5 C7 113.8(11) . . ? C8 C5 C7 109.8(13) . . ? C4 C5 C6 108.5(12) . . ? C8 C5 C6 104.3(14) . . ? C7 C5 C6 107.7(12) . . ? C10 C9 C4 126.8(9) . . ? C9 C10 C11 125.1(8) . . ? C9 C10 C1 118.4(9) . . ? C11 C10 C1 116.5(8) . . ? N1 C11 C10 124.3(7) . . ? N1 C12 C13 109.6(7) . . ? N1 C12 C17 108.9(7) . . ? C13 C12 C17 109.8(8) . . ? C12 C13 C14 109.2(8) . . ? C13 C14 C15 107.8(10) . . ? C14 C15 C16 110.6(9) . . ? C17 C16 C15 111.8(8) . . ? C16 C17 N2 109.5(7) . . ? C16 C17 C12 111.1(7) . . ? N2 C17 C12 109.9(7) . . ? N2 C18 C19 127.4(7) . . ? C20 C19 C28 119.6(9) . . ? C20 C19 C18 115.8(8) . . ? C28 C19 C18 124.6(8) . . ? C21 C20 C19 123.4(8) . . ? C20 C21 C26 116.6(9) . . ? C20 C21 C22 123.5(8) . . ? C26 C21 C22 119.9(10) . . ? C21 C22 C23 109.8(9) . . ? C21 C22 C25 113.0(11) . . ? C23 C22 C25 109.6(11) . . ? C21 C22 C24 109.7(9) . . ? C23 C22 C24 104.9(11) . . ? C25 C22 C24 109.5(11) . . ? C27 C26 C21 121.8(10) . . ? C26 C27 C28 122.0(8) . . ? C26 C27 C29 122.0(9) . . ? C28 C27 C29 115.9(9) . . ? O2 C28 C27 119.4(7) . . ? O2 C28 C19 124.1(8) . . ? C27 C28 C19 116.5(8) . . ? N3 C29 C27 123.3(8) . . ? N3 C30 C31 110.7(7) . . ? N3 C30 C35 110.5(7) . . ? C31 C30 C35 109.2(7) . . ? C32 C31 C30 112.7(7) . . ? C31 C32 C33 110.5(9) . . ? C32 C33 C34 111.0(8) . . ? C35 C34 C33 109.2(8) . . ? N4 C35 C30 110.0(7) . . ? N4 C35 C34 108.9(7) . . ? C30 C35 C34 110.8(8) . . ? N4 C36 C37 127.8(9) . . ? C46 C37 C38 120.1(9) . . ? C46 C37 C36 124.2(9) . . ? C38 C37 C36 115.7(9) . . ? C39 C38 C37 122.0(10) . . ? C44 C39 C38 115.8(10) . . ? C44 C39 C40 123.5(12) . . ? C38 C39 C40 120.6(11) . . ? C41 C40 C42 113.3(18) . . ? C41 C40 C43 114.5(19) . . ? C42 C40 C43 100.3(18) . . ? C41 C40 C39 113.9(13) . . ? C42 C40 C39 109.8(14) . . ? C43 C40 C39 103.8(16) . . ? C39 C44 C45 125.4(10) . . ? C44 C45 C46 119.9(9) . . ? C44 C45 C47 124.7(9) . . ? C46 C45 C47 115.4(8) . . ? O3 C46 C37 123.5(8) . . ? O3 C46 C45 119.6(8) . . ? C37 C46 C45 116.8(9) . . ? N5 C47 C45 123.6(8) . . ? N5 C48 C53 109.9(7) . . ? N5 C48 C49 109.2(8) . . ? C53 C48 C49 107.8(7) . . ? C50 C49 C48 108.4(9) . . ? C51 C50 C49 111.2(9) . . ? C50 C51 C52 106.7(9) . . ? C53 C52 C51 104.6(9) . . ? N6 C53 C52 106.0(9) . . ? N6 C53 C48 108.9(7) . . ? C52 C53 C48 107.6(7) . . ? N6 C54 C2 127.6(10) . . ? OW5 O14 C64 36.3(18) . . ? OW5 C64 O14 67(3) . . ? OW9 OW2 OW22 117(3) . . ? C64 OW5 O14 77(4) . . ? OW6 OW6 OW7 63(2) 2_455 2_455 ? OW6 OW6 OW7 60(2) 2_455 . ? OW7 OW6 OW7 94(4) 2_455 . ? OW6 OW6 OW91 172(3) 2_455 . ? OW7 OW6 OW91 123(3) 2_455 . ? OW7 OW6 OW91 121(3) . . ? OW6 OW7 OW6 56(3) 2_455 . ? OW2 OW9 OW91 159(5) . 4_445 ? OW9 OW91 OW6 150(4) 4_455 . ? _diffrn_measured_fraction_theta_max 0.791 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 3.396 _refine_diff_density_min -0.975 _refine_diff_density_rms 0.168 # Attachment '- complex4b.CIF' data_rthccznb _database_code_depnum_ccdc_archive 'CCDC 851730' #TrackingRef '- complex4b.CIF' _vrf_PLAT306_I ; PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .....OW2 through OW5 RESPONSE: A water molecule. No O-bonded hydrogen atoms have been localized ; _vrf_PLAT430_I ; PROBLEM: Short Inter D...A Contact OW7 .. OW9 .. 2.26 Ang. RESPONSE: They are disordered water molecules ; _vrf_PLAT761_I ; PROBLEM: CIF Contains no X-H Bonds ...................... ? RESPONSE: The data contain only C-bonded H atoms, calculated from geometry and set at standard distances... ; _vrf_PLAT762_I ; PROBLEM: CIF Contains no X-Y-H or H-Y-H Angles .......... ? RESPONSE: ...and angles ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C115.50 H172 Cl21 N12 O20 Zn3' _chemical_formula_weight 2989.21 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 29.114(11) _cell_length_b 18.422(5) _cell_length_c 17.181(6) _cell_angle_alpha 90.00 _cell_angle_beta 125.19(5) _cell_angle_gamma 90.00 _cell_volume 7531(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 12620 _cell_measurement_theta_min 2.79 _cell_measurement_theta_max 28.69 _exptl_crystal_description irregular _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.5623 _exptl_crystal_size_mid 0.4645 _exptl_crystal_size_min 0.1757 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.318 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3112 _exptl_absorpt_coefficient_mu 0.907 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.691 _exptl_absorpt_correction_T_max 0.880 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET) (compiled May 29 2009,17:40:42) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Kuma KM4 with a CCD counter' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 8.3359 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27161 _diffrn_reflns_av_R_equivalents 0.0271 _diffrn_reflns_av_sigmaI/netI 0.0669 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.80 _diffrn_reflns_theta_max 28.75 _reflns_number_total 16403 _reflns_number_gt 11124 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET) (compiled May 29 2009,17:40:42) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET) (compiled May 29 2009,17:40:42) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET) (compiled May 29 2009,17:40:42) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.053(19) _refine_ls_number_reflns 16403 _refine_ls_number_parameters 777 _refine_ls_number_restraints 34 _refine_ls_R_factor_all 0.1344 _refine_ls_R_factor_gt 0.1002 _refine_ls_wR_factor_ref 0.2677 _refine_ls_wR_factor_gt 0.2545 _refine_ls_goodness_of_fit_ref 1.654 _refine_ls_restrained_S_all 1.682 _refine_ls_shift/su_max 0.013 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.5000 0.16134(8) 0.0000 0.0349(3) Uani 1 2 d S . . Zn2 Zn 0.36781(3) -0.14047(5) -0.13702(5) 0.0292(2) Uani 1 1 d . . . O1 O 0.4446(2) 0.1101(3) 0.0058(4) 0.0372(13) Uani 1 1 d . . . O2 O 0.4244(2) -0.1818(3) -0.0154(4) 0.0335(13) Uani 1 1 d . . . O3 O 0.6255(2) -0.0551(3) 0.1940(4) 0.0388(14) Uani 1 1 d . . . N1 N 0.2953(3) 0.0289(4) -0.0816(5) 0.0298(14) Uani 1 1 d . . . N2 N 0.3100(2) -0.1249(3) -0.1092(4) 0.0279(14) Uani 1 1 d . . . N3 N 0.5498(3) -0.3015(3) 0.1864(4) 0.0276(13) Uani 1 1 d . . . N4 N 0.6446(3) -0.2088(4) 0.2391(4) 0.0324(15) Uani 1 1 d . . . N5 N 0.6407(3) 0.1499(4) 0.2811(5) 0.0423(17) Uani 1 1 d . . . N6 N 0.5349(3) 0.2144(4) 0.1234(5) 0.0369(16) Uani 1 1 d . . . C1 C 0.4267(3) 0.1323(5) 0.0564(5) 0.0310(17) Uani 1 1 d . . . C2 C 0.4562(4) 0.1831(5) 0.1325(6) 0.039(2) Uani 1 1 d . . . C3 C 0.4334(4) 0.2028(5) 0.1827(7) 0.044(2) Uani 1 1 d . . . H3 H 0.4534 0.2349 0.2335 0.053 Uiso 1 1 calc R . . C4 C 0.3822(4) 0.1764(5) 0.1600(7) 0.046(2) Uani 1 1 d . . . C5 C 0.3561(5) 0.2032(7) 0.2090(10) 0.080(4) Uani 1 1 d . . . C6 C 0.2957(6) 0.2390(9) 0.1312(10) 0.093(5) Uani 1 1 d . . . H6A H 0.2781 0.2129 0.0722 0.111 Uiso 1 1 calc R . . H6B H 0.3008 0.2888 0.1212 0.111 Uiso 1 1 calc R . . H6C H 0.2724 0.2366 0.1539 0.111 Uiso 1 1 calc R . . C7 C 0.3878(5) 0.2647(6) 0.2777(9) 0.067(4) Uani 1 1 d . . . H7A H 0.3778 0.2676 0.3219 0.081 Uiso 1 1 calc R . . H7B H 0.3783 0.3095 0.2431 0.081 Uiso 1 1 calc R . . H7C H 0.4274 0.2562 0.3118 0.081 Uiso 1 1 calc R . . C8 C 0.3404(6) 0.1473(8) 0.2454(10) 0.081(4) Uani 1 1 d . . . H8A H 0.3735 0.1257 0.2998 0.098 Uiso 1 1 calc R . . H8B H 0.3194 0.1110 0.1972 0.098 Uiso 1 1 calc R . . H8C H 0.3175 0.1671 0.2640 0.098 Uiso 1 1 calc R . . C9 C 0.3530(4) 0.1287(5) 0.0826(6) 0.040(2) Uani 1 1 d . . . H9 H 0.3179 0.1118 0.0639 0.048 Uiso 1 1 calc R . . C10 C 0.3744(3) 0.1063(5) 0.0337(5) 0.0346(18) Uani 1 1 d . . . C11 C 0.3419(3) 0.0588(5) -0.0517(5) 0.0319(17) Uani 1 1 d . . . H11 H 0.3571 0.0503 -0.0859 0.038 Uiso 1 1 calc R . . C12 C 0.2687(3) -0.0045(5) -0.1763(5) 0.0351(19) Uani 1 1 d . . . H12 H 0.2932 0.0019 -0.1976 0.042 Uiso 1 1 calc R . . C13 C 0.2127(3) 0.0342(5) -0.2461(6) 0.039(2) Uani 1 1 d . . . H13A H 0.1884 0.0288 -0.2247 0.047 Uiso 1 1 calc R . . H13B H 0.2194 0.0856 -0.2473 0.047 Uiso 1 1 calc R . . C14 C 0.1838(4) 0.0033(6) -0.3452(6) 0.049(2) Uani 1 1 d . . . H14A H 0.2069 0.0117 -0.3682 0.059 Uiso 1 1 calc R . . H14B H 0.1482 0.0279 -0.3877 0.059 Uiso 1 1 calc R . . C15 C 0.1733(3) -0.0786(5) -0.3463(5) 0.0376(19) Uani 1 1 d . . . H15A H 0.1571 -0.0979 -0.4096 0.045 Uiso 1 1 calc R . . H15B H 0.1469 -0.0870 -0.3300 0.045 Uiso 1 1 calc R . . C16 C 0.2293(3) -0.1178(5) -0.2739(5) 0.0345(19) Uani 1 1 d . . . H16A H 0.2221 -0.1691 -0.2726 0.041 Uiso 1 1 calc R . . H16B H 0.2542 -0.1132 -0.2939 0.041 Uiso 1 1 calc R . . C17 C 0.2574(3) -0.0863(5) -0.1752(5) 0.0307(17) Uani 1 1 d . . . H17 H 0.2325 -0.0926 -0.1545 0.037 Uiso 1 1 calc R . . C18 C 0.3196(3) -0.1489(5) -0.0295(5) 0.0286(16) Uani 1 1 d . . . H18 H 0.2920 -0.1389 -0.0199 0.034 Uiso 1 1 calc R . . C19 C 0.3676(3) -0.1889(4) 0.0454(5) 0.0273(16) Uani 1 1 d . . . C20 C 0.3640(3) -0.2116(4) 0.1189(5) 0.0267(15) Uani 1 1 d . . . H20 H 0.3316 -0.2002 0.1152 0.032 Uiso 1 1 calc R . . C21 C 0.4070(3) -0.2513(4) 0.1991(5) 0.0278(17) Uani 1 1 d . . . C22 C 0.4035(4) -0.2744(5) 0.2800(5) 0.039(2) Uani 1 1 d . . . C23 C 0.4141(5) -0.3550(6) 0.2980(8) 0.061(3) Uani 1 1 d . . . H23A H 0.4073 -0.3698 0.3441 0.073 Uiso 1 1 calc R . . H23B H 0.4524 -0.3655 0.3218 0.073 Uiso 1 1 calc R . . H23C H 0.3893 -0.3810 0.2396 0.073 Uiso 1 1 calc R . . C24 C 0.4464(4) -0.2327(7) 0.3688(6) 0.055(3) Uani 1 1 d . . . H24A H 0.4340 -0.1834 0.3629 0.066 Uiso 1 1 calc R . . H24B H 0.4818 -0.2333 0.3768 0.066 Uiso 1 1 calc R . . H24C H 0.4506 -0.2548 0.4231 0.066 Uiso 1 1 calc R . . C25 C 0.3442(4) -0.2629(6) 0.2551(7) 0.051(3) Uani 1 1 d . . . H25A H 0.3340 -0.2127 0.2401 0.062 Uiso 1 1 calc R . . H25B H 0.3436 -0.2765 0.3085 0.062 Uiso 1 1 calc R . . H25C H 0.3179 -0.2923 0.2011 0.062 Uiso 1 1 calc R . . C26 C 0.4553(3) -0.2668(4) 0.2009(5) 0.0276(15) Uani 1 1 d . . . H26 H 0.4847 -0.2929 0.2517 0.033 Uiso 1 1 calc R . . C27 C 0.4597(3) -0.2433(4) 0.1270(5) 0.0257(15) Uani 1 1 d . . . C28 C 0.4169(3) -0.2025(5) 0.0495(5) 0.0277(16) Uani 1 1 d . . . C29 C 0.5085(3) -0.2647(4) 0.1262(5) 0.0240(15) Uani 1 1 d . . . H29 H 0.5081 -0.2487 0.0745 0.029 Uiso 1 1 calc R . . C30 C 0.5888(3) -0.3195(4) 0.1596(5) 0.0270(16) Uani 1 1 d . . . H30 H 0.5739 -0.2974 0.0975 0.032 Uiso 1 1 calc R . . C31 C 0.5915(4) -0.4003(5) 0.1498(7) 0.042(2) Uani 1 1 d . . . H31A H 0.5540 -0.4186 0.1025 0.050 Uiso 1 1 calc R . . H31B H 0.6050 -0.4235 0.2101 0.050 Uiso 1 1 calc R . . C32 C 0.6305(4) -0.4192(6) 0.1201(9) 0.058(3) Uani 1 1 d . . . H32A H 0.6321 -0.4715 0.1156 0.069 Uiso 1 1 calc R . . H32B H 0.6155 -0.3988 0.0577 0.069 Uiso 1 1 calc R . . C33 C 0.6888(4) -0.3903(6) 0.1904(6) 0.049(2) Uani 1 1 d . . . H33A H 0.7123 -0.4009 0.1686 0.059 Uiso 1 1 calc R . . H33B H 0.7052 -0.4137 0.2517 0.059 Uiso 1 1 calc R . . C34 C 0.6864(3) -0.3086(6) 0.2011(6) 0.045(2) Uani 1 1 d . . . H34A H 0.7240 -0.2906 0.2481 0.054 Uiso 1 1 calc R . . H34B H 0.6728 -0.2852 0.1408 0.054 Uiso 1 1 calc R . . C35 C 0.6483(3) -0.2890(5) 0.2313(5) 0.0310(17) Uani 1 1 d . . . H35 H 0.6636 -0.3108 0.2938 0.037 Uiso 1 1 calc R . . C36 C 0.6508(3) -0.1894(5) 0.3141(6) 0.0324(18) Uani 1 1 d . . . C37 C 0.6502(3) -0.1117(5) 0.3377(6) 0.0362(19) Uani 1 1 d . . . C38 C 0.6633(4) -0.1002(6) 0.4299(6) 0.050(2) Uani 1 1 d . . . H38 H 0.6715 -0.1405 0.4685 0.060 Uiso 1 1 calc R . . C39 C 0.6647(4) -0.0334(6) 0.4655(6) 0.049(2) Uani 1 1 d . . . C40 C 0.6807(5) -0.0265(6) 0.5683(7) 0.061(3) Uani 1 1 d . . . C41 C 0.6743(6) 0.0470(7) 0.5916(8) 0.077(4) Uani 1 1 d . . . H41A H 0.6915 0.0504 0.6588 0.092 Uiso 1 1 calc R . . H41B H 0.6350 0.0585 0.5574 0.092 Uiso 1 1 calc R . . H41C H 0.6921 0.0805 0.5741 0.092 Uiso 1 1 calc R . . C42 C 0.7388(6) -0.0483(7) 0.6408(7) 0.084(4) Uani 1 1 d . . . H42A H 0.7641 -0.0151 0.6403 0.100 Uiso 1 1 calc R . . H42B H 0.7450 -0.0964 0.6272 0.100 Uiso 1 1 calc R . . H42C H 0.7454 -0.0476 0.7023 0.100 Uiso 1 1 calc R . . C43 C 0.6419(9) -0.0789(11) 0.5808(11) 0.122(7) Uani 1 1 d . . . H43A H 0.6631 -0.0974 0.6446 0.146 Uiso 1 1 calc R . . H43B H 0.6293 -0.1185 0.5366 0.146 Uiso 1 1 calc R . . H43C H 0.6101 -0.0523 0.5686 0.146 Uiso 1 1 calc R . . C44 C 0.6549(4) 0.0249(6) 0.4081(6) 0.047(2) Uani 1 1 d . . . H44 H 0.6575 0.0711 0.4322 0.056 Uiso 1 1 calc R . . C45 C 0.6416(4) 0.0194(5) 0.3181(6) 0.043(2) Uani 1 1 d . . . C46 C 0.6378(3) -0.0500(5) 0.2784(5) 0.0334(18) Uani 1 1 d . . . C47 C 0.6323(4) 0.0802(5) 0.2554(6) 0.0379(19) Uani 1 1 d . . . H47 H 0.6197 0.0693 0.1932 0.046 Uiso 1 1 calc R . . C48 C 0.6367(3) 0.1958(5) 0.2098(6) 0.0326(17) Uani 1 1 d . . . H48 H 0.6302 0.1658 0.1573 0.039 Uiso 1 1 calc R . . C49 C 0.6941(3) 0.2365(5) 0.2573(6) 0.0390(19) Uani 1 1 d . . . H49A H 0.7017 0.2641 0.3116 0.047 Uiso 1 1 calc R . . H49B H 0.7242 0.2013 0.2800 0.047 Uiso 1 1 calc R . . C50 C 0.6928(4) 0.2877(5) 0.1858(7) 0.044(2) Uani 1 1 d . . . H50A H 0.6879 0.2594 0.1339 0.053 Uiso 1 1 calc R . . H50B H 0.7285 0.3129 0.2169 0.053 Uiso 1 1 calc R . . C51 C 0.6451(4) 0.3436(5) 0.1454(7) 0.046(2) Uani 1 1 d . . . H51A H 0.6516 0.3752 0.1960 0.056 Uiso 1 1 calc R . . H51B H 0.6440 0.3732 0.0977 0.056 Uiso 1 1 calc R . . C52 C 0.5896(4) 0.3041(6) 0.1011(6) 0.046(2) Uani 1 1 d . . . H52A H 0.5819 0.2764 0.0467 0.055 Uiso 1 1 calc R . . H52B H 0.5599 0.3395 0.0782 0.055 Uiso 1 1 calc R . . C53 C 0.5890(3) 0.2525(5) 0.1706(6) 0.042(2) Uani 1 1 d . . . H53 H 0.5948 0.2808 0.2239 0.050 Uiso 1 1 calc R . . C54 C 0.5094(4) 0.2160(6) 0.1638(6) 0.044(2) Uani 1 1 d . . . H54 H 0.5272 0.2417 0.2208 0.053 Uiso 1 1 calc R . . C60 C 0.1508(3) -0.2422(5) -0.5572(6) 0.075(4) Uani 1 1 d D . . Cl61 Cl 0.0951(2) -0.2706(4) -0.5483(5) 0.0695(17) Uiso 0.50 1 d PD . . Cl62 Cl 0.1383(3) -0.1509(3) -0.5970(4) 0.0688(15) Uiso 0.50 1 d PD . . Cl63 Cl 0.2144(2) -0.2545(3) -0.4532(4) 0.0581(13) Uiso 0.50 1 d PD . . Cl64 Cl 0.0907(3) -0.2382(6) -0.5635(7) 0.103(3) Uiso 0.50 1 d PD . . Cl65 Cl 0.1738(5) -0.1553(6) -0.5657(10) 0.169(5) Uiso 0.50 1 d PD . . Cl66 Cl 0.2055(4) -0.2772(7) -0.4416(8) 0.151(5) Uiso 0.50 1 d PD . . C70 C 0.1150(3) 0.1325(4) 0.4072(6) 0.077(4) Uani 1 1 d D . . Cl71 Cl 0.1809(2) 0.0997(4) 0.4494(4) 0.0664(15) Uiso 0.50 1 d PD . . Cl72 Cl 0.1181(3) 0.2098(4) 0.4742(5) 0.087(2) Uiso 0.50 1 d PD . . Cl73 Cl 0.0701(2) 0.0731(3) 0.4092(4) 0.0690(15) Uiso 0.50 1 d PD . . Cl74 Cl 0.1876(2) 0.1322(4) 0.4744(4) 0.0650(15) Uiso 0.50 1 d PD . . Cl75 Cl 0.0918(5) 0.1767(6) 0.4664(9) 0.152(4) Uiso 0.50 1 d PD . . Cl76 Cl 0.0915(4) 0.0383(4) 0.3939(7) 0.114(3) Uiso 0.50 1 d PD . . C80 C 0.7823(6) -0.0001(9) 0.0092(9) 0.086(5) Uani 1 1 d . . . Cl81 Cl 0.81081(12) 0.0860(2) 0.0220(2) 0.0752(9) Uani 1 1 d . . . Cl82 Cl 0.83638(17) -0.0616(3) 0.0864(4) 0.130(2) Uani 1 1 d . . . Cl83 Cl 0.74611(17) -0.0321(2) -0.1082(3) 0.0866(10) Uani 1 1 d . . . C90 C 0.9981(5) -0.0358(6) 0.1994(8) 0.085(8) Uiso 0.50 1 d PD . . Cl91 Cl 0.9686(3) 0.0501(3) 0.1654(5) 0.0634(19) Uiso 0.50 1 d PD . . Cl92 Cl 0.9834(4) -0.0804(5) 0.2717(6) 0.111(3) Uiso 0.50 1 d PD . . Cl93 Cl 1.0671(6) -0.0469(10) 0.2397(15) 0.137(7) Uiso 0.25 1 d PD . . Cl94 Cl 0.9763(6) -0.0848(6) 0.0975(7) 0.075(3) Uiso 0.25 1 d PD . . OW1 O 0.0000 -0.1505(7) -0.5000 0.007(2) Uiso 0.50 2 d SP . . OW2 O 0.4816(3) -0.0344(3) 0.1496(5) 0.0433(15) Uani 1 1 d . . . OW3 O 0.4755(4) -0.0863(6) -0.3267(8) 0.097(3) Uani 1 1 d . . . OW4 O 0.4918(4) 0.0522(5) -0.3322(11) 0.138(5) Uani 1 1 d . . . OW5 O 0.9067(2) 0.4668(3) 0.2227(3) 0.0262(11) Uani 1 1 d . . . OW6 O 0.9673(4) -0.1202(5) 0.1448(7) 0.030(2) Uiso 0.50 1 d P . . OW7 O 0.9662(5) -0.0592(6) 0.3458(8) 0.035(2) Uiso 0.50 1 d P . . OW8 O 0.9682(5) 0.0371(7) 0.1425(9) 0.025(3) Uiso 0.50 1 d P . . OW9 O 0.9815(3) 0.0049(4) 0.4706(5) 0.0154(17) Uiso 0.50 1 d P . . OW10 O 0.9833(5) -0.0358(7) 0.0217(8) 0.038(3) Uiso 0.50 1 d P . . OC1 O 0.0179(5) -0.1449(9) -0.5023(8) 0.033(3) Uiso 0.25 1 d P . . CO1 C 0.0179(5) -0.1449(9) -0.5023(8) 0.033(3) Uiso 0.25 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0227(6) 0.0569(9) 0.0276(6) 0.000 0.0160(5) 0.000 Zn2 0.0261(4) 0.0451(5) 0.0214(4) 0.0066(4) 0.0167(3) 0.0069(4) O1 0.031(3) 0.057(4) 0.030(3) -0.002(3) 0.021(2) -0.002(3) O2 0.029(3) 0.055(4) 0.027(3) 0.012(2) 0.022(2) 0.008(2) O3 0.043(3) 0.055(4) 0.030(3) -0.006(3) 0.028(3) 0.000(3) N1 0.024(3) 0.035(4) 0.038(4) 0.007(3) 0.022(3) 0.008(3) N2 0.027(3) 0.038(4) 0.024(3) 0.000(3) 0.017(2) 0.001(3) N3 0.029(3) 0.029(3) 0.025(3) 0.000(3) 0.015(3) -0.002(3) N4 0.028(3) 0.047(4) 0.022(3) -0.004(3) 0.014(3) -0.004(3) N5 0.036(4) 0.050(5) 0.043(4) -0.009(3) 0.024(3) -0.002(3) N6 0.020(3) 0.059(5) 0.033(4) -0.006(3) 0.016(3) -0.007(3) C1 0.025(4) 0.048(5) 0.025(4) 0.003(3) 0.017(3) 0.001(3) C2 0.040(5) 0.052(6) 0.026(4) -0.003(4) 0.020(4) -0.001(4) C3 0.053(5) 0.049(6) 0.052(5) -0.011(4) 0.043(5) -0.006(4) C4 0.051(5) 0.056(6) 0.048(5) -0.010(4) 0.038(5) -0.006(5) C5 0.091(9) 0.082(9) 0.124(11) -0.066(8) 0.095(9) -0.047(7) C6 0.067(8) 0.104(11) 0.092(10) -0.039(9) 0.036(8) 0.018(8) C7 0.093(8) 0.064(7) 0.101(9) -0.038(6) 0.088(8) -0.025(6) C8 0.115(10) 0.097(10) 0.081(8) -0.026(7) 0.085(9) -0.020(8) C9 0.042(5) 0.042(5) 0.054(5) 0.003(4) 0.038(4) 0.005(4) C10 0.030(4) 0.046(5) 0.026(4) 0.004(3) 0.016(3) 0.008(4) C11 0.031(4) 0.044(5) 0.029(4) 0.003(3) 0.022(3) 0.006(3) C12 0.023(4) 0.057(6) 0.027(4) 0.008(4) 0.016(3) 0.004(4) C13 0.035(4) 0.032(5) 0.038(4) 0.011(4) 0.013(4) 0.014(4) C14 0.041(5) 0.072(7) 0.029(4) 0.019(4) 0.017(4) 0.024(5) C15 0.021(4) 0.056(6) 0.024(4) 0.008(4) 0.006(3) 0.006(4) C16 0.026(4) 0.059(6) 0.022(3) 0.003(3) 0.016(3) 0.003(3) C17 0.018(3) 0.056(5) 0.021(3) 0.003(3) 0.012(3) 0.001(3) C18 0.022(3) 0.039(5) 0.030(3) 0.003(4) 0.018(3) 0.000(3) C19 0.021(3) 0.042(5) 0.018(3) 0.004(3) 0.011(3) -0.004(3) C20 0.019(3) 0.041(5) 0.023(3) -0.007(3) 0.013(3) -0.009(3) C21 0.037(4) 0.040(5) 0.012(3) 0.001(3) 0.018(3) -0.008(3) C22 0.039(4) 0.058(6) 0.023(4) 0.000(4) 0.020(3) -0.003(4) C23 0.063(6) 0.069(8) 0.062(6) 0.028(5) 0.042(5) -0.006(5) C24 0.055(6) 0.085(8) 0.029(4) -0.003(5) 0.027(4) -0.015(5) C25 0.034(5) 0.087(8) 0.046(5) 0.033(5) 0.031(4) 0.013(5) C26 0.025(4) 0.031(4) 0.027(4) 0.000(3) 0.015(3) -0.005(3) C27 0.019(3) 0.037(4) 0.020(3) 0.002(3) 0.011(3) 0.005(3) C28 0.020(3) 0.045(5) 0.017(3) 0.002(3) 0.010(3) -0.001(3) C29 0.025(3) 0.028(4) 0.023(3) -0.001(3) 0.017(3) -0.007(3) C30 0.028(4) 0.030(4) 0.021(3) 0.002(3) 0.012(3) 0.003(3) C31 0.038(5) 0.040(5) 0.051(5) -0.009(4) 0.027(4) 0.000(4) C32 0.049(6) 0.044(6) 0.087(8) -0.006(5) 0.043(6) 0.005(5) C33 0.046(5) 0.065(7) 0.038(5) 0.003(4) 0.026(4) 0.013(5) C34 0.016(4) 0.078(7) 0.033(4) 0.009(4) 0.011(3) 0.012(4) C35 0.024(4) 0.048(5) 0.022(3) 0.005(3) 0.014(3) 0.000(3) C36 0.030(4) 0.040(5) 0.033(4) -0.003(3) 0.021(4) 0.000(3) C37 0.031(4) 0.048(5) 0.033(4) -0.011(4) 0.020(4) -0.009(4) C38 0.064(6) 0.052(6) 0.033(5) -0.010(4) 0.028(5) -0.001(5) C39 0.051(6) 0.065(7) 0.034(5) -0.005(5) 0.026(4) -0.003(5) C40 0.089(8) 0.066(7) 0.032(5) -0.019(5) 0.038(5) -0.013(6) C41 0.094(9) 0.092(9) 0.045(6) -0.022(6) 0.041(6) 0.016(8) C42 0.139(12) 0.052(7) 0.034(5) 0.010(5) 0.035(7) 0.037(7) C43 0.185(17) 0.153(15) 0.087(10) -0.042(10) 0.113(12) -0.077(14) C44 0.039(5) 0.069(7) 0.034(4) -0.017(4) 0.022(4) -0.005(4) C45 0.034(4) 0.057(6) 0.049(5) -0.024(4) 0.031(4) -0.015(4) C46 0.040(4) 0.037(5) 0.031(4) -0.011(3) 0.025(4) -0.010(4) C47 0.042(5) 0.045(5) 0.037(4) -0.014(4) 0.028(4) -0.004(4) C48 0.024(4) 0.045(5) 0.035(4) -0.009(4) 0.021(3) -0.006(3) C49 0.031(4) 0.045(5) 0.047(5) -0.006(4) 0.026(4) -0.012(4) C50 0.042(5) 0.035(5) 0.064(6) 0.004(4) 0.036(5) -0.005(4) C51 0.050(5) 0.053(7) 0.048(5) 0.005(4) 0.035(4) 0.004(4) C52 0.032(4) 0.059(6) 0.034(4) 0.000(4) 0.011(4) 0.001(4) C53 0.030(4) 0.054(6) 0.039(5) -0.009(4) 0.019(4) -0.004(4) C54 0.035(4) 0.071(7) 0.026(4) -0.002(4) 0.017(4) 0.015(4) C60 0.066(7) 0.108(11) 0.054(6) -0.029(7) 0.036(6) -0.014(7) C70 0.044(6) 0.146(13) 0.042(5) 0.006(7) 0.025(5) -0.016(7) C80 0.083(9) 0.130(12) 0.085(9) 0.062(9) 0.071(8) 0.057(9) Cl81 0.0497(15) 0.129(3) 0.0550(15) 0.0114(17) 0.0346(13) 0.0022(16) Cl82 0.103(3) 0.183(5) 0.165(4) 0.121(4) 0.113(3) 0.091(3) Cl83 0.113(3) 0.075(2) 0.109(3) 0.004(2) 0.085(2) 0.006(2) OW2 0.051(4) 0.035(3) 0.058(4) 0.008(3) 0.039(3) 0.002(3) OW3 0.074(6) 0.130(8) 0.127(8) -0.055(7) 0.080(6) -0.033(6) OW4 0.060(6) 0.049(6) 0.228(14) 0.025(7) 0.039(7) 0.002(5) OW5 0.036(3) 0.009(2) 0.031(3) 0.004(2) 0.017(2) 0.013(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O1 1.919(6) . yes Zn1 O1 1.919(6) 2_655 no Zn1 N6 2.000(7) . yes Zn1 N6 2.000(7) 2_655 no Zn2 O3 1.921(6) 2_655 yes Zn2 O2 1.921(5) . yes Zn2 N4 2.014(7) 2_655 yes Zn2 N2 2.016(6) . yes O1 C1 1.310(8) . no O2 C28 1.312(8) . no O3 C46 1.282(9) . no O3 Zn2 1.921(6) 2_655 no N1 C11 1.266(10) . no N1 C12 1.474(10) . no N2 C18 1.306(9) . no N2 C17 1.463(9) . no N3 C29 1.241(9) . no N3 C30 1.488(9) . no N4 C36 1.246(9) . no N4 C35 1.493(11) . no N4 Zn2 2.014(7) 2_655 no N5 C47 1.335(12) . no N5 C48 1.437(11) . no N6 C54 1.279(10) . no N6 C53 1.469(10) . no C1 C10 1.420(11) . no C1 C2 1.425(12) . no C2 C3 1.406(11) . no C2 C54 1.448(13) . no C3 C4 1.393(12) . no C4 C9 1.399(13) . no C4 C5 1.505(12) . no C5 C8 1.412(18) . no C5 C7 1.507(15) . no C5 C6 1.61(2) . no C9 C10 1.367(10) . no C10 C11 1.489(11) . no C12 C13 1.533(11) . no C12 C17 1.545(12) . no C13 C14 1.510(13) . no C14 C15 1.538(14) . no C15 C16 1.545(11) . no C16 C17 1.511(10) . no C18 C19 1.442(10) . no C19 C20 1.391(9) . no C19 C28 1.418(10) . no C20 C21 1.419(11) . no C21 C26 1.419(10) . no C21 C22 1.512(9) . no C22 C24 1.511(12) . no C22 C23 1.511(15) . no C22 C25 1.536(11) . no C26 C27 1.415(10) . no C27 C28 1.407(10) . no C27 C29 1.481(9) . no C30 C31 1.505(12) . no C30 C35 1.541(10) . no C31 C32 1.532(12) . no C32 C33 1.504(14) . no C33 C34 1.522(15) . no C34 C35 1.514(11) . no C36 C37 1.489(12) . no C37 C38 1.416(11) . no C37 C46 1.427(12) . no C38 C39 1.365(14) . no C39 C44 1.371(15) . no C39 C40 1.550(12) . no C40 C41 1.454(16) . no C40 C42 1.465(18) . no C40 C43 1.591(18) . no C44 C45 1.364(12) . no C45 C46 1.424(12) . no C45 C47 1.467(13) . no C48 C53 1.548(12) . no C48 C49 1.565(10) . no C49 C50 1.531(12) . no C50 C51 1.536(13) . no C51 C52 1.517(13) . no C52 C53 1.535(13) . no C60 Cl64 1.690(8) . no C60 Cl63 1.691(8) . no C60 Cl62 1.773(8) . no C60 Cl65 1.774(9) . no C60 Cl61 1.792(8) . no C60 Cl66 1.803(9) . no Cl61 Cl64 0.633(10) . no Cl62 Cl65 0.850(12) . no Cl62 Cl64 2.401(10) . no Cl63 Cl66 0.583(13) . no Cl63 Cl65 2.417(12) . no C70 Cl75 1.716(8) . no C70 Cl73 1.720(7) . no C70 Cl71 1.724(7) . no C70 Cl74 1.729(7) . no C70 Cl72 1.801(8) . no C70 Cl76 1.830(8) . no Cl71 Cl74 0.695(7) . no Cl71 Cl76 2.471(10) . no Cl72 Cl75 0.927(12) . no Cl72 Cl74 2.475(9) . no Cl73 Cl76 1.028(9) . no Cl73 Cl75 2.072(12) . no C80 Cl81 1.746(17) . no C80 Cl83 1.755(16) . no C80 Cl82 1.764(12) . no C90 OW8 1.593(17) . no C90 Cl93 1.718(9) . no C90 Cl94 1.732(10) . no C90 Cl91 1.733(9) . no C90 Cl92 1.737(9) . no C90 OW6 1.771(15) . no Cl92 OW7 1.661(13) . no Cl92 OW6 2.082(13) . no Cl93 Cl94 2.45(2) . no Cl94 OW6 1.184(14) . no Cl94 OW10 1.690(15) . no OW1 CO1 0.555(14) 2_554 no OW1 OC1 0.555(14) 2_554 no OW1 OC1 0.555(14) . no OW9 OW9 0.962(15) 2_756 no OW10 OW10 1.53(2) 2_755 no OC1 CO1 1.09(3) 2_554 no OC1 OC1 1.09(3) 2_554 no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn1 O1 121.1(4) . 2_655 no O1 Zn1 N6 96.6(2) . . no O1 Zn1 N6 111.5(2) 2_655 . no O1 Zn1 N6 111.5(2) . 2_655 no O1 Zn1 N6 96.6(2) 2_655 2_655 no N6 Zn1 N6 121.4(5) . 2_655 no O3 Zn2 O2 127.1(2) 2_655 . no O3 Zn2 N4 95.1(3) 2_655 2_655 no O2 Zn2 N4 108.1(3) . 2_655 no O3 Zn2 N2 110.3(2) 2_655 . no O2 Zn2 N2 96.3(2) . . no N4 Zn2 N2 122.6(3) 2_655 . no C1 O1 Zn1 123.3(5) . . no C28 O2 Zn2 125.5(5) . . no C46 O3 Zn2 126.3(6) . 2_655 no C11 N1 C12 112.9(6) . . no C18 N2 C17 118.2(6) . . no C18 N2 Zn2 119.7(5) . . no C17 N2 Zn2 122.1(4) . . no C29 N3 C30 114.2(6) . . no C36 N4 C35 113.6(7) . . no C36 N4 Zn2 124.6(6) . 2_655 no C35 N4 Zn2 121.8(5) . 2_655 no C47 N5 C48 112.0(7) . . no C54 N6 C53 117.6(7) . . no C54 N6 Zn1 119.2(6) . . no C53 N6 Zn1 123.2(5) . . no O1 C1 C10 119.2(7) . . no O1 C1 C2 123.7(7) . . no C10 C1 C2 117.1(7) . . no C3 C2 C1 119.1(8) . . no C3 C2 C54 116.5(8) . . no C1 C2 C54 124.5(7) . . no C4 C3 C2 123.0(8) . . no C3 C4 C9 116.8(7) . . no C3 C4 C5 122.1(8) . . no C9 C4 C5 120.7(8) . . no C8 C5 C4 114.0(11) . . no C8 C5 C7 114.2(11) . . no C4 C5 C7 114.0(8) . . no C8 C5 C6 100.9(11) . . no C4 C5 C6 109.3(11) . . no C7 C5 C6 102.9(11) . . no C10 C9 C4 122.0(8) . . no C9 C10 C1 121.8(8) . . no C9 C10 C11 121.8(7) . . no C1 C10 C11 116.1(6) . . no N1 C11 C10 125.4(7) . . no N1 C12 C13 108.4(7) . . no N1 C12 C17 112.0(6) . . no C13 C12 C17 109.0(6) . . no C14 C13 C12 110.9(7) . . no C13 C14 C15 111.2(7) . . no C14 C15 C16 109.8(7) . . no C17 C16 C15 111.2(7) . . no N2 C17 C16 109.3(6) . . no N2 C17 C12 110.4(6) . . no C16 C17 C12 110.0(6) . . no N2 C18 C19 128.4(6) . . no C20 C19 C28 120.4(7) . . no C20 C19 C18 115.0(6) . . no C28 C19 C18 124.5(6) . . no C19 C20 C21 123.4(7) . . no C26 C21 C20 115.7(6) . . no C26 C21 C22 121.0(7) . . no C20 C21 C22 123.4(7) . . no C24 C22 C21 109.3(7) . . no C24 C22 C23 110.0(8) . . no C21 C22 C23 110.6(7) . . no C24 C22 C25 110.7(8) . . no C21 C22 C25 111.4(7) . . no C23 C22 C25 104.9(8) . . no C27 C26 C21 121.4(7) . . no C28 C27 C26 121.6(6) . . no C28 C27 C29 117.7(6) . . no C26 C27 C29 120.7(6) . . no O2 C28 C27 118.0(6) . . no O2 C28 C19 124.5(6) . . no C27 C28 C19 117.5(6) . . no N3 C29 C27 127.7(6) . . no N3 C30 C31 110.6(6) . . no N3 C30 C35 112.3(6) . . no C31 C30 C35 110.1(6) . . no C30 C31 C32 111.0(8) . . no C33 C32 C31 111.2(9) . . no C32 C33 C34 109.8(8) . . no C35 C34 C33 111.7(8) . . no N4 C35 C34 111.8(7) . . no N4 C35 C30 109.1(6) . . no C34 C35 C30 110.3(6) . . no N4 C36 C37 122.6(8) . . no C38 C37 C46 118.2(8) . . no C38 C37 C36 114.3(8) . . no C46 C37 C36 127.5(7) . . no C39 C38 C37 123.8(9) . . no C38 C39 C44 116.3(8) . . no C38 C39 C40 119.7(10) . . no C44 C39 C40 123.8(9) . . no C41 C40 C42 106.8(10) . . no C41 C40 C39 112.8(10) . . no C42 C40 C39 112.9(9) . . no C41 C40 C43 108.2(12) . . no C42 C40 C43 106.3(12) . . no C39 C40 C43 109.4(9) . . no C45 C44 C39 124.2(9) . . no C44 C45 C46 120.1(9) . . no C44 C45 C47 126.1(9) . . no C46 C45 C47 113.7(7) . . no O3 C46 C45 120.1(8) . . no O3 C46 C37 122.7(7) . . no C45 C46 C37 117.1(7) . . no N5 C47 C45 124.7(7) . . no N5 C48 C53 112.3(6) . . no N5 C48 C49 107.4(6) . . no C53 C48 C49 109.0(7) . . no C50 C49 C48 110.6(7) . . no C49 C50 C51 112.0(7) . . no C52 C51 C50 109.2(8) . . no C51 C52 C53 113.2(7) . . no N6 C53 C52 110.8(7) . . no N6 C53 C48 109.1(7) . . no C52 C53 C48 110.2(7) . . no N6 C54 C2 128.4(8) . . no Cl64 C60 Cl63 122.4(6) . . no Cl64 C60 Cl62 87.8(5) . . no Cl63 C60 Cl62 113.0(5) . . no Cl64 C60 Cl65 112.5(6) . . no Cl63 C60 Cl65 88.4(6) . . no Cl62 C60 Cl65 27.7(4) . . no Cl64 C60 Cl61 20.7(4) . . no Cl63 C60 Cl61 111.4(5) . . no Cl62 C60 Cl61 108.4(5) . . no Cl65 C60 Cl61 132.4(7) . . no Cl64 C60 Cl66 108.1(6) . . no Cl63 C60 Cl66 18.8(4) . . no Cl62 C60 Cl66 128.2(7) . . no Cl65 C60 Cl66 106.1(6) . . no Cl61 C60 Cl66 94.1(5) . . no Cl64 Cl61 C60 70.6(8) . . no Cl65 Cl62 C60 76.2(7) . . no Cl65 Cl62 Cl64 116.3(7) . . no C60 Cl62 Cl64 44.7(3) . . no Cl66 Cl63 C60 91.6(10) . . no Cl66 Cl63 Cl65 135.0(11) . . no C60 Cl63 Cl65 47.2(3) . . no Cl61 Cl64 C60 88.7(9) . . no Cl61 Cl64 Cl62 136.2(9) . . no C60 Cl64 Cl62 47.5(3) . . no Cl62 Cl65 C60 76.1(7) . . no Cl62 Cl65 Cl63 115.7(7) . . no C60 Cl65 Cl63 44.4(3) . . no Cl63 Cl66 C60 69.6(9) . . no Cl75 C70 Cl73 74.2(5) . . no Cl75 C70 Cl71 129.8(6) . . no Cl73 C70 Cl71 116.3(5) . . no Cl75 C70 Cl74 110.6(6) . . no Cl73 C70 Cl74 129.4(6) . . no Cl71 C70 Cl74 23.2(3) . . no Cl75 C70 Cl72 30.5(4) . . no Cl73 C70 Cl72 104.5(4) . . no Cl71 C70 Cl72 112.0(5) . . no Cl74 C70 Cl72 89.0(4) . . no Cl75 C70 Cl76 106.1(5) . . no Cl73 C70 Cl76 33.5(3) . . no Cl71 C70 Cl76 88.0(5) . . no Cl74 C70 Cl76 107.8(5) . . no Cl72 C70 Cl76 135.1(6) . . no Cl74 Cl71 C70 78.8(6) . . no Cl74 Cl71 Cl76 119.2(7) . . no C70 Cl71 Cl76 47.8(3) . . no Cl75 Cl72 C70 69.7(6) . . no Cl75 Cl72 Cl74 103.1(7) . . no C70 Cl72 Cl74 44.3(3) . . no Cl76 Cl73 C70 79.2(5) . . no Cl76 Cl73 Cl75 129.1(6) . . no C70 Cl73 Cl75 52.8(3) . . no Cl71 Cl74 C70 78.0(6) . . no Cl71 Cl74 Cl72 124.0(7) . . no C70 Cl74 Cl72 46.7(3) . . no Cl72 Cl75 C70 79.9(6) . . no Cl72 Cl75 Cl73 132.5(7) . . no C70 Cl75 Cl73 53.0(3) . . no Cl73 Cl76 C70 67.4(5) . . no Cl73 Cl76 Cl71 106.0(5) . . no C70 Cl76 Cl71 44.2(3) . . no Cl81 C80 Cl83 112.1(6) . . no Cl81 C80 Cl82 109.5(8) . . no Cl83 C80 Cl82 109.4(8) . . no OW8 C90 Cl93 116.6(9) . . no OW8 C90 Cl94 93.8(8) . . no Cl93 C90 Cl94 90.5(11) . . no OW8 C90 Cl91 14.9(5) . . no Cl93 C90 Cl91 118.8(8) . . no Cl94 C90 Cl91 108.3(6) . . no OW8 C90 Cl92 124.4(8) . . no Cl93 C90 Cl92 111.6(7) . . no Cl94 C90 Cl92 112.2(7) . . no Cl91 C90 Cl92 113.2(6) . . no OW8 C90 OW6 119.0(9) . . no Cl93 C90 OW6 103.1(10) . . no Cl94 C90 OW6 39.5(5) . . no Cl91 C90 OW6 128.5(8) . . no Cl92 C90 OW6 72.8(6) . . no OW7 Cl92 C90 138.2(7) . . no OW7 Cl92 OW6 154.2(7) . . no C90 Cl92 OW6 54.3(5) . . no C90 Cl93 Cl94 45.0(6) . . no OW6 Cl94 OW10 174.9(12) . . no OW6 Cl94 C90 72.0(7) . . no OW10 Cl94 C90 111.3(8) . . no OW6 Cl94 Cl93 90.6(8) . . no OW10 Cl94 Cl93 94.4(7) . . no C90 Cl94 Cl93 44.5(6) . . no CO1 OW1 OC1 0(4) 2_554 2_554 no CO1 OW1 OC1 159(5) 2_554 . no OC1 OW1 OC1 159(5) 2_554 . no Cl94 OW6 C90 68.5(7) . . no Cl94 OW6 Cl92 121.3(8) . . no C90 OW6 Cl92 52.9(4) . . no OW10 OW10 Cl94 140.2(8) 2_755 . no OW1 OC1 CO1 11(3) . 2_554 no OW1 OC1 OC1 11(3) . 2_554 no CO1 OC1 OC1 0.0(12) 2_554 2_554 no _diffrn_measured_fraction_theta_max 0.938 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.732 _refine_diff_density_min -1.160 _refine_diff_density_rms 0.170