# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1993 data_global #====================================================================== #1. SUBMISSION DETAILS _publ_contact_author_name 'John M. Plater' _publ_contact_author_address ; Department of Chemistry University of Aberdeen Meston Walk Aberdeen AB24 3UE United Kingdom ; _publ_contact_author_phone ? _publ_contact_author_fax ? _publ_contact_author_email ? _publ_requested_journal 'J. Chem Soc., Dalton Trans.' _publ_requested_category ? _publ_requested_coeditor_name ? _publ_contact_letter ; Please consider this CIF submission for a structure to be published in J. Chem Soc., Dalton Trans. ; #====================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Synthesis an characterisations of infinite di- and tri-nuclear zinc co-ordination networks with flexible dipyridyl ligands ; loop_ _publ_author_name _publ_author_address ' Plater, M. John' ; Department of Chemistry University of Aberdeen Meston Walk Aberdeen AB24 3UE United Kingdom ; ' Foreman, Mark R. St. J.' ; Department of Chemistry University of Aberdeen Meston Walk Aberdeen AB24 3UE United Kingdom ; 'Gelbrich, Thomas' ; University of Southampton Department of Chemistry Highfield Southampton SO17 1BJ United Kingdom ; ' Hursthouse, Michael B.' ; University of Southampton Department of Chemistry Highfield Southampton SO17 1BJ United Kingdom ; data_s92 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H57 Cl3 N6 O15 Zn2' _chemical_formula_weight 1147.05 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.5216(6) _cell_length_b 16.7671(9) _cell_length_c 28.7044(16) _cell_angle_alpha 90.00 _cell_angle_beta 89.9880(10) _cell_angle_gamma 90.00 _cell_volume 5063.9(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.505 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2376 _exptl_absorpt_coefficient_mu 1.177 _exptl_absorpt_correction_type 'Empirical, SORTAV (R. H. Blessing, 1995, 1997)' _exptl_absorpt_correction_T_min 0.8432 _exptl_absorpt_correction_T_max 0.9117 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enraf Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf Nonius KappaCCD area detector' _diffrn_measurement_method '\p and \q scans to fill Ewald sphere' _diffrn_detector_area_resol_mean '9.091 pixels/mm' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20263 _diffrn_reflns_av_R_equivalents 0.0618 _diffrn_reflns_av_sigmaI/netI 0.0919 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 25.25 _reflns_number_total 8742 _reflns_number_gt 6701 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DENZO (Otwinowski and Minor, 1997) COLLECT (Hooft, 1998) ' _computing_cell_refinement 'DENZO and COLLECT' _computing_data_reduction 'DENZO and COLLECT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'PLATON (Spek, 1990)' _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^)+(0.0451P)^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 SHELXL _refine_ls_extinction_coef 0.00033(16) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 8742 _refine_ls_number_parameters 695 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0730 _refine_ls_R_factor_gt 0.0479 _refine_ls_wR_factor_ref 0.1085 _refine_ls_wR_factor_gt 0.0999 _refine_ls_goodness_of_fit_ref 0.975 _refine_ls_restrained_S_all 0.981 _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 0.08748(5) 0.72035(3) 0.18407(2) 0.02451(15) Uani 1 1 d . . . Zn2 Zn 0.08109(6) 0.76992(3) 0.06501(2) 0.02678(16) Uani 1 1 d . . . O13 O 0.1320(3) 0.77699(18) 0.12874(12) 0.0263(7) Uani 1 1 d D . . H1O H 0.194(3) 0.808(2) 0.1385(18) 0.042(17) Uiso 1 1 d D . . N11 N -0.0411(4) 0.6305(2) 0.17901(14) 0.0234(9) Uani 1 1 d . . . C101 C -0.1619(4) 0.6464(3) 0.16654(17) 0.0269(12) Uani 1 1 d . . . H101 H -0.1822 0.6993 0.1573 0.016(12) Uiso 1 1 calc R . . C102 C -0.2573(4) 0.5906(3) 0.16632(17) 0.0298(12) Uani 1 1 d . . . H102 H -0.3409 0.6050 0.1570 0.008(11) Uiso 1 1 calc R . . C103 C -0.2300(4) 0.5117(3) 0.18018(18) 0.0284(12) Uani 1 1 d . . . C104 C -0.1064(5) 0.4959(3) 0.19268(18) 0.0312(12) Uani 1 1 d . . . H104 H -0.0834 0.4435 0.2021 0.022(12) Uiso 1 1 calc R . . C105 C -0.0150(5) 0.5552(3) 0.19177(18) 0.0297(12) Uani 1 1 d . . . H105 H 0.0695 0.5422 0.2005 0.034(14) Uiso 1 1 calc R . . C106 C -0.3340(4) 0.4509(3) 0.1830(2) 0.0338(13) Uani 1 1 d . . . H10A H -0.2991 0.4009 0.1961 0.050(17) Uiso 1 1 calc R . . H10B H -0.3649 0.4392 0.1511 0.025(13) Uiso 1 1 calc R . . C107 C -0.4445(5) 0.4778(3) 0.21249(19) 0.0319(13) Uani 1 1 d . . . H10C H -0.4785 0.5280 0.1992 0.044(16) Uiso 1 1 calc R . . H10D H -0.4127 0.4899 0.2442 0.035(14) Uiso 1 1 calc R . . C108 C -0.4464(4) 0.9177(3) 0.28343(19) 0.0300(12) Uani 1 1 d . . . H10E H -0.4244 0.8973 0.3148 0.018(11) Uiso 1 1 calc R . . H10F H -0.4739 0.8720 0.2641 0.026(13) Uiso 1 1 calc R . . C109 C -0.3318(5) 0.9556(3) 0.2619(2) 0.0350(13) Uani 1 1 d . . . H10G H -0.3592 0.9831 0.2331 0.07(2) Uiso 1 1 calc R . . H10H H -0.3004 0.9971 0.2836 0.045(17) Uiso 1 1 calc R . . C110 C -0.2226(5) 0.9024(3) 0.24986(17) 0.0268(12) Uani 1 1 d . . . C111 C -0.2161(5) 0.8225(3) 0.26427(17) 0.0278(12) Uani 1 1 d . . . H111 H -0.2789 0.8017 0.2847 0.039(15) Uiso 1 1 calc R . . C112 C -0.1191(5) 0.7744(3) 0.24884(17) 0.0318(13) Uani 1 1 d . . . H112 H -0.1174 0.7203 0.2586 0.018(12) Uiso 1 1 calc R . . C113 C -0.0280(5) 0.8788(3) 0.20847(18) 0.0280(12) Uani 1 1 d . . . H113 H 0.0382 0.8992 0.1894 0.045(16) Uiso 1 1 calc R . . C114 C -0.1221(5) 0.9291(3) 0.22306(17) 0.0284(12) Uani 1 1 d . . . H114 H -0.1184 0.9838 0.2146 0.034 Uiso 1 1 calc R . . N12 N -0.0266(4) 0.8007(2) 0.22052(14) 0.0274(10) Uani 1 1 d . . . N21 N 0.2262(4) 0.6943(2) 0.23023(14) 0.0264(10) Uani 1 1 d . . . C201 C 0.1968(5) 0.6664(3) 0.27311(17) 0.0296(12) Uani 1 1 d . . . H201 H 0.1097 0.6629 0.2816 0.017(11) Uiso 1 1 calc R . . C202 C 0.2865(5) 0.6428(3) 0.30494(18) 0.0300(13) Uani 1 1 d . . . H202 H 0.2607 0.6229 0.3344 0.020(12) Uiso 1 1 calc R . . C203 C 0.4154(5) 0.6479(2) 0.29421(17) 0.0257(11) Uani 1 1 d . . . C204 C 0.4459(4) 0.6794(3) 0.25078(17) 0.0251(11) Uani 1 1 d . . . H204 H 0.5324 0.6863 0.2422 0.020(12) Uiso 1 1 calc R . . C205 C 0.3504(5) 0.7004(3) 0.22013(18) 0.0283(12) Uani 1 1 d . . . H205 H 0.3739 0.7203 0.1904 0.022(13) Uiso 1 1 calc R . . C206 C 0.5161(5) 0.6187(3) 0.32736(18) 0.0317(13) Uani 1 1 d . . . H20A H 0.6004 0.6308 0.3138 0.020(11) Uiso 1 1 calc R . . H20B H 0.5089 0.5600 0.3298 0.027(13) Uiso 1 1 calc R . . C207 C 0.5107(5) 0.6541(3) 0.37684(18) 0.0287(12) Uani 1 1 d . . . H20C H 0.4290 0.6394 0.3916 0.018(11) Uiso 1 1 calc R . . H20D H 0.5802 0.6312 0.3958 0.022(12) Uiso 1 1 calc R . . C208 C 0.5234(5) 0.7553(3) -0.1239(2) 0.0327(12) Uani 1 1 d . . . H20E H 0.5988 0.7407 -0.1427 0.039(14) Uiso 1 1 calc R . . H20F H 0.4476 0.7322 -0.1393 0.023(13) Uiso 1 1 calc R . . C209 C 0.5368(5) 0.7187(3) -0.07512(19) 0.0375(14) Uani 1 1 d . . . H20G H 0.5493 0.6605 -0.0785 0.019(12) Uiso 1 1 calc R . . H20H H 0.6143 0.7407 -0.0604 0.034(14) Uiso 1 1 calc R . . C210 C 0.4266(5) 0.7326(3) -0.04300(17) 0.0305(12) Uani 1 1 d . . . C211 C 0.3007(5) 0.7174(3) -0.0556(2) 0.0357(14) Uani 1 1 d . . . H211 H 0.2825 0.6994 -0.0862 0.039(15) Uiso 1 1 calc R . . C212 C 0.2037(5) 0.7280(3) -0.02486(19) 0.0326(13) Uani 1 1 d . . . H212 H 0.1192 0.7178 -0.0348 0.053(18) Uiso 1 1 calc R . . C213 C 0.3454(5) 0.7681(3) 0.03248(18) 0.0266(12) Uani 1 1 d . . . H213 H 0.3617 0.7854 0.0634 0.018(12) Uiso 1 1 calc R . . C214 C 0.4462(5) 0.7597(3) 0.00223(18) 0.0279(12) Uani 1 1 d . . . H214 H 0.5297 0.7724 0.0124 0.025(14) Uiso 1 1 calc R . . N22 N 0.2239(4) 0.7527(2) 0.01975(15) 0.0275(10) Uani 1 1 d . . . N31 N -0.0541(3) 0.6853(2) 0.05584(13) 0.0246(9) Uani 1 1 d . . . C302 C -0.2747(5) 0.6498(3) 0.05241(17) 0.0273(12) Uani 1 1 d . . . H302 H -0.3608 0.6666 0.0539 0.019(12) Uiso 1 1 calc R . . C301 C -0.1791(5) 0.7047(3) 0.05682(18) 0.0291(12) Uani 1 1 d . . . H301 H -0.2015 0.7592 0.0608 0.021(12) Uiso 1 1 calc R . . C303 C -0.2466(4) 0.5699(3) 0.04578(17) 0.0267(12) Uani 1 1 d . . . C304 C -0.1196(5) 0.5503(3) 0.04537(18) 0.0318(13) Uani 1 1 d . . . H304 H -0.0954 0.4961 0.0412 0.025(12) Uiso 1 1 calc R . . C305 C -0.0264(5) 0.6077(3) 0.05083(19) 0.0349(14) Uani 1 1 d . . . H305 H 0.0601 0.5917 0.0510 0.034(14) Uiso 1 1 calc R . . C306 C -0.3502(4) 0.5086(3) 0.03982(18) 0.0275(12) Uani 1 1 d . . . H30A H -0.3922 0.4998 0.0703 0.033(14) Uiso 1 1 calc R . . H30B H -0.3113 0.4574 0.0301 0.041(15) Uiso 1 1 calc R . . C307 C -0.4508(4) 0.5325(3) 0.00401(17) 0.0259(12) Uani 1 1 d . . . H30C H -0.4943 0.5815 0.0148 0.016(12) Uiso 1 1 calc R . . H30D H -0.4084 0.5450 -0.0259 0.032(13) Uiso 1 1 calc R . . C308 C -0.4399(5) 0.9767(3) 0.0062(2) 0.0408(14) Uani 1 1 d . . . H30E H -0.4480 0.9563 0.0384 0.042(15) Uiso 1 1 calc R . . H30F H -0.4330 0.9301 -0.0149 0.029(13) Uiso 1 1 calc R . . C309 C -0.3192(5) 1.0255(4) 0.0025(2) 0.0432(15) Uani 1 1 d . . . H30G H -0.3090 1.0449 -0.0298 0.043(16) Uiso 1 1 calc R . . H30H H -0.3254 1.0725 0.0233 0.026(14) Uiso 1 1 calc R . . C310 C -0.2041(5) 0.9764(3) 0.0160(2) 0.0351(14) Uani 1 1 d . . . C311 C -0.1547(5) 0.9770(3) 0.0602(2) 0.0407(14) Uani 1 1 d . . . H311 H -0.1843 1.0149 0.0823 0.09(2) Uiso 1 1 calc R . . C312 C -0.0623(5) 0.9230(3) 0.07263(19) 0.0358(13) Uani 1 1 d . . . H312 H -0.0311 0.9239 0.1037 0.039(15) Uiso 1 1 calc R . . C314 C -0.1516(6) 0.9240(4) -0.0155(2) 0.0487(16) Uani 1 1 d . . . H314 H -0.1801 0.9236 -0.0469 0.051(18) Uiso 1 1 calc R . . C313 C -0.0571(6) 0.8719(4) -0.0013(2) 0.0459(16) Uani 1 1 d . . . H313 H -0.0211 0.8368 -0.0237 0.10(3) Uiso 1 1 calc R . . N32 N -0.0140(4) 0.8689(3) 0.04278(14) 0.0300(10) Uani 1 1 d . . . Cl1 Cl 0.11137(14) 0.09648(8) 0.15463(5) 0.0423(4) Uani 1 1 d . . . O1 O 0.1148(6) 0.0839(3) 0.20383(14) 0.0746(15) Uani 1 1 d . . . O2 O 0.1655(4) 0.1716(3) 0.14481(17) 0.0705(14) Uani 1 1 d . . . O3 O 0.1848(4) 0.0367(3) 0.13157(15) 0.0654(13) Uani 1 1 d . . . O4 O -0.0149(4) 0.0940(4) 0.1384(2) 0.096(2) Uani 1 1 d . . . Cl2 Cl 0.37697(13) 0.35308(9) 0.36466(5) 0.0444(4) Uani 1 1 d . . . O5 O 0.2466(3) 0.3325(2) 0.35935(14) 0.0472(11) Uani 1 1 d . . . O6 O 0.4209(4) 0.3282(2) 0.40939(14) 0.0614(12) Uani 1 1 d . . . O7 O 0.4493(5) 0.3199(4) 0.32812(19) 0.123(2) Uani 1 1 d . . . O8 O 0.3849(6) 0.4390(3) 0.36114(18) 0.0957(19) Uani 1 1 d . . . Cl3 Cl -0.67122(12) 0.57526(8) 0.10810(5) 0.0351(3) Uani 1 1 d . . . O9 O -0.7212(3) 0.5832(2) 0.06137(14) 0.0449(10) Uani 1 1 d . . . O10 O -0.7696(4) 0.5925(2) 0.14159(14) 0.0500(11) Uani 1 1 d . . . O11 O -0.6252(4) 0.4961(2) 0.11466(14) 0.0582(12) Uani 1 1 d . . . O12 O -0.5677(3) 0.6299(2) 0.11419(15) 0.0573(12) Uani 1 1 d . . . O14 O 0.2909(5) 0.8913(3) 0.1637(2) 0.0845(18) Uani 1 1 d G . . H2O H 0.2855 0.9040 0.1348 0.101 Uiso 1 1 d G . . H3O H 0.3655 0.8753 0.1680 0.101 Uiso 1 1 d G . . C1 C -0.1343(7) 0.6427(5) -0.0771(3) 0.097(3) Uani 1 1 d D A 1 H1A H -0.2267 0.6371 -0.0828 0.146 Uiso 1 1 calc R A 1 H1B H -0.1096 0.6080 -0.0507 0.146 Uiso 1 1 calc R A 1 C2 C -0.061(2) 0.6244(7) -0.1189(7) 0.110(7) Uani 0.83(5) 1 d PD A 1 H2A H -0.0762 0.5690 -0.1281 0.165 Uiso 1 1 calc R A 1 H2B H 0.0301 0.6317 -0.1123 0.165 Uiso 1 1 calc R A 1 H2C H -0.0862 0.6602 -0.1442 0.165 Uiso 1 1 calc R A 1 O15 O -0.0998(9) 0.7256(4) -0.0683(3) 0.094(2) Uani 0.598(7) 1 d PD A 1 H4O H -0.0390 0.7386 -0.0857 0.141 Uiso 0.598(7) 1 calc PR A 1 C2' C -0.019(3) 0.6156(6) -0.1040(15) 0.110(7) Uani 0.17(5) 1 d PD A 2 O15' O 0.0273(10) 0.6927(7) -0.1213(5) 0.094(2) Uani 0.402(7) 1 d PD A 2 H4O' H 0.0153 0.7279 -0.1009 0.100 Uiso 0.402(7) 1 calc PRD A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0241(3) 0.0282(3) 0.0213(3) 0.0009(2) 0.0014(3) -0.0012(2) Zn2 0.0270(3) 0.0312(3) 0.0222(3) 0.0012(3) 0.0007(3) -0.0047(3) O13 0.0281(17) 0.0281(19) 0.0227(18) -0.0002(15) -0.0025(16) -0.0102(15) N11 0.025(2) 0.022(2) 0.023(2) 0.0036(18) 0.0061(18) -0.0008(17) C101 0.026(3) 0.028(3) 0.026(3) 0.006(2) 0.002(2) 0.004(2) C102 0.020(3) 0.038(3) 0.030(3) 0.003(2) 0.002(2) 0.000(2) C103 0.028(3) 0.030(3) 0.027(3) -0.004(2) 0.009(2) -0.004(2) C104 0.035(3) 0.023(3) 0.036(3) 0.003(2) 0.010(3) -0.001(2) C105 0.022(3) 0.036(3) 0.031(3) 0.003(2) -0.003(2) 0.003(2) C106 0.028(3) 0.034(3) 0.039(3) 0.001(3) 0.007(3) -0.003(2) C107 0.031(3) 0.028(3) 0.036(3) -0.004(2) 0.006(3) -0.003(2) C108 0.030(3) 0.027(3) 0.032(3) -0.001(2) 0.005(2) 0.008(2) C109 0.034(3) 0.025(3) 0.046(4) -0.004(3) 0.004(3) 0.001(2) C110 0.027(3) 0.033(3) 0.020(3) -0.005(2) 0.001(2) 0.008(2) C111 0.029(3) 0.030(3) 0.024(3) 0.000(2) 0.007(2) 0.007(2) C112 0.039(3) 0.036(3) 0.020(3) 0.005(2) 0.000(2) 0.003(3) C113 0.023(3) 0.030(3) 0.031(3) -0.002(2) -0.001(2) -0.006(2) C114 0.033(3) 0.023(3) 0.030(3) -0.005(2) 0.000(2) -0.005(2) N12 0.029(2) 0.039(3) 0.014(2) -0.0027(19) 0.0006(19) 0.002(2) N21 0.028(2) 0.028(2) 0.023(2) 0.0005(19) 0.0058(19) -0.0008(19) C201 0.023(3) 0.040(3) 0.026(3) -0.002(2) -0.003(2) 0.003(2) C202 0.035(3) 0.031(3) 0.024(3) 0.004(2) 0.009(2) 0.003(2) C203 0.027(3) 0.018(2) 0.032(3) -0.006(2) -0.004(2) 0.001(2) C204 0.021(3) 0.025(3) 0.029(3) 0.000(2) 0.003(2) 0.001(2) C205 0.030(3) 0.028(3) 0.027(3) 0.002(2) 0.003(2) 0.002(2) C206 0.031(3) 0.030(3) 0.035(3) -0.001(2) -0.004(2) 0.001(2) C207 0.030(3) 0.033(3) 0.023(3) -0.003(2) -0.008(2) -0.002(2) C208 0.034(3) 0.038(3) 0.026(3) 0.005(2) 0.000(3) 0.009(3) C209 0.039(3) 0.047(4) 0.027(3) 0.005(3) 0.008(3) 0.016(3) C210 0.035(3) 0.029(3) 0.027(3) 0.007(2) 0.004(3) 0.008(2) C211 0.047(3) 0.035(3) 0.026(3) 0.000(2) 0.001(3) 0.003(3) C212 0.034(3) 0.033(3) 0.031(3) 0.003(2) -0.007(3) -0.008(2) C213 0.031(3) 0.030(3) 0.019(3) 0.002(2) -0.007(2) 0.004(2) C214 0.029(3) 0.024(3) 0.031(3) 0.005(2) -0.004(2) 0.000(2) N22 0.030(2) 0.027(2) 0.026(2) 0.0005(19) 0.001(2) 0.0007(19) N31 0.026(2) 0.027(2) 0.021(2) -0.0027(18) 0.0001(18) -0.0040(18) C302 0.023(3) 0.028(3) 0.031(3) 0.000(2) 0.001(2) -0.002(2) C301 0.035(3) 0.023(3) 0.029(3) 0.003(2) 0.004(2) 0.002(2) C303 0.029(3) 0.025(3) 0.026(3) -0.001(2) -0.002(2) -0.004(2) C304 0.029(3) 0.023(3) 0.043(3) -0.002(2) 0.001(3) 0.004(2) C305 0.022(3) 0.042(4) 0.041(4) 0.004(3) -0.004(2) 0.002(3) C306 0.030(3) 0.025(3) 0.028(3) 0.000(2) -0.004(2) -0.004(2) C307 0.026(3) 0.027(3) 0.025(3) -0.002(2) 0.001(2) 0.001(2) C308 0.038(3) 0.045(4) 0.039(3) 0.010(3) -0.007(3) 0.000(3) C309 0.039(3) 0.039(4) 0.051(4) 0.015(3) -0.004(3) -0.001(3) C310 0.033(3) 0.029(3) 0.043(4) 0.014(3) -0.003(3) -0.004(2) C311 0.044(3) 0.040(3) 0.038(4) -0.002(3) -0.002(3) 0.004(3) C312 0.044(3) 0.030(3) 0.033(3) -0.001(3) -0.008(3) -0.007(3) C314 0.053(4) 0.066(4) 0.027(3) 0.013(3) -0.009(3) 0.015(3) C313 0.056(4) 0.058(4) 0.024(3) 0.008(3) 0.001(3) 0.009(3) N32 0.031(2) 0.036(3) 0.023(2) 0.008(2) -0.004(2) -0.002(2) Cl1 0.0422(8) 0.0495(9) 0.0352(8) -0.0115(7) 0.0099(7) -0.0099(7) O1 0.125(4) 0.064(3) 0.035(2) -0.004(2) 0.023(3) -0.002(3) O2 0.069(3) 0.051(3) 0.092(4) 0.023(3) -0.002(3) -0.016(2) O3 0.076(3) 0.080(3) 0.040(3) -0.020(2) 0.007(3) 0.028(3) O4 0.037(2) 0.145(5) 0.107(5) -0.066(4) -0.002(3) -0.009(3) Cl2 0.0383(8) 0.0608(10) 0.0341(8) 0.0029(7) -0.0028(7) 0.0034(7) O5 0.035(2) 0.054(3) 0.053(3) 0.004(2) -0.007(2) -0.0098(19) O6 0.063(3) 0.079(3) 0.042(3) 0.010(2) -0.017(2) 0.008(3) O7 0.078(4) 0.225(7) 0.066(4) -0.044(4) 0.001(3) 0.063(4) O8 0.128(5) 0.070(3) 0.089(4) 0.026(3) -0.021(4) -0.058(3) Cl3 0.0343(7) 0.0409(8) 0.0302(7) 0.0022(6) 0.0053(6) 0.0050(6) O9 0.037(2) 0.060(3) 0.037(2) 0.006(2) -0.0030(19) 0.0085(19) O10 0.047(2) 0.056(3) 0.047(3) -0.012(2) 0.022(2) -0.002(2) O11 0.085(3) 0.048(2) 0.041(3) 0.005(2) 0.003(2) 0.019(2) O12 0.032(2) 0.082(3) 0.058(3) -0.007(2) 0.006(2) -0.015(2) O14 0.051(3) 0.064(4) 0.139(6) -0.022(4) -0.010(3) -0.010(2) C1 0.070(5) 0.103(7) 0.120(8) -0.005(6) 0.012(6) -0.007(5) C2 0.140(13) 0.131(9) 0.059(10) -0.025(7) -0.007(11) 0.003(8) O15 0.111(6) 0.071(5) 0.101(6) 0.004(4) -0.033(6) 0.005(5) C2' 0.140(13) 0.131(9) 0.059(10) -0.025(7) -0.007(11) 0.003(8) O15' 0.111(6) 0.071(5) 0.101(6) 0.004(4) -0.033(6) 0.005(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O13 1.909(3) . ? Zn1 N21 2.019(4) . ? Zn1 N11 2.030(4) . ? Zn1 N12 2.085(4) . ? Zn2 O13 1.910(3) . ? Zn2 N22 2.007(4) . ? Zn2 N31 2.027(4) . ? Zn2 N32 2.041(4) . ? O13 H1O 0.877(5) . ? N11 C105 1.342(6) . ? N11 C101 1.347(6) . ? C101 C102 1.372(6) . ? C101 H101 0.9500 . ? C102 C103 1.411(7) . ? C102 H102 0.9500 . ? C103 C104 1.375(7) . ? C103 C106 1.498(6) . ? C104 C105 1.383(7) . ? C104 H104 0.9500 . ? C105 H105 0.9500 . ? C106 C107 1.507(7) . ? C106 H10A 0.9900 . ? C106 H10B 0.9900 . ? C107 C108 1.532(6) 2_445 ? C107 H10C 0.9900 . ? C107 H10D 0.9900 . ? C108 C109 1.497(7) . ? C108 C107 1.532(6) 2_455 ? C108 H10E 0.9900 . ? C108 H10F 0.9900 . ? C109 C110 1.495(7) . ? C109 H10G 0.9900 . ? C109 H10H 0.9900 . ? C110 C114 1.382(7) . ? C110 C111 1.404(7) . ? C111 C112 1.375(7) . ? C111 H111 0.9500 . ? C112 N12 1.342(6) . ? C112 H112 0.9500 . ? C113 N12 1.355(6) . ? C113 C114 1.366(7) . ? C113 H113 0.9500 . ? C114 H114 0.9500 . ? N21 C205 1.343(6) . ? N21 C201 1.353(6) . ? C201 C202 1.372(7) . ? C201 H201 0.9500 . ? C202 C203 1.393(7) . ? C202 H202 0.9500 . ? C203 C204 1.391(6) . ? C203 C206 1.506(7) . ? C204 C205 1.381(7) . ? C204 H204 0.9500 . ? C205 H205 0.9500 . ? C206 C207 1.541(7) . ? C206 H20A 0.9900 . ? C206 H20B 0.9900 . ? C207 C208 1.524(7) 4_576 ? C207 H20C 0.9900 . ? C207 H20D 0.9900 . ? C208 C207 1.524(7) 4_575 ? C208 C209 1.535(7) . ? C208 H20E 0.9900 . ? C208 H20F 0.9900 . ? C209 C210 1.500(7) . ? C209 H20G 0.9900 . ? C209 H20H 0.9900 . ? C210 C214 1.390(7) . ? C210 C211 1.396(7) . ? C211 C212 1.360(7) . ? C211 H211 0.9500 . ? C212 N22 1.363(7) . ? C212 H212 0.9500 . ? C213 N22 1.354(6) . ? C213 C214 1.378(7) . ? C213 H213 0.9500 . ? C214 H214 0.9500 . ? N31 C305 1.340(6) . ? N31 C301 1.356(6) . ? C302 C301 1.370(7) . ? C302 C303 1.386(7) . ? C302 H302 0.9500 . ? C301 H301 0.9500 . ? C303 C304 1.376(7) . ? C303 C306 1.508(6) . ? C304 C305 1.383(7) . ? C304 H304 0.9500 . ? C305 H305 0.9500 . ? C306 C307 1.529(6) . ? C306 H30A 0.9900 . ? C306 H30B 0.9900 . ? C307 C307 1.521(9) 3_465 ? C307 H30C 0.9900 . ? C307 H30D 0.9900 . ? C308 C309 1.516(7) . ? C308 C308 1.529(10) 3_475 ? C308 H30E 0.9900 . ? C308 H30F 0.9900 . ? C309 C310 1.514(7) . ? C309 H30G 0.9900 . ? C309 H30H 0.9900 . ? C310 C311 1.371(8) . ? C310 C314 1.376(8) . ? C311 C312 1.376(7) . ? C311 H311 0.9500 . ? C312 N32 1.347(6) . ? C312 H312 0.9500 . ? C314 C313 1.385(8) . ? C314 H314 0.9500 . ? C313 N32 1.346(6) . ? C313 H313 0.9500 . ? Cl1 O4 1.408(5) . ? Cl1 O2 1.410(4) . ? Cl1 O3 1.427(4) . ? Cl1 O1 1.429(4) . ? Cl2 O7 1.410(5) . ? Cl2 O5 1.422(4) . ? Cl2 O6 1.427(4) . ? Cl2 O8 1.447(5) . ? Cl3 O11 1.426(4) . ? Cl3 O12 1.434(4) . ? Cl3 O10 1.442(4) . ? Cl3 O9 1.447(4) . ? O14 H2O 0.8595 . ? O14 H3O 0.8386 . ? C1 O15 1.458(9) . ? C1 C2 1.461(7) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? O15 H4O 0.8400 . ? C2' O15' 1.470(12) . ? O15' H4O' 0.8400 . ? 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 O13 Zn1 N21 118.45(15) . . ? O13 Zn1 N11 118.23(15) . . ? N21 Zn1 N11 111.60(16) . . ? O13 Zn1 N12 103.73(15) . . ? N21 Zn1 N12 103.09(16) . . ? N11 Zn1 N12 97.58(15) . . ? O13 Zn2 N22 114.75(15) . . ? O13 Zn2 N31 111.40(14) . . ? N22 Zn2 N31 109.89(16) . . ? O13 Zn2 N32 112.75(15) . . ? N22 Zn2 N32 106.38(16) . . ? N31 Zn2 N32 100.67(16) . . ? Zn1 O13 Zn2 134.21(17) . . ? Zn1 O13 H1O 102(4) . . ? Zn2 O13 H1O 123(4) . . ? C105 N11 C101 116.8(4) . . ? C105 N11 Zn1 122.8(3) . . ? C101 N11 Zn1 120.1(3) . . ? N11 C101 C102 123.9(5) . . ? N11 C101 H101 118.1 . . ? C102 C101 H101 118.1 . . ? C101 C102 C103 119.2(4) . . ? C101 C102 H102 120.4 . . ? C103 C102 H102 120.4 . . ? C104 C103 C102 116.6(4) . . ? C104 C103 C106 123.1(4) . . ? C102 C103 C106 120.3(4) . . ? C103 C104 C105 120.9(5) . . ? C103 C104 H104 119.6 . . ? C105 C104 H104 119.6 . . ? N11 C105 C104 122.7(4) . . ? N11 C105 H105 118.7 . . ? C104 C105 H105 118.7 . . ? C103 C106 C107 112.9(4) . . ? C103 C106 H10A 109.0 . . ? C107 C106 H10A 109.0 . . ? C103 C106 H10B 109.0 . . ? C107 C106 H10B 109.0 . . ? H10A C106 H10B 107.8 . . ? C106 C107 C108 115.1(4) . 2_445 ? C106 C107 H10C 108.5 . . ? C108 C107 H10C 108.5 2_445 . ? C106 C107 H10D 108.5 . . ? C108 C107 H10D 108.5 2_445 . ? H10C C107 H10D 107.5 . . ? C109 C108 C107 110.8(4) . 2_455 ? C109 C108 H10E 109.5 . . ? C107 C108 H10E 109.5 2_455 . ? C109 C108 H10F 109.5 . . ? C107 C108 H10F 109.5 2_455 . ? H10E C108 H10F 108.1 . . ? C110 C109 C108 117.5(4) . . ? C110 C109 H10G 107.9 . . ? C108 C109 H10G 107.9 . . ? C110 C109 H10H 107.9 . . ? C108 C109 H10H 107.9 . . ? H10G C109 H10H 107.2 . . ? C114 C110 C111 115.8(4) . . ? C114 C110 C109 121.6(5) . . ? C111 C110 C109 122.6(4) . . ? C112 C111 C110 120.1(5) . . ? C112 C111 H111 120.0 . . ? C110 C111 H111 120.0 . . ? N12 C112 C111 122.7(5) . . ? N12 C112 H112 118.6 . . ? C111 C112 H112 118.6 . . ? N12 C113 C114 121.7(5) . . ? N12 C113 H113 119.1 . . ? C114 C113 H113 119.1 . . ? C113 C114 C110 121.7(5) . . ? C113 C114 H114 119.1 . . ? C110 C114 H114 119.1 . . ? C112 N12 C113 117.7(4) . . ? C112 N12 Zn1 120.6(3) . . ? C113 N12 Zn1 120.2(3) . . ? C205 N21 C201 116.4(4) . . ? C205 N21 Zn1 123.1(3) . . ? C201 N21 Zn1 120.5(3) . . ? N21 C201 C202 123.3(4) . . ? N21 C201 H201 118.4 . . ? C202 C201 H201 118.4 . . ? C201 C202 C203 120.3(5) . . ? C201 C202 H202 119.8 . . ? C203 C202 H202 119.8 . . ? C204 C203 C202 116.5(5) . . ? C204 C203 C206 121.9(4) . . ? C202 C203 C206 121.6(4) . . ? C205 C204 C203 120.0(4) . . ? C205 C204 H204 120.0 . . ? C203 C204 H204 120.0 . . ? N21 C205 C204 123.4(5) . . ? N21 C205 H205 118.3 . . ? C204 C205 H205 118.3 . . ? C203 C206 C207 115.6(4) . . ? C203 C206 H20A 108.4 . . ? C207 C206 H20A 108.4 . . ? C203 C206 H20B 108.4 . . ? C207 C206 H20B 108.4 . . ? H20A C206 H20B 107.5 . . ? C208 C207 C206 111.6(4) 4_576 . ? C208 C207 H20C 109.3 4_576 . ? C206 C207 H20C 109.3 . . ? C208 C207 H20D 109.3 4_576 . ? C206 C207 H20D 109.3 . . ? H20C C207 H20D 108.0 . . ? C207 C208 C209 113.1(5) 4_575 . ? C207 C208 H20E 108.9 4_575 . ? C209 C208 H20E 108.9 . . ? C207 C208 H20F 108.9 4_575 . ? C209 C208 H20F 108.9 . . ? H20E C208 H20F 107.8 . . ? C210 C209 C208 115.3(4) . . ? C210 C209 H20G 108.4 . . ? C208 C209 H20G 108.4 . . ? C210 C209 H20H 108.4 . . ? C208 C209 H20H 108.4 . . ? H20G C209 H20H 107.5 . . ? C214 C210 C211 116.2(5) . . ? C214 C210 C209 120.7(5) . . ? C211 C210 C209 123.1(5) . . ? C212 C211 C210 121.4(5) . . ? C212 C211 H211 119.3 . . ? C210 C211 H211 119.3 . . ? C211 C212 N22 122.1(5) . . ? C211 C212 H212 118.9 . . ? N22 C212 H212 118.9 . . ? N22 C213 C214 122.5(5) . . ? N22 C213 H213 118.8 . . ? C214 C213 H213 118.8 . . ? C213 C214 C210 120.5(5) . . ? C213 C214 H214 119.7 . . ? C210 C214 H214 119.7 . . ? C213 N22 C212 117.3(4) . . ? C213 N22 Zn2 120.3(3) . . ? C212 N22 Zn2 122.3(3) . . ? C305 N31 C301 116.5(4) . . ? C305 N31 Zn2 122.8(3) . . ? C301 N31 Zn2 120.6(3) . . ? C301 C302 C303 120.4(5) . . ? C301 C302 H302 119.8 . . ? C303 C302 H302 119.8 . . ? N31 C301 C302 123.3(5) . . ? N31 C301 H301 118.4 . . ? C302 C301 H301 118.4 . . ? C304 C303 C302 116.1(5) . . ? C304 C303 C306 122.5(5) . . ? C302 C303 C306 121.4(4) . . ? C303 C304 C305 121.4(5) . . ? C303 C304 H304 119.3 . . ? C305 C304 H304 119.3 . . ? N31 C305 C304 122.3(5) . . ? N31 C305 H305 118.9 . . ? C304 C305 H305 118.9 . . ? C303 C306 C307 113.4(4) . . ? C303 C306 H30A 108.9 . . ? C307 C306 H30A 108.9 . . ? C303 C306 H30B 108.9 . . ? C307 C306 H30B 108.9 . . ? H30A C306 H30B 107.7 . . ? C307 C307 C306 112.6(5) 3_465 . ? C307 C307 H30C 109.1 3_465 . ? C306 C307 H30C 109.1 . . ? C307 C307 H30D 109.1 3_465 . ? C306 C307 H30D 109.1 . . ? H30C C307 H30D 107.8 . . ? C309 C308 C308 113.6(5) . 3_475 ? C309 C308 H30E 108.8 . . ? C308 C308 H30E 108.8 3_475 . ? C309 C308 H30F 108.8 . . ? C308 C308 H30F 108.8 3_475 . ? H30E C308 H30F 107.7 . . ? C310 C309 C308 111.0(4) . . ? C310 C309 H30G 109.4 . . ? C308 C309 H30G 109.4 . . ? C310 C309 H30H 109.4 . . ? C308 C309 H30H 109.4 . . ? H30G C309 H30H 108.0 . . ? C311 C310 C314 117.4(5) . . ? C311 C310 C309 122.4(6) . . ? C314 C310 C309 120.0(5) . . ? C310 C311 C312 120.3(6) . . ? C310 C311 H311 119.9 . . ? C312 C311 H311 119.9 . . ? N32 C312 C311 123.0(5) . . ? N32 C312 H312 118.5 . . ? C311 C312 H312 118.5 . . ? C310 C314 C313 119.9(6) . . ? C310 C314 H314 120.1 . . ? C313 C314 H314 120.1 . . ? N32 C313 C314 122.8(6) . . ? N32 C313 H313 118.6 . . ? C314 C313 H313 118.6 . . ? C313 N32 C312 116.5(5) . . ? C313 N32 Zn2 119.3(4) . . ? C312 N32 Zn2 122.2(3) . . ? O4 Cl1 O2 110.0(3) . . ? O4 Cl1 O3 109.7(3) . . ? O2 Cl1 O3 108.4(3) . . ? O4 Cl1 O1 110.2(3) . . ? O2 Cl1 O1 108.6(3) . . ? O3 Cl1 O1 109.9(3) . . ? O7 Cl2 O5 110.2(3) . . ? O7 Cl2 O6 112.3(3) . . ? O5 Cl2 O6 109.7(3) . . ? O7 Cl2 O8 108.1(4) . . ? O5 Cl2 O8 106.8(3) . . ? O6 Cl2 O8 109.6(3) . . ? O11 Cl3 O12 108.7(3) . . ? O11 Cl3 O10 110.0(2) . . ? O12 Cl3 O10 109.6(2) . . ? O11 Cl3 O9 109.4(2) . . ? O12 Cl3 O9 109.3(2) . . ? O10 Cl3 O9 109.8(2) . . ? H2O O14 H3O 106.4 . . ? O15 C1 C2 102.1(5) . . ? O15 C1 H1A 111.3 . . ? C2 C1 H1A 111.3 . . ? O15 C1 H1B 111.3 . . ? C2 C1 H1B 111.3 . . ? H1A C1 H1B 109.2 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 O15 H4O 109.5 . . ? C2' O15' H4O' 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O13 H1O O14 0.877(5) 1.875(15) 2.734(6) 165(5) . O14 H3O O7 0.84 2.16 2.994(8) 171.5 2_655 _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.952 _refine_diff_density_max 0.489 _refine_diff_density_min -0.431 _refine_diff_density_rms 0.087 data_s92-2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H62.33 N9 O20.67 Zn3' _chemical_formula_weight 1184.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.1599(4) _cell_length_b 21.6360(10) _cell_length_c 19.4741(9) _cell_angle_alpha 90.00 _cell_angle_beta 103.855(2) _cell_angle_gamma 90.00 _cell_volume 5383.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.461 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2459 _exptl_absorpt_coefficient_mu 1.405 _exptl_absorpt_correction_type 'Empirical, SORTAV (R. H. Blessing, 1995, 1997)' _exptl_absorpt_correction_T_min 0.8169 _exptl_absorpt_correction_T_max 0.9330 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Enraf Nonius KappaCCD area detector' _diffrn_measurement_method '\p and \q scans to fill Ewald sphere' _diffrn_detector_area_resol_mean '9.091 pixels/mm' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 68514 _diffrn_reflns_av_R_equivalents 0.0706 _diffrn_reflns_av_sigmaI/netI 0.0995 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 25.05 _reflns_number_total 9523 _reflns_number_gt 5506 _reflns_threshold_expression >2sigma(I) _computing_data_reduction 'DENZO and COLLECT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'PLATON (Spek, 1990)' _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 w=1/[\s^2^(Fo^2^)+(0.0759P)^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 9523 _refine_ls_number_parameters 735 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1223 _refine_ls_R_factor_gt 0.0590 _refine_ls_wR_factor_ref 0.1504 _refine_ls_wR_factor_gt 0.1323 _refine_ls_goodness_of_fit_ref 0.952 _refine_ls_restrained_S_all 0.952 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.28316(4) 0.16386(2) 0.62163(3) 0.03021(17) Uani 1 d . . . Zn2 Zn 0.38458(4) 0.24749(3) 0.76415(3) 0.03359(18) Uani 1 d . . . Zn3 Zn 0.28516(4) 0.32480(2) 0.61248(3) 0.03024(17) Uani 1 d . . . O1 O 0.2673(3) 0.24279(14) 0.57395(19) 0.0326(8) Uani 1 d D . . H1 H 0.262(3) 0.2349(19) 0.5324(12) 0.019(14) Uiso 1 d D . . O2 O 0.3102(3) 0.17442(16) 0.72237(18) 0.0350(8) Uani 1 d D . . H2 H 0.334(3) 0.1428(15) 0.744(2) 0.034(16) Uiso 1 d D . . O3 O 0.3149(3) 0.31704(19) 0.7137(2) 0.0383(10) Uani 1 d . . . H3 H 0.318(5) 0.346(3) 0.733(3) 0.06(2) Uiso 1 d . . . N11 N 1.1485(3) 0.11464(17) 0.5939(2) 0.0293(9) Uani 1 d . . . N12 N 0.4016(3) 0.11833(18) 0.5928(2) 0.0312(10) Uani 1 d . . . N21 N 0.8931(3) 0.24833(17) 0.3679(2) 0.0346(10) Uani 1 d . . . N22 N 0.5298(3) 0.24234(18) 0.7457(2) 0.0327(10) Uani 1 d . . . N31 N 1.1504(3) 0.37327(17) 0.5809(2) 0.0302(10) Uani 1 d . . . N32 N 0.4067(3) 0.36674(18) 0.5843(2) 0.0305(10) Uani 1 d . . . C101 C 1.0918(4) 0.1150(2) 0.5268(3) 0.0299(12) Uani 1 d . . . H101 H 1.1197 0.1352 0.4920 0.017 Uiso 1 calc R . . C102 C 0.9949(4) 0.0875(2) 0.5062(3) 0.0335(12) Uani 1 d . . . H102 H 0.9570 0.0894 0.4582 0.036(14) Uiso 1 calc R . . C103 C 0.9525(4) 0.0567(2) 0.5555(3) 0.0317(12) Uani 1 d . . . C104 C 1.0134(4) 0.0566(2) 0.6251(3) 0.0429(14) Uani 1 d . . . H104 H 0.9884 0.0364 0.6611 0.042(14) Uiso 1 calc R . . C105 C 1.1078(4) 0.0853(2) 0.6412(3) 0.0401(13) Uani 1 d . . . H105 H 1.1472 0.0844 0.6890 0.050 Uiso 1 calc R . . C106 C 0.8478(3) 0.0258(2) 0.5351(3) 0.0335(12) Uani 1 d . . . H10A H 0.8536 -0.0160 0.5563 0.020(11) Uiso 1 calc R . . H10B H 0.8276 0.0209 0.4831 0.037(14) Uiso 1 calc R . . C107 C 0.7617(3) 0.0612(2) 0.5585(3) 0.0368(13) Uani 1 d . . . H10C H 0.7533 0.1027 0.5364 0.020(11) Uiso 1 calc R . . H10D H 0.7810 0.0666 0.6105 0.029(13) Uiso 1 calc R . . C108 C 0.6587(3) 0.0255(2) 0.5366(3) 0.0416(14) Uani 1 d . . . H10E H 0.6413 0.0194 0.4847 0.042(15) Uiso 1 calc R . . H10F H 0.6681 -0.0159 0.5590 0.049(16) Uiso 1 calc R . . C109 C 0.5689(3) 0.0576(2) 0.5569(3) 0.0349(13) Uani 1 d . . . C110 C 0.5194(4) 0.1080(2) 0.5175(3) 0.0416(14) Uani 1 d . . . H110 H 0.5421 0.1225 0.4776 0.022(12) Uiso 1 calc R . . C111 C 0.4370(4) 0.1364(2) 0.5377(3) 0.0371(13) Uani 1 d . . . H111 H 0.4040 0.1705 0.5107 0.028(13) Uiso 1 calc R . . C112 C 0.4493(4) 0.0708(2) 0.6305(3) 0.0368(13) Uani 1 d . . . H112 H 0.4250 0.0574 0.6703 0.032(13) Uiso 1 calc R . . C113 C 0.5327(4) 0.0400(2) 0.6144(3) 0.0350(12) Uani 1 d . . . H113 H 0.5650 0.0067 0.6432 0.070(19) Uiso 1 calc R . . C201 C 0.9847(4) 0.2502(2) 0.4165(3) 0.0355(12) Uani 1 d . . . H201 H 1.0473 0.2529 0.4005 0.027 Uiso 1 calc R . . C202 C 0.9928(4) 0.2486(2) 0.4878(3) 0.0372(13) Uani 1 d . . . H202 H 1.0595 0.2504 0.5201 0.044(15) Uiso 1 calc R . . C203 C 0.9030(4) 0.2442(2) 0.5123(3) 0.0347(12) Uani 1 d . . . C204 C 0.8070(4) 0.2421(3) 0.4619(3) 0.0509(16) Uani 1 d . . . H204 H 0.7434 0.2391 0.4767 0.08(2) Uiso 1 calc R . . C205 C 0.8052(4) 0.2446(2) 0.3905(3) 0.0477(15) Uani 1 d . . . H205 H 0.7398 0.2435 0.3568 0.049 Uiso 1 calc R . . C206 C 0.9129(4) 0.2404(3) 0.5910(3) 0.0472(15) Uani 1 d . . . H20A H 0.9502 0.2017 0.6087 0.055(17) Uiso 1 calc R . . H20B H 0.9570 0.2753 0.6138 0.069(19) Uiso 1 calc R . . C207 C 0.8117(4) 0.2419(2) 0.6141(3) 0.0399(13) Uani 1 d . . . H20C H 0.7670 0.2072 0.5915 0.035(13) Uiso 1 calc R . . H20D H 0.7745 0.2809 0.5976 0.034(13) Uiso 1 calc R . . C208 C 0.8282(4) 0.2371(3) 0.6948(3) 0.0455(15) Uani 1 d . . . H20E H 0.8650 0.1981 0.7118 0.051(16) Uiso 1 calc R . . H20F H 0.8722 0.2720 0.7179 0.025(12) Uiso 1 calc R . . C209 C 0.7253(4) 0.2387(2) 0.7144(3) 0.0367(13) Uani 1 d . . . C210 C 0.6755(4) 0.1855(3) 0.7282(3) 0.0387(13) Uani 1 d . . . H210 H 0.7084 0.1466 0.7270 0.048(15) Uiso 1 calc R . . C211 C 0.5803(4) 0.1883(2) 0.7434(3) 0.0363(13) Uani 1 d . . . H211 H 0.5480 0.1509 0.7526 0.026(12) Uiso 1 calc R . . C212 C 0.5762(4) 0.2946(2) 0.7314(2) 0.0334(12) Uani 1 d . . . H212 H 0.5411 0.3330 0.7318 0.050(16) Uiso 1 calc R . . C213 C 0.6731(4) 0.2940(3) 0.7160(3) 0.0437(14) Uani 1 d . . . H213 H 0.7041 0.3317 0.7065 0.051(16) Uiso 1 calc R . . C301 C 1.1027(4) 0.3815(2) 0.5125(3) 0.0340(12) Uani 1 d . . . H301 H 1.1371 0.3681 0.4775 0.051 Uiso 1 calc R . . C302 C 1.0054(4) 0.4089(2) 0.4912(3) 0.0344(12) Uani 1 d . . . H302 H 0.9737 0.4130 0.4422 0.030(13) Uiso 1 calc R . . C303 C 0.9544(3) 0.4300(2) 0.5401(3) 0.0305(12) Uani 1 d . . . C304 C 1.0051(4) 0.4214(2) 0.6113(3) 0.0398(13) Uani 1 d . . . H304 H 0.9731 0.4350 0.6475 0.051(16) Uiso 1 calc R . . C305 C 1.1005(4) 0.3936(2) 0.6284(3) 0.0386(13) Uani 1 d . . . H305 H 1.1335 0.3884 0.6771 0.025 Uiso 1 calc R . . C306 C 0.8495(3) 0.4605(2) 0.5202(3) 0.0391(14) Uani 1 d . . . H30A H 0.8301 0.4668 0.4683 0.048(16) Uiso 1 calc R . . H30B H 0.8546 0.5017 0.5428 0.046(15) Uiso 1 calc R . . C307 C 0.7630(3) 0.4237(2) 0.5416(3) 0.0362(13) Uani 1 d . . . H30C H 0.7557 0.3828 0.5181 0.029(12) Uiso 1 calc R . . H30D H 0.7817 0.4169 0.5934 0.027(13) Uiso 1 calc R . . C308 C 0.6595(3) 0.4586(2) 0.5205(3) 0.0403(14) Uani 1 d . . . H30E H 0.6689 0.5005 0.5416 0.036(14) Uiso 1 calc R . . H30F H 0.6397 0.4634 0.4685 0.059(18) Uiso 1 calc R . . C309 C 0.5725(4) 0.4266(2) 0.5438(3) 0.0361(13) Uani 1 d . . . C310 C 0.5344(4) 0.4471(2) 0.6003(3) 0.0400(14) Uani 1 d . . . H310 H 0.5654 0.4819 0.6270 0.045(15) Uiso 1 calc R . . C311 C 0.5258(4) 0.3741(2) 0.5093(3) 0.0420(14) Uani 1 d . . . H311 H 0.5493 0.3578 0.4705 0.026(12) Uiso 1 calc R . . C312 C 0.4513(4) 0.4170(2) 0.6178(3) 0.0426(14) Uani 1 d . . . H312 H 0.4249 0.4330 0.6555 0.037(14) Uiso 1 calc R . . C313 C 0.4452(4) 0.3457(2) 0.5312(3) 0.0438(14) Uani 1 d . . . H313 H 0.4156 0.3092 0.5073 0.021(11) Uiso 1 calc R . . N1 N 0.1285(4) 0.0921(2) 0.3352(3) 0.0523(13) Uani 1 d . . . O4 O 0.0533(3) 0.11220(18) 0.3583(2) 0.0558(11) Uani 1 d . . . O5 O 0.2204(3) 0.11046(18) 0.3645(2) 0.0597(11) Uani 1 d . . . O6 O 0.1140(4) 0.0547(2) 0.2862(2) 0.0736(13) Uani 1 d . . . N2 N 0.6067(5) 0.0941(3) 0.3332(3) 0.0728(17) Uani 1 d . . . O7 O 0.6943(4) 0.1073(2) 0.3742(3) 0.0963(17) Uani 1 d . . . O8 O 0.6024(4) 0.0544(2) 0.2868(2) 0.0773(14) Uani 1 d . . . O9 O 0.5245(4) 0.1216(2) 0.3394(3) 0.0890(16) Uani 1 d . . . N3 N 0.3230(4) 0.3643(2) 0.3672(2) 0.0478(12) Uani 1 d . . . O10 O 0.2465(3) 0.37518(19) 0.3930(2) 0.0581(11) Uani 1 d . . . O11 O 0.3603(3) 0.31004(17) 0.36983(19) 0.0479(10) Uani 1 d . . . O12 O 0.3610(3) 0.40656(19) 0.3370(2) 0.0686(12) Uani 1 d . . . O13 O 0.2388(3) 0.22633(19) 0.4292(2) 0.0529(10) Uani 1 d G . . H13A H 0.1734 0.2357 0.4182 0.079 Uiso 1 d G . . H13B H 0.2687 0.2518 0.4082 0.079 Uiso 1 d G . . O14 O 0.1029(3) 0.4601(2) 0.3054(3) 0.0581(11) Uani 1 d G . . H14A H 0.1221 0.4923 0.2859 0.049(19) Uiso 1 d G . . H14B H 0.1577 0.4445 0.3304 0.09(3) Uiso 1 d G . . O15 O 0.3377(4) 0.0708(2) 0.2494(2) 0.0756(13) Uani 1 d G . . H15A H 0.2815 0.0730 0.2643 0.113 Uiso 1 d G . . H15B H 0.3861 0.0845 0.2821 0.113 Uiso 1 d G . . O16 O 0.5542(3) 0.2505(2) 0.3648(3) 0.0857(16) Uani 1 d G . . H16A H 0.5021 0.2749 0.3631 0.129 Uiso 1 d G . . H16B H 0.5383 0.2168 0.3808 0.129 Uiso 1 d G . . O17 O 0.8448(3) 0.0758(2) 0.2921(2) 0.0648(12) Uani 1 d G . . H17A H 0.9089 0.0836 0.3127 0.097 Uiso 1 d G . . H17A H 0.8141 0.0684 0.3243 0.097 Uiso 1 d G . . O18 O 0.4005(4) 0.07905(18) 0.8063(2) 0.0531(10) Uani 1 d G . . H18A H 0.4591 0.0606 0.8087 0.07(2) Uiso 1 d G . . H18B H 0.3571 0.0514 0.8093 0.029(15) Uiso 1 d G . . O19 O 0.2270(3) 0.0120(2) 0.8185(2) 0.0694(12) Uani 1 d G . . H19A H 0.2097 -0.0137 0.7840 0.104 Uiso 1 d G . . H19B H 0.1746 0.0346 0.8166 0.104 Uiso 1 d G . . O20 O 0.0982(5) 0.1923(3) 0.7445(4) 0.0714(19) Uani 0.67 d PG . . H20A H 0.1609 0.1842 0.7415 0.107 Uiso 0.67 d PG . . H20B H 0.1031 0.2210 0.7741 0.107 Uiso 0.67 d PG . . O21 O 0.0697(5) 0.0959(8) 0.8213(4) 0.101(4) Uani 0.88(3) d PG A 1 H21A H 0.0046 0.1028 0.8185 0.151 Uiso 0.88(3) d PG A 1 H21B H 0.0725 0.0629 0.7991 0.151 Uiso 0.88(3) d PG A 1 O21' O 0.060(4) 0.1305(7) 0.818(3) 0.082(18) Uani 0.12(3) d PG A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0279(3) 0.0274(3) 0.0355(4) -0.0020(3) 0.0078(3) -0.0010(2) Zn2 0.0331(3) 0.0358(4) 0.0310(4) -0.0006(3) 0.0060(3) -0.0008(3) Zn3 0.0286(3) 0.0268(3) 0.0353(4) 0.0003(3) 0.0077(3) 0.0003(2) O1 0.043(2) 0.025(2) 0.029(2) -0.0016(17) 0.0078(17) 0.0001(15) O2 0.037(2) 0.032(2) 0.035(2) -0.0005(18) 0.0055(16) -0.0027(17) O3 0.044(2) 0.035(2) 0.034(2) 0.001(2) 0.0065(17) 0.0032(18) N11 0.031(2) 0.025(2) 0.031(3) 0.0001(19) 0.008(2) -0.0011(17) N12 0.032(2) 0.030(2) 0.033(3) -0.002(2) 0.011(2) 0.0006(18) N21 0.034(2) 0.041(3) 0.028(2) 0.0011(19) 0.007(2) 0.0008(19) N22 0.031(2) 0.036(3) 0.027(2) 0.0012(19) -0.0005(19) 0.0004(19) N31 0.028(2) 0.028(2) 0.034(3) 0.0007(19) 0.006(2) -0.0005(17) N32 0.030(2) 0.028(2) 0.034(3) -0.001(2) 0.0076(19) 0.0027(18) C101 0.039(3) 0.021(3) 0.034(3) -0.001(2) 0.017(3) -0.007(2) C102 0.035(3) 0.033(3) 0.031(3) -0.002(2) 0.006(3) 0.005(2) C103 0.037(3) 0.024(3) 0.036(3) 0.001(2) 0.014(3) 0.003(2) C104 0.041(3) 0.049(4) 0.041(4) 0.010(3) 0.014(3) -0.009(3) C105 0.036(3) 0.047(4) 0.037(3) 0.005(3) 0.008(3) -0.010(3) C106 0.032(3) 0.026(3) 0.043(4) 0.000(2) 0.010(2) -0.003(2) C107 0.036(3) 0.027(3) 0.051(4) -0.005(3) 0.019(3) 0.001(2) C108 0.028(3) 0.030(3) 0.065(4) -0.015(3) 0.009(3) -0.007(2) C109 0.024(3) 0.036(3) 0.043(3) -0.007(3) 0.004(2) -0.003(2) C110 0.041(3) 0.041(3) 0.051(4) 0.006(3) 0.025(3) -0.001(3) C111 0.035(3) 0.033(3) 0.044(4) 0.008(3) 0.011(3) 0.010(2) C112 0.040(3) 0.036(3) 0.035(3) 0.002(3) 0.010(3) 0.001(2) C113 0.036(3) 0.027(3) 0.039(3) 0.003(2) 0.004(3) 0.008(2) C201 0.034(3) 0.034(3) 0.036(3) 0.002(2) 0.004(2) 0.004(2) C202 0.042(3) 0.023(3) 0.043(4) 0.003(2) 0.002(3) -0.001(2) C203 0.044(3) 0.023(3) 0.037(3) -0.004(2) 0.009(3) 0.001(2) C204 0.044(3) 0.073(5) 0.038(4) 0.001(3) 0.014(3) 0.001(3) C205 0.039(3) 0.068(4) 0.035(4) -0.007(3) 0.008(3) -0.008(3) C206 0.043(3) 0.060(4) 0.040(4) -0.005(3) 0.012(3) 0.000(3) C207 0.042(3) 0.039(3) 0.039(3) -0.002(3) 0.009(3) 0.003(3) C208 0.045(3) 0.056(4) 0.037(3) -0.001(3) 0.013(3) 0.000(3) C209 0.036(3) 0.049(4) 0.026(3) 0.002(3) 0.009(2) 0.000(3) C210 0.041(3) 0.037(3) 0.037(3) 0.004(3) 0.008(3) 0.011(3) C211 0.035(3) 0.029(3) 0.043(3) 0.002(2) 0.007(3) -0.001(2) C212 0.035(3) 0.032(3) 0.033(3) -0.005(2) 0.008(2) -0.003(2) C213 0.050(4) 0.043(4) 0.035(3) -0.004(3) 0.004(3) -0.013(3) C301 0.043(3) 0.028(3) 0.036(3) 0.002(2) 0.018(3) 0.001(2) C302 0.033(3) 0.034(3) 0.037(3) 0.011(2) 0.009(3) -0.002(2) C303 0.030(3) 0.019(3) 0.042(3) 0.003(2) 0.009(3) -0.006(2) C304 0.034(3) 0.044(3) 0.045(4) -0.005(3) 0.015(3) 0.006(2) C305 0.040(3) 0.042(3) 0.034(3) -0.004(3) 0.008(3) 0.006(2) C306 0.033(3) 0.033(3) 0.052(4) 0.010(3) 0.010(3) -0.003(2) C307 0.035(3) 0.027(3) 0.047(4) 0.007(3) 0.011(3) 0.003(2) C308 0.031(3) 0.037(3) 0.054(4) 0.008(3) 0.012(3) 0.000(2) C309 0.028(3) 0.037(3) 0.045(3) 0.015(3) 0.010(3) 0.006(2) C310 0.034(3) 0.026(3) 0.062(4) -0.004(3) 0.015(3) -0.004(2) C311 0.039(3) 0.051(4) 0.038(3) -0.011(3) 0.015(3) -0.012(3) C312 0.044(3) 0.037(3) 0.053(4) -0.006(3) 0.024(3) 0.000(3) C313 0.044(3) 0.038(3) 0.048(4) -0.012(3) 0.007(3) -0.012(3) N1 0.073(4) 0.045(3) 0.041(3) 0.015(3) 0.016(3) 0.000(3) O4 0.060(3) 0.064(3) 0.048(3) -0.002(2) 0.022(2) -0.010(2) O5 0.051(3) 0.046(3) 0.078(3) 0.007(2) 0.008(2) -0.004(2) O6 0.116(4) 0.054(3) 0.055(3) -0.011(2) 0.029(3) -0.005(3) N2 0.095(5) 0.061(4) 0.070(5) 0.010(3) 0.035(4) -0.006(4) O7 0.091(4) 0.112(5) 0.081(4) -0.015(3) 0.010(3) -0.021(3) O8 0.113(4) 0.062(3) 0.060(3) -0.007(3) 0.027(3) -0.006(3) O9 0.091(4) 0.085(4) 0.101(4) -0.011(3) 0.044(3) 0.012(3) N3 0.048(3) 0.049(3) 0.043(3) 0.000(3) 0.005(2) -0.001(3) O10 0.052(2) 0.075(3) 0.056(3) 0.002(2) 0.029(2) 0.012(2) O11 0.048(2) 0.043(3) 0.051(3) -0.0045(19) 0.0088(19) 0.0050(19) O12 0.071(3) 0.051(3) 0.088(3) 0.006(2) 0.028(3) -0.013(2) O13 0.051(2) 0.062(3) 0.047(3) 0.003(2) 0.014(2) -0.008(2) O14 0.050(3) 0.046(3) 0.075(3) 0.001(2) 0.009(3) 0.006(2) O15 0.076(3) 0.072(3) 0.083(3) 0.017(3) 0.026(3) 0.024(3) O16 0.053(3) 0.086(4) 0.120(5) 0.016(3) 0.022(3) 0.006(3) O17 0.070(3) 0.056(3) 0.060(3) 0.016(2) -0.001(2) -0.003(2) O18 0.056(3) 0.047(3) 0.057(3) 0.010(2) 0.014(2) 0.002(2) O19 0.063(3) 0.075(4) 0.070(3) 0.009(2) 0.014(2) -0.012(2) O20 0.054(4) 0.082(6) 0.079(5) -0.013(4) 0.017(4) -0.007(4) O21 0.076(5) 0.120(12) 0.115(6) 0.007(6) 0.041(4) 0.028(5) O21' 0.11(4) 0.01(2) 0.11(4) 0.04(2) 0.00(3) 0.06(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 O2 1.922(3) . ? Zn1 O1 1.931(3) . ? Zn1 N11 2.027(4) 1_455 ? Zn1 N12 2.033(4) . ? Zn2 O3 1.908(4) . ? Zn2 O2 1.934(3) . ? Zn2 N21 2.000(4) 4_566 ? Zn2 N22 2.031(4) . ? Zn3 O1 1.919(3) . ? Zn3 O3 1.922(4) . ? Zn3 N31 2.025(4) 1_455 ? Zn3 N32 2.026(4) . ? O1 H1 0.813(19) . ? O2 H2 0.827(19) . ? O3 H3 0.73(5) . ? N11 C105 1.332(6) . ? N11 C101 1.340(6) . ? N11 Zn1 2.027(4) 1_655 ? N12 C111 1.327(6) . ? N12 C112 1.331(6) . ? N21 C205 1.334(6) . ? N21 C201 1.344(6) . ? N21 Zn2 2.000(4) 4_665 ? N22 C212 1.346(6) . ? N22 C211 1.352(6) . ? N31 C305 1.331(6) . ? N31 C301 1.341(6) . ? N31 Zn3 2.025(4) 1_655 ? N32 C312 1.330(6) . ? N32 C313 1.337(6) . ? C101 C102 1.377(6) . ? C101 H101 0.9500 . ? C102 C103 1.389(6) . ? C102 H102 0.9500 . ? C103 C104 1.400(7) . ? C103 C106 1.498(6) . ? C104 C105 1.357(6) . ? C104 H104 0.9500 . ? C105 H105 0.9500 . ? C106 C107 1.524(6) . ? C106 H10A 0.9900 . ? C106 H10B 0.9900 . ? C107 C108 1.529(6) . ? C107 H10C 0.9900 . ? C107 H10D 0.9900 . ? C108 C109 1.504(6) . ? C108 H10E 0.9900 . ? C108 H10F 0.9900 . ? C109 C113 1.372(7) . ? C109 C110 1.400(7) . ? C110 C111 1.383(6) . ? C110 H110 0.9500 . ? C111 H111 0.9500 . ? C112 C113 1.382(6) . ? C112 H112 0.9500 . ? C113 H113 0.9500 . ? C201 C202 1.368(7) . ? C201 H201 0.9500 . ? C202 C203 1.379(7) . ? C202 H202 0.9500 . ? C203 C204 1.402(7) . ? C203 C206 1.509(7) . ? C204 C205 1.387(8) . ? C204 H204 0.9500 . ? C205 H205 0.9500 . ? C206 C207 1.504(7) . ? C206 H20A 0.9900 . ? C206 H20B 0.9900 . ? C207 C208 1.539(7) . ? C207 H20C 0.9900 . ? C207 H20D 0.9900 . ? C208 C209 1.491(7) . ? C208 H20E 0.9900 . ? C208 H20F 0.9900 . ? C209 C210 1.382(7) . ? C209 C213 1.385(7) . ? C210 C211 1.355(6) . ? C210 H210 0.9500 . ? C211 H211 0.9500 . ? C212 C213 1.378(7) . ? C212 H212 0.9500 . ? C213 H213 0.9500 . ? C301 C302 1.380(6) . ? C301 H301 0.9500 . ? C302 C303 1.369(6) . ? C302 H302 0.9500 . ? C303 C304 1.400(7) . ? C303 C306 1.494(6) . ? C304 C305 1.360(6) . ? C304 H304 0.9500 . ? C305 H305 0.9500 . ? C306 C307 1.527(6) . ? C306 H30A 0.9900 . ? C306 H30B 0.9900 . ? C307 C308 1.526(6) . ? C307 H30C 0.9900 . ? C307 H30D 0.9900 . ? C308 C309 1.498(6) . ? C308 H30E 0.9900 . ? C308 H30F 0.9900 . ? C309 C310 1.386(7) . ? C309 C311 1.387(7) . ? C310 C312 1.383(7) . ? C310 H310 0.9500 . ? C311 C313 1.378(7) . ? C311 H311 0.9500 . ? C312 H312 0.9500 . ? C313 H313 0.9500 . ? N1 O6 1.230(6) . ? N1 O4 1.259(5) . ? N1 O5 1.272(5) . ? N2 O8 1.238(7) . ? N2 O9 1.266(6) . ? N2 O7 1.267(7) . ? N3 O10 1.249(5) . ? N3 O12 1.255(5) . ? N3 O11 1.269(5) . ? O13 H13A 0.8596 . ? O13 H13B 0.8387 . ? O14 H14A 0.8594 . ? O14 H14B 0.8389 . ? O15 H15A 0.8598 . ? O15 H15B 0.8388 . ? O16 H16A 0.8597 . ? O16 H16B 0.8380 . ? O17 H17A 0.8592 . ? O17 H17A 0.8390 . ? O18 H18A 0.8595 . ? O18 H18B 0.8393 . ? O19 H19A 0.8594 . ? O19 H19B 0.8383 . ? O20 H20A 0.8593 . ? O20 H20B 0.8393 . ? O21 H21A 0.8596 . ? O21 H21B 0.8384 . ? O21' H21A 0.9493 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Zn1 O1 110.98(15) . . ? O2 Zn1 N11 105.71(15) . 1_455 ? O1 Zn1 N11 110.47(15) . 1_455 ? O2 Zn1 N12 111.88(15) . . ? O1 Zn1 N12 107.30(16) . . ? N11 Zn1 N12 110.55(15) 1_455 . ? O3 Zn2 O2 107.20(17) . . ? O3 Zn2 N21 112.90(17) . 4_566 ? O2 Zn2 N21 111.24(15) . 4_566 ? O3 Zn2 N22 107.97(16) . . ? O2 Zn2 N22 106.50(15) . . ? N21 Zn2 N22 110.74(16) 4_566 . ? O1 Zn3 O3 107.21(16) . . ? O1 Zn3 N31 110.11(15) . 1_455 ? O3 Zn3 N31 107.79(16) . 1_455 ? O1 Zn3 N32 109.80(15) . . ? O3 Zn3 N32 109.66(16) . . ? N31 Zn3 N32 112.13(15) 1_455 . ? Zn3 O1 Zn1 129.8(2) . . ? Zn3 O1 H1 124(3) . . ? Zn1 O1 H1 106(3) . . ? Zn1 O2 Zn2 118.56(18) . . ? Zn1 O2 H2 112(3) . . ? Zn2 O2 H2 112(3) . . ? Zn2 O3 Zn3 123.5(2) . . ? Zn2 O3 H3 116(5) . . ? Zn3 O3 H3 116(5) . . ? C105 N11 C101 117.1(4) . . ? C105 N11 Zn1 122.4(3) . 1_655 ? C101 N11 Zn1 120.2(3) . 1_655 ? C111 N12 C112 117.6(4) . . ? C111 N12 Zn1 121.4(3) . . ? C112 N12 Zn1 120.9(3) . . ? C205 N21 C201 118.2(5) . . ? C205 N21 Zn2 119.5(3) . 4_665 ? C201 N21 Zn2 122.3(3) . 4_665 ? C212 N22 C211 118.0(4) . . ? C212 N22 Zn2 118.9(3) . . ? C211 N22 Zn2 123.0(3) . . ? C305 N31 C301 117.0(4) . . ? C305 N31 Zn3 120.1(3) . 1_655 ? C301 N31 Zn3 122.6(3) . 1_655 ? C312 N32 C313 117.0(4) . . ? C312 N32 Zn3 121.2(3) . . ? C313 N32 Zn3 121.8(3) . . ? N11 C101 C102 122.7(4) . . ? N11 C101 H101 118.6 . . ? C102 C101 H101 118.6 . . ? C101 C102 C103 120.2(5) . . ? C101 C102 H102 119.9 . . ? C103 C102 H102 119.9 . . ? C102 C103 C104 116.0(4) . . ? C102 C103 C106 121.8(4) . . ? C104 C103 C106 122.1(5) . . ? C105 C104 C103 120.2(5) . . ? C105 C104 H104 119.9 . . ? C103 C104 H104 119.9 . . ? N11 C105 C104 123.7(5) . . ? N11 C105 H105 118.2 . . ? C104 C105 H105 118.2 . . ? C103 C106 C107 113.6(4) . . ? C103 C106 H10A 108.8 . . ? C107 C106 H10A 108.8 . . ? C103 C106 H10B 108.8 . . ? C107 C106 H10B 108.8 . . ? H10A C106 H10B 107.7 . . ? C106 C107 C108 109.6(4) . . ? C106 C107 H10C 109.8 . . ? C108 C107 H10C 109.8 . . ? C106 C107 H10D 109.8 . . ? C108 C107 H10D 109.8 . . ? H10C C107 H10D 108.2 . . ? C109 C108 C107 113.1(4) . . ? C109 C108 H10E 109.0 . . ? C107 C108 H10E 109.0 . . ? C109 C108 H10F 109.0 . . ? C107 C108 H10F 109.0 . . ? H10E C108 H10F 107.8 . . ? C113 C109 C110 117.2(5) . . ? C113 C109 C108 122.3(5) . . ? C110 C109 C108 120.5(5) . . ? C111 C110 C109 118.9(5) . . ? C111 C110 H110 120.6 . . ? C109 C110 H110 120.6 . . ? N12 C111 C110 123.4(5) . . ? N12 C111 H111 118.3 . . ? C110 C111 H111 118.3 . . ? N12 C112 C113 122.8(5) . . ? N12 C112 H112 118.6 . . ? C113 C112 H112 118.6 . . ? C109 C113 C112 120.1(5) . . ? C109 C113 H113 119.9 . . ? C112 C113 H113 119.9 . . ? N21 C201 C202 123.5(5) . . ? N21 C201 H201 118.2 . . ? C202 C201 H201 118.2 . . ? C201 C202 C203 119.2(5) . . ? C201 C202 H202 120.4 . . ? C203 C202 H202 120.4 . . ? C202 C203 C204 117.7(5) . . ? C202 C203 C206 118.8(5) . . ? C204 C203 C206 123.5(5) . . ? C205 C204 C203 119.7(5) . . ? C205 C204 H204 120.2 . . ? C203 C204 H204 120.2 . . ? N21 C205 C204 121.7(5) . . ? N21 C205 H205 119.2 . . ? C204 C205 H205 119.2 . . ? C207 C206 C203 115.8(5) . . ? C207 C206 H20A 108.3 . . ? C203 C206 H20A 108.3 . . ? C207 C206 H20B 108.3 . . ? C203 C206 H20B 108.3 . . ? H20A C206 H20B 107.4 . . ? C206 C207 C208 112.7(4) . . ? C206 C207 H20C 109.0 . . ? C208 C207 H20C 109.0 . . ? C206 C207 H20D 109.0 . . ? C208 C207 H20D 109.0 . . ? H20C C207 H20D 107.8 . . ? C209 C208 C207 110.2(4) . . ? C209 C208 H20E 109.6 . . ? C207 C208 H20E 109.6 . . ? C209 C208 H20F 109.6 . . ? C207 C208 H20F 109.6 . . ? H20E C208 H20F 108.1 . . ? C210 C209 C213 117.0(5) . . ? C210 C209 C208 122.2(5) . . ? C213 C209 C208 120.8(5) . . ? C211 C210 C209 120.9(5) . . ? C211 C210 H210 119.6 . . ? C209 C210 H210 119.6 . . ? N22 C211 C210 122.2(5) . . ? N22 C211 H211 118.9 . . ? C210 C211 H211 118.9 . . ? N22 C212 C213 121.7(5) . . ? N22 C212 H212 119.1 . . ? C213 C212 H212 119.1 . . ? C212 C213 C209 120.2(5) . . ? C212 C213 H213 119.9 . . ? C209 C213 H213 119.9 . . ? N31 C301 C302 122.4(5) . . ? N31 C301 H301 118.8 . . ? C302 C301 H301 118.8 . . ? C303 C302 C301 120.5(5) . . ? C303 C302 H302 119.8 . . ? C301 C302 H302 119.8 . . ? C302 C303 C304 116.6(4) . . ? C302 C303 C306 122.9(5) . . ? C304 C303 C306 120.5(5) . . ? C305 C304 C303 119.6(5) . . ? C305 C304 H304 120.2 . . ? C303 C304 H304 120.2 . . ? N31 C305 C304 123.8(5) . . ? N31 C305 H305 118.1 . . ? C304 C305 H305 118.1 . . ? C303 C306 C307 113.7(4) . . ? C303 C306 H30A 108.8 . . ? C307 C306 H30A 108.8 . . ? C303 C306 H30B 108.8 . . ? C307 C306 H30B 108.8 . . ? H30A C306 H30B 107.7 . . ? C308 C307 C306 110.1(4) . . ? C308 C307 H30C 109.6 . . ? C306 C307 H30C 109.6 . . ? C308 C307 H30D 109.6 . . ? C306 C307 H30D 109.6 . . ? H30C C307 H30D 108.1 . . ? C309 C308 C307 112.7(4) . . ? C309 C308 H30E 109.0 . . ? C307 C308 H30E 109.0 . . ? C309 C308 H30F 109.0 . . ? C307 C308 H30F 109.0 . . ? H30E C308 H30F 107.8 . . ? C310 C309 C311 116.4(5) . . ? C310 C309 C308 122.7(5) . . ? C311 C309 C308 121.0(5) . . ? C312 C310 C309 120.1(5) . . ? C312 C310 H310 119.9 . . ? C309 C310 H310 119.9 . . ? C313 C311 C309 120.1(5) . . ? C313 C311 H311 120.0 . . ? C309 C311 H311 120.0 . . ? N32 C312 C310 123.1(5) . . ? N32 C312 H312 118.4 . . ? C310 C312 H312 118.4 . . ? N32 C313 C311 123.3(5) . . ? N32 C313 H313 118.4 . . ? C311 C313 H313 118.4 . . ? O6 N1 O4 121.1(5) . . ? O6 N1 O5 120.6(5) . . ? O4 N1 O5 118.4(5) . . ? O8 N2 O9 120.4(7) . . ? O8 N2 O7 119.4(7) . . ? O9 N2 O7 120.3(7) . . ? O10 N3 O12 120.0(5) . . ? O10 N3 O11 120.0(5) . . ? O12 N3 O11 119.9(5) . . ? H13A O13 H13B 106.3 . . ? H14A O14 H14B 106.3 . . ? H15A O15 H15B 106.3 . . ? H16A O16 H16B 106.4 . . ? H17A O17 H17A 106.4 . . ? H18A O18 H18B 106.3 . . ? H19A O19 H19B 106.4 . . ? H20A O20 H20B 106.4 . . ? 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 C103 C106 C107 C108 -179.0(4) . . . . ? C106 C107 C108 C109 -179.3(5) . . . . ? C203 C206 C207 C208 179.4(4) . . . . ? C206 C207 C208 C209 -179.9(4) . . . . ? C303 C306 C307 C308 179.0(5) . . . . ? C306 C307 C308 C309 -176.7(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 O13 0.813(19) 1.97(2) 2.776(5) 172(4) . O2 H2 O18 0.827(19) 1.90(2) 2.723(5) 171(5) . O13 H13B O11 0.84 2.01 2.839(5) 171.1 . O14 H14B O10 0.84 2.10 2.883(6) 154.9 . O15 H15A O6 0.86 2.38 3.212(6) 164.3 . O15 H15A O5 0.86 2.42 3.132(6) 140.4 . O15 H15B O9 0.84 2.06 2.874(7) 164.0 . O16 H16A O11 0.86 2.05 2.881(6) 162.9 . O16 H16B O9 0.84 2.20 2.842(8) 133.0 . O17 H17A O7 0.84 2.21 2.909(7) 141.3 . O18 H18B O19 0.84 1.96 2.763(6) 160.2 . O19 H19B O21 0.84 1.93 2.762(13) 170.8 . O19 H19B O21' 0.84 2.57 3.37(4) 161.5 . O20 H20A O2 0.86 2.10 2.948(7) 171.5 . O20 H20B O16 0.84 2.11 2.830(9) 143.5 4_566 O21 H21A O12 0.86 2.02 2.837(7) 159.2 4_566 O19 H19A O17 0.86 2.00 2.856(6) 173.4 3_656 O18 H18A O14 0.86 1.96 2.800(6) 164.7 4_666 O3 H3 O17 0.73(5) 2.03(5) 2.753(6) 173(6) 4_566 O14 H14A O15 0.86 1.95 2.807(6) 173.3 2 O17 H17A O4 0.86 1.99 2.850(5) 173.2 1_655 _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 0.626 _refine_diff_density_min -0.616 _refine_diff_density_rms 0.095 data_s92-3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C136 H180 Cl6 N16 O27 Zn4' _chemical_formula_weight 2945.14 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 Orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, z+1/2' 'x+1/2, y, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, -z-1/2' '-x-1/2, -y, z-1/2' 'x, -y-1/2, z' _cell_length_a 17.2550(4) _cell_length_b 34.4538(6) _cell_length_c 24.5191(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 14576.6(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.342 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6184 _exptl_absorpt_coefficient_mu 0.834 _exptl_absorpt_correction_type 'Empirical, SORTAV (R. H. Blessing, 1995, 1997)' _exptl_absorpt_correction_T_min 0.8852 _exptl_absorpt_correction_T_max 0.8852 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enraf Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf Nonius KappaCCD area detector' _diffrn_measurement_method '\p and \q scans to fill Ewald sphere' _diffrn_detector_area_resol_mean '9.091 pixels/mm' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 72134 _diffrn_reflns_av_R_equivalents 0.1513 _diffrn_reflns_av_sigmaI/netI 0.1070 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 23.00 _reflns_number_total 10274 _reflns_number_gt 3898 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DENZO (Otwinowski and Minor, 1997)COLLECT (Hooft, 1998) ' _computing_cell_refinement 'DENZO and COLLECT' _computing_data_reduction 'DENZO and COLLECT' _computing_structure_solution 'DIRDIF-96 (Beurskens, 1996)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'PLATON (Spek, 1990)' _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^)+(0.0000P)^2^+50.0000P] 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 10274 _refine_ls_number_parameters 722 _refine_ls_number_restraints 930 _refine_ls_R_factor_all 0.2385 _refine_ls_R_factor_gt 0.1108 _refine_ls_wR_factor_ref 0.2210 _refine_ls_wR_factor_gt 0.1996 _refine_ls_goodness_of_fit_ref 1.272 _refine_ls_restrained_S_all 1.278 _refine_ls_shift/su_max 0.029 _refine_ls_shift/su_mean 0.001 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 0.00925(7) 0.19925(3) 0.02645(5) 0.0746(4) Uani 1 1 d D . . O1 O -0.0002(6) 0.2500 0.0551(3) 0.070(2) Uani 1 2 d SD . . H1O H -0.007(10) 0.2500 0.0886(12) 0.139 Uiso 1 2 d SD . . N11 N -0.0849(5) 0.1676(3) 0.0475(4) 0.071(2) Uani 1 1 d D . . N12 N -0.3990(4) 0.1713(2) 0.4422(3) 0.063(2) Uani 1 1 d D . . C101 C -0.0976(7) 0.1323(3) 0.0268(4) 0.085(3) Uani 1 1 d D . . H101 H -0.0613 0.1219 0.0029 0.102 Uiso 1 1 calc R . . C102 C -0.1618(7) 0.1108(3) 0.0394(4) 0.088(4) Uani 1 1 d D . . H102 H -0.1693 0.0869 0.0225 0.106 Uiso 1 1 calc R . . C103 C -0.2153(6) 0.1238(4) 0.0763(5) 0.087(4) Uani 1 1 d D . . C104 C -0.2004(6) 0.1595(4) 0.0982(5) 0.108(4) Uani 1 1 d D . . H104 H -0.2344 0.1698 0.1238 0.129 Uiso 1 1 calc R . . C105 C -0.1366(6) 0.1805(3) 0.0833(4) 0.089(4) Uani 1 1 d D . . H105 H -0.1290 0.2048 0.0988 0.107 Uiso 1 1 calc R . . C106 C -0.2865(7) 0.1016(4) 0.0910(6) 0.144(6) Uani 1 1 d D . . H10A H -0.3250 0.1195 0.1052 0.173 Uiso 1 1 calc R . . H10B H -0.3077 0.0898 0.0583 0.173 Uiso 1 1 calc R . . C107 C -0.2723(8) 0.0718(5) 0.1308(5) 0.160(7) Uani 1 1 d D . . H10C H -0.3169 0.0547 0.1324 0.191 Uiso 1 1 calc R . . H10D H -0.2280 0.0565 0.1194 0.191 Uiso 1 1 calc R . . C108 C -0.2577(11) 0.0873(5) 0.1842(6) 0.207(8) Uiso 1 1 d D . . H10E H -0.3006 0.1045 0.1928 0.248 Uiso 1 1 calc R . . H10F H -0.2119 0.1035 0.1814 0.248 Uiso 1 1 calc R . . C109 C -0.2466(13) 0.0625(6) 0.2309(8) 0.282(12) Uiso 1 1 d D . . H10G H -0.2886 0.0439 0.2346 0.338 Uiso 1 1 calc R . . H10H H -0.1978 0.0486 0.2288 0.338 Uiso 1 1 calc R . . C110 C -0.2466(16) 0.0900(8) 0.2751(8) 0.346(15) Uiso 1 1 d D . . H11A H -0.2064 0.1086 0.2661 0.415 Uiso 1 1 calc R . . H11B H -0.2953 0.1039 0.2718 0.415 Uiso 1 1 calc R . . C111 C -0.2377(14) 0.0828(6) 0.3318(8) 0.280(13) Uiso 1 1 d D . . H11C H -0.2048 0.0601 0.3344 0.336 Uiso 1 1 calc R . . H11D H -0.2884 0.0748 0.3446 0.336 Uiso 1 1 calc R . . C112 C -0.2092(6) 0.1093(4) 0.3721(6) 0.143(6) Uani 1 1 d D . . H11E H -0.1736 0.1275 0.3554 0.171 Uiso 1 1 calc R . . H11F H -0.1815 0.0951 0.4001 0.171 Uiso 1 1 calc R . . C113 C -0.2751(6) 0.1306(3) 0.3969(4) 0.078(3) Uani 1 1 d D . . C114 C -0.3179(6) 0.1153(3) 0.4383(5) 0.081(3) Uani 1 1 d D . . H114 H -0.3057 0.0910 0.4522 0.097 Uiso 1 1 calc R . . C115 C -0.3787(6) 0.1356(3) 0.4592(4) 0.086(3) Uani 1 1 d D . . H115 H -0.4078 0.1242 0.4868 0.103 Uiso 1 1 calc R . . C116 C -0.3560(6) 0.1864(3) 0.4025(4) 0.085(4) Uani 1 1 d D . . H116 H -0.3675 0.2112 0.3901 0.102 Uiso 1 1 calc R . . C117 C -0.2955(6) 0.1667(3) 0.3792(5) 0.097(4) Uani 1 1 d D . . H117 H -0.2679 0.1782 0.3508 0.116 Uiso 1 1 calc R . . N21 N 0.0123(6) 0.1971(2) -0.0555(3) 0.073(2) Uani 1 1 d D . . N22 N -0.0248(7) -0.0824(4) -0.4600(5) 0.112(4) Uani 1 1 d D . . C201 C 0.0771(6) 0.1950(3) -0.0851(5) 0.085(4) Uani 1 1 d D . . H201 H 0.1243 0.1934 -0.0668 0.102 Uiso 1 1 calc R . . C202 C 0.0777(7) 0.1951(3) -0.1407(5) 0.093(4) Uani 1 1 d D . . H202 H 0.1247 0.1941 -0.1593 0.111 Uiso 1 1 calc R . . C203 C 0.0099(8) 0.1966(3) -0.1692(4) 0.080(3) Uani 1 1 d D . . C204 C -0.0561(7) 0.1986(3) -0.1387(5) 0.093(4) Uani 1 1 d D . . H204 H -0.1037 0.2003 -0.1564 0.112 Uiso 1 1 calc R . . C205 C -0.0542(6) 0.1984(3) -0.0832(5) 0.083(3) Uani 1 1 d D . . H205 H -0.1007 0.1991 -0.0641 0.099 Uiso 1 1 calc R . . C206 C 0.0120(8) 0.1963(3) -0.2319(4) 0.128(5) Uani 1 1 d D . . H20A H -0.0213 0.2171 -0.2446 0.154 Uiso 1 1 calc R . . H20B H 0.0644 0.2028 -0.2430 0.154 Uiso 1 1 calc R . . C207 C -0.0103(10) 0.1614(3) -0.2604(7) 0.222(8) Uiso 1 1 d D . . H20C H -0.0664 0.1598 -0.2585 0.266 Uiso 1 1 calc R . . H20D H 0.0027 0.1654 -0.2985 0.266 Uiso 1 1 calc R . . C208 C 0.0185(10) 0.1244(4) -0.2459(6) 0.258(10) Uiso 1 1 d D . . H20E H 0.0058 0.1206 -0.2077 0.309 Uiso 1 1 calc R . . H20F H 0.0746 0.1261 -0.2479 0.309 Uiso 1 1 calc R . . C209 C -0.0033(10) 0.0893(4) -0.2737(6) 0.269(11) Uiso 1 1 d D . . H20G H 0.0272 0.0685 -0.2579 0.322 Uiso 1 1 calc R . . H20H H -0.0569 0.0841 -0.2643 0.322 Uiso 1 1 calc R . . C210 C 0.0029(13) 0.0857(4) -0.3314(6) 0.313(13) Uiso 1 1 d D . . H21A H 0.0418 0.1042 -0.3432 0.376 Uiso 1 1 calc R . . H21B H -0.0461 0.0943 -0.3466 0.376 Uiso 1 1 calc R . . C211 C 0.0212(13) 0.0493(5) -0.3571(9) 0.406(19) Uiso 1 1 d D . . H21C H 0.0163 0.0533 -0.3961 0.488 Uiso 1 1 calc R . . H21D H 0.0755 0.0443 -0.3500 0.488 Uiso 1 1 calc R . . C212 C -0.0195(11) 0.0144(5) -0.3447(8) 0.261(10) Uiso 1 1 d D . . H21E H -0.0724 0.0214 -0.3358 0.313 Uiso 1 1 calc R . . H21F H 0.0034 0.0035 -0.3120 0.313 Uiso 1 1 calc R . . C213 C -0.0224(9) -0.0180(5) -0.3881(6) 0.150(7) Uani 1 1 d D . . C214 C 0.0119(10) -0.0527(6) -0.3769(6) 0.169(8) Uani 1 1 d D . . H214 H 0.0405 -0.0551 -0.3450 0.203 Uiso 1 1 calc R . . C215 C 0.0063(8) -0.0840(4) -0.4103(7) 0.134(5) Uani 1 1 d D . . H215 H 0.0251 -0.1077 -0.3979 0.161 Uiso 1 1 calc R . . C216 C -0.0573(8) -0.0484(4) -0.4720(5) 0.108(4) Uani 1 1 d D . . H216 H -0.0838 -0.0462 -0.5049 0.130 Uiso 1 1 calc R . . C217 C -0.0539(8) -0.0166(4) -0.4390(7) 0.129(6) Uani 1 1 d D . . H217 H -0.0737 0.0068 -0.4517 0.155 Uiso 1 1 calc R . . Zn2 Zn 0.00274(8) 0.19948(4) -0.45102(5) 0.0855(4) Uani 1 1 d D . . O2 O -0.0166(6) 0.2500 -0.4223(4) 0.102(3) Uani 1 2 d SD . . H2O H -0.015(4) 0.2500 -0.3885(4) 0.204 Uiso 1 2 d SD . . N31 N -0.0890(5) 0.1655(3) -0.4317(4) 0.076(3) Uani 1 1 d D . . N32 N -0.4042(5) 0.1729(3) -0.0784(4) 0.072(3) Uani 1 1 d D . . C301 C -0.0998(6) 0.1320(3) -0.4580(4) 0.082(3) Uani 1 1 d D . . H301 H -0.0637 0.1248 -0.4843 0.098 Uiso 1 1 calc R . . C302 C -0.1613(7) 0.1075(3) -0.4486(4) 0.086(4) Uani 1 1 d D . . H302 H -0.1661 0.0845 -0.4680 0.103 Uiso 1 1 calc R . . C303 C -0.2155(6) 0.1177(4) -0.4102(5) 0.084(4) Uani 1 1 d D . . C304 C -0.2038(8) 0.1513(4) -0.3814(5) 0.108(5) Uani 1 1 d D . . H304 H -0.2376 0.1582 -0.3536 0.130 Uiso 1 1 calc R . . C305 C -0.1420(7) 0.1746(3) -0.3940(5) 0.093(4) Uani 1 1 d D . . H305 H -0.1366 0.1979 -0.3753 0.111 Uiso 1 1 calc R . . C306 C -0.2855(7) 0.0925(4) -0.3965(6) 0.146(6) Uani 1 1 d D . . H30A H -0.3223 0.1080 -0.3759 0.175 Uiso 1 1 calc R . . H30B H -0.3106 0.0849 -0.4303 0.175 Uiso 1 1 calc R . . C307 C -0.2678(11) 0.0581(5) -0.3656(8) 0.219(9) Uiso 1 1 d D . . H30C H -0.3107 0.0400 -0.3680 0.263 Uiso 1 1 calc R . . H30D H -0.2222 0.0456 -0.3807 0.263 Uiso 1 1 calc R . . C308 C -0.2542(13) 0.0679(7) -0.3099(8) 0.279(11) Uiso 1 1 d D . . H30E H -0.2031 0.0796 -0.3122 0.334 Uiso 1 1 calc R . . H30F H -0.2891 0.0897 -0.3053 0.334 Uiso 1 1 calc R . . C309 C -0.2528(14) 0.0525(7) -0.2558(8) 0.279(11) Uiso 1 1 d D . . H30G H -0.2054 0.0374 -0.2551 0.335 Uiso 1 1 calc R . . H30H H -0.2944 0.0336 -0.2561 0.335 Uiso 1 1 calc R . . C310 C -0.2567(12) 0.0688(6) -0.2018(8) 0.248(10) Uiso 1 1 d D . . H31A H -0.3094 0.0774 -0.1952 0.297 Uiso 1 1 calc R . . H31B H -0.2453 0.0485 -0.1756 0.297 Uiso 1 1 calc R . . C311 C -0.2054(14) 0.1006(7) -0.1923(7) 0.310(14) Uiso 1 1 d D . . H31C H -0.2225 0.1232 -0.2124 0.372 Uiso 1 1 calc R . . H31D H -0.1534 0.0940 -0.2041 0.372 Uiso 1 1 calc R . . C312 C -0.2062(7) 0.1083(4) -0.1350(6) 0.163(7) Uani 1 1 d D . . H31E H -0.1591 0.1221 -0.1254 0.195 Uiso 1 1 calc R . . H31F H -0.2060 0.0838 -0.1155 0.195 Uiso 1 1 calc R . . C313 C -0.2752(6) 0.1320(4) -0.1164(5) 0.086(4) Uani 1 1 d D . . C314 C -0.2965(7) 0.1669(4) -0.1378(5) 0.101(4) Uani 1 1 d D . . H314 H -0.2674 0.1777 -0.1659 0.121 Uiso 1 1 calc R . . C315 C -0.3599(7) 0.1862(3) -0.1185(4) 0.086(4) Uani 1 1 d D . . H315 H -0.3727 0.2099 -0.1343 0.103 Uiso 1 1 calc R . . C316 C -0.3833(6) 0.1385(3) -0.0580(4) 0.085(4) Uani 1 1 d D . . H316 H -0.4139 0.1278 -0.0306 0.101 Uiso 1 1 calc R . . C317 C -0.3198(7) 0.1181(3) -0.0749(4) 0.085(4) Uani 1 1 d D . . H317 H -0.3071 0.0947 -0.0582 0.102 Uiso 1 1 calc R . . N41 N 0.0045(7) 0.1978(2) -0.5315(4) 0.079(2) Uani 1 1 d D . . N42 N -0.0246(7) -0.0771(4) -0.9500(6) 0.115(4) Uani 1 1 d D . . C401 C 0.0694(6) 0.1971(3) -0.5609(5) 0.095(4) Uani 1 1 d D . . H401 H 0.1164 0.1968 -0.5424 0.114 Uiso 1 1 calc R . . C402 C 0.0712(7) 0.1968(3) -0.6167(6) 0.093(4) Uani 1 1 d D . . H402 H 0.1188 0.1963 -0.6345 0.112 Uiso 1 1 calc R . . C403 C 0.0044(8) 0.1974(3) -0.6467(5) 0.085(3) Uani 1 1 d D . . C404 C -0.0628(7) 0.1995(3) -0.6175(6) 0.091(4) Uani 1 1 d D . . H404 H -0.1102 0.2015 -0.6352 0.109 Uiso 1 1 calc R . . C405 C -0.0595(6) 0.1987(3) -0.5619(6) 0.086(3) Uani 1 1 d D . . H405 H -0.1066 0.1987 -0.5434 0.103 Uiso 1 1 calc R . . C406 C 0.0040(8) 0.1950(3) -0.7079(5) 0.112(4) Uani 1 1 d D . . H40A H -0.0401 0.2093 -0.7219 0.135 Uiso 1 1 calc R . . H40B H 0.0507 0.2071 -0.7220 0.135 Uiso 1 1 calc R . . C407 C 0.0000(10) 0.1555(4) -0.7271(5) 0.157(6) Uani 1 1 d D . . H40C H 0.0448 0.1424 -0.7117 0.188 Uiso 1 1 calc R . . H40D H -0.0450 0.1441 -0.7095 0.188 Uiso 1 1 calc R . . C408 C -0.0037(14) 0.1434(7) -0.7831(6) 0.275(11) Uiso 1 1 d D . . H40E H 0.0393 0.1543 -0.8035 0.330 Uiso 1 1 calc R . . H40F H -0.0517 0.1523 -0.7996 0.330 Uiso 1 1 calc R . . C409 C 0.0000(15) 0.1012(7) -0.7844(10) 0.312(13) Uiso 1 1 d D . . H40G H 0.0463 0.0915 -0.7665 0.375 Uiso 1 1 calc R . . H40H H -0.0455 0.0895 -0.7682 0.375 Uiso 1 1 calc R . . C410 C 0.0026(16) 0.0956(7) -0.8418(10) 0.315(13) Uiso 1 1 d D . . H41A H 0.0408 0.1136 -0.8561 0.378 Uiso 1 1 calc R . . H41B H -0.0472 0.1037 -0.8561 0.378 Uiso 1 1 calc R . . C411 C 0.0193(14) 0.0583(7) -0.8653(10) 0.323(14) Uiso 1 1 d D . . H41C H 0.0141 0.0610 -0.9045 0.387 Uiso 1 1 calc R . . H41D H 0.0735 0.0528 -0.8581 0.387 Uiso 1 1 calc R . . C412 C -0.0237(13) 0.0248(6) -0.8497(9) 0.317(14) Uiso 1 1 d D . . H41E H -0.0766 0.0329 -0.8427 0.381 Uiso 1 1 calc R . . H41F H -0.0027 0.0156 -0.8154 0.381 Uiso 1 1 calc R . . C413 C -0.0266(9) -0.0093(4) -0.8886(6) 0.147(7) Uani 1 1 d D . . C414 C 0.0175(9) -0.0402(5) -0.8744(7) 0.164(7) Uani 1 1 d D . . H414 H 0.0526 -0.0381 -0.8457 0.197 Uiso 1 1 calc R . . C415 C 0.0106(8) -0.0743(5) -0.9019(7) 0.152(7) Uani 1 1 d D . . H415 H 0.0313 -0.0967 -0.8864 0.183 Uiso 1 1 calc R . . C416 C -0.0604(8) -0.0450(4) -0.9668(5) 0.115(5) Uani 1 1 d D . . H416 H -0.0876 -0.0460 -0.9995 0.138 Uiso 1 1 calc R . . C417 C -0.0595(8) -0.0108(4) -0.9390(7) 0.134(6) Uani 1 1 d D . . H417 H -0.0812 0.0114 -0.9544 0.161 Uiso 1 1 calc R . . Cl1 Cl 0.2528(2) -0.00056(11) 0.04446(16) 0.1128(11) Uani 1 1 d G . . O11 O 0.2756(5) 0.0304(2) 0.0113(4) 0.227(6) Uani 1 1 d G . . O12 O 0.2287(5) -0.0325(2) 0.0148(4) 0.238(7) Uani 1 1 d G . . O13 O 0.1915(4) 0.0113(3) 0.0789(4) 0.252(7) Uani 1 1 d G . . O14 O 0.3144(4) -0.0096(3) 0.0795(3) 0.239(6) Uani 1 1 d G . . Cl2 Cl 0.2371(3) 0.2437(5) -0.4878(2) 0.125(3) Uani 0.50 1 d PG . . O21 O 0.1611(4) 0.2500(7) -0.4696(4) 0.135(5) Uiso 1 2 d SG . . O22 O 0.2475(7) 0.2552(7) -0.5414(4) 0.200(8) Uiso 0.50 1 d PG . . O23 O 0.2579(8) 0.2042(5) -0.4832(5) 0.116(5) Uiso 0.50 1 d PG . . O24 O 0.2868(7) 0.2636(5) -0.4522(6) 0.326(18) Uiso 0.50 1 d PG . . Cl3 Cl 0.2511(3) 0.2417(4) 0.0010(2) 0.115(4) Uani 0.50 1 d PG . . O31 O 0.2544(6) 0.2018(4) -0.0095(6) 0.116(6) Uani 0.50 1 d PG . . O32 O 0.1784(6) 0.2573(6) -0.0085(5) 0.169(10) Uani 0.50 1 d PG . . O33 O 0.3053(8) 0.2616(5) -0.0322(5) 0.251(13) Uiso 0.50 1 d PG . . O34 O 0.2758(6) 0.2500(6) 0.0548(3) 0.154(5) Uani 1 2 d SG . . Cl4 Cl -0.2207(3) 0.2500 -0.2648(2) 0.145(2) Uani 1 2 d SG . . O41 O -0.1978(9) 0.2557(7) -0.2111(3) 0.276(7) Uiso 0.50 1 d PG . . O42 O -0.1649(7) 0.2590(6) -0.3022(5) 0.276(7) Uiso 0.50 1 d PG . . O43 O -0.2891(6) 0.2694(4) -0.2753(8) 0.276(7) Uiso 0.50 1 d PG . . O44 O -0.2420(10) 0.20888(15) -0.2711(10) 0.276(7) Uiso 0.50 1 d PG . . Cl5 Cl -0.2393(4) 0.2564(6) -0.7592(3) 0.239(5) Uiso 0.50 1 d PG . . O51 O -0.3034(9) 0.2337(7) -0.7453(11) 0.351(11) Uiso 0.50 1 d PG . . O52 O -0.1849(11) 0.2363(8) -0.7896(9) 0.351(11) Uiso 0.50 1 d PG . . O53 O -0.2032(14) 0.2704(8) -0.7114(7) 0.351(11) Uiso 0.50 1 d PG . . O54 O -0.2660(13) 0.2896(8) -0.7867(9) 0.351(11) Uiso 0.50 1 d PG . . O100 O -0.0230(12) 0.2500 -0.8328(8) 0.269(9) Uiso 1 2 d S . . 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 0.0856(9) 0.0503(8) 0.0878(9) -0.0038(7) -0.0020(8) 0.0019(7) O1 0.095(7) 0.041(5) 0.073(6) 0.000 0.003(7) 0.000 N11 0.078(6) 0.056(7) 0.077(6) 0.002(5) 0.010(5) 0.004(5) N12 0.066(6) 0.038(6) 0.085(7) 0.002(5) -0.003(5) 0.001(5) C101 0.094(10) 0.064(9) 0.096(9) -0.002(8) 0.018(7) -0.005(7) C102 0.098(10) 0.083(10) 0.084(9) -0.013(7) 0.000(8) -0.018(9) C103 0.082(9) 0.078(10) 0.101(10) 0.020(8) -0.008(8) -0.020(8) C104 0.065(9) 0.102(12) 0.156(13) -0.008(10) 0.009(9) 0.009(8) C105 0.086(9) 0.059(8) 0.123(11) -0.020(8) -0.007(8) -0.003(8) C106 0.112(12) 0.177(17) 0.143(14) 0.030(12) 0.006(10) -0.053(11) C107 0.141(13) 0.24(2) 0.094(11) -0.005(12) 0.014(10) -0.110(14) C112 0.092(10) 0.085(11) 0.252(18) -0.003(11) 0.022(11) 0.003(9) C113 0.065(8) 0.063(9) 0.106(10) -0.014(7) 0.006(7) 0.006(7) C114 0.078(8) 0.045(8) 0.121(11) -0.002(7) -0.002(8) 0.012(7) C115 0.090(9) 0.054(9) 0.115(10) 0.006(7) 0.018(8) -0.001(7) C116 0.093(9) 0.052(8) 0.111(10) 0.015(7) 0.005(8) -0.005(7) C117 0.083(9) 0.071(10) 0.137(11) -0.005(9) 0.028(8) -0.004(8) N21 0.071(6) 0.057(6) 0.090(7) -0.007(5) -0.013(6) 0.007(6) N22 0.105(9) 0.110(10) 0.121(10) -0.021(8) -0.008(7) 0.008(7) C201 0.056(8) 0.078(9) 0.120(12) -0.012(8) 0.000(8) 0.000(7) C202 0.103(11) 0.102(10) 0.073(9) -0.009(8) 0.024(9) -0.016(8) C203 0.099(9) 0.055(7) 0.087(9) -0.012(6) -0.021(10) 0.007(8) C204 0.073(9) 0.084(9) 0.122(13) -0.005(9) -0.018(9) 0.015(8) C205 0.085(10) 0.083(9) 0.080(9) -0.005(8) 0.014(8) 0.010(8) C206 0.170(13) 0.116(11) 0.098(10) -0.014(8) -0.032(9) -0.027(11) C213 0.187(19) 0.152(17) 0.112(13) -0.061(12) -0.020(12) -0.016(13) C214 0.153(15) 0.20(2) 0.156(15) -0.086(15) -0.071(12) 0.052(16) C215 0.117(12) 0.091(12) 0.193(17) -0.007(11) -0.034(13) 0.032(10) C216 0.116(11) 0.112(13) 0.096(10) -0.005(10) -0.001(8) -0.014(10) C217 0.161(14) 0.061(10) 0.166(16) -0.024(10) 0.042(13) -0.014(9) Zn2 0.1084(10) 0.0516(8) 0.0966(10) -0.0031(7) -0.0096(9) 0.0030(9) O2 0.115(9) 0.052(7) 0.139(9) 0.000 0.015(8) 0.000 N31 0.096(7) 0.045(7) 0.086(7) -0.012(5) -0.005(6) -0.003(5) N32 0.086(7) 0.046(6) 0.083(7) 0.012(5) -0.002(5) 0.003(5) C301 0.086(9) 0.067(9) 0.092(9) 0.011(8) 0.018(7) -0.001(7) C302 0.103(10) 0.075(9) 0.081(9) 0.004(7) 0.007(8) -0.007(8) C303 0.080(9) 0.089(11) 0.082(9) 0.000(8) -0.020(8) -0.021(8) C304 0.104(12) 0.130(15) 0.090(10) -0.005(10) 0.007(9) -0.005(10) C305 0.115(11) 0.068(10) 0.095(10) -0.018(8) -0.004(9) 0.019(9) C306 0.090(10) 0.161(16) 0.188(15) 0.011(13) -0.020(10) -0.031(11) C312 0.088(11) 0.216(19) 0.185(17) 0.034(14) 0.022(10) 0.037(12) C313 0.075(9) 0.081(11) 0.103(10) 0.022(8) 0.011(8) 0.005(8) C314 0.091(10) 0.115(13) 0.096(10) -0.011(10) 0.020(8) -0.029(9) C315 0.098(10) 0.060(9) 0.099(10) 0.016(7) 0.010(8) -0.004(8) C316 0.067(8) 0.089(11) 0.098(9) -0.008(8) 0.010(7) -0.010(7) C317 0.090(9) 0.079(9) 0.086(9) 0.006(8) -0.018(8) 0.006(8) N41 0.065(6) 0.061(6) 0.111(7) -0.005(5) -0.006(7) -0.009(6) N42 0.095(9) 0.100(10) 0.149(12) -0.019(8) 0.016(8) 0.008(7) C401 0.085(11) 0.097(10) 0.102(11) 0.003(9) -0.029(9) -0.021(9) C402 0.087(10) 0.086(10) 0.106(12) 0.001(9) 0.006(9) -0.014(8) C403 0.106(10) 0.054(7) 0.096(10) -0.014(7) 0.000(11) 0.003(9) C404 0.087(10) 0.087(10) 0.099(11) -0.008(9) -0.014(9) 0.010(8) C405 0.074(10) 0.065(8) 0.119(12) -0.007(9) 0.009(9) 0.005(7) C406 0.148(11) 0.085(9) 0.104(10) -0.013(8) -0.025(10) -0.001(10) C407 0.192(15) 0.160(15) 0.118(12) -0.065(10) -0.012(11) 0.016(13) C413 0.196(19) 0.097(13) 0.146(15) -0.082(12) -0.017(13) -0.007(11) C414 0.147(15) 0.167(18) 0.180(16) -0.095(15) -0.056(12) 0.036(14) C415 0.134(13) 0.153(17) 0.171(16) -0.055(13) -0.075(12) 0.054(12) C416 0.134(13) 0.109(13) 0.102(11) -0.009(11) -0.004(9) -0.027(11) C417 0.157(14) 0.083(12) 0.163(17) -0.035(11) 0.013(12) -0.018(10) Cl1 0.112(2) 0.068(2) 0.158(3) 0.002(2) -0.001(3) 0.0072(18) O11 0.276(15) 0.131(11) 0.273(15) 0.089(11) 0.084(12) 0.010(10) O12 0.275(15) 0.125(11) 0.313(17) -0.097(11) -0.055(12) -0.019(10) O13 0.220(13) 0.252(16) 0.284(16) -0.004(13) 0.106(13) 0.075(12) O14 0.207(13) 0.263(17) 0.247(14) 0.013(12) -0.066(12) 0.054(12) Cl2 0.115(4) 0.123(9) 0.138(5) 0.020(8) 0.001(4) 0.011(7) Cl3 0.106(5) 0.115(12) 0.124(5) -0.004(6) -0.023(4) -0.026(6) O31 0.078(10) 0.131(16) 0.138(14) -0.048(13) 0.026(10) -0.031(11) O32 0.235(17) 0.03(2) 0.245(18) -0.049(16) -0.161(16) 0.048(16) O34 0.124(11) 0.149(14) 0.189(15) 0.000 -0.028(11) 0.000 Cl4 0.179(6) 0.134(5) 0.121(4) 0.000 -0.037(4) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O1 1.892(3) . ? Zn1 N12 2.006(8) 3 ? Zn1 N21 2.011(8) . ? Zn1 N11 2.025(8) . ? O1 Zn1 1.892(3) 8_565 ? N11 C105 1.328(6) . ? N11 C101 1.336(6) . ? N12 C116 1.330(6) . ? N12 C115 1.343(6) . ? N12 Zn1 2.006(8) 3_455 ? C101 C102 1.368(6) . ? C102 C103 1.368(6) . ? C103 C104 1.368(6) . ? C103 C106 1.490(11) . ? C104 C105 1.368(6) . ? C106 C107 1.438(7) . ? C107 C108 1.438(7) . ? C108 C109 1.444(7) . ? C109 C110 1.440(7) . ? C110 C111 1.419(7) . ? C111 C112 1.430(7) . ? C112 C113 1.484(11) . ? C113 C114 1.361(6) . ? C113 C117 1.364(6) . ? C114 C115 1.362(6) . ? C116 C117 1.370(6) . ? N21 C205 1.335(6) . ? N21 C201 1.336(6) . ? N22 C216 1.331(6) . ? N22 C215 1.333(6) . ? C201 C202 1.364(6) . ? C202 C203 1.365(6) . ? C203 C204 1.363(6) . ? C203 C206 1.537(12) . ? C204 C205 1.361(6) . ? C206 C207 1.444(7) . ? C207 C208 1.415(7) . ? C208 C209 1.440(7) . ? C209 C210 1.425(7) . ? C210 C211 1.438(7) . ? C211 C212 1.423(7) . ? C212 C213 1.543(13) . ? C213 C217 1.362(6) . ? C213 C214 1.362(6) . ? C214 C215 1.356(6) . ? C216 C217 1.363(6) . ? Zn2 O2 1.907(5) . ? Zn2 N41 1.975(9) . ? Zn2 N32 1.984(8) 3_554 ? Zn2 N31 2.025(9) . ? O2 Zn2 1.907(5) 8_565 ? N31 C301 1.336(6) . ? N31 C305 1.338(6) . ? N32 C315 1.328(6) . ? N32 C316 1.335(6) . ? N32 Zn2 1.984(8) 3_454 ? C301 C302 1.373(6) . ? C302 C303 1.373(6) . ? C303 C304 1.370(6) . ? C303 C306 1.526(12) . ? C304 C305 1.368(6) . ? C306 C307 1.440(7) . ? C307 C308 1.429(7) . ? C308 C309 1.428(7) . ? C309 C310 1.440(7) . ? C310 C311 1.428(7) . ? C311 C312 1.430(7) . ? C312 C313 1.514(12) . ? C313 C317 1.362(6) . ? C313 C314 1.364(6) . ? C314 C315 1.364(6) . ? C316 C317 1.367(6) . ? N41 C405 1.332(6) . ? N41 C401 1.333(6) . ? N42 C415 1.331(6) . ? N42 C416 1.333(6) . ? C401 C402 1.367(6) . ? C402 C403 1.368(6) . ? C403 C404 1.366(6) . ? C403 C406 1.504(12) . ? C404 C405 1.364(6) . ? C406 C407 1.443(7) . ? C407 C408 1.437(7) . ? C408 C409 1.454(7) . ? C409 C410 1.423(7) . ? C410 C411 1.436(7) . ? C411 C412 1.426(7) . ? C412 C413 1.515(14) . ? C413 C414 1.354(6) . ? C413 C417 1.363(6) . ? C414 C415 1.360(6) . ? C416 C417 1.361(6) . ? Cl1 O12 1.3838 . ? Cl1 O11 1.3982 . ? Cl1 O14 1.4033 . ? Cl1 O13 1.4126 . ? Cl2 Cl2 0.44(3) 8_565 ? Cl2 O24 1.250(7) 8_565 ? Cl2 O22 1.3263(15) 8_565 ? Cl2 O22 1.3838 . ? Cl2 O21 1.4030 . ? Cl2 O24 1.4032 . ? Cl2 O23 1.4126 . ? Cl2 O23 1.84(3) 8_565 ? O21 Cl2 1.403(8) 8_565 ? O22 O22 0.36(5) 8_565 ? O22 Cl2 1.326(5) 8_565 ? O23 O24 1.44(3) 8_565 ? O23 Cl2 1.84(3) 8_565 ? O24 O24 0.94(4) 8_565 ? O24 Cl2 1.250(9) 8_565 ? O24 O23 1.44(3) 8_565 ? Cl3 Cl3 0.57(3) 8_565 ? Cl3 O33 1.244(3) 8_565 ? Cl3 O32 1.2759(12) 8_565 ? Cl3 O32 1.3837 . ? Cl3 O31 1.3982 . ? Cl3 O34 1.4154 . ? Cl3 O33 1.4165 . ? Cl3 O31 1.96(3) 8_565 ? O31 O33 1.63(3) 8_565 ? O31 Cl3 1.96(3) 8_565 ? O32 O32 0.50(4) 8_565 ? O32 Cl3 1.276(6) 8_565 ? O33 O33 0.80(3) 8_565 ? O33 Cl3 1.244(6) 8_565 ? O33 O31 1.63(2) 8_565 ? O34 Cl3 1.415(8) 8_565 ? Cl4 O42 1.365(9) 8_565 ? Cl4 O42 1.3654 . ? Cl4 O43 1.380(15) 8_565 ? Cl4 O43 1.3796 . ? Cl4 O41 1.3893 . ? Cl4 O41 1.389(6) 8_565 ? Cl4 O44 1.4712 . ? Cl4 O44 1.471(10) 8_565 ? O41 O41 0.39(5) 8_565 ? O42 O42 0.62(4) 8_565 ? O43 O44 1.110(7) 8_565 ? O43 O43 1.34(3) 8_565 ? O44 O43 1.11(2) 8_565 ? Cl5 Cl5 0.44(4) 8_565 ? Cl5 O51 1.207(15) 8_565 ? Cl5 O52 1.224(11) 8_565 ? Cl5 O52 1.3838 . ? Cl5 O51 1.3983 . ? Cl5 O54 1.4033 . ? Cl5 O53 1.4127 . ? Cl5 O53 1.62(3) 8_565 ? Cl5 O54 1.78(5) 8_565 ? O51 O51 1.12(5) 8_565 ? O51 Cl5 1.207(13) 8_565 ? O51 O54 1.44(3) 8_565 ? O52 O52 0.94(5) 8_565 ? O52 Cl5 1.224(10) 8_565 ? O52 O54 1.66(3) 8_565 ? O53 O53 1.41(5) 8_565 ? O53 Cl5 1.62(2) 8_565 ? O54 O51 1.44(3) 8_565 ? O54 O52 1.66(3) 8_565 ? O54 Cl5 1.78(4) 8_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn1 N12 111.7(4) . 3 ? O1 Zn1 N21 114.1(3) . . ? N12 Zn1 N21 110.2(4) 3 . ? O1 Zn1 N11 109.6(4) . . ? N12 Zn1 N11 106.0(3) 3 . ? N21 Zn1 N11 104.8(4) . . ? Zn1 O1 Zn1 135.1(4) . 8_565 ? C105 N11 C101 116.5(9) . . ? C105 N11 Zn1 121.7(8) . . ? C101 N11 Zn1 121.7(8) . . ? C116 N12 C115 116.0(9) . . ? C116 N12 Zn1 122.2(7) . 3_455 ? C115 N12 Zn1 121.8(8) . 3_455 ? N11 C101 C102 122.6(10) . . ? C101 C102 C103 121.3(10) . . ? C104 C103 C102 115.2(10) . . ? C104 C103 C106 121.5(12) . . ? C102 C103 C106 123.3(12) . . ? C103 C104 C105 121.5(11) . . ? N11 C105 C104 122.7(10) . . ? C107 C106 C103 112.9(11) . . ? C108 C107 C106 112.4(15) . . ? C107 C108 C109 121.7(18) . . ? C110 C109 C108 101.9(18) . . ? C111 C110 C109 128(2) . . ? C110 C111 C112 127(2) . . ? C111 C112 C113 109.6(13) . . ? C114 C113 C117 116.8(10) . . ? C114 C113 C112 122.0(11) . . ? C117 C113 C112 121.3(11) . . ? C113 C114 C115 120.0(10) . . ? N12 C115 C114 123.7(10) . . ? N12 C116 C117 122.5(10) . . ? C113 C117 C116 121.0(11) . . ? C205 N21 C201 116.4(8) . . ? C205 N21 Zn1 119.0(9) . . ? C201 N21 Zn1 124.5(9) . . ? C216 N22 C215 114.1(12) . . ? N21 C201 C202 123.3(10) . . ? C201 C202 C203 120.3(10) . . ? C204 C203 C202 116.0(9) . . ? C204 C203 C206 124.6(12) . . ? C202 C203 C206 119.4(12) . . ? C205 C204 C203 121.9(10) . . ? N21 C205 C204 122.0(9) . . ? C207 C206 C203 118.9(11) . . ? C208 C207 C206 122.3(9) . . ? C207 C208 C209 123.1(9) . . ? C210 C209 C208 121.6(9) . . ? C209 C210 C211 121.8(9) . . ? C212 C211 C210 122.3(9) . . ? C211 C212 C213 118.7(14) . . ? C217 C213 C214 112.8(14) . . ? C217 C213 C212 128.3(17) . . ? C214 C213 C212 118.9(16) . . ? C215 C214 C213 123.0(14) . . ? N22 C215 C214 123.2(13) . . ? N22 C216 C217 123.8(13) . . ? C213 C217 C216 122.3(13) . . ? O2 Zn2 N41 113.5(4) . . ? O2 Zn2 N32 115.4(4) . 3_554 ? N41 Zn2 N32 109.8(4) . 3_554 ? O2 Zn2 N31 107.7(4) . . ? N41 Zn2 N31 103.3(4) . . ? N32 Zn2 N31 106.2(3) 3_554 . ? Zn2 O2 Zn2 131.7(6) . 8_565 ? C301 N31 C305 116.1(10) . . ? C301 N31 Zn2 119.7(8) . . ? C305 N31 Zn2 124.1(9) . . ? C315 N32 C316 115.4(9) . . ? C315 N32 Zn2 125.1(8) . 3_454 ? C316 N32 Zn2 119.5(8) . 3_454 ? N31 C301 C302 123.9(10) . . ? C303 C302 C301 118.9(10) . . ? C304 C303 C302 118.0(11) . . ? C304 C303 C306 118.9(12) . . ? C302 C303 C306 123.0(12) . . ? C305 C304 C303 119.6(11) . . ? N31 C305 C304 123.4(11) . . ? C307 C306 C303 114.7(13) . . ? C308 C307 C306 110.0(18) . . ? C309 C308 C307 143(2) . . ? C308 C309 C310 135(2) . . ? C311 C310 C309 114.8(19) . . ? C310 C311 C312 107.3(18) . . ? C311 C312 C313 113.9(15) . . ? C317 C313 C314 116.4(11) . . ? C317 C313 C312 118.7(12) . . ? C314 C313 C312 124.9(12) . . ? C313 C314 C315 120.9(11) . . ? N32 C315 C314 123.3(10) . . ? N32 C316 C317 124.0(10) . . ? C313 C317 C316 119.9(11) . . ? C405 N41 C401 113.3(9) . . ? C405 N41 Zn2 123.0(10) . . ? C401 N41 Zn2 123.6(10) . . ? C415 N42 C416 115.1(12) . . ? N41 C401 C402 124.1(10) . . ? C401 C402 C403 121.2(10) . . ? C404 C403 C402 115.7(10) . . ? C404 C403 C406 121.6(13) . . ? C402 C403 C406 122.7(13) . . ? C405 C404 C403 119.3(10) . . ? N41 C405 C404 126.3(10) . . ? C407 C406 C403 112.2(10) . . ? C408 C407 C406 125.9(15) . . ? C407 C408 C409 107.9(18) . . ? C410 C409 C408 99.2(19) . . ? C409 C410 C411 122(3) . . ? C412 C411 C410 121(2) . . ? C411 C412 C413 118.5(17) . . ? C414 C413 C417 116.1(13) . . ? C414 C413 C412 115.5(17) . . ? C417 C413 C412 127.8(17) . . ? C413 C414 C415 120.1(14) . . ? N42 C415 C414 122.9(14) . . ? N42 C416 C417 124.1(13) . . ? C416 C417 C413 119.3(13) . . ? O12 Cl1 O11 112.8 . . ? O12 Cl1 O14 111.8 . . ? O11 Cl1 O14 108.3 . . ? O12 Cl1 O13 108.6 . . ? O11 Cl1 O13 109.6 . . ? O14 Cl1 O13 105.4 . . ? Cl2 Cl2 O24 101.5(15) 8_565 8_565 ? Cl2 Cl2 O22 88.3(17) 8_565 8_565 ? O24 Cl2 O22 127.3(6) 8_565 8_565 ? Cl2 Cl2 O22 73.3(6) 8_565 . ? O24 Cl2 O22 129.2(4) 8_565 . ? O22 Cl2 O22 15(2) 8_565 . ? Cl2 Cl2 O21 81.1(6) 8_565 . ? O24 Cl2 O21 116.79(12) 8_565 . ? O22 Cl2 O21 115.9(4) 8_565 . ? O22 Cl2 O21 112.2 . . ? Cl2 Cl2 O24 60.8(6) 8_565 . ? O24 Cl2 O24 40.8(16) 8_565 . ? O22 Cl2 O24 121.3(12) 8_565 . ? O22 Cl2 O24 111.8 . . ? O21 Cl2 O24 107.3 . . ? Cl2 Cl2 O23 164.6(6) 8_565 . ? O24 Cl2 O23 65.0(16) 8_565 . ? O22 Cl2 O23 94(2) 8_565 . ? O22 Cl2 O23 108.6 . . ? O21 Cl2 O23 111.2 . . ? O24 Cl2 O23 105.4 . . ? Cl2 Cl2 O23 11.8(6) 8_565 8_565 ? O24 Cl2 O23 91.1(14) 8_565 8_565 ? O22 Cl2 O23 90(2) 8_565 8_565 ? O22 Cl2 O23 75.7 . 8_565 ? O21 Cl2 O23 90.64(17) . 8_565 ? O24 Cl2 O23 50.52(18) . 8_565 ? O23 Cl2 O23 152.8(2) . 8_565 ? Cl2 O21 Cl2 17.9(14) . 8_565 ? O22 O22 Cl2 91.7(15) 8_565 8_565 ? O22 O22 Cl2 73.3 8_565 . ? Cl2 O22 Cl2 18.3(15) 8_565 . ? Cl2 O23 O24 52.0(9) . 8_565 ? Cl2 O23 Cl2 3.6(3) . 8_565 ? O24 O23 Cl2 48.9(10) 8_565 8_565 ? O24 O24 Cl2 78.5(16) 8_565 8_565 ? O24 O24 Cl2 60.8 8_565 . ? Cl2 O24 Cl2 17.7(16) 8_565 . ? O24 O24 O23 140.7(8) 8_565 8_565 ? Cl2 O24 O23 63.0(8) 8_565 8_565 ? Cl2 O24 O23 80.6(8) . 8_565 ? Cl3 Cl3 O33 95.3(13) 8_565 8_565 ? Cl3 Cl3 O32 88.4(14) 8_565 8_565 ? O33 Cl3 O32 128.5(2) 8_565 8_565 ? Cl3 Cl3 O32 67.2(6) 8_565 . ? O33 Cl3 O32 127.4(6) 8_565 . ? O32 Cl3 O32 21.2(18) 8_565 . ? Cl3 Cl3 O31 169.2(6) 8_565 . ? O33 Cl3 O31 76.1(15) 8_565 . ? O32 Cl3 O31 92.0(17) 8_565 . ? O32 Cl3 O31 112.8 . . ? Cl3 Cl3 O34 78.3(6) 8_565 . ? O33 Cl3 O34 113.6(3) 8_565 . ? O32 Cl3 O34 117.4(4) 8_565 . ? O32 Cl3 O34 110.5 . . ? O31 Cl3 O34 110.9 . . ? Cl3 Cl3 O33 61.0(5) 8_565 . ? O33 Cl3 O33 34.3(15) 8_565 . ? O32 Cl3 O33 122.1(11) 8_565 . ? O32 Cl3 O33 108.3 . . ? O31 Cl3 O33 110.1 . . ? O34 Cl3 O33 103.8 . . ? Cl3 Cl3 O31 7.7(6) 8_565 8_565 ? O33 Cl3 O31 89.1(14) 8_565 8_565 ? O32 Cl3 O31 88.7(18) 8_565 8_565 ? O32 Cl3 O31 67.7 . 8_565 ? O31 Cl3 O31 161.55(11) . 8_565 ? O34 Cl3 O31 84.95(9) . 8_565 ? O33 Cl3 O31 54.95(8) . 8_565 ? Cl3 O31 O33 47.7(7) . 8_565 ? Cl3 O31 Cl3 3.1(2) . 8_565 ? O33 O31 Cl3 45.2(7) 8_565 8_565 ? O32 O32 Cl3 91.6(12) 8_565 8_565 ? O32 O32 Cl3 67.2 8_565 . ? Cl3 O32 Cl3 24.4(12) 8_565 . ? O33 O33 Cl3 84.7(12) 8_565 8_565 ? O33 O33 Cl3 61.0 8_565 . ? Cl3 O33 Cl3 23.7(12) 8_565 . ? O33 O33 O31 140.5(6) 8_565 8_565 ? Cl3 O33 O31 56.2(7) 8_565 8_565 ? Cl3 O33 O31 79.8(6) . 8_565 ? Cl3 O34 Cl3 23.3(11) 8_565 . ? O42 Cl4 O42 26.1(16) 8_565 . ? O42 Cl4 O43 111.7(9) 8_565 8_565 ? O42 Cl4 O43 126.05(9) . 8_565 ? O42 Cl4 O43 126.0(7) 8_565 . ? O42 Cl4 O43 111.7 . . ? O43 Cl4 O43 58.0(11) 8_565 . ? O42 Cl4 O41 117.82(7) 8_565 . ? O42 Cl4 O41 113.8 . . ? O43 Cl4 O41 119.24(14) 8_565 . ? O43 Cl4 O41 110.6 . . ? O42 Cl4 O41 113.8(4) 8_565 8_565 ? O42 Cl4 O41 117.8(3) . 8_565 ? O43 Cl4 O41 110.6(9) 8_565 8_565 ? O43 Cl4 O41 119.2(9) . 8_565 ? O41 Cl4 O41 16.3(18) . 8_565 ? O42 Cl4 O44 83.6(15) 8_565 . ? O42 Cl4 O44 108.9 . . ? O43 Cl4 O44 45.7(11) 8_565 . ? O43 Cl4 O44 103.6 . . ? O41 Cl4 O44 107.8 . . ? O41 Cl4 O44 91.9(18) 8_565 . ? O42 Cl4 O44 108.9(15) 8_565 8_565 ? O42 Cl4 O44 83.6 . 8_565 ? O43 Cl4 O44 103.6(10) 8_565 8_565 ? O43 Cl4 O44 45.68(11) . 8_565 ? O41 Cl4 O44 91.92(7) . 8_565 ? O41 Cl4 O44 107.8(18) 8_565 8_565 ? O44 Cl4 O44 148.69(11) . 8_565 ? O41 O41 Cl4 81.9 8_565 . ? O42 O42 Cl4 76.9 8_565 . ? O44 O43 O43 132.4(4) 8_565 8_565 ? O44 O43 Cl4 71.5(4) 8_565 . ? O43 O43 Cl4 61.0 8_565 . ? O43 O44 Cl4 62.8(11) 8_565 . ? Cl5 Cl5 O51 106.4(19) 8_565 8_565 ? Cl5 Cl5 O52 102(2) 8_565 8_565 ? O51 Cl5 O52 145(3) 8_565 8_565 ? Cl5 Cl5 O52 60.0(8) 8_565 . ? O51 Cl5 O52 156.3(15) 8_565 . ? O52 Cl5 O52 42(2) 8_565 . ? Cl5 Cl5 O51 55.9(8) 8_565 . ? O51 Cl5 O51 50(2) 8_565 . ? O52 Cl5 O51 150(2) 8_565 . ? O52 Cl5 O51 112.8 . . ? Cl5 Cl5 O54 144.4(10) 8_565 . ? O51 Cl5 O54 66.7(19) 8_565 . ? O52 Cl5 O54 78(2) 8_565 . ? O52 Cl5 O54 111.8 . . ? O51 Cl5 O54 108.3 . . ? Cl5 Cl5 O53 109.9(10) 8_565 . ? O51 Cl5 O53 94.1(9) 8_565 . ? O52 Cl5 O53 95.7(9) 8_565 . ? O52 Cl5 O53 108.6 . . ? O51 Cl5 O53 109.6 . . ? O54 Cl5 O53 105.4 . . ? Cl5 Cl5 O53 55.2(11) 8_565 8_565 ? O51 Cl5 O53 107.9(12) 8_565 8_565 ? O52 Cl5 O53 105.3(13) 8_565 8_565 ? O52 Cl5 O53 81.0(8) . 8_565 ? O51 Cl5 O53 78.8(9) . 8_565 ? O54 Cl5 O53 159.9(16) . 8_565 ? O53 Cl5 O53 54.8(16) . 8_565 ? Cl5 Cl5 O54 27.2(7) 8_565 8_565 ? O51 Cl5 O54 96.9(19) 8_565 8_565 ? O52 Cl5 O54 99(2) 8_565 8_565 ? O52 Cl5 O54 61.79(16) . 8_565 ? O51 Cl5 O54 52.4 . 8_565 ? O54 Cl5 O54 117.2(8) . 8_565 ? O53 Cl5 O54 136.9(8) . 8_565 ? O53 Cl5 O54 82.3(18) 8_565 8_565 ? O51 O51 Cl5 73.6(18) 8_565 8_565 ? O51 O51 Cl5 55.9 8_565 . ? Cl5 O51 Cl5 17.7(18) 8_565 . ? O51 O51 O54 123.7(18) 8_565 8_565 ? Cl5 O51 O54 63.1(9) 8_565 8_565 ? Cl5 O51 O54 77.6(15) . 8_565 ? O52 O52 Cl5 78.2(18) 8_565 8_565 ? O52 O52 Cl5 60.0 8_565 . ? Cl5 O52 Cl5 18.3(18) 8_565 . ? O52 O52 O54 122.5(16) 8_565 8_565 ? Cl5 O52 O54 55.8(9) 8_565 8_565 ? Cl5 O52 O54 71.0(13) . 8_565 ? O53 O53 Cl5 70.1 8_565 . ? O53 O53 Cl5 55.2(12) 8_565 8_565 ? Cl5 O53 Cl5 14.9(12) . 8_565 ? Cl5 O54 O51 50.1(12) . 8_565 ? Cl5 O54 O52 46.1(11) . 8_565 ? O51 O54 O52 96.2(19) 8_565 8_565 ? Cl5 O54 Cl5 8.3(6) . 8_565 ? O51 O54 Cl5 50.0(13) 8_565 8_565 ? O52 O54 Cl5 47.2(11) 8_565 8_565 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 23.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.934 _refine_diff_density_min -0.629 _refine_diff_density_rms 0.108