Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 0222 _journal_name_full 'Dalton Trans.' loop_ _publ_author_name 'Andrea Bencini' 'Carla Bazzicalupu' 'Emanuela Berni' 'Claudia Giorgi' 'Sauro Maoggi' 'Barbara Valtancoli' _publ_contact_author_name 'Prof. Andrea Bencini' _publ_contact_author_address ; Department of Chemistry Università di Firenze Via della Lastruccia 3 Sesto Fiorentino-Firenze 50019 ITALY ; _publ_contact_author_email andrea.bencini@unifi.it _publ_section_title ; Zn(II) coordination to tren-based tris-macrocyles. Activity of their trinuclear Zn(II) complexes in carboxy- and phosphate ester htdrolysis. ; data_[Zn3LCl3](ClO4)3(H2O) _database_code_CSD 212434 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C30N13H69Zn3Cl3 3+), (ClO4 -1)3, (H2 O)' _chemical_formula_sum 'C30 H71 Cl6 N13 O13 Zn3' _chemical_formula_weight 1230.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.9390(10) _cell_length_b 29.5390(10) _cell_length_c 22.459(4) _cell_angle_alpha 90.000 _cell_angle_beta 99.000(5) _cell_angle_gamma 90.000 _cell_volume 5202.0(11) _cell_formula_units_Z 4 _cell_measurement_temperature 298 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 15 _cell_measurement_theta_max 30 _exptl_crystal_description prismatic _exptl_crystal_colour colorrless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.572 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2552 _exptl_absorpt_coefficient_mu 5.018 _exptl_absorpt_correction_type PSI-Scan _exptl_absorpt_correction_T_min 0.28 _exptl_absorpt_correction_T_max 0.60 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298 _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER P4' _diffrn_measurement_method \q/2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0 _diffrn_reflns_number 7063 _diffrn_reflns_av_R_equivalents 0.0458 _diffrn_reflns_av_sigmaI/netI 0.0549 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.49 _diffrn_reflns_theta_max 50.06 _reflns_number_total 5256 _reflns_number_gt 4052 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER, XSCANS' _computing_cell_refinement 'BRUKER, XSCANS' _computing_data_reduction 'BRUKER, XSCANS' _computing_structure_solution 'SIR97 (Altomare, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP_3 (Ver.1.01/b) (Farrugia, 1997)' _computing_publication_material 'PARST97 (Nardelli, 1997)' _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^)+(0.1469P)^2^+33.1004P] 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 0.00011(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5256 _refine_ls_number_parameters 561 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1170 _refine_ls_R_factor_gt 0.0909 _refine_ls_wR_factor_ref 0.2764 _refine_ls_wR_factor_gt 0.2379 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.089 _refine_ls_shift/su_max 0.008 _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 0.55932(17) 0.09391(5) 0.51808(6) 0.0533(5) Uani 1 1 d . . . Zn2 Zn 0.3287(2) 0.15649(6) 0.27240(7) 0.0658(6) Uani 1 1 d . . . Zn3 Zn -0.1289(2) 0.37423(6) 0.35047(8) 0.0693(6) Uani 1 1 d . . . Cl1 Cl 0.3299(4) 0.06550(11) 0.46109(15) 0.0694(9) Uani 1 1 d . . . Cl2 Cl 0.5554(4) 0.18179(12) 0.33482(15) 0.0743(10) Uani 1 1 d . . . Cl3 Cl 0.0953(5) 0.35026(16) 0.3122(2) 0.1056(14) Uani 1 1 d . . . Cl4 Cl 0.5566(4) 0.29158(16) 0.15467(17) 0.0897(12) Uani 1 1 d . . . O41 O 0.424(2) 0.2854(5) 0.1884(7) 0.160(6) Uani 1 1 d . . . O42 O 0.7105(18) 0.2818(7) 0.1893(9) 0.205(8) Uani 1 1 d . . . O43 O 0.5592(17) 0.3397(5) 0.1408(7) 0.139(5) Uani 1 1 d . . . O44 O 0.522(3) 0.2684(6) 0.1006(7) 0.185(7) Uani 1 1 d . . . Cl5 Cl 0.8215(5) 0.51183(14) 0.1703(2) 0.0945(12) Uani 1 1 d . . . O51 O 0.8795(17) 0.5539(4) 0.1536(6) 0.133(5) Uani 1 1 d . . . O52 O 0.763(3) 0.4874(7) 0.1182(10) 0.246(12) Uani 1 1 d . . . O53 O 0.701(3) 0.5171(7) 0.2038(13) 0.293(17) Uani 1 1 d . . . O54 O 0.9570(15) 0.4856(4) 0.2040(6) 0.126(4) Uani 1 1 d . . . N1 N 0.1411(12) 0.2387(3) 0.4484(4) 0.063(3) Uani 1 1 d . . . N2 N 0.5131(11) 0.1689(3) 0.5290(4) 0.056(2) Uani 1 1 d . . . N3 N 0.5339(12) 0.0943(3) 0.6102(4) 0.065(3) Uani 1 1 d . . . H3 H 0.4566 0.0726 0.6158 0.078 Uiso 1 1 calc R . . N4 N 0.7578(12) 0.0464(3) 0.5494(5) 0.066(3) Uani 1 1 d . . . H4 H 0.7347 0.0196 0.5298 0.079 Uiso 1 1 calc R . . N5 N 0.7467(11) 0.1199(4) 0.4703(4) 0.064(3) Uani 1 1 d . . . H5 H 0.7008 0.1245 0.4311 0.077 Uiso 1 1 calc R . . N6 N 0.0750(12) 0.1735(4) 0.2979(4) 0.068(3) Uani 1 1 d . . . N7 N 0.2547(16) 0.0909(4) 0.2862(6) 0.087(4) Uani 1 1 d . . . H7 H 0.3366 0.0777 0.3137 0.104 Uiso 1 1 calc R . . N9 N 0.2344(18) 0.1988(4) 0.1992(5) 0.090(4) Uani 1 1 d . . . H9 H 0.2814 0.2267 0.2065 0.108 Uiso 1 1 calc R . . N10 N -0.2009(13) 0.3299(4) 0.4222(5) 0.070(3) Uani 1 1 d . . . N11 N -0.3518(13) 0.3471(4) 0.3025(5) 0.080(3) Uani 1 1 d . . . H11 H -0.3251 0.3343 0.2683 0.096 Uiso 1 1 calc R . . N12 N -0.2289(16) 0.4350(4) 0.3034(6) 0.095(4) Uani 1 1 d . . . H12 H -0.1493 0.4463 0.2823 0.114 Uiso 1 1 calc R . . N13 N -0.0846(17) 0.4197(4) 0.4238(6) 0.091(4) Uani 1 1 d . . . H13 H 0.0261 0.4168 0.4416 0.109 Uiso 1 1 calc R . . C1 C 0.2948(16) 0.2307(4) 0.4930(6) 0.067(3) Uani 1 1 d . . . H1A H 0.2744 0.2407 0.5324 0.081 Uiso 1 1 calc R . . H1B H 0.3889 0.2482 0.4823 0.081 Uiso 1 1 calc R . . C2 C 0.3432(14) 0.1799(4) 0.4960(6) 0.066(3) Uani 1 1 d . . . H2A H 0.2589 0.1637 0.5146 0.079 Uiso 1 1 calc R . . H2B H 0.3362 0.1687 0.4551 0.079 Uiso 1 1 calc R . . C3 C 0.5345(18) 0.1758(5) 0.5937(5) 0.074(4) Uani 1 1 d . . . H3A H 0.4789 0.2038 0.6019 0.089 Uiso 1 1 calc R . . H3B H 0.6551 0.1788 0.6091 0.089 Uiso 1 1 calc R . . C4 C -0.172(2) 0.3570(6) 0.4790(7) 0.100(5) Uani 1 1 d . . . H4A H -0.0575 0.3512 0.5001 0.119 Uiso 1 1 calc R . . H4B H -0.2520 0.3476 0.5050 0.119 Uiso 1 1 calc R . . C5 C 0.6966(15) 0.0811(5) 0.6443(6) 0.075(4) Uani 1 1 d . . . H5A H 0.6841 0.0749 0.6857 0.089 Uiso 1 1 calc R . . H5B H 0.7785 0.1055 0.6441 0.089 Uiso 1 1 calc R . . C6 C 0.7586(17) 0.0393(5) 0.6156(7) 0.081(4) Uani 1 1 d . . . H6A H 0.8733 0.0321 0.6350 0.098 Uiso 1 1 calc R . . H6B H 0.6855 0.0139 0.6215 0.098 Uiso 1 1 calc R . . C7 C 0.9186(16) 0.0645(5) 0.5350(6) 0.076(4) Uani 1 1 d . . . H7A H 1.0016 0.0404 0.5356 0.091 Uiso 1 1 calc R . . H7B H 0.9641 0.0869 0.5648 0.091 Uiso 1 1 calc R . . C8 C 0.8863(16) 0.0855(6) 0.4744(7) 0.085(4) Uani 1 1 d . . . H8A H 0.8548 0.0622 0.4443 0.102 Uiso 1 1 calc R . . H8B H 0.9898 0.0999 0.4660 0.102 Uiso 1 1 calc R . . C9 C 0.7999(16) 0.1631(5) 0.4988(6) 0.068(3) Uani 1 1 d . . . H9A H 0.8771 0.1784 0.4760 0.082 Uiso 1 1 calc R . . H9B H 0.8594 0.1579 0.5393 0.082 Uiso 1 1 calc R . . C10 C 0.6481(15) 0.1914(5) 0.5009(6) 0.074(4) Uani 1 1 d . . . H10A H 0.6006 0.2002 0.4601 0.089 Uiso 1 1 calc R . . H10B H 0.6830 0.2188 0.5232 0.089 Uiso 1 1 calc R . . C11 C 0.1642(16) 0.2298(4) 0.3857(5) 0.065(3) Uani 1 1 d . . . H11A H 0.2842 0.2250 0.3839 0.078 Uiso 1 1 calc R . . H11B H 0.1263 0.2558 0.3608 0.078 Uiso 1 1 calc R . . C12 C 0.0617(15) 0.1877(4) 0.3609(5) 0.067(3) Uani 1 1 d . . . H12A H 0.0979 0.1624 0.3875 0.080 Uiso 1 1 calc R . . H12B H -0.0576 0.1932 0.3631 0.080 Uiso 1 1 calc R . . C13 C -0.0142(16) 0.1287(5) 0.2866(6) 0.074(4) Uani 1 1 d . . . H13A H -0.1146 0.1282 0.3063 0.088 Uiso 1 1 calc R . . H13B H -0.0510 0.1247 0.2437 0.088 Uiso 1 1 calc R . . C14 C 0.101(2) 0.0907(5) 0.3100(7) 0.089(5) Uani 1 1 d . . . H14A H 0.1264 0.0928 0.3536 0.107 Uiso 1 1 calc R . . H14B H 0.0426 0.0622 0.3000 0.107 Uiso 1 1 calc R . . C15 C 0.243(2) 0.0653(6) 0.2284(9) 0.116(6) Uani 1 1 d . . . H15A H 0.2425 0.0330 0.2358 0.173 Uiso 1 1 calc R . . H15B H 0.1397 0.0733 0.2015 0.173 Uiso 1 1 calc R . . C16 C 0.397(3) 0.0783(9) 0.2016(9) 0.141(8) Uani 1 1 d . . . H16A H 0.4933 0.0624 0.2238 0.211 Uiso 1 1 calc R . . H16B H 0.3807 0.0666 0.1607 0.211 Uiso 1 1 calc R . . C18 C 0.280(3) 0.1819(8) 0.1415(9) 0.126(6) Uiso 1 1 d . . . C19 C 0.050(2) 0.2032(6) 0.1936(7) 0.105(6) Uani 1 1 d . . . H19A H -0.0045 0.1765 0.1744 0.126 Uiso 1 1 calc R . . H19B H 0.0122 0.2293 0.1689 0.126 Uiso 1 1 calc R . . C20 C 0.002(2) 0.2089(6) 0.2561(6) 0.102(5) Uani 1 1 d . . . H20A H 0.0422 0.2382 0.2720 0.123 Uiso 1 1 calc R . . H20B H -0.1207 0.2084 0.2529 0.123 Uiso 1 1 calc R . . C21 C 0.0717(15) 0.2844(4) 0.4560(6) 0.064(3) Uani 1 1 d . . . H21A H 0.1301 0.3065 0.4347 0.077 Uiso 1 1 calc R . . H21B H 0.0889 0.2925 0.4984 0.077 Uiso 1 1 calc R . . C22 C -0.1155(16) 0.2843(4) 0.4314(6) 0.068(3) Uani 1 1 d . . . H22A H -0.1739 0.2668 0.4585 0.082 Uiso 1 1 calc R . . H22B H -0.1314 0.2686 0.3929 0.082 Uiso 1 1 calc R . . C23 C -0.3846(17) 0.3228(5) 0.4030(8) 0.094(5) Uani 1 1 d . . . H23A H -0.4456 0.3502 0.4103 0.113 Uiso 1 1 calc R . . H23B H -0.4236 0.2987 0.4269 0.113 Uiso 1 1 calc R . . C24 C -0.4241(19) 0.3107(5) 0.3376(8) 0.098(5) Uani 1 1 d . . . H24A H -0.5465 0.3085 0.3251 0.117 Uiso 1 1 calc R . . H24B H -0.3735 0.2816 0.3304 0.117 Uiso 1 1 calc R . . C25 C -0.4715(19) 0.3847(6) 0.2845(9) 0.109(6) Uani 1 1 d . . . H25A H -0.5634 0.3744 0.2539 0.130 Uiso 1 1 calc R . . H25B H -0.5206 0.3949 0.3191 0.130 Uiso 1 1 calc R . . C26 C -0.381(2) 0.4220(6) 0.2609(8) 0.104(5) Uani 1 1 d . . . H26A H -0.4570 0.4478 0.2534 0.124 Uiso 1 1 calc R . . H26B H -0.3478 0.4130 0.2229 0.124 Uiso 1 1 calc R . . C27 C -0.259(2) 0.4674(6) 0.3485(9) 0.106(5) Uani 1 1 d . . . H27A H -0.3632 0.4596 0.3637 0.127 Uiso 1 1 calc R . . H27B H -0.2729 0.4973 0.3307 0.127 Uiso 1 1 calc R . . C28 C -0.112(3) 0.4676(6) 0.3997(9) 0.130(7) Uani 1 1 d . . . H28A H -0.1366 0.4877 0.4314 0.156 Uiso 1 1 calc R . . H28B H -0.0096 0.4783 0.3856 0.156 Uiso 1 1 calc R . . C29 C -0.192(2) 0.4068(6) 0.4669(8) 0.106(6) Uani 1 1 d . . . H29A H -0.3103 0.4136 0.4511 0.127 Uiso 1 1 calc R . . H29B H -0.1604 0.4237 0.5040 0.127 Uiso 1 1 calc R . . C30 C 0.4640(19) 0.1386(5) 0.6257(6) 0.079(4) Uani 1 1 d . . . H30A H 0.3408 0.1382 0.6151 0.095 Uiso 1 1 calc R . . H30B H 0.4915 0.1435 0.6689 0.095 Uiso 1 1 calc R . . N8 N 0.443(3) 0.1233(6) 0.1988(9) 0.138(6) Uani 1 1 d . . . C17A C 0.455(7) 0.1552(18) 0.155(2) 0.088(14) Uiso 0.30 1 d P . . C17B C 0.288(4) 0.1429(12) 0.1400(14) 0.133(10) Uiso 0.70 1 d P . . Cl6 Cl -0.1768(15) 0.1020(3) 0.0673(5) 0.244(6) Uani 1 1 d . . . O61 O -0.317(4) 0.0807(10) 0.0461(14) 0.275(12) Uiso 1 1 d . . . O62 O -0.166(5) 0.0930(13) 0.1276(19) 0.339(18) Uiso 1 1 d . . . O63 O -0.154(5) 0.1410(14) 0.0488(17) 0.341(18) Uiso 1 1 d . . . O64 O -0.033(8) 0.0763(19) 0.077(3) 0.47(3) Uiso 1 1 d . . . O100 O 0.140(4) -0.035(2) 0.076(2) 0.57(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0359(9) 0.0635(10) 0.0584(10) -0.0038(7) 0.0009(7) 0.0006(7) Zn2 0.0526(10) 0.0794(12) 0.0642(11) -0.0035(8) 0.0055(8) -0.0052(8) Zn3 0.0527(10) 0.0804(13) 0.0745(12) 0.0131(9) 0.0094(8) 0.0013(8) Cl1 0.0456(17) 0.073(2) 0.084(2) -0.0133(17) -0.0080(15) -0.0011(15) Cl2 0.0470(17) 0.096(2) 0.078(2) -0.0075(18) 0.0038(15) -0.0054(16) Cl3 0.068(2) 0.143(4) 0.113(3) 0.039(3) 0.034(2) 0.016(2) Cl4 0.063(2) 0.122(3) 0.084(3) 0.019(2) 0.0119(19) -0.008(2) O41 0.168(13) 0.162(13) 0.173(13) -0.023(10) 0.094(11) -0.067(11) O42 0.098(10) 0.25(2) 0.25(2) 0.068(16) -0.037(11) 0.057(11) O43 0.118(10) 0.137(11) 0.157(12) 0.041(9) 0.000(8) -0.020(8) O44 0.28(2) 0.155(14) 0.113(11) -0.035(10) 0.019(12) 0.023(14) Cl5 0.064(2) 0.096(3) 0.124(3) 0.007(3) 0.015(2) 0.003(2) O51 0.152(11) 0.113(9) 0.122(9) 0.043(8) -0.019(8) -0.051(8) O52 0.24(2) 0.182(17) 0.26(2) -0.035(17) -0.14(2) 0.005(16) O53 0.219(19) 0.23(2) 0.49(4) 0.20(2) 0.26(3) 0.144(17) O54 0.106(9) 0.139(10) 0.132(10) 0.004(8) 0.015(7) 0.039(8) N1 0.056(6) 0.073(7) 0.060(6) 0.001(5) 0.012(5) 0.008(5) N2 0.049(6) 0.062(6) 0.054(6) -0.001(5) -0.003(5) 0.003(5) N3 0.051(6) 0.076(7) 0.070(7) 0.002(6) 0.013(5) -0.009(5) N4 0.057(6) 0.060(6) 0.077(7) -0.016(5) -0.003(5) 0.004(5) N5 0.042(6) 0.101(8) 0.048(6) -0.008(6) 0.003(4) 0.005(6) N6 0.057(6) 0.087(8) 0.053(6) -0.001(6) -0.010(5) -0.009(6) N7 0.076(8) 0.068(8) 0.107(10) 0.005(7) -0.016(7) 0.004(6) N9 0.120(11) 0.096(9) 0.060(7) 0.004(6) 0.030(7) -0.032(8) N10 0.056(7) 0.078(7) 0.078(7) 0.009(6) 0.020(5) 0.011(6) N11 0.054(6) 0.083(8) 0.097(8) 0.009(7) -0.001(6) 0.003(6) N12 0.077(8) 0.094(10) 0.113(10) 0.040(9) 0.015(8) 0.003(7) N13 0.102(9) 0.074(8) 0.090(9) 0.003(7) -0.008(8) 0.020(7) C1 0.059(8) 0.072(9) 0.065(8) 0.001(7) -0.008(6) 0.000(7) C2 0.050(8) 0.067(8) 0.079(9) 0.008(7) 0.005(6) 0.006(6) C3 0.091(10) 0.070(9) 0.063(9) 0.002(7) 0.011(7) 0.025(8) C4 0.111(13) 0.114(13) 0.075(10) 0.013(9) 0.019(9) 0.050(11) C5 0.050(8) 0.098(11) 0.075(9) 0.010(8) 0.007(7) -0.003(7) C6 0.058(8) 0.074(9) 0.103(12) 0.013(8) -0.012(8) 0.019(7) C7 0.057(8) 0.085(10) 0.093(11) -0.001(8) 0.033(7) 0.018(7) C8 0.047(8) 0.128(13) 0.085(10) -0.012(9) 0.022(7) 0.008(8) C9 0.059(8) 0.084(10) 0.061(8) -0.002(7) 0.010(6) -0.008(7) C10 0.050(8) 0.083(10) 0.089(10) -0.002(8) 0.010(7) -0.011(7) C11 0.061(8) 0.076(9) 0.059(8) 0.004(7) 0.012(6) 0.000(7) C12 0.052(7) 0.083(9) 0.064(8) -0.005(7) 0.005(6) 0.006(7) C13 0.046(7) 0.088(10) 0.082(9) -0.003(8) -0.004(6) -0.013(7) C14 0.097(12) 0.074(10) 0.088(10) 0.011(8) -0.013(9) -0.017(9) C15 0.086(11) 0.095(12) 0.161(17) -0.066(12) 0.004(12) -0.013(10) C16 0.14(2) 0.18(2) 0.094(13) 0.000(15) 0.003(13) 0.060(18) C19 0.138(16) 0.103(12) 0.068(10) 0.027(9) -0.002(10) 0.042(11) C20 0.123(14) 0.115(13) 0.064(10) 0.002(9) -0.005(9) 0.032(11) C21 0.063(8) 0.062(8) 0.064(8) 0.006(6) 0.002(6) 0.009(6) C22 0.068(9) 0.062(8) 0.078(9) 0.015(7) 0.021(7) 0.012(7) C23 0.060(9) 0.090(11) 0.139(15) 0.067(11) 0.033(9) 0.018(8) C24 0.065(10) 0.096(12) 0.128(15) 0.041(11) 0.003(9) -0.013(8) C25 0.063(10) 0.098(12) 0.155(16) 0.038(11) -0.017(10) -0.012(9) C26 0.088(11) 0.095(12) 0.115(13) 0.039(10) -0.023(10) 0.018(10) C27 0.109(13) 0.075(11) 0.130(15) 0.012(11) 0.003(12) 0.007(10) C28 0.161(19) 0.080(12) 0.133(16) -0.008(11) -0.026(14) 0.000(12) C29 0.121(14) 0.099(13) 0.092(12) 0.002(10) -0.003(11) 0.045(11) C30 0.096(11) 0.079(10) 0.066(9) -0.007(8) 0.022(8) 0.010(8) N8 0.170(17) 0.104(12) 0.143(15) -0.027(11) 0.036(12) 0.005(12) Cl6 0.241(10) 0.179(7) 0.256(11) 0.056(7) -0.141(8) -0.072(7) O100 0.20(3) 0.96(13) 0.54(7) 0.06(8) 0.06(4) -0.10(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 N3 2.110(10) . ? Zn1 N5 2.110(10) . ? Zn1 N4 2.145(10) . ? Zn1 Cl1 2.220(3) . ? Zn1 N2 2.264(10) . ? Zn2 N7 2.063(11) . ? Zn2 N9 2.107(12) . ? Zn2 Cl2 2.231(3) . ? Zn2 N8 2.234(17) . ? Zn2 N6 2.236(10) . ? Zn3 N11 2.083(11) . ? Zn3 N13 2.111(12) . ? Zn3 N12 2.170(12) . ? Zn3 Cl3 2.211(4) . ? Zn3 N10 2.220(10) . ? Cl4 O42 1.373(13) . ? Cl4 O44 1.383(14) . ? Cl4 O41 1.399(13) . ? Cl4 O43 1.455(14) . ? Cl5 O53 1.314(17) . ? Cl5 O52 1.392(19) . ? Cl5 O51 1.398(11) . ? Cl5 O54 1.440(12) . ? N1 C11 1.472(15) . ? N1 C1 1.472(15) . ? N1 C21 1.478(15) . ? N2 C3 1.452(15) . ? N2 C2 1.471(14) . ? N2 C10 1.484(15) . ? N3 C5 1.448(15) . ? N3 C30 1.484(16) . ? N4 C7 1.466(16) . ? N4 C6 1.501(17) . ? N5 C9 1.458(16) . ? N5 C8 1.496(16) . ? N6 C20 1.462(17) . ? N6 C12 1.494(15) . ? N6 C13 1.506(16) . ? N7 C14 1.406(19) . ? N7 C15 1.492(19) . ? N9 C19 1.453(19) . ? N9 C18 1.49(2) . ? N10 C23 1.469(17) . ? N10 C4 1.495(18) . ? N10 C22 1.507(15) . ? N11 C25 1.477(18) . ? N11 C24 1.500(17) . ? N12 C27 1.44(2) . ? N12 C26 1.470(19) . ? N13 C29 1.44(2) . ? N13 C28 1.52(2) . ? C1 C2 1.547(17) . ? C3 C30 1.471(18) . ? C4 C29 1.50(2) . ? C5 C6 1.511(19) . ? C7 C8 1.481(19) . ? C9 C10 1.474(17) . ? C11 C12 1.542(17) . ? C13 C14 1.488(19) . ? C15 C16 1.49(3) . ? C16 N8 1.38(3) . ? C18 C17B 1.16(3) . ? C18 C17A 1.58(6) . ? C19 C20 1.52(2) . ? C21 C22 1.503(17) . ? C23 C24 1.50(2) . ? C25 C26 1.46(2) . ? C27 C28 1.50(2) . ? N8 C17A 1.38(5) . ? N8 C17B 1.75(4) . ? C17A C17B 1.36(6) . ? Cl6 O63 1.25(4) . ? Cl6 O61 1.30(3) . ? Cl6 O64 1.36(6) . ? Cl6 O62 1.37(4) . ? O62 O64 1.74(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Zn1 N5 132.8(4) . . ? N3 Zn1 N4 82.0(4) . . ? N5 Zn1 N4 82.2(4) . . ? N3 Zn1 Cl1 111.8(3) . . ? N5 Zn1 Cl1 115.1(3) . . ? N4 Zn1 Cl1 115.8(3) . . ? N3 Zn1 N2 81.2(4) . . ? N5 Zn1 N2 80.7(4) . . ? N4 Zn1 N2 136.7(4) . . ? Cl1 Zn1 N2 107.4(2) . . ? N7 Zn2 N9 126.9(5) . . ? N7 Zn2 Cl2 116.2(3) . . ? N9 Zn2 Cl2 116.4(4) . . ? N7 Zn2 N8 81.8(6) . . ? N9 Zn2 N8 79.6(6) . . ? Cl2 Zn2 N8 103.4(5) . . ? N7 Zn2 N6 83.3(5) . . ? N9 Zn2 N6 80.9(4) . . ? Cl2 Zn2 N6 115.7(3) . . ? N8 Zn2 N6 140.8(6) . . ? N11 Zn3 N13 132.3(5) . . ? N11 Zn3 N12 81.4(5) . . ? N13 Zn3 N12 81.8(5) . . ? N11 Zn3 Cl3 110.2(4) . . ? N13 Zn3 Cl3 117.4(4) . . ? N12 Zn3 Cl3 109.3(4) . . ? N11 Zn3 N10 81.6(4) . . ? N13 Zn3 N10 80.8(5) . . ? N12 Zn3 N10 136.6(4) . . ? Cl3 Zn3 N10 114.0(3) . . ? O42 Cl4 O44 115.4(13) . . ? O42 Cl4 O41 110.0(11) . . ? O44 Cl4 O41 110.4(11) . . ? O42 Cl4 O43 106.6(10) . . ? O44 Cl4 O43 107.7(10) . . ? O41 Cl4 O43 106.2(9) . . ? O53 Cl5 O52 111.3(17) . . ? O53 Cl5 O51 110.4(12) . . ? O52 Cl5 O51 108.4(12) . . ? O53 Cl5 O54 108.2(11) . . ? O52 Cl5 O54 106.8(10) . . ? O51 Cl5 O54 111.7(8) . . ? C11 N1 C1 114.1(10) . . ? C11 N1 C21 112.3(9) . . ? C1 N1 C21 110.6(9) . . ? C3 N2 C2 115.3(10) . . ? C3 N2 C10 112.6(10) . . ? C2 N2 C10 110.7(9) . . ? C3 N2 Zn1 104.5(7) . . ? C2 N2 Zn1 108.3(7) . . ? C10 N2 Zn1 104.6(7) . . ? C5 N3 C30 116.6(11) . . ? C5 N3 Zn1 107.6(7) . . ? C30 N3 Zn1 109.4(8) . . ? C7 N4 C6 113.6(10) . . ? C7 N4 Zn1 108.0(8) . . ? C6 N4 Zn1 107.8(7) . . ? C9 N5 C8 113.9(10) . . ? C9 N5 Zn1 105.9(7) . . ? C8 N5 Zn1 107.2(8) . . ? C20 N6 C12 109.3(11) . . ? C20 N6 C13 113.2(11) . . ? C12 N6 C13 107.7(10) . . ? C20 N6 Zn2 106.0(9) . . ? C12 N6 Zn2 120.4(7) . . ? C13 N6 Zn2 100.2(8) . . ? C14 N7 C15 112.9(12) . . ? C14 N7 Zn2 110.2(9) . . ? C15 N7 Zn2 108.9(10) . . ? C19 N9 C18 109.6(13) . . ? C19 N9 Zn2 110.5(8) . . ? C18 N9 Zn2 112.1(12) . . ? C23 N10 C4 109.9(12) . . ? C23 N10 C22 108.5(11) . . ? C4 N10 C22 110.9(10) . . ? C23 N10 Zn3 103.2(8) . . ? C4 N10 Zn3 106.2(9) . . ? C22 N10 Zn3 117.7(7) . . ? C25 N11 C24 113.6(11) . . ? C25 N11 Zn3 108.0(9) . . ? C24 N11 Zn3 111.6(9) . . ? C27 N12 C26 114.9(14) . . ? C27 N12 Zn3 107.1(10) . . ? C26 N12 Zn3 107.5(9) . . ? C29 N13 C28 114.8(14) . . ? C29 N13 Zn3 108.3(10) . . ? C28 N13 Zn3 108.4(10) . . ? N1 C1 C2 111.1(10) . . ? N2 C2 C1 116.0(10) . . ? N2 C3 C30 113.0(12) . . ? N10 C4 C29 111.9(12) . . ? N3 C5 C6 108.5(11) . . ? N4 C6 C5 110.9(11) . . ? N4 C7 C8 108.9(11) . . ? C7 C8 N5 111.2(10) . . ? N5 C9 C10 109.1(10) . . ? C9 C10 N2 114.0(11) . . ? N1 C11 C12 110.6(10) . . ? N6 C12 C11 117.1(10) . . ? C14 C13 N6 110.9(10) . . ? N7 C14 C13 112.7(12) . . ? C16 C15 N7 106.2(14) . . ? N8 C16 C15 120.4(18) . . ? C17B C18 N9 112(2) . . ? C17B C18 C17A 57(3) . . ? N9 C18 C17A 109(2) . . ? N9 C19 C20 108.9(13) . . ? N6 C20 C19 112.7(13) . . ? N1 C21 C22 108.7(10) . . ? C21 C22 N10 116.5(11) . . ? N10 C23 C24 111.5(12) . . ? C23 C24 N11 107.8(13) . . ? C26 C25 N11 109.6(13) . . ? C25 C26 N12 111.3(13) . . ? N12 C27 C28 110.2(15) . . ? C27 C28 N13 108.6(14) . . ? N13 C29 C4 108.7(13) . . ? C3 C30 N3 111.0(11) . . ? C17A N8 C16 138(3) . . ? C17A N8 C17B 50(2) . . ? C16 N8 C17B 101.1(19) . . ? C17A N8 Zn2 108(2) . . ? C16 N8 Zn2 104.3(14) . . ? C17B N8 Zn2 95.4(13) . . ? C17B C17A N8 80(3) . . ? C17B C17A C18 45(2) . . ? N8 C17A C18 109(4) . . ? C18 C17B C17A 77(3) . . ? C18 C17B N8 110(3) . . ? C17A C17B N8 51(3) . . ? O63 Cl6 O61 119(2) . . ? O63 Cl6 O64 114(3) . . ? O61 Cl6 O64 116(3) . . ? O63 Cl6 O62 121(3) . . ? O61 Cl6 O62 101(2) . . ? O64 Cl6 O62 80(2) . . ? Cl6 O62 O64 50(2) . . ? Cl6 O64 O62 51(2) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 50.06 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.820 _refine_diff_density_min -0.773 _refine_diff_density_rms 0.126