# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_publication_text _journal_name_full 'Dalton Trans.' #TrackingRef '- BIS725c_new.cif' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Dirk Volkmer' _publ_contact_author_address ;Ulm University Institute of Inorganic Chemistry II Materials and Catalysis Albert-Einstein-Allee 11 D-89081 Ulm Germany and Institute of Physics Chair of Solid State Science Augsburg University Universit\"atsstrasse 1 D-86135 Augsburg Germany ; _publ_contact_author_email dirk.volkmer@physik.uni-augsburg.de _publ_contact_author_phone '(+)49 (0)821 598-3006' _publ_contact_author_fax '(+)49 (0)821 598-5955' loop_ _publ_author_name _publ_author_address S.Biswas ;Ulm University Institute of Inorganic Chemistry II Materials and Catalysis Albert-Einstein-Allee 11 D-89081 Ulm Germany ; M.Tonigold ;Ulm University Institute of Inorganic Chemistry II Materials and Catalysis Albert-Einstein-Allee 11 D-89081 Ulm Germany ; H.Kelm ;Technische Universit\"at Kaiserslautern Fachbereich Chemie Erwin-Schr\"odinger Strasse D-67663 Kaiserslautern Germany ; H.-J.Kruger ;Technische Universit\"at Kaiserslautern Fachbereich Chemie Erwin-Schr\"odinger Strasse D-67663 Kaiserslautern Germany ; D.Volkmer ;Ulm University Institute of Inorganic Chemistry II Materials and Catalysis Albert-Einstein-Allee 11 D-89081 Ulm Germany and Institute of Physics Chair of Solid State Science Augsburg University Universit\"atsstrasse 1 D-86135 Augsburg Germany ; data_bis725c _database_code_depnum_ccdc_archive 'CCDC 778555' #TrackingRef '- BIS725c_new.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C96 H96 Cl6 N36 O24 Zn9' _chemical_formula_sum 'C96 H96 Cl6 N36 O24 Zn9' _chemical_melting_point ? _exptl_crystal_description needle _exptl_crystal_colour colourless _diffrn_ambient_temperature 223(2) _chemical_formula_weight 2939.12 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 'P 21/n' _symmetry_int_tables_number 14 _chemical_absolute_configuration unk 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 21.848(4) _cell_length_b 15.490(3) _cell_length_c 22.499(5) _cell_angle_alpha 90.00 _cell_angle_beta 99.02(3) _cell_angle_gamma 90.00 _cell_volume 7520(3) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 14496 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 25.93 _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.19 _exptl_crystal_density_diffrn 1.298 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2976 _exptl_absorpt_coefficient_mu 1.581 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.5229 _exptl_absorpt_correction_T_max 0.5455 _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source_type 'STOE IPDS' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 58162 _diffrn_reflns_av_R_equivalents 0.0691 _diffrn_reflns_av_sigmaI/netI 0.0757 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 25.93 _reflns_number_total 14496 _reflns_number_gt 8398 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1358P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14496 _refine_ls_number_parameters 784 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1096 _refine_ls_R_factor_gt 0.0645 _refine_ls_wR_factor_ref 0.2319 _refine_ls_wR_factor_gt 0.2104 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.0000 0.0000 0.0000 0.0321(3) Uani 1 2 d S . . Zn2 Zn -0.13256(3) 0.04758(5) 0.08424(3) 0.0336(2) Uani 1 1 d . . . Zn3 Zn -0.07515(4) 0.09591(6) 0.23709(3) 0.0400(2) Uani 1 1 d . . . Zn4 Zn -0.21812(4) 0.22675(6) 0.01726(4) 0.0377(2) Uani 1 1 d . . . Zn5 Zn -0.23183(4) -0.13420(6) 0.08050(4) 0.0436(2) Uani 1 1 d . . . Cl1 Cl -0.27010(10) 0.33762(15) -0.02198(9) 0.0583(6) Uani 1 1 d . . . Cl2 Cl -0.29533(10) -0.24243(15) 0.07635(12) 0.0677(6) Uani 1 1 d . . . Cl3 Cl -0.04168(13) 0.12095(18) 0.33070(9) 0.0770(7) Uani 1 1 d . . . N1 N -0.1763(3) 0.2359(4) 0.1030(3) 0.0388(14) Uani 1 1 d . . . N2 N -0.1449(2) 0.1685(4) 0.1298(2) 0.0361(13) Uani 1 1 d . . . N3 N -0.1230(3) 0.1882(4) 0.1869(2) 0.0377(13) Uani 1 1 d . . . N4 N -0.2618(3) 0.1125(4) 0.0187(3) 0.0404(14) Uani 1 1 d . . . N5 N -0.2317(3) 0.0461(4) 0.0469(3) 0.0391(14) Uani 1 1 d . . . N6 N -0.2679(3) -0.0235(4) 0.0434(3) 0.0392(14) Uani 1 1 d . . . N7 N -0.1889(3) -0.0969(4) 0.1614(3) 0.0423(14) Uani 1 1 d . . . N8 N -0.1569(3) -0.0234(4) 0.1636(3) 0.0392(14) Uani 1 1 d . . . N9 N -0.1303(3) -0.0075(4) 0.2203(3) 0.0398(14) Uani 1 1 d . . . N10 N -0.0148(3) 0.0665(4) 0.1817(2) 0.0401(14) Uani 1 1 d . . . N11 N -0.0357(2) 0.0485(4) 0.1233(2) 0.0363(13) Uani 1 1 d . . . N12 N 0.0113(2) 0.0325(4) 0.0935(2) 0.0372(13) Uani 1 1 d . . . N13 N -0.1580(3) -0.1416(4) 0.0380(3) 0.0415(14) Uani 1 1 d . . . N14 N -0.1196(2) -0.0734(4) 0.0404(3) 0.0365(13) Uani 1 1 d . . . N15 N -0.0728(2) -0.0899(4) 0.0098(3) 0.0373(13) Uani 1 1 d . . . N16 N -0.1445(2) 0.1876(4) -0.0185(2) 0.0375(13) Uani 1 1 d . . . N17 N -0.1124(2) 0.1197(4) 0.0065(2) 0.0338(12) Uani 1 1 d . . . N18 N -0.0647(3) 0.1029(4) -0.0229(2) 0.0378(13) Uani 1 1 d . . . O1 O -0.2137(4) 0.5143(4) 0.1931(3) 0.078(2) Uani 1 1 d . . . O2 O -0.1532(3) 0.4601(4) 0.2904(3) 0.0642(17) Uani 1 1 d . . . O3 O -0.4721(4) 0.1118(6) -0.0911(6) 0.164(6) Uani 1 1 d . . . O4 O -0.4802(4) -0.0443(6) -0.0614(5) 0.141(4) Uani 1 1 d . . . O5 O -0.1352(4) -0.1892(6) 0.3980(3) 0.102(3) Uani 1 1 d . . . O6 O -0.2010(4) -0.2937(4) 0.3303(3) 0.082(2) Uani 1 1 d . . . O7 O 0.2322(3) 0.0393(8) 0.1770(3) 0.123(4) Uani 1 1 d . . . O8 O 0.2009(3) 0.0756(9) 0.2776(3) 0.152(5) Uani 1 1 d . . . O9 O -0.0436(5) -0.3541(5) -0.1012(5) 0.131(4) Uani 1 1 d . . . O10 O -0.1397(5) -0.4142(5) -0.0676(5) 0.147(5) Uani 1 1 d . . . O11 O -0.1019(3) 0.3544(5) -0.1925(3) 0.095(3) Uani 1 1 d . . . O12 O -0.0145(4) 0.2522(5) -0.2015(4) 0.107(3) Uani 1 1 d . . . C1 C -0.1406(3) 0.2697(5) 0.1968(3) 0.0386(16) Uani 1 1 d . . . C2 C -0.1306(3) 0.3224(5) 0.2498(3) 0.0454(18) Uani 1 1 d . . . H2 H -0.1075 0.3030 0.2862 0.054 Uiso 1 1 calc R . . C3 C -0.1566(4) 0.4023(5) 0.2443(4) 0.0505(19) Uani 1 1 d . . . C4 C -0.1917(4) 0.4326(6) 0.1889(4) 0.054(2) Uani 1 1 d . . . C5 C -0.2000(4) 0.3835(5) 0.1390(3) 0.0493(19) Uani 1 1 d . . . H5 H -0.2221 0.4039 0.1025 0.059 Uiso 1 1 calc R . . C6 C -0.1740(3) 0.3005(5) 0.1439(3) 0.0384(16) Uani 1 1 d . . . C7 C -0.2459(6) 0.5496(7) 0.1382(5) 0.095(4) Uani 1 1 d . . . H7A H -0.2613 0.6066 0.1458 0.143 Uiso 1 1 calc R . . H7B H -0.2804 0.5123 0.1227 0.143 Uiso 1 1 calc R . . H7C H -0.2178 0.5538 0.1090 0.143 Uiso 1 1 calc R . . C8 C -0.1167(5) 0.4371(6) 0.3460(4) 0.065(2) Uani 1 1 d . . . H8A H -0.1165 0.4844 0.3743 0.098 Uiso 1 1 calc R . . H8B H -0.0746 0.4251 0.3396 0.098 Uiso 1 1 calc R . . H8C H -0.1340 0.3861 0.3620 0.098 Uiso 1 1 calc R . . C9 C -0.3186(3) 0.0842(5) -0.0040(3) 0.0472(19) Uani 1 1 d . . . C10 C -0.3686(4) 0.1295(7) -0.0395(5) 0.079(3) Uani 1 1 d . . . H10 H -0.3657 0.1877 -0.0504 0.095 Uiso 1 1 calc R . . C11 C -0.4213(5) 0.0811(7) -0.0564(6) 0.097(4) Uani 1 1 d . . . C12 C -0.4248(4) -0.0080(8) -0.0410(6) 0.095(4) Uani 1 1 d . . . C13 C -0.3772(4) -0.0510(6) -0.0071(5) 0.064(2) Uani 1 1 d . . . H13 H -0.3803 -0.1093 0.0035 0.077 Uiso 1 1 calc R . . C14 C -0.3227(3) -0.0017(5) 0.0111(3) 0.0439(17) Uani 1 1 d . . . C15 C -0.4693(8) 0.1977(11) -0.1119(11) 0.243(15) Uani 1 1 d . . . H15A H -0.5105 0.2226 -0.1179 0.364 Uiso 1 1 calc R . . H15B H -0.4532 0.1979 -0.1497 0.364 Uiso 1 1 calc R . . H15C H -0.4422 0.2314 -0.0824 0.364 Uiso 1 1 calc R . . C16 C -0.4874(6) -0.1319(9) -0.0446(10) 0.168(9) Uani 1 1 d . . . H16A H -0.5273 -0.1533 -0.0640 0.251 Uiso 1 1 calc R . . H16B H -0.4851 -0.1357 -0.0013 0.251 Uiso 1 1 calc R . . H16C H -0.4546 -0.1666 -0.0570 0.251 Uiso 1 1 calc R . . C17 C -0.1455(4) -0.0729(5) 0.2554(3) 0.0455(18) Uani 1 1 d . . . C18 C -0.1275(4) -0.0885(6) 0.3178(4) 0.057(2) Uani 1 1 d . . . H18 H -0.1026 -0.0493 0.3427 0.068 Uiso 1 1 calc R . . C19 C -0.1478(5) -0.1626(7) 0.3395(4) 0.068(3) Uani 1 1 d . . . C20 C -0.1850(5) -0.2212(6) 0.3015(4) 0.064(3) Uani 1 1 d . . . C21 C -0.2030(4) -0.2073(5) 0.2412(4) 0.053(2) Uani 1 1 d . . . H21 H -0.2276 -0.2469 0.2163 0.063 Uiso 1 1 calc R . . C22 C -0.1819(3) -0.1287(5) 0.2191(3) 0.0436(18) Uani 1 1 d . . . C23 C -0.0981(8) -0.1335(12) 0.4380(6) 0.146(7) Uani 1 1 d . . . H23A H -0.0906 -0.1594 0.4777 0.219 Uiso 1 1 calc R . . H23B H -0.1194 -0.0788 0.4400 0.219 Uiso 1 1 calc R . . H23C H -0.0590 -0.1239 0.4239 0.219 Uiso 1 1 calc R . . C24 C -0.2290(5) -0.3600(7) 0.2951(5) 0.077(3) Uani 1 1 d . . . H24A H -0.2356 -0.4087 0.3204 0.116 Uiso 1 1 calc R . . H24B H -0.2026 -0.3774 0.2663 0.116 Uiso 1 1 calc R . . H24C H -0.2686 -0.3404 0.2737 0.116 Uiso 1 1 calc R . . C25 C 0.0483(3) 0.0618(6) 0.1887(3) 0.048(2) Uani 1 1 d . . . C26 C 0.0923(4) 0.0730(8) 0.2406(4) 0.078(3) Uani 1 1 d . . . H26 H 0.0807 0.0845 0.2783 0.094 Uiso 1 1 calc R . . C27 C 0.1520(4) 0.0663(9) 0.2331(4) 0.087(4) Uani 1 1 d . . . C28 C 0.1698(4) 0.0448(9) 0.1762(4) 0.088(4) Uani 1 1 d . . . C29 C 0.1269(3) 0.0312(7) 0.1261(4) 0.061(3) Uani 1 1 d . . . H29 H 0.1383 0.0168 0.0888 0.073 Uiso 1 1 calc R . . C30 C 0.0646(3) 0.0399(5) 0.1338(3) 0.0437(18) Uani 1 1 d . . . C31 C 0.2520(5) 0.0151(15) 0.1197(5) 0.175(10) Uani 1 1 d . . . H31A H 0.2935 -0.0087 0.1275 0.263 Uiso 1 1 calc R . . H31B H 0.2517 0.0659 0.0944 0.263 Uiso 1 1 calc R . . H31C H 0.2237 -0.0277 0.0994 0.263 Uiso 1 1 calc R . . C32 C 0.1849(6) 0.0900(15) 0.3370(5) 0.180(10) Uani 1 1 d . . . H32A H 0.2130 0.0577 0.3665 0.270 Uiso 1 1 calc R . . H32B H 0.1427 0.0708 0.3376 0.270 Uiso 1 1 calc R . . H32C H 0.1882 0.1510 0.3465 0.270 Uiso 1 1 calc R . . C33 C -0.0818(4) -0.1705(5) -0.0126(3) 0.0460(18) Uani 1 1 d . . . C34 C -0.0474(4) -0.2190(6) -0.0488(4) 0.065(3) Uani 1 1 d . . . H34 H -0.0107 -0.1975 -0.0600 0.078 Uiso 1 1 calc R . . C35 C -0.0698(6) -0.2988(7) -0.0669(5) 0.091(4) Uani 1 1 d . . . C36 C -0.1252(6) -0.3327(7) -0.0462(6) 0.097(4) Uani 1 1 d . . . C37 C -0.1569(5) -0.2872(6) -0.0104(5) 0.076(3) Uani 1 1 d . . . H37 H -0.1919 -0.3101 0.0036 0.091 Uiso 1 1 calc R . . C38 C -0.1353(3) -0.2036(5) 0.0052(4) 0.0472(19) Uani 1 1 d . . . C39 C 0.0109(11) -0.3193(10) -0.1255(11) 0.222(13) Uani 1 1 d . . . H39A H 0.0290 -0.3645 -0.1470 0.334 Uiso 1 1 calc R . . H39B H 0.0415 -0.2987 -0.0925 0.334 Uiso 1 1 calc R . . H39C H -0.0021 -0.2719 -0.1527 0.334 Uiso 1 1 calc R . . C40 C -0.1929(10) -0.4532(10) -0.0448(10) 0.214(13) Uani 1 1 d . . . H40A H -0.1900 -0.5156 -0.0466 0.321 Uiso 1 1 calc R . . H40B H -0.2311 -0.4343 -0.0693 0.321 Uiso 1 1 calc R . . H40C H -0.1927 -0.4354 -0.0035 0.321 Uiso 1 1 calc R . . C41 C -0.1169(3) 0.2151(5) -0.0658(3) 0.0383(16) Uani 1 1 d . . . C42 C -0.1317(4) 0.2835(6) -0.1064(4) 0.053(2) Uani 1 1 d . . . H42 H -0.1649 0.3211 -0.1037 0.064 Uiso 1 1 calc R . . C43 C -0.0955(4) 0.2925(6) -0.1497(4) 0.060(2) Uani 1 1 d . . . C44 C -0.0449(4) 0.2344(7) -0.1535(4) 0.064(3) Uani 1 1 d . . . C45 C -0.0296(4) 0.1707(6) -0.1133(4) 0.055(2) Uani 1 1 d . . . H45 H 0.0046 0.1344 -0.1151 0.066 Uiso 1 1 calc R . . C46 C -0.0672(3) 0.1609(5) -0.0684(3) 0.0408(17) Uani 1 1 d . . . C47 C -0.1511(7) 0.4147(10) -0.1916(6) 0.142(7) Uani 1 1 d . . . H47A H -0.1455 0.4632 -0.2175 0.213 Uiso 1 1 calc R . . H47B H -0.1508 0.4351 -0.1508 0.213 Uiso 1 1 calc R . . H47C H -0.1904 0.3868 -0.2059 0.213 Uiso 1 1 calc R . . C48 C 0.0347(8) 0.1913(11) -0.2087(8) 0.171(9) Uani 1 1 d . . . H48A H 0.0504 0.2036 -0.2458 0.257 Uiso 1 1 calc R . . H48B H 0.0185 0.1330 -0.2099 0.257 Uiso 1 1 calc R . . H48C H 0.0681 0.1970 -0.1750 0.257 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0293(5) 0.0354(7) 0.0321(5) -0.0007(5) 0.0061(4) 0.0027(4) Zn2 0.0294(4) 0.0362(5) 0.0356(4) 0.0017(3) 0.0063(3) 0.0038(3) Zn3 0.0404(4) 0.0463(6) 0.0342(4) 0.0033(4) 0.0088(3) 0.0085(4) Zn4 0.0350(4) 0.0397(5) 0.0386(4) 0.0059(4) 0.0069(3) 0.0077(3) Zn5 0.0369(4) 0.0393(5) 0.0565(5) 0.0024(4) 0.0136(4) -0.0019(4) Cl1 0.0625(12) 0.0546(14) 0.0572(12) 0.0180(10) 0.0076(10) 0.0200(10) Cl2 0.0519(12) 0.0470(14) 0.1036(18) 0.0083(12) 0.0102(12) -0.0119(10) Cl3 0.1044(19) 0.0846(19) 0.0386(11) -0.0058(11) 0.0007(11) -0.0033(15) N1 0.038(3) 0.040(4) 0.039(3) 0.002(3) 0.008(2) 0.003(3) N2 0.035(3) 0.038(4) 0.035(3) 0.007(3) 0.005(2) 0.009(3) N3 0.038(3) 0.037(4) 0.038(3) -0.001(3) 0.006(2) 0.007(3) N4 0.034(3) 0.043(4) 0.043(3) 0.004(3) 0.005(3) 0.004(3) N5 0.034(3) 0.041(4) 0.043(3) 0.006(3) 0.009(2) 0.005(3) N6 0.032(3) 0.039(4) 0.048(3) 0.003(3) 0.010(3) -0.003(3) N7 0.041(3) 0.038(4) 0.050(4) 0.007(3) 0.014(3) 0.004(3) N8 0.038(3) 0.038(4) 0.041(3) 0.004(3) 0.006(3) 0.003(3) N9 0.038(3) 0.044(4) 0.038(3) 0.007(3) 0.010(3) 0.006(3) N10 0.034(3) 0.056(4) 0.030(3) 0.002(3) 0.004(2) 0.008(3) N11 0.034(3) 0.039(4) 0.036(3) 0.001(3) 0.004(2) 0.003(2) N12 0.029(3) 0.046(4) 0.037(3) -0.003(3) 0.008(2) 0.004(2) N13 0.038(3) 0.038(4) 0.051(4) -0.003(3) 0.013(3) -0.005(3) N14 0.034(3) 0.036(4) 0.041(3) 0.000(3) 0.009(2) -0.001(2) N15 0.035(3) 0.036(4) 0.043(3) -0.002(3) 0.011(2) 0.001(3) N16 0.034(3) 0.041(4) 0.038(3) 0.002(3) 0.005(2) 0.009(3) N17 0.033(3) 0.034(3) 0.034(3) 0.001(2) 0.006(2) 0.005(2) N18 0.036(3) 0.040(4) 0.040(3) 0.006(3) 0.014(2) 0.005(3) O1 0.113(6) 0.043(4) 0.070(4) -0.009(3) -0.015(4) 0.031(4) O2 0.081(4) 0.051(4) 0.056(3) -0.017(3) -0.005(3) 0.016(3) O3 0.083(6) 0.086(7) 0.280(14) 0.045(8) -0.111(7) -0.012(5) O4 0.062(5) 0.083(7) 0.247(12) 0.024(7) -0.073(6) -0.024(4) O5 0.142(7) 0.111(7) 0.054(4) 0.030(4) 0.021(4) -0.029(6) O6 0.124(6) 0.054(4) 0.081(5) 0.014(4) 0.058(4) -0.006(4) O7 0.027(3) 0.281(13) 0.059(4) -0.044(6) -0.001(3) 0.010(5) O8 0.042(4) 0.357(17) 0.049(4) -0.066(7) -0.014(3) 0.011(6) O9 0.173(9) 0.064(5) 0.191(9) -0.062(6) 0.136(8) -0.042(5) O10 0.187(10) 0.070(6) 0.218(11) -0.087(7) 0.138(9) -0.075(6) O11 0.085(5) 0.113(6) 0.099(5) 0.074(5) 0.058(4) 0.058(4) O12 0.111(6) 0.118(7) 0.114(6) 0.079(5) 0.084(5) 0.068(5) C1 0.037(4) 0.042(5) 0.038(4) 0.000(3) 0.009(3) 0.006(3) C2 0.039(4) 0.052(5) 0.046(4) -0.003(4) 0.005(3) 0.001(3) C3 0.056(5) 0.041(5) 0.053(5) -0.010(4) 0.005(4) 0.004(4) C4 0.061(5) 0.042(5) 0.058(5) -0.001(4) 0.003(4) 0.009(4) C5 0.058(5) 0.042(5) 0.044(4) 0.001(4) -0.002(4) 0.007(4) C6 0.041(4) 0.036(4) 0.038(4) 0.002(3) 0.006(3) 0.002(3) C7 0.134(10) 0.048(7) 0.095(8) 0.010(6) -0.010(7) 0.038(7) C8 0.088(7) 0.058(6) 0.047(5) -0.012(4) -0.001(4) 0.006(5) C9 0.035(4) 0.052(5) 0.052(4) 0.002(4) 0.000(3) 0.000(3) C10 0.050(5) 0.053(6) 0.120(9) 0.015(6) -0.032(5) 0.000(4) C11 0.054(6) 0.065(8) 0.152(11) 0.018(7) -0.048(6) -0.004(5) C12 0.046(5) 0.070(8) 0.153(11) 0.009(7) -0.036(6) -0.014(5) C13 0.043(5) 0.051(6) 0.094(7) 0.006(5) 0.000(4) -0.003(4) C14 0.034(4) 0.042(5) 0.055(4) 0.003(4) 0.006(3) 0.001(3) C15 0.138(14) 0.099(13) 0.42(4) 0.118(18) -0.177(19) -0.028(10) C16 0.078(9) 0.082(11) 0.31(2) 0.038(13) -0.060(12) -0.037(8) C17 0.048(4) 0.046(5) 0.045(4) 0.008(4) 0.019(3) 0.005(4) C18 0.061(5) 0.066(6) 0.046(5) 0.014(4) 0.016(4) -0.001(4) C19 0.089(7) 0.067(7) 0.051(5) 0.013(5) 0.023(5) -0.003(5) C20 0.083(6) 0.052(6) 0.068(6) 0.016(5) 0.048(5) 0.011(5) C21 0.058(5) 0.048(5) 0.059(5) 0.000(4) 0.029(4) 0.000(4) C22 0.043(4) 0.040(5) 0.053(4) 0.009(4) 0.023(3) 0.009(3) C23 0.176(15) 0.199(19) 0.060(8) 0.047(10) 0.008(9) -0.049(14) C24 0.098(8) 0.050(6) 0.097(8) 0.009(6) 0.054(7) 0.004(6) C25 0.032(4) 0.075(6) 0.037(4) -0.001(4) 0.004(3) 0.003(4) C26 0.035(4) 0.157(11) 0.039(4) -0.024(5) -0.001(3) 0.009(5) C27 0.044(5) 0.170(12) 0.043(5) -0.029(6) -0.003(4) 0.003(6) C28 0.029(4) 0.182(13) 0.049(5) -0.018(6) -0.001(4) 0.004(6) C29 0.032(4) 0.110(8) 0.041(4) -0.012(5) 0.003(3) 0.002(4) C30 0.029(3) 0.066(6) 0.036(4) -0.004(4) 0.004(3) 0.007(3) C31 0.032(5) 0.42(3) 0.076(8) -0.045(13) 0.012(5) 0.024(10) C32 0.073(8) 0.40(3) 0.054(7) -0.074(12) -0.026(6) 0.033(13) C33 0.052(4) 0.035(5) 0.054(4) -0.006(4) 0.018(4) 0.000(3) C34 0.072(6) 0.044(5) 0.089(7) -0.018(5) 0.045(5) -0.011(4) C35 0.117(9) 0.061(7) 0.116(9) -0.041(6) 0.081(8) -0.026(6) C36 0.121(10) 0.052(7) 0.136(10) -0.037(7) 0.074(8) -0.036(6) C37 0.085(7) 0.045(6) 0.113(8) -0.030(5) 0.060(6) -0.030(5) C38 0.046(4) 0.043(5) 0.056(5) -0.008(4) 0.018(4) -0.004(3) C39 0.31(3) 0.093(11) 0.34(3) -0.106(14) 0.29(2) -0.082(14) C40 0.26(2) 0.097(12) 0.34(3) -0.134(16) 0.22(2) -0.124(14) C41 0.034(3) 0.048(5) 0.035(4) 0.007(3) 0.009(3) 0.002(3) C42 0.042(4) 0.062(6) 0.059(5) 0.020(4) 0.019(4) 0.018(4) C43 0.057(5) 0.066(6) 0.063(5) 0.035(5) 0.022(4) 0.023(4) C44 0.060(5) 0.081(7) 0.061(5) 0.026(5) 0.037(4) 0.027(5) C45 0.053(5) 0.057(6) 0.059(5) 0.024(4) 0.025(4) 0.022(4) C46 0.039(4) 0.044(5) 0.041(4) 0.009(3) 0.012(3) 0.007(3) C47 0.143(12) 0.171(15) 0.134(11) 0.114(11) 0.090(10) 0.120(11) C48 0.185(15) 0.174(15) 0.201(16) 0.124(13) 0.173(14) 0.117(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N12 2.139(5) 3 ? Zn1 N12 2.139(5) . ? Zn1 N18 2.139(6) . ? Zn1 N18 2.139(6) 3 ? Zn1 N15 2.150(6) 3 ? Zn1 N15 2.150(6) . ? Zn2 N14 2.157(6) . ? Zn2 N11 2.160(5) . ? Zn2 N2 2.172(6) . ? Zn2 N17 2.177(5) . ? Zn2 N5 2.197(6) . ? Zn2 N8 2.232(6) . ? Zn3 N10 2.004(5) . ? Zn3 N9 2.005(6) . ? Zn3 N3 2.011(6) . ? Zn3 Cl3 2.154(2) . ? Zn4 N16 2.002(5) . ? Zn4 N1 2.006(6) . ? Zn4 N4 2.014(6) . ? Zn4 Cl1 2.169(2) . ? Zn5 N7 1.997(6) . ? Zn5 N13 2.004(6) . ? Zn5 N6 2.012(6) . ? Zn5 Cl2 2.169(2) . ? N1 N2 1.339(8) . ? N1 C6 1.356(9) . ? N2 N3 1.334(8) . ? N3 C1 1.348(9) . ? N4 N5 1.328(8) . ? N4 C9 1.340(9) . ? N5 N6 1.332(8) . ? N6 C14 1.343(9) . ? N7 N8 1.333(8) . ? N7 C22 1.375(9) . ? N8 N9 1.339(8) . ? N9 C17 1.356(9) . ? N10 N11 1.351(8) . ? N10 C25 1.365(9) . ? N11 N12 1.335(7) . ? N12 C30 1.364(9) . ? N13 N14 1.343(8) . ? N13 C38 1.352(9) . ? N14 N15 1.345(7) . ? N15 C33 1.349(10) . ? N16 N17 1.339(8) . ? N16 C41 1.371(8) . ? N17 N18 1.345(7) . ? N18 C46 1.357(9) . ? O1 C4 1.362(10) . ? O1 C7 1.430(12) . ? O2 C3 1.363(9) . ? O2 C8 1.420(10) . ? O3 C11 1.338(11) . ? O3 C15 1.414(16) . ? O4 C12 1.348(11) . ? O4 C16 1.425(15) . ? O5 C19 1.366(11) . ? O5 C23 1.407(17) . ? O6 C20 1.371(10) . ? O6 C24 1.380(12) . ? O7 C28 1.363(10) . ? O7 C31 1.472(12) . ? O8 C27 1.352(10) . ? O8 C32 1.450(13) . ? O9 C35 1.341(11) . ? O9 C39 1.486(14) . ? O10 C36 1.371(12) . ? O10 C40 1.472(15) . ? O11 C43 1.351(9) . ? O11 C47 1.426(11) . ? O12 C44 1.381(9) . ? O12 C48 1.459(13) . ? C1 C6 1.380(10) . ? C1 C2 1.435(10) . ? C2 C3 1.359(11) . ? C3 C4 1.436(12) . ? C4 C5 1.345(11) . ? C5 C6 1.403(11) . ? C9 C14 1.379(11) . ? C9 C10 1.431(11) . ? C10 C11 1.377(13) . ? C11 C12 1.428(15) . ? C12 C13 1.362(13) . ? C13 C14 1.421(11) . ? C17 C22 1.358(11) . ? C17 C18 1.417(11) . ? C18 C19 1.349(13) . ? C19 C20 1.414(14) . ? C20 C21 1.368(12) . ? C21 C22 1.420(11) . ? C25 C30 1.380(10) . ? C25 C26 1.401(11) . ? C26 C27 1.347(12) . ? C27 C28 1.434(12) . ? C28 C29 1.364(11) . ? C29 C30 1.406(10) . ? C33 C38 1.392(10) . ? C33 C34 1.408(11) . ? C34 C35 1.367(13) . ? C35 C36 1.462(13) . ? C36 C37 1.341(13) . ? C37 C38 1.404(12) . ? C41 C46 1.381(10) . ? C41 C42 1.402(10) . ? C42 C43 1.355(10) . ? C43 C44 1.439(11) . ? C44 C45 1.345(11) . ? C45 C46 1.407(10) . ? 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 N12 Zn1 N12 180 3 . ? N12 Zn1 N18 88.2(2) 3 . ? N12 Zn1 N18 91.8(2) . . ? N12 Zn1 N18 91.8(2) 3 3 ? N12 Zn1 N18 88.2(2) . 3 ? N18 Zn1 N18 180 . 3 ? N12 Zn1 N15 91.4(2) 3 3 ? N12 Zn1 N15 88.6(2) . 3 ? N18 Zn1 N15 88.0(2) . 3 ? N18 Zn1 N15 92.0(2) 3 3 ? N12 Zn1 N15 88.6(2) 3 . ? N12 Zn1 N15 91.4(2) . . ? N18 Zn1 N15 92.0(2) . . ? N18 Zn1 N15 88.0(2) 3 . ? N15 Zn1 N15 180 3 . ? N14 Zn2 N11 90.1(2) . . ? N14 Zn2 N2 179.0(2) . . ? N11 Zn2 N2 89.3(2) . . ? N14 Zn2 N17 91.2(2) . . ? N11 Zn2 N17 90.8(2) . . ? N2 Zn2 N17 89.5(2) . . ? N14 Zn2 N5 90.5(2) . . ? N11 Zn2 N5 178.5(2) . . ? N2 Zn2 N5 90.1(2) . . ? N17 Zn2 N5 90.6(2) . . ? N14 Zn2 N8 90.1(2) . . ? N11 Zn2 N8 91.1(2) . . ? N2 Zn2 N8 89.1(2) . . ? N17 Zn2 N8 177.7(2) . . ? N5 Zn2 N8 87.5(2) . . ? N10 Zn3 N9 97.8(2) . . ? N10 Zn3 N3 98.5(2) . . ? N9 Zn3 N3 102.6(2) . . ? N10 Zn3 Cl3 119.57(18) . . ? N9 Zn3 Cl3 115.45(18) . . ? N3 Zn3 Cl3 119.22(19) . . ? N16 Zn4 N1 97.7(2) . . ? N16 Zn4 N4 98.8(2) . . ? N1 Zn4 N4 101.1(2) . . ? N16 Zn4 Cl1 118.59(18) . . ? N1 Zn4 Cl1 117.80(19) . . ? N4 Zn4 Cl1 118.90(18) . . ? N7 Zn5 N13 98.8(2) . . ? N7 Zn5 N6 103.2(2) . . ? N13 Zn5 N6 98.2(2) . . ? N7 Zn5 Cl2 117.94(19) . . ? N13 Zn5 Cl2 119.53(19) . . ? N6 Zn5 Cl2 115.77(18) . . ? N2 N1 C6 107.9(6) . . ? N2 N1 Zn4 120.1(5) . . ? C6 N1 Zn4 131.9(5) . . ? N3 N2 N1 109.6(5) . . ? N3 N2 Zn2 126.8(4) . . ? N1 N2 Zn2 123.5(4) . . ? N2 N3 C1 107.8(5) . . ? N2 N3 Zn3 117.0(4) . . ? C1 N3 Zn3 135.2(5) . . ? N5 N4 C9 106.8(6) . . ? N5 N4 Zn4 119.2(4) . . ? C9 N4 Zn4 134.0(5) . . ? N4 N5 N6 110.7(5) . . ? N4 N5 Zn2 124.0(4) . . ? N6 N5 Zn2 124.9(4) . . ? N5 N6 C14 107.4(6) . . ? N5 N6 Zn5 118.4(4) . . ? C14 N6 Zn5 134.2(5) . . ? N8 N7 C22 106.8(6) . . ? N8 N7 Zn5 116.8(4) . . ? C22 N7 Zn5 136.4(5) . . ? N7 N8 N9 109.9(5) . . ? N7 N8 Zn2 125.4(4) . . ? N9 N8 Zn2 123.4(4) . . ? N8 N9 C17 108.0(6) . . ? N8 N9 Zn3 118.9(4) . . ? C17 N9 Zn3 133.0(5) . . ? N11 N10 C25 106.5(5) . . ? N11 N10 Zn3 119.7(4) . . ? C25 N10 Zn3 133.7(5) . . ? N12 N11 N10 110.9(5) . . ? N12 N11 Zn2 125.1(4) . . ? N10 N11 Zn2 123.9(4) . . ? N11 N12 C30 107.0(5) . . ? N11 N12 Zn1 124.0(4) . . ? C30 N12 Zn1 129.0(4) . . ? N14 N13 C38 107.5(5) . . ? N14 N13 Zn5 118.6(4) . . ? C38 N13 Zn5 133.9(5) . . ? N13 N14 N15 110.5(5) . . ? N13 N14 Zn2 125.2(4) . . ? N15 N14 Zn2 124.3(4) . . ? N14 N15 C33 106.7(6) . . ? N14 N15 Zn1 124.4(4) . . ? C33 N15 Zn1 128.9(5) . . ? N17 N16 C41 107.8(5) . . ? N17 N16 Zn4 118.0(4) . . ? C41 N16 Zn4 134.2(5) . . ? N16 N17 N18 109.9(5) . . ? N16 N17 Zn2 125.6(4) . . ? N18 N17 Zn2 124.5(4) . . ? N17 N18 C46 107.5(5) . . ? N17 N18 Zn1 124.0(4) . . ? C46 N18 Zn1 128.5(4) . . ? C4 O1 C7 115.2(7) . . ? C3 O2 C8 117.4(7) . . ? C11 O3 C15 116.9(10) . . ? C12 O4 C16 115.9(9) . . ? C19 O5 C23 116.1(9) . . ? C20 O6 C24 117.4(8) . . ? C28 O7 C31 115.7(7) . . ? C27 O8 C32 115.0(8) . . ? C35 O9 C39 114.8(8) . . ? C36 O10 C40 114.0(9) . . ? C43 O11 C47 116.7(7) . . ? C44 O12 C48 114.2(7) . . ? N3 C1 C6 107.9(6) . . ? N3 C1 C2 131.3(7) . . ? C6 C1 C2 120.8(7) . . ? C3 C2 C1 115.8(7) . . ? C2 C3 O2 123.8(7) . . ? C2 C3 C4 122.4(7) . . ? O2 C3 C4 113.7(7) . . ? C5 C4 O1 125.5(8) . . ? C5 C4 C3 121.5(8) . . ? O1 C4 C3 112.9(7) . . ? C4 C5 C6 116.9(7) . . ? N1 C6 C1 106.8(6) . . ? N1 C6 C5 130.7(7) . . ? C1 C6 C5 122.5(7) . . ? N4 C9 C14 108.2(7) . . ? N4 C9 C10 129.3(8) . . ? C14 C9 C10 122.5(7) . . ? C11 C10 C9 114.8(9) . . ? O3 C11 C10 123.3(10) . . ? O3 C11 C12 114.5(9) . . ? C10 C11 C12 122.1(9) . . ? O4 C12 C13 123.5(10) . . ? O4 C12 C11 113.5(9) . . ? C13 C12 C11 123.0(9) . . ? C12 C13 C14 115.5(9) . . ? N6 C14 C9 106.9(6) . . ? N6 C14 C13 131.1(8) . . ? C9 C14 C13 122.0(7) . . ? N9 C17 C22 107.4(7) . . ? N9 C17 C18 130.4(8) . . ? C22 C17 C18 122.2(7) . . ? C19 C18 C17 116.6(9) . . ? C18 C19 O5 125.3(10) . . ? C18 C19 C20 121.2(8) . . ? O5 C19 C20 113.5(9) . . ? C21 C20 O6 122.9(10) . . ? C21 C20 C19 123.2(8) . . ? O6 C20 C19 113.9(8) . . ? C20 C21 C22 115.0(8) . . ? C17 C22 N7 108.0(7) . . ? C17 C22 C21 121.8(7) . . ? N7 C22 C21 130.1(8) . . ? N10 C25 C30 107.8(6) . . ? N10 C25 C26 129.6(7) . . ? C30 C25 C26 122.5(7) . . ? C27 C26 C25 115.9(8) . . ? C26 C27 O8 124.5(8) . . ? C26 C27 C28 122.2(8) . . ? O8 C27 C28 113.2(8) . . ? O7 C28 C29 123.9(8) . . ? O7 C28 C27 114.3(7) . . ? C29 C28 C27 121.7(8) . . ? C28 C29 C30 115.9(7) . . ? N12 C30 C25 107.7(6) . . ? N12 C30 C29 130.7(7) . . ? C25 C30 C29 121.6(7) . . ? N15 C33 C38 108.3(6) . . ? N15 C33 C34 130.6(7) . . ? C38 C33 C34 121.2(7) . . ? C35 C34 C33 117.2(8) . . ? O9 C35 C34 125.8(9) . . ? O9 C35 C36 113.8(9) . . ? C34 C35 C36 120.3(8) . . ? C37 C36 O10 125.7(9) . . ? C37 C36 C35 122.3(9) . . ? O10 C36 C35 112.1(9) . . ? C36 C37 C38 116.7(8) . . ? N13 C38 C33 107.0(7) . . ? N13 C38 C37 130.8(7) . . ? C33 C38 C37 122.2(7) . . ? N16 C41 C46 106.7(6) . . ? N16 C41 C42 131.0(6) . . ? C46 C41 C42 122.3(6) . . ? C43 C42 C41 116.4(7) . . ? O11 C43 C42 125.4(7) . . ? O11 C43 C44 113.3(7) . . ? C42 C43 C44 121.3(7) . . ? C45 C44 O12 125.0(7) . . ? C45 C44 C43 122.1(7) . . ? O12 C44 C43 112.9(7) . . ? C44 C45 C46 116.8(7) . . ? N18 C46 C41 108.1(6) . . ? N18 C46 C45 130.9(7) . . ? C41 C46 C45 121.0(7) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.93 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.678 _refine_diff_density_min -0.428 _refine_diff_density_rms 0.178 # Attachment '- bis721b_new.cif' #data_publication_text #TrackingRef '- bis721b_new.cif' data_bis721b _database_code_depnum_ccdc_archive 'CCDC 778556' #TrackingRef '- bis721b_new.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C96 H96 Cl6 Fe3 N36 O24 Zn6' _chemical_formula_sum 'C96 H96 Cl6 Fe3 N36 O24 Zn6' _chemical_melting_point ? _exptl_crystal_description needle _exptl_crystal_colour red _diffrn_ambient_temperature 223(2) _chemical_formula_weight 2910.72 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' N N 0.0061 0.0033 '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' Fe Fe 0.3463 0.8444 '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' O O 0.0106 0.0060 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_int_tables_number 14 _chemical_absolute_configuration unk 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 19.847(4) _cell_length_b 15.759(3) _cell_length_c 28.428(6) _cell_angle_alpha 90.00 _cell_angle_beta 110.43(3) _cell_angle_gamma 90.00 _cell_volume 8332(3) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 45149 _cell_measurement_theta_min 1.69 _cell_measurement_theta_max 24.02 _exptl_crystal_size_max 0.462 _exptl_crystal_size_mid 0.154 _exptl_crystal_size_min 0.077 _exptl_crystal_density_diffrn 1.160 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2952 _exptl_absorpt_coefficient_mu 1.257 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type 'STOE IPDS' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 45149 _diffrn_reflns_av_R_equivalents 0.1171 _diffrn_reflns_av_sigmaI/netI 0.1511 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 24.02 _reflns_number_total 13026 _reflns_number_gt 6319 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1533P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13026 _refine_ls_number_parameters 774 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1603 _refine_ls_R_factor_gt 0.0901 _refine_ls_wR_factor_ref 0.2949 _refine_ls_wR_factor_gt 0.2656 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.5000 0.0000 0.0000 0.0252(5) Uani 1 2 d S . . Fe2 Fe 0.37835(7) 0.04266(9) 0.07068(5) 0.0226(4) Uani 1 1 d . . . Zn1 Zn 0.37123(7) -0.13732(9) 0.14379(6) 0.0422(4) Uani 1 1 d . . . Zn2 Zn 0.44635(8) 0.21882(9) 0.15008(6) 0.0438(4) Uani 1 1 d . . . Zn3 Zn 0.20439(7) 0.08607(9) -0.01500(5) 0.0359(4) Uani 1 1 d . . . Cl1 Cl 0.3648(3) -0.2502(3) 0.18345(19) 0.0903(14) Uani 1 1 d . . . Cl2 Cl 0.4743(2) 0.3328(3) 0.19402(17) 0.0766(12) Uani 1 1 d . . . Cl3 Cl 0.09847(17) 0.1072(3) -0.07015(14) 0.0622(10) Uani 1 1 d . . . N1 N 0.2790(5) -0.1000(6) 0.0901(3) 0.034(2) Uani 1 1 d . . . N2 N 0.2792(5) -0.0285(6) 0.0645(4) 0.034(2) Uani 1 1 d . . . N3 N 0.2136(5) -0.0127(6) 0.0304(4) 0.033(2) Uani 1 1 d . . . N4 N 0.4352(5) 0.1085(6) 0.1824(4) 0.041(2) Uani 1 1 d . . . N5 N 0.4081(5) 0.0394(6) 0.1528(4) 0.038(2) Uani 1 1 d . . . N6 N 0.4008(5) -0.0247(6) 0.1799(4) 0.034(2) Uani 1 1 d . . . N7 N 0.3446(5) 0.2258(6) 0.0969(4) 0.038(2) Uani 1 1 d . . . N8 N 0.3182(5) 0.1599(6) 0.0670(4) 0.038(2) Uani 1 1 d . . . N9 N 0.2522(5) 0.1774(6) 0.0353(3) 0.035(2) Uani 1 1 d . . . N10 N 0.4357(5) -0.1391(6) 0.1014(4) 0.037(2) Uani 1 1 d . . . N11 N 0.4362(4) -0.0715(6) 0.0726(3) 0.030(2) Uani 1 1 d . . . N12 N 0.4805(5) -0.0852(6) 0.0471(3) 0.032(2) Uani 1 1 d . . . N13 N 0.4989(5) 0.1802(6) 0.1057(4) 0.037(2) Uani 1 1 d . . . N14 N 0.4740(5) 0.1131(6) 0.0751(3) 0.033(2) Uani 1 1 d . . . N15 N 0.5165(4) 0.0968(5) 0.0494(3) 0.028(2) Uani 1 1 d . . . N16 N 0.2832(5) 0.0583(6) -0.0417(3) 0.034(2) Uani 1 1 d . . . N17 N 0.3503(5) 0.0429(6) -0.0093(3) 0.031(2) Uani 1 1 d . . . N18 N 0.3955(4) 0.0270(5) -0.0339(3) 0.028(2) Uani 1 1 d . . . O1 O 0.0772(4) -0.2966(5) 0.0592(4) 0.059(3) Uani 1 1 d . . . O2 O 0.0010(4) -0.1958(5) -0.0068(4) 0.052(2) Uani 1 1 d . . . O3 O 0.4993(8) 0.1228(7) 0.3633(4) 0.090(4) Uani 1 1 d . . . O4 O 0.4523(7) -0.0262(7) 0.3608(4) 0.082(4) Uani 1 1 d . . . O5 O 0.1216(5) 0.4432(6) 0.0251(4) 0.066(3) Uani 1 1 d . . . O6 O 0.2292(6) 0.4977(7) 0.0960(5) 0.096(4) Uani 1 1 d . . . O7 O 0.6234(7) -0.3438(6) 0.0554(5) 0.089(4) Uani 1 1 d . . . O8 O 0.5680(8) -0.4042(7) 0.1173(6) 0.109(5) Uani 1 1 d . . . O9 O 0.7145(5) 0.3453(6) 0.1248(4) 0.077(4) Uani 1 1 d . . . O10 O 0.7353(5) 0.2520(7) 0.0593(4) 0.082(4) Uani 1 1 d . . . O11 O 0.2039(5) 0.0622(9) -0.2242(3) 0.095(4) Uani 1 1 d . . . O12 O 0.3319(5) 0.0325(9) -0.2172(3) 0.083(4) Uani 1 1 d . . . C1 C 0.2100(6) -0.1323(7) 0.0700(5) 0.035(3) Uani 1 1 d . . . C2 C 0.1827(6) -0.2078(8) 0.0816(5) 0.042(3) Uani 1 1 d . . . H2 H 0.2110 -0.2445 0.1069 0.050 Uiso 1 1 calc R . . C3 C 0.1134(6) -0.2253(8) 0.0545(5) 0.046(3) Uani 1 1 d . . . C4 C 0.0697(6) -0.1672(8) 0.0168(5) 0.038(3) Uani 1 1 d . . . C5 C 0.0972(6) -0.0945(7) 0.0063(5) 0.037(3) Uani 1 1 d . . . H5 H 0.0691 -0.0567 -0.0184 0.055 Uiso 1 1 calc R . . C6 C 0.1697(6) -0.0777(7) 0.0341(4) 0.032(3) Uani 1 1 d . . . C7 C 0.1207(8) -0.3610(10) 0.0898(8) 0.096(7) Uani 1 1 d . . . H7A H 0.0916 -0.4110 0.0887 0.144 Uiso 1 1 calc R . . H7B H 0.1409 -0.3408 0.1242 0.144 Uiso 1 1 calc R . . H7C H 0.1593 -0.3752 0.0777 0.144 Uiso 1 1 calc R . . C8 C -0.0449(7) -0.1426(10) -0.0448(5) 0.062(4) Uani 1 1 d . . . H8A H -0.0913 -0.1698 -0.0598 0.092 Uiso 1 1 calc R . . H8B H -0.0237 -0.1328 -0.0703 0.092 Uiso 1 1 calc R . . H8C H -0.0510 -0.0888 -0.0302 0.092 Uiso 1 1 calc R . . C9 C 0.4440(6) 0.0853(8) 0.2293(4) 0.039(3) Uani 1 1 d . . . C10 C 0.4713(8) 0.1300(9) 0.2727(5) 0.056(4) Uani 1 1 d . . . H10 H 0.4869 0.1864 0.2730 0.067 Uiso 1 1 calc R . . C11 C 0.4751(9) 0.0883(10) 0.3168(5) 0.064(4) Uani 1 1 d . . . C12 C 0.4489(8) 0.0027(9) 0.3151(5) 0.057(4) Uani 1 1 d . . . C13 C 0.4237(7) -0.0399(9) 0.2714(5) 0.050(3) Uani 1 1 d . . . H13 H 0.4072 -0.0960 0.2702 0.060 Uiso 1 1 calc R . . C14 C 0.4229(6) 0.0008(8) 0.2285(5) 0.040(3) Uani 1 1 d . . . C15 C 0.5235(15) 0.2089(12) 0.3675(7) 0.126(9) Uani 1 1 d . . . H15A H 0.5425 0.2251 0.4026 0.189 Uiso 1 1 calc R . . H15B H 0.4835 0.2457 0.3497 0.189 Uiso 1 1 calc R . . H15C H 0.5609 0.2144 0.3530 0.189 Uiso 1 1 calc R . . C16 C 0.4178(13) -0.1077(12) 0.3608(7) 0.104(7) Uani 1 1 d . . . H16A H 0.4126 -0.1167 0.3931 0.156 Uiso 1 1 calc R . . H16B H 0.4470 -0.1527 0.3546 0.156 Uiso 1 1 calc R . . H16C H 0.3707 -0.1082 0.3346 0.156 Uiso 1 1 calc R . . C17 C 0.2943(6) 0.2873(7) 0.0839(5) 0.039(3) Uani 1 1 d . . . C18 C 0.2956(7) 0.3695(8) 0.1034(5) 0.052(4) Uani 1 1 d . . . H18 H 0.3356 0.3900 0.1299 0.062 Uiso 1 1 calc R . . C19 C 0.2374(8) 0.4167(9) 0.0823(6) 0.063(4) Uani 1 1 d . . . C20 C 0.1756(6) 0.3846(8) 0.0426(5) 0.048(3) Uani 1 1 d . . . C21 C 0.1746(6) 0.3054(7) 0.0231(5) 0.039(3) Uani 1 1 d . . . H21 H 0.1348 0.2850 -0.0036 0.047 Uiso 1 1 calc R . . C22 C 0.2355(6) 0.2569(7) 0.0450(4) 0.034(3) Uani 1 1 d . . . C23 C 0.2898(12) 0.5313(13) 0.1364(11) 0.187(16) Uani 1 1 d . . . H23D H 0.2924 0.5922 0.1324 0.281 Uiso 1 1 calc R . . H23E H 0.3337 0.5051 0.1358 0.281 Uiso 1 1 calc R . . H23F H 0.2840 0.5192 0.1683 0.281 Uiso 1 1 calc R . . C24 C 0.0632(8) 0.4176(10) -0.0180(7) 0.084(6) Uani 1 1 d . . . H24A H 0.0279 0.4627 -0.0280 0.126 Uiso 1 1 calc R . . H24B H 0.0413 0.3670 -0.0102 0.126 Uiso 1 1 calc R . . H24C H 0.0807 0.4054 -0.0451 0.126 Uiso 1 1 calc R . . C25 C 0.4799(6) -0.1987(7) 0.0935(4) 0.035(3) Uani 1 1 d . . . C26 C 0.4962(8) -0.2789(9) 0.1133(6) 0.060(4) Uani 1 1 d . . . H26 H 0.4739 -0.3014 0.1348 0.071 Uiso 1 1 calc R . . C27 C 0.5452(9) -0.3243(9) 0.1010(6) 0.066(4) Uani 1 1 d . . . C28 C 0.5752(8) -0.2908(9) 0.0654(6) 0.060(4) Uani 1 1 d . . . C29 C 0.5566(7) -0.2117(8) 0.0446(5) 0.046(3) Uani 1 1 d . . . H29 H 0.5755 -0.1897 0.0211 0.055 Uiso 1 1 calc R . . H45 H 0.4220 0.0092 -0.1243 0.055 Uiso 1 1 d R . . C30 C 0.5084(6) -0.1659(7) 0.0602(4) 0.034(3) Uani 1 1 d . . . C31 C 0.5392(17) -0.4402(15) 0.1529(12) 0.192(17) Uani 1 1 d . . . H31A H 0.5278 -0.4996 0.1449 0.288 Uiso 1 1 calc R . . H31B H 0.4959 -0.4099 0.1512 0.288 Uiso 1 1 calc R . . H31C H 0.5745 -0.4355 0.1864 0.288 Uiso 1 1 calc R . . C32 C 0.6605(13) -0.3112(12) 0.0237(10) 0.140(11) Uani 1 1 d . . . H32A H 0.6956 -0.3524 0.0216 0.210 Uiso 1 1 calc R . . H32B H 0.6847 -0.2587 0.0377 0.210 Uiso 1 1 calc R . . H32C H 0.6260 -0.3005 -0.0097 0.210 Uiso 1 1 calc R . . C33 C 0.5594(6) 0.2070(7) 0.0983(4) 0.035(3) Uani 1 1 d . . . C34 C 0.6063(7) 0.2744(8) 0.1217(5) 0.047(3) Uani 1 1 d . . . H34 H 0.5982 0.3090 0.1461 0.057 Uiso 1 1 calc R . . C35 C 0.6632(7) 0.2858(8) 0.1069(5) 0.051(4) Uani 1 1 d . . . C36 C 0.6757(7) 0.2314(9) 0.0698(5) 0.051(4) Uani 1 1 d . . . C37 C 0.6301(6) 0.1677(8) 0.0482(5) 0.040(3) Uani 1 1 d . . . H37 H 0.6379 0.1330 0.0237 0.048 Uiso 1 1 calc R . . C38 C 0.5713(6) 0.1548(7) 0.0631(4) 0.031(3) Uani 1 1 d . . . C39 C 0.7078(9) 0.3979(13) 0.1650(8) 0.112(8) Uani 1 1 d . . . H39A H 0.7500 0.4336 0.1784 0.167 Uiso 1 1 calc R . . H39B H 0.7036 0.3619 0.1915 0.167 Uiso 1 1 calc R . . H39C H 0.6653 0.4333 0.1520 0.167 Uiso 1 1 calc R . . C40 C 0.7470(10) 0.2046(14) 0.0197(9) 0.132(10) Uani 1 1 d . . . H40A H 0.7909 0.2240 0.0154 0.198 Uiso 1 1 calc R . . H40B H 0.7068 0.2130 -0.0113 0.198 Uiso 1 1 calc R . . H40C H 0.7513 0.1447 0.0283 0.198 Uiso 1 1 calc R . . C41 C 0.2857(6) 0.0531(8) -0.0893(4) 0.040(3) Uani 1 1 d . . . C42 C 0.2307(7) 0.0627(9) -0.1351(5) 0.054(4) Uani 1 1 d . . . H42 H 0.1830 0.0740 -0.1376 0.064 Uiso 1 1 calc R . . C43 C 0.2507(7) 0.0544(11) -0.1762(5) 0.064(4) Uani 1 1 d . . . C44 C 0.3224(7) 0.0370(10) -0.1725(5) 0.057(4) Uani 1 1 d . . . C45 C 0.3749(6) 0.0246(9) -0.1269(5) 0.046(3) Uani 1 1 d . . . C46 C 0.3557(6) 0.0342(7) -0.0841(4) 0.034(3) Uani 1 1 d . . . C47 C 0.1304(8) 0.0758(17) -0.2299(6) 0.120(9) Uani 1 1 d . . . H47A H 0.1276 0.1170 -0.2053 0.179 Uiso 1 1 calc R . . H47B H 0.1092 0.0226 -0.2248 0.179 Uiso 1 1 calc R . . H47C H 0.1045 0.0969 -0.2634 0.179 Uiso 1 1 calc R . . C48 C 0.4042(9) 0.0209(17) -0.2152(6) 0.119(9) Uani 1 1 d . . . H48A H 0.4049 0.0156 -0.2491 0.179 Uiso 1 1 calc R . . H48B H 0.4238 -0.0302 -0.1964 0.179 Uiso 1 1 calc R . . H48C H 0.4330 0.0693 -0.1989 0.179 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0219(11) 0.0280(12) 0.0244(12) -0.0043(10) 0.0065(9) -0.0031(9) Fe2 0.0190(7) 0.0249(8) 0.0233(8) -0.0040(7) 0.0066(6) -0.0025(6) Zn1 0.0398(8) 0.0426(8) 0.0451(9) -0.0060(7) 0.0158(7) -0.0070(7) Zn2 0.0451(8) 0.0427(9) 0.0488(10) -0.0094(7) 0.0230(7) -0.0064(7) Zn3 0.0283(7) 0.0383(8) 0.0398(9) -0.0032(7) 0.0101(6) -0.0015(6) Cl1 0.109(3) 0.074(3) 0.093(3) 0.030(3) 0.042(3) -0.006(3) Cl2 0.064(2) 0.069(3) 0.084(3) -0.039(2) 0.010(2) -0.014(2) Cl3 0.0344(17) 0.081(3) 0.058(2) 0.009(2) 0.0001(16) 0.0079(17) N1 0.034(5) 0.040(6) 0.031(6) 0.000(5) 0.014(4) -0.006(4) N2 0.033(5) 0.034(6) 0.035(6) -0.004(5) 0.011(5) -0.012(4) N3 0.026(5) 0.033(5) 0.040(6) 0.001(4) 0.011(5) 0.000(4) N4 0.041(6) 0.045(6) 0.037(6) -0.012(5) 0.012(5) -0.005(5) N5 0.035(5) 0.044(6) 0.033(6) -0.007(5) 0.011(5) -0.004(5) N6 0.033(5) 0.035(6) 0.038(6) 0.002(5) 0.016(5) -0.007(4) N7 0.034(5) 0.035(6) 0.045(6) -0.014(5) 0.012(5) -0.007(5) N8 0.034(5) 0.034(6) 0.046(6) -0.003(5) 0.016(5) 0.004(4) N9 0.029(5) 0.034(6) 0.033(6) -0.004(5) 0.002(4) -0.001(4) N10 0.046(6) 0.030(5) 0.038(6) 0.004(5) 0.017(5) -0.001(5) N11 0.025(5) 0.037(5) 0.029(5) -0.006(4) 0.010(4) -0.001(4) N12 0.026(5) 0.032(5) 0.035(6) -0.003(4) 0.007(4) -0.005(4) N13 0.030(5) 0.044(6) 0.036(6) -0.008(5) 0.011(5) -0.001(4) N14 0.032(5) 0.031(5) 0.033(6) -0.006(4) 0.006(4) -0.010(4) N15 0.027(5) 0.034(5) 0.025(5) -0.005(4) 0.012(4) -0.003(4) N16 0.025(5) 0.041(6) 0.033(6) -0.001(5) 0.005(4) -0.004(4) N17 0.027(5) 0.039(5) 0.027(5) -0.005(4) 0.009(4) 0.001(4) N18 0.026(5) 0.030(5) 0.025(5) -0.007(4) 0.004(4) -0.003(4) O1 0.038(5) 0.037(5) 0.090(8) 0.016(5) 0.006(5) -0.012(4) O2 0.025(4) 0.050(5) 0.072(7) 0.011(5) 0.007(4) -0.007(4) O3 0.165(12) 0.065(7) 0.031(6) -0.014(5) 0.021(7) -0.024(7) O4 0.148(11) 0.067(7) 0.040(6) -0.007(5) 0.043(7) -0.018(7) O5 0.041(5) 0.053(6) 0.085(8) -0.022(5) -0.001(5) 0.013(4) O6 0.070(7) 0.051(6) 0.123(11) -0.041(7) -0.022(7) 0.015(5) O7 0.119(10) 0.051(6) 0.137(11) 0.034(7) 0.094(9) 0.040(6) O8 0.154(12) 0.063(7) 0.161(13) 0.058(8) 0.118(11) 0.062(8) O9 0.061(6) 0.077(7) 0.114(9) -0.061(7) 0.055(6) -0.045(6) O10 0.068(7) 0.094(8) 0.110(9) -0.068(7) 0.066(7) -0.059(6) O11 0.054(6) 0.198(14) 0.021(5) 0.010(7) -0.001(5) 0.047(8) O12 0.050(6) 0.167(12) 0.030(5) 0.006(6) 0.013(5) 0.031(7) C1 0.030(6) 0.033(6) 0.045(8) -0.001(6) 0.016(6) -0.008(5) C2 0.031(6) 0.039(7) 0.052(8) 0.008(6) 0.010(6) -0.002(6) C3 0.036(7) 0.042(8) 0.058(9) 0.001(7) 0.013(7) -0.004(6) C4 0.023(6) 0.044(7) 0.044(8) 0.000(6) 0.009(6) -0.004(5) C5 0.033(6) 0.037(7) 0.042(8) -0.004(6) 0.014(6) -0.003(5) C6 0.034(6) 0.032(6) 0.034(7) -0.007(5) 0.018(6) -0.008(5) C7 0.057(10) 0.051(10) 0.142(18) 0.038(11) -0.012(10) -0.021(8) C8 0.040(8) 0.073(10) 0.060(10) 0.015(8) 0.003(7) 0.000(7) C9 0.046(7) 0.048(8) 0.023(7) -0.016(6) 0.013(6) -0.008(6) C10 0.070(9) 0.046(8) 0.054(10) -0.006(7) 0.025(8) -0.012(7) C11 0.093(12) 0.063(10) 0.034(9) -0.010(8) 0.022(8) -0.003(9) C12 0.081(10) 0.058(9) 0.036(9) -0.006(7) 0.026(8) -0.006(8) C13 0.054(8) 0.060(9) 0.037(8) -0.001(7) 0.017(7) 0.004(7) C14 0.039(7) 0.047(8) 0.032(8) -0.009(6) 0.010(6) 0.000(6) C15 0.23(3) 0.088(15) 0.048(11) -0.030(10) 0.036(14) -0.061(16) C16 0.18(2) 0.093(14) 0.055(11) 0.012(10) 0.058(13) -0.023(14) C17 0.037(7) 0.037(7) 0.045(8) -0.008(6) 0.016(6) 0.000(6) C18 0.035(7) 0.050(8) 0.059(9) -0.026(7) 0.001(6) -0.003(6) C19 0.055(9) 0.050(9) 0.072(11) -0.036(8) 0.006(8) 0.004(7) C20 0.035(7) 0.045(8) 0.053(9) -0.007(7) 0.000(6) 0.003(6) C21 0.038(7) 0.036(7) 0.040(8) 0.003(6) 0.009(6) -0.005(6) C22 0.029(6) 0.033(7) 0.040(7) -0.008(6) 0.013(6) -0.003(5) C23 0.111(17) 0.092(16) 0.24(3) -0.116(19) -0.092(18) 0.038(13) C24 0.059(10) 0.062(10) 0.098(14) -0.014(10) -0.016(9) 0.023(8) C25 0.034(6) 0.032(7) 0.043(7) 0.004(6) 0.018(6) 0.007(5) C26 0.067(9) 0.049(8) 0.083(11) 0.011(8) 0.052(9) 0.008(7) C27 0.087(11) 0.037(8) 0.090(12) 0.009(8) 0.053(10) 0.017(8) C28 0.062(9) 0.051(9) 0.083(11) 0.008(8) 0.046(9) 0.014(7) C29 0.052(8) 0.038(7) 0.046(8) 0.010(6) 0.016(7) 0.008(6) C30 0.034(6) 0.030(6) 0.039(7) -0.005(5) 0.013(6) 0.003(5) C31 0.30(4) 0.116(18) 0.28(4) 0.14(2) 0.24(3) 0.13(2) C32 0.19(2) 0.075(13) 0.24(3) 0.056(16) 0.18(2) 0.065(14) C33 0.028(6) 0.040(7) 0.034(7) -0.008(6) 0.007(5) -0.011(5) C34 0.055(8) 0.041(7) 0.052(8) -0.019(6) 0.026(7) -0.015(6) C35 0.042(7) 0.055(8) 0.065(9) -0.030(7) 0.027(7) -0.025(7) C36 0.038(7) 0.062(9) 0.057(9) -0.026(7) 0.021(7) -0.014(7) C37 0.038(7) 0.042(7) 0.041(8) -0.016(6) 0.016(6) -0.010(6) C38 0.027(6) 0.028(6) 0.040(7) -0.004(5) 0.012(5) -0.007(5) C39 0.081(12) 0.125(16) 0.151(19) -0.110(15) 0.068(13) -0.069(12) C40 0.104(15) 0.16(2) 0.19(2) -0.121(18) 0.125(17) -0.088(14) C41 0.032(6) 0.054(8) 0.032(7) -0.005(6) 0.011(6) 0.003(6) C42 0.038(7) 0.086(11) 0.030(7) 0.000(7) 0.003(6) 0.019(7) C43 0.035(7) 0.115(13) 0.037(8) 0.001(8) 0.006(6) 0.020(8) C44 0.039(7) 0.096(11) 0.036(8) 0.008(8) 0.010(6) 0.011(7) C45 0.030(6) 0.067(9) 0.035(8) -0.005(7) 0.004(6) -0.003(6) C46 0.034(6) 0.039(7) 0.030(7) -0.006(5) 0.014(6) -0.008(5) C47 0.045(10) 0.24(3) 0.046(10) -0.013(14) -0.015(8) 0.055(13) C48 0.062(11) 0.25(3) 0.047(10) 0.026(14) 0.025(9) 0.050(14) _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 Fe1 N18 2.005(8) . ? Fe1 N18 2.005(8) 3_655 ? Fe1 N15 2.020(8) 3_655 ? Fe1 N15 2.020(8) . ? Fe1 N12 2.026(9) . ? Fe1 N12 2.026(9) 3_655 ? Fe2 N11 2.125(9) . ? Fe2 N17 2.143(9) . ? Fe2 N14 2.165(9) . ? Fe2 N8 2.182(9) . ? Fe2 N5 2.201(9) . ? Fe2 N2 2.219(8) . ? Zn1 N1 2.019(10) . ? Zn1 N6 2.032(9) . ? Zn1 N10 2.040(9) . ? Zn1 Cl1 2.134(4) . ? Zn2 N13 1.992(9) . ? Zn2 N4 2.014(10) . ? Zn2 N7 2.061(10) . ? Zn2 Cl2 2.148(4) . ? Zn3 N3 1.990(9) . ? Zn3 N16 2.010(9) . ? Zn3 N9 2.018(9) . ? Zn3 Cl3 2.165(4) . ? N1 N2 1.342(12) . ? N1 C1 1.384(14) . ? N2 N3 1.346(12) . ? N3 C6 1.372(13) . ? N4 C9 1.336(15) . ? N4 N5 1.365(13) . ? N5 N6 1.307(12) . ? N6 C14 1.357(14) . ? N7 N8 1.329(13) . ? N7 C17 1.346(15) . ? N8 N9 1.334(13) . ? N9 C22 1.348(14) . ? N10 N11 1.346(12) . ? N10 C25 1.356(14) . ? N11 N12 1.338(12) . ? N12 C30 1.385(14) . ? N13 N14 1.348(12) . ? N13 C33 1.357(13) . ? N14 N15 1.321(11) . ? N15 C38 1.369(13) . ? N16 N17 1.350(12) . ? N16 C41 1.376(14) . ? N17 N18 1.339(11) . ? N18 C46 1.375(14) . ? O1 C3 1.366(14) . ? O1 C7 1.417(17) . ? O2 C4 1.370(13) . ? O2 C8 1.418(15) . ? O3 C11 1.353(16) . ? O3 C15 1.43(2) . ? O4 C12 1.357(16) . ? O4 C16 1.46(2) . ? O5 C20 1.371(15) . ? O5 C24 1.419(17) . ? O6 C19 1.360(15) . ? O6 C23 1.443(19) . ? O7 C28 1.373(15) . ? O7 C32 1.443(18) . ? O8 C27 1.363(16) . ? O8 C31 1.44(2) . ? O9 C35 1.346(14) . ? O9 C39 1.455(17) . ? O10 C36 1.355(14) . ? O10 C40 1.436(17) . ? O11 C43 1.362(16) . ? O11 C47 1.427(17) . ? O12 C44 1.351(15) . ? O12 C48 1.428(17) . ? C1 C6 1.362(16) . ? C1 C2 1.394(16) . ? C2 C3 1.351(17) . ? C3 C4 1.445(17) . ? C4 C5 1.345(16) . ? C5 C6 1.404(16) . ? C9 C10 1.358(17) . ? C9 C14 1.393(17) . ? C10 C11 1.394(19) . ? C11 C12 1.44(2) . ? C12 C13 1.345(18) . ? C13 C14 1.373(17) . ? C17 C22 1.385(16) . ? C17 C18 1.406(17) . ? C18 C19 1.328(19) . ? C19 C20 1.438(18) . ? C20 C21 1.363(17) . ? C21 C22 1.381(16) . ? C25 C30 1.365(15) . ? C25 C26 1.375(17) . ? C26 C27 1.348(18) . ? C27 C28 1.443(19) . ? C28 C29 1.374(17) . ? C29 C30 1.388(16) . ? C33 C38 1.379(15) . ? C33 C34 1.415(16) . ? C34 C35 1.350(16) . ? C35 C36 1.447(17) . ? C36 C37 1.346(16) . ? C37 C38 1.389(15) . ? C41 C46 1.378(15) . ? C41 C42 1.383(17) . ? C42 C43 1.367(18) . ? C43 C44 1.416(17) . ? C44 C45 1.365(17) . ? C45 C46 1.404(16) . ? 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 N18 Fe1 N18 180 . 3_655 ? N18 Fe1 N15 86.4(3) . 3_655 ? N18 Fe1 N15 93.6(3) 3_655 3_655 ? N18 Fe1 N15 93.6(3) . . ? N18 Fe1 N15 86.4(3) 3_655 . ? N15 Fe1 N15 180 3_655 . ? N18 Fe1 N12 93.1(3) . . ? N18 Fe1 N12 86.9(3) 3_655 . ? N15 Fe1 N12 86.4(3) 3_655 . ? N15 Fe1 N12 93.6(3) . . ? N18 Fe1 N12 86.9(3) . 3_655 ? N18 Fe1 N12 93.1(3) 3_655 3_655 ? N15 Fe1 N12 93.6(3) 3_655 3_655 ? N15 Fe1 N12 86.4(3) . 3_655 ? N12 Fe1 N12 180 . 3_655 ? N11 Fe2 N17 88.1(3) . . ? N11 Fe2 N14 88.7(3) . . ? N17 Fe2 N14 87.6(3) . . ? N11 Fe2 N8 178.8(4) . . ? N17 Fe2 N8 90.7(4) . . ? N14 Fe2 N8 91.3(3) . . ? N11 Fe2 N5 90.6(4) . . ? N17 Fe2 N5 178.7(4) . . ? N14 Fe2 N5 92.6(3) . . ? N8 Fe2 N5 90.6(4) . . ? N11 Fe2 N2 91.8(3) . . ? N17 Fe2 N2 91.3(3) . . ? N14 Fe2 N2 178.8(4) . . ? N8 Fe2 N2 88.2(3) . . ? N5 Fe2 N2 88.5(3) . . ? N1 Zn1 N6 98.8(4) . . ? N1 Zn1 N10 98.5(4) . . ? N6 Zn1 N10 100.3(4) . . ? N1 Zn1 Cl1 115.9(3) . . ? N6 Zn1 Cl1 121.5(3) . . ? N10 Zn1 Cl1 117.7(3) . . ? N13 Zn2 N4 101.0(4) . . ? N13 Zn2 N7 98.4(4) . . ? N4 Zn2 N7 98.3(4) . . ? N13 Zn2 Cl2 122.5(3) . . ? N4 Zn2 Cl2 120.3(3) . . ? N7 Zn2 Cl2 111.7(3) . . ? N3 Zn3 N16 99.6(4) . . ? N3 Zn3 N9 100.6(4) . . ? N16 Zn3 N9 100.8(4) . . ? N3 Zn3 Cl3 115.9(3) . . ? N16 Zn3 Cl3 116.6(3) . . ? N9 Zn3 Cl3 120.1(3) . . ? N2 N1 C1 106.0(9) . . ? N2 N1 Zn1 118.7(7) . . ? C1 N1 Zn1 135.2(8) . . ? N1 N2 N3 111.1(8) . . ? N1 N2 Fe2 123.5(7) . . ? N3 N2 Fe2 124.8(7) . . ? N2 N3 C6 106.7(9) . . ? N2 N3 Zn3 117.3(6) . . ? C6 N3 Zn3 135.7(8) . . ? C9 N4 N5 106.4(9) . . ? C9 N4 Zn2 134.0(8) . . ? N5 N4 Zn2 119.4(7) . . ? N6 N5 N4 110.8(9) . . ? N6 N5 Fe2 126.7(7) . . ? N4 N5 Fe2 122.5(7) . . ? N5 N6 C14 107.9(9) . . ? N5 N6 Zn1 116.7(7) . . ? C14 N6 Zn1 135.0(8) . . ? N8 N7 C17 107.4(9) . . ? N8 N7 Zn2 119.6(7) . . ? C17 N7 Zn2 133.0(8) . . ? N7 N8 N9 110.1(8) . . ? N7 N8 Fe2 123.0(7) . . ? N9 N8 Fe2 126.9(7) . . ? N8 N9 C22 108.0(9) . . ? N8 N9 Zn3 115.9(7) . . ? C22 N9 Zn3 136.0(8) . . ? N11 N10 C25 107.7(8) . . ? N11 N10 Zn1 119.2(7) . . ? C25 N10 Zn1 133.0(8) . . ? N12 N11 N10 110.4(8) . . ? N12 N11 Fe2 125.0(7) . . ? N10 N11 Fe2 124.5(6) . . ? N11 N12 C30 106.2(8) . . ? N11 N12 Fe1 124.4(7) . . ? C30 N12 Fe1 129.4(7) . . ? N14 N13 C33 106.8(8) . . ? N14 N13 Zn2 119.6(7) . . ? C33 N13 Zn2 133.6(8) . . ? N15 N14 N13 110.4(8) . . ? N15 N14 Fe2 125.8(7) . . ? N13 N14 Fe2 123.8(7) . . ? N14 N15 C38 108.0(8) . . ? N14 N15 Fe1 123.5(6) . . ? C38 N15 Fe1 128.5(7) . . ? N17 N16 C41 107.2(8) . . ? N17 N16 Zn3 119.6(7) . . ? C41 N16 Zn3 133.2(7) . . ? N18 N17 N16 111.0(8) . . ? N18 N17 Fe2 125.4(7) . . ? N16 N17 Fe2 123.6(6) . . ? N17 N18 C46 106.3(8) . . ? N17 N18 Fe1 124.0(7) . . ? C46 N18 Fe1 129.7(7) . . ? C3 O1 C7 114.9(10) . . ? C4 O2 C8 116.3(10) . . ? C11 O3 C15 117.2(12) . . ? C12 O4 C16 115.5(12) . . ? C20 O5 C24 114.9(10) . . ? C19 O6 C23 115.0(12) . . ? C28 O7 C32 117.2(11) . . ? C27 O8 C31 115.8(12) . . ? C35 O9 C39 115.5(10) . . ? C36 O10 C40 116.1(10) . . ? C43 O11 C47 116.0(11) . . ? C44 O12 C48 116.0(11) . . ? C6 C1 N1 108.3(9) . . ? C6 C1 C2 122.9(11) . . ? N1 C1 C2 128.8(11) . . ? C3 C2 C1 116.1(12) . . ? C2 C3 O1 125.3(12) . . ? C2 C3 C4 121.5(11) . . ? O1 C3 C4 113.3(10) . . ? C5 C4 O2 125.7(11) . . ? C5 C4 C3 121.3(11) . . ? O2 C4 C3 113.0(10) . . ? C4 C5 C6 116.8(11) . . ? C1 C6 N3 107.8(10) . . ? C1 C6 C5 121.4(10) . . ? N3 C6 C5 130.7(11) . . ? N4 C9 C10 129.6(12) . . ? N4 C9 C14 108.1(10) . . ? C10 C9 C14 122.3(12) . . ? C9 C10 C11 116.8(13) . . ? O3 C11 C10 125.4(14) . . ? O3 C11 C12 114.2(12) . . ? C10 C11 C12 120.4(13) . . ? O4 C12 C13 126.6(13) . . ? O4 C12 C11 112.6(12) . . ? C13 C12 C11 120.8(13) . . ? C12 C13 C14 118.2(13) . . ? N6 C14 C9 106.8(11) . . ? N6 C14 C13 131.7(12) . . ? C9 C14 C13 121.4(12) . . ? N7 C17 C22 107.9(10) . . ? N7 C17 C18 130.3(11) . . ? C22 C17 C18 121.8(11) . . ? C19 C18 C17 116.5(12) . . ? C18 C19 O6 124.6(13) . . ? C18 C19 C20 121.8(12) . . ? O6 C19 C20 113.6(12) . . ? C21 C20 O5 124.8(11) . . ? C21 C20 C19 122.0(12) . . ? O5 C20 C19 113.1(11) . . ? C20 C21 C22 115.9(11) . . ? N9 C22 C17 106.6(10) . . ? N9 C22 C21 131.4(11) . . ? C17 C22 C21 122.0(11) . . ? N10 C25 C30 107.5(10) . . ? N10 C25 C26 130.0(11) . . ? C30 C25 C26 122.5(10) . . ? C27 C26 C25 118.0(12) . . ? C26 C27 O8 126.0(13) . . ? C26 C27 C28 120.0(13) . . ? O8 C27 C28 114.0(12) . . ? C29 C28 O7 124.4(12) . . ? C29 C28 C27 121.3(12) . . ? O7 C28 C27 114.3(12) . . ? C28 C29 C30 116.5(11) . . ? C25 C30 N12 108.1(9) . . ? C25 C30 C29 121.6(11) . . ? N12 C30 C29 130.3(11) . . ? N13 C33 C38 108.1(9) . . ? N13 C33 C34 129.3(10) . . ? C38 C33 C34 122.6(10) . . ? C35 C34 C33 116.0(11) . . ? O9 C35 C34 125.4(11) . . ? O9 C35 C36 113.0(10) . . ? C34 C35 C36 121.6(11) . . ? C37 C36 O10 125.3(11) . . ? C37 C36 C35 121.0(11) . . ? O10 C36 C35 113.7(10) . . ? C36 C37 C38 118.2(11) . . ? N15 C38 C33 106.6(9) . . ? N15 C38 C37 132.8(10) . . ? C33 C38 C37 120.6(10) . . ? N16 C41 C46 106.8(10) . . ? N16 C41 C42 129.2(10) . . ? C46 C41 C42 124.0(11) . . ? C43 C42 C41 115.1(11) . . ? O11 C43 C42 123.3(12) . . ? O11 C43 C44 114.1(12) . . ? C42 C43 C44 122.7(12) . . ? O12 C44 C45 125.1(11) . . ? O12 C44 C43 114.0(12) . . ? C45 C44 C43 120.8(12) . . ? C44 C45 C46 117.3(11) . . ? N18 C46 C41 108.7(9) . . ? N18 C46 C45 131.4(10) . . ? C41 C46 C45 119.9(11) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 24.02 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 2.362 _refine_diff_density_min -0.693 _refine_diff_density_rms 0.229