# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Wenbin Lin' _publ_contact_author_email wlin@unc.edu _publ_section_title ; A Chiral Metal-Organic Framework for Tandem Asymmetric Catalysis ; loop_ _publ_author_name 'Wenbin Lin' 'Feijie Song' 'Cheng Wang' # Attachment '- CMOF1.cif' data_cmof1 _database_code_depnum_ccdc_archive 'CCDC 806227' #TrackingRef '- CMOF1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C552 Cl12 Mn12 N24 O76 Zn16' _chemical_formula_weight 10312.36 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' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn -0.5299 2.8052 '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' Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M R3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' _cell_length_a 77.9421(3) _cell_length_b 77.9421(3) _cell_length_c 47.734(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 251133(11) _cell_formula_units_Z 3 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description hexagonal _exptl_crystal_colour brown _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.205 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 15216 _exptl_absorpt_coefficient_mu 0.654 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7799 _exptl_absorpt_correction_T_max 0.7799 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 70530 _diffrn_reflns_av_R_equivalents 0.0442 _diffrn_reflns_av_sigmaI/netI 0.1378 _diffrn_reflns_limit_h_min -41 _diffrn_reflns_limit_h_max 51 _diffrn_reflns_limit_k_min -54 _diffrn_reflns_limit_k_max 45 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.13 _diffrn_reflns_theta_max 33.41 _reflns_number_total 36814 _reflns_number_gt 18875 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.295(12) _refine_ls_number_reflns 36814 _refine_ls_number_parameters 501 _refine_ls_number_restraints 829 _refine_ls_R_factor_all 0.1298 _refine_ls_R_factor_gt 0.0982 _refine_ls_wR_factor_ref 0.2943 _refine_ls_wR_factor_gt 0.2656 _refine_ls_goodness_of_fit_ref 0.837 _refine_ls_restrained_S_all 0.849 _refine_ls_shift/su_max 0.003 _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 C1A C 0.6806(3) 0.4550(2) 0.7898(3) 0.356 Uiso 1 1 d GDU . . C2A C 0.6695(2) 0.4580(2) 0.7696(3) 0.341 Uiso 1 1 d GDU . . C3A C 0.6766(2) 0.4767(3) 0.7579(3) 0.352 Uiso 1 1 d GDU . . C4A C 0.6947(3) 0.4924(2) 0.7665(3) 0.343 Uiso 1 1 d GDU . . C5A C 0.7058(2) 0.4894(2) 0.7867(3) 0.333 Uiso 1 1 d GDU . . C6A C 0.6987(3) 0.4707(3) 0.7984(3) 0.342 Uiso 1 1 d GDU . . C7A C 0.6780(3) 0.3705(3) 0.8907(3) 0.224 Uiso 1 1 d DU . . C8A C 0.7254(3) 0.5084(3) 0.7950(5) 0.358 Uiso 1 1 d DU . . C9A C 0.7216(3) 0.5225(3) 0.8061(4) 0.304 Uiso 1 1 d DU . . C15A C 0.6839(3) 0.4181(3) 0.8413(3) 0.353 Uiso 1 1 d GDU . . C16A C 0.6995(2) 0.4210(2) 0.8585(4) 0.321 Uiso 1 1 d GDU . . C17A C 0.6979(2) 0.4055(3) 0.8748(3) 0.324 Uiso 1 1 d GDU . . C18A C 0.6808(3) 0.3871(3) 0.8739(3) 0.271 Uiso 1 1 d GDU . . C19A C 0.6651(2) 0.3842(2) 0.8567(4) 0.324 Uiso 1 1 d GDU . . C20A C 0.6667(2) 0.3997(3) 0.8404(3) 0.311 Uiso 1 1 d GDU . . C10A C 0.7347(4) 0.5022(4) 0.8160(6) 0.408 Uiso 1 1 d DU . . C11A C 0.7403(3) 0.5170(4) 0.7739(5) 0.339 Uiso 1 1 d DU . . C12A C 0.6637(3) 0.4782(3) 0.7379(4) 0.372 Uiso 1 1 d DU . . C1B C 0.7170(3) 0.5932(2) 0.6834(3) 0.404 Uiso 1 1 d GDU . . C2B C 0.7025(2) 0.5743(3) 0.6757(3) 0.380 Uiso 1 1 d GDU . . C3B C 0.70030(19) 0.5579(2) 0.6903(3) 0.357 Uiso 1 1 d GDU . . C4B C 0.7127(2) 0.5605(2) 0.7128(3) 0.372 Uiso 1 1 d GDU . . C5B C 0.7273(2) 0.5794(3) 0.7206(3) 0.359 Uiso 1 1 d GDU . . C6B C 0.7295(2) 0.5958(2) 0.7059(4) 0.371 Uiso 1 1 d GDU . . C13A C 0.6723(3) 0.4343(3) 0.8019(4) 0.373 Uiso 1 1 d DU . . C14A C 0.6856(4) 0.4351(3) 0.8232(4) 0.387 Uiso 1 1 d DU . . C15B C 0.7362(3) 0.6497(3) 0.6524(3) 0.361 Uiso 1 1 d GDU . . C16B C 0.7234(2) 0.6470(2) 0.6304(4) 0.334 Uiso 1 1 d GDU . . C17B C 0.7255(2) 0.6634(3) 0.6157(3) 0.329 Uiso 1 1 d GDU . . C18B C 0.7404(3) 0.6823(3) 0.6230(3) 0.311 Uiso 1 1 d GDU . . C19B C 0.7531(2) 0.6849(2) 0.6450(4) 0.324 Uiso 1 1 d GDU . . C20B C 0.7510(2) 0.6686(3) 0.6597(3) 0.347 Uiso 1 1 d GDU . . C7B C 0.7420(2) 0.6978(2) 0.6061(3) 0.205 Uiso 1 1 d DU . . C8B C 0.7424(3) 0.5840(3) 0.7457(4) 0.323 Uiso 1 1 d DU . . C9B C 0.7481(4) 0.6034(4) 0.7565(5) 0.368 Uiso 1 1 d DU . . C1D C 0.63334(18) 0.6061(2) 0.6872(3) 0.348 Uiso 1 1 d GDU . . C2D C 0.63596(19) 0.5972(2) 0.6636(4) 0.410 Uiso 1 1 d GDU . . C3D C 0.63332(19) 0.6029(2) 0.6371(3) 0.379 Uiso 1 1 d GDU . . C4D C 0.62806(19) 0.6174(2) 0.6341(3) 0.374 Uiso 1 1 d GDU . . C5D C 0.62544(19) 0.62627(19) 0.6578(4) 0.311 Uiso 1 1 d GDU . . C6D C 0.62808(19) 0.6206(2) 0.6843(3) 0.324 Uiso 1 1 d GDU . . C10B C 0.7612(3) 0.5868(4) 0.7355(5) 0.340 Uiso 1 1 d DU . . C11B C 0.7355(4) 0.5697(3) 0.7677(4) 0.403 Uiso 1 1 d DU . . C12B C 0.6842(3) 0.5394(2) 0.6797(4) 0.331 Uiso 1 1 d DU . . C15D C 0.6373(2) 0.6034(3) 0.7710(3) 0.397 Uiso 1 1 d GDU . . C16D C 0.6332(2) 0.6103(2) 0.7955(5) 0.359 Uiso 1 1 d GDU . . C17D C 0.6356(2) 0.6035(3) 0.8214(4) 0.343 Uiso 1 1 d GDU . . C18D C 0.64193(19) 0.5898(2) 0.8227(3) 0.295 Uiso 1 1 d GDU . . C19D C 0.6460(2) 0.5828(2) 0.7982(5) 0.303 Uiso 1 1 d GDU . . C20D C 0.6436(2) 0.5896(3) 0.7723(4) 0.355 Uiso 1 1 d GDU . . C13B C 0.7188(3) 0.6112(3) 0.6665(4) 0.374 Uiso 1 1 d DU . . C14B C 0.7339(3) 0.6313(3) 0.6694(4) 0.355 Uiso 1 1 d DU . . C1E C 0.6159(2) 0.6372(2) 0.4693(3) 0.405 Uiso 1 1 d GDU . . C2E C 0.6247(2) 0.6265(2) 0.4783(4) 0.396 Uiso 1 1 d GDU . . C3E C 0.62704(19) 0.62449(19) 0.5067(4) 0.380 Uiso 1 1 d GDU . . C4E C 0.6205(2) 0.6332(2) 0.5262(3) 0.399 Uiso 1 1 d GDU . . C5E C 0.6117(2) 0.6439(2) 0.5173(4) 0.387 Uiso 1 1 d GDU . . C6E C 0.6094(2) 0.6460(2) 0.4888(4) 0.402 Uiso 1 1 d GDU . . C1C C 0.6550(3) 0.4893(3) 0.6962(4) 0.358 Uiso 1 1 d DU . . C2C C 0.6373(3) 0.4682(3) 0.6876(5) 0.330 Uiso 1 1 d DU . . C3C C 0.6239(3) 0.4679(4) 0.6660(5) 0.334 Uiso 1 1 d DU . . C15E C 0.59836(19) 0.6510(3) 0.3959(3) 0.373 Uiso 1 1 d GDU . . C16E C 0.5913(2) 0.6639(3) 0.3912(4) 0.377 Uiso 1 1 d GDU . . C17E C 0.5866(2) 0.6669(2) 0.3642(5) 0.345 Uiso 1 1 d GDU . . C18E C 0.5889(2) 0.6568(3) 0.3419(3) 0.346 Uiso 1 1 d GDU . . C19E C 0.5960(3) 0.6438(3) 0.3465(4) 0.348 Uiso 1 1 d GDU . . C20E C 0.6007(2) 0.6409(2) 0.3735(5) 0.406 Uiso 1 1 d GDU . . C4C C 0.6328(4) 0.4834(4) 0.6448(5) 0.364 Uiso 1 1 d DU . . C5C C 0.6508(3) 0.5037(3) 0.6505(4) 0.345 Uiso 1 1 d DU . . C6C C 0.6657(3) 0.5028(3) 0.6747(4) 0.352 Uiso 1 1 d DU . . C1G C 0.4755(2) 0.6960(2) 0.3686(3) 0.353 Uiso 1 1 d GDU . . C2G C 0.4951(3) 0.7086(2) 0.3610(3) 0.365 Uiso 1 1 d GDU . . C3G C 0.5103(2) 0.70916(19) 0.3769(3) 0.331 Uiso 1 1 d GDU . . C4G C 0.5059(2) 0.6972(2) 0.4005(3) 0.335 Uiso 1 1 d GDU . . C5G C 0.4863(3) 0.6846(2) 0.4081(3) 0.337 Uiso 1 1 d GDU . . C6G C 0.4711(2) 0.6840(2) 0.3922(4) 0.331 Uiso 1 1 d GDU . . N1C N 0.6673(2) 0.4916(3) 0.7183(4) 0.359 Uiso 1 1 d DU . . N2C N 0.6805(2) 0.5211(2) 0.6862(3) 0.305 Uiso 1 1 d DU . . C15G C 0.4208(3) 0.6803(3) 0.3447(4) 0.357 Uiso 1 1 d GDU . . C16G C 0.4012(3) 0.6680(2) 0.3527(3) 0.370 Uiso 1 1 d GDU . . C17G C 0.3860(2) 0.6678(2) 0.3371(4) 0.308 Uiso 1 1 d GDU . . C18G C 0.3904(3) 0.6798(3) 0.3136(3) 0.285 Uiso 1 1 d GDU . . C19G C 0.4100(3) 0.6921(2) 0.3057(3) 0.304 Uiso 1 1 d GDU . . C20G C 0.4252(2) 0.6924(2) 0.3213(4) 0.301 Uiso 1 1 d GDU . . Mn1 Mn 0.69349(8) 0.51718(8) 0.71944(10) 0.303 Uiso 1 1 d DU . . Cl1 Cl 0.71723(11) 0.51325(12) 0.69600(16) 0.340 Uiso 1 1 d DU . . C1H C 0.6070(2) 0.7101(2) 0.4748(4) 0.360 Uiso 1 1 d GDU . . C2H C 0.6062(2) 0.71671(18) 0.4481(4) 0.320 Uiso 1 1 d GDU . . C3H C 0.5882(3) 0.71270(19) 0.4368(3) 0.354 Uiso 1 1 d GDU . . C4H C 0.5709(2) 0.7021(2) 0.4522(3) 0.339 Uiso 1 1 d GDU . . C5H C 0.5717(2) 0.69542(18) 0.4790(3) 0.282 Uiso 1 1 d GDU . . C6H C 0.5897(3) 0.6994(2) 0.4903(3) 0.352 Uiso 1 1 d GDU . . O1A O 0.6585(2) 0.3547(2) 0.8936(3) 0.223 Uiso 1 1 d DU . . O2A O 0.69635(15) 0.37387(14) 0.90125(18) 0.136 Uiso 1 1 d DU . . O3A O 0.7026(2) 0.5110(2) 0.7548(3) 0.344 Uiso 1 1 d DU . . C15H C 0.6487(2) 0.7143(2) 0.5280(4) 0.340 Uiso 1 1 d GDU . . C16H C 0.6508(2) 0.70906(18) 0.5550(4) 0.308 Uiso 1 1 d GDU . . C17H C 0.6695(3) 0.7140(2) 0.5651(3) 0.269 Uiso 1 1 d GDU . . C18H C 0.6860(2) 0.7241(2) 0.5480(4) 0.322 Uiso 1 1 d GDU . . C19H C 0.6839(3) 0.7293(2) 0.5209(4) 0.352 Uiso 1 1 d GDU . . C20H C 0.6653(3) 0.7244(2) 0.5109(3) 0.359 Uiso 1 1 d GDU . . O1B O 0.73113(14) 0.70582(14) 0.60217(18) 0.135 Uiso 1 1 d DU . . O2B O 0.75852(15) 0.70788(14) 0.58725(19) 0.138 Uiso 1 1 d DU . . O3B O 0.7120(2) 0.5441(2) 0.7264(3) 0.335 Uiso 1 1 d DU . . C1J C -0.0780(2) 0.82735(19) 0.5641(4) 0.396 Uiso 1 1 d GDU . . C2J C -0.0662(3) 0.8327(2) 0.5403(3) 0.372 Uiso 1 1 d GDU . . C3J C -0.0456(3) 0.8431(2) 0.5430(3) 0.404 Uiso 1 1 d GDU . . C4J C -0.0370(2) 0.8482(2) 0.5694(4) 0.410 Uiso 1 1 d GDU . . C5J C -0.0489(3) 0.8428(2) 0.5931(3) 0.399 Uiso 1 1 d GDU . . C6J C -0.0694(3) 0.8324(2) 0.5905(3) 0.355 Uiso 1 1 d GDU . . C7D C 0.6452(2) 0.58057(17) 0.8473(3) 0.205 Uiso 1 1 d DU . . C8D C 0.6200(3) 0.6426(3) 0.6545(5) 0.352 Uiso 1 1 d DU . . C9D C 0.6005(4) 0.6335(4) 0.6435(6) 0.422 Uiso 1 1 d DU . . C15J C -0.1344(2) 0.80046(19) 0.5838(5) 0.378 Uiso 1 1 d GDU . . C16J C -0.1450(3) 0.7962(3) 0.6087(4) 0.369 Uiso 1 1 d GDU . . C17J C -0.1656(3) 0.7854(3) 0.6082(3) 0.377 Uiso 1 1 d GDU . . C18J C -0.1755(2) 0.77886(19) 0.5829(5) 0.302 Uiso 1 1 d GDU . . C19J C -0.1649(3) 0.7831(3) 0.5580(3) 0.361 Uiso 1 1 d GDU . . C20J C -0.1443(3) 0.7939(3) 0.5584(4) 0.385 Uiso 1 1 d GDU . . C10D C 0.6203(5) 0.6498(4) 0.6820(5) 0.418 Uiso 1 1 d DU . . C11D C 0.6343(4) 0.6596(3) 0.6408(5) 0.349 Uiso 1 1 d DU . . C12D C 0.6360(3) 0.5924(3) 0.6144(4) 0.419 Uiso 1 1 d DU . . C1K C 0.0836(2) 0.9063(2) 0.5578(4) 0.400 Uiso 1 1 d GDU . . C2K C 0.0711(3) 0.8953(2) 0.5360(3) 0.403 Uiso 1 1 d GDU . . C3K C 0.0507(3) 0.8845(2) 0.5403(3) 0.412 Uiso 1 1 d GDU . . C4K C 0.0429(2) 0.8847(2) 0.5664(4) 0.402 Uiso 1 1 d GDU . . C5K C 0.0554(3) 0.8957(3) 0.5882(3) 0.438 Uiso 1 1 d GDU . . C6K C 0.0757(3) 0.9065(2) 0.5839(4) 0.417 Uiso 1 1 d GDU . . C13D C 0.6361(3) 0.6001(3) 0.7169(4) 0.364 Uiso 1 1 d DU . . C14D C 0.6350(3) 0.6102(3) 0.7408(4) 0.425 Uiso 1 1 d DU . . C15K C 0.1430(2) 0.9389(2) 0.5705(5) 0.407 Uiso 1 1 d GDU . . C16K C 0.1533(3) 0.9505(3) 0.5933(4) 0.420 Uiso 1 1 d GDU . . C17K C 0.1738(3) 0.9623(3) 0.5921(4) 0.407 Uiso 1 1 d GDU . . C18K C 0.1840(2) 0.9625(2) 0.5680(5) 0.353 Uiso 1 1 d GDU . . C19K C 0.1736(3) 0.9509(3) 0.5451(3) 0.414 Uiso 1 1 d GDU . . C20K C 0.1531(3) 0.9391(3) 0.5464(4) 0.386 Uiso 1 1 d GDU . . C4I C 0.5985(4) 0.7502(4) 0.3264(5) 0.373 Uiso 1 1 d DU . . C5I C 0.5994(3) 0.7395(4) 0.3529(5) 0.349 Uiso 1 1 d DU . . C6I C 0.5766(3) 0.7250(3) 0.3643(4) 0.303 Uiso 1 1 d DU . . C7E C 0.58461(19) 0.66034(15) 0.3133(4) 0.206 Uiso 1 1 d DU . . C8E C 0.6032(3) 0.6516(3) 0.5411(4) 0.341 Uiso 1 1 d DU . . C9E C 0.5858(3) 0.6330(3) 0.5526(5) 0.330 Uiso 1 1 d DU . . C10E C 0.5951(5) 0.6622(4) 0.5279(6) 0.420 Uiso 1 1 d DU . . C11E C 0.6153(3) 0.6628(2) 0.5629(5) 0.349 Uiso 1 1 d DU . . C12E C 0.6365(3) 0.6125(3) 0.5132(4) 0.359 Uiso 1 1 d DU . . C13E C 0.6142(3) 0.6390(3) 0.4365(4) 0.372 Uiso 1 1 d DU . . C14E C 0.6034(3) 0.6476(3) 0.4260(4) 0.396 Uiso 1 1 d DU . . C1F C 0.6461(4) 0.5888(3) 0.5690(5) 0.402 Uiso 1 1 d DU . . C2F C 0.6608(4) 0.5813(4) 0.5792(5) 0.372 Uiso 1 1 d DU . . C3F C 0.6702(4) 0.5749(4) 0.5576(6) 0.367 Uiso 1 1 d DU . . C4F C 0.6785(4) 0.5893(4) 0.5334(6) 0.363 Uiso 1 1 d DU . . C5F C 0.6637(4) 0.5948(4) 0.5200(4) 0.353 Uiso 1 1 d DU . . C6F C 0.6552(3) 0.6025(3) 0.5466(4) 0.360 Uiso 1 1 d DU . . N1F N 0.6397(4) 0.5974(3) 0.5873(4) 0.420 Uiso 1 1 d DU . . N2F N 0.6425(3) 0.6109(3) 0.5387(3) 0.363 Uiso 1 1 d DU . . Mn2 Mn 0.63549(8) 0.62004(8) 0.57407(12) 0.332 Uiso 1 1 d DU . . Cl2 Cl 0.66445(11) 0.64967(11) 0.57855(16) 0.344 Uiso 1 1 d DU . . O1E O 0.57092(15) 0.66690(14) 0.30962(19) 0.146 Uiso 1 1 d DU . . O2E O 0.59505(18) 0.65659(17) 0.2929(3) 0.195 Uiso 1 1 d DU . . O3E O 0.6216(2) 0.6314(2) 0.5563(3) 0.382 Uiso 1 1 d DU . . O1D O 0.62772(16) 0.57138(14) 0.8628(2) 0.154 Uiso 1 1 d DU . . O2D O 0.66197(15) 0.58188(13) 0.84896(17) 0.127 Uiso 1 1 d DU . . O3D O 0.6247(2) 0.6242(2) 0.6091(3) 0.356 Uiso 1 1 d DU . . C1I C 0.5644(3) 0.7326(3) 0.3626(4) 0.308 Uiso 1 1 d DU . . C2I C 0.5674(4) 0.7478(4) 0.3387(5) 0.377 Uiso 1 1 d DU . . C3I C 0.5886(4) 0.7619(3) 0.3308(6) 0.389 Uiso 1 1 d DU . . N1I N 0.5457(2) 0.7183(3) 0.3730(4) 0.340 Uiso 1 1 d DU . . N2I N 0.5738(2) 0.7164(3) 0.3916(3) 0.318 Uiso 1 1 d DU . . Mn3 Mn 0.54652(8) 0.70247(7) 0.40538(10) 0.301 Uiso 1 1 d DU . . Cl3 Cl 0.53732(12) 0.67188(11) 0.38523(16) 0.336 Uiso 1 1 d DU . . O1H O 0.70502(14) 0.71744(14) 0.57949(19) 0.136 Uiso 1 1 d DU . . O2H O 0.72093(16) 0.74732(16) 0.54620(19) 0.151 Uiso 1 1 d DU . . O3H O 0.5517(2) 0.6963(2) 0.4426(3) 0.345 Uiso 1 1 d DU . . O1G O 0.35710(15) 0.67034(14) 0.31724(19) 0.138 Uiso 1 1 d DU . . O2G O 0.37652(14) 0.68701(13) 0.2738(2) 0.134 Uiso 1 1 d DU . . O3G O 0.5210(2) 0.6975(2) 0.4168(3) 0.362 Uiso 1 1 d DU . . C7G C 0.3734(2) 0.67914(16) 0.2995(3) 0.204 Uiso 1 1 d DU . . C8G C 0.4800(3) 0.6699(3) 0.4333(4) 0.305 Uiso 1 1 d DU . . C9G C 0.4921(3) 0.6625(3) 0.4420(5) 0.324 Uiso 1 1 d DU . . C10G C 0.4627(4) 0.6525(4) 0.4223(6) 0.373 Uiso 1 1 d DU . . C11G C 0.4772(4) 0.6811(4) 0.4546(5) 0.377 Uiso 1 1 d DU . . C12G C 0.5299(3) 0.7207(3) 0.3698(5) 0.358 Uiso 1 1 d DU . . C13G C 0.4576(3) 0.6941(3) 0.3533(4) 0.350 Uiso 1 1 d DU . . C14G C 0.4382(3) 0.6809(3) 0.3616(4) 0.350 Uiso 1 1 d DU . . C7H C 0.7064(2) 0.7301(2) 0.5590(3) 0.203 Uiso 1 1 d DU . . C8H C 0.5513(3) 0.6829(3) 0.4949(4) 0.297 Uiso 1 1 d DU . . C9H C 0.5554(4) 0.6770(4) 0.5212(5) 0.385 Uiso 1 1 d DU . . C10H C 0.5407(3) 0.6921(3) 0.4989(4) 0.307 Uiso 1 1 d DU . . C11H C 0.5392(4) 0.6647(4) 0.4805(6) 0.389 Uiso 1 1 d DU . . C12H C 0.5892(3) 0.7201(3) 0.4087(4) 0.359 Uiso 1 1 d DU . . C13H C 0.6271(3) 0.7150(3) 0.4863(5) 0.394 Uiso 1 1 d DU . . C14H C 0.6288(3) 0.7098(3) 0.5137(5) 0.364 Uiso 1 1 d DU . . C7J C -0.1961(3) 0.7667(2) 0.5848(3) 0.230 Uiso 1 1 d DU . . C8J C -0.0396(4) 0.8487(3) 0.6233(4) 0.355 Uiso 1 1 d DU . . C9J C -0.0311(4) 0.8701(3) 0.6233(6) 0.378 Uiso 1 1 d DU . . C10J C -0.0242(3) 0.8437(3) 0.6267(4) 0.308 Uiso 1 1 d DU . . C11J C -0.0546(4) 0.8391(4) 0.6437(5) 0.384 Uiso 1 1 d DU . . C12J C -0.0355(3) 0.8472(3) 0.5172(4) 0.370 Uiso 1 1 d DU . . C13J C -0.1003(3) 0.8160(3) 0.5624(5) 0.373 Uiso 1 1 d DU . . C14J C -0.1115(3) 0.8128(3) 0.5859(5) 0.383 Uiso 1 1 d DU . . C7K C 0.2051(2) 0.97566(19) 0.5691(3) 0.204 Uiso 1 1 d DU . . C8K C 0.0479(4) 0.8968(3) 0.6186(4) 0.353 Uiso 1 1 d DU . . C9K C 0.0646(4) 0.9060(4) 0.6374(5) 0.399 Uiso 1 1 d DU . . C10K C 0.0356(4) 0.8776(3) 0.6313(5) 0.362 Uiso 1 1 d DU . . C11K C 0.0386(4) 0.9084(4) 0.6190(5) 0.334 Uiso 1 1 d DU . . C12K C 0.0397(3) 0.8741(3) 0.5161(4) 0.374 Uiso 1 1 d DU . . C13K C 0.1066(3) 0.9186(3) 0.5534(5) 0.388 Uiso 1 1 d DU . . C14K C 0.1202(3) 0.9265(3) 0.5749(5) 0.410 Uiso 1 1 d DU . . C1L C -0.0084(3) 0.8536(4) 0.4859(3) 0.351 Uiso 1 1 d DU . . C2L C -0.0201(3) 0.8440(4) 0.4584(4) 0.376 Uiso 1 1 d DU . . C3L C -0.0090(4) 0.8444(5) 0.4330(4) 0.414 Uiso 1 1 d DU . . C4L C 0.0063(4) 0.8389(4) 0.4395(5) 0.396 Uiso 1 1 d DU . . C5L C 0.0224(3) 0.8549(4) 0.4603(4) 0.394 Uiso 1 1 d DU . . C6L C 0.0089(3) 0.8510(4) 0.4896(3) 0.361 Uiso 1 1 d DU . . N1L N -0.0168(3) 0.8524(3) 0.5118(3) 0.357 Uiso 1 1 d DU . . N2L N 0.0207(2) 0.8620(3) 0.5138(3) 0.390 Uiso 1 1 d DU . . Mn4 Mn 0.00131(9) 0.85821(8) 0.54504(12) 0.335 Uiso 1 1 d DU . . Cl4 Cl 0.00074(12) 0.82884(11) 0.55951(16) 0.341 Uiso 1 1 d DU . . O1K O 0.21112(16) 0.98371(16) 0.5954(2) 0.154 Uiso 1 1 d DU . . O2K O 0.21527(14) 0.97726(13) 0.5442(2) 0.134 Uiso 1 1 d DU . . O3K O 0.0221(2) 0.8734(2) 0.5721(3) 0.350 Uiso 1 1 d DU . . O1J O -0.20687(14) 0.77011(13) 0.60287(18) 0.124 Uiso 1 1 d DU . . O2J O -0.20429(14) 0.75040(14) 0.56666(19) 0.137 Uiso 1 1 d DU . . O3J O -0.0159(2) 0.8592(2) 0.5725(3) 0.356 Uiso 1 1 d DU . . Zn1 Zn 0.01104(3) 0.25399(3) 0.54768(5) 0.127 Uiso 1 1 d U . . Zn2 Zn -0.00276(4) 0.22903(3) 0.60341(5) 0.126 Uiso 1 1 d U . . Zn3 Zn -0.00196(3) 0.27017(3) 0.59987(5) 0.127 Uiso 1 1 d U . . Zn4 Zn -0.03340(3) 0.23338(3) 0.56608(5) 0.115 Uiso 1 1 d U . . O1 O -0.01020(15) 0.24391(14) 0.5779(2) 0.140 Uiso 1 1 d U . . Zn5 Zn 0.02702(3) 0.01513(3) 0.57898(5) 0.132 Uiso 1 1 d U . . Zn6 Zn 0.0000 0.0000 0.63276(7) 0.123 Uiso 1 3 d SU . . O2 O 0.0000 0.0000 0.5933(3) 0.154 Uiso 1 3 d SU . . _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 C1A C2A 1.3900 . ? C1A C6A 1.3900 . ? C1A C13A 1.520(15) . ? C2A C3A 1.3900 . ? C3A C4A 1.3900 . ? C3A C12A 1.429(14) . ? C4A C5A 1.3900 . ? C4A O3A 1.382(13) . ? C5A C6A 1.3900 . ? C5A C8A 1.557(15) . ? C7A O2A 1.414(14) . ? C7A O1A 1.403(14) . ? C7A C18A 1.445(13) . ? C7A Zn5 2.265(18) 5 ? C8A C9A 1.386(16) . ? C8A C10A 1.453(17) . ? C8A C11A 1.426(16) . ? C15A C16A 1.3900 . ? C15A C20A 1.3900 . ? C15A C14A 1.528(15) . ? C16A C17A 1.3900 . ? C17A C18A 1.3900 . ? C18A C19A 1.3900 . ? C19A C20A 1.3900 . ? C12A N1C 1.326(15) . ? C1B C2B 1.3900 . ? C1B C6B 1.3900 . ? C1B C13B 1.563(15) . ? C2B C3B 1.3900 . ? C3B C4B 1.3900 . ? C3B C12B 1.452(14) . ? C4B C5B 1.3900 . ? C4B O3B 1.409(13) . ? C5B C6B 1.3900 . ? C5B C8B 1.589(14) . ? C13A C14A 1.432(17) . ? C15B C16B 1.3900 . ? C15B C20B 1.3900 . ? C15B C14B 1.578(14) . ? C16B C17B 1.3900 . ? C17B C18B 1.3900 . ? C18B C19B 1.3900 . ? C18B C7B 1.406(13) . ? C19B C20B 1.3900 . ? C7B O1B 1.291(13) . ? C7B O2B 1.439(13) . ? C8B C11B 1.429(16) . ? C8B C10B 1.460(16) . ? C8B C9B 1.439(16) . ? C1D C2D 1.3900 . ? C1D C6D 1.3900 . ? C1D C13D 1.542(14) . ? C2D C3D 1.3900 . ? C3D C12D 1.436(14) . ? C3D C4D 1.3900 . ? C4D O3D 1.385(13) . ? C4D C5D 1.3900 . ? C5D C6D 1.3900 . ? C5D C8D 1.539(15) . ? C12B N2C 1.343(15) . ? C15D C16D 1.3900 . ? C15D C20D 1.3900 . ? C15D C14D 1.574(15) . ? C16D C17D 1.3900 . ? C17D C18D 1.3900 . ? C18D C19D 1.3900 . ? C18D C7D 1.462(13) . ? C19D C20D 1.3900 . ? C13B C14B 1.416(17) . ? C1E C2E 1.3900 . ? C1E C6E 1.3900 . ? C1E C13E 1.581(15) . ? C2E C3E 1.3900 . ? C3E C4E 1.3900 . ? C3E C12E 1.483(14) . ? C4E C5E 1.3900 . ? C4E O3E 1.448(13) . ? C5E C6E 1.3900 . ? C5E C8E 1.579(14) . ? C1C N1C 1.375(14) . ? C1C C6C 1.405(16) . ? C1C C2C 1.585(15) . ? C2C C3C 1.462(16) . ? C3C C4C 1.456(17) . ? C15E C16E 1.3900 . ? C15E C20E 1.3900 . ? C15E C14E 1.546(14) . ? C16E C17E 1.3900 . ? C17E C18E 1.3900 . ? C18E C19E 1.3900 . ? C18E C7E 1.465(13) . ? C19E C20E 1.3900 . ? C4C C5C 1.529(16) . ? C5C C6C 1.665(15) . ? C6C N2C 1.422(14) . ? C1G C2G 1.3900 . ? C1G C6G 1.3900 . ? C1G C13G 1.513(14) . ? C2G C3G 1.3900 . ? C3G C12G 1.371(14) . ? C3G C4G 1.3900 . ? C4G O3G 1.397(13) . ? C4G C5G 1.3900 . ? C5G C6G 1.3900 . ? C5G C8G 1.562(14) . ? N1C Mn1 2.020(14) . ? N2C Mn1 1.986(13) . ? C15G C16G 1.3900 . ? C15G C20G 1.3900 . ? C15G C14G 1.559(15) . ? C16G C17G 1.3900 . ? C17G C18G 1.3900 . ? C18G C19G 1.3900 . ? C18G C7G 1.461(13) . ? C19G C20G 1.3900 . ? Mn1 O3B 1.891(12) . ? Mn1 O3A 1.981(12) . ? Mn1 Cl1 2.310(8) . ? C1H C2H 1.3900 . ? C1H C6H 1.3900 . ? C1H C13H 1.518(15) . ? C2H C3H 1.3900 . ? C3H C4H 1.3900 . ? C3H C12H 1.446(14) . ? C4H C5H 1.3900 . ? C4H O3H 1.408(13) . ? C5H C6H 1.3900 . ? C5H C8H 1.583(14) . ? O1A Zn5 1.110(13) 5 ? O2A Zn5 1.957(9) 4 ? C15H C16H 1.3900 . ? C15H C20H 1.3900 . ? C15H C14H 1.561(14) . ? C16H C17H 1.3900 . ? C17H C18H 1.3900 . ? C18H C19H 1.3900 . ? C18H C7H 1.506(13) . ? C19H C20H 1.3900 . ? O1B Zn3 1.775(10) 2_665 ? O2B Zn4 2.019(9) 2_665 ? C1J C2J 1.3900 . ? C1J C6J 1.3900 . ? C1J C13J 1.506(15) . ? C2J C3J 1.3900 . ? C3J C12J 1.409(14) . ? C3J C4J 1.3900 . ? C4J O3J 1.432(13) . ? C4J C5J 1.3900 . ? C5J C6J 1.3900 . ? C5J C8J 1.574(15) . ? C7D O2D 1.261(13) . ? C7D O1D 1.395(13) . ? C7D Zn4 2.688(16) 4 ? C8D C11D 1.397(17) . ? C8D C9D 1.418(17) . ? C8D C10D 1.424(17) . ? C15J C16J 1.3900 . ? C15J C20J 1.3900 . ? C15J C14J 1.552(15) . ? C16J C17J 1.3900 . ? C17J C18J 1.3900 . ? C18J C19J 1.3900 . ? C18J C7J 1.396(13) . ? C19J C20J 1.3900 . ? C12D N1F 1.343(15) . ? C1K C2K 1.3900 . ? C1K C6K 1.3900 . ? C1K C13K 1.566(15) . ? C2K C3K 1.3900 . ? C3K C4K 1.3900 . ? C3K C12K 1.425(14) . ? C4K C5K 1.3900 . ? C4K O3K 1.429(13) . ? C5K C6K 1.3900 . ? C5K C8K 1.586(14) . ? C13D C14D 1.409(17) . ? C15K C16K 1.3900 . ? C15K C20K 1.3900 . ? C15K C14K 1.552(15) . ? C16K C17K 1.3900 . ? C17K C18K 1.3900 . ? C18K C19K 1.3900 . ? C18K C7K 1.442(14) . ? C19K C20K 1.3900 . ? C4I C3I 1.474(17) . ? C4I C5I 1.537(17) . ? C5I C6I 1.651(15) . ? C6I C1I 1.348(16) . ? C6I N2I 1.434(14) . ? C7E O2E 1.388(13) . ? C7E O1E 1.405(13) . ? C7E Zn3 2.643(16) 9_554 ? C8E C11E 1.384(16) . ? C8E C10E 1.406(17) . ? C8E C9E 1.508(16) . ? C12E N2F 1.332(15) . ? C13E C14E 1.405(17) . ? C1F N1F 1.342(15) . ? C1F C6F 1.427(17) . ? C1F C2F 1.600(16) . ? C2F C3F 1.489(16) . ? C3F C4F 1.514(17) . ? C4F C5F 1.551(17) . ? C5F C6F 1.680(15) . ? C6F N2F 1.479(15) . ? N1F Mn2 2.046(14) . ? N2F Mn2 2.012(14) . ? Mn2 O3E 1.910(12) . ? Mn2 O3D 1.967(13) . ? Mn2 Cl2 2.294(8) . ? O1E Zn2 1.974(9) 9_554 ? O2E Zn3 1.538(12) 9_554 ? O1D Zn4 1.878(9) 4 ? O2D Zn1 1.872(9) 4 ? C1I N1I 1.414(14) . ? C1I C2I 1.572(15) . ? C2I C3I 1.507(17) . ? N1I C12G 1.342(15) . ? N1I Mn3 2.001(13) . ? N2I C12H 1.353(15) . ? N2I Mn3 1.957(13) . ? Mn3 O3H 1.933(12) . ? Mn3 O3G 1.911(12) . ? Mn3 Cl3 2.327(8) . ? O1H C7H 1.355(13) . ? O1H Zn3 1.943(9) 2_665 ? O2H C7H 1.394(13) . ? O2H Zn1 1.708(10) 2_665 ? O1G C7G 1.392(13) . ? O1G Zn6 1.925(10) 7_554 ? O2G C7G 1.334(13) . ? O2G Zn5 1.747(9) 7_554 ? C8G C9G 1.392(16) . ? C8G C11G 1.429(16) . ? C8G C10G 1.452(16) . ? C13G C14G 1.398(17) . ? C8H C10H 1.349(16) . ? C8H C9H 1.430(16) . ? C8H C11H 1.426(16) . ? C13H C14H 1.397(17) . ? C7J O1J 1.321(13) . ? C7J O2J 1.402(13) . ? C8J C10J 1.449(16) . ? C8J C11J 1.411(17) . ? C8J C9J 1.455(16) . ? C12J N1L 1.331(15) . ? C13J C14J 1.363(17) . ? C7K O2K 1.401(13) . ? C7K O1K 1.376(13) . ? C8K C11K 1.417(16) . ? C8K C10K 1.449(16) . ? C8K C9K 1.441(17) . ? C12K N2L 1.307(15) . ? C13K C14K 1.381(17) . ? C1L N1L 1.381(14) . ? C1L C6L 1.467(16) . ? C1L C2L 1.561(15) . ? C2L C3L 1.480(17) . ? C3L C4L 1.490(18) . ? C4L C5L 1.598(17) . ? C5L C6L 1.683(15) . ? C6L N2L 1.459(15) . ? N1L Mn4 2.016(13) . ? N2L Mn4 2.034(14) . ? Mn4 O3K 1.942(13) . ? Mn4 O3J 1.905(12) . ? Mn4 Cl4 2.370(8) . ? O1K Zn2 1.598(11) 3_565 ? O2K Zn1 1.883(9) 3_565 ? O1J Zn2 1.658(9) 2_565 ? O2J Zn4 1.975(9) 2_565 ? Zn1 O2H 1.708(10) 3_565 ? Zn1 O2D 1.872(9) 7_444 ? Zn1 O2K 1.883(9) 2_665 ? Zn1 O1 2.033(9) . ? Zn1 Zn4 3.128(3) . ? Zn1 Zn2 3.151(3) . ? Zn2 O1K 1.598(11) 2_665 ? Zn2 O1J 1.658(9) 3_455 ? Zn2 O1 1.960(9) . ? Zn2 O1E 1.974(9) 5 ? Zn2 Zn4 3.132(3) . ? Zn2 Zn3 3.181(3) . ? Zn3 O2E 1.538(12) 5 ? Zn3 O1B 1.775(10) 3_565 ? Zn3 O1H 1.943(9) 3_565 ? Zn3 O1 2.096(9) . ? Zn3 C7E 2.643(16) 5 ? Zn3 Zn4 3.131(3) . ? Zn4 O1 1.667(9) . ? Zn4 O1D 1.878(9) 7_444 ? Zn4 O2J 1.975(9) 3_455 ? Zn4 O2B 2.019(9) 3_565 ? Zn4 C7D 2.688(16) 7_444 ? Zn5 O1A 1.111(13) 9_554 ? Zn5 O2G 1.747(9) 4_445 ? Zn5 O2 1.952(6) . ? Zn5 O2A 1.957(9) 7_444 ? Zn5 C7A 2.265(18) 9_554 ? Zn5 Zn6 3.152(4) . ? Zn5 Zn5 3.166(4) 3 ? Zn5 Zn5 3.166(4) 2 ? Zn6 O2 1.881(16) . ? Zn6 O1G 1.925(10) 4_445 ? Zn6 O1G 1.925(10) 6_455 ? Zn6 O1G 1.925(10) 5 ? Zn6 Zn5 3.152(4) 3 ? Zn6 Zn5 3.152(4) 2 ? O2 Zn5 1.952(6) 3 ? O2 Zn5 1.952(6) 2 ? 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 C2A C1A C6A 120.0 . . ? C2A C1A C13A 117.9(14) . . ? C6A C1A C13A 122.1(14) . . ? C3A C2A C1A 120.0 . . ? C2A C3A C4A 120.0 . . ? C2A C3A C12A 115.3(14) . . ? C4A C3A C12A 124.7(14) . . ? C5A C4A C3A 120.0 . . ? C5A C4A O3A 117.9(14) . . ? C3A C4A O3A 122.1(14) . . ? C6A C5A C4A 120.0 . . ? C6A C5A C8A 125.4(13) . . ? C4A C5A C8A 114.6(13) . . ? C5A C6A C1A 120.0 . . ? O2A C7A O1A 132.5(16) . . ? O2A C7A C18A 110.4(14) . . ? O1A C7A C18A 117.2(15) . . ? O2A C7A Zn5 113.3(11) . 5 ? O1A C7A Zn5 22.6(6) . 5 ? C18A C7A Zn5 134.2(11) . 5 ? C9A C8A C10A 110.0(19) . . ? C9A C8A C11A 110(2) . . ? C10A C8A C11A 102.6(18) . . ? C9A C8A C5A 110.5(16) . . ? C10A C8A C5A 106.2(18) . . ? C11A C8A C5A 116.9(17) . . ? C16A C15A C20A 120.0 . . ? C16A C15A C14A 120.2(16) . . ? C20A C15A C14A 119.8(16) . . ? C17A C16A C15A 120.0 . . ? C18A C17A C16A 120.0 . . ? C19A C18A C17A 120.0 . . ? C19A C18A C7A 117.1(16) . . ? C17A C18A C7A 122.9(15) . . ? C18A C19A C20A 120.0 . . ? C19A C20A C15A 120.0 . . ? N1C C12A C3A 131.1(17) . . ? C2B C1B C6B 120.0 . . ? C2B C1B C13B 118.3(14) . . ? C6B C1B C13B 121.7(14) . . ? C3B C2B C1B 120.0 . . ? C2B C3B C4B 120.0 . . ? C2B C3B C12B 112.7(14) . . ? C4B C3B C12B 127.3(14) . . ? C5B C4B C3B 120.0 . . ? C5B C4B O3B 118.6(13) . . ? C3B C4B O3B 121.1(14) . . ? C4B C5B C6B 120.0 . . ? C4B C5B C8B 124.1(13) . . ? C6B C5B C8B 115.9(13) . . ? C5B C6B C1B 120.0 . . ? C14A C13A C1A 108.0(17) . . ? C13A C14A C15A 128.1(19) . . ? C16B C15B C20B 120.0 . . ? C16B C15B C14B 120.7(16) . . ? C20B C15B C14B 119.3(16) . . ? C15B C16B C17B 120.0 . . ? C18B C17B C16B 120.0 . . ? C17B C18B C19B 120.0 . . ? C17B C18B C7B 116.0(14) . . ? C19B C18B C7B 123.9(14) . . ? C18B C19B C20B 120.0 . . ? C19B C20B C15B 120.0 . . ? O1B C7B O2B 105.8(13) . . ? O1B C7B C18B 134.3(14) . . ? O2B C7B C18B 119.9(12) . . ? C11B C8B C10B 108.6(19) . . ? C11B C8B C9B 110.7(18) . . ? C10B C8B C9B 101.8(18) . . ? C11B C8B C5B 115.5(16) . . ? C10B C8B C5B 110.9(15) . . ? C9B C8B C5B 108.3(17) . . ? C2D C1D C6D 120.0 . . ? C2D C1D C13D 121.1(14) . . ? C6D C1D C13D 118.9(14) . . ? C3D C2D C1D 120.0 . . ? C12D C3D C2D 114.8(14) . . ? C12D C3D C4D 125.2(14) . . ? C2D C3D C4D 120.0 . . ? O3D C4D C3D 125.9(14) . . ? O3D C4D C5D 114.1(14) . . ? C3D C4D C5D 120.0 . . ? C6D C5D C4D 120.0 . . ? C6D C5D C8D 120.0(13) . . ? C4D C5D C8D 120.0(13) . . ? C5D C6D C1D 120.0 . . ? N2C C12B C3B 126.6(16) . . ? C16D C15D C20D 120.0 . . ? C16D C15D C14D 123.8(16) . . ? C20D C15D C14D 116.2(16) . . ? C17D C16D C15D 120.0 . . ? C16D C17D C18D 120.0 . . ? C19D C18D C17D 120.0 . . ? C19D C18D C7D 110.8(15) . . ? C17D C18D C7D 129.2(15) . . ? C18D C19D C20D 120.0 . . ? C19D C20D C15D 120.0 . . ? C14B C13B C1B 126.3(19) . . ? C13B C14B C15B 127.2(19) . . ? C2E C1E C6E 120.0 . . ? C2E C1E C13E 116.6(14) . . ? C6E C1E C13E 123.4(14) . . ? C1E C2E C3E 120.0 . . ? C2E C3E C4E 120.0 . . ? C2E C3E C12E 114.1(13) . . ? C4E C3E C12E 125.9(14) . . ? C5E C4E C3E 120.0 . . ? C5E C4E O3E 115.6(13) . . ? C3E C4E O3E 124.4(13) . . ? C4E C5E C6E 120.0 . . ? C4E C5E C8E 115.8(13) . . ? C6E C5E C8E 124.0(13) . . ? C5E C6E C1E 120.0 . . ? N1C C1C C6C 110.6(13) . . ? N1C C1C C2C 121.3(17) . . ? C6C C1C C2C 118.0(17) . . ? C3C C2C C1C 116.2(16) . . ? C4C C3C C2C 116.0(17) . . ? C16E C15E C20E 120.0 . . ? C16E C15E C14E 119.7(16) . . ? C20E C15E C14E 120.3(16) . . ? C17E C16E C15E 120.0 . . ? C18E C17E C16E 120.0 . . ? C17E C18E C19E 120.0 . . ? C17E C18E C7E 120.2(16) . . ? C19E C18E C7E 119.7(16) . . ? C20E C19E C18E 120.0 . . ? C19E C20E C15E 120.0 . . ? C3C C4C C5C 123.1(18) . . ? C4C C5C C6C 112.0(15) . . ? C1C C6C N2C 110.4(15) . . ? C1C C6C C5C 112.1(15) . . ? N2C C6C C5C 117.2(16) . . ? C2G C1G C6G 120.0 . . ? C2G C1G C13G 125.2(14) . . ? C6G C1G C13G 114.8(14) . . ? C1G C2G C3G 120.0 . . ? C12G C3G C4G 117.5(14) . . ? C12G C3G C2G 122.4(14) . . ? C4G C3G C2G 120.0 . . ? O3G C4G C3G 121.0(14) . . ? O3G C4G C5G 119.0(13) . . ? C3G C4G C5G 120.0 . . ? C6G C5G C4G 120.0 . . ? C6G C5G C8G 116.6(13) . . ? C4G C5G C8G 123.3(13) . . ? C5G C6G C1G 120.0 . . ? C12A N1C C1C 125.7(16) . . ? C12A N1C Mn1 118.0(13) . . ? C1C N1C Mn1 116.3(11) . . ? C12B N2C C6C 127.7(15) . . ? C12B N2C Mn1 119.4(13) . . ? C6C N2C Mn1 112.1(11) . . ? C16G C15G C20G 120.0 . . ? C16G C15G C14G 121.5(16) . . ? C20G C15G C14G 118.5(16) . . ? C15G C16G C17G 120.0 . . ? C16G C17G C18G 120.0 . . ? C19G C18G C17G 120.0 . . ? C19G C18G C7G 124.1(15) . . ? C17G C18G C7G 115.8(15) . . ? C20G C19G C18G 120.0 . . ? C19G C20G C15G 120.0 . . ? O3B Mn1 O3A 87.2(7) . . ? O3B Mn1 N2C 97.8(7) . . ? O3A Mn1 N2C 171.9(8) . . ? O3B Mn1 N1C 159.4(9) . . ? O3A Mn1 N1C 95.3(7) . . ? N2C Mn1 N1C 77.8(6) . . ? O3B Mn1 Cl1 90.8(5) . . ? O3A Mn1 Cl1 88.4(5) . . ? N2C Mn1 Cl1 97.8(6) . . ? N1C Mn1 Cl1 109.7(7) . . ? C2H C1H C6H 120.0 . . ? C2H C1H C13H 118.0(14) . . ? C6H C1H C13H 122.0(14) . . ? C1H C2H C3H 120.0 . . ? C4H C3H C2H 120.0 . . ? C4H C3H C12H 125.0(13) . . ? C2H C3H C12H 115.0(14) . . ? C3H C4H C5H 120.0 . . ? C3H C4H O3H 125.1(13) . . ? C5H C4H O3H 114.8(13) . . ? C4H C5H C6H 120.0 . . ? C4H C5H C8H 116.9(13) . . ? C6H C5H C8H 123.1(13) . . ? C5H C6H C1H 120.0 . . ? Zn5 O1A C7A 128.3(13) 5 . ? C7A O2A Zn5 108.9(9) . 4 ? C4A O3A Mn1 124.9(12) . . ? C16H C15H C20H 120.0 . . ? C16H C15H C14H 126.0(16) . . ? C20H C15H C14H 114.0(16) . . ? C17H C16H C15H 120.0 . . ? C16H C17H C18H 120.0 . . ? C19H C18H C17H 120.0 . . ? C19H C18H C7H 119.6(15) . . ? C17H C18H C7H 120.4(15) . . ? C18H C19H C20H 120.0 . . ? C19H C20H C15H 120.0 . . ? C7B O1B Zn3 147.6(9) . 2_665 ? C7B O2B Zn4 127.0(9) . 2_665 ? C4B O3B Mn1 125.9(12) . . ? C2J C1J C6J 120.0 . . ? C2J C1J C13J 122.1(14) . . ? C6J C1J C13J 117.9(14) . . ? C1J C2J C3J 120.0 . . ? C12J C3J C4J 126.1(14) . . ? C12J C3J C2J 113.9(14) . . ? C4J C3J C2J 120.0 . . ? O3J C4J C5J 119.1(14) . . ? O3J C4J C3J 120.8(14) . . ? C5J C4J C3J 120.0 . . ? C4J C5J C6J 120.0 . . ? C4J C5J C8J 121.3(13) . . ? C6J C5J C8J 118.7(13) . . ? C5J C6J C1J 120.0 . . ? O2D C7D O1D 135.6(16) . . ? O2D C7D C18D 116.1(14) . . ? O1D C7D C18D 108.3(12) . . ? O2D C7D Zn4 96.3(10) . 4 ? O1D C7D Zn4 41.2(6) . 4 ? C18D C7D Zn4 146.0(10) . 4 ? C11D C8D C9D 117(2) . . ? C11D C8D C10D 102.2(19) . . ? C9D C8D C10D 110(2) . . ? C11D C8D C5D 114.4(18) . . ? C9D C8D C5D 107.0(17) . . ? C10D C8D C5D 106.1(18) . . ? C16J C15J C20J 120.0 . . ? C16J C15J C14J 117.1(16) . . ? C20J C15J C14J 122.9(16) . . ? C15J C16J C17J 120.0 . . ? C16J C17J C18J 120.0 . . ? C17J C18J C19J 120.0 . . ? C17J C18J C7J 115.6(15) . . ? C19J C18J C7J 124.2(15) . . ? C20J C19J C18J 120.0 . . ? C19J C20J C15J 120.0 . . ? N1F C12D C3D 128.9(17) . . ? C2K C1K C6K 120.0 . . ? C2K C1K C13K 120.8(14) . . ? C6K C1K C13K 119.2(14) . . ? C1K C2K C3K 120.0 . . ? C4K C3K C2K 120.0 . . ? C4K C3K C12K 126.1(14) . . ? C2K C3K C12K 113.9(14) . . ? C3K C4K C5K 120.0 . . ? C3K C4K O3K 122.2(14) . . ? C5K C4K O3K 117.8(14) . . ? C6K C5K C4K 120.0 . . ? C6K C5K C8K 116.1(13) . . ? C4K C5K C8K 123.9(13) . . ? C5K C6K C1K 120.0 . . ? C14D C13D C1D 121.3(18) . . ? C13D C14D C15D 120.5(19) . . ? C16K C15K C20K 120.0 . . ? C16K C15K C14K 114.3(16) . . ? C20K C15K C14K 125.7(16) . . ? C17K C16K C15K 120.0 . . ? C18K C17K C16K 120.0 . . ? C17K C18K C19K 120.0 . . ? C17K C18K C7K 114.7(16) . . ? C19K C18K C7K 125.3(16) . . ? C20K C19K C18K 120.0 . . ? C19K C20K C15K 120.0 . . ? C3I C4I C5I 114(2) . . ? C4I C5I C6I 108.4(15) . . ? C1I C6I N2I 106.9(15) . . ? C1I C6I C5I 115.8(15) . . ? N2I C6I C5I 118.5(16) . . ? O2E C7E O1E 128.4(15) . . ? O2E C7E C18E 113.5(14) . . ? O1E C7E C18E 118.1(14) . . ? O2E C7E Zn3 26.8(6) . 9_554 ? O1E C7E Zn3 107.0(10) . 9_554 ? C18E C7E Zn3 131.4(10) . 9_554 ? C11E C8E C10E 109.3(19) . . ? C11E C8E C9E 109.5(18) . . ? C10E C8E C9E 106.3(19) . . ? C11E C8E C5E 119.8(17) . . ? C10E C8E C5E 107.2(18) . . ? C9E C8E C5E 103.9(15) . . ? N2F C12E C3E 123.9(16) . . ? C14E C13E C1E 119.6(18) . . ? C13E C14E C15E 132.6(19) . . ? N1F C1F C6F 106.3(14) . . ? N1F C1F C2F 120(2) . . ? C6F C1F C2F 108.9(17) . . ? C3F C2F C1F 118.2(17) . . ? C2F C3F C4F 112.3(18) . . ? C3F C4F C5F 114.8(19) . . ? C4F C5F C6F 105.6(15) . . ? C1F C6F N2F 109.3(16) . . ? C1F C6F C5F 115.7(15) . . ? N2F C6F C5F 116.0(15) . . ? C1F N1F C12D 123.9(16) . . ? C1F N1F Mn2 119.5(12) . . ? C12D N1F Mn2 116.7(13) . . ? C12E N2F C6F 128.2(16) . . ? C12E N2F Mn2 124.2(13) . . ? C6F N2F Mn2 107.6(10) . . ? O3E Mn2 O3D 85.0(7) . . ? O3E Mn2 N2F 96.3(7) . . ? O3D Mn2 N2F 170.0(9) . . ? O3E Mn2 N1F 155.5(10) . . ? O3D Mn2 N1F 98.4(7) . . ? N2F Mn2 N1F 76.4(7) . . ? O3E Mn2 Cl2 94.3(6) . . ? O3D Mn2 Cl2 92.4(5) . . ? N2F Mn2 Cl2 97.4(7) . . ? N1F Mn2 Cl2 109.7(8) . . ? C7E O1E Zn2 114.1(10) . 9_554 ? C7E O2E Zn3 129.1(10) . 9_554 ? C4E O3E Mn2 123.9(12) . . ? C7D O1D Zn4 109.5(9) . 4 ? C7D O2D Zn1 127.2(9) . 4 ? C4D O3D Mn2 119.6(12) . . ? C6I C1I N1I 107.9(14) . . ? C6I C1I C2I 120.2(16) . . ? N1I C1I C2I 123.5(16) . . ? C3I C2I C1I 115.1(16) . . ? C4I C3I C2I 107.9(19) . . ? C12G N1I C1I 120.5(16) . . ? C12G N1I Mn3 119.3(13) . . ? C1I N1I Mn3 114.7(11) . . ? C12H N2I C6I 122.6(15) . . ? C12H N2I Mn3 121.1(13) . . ? C6I N2I Mn3 115.5(11) . . ? O3H Mn3 O3G 90.7(7) . . ? O3H Mn3 N2I 98.2(7) . . ? O3G Mn3 N2I 160.6(8) . . ? O3H Mn3 N1I 159.8(8) . . ? O3G Mn3 N1I 89.5(7) . . ? N2I Mn3 N1I 76.2(6) . . ? O3H Mn3 Cl3 96.9(5) . . ? O3G Mn3 Cl3 99.0(5) . . ? N2I Mn3 Cl3 97.0(6) . . ? N1I Mn3 Cl3 102.9(7) . . ? C7H O1H Zn3 111.0(9) . 2_665 ? C7H O2H Zn1 127.6(10) . 2_665 ? C4H O3H Mn3 122.8(11) . . ? C7G O1G Zn6 112.2(9) . 7_554 ? C7G O2G Zn5 131.0(10) . 7_554 ? C4G O3G Mn3 128.6(12) . . ? O2G C7G O1G 134.1(15) . . ? O2G C7G C18G 117.1(14) . . ? O1G C7G C18G 108.8(13) . . ? C9G C8G C11G 112.7(19) . . ? C9G C8G C10G 103.0(17) . . ? C11G C8G C10G 118(2) . . ? C9G C8G C5G 120.4(17) . . ? C11G C8G C5G 100.9(15) . . ? C10G C8G C5G 102.2(16) . . ? C3G C12G N1I 132.5(17) . . ? C14G C13G C1G 122.7(18) . . ? C13G C14G C15G 118.9(18) . . ? O1H C7H O2H 138.3(15) . . ? O1H C7H C18H 109.9(13) . . ? O2H C7H C18H 111.7(13) . . ? C10H C8H C9H 110.0(18) . . ? C10H C8H C11H 109(2) . . ? C9H C8H C11H 104.2(19) . . ? C10H C8H C5H 115.6(16) . . ? C9H C8H C5H 107.5(17) . . ? C11H C8H C5H 110.1(16) . . ? N2I C12H C3H 127.4(17) . . ? C14H C13H C1H 120.1(19) . . ? C13H C14H C15H 124.7(19) . . ? O1J C7J O2J 122.5(15) . . ? O1J C7J C18J 122.5(15) . . ? O2J C7J C18J 115.0(13) . . ? C10J C8J C11J 111.1(18) . . ? C10J C8J C9J 110(2) . . ? C11J C8J C9J 113(2) . . ? C10J C8J C5J 110.2(15) . . ? C11J C8J C5J 109.7(18) . . ? C9J C8J C5J 102.3(16) . . ? N1L C12J C3J 130.0(17) . . ? C14J C13J C1J 120.3(18) . . ? C13J C14J C15J 119.4(19) . . ? O2K C7K O1K 133.2(15) . . ? O2K C7K C18K 115.3(14) . . ? O1K C7K C18K 111.5(14) . . ? C11K C8K C10K 112(2) . . ? C11K C8K C9K 107(2) . . ? C10K C8K C9K 102.8(19) . . ? C11K C8K C5K 111.6(16) . . ? C10K C8K C5K 113.4(17) . . ? C9K C8K C5K 109.4(18) . . ? N2L C12K C3K 128.4(18) . . ? C14K C13K C1K 124.4(19) . . ? C13K C14K C15K 124.2(19) . . ? N1L C1L C6L 108.6(13) . . ? N1L C1L C2L 125.4(19) . . ? C6L C1L C2L 112.9(16) . . ? C3L C2L C1L 119.0(17) . . ? C4L C3L C2L 111.3(19) . . ? C3L C4L C5L 109(2) . . ? C4L C5L C6L 101.5(15) . . ? C1L C6L N2L 111.5(16) . . ? C1L C6L C5L 114.1(16) . . ? N2L C6L C5L 113.5(15) . . ? C12J N1L C1L 127.2(16) . . ? C12J N1L Mn4 117.0(13) . . ? C1L N1L Mn4 115.8(11) . . ? C12K N2L C6L 130.1(16) . . ? C12K N2L Mn4 122.5(14) . . ? C6L N2L Mn4 107.0(10) . . ? O3K Mn4 O3J 84.8(7) . . ? O3K Mn4 N2L 93.7(7) . . ? O3J Mn4 N2L 170.0(9) . . ? O3K Mn4 N1L 159.3(9) . . ? O3J Mn4 N1L 97.0(7) . . ? N2L Mn4 N1L 80.9(7) . . ? O3K Mn4 Cl4 90.1(5) . . ? O3J Mn4 Cl4 99.5(5) . . ? N2L Mn4 Cl4 90.4(7) . . ? N1L Mn4 Cl4 109.8(7) . . ? C7K O1K Zn2 126.7(11) . 3_565 ? C7K O2K Zn1 115.4(9) . 3_565 ? C4K O3K Mn4 126.3(12) . . ? C7J O1J Zn2 137.1(9) . 2_565 ? C7J O2J Zn4 118.2(10) . 2_565 ? C4J O3J Mn4 121.6(12) . . ? O2H Zn1 O2D 103.3(4) 3_565 7_444 ? O2H Zn1 O2K 117.4(5) 3_565 2_665 ? O2D Zn1 O2K 104.8(4) 7_444 2_665 ? O2H Zn1 O1 116.2(4) 3_565 . ? O2D Zn1 O1 100.2(4) 7_444 . ? O2K Zn1 O1 112.2(4) 2_665 . ? O2H Zn1 Zn4 124.2(4) 3_565 . ? O2D Zn1 Zn4 71.4(3) 7_444 . ? O2K Zn1 Zn4 117.6(3) 2_665 . ? O1 Zn1 Zn4 28.8(3) . . ? O2H Zn1 Zn2 124.7(3) 3_565 . ? O2D Zn1 Zn2 124.6(3) 7_444 . ? O2K Zn1 Zn2 78.2(3) 2_665 . ? O1 Zn1 Zn2 37.1(3) . . ? Zn4 Zn1 Zn2 59.83(7) . . ? O1K Zn2 O1J 110.6(5) 2_665 3_455 ? O1K Zn2 O1 117.3(5) 2_665 . ? O1J Zn2 O1 101.4(4) 3_455 . ? O1K Zn2 O1E 108.2(5) 2_665 5 ? O1J Zn2 O1E 104.1(4) 3_455 5 ? O1 Zn2 O1E 114.2(4) . 5 ? O1K Zn2 Zn4 131.4(4) 2_665 . ? O1J Zn2 Zn4 73.9(3) 3_455 . ? O1 Zn2 Zn4 27.7(3) . . ? O1E Zn2 Zn4 117.7(3) 5 . ? O1K Zn2 Zn1 78.6(4) 2_665 . ? O1J Zn2 Zn1 118.9(3) 3_455 . ? O1 Zn2 Zn1 38.7(3) . . ? O1E Zn2 Zn1 131.1(3) 5 . ? Zn4 Zn2 Zn1 59.73(7) . . ? O1K Zn2 Zn3 121.1(4) 2_665 . ? O1J Zn2 Zn3 125.3(3) 3_455 . ? O1 Zn2 Zn3 39.9(3) . . ? O1E Zn2 Zn3 76.7(3) 5 . ? Zn4 Zn2 Zn3 59.47(7) . . ? Zn1 Zn2 Zn3 60.26(7) . . ? O2E Zn3 O1B 121.3(5) 5 3_565 ? O2E Zn3 O1H 107.7(6) 5 3_565 ? O1B Zn3 O1H 98.8(4) 3_565 3_565 ? O2E Zn3 O1 111.5(5) 5 . ? O1B Zn3 O1 99.8(4) 3_565 . ? O1H Zn3 O1 117.6(4) 3_565 . ? O2E Zn3 C7E 24.0(5) 5 5 ? O1B Zn3 C7E 111.1(4) 3_565 5 ? O1H Zn3 C7E 131.7(4) 3_565 5 ? O1 Zn3 C7E 94.2(5) . 5 ? O2E Zn3 Zn4 131.5(5) 5 . ? O1B Zn3 Zn4 70.7(3) 3_565 . ? O1H Zn3 Zn4 116.8(3) 3_565 . ? O1 Zn3 Zn4 29.5(3) . . ? C7E Zn3 Zn4 108.6(4) 5 . ? O2E Zn3 Zn2 75.1(5) 5 . ? O1B Zn3 Zn2 115.9(3) 3_565 . ? O1H Zn3 Zn2 137.8(3) 3_565 . ? O1 Zn3 Zn2 36.8(3) . . ? C7E Zn3 Zn2 57.8(4) 5 . ? Zn4 Zn3 Zn2 59.48(7) . . ? O1 Zn4 O1D 121.1(5) . 7_444 ? O1 Zn4 O2J 109.4(5) . 3_455 ? O1D Zn4 O2J 102.3(4) 7_444 3_455 ? O1 Zn4 O2B 113.9(5) . 3_565 ? O1D Zn4 O2B 98.7(4) 7_444 3_565 ? O2J Zn4 O2B 110.4(4) 3_455 3_565 ? O1 Zn4 C7D 92.4(5) . 7_444 ? O1D Zn4 C7D 29.3(4) 7_444 7_444 ? O2J Zn4 C7D 110.1(3) 3_455 7_444 ? O2B Zn4 C7D 119.3(4) 3_565 7_444 ? O1 Zn4 Zn2 33.1(3) . . ? O1D Zn4 Zn2 144.3(3) 7_444 . ? O2J Zn4 Zn2 79.3(3) 3_455 . ? O2B Zn4 Zn2 114.3(3) 3_565 . ? C7D Zn4 Zn2 116.2(3) 7_444 . ? O1 Zn4 Zn1 36.1(3) . . ? O1D Zn4 Zn1 86.7(3) 7_444 . ? O2J Zn4 Zn1 111.0(3) 3_455 . ? O2B Zn4 Zn1 136.0(3) 3_565 . ? C7D Zn4 Zn1 57.4(3) 7_444 . ? Zn2 Zn4 Zn1 60.44(7) . . ? O1 Zn4 Zn3 38.3(3) . . ? O1D Zn4 Zn3 116.9(3) 7_444 . ? O2J Zn4 Zn3 138.4(3) 3_455 . ? O2B Zn4 Zn3 78.1(3) 3_565 . ? C7D Zn4 Zn3 98.9(2) 7_444 . ? Zn2 Zn4 Zn3 61.05(7) . . ? Zn1 Zn4 Zn3 61.03(7) . . ? Zn4 O1 Zn2 119.2(5) . . ? Zn4 O1 Zn3 112.2(5) . . ? Zn2 O1 Zn3 103.3(4) . . ? Zn4 O1 Zn1 115.1(5) . . ? Zn2 O1 Zn1 104.2(5) . . ? Zn3 O1 Zn1 100.7(4) . . ? O1A Zn5 O2G 116.8(8) 9_554 4_445 ? O1A Zn5 O2 112.6(9) 9_554 . ? O2G Zn5 O2 107.7(5) 4_445 . ? O1A Zn5 O2A 108.9(8) 9_554 7_444 ? O2G Zn5 O2A 105.8(4) 4_445 7_444 ? O2 Zn5 O2A 104.0(3) . 7_444 ? O1A Zn5 C7A 29.1(8) 9_554 9_554 ? O2G Zn5 C7A 104.9(4) 4_445 9_554 ? O2 Zn5 C7A 94.1(5) . 9_554 ? O2A Zn5 C7A 137.2(5) 7_444 9_554 ? O1A Zn5 Zn6 135.8(8) 9_554 . ? O2G Zn5 Zn6 74.2(3) 4_445 . ? O2 Zn5 Zn6 34.0(4) . . ? O2A Zn5 Zn6 108.1(3) 7_444 . ? C7A Zn5 Zn6 108.4(4) 9_554 . ? O1A Zn5 Zn5 78.5(8) 9_554 3 ? O2G Zn5 Zn5 116.5(3) 4_445 3 ? O2 Zn5 Zn5 35.8(2) . 3 ? O2A Zn5 Zn5 127.7(3) 7_444 3 ? C7A Zn5 Zn5 58.3(4) 9_554 3 ? Zn6 Zn5 Zn5 59.85(5) . 3 ? O1A Zn5 Zn5 112.8(7) 9_554 2 ? O2G Zn5 Zn5 128.1(3) 4_445 2 ? O2 Zn5 Zn5 35.8(2) . 2 ? O2A Zn5 Zn5 70.2(3) 7_444 2 ? C7A Zn5 Zn5 111.1(3) 9_554 2 ? Zn6 Zn5 Zn5 59.85(5) . 2 ? Zn5 Zn5 Zn5 60.0 3 2 ? O2 Zn6 O1G 116.2(3) . 4_445 ? O2 Zn6 O1G 116.2(3) . 6_455 ? O1G Zn6 O1G 102.0(4) 4_445 6_455 ? O2 Zn6 O1G 116.2(3) . 5 ? O1G Zn6 O1G 102.0(4) 4_445 5 ? O1G Zn6 O1G 101.9(4) 6_455 5 ? O2 Zn6 Zn5 35.45(6) . 3 ? O1G Zn6 Zn5 113.5(3) 4_445 3 ? O1G Zn6 Zn5 83.7(3) 6_455 3 ? O1G Zn6 Zn5 142.2(3) 5 3 ? O2 Zn6 Zn5 35.45(6) . 2 ? O1G Zn6 Zn5 142.2(3) 4_445 2 ? O1G Zn6 Zn5 113.5(3) 6_455 2 ? O1G Zn6 Zn5 83.7(3) 5 2 ? Zn5 Zn6 Zn5 60.31(9) 3 2 ? O2 Zn6 Zn5 35.45(6) . . ? O1G Zn6 Zn5 83.7(3) 4_445 . ? O1G Zn6 Zn5 142.2(3) 6_455 . ? O1G Zn6 Zn5 113.5(3) 5 . ? Zn5 Zn6 Zn5 60.31(9) 3 . ? Zn5 Zn6 Zn5 60.31(9) 2 . ? Zn6 O2 Zn5 110.6(5) . 3 ? Zn6 O2 Zn5 110.6(5) . . ? Zn5 O2 Zn5 108.4(5) 3 . ? Zn6 O2 Zn5 110.6(5) . 2 ? Zn5 O2 Zn5 108.4(5) 3 2 ? Zn5 O2 Zn5 108.4(5) . 2 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 33.41 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.500 _refine_diff_density_min -0.513 _refine_diff_density_rms 0.027 # Attachment '- P212121.cif' data_p212121 _database_code_depnum_ccdc_archive 'CCDC 806228' #TrackingRef '- P212121.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H15 N3 O3' _chemical_formula_weight 249.27 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' 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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 8.9026(2) _cell_length_b 9.2288(2) _cell_length_c 14.7549(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1212.27(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.366 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 528 _exptl_absorpt_coefficient_mu 0.831 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7885 _exptl_absorpt_correction_T_max 0.8514 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8212 _diffrn_reflns_av_R_equivalents 0.0218 _diffrn_reflns_av_sigmaI/netI 0.0154 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 5.65 _diffrn_reflns_theta_max 71.89 _reflns_number_total 2313 _reflns_number_gt 2301 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0805P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.10(13) _chemical_absolute_configuration ad _refine_ls_number_reflns 2313 _refine_ls_number_parameters 223 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0321 _refine_ls_R_factor_gt 0.0320 _refine_ls_wR_factor_ref 0.0962 _refine_ls_wR_factor_gt 0.0961 _refine_ls_goodness_of_fit_ref 1.175 _refine_ls_restrained_S_all 1.175 _refine_ls_shift/su_max 0.002 _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 O1 O 0.29384(9) 0.37798(9) 0.84706(6) 0.0194(2) Uani 1 1 d . . . C7 C 0.27522(13) 0.58369(12) 0.99616(7) 0.0160(2) Uani 1 1 d . . . C3 C 0.41674(12) 0.40346(12) 0.90122(7) 0.0171(2) Uani 1 1 d . . . C1 C 0.54488(13) 0.51163(13) 1.02824(8) 0.0187(3) Uani 1 1 d . . . C5 C 0.67294(13) 0.43515(13) 1.00632(8) 0.0212(3) Uani 1 1 d . . . C4 C 0.54707(14) 0.32767(12) 0.87905(8) 0.0216(3) Uani 1 1 d . . . C2 C 0.41460(12) 0.49651(11) 0.97579(7) 0.0166(2) Uani 1 1 d . . . C8 C 0.13832(12) 0.51675(12) 0.95080(7) 0.0163(2) Uani 1 1 d . . . C10 C 0.21424(13) 0.61581(14) 0.79614(8) 0.0215(3) Uani 1 1 d . . . C6 C 0.67470(14) 0.34229(13) 0.93218(9) 0.0222(3) Uani 1 1 d . . . C11 C 0.03919(13) 0.40248(14) 0.80859(8) 0.0228(3) Uani 1 1 d . . . C9 C 0.17151(12) 0.48183(12) 0.85078(7) 0.0167(2) Uani 1 1 d . . . O2 O 0.01625(9) 0.61529(10) 0.95771(6) 0.0213(2) Uani 1 1 d . . . O3 O 0.80807(9) 0.44947(11) 1.05192(7) 0.0280(2) Uani 1 1 d . . . C12 C 0.80135(13) 0.48364(14) 1.14648(8) 0.0244(3) Uani 1 1 d . . . N1 N 0.25277(11) 0.58826(12) 1.09623(6) 0.0197(2) Uani 1 1 d . . . N2 N 0.18325(12) 0.69550(11) 1.12365(6) 0.0222(2) Uani 1 1 d . . . N3 N 0.12281(16) 0.78752(15) 1.15871(7) 0.0378(3) Uani 1 1 d . . . H8 H 0.309(2) 0.6562(18) 0.8175(13) 0.030(4) Uiso 1 1 d . . . H10 H 0.134(2) 0.689(2) 0.8043(14) 0.041(5) Uiso 1 1 d . . . H3 H 0.762(2) 0.291(2) 0.9194(11) 0.028(4) Uiso 1 1 d . . . H2 H 0.5461(18) 0.5791(18) 1.0792(12) 0.022(4) Uiso 1 1 d . . . H5 H 0.763(2) 0.572(2) 1.1576(14) 0.038(5) Uiso 1 1 d . . . H4 H 0.549(2) 0.264(2) 0.8280(12) 0.030(4) Uiso 1 1 d . . . H12 H 0.026(2) 0.312(2) 0.8468(13) 0.036(5) Uiso 1 1 d . . . H11 H -0.050(2) 0.463(2) 0.8081(13) 0.031(4) Uiso 1 1 d . . . H9 H 0.231(2) 0.593(2) 0.7302(15) 0.042(5) Uiso 1 1 d . . . H6 H 0.738(2) 0.413(2) 1.1786(14) 0.033(4) Uiso 1 1 d . . . H1 H 0.2895(17) 0.6806(17) 0.9752(10) 0.017(4) Uiso 1 1 d . . . H7 H 0.9069(19) 0.4791(18) 1.1697(12) 0.025(4) Uiso 1 1 d . . . H13 H 0.1115(17) 0.4258(17) 0.9820(11) 0.019(4) Uiso 1 1 d . . . H14 H 0.065(2) 0.375(2) 0.7493(14) 0.041(5) Uiso 1 1 d . . . H15 H -0.062(2) 0.563(2) 0.9857(14) 0.032(4) Uiso 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 O1 0.0187(4) 0.0186(4) 0.0208(4) -0.0052(3) -0.0001(3) 0.0013(3) C7 0.0185(5) 0.0163(6) 0.0131(5) 0.0004(4) 0.0010(3) 0.0005(4) C3 0.0162(5) 0.0157(5) 0.0194(5) 0.0011(4) 0.0032(4) -0.0020(4) C1 0.0183(5) 0.0217(5) 0.0163(5) 0.0022(4) 0.0009(4) -0.0003(4) C5 0.0161(5) 0.0255(6) 0.0219(5) 0.0062(4) 0.0020(4) -0.0015(4) C4 0.0237(6) 0.0172(5) 0.0238(5) -0.0013(5) 0.0058(5) -0.0009(4) C2 0.0174(5) 0.0160(5) 0.0164(5) 0.0030(4) 0.0032(4) 0.0010(4) C8 0.0163(5) 0.0160(5) 0.0166(5) 0.0026(4) 0.0015(4) 0.0019(4) C10 0.0266(6) 0.0213(6) 0.0165(5) 0.0003(4) 0.0002(4) -0.0020(5) C6 0.0180(5) 0.0207(6) 0.0280(6) 0.0043(4) 0.0070(5) 0.0034(5) C11 0.0202(5) 0.0258(6) 0.0224(5) -0.0053(5) -0.0020(4) -0.0041(5) C9 0.0161(5) 0.0182(5) 0.0158(5) -0.0006(4) 0.0008(4) 0.0004(4) O2 0.0165(4) 0.0240(4) 0.0233(4) -0.0017(3) 0.0013(3) 0.0049(3) O3 0.0155(4) 0.0438(6) 0.0246(4) 0.0033(4) 0.0003(3) 0.0027(4) C12 0.0223(6) 0.0247(6) 0.0263(6) -0.0016(5) -0.0027(4) 0.0039(4) N1 0.0205(5) 0.0247(5) 0.0139(4) 0.0009(3) 0.0011(4) 0.0063(4) N2 0.0256(5) 0.0283(5) 0.0127(4) -0.0010(4) -0.0006(4) 0.0064(4) N3 0.0554(8) 0.0396(7) 0.0183(5) -0.0028(5) -0.0007(5) 0.0238(6) _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 O1 C3 1.3751(13) . ? O1 C9 1.4517(12) . ? C7 N1 1.4905(13) . ? C7 C2 1.5091(14) . ? C7 C8 1.5215(15) . ? C3 C4 1.3937(16) . ? C3 C2 1.3959(16) . ? C1 C5 1.3793(16) . ? C1 C2 1.4012(16) . ? C5 O3 1.3848(14) . ? C5 C6 1.3897(18) . ? C4 C6 1.3870(18) . ? C8 O2 1.4207(13) . ? C8 C9 1.5393(14) . ? C10 C9 1.5243(15) . ? C11 C9 1.5203(15) . ? O3 C12 1.4316(16) . ? N1 N2 1.2355(15) . ? N2 N3 1.1306(17) . ? 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 C3 O1 C9 117.52(8) . . ? N1 C7 C2 108.82(9) . . ? N1 C7 C8 109.87(9) . . ? C2 C7 C8 110.77(9) . . ? O1 C3 C4 116.12(10) . . ? O1 C3 C2 123.53(10) . . ? C4 C3 C2 120.34(10) . . ? C5 C1 C2 120.24(11) . . ? C1 C5 O3 123.73(11) . . ? C1 C5 C6 120.63(12) . . ? O3 C5 C6 115.57(11) . . ? C6 C4 C3 120.03(11) . . ? C3 C2 C1 119.03(10) . . ? C3 C2 C7 119.75(9) . . ? C1 C2 C7 121.16(10) . . ? O2 C8 C7 108.74(9) . . ? O2 C8 C9 110.47(9) . . ? C7 C8 C9 110.67(9) . . ? C4 C6 C5 119.71(11) . . ? O1 C9 C11 104.35(9) . . ? O1 C9 C10 109.17(9) . . ? C11 C9 C10 111.57(10) . . ? O1 C9 C8 108.57(8) . . ? C11 C9 C8 110.16(9) . . ? C10 C9 C8 112.65(10) . . ? C5 O3 C12 117.28(9) . . ? N2 N1 C7 114.48(9) . . ? N3 N2 N1 171.89(12) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 71.89 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.200 _refine_diff_density_min -0.255 _refine_diff_density_rms 0.059