# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_FJI-3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H9 O22 Zn5' _chemical_formula_weight 1012.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Orthorhombic _symmetry_space_group_name_H-M Ibam loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x, -y, -z+1/2' '-x, y, -z+1/2' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z+1' '-x+1/2, y+1/2, -z+1' '-x, -y, -z' 'x, y, -z' '-x, y, z-1/2' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' '-x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z' _cell_length_a 19.7757(2) _cell_length_b 44.7064(5) _cell_length_c 28.6303(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 25312.1(5) _cell_formula_units_Z 16 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 15478 _cell_measurement_theta_min 3.3490 _cell_measurement_theta_max 74.6830 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.062 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7952 _exptl_absorpt_coefficient_mu 2.565 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7483 _exptl_absorpt_correction_T_max 0.9044 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54184 _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 26679 _diffrn_reflns_av_R_equivalents 0.0303 _diffrn_reflns_av_sigmaI/netI 0.0327 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 52 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 65.00 _reflns_number_total 10953 _reflns_number_gt 9262 _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^)+(0.1747P)^2^+267.2065P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10953 _refine_ls_number_parameters 536 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0960 _refine_ls_R_factor_gt 0.0850 _refine_ls_wR_factor_ref 0.2709 _refine_ls_wR_factor_gt 0.2496 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.003 -0.001 -0.014 15380 5866 ' ' _platon_squeeze_details ; ; 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 0.57498(3) 0.266622(14) 0.24687(2) 0.0136(2) Uani 1 1 d . . . Zn7 Zn 0.0000 0.53286(2) 0.2500 0.0157(3) Uani 1 2 d S . . Zn4 Zn 0.70084(5) 0.40744(2) 0.5000 0.0166(3) Uani 1 2 d S . . Zn3 Zn 0.34336(5) 0.42527(2) 0.5000 0.0182(3) Uani 1 2 d S . . Zn2 Zn 0.24271(4) 0.383818(19) 0.43394(3) 0.0330(3) Uani 1 1 d . . . Zn6 Zn 0.86304(7) 0.39708(3) 0.5000 0.0579(5) Uani 1 2 d S . . O4 O 0.3903(3) 0.40031(16) 0.4500(3) 0.074(2) Uani 1 1 d . . . O2 O 0.4395(2) 0.29926(10) 0.30064(15) 0.0303(9) Uani 1 1 d . . . O12 O 0.9398(2) 0.26423(10) 0.30560(16) 0.0323(10) Uani 1 1 d . . . O1 O 0.5530(2) 0.29727(10) 0.29809(15) 0.0324(10) Uani 1 1 d . . . O3 O 0.3273(2) 0.36561(10) 0.41520(17) 0.0345(10) Uani 1 1 d . . . O22 O 0.7757(3) 0.37897(13) 0.5000 0.0279(13) Uani 1 2 d S . . O17 O 0.2775(3) 0.56025(11) 0.4522(2) 0.0493(14) Uani 1 1 d . . . O15 O 0.0651(3) 0.52467(11) 0.30203(17) 0.0404(11) Uani 1 1 d . . . O13 O 0.2271(2) 0.42370(11) 0.40698(18) 0.0385(11) Uani 1 1 d . . . O16 O 0.0777(3) 0.47571(11) 0.29608(17) 0.0400(11) Uani 1 1 d . . . O11 O 1.0519(2) 0.26574(9) 0.29322(16) 0.0294(10) Uani 1 1 d . . . O9 O 1.1577(2) 0.36272(11) 0.4309(2) 0.0422(12) Uani 1 1 d . . . O5 O 0.6345(3) 0.39102(12) 0.4521(2) 0.0497(14) Uani 1 1 d . . . O7 O 0.9119(3) 0.37155(12) 0.4489(2) 0.0498(14) Uani 1 1 d . . . C11 C 1.0245(3) 0.34443(13) 0.4131(2) 0.0277(13) Uani 1 1 d . . . H11 H 1.0301 0.3602 0.4351 0.033 Uiso 1 1 calc R . . C4 C 0.5083(3) 0.37274(15) 0.4227(2) 0.0298(13) Uani 1 1 d . . . H4 H 0.5106 0.3874 0.4467 0.036 Uiso 1 1 calc R . . C14 C 1.0066(3) 0.29808(14) 0.3498(2) 0.0255(12) Uani 1 1 d . . . C2 C 0.4420(3) 0.34238(13) 0.3702(2) 0.0253(12) Uani 1 1 d . . . H2 H 0.3994 0.3360 0.3585 0.030 Uiso 1 1 calc R . . C10 C 0.9598(3) 0.33391(14) 0.4030(2) 0.0291(13) Uani 1 1 d . . . C6 C 0.5637(3) 0.33861(16) 0.3701(2) 0.0323(14) Uani 1 1 d . . . H6 H 0.6039 0.3295 0.3586 0.039 Uiso 1 1 calc R . . C19 C 0.2231(3) 0.47608(15) 0.4014(2) 0.0334(14) Uani 1 1 d . . . C3 C 0.4455(3) 0.36374(14) 0.4053(2) 0.0276(13) Uani 1 1 d . . . C5 C 0.5676(3) 0.36030(15) 0.4049(2) 0.0311(14) Uani 1 1 d . . . C1 C 0.5018(3) 0.33027(14) 0.3523(2) 0.0251(12) Uani 1 1 d . . . C22 C 0.1645(4) 0.52822(17) 0.3687(3) 0.0438(18) Uani 1 1 d . . . H22 H 0.1452 0.5461 0.3566 0.053 Uiso 1 1 calc R . . C8 C 0.3834(3) 0.37786(13) 0.4262(2) 0.0297(14) Uani 1 1 d . . . C17 C 1.1505(3) 0.34404(19) 0.3989(3) 0.049(2) Uani 1 1 d . . . C12 C 1.0807(3) 0.33212(15) 0.3916(2) 0.0317(14) Uani 1 1 d . . . C18 C 0.9983(3) 0.27411(14) 0.3140(2) 0.0246(12) Uani 1 1 d . . . C20 C 0.1742(3) 0.47493(15) 0.3661(2) 0.0337(14) Uani 1 1 d . . . H20 H 0.1613 0.4563 0.3527 0.040 Uiso 1 1 calc R . . C13 C 1.0710(3) 0.30829(14) 0.3600(2) 0.0290(13) Uani 1 1 d . . . H13 H 1.1091 0.2992 0.3455 0.035 Uiso 1 1 calc R . . C15 C 0.9513(3) 0.31109(13) 0.3708(2) 0.0268(13) Uani 1 1 d . . . H15 H 0.9070 0.3044 0.3632 0.032 Uiso 1 1 calc R . . C24 C 0.2417(3) 0.50352(16) 0.4201(2) 0.0346(15) Uani 1 1 d . . . H24 H 0.2748 0.5045 0.4441 0.042 Uiso 1 1 calc R . . C23 C 0.2107(4) 0.53007(18) 0.4032(3) 0.0471(19) Uani 1 1 d . . . C7 C 0.4978(3) 0.30700(14) 0.3136(2) 0.0274(13) Uani 1 1 d . . . C25 C 0.2508(3) 0.44767(15) 0.4212(2) 0.0297(13) Uani 1 1 d . . . C16 C 0.9005(3) 0.35060(15) 0.4238(2) 0.0331(15) Uani 1 1 d . . . C26 C 0.0931(3) 0.50045(15) 0.3128(2) 0.0320(14) Uani 1 1 d . . . C21 C 0.1448(4) 0.50148(15) 0.3510(2) 0.0354(15) Uani 1 1 d . . . C9 C 0.6350(4) 0.36925(18) 0.4253(2) 0.0402(17) Uani 1 1 d . . . C27 C 0.2289(5) 0.5592(2) 0.4270(4) 0.070(3) Uani 1 1 d . . . O18A O 0.2104(3) 0.58481(16) 0.4011(3) 0.0394(16) Uani 0.70 1 d P . . O8A O 0.8440(7) 0.3490(3) 0.4001(5) 0.035(3) Uani 0.50 1 d P . . Zn5A Zn 0.77434(7) 0.37411(3) 0.57258(5) 0.0180(3) Uani 0.50 1 d P . . Zn5B Zn 0.76466(8) 0.34558(4) 0.53587(6) 0.0289(4) Uani 0.50 1 d P . . O10A O 1.1926(5) 0.3439(2) 0.3654(4) 0.062(3) Uani 0.70 1 d P . . O20 O 0.7442(6) 0.3106(2) 0.5000 0.076(3) Uani 1 2 d S . . O19 O 0.6723(3) 0.26788(14) 0.2569(2) 0.0591(16) Uani 1 1 d . . . O23 O 0.4242(5) 0.4525(2) 0.5000 0.074(3) Uani 1 2 d S . . O25 O 0.0000 0.57470(18) 0.2500 0.097(4) Uani 1 2 d S . . O21 O 0.9159(10) 0.4309(3) 0.5000 0.233(14) Uani 1 2 d S . . O18B O 0.1731(9) 0.5747(3) 0.4356(5) 0.039(4) Uani 0.30 1 d P . . O8B O 0.8446(8) 0.3379(5) 0.4220(9) 0.102(9) Uani 0.50 1 d P . . O10B O 1.1992(12) 0.3266(8) 0.3912(15) 0.113(15) Uani 0.30 1 d P . . O24 O 0.2555(3) 0.39569(16) 0.5000 0.0356(15) Uani 1 2 d S . . O14 O 0.2974(3) 0.45082(13) 0.4513(2) 0.0532(14) Uani 1 1 d . . . O6 O 0.6855(3) 0.3576(2) 0.4097(3) 0.104(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0075(4) 0.0141(4) 0.0192(4) 0.0006(2) 0.0014(2) -0.0001(2) Zn7 0.0125(5) 0.0187(5) 0.0159(5) 0.000 0.0005(4) 0.000 Zn4 0.0101(5) 0.0161(5) 0.0238(5) 0.000 0.000 -0.0016(4) Zn3 0.0105(5) 0.0152(5) 0.0288(6) 0.000 0.000 0.0012(4) Zn2 0.0162(4) 0.0268(5) 0.0558(6) -0.0083(4) -0.0016(4) -0.0004(3) Zn6 0.0269(7) 0.0284(7) 0.1184(15) 0.000 0.000 0.0003(5) O4 0.043(3) 0.075(4) 0.104(5) -0.057(4) 0.017(3) -0.008(3) O2 0.026(2) 0.030(2) 0.035(2) -0.0093(18) -0.0052(18) -0.0007(17) O12 0.025(2) 0.034(2) 0.038(2) -0.0112(19) 0.0043(19) -0.0055(18) O1 0.031(2) 0.036(2) 0.031(2) -0.0106(19) 0.0012(19) 0.0025(19) O3 0.023(2) 0.033(2) 0.048(3) -0.010(2) 0.000(2) 0.0038(18) O22 0.016(3) 0.021(3) 0.047(4) 0.000 0.000 -0.001(2) O17 0.056(3) 0.038(3) 0.054(3) -0.014(2) -0.028(3) 0.012(2) O15 0.041(3) 0.042(3) 0.039(3) 0.000(2) -0.017(2) 0.007(2) O13 0.034(2) 0.034(2) 0.047(3) -0.010(2) -0.016(2) 0.002(2) O16 0.039(3) 0.043(3) 0.038(3) -0.009(2) -0.018(2) 0.000(2) O11 0.020(2) 0.032(2) 0.036(2) -0.0103(18) 0.0042(18) 0.0047(17) O9 0.020(2) 0.041(3) 0.066(3) -0.021(2) 0.000(2) -0.0012(19) O5 0.032(3) 0.051(3) 0.066(4) -0.027(3) -0.018(2) 0.005(2) O7 0.029(3) 0.039(3) 0.081(4) -0.026(3) 0.010(3) -0.003(2) C11 0.022(3) 0.026(3) 0.034(3) -0.013(2) -0.001(3) 0.001(2) C4 0.023(3) 0.036(3) 0.030(3) -0.014(3) 0.002(2) -0.005(2) C14 0.022(3) 0.029(3) 0.025(3) -0.012(2) 0.006(2) 0.002(2) C2 0.016(3) 0.027(3) 0.032(3) -0.013(2) -0.003(2) -0.001(2) C10 0.018(3) 0.033(3) 0.036(3) -0.011(3) 0.004(3) 0.002(2) C6 0.023(3) 0.044(4) 0.031(3) -0.009(3) 0.002(3) 0.006(3) C19 0.029(3) 0.038(4) 0.034(3) -0.004(3) -0.012(3) 0.005(3) C3 0.019(3) 0.033(3) 0.031(3) -0.007(3) 0.003(2) -0.001(2) C5 0.015(3) 0.042(4) 0.036(3) -0.011(3) -0.001(2) 0.000(2) C1 0.021(3) 0.032(3) 0.023(3) -0.009(2) -0.001(2) -0.002(2) C22 0.043(4) 0.037(4) 0.052(4) -0.008(3) -0.021(4) 0.007(3) C8 0.017(3) 0.020(3) 0.052(4) -0.009(3) 0.006(3) -0.005(2) C17 0.018(3) 0.054(5) 0.074(5) -0.030(4) 0.003(3) -0.010(3) C12 0.016(3) 0.034(3) 0.046(4) -0.011(3) -0.002(3) -0.006(2) C18 0.022(3) 0.025(3) 0.027(3) -0.010(2) -0.001(2) 0.001(2) C20 0.034(3) 0.036(3) 0.031(3) -0.007(3) -0.008(3) -0.002(3) C13 0.017(3) 0.030(3) 0.040(3) -0.009(3) 0.003(2) 0.001(2) C15 0.016(3) 0.026(3) 0.038(3) -0.012(3) 0.004(2) -0.004(2) C24 0.028(3) 0.043(4) 0.034(3) -0.009(3) -0.012(3) 0.005(3) C23 0.042(4) 0.042(4) 0.057(5) -0.019(4) -0.015(4) 0.011(3) C7 0.030(3) 0.027(3) 0.025(3) -0.007(2) 0.001(2) -0.003(2) C25 0.022(3) 0.033(3) 0.034(3) 0.001(3) -0.009(3) 0.002(2) C16 0.019(3) 0.034(3) 0.046(4) -0.020(3) 0.009(3) -0.001(3) C26 0.026(3) 0.039(4) 0.030(3) -0.008(3) -0.005(3) 0.004(3) C21 0.039(4) 0.035(3) 0.032(3) -0.006(3) -0.011(3) 0.011(3) C9 0.026(3) 0.058(5) 0.037(4) -0.021(3) 0.006(3) -0.006(3) C27 0.061(6) 0.048(5) 0.101(8) -0.034(5) -0.047(6) 0.019(4) O18A 0.033(3) 0.042(4) 0.043(4) 0.006(3) -0.003(3) -0.004(3) O8A 0.024(5) 0.038(6) 0.044(6) 0.008(5) -0.001(4) 0.008(4) Zn5A 0.0113(7) 0.0170(7) 0.0257(7) 0.0049(5) -0.0024(5) 0.0009(5) Zn5B 0.0197(8) 0.0253(8) 0.0418(9) 0.0038(7) -0.0010(7) 0.0020(6) O10A 0.033(5) 0.065(6) 0.089(8) -0.020(5) 0.010(5) 0.003(4) O20 0.080(7) 0.046(5) 0.102(8) 0.000 0.000 -0.002(5) O19 0.036(3) 0.067(4) 0.075(4) 0.009(3) -0.012(3) -0.003(3) O23 0.070(6) 0.054(5) 0.097(7) 0.000 0.000 -0.033(5) O25 0.141(12) 0.016(4) 0.134(11) 0.000 -0.006(8) 0.000 O21 0.131(15) 0.055(8) 0.51(5) 0.000 0.000 -0.058(9) O18B 0.050(10) 0.034(8) 0.034(8) -0.016(6) -0.014(8) 0.003(7) O8B 0.028(7) 0.090(14) 0.19(2) -0.110(15) -0.009(12) 0.005(9) O10B 0.025(11) 0.12(3) 0.19(4) -0.10(3) -0.027(17) 0.036(15) O24 0.023(3) 0.046(4) 0.038(4) 0.000 0.000 -0.006(3) O14 0.047(3) 0.055(3) 0.058(3) 0.009(3) -0.032(3) -0.008(3) O6 0.024(3) 0.151(8) 0.137(7) -0.110(7) -0.012(4) 0.012(4) _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 O19 1.946(6) . ? Zn1 O2 2.015(4) 4_655 ? Zn1 O11 2.016(4) 16_455 ? Zn1 O1 2.054(4) . ? Zn1 O12 2.060(4) 13_655 ? Zn1 Zn1 2.9712(13) 4_655 ? Zn7 O25 1.871(8) . ? Zn7 O15 2.003(5) 4 ? Zn7 O15 2.003(5) . ? Zn7 O16 2.060(4) 3_565 ? Zn7 O16 2.060(4) 2_565 ? Zn7 Zn7 2.938(2) 2_565 ? Zn4 O22 1.952(6) . ? Zn4 O5 2.035(5) . ? Zn4 O5 2.035(5) 10_556 ? Zn4 O17 2.036(5) 9_666 ? Zn4 O17 2.036(5) 2_665 ? Zn4 Zn5A 2.9413(15) 10_556 ? Zn4 Zn5A 2.9413(15) . ? Zn3 O23 2.007(9) . ? Zn3 O14 2.018(5) 10_556 ? Zn3 O14 2.018(5) . ? Zn3 O4 2.038(6) 10_556 ? Zn3 O4 2.038(6) . ? Zn3 O24 2.184(6) . ? Zn2 O9 1.930(5) 1_455 ? Zn2 O3 1.936(4) . ? Zn2 O13 1.967(5) . ? Zn2 O24 1.981(2) . ? Zn6 O21 1.836(12) . ? Zn6 O22 1.908(6) . ? Zn6 O7 2.092(5) . ? Zn6 O7 2.092(5) 10_556 ? Zn6 O18B 2.346(15) 2_665 ? Zn6 O18B 2.346(15) 9_666 ? Zn6 Zn5A 2.9070(17) 10_556 ? Zn6 Zn5A 2.9070(17) . ? O4 C8 1.220(8) . ? O2 C7 1.259(7) . ? O2 Zn1 2.015(4) 4_655 ? O12 C18 1.261(7) . ? O12 Zn1 2.060(4) 13_655 ? O1 C7 1.256(8) . ? O3 C8 1.277(8) . ? O22 Zn5B 1.825(5) 10_556 ? O22 Zn5B 1.825(5) . ? O22 Zn5A 2.0895(16) 10_556 ? O22 Zn5A 2.0895(16) . ? O17 C27 1.202(10) . ? O17 Zn4 2.036(5) 9_666 ? O15 C26 1.254(8) . ? O13 C25 1.238(8) . ? O16 C26 1.243(8) . ? O16 Zn7 2.060(4) 2_565 ? O11 C18 1.272(7) . ? O11 Zn1 2.016(4) 16 ? O9 C17 1.248(9) . ? O9 Zn2 1.930(5) 1_655 ? O5 C9 1.239(9) . ? O7 C16 1.201(8) . ? C11 C12 1.387(9) . ? C11 C10 1.393(9) . ? C11 H11 0.9500 . ? C4 C5 1.394(9) . ? C4 C3 1.398(9) . ? C4 H4 0.9500 . ? C14 C15 1.378(8) . ? C14 C13 1.384(8) . ? C14 C18 1.491(8) . ? C2 C3 1.386(8) . ? C2 C1 1.399(8) . ? C2 H2 0.9500 . ? C10 C15 1.385(8) . ? C10 C16 1.512(8) . ? C6 C1 1.377(9) . ? C6 C5 1.393(9) . ? C6 H6 0.9500 . ? C19 C24 1.388(10) . ? C19 C20 1.400(9) . ? C19 C25 1.495(9) . ? C3 C8 1.505(8) . ? C5 C9 1.509(9) . ? C1 C7 1.521(8) . ? C22 C23 1.347(11) . ? C22 C21 1.356(10) . ? C22 H22 0.9500 . ? C17 O10B 1.26(2) . ? C17 O10A 1.268(13) . ? C17 C12 1.493(8) . ? C12 C13 1.411(9) . ? C20 C21 1.391(9) . ? C20 H20 0.9500 . ? C13 H13 0.9500 . ? C15 H15 0.9500 . ? C24 C23 1.421(11) . ? C24 H24 0.9500 . ? C23 C27 1.512(11) . ? C25 O14 1.271(8) . ? C16 O8B 1.244(18) . ? C16 O8A 1.309(16) . ? C26 C21 1.499(9) . ? C9 O6 1.213(9) . ? C27 O18B 1.33(2) . ? C27 O18A 1.415(12) . ? O18A O18B 1.314(19) . ? O18A Zn5A 2.008(7) 9_666 ? O8A O8B 0.80(3) . ? O8A Zn5A 1.942(15) 10_556 ? O8A Zn5B 2.418(14) 10_556 ? Zn5A Zn5B 1.664(2) . ? Zn5A O8A 1.942(15) 10_556 ? Zn5A O6 1.972(6) 10_556 ? Zn5A O18A 2.008(7) 9_666 ? Zn5A O8B 2.137(18) 10_556 ? Zn5B O20 1.913(8) . ? Zn5B O8B 2.018(19) 10_556 ? Zn5B Zn5B 2.054(4) 10_556 ? Zn5B O6 2.274(9) 10_556 ? Zn5B O8A 2.418(14) 10_556 ? O10A O10B 1.08(5) . ? O20 Zn5B 1.913(8) 10_556 ? O18B Zn6 2.346(15) 9_666 ? O8B Zn5B 2.018(19) 10_556 ? O8B Zn5A 2.137(18) 10_556 ? O24 Zn2 1.981(2) 10_556 ? O6 Zn5A 1.972(6) 10_556 ? O6 Zn5B 2.274(9) 10_556 ? 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 O19 Zn1 O2 102.7(2) . 4_655 ? O19 Zn1 O11 98.5(2) . 16_455 ? O2 Zn1 O11 158.71(18) 4_655 16_455 ? O19 Zn1 O1 94.8(2) . . ? O2 Zn1 O1 88.20(19) 4_655 . ? O11 Zn1 O1 87.75(19) 16_455 . ? O19 Zn1 O12 105.5(2) . 13_655 ? O2 Zn1 O12 88.42(19) 4_655 13_655 ? O11 Zn1 O12 88.13(19) 16_455 13_655 ? O1 Zn1 O12 159.59(18) . 13_655 ? O19 Zn1 Zn1 167.9(2) . 4_655 ? O2 Zn1 Zn1 84.19(13) 4_655 4_655 ? O11 Zn1 Zn1 74.57(12) 16_455 4_655 ? O1 Zn1 Zn1 75.24(13) . 4_655 ? O12 Zn1 Zn1 84.39(12) 13_655 4_655 ? O25 Zn7 O15 100.53(15) . 4 ? O25 Zn7 O15 100.53(15) . . ? O15 Zn7 O15 158.9(3) 4 . ? O25 Zn7 O16 100.71(14) . 3_565 ? O15 Zn7 O16 88.2(2) 4 3_565 ? O15 Zn7 O16 87.9(2) . 3_565 ? O25 Zn7 O16 100.71(14) . 2_565 ? O15 Zn7 O16 87.9(2) 4 2_565 ? O15 Zn7 O16 88.2(2) . 2_565 ? O16 Zn7 O16 158.6(3) 3_565 2_565 ? O25 Zn7 Zn7 180.000(1) . 2_565 ? O15 Zn7 Zn7 79.47(15) 4 2_565 ? O15 Zn7 Zn7 79.47(15) . 2_565 ? O16 Zn7 Zn7 79.29(14) 3_565 2_565 ? O16 Zn7 Zn7 79.29(14) 2_565 2_565 ? O22 Zn4 O5 104.70(19) . . ? O22 Zn4 O5 104.70(19) . 10_556 ? O5 Zn4 O5 84.8(4) . 10_556 ? O22 Zn4 O17 107.66(19) . 9_666 ? O5 Zn4 O17 147.6(2) . 9_666 ? O5 Zn4 O17 86.4(3) 10_556 9_666 ? O22 Zn4 O17 107.66(19) . 2_665 ? O5 Zn4 O17 86.4(3) . 2_665 ? O5 Zn4 O17 147.6(2) 10_556 2_665 ? O17 Zn4 O17 84.5(3) 9_666 2_665 ? O22 Zn4 Zn5A 45.17(3) . 10_556 ? O5 Zn4 Zn5A 70.10(16) . 10_556 ? O5 Zn4 Zn5A 127.74(18) 10_556 10_556 ? O17 Zn4 Zn5A 136.96(19) 9_666 10_556 ? O17 Zn4 Zn5A 77.32(15) 2_665 10_556 ? O22 Zn4 Zn5A 45.17(3) . . ? O5 Zn4 Zn5A 127.74(18) . . ? O5 Zn4 Zn5A 70.10(16) 10_556 . ? O17 Zn4 Zn5A 77.32(15) 9_666 . ? O17 Zn4 Zn5A 136.96(19) 2_665 . ? Zn5A Zn4 Zn5A 89.90(6) 10_556 . ? O23 Zn3 O14 90.9(3) . 10_556 ? O23 Zn3 O14 90.9(3) . . ? O14 Zn3 O14 87.4(4) 10_556 . ? O23 Zn3 O4 88.2(3) . 10_556 ? O14 Zn3 O4 91.7(3) 10_556 10_556 ? O14 Zn3 O4 178.7(3) . 10_556 ? O23 Zn3 O4 88.2(3) . . ? O14 Zn3 O4 178.7(3) 10_556 . ? O14 Zn3 O4 91.7(3) . . ? O4 Zn3 O4 89.2(5) 10_556 . ? O23 Zn3 O24 180.0(4) . . ? O14 Zn3 O24 89.1(2) 10_556 . ? O14 Zn3 O24 89.1(2) . . ? O4 Zn3 O24 91.8(2) 10_556 . ? O4 Zn3 O24 91.8(2) . . ? O9 Zn2 O3 122.3(2) 1_455 . ? O9 Zn2 O13 106.8(2) 1_455 . ? O3 Zn2 O13 114.1(2) . . ? O9 Zn2 O24 106.6(2) 1_455 . ? O3 Zn2 O24 105.5(2) . . ? O13 Zn2 O24 98.7(2) . . ? O21 Zn6 O22 149.8(7) . . ? O21 Zn6 O7 100.7(5) . . ? O22 Zn6 O7 100.75(19) . . ? O21 Zn6 O7 100.7(5) . 10_556 ? O22 Zn6 O7 100.75(19) . 10_556 ? O7 Zn6 O7 88.8(4) . 10_556 ? O21 Zn6 O18B 74.4(6) . 2_665 ? O22 Zn6 O18B 87.3(4) . 2_665 ? O7 Zn6 O18B 83.4(4) . 2_665 ? O7 Zn6 O18B 169.7(4) 10_556 2_665 ? O21 Zn6 O18B 74.4(6) . 9_666 ? O22 Zn6 O18B 87.3(4) . 9_666 ? O7 Zn6 O18B 169.7(4) . 9_666 ? O7 Zn6 O18B 83.4(4) 10_556 9_666 ? O18B Zn6 O18B 103.5(8) 2_665 9_666 ? O21 Zn6 Zn5A 129.3(3) . 10_556 ? O22 Zn6 Zn5A 45.86(4) . 10_556 ? O7 Zn6 Zn5A 65.54(15) . 10_556 ? O7 Zn6 Zn5A 125.85(17) 10_556 10_556 ? O18B Zn6 Zn5A 56.3(4) 2_665 10_556 ? O18B Zn6 Zn5A 124.6(4) 9_666 10_556 ? O21 Zn6 Zn5A 129.3(3) . . ? O22 Zn6 Zn5A 45.86(4) . . ? O7 Zn6 Zn5A 125.85(17) . . ? O7 Zn6 Zn5A 65.54(15) 10_556 . ? O18B Zn6 Zn5A 124.6(4) 2_665 . ? O18B Zn6 Zn5A 56.3(4) 9_666 . ? Zn5A Zn6 Zn5A 91.26(7) 10_556 . ? C8 O4 Zn3 142.3(5) . . ? C7 O2 Zn1 121.9(4) . 4_655 ? C18 O12 Zn1 120.3(4) . 13_655 ? C7 O1 Zn1 131.9(4) . . ? C8 O3 Zn2 120.1(4) . . ? Zn5B O22 Zn5B 68.5(2) 10_556 . ? Zn5B O22 Zn6 117.1(3) 10_556 . ? Zn5B O22 Zn6 117.1(3) . . ? Zn5B O22 Zn4 116.3(3) 10_556 . ? Zn5B O22 Zn4 116.3(3) . . ? Zn6 O22 Zn4 114.2(3) . . ? Zn5B O22 Zn5A 49.74(9) 10_556 10_556 ? Zn5B O22 Zn5A 118.2(3) . 10_556 ? Zn6 O22 Zn5A 93.19(16) . 10_556 ? Zn4 O22 Zn5A 93.34(16) . 10_556 ? Zn5B O22 Zn5A 118.2(3) 10_556 . ? Zn5B O22 Zn5A 49.74(9) . . ? Zn6 O22 Zn5A 93.19(16) . . ? Zn4 O22 Zn5A 93.34(16) . . ? Zn5A O22 Zn5A 168.0(3) 10_556 . ? C27 O17 Zn4 126.8(5) . 9_666 ? C26 O15 Zn7 128.6(4) . . ? C25 O13 Zn2 126.6(4) . . ? C26 O16 Zn7 126.5(4) . 2_565 ? C18 O11 Zn1 135.1(4) . 16 ? C17 O9 Zn2 117.3(5) . 1_655 ? C9 O5 Zn4 134.1(5) . . ? C16 O7 Zn6 139.2(5) . . ? C12 C11 C10 120.7(5) . . ? C12 C11 H11 119.7 . . ? C10 C11 H11 119.7 . . ? C5 C4 C3 120.2(6) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? C15 C14 C13 120.0(5) . . ? C15 C14 C18 121.1(5) . . ? C13 C14 C18 118.9(5) . . ? C3 C2 C1 119.3(5) . . ? C3 C2 H2 120.3 . . ? C1 C2 H2 120.3 . . ? C15 C10 C11 119.9(5) . . ? C15 C10 C16 122.1(5) . . ? C11 C10 C16 117.6(5) . . ? C1 C6 C5 120.1(6) . . ? C1 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C24 C19 C20 119.6(6) . . ? C24 C19 C25 120.5(6) . . ? C20 C19 C25 119.7(6) . . ? C2 C3 C4 120.1(5) . . ? C2 C3 C8 122.4(5) . . ? C4 C3 C8 117.5(5) . . ? C6 C5 C4 119.5(6) . . ? C6 C5 C9 120.7(6) . . ? C4 C5 C9 119.7(6) . . ? C6 C1 C2 120.7(5) . . ? C6 C1 C7 120.0(5) . . ? C2 C1 C7 119.2(5) . . ? C23 C22 C21 121.5(7) . . ? C23 C22 H22 119.2 . . ? C21 C22 H22 119.2 . . ? O4 C8 O3 126.0(6) . . ? O4 C8 C3 118.4(6) . . ? O3 C8 C3 115.5(5) . . ? O9 C17 O10B 117.1(15) . . ? O9 C17 O10A 118.9(8) . . ? O10B C17 O10A 50(2) . . ? O9 C17 C12 116.5(6) . . ? O10B C17 C12 117.5(15) . . ? O10A C17 C12 119.9(8) . . ? C11 C12 C13 118.4(5) . . ? C11 C12 C17 122.5(6) . . ? C13 C12 C17 119.0(6) . . ? O12 C18 O11 124.8(5) . . ? O12 C18 C14 119.0(5) . . ? O11 C18 C14 116.2(5) . . ? C21 C20 C19 118.8(6) . . ? C21 C20 H20 120.6 . . ? C19 C20 H20 120.6 . . ? C14 C13 C12 120.6(5) . . ? C14 C13 H13 119.7 . . ? C12 C13 H13 119.7 . . ? C14 C15 C10 120.3(5) . . ? C14 C15 H15 119.8 . . ? C10 C15 H15 119.8 . . ? C19 C24 C23 119.5(6) . . ? C19 C24 H24 120.3 . . ? C23 C24 H24 120.3 . . ? C22 C23 C24 119.4(7) . . ? C22 C23 C27 123.0(7) . . ? C24 C23 C27 117.5(7) . . ? O1 C7 O2 126.5(6) . . ? O1 C7 C1 116.7(5) . . ? O2 C7 C1 116.8(5) . . ? O13 C25 O14 126.4(6) . . ? O13 C25 C19 118.2(5) . . ? O14 C25 C19 115.4(6) . . ? O7 C16 O8B 123.2(9) . . ? O7 C16 O8A 120.8(9) . . ? O8B C16 O8A 36.3(13) . . ? O7 C16 C10 118.4(6) . . ? O8B C16 C10 116.6(8) . . ? O8A C16 C10 115.5(8) . . ? O16 C26 O15 124.5(6) . . ? O16 C26 C21 118.4(6) . . ? O15 C26 C21 117.0(6) . . ? C22 C21 C20 121.1(6) . . ? C22 C21 C26 119.8(6) . . ? C20 C21 C26 119.1(6) . . ? O6 C9 O5 124.9(7) . . ? O6 C9 C5 118.1(6) . . ? O5 C9 C5 116.2(6) . . ? O17 C27 O18B 122.3(10) . . ? O17 C27 O18A 119.2(9) . . ? O18B C27 O18A 57.2(9) . . ? O17 C27 C23 119.7(7) . . ? O18B C27 C23 109.6(10) . . ? O18A C27 C23 113.5(8) . . ? O18B O18A C27 58.0(9) . . ? O18B O18A Zn5A 96.8(7) . 9_666 ? C27 O18A Zn5A 120.4(6) . 9_666 ? O8B O8A C16 67.5(18) . . ? O8B O8A Zn5A 93(2) . 10_556 ? C16 O8A Zn5A 111.4(10) . 10_556 ? O8B O8A Zn5B 51.3(18) . 10_556 ? C16 O8A Zn5B 99.5(8) . 10_556 ? Zn5A O8A Zn5B 43.2(3) 10_556 10_556 ? Zn5B Zn5A O8A 83.8(3) . 10_556 ? Zn5B Zn5A O6 76.9(4) . 10_556 ? O8A Zn5A O6 108.2(5) 10_556 10_556 ? Zn5B Zn5A O18A 162.9(2) . 9_666 ? O8A Zn5A O18A 105.7(4) 10_556 9_666 ? O6 Zn5A O18A 112.3(4) 10_556 9_666 ? Zn5B Zn5A O22 56.84(17) . . ? O8A Zn5A O22 116.8(4) 10_556 . ? O6 Zn5A O22 107.8(3) 10_556 . ? O18A Zn5A O22 106.0(3) 9_666 . ? Zn5B Zn5A O8B 62.7(8) . 10_556 ? O8A Zn5A O8B 21.9(8) 10_556 10_556 ? O6 Zn5A O8B 106.1(5) 10_556 10_556 ? O18A Zn5A O8B 124.5(7) 9_666 10_556 ? O22 Zn5A O8B 98.2(7) . 10_556 ? Zn5B Zn5A Zn6 83.61(8) . . ? O8A Zn5A Zn6 93.7(5) 10_556 . ? O6 Zn5A Zn6 148.6(3) 10_556 . ? O18A Zn5A Zn6 81.6(2) 9_666 . ? O22 Zn5A Zn6 40.95(16) . . ? O8B Zn5A Zn6 85.9(5) 10_556 . ? Zn5B Zn5A Zn4 83.41(8) . . ? O8A Zn5A Zn4 158.1(4) 10_556 . ? O6 Zn5A Zn4 86.06(19) 10_556 . ? O18A Zn5A Zn4 82.9(2) 9_666 . ? O22 Zn5A Zn4 41.49(16) . . ? O8B Zn5A Zn4 139.1(7) 10_556 . ? Zn6 Zn5A Zn4 67.30(4) . . ? Zn5A Zn5B O22 73.42(13) . . ? Zn5A Zn5B O20 171.7(3) . . ? O22 Zn5B O20 113.0(2) . . ? Zn5A Zn5B O8B 70.2(8) . 10_556 ? O22 Zn5B O8B 112.5(5) . 10_556 ? O20 Zn5B O8B 110.4(8) . 10_556 ? Zn5A Zn5B Zn5B 129.18(8) . 10_556 ? O22 Zn5B Zn5B 55.76(11) . 10_556 ? O20 Zn5B Zn5B 57.54(16) . 10_556 ? O8B Zn5B Zn5B 126.8(7) 10_556 10_556 ? Zn5A Zn5B O6 57.6(3) . 10_556 ? O22 Zn5B O6 105.9(2) . 10_556 ? O20 Zn5B O6 114.6(4) . 10_556 ? O8B Zn5B O6 99.7(8) 10_556 10_556 ? Zn5B Zn5B O6 133.29(19) 10_556 10_556 ? Zn5A Zn5B O8A 53.0(3) . 10_556 ? O22 Zn5B O8A 107.3(4) . 10_556 ? O20 Zn5B O8A 126.6(4) . 10_556 ? O8B Zn5B O8A 18.0(8) 10_556 10_556 ? Zn5B Zn5B O8A 139.3(3) 10_556 10_556 ? O6 Zn5B O8A 85.0(4) 10_556 10_556 ? O10B O10A C17 64.4(17) . . ? Zn5B O20 Zn5B 64.9(3) . 10_556 ? O18A O18B C27 64.8(11) . . ? O18A O18B Zn6 125.2(10) . 9_666 ? C27 O18B Zn6 132.9(10) . 9_666 ? O8A O8B C16 76(2) . . ? O8A O8B Zn5B 111(2) . 10_556 ? C16 O8B Zn5B 126.4(11) . 10_556 ? O8A O8B Zn5A 65.2(19) . 10_556 ? C16 O8B Zn5A 103.3(12) . 10_556 ? Zn5B O8B Zn5A 47.1(3) 10_556 10_556 ? O10A O10B C17 65.2(18) . . ? Zn2 O24 Zn2 145.5(4) . 10_556 ? Zn2 O24 Zn3 105.29(18) . . ? Zn2 O24 Zn3 105.29(18) 10_556 . ? C25 O14 Zn3 137.1(5) . . ? C9 O6 Zn5A 118.6(5) . 10_556 ? C9 O6 Zn5B 114.6(7) . 10_556 ? Zn5A O6 Zn5B 45.46(16) 10_556 10_556 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 65.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 2.533 _refine_diff_density_min -1.258 _refine_diff_density_rms 0.202 _database_code_depnum_ccdc_archive 'CCDC 967656'