# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1795 data_ZNBPYO _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H44 F6 N6 O11 Si Zn' _chemical_formula_weight 932.22 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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.174(3) _cell_length_b 28.313(5) _cell_length_c 13.865(4) _cell_angle_alpha 90.00 _cell_angle_beta 92.06(3) _cell_angle_gamma 90.00 _cell_volume 3991(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 56 _cell_measurement_theta_min 25 _cell_measurement_theta_max 35 _exptl_crystal_description Tablet _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.55 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1928 _exptl_absorpt_coefficient_mu 0.74 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.825 # VALUE FROM DATA SUMMARY SHEET _exptl_absorpt_correction_T_max 0.915 # VALUE FROM DATA SUMMARY SHEET _exptl_absorpt_process_details 'X-RED (Stoe & Cie, 1997b)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe Stadi-4 four-circle' _diffrn_measurement_method omega/theta _diffrn_detector_area_resol_mean MoK\a _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 'random variation +/-4.2' _diffrn_reflns_number 7821 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_av_sigmaI/netI 0.0895 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 25.99 _reflns_number_total 7821 _reflns_number_gt 5277 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe STADI4 v1.07 (Stoe & Cie, 1997a)' _computing_cell_refinement 'Stoe STADI4' _computing_data_reduction 'X-RED v1.09 (Stoe & Cie, 1997b)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC v5.03 (Sheldrick, 1994)' _computing_publication_material 'SHELXL-97; PLATON (Spek, 1998)' _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^)+21.158P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'heavy atom' _atom_sites_solution_secondary 'difference Fourier' _atom_sites_solution_hydrogens 'methanol H atoms from delta-F, others placed geometrically' _refine_ls_hydrogen_treatment 'methanol H atoms in rigid group, others riding' _refine_ls_extinction_method none _refine_ls_extinction_coef none _refine_ls_number_reflns 7821 _refine_ls_number_parameters 551 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.139 _refine_ls_R_factor_gt 0.0830 _refine_ls_wR_factor_ref 0.166 _refine_ls_wR_factor_gt 0.131 _refine_ls_goodness_of_fit_ref 1.255 _refine_ls_restrained_S_all 1.255 _refine_ls_shift/su_max <0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn Zn 0.53046(7) 0.78720(3) 0.08672(5) 0.01571(17) Uani 1 1 d . . . O1 O 0.4605(5) 0.73243(17) 0.0020(3) 0.0289(11) Uani 1 1 d . . . H1M H 0.5012 0.7068 -0.0031 0.043 Uiso 1 1 calc R . . O2 O 0.6054(4) 0.84314(16) 0.1723(3) 0.0226(10) Uani 1 1 d . . . H2M H 0.5591 0.8663 0.1878 0.034 Uiso 1 1 calc R . . O3 O 0.8928(6) 1.0689(3) -0.4324(5) 0.0635(19) Uani 1 1 d . . . H3M H 0.9262 1.0862 -0.4741 0.095 Uiso 1 1 calc R . . O4 O -0.0687(5) 0.6200(2) 0.4507(4) 0.0472(16) Uani 1 1 d . . . H4M H -0.0425 0.6142 0.3951 0.071 Uiso 1 1 calc R . . O5 O 0.1296(6) 0.5034(3) 0.3559(7) 0.093(3) Uani 1 1 d . . . H5M H 0.1069 0.5309 0.3396 0.140 Uiso 1 1 calc R . . O10 O 0.5047(4) 0.74889(15) 0.2128(3) 0.0215(10) Uani 1 1 d . . . O20 O 0.5540(5) 0.40824(17) 0.2595(4) 0.0424(15) Uani 1 1 d . . . O30 O 0.3391(4) 0.81589(16) 0.0900(3) 0.0221(10) Uani 1 1 d . . . O40 O 0.7234(4) 0.75976(16) 0.0835(3) 0.0217(10) Uani 1 1 d . . . O50 O 0.5402(4) 0.83036(14) -0.0364(3) 0.0177(10) Uani 1 1 d . . . O60 O 0.6209(5) 0.66453(17) -0.0301(4) 0.0373(13) Uani 1 1 d . . . N10 N 0.5133(5) 0.70213(17) 0.2161(3) 0.0165(11) Uani 1 1 d . . . N20 N 0.5473(5) 0.4542(2) 0.2552(4) 0.0279(14) Uani 1 1 d . . . N30 N 0.2502(5) 0.80558(19) 0.1557(4) 0.0176(11) Uani 1 1 d . . . N40 N 0.8000(5) 0.74833(19) 0.0110(4) 0.0192(12) Uani 1 1 d . . . N50 N 0.5293(5) 0.87673(17) -0.0250(4) 0.0159(11) Uani 1 1 d . . . N60 N 0.5861(6) 0.6197(2) -0.0208(4) 0.0282(14) Uani 1 1 d . . . C1 C 0.3635(7) 0.7363(3) -0.0742(5) 0.0316(17) Uani 1 1 d . . . H1A H 0.2899 0.7150 -0.0615 0.047 Uiso 1 1 calc R . . H1B H 0.4022 0.7275 -0.1353 0.047 Uiso 1 1 calc R . . H1C H 0.3315 0.7689 -0.0781 0.047 Uiso 1 1 calc R . . C2 C 0.7164(7) 0.8399(3) 0.2364(6) 0.041(2) Uani 1 1 d . . . H2A H 0.7688 0.8688 0.2324 0.062 Uiso 1 1 calc R . . H2B H 0.7700 0.8126 0.2187 0.062 Uiso 1 1 calc R . . H2C H 0.6872 0.8359 0.3025 0.062 Uiso 1 1 calc R . . C3 C 0.9917(11) 1.0396(5) -0.3891(9) 0.095(4) Uani 1 1 d . . . H3A H 0.9504 1.0146 -0.3520 0.143 Uiso 1 1 calc R . . H3B H 1.0488 1.0587 -0.3460 0.143 Uiso 1 1 calc R . . H3C H 1.0442 1.0255 -0.4395 0.143 Uiso 1 1 calc R . . C4 C 0.0333(8) 0.6410(3) 0.5064(6) 0.050(2) Uani 1 1 d . . . H4A H 0.0992 0.6171 0.5247 0.075 Uiso 1 1 calc R . . H4B H -0.0025 0.6548 0.5647 0.075 Uiso 1 1 calc R . . H4C H 0.0745 0.6659 0.4687 0.075 Uiso 1 1 calc R . . C5 C 0.0218(11) 0.4783(5) 0.3793(9) 0.094(4) Uani 1 1 d . . . H5A H -0.0539 0.4995 0.3827 0.141 Uiso 1 1 calc R . . H5B H 0.0378 0.4630 0.4421 0.141 Uiso 1 1 calc R . . H5C H 0.0037 0.4541 0.3300 0.141 Uiso 1 1 calc R . . C11 C 0.6311(6) 0.6805(2) 0.2139(5) 0.0222(15) Uani 1 1 d . . . H11A H 0.7080 0.6990 0.2064 0.027 Uiso 1 1 calc R . . C12 C 0.6426(6) 0.6324(2) 0.2221(5) 0.0210(14) Uani 1 1 d . . . H12A H 0.7269 0.6181 0.2210 0.025 Uiso 1 1 calc R . . C13 C 0.5309(6) 0.6043(2) 0.2320(4) 0.0194(14) Uani 1 1 d . . . C14 C 0.4107(7) 0.6279(2) 0.2348(5) 0.0289(17) Uani 1 1 d . . . H14A H 0.3322 0.6103 0.2424 0.035 Uiso 1 1 calc R . . C15 C 0.4043(7) 0.6762(2) 0.2267(5) 0.0262(16) Uani 1 1 d . . . H15A H 0.3214 0.6915 0.2287 0.031 Uiso 1 1 calc R . . C21 C 0.6587(7) 0.4800(3) 0.2515(6) 0.0331(18) Uani 1 1 d . . . H21A H 0.7411 0.4641 0.2529 0.040 Uiso 1 1 calc R . . C22 C 0.6568(6) 0.5282(2) 0.2457(5) 0.0269(16) Uani 1 1 d . . . H22A H 0.7373 0.5452 0.2451 0.032 Uiso 1 1 calc R . . C23 C 0.5376(6) 0.5526(2) 0.2407(4) 0.0194(14) Uani 1 1 d . . . C24 C 0.4236(6) 0.5251(2) 0.2435(5) 0.0205(14) Uani 1 1 d . . . H24A H 0.3401 0.5401 0.2401 0.025 Uiso 1 1 calc R . . C25 C 0.4299(6) 0.4764(2) 0.2511(5) 0.0204(14) Uani 1 1 d . . . H25A H 0.3511 0.4585 0.2534 0.025 Uiso 1 1 calc R . . C31 C 0.2232(6) 0.8386(2) 0.2219(5) 0.0215(14) Uani 1 1 d . . . H31A H 0.2681 0.8681 0.2222 0.026 Uiso 1 1 calc R . . C32 C 0.1294(6) 0.8295(2) 0.2895(4) 0.0208(14) Uani 1 1 d . . . H32A H 0.1081 0.8534 0.3346 0.025 Uiso 1 1 calc R . . C33 C 0.0665(6) 0.7864(2) 0.2926(4) 0.0171(13) Uani 1 1 d . . . C34 C 0.0983(6) 0.7529(2) 0.2219(5) 0.0216(14) Uani 1 1 d . . . H34A H 0.0564 0.7229 0.2208 0.026 Uiso 1 1 calc R . . C35 C 0.1890(6) 0.7635(2) 0.1548(4) 0.0194(14) Uani 1 1 d . . . H35A H 0.2090 0.7408 0.1070 0.023 Uiso 1 1 calc R . . C41 C 0.8809(6) 0.7111(2) 0.0235(5) 0.0238(14) Uani 1 1 d . . . H41A H 0.8783 0.6928 0.0809 0.029 Uiso 1 1 calc R . . C42 C 0.9675(6) 0.6995(2) -0.0468(5) 0.0214(15) Uani 1 1 d . . . H42A H 1.0253 0.6734 -0.0371 0.026 Uiso 1 1 calc R . . C43 C 0.9717(6) 0.7254(2) -0.1320(5) 0.0180(14) Uani 1 1 d . . . C44 C 0.8850(7) 0.7632(2) -0.1405(5) 0.0251(16) Uani 1 1 d . . . H44A H 0.8852 0.7823 -0.1969 0.030 Uiso 1 1 calc R . . C45 C 0.7993(6) 0.7737(2) -0.0697(5) 0.0243(15) Uani 1 1 d . . . H45A H 0.7392 0.7992 -0.0783 0.029 Uiso 1 1 calc R . . C51 C 0.4092(6) 0.8971(2) -0.0332(5) 0.0218(14) Uani 1 1 d . . . H51A H 0.3335 0.8781 -0.0451 0.026 Uiso 1 1 calc R . . C52 C 0.3959(6) 0.9454(2) -0.0243(5) 0.0210(14) Uani 1 1 d . . . H52A H 0.3113 0.9594 -0.0317 0.025 Uiso 1 1 calc R . . C53 C 0.5064(6) 0.9740(2) -0.0045(4) 0.0168(13) Uani 1 1 d . . . C54 C 0.6278(6) 0.9514(2) 0.0033(5) 0.0226(15) Uani 1 1 d . . . H54A H 0.7052 0.9694 0.0159 0.027 Uiso 1 1 calc R . . C55 C 0.6370(6) 0.9031(2) -0.0071(5) 0.0218(15) Uani 1 1 d . . . H55A H 0.7207 0.8883 -0.0016 0.026 Uiso 1 1 calc R . . C61 C 0.6805(7) 0.5866(3) -0.0091(5) 0.0313(17) Uani 1 1 d . . . H61A H 0.7701 0.5960 -0.0060 0.038 Uiso 1 1 calc R . . C62 C 0.6499(7) 0.5401(3) -0.0019(5) 0.0318(17) Uani 1 1 d . . . H62A H 0.7184 0.5174 0.0050 0.038 Uiso 1 1 calc R . . C63 C 0.5180(7) 0.5252(2) -0.0045(5) 0.0270(16) Uani 1 1 d . . . C64 C 0.4236(7) 0.5603(3) -0.0149(6) 0.0378(19) Uani 1 1 d . . . H64A H 0.3332 0.5519 -0.0168 0.045 Uiso 1 1 calc R . . C65 C 0.4579(8) 0.6071(3) -0.0224(6) 0.039(2) Uani 1 1 d . . . H65A H 0.3915 0.6306 -0.0287 0.046 Uiso 1 1 calc R . . Si Si 1.04031(18) 0.89085(7) -0.30906(14) 0.0237(4) Uani 1 1 d . . . F1 F 0.9319(4) 0.84697(14) -0.2902(3) 0.0302(9) Uani 1 1 d . . . F2 F 0.9551(4) 0.90474(18) -0.4110(4) 0.0550(14) Uani 1 1 d . . . F3 F 1.1338(4) 0.85335(15) -0.3703(3) 0.0362(10) Uani 1 1 d . . . F4 F 0.9448(4) 0.92759(17) -0.2456(4) 0.0599(16) Uani 1 1 d . . . F5 F 1.1234(4) 0.87639(19) -0.2061(3) 0.0468(13) Uani 1 1 d . . . F6 F 1.1460(4) 0.93504(16) -0.3274(4) 0.0545(14) 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 Zn 0.0148(3) 0.0146(3) 0.0180(3) 0.0003(3) 0.0048(3) 0.0005(3) O1 0.035(3) 0.022(3) 0.028(3) -0.009(2) -0.009(2) 0.000(2) O2 0.021(2) 0.019(2) 0.028(3) -0.007(2) -0.003(2) 0.0040(19) O3 0.042(4) 0.088(6) 0.062(5) 0.005(4) 0.016(3) 0.001(4) O4 0.024(3) 0.079(5) 0.039(3) -0.006(3) 0.001(2) -0.008(3) O5 0.036(4) 0.102(7) 0.141(7) 0.075(6) -0.018(4) -0.015(4) O10 0.028(3) 0.017(2) 0.021(2) 0.0027(19) 0.011(2) 0.0014(19) O20 0.031(3) 0.018(3) 0.079(4) 0.012(3) 0.015(3) 0.003(2) O30 0.016(2) 0.027(3) 0.023(2) 0.010(2) 0.0106(19) 0.0039(19) O40 0.018(2) 0.030(3) 0.018(2) 0.0012(19) 0.0094(19) 0.008(2) O50 0.025(2) 0.011(2) 0.018(2) 0.0042(17) 0.0056(19) 0.0034(18) O60 0.034(3) 0.024(3) 0.053(4) -0.011(2) 0.003(3) -0.003(2) N10 0.018(3) 0.019(3) 0.013(3) 0.003(2) 0.006(2) 0.003(2) N20 0.022(3) 0.020(3) 0.042(4) 0.006(3) 0.005(3) 0.002(2) N30 0.010(3) 0.027(3) 0.016(3) 0.005(2) 0.006(2) 0.004(2) N40 0.017(3) 0.026(3) 0.016(3) 0.000(2) 0.004(2) 0.003(2) N50 0.016(3) 0.016(3) 0.015(3) 0.005(2) 0.005(2) 0.001(2) N60 0.032(3) 0.023(3) 0.029(3) -0.005(3) -0.002(3) -0.001(3) C1 0.033(4) 0.034(4) 0.027(4) -0.004(3) -0.003(3) -0.006(3) C2 0.034(5) 0.043(5) 0.046(5) -0.016(4) -0.008(4) 0.012(4) C3 0.057(7) 0.125(12) 0.105(10) 0.040(9) 0.021(7) 0.019(7) C4 0.034(5) 0.076(7) 0.040(5) -0.008(5) -0.004(4) -0.010(5) C5 0.065(8) 0.110(11) 0.105(10) 0.053(8) -0.021(7) -0.024(7) C11 0.014(3) 0.026(4) 0.027(4) 0.007(3) 0.003(3) -0.001(3) C12 0.015(3) 0.026(4) 0.023(4) 0.002(3) 0.004(3) -0.002(3) C13 0.022(3) 0.025(4) 0.011(3) 0.001(3) -0.003(3) 0.000(3) C14 0.014(3) 0.025(4) 0.048(5) 0.008(3) 0.007(3) 0.005(3) C15 0.016(3) 0.026(4) 0.036(4) 0.007(3) 0.003(3) 0.003(3) C21 0.015(3) 0.027(4) 0.058(5) 0.015(4) 0.002(3) 0.007(3) C22 0.017(3) 0.021(4) 0.042(4) 0.011(3) -0.001(3) -0.003(3) C23 0.015(3) 0.024(4) 0.019(3) 0.001(3) 0.000(3) 0.000(3) C24 0.015(3) 0.025(4) 0.022(3) 0.004(3) 0.003(3) 0.003(3) C25 0.017(3) 0.022(3) 0.022(4) 0.003(3) 0.004(3) -0.002(3) C31 0.027(4) 0.017(3) 0.021(3) 0.003(3) 0.003(3) 0.002(3) C32 0.019(3) 0.029(4) 0.016(3) -0.005(3) 0.007(3) -0.001(3) C33 0.012(3) 0.021(3) 0.019(3) 0.002(3) 0.004(2) -0.002(3) C34 0.018(3) 0.025(4) 0.023(3) -0.002(3) 0.002(3) 0.001(3) C35 0.019(3) 0.024(4) 0.015(3) -0.003(3) 0.007(3) 0.002(3) C41 0.024(3) 0.026(4) 0.022(3) 0.003(3) 0.002(3) 0.011(3) C42 0.021(3) 0.019(3) 0.025(4) 0.000(3) 0.008(3) 0.004(3) C43 0.011(3) 0.023(4) 0.020(3) -0.005(3) 0.002(2) -0.004(3) C44 0.035(4) 0.023(4) 0.018(3) 0.011(3) 0.009(3) 0.013(3) C45 0.020(3) 0.030(4) 0.023(4) 0.008(3) 0.006(3) 0.006(3) C51 0.012(3) 0.024(4) 0.030(4) 0.001(3) 0.004(3) -0.004(3) C52 0.016(3) 0.018(3) 0.030(4) 0.006(3) 0.004(3) 0.003(3) C53 0.021(3) 0.016(3) 0.014(3) 0.003(2) 0.001(3) -0.002(3) C54 0.016(3) 0.022(4) 0.030(4) 0.003(3) 0.002(3) 0.005(3) C55 0.017(3) 0.018(3) 0.031(4) -0.001(3) -0.001(3) 0.007(3) C61 0.023(4) 0.037(4) 0.034(4) -0.001(3) 0.000(3) 0.005(3) C62 0.027(4) 0.030(4) 0.038(4) -0.003(3) 0.001(3) 0.002(3) C63 0.035(4) 0.030(4) 0.016(3) -0.005(3) -0.004(3) 0.001(3) C64 0.026(4) 0.030(4) 0.057(5) -0.003(4) -0.004(4) -0.002(3) C65 0.031(4) 0.028(4) 0.056(6) -0.004(4) -0.007(4) 0.007(3) Si 0.0139(9) 0.0236(10) 0.0331(11) -0.0025(8) -0.0054(8) 0.0001(8) F1 0.020(2) 0.029(2) 0.041(3) 0.0031(19) 0.0059(18) 0.0001(17) F2 0.034(3) 0.072(4) 0.057(3) 0.033(3) -0.020(2) -0.007(2) F3 0.023(2) 0.047(3) 0.039(3) -0.014(2) 0.0042(19) -0.0018(19) F4 0.022(2) 0.052(3) 0.106(4) -0.045(3) 0.000(3) 0.008(2) F5 0.024(2) 0.089(4) 0.027(2) -0.001(2) -0.0010(19) 0.006(2) F6 0.024(2) 0.031(3) 0.108(4) 0.013(3) -0.012(3) -0.010(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn O1 2.057(4) . yes Zn O2 2.106(4) . yes Zn O10 2.082(4) . yes Zn O30 2.112(4) . yes Zn O40 2.113(4) . yes Zn O50 2.105(4) . yes O1 C1 1.424(8) . ? O2 C2 1.414(8) . ? O3 C3 1.420(12) . ? O4 C4 1.405(9) . ? O5 C5 1.356(11) . ? O10 N10 1.328(6) . ? O20 N20 1.305(7) . ? O30 N30 1.339(6) . ? O40 N40 1.334(6) . ? O50 N50 1.328(6) . ? O60 N60 1.326(7) . ? N10 C15 1.341(8) . ? N10 C11 1.348(8) . ? N20 C25 1.350(8) . ? N20 C21 1.351(9) . ? N30 C35 1.345(8) . ? N30 C31 1.346(8) . ? N40 C45 1.330(8) . ? N40 C41 1.345(8) . ? N50 C55 1.342(8) . ? N50 C51 1.352(8) . ? N60 C61 1.347(9) . ? N60 C65 1.351(9) . ? C11 C12 1.370(9) . ? C12 C13 1.398(9) . ? C13 C14 1.395(9) . ? C13 C23 1.470(9) . ? C14 C15 1.373(9) . ? C21 C22 1.366(9) . ? C22 C23 1.396(9) . ? C23 C24 1.399(9) . ? C24 C25 1.383(9) . ? C31 C32 1.385(8) . ? C32 C33 1.380(9) . ? C33 C34 1.410(9) . ? C33 C43 1.486(8) 4_476 ? C34 C35 1.366(8) . ? C41 C42 1.378(8) . ? C42 C43 1.393(8) . ? C43 C44 1.389(9) . ? C43 C33 1.486(8) 4_675 ? C44 C45 1.369(9) . ? C51 C52 1.379(9) . ? C52 C53 1.405(9) . ? C53 C54 1.392(9) . ? C53 C53 1.483(12) 3_675 ? C54 C55 1.378(9) . ? C61 C62 1.357(10) . ? C62 C63 1.406(10) . ? C63 C64 1.387(10) . ? C63 C63 1.479(14) 3_665 ? C64 C65 1.375(10) . ? Si F1 1.688(4) . ? Si F2 1.679(5) . ? Si F3 1.677(4) . ? Si F4 1.692(5) . ? Si F5 1.683(5) . ? Si F6 1.675(5) . ? O1 O60 2.571(7) . yes O2 O20 2.652(6) 2_655 yes H1M O60 1.76 . yes H2M O20 1.82 2_655 yes loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn O10 92.0(2) . . yes O1 Zn O50 90.0(2) . . yes O1 Zn O2 179.0(2) . . yes O10 Zn O2 88.4(2) . . yes O50 Zn O2 89.6(2) . . yes O1 Zn O30 90.1(2) . . yes O2 Zn O30 90.8(2) . . yes O1 Zn O40 90.8(2) . . yes O2 Zn O40 88.3(2) . . yes O10 Zn O50 174.1(2) . . yes O10 Zn O30 92.2(2) . . yes O50 Zn O30 82.2(2) . . yes O10 Zn O40 88.4(2) . . yes O50 Zn O40 97.2(2) . . yes O30 Zn O40 178.9(2) . . yes N10 O10 Zn 122.6(3) . . ? N30 O30 Zn 125.2(3) . . ? N40 O40 Zn 132.4(4) . . ? N50 O50 Zn 118.0(3) . . ? O10 N10 C15 119.7(5) . . ? O10 N10 C11 120.6(5) . . ? C15 N10 C11 119.6(5) . . ? O20 N20 C25 120.7(6) . . ? O20 N20 C21 119.9(6) . . ? C25 N20 C21 119.3(6) . . ? O30 N30 C35 120.7(5) . . ? O30 N30 C31 118.2(5) . . ? C35 N30 C31 121.1(5) . . ? C45 N40 O40 121.2(5) . . ? C45 N40 C41 121.1(5) . . ? O40 N40 C41 117.7(5) . . ? O50 N50 C55 120.1(5) . . ? O50 N50 C51 119.5(5) . . ? C55 N50 C51 120.5(5) . . ? O60 N60 C61 119.1(6) . . ? O60 N60 C65 120.7(6) . . ? C61 N60 C65 120.2(6) . . ? N10 C11 C12 121.5(6) . . ? C11 C12 C13 120.5(6) . . ? C14 C13 C12 116.5(6) . . ? C14 C13 C23 120.9(6) . . ? C12 C13 C23 122.7(6) . . ? C15 C14 C13 120.9(6) . . ? N10 C15 C14 121.1(6) . . ? N20 C21 C22 122.1(6) . . ? C21 C22 C23 120.5(6) . . ? C22 C23 C24 116.2(6) . . ? C22 C23 C13 122.4(6) . . ? C24 C23 C13 121.4(6) . . ? C25 C24 C23 121.4(6) . . ? N20 C25 C24 120.4(6) . . ? N30 C31 C32 119.6(6) . . ? C33 C32 C31 121.1(6) . . ? C32 C33 C34 117.1(5) . . ? C32 C33 C43 122.3(6) . 4_476 ? C34 C33 C43 120.5(6) . 4_476 ? C35 C34 C33 120.2(6) . . ? N30 C35 C34 120.8(6) . . ? N40 C41 C42 120.0(6) . . ? C41 C42 C43 121.0(6) . . ? C44 C43 C42 116.1(6) . . ? C44 C43 C33 122.7(6) . 4_675 ? C42 C43 C33 121.2(6) . 4_675 ? C45 C44 C43 121.7(6) . . ? N40 C45 C44 120.1(6) . . ? N50 C51 C52 120.5(6) . . ? C51 C52 C53 120.5(6) . . ? C54 C53 C52 116.8(6) . . ? C54 C53 C53 122.0(7) . 3_675 ? C52 C53 C53 121.1(7) . 3_675 ? C55 C54 C53 120.8(6) . . ? N50 C55 C54 120.9(6) . . ? N60 C61 C62 121.3(7) . . ? C61 C62 C63 120.7(7) . . ? C64 C63 C62 116.4(7) . . ? C64 C63 C63 121.8(8) . 3_665 ? C62 C63 C63 121.8(8) . 3_665 ? C65 C64 C63 121.5(7) . . ? N60 C65 C64 119.9(7) . . ? F6 Si F3 91.0(2) . . ? F6 Si F2 90.7(3) . . ? F3 Si F2 90.4(3) . . ? F6 Si F5 90.3(3) . . ? F3 Si F5 89.9(2) . . ? F2 Si F5 179.0(3) . . ? F6 Si F1 179.1(2) . . ? F3 Si F1 89.9(2) . . ? F2 Si F1 89.0(2) . . ? F5 Si F1 90.0(2) . . ? F6 Si F4 90.2(3) . . ? F3 Si F4 178.6(3) . . ? F2 Si F4 90.3(3) . . ? F5 Si F4 89.4(3) . . ? F1 Si F4 88.9(2) . . ? O1 H1M O60 162.5 . . yes O2 H2M O20 168.1 . 2_655 yes _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.50 _refine_diff_density_min -0.54 _refine_diff_density_rms 0.12 data_ZNPYNT _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H48 N14 O18 Zn' _chemical_formula_weight 1318.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.8202(9) _cell_length_b 11.6805(10) _cell_length_c 14.006(2) _cell_angle_alpha 104.589(6) _cell_angle_beta 96.265(6) _cell_angle_gamma 99.082(6) _cell_volume 1362.1(3) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 17405 _cell_measurement_theta_min 1.84 _cell_measurement_theta_max 27.56 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.607 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 680 _exptl_absorpt_coefficient_mu 0.546 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.892 _exptl_absorpt_correction_T_max 0.965 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV. (Blessing, 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf Nonius KappaCCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 17405 _diffrn_reflns_av_R_equivalents 0.0994 _diffrn_reflns_av_sigmaI/netI 0.1437 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 27.56 _reflns_number_total 6140 _reflns_number_gt 3378 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DENZO (Otwinowski & Minor, 1997); COLLECT (Hooft, 1998)' _computing_cell_refinement 'DENZO and COLLECT' _computing_data_reduction 'DENZO and COLLECT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC v5.03 (Sheldrick, 1994)' _computing_publication_material 'SHELXTL/PC v5.03 (Sheldrick, 1994)' _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^)+(0.0859P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary 'difference Fourier methods' _atom_sites_solution_hydrogens 'placed geometrically' _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0044(14) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6140 _refine_ls_number_parameters 422 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.145 _refine_ls_R_factor_gt 0.069 _refine_ls_wR_factor_ref 0.179 _refine_ls_wR_factor_gt 0.146 _refine_ls_goodness_of_fit_ref 0.97 _refine_ls_restrained_S_all 0.97 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn Zn 0.0000 0.0000 0.5000 0.0244(2) Uani 1 2 d S . . O10 O -0.2325(3) -0.0225(2) 0.44465(19) 0.0272(6) Uani 1 1 d . . . O20 O -0.8214(3) 0.6156(2) 0.5810(2) 0.0353(7) Uani 1 1 d . . . O30 O -0.0200(3) -0.1864(2) 0.46229(18) 0.0268(6) Uani 1 1 d . . . O40 O -0.2005(3) -0.7402(2) -0.1968(2) 0.0349(7) Uani 1 1 d . . . O50 O -0.0724(3) -0.0141(2) 0.63588(19) 0.0280(6) Uani 1 1 d . . . O60 O 0.5651(3) -0.1549(3) 1.1865(2) 0.0395(8) Uani 1 1 d . . . N10 N -0.3187(4) 0.0615(3) 0.4681(2) 0.0229(7) Uani 1 1 d . . . N20 N -0.7442(4) 0.5271(3) 0.5641(2) 0.0267(8) Uani 1 1 d . . . N30 N -0.0609(4) -0.2664(3) 0.3728(2) 0.0247(8) Uani 1 1 d . . . N40 N -0.1909(4) -0.6712(3) -0.1071(2) 0.0284(8) Uani 1 1 d . . . N50 N 0.0146(4) -0.0366(3) 0.7100(2) 0.0239(7) Uani 1 1 d . . . N60 N 0.4795(4) -0.1370(3) 1.1123(3) 0.0292(8) Uani 1 1 d . . . C11 C -0.3125(4) 0.1262(3) 0.5632(3) 0.0261(9) Uani 1 1 d . . . H11A H -0.2474 0.1114 0.6156 0.031 Uiso 1 1 calc R . . C12 C -0.4006(4) 0.2132(3) 0.5840(3) 0.0257(9) Uani 1 1 d . . . H12A H -0.3960 0.2581 0.6513 0.031 Uiso 1 1 calc R . . C13 C -0.4968(4) 0.2376(3) 0.5088(3) 0.0243(9) Uani 1 1 d . . . C14 C -0.5046(4) 0.1647(3) 0.4118(3) 0.0260(9) Uani 1 1 d . . . H14A H -0.5721 0.1754 0.3584 0.031 Uiso 1 1 calc R . . C15 C -0.4148(4) 0.0772(3) 0.3931(3) 0.0258(9) Uani 1 1 d . . . H15A H -0.4210 0.0279 0.3270 0.031 Uiso 1 1 calc R . . C21 C -0.7988(5) 0.4269(3) 0.4860(3) 0.0280(9) Uani 1 1 d . . . H21A H -0.8925 0.4221 0.4434 0.034 Uiso 1 1 calc R . . C22 C -0.7208(4) 0.3334(3) 0.4681(3) 0.0260(9) Uani 1 1 d . . . H22A H -0.7606 0.2651 0.4127 0.031 Uiso 1 1 calc R . . C23 C -0.5844(5) 0.3362(3) 0.5295(3) 0.0257(9) Uani 1 1 d . . . C24 C -0.5304(5) 0.4409(3) 0.6089(3) 0.0276(9) Uani 1 1 d . . . H24A H -0.4372 0.4473 0.6525 0.033 Uiso 1 1 calc R . . C25 C -0.6100(5) 0.5338(3) 0.6244(3) 0.0286(9) Uani 1 1 d . . . H25A H -0.5707 0.6040 0.6782 0.034 Uiso 1 1 calc R . . C31 C 0.0048(5) -0.3656(3) 0.3560(3) 0.0264(9) Uani 1 1 d . . . H31A H 0.0770 -0.3762 0.4071 0.032 Uiso 1 1 calc R . . C32 C -0.0330(5) -0.4501(3) 0.2657(3) 0.0281(9) Uani 1 1 d . . . H32A H 0.0124 -0.5200 0.2554 0.034 Uiso 1 1 calc R . . C33 C -0.1359(4) -0.4370(3) 0.1885(3) 0.0242(9) Uani 1 1 d . . . C34 C -0.2055(5) -0.3349(3) 0.2107(3) 0.0270(9) Uani 1 1 d . . . H34A H -0.2801 -0.3231 0.1616 0.032 Uiso 1 1 calc R . . C35 C -0.1663(5) -0.2515(3) 0.3035(3) 0.0267(9) Uani 1 1 d . . . H35A H -0.2147 -0.1833 0.3179 0.032 Uiso 1 1 calc R . . C41 C -0.2832(5) -0.5880(4) -0.0860(3) 0.0328(10) Uani 1 1 d . . . H41A H -0.3571 -0.5805 -0.1376 0.039 Uiso 1 1 calc R . . C42 C -0.2706(5) -0.5149(3) 0.0089(3) 0.0289(10) Uani 1 1 d . . . H42A H -0.3365 -0.4576 0.0216 0.035 Uiso 1 1 calc R . . C43 C -0.1645(4) -0.5221(3) 0.0871(3) 0.0244(9) Uani 1 1 d . . . C44 C -0.0731(5) -0.6095(3) 0.0632(3) 0.0258(9) Uani 1 1 d . . . H44A H 0.0001 -0.6195 0.1141 0.031 Uiso 1 1 calc R . . C45 C -0.0875(5) -0.6806(3) -0.0317(3) 0.0279(9) Uani 1 1 d . . . H45A H -0.0230 -0.7387 -0.0456 0.033 Uiso 1 1 calc R . . C51 C 0.0839(4) -0.1337(3) 0.6935(3) 0.0260(9) Uani 1 1 d . . . H51A H 0.0710 -0.1866 0.6282 0.031 Uiso 1 1 calc R . . C52 C 0.1735(5) -0.1560(3) 0.7717(3) 0.0273(9) Uani 1 1 d . . . H52A H 0.2219 -0.2243 0.7595 0.033 Uiso 1 1 calc R . . C53 C 0.1939(4) -0.0796(3) 0.8680(3) 0.0241(9) Uani 1 1 d . . . C54 C 0.1178(5) 0.0181(3) 0.8814(3) 0.0270(9) Uani 1 1 d . . . H54A H 0.1273 0.0717 0.9461 0.032 Uiso 1 1 calc R . . C55 C 0.0294(4) 0.0379(3) 0.8023(3) 0.0272(9) Uani 1 1 d . . . H55A H -0.0216 0.1047 0.8129 0.033 Uiso 1 1 calc R . . C61 C 0.3731(5) -0.0640(3) 1.1286(3) 0.0269(9) Uani 1 1 d . . . H61A H 0.3619 -0.0259 1.1952 0.032 Uiso 1 1 calc R . . C62 C 0.2830(5) -0.0448(3) 1.0516(3) 0.0264(9) Uani 1 1 d . . . H62A H 0.2108 0.0073 1.0655 0.032 Uiso 1 1 calc R . . C63 C 0.2935(4) -0.0994(3) 0.9523(3) 0.0258(9) Uani 1 1 d . . . C64 C 0.4044(4) -0.1725(3) 0.9375(3) 0.0265(9) Uani 1 1 d . . . H64A H 0.4174 -0.2115 0.8715 0.032 Uiso 1 1 calc R . . C65 C 0.4943(5) -0.1885(4) 1.0168(3) 0.0306(10) Uani 1 1 d . . . H65A H 0.5701 -0.2376 1.0045 0.037 Uiso 1 1 calc R . . N1 N -0.2549(5) 0.7237(3) 0.8268(3) 0.0444(10) Uani 1 1 d . . . O1 O -0.1850(4) 0.7631(3) 0.9130(3) 0.0616(11) Uani 1 1 d . . . O2 O -0.3239(6) 0.7812(4) 0.7829(3) 0.0854(14) Uani 1 1 d . . . O3 O -0.2385(6) 0.6213(4) 0.7774(4) 0.1061(18) 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 Zn 0.0245(4) 0.0236(4) 0.0251(4) 0.0048(3) -0.0001(3) 0.0103(3) O10 0.0256(15) 0.0227(14) 0.0310(16) -0.0004(12) -0.0021(12) 0.0147(12) O20 0.0342(17) 0.0273(15) 0.0454(19) 0.0065(13) 0.0027(14) 0.0168(13) O30 0.0370(16) 0.0205(13) 0.0183(15) -0.0007(11) -0.0041(12) 0.0070(12) O40 0.0416(18) 0.0352(16) 0.0217(16) -0.0010(13) 0.0033(13) 0.0052(14) O50 0.0290(15) 0.0370(15) 0.0210(15) 0.0084(12) 0.0010(12) 0.0169(13) O60 0.0355(17) 0.0521(18) 0.0341(18) 0.0191(15) -0.0087(14) 0.0159(15) N10 0.0217(17) 0.0231(16) 0.0233(19) 0.0038(14) 0.0019(14) 0.0081(14) N20 0.0238(18) 0.0244(17) 0.033(2) 0.0066(15) 0.0052(16) 0.0108(15) N30 0.0245(18) 0.0229(16) 0.0255(19) 0.0062(14) 0.0002(15) 0.0036(15) N40 0.033(2) 0.0281(18) 0.022(2) 0.0054(15) 0.0047(16) 0.0030(16) N50 0.0241(17) 0.0273(17) 0.0235(19) 0.0092(14) 0.0036(15) 0.0106(15) N60 0.0260(19) 0.0319(18) 0.031(2) 0.0123(16) -0.0007(16) 0.0052(16) C11 0.025(2) 0.030(2) 0.023(2) 0.0040(17) 0.0002(17) 0.0098(18) C12 0.028(2) 0.026(2) 0.023(2) 0.0023(17) 0.0039(18) 0.0090(18) C13 0.022(2) 0.025(2) 0.026(2) 0.0066(17) 0.0004(17) 0.0053(17) C14 0.022(2) 0.031(2) 0.026(2) 0.0075(17) -0.0011(17) 0.0090(18) C15 0.022(2) 0.030(2) 0.022(2) 0.0037(17) -0.0017(17) 0.0058(18) C21 0.024(2) 0.034(2) 0.027(2) 0.0102(18) -0.0005(18) 0.0087(19) C22 0.023(2) 0.025(2) 0.028(2) 0.0045(17) 0.0024(18) 0.0071(18) C23 0.026(2) 0.025(2) 0.028(2) 0.0091(17) 0.0043(18) 0.0063(18) C24 0.026(2) 0.033(2) 0.022(2) 0.0058(17) -0.0020(17) 0.0093(19) C25 0.028(2) 0.026(2) 0.030(2) 0.0038(17) -0.0001(19) 0.0077(18) C31 0.028(2) 0.025(2) 0.030(2) 0.0108(17) 0.0005(18) 0.0130(18) C32 0.030(2) 0.027(2) 0.029(2) 0.0061(18) 0.0036(19) 0.0128(18) C33 0.025(2) 0.0223(19) 0.025(2) 0.0054(16) 0.0057(18) 0.0066(17) C34 0.025(2) 0.027(2) 0.028(2) 0.0099(17) -0.0046(18) 0.0043(18) C35 0.030(2) 0.0227(19) 0.030(2) 0.0078(17) 0.0041(19) 0.0106(18) C41 0.033(2) 0.035(2) 0.029(2) 0.0090(19) -0.0022(19) 0.009(2) C42 0.031(2) 0.022(2) 0.031(2) 0.0035(17) 0.0009(19) 0.0057(18) C43 0.026(2) 0.0215(19) 0.025(2) 0.0075(16) 0.0019(18) 0.0037(17) C44 0.028(2) 0.024(2) 0.025(2) 0.0043(17) 0.0033(18) 0.0075(18) C45 0.029(2) 0.023(2) 0.031(2) 0.0054(17) 0.0035(19) 0.0072(18) C51 0.028(2) 0.023(2) 0.027(2) 0.0051(17) 0.0032(18) 0.0082(18) C52 0.032(2) 0.024(2) 0.025(2) 0.0052(17) 0.0019(18) 0.0091(18) C53 0.024(2) 0.027(2) 0.022(2) 0.0092(17) 0.0013(17) 0.0044(18) C54 0.029(2) 0.026(2) 0.023(2) 0.0033(17) -0.0006(18) 0.0061(18) C55 0.028(2) 0.027(2) 0.027(2) 0.0032(17) 0.0052(18) 0.0097(18) C61 0.031(2) 0.025(2) 0.025(2) 0.0071(17) 0.0010(18) 0.0070(18) C62 0.026(2) 0.0219(19) 0.032(2) 0.0076(17) 0.0015(18) 0.0076(17) C63 0.025(2) 0.0218(19) 0.030(2) 0.0096(17) 0.0000(18) 0.0025(17) C64 0.026(2) 0.030(2) 0.025(2) 0.0095(17) 0.0043(18) 0.0073(19) C65 0.027(2) 0.035(2) 0.034(3) 0.0124(19) 0.006(2) 0.0129(19) N1 0.053(3) 0.037(2) 0.041(3) 0.0019(19) -0.006(2) 0.024(2) O1 0.073(3) 0.065(2) 0.036(2) -0.0132(17) -0.0176(19) 0.043(2) O2 0.143(4) 0.079(3) 0.041(2) 0.007(2) -0.012(2) 0.076(3) O3 0.144(5) 0.062(3) 0.087(3) -0.009(2) -0.052(3) 0.039(3) _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 Zn O10 2.063(3) . yes Zn O10 2.063(3) 2_556 ? Zn O30 2.081(2) 2_556 ? Zn O30 2.081(2) . yes Zn O50 2.109(3) 2_556 ? Zn O50 2.109(3) . yes O10 N10 1.332(4) . yes O20 N20 1.312(4) . yes O30 N30 1.334(4) . yes O40 N40 1.296(4) . yes O50 N50 1.327(4) . yes O60 N60 1.297(4) . yes N10 C15 1.344(5) . ? N10 C11 1.347(5) . ? N20 C25 1.357(5) . ? N20 C21 1.364(5) . ? N30 C35 1.332(5) . ? N30 C31 1.355(5) . ? N40 C45 1.357(5) . ? N40 C41 1.361(5) . ? N50 C55 1.343(5) . ? N50 C51 1.354(5) . ? N60 C65 1.351(5) . ? N60 C61 1.365(5) . ? C11 C12 1.367(5) . ? C12 C13 1.393(5) . ? C13 C14 1.398(5) . ? C13 C23 1.473(5) . ? C14 C15 1.381(5) . ? C21 C22 1.367(5) . ? C22 C23 1.391(6) . ? C23 C24 1.405(5) . ? C24 C25 1.368(5) . ? C31 C32 1.364(5) . ? C32 C33 1.390(5) . ? C33 C34 1.408(5) . ? C33 C43 1.482(5) . ? C34 C35 1.385(5) . ? C41 C42 1.368(5) . ? C42 C43 1.390(6) . ? C43 C44 1.397(5) . ? C44 C45 1.359(5) . ? C51 C52 1.382(6) . ? C52 C53 1.392(5) . ? C53 C54 1.397(5) . ? C53 C63 1.482(5) . ? C54 C55 1.373(5) . ? C61 C62 1.355(6) . ? C62 C63 1.396(5) . ? C63 C64 1.395(5) . ? C64 C65 1.362(6) . ? N1 O2 1.206(5) . ? N1 O1 1.233(5) . ? N1 O3 1.261(5) . ? 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 O10 Zn O10 180 . 2_556 ? O10 Zn O30 90.50(10) . 2_556 yes O10 Zn O30 89.50(10) 2_556 2_556 ? O10 Zn O30 89.50(10) . . yes O10 Zn O30 90.50(10) 2_556 . yes O30 Zn O30 180 2_556 . ? O10 Zn O50 93.46(10) . 2_556 yes O10 Zn O50 86.54(10) 2_556 2_556 ? O30 Zn O50 86.54(10) 2_556 2_556 ? O30 Zn O50 93.46(10) . 2_556 yes O10 Zn O50 86.54(10) . . yes O10 Zn O50 93.46(10) 2_556 . yes O30 Zn O50 93.46(10) 2_556 . yes O30 Zn O50 86.54(10) . . yes O50 Zn O50 180 2_556 . ? N10 O10 Zn 124.4(2) . . ? N30 O30 Zn 129.2(2) . . ? N50 O50 Zn 125.0(2) . . ? O10 N10 C15 117.3(3) . . ? O10 N10 C11 121.5(3) . . ? C15 N10 C11 121.2(3) . . ? O20 N20 C25 120.5(3) . . ? O20 N20 C21 120.2(3) . . ? C25 N20 C21 119.3(3) . . ? C35 N30 O30 121.3(3) . . ? C35 N30 C31 121.1(3) . . ? O30 N30 C31 117.6(3) . . ? O40 N40 C45 120.3(3) . . ? O40 N40 C41 121.4(3) . . ? C45 N40 C41 118.3(3) . . ? O50 N50 C55 118.4(3) . . ? O50 N50 C51 120.9(3) . . ? C55 N50 C51 120.7(3) . . ? O60 N60 C65 121.2(3) . . ? O60 N60 C61 120.8(3) . . ? C65 N60 C61 118.0(4) . . ? N10 C11 C12 119.7(4) . . ? C11 C12 C13 121.6(4) . . ? C12 C13 C14 116.7(4) . . ? C12 C13 C23 122.1(3) . . ? C14 C13 C23 121.2(4) . . ? C15 C14 C13 120.3(4) . . ? N10 C15 C14 120.3(4) . . ? N20 C21 C22 120.9(4) . . ? C21 C22 C23 121.3(4) . . ? C22 C23 C24 116.4(4) . . ? C22 C23 C13 121.6(3) . . ? C24 C23 C13 121.8(4) . . ? C25 C24 C23 121.0(4) . . ? N20 C25 C24 121.0(4) . . ? N30 C31 C32 119.9(4) . . ? C31 C32 C33 121.9(4) . . ? C32 C33 C34 116.1(3) . . ? C32 C33 C43 121.9(3) . . ? C34 C33 C43 121.9(4) . . ? C35 C34 C33 120.6(4) . . ? N30 C35 C34 120.3(4) . . ? N40 C41 C42 120.7(4) . . ? C41 C42 C43 122.0(4) . . ? C42 C43 C44 115.9(3) . . ? C42 C43 C33 123.7(4) . . ? C44 C43 C33 120.2(4) . . ? C45 C44 C43 121.0(4) . . ? N40 C45 C44 122.2(4) . . ? N50 C51 C52 120.1(4) . . ? C51 C52 C53 120.9(4) . . ? C52 C53 C54 116.8(4) . . ? C52 C53 C63 121.8(4) . . ? C54 C53 C63 121.3(3) . . ? C55 C54 C53 120.9(4) . . ? N50 C55 C54 120.6(4) . . ? C62 C61 N60 121.2(4) . . ? C61 C62 C63 121.7(4) . . ? C64 C63 C62 116.0(4) . . ? C64 C63 C53 122.2(4) . . ? C62 C63 C53 121.8(4) . . ? C65 C64 C63 120.6(4) . . ? N60 C65 C64 122.4(4) . . ? O2 N1 O1 124.4(4) . . ? O2 N1 O3 117.5(4) . . ? O1 N1 O3 117.6(4) . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 1.36 _refine_diff_density_min -0.79 _refine_diff_density_rms 0.10