# Electronic Supplementary Material (ESI) for CrystEngComm # 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_f1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C108 H146 N10 O32 P6 Zn7' _chemical_formula_weight 2739.76 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' P P 0.1023 0.0942 '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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.8046(10) _cell_length_b 18.7688(10) _cell_length_c 20.6949(12) _cell_angle_alpha 90.00 _cell_angle_beta 102.839(3) _cell_angle_gamma 90.00 _cell_volume 5985.3(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 11565 _cell_measurement_theta_min 2.2922 _cell_measurement_theta_max 27.4934 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.3000 _exptl_crystal_size_mid 0.2000 _exptl_crystal_size_min 0.1500 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.520 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2840 _exptl_absorpt_coefficient_mu 1.539 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9109 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Mercury70 (2x2 bin mode)' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46114 _diffrn_reflns_av_R_equivalents 0.0478 _diffrn_reflns_av_sigmaI/netI 0.0530 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 27.49 _reflns_number_total 13700 _reflns_number_gt 10251 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _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. Due to the moderate diffraction intensity and slightly abnormal triethylamine cation, so hydrogen atoms were generated geometrically. The free triethylamine cation N4(C43C44)(C45C46)(C47C48),C39 and C54 are slightly abnormal, so the distance/angle and isotropic are restrained. The restraints used in the refinement are listed as follows: dfix 1.51 0.01 n4 c43 c43 c44 n4 c45 c45 c46 n4 c47 c47 c48 DFIX 2.48 C43 C45 C43 C47 C45 C47 isor 0.01 c39 c43 c44 c45 c46 c47 c48 c54 simu 0.02 0.04 2.0 n4 c43 > c48 ; _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^)+(0.0625P)^2^+8.4052P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13700 _refine_ls_number_parameters 736 _refine_ls_number_restraints 93 _refine_ls_R_factor_all 0.0887 _refine_ls_R_factor_gt 0.0632 _refine_ls_wR_factor_ref 0.1593 _refine_ls_wR_factor_gt 0.1422 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.115 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.5000 0.0000 0.5000 0.03156(16) Uani 1 2 d S . . Zn2 Zn 0.63107(3) -0.10126(3) 0.63636(2) 0.03509(13) Uani 1 1 d . . . Zn3 Zn 0.42541(3) 0.15729(3) 0.57765(3) 0.03904(14) Uani 1 1 d . . . Zn4 Zn 0.34425(3) -0.07071(3) 0.59205(3) 0.03799(14) Uani 1 1 d . . . P1 P 0.52418(7) 0.16664(6) 0.46213(6) 0.0350(2) Uani 1 1 d . . . P2 P 0.30084(7) 0.05391(6) 0.48762(6) 0.0350(3) Uani 1 1 d . . . P3 P 0.50132(8) 0.01848(6) 0.65676(5) 0.0354(3) Uani 1 1 d . . . O1 O 0.50064(19) 0.11271(15) 0.51066(14) 0.0348(6) Uani 1 1 d . . . O2 O 0.4511(2) 0.17602(16) 0.40087(15) 0.0425(7) Uani 1 1 d . . . O3 O 0.6118(2) 0.15357(16) 0.44619(17) 0.0449(8) Uani 1 1 d . . . O4 O 0.3862(3) 0.2268(2) 0.64088(18) 0.0596(10) Uani 1 1 d . . . O5 O 0.4218(3) 0.3295(3) 0.6930(2) 0.0816(14) Uani 1 1 d . . . O6 O 0.37274(18) -0.00046(15) 0.51594(14) 0.0338(6) Uani 1 1 d . . . O7 O 0.3133(2) 0.12387(16) 0.52537(17) 0.0447(8) Uani 1 1 d . . . O8 O 0.2872(2) 0.06344(18) 0.41318(15) 0.0454(8) Uani 1 1 d . . . O9 O 0.2752(2) -0.1335(2) 0.64524(19) 0.0559(9) Uani 1 1 d . . . O10 O 0.1457(3) -0.1831(2) 0.6355(2) 0.0655(11) Uani 1 1 d . . . O11 O 0.54155(18) -0.01485(15) 0.60306(13) 0.0338(6) Uani 1 1 d . . . O12 O 0.4893(2) 0.09816(17) 0.65019(16) 0.0476(8) Uani 1 1 d . . . O13 O 0.4206(2) -0.02107(18) 0.66526(15) 0.0434(8) Uani 1 1 d . . . O14 O 0.7313(2) -0.15960(18) 0.69707(15) 0.0458(8) Uani 1 1 d . . . O15 O 0.8330(2) -0.1472(2) 0.7896(2) 0.0687(12) Uani 1 1 d . . . O16 O 0.3055(4) -0.0989(3) 0.3884(3) 0.115(2) Uani 1 1 d . . . H1 H 0.3567 -0.0986 0.3817 0.138 Uiso 1 1 d R . . H2 H 0.2848 -0.0569 0.3847 0.138 Uiso 1 1 d R . . N1 N 0.4632(2) 0.25906(19) 0.54220(17) 0.0366(8) Uani 1 1 d . . . N2 N 0.2168(2) -0.02309(19) 0.56621(17) 0.0343(8) Uani 1 1 d . . . N3 N 0.6218(2) -0.06768(18) 0.73451(17) 0.0341(8) Uani 1 1 d . . . N4 N 0.2248(6) 0.2352(5) 0.7741(4) 0.146(3) Uani 1 1 d DU . . H3 H 0.2629 0.2691 0.7942 0.175 Uiso 1 1 calc R . . N5 N -0.1431(3) -0.2510(3) 0.6695(2) 0.0655(13) Uani 1 1 d . . . H4 H -0.1835 -0.2185 0.6754 0.079 Uiso 1 1 calc R . . C1 C 0.5370(3) 0.2490(2) 0.5096(2) 0.0397(10) Uani 1 1 d . . . H5 H 0.5909 0.2475 0.5429 0.048 Uiso 1 1 calc R . . H6 H 0.5398 0.2889 0.4804 0.048 Uiso 1 1 calc R . . C2 C 0.4263(4) 0.2859(3) 0.6493(2) 0.0538(13) Uani 1 1 d . . . C3 C 0.4851(3) 0.3032(3) 0.6025(2) 0.0482(12) Uani 1 1 d . . . H7 H 0.4791 0.3531 0.5904 0.058 Uiso 1 1 calc R . . H8 H 0.5450 0.2948 0.6249 0.058 Uiso 1 1 calc R . . C4 C 0.3832(3) 0.2866(2) 0.4958(2) 0.0439(11) Uani 1 1 d . . . H9 H 0.3373 0.2897 0.5199 0.053 Uiso 1 1 calc R . . H10 H 0.3652 0.2518 0.4608 0.053 Uiso 1 1 calc R . . C5 C 0.3903(3) 0.3584(3) 0.4637(3) 0.0481(12) Uani 1 1 d . . . C6 C 0.4192(4) 0.3594(4) 0.4063(3) 0.0690(17) Uani 1 1 d . . . H11 H 0.4337 0.3167 0.3888 0.083 Uiso 1 1 calc R . . C7 C 0.4276(6) 0.4233(5) 0.3728(4) 0.099(3) Uani 1 1 d . . . H12 H 0.4495 0.4223 0.3346 0.119 Uiso 1 1 calc R . . C8 C 0.4045(5) 0.4854(4) 0.3952(5) 0.099(3) Uani 1 1 d . . . H13 H 0.4106 0.5272 0.3726 0.119 Uiso 1 1 calc R . . C9 C 0.3713(5) 0.4883(3) 0.4525(4) 0.082(2) Uani 1 1 d . . . C10 C 0.3439(7) 0.5517(4) 0.4762(7) 0.130(4) Uani 1 1 d . . . H14 H 0.3478 0.5937 0.4532 0.156 Uiso 1 1 calc R . . C11 C 0.3118(9) 0.5542(6) 0.5314(7) 0.161(6) Uani 1 1 d . . . H15 H 0.2938 0.5974 0.5459 0.193 Uiso 1 1 calc R . . C12 C 0.3057(7) 0.4926(5) 0.5663(5) 0.136(4) Uani 1 1 d . . . H16 H 0.2843 0.4947 0.6046 0.163 Uiso 1 1 calc R . . C13 C 0.3308(5) 0.4287(4) 0.5455(4) 0.084(2) Uani 1 1 d . . . H17 H 0.3255 0.3878 0.5696 0.101 Uiso 1 1 calc R . . C14 C 0.3639(4) 0.4234(3) 0.4888(3) 0.0643(16) Uani 1 1 d . . . C15 C 0.2034(3) 0.0097(2) 0.4997(2) 0.0371(10) Uani 1 1 d . . . H18 H 0.1565 0.0440 0.4943 0.045 Uiso 1 1 calc R . . H19 H 0.1867 -0.0269 0.4662 0.045 Uiso 1 1 calc R . . C16 C 0.1943(3) -0.1370(3) 0.6206(2) 0.0458(11) Uani 1 1 d . . . C17 C 0.1555(3) -0.0825(2) 0.5685(2) 0.0414(10) Uani 1 1 d . . . H20 H 0.1406 -0.1055 0.5255 0.050 Uiso 1 1 calc R . . H21 H 0.1026 -0.0636 0.5783 0.050 Uiso 1 1 calc R . . C18 C 0.2169(3) 0.0299(3) 0.6203(2) 0.0396(10) Uani 1 1 d . . . H22 H 0.2640 0.0632 0.6209 0.048 Uiso 1 1 calc R . . H23 H 0.2295 0.0047 0.6622 0.048 Uiso 1 1 calc R . . C19 C 0.1344(3) 0.0721(2) 0.6158(2) 0.0403(10) Uani 1 1 d . . . C20 C 0.1240(4) 0.1330(3) 0.5785(3) 0.0569(14) Uani 1 1 d . . . H24 H 0.1685 0.1479 0.5589 0.068 Uiso 1 1 calc R . . C21 C 0.0465(5) 0.1737(3) 0.5691(3) 0.0723(18) Uani 1 1 d . . . H25 H 0.0402 0.2146 0.5432 0.087 Uiso 1 1 calc R . . C22 C -0.0168(4) 0.1529(4) 0.5975(3) 0.0721(19) Uani 1 1 d . . . H26 H -0.0680 0.1791 0.5898 0.087 Uiso 1 1 calc R . . C23 C -0.0091(4) 0.0925(3) 0.6389(3) 0.0579(14) Uani 1 1 d . . . C24 C -0.0760(4) 0.0714(5) 0.6702(4) 0.086(2) Uani 1 1 d . . . H27 H -0.1278 0.0968 0.6621 0.103 Uiso 1 1 calc R . . C25 C -0.0657(5) 0.0149(5) 0.7116(4) 0.092(3) Uani 1 1 d . . . H28 H -0.1110 0.0014 0.7310 0.110 Uiso 1 1 calc R . . C26 C 0.0120(5) -0.0237(4) 0.7257(4) 0.083(2) Uani 1 1 d . . . H29 H 0.0193 -0.0611 0.7559 0.100 Uiso 1 1 calc R . . C27 C 0.0774(4) -0.0060(3) 0.6946(3) 0.0607(15) Uani 1 1 d . . . H30 H 0.1286 -0.0322 0.7035 0.073 Uiso 1 1 calc R . . C28 C 0.0682(3) 0.0515(3) 0.6494(2) 0.0475(12) Uani 1 1 d . . . C29 C 0.5854(3) 0.0057(2) 0.7316(2) 0.0370(10) Uani 1 1 d . . . H31 H 0.6315 0.0401 0.7326 0.044 Uiso 1 1 calc R . . H32 H 0.5612 0.0139 0.7701 0.044 Uiso 1 1 calc R . . C30 C 0.7641(3) -0.1307(3) 0.7534(2) 0.0442(11) Uani 1 1 d . . . C31 C 0.7117(3) -0.0703(2) 0.7743(2) 0.0401(10) Uani 1 1 d . . . H33 H 0.7104 -0.0762 0.8206 0.048 Uiso 1 1 calc R . . H34 H 0.7401 -0.0253 0.7697 0.048 Uiso 1 1 calc R . . C32 C 0.5640(3) -0.1216(3) 0.7566(2) 0.0400(10) Uani 1 1 d . . . H35 H 0.5868 -0.1687 0.7512 0.048 Uiso 1 1 calc R . . H36 H 0.5070 -0.1186 0.7271 0.048 Uiso 1 1 calc R . . C33 C 0.5529(3) -0.1149(3) 0.8276(2) 0.0461(11) Uani 1 1 d . . . C34 C 0.4899(4) -0.0706(3) 0.8396(3) 0.0691(17) Uani 1 1 d . . . H37 H 0.4556 -0.0453 0.8048 0.083 Uiso 1 1 calc R . . C35 C 0.4760(6) -0.0625(5) 0.9041(5) 0.096(3) Uani 1 1 d . . . H38 H 0.4330 -0.0321 0.9120 0.115 Uiso 1 1 calc R . . C36 C 0.5267(6) -0.1001(5) 0.9549(4) 0.096(3) Uani 1 1 d . . . H39 H 0.5183 -0.0935 0.9975 0.116 Uiso 1 1 calc R . . C37 C 0.5906(5) -0.1478(4) 0.9455(3) 0.0721(19) Uani 1 1 d . . . C38 C 0.6411(6) -0.1898(5) 0.9982(3) 0.095(3) Uani 1 1 d . . . H40 H 0.6313 -0.1859 1.0407 0.114 Uiso 1 1 calc R . . C39 C 0.7035(6) -0.2355(5) 0.9867(4) 0.095(3) Uani 1 1 d U . . H41 H 0.7367 -0.2616 1.0214 0.115 Uiso 1 1 calc R . . C40 C 0.7168(4) -0.2427(4) 0.9240(4) 0.079(2) Uani 1 1 d . . . H42 H 0.7589 -0.2744 0.9166 0.095 Uiso 1 1 calc R . . C41 C 0.6702(3) -0.2047(3) 0.8717(3) 0.0602(15) Uani 1 1 d . . . H43 H 0.6812 -0.2109 0.8297 0.072 Uiso 1 1 calc R . . C42 C 0.6051(4) -0.1556(3) 0.8808(3) 0.0539(14) Uani 1 1 d . . . C43 C 0.1822(11) 0.2017(10) 0.8275(7) 0.266(7) Uani 1 1 d DU . . H44 H 0.2022 0.1530 0.8362 0.320 Uiso 1 1 calc R . . H45 H 0.1985 0.2285 0.8685 0.320 Uiso 1 1 calc R . . C44 C 0.0854(12) 0.2027(13) 0.8032(11) 0.339(12) Uani 1 1 d DU . . H46 H 0.0586 0.1833 0.8367 0.508 Uiso 1 1 calc R . . H47 H 0.0694 0.1745 0.7637 0.508 Uiso 1 1 calc R . . H48 H 0.0661 0.2509 0.7938 0.508 Uiso 1 1 calc R . . C45 C 0.1602(8) 0.2701(7) 0.7222(6) 0.208(6) Uani 1 1 d DU . . H49 H 0.1188 0.2965 0.7412 0.250 Uiso 1 1 calc R . . H50 H 0.1290 0.2353 0.6912 0.250 Uiso 1 1 calc R . . C46 C 0.2124(7) 0.3203(7) 0.6878(6) 0.163(5) Uani 1 1 d DU . . H51 H 0.1737 0.3452 0.6527 0.245 Uiso 1 1 calc R . . H52 H 0.2533 0.2933 0.6698 0.245 Uiso 1 1 calc R . . H53 H 0.2430 0.3541 0.7193 0.245 Uiso 1 1 calc R . . C47 C 0.2757(8) 0.1779(7) 0.7502(6) 0.177(5) Uani 1 1 d DU . . H54 H 0.2344 0.1412 0.7309 0.213 Uiso 1 1 calc R . . H55 H 0.2976 0.1982 0.7140 0.213 Uiso 1 1 calc R . . C48 C 0.3503(9) 0.1405(8) 0.7940(7) 0.200(6) Uani 1 1 d DU . . H56 H 0.3734 0.1056 0.7687 0.300 Uiso 1 1 calc R . . H57 H 0.3308 0.1173 0.8295 0.300 Uiso 1 1 calc R . . H58 H 0.3946 0.1745 0.8121 0.300 Uiso 1 1 calc R . . C49 C -0.1815(5) -0.2879(5) 0.6068(4) 0.093(2) Uani 1 1 d . . . H59 H -0.1965 -0.2527 0.5718 0.111 Uiso 1 1 calc R . . H80 H -0.2349 -0.3109 0.6114 0.111 Uiso 1 1 calc R . . C50 C -0.1234(8) -0.3430(7) 0.5863(6) 0.177(6) Uani 1 1 d . . . H61 H -0.1526 -0.3644 0.5453 0.266 Uiso 1 1 calc R . . H62 H -0.1096 -0.3791 0.6199 0.266 Uiso 1 1 calc R . . H63 H -0.0708 -0.3207 0.5806 0.266 Uiso 1 1 calc R . . C51 C -0.0625(4) -0.2082(4) 0.6668(4) 0.086(2) Uani 1 1 d . . . H64 H -0.0422 -0.1842 0.7090 0.103 Uiso 1 1 calc R . . H65 H -0.0171 -0.2405 0.6604 0.103 Uiso 1 1 calc R . . C52 C -0.0781(5) -0.1544(4) 0.6129(4) 0.093(2) Uani 1 1 d . . . H66 H -0.0253 -0.1290 0.6133 0.139 Uiso 1 1 calc R . . H67 H -0.1220 -0.1216 0.6196 0.139 Uiso 1 1 calc R . . H68 H -0.0972 -0.1779 0.5710 0.139 Uiso 1 1 calc R . . C53 C -0.1281(7) -0.2978(4) 0.7294(4) 0.108(3) Uani 1 1 d . . . H69 H -0.1036 -0.2699 0.7686 0.129 Uiso 1 1 calc R . . H70 H -0.0870 -0.3350 0.7253 0.129 Uiso 1 1 calc R . . C54 C -0.2149(7) -0.3320(5) 0.7371(5) 0.127(3) Uani 1 1 d U . . H71 H -0.2558 -0.2951 0.7405 0.190 Uiso 1 1 calc R . . H72 H -0.2047 -0.3608 0.7764 0.190 Uiso 1 1 calc R . . H73 H -0.2378 -0.3612 0.6991 0.190 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0304(4) 0.0290(4) 0.0341(3) 0.0030(3) 0.0046(3) 0.0039(3) Zn2 0.0362(3) 0.0334(3) 0.0341(3) 0.0040(2) 0.0045(2) 0.0048(2) Zn3 0.0405(3) 0.0325(3) 0.0434(3) 0.0035(2) 0.0078(2) 0.0074(2) Zn4 0.0330(3) 0.0385(3) 0.0425(3) 0.0055(2) 0.0084(2) 0.0065(2) P1 0.0357(6) 0.0277(6) 0.0410(6) 0.0020(4) 0.0073(5) 0.0018(5) P2 0.0295(6) 0.0347(6) 0.0399(6) 0.0075(5) 0.0063(4) 0.0052(4) P3 0.0371(6) 0.0347(6) 0.0327(5) 0.0026(4) 0.0042(4) 0.0081(5) O1 0.0353(16) 0.0295(16) 0.0391(16) 0.0019(12) 0.0072(12) 0.0014(12) O2 0.0510(19) 0.0285(16) 0.0433(17) 0.0047(13) 0.0004(14) 0.0027(14) O3 0.0415(18) 0.0348(18) 0.064(2) 0.0001(15) 0.0240(16) 0.0013(14) O4 0.078(3) 0.046(2) 0.060(2) 0.0023(17) 0.026(2) 0.017(2) O5 0.093(3) 0.092(3) 0.059(3) -0.035(2) 0.017(2) 0.005(3) O6 0.0307(15) 0.0330(16) 0.0371(15) 0.0061(12) 0.0064(12) 0.0037(12) O7 0.0371(18) 0.0331(17) 0.064(2) 0.0004(15) 0.0116(15) 0.0042(14) O8 0.0322(17) 0.061(2) 0.0418(17) 0.0158(15) 0.0049(13) 0.0055(15) O9 0.047(2) 0.055(2) 0.068(2) 0.0243(18) 0.0177(18) 0.0081(17) O10 0.066(3) 0.059(2) 0.075(3) 0.018(2) 0.023(2) -0.010(2) O11 0.0346(16) 0.0323(16) 0.0330(15) 0.0032(12) 0.0043(12) 0.0073(12) O12 0.065(2) 0.0337(18) 0.0410(17) 0.0008(13) 0.0043(15) 0.0154(16) O13 0.0349(17) 0.057(2) 0.0376(16) 0.0026(14) 0.0057(13) 0.0022(15) O14 0.0464(19) 0.048(2) 0.0400(17) 0.0086(14) 0.0033(14) 0.0126(15) O15 0.042(2) 0.083(3) 0.070(3) 0.003(2) -0.0119(18) 0.023(2) O16 0.090(4) 0.103(4) 0.146(5) -0.041(4) 0.014(4) -0.022(3) N1 0.036(2) 0.030(2) 0.0388(19) -0.0046(15) -0.0008(15) 0.0062(15) N2 0.0287(18) 0.037(2) 0.0368(19) 0.0024(15) 0.0057(14) 0.0008(15) N3 0.0319(19) 0.0304(19) 0.0363(18) 0.0040(14) -0.0001(14) 0.0018(15) N4 0.178(8) 0.126(6) 0.130(6) -0.053(5) 0.025(6) -0.023(6) N5 0.064(3) 0.066(3) 0.061(3) 0.001(2) 0.002(2) 0.023(3) C1 0.036(2) 0.033(2) 0.047(3) -0.0006(19) 0.0027(19) 0.0031(19) C2 0.060(3) 0.055(3) 0.041(3) -0.005(2) 0.000(2) 0.017(3) C3 0.049(3) 0.044(3) 0.045(3) -0.011(2) -0.004(2) 0.006(2) C4 0.036(2) 0.039(3) 0.052(3) 0.000(2) 0.000(2) 0.010(2) C5 0.048(3) 0.035(3) 0.055(3) 0.003(2) 0.000(2) 0.009(2) C6 0.070(4) 0.065(4) 0.072(4) 0.028(3) 0.015(3) 0.016(3) C7 0.106(6) 0.092(6) 0.100(6) 0.050(5) 0.025(5) 0.015(5) C8 0.094(6) 0.069(5) 0.122(7) 0.055(5) -0.001(5) -0.007(4) C9 0.078(5) 0.036(3) 0.111(6) 0.014(3) -0.021(4) 0.005(3) C10 0.140(9) 0.036(4) 0.183(11) 0.002(5) -0.028(8) 0.017(5) C11 0.205(13) 0.078(7) 0.175(12) -0.031(8) -0.010(10) 0.086(8) C12 0.176(10) 0.096(7) 0.126(8) -0.027(6) 0.012(7) 0.082(7) C13 0.103(6) 0.061(4) 0.084(5) -0.009(3) 0.011(4) 0.036(4) C14 0.066(4) 0.041(3) 0.076(4) 0.008(3) -0.007(3) 0.012(3) C15 0.031(2) 0.041(3) 0.039(2) 0.0065(18) 0.0062(18) 0.0073(18) C16 0.056(3) 0.037(3) 0.049(3) 0.003(2) 0.021(2) 0.001(2) C17 0.038(2) 0.040(3) 0.046(3) 0.000(2) 0.010(2) -0.004(2) C18 0.035(2) 0.045(3) 0.038(2) -0.0010(19) 0.0070(18) 0.002(2) C19 0.042(3) 0.038(3) 0.040(2) -0.0033(19) 0.0074(19) 0.007(2) C20 0.070(4) 0.049(3) 0.054(3) 0.005(2) 0.018(3) 0.018(3) C21 0.093(5) 0.060(4) 0.065(4) 0.014(3) 0.020(3) 0.038(4) C22 0.065(4) 0.087(5) 0.059(4) -0.012(3) 0.001(3) 0.039(4) C23 0.046(3) 0.072(4) 0.054(3) -0.022(3) 0.009(2) 0.009(3) C24 0.051(4) 0.125(7) 0.086(5) -0.037(5) 0.025(3) 0.002(4) C25 0.084(5) 0.109(7) 0.100(6) -0.037(5) 0.059(5) -0.026(5) C26 0.103(6) 0.071(5) 0.093(5) -0.006(4) 0.059(4) -0.017(4) C27 0.077(4) 0.053(3) 0.059(3) -0.002(3) 0.030(3) 0.004(3) C28 0.042(3) 0.055(3) 0.046(3) -0.011(2) 0.012(2) 0.002(2) C29 0.043(3) 0.031(2) 0.034(2) 0.0018(17) 0.0031(18) 0.0025(19) C30 0.037(3) 0.050(3) 0.043(3) 0.010(2) 0.005(2) 0.004(2) C31 0.036(2) 0.043(3) 0.038(2) 0.0040(19) 0.0006(18) -0.005(2) C32 0.035(2) 0.042(3) 0.040(2) 0.0035(19) 0.0023(18) 0.0015(19) C33 0.044(3) 0.051(3) 0.043(3) 0.000(2) 0.009(2) -0.009(2) C34 0.066(4) 0.073(4) 0.075(4) 0.001(3) 0.032(3) 0.006(3) C35 0.099(6) 0.095(6) 0.113(7) -0.020(5) 0.061(5) 0.000(5) C36 0.126(7) 0.106(7) 0.070(5) -0.021(4) 0.048(5) -0.038(6) C37 0.092(5) 0.079(5) 0.045(3) 0.004(3) 0.015(3) -0.029(4) C38 0.131(7) 0.101(6) 0.045(3) 0.013(4) 0.003(4) -0.059(5) C39 0.099(5) 0.085(5) 0.083(5) 0.034(4) -0.020(4) -0.036(4) C40 0.062(4) 0.070(4) 0.089(5) 0.038(4) -0.018(3) -0.024(3) C41 0.047(3) 0.058(4) 0.071(4) 0.026(3) 0.004(3) -0.006(3) C42 0.057(3) 0.058(3) 0.045(3) 0.006(2) 0.007(2) -0.021(3) C43 0.280(10) 0.265(10) 0.248(10) -0.002(8) 0.049(8) -0.031(8) C44 0.312(14) 0.357(14) 0.343(14) -0.006(9) 0.065(9) -0.012(9) C45 0.218(9) 0.203(9) 0.184(8) -0.026(7) 0.003(7) 0.018(8) C46 0.128(7) 0.194(9) 0.185(8) 0.027(7) 0.074(6) 0.010(7) C47 0.169(8) 0.192(8) 0.172(8) -0.054(7) 0.039(7) 0.028(7) C48 0.221(10) 0.182(9) 0.181(9) 0.000(7) 0.012(8) 0.018(8) C49 0.070(5) 0.117(7) 0.078(5) -0.025(4) -0.013(4) 0.005(4) C50 0.161(11) 0.204(13) 0.153(10) -0.121(9) 0.006(8) 0.043(9) C51 0.060(4) 0.092(5) 0.096(5) -0.015(4) -0.004(4) 0.012(4) C52 0.075(5) 0.112(7) 0.090(5) 0.011(5) 0.017(4) 0.000(4) C53 0.157(9) 0.072(5) 0.080(5) 0.008(4) -0.005(5) 0.046(5) C54 0.151(7) 0.090(6) 0.152(7) 0.043(5) 0.059(6) 0.041(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O11 2.106(3) 3_656 ? Zn1 O11 2.106(3) . ? Zn1 O6 2.109(3) . ? Zn1 O6 2.109(3) 3_656 ? Zn1 O1 2.127(3) . ? Zn1 O1 2.127(3) 3_656 ? Zn2 O2 1.951(3) 3_656 ? Zn2 O8 1.952(3) 3_656 ? Zn2 O14 2.099(3) . ? Zn2 O11 2.162(3) . ? Zn2 N3 2.163(4) . ? Zn3 O12 1.957(3) . ? Zn3 O7 1.962(3) . ? Zn3 O4 2.040(4) . ? Zn3 N1 2.177(4) . ? Zn3 O1 2.184(3) . ? Zn4 O3 1.942(3) 3_656 ? Zn4 O13 1.951(3) . ? Zn4 O9 2.079(3) . ? Zn4 N2 2.159(3) . ? Zn4 O6 2.177(3) . ? P1 O3 1.513(3) . ? P1 O2 1.523(3) . ? P1 O1 1.529(3) . ? P1 C1 1.819(5) . ? P2 O8 1.518(3) . ? P2 O7 1.518(3) . ? P2 O6 1.543(3) . ? P2 C15 1.815(5) . ? P3 O12 1.510(3) . ? P3 O13 1.520(3) . ? P3 O11 1.531(3) . ? P3 C29 1.819(4) . ? O2 Zn2 1.951(3) 3_656 ? O3 Zn4 1.942(3) 3_656 ? O4 C2 1.270(7) . ? O5 C2 1.234(6) . ? O8 Zn2 1.952(3) 3_656 ? O9 C16 1.269(6) . ? O10 C16 1.242(6) . ? O14 C30 1.286(6) . ? O15 C30 1.217(5) . ? O16 H1 0.8501 . ? O16 H2 0.8502 . ? N1 C3 1.473(6) . ? N1 C1 1.484(6) . ? N1 C4 1.501(5) . ? N2 C15 1.480(5) . ? N2 C17 1.485(6) . ? N2 C18 1.496(6) . ? N3 C31 1.476(5) . ? N3 C29 1.488(5) . ? N3 C32 1.501(6) . ? N4 C45 1.462(8) . ? N4 C47 1.493(8) . ? N4 C43 1.549(9) . ? N4 H3 0.9100 . ? N5 C49 1.477(8) . ? N5 C53 1.496(9) . ? N5 C51 1.518(9) . ? N5 H4 0.9100 . ? C1 H5 0.9700 . ? C1 H6 0.9700 . ? C2 C3 1.519(8) . ? C3 H7 0.9700 . ? C3 H8 0.9700 . ? C4 C5 1.516(7) . ? C4 H9 0.9700 . ? C4 H10 0.9700 . ? C5 C6 1.364(8) . ? C5 C14 1.424(8) . ? C6 C7 1.406(9) . ? C6 H11 0.9300 . ? C7 C8 1.335(12) . ? C7 H12 0.9300 . ? C8 C9 1.401(12) . ? C8 H13 0.9300 . ? C9 C10 1.392(12) . ? C9 C14 1.450(9) . ? C10 C11 1.350(16) . ? C10 H14 0.9300 . ? C11 C12 1.377(16) . ? C11 H15 0.9300 . ? C12 C13 1.363(9) . ? C12 H16 0.9300 . ? C13 C14 1.390(10) . ? C13 H17 0.9300 . ? C15 H18 0.9700 . ? C15 H19 0.9700 . ? C16 C17 1.512(7) . ? C17 H20 0.9700 . ? C17 H21 0.9700 . ? C18 C19 1.512(6) . ? C18 H22 0.9700 . ? C18 H23 0.9700 . ? C19 C20 1.368(7) . ? C19 C28 1.432(7) . ? C20 C21 1.419(8) . ? C20 H24 0.9300 . ? C21 C22 1.326(9) . ? C21 H25 0.9300 . ? C22 C23 1.411(9) . ? C22 H26 0.9300 . ? C23 C24 1.412(9) . ? C23 C28 1.420(7) . ? C24 C25 1.350(11) . ? C24 H27 0.9300 . ? C25 C26 1.400(11) . ? C25 H28 0.9300 . ? C26 C27 1.373(8) . ? C26 H29 0.9300 . ? C27 C28 1.414(8) . ? C27 H30 0.9300 . ? C29 H31 0.9700 . ? C29 H32 0.9700 . ? C30 C31 1.522(7) . ? C31 H33 0.9700 . ? C31 H34 0.9700 . ? C32 C33 1.524(6) . ? C32 H35 0.9700 . ? C32 H36 0.9700 . ? C33 C34 1.362(8) . ? C33 C42 1.440(7) . ? C34 C35 1.407(10) . ? C34 H37 0.9300 . ? C35 C36 1.368(12) . ? C35 H38 0.9300 . ? C36 C37 1.396(11) . ? C36 H39 0.9300 . ? C37 C42 1.416(8) . ? C37 C38 1.435(10) . ? C38 C39 1.366(12) . ? C38 H40 0.9300 . ? C39 C40 1.367(11) . ? C39 H41 0.9300 . ? C40 C41 1.367(7) . ? C40 H42 0.9300 . ? C41 C42 1.424(8) . ? C41 H43 0.9300 . ? C43 C44 1.501(10) . ? C43 H44 0.9700 . ? C43 H45 0.9700 . ? C44 H46 0.9600 . ? C44 H47 0.9600 . ? C44 H48 0.9600 . ? C45 C46 1.530(9) . ? C45 H49 0.9700 . ? C45 H50 0.9700 . ? C46 H51 0.9600 . ? C46 H52 0.9600 . ? C46 H53 0.9600 . ? C47 C48 1.493(9) . ? C47 H54 0.9700 . ? C47 H55 0.9700 . ? C48 H56 0.9600 . ? C48 H57 0.9600 . ? C48 H58 0.9600 . ? C49 C50 1.506(11) . ? C49 H59 0.9700 . ? C49 H80 0.9700 . ? C50 H61 0.9600 . ? C50 H62 0.9600 . ? C50 H63 0.9600 . ? C51 C52 1.484(10) . ? C51 H64 0.9700 . ? C51 H65 0.9700 . ? C52 H66 0.9600 . ? C52 H67 0.9600 . ? C52 H68 0.9600 . ? C53 C54 1.553(13) . ? C53 H69 0.9700 . ? C53 H70 0.9700 . ? C54 H71 0.9600 . ? C54 H72 0.9600 . ? C54 H73 0.9600 . ? 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 O11 Zn1 O11 180.000(1) 3_656 . ? O11 Zn1 O6 93.75(11) 3_656 . ? O11 Zn1 O6 86.25(11) . . ? O11 Zn1 O6 86.25(11) 3_656 3_656 ? O11 Zn1 O6 93.75(11) . 3_656 ? O6 Zn1 O6 180.0 . 3_656 ? O11 Zn1 O1 88.09(11) 3_656 . ? O11 Zn1 O1 91.91(11) . . ? O6 Zn1 O1 88.31(11) . . ? O6 Zn1 O1 91.69(11) 3_656 . ? O11 Zn1 O1 91.91(11) 3_656 3_656 ? O11 Zn1 O1 88.09(11) . 3_656 ? O6 Zn1 O1 91.69(11) . 3_656 ? O6 Zn1 O1 88.31(11) 3_656 3_656 ? O1 Zn1 O1 180.00(16) . 3_656 ? O2 Zn2 O8 120.95(14) 3_656 3_656 ? O2 Zn2 O14 102.08(13) 3_656 . ? O8 Zn2 O14 90.27(13) 3_656 . ? O2 Zn2 O11 94.73(12) 3_656 . ? O8 Zn2 O11 91.27(12) 3_656 . ? O14 Zn2 O11 159.37(12) . . ? O2 Zn2 N3 113.72(14) 3_656 . ? O8 Zn2 N3 125.32(14) 3_656 . ? O14 Zn2 N3 77.86(13) . . ? O11 Zn2 N3 84.52(12) . . ? O12 Zn3 O7 119.37(14) . . ? O12 Zn3 O4 92.83(14) . . ? O7 Zn3 O4 101.09(15) . . ? O12 Zn3 N1 128.50(14) . . ? O7 Zn3 N1 112.11(13) . . ? O4 Zn3 N1 78.47(15) . . ? O12 Zn3 O1 90.50(12) . . ? O7 Zn3 O1 94.56(12) . . ? O4 Zn3 O1 159.81(15) . . ? N1 Zn3 O1 83.88(12) . . ? O3 Zn4 O13 118.90(14) 3_656 . ? O3 Zn4 O9 92.25(14) 3_656 . ? O13 Zn4 O9 99.57(15) . . ? O3 Zn4 N2 128.97(14) 3_656 . ? O13 Zn4 N2 112.12(14) . . ? O9 Zn4 N2 78.20(13) . . ? O3 Zn4 O6 92.28(12) 3_656 . ? O13 Zn4 O6 94.64(12) . . ? O9 Zn4 O6 160.67(13) . . ? N2 Zn4 O6 84.35(12) . . ? O3 P1 O2 113.5(2) . . ? O3 P1 O1 113.82(18) . . ? O2 P1 O1 111.91(18) . . ? O3 P1 C1 105.0(2) . . ? O2 P1 C1 108.91(19) . . ? O1 P1 C1 102.84(19) . . ? O8 P2 O7 113.2(2) . . ? O8 P2 O6 112.94(18) . . ? O7 P2 O6 112.09(18) . . ? O8 P2 C15 105.09(19) . . ? O7 P2 C15 110.0(2) . . ? O6 P2 C15 102.77(18) . . ? O12 P3 O13 113.7(2) . . ? O12 P3 O11 113.80(18) . . ? O13 P3 O11 112.28(18) . . ? O12 P3 C29 105.11(19) . . ? O13 P3 C29 108.1(2) . . ? O11 P3 C29 102.81(19) . . ? P1 O1 Zn1 125.92(17) . . ? P1 O1 Zn3 114.19(16) . . ? Zn1 O1 Zn3 117.15(13) . . ? P1 O2 Zn2 124.10(18) . 3_656 ? P1 O3 Zn4 130.3(2) . 3_656 ? C2 O4 Zn3 115.7(4) . . ? P2 O6 Zn1 125.82(16) . . ? P2 O6 Zn4 114.98(16) . . ? Zn1 O6 Zn4 118.26(12) . . ? P2 O7 Zn3 123.95(19) . . ? P2 O8 Zn2 127.9(2) . 3_656 ? C16 O9 Zn4 114.6(3) . . ? P3 O11 Zn1 126.49(16) . . ? P3 O11 Zn2 115.03(15) . . ? Zn1 O11 Zn2 117.18(13) . . ? P3 O12 Zn3 131.6(2) . . ? P3 O13 Zn4 122.26(19) . . ? C30 O14 Zn2 114.9(3) . . ? H1 O16 H2 110.0 . . ? C3 N1 C1 113.4(4) . . ? C3 N1 C4 110.8(3) . . ? C1 N1 C4 112.9(4) . . ? C3 N1 Zn3 103.8(3) . . ? C1 N1 Zn3 110.1(3) . . ? C4 N1 Zn3 105.3(3) . . ? C15 N2 C17 112.5(3) . . ? C15 N2 C18 113.3(4) . . ? C17 N2 C18 111.6(3) . . ? C15 N2 Zn4 109.6(2) . . ? C17 N2 Zn4 105.1(3) . . ? C18 N2 Zn4 104.1(2) . . ? C31 N3 C29 111.6(3) . . ? C31 N3 C32 112.6(3) . . ? C29 N3 C32 112.4(3) . . ? C31 N3 Zn2 104.8(3) . . ? C29 N3 Zn2 109.8(2) . . ? C32 N3 Zn2 105.2(3) . . ? C45 N4 C47 114.7(9) . . ? C45 N4 C43 111.2(9) . . ? C47 N4 C43 107.2(9) . . ? C45 N4 H3 107.8 . . ? C47 N4 H3 107.8 . . ? C43 N4 H3 107.8 . . ? C49 N5 C53 114.3(6) . . ? C49 N5 C51 113.7(6) . . ? C53 N5 C51 111.2(6) . . ? C49 N5 H4 105.6 . . ? C53 N5 H4 105.6 . . ? C51 N5 H4 105.6 . . ? N1 C1 P1 110.5(3) . . ? N1 C1 H5 109.6 . . ? P1 C1 H5 109.6 . . ? N1 C1 H6 109.6 . . ? P1 C1 H6 109.6 . . ? H5 C1 H6 108.1 . . ? O5 C2 O4 124.9(6) . . ? O5 C2 C3 117.9(6) . . ? O4 C2 C3 117.1(4) . . ? N1 C3 C2 111.0(4) . . ? N1 C3 H7 109.4 . . ? C2 C3 H7 109.4 . . ? N1 C3 H8 109.4 . . ? C2 C3 H8 109.4 . . ? H7 C3 H8 108.0 . . ? N1 C4 C5 116.9(4) . . ? N1 C4 H9 108.1 . . ? C5 C4 H9 108.1 . . ? N1 C4 H10 108.1 . . ? C5 C4 H10 108.1 . . ? H9 C4 H10 107.3 . . ? C6 C5 C14 119.1(5) . . ? C6 C5 C4 117.8(5) . . ? C14 C5 C4 123.0(5) . . ? C5 C6 C7 122.0(7) . . ? C5 C6 H11 119.0 . . ? C7 C6 H11 119.0 . . ? C8 C7 C6 120.6(8) . . ? C8 C7 H12 119.7 . . ? C6 C7 H12 119.7 . . ? C7 C8 C9 120.8(7) . . ? C7 C8 H13 119.6 . . ? C9 C8 H13 119.6 . . ? C10 C9 C8 122.4(8) . . ? C10 C9 C14 118.0(9) . . ? C8 C9 C14 119.5(7) . . ? C11 C10 C9 122.2(10) . . ? C11 C10 H14 118.9 . . ? C9 C10 H14 118.9 . . ? C10 C11 C12 119.8(9) . . ? C10 C11 H15 120.1 . . ? C12 C11 H15 120.1 . . ? C13 C12 C11 121.0(11) . . ? C13 C12 H16 119.5 . . ? C11 C12 H16 119.5 . . ? C12 C13 C14 121.4(8) . . ? C12 C13 H17 119.3 . . ? C14 C13 H17 119.3 . . ? C13 C14 C5 124.4(6) . . ? C13 C14 C9 117.7(6) . . ? C5 C14 C9 117.9(6) . . ? N2 C15 P2 111.6(3) . . ? N2 C15 H18 109.3 . . ? P2 C15 H18 109.3 . . ? N2 C15 H19 109.3 . . ? P2 C15 H19 109.3 . . ? H18 C15 H19 108.0 . . ? O10 C16 O9 124.0(5) . . ? O10 C16 C17 118.2(5) . . ? O9 C16 C17 117.7(4) . . ? N2 C17 C16 111.5(4) . . ? N2 C17 H20 109.3 . . ? C16 C17 H20 109.3 . . ? N2 C17 H21 109.3 . . ? C16 C17 H21 109.3 . . ? H20 C17 H21 108.0 . . ? N2 C18 C19 116.5(4) . . ? N2 C18 H22 108.2 . . ? C19 C18 H22 108.2 . . ? N2 C18 H23 108.2 . . ? C19 C18 H23 108.2 . . ? H22 C18 H23 107.3 . . ? C20 C19 C28 119.4(5) . . ? C20 C19 C18 117.8(5) . . ? C28 C19 C18 122.8(4) . . ? C19 C20 C21 121.2(6) . . ? C19 C20 H24 119.4 . . ? C21 C20 H24 119.4 . . ? C22 C21 C20 119.6(6) . . ? C22 C21 H25 120.2 . . ? C20 C21 H25 120.2 . . ? C21 C22 C23 122.3(5) . . ? C21 C22 H26 118.9 . . ? C23 C22 H26 118.9 . . ? C22 C23 C24 122.1(6) . . ? C22 C23 C28 118.9(5) . . ? C24 C23 C28 119.0(6) . . ? C25 C24 C23 120.9(7) . . ? C25 C24 H27 119.5 . . ? C23 C24 H27 119.5 . . ? C24 C25 C26 121.0(7) . . ? C24 C25 H28 119.5 . . ? C26 C25 H28 119.5 . . ? C27 C26 C25 119.6(7) . . ? C27 C26 H29 120.2 . . ? C25 C26 H29 120.2 . . ? C26 C27 C28 121.2(6) . . ? C26 C27 H30 119.4 . . ? C28 C27 H30 119.4 . . ? C27 C28 C23 118.2(5) . . ? C27 C28 C19 123.3(5) . . ? C23 C28 C19 118.4(5) . . ? N3 C29 P3 111.0(3) . . ? N3 C29 H31 109.4 . . ? P3 C29 H31 109.4 . . ? N3 C29 H32 109.4 . . ? P3 C29 H32 109.4 . . ? H31 C29 H32 108.0 . . ? O15 C30 O14 125.0(5) . . ? O15 C30 C31 119.0(5) . . ? O14 C30 C31 115.9(4) . . ? N3 C31 C30 112.6(4) . . ? N3 C31 H33 109.1 . . ? C30 C31 H33 109.1 . . ? N3 C31 H34 109.1 . . ? C30 C31 H34 109.1 . . ? H33 C31 H34 107.8 . . ? N3 C32 C33 116.5(4) . . ? N3 C32 H35 108.2 . . ? C33 C32 H35 108.2 . . ? N3 C32 H36 108.2 . . ? C33 C32 H36 108.2 . . ? H35 C32 H36 107.3 . . ? C34 C33 C42 120.2(5) . . ? C34 C33 C32 118.2(5) . . ? C42 C33 C32 121.6(5) . . ? C33 C34 C35 120.9(7) . . ? C33 C34 H37 119.6 . . ? C35 C34 H37 119.6 . . ? C36 C35 C34 119.0(7) . . ? C36 C35 H38 120.5 . . ? C34 C35 H38 120.5 . . ? C35 C36 C37 122.9(7) . . ? C35 C36 H39 118.5 . . ? C37 C36 H39 118.5 . . ? C36 C37 C42 118.1(6) . . ? C36 C37 C38 123.0(7) . . ? C42 C37 C38 118.9(7) . . ? C39 C38 C37 120.9(7) . . ? C39 C38 H40 119.6 . . ? C37 C38 H40 119.6 . . ? C38 C39 C40 119.7(7) . . ? C38 C39 H41 120.1 . . ? C40 C39 H41 120.1 . . ? C41 C40 C39 122.0(8) . . ? C41 C40 H42 119.0 . . ? C39 C40 H42 119.0 . . ? C40 C41 C42 120.7(6) . . ? C40 C41 H43 119.6 . . ? C42 C41 H43 119.6 . . ? C37 C42 C41 117.7(6) . . ? C37 C42 C33 118.9(6) . . ? C41 C42 C33 123.4(5) . . ? C44 C43 N4 109.2(14) . . ? C44 C43 H44 109.8 . . ? N4 C43 H44 109.8 . . ? C44 C43 H45 109.8 . . ? N4 C43 H45 109.8 . . ? H44 C43 H45 108.3 . . ? C43 C44 H46 109.5 . . ? C43 C44 H47 109.5 . . ? H46 C44 H47 109.5 . . ? C43 C44 H48 109.5 . . ? H46 C44 H48 109.5 . . ? H47 C44 H48 109.5 . . ? N4 C45 C46 104.9(10) . . ? N4 C45 H49 110.8 . . ? C46 C45 H49 110.8 . . ? N4 C45 H50 110.8 . . ? C46 C45 H50 110.8 . . ? H49 C45 H50 108.8 . . ? C45 C46 H51 109.5 . . ? C45 C46 H52 109.5 . . ? H51 C46 H52 109.5 . . ? C45 C46 H53 109.5 . . ? H51 C46 H53 109.5 . . ? H52 C46 H53 109.5 . . ? C48 C47 N4 123.2(11) . . ? C48 C47 H54 106.5 . . ? N4 C47 H54 106.5 . . ? C48 C47 H55 106.5 . . ? N4 C47 H55 106.5 . . ? H54 C47 H55 106.5 . . ? C47 C48 H56 109.5 . . ? C47 C48 H57 109.5 . . ? H56 C48 H57 109.5 . . ? C47 C48 H58 109.5 . . ? H56 C48 H58 109.5 . . ? H57 C48 H58 109.5 . . ? N5 C49 C50 114.4(6) . . ? N5 C49 H59 108.7 . . ? C50 C49 H59 108.7 . . ? N5 C49 H80 108.7 . . ? C50 C49 H80 108.7 . . ? H59 C49 H80 107.6 . . ? C49 C50 H61 109.5 . . ? C49 C50 H62 109.5 . . ? H61 C50 H62 109.5 . . ? C49 C50 H63 109.5 . . ? H61 C50 H63 109.5 . . ? H62 C50 H63 109.5 . . ? C52 C51 N5 112.7(6) . . ? C52 C51 H64 109.1 . . ? N5 C51 H64 109.1 . . ? C52 C51 H65 109.1 . . ? N5 C51 H65 109.1 . . ? H64 C51 H65 107.8 . . ? C51 C52 H66 109.5 . . ? C51 C52 H67 109.5 . . ? H66 C52 H67 109.5 . . ? C51 C52 H68 109.5 . . ? H66 C52 H68 109.5 . . ? H67 C52 H68 109.5 . . ? N5 C53 C54 110.3(7) . . ? N5 C53 H69 109.6 . . ? C54 C53 H69 109.6 . . ? N5 C53 H70 109.6 . . ? C54 C53 H70 109.6 . . ? H69 C53 H70 108.1 . . ? C53 C54 H71 109.5 . . ? C53 C54 H72 109.5 . . ? H71 C54 H72 109.5 . . ? C53 C54 H73 109.5 . . ? H71 C54 H73 109.5 . . ? H72 C54 H73 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N4 H3 O10 0.91 2.02 2.887(9) 159.2 2_556 N5 H4 O14 0.91 1.87 2.776(6) 172.2 1_455 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.058 _refine_diff_density_min -0.721 _refine_diff_density_rms 0.091 _database_code_depnum_ccdc_archive 'CCDC 925302' ####################################################################### # # 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_f1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C96 H150 N14 O48 P6 Zn9' _chemical_formula_weight 3042.45 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' P P 0.1023 0.0942 '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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.836(6) _cell_length_b 22.682(8) _cell_length_c 18.490(7) _cell_angle_alpha 90.00 _cell_angle_beta 105.990(6) _cell_angle_gamma 90.00 _cell_volume 6384(4) _cell_formula_units_Z 2 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 18299 _cell_measurement_theta_min 2.6048 _cell_measurement_theta_max 27.3699 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.2800 _exptl_crystal_size_mid 0.2300 _exptl_crystal_size_min 0.2000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.583 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3136 _exptl_absorpt_coefficient_mu 1.824 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8388 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(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 'Saturn724+ (2x2 bin mode)' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 49552 _diffrn_reflns_av_R_equivalents 0.0310 _diffrn_reflns_av_sigmaI/netI 0.0311 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 27.37 _reflns_number_total 14387 _reflns_number_gt 13184 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _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. Due to the moderate diffraction intensity, as well as abnormal phosphonate ligand and triethylenetetramine, so hydrogen atoms were generated geometrically. One phosphonate ligand (N3C32C33C34C35C36C37C38C39C40C41C42) and one triethylenetetramine(N4C43C44N5C45C46N6C47C48N7),as well as four free water molecules (O15,O19,O20,O23) are abnormal, so the distance/angle and isotropic are restrained. The restraints used in the refinement are listed as follows: exyz n5 n5a eadp n5 n5a eadp c32 c32a dfix 1.46 0.01 n4 c43 n5 c44 n5 c45 n6 c46 n6 c47 n7 c48 dfix 1.52 0.01 c43 c44 c45 c46 c47 c48 c45a c46a c47a c48a dfix 1.46 n5a c45a n6a c46a n6a c47a n7a c48a dfix 1.51 0.01 c32 c33 n3 c32 dfix 1.38 0.01 c37 c38 c38 c39 c39 c40 c40 c41 c41 c42 dfix 2.39 c37 c39 c38 c40 c39 c41 c40 c42 c41 c37 flat 0.01 c35 c37 c38 c39 c40 c41 c42 c32 dfix 1.51 0.01 c32a c33a n3 c32a dfix 1.38 0.01 c37a c38a c38a c39a c39a c40a c40a c41a c41a c42a dfix 2.39 c37a c39a c38a c40a c39a c41a c40a c42a c41a c37a flat 0.01 c35a c37a c38a c39a c40a c41a c42a c32a isor 0.01 o15 o19 o20 o23 c32a c48 n7a ; _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^)+(0.0880P)^2^+10.8502P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14387 _refine_ls_number_parameters 906 _refine_ls_number_restraints 91 _refine_ls_R_factor_all 0.0658 _refine_ls_R_factor_gt 0.0609 _refine_ls_wR_factor_ref 0.1730 _refine_ls_wR_factor_gt 0.1685 _refine_ls_goodness_of_fit_ref 1.121 _refine_ls_restrained_S_all 1.144 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.0000 0.5000 0.5000 0.02626(14) Uani 1 2 d S . . Zn2 Zn 0.21676(3) 0.55842(2) 0.58950(2) 0.03145(12) Uani 1 1 d . . . Zn3 Zn 0.05763(3) 0.58476(2) 0.35422(2) 0.03228(12) Uani 1 1 d . . . Zn4 Zn 0.14991(3) 0.37128(2) 0.53131(3) 0.03415(13) Uani 1 1 d . . . Zn5 Zn 0.41663(5) 0.73449(3) 0.66709(4) 0.0679(2) Uani 1 1 d . . . P1 P -0.05538(6) 0.36102(4) 0.49320(5) 0.0289(2) Uani 1 1 d . . . P2 P 0.13626(7) 0.45586(5) 0.65936(6) 0.0326(2) Uani 1 1 d . . . P3 P 0.18001(6) 0.48565(5) 0.44405(6) 0.0314(2) Uani 1 1 d . . . O1 O 0.01568(17) 0.40793(11) 0.49606(15) 0.0302(5) Uani 1 1 d . . . O2 O -0.14094(18) 0.37103(12) 0.43143(17) 0.0371(6) Uani 1 1 d . . . O3 O -0.07005(19) 0.35139(12) 0.57079(16) 0.0353(6) Uani 1 1 d . . . O4 O 0.2559(2) 0.31394(14) 0.5462(2) 0.0515(8) Uani 1 1 d . . . O5 O 0.2939(2) 0.23045(16) 0.4983(3) 0.0613(10) Uani 1 1 d . . . O6 O 0.11028(17) 0.50184(11) 0.59552(14) 0.0300(5) Uani 1 1 d . . . O7 O 0.0628(2) 0.44281(14) 0.69613(16) 0.0407(7) Uani 1 1 d . . . O8 O 0.1746(2) 0.39984(12) 0.63492(16) 0.0386(6) Uani 1 1 d . . . O9 O 0.32789(19) 0.61462(13) 0.61935(16) 0.0395(6) Uani 1 1 d . B . O10 O 0.3998(3) 0.66296(16) 0.72373(19) 0.0600(10) Uani 1 1 d . B . O11 O 0.08760(17) 0.51286(11) 0.43097(14) 0.0291(5) Uani 1 1 d . . . O12 O 0.24697(19) 0.51591(14) 0.50888(17) 0.0412(7) Uani 1 1 d . . . O13 O 0.18085(19) 0.41861(12) 0.45165(16) 0.0360(6) Uani 1 1 d . . . O14 O 0.0537(2) 0.63724(15) 0.26053(18) 0.0481(8) Uani 1 1 d . A . O15 O 0.0910(4) 0.6363(2) 0.1525(3) 0.0956(17) Uani 1 1 d U A . O16 O 0.7787(4) 0.2155(3) 0.2223(3) 0.1058(19) Uani 1 1 d . . . O17 O 0.8201(4) 0.3856(2) 0.9521(3) 0.1035(19) Uani 1 1 d . . . O18 O 0.8395(4) 0.3283(3) 0.2799(4) 0.124(2) Uani 1 1 d . . . O19 O 1.1339(5) 0.3492(3) 0.3208(3) 0.124(2) Uani 1 1 d U . . O20 O 0.9597(5) 0.4921(4) 0.1805(5) 0.145(3) Uani 1 1 d U . . O21 O 0.5464(5) 0.8085(4) 0.4094(4) 0.153(3) Uani 1 1 d . . . O22 O 0.9595(7) 0.3748(5) 0.2159(6) 0.181(4) Uani 1 1 d . . . O23 O -0.2028(11) 0.6637(7) -0.1963(8) 0.276(6) Uani 1 1 d U . . O24 O 0.8868(12) 0.4861(8) 1.0236(8) 0.309(9) Uani 1 1 d . . . N1 N 0.0848(2) 0.28657(14) 0.51051(18) 0.0314(7) Uani 1 1 d . . . N2 N 0.2865(2) 0.52244(15) 0.69606(18) 0.0339(7) Uani 1 1 d . . . N3 N 0.1812(2) 0.56302(15) 0.3311(2) 0.0402(8) Uani 1 1 d D . . C1 C -0.0080(3) 0.29493(17) 0.4632(2) 0.0319(8) Uani 1 1 d . . . H1 H -0.0428 0.2607 0.4680 0.038 Uiso 1 1 calc R . . H2 H -0.0088 0.2987 0.4108 0.038 Uiso 1 1 calc R . . C2 C 0.1399(3) 0.25418(18) 0.4701(2) 0.0381(9) Uani 1 1 d . . . H3 H 0.1246 0.2664 0.4178 0.046 Uiso 1 1 calc R . . H4 H 0.1293 0.2122 0.4716 0.046 Uiso 1 1 calc R . . C3 C 0.2385(3) 0.2675(2) 0.5080(3) 0.0457(10) Uani 1 1 d . . . C4 C 0.0883(3) 0.25860(18) 0.5855(2) 0.0355(8) Uani 1 1 d . . . H5 H 0.0612 0.2854 0.6133 0.043 Uiso 1 1 calc R . . H6 H 0.1495 0.2545 0.6137 0.043 Uiso 1 1 calc R . . C5 C 0.0442(3) 0.19844(19) 0.5828(2) 0.0396(9) Uani 1 1 d . . . C6 C -0.0429(3) 0.1965(2) 0.5835(3) 0.0510(12) Uani 1 1 d . . . H7 H -0.0720 0.2315 0.5869 0.061 Uiso 1 1 calc R . . C7 C -0.0891(4) 0.1423(3) 0.5792(3) 0.0643(16) Uani 1 1 d . . . H8 H -0.1473 0.1423 0.5807 0.077 Uiso 1 1 calc R . . C8 C -0.0487(4) 0.0908(3) 0.5729(3) 0.0604(15) Uani 1 1 d . . . H9 H -0.0802 0.0558 0.5685 0.073 Uiso 1 1 calc R . . C9 C 0.0413(4) 0.0892(2) 0.5728(3) 0.0493(12) Uani 1 1 d . . . C10 C 0.0847(4) 0.0362(2) 0.5697(3) 0.0552(13) Uani 1 1 d . . . H10 H 0.0533 0.0011 0.5648 0.066 Uiso 1 1 calc R . . C11 C 0.1731(4) 0.0344(2) 0.5735(3) 0.0582(14) Uani 1 1 d . . . H11 H 0.2004 -0.0014 0.5699 0.070 Uiso 1 1 calc R . . C12 C 0.2213(4) 0.0872(2) 0.5830(3) 0.0503(11) Uani 1 1 d . . . H12 H 0.2811 0.0860 0.5869 0.060 Uiso 1 1 calc R . . C13 C 0.1814(3) 0.1404(2) 0.5866(2) 0.0433(10) Uani 1 1 d . . . H13 H 0.2148 0.1747 0.5934 0.052 Uiso 1 1 calc R . . C14 C 0.0901(3) 0.1441(2) 0.5802(2) 0.0412(9) Uani 1 1 d . . . C15 C 0.2227(3) 0.49357(18) 0.7311(2) 0.0347(8) Uani 1 1 d . . . H14 H 0.1965 0.5231 0.7562 0.042 Uiso 1 1 calc R . . H15 H 0.2534 0.4653 0.7686 0.042 Uiso 1 1 calc R . . C16 C 0.3310(3) 0.57363(18) 0.7400(2) 0.0352(8) Uani 1 1 d . B . H16 H 0.3840 0.5604 0.7767 0.042 Uiso 1 1 calc R . . H17 H 0.2927 0.5910 0.7671 0.042 Uiso 1 1 calc R . . C17 C 0.3547(3) 0.6200(2) 0.6896(3) 0.0410(9) Uani 1 1 d . . . C18 C 0.3516(3) 0.47903(19) 0.6788(2) 0.0370(8) Uani 1 1 d . . . H18 H 0.3799 0.4978 0.6445 0.044 Uiso 1 1 calc R . . H19 H 0.3191 0.4454 0.6528 0.044 Uiso 1 1 calc R . . C19 C 0.4226(3) 0.45660(19) 0.7466(3) 0.0405(9) Uani 1 1 d . . . C20 C 0.4052(4) 0.4098(2) 0.7888(3) 0.0507(11) Uani 1 1 d . . . H20 H 0.3498 0.3925 0.7749 0.061 Uiso 1 1 calc R . . C21 C 0.4693(4) 0.3876(2) 0.8523(3) 0.0616(14) Uani 1 1 d . . . H21 H 0.4552 0.3572 0.8806 0.074 Uiso 1 1 calc R . . C22 C 0.5523(4) 0.4111(2) 0.8719(3) 0.0574(14) Uani 1 1 d . . . H22 H 0.5942 0.3964 0.9136 0.069 Uiso 1 1 calc R . . C23 C 0.5750(3) 0.4571(2) 0.8298(3) 0.0497(12) Uani 1 1 d . . . C24 C 0.6617(3) 0.4817(3) 0.8495(3) 0.0614(15) Uani 1 1 d . . . H23 H 0.7042 0.4663 0.8903 0.074 Uiso 1 1 calc R . . C25 C 0.6830(3) 0.5268(3) 0.8099(4) 0.0699(18) Uani 1 1 d . . . H24 H 0.7395 0.5424 0.8244 0.084 Uiso 1 1 calc R . . C26 C 0.6206(3) 0.5507(3) 0.7469(4) 0.0594(14) Uani 1 1 d . . . H25 H 0.6361 0.5812 0.7195 0.071 Uiso 1 1 calc R . . C27 C 0.5369(3) 0.5283(2) 0.7265(3) 0.0491(11) Uani 1 1 d . . . H26 H 0.4960 0.5444 0.6850 0.059 Uiso 1 1 calc R . . C28 C 0.5103(3) 0.4812(2) 0.7668(2) 0.0407(9) Uani 1 1 d . . . C29 C 0.2106(3) 0.50217(19) 0.3578(2) 0.0377(9) Uani 1 1 d . A . H27 H 0.2738 0.4992 0.3673 0.045 Uiso 1 1 calc R . . H28 H 0.1835 0.4737 0.3192 0.045 Uiso 1 1 calc R . . C30 C 0.1647(4) 0.5696(2) 0.2482(3) 0.0585(15) Uani 1 1 d . A . H29 H 0.1424 0.5327 0.2237 0.070 Uiso 1 1 calc R . . H30 H 0.2196 0.5784 0.2367 0.070 Uiso 1 1 calc R . . C31 C 0.0989(4) 0.6185(2) 0.2177(3) 0.0606(15) Uani 1 1 d . . . C32 C 0.2479(5) 0.6045(3) 0.3810(5) 0.035(2) Uani 0.543(7) 1 d PD A 1 H32A H 0.2438 0.5979 0.4318 0.042 Uiso 0.543(7) 1 calc PR A 1 H32B H 0.2257 0.6440 0.3674 0.042 Uiso 0.543(7) 1 calc PR A 1 C33 C 0.3475(3) 0.6072(2) 0.3872(3) 0.042(2) Uani 0.543(7) 1 d PGD A 1 C34 C 0.4027(4) 0.5737(3) 0.4438(3) 0.037(3) Uani 0.543(7) 1 d PG A 1 H34A H 0.3791 0.5492 0.4736 0.044 Uiso 0.543(7) 1 calc PR A 1 C35 C 0.4932(4) 0.5770(4) 0.4561(4) 0.062(4) Uani 0.543(7) 1 d PGD A 1 H35A H 0.5301 0.5546 0.4940 0.074 Uiso 0.543(7) 1 calc PR A 1 C36 C 0.5285(3) 0.6136(4) 0.4117(5) 0.076(5) Uani 0.543(7) 1 d PG A 1 H36A H 0.5891 0.6158 0.4199 0.091 Uiso 0.543(7) 1 calc PR A 1 C37 C 0.4734(4) 0.6470(3) 0.3550(4) 0.044(3) Uani 0.543(7) 1 d PGD A 1 C42 C 0.3828(4) 0.64381(19) 0.3427(3) 0.049(2) Uani 0.543(7) 1 d PGD A 1 C38 C 0.5102(7) 0.6830(3) 0.3105(5) 0.069(3) Uani 0.543(7) 1 d PD A 1 H38A H 0.5709 0.6834 0.3191 0.082 Uiso 0.543(7) 1 calc PR A 1 C39 C 0.4597(6) 0.7177(4) 0.2544(5) 0.081(4) Uani 0.543(7) 1 d PD A 1 H39A H 0.4849 0.7417 0.2252 0.098 Uiso 0.543(7) 1 calc PR A 1 C40 C 0.3702(7) 0.7155(4) 0.2429(6) 0.074(4) Uani 0.543(7) 1 d PD A 1 H40A H 0.3346 0.7386 0.2050 0.088 Uiso 0.543(7) 1 calc PR A 1 C41 C 0.3312(7) 0.6802(3) 0.2857(5) 0.052(3) Uani 0.543(7) 1 d PD A 1 H41A H 0.2704 0.6805 0.2768 0.062 Uiso 0.543(7) 1 calc PR A 1 C32A C 0.2301(6) 0.6169(4) 0.3628(7) 0.035(2) Uani 0.46 1 d PDU A 2 H32C H 0.2444 0.6139 0.4172 0.042 Uiso 0.457(7) 1 calc PR A 2 H32D H 0.1903 0.6500 0.3482 0.042 Uiso 0.457(7) 1 calc PR A 2 C33A C 0.3145(3) 0.6322(3) 0.3425(4) 0.037(2) Uani 0.457(7) 1 d PGD A 2 C34A C 0.3036(4) 0.6672(3) 0.2788(4) 0.048(4) Uani 0.457(7) 1 d PG A 2 H34B H 0.2475 0.6769 0.2498 0.058 Uiso 0.457(7) 1 calc PR A 2 C35A C 0.3767(6) 0.6875(3) 0.2586(4) 0.068(4) Uani 0.457(7) 1 d PGD A 2 H35B H 0.3694 0.7109 0.2160 0.082 Uiso 0.457(7) 1 calc PR A 2 C36A C 0.4606(5) 0.6729(4) 0.3019(5) 0.064(4) Uani 0.457(7) 1 d PG A 2 H36B H 0.5095 0.6865 0.2883 0.077 Uiso 0.457(7) 1 calc PR A 2 C37A C 0.4715(3) 0.6379(3) 0.3655(5) 0.058(5) Uani 0.457(7) 1 d PGD A 2 C42A C 0.3984(4) 0.6175(2) 0.3858(3) 0.038(2) Uani 0.457(7) 1 d PGD A 2 C38A C 0.5561(7) 0.6235(4) 0.4067(6) 0.059(4) Uani 0.457(7) 1 d PD A 2 H38B H 0.6035 0.6367 0.3906 0.071 Uiso 0.457(7) 1 calc PR A 2 C39A C 0.5707(6) 0.5902(5) 0.4708(6) 0.072(4) Uani 0.457(7) 1 d PD A 2 H39B H 0.6276 0.5812 0.4987 0.087 Uiso 0.457(7) 1 calc PR A 2 C40A C 0.4997(7) 0.5702(5) 0.4933(6) 0.068(5) Uani 0.457(7) 1 d PD A 2 H40B H 0.5087 0.5473 0.5365 0.082 Uiso 0.457(7) 1 calc PR A 2 C41A C 0.4151(8) 0.5842(4) 0.4521(5) 0.062(5) Uani 0.457(7) 1 d PD A 2 H41B H 0.3680 0.5712 0.4688 0.074 Uiso 0.457(7) 1 calc PR A 2 N4 N 0.3714(5) 0.8099(2) 0.7090(3) 0.090(2) Uani 1 1 d D B . H4A H 0.3447 0.8001 0.7444 0.109 Uiso 1 1 calc R . . H4B H 0.4167 0.8340 0.7300 0.109 Uiso 1 1 calc R . . C43 C 0.3078(6) 0.8404(3) 0.6445(5) 0.101(3) Uani 1 1 d D . . H43A H 0.3387 0.8575 0.6110 0.122 Uiso 1 1 calc R B . H43B H 0.2777 0.8718 0.6631 0.122 Uiso 1 1 calc R . . C44 C 0.2425(5) 0.7954(3) 0.6030(4) 0.084(2) Uani 1 1 d D B . H44A H 0.2065 0.8129 0.5576 0.101 Uiso 1 1 d R . . H44B H 0.2049 0.7844 0.6336 0.101 Uiso 1 1 d R . . N5 N 0.2842(3) 0.7432(2) 0.5833(3) 0.0622(15) Uani 0.550(11) 1 d PD B 1 H5A H 0.2508 0.7104 0.5823 0.075 Uiso 0.550(11) 1 calc PR B 1 C45 C 0.3080(13) 0.7509(10) 0.5126(7) 0.079(6) Uani 0.550(11) 1 d PD B 1 H45A H 0.3118 0.7927 0.5026 0.095 Uiso 0.550(11) 1 calc PR B 1 H45B H 0.2624 0.7340 0.4716 0.095 Uiso 0.550(11) 1 calc PR B 1 C46 C 0.3957(10) 0.7216(7) 0.5156(9) 0.080(5) Uani 0.550(11) 1 d PD B 1 H46A H 0.3890 0.6791 0.5177 0.096 Uiso 0.550(11) 1 calc PR B 1 H46B H 0.4114 0.7307 0.4697 0.096 Uiso 0.550(11) 1 calc PR B 1 N6 N 0.4669(9) 0.7404(6) 0.5801(7) 0.079(4) Uani 0.550(11) 1 d PD B 1 H6A H 0.4824 0.7783 0.5739 0.095 Uiso 0.550(11) 1 calc PR B 1 C47 C 0.5448(10) 0.7026(7) 0.6013(10) 0.100(6) Uani 0.550(11) 1 d PD B 1 H47A H 0.5759 0.7050 0.5629 0.119 Uiso 0.550(11) 1 calc PR B 1 H47B H 0.5269 0.6620 0.6043 0.119 Uiso 0.550(11) 1 calc PR B 1 C48 C 0.6064(11) 0.7211(8) 0.6769(9) 0.090(5) Uani 0.550(11) 1 d PDU B 1 H48A H 0.6516 0.6914 0.6943 0.108 Uiso 0.550(11) 1 calc PR B 1 H48B H 0.6347 0.7581 0.6716 0.108 Uiso 0.550(11) 1 calc PR B 1 N7 N 0.5544(8) 0.7276(5) 0.7315(9) 0.074(3) Uani 0.550(11) 1 d PD B 1 H7A H 0.5712 0.7602 0.7595 0.089 Uiso 0.550(11) 1 calc PR B 1 H7B H 0.5624 0.6962 0.7623 0.089 Uiso 0.550(11) 1 calc PR B 1 N5A N 0.2842(3) 0.7432(2) 0.5833(3) 0.0622(15) Uani 0.45 1 d PD B 2 H5B H 0.2526 0.7128 0.5947 0.075 Uiso 0.450(11) 1 calc PR B 2 C45A C 0.2805(13) 0.7335(13) 0.5047(10) 0.089(9) Uani 0.450(11) 1 d PD B 2 H45C H 0.2362 0.7585 0.4722 0.107 Uiso 0.450(11) 1 calc PR B 2 H45D H 0.2666 0.6927 0.4908 0.107 Uiso 0.450(11) 1 calc PR B 2 C46A C 0.3717(11) 0.7493(7) 0.4979(8) 0.061(4) Uani 0.450(11) 1 d PD B 2 H46C H 0.3746 0.7407 0.4473 0.073 Uiso 0.450(11) 1 calc PR B 2 H46D H 0.3816 0.7912 0.5066 0.073 Uiso 0.450(11) 1 calc PR B 2 N6A N 0.4418(8) 0.7158(6) 0.5528(8) 0.054(3) Uani 0.450(11) 1 d PD B 2 H6AA H 0.4342 0.6766 0.5426 0.065 Uiso 0.450(11) 1 calc PR B 2 C47A C 0.5306(8) 0.7322(7) 0.5540(9) 0.076(5) Uani 0.450(11) 1 d PD B 2 H47C H 0.5353 0.7747 0.5508 0.092 Uiso 0.450(11) 1 calc PR B 2 H47D H 0.5458 0.7148 0.5113 0.092 Uiso 0.450(11) 1 calc PR B 2 C48A C 0.5931(12) 0.7098(10) 0.6272(11) 0.090(7) Uani 0.450(11) 1 d PD B 2 H48C H 0.5949 0.6671 0.6268 0.109 Uiso 0.450(11) 1 calc PR B 2 H48D H 0.6519 0.7245 0.6320 0.109 Uiso 0.450(11) 1 calc PR B 2 N7A N 0.5625(12) 0.7303(8) 0.6911(10) 0.080(5) Uani 0.450(11) 1 d PDU B 2 H7C H 0.5848 0.7664 0.7047 0.095 Uiso 0.450(11) 1 calc PR B 2 H7D H 0.5837 0.7059 0.7303 0.095 Uiso 0.450(11) 1 calc PR B 2 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 0.0263(3) 0.0258(3) 0.0273(3) -0.0008(2) 0.0084(2) -0.0051(2) Zn2 0.0287(2) 0.0328(2) 0.0306(2) -0.00136(17) 0.00450(17) -0.00621(17) Zn3 0.0364(3) 0.0326(2) 0.0308(2) 0.00201(17) 0.01429(19) -0.00408(18) Zn4 0.0330(3) 0.0287(2) 0.0400(3) -0.00038(17) 0.00877(19) -0.00385(17) Zn5 0.0620(4) 0.0578(4) 0.0746(4) 0.0171(3) 0.0032(3) -0.0176(3) P1 0.0295(5) 0.0261(5) 0.0315(5) -0.0015(3) 0.0090(4) -0.0054(4) P2 0.0336(5) 0.0315(5) 0.0303(5) 0.0021(4) 0.0046(4) -0.0056(4) P3 0.0282(5) 0.0344(5) 0.0337(5) -0.0041(4) 0.0120(4) -0.0050(4) O1 0.0293(13) 0.0274(13) 0.0342(13) -0.0019(10) 0.0092(11) -0.0049(10) O2 0.0312(14) 0.0314(14) 0.0447(16) -0.0008(11) 0.0039(12) -0.0057(11) O3 0.0403(15) 0.0328(14) 0.0371(14) -0.0001(11) 0.0180(12) -0.0036(12) O4 0.0389(17) 0.0363(17) 0.077(2) 0.0012(16) 0.0123(16) 0.0002(13) O5 0.049(2) 0.050(2) 0.092(3) 0.0020(19) 0.032(2) 0.0068(16) O6 0.0277(13) 0.0313(14) 0.0293(12) 0.0008(10) 0.0049(10) -0.0058(10) O7 0.0401(16) 0.0480(18) 0.0324(14) 0.0054(12) 0.0076(12) -0.0093(13) O8 0.0411(16) 0.0289(14) 0.0403(15) -0.0005(11) 0.0021(12) -0.0022(12) O9 0.0359(15) 0.0408(16) 0.0381(15) -0.0024(12) 0.0041(12) -0.0115(12) O10 0.072(2) 0.048(2) 0.0458(18) 0.0013(15) -0.0082(17) -0.0280(18) O11 0.0286(13) 0.0294(13) 0.0325(13) -0.0010(10) 0.0140(10) -0.0035(10) O12 0.0295(14) 0.0505(18) 0.0448(16) -0.0115(13) 0.0123(12) -0.0086(13) O13 0.0343(15) 0.0330(15) 0.0428(15) -0.0003(12) 0.0139(12) 0.0007(11) O14 0.062(2) 0.0460(18) 0.0435(17) 0.0110(14) 0.0273(15) 0.0003(15) O15 0.166(5) 0.074(3) 0.075(3) 0.035(2) 0.080(3) 0.034(3) O16 0.088(4) 0.117(5) 0.092(4) -0.019(3) -0.009(3) 0.027(3) O17 0.157(5) 0.087(4) 0.086(3) 0.023(3) 0.066(4) 0.048(4) O18 0.125(5) 0.126(5) 0.095(4) -0.028(4) -0.015(4) 0.028(4) O19 0.213(6) 0.078(3) 0.070(3) -0.013(3) 0.024(4) -0.029(4) O20 0.147(6) 0.155(6) 0.153(6) -0.054(5) 0.076(5) -0.045(5) O21 0.098(5) 0.220(9) 0.119(5) 0.036(6) -0.008(4) -0.007(5) O22 0.207(10) 0.185(9) 0.162(8) -0.034(7) 0.071(7) -0.019(8) O23 0.354(11) 0.252(10) 0.249(10) 0.007(8) 0.130(8) -0.051(8) O24 0.41(2) 0.35(2) 0.192(12) -0.087(13) 0.116(14) -0.150(18) N1 0.0326(16) 0.0274(16) 0.0344(16) -0.0005(12) 0.0098(13) -0.0025(13) N2 0.0326(17) 0.0325(17) 0.0338(16) -0.0044(13) 0.0047(13) -0.0033(13) N3 0.050(2) 0.0330(18) 0.047(2) -0.0027(15) 0.0303(17) -0.0074(15) C1 0.037(2) 0.0284(18) 0.0295(17) -0.0019(14) 0.0085(15) -0.0055(15) C2 0.047(2) 0.033(2) 0.038(2) 0.0011(16) 0.0181(18) 0.0026(17) C3 0.043(2) 0.038(2) 0.062(3) 0.010(2) 0.024(2) 0.0048(19) C4 0.042(2) 0.032(2) 0.0321(18) 0.0000(15) 0.0099(16) -0.0001(16) C5 0.046(2) 0.038(2) 0.0323(19) 0.0074(16) 0.0073(17) -0.0053(18) C6 0.047(3) 0.055(3) 0.052(3) 0.019(2) 0.016(2) -0.003(2) C7 0.047(3) 0.070(4) 0.073(4) 0.034(3) 0.013(3) -0.010(3) C8 0.057(3) 0.056(3) 0.059(3) 0.023(2) 0.001(2) -0.022(3) C9 0.066(3) 0.039(2) 0.036(2) 0.0105(18) 0.002(2) -0.012(2) C10 0.080(4) 0.039(3) 0.038(2) 0.0037(19) 0.002(2) -0.012(2) C11 0.095(5) 0.040(3) 0.038(2) 0.0041(19) 0.016(3) 0.005(3) C12 0.064(3) 0.046(3) 0.042(2) 0.0075(19) 0.017(2) 0.007(2) C13 0.055(3) 0.037(2) 0.037(2) 0.0089(17) 0.0127(19) -0.0022(19) C14 0.049(3) 0.038(2) 0.0330(19) 0.0067(16) 0.0064(18) -0.0066(18) C15 0.037(2) 0.035(2) 0.0302(18) 0.0008(15) 0.0059(16) -0.0055(16) C16 0.034(2) 0.032(2) 0.0345(19) -0.0046(15) 0.0013(16) -0.0062(16) C17 0.033(2) 0.039(2) 0.045(2) -0.0024(18) 0.0009(17) -0.0073(17) C18 0.033(2) 0.035(2) 0.040(2) -0.0048(16) 0.0051(16) -0.0021(16) C19 0.041(2) 0.034(2) 0.045(2) -0.0033(17) 0.0082(18) 0.0051(17) C20 0.054(3) 0.035(2) 0.062(3) 0.004(2) 0.016(2) 0.004(2) C21 0.080(4) 0.043(3) 0.063(3) 0.011(2) 0.021(3) 0.019(3) C22 0.068(4) 0.049(3) 0.048(3) 0.000(2) 0.005(2) 0.023(3) C23 0.046(3) 0.051(3) 0.047(2) -0.014(2) 0.004(2) 0.017(2) C24 0.038(3) 0.071(4) 0.066(3) -0.024(3) -0.002(2) 0.022(3) C25 0.033(3) 0.080(4) 0.096(5) -0.038(4) 0.015(3) 0.001(3) C26 0.041(3) 0.060(3) 0.082(4) -0.016(3) 0.025(3) -0.003(2) C27 0.039(2) 0.052(3) 0.057(3) -0.006(2) 0.015(2) 0.001(2) C28 0.036(2) 0.041(2) 0.043(2) -0.0096(18) 0.0066(18) 0.0073(17) C29 0.036(2) 0.039(2) 0.043(2) -0.0075(17) 0.0196(18) -0.0046(16) C30 0.099(4) 0.039(2) 0.059(3) 0.001(2) 0.057(3) -0.004(3) C31 0.102(5) 0.045(3) 0.051(3) 0.008(2) 0.048(3) -0.001(3) C32 0.035(4) 0.023(4) 0.052(5) 0.007(3) 0.020(3) 0.006(3) C33 0.040(5) 0.031(4) 0.059(5) 0.001(4) 0.021(4) -0.003(4) C34 0.030(5) 0.021(4) 0.058(6) 0.006(4) 0.012(4) -0.002(4) C35 0.040(7) 0.045(6) 0.095(11) -0.003(6) 0.009(6) 0.003(5) C36 0.068(10) 0.062(8) 0.121(13) -0.028(8) 0.065(10) -0.023(7) C37 0.036(7) 0.047(6) 0.061(7) -0.009(6) 0.031(6) -0.014(5) C42 0.060(6) 0.035(4) 0.067(6) -0.001(4) 0.040(5) -0.011(4) C38 0.070(8) 0.075(8) 0.078(8) -0.009(6) 0.047(7) -0.016(6) C39 0.099(10) 0.071(8) 0.098(9) 0.005(7) 0.067(8) -0.029(7) C40 0.089(9) 0.069(9) 0.081(8) -0.008(7) 0.053(7) -0.042(7) C41 0.069(8) 0.033(5) 0.064(7) 0.008(4) 0.036(6) -0.007(6) C32A 0.035(4) 0.023(4) 0.052(5) 0.007(3) 0.020(3) 0.006(3) C33A 0.037(5) 0.027(4) 0.053(6) 0.003(4) 0.025(4) -0.003(4) C34A 0.042(7) 0.050(8) 0.052(7) 0.003(5) 0.010(5) -0.010(6) C35A 0.092(11) 0.051(9) 0.079(9) 0.000(7) 0.052(9) -0.029(8) C36A 0.048(7) 0.061(8) 0.104(11) -0.026(7) 0.056(8) -0.028(6) C37A 0.053(12) 0.038(7) 0.081(11) -0.012(7) 0.012(9) 0.012(7) C42A 0.032(5) 0.033(5) 0.055(6) -0.002(4) 0.020(4) -0.005(4) C38A 0.041(7) 0.060(9) 0.081(10) -0.018(7) 0.025(7) -0.001(6) C39A 0.027(6) 0.085(10) 0.098(11) -0.037(8) 0.004(6) -0.002(6) C40A 0.033(6) 0.044(7) 0.103(13) -0.008(8) -0.024(7) 0.002(5) C41A 0.031(7) 0.064(10) 0.083(12) -0.013(8) 0.004(7) -0.015(7) N4 0.124(5) 0.061(3) 0.068(3) -0.011(3) -0.004(3) -0.033(3) C43 0.117(7) 0.064(4) 0.097(6) -0.015(4) -0.014(5) 0.011(4) C44 0.107(6) 0.073(4) 0.061(4) -0.006(3) 0.006(4) 0.020(4) N5 0.078(3) 0.047(3) 0.055(3) -0.006(2) 0.007(2) -0.007(2) C45 0.108(17) 0.087(13) 0.037(6) -0.002(6) 0.011(8) 0.034(11) C46 0.124(16) 0.062(10) 0.065(10) -0.013(8) 0.044(10) 0.003(10) N6 0.094(9) 0.059(7) 0.091(9) -0.001(6) 0.037(7) -0.012(6) C47 0.119(15) 0.070(10) 0.139(17) 0.001(11) 0.085(14) 0.001(11) C48 0.088(8) 0.079(8) 0.115(9) 0.002(7) 0.046(8) -0.006(7) N7 0.061(6) 0.048(6) 0.112(11) -0.018(7) 0.020(7) -0.012(4) N5A 0.078(3) 0.047(3) 0.055(3) -0.006(2) 0.007(2) -0.007(2) C45A 0.072(12) 0.083(16) 0.088(15) -0.017(10) -0.019(9) 0.011(10) C46A 0.087(11) 0.039(7) 0.052(7) 0.007(6) 0.009(7) 0.006(7) N6A 0.051(7) 0.047(7) 0.057(7) 0.002(6) 0.002(5) -0.002(6) C47A 0.072(9) 0.053(8) 0.122(14) 0.008(8) 0.057(10) -0.005(7) C48A 0.062(11) 0.079(13) 0.123(19) 0.022(13) 0.013(12) 0.000(10) N7A 0.073(8) 0.062(7) 0.090(8) 0.001(7) -0.001(7) -0.016(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 Zn1 O1 2.107(3) 3_566 ? Zn1 O1 2.107(3) . ? Zn1 O6 2.115(3) . ? Zn1 O6 2.115(3) 3_566 ? Zn1 O11 2.148(2) . ? Zn1 O11 2.148(2) 3_566 ? Zn2 O12 1.942(3) . ? Zn2 O2 1.974(3) 3_566 ? Zn2 O9 2.119(3) . ? Zn2 N2 2.138(3) . ? Zn2 O6 2.146(3) . ? Zn3 O3 1.977(3) 3_566 ? Zn3 O7 1.979(3) 3_566 ? Zn3 O14 2.089(3) . ? Zn3 O11 2.128(3) . ? Zn3 N3 2.171(4) . ? Zn4 O8 1.957(3) . ? Zn4 O13 1.990(3) . ? Zn4 O4 2.080(3) . ? Zn4 N1 2.164(3) . ? Zn4 O1 2.207(3) . ? Zn5 N6 1.986(12) . ? Zn5 O10 1.988(4) . ? Zn5 N4 2.085(6) . ? Zn5 N7 2.185(13) . ? Zn5 N7A 2.23(2) . ? Zn5 N5 2.246(5) . ? Zn5 N6A 2.295(15) . ? P1 O2 1.529(3) . ? P1 O3 1.531(3) . ? P1 O1 1.539(3) . ? P1 C1 1.829(4) . ? P2 O8 1.529(3) . ? P2 O7 1.529(3) . ? P2 O6 1.544(3) . ? P2 C15 1.835(4) . ? P3 O13 1.527(3) . ? P3 O12 1.527(3) . ? P3 O11 1.545(3) . ? P3 C29 1.828(4) . ? O2 Zn2 1.974(3) 3_566 ? O3 Zn3 1.977(3) 3_566 ? O4 C3 1.257(6) . ? O5 C3 1.263(6) . ? O7 Zn3 1.979(3) 3_566 ? O9 C17 1.256(5) . ? O10 C17 1.269(5) . ? O14 C31 1.277(6) . ? O15 C31 1.245(6) . ? N1 C2 1.491(5) . ? N1 C1 1.500(5) . ? N1 C4 1.512(5) . ? N2 C16 1.480(5) . ? N2 C15 1.493(5) . ? N2 C18 1.521(5) . ? N3 C32A 1.479(8) . ? N3 C30 1.489(6) . ? N3 C29 1.496(6) . ? N3 C32 1.523(7) . ? C1 H1 0.9700 . ? C1 H2 0.9700 . ? C2 C3 1.554(7) . ? C2 H3 0.9700 . ? C2 H4 0.9700 . ? C4 C5 1.527(6) . ? C4 H5 0.9700 . ? C4 H6 0.9700 . ? C5 C6 1.384(7) . ? C5 C14 1.437(6) . ? C6 C7 1.420(7) . ? C6 H7 0.9300 . ? C7 C8 1.353(9) . ? C7 H8 0.9300 . ? C8 C9 1.426(8) . ? C8 H9 0.9300 . ? C9 C10 1.394(8) . ? C9 C14 1.453(6) . ? C10 C11 1.383(9) . ? C10 H10 0.9300 . ? C11 C12 1.405(8) . ? C11 H11 0.9300 . ? C12 C13 1.374(7) . ? C12 H12 0.9300 . ? C13 C14 1.421(7) . ? C13 H13 0.9300 . ? C15 H14 0.9700 . ? C15 H15 0.9700 . ? C16 C17 1.519(6) . ? C16 H16 0.9700 . ? C16 H17 0.9700 . ? C18 C19 1.523(6) . ? C18 H18 0.9700 . ? C18 H19 0.9700 . ? C19 C20 1.389(7) . ? C19 C28 1.448(6) . ? C20 C21 1.416(8) . ? C20 H20 0.9300 . ? C21 C22 1.371(9) . ? C21 H21 0.9300 . ? C22 C23 1.407(8) . ? C22 H22 0.9300 . ? C23 C28 1.431(6) . ? C23 C24 1.432(8) . ? C24 C25 1.355(10) . ? C24 H23 0.9300 . ? C25 C26 1.411(9) . ? C25 H24 0.9300 . ? C26 C27 1.371(7) . ? C26 H25 0.9300 . ? C27 C28 1.431(7) . ? C27 H26 0.9300 . ? C29 H27 0.9700 . ? C29 H28 0.9700 . ? C30 C31 1.521(8) . ? C30 H29 0.9700 . ? C30 H30 0.9700 . ? C32 C33 1.552(7) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.3900 . ? C33 C42 1.3900 . ? C34 C35 1.3900 . ? C34 H34A 0.9300 . ? C35 C36 1.3900 . ? C35 H35A 0.9300 . ? C36 C37 1.3900 . ? C36 H36A 0.9300 . ? C37 C42 1.3900 . ? C37 C38 1.396(8) . ? C42 C41 1.410(8) . ? C38 C39 1.370(9) . ? C38 H38A 0.9300 . ? C39 C40 1.375(9) . ? C39 H39A 0.9300 . ? C40 C41 1.386(8) . ? C40 H40A 0.9300 . ? C41 H41A 0.9300 . ? C32A C33A 1.525(8) . ? C32A H32C 0.9700 . ? C32A H32D 0.9700 . ? C33A C34A 1.3900 . ? C33A C42A 1.3900 . ? C34A C35A 1.3900 . ? C34A H34B 0.9300 . ? C35A C36A 1.3900 . ? C35A H35B 0.9300 . ? C36A C37A 1.3900 . ? C36A H36B 0.9300 . ? C37A C38A 1.385(9) . ? C37A C42A 1.3900 . ? C42A C41A 1.401(9) . ? C38A C39A 1.372(9) . ? C38A H38B 0.9300 . ? C39A C40A 1.378(9) . ? C39A H39B 0.9300 . ? C40A C41A 1.384(9) . ? C40A H40B 0.9300 . ? C41A H41B 0.9300 . ? N4 C43 1.501(7) . ? N4 H4A 0.9000 . ? N4 H4B 0.9000 . ? C43 C44 1.503(7) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 N5 1.451(6) . ? C44 H44A 0.9602 . ? C44 H44B 0.9599 . ? N5 C45 1.468(9) . ? N5 H5A 0.9100 . ? C45 C46 1.527(10) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 N6 1.461(9) . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? N6 C47 1.465(10) . ? N6 H6A 0.9100 . ? C47 C48 1.525(10) . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C48 N7 1.475(10) . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? N7 H7A 0.9000 . ? N7 H7B 0.9000 . ? C45A C46A 1.525(10) . ? C45A H45C 0.9700 . ? C45A H45D 0.9700 . ? C46A N6A 1.489(14) . ? C46A H46C 0.9700 . ? C46A H46D 0.9700 . ? N6A C47A 1.449(14) . ? N6A H6AA 0.9100 . ? C47A C48A 1.527(10) . ? C47A H47C 0.9700 . ? C47A H47D 0.9700 . ? C48A N7A 1.470(17) . ? C48A H48C 0.9700 . ? C48A H48D 0.9700 . ? N7A H7C 0.9000 . ? N7A H7D 0.9000 . ? 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 Zn1 O1 180.000(1) 3_566 . ? O1 Zn1 O6 91.70(10) 3_566 . ? O1 Zn1 O6 88.30(10) . . ? O1 Zn1 O6 88.30(10) 3_566 3_566 ? O1 Zn1 O6 91.70(10) . 3_566 ? O6 Zn1 O6 180.0 . 3_566 ? O1 Zn1 O11 89.28(10) 3_566 . ? O1 Zn1 O11 90.72(10) . . ? O6 Zn1 O11 88.49(10) . . ? O6 Zn1 O11 91.51(10) 3_566 . ? O1 Zn1 O11 90.72(10) 3_566 3_566 ? O1 Zn1 O11 89.28(10) . 3_566 ? O6 Zn1 O11 91.51(10) . 3_566 ? O6 Zn1 O11 88.49(10) 3_566 3_566 ? O11 Zn1 O11 180.000(1) . 3_566 ? O12 Zn2 O2 121.14(13) . 3_566 ? O12 Zn2 O9 97.82(12) . . ? O2 Zn2 O9 88.86(12) 3_566 . ? O12 Zn2 N2 110.11(14) . . ? O2 Zn2 N2 128.48(13) 3_566 . ? O9 Zn2 N2 78.95(12) . . ? O12 Zn2 O6 96.09(11) . . ? O2 Zn2 O6 92.91(11) 3_566 . ? O9 Zn2 O6 162.56(11) . . ? N2 Zn2 O6 86.43(12) . . ? O3 Zn3 O7 117.27(13) 3_566 3_566 ? O3 Zn3 O14 97.98(13) 3_566 . ? O7 Zn3 O14 89.17(13) 3_566 . ? O3 Zn3 O11 97.64(11) 3_566 . ? O7 Zn3 O11 94.62(11) 3_566 . ? O14 Zn3 O11 160.07(12) . . ? O3 Zn3 N3 112.56(12) 3_566 . ? O7 Zn3 N3 129.74(13) 3_566 . ? O14 Zn3 N3 77.78(14) . . ? O11 Zn3 N3 84.83(12) . . ? O8 Zn4 O13 121.50(12) . . ? O8 Zn4 O4 98.11(14) . . ? O13 Zn4 O4 94.66(13) . . ? O8 Zn4 N1 115.13(12) . . ? O13 Zn4 N1 123.36(12) . . ? O4 Zn4 N1 78.24(13) . . ? O8 Zn4 O1 94.63(11) . . ? O13 Zn4 O1 89.53(11) . . ? O4 Zn4 O1 161.92(12) . . ? N1 Zn4 O1 84.76(11) . . ? N6 Zn5 O10 128.6(4) . . ? N6 Zn5 N4 120.0(4) . . ? O10 Zn5 N4 111.4(2) . . ? N6 Zn5 N7 83.3(5) . . ? O10 Zn5 N7 85.1(4) . . ? N4 Zn5 N7 104.5(4) . . ? N6 Zn5 N7A 62.6(6) . . ? O10 Zn5 N7A 98.2(5) . . ? N4 Zn5 N7A 113.8(5) . . ? N7 Zn5 N7A 20.7(4) . . ? N6 Zn5 N5 86.6(4) . . ? O10 Zn5 N5 101.52(17) . . ? N4 Zn5 N5 80.40(19) . . ? N7 Zn5 N5 169.9(4) . . ? N7A Zn5 N5 149.3(5) . . ? N6 Zn5 N6A 19.4(4) . . ? O10 Zn5 N6A 114.6(3) . . ? N4 Zn5 N6A 131.1(3) . . ? N7 Zn5 N6A 95.0(5) . . ? N7A Zn5 N6A 75.1(6) . . ? N5 Zn5 N6A 75.4(3) . . ? O2 P1 O3 112.89(17) . . ? O2 P1 O1 114.34(16) . . ? O3 P1 O1 111.39(15) . . ? O2 P1 C1 104.39(17) . . ? O3 P1 C1 110.36(17) . . ? O1 P1 C1 102.69(17) . . ? O8 P2 O7 112.52(18) . . ? O8 P2 O6 112.29(16) . . ? O7 P2 O6 113.30(17) . . ? O8 P2 C15 108.86(19) . . ? O7 P2 C15 106.05(18) . . ? O6 P2 C15 103.09(17) . . ? O13 P3 O12 112.88(18) . . ? O13 P3 O11 113.34(15) . . ? O12 P3 O11 111.49(16) . . ? O13 P3 C29 106.67(18) . . ? O12 P3 C29 107.41(19) . . ? O11 P3 C29 104.38(18) . . ? P1 O1 Zn1 126.48(16) . . ? P1 O1 Zn4 112.67(15) . . ? Zn1 O1 Zn4 118.44(12) . . ? P1 O2 Zn2 129.24(17) . 3_566 ? P1 O3 Zn3 122.77(17) . 3_566 ? C3 O4 Zn4 113.9(3) . . ? P2 O6 Zn1 127.60(15) . . ? P2 O6 Zn2 113.33(15) . . ? Zn1 O6 Zn2 116.64(12) . . ? P2 O7 Zn3 127.20(18) . 3_566 ? P2 O8 Zn4 125.17(17) . . ? C17 O9 Zn2 110.3(3) . . ? C17 O10 Zn5 120.3(3) . . ? P3 O11 Zn3 116.00(14) . . ? P3 O11 Zn1 126.28(15) . . ? Zn3 O11 Zn1 116.00(12) . . ? P3 O12 Zn2 124.12(17) . . ? P3 O13 Zn4 127.43(17) . . ? C31 O14 Zn3 115.5(3) . . ? C2 N1 C1 112.6(3) . . ? C2 N1 C4 112.0(3) . . ? C1 N1 C4 111.8(3) . . ? C2 N1 Zn4 102.1(2) . . ? C1 N1 Zn4 109.5(2) . . ? C4 N1 Zn4 108.3(2) . . ? C16 N2 C15 112.5(3) . . ? C16 N2 C18 112.1(3) . . ? C15 N2 C18 112.7(3) . . ? C16 N2 Zn2 104.7(2) . . ? C15 N2 Zn2 109.1(2) . . ? C18 N2 Zn2 105.1(2) . . ? C32A N3 C30 104.5(6) . . ? C32A N3 C29 123.3(6) . . ? C30 N3 C29 112.5(3) . . ? C32A N3 C32 17.9(6) . . ? C30 N3 C32 117.3(5) . . ? C29 N3 C32 105.6(4) . . ? C32A N3 Zn3 97.8(4) . . ? C30 N3 Zn3 105.6(3) . . ? C29 N3 Zn3 111.1(2) . . ? C32 N3 Zn3 104.6(4) . . ? N1 C1 P1 110.2(2) . . ? N1 C1 H1 109.6 . . ? P1 C1 H1 109.6 . . ? N1 C1 H2 109.6 . . ? P1 C1 H2 109.6 . . ? H1 C1 H2 108.1 . . ? N1 C2 C3 109.4(3) . . ? N1 C2 H3 109.8 . . ? C3 C2 H3 109.8 . . ? N1 C2 H4 109.8 . . ? C3 C2 H4 109.8 . . ? H3 C2 H4 108.2 . . ? O4 C3 O5 125.7(5) . . ? O4 C3 C2 117.0(4) . . ? O5 C3 C2 117.3(4) . . ? N1 C4 C5 116.3(3) . . ? N1 C4 H5 108.2 . . ? C5 C4 H5 108.2 . . ? N1 C4 H6 108.2 . . ? C5 C4 H6 108.2 . . ? H5 C4 H6 107.4 . . ? C6 C5 C14 119.1(4) . . ? C6 C5 C4 118.5(4) . . ? C14 C5 C4 122.4(4) . . ? C5 C6 C7 121.8(5) . . ? C5 C6 H7 119.1 . . ? C7 C6 H7 119.1 . . ? C8 C7 C6 120.2(5) . . ? C8 C7 H8 119.9 . . ? C6 C7 H8 119.9 . . ? C7 C8 C9 121.3(5) . . ? C7 C8 H9 119.4 . . ? C9 C8 H9 119.4 . . ? C10 C9 C8 121.8(5) . . ? C10 C9 C14 119.3(5) . . ? C8 C9 C14 118.9(5) . . ? C11 C10 C9 121.8(5) . . ? C11 C10 H10 119.1 . . ? C9 C10 H10 119.1 . . ? C10 C11 C12 119.3(5) . . ? C10 C11 H11 120.4 . . ? C12 C11 H11 120.4 . . ? C13 C12 C11 120.9(5) . . ? C13 C12 H12 119.5 . . ? C11 C12 H12 119.5 . . ? C12 C13 C14 121.3(5) . . ? C12 C13 H13 119.3 . . ? C14 C13 H13 119.3 . . ? C13 C14 C5 124.1(4) . . ? C13 C14 C9 117.3(4) . . ? C5 C14 C9 118.6(4) . . ? N2 C15 P2 110.5(3) . . ? N2 C15 H14 109.6 . . ? P2 C15 H14 109.6 . . ? N2 C15 H15 109.6 . . ? P2 C15 H15 109.6 . . ? H14 C15 H15 108.1 . . ? N2 C16 C17 111.5(3) . . ? N2 C16 H16 109.3 . . ? C17 C16 H16 109.3 . . ? N2 C16 H17 109.3 . . ? C17 C16 H17 109.3 . . ? H16 C16 H17 108.0 . . ? O9 C17 O10 124.9(4) . . ? O9 C17 C16 119.8(4) . . ? O10 C17 C16 115.3(4) . . ? N2 C18 C19 115.6(3) . . ? N2 C18 H18 108.4 . . ? C19 C18 H18 108.4 . . ? N2 C18 H19 108.4 . . ? C19 C18 H19 108.4 . . ? H18 C18 H19 107.4 . . ? C20 C19 C28 118.3(4) . . ? C20 C19 C18 120.1(4) . . ? C28 C19 C18 121.4(4) . . ? C19 C20 C21 121.9(5) . . ? C19 C20 H20 119.0 . . ? C21 C20 H20 119.0 . . ? C22 C21 C20 119.9(5) . . ? C22 C21 H21 120.1 . . ? C20 C21 H21 120.1 . . ? C21 C22 C23 120.9(5) . . ? C21 C22 H22 119.5 . . ? C23 C22 H22 119.5 . . ? C22 C23 C28 120.0(5) . . ? C22 C23 C24 121.4(5) . . ? C28 C23 C24 118.7(5) . . ? C25 C24 C23 121.3(5) . . ? C25 C24 H23 119.3 . . ? C23 C24 H23 119.3 . . ? C24 C25 C26 120.9(5) . . ? C24 C25 H24 119.5 . . ? C26 C25 H24 119.5 . . ? C27 C26 C25 119.3(6) . . ? C27 C26 H25 120.3 . . ? C25 C26 H25 120.3 . . ? C26 C27 C28 122.2(5) . . ? C26 C27 H26 118.9 . . ? C28 C27 H26 118.9 . . ? C27 C28 C23 117.5(4) . . ? C27 C28 C19 123.6(4) . . ? C23 C28 C19 118.9(5) . . ? N3 C29 P3 110.1(3) . . ? N3 C29 H27 109.6 . . ? P3 C29 H27 109.6 . . ? N3 C29 H28 109.6 . . ? P3 C29 H28 109.6 . . ? H27 C29 H28 108.1 . . ? N3 C30 C31 111.2(4) . . ? N3 C30 H29 109.4 . . ? C31 C30 H29 109.4 . . ? N3 C30 H30 109.4 . . ? C31 C30 H30 109.4 . . ? H29 C30 H30 108.0 . . ? O15 C31 O14 124.7(6) . . ? O15 C31 C30 118.1(5) . . ? O14 C31 C30 117.2(4) . . ? N3 C32 C33 126.2(6) . . ? N3 C32 H32A 105.8 . . ? C33 C32 H32A 105.8 . . ? N3 C32 H32B 105.8 . . ? C33 C32 H32B 105.8 . . ? H32A C32 H32B 106.2 . . ? C34 C33 C42 120.0 . . ? C34 C33 C32 116.7(5) . . ? C42 C33 C32 123.1(5) . . ? C35 C34 C33 120.0 . . ? C35 C34 H34A 120.0 . . ? C33 C34 H34A 120.0 . . ? C34 C35 C36 120.0 . . ? C34 C35 H35A 120.0 . . ? C36 C35 H35A 120.0 . . ? C37 C36 C35 120.0 . . ? C37 C36 H36A 120.0 . . ? C35 C36 H36A 120.0 . . ? C42 C37 C36 120.0 . . ? C42 C37 C38 121.0(6) . . ? C36 C37 C38 119.0(6) . . ? C37 C42 C33 120.0 . . ? C37 C42 C41 116.8(6) . . ? C33 C42 C41 123.2(6) . . ? C39 C38 C37 122.0(8) . . ? C39 C38 H38A 119.0 . . ? C37 C38 H38A 119.0 . . ? C38 C39 C40 117.3(8) . . ? C38 C39 H39A 121.3 . . ? C40 C39 H39A 121.3 . . ? C39 C40 C41 122.3(9) . . ? C39 C40 H40A 118.8 . . ? C41 C40 H40A 118.8 . . ? C40 C41 C42 120.5(9) . . ? C40 C41 H41A 119.8 . . ? C42 C41 H41A 119.8 . . ? N3 C32A C33A 119.2(6) . . ? N3 C32A H32C 107.5 . . ? C33A C32A H32C 107.5 . . ? N3 C32A H32D 107.5 . . ? C33A C32A H32D 107.5 . . ? H32C C32A H32D 107.0 . . ? C34A C33A C42A 120.0 . . ? C34A C33A C32A 115.2(7) . . ? C42A C33A C32A 124.6(7) . . ? C33A C34A C35A 120.0 . . ? C33A C34A H34B 120.0 . . ? C35A C34A H34B 120.0 . . ? C36A C35A C34A 120.0 . . ? C36A C35A H35B 120.0 . . ? C34A C35A H35B 120.0 . . ? C35A C36A C37A 120.0 . . ? C35A C36A H36B 120.0 . . ? C37A C36A H36B 120.0 . . ? C38A C37A C42A 121.7(8) . . ? C38A C37A C36A 118.3(8) . . ? C42A C37A C36A 120.0 . . ? C37A C42A C33A 120.0 . . ? C37A C42A C41A 116.4(7) . . ? C33A C42A C41A 123.5(7) . . ? C39A C38A C37A 120.8(10) . . ? C39A C38A H38B 119.6 . . ? C37A C38A H38B 119.6 . . ? C38A C39A C40A 119.0(9) . . ? C38A C39A H39B 120.5 . . ? C40A C39A H39B 120.5 . . ? C39A C40A C41A 120.3(10) . . ? C39A C40A H40B 119.8 . . ? C41A C40A H40B 119.8 . . ? C40A C41A C42A 121.7(10) . . ? C40A C41A H41B 119.1 . . ? C42A C41A H41B 119.1 . . ? C43 N4 Zn5 107.9(4) . . ? C43 N4 H4A 110.1 . . ? Zn5 N4 H4A 110.1 . . ? C43 N4 H4B 110.1 . . ? Zn5 N4 H4B 110.1 . . ? H4A N4 H4B 108.4 . . ? N4 C43 C44 108.1(6) . . ? N4 C43 H43A 110.1 . . ? C44 C43 H43A 110.1 . . ? N4 C43 H43B 110.1 . . ? C44 C43 H43B 110.1 . . ? H43A C43 H43B 108.4 . . ? N5 C44 C43 112.7(6) . . ? N5 C44 H44A 108.6 . . ? C43 C44 H44A 109.0 . . ? N5 C44 H44B 109.5 . . ? C43 C44 H44B 109.1 . . ? H44A C44 H44B 107.9 . . ? C44 N5 C45 111.9(9) . . ? C44 N5 Zn5 107.6(4) . . ? C45 N5 Zn5 101.8(8) . . ? C44 N5 H5A 111.7 . . ? C45 N5 H5A 111.7 . . ? Zn5 N5 H5A 111.7 . . ? N5 C45 C46 111.7(10) . . ? N5 C45 H45A 109.3 . . ? C46 C45 H45A 109.3 . . ? N5 C45 H45B 109.3 . . ? C46 C45 H45B 109.3 . . ? H45A C45 H45B 107.9 . . ? N6 C46 C45 113.0(12) . . ? N6 C46 H46A 109.0 . . ? C45 C46 H46A 109.0 . . ? N6 C46 H46B 109.0 . . ? C45 C46 H46B 109.0 . . ? H46A C46 H46B 107.8 . . ? C46 N6 C47 116.8(14) . . ? C46 N6 Zn5 104.5(9) . . ? C47 N6 Zn5 103.9(9) . . ? C46 N6 H6A 110.4 . . ? C47 N6 H6A 110.4 . . ? Zn5 N6 H6A 110.4 . . ? N6 C47 C48 111.4(13) . . ? N6 C47 H47A 109.4 . . ? C48 C47 H47A 109.4 . . ? N6 C47 H47B 109.4 . . ? C48 C47 H47B 109.4 . . ? H47A C47 H47B 108.0 . . ? N7 C48 C47 108.5(13) . . ? N7 C48 H48A 110.0 . . ? C47 C48 H48A 110.0 . . ? N7 C48 H48B 110.0 . . ? C47 C48 H48B 110.0 . . ? H48A C48 H48B 108.4 . . ? C48 N7 Zn5 107.2(10) . . ? C48 N7 H7A 110.3 . . ? Zn5 N7 H7A 110.3 . . ? C48 N7 H7B 110.3 . . ? Zn5 N7 H7B 110.3 . . ? H7A N7 H7B 108.5 . . ? C46A C45A H45C 110.6 . . ? C46A C45A H45D 110.6 . . ? H45C C45A H45D 108.8 . . ? N6A C46A C45A 111.8(16) . . ? N6A C46A H46C 109.3 . . ? C45A C46A H46C 109.3 . . ? N6A C46A H46D 109.3 . . ? C45A C46A H46D 109.3 . . ? H46C C46A H46D 107.9 . . ? C47A N6A C46A 114.8(12) . . ? C47A N6A Zn5 110.7(10) . . ? C46A N6A Zn5 104.3(10) . . ? C47A N6A H6AA 109.0 . . ? C46A N6A H6AA 109.0 . . ? Zn5 N6A H6AA 109.0 . . ? N6A C47A C48A 108.5(13) . . ? N6A C47A H47C 110.0 . . ? C48A C47A H47C 110.0 . . ? N6A C47A H47D 110.0 . . ? C48A C47A H47D 110.0 . . ? H47C C47A H47D 108.4 . . ? N7A C48A C47A 109.4(15) . . ? N7A C48A H48C 109.8 . . ? C47A C48A H48C 109.8 . . ? N7A C48A H48D 109.8 . . ? C47A C48A H48D 109.8 . . ? H48C C48A H48D 108.2 . . ? C48A N7A Zn5 114.0(11) . . ? C48A N7A H7C 108.8 . . ? Zn5 N7A H7C 108.8 . . ? C48A N7A H7D 108.8 . . ? Zn5 N7A H7D 108.8 . . ? H7C N7A H7D 107.7 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.37 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.824 _refine_diff_density_min -1.796 _refine_diff_density_rms 0.111 _database_code_depnum_ccdc_archive 'CCDC 925303' ####################################################################### # # 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_f1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C96 H150 N14 O48 P6 Zn9' _chemical_formula_weight 3042.45 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' P P 0.1023 0.0942 '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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.827(6) _cell_length_b 22.632(8) _cell_length_c 18.636(6) _cell_angle_alpha 90.00 _cell_angle_beta 106.024(6) _cell_angle_gamma 90.00 _cell_volume 6416(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 17932 _cell_measurement_theta_min 2.6045 _cell_measurement_theta_max 27.5515 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.3000 _exptl_crystal_size_mid 0.2000 _exptl_crystal_size_min 0.2000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.575 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3136 _exptl_absorpt_coefficient_mu 1.815 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7492 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2008)' _exptl_special_details ; The single crystal has been irradiated under a UV lamp at 254 and 365 nm for 24 hours. ; _diffrn_ambient_temperature 293(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 'Saturn724+ (2x2 bin mode)' _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 50612 _diffrn_reflns_av_R_equivalents 0.0641 _diffrn_reflns_av_sigmaI/netI 0.0636 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 27.45 _reflns_number_total 14561 _reflns_number_gt 12053 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _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. Due to the moderate diffraction intensity, as well as abnormal phosphonate ligand and triethylenetetramine, so hydrogen atoms were generated geometrically. One phosphonate ligand (N3C32C33C34C35C36C37C38C39C40C41C42) and one triethylenetetramine(N4C43C44N5C45C46N6C47C48N7),as well as four free water molecules (O15,O19,O20,O23) are abnormal, so the distance/angle and isotropic are restrained. The restraints used in the refinement are listed as follows: DFIX 3.0 ZN5 C47 exyz n5 n5a eadp n5 n5a eadp c32 c32a dfix 1.46 0.01 n4 c43 n5 c44 n5 c45 n6 c46 n6 c47 n7 c48 dfix 1.52 0.01 c43 c44 c45 c46 c47 c48 c45a c46a c47a c48a dfix 1.46 n5a c45a n6a c46a n6a c47a n7a c48a REM DFIX 2.47 N5 C46 C45 N6 C46 C47 N6 C48 C47 N7 SIMU 0.02 0.04 N4 > C48A dfix 1.51 0.01 c32 c33 n3 c32 dfix 1.38 0.01 c37 c38 c38 c39 c39 c40 c40 c41 c41 c42 dfix 2.39 c37 c39 c38 c40 c39 c41 c40 c42 c41 c37 flat 0.01 c35 c37 c38 c39 c40 c41 c42 c32 dfix 1.51 0.01 c32a c33a n3 c32a dfix 1.38 0.01 c37a c38a c38a c39a c39a c40a c40a c41a c41a c42a dfix 2.39 c37a c39a c38a c40a c39a c41a c40a c42a c41a c37a flat 0.01 c35a c37a c38a c39a c40a c41a c42a c32a isor 0.01 o15 o19 o20 o23 c32a c48 n7a ; _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^)+(0.0731P)^2^+10.8100P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14561 _refine_ls_number_parameters 896 _refine_ls_number_restraints 248 _refine_ls_R_factor_all 0.1048 _refine_ls_R_factor_gt 0.0859 _refine_ls_wR_factor_ref 0.2085 _refine_ls_wR_factor_gt 0.1974 _refine_ls_goodness_of_fit_ref 1.204 _refine_ls_restrained_S_all 1.211 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.0000 0.5000 0.5000 0.0373(2) Uani 1 2 d S . . Zn2 Zn 0.21595(4) 0.55871(3) 0.58943(4) 0.04451(18) Uani 1 1 d . . . Zn3 Zn 0.05736(5) 0.58588(3) 0.35594(4) 0.04600(18) Uani 1 1 d . . . Zn4 Zn 0.15070(5) 0.37163(3) 0.53040(4) 0.04707(19) Uani 1 1 d . . . Zn5 Zn 0.41543(8) 0.73391(5) 0.66747(7) 0.0976(4) Uani 1 1 d D . . P1 P -0.05494(10) 0.36094(6) 0.49293(9) 0.0416(3) Uani 1 1 d . . . P2 P 0.13629(10) 0.45525(7) 0.65761(8) 0.0437(3) Uani 1 1 d . . . P3 P 0.17979(10) 0.48664(6) 0.44523(9) 0.0426(3) Uani 1 1 d . . . O1 O 0.0154(2) 0.40797(15) 0.4954(2) 0.0418(9) Uani 1 1 d . . . O2 O -0.1402(3) 0.37107(17) 0.4324(3) 0.0543(11) Uani 1 1 d . . . O3 O -0.0691(3) 0.35126(17) 0.5696(2) 0.0498(10) Uani 1 1 d . . . O4 O 0.2560(3) 0.3148(2) 0.5426(3) 0.0682(13) Uani 1 1 d . . . O5 O 0.2927(4) 0.2323(3) 0.4943(4) 0.097(2) Uani 1 1 d . . . O6 O 0.1100(3) 0.50176(16) 0.5951(2) 0.0432(9) Uani 1 1 d . . . O7 O 0.0634(3) 0.44195(19) 0.6933(2) 0.0541(10) Uani 1 1 d . . . O8 O 0.1749(3) 0.39972(18) 0.6332(2) 0.0540(10) Uani 1 1 d . . . O9 O 0.3273(3) 0.6147(2) 0.6212(3) 0.0571(11) Uani 1 1 d . B . O10 O 0.3969(4) 0.6640(2) 0.7234(3) 0.0860(18) Uani 1 1 d . B . O11 O 0.0874(2) 0.51360(16) 0.4318(2) 0.0421(8) Uani 1 1 d . . . O12 O 0.2464(3) 0.5171(2) 0.5097(2) 0.0566(11) Uani 1 1 d . . . O13 O 0.1804(3) 0.41977(17) 0.4526(2) 0.0525(10) Uani 1 1 d . . . O14 O 0.0541(4) 0.6382(2) 0.2635(3) 0.0700(13) Uani 1 1 d . A . O15 O 0.0929(6) 0.6382(3) 0.1583(4) 0.119(2) Uani 1 1 d U A . O16 O 0.7837(8) 0.2196(6) 0.2190(6) 0.210(5) Uani 1 1 d . . . O17 O 0.8250(8) 0.3829(4) 0.9485(5) 0.165(4) Uani 1 1 d . . . O18 O 0.8494(9) 0.3300(7) 0.2766(7) 0.255(7) Uani 1 1 d . . . O19 O 1.1561(12) 0.3505(7) 0.3235(9) 0.264(7) Uani 1 1 d U . . O20 O 0.9612(10) 0.4904(7) 0.1857(8) 0.228(6) Uani 1 1 d U . . O21 O 0.5558(12) 0.8101(9) 0.4031(11) 0.357(12) Uani 1 1 d . . . O22 O 0.9881(15) 0.4017(8) 0.3081(9) 0.311(10) Uani 1 1 d . . . O23 O -0.170(3) 0.649(2) -0.172(2) 0.65(3) Uiso 1 1 d . . . O24 O 0.9003(19) 0.4813(14) 1.0192(17) 0.467(16) Uiso 1 1 d . . . N1 N 0.0856(3) 0.2866(2) 0.5099(3) 0.0458(11) Uani 1 1 d . . . N2 N 0.2861(3) 0.5224(2) 0.6954(3) 0.0478(11) Uani 1 1 d . . . N3 N 0.1821(4) 0.5640(2) 0.3349(3) 0.0526(13) Uani 1 1 d D . . C1 C -0.0079(4) 0.2950(2) 0.4640(3) 0.0458(13) Uani 1 1 d . . . H1 H -0.0425 0.2608 0.4698 0.055 Uiso 1 1 calc R . . H2 H -0.0098 0.2983 0.4117 0.055 Uiso 1 1 calc R . . C2 C 0.1401(4) 0.2551(3) 0.4689(3) 0.0505(14) Uani 1 1 d . . . H3 H 0.1237 0.2677 0.4172 0.061 Uiso 1 1 calc R . . H4 H 0.1297 0.2129 0.4700 0.061 Uiso 1 1 calc R . . C3 C 0.2374(5) 0.2681(3) 0.5046(4) 0.0630(18) Uani 1 1 d . . . C4 C 0.0907(4) 0.2586(3) 0.5843(3) 0.0489(14) Uani 1 1 d . . . H5 H 0.0633 0.2850 0.6121 0.059 Uiso 1 1 calc R . . H6 H 0.1522 0.2551 0.6119 0.059 Uiso 1 1 calc R . . C5 C 0.0480(4) 0.1978(3) 0.5817(4) 0.0556(16) Uani 1 1 d . . . C6 C -0.0399(5) 0.1960(4) 0.5829(5) 0.076(2) Uani 1 1 d . . . H7 H -0.0690 0.2311 0.5863 0.091 Uiso 1 1 calc R . . C7 C -0.0853(6) 0.1419(5) 0.5789(5) 0.096(3) Uani 1 1 d . . . H8 H -0.1436 0.1418 0.5800 0.115 Uiso 1 1 calc R . . C8 C -0.0460(6) 0.0920(4) 0.5736(5) 0.092(3) Uani 1 1 d . . . H9 H -0.0776 0.0569 0.5699 0.110 Uiso 1 1 calc R . . C9 C 0.0433(6) 0.0898(3) 0.5732(4) 0.072(2) Uani 1 1 d . . . C10 C 0.0848(8) 0.0364(4) 0.5701(5) 0.091(3) Uani 1 1 d . . . H10 H 0.0527 0.0015 0.5657 0.110 Uiso 1 1 calc R . . C11 C 0.1715(9) 0.0342(4) 0.5735(5) 0.099(3) Uani 1 1 d . . . H11 H 0.1980 -0.0021 0.5706 0.119 Uiso 1 1 calc R . . C12 C 0.2224(7) 0.0870(4) 0.5813(5) 0.084(2) Uani 1 1 d . . . H12 H 0.2821 0.0855 0.5846 0.101 Uiso 1 1 calc R . . C13 C 0.1819(5) 0.1399(3) 0.5838(4) 0.0657(19) Uani 1 1 d . . . H13 H 0.2148 0.1745 0.5887 0.079 Uiso 1 1 calc R . . C14 C 0.0924(5) 0.1437(3) 0.5793(4) 0.0580(16) Uani 1 1 d . . . C15 C 0.2224(4) 0.4925(3) 0.7294(3) 0.0463(13) Uani 1 1 d . . . H14 H 0.1959 0.5216 0.7548 0.056 Uiso 1 1 calc R . . H15 H 0.2532 0.4639 0.7660 0.056 Uiso 1 1 calc R . . C16 C 0.3298(4) 0.5735(3) 0.7390(4) 0.0516(14) Uani 1 1 d . B . H16 H 0.3828 0.5603 0.7755 0.062 Uiso 1 1 calc R . . H17 H 0.2912 0.5904 0.7659 0.062 Uiso 1 1 calc R . . C17 C 0.3536(4) 0.6205(3) 0.6905(4) 0.0575(16) Uani 1 1 d . . . C18 C 0.3521(4) 0.4795(3) 0.6785(4) 0.0549(15) Uani 1 1 d . . . H18 H 0.3200 0.4458 0.6524 0.066 Uiso 1 1 calc R . . H19 H 0.3804 0.4988 0.6448 0.066 Uiso 1 1 calc R . . C19 C 0.4229(5) 0.4570(3) 0.7453(4) 0.0614(17) Uani 1 1 d . . . C20 C 0.4060(6) 0.4103(3) 0.7862(5) 0.080(2) Uani 1 1 d . . . H20 H 0.3507 0.3928 0.7719 0.096 Uiso 1 1 calc R . . C21 C 0.4695(8) 0.3878(4) 0.8496(6) 0.104(3) Uani 1 1 d . . . H21 H 0.4551 0.3571 0.8773 0.125 Uiso 1 1 calc R . . C22 C 0.5515(8) 0.4113(4) 0.8696(6) 0.095(3) Uani 1 1 d . . . H22 H 0.5930 0.3969 0.9115 0.114 Uiso 1 1 calc R . . C23 C 0.5743(5) 0.4566(4) 0.8287(5) 0.077(2) Uani 1 1 d . . . C24 C 0.6602(6) 0.4811(5) 0.8470(6) 0.103(4) Uani 1 1 d . . . H23 H 0.7030 0.4655 0.8872 0.124 Uiso 1 1 calc R . . C25 C 0.6823(6) 0.5267(6) 0.8076(7) 0.108(4) Uani 1 1 d . . . H24 H 0.7389 0.5422 0.8221 0.130 Uiso 1 1 calc R . . C26 C 0.6214(6) 0.5495(4) 0.7470(6) 0.093(3) Uani 1 1 d . . . H25 H 0.6371 0.5799 0.7196 0.111 Uiso 1 1 calc R . . C27 C 0.5369(5) 0.5277(4) 0.7266(5) 0.074(2) Uani 1 1 d . . . H26 H 0.4963 0.5445 0.6859 0.089 Uiso 1 1 calc R . . C28 C 0.5093(4) 0.4810(3) 0.7649(4) 0.0625(18) Uani 1 1 d . . . C29 C 0.2103(4) 0.5039(3) 0.3605(4) 0.0492(14) Uani 1 1 d . A . H27 H 0.2736 0.5007 0.3700 0.059 Uiso 1 1 calc R . . H28 H 0.1831 0.4757 0.3219 0.059 Uiso 1 1 calc R . . C30 C 0.1664(6) 0.5711(3) 0.2532(4) 0.074(2) Uani 1 1 d . A . H29 H 0.1449 0.5341 0.2285 0.089 Uiso 1 1 calc R . . H30 H 0.2213 0.5806 0.2423 0.089 Uiso 1 1 calc R . . C31 C 0.1002(7) 0.6193(4) 0.2233(5) 0.080(2) Uani 1 1 d . . . C32 C 0.2485(5) 0.6055(4) 0.3834(6) 0.050(3) Uani 0.620(10) 1 d PD A 1 H32A H 0.2446 0.5992 0.4339 0.060 Uiso 0.620(10) 1 calc PR A 1 H32B H 0.2259 0.6450 0.3695 0.060 Uiso 0.620(10) 1 calc PR A 1 C33 C 0.3471(4) 0.6088(3) 0.3897(4) 0.061(3) Uani 0.620(10) 1 d PGD A 1 C34 C 0.4022(6) 0.5750(4) 0.4457(5) 0.052(4) Uani 0.620(10) 1 d PG A 1 H34A H 0.3784 0.5504 0.4751 0.062 Uiso 0.620(10) 1 calc PR A 1 C35 C 0.4928(6) 0.5781(5) 0.4579(6) 0.100(6) Uani 0.620(10) 1 d PGD A 1 H35A H 0.5296 0.5555 0.4955 0.120 Uiso 0.620(10) 1 calc PR A 1 C36 C 0.5283(4) 0.6149(5) 0.4141(7) 0.098(8) Uani 0.620(10) 1 d PG A 1 H36A H 0.5889 0.6170 0.4223 0.118 Uiso 0.620(10) 1 calc PR A 1 C37 C 0.4732(6) 0.6487(4) 0.3580(5) 0.066(4) Uani 0.620(10) 1 d PGD A 1 C42 C 0.3826(5) 0.6456(3) 0.3458(4) 0.071(4) Uani 0.620(10) 1 d PGD A 1 C38 C 0.5114(9) 0.6844(5) 0.3150(7) 0.109(6) Uani 0.620(10) 1 d PD A 1 H38A H 0.5722 0.6848 0.3237 0.131 Uiso 0.620(10) 1 calc PR A 1 C39 C 0.4596(10) 0.7191(5) 0.2595(7) 0.136(8) Uani 0.620(10) 1 d PD A 1 H39A H 0.4846 0.7433 0.2306 0.163 Uiso 0.620(10) 1 calc PR A 1 C40 C 0.3694(10) 0.7172(5) 0.2476(7) 0.110(7) Uani 0.620(10) 1 d PD A 1 H40A H 0.3338 0.7405 0.2102 0.132 Uiso 0.620(10) 1 calc PR A 1 C41 C 0.3308(9) 0.6817(4) 0.2899(6) 0.085(5) Uani 0.620(10) 1 d PD A 1 H41A H 0.2700 0.6819 0.2812 0.102 Uiso 0.620(10) 1 calc PR A 1 C32A C 0.2296(10) 0.6191(6) 0.3663(12) 0.050(3) Uani 0.38 1 d PDU A 2 H32C H 0.2439 0.6167 0.4203 0.060 Uiso 0.380(10) 1 calc PR A 2 H32D H 0.1896 0.6521 0.3509 0.060 Uiso 0.380(10) 1 calc PR A 2 C33A C 0.3133(7) 0.6330(5) 0.3455(7) 0.062(5) Uani 0.380(10) 1 d PGD A 2 C34A C 0.3028(9) 0.6658(6) 0.2805(8) 0.071(7) Uani 0.380(10) 1 d PG A 2 H34B H 0.2467 0.6761 0.2518 0.085 Uiso 0.380(10) 1 calc PR A 2 C35A C 0.3760(12) 0.6832(7) 0.2584(8) 0.104(11) Uani 0.380(10) 1 d PGD A 2 H35B H 0.3690 0.7051 0.2149 0.125 Uiso 0.380(10) 1 calc PR A 2 C36A C 0.4598(10) 0.6678(7) 0.3012(10) 0.090(9) Uani 0.380(10) 1 d PG A 2 H36B H 0.5088 0.6794 0.2864 0.107 Uiso 0.380(10) 1 calc PR A 2 C37A C 0.4703(6) 0.6350(6) 0.3662(9) 0.106(15) Uani 0.380(10) 1 d PGD A 2 C42A C 0.3971(8) 0.6177(4) 0.3883(6) 0.064(6) Uani 0.380(10) 1 d PGD A 2 C38A C 0.5539(10) 0.6197(8) 0.4079(11) 0.083(10) Uani 0.380(10) 1 d PD A 2 H38B H 0.6023 0.6309 0.3920 0.100 Uiso 0.380(10) 1 calc PR A 2 C39A C 0.5658(11) 0.5879(8) 0.4727(11) 0.116(12) Uani 0.380(10) 1 d PD A 2 H39B H 0.6222 0.5778 0.5008 0.139 Uiso 0.380(10) 1 calc PR A 2 C40A C 0.4939(12) 0.5709(8) 0.4960(11) 0.118(15) Uani 0.380(10) 1 d PD A 2 H40B H 0.5015 0.5493 0.5397 0.142 Uiso 0.380(10) 1 calc PR A 2 C41A C 0.4107(12) 0.5863(6) 0.4540(8) 0.096(13) Uani 0.380(10) 1 d PD A 2 H41B H 0.3625 0.5753 0.4704 0.116 Uiso 0.380(10) 1 calc PR A 2 N4 N 0.3740(7) 0.8090(4) 0.7122(5) 0.125(3) Uani 1 1 d DU B . H4A H 0.3505 0.7989 0.7493 0.151 Uiso 1 1 calc R . . H4B H 0.4200 0.8331 0.7311 0.151 Uiso 1 1 calc R . . C43 C 0.3079(8) 0.8394(5) 0.6526(7) 0.143(4) Uani 1 1 d DU . . H43A H 0.3372 0.8597 0.6203 0.172 Uiso 1 1 calc R B . H43B H 0.2783 0.8689 0.6747 0.172 Uiso 1 1 calc R . . C44 C 0.2409(7) 0.7973(4) 0.6067(7) 0.129(4) Uani 1 1 d DU B . H44A H 0.2081 0.8167 0.5618 0.155 Uiso 1 1 d R . . H44B H 0.2006 0.7859 0.6343 0.155 Uiso 1 1 d R . . N5 N 0.2828(6) 0.7448(3) 0.5867(4) 0.100(3) Uani 0.467(11) 1 d PDU B 1 H5A H 0.2488 0.7119 0.5835 0.120 Uiso 0.467(11) 1 calc PR B 1 C45 C 0.3107(18) 0.7548(13) 0.5187(11) 0.115(5) Uani 0.467(11) 1 d PDU B 1 H45A H 0.3161 0.7969 0.5117 0.137 Uiso 0.467(11) 1 calc PR B 1 H45B H 0.2657 0.7398 0.4760 0.137 Uiso 0.467(11) 1 calc PR B 1 C46 C 0.3981(16) 0.7249(15) 0.5215(16) 0.120(6) Uani 0.467(11) 1 d PDU B 1 H46A H 0.3889 0.6825 0.5196 0.144 Uiso 0.467(11) 1 calc PR B 1 H46B H 0.4145 0.7360 0.4769 0.144 Uiso 0.467(11) 1 calc PR B 1 N6 N 0.4723(15) 0.7382(10) 0.5863(12) 0.120(5) Uani 0.467(11) 1 d PDU B 1 H6A H 0.4890 0.7763 0.5824 0.144 Uiso 0.467(11) 1 calc PR B 1 C47 C 0.5516(13) 0.7003(14) 0.6000(13) 0.124(6) Uani 0.467(11) 1 d PDU B 1 H47A H 0.5868 0.7094 0.5663 0.149 Uiso 0.467(11) 1 calc PR B 1 H47B H 0.5369 0.6586 0.5966 0.149 Uiso 0.467(11) 1 calc PR B 1 C48 C 0.5969(17) 0.7190(14) 0.6801(13) 0.112(6) Uani 0.467(11) 1 d PDU B 1 H48A H 0.6433 0.6905 0.6995 0.134 Uiso 0.467(11) 1 calc PR B 1 H48B H 0.6257 0.7564 0.6767 0.134 Uiso 0.467(11) 1 calc PR B 1 N7 N 0.5509(14) 0.7266(9) 0.7379(13) 0.113(6) Uani 0.467(11) 1 d PDU B 1 H7A H 0.5684 0.7596 0.7650 0.135 Uiso 0.467(11) 1 calc PR B 1 H7B H 0.5582 0.6951 0.7685 0.135 Uiso 0.467(11) 1 calc PR B 1 N5A N 0.2828(6) 0.7448(3) 0.5867(4) 0.100(3) Uani 0.53 1 d PDU B 2 H5AA H 0.2509 0.7144 0.5977 0.120 Uiso 0.533(11) 1 calc PR B 2 C45A C 0.2764(15) 0.7363(12) 0.5072(9) 0.116(5) Uani 0.533(11) 1 d PDU B 2 H45C H 0.2319 0.7620 0.4766 0.139 Uiso 0.533(11) 1 calc PR B 2 H45D H 0.2612 0.6957 0.4926 0.139 Uiso 0.533(11) 1 calc PR B 2 C46A C 0.3670(13) 0.7515(12) 0.4980(13) 0.121(6) Uani 0.533(11) 1 d PDU B 2 H46C H 0.3684 0.7422 0.4476 0.145 Uiso 0.533(11) 1 calc PR B 2 H46D H 0.3776 0.7935 0.5059 0.145 Uiso 0.533(11) 1 calc PR B 2 N6A N 0.4365(13) 0.7184(10) 0.5513(12) 0.115(5) Uani 0.533(11) 1 d PDU B 2 H6AA H 0.4276 0.6793 0.5404 0.138 Uiso 0.533(11) 1 calc PR B 2 C47A C 0.5258(13) 0.7317(11) 0.5540(12) 0.121(5) Uani 0.533(11) 1 d PDU B 2 H47C H 0.5332 0.7739 0.5489 0.145 Uiso 0.533(11) 1 calc PR B 2 H47D H 0.5424 0.7117 0.5139 0.145 Uiso 0.533(11) 1 calc PR B 2 C48A C 0.5825(16) 0.7102(12) 0.6299(12) 0.120(6) Uani 0.533(11) 1 d PDU B 2 H48C H 0.5818 0.6673 0.6302 0.144 Uiso 0.533(11) 1 calc PR B 2 H48D H 0.6427 0.7226 0.6358 0.144 Uiso 0.533(11) 1 calc PR B 2 N7A N 0.5551(15) 0.7312(11) 0.6936(12) 0.117(7) Uani 0.533(11) 1 d PDU B 2 H7C H 0.5770 0.7676 0.7063 0.140 Uiso 0.533(11) 1 calc PR B 2 H7D H 0.5763 0.7071 0.7328 0.140 Uiso 0.533(11) 1 calc PR B 2 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 0.0399(5) 0.0338(4) 0.0388(5) -0.0005(3) 0.0116(4) -0.0052(3) Zn2 0.0428(4) 0.0439(4) 0.0440(4) -0.0013(3) 0.0073(3) -0.0062(3) Zn3 0.0516(4) 0.0435(4) 0.0469(4) 0.0043(3) 0.0204(3) -0.0031(3) Zn4 0.0491(4) 0.0371(3) 0.0548(4) -0.0002(3) 0.0140(3) -0.0045(3) Zn5 0.0922(8) 0.0712(6) 0.1177(9) 0.0178(6) 0.0091(7) -0.0196(5) P1 0.0430(7) 0.0333(7) 0.0487(9) -0.0011(6) 0.0132(6) -0.0054(5) P2 0.0466(8) 0.0425(7) 0.0388(8) 0.0024(6) 0.0067(6) -0.0064(6) P3 0.0418(7) 0.0423(7) 0.0468(9) -0.0017(6) 0.0170(6) -0.0033(6) O1 0.044(2) 0.0303(17) 0.052(2) -0.0004(16) 0.0148(17) -0.0052(15) O2 0.048(2) 0.042(2) 0.067(3) -0.0022(19) 0.007(2) -0.0049(18) O3 0.060(2) 0.042(2) 0.055(3) 0.0013(18) 0.029(2) -0.0028(18) O4 0.050(3) 0.048(3) 0.105(4) 0.003(3) 0.019(3) 0.000(2) O5 0.065(3) 0.077(4) 0.162(6) -0.013(4) 0.055(4) 0.009(3) O6 0.046(2) 0.039(2) 0.040(2) 0.0033(16) 0.0057(17) -0.0081(16) O7 0.053(2) 0.065(3) 0.045(2) 0.008(2) 0.0144(19) -0.012(2) O8 0.060(3) 0.043(2) 0.051(3) -0.0016(18) 0.003(2) 0.0006(19) O9 0.052(2) 0.057(3) 0.059(3) -0.001(2) 0.009(2) -0.014(2) O10 0.102(4) 0.060(3) 0.075(4) 0.000(3) -0.012(3) -0.036(3) O11 0.042(2) 0.043(2) 0.044(2) 0.0035(16) 0.0158(17) 0.0003(16) O12 0.045(2) 0.072(3) 0.054(3) -0.011(2) 0.017(2) -0.011(2) O13 0.059(3) 0.041(2) 0.064(3) 0.0042(19) 0.027(2) 0.0046(18) O14 0.085(4) 0.066(3) 0.070(3) 0.023(2) 0.041(3) 0.009(3) O15 0.177(6) 0.108(5) 0.097(4) 0.039(4) 0.078(4) 0.039(4) O16 0.178(11) 0.249(14) 0.174(10) 0.003(9) 0.003(8) 0.055(10) O17 0.260(12) 0.115(6) 0.163(8) 0.022(6) 0.133(8) 0.036(7) O18 0.225(14) 0.298(18) 0.187(12) -0.032(11) -0.034(10) 0.081(13) O19 0.322(11) 0.223(10) 0.245(10) -0.009(8) 0.077(8) -0.003(8) O20 0.238(9) 0.244(9) 0.221(9) -0.056(7) 0.093(7) -0.032(7) O21 0.274(19) 0.31(2) 0.36(2) 0.024(19) -0.129(16) -0.009(16) O22 0.47(3) 0.242(17) 0.235(16) -0.038(13) 0.127(18) -0.082(18) N1 0.052(3) 0.036(2) 0.051(3) 0.000(2) 0.016(2) -0.001(2) N2 0.046(3) 0.042(3) 0.053(3) -0.005(2) 0.009(2) -0.004(2) N3 0.070(3) 0.042(3) 0.058(3) 0.000(2) 0.038(3) -0.008(2) C1 0.051(3) 0.039(3) 0.044(3) 0.001(2) 0.008(3) -0.005(2) C2 0.062(4) 0.041(3) 0.050(4) -0.001(3) 0.019(3) 0.005(3) C3 0.058(4) 0.047(4) 0.089(5) 0.006(3) 0.029(4) 0.005(3) C4 0.058(4) 0.043(3) 0.046(3) 0.004(2) 0.013(3) 0.001(3) C5 0.060(4) 0.055(4) 0.049(4) 0.012(3) 0.011(3) -0.007(3) C6 0.071(5) 0.077(5) 0.082(6) 0.027(4) 0.024(4) -0.004(4) C7 0.077(6) 0.096(7) 0.106(7) 0.043(6) 0.012(5) -0.024(5) C8 0.093(6) 0.072(6) 0.089(6) 0.035(5) -0.008(5) -0.035(5) C9 0.101(6) 0.048(4) 0.054(4) 0.015(3) 0.002(4) -0.009(4) C10 0.139(9) 0.059(5) 0.067(6) 0.004(4) 0.014(6) -0.019(5) C11 0.176(11) 0.054(5) 0.066(6) 0.004(4) 0.031(7) 0.012(6) C12 0.110(7) 0.068(5) 0.073(6) 0.006(4) 0.023(5) 0.018(5) C13 0.087(5) 0.050(4) 0.060(5) 0.012(3) 0.021(4) 0.004(3) C14 0.072(4) 0.050(3) 0.045(4) 0.009(3) 0.005(3) -0.006(3) C15 0.051(3) 0.046(3) 0.040(3) 0.000(2) 0.008(3) -0.001(2) C16 0.045(3) 0.053(3) 0.051(4) -0.002(3) 0.004(3) -0.004(3) C17 0.045(3) 0.054(4) 0.066(5) 0.002(3) 0.003(3) -0.006(3) C18 0.052(4) 0.051(3) 0.056(4) -0.008(3) 0.006(3) -0.002(3) C19 0.064(4) 0.052(4) 0.067(5) -0.007(3) 0.016(3) 0.005(3) C20 0.078(5) 0.064(5) 0.097(6) 0.016(4) 0.025(5) 0.005(4) C21 0.137(10) 0.078(6) 0.102(8) 0.032(5) 0.039(7) 0.038(6) C22 0.112(8) 0.079(6) 0.091(7) 0.009(5) 0.023(6) 0.042(6) C23 0.066(5) 0.078(5) 0.075(5) -0.019(4) -0.002(4) 0.029(4) C24 0.064(5) 0.117(8) 0.107(8) -0.043(7) -0.011(5) 0.041(6) C25 0.053(5) 0.115(9) 0.151(11) -0.039(8) 0.019(6) 0.005(5) C26 0.061(5) 0.093(6) 0.129(8) -0.021(6) 0.036(5) 0.000(4) C27 0.052(4) 0.077(5) 0.094(6) -0.010(4) 0.021(4) 0.001(4) C28 0.047(4) 0.061(4) 0.073(5) -0.012(3) 0.006(3) 0.008(3) C29 0.055(3) 0.044(3) 0.056(4) -0.002(3) 0.027(3) -0.002(3) C30 0.121(7) 0.053(4) 0.068(5) 0.009(3) 0.057(5) 0.001(4) C31 0.128(8) 0.066(5) 0.062(5) 0.016(4) 0.052(5) 0.006(5) C32 0.051(5) 0.037(5) 0.065(6) 0.006(4) 0.022(5) 0.001(4) C33 0.075(9) 0.037(6) 0.078(9) -0.004(5) 0.035(7) -0.009(6) C34 0.048(7) 0.035(5) 0.069(9) -0.004(5) 0.012(6) -0.004(5) C35 0.058(11) 0.094(13) 0.135(17) -0.008(11) 0.004(9) 0.000(9) C36 0.082(14) 0.084(12) 0.16(2) -0.029(13) 0.089(15) -0.011(10) C37 0.060(9) 0.067(8) 0.077(11) -0.012(7) 0.032(8) -0.018(7) C42 0.085(9) 0.061(7) 0.084(10) -0.008(7) 0.050(8) -0.016(7) C38 0.098(13) 0.118(15) 0.123(15) -0.013(12) 0.051(12) -0.029(11) C39 0.155(19) 0.121(15) 0.161(19) 0.016(13) 0.093(16) -0.061(14) C40 0.135(17) 0.111(15) 0.100(13) 0.014(11) 0.057(12) -0.036(13) C41 0.107(14) 0.074(10) 0.078(12) 0.018(9) 0.034(10) -0.019(10) C32A 0.051(5) 0.037(5) 0.065(6) 0.006(4) 0.022(5) 0.001(4) C33A 0.073(13) 0.056(11) 0.071(14) 0.011(9) 0.044(11) -0.011(9) C34A 0.067(14) 0.076(16) 0.064(15) -0.007(12) 0.010(11) -0.018(12) C35A 0.15(3) 0.080(19) 0.10(2) 0.027(16) 0.05(2) -0.034(19) C36A 0.063(15) 0.092(18) 0.13(2) -0.040(17) 0.051(16) -0.034(13) C37A 0.10(2) 0.041(11) 0.22(4) 0.022(17) 0.10(3) 0.024(12) C42A 0.057(12) 0.056(11) 0.086(16) 0.015(10) 0.034(11) -0.006(9) C38A 0.035(11) 0.094(19) 0.13(3) -0.023(17) 0.037(13) 0.000(11) C39A 0.068(16) 0.088(18) 0.16(3) -0.024(18) -0.031(17) 0.036(14) C40A 0.042(14) 0.067(17) 0.21(4) -0.043(19) -0.023(16) 0.007(11) C41A 0.062(18) 0.049(13) 0.17(4) -0.029(18) 0.016(19) -0.021(12) N4 0.160(8) 0.081(5) 0.110(7) -0.023(5) -0.005(6) -0.038(5) C43 0.153(9) 0.106(8) 0.148(9) -0.040(7) 0.003(8) 0.018(7) C44 0.137(8) 0.108(7) 0.119(7) -0.021(6) -0.002(6) 0.020(6) N5 0.129(6) 0.076(4) 0.084(5) -0.006(4) 0.010(4) -0.006(4) C45 0.139(11) 0.100(9) 0.093(9) -0.011(8) 0.013(9) 0.007(9) C46 0.139(13) 0.115(11) 0.101(12) -0.003(10) 0.023(10) 0.016(10) N6 0.135(12) 0.124(10) 0.109(11) 0.000(9) 0.049(9) -0.003(10) C47 0.143(12) 0.122(11) 0.114(12) -0.002(10) 0.046(10) 0.009(10) C48 0.123(9) 0.100(8) 0.115(10) -0.001(8) 0.039(8) -0.010(7) N7 0.122(13) 0.078(10) 0.133(15) -0.019(11) 0.028(13) -0.025(9) N5A 0.129(6) 0.076(4) 0.084(5) -0.006(4) 0.010(4) -0.006(4) C45A 0.134(11) 0.105(10) 0.094(9) -0.009(8) 0.006(9) 0.004(9) C46A 0.133(12) 0.121(10) 0.096(10) 0.002(9) 0.012(9) 0.006(10) N6A 0.113(11) 0.121(10) 0.106(12) 0.011(9) 0.023(9) 0.004(9) C47A 0.130(11) 0.123(10) 0.123(11) -0.008(9) 0.059(10) 0.006(10) C48A 0.136(12) 0.117(11) 0.113(13) 0.000(11) 0.043(11) -0.004(10) N7A 0.119(10) 0.104(10) 0.123(10) 0.005(8) 0.025(9) -0.010(8) _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 O1 2.102(3) 3_566 ? Zn1 O1 2.102(3) . ? Zn1 O6 2.114(4) 3_566 ? Zn1 O6 2.114(4) . ? Zn1 O11 2.144(4) . ? Zn1 O11 2.144(4) 3_566 ? Zn2 O12 1.928(4) . ? Zn2 O2 1.965(4) 3_566 ? Zn2 O9 2.118(4) . ? Zn2 O6 2.141(4) . ? Zn2 N2 2.145(5) . ? Zn3 O3 1.961(4) 3_566 ? Zn3 O7 1.981(4) 3_566 ? Zn3 O14 2.080(5) . ? Zn3 O11 2.128(4) . ? Zn3 N3 2.173(5) . ? Zn4 O8 1.953(4) . ? Zn4 O13 1.971(4) . ? Zn4 O4 2.067(5) . ? Zn4 N1 2.167(5) . ? Zn4 O1 2.217(4) . ? Zn5 O10 1.960(5) . ? Zn5 N6 1.96(2) . ? Zn5 N4 2.078(9) . ? Zn5 N7A 2.13(2) . ? Zn5 N7 2.19(2) . ? Zn5 N5 2.234(8) . ? Zn5 N6A 2.31(2) . ? P1 O2 1.518(4) . ? P1 O3 1.521(4) . ? P1 O1 1.532(4) . ? P1 C1 1.815(6) . ? P2 O7 1.512(4) . ? P2 O8 1.522(4) . ? P2 O6 1.540(4) . ? P2 C15 1.831(6) . ? P3 O13 1.519(4) . ? P3 O12 1.527(4) . ? P3 O11 1.540(4) . ? P3 C29 1.816(6) . ? O2 Zn2 1.965(4) 3_566 ? O3 Zn3 1.961(4) 3_566 ? O4 C3 1.262(8) . ? O5 C3 1.245(8) . ? O7 Zn3 1.981(4) 3_566 ? O9 C17 1.249(8) . ? O10 C17 1.259(8) . ? O14 C31 1.257(9) . ? O15 C31 1.260(9) . ? N1 C2 1.483(7) . ? N1 C1 1.503(7) . ? N1 C4 1.506(7) . ? N2 C16 1.472(7) . ? N2 C15 1.492(8) . ? N2 C18 1.520(8) . ? N3 C29 1.471(7) . ? N3 C30 1.482(9) . ? N3 C32A 1.489(9) . ? N3 C32 1.510(8) . ? C1 H1 0.9700 . ? C1 H2 0.9700 . ? C2 C3 1.528(9) . ? C2 H3 0.9700 . ? C2 H4 0.9700 . ? C4 C5 1.527(8) . ? C4 H5 0.9700 . ? C4 H6 0.9700 . ? C5 C6 1.398(10) . ? C5 C14 1.418(9) . ? C6 C7 1.411(11) . ? C6 H7 0.9300 . ? C7 C8 1.305(14) . ? C7 H8 0.9300 . ? C8 C9 1.416(13) . ? C8 H9 0.9300 . ? C9 C10 1.382(12) . ? C9 C14 1.434(9) . ? C10 C11 1.359(14) . ? C10 H10 0.9300 . ? C11 C12 1.426(14) . ? C11 H11 0.9300 . ? C12 C13 1.365(10) . ? C12 H12 0.9300 . ? C13 C14 1.398(10) . ? C13 H13 0.9300 . ? C15 H14 0.9700 . ? C15 H15 0.9700 . ? C16 C17 1.508(9) . ? C16 H16 0.9700 . ? C16 H17 0.9700 . ? C18 C19 1.515(9) . ? C18 H18 0.9700 . ? C18 H19 0.9700 . ? C19 C20 1.373(10) . ? C19 C28 1.422(10) . ? C20 C21 1.418(13) . ? C20 H20 0.9300 . ? C21 C22 1.357(15) . ? C21 H21 0.9300 . ? C22 C23 1.382(14) . ? C22 H22 0.9300 . ? C23 C24 1.421(14) . ? C23 C28 1.450(10) . ? C24 C25 1.367(16) . ? C24 H23 0.9300 . ? C25 C26 1.367(15) . ? C25 H24 0.9300 . ? C26 C27 1.378(11) . ? C26 H25 0.9300 . ? C27 C28 1.410(11) . ? C27 H26 0.9300 . ? C29 H27 0.9700 . ? C29 H28 0.9700 . ? C30 C31 1.508(12) . ? C30 H29 0.9700 . ? C30 H30 0.9700 . ? C32 C33 1.535(8) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.3900 . ? C33 C42 1.3900 . ? C34 C35 1.3900 . ? C34 H34A 0.9300 . ? C35 C36 1.3900 . ? C35 H35A 0.9300 . ? C36 C37 1.3900 . ? C36 H36A 0.9300 . ? C37 C38 1.389(9) . ? C37 C42 1.3900 . ? C42 C41 1.398(8) . ? C38 C39 1.376(9) . ? C38 H38A 0.9300 . ? C39 C40 1.383(9) . ? C39 H39A 0.9300 . ? C40 C41 1.381(9) . ? C40 H40A 0.9300 . ? C41 H41A 0.9300 . ? C32A C33A 1.513(10) . ? C32A H32C 0.9700 . ? C32A H32D 0.9700 . ? C33A C34A 1.3900 . ? C33A C42A 1.3900 . ? C34A C35A 1.3900 . ? C34A H34B 0.9300 . ? C35A C36A 1.3900 . ? C35A H35B 0.9300 . ? C36A C37A 1.3900 . ? C36A H36B 0.9300 . ? C37A C38A 1.381(10) . ? C37A C42A 1.3900 . ? C42A C41A 1.379(9) . ? C38A C39A 1.373(9) . ? C38A H38B 0.9300 . ? C39A C40A 1.380(9) . ? C39A H39B 0.9300 . ? C40A C41A 1.378(9) . ? C40A H40B 0.9300 . ? C41A H41B 0.9300 . ? N4 C43 1.469(8) . ? N4 H4A 0.9000 . ? N4 H4B 0.9000 . ? C43 C44 1.506(9) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 N5 1.458(8) . ? C44 H44A 0.9599 . ? C44 H44B 0.9598 . ? N5 C45 1.471(10) . ? N5 H5A 0.9100 . ? C45 C46 1.528(10) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 N6 1.464(10) . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? N6 C47 1.483(10) . ? N6 H6A 0.9100 . ? C47 C48 1.527(10) . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C48 N7 1.467(10) . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? N7 H7A 0.9000 . ? N7 H7B 0.9000 . ? C45A C46A 1.529(10) . ? C45A H45C 0.9700 . ? C45A H45D 0.9700 . ? C46A N6A 1.467(17) . ? C46A H46C 0.9700 . ? C46A H46D 0.9700 . ? N6A C47A 1.433(17) . ? N6A H6AA 0.9100 . ? C47A C48A 1.531(10) . ? C47A H47C 0.9700 . ? C47A H47D 0.9700 . ? C48A N7A 1.452(17) . ? C48A H48C 0.9700 . ? C48A H48D 0.9700 . ? N7A H7C 0.9000 . ? N7A H7D 0.9000 . ? 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 Zn1 O1 180.000(1) 3_566 . ? O1 Zn1 O6 88.57(14) 3_566 3_566 ? O1 Zn1 O6 91.43(14) . 3_566 ? O1 Zn1 O6 91.43(14) 3_566 . ? O1 Zn1 O6 88.57(14) . . ? O6 Zn1 O6 180.000(1) 3_566 . ? O1 Zn1 O11 89.04(14) 3_566 . ? O1 Zn1 O11 90.96(14) . . ? O6 Zn1 O11 91.27(15) 3_566 . ? O6 Zn1 O11 88.73(15) . . ? O1 Zn1 O11 90.96(14) 3_566 3_566 ? O1 Zn1 O11 89.04(14) . 3_566 ? O6 Zn1 O11 88.73(15) 3_566 3_566 ? O6 Zn1 O11 91.27(15) . 3_566 ? O11 Zn1 O11 180.000(1) . 3_566 ? O12 Zn2 O2 120.2(2) . 3_566 ? O12 Zn2 O9 98.16(18) . . ? O2 Zn2 O9 89.31(17) 3_566 . ? O12 Zn2 O6 96.31(17) . . ? O2 Zn2 O6 93.17(16) 3_566 . ? O9 Zn2 O6 161.62(17) . . ? O12 Zn2 N2 110.3(2) . . ? O2 Zn2 N2 129.20(19) 3_566 . ? O9 Zn2 N2 77.98(18) . . ? O6 Zn2 N2 86.41(16) . . ? O3 Zn3 O7 116.73(18) 3_566 3_566 ? O3 Zn3 O14 98.58(19) 3_566 . ? O7 Zn3 O14 89.82(19) 3_566 . ? O3 Zn3 O11 97.31(16) 3_566 . ? O7 Zn3 O11 94.22(16) 3_566 . ? O14 Zn3 O11 159.71(18) . . ? O3 Zn3 N3 112.29(18) 3_566 . ? O7 Zn3 N3 130.74(19) 3_566 . ? O14 Zn3 N3 78.2(2) . . ? O11 Zn3 N3 84.12(17) . . ? O8 Zn4 O13 121.28(18) . . ? O8 Zn4 O4 99.2(2) . . ? O13 Zn4 O4 94.39(19) . . ? O8 Zn4 N1 114.66(18) . . ? O13 Zn4 N1 124.03(19) . . ? O4 Zn4 N1 78.27(18) . . ? O8 Zn4 O1 94.60(16) . . ? O13 Zn4 O1 89.15(16) . . ? O4 Zn4 O1 161.24(17) . . ? N1 Zn4 O1 84.48(16) . . ? O10 Zn5 N6 128.1(7) . . ? O10 Zn5 N4 109.7(3) . . ? N6 Zn5 N4 122.1(7) . . ? O10 Zn5 N7A 98.8(7) . . ? N6 Zn5 N7A 60.6(8) . . ? N4 Zn5 N7A 110.8(7) . . ? O10 Zn5 N7 83.4(6) . . ? N6 Zn5 N7 83.3(8) . . ? N4 Zn5 N7 100.8(6) . . ? N7A Zn5 N7 22.7(6) . . ? O10 Zn5 N5 101.3(3) . . ? N6 Zn5 N5 91.2(7) . . ? N4 Zn5 N5 80.7(3) . . ? N7A Zn5 N5 151.7(6) . . ? N7 Zn5 N5 174.3(6) . . ? O10 Zn5 N6A 117.2(6) . . ? N6 Zn5 N6A 21.4(7) . . ? N4 Zn5 N6A 130.1(6) . . ? N7A Zn5 N6A 78.5(7) . . ? N7 Zn5 N6A 100.3(7) . . ? N5 Zn5 N6A 74.7(5) . . ? O2 P1 O3 112.8(3) . . ? O2 P1 O1 114.0(2) . . ? O3 P1 O1 111.5(2) . . ? O2 P1 C1 104.9(3) . . ? O3 P1 C1 109.8(3) . . ? O1 P1 C1 103.1(2) . . ? O7 P2 O8 112.7(3) . . ? O7 P2 O6 112.9(2) . . ? O8 P2 O6 112.7(2) . . ? O7 P2 C15 105.9(3) . . ? O8 P2 C15 108.7(3) . . ? O6 P2 C15 103.2(2) . . ? O13 P3 O12 113.2(3) . . ? O13 P3 O11 113.0(2) . . ? O12 P3 O11 111.5(2) . . ? O13 P3 C29 107.3(3) . . ? O12 P3 C29 107.2(3) . . ? O11 P3 C29 104.0(3) . . ? P1 O1 Zn1 126.7(2) . . ? P1 O1 Zn4 112.7(2) . . ? Zn1 O1 Zn4 117.98(16) . . ? P1 O2 Zn2 130.0(3) . 3_566 ? P1 O3 Zn3 123.4(2) . 3_566 ? C3 O4 Zn4 113.8(4) . . ? P2 O6 Zn1 127.6(2) . . ? P2 O6 Zn2 113.4(2) . . ? Zn1 O6 Zn2 116.41(17) . . ? P2 O7 Zn3 127.9(3) . 3_566 ? P2 O8 Zn4 125.2(3) . . ? C17 O9 Zn2 111.4(4) . . ? C17 O10 Zn5 121.0(5) . . ? P3 O11 Zn3 116.2(2) . . ? P3 O11 Zn1 125.9(2) . . ? Zn3 O11 Zn1 116.22(17) . . ? P3 O12 Zn2 124.2(3) . . ? P3 O13 Zn4 128.4(3) . . ? C31 O14 Zn3 114.4(5) . . ? C2 N1 C1 112.9(5) . . ? C2 N1 C4 112.3(5) . . ? C1 N1 C4 111.8(5) . . ? C2 N1 Zn4 101.7(3) . . ? C1 N1 Zn4 109.5(3) . . ? C4 N1 Zn4 108.0(3) . . ? C16 N2 C15 113.1(5) . . ? C16 N2 C18 111.8(5) . . ? C15 N2 C18 112.5(5) . . ? C16 N2 Zn2 104.6(4) . . ? C15 N2 Zn2 109.0(3) . . ? C18 N2 Zn2 105.3(4) . . ? C29 N3 C30 112.5(5) . . ? C29 N3 C32A 124.8(10) . . ? C30 N3 C32A 103.7(10) . . ? C29 N3 C32 106.4(6) . . ? C30 N3 C32 116.1(6) . . ? C32A N3 C32 18.5(11) . . ? C29 N3 Zn3 111.2(3) . . ? C30 N3 Zn3 104.9(5) . . ? C32A N3 Zn3 97.2(6) . . ? C32 N3 Zn3 105.5(4) . . ? N1 C1 P1 110.8(4) . . ? N1 C1 H1 109.5 . . ? P1 C1 H1 109.5 . . ? N1 C1 H2 109.5 . . ? P1 C1 H2 109.5 . . ? H1 C1 H2 108.1 . . ? N1 C2 C3 110.0(5) . . ? N1 C2 H3 109.7 . . ? C3 C2 H3 109.7 . . ? N1 C2 H4 109.7 . . ? C3 C2 H4 109.7 . . ? H3 C2 H4 108.2 . . ? O5 C3 O4 124.4(7) . . ? O5 C3 C2 118.3(7) . . ? O4 C3 C2 117.2(6) . . ? N1 C4 C5 116.1(5) . . ? N1 C4 H5 108.3 . . ? C5 C4 H5 108.3 . . ? N1 C4 H6 108.3 . . ? C5 C4 H6 108.3 . . ? H5 C4 H6 107.4 . . ? C6 C5 C14 118.6(6) . . ? C6 C5 C4 117.4(6) . . ? C14 C5 C4 124.0(6) . . ? C5 C6 C7 121.3(8) . . ? C5 C6 H7 119.4 . . ? C7 C6 H7 119.4 . . ? C8 C7 C6 120.6(9) . . ? C8 C7 H8 119.7 . . ? C6 C7 H8 119.7 . . ? C7 C8 C9 121.8(7) . . ? C7 C8 H9 119.1 . . ? C9 C8 H9 119.1 . . ? C10 C9 C8 121.1(8) . . ? C10 C9 C14 119.6(9) . . ? C8 C9 C14 119.3(7) . . ? C11 C10 C9 121.1(9) . . ? C11 C10 H10 119.4 . . ? C9 C10 H10 119.4 . . ? C10 C11 C12 120.5(9) . . ? C10 C11 H11 119.7 . . ? C12 C11 H11 119.7 . . ? C13 C12 C11 118.8(10) . . ? C13 C12 H12 120.6 . . ? C11 C12 H12 120.6 . . ? C12 C13 C14 122.0(8) . . ? C12 C13 H13 119.0 . . ? C14 C13 H13 119.0 . . ? C13 C14 C5 123.6(6) . . ? C13 C14 C9 118.1(7) . . ? C5 C14 C9 118.4(7) . . ? N2 C15 P2 110.7(4) . . ? N2 C15 H14 109.5 . . ? P2 C15 H14 109.5 . . ? N2 C15 H15 109.5 . . ? P2 C15 H15 109.5 . . ? H14 C15 H15 108.1 . . ? N2 C16 C17 112.3(5) . . ? N2 C16 H16 109.1 . . ? C17 C16 H16 109.1 . . ? N2 C16 H17 109.1 . . ? C17 C16 H17 109.1 . . ? H16 C16 H17 107.9 . . ? O9 C17 O10 124.4(7) . . ? O9 C17 C16 118.6(6) . . ? O10 C17 C16 116.9(6) . . ? C19 C18 N2 116.0(5) . . ? C19 C18 H18 108.3 . . ? N2 C18 H18 108.3 . . ? C19 C18 H19 108.3 . . ? N2 C18 H19 108.3 . . ? H18 C18 H19 107.4 . . ? C20 C19 C28 118.2(7) . . ? C20 C19 C18 120.1(7) . . ? C28 C19 C18 121.6(7) . . ? C19 C20 C21 122.5(9) . . ? C19 C20 H20 118.7 . . ? C21 C20 H20 118.7 . . ? C22 C21 C20 119.4(10) . . ? C22 C21 H21 120.3 . . ? C20 C21 H21 120.3 . . ? C21 C22 C23 121.0(9) . . ? C21 C22 H22 119.5 . . ? C23 C22 H22 119.5 . . ? C22 C23 C24 122.4(9) . . ? C22 C23 C28 120.1(9) . . ? C24 C23 C28 117.5(9) . . ? C25 C24 C23 122.5(9) . . ? C25 C24 H23 118.8 . . ? C23 C24 H23 118.8 . . ? C24 C25 C26 120.1(10) . . ? C24 C25 H24 119.9 . . ? C26 C25 H24 119.9 . . ? C25 C26 C27 120.1(10) . . ? C25 C26 H25 119.9 . . ? C27 C26 H25 119.9 . . ? C26 C27 C28 122.8(9) . . ? C26 C27 H26 118.6 . . ? C28 C27 H26 118.6 . . ? C27 C28 C19 124.5(7) . . ? C27 C28 C23 116.9(7) . . ? C19 C28 C23 118.6(8) . . ? N3 C29 P3 110.6(4) . . ? N3 C29 H27 109.5 . . ? P3 C29 H27 109.5 . . ? N3 C29 H28 109.5 . . ? P3 C29 H28 109.5 . . ? H27 C29 H28 108.1 . . ? N3 C30 C31 111.1(6) . . ? N3 C30 H29 109.4 . . ? C31 C30 H29 109.4 . . ? N3 C30 H30 109.4 . . ? C31 C30 H30 109.4 . . ? H29 C30 H30 108.0 . . ? O14 C31 O15 122.9(8) . . ? O14 C31 C30 119.0(6) . . ? O15 C31 C30 118.1(7) . . ? N3 C32 C33 126.9(6) . . ? N3 C32 H32A 105.6 . . ? C33 C32 H32A 105.6 . . ? N3 C32 H32B 105.6 . . ? C33 C32 H32B 105.6 . . ? H32A C32 H32B 106.1 . . ? C34 C33 C42 120.0 . . ? C34 C33 C32 116.4(7) . . ? C42 C33 C32 123.5(7) . . ? C35 C34 C33 120.0 . . ? C35 C34 H34A 120.0 . . ? C33 C34 H34A 120.0 . . ? C34 C35 C36 120.0 . . ? C34 C35 H35A 120.0 . . ? C36 C35 H35A 120.0 . . ? C35 C36 C37 120.0 . . ? C35 C36 H36A 120.0 . . ? C37 C36 H36A 120.0 . . ? C38 C37 C42 121.9(9) . . ? C38 C37 C36 118.1(9) . . ? C42 C37 C36 120.0 . . ? C37 C42 C33 120.0 . . ? C37 C42 C41 117.4(7) . . ? C33 C42 C41 122.6(7) . . ? C39 C38 C37 120.1(11) . . ? C39 C38 H38A 119.9 . . ? C37 C38 H38A 119.9 . . ? C38 C39 C40 118.6(10) . . ? C38 C39 H39A 120.7 . . ? C40 C39 H39A 120.7 . . ? C41 C40 C39 121.7(10) . . ? C41 C40 H40A 119.1 . . ? C39 C40 H40A 119.1 . . ? C40 C41 C42 120.3(10) . . ? C40 C41 H41A 119.9 . . ? C42 C41 H41A 119.9 . . ? N3 C32A C33A 117.2(8) . . ? N3 C32A H32C 108.0 . . ? C33A C32A H32C 108.0 . . ? N3 C32A H32D 108.0 . . ? C33A C32A H32D 108.0 . . ? H32C C32A H32D 107.2 . . ? C34A C33A C42A 120.0 . . ? C34A C33A C32A 115.6(13) . . ? C42A C33A C32A 124.3(13) . . ? C35A C34A C33A 120.0 . . ? C35A C34A H34B 120.0 . . ? C33A C34A H34B 120.0 . . ? C36A C35A C34A 120.0 . . ? C36A C35A H35B 120.0 . . ? C34A C35A H35B 120.0 . . ? C35A C36A C37A 120.0 . . ? C35A C36A H36B 120.0 . . ? C37A C36A H36B 120.0 . . ? C38A C37A C42A 120.6(12) . . ? C38A C37A C36A 119.4(12) . . ? C42A C37A C36A 120.0 . . ? C41A C42A C37A 118.0(10) . . ? C41A C42A C33A 122.0(10) . . ? C37A C42A C33A 120.0 . . ? C39A C38A C37A 120.3(13) . . ? C39A C38A H38B 119.8 . . ? C37A C38A H38B 119.8 . . ? C38A C39A C40A 119.8(11) . . ? C38A C39A H39B 120.1 . . ? C40A C39A H39B 120.1 . . ? C41A C40A C39A 119.6(12) . . ? C41A C40A H40B 120.2 . . ? C39A C40A H40B 120.2 . . ? C40A C41A C42A 121.7(12) . . ? C40A C41A H41B 119.2 . . ? C42A C41A H41B 119.2 . . ? C43 N4 Zn5 108.5(7) . . ? C43 N4 H4A 110.0 . . ? Zn5 N4 H4A 110.0 . . ? C43 N4 H4B 110.0 . . ? Zn5 N4 H4B 110.0 . . ? H4A N4 H4B 108.4 . . ? N4 C43 C44 112.1(9) . . ? N4 C43 H43A 109.2 . . ? C44 C43 H43A 109.2 . . ? N4 C43 H43B 109.2 . . ? C44 C43 H43B 109.2 . . ? H43A C43 H43B 107.9 . . ? N5 C44 C43 111.3(9) . . ? N5 C44 H44A 109.0 . . ? C43 C44 H44A 109.4 . . ? N5 C44 H44B 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 108.0 . . ? C44 N5 C45 111.2(13) . . ? C44 N5 Zn5 109.1(6) . . ? C45 N5 Zn5 98.5(12) . . ? C44 N5 H5A 112.4 . . ? C45 N5 H5A 112.4 . . ? Zn5 N5 H5A 112.4 . . ? N5 C45 C46 113(2) . . ? N5 C45 H45A 109.0 . . ? C46 C45 H45A 109.0 . . ? N5 C45 H45B 109.0 . . ? C46 C45 H45B 109.0 . . ? H45A C45 H45B 107.8 . . ? N6 C46 C45 117(2) . . ? N6 C46 H46A 108.1 . . ? C45 C46 H46A 108.1 . . ? N6 C46 H46B 108.1 . . ? C45 C46 H46B 108.1 . . ? H46A C46 H46B 107.3 . . ? C46 N6 C47 118(2) . . ? C46 N6 Zn5 101.0(19) . . ? C47 N6 Zn5 112.6(15) . . ? C46 N6 H6A 108.2 . . ? C47 N6 H6A 108.2 . . ? Zn5 N6 H6A 108.2 . . ? N6 C47 C48 98.9(19) . . ? N6 C47 H47A 112.0 . . ? C48 C47 H47A 112.0 . . ? N6 C47 H47B 112.0 . . ? C48 C47 H47B 112.0 . . ? H47A C47 H47B 109.7 . . ? N7 C48 C47 124(2) . . ? N7 C48 H48A 106.4 . . ? C47 C48 H48A 106.4 . . ? N7 C48 H48B 106.4 . . ? C47 C48 H48B 106.4 . . ? H48A C48 H48B 106.5 . . ? C48 N7 Zn5 99.9(16) . . ? C48 N7 H7A 111.8 . . ? Zn5 N7 H7A 111.8 . . ? C48 N7 H7B 111.8 . . ? Zn5 N7 H7B 111.8 . . ? H7A N7 H7B 109.5 . . ? C46A C45A H45C 110.5 . . ? C46A C45A H45D 110.5 . . ? H45C C45A H45D 108.7 . . ? N6A C46A C45A 111(2) . . ? N6A C46A H46C 109.4 . . ? C45A C46A H46C 109.4 . . ? N6A C46A H46D 109.4 . . ? C45A C46A H46D 109.4 . . ? H46C C46A H46D 108.0 . . ? C47A N6A C46A 117.7(19) . . ? C47A N6A Zn5 109.4(16) . . ? C46A N6A Zn5 106.4(16) . . ? C47A N6A H6AA 107.7 . . ? C46A N6A H6AA 107.7 . . ? Zn5 N6A H6AA 107.7 . . ? N6A C47A C48A 106.6(19) . . ? N6A C47A H47C 110.4 . . ? C48A C47A H47C 110.4 . . ? N6A C47A H47D 110.4 . . ? C48A C47A H47D 110.4 . . ? H47C C47A H47D 108.6 . . ? N7A C48A C47A 114.8(19) . . ? N7A C48A H48C 108.6 . . ? C47A C48A H48C 108.6 . . ? N7A C48A H48D 108.6 . . ? C47A C48A H48D 108.6 . . ? H48C C48A H48D 107.6 . . ? C48A N7A Zn5 110.4(16) . . ? C48A N7A H7C 109.6 . . ? Zn5 N7A H7C 109.6 . . ? C48A N7A H7D 109.6 . . ? Zn5 N7A H7D 109.6 . . ? H7C N7A H7D 108.1 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.848 _refine_diff_density_min -0.755 _refine_diff_density_rms 0.095 _database_code_depnum_ccdc_archive 'CCDC 954975' ####################################################################### # # 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_f1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C108 H146 N10 O32 P6 Zn7' _chemical_formula_weight 2739.76 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' P P 0.1023 0.0942 '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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.789(6) _cell_length_b 18.802(7) _cell_length_c 20.840(8) _cell_angle_alpha 90.00 _cell_angle_beta 103.286(7) _cell_angle_gamma 90.00 _cell_volume 6021(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 20328 _cell_measurement_theta_min 2.1323 _cell_measurement_theta_max 27.4855 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.2200 _exptl_crystal_size_mid 0.1900 _exptl_crystal_size_min 0.1500 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.511 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2840 _exptl_absorpt_coefficient_mu 1.530 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7524 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2007)' _exptl_special_details ; The single crystal has been irradiated under a UV lamp at 254 and 365 nm for 24 hours. ; _diffrn_ambient_temperature 293(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 'Saturn724+ (2x2 bin mode)' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 50745 _diffrn_reflns_av_R_equivalents 0.0364 _diffrn_reflns_av_sigmaI/netI 0.0518 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 27.53 _reflns_number_total 13638 _reflns_number_gt 10860 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Due to the moderate diffraction intensity and slightly abnormal triethylamine cation, so hydrogen atoms were generated geometrically. The free triethylamine cation N4(C43C44)(C45C46)(C47C48), C39 and C54 are slightly abnormal, so the distance/angle and isotropic are restrained. The restraints used in the refinement are listed as follows: dfix 1.51 0.01 n4 c43 c43 c44 n4 c45 c45 c46 n4 c47 c47 c48 DFIX 2.48 C43 C45 C43 C47 C45 C47 isor 0.01 c39 c43 c44 c45 c46 c47 c48 c54 ; _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^)+(0.0744P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13638 _refine_ls_number_parameters 736 _refine_ls_number_restraints 57 _refine_ls_R_factor_all 0.0595 _refine_ls_R_factor_gt 0.0451 _refine_ls_wR_factor_ref 0.1338 _refine_ls_wR_factor_gt 0.1227 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.060 _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 Zn1 Zn 0.5000 0.0000 0.5000 0.02813(12) Uani 1 2 d S . . Zn2 Zn 0.63170(2) -0.100972(17) 0.636305(17) 0.03178(10) Uani 1 1 d . . . Zn3 Zn 0.42591(2) 0.157663(18) 0.577323(19) 0.03518(10) Uani 1 1 d . . . Zn4 Zn 0.34472(2) -0.070082(18) 0.591793(19) 0.03468(10) Uani 1 1 d . . . P1 P 0.52410(5) 0.16637(4) 0.46179(4) 0.03103(17) Uani 1 1 d . . . P2 P 0.30087(5) 0.05422(4) 0.48754(4) 0.03150(17) Uani 1 1 d . . . P3 P 0.50220(5) 0.01900(4) 0.65641(4) 0.03249(17) Uani 1 1 d . . . O1 O 0.50094(13) 0.11248(10) 0.51028(10) 0.0320(4) Uani 1 1 d . . . O2 O 0.45048(14) 0.17559(11) 0.40079(11) 0.0388(5) Uani 1 1 d . . . O3 O 0.61178(14) 0.15301(11) 0.44620(13) 0.0423(6) Uani 1 1 d . . . O4 O 0.38737(19) 0.22747(13) 0.63993(14) 0.0568(7) Uani 1 1 d . . . O5 O 0.4228(2) 0.32992(17) 0.69135(16) 0.0749(9) Uani 1 1 d . . . O6 O 0.37268(12) -0.00002(10) 0.51577(11) 0.0314(4) Uani 1 1 d . . . O7 O 0.31370(13) 0.12390(11) 0.52536(12) 0.0409(5) Uani 1 1 d . . . O8 O 0.28674(13) 0.06331(12) 0.41353(12) 0.0417(5) Uani 1 1 d . . . O9 O 0.27595(16) -0.13280(14) 0.64514(14) 0.0536(7) Uani 1 1 d . . . O10 O 0.14727(19) -0.18272(15) 0.63552(16) 0.0640(8) Uani 1 1 d . . . O11 O 0.54235(12) -0.01469(10) 0.60312(10) 0.0306(4) Uani 1 1 d . . . O12 O 0.49081(16) 0.09860(11) 0.64962(12) 0.0454(6) Uani 1 1 d . . . O13 O 0.42116(14) -0.02023(13) 0.66444(11) 0.0413(5) Uani 1 1 d . . . O14 O 0.73209(15) -0.15903(12) 0.69722(12) 0.0430(5) Uani 1 1 d . . . O15 O 0.83371(16) -0.14674(16) 0.78993(15) 0.0657(8) Uani 1 1 d . . . O16 O 0.3048(3) -0.0988(2) 0.3887(2) 0.1098(14) Uani 1 1 d . . . H1 H 0.3560 -0.0985 0.3820 0.132 Uiso 1 1 d R . . H2 H 0.2841 -0.0568 0.3850 0.132 Uiso 1 1 d R . . N1 N 0.46353(15) 0.25934(12) 0.54148(13) 0.0325(5) Uani 1 1 d . . . N2 N 0.21689(15) -0.02256(13) 0.56629(13) 0.0308(5) Uani 1 1 d . . . N3 N 0.62262(16) -0.06723(12) 0.73447(13) 0.0315(5) Uani 1 1 d . . . N4 N 0.2240(3) 0.2358(3) 0.7748(3) 0.0969(15) Uani 1 1 d D . . H3 H 0.2620 0.2694 0.7956 0.116 Uiso 1 1 calc R . . N5 N -0.1419(2) -0.25045(18) 0.67015(18) 0.0614(9) Uani 1 1 d . . . H4 H -0.1819 -0.2178 0.6760 0.074 Uiso 1 1 calc R . . C1 C 0.53711(19) 0.24870(15) 0.50902(16) 0.0354(7) Uani 1 1 d . . . H5 H 0.5913 0.2472 0.5422 0.042 Uiso 1 1 calc R . . H6 H 0.5398 0.2885 0.4799 0.042 Uiso 1 1 calc R . . C2 C 0.4275(2) 0.28684(19) 0.64844(18) 0.0474(8) Uani 1 1 d . . . C3 C 0.4862(2) 0.30317(18) 0.60155(17) 0.0445(8) Uani 1 1 d . . . H7 H 0.4808 0.3531 0.5895 0.053 Uiso 1 1 calc R . . H8 H 0.5463 0.2943 0.6238 0.053 Uiso 1 1 calc R . . C4 C 0.38336(19) 0.28677(16) 0.49504(16) 0.0374(7) Uani 1 1 d . . . H9 H 0.3374 0.2898 0.5188 0.045 Uiso 1 1 calc R . . H10 H 0.3653 0.2520 0.4602 0.045 Uiso 1 1 calc R . . C5 C 0.3906(2) 0.35840(17) 0.46332(19) 0.0440(8) Uani 1 1 d . . . C6 C 0.4191(3) 0.3589(2) 0.4056(2) 0.0651(11) Uani 1 1 d . . . H11 H 0.4338 0.3161 0.3886 0.078 Uiso 1 1 calc R . . C7 C 0.4264(4) 0.4233(3) 0.3715(3) 0.0893(17) Uani 1 1 d . . . H12 H 0.4474 0.4225 0.3333 0.107 Uiso 1 1 calc R . . C8 C 0.4033(4) 0.4852(3) 0.3945(3) 0.0898(18) Uani 1 1 d . . . H13 H 0.4086 0.5271 0.3720 0.108 Uiso 1 1 calc R . . C9 C 0.3712(3) 0.4877(2) 0.4516(3) 0.0754(15) Uani 1 1 d . . . C10 C 0.3445(5) 0.5522(3) 0.4742(5) 0.121(3) Uani 1 1 d . . . H14 H 0.3491 0.5941 0.4516 0.145 Uiso 1 1 calc R . . C11 C 0.3115(6) 0.5537(4) 0.5295(5) 0.147(4) Uani 1 1 d . . . H15 H 0.2928 0.5966 0.5437 0.177 Uiso 1 1 calc R . . C12 C 0.3056(5) 0.4922(3) 0.5645(4) 0.128(3) Uani 1 1 d . . . H16 H 0.2837 0.4945 0.6023 0.154 Uiso 1 1 calc R . . C13 C 0.3311(4) 0.4280(3) 0.5449(3) 0.0810(15) Uani 1 1 d . . . H17 H 0.3263 0.3874 0.5692 0.097 Uiso 1 1 calc R . . C14 C 0.3645(3) 0.42310(19) 0.4883(2) 0.0571(11) Uani 1 1 d . . . C15 C 0.20305(18) 0.01023(16) 0.49945(16) 0.0342(6) Uani 1 1 d . . . H18 H 0.1561 0.0446 0.4939 0.041 Uiso 1 1 calc R . . H19 H 0.1860 -0.0264 0.4662 0.041 Uiso 1 1 calc R . . C16 C 0.1947(2) -0.13655(17) 0.62034(19) 0.0436(8) Uani 1 1 d . . . C17 C 0.1559(2) -0.08202(16) 0.56839(18) 0.0390(7) Uani 1 1 d . . . H20 H 0.1410 -0.1049 0.5256 0.047 Uiso 1 1 calc R . . H21 H 0.1028 -0.0633 0.5777 0.047 Uiso 1 1 calc R . . C18 C 0.21792(19) 0.03080(17) 0.62035(16) 0.0363(7) Uani 1 1 d . . . H22 H 0.2649 0.0642 0.6208 0.044 Uiso 1 1 calc R . . H23 H 0.2310 0.0059 0.6622 0.044 Uiso 1 1 calc R . . C19 C 0.1347(2) 0.07249(17) 0.61530(17) 0.0377(7) Uani 1 1 d . . . C20 C 0.1229(3) 0.13244(19) 0.5784(2) 0.0533(9) Uani 1 1 d . . . H24 H 0.1670 0.1474 0.5585 0.064 Uiso 1 1 calc R . . C21 C 0.0458(3) 0.1730(3) 0.5690(2) 0.0712(13) Uani 1 1 d . . . H25 H 0.0391 0.2138 0.5430 0.085 Uiso 1 1 calc R . . C22 C -0.0175(3) 0.1525(3) 0.5978(2) 0.0717(14) Uani 1 1 d . . . H26 H -0.0687 0.1788 0.5908 0.086 Uiso 1 1 calc R . . C23 C -0.0088(2) 0.0919(2) 0.6387(2) 0.0549(10) Uani 1 1 d . . . C24 C -0.0756(3) 0.0715(3) 0.6692(3) 0.0777(15) Uani 1 1 d . . . H27 H -0.1278 0.0965 0.6605 0.093 Uiso 1 1 calc R . . C25 C -0.0642(4) 0.0153(3) 0.7116(3) 0.0880(18) Uani 1 1 d . . . H28 H -0.1087 0.0028 0.7319 0.106 Uiso 1 1 calc R . . C26 C 0.0140(4) -0.0242(3) 0.7254(3) 0.0790(15) Uani 1 1 d . . . H29 H 0.0218 -0.0618 0.7551 0.095 Uiso 1 1 calc R . . C27 C 0.0780(3) -0.0060(2) 0.6940(2) 0.0563(10) Uani 1 1 d . . . H30 H 0.1291 -0.0325 0.7024 0.068 Uiso 1 1 calc R . . C28 C 0.0694(2) 0.05131(18) 0.64925(18) 0.0434(8) Uani 1 1 d . . . C29 C 0.5865(2) 0.00608(15) 0.73108(16) 0.0346(7) Uani 1 1 d . . . H31 H 0.6328 0.0402 0.7321 0.042 Uiso 1 1 calc R . . H32 H 0.5623 0.0145 0.7692 0.042 Uiso 1 1 calc R . . C30 C 0.7645(2) -0.13037(18) 0.75339(18) 0.0408(7) Uani 1 1 d . . . C31 C 0.71271(19) -0.07003(16) 0.77422(16) 0.0366(7) Uani 1 1 d . . . H33 H 0.7118 -0.0760 0.8203 0.044 Uiso 1 1 calc R . . H34 H 0.7414 -0.0253 0.7699 0.044 Uiso 1 1 calc R . . C32 C 0.5646(2) -0.12137(17) 0.75614(16) 0.0386(7) Uani 1 1 d . . . H35 H 0.5878 -0.1683 0.7511 0.046 Uiso 1 1 calc R . . H36 H 0.5076 -0.1186 0.7265 0.046 Uiso 1 1 calc R . . C33 C 0.5533(2) -0.11441(19) 0.82693(19) 0.0451(8) Uani 1 1 d . . . C34 C 0.4902(3) -0.0700(2) 0.8388(2) 0.0644(11) Uani 1 1 d . . . H37 H 0.4555 -0.0451 0.8039 0.077 Uiso 1 1 calc R . . C35 C 0.4764(4) -0.0613(3) 0.9026(3) 0.0933(18) Uani 1 1 d . . . H38 H 0.4343 -0.0299 0.9102 0.112 Uiso 1 1 calc R . . C36 C 0.5261(5) -0.0998(3) 0.9535(3) 0.0929(19) Uani 1 1 d . . . H39 H 0.5170 -0.0939 0.9957 0.111 Uiso 1 1 calc R . . C37 C 0.5896(4) -0.1473(3) 0.9440(2) 0.0711(13) Uani 1 1 d . . . C38 C 0.6403(4) -0.1895(3) 0.9972(2) 0.093(2) Uani 1 1 d . . . H40 H 0.6303 -0.1857 1.0393 0.111 Uiso 1 1 calc R . . C39 C 0.7025(4) -0.2347(3) 0.9860(3) 0.098(2) Uani 1 1 d U . . H41 H 0.7358 -0.2606 1.0209 0.118 Uiso 1 1 calc R . . C40 C 0.7170(3) -0.2428(3) 0.9232(3) 0.0805(17) Uani 1 1 d . . . H42 H 0.7590 -0.2746 0.9162 0.097 Uiso 1 1 calc R . . C41 C 0.6696(2) -0.2042(2) 0.8716(2) 0.0571(10) Uani 1 1 d . . . H43 H 0.6802 -0.2104 0.8299 0.068 Uiso 1 1 calc R . . C42 C 0.6047(2) -0.1548(2) 0.87965(19) 0.0523(10) Uani 1 1 d . . . C43 C 0.1864(9) 0.1975(8) 0.8267(6) 0.303(8) Uani 1 1 d DU . . H44 H 0.2087 0.1493 0.8324 0.364 Uiso 1 1 calc R . . H45 H 0.2040 0.2219 0.8687 0.364 Uiso 1 1 calc R . . C44 C 0.0906(9) 0.1960(9) 0.8059(7) 0.293(8) Uani 1 1 d DU . . H46 H 0.0670 0.1772 0.8409 0.440 Uiso 1 1 calc R . . H47 H 0.0732 0.1664 0.7676 0.440 Uiso 1 1 calc R . . H48 H 0.0691 0.2434 0.7956 0.440 Uiso 1 1 calc R . . C45 C 0.1600(6) 0.2706(5) 0.7232(5) 0.216(5) Uani 1 1 d DU . . H49 H 0.1191 0.2976 0.7419 0.259 Uiso 1 1 calc R . . H50 H 0.1280 0.2359 0.6926 0.259 Uiso 1 1 calc R . . C46 C 0.2132(5) 0.3208(5) 0.6880(5) 0.152(3) Uani 1 1 d DU . . H51 H 0.1743 0.3455 0.6529 0.228 Uiso 1 1 calc R . . H52 H 0.2536 0.2932 0.6702 0.228 Uiso 1 1 calc R . . H53 H 0.2444 0.3547 0.7191 0.228 Uiso 1 1 calc R . . C47 C 0.2752(6) 0.1795(5) 0.7480(4) 0.163(4) Uani 1 1 d DU . . H54 H 0.2343 0.1433 0.7269 0.195 Uiso 1 1 calc R . . H55 H 0.2987 0.2015 0.7137 0.195 Uiso 1 1 calc R . . C48 C 0.3486(7) 0.1426(5) 0.7944(5) 0.184(4) Uani 1 1 d DU . . H56 H 0.3732 0.1073 0.7707 0.276 Uiso 1 1 calc R . . H57 H 0.3271 0.1200 0.8288 0.276 Uiso 1 1 calc R . . H58 H 0.3924 0.1767 0.8133 0.276 Uiso 1 1 calc R . . C49 C -0.1813(3) -0.2871(3) 0.6079(3) 0.0933(17) Uani 1 1 d . . . H59 H -0.1981 -0.2518 0.5734 0.112 Uiso 1 1 calc R . . H80 H -0.2339 -0.3110 0.6129 0.112 Uiso 1 1 calc R . . C50 C -0.1227(6) -0.3414(5) 0.5858(4) 0.170(4) Uani 1 1 d . . . H61 H -0.1528 -0.3622 0.5448 0.255 Uiso 1 1 calc R . . H62 H -0.1076 -0.3779 0.6186 0.255 Uiso 1 1 calc R . . H63 H -0.0708 -0.3184 0.5799 0.255 Uiso 1 1 calc R . . C51 C -0.0611(3) -0.2078(3) 0.6661(3) 0.0805(15) Uani 1 1 d . . . H64 H -0.0392 -0.1839 0.7079 0.097 Uiso 1 1 calc R . . H65 H -0.0164 -0.2404 0.6592 0.097 Uiso 1 1 calc R . . C52 C -0.0769(4) -0.1543(3) 0.6129(3) 0.0893(16) Uani 1 1 d . . . H66 H -0.0240 -0.1289 0.6134 0.134 Uiso 1 1 calc R . . H67 H -0.1207 -0.1215 0.6195 0.134 Uiso 1 1 calc R . . H68 H -0.0963 -0.1776 0.5711 0.134 Uiso 1 1 calc R . . C53 C -0.1267(5) -0.2971(3) 0.7298(3) 0.104(2) Uani 1 1 d . . . H69 H -0.1002 -0.2693 0.7684 0.125 Uiso 1 1 calc R . . H70 H -0.0865 -0.3348 0.7252 0.125 Uiso 1 1 calc R . . C54 C -0.2123(5) -0.3304(3) 0.7398(4) 0.123(3) Uani 1 1 d U . . H71 H -0.2528 -0.2933 0.7431 0.185 Uiso 1 1 calc R . . H72 H -0.2005 -0.3581 0.7795 0.185 Uiso 1 1 calc R . . H73 H -0.2367 -0.3604 0.7030 0.185 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0279(2) 0.0263(2) 0.0288(3) 0.00271(18) 0.00379(18) 0.00417(16) Zn2 0.03421(18) 0.03041(18) 0.0289(2) 0.00392(13) 0.00363(14) 0.00456(13) Zn3 0.03764(19) 0.02912(18) 0.0380(2) 0.00356(14) 0.00702(15) 0.00703(13) Zn4 0.03100(18) 0.03594(19) 0.0372(2) 0.00556(15) 0.00802(15) 0.00686(13) P1 0.0327(4) 0.0245(3) 0.0351(4) 0.0018(3) 0.0063(3) 0.0022(3) P2 0.0267(3) 0.0324(4) 0.0347(4) 0.0072(3) 0.0055(3) 0.0055(3) P3 0.0355(4) 0.0313(4) 0.0285(4) 0.0024(3) 0.0028(3) 0.0084(3) O1 0.0347(10) 0.0275(10) 0.0337(12) 0.0004(8) 0.0078(9) 0.0034(8) O2 0.0474(12) 0.0289(10) 0.0352(13) 0.0029(9) -0.0005(10) 0.0029(9) O3 0.0410(12) 0.0296(11) 0.0611(16) 0.0019(10) 0.0214(11) 0.0015(9) O4 0.0757(18) 0.0467(14) 0.0541(17) 0.0016(12) 0.0275(14) 0.0144(13) O5 0.085(2) 0.080(2) 0.058(2) -0.0302(17) 0.0134(16) 0.0046(17) O6 0.0271(9) 0.0331(10) 0.0334(12) 0.0075(8) 0.0054(8) 0.0053(8) O7 0.0316(10) 0.0320(11) 0.0586(16) 0.0015(10) 0.0092(10) 0.0045(8) O8 0.0298(10) 0.0572(14) 0.0374(13) 0.0139(11) 0.0065(9) 0.0067(9) O9 0.0488(14) 0.0530(15) 0.0643(18) 0.0256(13) 0.0237(13) 0.0097(11) O10 0.0668(17) 0.0540(16) 0.074(2) 0.0183(14) 0.0226(15) -0.0102(13) O11 0.0320(10) 0.0294(10) 0.0288(11) 0.0031(8) 0.0034(8) 0.0081(8) O12 0.0626(15) 0.0345(12) 0.0346(13) 0.0002(9) 0.0021(11) 0.0170(10) O13 0.0343(11) 0.0579(14) 0.0304(12) 0.0026(10) 0.0052(9) 0.0060(10) O14 0.0446(12) 0.0444(13) 0.0366(14) 0.0087(10) 0.0024(10) 0.0151(10) O15 0.0442(14) 0.0771(19) 0.063(2) -0.0006(15) -0.0135(13) 0.0229(13) O16 0.088(3) 0.101(3) 0.136(4) -0.046(3) 0.016(3) -0.024(2) N1 0.0334(12) 0.0296(12) 0.0310(14) -0.0023(10) 0.0001(10) 0.0048(9) N2 0.0267(11) 0.0317(12) 0.0339(14) 0.0022(10) 0.0063(10) 0.0014(9) N3 0.0326(12) 0.0289(12) 0.0301(14) 0.0033(10) 0.0012(10) 0.0020(9) N4 0.096(3) 0.106(4) 0.088(4) -0.036(3) 0.019(3) -0.030(3) N5 0.0592(19) 0.062(2) 0.057(2) -0.0044(17) 0.0016(16) 0.0241(16) C1 0.0325(14) 0.0295(14) 0.0415(19) -0.0007(13) 0.0029(13) 0.0002(11) C2 0.054(2) 0.0461(19) 0.037(2) -0.0063(16) 0.0008(15) 0.0139(16) C3 0.0451(18) 0.0395(17) 0.041(2) -0.0105(15) -0.0055(14) 0.0040(14) C4 0.0364(15) 0.0329(15) 0.0385(18) 0.0017(13) -0.0006(13) 0.0070(12) C5 0.0439(18) 0.0372(17) 0.047(2) 0.0063(15) 0.0016(15) 0.0066(13) C6 0.073(3) 0.063(3) 0.059(3) 0.021(2) 0.012(2) 0.018(2) C7 0.096(4) 0.089(4) 0.087(4) 0.049(3) 0.029(3) 0.017(3) C8 0.085(4) 0.064(3) 0.109(5) 0.046(3) 0.000(3) -0.005(3) C9 0.071(3) 0.038(2) 0.099(4) 0.009(2) -0.018(3) 0.0103(19) C10 0.132(6) 0.037(3) 0.164(8) -0.003(4) -0.028(5) 0.024(3) C11 0.190(8) 0.067(4) 0.165(9) -0.024(5) 0.001(7) 0.075(5) C12 0.169(7) 0.083(4) 0.123(6) -0.023(4) 0.015(5) 0.067(4) C13 0.099(4) 0.064(3) 0.076(4) -0.010(2) 0.012(3) 0.039(3) C14 0.057(2) 0.0378(18) 0.065(3) 0.0023(18) -0.0092(19) 0.0131(16) C15 0.0286(14) 0.0390(16) 0.0329(17) 0.0045(13) 0.0027(12) 0.0039(11) C16 0.0511(19) 0.0340(16) 0.050(2) 0.0033(15) 0.0210(16) 0.0006(14) C17 0.0360(16) 0.0370(16) 0.044(2) -0.0009(14) 0.0105(14) -0.0031(12) C18 0.0343(15) 0.0381(16) 0.0346(17) -0.0008(13) 0.0044(13) 0.0038(12) C19 0.0391(16) 0.0401(16) 0.0330(17) -0.0037(13) 0.0066(13) 0.0078(13) C20 0.069(2) 0.0449(19) 0.050(2) 0.0023(17) 0.0214(19) 0.0167(18) C21 0.093(3) 0.070(3) 0.050(3) 0.010(2) 0.015(2) 0.044(3) C22 0.061(3) 0.093(3) 0.054(3) -0.012(2) -0.001(2) 0.042(2) C23 0.0409(19) 0.073(3) 0.049(2) -0.023(2) 0.0073(16) 0.0096(17) C24 0.050(2) 0.109(4) 0.079(4) -0.032(3) 0.024(2) 0.000(2) C25 0.076(3) 0.111(4) 0.095(4) -0.041(4) 0.056(3) -0.025(3) C26 0.105(4) 0.068(3) 0.078(4) -0.006(3) 0.050(3) -0.018(3) C27 0.065(2) 0.051(2) 0.060(3) -0.0040(18) 0.030(2) -0.0001(18) C28 0.0427(17) 0.0455(18) 0.041(2) -0.0115(15) 0.0084(15) 0.0034(14) C29 0.0396(16) 0.0291(14) 0.0309(17) -0.0003(12) -0.0005(13) 0.0041(11) C30 0.0366(16) 0.0412(17) 0.041(2) 0.0107(15) 0.0026(14) 0.0023(13) C31 0.0327(15) 0.0394(16) 0.0336(18) 0.0034(13) -0.0013(13) -0.0013(12) C32 0.0385(16) 0.0384(16) 0.0357(18) 0.0045(14) 0.0022(13) -0.0046(13) C33 0.0415(17) 0.0507(19) 0.044(2) 0.0044(16) 0.0108(15) -0.0086(14) C34 0.063(3) 0.069(3) 0.069(3) 0.002(2) 0.032(2) 0.003(2) C35 0.100(4) 0.094(4) 0.102(5) -0.020(4) 0.057(4) -0.003(3) C36 0.128(5) 0.108(4) 0.053(3) -0.015(3) 0.042(3) -0.040(4) C37 0.092(3) 0.079(3) 0.041(2) 0.000(2) 0.014(2) -0.035(3) C38 0.121(5) 0.107(4) 0.039(3) 0.017(3) -0.003(3) -0.060(4) C39 0.100(4) 0.089(4) 0.082(4) 0.040(3) -0.026(3) -0.043(3) C40 0.064(3) 0.071(3) 0.089(4) 0.040(3) -0.020(2) -0.022(2) C41 0.052(2) 0.054(2) 0.061(3) 0.0236(19) 0.0028(18) -0.0082(17) C42 0.055(2) 0.058(2) 0.040(2) 0.0100(17) 0.0035(16) -0.0239(17) C43 0.322(12) 0.303(11) 0.288(12) 0.024(9) 0.076(9) -0.070(9) C44 0.262(11) 0.337(12) 0.284(11) -0.004(9) 0.068(9) -0.044(9) C45 0.218(9) 0.213(8) 0.188(8) -0.037(7) -0.013(7) 0.057(7) C46 0.114(5) 0.185(7) 0.179(7) 0.056(6) 0.077(5) 0.018(5) C47 0.149(6) 0.192(7) 0.144(7) -0.065(6) 0.027(5) 0.033(6) C48 0.197(8) 0.170(7) 0.167(8) -0.008(6) 0.005(6) 0.035(6) C49 0.072(3) 0.118(5) 0.075(4) -0.018(3) -0.014(3) 0.001(3) C50 0.151(7) 0.187(8) 0.153(8) -0.116(7) -0.003(6) 0.038(6) C51 0.055(2) 0.092(4) 0.082(4) -0.015(3) -0.010(2) 0.013(2) C52 0.076(3) 0.109(4) 0.082(4) 0.005(3) 0.016(3) 0.002(3) C53 0.159(6) 0.069(3) 0.071(4) 0.010(3) -0.001(4) 0.050(4) C54 0.151(6) 0.088(4) 0.147(6) 0.051(4) 0.068(5) 0.042(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 O6 2.110(2) . ? Zn1 O6 2.110(2) 3_656 ? Zn1 O11 2.117(2) 3_656 ? Zn1 O11 2.117(2) . ? Zn1 O1 2.125(2) 3_656 ? Zn1 O1 2.125(2) . ? Zn2 O2 1.946(2) 3_656 ? Zn2 O8 1.963(2) 3_656 ? Zn2 O14 2.095(2) . ? Zn2 O11 2.1568(19) . ? Zn2 N3 2.178(3) . ? Zn3 O7 1.958(2) . ? Zn3 O12 1.960(2) . ? Zn3 O4 2.040(3) . ? Zn3 N1 2.184(3) . ? Zn3 O1 2.200(2) . ? Zn4 O3 1.944(2) 3_656 ? Zn4 O13 1.946(2) . ? Zn4 O9 2.088(2) . ? Zn4 N2 2.159(2) . ? Zn4 O6 2.182(2) . ? P1 O3 1.514(2) . ? P1 O2 1.522(2) . ? P1 O1 1.533(2) . ? P1 C1 1.820(3) . ? P2 O8 1.516(3) . ? P2 O7 1.518(2) . ? P2 O6 1.538(2) . ? P2 C15 1.819(3) . ? P3 O12 1.510(2) . ? P3 O13 1.519(2) . ? P3 O11 1.536(2) . ? P3 C29 1.816(3) . ? O2 Zn2 1.946(2) 3_656 ? O3 Zn4 1.944(2) 3_656 ? O4 C2 1.276(5) . ? O5 C2 1.222(4) . ? O8 Zn2 1.963(2) 3_656 ? O9 C16 1.270(4) . ? O10 C16 1.234(4) . ? O14 C30 1.283(4) . ? O15 C30 1.220(4) . ? O16 H1 0.8505 . ? O16 H2 0.8511 . ? N1 C3 1.472(4) . ? N1 C1 1.486(4) . ? N1 C4 1.497(4) . ? N2 C17 1.483(4) . ? N2 C15 1.493(4) . ? N2 C18 1.506(4) . ? N3 C31 1.473(4) . ? N3 C29 1.487(4) . ? N3 C32 1.506(4) . ? N4 C45 1.451(7) . ? N4 C47 1.515(6) . ? N4 C43 1.528(8) . ? N4 H3 0.9100 . ? N5 C49 1.476(6) . ? N5 C53 1.496(6) . ? N5 C51 1.525(6) . ? N5 H4 0.9100 . ? C1 H5 0.9700 . ? C1 H6 0.9700 . ? C2 C3 1.524(5) . ? C3 H7 0.9700 . ? C3 H8 0.9700 . ? C4 C5 1.516(4) . ? C4 H9 0.9700 . ? C4 H10 0.9700 . ? C5 C6 1.377(6) . ? C5 C14 1.421(5) . ? C6 C7 1.423(6) . ? C6 H11 0.9300 . ? C7 C8 1.340(8) . ? C7 H12 0.9300 . ? C8 C9 1.398(8) . ? C8 H13 0.9300 . ? C9 C10 1.400(8) . ? C9 C14 1.452(6) . ? C10 C11 1.371(11) . ? C10 H14 0.9300 . ? C11 C12 1.383(11) . ? C11 H15 0.9300 . ? C12 C13 1.363(6) . ? C12 H16 0.9300 . ? C13 C14 1.401(7) . ? C13 H17 0.9300 . ? C15 H18 0.9700 . ? C15 H19 0.9700 . ? C16 C17 1.515(5) . ? C17 H20 0.9700 . ? C17 H21 0.9700 . ? C18 C19 1.513(4) . ? C18 H22 0.9700 . ? C18 H23 0.9700 . ? C19 C20 1.353(5) . ? C19 C28 1.435(5) . ? C20 C21 1.412(5) . ? C20 H24 0.9300 . ? C21 C22 1.336(7) . ? C21 H25 0.9300 . ? C22 C23 1.410(7) . ? C22 H26 0.9300 . ? C23 C24 1.404(7) . ? C23 C28 1.424(5) . ? C24 C25 1.362(8) . ? C24 H27 0.9300 . ? C25 C26 1.413(8) . ? C25 H28 0.9300 . ? C26 C27 1.367(6) . ? C26 H29 0.9300 . ? C27 C28 1.411(5) . ? C27 H30 0.9300 . ? C29 H31 0.9700 . ? C29 H32 0.9700 . ? C30 C31 1.519(5) . ? C31 H33 0.9700 . ? C31 H34 0.9700 . ? C32 C33 1.532(5) . ? C32 H35 0.9700 . ? C32 H36 0.9700 . ? C33 C34 1.365(6) . ? C33 C42 1.426(5) . ? C34 C35 1.406(7) . ? C34 H37 0.9300 . ? C35 C36 1.371(9) . ? C35 H38 0.9300 . ? C36 C37 1.390(8) . ? C36 H39 0.9300 . ? C37 C42 1.422(6) . ? C37 C38 1.447(8) . ? C38 C39 1.359(9) . ? C38 H40 0.9300 . ? C39 C40 1.387(9) . ? C39 H41 0.9300 . ? C40 C41 1.369(5) . ? C40 H42 0.9300 . ? C41 C42 1.420(6) . ? C41 H43 0.9300 . ? C43 C44 1.475(9) . ? C43 H44 0.9700 . ? C43 H45 0.9700 . ? C44 H46 0.9600 . ? C44 H47 0.9600 . ? C44 H48 0.9600 . ? C45 C46 1.556(8) . ? C45 H49 0.9700 . ? C45 H50 0.9700 . ? C46 H51 0.9600 . ? C46 H52 0.9600 . ? C46 H53 0.9600 . ? C47 C48 1.498(8) . ? C47 H54 0.9700 . ? C47 H55 0.9700 . ? C48 H56 0.9600 . ? C48 H57 0.9600 . ? C48 H58 0.9600 . ? C49 C50 1.517(8) . ? C49 H59 0.9700 . ? C49 H80 0.9700 . ? C50 H61 0.9600 . ? C50 H62 0.9600 . ? C50 H63 0.9600 . ? C51 C52 1.476(7) . ? C51 H64 0.9700 . ? C51 H65 0.9700 . ? C52 H66 0.9600 . ? C52 H67 0.9600 . ? C52 H68 0.9600 . ? C53 C54 1.547(9) . ? C53 H69 0.9700 . ? C53 H70 0.9700 . ? C54 H71 0.9600 . ? C54 H72 0.9600 . ? C54 H73 0.9600 . ? 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 O6 Zn1 O6 180.000(1) . 3_656 ? O6 Zn1 O11 93.91(8) . 3_656 ? O6 Zn1 O11 86.09(8) 3_656 3_656 ? O6 Zn1 O11 86.09(8) . . ? O6 Zn1 O11 93.91(8) 3_656 . ? O11 Zn1 O11 180.00(4) 3_656 . ? O6 Zn1 O1 91.76(7) . 3_656 ? O6 Zn1 O1 88.24(7) 3_656 3_656 ? O11 Zn1 O1 91.96(8) 3_656 3_656 ? O11 Zn1 O1 88.04(8) . 3_656 ? O6 Zn1 O1 88.24(7) . . ? O6 Zn1 O1 91.76(7) 3_656 . ? O11 Zn1 O1 88.04(8) 3_656 . ? O11 Zn1 O1 91.96(8) . . ? O1 Zn1 O1 180.00(12) 3_656 . ? O2 Zn2 O8 120.56(10) 3_656 3_656 ? O2 Zn2 O14 101.98(9) 3_656 . ? O8 Zn2 O14 90.67(9) 3_656 . ? O2 Zn2 O11 95.02(9) 3_656 . ? O8 Zn2 O11 91.10(9) 3_656 . ? O14 Zn2 O11 159.08(9) . . ? O2 Zn2 N3 113.66(10) 3_656 . ? O8 Zn2 N3 125.78(10) 3_656 . ? O14 Zn2 N3 77.68(9) . . ? O11 Zn2 N3 84.42(8) . . ? O7 Zn3 O12 119.22(10) . . ? O7 Zn3 O4 101.39(11) . . ? O12 Zn3 O4 93.04(11) . . ? O7 Zn3 N1 112.17(9) . . ? O12 Zn3 N1 128.57(10) . . ? O4 Zn3 N1 78.47(10) . . ? O7 Zn3 O1 94.27(9) . . ? O12 Zn3 O1 90.38(9) . . ? O4 Zn3 O1 159.76(10) . . ? N1 Zn3 O1 83.82(9) . . ? O3 Zn4 O13 119.28(10) 3_656 . ? O3 Zn4 O9 92.27(10) 3_656 . ? O13 Zn4 O9 99.39(11) . . ? O3 Zn4 N2 129.01(10) 3_656 . ? O13 Zn4 N2 111.70(9) . . ? O9 Zn4 N2 78.09(10) . . ? O3 Zn4 O6 92.24(9) 3_656 . ? O13 Zn4 O6 94.66(9) . . ? O9 Zn4 O6 160.76(9) . . ? N2 Zn4 O6 84.55(8) . . ? O3 P1 O2 113.58(15) . . ? O3 P1 O1 113.59(12) . . ? O2 P1 O1 111.93(12) . . ? O3 P1 C1 105.19(13) . . ? O2 P1 C1 108.92(13) . . ? O1 P1 C1 102.71(14) . . ? O8 P2 O7 113.68(14) . . ? O8 P2 O6 112.76(13) . . ? O7 P2 O6 112.02(12) . . ? O8 P2 C15 105.01(13) . . ? O7 P2 C15 109.74(14) . . ? O6 P2 C15 102.76(13) . . ? O12 P3 O13 113.98(14) . . ? O12 P3 O11 113.64(13) . . ? O13 P3 O11 112.18(13) . . ? O12 P3 C29 105.12(14) . . ? O13 P3 C29 108.07(14) . . ? O11 P3 C29 102.79(13) . . ? P1 O1 Zn1 126.03(12) . . ? P1 O1 Zn3 114.09(11) . . ? Zn1 O1 Zn3 117.13(9) . . ? P1 O2 Zn2 124.12(13) . 3_656 ? P1 O3 Zn4 130.28(14) . 3_656 ? C2 O4 Zn3 116.1(2) . . ? P2 O6 Zn1 125.83(12) . . ? P2 O6 Zn4 115.06(11) . . ? Zn1 O6 Zn4 118.17(9) . . ? P2 O7 Zn3 124.25(12) . . ? P2 O8 Zn2 128.15(14) . 3_656 ? C16 O9 Zn4 114.5(2) . . ? P3 O11 Zn1 126.40(11) . . ? P3 O11 Zn2 115.25(11) . . ? Zn1 O11 Zn2 117.03(9) . . ? P3 O12 Zn3 131.55(15) . . ? P3 O13 Zn4 122.38(14) . . ? C30 O14 Zn2 114.9(2) . . ? H1 O16 H2 109.8 . . ? C3 N1 C1 113.6(2) . . ? C3 N1 C4 111.2(2) . . ? C1 N1 C4 112.7(3) . . ? C3 N1 Zn3 103.4(2) . . ? C1 N1 Zn3 109.91(17) . . ? C4 N1 Zn3 105.46(18) . . ? C17 N2 C15 112.5(2) . . ? C17 N2 C18 112.1(2) . . ? C15 N2 C18 113.4(2) . . ? C17 N2 Zn4 104.91(17) . . ? C15 N2 Zn4 109.19(17) . . ? C18 N2 Zn4 104.05(17) . . ? C31 N3 C29 111.7(2) . . ? C31 N3 C32 112.5(2) . . ? C29 N3 C32 112.8(2) . . ? C31 N3 Zn2 104.73(19) . . ? C29 N3 Zn2 109.43(19) . . ? C32 N3 Zn2 105.11(18) . . ? C45 N4 C47 112.4(6) . . ? C45 N4 C43 114.8(7) . . ? C47 N4 C43 105.0(7) . . ? C45 N4 H3 108.1 . . ? C47 N4 H3 108.1 . . ? C43 N4 H3 108.1 . . ? C49 N5 C53 114.3(4) . . ? C49 N5 C51 112.7(4) . . ? C53 N5 C51 112.2(4) . . ? C49 N5 H4 105.6 . . ? C53 N5 H4 105.6 . . ? C51 N5 H4 105.6 . . ? N1 C1 P1 110.96(19) . . ? N1 C1 H5 109.4 . . ? P1 C1 H5 109.4 . . ? N1 C1 H6 109.4 . . ? P1 C1 H6 109.4 . . ? H5 C1 H6 108.0 . . ? O5 C2 O4 124.7(4) . . ? O5 C2 C3 118.9(4) . . ? O4 C2 C3 116.3(3) . . ? N1 C3 C2 111.6(3) . . ? N1 C3 H7 109.3 . . ? C2 C3 H7 109.3 . . ? N1 C3 H8 109.3 . . ? C2 C3 H8 109.3 . . ? H7 C3 H8 108.0 . . ? N1 C4 C5 116.8(3) . . ? N1 C4 H9 108.1 . . ? C5 C4 H9 108.1 . . ? N1 C4 H10 108.1 . . ? C5 C4 H10 108.1 . . ? H9 C4 H10 107.3 . . ? C6 C5 C14 119.7(4) . . ? C6 C5 C4 117.3(3) . . ? C14 C5 C4 122.9(3) . . ? C5 C6 C7 121.5(5) . . ? C5 C6 H11 119.3 . . ? C7 C6 H11 119.3 . . ? C8 C7 C6 120.1(5) . . ? C8 C7 H12 120.0 . . ? C6 C7 H12 120.0 . . ? C7 C8 C9 121.0(4) . . ? C7 C8 H13 119.5 . . ? C9 C8 H13 119.5 . . ? C8 C9 C10 120.8(6) . . ? C8 C9 C14 120.3(4) . . ? C10 C9 C14 118.9(6) . . ? C11 C10 C9 120.2(7) . . ? C11 C10 H14 119.9 . . ? C9 C10 H14 119.9 . . ? C10 C11 C12 120.7(6) . . ? C10 C11 H15 119.6 . . ? C12 C11 H15 119.6 . . ? C13 C12 C11 121.5(8) . . ? C13 C12 H16 119.3 . . ? C11 C12 H16 119.3 . . ? C12 C13 C14 120.3(6) . . ? C12 C13 H17 119.8 . . ? C14 C13 H17 119.8 . . ? C13 C14 C5 124.2(4) . . ? C13 C14 C9 118.3(4) . . ? C5 C14 C9 117.5(4) . . ? N2 C15 P2 111.61(19) . . ? N2 C15 H18 109.3 . . ? P2 C15 H18 109.3 . . ? N2 C15 H19 109.3 . . ? P2 C15 H19 109.3 . . ? H18 C15 H19 108.0 . . ? O10 C16 O9 123.4(3) . . ? O10 C16 C17 119.3(3) . . ? O9 C16 C17 117.2(3) . . ? N2 C17 C16 111.9(3) . . ? N2 C17 H20 109.2 . . ? C16 C17 H20 109.2 . . ? N2 C17 H21 109.2 . . ? C16 C17 H21 109.2 . . ? H20 C17 H21 107.9 . . ? N2 C18 C19 115.7(2) . . ? N2 C18 H22 108.4 . . ? C19 C18 H22 108.4 . . ? N2 C18 H23 108.4 . . ? C19 C18 H23 108.4 . . ? H22 C18 H23 107.4 . . ? C20 C19 C28 119.4(3) . . ? C20 C19 C18 118.3(3) . . ? C28 C19 C18 122.2(3) . . ? C19 C20 C21 122.0(4) . . ? C19 C20 H24 119.0 . . ? C21 C20 H24 119.0 . . ? C22 C21 C20 119.5(4) . . ? C22 C21 H25 120.2 . . ? C20 C21 H25 120.2 . . ? C21 C22 C23 121.7(4) . . ? C21 C22 H26 119.2 . . ? C23 C22 H26 119.2 . . ? C24 C23 C22 121.0(4) . . ? C24 C23 C28 119.9(4) . . ? C22 C23 C28 119.1(4) . . ? C25 C24 C23 120.3(5) . . ? C25 C24 H27 119.8 . . ? C23 C24 H27 119.8 . . ? C24 C25 C26 121.2(5) . . ? C24 C25 H28 119.4 . . ? C26 C25 H28 119.4 . . ? C27 C26 C25 118.6(5) . . ? C27 C26 H29 120.7 . . ? C25 C26 H29 120.7 . . ? C26 C27 C28 122.5(4) . . ? C26 C27 H30 118.7 . . ? C28 C27 H30 118.7 . . ? C27 C28 C23 117.3(4) . . ? C27 C28 C19 124.5(3) . . ? C23 C28 C19 118.1(3) . . ? N3 C29 P3 111.2(2) . . ? N3 C29 H31 109.4 . . ? P3 C29 H31 109.4 . . ? N3 C29 H32 109.4 . . ? P3 C29 H32 109.4 . . ? H31 C29 H32 108.0 . . ? O15 C30 O14 125.1(3) . . ? O15 C30 C31 118.3(3) . . ? O14 C30 C31 116.5(3) . . ? N3 C31 C30 112.3(3) . . ? N3 C31 H33 109.1 . . ? C30 C31 H33 109.1 . . ? N3 C31 H34 109.1 . . ? C30 C31 H34 109.1 . . ? H33 C31 H34 107.9 . . ? N3 C32 C33 116.4(3) . . ? N3 C32 H35 108.2 . . ? C33 C32 H35 108.2 . . ? N3 C32 H36 108.2 . . ? C33 C32 H36 108.2 . . ? H35 C32 H36 107.3 . . ? C34 C33 C42 119.8(4) . . ? C34 C33 C32 118.6(4) . . ? C42 C33 C32 121.6(3) . . ? C33 C34 C35 121.3(5) . . ? C33 C34 H37 119.3 . . ? C35 C34 H37 119.3 . . ? C36 C35 C34 119.0(5) . . ? C36 C35 H38 120.5 . . ? C34 C35 H38 120.5 . . ? C35 C36 C37 122.2(5) . . ? C35 C36 H39 118.9 . . ? C37 C36 H39 118.9 . . ? C36 C37 C42 118.7(5) . . ? C36 C37 C38 122.3(5) . . ? C42 C37 C38 119.0(5) . . ? C39 C38 C37 120.4(5) . . ? C39 C38 H40 119.8 . . ? C37 C38 H40 119.8 . . ? C38 C39 C40 120.9(5) . . ? C38 C39 H41 119.6 . . ? C40 C39 H41 119.6 . . ? C41 C40 C39 120.2(6) . . ? C41 C40 H42 119.9 . . ? C39 C40 H42 119.9 . . ? C40 C41 C42 122.2(5) . . ? C40 C41 H43 118.9 . . ? C42 C41 H43 118.9 . . ? C41 C42 C37 117.3(4) . . ? C41 C42 C33 123.8(4) . . ? C37 C42 C33 118.9(4) . . ? C44 C43 N4 109.8(11) . . ? C44 C43 H44 109.7 . . ? N4 C43 H44 109.7 . . ? C44 C43 H45 109.7 . . ? N4 C43 H45 109.7 . . ? H44 C43 H45 108.2 . . ? C43 C44 H46 109.5 . . ? C43 C44 H47 109.5 . . ? H46 C44 H47 109.5 . . ? C43 C44 H48 109.5 . . ? H46 C44 H48 109.5 . . ? H47 C44 H48 109.5 . . ? N4 C45 C46 105.3(7) . . ? N4 C45 H49 110.7 . . ? C46 C45 H49 110.7 . . ? N4 C45 H50 110.7 . . ? C46 C45 H50 110.7 . . ? H49 C45 H50 108.8 . . ? C45 C46 H51 109.5 . . ? C45 C46 H52 109.5 . . ? H51 C46 H52 109.5 . . ? C45 C46 H53 109.5 . . ? H51 C46 H53 109.5 . . ? H52 C46 H53 109.5 . . ? C48 C47 N4 119.0(7) . . ? C48 C47 H54 107.6 . . ? N4 C47 H54 107.6 . . ? C48 C47 H55 107.6 . . ? N4 C47 H55 107.6 . . ? H54 C47 H55 107.0 . . ? C47 C48 H56 109.5 . . ? C47 C48 H57 109.5 . . ? H56 C48 H57 109.5 . . ? C47 C48 H58 109.5 . . ? H56 C48 H58 109.5 . . ? H57 C48 H58 109.5 . . ? N5 C49 C50 114.7(5) . . ? N5 C49 H59 108.6 . . ? C50 C49 H59 108.6 . . ? N5 C49 H80 108.6 . . ? C50 C49 H80 108.6 . . ? H59 C49 H80 107.6 . . ? C49 C50 H61 109.5 . . ? C49 C50 H62 109.5 . . ? H61 C50 H62 109.5 . . ? C49 C50 H63 109.5 . . ? H61 C50 H63 109.5 . . ? H62 C50 H63 109.5 . . ? C52 C51 N5 113.6(4) . . ? C52 C51 H64 108.8 . . ? N5 C51 H64 108.8 . . ? C52 C51 H65 108.8 . . ? N5 C51 H65 108.8 . . ? H64 C51 H65 107.7 . . ? C51 C52 H66 109.5 . . ? C51 C52 H67 109.5 . . ? H66 C52 H67 109.5 . . ? C51 C52 H68 109.5 . . ? H66 C52 H68 109.5 . . ? H67 C52 H68 109.5 . . ? N5 C53 C54 111.8(5) . . ? N5 C53 H69 109.3 . . ? C54 C53 H69 109.3 . . ? N5 C53 H70 109.3 . . ? C54 C53 H70 109.3 . . ? H69 C53 H70 107.9 . . ? C53 C54 H71 109.5 . . ? C53 C54 H72 109.5 . . ? H71 C54 H72 109.5 . . ? C53 C54 H73 109.5 . . ? H71 C54 H73 109.5 . . ? H72 C54 H73 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N4 H3 O10 0.91 1.99 2.868(5) 160.5 2_556 N5 H4 O14 0.91 1.88 2.784(4) 171.9 1_455 _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 1.070 _refine_diff_density_min -0.503 _refine_diff_density_rms 0.103 _database_code_depnum_ccdc_archive 'CCDC 958269'