# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Jubaraj Baruah' _publ_contact_author_email JUBA@IITG.ERNET.IN _publ_section_title ; Coordination polymers of zinc with (4-carboxymethoxy-2,3-bis-phenylsulfanylnaphthalene-1-yloxy)acetic acid ; loop_ _publ_author_name 'Jubaraj Baruah' 'W Marjit Singh' # Attachment '2ch3znpy1.cif' data_2ch3znpy1 _database_code_depnum_ccdc_archive 'CCDC 699021' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H27 N O6 S2 Zn' _chemical_formula_weight 663.05 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.8512(5) _cell_length_b 12.7441(6) _cell_length_c 13.0361(6) _cell_angle_alpha 63.497(2) _cell_angle_beta 65.669(2) _cell_angle_gamma 68.600(2) _cell_volume 1565.42(12) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2540 _cell_measurement_theta_min 3.01 _cell_measurement_theta_max 20.17 _exptl_crystal_description blocks _exptl_crystal_colour colorless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.407 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 684 _exptl_absorpt_coefficient_mu 0.963 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16117 _diffrn_reflns_av_R_equivalents 0.0472 _diffrn_reflns_av_sigmaI/netI 0.1122 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 28.24 _reflns_number_total 7553 _reflns_number_gt 3604 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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. One pyridine was disordered.It was approximated by two orientations, (i) N(1) and C(27) to C(31) (ii) N(1)'and C(27)' to C(31)' [with their hydrogens],having occupancies of 1/2. Another sulphenyl toluene ring was also disordered.It was approximated by two orientations,(i) C(12) and C(13) (ii) C(12)'and C(13)' [with their hydrogens]having occupancies of 1/2. The atoms are refine isotropically. ; _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^)+(0.1030P)^2^+0.4912P] 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 7553 _refine_ls_number_parameters 337 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1677 _refine_ls_R_factor_gt 0.0727 _refine_ls_wR_factor_ref 0.2204 _refine_ls_wR_factor_gt 0.1775 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.8318(8) -0.0277(10) 0.3842(10) 0.066(10) Uiso 0.461(7) 1 d PG A 1 C27 C 0.9146(13) -0.1005(11) 0.3175(12) 0.103(6) Uiso 0.461(7) 1 d PG A 1 H27 H 0.8830 -0.1429 0.2969 0.123 Uiso 0.461(7) 1 calc PR A 1 C28 C 1.0448(12) -0.1100(11) 0.2817(12) 0.122(7) Uiso 0.461(7) 1 d PG A 1 H28 H 1.1002 -0.1588 0.2372 0.146 Uiso 0.461(7) 1 calc PR A 1 C29 C 1.0920(8) -0.0467(11) 0.3126(12) 0.102(11) Uiso 0.461(7) 1 d PG A 1 H29 H 1.1791 -0.0530 0.2886 0.122 Uiso 0.461(7) 1 calc PR A 1 C30 C 1.0092(11) 0.0262(11) 0.3792(11) 0.092(5) Uiso 0.461(7) 1 d PG A 1 H30 H 1.0408 0.0686 0.3998 0.111 Uiso 0.461(7) 1 calc PR A 1 C31 C 0.8790(10) 0.0357(10) 0.4150(10) 0.078(5) Uiso 0.461(7) 1 d PG A 1 H31 H 0.8236 0.0844 0.4595 0.094 Uiso 0.461(7) 1 calc PR A 1 N1' N 0.8280(6) -0.0228(6) 0.3937(7) 0.043(6) Uiso 0.539(7) 1 d PG A 2 C27' C 0.9100(7) -0.1348(5) 0.4220(7) 0.064(3) Uiso 0.539(7) 1 d PG A 2 H27' H 0.8784 -0.2043 0.4620 0.076 Uiso 0.539(7) 1 calc PR A 2 C28' C 1.0394(7) -0.1431(6) 0.3904(9) 0.087(4) Uiso 0.539(7) 1 d PG A 2 H28' H 1.0943 -0.2180 0.4093 0.104 Uiso 0.539(7) 1 calc PR A 2 C29' C 1.0867(5) -0.0393(9) 0.3305(10) 0.118(11) Uiso 0.539(7) 1 d PG A 2 H29' H 1.1733 -0.0448 0.3094 0.141 Uiso 0.539(7) 1 calc PR A 2 C30' C 1.0047(8) 0.0727(7) 0.3023(9) 0.089(4) Uiso 0.539(7) 1 d PG A 2 H30' H 1.0363 0.1422 0.2622 0.106 Uiso 0.539(7) 1 calc PR A 2 C31' C 0.8753(7) 0.0810(5) 0.3338(7) 0.065(3) Uiso 0.539(7) 1 d PG A 2 H31' H 0.8204 0.1559 0.3149 0.078 Uiso 0.539(7) 1 calc PR A 2 C11 C 0.7881(4) 0.3112(5) 0.9371(5) 0.0636(16) Uiso 1 1 d G . . C12 C 0.8049(6) 0.2521(7) 1.0505(4) 0.075(4) Uiso 0.461(7) 1 d PG A 1 H12 H 0.7355 0.2536 1.1185 0.090 Uiso 0.461(7) 1 calc PR A 1 C13 C 0.9253(7) 0.1907(8) 1.0623(5) 0.105(6) Uiso 0.461(7) 1 d PG A 1 H13 H 0.9365 0.1512 1.1382 0.126 Uiso 0.461(7) 1 calc PR A 1 C14 C 1.0290(5) 0.1884(6) 0.9607(7) 0.112(3) Uiso 1 1 d G A . C16 C 1.0122(4) 0.2475(6) 0.8473(5) 0.119(3) Uani 1 1 d G A . H16 H 1.0816 0.2460 0.7793 0.142 Uiso 1 1 calc R . . C17 C 0.8917(5) 0.3089(5) 0.8355(4) 0.131(4) Uani 1 1 d G A . H17 H 0.8805 0.3484 0.7596 0.158 Uiso 1 1 calc R . . C12' C 0.7945(13) 0.1908(12) 1.0366(12) 0.081(4) Uiso 0.539(7) 1 d P A 2 H12' H 0.7204 0.1659 1.0909 0.097 Uiso 0.539(7) 1 calc PR A 2 C13' C 0.9156(14) 0.1151(14) 1.0468(13) 0.089(4) Uiso 0.539(7) 1 d P A 2 H13' H 0.9283 0.0346 1.0960 0.107 Uiso 0.539(7) 1 calc PR A 2 C1 C 0.6744(5) 0.3403(6) 0.4767(6) 0.0611(16) Uani 1 1 d . . . H1 H 0.6619 0.2716 0.4783 0.073 Uiso 1 1 calc R . . C2 C 0.7088(6) 0.4306(7) 0.3697(6) 0.078(2) Uani 1 1 d . . . H2 H 0.7210 0.4213 0.2988 0.093 Uiso 1 1 calc R . . C3 C 0.7261(6) 0.5369(6) 0.3635(6) 0.075(2) Uani 1 1 d . . . H3 H 0.7504 0.5961 0.2893 0.090 Uiso 1 1 calc R . . C4 C 0.7074(6) 0.5530(6) 0.4656(6) 0.0637(17) Uani 1 1 d . . . H4 H 0.7176 0.6241 0.4611 0.076 Uiso 1 1 calc R . . C5 C 0.6722(5) 0.4621(5) 0.5806(5) 0.0481(13) Uani 1 1 d . . . C6 C 0.6560(5) 0.4727(4) 0.6899(6) 0.0486(14) Uani 1 1 d . A . C7 C 0.6324(5) 0.3812(5) 0.7983(5) 0.0482(13) Uani 1 1 d . . . C8 C 0.6101(5) 0.2733(4) 0.8046(5) 0.0493(14) Uani 1 1 d . A . C9 C 0.6243(5) 0.2629(4) 0.6992(5) 0.0460(13) Uani 1 1 d . . . C10 C 0.6582(5) 0.3530(5) 0.5849(5) 0.0493(13) Uani 1 1 d . A . C15 C 1.1632(8) 0.1027(12) 0.9688(10) 0.186(6) Uani 1 1 d . . . H15A H 1.1606 0.0605 1.0516 0.279 Uiso 1 1 calc R A . H15B H 1.2265 0.1497 0.9288 0.279 Uiso 1 1 calc R . . H15C H 1.1839 0.0457 0.9309 0.279 Uiso 1 1 calc R . . C18 C 0.4162(5) 0.2299(5) 1.0134(5) 0.0528(14) Uani 1 1 d . A . C19 C 0.3416(6) 0.3320(6) 0.9551(7) 0.082(2) Uani 1 1 d . . . H19 H 0.3697 0.3686 0.8721 0.098 Uiso 1 1 calc R . . C20 C 0.2236(8) 0.3801(7) 1.0213(10) 0.111(3) Uani 1 1 d . . . H20 H 0.1743 0.4495 0.9805 0.133 Uiso 1 1 calc R . . C21 C 0.1756(8) 0.3309(9) 1.1441(10) 0.099(3) Uani 1 1 d . . . C22 C 0.0471(10) 0.3875(10) 1.2137(11) 0.173(5) Uani 1 1 d . . . H22A H -0.0191 0.3738 1.1999 0.260 Uiso 1 1 calc R . . H22B H 0.0399 0.4724 1.1873 0.260 Uiso 1 1 calc R . . H22C H 0.0392 0.3521 1.2979 0.260 Uiso 1 1 calc R . . C23 C 0.2526(9) 0.2281(9) 1.1996(8) 0.102(3) Uani 1 1 d . . . H23 H 0.2237 0.1898 1.2822 0.123 Uiso 1 1 calc R . . C24 C 0.3702(7) 0.1807(7) 1.1367(6) 0.078(2) Uani 1 1 d . . . H24 H 0.4207 0.1134 1.1782 0.094 Uiso 1 1 calc R . . C25 C 0.4879(5) 0.1526(5) 0.7206(6) 0.0564(15) Uani 1 1 d . . . H25A H 0.4362 0.2336 0.6992 0.068 Uiso 1 1 calc R A . H25B H 0.4515 0.1109 0.8055 0.068 Uiso 1 1 calc R . . C26 C 0.4858(6) 0.0879(4) 0.6481(5) 0.0467(13) Uani 1 1 d . . . C32 C 0.5373(6) -0.2168(5) 0.6441(5) 0.0503(14) Uani 1 1 d . . . C33 C 0.5557(6) 0.6545(4) 0.7310(6) 0.0603(16) Uani 1 1 d . . . H33A H 0.5583 0.6535 0.8048 0.072 Uiso 1 1 calc R . . H33B H 0.4841 0.6221 0.7504 0.072 Uiso 1 1 calc R . . O1 O 0.6132(3) 0.1579(3) 0.6995(4) 0.0538(10) Uani 1 1 d . A . O2 O 0.5864(4) 0.0563(3) 0.5760(4) 0.0604(11) Uani 1 1 d . . . O3 O 0.6303(4) -0.1783(3) 0.5680(4) 0.0597(11) Uani 1 1 d . . . O4 O 0.6210(4) -0.0749(4) 0.3323(4) 0.0663(11) Uani 1 1 d . . . O5 O 0.5765(4) 0.1607(3) 0.3377(4) 0.0664(12) Uani 1 1 d . . . O6 O 0.6710(3) 0.5798(3) 0.6812(4) 0.0597(11) Uani 1 1 d . . . S1 S 0.63169(15) 0.39207(14) 0.92986(16) 0.0613(4) Uani 1 1 d . A . S2 S 0.56642(15) 0.15726(13) 0.94138(15) 0.0607(4) Uani 1 1 d . . . Zn1 Zn 0.63977(5) -0.01089(5) 0.44020(6) 0.0451(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C16 0.061(5) 0.169(9) 0.096(7) -0.029(6) -0.008(5) -0.032(5) C17 0.059(5) 0.193(10) 0.077(6) -0.001(6) -0.015(4) -0.025(6) C1 0.056(4) 0.076(4) 0.062(4) -0.038(4) -0.020(3) -0.006(3) C2 0.071(5) 0.093(5) 0.053(4) -0.024(4) -0.018(4) -0.003(4) C3 0.077(5) 0.069(4) 0.051(4) -0.009(4) -0.016(4) -0.005(3) C4 0.056(4) 0.058(4) 0.062(4) -0.016(3) -0.012(3) -0.009(3) C5 0.038(3) 0.050(3) 0.051(4) -0.022(3) -0.010(3) -0.003(2) C6 0.043(3) 0.036(3) 0.068(4) -0.020(3) -0.018(3) -0.006(2) C7 0.051(3) 0.040(3) 0.061(4) -0.025(3) -0.023(3) -0.002(2) C8 0.049(3) 0.039(3) 0.063(4) -0.020(3) -0.022(3) -0.004(2) C9 0.042(3) 0.040(3) 0.061(4) -0.026(3) -0.016(3) -0.003(2) C10 0.044(3) 0.053(3) 0.051(4) -0.021(3) -0.019(3) -0.003(2) C15 0.056(6) 0.277(15) 0.152(10) -0.062(11) -0.036(6) 0.031(7) C18 0.059(4) 0.051(3) 0.055(4) -0.015(3) -0.019(3) -0.020(3) C19 0.062(4) 0.076(5) 0.077(5) -0.018(4) -0.016(4) 0.000(3) C20 0.077(6) 0.082(6) 0.139(9) -0.028(6) -0.026(6) -0.002(4) C21 0.066(5) 0.111(7) 0.115(8) -0.057(6) 0.011(5) -0.036(5) C22 0.094(8) 0.180(12) 0.210(13) -0.108(11) 0.043(8) -0.044(7) C23 0.089(6) 0.147(9) 0.073(6) -0.042(6) 0.000(5) -0.051(6) C24 0.075(5) 0.089(5) 0.055(4) -0.007(4) -0.016(4) -0.027(4) C25 0.046(3) 0.062(4) 0.072(4) -0.037(3) -0.014(3) -0.011(3) C26 0.053(3) 0.035(3) 0.049(3) -0.010(3) -0.018(3) -0.010(2) C32 0.057(4) 0.046(3) 0.054(4) -0.026(3) -0.014(3) -0.011(3) C33 0.062(4) 0.039(3) 0.070(4) -0.022(3) -0.011(3) -0.007(3) O1 0.045(2) 0.051(2) 0.077(3) -0.035(2) -0.021(2) -0.0041(16) O2 0.061(3) 0.059(2) 0.069(3) -0.036(2) -0.014(2) -0.0110(19) O3 0.058(3) 0.044(2) 0.065(3) -0.011(2) -0.014(2) -0.0164(18) O4 0.060(3) 0.082(3) 0.074(3) -0.037(3) -0.014(2) -0.027(2) O5 0.057(3) 0.052(2) 0.074(3) -0.019(2) -0.015(2) -0.0036(19) O6 0.051(2) 0.045(2) 0.082(3) -0.028(2) -0.011(2) -0.0114(17) S1 0.0667(10) 0.0589(9) 0.0714(11) -0.0363(9) -0.0305(9) 0.0009(7) S2 0.0715(10) 0.0416(8) 0.0601(10) -0.0114(7) -0.0240(8) -0.0064(7) Zn1 0.0352(3) 0.0470(4) 0.0559(4) -0.0231(3) -0.0092(3) -0.0106(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C27 1.3900 . ? N1 C31 1.3900 . ? N1 Zn1 2.042(8) . ? C27 C28 1.3900 . ? C28 C29 1.3900 . ? C29 C30 1.3900 . ? C30 C31 1.3900 . ? N1' C27' 1.3900 . ? N1' C31' 1.3900 . ? N1' Zn1 2.021(6) . ? C27' C28' 1.3900 . ? C28' C29' 1.3900 . ? C29' C30' 1.3900 . ? C30' C31' 1.3900 . ? C11 C12 1.3900 . ? C11 C17 1.3900 . ? C11 C12' 1.504(14) . ? C11 S1 1.780(4) . ? C12 C13 1.3900 . ? C13 C14 1.3900 . ? C14 C16 1.3900 . ? C14 C15 1.582(9) . ? C14 C13' 1.636(16) . ? C16 C17 1.3900 . ? C12' C13' 1.428(18) . ? C1 C2 1.371(9) . ? C1 C10 1.418(8) . ? C2 C3 1.406(9) . ? C3 C4 1.353(9) . ? C4 C5 1.432(8) . ? C5 C6 1.419(8) . ? C5 C10 1.434(7) . ? C6 C7 1.370(8) . ? C6 O6 1.388(6) . ? C7 C8 1.453(7) . ? C7 S1 1.778(6) . ? C8 C9 1.375(7) . ? C8 S2 1.755(6) . ? C9 O1 1.389(6) . ? C9 C10 1.420(8) . ? C18 C19 1.373(8) . ? C18 C24 1.378(8) . ? C18 S2 1.762(6) . ? C19 C20 1.389(10) . ? C20 C21 1.375(12) . ? C21 C23 1.378(12) . ? C21 C22 1.519(12) . ? C23 C24 1.365(11) . ? C25 O1 1.416(6) . ? C25 C26 1.519(7) . ? C26 O2 1.237(6) . ? C26 O4 1.242(6) 2_656 ? C32 O3 1.224(6) . ? C32 O5 1.254(6) 2_656 ? C32 C33 1.519(7) 1_545 ? C33 O6 1.437(6) . ? C33 C32 1.519(7) 1_565 ? O2 Zn1 2.074(4) . ? O3 Zn1 2.046(4) . ? O4 C26 1.242(6) 2_656 ? O4 Zn1 2.027(4) . ? O5 C32 1.254(6) 2_656 ? O5 Zn1 2.037(4) . ? Zn1 Zn1 2.9904(12) 2_656 ? 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 C27 N1 C31 120.0 . . ? C27 N1 Zn1 121.8(7) . . ? C31 N1 Zn1 118.2(7) . . ? C28 C27 N1 120.0 . . ? C27 C28 C29 120.0 . . ? C30 C29 C28 120.0 . . ? C31 C30 C29 120.0 . . ? C30 C31 N1 120.0 . . ? C27' N1' C31' 120.0 . . ? C27' N1' Zn1 120.0(4) . . ? C31' N1' Zn1 120.0(4) . . ? C28' C27' N1' 120.0 . . ? C27' C28' C29' 120.0 . . ? C30' C29' C28' 120.0 . . ? C31' C30' C29' 120.0 . . ? C30' C31' N1' 120.0 . . ? C12 C11 C17 120.0 . . ? C12 C11 C12' 37.4(5) . . ? C17 C11 C12' 111.4(6) . . ? C12 C11 S1 117.0(3) . . ? C17 C11 S1 122.9(3) . . ? C12' C11 S1 114.5(6) . . ? C11 C12 C13 120.0 . . ? C12 C13 C14 120.0 . . ? C16 C14 C13 120.0 . . ? C16 C14 C15 117.1(6) . . ? C13 C14 C15 122.1(6) . . ? C16 C14 C13' 107.3(6) . . ? C13 C14 C13' 42.5(6) . . ? C15 C14 C13' 110.8(8) . . ? C14 C16 C17 120.0 . . ? C16 C17 C11 120.0 . . ? C13' C12' C11 119.4(12) . . ? C12' C13' C14 111.1(11) . . ? C2 C1 C10 119.1(6) . . ? C1 C2 C3 122.2(7) . . ? C4 C3 C2 119.9(7) . . ? C3 C4 C5 120.9(6) . . ? C6 C5 C4 123.1(5) . . ? C6 C5 C10 118.5(5) . . ? C4 C5 C10 118.4(5) . . ? C7 C6 O6 121.0(5) . . ? C7 C6 C5 122.5(5) . . ? O6 C6 C5 116.4(5) . . ? C6 C7 C8 119.3(5) . . ? C6 C7 S1 120.8(4) . . ? C8 C7 S1 119.9(4) . . ? C9 C8 C7 118.3(5) . . ? C9 C8 S2 119.5(4) . . ? C7 C8 S2 122.2(4) . . ? C8 C9 O1 120.5(5) . . ? C8 C9 C10 123.1(5) . . ? O1 C9 C10 116.3(5) . . ? C1 C10 C9 122.5(5) . . ? C1 C10 C5 119.4(5) . . ? C9 C10 C5 118.0(5) . . ? C19 C18 C24 117.8(6) . . ? C19 C18 S2 124.4(5) . . ? C24 C18 S2 117.8(5) . . ? C18 C19 C20 119.3(7) . . ? C21 C20 C19 123.6(8) . . ? C20 C21 C23 115.6(8) . . ? C20 C21 C22 122.0(10) . . ? C23 C21 C22 122.4(10) . . ? C24 C23 C21 121.9(8) . . ? C23 C24 C18 121.9(7) . . ? O1 C25 C26 111.4(4) . . ? O2 C26 O4 127.2(5) . 2_656 ? O2 C26 C25 118.5(5) . . ? O4 C26 C25 114.3(5) 2_656 . ? O3 C32 O5 127.4(6) . 2_656 ? O3 C32 C33 119.3(5) . 1_545 ? O5 C32 C33 113.3(5) 2_656 1_545 ? O6 C33 C32 111.6(5) . 1_565 ? C9 O1 C25 115.0(4) . . ? C26 O2 Zn1 136.5(4) . . ? C32 O3 Zn1 129.4(4) . . ? C26 O4 Zn1 117.6(4) 2_656 . ? C32 O5 Zn1 124.9(4) 2_656 . ? C6 O6 C33 114.4(4) . . ? C7 S1 C11 101.4(3) . . ? C8 S2 C18 101.6(3) . . ? N1' Zn1 O4 105.5(3) . . ? N1' Zn1 O5 102.8(2) . . ? O4 Zn1 O5 90.31(18) . . ? N1' Zn1 N1 4.1(5) . . ? O4 Zn1 N1 101.4(4) . . ? O5 Zn1 N1 103.0(3) . . ? N1' Zn1 O3 98.9(2) . . ? O4 Zn1 O3 86.23(17) . . ? O5 Zn1 O3 158.10(16) . . ? N1 Zn1 O3 98.9(3) . . ? N1' Zn1 O2 96.2(3) . . ? O4 Zn1 O2 158.32(16) . . ? O5 Zn1 O2 86.44(17) . . ? N1 Zn1 O2 100.3(4) . . ? O3 Zn1 O2 88.84(16) . . ? N1' Zn1 Zn1 166.9(3) . 2_656 ? O4 Zn1 Zn1 87.01(12) . 2_656 ? O5 Zn1 Zn1 80.69(12) . 2_656 ? N1 Zn1 Zn1 170.8(3) . 2_656 ? O3 Zn1 Zn1 77.54(11) . 2_656 ? O2 Zn1 Zn1 71.32(11) . 2_656 ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 28.24 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 1.018 _refine_diff_density_min -0.684 _refine_diff_density_rms 0.088 # Attachment '2tpZn.cif' data_2tpzn _database_code_depnum_ccdc_archive 'CCDC 699022' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H25 N O8 S2 Zn' _chemical_formula_weight 644.99 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' S S 0.1246 0.1234 '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 P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.9449(3) _cell_length_b 10.8468(3) _cell_length_c 25.1629(8) _cell_angle_alpha 90.00 _cell_angle_beta 97.845(2) _cell_angle_gamma 90.00 _cell_volume 2959.31(15) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description blocks _exptl_crystal_colour colorless _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.448 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1328 _exptl_absorpt_coefficient_mu 1.021 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24505 _diffrn_reflns_av_R_equivalents 0.0291 _diffrn_reflns_av_sigmaI/netI 0.0267 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 25.50 _reflns_number_total 5482 _reflns_number_gt 4371 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0694P)^2^+1.5143P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5482 _refine_ls_number_parameters 376 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0513 _refine_ls_R_factor_gt 0.0381 _refine_ls_wR_factor_ref 0.1173 _refine_ls_wR_factor_gt 0.1074 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _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 0.36516(3) 0.46697(3) -0.011058(12) 0.03327(12) Uani 1 1 d . . . S1 S 0.37074(8) 0.41988(8) 0.34748(3) 0.0517(2) Uani 1 1 d . . . S2 S 0.38100(7) 0.38474(7) 0.22140(3) 0.0441(2) Uani 1 1 d . . . O1 O 0.33112(19) 0.6863(2) 0.37779(7) 0.0424(5) Uani 1 1 d . . . O2 O 0.32794(17) 0.61737(19) 0.15921(7) 0.0386(5) Uani 1 1 d . . . O4 O 0.3648(2) 0.5549(2) 0.05985(8) 0.0475(5) Uani 1 1 d . . . O5 O 0.18699(18) 0.4354(2) -0.03374(8) 0.0429(5) Uani 1 1 d . . . O3 O 0.56500(19) 0.6032(2) 0.07600(8) 0.0498(6) Uani 1 1 d . . . O6 O 0.3762(2) 0.8636(2) 0.45123(9) 0.0529(6) Uani 1 1 d . . . O7 O 0.5758(2) 0.8149(2) 0.46749(9) 0.0561(6) Uani 1 1 d . . . N1 N 0.0312(2) 0.3930(2) -0.09958(10) 0.0443(6) Uani 1 1 d . . . C2 C 0.4500(3) 0.6880(3) 0.40913(13) 0.0529(9) Uani 1 1 d . . . H2A H 0.5128 0.6885 0.3854 0.063 Uiso 1 1 calc R . . H2B H 0.4606 0.6136 0.4306 0.063 Uiso 1 1 calc R . . C3 C 0.3308(2) 0.6661(3) 0.32377(11) 0.0344(6) Uani 1 1 d . . . C4 C 0.3457(3) 0.5491(3) 0.30410(11) 0.0356(6) Uani 1 1 d . . . C5 C 0.3472(3) 0.5321(3) 0.24767(11) 0.0347(6) Uani 1 1 d . . . C6 C 0.3280(2) 0.6319(3) 0.21383(10) 0.0337(6) Uani 1 1 d . . . C7 C 0.3059(2) 0.7524(3) 0.23313(11) 0.0346(6) Uani 1 1 d . . . C8 C 0.2853(3) 0.8552(3) 0.19880(13) 0.0472(8) Uani 1 1 d . . . H8 H 0.2824 0.8448 0.1620 0.057 Uiso 1 1 calc R . . C9 C 0.2696(3) 0.9699(3) 0.21919(15) 0.0552(9) Uani 1 1 d . . . H9 H 0.2560 1.0370 0.1961 0.066 Uiso 1 1 calc R . . C10 C 0.2738(3) 0.9873(3) 0.27480(14) 0.0503(8) Uani 1 1 d . . . H10 H 0.2636 1.0659 0.2883 0.060 Uiso 1 1 calc R . . C11 C 0.2925(3) 0.8905(3) 0.30892(13) 0.0429(7) Uani 1 1 d . . . H11 H 0.2952 0.9034 0.3456 0.051 Uiso 1 1 calc R . . C12 C 0.3081(2) 0.7692(3) 0.28919(11) 0.0332(6) Uani 1 1 d . . . C18 C 0.2497(3) 0.4264(3) 0.38766(13) 0.0493(8) Uani 1 1 d . . . C19 C 0.2778(5) 0.3820(3) 0.43977(15) 0.0690(11) Uani 1 1 d . . . H19 H 0.3580 0.3583 0.4527 0.083 Uiso 1 1 calc R . . C20 C 0.1868(7) 0.3733(4) 0.4719(2) 0.0988(19) Uani 1 1 d . . . H20 H 0.2057 0.3443 0.5068 0.119 Uiso 1 1 calc R . . C21 C 0.0684(6) 0.4069(5) 0.4530(3) 0.102(2) Uani 1 1 d . . . H21 H 0.0066 0.3982 0.4747 0.123 Uiso 1 1 calc R . . C22 C 0.0407(5) 0.4537(4) 0.4017(3) 0.0899(16) Uani 1 1 d . . . H22 H -0.0391 0.4799 0.3894 0.108 Uiso 1 1 calc R . . C23 C 0.1314(4) 0.4618(3) 0.36849(18) 0.0646(10) Uani 1 1 d . . . H23 H 0.1124 0.4910 0.3336 0.077 Uiso 1 1 calc R . . C24 C 0.2310(3) 0.3390(3) 0.19135(13) 0.0408(7) Uani 1 1 d . . . C25 C 0.1391(3) 0.3169(3) 0.22302(16) 0.0573(9) Uani 1 1 d . . . H25 H 0.1562 0.3245 0.2601 0.069 Uiso 1 1 calc R . . C26 C 0.0227(4) 0.2839(4) 0.19973(19) 0.0718(11) Uani 1 1 d . . . H26 H -0.0390 0.2718 0.2212 0.086 Uiso 1 1 calc R . . C27 C -0.0032(4) 0.2686(4) 0.1460(2) 0.0778(13) Uani 1 1 d . . . H27 H -0.0820 0.2451 0.1309 0.093 Uiso 1 1 calc R . . C28 C 0.0878(4) 0.2880(4) 0.11340(18) 0.0774(12) Uani 1 1 d . . . H28 H 0.0701 0.2769 0.0765 0.093 Uiso 1 1 calc R . . C29 C 0.2063(3) 0.3243(3) 0.13625(14) 0.0576(9) Uani 1 1 d . . . H29 H 0.2675 0.3383 0.1147 0.069 Uiso 1 1 calc R . . C13 C 0.4496(3) 0.6350(3) 0.14515(12) 0.0477(8) Uani 1 1 d . . . H13A H 0.5083 0.5883 0.1696 0.057 Uiso 1 1 calc R . . H13B H 0.4715 0.7215 0.1490 0.057 Uiso 1 1 calc R . . C14 C 0.4578(3) 0.5947(3) 0.08849(11) 0.0355(6) Uani 1 1 d . . . C15 C 0.1475(3) 0.4118(3) -0.08181(12) 0.0394(7) Uani 1 1 d . . . C16 C -0.0093(3) 0.3679(4) -0.15623(14) 0.0626(10) Uani 1 1 d . . . H16A H 0.0605 0.3695 -0.1755 0.094 Uiso 1 1 calc R . . H16B H -0.0676 0.4296 -0.1705 0.094 Uiso 1 1 calc R . . H16C H -0.0475 0.2881 -0.1599 0.094 Uiso 1 1 calc R . . C17 C -0.0634(3) 0.3929(4) -0.06335(15) 0.0661(11) Uani 1 1 d . . . H17A H -0.0253 0.4092 -0.0274 0.099 Uiso 1 1 calc R . . H17B H -0.1031 0.3139 -0.0647 0.099 Uiso 1 1 calc R . . H17C H -0.1234 0.4556 -0.0743 0.099 Uiso 1 1 calc R . . C1 C 0.4673(3) 0.7987(3) 0.44548(11) 0.0404(7) Uani 1 1 d . . . O8 O 0.7923(11) 0.1868(8) 0.0082(6) 0.428(10) Uani 1 1 d . . . H15 H 0.206(2) 0.401(2) -0.1117(11) 0.027(7) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.02589(18) 0.0471(2) 0.02625(18) 0.00016(13) 0.00152(12) -0.00300(13) S1 0.0604(5) 0.0485(5) 0.0476(5) 0.0049(4) 0.0125(4) 0.0198(4) S2 0.0367(4) 0.0458(4) 0.0505(5) -0.0171(4) 0.0084(3) 0.0049(3) O1 0.0428(12) 0.0563(13) 0.0273(10) -0.0118(9) 0.0019(8) 0.0026(9) O2 0.0319(10) 0.0565(13) 0.0283(10) -0.0108(9) 0.0068(8) -0.0063(9) O4 0.0413(12) 0.0722(15) 0.0296(10) -0.0114(10) 0.0073(9) -0.0067(10) O5 0.0287(10) 0.0617(14) 0.0371(11) -0.0054(10) 0.0006(8) -0.0046(9) O3 0.0381(12) 0.0715(16) 0.0430(12) -0.0101(11) 0.0168(10) -0.0050(10) O6 0.0588(15) 0.0548(14) 0.0440(13) -0.0171(11) 0.0026(11) 0.0019(11) O7 0.0558(15) 0.0617(15) 0.0469(13) -0.0128(11) -0.0073(11) -0.0048(11) N1 0.0313(13) 0.0556(16) 0.0442(15) -0.0034(12) -0.0010(11) -0.0036(11) C2 0.052(2) 0.060(2) 0.0417(18) -0.0155(16) -0.0104(15) 0.0097(16) C3 0.0285(14) 0.0461(17) 0.0287(14) -0.0083(12) 0.0041(11) -0.0003(12) C4 0.0330(15) 0.0408(16) 0.0331(15) -0.0050(12) 0.0054(11) 0.0021(12) C5 0.0291(14) 0.0385(16) 0.0369(15) -0.0122(12) 0.0058(11) -0.0003(11) C6 0.0257(14) 0.0478(17) 0.0279(14) -0.0113(12) 0.0042(11) -0.0050(11) C7 0.0259(14) 0.0432(16) 0.0345(15) -0.0041(12) 0.0040(11) -0.0027(11) C8 0.0501(19) 0.053(2) 0.0383(17) 0.0007(14) 0.0049(14) -0.0011(15) C9 0.062(2) 0.044(2) 0.058(2) 0.0069(16) 0.0040(17) 0.0062(15) C10 0.052(2) 0.0406(18) 0.058(2) -0.0091(16) 0.0057(16) 0.0051(14) C11 0.0398(17) 0.0428(18) 0.0457(18) -0.0124(14) 0.0045(13) 0.0017(13) C12 0.0253(14) 0.0393(16) 0.0350(15) -0.0083(12) 0.0042(11) -0.0004(11) C18 0.065(2) 0.0355(17) 0.0495(19) -0.0028(14) 0.0167(16) 0.0016(15) C19 0.104(3) 0.053(2) 0.052(2) 0.0050(18) 0.021(2) 0.004(2) C20 0.170(6) 0.064(3) 0.077(3) 0.007(2) 0.068(4) 0.000(3) C21 0.139(5) 0.058(3) 0.130(5) -0.009(3) 0.093(4) -0.018(3) C22 0.071(3) 0.070(3) 0.137(5) -0.016(3) 0.043(3) -0.005(2) C23 0.065(3) 0.058(2) 0.073(3) -0.0055(19) 0.018(2) 0.0029(18) C24 0.0423(17) 0.0321(15) 0.0485(18) -0.0085(13) 0.0082(13) -0.0017(12) C25 0.053(2) 0.057(2) 0.065(2) -0.0057(18) 0.0183(17) -0.0070(16) C26 0.046(2) 0.078(3) 0.093(3) -0.002(2) 0.017(2) -0.0144(19) C27 0.050(2) 0.070(3) 0.109(4) -0.015(3) -0.004(2) -0.0204(19) C28 0.074(3) 0.081(3) 0.071(3) -0.026(2) -0.013(2) -0.010(2) C29 0.059(2) 0.061(2) 0.053(2) -0.0162(17) 0.0096(17) -0.0096(17) C13 0.0352(16) 0.071(2) 0.0385(17) -0.0167(15) 0.0123(13) -0.0177(15) C14 0.0400(16) 0.0369(16) 0.0311(15) -0.0018(12) 0.0106(12) -0.0005(12) C15 0.0304(15) 0.0477(18) 0.0387(17) 0.0008(13) -0.0001(13) -0.0014(13) C16 0.050(2) 0.085(3) 0.048(2) -0.0068(19) -0.0109(16) -0.0086(19) C17 0.0313(17) 0.102(3) 0.066(2) -0.010(2) 0.0082(16) -0.0070(18) C1 0.0524(19) 0.0426(17) 0.0247(14) 0.0005(12) -0.0003(13) -0.0018(14) O8 0.444(15) 0.213(8) 0.73(2) 0.229(11) 0.464(17) 0.182(9) _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 O5 1.9854(19) . ? Zn1 O4 2.024(2) . ? Zn1 O7 2.037(2) 2_645 ? Zn1 O3 2.043(2) 3_665 ? Zn1 O6 2.079(2) 4_575 ? Zn1 Zn1 3.0144(6) 3_665 ? S1 C4 1.774(3) . ? S1 C18 1.774(3) . ? S2 C24 1.781(3) . ? S2 C5 1.788(3) . ? O1 C3 1.376(3) . ? O1 C2 1.426(4) . ? O2 C6 1.383(3) . ? O2 C13 1.436(3) . ? O4 C14 1.241(3) . ? O5 C15 1.254(3) . ? O3 C14 1.259(3) . ? O3 Zn1 2.043(2) 3_665 ? O6 C1 1.245(4) . ? O6 Zn1 2.079(2) 4_576 ? O7 C1 1.252(4) . ? O7 Zn1 2.037(2) 2_655 ? N1 C15 1.305(4) . ? N1 C16 1.460(4) . ? N1 C17 1.470(4) . ? C2 C1 1.506(4) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.381(4) . ? C3 C12 1.417(4) . ? C4 C5 1.434(4) . ? C5 C6 1.376(4) . ? C6 C7 1.425(4) . ? C7 C8 1.410(4) . ? C7 C12 1.420(4) . ? C8 C9 1.366(5) . ? C8 H8 0.9300 . ? C9 C10 1.407(5) . ? C9 H9 0.9300 . ? C10 C11 1.354(5) . ? C10 H10 0.9300 . ? C11 C12 1.425(4) . ? C11 H11 0.9300 . ? C18 C23 1.373(5) . ? C18 C19 1.392(5) . ? C19 C20 1.369(6) . ? C19 H19 0.9300 . ? C20 C21 1.368(8) . ? C20 H20 0.9300 . ? C21 C22 1.382(8) . ? C21 H21 0.9300 . ? C22 C23 1.385(6) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 C29 1.385(5) . ? C24 C25 1.387(5) . ? C25 C26 1.375(5) . ? C25 H25 0.9300 . ? C26 C27 1.352(6) . ? C26 H26 0.9300 . ? C27 C28 1.391(6) . ? C27 H27 0.9300 . ? C28 C29 1.401(5) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C13 C14 1.506(4) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C15 H15 1.06(3) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 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 O5 Zn1 O4 102.41(8) . . ? O5 Zn1 O7 104.01(9) . 2_645 ? O4 Zn1 O7 86.89(10) . 2_645 ? O5 Zn1 O3 99.54(8) . 3_665 ? O4 Zn1 O3 157.92(9) . 3_665 ? O7 Zn1 O3 90.15(10) 2_645 3_665 ? O5 Zn1 O6 97.88(9) . 4_575 ? O4 Zn1 O6 89.60(9) . 4_575 ? O7 Zn1 O6 158.07(10) 2_645 4_575 ? O3 Zn1 O6 85.01(10) 3_665 4_575 ? O5 Zn1 Zn1 173.04(6) . 3_665 ? O4 Zn1 Zn1 81.08(6) . 3_665 ? O7 Zn1 Zn1 82.08(7) 2_645 3_665 ? O3 Zn1 Zn1 76.85(6) 3_665 3_665 ? O6 Zn1 Zn1 75.99(7) 4_575 3_665 ? C4 S1 C18 104.72(15) . . ? C24 S2 C5 100.43(13) . . ? C3 O1 C2 115.3(2) . . ? C6 O2 C13 110.8(2) . . ? C14 O4 Zn1 125.13(19) . . ? C15 O5 Zn1 120.56(19) . . ? C14 O3 Zn1 129.44(19) . 3_665 ? C1 O6 Zn1 130.5(2) . 4_576 ? C1 O7 Zn1 124.3(2) . 2_655 ? C15 N1 C16 121.1(3) . . ? C15 N1 C17 121.6(3) . . ? C16 N1 C17 117.4(3) . . ? O1 C2 C1 112.1(3) . . ? O1 C2 H2A 109.2 . . ? C1 C2 H2A 109.2 . . ? O1 C2 H2B 109.2 . . ? C1 C2 H2B 109.2 . . ? H2A C2 H2B 107.9 . . ? O1 C3 C4 121.0(3) . . ? O1 C3 C12 117.2(2) . . ? C4 C3 C12 121.7(2) . . ? C3 C4 C5 119.4(3) . . ? C3 C4 S1 121.5(2) . . ? C5 C4 S1 119.1(2) . . ? C6 C5 C4 119.4(2) . . ? C6 C5 S2 119.8(2) . . ? C4 C5 S2 120.8(2) . . ? C5 C6 O2 120.3(2) . . ? C5 C6 C7 121.9(2) . . ? O2 C6 C7 117.8(3) . . ? C8 C7 C12 119.1(3) . . ? C8 C7 C6 122.4(3) . . ? C12 C7 C6 118.4(3) . . ? C9 C8 C7 120.6(3) . . ? C9 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? C8 C9 C10 120.5(3) . . ? C8 C9 H9 119.8 . . ? C10 C9 H9 119.8 . . ? C11 C10 C9 120.5(3) . . ? C11 C10 H10 119.7 . . ? C9 C10 H10 119.7 . . ? C10 C11 C12 120.7(3) . . ? C10 C11 H11 119.7 . . ? C12 C11 H11 119.7 . . ? C3 C12 C7 119.1(2) . . ? C3 C12 C11 122.3(3) . . ? C7 C12 C11 118.6(3) . . ? C23 C18 C19 120.3(4) . . ? C23 C18 S1 123.5(3) . . ? C19 C18 S1 115.9(3) . . ? C20 C19 C18 119.7(5) . . ? C20 C19 H19 120.2 . . ? C18 C19 H19 120.2 . . ? C21 C20 C19 120.5(5) . . ? C21 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C20 C21 C22 119.9(5) . . ? C20 C21 H21 120.0 . . ? C22 C21 H21 120.0 . . ? C21 C22 C23 120.2(5) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? C18 C23 C22 119.3(4) . . ? C18 C23 H23 120.4 . . ? C22 C23 H23 120.4 . . ? C29 C24 C25 119.8(3) . . ? C29 C24 S2 120.0(3) . . ? C25 C24 S2 120.2(3) . . ? C26 C25 C24 120.2(4) . . ? C26 C25 H25 119.9 . . ? C24 C25 H25 119.9 . . ? C27 C26 C25 120.9(4) . . ? C27 C26 H26 119.6 . . ? C25 C26 H26 119.6 . . ? C26 C27 C28 120.1(4) . . ? C26 C27 H27 119.9 . . ? C28 C27 H27 119.9 . . ? C27 C28 C29 119.8(4) . . ? C27 C28 H28 120.1 . . ? C29 C28 H28 120.1 . . ? C24 C29 C28 119.1(4) . . ? C24 C29 H29 120.4 . . ? C28 C29 H29 120.4 . . ? O2 C13 C14 111.8(2) . . ? O2 C13 H13A 109.3 . . ? C14 C13 H13A 109.3 . . ? O2 C13 H13B 109.3 . . ? C14 C13 H13B 109.3 . . ? H13A C13 H13B 107.9 . . ? O4 C14 O3 126.8(3) . . ? O4 C14 C13 120.0(3) . . ? O3 C14 C13 113.2(3) . . ? O5 C15 N1 123.6(3) . . ? O5 C15 H15 123.1(14) . . ? N1 C15 H15 113.2(14) . . ? N1 C16 H16A 109.5 . . ? N1 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N1 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N1 C17 H17A 109.5 . . ? N1 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N1 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O6 C1 O7 126.5(3) . . ? O6 C1 C2 119.0(3) . . ? O7 C1 C2 114.4(3) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.121 _refine_diff_density_min -0.690 _refine_diff_density_rms 0.066 # Attachment '2tpznpyra.cif' data_2tpznpyra _database_code_depnum_ccdc_archive 'CCDC 699024' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H52 N2 O16 S4 Zn2' _chemical_formula_weight 1292.00 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.329(5) _cell_length_b 15.393(7) _cell_length_c 18.958(9) _cell_angle_alpha 94.935(8) _cell_angle_beta 96.422(8) _cell_angle_gamma 99.363(10) _cell_volume 2939(2) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2155 _cell_measurement_theta_min 4.04 _cell_measurement_theta_max 22.89 _exptl_crystal_description blocks _exptl_crystal_colour colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.460 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1332 _exptl_absorpt_coefficient_mu 1.028 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17239 _diffrn_reflns_av_R_equivalents 0.0785 _diffrn_reflns_av_sigmaI/netI 0.1323 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.85 _diffrn_reflns_theta_max 25.50 _reflns_number_total 10504 _reflns_number_gt 5478 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1031P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10504 _refine_ls_number_parameters 751 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1467 _refine_ls_R_factor_gt 0.0702 _refine_ls_wR_factor_ref 0.2098 _refine_ls_wR_factor_gt 0.1627 _refine_ls_goodness_of_fit_ref 0.983 _refine_ls_restrained_S_all 0.983 _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 1.04922(8) 0.67957(5) 0.20856(4) 0.0389(2) Uani 1 1 d . . . Zn2 Zn 1.02516(7) 0.83391(5) 0.31326(4) 0.0364(2) Uani 1 1 d . . . S1 S 0.43430(17) 0.95034(13) -0.10382(10) 0.0459(5) Uani 1 1 d . . . S2 S 0.47509(17) 0.81738(13) 0.01804(9) 0.0451(5) Uani 1 1 d . . . S3 S 1.58729(18) 0.66517(14) 0.52511(11) 0.0532(5) Uani 1 1 d . . . S4 S 1.54642(18) 0.51622(12) 0.63295(10) 0.0453(5) Uani 1 1 d . . . O1 O 0.6826(4) 0.9972(3) -0.1766(2) 0.0410(11) Uani 1 1 d . . . O2 O 0.7550(5) 0.7896(3) 0.0468(2) 0.0402(11) Uani 1 1 d . . . O3 O 0.8883(5) 0.8475(4) 0.2294(3) 0.0567(14) Uani 1 1 d . . . O4 O 0.9112(5) 0.7368(4) 0.1505(3) 0.0555(13) Uani 1 1 d . . . O6 O 0.8876(5) 0.7390(4) 0.3441(3) 0.0609(15) Uani 1 1 d . . . O7 O 0.9023(5) 0.6258(3) 0.2640(3) 0.0572(14) Uani 1 1 d . . . O9 O 1.1686(5) 0.7813(3) 0.3683(3) 0.0510(13) Uani 1 1 d . . . O8 O 1.1825(5) 0.6660(4) 0.2923(3) 0.0591(14) Uani 1 1 d . . . O11 O 1.3272(5) 0.7243(3) 0.4732(2) 0.0432(11) Uani 1 1 d . . . O12 O 1.2750(5) 0.4853(3) 0.6776(2) 0.0484(12) Uani 1 1 d . . . O10 O 1.0130(5) 0.9447(3) 0.3727(2) 0.0463(12) Uani 1 1 d . . . N1 N 1.0305(7) 1.0948(4) 0.3767(3) 0.0524(16) Uani 1 1 d . . . C3 C 0.6964(6) 0.9457(4) -0.1202(3) 0.0313(14) Uani 1 1 d . . . C4 C 0.8236(6) 0.9239(4) -0.1009(3) 0.0339(15) Uani 1 1 d . . . C5 C 0.9316(7) 0.9531(5) -0.1390(4) 0.0459(18) Uani 1 1 d . . . H5 H 0.9203 0.9874 -0.1765 0.055 Uiso 1 1 calc R . . C6 C 1.0532(7) 0.9298(5) -0.1194(4) 0.056(2) Uani 1 1 d . . . H6 H 1.1226 0.9462 -0.1455 0.067 Uiso 1 1 calc R . . C7 C 1.0736(7) 0.8824(5) -0.0615(4) 0.054(2) Uani 1 1 d . . . H7 H 1.1574 0.8697 -0.0483 0.065 Uiso 1 1 calc R . . C8 C 0.9725(7) 0.8538(5) -0.0233(4) 0.0463(18) Uani 1 1 d . . . H8 H 0.9874 0.8216 0.0152 0.056 Uiso 1 1 calc R . . C9 C 0.8438(6) 0.8743(4) -0.0433(3) 0.0352(15) Uani 1 1 d . . . C10 C 0.7331(6) 0.8424(4) -0.0082(3) 0.0354(15) Uani 1 1 d . . . C11 C 0.6079(6) 0.8606(4) -0.0281(3) 0.0364(15) Uani 1 1 d . . . C12 C 0.5897(6) 0.9152(4) -0.0850(3) 0.0366(15) Uani 1 1 d . . . C19 C 0.3924(7) 0.7260(5) -0.0416(4) 0.0442(17) Uani 1 1 d . . . C20 C 0.2589(7) 0.6933(5) -0.0335(4) 0.056(2) Uani 1 1 d . . . H20 H 0.2187 0.7190 0.0026 0.067 Uiso 1 1 calc R . . C21 C 0.1893(9) 0.6225(6) -0.0801(6) 0.076(3) Uani 1 1 d . . . H21 H 0.1018 0.6013 -0.0746 0.091 Uiso 1 1 calc R . . C24 C 0.4496(9) 0.6811(6) -0.0940(5) 0.067(2) Uani 1 1 d . . . H24 H 0.5389 0.6986 -0.0977 0.080 Uiso 1 1 calc R . . C23 C 0.3782(10) 0.6123(6) -0.1400(5) 0.073(3) Uani 1 1 d . . . H23 H 0.4181 0.5851 -0.1754 0.088 Uiso 1 1 calc R . . C13 C 0.3861(6) 0.9143(5) -0.1958(4) 0.0499(19) Uani 1 1 d . . . C25 C 0.7712(8) 0.8384(5) 0.1162(4) 0.0529(19) Uani 1 1 d . . . H25A H 0.6856 0.8346 0.1332 0.064 Uiso 1 1 calc R . . H25B H 0.8043 0.9002 0.1122 0.064 Uiso 1 1 calc R . . C26 C 0.8650(7) 0.8049(5) 0.1700(4) 0.0408(16) Uani 1 1 d . . . C32 C 1.2131(7) 0.7125(5) 0.3506(4) 0.0422(17) Uani 1 1 d . . . C27 C 0.8558(7) 0.6615(5) 0.3164(4) 0.0415(17) Uani 1 1 d . . . C33 C 1.3174(8) 0.6845(5) 0.4013(4) 0.054(2) Uani 1 1 d . . . H33A H 1.2982 0.6206 0.4011 0.065 Uiso 1 1 calc R . . H33B H 1.4024 0.6994 0.3841 0.065 Uiso 1 1 calc R . . C34 C 1.3191(6) 0.6654(4) 0.5240(3) 0.0369(15) Uani 1 1 d . . . C35 C 1.1910(6) 0.6363(4) 0.5449(3) 0.0373(16) Uani 1 1 d . . . C36 C 1.0783(7) 0.6685(5) 0.5138(4) 0.0465(18) Uani 1 1 d . . . H36 H 1.0862 0.7088 0.4800 0.056 Uiso 1 1 calc R . . C37 C 0.9561(8) 0.6381(6) 0.5355(5) 0.061(2) Uani 1 1 d . . . H37 H 0.8820 0.6584 0.5152 0.073 Uiso 1 1 calc R . . C38 C 0.9409(8) 0.5800(6) 0.5851(5) 0.064(2) Uani 1 1 d . . . H38 H 0.8573 0.5611 0.5977 0.077 Uiso 1 1 calc R . . C39 C 1.0516(7) 0.5478(5) 0.6179(4) 0.055(2) Uani 1 1 d . . . H39 H 1.0415 0.5084 0.6522 0.066 Uiso 1 1 calc R . . C40 C 1.1763(6) 0.5768(5) 0.5973(4) 0.0416(17) Uani 1 1 d . . . C41 C 1.2911(7) 0.5435(4) 0.6255(3) 0.0380(16) Uani 1 1 d . . . C42 C 1.4142(6) 0.5712(4) 0.6040(3) 0.0360(15) Uani 1 1 d . . . C43 C 1.4287(6) 0.6333(4) 0.5531(3) 0.0359(15) Uani 1 1 d . . . C50 C 1.6449(7) 0.5905(5) 0.7030(3) 0.0404(16) Uani 1 1 d . . . C51 C 1.6163(8) 0.6701(5) 0.7282(4) 0.053(2) Uani 1 1 d . . . H51 H 1.5390 0.6879 0.7093 0.064 Uiso 1 1 calc R . . C52 C 1.7007(10) 0.7242(6) 0.7813(5) 0.068(2) Uani 1 1 d . . . H52 H 1.6796 0.7780 0.7982 0.082 Uiso 1 1 calc R . . C53 C 1.8169(10) 0.6994(7) 0.8098(5) 0.074(3) Uani 1 1 d . . . H53 H 1.8756 0.7367 0.8446 0.088 Uiso 1 1 calc R . . C54 C 1.8422(10) 0.6204(7) 0.7859(5) 0.080(3) Uani 1 1 d . . . H54 H 1.9187 0.6025 0.8057 0.096 Uiso 1 1 calc R . . C55 C 1.7592(8) 0.5644(6) 0.7330(4) 0.060(2) Uani 1 1 d . . . H55 H 1.7797 0.5098 0.7176 0.072 Uiso 1 1 calc R . . C44 C 1.6073(7) 0.7810(6) 0.5272(5) 0.066(2) Uani 1 1 d . . . C45 C 1.5925(12) 0.8365(8) 0.5846(8) 0.112(4) Uani 1 1 d . . . H45 H 1.5650 0.8118 0.6247 0.134 Uiso 1 1 calc R . . C46 C 1.6163(13) 0.9269(9) 0.5863(11) 0.149(7) Uani 1 1 d . . . H46 H 1.6004 0.9620 0.6258 0.179 Uiso 1 1 calc R . . C49 C 1.6584(13) 0.8180(9) 0.4687(7) 0.118(5) Uani 1 1 d . . . H49 H 1.6728 0.7828 0.4290 0.141 Uiso 1 1 calc R . . C28 C 0.7490(8) 0.6053(5) 0.3489(4) 0.053(2) Uani 1 1 d . . . H45A H 0.7738 0.6104 0.4002 0.063 Uiso 1 1 calc R . . H45B H 0.6675 0.6285 0.3402 0.063 Uiso 1 1 calc R . . C14 C 0.3604(12) 0.8258(7) -0.2212(6) 0.104(4) Uani 1 1 d . . . H14 H 0.3750 0.7840 -0.1900 0.124 Uiso 1 1 calc R . . C16 C 0.2987(15) 0.8548(16) -0.3379(8) 0.137(7) Uani 1 1 d . . . H16 H 0.2736 0.8348 -0.3860 0.164 Uiso 1 1 calc R . . C29 C 1.0374(8) 1.0164(5) 0.3463(4) 0.054(2) Uani 1 1 d . . . H29 H 1.0628 1.0138 0.3008 0.065 Uiso 1 1 calc R . . C30 C 0.9937(11) 1.1053(6) 0.4478(5) 0.073(3) Uani 1 1 d . . . H30A H 0.9413 1.0512 0.4575 0.110 Uiso 1 1 calc R . . H30B H 0.9432 1.1523 0.4514 0.110 Uiso 1 1 calc R . . H30C H 1.0720 1.1195 0.4819 0.110 Uiso 1 1 calc R . . C31 C 1.0645(11) 1.1744(6) 0.3414(5) 0.081(3) Uani 1 1 d . . . H31A H 1.1423 1.2109 0.3675 0.121 Uiso 1 1 calc R . . H31B H 0.9924 1.2068 0.3398 0.121 Uiso 1 1 calc R . . H31C H 1.0813 1.1581 0.2937 0.121 Uiso 1 1 calc R . . C22 C 0.2435(11) 0.5827(6) -0.1336(6) 0.080(3) Uani 1 1 d . . . H22 H 0.1931 0.5370 -0.1653 0.096 Uiso 1 1 calc R . . C18 C 0.3666(12) 0.9728(8) -0.2435(6) 0.093(3) Uani 1 1 d . . . H18 H 0.3845 1.0332 -0.2285 0.111 Uiso 1 1 calc R . . C17 C 0.3193(15) 0.9434(13) -0.3162(7) 0.132(6) Uani 1 1 d . . . H17 H 0.3026 0.9837 -0.3484 0.159 Uiso 1 1 calc R . . C48 C 1.686(2) 0.9107(17) 0.4733(14) 0.196(11) Uani 1 1 d . . . H48 H 1.7227 0.9370 0.4360 0.236 Uiso 1 1 calc R . . C47 C 1.6626(18) 0.9647(11) 0.5307(18) 0.187(13) Uani 1 1 d . . . H47 H 1.6782 1.0260 0.5308 0.224 Uiso 1 1 calc R . . C15 C 0.3139(16) 0.7978(11) -0.2917(9) 0.149(8) Uani 1 1 d . . . H15 H 0.2930 0.7375 -0.3066 0.179 Uiso 1 1 calc R . . O15 O 0.2521(6) 0.5119(5) 0.0863(3) 0.0809(18) Uani 1 1 d . . . N2 N 0.4564(7) 0.5900(5) 0.1271(4) 0.068(2) Uani 1 1 d . . . C56 C 0.3730(11) 0.5319(8) 0.0830(6) 0.089(3) Uani 1 1 d . . . H56 H 0.4067 0.5029 0.0459 0.107 Uiso 1 1 calc R . . O5 O 1.0464(6) 0.5804(4) 0.1343(4) 0.0535(14) Uani 1 1 d . . . C1 C 0.7907(7) 1.1456(5) -0.1989(4) 0.0400(16) Uani 1 1 d . . . C2 C 0.7005(8) 1.0897(5) -0.1566(4) 0.0494(19) Uani 1 1 d . . . H2A H 0.7361 1.1015 -0.1065 0.059 Uiso 1 1 calc R . . H2B H 0.6147 1.1080 -0.1619 0.059 Uiso 1 1 calc R . . O14 O 0.8338(5) 1.1088(3) -0.2513(3) 0.0517(13) Uani 1 1 d . . . O13 O 0.8122(5) 1.2252(3) -0.1777(3) 0.0588(14) Uani 1 1 d . . . O16 O 0.8963(7) 0.6165(5) 0.0182(3) 0.088(2) Uani 1 1 d . . . C58 C 0.5946(12) 0.6109(9) 0.1130(9) 0.144(6) Uani 1 1 d . . . H58A H 0.6056 0.5768 0.0700 0.217 Uiso 1 1 calc R . . H58B H 0.6519 0.5967 0.1522 0.217 Uiso 1 1 calc R . . H58C H 0.6165 0.6728 0.1078 0.217 Uiso 1 1 calc R . . C57 C 0.4159(14) 0.6402(11) 0.1823(8) 0.157(6) Uani 1 1 d . . . H57A H 0.3774 0.6875 0.1636 0.235 Uiso 1 1 calc R . . H57B H 0.4909 0.6645 0.2170 0.235 Uiso 1 1 calc R . . H57C H 0.3516 0.6033 0.2045 0.235 Uiso 1 1 calc R . . H5OA H 1.011(8) 0.573(5) 0.095(4) 0.05(3) Uiso 1 1 d . . . H5OB H 1.123(12) 0.557(7) 0.123(5) 0.10(3) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0358(4) 0.0392(5) 0.0442(5) 0.0060(4) 0.0127(4) 0.0082(4) Zn2 0.0338(4) 0.0363(5) 0.0415(5) 0.0069(3) 0.0107(3) 0.0076(3) S1 0.0313(9) 0.0608(12) 0.0510(11) 0.0077(9) 0.0129(8) 0.0177(9) S2 0.0351(9) 0.0549(12) 0.0461(10) 0.0070(8) 0.0179(8) 0.0002(8) S3 0.0302(9) 0.0685(14) 0.0669(13) 0.0182(10) 0.0197(9) 0.0111(9) S4 0.0359(9) 0.0438(11) 0.0567(11) 0.0046(8) 0.0019(8) 0.0112(8) O1 0.037(3) 0.040(3) 0.048(3) 0.013(2) 0.010(2) 0.006(2) O2 0.043(3) 0.038(3) 0.040(3) 0.005(2) 0.003(2) 0.009(2) O3 0.057(3) 0.066(4) 0.048(3) 0.004(3) -0.002(3) 0.022(3) O4 0.059(3) 0.061(3) 0.050(3) 0.010(3) 0.001(3) 0.025(3) O6 0.053(3) 0.046(3) 0.084(4) 0.012(3) 0.025(3) -0.002(3) O7 0.049(3) 0.061(3) 0.065(3) 0.017(3) 0.022(3) 0.005(3) O9 0.048(3) 0.052(3) 0.057(3) 0.016(3) 0.006(2) 0.013(3) O8 0.050(3) 0.075(4) 0.056(3) 0.010(3) 0.002(3) 0.024(3) O11 0.041(3) 0.045(3) 0.047(3) 0.015(2) 0.006(2) 0.013(2) O12 0.053(3) 0.039(3) 0.052(3) 0.007(2) 0.016(2) 0.000(2) O10 0.052(3) 0.039(3) 0.053(3) 0.010(2) 0.015(2) 0.012(2) N1 0.057(4) 0.040(4) 0.061(4) 0.006(3) 0.010(3) 0.011(3) C3 0.027(3) 0.033(4) 0.036(4) 0.010(3) 0.010(3) 0.003(3) C4 0.030(3) 0.027(3) 0.044(4) 0.003(3) 0.013(3) -0.002(3) C5 0.038(4) 0.046(4) 0.061(5) 0.015(4) 0.019(3) 0.012(3) C6 0.034(4) 0.062(5) 0.076(6) 0.012(4) 0.026(4) 0.012(4) C7 0.021(3) 0.059(5) 0.084(6) 0.011(4) 0.012(4) 0.009(3) C8 0.032(4) 0.053(5) 0.058(5) 0.013(4) 0.007(3) 0.016(3) C9 0.025(3) 0.035(4) 0.044(4) 0.000(3) 0.004(3) 0.004(3) C10 0.034(4) 0.035(4) 0.039(4) 0.010(3) 0.009(3) 0.003(3) C11 0.031(3) 0.040(4) 0.041(4) 0.014(3) 0.011(3) 0.006(3) C12 0.028(3) 0.034(4) 0.046(4) -0.001(3) 0.011(3) 0.002(3) C19 0.036(4) 0.042(4) 0.057(4) 0.013(3) 0.011(3) 0.005(3) C20 0.038(4) 0.048(5) 0.080(6) 0.010(4) 0.009(4) 0.002(4) C21 0.042(5) 0.067(6) 0.111(8) 0.018(6) 0.003(5) -0.011(5) C24 0.054(5) 0.065(6) 0.080(6) 0.002(5) 0.025(5) 0.000(4) C23 0.081(7) 0.050(5) 0.086(6) -0.009(5) 0.026(5) 0.000(5) C13 0.017(3) 0.069(5) 0.065(5) 0.005(4) 0.000(3) 0.017(3) C25 0.062(5) 0.058(5) 0.041(4) 0.013(4) 0.002(4) 0.016(4) C26 0.035(4) 0.048(4) 0.040(4) 0.009(3) 0.012(3) 0.004(3) C32 0.040(4) 0.047(5) 0.043(4) 0.019(4) 0.012(3) 0.007(4) C27 0.030(4) 0.052(5) 0.044(4) 0.011(4) 0.006(3) 0.005(3) C33 0.057(5) 0.072(5) 0.043(4) 0.009(4) 0.013(4) 0.033(4) C34 0.031(3) 0.038(4) 0.041(4) 0.007(3) 0.004(3) 0.004(3) C35 0.026(3) 0.037(4) 0.047(4) -0.001(3) 0.004(3) 0.001(3) C36 0.033(4) 0.049(4) 0.059(5) 0.002(4) 0.008(3) 0.012(3) C37 0.036(4) 0.067(6) 0.079(6) -0.008(5) 0.005(4) 0.017(4) C38 0.032(4) 0.078(6) 0.085(6) 0.001(5) 0.022(4) 0.010(4) C39 0.035(4) 0.059(5) 0.072(5) 0.008(4) 0.023(4) 0.002(4) C40 0.026(3) 0.047(4) 0.050(4) -0.001(3) 0.006(3) 0.006(3) C41 0.038(4) 0.032(4) 0.042(4) 0.005(3) 0.012(3) -0.003(3) C42 0.028(3) 0.037(4) 0.044(4) 0.006(3) 0.005(3) 0.005(3) C43 0.021(3) 0.045(4) 0.043(4) 0.008(3) 0.007(3) 0.006(3) C50 0.036(4) 0.045(4) 0.041(4) 0.008(3) 0.014(3) 0.005(3) C51 0.045(4) 0.062(5) 0.050(5) -0.005(4) 0.008(4) 0.005(4) C52 0.065(6) 0.062(6) 0.072(6) -0.011(5) 0.014(5) 0.005(5) C53 0.064(6) 0.077(7) 0.067(6) -0.014(5) -0.002(5) -0.007(5) C54 0.063(6) 0.100(8) 0.070(6) 0.010(6) -0.020(5) 0.011(6) C55 0.046(5) 0.070(6) 0.060(5) 0.002(4) -0.010(4) 0.016(4) C44 0.026(4) 0.077(6) 0.096(7) 0.038(6) 0.001(4) 0.000(4) C45 0.088(8) 0.072(8) 0.194(13) 0.033(8) 0.081(9) 0.013(6) C46 0.071(8) 0.069(9) 0.33(2) 0.039(11) 0.076(11) 0.016(6) C49 0.117(10) 0.112(10) 0.115(9) 0.066(8) 0.011(8) -0.030(8) C28 0.053(5) 0.042(5) 0.063(5) 0.009(4) 0.022(4) -0.001(4) C14 0.112(9) 0.070(7) 0.113(9) -0.028(6) -0.057(7) 0.038(6) C16 0.091(10) 0.21(2) 0.099(11) -0.060(13) -0.007(8) 0.062(12) C29 0.064(5) 0.048(5) 0.055(5) 0.004(4) 0.018(4) 0.019(4) C30 0.101(8) 0.056(5) 0.075(6) 0.008(4) 0.023(5) 0.040(5) C31 0.103(8) 0.055(6) 0.092(7) 0.020(5) 0.036(6) 0.012(5) C22 0.071(7) 0.063(6) 0.094(7) -0.003(5) 0.004(6) -0.017(5) C18 0.100(9) 0.096(8) 0.074(7) 0.025(6) -0.009(6) -0.003(7) C17 0.124(12) 0.184(16) 0.076(9) 0.043(10) -0.026(8) -0.002(11) C48 0.16(2) 0.17(2) 0.25(3) 0.152(19) -0.007(18) -0.043(18) C47 0.074(10) 0.074(11) 0.41(4) 0.103(17) -0.027(17) -0.008(9) C15 0.162(15) 0.140(13) 0.131(12) -0.072(10) -0.088(11) 0.098(11) O15 0.056(4) 0.109(5) 0.082(4) 0.003(4) 0.019(3) 0.024(4) N2 0.051(4) 0.068(5) 0.091(5) 0.011(4) 0.025(4) 0.015(4) C56 0.067(7) 0.108(9) 0.093(8) -0.016(6) 0.025(6) 0.020(6) O5 0.044(3) 0.059(4) 0.054(4) -0.012(3) 0.008(3) 0.008(3) C1 0.033(4) 0.039(4) 0.049(4) 0.015(3) 0.011(3) -0.001(3) C2 0.051(4) 0.045(4) 0.063(5) 0.016(4) 0.033(4) 0.015(4) O14 0.052(3) 0.053(3) 0.057(3) 0.017(2) 0.026(3) 0.010(3) O13 0.052(3) 0.042(3) 0.083(4) 0.009(3) 0.023(3) 0.000(3) O16 0.078(5) 0.105(5) 0.079(4) -0.004(4) 0.000(4) 0.025(4) C58 0.074(8) 0.123(11) 0.248(17) 0.025(11) 0.091(10) 0.002(8) C57 0.080(9) 0.204(16) 0.170(14) -0.064(12) 0.020(9) 0.017(10) _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 O5 1.980(6) . ? Zn1 O8 2.030(5) . ? Zn1 O13 2.047(5) 2_775 ? Zn1 O7 2.048(5) . ? Zn1 O4 2.060(5) . ? Zn2 O10 1.991(5) . ? Zn2 O9 2.033(5) . ? Zn2 O6 2.038(5) . ? Zn2 O3 2.055(5) . ? Zn2 O14 2.103(5) 2_775 ? S1 C13 1.773(8) . ? S1 C12 1.784(7) . ? S2 C19 1.763(7) . ? S2 C11 1.777(6) . ? S3 C44 1.758(10) . ? S3 C43 1.784(6) . ? S4 C50 1.779(7) . ? S4 C42 1.781(7) . ? O1 C3 1.393(7) . ? O1 C2 1.418(8) . ? O2 C10 1.397(7) . ? O2 C25 1.437(8) . ? O3 C26 1.231(8) . ? O4 C26 1.265(8) . ? O6 C27 1.238(8) . ? O7 C27 1.271(8) . ? O9 C32 1.255(8) . ? O8 C32 1.244(8) . ? O11 C34 1.380(7) . ? O11 C33 1.432(8) . ? O12 C41 1.396(8) . ? O12 C28 1.413(8) 2_766 ? O10 C29 1.252(8) . ? N1 C29 1.307(9) . ? N1 C30 1.446(10) . ? N1 C31 1.459(10) . ? C3 C12 1.390(8) . ? C3 C4 1.424(9) . ? C4 C9 1.403(9) . ? C4 C5 1.428(9) . ? C5 C6 1.382(10) . ? C5 H5 0.9300 . ? C6 C7 1.384(11) . ? C6 H6 0.9300 . ? C7 C8 1.373(10) . ? C7 H7 0.9300 . ? C8 C9 1.433(9) . ? C8 H8 0.9300 . ? C9 C10 1.426(8) . ? C10 C11 1.385(9) . ? C11 C12 1.438(9) . ? C19 C24 1.399(11) . ? C19 C20 1.420(10) . ? C20 C21 1.387(11) . ? C20 H20 0.9300 . ? C21 C22 1.360(14) . ? C21 H21 0.9300 . ? C24 C23 1.367(11) . ? C24 H24 0.9300 . ? C23 C22 1.414(14) . ? C23 H23 0.9300 . ? C13 C18 1.354(12) . ? C13 C14 1.378(12) . ? C25 C26 1.508(10) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C32 C33 1.503(10) . ? C27 C28 1.511(9) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C43 1.385(9) . ? C34 C35 1.437(9) . ? C35 C40 1.413(9) . ? C35 C36 1.425(10) . ? C36 C37 1.392(11) . ? C36 H36 0.9300 . ? C37 C38 1.356(11) . ? C37 H37 0.9300 . ? C38 C39 1.420(12) . ? C38 H38 0.9300 . ? C39 C40 1.403(9) . ? C39 H39 0.9300 . ? C40 C41 1.434(10) . ? C41 C42 1.391(9) . ? C42 C43 1.418(9) . ? C50 C51 1.366(10) . ? C50 C55 1.387(11) . ? C51 C52 1.374(11) . ? C51 H51 0.9300 . ? C52 C53 1.384(14) . ? C52 H52 0.9300 . ? C53 C54 1.338(13) . ? C53 H53 0.9300 . ? C54 C55 1.379(12) . ? C54 H54 0.9300 . ? C55 H55 0.9300 . ? C44 C45 1.364(15) . ? C44 C49 1.404(13) . ? C45 C46 1.369(16) . ? C45 H45 0.9300 . ? C46 C47 1.35(3) . ? C46 H46 0.9300 . ? C49 C48 1.40(2) . ? C49 H49 0.9300 . ? C28 O12 1.413(8) 2_766 ? C28 H45A 0.9700 . ? C28 H45B 0.9700 . ? C14 C15 1.374(16) . ? C14 H14 0.9300 . ? C16 C15 1.31(2) . ? C16 C17 1.365(19) . ? C16 H16 0.9300 . ? C29 H29 0.9300 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C22 H22 0.9300 . ? C18 C17 1.418(16) . ? C18 H18 0.9300 . ? C17 H17 0.9300 . ? C48 C47 1.38(3) . ? C48 H48 0.9300 . ? C47 H47 0.9300 . ? C15 H15 0.9300 . ? O15 C56 1.247(12) . ? N2 C56 1.303(12) . ? N2 C57 1.390(14) . ? N2 C58 1.471(12) . ? C56 H56 0.9300 . ? O5 H5OA 0.78(8) . ? O5 H5OB 0.95(13) . ? C1 O13 1.233(8) . ? C1 O14 1.262(8) . ? C1 C2 1.508(9) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? O14 Zn2 2.103(5) 2_775 ? O13 Zn1 2.047(5) 2_775 ? C58 H58A 0.9600 . ? C58 H58B 0.9600 . ? C58 H58C 0.9600 . ? C57 H57A 0.9600 . ? C57 H57B 0.9600 . ? C57 H57C 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 O5 Zn1 O8 107.5(3) . . ? O5 Zn1 O13 100.9(2) . 2_775 ? O8 Zn1 O13 88.9(2) . 2_775 ? O5 Zn1 O7 100.7(2) . . ? O8 Zn1 O7 88.3(2) . . ? O13 Zn1 O7 158.0(2) 2_775 . ? O5 Zn1 O4 95.2(3) . . ? O8 Zn1 O4 157.3(2) . . ? O13 Zn1 O4 86.0(2) 2_775 . ? O7 Zn1 O4 88.3(2) . . ? O10 Zn2 O9 105.3(2) . . ? O10 Zn2 O6 104.9(2) . . ? O9 Zn2 O6 88.7(2) . . ? O10 Zn2 O3 96.9(2) . . ? O9 Zn2 O3 157.6(2) . . ? O6 Zn2 O3 88.4(2) . . ? O10 Zn2 O14 96.90(19) . 2_775 ? O9 Zn2 O14 89.2(2) . 2_775 ? O6 Zn2 O14 157.9(2) . 2_775 ? O3 Zn2 O14 85.2(2) . 2_775 ? C13 S1 C12 103.7(3) . . ? C19 S2 C11 102.2(3) . . ? C44 S3 C43 104.5(4) . . ? C50 S4 C42 104.9(3) . . ? C3 O1 C2 115.2(5) . . ? C10 O2 C25 112.4(5) . . ? C26 O3 Zn2 128.1(5) . . ? C26 O4 Zn1 127.4(5) . . ? C27 O6 Zn2 125.9(5) . . ? C27 O7 Zn1 128.9(5) . . ? C32 O9 Zn2 128.2(5) . . ? C32 O8 Zn1 128.9(5) . . ? C34 O11 C33 114.8(5) . . ? C41 O12 C28 114.4(5) . 2_766 ? C29 O10 Zn2 117.9(4) . . ? C29 N1 C30 120.6(7) . . ? C29 N1 C31 121.5(7) . . ? C30 N1 C31 117.9(7) . . ? C12 C3 O1 121.3(6) . . ? C12 C3 C4 121.2(6) . . ? O1 C3 C4 117.4(5) . . ? C9 C4 C3 119.7(5) . . ? C9 C4 C5 119.4(6) . . ? C3 C4 C5 120.9(6) . . ? C6 C5 C4 119.3(7) . . ? C6 C5 H5 120.4 . . ? C4 C5 H5 120.4 . . ? C5 C6 C7 121.1(7) . . ? C5 C6 H6 119.4 . . ? C7 C6 H6 119.4 . . ? C8 C7 C6 121.3(7) . . ? C8 C7 H7 119.4 . . ? C6 C7 H7 119.4 . . ? C7 C8 C9 119.3(7) . . ? C7 C8 H8 120.4 . . ? C9 C8 H8 120.4 . . ? C4 C9 C10 118.4(6) . . ? C4 C9 C8 119.6(6) . . ? C10 C9 C8 122.0(6) . . ? C11 C10 O2 120.6(5) . . ? C11 C10 C9 122.3(6) . . ? O2 C10 C9 117.1(6) . . ? C10 C11 C12 118.8(5) . . ? C10 C11 S2 119.4(5) . . ? C12 C11 S2 121.8(5) . . ? C3 C12 C11 119.4(6) . . ? C3 C12 S1 121.1(5) . . ? C11 C12 S1 119.2(4) . . ? C24 C19 C20 117.8(7) . . ? C24 C19 S2 125.2(6) . . ? C20 C19 S2 116.9(6) . . ? C21 C20 C19 118.9(8) . . ? C21 C20 H20 120.6 . . ? C19 C20 H20 120.6 . . ? C22 C21 C20 122.8(8) . . ? C22 C21 H21 118.6 . . ? C20 C21 H21 118.6 . . ? C23 C24 C19 122.0(8) . . ? C23 C24 H24 119.0 . . ? C19 C24 H24 119.0 . . ? C24 C23 C22 119.8(9) . . ? C24 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? C18 C13 C14 117.1(9) . . ? C18 C13 S1 121.0(7) . . ? C14 C13 S1 121.9(7) . . ? O2 C25 C26 112.9(6) . . ? O2 C25 H25A 109.0 . . ? C26 C25 H25A 109.0 . . ? O2 C25 H25B 109.0 . . ? C26 C25 H25B 109.0 . . ? H25A C25 H25B 107.8 . . ? O3 C26 O4 126.5(7) . . ? O3 C26 C25 115.6(7) . . ? O4 C26 C25 117.9(6) . . ? O8 C32 O9 125.5(7) . . ? O8 C32 C33 115.5(7) . . ? O9 C32 C33 119.0(7) . . ? O6 C27 O7 127.1(6) . . ? O6 C27 C28 115.0(6) . . ? O7 C27 C28 117.8(7) . . ? O11 C33 C32 114.1(6) . . ? O11 C33 H33A 108.7 . . ? C32 C33 H33A 108.7 . . ? O11 C33 H33B 108.7 . . ? C32 C33 H33B 108.7 . . ? H33A C33 H33B 107.6 . . ? O11 C34 C43 122.0(6) . . ? O11 C34 C35 117.3(6) . . ? C43 C34 C35 120.7(6) . . ? C40 C35 C36 119.6(6) . . ? C40 C35 C34 120.1(6) . . ? C36 C35 C34 120.3(6) . . ? C37 C36 C35 118.2(7) . . ? C37 C36 H36 120.9 . . ? C35 C36 H36 120.9 . . ? C38 C37 C36 122.6(8) . . ? C38 C37 H37 118.7 . . ? C36 C37 H37 118.7 . . ? C37 C38 C39 120.6(7) . . ? C37 C38 H38 119.7 . . ? C39 C38 H38 119.7 . . ? C40 C39 C38 118.5(7) . . ? C40 C39 H39 120.7 . . ? C38 C39 H39 120.7 . . ? C39 C40 C35 120.5(7) . . ? C39 C40 C41 121.4(7) . . ? C35 C40 C41 118.0(6) . . ? C42 C41 O12 121.5(6) . . ? C42 C41 C40 121.3(6) . . ? O12 C41 C40 117.2(6) . . ? C41 C42 C43 120.3(6) . . ? C41 C42 S4 118.1(5) . . ? C43 C42 S4 121.1(5) . . ? C34 C43 C42 119.7(5) . . ? C34 C43 S3 121.2(5) . . ? C42 C43 S3 119.1(5) . . ? C51 C50 C55 118.8(7) . . ? C51 C50 S4 124.9(6) . . ? C55 C50 S4 116.3(6) . . ? C50 C51 C52 120.7(8) . . ? C50 C51 H51 119.7 . . ? C52 C51 H51 119.7 . . ? C51 C52 C53 120.6(9) . . ? C51 C52 H52 119.7 . . ? C53 C52 H52 119.7 . . ? C54 C53 C52 118.1(9) . . ? C54 C53 H53 120.9 . . ? C52 C53 H53 120.9 . . ? C53 C54 C55 122.6(9) . . ? C53 C54 H54 118.7 . . ? C55 C54 H54 118.7 . . ? C54 C55 C50 119.1(8) . . ? C54 C55 H55 120.4 . . ? C50 C55 H55 120.4 . . ? C45 C44 C49 118.6(10) . . ? C45 C44 S3 124.4(8) . . ? C49 C44 S3 116.5(10) . . ? C44 C45 C46 123.3(13) . . ? C44 C45 H45 118.4 . . ? C46 C45 H45 118.4 . . ? C47 C46 C45 119.7(18) . . ? C47 C46 H46 120.1 . . ? C45 C46 H46 120.1 . . ? C48 C49 C44 116.6(16) . . ? C48 C49 H49 121.7 . . ? C44 C49 H49 121.7 . . ? O12 C28 C27 114.2(6) 2_766 . ? O12 C28 H45A 108.7 2_766 . ? C27 C28 H45A 108.7 . . ? O12 C28 H45B 108.7 2_766 . ? C27 C28 H45B 108.7 . . ? H45A C28 H45B 107.6 . . ? C15 C14 C13 121.7(12) . . ? C15 C14 H14 119.2 . . ? C13 C14 H14 119.2 . . ? C15 C16 C17 120.5(14) . . ? C15 C16 H16 119.7 . . ? C17 C16 H16 119.7 . . ? O10 C29 N1 126.2(7) . . ? O10 C29 H29 116.9 . . ? N1 C29 H29 116.9 . . ? N1 C30 H30A 109.5 . . ? N1 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? N1 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N1 C31 H31A 109.5 . . ? N1 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? N1 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C21 C22 C23 118.5(9) . . ? C21 C22 H22 120.7 . . ? C23 C22 H22 120.7 . . ? C13 C18 C17 120.8(12) . . ? C13 C18 H18 119.6 . . ? C17 C18 H18 119.6 . . ? C16 C17 C18 118.8(14) . . ? C16 C17 H17 120.6 . . ? C18 C17 H17 120.6 . . ? C47 C48 C49 123(2) . . ? C47 C48 H48 118.5 . . ? C49 C48 H48 118.5 . . ? C46 C47 C48 118.6(17) . . ? C46 C47 H47 120.7 . . ? C48 C47 H47 120.7 . . ? C16 C15 C14 120.9(14) . . ? C16 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? C56 N2 C57 122.1(9) . . ? C56 N2 C58 119.1(9) . . ? C57 N2 C58 118.5(10) . . ? O15 C56 N2 125.6(9) . . ? O15 C56 H56 117.2 . . ? N2 C56 H56 117.2 . . ? Zn1 O5 H5OA 128(6) . . ? Zn1 O5 H5OB 124(6) . . ? H5OA O5 H5OB 96(8) . . ? O13 C1 O14 126.8(6) . . ? O13 C1 C2 114.0(6) . . ? O14 C1 C2 119.1(6) . . ? O1 C2 C1 114.9(5) . . ? O1 C2 H2A 108.6 . . ? C1 C2 H2A 108.5 . . ? O1 C2 H2B 108.5 . . ? C1 C2 H2B 108.6 . . ? H2A C2 H2B 107.5 . . ? C1 O14 Zn2 127.8(4) . 2_775 ? C1 O13 Zn1 126.6(5) . 2_775 ? N2 C58 H58A 109.5 . . ? N2 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? N2 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? N2 C57 H57A 109.5 . . ? N2 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? N2 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.959 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.959 _refine_diff_density_max 0.892 _refine_diff_density_min -1.191 _refine_diff_density_rms 0.106 # Attachment 'zn2tppy1.cif' data_zn2tppy1 _database_code_depnum_ccdc_archive 'CCDC 699025' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H23 N O6 S2 Zn' _chemical_formula_weight 634.99 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.3255(18) _cell_length_b 12.302(2) _cell_length_c 12.901(2) _cell_angle_alpha 65.031(12) _cell_angle_beta 73.605(13) _cell_angle_gamma 87.517(13) _cell_volume 1419.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2395 _cell_measurement_theta_min 2.56 _cell_measurement_theta_max 22.50 _exptl_crystal_description blocks _exptl_crystal_colour colorless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.485 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 652 _exptl_absorpt_coefficient_mu 1.058 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15778 _diffrn_reflns_av_R_equivalents 0.1124 _diffrn_reflns_av_sigmaI/netI 0.1417 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 25.50 _reflns_number_total 5135 _reflns_number_gt 2523 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0969P)^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 5135 _refine_ls_number_parameters 370 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1586 _refine_ls_R_factor_gt 0.0659 _refine_ls_wR_factor_ref 0.1961 _refine_ls_wR_factor_gt 0.1501 _refine_ls_goodness_of_fit_ref 0.974 _refine_ls_restrained_S_all 0.974 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn -0.00488(7) 0.56207(6) 0.37218(6) 0.0505(3) Uani 1 1 d . . . S1 S 0.57881(16) 1.18516(15) 0.31858(15) 0.0566(5) Uani 1 1 d . . . S2 S 0.58357(17) 0.92896(17) 0.31965(17) 0.0621(5) Uani 1 1 d . . . C6 C 0.3092(6) 0.9446(5) 0.3333(5) 0.0473(15) Uani 1 1 d . . . C5 C 0.1921(6) 1.0075(6) 0.3280(5) 0.0483(16) Uani 1 1 d . . . C7 C 0.4316(6) 1.0010(6) 0.3205(5) 0.0464(15) Uani 1 1 d . . . C9 C 0.3179(6) 1.1824(6) 0.3080(5) 0.0465(15) Uani 1 1 d . . . C12 C 0.6030(9) 1.3286(8) 0.0780(7) 0.093(3) Uani 1 1 d . . . H12 H 0.5317 1.2804 0.0842 0.111 Uiso 1 1 calc R . . C8 C 0.4317(6) 1.1210(5) 0.3106(5) 0.0449(15) Uani 1 1 d . . . C10 C 0.1946(6) 1.1274(6) 0.3141(5) 0.0464(15) Uani 1 1 d . . . C11 C 0.6444(6) 1.3061(6) 0.1773(6) 0.0534(17) Uani 1 1 d . . . C17 C 0.5804(6) 0.8372(7) 0.2457(7) 0.0601(18) Uani 1 1 d . . . C4 C 0.0683(6) 0.9506(6) 0.3397(6) 0.0634(19) Uani 1 1 d . . . H4 H 0.0644 0.8713 0.3496 0.076 Uiso 1 1 calc R . . C16 C 0.7473(6) 1.3822(6) 0.1666(7) 0.0633(19) Uani 1 1 d . . . H16 H 0.7744 1.3715 0.2329 0.076 Uiso 1 1 calc R . . C1 C 0.0760(6) 1.1889(6) 0.3095(6) 0.0604(18) Uani 1 1 d . . . H1 H 0.0773 1.2687 0.2982 0.072 Uiso 1 1 calc R . . C3 C -0.0450(7) 1.0123(8) 0.3363(6) 0.072(2) Uani 1 1 d . . . H3 H -0.1256 0.9747 0.3440 0.087 Uiso 1 1 calc R . . C2 C -0.0404(7) 1.1305(8) 0.3216(6) 0.073(2) Uani 1 1 d . . . H2 H -0.1186 1.1710 0.3199 0.087 Uiso 1 1 calc R . . C19 C 0.5602(10) 0.8065(11) 0.0798(9) 0.110(3) Uani 1 1 d . . . H19 H 0.5428 0.8364 0.0062 0.132 Uiso 1 1 calc R . . C18 C 0.5525(8) 0.8801(8) 0.1359(7) 0.082(2) Uani 1 1 d . . . H18 H 0.5288 0.9584 0.1013 0.099 Uiso 1 1 calc R . . C22 C 0.6143(9) 0.7207(8) 0.2951(9) 0.091(3) Uani 1 1 d . . . H22 H 0.6341 0.6910 0.3677 0.110 Uiso 1 1 calc R . . C14 C 0.7686(10) 1.4944(9) -0.0426(9) 0.099(3) Uani 1 1 d . . . H14 H 0.8108 1.5567 -0.1165 0.119 Uiso 1 1 calc R . . C15 C 0.8098(9) 1.4752(7) 0.0546(9) 0.088(3) Uani 1 1 d . . . H15 H 0.8808 1.5250 0.0464 0.105 Uiso 1 1 calc R . . C20 C 0.5928(11) 0.6905(11) 0.1282(11) 0.119(4) Uani 1 1 d . . . H20 H 0.5970 0.6416 0.0888 0.143 Uiso 1 1 calc R . . C13 C 0.6665(11) 1.4221(10) -0.0302(8) 0.122(4) Uani 1 1 d . . . H13 H 0.6379 1.4353 -0.0965 0.147 Uiso 1 1 calc R . . C21 C 0.6191(11) 0.6476(10) 0.2367(11) 0.125(4) Uani 1 1 d . . . H21 H 0.6405 0.5685 0.2714 0.150 Uiso 1 1 calc R . . C25 C 0.1788(6) 0.6391(6) 0.5000(7) 0.0504(16) Uani 1 1 d . . . C24 C 0.2817(7) 0.7401(6) 0.4685(6) 0.0625(19) Uani 1 1 d . . . H24A H 0.2503 0.7781 0.5224 0.075 Uiso 1 1 calc R . . H24B H 0.3670 0.7076 0.4783 0.075 Uiso 1 1 calc R . . C23 C 0.3043(8) 1.3085(7) 0.4062(7) 0.069(2) Uani 1 1 d . . . H23A H 0.3878 1.3477 0.3993 0.083 Uiso 1 1 calc R . . H23B H 0.2917 1.2284 0.4710 0.083 Uiso 1 1 calc R . . C30 C -0.0326(10) 0.6988(10) 0.1308(10) 0.118(3) Uani 1 1 d . . . H30 H -0.1041 0.6406 0.1585 0.141 Uiso 1 1 calc R . . C26 C 0.1348(12) 0.7728(9) 0.1555(9) 0.119(4) Uani 1 1 d . . . H26 H 0.1893 0.7707 0.2026 0.143 Uiso 1 1 calc R . . C28 C 0.0969(17) 0.8680(12) -0.0301(13) 0.138(4) Uani 1 1 d . . . H28 H 0.1218 0.9238 -0.1098 0.166 Uiso 1 1 calc R . . C27 C 0.1676(16) 0.8671(13) 0.0387(11) 0.162(5) Uani 1 1 d . . . H27 H 0.2374 0.9264 0.0122 0.195 Uiso 1 1 calc R . . O1 O 0.3021(4) 0.8278(4) 0.3480(4) 0.0545(11) Uani 1 1 d . . . O2 O 0.3173(4) 1.2980(4) 0.2970(4) 0.0546(11) Uani 1 1 d . . . O4 O 0.1364(4) 0.4463(4) 0.3563(4) 0.0567(12) Uani 1 1 d . . . O3 O 0.1306(5) 0.6399(4) 0.4217(4) 0.0629(12) Uani 1 1 d . . . O6 O -0.1515(5) 0.6371(4) 0.4563(4) 0.0593(12) Uani 1 1 d . . . O5 O -0.1513(5) 0.4402(4) 0.3934(4) 0.0644(12) Uani 1 1 d . . . N1 N 0.0381(6) 0.6908(5) 0.2022(5) 0.0569(14) Uani 1 1 d . . . C29 C -0.0063(14) 0.7934(13) 0.0100(10) 0.142(5) Uani 1 1 d . . . H29 H -0.0630 0.7992 -0.0365 0.170 Uiso 1 1 calc R . . C31 C 0.1871(6) 0.3789(6) 0.4371(6) 0.0520(16) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0586(5) 0.0495(5) 0.0455(5) -0.0184(4) -0.0213(4) 0.0060(3) S1 0.0480(9) 0.0629(11) 0.0609(12) -0.0231(9) -0.0228(8) -0.0034(8) S2 0.0465(9) 0.0772(13) 0.0841(14) -0.0457(11) -0.0350(9) 0.0180(8) C6 0.042(3) 0.044(4) 0.052(4) -0.016(3) -0.015(3) -0.002(3) C5 0.034(3) 0.053(4) 0.054(4) -0.019(3) -0.016(3) 0.003(3) C7 0.037(3) 0.055(4) 0.046(4) -0.019(3) -0.015(3) 0.007(3) C9 0.048(4) 0.054(4) 0.038(4) -0.017(3) -0.017(3) 0.002(3) C12 0.088(6) 0.125(7) 0.042(5) -0.018(5) -0.006(4) -0.041(5) C8 0.035(3) 0.055(4) 0.046(4) -0.021(3) -0.014(3) -0.001(3) C10 0.036(3) 0.054(4) 0.043(4) -0.014(3) -0.012(3) 0.005(3) C11 0.046(4) 0.056(4) 0.052(5) -0.022(4) -0.006(3) -0.001(3) C17 0.042(4) 0.076(5) 0.081(5) -0.045(4) -0.027(4) 0.020(3) C4 0.047(4) 0.066(5) 0.071(5) -0.018(4) -0.024(3) -0.003(3) C16 0.045(4) 0.064(5) 0.077(5) -0.027(4) -0.015(4) -0.003(3) C1 0.050(4) 0.069(5) 0.060(5) -0.027(4) -0.015(3) 0.016(3) C3 0.040(4) 0.091(6) 0.080(6) -0.027(5) -0.023(4) -0.004(4) C2 0.035(4) 0.103(7) 0.072(5) -0.031(5) -0.016(3) 0.020(4) C19 0.119(8) 0.146(9) 0.131(9) -0.098(8) -0.079(7) 0.063(7) C18 0.089(6) 0.099(6) 0.085(6) -0.051(5) -0.048(5) 0.032(5) C22 0.099(7) 0.094(7) 0.120(8) -0.067(6) -0.061(6) 0.049(5) C14 0.083(7) 0.099(7) 0.078(7) -0.017(6) 0.003(5) -0.015(5) C15 0.069(5) 0.070(6) 0.109(8) -0.028(6) -0.016(5) -0.018(4) C20 0.119(8) 0.146(10) 0.182(12) -0.122(9) -0.098(8) 0.064(7) C13 0.127(9) 0.157(10) 0.063(7) -0.028(7) -0.020(6) -0.045(8) C21 0.138(10) 0.118(8) 0.192(12) -0.109(9) -0.097(9) 0.078(7) C25 0.050(4) 0.048(4) 0.060(5) -0.028(4) -0.019(3) 0.008(3) C24 0.063(4) 0.059(5) 0.068(5) -0.021(4) -0.031(4) -0.001(3) C23 0.079(5) 0.082(5) 0.073(5) -0.049(5) -0.037(4) 0.023(4) C30 0.092(7) 0.140(9) 0.119(9) -0.046(8) -0.036(6) -0.024(6) C26 0.130(9) 0.117(8) 0.064(7) 0.004(6) -0.021(6) -0.024(7) C28 0.159(13) 0.127(11) 0.103(10) -0.019(8) -0.049(10) 0.015(9) C27 0.180(14) 0.188(14) 0.079(9) -0.018(9) -0.038(9) -0.003(11) O1 0.053(3) 0.053(3) 0.063(3) -0.024(3) -0.025(2) 0.003(2) O2 0.065(3) 0.047(3) 0.055(3) -0.023(2) -0.020(2) 0.011(2) O4 0.065(3) 0.061(3) 0.052(3) -0.029(2) -0.022(2) 0.016(2) O3 0.072(3) 0.058(3) 0.071(3) -0.029(3) -0.036(3) 0.003(2) O6 0.067(3) 0.069(3) 0.051(3) -0.030(3) -0.025(2) 0.014(2) O5 0.068(3) 0.063(3) 0.061(3) -0.023(3) -0.021(2) -0.004(2) N1 0.059(4) 0.069(4) 0.050(4) -0.030(3) -0.021(3) 0.015(3) C29 0.146(12) 0.171(12) 0.070(8) 0.000(8) -0.052(7) -0.009(9) C31 0.055(4) 0.052(4) 0.055(5) -0.026(4) -0.023(3) 0.012(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N1 2.023(6) . ? Zn1 O4 2.024(4) . ? Zn1 O6 2.030(4) . ? Zn1 O5 2.055(4) . ? Zn1 O3 2.101(4) . ? Zn1 Zn1 3.0235(15) 2_566 ? S1 C11 1.759(6) . ? S1 C8 1.790(6) . ? S2 C17 1.766(7) . ? S2 C7 1.768(6) . ? C6 O1 1.371(7) . ? C6 C7 1.403(8) . ? C6 C5 1.409(8) . ? C5 C10 1.410(8) . ? C5 C4 1.424(8) . ? C7 C8 1.427(8) . ? C9 O2 1.369(7) . ? C9 C8 1.370(8) . ? C9 C10 1.435(8) . ? C12 C13 1.377(11) . ? C12 C11 1.379(10) . ? C12 H12 0.9300 . ? C10 C1 1.414(8) . ? C11 C16 1.384(9) . ? C17 C22 1.376(10) . ? C17 C18 1.397(10) . ? C4 C3 1.367(9) . ? C4 H4 0.9300 . ? C16 C15 1.398(10) . ? C16 H16 0.9300 . ? C1 C2 1.363(9) . ? C1 H1 0.9300 . ? C3 C2 1.385(10) . ? C3 H3 0.9300 . ? C2 H2 0.9300 . ? C19 C18 1.366(11) . ? C19 C20 1.366(13) . ? C19 H19 0.9300 . ? C18 H18 0.9300 . ? C22 C21 1.388(11) . ? C22 H22 0.9300 . ? C14 C13 1.339(12) . ? C14 C15 1.360(12) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C20 C21 1.374(14) . ? C20 H20 0.9300 . ? C13 H13 0.9300 . ? C21 H21 0.9300 . ? C25 O3 1.243(7) . ? C25 O5 1.264(7) 2_566 ? C25 C24 1.510(8) . ? C24 O1 1.430(7) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C23 O2 1.436(7) . ? C23 C31 1.518(9) 1_565 ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C30 N1 1.300(11) . ? C30 C29 1.454(14) . ? C30 H30 0.9300 . ? C26 N1 1.270(10) . ? C26 C27 1.414(14) . ? C26 H26 0.9300 . ? C28 C29 1.272(15) . ? C28 C27 1.296(17) . ? C28 H28 0.9300 . ? C27 H27 0.9300 . ? O4 C31 1.261(7) . ? O6 C31 1.247(7) 2_566 ? O5 C25 1.264(7) 2_566 ? C29 H29 0.9300 . ? C31 O6 1.247(7) 2_566 ? C31 C23 1.518(9) 1_545 ? 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 N1 Zn1 O4 101.75(19) . . ? N1 Zn1 O6 100.2(2) . . ? O4 Zn1 O6 157.40(18) . . ? N1 Zn1 O5 107.3(2) . . ? O4 Zn1 O5 89.52(18) . . ? O6 Zn1 O5 88.90(18) . . ? N1 Zn1 O3 95.3(2) . . ? O4 Zn1 O3 86.80(17) . . ? O6 Zn1 O3 86.03(17) . . ? O5 Zn1 O3 157.37(19) . . ? N1 Zn1 Zn1 157.68(17) . 2_566 ? O4 Zn1 Zn1 80.18(12) . 2_566 ? O6 Zn1 Zn1 77.50(13) . 2_566 ? O5 Zn1 Zn1 94.91(14) . 2_566 ? O3 Zn1 Zn1 62.46(13) . 2_566 ? C11 S1 C8 105.3(3) . . ? C17 S2 C7 105.3(3) . . ? O1 C6 C7 120.5(5) . . ? O1 C6 C5 118.6(5) . . ? C7 C6 C5 120.9(5) . . ? C6 C5 C10 120.4(5) . . ? C6 C5 C4 120.9(6) . . ? C10 C5 C4 118.7(5) . . ? C6 C7 C8 118.0(5) . . ? C6 C7 S2 123.0(5) . . ? C8 C7 S2 118.9(4) . . ? O2 C9 C8 122.1(5) . . ? O2 C9 C10 117.4(5) . . ? C8 C9 C10 120.4(6) . . ? C13 C12 C11 120.4(8) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C9 C8 C7 121.6(5) . . ? C9 C8 S1 119.5(5) . . ? C7 C8 S1 118.5(4) . . ? C5 C10 C1 119.6(6) . . ? C5 C10 C9 118.4(5) . . ? C1 C10 C9 122.0(6) . . ? C12 C11 C16 118.5(7) . . ? C12 C11 S1 125.1(6) . . ? C16 C11 S1 116.3(5) . . ? C22 C17 C18 118.9(7) . . ? C22 C17 S2 118.4(6) . . ? C18 C17 S2 122.6(6) . . ? C3 C4 C5 120.1(7) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C11 C16 C15 119.0(7) . . ? C11 C16 H16 120.5 . . ? C15 C16 H16 120.5 . . ? C2 C1 C10 119.6(7) . . ? C2 C1 H1 120.2 . . ? C10 C1 H1 120.2 . . ? C4 C3 C2 120.5(7) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C1 C2 C3 121.5(6) . . ? C1 C2 H2 119.2 . . ? C3 C2 H2 119.2 . . ? C18 C19 C20 122.1(9) . . ? C18 C19 H19 119.0 . . ? C20 C19 H19 119.0 . . ? C19 C18 C17 119.7(8) . . ? C19 C18 H18 120.2 . . ? C17 C18 H18 120.2 . . ? C17 C22 C21 120.0(9) . . ? C17 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C13 C14 C15 119.0(9) . . ? C13 C14 H14 120.5 . . ? C15 C14 H14 120.5 . . ? C14 C15 C16 121.3(8) . . ? C14 C15 H15 119.4 . . ? C16 C15 H15 119.4 . . ? C19 C20 C21 118.4(9) . . ? C19 C20 H20 120.8 . . ? C21 C20 H20 120.8 . . ? C14 C13 C12 121.7(9) . . ? C14 C13 H13 119.2 . . ? C12 C13 H13 119.2 . . ? C20 C21 C22 120.9(9) . . ? C20 C21 H21 119.5 . . ? C22 C21 H21 119.5 . . ? O3 C25 O5 126.2(6) . 2_566 ? O3 C25 C24 119.0(7) . . ? O5 C25 C24 114.7(6) 2_566 . ? O1 C24 C25 110.8(5) . . ? O1 C24 H24A 109.5 . . ? C25 C24 H24A 109.5 . . ? O1 C24 H24B 109.5 . . ? C25 C24 H24B 109.5 . . ? H24A C24 H24B 108.1 . . ? O2 C23 C31 113.4(6) . 1_565 ? O2 C23 H23A 108.9 . . ? C31 C23 H23A 108.9 1_565 . ? O2 C23 H23B 108.9 . . ? C31 C23 H23B 108.9 1_565 . ? H23A C23 H23B 107.7 . . ? N1 C30 C29 123.7(10) . . ? N1 C30 H30 118.1 . . ? C29 C30 H30 118.1 . . ? N1 C26 C27 126.3(11) . . ? N1 C26 H26 116.8 . . ? C27 C26 H26 116.8 . . ? C29 C28 C27 120.8(16) . . ? C29 C28 H28 119.6 . . ? C27 C28 H28 119.6 . . ? C28 C27 C26 117.6(15) . . ? C28 C27 H27 121.2 . . ? C26 C27 H27 121.2 . . ? C6 O1 C24 114.2(5) . . ? C9 O2 C23 114.5(5) . . ? C31 O4 Zn1 125.7(4) . . ? C25 O3 Zn1 149.4(5) . . ? C31 O6 Zn1 129.5(4) 2_566 . ? C25 O5 Zn1 107.0(4) 2_566 . ? C26 N1 C30 113.4(9) . . ? C26 N1 Zn1 123.6(6) . . ? C30 N1 Zn1 123.0(7) . . ? C28 C29 C30 117.8(12) . . ? C28 C29 H29 121.1 . . ? C30 C29 H29 121.1 . . ? O6 C31 O4 126.8(6) 2_566 . ? O6 C31 C23 114.3(6) 2_566 1_545 ? O4 C31 C23 119.0(6) . 1_545 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C6 C5 C10 179.4(5) . . . . ? C7 C6 C5 C10 -2.4(9) . . . . ? O1 C6 C5 C4 1.1(9) . . . . ? C7 C6 C5 C4 179.3(6) . . . . ? O1 C6 C7 C8 -177.4(5) . . . . ? C5 C6 C7 C8 4.4(9) . . . . ? O1 C6 C7 S2 1.1(8) . . . . ? C5 C6 C7 S2 -177.1(5) . . . . ? C17 S2 C7 C6 35.8(6) . . . . ? C17 S2 C7 C8 -145.8(5) . . . . ? O2 C9 C8 C7 -179.1(5) . . . . ? C10 C9 C8 C7 -0.6(9) . . . . ? O2 C9 C8 S1 8.0(8) . . . . ? C10 C9 C8 S1 -173.5(4) . . . . ? C6 C7 C8 C9 -3.0(9) . . . . ? S2 C7 C8 C9 178.5(5) . . . . ? C6 C7 C8 S1 170.0(4) . . . . ? S2 C7 C8 S1 -8.5(7) . . . . ? C11 S1 C8 C9 -71.4(5) . . . . ? C11 S1 C8 C7 115.5(5) . . . . ? C6 C5 C10 C1 -179.8(6) . . . . ? C4 C5 C10 C1 -1.4(9) . . . . ? C6 C5 C10 C9 -1.2(9) . . . . ? C4 C5 C10 C9 177.1(5) . . . . ? O2 C9 C10 C5 -178.7(5) . . . . ? C8 C9 C10 C5 2.7(8) . . . . ? O2 C9 C10 C1 -0.2(8) . . . . ? C8 C9 C10 C1 -178.8(6) . . . . ? C13 C12 C11 C16 2.5(13) . . . . ? C13 C12 C11 S1 -176.3(7) . . . . ? C8 S1 C11 C12 -10.8(8) . . . . ? C8 S1 C11 C16 170.4(5) . . . . ? C7 S2 C17 C22 -134.5(6) . . . . ? C7 S2 C17 C18 49.3(7) . . . . ? C6 C5 C4 C3 178.9(6) . . . . ? C10 C5 C4 C3 0.5(10) . . . . ? C12 C11 C16 C15 -3.1(11) . . . . ? S1 C11 C16 C15 175.8(6) . . . . ? C5 C10 C1 C2 1.7(9) . . . . ? C9 C10 C1 C2 -176.8(6) . . . . ? C5 C4 C3 C2 0.0(11) . . . . ? C10 C1 C2 C3 -1.2(11) . . . . ? C4 C3 C2 C1 0.3(12) . . . . ? C20 C19 C18 C17 0.9(15) . . . . ? C22 C17 C18 C19 -0.4(12) . . . . ? S2 C17 C18 C19 175.8(7) . . . . ? C18 C17 C22 C21 -0.7(13) . . . . ? S2 C17 C22 C21 -177.0(8) . . . . ? C13 C14 C15 C16 -0.3(15) . . . . ? C11 C16 C15 C14 2.0(12) . . . . ? C18 C19 C20 C21 -0.4(17) . . . . ? C15 C14 C13 C12 -0.4(16) . . . . ? C11 C12 C13 C14 -0.7(16) . . . . ? C19 C20 C21 C22 -0.7(18) . . . . ? C17 C22 C21 C20 1.2(17) . . . . ? O3 C25 C24 O1 3.1(8) . . . . ? O5 C25 C24 O1 -177.6(5) 2_566 . . . ? C29 C28 C27 C26 7(2) . . . . ? N1 C26 C27 C28 -3(2) . . . . ? C7 C6 O1 C24 83.6(7) . . . . ? C5 C6 O1 C24 -98.2(6) . . . . ? C25 C24 O1 C6 137.4(5) . . . . ? C8 C9 O2 C23 -80.3(7) . . . . ? C10 C9 O2 C23 101.1(6) . . . . ? C31 C23 O2 C9 -125.3(6) 1_565 . . . ? N1 Zn1 O4 C31 151.0(5) . . . . ? O6 Zn1 O4 C31 -15.4(8) . . . . ? O5 Zn1 O4 C31 -101.4(5) . . . . ? O3 Zn1 O4 C31 56.2(5) . . . . ? Zn1 Zn1 O4 C31 -6.3(5) 2_566 . . . ? O5 C25 O3 Zn1 4.4(13) 2_566 . . . ? C24 C25 O3 Zn1 -176.4(6) . . . . ? N1 Zn1 O3 C25 175.7(8) . . . . ? O4 Zn1 O3 C25 -82.8(9) . . . . ? O6 Zn1 O3 C25 75.8(9) . . . . ? O5 Zn1 O3 C25 -1.7(11) . . . . ? Zn1 Zn1 O3 C25 -2.2(8) 2_566 . . . ? N1 Zn1 O6 C31 -154.7(6) . . . 2_566 ? O4 Zn1 O6 C31 11.9(8) . . . 2_566 ? O5 Zn1 O6 C31 98.0(6) . . . 2_566 ? O3 Zn1 O6 C31 -60.0(5) . . . 2_566 ? Zn1 Zn1 O6 C31 2.7(5) 2_566 . . 2_566 ? N1 Zn1 O5 C25 -179.2(4) . . . 2_566 ? O4 Zn1 O5 C25 78.6(4) . . . 2_566 ? O6 Zn1 O5 C25 -78.9(4) . . . 2_566 ? O3 Zn1 O5 C25 -1.9(7) . . . 2_566 ? Zn1 Zn1 O5 C25 -1.5(4) 2_566 . . 2_566 ? C27 C26 N1 C30 0.8(16) . . . . ? C27 C26 N1 Zn1 -178.1(9) . . . . ? C29 C30 N1 C26 -1.3(15) . . . . ? C29 C30 N1 Zn1 177.6(8) . . . . ? O4 Zn1 N1 C26 -78.8(8) . . . . ? O6 Zn1 N1 C26 95.9(8) . . . . ? O5 Zn1 N1 C26 -172.0(7) . . . . ? O3 Zn1 N1 C26 9.0(8) . . . . ? Zn1 Zn1 N1 C26 13.9(10) 2_566 . . . ? O4 Zn1 N1 C30 102.4(7) . . . . ? O6 Zn1 N1 C30 -82.9(7) . . . . ? O5 Zn1 N1 C30 9.2(7) . . . . ? O3 Zn1 N1 C30 -169.8(7) . . . . ? Zn1 Zn1 N1 C30 -164.9(6) 2_566 . . . ? C27 C28 C29 C30 -7(2) . . . . ? N1 C30 C29 C28 4.5(19) . . . . ? Zn1 O4 C31 O6 7.0(10) . . . 2_566 ? Zn1 O4 C31 C23 -172.7(4) . . . 1_545 ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 0.948 _refine_diff_density_min -0.744 _refine_diff_density_rms 0.097