# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _publ_section_title ;Sulfate ion encapsulation in caged supramolecular structures assembled by second-sphere coordination ; _publ_contact_author_name 'Biao Wu' _publ_contact_author_email WUBIAO@LZB.AC.CN loop_ _publ_author_name 'Biao Wu' C.Janiak 'Chuandong Jia' 'Jianjun Liang' 'Ning Tang' ; Jin Yang ; 'Xiao-Juan Yang' 'Hongrui Zhang' # Attachment 'CC.cif' data_ligand _database_code_depnum_ccdc_archive 'CCDC 670346' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H30 N10 O3 0.3(H2O)' _chemical_formula_sum 'C24 H30.60 N10 O3.30' _chemical_formula_weight 511.98 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 25.496(2) _cell_length_b 9.7959(8) _cell_length_c 20.3394(16) _cell_angle_alpha 90.00 _cell_angle_beta 94.159(2) _cell_angle_gamma 90.00 _cell_volume 5066.5(7) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2168 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 21.53 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.342 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2168 _exptl_absorpt_coefficient_mu 0.094 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8302 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details SADABS _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 'Bruker APEX II CCD area detector' _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 14978 _diffrn_reflns_av_R_equivalents 0.0401 _diffrn_reflns_av_sigmaI/netI 0.0557 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 28.34 _reflns_number_total 6001 _reflns_number_gt 3192 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2006)' _computing_cell_refinement 'SAINT (Bruker, 2006)' _computing_data_reduction SAINT _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. The occupancy of O4 atom is refined to 0.3. ; _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^)+(0.0669P)^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 6001 _refine_ls_number_parameters 339 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1117 _refine_ls_R_factor_gt 0.0527 _refine_ls_wR_factor_ref 0.1494 _refine_ls_wR_factor_gt 0.1242 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _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 O1 O 0.17466(5) 0.41641(14) 0.08141(6) 0.0493(4) Uani 1 1 d . . . O2 O 0.32530(5) 0.64436(15) 0.03046(6) 0.0571(4) Uani 1 1 d . . . O3 O 0.00974(5) 0.65184(17) -0.03848(8) 0.0705(5) Uani 1 1 d . . . N1 N 0.14277(9) 0.7772(2) 0.17253(13) 0.0910(7) Uani 1 1 d . . . N2 N 0.08840(6) 0.46446(18) 0.09338(8) 0.0518(4) Uani 1 1 d . . . H2B H 0.0566 0.4392 0.0830 0.062 Uiso 1 1 calc R . . N3 N 0.11109(6) 0.30323(18) 0.01946(8) 0.0527(5) Uani 1 1 d . . . H3B H 0.0779 0.2873 0.0135 0.063 Uiso 1 1 calc R . . N4 N 0.38489(7) 0.6693(2) 0.22300(9) 0.0662(5) Uani 1 1 d . . . N5 N 0.27308(6) 0.56648(18) 0.10897(7) 0.0520(5) Uani 1 1 d . . . H5B H 0.2461 0.5172 0.1159 0.062 Uiso 1 1 calc R . . N6 N 0.25049(6) 0.52986(19) 0.00015(7) 0.0519(5) Uani 1 1 d . . . H6A H 0.2239 0.4871 0.0139 0.062 Uiso 1 1 calc R . . N7 N -0.02991(8) 0.8689(4) 0.12756(11) 0.1009(9) Uani 1 1 d . . . N8 N 0.06900(6) 0.80664(19) 0.00807(9) 0.0569(5) Uani 1 1 d . . . H8C H 0.1001 0.8387 0.0046 0.068 Uiso 1 1 calc R . . N9 N 0.09383(7) 0.65212(19) -0.06654(9) 0.0608(5) Uani 1 1 d . . . H9B H 0.1250 0.6825 -0.0564 0.073 Uiso 1 1 calc R . . N10 N 0.16939(6) 0.42109(17) -0.09169(7) 0.0467(4) Uani 1 1 d . . . C1 C 0.11007(15) 0.7884(3) 0.21981(17) 0.0961(10) Uani 1 1 d . . . H1A H 0.1149 0.8623 0.2483 0.115 Uiso 1 1 calc R . . C2 C 0.06962(12) 0.7003(4) 0.23041(12) 0.0859(9) Uani 1 1 d . . . H2A H 0.0476 0.7151 0.2642 0.103 Uiso 1 1 calc R . . C3 C 0.06286(9) 0.5886(3) 0.18889(11) 0.0701(7) Uani 1 1 d . . . H3A H 0.0364 0.5253 0.1948 0.084 Uiso 1 1 calc R . . C4 C 0.09625(7) 0.5727(2) 0.13829(10) 0.0501(5) Uani 1 1 d . . . C5 C 0.13470(8) 0.6701(2) 0.13266(12) 0.0619(6) Uani 1 1 d . . . H5A H 0.1567 0.6603 0.0984 0.074 Uiso 1 1 calc R . . C6 C 0.12766(7) 0.3965(2) 0.06497(9) 0.0430(5) Uani 1 1 d . . . C7 C 0.14630(8) 0.2288(2) -0.01984(10) 0.0561(6) Uani 1 1 d . . . H7A H 0.1358 0.1336 -0.0215 0.067 Uiso 1 1 calc R . . H7B H 0.1816 0.2332 0.0014 0.067 Uiso 1 1 calc R . . C8 C 0.14734(8) 0.2824(2) -0.08953(10) 0.0548(6) Uani 1 1 d . . . H8A H 0.1682 0.2214 -0.1147 0.066 Uiso 1 1 calc R . . H8B H 0.1118 0.2830 -0.1101 0.066 Uiso 1 1 calc R . . C9 C 0.35881(10) 0.7312(3) 0.26910(11) 0.0707(7) Uani 1 1 d . . . H9A H 0.3782 0.7699 0.3049 0.085 Uiso 1 1 calc R . . C10 C 0.30546(10) 0.7410(3) 0.26663(11) 0.0730(7) Uani 1 1 d . . . H10A H 0.2891 0.7834 0.3005 0.088 Uiso 1 1 calc R . . C11 C 0.27590(9) 0.6871(3) 0.21312(10) 0.0638(6) Uani 1 1 d . . . H11A H 0.2394 0.6937 0.2100 0.077 Uiso 1 1 calc R . . C12 C 0.30179(7) 0.6235(2) 0.16451(9) 0.0466(5) Uani 1 1 d . . . C13 C 0.35612(8) 0.6158(2) 0.17204(10) 0.0541(5) Uani 1 1 d . . . H13A H 0.3735 0.5709 0.1397 0.065 Uiso 1 1 calc R . . C14 C 0.28518(7) 0.5842(2) 0.04477(9) 0.0434(5) Uani 1 1 d . . . C15 C 0.25496(8) 0.5387(2) -0.07006(9) 0.0536(6) Uani 1 1 d . . . H15A H 0.2917 0.5358 -0.0796 0.064 Uiso 1 1 calc R . . H15B H 0.2401 0.6241 -0.0868 0.064 Uiso 1 1 calc R . . C16 C 0.22557(8) 0.4194(2) -0.10292(10) 0.0549(6) Uani 1 1 d . . . H16A H 0.2296 0.4222 -0.1500 0.066 Uiso 1 1 calc R . . H16B H 0.2409 0.3347 -0.0859 0.066 Uiso 1 1 calc R . . C17 C -0.01439(10) 0.9930(4) 0.14929(14) 0.0940(10) Uani 1 1 d . . . H17A H -0.0330 1.0355 0.1812 0.113 Uiso 1 1 calc R . . C18 C 0.02733(10) 1.0582(3) 0.12634(13) 0.0819(8) Uani 1 1 d . . . H18A H 0.0373 1.1438 0.1425 0.098 Uiso 1 1 calc R . . C19 C 0.05484(9) 0.9960(3) 0.07865(12) 0.0719(7) Uani 1 1 d . . . H19A H 0.0837 1.0397 0.0627 0.086 Uiso 1 1 calc R . . C20 C 0.03967(7) 0.8696(2) 0.05461(10) 0.0525(6) Uani 1 1 d . . . C21 C -0.00296(8) 0.8092(3) 0.08171(11) 0.0751(8) Uani 1 1 d . . . H21A H -0.0133 0.7226 0.0672 0.090 Uiso 1 1 calc R . . C22 C 0.05452(8) 0.7000(2) -0.03291(11) 0.0538(6) Uani 1 1 d . . . C23 C 0.08697(8) 0.5524(2) -0.11890(11) 0.0646(6) Uani 1 1 d . . . H23A H 0.0664 0.5919 -0.1561 0.078 Uiso 1 1 calc R . . H23B H 0.0680 0.4741 -0.1036 0.078 Uiso 1 1 calc R . . C24 C 0.13981(8) 0.5069(2) -0.14037(10) 0.0565(6) Uani 1 1 d . . . H24A H 0.1344 0.4566 -0.1814 0.068 Uiso 1 1 calc R . . H24B H 0.1606 0.5871 -0.1489 0.068 Uiso 1 1 calc R . . O4 O 0.0000 0.7113(5) -0.2500 0.0987(14) Uani 0.60 2 d SP . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0351(7) 0.0624(9) 0.0499(7) -0.0001(7) -0.0002(6) -0.0089(6) O2 0.0442(8) 0.0719(10) 0.0561(8) -0.0112(8) 0.0087(6) -0.0260(7) O3 0.0384(8) 0.0771(11) 0.0939(11) 0.0100(10) -0.0081(8) -0.0219(7) N1 0.0887(17) 0.0710(16) 0.1096(19) -0.0191(15) -0.0171(15) 0.0119(13) N2 0.0317(8) 0.0672(12) 0.0561(10) -0.0035(10) -0.0001(7) -0.0051(8) N3 0.0427(9) 0.0539(11) 0.0610(11) -0.0039(9) 0.0000(8) -0.0104(8) N4 0.0600(12) 0.0760(14) 0.0598(11) -0.0062(11) -0.0146(9) -0.0007(10) N5 0.0443(9) 0.0646(12) 0.0473(9) -0.0042(9) 0.0053(7) -0.0216(8) N6 0.0408(9) 0.0713(13) 0.0440(9) -0.0071(9) 0.0054(7) -0.0231(8) N7 0.0423(12) 0.189(3) 0.0720(15) 0.0011(18) 0.0119(10) -0.0248(15) N8 0.0378(9) 0.0654(13) 0.0677(11) 0.0062(10) 0.0050(8) -0.0193(8) N9 0.0421(10) 0.0615(12) 0.0771(12) -0.0064(11) -0.0067(9) -0.0165(9) N10 0.0495(10) 0.0423(10) 0.0470(9) -0.0037(8) -0.0060(7) -0.0105(7) C1 0.107(3) 0.085(2) 0.090(2) -0.0238(19) -0.0347(19) 0.035(2) C2 0.089(2) 0.115(3) 0.0510(14) -0.0131(17) -0.0066(14) 0.0464(19) C3 0.0582(14) 0.097(2) 0.0545(13) 0.0062(14) 0.0029(11) 0.0102(13) C4 0.0423(11) 0.0599(14) 0.0468(11) 0.0026(11) -0.0064(9) 0.0059(10) C5 0.0572(14) 0.0535(15) 0.0736(15) -0.0036(13) -0.0046(11) 0.0060(11) C6 0.0391(11) 0.0482(13) 0.0413(10) 0.0097(10) -0.0001(8) -0.0094(9) C7 0.0614(13) 0.0414(13) 0.0648(14) 0.0024(11) -0.0003(11) -0.0063(10) C8 0.0601(13) 0.0464(13) 0.0572(13) -0.0099(11) -0.0004(10) -0.0109(10) C9 0.0770(18) 0.0836(19) 0.0495(13) -0.0100(13) -0.0093(12) -0.0111(14) C10 0.0766(18) 0.094(2) 0.0491(13) -0.0149(14) 0.0118(12) -0.0108(14) C11 0.0545(13) 0.0843(18) 0.0536(13) -0.0060(13) 0.0116(11) -0.0111(12) C12 0.0486(11) 0.0483(13) 0.0426(10) -0.0004(10) 0.0017(9) -0.0103(9) C13 0.0534(13) 0.0557(14) 0.0517(12) -0.0068(11) -0.0059(10) 0.0018(10) C14 0.0373(10) 0.0444(12) 0.0490(11) -0.0080(10) 0.0069(8) -0.0083(9) C15 0.0474(12) 0.0676(15) 0.0461(11) -0.0055(11) 0.0049(9) -0.0129(10) C16 0.0555(13) 0.0625(15) 0.0464(11) -0.0102(11) 0.0021(9) -0.0046(11) C17 0.0457(15) 0.154(3) 0.0821(19) -0.003(2) 0.0022(13) 0.0125(18) C18 0.0760(18) 0.085(2) 0.0866(18) 0.0072(16) 0.0149(14) 0.0131(15) C19 0.0670(15) 0.0663(18) 0.0848(17) 0.0184(15) 0.0209(13) -0.0027(13) C20 0.0348(10) 0.0676(16) 0.0548(12) 0.0216(12) 0.0006(9) -0.0015(10) C21 0.0463(13) 0.118(2) 0.0607(14) 0.0167(15) 0.0004(11) -0.0252(14) C22 0.0361(11) 0.0574(14) 0.0669(14) 0.0216(12) -0.0043(10) -0.0116(10) C23 0.0544(13) 0.0567(15) 0.0790(15) 0.0038(13) -0.0200(11) -0.0149(11) C24 0.0627(14) 0.0544(14) 0.0504(11) 0.0022(11) -0.0093(10) -0.0149(11) O4 0.087(3) 0.092(3) 0.117(4) 0.000 0.001(3) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C6 1.236(2) . ? O2 C14 1.234(2) . ? O3 C22 1.233(2) . ? N1 C1 1.322(4) . ? N1 C5 1.333(3) . ? N2 C6 1.365(2) . ? N2 C4 1.404(3) . ? N2 H2B 0.8600 . ? N3 C6 1.346(2) . ? N3 C7 1.442(2) . ? N3 H3B 0.8600 . ? N4 C13 1.333(2) . ? N4 C9 1.334(3) . ? N5 C14 1.374(2) . ? N5 C12 1.416(2) . ? N5 H5B 0.8600 . ? N6 C14 1.331(2) . ? N6 C15 1.443(2) . ? N6 H6A 0.8600 . ? N7 C21 1.333(3) . ? N7 C17 1.343(4) . ? N8 C22 1.370(3) . ? N8 C20 1.392(3) . ? N8 H8C 0.8600 . ? N9 C22 1.339(3) . ? N9 C23 1.446(3) . ? N9 H9B 0.8600 . ? N10 C24 1.466(2) . ? N10 C16 1.467(2) . ? N10 C8 1.472(2) . ? C1 C2 1.374(4) . ? C1 H1A 0.9300 . ? C2 C3 1.385(4) . ? C2 H2A 0.9300 . ? C3 C4 1.391(3) . ? C3 H3A 0.9300 . ? C4 C5 1.378(3) . ? C5 H5A 0.9300 . ? C7 C8 1.514(3) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.361(3) . ? C9 H9A 0.9300 . ? C10 C11 1.383(3) . ? C10 H10A 0.9300 . ? C11 C12 1.377(3) . ? C11 H11A 0.9300 . ? C12 C13 1.384(3) . ? C13 H13A 0.9300 . ? C15 C16 1.518(3) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.353(4) . ? C17 H17A 0.9300 . ? C18 C19 1.379(3) . ? C18 H18A 0.9300 . ? C19 C20 1.377(3) . ? C19 H19A 0.9300 . ? C20 C21 1.386(3) . ? C21 H21A 0.9300 . ? C23 C24 1.513(3) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? 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 C1 N1 C5 115.5(3) . . ? C6 N2 C4 124.71(16) . . ? C6 N2 H2B 117.6 . . ? C4 N2 H2B 117.6 . . ? C6 N3 C7 123.18(17) . . ? C6 N3 H3B 118.4 . . ? C7 N3 H3B 118.4 . . ? C13 N4 C9 116.8(2) . . ? C14 N5 C12 124.73(16) . . ? C14 N5 H5B 117.6 . . ? C12 N5 H5B 117.6 . . ? C14 N6 C15 123.64(16) . . ? C14 N6 H6A 118.2 . . ? C15 N6 H6A 118.2 . . ? C21 N7 C17 118.2(2) . . ? C22 N8 C20 128.10(17) . . ? C22 N8 H8C 116.0 . . ? C20 N8 H8C 116.0 . . ? C22 N9 C23 123.91(17) . . ? C22 N9 H9B 118.0 . . ? C23 N9 H9B 118.0 . . ? C24 N10 C16 111.21(16) . . ? C24 N10 C8 111.76(15) . . ? C16 N10 C8 111.93(16) . . ? N1 C1 C2 125.6(3) . . ? N1 C1 H1A 117.2 . . ? C2 C1 H1A 117.2 . . ? C1 C2 C3 117.5(3) . . ? C1 C2 H2A 121.2 . . ? C3 C2 H2A 121.2 . . ? C2 C3 C4 118.9(3) . . ? C2 C3 H3A 120.5 . . ? C4 C3 H3A 120.5 . . ? C5 C4 C3 117.4(2) . . ? C5 C4 N2 122.49(19) . . ? C3 C4 N2 120.0(2) . . ? N1 C5 C4 125.0(2) . . ? N1 C5 H5A 117.5 . . ? C4 C5 H5A 117.5 . . ? O1 C6 N3 122.87(18) . . ? O1 C6 N2 122.32(18) . . ? N3 C6 N2 114.77(17) . . ? N3 C7 C8 113.41(18) . . ? N3 C7 H7A 108.9 . . ? C8 C7 H7A 108.9 . . ? N3 C7 H7B 108.9 . . ? C8 C7 H7B 108.9 . . ? H7A C7 H7B 107.7 . . ? N10 C8 C7 112.38(16) . . ? N10 C8 H8A 109.1 . . ? C7 C8 H8A 109.1 . . ? N10 C8 H8B 109.1 . . ? C7 C8 H8B 109.1 . . ? H8A C8 H8B 107.9 . . ? N4 C9 C10 123.6(2) . . ? N4 C9 H9A 118.2 . . ? C10 C9 H9A 118.2 . . ? C9 C10 C11 119.2(2) . . ? C9 C10 H10A 120.4 . . ? C11 C10 H10A 120.4 . . ? C12 C11 C10 118.4(2) . . ? C12 C11 H11A 120.8 . . ? C10 C11 H11A 120.8 . . ? C11 C12 C13 118.22(19) . . ? C11 C12 N5 120.29(18) . . ? C13 C12 N5 121.48(18) . . ? N4 C13 C12 123.7(2) . . ? N4 C13 H13A 118.2 . . ? C12 C13 H13A 118.2 . . ? O2 C14 N6 123.47(17) . . ? O2 C14 N5 122.11(17) . . ? N6 C14 N5 114.41(16) . . ? N6 C15 C16 108.51(17) . . ? N6 C15 H15A 110.0 . . ? C16 C15 H15A 110.0 . . ? N6 C15 H15B 110.0 . . ? C16 C15 H15B 110.0 . . ? H15A C15 H15B 108.4 . . ? N10 C16 C15 112.28(17) . . ? N10 C16 H16A 109.1 . . ? C15 C16 H16A 109.1 . . ? N10 C16 H16B 109.1 . . ? C15 C16 H16B 109.1 . . ? H16A C16 H16B 107.9 . . ? N7 C17 C18 122.3(3) . . ? N7 C17 H17A 118.9 . . ? C18 C17 H17A 118.8 . . ? C17 C18 C19 119.1(3) . . ? C17 C18 H18A 120.4 . . ? C19 C18 H18A 120.4 . . ? C20 C19 C18 120.2(2) . . ? C20 C19 H19A 119.9 . . ? C18 C19 H19A 119.9 . . ? C19 C20 C21 116.8(2) . . ? C19 C20 N8 119.27(19) . . ? C21 C20 N8 123.8(2) . . ? N7 C21 C20 123.3(3) . . ? N7 C21 H21A 118.3 . . ? C20 C21 H21A 118.3 . . ? O3 C22 N9 122.8(2) . . ? O3 C22 N8 123.7(2) . . ? N9 C22 N8 113.54(17) . . ? N9 C23 C24 110.41(16) . . ? N9 C23 H23A 109.6 . . ? C24 C23 H23A 109.6 . . ? N9 C23 H23B 109.6 . . ? C24 C23 H23B 109.6 . . ? H23A C23 H23B 108.1 . . ? N10 C24 C23 113.54(17) . . ? N10 C24 H24A 108.9 . . ? C23 C24 H24A 108.9 . . ? N10 C24 H24B 108.9 . . ? C23 C24 H24B 108.9 . . ? H24A C24 H24B 107.7 . . ? 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 C5 N1 C1 C2 0.0(4) . . . . ? N1 C1 C2 C3 1.2(4) . . . . ? C1 C2 C3 C4 -1.3(3) . . . . ? C2 C3 C4 C5 0.3(3) . . . . ? C2 C3 C4 N2 -176.54(19) . . . . ? C6 N2 C4 C5 37.4(3) . . . . ? C6 N2 C4 C3 -145.97(19) . . . . ? C1 N1 C5 C4 -1.1(4) . . . . ? C3 C4 C5 N1 1.0(3) . . . . ? N2 C4 C5 N1 177.7(2) . . . . ? C7 N3 C6 O1 -7.3(3) . . . . ? C7 N3 C6 N2 174.84(16) . . . . ? C4 N2 C6 O1 7.1(3) . . . . ? C4 N2 C6 N3 -175.05(17) . . . . ? C6 N3 C7 C8 -102.4(2) . . . . ? C24 N10 C8 C7 -138.93(18) . . . . ? C16 N10 C8 C7 95.6(2) . . . . ? N3 C7 C8 N10 65.9(2) . . . . ? C13 N4 C9 C10 0.5(4) . . . . ? N4 C9 C10 C11 -1.5(4) . . . . ? C9 C10 C11 C12 0.9(4) . . . . ? C10 C11 C12 C13 0.5(3) . . . . ? C10 C11 C12 N5 179.8(2) . . . . ? C14 N5 C12 C11 133.7(2) . . . . ? C14 N5 C12 C13 -47.1(3) . . . . ? C9 N4 C13 C12 1.0(3) . . . . ? C11 C12 C13 N4 -1.6(3) . . . . ? N5 C12 C13 N4 179.2(2) . . . . ? C15 N6 C14 O2 -2.0(3) . . . . ? C15 N6 C14 N5 178.76(19) . . . . ? C12 N5 C14 O2 5.6(3) . . . . ? C12 N5 C14 N6 -175.13(19) . . . . ? C14 N6 C15 C16 154.87(19) . . . . ? C24 N10 C16 C15 85.5(2) . . . . ? C8 N10 C16 C15 -148.74(17) . . . . ? N6 C15 C16 N10 61.3(2) . . . . ? C21 N7 C17 C18 -0.1(4) . . . . ? N7 C17 C18 C19 0.4(4) . . . . ? C17 C18 C19 C20 0.4(4) . . . . ? C18 C19 C20 C21 -1.4(3) . . . . ? C18 C19 C20 N8 -177.9(2) . . . . ? C22 N8 C20 C19 -163.0(2) . . . . ? C22 N8 C20 C21 20.8(3) . . . . ? C17 N7 C21 C20 -1.1(4) . . . . ? C19 C20 C21 N7 1.9(3) . . . . ? N8 C20 C21 N7 178.1(2) . . . . ? C23 N9 C22 O3 8.5(3) . . . . ? C23 N9 C22 N8 -171.66(19) . . . . ? C20 N8 C22 O3 7.3(3) . . . . ? C20 N8 C22 N9 -172.47(18) . . . . ? C22 N9 C23 C24 -172.64(19) . . . . ? C16 N10 C24 C23 -160.12(17) . . . . ? C8 N10 C24 C23 74.0(2) . . . . ? N9 C23 C24 N10 71.1(2) . . . . ? 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 N5 H5B O1 0.86 2.14 2.9269(19) 151.0 . N6 H6A O1 0.86 2.05 2.8580(19) 156.8 . N8 H8C O2 0.86 2.09 2.901(2) 157.8 7_565 N9 H9B O2 0.86 2.16 2.923(2) 147.8 7_565 N2 H2B O3 0.86 2.06 2.898(2) 164.0 5_565 N3 H3B O3 0.86 2.40 3.164(2) 147.8 5_565 _diffrn_measured_fraction_theta_max 0.950 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.249 _refine_diff_density_min -0.201 _refine_diff_density_rms 0.039 ################## data_mn _database_code_depnum_ccdc_archive 'CCDC 670347' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H72 Mn N20 O16 S' _chemical_formula_weight 1272.26 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' Mn Mn 0.3368 0.7283 '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 12.516(3) _cell_length_b 18.505(4) _cell_length_c 13.186(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.38(3) _cell_angle_gamma 90.00 _cell_volume 3053.1(11) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour pale-pink _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.384 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1338 _exptl_absorpt_coefficient_mu 0.332 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8734 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details SADABS _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 'Bruker APEX II CCD area detector' _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 17921 _diffrn_reflns_av_R_equivalents 0.0246 _diffrn_reflns_av_sigmaI/netI 0.0305 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 27.92 _reflns_number_total 6945 _reflns_number_gt 4886 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2006)' _computing_cell_refinement 'SAINT (Bruker, 2006)' _computing_data_reduction SAINT _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. The hydrogen atoms on water molecules are located by Foureir difference syntheses and the bond distances of O-H are fixed as 0.85(2) \%A. ; _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^)+(0.0446P)^2^+0.4235P] 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 6945 _refine_ls_number_parameters 427 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0579 _refine_ls_R_factor_gt 0.0362 _refine_ls_wR_factor_ref 0.0995 _refine_ls_wR_factor_gt 0.0886 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.032 _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 Mn1 Mn 0.0000 0.0000 0.5000 0.03124(10) Uani 1 2 d S . . S1 S 0.0000 0.5000 0.5000 0.04052(14) Uani 1 2 d S . . O1 O 0.40110(10) 0.42588(7) 0.32030(11) 0.0573(4) Uani 1 1 d . . . O2 O -0.01758(9) 0.78400(6) 0.35254(10) 0.0488(3) Uani 1 1 d . . . O3 O 0.21938(8) 0.60206(6) 0.85249(9) 0.0431(3) Uani 1 1 d . . . O4 O -0.10879(10) 0.00935(8) 0.62542(10) 0.0518(3) Uani 1 1 d D . . H4A H -0.1754(13) 0.0202(12) 0.6164(18) 0.080 Uiso 1 1 d D . . H4B H -0.0902(18) 0.0329(12) 0.6764(15) 0.080 Uiso 1 1 d D . . O5 O 0.12474(10) 0.00259(7) 0.61189(11) 0.0492(3) Uani 1 1 d D . . H5C H 0.1671(16) 0.0374(10) 0.6178(18) 0.080 Uiso 1 1 d D . . H5D H 0.1403(17) -0.0313(11) 0.6532(16) 0.080 Uiso 1 1 d D . . O6 O 0.00868(11) 0.11734(6) 0.49051(11) 0.0489(3) Uani 1 1 d D . . H6B H 0.0559(15) 0.1399(12) 0.4572(16) 0.080 Uiso 1 1 d D . . H6C H 0.0045(18) 0.1419(12) 0.5454(14) 0.080 Uiso 1 1 d D . . N1 N 0.16117(16) 0.20366(9) 0.39847(14) 0.0672(5) Uani 1 1 d . . . N2 N 0.24698(12) 0.39158(8) 0.39598(13) 0.0517(4) Uani 1 1 d . . . H2A H 0.1918 0.4076 0.4265 0.062 Uiso 1 1 calc R . . N3 N 0.29553(14) 0.51041(8) 0.38921(14) 0.0620(5) Uani 1 1 d . . . H3A H 0.2382 0.5191 0.4218 0.074 Uiso 1 1 calc R . . N4 N -0.31578(13) 0.60839(9) 0.23710(14) 0.0619(5) Uani 1 1 d . . . N5 N -0.06567(11) 0.66537(7) 0.35788(12) 0.0495(4) Uani 1 1 d . . . H5A H -0.0408 0.6225 0.3675 0.059 Uiso 1 1 calc R . . N6 N 0.09296(12) 0.70230(8) 0.42842(14) 0.0556(4) Uani 1 1 d . . . H6A H 0.1008 0.6579 0.4463 0.067 Uiso 1 1 calc R . . N8 N 0.06415(11) 0.57255(8) 0.76783(12) 0.0500(4) Uani 1 1 d . . . H8A H 0.0369 0.5609 0.7096 0.060 Uiso 1 1 calc R . . N9 N 0.21850(11) 0.58865(9) 0.68212(12) 0.0523(4) Uani 1 1 d . . . H9A H 0.1822 0.5753 0.6292 0.063 Uiso 1 1 calc R . . N10 N 0.31024(10) 0.65535(7) 0.49441(11) 0.0403(3) Uani 1 1 d . . . C18 C -0.05844(16) 0.59931(12) 1.01743(17) 0.0644(6) Uani 1 1 d . . . H18A H -0.0437 0.6170 1.0823 0.077 Uiso 1 1 calc R . . C1 C 0.2487(2) 0.16988(11) 0.37002(17) 0.0650(6) Uani 1 1 d . . . H1A H 0.2490 0.1196 0.3692 0.078 Uiso 1 1 calc R . . C2 C 0.33872(17) 0.20588(11) 0.34172(17) 0.0626(5) Uani 1 1 d . . . H2B H 0.3974 0.1803 0.3188 0.075 Uiso 1 1 calc R . . C3 C 0.34188(15) 0.28065(10) 0.34738(17) 0.0562(5) Uani 1 1 d . . . H3B H 0.4025 0.3059 0.3286 0.067 Uiso 1 1 calc R . . C4 C 0.25308(14) 0.31683(9) 0.38159(13) 0.0439(4) Uani 1 1 d . . . C5 C 0.16404(16) 0.27556(11) 0.40372(16) 0.0585(5) Uani 1 1 d . . . H5B H 0.1026 0.2995 0.4234 0.070 Uiso 1 1 calc R . . C6 C 0.32059(14) 0.44206(9) 0.36607(14) 0.0454(4) Uani 1 1 d . . . C7 C 0.3636(2) 0.57001(11) 0.36015(17) 0.0667(6) Uani 1 1 d . . . H7A H 0.3254 0.5999 0.3109 0.080 Uiso 1 1 calc R . . H7B H 0.4265 0.5509 0.3278 0.080 Uiso 1 1 calc R . . C8 C 0.39814(14) 0.61581(10) 0.44863(15) 0.0512(5) Uani 1 1 d . . . H8B H 0.4318 0.5852 0.4998 0.061 Uiso 1 1 calc R . . H8C H 0.4512 0.6502 0.4265 0.061 Uiso 1 1 calc R . . C9 C -0.37739(16) 0.66594(11) 0.25106(17) 0.0589(5) Uani 1 1 d . . . H9B H -0.4476 0.6649 0.2263 0.071 Uiso 1 1 calc R . . C10 C -0.34138(15) 0.72657(10) 0.30048(17) 0.0541(5) Uani 1 1 d . . . H10A H -0.3870 0.7656 0.3094 0.065 Uiso 1 1 calc R . . C11 C -0.23757(14) 0.72965(9) 0.33692(15) 0.0480(4) Uani 1 1 d . . . H11A H -0.2122 0.7706 0.3707 0.058 Uiso 1 1 calc R . . C12 C -0.17166(13) 0.67073(9) 0.32241(13) 0.0409(4) Uani 1 1 d . . . C13 C -0.21519(16) 0.61168(10) 0.27211(16) 0.0549(5) Uani 1 1 d . . . H13A H -0.1715 0.5718 0.2621 0.066 Uiso 1 1 calc R . . C14 C 0.00231(13) 0.72166(9) 0.37876(14) 0.0418(4) Uani 1 1 d . . . C15 C 0.17810(15) 0.75299(10) 0.45322(19) 0.0584(5) Uani 1 1 d . . . H15A H 0.1740 0.7668 0.5240 0.070 Uiso 1 1 calc R . . H15B H 0.1689 0.7962 0.4124 0.070 Uiso 1 1 calc R . . C16 C 0.28664(14) 0.72065(10) 0.43441(16) 0.0505(5) Uani 1 1 d . . . H16A H 0.2910 0.7088 0.3630 0.061 Uiso 1 1 calc R . . H16B H 0.3409 0.7567 0.4498 0.061 Uiso 1 1 calc R . . C17 C -0.15657(16) 0.57187(13) 0.99396(18) 0.0671(6) Uani 1 1 d . . . H17A H -0.2086 0.5723 1.0432 0.081 Uiso 1 1 calc R . . N7 N -0.18092(13) 0.54447(11) 0.90314(15) 0.0683(5) Uani 1 1 d . . . C21 C -0.10602(14) 0.54550(12) 0.83342(16) 0.0576(5) Uani 1 1 d . . . H21A H -0.1228 0.5264 0.7698 0.069 Uiso 1 1 calc R . . C20 C -0.00446(13) 0.57337(9) 0.84986(14) 0.0425(4) Uani 1 1 d . . . C19 C 0.01923(15) 0.60097(11) 0.94529(15) 0.0549(5) Uani 1 1 d . . . H19A H 0.0863 0.6203 0.9604 0.066 Uiso 1 1 calc R . . C22 C 0.17175(12) 0.58870(9) 0.77203(14) 0.0387(4) Uani 1 1 d . . . C23 C 0.32942(14) 0.61057(12) 0.67124(16) 0.0562(5) Uani 1 1 d . . . H23A H 0.3703 0.5702 0.6456 0.067 Uiso 1 1 calc R . . H23B H 0.3595 0.6237 0.7372 0.067 Uiso 1 1 calc R . . C24 C 0.33854(14) 0.67372(10) 0.59993(14) 0.0493(4) Uani 1 1 d . . . H24A H 0.2920 0.7122 0.6223 0.059 Uiso 1 1 calc R . . H24B H 0.4113 0.6917 0.6031 0.059 Uiso 1 1 calc R . . O7 O 0.0789(2) 0.54950(15) 0.4903(3) 0.0763(9) Uani 0.50 1 d P . . O9 O -0.10887(18) 0.52649(14) 0.4646(2) 0.0518(6) Uani 0.50 1 d P . . O8 O 0.0177(2) 0.43147(13) 0.44036(19) 0.0535(6) Uani 0.50 1 d P . . O10 O -0.0160(2) 0.47476(14) 0.60691(19) 0.0579(7) Uani 0.50 1 d P . . 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 Mn1 0.02830(17) 0.03043(17) 0.03490(19) -0.00048(14) -0.00140(13) 0.00034(13) S1 0.0411(3) 0.0385(3) 0.0417(3) 0.0006(3) -0.0019(3) 0.0040(3) O1 0.0517(8) 0.0490(7) 0.0721(10) 0.0073(7) 0.0209(7) 0.0027(6) O2 0.0513(7) 0.0336(6) 0.0614(8) 0.0026(6) -0.0047(6) -0.0012(5) O3 0.0355(6) 0.0497(7) 0.0437(7) -0.0012(6) -0.0051(5) 0.0007(5) O4 0.0360(7) 0.0758(10) 0.0440(8) -0.0036(7) 0.0054(6) 0.0071(6) O5 0.0462(7) 0.0442(7) 0.0562(8) 0.0100(6) -0.0207(6) -0.0084(6) O6 0.0587(8) 0.0312(6) 0.0571(9) -0.0003(6) 0.0053(7) -0.0042(5) N1 0.0830(13) 0.0552(11) 0.0639(12) 0.0000(9) 0.0120(10) -0.0212(9) N2 0.0490(9) 0.0449(9) 0.0620(11) -0.0005(7) 0.0186(8) -0.0008(7) N3 0.0711(11) 0.0460(9) 0.0700(12) -0.0091(8) 0.0259(9) -0.0047(8) N4 0.0605(10) 0.0535(10) 0.0706(12) -0.0180(9) -0.0189(9) -0.0023(8) N5 0.0501(8) 0.0299(7) 0.0678(11) 0.0017(7) -0.0139(8) 0.0005(6) N6 0.0470(9) 0.0393(8) 0.0797(12) 0.0077(8) -0.0154(8) -0.0032(7) N8 0.0362(8) 0.0708(10) 0.0428(9) -0.0064(8) -0.0021(7) -0.0102(7) N9 0.0381(8) 0.0781(11) 0.0407(9) -0.0020(8) -0.0007(7) -0.0123(7) N10 0.0356(7) 0.0421(8) 0.0433(8) -0.0024(6) 0.0015(6) -0.0043(6) C18 0.0574(12) 0.0830(15) 0.0531(13) -0.0081(11) 0.0099(10) -0.0088(11) C1 0.0940(17) 0.0446(11) 0.0561(13) 0.0012(10) -0.0009(12) -0.0061(11) C2 0.0682(13) 0.0495(11) 0.0700(15) 0.0006(10) 0.0003(11) 0.0088(10) C3 0.0488(11) 0.0479(11) 0.0718(14) 0.0055(10) 0.0012(10) 0.0002(9) C4 0.0482(10) 0.0441(10) 0.0395(10) 0.0024(8) 0.0020(8) -0.0017(8) C5 0.0600(12) 0.0571(12) 0.0593(13) -0.0006(10) 0.0162(10) -0.0090(10) C6 0.0471(10) 0.0446(10) 0.0445(10) 0.0019(8) 0.0029(8) -0.0004(8) C7 0.0971(17) 0.0451(11) 0.0590(14) -0.0025(10) 0.0248(12) -0.0093(11) C8 0.0469(10) 0.0500(10) 0.0572(12) 0.0012(9) 0.0128(9) -0.0025(8) C9 0.0491(11) 0.0607(12) 0.0662(14) -0.0057(11) -0.0109(10) -0.0045(9) C10 0.0470(10) 0.0458(10) 0.0693(14) -0.0018(10) -0.0020(9) 0.0018(8) C11 0.0522(11) 0.0360(9) 0.0556(12) -0.0027(8) -0.0042(9) -0.0037(8) C12 0.0470(9) 0.0346(8) 0.0409(10) 0.0024(7) -0.0051(8) -0.0022(7) C13 0.0594(12) 0.0433(10) 0.0615(13) -0.0129(9) -0.0109(10) 0.0033(9) C14 0.0436(9) 0.0361(9) 0.0457(10) -0.0016(8) 0.0004(8) 0.0005(7) C15 0.0483(11) 0.0442(10) 0.0821(16) -0.0062(10) -0.0130(10) -0.0010(8) C16 0.0481(10) 0.0438(10) 0.0594(12) 0.0006(9) -0.0031(9) -0.0081(8) C17 0.0485(12) 0.0896(16) 0.0640(15) 0.0040(12) 0.0159(11) -0.0072(11) N7 0.0395(9) 0.0986(14) 0.0671(13) 0.0054(11) 0.0065(8) -0.0156(9) C21 0.0372(10) 0.0821(14) 0.0534(12) 0.0025(11) -0.0031(9) -0.0099(9) C20 0.0347(8) 0.0469(10) 0.0458(10) 0.0047(8) 0.0009(8) -0.0017(7) C19 0.0429(10) 0.0661(13) 0.0559(13) -0.0117(10) 0.0031(9) -0.0090(9) C22 0.0335(8) 0.0364(8) 0.0460(10) 0.0023(8) -0.0012(7) -0.0009(7) C23 0.0346(9) 0.0843(14) 0.0497(12) 0.0079(10) 0.0030(8) -0.0052(9) C24 0.0386(9) 0.0611(11) 0.0484(11) -0.0075(9) 0.0010(8) -0.0117(8) O7 0.0561(17) 0.0556(17) 0.117(3) 0.0105(18) 0.0021(17) -0.0255(14) O9 0.0422(13) 0.0526(14) 0.0603(17) 0.0036(13) -0.0052(12) 0.0085(11) O8 0.0662(16) 0.0483(14) 0.0461(16) -0.0086(12) 0.0023(13) 0.0111(12) O10 0.086(2) 0.0504(15) 0.0367(14) 0.0020(12) 0.0006(14) 0.0143(14) _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 Mn1 O5 2.1226(13) . ? Mn1 O5 2.1226(13) 3_556 ? Mn1 O4 2.1742(14) . ? Mn1 O4 2.1742(14) 3_556 ? Mn1 O6 2.1779(12) 3_556 ? Mn1 O6 2.1779(12) . ? S1 O7 1.355(3) . ? S1 O7 1.355(3) 3_566 ? S1 O10 1.503(3) 3_566 ? S1 O10 1.503(3) . ? S1 O8 1.511(2) . ? S1 O8 1.511(2) 3_566 ? S1 O9 1.512(2) . ? S1 O9 1.512(2) 3_566 ? O1 C6 1.224(2) . ? O2 C14 1.2282(19) . ? O3 C22 1.229(2) . ? O4 H4A 0.863(15) . ? O4 H4B 0.830(15) . ? O5 H5C 0.836(15) . ? O5 H5D 0.850(16) . ? O6 H6B 0.854(16) . ? O6 H6C 0.857(16) . ? N1 C1 1.323(3) . ? N1 C5 1.333(3) . ? N2 C6 1.376(2) . ? N2 C4 1.399(2) . ? N2 H2A 0.8600 . ? N3 C6 1.340(2) . ? N3 C7 1.451(2) . ? N3 H3A 0.8600 . ? N4 C9 1.330(2) . ? N4 C13 1.332(2) . ? N5 C14 1.369(2) . ? N5 C12 1.399(2) . ? N5 H5A 0.8600 . ? N6 C14 1.345(2) . ? N6 C15 1.451(2) . ? N6 H6A 0.8600 . ? N8 C22 1.379(2) . ? N8 C20 1.397(2) . ? N8 H8A 0.8600 . ? N9 C22 1.335(2) . ? N9 C23 1.457(2) . ? N9 H9A 0.8600 . ? N10 C8 1.464(2) . ? N10 C24 1.467(2) . ? N10 C16 1.470(2) . ? C18 C17 1.358(3) . ? C18 C19 1.377(3) . ? C18 H18A 0.9300 . ? C1 C2 1.369(3) . ? C1 H1A 0.9300 . ? C2 C3 1.386(3) . ? C2 H2B 0.9300 . ? C3 C4 1.382(3) . ? C3 H3B 0.9300 . ? C4 C5 1.388(3) . ? C5 H5B 0.9300 . ? C7 C8 1.497(3) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C9 C10 1.368(3) . ? C9 H9B 0.9300 . ? C10 C11 1.376(3) . ? C10 H10A 0.9300 . ? C11 C12 1.383(2) . ? C11 H11A 0.9300 . ? C12 C13 1.383(2) . ? C13 H13A 0.9300 . ? C15 C16 1.510(3) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 N7 1.329(3) . ? C17 H17A 0.9300 . ? N7 C21 1.329(3) . ? C21 C20 1.384(2) . ? C21 H21A 0.9300 . ? C20 C19 1.383(3) . ? C19 H19A 0.9300 . ? C23 C24 1.506(3) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? O7 O10 1.555(4) 3_566 ? O7 O9 1.569(4) 3_566 ? O7 O8 1.573(4) 3_566 ? O9 O7 1.569(4) 3_566 ? O8 O7 1.573(4) 3_566 ? O10 O7 1.555(4) 3_566 ? 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 Mn1 O5 180.0 . 3_556 ? O5 Mn1 O4 86.17(6) . . ? O5 Mn1 O4 93.83(6) 3_556 . ? O5 Mn1 O4 93.83(6) . 3_556 ? O5 Mn1 O4 86.17(6) 3_556 3_556 ? O4 Mn1 O4 180.0 . 3_556 ? O5 Mn1 O6 91.11(5) . 3_556 ? O5 Mn1 O6 88.89(5) 3_556 3_556 ? O4 Mn1 O6 90.15(5) . 3_556 ? O4 Mn1 O6 89.85(5) 3_556 3_556 ? O5 Mn1 O6 88.89(5) . . ? O5 Mn1 O6 91.11(5) 3_556 . ? O4 Mn1 O6 89.85(5) . . ? O4 Mn1 O6 90.15(5) 3_556 . ? O6 Mn1 O6 180.0 3_556 . ? O7 S1 O7 180.0 . 3_566 ? O7 S1 O10 65.68(19) . 3_566 ? O7 S1 O10 114.32(19) 3_566 3_566 ? O7 S1 O10 114.32(19) . . ? O7 S1 O10 65.68(19) 3_566 . ? O10 S1 O10 180.000(1) 3_566 . ? O7 S1 O8 113.70(18) . . ? O7 S1 O8 66.30(17) 3_566 . ? O10 S1 O8 75.42(14) 3_566 . ? O10 S1 O8 104.58(14) . . ? O7 S1 O8 66.30(17) . 3_566 ? O7 S1 O8 113.70(17) 3_566 3_566 ? O10 S1 O8 104.58(14) 3_566 3_566 ? O10 S1 O8 75.42(14) . 3_566 ? O8 S1 O8 180.00(17) . 3_566 ? O7 S1 O9 113.92(16) . . ? O7 S1 O9 66.08(16) 3_566 . ? O10 S1 O9 75.45(15) 3_566 . ? O10 S1 O9 104.55(15) . . ? O8 S1 O9 104.70(14) . . ? O8 S1 O9 75.30(14) 3_566 . ? O7 S1 O9 66.08(16) . 3_566 ? O7 S1 O9 113.92(16) 3_566 3_566 ? O10 S1 O9 104.55(15) 3_566 3_566 ? O10 S1 O9 75.45(15) . 3_566 ? O8 S1 O9 75.30(14) . 3_566 ? O8 S1 O9 104.70(14) 3_566 3_566 ? O9 S1 O9 180.000(1) . 3_566 ? Mn1 O4 H4A 122.3(16) . . ? Mn1 O4 H4B 119.3(16) . . ? H4A O4 H4B 104(2) . . ? Mn1 O5 H5C 122.4(16) . . ? Mn1 O5 H5D 125.6(15) . . ? H5C O5 H5D 112(2) . . ? Mn1 O6 H6B 123.6(16) . . ? Mn1 O6 H6C 118.4(16) . . ? H6B O6 H6C 103(2) . . ? C1 N1 C5 117.70(18) . . ? C6 N2 C4 126.38(15) . . ? C6 N2 H2A 116.8 . . ? C4 N2 H2A 116.8 . . ? C6 N3 C7 121.00(17) . . ? C6 N3 H3A 119.5 . . ? C7 N3 H3A 119.5 . . ? C9 N4 C13 117.50(16) . . ? C14 N5 C12 126.37(14) . . ? C14 N5 H5A 116.8 . . ? C12 N5 H5A 116.8 . . ? C14 N6 C15 122.95(15) . . ? C14 N6 H6A 118.5 . . ? C15 N6 H6A 118.5 . . ? C22 N8 C20 125.75(15) . . ? C22 N8 H8A 117.1 . . ? C20 N8 H8A 117.1 . . ? C22 N9 C23 121.76(16) . . ? C22 N9 H9A 119.1 . . ? C23 N9 H9A 119.1 . . ? C8 N10 C24 109.89(14) . . ? C8 N10 C16 109.41(14) . . ? C24 N10 C16 111.14(14) . . ? C17 C18 C19 120.0(2) . . ? C17 C18 H18A 120.0 . . ? C19 C18 H18A 120.0 . . ? N1 C1 C2 122.7(2) . . ? N1 C1 H1A 118.7 . . ? C2 C1 H1A 118.7 . . ? C1 C2 C3 119.6(2) . . ? C1 C2 H2B 120.2 . . ? C3 C2 H2B 120.2 . . ? C4 C3 C2 118.61(18) . . ? C4 C3 H3B 120.7 . . ? C2 C3 H3B 120.7 . . ? C3 C4 C5 117.27(17) . . ? C3 C4 N2 124.77(16) . . ? C5 C4 N2 117.96(17) . . ? N1 C5 C4 124.00(19) . . ? N1 C5 H5B 118.0 . . ? C4 C5 H5B 118.0 . . ? O1 C6 N3 122.89(17) . . ? O1 C6 N2 122.68(16) . . ? N3 C6 N2 114.41(16) . . ? N3 C7 C8 112.63(17) . . ? N3 C7 H7A 109.1 . . ? C8 C7 H7A 109.1 . . ? N3 C7 H7B 109.1 . . ? C8 C7 H7B 109.1 . . ? H7A C7 H7B 107.8 . . ? N10 C8 C7 113.51(16) . . ? N10 C8 H8B 108.9 . . ? C7 C8 H8B 108.9 . . ? N10 C8 H8C 108.9 . . ? C7 C8 H8C 108.9 . . ? H8B C8 H8C 107.7 . . ? N4 C9 C10 122.48(18) . . ? N4 C9 H9B 118.8 . . ? C10 C9 H9B 118.8 . . ? C9 C10 C11 119.86(18) . . ? C9 C10 H10A 120.1 . . ? C11 C10 H10A 120.1 . . ? C10 C11 C12 118.71(17) . . ? C10 C11 H11A 120.6 . . ? C12 C11 H11A 120.6 . . ? C13 C12 C11 117.36(16) . . ? C13 C12 N5 117.62(15) . . ? C11 C12 N5 124.97(15) . . ? N4 C13 C12 124.09(17) . . ? N4 C13 H13A 118.0 . . ? C12 C13 H13A 118.0 . . ? O2 C14 N6 123.38(16) . . ? O2 C14 N5 122.50(15) . . ? N6 C14 N5 114.10(15) . . ? N6 C15 C16 111.43(15) . . ? N6 C15 H15A 109.3 . . ? C16 C15 H15A 109.3 . . ? N6 C15 H15B 109.3 . . ? C16 C15 H15B 109.3 . . ? H15A C15 H15B 108.0 . . ? N10 C16 C15 114.02(16) . . ? N10 C16 H16A 108.7 . . ? C15 C16 H16A 108.7 . . ? N10 C16 H16B 108.7 . . ? C15 C16 H16B 108.7 . . ? H16A C16 H16B 107.6 . . ? N7 C17 C18 122.3(2) . . ? N7 C17 H17A 118.8 . . ? C18 C17 H17A 118.8 . . ? C21 N7 C17 117.87(18) . . ? N7 C21 C20 123.9(2) . . ? N7 C21 H21A 118.1 . . ? C20 C21 H21A 118.1 . . ? C19 C20 C21 117.12(18) . . ? C19 C20 N8 125.86(16) . . ? C21 C20 N8 117.00(17) . . ? C18 C19 C20 118.74(18) . . ? C18 C19 H19A 120.6 . . ? C20 C19 H19A 120.6 . . ? O3 C22 N9 123.56(15) . . ? O3 C22 N8 122.07(16) . . ? N9 C22 N8 114.37(16) . . ? N9 C23 C24 111.36(15) . . ? N9 C23 H23A 109.4 . . ? C24 C23 H23A 109.4 . . ? N9 C23 H23B 109.4 . . ? C24 C23 H23B 109.4 . . ? H23A C23 H23B 108.0 . . ? N10 C24 C23 113.08(15) . . ? N10 C24 H24A 109.0 . . ? C23 C24 H24A 109.0 . . ? N10 C24 H24B 109.0 . . ? C23 C24 H24B 109.0 . . ? H24A C24 H24B 107.8 . . ? S1 O7 O10 61.73(16) . 3_566 ? S1 O7 O9 61.74(14) . 3_566 ? O10 O7 O9 99.5(2) 3_566 3_566 ? S1 O7 O8 61.61(15) . 3_566 ? O10 O7 O8 99.3(2) 3_566 3_566 ? O9 O7 O8 99.2(2) 3_566 3_566 ? S1 O9 O7 52.17(12) . 3_566 ? S1 O8 O7 52.09(12) . 3_566 ? S1 O10 O7 52.59(13) . 3_566 ? 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 C5 N1 C1 C2 -3.1(3) . . . . ? N1 C1 C2 C3 3.3(3) . . . . ? C1 C2 C3 C4 -0.1(3) . . . . ? C2 C3 C4 C5 -2.9(3) . . . . ? C2 C3 C4 N2 176.63(18) . . . . ? C6 N2 C4 C3 9.6(3) . . . . ? C6 N2 C4 C5 -170.84(18) . . . . ? C1 N1 C5 C4 -0.3(3) . . . . ? C3 C4 C5 N1 3.3(3) . . . . ? N2 C4 C5 N1 -176.33(19) . . . . ? C7 N3 C6 O1 0.3(3) . . . . ? C7 N3 C6 N2 -178.24(18) . . . . ? C4 N2 C6 O1 1.4(3) . . . . ? C4 N2 C6 N3 -179.97(18) . . . . ? C6 N3 C7 C8 -124.6(2) . . . . ? C24 N10 C8 C7 156.84(16) . . . . ? C16 N10 C8 C7 -80.88(19) . . . . ? N3 C7 C8 N10 -66.7(2) . . . . ? C13 N4 C9 C10 -0.9(3) . . . . ? N4 C9 C10 C11 0.6(3) . . . . ? C9 C10 C11 C12 0.0(3) . . . . ? C10 C11 C12 C13 -0.4(3) . . . . ? C10 C11 C12 N5 -177.97(18) . . . . ? C14 N5 C12 C13 157.36(19) . . . . ? C14 N5 C12 C11 -25.1(3) . . . . ? C9 N4 C13 C12 0.5(3) . . . . ? C11 C12 C13 N4 0.1(3) . . . . ? N5 C12 C13 N4 177.88(19) . . . . ? C15 N6 C14 O2 -2.0(3) . . . . ? C15 N6 C14 N5 176.75(18) . . . . ? C12 N5 C14 O2 -12.3(3) . . . . ? C12 N5 C14 N6 168.90(17) . . . . ? C14 N6 C15 C16 -137.78(19) . . . . ? C8 N10 C16 C15 161.83(16) . . . . ? C24 N10 C16 C15 -76.64(19) . . . . ? N6 C15 C16 N10 -60.3(2) . . . . ? C19 C18 C17 N7 1.5(4) . . . . ? C18 C17 N7 C21 -1.1(4) . . . . ? C17 N7 C21 C20 0.0(3) . . . . ? N7 C21 C20 C19 0.6(3) . . . . ? N7 C21 C20 N8 -178.0(2) . . . . ? C22 N8 C20 C19 10.6(3) . . . . ? C22 N8 C20 C21 -170.88(17) . . . . ? C17 C18 C19 C20 -0.9(3) . . . . ? C21 C20 C19 C18 -0.1(3) . . . . ? N8 C20 C19 C18 178.37(19) . . . . ? C23 N9 C22 O3 -5.2(3) . . . . ? C23 N9 C22 N8 174.64(16) . . . . ? C20 N8 C22 O3 4.0(3) . . . . ? C20 N8 C22 N9 -175.82(16) . . . . ? C22 N9 C23 C24 -120.66(19) . . . . ? C8 N10 C24 C23 -76.98(18) . . . . ? C16 N10 C24 C23 161.77(15) . . . . ? N9 C23 C24 N10 -67.9(2) . . . . ? O7 S1 O7 O10 -38(100) 3_566 . . 3_566 ? O10 S1 O7 O10 180.0 . . . 3_566 ? O8 S1 O7 O10 60.00(18) . . . 3_566 ? O8 S1 O7 O10 -120.00(18) 3_566 . . 3_566 ? O9 S1 O7 O10 -59.86(19) . . . 3_566 ? O9 S1 O7 O10 120.14(19) 3_566 . . 3_566 ? O7 S1 O7 O9 -158(100) 3_566 . . 3_566 ? O10 S1 O7 O9 -120.14(19) 3_566 . . 3_566 ? O10 S1 O7 O9 59.86(19) . . . 3_566 ? O8 S1 O7 O9 -60.14(19) . . . 3_566 ? O8 S1 O7 O9 119.86(19) 3_566 . . 3_566 ? O9 S1 O7 O9 180.0 . . . 3_566 ? O7 S1 O7 O8 82(100) 3_566 . . 3_566 ? O10 S1 O7 O8 120.00(18) 3_566 . . 3_566 ? O10 S1 O7 O8 -60.00(18) . . . 3_566 ? O8 S1 O7 O8 180.0 . . . 3_566 ? O9 S1 O7 O8 60.14(19) . . . 3_566 ? O9 S1 O7 O8 -119.86(19) 3_566 . . 3_566 ? O7 S1 O9 O7 180.0 . . . 3_566 ? O10 S1 O9 O7 125.5(2) 3_566 . . 3_566 ? O10 S1 O9 O7 -54.5(2) . . . 3_566 ? O8 S1 O9 O7 55.2(2) . . . 3_566 ? O8 S1 O9 O7 -124.8(2) 3_566 . . 3_566 ? O9 S1 O9 O7 -159(100) 3_566 . . 3_566 ? O7 S1 O8 O7 180.0 . . . 3_566 ? O10 S1 O8 O7 -125.4(2) 3_566 . . 3_566 ? O10 S1 O8 O7 54.6(2) . . . 3_566 ? O8 S1 O8 O7 -126(48) 3_566 . . 3_566 ? O9 S1 O8 O7 -55.0(2) . . . 3_566 ? O9 S1 O8 O7 125.0(2) 3_566 . . 3_566 ? O7 S1 O10 O7 180.0 . . . 3_566 ? O10 S1 O10 O7 133(100) 3_566 . . 3_566 ? O8 S1 O10 O7 -55.02(18) . . . 3_566 ? O8 S1 O10 O7 124.98(18) 3_566 . . 3_566 ? O9 S1 O10 O7 54.76(19) . . . 3_566 ? O9 S1 O10 O7 -125.24(19) 3_566 . . 3_566 ? 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 C3 H3B O1 0.93 2.22 2.813(2) 120.7 . O4 H4B O1 0.830(15) 2.051(17) 2.835(2) 158(2) 4_566 C11 H11A O2 0.93 2.47 2.934(2) 111.3 . O6 H6C O2 0.857(16) 1.926(17) 2.7599(19) 164(2) 3_566 C19 H19A O3 0.93 2.24 2.814(2) 119.1 . O5 H5C O3 0.836(15) 1.892(16) 2.7151(16) 168(2) 2_546 N3 H3A O7 0.86 2.28 3.135(4) 172.8 . N5 H5A O7 0.86 2.56 3.282(4) 141.5 . N6 H6A O7 0.86 2.11 2.950(3) 166.0 . N9 H9A O7 0.86 2.27 3.124(4) 175.0 . N2 H2A O8 0.86 2.24 3.034(3) 154.3 . N5 H5A O8 0.86 2.73 3.252(3) 120.3 3_566 N6 H6A O8 0.86 2.70 3.340(3) 132.6 3_566 N8 H8A O8 0.86 2.08 2.908(3) 161.0 3_566 N9 H9A O8 0.86 2.65 3.355(3) 140.5 3_566 N2 H2A O9 0.86 2.17 2.970(3) 155.0 3_566 N3 H3A O9 0.86 2.39 3.140(3) 146.5 3_566 N5 H5A O9 0.86 2.36 2.986(3) 129.8 . N9 H9A O9 0.86 2.42 3.168(3) 145.5 3_566 N3 H3A O10 0.86 2.80 3.511(3) 141.1 3_566 N5 H5A O10 0.86 1.96 2.822(3) 178.6 3_566 N6 H6A O10 0.86 2.76 3.444(3) 137.7 3_566 N8 H8A O10 0.86 2.18 2.946(3) 147.5 . O6 H6B N1 0.854(16) 1.943(16) 2.789(2) 170(2) . O5 H5D N4 0.850(16) 1.879(16) 2.727(2) 175(2) 4_666 O4 H4A N7 0.863(15) 1.865(16) 2.728(2) 180(2) 2_446 _diffrn_measured_fraction_theta_max 0.949 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.209 _refine_diff_density_min -0.247 _refine_diff_density_rms 0.038 ########################### data_zn _database_code_depnum_ccdc_archive 'CCDC 670348' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H72 N20 O16 S Zn' _chemical_formula_weight 1282.69 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 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 12.4531(11) _cell_length_b 18.4139(17) _cell_length_c 13.1241(12) _cell_angle_alpha 90.00 _cell_angle_beta 91.499(1) _cell_angle_gamma 90.00 _cell_volume 3008.5(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.416 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1348 _exptl_absorpt_coefficient_mu 0.525 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7479 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details SADABS _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 'Bruker APEX II CCD area detector' _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 18094 _diffrn_reflns_av_R_equivalents 0.0342 _diffrn_reflns_av_sigmaI/netI 0.0452 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 28.41 _reflns_number_total 7126 _reflns_number_gt 4687 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2006)' _computing_cell_refinement 'SAINT (Bruker, 2006)' _computing_data_reduction SAINT _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. The hydrogen atoms on water molecules are located by Foureir difference syntheses and the bond distances of O-H are fixed as 0.85(2) \%A. ; _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^)+(0.0484P)^2^+0.1561P] 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 7126 _refine_ls_number_parameters 427 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0695 _refine_ls_R_factor_gt 0.0388 _refine_ls_wR_factor_ref 0.1042 _refine_ls_wR_factor_gt 0.0905 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _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 0.0000 0.0000 0.5000 0.03015(10) Uani 1 2 d S . . S1 S 0.0000 0.5000 0.5000 0.03777(17) Uani 1 2 d S . . O1 O 0.40012(12) 0.42447(8) 0.31521(12) 0.0541(4) Uani 1 1 d . . . O2 O -0.01878(11) 0.78554(8) 0.35375(11) 0.0451(4) Uani 1 1 d . . . O3 O 0.22029(10) 0.59981(8) 0.85567(10) 0.0393(3) Uani 1 1 d . . . O4 O -0.10649(11) 0.00655(9) 0.62075(11) 0.0438(4) Uani 1 1 d D . . H4A H -0.1701(15) 0.0193(14) 0.613(2) 0.080 Uiso 1 1 d D . . H4B H -0.084(2) 0.0307(14) 0.6685(17) 0.080 Uiso 1 1 d D . . O5 O 0.12027(12) 0.00218(8) 0.60818(12) 0.0444(4) Uani 1 1 d D . . H5C H 0.1662(18) 0.0354(12) 0.612(2) 0.080 Uiso 1 1 d D . . H5D H 0.129(2) -0.0314(12) 0.6484(18) 0.080 Uiso 1 1 d D . . O6 O 0.00555(12) 0.11368(8) 0.49060(11) 0.0422(3) Uani 1 1 d D . . H6B H 0.0532(17) 0.1353(14) 0.4568(18) 0.080 Uiso 1 1 d D . . H6C H 0.001(2) 0.1368(14) 0.5442(15) 0.080 Uiso 1 1 d D . . N1 N 0.16013(18) 0.20104(11) 0.39795(16) 0.0613(5) Uani 1 1 d . . . N2 N 0.24614(14) 0.39002(10) 0.39338(14) 0.0487(5) Uani 1 1 d . . . H2A H 0.1908 0.4063 0.4239 0.058 Uiso 1 1 calc R . . N3 N 0.29684(17) 0.50919(10) 0.38805(15) 0.0578(5) Uani 1 1 d . . . H3A H 0.2397 0.5180 0.4214 0.069 Uiso 1 1 calc R . . N4 N -0.31954(15) 0.60951(11) 0.23538(15) 0.0569(5) Uani 1 1 d . . . N5 N -0.06756(13) 0.66608(9) 0.35816(13) 0.0462(4) Uani 1 1 d . . . H5A H -0.0428 0.6230 0.3678 0.055 Uiso 1 1 calc R . . N6 N 0.09256(14) 0.70248(10) 0.42871(15) 0.0516(5) Uani 1 1 d . . . H6A H 0.1005 0.6577 0.4461 0.062 Uiso 1 1 calc R . . N8 N 0.06380(12) 0.57117(10) 0.77061(13) 0.0458(5) Uani 1 1 d . . . H8A H 0.0364 0.5592 0.7122 0.055 Uiso 1 1 calc R . . N9 N 0.21868(13) 0.58745(10) 0.68423(13) 0.0486(5) Uani 1 1 d . . . H9A H 0.1819 0.5744 0.6309 0.058 Uiso 1 1 calc R . . N10 N 0.31080(12) 0.65449(9) 0.49518(12) 0.0369(4) Uani 1 1 d . . . C18 C -0.05971(18) 0.60073(14) 1.02031(18) 0.0592(7) Uani 1 1 d . . . H18A H -0.0449 0.6191 1.0851 0.071 Uiso 1 1 calc R . . C1 C 0.2479(2) 0.16706(14) 0.36918(18) 0.0591(6) Uani 1 1 d . . . H1A H 0.2485 0.1166 0.3689 0.071 Uiso 1 1 calc R . . C2 C 0.3381(2) 0.20345(13) 0.33975(18) 0.0575(6) Uani 1 1 d . . . H2B H 0.3970 0.1777 0.3167 0.069 Uiso 1 1 calc R . . C3 C 0.34139(17) 0.27831(13) 0.34443(18) 0.0512(6) Uani 1 1 d . . . H3B H 0.4021 0.3036 0.3247 0.061 Uiso 1 1 calc R . . C4 C 0.25195(16) 0.31515(12) 0.37932(15) 0.0411(5) Uani 1 1 d . . . C5 C 0.16265(19) 0.27347(13) 0.40250(18) 0.0546(6) Uani 1 1 d . . . H5B H 0.1010 0.2975 0.4224 0.066 Uiso 1 1 calc R . . C6 C 0.32054(17) 0.44065(12) 0.36309(16) 0.0429(5) Uani 1 1 d . . . C7 C 0.3661(2) 0.56906(13) 0.35978(18) 0.0612(7) Uani 1 1 d . . . H7A H 0.3284 0.5994 0.3102 0.073 Uiso 1 1 calc R . . H7B H 0.4295 0.5498 0.3279 0.073 Uiso 1 1 calc R . . C8 C 0.40002(17) 0.61455(12) 0.44989(17) 0.0475(5) Uani 1 1 d . . . H8B H 0.4329 0.5833 0.5014 0.057 Uiso 1 1 calc R . . H8C H 0.4540 0.6491 0.4288 0.057 Uiso 1 1 calc R . . C9 C -0.38121(18) 0.66730(14) 0.24989(18) 0.0540(6) Uani 1 1 d . . . H9B H -0.4516 0.6666 0.2245 0.065 Uiso 1 1 calc R . . C10 C -0.34494(17) 0.72780(13) 0.30078(18) 0.0500(6) Uani 1 1 d . . . H10A H -0.3907 0.7670 0.3103 0.060 Uiso 1 1 calc R . . C11 C -0.24072(17) 0.73054(11) 0.33780(16) 0.0439(5) Uani 1 1 d . . . H11A H -0.2154 0.7713 0.3727 0.053 Uiso 1 1 calc R . . C12 C -0.17418(16) 0.67168(11) 0.32222(15) 0.0372(5) Uani 1 1 d . . . C13 C -0.21856(18) 0.61239(12) 0.27112(17) 0.0496(6) Uani 1 1 d . . . H13A H -0.1750 0.5721 0.2612 0.059 Uiso 1 1 calc R . . C14 C 0.00101(16) 0.72241(12) 0.37938(15) 0.0389(5) Uani 1 1 d . . . C15 C 0.17823(17) 0.75329(12) 0.4538(2) 0.0542(6) Uani 1 1 d . . . H15A H 0.1742 0.7672 0.5249 0.065 Uiso 1 1 calc R . . H15B H 0.1692 0.7968 0.4127 0.065 Uiso 1 1 calc R . . C16 C 0.28764(16) 0.72014(12) 0.43486(18) 0.0478(5) Uani 1 1 d . . . H16A H 0.2919 0.7082 0.3631 0.057 Uiso 1 1 calc R . . H16B H 0.3426 0.7561 0.4504 0.057 Uiso 1 1 calc R . . C17 C -0.15886(18) 0.57334(14) 0.9970(2) 0.0600(7) Uani 1 1 d . . . H17A H -0.2112 0.5746 1.0463 0.072 Uiso 1 1 calc R . . N7 N -0.18341(14) 0.54492(12) 0.90633(16) 0.0609(6) Uani 1 1 d . . . C21 C -0.10798(17) 0.54506(14) 0.83669(17) 0.0533(6) Uani 1 1 d . . . H21A H -0.1250 0.5253 0.7731 0.064 Uiso 1 1 calc R . . C20 C -0.00559(15) 0.57276(11) 0.85291(15) 0.0393(5) Uani 1 1 d . . . C19 C 0.01867(17) 0.60131(13) 0.94836(17) 0.0503(6) Uani 1 1 d . . . H19A H 0.0864 0.6204 0.9635 0.060 Uiso 1 1 calc R . . C22 C 0.17196(15) 0.58697(11) 0.77476(15) 0.0357(4) Uani 1 1 d . . . C23 C 0.33012(16) 0.60947(14) 0.67332(16) 0.0516(6) Uani 1 1 d . . . H23A H 0.3711 0.5689 0.6477 0.062 Uiso 1 1 calc R . . H23B H 0.3604 0.6228 0.7396 0.062 Uiso 1 1 calc R . . C24 C 0.33926(16) 0.67318(12) 0.60115(16) 0.0468(5) Uani 1 1 d . . . H24A H 0.2925 0.7119 0.6234 0.056 Uiso 1 1 calc R . . H24B H 0.4124 0.6913 0.6044 0.056 Uiso 1 1 calc R . . O7 O 0.0798(3) 0.54909(19) 0.4916(3) 0.0702(10) Uani 0.50 1 d P . . O9 O -0.1093(2) 0.52711(17) 0.4651(2) 0.0483(7) Uani 0.50 1 d P . . O8 O 0.0164(2) 0.43072(16) 0.4397(2) 0.0487(7) Uani 0.50 1 d P . . O10 O -0.0163(3) 0.47420(17) 0.6078(2) 0.0539(8) Uani 0.50 1 d P . . 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 0.02711(16) 0.02941(18) 0.03379(17) -0.00030(13) -0.00186(12) 0.00030(13) S1 0.0396(4) 0.0355(4) 0.0379(4) -0.0002(3) -0.0030(3) 0.0045(4) O1 0.0507(9) 0.0444(9) 0.0684(11) 0.0067(8) 0.0214(8) 0.0031(7) O2 0.0473(8) 0.0318(8) 0.0558(9) 0.0035(7) -0.0058(7) -0.0015(7) O3 0.0312(7) 0.0466(9) 0.0399(8) -0.0010(6) -0.0058(6) -0.0003(6) O4 0.0323(7) 0.0596(11) 0.0395(8) -0.0028(7) 0.0041(6) 0.0047(7) O5 0.0405(8) 0.0401(9) 0.0516(9) 0.0098(7) -0.0176(7) -0.0077(7) O6 0.0492(9) 0.0279(8) 0.0496(9) 0.0001(6) 0.0042(7) -0.0034(7) N1 0.0730(14) 0.0486(13) 0.0626(13) 0.0003(10) 0.0104(11) -0.0195(11) N2 0.0456(10) 0.0426(11) 0.0588(12) -0.0015(9) 0.0174(9) -0.0003(9) N3 0.0660(13) 0.0428(13) 0.0659(13) -0.0096(9) 0.0263(11) -0.0062(10) N4 0.0548(12) 0.0492(12) 0.0657(13) -0.0175(10) -0.0167(10) -0.0009(10) N5 0.0465(10) 0.0263(9) 0.0650(12) 0.0007(8) -0.0128(9) 0.0014(8) N6 0.0425(10) 0.0347(10) 0.0767(14) 0.0068(9) -0.0144(9) -0.0020(8) N8 0.0318(8) 0.0674(13) 0.0381(9) -0.0058(9) -0.0030(7) -0.0091(9) N9 0.0355(9) 0.0719(14) 0.0382(10) -0.0019(9) -0.0001(7) -0.0127(9) N10 0.0316(8) 0.0395(10) 0.0395(9) -0.0025(7) 0.0007(7) -0.0032(7) C18 0.0518(14) 0.0754(19) 0.0507(14) -0.0115(13) 0.0085(11) -0.0078(13) C1 0.0846(18) 0.0389(14) 0.0535(15) 0.0041(11) -0.0037(13) -0.0082(14) C2 0.0610(15) 0.0460(15) 0.0653(16) 0.0015(12) -0.0015(12) 0.0076(12) C3 0.0429(12) 0.0459(14) 0.0649(15) 0.0073(12) 0.0014(11) -0.0026(11) C4 0.0447(11) 0.0422(13) 0.0362(11) 0.0018(9) 0.0001(9) -0.0047(10) C5 0.0547(14) 0.0543(15) 0.0555(14) -0.0008(12) 0.0139(11) -0.0083(12) C6 0.0447(12) 0.0418(13) 0.0422(12) 0.0026(10) 0.0022(10) -0.0004(10) C7 0.0880(19) 0.0414(14) 0.0552(15) -0.0031(11) 0.0199(13) -0.0050(13) C8 0.0442(12) 0.0444(14) 0.0547(14) 0.0005(10) 0.0114(10) -0.0034(10) C9 0.0439(12) 0.0581(16) 0.0594(15) -0.0047(12) -0.0082(11) -0.0039(12) C10 0.0414(12) 0.0435(13) 0.0652(15) -0.0036(11) -0.0008(10) 0.0039(10) C11 0.0481(12) 0.0346(12) 0.0488(13) -0.0050(9) -0.0030(10) -0.0047(10) C12 0.0436(11) 0.0309(11) 0.0369(11) 0.0030(9) -0.0046(9) -0.0032(9) C13 0.0534(13) 0.0379(13) 0.0569(14) -0.0111(10) -0.0085(11) 0.0027(11) C14 0.0416(11) 0.0331(12) 0.0418(12) -0.0013(9) 0.0003(9) 0.0001(10) C15 0.0445(12) 0.0404(13) 0.0767(17) -0.0061(12) -0.0127(11) 0.0002(11) C16 0.0423(12) 0.0414(13) 0.0594(14) 0.0014(11) -0.0038(10) -0.0072(10) C17 0.0465(13) 0.0741(18) 0.0602(16) 0.0057(13) 0.0160(12) -0.0079(13) N7 0.0366(10) 0.0872(17) 0.0590(13) 0.0053(12) 0.0044(9) -0.0121(10) C21 0.0370(11) 0.0743(18) 0.0485(13) 0.0019(12) -0.0041(10) -0.0090(12) C20 0.0332(10) 0.0412(12) 0.0435(12) 0.0051(9) -0.0014(9) -0.0014(9) C19 0.0396(11) 0.0609(16) 0.0503(14) -0.0095(11) 0.0020(10) -0.0099(11) C22 0.0331(10) 0.0317(11) 0.0421(11) 0.0018(9) -0.0009(9) -0.0003(9) C23 0.0328(11) 0.0781(18) 0.0441(13) 0.0050(12) 0.0023(9) -0.0040(11) C24 0.0369(11) 0.0575(15) 0.0460(12) -0.0092(11) 0.0007(9) -0.0118(11) O7 0.053(2) 0.050(2) 0.108(3) 0.008(2) 0.000(2) -0.0237(17) O9 0.0393(16) 0.0473(18) 0.0579(19) 0.0053(15) -0.0035(14) 0.0085(14) O8 0.0600(19) 0.0443(19) 0.0418(17) -0.0086(13) 0.0008(14) 0.0083(15) O10 0.078(2) 0.0443(18) 0.0395(17) 0.0032(14) 0.0015(15) 0.0133(17) _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 2.0370(13) 3_556 ? Zn1 O5 2.0370(13) . ? Zn1 O4 2.0963(14) 3_556 ? Zn1 O4 2.0963(14) . ? Zn1 O6 2.0982(15) 3_556 ? Zn1 O6 2.0982(15) . ? S1 O7 1.350(3) . ? S1 O7 1.350(3) 3_566 ? S1 O9 1.510(3) . ? S1 O9 1.510(3) 3_566 ? S1 O10 1.511(3) 3_566 ? S1 O10 1.511(3) . ? S1 O8 1.518(3) 3_566 ? S1 O8 1.518(3) . ? O1 C6 1.224(2) . ? O2 C14 1.233(2) . ? O3 C22 1.230(2) . ? O4 H4A 0.830(16) . ? O4 H4B 0.813(16) . ? O5 H5C 0.838(17) . ? O5 H5D 0.819(16) . ? O6 H6B 0.849(16) . ? O6 H6C 0.826(16) . ? N1 C1 1.323(3) . ? N1 C5 1.335(3) . ? N2 C6 1.380(3) . ? N2 C4 1.393(3) . ? N2 H2A 0.8600 . ? N3 C6 1.339(3) . ? N3 C7 1.454(3) . ? N3 H3A 0.8600 . ? N4 C9 1.329(3) . ? N4 C13 1.332(3) . ? N5 C14 1.368(2) . ? N5 C12 1.401(2) . ? N5 H5A 0.8600 . ? N6 C14 1.347(2) . ? N6 C15 1.450(3) . ? N6 H6A 0.8600 . ? N8 C22 1.378(2) . ? N8 C20 1.401(3) . ? N8 H8A 0.8600 . ? N9 C22 1.336(2) . ? N9 C23 1.456(2) . ? N9 H9A 0.8600 . ? N10 C24 1.467(2) . ? N10 C16 1.469(3) . ? N10 C8 1.471(2) . ? C18 C17 1.361(3) . ? C18 C19 1.376(3) . ? C18 H18A 0.9300 . ? C1 C2 1.372(3) . ? C1 H1A 0.9300 . ? C2 C3 1.380(3) . ? C2 H2B 0.9300 . ? C3 C4 1.392(3) . ? C3 H3B 0.9300 . ? C4 C5 1.391(3) . ? C5 H5B 0.9300 . ? C7 C8 1.501(3) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C9 C10 1.369(3) . ? C9 H9B 0.9300 . ? C10 C11 1.375(3) . ? C10 H10A 0.9300 . ? C11 C12 1.383(3) . ? C11 H11A 0.9300 . ? C12 C13 1.388(3) . ? C13 H13A 0.9300 . ? C15 C16 1.519(3) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 N7 1.329(3) . ? C17 H17A 0.9300 . ? N7 C21 1.328(3) . ? C21 C20 1.385(3) . ? C21 H21A 0.9300 . ? C20 C19 1.385(3) . ? C19 H19A 0.9300 . ? C23 C24 1.514(3) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? O7 O9 1.554(5) 3_566 ? O7 O8 1.563(4) 3_566 ? O7 O10 1.568(5) 3_566 ? O9 O7 1.554(5) 3_566 ? O8 O7 1.563(4) 3_566 ? O10 O7 1.568(5) 3_566 ? 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 O5 180.00(6) 3_556 . ? O5 Zn1 O4 86.56(6) 3_556 3_556 ? O5 Zn1 O4 93.44(6) . 3_556 ? O5 Zn1 O4 93.44(6) 3_556 . ? O5 Zn1 O4 86.56(6) . . ? O4 Zn1 O4 180.0 3_556 . ? O5 Zn1 O6 89.80(6) 3_556 3_556 ? O5 Zn1 O6 90.20(6) . 3_556 ? O4 Zn1 O6 90.55(6) 3_556 3_556 ? O4 Zn1 O6 89.45(6) . 3_556 ? O5 Zn1 O6 90.20(6) 3_556 . ? O5 Zn1 O6 89.80(6) . . ? O4 Zn1 O6 89.45(6) 3_556 . ? O4 Zn1 O6 90.55(6) . . ? O6 Zn1 O6 180.0 3_556 . ? O7 S1 O7 180.0(2) . 3_566 ? O7 S1 O9 114.45(19) . . ? O7 S1 O9 65.55(19) 3_566 . ? O7 S1 O9 65.55(19) . 3_566 ? O7 S1 O9 114.45(19) 3_566 3_566 ? O9 S1 O9 180.000(1) . 3_566 ? O7 S1 O10 66.2(2) . 3_566 ? O7 S1 O10 113.8(2) 3_566 3_566 ? O9 S1 O10 75.79(16) . 3_566 ? O9 S1 O10 104.21(16) 3_566 3_566 ? O7 S1 O10 113.8(2) . . ? O7 S1 O10 66.2(2) 3_566 . ? O9 S1 O10 104.21(16) . . ? O9 S1 O10 75.79(16) 3_566 . ? O10 S1 O10 180.000(1) 3_566 . ? O7 S1 O8 65.7(2) . 3_566 ? O7 S1 O8 114.3(2) 3_566 3_566 ? O9 S1 O8 75.41(16) . 3_566 ? O9 S1 O8 104.59(16) 3_566 3_566 ? O10 S1 O8 104.31(16) 3_566 3_566 ? O10 S1 O8 75.69(16) . 3_566 ? O7 S1 O8 114.3(2) . . ? O7 S1 O8 65.7(2) 3_566 . ? O9 S1 O8 104.59(16) . . ? O9 S1 O8 75.41(16) 3_566 . ? O10 S1 O8 75.69(16) 3_566 . ? O10 S1 O8 104.31(16) . . ? O8 S1 O8 180.000(1) 3_566 . ? Zn1 O4 H4A 122.9(18) . . ? Zn1 O4 H4B 114(2) . . ? H4A O4 H4B 104(3) . . ? Zn1 O5 H5C 123.1(18) . . ? Zn1 O5 H5D 121.5(19) . . ? H5C O5 H5D 115(3) . . ? Zn1 O6 H6B 121.6(18) . . ? Zn1 O6 H6C 117(2) . . ? H6B O6 H6C 106(3) . . ? C1 N1 C5 117.8(2) . . ? C6 N2 C4 126.36(18) . . ? C6 N2 H2A 116.8 . . ? C4 N2 H2A 116.8 . . ? C6 N3 C7 121.1(2) . . ? C6 N3 H3A 119.5 . . ? C7 N3 H3A 119.5 . . ? C9 N4 C13 117.49(19) . . ? C14 N5 C12 126.43(17) . . ? C14 N5 H5A 116.8 . . ? C12 N5 H5A 116.8 . . ? C14 N6 C15 122.79(18) . . ? C14 N6 H6A 118.6 . . ? C15 N6 H6A 118.6 . . ? C22 N8 C20 125.96(17) . . ? C22 N8 H8A 117.0 . . ? C20 N8 H8A 117.0 . . ? C22 N9 C23 121.83(17) . . ? C22 N9 H9A 119.1 . . ? C23 N9 H9A 119.1 . . ? C24 N10 C16 110.91(17) . . ? C24 N10 C8 109.52(16) . . ? C16 N10 C8 109.47(16) . . ? C17 C18 C19 120.3(2) . . ? C17 C18 H18A 119.8 . . ? C19 C18 H18A 119.8 . . ? N1 C1 C2 122.6(2) . . ? N1 C1 H1A 118.7 . . ? C2 C1 H1A 118.7 . . ? C1 C2 C3 119.9(2) . . ? C1 C2 H2B 120.1 . . ? C3 C2 H2B 120.1 . . ? C2 C3 C4 118.6(2) . . ? C2 C3 H3B 120.7 . . ? C4 C3 H3B 120.7 . . ? C5 C4 C3 117.0(2) . . ? C5 C4 N2 118.2(2) . . ? C3 C4 N2 124.80(19) . . ? N1 C5 C4 124.0(2) . . ? N1 C5 H5B 118.0 . . ? C4 C5 H5B 118.0 . . ? O1 C6 N3 122.8(2) . . ? O1 C6 N2 122.8(2) . . ? N3 C6 N2 114.36(19) . . ? N3 C7 C8 112.26(19) . . ? N3 C7 H7A 109.2 . . ? C8 C7 H7A 109.2 . . ? N3 C7 H7B 109.2 . . ? C8 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? N10 C8 C7 113.42(18) . . ? N10 C8 H8B 108.9 . . ? C7 C8 H8B 108.9 . . ? N10 C8 H8C 108.9 . . ? C7 C8 H8C 108.9 . . ? H8B C8 H8C 107.7 . . ? N4 C9 C10 122.5(2) . . ? N4 C9 H9B 118.8 . . ? C10 C9 H9B 118.8 . . ? C9 C10 C11 119.9(2) . . ? C9 C10 H10A 120.0 . . ? C11 C10 H10A 120.0 . . ? C10 C11 C12 118.9(2) . . ? C10 C11 H11A 120.6 . . ? C12 C11 H11A 120.6 . . ? C11 C12 C13 117.08(19) . . ? C11 C12 N5 125.04(18) . . ? C13 C12 N5 117.81(19) . . ? N4 C13 C12 124.2(2) . . ? N4 C13 H13A 117.9 . . ? C12 C13 H13A 117.9 . . ? O2 C14 N6 123.26(19) . . ? O2 C14 N5 122.69(18) . . ? N6 C14 N5 114.03(18) . . ? N6 C15 C16 111.17(18) . . ? N6 C15 H15A 109.4 . . ? C16 C15 H15A 109.4 . . ? N6 C15 H15B 109.4 . . ? C16 C15 H15B 109.4 . . ? H15A C15 H15B 108.0 . . ? N10 C16 C15 114.00(18) . . ? N10 C16 H16A 108.8 . . ? C15 C16 H16A 108.8 . . ? N10 C16 H16B 108.8 . . ? C15 C16 H16B 108.8 . . ? H16A C16 H16B 107.6 . . ? N7 C17 C18 122.2(2) . . ? N7 C17 H17A 118.9 . . ? C18 C17 H17A 118.9 . . ? C21 N7 C17 117.8(2) . . ? N7 C21 C20 124.1(2) . . ? N7 C21 H21A 118.0 . . ? C20 C21 H21A 118.0 . . ? C21 C20 C19 117.2(2) . . ? C21 C20 N8 117.25(19) . . ? C19 C20 N8 125.52(18) . . ? C18 C19 C20 118.4(2) . . ? C18 C19 H19A 120.8 . . ? C20 C19 H19A 120.8 . . ? O3 C22 N9 123.48(18) . . ? O3 C22 N8 122.05(18) . . ? N9 C22 N8 114.47(17) . . ? N9 C23 C24 111.39(18) . . ? N9 C23 H23A 109.4 . . ? C24 C23 H23A 109.4 . . ? N9 C23 H23B 109.4 . . ? C24 C23 H23B 109.4 . . ? H23A C23 H23B 108.0 . . ? N10 C24 C23 113.02(18) . . ? N10 C24 H24A 109.0 . . ? C23 C24 H24A 109.0 . . ? N10 C24 H24B 109.0 . . ? C23 C24 H24B 109.0 . . ? H24A C24 H24B 107.8 . . ? S1 O7 O9 62.18(17) . 3_566 ? S1 O7 O8 62.30(18) . 3_566 ? O9 O7 O8 100.5(3) 3_566 3_566 ? S1 O7 O10 61.84(18) . 3_566 ? O9 O7 O10 99.6(2) 3_566 3_566 ? O8 O7 O10 99.6(2) 3_566 3_566 ? S1 O9 O7 52.27(14) . 3_566 ? S1 O8 O7 51.97(15) . 3_566 ? S1 O10 O7 51.99(15) . 3_566 ? 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 C5 N1 C1 C2 -3.1(4) . . . . ? N1 C1 C2 C3 3.3(4) . . . . ? C1 C2 C3 C4 0.0(3) . . . . ? C2 C3 C4 C5 -3.1(3) . . . . ? C2 C3 C4 N2 176.3(2) . . . . ? C6 N2 C4 C5 -171.4(2) . . . . ? C6 N2 C4 C3 9.2(3) . . . . ? C1 N1 C5 C4 -0.3(4) . . . . ? C3 C4 C5 N1 3.4(3) . . . . ? N2 C4 C5 N1 -176.0(2) . . . . ? C7 N3 C6 O1 -0.5(4) . . . . ? C7 N3 C6 N2 -178.8(2) . . . . ? C4 N2 C6 O1 3.2(3) . . . . ? C4 N2 C6 N3 -178.5(2) . . . . ? C6 N3 C7 C8 -125.8(2) . . . . ? C24 N10 C8 C7 157.85(18) . . . . ? C16 N10 C8 C7 -80.3(2) . . . . ? N3 C7 C8 N10 -66.8(3) . . . . ? C13 N4 C9 C10 -1.0(4) . . . . ? N4 C9 C10 C11 0.9(4) . . . . ? C9 C10 C11 C12 0.3(3) . . . . ? C10 C11 C12 C13 -1.2(3) . . . . ? C10 C11 C12 N5 -178.0(2) . . . . ? C14 N5 C12 C11 -26.0(3) . . . . ? C14 N5 C12 C13 157.2(2) . . . . ? C9 N4 C13 C12 0.0(4) . . . . ? C11 C12 C13 N4 1.1(3) . . . . ? N5 C12 C13 N4 178.1(2) . . . . ? C15 N6 C14 O2 -1.9(3) . . . . ? C15 N6 C14 N5 176.8(2) . . . . ? C12 N5 C14 O2 -11.8(3) . . . . ? C12 N5 C14 N6 169.49(19) . . . . ? C14 N6 C15 C16 -138.4(2) . . . . ? C24 N10 C16 C15 -76.5(2) . . . . ? C8 N10 C16 C15 162.52(17) . . . . ? N6 C15 C16 N10 -60.3(3) . . . . ? C19 C18 C17 N7 1.5(4) . . . . ? C18 C17 N7 C21 -1.2(4) . . . . ? C17 N7 C21 C20 0.2(4) . . . . ? N7 C21 C20 C19 0.6(4) . . . . ? N7 C21 C20 N8 -177.9(2) . . . . ? C22 N8 C20 C21 -170.9(2) . . . . ? C22 N8 C20 C19 10.8(3) . . . . ? C17 C18 C19 C20 -0.7(4) . . . . ? C21 C20 C19 C18 -0.3(3) . . . . ? N8 C20 C19 C18 178.0(2) . . . . ? C23 N9 C22 O3 -5.3(3) . . . . ? C23 N9 C22 N8 174.36(19) . . . . ? C20 N8 C22 O3 5.0(3) . . . . ? C20 N8 C22 N9 -174.66(19) . . . . ? C22 N9 C23 C24 -121.3(2) . . . . ? C16 N10 C24 C23 162.08(17) . . . . ? C8 N10 C24 C23 -77.0(2) . . . . ? N9 C23 C24 N10 -67.9(2) . . . . ? O7 S1 O7 O9 159(6) 3_566 . . 3_566 ? O9 S1 O7 O9 180.0 . . . 3_566 ? O10 S1 O7 O9 -119.7(2) 3_566 . . 3_566 ? O10 S1 O7 O9 60.3(2) . . . 3_566 ? O8 S1 O7 O9 120.6(2) 3_566 . . 3_566 ? O8 S1 O7 O9 -59.4(2) . . . 3_566 ? O7 S1 O7 O8 39(6) 3_566 . . 3_566 ? O9 S1 O7 O8 59.4(2) . . . 3_566 ? O9 S1 O7 O8 -120.6(2) 3_566 . . 3_566 ? O10 S1 O7 O8 119.7(2) 3_566 . . 3_566 ? O10 S1 O7 O8 -60.3(2) . . . 3_566 ? O8 S1 O7 O8 180.0 . . . 3_566 ? O7 S1 O7 O10 -81(6) 3_566 . . 3_566 ? O9 S1 O7 O10 -60.3(2) . . . 3_566 ? O9 S1 O7 O10 119.7(2) 3_566 . . 3_566 ? O10 S1 O7 O10 180.0 . . . 3_566 ? O8 S1 O7 O10 -119.7(2) 3_566 . . 3_566 ? O8 S1 O7 O10 60.3(2) . . . 3_566 ? O7 S1 O9 O7 180.0 . . . 3_566 ? O9 S1 O9 O7 0(100) 3_566 . . 3_566 ? O10 S1 O9 O7 125.0(2) 3_566 . . 3_566 ? O10 S1 O9 O7 -55.0(2) . . . 3_566 ? O8 S1 O9 O7 -125.8(2) 3_566 . . 3_566 ? O8 S1 O9 O7 54.2(2) . . . 3_566 ? O7 S1 O8 O7 180.0 . . . 3_566 ? O9 S1 O8 O7 -54.1(2) . . . 3_566 ? O9 S1 O8 O7 125.9(2) 3_566 . . 3_566 ? O10 S1 O8 O7 -124.9(2) 3_566 . . 3_566 ? O10 S1 O8 O7 55.1(2) . . . 3_566 ? O8 S1 O8 O7 -131(50) 3_566 . . 3_566 ? O7 S1 O10 O7 180.0 . . . 3_566 ? O9 S1 O10 O7 54.6(2) . . . 3_566 ? O9 S1 O10 O7 -125.4(2) 3_566 . . 3_566 ? O10 S1 O10 O7 129(100) 3_566 . . 3_566 ? O8 S1 O10 O7 125.2(2) 3_566 . . 3_566 ? O8 S1 O10 O7 -54.8(2) . . . 3_566 ? 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 C3 H3B O1 0.93 2.23 2.818(3) 120.5 . O4 H4B O1 0.813(16) 2.108(19) 2.850(2) 152(3) 4_566 C11 H11A O2 0.93 2.48 2.946(2) 111.0 . O6 H6C O2 0.826(16) 1.968(18) 2.762(2) 161(3) 3_566 C19 H19A O3 0.93 2.25 2.819(2) 119.0 . O5 H5C O3 0.838(17) 1.884(17) 2.7111(19) 169(3) 2_546 N3 H3A O7 0.86 2.29 3.144(4) 172.6 . N5 H5A O7 0.86 2.59 3.303(4) 141.4 . N6 H6A O7 0.86 2.11 2.948(4) 166.2 . N9 H9A O7 0.86 2.25 3.106(4) 175.4 . N2 H2A O8 0.86 2.23 3.035(3) 155.0 . N5 H5A O8 0.86 2.72 3.246(3) 120.4 3_566 N6 H6A O8 0.86 2.67 3.311(4) 132.2 3_566 N8 H8A O8 0.86 2.09 2.911(3) 159.3 3_566 N9 H9A O8 0.86 2.62 3.328(3) 140.9 3_566 N2 H2A O9 0.86 2.18 2.974(3) 154.4 3_566 N3 H3A O9 0.86 2.38 3.138(4) 147.1 3_566 N5 H5A O9 0.86 2.34 2.971(4) 130.2 . N9 H9A O9 0.86 2.42 3.163(4) 145.5 3_566 N3 H3A O10 0.86 2.80 3.508(4) 140.5 3_566 N5 H5A O10 0.86 1.96 2.818(4) 178.5 3_566 N6 H6A O10 0.86 2.73 3.419(4) 138.0 3_566 N8 H8A O10 0.86 2.17 2.939(4) 148.6 . O6 H6B N1 0.849(16) 1.972(17) 2.810(2) 169(3) . O5 H5D N4 0.819(16) 1.933(17) 2.741(2) 169(3) 4_666 O4 H4A N7 0.830(16) 1.895(17) 2.724(2) 178(3) 2_446 _diffrn_measured_fraction_theta_max 0.942 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.230 _refine_diff_density_min -0.421 _refine_diff_density_rms 0.051 ###############END