# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2003 data_(1) _audit_creation_method 'SHELXL' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C15 H35 N6 O11 S Zn' _chemical_formula_weight 572.92 _chemical_melting_point ? _chemical_compound_source ? 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 12.285(3) _cell_length_b 16.375(3) _cell_length_c 12.407(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.45(3) _cell_angle_gamma 90.00 _cell_volume 2495.1(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 27 _cell_measurement_theta_min 5.23 _cell_measurement_theta_max 10.56 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.525 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1204 _exptl_absorpt_coefficient_mu 1.132 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.21371 _exptl_absorpt_correction_T_max 0.30843 _exptl_special_details ; Correction for absorption was applied using a psi-scan technique. (North et al., 1968) ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4 diffractometer' _diffrn_measurement_method \w--2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 5604 _diffrn_reflns_av_R_equivalents 0.0359 _diffrn_reflns_av_sigmaI/netI 0.0857 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 25.01 _reflns_number_total 4388 _reflns_number_observed 2705 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_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 w=1/[\s^2^(Fo^2^)+(0.0769P)^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 4388 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0844 _refine_ls_R_factor_gt 0.0513 _refine_ls_wR_factor_all 0.1373 _refine_ls_wR_factor_ref 0.1282 _refine_ls_goodness_of_fit_all 0.905 _refine_ls_goodness_of_fit_ref 1.101 _refine_ls_restrained_S_all 0.905 _refine_ls_restrained_S_obs 1.101 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Zn1 Zn 0.74913(4) 0.78052(3) 0.81522(4) 0.0369(2) Uani 1 d . . S1 S 0.57294(10) 0.67820(8) 0.62473(9) 0.0374(3) Uani 1 d . . O1 O 0.6300(4) 0.7224(3) 0.7100(3) 0.088(2) Uani 1 d . . O2 O 0.6103(8) 0.7170(6) 0.5224(6) 0.065(2) Uani 0.50 d P . O2' O 0.6373(8) 0.6483(9) 0.5357(8) 0.095(3) Uani 0.50 d P . O3 O 0.6077(10) 0.5987(5) 0.6344(9) 0.098(3) Uani 0.50 d P . O3' O 0.5192(8) 0.6069(6) 0.6759(8) 0.082(3) Uani 0.50 d P . O4 O 0.4559(7) 0.6829(7) 0.6235(7) 0.063(2) Uani 0.50 d P . O4' O 0.4912(8) 0.7311(6) 0.5876(9) 0.075(3) Uani 0.50 d P . N1 N 0.7191(3) 0.8852(2) 0.7359(3) 0.0355(9) Uani 1 d . . N2 N 0.6877(3) 0.9628(2) 0.5948(3) 0.0411(10) Uani 1 d . . N3 N 0.8784(3) 0.7213(2) 0.7567(3) 0.0377(9) Uani 1 d . . N4 N 0.9819(3) 0.6545(2) 0.6455(3) 0.0449(10) Uani 1 d . . N5 N 0.6808(3) 0.7257(2) 0.9400(3) 0.0348(9) Uani 1 d . . N6 N 0.5642(3) 0.6543(2) 1.0340(3) 0.0406(10) Uani 1 d . . C1 C 0.7372(4) 0.9648(3) 0.7633(4) 0.0442(12) Uani 1 d . . H1 H 0.7601(4) 0.9830(3) 0.8312(4) 0.080 Uiso 1 calc R . C2 C 0.7171(4) 1.0130(3) 0.6775(4) 0.0496(13) Uani 1 d . . H2 H 0.7222(4) 1.0696(3) 0.6753(4) 0.080 Uiso 1 calc R . C3 C 0.6888(4) 0.8870(3) 0.6322(4) 0.0389(11) Uani 1 d . . H3 H 0.6709(4) 0.8411(3) 0.5914(4) 0.080 Uiso 1 calc R . C4 C 0.6564(4) 0.9867(4) 0.4847(4) 0.057(2) Uani 1 d . . H4A H 0.6568(4) 0.9389(4) 0.4387(4) 0.080 Uiso 1 calc R . H4B H 0.7096(4) 1.0250(4) 0.4580(4) 0.080 Uiso 1 calc R . C5 C 0.5444(4) 1.0258(4) 0.4786(5) 0.062(2) Uani 1 d . . H5A H 0.5470(4) 1.0767(4) 0.5185(5) 0.080 Uiso 1 calc R . H5B H 0.5270(4) 1.0388(4) 0.4039(5) 0.080 Uiso 1 calc R . C6 C 0.8839(4) 0.6873(3) 0.6604(4) 0.0447(12) Uani 1 d . . H6 H 0.8270(4) 0.6863(3) 0.6096(4) 0.080 Uiso 1 calc R . C7 C 0.9785(4) 0.7097(3) 0.8048(4) 0.0494(13) Uani 1 d . . H7 H 0.9991(4) 0.7274(3) 0.8736(4) 0.080 Uiso 1 calc R . C8 C 1.0427(5) 0.6685(4) 0.7370(5) 0.060(2) Uani 1 d . . H8 H 1.1146(5) 0.6527(4) 0.7502(5) 0.080 Uiso 1 calc R . C9 C 1.0178(5) 0.6102(3) 0.5496(4) 0.0544(15) Uani 1 d . . H9A H 1.0967(5) 0.6106(3) 0.5483(4) 0.080 Uiso 1 calc R . H9B H 0.9905(5) 0.6379(3) 0.4853(4) 0.080 Uiso 1 calc R . C10 C 0.9777(4) 0.5227(3) 0.5487(4) 0.0497(14) Uani 1 d . . H10A H 0.8988(4) 0.5219(3) 0.5453(4) 0.080 Uiso 1 calc R . H10B H 1.0016(4) 0.4955(3) 0.6146(4) 0.080 Uiso 1 calc R . C11 C 0.7231(4) 0.7114(3) 1.0418(4) 0.0503(13) Uani 1 d . . H11 H 0.7906(4) 0.7297(3) 1.0674(4) 0.080 Uiso 1 calc R . C12 C 0.6534(4) 0.6677(3) 1.0984(4) 0.0526(14) Uani 1 d . . H12 H 0.6638(4) 0.6496(3) 1.1690(4) 0.080 Uiso 1 calc R . C13 C 0.5846(4) 0.6893(3) 0.9386(4) 0.0400(11) Uani 1 d . . H13 H 0.5370(4) 0.6881(3) 0.8791(4) 0.080 Uiso 1 calc R . C14 C 0.4674(4) 0.6060(3) 1.0591(5) 0.0530(14) Uani 1 d . . H14A H 0.4093(4) 0.6189(3) 1.0075(5) 0.080 Uiso 1 calc R . H14B H 0.4430(4) 0.6209(3) 1.1302(5) 0.080 Uiso 1 calc R . C15 C 0.4893(5) 0.5161(3) 1.0563(4) 0.0531(14) Uani 1 d . . H15A H 0.4273(5) 0.4874(3) 1.0849(4) 0.080 Uiso 1 calc R . H15B H 0.5520(5) 0.5042(3) 1.1028(4) 0.080 Uiso 1 calc R . OW1 O 0.8581(3) 0.8533(2) 0.9303(3) 0.0466(9) Uani 1 d . . OW2 O 0.7906(5) 0.7346(4) 0.4036(5) 0.113(2) Uani 1 d . . OW3 O 0.7156(4) 1.0164(3) 1.2303(4) 0.093(2) Uani 1 d . . OW4 O 0.8144(4) 1.0123(3) 1.0366(4) 0.105(2) Uani 1 d . . OW5 O 1.0036(4) 0.9480(3) 0.8298(4) 0.100(2) Uani 1 d . . OW6 O 0.4226(4) 0.8498(3) 0.7614(4) 0.097(2) Uani 1 d . . OW7 O 0.3218(4) 0.6271(3) 0.7862(4) 0.0845(14) Uani 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 0.0440(3) 0.0347(3) 0.0320(3) 0.0044(3) 0.0021(2) 0.0016(3) S1 0.0364(7) 0.0426(7) 0.0330(6) -0.0029(5) -0.0059(5) -0.0036(6) O1 0.111(4) 0.105(4) 0.047(2) 0.012(2) -0.034(2) -0.065(3) O2 0.098(7) 0.075(6) 0.023(4) 0.006(4) 0.005(4) -0.005(6) O2' 0.074(7) 0.144(10) 0.069(7) -0.038(7) 0.032(5) -0.013(7) O3 0.126(9) 0.045(5) 0.125(9) 0.012(6) 0.035(8) 0.039(6) O3' 0.079(6) 0.060(6) 0.106(8) 0.016(5) 0.002(6) -0.024(5) O4 0.044(5) 0.089(7) 0.057(5) 0.007(5) 0.000(4) -0.003(5) O4' 0.073(7) 0.067(7) 0.082(7) -0.013(5) -0.037(6) 0.024(5) N1 0.040(2) 0.036(2) 0.031(2) 0.002(2) -0.003(2) 0.004(2) N2 0.042(2) 0.047(2) 0.034(2) 0.011(2) -0.003(2) 0.007(2) N3 0.043(2) 0.038(2) 0.032(2) -0.005(2) 0.001(2) 0.005(2) N4 0.051(3) 0.043(2) 0.041(2) -0.005(2) 0.006(2) 0.000(2) N5 0.039(2) 0.034(2) 0.031(2) 0.002(2) -0.001(2) -0.002(2) N6 0.044(2) 0.040(2) 0.038(2) 0.005(2) 0.010(2) 0.001(2) C1 0.051(3) 0.040(3) 0.041(3) -0.003(2) 0.003(2) 0.007(2) C2 0.056(3) 0.034(3) 0.059(4) 0.002(3) 0.002(3) 0.005(2) C3 0.041(3) 0.042(3) 0.033(3) 0.004(2) -0.005(2) 0.003(2) C4 0.059(3) 0.072(4) 0.042(3) 0.023(3) 0.007(3) 0.013(3) C5 0.064(4) 0.073(4) 0.049(3) 0.027(3) -0.003(3) 0.007(3) C6 0.051(3) 0.044(3) 0.039(3) -0.003(2) -0.001(2) 0.002(3) C7 0.056(3) 0.049(3) 0.043(3) -0.008(3) -0.011(2) 0.015(3) C8 0.053(3) 0.071(4) 0.057(4) -0.005(3) -0.009(3) 0.020(3) C9 0.069(4) 0.049(3) 0.047(3) -0.011(3) 0.025(3) -0.002(3) C10 0.056(3) 0.047(3) 0.047(3) -0.008(3) 0.017(3) -0.001(3) C11 0.048(3) 0.063(3) 0.039(3) 0.007(3) -0.014(2) -0.006(3) C12 0.062(3) 0.062(4) 0.034(3) 0.015(3) -0.006(3) -0.009(3) C13 0.043(3) 0.041(3) 0.036(3) 0.002(2) -0.002(2) 0.002(2) C14 0.051(3) 0.051(3) 0.059(3) 0.003(3) 0.020(3) 0.000(3) C15 0.056(3) 0.051(3) 0.054(3) 0.008(3) 0.022(3) -0.006(3) OW1 0.051(2) 0.050(2) 0.039(2) -0.004(2) -0.012(2) -0.006(2) OW2 0.117(4) 0.120(5) 0.105(4) 0.029(4) 0.030(3) 0.026(4) OW3 0.119(4) 0.092(4) 0.069(3) 0.008(3) 0.009(3) 0.023(3) OW4 0.131(4) 0.109(4) 0.076(3) -0.003(3) 0.024(3) 0.003(4) OW5 0.120(4) 0.080(3) 0.101(4) -0.002(3) 0.042(3) -0.023(3) OW6 0.118(4) 0.079(3) 0.095(4) -0.001(3) 0.025(3) 0.013(3) OW7 0.077(3) 0.086(3) 0.091(3) -0.012(3) 0.019(3) 0.007(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 N5 1.993(4) . yes Zn1 N1 2.007(4) . yes Zn1 N3 2.012(4) . yes Zn1 O1 2.157(4) . yes Zn1 OW1 2.270(3) . yes S1 O3 1.374(8) . ? S1 O4' 1.395(8) . ? S1 O4 1.440(8) . ? S1 O1 1.448(4) . ? S1 O2' 1.459(9) . ? S1 O3' 1.491(8) . ? S1 O2 1.501(7) . ? O2 O2' 1.182(13) . ? O2 O4' 1.705(14) . ? O2' O3 1.522(15) . ? O3 O3' 1.221(12) . ? O3' O4 1.597(13) . ? O4 O4' 1.010(11) . ? N1 C3 1.330(6) . ? N1 C1 1.364(6) . ? N2 C3 1.326(6) . ? N2 C2 1.356(6) . ? N2 C4 1.463(6) . ? N3 C6 1.322(6) . ? N3 C7 1.367(6) . ? N4 C6 1.335(6) . ? N4 C8 1.363(7) . ? N4 C9 1.470(6) . ? N5 C13 1.323(6) . ? N5 C11 1.374(6) . ? N6 C13 1.343(6) . ? N6 C12 1.358(6) . ? N6 C14 1.469(6) . ? C1 C2 1.342(7) . ? C4 C5 1.517(7) . ? C5 C5 1.489(11) 3_676 ? C7 C8 1.348(7) . ? C9 C10 1.516(7) . ? C10 C10 1.531(9) 3_766 ? C11 C12 1.331(7) . ? C14 C15 1.498(7) . ? C15 C15 1.522(10) 3_667 ? 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 N5 Zn1 N1 133.61(15) . . yes N5 Zn1 N3 114.5(2) . . yes N1 Zn1 N3 111.9(2) . . yes N5 Zn1 O1 88.8(2) . . yes N1 Zn1 O1 88.1(2) . . yes N3 Zn1 O1 95.7(2) . . yes N5 Zn1 OW1 90.06(14) . . yes N1 Zn1 OW1 87.62(14) . . yes N3 Zn1 OW1 91.24(14) . . yes O1 Zn1 OW1 172.8(2) . . yes O3 S1 O4' 146.7(7) . . ? O3 S1 O4 111.0(7) . . ? O4' S1 O4 41.7(5) . . ? O3 S1 O1 105.5(6) . . ? O4' S1 O1 105.2(4) . . ? O4 S1 O1 116.5(4) . . ? O3 S1 O2' 64.9(7) . . ? O4' S1 O2' 110.9(7) . . ? O4 S1 O2' 124.7(5) . . ? O1 S1 O2' 117.3(5) . . ? O3 S1 O3' 50.3(5) . . ? O4' S1 O3' 107.7(7) . . ? O4 S1 O3' 66.0(6) . . ? O1 S1 O3' 107.0(4) . . ? O2' S1 O3' 108.3(7) . . ? O3 S1 O2 111.9(6) . . ? O4' S1 O2 72.0(6) . . ? O4 S1 O2 107.2(5) . . ? O1 S1 O2 104.7(4) . . ? O2' S1 O2 47.0(5) . . ? O3' S1 O2 147.0(5) . . ? S1 O1 Zn1 166.2(3) . . ? O2' O2 S1 64.6(6) . . ? O2' O2 O4' 107.7(8) . . ? S1 O2 O4' 51.1(4) . . ? O2 O2' S1 68.4(7) . . ? O2 O2' O3 123.2(9) . . ? S1 O2' O3 54.9(5) . . ? O3' O3 S1 69.8(6) . . ? O3' O3 O2' 120.9(10) . . ? S1 O3 O2' 60.2(6) . . ? O3 O3' S1 59.9(6) . . ? O3 O3' O4 110.1(8) . . ? S1 O3' O4 55.5(4) . . ? O4' O4 S1 66.8(7) . . ? O4' O4 O3' 125.3(10) . . ? S1 O4 O3' 58.5(5) . . ? O4 O4' S1 71.5(8) . . ? O4 O4' O2 119.1(10) . . ? S1 O4' O2 56.9(5) . . ? C3 N1 C1 105.1(4) . . ? C3 N1 Zn1 122.4(3) . . ? C1 N1 Zn1 131.9(3) . . ? C3 N2 C2 107.6(4) . . ? C3 N2 C4 125.3(5) . . ? C2 N2 C4 127.1(4) . . ? C6 N3 C7 105.6(4) . . ? C6 N3 Zn1 126.0(3) . . ? C7 N3 Zn1 128.3(3) . . ? C6 N4 C8 107.1(4) . . ? C6 N4 C9 126.8(5) . . ? C8 N4 C9 126.0(5) . . ? C13 N5 C11 104.6(4) . . ? C13 N5 Zn1 125.9(3) . . ? C11 N5 Zn1 129.3(3) . . ? C13 N6 C12 106.5(4) . . ? C13 N6 C14 125.9(4) . . ? C12 N6 C14 127.4(4) . . ? C2 C1 N1 109.8(5) . . ? C1 C2 N2 106.5(4) . . ? N2 C3 N1 111.0(4) . . ? N2 C4 C5 112.0(4) . . ? C5 C5 C4 114.6(6) 3_676 . ? N3 C6 N4 111.2(4) . . ? C8 C7 N3 109.4(5) . . ? C7 C8 N4 106.7(5) . . ? N4 C9 C10 111.6(4) . . ? C9 C10 C10 110.0(5) . 3_766 ? C12 C11 N5 110.1(4) . . ? C11 C12 N6 107.2(4) . . ? N5 C13 N6 111.6(4) . . ? N6 C14 C15 112.2(4) . . ? C14 C15 C15 113.4(6) . 3_667 ? 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 O3 S1 O1 Zn1 64.7(13) . . . . ? O4' S1 O1 Zn1 -128.5(13) . . . . ? O4 S1 O1 Zn1 -171.6(12) . . . . ? O2' S1 O1 Zn1 -4.6(15) . . . . ? O3' S1 O1 Zn1 117.2(12) . . . . ? O2 S1 O1 Zn1 -53.5(13) . . . . ? N5 Zn1 O1 S1 -130.9(12) . . . . ? N1 Zn1 O1 S1 95.4(12) . . . . ? N3 Zn1 O1 S1 -16.4(12) . . . . ? OW1 Zn1 O1 S1 148.4(11) . . . . ? O3 S1 O2 O2' 0.1(10) . . . . ? O4' S1 O2 O2' -144.6(9) . . . . ? O4 S1 O2 O2' -121.8(8) . . . . ? O1 S1 O2 O2' 113.9(7) . . . . ? O2' S1 O2 O2' 0.000(5) . . . . ? O3' S1 O2 O2' -49.7(13) . . . . ? O3 S1 O2 O4' 144.8(7) . . . . ? O4' S1 O2 O4' 0.000(3) . . . . ? O4 S1 O2 O4' 22.8(6) . . . . ? O1 S1 O2 O4' -101.5(5) . . . . ? O2' S1 O2 O4' 144.6(9) . . . . ? O3' S1 O2 O4' 94.9(11) . . . . ? S1 O2 O2' S1 0.000(4) . . . . ? O4' O2 O2' S1 -28.2(6) . . . . ? S1 O2 O2' O3 -0.1(10) . . . . ? O4' O2 O2' O3 -28.3(14) . . . . ? O3 S1 O2' O2 -179.9(10) . . . . ? O4' S1 O2' O2 36.1(9) . . . . ? O4 S1 O2' O2 81.1(9) . . . . ? O1 S1 O2' O2 -84.7(8) . . . . ? O3' S1 O2' O2 154.1(7) . . . . ? O2 S1 O2' O2 0.000(5) . . . . ? O3 S1 O2' O3 0.000(5) . . . . ? O4' S1 O2' O3 -144.0(8) . . . . ? O4 S1 O2' O3 -99.1(9) . . . . ? O1 S1 O2' O3 95.1(7) . . . . ? O3' S1 O2' O3 -26.0(8) . . . . ? O2 S1 O2' O3 179.9(10) . . . . ? O4' S1 O3 O3' -56.9(15) . . . . ? O4 S1 O3 O3' -27.6(9) . . . . ? O1 S1 O3 O3' 99.5(7) . . . . ? O2' S1 O3 O3' -147.2(10) . . . . ? O3' S1 O3 O3' 0.000(3) . . . . ? O2 S1 O3 O3' -147.3(7) . . . . ? O4' S1 O3 O2' 90.3(13) . . . . ? O4 S1 O3 O2' 119.6(6) . . . . ? O1 S1 O3 O2' -113.3(5) . . . . ? O2' S1 O3 O2' 0.000(5) . . . . ? O3' S1 O3 O2' 147.2(10) . . . . ? O2 S1 O3 O2' -0.1(8) . . . . ? O2 O2' O3 O3' 36.5(18) . . . . ? S1 O2' O3 O3' 36.4(9) . . . . ? O2 O2' O3 S1 0.1(11) . . . . ? S1 O2' O3 S1 0.000(6) . . . . ? S1 O3 O3' S1 0.000(3) . . . . ? O2' O3 O3' S1 -33.3(9) . . . . ? S1 O3 O3' O4 24.5(8) . . . . ? O2' O3 O3' O4 -8.7(15) . . . . ? O3 S1 O3' O3 0.000(3) . . . . ? O4' S1 O3' O3 151.2(8) . . . . ? O4 S1 O3' O3 151.8(10) . . . . ? O1 S1 O3' O3 -96.2(8) . . . . ? O2' S1 O3' O3 31.1(9) . . . . ? O2 S1 O3' O3 67.1(12) . . . . ? O3 S1 O3' O4 -151.8(9) . . . . ? O4' S1 O3' O4 -0.6(7) . . . . ? O4 S1 O3' O4 0.000(1) . . . . ? O1 S1 O3' O4 112.0(5) . . . . ? O2' S1 O3' O4 -120.7(6) . . . . ? O2 S1 O3' O4 -84.6(11) . . . . ? O3 S1 O4 O4' -156.2(9) . . . . ? O4' S1 O4 O4' 0.000(1) . . . . ? O1 S1 O4 O4' 83.1(8) . . . . ? O2' S1 O4 O4' -82.8(12) . . . . ? O3' S1 O4 O4' -179.1(10) . . . . ? O2 S1 O4 O4' -33.6(10) . . . . ? O3 S1 O4 O3' 22.9(7) . . . . ? O4' S1 O4 O3' 179.1(10) . . . . ? O1 S1 O4 O3' -97.8(5) . . . . ? O2' S1 O4 O3' 96.3(9) . . . . ? O3' S1 O4 O3' 0.0 . . . . ? O2 S1 O4 O3' 145.5(6) . . . . ? O3 O3' O4 O4' -24.8(17) . . . . ? S1 O3' O4 O4' 1.0(12) . . . . ? O3 O3' O4 S1 -25.8(8) . . . . ? S1 O3' O4 S1 0.000(1) . . . . ? S1 O4 O4' S1 0.000(1) . . . . ? O3' O4 O4' S1 -0.9(11) . . . . ? S1 O4 O4' O2 32.3(8) . . . . ? O3' O4 O4' O2 31.3(17) . . . . ? O3 S1 O4' O4 43.4(16) . . . . ? O4 S1 O4' O4 0.000(1) . . . . ? O1 S1 O4' O4 -113.0(8) . . . . ? O2' S1 O4' O4 119.2(9) . . . . ? O3' S1 O4' O4 0.8(10) . . . . ? O2 S1 O4' O4 146.2(10) . . . . ? O3 S1 O4' O2 -102.8(12) . . . . ? O4 S1 O4' O2 -146.2(10) . . . . ? O1 S1 O4' O2 100.8(4) . . . . ? O2' S1 O4' O2 -27.0(6) . . . . ? O3' S1 O4' O2 -145.3(6) . . . . ? O2 S1 O4' O2 0.000(3) . . . . ? O2' O2 O4' O4 -3.9(15) . . . . ? S1 O2 O4' O4 -37.2(10) . . . . ? O2' O2 O4' S1 33.3(8) . . . . ? S1 O2 O4' S1 0.000(4) . . . . ? N5 Zn1 N1 C3 -117.1(4) . . . . ? N3 Zn1 N1 C3 64.8(4) . . . . ? O1 Zn1 N1 C3 -30.6(4) . . . . ? OW1 Zn1 N1 C3 155.1(4) . . . . ? N5 Zn1 N1 C1 73.4(5) . . . . ? N3 Zn1 N1 C1 -104.8(4) . . . . ? O1 Zn1 N1 C1 159.9(4) . . . . ? OW1 Zn1 N1 C1 -14.4(4) . . . . ? N5 Zn1 N3 C6 114.1(4) . . . . ? N1 Zn1 N3 C6 -67.3(4) . . . . ? O1 Zn1 N3 C6 22.9(4) . . . . ? OW1 Zn1 N3 C6 -155.3(4) . . . . ? N5 Zn1 N3 C7 -68.1(4) . . . . ? N1 Zn1 N3 C7 110.5(4) . . . . ? O1 Zn1 N3 C7 -159.3(4) . . . . ? OW1 Zn1 N3 C7 22.6(4) . . . . ? N1 Zn1 N5 C13 72.2(4) . . . . ? N3 Zn1 N5 C13 -109.7(4) . . . . ? O1 Zn1 N5 C13 -14.0(4) . . . . ? OW1 Zn1 N5 C13 159.0(4) . . . . ? N1 Zn1 N5 C11 -113.1(4) . . . . ? N3 Zn1 N5 C11 65.0(5) . . . . ? O1 Zn1 N5 C11 160.7(4) . . . . ? OW1 Zn1 N5 C11 -26.4(4) . . . . ? C3 N1 C1 C2 0.6(5) . . . . ? Zn1 N1 C1 C2 171.4(3) . . . . ? N1 C1 C2 N2 -1.0(6) . . . . ? C3 N2 C2 C1 1.1(6) . . . . ? C4 N2 C2 C1 179.2(4) . . . . ? C2 N2 C3 N1 -0.7(5) . . . . ? C4 N2 C3 N1 -178.9(4) . . . . ? C1 N1 C3 N2 0.1(5) . . . . ? Zn1 N1 C3 N2 -171.8(3) . . . . ? C3 N2 C4 C5 105.1(6) . . . . ? C2 N2 C4 C5 -72.7(7) . . . . ? N2 C4 C5 C5 -56.6(9) . . . 3_676 ? C7 N3 C6 N4 0.3(6) . . . . ? Zn1 N3 C6 N4 178.5(3) . . . . ? C8 N4 C6 N3 -0.3(6) . . . . ? C9 N4 C6 N3 178.8(4) . . . . ? C6 N3 C7 C8 -0.3(6) . . . . ? Zn1 N3 C7 C8 -178.4(4) . . . . ? N3 C7 C8 N4 0.1(6) . . . . ? C6 N4 C8 C7 0.1(6) . . . . ? C9 N4 C8 C7 -179.0(5) . . . . ? C6 N4 C9 C10 -79.7(6) . . . . ? C8 N4 C9 C10 99.2(6) . . . . ? N4 C9 C10 C10 -176.7(5) . . . 3_766 ? C13 N5 C11 C12 0.1(6) . . . . ? Zn1 N5 C11 C12 -175.5(4) . . . . ? N5 C11 C12 N6 -1.0(6) . . . . ? C13 N6 C12 C11 1.4(6) . . . . ? C14 N6 C12 C11 177.1(5) . . . . ? C11 N5 C13 N6 0.8(5) . . . . ? Zn1 N5 C13 N6 176.6(3) . . . . ? C12 N6 C13 N5 -1.5(6) . . . . ? C14 N6 C13 N5 -177.2(4) . . . . ? C13 N6 C14 C15 100.7(6) . . . . ? C12 N6 C14 C15 -74.2(7) . . . . ? N6 C14 C15 C15 -68.0(8) . . . 3_667 ? _refine_diff_density_max 0.629 _refine_diff_density_min -0.547 _refine_diff_density_rms 0.086 #===END data_(2) _audit_creation_method 'SHELXL' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C15 H29 N8 O10 Zn' _chemical_formula_weight 546.83 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.335(2) _cell_length_b 11.173(2) _cell_length_c 13.049(3) _cell_angle_alpha 87.36(3) _cell_angle_beta 83.12(3) _cell_angle_gamma 83.49(3) _cell_volume 1198.0(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 4.79 _cell_measurement_theta_max 11.02 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.44 _exptl_crystal_size_min 0.42 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.516 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 570 _exptl_absorpt_coefficient_mu 1.091 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.27530 _exptl_absorpt_correction_T_max 0.31826 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4 diffractometer' _diffrn_measurement_method \w--2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 4352 _diffrn_reflns_av_R_equivalents 0.1789 _diffrn_reflns_av_sigmaI/netI 0.1787 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3466 _reflns_number_observed 2443 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_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 w=1/[\s^2^(Fo^2^)+(0.0698P)^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 3466 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0653 _refine_ls_R_factor_gt 0.0428 _refine_ls_wR_factor_all 0.1141 _refine_ls_wR_factor_ref 0.1082 _refine_ls_goodness_of_fit_all 0.894 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 0.894 _refine_ls_restrained_S_obs 1.028 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Zn Zn -0.04760(6) -0.19010(5) 0.28474(4) 0.0391(2) Uani 1 d . . O1 O 0.2072(8) -0.2454(6) 0.9308(5) 0.161(3) Uani 1 d . . O2 O 0.0119(11) -0.3490(6) 0.9660(4) 0.166(3) Uani 1 d . . O3 O 0.1288(5) -0.3380(4) 0.8130(3) 0.0838(12) Uani 1 d . . O4 O -0.2047(8) -0.2705(6) 0.5582(6) 0.177(3) Uani 1 d . . O5 O -0.3806(7) -0.1164(6) 0.5701(4) 0.120(2) Uani 1 d . . O6 O -0.3853(6) -0.2598(4) 0.6865(4) 0.0910(13) Uani 1 d . . N1 N 0.0876(4) -0.2534(3) 0.3964(3) 0.0392(9) Uani 1 d . . N2 N 0.2121(4) -0.3676(4) 0.5096(3) 0.0489(10) Uani 1 d . . N3 N -0.2487(4) -0.2561(3) 0.2496(2) 0.0359(8) Uani 1 d . . N4 N -0.4132(4) -0.3695(3) 0.1898(3) 0.0398(9) Uani 1 d . . N5 N 0.0568(4) -0.0571(3) 0.2029(3) 0.0395(9) Uani 1 d . . N6 N 0.1938(4) 0.0457(3) 0.0814(3) 0.0439(9) Uani 1 d . . N7 N 0.1108(8) -0.3144(5) 0.9045(5) 0.088(2) Uani 1 d . . N8 N -0.3230(7) -0.2144(6) 0.6032(5) 0.084(2) Uani 1 d . . C1 C 0.1288(5) -0.3647(4) 0.4280(3) 0.0444(11) Uani 1 d . . H1 H 0.1033(5) -0.4328(4) 0.3976(3) 0.080 Uiso 1 calc R . C2 C 0.1504(6) -0.1830(5) 0.4608(4) 0.0620(14) Uani 1 d . . H2 H 0.1414(6) -0.0993(5) 0.4570(4) 0.080 Uiso 1 calc R . C3 C 0.2272(7) -0.2525(5) 0.5306(4) 0.068(2) Uani 1 d . . H3 H 0.2802(7) -0.2265(5) 0.5829(4) 0.080 Uiso 1 calc R . C4 C 0.2776(6) -0.4764(5) 0.5655(4) 0.0642(15) Uani 1 d . . H4A H 0.2369(6) -0.5463(5) 0.5406(4) 0.080 Uiso 1 calc R . H4B H 0.2388(6) -0.4703(5) 0.6384(4) 0.080 Uiso 1 calc R . C5 C 0.4611(7) -0.4946(6) 0.5527(4) 0.074(2) Uani 1 d . . H5A H 0.5003(7) -0.4272(6) 0.5828(4) 0.080 Uiso 1 calc R . H5B H 0.4956(7) -0.5668(6) 0.5919(4) 0.080 Uiso 1 calc R . C6 C -0.2583(5) -0.3542(4) 0.1983(3) 0.0403(11) Uani 1 d . . H6 H -0.1691(5) -0.4058(4) 0.1716(3) 0.080 Uiso 1 calc R . C7 C -0.4076(5) -0.2071(4) 0.2753(3) 0.0434(11) Uani 1 d . . H7 H -0.4401(5) -0.1374(4) 0.3121(3) 0.080 Uiso 1 calc R . C8 C -0.5079(5) -0.2774(4) 0.2381(3) 0.0454(11) Uani 1 d . . H8 H -0.6208(5) -0.2648(4) 0.2444(3) 0.080 Uiso 1 calc R . C9 C -0.4690(6) -0.4699(4) 0.1396(3) 0.0490(12) Uani 1 d . . H9A H -0.5787(6) -0.4813(4) 0.1695(3) 0.080 Uiso 1 calc R . H9B H -0.3995(6) -0.5433(4) 0.1527(3) 0.080 Uiso 1 calc R . C10 C -0.4670(6) -0.4478(4) 0.0244(3) 0.0542(13) Uani 1 d . . H10A H -0.3567(6) -0.4402(4) -0.0064(3) 0.080 Uiso 1 calc R . H10B H -0.5332(6) -0.3729(4) 0.0108(3) 0.080 Uiso 1 calc R . C11 C 0.1211(5) -0.0543(4) 0.1051(3) 0.0429(11) Uani 1 d . . H11 H 0.1163(5) -0.1142(4) 0.0587(3) 0.080 Uiso 1 calc R . C12 C 0.0909(6) 0.0479(4) 0.2424(4) 0.0535(13) Uani 1 d . . H12 H 0.0594(6) 0.0720(4) 0.3097(4) 0.080 Uiso 1 calc R . C13 C 0.1774(6) 0.1109(4) 0.1682(4) 0.0556(13) Uani 1 d . . H13 H 0.2175(6) 0.1841(4) 0.1753(4) 0.080 Uiso 1 calc R . C14 C 0.2837(5) 0.0758(5) -0.0194(4) 0.0557(13) Uani 1 d . . H14A H 0.2487(5) 0.1581(5) -0.0403(4) 0.080 Uiso 1 calc R . H14B H 0.2595(5) 0.0230(5) -0.0712(4) 0.080 Uiso 1 calc R . C15 C 0.4667(6) 0.0617(5) -0.0127(4) 0.0649(15) Uani 1 d . . H15A H 0.5218(6) 0.0874(5) -0.0785(4) 0.080 Uiso 1 calc R . H15B H 0.4894(6) 0.1147(5) 0.0393(4) 0.080 Uiso 1 calc R . OW1 O -0.1834(4) -0.0575(3) 0.3842(2) 0.0515(8) Uani 1 d . . OW2 O 0.1080(3) -0.3279(3) 0.1756(2) 0.0489(8) Uani 1 d . . OW3 O 0.8654(6) -0.4392(3) 0.7529(4) 0.0997(15) Uani 1 d . . OW4 O 0.3335(5) -0.1025(4) 0.7467(3) 0.0966(14) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn 0.0359(3) 0.0439(3) 0.0404(3) -0.0005(2) -0.0115(2) -0.0102(2) O1 0.143(5) 0.180(6) 0.174(6) -0.119(5) -0.070(5) 0.028(4) O2 0.229(8) 0.177(7) 0.072(4) 0.045(4) 0.013(5) 0.008(6) O3 0.096(3) 0.093(3) 0.065(3) -0.028(2) -0.024(2) 0.006(2) O4 0.138(5) 0.148(5) 0.220(7) -0.016(5) 0.090(5) -0.015(5) O5 0.134(5) 0.128(5) 0.097(4) 0.018(4) -0.004(3) -0.020(4) O6 0.089(3) 0.106(3) 0.078(3) 0.004(3) 0.001(3) -0.027(3) N1 0.041(2) 0.042(2) 0.037(2) -0.006(2) -0.012(2) -0.003(2) N2 0.048(2) 0.056(3) 0.041(2) -0.001(2) -0.010(2) 0.003(2) N3 0.035(2) 0.040(2) 0.034(2) -0.002(2) -0.009(2) -0.007(2) N4 0.038(2) 0.046(2) 0.038(2) -0.006(2) -0.011(2) -0.010(2) N5 0.038(2) 0.040(2) 0.042(2) -0.003(2) -0.003(2) -0.007(2) N6 0.038(2) 0.047(2) 0.046(2) 0.006(2) -0.003(2) -0.004(2) N7 0.115(5) 0.078(4) 0.074(4) -0.025(4) -0.049(4) 0.027(4) N8 0.072(4) 0.094(4) 0.090(5) -0.018(4) 0.003(3) -0.027(4) C1 0.038(2) 0.055(3) 0.042(3) -0.003(3) -0.009(2) -0.008(2) C2 0.070(3) 0.052(3) 0.070(3) -0.017(3) -0.036(3) 0.003(3) C3 0.079(4) 0.066(4) 0.065(3) -0.020(3) -0.043(3) 0.003(3) C4 0.060(3) 0.072(4) 0.055(3) 0.021(3) -0.006(3) 0.008(3) C5 0.071(4) 0.082(4) 0.063(3) 0.025(4) -0.011(3) 0.015(3) C6 0.037(2) 0.046(3) 0.039(2) -0.007(2) -0.008(2) -0.005(2) C7 0.035(2) 0.048(3) 0.046(3) -0.006(2) -0.004(2) -0.002(2) C8 0.032(2) 0.055(3) 0.051(3) -0.007(3) -0.007(2) -0.005(2) C9 0.047(3) 0.051(3) 0.055(3) -0.010(3) -0.014(2) -0.016(2) C10 0.060(3) 0.056(3) 0.052(3) -0.013(3) -0.015(2) -0.018(2) C11 0.044(3) 0.047(3) 0.040(3) -0.006(3) -0.009(2) -0.005(2) C12 0.064(3) 0.048(3) 0.048(3) -0.015(3) 0.005(3) -0.016(3) C13 0.068(3) 0.044(3) 0.057(3) -0.014(3) 0.002(3) -0.018(3) C14 0.046(3) 0.070(3) 0.049(3) 0.021(3) -0.007(2) -0.006(3) C15 0.052(3) 0.076(4) 0.062(3) 0.024(3) 0.006(3) -0.010(3) OW1 0.054(2) 0.053(2) 0.049(2) -0.017(2) -0.003(2) -0.008(2) OW2 0.041(2) 0.051(2) 0.054(2) -0.013(2) -0.0010(15) -0.0035(14) OW3 0.116(4) 0.059(2) 0.133(4) -0.015(3) -0.039(3) -0.018(2) OW4 0.098(3) 0.090(3) 0.101(3) -0.020(3) -0.034(3) 0.026(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn N1 2.002(3) . yes Zn N5 2.007(3) . yes Zn N3 2.015(3) . yes Zn OW1 2.146(3) . yes Zn OW2 2.321(3) . yes O1 N7 1.261(8) . ? O2 N7 1.166(8) . ? O3 N7 1.222(6) . ? O4 N8 1.211(7) . ? O5 N8 1.226(7) . ? O6 N8 1.258(6) . ? N1 C1 1.314(5) . ? N1 C2 1.364(5) . ? N2 C1 1.336(5) . ? N2 C3 1.350(6) . ? N2 C4 1.474(6) . ? N3 C6 1.325(5) . ? N3 C7 1.383(5) . ? N4 C6 1.339(5) . ? N4 C8 1.354(5) . ? N4 C9 1.471(5) . ? N5 C11 1.325(5) . ? N5 C12 1.375(5) . ? N6 C11 1.336(5) . ? N6 C13 1.359(6) . ? N6 C14 1.479(5) . ? C2 C3 1.343(6) . ? C4 C5 1.510(7) . ? C5 C5 1.453(10) 2_646 ? C7 C8 1.354(6) . ? C9 C10 1.510(6) . ? C10 C10 1.539(8) 2_445 ? C12 C13 1.355(6) . ? C14 C15 1.528(6) . ? C15 C15 1.467(10) 2_655 ? 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 Zn N5 109.85(14) . . yes N1 Zn N3 126.21(14) . . yes N5 Zn N3 123.77(13) . . yes N1 Zn OW1 91.59(13) . . yes N5 Zn OW1 88.93(13) . . yes N3 Zn OW1 93.31(13) . . yes N1 Zn OW2 88.12(13) . . yes N5 Zn OW2 88.86(13) . . yes N3 Zn OW2 88.84(12) . . yes OW1 Zn OW2 177.53(11) . . yes C1 N1 C2 105.1(4) . . ? C1 N1 Zn 130.3(3) . . ? C2 N1 Zn 124.5(3) . . ? C1 N2 C3 107.5(4) . . ? C1 N2 C4 126.3(4) . . ? C3 N2 C4 126.2(4) . . ? C6 N3 C7 105.5(3) . . ? C6 N3 Zn 128.1(3) . . ? C7 N3 Zn 126.3(3) . . ? C6 N4 C8 107.4(3) . . ? C6 N4 C9 125.9(4) . . ? C8 N4 C9 126.7(4) . . ? C11 N5 C12 105.1(4) . . ? C11 N5 Zn 129.2(3) . . ? C12 N5 Zn 125.4(3) . . ? C11 N6 C13 107.6(4) . . ? C11 N6 C14 125.9(4) . . ? C13 N6 C14 126.4(4) . . ? O2 N7 O3 125.1(7) . . ? O2 N7 O1 119.6(7) . . ? O3 N7 O1 115.4(7) . . ? O4 N8 O5 121.9(7) . . ? O4 N8 O6 117.6(7) . . ? O5 N8 O6 120.5(6) . . ? N1 C1 N2 111.2(4) . . ? C3 C2 N1 110.0(4) . . ? C2 C3 N2 106.2(4) . . ? N2 C4 C5 112.8(4) . . ? C5 C5 C4 115.9(6) 2_646 . ? N3 C6 N4 111.2(4) . . ? C8 C7 N3 108.6(4) . . ? N4 C8 C7 107.3(4) . . ? N4 C9 C10 112.2(4) . . ? C9 C10 C10 110.5(5) . 2_445 ? N5 C11 N6 111.4(4) . . ? C13 C12 N5 109.7(4) . . ? C12 C13 N6 106.2(4) . . ? N6 C14 C15 110.7(4) . . ? C15 C15 C14 113.8(5) 2_655 . ? 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 N5 Zn N1 C1 -137.2(4) . . . . ? N3 Zn N1 C1 38.1(4) . . . . ? OW1 Zn N1 C1 133.4(4) . . . . ? OW2 Zn N1 C1 -49.1(4) . . . . ? N5 Zn N1 C2 46.6(4) . . . . ? N3 Zn N1 C2 -138.1(4) . . . . ? OW1 Zn N1 C2 -42.8(4) . . . . ? OW2 Zn N1 C2 134.7(4) . . . . ? N1 Zn N3 C6 -76.7(4) . . . . ? N5 Zn N3 C6 98.0(4) . . . . ? OW1 Zn N3 C6 -171.1(3) . . . . ? OW2 Zn N3 C6 10.2(3) . . . . ? N1 Zn N3 C7 103.0(4) . . . . ? N5 Zn N3 C7 -82.3(4) . . . . ? OW1 Zn N3 C7 8.6(3) . . . . ? OW2 Zn N3 C7 -170.2(3) . . . . ? N1 Zn N5 C11 113.9(4) . . . . ? N3 Zn N5 C11 -61.5(4) . . . . ? OW1 Zn N5 C11 -154.8(4) . . . . ? OW2 Zn N5 C11 26.3(4) . . . . ? N1 Zn N5 C12 -58.9(4) . . . . ? N3 Zn N5 C12 125.7(4) . . . . ? OW1 Zn N5 C12 32.4(4) . . . . ? OW2 Zn N5 C12 -146.5(4) . . . . ? C2 N1 C1 N2 0.8(5) . . . . ? Zn N1 C1 N2 -175.9(3) . . . . ? C3 N2 C1 N1 -0.9(5) . . . . ? C4 N2 C1 N1 179.9(4) . . . . ? C1 N1 C2 C3 -0.5(6) . . . . ? Zn N1 C2 C3 176.5(4) . . . . ? N1 C2 C3 N2 0.0(6) . . . . ? C1 N2 C3 C2 0.5(6) . . . . ? C4 N2 C3 C2 179.7(4) . . . . ? C1 N2 C4 C5 112.7(6) . . . . ? C3 N2 C4 C5 -66.4(7) . . . . ? N2 C4 C5 C5 -58.7(9) . . . 2_646 ? C7 N3 C6 N4 0.3(5) . . . . ? Zn N3 C6 N4 -180.0(3) . . . . ? C8 N4 C6 N3 -0.2(5) . . . . ? C9 N4 C6 N3 -178.7(4) . . . . ? C6 N3 C7 C8 -0.2(5) . . . . ? Zn N3 C7 C8 -180.0(3) . . . . ? C6 N4 C8 C7 0.0(5) . . . . ? C9 N4 C8 C7 178.6(4) . . . . ? N3 C7 C8 N4 0.1(5) . . . . ? C6 N4 C9 C10 -84.7(5) . . . . ? C8 N4 C9 C10 97.0(5) . . . . ? N4 C9 C10 C10 -177.6(5) . . . 2_445 ? C12 N5 C11 N6 0.3(5) . . . . ? Zn N5 C11 N6 -173.6(3) . . . . ? C13 N6 C11 N5 0.5(5) . . . . ? C14 N6 C11 N5 177.3(4) . . . . ? C11 N5 C12 C13 -1.1(5) . . . . ? Zn N5 C12 C13 173.2(3) . . . . ? N5 C12 C13 N6 1.4(6) . . . . ? C11 N6 C13 C12 -1.1(5) . . . . ? C14 N6 C13 C12 -177.9(4) . . . . ? C11 N6 C14 C15 -106.5(5) . . . . ? C13 N6 C14 C15 69.8(6) . . . . ? N6 C14 C15 C15 62.4(7) . . . 2_655 ? _refine_diff_density_max 0.441 _refine_diff_density_min -0.307 _refine_diff_density_rms 0.066 #===END data_(3) _audit_creation_method 'SHELXL' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C15 H33 Cd N6 O10 S' _chemical_formula_weight 601.93 _chemical_melting_point ? _chemical_compound_source ? 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' 'Cd' 'Cd' -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.561(2) _cell_length_b 11.054(2) _cell_length_c 13.012(3) _cell_angle_alpha 85.99(3) _cell_angle_beta 83.91(3) _cell_angle_gamma 85.62(3) _cell_volume 1218.5(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 4.72 _cell_measurement_theta_max 9.27 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.641 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 618 _exptl_absorpt_coefficient_mu 1.042 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.24952 _exptl_absorpt_correction_T_max 0.31971 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4 diffractometer' _diffrn_measurement_method \w--2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 5405 _diffrn_reflns_av_R_equivalents 0.0216 _diffrn_reflns_av_sigmaI/netI 0.0505 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 25.01 _reflns_number_total 4291 _reflns_number_observed 3474 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_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 w=1/[\s^2^(Fo^2^)+(0.0962P)^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 4291 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0627 _refine_ls_R_factor_gt 0.0511 _refine_ls_wR_factor_all 0.1503 _refine_ls_wR_factor_ref 0.1458 _refine_ls_goodness_of_fit_all 1.089 _refine_ls_goodness_of_fit_ref 1.183 _refine_ls_restrained_S_all 1.089 _refine_ls_restrained_S_obs 1.183 _refine_ls_shift/esd_max -0.039 _refine_ls_shift/esd_mean 0.007 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cd Cd 0.06271(5) -0.82653(4) 0.19662(3) 0.0327(2) Uani 1 d . . S S 0.1734(2) -1.13507(14) 0.15723(12) 0.0391(4) Uani 1 d . . O1 O 0.1766(6) -1.0237(4) 0.2122(4) 0.0510(12) Uani 1 d . . O2 O 0.2584(7) -1.1201(6) 0.0539(4) 0.069(2) Uani 1 d . . O3 O 0.0083(6) -1.1572(4) 0.1447(4) 0.0537(12) Uani 1 d . . O4 O 0.2450(7) -1.2365(4) 0.2168(4) 0.0584(13) Uani 1 d . . N1 N -0.0687(6) -0.6500(5) 0.1431(4) 0.0380(12) Uani 1 d . . N2 N -0.2005(6) -0.5241(5) 0.0403(4) 0.0402(12) Uani 1 d . . N3 N -0.0655(6) -0.8531(5) 0.3571(4) 0.0401(12) Uani 1 d . . N4 N -0.2023(6) -0.9484(6) 0.4871(4) 0.0460(13) Uani 1 d . . N5 N 0.2855(6) -0.7525(4) 0.2419(4) 0.0352(11) Uani 1 d . . N6 N 0.4454(7) -0.6377(5) 0.3065(4) 0.0481(14) Uani 1 d . . C1 C -0.1290(8) -0.6365(6) 0.0543(5) 0.0411(14) Uani 1 d . . H1 H -0.1233(8) -0.6965(6) 0.0070(5) 0.080 Uiso 1 calc R . C2 C -0.1013(8) -0.5413(6) 0.1887(5) 0.0417(15) Uani 1 d . . H2 H -0.0724(8) -0.5242(6) 0.2528(5) 0.080 Uiso 1 calc R . C3 C -0.1824(8) -0.4625(6) 0.1251(6) 0.048(2) Uani 1 d . . H3 H -0.2183(8) -0.3827(6) 0.1371(6) 0.080 Uiso 1 calc R . C4 C -0.2811(8) -0.4798(8) -0.0504(5) 0.055(2) Uani 1 d . . H4A H -0.2373(8) -0.5245(8) -0.1095(5) 0.080 Uiso 1 calc R . H4B H -0.2633(8) -0.3946(8) -0.0665(5) 0.080 Uiso 1 calc R . C5 C -0.4519(11) -0.4940(19) -0.0321(8) 0.182(9) Uani 1 d . . H5A H -0.4940(11) -0.4238(19) -0.0719(8) 0.080 Uiso 1 calc R . H5B H -0.4630(11) -0.5624(19) -0.0730(8) 0.080 Uiso 1 calc R . C6 C -0.1352(8) -0.9544(6) 0.3904(5) 0.045(2) Uani 1 d . . H6 H -0.1367(8) -1.0212(6) 0.3509(5) 0.080 Uiso 1 calc R . C7 C -0.0942(9) -0.7773(7) 0.4393(5) 0.049(2) Uani 1 d . . H7 H -0.0622(9) -0.6989(7) 0.4399(5) 0.080 Uiso 1 calc R . C8 C -0.1770(9) -0.8385(8) 0.5181(5) 0.057(2) Uani 1 d . . H8 H -0.2107(9) -0.8094(8) 0.5827(5) 0.080 Uiso 1 calc R . C9 C -0.2946(9) -1.0429(8) 0.5446(6) 0.065(2) Uani 1 d . . H9A H -0.2485(9) -1.1226(8) 0.5269(6) 0.080 Uiso 1 calc R . H9B H -0.2919(9) -1.0367(8) 0.6184(6) 0.080 Uiso 1 calc R . C10 C -0.4567(13) -1.0289(15) 0.5197(14) 0.191(10) Uani 1 d . . H10A H -0.4648(13) -1.1055(15) 0.4892(14) 0.080 Uiso 1 calc R . H10B H -0.5124(13) -1.0389(15) 0.5884(14) 0.080 Uiso 1 calc R . C11 C 0.2958(8) -0.6556(6) 0.2952(5) 0.0421(15) Uani 1 d . . H11 H 0.2097(8) -0.6065(6) 0.3212(5) 0.080 Uiso 1 calc R . C12 C 0.4396(8) -0.7979(7) 0.2198(5) 0.046(2) Uani 1 d . . H12 H 0.4705(8) -0.8661(7) 0.1827(5) 0.080 Uiso 1 calc R . C13 C 0.5385(8) -0.7291(7) 0.2598(5) 0.052(2) Uani 1 d . . H13 H 0.6476(8) -0.7410(7) 0.2564(5) 0.080 Uiso 1 calc R . C14 C 0.4994(12) -0.5379(8) 0.3588(6) 0.070(3) Uani 1 d . . H14A H 0.4443(12) -0.4625(8) 0.3360(6) 0.080 Uiso 1 calc R . H14B H 0.6108(12) -0.5314(8) 0.3380(6) 0.080 Uiso 1 calc R . C15 C 0.4745(10) -0.5528(7) 0.4735(5) 0.056(2) Uani 1 d . . H15A H 0.5326(10) -0.6267(7) 0.4966(5) 0.080 Uiso 1 calc R . H15B H 0.3636(10) -0.5620(7) 0.4942(5) 0.080 Uiso 1 calc R . OW1 O -0.1489(6) -0.9265(4) 0.1383(4) 0.0514(12) Uani 1 d . . OW2 O 0.1757(7) -0.8289(5) 0.0196(4) 0.0621(14) Uani 1 d . . OW3 O 0.4405(13) -0.9461(11) -0.0396(10) 0.169(5) Uani 1 d . . OW4 O 0.0488(19) -0.4359(13) 0.3921(12) 0.308(13) Uani 1 d . . OW5 O -0.5634(10) -0.7907(9) -0.2257(7) 0.122(3) Uani 1 d . . OW6 O 0.1658(8) -0.7389(6) 0.6731(5) 0.081(2) Uani 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 Cd 0.0326(3) 0.0340(3) 0.0332(3) -0.0048(2) -0.0082(2) -0.0041(2) S 0.0470(9) 0.0368(8) 0.0355(8) -0.0064(6) -0.0101(7) -0.0045(7) O1 0.062(3) 0.038(2) 0.058(3) -0.012(2) -0.030(3) 0.002(2) O2 0.073(4) 0.100(4) 0.037(3) -0.013(3) -0.004(3) -0.027(3) O3 0.052(3) 0.053(3) 0.061(3) -0.010(2) -0.017(2) -0.011(2) O4 0.066(3) 0.043(3) 0.066(3) 0.001(2) -0.015(3) 0.004(2) N1 0.037(3) 0.038(3) 0.040(3) -0.004(2) -0.009(2) 0.001(2) N2 0.032(3) 0.048(3) 0.041(3) 0.006(2) -0.007(2) -0.005(2) N3 0.037(3) 0.048(3) 0.035(3) -0.007(2) -0.003(2) -0.006(2) N4 0.034(3) 0.061(4) 0.043(3) 0.011(3) -0.008(2) -0.006(3) N5 0.038(3) 0.035(3) 0.035(3) -0.005(2) -0.009(2) -0.008(2) N6 0.053(4) 0.061(4) 0.035(3) -0.012(3) -0.003(3) -0.028(3) C1 0.044(4) 0.037(3) 0.045(3) -0.004(3) -0.014(3) -0.005(3) C2 0.043(4) 0.042(3) 0.041(3) -0.009(3) -0.011(3) -0.001(3) C3 0.045(4) 0.040(4) 0.058(4) -0.011(3) -0.008(3) 0.003(3) C4 0.039(4) 0.084(5) 0.040(4) 0.024(4) -0.010(3) -0.005(4) C5 0.038(5) 0.421(26) 0.076(7) 0.126(12) -0.028(5) -0.036(10) C6 0.041(4) 0.051(4) 0.043(4) 0.002(3) -0.006(3) -0.009(3) C7 0.051(4) 0.057(4) 0.042(4) -0.013(3) -0.006(3) -0.004(3) C8 0.049(4) 0.085(6) 0.036(4) -0.006(4) 0.003(3) -0.001(4) C9 0.043(4) 0.085(6) 0.063(5) 0.042(4) -0.012(4) -0.017(4) C10 0.062(7) 0.228(16) 0.270(19) 0.214(15) -0.068(9) -0.070(9) C11 0.046(4) 0.043(3) 0.039(3) -0.012(3) -0.003(3) -0.008(3) C12 0.043(4) 0.056(4) 0.040(3) -0.012(3) -0.006(3) -0.005(3) C13 0.035(4) 0.073(5) 0.051(4) -0.010(4) -0.007(3) -0.011(3) C14 0.091(6) 0.078(6) 0.049(4) -0.017(4) -0.004(4) -0.051(5) C15 0.061(5) 0.063(5) 0.050(4) -0.012(3) -0.015(4) -0.025(4) OW1 0.052(3) 0.053(3) 0.056(3) -0.010(2) -0.023(2) -0.012(2) OW2 0.060(3) 0.091(4) 0.039(3) -0.017(3) -0.006(2) -0.012(3) OW3 0.122(9) 0.184(11) 0.199(12) 0.011(9) -0.026(8) -0.004(8) OW4 0.339(19) 0.296(16) 0.338(18) -0.275(15) -0.282(17) 0.246(16) OW5 0.083(5) 0.144(8) 0.139(7) 0.022(6) -0.037(5) 0.000(5) OW6 0.092(5) 0.079(4) 0.072(4) -0.004(3) 0.001(4) -0.019(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd N3 2.264(5) . yes Cd N5 2.280(5) . yes Cd N1 2.280(5) . yes Cd O1 2.323(4) . yes Cd OW2 2.403(5) . yes Cd OW1 2.407(5) . yes S O4 1.452(5) . ? S O2 1.465(5) . ? S O1 1.469(5) . ? S O3 1.480(5) . ? N1 C1 1.310(8) . ? N1 C2 1.373(8) . ? N2 C1 1.353(8) . ? N2 C3 1.365(9) . ? N2 C4 1.465(8) . ? N3 C6 1.334(8) . ? N3 C7 1.394(8) . ? N4 C6 1.331(9) . ? N4 C8 1.347(10) . ? N4 C9 1.471(8) . ? N5 C11 1.329(8) . ? N5 C12 1.383(9) . ? N6 C11 1.336(9) . ? N6 C13 1.373(9) . ? N6 C14 1.464(9) . ? C2 C3 1.361(9) . ? C4 C5 1.475(11) . ? C5 C5 1.12(2) 2_445 ? C7 C8 1.354(10) . ? C9 C10 1.453(12) . ? C10 C10 1.09(2) 2_436 ? C12 C13 1.346(10) . ? C14 C15 1.484(10) . ? C15 C15 1.511(13) 2_646 ? 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 N3 Cd N5 98.4(2) . . yes N3 Cd N1 98.9(2) . . yes N5 Cd N1 100.2(2) . . yes N3 Cd O1 89.8(2) . . yes N5 Cd O1 90.4(2) . . yes N1 Cd O1 165.2(2) . . yes N3 Cd OW2 169.9(2) . . yes N5 Cd OW2 90.2(2) . . yes N1 Cd OW2 84.8(2) . . yes O1 Cd OW2 84.8(2) . . yes N3 Cd OW1 85.8(2) . . yes N5 Cd OW1 172.1(2) . . yes N1 Cd OW1 85.7(2) . . yes O1 Cd OW1 82.9(2) . . yes OW2 Cd OW1 85.1(2) . . yes O4 S O2 110.7(4) . . ? O4 S O1 109.0(3) . . ? O2 S O1 109.7(3) . . ? O4 S O3 110.0(3) . . ? O2 S O3 108.0(3) . . ? O1 S O3 109.4(3) . . ? S O1 Cd 135.7(3) . . ? C1 N1 C2 106.2(5) . . ? C1 N1 Cd 122.3(4) . . ? C2 N1 Cd 131.5(4) . . ? C1 N2 C3 107.2(5) . . ? C1 N2 C4 125.1(6) . . ? C3 N2 C4 127.8(6) . . ? C6 N3 C7 105.0(6) . . ? C6 N3 Cd 122.9(4) . . ? C7 N3 Cd 132.0(5) . . ? C6 N4 C8 107.0(6) . . ? C6 N4 C9 125.2(7) . . ? C8 N4 C9 127.7(7) . . ? C11 N5 C12 104.7(5) . . ? C11 N5 Cd 127.5(4) . . ? C12 N5 Cd 127.8(4) . . ? C11 N6 C13 107.6(6) . . ? C11 N6 C14 125.9(7) . . ? C13 N6 C14 126.5(7) . . ? N1 C1 N2 111.1(6) . . ? C3 C2 N1 109.2(6) . . ? C2 C3 N2 106.3(6) . . ? N2 C4 C5 111.5(6) . . ? C5 C5 C4 141.3(15) 2_445 . ? N4 C6 N3 111.8(6) . . ? C8 C7 N3 107.7(7) . . ? N4 C8 C7 108.5(6) . . ? C10 C9 N4 110.3(6) . . ? C10 C10 C9 145.2(15) 2_436 . ? N5 C11 N6 111.5(6) . . ? C13 C12 N5 110.2(6) . . ? C12 C13 N6 106.0(6) . . ? N6 C14 C15 113.8(6) . . ? C14 C15 C15 113.3(8) . 2_646 ? 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 O4 S O1 Cd -168.8(4) . . . . ? O2 S O1 Cd 69.9(5) . . . . ? O3 S O1 Cd -48.4(5) . . . . ? N3 Cd O1 S 118.1(5) . . . . ? N5 Cd O1 S -143.5(5) . . . . ? N1 Cd O1 S -7.8(11) . . . . ? OW2 Cd O1 S -53.4(5) . . . . ? OW1 Cd O1 S 32.3(4) . . . . ? N3 Cd N1 C1 -129.7(5) . . . . ? N5 Cd N1 C1 130.0(5) . . . . ? O1 Cd N1 C1 -4.7(10) . . . . ? OW2 Cd N1 C1 40.8(5) . . . . ? OW1 Cd N1 C1 -44.7(5) . . . . ? N3 Cd N1 C2 51.1(6) . . . . ? N5 Cd N1 C2 -49.2(6) . . . . ? O1 Cd N1 C2 176.1(6) . . . . ? OW2 Cd N1 C2 -138.4(6) . . . . ? OW1 Cd N1 C2 136.1(6) . . . . ? N5 Cd N3 C6 -133.2(5) . . . . ? N1 Cd N3 C6 125.1(5) . . . . ? O1 Cd N3 C6 -42.8(5) . . . . ? OW2 Cd N3 C6 14.5(14) . . . . ? OW1 Cd N3 C6 40.1(5) . . . . ? N5 Cd N3 C7 48.1(6) . . . . ? N1 Cd N3 C7 -53.7(6) . . . . ? O1 Cd N3 C7 138.4(6) . . . . ? OW2 Cd N3 C7 -164.2(9) . . . . ? OW1 Cd N3 C7 -138.7(6) . . . . ? N3 Cd N5 C11 -56.8(5) . . . . ? N1 Cd N5 C11 43.9(5) . . . . ? O1 Cd N5 C11 -146.6(5) . . . . ? OW2 Cd N5 C11 128.6(5) . . . . ? OW1 Cd N5 C11 -178.4(10) . . . . ? N3 Cd N5 C12 123.5(5) . . . . ? N1 Cd N5 C12 -135.9(5) . . . . ? O1 Cd N5 C12 33.6(5) . . . . ? OW2 Cd N5 C12 -51.2(5) . . . . ? OW1 Cd N5 C12 1.9(15) . . . . ? C2 N1 C1 N2 -0.5(7) . . . . ? Cd N1 C1 N2 -179.9(4) . . . . ? C3 N2 C1 N1 0.8(8) . . . . ? C4 N2 C1 N1 -179.3(6) . . . . ? C1 N1 C2 C3 0.1(8) . . . . ? Cd N1 C2 C3 179.4(5) . . . . ? N1 C2 C3 N2 0.4(8) . . . . ? C1 N2 C3 C2 -0.7(8) . . . . ? C4 N2 C3 C2 179.4(6) . . . . ? C1 N2 C4 C5 95.3(12) . . . . ? C3 N2 C4 C5 -84.8(13) . . . . ? N2 C4 C5 C5 20.4(50) . . . 2_445 ? C8 N4 C6 N3 0.6(8) . . . . ? C9 N4 C6 N3 177.1(6) . . . . ? C7 N3 C6 N4 -1.1(7) . . . . ? Cd N3 C6 N4 179.9(4) . . . . ? C6 N3 C7 C8 1.1(8) . . . . ? Cd N3 C7 C8 -180.0(5) . . . . ? C6 N4 C8 C7 0.2(8) . . . . ? C9 N4 C8 C7 -176.2(6) . . . . ? N3 C7 C8 N4 -0.8(8) . . . . ? C6 N4 C9 C10 -84.0(13) . . . . ? C8 N4 C9 C10 91.7(13) . . . . ? N4 C9 C10 C10 -8.5(59) . . . 2_436 ? C12 N5 C11 N6 0.5(7) . . . . ? Cd N5 C11 N6 -179.2(4) . . . . ? C13 N6 C11 N5 -1.1(8) . . . . ? C14 N6 C11 N5 178.4(6) . . . . ? C11 N5 C12 C13 0.2(7) . . . . ? Cd N5 C12 C13 180.0(4) . . . . ? N5 C12 C13 N6 -0.9(8) . . . . ? C11 N6 C13 C12 1.2(8) . . . . ? C14 N6 C13 C12 -178.3(6) . . . . ? C11 N6 C14 C15 76.0(11) . . . . ? C13 N6 C14 C15 -104.5(9) . . . . ? N6 C14 C15 C15 -178.1(9) . . . 2_646 ? _refine_diff_density_max 1.424 _refine_diff_density_min -1.746 _refine_diff_density_rms 0.456 #===END