Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Renzo Cini' 'Gabriella Tamasi' _publ_contact_author_name 'Prof Renzo Cini ' _publ_contact_author_address ; Dept of Chemical and Biosystem Sciences and Technologies University of Siena Via Aldo Moro 2 Siena I-53100 ITALY ; _publ_contact_author_email CINI@UNISI.IT _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Synthesis, X-ray Structures, Semi-empirical Quantum Mechanics and Density Functional Modelling of Binary and Ternary Zn(II), Cd(II), Mg(II) and Ca(II) Complexes Containing Sulphato and Terpyridine Ligands. Molecular Models for Selected Not-Catalytic Metal Sites in Sulfurylase ; data_12se02ab _database_code_CSD 205815 _chemical_name_systematic ; (\m-o,o-sulfate)(2,2':6'2"-terpyridine)cadmium(II) dimer di-hydrate ; _chemical_formula_sum 'C30 H26 Cd2 N6 O10 S2' _chemical_formula_iupac '[Cd (C15 H11 N3) (S O4)]2 2H2 O' _chemical_formula_weight 919.52 _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 9.079(1) _cell_length_b 10.402(1) _cell_length_c 10.533(1) _cell_angle_alpha 119.23(1) _cell_angle_beta 105.12(1) _cell_angle_gamma 99.54(1) _cell_volume 785.66(14) _cell_formula_units_Z 1 _cell_measurement_reflns_used 29 _cell_measurement_theta_min 5.0 _cell_measurement_theta_max 22.0 _cell_measurement_temperature 293(2) _exptl_crystal_description prism _exptl_crystal_colour 'pale yallow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.943 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 456 _exptl_absorpt_coefficient_mu 1.556 _exptl_absorpt_correction_type '\y scan' _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min 0.583 _exptl_absorpt_correction_T_max 0.560 _diffrn_ambient_temperature 293(2) _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens P4' _diffrn_measurement_method \w _diffrn_reflns_number 3082 _diffrn_reflns_av_R_equivalents 0.0084 _diffrn_reflns_av_sigmaI/netI 0.0158 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_decay_% 0 _reflns_number_total 2545 _reflns_number_gt 2354 _reflns_observed_criterion I>2\s(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_gt 0.0182 _refine_ls_R_factor_all 0.0214 _refine_ls_wR_factor_gt 0.0448 _refine_ls_wR_factor_all 0.0462 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.077 _refine_ls_number_reflns 2545 _refine_ls_number_parameters 234 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment mixed _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0260P)^2^+0.2221P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_extinction_method none _refine_ls_extinction_coef ? 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' _computing_data_collection 'XSCANS (Siemens, 1994)' _computing_cell_refinement 'XSCANS (Siemens, 1994)' _computing_data_reduction 'XSCANS (Siemens, 1994)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-32/ORTEP-III (Farugia, 1998)' _computing_publication_material 'CIFTAB (Shldrick, 1997)' 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.62157(2) 0.727817(19) 0.597196(19) 0.03196(7) Uani 1 d . . . S1 S 0.46920(7) 0.44481(7) 0.25663(7) 0.03570(15) Uani 1 d . . . N1 N 0.4362(2) 0.8568(2) 0.5707(2) 0.0352(5) Uani 1 d . . . N2 N 0.7542(2) 0.9977(2) 0.7598(2) 0.0321(4) Uani 1 d . . . N3 N 0.9065(2) 0.7901(2) 0.7027(2) 0.0373(5) Uani 1 d . . . O1 O 0.4776(2) 0.2922(2) 0.2210(2) 0.0502(5) Uani 1 d . . . O2 O 0.6340(2) 0.5672(2) 0.3532(2) 0.0447(4) Uani 1 d . . . O3 O 0.3774(2) 0.4890(2) 0.3616(3) 0.0568(5) Uani 1 d . . . O4 O 0.3935(3) 0.4407(3) 0.1162(3) 0.0750(7) Uani 1 d . . . C2 C 0.4901(3) 1.0146(3) 0.6736(3) 0.0356(6) Uani 1 d . . . C3 C 0.3867(4) 1.0987(3) 0.6751(3) 0.0490(7) Uani 1 d . . . H3 H 0.4250 1.2071 0.7473 0.059 Uiso 1 calc R . . C4 C 0.2271(4) 1.0210(4) 0.5694(4) 0.0531(7) Uani 1 d . . . H4 H 0.1568 1.0766 0.5688 0.064 Uiso 1 calc R . . C5 C 0.1719(3) 0.8608(4) 0.4645(3) 0.0491(7) Uani 1 d . . . H5 H 0.0641 0.8060 0.3923 0.059 Uiso 1 calc R . . C6 C 0.2804(3) 0.7836(3) 0.4690(3) 0.0415(6) Uani 1 d . . . H6 H 0.2434 0.6752 0.3977 0.050 Uiso 1 calc R . . C2' C 0.6657(3) 1.0914(3) 0.7800(3) 0.0352(6) Uani 1 d . . . C3' C 0.7382(4) 1.2533(3) 0.8929(3) 0.0469(7) Uani 1 d . . . H3' H 0.6764 1.3183 0.9082 0.056 Uiso 1 calc R . . C4' C 0.9030(4) 1.3144(3) 0.9808(3) 0.0498(7) Uani 1 d . . . H4' H 0.9532 1.4216 1.0579 0.060 Uiso 1 calc R . . C5' C 0.9940(3) 1.2180(3) 0.9554(3) 0.0436(7) Uani 1 d . . . H5' H 1.1062 1.2593 1.0121 0.052 Uiso 1 calc R . . C6' C 0.9152(3) 1.0575(3) 0.8434(3) 0.0329(5) Uani 1 d . . . C2" C 1.0013(3) 0.9418(3) 0.8068(3) 0.0335(5) Uani 1 d . . . C3" C 1.1697(3) 0.9866(3) 0.8752(3) 0.0443(7) Uani 1 d . . . H3" H 1.2340 1.0921 0.9473 0.053 Uiso 1 calc R . . C4" C 1.2401(3) 0.8723(4) 0.8347(3) 0.0496(7) Uani 1 d . . . H4" H 1.3525 0.9003 0.8795 0.060 Uiso 1 calc R . . C5" C 1.1433(3) 0.7169(4) 0.7278(3) 0.0501(7) Uani 1 d . . . H5" H 1.1885 0.6381 0.6989 0.060 Uiso 1 calc R . . C6" C 0.9768(3) 0.6810(3) 0.6644(3) 0.0474(7) Uani 1 d . . . H6" H 0.9107 0.5760 0.5917 0.057 Uiso 1 calc R . . O1W O 0.1979(3) 0.3713(3) 0.8156(3) 0.0559(6) Uani 1 d . . . H1W H 0.253(5) 0.402(5) 0.782(5) 0.082(14) Uiso 1 d . . . H2W H 0.258(5) 0.379(5) 0.888(5) 0.079(14) Uiso 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 Cd1 0.02525(10) 0.02622(11) 0.03351(10) 0.01416(8) 0.00499(7) 0.00370(7) S1 0.0293(3) 0.0340(3) 0.0341(3) 0.0186(3) 0.0051(2) 0.0028(3) N1 0.0291(10) 0.0360(11) 0.0371(11) 0.0211(9) 0.0083(9) 0.0097(9) N2 0.0273(10) 0.0301(10) 0.0316(10) 0.0169(9) 0.0061(8) 0.0036(9) N3 0.0292(11) 0.0356(11) 0.0362(11) 0.0170(9) 0.0061(9) 0.0082(9) O1 0.0527(12) 0.0346(10) 0.0547(11) 0.0207(9) 0.0203(10) 0.0120(9) O2 0.0355(10) 0.0417(10) 0.0353(9) 0.0161(8) 0.0067(8) -0.0043(8) O3 0.0460(11) 0.0539(12) 0.0745(14) 0.0341(11) 0.0327(11) 0.0182(10) O4 0.0616(14) 0.0860(17) 0.0573(13) 0.0510(13) -0.0086(11) -0.0044(12) C2 0.0368(13) 0.0352(13) 0.0354(13) 0.0207(11) 0.0140(11) 0.0113(11) C3 0.0499(17) 0.0408(15) 0.0545(17) 0.0237(13) 0.0205(14) 0.0216(14) C4 0.0451(16) 0.0590(19) 0.0592(18) 0.0328(16) 0.0189(14) 0.0307(15) C5 0.0347(14) 0.0641(19) 0.0492(16) 0.0338(15) 0.0121(12) 0.0190(14) C6 0.0317(13) 0.0418(15) 0.0420(14) 0.0214(12) 0.0085(11) 0.0088(12) C2' 0.0376(14) 0.0323(13) 0.0339(12) 0.0192(11) 0.0121(11) 0.0090(11) C3' 0.0540(17) 0.0322(14) 0.0459(15) 0.0193(12) 0.0142(13) 0.0127(13) C4' 0.0543(18) 0.0301(14) 0.0423(15) 0.0135(12) 0.0097(13) 0.0014(13) C5' 0.0379(14) 0.0376(15) 0.0361(13) 0.0180(12) 0.0048(11) -0.0052(12) C6' 0.0301(12) 0.0332(13) 0.0302(12) 0.0183(10) 0.0087(10) 0.0026(10) C2" 0.0258(12) 0.0405(14) 0.0277(11) 0.0189(11) 0.0067(10) 0.0035(11) C3" 0.0312(13) 0.0497(16) 0.0362(13) 0.0201(12) 0.0073(11) 0.0021(12) C4" 0.0259(13) 0.071(2) 0.0433(15) 0.0306(15) 0.0083(12) 0.0109(14) C5" 0.0408(15) 0.0615(19) 0.0518(16) 0.0311(15) 0.0197(13) 0.0261(15) C6" 0.0394(15) 0.0434(16) 0.0455(15) 0.0192(13) 0.0104(12) 0.0125(13) O1W 0.0436(12) 0.0661(15) 0.0484(13) 0.0294(12) 0.0162(11) 0.0098(11) _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 Cd1 N2 2.318(2) . y Cd1 O2 2.3300(18) . y Cd1 N1 2.362(2) . y Cd1 N3 2.364(2) . y Cd1 O1 2.397(2) 2_666 y Cd1 O3 2.496(2) 2_666 y Cd1 O3 2.555(2) . y S1 O4 1.435(2) . y S1 O1 1.463(2) . y S1 O2 1.4843(18) . y S1 O3 1.497(2) . y N1 C6 1.336(3) . y N1 C2 1.353(3) . y N2 C2' 1.337(3) . y N2 C6' 1.338(3) . y N3 C6" 1.337(3) . y N3 C2" 1.342(3) . y C2 C3 1.383(4) . ? C2 C2' 1.486(3) . y C3 C4 1.372(4) . ? C4 C5 1.373(4) . ? C5 C6 1.376(4) . ? C2' C3' 1.397(4) . ? C3' C4' 1.373(4) . ? C4' C5' 1.375(4) . ? C5' C6' 1.390(3) . ? C6' C2" 1.491(4) . y C2" C3" 1.391(3) . ? C3" C4" 1.378(4) . ? C4" C5" 1.375(4) . ? C5" C6" 1.383(4) . ? 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 N2 Cd1 O2 123.73(7) . . y N2 Cd1 N1 69.96(7) . . y O2 Cd1 N1 109.84(7) . . y N2 Cd1 N3 69.32(7) . . y O2 Cd1 N3 85.03(7) . . y N1 Cd1 N3 138.05(7) . . y N2 Cd1 O1 95.97(7) . 2_666 y O2 Cd1 O1 140.00(6) . 2_666 y N1 Cd1 O1 86.60(7) . 2_666 y N3 Cd1 O1 107.17(7) . 2_666 y N2 Cd1 O3 133.44(7) . 2_666 y O2 Cd1 O3 87.88(7) . 2_666 y N1 Cd1 O3 135.32(7) . 2_666 y N3 Cd1 O3 82.19(7) . 2_666 y O1 Cd1 O3 57.62(6) 2_666 2_666 y N2 Cd1 O3 149.80(7) . . y O2 Cd1 O3 57.99(6) . . y N1 Cd1 O3 81.17(7) . . y N3 Cd1 O3 136.05(7) . . y O1 Cd1 O3 90.85(7) 2_666 . y O3 Cd1 O3 74.24(8) 2_666 . y O4 S1 O1 112.46(14) . . y O4 S1 O2 110.07(12) . . y O1 S1 O2 110.59(12) . . y O4 S1 O3 112.01(15) . . y O1 S1 O3 105.73(12) . . y O2 S1 O3 105.70(11) . . y C6 N1 C2 118.3(2) . . y C6 N1 Cd1 124.49(17) . . y C2 N1 Cd1 117.01(16) . . y C2' N2 C6' 120.8(2) . . y C2' N2 Cd1 118.89(15) . . y C6' N2 Cd1 120.05(16) . . y C6" N3 C2" 118.8(2) . . y C6" N3 Cd1 122.90(17) . . y C2" N3 Cd1 118.35(16) . . y S1 O1 Cd1 100.36(10) . 2_666 y S1 O2 Cd1 103.07(10) . . y S1 O3 Cd1 95.17(10) . 2_666 y S1 O3 Cd1 93.21(9) . . y Cd1 O3 Cd1 105.76(8) 2_666 . y N1 C2 C3 121.1(2) . . y N1 C2 C2' 116.4(2) . . y C3 C2 C2' 122.5(2) . . ? C4 C3 C2 119.5(3) . . ? C3 C4 C5 119.6(3) . . ? C4 C5 C6 118.2(3) . . ? N1 C6 C5 123.2(3) . . ? N2 C2' C3' 120.7(2) . . ? N2 C2' C2 116.5(2) . . y C3' C2' C2 122.7(2) . . ? C4' C3' C2' 118.5(3) . . ? C5' C4' C3' 120.4(2) . . ? C4' C5' C6' 118.7(2) . . ? N2 C6' C5' 120.9(2) . . ? N2 C6' C2" 115.8(2) . . y C5' C6' C2" 123.3(2) . . ? N3 C2" C3" 121.3(2) . . ? N3 C2" C6' 116.0(2) . . y C3" C2" C6' 122.7(2) . . ? C4" C3" C2" 119.1(3) . . ? C5" C4" C3" 119.7(2) . . ? C4" C5" C6" 118.1(3) . . ? N3 C6" C5" 123.0(3) . . ? _diffrn_measured_fraction_theta_max 0.917 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.917 _refine_diff_density_max 0.221 _refine_diff_density_min -0.361 _refine_diff_density_rms 0.054 #===END data_znterpab _database_code_CSD 205816 _audit_creation_method SHELXL-97 _chemical_name_systematic ; (\m-o,o'-sulphato)(2,2':6'2"-terpyridine) zinc(II) dimer di-hydrate ; _chemical_formula_sum 'C30 H26 N6 O10 S2 Zn2' _chemical_formula_iupac '[Zn (C15 H11 N3) (S O4)]2 2H2 O' _chemical_formula_weight 412.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7050(1) _cell_length_b 9.767(2) _cell_length_c 10.3220(1) _cell_angle_alpha 110.14(3) _cell_angle_beta 116.620(1) _cell_angle_gamma 98.910(1) _cell_volume 763.47(19) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 29 _cell_measurement_theta_min 5.0 _cell_measurement_theta_max 22.0 _exptl_crystal_description prism _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.795 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 420 _exptl_absorpt_coefficient_mu 1.780 _exptl_absorpt_correction_type '\y scan' _exptl_absorpt_correction_T_min 0.555 _exptl_absorpt_correction_T_max 0.497 _exptl_absorpt_process_details ? _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 'Siemens P4' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 3091 _diffrn_reflns_av_R_equivalents 0.0188 _diffrn_reflns_av_sigmaI/netI 0.0276 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2587 _reflns_number_gt 2284 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XSCANS (Siemens, 1994)' _computing_cell_refinement 'XSCANS (Siemens, 1994)' _computing_data_reduction 'XSCANS (Siemens, 1994)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-32/ORTEP-III (Farugia, 1998)' _computing_publication_material 'CIFTAB (Shldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0418P)^2^+0.2961P] 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 SHELXL _refine_ls_extinction_coef 0.0095(13) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2587 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0369 _refine_ls_R_factor_gt 0.0302 _refine_ls_wR_factor_ref 0.0765 _refine_ls_wR_factor_gt 0.0732 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _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 0.76319(4) 0.35590(4) 0.40924(4) 0.02811(13) Uani 1 1 d . . . S1 S 0.92070(8) 0.47396(8) 0.23533(8) 0.02837(18) Uani 1 1 d . . . O3 O 0.8883(3) 0.3729(2) 0.3069(3) 0.0372(5) Uani 1 1 d . . . O1W O 0.8386(4) 0.2021(3) -0.2238(4) 0.0546(7) Uani 1 1 d . . . O1 O 0.7880(3) 0.5287(3) 0.1764(4) 0.0624(7) Uani 1 1 d . . . O4 O 0.9428(3) 0.3828(3) 0.1077(3) 0.0555(7) Uani 1 1 d . . . N1' N 0.5068(3) 0.2527(3) 0.2495(3) 0.0285(5) Uani 1 1 d . . . O2 O 1.0789(3) 0.6098(3) 0.3680(3) 0.0531(7) Uani 1 1 d . . . N1 N 0.7046(3) 0.1007(3) 0.3125(3) 0.0314(5) Uani 1 1 d . . . C5 C 0.4921(4) -0.1524(3) 0.1157(4) 0.0380(7) Uani 1 1 d . . . H5 H 0.3805 -0.2130 0.0372 0.046 Uiso 1 1 calc R . . N1" N 0.6835(3) 0.5531(3) 0.4476(3) 0.0326(5) Uani 1 1 d . . . C2' C 0.4317(3) 0.0965(3) 0.1604(3) 0.0288(6) Uani 1 1 d . . . C3' C 0.2621(4) 0.0268(4) 0.0444(4) 0.0394(7) Uani 1 1 d . . . H3' H 0.2098 -0.0817 -0.0169 0.047 Uiso 1 1 calc R . . C3 C 0.7710(4) -0.1303(4) 0.2701(4) 0.0421(8) Uani 1 1 d . . . H3A H 0.8510 -0.1750 0.2966 0.051 Uiso 1 1 calc R . . C6' C 0.4206(4) 0.3463(3) 0.2311(4) 0.0324(6) Uani 1 1 d . . . C2" C 0.5204(4) 0.5161(3) 0.3451(4) 0.0328(6) Uani 1 1 d . . . C5' C 0.2511(4) 0.2840(4) 0.1151(4) 0.0437(8) Uani 1 1 d . . . H5' H 0.1916 0.3492 0.1002 0.052 Uiso 1 1 calc R . . C4 C 0.6071(4) -0.2229(4) 0.1531(4) 0.0420(8) Uani 1 1 d . . . H4 H 0.5741 -0.3315 0.0999 0.050 Uiso 1 1 calc R . . C6 C 0.5448(3) 0.0094(3) 0.1963(3) 0.0296(6) Uani 1 1 d . . . C4' C 0.1737(4) 0.1237(4) 0.0228(4) 0.0445(8) Uani 1 1 d . . . H4' H 0.0603 0.0799 -0.0550 0.053 Uiso 1 1 calc R . . C2 C 0.8146(4) 0.0296(4) 0.3472(4) 0.0402(7) Uani 1 1 d . . . H2 H 0.9256 0.0916 0.4273 0.048 Uiso 1 1 calc R . . C3" C 0.4496(5) 0.6290(4) 0.3486(4) 0.0453(8) Uani 1 1 d . . . H3" H 0.3366 0.6010 0.2769 0.054 Uiso 1 1 calc R . . C5" C 0.7160(5) 0.8226(4) 0.5657(4) 0.0457(8) Uani 1 1 d . . . H5" H 0.7850 0.9264 0.6423 0.055 Uiso 1 1 calc R . . C4" C 0.5501(5) 0.7841(4) 0.4605(4) 0.0494(9) Uani 1 1 d . . . H4" H 0.5054 0.8620 0.4645 0.059 Uiso 1 1 calc R . . C6" C 0.7786(4) 0.7046(3) 0.5557(4) 0.0415(8) Uani 1 1 d . . . H6" H 0.8913 0.7310 0.6268 0.050 Uiso 1 1 calc R . . H2W H 0.862(6) 0.271(6) -0.134(6) 0.084(17) Uiso 1 1 d . . . H1W H 0.875(5) 0.260(5) -0.254(5) 0.059(13) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.02295(19) 0.0233(2) 0.02789(19) 0.00699(14) 0.01124(14) 0.00418(13) S1 0.0247(4) 0.0222(4) 0.0273(3) 0.0068(3) 0.0109(3) 0.0046(3) O3 0.0368(11) 0.0332(11) 0.0508(13) 0.0213(10) 0.0291(11) 0.0129(9) O1W 0.0698(18) 0.0349(14) 0.0518(16) 0.0183(13) 0.0308(15) 0.0137(13) O1 0.0486(15) 0.0506(15) 0.089(2) 0.0397(15) 0.0295(15) 0.0280(13) O4 0.0666(17) 0.0529(15) 0.0429(13) 0.0116(11) 0.0369(13) 0.0146(13) N1' 0.0248(12) 0.0277(12) 0.0307(12) 0.0114(10) 0.0154(10) 0.0083(10) O2 0.0435(14) 0.0437(13) 0.0303(11) 0.0145(10) 0.0010(10) -0.0151(11) N1 0.0251(12) 0.0258(12) 0.0276(12) 0.0081(10) 0.0082(10) 0.0028(10) C5 0.0380(17) 0.0257(15) 0.0341(16) 0.0073(13) 0.0156(14) 0.0021(13) N1" 0.0338(13) 0.0253(12) 0.0356(13) 0.0080(10) 0.0214(11) 0.0098(10) C2' 0.0249(14) 0.0280(15) 0.0256(14) 0.0095(12) 0.0121(12) 0.0032(12) C3' 0.0287(16) 0.0372(17) 0.0347(16) 0.0109(14) 0.0120(14) 0.0007(13) C3 0.0485(19) 0.0374(18) 0.0465(19) 0.0225(15) 0.0255(17) 0.0239(16) C6' 0.0289(15) 0.0359(16) 0.0333(15) 0.0144(13) 0.0189(13) 0.0121(13) C2" 0.0358(16) 0.0332(16) 0.0392(16) 0.0178(13) 0.0259(14) 0.0162(13) C5' 0.0315(17) 0.050(2) 0.0514(19) 0.0244(17) 0.0217(15) 0.0192(15) C4 0.057(2) 0.0239(15) 0.0418(18) 0.0132(13) 0.0261(17) 0.0136(15) C6 0.0288(15) 0.0266(15) 0.0254(14) 0.0093(11) 0.0129(12) 0.0038(12) C4' 0.0224(15) 0.053(2) 0.0444(18) 0.0210(16) 0.0111(14) 0.0096(15) C2 0.0322(16) 0.0389(18) 0.0403(17) 0.0180(14) 0.0133(14) 0.0130(14) C3" 0.051(2) 0.0441(19) 0.054(2) 0.0258(17) 0.0327(18) 0.0276(17) C5" 0.067(2) 0.0286(17) 0.048(2) 0.0144(15) 0.0385(19) 0.0178(16) C4" 0.072(3) 0.041(2) 0.058(2) 0.0283(17) 0.045(2) 0.0343(19) C6" 0.0446(19) 0.0262(16) 0.0446(18) 0.0079(14) 0.0250(16) 0.0094(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 Zn1 O3 1.956(2) . ? Zn1 O2 1.975(2) 2_766 ? Zn1 N1' 2.080(2) . ? Zn1 N1" 2.163(2) . ? Zn1 N1 2.207(2) . ? S1 O1 1.432(2) . ? S1 O4 1.441(2) . ? S1 O2 1.492(2) . ? S1 O3 1.495(2) . ? N1' C6' 1.337(4) . ? N1' C2' 1.339(4) . ? O2 Zn1 1.975(2) 2_766 ? N1 C6 1.344(4) . ? N1 C2 1.346(4) . ? C5 C4 1.379(5) . ? C5 C6 1.384(4) . ? N1" C6" 1.343(4) . ? N1" C2" 1.347(4) . ? C2' C3' 1.390(4) . ? C2' C6 1.486(4) . ? C3' C4' 1.381(5) . ? C3 C4 1.374(5) . ? C3 C2 1.374(4) . ? C6' C5' 1.390(4) . ? C6' C2" 1.486(4) . ? C2" C3" 1.386(4) . ? C5' C4' 1.375(5) . ? C3" C4" 1.381(5) . ? C5" C4" 1.370(5) . ? C5" C6" 1.378(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Zn1 O2 107.32(10) . 2_766 ? O3 Zn1 N1' 115.42(9) . . ? O2 Zn1 N1' 134.70(10) 2_766 . ? O3 Zn1 N1" 107.66(9) . . ? O2 Zn1 N1" 104.83(11) 2_766 . ? N1' Zn1 N1" 76.45(9) . . ? O3 Zn1 N1 91.87(9) . . ? O2 Zn1 N1 90.30(10) 2_766 . ? N1' Zn1 N1 74.47(9) . . ? N1" Zn1 N1 149.88(9) . . ? O1 S1 O4 112.56(17) . . ? O1 S1 O2 109.97(15) . . ? O4 S1 O2 108.77(15) . . ? O1 S1 O3 110.37(14) . . ? O4 S1 O3 107.55(14) . . ? O2 S1 O3 107.46(13) . . ? S1 O3 Zn1 135.48(13) . . ? C6' N1' C2' 121.0(2) . . ? C6' N1' Zn1 118.33(18) . . ? C2' N1' Zn1 120.57(19) . . ? S1 O2 Zn1 128.16(14) . 2_766 ? C6 N1 C2 117.7(2) . . ? C6 N1 Zn1 115.80(19) . . ? C2 N1 Zn1 126.23(19) . . ? C4 C5 C6 119.2(3) . . ? C6" N1" C2" 118.3(3) . . ? C6" N1" Zn1 127.3(2) . . ? C2" N1" Zn1 114.38(19) . . ? N1' C2' C3' 121.1(3) . . ? N1' C2' C6 114.3(2) . . ? C3' C2' C6 124.6(3) . . ? C4' C3' C2' 117.9(3) . . ? C4 C3 C2 118.8(3) . . ? N1' C6' C5' 120.7(3) . . ? N1' C6' C2" 114.4(2) . . ? C5' C6' C2" 124.9(3) . . ? N1" C2" C3" 122.0(3) . . ? N1" C2" C6' 115.9(3) . . ? C3" C2" C6' 122.1(3) . . ? C4' C5' C6' 118.4(3) . . ? C3 C4 C5 119.0(3) . . ? N1 C6 C5 122.1(3) . . ? N1 C6 C2' 114.6(2) . . ? C5 C6 C2' 123.3(3) . . ? C5' C4' C3' 120.8(3) . . ? N1 C2 C3 123.2(3) . . ? C4" C3" C2" 118.7(3) . . ? C4" C5" C6" 118.7(3) . . ? C5" C4" C3" 119.7(3) . . ? N1" C6" C5" 122.7(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 S1 O3 Zn1 -26.7(2) . . . . ? O4 S1 O3 Zn1 -149.79(19) . . . . ? O2 S1 O3 Zn1 93.3(2) . . . . ? O2 Zn1 O3 S1 -121.19(19) 2_766 . . . ? N1' Zn1 O3 S1 74.2(2) . . . . ? N1" Zn1 O3 S1 -8.8(2) . . . . ? N1 Zn1 O3 S1 147.91(19) . . . . ? O3 Zn1 N1' C6' -96.4(2) . . . . ? O2 Zn1 N1' C6' 104.5(2) 2_766 . . . ? N1" Zn1 N1' C6' 6.9(2) . . . . ? N1 Zn1 N1' C6' 179.0(2) . . . . ? O3 Zn1 N1' C2' 79.7(2) . . . . ? O2 Zn1 N1' C2' -79.3(2) 2_766 . . . ? N1" Zn1 N1' C2' -176.9(2) . . . . ? N1 Zn1 N1' C2' -4.9(2) . . . . ? O1 S1 O2 Zn1 127.3(2) . . . 2_766 ? O4 S1 O2 Zn1 -109.0(2) . . . 2_766 ? O3 S1 O2 Zn1 7.1(2) . . . 2_766 ? O3 Zn1 N1 C6 -111.2(2) . . . . ? O2 Zn1 N1 C6 141.5(2) 2_766 . . . ? N1' Zn1 N1 C6 4.68(19) . . . . ? N1" Zn1 N1 C6 20.2(3) . . . . ? O3 Zn1 N1 C2 62.1(3) . . . . ? O2 Zn1 N1 C2 -45.3(3) 2_766 . . . ? N1' Zn1 N1 C2 178.0(3) . . . . ? N1" Zn1 N1 C2 -166.5(2) . . . . ? O3 Zn1 N1" C6" -70.3(3) . . . . ? O2 Zn1 N1" C6" 43.8(3) 2_766 . . . ? N1' Zn1 N1" C6" 177.0(3) . . . . ? N1 Zn1 N1" C6" 161.6(2) . . . . ? O3 Zn1 N1" C2" 107.1(2) . . . . ? O2 Zn1 N1" C2" -138.9(2) 2_766 . . . ? N1' Zn1 N1" C2" -5.7(2) . . . . ? N1 Zn1 N1" C2" -21.0(3) . . . . ? C6' N1' C2' C3' 0.9(4) . . . . ? Zn1 N1' C2' C3' -175.1(2) . . . . ? C6' N1' C2' C6 -179.6(2) . . . . ? Zn1 N1' C2' C6 4.3(3) . . . . ? N1' C2' C3' C4' 0.5(4) . . . . ? C6 C2' C3' C4' -178.8(3) . . . . ? C2' N1' C6' C5' -2.1(4) . . . . ? Zn1 N1' C6' C5' 174.0(2) . . . . ? C2' N1' C6' C2" 176.9(2) . . . . ? Zn1 N1' C6' C2" -7.0(3) . . . . ? C6" N1" C2" C3" 0.0(4) . . . . ? Zn1 N1" C2" C3" -177.5(2) . . . . ? C6" N1" C2" C6' -178.5(3) . . . . ? Zn1 N1" C2" C6' 4.0(3) . . . . ? N1' C6' C2" N1" 1.7(4) . . . . ? C5' C6' C2" N1" -179.3(3) . . . . ? N1' C6' C2" C3" -176.8(3) . . . . ? C5' C6' C2" C3" 2.2(5) . . . . ? N1' C6' C5' C4' 1.7(5) . . . . ? C2" C6' C5' C4' -177.1(3) . . . . ? C2 C3 C4 C5 0.7(5) . . . . ? C6 C5 C4 C3 0.3(5) . . . . ? C2 N1 C6 C5 1.1(4) . . . . ? Zn1 N1 C6 C5 175.0(2) . . . . ? C2 N1 C6 C2' -177.9(3) . . . . ? Zn1 N1 C6 C2' -4.0(3) . . . . ? C4 C5 C6 N1 -1.2(5) . . . . ? C4 C5 C6 C2' 177.7(3) . . . . ? N1' C2' C6 N1 0.1(4) . . . . ? C3' C2' C6 N1 179.5(3) . . . . ? N1' C2' C6 C5 -178.9(3) . . . . ? C3' C2' C6 C5 0.5(5) . . . . ? C6' C5' C4' C3' -0.3(5) . . . . ? C2' C3' C4' C5' -0.8(5) . . . . ? C6 N1 C2 C3 -0.1(5) . . . . ? Zn1 N1 C2 C3 -173.3(2) . . . . ? C4 C3 C2 N1 -0.8(5) . . . . ? N1" C2" C3" C4" 0.2(5) . . . . ? C6' C2" C3" C4" 178.6(3) . . . . ? C6" C5" C4" C3" 0.5(5) . . . . ? C2" C3" C4" C5" -0.5(5) . . . . ? C2" N1" C6" C5" 0.0(5) . . . . ? Zn1 N1" C6" C5" 177.3(2) . . . . ? C4" C5" C6" N1" -0.3(5) . . . . ? _diffrn_measured_fraction_theta_max 0.955 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.955 _refine_diff_density_max 0.464 _refine_diff_density_min -0.383 _refine_diff_density_rms 0.064