# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Prof. Dongrong Xiao' _publ_contact_author_email xiaodr98@yahoo.com.cn _publ_section_title ; Unusual self-threading and interdigitated architectures self-assembled from long flexible ligands and d10 metal salts ; loop_ _publ_author_name 'Haiyan Chen' 'Dongrong Xiao' 'Linlin Fan' 'Jianghong He' 'Shiwei Yan' ; Guangju Zhang ; 'Dianzhen Sun' 'Zhongli Ye' 'Ruo Yuan' 'Enbo Wang' # Attachment '- compounds 1-3.CIF' data_compound-1 _database_code_depnum_ccdc_archive 'CCDC 825670' #TrackingRef '- compounds 1-3.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H56 Cd2 N10 O19 S2' _chemical_formula_weight 1558.11 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 14.362(2) _cell_length_b 14.580(2) _cell_length_c 15.887(2) _cell_angle_alpha 86.106(2) _cell_angle_beta 80.269(2) _cell_angle_gamma 87.555(2) _cell_volume 3269.7(8) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 29034 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 27.00 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.43 _exptl_crystal_size_min 0.38 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.583 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1580 _exptl_absorpt_coefficient_mu 0.796 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7061 _exptl_absorpt_correction_T_max 0.7519 _exptl_absorpt_process_details 'SADABS(Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29034 _diffrn_reflns_av_R_equivalents 0.0354 _diffrn_reflns_av_sigmaI/netI 0.0531 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 27.00 _reflns_number_total 14110 _reflns_number_gt 10574 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material 'SHELXL-97 (Sheldrick, 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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14110 _refine_ls_number_parameters 937 _refine_ls_number_restraints 101 _refine_ls_R_factor_all 0.0695 _refine_ls_R_factor_gt 0.0497 _refine_ls_wR_factor_ref 0.1562 _refine_ls_wR_factor_gt 0.1387 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.073 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.598260(19) 0.304147(18) -0.915146(19) 0.03615(10) Uani 1 1 d U . . Cd2 Cd 0.737825(19) 1.03148(2) -1.38282(2) 0.03882(11) Uani 1 1 d . . . S1 S 0.79323(10) 0.44322(8) -1.46126(8) 0.0545(3) Uani 1 1 d . . . S2 S -0.01708(9) 0.33841(12) -0.85784(10) 0.0704(4) Uani 1 1 d DU . . C1 C 0.6450(3) 0.3458(3) -1.2383(3) 0.0516(11) Uani 1 1 d . . . H1A H 0.5837 0.3276 -1.2178 0.062 Uiso 1 1 calc R . . C2 C 0.6715(3) 0.3721(3) -1.3251(3) 0.0512(11) Uani 1 1 d . . . H2A H 0.6282 0.3710 -1.3624 0.061 Uiso 1 1 calc R . . C3 C 0.7620(3) 0.3995(3) -1.3544(3) 0.0441(10) Uani 1 1 d . . . C4 C 0.8283(3) 0.3998(3) -1.3003(3) 0.0469(10) Uani 1 1 d . . . H4A H 0.8896 0.4182 -1.3209 0.056 Uiso 1 1 calc R . . C5 C 0.8009(3) 0.3717(3) -1.2146(3) 0.0479(11) Uani 1 1 d . . . H5A H 0.8451 0.3698 -1.1779 0.058 Uiso 1 1 calc R . . C6 C 0.7092(3) 0.3466(3) -1.1829(3) 0.0416(9) Uani 1 1 d . . . C7 C 0.6796(4) 0.3211(3) -1.0884(3) 0.0488(11) Uani 1 1 d . . . C8 C 0.7813(3) 0.5636(3) -1.4500(3) 0.0482(11) Uani 1 1 d . . . C9 C 0.6909(4) 0.6038(3) -1.4428(3) 0.0569(12) Uani 1 1 d . . . H9A H 0.6392 0.5690 -1.4466 0.068 Uiso 1 1 calc R . . C10 C 0.6798(3) 0.6963(3) -1.4299(3) 0.0548(12) Uani 1 1 d . . . H10A H 0.6203 0.7248 -1.4271 0.066 Uiso 1 1 calc R . . C11 C 0.7558(3) 0.7470(3) -1.4213(3) 0.0438(10) Uani 1 1 d . . . C12 C 0.8450(3) 0.7056(3) -1.4294(3) 0.0525(11) Uani 1 1 d . . . H12A H 0.8967 0.7403 -1.4252 0.063 Uiso 1 1 calc R . . C13 C 0.8584(4) 0.6128(3) -1.4439(3) 0.0533(11) Uani 1 1 d . . . H13A H 0.9184 0.5849 -1.4493 0.064 Uiso 1 1 calc R . . C14 C 0.7424(3) 0.8487(3) -1.4065(3) 0.0483(11) Uani 1 1 d . . . C15 C 0.4043(3) 0.2991(4) -0.8770(3) 0.0547(12) Uani 1 1 d . . . C16 C 0.2976(3) 0.3031(3) -0.8634(3) 0.0471(10) Uani 1 1 d . . . C17 C 0.2510(3) 0.3837(4) -0.8394(4) 0.0706(16) Uani 1 1 d . C . H17A H 0.2851 0.4327 -0.8274 0.085 Uiso 1 1 calc R . . C18 C 0.1537(4) 0.3927(4) -0.8329(4) 0.0721(16) Uani 1 1 d . . . H18A H 0.1221 0.4469 -0.8152 0.087 Uiso 1 1 calc R C . C19 C 0.1051(3) 0.3219(3) -0.8525(3) 0.0505(11) Uani 1 1 d . C . C20 C 0.1493(4) 0.2402(4) -0.8765(4) 0.0630(13) Uani 1 1 d . . . H20A H 0.1148 0.1925 -0.8904 0.076 Uiso 1 1 calc R C . C21 C 0.2471(3) 0.2301(3) -0.8798(4) 0.0610(13) Uani 1 1 d . C . H21A H 0.2779 0.1742 -0.8930 0.073 Uiso 1 1 calc R . . C22 C -0.0795(3) 0.2694(3) -0.7731(3) 0.0469(10) Uani 1 1 d . C . C23 C -0.1371(4) 0.2045(4) -0.7913(4) 0.0658(14) Uani 1 1 d . . . H23A H -0.1409 0.1943 -0.8478 0.079 Uiso 1 1 calc R C . C24 C -0.1895(4) 0.1543(4) -0.7248(4) 0.0691(16) Uani 1 1 d . C . H24A H -0.2293 0.1101 -0.7370 0.083 Uiso 1 1 calc R . . C25 C -0.1848(3) 0.1677(3) -0.6416(3) 0.0499(11) Uani 1 1 d . . . C26 C -0.1280(4) 0.2352(4) -0.6244(4) 0.0703(16) Uani 1 1 d . C . H26A H -0.1257 0.2467 -0.5679 0.084 Uiso 1 1 calc R . . C27 C -0.0743(4) 0.2863(4) -0.6905(4) 0.0722(16) Uani 1 1 d . . . H27A H -0.0352 0.3314 -0.6788 0.087 Uiso 1 1 calc R C . C28 C -0.2401(3) 0.1100(4) -0.5687(4) 0.0739(18) Uani 1 1 d DU . . C29 C 0.5937(3) 0.5284(3) -0.9080(3) 0.0477(11) Uani 1 1 d . . . H29A H 0.5292 0.5194 -0.9033 0.057 Uiso 1 1 calc R . . C30 C 0.6235(3) 0.6165(3) -0.9033(3) 0.0440(10) Uani 1 1 d . . . H30A H 0.5796 0.6652 -0.8952 0.053 Uiso 1 1 calc R . . C31 C 0.7185(3) 0.6319(3) -0.9105(2) 0.0337(8) Uani 1 1 d . . . C32 C 0.7805(3) 0.5574(3) -0.9259(3) 0.0454(10) Uani 1 1 d . . . H32A H 0.8455 0.5651 -0.9337 0.054 Uiso 1 1 calc R . . C33 C 0.7450(3) 0.4718(3) -0.9294(3) 0.0463(10) Uani 1 1 d . . . H33A H 0.7878 0.4225 -0.9397 0.056 Uiso 1 1 calc R . . C34 C 0.7524(3) 0.7238(2) -0.9012(2) 0.0332(8) Uani 1 1 d . . . C35 C 0.7604(3) 0.8705(3) -0.8943(3) 0.0359(8) Uani 1 1 d . . . C36 C 0.8495(3) 0.8330(3) -0.8866(3) 0.0362(8) Uani 1 1 d . . . C37 C 0.9349(3) 0.8731(3) -0.8686(3) 0.0393(9) Uani 1 1 d . . . C38 C 0.9347(4) 0.9579(3) -0.8346(4) 0.0597(13) Uani 1 1 d . . . H38A H 0.8787 0.9928 -0.8237 0.072 Uiso 1 1 calc R . . C39 C 1.0171(4) 0.9909(4) -0.8168(4) 0.0674(15) Uani 1 1 d . . . H39A H 1.0146 1.0492 -0.7961 0.081 Uiso 1 1 calc R . . C40 C 1.0989(4) 0.8635(4) -0.8557(4) 0.0632(14) Uani 1 1 d . . . H40A H 1.1549 0.8282 -0.8605 0.076 Uiso 1 1 calc R . . C41 C 1.0215(3) 0.8260(3) -0.8793(4) 0.0568(12) Uani 1 1 d . . . H41A H 1.0274 0.7688 -0.9025 0.068 Uiso 1 1 calc R . . C42 C 0.7266(3) 0.9674(2) -0.8985(3) 0.0342(8) Uani 1 1 d . . . C43 C 0.6436(3) 0.9971(3) -0.8509(3) 0.0547(12) Uani 1 1 d . . . H43A H 0.6073 0.9556 -0.8133 0.066 Uiso 1 1 calc R . . C44 C 0.6132(3) 1.0877(3) -0.8583(3) 0.0527(12) Uani 1 1 d . . . H44A H 0.5557 1.1047 -0.8258 0.063 Uiso 1 1 calc R . . C45 C 0.7423(3) 1.1246(3) -0.9537(3) 0.0545(12) Uani 1 1 d . . . H45A H 0.7773 1.1686 -0.9892 0.065 Uiso 1 1 calc R . . C46 C 0.7785(3) 1.0346(3) -0.9509(3) 0.0540(12) Uani 1 1 d . . . H46A H 0.8364 1.0194 -0.9836 0.065 Uiso 1 1 calc R . . C47 C -0.1021(3) 1.1763(3) -1.3729(4) 0.0628(15) Uani 1 1 d . . . H47A H -0.1553 1.2155 -1.3684 0.075 Uiso 1 1 calc R . . C48 C -0.0168(3) 1.2125(3) -1.3664(4) 0.0617(14) Uani 1 1 d . . . H48A H -0.0138 1.2743 -1.3565 0.074 Uiso 1 1 calc R . . C49 C 0.0637(3) 1.1577(3) -1.3743(3) 0.0383(9) Uani 1 1 d . . . C50 C 0.0531(3) 1.0672(3) -1.3907(4) 0.0588(14) Uani 1 1 d . . . H50A H 0.1056 1.0273 -1.3992 0.071 Uiso 1 1 calc R . . C51 C -0.0349(3) 1.0362(3) -1.3944(4) 0.0590(13) Uani 1 1 d . . . H51A H -0.0402 0.9745 -1.4038 0.071 Uiso 1 1 calc R . . C52 C 0.1543(3) 1.1943(3) -1.3650(3) 0.0364(8) Uani 1 1 d . . . C53 C 0.2606(3) 1.2851(3) -1.3424(2) 0.0358(8) Uani 1 1 d . . . C54 C 0.3052(3) 1.2009(3) -1.3579(3) 0.0352(8) Uani 1 1 d . . . C55 C 0.4031(3) 1.1648(3) -1.3598(2) 0.0344(8) Uani 1 1 d . . . C56 C 0.4559(3) 1.1827(3) -1.2972(3) 0.0419(9) Uani 1 1 d . . . H56A H 0.4306 1.2200 -1.2532 0.050 Uiso 1 1 calc R . . C57 C 0.5458(3) 1.1447(3) -1.3008(3) 0.0411(9) Uani 1 1 d . . . H57A H 0.5800 1.1567 -1.2582 0.049 Uiso 1 1 calc R . . C58 C 0.5357(3) 1.0766(4) -1.4235(3) 0.0624(15) Uani 1 1 d . . . H58A H 0.5630 1.0406 -1.4679 0.075 Uiso 1 1 calc R . . C59 C 0.4455(3) 1.1117(4) -1.4232(3) 0.0533(12) Uani 1 1 d . . . H59A H 0.4131 1.0991 -1.4669 0.064 Uiso 1 1 calc R . . C60 C 0.2987(3) 1.3742(3) -1.3308(3) 0.0394(9) Uani 1 1 d . . . C61 C 0.2413(4) 1.4436(4) -1.2968(4) 0.0630(14) Uani 1 1 d . . . H61A H 0.1770 1.4341 -1.2796 0.076 Uiso 1 1 calc R . . C62 C 0.2775(5) 1.5283(4) -1.2877(4) 0.0720(16) Uani 1 1 d . . . H62A H 0.2355 1.5743 -1.2655 0.086 Uiso 1 1 calc R . . C63 C 0.4231(4) 1.4806(4) -1.3434(5) 0.0787(18) Uani 1 1 d . . . H63A H 0.4870 1.4924 -1.3595 0.094 Uiso 1 1 calc R . . C64 C 0.3935(4) 1.3951(3) -1.3577(4) 0.0642(14) Uani 1 1 d . . . H64A H 0.4360 1.3522 -1.3848 0.077 Uiso 1 1 calc R . . N1 N 0.6530(2) 0.4554(2) -0.9191(2) 0.0390(8) Uani 1 1 d . . . N2 N 0.7012(2) 0.8017(2) -0.9030(2) 0.0354(7) Uani 1 1 d . . . N3 N 0.8423(2) 0.7402(2) -0.8912(2) 0.0352(7) Uani 1 1 d D . . H3A H 0.893(2) 0.704(3) -0.888(3) 0.061(15) Uiso 1 1 d D . . N4 N 0.6600(2) 1.1512(2) -0.9080(2) 0.0387(7) Uani 1 1 d . . . N5 N 1.0990(3) 0.9459(3) -0.8269(3) 0.0553(10) Uani 1 1 d . . . N6 N -0.1125(2) 1.0891(2) -1.3854(2) 0.0434(8) Uani 1 1 d . . . N7 N 0.1661(2) 1.2794(2) -1.3471(2) 0.0390(8) Uani 1 1 d . . . N8 N 0.2364(2) 1.1442(2) -1.3726(2) 0.0358(7) Uani 1 1 d D . . H8A H 0.239(3) 1.0843(10) -1.383(3) 0.037(11) Uiso 1 1 d D . . N9 N 0.3661(4) 1.5478(3) -1.3080(3) 0.0719(13) Uani 1 1 d . . . N10 N 0.5859(2) 1.0918(2) -1.3625(2) 0.0420(8) Uani 1 1 d . . . O1 O 0.5929(3) 0.3113(3) -1.0605(2) 0.0626(9) Uani 1 1 d . . . OW1 O 0.6141(3) 0.2939(2) -0.7730(2) 0.0626(10) Uani 1 1 d . . . HW1B H 0.6051 0.3456 -0.7499 0.075 Uiso 1 1 d R . . HW1A H 0.6411 0.2603 -0.7520 0.075 Uiso 1 1 d R . . OW2 O 0.7335(2) 1.0334(3) -1.2388(2) 0.0711(11) Uani 1 1 d . . . HW2A H 0.7732 1.0499 -1.2113 0.085 Uiso 1 1 d R . . HW2B H 0.6955 1.0084 -1.1995 0.085 Uiso 1 1 d R . . O2 O 0.7425(3) 0.3145(2) -1.0429(2) 0.0575(8) Uani 1 1 d . . . OW3 O 0.5368(3) 0.1597(3) -0.6484(3) 0.0883(13) Uani 1 1 d . . . HW3A H 0.4769 0.1545 -0.6488 0.106 Uiso 1 1 d R . . HW3B H 0.5514 0.1626 -0.7101 0.106 Uiso 1 1 d R . . O3 O 0.6620(2) 0.8852(2) -1.3973(2) 0.0571(8) Uani 1 1 d . . . O4 O 0.8148(2) 0.8927(2) -1.4061(3) 0.0683(10) Uani 1 1 d . . . OW4 O 0.5999(3) 0.9786(4) -1.1094(3) 0.1088(16) Uani 1 1 d U . . HW4B H 0.5771 0.9468 -1.0635 0.131 Uiso 1 1 d R . . HW4A H 0.5972 1.0333 -1.0991 0.131 Uiso 1 1 d R . . OW5 O 0.5066(4) 0.8573(4) -0.9273(4) 0.1193(18) Uani 1 1 d U . . HW5A H 0.4718 0.8110 -0.9157 0.143 Uiso 1 1 d R . . HW5B H 0.5280 0.8420 -0.8825 0.143 Uiso 1 1 d R . . O5 O 0.7227(3) 0.4161(2) -1.5080(2) 0.0720(11) Uani 1 1 d . . . OW6 O 0.5755(4) 0.2878(4) -1.5212(4) 0.130(2) Uani 1 1 d U . . HW6A H 0.5775 0.2503 -1.5645 0.156 Uiso 1 1 d R . . HW6B H 0.5870 0.3431 -1.5502 0.156 Uiso 1 1 d R . . O6 O 0.8912(3) 0.4202(3) -1.4899(3) 0.0753(11) Uani 1 1 d . . . OW7 O 0.0012(4) 0.6096(4) -0.8944(5) 0.0582(17) Uani 0.50 1 d PU A 1 OW9 O -0.0307(8) 0.6187(9) -0.8104(9) 0.055(3) Uani 0.25 1 d PU B 2 O7 O 0.4465(2) 0.2226(3) -0.8919(3) 0.0675(10) Uani 1 1 d U . . OW8 O 0.0450(8) 1.4473(9) -1.3520(8) 0.046(3) Uani 0.25 1 d PU . . HW8A H 0.0522 1.4704 -1.4019 0.055 Uiso 0.25 1 d PR . . HW8B H 0.0570 1.4844 -1.3175 0.055 Uiso 0.25 1 d PR . . O8 O 0.4471(2) 0.3700(3) -0.8775(3) 0.0743(11) Uani 1 1 d . . . O9 O -0.2526(7) 0.0316(5) -0.5523(7) 0.059(3) Uani 0.40 1 d PD . 1 O9A O -0.2826(5) 0.0427(4) -0.6004(5) 0.075(2) Uani 0.60 1 d PDU . 2 O10 O -0.2578(10) 0.1563(9) -0.4993(7) 0.077(4) Uani 0.40 1 d PDU . 1 O10A O -0.2401(9) 0.1243(8) -0.4954(6) 0.096(4) Uani 0.60 1 d PDU . 2 O11 O -0.0399(9) 0.4328(6) -0.8253(7) 0.071(3) Uani 0.50 1 d PDU C 1 O11A O -0.0450(11) 0.4332(6) -0.8578(8) 0.075(4) Uani 0.50 1 d PDU C 2 O12 O -0.0370(12) 0.3236(9) -0.9400(7) 0.085(4) Uani 0.50 1 d PDU C 1 O12A O -0.0302(13) 0.2872(9) -0.9322(7) 0.085(4) Uani 0.50 1 d PDU C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.03433(17) 0.02301(15) 0.05158(19) -0.00481(12) -0.00764(13) -0.00048(11) Cd2 0.02580(16) 0.03379(17) 0.0581(2) -0.00515(13) -0.00939(13) -0.00164(11) S1 0.0792(9) 0.0336(6) 0.0490(6) -0.0059(5) -0.0043(6) -0.0032(6) S2 0.0356(6) 0.0877(11) 0.0817(10) 0.0293(8) -0.0067(6) 0.0031(6) C1 0.048(3) 0.046(3) 0.060(3) 0.003(2) -0.007(2) -0.006(2) C2 0.057(3) 0.049(3) 0.052(3) -0.003(2) -0.020(2) -0.005(2) C3 0.057(3) 0.0227(19) 0.052(3) -0.0061(17) -0.008(2) 0.0020(18) C4 0.046(2) 0.032(2) 0.063(3) -0.007(2) -0.008(2) 0.0025(18) C5 0.053(3) 0.035(2) 0.060(3) -0.010(2) -0.020(2) 0.0060(19) C6 0.047(2) 0.0250(19) 0.054(2) -0.0019(17) -0.0113(19) -0.0015(17) C7 0.069(3) 0.029(2) 0.050(3) -0.0058(18) -0.013(2) 0.003(2) C8 0.064(3) 0.032(2) 0.047(2) 0.0014(18) -0.007(2) -0.002(2) C9 0.057(3) 0.034(2) 0.084(4) -0.005(2) -0.021(3) -0.010(2) C10 0.047(3) 0.038(2) 0.082(3) -0.003(2) -0.015(2) -0.002(2) C11 0.049(2) 0.029(2) 0.055(3) -0.0013(18) -0.014(2) -0.0059(18) C12 0.047(3) 0.039(2) 0.073(3) 0.001(2) -0.015(2) -0.009(2) C13 0.051(3) 0.038(2) 0.070(3) 0.000(2) -0.012(2) 0.003(2) C14 0.058(3) 0.035(2) 0.055(3) -0.0030(19) -0.015(2) -0.004(2) C15 0.037(2) 0.059(3) 0.064(3) 0.009(2) -0.001(2) 0.001(2) C16 0.030(2) 0.052(3) 0.057(3) -0.001(2) -0.0018(18) -0.0002(19) C17 0.037(3) 0.052(3) 0.123(5) -0.020(3) -0.009(3) 0.001(2) C18 0.039(3) 0.057(3) 0.119(5) -0.023(3) -0.007(3) 0.012(2) C19 0.030(2) 0.056(3) 0.061(3) 0.010(2) -0.0021(19) 0.0059(19) C20 0.047(3) 0.054(3) 0.087(4) -0.002(3) -0.007(3) -0.008(2) C21 0.044(3) 0.042(3) 0.092(4) -0.005(3) 0.001(2) 0.005(2) C22 0.033(2) 0.043(2) 0.064(3) 0.001(2) -0.0059(19) 0.0016(18) C23 0.059(3) 0.073(4) 0.068(3) -0.023(3) -0.010(3) -0.014(3) C24 0.054(3) 0.054(3) 0.102(5) -0.028(3) -0.007(3) -0.021(3) C25 0.031(2) 0.032(2) 0.084(3) 0.003(2) -0.003(2) -0.0015(17) C26 0.067(3) 0.083(4) 0.062(3) 0.002(3) -0.010(3) -0.031(3) C27 0.067(4) 0.079(4) 0.076(4) -0.002(3) -0.020(3) -0.041(3) C28 0.028(2) 0.059(3) 0.122(5) 0.023(3) 0.009(3) 0.008(2) C29 0.033(2) 0.034(2) 0.076(3) -0.008(2) -0.008(2) -0.0020(17) C30 0.034(2) 0.025(2) 0.073(3) -0.0040(19) -0.0078(19) 0.0045(16) C31 0.035(2) 0.0248(18) 0.042(2) -0.0004(15) -0.0093(16) -0.0007(15) C32 0.031(2) 0.030(2) 0.077(3) -0.011(2) -0.013(2) -0.0001(16) C33 0.038(2) 0.028(2) 0.075(3) -0.009(2) -0.015(2) 0.0047(17) C34 0.034(2) 0.0227(18) 0.043(2) -0.0032(15) -0.0085(16) 0.0021(15) C35 0.039(2) 0.0230(18) 0.046(2) -0.0042(16) -0.0087(17) 0.0005(15) C36 0.033(2) 0.0251(19) 0.052(2) -0.0050(16) -0.0112(17) 0.0007(15) C37 0.042(2) 0.031(2) 0.046(2) -0.0027(17) -0.0104(18) -0.0037(17) C38 0.050(3) 0.039(3) 0.098(4) -0.018(3) -0.028(3) -0.001(2) C39 0.064(3) 0.044(3) 0.102(4) -0.011(3) -0.031(3) -0.013(2) C40 0.042(3) 0.060(3) 0.090(4) -0.008(3) -0.019(3) 0.003(2) C41 0.044(3) 0.040(3) 0.090(4) -0.016(2) -0.018(2) 0.001(2) C42 0.033(2) 0.0227(18) 0.049(2) -0.0048(16) -0.0115(16) 0.0004(15) C43 0.056(3) 0.025(2) 0.075(3) 0.003(2) 0.008(2) -0.0010(19) C44 0.046(3) 0.032(2) 0.073(3) 0.000(2) 0.008(2) 0.0065(19) C45 0.054(3) 0.034(2) 0.069(3) 0.008(2) 0.003(2) 0.002(2) C46 0.046(3) 0.036(2) 0.073(3) 0.002(2) 0.003(2) 0.010(2) C47 0.028(2) 0.040(3) 0.124(5) -0.025(3) -0.015(2) 0.0044(19) C48 0.033(2) 0.035(2) 0.120(5) -0.021(3) -0.019(3) 0.0030(19) C49 0.030(2) 0.036(2) 0.049(2) -0.0026(17) -0.0045(17) -0.0045(16) C50 0.030(2) 0.038(3) 0.110(4) -0.021(3) -0.012(2) 0.0033(18) C51 0.038(2) 0.035(2) 0.106(4) -0.017(3) -0.012(2) -0.0029(19) C52 0.0263(19) 0.034(2) 0.049(2) -0.0024(17) -0.0063(16) -0.0016(15) C53 0.0275(19) 0.036(2) 0.043(2) -0.0026(17) -0.0040(16) -0.0028(15) C54 0.0271(19) 0.034(2) 0.045(2) -0.0017(17) -0.0075(16) -0.0024(15) C55 0.0279(19) 0.031(2) 0.044(2) -0.0021(16) -0.0054(16) -0.0012(15) C56 0.034(2) 0.044(2) 0.049(2) -0.0091(19) -0.0101(18) 0.0026(18) C57 0.034(2) 0.043(2) 0.049(2) -0.0058(19) -0.0143(18) -0.0014(17) C58 0.044(3) 0.074(4) 0.077(3) -0.041(3) -0.022(2) 0.024(2) C59 0.043(2) 0.061(3) 0.063(3) -0.025(2) -0.023(2) 0.009(2) C60 0.039(2) 0.035(2) 0.047(2) -0.0057(17) -0.0148(18) 0.0020(17) C61 0.060(3) 0.048(3) 0.079(4) -0.020(3) -0.003(3) 0.002(2) C62 0.085(4) 0.048(3) 0.087(4) -0.026(3) -0.022(3) 0.008(3) C63 0.053(3) 0.049(3) 0.141(6) -0.015(3) -0.030(3) -0.008(3) C64 0.050(3) 0.036(3) 0.110(4) -0.010(3) -0.022(3) 0.000(2) N1 0.0364(18) 0.0253(17) 0.056(2) -0.0065(15) -0.0081(15) -0.0021(13) N2 0.0339(17) 0.0214(15) 0.0526(19) -0.0040(14) -0.0123(14) 0.0012(13) N3 0.0317(17) 0.0233(16) 0.052(2) -0.0049(14) -0.0114(14) 0.0015(13) N4 0.0385(18) 0.0276(17) 0.050(2) -0.0036(14) -0.0079(15) 0.0044(14) N5 0.042(2) 0.059(3) 0.069(3) -0.002(2) -0.0168(19) -0.0144(19) N6 0.0272(17) 0.0349(19) 0.069(2) -0.0053(17) -0.0086(16) -0.0031(14) N7 0.0299(17) 0.0345(18) 0.053(2) -0.0076(15) -0.0053(14) 0.0013(14) N8 0.0258(16) 0.0288(17) 0.053(2) -0.0061(15) -0.0055(14) -0.0008(13) N9 0.088(4) 0.042(2) 0.095(4) -0.013(2) -0.041(3) -0.007(2) N10 0.0300(17) 0.041(2) 0.057(2) -0.0099(16) -0.0127(15) 0.0057(14) O1 0.063(2) 0.063(2) 0.060(2) 0.0024(17) -0.0065(17) -0.0089(18) OW1 0.103(3) 0.0310(17) 0.058(2) -0.0076(14) -0.0263(19) -0.0008(17) OW2 0.0417(19) 0.118(4) 0.056(2) 0.005(2) -0.0155(16) -0.022(2) O2 0.078(2) 0.0393(18) 0.0568(19) -0.0015(15) -0.0204(17) 0.0074(16) OW3 0.083(3) 0.092(3) 0.084(3) 0.015(2) 0.000(2) -0.020(3) O3 0.051(2) 0.0364(17) 0.085(2) -0.0059(16) -0.0172(17) 0.0032(15) O4 0.055(2) 0.0374(18) 0.117(3) -0.0139(19) -0.020(2) -0.0100(16) OW4 0.087(3) 0.109(3) 0.116(3) 0.010(3) 0.018(2) -0.010(3) OW5 0.112(3) 0.107(3) 0.158(4) -0.049(3) -0.063(3) 0.004(3) O5 0.114(3) 0.052(2) 0.056(2) -0.0058(17) -0.026(2) -0.018(2) OW6 0.130(4) 0.122(4) 0.138(4) -0.003(3) -0.019(3) -0.043(3) O6 0.087(3) 0.048(2) 0.079(3) -0.0106(18) 0.020(2) 0.0065(19) OW7 0.042(3) 0.037(3) 0.098(5) 0.001(3) -0.023(3) 0.006(3) OW9 0.025(5) 0.059(7) 0.080(7) 0.034(6) -0.022(5) -0.011(5) O7 0.0292(14) 0.063(2) 0.107(3) -0.001(2) -0.0024(17) -0.0009(12) OW8 0.033(5) 0.057(6) 0.049(6) -0.017(5) -0.004(4) -0.005(5) O8 0.0391(19) 0.060(2) 0.122(3) -0.003(2) -0.0068(19) -0.0081(17) O9 0.044(5) 0.036(5) 0.087(7) 0.024(5) 0.006(5) 0.008(4) O9A 0.070(5) 0.033(3) 0.108(6) 0.008(4) 0.020(4) -0.009(3) O10 0.050(6) 0.096(8) 0.086(7) 0.062(6) -0.031(5) -0.020(6) O10A 0.083(5) 0.115(6) 0.093(5) 0.048(4) -0.038(4) -0.023(4) O11 0.047(5) 0.057(5) 0.098(7) 0.043(5) -0.002(6) 0.014(3) O11A 0.062(5) 0.071(5) 0.085(6) 0.036(4) -0.015(4) 0.014(3) O12 0.053(5) 0.128(8) 0.071(6) 0.047(6) -0.022(4) 0.008(6) O12A 0.075(7) 0.124(9) 0.058(5) 0.026(6) -0.028(4) -0.011(7) _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 OW1 2.302(3) . ? Cd1 O1 2.319(4) . ? Cd1 O8 2.336(4) . ? Cd1 N4 2.366(3) 1_545 ? Cd1 N1 2.366(3) . ? Cd1 O7 2.488(3) . ? Cd1 O2 2.645(4) . ? Cd1 C15 2.751(5) . ? Cd2 O10A 2.156(10) 1_664 ? Cd2 OW2 2.280(3) . ? Cd2 O4 2.286(4) . ? Cd2 N10 2.297(3) . ? Cd2 N6 2.334(3) 1_655 ? Cd2 O3 2.477(3) . ? Cd2 O10 2.501(13) 1_664 ? Cd2 C14 2.714(4) . ? S1 O5 1.437(4) . ? S1 O6 1.437(4) . ? S1 C3 1.763(5) . ? S1 C8 1.775(5) . ? S2 O12 1.415(9) . ? S2 O11A 1.422(8) . ? S2 O12A 1.482(8) . ? S2 O11 1.507(8) . ? S2 C22 1.765(5) . ? S2 C19 1.776(4) . ? C1 C6 1.378(6) . ? C1 C2 1.398(6) . ? C1 H1A 0.9300 . ? C2 C3 1.373(6) . ? C2 H2A 0.9300 . ? C3 C4 1.386(6) . ? C4 C5 1.391(6) . ? C4 H4A 0.9300 . ? C5 C6 1.384(6) . ? C5 H5A 0.9300 . ? C6 C7 1.515(6) . ? C7 O2 1.246(6) . ? C7 O1 1.260(6) . ? C8 C13 1.365(7) . ? C8 C9 1.391(7) . ? C9 C10 1.377(6) . ? C9 H9A 0.9300 . ? C10 C11 1.375(6) . ? C10 H10A 0.9300 . ? C11 C12 1.383(6) . ? C11 C14 1.515(6) . ? C12 C13 1.387(7) . ? C12 H12A 0.9300 . ? C13 H13A 0.9300 . ? C14 O3 1.241(6) . ? C14 O4 1.246(5) . ? C15 O8 1.223(6) . ? C15 O7 1.264(6) . ? C15 C16 1.511(6) . ? C16 C17 1.371(7) . ? C16 C21 1.378(7) . ? C17 C18 1.385(7) . ? C17 H17A 0.9300 . ? C18 C19 1.353(7) . ? C18 H18A 0.9300 . ? C19 C20 1.372(7) . ? C20 C21 1.398(7) . ? C20 H20A 0.9300 . ? C21 H21A 0.9300 . ? C22 C23 1.359(7) . ? C22 C27 1.366(7) . ? C23 C24 1.376(8) . ? C23 H23A 0.9300 . ? C24 C25 1.363(8) . ? C24 H24A 0.9300 . ? C25 C26 1.374(7) . ? C25 C28 1.514(7) . ? C26 C27 1.387(7) . ? C26 H26A 0.9300 . ? C27 H27A 0.9300 . ? C28 O9 1.170(8) . ? C28 O10A 1.198(9) . ? C28 O10 1.314(9) . ? C28 O9A 1.346(7) . ? C29 N1 1.337(5) . ? C29 C30 1.383(6) . ? C29 H29A 0.9300 . ? C30 C31 1.376(5) . ? C30 H30A 0.9300 . ? C31 C32 1.383(5) . ? C31 C34 1.471(5) . ? C32 C33 1.376(6) . ? C32 H32A 0.9300 . ? C33 N1 1.334(5) . ? C33 H33A 0.9300 . ? C34 N2 1.327(5) . ? C34 N3 1.360(5) . ? C35 N2 1.371(5) . ? C35 C36 1.390(5) . ? C35 C42 1.475(5) . ? C36 N3 1.370(5) . ? C36 C37 1.460(5) . ? C37 C41 1.385(6) . ? C37 C38 1.383(6) . ? C38 C39 1.375(7) . ? C38 H38A 0.9300 . ? C39 N5 1.313(7) . ? C39 H39A 0.9300 . ? C40 N5 1.314(7) . ? C40 C41 1.378(7) . ? C40 H40A 0.9300 . ? C41 H41A 0.9300 . ? C42 C43 1.370(6) . ? C42 C46 1.397(6) . ? C43 C44 1.377(6) . ? C43 H43A 0.9300 . ? C44 N4 1.307(5) . ? C44 H44A 0.9300 . ? C45 N4 1.336(6) . ? C45 C46 1.391(6) . ? C45 H45A 0.9300 . ? C46 H46A 0.9300 . ? C47 N6 1.319(6) . ? C47 C48 1.377(6) . ? C47 H47A 0.9300 . ? C48 C49 1.369(6) . ? C48 H48A 0.9300 . ? C49 C50 1.383(6) . ? C49 C52 1.461(5) . ? C50 C51 1.371(6) . ? C50 H50A 0.9300 . ? C51 N6 1.321(5) . ? C51 H51A 0.9300 . ? C52 N7 1.316(5) . ? C52 N8 1.352(5) . ? C53 N7 1.379(5) . ? C53 C54 1.379(5) . ? C53 C60 1.465(6) . ? C54 N8 1.374(5) . ? C54 C55 1.475(5) . ? C55 C59 1.358(6) . ? C55 C56 1.392(5) . ? C56 C57 1.378(5) . ? C56 H56A 0.9300 . ? C57 N10 1.327(5) . ? C57 H57A 0.9300 . ? C58 N10 1.337(6) . ? C58 C59 1.372(6) . ? C58 H58A 0.9300 . ? C59 H59A 0.9300 . ? C60 C61 1.359(6) . ? C60 C64 1.397(6) . ? C61 C62 1.387(7) . ? C61 H61A 0.9300 . ? C62 N9 1.297(7) . ? C62 H62A 0.9300 . ? C63 N9 1.341(7) . ? C63 C64 1.378(7) . ? C63 H63A 0.9300 . ? C64 H64A 0.9300 . ? N3 H3A 0.888(11) . ? N4 Cd1 2.366(3) 1_565 ? N6 Cd2 2.334(3) 1_455 ? N8 H8A 0.897(11) . ? OW1 HW1B 0.8558 . ? OW1 HW1A 0.7128 . ? OW2 HW2A 0.8272 . ? OW2 HW2B 0.8320 . ? OW3 HW3A 0.8679 . ? OW3 HW3B 0.9654 . ? OW4 HW4B 0.8597 . ? OW4 HW4A 0.8235 . ? OW5 HW5A 0.8481 . ? OW5 HW5B 0.8351 . ? OW6 HW6A 0.9032 . ? OW6 HW6B 0.9080 . ? OW8 HW8A 0.8307 . ? OW8 HW8B 0.8379 . ? O10 Cd2 2.501(13) 1_446 ? O10A Cd2 2.156(10) 1_446 ? 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 OW1 Cd1 O1 176.14(13) . . ? OW1 Cd1 O8 89.24(15) . . ? O1 Cd1 O8 94.60(15) . . ? OW1 Cd1 N4 81.94(12) . 1_545 ? O1 Cd1 N4 95.73(13) . 1_545 ? O8 Cd1 N4 133.29(13) . 1_545 ? OW1 Cd1 N1 86.20(12) . . ? O1 Cd1 N1 93.58(13) . . ? O8 Cd1 N1 85.98(12) . . ? N4 Cd1 N1 138.37(12) 1_545 . ? OW1 Cd1 O7 94.87(13) . . ? O1 Cd1 O7 87.80(13) . . ? O8 Cd1 O7 53.55(12) . . ? N4 Cd1 O7 81.49(12) 1_545 . ? N1 Cd1 O7 139.44(12) . . ? OW1 Cd1 O2 123.82(12) . . ? O1 Cd1 O2 52.54(12) . . ? O8 Cd1 O2 139.08(13) . . ? N4 Cd1 O2 79.67(11) 1_545 . ? N1 Cd1 O2 74.30(11) . . ? O7 Cd1 O2 133.37(12) . . ? OW1 Cd1 C15 92.65(15) . . ? O1 Cd1 C15 91.00(14) . . ? O8 Cd1 C15 26.22(14) . . ? N4 Cd1 C15 108.16(14) 1_545 . ? N1 Cd1 C15 112.14(14) . . ? O7 Cd1 C15 27.33(14) . . ? O2 Cd1 C15 143.53(13) . . ? O10A Cd2 OW2 139.3(3) 1_664 . ? O10A Cd2 O4 111.9(3) 1_664 . ? OW2 Cd2 O4 99.37(16) . . ? O10A Cd2 N10 85.3(3) 1_664 . ? OW2 Cd2 N10 87.97(13) . . ? O4 Cd2 N10 138.80(12) . . ? O10A Cd2 N6 75.4(3) 1_664 1_655 ? OW2 Cd2 N6 81.79(13) . 1_655 ? O4 Cd2 N6 85.84(12) . 1_655 ? N10 Cd2 N6 135.34(12) . 1_655 ? O10A Cd2 O3 116.2(3) 1_664 . ? OW2 Cd2 O3 102.95(14) . . ? O4 Cd2 O3 54.33(11) . . ? N10 Cd2 O3 84.49(12) . . ? N6 Cd2 O3 140.17(12) 1_655 . ? O10A Cd2 O10 9.8(5) 1_664 1_664 ? OW2 Cd2 O10 132.7(3) . 1_664 ? O4 Cd2 O10 121.5(3) . 1_664 ? N10 Cd2 O10 76.8(3) . 1_664 ? N6 Cd2 O10 78.9(3) 1_655 1_664 ? O3 Cd2 O10 119.4(3) . 1_664 ? O10A Cd2 C14 117.5(3) 1_664 . ? OW2 Cd2 C14 102.32(15) . . ? O4 Cd2 C14 27.16(13) . . ? N10 Cd2 C14 111.64(14) . . ? N6 Cd2 C14 113.01(13) 1_655 . ? O3 Cd2 C14 27.17(12) . . ? O10 Cd2 C14 125.0(3) 1_664 . ? O5 S1 O6 120.0(3) . . ? O5 S1 C3 107.7(2) . . ? O6 S1 C3 108.5(2) . . ? O5 S1 C8 109.0(2) . . ? O6 S1 C8 108.4(2) . . ? C3 S1 C8 101.7(2) . . ? O12 S2 O11A 96.6(7) . . ? O12 S2 O12A 21.5(8) . . ? O11A S2 O12A 117.9(7) . . ? O12 S2 O11 117.2(7) . . ? O11A S2 O11 20.7(7) . . ? O12A S2 O11 138.3(7) . . ? O12 S2 C22 115.1(7) . . ? O11A S2 C22 114.2(6) . . ? O12A S2 C22 100.7(6) . . ? O11 S2 C22 100.8(5) . . ? O12 S2 C19 112.1(7) . . ? O11A S2 C19 111.5(7) . . ? O12A S2 C19 104.1(7) . . ? O11 S2 C19 103.1(6) . . ? C22 S2 C19 107.1(2) . . ? C6 C1 C2 120.6(4) . . ? C6 C1 H1A 119.7 . . ? C2 C1 H1A 119.7 . . ? C3 C2 C1 119.2(4) . . ? C3 C2 H2A 120.4 . . ? C1 C2 H2A 120.4 . . ? C2 C3 C4 121.4(4) . . ? C2 C3 S1 119.7(4) . . ? C4 C3 S1 118.8(4) . . ? C3 C4 C5 118.4(4) . . ? C3 C4 H4A 120.8 . . ? C5 C4 H4A 120.8 . . ? C6 C5 C4 121.3(4) . . ? C6 C5 H5A 119.4 . . ? C4 C5 H5A 119.4 . . ? C1 C6 C5 119.1(4) . . ? C1 C6 C7 120.6(4) . . ? C5 C6 C7 120.3(4) . . ? O2 C7 O1 124.4(5) . . ? O2 C7 C6 117.6(5) . . ? O1 C7 C6 118.0(4) . . ? C13 C8 C9 122.1(4) . . ? C13 C8 S1 120.1(4) . . ? C9 C8 S1 117.7(4) . . ? C10 C9 C8 118.5(4) . . ? C10 C9 H9A 120.8 . . ? C8 C9 H9A 120.8 . . ? C9 C10 C11 120.7(4) . . ? C9 C10 H10A 119.7 . . ? C11 C10 H10A 119.7 . . ? C10 C11 C12 119.6(4) . . ? C10 C11 C14 120.1(4) . . ? C12 C11 C14 120.2(4) . . ? C11 C12 C13 120.8(4) . . ? C11 C12 H12A 119.6 . . ? C13 C12 H12A 119.6 . . ? C8 C13 C12 118.3(4) . . ? C8 C13 H13A 120.9 . . ? C12 C13 H13A 120.9 . . ? O3 C14 O4 122.7(4) . . ? O3 C14 C11 120.1(4) . . ? O4 C14 C11 117.3(4) . . ? O3 C14 Cd2 65.7(2) . . ? O4 C14 Cd2 56.9(2) . . ? C11 C14 Cd2 174.2(3) . . ? O8 C15 O7 122.2(4) . . ? O8 C15 C16 119.4(5) . . ? O7 C15 C16 118.3(5) . . ? O8 C15 Cd1 57.6(3) . . ? O7 C15 Cd1 64.7(2) . . ? C16 C15 Cd1 174.4(3) . . ? C17 C16 C21 119.8(4) . . ? C17 C16 C15 118.6(4) . . ? C21 C16 C15 121.4(4) . . ? C16 C17 C18 120.5(5) . . ? C16 C17 H17A 119.8 . . ? C18 C17 H17A 119.8 . . ? C19 C18 C17 119.3(5) . . ? C19 C18 H18A 120.3 . . ? C17 C18 H18A 120.3 . . ? C18 C19 C20 121.8(4) . . ? C18 C19 S2 119.3(4) . . ? C20 C19 S2 118.6(4) . . ? C19 C20 C21 118.8(5) . . ? C19 C20 H20A 120.6 . . ? C21 C20 H20A 120.6 . . ? C16 C21 C20 119.7(5) . . ? C16 C21 H21A 120.1 . . ? C20 C21 H21A 120.1 . . ? C23 C22 C27 121.3(5) . . ? C23 C22 S2 119.0(4) . . ? C27 C22 S2 119.6(4) . . ? C22 C23 C24 118.8(5) . . ? C22 C23 H23A 120.6 . . ? C24 C23 H23A 120.6 . . ? C25 C24 C23 121.7(4) . . ? C25 C24 H24A 119.1 . . ? C23 C24 H24A 119.1 . . ? C24 C25 C26 118.6(5) . . ? C24 C25 C28 121.6(5) . . ? C26 C25 C28 119.9(5) . . ? C25 C26 C27 120.5(5) . . ? C25 C26 H26A 119.7 . . ? C27 C26 H26A 119.7 . . ? C22 C27 C26 119.0(5) . . ? C22 C27 H27A 120.5 . . ? C26 C27 H27A 120.5 . . ? O9 C28 O10A 92.4(9) . . ? O9 C28 O10 110.9(10) . . ? O10A C28 O10 23.6(8) . . ? O9 C28 O9A 43.2(5) . . ? O10A C28 O9A 128.4(9) . . ? O10 C28 O9A 135.3(8) . . ? O9 C28 C25 136.1(7) . . ? O10A C28 C25 122.0(8) . . ? O10 C28 C25 110.3(7) . . ? O9A C28 C25 109.5(6) . . ? N1 C29 C30 123.1(4) . . ? N1 C29 H29A 118.4 . . ? C30 C29 H29A 118.4 . . ? C31 C30 C29 119.7(4) . . ? C31 C30 H30A 120.1 . . ? C29 C30 H30A 120.1 . . ? C30 C31 C32 117.4(4) . . ? C30 C31 C34 121.1(3) . . ? C32 C31 C34 121.4(3) . . ? C33 C32 C31 119.2(4) . . ? C33 C32 H32A 120.4 . . ? C31 C32 H32A 120.4 . . ? N1 C33 C32 123.9(4) . . ? N1 C33 H33A 118.0 . . ? C32 C33 H33A 118.0 . . ? N2 C34 N3 110.9(3) . . ? N2 C34 C31 125.3(3) . . ? N3 C34 C31 123.8(3) . . ? N2 C35 C36 109.7(3) . . ? N2 C35 C42 120.0(3) . . ? C36 C35 C42 130.2(4) . . ? N3 C36 C35 105.3(3) . . ? N3 C36 C37 122.0(3) . . ? C35 C36 C37 132.5(4) . . ? C41 C37 C38 114.9(4) . . ? C41 C37 C36 122.2(4) . . ? C38 C37 C36 122.9(4) . . ? C39 C38 C37 120.2(5) . . ? C39 C38 H38A 119.9 . . ? C37 C38 H38A 119.9 . . ? N5 C39 C38 124.7(5) . . ? N5 C39 H39A 117.6 . . ? C38 C39 H39A 117.6 . . ? N5 C40 C41 124.3(5) . . ? N5 C40 H40A 117.9 . . ? C41 C40 H40A 117.9 . . ? C40 C41 C37 120.3(5) . . ? C40 C41 H41A 119.8 . . ? C37 C41 H41A 119.8 . . ? C43 C42 C46 116.0(4) . . ? C43 C42 C35 122.4(4) . . ? C46 C42 C35 121.6(4) . . ? C42 C43 C44 120.6(4) . . ? C42 C43 H43A 119.7 . . ? C44 C43 H43A 119.7 . . ? N4 C44 C43 124.2(4) . . ? N4 C44 H44A 117.9 . . ? C43 C44 H44A 117.9 . . ? N4 C45 C46 123.5(4) . . ? N4 C45 H45A 118.3 . . ? C46 C45 H45A 118.3 . . ? C45 C46 C42 119.1(4) . . ? C45 C46 H46A 120.4 . . ? C42 C46 H46A 120.4 . . ? N6 C47 C48 123.5(4) . . ? N6 C47 H47A 118.3 . . ? C48 C47 H47A 118.3 . . ? C49 C48 C47 120.3(4) . . ? C49 C48 H48A 119.8 . . ? C47 C48 H48A 119.8 . . ? C48 C49 C50 116.0(4) . . ? C48 C49 C52 121.0(4) . . ? C50 C49 C52 123.0(4) . . ? C51 C50 C49 120.0(4) . . ? C51 C50 H50A 120.0 . . ? C49 C50 H50A 120.0 . . ? N6 C51 C50 123.7(4) . . ? N6 C51 H51A 118.2 . . ? C50 C51 H51A 118.2 . . ? N7 C52 N8 111.6(3) . . ? N7 C52 C49 124.4(3) . . ? N8 C52 C49 124.0(4) . . ? N7 C53 C54 109.2(3) . . ? N7 C53 C60 119.6(3) . . ? C54 C53 C60 130.9(4) . . ? N8 C54 C53 105.8(3) . . ? N8 C54 C55 120.1(3) . . ? C53 C54 C55 134.1(4) . . ? C59 C55 C56 117.0(4) . . ? C59 C55 C54 120.9(4) . . ? C56 C55 C54 122.2(4) . . ? C57 C56 C55 119.6(4) . . ? C57 C56 H56A 120.2 . . ? C55 C56 H56A 120.2 . . ? N10 C57 C56 122.8(4) . . ? N10 C57 H57A 118.6 . . ? C56 C57 H57A 118.6 . . ? N10 C58 C59 122.7(4) . . ? N10 C58 H58A 118.7 . . ? C59 C58 H58A 118.7 . . ? C55 C59 C58 120.6(4) . . ? C55 C59 H59A 119.7 . . ? C58 C59 H59A 119.7 . . ? C61 C60 C64 116.0(4) . . ? C61 C60 C53 120.9(4) . . ? C64 C60 C53 123.0(4) . . ? C60 C61 C62 120.6(5) . . ? C60 C61 H61A 119.7 . . ? C62 C61 H61A 119.7 . . ? N9 C62 C61 124.5(5) . . ? N9 C62 H62A 117.8 . . ? C61 C62 H62A 117.8 . . ? N9 C63 C64 124.5(5) . . ? N9 C63 H63A 117.8 . . ? C64 C63 H63A 117.8 . . ? C63 C64 C60 118.9(5) . . ? C63 C64 H64A 120.6 . . ? C60 C64 H64A 120.6 . . ? C33 N1 C29 116.5(3) . . ? C33 N1 Cd1 121.5(3) . . ? C29 N1 Cd1 122.0(3) . . ? C34 N2 C35 106.1(3) . . ? C34 N3 C36 108.0(3) . . ? C34 N3 H3A 133(3) . . ? C36 N3 H3A 118(3) . . ? C44 N4 C45 116.5(4) . . ? C44 N4 Cd1 120.5(3) . 1_565 ? C45 N4 Cd1 123.1(3) . 1_565 ? C39 N5 C40 115.5(4) . . ? C47 N6 C51 116.5(4) . . ? C47 N6 Cd2 120.9(3) . 1_455 ? C51 N6 Cd2 122.5(3) . 1_455 ? C52 N7 C53 106.1(3) . . ? C52 N8 C54 107.3(3) . . ? C52 N8 H8A 122(3) . . ? C54 N8 H8A 130(3) . . ? C62 N9 C63 115.4(5) . . ? C57 N10 C58 117.3(4) . . ? C57 N10 Cd2 127.1(3) . . ? C58 N10 Cd2 115.3(3) . . ? C7 O1 Cd1 98.7(3) . . ? Cd1 OW1 HW1B 113.0 . . ? Cd1 OW1 HW1A 127.2 . . ? HW1B OW1 HW1A 115.3 . . ? Cd2 OW2 HW2A 130.6 . . ? Cd2 OW2 HW2B 128.4 . . ? HW2A OW2 HW2B 100.1 . . ? C7 O2 Cd1 83.9(3) . . ? HW3A OW3 HW3B 92.2 . . ? C14 O3 Cd2 87.1(3) . . ? C14 O4 Cd2 95.9(3) . . ? HW4B OW4 HW4A 108.6 . . ? HW5A OW5 HW5B 87.0 . . ? HW6A OW6 HW6B 101.5 . . ? C15 O7 Cd1 88.0(3) . . ? HW8A OW8 HW8B 111.9 . . ? C15 O8 Cd1 96.2(3) . . ? C28 O10 Cd2 102.3(8) . 1_446 ? C28 O10A Cd2 129.8(9) . 1_446 ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.334 _refine_diff_density_min -0.739 _refine_diff_density_rms 0.106 #===END data_compound-2 _database_code_depnum_ccdc_archive 'CCDC 825671' #TrackingRef '- compounds 1-3.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H21 N5 O6 S Zn' _chemical_formula_weight 668.97 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 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 24.122(3) _cell_length_b 12.7390(14) _cell_length_c 20.106(2) _cell_angle_alpha 90.00 _cell_angle_beta 108.8320(10) _cell_angle_gamma 90.00 _cell_volume 5847.8(11) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 26363 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 27.56 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.46 _exptl_crystal_size_min 0.39 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.520 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2736 _exptl_absorpt_coefficient_mu 0.967 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6594 _exptl_absorpt_correction_T_max 0.7043 _exptl_absorpt_process_details 'SADABS(Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26363 _diffrn_reflns_av_R_equivalents 0.0337 _diffrn_reflns_av_sigmaI/netI 0.0336 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 27.56 _reflns_number_total 6719 _reflns_number_gt 4783 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material 'SHELXL-97 (Sheldrick, 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^)+(0.0873P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6719 _refine_ls_number_parameters 410 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0643 _refine_ls_R_factor_gt 0.0405 _refine_ls_wR_factor_ref 0.1337 _refine_ls_wR_factor_gt 0.1182 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.000 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.074849(11) 0.74905(2) 0.495849(13) 0.03696(11) Uani 1 1 d . . . S1 S 0.12749(4) 0.60281(6) 0.92321(3) 0.0541(2) Uani 1 1 d . . . C1 C 0.07938(13) 0.6268(3) 0.71332(15) 0.0701(10) Uani 1 1 d . . . H1A H 0.0446 0.6220 0.6759 0.084 Uiso 1 1 calc R . . C2 C 0.07872(14) 0.6127(3) 0.78145(16) 0.0731(10) Uani 1 1 d . . . H2A H 0.0437 0.5982 0.7896 0.088 Uiso 1 1 calc R . . C3 C 0.12962(12) 0.6200(2) 0.83646(13) 0.0452(6) Uani 1 1 d . . . C4 C 0.18143(13) 0.6389(3) 0.82402(15) 0.0611(8) Uani 1 1 d . . . H4A H 0.2162 0.6430 0.8615 0.073 Uiso 1 1 calc R . . C5 C 0.18211(12) 0.6519(3) 0.75629(14) 0.0557(8) Uani 1 1 d . . . H5A H 0.2175 0.6633 0.7483 0.067 Uiso 1 1 calc R . . C6 C 0.13108(11) 0.64805(19) 0.70037(13) 0.0409(6) Uani 1 1 d . . . C7 C 0.13062(13) 0.6706(2) 0.62673(13) 0.0449(6) Uani 1 1 d . . . C8 C 0.12348(13) 0.7322(2) 0.95370(14) 0.0456(6) Uani 1 1 d . . . C9 C 0.17145(15) 0.7751(3) 1.0010(2) 0.0733(10) Uani 1 1 d . . . H9A H 0.2062 0.7372 1.0175 0.088 Uiso 1 1 calc R . . C10 C 0.16806(13) 0.8762(3) 1.02442(18) 0.0744(11) Uani 1 1 d . . . H10A H 0.2008 0.9057 1.0573 0.089 Uiso 1 1 calc R . . C11 C 0.11781(10) 0.9339(2) 1.00057(12) 0.0402(6) Uani 1 1 d . . . C12 C 0.06922(12) 0.8876(2) 0.95464(18) 0.0605(8) Uani 1 1 d . . . H12A H 0.0342 0.9247 0.9392 0.073 Uiso 1 1 calc R . . C13 C 0.07176(14) 0.7869(3) 0.93110(19) 0.0693(10) Uani 1 1 d . . . H13A H 0.0385 0.7560 0.9000 0.083 Uiso 1 1 calc R . . C14 C 0.11671(11) 1.0458(2) 1.02368(12) 0.0410(6) Uani 1 1 d . . . C15 C -0.03946(11) 0.6355(2) 0.44462(13) 0.0433(6) Uani 1 1 d . . . H15A H -0.0211 0.5915 0.4821 0.052 Uiso 1 1 calc R . . C16 C -0.09461(10) 0.6093(2) 0.40137(12) 0.0420(6) Uani 1 1 d . . . H16A H -0.1131 0.5493 0.4101 0.050 Uiso 1 1 calc R . . C17 C -0.12249(10) 0.67339(19) 0.34458(12) 0.0371(5) Uani 1 1 d . . . C18 C -0.09424(12) 0.7644(2) 0.33681(14) 0.0443(6) Uani 1 1 d . . . H18A H -0.1122 0.8112 0.3008 0.053 Uiso 1 1 calc R . . C19 C -0.03921(11) 0.7856(2) 0.38269(14) 0.0451(6) Uani 1 1 d . . . H19A H -0.0208 0.8474 0.3768 0.054 Uiso 1 1 calc R . . C20 C -0.18054(10) 0.6436(2) 0.29624(12) 0.0397(5) Uani 1 1 d . . . C21 C -0.20273(10) 0.6454(2) 0.22370(13) 0.0398(5) Uani 1 1 d . . . C22 C -0.17462(10) 0.6651(2) 0.17037(12) 0.0396(6) Uani 1 1 d . . . C23 C -0.11487(11) 0.6545(2) 0.18598(13) 0.0448(6) Uani 1 1 d . . . H23A H -0.0920 0.6336 0.2308 0.054 Uiso 1 1 calc R . . C24 C -0.08900(11) 0.6746(2) 0.13591(13) 0.0444(6) Uani 1 1 d . . . H24A H -0.0485 0.6684 0.1484 0.053 Uiso 1 1 calc R . . C25 C -0.17629(13) 0.7050(3) 0.05397(15) 0.0709(10) Uani 1 1 d . . . H25A H -0.1984 0.7189 0.0076 0.085 Uiso 1 1 calc R . . C26 C -0.20550(12) 0.6880(3) 0.10165(15) 0.0703(10) Uani 1 1 d . . . H26A H -0.2462 0.6920 0.0873 0.084 Uiso 1 1 calc R . . C27 C -0.26888(10) 0.5884(2) 0.26855(13) 0.0432(6) Uani 1 1 d . . . C28 C -0.32411(11) 0.5476(2) 0.27531(14) 0.0463(6) Uani 1 1 d . . . C29 C -0.32225(13) 0.4943(3) 0.33588(16) 0.0643(8) Uani 1 1 d . . . H29A H -0.2869 0.4840 0.3716 0.077 Uiso 1 1 calc R . . C30 C -0.37353(15) 0.4570(3) 0.34214(18) 0.0715(9) Uani 1 1 d . . . H30A H -0.3716 0.4201 0.3827 0.086 Uiso 1 1 calc R . . C31 C -0.42708(12) 0.5209(3) 0.23646(18) 0.0635(8) Uani 1 1 d . . . H31A H -0.4632 0.5302 0.2019 0.076 Uiso 1 1 calc R . . C32 C -0.37799(11) 0.5613(2) 0.22415(16) 0.0523(7) Uani 1 1 d . . . H32A H -0.3811 0.5967 0.1826 0.063 Uiso 1 1 calc R . . N1 N -0.01104(9) 0.72149(17) 0.43516(10) 0.0375(5) Uani 1 1 d . . . N2 N -0.11867(9) 0.70255(18) 0.07044(10) 0.0418(5) Uani 1 1 d . . . N3 N -0.25943(9) 0.61105(18) 0.20772(11) 0.0423(5) Uani 1 1 d D . . N4 N -0.22214(9) 0.60724(18) 0.32378(11) 0.0439(5) Uani 1 1 d . . . N5 N -0.42582(11) 0.4698(2) 0.29433(16) 0.0698(8) Uani 1 1 d . . . O1 O 0.07932(8) 0.68292(16) 0.58240(9) 0.0561(5) Uani 1 1 d . . . O2 O 0.17652(9) 0.67797(18) 0.61377(11) 0.0652(6) Uani 1 1 d . . . O3 O 0.15834(9) 1.08235(18) 1.07037(12) 0.0718(6) Uani 1 1 d . . . O4 O 0.07199(8) 1.09873(15) 0.98965(10) 0.0551(5) Uani 1 1 d . . . O5 O 0.07281(11) 0.55107(16) 0.91783(11) 0.0692(6) Uani 1 1 d . . . O6 O 0.18221(11) 0.55810(18) 0.96470(10) 0.0739(7) Uani 1 1 d . . . H3A H -0.2805(12) 0.602(3) 0.1628(7) 0.079(11) Uiso 1 1 d 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 0.03553(17) 0.04778(19) 0.02571(16) 0.00148(11) 0.00729(12) -0.00329(12) S1 0.0852(5) 0.0470(4) 0.0336(3) 0.0030(3) 0.0240(3) 0.0115(4) C1 0.0478(16) 0.123(3) 0.0335(15) 0.0082(17) 0.0047(13) -0.0097(18) C2 0.0564(18) 0.125(3) 0.0400(16) 0.0059(18) 0.0190(14) -0.0081(19) C3 0.0595(16) 0.0468(15) 0.0295(12) 0.0022(10) 0.0147(12) 0.0074(12) C4 0.0519(16) 0.091(2) 0.0345(15) 0.0077(15) 0.0057(13) 0.0137(16) C5 0.0451(15) 0.079(2) 0.0420(16) 0.0108(14) 0.0124(13) 0.0129(14) C6 0.0493(14) 0.0426(14) 0.0292(12) 0.0009(10) 0.0103(11) 0.0023(11) C7 0.0581(16) 0.0425(14) 0.0332(13) 0.0023(10) 0.0134(12) -0.0026(12) C8 0.0622(18) 0.0442(15) 0.0307(13) -0.0004(10) 0.0154(12) 0.0041(12) C9 0.0557(19) 0.075(2) 0.073(2) -0.0145(18) -0.0019(17) 0.0218(16) C10 0.0535(17) 0.071(2) 0.072(2) -0.0244(18) -0.0164(16) 0.0115(16) C11 0.0405(13) 0.0483(15) 0.0301(12) 0.0017(10) 0.0093(10) 0.0020(11) C12 0.0480(16) 0.0444(16) 0.073(2) -0.0094(14) -0.0030(14) 0.0058(12) C13 0.0596(19) 0.0528(18) 0.074(2) -0.0161(17) -0.0086(17) -0.0018(15) C14 0.0432(13) 0.0478(15) 0.0311(12) -0.0031(11) 0.0108(11) -0.0038(12) C15 0.0457(14) 0.0499(15) 0.0318(12) 0.0068(11) 0.0091(11) -0.0028(12) C16 0.0438(13) 0.0488(15) 0.0321(12) 0.0037(11) 0.0103(11) -0.0113(11) C17 0.0343(12) 0.0491(14) 0.0278(12) -0.0022(10) 0.0098(10) -0.0027(10) C18 0.0418(13) 0.0471(15) 0.0361(14) 0.0087(11) 0.0019(11) -0.0017(11) C19 0.0450(14) 0.0426(13) 0.0411(14) 0.0018(11) 0.0049(12) -0.0069(12) C20 0.0353(12) 0.0512(15) 0.0320(12) -0.0014(11) 0.0101(10) -0.0043(11) C21 0.0325(12) 0.0499(14) 0.0344(13) 0.0018(11) 0.0072(10) -0.0043(11) C22 0.0371(12) 0.0489(15) 0.0309(12) -0.0010(10) 0.0085(10) -0.0035(11) C23 0.0400(13) 0.0622(17) 0.0298(12) 0.0060(11) 0.0080(11) 0.0041(12) C24 0.0348(12) 0.0600(17) 0.0381(14) 0.0035(12) 0.0114(11) 0.0036(11) C25 0.0412(15) 0.137(3) 0.0313(15) 0.0212(18) 0.0068(12) 0.0060(18) C26 0.0346(14) 0.132(3) 0.0418(17) 0.0227(18) 0.0083(12) 0.0050(17) C27 0.0371(13) 0.0537(15) 0.0377(13) 0.0008(11) 0.0108(11) -0.0059(11) C28 0.0409(13) 0.0549(17) 0.0451(14) -0.0041(12) 0.0166(11) -0.0082(12) C29 0.0542(17) 0.087(2) 0.0514(17) 0.0081(17) 0.0171(14) -0.0147(16) C30 0.073(2) 0.090(3) 0.062(2) 0.0011(18) 0.0372(18) -0.0202(19) C31 0.0396(15) 0.076(2) 0.075(2) -0.0145(18) 0.0185(15) -0.0070(14) C32 0.0403(14) 0.0619(18) 0.0532(17) -0.0056(14) 0.0130(12) -0.0041(13) N1 0.0346(10) 0.0488(12) 0.0269(10) 0.0003(8) 0.0070(8) -0.0022(9) N2 0.0378(11) 0.0564(13) 0.0310(11) 0.0018(10) 0.0106(9) 0.0002(10) N3 0.0331(10) 0.0586(14) 0.0313(11) -0.0020(10) 0.0051(9) -0.0067(9) N4 0.0372(10) 0.0590(14) 0.0340(11) 0.0023(10) 0.0094(9) -0.0086(10) N5 0.0512(15) 0.089(2) 0.0761(19) -0.0145(16) 0.0305(14) -0.0190(14) O1 0.0568(12) 0.0757(14) 0.0307(9) 0.0128(9) 0.0072(9) -0.0087(10) O2 0.0684(14) 0.0868(17) 0.0476(12) 0.0067(11) 0.0288(11) 0.0009(11) O3 0.0649(13) 0.0689(14) 0.0616(14) -0.0212(11) -0.0072(11) -0.0019(11) O4 0.0536(11) 0.0448(11) 0.0565(12) -0.0039(9) 0.0034(9) 0.0045(9) O5 0.1129(18) 0.0523(12) 0.0583(13) -0.0076(10) 0.0498(13) -0.0145(12) O6 0.1120(18) 0.0678(14) 0.0377(11) 0.0094(10) 0.0183(11) 0.0400(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O1 1.9047(18) . ? Zn1 O4 1.943(2) 6_575 ? Zn1 N2 2.038(2) 2 ? Zn1 N1 2.067(2) . ? S1 O6 1.432(2) . ? S1 O5 1.447(2) . ? S1 C8 1.772(3) . ? S1 C3 1.775(3) . ? C1 C6 1.380(4) . ? C1 C2 1.387(4) . ? C1 H1A 0.9300 . ? C2 C3 1.365(4) . ? C2 H2A 0.9300 . ? C3 C4 1.373(4) . ? C4 C5 1.377(4) . ? C4 H4A 0.9300 . ? C5 C6 1.374(4) . ? C5 H5A 0.9300 . ? C6 C7 1.505(3) . ? C7 O2 1.220(3) . ? C7 O1 1.280(3) . ? C8 C9 1.353(4) . ? C8 C13 1.372(4) . ? C9 C10 1.383(5) . ? C9 H9A 0.9300 . ? C10 C11 1.365(4) . ? C10 H10A 0.9300 . ? C11 C12 1.369(4) . ? C11 C14 1.503(4) . ? C12 C13 1.376(4) . ? C12 H12A 0.9300 . ? C13 H13A 0.9300 . ? C14 O3 1.224(3) . ? C14 O4 1.269(3) . ? C15 N1 1.338(3) . ? C15 C16 1.375(3) . ? C15 H15A 0.9300 . ? C16 C17 1.388(3) . ? C16 H16A 0.9300 . ? C17 C18 1.379(3) . ? C17 C20 1.473(3) . ? C18 C19 1.377(4) . ? C18 H18A 0.9300 . ? C19 N1 1.334(3) . ? C19 H19A 0.9300 . ? C20 N4 1.374(3) . ? C20 C21 1.382(3) . ? C21 N3 1.372(3) . ? C21 C22 1.463(3) . ? C22 C26 1.373(4) . ? C22 C23 1.379(3) . ? C23 C24 1.369(4) . ? C23 H23A 0.9300 . ? C24 N2 1.328(3) . ? C24 H24A 0.9300 . ? C25 N2 1.321(3) . ? C25 C26 1.378(4) . ? C25 H25A 0.9300 . ? C26 H26A 0.9300 . ? C27 N4 1.324(3) . ? C27 N3 1.346(3) . ? C27 C28 1.476(3) . ? C28 C29 1.383(4) . ? C28 C32 1.384(4) . ? C29 C30 1.369(4) . ? C29 H29A 0.9300 . ? C30 N5 1.326(4) . ? C30 H30A 0.9300 . ? C31 N5 1.325(4) . ? C31 C32 1.385(4) . ? C31 H31A 0.9300 . ? C32 H32A 0.9300 . ? N2 Zn1 2.038(2) 2 ? N3 H3A 0.889(10) . ? O4 Zn1 1.943(2) 6_576 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn1 O4 119.36(9) . 6_575 ? O1 Zn1 N2 125.49(9) . 2 ? O4 Zn1 N2 105.26(9) 6_575 2 ? O1 Zn1 N1 102.39(8) . . ? O4 Zn1 N1 97.10(8) 6_575 . ? N2 Zn1 N1 101.37(8) 2 . ? O6 S1 O5 120.59(15) . . ? O6 S1 C8 108.15(14) . . ? O5 S1 C8 107.41(14) . . ? O6 S1 C3 107.94(13) . . ? O5 S1 C3 107.32(13) . . ? C8 S1 C3 104.30(13) . . ? C6 C1 C2 120.7(3) . . ? C6 C1 H1A 119.6 . . ? C2 C1 H1A 119.6 . . ? C3 C2 C1 119.8(3) . . ? C3 C2 H2A 120.1 . . ? C1 C2 H2A 120.1 . . ? C2 C3 C4 119.9(3) . . ? C2 C3 S1 118.9(2) . . ? C4 C3 S1 121.2(2) . . ? C3 C4 C5 120.2(3) . . ? C3 C4 H4A 119.9 . . ? C5 C4 H4A 119.9 . . ? C6 C5 C4 120.8(3) . . ? C6 C5 H5A 119.6 . . ? C4 C5 H5A 119.6 . . ? C5 C6 C1 118.5(2) . . ? C5 C6 C7 121.2(2) . . ? C1 C6 C7 120.2(2) . . ? O2 C7 O1 125.6(2) . . ? O2 C7 C6 120.4(2) . . ? O1 C7 C6 114.0(2) . . ? C9 C8 C13 120.5(3) . . ? C9 C8 S1 119.3(2) . . ? C13 C8 S1 120.2(2) . . ? C8 C9 C10 119.0(3) . . ? C8 C9 H9A 120.5 . . ? C10 C9 H9A 120.5 . . ? C11 C10 C9 121.7(3) . . ? C11 C10 H10A 119.2 . . ? C9 C10 H10A 119.2 . . ? C10 C11 C12 118.4(3) . . ? C10 C11 C14 120.3(2) . . ? C12 C11 C14 121.3(2) . . ? C11 C12 C13 120.6(3) . . ? C11 C12 H12A 119.7 . . ? C13 C12 H12A 119.7 . . ? C8 C13 C12 119.8(3) . . ? C8 C13 H13A 120.1 . . ? C12 C13 H13A 120.1 . . ? O3 C14 O4 123.8(3) . . ? O3 C14 C11 120.4(2) . . ? O4 C14 C11 115.7(2) . . ? N1 C15 C16 123.0(2) . . ? N1 C15 H15A 118.5 . . ? C16 C15 H15A 118.5 . . ? C15 C16 C17 119.4(2) . . ? C15 C16 H16A 120.3 . . ? C17 C16 H16A 120.3 . . ? C18 C17 C16 117.5(2) . . ? C18 C17 C20 122.7(2) . . ? C16 C17 C20 119.8(2) . . ? C19 C18 C17 119.6(2) . . ? C19 C18 H18A 120.2 . . ? C17 C18 H18A 120.2 . . ? N1 C19 C18 123.0(2) . . ? N1 C19 H19A 118.5 . . ? C18 C19 H19A 118.5 . . ? N4 C20 C21 110.3(2) . . ? N4 C20 C17 118.9(2) . . ? C21 C20 C17 130.8(2) . . ? N3 C21 C20 105.0(2) . . ? N3 C21 C22 123.1(2) . . ? C20 C21 C22 131.5(2) . . ? C26 C22 C23 116.0(2) . . ? C26 C22 C21 123.0(2) . . ? C23 C22 C21 120.9(2) . . ? C24 C23 C22 120.4(2) . . ? C24 C23 H23A 119.8 . . ? C22 C23 H23A 119.8 . . ? N2 C24 C23 123.5(2) . . ? N2 C24 H24A 118.3 . . ? C23 C24 H24A 118.3 . . ? N2 C25 C26 123.7(3) . . ? N2 C25 H25A 118.2 . . ? C26 C25 H25A 118.2 . . ? C22 C26 C25 120.0(3) . . ? C22 C26 H26A 120.0 . . ? C25 C26 H26A 120.0 . . ? N4 C27 N3 112.0(2) . . ? N4 C27 C28 122.4(2) . . ? N3 C27 C28 125.6(2) . . ? C29 C28 C32 118.2(2) . . ? C29 C28 C27 118.7(2) . . ? C32 C28 C27 123.1(3) . . ? C30 C29 C28 118.6(3) . . ? C30 C29 H29A 120.7 . . ? C28 C29 H29A 120.7 . . ? N5 C30 C29 124.5(3) . . ? N5 C30 H30A 117.7 . . ? C29 C30 H30A 117.7 . . ? N5 C31 C32 124.1(3) . . ? N5 C31 H31A 117.9 . . ? C32 C31 H31A 117.9 . . ? C28 C32 C31 118.2(3) . . ? C28 C32 H32A 120.9 . . ? C31 C32 H32A 120.9 . . ? C19 N1 C15 117.4(2) . . ? C19 N1 Zn1 121.37(17) . . ? C15 N1 Zn1 121.14(17) . . ? C25 N2 C24 116.2(2) . . ? C25 N2 Zn1 123.71(18) . 2 ? C24 N2 Zn1 119.92(17) . 2 ? C27 N3 C21 107.7(2) . . ? C27 N3 H3A 133(2) . . ? C21 N3 H3A 119(2) . . ? C27 N4 C20 105.0(2) . . ? C31 N5 C30 116.4(3) . . ? C7 O1 Zn1 116.58(17) . . ? C14 O4 Zn1 119.29(17) . 6_576 ? 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 N3 H3A O3 0.889(10) 1.981(12) 2.856(3) 168(3) 3_444 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.206 _refine_diff_density_min -0.357 _refine_diff_density_rms 0.058 #===END data_compound-3 _database_code_depnum_ccdc_archive 'CCDC 825672' #TrackingRef '- compounds 1-3.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H22 Cd N4 O6 S' _chemical_formula_weight 606.92 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.8037(4) _cell_length_b 16.6966(6) _cell_length_c 12.9072(4) _cell_angle_alpha 90.00 _cell_angle_beta 106.7260(10) _cell_angle_gamma 90.00 _cell_volume 2436.15(14) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 20974 _cell_measurement_theta_min 1.80 _cell_measurement_theta_max 27.51 _exptl_crystal_description block _exptl_crystal_colour 'light pink' _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.31 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.655 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 _exptl_absorpt_coefficient_mu 1.030 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6715 _exptl_absorpt_correction_T_max 0.7407 _exptl_absorpt_process_details 'SADABS(Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20974 _diffrn_reflns_av_R_equivalents 0.0220 _diffrn_reflns_av_sigmaI/netI 0.0214 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 27.51 _reflns_number_total 5528 _reflns_number_gt 4961 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material 'SHELXL-97 (Sheldrick, 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^)+(0.1000P)^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 5528 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0471 _refine_ls_R_factor_gt 0.0428 _refine_ls_wR_factor_ref 0.1591 _refine_ls_wR_factor_gt 0.1558 _refine_ls_goodness_of_fit_ref 1.318 _refine_ls_restrained_S_all 1.318 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.20547(2) 0.075147(15) 0.732297(19) 0.03476(13) Uani 1 1 d . . . S1 S 0.69252(8) 0.35171(5) 1.24309(6) 0.0355(2) Uani 1 1 d . . . C1 C 0.4359(3) 0.2008(2) 0.9908(3) 0.0367(7) Uani 1 1 d . . . C2 C 0.3987(3) 0.2695(2) 1.0298(3) 0.0387(7) Uani 1 1 d . . . H2A H 0.3212 0.2870 1.0009 0.046 Uiso 1 1 calc R . . C3 C 0.4752(3) 0.3129(2) 1.1114(3) 0.0363(7) Uani 1 1 d . . . H3A H 0.4487 0.3577 1.1402 0.044 Uiso 1 1 calc R . . C4 C 0.5931(3) 0.2885(2) 1.1503(2) 0.0320(6) Uani 1 1 d . . . C5 C 0.6325(3) 0.2192(2) 1.1114(3) 0.0436(9) Uani 1 1 d . . . H5A H 0.7111 0.2032 1.1376 0.052 Uiso 1 1 calc R . . C6 C 0.5526(3) 0.1741(2) 1.0326(3) 0.0452(9) Uani 1 1 d . . . H6A H 0.5766 0.1266 1.0079 0.054 Uiso 1 1 calc R . . C7 C 0.3523(3) 0.1516(2) 0.9046(3) 0.0435(8) Uani 1 1 d . . . C8 C 0.7996(3) 0.2879(2) 1.3249(2) 0.0328(6) Uani 1 1 d . . . C9 C 0.9156(3) 0.2906(2) 1.3197(3) 0.0392(8) Uani 1 1 d . . . H9A H 0.9363 0.3233 1.2696 0.047 Uiso 1 1 calc R . . C10 C 1.0002(3) 0.2434(2) 1.3913(3) 0.0392(8) Uani 1 1 d . . . H10A H 1.0781 0.2444 1.3889 0.047 Uiso 1 1 calc R . . C11 C 0.9690(3) 0.1945(2) 1.4666(3) 0.0358(7) Uani 1 1 d . . . C12 C 0.8516(3) 0.1913(2) 1.4681(3) 0.0429(8) Uani 1 1 d . . . H12A H 0.8303 0.1582 1.5173 0.051 Uiso 1 1 calc R . . C13 C 0.7664(3) 0.2372(2) 1.3966(3) 0.0398(8) Uani 1 1 d . . . H13A H 0.6877 0.2342 1.3964 0.048 Uiso 1 1 calc R . . C14 C 1.0613(3) 0.1481(2) 1.5488(3) 0.0425(8) Uani 1 1 d . . . C15 C 0.0024(4) -0.0441(3) 0.7605(4) 0.0538(10) Uani 1 1 d . . . H15A H -0.0452 -0.0305 0.6919 0.065 Uiso 1 1 calc R . . C16 C 0.1469(4) -0.0466(3) 0.9071(4) 0.0597(11) Uani 1 1 d . . . H16A H 0.2193 -0.0366 0.9578 0.072 Uiso 1 1 calc R . . C17 C 0.0656(4) -0.0997(3) 0.9176(4) 0.0658(13) Uani 1 1 d . . . H17A H 0.0694 -0.1305 0.9785 0.079 Uiso 1 1 calc R . . C18 C -0.1250(4) -0.1562(3) 0.7951(4) 0.0555(10) Uani 1 1 d . . . H18A H -0.0947 -0.2105 0.8036 0.067 Uiso 1 1 calc R . . H18B H -0.1692 -0.1490 0.7197 0.067 Uiso 1 1 calc R . . C19 C -0.2083(4) -0.1461(3) 0.8634(4) 0.0602(11) Uani 1 1 d . . . H19A H -0.1627 -0.1285 0.9348 0.072 Uiso 1 1 calc R . . H19B H -0.2413 -0.1981 0.8715 0.072 Uiso 1 1 calc R . . C20 C -0.3100(4) -0.0876(3) 0.8208(4) 0.0537(10) Uani 1 1 d . . . H20A H -0.3415 -0.0717 0.8793 0.064 Uiso 1 1 calc R . . H20B H -0.2812 -0.0400 0.7935 0.064 Uiso 1 1 calc R . . C21 C -0.4044(4) -0.1247(3) 0.7337(5) 0.0702(14) Uani 1 1 d . . . H21A H -0.4305 -0.1730 0.7618 0.084 Uiso 1 1 calc R . . H21B H -0.3712 -0.1406 0.6762 0.084 Uiso 1 1 calc R . . C22 C -0.5696(4) -0.0313(2) 0.7413(3) 0.0457(9) Uani 1 1 d . . . H22A H -0.5465 -0.0269 0.8163 0.055 Uiso 1 1 calc R . . C23 C -0.6658(4) -0.0174(3) 0.5745(3) 0.0509(9) Uani 1 1 d . . . H23A H -0.7226 -0.0016 0.5116 0.061 Uiso 1 1 calc R . . C24 C -0.5711(5) -0.0639(3) 0.5789(4) 0.0596(12) Uani 1 1 d . . . H24A H -0.5508 -0.0858 0.5205 0.072 Uiso 1 1 calc R . . N1 N 0.1046(3) -0.0095(2) 0.8083(3) 0.0496(8) Uani 1 1 d . . . N2 N -0.0246(3) -0.1005(2) 0.8216(3) 0.0469(7) Uani 1 1 d . . . N3 N -0.5105(3) -0.07261(19) 0.6860(3) 0.0492(8) Uani 1 1 d . . . N4 N -0.6648(3) 0.00269(19) 0.6773(2) 0.0412(7) Uani 1 1 d . . . O1 O 0.2744(3) 0.1878(2) 0.8324(2) 0.0603(8) Uani 1 1 d . . . O2 O 0.3643(3) 0.07710(17) 0.9078(3) 0.0531(8) Uani 1 1 d . . . O3 O 1.0339(3) 0.1234(2) 1.6297(2) 0.0679(9) Uani 1 1 d . . . O4 O 1.1596(3) 0.1383(2) 1.5365(4) 0.0817(12) Uani 1 1 d . . . O5 O 0.7491(3) 0.40219(18) 1.1824(2) 0.0500(7) Uani 1 1 d . . . O6 O 0.6283(2) 0.38805(17) 1.3099(2) 0.0495(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.02800(18) 0.0390(2) 0.03518(18) 0.00277(9) 0.00577(12) -0.00029(9) S1 0.0386(4) 0.0340(4) 0.0305(4) -0.0005(3) 0.0045(3) 0.0026(3) C1 0.0319(16) 0.0453(19) 0.0328(15) 0.0007(14) 0.0090(13) -0.0037(14) C2 0.0278(16) 0.0438(19) 0.0430(17) 0.0084(15) 0.0078(14) 0.0043(14) C3 0.0325(16) 0.0381(18) 0.0382(16) 0.0029(14) 0.0100(14) 0.0071(14) C4 0.0300(15) 0.0362(17) 0.0281(13) -0.0010(12) 0.0055(12) 0.0016(13) C5 0.0296(17) 0.053(2) 0.0431(18) -0.0130(16) 0.0024(14) 0.0097(16) C6 0.0366(19) 0.053(2) 0.0431(18) -0.0167(17) 0.0065(15) 0.0020(16) C7 0.0328(18) 0.056(2) 0.0408(17) -0.0043(16) 0.0088(15) -0.0060(16) C8 0.0322(16) 0.0349(17) 0.0265(13) 0.0006(12) 0.0010(12) 0.0008(13) C9 0.0347(17) 0.049(2) 0.0321(15) -0.0001(14) 0.0071(14) -0.0029(15) C10 0.0317(17) 0.046(2) 0.0395(17) -0.0010(15) 0.0096(14) 0.0032(15) C11 0.0320(16) 0.0373(17) 0.0346(15) -0.0032(13) 0.0038(13) -0.0001(14) C12 0.0338(17) 0.050(2) 0.0426(17) 0.0121(16) 0.0071(15) -0.0009(15) C13 0.0284(16) 0.046(2) 0.0420(17) 0.0056(15) 0.0057(14) -0.0014(14) C14 0.0326(18) 0.0393(19) 0.0477(19) -0.0009(15) -0.0008(15) 0.0001(15) C15 0.039(2) 0.066(3) 0.051(2) 0.018(2) 0.0050(17) -0.008(2) C16 0.042(2) 0.074(3) 0.053(2) 0.020(2) -0.0033(19) -0.004(2) C17 0.051(3) 0.078(3) 0.058(3) 0.034(2) 0.000(2) -0.009(2) C18 0.047(2) 0.051(2) 0.073(3) 0.000(2) 0.023(2) -0.0088(18) C19 0.042(2) 0.073(3) 0.066(3) 0.014(2) 0.016(2) 0.004(2) C20 0.052(3) 0.051(2) 0.062(3) 0.0030(19) 0.023(2) 0.0041(19) C21 0.066(3) 0.056(3) 0.087(3) -0.012(3) 0.019(3) 0.014(2) C22 0.046(2) 0.047(2) 0.0412(18) -0.0055(16) 0.0073(16) 0.0113(17) C23 0.058(2) 0.053(2) 0.0382(18) -0.0028(16) 0.0080(17) 0.0033(19) C24 0.066(3) 0.064(3) 0.050(2) -0.012(2) 0.018(2) 0.006(2) N1 0.0397(17) 0.053(2) 0.0510(17) 0.0165(15) 0.0045(14) -0.0056(15) N2 0.0391(17) 0.0505(19) 0.0514(18) 0.0059(16) 0.0137(15) -0.0047(15) N3 0.044(2) 0.048(2) 0.054(2) -0.0112(14) 0.0122(17) 0.0043(14) N4 0.0409(16) 0.0415(17) 0.0407(15) -0.0003(13) 0.0111(13) 0.0026(13) O1 0.0519(17) 0.0592(18) 0.0510(16) -0.0021(14) -0.0150(13) -0.0001(14) O2 0.0498(18) 0.0533(19) 0.0500(17) -0.0094(12) 0.0043(14) -0.0047(12) O3 0.0562(19) 0.095(3) 0.0469(16) 0.0214(17) 0.0055(14) 0.0229(18) O4 0.0394(17) 0.087(2) 0.117(3) 0.044(2) 0.0196(19) 0.0160(17) O5 0.0535(17) 0.0450(15) 0.0460(14) 0.0082(12) 0.0056(13) -0.0096(13) O6 0.0572(17) 0.0496(16) 0.0386(12) -0.0088(12) 0.0086(12) 0.0138(13) _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 N4 2.222(3) 1_655 ? Cd1 O3 2.227(3) 1_454 ? Cd1 N1 2.247(3) . ? Cd1 O1 2.294(3) . ? Cd1 O2 2.491(3) . ? Cd1 O4 2.647(4) 1_454 ? Cd1 C7 2.713(4) . ? S1 O6 1.436(3) . ? S1 O5 1.439(3) . ? S1 C8 1.755(3) . ? S1 C4 1.765(3) . ? C1 C2 1.376(5) . ? C1 C6 1.399(5) . ? C1 C7 1.501(5) . ? C2 C3 1.379(5) . ? C2 H2A 0.9300 . ? C3 C4 1.397(5) . ? C3 H3A 0.9300 . ? C4 C5 1.395(5) . ? C5 C6 1.392(5) . ? C5 H5A 0.9300 . ? C6 H6A 0.9300 . ? C7 O1 1.259(5) . ? C7 O2 1.252(5) . ? C8 C13 1.390(5) . ? C8 C9 1.391(4) . ? C9 C10 1.393(5) . ? C9 H9A 0.9300 . ? C10 C11 1.397(5) . ? C10 H10A 0.9300 . ? C11 C12 1.393(5) . ? C11 C14 1.499(5) . ? C12 C13 1.385(5) . ? C12 H12A 0.9300 . ? C13 H13A 0.9300 . ? C14 O4 1.226(5) . ? C14 O3 1.250(5) . ? C15 N1 1.319(5) . ? C15 N2 1.325(5) . ? C15 H15A 0.9300 . ? C16 C17 1.342(7) . ? C16 N1 1.376(5) . ? C16 H16A 0.9300 . ? C17 N2 1.382(6) . ? C17 H17A 0.9300 . ? C18 N2 1.467(5) . ? C18 C19 1.507(6) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.522(6) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.472(7) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 N3 1.504(6) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 N3 1.325(5) . ? C22 N4 1.317(5) . ? C22 H22A 0.9300 . ? C23 C24 1.350(6) . ? C23 N4 1.366(5) . ? C23 H23A 0.9300 . ? C24 N3 1.369(6) . ? C24 H24A 0.9300 . ? N4 Cd1 2.222(3) 1_455 ? O3 Cd1 2.227(3) 1_656 ? O4 Cd1 2.647(4) 1_656 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Cd1 O3 126.84(12) 1_655 1_454 ? N4 Cd1 N1 107.31(13) 1_655 . ? O3 Cd1 N1 88.91(12) 1_454 . ? N4 Cd1 O1 117.45(11) 1_655 . ? O3 Cd1 O1 98.79(13) 1_454 . ? N1 Cd1 O1 114.61(13) . . ? N4 Cd1 O2 83.68(11) 1_655 . ? O3 Cd1 O2 148.61(12) 1_454 . ? N1 Cd1 O2 88.06(12) . . ? O1 Cd1 O2 54.90(9) . . ? N4 Cd1 O4 83.26(11) 1_655 1_454 ? O3 Cd1 O4 52.21(11) 1_454 1_454 ? N1 Cd1 O4 132.75(12) . 1_454 ? O1 Cd1 O4 98.78(12) . 1_454 ? O2 Cd1 O4 139.18(11) . 1_454 ? N4 Cd1 C7 100.47(11) 1_655 . ? O3 Cd1 C7 125.04(13) 1_454 . ? N1 Cd1 C7 103.42(12) . . ? O1 Cd1 C7 27.54(11) . . ? O2 Cd1 C7 27.41(10) . . ? O4 Cd1 C7 120.13(12) 1_454 . ? O6 S1 O5 119.16(19) . . ? O6 S1 C8 107.98(15) . . ? O5 S1 C8 108.43(17) . . ? O6 S1 C4 107.28(16) . . ? O5 S1 C4 107.62(16) . . ? C8 S1 C4 105.58(17) . . ? C2 C1 C6 120.4(3) . . ? C2 C1 C7 121.1(3) . . ? C6 C1 C7 118.5(3) . . ? C1 C2 C3 120.6(3) . . ? C1 C2 H2A 119.7 . . ? C3 C2 H2A 119.7 . . ? C2 C3 C4 119.2(3) . . ? C2 C3 H3A 120.4 . . ? C4 C3 H3A 120.4 . . ? C3 C4 C5 120.9(3) . . ? C3 C4 S1 118.0(3) . . ? C5 C4 S1 121.0(3) . . ? C6 C5 C4 119.1(3) . . ? C6 C5 H5A 120.5 . . ? C4 C5 H5A 120.5 . . ? C5 C6 C1 119.7(3) . . ? C5 C6 H6A 120.2 . . ? C1 C6 H6A 120.2 . . ? O1 C7 O2 123.6(4) . . ? O1 C7 C1 118.1(4) . . ? O2 C7 C1 118.3(4) . . ? O1 C7 Cd1 57.4(2) . . ? O2 C7 Cd1 66.4(2) . . ? C1 C7 Cd1 173.4(3) . . ? C13 C8 C9 121.5(3) . . ? C13 C8 S1 118.5(3) . . ? C9 C8 S1 120.0(3) . . ? C8 C9 C10 118.5(3) . . ? C8 C9 H9A 120.8 . . ? C10 C9 H9A 120.8 . . ? C9 C10 C11 120.7(3) . . ? C9 C10 H10A 119.6 . . ? C11 C10 H10A 119.6 . . ? C12 C11 C10 119.6(3) . . ? C12 C11 C14 119.6(3) . . ? C10 C11 C14 120.8(3) . . ? C11 C12 C13 120.3(3) . . ? C11 C12 H12A 119.9 . . ? C13 C12 H12A 119.9 . . ? C8 C13 C12 119.4(3) . . ? C8 C13 H13A 120.3 . . ? C12 C13 H13A 120.3 . . ? O4 C14 O3 123.1(4) . . ? O4 C14 C11 119.9(4) . . ? O3 C14 C11 116.9(3) . . ? N1 C15 N2 112.1(4) . . ? N1 C15 H15A 123.9 . . ? N2 C15 H15A 123.9 . . ? C17 C16 N1 108.1(4) . . ? C17 C16 H16A 125.9 . . ? N1 C16 H16A 125.9 . . ? C16 C17 N2 107.8(4) . . ? C16 C17 H17A 126.1 . . ? N2 C17 H17A 126.1 . . ? N2 C18 C19 114.3(4) . . ? N2 C18 H18A 108.7 . . ? C19 C18 H18A 108.7 . . ? N2 C18 H18B 108.7 . . ? C19 C18 H18B 108.7 . . ? H18A C18 H18B 107.6 . . ? C18 C19 C20 116.1(4) . . ? C18 C19 H19A 108.3 . . ? C20 C19 H19A 108.3 . . ? C18 C19 H19B 108.3 . . ? C20 C19 H19B 108.3 . . ? H19A C19 H19B 107.4 . . ? C21 C20 C19 110.5(4) . . ? C21 C20 H20A 109.5 . . ? C19 C20 H20A 109.5 . . ? C21 C20 H20B 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 108.1 . . ? C20 C21 N3 115.3(4) . . ? C20 C21 H21A 108.5 . . ? N3 C21 H21A 108.5 . . ? C20 C21 H21B 108.5 . . ? N3 C21 H21B 108.5 . . ? H21A C21 H21B 107.5 . . ? N3 C22 N4 111.9(4) . . ? N3 C22 H22A 124.0 . . ? N4 C22 H22A 124.0 . . ? C24 C23 N4 108.9(4) . . ? C24 C23 H23A 125.5 . . ? N4 C23 H23A 125.5 . . ? C23 C24 N3 106.9(4) . . ? C23 C24 H24A 126.6 . . ? N3 C24 H24A 126.6 . . ? C15 N1 C16 106.0(3) . . ? C15 N1 Cd1 126.8(3) . . ? C16 N1 Cd1 126.2(3) . . ? C15 N2 C17 105.8(3) . . ? C15 N2 C18 128.9(4) . . ? C17 N2 C18 125.3(4) . . ? C22 N3 C24 106.6(4) . . ? C22 N3 C21 125.9(4) . . ? C24 N3 C21 127.3(4) . . ? C22 N4 C23 105.7(3) . . ? C22 N4 Cd1 125.3(2) . 1_455 ? C23 N4 Cd1 129.0(3) . 1_455 ? C7 O1 Cd1 95.1(3) . . ? C7 O2 Cd1 86.2(2) . . ? C14 O3 Cd1 101.9(2) . 1_656 ? C14 O4 Cd1 82.6(3) . 1_656 ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.837 _refine_diff_density_min -1.169 _refine_diff_density_rms 0.087 #===END # Attachment '- compound 4.CIF' data_compound-4 _database_code_depnum_ccdc_archive 'CCDC 825673' #TrackingRef '- compound 4.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H20 Cd N4 O6 S' _chemical_formula_weight 592.89 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.5434(8) _cell_length_b 16.3088(12) _cell_length_c 12.8836(10) _cell_angle_alpha 90.00 _cell_angle_beta 106.192(4) _cell_angle_gamma 90.00 _cell_volume 2329.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 18003 _cell_measurement_theta_min 1.84 _cell_measurement_theta_max 27.00 _exptl_crystal_description block _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.44 _exptl_crystal_size_min 0.33 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.691 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1192 _exptl_absorpt_coefficient_mu 1.075 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6319 _exptl_absorpt_correction_T_max 0.7179 _exptl_absorpt_process_details 'SADABS(Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18003 _diffrn_reflns_av_R_equivalents 0.0375 _diffrn_reflns_av_sigmaI/netI 0.0381 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 27.00 _reflns_number_total 5018 _reflns_number_gt 4208 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material 'SHELXL-97 (Sheldrick, 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^)+(0.6500P)^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 5018 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1797 _refine_ls_R_factor_gt 0.1723 _refine_ls_wR_factor_ref 0.6109 _refine_ls_wR_factor_gt 0.5961 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _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 Cd1 Cd 0.20201(8) 0.06274(6) 0.22911(8) 0.0352(7) Uani 1 1 d . . . S1 S -0.3051(3) 0.3498(2) -0.2652(2) 0.0334(9) Uani 1 1 d . . . C1 C -0.1453(14) 0.1870(9) -0.0365(12) 0.042(3) Uani 1 1 d . . . H1A H -0.1670 0.1555 0.0153 0.050 Uiso 1 1 calc R . . C2 C -0.2327(13) 0.2354(9) -0.1079(11) 0.041(3) Uani 1 1 d . . . H2A H -0.3121 0.2358 -0.1047 0.049 Uiso 1 1 calc R . . C3 C -0.1976(13) 0.2827(8) -0.1836(10) 0.034(3) Uani 1 1 d . . . C4 C -0.0799(15) 0.2830(10) -0.1915(12) 0.042(3) Uani 1 1 d . . . H4A H -0.0580 0.3147 -0.2430 0.051 Uiso 1 1 calc R . . C5 C 0.0040(14) 0.2340(10) -0.1194(11) 0.043(3) Uani 1 1 d . . . H5A H 0.0835 0.2333 -0.1227 0.052 Uiso 1 1 calc R . . C6 C -0.0281(14) 0.1857(8) -0.0421(12) 0.038(3) Uani 1 1 d . . . C7 C -0.4089(13) 0.2849(8) -0.3561(10) 0.033(3) Uani 1 1 d . . . C8 C -0.3650(15) 0.2169(10) -0.3979(13) 0.044(3) Uani 1 1 d . . . H8A H -0.2838 0.2027 -0.3751 0.053 Uiso 1 1 calc R . . C9 C -0.4492(15) 0.1702(9) -0.4769(12) 0.045(3) Uani 1 1 d . . . H9A H -0.4241 0.1231 -0.5050 0.054 Uiso 1 1 calc R . . C10 C -0.5664(14) 0.1941(8) -0.5118(11) 0.037(3) Uani 1 1 d . . . C11 C -0.6086(13) 0.2648(8) -0.4715(12) 0.041(3) Uani 1 1 d . . . H11A H -0.6881 0.2818 -0.4989 0.049 Uiso 1 1 calc R . . C12 C -0.5295(14) 0.3080(9) -0.3907(12) 0.040(3) Uani 1 1 d . . . H12A H -0.5566 0.3527 -0.3592 0.048 Uiso 1 1 calc R . . C13 C 0.0637(14) 0.1375(9) 0.0402(13) 0.043(3) Uani 1 1 d . . . C14 C -0.6551(13) 0.1441(9) -0.5990(12) 0.041(3) Uani 1 1 d . . . C15 C 0.4383(15) -0.0409(10) 0.2513(15) 0.046(3) Uani 1 1 d . . . H15A H 0.4555 -0.0374 0.3261 0.055 Uiso 1 1 calc R . . C16 C 0.453(2) -0.0709(11) 0.0925(17) 0.052(5) Uani 1 1 d . . . H16A H 0.4805 -0.0914 0.0364 0.063 Uiso 1 1 calc R . . C17 C 0.3545(16) -0.0241(10) 0.0822(14) 0.049(4) Uani 1 1 d . . . H17A H 0.3009 -0.0073 0.0176 0.059 Uiso 1 1 calc R . . C18 C 0.6116(16) -0.1333(9) 0.2492(15) 0.050(4) Uani 1 1 d . . . H18A H 0.6095 -0.1825 0.2063 0.060 Uiso 1 1 calc R . . H18B H 0.6094 -0.1501 0.3208 0.060 Uiso 1 1 calc R . . C19 C 0.7257(18) -0.0884(12) 0.2574(19) 0.061(5) Uani 1 1 d . . . H19A H 0.7260 -0.0375 0.2963 0.073 Uiso 1 1 calc R . . H19B H 0.7312 -0.0751 0.1855 0.073 Uiso 1 1 calc R . . C20 C 0.8368(16) -0.1414(11) 0.3175(17) 0.057(4) Uani 1 1 d . . . H20A H 0.8277 -0.1584 0.3869 0.069 Uiso 1 1 calc R . . H20B H 0.8398 -0.1903 0.2755 0.069 Uiso 1 1 calc R . . C21 C 0.9850(17) -0.0478(10) 0.2635(16) 0.049(4) Uani 1 1 d . . . H21A H 0.9381 -0.0360 0.1938 0.059 Uiso 1 1 calc R . . C22 C 1.134(2) -0.0532(12) 0.4074(19) 0.061(5) Uani 1 1 d . . . H22A H 1.2093 -0.0453 0.4558 0.073 Uiso 1 1 calc R . . C23 C 1.043(2) -0.1001(12) 0.4258(17) 0.071(6) Uani 1 1 d . . . H23A H 1.0454 -0.1292 0.4884 0.086 Uiso 1 1 calc R . . N1 N 0.3475(11) -0.0055(7) 0.1841(11) 0.039(3) Uani 1 1 d . . . N2 N 0.5039(12) -0.0829(8) 0.1994(11) 0.041(3) Uani 1 1 d . . . N3 N 0.9496(13) -0.0957(9) 0.3342(12) 0.046(3) Uani 1 1 d . . . N4 N 1.0949(12) -0.0199(7) 0.3067(11) 0.042(3) Uani 1 1 d . . . O1 O 0.0354(12) 0.1145(11) 0.1210(11) 0.069(4) Uani 1 1 d . . . O2 O 0.1636(12) 0.1250(11) 0.0261(15) 0.081(4) Uani 1 1 d . . . O3 O -0.6448(15) 0.0674(7) -0.5901(13) 0.057(3) Uani 1 1 d . . . O4 O -0.7286(13) 0.1787(8) -0.6729(11) 0.064(4) Uani 1 1 d . . . O5 O -0.2457(11) 0.3994(6) -0.3269(8) 0.043(2) Uani 1 1 d . . . O6 O -0.3706(12) 0.3897(7) -0.1994(9) 0.051(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0253(9) 0.0435(10) 0.0354(9) 0.0022(3) 0.0063(6) 0.0003(3) S1 0.0384(19) 0.0327(17) 0.0277(16) -0.0009(10) 0.0067(14) 0.0039(11) C1 0.033(7) 0.048(7) 0.040(7) 0.010(6) 0.004(6) -0.011(5) C2 0.036(7) 0.050(7) 0.038(7) 0.007(6) 0.012(6) -0.004(6) C3 0.033(6) 0.040(6) 0.026(6) 0.000(5) 0.002(5) -0.007(5) C4 0.043(8) 0.052(8) 0.038(7) -0.002(6) 0.022(6) 0.003(6) C5 0.037(7) 0.058(8) 0.036(6) 0.000(6) 0.013(6) -0.009(6) C6 0.033(7) 0.043(7) 0.033(6) 0.001(5) 0.003(6) 0.003(5) C7 0.035(7) 0.036(6) 0.027(5) 0.001(5) 0.009(5) 0.008(5) C8 0.035(7) 0.051(8) 0.045(8) -0.003(6) 0.010(6) 0.009(6) C9 0.052(9) 0.047(7) 0.039(7) -0.016(6) 0.018(7) 0.004(7) C10 0.036(7) 0.045(7) 0.030(6) -0.006(5) 0.010(5) -0.005(5) C11 0.032(7) 0.037(6) 0.050(8) 0.008(6) 0.005(6) 0.012(5) C12 0.037(7) 0.038(6) 0.044(7) -0.001(6) 0.010(6) -0.002(5) C13 0.036(8) 0.046(7) 0.043(7) 0.008(6) 0.003(6) -0.002(6) C14 0.033(7) 0.050(7) 0.046(8) -0.008(6) 0.018(6) -0.012(6) C15 0.042(8) 0.046(7) 0.053(9) 0.006(7) 0.017(7) 0.011(7) C16 0.059(12) 0.058(9) 0.044(9) 0.004(7) 0.021(9) 0.001(7) C17 0.052(9) 0.054(8) 0.045(8) 0.000(7) 0.020(7) -0.001(7) C18 0.058(10) 0.042(7) 0.061(10) 0.005(7) 0.034(8) 0.006(7) C19 0.052(10) 0.047(9) 0.078(12) 0.024(9) 0.008(9) -0.004(8) C20 0.047(9) 0.053(9) 0.073(11) 0.018(8) 0.021(8) 0.001(7) C21 0.035(8) 0.058(8) 0.051(9) 0.015(8) 0.006(7) -0.002(7) C22 0.041(10) 0.077(11) 0.058(11) 0.017(9) 0.000(9) -0.003(7) C23 0.071(13) 0.072(12) 0.066(11) 0.039(10) 0.012(10) -0.014(10) N1 0.026(5) 0.040(5) 0.054(7) -0.003(5) 0.016(5) -0.001(4) N2 0.035(6) 0.042(5) 0.052(7) -0.001(5) 0.024(6) -0.001(5) N3 0.039(7) 0.048(7) 0.055(8) 0.013(6) 0.020(6) 0.004(5) N4 0.034(6) 0.048(6) 0.042(6) 0.008(5) 0.006(5) -0.002(5) O1 0.048(7) 0.105(11) 0.048(7) 0.020(7) 0.004(5) 0.027(7) O2 0.040(7) 0.096(10) 0.103(11) 0.043(9) 0.014(7) 0.019(7) O3 0.056(8) 0.051(7) 0.060(8) -0.009(5) 0.008(7) -0.007(5) O4 0.062(8) 0.053(6) 0.059(7) -0.011(5) -0.012(6) -0.001(5) O5 0.049(6) 0.037(5) 0.040(5) 0.001(4) 0.007(4) -0.009(4) O6 0.062(7) 0.047(5) 0.042(5) -0.012(4) 0.009(5) 0.011(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O1 2.204(12) . ? Cd1 N1 2.222(11) . ? Cd1 N4 2.243(13) 1_455 ? Cd1 O4 2.290(12) 1_656 ? Cd1 O3 2.502(15) 1_656 ? Cd1 C14 2.711(15) 1_656 ? S1 O6 1.438(11) . ? S1 O5 1.436(11) . ? S1 C3 1.765(14) . ? S1 C7 1.772(14) . ? C1 C6 1.38(2) . ? C1 C2 1.40(2) . ? C1 H1A 0.9300 . ? C2 C3 1.389(19) . ? C2 H2A 0.9300 . ? C3 C4 1.39(2) . ? C4 C5 1.39(2) . ? C4 H4A 0.9300 . ? C5 C6 1.40(2) . ? C5 H5A 0.9300 . ? C6 C13 1.497(19) . ? C7 C12 1.39(2) . ? C7 C8 1.389(19) . ? C8 C9 1.42(2) . ? C8 H8A 0.9300 . ? C9 C10 1.36(2) . ? C9 H9A 0.9300 . ? C10 C11 1.405(19) . ? C10 C14 1.528(19) . ? C11 C12 1.37(2) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? C13 O2 1.23(2) . ? C13 O1 1.23(2) . ? C14 O4 1.22(2) . ? C14 O3 1.259(19) . ? C14 Cd1 2.711(15) 1_454 ? C15 N2 1.33(2) . ? C15 N1 1.29(2) . ? C15 H15A 0.9300 . ? C16 N2 1.35(3) . ? C16 C17 1.34(3) . ? C16 H16A 0.9300 . ? C17 N1 1.37(2) . ? C17 H17A 0.9300 . ? C18 N2 1.48(2) . ? C18 C19 1.49(2) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.56(3) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 N3 1.46(2) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 N4 1.32(2) . ? C21 N3 1.35(2) . ? C21 H21A 0.9300 . ? C22 N4 1.36(2) . ? C22 C23 1.37(3) . ? C22 H22A 0.9300 . ? C23 N3 1.36(3) . ? C23 H23A 0.9300 . ? N4 Cd1 2.243(13) 1_655 ? O3 Cd1 2.502(15) 1_454 ? O4 Cd1 2.290(12) 1_454 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cd1 N1 128.1(5) . . ? O1 Cd1 N4 91.1(5) . 1_455 ? N1 Cd1 N4 111.5(5) . 1_455 ? O1 Cd1 O4 98.1(6) . 1_656 ? N1 Cd1 O4 112.6(5) . 1_656 ? N4 Cd1 O4 113.7(5) 1_455 1_656 ? O1 Cd1 O3 147.4(5) . 1_656 ? N1 Cd1 O3 82.5(5) . 1_656 ? N4 Cd1 O3 86.4(5) 1_455 1_656 ? O4 Cd1 O3 54.1(4) 1_656 1_656 ? O1 Cd1 C14 123.6(6) . 1_656 ? N1 Cd1 C14 97.3(4) . 1_656 ? N4 Cd1 C14 102.4(5) 1_455 1_656 ? O4 Cd1 C14 26.6(5) 1_656 1_656 ? O3 Cd1 C14 27.6(4) 1_656 1_656 ? O6 S1 O5 118.8(7) . . ? O6 S1 C3 109.1(6) . . ? O5 S1 C3 108.3(7) . . ? O6 S1 C7 106.8(7) . . ? O5 S1 C7 108.0(6) . . ? C3 S1 C7 104.9(7) . . ? C6 C1 C2 120.8(14) . . ? C6 C1 H1A 119.6 . . ? C2 C1 H1A 119.6 . . ? C3 C2 C1 118.4(14) . . ? C3 C2 H2A 120.8 . . ? C1 C2 H2A 120.8 . . ? C2 C3 C4 122.3(14) . . ? C2 C3 S1 117.9(11) . . ? C4 C3 S1 119.6(11) . . ? C5 C4 C3 117.5(14) . . ? C5 C4 H4A 121.3 . . ? C3 C4 H4A 121.3 . . ? C4 C5 C6 121.7(14) . . ? C4 C5 H5A 119.2 . . ? C6 C5 H5A 119.2 . . ? C1 C6 C5 119.3(13) . . ? C1 C6 C13 118.9(14) . . ? C5 C6 C13 121.6(14) . . ? C12 C7 C8 122.2(13) . . ? C12 C7 S1 118.8(10) . . ? C8 C7 S1 118.7(11) . . ? C7 C8 C9 117.2(14) . . ? C7 C8 H8A 121.4 . . ? C9 C8 H8A 121.4 . . ? C10 C9 C8 120.2(13) . . ? C10 C9 H9A 119.9 . . ? C8 C9 H9A 119.9 . . ? C9 C10 C11 121.9(13) . . ? C9 C10 C14 119.5(13) . . ? C11 C10 C14 118.6(13) . . ? C12 C11 C10 118.4(13) . . ? C12 C11 H11A 120.8 . . ? C10 C11 H11A 120.8 . . ? C11 C12 C7 119.9(13) . . ? C11 C12 H12A 120.0 . . ? C7 C12 H12A 120.0 . . ? O2 C13 O1 123.5(16) . . ? O2 C13 C6 119.3(15) . . ? O1 C13 C6 117.1(14) . . ? O4 C14 O3 123.9(15) . . ? O4 C14 C10 120.3(14) . . ? O3 C14 C10 115.9(15) . . ? O4 C14 Cd1 57.1(8) . 1_454 ? O3 C14 Cd1 67.0(9) . 1_454 ? C10 C14 Cd1 172.9(10) . 1_454 ? N2 C15 N1 111.2(16) . . ? N2 C15 H15A 124.4 . . ? N1 C15 H15A 124.4 . . ? N2 C16 C17 107.4(17) . . ? N2 C16 H16A 126.3 . . ? C17 C16 H16A 126.3 . . ? N1 C17 C16 107.7(16) . . ? N1 C17 H17A 126.1 . . ? C16 C17 H17A 126.1 . . ? N2 C18 C19 112.2(13) . . ? N2 C18 H18A 109.2 . . ? C19 C18 H18A 109.2 . . ? N2 C18 H18B 109.2 . . ? C19 C18 H18B 109.2 . . ? H18A C18 H18B 107.9 . . ? C18 C19 C20 110.6(14) . . ? C18 C19 H19A 109.5 . . ? C20 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? C20 C19 H19B 109.5 . . ? H19A C19 H19B 108.1 . . ? N3 C20 C19 111.5(14) . . ? N3 C20 H20A 109.3 . . ? C19 C20 H20A 109.3 . . ? N3 C20 H20B 109.3 . . ? C19 C20 H20B 109.3 . . ? H20A C20 H20B 108.0 . . ? N4 C21 N3 110.7(16) . . ? N4 C21 H21A 124.6 . . ? N3 C21 H21A 124.6 . . ? N4 C22 C23 109.0(18) . . ? N4 C22 H22A 125.5 . . ? C23 C22 H22A 125.5 . . ? N3 C23 C22 106.3(16) . . ? N3 C23 H23A 126.8 . . ? C22 C23 H23A 126.8 . . ? C15 N1 C17 106.8(13) . . ? C15 N1 Cd1 125.4(12) . . ? C17 N1 Cd1 127.7(11) . . ? C15 N2 C16 106.8(15) . . ? C15 N2 C18 126.5(14) . . ? C16 N2 C18 126.7(14) . . ? C23 N3 C21 107.3(15) . . ? C23 N3 C20 124.1(14) . . ? C21 N3 C20 128.4(16) . . ? C21 N4 C22 106.6(15) . . ? C21 N4 Cd1 127.3(11) . 1_655 ? C22 N4 Cd1 126.1(12) . 1_655 ? C13 O1 Cd1 105.1(11) . . ? C14 O3 Cd1 85.5(10) . 1_454 ? C14 O4 Cd1 96.2(10) . 1_454 ? 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 C6 C1 C2 C3 -1(2) . . . . ? C1 C2 C3 C4 1(2) . . . . ? C1 C2 C3 S1 -174.7(11) . . . . ? O6 S1 C3 C2 42.1(13) . . . . ? O5 S1 C3 C2 172.8(11) . . . . ? C7 S1 C3 C2 -72.0(12) . . . . ? O6 S1 C3 C4 -133.4(12) . . . . ? O5 S1 C3 C4 -2.7(13) . . . . ? C7 S1 C3 C4 112.4(12) . . . . ? C2 C3 C4 C5 -1(2) . . . . ? S1 C3 C4 C5 174.8(11) . . . . ? C3 C4 C5 C6 0(2) . . . . ? C2 C1 C6 C5 1(2) . . . . ? C2 C1 C6 C13 176.1(13) . . . . ? C4 C5 C6 C1 -1(2) . . . . ? C4 C5 C6 C13 -175.8(14) . . . . ? O6 S1 C7 C12 31.3(13) . . . . ? O5 S1 C7 C12 -97.6(12) . . . . ? C3 S1 C7 C12 147.0(12) . . . . ? O6 S1 C7 C8 -154.7(12) . . . . ? O5 S1 C7 C8 76.4(13) . . . . ? C3 S1 C7 C8 -38.9(12) . . . . ? C12 C7 C8 C9 -1(2) . . . . ? S1 C7 C8 C9 -175.0(12) . . . . ? C7 C8 C9 C10 2(2) . . . . ? C8 C9 C10 C11 0(2) . . . . ? C8 C9 C10 C14 178.5(14) . . . . ? C9 C10 C11 C12 -3(2) . . . . ? C14 C10 C11 C12 177.9(13) . . . . ? C10 C11 C12 C7 5(2) . . . . ? C8 C7 C12 C11 -2(2) . . . . ? S1 C7 C12 C11 171.5(11) . . . . ? C1 C6 C13 O2 168.4(17) . . . . ? C5 C6 C13 O2 -16(2) . . . . ? C1 C6 C13 O1 -14(2) . . . . ? C5 C6 C13 O1 161.5(16) . . . . ? C9 C10 C14 O4 -137.3(17) . . . . ? C11 C10 C14 O4 41(2) . . . . ? C9 C10 C14 O3 41(2) . . . . ? C11 C10 C14 O3 -140.1(15) . . . . ? C9 C10 C14 Cd1 -71(10) . . . 1_454 ? C11 C10 C14 Cd1 108(9) . . . 1_454 ? N2 C16 C17 N1 2(2) . . . . ? N2 C18 C19 C20 176.0(16) . . . . ? C18 C19 C20 N3 -175.4(17) . . . . ? N4 C22 C23 N3 1(3) . . . . ? N2 C15 N1 C17 -1.0(18) . . . . ? N2 C15 N1 Cd1 174.4(9) . . . . ? C16 C17 N1 C15 -0.4(18) . . . . ? C16 C17 N1 Cd1 -175.6(11) . . . . ? O1 Cd1 N1 C15 -173.5(13) . . . . ? N4 Cd1 N1 C15 -63.9(14) 1_455 . . . ? O4 Cd1 N1 C15 65.2(13) 1_656 . . . ? O3 Cd1 N1 C15 19.2(13) 1_656 . . . ? C14 Cd1 N1 C15 42.5(13) 1_656 . . . ? O1 Cd1 N1 C17 0.9(15) . . . . ? N4 Cd1 N1 C17 110.4(12) 1_455 . . . ? O4 Cd1 N1 C17 -120.5(12) 1_656 . . . ? O3 Cd1 N1 C17 -166.5(12) 1_656 . . . ? C14 Cd1 N1 C17 -143.1(12) 1_656 . . . ? N1 C15 N2 C16 2.0(19) . . . . ? N1 C15 N2 C18 -177.7(13) . . . . ? C17 C16 N2 C15 -2(2) . . . . ? C17 C16 N2 C18 177.5(14) . . . . ? C19 C18 N2 C15 -98(2) . . . . ? C19 C18 N2 C16 82(2) . . . . ? C22 C23 N3 C21 0(2) . . . . ? C22 C23 N3 C20 176.3(18) . . . . ? N4 C21 N3 C23 -2(2) . . . . ? N4 C21 N3 C20 -177.2(16) . . . . ? C19 C20 N3 C23 141(2) . . . . ? C19 C20 N3 C21 -44(3) . . . . ? N3 C21 N4 C22 2(2) . . . . ? N3 C21 N4 Cd1 -179.9(11) . . . 1_655 ? C23 C22 N4 C21 -2(2) . . . . ? C23 C22 N4 Cd1 -179.8(14) . . . 1_655 ? O2 C13 O1 Cd1 6(2) . . . . ? C6 C13 O1 Cd1 -172.2(10) . . . . ? N1 Cd1 O1 C13 -34.6(16) . . . . ? N4 Cd1 O1 C13 -153.3(13) 1_455 . . . ? O4 Cd1 O1 C13 92.6(13) 1_656 . . . ? O3 Cd1 O1 C13 121.6(12) 1_656 . . . ? C14 Cd1 O1 C13 101.0(13) 1_656 . . . ? O4 C14 O3 Cd1 5.6(17) . . . 1_454 ? C10 C14 O3 Cd1 -172.9(11) . . . 1_454 ? O3 C14 O4 Cd1 -6.1(19) . . . 1_454 ? C10 C14 O4 Cd1 172.3(11) . . . 1_454 ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 5.743 _refine_diff_density_min -3.074 _refine_diff_density_rms 0.367