Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Prof Martin Schroder' _publ_contact_author_address ; School of Chemistry University of Nottingham University Park Nottingham NG7 2RD UNITED KINGDOM ; _publ_contact_author_email M.SCHRODER@NOTTINGHAM.AC.UK _publ_section_title ; Conformational and Stereochemical Flexibility in Cadmium(II) Complexes of Aza-thioether Macrocycles ; loop_ _publ_author_name 'Martin Schroder' 'Alexander J. Blake' 'Willem L. Driessen' 'Mark W. Glenny' 'Jan Reedijk' ; L.G.A.v.d.Water ; #===END of CIF data_CDN2S2_complex_1 _database_code_depnum_ccdc_archive 'CCDC 225828' _refine_special_details ; Disorder in an ethylene unit of one of the independent molecules in the asymmetric unit was modelled by isotropic refinement for two components with a ratio of 59:41. Final residual electron density had a maximum of 1.51e/A**3 located 0.74 Angstroms from CdA. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[C8 H18 Cd N4 O6 S2]2 0.5 C H2 Cl2' _chemical_formula_sum 'C8.25 H18 Cd Cl0.50 N4 O6 S2' _chemical_formula_weight 463.51 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' Cl Cl 0.1484 0.1585 '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 9.2900(6) _cell_length_b 12.9338(8) _cell_length_c 13.6222(8) _cell_angle_alpha 87.766(1) _cell_angle_beta 84.806(1) _cell_angle_gamma 82.483(1) _cell_volume 1615.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6450 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 28.25 _exptl_crystal_description Tablet _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.906 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 928 _exptl_absorpt_coefficient_mu 1.724 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.504 _exptl_absorpt_correction_T_max 0.634 _exptl_absorpt_process_details SADABS _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART1000 CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15687 _diffrn_reflns_av_R_equivalents 0.014 _diffrn_reflns_av_sigmaI/netI 0.009 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 28.39 _reflns_number_total 7110 _reflns_number_gt 6655 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL; PLATON (Spek, 2003)' _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^)+(0.036P)^2^+2.599P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'direct methods' _atom_sites_solution_secondary 'difference Fourier' _atom_sites_solution_hydrogens 'geometrically placed' _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7104 _refine_ls_number_parameters 395 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0295 _refine_ls_R_factor_gt 0.0275 _refine_ls_wR_factor_ref 0.0718 _refine_ls_wR_factor_gt 0.0699 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.047 _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 Cd Cd 0.203915(18) 0.322196(13) 0.505209(13) 0.02379(6) Uani 1 1 d . . . S1 S 0.07334(7) 0.14279(5) 0.49062(5) 0.03080(14) Uani 1 1 d . . . O1 O 0.0158(2) 0.38267(16) 0.38575(15) 0.0349(4) Uani 1 1 d . . . C1 C 0.1886(3) 0.4141(2) 0.7152(2) 0.0321(5) Uani 1 1 d . . . H1A H 0.1594 0.4865 0.6916 0.038 Uiso 1 1 calc R . . H1B H 0.2230 0.4171 0.7816 0.038 Uiso 1 1 calc R . . N1 N 0.3086(2) 0.36443(16) 0.64757(16) 0.0263(4) Uani 1 1 d . . . H1C H 0.3704 0.4142 0.6290 0.032 Uiso 1 1 calc R . . S2 S 0.43117(7) 0.17010(5) 0.51410(5) 0.02955(13) Uani 1 1 d . . . O2 O 0.2291(2) 0.31089(16) 0.32903(15) 0.0354(4) Uani 1 1 d . . . N2 N 0.0032(2) 0.34706(18) 0.62432(17) 0.0289(4) Uani 1 1 d . . . H2C H -0.0487 0.4115 0.6099 0.035 Uiso 1 1 calc R . . C2 C 0.0576(3) 0.3547(2) 0.7221(2) 0.0325(6) Uani 1 1 d . . . H2A H 0.0850 0.2837 0.7498 0.039 Uiso 1 1 calc R . . H2B H -0.0210 0.3906 0.7673 0.039 Uiso 1 1 calc R . . N3 N 0.1037(3) 0.35717(18) 0.31283(17) 0.0310(5) Uani 1 1 d . . . O3 O 0.0702(3) 0.3765(2) 0.22828(16) 0.0529(6) Uani 1 1 d . . . C3 C -0.0986(3) 0.2685(2) 0.6222(2) 0.0342(6) Uani 1 1 d . . . H3A H -0.1585 0.2851 0.5658 0.041 Uiso 1 1 calc R . . H3B H -0.1651 0.2728 0.6833 0.041 Uiso 1 1 calc R . . N4 N 0.3653(2) 0.48921(17) 0.40935(17) 0.0297(5) Uani 1 1 d . . . O4 O 0.2369(2) 0.49485(15) 0.45183(15) 0.0325(4) Uani 1 1 d . . . C4 C -0.0215(3) 0.1577(2) 0.6131(2) 0.0335(6) Uani 1 1 d . . . H4A H -0.0935 0.1074 0.6238 0.040 Uiso 1 1 calc R . . H4B H 0.0491 0.1433 0.6637 0.040 Uiso 1 1 calc R . . O5 O 0.4570(2) 0.41456(18) 0.43172(17) 0.0425(5) Uani 1 1 d . . . C5 C 0.2207(3) 0.0395(2) 0.5092(2) 0.0322(6) Uani 1 1 d . . . H5A H 0.1786 -0.0217 0.5399 0.039 Uiso 1 1 calc R . . H5B H 0.2691 0.0186 0.4439 0.039 Uiso 1 1 calc R . . C6 C 0.3359(3) 0.0669(2) 0.5729(2) 0.0295(5) Uani 1 1 d . . . H6A H 0.4066 0.0042 0.5838 0.035 Uiso 1 1 calc R . . H6B H 0.2889 0.0899 0.6379 0.035 Uiso 1 1 calc R . . O6 O 0.3965(2) 0.55631(17) 0.34736(17) 0.0438(5) Uani 1 1 d . . . C7 C 0.5078(3) 0.2193(2) 0.6178(2) 0.0328(6) Uani 1 1 d . . . H7A H 0.5638 0.1601 0.6517 0.039 Uiso 1 1 calc R . . H7B H 0.5770 0.2681 0.5927 0.039 Uiso 1 1 calc R . . C8 C 0.3958(3) 0.2750(2) 0.6927(2) 0.0296(5) Uani 1 1 d . . . H8A H 0.3302 0.2253 0.7218 0.035 Uiso 1 1 calc R . . H8B H 0.4463 0.2996 0.7465 0.035 Uiso 1 1 calc R . . CdA Cd 0.59987(2) 0.114186(15) 0.137139(15) 0.03118(6) Uani 1 1 d . A . S1A S 0.78395(10) 0.14178(7) 0.27344(7) 0.0477(2) Uani 1 1 d . . . N1A N 0.5480(3) 0.2165(2) -0.00791(19) 0.0394(6) Uani 1 1 d . . . H1AC H 0.4640 0.1958 -0.0289 0.047 Uiso 1 1 calc R A . C1A C 0.5119(4) 0.3274(3) 0.0164(2) 0.0450(7) Uani 1 1 d . A . H1AA H 0.4516 0.3638 -0.0338 0.054 Uiso 1 1 calc R . . H1AB H 0.6028 0.3599 0.0149 0.054 Uiso 1 1 calc R . . O1A O 0.3464(2) 0.07871(18) 0.14116(16) 0.0410(5) Uani 1 1 d . . . N2A N 0.5120(3) 0.28407(19) 0.19537(19) 0.0354(5) Uani 1 1 d . . . H2AC H 0.4480 0.2772 0.2511 0.043 Uiso 1 1 calc R A . S2A S 0.85595(10) 0.09667(9) 0.02497(8) 0.0628(3) Uani 1 1 d . . . C2A C 0.4295(3) 0.3403(3) 0.1178(3) 0.0457(7) Uani 1 1 d . A . H2AA H 0.4103 0.4154 0.1328 0.055 Uiso 1 1 calc R . . H2AB H 0.3344 0.3136 0.1174 0.055 Uiso 1 1 calc R . . O2A O 0.4463(2) 0.04940(19) 0.27788(16) 0.0430(5) Uani 1 1 d . . . C3A C 0.6330(3) 0.3369(2) 0.2232(2) 0.0398(7) Uani 1 1 d . A . H3AA H 0.5940 0.4069 0.2477 0.048 Uiso 1 1 calc R . . H3AB H 0.7012 0.3460 0.1643 0.048 Uiso 1 1 calc R . . N3A N 0.3414(3) 0.0416(2) 0.22784(18) 0.0334(5) Uani 1 1 d . A . O3A O 0.2384(3) -0.0034(2) 0.26266(18) 0.0530(6) Uani 1 1 d . . . N4A N 0.7370(3) -0.12272(19) 0.11976(17) 0.0322(5) Uani 1 1 d . A . O4A O 0.6203(2) -0.06489(18) 0.10319(19) 0.0456(5) Uani 1 1 d . . . C4A C 0.7149(4) 0.2752(3) 0.3023(2) 0.0420(7) Uani 1 1 d . A . H4AA H 0.6492 0.2751 0.3637 0.050 Uiso 1 1 calc R . . H4AB H 0.7979 0.3119 0.3156 0.050 Uiso 1 1 calc R . . O5A O 0.8212(3) -0.09171(18) 0.17483(18) 0.0484(6) Uani 1 1 d . . . C5A C 0.9546(6) 0.1350(5) 0.2157(4) 0.0421(11) Uiso 0.59 1 d P A 1 H5AA H 1.0140 0.1738 0.2544 0.051 Uiso 0.59 1 calc PR A 1 H5AB H 0.9989 0.0611 0.2157 0.051 Uiso 0.59 1 calc PR A 1 C5A' C 0.9442(8) 0.1835(6) 0.1721(6) 0.0336(14) Uiso 0.41 1 d P A 2 H5AC H 0.9093 0.2515 0.1410 0.040 Uiso 0.41 1 calc PR A 2 H5AD H 1.0305 0.1928 0.2069 0.040 Uiso 0.41 1 calc PR A 2 C6A C 0.9629(6) 0.1776(4) 0.1107(4) 0.0397(11) Uiso 0.59 1 d P A 1 H6AA H 1.0662 0.1738 0.0843 0.048 Uiso 0.59 1 calc PR A 1 H6AB H 0.9199 0.2518 0.1096 0.048 Uiso 0.59 1 calc PR A 1 C6A' C 0.9894(7) 0.1054(6) 0.0928(5) 0.0333(14) Uiso 0.41 1 d P A 2 H6AC H 1.0202 0.0363 0.1233 0.040 Uiso 0.41 1 calc PR A 2 H6AD H 1.0737 0.1267 0.0507 0.040 Uiso 0.41 1 calc PR A 2 O6A O 0.7617(2) -0.20939(17) 0.08231(17) 0.0420(5) Uani 1 1 d . . . C7A C 0.8144(4) 0.2017(3) -0.0605(2) 0.0439(7) Uani 1 1 d . A . H7AA H 0.8209 0.2689 -0.0298 0.053 Uiso 1 1 calc R . . H7AB H 0.8854 0.1947 -0.1193 0.053 Uiso 1 1 calc R . . C8A C 0.6608(4) 0.2001(3) -0.0909(2) 0.0472(8) Uani 1 1 d . A . H8AA H 0.6410 0.2551 -0.1422 0.057 Uiso 1 1 calc R . . H8AB H 0.6552 0.1320 -0.1202 0.057 Uiso 1 1 calc R . . Cl1S Cl 0.15302(14) 0.51600(9) -0.00658(11) 0.0818(4) Uani 1 1 d D . . C1S C 0.0299(4) 0.4260(6) 0.0024(6) 0.0571(18) Uani 0.50 1 d PD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd 0.02213(9) 0.02496(10) 0.02475(9) 0.00458(7) -0.00368(6) -0.00521(6) S1 0.0298(3) 0.0336(3) 0.0319(3) 0.0055(3) -0.0092(2) -0.0124(3) O1 0.0293(9) 0.0424(11) 0.0317(10) 0.0041(8) -0.0030(8) -0.0008(8) C1 0.0344(14) 0.0297(13) 0.0319(13) -0.0036(10) -0.0026(11) -0.0025(11) N1 0.0249(10) 0.0233(10) 0.0315(11) 0.0020(8) -0.0047(8) -0.0054(8) S2 0.0242(3) 0.0264(3) 0.0379(3) -0.0017(3) -0.0008(2) -0.0039(2) O2 0.0305(10) 0.0406(11) 0.0335(10) 0.0023(8) -0.0008(8) -0.0012(8) N2 0.0227(10) 0.0305(11) 0.0325(11) 0.0069(9) -0.0040(8) -0.0003(8) C2 0.0303(13) 0.0363(14) 0.0296(13) 0.0014(11) 0.0001(10) -0.0018(11) N3 0.0325(11) 0.0339(12) 0.0282(11) 0.0029(9) -0.0067(9) -0.0079(9) O3 0.0576(15) 0.0743(17) 0.0264(11) 0.0038(11) -0.0137(10) -0.0008(13) C3 0.0208(12) 0.0420(15) 0.0398(15) 0.0063(12) -0.0028(10) -0.0068(11) N4 0.0294(11) 0.0260(11) 0.0352(12) -0.0001(9) -0.0035(9) -0.0093(9) O4 0.0274(9) 0.0294(9) 0.0397(11) 0.0057(8) -0.0003(8) -0.0035(7) C4 0.0295(13) 0.0373(14) 0.0356(14) 0.0074(11) -0.0023(11) -0.0146(11) O5 0.0346(11) 0.0436(12) 0.0461(12) 0.0047(10) -0.0007(9) 0.0037(9) C5 0.0376(14) 0.0255(12) 0.0355(14) -0.0012(10) -0.0063(11) -0.0091(11) C6 0.0297(12) 0.0224(12) 0.0370(14) 0.0024(10) -0.0061(11) -0.0040(10) O6 0.0474(12) 0.0365(11) 0.0488(13) 0.0106(9) 0.0021(10) -0.0178(9) C7 0.0221(12) 0.0303(13) 0.0477(16) -0.0002(12) -0.0120(11) -0.0033(10) C8 0.0299(12) 0.0279(12) 0.0326(13) 0.0044(10) -0.0119(10) -0.0053(10) CdA 0.02845(10) 0.03103(11) 0.03545(11) 0.00380(8) -0.00284(8) -0.01030(8) S1A 0.0463(4) 0.0400(4) 0.0607(5) 0.0064(4) -0.0250(4) -0.0083(3) N1A 0.0344(12) 0.0476(15) 0.0389(13) -0.0004(11) -0.0095(10) -0.0115(11) C1A 0.0445(17) 0.0466(18) 0.0419(17) 0.0095(14) -0.0048(13) -0.0013(14) O1A 0.0352(11) 0.0554(13) 0.0346(11) 0.0129(9) -0.0089(8) -0.0142(9) N2A 0.0290(11) 0.0387(13) 0.0366(13) 0.0014(10) 0.0040(9) -0.0020(10) S2A 0.0340(4) 0.0825(7) 0.0629(6) 0.0369(5) 0.0085(4) 0.0063(4) C2A 0.0351(15) 0.0461(18) 0.0511(19) 0.0083(14) 0.0010(13) 0.0064(13) O2A 0.0371(11) 0.0590(14) 0.0367(11) 0.0101(10) -0.0124(9) -0.0175(10) C3A 0.0412(16) 0.0321(14) 0.0448(17) -0.0065(12) 0.0048(13) -0.0039(12) N3A 0.0284(11) 0.0405(13) 0.0324(12) 0.0028(10) -0.0026(9) -0.0094(10) O3A 0.0402(12) 0.0798(18) 0.0436(13) 0.0064(12) 0.0034(10) -0.0322(12) N4A 0.0340(12) 0.0365(12) 0.0274(11) 0.0067(9) -0.0019(9) -0.0122(10) O4A 0.0311(10) 0.0416(12) 0.0655(15) -0.0105(11) -0.0088(10) -0.0044(9) C4A 0.0405(16) 0.0504(18) 0.0360(15) -0.0114(13) 0.0010(12) -0.0089(13) O5A 0.0574(14) 0.0461(13) 0.0484(13) 0.0143(10) -0.0259(11) -0.0220(11) O6A 0.0466(12) 0.0361(11) 0.0422(12) 0.0004(9) -0.0027(9) -0.0024(9) C7A 0.0431(17) 0.0482(18) 0.0390(16) 0.0050(13) 0.0059(13) -0.0094(14) C8A 0.0523(19) 0.059(2) 0.0313(15) -0.0032(14) -0.0063(13) -0.0069(16) Cl1S 0.0780(7) 0.0586(6) 0.1125(10) 0.0095(6) -0.0275(7) -0.0122(5) C1S 0.065(5) 0.052(4) 0.058(4) 0.003(3) -0.006(4) -0.023(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd N1 2.360(2) . y Cd N2 2.356(2) . y Cd O1 2.524(2) . y Cd O2 2.398(2) . y Cd O4 2.3710(19) . y Cd S1 2.7769(10) . y Cd S2 2.6986(11) . y N1 C1 1.476(3) . ? N1 C8 1.470(3) . ? N2 C2 1.478(4) . ? N2 C3 1.479(3) . ? O1 N3 1.253(3) . ? O2 N3 1.272(3) . ? O3 N3 1.228(3) . ? O4 N4 1.272(3) . ? O5 N4 1.249(3) . ? O6 N4 1.231(3) . ? S1 C4 1.820(3) . ? S1 C5 1.812(3) . ? S2 C6 1.818(3) . ? S2 C7 1.811(3) . ? C1 C2 1.516(4) . ? C3 C4 1.520(4) . ? C5 C6 1.521(4) . ? C7 C8 1.520(4) . ? CdA N1A 2.385(3) . y CdA N2A 2.382(3) . y CdA O1A 2.453(2) . y CdA O2A 2.471(2) . y CdA O4A 2.359(2) . y CdA S1A 2.6992(11) . y CdA S2A 2.6969(12) . y N1A C1A 1.472(4) . ? N1A C8A 1.472(4) . ? N2A C2A 1.474(4) . ? N2A C3A 1.474(4) . ? O1A N3A 1.256(3) . ? O2A N3A 1.255(3) . ? O3A N3A 1.233(3) . ? O4A N4A 1.267(3) . ? O5A N4A 1.244(3) . ? O6A N4A 1.235(3) . ? S1A C4A 1.806(3) . ? S1A C5A 1.698(6) . ? S1A C5A' 2.047(7) . ? S2A C6A 2.006(6) . ? S2A C6A' 1.630(7) . ? S2A C7A 1.781(3) . ? C1A C2A 1.521(5) . ? C3A C4A 1.515(5) . ? C5A C6A 1.511(8) . ? C5A' C6A' 1.502(10) . ? C7A C8A 1.524(5) . ? Cl1S C1S 1.729(5) . ? Cl1S C1S 1.762(5) 2_565 ? C1S Cl1S 1.762(5) 2_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cd N2 76.57(8) . . y N1 Cd O1 145.00(7) . . y N1 Cd O2 146.89(7) . . y N1 Cd O4 84.29(8) . . y N1 Cd S1 123.58(6) . . y N1 Cd S2 77.77(6) . . y N1 C1 C2 111.6(2) . . ? N1 C8 C7 111.8(2) . . ? N2 Cd O1 83.70(7) . . y N2 Cd O2 134.11(7) . . y N2 Cd O4 103.09(8) . . y N2 Cd S1 77.51(6) . . y N2 Cd S2 124.90(6) . . y N2 C2 C1 111.3(2) . . ? N2 C3 C4 113.1(2) . . ? N3 O1 Cd 92.13(15) . . ? N3 O2 Cd 97.60(15) . . ? N4 O4 Cd 105.89(15) . . ? O1 Cd O2 52.09(7) . . y O1 Cd S1 78.59(6) . . y O1 Cd S2 136.74(5) . . y O2 Cd S1 81.70(6) . . y O2 Cd S2 88.95(6) . . y O4 Cd O1 72.29(7) . . y O4 Cd O2 77.14(8) . . y O4 Cd S1 150.56(5) . . y O4 Cd S2 121.73(5) . . y S1 Cd S2 77.64(3) . . y O1 N3 O2 118.0(2) . . ? O1 N3 O3 121.2(2) . . ? O3 N3 O2 120.9(2) . . ? O4 N4 O5 118.6(2) . . ? O4 N4 O6 119.9(2) . . ? O5 N4 O6 121.5(2) . . ? C1 N1 Cd 106.85(15) . . ? C1 N1 C8 113.5(2) . . ? C2 N2 C3 113.3(2) . . ? C2 N2 Cd 108.77(15) . . ? C3 N2 Cd 113.66(17) . . ? C3 C4 S1 109.12(19) . . ? C4 S1 Cd 92.35(9) . . ? C5 S1 C4 103.19(14) . . ? C5 S1 Cd 102.88(9) . . ? C5 C6 S2 110.73(19) . . ? C6 C5 S1 115.28(19) . . ? C6 S2 Cd 99.25(9) . . ? C7 S2 Cd 96.91(9) . . ? C7 S2 C6 101.58(13) . . ? C8 N1 Cd 113.44(16) . . ? C8 C7 S2 114.36(18) . . ? N1A CdA N2A 75.34(9) . . y N1A CdA O1A 85.13(8) . . y N1A CdA O2A 133.67(8) . . y N1A CdA O4A 109.99(9) . . y N1A CdA S1A 129.15(7) . . y N1A CdA S2A 75.79(7) . . y N1A C1A C2A 111.4(3) . . ? N1A C8A C7A 113.0(3) . . ? N2A CdA O1A 88.55(9) . . y N2A CdA O2A 85.93(9) . . y N2A CdA O4A 162.93(8) . . y N2A CdA S1A 76.79(7) . . y N2A CdA S2A 115.83(7) . . y N2A C2A C1A 111.7(2) . . ? N2A C3A C4A 111.6(3) . . ? N3A O2A CdA 94.18(16) . . ? N3A O1A CdA 95.01(15) . . ? N4A O4A CdA 118.74(17) . . ? O1A CdA O2A 51.89(7) . . y O1A CdA O4A 76.04(8) . . y O1A CdA S1A 135.49(6) . . y O1A CdA S2A 143.11(6) . . y O2A CdA O4A 78.83(9) . . y O2A CdA S1A 84.92(5) . . y O2A CdA S2A 148.95(6) . . y O4A CdA S1A 109.10(7) . . y O4A CdA S2A 81.22(7) . . y O1A N3A O2A 118.1(2) . . ? O1A N3A O3A 121.4(2) . . ? O2A N3A O3A 120.5(2) . . ? O4A N4A O5A 119.2(3) . . ? O4A N4A O6A 118.6(2) . . ? O5A N4A O6A 122.1(3) . . ? S1A CdA S2A 79.42(4) . . ? C1A N1A CdA 110.12(19) . . ? C2A N2A CdA 107.3(2) . . ? C2A N2A C3A 113.9(3) . . ? C3A N2A CdA 110.67(17) . . ? C3A C4A S1A 115.5(2) . . ? C4A S1A CdA 98.11(11) . . ? C4A S1A C5A' 93.5(2) . . ? C5A S1A C4A 110.3(2) . . ? C5A S1A CdA 107.8(2) . . ? C5A' S1A CdA 94.4(2) . . ? C5A C6A S2A 111.1(4) . . ? C5A' C6A' S2A 111.0(5) . . ? C6A S2A CdA 97.21(17) . . ? C6A' S2A CdA 110.3(3) . . ? C6A' S2A C7A 116.7(3) . . ? C6A C5A S1A 115.1(4) . . ? C6A' C5A' S1A 113.8(5) . . ? C7A S2A CdA 98.61(11) . . ? C7A S2A C6A 95.3(2) . . ? C8A N1A C1A 112.4(3) . . ? C8A N1A CdA 114.6(2) . . ? C8A C7A S2A 109.3(2) . . ? Cl1S C1S Cl1S 113.2(4) . 2_565 ? 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 N2 Cd S1 C5 -124.79(11) . . . . ? N1 Cd S1 C5 -60.42(12) . . . . ? O4 Cd S1 C5 140.64(14) . . . . ? O2 Cd S1 C5 96.38(11) . . . . ? O1 Cd S1 C5 149.22(11) . . . . ? S2 Cd S1 C5 5.63(10) . . . . ? N2 Cd S1 C4 -20.69(11) . . . . ? N1 Cd S1 C4 43.68(12) . . . . ? O4 Cd S1 C4 -115.26(14) . . . . ? O2 Cd S1 C4 -159.52(11) . . . . ? O1 Cd S1 C4 -106.67(11) . . . . ? S2 Cd S1 C4 109.73(10) . . . . ? N2 Cd O1 N3 -169.54(16) . . . . ? N1 Cd O1 N3 134.87(16) . . . . ? O4 Cd O1 N3 84.53(16) . . . . ? O2 Cd O1 N3 -2.75(14) . . . . ? S2 Cd O1 N3 -33.27(18) . . . . ? S1 Cd O1 N3 -91.05(15) . . . . ? C2 C1 N1 C8 -80.7(3) . . . . y C2 C1 N1 Cd 45.1(2) . . . . ? N2 Cd N1 C8 107.69(18) . . . . ? O4 Cd N1 C8 -147.36(17) . . . . ? O2 Cd N1 C8 -91.6(2) . . . . ? O1 Cd N1 C8 165.16(15) . . . . ? S2 Cd N1 C8 -23.13(16) . . . . ? S1 Cd N1 C8 42.86(19) . . . . ? N2 Cd N1 C1 -18.10(16) . . . . ? O4 Cd N1 C1 86.85(16) . . . . ? O2 Cd N1 C1 142.59(16) . . . . ? O1 Cd N1 C1 39.4(2) . . . . ? S2 Cd N1 C1 -148.91(16) . . . . ? S1 Cd N1 C1 -82.92(16) . . . . ? N2 Cd S2 C7 -68.69(12) . . . . ? N1 Cd S2 C7 -4.85(11) . . . . ? O4 Cd S2 C7 70.44(11) . . . . ? O2 Cd S2 C7 144.59(11) . . . . ? O1 Cd S2 C7 168.21(12) . . . . ? S1 Cd S2 C7 -133.68(10) . . . . ? N2 Cd S2 C6 34.29(12) . . . . ? N1 Cd S2 C6 98.13(11) . . . . ? O4 Cd S2 C6 173.42(11) . . . . ? O2 Cd S2 C6 -112.43(11) . . . . ? O1 Cd S2 C6 -88.81(12) . . . . ? S1 Cd S2 C6 -30.70(9) . . . . ? N2 Cd O2 N3 21.2(2) . . . . ? N1 Cd O2 N3 -132.22(16) . . . . ? O4 Cd O2 N3 -74.70(15) . . . . ? O1 Cd O2 N3 2.73(14) . . . . ? S2 Cd O2 N3 162.36(15) . . . . ? S1 Cd O2 N3 84.70(15) . . . . ? N1 Cd N2 C2 -10.46(16) . . . . ? O4 Cd N2 C2 -91.22(17) . . . . ? O2 Cd N2 C2 -175.89(15) . . . . ? O1 Cd N2 C2 -161.35(18) . . . . ? S2 Cd N2 C2 53.93(19) . . . . ? S1 Cd N2 C2 118.98(17) . . . . ? N1 Cd N2 C3 -137.73(18) . . . . ? O4 Cd N2 C3 141.52(17) . . . . ? O2 Cd N2 C3 56.8(2) . . . . ? O1 Cd N2 C3 71.39(17) . . . . ? S2 Cd N2 C3 -73.33(18) . . . . ? S1 Cd N2 C3 -8.28(16) . . . . ? C3 N2 C2 C1 165.3(2) . . . . y Cd N2 C2 C1 37.9(3) . . . . ? N1 C1 C2 N2 -58.3(3) . . . . y Cd O1 N3 O3 -175.2(2) . . . . ? Cd O1 N3 O2 4.6(2) . . . . ? Cd O2 N3 O3 174.9(2) . . . . ? Cd O2 N3 O1 -4.9(2) . . . . ? C2 N2 C3 C4 -80.2(3) . . . . y Cd N2 C3 C4 44.7(3) . . . . ? O6 N4 O4 Cd 155.9(2) . . . . ? O5 N4 O4 Cd -23.7(3) . . . . ? N2 Cd O4 N4 162.10(16) . . . . ? N1 Cd O4 N4 87.34(17) . . . . ? O2 Cd O4 N4 -65.07(16) . . . . ? O1 Cd O4 N4 -119.00(17) . . . . ? S2 Cd O4 N4 15.54(18) . . . . ? S1 Cd O4 N4 -110.16(16) . . . . ? N2 C3 C4 S1 -69.5(3) . . . . y C5 S1 C4 C3 153.64(19) . . . . y Cd S1 C4 C3 49.83(18) . . . . ? C4 S1 C5 C6 -67.0(2) . . . . y Cd S1 C5 C6 28.5(2) . . . . ? S1 C5 C6 S2 -64.2(2) . . . . y C7 S2 C6 C5 160.13(19) . . . . y Cd S2 C6 C5 61.05(19) . . . . ? C6 S2 C7 C8 -68.2(2) . . . . y Cd S2 C7 C8 32.7(2) . . . . ? C1 N1 C8 C7 174.0(2) . . . . y Cd N1 C8 C7 51.9(2) . . . . ? S2 C7 C8 N1 -58.7(3) . . . . y O4A CdA S1A C5A 77.5(2) . . . . ? N2A CdA S1A C5A -119.2(2) . . . . ? N1A CdA S1A C5A -60.9(2) . . . . ? O1A CdA S1A C5A 166.9(2) . . . . ? O2A CdA S1A C5A 153.9(2) . . . . ? S2A CdA S1A C5A 0.8(2) . . . . ? O4A CdA S1A C4A -168.02(12) . . . . ? N2A CdA S1A C4A -4.72(12) . . . . ? N1A CdA S1A C4A 53.52(14) . . . . ? O1A CdA S1A C4A -78.70(14) . . . . ? O2A CdA S1A C4A -91.71(13) . . . . ? S2A CdA S1A C4A 115.22(12) . . . . ? O4A CdA S1A C5A' 97.8(2) . . . . ? N2A CdA S1A C5A' -98.9(2) . . . . ? N1A CdA S1A C5A' -40.7(2) . . . . ? O1A CdA S1A C5A' -172.9(2) . . . . ? O2A CdA S1A C5A' 174.1(2) . . . . ? S2A CdA S1A C5A' 21.0(2) . . . . ? O4A CdA N1A C8A -61.2(2) . . . . ? N2A CdA N1A C8A 135.8(2) . . . . ? O1A CdA N1A C8A -134.4(2) . . . . ? O2A CdA N1A C8A -154.8(2) . . . . ? S2A CdA N1A C8A 13.7(2) . . . . ? S1A CdA N1A C8A 77.0(2) . . . . ? O4A CdA N1A C1A 170.89(19) . . . . ? N2A CdA N1A C1A 7.89(19) . . . . ? O1A CdA N1A C1A 97.7(2) . . . . ? O2A CdA N1A C1A 77.3(2) . . . . ? S2A CdA N1A C1A -114.2(2) . . . . ? S1A CdA N1A C1A -50.9(2) . . . . ? C8A N1A C1A C2A -163.9(3) . . . . y CdA N1A C1A C2A -34.9(3) . . . . ? O4A CdA O1A N3A 81.57(18) . . . . ? N2A CdA O1A N3A -91.01(18) . . . . ? N1A CdA O1A N3A -166.42(18) . . . . ? O2A CdA O1A N3A -5.05(16) . . . . ? S2A CdA O1A N3A 135.18(15) . . . . ? S1A CdA O1A N3A -21.6(2) . . . . ? O4A CdA N2A C2A -90.4(3) . . . . ? N1A CdA N2A C2A 20.19(18) . . . . ? O1A CdA N2A C2A -65.16(19) . . . . ? O2A CdA N2A C2A -117.05(19) . . . . ? S2A CdA N2A C2A 86.07(19) . . . . ? S1A CdA N2A C2A 157.22(19) . . . . ? O4A CdA N2A C3A 144.8(3) . . . . ? N1A CdA N2A C3A -104.6(2) . . . . ? O1A CdA N2A C3A 170.08(19) . . . . ? O2A CdA N2A C3A 118.19(19) . . . . ? S2A CdA N2A C3A -38.7(2) . . . . ? S1A CdA N2A C3A 32.46(18) . . . . ? O4A CdA S2A C6A' -108.9(3) . . . . ? N2A CdA S2A C6A' 72.2(3) . . . . ? N1A CdA S2A C6A' 137.8(3) . . . . ? O1A CdA S2A C6A' -161.1(3) . . . . ? O2A CdA S2A C6A' -58.4(3) . . . . ? S1A CdA S2A C6A' 2.6(3) . . . . ? O4A CdA S2A C7A 128.39(14) . . . . ? N2A CdA S2A C7A -50.56(15) . . . . ? N1A CdA S2A C7A 15.06(14) . . . . ? O1A CdA S2A C7A 76.17(16) . . . . ? O2A CdA S2A C7A 178.84(15) . . . . ? S1A CdA S2A C7A -120.15(13) . . . . ? O4A CdA S2A C6A -135.11(17) . . . . ? N2A CdA S2A C6A 45.93(18) . . . . ? N1A CdA S2A C6A 111.56(17) . . . . ? O1A CdA S2A C6A 172.66(18) . . . . ? O2A CdA S2A C6A -84.7(2) . . . . ? S1A CdA S2A C6A -23.66(16) . . . . ? C3A N2A C2A C1A 76.4(3) . . . . y CdA N2A C2A C1A -46.4(3) . . . . ? N1A C1A C2A N2A 56.8(4) . . . . y O4A CdA O2A N3A -75.88(18) . . . . ? N2A CdA O2A N3A 96.41(18) . . . . ? N1A CdA O2A N3A 31.2(2) . . . . ? O1A CdA O2A N3A 5.05(16) . . . . ? S2A CdA O2A N3A -126.84(16) . . . . ? S1A CdA O2A N3A 173.48(17) . . . . ? C2A N2A C3A C4A -179.4(2) . . . . y CdA N2A C3A C4A -58.5(3) . . . . ? CdA O2A N3A O3A 169.6(3) . . . . ? CdA O2A N3A O1A -8.8(3) . . . . ? CdA O1A N3A O3A -169.5(3) . . . . ? CdA O1A N3A O2A 8.9(3) . . . . ? O6A N4A O4A CdA -163.92(18) . . . . ? O5A N4A O4A CdA 17.8(3) . . . . ? N2A CdA O4A N4A -131.4(3) . . . . ? N1A CdA O4A N4A 123.1(2) . . . . ? O1A CdA O4A N4A -157.4(2) . . . . ? O2A CdA O4A N4A -104.3(2) . . . . ? S2A CdA O4A N4A 51.8(2) . . . . ? S1A CdA O4A N4A -23.7(2) . . . . ? N2A C3A C4A S1A 55.1(3) . . . . ? C5A S1A C4A C3A 89.8(3) . . . . y C5A' S1A C4A C3A 72.3(3) . . . . y CdA S1A C4A C3A -22.7(2) . . . . ? C4A S1A C5A C6A -72.1(4) . . . . y C5A' S1A C5A C6A -24.4(6) . . . . ? CdA S1A C5A C6A 33.9(5) . . . . ? C5A S1A C5A' C6A' 71.5(8) . . . . ? C4A S1A C5A' C6A' -152.6(5) . . . . y CdA S1A C5A' C6A' -54.2(5) . . . . ? S1A C5A C6A S2A -62.0(5) . . . . y C6A' S2A C6A C5A -66.6(6) . . . . ? C7A S2A C6A C5A 152.7(4) . . . . y CdA S2A C6A C5A 53.3(4) . . . . ? S1A C5A' C6A' S2A 65.0(6) . . . . y C7A S2A C6A' C5A' 74.4(5) . . . . ? C6A S2A C6A' C5A' 29.6(5) . . . . ? CdA S2A C6A' C5A' -36.9(6) . . . . ? C6A' S2A C7A C8A -160.8(3) . . . . ? C6A S2A C7A C8A -141.0(3) . . . . y CdA S2A C7A C8A -42.9(2) . . . . ? C1A N1A C8A C7A 79.7(4) . . . . y CdA N1A C8A C7A -47.0(3) . . . . ? S2A C7A C8A N1A 63.0(3) . . . . y 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 N1 H1C O6 0.93 2.30 3.055(3) 138.0 2_666 N2 H2C O4 0.93 2.21 3.049(3) 150.3 2_566 N1A H1AC O6A 0.93 2.26 3.149(3) 159.0 2_655 N1A H1AC O4A 0.93 2.26 3.057(3) 142.8 2_655 N1A H1AC N4A 0.93 2.62 3.539(4) 168.1 2_655 N2A H2AC O2 0.93 2.21 3.047(3) 150.1 . _diffrn_measured_fraction_theta_max 0.875 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.946 _refine_diff_density_max 1.51 _refine_diff_density_min -1.07 _refine_diff_density_rms 0.08 #===END of CIF #===END of CIF data_cds3no _database_code_depnum_ccdc_archive 'CCDC 225829' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H17 Cd N3 O6 S3' _chemical_formula_weight 459.83 _exptl_special_details ; There are three molecules in the asymmetric unit. Part of the macrocycle of the 3rd molecule has been modelled over two sites in the ratio 7:3. Distance and angle restraints have been applied to all molecules. There remain some large peaks in the residual density, primarily around the Cd atoms. Alternative absorption corrections have been tried and modelling of the disorder but neither of these has solved the problem entirely. ; 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 Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 8.8025(3) _cell_length_b 14.5648(6) _cell_length_c 37.518(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4810.1(4) _cell_formula_units_Z 12 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7672 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 30.44 _exptl_crystal_description 'hexagonal prism' _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.905 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2760 _exptl_absorpt_coefficient_mu 1.779 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.472 _exptl_absorpt_correction_T_max 0.676 _exptl_absorpt_process_details ? _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART1000 CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 46217 _diffrn_reflns_av_R_equivalents 0.0300 _diffrn_reflns_av_sigmaI/netI 0.0135 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -47 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 2.76 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8172 _reflns_number_gt 8059 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.056P)^2^+24.15P] 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 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.07(3) _refine_ls_number_reflns 8172 _refine_ls_number_parameters 575 _refine_ls_number_restraints 448 _refine_ls_R_factor_all 0.0451 _refine_ls_R_factor_gt 0.0444 _refine_ls_wR_factor_ref 0.115 _refine_ls_wR_factor_gt 0.115 _refine_ls_goodness_of_fit_ref 1.07 _refine_ls_restrained_S_all 1.07 _refine_ls_shift/su_max 0.017 _refine_ls_shift/su_mean 0.002 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 0.39469(6) 0.52389(3) 0.087471(13) 0.02806(13) Uani 1 1 d U . . S1A S 0.6275(2) 0.48189(15) 0.04228(6) 0.0474(5) Uani 1 1 d DU . . N1A N 0.3447(7) 0.6203(4) 0.03705(17) 0.0382(14) Uani 1 1 d DU . . H1AC H 0.2580 0.5959 0.0265 0.046 Uiso 1 1 calc R . . O1A O 0.1289(6) 0.4800(4) 0.08708(14) 0.0411(12) Uani 1 1 d U . . C1A C 0.4607(10) 0.6207(6) 0.0085(2) 0.054(2) Uani 1 1 d DU . . H1AA H 0.5384 0.6676 0.0143 0.064 Uiso 1 1 calc R . . H1AB H 0.4116 0.6392 -0.0141 0.064 Uiso 1 1 calc R . . S2A S 0.6480(3) 0.59003(17) 0.12067(6) 0.0516(6) Uani 1 1 d DU . . N2A N 0.1376(7) 0.4197(4) 0.06296(17) 0.0333(13) Uani 1 1 d U . . O2A O 0.2641(6) 0.4087(4) 0.04770(14) 0.0367(12) Uani 1 1 d U . . C2A C 0.5384(10) 0.5303(6) 0.00300(18) 0.058(2) Uani 1 1 d DU . . H2AA H 0.6170 0.5380 -0.0156 0.070 Uiso 1 1 calc R . . H2AB H 0.4628 0.4857 -0.0061 0.070 Uiso 1 1 calc R . . S3A S 0.2765(3) 0.67076(15) 0.11978(7) 0.0507(6) Uani 1 1 d DU . . N3A N 0.4392(7) 0.3968(5) 0.14846(17) 0.0376(14) Uani 1 1 d U . . O3A O 0.0247(7) 0.3763(4) 0.05339(19) 0.0556(17) Uani 1 1 d U . . C3A C 0.7746(8) 0.5622(6) 0.0557(3) 0.062(2) Uani 1 1 d DU . . H3AA H 0.8566 0.5270 0.0675 0.074 Uiso 1 1 calc R . . H3AB H 0.8184 0.5897 0.0338 0.074 Uiso 1 1 calc R . . O4A O 0.4421(7) 0.3834(4) 0.11519(14) 0.0452(13) Uani 1 1 d U . . C4A C 0.7280(10) 0.6400(6) 0.08038(19) 0.056(2) Uani 1 1 d DU . . H4AA H 0.6517 0.6796 0.0685 0.068 Uiso 1 1 calc R . . H4AB H 0.8174 0.6782 0.0864 0.068 Uiso 1 1 calc R . . O5A O 0.3990(8) 0.4732(4) 0.15971(16) 0.0603(17) Uani 1 1 d U . . C5A C 0.5765(10) 0.6893(5) 0.1445(2) 0.061(2) Uani 1 1 d DU . . H5AA H 0.5453 0.6691 0.1686 0.073 Uiso 1 1 calc R . . H5AB H 0.6615 0.7332 0.1476 0.073 Uiso 1 1 calc R . . O6A O 0.4675(7) 0.3339(4) 0.16897(15) 0.0455(14) Uani 1 1 d U . . C6A C 0.4447(8) 0.7404(6) 0.1279(2) 0.057(2) Uani 1 1 d DU . . H6AA H 0.4787 0.7670 0.1050 0.068 Uiso 1 1 calc R . . H6AB H 0.4163 0.7919 0.1438 0.068 Uiso 1 1 calc R . . C7A C 0.2012(10) 0.7200(6) 0.07878(19) 0.056(2) Uani 1 1 d DU . . H7AA H 0.1050 0.6882 0.0729 0.067 Uiso 1 1 calc R . . H7AB H 0.1765 0.7853 0.0833 0.067 Uiso 1 1 calc R . . C8A C 0.3034(10) 0.7150(5) 0.0469(3) 0.052(2) Uani 1 1 d DU . . H8AA H 0.2521 0.7445 0.0264 0.063 Uiso 1 1 calc R . . H8AB H 0.3974 0.7501 0.0519 0.063 Uiso 1 1 calc R . . Cd2 Cd 0.60411(6) 0.02921(3) 0.077613(13) 0.03032(14) Uani 1 1 d U . . S1B S 0.3535(2) 0.01695(13) 0.11988(5) 0.0375(4) Uani 1 1 d DU . . N1B N 0.6804(7) 0.1112(4) 0.12836(15) 0.0347(13) Uani 1 1 d DU . . H1BC H 0.7776 0.0909 0.1341 0.042 Uiso 1 1 calc R . . O1B O 0.6429(7) -0.0451(4) 0.02236(17) 0.0575(15) Uani 1 1 d U . . C1B C 0.5839(8) 0.0927(6) 0.15963(18) 0.0434(18) Uani 1 1 d DU . . H1BA H 0.6128 0.1358 0.1789 0.052 Uiso 1 1 calc R . . H1BB H 0.6056 0.0298 0.1682 0.052 Uiso 1 1 calc R . . S2B S 0.4018(2) 0.13663(12) 0.04039(5) 0.0321(4) Uani 1 1 d DU . . N2B N 0.5299(8) -0.0955(4) 0.02030(18) 0.0371(14) Uani 1 1 d U . . O2B O 0.4307(9) -0.0854(4) 0.04360(18) 0.0612(16) Uani 1 1 d U . . C2B C 0.4158(8) 0.1012(6) 0.1532(2) 0.0459(19) Uani 1 1 d DU . . H2BA H 0.3919 0.1639 0.1448 0.055 Uiso 1 1 calc R . . H2BB H 0.3604 0.0908 0.1758 0.055 Uiso 1 1 calc R . . S3B S 0.7900(2) 0.16261(13) 0.05006(5) 0.0353(4) Uani 1 1 d DU . . N3B N 0.8303(8) -0.1049(4) 0.10040(18) 0.0390(15) Uani 1 1 d U . . O3B O 0.5164(7) -0.1504(4) -0.00442(16) 0.0502(15) Uani 1 1 d U . . C3B C 0.2118(8) 0.0788(5) 0.0945(2) 0.0411(18) Uani 1 1 d DU . . H3BA H 0.1675 0.0359 0.0768 0.049 Uiso 1 1 calc R . . H3BB H 0.1292 0.0969 0.1110 0.049 Uiso 1 1 calc R . . O4B O 0.6887(6) -0.1078(4) 0.10457(19) 0.0547(16) Uani 1 1 d U . . C4B C 0.2636(8) 0.1644(5) 0.07465(18) 0.0381(17) Uani 1 1 d DU . . H4BA H 0.3092 0.2081 0.0918 0.046 Uiso 1 1 calc R . . H4BB H 0.1746 0.1945 0.0635 0.046 Uiso 1 1 calc R . . O5B O 0.9093(7) -0.1681(4) 0.11148(18) 0.0575(16) Uani 1 1 d U . . C5B C 0.5044(7) 0.2447(4) 0.0365(2) 0.0339(16) Uani 1 1 d DU . . H5BA H 0.4485 0.2862 0.0202 0.041 Uiso 1 1 calc R . . H5BB H 0.5097 0.2746 0.0602 0.041 Uiso 1 1 calc R . . O6B O 0.8835(7) -0.0383(4) 0.08471(17) 0.0543(15) Uani 1 1 d U . . C6B C 0.6644(7) 0.2301(5) 0.02238(17) 0.0335(16) Uani 1 1 d DU . . H6BA H 0.7116 0.2910 0.0186 0.040 Uiso 1 1 calc R . . H6BB H 0.6570 0.1999 -0.0012 0.040 Uiso 1 1 calc R . . C7B C 0.8101(9) 0.2278(5) 0.09116(17) 0.0400(18) Uani 1 1 d DU . . H7BA H 0.9118 0.2150 0.1012 0.048 Uiso 1 1 calc R . . H7BB H 0.8066 0.2940 0.0852 0.048 Uiso 1 1 calc R . . C8B C 0.6935(9) 0.2096(4) 0.1197(2) 0.0386(17) Uani 1 1 d DU . . H8BA H 0.7216 0.2439 0.1415 0.046 Uiso 1 1 calc R . . H8BB H 0.5935 0.2325 0.1115 0.046 Uiso 1 1 calc R . . Cd3 Cd -0.07824(5) -0.00415(3) 0.242589(13) 0.02827(13) Uani 1 1 d U . . N1C N -0.1558(7) -0.0972(4) 0.29010(16) 0.0364(14) Uani 1 1 d DU A . H1CA H -0.2487 -0.0729 0.2972 0.044 Uiso 1 1 calc R . . O1C O -0.3517(6) 0.0388(4) 0.24352(15) 0.0469(12) Uani 1 1 d U A . C1C C -0.0619(11) -0.0967(8) 0.3226(2) 0.073(3) Uani 1 1 d DU . . S1C S 0.1347(4) 0.0356(3) 0.29275(8) 0.0363(7) Uani 0.70 1 d PDU A 1 S1C' S 0.1727(11) -0.0022(6) 0.2900(3) 0.044(2) Uani 0.30 1 d PDU A 2 S2C S 0.1832(3) -0.07189(17) 0.21322(7) 0.0536(6) Uani 1 1 d DU A . N2C N -0.3404(8) 0.1056(5) 0.26424(18) 0.0423(16) Uani 1 1 d U . . O2C O -0.2127(8) 0.1187(4) 0.2787(2) 0.0586(16) Uani 1 1 d U A . C2C C 0.0198(13) -0.0088(8) 0.3290(3) 0.053(3) Uiso 0.70 1 d PDU A 1 H2CA H 0.0865 -0.0173 0.3500 0.063 Uiso 0.70 1 calc PR A 1 H2CB H -0.0564 0.0384 0.3354 0.063 Uiso 0.70 1 calc PR A 1 C2C' C 0.1052(14) -0.0841(14) 0.3227(5) 0.037(5) Uiso 0.30 1 d PDU A 2 H2CC H 0.1541 -0.1441 0.3181 0.044 Uiso 0.30 1 calc PR A 2 H2CD H 0.1370 -0.0633 0.3467 0.044 Uiso 0.30 1 calc PR A 2 S3C S -0.1911(3) -0.14506(16) 0.20581(6) 0.0497(6) Uani 1 1 d DU A . N3C N -0.0177(8) 0.1197(5) 0.18113(18) 0.0403(15) Uani 1 1 d U . . O3C O -0.4487(8) 0.1539(5) 0.2712(2) 0.074(2) Uani 1 1 d U A . C3C C 0.2814(11) -0.0499(7) 0.2839(3) 0.049(3) Uiso 0.70 1 d PDU A 1 H3CA H 0.3750 -0.0172 0.2766 0.059 Uiso 0.70 1 calc PR A 1 H3CC H 0.3039 -0.0822 0.3065 0.059 Uiso 0.70 1 calc PR A 1 C3C' C 0.320(3) -0.0694(17) 0.2668(7) 0.041(6) Uiso 0.30 1 d PDU A 2 H3CB H 0.3754 -0.0279 0.2505 0.050 Uiso 0.30 1 calc PR A 2 H3CD H 0.3931 -0.0920 0.2848 0.050 Uiso 0.30 1 calc PR A 2 O4C O -0.0345(9) 0.1320(4) 0.21358(17) 0.0648(18) Uani 1 1 d U A . C4C C 0.2458(12) -0.1220(7) 0.2555(2) 0.035(2) Uiso 0.70 1 d PDU A 1 H4CA H 0.1653 -0.1633 0.2646 0.042 Uiso 0.70 1 calc PR A 1 H4CB H 0.3377 -0.1595 0.2512 0.042 Uiso 0.70 1 calc PR A 1 C4C' C 0.263(3) -0.1512(13) 0.2454(6) 0.054(8) Uiso 0.30 1 d PDU A 2 H4CC H 0.1860 -0.1887 0.2579 0.065 Uiso 0.30 1 calc PR A 2 H4CD H 0.3452 -0.1902 0.2356 0.065 Uiso 0.30 1 calc PR A 2 O5C O -0.0515(10) 0.0450(4) 0.1704(2) 0.081(3) Uani 1 1 d U A . C5C C 0.1130(10) -0.1665(5) 0.1872(2) 0.060(2) Uani 1 1 d DU . . H5CA H 0.0897 -0.1429 0.1631 0.073 Uiso 1 1 calc R A . H5CB H 0.1970 -0.2112 0.1846 0.073 Uiso 1 1 calc R . . O6C O 0.0153(9) 0.1837(5) 0.16151(16) 0.066(2) Uani 1 1 d U A . C6C C -0.0249(8) -0.2186(5) 0.2002(2) 0.053(2) Uani 1 1 d DU A . H6CA H -0.0008 -0.2483 0.2232 0.063 Uiso 1 1 calc R . . H6CB H -0.0493 -0.2677 0.1828 0.063 Uiso 1 1 calc R . . C7C C -0.2806(8) -0.1966(5) 0.24451(19) 0.061(2) Uani 1 1 d DU . . H7CA H -0.3796 -0.1659 0.2484 0.073 Uiso 1 1 calc R A . H7CB H -0.3018 -0.2618 0.2391 0.073 Uiso 1 1 calc R . . C8C C -0.1910(9) -0.1923(5) 0.2788(2) 0.050(2) Uani 1 1 d DU A . H8CA H -0.2496 -0.2230 0.2979 0.060 Uiso 1 1 calc R . . H8CB H -0.0947 -0.2264 0.2757 0.060 Uiso 1 1 calc R . . 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 0.0280(2) 0.0262(3) 0.0299(3) -0.00350(18) 0.0031(2) -0.0026(2) S1A 0.0385(10) 0.0469(12) 0.0569(13) -0.0055(10) 0.0138(9) 0.0049(9) N1A 0.038(3) 0.034(3) 0.043(3) -0.004(3) 0.002(3) -0.004(3) O1A 0.039(3) 0.043(3) 0.041(3) -0.012(2) 0.007(2) -0.008(2) C1A 0.066(6) 0.061(5) 0.033(5) 0.011(4) 0.010(4) 0.007(4) S2A 0.0472(12) 0.0576(14) 0.0501(13) 0.0047(10) -0.0158(10) -0.0131(10) N2A 0.030(3) 0.028(3) 0.041(4) 0.001(3) 0.002(3) -0.007(2) O2A 0.031(2) 0.038(3) 0.041(3) -0.009(2) 0.001(2) -0.006(2) C2A 0.066(5) 0.069(6) 0.039(4) -0.016(4) 0.018(4) -0.004(4) S3A 0.0501(12) 0.0390(12) 0.0630(14) -0.0245(10) 0.0290(11) -0.0135(10) N3A 0.040(3) 0.039(3) 0.034(3) 0.002(3) 0.007(3) -0.003(3) O3A 0.039(3) 0.047(4) 0.081(5) -0.019(3) 0.009(3) -0.018(3) C3A 0.028(4) 0.066(6) 0.090(7) -0.002(5) 0.015(4) -0.002(4) O4A 0.061(4) 0.040(3) 0.034(3) -0.006(2) 0.005(3) 0.005(3) C4A 0.043(5) 0.061(6) 0.065(6) -0.005(4) 0.010(4) -0.022(4) O5A 0.091(5) 0.039(3) 0.051(4) -0.005(3) 0.030(4) -0.005(3) C5A 0.072(6) 0.074(6) 0.037(5) -0.015(4) 0.001(4) -0.034(5) O6A 0.048(3) 0.055(3) 0.034(3) 0.008(3) -0.001(3) 0.002(3) C6A 0.055(5) 0.051(5) 0.063(6) -0.030(4) 0.022(4) -0.022(4) C7A 0.047(5) 0.031(4) 0.090(6) -0.013(4) 0.007(4) 0.004(4) C8A 0.046(5) 0.029(4) 0.082(6) -0.001(4) 0.009(4) -0.002(4) Cd2 0.0329(3) 0.0252(3) 0.0329(3) 0.0053(2) 0.0014(2) 0.0025(2) S1B 0.0400(9) 0.0379(11) 0.0348(10) 0.0067(8) 0.0039(7) -0.0076(8) N1B 0.033(3) 0.041(3) 0.030(3) 0.007(2) 0.000(2) 0.001(3) O1B 0.058(4) 0.054(4) 0.060(4) -0.018(3) 0.006(3) -0.003(3) C1B 0.043(4) 0.058(5) 0.029(4) 0.007(3) -0.008(3) -0.002(4) S2B 0.0348(9) 0.0356(9) 0.0260(9) 0.0019(7) -0.0016(8) 0.0053(8) N2B 0.047(4) 0.029(3) 0.035(4) 0.001(3) 0.004(3) 0.006(3) O2B 0.087(4) 0.034(3) 0.063(4) -0.003(3) 0.017(3) -0.012(3) C2B 0.044(4) 0.068(5) 0.026(4) -0.003(3) 0.008(3) -0.018(4) S3B 0.0362(9) 0.0320(10) 0.0379(11) 0.0042(8) 0.0067(8) 0.0018(8) N3B 0.044(4) 0.030(3) 0.043(4) 0.002(3) -0.004(3) 0.010(3) O3B 0.064(4) 0.044(3) 0.042(3) -0.007(3) -0.002(3) -0.002(3) C3B 0.033(4) 0.053(5) 0.038(4) 0.003(3) 0.002(3) 0.006(3) O4B 0.036(3) 0.038(3) 0.090(5) 0.023(3) 0.007(3) 0.004(2) C4B 0.034(4) 0.052(5) 0.028(4) 0.002(3) 0.002(3) 0.008(3) O5B 0.055(4) 0.050(3) 0.068(4) -0.004(3) -0.010(3) 0.028(3) C5B 0.040(4) 0.027(3) 0.035(4) 0.006(3) 0.004(3) 0.010(3) O6B 0.045(3) 0.050(3) 0.068(4) 0.008(3) 0.007(3) -0.004(3) C6B 0.043(4) 0.029(4) 0.029(4) 0.004(3) 0.006(3) 0.003(3) C7B 0.041(4) 0.035(4) 0.044(4) -0.002(3) 0.005(3) -0.006(3) C8B 0.041(4) 0.034(4) 0.040(4) -0.005(3) -0.001(3) 0.000(3) Cd3 0.0286(2) 0.0289(2) 0.0272(3) -0.0013(2) -0.0015(2) -0.00087(19) N1C 0.028(3) 0.035(3) 0.046(4) 0.009(3) 0.001(3) 0.003(2) O1C 0.048(3) 0.051(3) 0.042(3) 0.005(3) -0.011(2) 0.007(2) C1C 0.060(6) 0.121(9) 0.038(5) 0.034(5) -0.013(4) -0.021(6) S1C 0.0346(18) 0.046(2) 0.0279(15) -0.0022(15) -0.0066(12) -0.0063(16) S1C' 0.039(4) 0.030(5) 0.064(5) -0.020(4) -0.011(3) 0.006(3) S2C 0.0421(11) 0.0594(14) 0.0595(15) 0.0140(11) 0.0171(10) 0.0079(10) N2C 0.044(3) 0.048(4) 0.036(4) 0.005(3) 0.003(3) 0.019(3) O2C 0.054(3) 0.035(3) 0.087(5) -0.011(3) -0.010(3) 0.013(3) S3C 0.0481(12) 0.0424(12) 0.0585(14) -0.0170(10) -0.0223(10) 0.0057(10) N3C 0.055(4) 0.034(3) 0.032(4) 0.003(3) -0.002(3) -0.002(3) O3C 0.071(4) 0.075(5) 0.076(5) 0.019(4) 0.020(4) 0.047(4) O4C 0.102(5) 0.046(3) 0.046(3) 0.012(3) 0.006(3) -0.012(3) O5C 0.111(6) 0.032(3) 0.098(5) 0.006(3) -0.074(5) 0.000(3) C5C 0.058(5) 0.066(6) 0.057(6) 0.001(4) 0.008(5) 0.026(4) O6C 0.114(6) 0.054(4) 0.029(3) 0.010(3) -0.011(3) -0.023(4) C6C 0.064(5) 0.048(5) 0.047(5) -0.026(4) 0.000(4) 0.011(4) C7C 0.032(4) 0.041(4) 0.109(7) -0.039(5) 0.000(4) -0.005(3) C8C 0.036(4) 0.023(4) 0.091(6) 0.016(4) 0.018(4) 0.000(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O4A 2.332(6) . y Cd1 N1A 2.396(7) . y Cd1 O1A 2.426(5) . y Cd1 O2A 2.523(5) . y Cd1 S3A 2.670(2) . y Cd1 S1A 2.7288(19) . y Cd1 S2A 2.729(2) . y S1A C2A 1.812(6) . ? S1A C3A 1.817(6) . ? N1A C8A 1.474(7) . ? N1A C1A 1.480(7) . ? O1A N2A 1.263(8) . ? C1A C2A 1.499(8) . ? S2A C5A 1.813(6) . ? S2A C4A 1.820(6) . ? N2A O3A 1.231(8) . ? N2A O2A 1.262(8) . ? S3A C6A 1.820(6) . ? S3A C7A 1.822(6) . ? N3A O6A 1.223(9) . ? N3A O5A 1.241(9) . ? N3A O4A 1.264(8) . ? C3A C4A 1.521(8) . ? C5A C6A 1.512(8) . ? C7A C8A 1.498(8) . ? Cd2 N1B 2.346(6) . y Cd2 O4B 2.357(6) . y Cd2 O1B 2.364(6) . y Cd2 O2B 2.596(7) . y Cd2 O6B 2.662(8) . y Cd2 S1B 2.7227(19) . y Cd2 S3B 2.7423(19) . y Cd2 S2B 2.7509(18) . y S1B C3B 1.811(6) . ? S1B C2B 1.836(8) . ? N1B C8B 1.473(7) . ? N1B C1B 1.473(7) . ? O1B N2B 1.238(9) . ? C1B C2B 1.505(8) . ? S2B C4B 1.815(5) . ? S2B C5B 1.821(5) . ? N2B O3B 1.230(9) . ? N2B O2B 1.244(9) . ? S3B C6B 1.807(5) . ? S3B C7B 1.820(6) . ? N3B O5B 1.226(8) . ? N3B O6B 1.228(9) . ? N3B O4B 1.257(9) . ? C3B C4B 1.521(7) . ? C5B C6B 1.520(7) . ? C7B C8B 1.506(8) . ? Cd3 O4C 2.295(6) . y Cd3 N1C 2.341(6) . y Cd3 O1C 2.487(5) . y Cd3 O2C 2.537(6) . y Cd3 S3C 2.665(2) . y Cd3 S1C 2.718(3) . y Cd3 S2C 2.735(2) . y Cd3 S1C' 2.836(9) . ? N1C C1C 1.472(7) . ? N1C C8C 1.480(7) . ? O1C N2C 1.249(9) . ? C1C C2C' 1.482(9) . ? C1C C2C 1.487(9) . ? S1C C2C 1.815(7) . ? S1C C3C 1.824(7) . ? S1C' C2C' 1.811(8) . ? S1C' C3C' 1.84(3) . ? S2C C5C 1.797(6) . ? S2C C4C' 1.811(8) . ? S2C C4C 1.831(6) . ? N2C O3C 1.212(9) . ? N2C O2C 1.262(9) . ? S3C C7C 1.814(6) . ? S3C C6C 1.826(6) . ? N3C O5C 1.197(9) . ? N3C O6C 1.224(9) . ? N3C O4C 1.239(9) . ? C3C C4C 1.528(8) . ? C3C' C4C' 1.522(9) . ? C5C C6C 1.512(8) . ? C7C C8C 1.511(8) . ? 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 O4A Cd1 N1A 153.97(19) . . ? O4A Cd1 O1A 86.8(2) . . ? N1A Cd1 O1A 88.4(2) . . ? O4A Cd1 O2A 76.23(19) . . ? N1A Cd1 O2A 80.74(19) . . ? O1A Cd1 O2A 51.78(16) . . ? O4A Cd1 S3A 124.75(14) . . ? N1A Cd1 S3A 79.49(14) . . ? O1A Cd1 S3A 80.69(13) . . ? O2A Cd1 S3A 128.60(13) . . ? O4A Cd1 S1A 86.90(15) . . ? N1A Cd1 S1A 77.21(14) . . ? O1A Cd1 S1A 131.41(13) . . ? O2A Cd1 S1A 79.96(12) . . ? S3A Cd1 S1A 138.96(7) . . ? O4A Cd1 S2A 87.69(16) . . ? N1A Cd1 S2A 107.66(16) . . ? O1A Cd1 S2A 152.09(13) . . ? O2A Cd1 S2A 151.28(13) . . ? S3A Cd1 S2A 80.11(8) . . ? S1A Cd1 S2A 75.49(7) . . ? C2A S1A C3A 106.4(5) . . ? C2A S1A Cd1 95.4(3) . . ? C3A S1A Cd1 102.7(3) . . ? C8A N1A C1A 110.3(6) . . ? C8A N1A Cd1 113.3(5) . . ? C1A N1A Cd1 116.6(5) . . ? N2A O1A Cd1 97.4(4) . . ? N1A C1A C2A 114.2(7) . . ? C5A S2A C4A 103.0(4) . . ? C5A S2A Cd1 102.9(3) . . ? C4A S2A Cd1 94.5(3) . . ? O3A N2A O2A 121.0(6) . . ? O3A N2A O1A 121.1(6) . . ? O2A N2A O1A 117.8(6) . . ? N2A O2A Cd1 92.8(4) . . ? C1A C2A S1A 115.3(6) . . ? C6A S3A C7A 102.6(4) . . ? C6A S3A Cd1 101.9(3) . . ? C7A S3A Cd1 94.2(3) . . ? O6A N3A O5A 121.1(7) . . ? O6A N3A O4A 120.1(7) . . ? O5A N3A O4A 118.7(7) . . ? C4A C3A S1A 117.1(5) . . ? N3A O4A Cd1 107.5(4) . . ? C3A C4A S2A 108.3(6) . . ? C6A C5A S2A 117.1(6) . . ? C5A C6A S3A 114.8(6) . . ? C8A C7A S3A 115.9(6) . . ? N1A C8A C7A 113.2(6) . . ? N1B Cd2 O4B 89.6(2) . . ? N1B Cd2 O1B 154.7(2) . . ? O4B Cd2 O1B 86.7(2) . . ? N1B Cd2 O2B 153.44(19) . . ? O4B Cd2 O2B 81.5(2) . . ? O1B Cd2 O2B 50.2(2) . . ? N1B Cd2 S1B 78.04(15) . . ? O4B Cd2 S1B 87.17(15) . . ? O1B Cd2 S1B 126.71(16) . . ? O2B Cd2 S1B 76.57(15) . . ? N1B Cd2 S3B 76.95(13) . . ? O4B Cd2 S3B 124.96(14) . . ? O1B Cd2 S3B 84.71(17) . . ? O2B Cd2 S3B 128.37(15) . . ? S1B Cd2 S3B 138.53(6) . . ? N1B Cd2 S2B 107.92(15) . . ? O4B Cd2 S2B 154.62(16) . . ? O1B Cd2 S2B 84.77(17) . . ? O2B Cd2 S2B 74.67(16) . . ? S1B Cd2 S2B 78.96(6) . . ? S3B Cd2 S2B 77.98(6) . . ? C3B S1B C2B 103.4(4) . . ? C3B S1B Cd2 102.6(2) . . ? C2B S1B Cd2 96.4(2) . . ? C8B N1B C1B 113.5(6) . . ? C8B N1B Cd2 109.7(4) . . ? C1B N1B Cd2 112.8(5) . . ? N2B O1B Cd2 102.1(5) . . ? N1B C1B C2B 115.2(6) . . ? C4B S2B C5B 101.3(3) . . ? C4B S2B Cd2 101.6(2) . . ? C5B S2B Cd2 102.2(2) . . ? O3B N2B O1B 120.7(7) . . ? O3B N2B O2B 122.6(7) . . ? O1B N2B O2B 116.7(7) . . ? N2B O2B Cd2 90.5(5) . . ? C1B C2B S1B 110.4(6) . . ? C6B S3B C7B 105.2(4) . . ? C6B S3B Cd2 103.7(2) . . ? C7B S3B Cd2 96.2(2) . . ? O5B N3B O6B 122.6(7) . . ? O5B N3B O4B 119.7(7) . . ? O6B N3B O4B 117.6(6) . . ? C4B C3B S1B 117.3(5) . . ? N3B O4B Cd2 103.4(4) . . ? C3B C4B S2B 111.4(5) . . ? C6B C5B S2B 111.5(4) . . ? C5B C6B S3B 116.3(5) . . ? C8B C7B S3B 116.3(5) . . ? N1B C8B C7B 112.5(6) . . ? O4C Cd3 N1C 155.6(2) . . ? O4C Cd3 O1C 87.2(2) . . ? N1C Cd3 O1C 81.5(2) . . ? O4C Cd3 O2C 73.9(2) . . ? N1C Cd3 O2C 82.3(2) . . ? O1C Cd3 O2C 50.5(2) . . ? O4C Cd3 S3C 118.85(18) . . ? N1C Cd3 S3C 80.77(15) . . ? O1C Cd3 S3C 80.81(14) . . ? O2C Cd3 S3C 130.21(16) . . ? O4C Cd3 S1C 91.6(2) . . ? N1C Cd3 S1C 78.31(15) . . ? O1C Cd3 S1C 127.15(16) . . ? O2C Cd3 S1C 78.57(17) . . ? S3C Cd3 S1C 141.21(10) . . ? O4C Cd3 S2C 88.8(2) . . ? N1C Cd3 S2C 110.08(16) . . ? O1C Cd3 S2C 155.57(15) . . ? O2C Cd3 S2C 149.52(16) . . ? S3C Cd3 S2C 80.06(8) . . ? S1C Cd3 S2C 77.04(10) . . ? O4C Cd3 S1C' 99.1(3) . . ? N1C Cd3 S1C' 75.8(2) . . ? O1C Cd3 S1C' 137.9(2) . . ? O2C Cd3 S1C' 91.2(2) . . ? S3C Cd3 S1C' 128.52(17) . . ? S1C Cd3 S1C' 13.28(14) . . ? S2C Cd3 S1C' 66.5(2) . . ? C1C N1C C8C 111.0(7) . . ? C1C N1C Cd3 117.6(5) . . ? C8C N1C Cd3 112.6(5) . . ? N2C O1C Cd3 97.3(4) . . ? N1C C1C C2C' 124.1(11) . . ? N1C C1C C2C 114.2(8) . . ? C2C' C1C C2C 54.1(11) . . ? C2C S1C C3C 106.7(6) . . ? C2C S1C Cd3 93.4(4) . . ? C3C S1C Cd3 102.5(4) . . ? C2C' S1C' C3C' 101.5(12) . . ? C2C' S1C' Cd3 99.4(7) . . ? C3C' S1C' Cd3 104.2(9) . . ? C5C S2C C4C' 90.3(8) . . ? C5C S2C C4C 105.5(5) . . ? C4C' S2C C4C 18.7(9) . . ? C5C S2C Cd3 101.9(3) . . ? C4C' S2C Cd3 106.7(11) . . ? C4C S2C Cd3 92.7(4) . . ? O3C N2C O1C 121.5(8) . . ? O3C N2C O2C 121.4(8) . . ? O1C N2C O2C 117.1(6) . . ? N2C O2C Cd3 94.6(5) . . ? C1C C2C S1C 117.0(7) . . ? C1C C2C' S1C' 113.9(10) . . ? C7C S3C C6C 101.4(4) . . ? C7C S3C Cd3 93.8(2) . . ? C6C S3C Cd3 102.3(3) . . ? O5C N3C O6C 123.3(8) . . ? O5C N3C O4C 115.7(8) . . ? O6C N3C O4C 120.6(7) . . ? C4C C3C S1C 116.8(7) . . ? C4C' C3C' S1C' 116(2) . . ? N3C O4C Cd3 111.1(5) . . ? C3C C4C S2C 113.1(7) . . ? C3C' C4C' S2C 88.9(13) . . ? C6C C5C S2C 119.2(6) . . ? C5C C6C S3C 112.7(6) . . ? C8C C7C S3C 115.9(5) . . ? N1C C8C C7C 113.0(6) . . ? 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 O4A Cd1 S1A C2A 142.3(3) . . . . ? N1A Cd1 S1A C2A -17.0(3) . . . . ? O1A Cd1 S1A C2A 59.3(4) . . . . ? O2A Cd1 S1A C2A 65.7(3) . . . . ? S3A Cd1 S1A C2A -73.9(3) . . . . ? S2A Cd1 S1A C2A -129.3(3) . . . . ? O4A Cd1 S1A C3A -109.6(4) . . . . ? N1A Cd1 S1A C3A 91.2(4) . . . . ? O1A Cd1 S1A C3A 167.5(4) . . . . ? O2A Cd1 S1A C3A 173.9(4) . . . . ? S3A Cd1 S1A C3A 34.3(4) . . . . ? S2A Cd1 S1A C3A -21.1(4) . . . . ? O4A Cd1 N1A C8A 170.8(5) . . . . ? O1A Cd1 N1A C8A 91.3(5) . . . . ? O2A Cd1 N1A C8A 142.8(5) . . . . ? S3A Cd1 N1A C8A 10.5(5) . . . . ? S1A Cd1 N1A C8A -135.5(5) . . . . ? S2A Cd1 N1A C8A -65.5(5) . . . . ? O4A Cd1 N1A C1A -59.5(8) . . . . ? O1A Cd1 N1A C1A -139.0(6) . . . . ? O2A Cd1 N1A C1A -87.5(6) . . . . ? S3A Cd1 N1A C1A 140.2(6) . . . . ? S1A Cd1 N1A C1A -5.8(5) . . . . ? S2A Cd1 N1A C1A 64.2(6) . . . . ? O4A Cd1 O1A N2A -72.7(4) . . . . ? N1A Cd1 O1A N2A 81.7(4) . . . . ? O2A Cd1 O1A N2A 2.2(4) . . . . ? S3A Cd1 O1A N2A 161.3(4) . . . . ? S1A Cd1 O1A N2A 10.3(5) . . . . ? S2A Cd1 O1A N2A -151.7(3) . . . . ? C8A N1A C1A C2A 165.4(8) . . . . ? Cd1 N1A C1A C2A 34.3(9) . . . . ? O4A Cd1 S2A C5A -124.4(3) . . . . ? N1A Cd1 S2A C5A 77.0(4) . . . . ? O1A Cd1 S2A C5A -45.7(5) . . . . ? O2A Cd1 S2A C5A -179.7(4) . . . . ? S3A Cd1 S2A C5A 1.5(3) . . . . ? S1A Cd1 S2A C5A 148.2(3) . . . . ? O4A Cd1 S2A C4A 131.1(3) . . . . ? N1A Cd1 S2A C4A -27.5(3) . . . . ? O1A Cd1 S2A C4A -150.1(4) . . . . ? O2A Cd1 S2A C4A 75.8(4) . . . . ? S3A Cd1 S2A C4A -103.0(3) . . . . ? S1A Cd1 S2A C4A 43.7(3) . . . . ? Cd1 O1A N2A O3A 179.6(6) . . . . ? Cd1 O1A N2A O2A -4.0(7) . . . . ? O3A N2A O2A Cd1 -179.8(6) . . . . ? O1A N2A O2A Cd1 3.8(6) . . . . ? O4A Cd1 O2A N2A 94.7(4) . . . . ? N1A Cd1 O2A N2A -97.6(4) . . . . ? O1A Cd1 O2A N2A -2.2(4) . . . . ? S3A Cd1 O2A N2A -29.1(5) . . . . ? S1A Cd1 O2A N2A -176.1(4) . . . . ? S2A Cd1 O2A N2A 152.4(3) . . . . ? N1A C1A C2A S1A -55.4(10) . . . . ? C3A S1A C2A C1A -62.6(8) . . . . ? Cd1 S1A C2A C1A 42.4(7) . . . . ? O4A Cd1 S3A C6A 100.8(4) . . . . ? N1A Cd1 S3A C6A -89.6(4) . . . . ? O1A Cd1 S3A C6A -179.7(4) . . . . ? O2A Cd1 S3A C6A -158.7(4) . . . . ? S1A Cd1 S3A C6A -33.4(4) . . . . ? S2A Cd1 S3A C6A 20.6(3) . . . . ? O4A Cd1 S3A C7A -155.3(3) . . . . ? N1A Cd1 S3A C7A 14.3(3) . . . . ? O1A Cd1 S3A C7A -75.9(3) . . . . ? O2A Cd1 S3A C7A -54.8(3) . . . . ? S1A Cd1 S3A C7A 70.5(3) . . . . ? S2A Cd1 S3A C7A 124.5(3) . . . . ? C2A S1A C3A C4A 87.4(8) . . . . ? Cd1 S1A C3A C4A -12.2(8) . . . . ? O6A N3A O4A Cd1 -176.9(5) . . . . ? O5A N3A O4A Cd1 7.1(8) . . . . ? N1A Cd1 O4A N3A -172.4(5) . . . . ? O1A Cd1 O4A N3A -92.6(5) . . . . ? O2A Cd1 O4A N3A -144.0(5) . . . . ? S3A Cd1 O4A N3A -16.3(5) . . . . ? S1A Cd1 O4A N3A 135.6(5) . . . . ? S2A Cd1 O4A N3A 60.0(5) . . . . ? S1A C3A C4A S2A 58.1(9) . . . . ? C5A S2A C4A C3A -173.0(6) . . . . ? Cd1 S2A C4A C3A -68.6(6) . . . . ? C4A S2A C5A C6A 66.6(8) . . . . ? Cd1 S2A C5A C6A -31.1(7) . . . . ? S2A C5A C6A S3A 57.3(9) . . . . ? C7A S3A C6A C5A -145.3(6) . . . . ? Cd1 S3A C6A C5A -48.2(6) . . . . ? C6A S3A C7A C8A 61.2(7) . . . . ? Cd1 S3A C7A C8A -42.0(6) . . . . ? C1A N1A C8A C7A -172.7(7) . . . . ? Cd1 N1A C8A C7A -39.9(9) . . . . ? S3A C7A C8A N1A 59.6(10) . . . . ? N1B Cd2 S1B C3B 115.9(3) . . . . ? O4B Cd2 S1B C3B -154.0(3) . . . . ? O1B Cd2 S1B C3B -70.2(4) . . . . ? O2B Cd2 S1B C3B -72.0(3) . . . . ? S3B Cd2 S1B C3B 61.9(3) . . . . ? S2B Cd2 S1B C3B 4.7(3) . . . . ? N1B Cd2 S1B C2B 10.5(3) . . . . ? O4B Cd2 S1B C2B 100.7(3) . . . . ? O1B Cd2 S1B C2B -175.5(3) . . . . ? O2B Cd2 S1B C2B -177.3(3) . . . . ? S3B Cd2 S1B C2B -43.4(3) . . . . ? S2B Cd2 S1B C2B -100.7(3) . . . . ? O4B Cd2 N1B C8B 162.1(5) . . . . ? O1B Cd2 N1B C8B 80.7(7) . . . . ? O2B Cd2 N1B C8B -128.1(5) . . . . ? S1B Cd2 N1B C8B -110.7(5) . . . . ? S3B Cd2 N1B C8B 35.9(4) . . . . ? S2B Cd2 N1B C8B -36.6(5) . . . . ? O4B Cd2 N1B C1B -70.2(5) . . . . ? O1B Cd2 N1B C1B -151.6(5) . . . . ? O2B Cd2 N1B C1B -0.4(8) . . . . ? S1B Cd2 N1B C1B 17.0(4) . . . . ? S3B Cd2 N1B C1B 163.6(5) . . . . ? S2B Cd2 N1B C1B 91.0(5) . . . . ? N1B Cd2 O1B N2B 159.7(5) . . . . ? O4B Cd2 O1B N2B 77.6(5) . . . . ? O2B Cd2 O1B N2B -4.1(4) . . . . ? S1B Cd2 O1B N2B -6.4(6) . . . . ? S3B Cd2 O1B N2B -156.8(5) . . . . ? S2B Cd2 O1B N2B -78.4(5) . . . . ? C8B N1B C1B C2B 75.5(9) . . . . ? Cd2 N1B C1B C2B -50.2(8) . . . . ? N1B Cd2 S2B C4B -53.2(3) . . . . ? O4B Cd2 S2B C4B 78.3(5) . . . . ? O1B Cd2 S2B C4B 149.2(3) . . . . ? O2B Cd2 S2B C4B 99.2(3) . . . . ? S1B Cd2 S2B C4B 20.2(3) . . . . ? S3B Cd2 S2B C4B -125.1(3) . . . . ? N1B Cd2 S2B C5B 51.2(3) . . . . ? O4B Cd2 S2B C5B -177.3(5) . . . . ? O1B Cd2 S2B C5B -106.3(3) . . . . ? O2B Cd2 S2B C5B -156.4(3) . . . . ? S1B Cd2 S2B C5B 124.7(2) . . . . ? S3B Cd2 S2B C5B -20.6(2) . . . . ? Cd2 O1B N2B O3B -174.9(6) . . . . ? Cd2 O1B N2B O2B 7.3(8) . . . . ? O3B N2B O2B Cd2 175.8(6) . . . . ? O1B N2B O2B Cd2 -6.5(7) . . . . ? N1B Cd2 O2B N2B -160.5(5) . . . . ? O4B Cd2 O2B N2B -88.9(5) . . . . ? O1B Cd2 O2B N2B 3.9(4) . . . . ? S1B Cd2 O2B N2B -178.0(5) . . . . ? S3B Cd2 O2B N2B 39.5(5) . . . . ? S2B Cd2 O2B N2B 100.0(4) . . . . ? N1B C1B C2B S1B 62.2(9) . . . . ? C3B S1B C2B C1B -142.3(6) . . . . ? Cd2 S1B C2B C1B -37.7(6) . . . . ? N1B Cd2 S3B C6B -116.2(3) . . . . ? O4B Cd2 S3B C6B 163.7(3) . . . . ? O1B Cd2 S3B C6B 81.4(3) . . . . ? O2B Cd2 S3B C6B 54.7(3) . . . . ? S1B Cd2 S3B C6B -61.9(3) . . . . ? S2B Cd2 S3B C6B -4.4(2) . . . . ? N1B Cd2 S3B C7B -8.8(3) . . . . ? O4B Cd2 S3B C7B -89.0(4) . . . . ? O1B Cd2 S3B C7B -171.2(3) . . . . ? O2B Cd2 S3B C7B 162.1(4) . . . . ? S1B Cd2 S3B C7B 45.5(3) . . . . ? S2B Cd2 S3B C7B 103.0(3) . . . . ? C2B S1B C3B C4B 61.7(7) . . . . ? Cd2 S1B C3B C4B -38.2(6) . . . . ? O5B N3B O4B Cd2 -179.4(6) . . . . ? O6B N3B O4B Cd2 -0.4(9) . . . . ? N1B Cd2 O4B N3B -78.3(5) . . . . ? O1B Cd2 O4B N3B 76.7(5) . . . . ? O2B Cd2 O4B N3B 126.9(6) . . . . ? S1B Cd2 O4B N3B -156.3(5) . . . . ? S3B Cd2 O4B N3B -4.6(6) . . . . ? S2B Cd2 O4B N3B 147.2(4) . . . . ? S1B C3B C4B S2B 63.7(7) . . . . ? C5B S2B C4B C3B -154.6(5) . . . . ? Cd2 S2B C4B C3B -49.4(5) . . . . ? C4B S2B C5B C6B 155.0(5) . . . . ? Cd2 S2B C5B C6B 50.4(5) . . . . ? S2B C5B C6B S3B -63.3(7) . . . . ? C7B S3B C6B C5B -62.8(6) . . . . ? Cd2 S3B C6B C5B 37.6(6) . . . . ? C6B S3B C7B C8B 88.1(7) . . . . ? Cd2 S3B C7B C8B -18.0(6) . . . . ? C1B N1B C8B C7B 171.6(6) . . . . ? Cd2 N1B C8B C7B -61.1(7) . . . . ? S3B C7B C8B N1B 53.2(9) . . . . ? O4C Cd3 N1C C1C -69.6(9) . . . . ? O1C Cd3 N1C C1C -133.1(7) . . . . ? O2C Cd3 N1C C1C -82.1(7) . . . . ? S3C Cd3 N1C C1C 144.9(7) . . . . ? S1C Cd3 N1C C1C -2.2(6) . . . . ? S2C Cd3 N1C C1C 69.2(7) . . . . ? S1C' Cd3 N1C C1C 11.2(7) . . . . ? O4C Cd3 N1C C8C 159.4(6) . . . . ? O1C Cd3 N1C C8C 95.9(5) . . . . ? O2C Cd3 N1C C8C 146.9(5) . . . . ? S3C Cd3 N1C C8C 13.9(5) . . . . ? S1C Cd3 N1C C8C -133.2(5) . . . . ? S2C Cd3 N1C C8C -61.9(5) . . . . ? S1C' Cd3 N1C C8C -119.9(5) . . . . ? O4C Cd3 O1C N2C -67.1(5) . . . . ? N1C Cd3 O1C N2C 91.1(4) . . . . ? O2C Cd3 O1C N2C 4.1(4) . . . . ? S3C Cd3 O1C N2C 173.0(4) . . . . ? S1C Cd3 O1C N2C 22.8(5) . . . . ? S2C Cd3 O1C N2C -148.1(4) . . . . ? S1C' Cd3 O1C N2C 33.4(6) . . . . ? C8C N1C C1C C2C' 99.2(14) . . . . ? Cd3 N1C C1C C2C' -32.6(16) . . . . ? C8C N1C C1C C2C 161.0(8) . . . . ? Cd3 N1C C1C C2C 29.2(11) . . . . ? O4C Cd3 S1C C2C 139.2(5) . . . . ? N1C Cd3 S1C C2C -18.3(4) . . . . ? O1C Cd3 S1C C2C 51.5(5) . . . . ? O2C Cd3 S1C C2C 66.1(4) . . . . ? S3C Cd3 S1C C2C -77.0(4) . . . . ? S2C Cd3 S1C C2C -132.3(4) . . . . ? S1C' Cd3 S1C C2C -96.2(12) . . . . ? O4C Cd3 S1C C3C -112.8(5) . . . . ? N1C Cd3 S1C C3C 89.6(5) . . . . ? O1C Cd3 S1C C3C 159.4(5) . . . . ? O2C Cd3 S1C C3C 174.0(5) . . . . ? S3C Cd3 S1C C3C 30.9(5) . . . . ? S2C Cd3 S1C C3C -24.4(5) . . . . ? S1C' Cd3 S1C C3C 11.8(11) . . . . ? O4C Cd3 S1C' C2C' 160.7(8) . . . . ? N1C Cd3 S1C' C2C' 5.2(8) . . . . ? O1C Cd3 S1C' C2C' 64.8(9) . . . . ? O2C Cd3 S1C' C2C' 86.9(8) . . . . ? S3C Cd3 S1C' C2C' -60.5(9) . . . . ? S1C Cd3 S1C' C2C' 104.3(15) . . . . ? S2C Cd3 S1C' C2C' -114.6(8) . . . . ? O4C Cd3 S1C' C3C' -94.7(10) . . . . ? N1C Cd3 S1C' C3C' 109.7(10) . . . . ? O1C Cd3 S1C' C3C' 169.3(9) . . . . ? O2C Cd3 S1C' C3C' -168.6(10) . . . . ? S3C Cd3 S1C' C3C' 44.0(10) . . . . ? S1C Cd3 S1C' C3C' -151.2(16) . . . . ? S2C Cd3 S1C' C3C' -10.0(9) . . . . ? O4C Cd3 S2C C5C -118.5(4) . . . . ? N1C Cd3 S2C C5C 77.3(4) . . . . ? O1C Cd3 S2C C5C -37.9(5) . . . . ? O2C Cd3 S2C C5C -172.9(4) . . . . ? S3C Cd3 S2C C5C 1.0(3) . . . . ? S1C Cd3 S2C C5C 149.5(3) . . . . ? S1C' Cd3 S2C C5C 141.0(4) . . . . ? O4C Cd3 S2C C4C' 147.5(8) . . . . ? N1C Cd3 S2C C4C' -16.6(8) . . . . ? O1C Cd3 S2C C4C' -131.8(9) . . . . ? O2C Cd3 S2C C4C' 93.2(8) . . . . ? S3C Cd3 S2C C4C' -92.9(8) . . . . ? S1C Cd3 S2C C4C' 55.6(8) . . . . ? S1C' Cd3 S2C C4C' 47.1(8) . . . . ? O4C Cd3 S2C C4C 135.0(4) . . . . ? N1C Cd3 S2C C4C -29.2(4) . . . . ? O1C Cd3 S2C C4C -144.4(5) . . . . ? O2C Cd3 S2C C4C 80.6(5) . . . . ? S3C Cd3 S2C C4C -105.5(3) . . . . ? S1C Cd3 S2C C4C 43.0(3) . . . . ? S1C' Cd3 S2C C4C 34.5(4) . . . . ? Cd3 O1C N2C O3C 175.3(7) . . . . ? Cd3 O1C N2C O2C -7.2(8) . . . . ? O3C N2C O2C Cd3 -175.5(7) . . . . ? O1C N2C O2C Cd3 7.1(7) . . . . ? O4C Cd3 O2C N2C 95.9(5) . . . . ? N1C Cd3 O2C N2C -89.4(5) . . . . ? O1C Cd3 O2C N2C -4.1(4) . . . . ? S3C Cd3 O2C N2C -18.5(6) . . . . ? S1C Cd3 O2C N2C -169.0(5) . . . . ? S2C Cd3 O2C N2C 153.6(4) . . . . ? S1C' Cd3 O2C N2C -165.0(5) . . . . ? N1C C1C C2C S1C -52.7(13) . . . . ? C2C' C1C C2C S1C 62.9(10) . . . . ? C3C S1C C2C C1C -61.6(10) . . . . ? Cd3 S1C C2C C1C 42.5(9) . . . . ? N1C C1C C2C' S1C' 38(2) . . . . ? C2C C1C C2C' S1C' -59.4(12) . . . . ? C3C' S1C' C2C' C1C -127.8(16) . . . . ? Cd3 S1C' C2C' C1C -21.1(17) . . . . ? O4C Cd3 S3C C7C -152.9(3) . . . . ? N1C Cd3 S3C C7C 11.6(3) . . . . ? O1C Cd3 S3C C7C -71.2(3) . . . . ? O2C Cd3 S3C C7C -60.0(4) . . . . ? S1C Cd3 S3C C7C 69.6(3) . . . . ? S2C Cd3 S3C C7C 124.0(3) . . . . ? S1C' Cd3 S3C C7C 75.1(4) . . . . ? O4C Cd3 S3C C6C 104.5(4) . . . . ? N1C Cd3 S3C C6C -91.0(4) . . . . ? O1C Cd3 S3C C6C -173.8(3) . . . . ? O2C Cd3 S3C C6C -162.6(4) . . . . ? S1C Cd3 S3C C6C -33.0(4) . . . . ? S2C Cd3 S3C C6C 21.4(3) . . . . ? S1C' Cd3 S3C C6C -27.5(4) . . . . ? C2C S1C C3C C4C 92.2(10) . . . . ? Cd3 S1C C3C C4C -5.2(10) . . . . ? C2C' S1C' C3C' C4C' 66.5(19) . . . . ? Cd3 S1C' C3C' C4C' -36.4(19) . . . . ? O5C N3C O4C Cd3 11.8(10) . . . . ? O6C N3C O4C Cd3 -175.8(7) . . . . ? N1C Cd3 O4C N3C -163.7(5) . . . . ? O1C Cd3 O4C N3C -101.3(6) . . . . ? O2C Cd3 O4C N3C -150.8(7) . . . . ? S3C Cd3 O4C N3C -23.4(7) . . . . ? S1C Cd3 O4C N3C 131.6(6) . . . . ? S2C Cd3 O4C N3C 54.6(6) . . . . ? S1C' Cd3 O4C N3C 120.5(6) . . . . ? S1C C3C C4C S2C 52.2(11) . . . . ? C5C S2C C4C C3C -169.1(7) . . . . ? C4C' S2C C4C C3C 155(4) . . . . ? Cd3 S2C C4C C3C -65.9(7) . . . . ? S1C' C3C' C4C' S2C 71(2) . . . . ? C5C S2C C4C' C3C' -179.6(17) . . . . ? C4C S2C C4C' C3C' -34(2) . . . . ? Cd3 S2C C4C' C3C' -77.1(17) . . . . ? C4C' S2C C5C C6C 75.1(13) . . . . ? C4C S2C C5C C6C 64.2(8) . . . . ? Cd3 S2C C5C C6C -32.1(7) . . . . ? S2C C5C C6C S3C 58.1(9) . . . . ? C7C S3C C6C C5C -144.5(6) . . . . ? Cd3 S3C C6C C5C -48.0(6) . . . . ? C6C S3C C7C C8C 64.3(7) . . . . ? Cd3 S3C C7C C8C -39.1(6) . . . . ? C1C N1C C8C C7C -177.1(7) . . . . ? Cd3 N1C C8C C7C -42.8(7) . . . . ? S3C C7C C8C N1C 59.5(8) . . . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 2.09 _refine_diff_density_min -0.61 _refine_diff_density_rms 0.13 data_CDSONO_complex_3 _database_code_depnum_ccdc_archive 'CCDC 225830' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H21 Cd N3 O8 S2' _chemical_formula_sum 'C10 H21 Cd N3 O8 S2' _chemical_formula_weight 487.82 _chemical_absolute_configuration ad 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 Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 10.2949(7) _cell_length_b 12.8171(8) _cell_length_c 12.8662(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1697.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4580 _cell_measurement_theta_min 2.535 _cell_measurement_theta_max 28.435 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.37 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.909 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 984 _exptl_absorpt_coefficient_mu 1.576 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.608 _exptl_absorpt_correction_T_max 0.704 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 10625 _diffrn_reflns_av_R_equivalents 0.016 _diffrn_reflns_av_sigmaI/netI 0.014 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 28.53 _reflns_number_total 3959 _reflns_number_gt 3903 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL; PLATON (Spek, 2003)' _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^)+(0.025P)^2^+0.222P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary 'difference Fourier' _atom_sites_solution_hydrogens 'geometrically placed' _refine_ls_hydrogen_treatment 'riding on parent atom' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.005(14) _refine_ls_number_reflns 3959 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0156 _refine_ls_R_factor_gt 0.0153 _refine_ls_wR_factor_ref 0.0397 _refine_ls_wR_factor_gt 0.0395 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.003 _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 Cd Cd 0.149128(11) -0.005659(9) 0.444487(9) 0.01856(4) Uani 1 1 d . . . N1 N 0.09159(15) 0.10634(12) 0.57842(12) 0.0217(3) Uani 1 1 d . . . H1 H 0.1630 0.1103 0.6226 0.026 Uiso 1 1 calc R . . C1 C 0.06696(18) 0.21349(14) 0.54079(15) 0.0231(4) Uani 1 1 d . . . H1A H 0.0415 0.2584 0.6000 0.028 Uiso 1 1 calc R . . H1B H -0.0058 0.2126 0.4905 0.028 Uiso 1 1 calc R . . C2 C 0.18675(18) 0.25837(14) 0.48910(16) 0.0226(4) Uani 1 1 d . . . H2A H 0.2583 0.2594 0.5405 0.027 Uiso 1 1 calc R . . H2B H 0.1684 0.3315 0.4692 0.027 Uiso 1 1 calc R . . S1 S 0.24154(4) 0.18810(3) 0.37429(4) 0.02152(9) Uani 1 1 d . . . C3 C 0.11947(19) 0.22843(14) 0.27983(15) 0.0254(4) Uani 1 1 d . . . H3A H 0.0572 0.2764 0.3137 0.030 Uiso 1 1 calc R . . H3B H 0.1624 0.2669 0.2226 0.030 Uiso 1 1 calc R . . C4 C 0.0464(2) 0.13664(14) 0.23537(14) 0.0245(4) Uani 1 1 d . . . H4A H -0.0186 0.1609 0.1841 0.029 Uiso 1 1 calc R . . H4B H 0.1073 0.0886 0.1999 0.029 Uiso 1 1 calc R . . O1 O -0.01703(13) 0.08384(10) 0.31992(10) 0.0234(3) Uani 1 1 d . . . C5 C -0.11583(17) 0.01531(15) 0.28321(15) 0.0254(4) Uani 1 1 d . . . H5A H -0.0776 -0.0392 0.2381 0.031 Uiso 1 1 calc R . . H5B H -0.1810 0.0546 0.2423 0.031 Uiso 1 1 calc R . . C6 C -0.17848(17) -0.03342(15) 0.37649(17) 0.0262(4) Uani 1 1 d . . . H6A H -0.2159 0.0212 0.4219 0.031 Uiso 1 1 calc R . . H6B H -0.2492 -0.0809 0.3546 0.031 Uiso 1 1 calc R . . O2 O -0.08044(12) -0.09039(10) 0.43130(10) 0.0244(3) Uani 1 1 d . . . C7 C -0.13511(19) -0.15388(15) 0.51180(16) 0.0285(4) Uani 1 1 d . . . H7A H -0.1965 -0.2047 0.4810 0.034 Uiso 1 1 calc R . . H7B H -0.1839 -0.1094 0.5611 0.034 Uiso 1 1 calc R . . C8 C -0.0294(2) -0.21131(15) 0.56904(16) 0.0279(4) Uani 1 1 d . . . H8A H 0.0072 -0.2650 0.5221 0.034 Uiso 1 1 calc R . . H8B H -0.0689 -0.2481 0.6289 0.034 Uiso 1 1 calc R . . S2 S 0.10266(5) -0.13087(4) 0.61664(4) 0.02420(10) Uani 1 1 d . . . C9 C 0.0203(2) -0.03492(15) 0.69732(15) 0.0282(4) Uani 1 1 d . . . H9A H -0.0594 -0.0670 0.7261 0.034 Uiso 1 1 calc R . . H9B H 0.0775 -0.0169 0.7565 0.034 Uiso 1 1 calc R . . C10 C -0.01712(19) 0.06542(15) 0.64098(15) 0.0261(4) Uani 1 1 d . . . H10A H -0.0923 0.0516 0.5950 0.031 Uiso 1 1 calc R . . H10B H -0.0436 0.1186 0.6926 0.031 Uiso 1 1 calc R . . N2 N 0.20647(15) -0.16934(12) 0.29824(12) 0.0220(3) Uani 1 1 d . . . O3 O 0.20331(16) -0.07241(11) 0.27747(11) 0.0320(3) Uani 1 1 d . . . O4 O 0.16823(14) -0.19830(11) 0.38556(11) 0.0300(3) Uani 1 1 d . . . O5 O 0.24802(15) -0.23229(11) 0.23312(11) 0.0316(3) Uani 1 1 d . . . N3 N 0.44551(14) 0.00884(13) 0.50889(11) 0.0227(3) Uani 1 1 d . . . O6 O 0.36680(13) -0.05266(10) 0.46290(12) 0.0316(3) Uani 1 1 d . . . O7 O 0.56295(13) -0.01341(13) 0.50943(13) 0.0391(4) Uani 1 1 d . . . O8 O 0.40367(14) 0.08795(10) 0.55260(12) 0.0302(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 Cd 0.01855(6) 0.01720(6) 0.01992(6) -0.00018(5) 0.00142(4) 0.00054(5) N1 0.0186(7) 0.0233(8) 0.0233(8) -0.0007(6) -0.0004(6) -0.0005(6) C1 0.0207(9) 0.0214(8) 0.0272(10) -0.0028(7) 0.0016(8) 0.0031(6) C2 0.0230(9) 0.0179(8) 0.0270(9) -0.0039(7) -0.0002(8) -0.0004(7) S1 0.0199(2) 0.0200(2) 0.0246(2) -0.00047(17) 0.00051(19) -0.00085(17) C3 0.0283(10) 0.0218(9) 0.0261(9) 0.0057(7) -0.0024(8) 0.0015(7) C4 0.0290(10) 0.0225(9) 0.0221(9) 0.0037(7) -0.0031(8) 0.0030(7) O1 0.0229(7) 0.0239(6) 0.0235(7) 0.0013(5) -0.0039(5) -0.0029(5) C5 0.0216(8) 0.0228(9) 0.0319(9) -0.0022(8) -0.0095(7) 0.0017(7) C6 0.0163(8) 0.0279(9) 0.0344(10) -0.0041(8) -0.0029(8) 0.0000(7) O2 0.0188(6) 0.0279(7) 0.0266(7) 0.0045(5) 0.0013(5) -0.0037(5) C7 0.0267(10) 0.0301(10) 0.0288(9) 0.0013(8) 0.0032(8) -0.0125(8) C8 0.0335(11) 0.0230(9) 0.0273(10) 0.0022(8) 0.0030(8) -0.0093(8) S2 0.0237(2) 0.0240(2) 0.0249(2) 0.00291(18) 0.00111(19) -0.00072(17) C9 0.0311(10) 0.0321(10) 0.0213(9) -0.0004(7) 0.0056(8) -0.0037(8) C10 0.0243(10) 0.0271(10) 0.0268(10) -0.0033(8) 0.0069(8) -0.0001(7) N2 0.0192(7) 0.0247(8) 0.0220(8) -0.0027(6) -0.0034(6) 0.0005(6) O3 0.0446(9) 0.0214(7) 0.0299(7) -0.0003(6) -0.0083(7) 0.0045(6) O4 0.0274(7) 0.0397(8) 0.0227(7) -0.0013(6) 0.0038(6) -0.0042(6) O5 0.0413(8) 0.0260(7) 0.0274(7) -0.0047(6) 0.0070(7) 0.0033(6) N3 0.0197(7) 0.0228(7) 0.0256(7) 0.0036(7) 0.0022(6) -0.0023(7) O6 0.0222(7) 0.0242(7) 0.0483(9) -0.0063(6) -0.0048(7) 0.0006(5) O7 0.0158(6) 0.0419(9) 0.0597(10) -0.0044(8) 0.0019(6) 0.0022(6) O8 0.0298(7) 0.0267(7) 0.0341(7) -0.0056(7) -0.0001(6) 0.0029(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd N1 2.3197(15) . ? Cd O6 2.3325(13) . ? Cd O3 2.3792(15) . ? Cd O4 2.5904(15) . ? Cd O2 2.6065(12) . ? Cd O1 2.6097(13) . ? Cd S2 2.7768(5) . ? Cd S1 2.8086(5) . ? N1 C10 1.475(2) . ? N1 C1 1.478(2) . ? C1 C2 1.515(3) . ? C2 S1 1.820(2) . ? S1 C3 1.823(2) . ? C3 C4 1.509(3) . ? C4 O1 1.438(2) . ? O1 C5 1.424(2) . ? C5 C6 1.499(3) . ? C6 O2 1.432(2) . ? O2 C7 1.432(2) . ? C7 C8 1.506(3) . ? C8 S2 1.8131(19) . ? S2 C9 1.819(2) . ? C9 C10 1.526(3) . ? N2 O5 1.239(2) . ? N2 O4 1.247(2) . ? N2 O3 1.271(2) . ? N3 O8 1.237(2) . ? N3 O7 1.242(2) . ? N3 O6 1.276(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cd O6 109.25(5) . . ? N1 Cd O3 162.42(5) . . ? O6 Cd O3 76.92(5) . . ? N1 Cd O4 145.76(5) . . ? O6 Cd O4 73.18(5) . . ? O3 Cd O4 51.33(4) . . ? N1 Cd O2 94.28(5) . . ? O6 Cd O2 140.37(4) . . ? O3 Cd O2 90.23(5) . . ? O4 Cd O2 69.67(4) . . ? N1 Cd O1 90.96(5) . . ? O6 Cd O1 143.67(5) . . ? O3 Cd O1 75.94(4) . . ? O4 Cd O1 106.80(4) . . ? O2 Cd O1 63.18(4) . . ? N1 Cd S2 73.81(4) . . ? O6 Cd S2 86.29(4) . . ? O3 Cd S2 123.57(3) . . ? O4 Cd S2 72.28(3) . . ? O2 Cd S2 69.81(3) . . ? O1 Cd S2 129.12(3) . . ? N1 Cd S1 77.18(4) . . ? O6 Cd S1 86.31(4) . . ? O3 Cd S1 87.02(4) . . ? O4 Cd S1 136.30(3) . . ? O2 Cd S1 130.89(3) . . ? O1 Cd S1 68.65(3) . . ? S2 Cd S1 145.681(15) . . ? C10 N1 C1 112.27(14) . . ? C10 N1 Cd 112.28(11) . . ? C1 N1 Cd 112.05(11) . . ? N1 C1 C2 110.92(15) . . ? C1 C2 S1 114.89(13) . . ? C2 S1 C3 100.79(9) . . ? C2 S1 Cd 94.10(6) . . ? C3 S1 Cd 103.39(6) . . ? C4 C3 S1 112.03(13) . . ? O1 C4 C3 107.86(15) . . ? C5 O1 C4 111.33(14) . . ? C5 O1 Cd 113.62(10) . . ? C4 O1 Cd 111.93(10) . . ? O1 C5 C6 107.38(15) . . ? O2 C6 C5 107.68(14) . . ? C6 O2 C7 111.65(14) . . ? C6 O2 Cd 117.31(10) . . ? C7 O2 Cd 123.09(11) . . ? O2 C7 C8 110.33(15) . . ? C7 C8 S2 115.41(13) . . ? C8 S2 C9 103.15(10) . . ? C8 S2 Cd 100.86(7) . . ? C9 S2 Cd 98.32(6) . . ? C10 C9 S2 114.61(14) . . ? N1 C10 C9 111.56(16) . . ? O5 N2 O4 121.62(16) . . ? O5 N2 O3 120.20(16) . . ? O4 N2 O3 118.18(16) . . ? N2 O3 Cd 99.65(11) . . ? N2 O4 Cd 90.23(11) . . ? O8 N3 O7 121.64(16) . . ? O8 N3 O6 119.74(14) . . ? O7 N3 O6 118.62(16) . . ? N3 O6 Cd 119.85(11) . . ? 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 O6 Cd N1 C10 -121.52(12) . . . . ? O3 Cd N1 C10 130.51(18) . . . . ? O4 Cd N1 C10 -33.34(17) . . . . ? O2 Cd N1 C10 26.06(13) . . . . ? O1 Cd N1 C10 89.24(12) . . . . ? S2 Cd N1 C10 -41.48(12) . . . . ? S1 Cd N1 C10 157.07(13) . . . . ? O6 Cd N1 C1 111.05(12) . . . . ? O3 Cd N1 C1 3.1(2) . . . . ? O4 Cd N1 C1 -160.77(10) . . . . ? O2 Cd N1 C1 -101.37(12) . . . . ? O1 Cd N1 C1 -38.19(12) . . . . ? S2 Cd N1 C1 -168.91(12) . . . . ? S1 Cd N1 C1 29.64(11) . . . . ? C10 N1 C1 C2 172.58(16) . . . . ? Cd N1 C1 C2 -59.98(17) . . . . ? N1 C1 C2 S1 62.04(19) . . . . ? C1 C2 S1 C3 74.40(16) . . . . ? C1 C2 S1 Cd -30.08(14) . . . . ? N1 Cd S1 C2 0.25(7) . . . . ? O6 Cd S1 C2 -110.45(7) . . . . ? O3 Cd S1 C2 172.48(7) . . . . ? O4 Cd S1 C2 -171.29(8) . . . . ? O2 Cd S1 C2 84.76(8) . . . . ? O1 Cd S1 C2 96.42(7) . . . . ? S2 Cd S1 C2 -32.55(7) . . . . ? N1 Cd S1 C3 -101.87(8) . . . . ? O6 Cd S1 C3 147.43(8) . . . . ? O3 Cd S1 C3 70.36(8) . . . . ? O4 Cd S1 C3 86.59(8) . . . . ? O2 Cd S1 C3 -17.36(8) . . . . ? O1 Cd S1 C3 -5.70(7) . . . . ? S2 Cd S1 C3 -134.68(7) . . . . ? C2 S1 C3 C4 -121.00(15) . . . . ? Cd S1 C3 C4 -24.09(15) . . . . ? S1 C3 C4 O1 60.12(18) . . . . ? C3 C4 O1 C5 163.65(15) . . . . ? C3 C4 O1 Cd -67.97(15) . . . . ? N1 Cd O1 C5 -118.62(12) . . . . ? O6 Cd O1 C5 115.97(12) . . . . ? O3 Cd O1 C5 73.23(12) . . . . ? O4 Cd O1 C5 31.69(12) . . . . ? O2 Cd O1 C5 -24.31(11) . . . . ? S2 Cd O1 C5 -48.85(12) . . . . ? S1 Cd O1 C5 165.55(12) . . . . ? N1 Cd O1 C4 114.21(11) . . . . ? O6 Cd O1 C4 -11.20(14) . . . . ? O3 Cd O1 C4 -53.94(11) . . . . ? O4 Cd O1 C4 -95.48(11) . . . . ? O2 Cd O1 C4 -151.48(12) . . . . ? S2 Cd O1 C4 -176.02(9) . . . . ? S1 Cd O1 C4 38.38(10) . . . . ? C4 O1 C5 C6 -178.41(15) . . . . ? Cd O1 C5 C6 54.12(15) . . . . ? O1 C5 C6 O2 -60.84(18) . . . . ? C5 C6 O2 C7 -170.25(15) . . . . ? C5 C6 O2 Cd 39.74(17) . . . . ? N1 Cd O2 C6 79.33(13) . . . . ? O6 Cd O2 C6 -153.17(12) . . . . ? O3 Cd O2 C6 -83.66(12) . . . . ? O4 Cd O2 C6 -131.76(13) . . . . ? O1 Cd O2 C6 -9.58(12) . . . . ? S2 Cd O2 C6 150.34(13) . . . . ? S1 Cd O2 C6 2.60(14) . . . . ? N1 Cd O2 C7 -66.99(14) . . . . ? O6 Cd O2 C7 60.51(16) . . . . ? O3 Cd O2 C7 130.01(13) . . . . ? O4 Cd O2 C7 81.92(13) . . . . ? O1 Cd O2 C7 -155.90(14) . . . . ? S2 Cd O2 C7 4.02(13) . . . . ? S1 Cd O2 C7 -143.73(12) . . . . ? C6 O2 C7 C8 -179.06(15) . . . . ? Cd O2 C7 C8 -31.1(2) . . . . ? O2 C7 C8 S2 51.9(2) . . . . ? C7 C8 S2 C9 56.46(16) . . . . ? C7 C8 S2 Cd -44.85(15) . . . . ? N1 Cd S2 C8 119.46(8) . . . . ? O6 Cd S2 C8 -129.26(8) . . . . ? O3 Cd S2 C8 -57.64(8) . . . . ? O4 Cd S2 C8 -55.74(8) . . . . ? O2 Cd S2 C8 18.53(7) . . . . ? O1 Cd S2 C8 41.80(8) . . . . ? S1 Cd S2 C8 152.84(7) . . . . ? N1 Cd S2 C9 14.26(8) . . . . ? O6 Cd S2 C9 125.54(8) . . . . ? O3 Cd S2 C9 -162.84(8) . . . . ? O4 Cd S2 C9 -160.94(8) . . . . ? O2 Cd S2 C9 -86.67(8) . . . . ? O1 Cd S2 C9 -63.41(8) . . . . ? S1 Cd S2 C9 47.63(8) . . . . ? C8 S2 C9 C10 -92.25(16) . . . . ? Cd S2 C9 C10 11.03(15) . . . . ? C1 N1 C10 C9 -168.33(16) . . . . ? Cd N1 C10 C9 64.35(18) . . . . ? S2 C9 C10 N1 -46.9(2) . . . . ? O5 N2 O3 Cd -170.89(14) . . . . ? O4 N2 O3 Cd 8.33(18) . . . . ? N1 Cd O3 N2 -172.95(15) . . . . ? O6 Cd O3 N2 74.27(11) . . . . ? O4 Cd O3 N2 -4.52(10) . . . . ? O2 Cd O3 N2 -67.89(11) . . . . ? O1 Cd O3 N2 -130.11(12) . . . . ? S2 Cd O3 N2 -2.20(13) . . . . ? S1 Cd O3 N2 161.16(11) . . . . ? O5 N2 O4 Cd 171.67(16) . . . . ? O3 N2 O4 Cd -7.54(16) . . . . ? N1 Cd O4 N2 178.36(10) . . . . ? O6 Cd O4 N2 -81.96(10) . . . . ? O3 Cd O4 N2 4.54(10) . . . . ? O2 Cd O4 N2 112.12(11) . . . . ? O1 Cd O4 N2 60.02(11) . . . . ? S2 Cd O4 N2 -173.43(11) . . . . ? S1 Cd O4 N2 -16.41(12) . . . . ? O8 N3 O6 Cd 7.3(2) . . . . ? O7 N3 O6 Cd -173.53(13) . . . . ? N1 Cd O6 N3 -27.13(14) . . . . ? O3 Cd O6 N3 135.71(14) . . . . ? O4 Cd O6 N3 -171.15(14) . . . . ? O2 Cd O6 N3 -150.20(11) . . . . ? O1 Cd O6 N3 93.19(15) . . . . ? S2 Cd O6 N3 -98.55(13) . . . . ? S1 Cd O6 N3 47.92(13) . . . . ? _diffrn_measured_fraction_theta_max 0.949 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.43 _refine_diff_density_min -0.27 _refine_diff_density_rms 0.05 data_CDSNON_complex_4 _database_code_depnum_ccdc_archive 'CCDC 225831' _refine_special_details ; Complete disorder of one macrocycle (coordinated to Cd2) was modelled over two sites with occupancy 0.65:0.35 and one common C atom. Distance restraints were applied and disordered atoms were modelled isotropically. The largest two peaks of residual electron density suggest similar disorder - but to much lesser extent - in the macrocycle coordinated to Cd1: these peaks have heights of 1.9 and 1.6 electrons/A**3 but it is not possible to locate enough of the rest of the macrocyle to apply a sensible disorder model. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C10 H22 Cd N3 O5 S), 0.5(Cd2 Cl2 H4 N4 O14), 2.5(C2 H3 N)' _chemical_formula_sum 'C25 H49.50 Cd3 Cl N11.50 O20 S2' _chemical_formula_weight 1268.03 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.4869(5) _cell_length_b 30.608(2) _cell_length_c 16.5411(9) _cell_angle_alpha 90.00 _cell_angle_beta 94.385(2) _cell_angle_gamma 90.00 _cell_volume 4789.0(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6416 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 27.75 _exptl_crystal_description tablet _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.759 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2532 _exptl_absorpt_coefficient_mu 1.543 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.856 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART1000 CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 21654 _diffrn_reflns_av_R_equivalents 0.032 _diffrn_reflns_av_sigmaI/netI 0.050 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 27.50 _reflns_number_total 11235 _reflns_number_gt 8131 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART version 5.054 (Bruker, 1998)' _computing_cell_refinement 'Bruker SAINT version 6.02a (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'SHELXL-97; PLATON (Spek, 2003)' _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^)+(0.0566P)^2^+20.205P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'direct methods' _atom_sites_solution_secondary 'difference Fourier' _atom_sites_solution_hydrogens 'geometrically placed, H2O, MeCN from delta-F' _refine_ls_hydrogen_treatment 'riding model, MeCN rigid rotating group, H2O refined with restraints' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10720 _refine_ls_number_parameters 562 _refine_ls_number_restraints 118 _refine_ls_R_factor_all 0.0743 _refine_ls_R_factor_gt 0.0521 _refine_ls_wR_factor_ref 0.133 _refine_ls_wR_factor_gt 0.122 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.027 _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 0.18996(4) 0.159327(12) 0.23209(2) 0.02514(10) Uani 1 1 d . . . S1 S 0.0783(2) 0.09221(6) 0.31622(11) 0.0494(4) Uani 1 1 d . . . O1 O 0.1635(5) 0.23625(11) 0.1786(2) 0.0354(10) Uani 1 1 d . . . N1 N 0.3307(6) 0.10152(18) 0.1996(3) 0.0429(13) Uani 1 1 d . . . H1C H 0.2941 0.0903 0.1501 0.052 Uiso 1 1 calc R . . C1 C 0.3324(9) 0.0669(3) 0.2578(5) 0.059(2) Uani 1 1 d . . . H1A H 0.3777 0.0775 0.3101 0.071 Uiso 1 1 calc R . . H1B H 0.3902 0.0425 0.2392 0.071 Uiso 1 1 calc R . . N2 N -0.0401(5) 0.16349(15) 0.1812(3) 0.0313(10) Uani 1 1 d . . . H2C H -0.0475 0.1483 0.1324 0.038 Uiso 1 1 calc R . . O2 O 0.3902(5) 0.18840(14) 0.1588(3) 0.0442(11) Uani 1 1 d . . . C2 C 0.1806(9) 0.0497(2) 0.2714(5) 0.0542(19) Uani 1 1 d . . . H2A H 0.1875 0.0239 0.3076 0.065 Uiso 1 1 calc R . . H2B H 0.1326 0.0406 0.2188 0.065 Uiso 1 1 calc R . . C3 C -0.0880(7) 0.0952(2) 0.2537(4) 0.0385(14) Uani 1 1 d . . . H3A H -0.0776 0.0796 0.2021 0.046 Uiso 1 1 calc R . . H3B H -0.1625 0.0802 0.2820 0.046 Uiso 1 1 calc R . . C4 C -0.1343(6) 0.1422(2) 0.2352(4) 0.0353(13) Uani 1 1 d . . . H4A H -0.2319 0.1423 0.2094 0.042 Uiso 1 1 calc R . . H4B H -0.1341 0.1589 0.2864 0.042 Uiso 1 1 calc R . . C5 C -0.0832(6) 0.2091(2) 0.1636(4) 0.0379(14) Uani 1 1 d . . . H5A H -0.0998 0.2242 0.2149 0.045 Uiso 1 1 calc R . . H5B H -0.1728 0.2093 0.1288 0.045 Uiso 1 1 calc R . . C6 C 0.0304(7) 0.2333(2) 0.1210(4) 0.0400(15) Uani 1 1 d . . . H6A H -0.0031 0.2630 0.1055 0.048 Uiso 1 1 calc R . . H6B H 0.0513 0.2175 0.0711 0.048 Uiso 1 1 calc R . . C7 C 0.2685(9) 0.2549(3) 0.1515(5) 0.057(2) Uani 1 1 d . . . H7A H 0.3303 0.2669 0.1972 0.068 Uiso 1 1 calc R . . H7B H 0.2359 0.2795 0.1160 0.068 Uiso 1 1 calc R . . C8 C 0.3511(7) 0.22278(19) 0.1041(4) 0.0386(14) Uani 1 1 d . . . H8A H 0.2919 0.2115 0.0567 0.046 Uiso 1 1 calc R . . H8B H 0.4361 0.2369 0.0846 0.046 Uiso 1 1 calc R . . C9 C 0.4650(7) 0.1544(2) 0.1270(4) 0.0451(16) Uani 1 1 d . . . H9A H 0.5612 0.1643 0.1164 0.054 Uiso 1 1 calc R . . H9B H 0.4165 0.1444 0.0752 0.054 Uiso 1 1 calc R . . C10 C 0.4740(6) 0.1166(2) 0.1893(4) 0.0346(13) Uani 1 1 d . . . H10A H 0.5316 0.0924 0.1696 0.041 Uiso 1 1 calc R . . H10B H 0.5191 0.1270 0.2418 0.041 Uiso 1 1 calc R . . N1N N 0.2150(6) 0.20122(16) 0.3853(3) 0.0357(11) Uani 1 1 d . . . O1N O 0.3169(5) 0.18811(16) 0.3470(3) 0.0456(11) Uani 1 1 d . . . O2N O 0.2359(6) 0.21872(18) 0.4522(3) 0.0578(14) Uani 1 1 d . . . O3N O 0.0926(5) 0.19617(15) 0.3531(3) 0.0449(11) Uani 1 1 d . . . Cd2 Cd 0.67481(4) 0.337968(13) 0.27763(2) 0.02536(10) Uani 1 1 d . . . S1A S 0.7445(4) 0.41123(9) 0.19009(16) 0.0436(6) Uani 0.65 1 d PD A 1 C1A C 0.4738(10) 0.4202(3) 0.2416(6) 0.039(2) Uiso 0.65 1 d PD A 1 H1AA H 0.3998 0.4407 0.2570 0.046 Uiso 0.65 1 calc PR A 1 H1AB H 0.4391 0.4056 0.1905 0.046 Uiso 0.65 1 calc PR A 1 N1A N 0.4995(7) 0.3875(2) 0.3052(5) 0.0338(17) Uiso 0.65 1 d PD A 1 O1A O 0.7602(7) 0.2667(2) 0.3271(4) 0.0418(17) Uiso 0.65 1 d PD A 1 C2A C 0.6047(10) 0.4448(3) 0.2286(8) 0.056(3) Uiso 0.65 1 d PD A 1 H2AA H 0.6409 0.4582 0.2806 0.068 Uiso 0.65 1 calc PR A 1 H2AB H 0.5813 0.4688 0.1896 0.068 Uiso 0.65 1 calc PR A 1 O2A O 0.5019(7) 0.2995(2) 0.3477(4) 0.0363(15) Uiso 0.65 1 d PD A 1 N2A N 0.9030(8) 0.3495(2) 0.3306(5) 0.0330(18) Uiso 0.65 1 d PD A 1 C3A C 0.9007(11) 0.4202(3) 0.2594(6) 0.046(3) Uiso 0.65 1 d PD A 1 H3AA H 0.9646 0.4410 0.2345 0.055 Uiso 0.65 1 calc PR A 1 H3AB H 0.8716 0.4336 0.3101 0.055 Uiso 0.65 1 calc PR A 1 C4A C 0.9784(11) 0.3791(3) 0.2794(7) 0.052(3) Uiso 0.65 1 d PD A 1 H4AA H 0.9962 0.3639 0.2284 0.062 Uiso 0.65 1 calc PR A 1 H4AB H 1.0713 0.3864 0.3076 0.062 Uiso 0.65 1 calc PR A 1 C5A C 0.9768(10) 0.3079(3) 0.3451(7) 0.039(2) Uiso 0.65 1 d PD A 1 H5AA H 1.0629 0.3127 0.3817 0.047 Uiso 0.65 1 calc PR A 1 H5AB H 1.0061 0.2962 0.2932 0.047 Uiso 0.65 1 calc PR A 1 C6A C 0.8841(10) 0.2760(3) 0.3820(6) 0.043(2) Uiso 0.65 1 d PD A 1 H6AA H 0.9371 0.2486 0.3942 0.052 Uiso 0.65 1 calc PR A 1 H6AB H 0.8538 0.2878 0.4336 0.052 Uiso 0.65 1 calc PR A 1 C7A C 0.6424(7) 0.2405(2) 0.3557(5) 0.060(2) Uiso 0.65 1 d PD A 1 H7AA H 0.5829 0.2293 0.3084 0.071 Uiso 0.65 1 calc PR A 1 H7AB H 0.6809 0.2152 0.3874 0.071 Uiso 0.65 1 calc PR A 1 C8A C 0.5558(11) 0.2671(3) 0.4062(5) 0.045(2) Uiso 0.65 1 d PD A 1 H8AA H 0.4785 0.2499 0.4275 0.054 Uiso 0.65 1 calc PR A 1 H8AB H 0.6133 0.2807 0.4520 0.054 Uiso 0.65 1 calc PR A 1 C9A C 0.4011(11) 0.3287(3) 0.3816(6) 0.041(3) Uiso 0.65 1 d PD A 1 H9AA H 0.4413 0.3407 0.4340 0.049 Uiso 0.65 1 calc PR A 1 H9AB H 0.3132 0.3127 0.3912 0.049 Uiso 0.65 1 calc PR A 1 C10A C 0.3704(9) 0.3645(3) 0.3226(6) 0.045(2) Uiso 0.65 1 d PD A 1 H10C H 0.3250 0.3522 0.2717 0.054 Uiso 0.65 1 calc PR A 1 H10D H 0.3036 0.3853 0.3448 0.054 Uiso 0.65 1 calc PR A 1 S1B S 0.6509(8) 0.41605(18) 0.1960(3) 0.0514(14) Uani 0.35 1 d PD A 2 C1B C 0.416(2) 0.4044(6) 0.2831(15) 0.065(6) Uiso 0.35 1 d PD A 2 H1BA H 0.3439 0.4189 0.3144 0.078 Uiso 0.35 1 calc PR A 2 H1BB H 0.3661 0.3915 0.2339 0.078 Uiso 0.35 1 calc PR A 2 N1B N 0.4826(16) 0.3694(5) 0.3322(10) 0.045(4) Uiso 0.35 1 d PD A 2 O1B O 0.8193(10) 0.2788(3) 0.3346(6) 0.022(2) Uiso 0.35 1 d PD A 2 C2B C 0.5170(19) 0.4374(6) 0.2586(12) 0.050(5) Uiso 0.35 1 d PD A 2 H2BA H 0.5648 0.4507 0.3080 0.059 Uiso 0.35 1 calc PR A 2 H2BB H 0.4642 0.4609 0.2283 0.059 Uiso 0.35 1 calc PR A 2 O2B O 0.5405(12) 0.2765(4) 0.3356(7) 0.043(3) Uiso 0.35 1 d PD A 2 N2B N 0.8897(11) 0.3668(4) 0.3115(7) 0.017(2) Uiso 0.35 1 d PD A 2 C3B C 0.8209(14) 0.4343(5) 0.2448(11) 0.040(4) Uiso 0.35 1 d PD A 2 H3BA H 0.8566 0.4583 0.2119 0.048 Uiso 0.35 1 calc PR A 2 H3BB H 0.8037 0.4467 0.2985 0.048 Uiso 0.35 1 calc PR A 2 C4B C 0.9335(17) 0.4009(5) 0.2566(10) 0.037(4) Uiso 0.35 1 d PD A 2 H4BA H 0.9519 0.3878 0.2037 0.045 Uiso 0.35 1 calc PR A 2 H4BB H 1.0220 0.4147 0.2797 0.045 Uiso 0.35 1 calc PR A 2 C5B C 0.9943(15) 0.3316(5) 0.3169(10) 0.035(4) Uiso 0.35 1 d PD A 2 H5BA H 1.0866 0.3436 0.3385 0.042 Uiso 0.35 1 calc PR A 2 H5BB H 1.0059 0.3202 0.2618 0.042 Uiso 0.35 1 calc PR A 2 C6B C 0.9546(13) 0.2953(4) 0.3693(8) 0.021(3) Uiso 0.35 1 d PD A 2 H6BA H 1.0270 0.2720 0.3705 0.025 Uiso 0.35 1 calc PR A 2 H6BB H 0.9461 0.3057 0.4253 0.025 Uiso 0.35 1 calc PR A 2 C7B C 0.7756(15) 0.2517(6) 0.4007(8) 0.054(5) Uiso 0.35 1 d PD A 2 H7BA H 0.8379 0.2261 0.4123 0.065 Uiso 0.35 1 calc PR A 2 H7BB H 0.7632 0.2683 0.4510 0.065 Uiso 0.35 1 calc PR A 2 C8B C 0.6424(7) 0.2405(2) 0.3557(5) 0.060(2) Uiso 0.35 1 d PD A 2 H8BA H 0.5941 0.2184 0.3874 0.071 Uiso 0.35 1 calc PR A 2 H8BB H 0.6646 0.2265 0.3043 0.071 Uiso 0.35 1 calc PR A 2 C9B C 0.450(2) 0.2987(6) 0.3910(11) 0.053(5) Uiso 0.35 1 d PD A 2 H9BA H 0.5086 0.3074 0.4405 0.063 Uiso 0.35 1 calc PR A 2 H9BB H 0.3777 0.2778 0.4073 0.063 Uiso 0.35 1 calc PR A 2 C10B C 0.3786(19) 0.3378(6) 0.3553(15) 0.051(6) Uiso 0.35 1 d PD A 2 H10E H 0.3166 0.3293 0.3070 0.062 Uiso 0.35 1 calc PR A 2 H10F H 0.3189 0.3511 0.3953 0.062 Uiso 0.35 1 calc PR A 2 N2N N 0.6821(6) 0.29822(15) 0.1230(3) 0.0342(11) Uani 1 1 d . . . O4N O 0.5751(5) 0.30370(17) 0.1632(3) 0.0477(12) Uani 1 1 d . A . O5N O 0.6702(6) 0.28088(17) 0.0558(3) 0.0565(14) Uani 1 1 d . A . O6N O 0.7973(5) 0.31014(16) 0.1558(3) 0.0450(11) Uani 1 1 d . A . Cd3 Cd 0.31851(4) -0.022989(13) -0.02978(3) 0.02966(11) Uani 1 1 d . . . Cl1 Cl 0.42452(15) 0.05271(5) 0.00281(11) 0.0429(4) Uani 1 1 d . . . O3 O 0.1538(5) -0.01108(14) 0.0603(3) 0.0377(10) Uani 1 1 d D . . H1W H 0.089(6) -0.0297(19) 0.055(5) 0.057 Uiso 1 1 d D . . H2W H 0.136(8) 0.0156(7) 0.065(5) 0.057 Uiso 1 1 d D . . N3N N 0.2587(5) -0.11553(17) -0.0054(3) 0.0349(11) Uani 1 1 d . . . O7N O 0.2455(4) -0.09388(12) -0.0701(2) 0.0314(9) Uani 1 1 d . . . O8N O 0.2372(7) -0.15446(16) -0.0057(4) 0.0748(19) Uani 1 1 d . . . O9N O 0.2940(5) -0.09490(19) 0.0589(3) 0.0539(13) Uani 1 1 d . . . N4N N 0.2174(5) -0.00062(15) -0.1875(3) 0.0335(11) Uani 1 1 d . . . O10N O 0.1378(4) -0.00004(15) -0.1300(3) 0.0413(10) Uani 1 1 d . . . O11N O 0.1736(5) 0.01096(16) -0.2557(3) 0.0508(12) Uani 1 1 d . . . O12N O 0.3425(4) -0.01369(14) -0.1720(3) 0.0391(10) Uani 1 1 d . . . N5N N 0.0867(5) 0.10035(16) 0.0188(3) 0.0307(10) Uani 1 1 d . . . O13N O 0.0995(5) 0.07577(15) 0.0801(3) 0.0407(10) Uani 1 1 d . . . O14N O 0.0316(5) 0.08539(14) -0.0465(3) 0.0414(10) Uani 1 1 d . . . O15N O 0.1303(6) 0.13855(15) 0.0235(3) 0.0534(13) Uani 1 1 d . . . N1S N 0.6595(8) 0.1205(3) 0.3943(5) 0.076(2) Uani 1 1 d D . . C2S C 0.5762(8) 0.1242(3) 0.4385(4) 0.0521(18) Uani 1 1 d D . . C3S C 0.4689(9) 0.1276(3) 0.4953(4) 0.066(2) Uani 1 1 d D . . H3S1 H 0.3788 0.1168 0.4701 0.099 Uiso 1 1 calc R . . H3S2 H 0.4584 0.1583 0.5109 0.099 Uiso 1 1 calc R . . H3S3 H 0.4966 0.1102 0.5436 0.099 Uiso 1 1 calc R . . N4S N 0.1852(9) 0.1195(4) 0.6023(6) 0.116(4) Uani 1 1 d D . . C5S C 0.0889(9) 0.1275(3) 0.5616(5) 0.069(2) Uani 1 1 d D . . C6S C -0.0349(9) 0.1388(3) 0.5109(5) 0.071(2) Uani 1 1 d D . . H6S1 H -0.0910 0.1601 0.5390 0.106 Uiso 1 1 calc R . . H6S2 H -0.0915 0.1125 0.4987 0.106 Uiso 1 1 calc R . . H6S3 H -0.0068 0.1516 0.4603 0.106 Uiso 1 1 calc R . . N7S N 0.354(2) 0.0154(7) 0.4412(11) 0.106(6) Uiso 0.50 1 d PD . . C8S C 0.304(2) 0.0052(6) 0.4974(10) 0.072(5) Uiso 0.50 1 d PD . . C9S C 0.271(3) -0.0034(8) 0.5788(11) 0.105(8) Uiso 0.50 1 d PD . . H9S1 H 0.3139 -0.0312 0.5969 0.157 Uiso 0.50 1 calc PR . . H9S2 H 0.1684 -0.0050 0.5809 0.157 Uiso 0.50 1 calc PR . . H9S3 H 0.3088 0.0202 0.6143 0.157 Uiso 0.50 1 calc PR . . 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 0.02137(19) 0.02476(19) 0.0291(2) -0.00269(16) 0.00063(15) 0.00333(15) S1 0.0595(11) 0.0467(10) 0.0436(10) -0.0026(8) 0.0148(8) -0.0071(8) O1 0.065(3) 0.0135(17) 0.025(2) -0.0001(15) -0.011(2) 0.0018(18) N1 0.045(3) 0.043(3) 0.040(3) -0.004(2) 0.002(3) 0.005(2) C1 0.062(5) 0.051(4) 0.061(5) 0.021(4) -0.015(4) 0.004(4) N2 0.026(2) 0.033(3) 0.035(3) -0.004(2) 0.000(2) 0.000(2) O2 0.057(3) 0.034(2) 0.041(3) -0.0005(19) -0.001(2) 0.003(2) C2 0.077(5) 0.031(3) 0.055(5) 0.003(3) 0.006(4) -0.002(3) C3 0.034(3) 0.038(3) 0.045(4) -0.004(3) 0.012(3) -0.008(3) C4 0.026(3) 0.045(3) 0.035(3) -0.010(3) 0.004(2) -0.005(3) C5 0.030(3) 0.039(3) 0.043(4) -0.001(3) -0.003(3) 0.009(3) C6 0.042(4) 0.032(3) 0.045(4) 0.007(3) -0.003(3) 0.008(3) C7 0.071(5) 0.051(4) 0.047(4) -0.009(4) -0.003(4) 0.011(4) C8 0.054(4) 0.031(3) 0.031(3) 0.007(3) 0.009(3) -0.009(3) C9 0.032(3) 0.062(4) 0.042(4) -0.004(3) 0.008(3) 0.009(3) C10 0.021(3) 0.041(3) 0.041(3) -0.004(3) 0.003(2) 0.005(2) N1N 0.041(3) 0.031(3) 0.035(3) -0.008(2) 0.003(2) -0.004(2) O1N 0.035(2) 0.062(3) 0.040(3) -0.014(2) 0.005(2) -0.007(2) O2N 0.060(3) 0.075(4) 0.037(3) -0.025(3) 0.000(2) -0.013(3) O3N 0.041(3) 0.052(3) 0.041(3) -0.017(2) -0.002(2) 0.003(2) Cd2 0.02116(19) 0.0281(2) 0.0268(2) -0.00290(16) 0.00233(15) 0.00107(15) S1A 0.0636(19) 0.0338(13) 0.0339(14) -0.0013(11) 0.0080(14) -0.0107(14) S1B 0.077(4) 0.041(3) 0.034(3) -0.003(2) -0.011(3) 0.020(3) N2N 0.048(3) 0.027(2) 0.028(3) -0.004(2) 0.004(2) 0.004(2) O4N 0.042(3) 0.064(3) 0.038(2) -0.016(2) 0.006(2) -0.012(2) O5N 0.079(4) 0.062(3) 0.028(2) -0.017(2) 0.000(2) 0.006(3) O6N 0.039(3) 0.058(3) 0.039(2) -0.013(2) 0.005(2) 0.003(2) Cd3 0.0266(2) 0.0270(2) 0.0359(2) -0.00160(17) 0.00570(16) -0.00384(16) Cl1 0.0270(7) 0.0342(7) 0.0675(11) -0.0090(7) 0.0031(7) -0.0018(6) O3 0.035(2) 0.041(2) 0.038(2) 0.000(2) 0.0070(19) -0.0067(19) N3N 0.023(2) 0.040(3) 0.042(3) 0.010(2) 0.006(2) 0.002(2) O7N 0.036(2) 0.029(2) 0.028(2) 0.0013(17) -0.0021(17) -0.0020(17) O8N 0.090(4) 0.031(3) 0.109(5) 0.025(3) 0.040(4) 0.004(3) O9N 0.036(3) 0.098(4) 0.027(2) 0.001(3) -0.0012(19) 0.009(3) N4N 0.037(3) 0.021(2) 0.042(3) 0.005(2) 0.005(2) -0.001(2) O10N 0.033(2) 0.045(3) 0.047(3) -0.001(2) 0.012(2) 0.0051(19) O11N 0.058(3) 0.048(3) 0.045(3) 0.014(2) -0.005(2) -0.001(2) O12N 0.032(2) 0.043(2) 0.044(3) 0.008(2) 0.0137(19) 0.0064(19) N5N 0.023(2) 0.033(3) 0.037(3) -0.004(2) 0.002(2) 0.0021(19) O13N 0.039(2) 0.049(3) 0.034(2) 0.003(2) 0.0051(19) 0.008(2) O14N 0.042(2) 0.039(2) 0.041(3) -0.003(2) -0.012(2) -0.0018(19) O15N 0.061(3) 0.029(2) 0.068(3) -0.005(2) -0.005(3) -0.004(2) N1S 0.067(5) 0.102(6) 0.059(5) -0.010(4) 0.011(4) -0.006(4) C2S 0.055(5) 0.061(5) 0.039(4) 0.000(3) -0.005(3) -0.006(4) C3S 0.074(6) 0.085(6) 0.039(4) 0.004(4) 0.009(4) -0.005(5) N4S 0.070(6) 0.189(12) 0.090(7) 0.041(7) 0.009(5) 0.010(7) C5S 0.065(6) 0.085(7) 0.060(6) 0.011(5) 0.024(5) 0.001(5) C6S 0.071(6) 0.092(7) 0.050(5) -0.001(5) 0.013(4) 0.014(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 N1 2.305(5) . y Cd1 N2 2.282(5) . y Cd1 O1 2.521(4) . y Cd1 O2 2.495(5) . y Cd1 O1N 2.343(4) . y Cd1 O3N 2.533(4) . y Cd1 S1 2.7394(18) . y N1 C1 1.430(9) . ? N1 C10 1.458(8) . ? N2 C4 1.462(8) . ? N2 C5 1.477(7) . ? O1 C6 1.525(7) . ? O1 C7 1.261(9) . ? O2 C8 1.419(7) . ? O2 C9 1.386(8) . ? S1 C2 1.815(8) . ? S1 C3 1.821(7) . ? C1 C2 1.566(11) . ? C3 C4 1.529(9) . ? C5 C6 1.525(9) . ? C7 C8 1.514(10) . ? C9 C10 1.547(9) . ? N1N O1N 1.261(7) . ? N1N O2N 1.231(6) . ? N1N O3N 1.250(7) . ? Cd2 N1A 2.321(8) . y Cd2 N2A 2.300(8) . y Cd2 O1A 2.447(7) . y Cd2 O2A 2.390(6) . y Cd2 S1A 2.776(3) . y Cd2 O4N 2.303(4) . y Cd2 O6N 2.549(4) . y N1A C1A 1.459(8) . ? N1A C10A 1.460(8) . ? N2A C4A 1.464(8) . ? N2A C5A 1.462(8) . ? O1A C6A 1.457(7) . ? O1A C7A 1.481(7) . ? O2A C8A 1.450(7) . ? O2A C9A 1.453(7) . ? S1A C2A 1.831(9) . ? S1A C3A 1.824(9) . ? C1A C2A 1.482(8) . ? C3A C4A 1.483(8) . ? C5A C6A 1.478(8) . ? C7A C8A 1.463(8) . ? C9A C10A 1.482(8) . ? Cd2 N1B 2.306(16) . y Cd2 N2B 2.252(11) . y Cd2 O1B 2.418(10) . y Cd2 O2B 2.503(13) . y Cd2 S1B 2.746(5) . y N1B C1B 1.458(9) . ? N1B C10B 1.456(9) . ? N2B C4B 1.465(9) . ? N2B C5B 1.462(9) . ? O1B C6B 1.455(8) . ? O1B C7B 1.459(8) . ? O2B C9B 1.468(8) . ? S1B C2B 1.821(10) . ? S1B C3B 1.835(10) . ? C1B C2B 1.474(9) . ? C3B C4B 1.482(9) . ? C5B C6B 1.476(9) . ? C9B C10B 1.477(9) . ? N2N O5N 1.229(6) . ? N2N O6N 1.237(7) . ? N2N O4N 1.266(7) . ? Cd3 O3 2.269(5) . y Cd3 O7N 2.359(4) . y Cd3 O10N 2.397(5) . y Cd3 O12N 2.398(4) . y Cd3 Cl1 2.5665(15) . y Cd3 Cl1 2.6083(15) 3_655 y Cl1 Cd3 2.6083(15) 3_655 ? N3N O8N 1.209(7) . ? N3N O7N 1.258(6) . ? N3N O9N 1.260(7) . ? N4N O11N 1.224(7) . ? N4N O10N 1.260(6) . ? N4N O12N 1.260(6) . ? N5N O15N 1.241(6) . ? N5N O14N 1.251(6) . ? N5N O13N 1.261(6) . ? N1S C2S 1.122(8) . ? C2S C3S 1.442(9) . ? N4S C5S 1.118(9) . ? C5S C6S 1.433(9) . ? N7S C8S 1.117(10) . ? C8S C9S 1.430(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cd1 N2 120.79(19) . . y N1 Cd1 O1N 101.94(18) . . y N1 Cd1 O1 132.77(18) . . y N1 Cd1 O2 71.59(17) . . y N1 Cd1 O3N 141.16(18) . . y N1 Cd1 S1 78.24(15) . . y N2 Cd1 O1 75.62(16) . . y N2 Cd1 O2 122.91(16) . . y N2 Cd1 O1N 134.09(17) . . y N2 Cd1 O3N 82.54(16) . . y N2 Cd1 S1 80.39(13) . . y O1 Cd1 O2 63.61(15) . . y O1 Cd1 O1N 87.98(15) . . y O1 Cd1 O3N 80.15(15) . . y O1 Cd1 S1 147.85(12) . . y O1N Cd1 O2 84.09(15) . . y O1N Cd1 O3N 52.21(15) . . y O1N Cd1 S1 93.70(13) . . y O2 Cd1 O3N 124.24(15) . . y O2 Cd1 S1 148.52(11) . . y O3N Cd1 S1 75.75(12) . . y C2 S1 C3 105.7(3) . . ? C2 S1 Cd1 95.2(2) . . ? C3 S1 Cd1 91.5(2) . . ? C7 O1 C6 116.4(5) . . ? C7 O1 Cd1 119.2(4) . . ? C6 O1 Cd1 102.7(3) . . ? C1 N1 C10 110.5(6) . . ? C1 N1 Cd1 112.8(5) . . ? C10 N1 Cd1 110.2(4) . . ? N1 C1 C2 112.5(6) . . ? C4 N2 C5 111.6(5) . . ? C4 N2 Cd1 111.2(4) . . ? C5 N2 Cd1 111.6(3) . . ? C9 O2 C8 115.6(5) . . ? C9 O2 Cd1 110.4(4) . . ? C8 O2 Cd1 113.8(4) . . ? C1 C2 S1 110.1(5) . . ? C4 C3 S1 112.6(4) . . ? N2 C4 C3 111.2(5) . . ? N2 C5 C6 110.9(5) . . ? C5 C6 O1 108.7(5) . . ? O1 C7 C8 110.1(6) . . ? O2 C8 C7 105.8(5) . . ? O2 C9 C10 108.2(5) . . ? N1 C10 C9 108.1(5) . . ? O2N N1N O3N 121.1(5) . . ? O2N N1N O1N 120.9(5) . . ? O3N N1N O1N 118.0(5) . . ? N1N O1N Cd1 99.3(3) . . ? N1N O3N Cd1 90.5(3) . . ? N2B Cd2 O4N 133.6(3) . . ? N2A Cd2 O4N 134.3(2) . . ? N2B Cd2 N1B 117.8(5) . . ? O4N Cd2 N1B 103.0(4) . . ? N2A Cd2 N1A 119.6(3) . . ? O4N Cd2 N1A 101.7(2) . . ? N2A Cd2 O2A 123.5(2) . . ? O4N Cd2 O2A 85.42(19) . . ? N1A Cd2 O2A 72.4(2) . . ? N2B Cd2 O1B 73.8(3) . . ? O4N Cd2 O1B 99.5(3) . . ? N1B Cd2 O1B 127.0(4) . . ? N2A Cd2 O1A 74.4(2) . . ? O4N Cd2 O1A 88.5(2) . . ? N1A Cd2 O1A 137.8(2) . . ? O2A Cd2 O1A 67.7(2) . . ? N2B Cd2 O2B 132.6(4) . . ? O4N Cd2 O2B 77.5(3) . . ? N1B Cd2 O2B 73.9(4) . . ? O1B Cd2 O2B 65.0(3) . . ? N2B Cd2 O6N 82.5(3) . . ? N2A Cd2 O6N 83.1(2) . . ? O4N Cd2 O6N 51.77(15) . . ? N1B Cd2 O6N 150.6(4) . . ? N1A Cd2 O6N 138.6(2) . . ? O2A Cd2 O6N 126.16(19) . . ? O1B Cd2 O6N 77.2(3) . . ? O1A Cd2 O6N 78.9(2) . . ? O2B Cd2 O6N 109.1(3) . . ? N2B Cd2 S1B 79.7(3) . . ? O4N Cd2 S1B 88.80(17) . . ? N1B Cd2 S1B 77.9(4) . . ? O1B Cd2 S1B 150.0(3) . . ? O2B Cd2 S1B 144.8(3) . . ? O6N Cd2 S1B 85.84(17) . . ? N2A Cd2 S1A 79.64(19) . . ? O4N Cd2 S1A 92.20(14) . . ? N1A Cd2 S1A 77.17(19) . . ? O2A Cd2 S1A 148.30(16) . . ? O1A Cd2 S1A 143.96(17) . . ? O6N Cd2 S1A 73.51(13) . . ? C3A S1A C2A 105.8(5) . . ? C3A S1A Cd2 90.5(3) . . ? C2A S1A Cd2 93.7(4) . . ? N1A C1A C2A 111.0(8) . . ? C1A N1A C10A 112.2(7) . . ? C1A N1A Cd2 112.9(6) . . ? C10A N1A Cd2 110.3(6) . . ? C6A O1A C7A 119.9(6) . . ? C6A O1A Cd2 105.4(5) . . ? C7A O1A Cd2 110.5(5) . . ? C1A C2A S1A 113.7(7) . . ? C8A O2A C9A 111.8(7) . . ? C8A O2A Cd2 116.1(5) . . ? C9A O2A Cd2 112.4(5) . . ? C5A N2A C4A 112.7(7) . . ? C5A N2A Cd2 110.8(5) . . ? C4A N2A Cd2 111.2(6) . . ? C4A C3A S1A 112.2(7) . . ? N2A C4A C3A 113.5(9) . . ? N2A C5A C6A 110.6(8) . . ? O1A C6A C5A 110.4(8) . . ? C8A C7A O1A 110.6(7) . . ? O2A C8A C7A 100.5(6) . . ? O2A C9A C10A 107.6(8) . . ? N1A C10A C9A 111.2(8) . . ? C2B S1B C3B 105.5(9) . . ? C2B S1B Cd2 93.9(7) . . ? C3B S1B Cd2 90.7(6) . . ? N1B C1B C2B 113.0(17) . . ? C10B N1B C1B 111.1(14) . . ? C10B N1B Cd2 113.4(12) . . ? C1B N1B Cd2 114.4(13) . . ? C6B O1B C7B 101.2(9) . . ? C6B O1B Cd2 110.6(7) . . ? C7B O1B Cd2 122.3(10) . . ? C1B C2B S1B 114.1(15) . . ? C9B O2B Cd2 103.4(10) . . ? C5B N2B C4B 109.7(11) . . ? C5B N2B Cd2 108.9(9) . . ? C4B N2B Cd2 114.8(9) . . ? C4B C3B S1B 116.6(12) . . ? N2B C4B C3B 109.7(13) . . ? N2B C5B C6B 112.8(12) . . ? O1B C6B C5B 106.7(11) . . ? O2B C9B C10B 113.4(15) . . ? N1B C10B C9B 110.2(16) . . ? O5N N2N O6N 122.7(6) . . ? O5N N2N O4N 120.7(6) . . ? O6N N2N O4N 116.6(5) . . ? N2N O4N Cd2 101.3(3) . . ? N2N O6N Cd2 90.2(3) . . ? O3 Cd3 O7N 97.55(15) . . y O3 Cd3 O10N 85.11(15) . . y O7N Cd3 O10N 83.97(14) . . y O3 Cd3 O12N 138.31(15) . . y O7N Cd3 O12N 83.08(14) . . y O10N Cd3 O12N 53.38(14) . . y O3 Cd3 Cl1 89.75(12) . . y O7N Cd3 Cl1 172.67(11) . . y O10N Cd3 Cl1 97.40(11) . . y O12N Cd3 Cl1 91.94(11) . . y O3 Cd3 Cl1 128.69(12) . 3_655 y O7N Cd3 Cl1 88.74(10) . 3_655 y O10N Cd3 Cl1 146.14(11) . 3_655 y O12N Cd3 Cl1 92.96(11) . 3_655 y Cl1 Cd3 Cl1 86.14(5) . 3_655 y Cd3 Cl1 Cd3 93.86(5) . 3_655 y O8N N3N O7N 120.6(6) . . ? O8N N3N O9N 122.2(6) . . ? O7N N3N O9N 117.2(5) . . ? N3N O7N Cd3 103.6(3) . . ? O11N N4N O10N 120.7(5) . . ? O11N N4N O12N 121.8(5) . . ? O10N N4N O12N 117.5(5) . . ? N4N O10N Cd3 94.6(3) . . ? N4N O12N Cd3 94.5(3) . . ? O15N N5N O14N 121.0(5) . . ? O15N N5N O13N 120.1(5) . . ? O14N N5N O13N 119.0(5) . . ? N1S C2S C3S 178.5(10) . . ? N4S C5S C6S 178.3(13) . . ? N7S C8S C9S 166(2) . . ? 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 C10 N1 C1 C2 179.7(6) . . . . y C3 S1 C2 C1 129.5(5) . . . . y C2 S1 C3 C4 -136.3(5) . . . . y C5 N2 C4 C3 -179.4(5) . . . . y S1 C3 C4 N2 68.7(6) . . . . y C4 N2 C5 C6 169.3(5) . . . . y N2 C5 C6 O1 -64.2(6) . . . . y C7 O1 C6 C5 178.9(6) . . . . y C6 O1 C7 C8 -84.6(7) . . . . y C9 O2 C8 C7 178.6(6) . . . . y O1 C7 C8 O2 -57.8(7) . . . . y C8 O2 C9 C10 -169.7(5) . . . . y C1 N1 C10 C9 -179.1(6) . . . . y O2 C9 C10 N1 62.8(7) . . . . y N1 C1 C2 S1 -65.1(8) . . . . y C2A C1A N1A C10A 176.7(9) . . . . ? N1A C1A C2A S1A 64.8(11) . . . . ? C3A S1A C2A C1A -126.6(8) . . . . ? C2A S1A C3A C4A 137.6(8) . . . . ? C5A N2A C4A C3A 176.2(9) . . . . ? S1A C3A C4A N2A -70.0(11) . . . . ? C4A N2A C5A C6A -168.2(9) . . . . ? C7A O1A C6A C5A -171.1(7) . . . . ? N2A C5A C6A O1A 62.3(11) . . . . ? C6A O1A C7A C8A 77.3(9) . . . . ? C9A O2A C8A C7A 175.3(7) . . . . ? O1A C7A C8A O2A 63.5(9) . . . . ? C8A O2A C9A C10A 170.9(8) . . . . ? C1A N1A C10A C9A 174.6(8) . . . . ? O2A C9A C10A N1A -57.7(11) . . . . ? C2B C1B N1B C10B 179.7(18) . . . . ? N1B C1B C2B S1B 62(2) . . . . ? C3B S1B C2B C1B -128.6(16) . . . . ? C2B S1B C3B C4B 132.4(14) . . . . ? C5B N2B C4B C3B 174.4(13) . . . . ? S1B C3B C4B N2B -63.3(18) . . . . ? C4B N2B C5B C6B -178.0(13) . . . . ? C7B O1B C6B C5B -166.4(13) . . . . ? N2B C5B C6B O1B 59.0(16) . . . . ? C1B N1B C10B C9B 169.1(18) . . . . ? O2B C9B C10B N1B -60(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1C O13N 0.93 2.15 2.946(7) 143 . N2 H2C O15N 0.93 2.58 3.263(7) 131 . N2 H2C O7N 0.93 2.66 3.341(6) 131 3 O3 H1W O14N 0.84(3) 2.05(6) 2.874(6) 167(7) 3 O3 H2W O13N 0.84(3) 1.89(3) 2.732(6) 178(8) . _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 1.91 _refine_diff_density_min -1.07 _refine_diff_density_rms 0.14