# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_compound1 _database_code_depnum_ccdc_archive 'CCDC 894377' #TrackingRef '894377.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H16 Cd N2 O10 S' _chemical_formula_weight 684.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 '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' _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 7.4706(18) _cell_length_b 10.994(2) _cell_length_c 16.357(4) _cell_angle_alpha 71.743(7) _cell_angle_beta 86.791(7) _cell_angle_gamma 76.869(7) _cell_volume 1242.3(5) _cell_formula_units_Z 2 _cell_measurement_reflns_used 3572 _cell_measurement_theta_min 2.7637 _cell_measurement_theta_max 27.5399 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.831 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 684 _exptl_absorpt_coefficient_mu 1.032 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9347 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details '(CrystalClear; Rigaku, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type \w _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13465 _diffrn_reflns_av_R_equivalents 0.0161 _diffrn_reflns_av_sigmaI/netI 0.0213 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.71 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5660 _reflns_number_gt 5221 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _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^)+(0.0264P)^2^+0.5568P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5660 _refine_ls_number_parameters 379 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0261 _refine_ls_R_factor_gt 0.0229 _refine_ls_wR_factor_ref 0.0544 _refine_ls_wR_factor_gt 0.0526 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.066 _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 Cd1 Cd 0.331275(17) 0.110946(12) 0.556619(8) 0.02183(5) Uani 1 1 d U . . S1 S 0.70544(6) -0.41840(4) 0.89931(3) 0.02112(9) Uani 1 1 d . . . O10 O 0.83892(19) -0.53141(13) 0.94741(9) 0.0314(3) Uani 1 1 d . . . O9 O 0.55635(19) -0.43586(14) 0.85543(9) 0.0303(3) Uani 1 1 d . . . O4 O 0.60202(19) 0.07929(13) 0.65335(9) 0.0303(3) Uani 1 1 d U . . O2 O 1.28052(18) -0.07360(14) 0.65364(10) 0.0349(3) Uani 1 1 d . . . O1 O 1.02155(19) 0.05002(13) 0.58818(9) 0.0322(3) Uani 1 1 d . . . O7 O 0.0459(2) -0.14853(17) 1.07482(11) 0.0419(4) Uani 1 1 d . . . O5 O 0.2847(2) 0.00739(15) 1.11096(10) 0.0407(4) Uani 1 1 d . . . O3 O 0.64920(18) -0.03253(14) 0.56222(8) 0.0287(3) Uani 1 1 d U . . O6 O 0.4432(3) -0.16187(16) 1.21373(9) 0.0480(4) Uani 1 1 d . . . O8 O 0.0711(2) -0.13136(18) 0.93541(11) 0.0487(4) Uani 1 1 d . . . N1 N 0.3590(2) 0.31233(15) 0.46772(10) 0.0241(3) Uani 1 1 d . . . N2 N 0.1944(2) 0.26851(16) 0.62512(10) 0.0269(3) Uani 1 1 d . . . C13 C 0.3432(2) -0.20122(18) 1.01658(11) 0.0226(4) Uani 1 1 d . . . C8 C 0.6874(2) -0.01690(17) 0.63127(11) 0.0189(3) Uani 1 1 d . . . C3 C 1.1023(2) -0.24745(19) 0.76980(12) 0.0239(4) Uani 1 1 d . . . H3 H 1.2294 -0.2603 0.7733 0.029 Uiso 1 1 calc R . . C6 C 0.7244(2) -0.21090(17) 0.75748(11) 0.0209(3) Uani 1 1 d . . . H6 H 0.5975 -0.1996 0.7540 0.025 Uiso 1 1 calc R . . C10 C 0.7202(3) -0.3104(2) 1.02777(12) 0.0286(4) Uani 1 1 d . . . H10 H 0.8458 -0.3468 1.0312 0.034 Uiso 1 1 calc R . . C4 C 1.0050(2) -0.14312(17) 0.70344(11) 0.0193(3) Uani 1 1 d . . . C1 C 0.8250(2) -0.31318(17) 0.82318(11) 0.0196(3) Uani 1 1 d . . . C7 C 1.1072(2) -0.04872(18) 0.64324(12) 0.0222(4) Uani 1 1 d . . . C15 C 0.3792(3) -0.1017(2) 1.13470(12) 0.0268(4) Uani 1 1 d . . . C5 C 0.8139(2) -0.12570(16) 0.69711(10) 0.0181(3) Uani 1 1 d . . . C9 C 0.6093(2) -0.32660(18) 0.96866(11) 0.0218(4) Uani 1 1 d . . . C2 C 1.0140(2) -0.33187(18) 0.83036(12) 0.0236(4) Uani 1 1 d . . . H2 H 1.0799 -0.3998 0.8750 0.028 Uiso 1 1 calc R . . C22 C 0.1986(2) 0.39337(18) 0.57844(12) 0.0251(4) Uani 1 1 d . . . C17 C 0.4431(3) 0.3328(2) 0.39255(13) 0.0327(4) Uani 1 1 d . . . H17 H 0.4937 0.2611 0.3736 0.039 Uiso 1 1 calc R . . C21 C 0.2872(2) 0.41631(18) 0.49607(12) 0.0235(4) Uani 1 1 d . . . C16 C 0.1374(3) -0.1565(2) 1.01366(14) 0.0295(4) Uani 1 1 d . . . C14 C 0.4228(2) -0.27184(18) 0.96193(12) 0.0242(4) Uani 1 1 d . . . H14 H 0.3511 -0.2823 0.9210 0.029 Uiso 1 1 calc R . . C11 C 0.6403(3) -0.2388(2) 1.08157(13) 0.0313(4) Uani 1 1 d . . . H11 H 0.7132 -0.2271 1.1215 0.038 Uiso 1 1 calc R . . C12 C 0.4519(3) -0.18391(19) 1.07686(12) 0.0252(4) Uani 1 1 d . . . C23 C 0.1193(3) 0.5015(2) 0.60758(14) 0.0340(5) Uani 1 1 d . . . C20 C 0.2961(3) 0.54576(19) 0.44713(14) 0.0319(4) Uani 1 1 d . . . C18 C 0.4586(3) 0.4578(2) 0.34068(14) 0.0414(5) Uani 1 1 d . . . H18 H 0.5177 0.4689 0.2881 0.050 Uiso 1 1 calc R . . C19 C 0.3865(3) 0.5625(2) 0.36812(15) 0.0413(5) Uani 1 1 d . . . H19 H 0.3968 0.6461 0.3344 0.050 Uiso 1 1 calc R . . C28 C 0.1123(3) 0.2476(2) 0.70059(14) 0.0377(5) Uani 1 1 d . . . H28 H 0.1093 0.1617 0.7327 0.045 Uiso 1 1 calc R . . C25 C 0.2145(3) 0.6523(2) 0.47915(18) 0.0426(6) Uani 1 1 d . . . H25 H 0.2208 0.7374 0.4469 0.051 Uiso 1 1 calc R . . C24 C 0.1290(3) 0.6312(2) 0.55486(19) 0.0452(6) Uani 1 1 d . . . H24 H 0.0748 0.7025 0.5737 0.054 Uiso 1 1 calc R . . C26 C 0.0333(3) 0.4743(3) 0.68773(16) 0.0457(6) Uani 1 1 d . . . H26 H -0.0217 0.5426 0.7092 0.055 Uiso 1 1 calc R . . C27 C 0.0301(3) 0.3489(3) 0.73399(15) 0.0469(6) Uani 1 1 d . . . H27 H -0.0261 0.3305 0.7873 0.056 Uiso 1 1 calc R . . H6A H 0.4082 -0.1153 1.2501 0.056 Uiso 1 1 d R . . H8A H -0.0531 -0.1082 0.9355 0.056 Uiso 1 1 d 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 0.02307(7) 0.01725(7) 0.02284(7) -0.00302(5) 0.00042(5) -0.00431(5) S1 0.0223(2) 0.0191(2) 0.0203(2) -0.00313(17) 0.00337(16) -0.00634(16) O10 0.0308(7) 0.0212(7) 0.0338(8) 0.0008(6) 0.0034(6) -0.0027(5) O9 0.0309(7) 0.0346(8) 0.0308(7) -0.0125(6) 0.0030(6) -0.0154(6) O4 0.0316(7) 0.0282(7) 0.0248(7) -0.0080(6) -0.0033(5) 0.0065(6) O2 0.0198(7) 0.0329(8) 0.0440(9) 0.0014(7) 0.0040(6) -0.0092(6) O1 0.0296(7) 0.0263(7) 0.0334(8) 0.0029(6) 0.0004(6) -0.0089(6) O7 0.0261(7) 0.0539(10) 0.0484(9) -0.0208(8) 0.0080(7) -0.0084(7) O5 0.0411(9) 0.0354(9) 0.0420(9) -0.0155(7) -0.0129(7) 0.0071(7) O3 0.0320(6) 0.0333(8) 0.0211(6) -0.0084(6) -0.0050(5) -0.0066(5) O6 0.0776(12) 0.0356(9) 0.0230(7) -0.0121(7) -0.0062(7) 0.0088(8) O8 0.0305(8) 0.0650(11) 0.0516(10) -0.0345(9) -0.0166(7) 0.0148(7) N1 0.0236(8) 0.0227(8) 0.0250(8) -0.0041(6) -0.0011(6) -0.0076(6) N2 0.0242(8) 0.0298(9) 0.0266(8) -0.0082(7) -0.0016(6) -0.0060(6) C13 0.0212(9) 0.0221(9) 0.0223(9) -0.0045(7) -0.0005(7) -0.0036(7) C8 0.0163(8) 0.0214(9) 0.0179(8) -0.0021(7) 0.0016(6) -0.0078(6) C3 0.0178(8) 0.0275(10) 0.0250(9) -0.0056(8) -0.0003(7) -0.0057(7) C6 0.0172(8) 0.0232(9) 0.0216(8) -0.0054(7) 0.0016(6) -0.0053(7) C10 0.0197(9) 0.0367(11) 0.0271(10) -0.0085(8) -0.0005(7) -0.0035(8) C4 0.0194(8) 0.0197(8) 0.0196(8) -0.0070(7) 0.0027(6) -0.0051(6) C1 0.0231(8) 0.0195(8) 0.0164(8) -0.0047(7) 0.0034(6) -0.0072(7) C7 0.0227(9) 0.0213(9) 0.0248(9) -0.0089(7) 0.0050(7) -0.0076(7) C15 0.0253(9) 0.0308(10) 0.0256(9) -0.0096(8) 0.0000(7) -0.0070(8) C5 0.0197(8) 0.0176(8) 0.0166(8) -0.0056(7) -0.0002(6) -0.0032(6) C9 0.0233(9) 0.0229(9) 0.0175(8) -0.0033(7) 0.0030(6) -0.0065(7) C2 0.0231(9) 0.0235(9) 0.0205(8) -0.0025(7) -0.0025(7) -0.0032(7) C22 0.0193(8) 0.0254(10) 0.0323(10) -0.0120(8) -0.0070(7) -0.0023(7) C17 0.0306(10) 0.0405(12) 0.0281(10) -0.0082(9) 0.0021(8) -0.0135(9) C21 0.0189(8) 0.0193(9) 0.0312(10) -0.0046(7) -0.0078(7) -0.0045(7) C16 0.0248(9) 0.0281(10) 0.0396(11) -0.0167(9) -0.0034(8) -0.0039(8) C14 0.0224(9) 0.0269(10) 0.0229(9) -0.0066(7) -0.0023(7) -0.0059(7) C11 0.0260(10) 0.0431(12) 0.0267(10) -0.0139(9) -0.0046(8) -0.0058(8) C12 0.0269(9) 0.0273(10) 0.0204(9) -0.0058(7) 0.0003(7) -0.0065(7) C23 0.0241(10) 0.0377(12) 0.0465(12) -0.0246(10) -0.0114(9) -0.0002(8) C20 0.0298(10) 0.0203(9) 0.0429(12) -0.0006(8) -0.0162(9) -0.0094(8) C18 0.0400(12) 0.0530(15) 0.0285(11) 0.0005(10) -0.0025(9) -0.0226(11) C19 0.0411(12) 0.0351(12) 0.0391(12) 0.0112(10) -0.0134(10) -0.0202(10) C28 0.0336(11) 0.0485(13) 0.0281(10) -0.0084(10) 0.0003(8) -0.0082(10) C25 0.0393(12) 0.0198(10) 0.0674(17) -0.0088(11) -0.0216(12) -0.0054(9) C24 0.0371(12) 0.0283(12) 0.0767(18) -0.0296(12) -0.0209(12) 0.0038(9) C26 0.0332(12) 0.0626(17) 0.0516(14) -0.0396(14) -0.0077(10) 0.0020(11) C27 0.0355(12) 0.077(2) 0.0319(12) -0.0267(13) 0.0004(9) -0.0046(12) _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 O2 2.2457(14) 1_455 ? Cd1 N1 2.2839(16) . ? Cd1 O3 2.3461(14) 2_656 ? Cd1 N2 2.3632(16) . ? Cd1 O3 2.5237(14) . ? Cd1 O4 2.5316(15) . ? Cd1 O1 2.5343(15) 1_455 ? Cd1 C7 2.7210(18) 1_455 ? S1 O9 1.4371(14) . ? S1 O10 1.4386(14) . ? S1 C9 1.7659(18) . ? S1 C1 1.7691(18) . ? O4 C8 1.250(2) . ? O2 C7 1.271(2) . ? O2 Cd1 2.2457(14) 1_655 ? O1 C7 1.239(2) . ? O1 Cd1 2.5343(15) 1_655 ? O7 C16 1.195(3) . ? O5 C15 1.201(2) . ? O3 C8 1.252(2) . ? O3 Cd1 2.3461(14) 2_656 ? O6 C15 1.314(2) . ? O6 H6A 0.8935 . ? O8 C16 1.322(3) . ? O8 H8A 0.9045 . ? N1 C17 1.327(3) . ? N1 C21 1.355(2) . ? N2 C28 1.325(3) . ? N2 C22 1.352(3) . ? C13 C14 1.386(3) . ? C13 C12 1.395(3) . ? C13 C16 1.503(3) . ? C8 C5 1.509(2) . ? C3 C2 1.381(3) . ? C3 C4 1.397(2) . ? C3 H3 0.9300 . ? C6 C5 1.389(2) . ? C6 C1 1.391(2) . ? C6 H6 0.9300 . ? C10 C11 1.382(3) . ? C10 C9 1.385(3) . ? C10 H10 0.9300 . ? C4 C5 1.402(2) . ? C4 C7 1.505(2) . ? C1 C2 1.386(2) . ? C7 Cd1 2.7210(18) 1_655 ? C15 C12 1.504(3) . ? C9 C14 1.382(2) . ? C2 H2 0.9300 . ? C22 C23 1.412(3) . ? C22 C21 1.442(3) . ? C17 C18 1.398(3) . ? C17 H17 0.9300 . ? C21 C20 1.412(3) . ? C14 H14 0.9300 . ? C11 C12 1.395(3) . ? C11 H11 0.9300 . ? C23 C26 1.403(3) . ? C23 C24 1.433(3) . ? C20 C19 1.403(3) . ? C20 C25 1.429(3) . ? C18 C19 1.353(4) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C28 C27 1.396(3) . ? C28 H28 0.9300 . ? C25 C24 1.339(4) . ? C25 H25 0.9300 . ? C24 H24 0.9300 . ? C26 C27 1.353(4) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? 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 O2 Cd1 N1 172.91(5) 1_455 . ? O2 Cd1 O3 95.70(6) 1_455 2_656 ? N1 Cd1 O3 90.10(5) . 2_656 ? O2 Cd1 N2 100.77(6) 1_455 . ? N1 Cd1 N2 72.25(6) . . ? O3 Cd1 N2 149.97(5) 2_656 . ? O2 Cd1 O3 81.34(5) 1_455 . ? N1 Cd1 O3 104.30(5) . . ? O3 Cd1 O3 73.43(5) 2_656 . ? N2 Cd1 O3 133.66(5) . . ? O2 Cd1 O4 84.80(5) 1_455 . ? N1 Cd1 O4 95.38(5) . . ? O3 Cd1 O4 123.88(5) 2_656 . ? N2 Cd1 O4 82.79(5) . . ? O3 Cd1 O4 51.08(4) . . ? O2 Cd1 O1 54.54(5) 1_455 1_455 ? N1 Cd1 O1 121.80(5) . 1_455 ? O3 Cd1 O1 88.15(5) 2_656 1_455 ? N2 Cd1 O1 81.36(5) . 1_455 ? O3 Cd1 O1 130.35(5) . 1_455 ? O4 Cd1 O1 131.96(5) . 1_455 ? O2 Cd1 C7 27.59(5) 1_455 1_455 ? N1 Cd1 C7 148.22(5) . 1_455 ? O3 Cd1 C7 93.01(5) 2_656 1_455 ? N2 Cd1 C7 90.23(6) . 1_455 ? O3 Cd1 C7 106.90(5) . 1_455 ? O4 Cd1 C7 108.80(5) . 1_455 ? O1 Cd1 C7 26.97(5) 1_455 1_455 ? O9 S1 O10 119.66(9) . . ? O9 S1 C9 107.63(8) . . ? O10 S1 C9 108.53(9) . . ? O9 S1 C1 108.30(8) . . ? O10 S1 C1 107.77(8) . . ? C9 S1 C1 103.83(8) . . ? C8 O4 Cd1 91.47(11) . . ? C7 O2 Cd1 97.50(11) . 1_655 ? C7 O1 Cd1 84.94(11) . 1_655 ? C8 O3 Cd1 161.43(12) . 2_656 ? C8 O3 Cd1 91.80(10) . . ? Cd1 O3 Cd1 106.57(5) 2_656 . ? C15 O6 H6A 114.2 . . ? C16 O8 H8A 109.8 . . ? C17 N1 C21 118.88(17) . . ? C17 N1 Cd1 124.62(14) . . ? C21 N1 Cd1 116.48(12) . . ? C28 N2 C22 118.55(18) . . ? C28 N2 Cd1 127.47(15) . . ? C22 N2 Cd1 113.94(12) . . ? C14 C13 C12 119.95(17) . . ? C14 C13 C16 117.64(16) . . ? C12 C13 C16 122.16(16) . . ? O4 C8 O3 121.19(16) . . ? O4 C8 C5 117.67(15) . . ? O3 C8 C5 120.26(15) . . ? C2 C3 C4 121.48(17) . . ? C2 C3 H3 119.3 . . ? C4 C3 H3 119.3 . . ? C5 C6 C1 119.82(16) . . ? C5 C6 H6 120.1 . . ? C1 C6 H6 120.1 . . ? C11 C10 C9 118.57(17) . . ? C11 C10 H10 120.7 . . ? C9 C10 H10 120.7 . . ? C3 C4 C5 119.18(16) . . ? C3 C4 C7 118.99(16) . . ? C5 C4 C7 121.76(16) . . ? C2 C1 C6 121.34(16) . . ? C2 C1 S1 120.29(14) . . ? C6 C1 S1 118.36(13) . . ? O1 C7 O2 122.91(17) . . ? O1 C7 C4 119.99(16) . . ? O2 C7 C4 117.07(16) . . ? O1 C7 Cd1 68.09(10) . 1_655 ? O2 C7 Cd1 54.91(9) . 1_655 ? C4 C7 Cd1 170.53(13) . 1_655 ? O5 C15 O6 124.39(18) . . ? O5 C15 C12 124.67(18) . . ? O6 C15 C12 110.78(16) . . ? C6 C5 C4 119.60(16) . . ? C6 C5 C8 114.17(15) . . ? C4 C5 C8 126.18(15) . . ? C14 C9 C10 121.54(17) . . ? C14 C9 S1 118.40(14) . . ? C10 C9 S1 120.06(14) . . ? C3 C2 C1 118.57(17) . . ? C3 C2 H2 120.7 . . ? C1 C2 H2 120.7 . . ? N2 C22 C23 122.27(19) . . ? N2 C22 C21 118.60(16) . . ? C23 C22 C21 119.13(18) . . ? N1 C17 C18 122.6(2) . . ? N1 C17 H17 118.7 . . ? C18 C17 H17 118.7 . . ? N1 C21 C20 121.86(18) . . ? N1 C21 C22 118.71(16) . . ? C20 C21 C22 119.43(18) . . ? O7 C16 O8 124.65(19) . . ? O7 C16 C13 124.17(19) . . ? O8 C16 C13 111.15(17) . . ? C9 C14 C13 119.59(17) . . ? C9 C14 H14 120.2 . . ? C13 C14 H14 120.2 . . ? C10 C11 C12 121.05(18) . . ? C10 C11 H11 119.5 . . ? C12 C11 H11 119.5 . . ? C13 C12 C11 119.29(17) . . ? C13 C12 C15 123.41(17) . . ? C11 C12 C15 117.20(17) . . ? C26 C23 C22 117.0(2) . . ? C26 C23 C24 123.7(2) . . ? C22 C23 C24 119.3(2) . . ? C19 C20 C21 117.2(2) . . ? C19 C20 C25 123.2(2) . . ? C21 C20 C25 119.6(2) . . ? C19 C18 C17 119.0(2) . . ? C19 C18 H18 120.5 . . ? C17 C18 H18 120.5 . . ? C18 C19 C20 120.4(2) . . ? C18 C19 H19 119.8 . . ? C20 C19 H19 119.8 . . ? N2 C28 C27 122.8(2) . . ? N2 C28 H28 118.6 . . ? C27 C28 H28 118.6 . . ? C24 C25 C20 121.0(2) . . ? C24 C25 H25 119.5 . . ? C20 C25 H25 119.5 . . ? C25 C24 C23 121.5(2) . . ? C25 C24 H24 119.2 . . ? C23 C24 H24 119.2 . . ? C27 C26 C23 120.3(2) . . ? C27 C26 H26 119.9 . . ? C23 C26 H26 119.9 . . ? C26 C27 C28 119.1(2) . . ? C26 C27 H27 120.4 . . ? C28 C27 H27 120.4 . . ? 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 O6 H6A O4 0.89 1.74 2.585(2) 157.3 2_657 O8 H8A O5 0.90 1.88 2.726(2) 154.0 2_557 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.392 _refine_diff_density_min -0.361 _refine_diff_density_rms 0.058 data_compound2 _database_code_depnum_ccdc_archive 'CCDC 894378' #TrackingRef '894378.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H31 Cd2 N4 O14.50 S' _chemical_formula_weight 1056.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.905(5) _cell_length_b 13.194(7) _cell_length_c 14.970(8) _cell_angle_alpha 110.429(7) _cell_angle_beta 95.307(6) _cell_angle_gamma 91.644(6) _cell_volume 2005.5(17) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2111 _cell_measurement_theta_min 2.2506 _cell_measurement_theta_max 27.4835 _exptl_crystal_description lamellar _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.750 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1054 _exptl_absorpt_coefficient_mu 1.189 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8060 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details '(CrystalClear; Rigaku, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type \w _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15581 _diffrn_reflns_av_R_equivalents 0.0300 _diffrn_reflns_av_sigmaI/netI 0.0664 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 27.45 _reflns_number_total 9042 _reflns_number_gt 7048 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _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^)+(0.0657P)^2^+0.6533P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9042 _refine_ls_number_parameters 559 _refine_ls_number_restraints 37 _refine_ls_R_factor_all 0.0699 _refine_ls_R_factor_gt 0.0523 _refine_ls_wR_factor_ref 0.1464 _refine_ls_wR_factor_gt 0.1345 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.098 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.07892(3) -0.00973(3) 0.61082(3) 0.03012(12) Uani 1 1 d . . . S1 S -0.37363(11) 0.49271(10) 0.70088(11) 0.0358(3) Uani 1 1 d . . . O1 O -0.0130(4) 0.2526(4) 0.5378(3) 0.0535(11) Uani 1 1 d . . . N1 N 0.2649(4) 0.0826(4) 0.6069(3) 0.0391(11) Uani 1 1 d . . . C1 C -0.0620(5) 0.1997(4) 0.5800(4) 0.0345(11) Uani 1 1 d . . . Cd2 Cd 0.08591(3) 0.04417(3) 0.89242(3) 0.03395(12) Uani 1 1 d . . . O2 O -0.0706(4) 0.0967(3) 0.5534(3) 0.0409(9) Uani 1 1 d . . . N2 N 0.2490(4) -0.1191(4) 0.6193(3) 0.0389(10) Uani 1 1 d . . . C2 C -0.1279(4) 0.2639(4) 0.6662(4) 0.0288(10) Uani 1 1 d . . . O3 O 0.0654(3) 0.1530(3) 0.7355(3) 0.0400(9) Uani 1 1 d . . . N3 N 0.2855(4) 0.1066(4) 0.8744(4) 0.0451(12) Uani 1 1 d . . . C3 C -0.0266(5) 0.1775(4) 0.7816(4) 0.0354(11) Uani 1 1 d . . . O4 O -0.0494(4) 0.1482(4) 0.8497(3) 0.0500(11) Uani 1 1 d . . . N4 N 0.2288(4) -0.0800(4) 0.9062(4) 0.0438(11) Uani 1 1 d . . . C4 C -0.1162(5) 0.2521(4) 0.7560(4) 0.0316(11) Uani 1 1 d . . . O5 O -0.0966(3) 0.9517(3) 0.9004(3) 0.0411(9) Uani 1 1 d . . . C5 C -0.1814(5) 0.3157(5) 0.8283(4) 0.0414(13) Uani 1 1 d . . . H5 H -0.1721 0.3082 0.8881 0.050 Uiso 1 1 calc R . . O6 O -0.1088(4) 0.8203(3) 0.9605(3) 0.0485(10) Uani 1 1 d . . . C6 C -0.2603(5) 0.3901(4) 0.8132(4) 0.0411(13) Uani 1 1 d . . . H6 H -0.3045 0.4319 0.8617 0.049 Uiso 1 1 calc R . . O7 O 0.0465(3) 0.9015(3) 0.7440(3) 0.0438(9) Uani 1 1 d . . . C7 C -0.2715(4) 0.4004(4) 0.7238(4) 0.0319(11) Uani 1 1 d . . . O8 O -0.1001(4) 0.9160(3) 0.6376(3) 0.0429(9) Uani 1 1 d . . . C8 C -0.2065(4) 0.3389(4) 0.6518(4) 0.0322(11) Uani 1 1 d . . . H8 H -0.2153 0.3476 0.5926 0.039 Uiso 1 1 calc R . . O9 O -0.4346(4) 0.4426(3) 0.6054(3) 0.0487(10) Uani 1 1 d . . . C9 C -0.1177(4) 0.8550(4) 0.8905(4) 0.0344(11) Uani 1 1 d . . . O10 O -0.4464(3) 0.5311(3) 0.7808(3) 0.0507(11) Uani 1 1 d . . . C10 C -0.1590(4) 0.7719(4) 0.7927(4) 0.0289(10) Uani 1 1 d . . . C11 C -0.0588(5) 0.8757(4) 0.6983(4) 0.0344(11) Uani 1 1 d . . . C12 C -0.1376(4) 0.7834(4) 0.7059(4) 0.0301(10) Uani 1 1 d . . . C13 C -0.1829(5) 0.7040(4) 0.6198(4) 0.0358(12) Uani 1 1 d . . . H13 H -0.1657 0.7115 0.5627 0.043 Uiso 1 1 calc R . . C14 C -0.2531(5) 0.6135(4) 0.6169(4) 0.0370(12) Uani 1 1 d . . . H14 H -0.2834 0.5609 0.5586 0.044 Uiso 1 1 calc R . . C15 C -0.2771(4) 0.6032(4) 0.7016(4) 0.0333(11) Uani 1 1 d . . . C16 C -0.2305(4) 0.6804(4) 0.7897(4) 0.0322(11) Uani 1 1 d . . . H16 H -0.2468 0.6713 0.8464 0.039 Uiso 1 1 calc R . . C17 C 0.2711(6) 0.1796(5) 0.6009(5) 0.0516(16) Uani 1 1 d . . . H17 H 0.1978 0.2123 0.5955 0.062 Uiso 1 1 calc R . . C18 C 0.3818(7) 0.2362(6) 0.6022(6) 0.065(2) Uani 1 1 d . . . H18 H 0.3821 0.3047 0.5977 0.078 Uiso 1 1 calc R . . C19 C 0.4887(6) 0.1890(6) 0.6103(5) 0.065(2) Uani 1 1 d . . . H19 H 0.5634 0.2257 0.6118 0.078 Uiso 1 1 calc R . . C20 C 0.4883(5) 0.0843(6) 0.6165(4) 0.0545(17) Uani 1 1 d . . . C21 C 0.5968(5) 0.0279(7) 0.6235(5) 0.064(2) Uani 1 1 d U . . H21 H 0.6740 0.0607 0.6253 0.076 Uiso 1 1 calc R . . C22 C 0.5881(7) -0.0710(7) 0.6275(6) 0.0669(19) Uani 1 1 d U . . H22 H 0.6599 -0.1063 0.6315 0.080 Uiso 1 1 calc R . . C23 C 0.4736(6) -0.1241(6) 0.6260(5) 0.0555(18) Uani 1 1 d . . . C24 C 0.4608(7) -0.2281(7) 0.6296(5) 0.069(2) Uani 1 1 d . . . H24 H 0.5311 -0.2656 0.6327 0.083 Uiso 1 1 calc R . . C25 C 0.3470(8) -0.2768(7) 0.6288(6) 0.069(2) Uani 1 1 d . . . H25 H 0.3387 -0.3464 0.6306 0.083 Uiso 1 1 calc R . . C26 C 0.2443(6) -0.2162(5) 0.6250(5) 0.0512(15) Uani 1 1 d . . . H26 H 0.1672 -0.2470 0.6267 0.061 Uiso 1 1 calc R . . C27 C 0.3632(5) -0.0730(5) 0.6202(4) 0.0419(13) Uani 1 1 d . . . C28 C 0.3690(5) 0.0352(5) 0.6144(4) 0.0411(13) Uani 1 1 d . . . C29 C 0.3129(6) 0.2014(6) 0.8653(5) 0.0561(17) Uani 1 1 d . . . H29 H 0.2506 0.2478 0.8645 0.067 Uiso 1 1 calc R . . C30 C 0.4345(7) 0.2323(7) 0.8567(5) 0.069(2) Uani 1 1 d . . . H30 H 0.4521 0.2994 0.8517 0.083 Uiso 1 1 calc R . . C31 C 0.5246(7) 0.1657(8) 0.8557(5) 0.072(2) Uani 1 1 d . . . H31 H 0.6045 0.1859 0.8487 0.087 Uiso 1 1 calc R . . C32 C 0.4996(5) 0.0665(7) 0.8650(5) 0.060(2) Uani 1 1 d . . . C33 C 0.5905(6) -0.0102(9) 0.8663(5) 0.075(3) Uani 1 1 d . . . H33 H 0.6720 0.0057 0.8595 0.090 Uiso 1 1 calc R . . C34 C 0.5599(6) -0.1042(8) 0.8771(5) 0.076(3) Uani 1 1 d . . . H34 H 0.6210 -0.1520 0.8766 0.092 Uiso 1 1 calc R . . C35 C 0.4384(6) -0.1334(6) 0.8893(5) 0.0557(17) Uani 1 1 d . . . C36 C 0.4048(7) -0.2291(7) 0.9035(5) 0.066(2) Uani 1 1 d . . . H36 H 0.4630 -0.2797 0.9020 0.080 Uiso 1 1 calc R . . C37 C 0.2888(7) -0.2481(6) 0.9192(6) 0.071(2) Uani 1 1 d . . . H37 H 0.2658 -0.3120 0.9282 0.086 Uiso 1 1 calc R . . C38 C 0.2026(6) -0.1709(6) 0.9220(6) 0.0628(19) Uani 1 1 d . . . H38 H 0.1233 -0.1837 0.9355 0.075 Uiso 1 1 calc R . . C39 C 0.3448(5) -0.0603(5) 0.8907(4) 0.0448(14) Uani 1 1 d . . . C40 C 0.3752(5) 0.0374(6) 0.8755(4) 0.0441(14) Uani 1 1 d . . . O11 O -0.0631(8) 0.6146(7) 0.9702(7) 0.157(3) Uani 1 1 d U . . H11A H -0.0702 0.6886 0.9885 0.188 Uiso 1 1 d R . . H11B H -0.0252 0.5968 0.9142 0.188 Uiso 1 1 d R . . O12 O 0.0461(11) 0.4708(9) 0.5832(9) 0.218(5) Uani 1 1 d U . . H12A H 0.0812 0.4112 0.5765 0.262 Uiso 1 1 d R . . H12B H -0.0179 0.4559 0.5335 0.262 Uiso 1 1 d R . . O13 O -0.4183(13) 0.4855(11) 1.0646(10) 0.257(6) Uani 1 1 d U . . H13A H -0.4145 0.4605 1.0037 0.308 Uiso 1 1 d R . . H13B H -0.3417 0.5085 1.0891 0.308 Uiso 1 1 d R . . O14 O -0.1603(15) 0.5238(14) 1.0866(12) 0.315(8) Uani 1 1 d U . . H14A H -0.1540 0.5828 1.0699 0.378 Uiso 1 1 d R . . H14B H -0.1544 0.4631 1.0321 0.378 Uiso 1 1 d R . . O15 O 0.045(2) 0.5452(19) 0.7856(17) 0.210(10) Uani 0.50 1 d PU . . H15A H 0.0602 0.5297 0.7244 0.252 Uiso 0.50 1 d PR . . H15B H 0.1061 0.5234 0.8162 0.252 Uiso 0.50 1 d 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 0.0262(2) 0.0283(2) 0.0361(2) 0.01141(16) 0.00494(15) 0.00105(14) S1 0.0280(6) 0.0261(6) 0.0555(9) 0.0171(6) 0.0047(6) 0.0032(5) O1 0.064(3) 0.053(3) 0.058(3) 0.030(2) 0.031(2) 0.016(2) N1 0.031(2) 0.038(3) 0.047(3) 0.015(2) 0.004(2) -0.0051(18) C1 0.040(3) 0.027(3) 0.036(3) 0.011(2) 0.003(2) 0.007(2) Cd2 0.0288(2) 0.0304(2) 0.0414(2) 0.01164(17) 0.00141(16) 0.00277(14) O2 0.056(2) 0.032(2) 0.034(2) 0.0098(17) 0.0049(18) 0.0161(17) N2 0.035(2) 0.044(3) 0.041(3) 0.017(2) 0.009(2) 0.0125(19) C2 0.028(2) 0.022(2) 0.035(3) 0.009(2) 0.004(2) 0.0010(18) O3 0.0326(19) 0.037(2) 0.045(2) 0.0076(18) 0.0011(17) 0.0083(15) N3 0.029(2) 0.059(3) 0.046(3) 0.018(3) -0.001(2) -0.006(2) C3 0.038(3) 0.031(3) 0.035(3) 0.011(2) -0.005(2) 0.005(2) O4 0.066(3) 0.051(3) 0.041(2) 0.025(2) 0.006(2) 0.022(2) N4 0.033(2) 0.048(3) 0.050(3) 0.016(2) 0.004(2) 0.009(2) C4 0.034(3) 0.026(3) 0.036(3) 0.012(2) 0.006(2) 0.0029(19) O5 0.038(2) 0.033(2) 0.050(2) 0.0103(18) 0.0083(18) -0.0027(16) C5 0.050(3) 0.041(3) 0.036(3) 0.015(3) 0.010(3) 0.012(2) O6 0.064(3) 0.047(3) 0.033(2) 0.0139(19) -0.0023(19) -0.003(2) C6 0.049(3) 0.035(3) 0.041(3) 0.012(3) 0.015(3) 0.012(2) O7 0.0291(19) 0.047(2) 0.047(2) 0.0062(19) 0.0086(18) -0.0026(16) C7 0.033(3) 0.021(2) 0.041(3) 0.009(2) 0.004(2) -0.0026(18) O8 0.043(2) 0.046(2) 0.045(2) 0.022(2) 0.0091(18) -0.0011(17) C8 0.030(3) 0.028(3) 0.038(3) 0.012(2) 0.000(2) 0.0032(19) O9 0.042(2) 0.035(2) 0.065(3) 0.018(2) -0.013(2) -0.0056(16) C9 0.024(2) 0.039(3) 0.041(3) 0.015(2) 0.006(2) -0.001(2) O10 0.035(2) 0.045(2) 0.083(3) 0.031(2) 0.026(2) 0.0128(17) C10 0.024(2) 0.029(3) 0.035(3) 0.012(2) 0.006(2) 0.0042(18) C11 0.041(3) 0.028(3) 0.033(3) 0.006(2) 0.013(2) 0.004(2) C12 0.029(2) 0.026(2) 0.039(3) 0.016(2) 0.005(2) 0.0022(18) C13 0.041(3) 0.033(3) 0.032(3) 0.009(2) 0.005(2) -0.005(2) C14 0.042(3) 0.029(3) 0.039(3) 0.011(2) 0.003(2) 0.003(2) C15 0.031(3) 0.025(3) 0.047(3) 0.016(2) 0.005(2) 0.0057(19) C16 0.031(3) 0.031(3) 0.037(3) 0.015(2) 0.003(2) 0.004(2) C17 0.046(3) 0.042(4) 0.066(4) 0.018(3) 0.007(3) -0.007(3) C18 0.059(4) 0.058(4) 0.076(5) 0.022(4) 0.007(4) -0.024(3) C19 0.046(4) 0.080(5) 0.058(4) 0.011(4) 0.011(3) -0.030(4) C20 0.031(3) 0.082(5) 0.036(3) 0.005(3) 0.003(3) -0.010(3) C21 0.023(3) 0.104(6) 0.050(4) 0.011(4) 0.002(3) -0.001(3) C22 0.065(2) 0.068(2) 0.066(2) 0.0221(12) 0.0068(10) 0.0060(10) C23 0.039(3) 0.086(5) 0.044(4) 0.024(4) 0.006(3) 0.026(3) C24 0.056(4) 0.094(6) 0.059(5) 0.027(4) 0.009(4) 0.041(4) C25 0.086(6) 0.068(5) 0.068(5) 0.036(4) 0.022(4) 0.039(4) C26 0.060(4) 0.048(4) 0.049(4) 0.020(3) 0.010(3) 0.014(3) C27 0.034(3) 0.060(4) 0.030(3) 0.012(3) 0.005(2) 0.006(2) C28 0.029(3) 0.058(4) 0.031(3) 0.008(3) 0.006(2) -0.001(2) C29 0.051(4) 0.056(4) 0.059(4) 0.019(3) 0.001(3) -0.012(3) C30 0.065(5) 0.074(5) 0.061(5) 0.021(4) -0.003(4) -0.029(4) C31 0.049(4) 0.112(7) 0.051(4) 0.026(5) 0.001(3) -0.027(4) C32 0.028(3) 0.106(6) 0.035(3) 0.012(4) -0.003(3) -0.008(3) C33 0.028(3) 0.146(9) 0.046(4) 0.027(5) 0.007(3) 0.010(4) C34 0.036(4) 0.130(8) 0.046(4) 0.009(5) 0.002(3) 0.034(4) C35 0.041(3) 0.080(5) 0.042(4) 0.014(3) 0.006(3) 0.024(3) C36 0.064(5) 0.072(5) 0.055(4) 0.012(4) -0.001(4) 0.040(4) C37 0.072(5) 0.050(4) 0.090(6) 0.024(4) -0.003(4) 0.019(4) C38 0.045(4) 0.060(5) 0.089(6) 0.035(4) 0.004(4) 0.006(3) C39 0.031(3) 0.067(4) 0.028(3) 0.006(3) 0.001(2) 0.017(3) C40 0.023(3) 0.073(4) 0.027(3) 0.009(3) -0.002(2) 0.003(2) O11 0.200(7) 0.093(5) 0.175(7) 0.058(5) -0.033(6) 0.009(5) O12 0.254(9) 0.160(8) 0.249(9) 0.071(7) 0.079(8) 0.001(7) O13 0.282(10) 0.249(10) 0.260(10) 0.111(8) 0.041(8) 0.031(8) O14 0.345(12) 0.288(11) 0.338(12) 0.143(9) 0.048(9) -0.011(9) O15 0.189(12) 0.205(13) 0.215(13) 0.056(9) -0.007(9) 0.024(9) _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 O8 2.289(4) 1_545 ? Cd1 O2 2.313(4) 2_556 ? Cd1 O3 2.321(4) . ? Cd1 N1 2.352(4) . ? Cd1 N2 2.403(4) . ? Cd1 O2 2.467(4) . ? S1 O9 1.436(4) . ? S1 O10 1.447(4) . ? S1 C15 1.770(5) . ? S1 C7 1.772(5) . ? O1 C1 1.233(6) . ? N1 C17 1.314(7) . ? N1 C28 1.326(7) . ? C1 O2 1.274(6) . ? C1 C2 1.530(7) . ? Cd2 O4 2.242(4) . ? Cd2 O6 2.288(4) 2_567 ? Cd2 O5 2.339(4) 1_545 ? Cd2 N4 2.340(5) . ? Cd2 O7 2.350(4) 1_545 ? Cd2 N3 2.377(5) . ? O2 Cd1 2.313(4) 2_556 ? N2 C26 1.314(7) . ? N2 C27 1.367(7) . ? C2 C8 1.387(7) . ? C2 C4 1.401(7) . ? O3 C3 1.257(6) . ? N3 C29 1.333(8) . ? N3 C40 1.360(8) . ? C3 O4 1.252(6) . ? C3 C4 1.523(7) . ? N4 C38 1.330(8) . ? N4 C39 1.341(7) . ? C4 C5 1.388(7) . ? O5 C9 1.243(6) . ? O5 Cd2 2.339(4) 1_565 ? C5 C6 1.387(8) . ? C5 H5 0.9300 . ? O6 C9 1.279(6) . ? O6 Cd2 2.288(4) 2_567 ? C6 C7 1.387(7) . ? C6 H6 0.9300 . ? O7 C11 1.254(6) . ? O7 Cd2 2.350(4) 1_565 ? C7 C8 1.374(7) . ? O8 C11 1.260(6) . ? O8 Cd1 2.289(4) 1_565 ? C8 H8 0.9300 . ? C9 C10 1.509(7) . ? C10 C12 1.400(7) . ? C10 C16 1.403(7) . ? C11 C12 1.513(7) . ? C12 C13 1.383(7) . ? C13 C14 1.385(7) . ? C13 H13 0.9300 . ? C14 C15 1.369(7) . ? C14 H14 0.9300 . ? C15 C16 1.395(7) . ? C16 H16 0.9300 . ? C17 C18 1.397(8) . ? C17 H17 0.9300 . ? C18 C19 1.352(11) . ? C18 H18 0.9300 . ? C19 C20 1.417(11) . ? C19 H19 0.9300 . ? C20 C28 1.429(8) . ? C20 C21 1.430(10) . ? C21 C22 1.327(11) . ? C21 H21 0.9300 . ? C22 C23 1.409(10) . ? C22 H22 0.9300 . ? C23 C24 1.396(11) . ? C23 C27 1.407(8) . ? C24 C25 1.379(11) . ? C24 H24 0.9300 . ? C25 C26 1.403(9) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 C28 1.460(9) . ? C29 C30 1.406(9) . ? C29 H29 0.9300 . ? C30 C31 1.335(12) . ? C30 H30 0.9300 . ? C31 C32 1.386(11) . ? C31 H31 0.9300 . ? C32 C40 1.437(8) . ? C32 C33 1.440(11) . ? C33 C34 1.342(12) . ? C33 H33 0.9300 . ? C34 C35 1.415(10) . ? C34 H34 0.9300 . ? C35 C36 1.395(11) . ? C35 C39 1.421(8) . ? C36 C37 1.341(11) . ? C36 H36 0.9300 . ? C37 C38 1.398(10) . ? C37 H37 0.9300 . ? C38 H38 0.9300 . ? C39 C40 1.420(9) . ? O11 H11A 0.9255 . ? O11 H11B 0.9284 . ? O12 H12A 0.8626 . ? O12 H12B 0.9356 . ? O13 H13A 0.8599 . ? O13 H13B 0.8805 . ? O14 H14A 0.8991 . ? O14 H14B 0.9311 . ? O15 H15A 0.8977 . ? O15 H15B 0.8825 . ? 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 O8 Cd1 O2 99.48(15) 1_545 2_556 ? O8 Cd1 O3 92.92(14) 1_545 . ? O2 Cd1 O3 146.29(13) 2_556 . ? O8 Cd1 N1 171.67(16) 1_545 . ? O2 Cd1 N1 88.80(16) 2_556 . ? O3 Cd1 N1 79.57(15) . . ? O8 Cd1 N2 111.17(15) 1_545 . ? O2 Cd1 N2 85.15(14) 2_556 . ? O3 Cd1 N2 119.28(15) . . ? N1 Cd1 N2 70.15(16) . . ? O8 Cd1 O2 80.71(14) 1_545 . ? O2 Cd1 O2 79.08(14) 2_556 . ? O3 Cd1 O2 72.14(13) . . ? N1 Cd1 O2 100.17(15) . . ? N2 Cd1 O2 161.75(14) . . ? O9 S1 O10 119.6(3) . . ? O9 S1 C15 107.5(2) . . ? O10 S1 C15 108.0(3) . . ? O9 S1 C7 108.0(2) . . ? O10 S1 C7 107.8(2) . . ? C15 S1 C7 105.1(2) . . ? C17 N1 C28 118.6(5) . . ? C17 N1 Cd1 123.5(4) . . ? C28 N1 Cd1 117.8(4) . . ? O1 C1 O2 125.5(5) . . ? O1 C1 C2 116.4(5) . . ? O2 C1 C2 117.8(4) . . ? O4 Cd2 O6 85.47(16) . 2_567 ? O4 Cd2 O5 81.42(15) . 1_545 ? O6 Cd2 O5 101.21(14) 2_567 1_545 ? O4 Cd2 N4 169.29(17) . . ? O6 Cd2 N4 104.57(17) 2_567 . ? O5 Cd2 N4 99.90(16) 1_545 . ? O4 Cd2 O7 93.02(15) . 1_545 ? O6 Cd2 O7 175.39(13) 2_567 1_545 ? O5 Cd2 O7 74.24(13) 1_545 1_545 ? N4 Cd2 O7 77.24(16) . 1_545 ? O4 Cd2 N3 106.97(17) . . ? O6 Cd2 N3 85.73(17) 2_567 . ? O5 Cd2 N3 169.66(16) 1_545 . ? N4 Cd2 N3 70.72(17) . . ? O7 Cd2 N3 98.88(16) 1_545 . ? C1 O2 Cd1 113.8(3) . 2_556 ? C1 O2 Cd1 123.9(3) . . ? Cd1 O2 Cd1 100.92(14) 2_556 . ? C26 N2 C27 117.1(5) . . ? C26 N2 Cd1 127.4(4) . . ? C27 N2 Cd1 115.5(4) . . ? C8 C2 C4 118.5(5) . . ? C8 C2 C1 115.8(4) . . ? C4 C2 C1 125.7(4) . . ? C3 O3 Cd1 124.4(3) . . ? C29 N3 C40 120.4(5) . . ? C29 N3 Cd2 125.2(4) . . ? C40 N3 Cd2 114.4(4) . . ? O4 C3 O3 125.2(5) . . ? O4 C3 C4 116.5(5) . . ? O3 C3 C4 118.2(4) . . ? C3 O4 Cd2 117.0(4) . . ? C38 N4 C39 117.9(5) . . ? C38 N4 Cd2 125.4(4) . . ? C39 N4 Cd2 116.6(4) . . ? C5 C4 C2 119.9(5) . . ? C5 C4 C3 117.0(5) . . ? C2 C4 C3 122.9(4) . . ? C9 O5 Cd2 130.3(3) . 1_565 ? C6 C5 C4 121.2(5) . . ? C6 C5 H5 119.4 . . ? C4 C5 H5 119.4 . . ? C9 O6 Cd2 113.4(4) . 2_567 ? C5 C6 C7 118.2(5) . . ? C5 C6 H6 120.9 . . ? C7 C6 H6 120.9 . . ? C11 O7 Cd2 123.1(3) . 1_565 ? C8 C7 C6 121.2(5) . . ? C8 C7 S1 119.2(4) . . ? C6 C7 S1 119.6(4) . . ? C11 O8 Cd1 100.4(3) . 1_565 ? C7 C8 C2 120.9(5) . . ? C7 C8 H8 119.5 . . ? C2 C8 H8 119.5 . . ? O5 C9 O6 123.4(5) . . ? O5 C9 C10 120.4(5) . . ? O6 C9 C10 116.2(5) . . ? C12 C10 C16 118.4(5) . . ? C12 C10 C9 124.5(4) . . ? C16 C10 C9 117.0(4) . . ? O7 C11 O8 123.2(5) . . ? O7 C11 C12 120.2(5) . . ? O8 C11 C12 116.2(5) . . ? C13 C12 C10 120.1(4) . . ? C13 C12 C11 115.7(4) . . ? C10 C12 C11 124.1(5) . . ? C12 C13 C14 121.5(5) . . ? C12 C13 H13 119.3 . . ? C14 C13 H13 119.3 . . ? C15 C14 C13 118.7(5) . . ? C15 C14 H14 120.7 . . ? C13 C14 H14 120.7 . . ? C14 C15 C16 121.4(5) . . ? C14 C15 S1 120.0(4) . . ? C16 C15 S1 118.5(4) . . ? C15 C16 C10 119.9(5) . . ? C15 C16 H16 120.0 . . ? C10 C16 H16 120.0 . . ? N1 C17 C18 123.6(7) . . ? N1 C17 H17 118.2 . . ? C18 C17 H17 118.2 . . ? C19 C18 C17 118.4(7) . . ? C19 C18 H18 120.8 . . ? C17 C18 H18 120.8 . . ? C18 C19 C20 120.8(6) . . ? C18 C19 H19 119.6 . . ? C20 C19 H19 119.6 . . ? C19 C20 C28 115.2(6) . . ? C19 C20 C21 124.4(6) . . ? C28 C20 C21 120.4(7) . . ? C22 C21 C20 120.5(7) . . ? C22 C21 H21 119.7 . . ? C20 C21 H21 119.7 . . ? C21 C22 C23 122.1(7) . . ? C21 C22 H22 119.0 . . ? C23 C22 H22 119.0 . . ? C24 C23 C27 115.9(6) . . ? C24 C23 C22 123.7(6) . . ? C27 C23 C22 120.4(7) . . ? C25 C24 C23 121.8(6) . . ? C25 C24 H24 119.1 . . ? C23 C24 H24 119.1 . . ? C24 C25 C26 116.6(7) . . ? C24 C25 H25 121.7 . . ? C26 C25 H25 121.7 . . ? N2 C26 C25 124.9(7) . . ? N2 C26 H26 117.6 . . ? C25 C26 H26 117.6 . . ? N2 C27 C23 123.7(6) . . ? N2 C27 C28 117.3(5) . . ? C23 C27 C28 119.0(5) . . ? N1 C28 C20 123.4(6) . . ? N1 C28 C27 119.1(5) . . ? C20 C28 C27 117.5(6) . . ? N3 C29 C30 121.1(7) . . ? N3 C29 H29 119.4 . . ? C30 C29 H29 119.4 . . ? C31 C30 C29 120.2(7) . . ? C31 C30 H30 119.9 . . ? C29 C30 H30 119.9 . . ? C30 C31 C32 120.3(7) . . ? C30 C31 H31 119.8 . . ? C32 C31 H31 119.8 . . ? C31 C32 C40 118.6(7) . . ? C31 C32 C33 124.6(7) . . ? C40 C32 C33 116.9(7) . . ? C34 C33 C32 121.3(7) . . ? C34 C33 H33 119.4 . . ? C32 C33 H33 119.4 . . ? C33 C34 C35 122.7(7) . . ? C33 C34 H34 118.7 . . ? C35 C34 H34 118.7 . . ? C36 C35 C34 123.8(7) . . ? C36 C35 C39 117.3(6) . . ? C34 C35 C39 118.8(7) . . ? C37 C36 C35 120.0(6) . . ? C37 C36 H36 120.0 . . ? C35 C36 H36 120.0 . . ? C36 C37 C38 119.3(7) . . ? C36 C37 H37 120.3 . . ? C38 C37 H37 120.3 . . ? N4 C38 C37 123.0(6) . . ? N4 C38 H38 118.5 . . ? C37 C38 H38 118.5 . . ? N4 C39 C35 122.4(6) . . ? N4 C39 C40 118.7(5) . . ? C35 C39 C40 118.9(6) . . ? N3 C40 C39 119.3(5) . . ? N3 C40 C32 119.3(6) . . ? C39 C40 C32 121.3(6) . . ? H11A O11 H11B 104.2 . . ? H12A O12 H12B 107.4 . . ? H13A O13 H13B 104.1 . . ? H14A O14 H14B 107.8 . . ? H15A O15 H15B 109.0 . . ? 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 O8 Cd1 N1 C17 -79.4(12) 1_545 . . . ? O2 Cd1 N1 C17 94.7(5) 2_556 . . . ? O3 Cd1 N1 C17 -53.5(5) . . . . ? N2 Cd1 N1 C17 180.0(5) . . . . ? O2 Cd1 N1 C17 16.0(5) . . . . ? O8 Cd1 N1 C28 98.4(11) 1_545 . . . ? O2 Cd1 N1 C28 -87.6(4) 2_556 . . . ? O3 Cd1 N1 C28 124.2(4) . . . . ? N2 Cd1 N1 C28 -2.3(4) . . . . ? O2 Cd1 N1 C28 -166.3(4) . . . . ? O1 C1 O2 Cd1 -29.2(7) . . . 2_556 ? C2 C1 O2 Cd1 144.8(4) . . . 2_556 ? O1 C1 O2 Cd1 93.9(6) . . . . ? C2 C1 O2 Cd1 -92.0(5) . . . . ? O8 Cd1 O2 C1 129.6(4) 1_545 . . . ? O2 Cd1 O2 C1 -128.7(5) 2_556 . . . ? O3 Cd1 O2 C1 33.5(4) . . . . ? N1 Cd1 O2 C1 -42.0(4) . . . . ? N2 Cd1 O2 C1 -98.1(6) . . . . ? O8 Cd1 O2 Cd1 -101.63(17) 1_545 . . 2_556 ? O2 Cd1 O2 Cd1 0.0 2_556 . . 2_556 ? O3 Cd1 O2 Cd1 162.24(18) . . . 2_556 ? N1 Cd1 O2 Cd1 86.77(17) . . . 2_556 ? N2 Cd1 O2 Cd1 30.7(5) . . . 2_556 ? O8 Cd1 N2 C26 8.9(5) 1_545 . . . ? O2 Cd1 N2 C26 -89.4(5) 2_556 . . . ? O3 Cd1 N2 C26 115.2(5) . . . . ? N1 Cd1 N2 C26 -179.8(5) . . . . ? O2 Cd1 N2 C26 -119.5(6) . . . . ? O8 Cd1 N2 C27 -169.6(4) 1_545 . . . ? O2 Cd1 N2 C27 92.1(4) 2_556 . . . ? O3 Cd1 N2 C27 -63.3(4) . . . . ? N1 Cd1 N2 C27 1.7(4) . . . . ? O2 Cd1 N2 C27 62.0(7) . . . . ? O1 C1 C2 C8 47.4(7) . . . . ? O2 C1 C2 C8 -127.1(5) . . . . ? O1 C1 C2 C4 -133.2(5) . . . . ? O2 C1 C2 C4 52.2(7) . . . . ? O8 Cd1 O3 C3 -8.5(4) 1_545 . . . ? O2 Cd1 O3 C3 103.5(4) 2_556 . . . ? N1 Cd1 O3 C3 175.2(4) . . . . ? N2 Cd1 O3 C3 -124.8(4) . . . . ? O2 Cd1 O3 C3 70.8(4) . . . . ? O4 Cd2 N3 C29 15.7(6) . . . . ? O6 Cd2 N3 C29 -68.3(5) 2_567 . . . ? O5 Cd2 N3 C29 159.1(8) 1_545 . . . ? N4 Cd2 N3 C29 -175.3(6) . . . . ? O7 Cd2 N3 C29 111.6(5) 1_545 . . . ? O4 Cd2 N3 C40 -165.3(4) . . . . ? O6 Cd2 N3 C40 110.8(4) 2_567 . . . ? O5 Cd2 N3 C40 -21.9(11) 1_545 . . . ? N4 Cd2 N3 C40 3.7(4) . . . . ? O7 Cd2 N3 C40 -69.4(4) 1_545 . . . ? Cd1 O3 C3 O4 81.8(6) . . . . ? Cd1 O3 C3 C4 -100.5(5) . . . . ? O3 C3 O4 Cd2 0.2(7) . . . . ? C4 C3 O4 Cd2 -177.5(3) . . . . ? O6 Cd2 O4 C3 120.6(4) 2_567 . . . ? O5 Cd2 O4 C3 -137.3(4) 1_545 . . . ? N4 Cd2 O4 C3 -39.3(11) . . . . ? O7 Cd2 O4 C3 -63.7(4) 1_545 . . . ? N3 Cd2 O4 C3 36.5(5) . . . . ? O4 Cd2 N4 C38 -101.0(10) . . . . ? O6 Cd2 N4 C38 99.7(6) 2_567 . . . ? O5 Cd2 N4 C38 -4.8(6) 1_545 . . . ? O7 Cd2 N4 C38 -76.0(6) 1_545 . . . ? N3 Cd2 N4 C38 179.7(6) . . . . ? O4 Cd2 N4 C39 74.6(10) . . . . ? O6 Cd2 N4 C39 -84.8(4) 2_567 . . . ? O5 Cd2 N4 C39 170.8(4) 1_545 . . . ? O7 Cd2 N4 C39 99.6(4) 1_545 . . . ? N3 Cd2 N4 C39 -4.7(4) . . . . ? C8 C2 C4 C5 -0.7(7) . . . . ? C1 C2 C4 C5 180.0(5) . . . . ? C8 C2 C4 C3 -176.0(4) . . . . ? C1 C2 C4 C3 4.6(8) . . . . ? O4 C3 C4 C5 25.7(7) . . . . ? O3 C3 C4 C5 -152.2(5) . . . . ? O4 C3 C4 C2 -158.9(5) . . . . ? O3 C3 C4 C2 23.3(7) . . . . ? C2 C4 C5 C6 1.0(8) . . . . ? C3 C4 C5 C6 176.7(5) . . . . ? C4 C5 C6 C7 -0.7(9) . . . . ? C5 C6 C7 C8 0.0(8) . . . . ? C5 C6 C7 S1 178.8(4) . . . . ? O9 S1 C7 C8 38.9(5) . . . . ? O10 S1 C7 C8 169.4(4) . . . . ? C15 S1 C7 C8 -75.6(4) . . . . ? O9 S1 C7 C6 -140.0(4) . . . . ? O10 S1 C7 C6 -9.5(5) . . . . ? C15 S1 C7 C6 105.5(5) . . . . ? C6 C7 C8 C2 0.4(8) . . . . ? S1 C7 C8 C2 -178.5(4) . . . . ? C4 C2 C8 C7 0.0(7) . . . . ? C1 C2 C8 C7 179.4(4) . . . . ? Cd2 O5 C9 O6 91.9(6) 1_565 . . . ? Cd2 O5 C9 C10 -89.7(5) 1_565 . . . ? Cd2 O6 C9 O5 10.7(6) 2_567 . . . ? Cd2 O6 C9 C10 -167.8(3) 2_567 . . . ? O5 C9 C10 C12 22.8(7) . . . . ? O6 C9 C10 C12 -158.7(5) . . . . ? O5 C9 C10 C16 -152.9(5) . . . . ? O6 C9 C10 C16 25.6(7) . . . . ? Cd2 O7 C11 O8 89.8(6) 1_565 . . . ? Cd2 O7 C11 C12 -97.3(5) 1_565 . . . ? Cd1 O8 C11 O7 16.3(6) 1_565 . . . ? Cd1 O8 C11 C12 -156.8(4) 1_565 . . . ? C16 C10 C12 C13 -2.3(7) . . . . ? C9 C10 C12 C13 -177.9(5) . . . . ? C16 C10 C12 C11 -177.8(4) . . . . ? C9 C10 C12 C11 6.6(8) . . . . ? O7 C11 C12 C13 -127.1(5) . . . . ? O8 C11 C12 C13 46.2(7) . . . . ? O7 C11 C12 C10 48.6(7) . . . . ? O8 C11 C12 C10 -138.1(5) . . . . ? C10 C12 C13 C14 2.1(8) . . . . ? C11 C12 C13 C14 178.0(5) . . . . ? C12 C13 C14 C15 -0.4(8) . . . . ? C13 C14 C15 C16 -1.2(8) . . . . ? C13 C14 C15 S1 176.5(4) . . . . ? O9 S1 C15 C14 -12.8(5) . . . . ? O10 S1 C15 C14 -143.1(4) . . . . ? C7 S1 C15 C14 102.0(4) . . . . ? O9 S1 C15 C16 164.9(4) . . . . ? O10 S1 C15 C16 34.7(5) . . . . ? C7 S1 C15 C16 -80.2(4) . . . . ? C14 C15 C16 C10 1.0(8) . . . . ? S1 C15 C16 C10 -176.7(4) . . . . ? C12 C10 C16 C15 0.7(7) . . . . ? C9 C10 C16 C15 176.7(4) . . . . ? C28 N1 C17 C18 -0.2(10) . . . . ? Cd1 N1 C17 C18 177.5(5) . . . . ? N1 C17 C18 C19 -0.1(11) . . . . ? C17 C18 C19 C20 0.5(11) . . . . ? C18 C19 C20 C28 -0.5(10) . . . . ? C18 C19 C20 C21 178.9(7) . . . . ? C19 C20 C21 C22 -178.9(7) . . . . ? C28 C20 C21 C22 0.4(10) . . . . ? C20 C21 C22 C23 -0.6(12) . . . . ? C21 C22 C23 C24 179.7(7) . . . . ? C21 C22 C23 C27 0.0(11) . . . . ? C27 C23 C24 C25 -0.8(11) . . . . ? C22 C23 C24 C25 179.4(7) . . . . ? C23 C24 C25 C26 -0.6(11) . . . . ? C27 N2 C26 C25 -2.2(10) . . . . ? Cd1 N2 C26 C25 179.3(5) . . . . ? C24 C25 C26 N2 2.2(11) . . . . ? C26 N2 C27 C23 0.5(9) . . . . ? Cd1 N2 C27 C23 179.2(5) . . . . ? C26 N2 C27 C28 -179.6(5) . . . . ? Cd1 N2 C27 C28 -1.0(6) . . . . ? C24 C23 C27 N2 0.9(9) . . . . ? C22 C23 C27 N2 -179.4(6) . . . . ? C24 C23 C27 C28 -178.9(6) . . . . ? C22 C23 C27 C28 0.8(9) . . . . ? C17 N1 C28 C20 0.2(9) . . . . ? Cd1 N1 C28 C20 -177.7(4) . . . . ? C17 N1 C28 C27 -179.4(5) . . . . ? Cd1 N1 C28 C27 2.7(7) . . . . ? C19 C20 C28 N1 0.2(9) . . . . ? C21 C20 C28 N1 -179.3(6) . . . . ? C19 C20 C28 C27 179.8(5) . . . . ? C21 C20 C28 C27 0.3(9) . . . . ? N2 C27 C28 N1 -1.1(8) . . . . ? C23 C27 C28 N1 178.7(5) . . . . ? N2 C27 C28 C20 179.2(5) . . . . ? C23 C27 C28 C20 -0.9(8) . . . . ? C40 N3 C29 C30 -0.1(10) . . . . ? Cd2 N3 C29 C30 178.9(5) . . . . ? N3 C29 C30 C31 1.3(11) . . . . ? C29 C30 C31 C32 -1.3(12) . . . . ? C30 C31 C32 C40 0.1(11) . . . . ? C30 C31 C32 C33 -179.0(7) . . . . ? C31 C32 C33 C34 179.0(8) . . . . ? C40 C32 C33 C34 -0.2(10) . . . . ? C32 C33 C34 C35 -1.0(12) . . . . ? C33 C34 C35 C36 -178.1(7) . . . . ? C33 C34 C35 C39 -0.4(11) . . . . ? C34 C35 C36 C37 176.6(7) . . . . ? C39 C35 C36 C37 -1.1(11) . . . . ? C35 C36 C37 C38 -0.5(12) . . . . ? C39 N4 C38 C37 -2.7(11) . . . . ? Cd2 N4 C38 C37 172.8(6) . . . . ? C36 C37 C38 N4 2.5(13) . . . . ? C38 N4 C39 C35 1.0(9) . . . . ? Cd2 N4 C39 C35 -174.9(5) . . . . ? C38 N4 C39 C40 -178.8(6) . . . . ? Cd2 N4 C39 C40 5.3(7) . . . . ? C36 C35 C39 N4 0.9(9) . . . . ? C34 C35 C39 N4 -177.0(6) . . . . ? C36 C35 C39 C40 -179.3(6) . . . . ? C34 C35 C39 C40 2.9(9) . . . . ? C29 N3 C40 C39 176.5(6) . . . . ? Cd2 N3 C40 C39 -2.6(7) . . . . ? C29 N3 C40 C32 -1.1(9) . . . . ? Cd2 N3 C40 C32 179.9(4) . . . . ? N4 C39 C40 N3 -1.8(8) . . . . ? C35 C39 C40 N3 178.4(5) . . . . ? N4 C39 C40 C32 175.8(5) . . . . ? C35 C39 C40 C32 -4.1(9) . . . . ? C31 C32 C40 N3 1.1(9) . . . . ? C33 C32 C40 N3 -179.8(6) . . . . ? C31 C32 C40 C39 -176.5(6) . . . . ? C33 C32 C40 C39 2.7(9) . . . . ? 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 O11 H11A O6 0.93 1.97 2.824(9) 152.2 . O11 H11B O15 0.93 2.04 2.96(3) 174.3 . O12 H12A O1 0.86 2.17 2.760(12) 125.7 . O12 H12B O12 0.94 2.28 2.96(2) 129.0 2_566 O13 H13A O13 0.86 2.26 2.64(3) 106.8 2_467 O13 H13B O14 0.88 1.99 2.81(2) 155.4 . O14 H14A O11 0.90 2.02 2.705(16) 132.2 . O15 H15A O12 0.90 1.97 2.84(3) 163.1 . O15 H15B O14 0.88 1.83 2.63(3) 149.0 2_567 _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.016 _refine_diff_density_min -0.781 _refine_diff_density_rms 0.111 data_compound3 _database_code_depnum_ccdc_archive 'CCDC 894379' #TrackingRef '894379.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H24 Cd2 N4 O11 S' _chemical_formula_weight 993.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.8489(7) _cell_length_b 16.7123(6) _cell_length_c 18.8636(11) _cell_angle_alpha 90 _cell_angle_beta 105.170(4) _cell_angle_gamma 90 _cell_volume 3605.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8330 _cell_measurement_theta_min 2.1574 _cell_measurement_theta_max 27.4835 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.830 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1968 _exptl_absorpt_coefficient_mu 1.310 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6065 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details '(CrystalClear; Rigaku, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type \w _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27780 _diffrn_reflns_av_R_equivalents 0.0376 _diffrn_reflns_av_sigmaI/netI 0.0426 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 27.47 _reflns_number_total 8229 _reflns_number_gt 6858 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _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^)+(0.0445P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8229 _refine_ls_number_parameters 525 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0519 _refine_ls_R_factor_gt 0.0394 _refine_ls_wR_factor_ref 0.0973 _refine_ls_wR_factor_gt 0.0888 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.077 _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 0.02556(2) 0.443487(14) 0.109917(13) 0.03468(8) Uani 1 1 d . . . S1 S 0.33631(8) 0.08829(5) -0.01892(4) 0.03432(18) Uani 1 1 d . . . O1 O 0.3858(2) 0.37211(16) 0.10782(14) 0.0495(7) Uani 1 1 d . . . N1 N 0.5690(3) 0.5313(2) 0.19241(16) 0.0436(7) Uani 1 1 d . . . C1 C 0.2542(3) 0.17788(18) -0.02626(16) 0.0310(7) Uani 1 1 d . . . Cd2 Cd 0.37674(2) 0.486582(15) 0.173657(14) 0.03919(9) Uani 1 1 d . . . O2 O 0.2232(2) 0.44051(14) 0.06823(13) 0.0441(6) Uani 1 1 d . . . N2 N 0.3692(2) 0.61754(18) 0.13936(16) 0.0406(7) Uani 1 1 d . . . C2 C 0.2971(3) 0.24059(19) 0.02062(16) 0.0322(7) Uani 1 1 d . . . H2 H 0.3675 0.2350 0.0563 0.039 Uiso 1 1 calc R . . O3 O 0.0680(3) 0.44026(15) -0.10049(14) 0.0518(7) Uani 1 1 d . . . N3 N 0.0491(3) 0.30765(17) 0.14396(15) 0.0402(7) Uani 1 1 d . . . C3 C 0.2352(3) 0.31229(18) 0.01473(16) 0.0297(6) Uani 1 1 d . . . O4 O -0.0166(2) 0.40614(17) -0.01332(14) 0.0496(7) Uani 1 1 d . . . N4 N -0.1612(3) 0.3838(2) 0.09258(16) 0.0444(7) Uani 1 1 d . . . C4 C 0.1284(3) 0.31993(19) -0.03853(16) 0.0312(7) Uani 1 1 d . . . O5 O 0.4621(2) -0.03779(18) 0.25662(13) 0.0489(6) Uani 1 1 d . . . C5 C 0.0866(3) 0.2560(2) -0.08488(17) 0.0372(7) Uani 1 1 d . . . H5 H 0.0154 0.2608 -0.1200 0.045 Uiso 1 1 calc R . . O6 O 0.3032(2) -0.02224(17) 0.29344(12) 0.0454(6) Uani 1 1 d . . . C6 C 0.1489(3) 0.1850(2) -0.07989(17) 0.0367(7) Uani 1 1 d . . . H6 H 0.1207 0.1429 -0.1119 0.044 Uiso 1 1 calc R . . O7 O 0.1370(2) -0.17169(16) 0.19478(14) 0.0512(7) Uani 1 1 d . . . C7 C 0.0559(3) 0.3952(2) -0.04971(17) 0.0370(8) Uani 1 1 d . . . O8 O 0.0509(2) -0.05777(16) 0.21219(14) 0.0482(6) Uani 1 1 d . . . C8 C 0.2845(3) 0.37974(19) 0.06642(17) 0.0333(7) Uani 1 1 d . . . O9 O 0.4564(2) 0.10700(15) 0.01586(14) 0.0449(6) Uani 1 1 d . . . C9 C 0.2798(3) 0.02961(19) 0.04234(17) 0.0335(7) Uani 1 1 d . . . O10 O 0.3052(2) 0.04992(14) -0.08951(13) 0.0458(6) Uani 1 1 d . . . C10 C 0.3389(3) 0.02433(19) 0.11586(17) 0.0342(7) Uani 1 1 d . . . H10 H 0.4116 0.0485 0.1332 0.041 Uiso 1 1 calc R . . O11 O 0.0028(5) -0.2479(3) 0.2828(2) 0.147(2) Uani 1 1 d . . . C11 C 0.2885(3) -0.01772(19) 0.16398(17) 0.0317(7) Uani 1 1 d . . . C12 C 0.1740(3) -0.0084(2) 0.01480(19) 0.0395(8) Uani 1 1 d . . . H12 H 0.1360 -0.0051 -0.0349 0.047 Uiso 1 1 calc R . . C13 C 0.1251(3) -0.0515(2) 0.06206(18) 0.0395(8) Uani 1 1 d . . . H13 H 0.0546 -0.0782 0.0437 0.047 Uiso 1 1 calc R . . C14 C 0.1805(3) -0.05515(19) 0.13694(17) 0.0331(7) Uani 1 1 d . . . C15 C 0.1199(3) -0.0997(2) 0.18598(17) 0.0359(7) Uani 1 1 d . . . C16 C 0.3560(3) -0.0259(2) 0.24281(18) 0.0355(7) Uani 1 1 d . . . C17 C 0.6668(4) 0.4893(3) 0.2200(2) 0.0598(11) Uani 1 1 d . . . H17 H 0.6606 0.4349 0.2285 0.072 Uiso 1 1 calc R . . C18 C 0.7750(4) 0.5232(4) 0.2363(2) 0.0732(15) Uani 1 1 d . . . H18 H 0.8410 0.4916 0.2540 0.088 Uiso 1 1 calc R . . C19 C 0.7867(4) 0.6026(4) 0.2269(2) 0.0721(16) Uani 1 1 d . . . H19 H 0.8608 0.6256 0.2376 0.086 Uiso 1 1 calc R . . C20 C 0.6872(4) 0.6504(3) 0.2010(2) 0.0562(11) Uani 1 1 d . . . C21 C 0.6889(5) 0.7357(3) 0.1931(2) 0.0735(15) Uani 1 1 d . . . H21 H 0.7601 0.7625 0.2073 0.088 Uiso 1 1 calc R . . C22 C 0.5914(5) 0.7779(3) 0.1661(3) 0.0780(16) Uani 1 1 d . . . H22 H 0.5961 0.8331 0.1608 0.094 Uiso 1 1 calc R . . C23 C 0.4798(4) 0.7391(2) 0.1451(2) 0.0548(10) Uani 1 1 d . . . C24 C 0.3746(5) 0.7804(3) 0.1151(2) 0.0714(14) Uani 1 1 d . . . H24 H 0.3754 0.8354 0.1076 0.086 Uiso 1 1 calc R . . C25 C 0.2713(5) 0.7394(3) 0.0971(2) 0.0698(13) Uani 1 1 d . . . H25 H 0.2015 0.7658 0.0761 0.084 Uiso 1 1 calc R . . C26 C 0.2721(4) 0.6581(3) 0.1105(2) 0.0558(10) Uani 1 1 d . . . H26 H 0.2013 0.6307 0.0987 0.067 Uiso 1 1 calc R . . C27 C 0.5786(3) 0.6111(2) 0.18316(18) 0.0413(8) Uani 1 1 d . . . C28 C 0.4729(3) 0.6562(2) 0.15560(17) 0.0393(8) Uani 1 1 d . . . C29 C 0.1499(4) 0.2706(2) 0.1707(2) 0.0502(9) Uani 1 1 d . . . H29 H 0.2181 0.3009 0.1812 0.060 Uiso 1 1 calc R . . C30 C 0.1591(5) 0.1885(3) 0.1839(2) 0.0685(14) Uani 1 1 d . . . H30 H 0.2319 0.1649 0.2026 0.082 Uiso 1 1 calc R . . C31 C 0.0605(6) 0.1436(3) 0.1691(2) 0.0773(17) Uani 1 1 d . . . H31 H 0.0651 0.0886 0.1770 0.093 Uiso 1 1 calc R . . C32 C -0.0480(5) 0.1805(2) 0.1420(2) 0.0584(12) Uani 1 1 d . . . C33 C -0.1564(6) 0.1377(3) 0.1269(3) 0.0831(19) Uani 1 1 d . . . H33 H -0.1550 0.0829 0.1356 0.100 Uiso 1 1 calc R . . C34 C -0.2589(6) 0.1738(4) 0.1009(3) 0.090(2) Uani 1 1 d . . . H34 H -0.3272 0.1437 0.0909 0.108 Uiso 1 1 calc R . . C35 C -0.2657(4) 0.2586(3) 0.0878(2) 0.0664(14) Uani 1 1 d . . . C36 C -0.3704(5) 0.2998(5) 0.0608(3) 0.091(2) Uani 1 1 d . . . H36 H -0.4410 0.2722 0.0503 0.109 Uiso 1 1 calc R . . C37 C -0.3698(4) 0.3795(5) 0.0500(3) 0.0852(19) Uani 1 1 d . . . H37 H -0.4400 0.4065 0.0317 0.102 Uiso 1 1 calc R . . C38 C -0.2637(4) 0.4222(3) 0.0661(2) 0.0618(12) Uani 1 1 d . . . H38 H -0.2642 0.4771 0.0585 0.074 Uiso 1 1 calc R . . C39 C -0.1614(3) 0.3045(3) 0.10261(18) 0.0471(9) Uani 1 1 d . . . C40 C -0.0506(4) 0.2635(2) 0.12995(18) 0.0440(9) Uani 1 1 d . . . H11A H 0.0543 -0.2304 0.2534 0.16(3) Uiso 1 1 d R . . H11B H 0.0201 -0.2170 0.3237 0.16(3) Uiso 1 1 d 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 0.03318(14) 0.02970(14) 0.03756(15) 0.00067(9) 0.00287(11) 0.00164(9) S1 0.0408(5) 0.0264(4) 0.0374(4) 0.0017(3) 0.0131(4) 0.0018(3) O1 0.0345(13) 0.0453(15) 0.0594(16) -0.0227(12) -0.0043(12) 0.0036(11) N1 0.0347(16) 0.0510(19) 0.0463(17) -0.0033(14) 0.0124(14) -0.0014(14) C1 0.0351(17) 0.0264(15) 0.0321(16) 0.0003(12) 0.0096(13) 0.0004(13) Cd2 0.03997(16) 0.03576(15) 0.04210(16) -0.00906(10) 0.01117(12) -0.01051(11) O2 0.0450(14) 0.0338(14) 0.0467(14) -0.0101(11) -0.0003(12) 0.0041(11) N2 0.0352(15) 0.0390(16) 0.0476(17) -0.0044(13) 0.0107(13) -0.0046(13) C2 0.0311(16) 0.0297(16) 0.0326(16) 0.0000(13) 0.0026(13) -0.0008(13) O3 0.0710(19) 0.0386(15) 0.0454(15) 0.0089(11) 0.0149(13) 0.0190(13) N3 0.0489(18) 0.0326(15) 0.0401(16) 0.0017(12) 0.0133(14) 0.0009(13) C3 0.0296(15) 0.0281(16) 0.0301(15) -0.0015(12) 0.0053(13) -0.0012(13) O4 0.0357(13) 0.0607(18) 0.0503(15) -0.0137(13) 0.0078(11) 0.0082(12) N4 0.0346(16) 0.057(2) 0.0411(16) -0.0027(14) 0.0095(13) -0.0017(15) C4 0.0329(16) 0.0302(16) 0.0295(16) -0.0013(13) 0.0063(13) 0.0008(13) O5 0.0312(13) 0.0721(19) 0.0404(14) 0.0043(13) 0.0036(11) 0.0002(13) C5 0.0346(17) 0.0378(19) 0.0326(17) -0.0015(14) -0.0028(14) 0.0007(14) O6 0.0368(13) 0.0653(18) 0.0333(13) 0.0007(12) 0.0077(11) 0.0033(12) C6 0.0392(18) 0.0306(17) 0.0355(17) -0.0071(14) 0.0014(14) -0.0022(14) O7 0.0620(18) 0.0384(14) 0.0554(16) 0.0029(12) 0.0196(14) -0.0073(13) C7 0.0350(18) 0.0373(19) 0.0326(17) -0.0052(14) -0.0019(14) 0.0051(14) O8 0.0374(14) 0.0579(18) 0.0507(15) -0.0035(12) 0.0140(12) -0.0007(12) C8 0.0321(16) 0.0306(17) 0.0346(17) -0.0052(13) 0.0040(14) -0.0027(13) O9 0.0373(13) 0.0385(14) 0.0596(16) 0.0057(12) 0.0139(12) 0.0013(11) C9 0.0395(18) 0.0245(15) 0.0365(17) 0.0033(13) 0.0101(14) 0.0030(14) O10 0.0692(18) 0.0346(13) 0.0376(13) -0.0052(10) 0.0210(12) 0.0018(12) C10 0.0319(17) 0.0309(17) 0.0372(17) -0.0002(13) 0.0046(14) -0.0031(13) O11 0.172(5) 0.196(6) 0.078(3) -0.029(3) 0.040(3) -0.138(4) C11 0.0296(16) 0.0302(17) 0.0327(16) -0.0006(13) 0.0035(13) 0.0008(13) C12 0.0401(19) 0.0390(19) 0.0350(17) 0.0008(14) 0.0020(15) -0.0028(15) C13 0.0329(17) 0.042(2) 0.0398(18) -0.0032(15) 0.0033(15) -0.0098(15) C14 0.0321(17) 0.0298(16) 0.0363(17) -0.0037(13) 0.0071(14) -0.0018(13) C15 0.0319(17) 0.0388(19) 0.0344(17) -0.0028(14) 0.0043(14) -0.0079(15) C16 0.0326(17) 0.0327(17) 0.0376(18) 0.0007(14) 0.0028(14) -0.0078(14) C17 0.051(3) 0.069(3) 0.061(3) 0.001(2) 0.018(2) 0.016(2) C18 0.036(2) 0.123(5) 0.058(3) 0.004(3) 0.010(2) 0.015(3) C19 0.033(2) 0.133(5) 0.052(3) -0.007(3) 0.0144(19) -0.021(3) C20 0.047(2) 0.082(3) 0.043(2) -0.007(2) 0.0182(18) -0.025(2) C21 0.082(4) 0.077(4) 0.065(3) -0.010(3) 0.026(3) -0.055(3) C22 0.114(5) 0.059(3) 0.066(3) -0.003(2) 0.031(3) -0.041(3) C23 0.078(3) 0.041(2) 0.049(2) -0.0009(18) 0.023(2) -0.011(2) C24 0.116(4) 0.040(2) 0.066(3) 0.002(2) 0.038(3) 0.011(3) C25 0.079(3) 0.067(3) 0.066(3) 0.007(2) 0.024(3) 0.028(3) C26 0.050(2) 0.066(3) 0.052(2) -0.005(2) 0.0152(19) 0.006(2) C27 0.0393(19) 0.050(2) 0.0374(18) -0.0051(16) 0.0146(15) -0.0121(16) C28 0.045(2) 0.041(2) 0.0334(17) -0.0053(14) 0.0131(15) -0.0077(16) C29 0.056(2) 0.046(2) 0.047(2) 0.0068(17) 0.0120(18) 0.0124(19) C30 0.099(4) 0.054(3) 0.059(3) 0.023(2) 0.033(3) 0.034(3) C31 0.150(5) 0.036(2) 0.062(3) 0.010(2) 0.055(3) 0.011(3) C32 0.103(4) 0.036(2) 0.043(2) -0.0025(17) 0.032(2) -0.018(2) C33 0.145(6) 0.060(3) 0.059(3) -0.019(2) 0.054(4) -0.051(4) C34 0.122(5) 0.097(5) 0.063(3) -0.028(3) 0.046(3) -0.077(4) C35 0.065(3) 0.094(4) 0.044(2) -0.016(2) 0.022(2) -0.040(3) C36 0.054(3) 0.158(7) 0.065(3) -0.019(4) 0.023(3) -0.046(4) C37 0.036(2) 0.155(6) 0.064(3) -0.007(4) 0.013(2) 0.006(3) C38 0.042(2) 0.092(4) 0.053(2) -0.003(2) 0.0151(19) 0.006(2) C39 0.050(2) 0.059(3) 0.0346(18) -0.0110(17) 0.0150(16) -0.0209(19) C40 0.060(2) 0.0372(19) 0.0384(19) -0.0035(15) 0.0199(17) -0.0127(18) _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 O3 2.221(2) 3_565 ? Cd1 O4 2.331(2) . ? Cd1 N3 2.356(3) . ? Cd1 N4 2.371(3) . ? Cd1 O6 2.415(2) 2 ? Cd1 O5 2.503(2) 2 ? S1 O10 1.436(2) . ? S1 O9 1.437(2) . ? S1 C1 1.771(3) . ? S1 C9 1.775(3) . ? O1 C8 1.256(4) . ? O1 Cd2 2.299(2) . ? N1 C17 1.338(5) . ? N1 C27 1.354(5) . ? N1 Cd2 2.334(3) . ? C1 C2 1.379(4) . ? C1 C6 1.391(4) . ? Cd2 O8 2.226(3) 2 ? Cd2 N2 2.277(3) . ? Cd2 O6 2.375(2) 2 ? Cd2 O2 2.442(2) . ? Cd2 C8 2.705(3) . ? O2 C8 1.254(4) . ? N2 C26 1.324(5) . ? N2 C28 1.351(4) . ? C2 C3 1.394(4) . ? C2 H2 0.9300 . ? O3 C7 1.256(4) . ? O3 Cd1 2.221(2) 3_565 ? N3 C29 1.322(5) . ? N3 C40 1.359(5) . ? C3 C4 1.401(4) . ? C3 C8 1.505(4) . ? O4 C7 1.245(4) . ? N4 C39 1.339(5) . ? N4 C38 1.348(5) . ? C4 C5 1.387(4) . ? C4 C7 1.507(4) . ? O5 C16 1.231(4) . ? O5 Cd1 2.503(2) 2_545 ? C5 C6 1.388(5) . ? C5 H5 0.9300 . ? O6 C16 1.274(4) . ? O6 Cd2 2.375(2) 2_545 ? O6 Cd1 2.415(2) 2_545 ? C6 H6 0.9300 . ? O7 C15 1.224(4) . ? O8 C15 1.271(4) . ? O8 Cd2 2.226(3) 2_545 ? C9 C12 1.380(5) . ? C9 C10 1.383(4) . ? C10 C11 1.399(4) . ? C10 H10 0.9300 . ? O11 H11A 0.9705 . ? O11 H11B 0.9059 . ? C11 C14 1.395(4) . ? C11 C16 1.499(4) . ? C12 C13 1.386(5) . ? C12 H12 0.9300 . ? C13 C14 1.395(4) . ? C13 H13 0.9300 . ? C14 C15 1.508(4) . ? C17 C18 1.361(7) . ? C17 H17 0.9300 . ? C18 C19 1.351(8) . ? C18 H18 0.9300 . ? C19 C20 1.402(7) . ? C19 H19 0.9300 . ? C20 C27 1.405(5) . ? C20 C21 1.434(7) . ? C21 C22 1.335(7) . ? C21 H21 0.9300 . ? C22 C23 1.433(6) . ? C22 H22 0.9300 . ? C23 C28 1.405(5) . ? C23 C24 1.407(6) . ? C24 C25 1.366(7) . ? C24 H24 0.9300 . ? C25 C26 1.382(6) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 C28 1.438(5) . ? C29 C30 1.394(6) . ? C29 H29 0.9300 . ? C30 C31 1.354(7) . ? C30 H30 0.9300 . ? C31 C32 1.397(7) . ? C31 H31 0.9300 . ? C32 C40 1.404(5) . ? C32 C33 1.431(7) . ? C33 C34 1.329(8) . ? C33 H33 0.9300 . ? C34 C35 1.438(8) . ? C34 H34 0.9300 . ? C35 C36 1.392(8) . ? C35 C39 1.418(5) . ? C36 C37 1.348(8) . ? C36 H36 0.9300 . ? C37 C38 1.408(7) . ? C37 H37 0.9300 . ? C38 H38 0.9300 . ? C39 C40 1.451(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Cd1 O4 100.50(9) 3_565 . ? O3 Cd1 N3 152.35(10) 3_565 . ? O4 Cd1 N3 89.60(10) . . ? O3 Cd1 N4 85.92(11) 3_565 . ? O4 Cd1 N4 78.53(9) . . ? N3 Cd1 N4 70.83(11) . . ? O3 Cd1 O6 98.99(10) 3_565 2 ? O4 Cd1 O6 137.26(8) . 2 ? N3 Cd1 O6 90.38(10) . 2 ? N4 Cd1 O6 140.67(9) . 2 ? O3 Cd1 O5 82.41(9) 3_565 2 ? O4 Cd1 O5 167.77(9) . 2 ? N3 Cd1 O5 82.80(10) . 2 ? N4 Cd1 O5 89.89(9) . 2 ? O6 Cd1 O5 52.75(8) 2 2 ? O10 S1 O9 120.22(16) . . ? O10 S1 C1 107.61(15) . . ? O9 S1 C1 108.05(15) . . ? O10 S1 C9 107.93(15) . . ? O9 S1 C9 108.69(15) . . ? C1 S1 C9 103.00(15) . . ? C8 O1 Cd2 94.5(2) . . ? C17 N1 C27 118.2(4) . . ? C17 N1 Cd2 127.0(3) . . ? C27 N1 Cd2 114.1(2) . . ? C2 C1 C6 120.7(3) . . ? C2 C1 S1 119.3(2) . . ? C6 C1 S1 119.9(2) . . ? O8 Cd2 N2 124.85(10) 2 . ? O8 Cd2 O1 100.65(10) 2 . ? N2 Cd2 O1 130.56(10) . . ? O8 Cd2 N1 81.17(10) 2 . ? N2 Cd2 N1 72.52(11) . . ? O1 Cd2 N1 99.58(10) . . ? O8 Cd2 O6 82.61(8) 2 2 ? N2 Cd2 O6 99.37(10) . 2 ? O1 Cd2 O6 105.16(9) . 2 ? N1 Cd2 O6 152.49(9) . 2 ? O8 Cd2 O2 134.35(9) 2 . ? N2 Cd2 O2 96.10(9) . . ? O1 Cd2 O2 55.09(8) . . ? N1 Cd2 O2 135.52(9) . . ? O6 Cd2 O2 70.44(8) 2 . ? O8 Cd2 C8 118.78(10) 2 . ? N2 Cd2 C8 116.35(10) . . ? O1 Cd2 C8 27.57(9) . . ? N1 Cd2 C8 120.79(10) . . ? O6 Cd2 C8 86.55(9) 2 . ? O2 Cd2 C8 27.59(8) . . ? C8 O2 Cd2 87.97(19) . . ? C26 N2 C28 119.3(4) . . ? C26 N2 Cd2 125.0(3) . . ? C28 N2 Cd2 115.5(2) . . ? C1 C2 C3 120.3(3) . . ? C1 C2 H2 119.8 . . ? C3 C2 H2 119.8 . . ? C7 O3 Cd1 115.5(2) . 3_565 ? C29 N3 C40 118.1(3) . . ? C29 N3 Cd1 125.9(3) . . ? C40 N3 Cd1 115.8(2) . . ? C2 C3 C4 119.5(3) . . ? C2 C3 C8 119.1(3) . . ? C4 C3 C8 121.4(3) . . ? C7 O4 Cd1 126.2(2) . . ? C39 N4 C38 119.3(4) . . ? C39 N4 Cd1 115.7(2) . . ? C38 N4 Cd1 124.6(3) . . ? C5 C4 C3 119.2(3) . . ? C5 C4 C7 117.3(3) . . ? C3 C4 C7 123.5(3) . . ? C16 O5 Cd1 91.2(2) . 2_545 ? C4 C5 C6 121.4(3) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C16 O6 Cd2 148.2(2) . 2_545 ? C16 O6 Cd1 94.2(2) . 2_545 ? Cd2 O6 Cd1 116.86(9) 2_545 2_545 ? C5 C6 C1 118.8(3) . . ? C5 C6 H6 120.6 . . ? C1 C6 H6 120.6 . . ? O4 C7 O3 124.4(3) . . ? O4 C7 C4 119.7(3) . . ? O3 C7 C4 115.6(3) . . ? C15 O8 Cd2 115.9(2) . 2_545 ? O2 C8 O1 122.1(3) . . ? O2 C8 C3 119.7(3) . . ? O1 C8 C3 118.2(3) . . ? O2 C8 Cd2 64.44(17) . . ? O1 C8 Cd2 57.89(16) . . ? C3 C8 Cd2 172.5(2) . . ? C12 C9 C10 121.3(3) . . ? C12 C9 S1 118.0(3) . . ? C10 C9 S1 120.6(3) . . ? C9 C10 C11 119.5(3) . . ? C9 C10 H10 120.3 . . ? C11 C10 H10 120.3 . . ? H11A O11 H11B 106.2 . . ? C14 C11 C10 119.6(3) . . ? C14 C11 C16 121.5(3) . . ? C10 C11 C16 118.8(3) . . ? C9 C12 C13 119.3(3) . . ? C9 C12 H12 120.4 . . ? C13 C12 H12 120.4 . . ? C12 C13 C14 120.6(3) . . ? C12 C13 H13 119.7 . . ? C14 C13 H13 119.7 . . ? C13 C14 C11 119.6(3) . . ? C13 C14 C15 118.0(3) . . ? C11 C14 C15 122.4(3) . . ? O7 C15 O8 126.2(3) . . ? O7 C15 C14 118.7(3) . . ? O8 C15 C14 115.1(3) . . ? O5 C16 O6 121.6(3) . . ? O5 C16 C11 118.4(3) . . ? O6 C16 C11 120.0(3) . . ? N1 C17 C18 122.6(5) . . ? N1 C17 H17 118.7 . . ? C18 C17 H17 118.7 . . ? C19 C18 C17 120.2(5) . . ? C19 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? C18 C19 C20 119.9(4) . . ? C18 C19 H19 120.0 . . ? C20 C19 H19 120.0 . . ? C27 C20 C19 116.8(5) . . ? C27 C20 C21 118.5(4) . . ? C19 C20 C21 124.7(4) . . ? C22 C21 C20 122.1(4) . . ? C22 C21 H21 119.0 . . ? C20 C21 H21 119.0 . . ? C21 C22 C23 120.7(5) . . ? C21 C22 H22 119.7 . . ? C23 C22 H22 119.7 . . ? C28 C23 C24 117.5(4) . . ? C28 C23 C22 119.4(4) . . ? C24 C23 C22 123.1(5) . . ? C25 C24 C23 119.7(4) . . ? C25 C24 H24 120.1 . . ? C23 C24 H24 120.1 . . ? C24 C25 C26 119.1(5) . . ? C24 C25 H25 120.5 . . ? C26 C25 H25 120.5 . . ? N2 C26 C25 122.8(4) . . ? N2 C26 H26 118.6 . . ? C25 C26 H26 118.6 . . ? N1 C27 C20 122.2(4) . . ? N1 C27 C28 117.9(3) . . ? C20 C27 C28 119.8(4) . . ? N2 C28 C23 121.5(4) . . ? N2 C28 C27 119.0(3) . . ? C23 C28 C27 119.4(4) . . ? N3 C29 C30 123.4(4) . . ? N3 C29 H29 118.3 . . ? C30 C29 H29 118.3 . . ? C31 C30 C29 119.1(5) . . ? C31 C30 H30 120.5 . . ? C29 C30 H30 120.5 . . ? C30 C31 C32 119.5(4) . . ? C30 C31 H31 120.3 . . ? C32 C31 H31 120.3 . . ? C31 C32 C40 118.3(4) . . ? C31 C32 C33 123.0(5) . . ? C40 C32 C33 118.7(5) . . ? C34 C33 C32 122.2(5) . . ? C34 C33 H33 118.9 . . ? C32 C33 H33 118.9 . . ? C33 C34 C35 121.0(5) . . ? C33 C34 H34 119.5 . . ? C35 C34 H34 119.5 . . ? C36 C35 C39 116.9(5) . . ? C36 C35 C34 123.7(5) . . ? C39 C35 C34 119.4(5) . . ? C37 C36 C35 120.3(5) . . ? C37 C36 H36 119.9 . . ? C35 C36 H36 119.9 . . ? C36 C37 C38 120.5(5) . . ? C36 C37 H37 119.7 . . ? C38 C37 H37 119.7 . . ? N4 C38 C37 120.4(5) . . ? N4 C38 H38 119.8 . . ? C37 C38 H38 119.8 . . ? N4 C39 C35 122.7(4) . . ? N4 C39 C40 118.9(3) . . ? C35 C39 C40 118.4(4) . . ? N3 C40 C32 121.6(4) . . ? N3 C40 C39 118.2(3) . . ? C32 C40 C39 120.2(4) . . ? 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 O10 S1 C1 C2 -154.1(2) . . . . ? O9 S1 C1 C2 -22.9(3) . . . . ? C9 S1 C1 C2 92.1(3) . . . . ? O10 S1 C1 C6 24.6(3) . . . . ? O9 S1 C1 C6 155.9(3) . . . . ? C9 S1 C1 C6 -89.2(3) . . . . ? C8 O1 Cd2 O8 134.3(2) . . . 2 ? C8 O1 Cd2 N2 -67.8(2) . . . . ? C8 O1 Cd2 N1 -143.0(2) . . . . ? C8 O1 Cd2 O6 49.2(2) . . . 2 ? C8 O1 Cd2 O2 -3.10(19) . . . . ? C17 N1 Cd2 O8 47.4(3) . . . 2 ? C27 N1 Cd2 O8 -123.0(2) . . . 2 ? C17 N1 Cd2 N2 178.3(3) . . . . ? C27 N1 Cd2 N2 7.9(2) . . . . ? C17 N1 Cd2 O1 -52.0(3) . . . . ? C27 N1 Cd2 O1 137.6(2) . . . . ? C17 N1 Cd2 O6 101.9(4) . . . 2 ? C27 N1 Cd2 O6 -68.4(3) . . . 2 ? C17 N1 Cd2 O2 -101.0(3) . . . . ? C27 N1 Cd2 O2 88.6(3) . . . . ? C17 N1 Cd2 C8 -71.0(3) . . . . ? C27 N1 Cd2 C8 118.7(2) . . . . ? O8 Cd2 O2 C8 -65.4(2) 2 . . . ? N2 Cd2 O2 C8 139.4(2) . . . . ? O1 Cd2 O2 C8 3.10(19) . . . . ? N1 Cd2 O2 C8 68.2(2) . . . . ? O6 Cd2 O2 C8 -122.8(2) 2 . . . ? O8 Cd2 N2 C26 -117.8(3) 2 . . . ? O1 Cd2 N2 C26 89.0(3) . . . . ? N1 Cd2 N2 C26 176.7(3) . . . . ? O6 Cd2 N2 C26 -30.4(3) 2 . . . ? O2 Cd2 N2 C26 40.7(3) . . . . ? C8 Cd2 N2 C26 60.4(3) . . . . ? O8 Cd2 N2 C28 57.1(3) 2 . . . ? O1 Cd2 N2 C28 -96.1(2) . . . . ? N1 Cd2 N2 C28 -8.4(2) . . . . ? O6 Cd2 N2 C28 144.5(2) 2 . . . ? O2 Cd2 N2 C28 -144.3(2) . . . . ? C8 Cd2 N2 C28 -124.7(2) . . . . ? C6 C1 C2 C3 -0.2(5) . . . . ? S1 C1 C2 C3 178.5(2) . . . . ? O3 Cd1 N3 C29 -143.7(3) 3_565 . . . ? O4 Cd1 N3 C29 104.0(3) . . . . ? N4 Cd1 N3 C29 -178.0(3) . . . . ? O6 Cd1 N3 C29 -33.3(3) 2 . . . ? O5 Cd1 N3 C29 -85.6(3) 2 . . . ? O3 Cd1 N3 C40 40.7(4) 3_565 . . . ? O4 Cd1 N3 C40 -71.5(2) . . . . ? N4 Cd1 N3 C40 6.4(2) . . . . ? O6 Cd1 N3 C40 151.2(2) 2 . . . ? O5 Cd1 N3 C40 98.8(2) 2 . . . ? C1 C2 C3 C4 0.8(5) . . . . ? C1 C2 C3 C8 -179.7(3) . . . . ? O3 Cd1 O4 C7 118.5(3) 3_565 . . . ? N3 Cd1 O4 C7 -87.4(3) . . . . ? N4 Cd1 O4 C7 -157.9(3) . . . . ? O6 Cd1 O4 C7 2.7(4) 2 . . . ? O5 Cd1 O4 C7 -138.8(4) 2 . . . ? O3 Cd1 N4 C39 -171.4(2) 3_565 . . . ? O4 Cd1 N4 C39 87.0(2) . . . . ? N3 Cd1 N4 C39 -6.6(2) . . . . ? O6 Cd1 N4 C39 -72.2(3) 2 . . . ? O5 Cd1 N4 C39 -89.0(2) 2 . . . ? O3 Cd1 N4 C38 16.3(3) 3_565 . . . ? O4 Cd1 N4 C38 -85.3(3) . . . . ? N3 Cd1 N4 C38 -178.9(3) . . . . ? O6 Cd1 N4 C38 115.5(3) 2 . . . ? O5 Cd1 N4 C38 98.7(3) 2 . . . ? C2 C3 C4 C5 -0.5(5) . . . . ? C8 C3 C4 C5 -180.0(3) . . . . ? C2 C3 C4 C7 -179.3(3) . . . . ? C8 C3 C4 C7 1.3(5) . . . . ? C3 C4 C5 C6 -0.5(5) . . . . ? C7 C4 C5 C6 178.4(3) . . . . ? C4 C5 C6 C1 1.2(5) . . . . ? C2 C1 C6 C5 -0.8(5) . . . . ? S1 C1 C6 C5 -179.5(3) . . . . ? Cd1 O4 C7 O3 -110.1(3) . . . . ? Cd1 O4 C7 C4 75.6(4) . . . . ? Cd1 O3 C7 O4 11.2(5) 3_565 . . . ? Cd1 O3 C7 C4 -174.3(2) 3_565 . . . ? C5 C4 C7 O4 93.7(4) . . . . ? C3 C4 C7 O4 -87.5(4) . . . . ? C5 C4 C7 O3 -81.1(4) . . . . ? C3 C4 C7 O3 97.7(4) . . . . ? Cd2 O2 C8 O1 -5.5(3) . . . . ? Cd2 O2 C8 C3 172.9(3) . . . . ? Cd2 O1 C8 O2 5.9(4) . . . . ? Cd2 O1 C8 C3 -172.5(2) . . . . ? C2 C3 C8 O2 -170.8(3) . . . . ? C4 C3 C8 O2 8.7(5) . . . . ? C2 C3 C8 O1 7.6(5) . . . . ? C4 C3 C8 O1 -172.9(3) . . . . ? C2 C3 C8 Cd2 -49.4(18) . . . . ? C4 C3 C8 Cd2 130.1(16) . . . . ? O8 Cd2 C8 O2 132.13(19) 2 . . . ? N2 Cd2 C8 O2 -46.2(2) . . . . ? O1 Cd2 C8 O2 -174.5(3) . . . . ? N1 Cd2 C8 O2 -130.8(2) . . . . ? O6 Cd2 C8 O2 52.5(2) 2 . . . ? O8 Cd2 C8 O1 -53.4(2) 2 . . . ? N2 Cd2 C8 O1 128.3(2) . . . . ? N1 Cd2 C8 O1 43.7(2) . . . . ? O6 Cd2 C8 O1 -133.0(2) 2 . . . ? O2 Cd2 C8 O1 174.5(3) . . . . ? O8 Cd2 C8 C3 7.4(17) 2 . . . ? N2 Cd2 C8 C3 -171.0(17) . . . . ? O1 Cd2 C8 C3 60.8(17) . . . . ? N1 Cd2 C8 C3 104.5(17) . . . . ? O6 Cd2 C8 C3 -72.2(17) 2 . . . ? O2 Cd2 C8 C3 -124.7(18) . . . . ? O10 S1 C9 C12 -35.2(3) . . . . ? O9 S1 C9 C12 -167.1(3) . . . . ? C1 S1 C9 C12 78.5(3) . . . . ? O10 S1 C9 C10 146.7(3) . . . . ? O9 S1 C9 C10 14.7(3) . . . . ? C1 S1 C9 C10 -99.7(3) . . . . ? C12 C9 C10 C11 -2.6(5) . . . . ? S1 C9 C10 C11 175.5(2) . . . . ? C9 C10 C11 C14 1.3(5) . . . . ? C9 C10 C11 C16 177.4(3) . . . . ? C10 C9 C12 C13 1.2(5) . . . . ? S1 C9 C12 C13 -177.0(3) . . . . ? C9 C12 C13 C14 1.4(5) . . . . ? C12 C13 C14 C11 -2.6(5) . . . . ? C12 C13 C14 C15 177.1(3) . . . . ? C10 C11 C14 C13 1.2(5) . . . . ? C16 C11 C14 C13 -174.7(3) . . . . ? C10 C11 C14 C15 -178.5(3) . . . . ? C16 C11 C14 C15 5.6(5) . . . . ? Cd2 O8 C15 O7 84.5(4) 2_545 . . . ? Cd2 O8 C15 C14 -98.4(3) 2_545 . . . ? C13 C14 C15 O7 88.0(4) . . . . ? C11 C14 C15 O7 -92.3(4) . . . . ? C13 C14 C15 O8 -89.3(4) . . . . ? C11 C14 C15 O8 90.3(4) . . . . ? Cd1 O5 C16 O6 4.5(3) 2_545 . . . ? Cd1 O5 C16 C11 -173.8(3) 2_545 . . . ? Cd2 O6 C16 O5 -173.1(3) 2_545 . . . ? Cd1 O6 C16 O5 -4.7(4) 2_545 . . . ? Cd2 O6 C16 C11 5.3(6) 2_545 . . . ? Cd1 O6 C16 C11 173.6(3) 2_545 . . . ? C14 C11 C16 O5 136.5(3) . . . . ? C10 C11 C16 O5 -39.5(5) . . . . ? C14 C11 C16 O6 -41.9(5) . . . . ? C10 C11 C16 O6 142.1(3) . . . . ? C27 N1 C17 C18 -2.6(6) . . . . ? Cd2 N1 C17 C18 -172.6(3) . . . . ? N1 C17 C18 C19 2.1(7) . . . . ? C17 C18 C19 C20 0.6(7) . . . . ? C18 C19 C20 C27 -2.5(6) . . . . ? C18 C19 C20 C21 176.1(4) . . . . ? C27 C20 C21 C22 -3.5(7) . . . . ? C19 C20 C21 C22 178.0(4) . . . . ? C20 C21 C22 C23 1.4(8) . . . . ? C21 C22 C23 C28 2.2(7) . . . . ? C21 C22 C23 C24 -178.8(4) . . . . ? C28 C23 C24 C25 -0.4(6) . . . . ? C22 C23 C24 C25 -179.4(4) . . . . ? C23 C24 C25 C26 1.6(7) . . . . ? C28 N2 C26 C25 -1.1(6) . . . . ? Cd2 N2 C26 C25 173.6(3) . . . . ? C24 C25 C26 N2 -0.9(7) . . . . ? C17 N1 C27 C20 0.6(5) . . . . ? Cd2 N1 C27 C20 171.8(3) . . . . ? C17 N1 C27 C28 -178.1(3) . . . . ? Cd2 N1 C27 C28 -6.8(4) . . . . ? C19 C20 C27 N1 1.9(5) . . . . ? C21 C20 C27 N1 -176.7(3) . . . . ? C19 C20 C27 C28 -179.4(3) . . . . ? C21 C20 C27 C28 1.9(5) . . . . ? C26 N2 C28 C23 2.4(5) . . . . ? Cd2 N2 C28 C23 -172.8(3) . . . . ? C26 N2 C28 C27 -176.6(3) . . . . ? Cd2 N2 C28 C27 8.2(4) . . . . ? C24 C23 C28 N2 -1.6(5) . . . . ? C22 C23 C28 N2 177.4(4) . . . . ? C24 C23 C28 C27 177.3(3) . . . . ? C22 C23 C28 C27 -3.7(5) . . . . ? N1 C27 C28 N2 -0.8(5) . . . . ? C20 C27 C28 N2 -179.4(3) . . . . ? N1 C27 C28 C23 -179.8(3) . . . . ? C20 C27 C28 C23 1.6(5) . . . . ? C40 N3 C29 C30 1.2(6) . . . . ? Cd1 N3 C29 C30 -174.2(3) . . . . ? N3 C29 C30 C31 -0.2(6) . . . . ? C29 C30 C31 C32 -0.9(6) . . . . ? C30 C31 C32 C40 1.0(6) . . . . ? C30 C31 C32 C33 -178.2(4) . . . . ? C31 C32 C33 C34 -179.7(5) . . . . ? C40 C32 C33 C34 1.0(7) . . . . ? C32 C33 C34 C35 -1.2(8) . . . . ? C33 C34 C35 C36 -179.8(5) . . . . ? C33 C34 C35 C39 0.4(7) . . . . ? C39 C35 C36 C37 -0.1(7) . . . . ? C34 C35 C36 C37 -180.0(5) . . . . ? C35 C36 C37 C38 -0.4(8) . . . . ? C39 N4 C38 C37 0.7(6) . . . . ? Cd1 N4 C38 C37 172.8(3) . . . . ? C36 C37 C38 N4 0.1(7) . . . . ? C38 N4 C39 C35 -1.2(5) . . . . ? Cd1 N4 C39 C35 -174.0(3) . . . . ? C38 N4 C39 C40 179.0(3) . . . . ? Cd1 N4 C39 C40 6.2(4) . . . . ? C36 C35 C39 N4 1.0(6) . . . . ? C34 C35 C39 N4 -179.2(4) . . . . ? C36 C35 C39 C40 -179.3(4) . . . . ? C34 C35 C39 C40 0.6(5) . . . . ? C29 N3 C40 C32 -1.1(5) . . . . ? Cd1 N3 C40 C32 174.8(3) . . . . ? C29 N3 C40 C39 178.2(3) . . . . ? Cd1 N3 C40 C39 -5.9(4) . . . . ? C31 C32 C40 N3 0.0(5) . . . . ? C33 C32 C40 N3 179.3(3) . . . . ? C31 C32 C40 C39 -179.3(3) . . . . ? C33 C32 C40 C39 -0.1(5) . . . . ? N4 C39 C40 N3 -0.3(5) . . . . ? C35 C39 C40 N3 179.9(3) . . . . ? N4 C39 C40 C32 179.1(3) . . . . ? C35 C39 C40 C32 -0.7(5) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.662 _refine_diff_density_min -0.802 _refine_diff_density_rms 0.094 data_compound4 _database_code_depnum_ccdc_archive 'CCDC 894380' #TrackingRef '894380.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H54 Cd2 N8 O18 S' _chemical_formula_weight 1480.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.885(3) _cell_length_b 14.331(4) _cell_length_c 21.418(7) _cell_angle_alpha 85.964(5) _cell_angle_beta 89.432(6) _cell_angle_gamma 86.079(6) _cell_volume 3019.6(16) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 7282 _cell_measurement_theta_min 2.2700 _cell_measurement_theta_max 27.4835 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.628 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1500 _exptl_absorpt_coefficient_mu 0.822 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8242 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details '(CrystalClear; Rigaku, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type \w _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22597 _diffrn_reflns_av_R_equivalents 0.0199 _diffrn_reflns_av_sigmaI/netI 0.0299 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 27.50 _reflns_number_total 13092 _reflns_number_gt 10585 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _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^)+(0.0823P)^2^+2.8061P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment Constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13092 _refine_ls_number_parameters 838 _refine_ls_number_restraints 51 _refine_ls_R_factor_all 0.0599 _refine_ls_R_factor_gt 0.0474 _refine_ls_wR_factor_ref 0.1438 _refine_ls_wR_factor_gt 0.1284 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.046 _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 0.79716(2) 0.219386(16) -0.000363(11) 0.03815(9) Uani 1 1 d . . . Cd2 Cd 0.81958(3) 0.26382(2) 0.478478(12) 0.04928(10) Uani 1 1 d . . . S1 S 1.35902(9) 0.24229(6) 0.22872(5) 0.0448(2) Uani 1 1 d . . . O1 O 0.9301(3) 0.20582(18) 0.08463(13) 0.0514(6) Uani 1 1 d . . . O2 O 0.9510(3) 0.05537(18) 0.06651(13) 0.0504(6) Uani 1 1 d . . . O3 O 0.8374(3) -0.0120(2) 0.20155(17) 0.0646(8) Uani 1 1 d . . . O4 O 0.9882(3) -0.12821(18) 0.18328(14) 0.0558(7) Uani 1 1 d . . . O5 O 0.8850(5) 0.5744(3) 0.30678(19) 0.0999(15) Uani 1 1 d . . . O6 O 1.0711(6) 0.6274(2) 0.34348(19) 0.1035(16) Uani 1 1 d . . . O7 O 0.9762(4) 0.4401(2) 0.42112(14) 0.0631(8) Uani 1 1 d . . . O8 O 0.9557(3) 0.2928(2) 0.39599(13) 0.0545(7) Uani 1 1 d . . . O9 O 1.4170(3) 0.2761(2) 0.17036(15) 0.0618(8) Uani 1 1 d . . . O10 O 1.4484(3) 0.2052(2) 0.27867(16) 0.0623(8) Uani 1 1 d . . . O11 O 0.8863(3) 0.11187(18) -0.06779(13) 0.0542(7) Uani 1 1 d . . . H11A H 0.9346 0.0713 -0.0454 0.065 Uiso 1 1 d R . . H11B H 0.9124 0.1084 -0.1055 0.065 Uiso 1 1 d R . . O12 O 0.9555(4) 0.3455(3) 0.53629(16) 0.0895(12) Uani 1 1 d . . . H12A H 0.9806 0.4002 0.5264 0.107 Uiso 1 1 d R . . H12B H 0.9909 0.3270 0.5714 0.107 Uiso 1 1 d R . . O13 O 1.1889(4) 0.7503(3) 0.2528(2) 0.0950(14) Uani 1 1 d . . . H13A H 1.1287 0.7885 0.2351 0.114 Uiso 1 1 d R . . H13B H 1.1484 0.6995 0.2629 0.114 Uiso 1 1 d R . . O14 O 0.8187(5) 0.7729(3) 0.2772(3) 0.127(2) Uani 1 1 d . . . H14A H 0.8470 0.7169 0.2669 0.152 Uiso 1 1 d R . . H14B H 0.8579 0.8105 0.2507 0.152 Uiso 1 1 d R . . O15 O 0.8478(7) 0.3159(4) 0.1929(3) 0.138(2) Uani 1 1 d . . . H15A H 0.8777 0.2848 0.1617 0.166 Uiso 1 1 d R . . H15B H 0.8391 0.2726 0.2233 0.166 Uiso 1 1 d R . . O16 O 0.7090(6) 0.4935(5) 0.2274(3) 0.135(2) Uani 1 1 d . . . H16A H 0.7465 0.4363 0.2213 0.162 Uiso 1 1 d R . . H16B H 0.7673 0.5128 0.2547 0.162 Uiso 1 1 d R . . O17 O 0.7616(6) 0.1527(4) 0.2627(3) 0.1277(19) Uani 1 1 d . . . H17A H 0.6771 0.1700 0.2550 0.153 Uiso 1 1 d R . . H17B H 0.7842 0.1155 0.2330 0.153 Uiso 1 1 d R . . O18 O 0.6053(6) -0.0777(5) 0.2674(3) 0.151(2) Uani 1 1 d . . . H18A H 0.6453 -0.1331 0.2820 0.181 Uiso 1 1 d R . . H18B H 0.6728 -0.0487 0.2520 0.181 Uiso 1 1 d R . . N1 N 0.9073(3) 0.33688(19) -0.05995(13) 0.0393(6) Uani 1 1 d . . . N2 N 0.7118(3) 0.3694(2) 0.02974(14) 0.0427(6) Uani 1 1 d . . . N3 N 0.6145(3) 0.2339(2) -0.07303(15) 0.0482(7) Uani 1 1 d . . . N4 N 0.6145(3) 0.1429(2) 0.04332(16) 0.0450(7) Uani 1 1 d . . . N5 N 0.6351(3) 0.3544(3) 0.43190(17) 0.0538(8) Uani 1 1 d . . . N6 N 0.6438(4) 0.2836(3) 0.55416(17) 0.0626(9) Uani 1 1 d . . . N7 N 0.7178(4) 0.1261(3) 0.45094(17) 0.0596(9) Uani 1 1 d U . . N8 N 0.9043(4) 0.1287(4) 0.54279(17) 0.0729(12) Uani 1 1 d U . . C1 C 1.0650(3) 0.1057(2) 0.15393(15) 0.0354(6) Uani 1 1 d . . . C2 C 1.1571(4) 0.1713(2) 0.16540(16) 0.0388(7) Uani 1 1 d . . . H2 H 1.1574 0.2267 0.1401 0.047 Uiso 1 1 calc R . . C3 C 1.2484(4) 0.1549(2) 0.21411(16) 0.0407(7) Uani 1 1 d . . . C4 C 1.2530(4) 0.0722(3) 0.25154(18) 0.0492(9) Uani 1 1 d . . . H4 H 1.3163 0.0608 0.2835 0.059 Uiso 1 1 calc R . . C5 C 1.1610(4) 0.0066(3) 0.24032(17) 0.0490(9) Uani 1 1 d . . . H5 H 1.1637 -0.0497 0.2648 0.059 Uiso 1 1 calc R . . C6 C 1.0650(4) 0.0230(2) 0.19338(15) 0.0379(7) Uani 1 1 d . . . C7 C 0.9746(3) 0.1220(2) 0.09769(16) 0.0365(7) Uani 1 1 d . . . C8 C 0.9531(4) -0.0442(2) 0.19178(16) 0.0435(8) Uani 1 1 d . . . C9 C 1.0837(4) 0.3920(2) 0.32828(16) 0.0407(7) Uani 1 1 d . . . C10 C 1.1639(4) 0.3192(2) 0.30564(17) 0.0423(7) Uani 1 1 d . . . H10 H 1.1600 0.2589 0.3245 0.051 Uiso 1 1 calc R . . C11 C 1.2504(4) 0.3347(2) 0.25514(16) 0.0394(7) Uani 1 1 d . . . C12 C 1.2563(4) 0.4230(3) 0.22657(17) 0.0489(9) Uani 1 1 d . . . H12 H 1.3137 0.4334 0.1925 0.059 Uiso 1 1 calc R . . C13 C 1.1766(5) 0.4965(3) 0.24875(17) 0.0499(9) Uani 1 1 d . . . H13 H 1.1812 0.5564 0.2295 0.060 Uiso 1 1 calc R . . C14 C 1.0894(4) 0.4823(2) 0.29936(16) 0.0432(8) Uani 1 1 d . . . C15 C 1.0060(6) 0.5673(3) 0.31925(18) 0.0613(12) Uani 1 1 d . . . C16 C 0.9972(4) 0.3749(3) 0.38637(17) 0.0446(8) Uani 1 1 d . . . C17 C 0.6187(5) 0.3850(3) 0.0730(2) 0.0564(10) Uani 1 1 d . . . H17 H 0.5839 0.3338 0.0952 0.068 Uiso 1 1 calc R . . C18 C 0.5700(5) 0.4747(4) 0.0870(2) 0.0688(13) Uani 1 1 d . . . H18 H 0.5030 0.4828 0.1173 0.083 Uiso 1 1 calc R . . C19 C 0.6214(5) 0.5496(3) 0.0560(2) 0.0639(12) Uani 1 1 d . . . H19 H 0.5899 0.6099 0.0649 0.077 Uiso 1 1 calc R . . C20 C 0.7230(4) 0.5366(3) 0.0101(2) 0.0492(9) Uani 1 1 d . . . C21 C 0.7651(4) 0.4441(2) -0.00119(16) 0.0380(7) Uani 1 1 d . . . C22 C 0.8694(4) 0.4274(2) -0.04769(16) 0.0369(7) Uani 1 1 d . . . C23 C 0.9292(4) 0.5033(3) -0.07840(18) 0.0470(8) Uani 1 1 d . . . C24 C 0.8869(5) 0.5960(3) -0.0634(2) 0.0578(11) Uani 1 1 d . . . H24 H 0.9296 0.6463 -0.0827 0.069 Uiso 1 1 calc R . . C25 C 0.7872(5) 0.6124(3) -0.0222(2) 0.0604(11) Uani 1 1 d . . . H25 H 0.7593 0.6739 -0.0145 0.072 Uiso 1 1 calc R . . C26 C 1.0321(5) 0.4840(3) -0.1228(2) 0.0564(10) Uani 1 1 d . . . H26 H 1.0747 0.5329 -0.1438 0.068 Uiso 1 1 calc R . . C27 C 1.0682(5) 0.3948(3) -0.1345(2) 0.0565(10) Uani 1 1 d . . . H27 H 1.1357 0.3815 -0.1638 0.068 Uiso 1 1 calc R . . C28 C 1.0033(4) 0.3228(3) -0.10243(19) 0.0481(8) Uani 1 1 d . . . H28 H 1.0286 0.2614 -0.1113 0.058 Uiso 1 1 calc R . . C29 C 0.6142(5) 0.2777(4) -0.1299(2) 0.0675(12) Uani 1 1 d . . . H29 H 0.6911 0.3077 -0.1431 0.081 Uiso 1 1 calc R . . C30 C 0.5045(7) 0.2812(5) -0.1708(2) 0.0889(19) Uani 1 1 d . . . H30 H 0.5071 0.3145 -0.2096 0.107 Uiso 1 1 calc R . . C31 C 0.3941(6) 0.2350(5) -0.1525(3) 0.0870(19) Uani 1 1 d . . . H31 H 0.3210 0.2352 -0.1795 0.104 Uiso 1 1 calc R . . C32 C 0.3889(5) 0.1873(3) -0.0938(3) 0.0683(14) Uani 1 1 d . . . C33 C 0.2774(5) 0.1373(5) -0.0719(4) 0.089(2) Uani 1 1 d . . . H33 H 0.2026 0.1357 -0.0977 0.107 Uiso 1 1 calc R . . C34 C 0.2767(5) 0.0919(4) -0.0147(4) 0.086(2) Uani 1 1 d . . . H34 H 0.2016 0.0596 -0.0019 0.104 Uiso 1 1 calc R . . C35 C 0.3897(4) 0.0922(3) 0.0271(3) 0.0647(13) Uani 1 1 d . . . C36 C 0.3962(5) 0.0440(3) 0.0858(3) 0.0739(16) Uani 1 1 d . . . H36 H 0.3236 0.0104 0.1003 0.089 Uiso 1 1 calc R . . C37 C 0.5071(5) 0.0456(3) 0.1217(3) 0.0690(14) Uani 1 1 d . . . H37 H 0.5119 0.0135 0.1610 0.083 Uiso 1 1 calc R . . C38 C 0.6153(5) 0.0969(3) 0.0986(2) 0.0575(10) Uani 1 1 d . . . H38 H 0.6913 0.0983 0.1237 0.069 Uiso 1 1 calc R . . C39 C 0.5040(4) 0.1891(3) -0.0543(2) 0.0492(9) Uani 1 1 d . . . C40 C 0.5036(4) 0.1414(2) 0.0069(2) 0.0472(9) Uani 1 1 d . . . C41 C 0.6322(5) 0.3894(4) 0.3736(2) 0.0672(12) Uani 1 1 d . . . H41 H 0.7071 0.3774 0.3481 0.081 Uiso 1 1 calc R . . C42 C 0.5194(6) 0.4449(4) 0.3480(3) 0.0809(15) Uani 1 1 d . . . H42 H 0.5199 0.4699 0.3067 0.097 Uiso 1 1 calc R . . C43 C 0.4110(6) 0.4600(4) 0.3857(3) 0.0808(16) Uani 1 1 d . . . H43 H 0.3358 0.4964 0.3700 0.097 Uiso 1 1 calc R . . C44 C 0.4087(5) 0.4233(4) 0.4466(3) 0.0735(14) Uani 1 1 d . . . C45 C 0.5245(4) 0.3698(3) 0.4697(2) 0.0558(10) Uani 1 1 d . . . C46 C 0.2954(5) 0.4386(5) 0.4888(4) 0.094(2) Uani 1 1 d . . . H46 H 0.2180 0.4741 0.4747 0.112 Uiso 1 1 calc R . . C47 C 0.3014(6) 0.4013(5) 0.5492(4) 0.097(2) Uani 1 1 d . . . H47 H 0.2274 0.4120 0.5755 0.117 Uiso 1 1 calc R . . C48 C 0.4161(5) 0.3471(4) 0.5728(3) 0.0762(15) Uani 1 1 d . . . C49 C 0.4265(7) 0.3092(5) 0.6347(3) 0.096(2) Uani 1 1 d . . . H49 H 0.3540 0.3177 0.6621 0.116 Uiso 1 1 calc R . . C50 C 0.5419(8) 0.2600(6) 0.6548(3) 0.101(2) Uani 1 1 d . . . H50 H 0.5488 0.2342 0.6958 0.121 Uiso 1 1 calc R . . C51 C 0.6500(6) 0.2487(4) 0.6130(2) 0.0765(14) Uani 1 1 d . . . H51 H 0.7293 0.2156 0.6271 0.092 Uiso 1 1 calc R . . C52 C 0.5307(5) 0.3309(3) 0.5331(2) 0.0602(11) Uani 1 1 d . . . C53 C 0.6278(6) 0.1239(4) 0.4051(2) 0.0732(13) Uani 1 1 d . . . H53 H 0.6071 0.1787 0.3801 0.088 Uiso 1 1 calc R . . C54 C 0.5637(8) 0.0444(5) 0.3926(4) 0.101(2) Uani 1 1 d U . . H54 H 0.5017 0.0466 0.3600 0.121 Uiso 1 1 calc R . . C55 C 0.5910(8) -0.0342(5) 0.4269(4) 0.101(2) Uani 1 1 d U . . H55 H 0.5475 -0.0876 0.4188 0.122 Uiso 1 1 calc R . . C56 C 0.6839(7) -0.0382(4) 0.4751(3) 0.0879(18) Uani 1 1 d U . . C57 C 0.7232(9) -0.1204(5) 0.5134(4) 0.115(3) Uani 1 1 d U . . H57 H 0.6824 -0.1757 0.5076 0.138 Uiso 1 1 calc R . . C58 C 0.8155(9) -0.1201(4) 0.5568(4) 0.105(2) Uani 1 1 d U . . H58 H 0.8397 -0.1759 0.5801 0.125 Uiso 1 1 calc R . . C59 C 0.8811(6) -0.0373(5) 0.5700(3) 0.0883(18) Uani 1 1 d U . . C60 C 0.9803(8) -0.0330(6) 0.6147(3) 0.110(2) Uani 1 1 d U . . H60 H 1.0077 -0.0875 0.6387 0.132 Uiso 1 1 calc R . . C61 C 1.0382(7) 0.0458(6) 0.6248(3) 0.098(2) Uani 1 1 d U . . H61 H 1.1032 0.0462 0.6559 0.117 Uiso 1 1 calc R . . C62 C 0.9989(6) 0.1312(6) 0.5868(2) 0.094(2) Uani 1 1 d U . . H62 H 1.0389 0.1867 0.5929 0.113 Uiso 1 1 calc R . . C63 C 0.8453(5) 0.0469(4) 0.5340(2) 0.0696(13) Uani 1 1 d U . . C64 C 0.7477(5) 0.0461(3) 0.4867(2) 0.0646(12) Uani 1 1 d U . . 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 0.03723(15) 0.03627(13) 0.04180(14) -0.00321(10) 0.00357(10) -0.00870(10) Cd2 0.04756(18) 0.05968(18) 0.03942(15) 0.00201(12) 0.00714(11) -0.00186(13) S1 0.0375(5) 0.0454(5) 0.0529(5) -0.0096(4) 0.0049(4) -0.0077(4) O1 0.0581(17) 0.0390(13) 0.0556(15) 0.0050(11) -0.0145(13) 0.0004(12) O2 0.0574(17) 0.0453(14) 0.0491(14) -0.0054(11) -0.0091(12) -0.0048(12) O3 0.0488(18) 0.0638(18) 0.082(2) -0.0055(16) 0.0173(15) -0.0117(14) O4 0.0679(19) 0.0353(12) 0.0647(17) -0.0018(12) 0.0019(14) -0.0093(12) O5 0.110(3) 0.109(3) 0.073(2) -0.008(2) 0.005(2) 0.051(3) O6 0.189(5) 0.0530(19) 0.073(2) -0.0242(17) 0.050(3) -0.032(2) O7 0.083(2) 0.0578(17) 0.0471(15) -0.0036(13) 0.0195(14) 0.0031(16) O8 0.0572(17) 0.0521(15) 0.0529(15) 0.0046(12) 0.0185(13) -0.0055(13) O9 0.0589(18) 0.0603(17) 0.0687(19) -0.0128(15) 0.0290(15) -0.0166(14) O10 0.0483(17) 0.0588(17) 0.081(2) -0.0110(15) -0.0183(15) -0.0013(13) O11 0.0725(19) 0.0376(13) 0.0501(15) -0.0021(11) 0.0062(13) 0.0112(13) O12 0.106(3) 0.112(3) 0.0551(19) 0.0068(19) -0.0048(19) -0.054(3) O13 0.078(3) 0.089(3) 0.112(3) 0.032(3) 0.005(2) 0.000(2) O14 0.087(3) 0.101(3) 0.178(5) 0.070(4) 0.029(3) 0.005(3) O15 0.193(6) 0.082(3) 0.140(5) -0.013(3) 0.045(4) -0.018(4) O16 0.139(5) 0.162(5) 0.106(4) -0.016(4) 0.026(3) -0.022(4) O17 0.125(4) 0.132(4) 0.127(4) -0.029(3) 0.034(3) 0.000(4) O18 0.144(5) 0.137(5) 0.174(6) -0.014(4) 0.041(5) -0.033(4) N1 0.0414(16) 0.0342(13) 0.0433(15) -0.0066(11) 0.0031(12) -0.0060(12) N2 0.0463(17) 0.0388(14) 0.0432(15) -0.0042(12) 0.0062(13) -0.0033(12) N3 0.0453(18) 0.0489(17) 0.0506(17) -0.0119(14) -0.0017(14) 0.0033(14) N4 0.0374(16) 0.0347(14) 0.0626(19) -0.0020(13) 0.0067(14) -0.0027(12) N5 0.0470(19) 0.0570(19) 0.0571(19) -0.0024(16) 0.0027(15) -0.0032(15) N6 0.057(2) 0.080(3) 0.053(2) -0.0140(18) 0.0173(17) -0.0129(19) N7 0.069(2) 0.0548(19) 0.0537(19) -0.0002(16) 0.0144(17) -0.0008(17) N8 0.061(2) 0.108(3) 0.0432(19) 0.012(2) 0.0107(16) 0.021(2) C1 0.0394(18) 0.0298(14) 0.0363(15) -0.0007(12) 0.0044(13) -0.0002(12) C2 0.0419(19) 0.0316(15) 0.0422(17) 0.0003(13) 0.0043(14) -0.0024(13) C3 0.0390(18) 0.0413(17) 0.0426(17) -0.0056(14) 0.0023(14) -0.0065(14) C4 0.057(2) 0.0468(19) 0.0444(19) 0.0009(15) -0.0101(16) -0.0067(17) C5 0.064(2) 0.0402(17) 0.0418(18) 0.0059(14) -0.0046(17) -0.0064(17) C6 0.0467(19) 0.0315(14) 0.0352(15) -0.0007(12) 0.0048(13) -0.0025(13) C7 0.0333(17) 0.0354(15) 0.0403(16) 0.0027(13) 0.0036(13) -0.0057(13) C8 0.055(2) 0.0377(16) 0.0380(17) 0.0038(13) 0.0043(15) -0.0081(15) C9 0.046(2) 0.0413(17) 0.0349(16) 0.0000(13) 0.0034(14) -0.0060(15) C10 0.045(2) 0.0373(16) 0.0437(18) 0.0018(14) 0.0047(14) -0.0044(14) C11 0.0398(18) 0.0379(16) 0.0416(17) -0.0052(13) 0.0033(14) -0.0078(14) C12 0.062(2) 0.0463(19) 0.0388(17) -0.0032(15) 0.0121(16) -0.0116(17) C13 0.073(3) 0.0366(17) 0.0398(18) 0.0023(14) 0.0090(17) -0.0102(17) C14 0.057(2) 0.0390(17) 0.0334(16) -0.0019(13) 0.0018(14) -0.0032(15) C15 0.101(4) 0.044(2) 0.0363(19) 0.0024(16) 0.018(2) 0.007(2) C16 0.046(2) 0.0470(19) 0.0387(17) 0.0035(15) 0.0043(14) 0.0027(16) C17 0.059(3) 0.056(2) 0.054(2) -0.0080(18) 0.0152(19) -0.0028(19) C18 0.062(3) 0.075(3) 0.070(3) -0.026(2) 0.021(2) 0.004(2) C19 0.059(3) 0.050(2) 0.084(3) -0.027(2) 0.002(2) 0.008(2) C20 0.048(2) 0.0372(17) 0.062(2) -0.0119(16) -0.0099(17) 0.0048(15) C21 0.0385(18) 0.0331(15) 0.0429(17) -0.0060(13) -0.0049(13) -0.0023(13) C22 0.0404(18) 0.0292(14) 0.0411(16) -0.0004(12) -0.0050(13) -0.0031(13) C23 0.052(2) 0.0376(17) 0.051(2) 0.0062(15) -0.0088(16) -0.0085(16) C24 0.063(3) 0.0334(17) 0.076(3) 0.0096(18) -0.010(2) -0.0085(17) C25 0.069(3) 0.0303(17) 0.081(3) -0.0064(18) -0.016(2) 0.0047(18) C26 0.059(3) 0.055(2) 0.056(2) 0.0123(18) 0.0024(19) -0.0194(19) C27 0.054(2) 0.062(2) 0.053(2) 0.0019(19) 0.0146(18) -0.0122(19) C28 0.048(2) 0.0434(18) 0.054(2) -0.0084(16) 0.0130(16) -0.0070(16) C29 0.074(3) 0.078(3) 0.049(2) -0.010(2) 0.000(2) 0.012(3) C30 0.100(5) 0.113(5) 0.051(3) -0.022(3) -0.021(3) 0.031(4) C31 0.076(4) 0.104(4) 0.083(4) -0.049(3) -0.034(3) 0.029(3) C32 0.051(3) 0.061(3) 0.096(4) -0.045(3) -0.020(2) 0.014(2) C33 0.042(3) 0.088(4) 0.145(6) -0.064(4) -0.018(3) 0.002(3) C34 0.034(2) 0.065(3) 0.169(7) -0.054(4) 0.005(3) -0.015(2) C35 0.044(2) 0.0383(19) 0.115(4) -0.027(2) 0.021(2) -0.0084(16) C36 0.058(3) 0.038(2) 0.127(5) -0.016(3) 0.043(3) -0.0111(19) C37 0.070(3) 0.044(2) 0.090(3) 0.005(2) 0.041(3) -0.001(2) C38 0.054(2) 0.052(2) 0.065(3) 0.0017(19) 0.019(2) 0.0000(18) C39 0.041(2) 0.0399(17) 0.069(2) -0.0273(17) -0.0065(17) 0.0055(15) C40 0.0320(18) 0.0321(15) 0.080(3) -0.0228(17) 0.0088(17) -0.0025(13) C41 0.064(3) 0.071(3) 0.066(3) 0.002(2) -0.008(2) -0.005(2) C42 0.072(4) 0.086(4) 0.084(4) 0.007(3) -0.024(3) -0.008(3) C43 0.063(3) 0.070(3) 0.111(5) -0.006(3) -0.032(3) -0.006(3) C44 0.046(3) 0.073(3) 0.105(4) -0.031(3) -0.011(2) -0.004(2) C45 0.039(2) 0.052(2) 0.080(3) -0.022(2) 0.0019(19) -0.0075(17) C46 0.034(3) 0.109(5) 0.143(6) -0.051(5) 0.000(3) 0.004(3) C47 0.053(3) 0.123(5) 0.123(6) -0.051(5) 0.029(3) -0.020(3) C48 0.057(3) 0.090(4) 0.088(4) -0.039(3) 0.025(3) -0.027(3) C49 0.083(4) 0.132(6) 0.082(4) -0.040(4) 0.043(3) -0.045(4) C50 0.100(5) 0.145(6) 0.063(3) -0.022(4) 0.038(3) -0.032(5) C51 0.085(4) 0.096(4) 0.050(2) -0.007(2) 0.021(2) -0.016(3) C52 0.054(3) 0.067(3) 0.064(3) -0.019(2) 0.006(2) -0.025(2) C53 0.083(4) 0.070(3) 0.068(3) -0.010(2) -0.008(3) -0.009(3) C54 0.104(5) 0.083(4) 0.120(5) -0.017(4) -0.012(4) -0.023(4) C55 0.098(5) 0.088(4) 0.121(6) -0.016(4) 0.001(4) -0.020(4) C56 0.099(4) 0.051(3) 0.110(4) 0.010(3) 0.047(3) 0.003(3) C57 0.123(6) 0.069(4) 0.145(7) 0.034(4) 0.049(5) 0.014(4) C58 0.129(6) 0.059(3) 0.115(5) 0.035(3) 0.059(4) 0.027(3) C59 0.083(3) 0.100(4) 0.070(3) 0.030(3) 0.032(3) 0.038(3) C60 0.099(5) 0.138(5) 0.079(4) 0.029(4) 0.031(3) 0.045(4) C61 0.078(4) 0.159(6) 0.048(3) 0.008(3) 0.002(2) 0.036(4) C62 0.068(3) 0.154(6) 0.053(3) 0.005(3) 0.003(2) 0.026(4) C63 0.072(3) 0.066(3) 0.064(3) 0.017(2) 0.033(2) 0.020(2) C64 0.071(3) 0.060(2) 0.058(2) 0.011(2) 0.025(2) 0.009(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O1 2.245(3) . ? Cd1 O11 2.310(3) . ? Cd1 N4 2.331(3) . ? Cd1 N1 2.360(3) . ? Cd1 N2 2.384(3) . ? Cd1 N3 2.385(3) . ? Cd2 O8 2.243(3) . ? Cd2 O12 2.272(4) . ? Cd2 N5 2.353(4) . ? Cd2 N6 2.381(4) . ? Cd2 N7 2.389(4) . ? Cd2 N8 2.403(4) . ? S1 O9 1.436(3) . ? S1 O10 1.443(3) . ? S1 C3 1.765(4) . ? S1 C11 1.768(4) . ? O1 C7 1.263(4) . ? O2 C7 1.239(4) . ? O3 C8 1.226(5) . ? O4 C8 1.255(4) . ? O5 C15 1.224(7) . ? O6 C15 1.253(7) . ? O7 C16 1.240(5) . ? O8 C16 1.275(5) . ? N1 C28 1.323(5) . ? N1 C22 1.368(4) . ? N2 C17 1.320(5) . ? N2 C21 1.354(4) . ? N3 C29 1.330(6) . ? N3 C39 1.348(5) . ? N4 C38 1.314(5) . ? N4 C40 1.354(5) . ? N5 C41 1.313(6) . ? N5 C45 1.369(5) . ? N6 C51 1.323(6) . ? N6 C52 1.333(6) . ? N7 C53 1.335(6) . ? N7 C64 1.349(6) . ? N8 C62 1.338(7) . ? N8 C63 1.370(7) . ? C1 C2 1.387(5) . ? C1 C6 1.407(4) . ? C1 C7 1.503(5) . ? C2 C3 1.383(5) . ? C3 C4 1.381(5) . ? C4 C5 1.386(5) . ? C5 C6 1.386(5) . ? C6 C8 1.517(5) . ? C9 C10 1.379(5) . ? C9 C14 1.399(5) . ? C9 C16 1.518(5) . ? C10 C11 1.387(5) . ? C11 C12 1.371(5) . ? C12 C13 1.380(6) . ? C13 C14 1.391(5) . ? C14 C15 1.509(6) . ? C17 C18 1.392(6) . ? C18 C19 1.348(7) . ? C19 C20 1.411(7) . ? C20 C21 1.398(5) . ? C20 C25 1.430(6) . ? C21 C22 1.446(5) . ? C22 C23 1.394(5) . ? C23 C26 1.412(6) . ? C23 C24 1.423(6) . ? C24 C25 1.336(7) . ? C26 C27 1.343(6) . ? C27 C28 1.391(5) . ? C29 C30 1.397(7) . ? C30 C31 1.355(9) . ? C31 C32 1.391(9) . ? C32 C33 1.413(9) . ? C32 C39 1.427(6) . ? C33 C34 1.346(9) . ? C34 C35 1.438(8) . ? C35 C36 1.391(8) . ? C35 C40 1.418(6) . ? C36 C37 1.348(8) . ? C37 C38 1.405(6) . ? C39 C40 1.434(6) . ? C41 C42 1.415(7) . ? C42 C43 1.351(9) . ? C43 C44 1.372(9) . ? C44 C45 1.407(7) . ? C44 C46 1.447(8) . ? C45 C52 1.430(7) . ? C46 C47 1.364(10) . ? C47 C48 1.408(9) . ? C48 C49 1.397(9) . ? C48 C52 1.426(7) . ? C49 C50 1.357(10) . ? C50 C51 1.395(7) . ? C53 C54 1.384(8) . ? C54 C55 1.315(10) . ? C55 C56 1.385(10) . ? C56 C57 1.422(9) . ? C56 C64 1.438(8) . ? C57 C58 1.308(12) . ? C58 C59 1.437(11) . ? C59 C60 1.384(11) . ? C59 C63 1.412(7) . ? C60 C61 1.332(11) . ? C61 C62 1.453(10) . ? C63 C64 1.407(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 O1 Cd1 O11 106.84(10) . . ? O1 Cd1 N4 97.75(11) . . ? O11 Cd1 N4 101.63(11) . . ? O1 Cd1 N1 99.20(10) . . ? O11 Cd1 N1 88.59(10) . . ? N4 Cd1 N1 156.73(10) . . ? O1 Cd1 N2 88.81(10) . . ? O11 Cd1 N2 156.17(10) . . ? N4 Cd1 N2 93.69(11) . . ? N1 Cd1 N2 70.90(10) . . ? O1 Cd1 N3 166.65(11) . . ? O11 Cd1 N3 82.71(11) . . ? N4 Cd1 N3 70.74(12) . . ? N1 Cd1 N3 90.20(11) . . ? N2 Cd1 N3 85.30(11) . . ? O8 Cd2 O12 88.47(13) . . ? O8 Cd2 N5 92.78(12) . . ? O12 Cd2 N5 114.28(15) . . ? O8 Cd2 N6 160.82(13) . . ? O12 Cd2 N6 89.49(14) . . ? N5 Cd2 N6 70.76(14) . . ? O8 Cd2 N7 101.89(12) . . ? O12 Cd2 N7 154.45(14) . . ? N5 Cd2 N7 88.75(13) . . ? N6 Cd2 N7 87.92(13) . . ? O8 Cd2 N8 111.56(12) . . ? O12 Cd2 N8 85.52(17) . . ? N5 Cd2 N8 149.48(14) . . ? N6 Cd2 N8 87.28(14) . . ? N7 Cd2 N8 68.98(16) . . ? O9 S1 O10 118.9(2) . . ? O9 S1 C3 108.78(18) . . ? O10 S1 C3 107.55(18) . . ? O9 S1 C11 107.07(18) . . ? O10 S1 C11 109.60(18) . . ? C3 S1 C11 103.94(17) . . ? C7 O1 Cd1 112.0(2) . . ? C16 O8 Cd2 118.4(2) . . ? C28 N1 C22 117.9(3) . . ? C28 N1 Cd1 126.0(2) . . ? C22 N1 Cd1 116.0(2) . . ? C17 N2 C21 118.3(3) . . ? C17 N2 Cd1 125.9(3) . . ? C21 N2 Cd1 115.7(2) . . ? C29 N3 C39 118.3(4) . . ? C29 N3 Cd1 126.5(3) . . ? C39 N3 Cd1 115.1(3) . . ? C38 N4 C40 118.5(4) . . ? C38 N4 Cd1 124.6(3) . . ? C40 N4 Cd1 116.7(3) . . ? C41 N5 C45 119.5(4) . . ? C41 N5 Cd2 124.7(3) . . ? C45 N5 Cd2 115.8(3) . . ? C51 N6 C52 119.7(4) . . ? C51 N6 Cd2 124.9(4) . . ? C52 N6 Cd2 115.3(3) . . ? C53 N7 C64 117.9(5) . . ? C53 N7 Cd2 124.6(3) . . ? C64 N7 Cd2 117.4(3) . . ? C62 N8 C63 120.4(5) . . ? C62 N8 Cd2 123.7(5) . . ? C63 N8 Cd2 115.9(3) . . ? C2 C1 C6 118.7(3) . . ? C2 C1 C7 119.4(3) . . ? C6 C1 C7 121.8(3) . . ? C3 C2 C1 120.6(3) . . ? C4 C3 C2 121.2(3) . . ? C4 C3 S1 119.9(3) . . ? C2 C3 S1 118.9(3) . . ? C3 C4 C5 118.4(3) . . ? C6 C5 C4 121.5(3) . . ? C5 C6 C1 119.5(3) . . ? C5 C6 C8 117.8(3) . . ? C1 C6 C8 122.3(3) . . ? O2 C7 O1 124.3(3) . . ? O2 C7 C1 119.7(3) . . ? O1 C7 C1 116.0(3) . . ? O3 C8 O4 126.1(4) . . ? O3 C8 C6 116.7(3) . . ? O4 C8 C6 117.1(3) . . ? C10 C9 C14 119.2(3) . . ? C10 C9 C16 120.0(3) . . ? C14 C9 C16 120.6(3) . . ? C9 C10 C11 120.8(3) . . ? C12 C11 C10 120.2(3) . . ? C12 C11 S1 119.1(3) . . ? C10 C11 S1 120.6(3) . . ? C11 C12 C13 119.5(3) . . ? C12 C13 C14 121.1(3) . . ? C13 C14 C9 119.1(3) . . ? C13 C14 C15 116.6(3) . . ? C9 C14 C15 124.3(3) . . ? O5 C15 O6 126.3(5) . . ? O5 C15 C14 118.0(5) . . ? O6 C15 C14 115.5(5) . . ? O7 C16 O8 125.6(4) . . ? O7 C16 C9 118.0(3) . . ? O8 C16 C9 116.3(3) . . ? N2 C17 C18 123.0(4) . . ? C19 C18 C17 119.1(4) . . ? C18 C19 C20 120.0(4) . . ? C21 C20 C19 117.0(4) . . ? C21 C20 C25 119.9(4) . . ? C19 C20 C25 123.1(4) . . ? N2 C21 C20 122.5(3) . . ? N2 C21 C22 118.6(3) . . ? C20 C21 C22 118.9(3) . . ? N1 C22 C23 121.8(3) . . ? N1 C22 C21 118.7(3) . . ? C23 C22 C21 119.5(3) . . ? C22 C23 C26 117.8(4) . . ? C22 C23 C24 119.5(4) . . ? C26 C23 C24 122.7(4) . . ? C25 C24 C23 121.5(4) . . ? C24 C25 C20 120.6(4) . . ? C27 C26 C23 119.9(4) . . ? C26 C27 C28 119.1(4) . . ? N1 C28 C27 123.5(4) . . ? N3 C29 C30 123.4(6) . . ? C31 C30 C29 118.4(6) . . ? C30 C31 C32 120.7(5) . . ? C31 C32 C33 123.7(5) . . ? C31 C32 C39 117.3(5) . . ? C33 C32 C39 119.1(6) . . ? C34 C33 C32 121.7(5) . . ? C33 C34 C35 121.4(5) . . ? C36 C35 C40 117.5(5) . . ? C36 C35 C34 123.8(5) . . ? C40 C35 C34 118.6(5) . . ? C37 C36 C35 120.4(4) . . ? C36 C37 C38 118.6(5) . . ? N4 C38 C37 123.3(5) . . ? N3 C39 C32 121.8(4) . . ? N3 C39 C40 118.6(3) . . ? C32 C39 C40 119.5(4) . . ? N4 C40 C35 121.7(4) . . ? N4 C40 C39 118.7(3) . . ? C35 C40 C39 119.6(4) . . ? N5 C41 C42 122.6(5) . . ? C43 C42 C41 117.5(5) . . ? C42 C43 C44 121.9(5) . . ? C43 C44 C45 118.0(5) . . ? C43 C44 C46 123.7(6) . . ? C45 C44 C46 118.3(6) . . ? N5 C45 C44 120.5(5) . . ? N5 C45 C52 118.2(4) . . ? C44 C45 C52 121.2(5) . . ? C47 C46 C44 120.4(6) . . ? C46 C47 C48 122.0(5) . . ? C49 C48 C47 123.5(6) . . ? C49 C48 C52 117.0(6) . . ? C47 C48 C52 119.5(6) . . ? C50 C49 C48 120.3(5) . . ? C49 C50 C51 118.9(6) . . ? N6 C51 C50 122.4(6) . . ? N6 C52 C48 121.6(5) . . ? N6 C52 C45 119.8(4) . . ? C48 C52 C45 118.6(5) . . ? N7 C53 C54 123.6(6) . . ? C55 C54 C53 119.6(7) . . ? C54 C55 C56 120.5(7) . . ? C55 C56 C57 124.6(7) . . ? C55 C56 C64 118.0(5) . . ? C57 C56 C64 117.4(8) . . ? C58 C57 C56 121.5(8) . . ? C57 C58 C59 122.9(6) . . ? C60 C59 C63 116.3(7) . . ? C60 C59 C58 125.4(6) . . ? C63 C59 C58 118.3(6) . . ? C61 C60 C59 122.8(7) . . ? C60 C61 C62 119.4(6) . . ? N8 C62 C61 118.9(7) . . ? N8 C63 C64 119.0(4) . . ? N8 C63 C59 122.2(6) . . ? C64 C63 C59 118.8(6) . . ? N7 C64 C63 118.4(5) . . ? N7 C64 C56 120.4(5) . . ? C63 C64 C56 121.2(5) . . ? 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 O13 H13A O4 0.85 2.05 2.899(5) 173.2 1_565 O13 H13B O6 0.87 2.11 2.826(5) 139.1 . O14 H14A O5 0.87 2.17 2.903(6) 141.4 . O14 H14B O4 0.86 2.11 2.952(5) 165.2 1_565 O15 H15A O1 0.87 2.11 2.972(7) 174.2 . O15 H15B O17 0.87 2.05 2.861(8) 153.2 . O16 H16A O15 0.89 2.06 2.945(8) 169.7 . O16 H16B O5 0.89 1.92 2.805(8) 170.6 . O17 H17B O3 0.88 2.03 2.832(6) 152.5 . O18 H18A O14 0.90 2.11 2.899(8) 145.5 1_545 O18 H18B O3 0.86 2.02 2.861(7) 164.1 . O11 H11A O2 0.85 2.15 2.792(4) 132.5 2_755 O11 H11B O4 0.85 1.94 2.758(4) 161.8 2_755 O12 H12B O6 0.85 2.05 2.639(5) 125.4 2_766 _diffrn_measured_fraction_theta_max 0.943 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.943 _refine_diff_density_max 1.341 _refine_diff_density_min -1.294 _refine_diff_density_rms 0.095