# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2070 data_Compound1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H17 Cd N2 O4.50 S2' _chemical_formula_weight 581.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cd' 'Cd' -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.0989(7) _cell_length_b 20.3404(10) _cell_length_c 15.1155(7) _cell_angle_alpha 90.00 _cell_angle_beta 97.9820(10) _cell_angle_gamma 90.00 _cell_volume 4597.3(4) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.682 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2328 _exptl_absorpt_coefficient_mu 1.169 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 ? _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 24375 _diffrn_reflns_av_R_equivalents 0.0875 _diffrn_reflns_av_sigmaI/netI 0.1045 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.36 _diffrn_reflns_theta_max 25.05 _reflns_number_total 8106 _reflns_number_gt 4721 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0814P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8106 _refine_ls_number_parameters 612 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1245 _refine_ls_R_factor_gt 0.0611 _refine_ls_wR_factor_ref 0.1615 _refine_ls_wR_factor_gt 0.1415 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.001 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 0.36137(4) 0.13077(3) 0.72780(4) 0.03729(19) Uani 1 1 d . . . Cd2 Cd 0.12486(4) 0.08089(3) 0.73758(4) 0.0386(2) Uani 1 1 d . . . O9 O 0.2605(3) 0.1062(3) 0.8251(4) 0.0384(14) Uani 1 1 d . . . O5 O 0.3740(3) 0.2331(3) 0.7898(4) 0.0436(14) Uani 1 1 d . . . O4 O 0.3532(3) 0.0258(3) 0.6864(4) 0.0442(14) Uani 1 1 d . . . O2 O 0.1229(3) 0.1856(3) 0.6945(4) 0.0433(14) Uani 1 1 d . . . O1 O 0.2487(4) 0.1842(3) 0.6310(4) 0.0448(15) Uani 1 1 d . . . O7 O 0.1301(4) -0.0127(3) 0.8161(4) 0.0575(17) Uani 1 1 d . . . O3 O 0.2058(4) 0.0148(3) 0.6493(4) 0.0448(14) Uani 1 1 d . . . C31 C 0.3754(5) 0.3692(4) 0.8022(6) 0.041(2) Uani 1 1 d . . . H31 H 0.3891 0.3517 0.7475 0.049 Uiso 1 1 calc R . . C15 C 0.3751(5) -0.1096(4) 0.7055(6) 0.041(2) Uani 1 1 d . . . H15 H 0.4220 -0.0821 0.7329 0.049 Uiso 1 1 calc R . . C16 C 0.3881(5) -0.1761(4) 0.7052(5) 0.042(2) Uani 1 1 d . . . H16 H 0.4434 -0.1939 0.7324 0.050 Uiso 1 1 calc R . . C28 C 0.3339(5) 0.4218(4) 0.9593(5) 0.045(2) Uani 1 1 d . . . H28 H 0.3182 0.4401 1.0128 0.054 Uiso 1 1 calc R . . C30 C 0.3948(5) 0.4339(4) 0.8228(6) 0.045(2) Uani 1 1 d . . . H30 H 0.4205 0.4609 0.7818 0.053 Uiso 1 1 calc R . . C26 C 0.3359(5) 0.3288(4) 0.8602(5) 0.0328(19) Uani 1 1 d . . . C14 C 0.2950(5) -0.0809(4) 0.6668(5) 0.0342(19) Uani 1 1 d . . . C29 C 0.3770(5) 0.4600(4) 0.9035(6) 0.046(2) Uani 1 1 d . . . C27 C 0.3134(5) 0.3572(4) 0.9378(6) 0.044(2) Uani 1 1 d . . . H27 H 0.2833 0.3315 0.9769 0.053 Uiso 1 1 calc R . . C13 C 0.2830(6) -0.0078(4) 0.6668(5) 0.039(2) Uani 1 1 d . . . C17 C 0.3217(5) -0.2179(4) 0.6658(5) 0.039(2) Uani 1 1 d . . . C18 C 0.2410(5) -0.1898(4) 0.6299(6) 0.051(2) Uani 1 1 d . . . H18 H 0.1935 -0.2176 0.6049 0.061 Uiso 1 1 calc R . . O6 O 0.2707(4) 0.2259(3) 0.8819(4) 0.0538(16) Uani 1 1 d . . . O8 O 0.2703(4) -0.0151(3) 0.8875(4) 0.0495(15) Uani 1 1 d . . . C1 C 0.1835(5) 0.2138(4) 0.6571(5) 0.038(2) Uani 1 1 d . . . C38 C 0.1925(5) -0.1153(4) 0.8594(5) 0.036(2) Uani 1 1 d . . . C25 C 0.3252(5) 0.2575(4) 0.8427(5) 0.042(2) Uani 1 1 d . . . C37 C 0.1991(6) -0.0420(4) 0.8531(5) 0.039(2) Uani 1 1 d . . . C19 C 0.2279(5) -0.1230(4) 0.6296(6) 0.046(2) Uani 1 1 d . . . H19 H 0.1720 -0.1055 0.6035 0.056 Uiso 1 1 calc R . . C39 C 0.2620(5) -0.1542(4) 0.8984(6) 0.047(2) Uani 1 1 d . . . H39 H 0.3179 -0.1349 0.9211 0.056 Uiso 1 1 calc R . . C32 C 0.4051(6) 0.5302(5) 0.9278(7) 0.068(3) Uani 1 1 d . . . H32 H 0.3798 0.5495 0.9758 0.081 Uiso 1 1 calc R . . C43 C 0.1124(6) -0.1464(4) 0.8252(7) 0.059(3) Uani 1 1 d . . . H43 H 0.0637 -0.1208 0.7974 0.070 Uiso 1 1 calc R . . S4 S 0.15724(16) -0.47669(12) 0.93369(19) 0.0611(7) Uani 1 1 d . . . N4 N -0.0011(4) -0.4581(3) 0.8559(4) 0.0367(16) Uani 1 1 d . . . C46 C 0.0747(5) -0.4266(4) 0.8800(6) 0.044(2) Uani 1 1 d . . . C47 C 0.0855(6) -0.5415(4) 0.9225(6) 0.054(3) Uani 1 1 d . . . H47 H 0.0999 -0.5848 0.9432 0.065 Uiso 1 1 calc R . . C48 C 0.0062(5) -0.5226(4) 0.8805(6) 0.041(2) Uani 1 1 d . . . H48 H -0.0425 -0.5523 0.8684 0.050 Uiso 1 1 calc R . . C45 C 0.0863(5) -0.3577(4) 0.8656(5) 0.038(2) Uani 1 1 d . . . H45 H 0.0352 -0.3337 0.8397 0.046 Uiso 1 1 calc R . . C41 C 0.1717(5) -0.2525(4) 0.8724(6) 0.042(2) Uani 1 1 d . . . C42 C 0.1029(6) -0.2135(5) 0.8313(6) 0.060(3) Uani 1 1 d . . . H42 H 0.0481 -0.2335 0.8067 0.072 Uiso 1 1 calc R . . C40 C 0.2505(5) -0.2206(4) 0.9044(7) 0.059(3) Uani 1 1 d . . . H40 H 0.2992 -0.2462 0.9321 0.071 Uiso 1 1 calc R . . C44 C 0.1623(6) -0.3241(4) 0.8853(7) 0.057(3) Uani 1 1 d . . . H44 H 0.2142 -0.3480 0.9093 0.068 Uiso 1 1 calc R . . S3 S 0.44698(15) 0.67425(14) 0.99677(16) 0.0597(7) Uani 1 1 d . . . N3 N 0.5435(4) 0.6667(4) 0.8713(5) 0.0466(19) Uani 1 1 d . . . C34 C 0.4890(6) 0.6327(5) 0.9122(6) 0.054(3) Uani 1 1 d . . . C36 C 0.5534(6) 0.7288(5) 0.9053(6) 0.057(3) Uani 1 1 d . . . H36 H 0.5914 0.7603 0.8833 0.069 Uiso 1 1 calc R . . C35 C 0.5060(6) 0.7423(5) 0.9716(6) 0.063(3) Uani 1 1 d . . . H35 H 0.5051 0.7836 1.0006 0.076 Uiso 1 1 calc R . . C33 C 0.4619(6) 0.5681(5) 0.8888(7) 0.065(3) Uani 1 1 d . . . H33 H 0.4863 0.5490 0.8402 0.078 Uiso 1 1 calc R . . S2 S 0.35460(16) -0.43981(12) 0.59943(19) 0.0624(7) Uani 1 1 d . . . N2 N 0.5152(4) -0.4125(3) 0.6667(4) 0.0374(16) Uani 1 1 d . . . C20 C 0.3356(5) -0.2886(4) 0.6554(5) 0.041(2) Uani 1 1 d . . . H20 H 0.2846 -0.3152 0.6370 0.049 Uiso 1 1 calc R . . C24 C 0.4369(6) -0.4978(5) 0.5985(6) 0.053(2) Uani 1 1 d . . . H24 H 0.4273 -0.5409 0.5749 0.064 Uiso 1 1 calc R . . C22 C 0.4334(5) -0.3867(4) 0.6517(5) 0.039(2) Uani 1 1 d . . . C23 C 0.5145(6) -0.4751(4) 0.6344(5) 0.043(2) Uani 1 1 d . . . H23 H 0.5675 -0.5007 0.6378 0.052 Uiso 1 1 calc R . . C21 C 0.4155(5) -0.3181(4) 0.6703(5) 0.038(2) Uani 1 1 d . . . H21 H 0.4649 -0.2919 0.6953 0.046 Uiso 1 1 calc R . . S1 S 0.07944(16) 0.64060(12) 0.54460(18) 0.0590(7) Uani 1 1 d . . . N1 N -0.0301(4) 0.6228(3) 0.6569(4) 0.0415(17) Uani 1 1 d . . . C3 C 0.1350(5) 0.3245(4) 0.7050(6) 0.047(2) Uani 1 1 d . . . H3 H 0.1154 0.3036 0.7551 0.056 Uiso 1 1 calc R . . C8 C 0.1206(5) 0.4912(4) 0.6002(6) 0.042(2) Uani 1 1 d . . . H8 H 0.1492 0.5134 0.5567 0.051 Uiso 1 1 calc R . . C4 C 0.1219(5) 0.3896(4) 0.6943(6) 0.041(2) Uani 1 1 d . . . H4 H 0.0964 0.4137 0.7384 0.050 Uiso 1 1 calc R . . C11 C -0.0437(6) 0.6846(4) 0.6232(6) 0.048(2) Uani 1 1 d . . . H11 H -0.0881 0.7129 0.6411 0.057 Uiso 1 1 calc R . . C5 C 0.1450(5) 0.4226(4) 0.6194(6) 0.042(2) Uani 1 1 d . . . C10 C 0.0336(5) 0.5921(4) 0.6196(5) 0.038(2) Uani 1 1 d . . . C2 C 0.1759(5) 0.2864(4) 0.6462(5) 0.0350(19) Uani 1 1 d . . . C9 C 0.0612(5) 0.5247(4) 0.6392(6) 0.047(2) Uani 1 1 d . . . H9 H 0.0344 0.5025 0.6841 0.056 Uiso 1 1 calc R . . C12 C 0.0096(6) 0.7033(4) 0.5629(6) 0.056(3) Uani 1 1 d . . . H12 H 0.0083 0.7451 0.5348 0.067 Uiso 1 1 calc R . . C6 C 0.1882(5) 0.3858(4) 0.5617(6) 0.043(2) Uani 1 1 d . . . H6 H 0.2068 0.4067 0.5112 0.052 Uiso 1 1 calc R . . C7 C 0.2055(5) 0.3191(4) 0.5749(6) 0.042(2) Uani 1 1 d . . . H7 H 0.2377 0.2958 0.5352 0.050 Uiso 1 1 calc R . . H9B H 0.269(6) 0.059(5) 0.853(6) 0.08(3) Uiso 1 1 d . . . H9A H 0.245(7) 0.162(6) 0.848(7) 0.12(4) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0320(3) 0.0379(4) 0.0424(4) 0.0033(3) 0.0065(3) -0.0025(3) Cd2 0.0309(3) 0.0349(4) 0.0495(4) 0.0019(3) 0.0038(3) 0.0005(3) O9 0.033(3) 0.043(4) 0.039(3) 0.006(3) 0.005(3) -0.004(3) O5 0.040(3) 0.041(4) 0.051(4) 0.002(3) 0.015(3) 0.001(3) O4 0.035(3) 0.041(4) 0.056(4) 0.001(3) 0.006(3) -0.004(3) O2 0.035(3) 0.032(3) 0.063(4) -0.001(3) 0.008(3) -0.002(3) O1 0.048(4) 0.041(4) 0.047(4) 0.008(3) 0.011(3) 0.013(3) O7 0.031(3) 0.049(4) 0.092(5) 0.024(4) 0.007(3) 0.000(3) O3 0.037(3) 0.039(4) 0.056(4) -0.007(3) -0.001(3) 0.007(3) C31 0.033(5) 0.053(6) 0.036(5) -0.002(4) 0.003(4) -0.005(4) C15 0.030(5) 0.037(5) 0.054(6) -0.006(4) -0.005(4) -0.003(4) C16 0.027(5) 0.046(6) 0.050(6) -0.007(4) -0.002(4) 0.003(4) C28 0.046(5) 0.058(6) 0.030(5) -0.004(5) -0.001(4) 0.024(5) C30 0.031(5) 0.052(6) 0.051(6) -0.013(5) 0.010(4) -0.008(4) C26 0.027(4) 0.048(5) 0.025(4) 0.003(4) 0.008(3) 0.002(4) C14 0.031(4) 0.042(5) 0.030(4) 0.001(4) 0.008(3) 0.003(4) C29 0.028(5) 0.057(6) 0.054(6) -0.013(5) 0.010(4) -0.002(4) C27 0.046(5) 0.049(6) 0.039(5) 0.017(4) 0.013(4) 0.014(4) C13 0.046(6) 0.045(6) 0.027(5) -0.001(4) 0.009(4) 0.004(5) C17 0.037(5) 0.036(5) 0.045(5) 0.005(4) 0.010(4) 0.005(4) C18 0.029(5) 0.039(6) 0.082(7) -0.006(5) 0.000(5) -0.005(4) O6 0.059(4) 0.050(4) 0.057(4) 0.002(3) 0.025(3) -0.008(3) O8 0.044(4) 0.047(4) 0.054(4) 0.008(3) -0.006(3) -0.012(3) C1 0.037(5) 0.040(5) 0.037(5) 0.001(4) 0.001(4) 0.005(4) C38 0.032(5) 0.042(5) 0.034(5) 0.007(4) 0.009(4) 0.000(4) C25 0.034(5) 0.056(6) 0.035(5) 0.005(4) 0.004(4) 0.007(4) C37 0.042(5) 0.039(5) 0.037(5) 0.014(4) 0.008(4) 0.004(4) C19 0.028(5) 0.039(6) 0.068(6) -0.003(5) -0.006(4) 0.005(4) C39 0.026(5) 0.048(6) 0.064(6) 0.005(5) -0.001(4) -0.004(4) C32 0.051(6) 0.078(8) 0.078(8) -0.026(6) 0.021(6) -0.011(6) C43 0.041(5) 0.046(6) 0.080(7) 0.021(5) -0.021(5) -0.012(4) S4 0.0459(14) 0.0407(15) 0.090(2) 0.0103(13) -0.0145(13) 0.0003(11) N4 0.034(4) 0.033(4) 0.041(4) 0.003(3) 0.000(3) -0.004(3) C46 0.036(5) 0.047(6) 0.048(5) 0.006(4) 0.002(4) -0.002(4) C47 0.055(6) 0.036(6) 0.071(7) 0.017(5) 0.004(5) 0.000(4) C48 0.033(5) 0.031(5) 0.058(6) 0.002(4) -0.001(4) -0.004(4) C45 0.035(5) 0.030(5) 0.047(5) -0.002(4) -0.001(4) -0.006(4) C41 0.026(4) 0.038(5) 0.057(6) 0.002(4) -0.006(4) -0.003(4) C42 0.048(6) 0.060(7) 0.065(7) 0.021(5) -0.016(5) -0.019(5) C40 0.033(5) 0.044(6) 0.096(8) 0.012(5) -0.009(5) 0.003(4) C44 0.041(6) 0.040(6) 0.088(8) 0.007(5) 0.003(5) 0.001(4) S3 0.0420(14) 0.088(2) 0.0503(15) -0.0168(14) 0.0103(11) 0.0167(13) N3 0.030(4) 0.067(6) 0.041(4) -0.010(4) -0.001(3) -0.004(4) C34 0.037(5) 0.066(7) 0.057(6) -0.031(5) 0.002(5) -0.008(5) C36 0.064(7) 0.055(7) 0.055(6) 0.010(5) 0.018(5) 0.023(5) C35 0.068(7) 0.057(7) 0.067(7) -0.002(5) 0.020(6) 0.032(5) C33 0.044(6) 0.062(7) 0.095(8) -0.004(6) 0.027(6) -0.009(5) S2 0.0494(15) 0.0496(16) 0.0811(19) -0.0156(13) -0.0161(13) 0.0025(12) N2 0.046(4) 0.032(4) 0.033(4) -0.003(3) 0.004(3) 0.006(3) C20 0.026(4) 0.045(5) 0.050(6) 0.004(4) 0.000(4) 0.000(4) C24 0.060(6) 0.046(6) 0.049(6) -0.013(5) -0.005(5) -0.003(5) C22 0.032(5) 0.044(5) 0.039(5) 0.005(4) -0.001(4) 0.005(4) C23 0.052(6) 0.045(6) 0.034(5) -0.005(4) 0.012(4) 0.005(4) C21 0.038(5) 0.039(5) 0.038(5) -0.003(4) 0.002(4) -0.002(4) S1 0.0556(15) 0.0508(16) 0.0767(18) 0.0152(13) 0.0301(14) 0.0059(12) N1 0.042(4) 0.043(5) 0.039(4) -0.003(4) 0.003(3) 0.005(3) C3 0.049(6) 0.039(6) 0.056(6) 0.001(4) 0.021(5) -0.001(4) C8 0.038(5) 0.041(5) 0.051(6) 0.004(4) 0.015(4) 0.002(4) C4 0.042(5) 0.035(5) 0.051(6) 0.003(4) 0.016(4) 0.007(4) C11 0.047(6) 0.041(6) 0.054(6) -0.002(5) 0.006(5) 0.008(4) C5 0.032(5) 0.045(6) 0.051(6) -0.005(5) 0.013(4) 0.002(4) C10 0.034(5) 0.037(5) 0.045(5) 0.001(4) 0.014(4) -0.003(4) C2 0.026(4) 0.043(5) 0.035(5) -0.005(4) -0.001(4) -0.004(4) C9 0.045(5) 0.050(6) 0.047(6) -0.001(5) 0.012(4) 0.005(4) C12 0.059(6) 0.046(6) 0.063(7) 0.013(5) 0.009(5) 0.008(5) C6 0.047(5) 0.039(6) 0.046(5) 0.004(4) 0.015(4) -0.004(4) C7 0.039(5) 0.042(6) 0.046(6) -0.002(4) 0.011(4) 0.004(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O4 2.223(6) . ? Cd1 O5 2.280(6) . ? Cd1 O9 2.314(5) . ? Cd1 N3 2.332(7) 2_646 ? Cd1 O1 2.350(5) . ? Cd1 N2 2.442(6) 2_656 ? Cd2 O2 2.225(5) . ? Cd2 O7 2.238(6) . ? Cd2 N4 2.320(6) 2_556 ? Cd2 O9 2.336(5) . ? Cd2 O3 2.352(5) . ? Cd2 N1 2.440(7) 2_546 ? O5 C25 1.261(9) . ? O4 C13 1.262(9) . ? O2 C1 1.277(9) . ? O1 C1 1.264(9) . ? O7 C37 1.262(9) . ? O3 C13 1.247(9) . ? C31 C30 1.375(11) . ? C31 C26 1.394(10) . ? C15 C16 1.367(11) . ? C15 C14 1.396(10) . ? C16 C17 1.384(11) . ? C28 C29 1.374(12) . ? C28 C27 1.379(11) . ? C30 C29 1.390(11) . ? C26 C27 1.392(11) . ? C26 C25 1.479(11) . ? C14 C19 1.385(11) . ? C14 C13 1.498(11) . ? C29 C32 1.519(12) . ? C17 C18 1.386(11) . ? C17 C20 1.464(11) . ? C18 C19 1.373(11) . ? O6 C25 1.256(9) . ? O8 C37 1.253(9) . ? C1 C2 1.489(11) . ? C38 C39 1.380(11) . ? C38 C43 1.400(11) . ? C38 C37 1.497(11) . ? C39 C40 1.366(11) . ? C32 C33 1.348(12) . ? C43 C42 1.377(12) . ? S4 C47 1.699(9) . ? S4 C46 1.722(8) . ? N4 C46 1.319(10) . ? N4 C48 1.364(9) . ? N4 Cd2 2.320(6) 2_546 ? C46 C45 1.434(11) . ? C47 C48 1.332(11) . ? C45 C44 1.332(11) . ? C41 C40 1.383(11) . ? C41 C42 1.383(11) . ? C41 C44 1.479(11) . ? S3 C35 1.717(10) . ? S3 C34 1.725(9) . ? N3 C34 1.295(11) . ? N3 C36 1.364(11) . ? N3 Cd1 2.332(7) 2_656 ? C34 C33 1.408(12) . ? C36 C35 1.339(11) . ? S2 C24 1.715(9) . ? S2 C22 1.716(8) . ? N2 C22 1.332(9) . ? N2 C23 1.364(9) . ? N2 Cd1 2.442(6) 2_646 ? C20 C21 1.339(10) . ? C24 C23 1.305(11) . ? C22 C21 1.457(11) . ? S1 C12 1.700(9) . ? S1 C10 1.719(8) . ? N1 C10 1.334(9) . ? N1 C11 1.361(10) . ? N1 Cd2 2.440(7) 2_556 ? C3 C4 1.346(11) . ? C3 C2 1.387(11) . ? C8 C9 1.327(10) . ? C8 C5 1.462(11) . ? C4 C5 1.401(11) . ? C11 C12 1.353(12) . ? C5 C6 1.380(11) . ? C10 C9 1.454(11) . ? C2 C7 1.393(11) . ? C6 C7 1.389(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Cd1 O5 172.1(2) . . ? O4 Cd1 O9 87.5(2) . . ? O5 Cd1 O9 87.8(2) . . ? O4 Cd1 N3 97.8(2) . 2_646 ? O5 Cd1 N3 87.4(2) . 2_646 ? O9 Cd1 N3 173.9(2) . 2_646 ? O4 Cd1 O1 105.2(2) . . ? O5 Cd1 O1 81.14(19) . . ? O9 Cd1 O1 90.70(19) . . ? N3 Cd1 O1 85.0(2) 2_646 . ? O4 Cd1 N2 81.1(2) . 2_656 ? O5 Cd1 N2 92.7(2) . 2_656 ? O9 Cd1 N2 91.0(2) . 2_656 ? N3 Cd1 N2 92.9(2) 2_646 2_656 ? O1 Cd1 N2 173.6(2) . 2_656 ? O2 Cd2 O7 165.1(2) . . ? O2 Cd2 N4 99.9(2) . 2_556 ? O7 Cd2 N4 89.9(2) . 2_556 ? O2 Cd2 O9 86.0(2) . . ? O7 Cd2 O9 85.6(2) . . ? N4 Cd2 O9 171.4(2) 2_556 . ? O2 Cd2 O3 111.6(2) . . ? O7 Cd2 O3 80.3(2) . . ? N4 Cd2 O3 84.1(2) 2_556 . ? O9 Cd2 O3 87.92(19) . . ? O2 Cd2 N1 82.6(2) . 2_546 ? O7 Cd2 N1 86.0(2) . 2_546 ? N4 Cd2 N1 91.2(2) 2_556 2_546 ? O9 Cd2 N1 95.8(2) . 2_546 ? O3 Cd2 N1 165.6(2) . 2_546 ? Cd1 O9 Cd2 106.9(2) . . ? C25 O5 Cd1 126.6(5) . . ? C13 O4 Cd1 126.8(5) . . ? C1 O2 Cd2 125.3(5) . . ? C1 O1 Cd1 123.7(5) . . ? C37 O7 Cd2 127.1(5) . . ? C13 O3 Cd2 129.4(5) . . ? C30 C31 C26 121.3(8) . . ? C16 C15 C14 121.8(7) . . ? C15 C16 C17 120.9(7) . . ? C29 C28 C27 120.3(8) . . ? C31 C30 C29 120.1(8) . . ? C27 C26 C31 117.4(8) . . ? C27 C26 C25 121.6(7) . . ? C31 C26 C25 120.8(7) . . ? C19 C14 C15 117.1(7) . . ? C19 C14 C13 122.1(7) . . ? C15 C14 C13 120.8(7) . . ? C28 C29 C30 119.3(8) . . ? C28 C29 C32 121.5(8) . . ? C30 C29 C32 119.2(8) . . ? C28 C27 C26 121.4(8) . . ? O3 C13 O4 125.4(8) . . ? O3 C13 C14 118.4(7) . . ? O4 C13 C14 116.2(7) . . ? C16 C17 C18 117.4(8) . . ? C16 C17 C20 122.9(7) . . ? C18 C17 C20 119.6(8) . . ? C19 C18 C17 121.9(8) . . ? O1 C1 O2 124.2(8) . . ? O1 C1 C2 119.3(7) . . ? O2 C1 C2 116.5(7) . . ? C39 C38 C43 117.7(8) . . ? C39 C38 C37 123.0(7) . . ? C43 C38 C37 119.3(7) . . ? O6 C25 O5 125.3(8) . . ? O6 C25 C26 118.6(7) . . ? O5 C25 C26 116.1(7) . . ? O8 C37 O7 125.8(8) . . ? O8 C37 C38 118.0(7) . . ? O7 C37 C38 116.2(8) . . ? C18 C19 C14 120.8(7) . . ? C40 C39 C38 119.9(8) . . ? C33 C32 C29 127.2(9) . . ? C42 C43 C38 121.1(8) . . ? C47 S4 C46 90.1(4) . . ? C46 N4 C48 110.9(7) . . ? C46 N4 Cd2 126.7(5) . 2_546 ? C48 N4 Cd2 121.5(5) . 2_546 ? N4 C46 C45 123.5(7) . . ? N4 C46 S4 112.8(6) . . ? C45 C46 S4 123.7(6) . . ? C48 C47 S4 110.0(7) . . ? C47 C48 N4 116.2(7) . . ? C44 C45 C46 125.9(8) . . ? C40 C41 C42 116.3(8) . . ? C40 C41 C44 120.7(8) . . ? C42 C41 C44 123.0(8) . . ? C43 C42 C41 121.3(8) . . ? C39 C40 C41 123.6(8) . . ? C45 C44 C41 124.8(8) . . ? C35 S3 C34 88.5(5) . . ? C34 N3 C36 111.0(7) . . ? C34 N3 Cd1 128.9(6) . 2_656 ? C36 N3 Cd1 119.1(6) . 2_656 ? N3 C34 C33 124.1(8) . . ? N3 C34 S3 114.6(7) . . ? C33 C34 S3 121.3(8) . . ? C35 C36 N3 115.4(9) . . ? C36 C35 S3 110.4(8) . . ? C32 C33 C34 127.3(10) . . ? C24 S2 C22 88.8(4) . . ? C22 N2 C23 110.2(7) . . ? C22 N2 Cd1 125.1(5) . 2_646 ? C23 N2 Cd1 122.5(5) . 2_646 ? C21 C20 C17 124.1(7) . . ? C23 C24 S2 111.3(7) . . ? N2 C22 C21 122.5(7) . . ? N2 C22 S2 113.5(6) . . ? C21 C22 S2 123.8(6) . . ? C24 C23 N2 116.2(8) . . ? C20 C21 C22 125.7(8) . . ? C12 S1 C10 90.4(4) . . ? C10 N1 C11 110.8(7) . . ? C10 N1 Cd2 129.4(5) . 2_556 ? C11 N1 Cd2 119.7(5) . 2_556 ? C4 C3 C2 123.0(8) . . ? C9 C8 C5 124.7(8) . . ? C3 C4 C5 121.3(8) . . ? C12 C11 N1 115.9(8) . . ? C6 C5 C4 116.3(8) . . ? C6 C5 C8 121.4(8) . . ? C4 C5 C8 122.2(7) . . ? N1 C10 C9 124.0(7) . . ? N1 C10 S1 113.0(6) . . ? C9 C10 S1 123.0(6) . . ? C3 C2 C7 116.6(8) . . ? C3 C2 C1 121.2(7) . . ? C7 C2 C1 122.2(7) . . ? C8 C9 C10 125.9(8) . . ? C11 C12 S1 109.9(7) . . ? C5 C6 C7 122.3(8) . . ? C6 C7 C2 120.2(8) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.217 _refine_diff_density_min -0.635 _refine_diff_density_rms 0.123 #===END data_compound2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H19 Cd N2 O4.50' _chemical_formula_weight 567.85 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' 'Cd' 'Cd' -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 11.4582(17) _cell_length_b 16.087(2) _cell_length_c 25.536(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.230(3) _cell_angle_gamma 90.00 _cell_volume 4705.7(12) _cell_formula_units_Z 8 _cell_measurement_temperature 198(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.603 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2280 _exptl_absorpt_coefficient_mu 0.969 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 198(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 ? _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 9312 _diffrn_reflns_av_R_equivalents 0.0639 _diffrn_reflns_av_sigmaI/netI 0.0913 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 28.27 _reflns_number_total 3996 _reflns_number_gt 2238 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1276P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3996 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1224 _refine_ls_R_factor_gt 0.0661 _refine_ls_wR_factor_ref 0.2034 _refine_ls_wR_factor_gt 0.1733 _refine_ls_goodness_of_fit_ref 0.980 _refine_ls_restrained_S_all 0.980 _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 0.84911(5) 0.21012(4) 0.72151(2) 0.0367(2) Uani 1 1 d . . . O5 O 1.0000 0.2960(6) 0.7500 0.043(2) Uani 1 2 d S . . O3 O 0.8496(5) 0.2900(4) 0.6457(2) 0.0466(16) Uani 1 1 d . . . O1 O 0.8261(5) 0.1191(4) 0.7890(2) 0.0389(14) Uani 1 1 d . . . C3 C 0.7838(7) 0.0149(6) 0.8776(3) 0.043(2) Uani 1 1 d . . . H3 H 0.7436 -0.0020 0.8464 0.051 Uiso 1 1 calc R . . C1 C 0.9052(7) 0.1137(5) 0.8243(3) 0.0315(19) Uani 1 1 d . . . C2 C 0.8711(6) 0.0739(5) 0.8755(3) 0.0308(18) Uani 1 1 d . . . C7 C 0.9306(7) 0.0962(6) 0.9218(4) 0.042(2) Uani 1 1 d . . . H7 H 0.9930 0.1350 0.9204 0.050 Uiso 1 1 calc R . . C6 C 0.9007(7) 0.0634(6) 0.9691(3) 0.041(2) Uani 1 1 d . . . H6 H 0.9415 0.0808 1.0000 0.049 Uiso 1 1 calc R . . C5 C 0.8120(7) 0.0053(5) 0.9728(3) 0.039(2) Uani 1 1 d . . . O4 O 1.0147(7) 0.3624(5) 0.6596(3) 0.065(2) Uani 1 1 d . . . C15 C 0.9424(8) 0.3227(6) 0.6306(4) 0.046(2) Uani 1 1 d . . . C17 C 0.9021(8) 0.2697(6) 0.5390(4) 0.047(2) Uani 1 1 d . . . H17 H 0.8260 0.2543 0.5494 0.056 Uiso 1 1 calc R . . C16 C 0.9759(8) 0.3105(6) 0.5745(4) 0.042(2) Uani 1 1 d . . . C4 C 0.7545(7) -0.0203(6) 0.9262(4) 0.044(2) Uani 1 1 d . . . H4 H 0.6955 -0.0617 0.9276 0.052 Uiso 1 1 calc R . . O2 O 1.0089(5) 0.1349(4) 0.8207(3) 0.0519(18) Uani 1 1 d . . . C18 C 0.9370(8) 0.2515(6) 0.4894(4) 0.044(2) Uani 1 1 d . . . H18 H 0.8842 0.2241 0.4660 0.053 Uiso 1 1 calc R . . C21 C 1.0837(8) 0.3356(7) 0.5577(4) 0.053(3) Uani 1 1 d . . . H21 H 1.1345 0.3655 0.5808 0.063 Uiso 1 1 calc R . . N1 N 0.7082(6) -0.1338(5) 1.1751(3) 0.0383(17) Uani 1 1 d . . . C9 C 0.6733(7) -0.0475(6) 1.0389(3) 0.037(2) Uani 1 1 d . . . H9 H 0.6121 -0.0474 1.0132 0.044 Uiso 1 1 calc R . . C14 C 0.7279(7) -0.1129(6) 1.1257(3) 0.040(2) Uani 1 1 d . . . H14 H 0.8017 -0.1260 1.1116 0.048 Uiso 1 1 calc R . . C10 C 0.6458(7) -0.0725(5) 1.0937(4) 0.039(2) Uani 1 1 d . . . C11 C 0.5403(8) -0.0560(7) 1.1155(4) 0.056(3) Uani 1 1 d . . . H11 H 0.4813 -0.0286 1.0953 0.067 Uiso 1 1 calc R . . C8 C 0.7799(7) -0.0252(6) 1.0247(3) 0.044(2) Uani 1 1 d . . . H8 H 0.8406 -0.0295 1.0504 0.053 Uiso 1 1 calc R . . C13 C 0.6060(8) -0.1165(7) 1.1948(4) 0.054(3) Uani 1 1 d . . . H13 H 0.5924 -0.1309 1.2302 0.064 Uiso 1 1 calc R . . C12 C 0.5184(9) -0.0785(8) 1.1666(5) 0.078(4) Uani 1 1 d . . . H12 H 0.4447 -0.0680 1.1816 0.093 Uiso 1 1 calc R . . N2 N 1.2235(6) 0.1994(5) 0.2658(3) 0.0414(18) Uani 1 1 d . . . C28 C 1.1727(8) 0.2190(6) 0.3114(4) 0.047(2) Uani 1 1 d . . . H28 H 1.1821 0.2742 0.3241 0.056 Uiso 1 1 calc R . . C24 C 1.1085(8) 0.1649(6) 0.3407(4) 0.046(2) Uani 1 1 d . . . C26 C 1.1535(8) 0.0625(6) 0.2763(4) 0.056(3) Uani 1 1 d . . . H26 H 1.1480 0.0075 0.2629 0.067 Uiso 1 1 calc R . . C25 C 1.0989(8) 0.0833(6) 0.3215(4) 0.055(3) Uani 1 1 d . . . H25 H 1.0550 0.0430 0.3399 0.066 Uiso 1 1 calc R . . C22 C 1.0949(8) 0.2503(7) 0.4206(4) 0.052(2) Uani 1 1 d . . . H22 H 1.1584 0.2822 0.4082 0.062 Uiso 1 1 calc R . . C27 C 1.2161(8) 0.1217(7) 0.2505(4) 0.056(3) Uani 1 1 d . . . H27 H 1.2563 0.1056 0.2199 0.067 Uiso 1 1 calc R . . C23 C 1.0542(9) 0.1888(7) 0.3897(4) 0.058(3) Uani 1 1 d . . . H23 H 0.9867 0.1594 0.4002 0.070 Uiso 1 1 calc R . . C19 C 1.0488(8) 0.2723(5) 0.4725(4) 0.040(2) Uani 1 1 d . . . C20 C 1.1185(9) 0.3173(7) 0.5071(4) 0.055(3) Uani 1 1 d . . . H20 H 1.1925 0.3363 0.4959 0.066 Uiso 1 1 calc R . . H5 H 1.009(6) 0.334(5) 0.721(3) 0.03(2) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0445(4) 0.0466(4) 0.0191(3) 0.0001(3) 0.0068(2) 0.0028(3) O5 0.046(6) 0.056(6) 0.025(5) 0.000 0.006(4) 0.000 O3 0.060(4) 0.059(4) 0.021(3) 0.007(3) 0.012(3) 0.001(3) O1 0.052(4) 0.044(4) 0.020(3) 0.003(3) 0.000(2) 0.003(3) C3 0.047(6) 0.057(6) 0.023(5) 0.003(4) -0.005(3) -0.006(4) C1 0.035(5) 0.034(5) 0.026(5) 0.002(4) 0.009(3) 0.003(3) C2 0.028(4) 0.041(5) 0.023(4) 0.005(4) 0.002(3) 0.003(3) C7 0.034(5) 0.056(6) 0.035(5) -0.005(4) 0.000(4) -0.006(4) C6 0.047(6) 0.050(6) 0.027(5) 0.000(4) -0.004(4) -0.004(4) C5 0.053(6) 0.037(5) 0.026(5) 0.005(4) 0.002(4) -0.005(4) O4 0.104(6) 0.070(5) 0.022(4) 0.001(4) 0.012(3) -0.024(4) C15 0.057(7) 0.047(5) 0.035(6) 0.004(5) 0.012(4) 0.008(5) C17 0.049(6) 0.058(7) 0.034(6) 0.013(4) 0.009(4) 0.003(4) C16 0.048(6) 0.048(6) 0.031(5) 0.006(4) 0.011(4) 0.003(4) C4 0.032(5) 0.056(6) 0.042(6) 0.012(4) 0.003(4) -0.012(4) O2 0.046(4) 0.071(5) 0.040(4) 0.013(4) 0.013(3) -0.011(3) C18 0.043(6) 0.058(6) 0.030(5) -0.001(4) -0.001(4) 0.009(4) C21 0.050(6) 0.068(7) 0.040(6) -0.002(5) 0.012(4) -0.003(5) N1 0.037(4) 0.055(5) 0.023(4) 0.004(3) 0.005(3) 0.000(3) C9 0.037(5) 0.045(5) 0.028(5) 0.007(4) 0.004(3) -0.005(4) C14 0.044(6) 0.048(5) 0.028(5) 0.002(4) 0.006(4) 0.000(4) C10 0.043(6) 0.042(5) 0.033(5) 0.007(4) 0.007(4) -0.003(4) C11 0.057(7) 0.065(7) 0.047(7) 0.021(5) 0.018(5) 0.016(5) C8 0.038(5) 0.069(7) 0.024(5) 0.007(4) 0.000(3) -0.003(4) C13 0.044(6) 0.077(7) 0.040(6) 0.009(5) 0.019(4) 0.016(5) C12 0.049(7) 0.119(11) 0.066(9) 0.030(7) 0.034(6) 0.026(6) N2 0.053(5) 0.046(5) 0.025(4) -0.002(3) 0.014(3) -0.004(3) C28 0.075(7) 0.042(6) 0.024(5) -0.001(4) 0.014(4) -0.011(4) C24 0.056(6) 0.050(6) 0.031(5) -0.003(4) 0.011(4) -0.008(4) C26 0.067(7) 0.050(6) 0.050(7) -0.009(5) 0.018(5) -0.015(5) C25 0.057(6) 0.063(7) 0.045(6) -0.012(5) 0.018(4) -0.027(5) C22 0.065(7) 0.059(6) 0.032(6) -0.002(5) 0.018(4) -0.008(5) C27 0.071(7) 0.058(7) 0.038(6) -0.007(5) 0.022(5) -0.013(5) C23 0.075(7) 0.063(7) 0.037(6) -0.007(5) 0.023(5) -0.026(5) C19 0.046(6) 0.049(6) 0.026(5) 0.006(4) 0.008(4) 0.005(4) C20 0.063(7) 0.057(6) 0.045(7) -0.013(5) 0.015(5) -0.020(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O1 2.280(6) . ? Cd1 O2 2.313(6) 2_756 ? Cd1 O5 2.318(6) . ? Cd1 O3 2.322(6) . ? Cd1 N1 2.331(7) 6 ? Cd1 N2 2.353(7) 8_456 ? O5 Cd1 2.318(6) 2_756 ? O3 C15 1.256(11) . ? O1 C1 1.268(10) . ? C3 C2 1.381(12) . ? C3 C4 1.413(12) . ? C1 O2 1.242(9) . ? C1 C2 1.513(11) . ? C2 C7 1.400(12) . ? C7 C6 1.369(12) . ? C6 C5 1.386(11) . ? C5 C4 1.408(12) . ? C5 C8 1.467(11) . ? O4 C15 1.271(12) . ? C15 C16 1.503(13) . ? C17 C18 1.367(13) . ? C17 C16 1.390(14) . ? C16 C21 1.377(12) . ? O2 Cd1 2.313(6) 2_756 ? C18 C19 1.402(12) . ? C21 C20 1.393(13) . ? N1 C13 1.314(10) . ? N1 C14 1.329(11) . ? N1 Cd1 2.331(7) 6_556 ? C9 C8 1.331(11) . ? C9 C10 1.497(12) . ? C14 C10 1.394(12) . ? C10 C11 1.368(12) . ? C11 C12 1.381(14) . ? C13 C12 1.367(15) . ? N2 C27 1.312(11) . ? N2 C28 1.351(11) . ? N2 Cd1 2.353(7) 8 ? C28 C24 1.371(12) . ? C24 C25 1.405(13) . ? C24 C23 1.462(13) . ? C26 C25 1.368(12) . ? C26 C27 1.370(13) . ? C22 C23 1.344(14) . ? C22 C19 1.479(12) . ? C19 C20 1.383(14) . ? 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 O2 96.3(2) . 2_756 ? O1 Cd1 O5 104.06(19) . . ? O2 Cd1 O5 86.0(2) 2_756 . ? O1 Cd1 O3 170.7(2) . . ? O2 Cd1 O3 83.5(2) 2_756 . ? O5 Cd1 O3 85.2(2) . . ? O1 Cd1 N1 87.5(2) . 6 ? O2 Cd1 N1 88.5(2) 2_756 6 ? O5 Cd1 N1 167.71(18) . 6 ? O3 Cd1 N1 83.2(2) . 6 ? O1 Cd1 N2 87.3(2) . 8_456 ? O2 Cd1 N2 172.4(3) 2_756 8_456 ? O5 Cd1 N2 86.6(2) . 8_456 ? O3 Cd1 N2 94.0(2) . 8_456 ? N1 Cd1 N2 98.3(3) 6 8_456 ? Cd1 O5 Cd1 106.8(4) . 2_756 ? C15 O3 Cd1 120.4(6) . . ? C1 O1 Cd1 119.3(5) . . ? C2 C3 C4 119.7(8) . . ? O2 C1 O1 126.7(8) . . ? O2 C1 C2 116.5(7) . . ? O1 C1 C2 116.8(7) . . ? C3 C2 C7 118.9(8) . . ? C3 C2 C1 121.7(7) . . ? C7 C2 C1 119.4(7) . . ? C6 C7 C2 121.4(8) . . ? C7 C6 C5 121.1(8) . . ? C6 C5 C4 118.1(8) . . ? C6 C5 C8 119.0(8) . . ? C4 C5 C8 122.9(8) . . ? O3 C15 O4 125.2(9) . . ? O3 C15 C16 118.3(9) . . ? O4 C15 C16 116.4(8) . . ? C18 C17 C16 121.3(9) . . ? C21 C16 C17 118.2(9) . . ? C21 C16 C15 120.5(9) . . ? C17 C16 C15 121.3(8) . . ? C5 C4 C3 120.7(8) . . ? C1 O2 Cd1 149.6(6) . 2_756 ? C17 C18 C19 121.4(9) . . ? C16 C21 C20 120.3(9) . . ? C13 N1 C14 118.7(8) . . ? C13 N1 Cd1 122.0(6) . 6_556 ? C14 N1 Cd1 119.0(5) . 6_556 ? C8 C9 C10 122.7(8) . . ? N1 C14 C10 123.2(8) . . ? C11 C10 C14 116.3(9) . . ? C11 C10 C9 122.3(8) . . ? C14 C10 C9 121.4(8) . . ? C10 C11 C12 120.9(10) . . ? C9 C8 C5 125.9(8) . . ? N1 C13 C12 122.9(10) . . ? C13 C12 C11 118.0(9) . . ? C27 N2 C28 116.9(8) . . ? C27 N2 Cd1 118.8(6) . 8 ? C28 N2 Cd1 123.3(6) . 8 ? N2 C28 C24 124.6(9) . . ? C28 C24 C25 116.3(9) . . ? C28 C24 C23 122.9(9) . . ? C25 C24 C23 120.8(8) . . ? C25 C26 C27 119.4(10) . . ? C26 C25 C24 119.3(9) . . ? C23 C22 C19 125.1(9) . . ? N2 C27 C26 123.4(9) . . ? C22 C23 C24 123.2(9) . . ? C20 C19 C18 116.6(8) . . ? C20 C19 C22 118.9(8) . . ? C18 C19 C22 124.5(9) . . ? C19 C20 C21 122.0(9) . . ? _diffrn_measured_fraction_theta_max 0.684 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.684 _refine_diff_density_max 1.667 _refine_diff_density_min -1.328 _refine_diff_density_rms 0.157 #===END