# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_publication_text _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author_name 'Christopher Sumby' _publ_contact_author_address ;School of Chemistry & Physics The University of Adelaide Adelaide SA 5005 Australia ; _publ_contact_author_email christopher.sumby@adelaide.edu.au _publ_contact_author_phone '+61 8 83037406' _publ_contact_author_fax '+61 8 83034358' loop_ _publ_author_name M.Abdul-Kadir L.Hanton C.Sumby data_compound_5 _database_code_depnum_ccdc_archive 'CCDC 823062' #TrackingRef '- AdelCS9_MAK1resub.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H16 Cd N4 O9' _chemical_formula_weight 484.70 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' _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 6.1440(12) _cell_length_b 10.443(2) _cell_length_c 15.363(3) _cell_angle_alpha 108.94(3) _cell_angle_beta 91.62(3) _cell_angle_gamma 103.19(3) _cell_volume 902.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 10765 _cell_measurement_theta_min 2.8120 _cell_measurement_theta_max 29.2021 _exptl_crystal_description rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.784 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 484 _exptl_absorpt_coefficient_mu 1.266 _exptl_absorpt_correction_T_min 0.96944 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_detector_area_resol_mean 16.2413 _diffrn_measurement_method '\w scans' _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 43.00 89.00 1.0000 11.0000 omega____ theta____ kappa____ phi______ frames - 18.9393 54.0000 -1.0000 46 #__ type_ start__ end____ width___ exp.time_ 2 omega -52.00 88.00 1.0000 11.0000 omega____ theta____ kappa____ phi______ frames - 18.9393 0.0000 -180.0000 140 #__ type_ start__ end____ width___ exp.time_ 3 omega -100.00 -60.00 1.0000 11.0000 omega____ theta____ kappa____ phi______ frames - -20.1111 179.0000 30.0000 40 #__ type_ start__ end____ width___ exp.time_ 4 omega -100.00 -57.00 1.0000 11.0000 omega____ theta____ kappa____ phi______ frames - -20.1111 179.0000 -150.0000 43 #__ type_ start__ end____ width___ exp.time_ 5 omega -79.00 12.00 1.0000 11.0000 omega____ theta____ kappa____ phi______ frames - -20.1111 -77.0000 -180.0000 91 #__ type_ start__ end____ width___ exp.time_ 6 omega -30.00 11.00 1.0000 11.0000 omega____ theta____ kappa____ phi______ frames - -20.1111 -77.0000 0.0000 41 #__ type_ start__ end____ width___ exp.time_ 7 omega 34.00 97.00 1.0000 11.0000 omega____ theta____ kappa____ phi______ frames - 18.9393 179.0000 150.0000 63 #__ type_ start__ end____ width___ exp.time_ 8 omega -9.00 92.00 1.0000 11.0000 omega____ theta____ kappa____ phi______ frames - 18.9393 37.0000 -30.0000 101 #__ type_ start__ end____ width___ exp.time_ 9 omega -54.00 46.00 1.0000 11.0000 omega____ theta____ kappa____ phi______ frames - 18.9393 -37.0000 -30.0000 100 #__ type_ start__ end____ width___ exp.time_ 10 omega -3.00 89.00 1.0000 11.0000 omega____ theta____ kappa____ phi______ frames - 18.9393 54.0000 145.0000 92 #__ type_ start__ end____ width___ exp.time_ 11 omega -100.00 -32.00 1.0000 11.0000 omega____ theta____ kappa____ phi______ frames - -20.1111 179.0000 60.0000 68 #__ type_ start__ end____ width___ exp.time_ 12 omega -100.00 -32.00 1.0000 11.0000 omega____ theta____ kappa____ phi______ frames - -20.1111 179.0000 150.0000 68 ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16419 _diffrn_reflns_av_R_equivalents 0.0303 _diffrn_reflns_av_sigmaI/netI 0.0400 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.82 _diffrn_reflns_theta_max 29.30 _reflns_number_total 4401 _reflns_number_gt 3782 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour)' _computing_publication_material 'local program' _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^)+(0.0424P)^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 4401 _refine_ls_number_parameters 299 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0348 _refine_ls_R_factor_gt 0.0275 _refine_ls_wR_factor_ref 0.0677 _refine_ls_wR_factor_gt 0.0667 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 0.999 _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 0.26201(3) 0.491164(19) 0.069541(13) 0.01209(6) Uani 1 1 d . . . N1 N 0.1342(3) 0.2847(2) 0.10439(14) 0.0122(4) Uani 1 1 d . . . C2 C -0.0727(4) 0.2053(3) 0.07043(17) 0.0133(5) Uani 1 1 d . . . C3 C -0.1557(4) 0.0790(3) 0.08496(18) 0.0168(5) Uani 1 1 d . . . H3 H -0.3041 0.0241 0.0607 0.020 Uiso 1 1 calc R . . C4 C -0.0167(4) 0.0357(3) 0.13563(19) 0.0200(6) Uani 1 1 d . . . H4 H -0.0686 -0.0500 0.1466 0.024 Uiso 1 1 calc R . . C5 C 0.1992(4) 0.1181(3) 0.17048(18) 0.0180(5) Uani 1 1 d . . . H5 H 0.2972 0.0894 0.2050 0.022 Uiso 1 1 calc R . . C6 C 0.2686(4) 0.2430(3) 0.15384(17) 0.0136(5) Uani 1 1 d . . . C12 C -0.2129(4) 0.2611(3) 0.01554(18) 0.0141(5) Uani 1 1 d . . . O13 O -0.1203(3) 0.37717(18) 0.00680(12) 0.0157(4) Uani 1 1 d . . . O14 O -0.4075(3) 0.18883(19) -0.01620(14) 0.0207(4) Uani 1 1 d . . . C16 C 0.4936(4) 0.3474(3) 0.18899(17) 0.0141(5) Uani 1 1 d . . . O17 O 0.5430(3) 0.44986(19) 0.16347(13) 0.0194(4) Uani 1 1 d . . . N18 N 0.6302(4) 0.3257(2) 0.24820(15) 0.0173(5) Uani 1 1 d . B . H18 H 0.5907 0.2502 0.2636 0.021 Uiso 1 1 calc R . . C19 C 0.8460(4) 0.4265(3) 0.28807(19) 0.0227(6) Uani 1 1 d . . . H19A H 0.9069 0.4683 0.2417 0.027 Uiso 1 1 calc R A 1 H19B H 0.9537 0.3769 0.3027 0.027 Uiso 1 1 calc R A 1 N21 N 0.989(4) 0.702(3) 0.5308(17) 0.045(6) Uani 0.485(9) 1 d P B 1 C22 C 0.987(3) 0.602(3) 0.446(2) 0.037(4) Uani 0.485(9) 1 d P B 1 H22 H 1.1184 0.5691 0.4349 0.044 Uiso 0.485(9) 1 calc PR B 1 C23 C 0.824(6) 0.550(3) 0.3812(19) 0.021(4) Uani 0.485(9) 1 d P B 1 C24 C 0.6368(11) 0.6031(8) 0.3893(5) 0.031(2) Uani 0.485(9) 1 d P B 1 H24 H 0.5186 0.5694 0.3400 0.038 Uiso 0.485(9) 1 calc PR B 1 C25 C 0.6262(12) 0.7077(8) 0.4718(5) 0.037(2) Uani 0.485(9) 1 d P B 1 H25 H 0.5008 0.7477 0.4805 0.044 Uiso 0.485(9) 1 calc PR B 1 C26 C 0.800(2) 0.7504(13) 0.5392(9) 0.046(3) Uani 0.485(9) 1 d P B 1 H26 H 0.7903 0.8192 0.5963 0.055 Uiso 0.485(9) 1 calc PR B 1 N31 N 1.054(4) 0.703(3) 0.5166(19) 0.036(4) Uani 0.515(9) 1 d P B 2 C32 C 1.050(3) 0.610(2) 0.4352(18) 0.028(3) Uani 0.515(9) 1 d P B 2 H32 H 1.1885 0.5993 0.4121 0.033 Uiso 0.515(9) 1 calc PR B 2 C33 C 0.837(5) 0.521(3) 0.377(2) 0.020(4) Uani 0.515(9) 1 d P B 2 C34 C 0.6485(11) 0.5401(8) 0.4184(5) 0.0305(17) Uani 0.515(9) 1 d P B 2 H34 H 0.5061 0.4842 0.3865 0.037 Uiso 0.515(9) 1 calc PR B 2 C35 C 0.6565(12) 0.6371(8) 0.5049(5) 0.038(2) Uani 0.515(9) 1 d P B 2 H35 H 0.5218 0.6504 0.5312 0.045 Uiso 0.515(9) 1 calc PR B 2 C36 C 0.860(2) 0.7135(12) 0.5520(9) 0.038(3) Uani 0.515(9) 1 d P B 2 H36 H 0.8649 0.7769 0.6129 0.046 Uiso 0.515(9) 1 calc PR B 2 O40 O 0.6071(3) 0.64041(18) 0.06138(12) 0.0135(4) Uani 1 1 d . . . H40A H 0.5681 0.6951 0.0405 0.020 Uiso 1 1 d R . . H40B H 0.7021 0.6675 0.1082 0.020 Uiso 1 1 d R . . O41 O 0.2357(3) 0.6474(2) 0.20772(13) 0.0217(4) Uani 1 1 d . . . H41A H 0.3504 0.7141 0.2259 0.033 Uiso 1 1 d R . . H41B H 0.1469 0.7065 0.2161 0.033 Uiso 1 1 d R . . N42 N 0.8101(5) 0.8316(3) 0.2802(2) 0.0404(7) Uani 1 1 d . . . O43 O 0.6207(4) 0.8568(2) 0.27814(17) 0.0397(6) Uani 1 1 d . . . O44 O 0.8790(3) 0.7515(2) 0.21276(13) 0.0239(4) Uani 1 1 d . . . O45 O 0.9759(8) 0.9043(4) 0.3693(3) 0.1128(16) Uani 1 1 d . . . O46 O 0.5936(4) 0.1301(2) 0.34022(15) 0.0347(5) Uani 1 1 d . . . H46A H 0.5967 0.0442 0.3260 0.052 Uiso 1 1 d R . . H46B H 0.6853 0.1741 0.3880 0.052 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 0.00872(9) 0.01149(10) 0.01571(10) 0.00614(7) 0.00008(6) -0.00023(6) N1 0.0120(10) 0.0129(10) 0.0124(10) 0.0056(8) 0.0019(8) 0.0022(8) C2 0.0115(11) 0.0152(12) 0.0131(12) 0.0041(10) 0.0027(9) 0.0037(9) C3 0.0144(12) 0.0147(12) 0.0205(13) 0.0076(11) 0.0006(10) -0.0004(10) C4 0.0233(14) 0.0148(13) 0.0231(14) 0.0116(11) 0.0014(11) -0.0008(11) C5 0.0190(13) 0.0183(13) 0.0185(13) 0.0098(11) -0.0007(11) 0.0037(10) C6 0.0126(11) 0.0146(12) 0.0139(12) 0.0054(10) 0.0022(10) 0.0034(10) C12 0.0132(11) 0.0127(12) 0.0167(13) 0.0047(10) 0.0017(10) 0.0041(10) O13 0.0110(8) 0.0132(9) 0.0231(10) 0.0095(8) -0.0013(7) -0.0010(7) O14 0.0113(9) 0.0139(9) 0.0343(11) 0.0104(8) -0.0054(8) -0.0037(7) C16 0.0130(12) 0.0156(12) 0.0125(12) 0.0035(10) 0.0011(10) 0.0031(10) O17 0.0134(9) 0.0194(10) 0.0260(10) 0.0124(8) -0.0032(8) -0.0011(7) N18 0.0161(10) 0.0162(11) 0.0195(11) 0.0083(9) -0.0035(9) 0.0014(9) C19 0.0172(13) 0.0259(15) 0.0225(15) 0.0088(12) -0.0041(11) 0.0002(11) N21 0.069(17) 0.030(6) 0.019(9) 0.003(6) -0.019(10) -0.007(10) C22 0.022(9) 0.033(7) 0.051(9) 0.010(5) -0.014(8) 0.009(8) C23 0.038(8) 0.009(9) 0.009(4) -0.003(5) 0.002(4) -0.001(6) C24 0.025(3) 0.030(4) 0.030(4) 0.002(3) 0.002(3) 0.001(3) C25 0.034(4) 0.033(4) 0.035(4) 0.002(3) 0.009(3) 0.005(3) C26 0.060(8) 0.037(7) 0.032(6) 0.002(4) 0.010(5) 0.005(5) N31 0.052(9) 0.021(4) 0.033(8) 0.008(4) -0.007(6) 0.006(6) C32 0.017(7) 0.018(4) 0.037(6) -0.001(4) -0.013(6) 0.002(6) C33 0.019(4) 0.009(9) 0.029(6) 0.003(6) 0.001(4) 0.003(6) C34 0.030(3) 0.033(4) 0.031(4) 0.011(3) 0.005(3) 0.012(3) C35 0.039(4) 0.036(4) 0.032(4) -0.001(3) 0.006(3) 0.016(3) C36 0.063(9) 0.029(5) 0.019(4) 0.001(4) 0.002(5) 0.016(5) O40 0.0104(8) 0.0142(9) 0.0157(9) 0.0066(7) -0.0017(7) 0.0008(7) O41 0.0191(9) 0.0176(10) 0.0238(10) 0.0019(8) 0.0008(8) 0.0033(8) N42 0.0482(18) 0.0286(15) 0.0400(17) 0.0128(13) -0.0029(14) 0.0003(13) O43 0.0242(11) 0.0282(12) 0.0525(15) -0.0053(11) -0.0017(11) 0.0076(9) O44 0.0223(10) 0.0271(11) 0.0182(10) 0.0012(9) -0.0015(8) 0.0087(8) O45 0.155(4) 0.085(3) 0.073(3) -0.004(2) -0.047(3) 0.032(3) O46 0.0498(14) 0.0236(11) 0.0299(12) 0.0069(10) -0.0076(11) 0.0122(10) _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 O41 2.255(2) . ? Cd1 O40 2.3198(19) 2_665 ? Cd1 N1 2.357(2) . ? Cd1 O13 2.3580(18) 2_565 ? Cd1 O40 2.3611(18) . ? Cd1 O13 2.3903(19) . ? Cd1 O17 2.4190(18) . ? N1 C2 1.333(3) . ? N1 C6 1.339(3) . ? C2 C3 1.392(4) . ? C2 C12 1.517(3) . ? C3 C4 1.381(4) . ? C3 H3 0.9500 . ? C4 C5 1.388(4) . ? C4 H4 0.9500 . ? C5 C6 1.384(4) . ? C5 H5 0.9500 . ? C6 C16 1.510(3) . ? C12 O14 1.246(3) . ? C12 O13 1.268(3) . ? O13 Cd1 2.3580(18) 2_565 ? C16 O17 1.234(3) . ? C16 N18 1.326(3) . ? N18 C19 1.463(3) . ? N18 H18 0.8800 . ? C19 C33 1.41(3) . ? C19 C23 1.62(3) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? N21 C26 1.36(3) . ? N21 C22 1.37(4) . ? C22 C23 1.28(4) . ? C22 H22 0.9500 . ? C23 C24 1.38(3) . ? C24 C25 1.394(9) . ? C24 H24 0.9500 . ? C25 C26 1.355(14) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? N31 C32 1.31(4) . ? N31 C36 1.34(2) . ? C32 C33 1.49(3) . ? C32 H32 0.9500 . ? C33 C34 1.36(3) . ? C34 C35 1.377(9) . ? C34 H34 0.9500 . ? C35 C36 1.358(15) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? O40 Cd1 2.3198(19) 2_665 ? O40 H40A 0.8147 . ? O40 H40B 0.8402 . ? O41 H41A 0.8354 . ? O41 H41B 0.8954 . ? N42 O43 1.252(4) . ? N42 O44 1.256(4) . ? N42 O45 1.542(4) . ? O46 H46A 0.8570 . ? O46 H46B 0.8411 . ? 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 O41 Cd1 O40 164.33(6) . 2_665 ? O41 Cd1 N1 98.54(7) . . ? O40 Cd1 N1 88.13(7) 2_665 . ? O41 Cd1 O13 90.12(7) . 2_565 ? O40 Cd1 O13 94.23(6) 2_665 2_565 ? N1 Cd1 O13 138.53(7) . 2_565 ? O41 Cd1 O40 89.28(7) . . ? O40 Cd1 O40 76.49(7) 2_665 . ? N1 Cd1 O40 138.44(7) . . ? O13 Cd1 O40 81.70(6) 2_565 . ? O41 Cd1 O13 104.08(7) . . ? O40 Cd1 O13 91.56(7) 2_665 . ? N1 Cd1 O13 68.41(7) . . ? O13 Cd1 O13 70.14(7) 2_565 . ? O40 Cd1 O13 148.56(6) . . ? O41 Cd1 O17 80.94(7) . . ? O40 Cd1 O17 88.72(7) 2_665 . ? N1 Cd1 O17 67.19(7) . . ? O13 Cd1 O17 154.12(6) 2_565 . ? O40 Cd1 O17 74.00(6) . . ? O13 Cd1 O17 135.56(6) . . ? C2 N1 C6 119.7(2) . . ? C2 N1 Cd1 118.93(16) . . ? C6 N1 Cd1 121.27(16) . . ? N1 C2 C3 122.0(2) . . ? N1 C2 C12 116.0(2) . . ? C3 C2 C12 122.0(2) . . ? C4 C3 C2 118.3(2) . . ? C4 C3 H3 120.9 . . ? C2 C3 H3 120.9 . . ? C3 C4 C5 119.7(2) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? C6 C5 C4 118.6(2) . . ? C6 C5 H5 120.7 . . ? C4 C5 H5 120.7 . . ? N1 C6 C5 121.7(2) . . ? N1 C6 C16 112.5(2) . . ? C5 C6 C16 125.8(2) . . ? O14 C12 O13 126.5(2) . . ? O14 C12 C2 117.0(2) . . ? O13 C12 C2 116.5(2) . . ? C12 O13 Cd1 130.16(16) . 2_565 ? C12 O13 Cd1 119.95(15) . . ? Cd1 O13 Cd1 109.86(7) 2_565 . ? O17 C16 N18 122.4(2) . . ? O17 C16 C6 119.7(2) . . ? N18 C16 C6 117.9(2) . . ? C16 O17 Cd1 118.96(16) . . ? C16 N18 C19 120.5(2) . . ? C16 N18 H18 119.8 . . ? C19 N18 H18 119.8 . . ? C33 C19 N18 112.9(12) . . ? C33 C19 C23 9.0(19) . . ? N18 C19 C23 112.4(12) . . ? C33 C19 H19A 116.3 . . ? N18 C19 H19A 109.1 . . ? C23 C19 H19A 109.1 . . ? C33 C19 H19B 101.0 . . ? N18 C19 H19B 109.1 . . ? C23 C19 H19B 109.1 . . ? H19A C19 H19B 107.9 . . ? C26 N21 C22 113(2) . . ? N21 C22 C23 126(2) . . ? N21 C22 H22 116.9 . . ? C23 C22 H22 116.9 . . ? C24 C23 C22 120(2) . . ? C24 C23 C19 121(2) . . ? C22 C23 C19 119(2) . . ? C23 C24 C25 118.0(13) . . ? C23 C24 H24 121.0 . . ? C25 C24 H24 121.0 . . ? C26 C25 C24 117.9(8) . . ? C26 C25 H25 121.1 . . ? C24 C25 H25 121.1 . . ? N21 C26 C25 124.5(14) . . ? N21 C26 H26 117.7 . . ? C25 C26 H26 117.7 . . ? C32 N31 C36 119(2) . . ? N31 C32 C33 123.1(18) . . ? N31 C32 H32 118.4 . . ? C33 C32 H32 118.4 . . ? C34 C33 C32 114(2) . . ? C34 C33 C19 127(2) . . ? C32 C33 C19 120(2) . . ? C35 C34 C33 122.5(14) . . ? C35 C34 H34 118.8 . . ? C33 C34 H34 118.8 . . ? C36 C35 C34 118.9(8) . . ? C36 C35 H35 120.6 . . ? C34 C35 H35 120.6 . . ? N31 C36 C35 123.0(18) . . ? N31 C36 H36 118.5 . . ? C35 C36 H36 118.5 . . ? Cd1 O40 Cd1 103.51(7) 2_665 . ? Cd1 O40 H40A 98.8 2_665 . ? Cd1 O40 H40A 103.1 . . ? Cd1 O40 H40B 111.4 2_665 . ? Cd1 O40 H40B 115.4 . . ? H40A O40 H40B 122.0 . . ? Cd1 O41 H41A 112.1 . . ? Cd1 O41 H41B 124.2 . . ? H41A O41 H41B 91.1 . . ? O43 N42 O44 124.1(3) . . ? O43 N42 O45 119.5(3) . . ? O44 N42 O45 116.4(3) . . ? H46A O46 H46B 106.0 . . ? 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 O41 Cd1 N1 C2 105.04(18) . . . . ? O40 Cd1 N1 C2 -89.21(18) 2_665 . . . ? O13 Cd1 N1 C2 5.1(2) 2_565 . . . ? O40 Cd1 N1 C2 -156.31(16) . . . . ? O13 Cd1 N1 C2 3.21(17) . . . . ? O17 Cd1 N1 C2 -178.6(2) . . . . ? O41 Cd1 N1 C6 -78.01(19) . . . . ? O40 Cd1 N1 C6 87.74(19) 2_665 . . . ? O13 Cd1 N1 C6 -177.98(16) 2_565 . . . ? O40 Cd1 N1 C6 20.6(2) . . . . ? O13 Cd1 N1 C6 -179.8(2) . . . . ? O17 Cd1 N1 C6 -1.65(17) . . . . ? C6 N1 C2 C3 0.3(4) . . . . ? Cd1 N1 C2 C3 177.25(19) . . . . ? C6 N1 C2 C12 179.8(2) . . . . ? Cd1 N1 C2 C12 -3.2(3) . . . . ? N1 C2 C3 C4 -0.5(4) . . . . ? C12 C2 C3 C4 179.9(2) . . . . ? C2 C3 C4 C5 0.1(4) . . . . ? C3 C4 C5 C6 0.5(4) . . . . ? C2 N1 C6 C5 0.4(4) . . . . ? Cd1 N1 C6 C5 -176.50(19) . . . . ? C2 N1 C6 C16 -178.4(2) . . . . ? Cd1 N1 C6 C16 4.7(3) . . . . ? C4 C5 C6 N1 -0.8(4) . . . . ? C4 C5 C6 C16 177.8(2) . . . . ? N1 C2 C12 O14 -179.5(2) . . . . ? C3 C2 C12 O14 0.1(4) . . . . ? N1 C2 C12 O13 0.3(3) . . . . ? C3 C2 C12 O13 179.9(2) . . . . ? O14 C12 O13 Cd1 0.2(4) . . . 2_565 ? C2 C12 O13 Cd1 -179.55(15) . . . 2_565 ? O14 C12 O13 Cd1 -177.6(2) . . . . ? C2 C12 O13 Cd1 2.7(3) . . . . ? O41 Cd1 O13 C12 -96.87(19) . . . . ? O40 Cd1 O13 C12 84.26(19) 2_665 . . . ? N1 Cd1 O13 C12 -3.11(18) . . . . ? O13 Cd1 O13 C12 178.2(2) 2_565 . . . ? O40 Cd1 O13 C12 150.46(17) . . . . ? O17 Cd1 O13 C12 -5.5(2) . . . . ? O41 Cd1 O13 Cd1 84.93(8) . . . 2_565 ? O40 Cd1 O13 Cd1 -93.94(8) 2_665 . . 2_565 ? N1 Cd1 O13 Cd1 178.69(10) . . . 2_565 ? O13 Cd1 O13 Cd1 0.0 2_565 . . 2_565 ? O40 Cd1 O13 Cd1 -27.74(15) . . . 2_565 ? O17 Cd1 O13 Cd1 176.31(7) . . . 2_565 ? N1 C6 C16 O17 -6.9(3) . . . . ? C5 C6 C16 O17 174.3(3) . . . . ? N1 C6 C16 N18 171.9(2) . . . . ? C5 C6 C16 N18 -6.9(4) . . . . ? N18 C16 O17 Cd1 -172.91(18) . . . . ? C6 C16 O17 Cd1 5.8(3) . . . . ? O41 Cd1 O17 C16 100.9(2) . . . . ? O40 Cd1 O17 C16 -90.95(19) 2_665 . . . ? N1 Cd1 O17 C16 -2.43(18) . . . . ? O13 Cd1 O17 C16 171.99(17) 2_565 . . . ? O40 Cd1 O17 C16 -167.3(2) . . . . ? O13 Cd1 O17 C16 0.0(2) . . . . ? O17 C16 N18 C19 1.7(4) . . . . ? C6 C16 N18 C19 -177.1(2) . . . . ? C16 N18 C19 C33 97.2(12) . . . . ? C16 N18 C19 C23 87.4(10) . . . . ? C26 N21 C22 C23 -4(4) . . . . ? N21 C22 C23 C24 6(4) . . . . ? N21 C22 C23 C19 -176(2) . . . . ? C33 C19 C23 C24 -132(17) . . . . ? N18 C19 C23 C24 -37(2) . . . . ? C33 C19 C23 C22 51(14) . . . . ? N18 C19 C23 C22 146(2) . . . . ? C22 C23 C24 C25 -4(3) . . . . ? C19 C23 C24 C25 178.9(13) . . . . ? C23 C24 C25 C26 -0.2(18) . . . . ? C22 N21 C26 C25 0(3) . . . . ? C24 C25 C26 N21 2(2) . . . . ? C36 N31 C32 C33 4(4) . . . . ? N31 C32 C33 C34 -3(4) . . . . ? N31 C32 C33 C19 178(2) . . . . ? N18 C19 C33 C34 -11(3) . . . . ? C23 C19 C33 C34 77(15) . . . . ? N18 C19 C33 C32 167.2(18) . . . . ? C23 C19 C33 C32 -104(16) . . . . ? C32 C33 C34 C35 2(3) . . . . ? C19 C33 C34 C35 -178.9(15) . . . . ? C33 C34 C35 C36 -2.4(17) . . . . ? C32 N31 C36 C35 -4(3) . . . . ? C34 C35 C36 N31 3(2) . . . . ? O41 Cd1 O40 Cd1 173.36(7) . . . 2_665 ? O40 Cd1 O40 Cd1 0.0 2_665 . . 2_665 ? N1 Cd1 O40 Cd1 71.25(11) . . . 2_665 ? O13 Cd1 O40 Cd1 -96.42(7) 2_565 . . 2_665 ? O13 Cd1 O40 Cd1 -70.16(13) . . . 2_665 ? O17 Cd1 O40 Cd1 92.58(8) . . . 2_665 ? _diffrn_measured_fraction_theta_max 0.889 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.130 _refine_diff_density_min -0.851 _refine_diff_density_rms 0.097 #######END data_compound_6 _database_code_depnum_ccdc_archive 'CCDC 823063' #TrackingRef '- AdelCS9_MAK1resub.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H9 Cu N3 O3' _chemical_formula_weight 318.77 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 15.507(3) _cell_length_b 7.0840(14) _cell_length_c 20.918(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2297.9(8) _cell_formula_units_Z 8 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 1979 _cell_measurement_theta_min 3.27 _cell_measurement_theta_max 24.99 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.843 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1288 _exptl_absorpt_coefficient_mu 1.912 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8172 _exptl_absorpt_correction_T_max 0.8939 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SADABS. See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'CCD area detector' _diffrn_measurement_method 'phi scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23066 _diffrn_reflns_av_R_equivalents 0.0537 _diffrn_reflns_av_sigmaI/netI 0.0231 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.27 _diffrn_reflns_theta_max 24.99 _reflns_number_total 1979 _reflns_number_gt 1920 _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 'XSeed (Barbour, 2001)' _computing_publication_material 'local program' _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^)+(0.0567P)^2^+4.5209P] 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 1979 _refine_ls_number_parameters 181 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0362 _refine_ls_R_factor_gt 0.0352 _refine_ls_wR_factor_ref 0.1003 _refine_ls_wR_factor_gt 0.0986 _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_restrained_S_all 1.105 _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 Cu1 Cu 0.439600(19) 0.12267(5) 0.337520(14) 0.01008(17) Uani 1 1 d . . . O1 O 0.47129(14) -0.1337(3) 0.16496(8) 0.0127(4) Uani 1 1 d . . . N2 N 0.47942(13) 0.0077(3) 0.60070(10) 0.0099(4) Uani 1 1 d . . . O3 O 0.19623(12) 0.2537(3) 0.39497(9) 0.0162(4) Uani 1 1 d . . . O4 O 0.49885(12) -0.0097(3) 0.26143(8) 0.0144(4) Uani 1 1 d . . . N6 N 0.34330(14) 0.0861(3) 0.28072(10) 0.0093(4) Uani 1 1 d . . . N7 N 0.34587(14) 0.2262(3) 0.39257(10) 0.0103(4) Uani 1 1 d . . . C9 C 0.42696(17) -0.0777(4) 0.55797(13) 0.0123(5) Uani 1 1 d . . . H9 H 0.4192 -0.2104 0.5609 0.015 Uiso 1 1 calc R . . C10 C 0.26505(17) 0.1210(3) 0.30346(12) 0.0093(5) Uani 1 1 d . . . C11 C 0.35660(16) 0.0067(4) 0.22384(11) 0.0100(5) Uani 1 1 d . . . C12 C 0.38401(17) 0.0192(4) 0.51022(12) 0.0127(5) Uani 1 1 d . . . H12 H 0.3480 -0.0462 0.4809 0.015 Uiso 1 1 calc R . . C13 C 0.39433(16) 0.2162(4) 0.50571(12) 0.0121(5) Uani 1 1 d . . . C14 C 0.20444(17) 0.0032(4) 0.20649(13) 0.0145(6) Uani 1 1 d . . . H14 H 0.1560 -0.0225 0.1801 0.017 Uiso 1 1 calc R . . C15 C 0.44438(16) 0.3044(4) 0.55231(13) 0.0144(6) Uani 1 1 d . . . H15 H 0.4498 0.4380 0.5527 0.017 Uiso 1 1 calc R . . C16 C 0.48591(17) 0.1974(4) 0.59784(12) 0.0125(5) Uani 1 1 d . . . H16 H 0.5207 0.2601 0.6286 0.015 Uiso 1 1 calc R . . C17 C 0.28754(17) -0.0322(4) 0.18381(12) 0.0125(5) Uani 1 1 d . . . H17 H 0.2965 -0.0816 0.1421 0.015 Uiso 1 1 calc R . . C18 C 0.35392(18) 0.3303(4) 0.45253(12) 0.0159(6) Uani 1 1 d . . . H18A H 0.2959 0.3723 0.4663 0.019 Uiso 1 1 calc R . . H18B H 0.3893 0.4445 0.4450 0.019 Uiso 1 1 calc R . . C19 C 0.26586(16) 0.2075(3) 0.36989(11) 0.0108(5) Uani 1 1 d . . . C20 C 0.45020(16) -0.0492(4) 0.21470(12) 0.0098(5) Uani 1 1 d . . . C23 C 0.19238(17) 0.0766(4) 0.26800(13) 0.0132(5) Uani 1 1 d . . . H23 H 0.1362 0.0952 0.2849 0.016 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0047(2) 0.0208(3) 0.0047(2) -0.00252(11) -0.00098(10) 0.00069(11) O1 0.0131(11) 0.0198(10) 0.0051(10) -0.0011(7) 0.0019(7) 0.0043(7) N2 0.0044(10) 0.0211(11) 0.0042(10) -0.0021(9) 0.0003(8) 0.0007(9) O3 0.0115(10) 0.0238(10) 0.0133(9) -0.0036(8) 0.0049(8) 0.0007(8) O4 0.0060(8) 0.0290(10) 0.0083(9) -0.0042(8) -0.0008(7) 0.0018(8) N6 0.0091(10) 0.0140(10) 0.0047(10) 0.0010(8) 0.0003(8) 0.0022(9) N7 0.0102(10) 0.0171(11) 0.0036(9) -0.0008(8) 0.0006(9) 0.0027(9) C9 0.0091(12) 0.0197(13) 0.0082(13) -0.0014(11) 0.0022(10) -0.0012(10) C10 0.0096(13) 0.0113(12) 0.0071(12) 0.0021(9) 0.0010(10) 0.0006(9) C11 0.0119(13) 0.0119(12) 0.0061(11) 0.0017(9) 0.0010(10) -0.0011(10) C12 0.0106(12) 0.0203(14) 0.0073(12) -0.0024(10) 0.0012(10) -0.0016(11) C13 0.0089(12) 0.0210(14) 0.0065(12) -0.0029(10) 0.0022(10) 0.0023(10) C14 0.0098(12) 0.0201(13) 0.0135(13) -0.0001(11) -0.0047(11) -0.0006(11) C15 0.0134(13) 0.0181(14) 0.0119(13) -0.0021(11) 0.0012(10) 0.0005(10) C16 0.0099(12) 0.0203(13) 0.0074(12) -0.0029(11) 0.0007(10) -0.0022(10) C17 0.0136(13) 0.0169(12) 0.0070(12) -0.0007(10) -0.0036(10) 0.0002(10) C18 0.0178(14) 0.0199(13) 0.0099(13) -0.0033(11) -0.0032(11) 0.0037(11) C19 0.0129(13) 0.0126(12) 0.0069(11) 0.0012(10) 0.0021(10) 0.0006(10) C20 0.0083(12) 0.0140(13) 0.0070(13) 0.0021(10) -0.0005(10) -0.0004(9) C23 0.0097(13) 0.0168(13) 0.0132(13) 0.0023(11) -0.0003(10) 0.0010(10) _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 Cu1 N6 1.926(2) . ? Cu1 N7 1.994(2) . ? Cu1 N2 2.025(2) 5_656 ? Cu1 O4 2.0633(18) . ? Cu1 O1 2.212(2) 4_655 ? O1 C20 1.244(3) . ? O1 Cu1 2.212(2) 4_645 ? N2 C16 1.349(4) . ? N2 C9 1.351(4) . ? N2 Cu1 2.025(2) 5_656 ? O3 C19 1.244(3) . ? O4 C20 1.266(3) . ? N6 C10 1.327(3) . ? N6 C11 1.332(3) . ? N7 C19 1.335(3) . ? N7 C18 1.460(3) . ? C9 C12 1.383(4) . ? C9 H9 0.9500 . ? C10 C23 1.385(4) . ? C10 C19 1.519(3) . ? C11 C17 1.387(4) . ? C11 C20 1.516(3) . ? C12 C13 1.408(4) . ? C12 H12 0.9500 . ? C13 C15 1.394(4) . ? C13 C18 1.511(4) . ? C14 C17 1.396(4) . ? C14 C23 1.400(4) . ? C14 H14 0.9500 . ? C15 C16 1.377(4) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C23 H23 0.9500 . ? 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 N6 Cu1 N7 80.83(9) . . ? N6 Cu1 N2 144.42(9) . 5_656 ? N7 Cu1 N2 104.55(9) . 5_656 ? N6 Cu1 O4 78.94(8) . . ? N7 Cu1 O4 159.59(8) . . ? N2 Cu1 O4 90.50(8) 5_656 . ? N6 Cu1 O1 125.10(8) . 4_655 ? N7 Cu1 O1 100.48(8) . 4_655 ? N2 Cu1 O1 89.06(8) 5_656 4_655 ? O4 Cu1 O1 93.35(7) . 4_655 ? C20 O1 Cu1 124.01(16) . 4_645 ? C16 N2 C9 117.5(2) . . ? C16 N2 Cu1 115.88(16) . 5_656 ? C9 N2 Cu1 126.23(19) . 5_656 ? C20 O4 Cu1 115.50(16) . . ? C10 N6 C11 122.7(2) . . ? C10 N6 Cu1 117.57(17) . . ? C11 N6 Cu1 119.20(17) . . ? C19 N7 C18 115.8(2) . . ? C19 N7 Cu1 115.84(16) . . ? C18 N7 Cu1 128.27(17) . . ? N2 C9 C12 123.0(3) . . ? N2 C9 H9 118.5 . . ? C12 C9 H9 118.5 . . ? N6 C10 C23 120.6(2) . . ? N6 C10 C19 113.3(2) . . ? C23 C10 C19 126.0(2) . . ? N6 C11 C17 120.2(2) . . ? N6 C11 C20 111.8(2) . . ? C17 C11 C20 127.7(2) . . ? C9 C12 C13 119.1(2) . . ? C9 C12 H12 120.5 . . ? C13 C12 H12 120.5 . . ? C15 C13 C12 117.4(2) . . ? C15 C13 C18 120.4(2) . . ? C12 C13 C18 122.2(2) . . ? C17 C14 C23 120.2(2) . . ? C17 C14 H14 119.9 . . ? C23 C14 H14 119.9 . . ? C16 C15 C13 119.8(3) . . ? C16 C15 H15 120.1 . . ? C13 C15 H15 120.1 . . ? N2 C16 C15 122.9(2) . . ? N2 C16 H16 118.5 . . ? C15 C16 H16 118.5 . . ? C11 C17 C14 118.1(2) . . ? C11 C17 H17 120.9 . . ? C14 C17 H17 120.9 . . ? N7 C18 C13 113.4(2) . . ? N7 C18 H18A 108.9 . . ? C13 C18 H18A 108.9 . . ? N7 C18 H18B 108.9 . . ? C13 C18 H18B 108.9 . . ? H18A C18 H18B 107.7 . . ? O3 C19 N7 129.1(2) . . ? O3 C19 C10 119.0(2) . . ? N7 C19 C10 111.9(2) . . ? O1 C20 O4 126.5(2) . . ? O1 C20 C11 118.9(2) . . ? O4 C20 C11 114.5(2) . . ? C10 C23 C14 117.9(2) . . ? C10 C23 H23 121.1 . . ? C14 C23 H23 121.1 . . ? 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 N6 Cu1 O4 C20 1.32(18) . . . . ? N7 Cu1 O4 C20 9.0(3) . . . . ? N2 Cu1 O4 C20 147.11(19) 5_656 . . . ? O1 Cu1 O4 C20 -123.81(19) 4_655 . . . ? N7 Cu1 N6 C10 -6.99(18) . . . . ? N2 Cu1 N6 C10 95.2(2) 5_656 . . . ? O4 Cu1 N6 C10 170.3(2) . . . . ? O1 Cu1 N6 C10 -103.40(19) 4_655 . . . ? N7 Cu1 N6 C11 -179.1(2) . . . . ? N2 Cu1 N6 C11 -76.9(2) 5_656 . . . ? O4 Cu1 N6 C11 -1.81(18) . . . . ? O1 Cu1 N6 C11 84.5(2) 4_655 . . . ? N6 Cu1 N7 C19 5.91(18) . . . . ? N2 Cu1 N7 C19 -138.10(18) 5_656 . . . ? O4 Cu1 N7 C19 -1.7(4) . . . . ? O1 Cu1 N7 C19 130.14(18) 4_655 . . . ? N6 Cu1 N7 C18 -169.8(2) . . . . ? N2 Cu1 N7 C18 46.2(2) 5_656 . . . ? O4 Cu1 N7 C18 -177.5(2) . . . . ? O1 Cu1 N7 C18 -45.6(2) 4_655 . . . ? C16 N2 C9 C12 3.4(4) . . . . ? Cu1 N2 C9 C12 -169.02(19) 5_656 . . . ? C11 N6 C10 C23 -0.5(4) . . . . ? Cu1 N6 C10 C23 -172.26(19) . . . . ? C11 N6 C10 C19 178.5(2) . . . . ? Cu1 N6 C10 C19 6.7(3) . . . . ? C10 N6 C11 C17 4.2(4) . . . . ? Cu1 N6 C11 C17 175.83(19) . . . . ? C10 N6 C11 C20 -169.7(2) . . . . ? Cu1 N6 C11 C20 1.9(3) . . . . ? N2 C9 C12 C13 -0.5(4) . . . . ? C9 C12 C13 C15 -3.3(4) . . . . ? C9 C12 C13 C18 176.2(2) . . . . ? C12 C13 C15 C16 4.2(4) . . . . ? C18 C13 C15 C16 -175.4(2) . . . . ? C9 N2 C16 C15 -2.5(4) . . . . ? Cu1 N2 C16 C15 170.7(2) 5_656 . . . ? C13 C15 C16 N2 -1.3(4) . . . . ? N6 C11 C17 C14 -3.9(4) . . . . ? C20 C11 C17 C14 168.9(2) . . . . ? C23 C14 C17 C11 0.2(4) . . . . ? C19 N7 C18 C13 120.6(2) . . . . ? Cu1 N7 C18 C13 -63.6(3) . . . . ? C15 C13 C18 N7 148.3(2) . . . . ? C12 C13 C18 N7 -31.2(3) . . . . ? C18 N7 C19 O3 -6.1(4) . . . . ? Cu1 N7 C19 O3 177.6(2) . . . . ? C18 N7 C19 C10 172.3(2) . . . . ? Cu1 N7 C19 C10 -3.9(3) . . . . ? N6 C10 C19 O3 177.0(2) . . . . ? C23 C10 C19 O3 -4.1(4) . . . . ? N6 C10 C19 N7 -1.6(3) . . . . ? C23 C10 C19 N7 177.3(2) . . . . ? Cu1 O1 C20 O4 39.4(4) 4_645 . . . ? Cu1 O1 C20 C11 -137.43(19) 4_645 . . . ? Cu1 O4 C20 O1 -177.6(2) . . . . ? Cu1 O4 C20 C11 -0.7(3) . . . . ? N6 C11 C20 O1 176.5(2) . . . . ? C17 C11 C20 O1 3.1(4) . . . . ? N6 C11 C20 O4 -0.7(3) . . . . ? C17 C11 C20 O4 -174.1(2) . . . . ? N6 C10 C23 C14 -3.2(4) . . . . ? C19 C10 C23 C14 177.9(2) . . . . ? C17 C14 C23 C10 3.3(4) . . . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.458 _refine_diff_density_min -0.838 _refine_diff_density_rms 0.096 #######END data_compound_7 _database_code_depnum_ccdc_archive 'CCDC 823064' #TrackingRef '- AdelCS9_MAK1resub.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H24 Cd N4 O10' _chemical_formula_weight 544.79 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' _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 8.109(6) _cell_length_b 11.029(9) _cell_length_c 13.128(10) _cell_angle_alpha 104.427(12) _cell_angle_beta 104.395(3) _cell_angle_gamma 104.536(11) _cell_volume 1038.3(14) _cell_formula_units_Z 2 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 2308 _cell_measurement_theta_min 3.0432 _cell_measurement_theta_max 27.4430 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.743 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 552 _exptl_absorpt_coefficient_mu 1.114 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6643 _exptl_absorpt_correction_T_max 0.8079 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SADABS. See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'Graphite Monochromator' _diffrn_radiation_detector CCD _diffrn_measurement_method 'phi and omega scans' _diffrn_measurement_device ; Saturn724 (4x4 bin mode) ; _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16110 _diffrn_reflns_av_R_equivalents 0.0266 _diffrn_reflns_av_sigmaI/netI 0.0287 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 27.49 _reflns_number_total 4645 _reflns_number_gt 4345 _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 'XSeed (Barbour, 2001)' _computing_publication_material 'local program' _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^)+(0.0531P)^2^+1.6719P] 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 4645 _refine_ls_number_parameters 294 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0370 _refine_ls_R_factor_gt 0.0346 _refine_ls_wR_factor_ref 0.0912 _refine_ls_wR_factor_gt 0.0900 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _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 0.10319(3) 0.696570(18) 0.060387(16) 0.01522(8) Uani 1 1 d . . . N1 N 0.3398(3) 0.7372(2) 0.2249(2) 0.0162(5) Uani 1 1 d . . . H30B H -0.003(5) 0.862(3) -0.063(3) 0.024 Uiso 1 1 d D . . H30A H -0.133(4) 0.753(3) -0.083(2) 0.024 Uiso 1 1 d D . . H31 H -0.061(5) 0.704(4) 0.2174(18) 0.024 Uiso 1 1 d D . . C2 C 0.3772(4) 0.6337(3) 0.2480(2) 0.0193(6) Uani 1 1 d . . . C3 C 0.5187(5) 0.6494(3) 0.3412(3) 0.0293(7) Uani 1 1 d . . . H3 H 0.5424 0.5744 0.3562 0.035 Uiso 1 1 calc R . . C4 C 0.6242(5) 0.7771(4) 0.4113(3) 0.0368(9) Uani 1 1 d . . . H4 H 0.7232 0.7908 0.4746 0.044 Uiso 1 1 calc R . . C5 C 0.5843(5) 0.8849(3) 0.3887(3) 0.0300(7) Uani 1 1 d . . . H5 H 0.6535 0.9729 0.4369 0.036 Uiso 1 1 calc R . . C6 C 0.4406(4) 0.8611(3) 0.2938(2) 0.0187(6) Uani 1 1 d . . . C12 C 0.2584(4) 0.4971(3) 0.1665(2) 0.0189(6) Uani 1 1 d . . . O13 O 0.2950(3) 0.4007(2) 0.1858(2) 0.0309(5) Uani 1 1 d . . . O14 O 0.1321(3) 0.49237(19) 0.08420(17) 0.0177(4) Uani 1 1 d . . . C16 C 0.3839(4) 0.9672(3) 0.2561(2) 0.0181(6) Uani 1 1 d . . . O17 O 0.2532(3) 0.9345(2) 0.17007(17) 0.0204(4) Uani 1 1 d . . . N18 N 0.4807(4) 1.0935(2) 0.3177(2) 0.0208(5) Uani 1 1 d . . . H18 H 0.5679 1.1108 0.3801 0.025 Uiso 1 1 calc R . . C19 C 0.4450(5) 1.2041(3) 0.2837(3) 0.0229(6) Uani 1 1 d . . . H19A H 0.4850 1.2839 0.3505 0.028 Uiso 1 1 calc R . . H19B H 0.3135 1.1809 0.2471 0.028 Uiso 1 1 calc R . . N21 N 0.7258(3) 1.2855(2) 0.0560(2) 0.0168(5) Uani 1 1 d . . . C22 C 0.7899(4) 1.3617(3) 0.1637(3) 0.0214(6) Uani 1 1 d . . . H22 H 0.8998 1.4339 0.1892 0.026 Uiso 1 1 calc R . . C23 C 0.7034(4) 1.3401(3) 0.2399(3) 0.0230(6) Uani 1 1 d . . . H23 H 0.7533 1.3966 0.3155 0.028 Uiso 1 1 calc R . . C24 C 0.5431(4) 1.2348(3) 0.2040(2) 0.0183(6) Uani 1 1 d . . . C25 C 0.4753(4) 1.1567(3) 0.0919(2) 0.0188(6) Uani 1 1 d . . . H25 H 0.3648 1.0847 0.0640 0.023 Uiso 1 1 calc R . . C26 C 0.5697(4) 1.1846(3) 0.0217(2) 0.0177(5) Uani 1 1 d . . . H26 H 0.5220 1.1299 -0.0544 0.021 Uiso 1 1 calc R . . O30 O -0.0508(3) 0.8144(2) -0.03001(18) 0.0207(4) Uani 1 1 d D . . O31 O -0.1008(3) 0.6999(3) 0.1534(2) 0.0301(5) Uani 1 1 d D . . C32 C -0.2928(5) 0.6537(4) 0.1077(3) 0.0300(7) Uani 1 1 d . . . H32A H -0.3294 0.6495 0.0296 0.045 Uiso 1 1 calc R . . H32B H -0.3403 0.7147 0.1501 0.045 Uiso 1 1 calc R . . H32C H -0.3409 0.5649 0.1121 0.045 Uiso 1 1 calc R . . N33 N 0.8965(5) 0.2409(4) 0.5754(3) 0.0493(9) Uani 1 1 d . . . O34 O 0.8137(9) 0.2371(4) 0.4858(4) 0.149(3) Uani 1 1 d . . . O35 O 0.8793(7) 0.1377(4) 0.5992(3) 0.0902(15) Uani 1 1 d . . . O36 O 1.0101(6) 0.3436(3) 0.6490(3) 0.0781(14) Uani 1 1 d . . . C40 C 0.9173(5) 0.0403(4) 0.2412(3) 0.0358(8) Uani 1 1 d . . . H40A H 1.0444 0.0544 0.2792 0.054 Uiso 1 1 calc R . . H40B H 0.8404 -0.0356 0.2527 0.054 Uiso 1 1 calc R . . H40C H 0.8887 0.1200 0.2717 0.054 Uiso 1 1 calc R . . O41 O 0.8860(3) 0.0143(2) 0.1244(2) 0.0290(5) Uani 1 1 d . . . H41 H 0.9302 -0.0438 0.1010 0.035 Uiso 1 1 calc R . . C42 C 0.8163(9) 0.5762(7) 0.5744(5) 0.0719(16) Uani 1 1 d . . . H42A H 0.9136 0.6076 0.5457 0.108 Uiso 1 1 calc R . . H42B H 0.8625 0.5459 0.6364 0.108 Uiso 1 1 calc R . . H42C H 0.7720 0.6489 0.6008 0.108 Uiso 1 1 calc R . . O43 O 0.6950(12) 0.4859(6) 0.5015(4) 0.140(3) Uani 1 1 d . . . H43 H 0.7017 0.4888 0.4392 0.168 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.01378(12) 0.01109(12) 0.02201(12) 0.00751(8) 0.00612(8) 0.00402(8) N1 0.0170(12) 0.0129(11) 0.0210(11) 0.0069(9) 0.0084(9) 0.0052(9) C2 0.0176(14) 0.0164(14) 0.0234(14) 0.0070(11) 0.0052(11) 0.0060(11) C3 0.0294(17) 0.0198(15) 0.0314(16) 0.0074(13) -0.0019(14) 0.0090(14) C4 0.036(2) 0.0261(18) 0.0340(18) 0.0045(14) -0.0066(15) 0.0097(16) C5 0.0323(19) 0.0161(15) 0.0285(16) 0.0021(12) -0.0012(14) 0.0028(14) C6 0.0189(14) 0.0151(13) 0.0204(13) 0.0053(11) 0.0064(11) 0.0037(11) C12 0.0160(14) 0.0146(13) 0.0261(14) 0.0073(11) 0.0055(11) 0.0062(11) O13 0.0297(13) 0.0154(11) 0.0378(13) 0.0081(9) -0.0062(10) 0.0094(10) O14 0.0148(10) 0.0127(9) 0.0237(10) 0.0076(8) 0.0022(8) 0.0037(8) C16 0.0221(15) 0.0128(13) 0.0228(13) 0.0074(11) 0.0129(12) 0.0049(11) O17 0.0200(11) 0.0148(10) 0.0257(10) 0.0073(8) 0.0062(8) 0.0056(8) N18 0.0279(14) 0.0128(12) 0.0205(11) 0.0056(9) 0.0097(10) 0.0030(10) C19 0.0312(17) 0.0119(13) 0.0314(15) 0.0084(12) 0.0177(13) 0.0082(12) N21 0.0150(12) 0.0136(11) 0.0231(11) 0.0085(9) 0.0070(9) 0.0039(9) C22 0.0197(15) 0.0145(14) 0.0265(14) 0.0059(11) 0.0075(12) 0.0009(12) C23 0.0269(16) 0.0168(14) 0.0230(14) 0.0049(11) 0.0095(12) 0.0041(12) C24 0.0218(15) 0.0116(13) 0.0269(14) 0.0095(11) 0.0117(12) 0.0080(11) C25 0.0156(14) 0.0151(13) 0.0264(14) 0.0081(11) 0.0069(11) 0.0051(11) C26 0.0165(13) 0.0135(13) 0.0226(13) 0.0064(10) 0.0051(11) 0.0052(11) O30 0.0199(11) 0.0138(10) 0.0264(11) 0.0084(8) 0.0029(9) 0.0054(8) O31 0.0218(12) 0.0447(15) 0.0260(11) 0.0114(11) 0.0121(10) 0.0111(11) C32 0.0208(16) 0.0321(18) 0.0451(19) 0.0187(15) 0.0164(14) 0.0109(14) N33 0.052(2) 0.043(2) 0.0331(17) -0.0052(15) -0.0074(15) 0.0212(18) O34 0.207(6) 0.054(3) 0.068(3) 0.013(2) -0.089(3) -0.010(3) O35 0.123(4) 0.056(2) 0.060(2) 0.0105(19) 0.000(2) 0.016(3) O36 0.094(3) 0.0421(19) 0.0358(16) 0.0086(14) -0.0276(17) -0.0292(19) C40 0.038(2) 0.034(2) 0.0360(18) 0.0076(15) 0.0167(16) 0.0127(17) O41 0.0354(13) 0.0201(11) 0.0325(12) 0.0058(9) 0.0123(10) 0.0124(10) C42 0.073(4) 0.090(4) 0.057(3) 0.018(3) 0.016(3) 0.046(4) O43 0.247(8) 0.119(5) 0.048(3) 0.025(3) 0.028(4) 0.075(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 O31 2.289(3) . ? Cd1 N21 2.315(3) 2_675 ? Cd1 O30 2.346(2) . ? Cd1 N1 2.361(3) . ? Cd1 O14 2.409(3) . ? Cd1 O14 2.412(2) 2_565 ? Cd1 O17 2.467(3) . ? N1 C2 1.337(4) . ? N1 C6 1.346(4) . ? C2 C3 1.393(4) . ? C2 C12 1.516(4) . ? C3 C4 1.386(5) . ? C3 H3 0.9500 . ? C4 C5 1.388(5) . ? C4 H4 0.9500 . ? C5 C6 1.393(5) . ? C5 H5 0.9500 . ? C6 C16 1.507(4) . ? C12 O13 1.240(4) . ? C12 O14 1.270(4) . ? O14 Cd1 2.412(2) 2_565 ? C16 O17 1.240(4) . ? C16 N18 1.336(4) . ? N18 C19 1.468(4) . ? N18 H18 0.8800 . ? C19 C24 1.515(4) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? N21 C22 1.342(4) . ? N21 C26 1.343(4) . ? N21 Cd1 2.315(3) 2_675 ? C22 C23 1.390(4) . ? C22 H22 0.9500 . ? C23 C24 1.388(4) . ? C23 H23 0.9500 . ? C24 C25 1.392(4) . ? C25 C26 1.380(4) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? O30 H30B 0.839(19) . ? O30 H30A 0.832(19) . ? O31 C32 1.424(4) . ? O31 H31 0.809(18) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? N33 O34 1.185(5) . ? N33 O35 1.238(6) . ? N33 O36 1.246(5) . ? C40 O41 1.431(4) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? O41 H41 0.8400 . ? C42 O43 1.201(8) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? O43 H43 0.8400 . ? 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 O31 Cd1 N21 167.59(9) . 2_675 ? O31 Cd1 O30 82.27(10) . . ? N21 Cd1 O30 85.37(9) 2_675 . ? O31 Cd1 N1 92.15(10) . . ? N21 Cd1 N1 97.93(10) 2_675 . ? O30 Cd1 N1 139.20(8) . . ? O31 Cd1 O14 93.00(9) . . ? N21 Cd1 O14 97.39(8) 2_675 . ? O30 Cd1 O14 151.66(7) . . ? N1 Cd1 O14 68.59(8) . . ? O31 Cd1 O14 86.22(10) . 2_565 ? N21 Cd1 O14 91.11(9) 2_675 2_565 ? O30 Cd1 O14 82.47(9) . 2_565 ? N1 Cd1 O14 137.72(8) . 2_565 ? O14 Cd1 O14 69.32(9) . 2_565 ? O31 Cd1 O17 86.63(9) . . ? N21 Cd1 O17 90.73(8) 2_675 . ? O30 Cd1 O17 72.66(9) . . ? N1 Cd1 O17 66.66(8) . . ? O14 Cd1 O17 135.20(8) . . ? O14 Cd1 O17 154.82(7) 2_565 . ? C2 N1 C6 119.4(3) . . ? C2 N1 Cd1 118.67(19) . . ? C6 N1 Cd1 121.89(19) . . ? N1 C2 C3 122.3(3) . . ? N1 C2 C12 116.5(3) . . ? C3 C2 C12 121.2(3) . . ? C4 C3 C2 118.3(3) . . ? C4 C3 H3 120.8 . . ? C2 C3 H3 120.8 . . ? C3 C4 C5 119.6(3) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? C4 C5 C6 118.6(3) . . ? C4 C5 H5 120.7 . . ? C6 C5 H5 120.7 . . ? N1 C6 C5 121.7(3) . . ? N1 C6 C16 113.3(3) . . ? C5 C6 C16 125.0(3) . . ? O13 C12 O14 126.2(3) . . ? O13 C12 C2 116.9(3) . . ? O14 C12 C2 116.9(3) . . ? C12 O14 Cd1 119.25(18) . . ? C12 O14 Cd1 130.06(19) . 2_565 ? Cd1 O14 Cd1 110.68(9) . 2_565 ? O17 C16 N18 123.3(3) . . ? O17 C16 C6 119.5(3) . . ? N18 C16 C6 117.3(3) . . ? C16 O17 Cd1 118.62(18) . . ? C16 N18 C19 121.5(3) . . ? C16 N18 H18 119.2 . . ? C19 N18 H18 119.2 . . ? N18 C19 C24 111.1(2) . . ? N18 C19 H19A 109.4 . . ? C24 C19 H19A 109.4 . . ? N18 C19 H19B 109.4 . . ? C24 C19 H19B 109.4 . . ? H19A C19 H19B 108.0 . . ? C22 N21 C26 117.3(3) . . ? C22 N21 Cd1 121.7(2) . 2_675 ? C26 N21 Cd1 120.24(19) . 2_675 ? N21 C22 C23 123.2(3) . . ? N21 C22 H22 118.4 . . ? C23 C22 H22 118.4 . . ? C24 C23 C22 119.1(3) . . ? C24 C23 H23 120.4 . . ? C22 C23 H23 120.4 . . ? C23 C24 C25 117.7(3) . . ? C23 C24 C19 121.6(3) . . ? C25 C24 C19 120.7(3) . . ? C26 C25 C24 119.6(3) . . ? C26 C25 H25 120.2 . . ? C24 C25 H25 120.2 . . ? N21 C26 C25 123.1(3) . . ? N21 C26 H26 118.5 . . ? C25 C26 H26 118.5 . . ? Cd1 O30 H30B 121(3) . . ? Cd1 O30 H30A 102(3) . . ? H30B O30 H30A 103(4) . . ? C32 O31 Cd1 128.2(2) . . ? C32 O31 H31 115(3) . . ? Cd1 O31 H31 113(3) . . ? O31 C32 H32A 109.5 . . ? O31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? O31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? O34 N33 O35 120.2(4) . . ? O34 N33 O36 124.2(5) . . ? O35 N33 O36 115.5(4) . . ? O41 C40 H40A 109.5 . . ? O41 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? O41 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C40 O41 H41 109.5 . . ? O43 C42 H42A 109.5 . . ? O43 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? O43 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C42 O43 H43 109.5 . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 2.226 _refine_diff_density_min -1.118 _refine_diff_density_rms 0.106 #######END data_compound_15 _database_code_depnum_ccdc_archive 'CCDC 823065' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H12 Cd N3 O6 S0.50' _chemical_formula_weight 434.69 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 11.5605(11) _cell_length_b 19.9973(12) _cell_length_c 19.0547(13) _cell_angle_alpha 90.00 _cell_angle_beta 103.352(9) _cell_angle_gamma 90.00 _cell_volume 4286.0(6) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7238 _cell_measurement_theta_min 2.5330 _cell_measurement_theta_max 29.7922 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.347 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1720 _exptl_absorpt_coefficient_mu 1.093 _exptl_absorpt_correction_T_min 0.53040 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 12.00 77.00 1.0000 60.0000 omega____ theta____ kappa____ phi______ frames - 23.2851 37.0000 -120.0000 65 #__ type_ start__ end____ width___ exp.time_ 2 omega 34.00 71.00 1.0000 60.0000 omega____ theta____ kappa____ phi______ frames - 23.2851 179.0000 90.0000 37 #__ type_ start__ end____ width___ exp.time_ 3 omega 34.00 102.00 1.0000 60.0000 omega____ theta____ kappa____ phi______ frames - 23.2851 179.0000 -180.0000 68 #__ type_ start__ end____ width___ exp.time_ 4 omega -9.00 73.00 1.0000 60.0000 omega____ theta____ kappa____ phi______ frames - 23.2851 37.0000 -30.0000 82 #__ type_ start__ end____ width___ exp.time_ 5 omega -10.00 96.00 1.0000 60.0000 omega____ theta____ kappa____ phi______ frames - 23.2851 77.0000 120.0000 106 #__ type_ start__ end____ width___ exp.time_ 6 omega 34.00 59.00 1.0000 60.0000 omega____ theta____ kappa____ phi______ frames - 23.2851 179.0000 -90.0000 25 #__ type_ start__ end____ width___ exp.time_ 7 omega -99.00 51.00 1.0000 60.0000 omega____ theta____ kappa____ phi______ frames - -23.7539 0.0000 -30.0000 150 ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.1695 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17934 _diffrn_reflns_av_R_equivalents 0.0984 _diffrn_reflns_av_sigmaI/netI 0.1194 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 29.86 _reflns_number_total 5550 _reflns_number_gt 3195 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 2003)' _computing_publication_material 'CIFTAB (Sheldrick)' _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^)+(0.0632P)^2^+202.9395P] 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 5550 _refine_ls_number_parameters 253 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1819 _refine_ls_R_factor_gt 0.1094 _refine_ls_wR_factor_ref 0.2909 _refine_ls_wR_factor_gt 0.2719 _refine_ls_goodness_of_fit_ref 1.183 _refine_ls_restrained_S_all 1.183 _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 0.40919(9) 0.40994(4) 0.15155(4) 0.0330(3) Uani 1 1 d . . . N1 N 0.5537(9) 0.4135(4) 0.0826(4) 0.027(2) Uani 1 1 d . . . S2 S 0.5000 0.55587(19) 0.2500 0.0358(11) Uani 1 2 d S . . C2 C 0.6679(11) 0.4121(6) 0.1167(6) 0.032(2) Uani 1 1 d . . . C3 C 0.7578(13) 0.4161(6) 0.0799(7) 0.043(3) Uani 1 1 d . . . H3 H 0.8388 0.4163 0.1054 0.051 Uiso 1 1 calc R . . C4 C 0.7280(14) 0.4199(7) 0.0054(7) 0.046(3) Uani 1 1 d . . . H4 H 0.7877 0.4219 -0.0215 0.056 Uiso 1 1 calc R . . C5 C 0.6075(12) 0.4207(6) -0.0293(6) 0.037(3) Uani 1 1 d . . . H5 H 0.5849 0.4235 -0.0804 0.044 Uiso 1 1 calc R . . C6 C 0.5220(11) 0.4175(5) 0.0092(5) 0.027(2) Uani 1 1 d . . . C12 C 0.6943(10) 0.4071(5) 0.1986(6) 0.028(2) Uani 1 1 d . . . O13 O 0.6075(8) 0.3960(4) 0.2253(4) 0.040(2) Uani 1 1 d . . . O14 O 0.7983(9) 0.4155(6) 0.2310(5) 0.053(3) Uani 1 1 d . . . C16 C 0.3917(10) 0.4153(5) -0.0207(5) 0.027(2) Uani 1 1 d . . . O17 O 0.3217(8) 0.4101(5) 0.0198(4) 0.040(2) Uani 1 1 d . . . N18 N 0.3526(10) 0.4200(4) -0.0917(5) 0.035(2) Uani 1 1 d . . . H18 H 0.4032 0.4280 -0.1188 0.042 Uiso 1 1 calc R . . C19 C 0.2266(13) 0.4121(6) -0.1254(6) 0.045(3) Uani 1 1 d . A . H19A H 0.2090 0.4331 -0.1738 0.054 Uiso 1 1 calc R . . H19B H 0.1786 0.4352 -0.0959 0.054 Uiso 1 1 calc R . . N21 N 0.1340(9) 0.2038(5) -0.1433(5) 0.032(2) Uani 1 1 d . . . O22 O 0.2150(14) 0.4414(8) 0.1331(6) 0.095(5) Uani 1 1 d . . . C22 C 0.094(3) 0.2431(10) -0.1002(18) 0.064(10) Uani 0.579(17) 1 d P A 1 H22 H 0.0439 0.2241 -0.0725 0.077 Uiso 0.579(17) 1 calc PR A 1 C22B C 0.060(3) 0.2534(15) -0.174(2) 0.064(13) Uani 0.421(17) 1 d PD A 2 H22B H -0.0198 0.2423 -0.1968 0.077 Uiso 0.421(17) 1 calc PR A 2 O23 O 0.4835(19) 0.5193(7) 0.1851(7) 0.041(6) Uani 0.56(2) 1 d P . 1 C23 C 0.119(3) 0.3102(11) -0.0917(17) 0.067(8) Uani 0.579(17) 1 d P A 1 H23 H 0.0873 0.3367 -0.0592 0.080 Uiso 0.579(17) 1 calc PR A 1 C23B C 0.095(4) 0.3180(14) -0.174(2) 0.067(8) Uani 0.421(17) 1 d PD A 2 H23B H 0.0460 0.3491 -0.2057 0.080 Uiso 0.421(17) 1 calc PR A 2 O24 O 0.4062(18) 0.5688(10) 0.2760(9) 0.057(6) Uani 0.56(2) 1 d P . 1 C24 C 0.1922(13) 0.3377(6) -0.1326(6) 0.041(3) Uani 1 1 d . . . O25 O 0.3982(16) 0.5187(7) 0.1898(8) 0.017(4) Uiso 0.44(2) 1 d P . 2 C25 C 0.235(5) 0.2990(16) -0.1743(19) 0.13(2) Uani 0.579(17) 1 d P A 1 H25 H 0.2882 0.3159 -0.2013 0.154 Uiso 0.579(17) 1 calc PR A 1 C25B C 0.278(3) 0.2867(12) -0.110(2) 0.057(11) Uani 0.421(17) 1 d PD A 2 H25B H 0.3589 0.2981 -0.0909 0.069 Uiso 0.421(17) 1 calc PR A 2 O26 O 0.5701(15) 0.6202(9) 0.2436(9) 0.026(5) Uiso 0.44(2) 1 d P . 2 C26 C 0.201(5) 0.2299(17) -0.179(2) 0.12(2) Uani 0.579(17) 1 d P A 1 H26 H 0.2316 0.2020 -0.2112 0.142 Uiso 0.579(17) 1 calc PR A 1 C26B C 0.243(3) 0.2216(12) -0.114(2) 0.059(12) Uani 0.421(17) 1 d PD A 2 H26B H 0.3006 0.1879 -0.0962 0.071 Uiso 0.421(17) 1 calc PR A 2 H22C H 0.1786 0.4308 0.1677 0.089 Uiso 1 1 d R . . H22D H 0.1839 0.4045 0.1218 0.089 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 0.0592(6) 0.0244(4) 0.0154(4) -0.0025(3) 0.0087(3) -0.0065(4) N1 0.051(6) 0.014(4) 0.016(4) 0.002(3) 0.007(4) 0.000(4) S2 0.073(3) 0.0190(18) 0.0217(18) 0.000 0.025(2) 0.000 C2 0.053(7) 0.021(5) 0.022(5) 0.003(4) 0.012(5) -0.001(6) C3 0.059(9) 0.037(7) 0.038(7) 0.004(6) 0.022(6) 0.011(6) C4 0.065(10) 0.049(8) 0.031(6) 0.004(6) 0.024(6) 0.020(7) C5 0.059(9) 0.036(7) 0.018(5) 0.005(4) 0.014(5) -0.006(6) C6 0.052(7) 0.010(4) 0.020(5) -0.001(4) 0.012(5) -0.007(4) C12 0.036(6) 0.021(5) 0.025(5) 0.005(4) 0.006(5) 0.002(5) O13 0.062(6) 0.040(5) 0.016(4) 0.004(3) 0.006(4) -0.017(4) O14 0.050(6) 0.075(7) 0.032(5) 0.009(5) 0.004(4) -0.003(6) C16 0.044(6) 0.019(5) 0.015(4) -0.002(4) 0.003(4) -0.016(5) O17 0.045(5) 0.053(5) 0.021(4) -0.003(4) 0.005(4) -0.028(5) N18 0.060(7) 0.024(5) 0.018(4) -0.003(4) 0.007(4) -0.019(5) C19 0.073(10) 0.031(6) 0.020(5) 0.006(5) -0.009(6) -0.021(7) N21 0.045(6) 0.029(5) 0.021(5) -0.007(4) 0.006(4) -0.007(4) O22 0.129(12) 0.123(12) 0.031(6) 0.000(7) 0.016(7) 0.065(10) C22 0.08(2) 0.012(9) 0.13(3) -0.005(12) 0.08(2) -0.013(11) C22B 0.06(2) 0.06(2) 0.05(2) 0.007(18) -0.044(19) -0.010(19) O23 0.089(16) 0.021(7) 0.017(7) -0.004(5) 0.019(8) 0.003(8) C23 0.11(2) 0.021(9) 0.089(18) -0.003(10) 0.063(17) -0.001(11) C23B 0.11(2) 0.021(9) 0.089(18) -0.003(10) 0.063(17) -0.001(11) O24 0.075(14) 0.065(13) 0.037(10) -0.017(9) 0.023(9) 0.001(10) C24 0.063(9) 0.029(6) 0.022(6) -0.002(5) -0.005(6) -0.025(6) C25 0.29(6) 0.060(19) 0.08(2) -0.053(18) 0.14(3) -0.10(3) C25B 0.04(2) 0.031(17) 0.09(3) -0.018(17) -0.008(19) 0.015(15) C26 0.24(6) 0.057(19) 0.10(3) -0.05(2) 0.12(4) -0.06(3) C26B 0.05(2) 0.019(14) 0.09(3) -0.002(17) -0.02(2) 0.017(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O22 2.280(14) . ? Cd1 O25 2.307(15) . ? Cd1 N21 2.326(9) 7 ? Cd1 N1 2.354(9) . ? Cd1 O23 2.382(15) . ? Cd1 O13 2.412(9) . ? Cd1 O13 2.414(8) 2_655 ? Cd1 O17 2.480(8) . ? N1 C2 1.330(15) . ? N1 C6 1.363(13) . ? S2 O24 1.318(19) 2_655 ? S2 O24 1.318(19) . ? S2 O23 1.411(13) 2_655 ? S2 O23 1.411(13) . ? S2 O26 1.539(17) 2_655 ? S2 O26 1.539(18) . ? S2 O25 1.621(16) 2_655 ? S2 O25 1.621(16) . ? C2 C3 1.384(17) . ? C2 C12 1.523(14) . ? C3 C4 1.384(17) . ? C3 H3 0.9500 . ? C4 C5 1.40(2) . ? C4 H4 0.9500 . ? C5 C6 1.361(16) . ? C5 H5 0.9500 . ? C6 C16 1.482(16) . ? C12 O14 1.230(14) . ? C12 O13 1.246(14) . ? O13 Cd1 2.414(8) 2_655 ? C16 O17 1.246(13) . ? C16 N18 1.327(13) . ? N18 C19 1.458(17) . ? N18 H18 0.8800 . ? C19 C24 1.539(16) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? N21 C26 1.26(3) . ? N21 C22 1.29(3) . ? N21 C26B 1.31(3) . ? N21 C22B 1.35(3) . ? N21 Cd1 2.326(9) 7 ? O22 H22C 0.8846 . ? O22 H22D 0.8281 . ? C22 C23 1.37(3) . ? C22 H22 0.9500 . ? C22B C23B 1.352(19) . ? C22B H22B 0.9500 . ? O23 O24 1.65(3) 2_655 ? C23 C24 1.39(3) . ? C23 H23 0.9500 . ? C23B C24 1.28(5) . ? C23B H23B 0.9500 . ? O24 O23 1.65(3) 2_655 ? C24 C25 1.29(3) . ? C24 C25B 1.42(3) . ? C25 C26 1.43(4) . ? C25 H25 0.9500 . ? C25B C26B 1.360(19) . ? C25B H25B 0.9500 . ? O26 O26 1.69(3) 2_655 ? C26 H26 0.9500 . ? C26B H26B 0.9500 . ? 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 O22 Cd1 O25 70.4(6) . . ? O22 Cd1 N21 94.1(5) . 7 ? O25 Cd1 N21 156.5(5) . 7 ? O22 Cd1 N1 135.0(4) . . ? O25 Cd1 N1 104.3(5) . . ? N21 Cd1 N1 99.2(3) 7 . ? O22 Cd1 O23 94.0(6) . . ? O25 Cd1 O23 24.8(5) . . ? N21 Cd1 O23 167.0(5) 7 . ? N1 Cd1 O23 82.2(5) . . ? O22 Cd1 O13 153.0(3) . . ? O25 Cd1 O13 92.3(5) . . ? N21 Cd1 O13 94.9(3) 7 . ? N1 Cd1 O13 68.1(3) . . ? O23 Cd1 O13 73.4(5) . . ? O22 Cd1 O13 83.4(4) . 2_655 ? O25 Cd1 O13 77.3(4) . 2_655 ? N21 Cd1 O13 83.6(3) 7 2_655 ? N1 Cd1 O13 140.6(3) . 2_655 ? O23 Cd1 O13 87.1(4) . 2_655 ? O13 Cd1 O13 72.5(4) . 2_655 ? O22 Cd1 O17 71.7(3) . . ? O25 Cd1 O17 106.2(4) . . ? N21 Cd1 O17 84.4(3) 7 . ? N1 Cd1 O17 67.1(3) . . ? O23 Cd1 O17 107.9(4) . . ? O13 Cd1 O17 134.5(3) . . ? O13 Cd1 O17 151.4(3) 2_655 . ? C2 N1 C6 120.3(10) . . ? C2 N1 Cd1 118.6(6) . . ? C6 N1 Cd1 121.1(8) . . ? O24 S2 O24 157.4(18) 2_655 . ? O24 S2 O23 118.3(12) 2_655 2_655 ? O24 S2 O23 74.2(12) . 2_655 ? O24 S2 O23 74.2(12) 2_655 . ? O24 S2 O23 118.3(12) . . ? O23 S2 O23 117.6(12) 2_655 . ? O24 S2 O26 111.1(12) 2_655 2_655 ? O24 S2 O26 46.6(10) . 2_655 ? O23 S2 O26 109.3(9) 2_655 2_655 ? O23 S2 O26 122.4(10) . 2_655 ? O24 S2 O26 46.6(10) 2_655 . ? O24 S2 O26 111.1(12) . . ? O23 S2 O26 122.4(10) 2_655 . ? O23 S2 O26 109.3(9) . . ? O26 S2 O26 66.7(13) 2_655 . ? O24 S2 O25 80.2(10) 2_655 2_655 ? O24 S2 O25 110.5(11) . 2_655 ? O23 S2 O25 38.2(8) 2_655 2_655 ? O23 S2 O25 108.2(8) . 2_655 ? O26 S2 O25 129.5(8) 2_655 2_655 ? O26 S2 O25 97.4(9) . 2_655 ? O24 S2 O25 110.5(11) 2_655 . ? O24 S2 O25 80.2(10) . . ? O23 S2 O25 108.2(8) 2_655 . ? O23 S2 O25 38.2(8) . . ? O26 S2 O25 97.4(9) 2_655 . ? O26 S2 O25 129.5(8) . . ? O25 S2 O25 125.5(11) 2_655 . ? N1 C2 C3 121.8(10) . . ? N1 C2 C12 116.4(10) . . ? C3 C2 C12 121.8(12) . . ? C4 C3 C2 119.0(14) . . ? C4 C3 H3 120.5 . . ? C2 C3 H3 120.5 . . ? C3 C4 C5 118.0(12) . . ? C3 C4 H4 121.0 . . ? C5 C4 H4 121.0 . . ? C6 C5 C4 120.9(11) . . ? C6 C5 H5 119.5 . . ? C4 C5 H5 119.5 . . ? C5 C6 N1 119.8(11) . . ? C5 C6 C16 126.4(10) . . ? N1 C6 C16 113.7(9) . . ? O14 C12 O13 127.3(11) . . ? O14 C12 C2 116.6(10) . . ? O13 C12 C2 116.1(10) . . ? C12 O13 Cd1 119.2(7) . . ? C12 O13 Cd1 129.0(7) . 2_655 ? Cd1 O13 Cd1 105.9(4) . 2_655 ? O17 C16 N18 121.3(11) . . ? O17 C16 C6 120.8(9) . . ? N18 C16 C6 117.8(10) . . ? C16 O17 Cd1 117.1(7) . . ? C16 N18 C19 120.8(10) . . ? C16 N18 H18 119.6 . . ? C19 N18 H18 119.6 . . ? N18 C19 C24 110.8(11) . . ? N18 C19 H19A 109.5 . . ? C24 C19 H19A 109.5 . . ? N18 C19 H19B 109.5 . . ? C24 C19 H19B 109.5 . . ? H19A C19 H19B 108.1 . . ? C26 N21 C22 116.6(17) . . ? C26 N21 C26B 57(3) . . ? C22 N21 C26B 91(2) . . ? C26 N21 C22B 82(3) . . ? C22 N21 C22B 63(2) . . ? C26B N21 C22B 116.0(18) . . ? C26 N21 Cd1 121.1(15) . 7 ? C22 N21 Cd1 122.3(11) . 7 ? C26B N21 Cd1 117.7(13) . 7 ? C22B N21 Cd1 125.7(13) . 7 ? Cd1 O22 H22C 116.0 . . ? Cd1 O22 H22D 98.4 . . ? H22C O22 H22D 74.2 . . ? N21 C22 C23 125(2) . . ? N21 C22 H22 117.5 . . ? C23 C22 H22 117.5 . . ? N21 C22B C23B 123(3) . . ? N21 C22B H22B 118.5 . . ? C23B C22B H22B 118.5 . . ? S2 O23 O24 50.3(8) . 2_655 ? S2 O23 Cd1 132.7(9) . . ? O24 O23 Cd1 149.9(12) 2_655 . ? C22 C23 C24 117(2) . . ? C22 C23 H23 121.4 . . ? C24 C23 H23 121.4 . . ? C24 C23B C22B 121(4) . . ? C24 C23B H23B 119.7 . . ? C22B C23B H23B 119.7 . . ? S2 O24 O23 55.5(9) . 2_655 ? C23B C24 C25 81(3) . . ? C23B C24 C23 70(2) . . ? C25 C24 C23 118.7(17) . . ? C23B C24 C25B 115(2) . . ? C25 C24 C25B 54(3) . . ? C23 C24 C25B 91(2) . . ? C23B C24 C19 121.6(18) . . ? C25 C24 C19 120.5(16) . . ? C23 C24 C19 120.7(15) . . ? C25B C24 C19 121.3(16) . . ? S2 O25 Cd1 124.8(9) . . ? C24 C25 C26 119(3) . . ? C24 C25 H25 120.6 . . ? C26 C25 H25 120.6 . . ? C26B C25B C24 120(3) . . ? C26B C25B H25B 120.2 . . ? C24 C25B H25B 120.2 . . ? S2 O26 O26 56.6(7) . 2_655 ? N21 C26 C25 124(3) . . ? N21 C26 H26 118.1 . . ? C25 C26 H26 118.1 . . ? N21 C26B C25B 122(3) . . ? N21 C26B H26B 119.1 . . ? C25B C26B H26B 119.1 . . ? 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 O22 Cd1 N1 C2 157.4(9) . . . . ? O25 Cd1 N1 C2 81.1(9) . . . . ? N21 Cd1 N1 C2 -97.2(8) 7 . . . ? O23 Cd1 N1 C2 69.7(9) . . . . ? O13 Cd1 N1 C2 -5.6(7) . . . . ? O13 Cd1 N1 C2 -6.1(10) 2_655 . . . ? O17 Cd1 N1 C2 -177.1(9) . . . . ? O22 Cd1 N1 C6 -21.9(10) . . . . ? O25 Cd1 N1 C6 -98.3(8) . . . . ? N21 Cd1 N1 C6 83.4(8) 7 . . . ? O23 Cd1 N1 C6 -109.7(8) . . . . ? O13 Cd1 N1 C6 175.1(8) . . . . ? O13 Cd1 N1 C6 174.5(6) 2_655 . . . ? O17 Cd1 N1 C6 3.6(7) . . . . ? C6 N1 C2 C3 1.4(16) . . . . ? Cd1 N1 C2 C3 -177.9(9) . . . . ? C6 N1 C2 C12 -179.7(9) . . . . ? Cd1 N1 C2 C12 1.0(12) . . . . ? N1 C2 C3 C4 -1.7(19) . . . . ? C12 C2 C3 C4 179.4(11) . . . . ? C2 C3 C4 C5 1.2(19) . . . . ? C3 C4 C5 C6 -0.3(19) . . . . ? C4 C5 C6 N1 0.0(17) . . . . ? C4 C5 C6 C16 -177.5(11) . . . . ? C2 N1 C6 C5 -0.6(15) . . . . ? Cd1 N1 C6 C5 178.8(8) . . . . ? C2 N1 C6 C16 177.2(9) . . . . ? Cd1 N1 C6 C16 -3.4(11) . . . . ? N1 C2 C12 O14 -169.8(11) . . . . ? C3 C2 C12 O14 9.1(17) . . . . ? N1 C2 C12 O13 9.2(15) . . . . ? C3 C2 C12 O13 -172.0(11) . . . . ? O14 C12 O13 Cd1 164.3(10) . . . . ? C2 C12 O13 Cd1 -14.6(13) . . . . ? O14 C12 O13 Cd1 15.3(18) . . . 2_655 ? C2 C12 O13 Cd1 -163.5(7) . . . 2_655 ? O22 Cd1 O13 C12 -141.6(12) . . . . ? O25 Cd1 O13 C12 -93.3(9) . . . . ? N21 Cd1 O13 C12 109.2(8) 7 . . . ? N1 Cd1 O13 C12 11.2(8) . . . . ? O23 Cd1 O13 C12 -76.9(9) . . . . ? O13 Cd1 O13 C12 -169.1(7) 2_655 . . . ? O17 Cd1 O13 C12 22.2(10) . . . . ? O22 Cd1 O13 Cd1 13.7(11) . . . 2_655 ? O25 Cd1 O13 Cd1 62.1(5) . . . 2_655 ? N21 Cd1 O13 Cd1 -95.5(3) 7 . . 2_655 ? N1 Cd1 O13 Cd1 166.6(4) . . . 2_655 ? O23 Cd1 O13 Cd1 78.5(5) . . . 2_655 ? O13 Cd1 O13 Cd1 -13.8(4) 2_655 . . 2_655 ? O17 Cd1 O13 Cd1 177.6(3) . . . 2_655 ? C5 C6 C16 O17 177.6(11) . . . . ? N1 C6 C16 O17 -0.1(14) . . . . ? C5 C6 C16 N18 -3.4(16) . . . . ? N1 C6 C16 N18 178.9(9) . . . . ? N18 C16 O17 Cd1 -175.8(7) . . . . ? C6 C16 O17 Cd1 3.2(13) . . . . ? O22 Cd1 O17 C16 157.8(10) . . . . ? O25 Cd1 O17 C16 95.5(10) . . . . ? N21 Cd1 O17 C16 -106.0(9) 7 . . . ? N1 Cd1 O17 C16 -3.5(8) . . . . ? O23 Cd1 O17 C16 69.6(10) . . . . ? O13 Cd1 O17 C16 -14.5(10) . . . . ? O13 Cd1 O17 C16 -171.5(7) 2_655 . . . ? O17 C16 N18 C19 -6.6(16) . . . . ? C6 C16 N18 C19 174.4(10) . . . . ? C16 N18 C19 C24 -80.0(14) . . . . ? C26 N21 C22 C23 1(5) . . . . ? C26B N21 C22 C23 54(4) . . . . ? C22B N21 C22 C23 -65(4) . . . . ? Cd1 N21 C22 C23 178(3) 7 . . . ? C26 N21 C22B C23B -49(4) . . . . ? C22 N21 C22B C23B 76(4) . . . . ? C26B N21 C22B C23B -2(6) . . . . ? Cd1 N21 C22B C23B -172(3) 7 . . . ? O24 S2 O23 O24 159.7(17) . . . 2_655 ? O23 S2 O23 O24 -114.1(11) 2_655 . . 2_655 ? O26 S2 O23 O24 105.3(13) 2_655 . . 2_655 ? O26 S2 O23 O24 31.2(11) . . . 2_655 ? O25 S2 O23 O24 -73.8(10) 2_655 . . 2_655 ? O25 S2 O23 O24 161.3(15) . . . 2_655 ? O24 S2 O23 Cd1 139.8(18) 2_655 . . . ? O24 S2 O23 Cd1 -60.5(19) . . . . ? O23 S2 O23 Cd1 25.7(9) 2_655 . . . ? O26 S2 O23 Cd1 -114.9(14) 2_655 . . . ? O26 S2 O23 Cd1 171.0(13) . . . . ? O25 S2 O23 Cd1 66.0(15) 2_655 . . . ? O25 S2 O23 Cd1 -58.8(15) . . . . ? O22 Cd1 O23 S2 80.1(16) . . . . ? O25 Cd1 O23 S2 62.2(15) . . . . ? N21 Cd1 O23 S2 -48(3) 7 . . . ? N1 Cd1 O23 S2 -145.0(16) . . . . ? O13 Cd1 O23 S2 -75.6(15) . . . . ? O13 Cd1 O23 S2 -3.1(16) 2_655 . . . ? O17 Cd1 O23 S2 152.2(14) . . . . ? O22 Cd1 O23 O24 162.0(19) . . . 2_655 ? O25 Cd1 O23 O24 144(3) . . . 2_655 ? N21 Cd1 O23 O24 34(4) 7 . . 2_655 ? N1 Cd1 O23 O24 -63.2(19) . . . 2_655 ? O13 Cd1 O23 O24 6.3(18) . . . 2_655 ? O13 Cd1 O23 O24 78.8(19) 2_655 . . 2_655 ? O17 Cd1 O23 O24 -126.0(18) . . . 2_655 ? N21 C22 C23 C24 0(5) . . . . ? N21 C22B C23B C24 -14(6) . . . . ? O24 S2 O24 O23 -127.3(7) 2_655 . . 2_655 ? O23 S2 O24 O23 113.2(14) . . . 2_655 ? O26 S2 O24 O23 -137.7(14) 2_655 . . 2_655 ? O26 S2 O24 O23 -119.1(10) . . . 2_655 ? O25 S2 O24 O23 -12.2(10) 2_655 . . 2_655 ? O25 S2 O24 O23 112.2(9) . . . 2_655 ? C22B C23B C24 C25 67(4) . . . . ? C22B C23B C24 C23 -58(4) . . . . ? C22B C23B C24 C25B 23(5) . . . . ? C22B C23B C24 C19 -173(3) . . . . ? C22 C23 C24 C23B 65(3) . . . . ? C22 C23 C24 C25 -2(5) . . . . ? C22 C23 C24 C25B -51(3) . . . . ? C22 C23 C24 C19 -179(2) . . . . ? N18 C19 C24 C23B -164(2) . . . . ? N18 C19 C24 C25 -66(3) . . . . ? N18 C19 C24 C23 111(2) . . . . ? N18 C19 C24 C25B -1(3) . . . . ? O24 S2 O25 Cd1 71.5(13) 2_655 . . . ? O24 S2 O25 Cd1 -129.2(14) . . . . ? O23 S2 O25 Cd1 -59.5(11) 2_655 . . . ? O23 S2 O25 Cd1 52.3(12) . . . . ? O26 S2 O25 Cd1 -172.7(11) 2_655 . . . ? O26 S2 O25 Cd1 121.5(11) . . . . ? O25 S2 O25 Cd1 -21.0(6) 2_655 . . . ? O22 Cd1 O25 S2 155.4(12) . . . . ? N21 Cd1 O25 S2 104.4(14) 7 . . . ? N1 Cd1 O25 S2 -71.5(10) . . . . ? O23 Cd1 O25 S2 -43.6(11) . . . . ? O13 Cd1 O25 S2 -3.5(10) . . . . ? O13 Cd1 O25 S2 67.9(10) 2_655 . . . ? O17 Cd1 O25 S2 -141.4(9) . . . . ? C23B C24 C25 C26 -59(5) . . . . ? C23 C24 C25 C26 3(7) . . . . ? C25B C24 C25 C26 71(5) . . . . ? C19 C24 C25 C26 180(4) . . . . ? C23B C24 C25B C26B -18(5) . . . . ? C25 C24 C25B C26B -75(4) . . . . ? C23 C24 C25B C26B 50(4) . . . . ? C19 C24 C25B C26B 178(3) . . . . ? O24 S2 O26 O26 161.1(19) 2_655 . . 2_655 ? O24 S2 O26 O26 -14.6(15) . . . 2_655 ? O23 S2 O26 O26 -98.8(13) 2_655 . . 2_655 ? O23 S2 O26 O26 117.8(12) . . . 2_655 ? O25 S2 O26 O26 -129.9(11) 2_655 . . 2_655 ? O25 S2 O26 O26 80.1(14) . . . 2_655 ? C22 N21 C26 C25 0(7) . . . . ? C26B N21 C26 C25 -73(5) . . . . ? C22B N21 C26 C25 55(5) . . . . ? Cd1 N21 C26 C25 -177(4) 7 . . . ? C24 C25 C26 N21 -2(9) . . . . ? C26 N21 C26B C25B 67(4) . . . . ? C22 N21 C26B C25B -54(5) . . . . ? C22B N21 C26B C25B 6(6) . . . . ? Cd1 N21 C26B C25B 178(3) 7 . . . ? C24 C25B C26B N21 4(7) . . . . ? _diffrn_measured_fraction_theta_max 0.899 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.449 _refine_diff_density_min -1.173 _refine_diff_density_rms 0.208 ######END data_compound_16 _database_code_depnum_ccdc_archive 'CCDC 823066' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H48 Cd3 N15 O22.50' _chemical_formula_weight 1604.27 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 monoclinic _symmetry_space_group_name_H-M P2(1)/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 10.403(2) _cell_length_b 33.827(7) _cell_length_c 19.688(4) _cell_angle_alpha 90.00 _cell_angle_beta 92.82(3) _cell_angle_gamma 90.00 _cell_volume 6920(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 13532 _cell_measurement_theta_min 1.59 _cell_measurement_theta_max 26.00 _exptl_crystal_description rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.540 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3204 _exptl_absorpt_coefficient_mu 0.995 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.953 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SADABS. See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _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 'CCD area detector' _diffrn_measurement_method 'phi scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 93958 _diffrn_reflns_av_R_equivalents 0.0721 _diffrn_reflns_av_sigmaI/netI 0.0359 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -41 _diffrn_reflns_limit_k_max 41 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 26.00 _reflns_number_total 13532 _reflns_number_gt 12000 _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 'XSeed (Barbour, 2001)' _computing_publication_material 'local program' _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^)+(0.1197P)^2^+29.2166P] 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 13532 _refine_ls_number_parameters 872 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0733 _refine_ls_R_factor_gt 0.0676 _refine_ls_wR_factor_ref 0.2042 _refine_ls_wR_factor_gt 0.1995 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.005 _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 0.37807(4) 0.175096(12) 0.85574(2) 0.03745(14) Uani 1 1 d . . . N1A N 0.4164(4) 0.12028(14) 0.7871(2) 0.0348(10) Uani 1 1 d . . . N1B N 0.3073(5) 0.08060(14) 1.1438(2) 0.0365(10) Uani 1 1 d . . . N1C N 0.2822(4) 0.28309(15) 1.0175(3) 0.0426(12) Uani 1 1 d . . . N1D N 1.0338(6) 0.1381(2) 1.3167(3) 0.0599(15) Uani 1 1 d . . . Cd2 Cd 0.33763(4) 0.083551(13) 1.02605(2) 0.03667(14) Uani 1 1 d . . . C2A C 0.4170(5) 0.08441(17) 0.8150(3) 0.0368(12) Uani 1 1 d . . . C2B C 0.3158(5) 0.11403(19) 1.1792(3) 0.0391(12) Uani 1 1 d . . . C2C C 0.2856(6) 0.28390(18) 0.9499(4) 0.0453(14) Uani 1 1 d . . . C2D C 1.0713(8) 0.1573(3) 1.3734(4) 0.066(2) Uani 1 1 d . . . Cd3 Cd 0.31881(4) 0.223098(13) 1.07318(3) 0.04363(15) Uani 1 1 d . . . C3A C 0.4368(6) 0.0509(2) 0.7768(3) 0.0474(14) Uani 1 1 d . . . H3A H 0.4365 0.0254 0.7972 0.057 Uiso 1 1 calc R . . C3B C 0.3159(6) 0.1142(2) 1.2500(3) 0.0493(15) Uani 1 1 d . . . H3B H 0.3239 0.1383 1.2745 0.059 Uiso 1 1 calc R . . C3C C 0.2623(7) 0.3180(2) 0.9121(4) 0.0573(18) Uani 1 1 d . . . H3C H 0.2663 0.3182 0.8640 0.069 Uiso 1 1 calc R . . C3D C 1.1110(9) 0.1975(3) 1.3731(5) 0.077(2) Uani 1 1 d . . . H3D H 1.1361 0.2108 1.4141 0.093 Uiso 1 1 calc R . . C4A C 0.4572(8) 0.0551(2) 0.7082(4) 0.0561(17) Uani 1 1 d . . . H4A H 0.4715 0.0325 0.6809 0.067 Uiso 1 1 calc R . . C4B C 0.3044(8) 0.0792(2) 1.2833(4) 0.0582(18) Uani 1 1 d . . . H4B H 0.3027 0.0788 1.3314 0.070 Uiso 1 1 calc R . . C4C C 0.2332(9) 0.3517(2) 0.9478(5) 0.069(2) Uani 1 1 d . . . H4C H 0.2155 0.3756 0.9238 0.083 Uiso 1 1 calc R . . C4D C 1.1119(10) 0.2163(3) 1.3118(6) 0.084(3) Uani 1 1 d . . . H4D H 1.1382 0.2432 1.3097 0.101 Uiso 1 1 calc R . . C5A C 0.4566(7) 0.0928(2) 0.6796(3) 0.0508(15) Uani 1 1 d . . . H5A H 0.4707 0.0964 0.6327 0.061 Uiso 1 1 calc R . . C5B C 0.2953(8) 0.0442(2) 1.2466(3) 0.0560(17) Uani 1 1 d . . . H5B H 0.2878 0.0195 1.2691 0.067 Uiso 1 1 calc R . . C5C C 0.2294(8) 0.3512(2) 1.0178(5) 0.063(2) Uani 1 1 d . . . H5C H 0.2097 0.3745 1.0422 0.076 Uiso 1 1 calc R . . C5D C 1.0758(9) 0.1971(3) 1.2546(5) 0.073(2) Uani 1 1 d . . . H5D H 1.0768 0.2099 1.2117 0.088 Uiso 1 1 calc R . . C6A C 0.4350(5) 0.12452(18) 0.7211(3) 0.0373(12) Uani 1 1 d . . . C6B C 0.2973(6) 0.04604(19) 1.1756(3) 0.0418(13) Uani 1 1 d . . . C6C C 0.2547(6) 0.31614(19) 1.0518(4) 0.0490(16) Uani 1 1 d . . . C6D C 1.0377(6) 0.1587(3) 1.2595(4) 0.062(2) Uani 1 1 d . . . C12A C 0.3915(5) 0.08350(18) 0.8898(3) 0.0363(12) Uani 1 1 d . . . C12B C 0.3240(5) 0.15097(19) 1.1376(3) 0.0414(13) Uani 1 1 d . . . C12C C 0.3172(6) 0.24520(19) 0.9167(4) 0.0450(14) Uani 1 1 d . . . C12D C 1.0654(11) 0.1338(4) 1.4353(6) 0.093(3) Uani 1 1 d . . . O13A O 0.3659(4) 0.11547(12) 0.9188(2) 0.0391(9) Uani 1 1 d . . . O13B O 0.3285(4) 0.14807(13) 1.0739(2) 0.0413(9) Uani 1 1 d . . . O13C O 0.3291(4) 0.21494(13) 0.9545(2) 0.0467(10) Uani 1 1 d . . . O13D O 1.0527(12) 0.0987(4) 1.4375(5) 0.134(4) Uani 1 1 d . . . O14A O 0.3952(4) 0.05059(13) 0.9197(2) 0.0443(10) Uani 1 1 d . . . O14B O 0.3248(5) 0.18320(14) 1.1685(3) 0.0503(11) Uani 1 1 d . . . O14C O 0.3279(4) 0.24425(14) 0.8540(3) 0.0495(11) Uani 1 1 d . . . O14D O 1.0785(7) 0.1556(3) 1.4918(3) 0.109(3) Uani 1 1 d . . . C15D C 1.0780(14) 0.1333(7) 1.5547(7) 0.163(8) Uani 1 1 d . . . H15A H 1.0028 0.1158 1.5537 0.244 Uiso 1 1 calc R . . H15B H 1.0742 0.1516 1.5931 0.244 Uiso 1 1 calc R . . H15C H 1.1567 0.1174 1.5597 0.244 Uiso 1 1 calc R . . C16A C 0.4313(5) 0.1678(2) 0.7003(3) 0.0393(13) Uani 1 1 d . . . C16B C 0.2900(6) 0.01113(18) 1.1285(3) 0.0396(13) Uani 1 1 d . . . C16C C 0.2601(5) 0.31039(19) 1.1274(4) 0.0483(16) Uani 1 1 d . . . C16D C 1.0029(7) 0.1337(4) 1.1943(4) 0.076(3) Uani 1 1 d . . . O17A O 0.4348(5) 0.19384(14) 0.7446(2) 0.0469(10) Uani 1 1 d . . . O17B O 0.3103(4) 0.01565(13) 1.0675(2) 0.0436(10) Uani 1 1 d . . . O17C O 0.2694(5) 0.27664(14) 1.1517(3) 0.0536(12) Uani 1 1 d . . . O17D O 1.0207(6) 0.1480(2) 1.1376(4) 0.089(2) Uani 1 1 d . . . N18A N 0.4252(5) 0.17684(17) 0.6345(3) 0.0419(11) Uani 1 1 d . . . H18A H 0.4218 0.1579 0.6038 0.050 Uiso 1 1 calc R . . N18B N 0.2602(5) -0.02334(16) 1.1548(3) 0.0464(12) Uani 1 1 d . . . H18B H 0.2476 -0.0249 1.1986 0.056 Uiso 1 1 calc R . . N18C N 0.2553(5) 0.34234(17) 1.1662(3) 0.0502(14) Uani 1 1 d . . . H18C H 0.2475 0.3658 1.1471 0.060 Uiso 1 1 calc R . . N18D N 0.9616(7) 0.0985(3) 1.2040(5) 0.078(2) Uani 1 1 d . . . H18D H 0.9495 0.0909 1.2459 0.093 Uiso 1 1 calc R . . C19A C 0.4243(6) 0.2182(2) 0.6131(3) 0.0493(15) Uani 1 1 d . . . H19A H 0.4645 0.2204 0.5688 0.059 Uiso 1 1 calc R . . H19B H 0.4766 0.2340 0.6467 0.059 Uiso 1 1 calc R . . C19B C 0.2477(6) -0.0591(2) 1.1132(4) 0.0484(15) Uani 1 1 d . . . H19C H 0.2690 -0.0823 1.1421 0.058 Uiso 1 1 calc R . . H19D H 0.3108 -0.0579 1.0772 0.058 Uiso 1 1 calc R . . C19C C 0.2628(6) 0.3390(2) 1.2400(4) 0.0542(17) Uani 1 1 d . . . H19E H 0.2148 0.3153 1.2537 0.065 Uiso 1 1 calc R . . H19F H 0.2219 0.3625 1.2599 0.065 Uiso 1 1 calc R . . C19D C 0.9333(9) 0.0702(3) 1.1475(7) 0.096(4) Uani 1 1 d . . . H19G H 0.9453 0.0430 1.1653 0.115 Uiso 1 1 calc R . . H19H H 0.9965 0.0743 1.1122 0.115 Uiso 1 1 calc R . . N21A N 0.0374(5) 0.26404(16) 0.5909(3) 0.0454(12) Uani 1 1 d . . . N21B N -0.1298(5) -0.07596(17) 1.0171(3) 0.0468(12) Uani 1 1 d . . . N21C N 0.6572(5) 0.33082(16) 1.3178(3) 0.0466(12) Uani 1 1 d . . . N21D N 0.5538(5) 0.08072(17) 1.0552(3) 0.0456(12) Uani 1 1 d . . . C22A C 0.0958(10) 0.2597(4) 0.6507(5) 0.098(4) Uani 1 1 d . . . H22A H 0.0502 0.2667 0.6895 0.118 Uiso 1 1 calc R . . C22B C -0.0454(10) -0.1053(3) 1.0238(7) 0.102(4) Uani 1 1 d . . . H22B H -0.0688 -0.1306 1.0060 0.123 Uiso 1 1 calc R . . C22C C 0.5761(9) 0.2998(3) 1.3147(6) 0.083(3) Uani 1 1 d . . . H22C H 0.6082 0.2750 1.3306 0.099 Uiso 1 1 calc R . . C22D C 0.6231(7) 0.1128(3) 1.0626(6) 0.079(3) Uani 1 1 d . . . H22D H 0.5888 0.1375 1.0471 0.095 Uiso 1 1 calc R . . C23A C 0.2199(10) 0.2455(4) 0.6610(5) 0.096(4) Uani 1 1 d . . . H23A H 0.2566 0.2428 0.7060 0.115 Uiso 1 1 calc R . . C23B C 0.0752(9) -0.1007(3) 1.0556(6) 0.098(4) Uani 1 1 d . . . H23B H 0.1313 -0.1228 1.0605 0.117 Uiso 1 1 calc R . . C23C C 0.4478(8) 0.3015(3) 1.2898(6) 0.078(3) Uani 1 1 d . . . H23C H 0.3954 0.2785 1.2888 0.094 Uiso 1 1 calc R . . C23D C 0.7474(9) 0.1112(4) 1.0931(8) 0.107(4) Uani 1 1 d . . . H23D H 0.7974 0.1345 1.0996 0.128 Uiso 1 1 calc R . . C24A C 0.2899(6) 0.2352(2) 0.6067(3) 0.0440(14) Uani 1 1 d . . . C24B C 0.1142(6) -0.0645(2) 1.0802(3) 0.0445(14) Uani 1 1 d . . . C24C C 0.4008(6) 0.3361(2) 1.2675(4) 0.0492(15) Uani 1 1 d . . . C24D C 0.7969(8) 0.0737(3) 1.1142(5) 0.073(2) Uani 1 1 d . . . C25A C 0.2322(7) 0.2438(3) 0.5445(4) 0.065(2) Uani 1 1 d . . . H25A H 0.2784 0.2402 0.5045 0.077 Uiso 1 1 calc R . . C25B C 0.0267(7) -0.0348(2) 1.0724(5) 0.063(2) Uani 1 1 d . . . H25B H 0.0481 -0.0090 1.0887 0.075 Uiso 1 1 calc R . . C25C C 0.4778(8) 0.3680(3) 1.2729(8) 0.108(5) Uani 1 1 d . . . H25C H 0.4467 0.3932 1.2587 0.130 Uiso 1 1 calc R . . C25D C 0.7269(7) 0.0418(3) 1.1038(4) 0.063(2) Uani 1 1 d . . . H25D H 0.7600 0.0165 1.1166 0.076 Uiso 1 1 calc R . . C26A C 0.1082(7) 0.2577(3) 0.5395(4) 0.064(2) Uani 1 1 d . . . H26A H 0.0715 0.2631 0.4953 0.077 Uiso 1 1 calc R . . C26B C -0.0929(6) -0.0416(2) 1.0410(5) 0.0589(19) Uani 1 1 d . . . H26B H -0.1515 -0.0201 1.0366 0.071 Uiso 1 1 calc R . . C26C C 0.6034(9) 0.3637(3) 1.2996(8) 0.111(5) Uani 1 1 d . . . H26C H 0.6537 0.3870 1.3048 0.133 Uiso 1 1 calc R . . C26D C 0.6067(7) 0.0453(3) 1.0744(4) 0.0567(17) Uani 1 1 d . . . H26D H 0.5570 0.0220 1.0668 0.068 Uiso 1 1 calc R . . N30 N 0.6621(5) 0.17722(19) 0.9041(4) 0.0560(15) Uani 1 1 d . . . O31 O 0.5768(5) 0.20091(18) 0.8900(3) 0.0735(16) Uani 1 1 d . . . O32 O 0.6411(7) 0.1428(2) 0.8899(5) 0.116(3) Uani 1 1 d . . . O33 O 0.7647(6) 0.1878(2) 0.9290(5) 0.116(3) Uani 1 1 d . . . N34 N 0.7590(10) 0.0527(3) 0.6577(5) 0.093(3) Uani 1 1 d . . . O35 O 0.7667(7) 0.0617(2) 0.7176(4) 0.092(2) Uani 1 1 d . . . O36 O 0.7765(10) 0.07805(19) 0.6166(4) 0.107(3) Uani 1 1 d . . . O37 O 0.7231(13) 0.0189(3) 0.6386(5) 0.143(4) Uani 1 1 d . . . N38 N -0.0878(11) 0.3596(5) 0.9705(7) 0.085(4) Uani 0.650(12) 1 d P A 1 O39 O -0.0937(9) 0.3777(3) 1.0230(3) 0.061(3) Uani 0.650(12) 1 d P A 1 O40 O -0.0887(16) 0.3700(5) 0.9099(5) 0.189(6) Uani 0.650(12) 1 d P A 1 O41 O -0.0748(12) 0.3168(6) 0.9605(8) 0.216(9) Uani 0.650(12) 1 d P A 1 O42 O 0.1024(5) 0.20968(16) 1.0642(4) 0.0660(15) Uani 1 1 d D . . H42 H 0.0701 0.1909 1.0854 0.079 Uiso 1 1 d R . . C43 C 0.0341(15) 0.2120(5) 0.9958(8) 0.238(15) Uani 1 1 d DU . . H43A H 0.0306 0.2395 0.9806 0.358 Uiso 1 1 calc R . . H43B H -0.0536 0.2017 0.9987 0.358 Uiso 1 1 calc R . . H43C H 0.0804 0.1961 0.9633 0.358 Uiso 1 1 calc R . . N44 N -0.061(2) 0.3288(8) 0.8904(9) 0.22(4) Uani 0.350(12) 1 d PD A 2 O45 O -0.0279(15) 0.3039(5) 0.8333(9) 0.083(7) Uani 0.350(12) 1 d PD A 2 O46 O -0.0748(12) 0.3168(6) 0.9605(8) 0.216(9) Uani 0.350(12) 1 d PD A 2 O47 O -0.0887(16) 0.3700(5) 0.9099(5) 0.189(6) Uani 0.350(12) 1 d PD A 2 O48 O 0.937(3) 0.0506(8) 1.3283(13) 0.164(9) Uiso 0.50 1 d P . . 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 0.0352(2) 0.0370(2) 0.0393(2) -0.00474(16) -0.00709(17) -0.00386(16) N1A 0.024(2) 0.043(3) 0.036(2) -0.002(2) -0.0106(17) 0.0000(18) N1B 0.031(2) 0.042(3) 0.036(2) -0.001(2) -0.0042(19) 0.0036(19) N1C 0.026(2) 0.036(2) 0.065(3) -0.010(2) -0.009(2) -0.0017(19) N1D 0.041(3) 0.074(4) 0.065(4) -0.002(3) 0.002(3) 0.002(3) Cd2 0.0333(2) 0.0424(3) 0.0334(2) 0.00135(16) -0.00700(16) 0.00408(16) C2A 0.026(2) 0.046(3) 0.037(3) -0.001(2) -0.008(2) 0.008(2) C2B 0.026(3) 0.051(3) 0.040(3) -0.006(3) -0.005(2) 0.000(2) C2C 0.031(3) 0.039(3) 0.065(4) -0.010(3) -0.011(3) 0.001(2) C2D 0.048(4) 0.094(6) 0.058(4) -0.008(4) 0.005(3) 0.012(4) Cd3 0.0344(2) 0.0349(2) 0.0613(3) -0.00739(19) 0.0000(2) -0.00550(16) C3A 0.047(3) 0.047(3) 0.048(3) 0.001(3) -0.008(3) 0.010(3) C3B 0.044(3) 0.062(4) 0.041(3) -0.009(3) -0.009(3) 0.004(3) C3C 0.053(4) 0.049(4) 0.068(5) -0.005(3) -0.013(3) 0.007(3) C3D 0.071(6) 0.088(6) 0.073(6) -0.025(5) 0.004(4) 0.007(5) C4A 0.067(5) 0.053(4) 0.048(4) -0.010(3) 0.006(3) 0.018(3) C4B 0.067(5) 0.072(5) 0.035(3) -0.002(3) -0.012(3) 0.005(4) C4C 0.080(6) 0.043(4) 0.081(6) -0.002(4) -0.022(4) 0.018(4) C4D 0.088(7) 0.068(5) 0.099(8) 0.000(5) 0.034(6) 0.014(5) C5A 0.050(4) 0.067(4) 0.036(3) -0.002(3) -0.001(3) 0.005(3) C5B 0.071(5) 0.062(4) 0.034(3) 0.010(3) -0.011(3) 0.001(4) C5C 0.057(4) 0.045(4) 0.085(6) -0.019(4) -0.025(4) 0.015(3) C5D 0.063(5) 0.082(6) 0.075(6) 0.006(5) 0.009(4) 0.014(4) C6A 0.024(2) 0.051(3) 0.036(3) -0.001(2) -0.008(2) 0.001(2) C6B 0.039(3) 0.050(3) 0.036(3) 0.006(3) -0.010(2) 0.002(3) C6C 0.028(3) 0.042(3) 0.076(5) -0.014(3) -0.013(3) 0.003(2) C6D 0.029(3) 0.085(6) 0.071(5) 0.012(4) 0.001(3) 0.002(3) C12A 0.024(2) 0.047(3) 0.037(3) 0.005(2) -0.008(2) 0.005(2) C12B 0.023(2) 0.049(3) 0.052(4) -0.008(3) -0.005(2) -0.001(2) C12C 0.029(3) 0.042(3) 0.063(4) -0.014(3) -0.006(3) -0.003(2) C12D 0.075(6) 0.120(10) 0.084(7) 0.012(7) 0.002(5) 0.008(6) O13A 0.038(2) 0.042(2) 0.037(2) -0.0010(17) -0.0060(16) 0.0077(17) O13B 0.037(2) 0.041(2) 0.046(2) 0.0001(18) -0.0013(17) 0.0044(17) O13C 0.047(2) 0.036(2) 0.056(3) -0.006(2) -0.003(2) -0.0033(18) O13D 0.182(11) 0.124(8) 0.095(6) 0.034(6) 0.002(6) 0.008(7) O14A 0.043(2) 0.051(2) 0.038(2) 0.0010(19) -0.0051(17) 0.0098(19) O14B 0.048(3) 0.044(2) 0.059(3) -0.009(2) 0.006(2) -0.010(2) O14C 0.042(2) 0.046(2) 0.060(3) -0.005(2) -0.008(2) -0.0018(19) O14D 0.082(5) 0.191(9) 0.056(4) 0.002(5) 0.007(3) 0.000(5) C15D 0.097(10) 0.31(3) 0.083(8) 0.063(12) 0.015(7) 0.037(13) C16A 0.021(2) 0.058(4) 0.038(3) 0.006(3) -0.010(2) -0.002(2) C16B 0.038(3) 0.043(3) 0.037(3) 0.005(2) -0.013(2) 0.005(2) C16C 0.020(2) 0.044(3) 0.080(5) -0.017(3) -0.006(3) -0.002(2) C16D 0.027(3) 0.137(9) 0.063(5) 0.024(5) 0.003(3) 0.004(4) O17A 0.052(3) 0.045(2) 0.042(2) -0.0007(19) -0.0067(19) -0.006(2) O17B 0.045(2) 0.044(2) 0.041(2) 0.0026(18) -0.0077(18) 0.0017(18) O17C 0.044(2) 0.047(3) 0.070(3) -0.011(2) -0.002(2) -0.0030(19) O17D 0.060(4) 0.124(6) 0.084(4) -0.004(4) -0.001(3) -0.033(4) N18A 0.030(2) 0.059(3) 0.036(3) 0.007(2) -0.0064(19) 0.002(2) N18B 0.054(3) 0.044(3) 0.039(3) 0.003(2) -0.017(2) 0.005(2) N18C 0.026(2) 0.049(3) 0.074(4) -0.017(3) -0.012(2) 0.005(2) N18D 0.047(4) 0.089(5) 0.096(6) -0.010(5) -0.013(4) 0.003(4) C19A 0.038(3) 0.064(4) 0.044(3) 0.015(3) -0.008(3) -0.002(3) C19B 0.045(3) 0.045(3) 0.053(4) 0.006(3) -0.016(3) 0.007(3) C19C 0.034(3) 0.062(4) 0.065(4) -0.021(4) -0.002(3) -0.002(3) C19D 0.050(5) 0.094(7) 0.141(10) -0.029(7) -0.023(5) 0.015(5) N21A 0.038(3) 0.045(3) 0.053(3) 0.004(2) -0.004(2) 0.003(2) N21B 0.039(3) 0.055(3) 0.046(3) -0.002(2) -0.008(2) 0.008(2) N21C 0.037(3) 0.046(3) 0.056(3) -0.001(2) -0.011(2) 0.002(2) N21D 0.033(3) 0.062(3) 0.041(3) -0.006(2) -0.005(2) 0.008(2) C22A 0.069(6) 0.164(11) 0.060(5) -0.014(6) -0.008(4) 0.051(7) C22B 0.079(6) 0.073(6) 0.148(10) -0.059(6) -0.066(7) 0.038(5) C22C 0.057(5) 0.069(5) 0.119(8) 0.023(5) -0.019(5) -0.008(4) C22D 0.036(4) 0.078(6) 0.122(8) -0.030(5) -0.009(4) 0.005(4) C23A 0.072(6) 0.164(11) 0.051(5) -0.003(6) -0.011(4) 0.058(7) C23B 0.074(6) 0.078(6) 0.133(9) -0.062(6) -0.066(6) 0.043(5) C23C 0.046(4) 0.068(5) 0.118(8) 0.017(5) -0.017(4) -0.010(4) C23D 0.043(4) 0.095(7) 0.181(13) -0.049(8) -0.021(6) -0.003(5) C24A 0.036(3) 0.050(3) 0.045(3) 0.011(3) -0.004(2) -0.001(3) C24B 0.043(3) 0.050(3) 0.040(3) 0.002(3) -0.007(3) 0.007(3) C24C 0.031(3) 0.052(4) 0.064(4) -0.016(3) -0.005(3) -0.001(3) C24D 0.046(4) 0.083(6) 0.090(6) -0.015(5) 0.000(4) 0.024(4) C25A 0.041(4) 0.098(6) 0.053(4) -0.007(4) -0.005(3) 0.009(4) C25B 0.039(3) 0.036(3) 0.112(7) 0.004(4) -0.012(4) -0.003(3) C25C 0.044(4) 0.054(5) 0.223(15) -0.012(7) -0.045(6) 0.007(4) C25D 0.048(4) 0.075(5) 0.065(5) -0.005(4) -0.004(3) 0.015(4) C26A 0.046(4) 0.091(6) 0.054(4) -0.001(4) -0.014(3) 0.010(4) C26B 0.035(3) 0.041(3) 0.099(6) 0.009(4) -0.012(3) 0.003(3) C26C 0.052(5) 0.052(5) 0.222(15) 0.000(7) -0.055(7) -0.002(4) C26D 0.045(4) 0.070(5) 0.054(4) 0.000(3) -0.003(3) 0.017(3) N30 0.030(3) 0.059(4) 0.078(4) 0.008(3) -0.013(3) 0.003(2) O31 0.050(3) 0.070(4) 0.097(4) -0.007(3) -0.020(3) 0.017(3) O32 0.079(5) 0.080(5) 0.184(9) -0.024(5) -0.062(5) 0.001(4) O33 0.046(3) 0.094(5) 0.201(9) -0.057(6) -0.054(4) 0.016(3) N34 0.119(7) 0.069(5) 0.090(6) 0.028(5) 0.005(5) 0.005(5) O35 0.088(5) 0.109(6) 0.076(4) 0.035(4) -0.017(4) -0.027(4) O36 0.191(9) 0.052(4) 0.080(5) 0.027(3) 0.019(5) -0.003(4) O37 0.226(13) 0.066(5) 0.136(8) 0.031(5) 0.008(8) -0.019(6) N38 0.057(6) 0.124(11) 0.072(8) 0.055(8) -0.015(5) -0.005(7) O39 0.083(6) 0.077(6) 0.021(3) 0.012(3) -0.003(3) 0.001(4) O40 0.239(16) 0.249(16) 0.077(6) 0.074(8) -0.023(8) 0.003(12) O41 0.112(8) 0.32(2) 0.215(15) 0.171(15) -0.024(9) -0.072(11) O42 0.036(2) 0.048(3) 0.112(5) 0.001(3) -0.009(3) -0.003(2) C43 0.169(17) 0.23(2) 0.33(3) -0.20(2) 0.16(2) -0.131(16) N44 0.047(14) 0.55(11) 0.051(15) -0.10(3) 0.005(11) -0.03(3) O45 0.058(10) 0.065(10) 0.122(16) 0.031(10) -0.046(10) -0.019(8) O46 0.112(8) 0.32(2) 0.215(15) 0.171(15) -0.024(9) -0.072(11) O47 0.239(16) 0.249(16) 0.077(6) 0.074(8) -0.023(8) 0.003(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 O31 2.314(6) . ? Cd1 N1A 2.340(5) . ? Cd1 O13A 2.375(4) . ? Cd1 O17A 2.381(5) . ? Cd1 N21C 2.389(5) 4_565 ? Cd1 O14C 2.397(5) . ? Cd1 O13C 2.440(5) . ? Cd1 C12C 2.746(6) . ? N1A C6A 1.331(8) . ? N1A C2A 1.332(8) . ? N1B C2B 1.329(8) . ? N1B C6B 1.333(8) . ? N1B Cd2 2.357(5) . ? N1C C2C 1.332(9) . ? N1C C6C 1.344(8) . ? N1C Cd3 2.329(5) . ? N1D C6D 1.328(10) . ? N1D C2D 1.332(11) . ? Cd2 N21D 2.296(5) . ? Cd2 N21B 2.298(5) 3_557 ? Cd2 O13B 2.381(4) . ? Cd2 O13A 2.403(4) . ? Cd2 O17B 2.459(4) . ? Cd2 O14A 2.472(4) . ? C2A C3A 1.382(9) . ? C2A C12A 1.510(8) . ? C2B C3B 1.394(9) . ? C2B C12B 1.499(9) . ? C2C C3C 1.388(10) . ? C2C C12C 1.507(9) . ? C2D C3D 1.422(14) . ? C2D C12D 1.458(15) . ? Cd3 O42 2.294(5) . ? Cd3 O14B 2.309(5) . ? Cd3 N21A 2.324(5) 4_666 ? Cd3 O13C 2.360(5) . ? Cd3 O17C 2.452(5) . ? Cd3 O13B 2.540(4) . ? Cd3 C12B 2.749(7) . ? C3A C4A 1.384(10) . ? C3A H3A 0.9500 . ? C3B C4B 1.361(11) . ? C3B H3B 0.9500 . ? C3C C4C 1.379(11) . ? C3C H3C 0.9500 . ? C3D C4D 1.365(15) . ? C3D H3D 0.9500 . ? C4A C5A 1.394(11) . ? C4A H4A 0.9500 . ? C4B C5B 1.388(11) . ? C4B H4B 0.9500 . ? C4C C5C 1.382(12) . ? C4C H4C 0.9500 . ? C4D C5D 1.338(14) . ? C4D H4D 0.9500 . ? C5A C6A 1.375(9) . ? C5A H5A 0.9500 . ? C5B C6B 1.399(9) . ? C5B H5B 0.9500 . ? C5C C6C 1.380(11) . ? C5C H5C 0.9500 . ? C5D C6D 1.363(13) . ? C5D H5D 0.9500 . ? C6A C16A 1.521(9) . ? C6B C16B 1.501(9) . ? C6C C16C 1.498(11) . ? C6D C16D 1.566(14) . ? C12A O13A 1.257(7) . ? C12A O14A 1.258(7) . ? C12B O14B 1.248(8) . ? C12B O13B 1.261(7) . ? C12C O14C 1.247(9) . ? C12C O13C 1.268(8) . ? C12D O13D 1.197(16) . ? C12D O14D 1.336(15) . ? O14D C15D 1.450(15) . ? C15D H15A 0.9800 . ? C15D H15B 0.9800 . ? C15D H15C 0.9800 . ? C16A O17A 1.238(8) . ? C16A N18A 1.330(8) . ? C16B O17B 1.240(7) . ? C16B N18B 1.319(8) . ? C16C O17C 1.240(9) . ? C16C N18C 1.326(8) . ? C16D O17D 1.239(10) . ? C16D N18D 1.281(13) . ? N18A C19A 1.462(9) . ? N18A H18A 0.8800 . ? N18B C19B 1.462(9) . ? N18B H18B 0.8800 . ? N18C C19C 1.456(10) . ? N18C H18C 0.8800 . ? N18D C19D 1.487(13) . ? N18D H18D 0.8800 . ? C19A C24A 1.511(9) . ? C19A H19A 0.9900 . ? C19A H19B 0.9900 . ? C19B C24B 1.515(9) . ? C19B H19C 0.9900 . ? C19B H19D 0.9900 . ? C19C C24C 1.512(9) . ? C19C H19E 0.9900 . ? C19C H19F 0.9900 . ? C19D C24D 1.538(12) . ? C19D H19G 0.9900 . ? C19D H19H 0.9900 . ? N21A C26A 1.300(10) . ? N21A C22A 1.305(11) . ? N21A Cd3 2.324(5) 4_565 ? N21B C26B 1.305(9) . ? N21B C22B 1.329(10) . ? N21B Cd2 2.298(5) 3_557 ? N21C C26C 1.287(11) . ? N21C C22C 1.345(11) . ? N21C Cd1 2.389(5) 4_666 ? N21D C22D 1.308(11) . ? N21D C26D 1.363(9) . ? C22A C23A 1.384(12) . ? C22A H22A 0.9500 . ? C22B C23B 1.383(11) . ? C22B H22B 0.9500 . ? C22C C23C 1.401(12) . ? C22C H22C 0.9500 . ? C22D C23D 1.400(12) . ? C22D H22D 0.9500 . ? C23A C24A 1.368(11) . ? C23A H23A 0.9500 . ? C23B C24B 1.372(11) . ? C23B H23B 0.9500 . ? C23C C24C 1.334(11) . ? C23C H23C 0.9500 . ? C23D C24D 1.424(15) . ? C23D H23D 0.9500 . ? C24A C25A 1.369(10) . ? C24B C25B 1.361(9) . ? C24C C25C 1.345(11) . ? C24D C25D 1.313(13) . ? C25A C26A 1.373(10) . ? C25A H25A 0.9500 . ? C25B C26B 1.381(10) . ? C25B H25B 0.9500 . ? C25C C26C 1.391(12) . ? C25C H25C 0.9500 . ? C25D C26D 1.358(10) . ? C25D H25D 0.9500 . ? C26A H26A 0.9500 . ? C26B H26B 0.9500 . ? C26C H26C 0.9500 . ? C26D H26D 0.9500 . ? N30 O33 1.206(8) . ? N30 O32 1.214(9) . ? N30 O31 1.218(8) . ? N34 O36 1.199(10) . ? N34 O35 1.217(11) . ? N34 O37 1.255(13) . ? N38 O39 1.204(18) . ? N38 O40 1.245(14) . ? N38 O41 1.47(2) . ? O42 C43 1.492(17) . ? O42 H42 0.8400 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? N44 O45 1.460(17) . ? 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 O31 Cd1 N1A 107.01(18) . . ? O31 Cd1 O13A 103.76(18) . . ? N1A Cd1 O13A 69.13(16) . . ? O31 Cd1 O17A 84.8(2) . . ? N1A Cd1 O17A 67.87(16) . . ? O13A Cd1 O17A 136.77(15) . . ? O31 Cd1 N21C 162.62(19) . 4_565 ? N1A Cd1 N21C 86.65(17) . 4_565 ? O13A Cd1 N21C 90.99(17) . 4_565 ? O17A Cd1 N21C 90.73(18) . 4_565 ? O31 Cd1 O14C 80.02(18) . . ? N1A Cd1 O14C 143.92(17) . . ? O13A Cd1 O14C 145.02(16) . . ? O17A Cd1 O14C 77.90(17) . . ? N21C Cd1 O14C 82.63(17) 4_565 . ? O31 Cd1 O13C 77.14(19) . . ? N1A Cd1 O13C 161.07(16) . . ? O13A Cd1 O13C 91.95(15) . . ? O17A Cd1 O13C 131.03(15) . . ? N21C Cd1 O13C 93.45(18) 4_565 . ? O14C Cd1 O13C 54.45(16) . . ? O31 Cd1 C12C 76.61(19) . . ? N1A Cd1 C12C 170.49(19) . . ? O13A Cd1 C12C 119.04(19) . . ? O17A Cd1 C12C 104.18(19) . . ? N21C Cd1 C12C 88.29(18) 4_565 . ? O14C Cd1 C12C 26.97(19) . . ? O13C Cd1 C12C 27.49(19) . . ? C6A N1A C2A 120.2(5) . . ? C6A N1A Cd1 121.0(4) . . ? C2A N1A Cd1 118.8(4) . . ? C2B N1B C6B 120.3(5) . . ? C2B N1B Cd2 118.1(4) . . ? C6B N1B Cd2 121.1(4) . . ? C2C N1C C6C 120.1(6) . . ? C2C N1C Cd3 118.4(4) . . ? C6C N1C Cd3 121.4(5) . . ? C6D N1D C2D 115.8(8) . . ? N21D Cd2 N21B 168.5(2) . 3_557 ? N21D Cd2 N1B 85.96(18) . . ? N21B Cd2 N1B 100.92(19) 3_557 . ? N21D Cd2 O13B 89.83(17) . . ? N21B Cd2 O13B 101.15(17) 3_557 . ? N1B Cd2 O13B 68.90(16) . . ? N21D Cd2 O13A 94.43(17) . . ? N21B Cd2 O13A 83.07(18) 3_557 . ? N1B Cd2 O13A 155.72(15) . . ? O13B Cd2 O13A 86.82(14) . . ? N21D Cd2 O17B 90.36(18) . . ? N21B Cd2 O17B 84.02(18) 3_557 . ? N1B Cd2 O17B 67.10(16) . . ? O13B Cd2 O17B 135.87(15) . . ? O13A Cd2 O17B 137.10(14) . . ? N21D Cd2 O14A 85.28(17) . . ? N21B Cd2 O14A 84.22(18) 3_557 . ? N1B Cd2 O14A 149.76(15) . . ? O13B Cd2 O14A 139.87(15) . . ? O13A Cd2 O14A 54.04(15) . . ? O17B Cd2 O14A 84.06(15) . . ? N1A C2A C3A 121.4(6) . . ? N1A C2A C12A 115.0(5) . . ? C3A C2A C12A 123.5(6) . . ? N1B C2B C3B 121.6(6) . . ? N1B C2B C12B 115.3(5) . . ? C3B C2B C12B 123.1(6) . . ? N1C C2C C3C 122.6(6) . . ? N1C C2C C12C 115.6(6) . . ? C3C C2C C12C 121.8(7) . . ? N1D C2D C3D 122.3(8) . . ? N1D C2D C12D 114.4(10) . . ? C3D C2D C12D 123.3(9) . . ? O42 Cd3 O14B 86.2(2) . . ? O42 Cd3 N21A 175.8(2) . 4_666 ? O14B Cd3 N21A 90.01(19) . 4_666 ? O42 Cd3 N1C 89.94(18) . . ? O14B Cd3 N1C 152.74(18) . . ? N21A Cd3 N1C 92.50(18) 4_666 . ? O42 Cd3 O13C 89.6(2) . . ? O14B Cd3 O13C 137.31(16) . . ? N21A Cd3 O13C 94.53(18) 4_666 . ? N1C Cd3 O13C 69.52(17) . . ? O42 Cd3 O17C 87.69(19) . . ? O14B Cd3 O17C 85.26(17) . . ? N21A Cd3 O17C 90.03(18) 4_666 . ? N1C Cd3 O17C 67.61(19) . . ? O13C Cd3 O17C 137.03(17) . . ? O42 Cd3 O13B 80.87(16) . . ? O14B Cd3 O13B 54.00(15) . . ? N21A Cd3 O13B 98.51(17) 4_666 . ? N1C Cd3 O13B 151.48(16) . . ? O13C Cd3 O13B 83.38(14) . . ? O17C Cd3 O13B 138.08(16) . . ? O42 Cd3 C12B 81.78(18) . . ? O14B Cd3 C12B 26.82(17) . . ? N21A Cd3 C12B 95.73(18) 4_666 . ? N1C Cd3 C12B 171.72(16) . . ? O13C Cd3 C12B 110.60(17) . . ? O17C Cd3 C12B 111.39(18) . . ? O13B Cd3 C12B 27.22(16) . . ? C2A C3A C4A 118.7(6) . . ? C2A C3A H3A 120.6 . . ? C4A C3A H3A 120.6 . . ? C4B C3B C2B 118.8(6) . . ? C4B C3B H3B 120.6 . . ? C2B C3B H3B 120.6 . . ? C4C C3C C2C 116.8(8) . . ? C4C C3C H3C 121.6 . . ? C2C C3C H3C 121.6 . . ? C4D C3D C2D 117.7(9) . . ? C4D C3D H3D 121.1 . . ? C2D C3D H3D 121.1 . . ? C3A C4A C5A 119.4(6) . . ? C3A C4A H4A 120.3 . . ? C5A C4A H4A 120.3 . . ? C3B C4B C5B 119.8(6) . . ? C3B C4B H4B 120.1 . . ? C5B C4B H4B 120.1 . . ? C3C C4C C5C 121.0(7) . . ? C3C C4C H4C 119.5 . . ? C5C C4C H4C 119.5 . . ? C5D C4D C3D 120.2(10) . . ? C5D C4D H4D 119.9 . . ? C3D C4D H4D 119.9 . . ? C6A C5A C4A 118.1(6) . . ? C6A C5A H5A 120.9 . . ? C4A C5A H5A 120.9 . . ? C4B C5B C6B 118.5(7) . . ? C4B C5B H5B 120.7 . . ? C6B C5B H5B 120.7 . . ? C6C C5C C4C 118.7(7) . . ? C6C C5C H5C 120.7 . . ? C4C C5C H5C 120.7 . . ? C4D C5D C6D 118.3(9) . . ? C4D C5D H5D 120.8 . . ? C6D C5D H5D 120.8 . . ? N1A C6A C5A 122.2(6) . . ? N1A C6A C16A 111.3(5) . . ? C5A C6A C16A 126.5(6) . . ? N1B C6B C5B 120.9(6) . . ? N1B C6B C16B 113.7(5) . . ? C5B C6B C16B 125.4(6) . . ? N1C C6C C5C 120.7(7) . . ? N1C C6C C16C 113.1(6) . . ? C5C C6C C16C 126.1(6) . . ? N1D C6D C5D 125.6(9) . . ? N1D C6D C16D 113.4(8) . . ? C5D C6D C16D 121.0(8) . . ? O13A C12A O14A 123.5(5) . . ? O13A C12A C2A 118.4(5) . . ? O14A C12A C2A 118.1(5) . . ? O14B C12B O13B 123.6(6) . . ? O14B C12B C2B 117.4(6) . . ? O13B C12B C2B 119.0(5) . . ? O14B C12B Cd3 56.6(3) . . ? O13B C12B Cd3 67.1(3) . . ? C2B C12B Cd3 172.6(4) . . ? O14C C12C O13C 123.3(6) . . ? O14C C12C C2C 119.0(6) . . ? O13C C12C C2C 117.7(6) . . ? O14C C12C Cd1 60.7(3) . . ? O13C C12C Cd1 62.7(3) . . ? C2C C12C Cd1 179.2(5) . . ? O13D C12D O14D 121.7(12) . . ? O13D C12D C2D 125.4(12) . . ? O14D C12D C2D 112.9(12) . . ? C12A O13A Cd1 118.4(4) . . ? C12A O13A Cd2 92.8(3) . . ? Cd1 O13A Cd2 148.54(19) . . ? C12B O13B Cd2 118.0(4) . . ? C12B O13B Cd3 85.7(4) . . ? Cd2 O13B Cd3 156.38(19) . . ? C12C O13C Cd3 118.6(4) . . ? C12C O13C Cd1 89.8(4) . . ? Cd3 O13C Cd1 151.0(2) . . ? C12A O14A Cd2 89.6(4) . . ? C12B O14B Cd3 96.6(4) . . ? C12C O14C Cd1 92.3(4) . . ? C12D O14D C15D 114.7(13) . . ? O14D C15D H15A 109.5 . . ? O14D C15D H15B 109.5 . . ? H15A C15D H15B 109.5 . . ? O14D C15D H15C 109.5 . . ? H15A C15D H15C 109.5 . . ? H15B C15D H15C 109.5 . . ? O17A C16A N18A 121.4(6) . . ? O17A C16A C6A 119.7(5) . . ? N18A C16A C6A 118.9(6) . . ? O17B C16B N18B 122.9(6) . . ? O17B C16B C6B 119.8(5) . . ? N18B C16B C6B 117.3(5) . . ? O17C C16C N18C 122.1(7) . . ? O17C C16C C6C 120.1(6) . . ? N18C C16C C6C 117.8(6) . . ? O17D C16D N18D 124.2(11) . . ? O17D C16D C6D 119.3(10) . . ? N18D C16D C6D 116.5(8) . . ? C16A O17A Cd1 117.3(4) . . ? C16B O17B Cd2 117.7(4) . . ? C16C O17C Cd3 116.8(5) . . ? C16A N18A C19A 119.9(6) . . ? C16A N18A H18A 120.0 . . ? C19A N18A H18A 120.0 . . ? C16B N18B C19B 121.8(6) . . ? C16B N18B H18B 119.1 . . ? C19B N18B H18B 119.1 . . ? C16C N18C C19C 120.7(7) . . ? C16C N18C H18C 119.6 . . ? C19C N18C H18C 119.6 . . ? C16D N18D C19D 122.9(10) . . ? C16D N18D H18D 118.6 . . ? C19D N18D H18D 118.6 . . ? N18A C19A C24A 112.3(5) . . ? N18A C19A H19A 109.1 . . ? C24A C19A H19A 109.1 . . ? N18A C19A H19B 109.1 . . ? C24A C19A H19B 109.1 . . ? H19A C19A H19B 107.9 . . ? N18B C19B C24B 113.3(5) . . ? N18B C19B H19C 108.9 . . ? C24B C19B H19C 108.9 . . ? N18B C19B H19D 108.9 . . ? C24B C19B H19D 108.9 . . ? H19C C19B H19D 107.7 . . ? N18C C19C C24C 111.5(6) . . ? N18C C19C H19E 109.3 . . ? C24C C19C H19E 109.3 . . ? N18C C19C H19F 109.3 . . ? C24C C19C H19F 109.3 . . ? H19E C19C H19F 108.0 . . ? N18D C19D C24D 114.4(8) . . ? N18D C19D H19G 108.7 . . ? C24D C19D H19G 108.7 . . ? N18D C19D H19H 108.7 . . ? C24D C19D H19H 108.7 . . ? H19G C19D H19H 107.6 . . ? C26A N21A C22A 115.3(7) . . ? C26A N21A Cd3 120.1(5) . 4_565 ? C22A N21A Cd3 124.4(6) . 4_565 ? C26B N21B C22B 116.7(6) . . ? C26B N21B Cd2 119.2(4) . 3_557 ? C22B N21B Cd2 124.0(5) . 3_557 ? C26C N21C C22C 113.3(7) . . ? C26C N21C Cd1 123.9(5) . 4_666 ? C22C N21C Cd1 122.7(5) . 4_666 ? C22D N21D C26D 119.1(7) . . ? C22D N21D Cd2 121.4(5) . . ? C26D N21D Cd2 118.8(5) . . ? N21A C22A C23A 124.2(9) . . ? N21A C22A H22A 117.9 . . ? C23A C22A H22A 117.9 . . ? N21B C22B C23B 122.8(8) . . ? N21B C22B H22B 118.6 . . ? C23B C22B H22B 118.6 . . ? N21C C22C C23C 124.8(8) . . ? N21C C22C H22C 117.6 . . ? C23C C22C H22C 117.6 . . ? N21D C22D C23D 120.5(10) . . ? N21D C22D H22D 119.8 . . ? C23D C22D H22D 119.8 . . ? C24A C23A C22A 120.1(8) . . ? C24A C23A H23A 119.9 . . ? C22A C23A H23A 119.9 . . ? C24B C23B C22B 120.4(7) . . ? C24B C23B H23B 119.8 . . ? C22B C23B H23B 119.8 . . ? C24C C23C C22C 118.5(8) . . ? C24C C23C H23C 120.7 . . ? C22C C23C H23C 120.7 . . ? C22D C23D C24D 118.3(10) . . ? C22D C23D H23D 120.9 . . ? C24D C23D H23D 120.9 . . ? C23A C24A C25A 114.7(7) . . ? C23A C24A C19A 123.9(6) . . ? C25A C24A C19A 121.2(6) . . ? C25B C24B C23B 115.9(6) . . ? C25B C24B C19B 123.5(6) . . ? C23B C24B C19B 120.6(6) . . ? C23C C24C C25C 118.0(7) . . ? C23C C24C C19C 120.2(7) . . ? C25C C24C C19C 121.7(7) . . ? C25D C24D C23D 119.8(8) . . ? C25D C24D C19D 119.7(9) . . ? C23D C24D C19D 120.4(9) . . ? C24A C25A C26A 120.4(7) . . ? C24A C25A H25A 119.8 . . ? C26A C25A H25A 119.8 . . ? C24B C25B C26B 120.6(7) . . ? C24B C25B H25B 119.7 . . ? C26B C25B H25B 119.7 . . ? C24C C25C C26C 119.4(9) . . ? C24C C25C H25C 120.3 . . ? C26C C25C H25C 120.3 . . ? C24D C25D C26D 119.1(8) . . ? C24D C25D H25D 120.4 . . ? C26D C25D H25D 120.4 . . ? N21A C26A C25A 124.5(7) . . ? N21A C26A H26A 117.7 . . ? C25A C26A H26A 117.7 . . ? N21B C26B C25B 123.6(6) . . ? N21B C26B H26B 118.2 . . ? C25B C26B H26B 118.2 . . ? N21C C26C C25C 125.7(8) . . ? N21C C26C H26C 117.2 . . ? C25C C26C H26C 117.2 . . ? C25D C26D N21D 123.1(8) . . ? C25D C26D H26D 118.4 . . ? N21D C26D H26D 118.4 . . ? O33 N30 O32 121.5(7) . . ? O33 N30 O31 121.2(7) . . ? O32 N30 O31 117.2(6) . . ? N30 O31 Cd1 116.7(5) . . ? O36 N34 O35 118.1(10) . . ? O36 N34 O37 120.2(11) . . ? O35 N34 O37 121.5(9) . . ? O39 N38 O40 133.0(17) . . ? O39 N38 O41 128.6(11) . . ? O40 N38 O41 98.4(15) . . ? C43 O42 Cd3 118.8(7) . . ? C43 O42 H42 107.7 . . ? Cd3 O42 H42 121.7 . . ? O42 C43 H43A 109.5 . . ? O42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? O42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? 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 O31 Cd1 N1A C6A -84.5(4) . . . . ? O13A Cd1 N1A C6A 176.9(4) . . . . ? O17A Cd1 N1A C6A -7.6(4) . . . . ? N21C Cd1 N1A C6A 84.5(4) 4_565 . . . ? O14C Cd1 N1A C6A 11.9(5) . . . . ? O13C Cd1 N1A C6A 175.4(4) . . . . ? C12C Cd1 N1A C6A 26.6(12) . . . . ? O31 Cd1 N1A C2A 96.6(4) . . . . ? O13A Cd1 N1A C2A -2.0(4) . . . . ? O17A Cd1 N1A C2A 173.5(4) . . . . ? N21C Cd1 N1A C2A -94.3(4) 4_565 . . . ? O14C Cd1 N1A C2A -166.9(3) . . . . ? O13C Cd1 N1A C2A -3.4(7) . . . . ? C12C Cd1 N1A C2A -152.3(9) . . . . ? C2B N1B Cd2 N21D 83.4(4) . . . . ? C6B N1B Cd2 N21D -88.7(5) . . . . ? C2B N1B Cd2 N21B -105.9(4) . . . 3_557 ? C6B N1B Cd2 N21B 82.1(5) . . . 3_557 ? C2B N1B Cd2 O13B -8.0(4) . . . . ? C6B N1B Cd2 O13B 179.9(5) . . . . ? C2B N1B Cd2 O13A -8.5(7) . . . . ? C6B N1B Cd2 O13A 179.5(4) . . . . ? C2B N1B Cd2 O17B 175.5(4) . . . . ? C6B N1B Cd2 O17B 3.4(4) . . . . ? C2B N1B Cd2 O14A 156.8(4) . . . . ? C6B N1B Cd2 O14A -15.2(6) . . . . ? C6A N1A C2A C3A 0.0(8) . . . . ? Cd1 N1A C2A C3A 178.9(4) . . . . ? C6A N1A C2A C12A -178.6(5) . . . . ? Cd1 N1A C2A C12A 0.3(6) . . . . ? C6B N1B C2B C3B 0.6(8) . . . . ? Cd2 N1B C2B C3B -171.5(4) . . . . ? C6B N1B C2B C12B -178.9(5) . . . . ? Cd2 N1B C2B C12B 9.0(6) . . . . ? C6C N1C C2C C3C 0.4(9) . . . . ? Cd3 N1C C2C C3C 178.6(5) . . . . ? C6C N1C C2C C12C -179.9(5) . . . . ? Cd3 N1C C2C C12C -1.7(7) . . . . ? C6D N1D C2D C3D 1.0(11) . . . . ? C6D N1D C2D C12D 179.8(7) . . . . ? C2C N1C Cd3 O42 -90.1(4) . . . . ? C6C N1C Cd3 O42 88.1(5) . . . . ? C2C N1C Cd3 O14B -171.7(4) . . . . ? C6C N1C Cd3 O14B 6.5(7) . . . . ? C2C N1C Cd3 N21A 93.4(4) . . . 4_666 ? C6C N1C Cd3 N21A -88.4(4) . . . 4_666 ? C2C N1C Cd3 O13C -0.5(4) . . . . ? C6C N1C Cd3 O13C 177.7(5) . . . . ? C2C N1C Cd3 O17C -177.6(5) . . . . ? C6C N1C Cd3 O17C 0.6(4) . . . . ? C2C N1C Cd3 O13B -19.6(6) . . . . ? C6C N1C Cd3 O13B 158.6(4) . . . . ? C2C N1C Cd3 C12B -92.9(14) . . . . ? C6C N1C Cd3 C12B 85.3(14) . . . . ? N1A C2A C3A C4A 0.4(9) . . . . ? C12A C2A C3A C4A 178.9(6) . . . . ? N1B C2B C3B C4B -1.3(10) . . . . ? C12B C2B C3B C4B 178.1(6) . . . . ? N1C C2C C3C C4C -0.9(11) . . . . ? C12C C2C C3C C4C 179.5(7) . . . . ? N1D C2D C3D C4D -1.1(13) . . . . ? C12D C2D C3D C4D -179.7(9) . . . . ? C2A C3A C4A C5A -0.3(11) . . . . ? C2B C3B C4B C5B 1.2(11) . . . . ? C2C C3C C4C C5C 0.8(12) . . . . ? C2D C3D C4D C5D 0.2(14) . . . . ? C3A C4A C5A C6A -0.2(11) . . . . ? C3B C4B C5B C6B -0.4(12) . . . . ? C3C C4C C5C C6C -0.3(13) . . . . ? C3D C4D C5D C6D 0.5(14) . . . . ? C2A N1A C6A C5A -0.6(8) . . . . ? Cd1 N1A C6A C5A -179.4(4) . . . . ? C2A N1A C6A C16A -179.7(5) . . . . ? Cd1 N1A C6A C16A 1.5(6) . . . . ? C4A C5A C6A N1A 0.7(10) . . . . ? C4A C5A C6A C16A 179.6(6) . . . . ? C2B N1B C6B C5B 0.2(9) . . . . ? Cd2 N1B C6B C5B 172.0(5) . . . . ? C2B N1B C6B C16B -179.4(5) . . . . ? Cd2 N1B C6B C16B -7.5(7) . . . . ? C4B C5B C6B N1B -0.3(11) . . . . ? C4B C5B C6B C16B 179.2(7) . . . . ? C2C N1C C6C C5C 0.1(9) . . . . ? Cd3 N1C C6C C5C -178.0(5) . . . . ? C2C N1C C6C C16C -177.7(5) . . . . ? Cd3 N1C C6C C16C 4.1(7) . . . . ? C4C C5C C6C N1C -0.2(11) . . . . ? C4C C5C C6C C16C 177.4(7) . . . . ? C2D N1D C6D C5D -0.2(11) . . . . ? C2D N1D C6D C16D 175.5(6) . . . . ? C4D C5D C6D N1D -0.5(13) . . . . ? C4D C5D C6D C16D -176.0(8) . . . . ? N1A C2A C12A O13A 3.4(7) . . . . ? C3A C2A C12A O13A -175.2(5) . . . . ? N1A C2A C12A O14A -177.6(5) . . . . ? C3A C2A C12A O14A 3.8(8) . . . . ? N1B C2B C12B O14B 176.0(5) . . . . ? C3B C2B C12B O14B -3.5(8) . . . . ? N1B C2B C12B O13B -3.3(7) . . . . ? C3B C2B C12B O13B 177.2(5) . . . . ? N1B C2B C12B Cd3 141(3) . . . . ? C3B C2B C12B Cd3 -38(3) . . . . ? O42 Cd3 C12B O14B -98.0(4) . . . . ? N21A Cd3 C12B O14B 78.6(4) 4_666 . . . ? N1C Cd3 C12B O14B -95.1(13) . . . . ? O13C Cd3 C12B O14B 175.6(3) . . . . ? O17C Cd3 C12B O14B -13.7(4) . . . . ? O13B Cd3 C12B O14B 176.1(5) . . . . ? O42 Cd3 C12B O13B 86.0(3) . . . . ? O14B Cd3 C12B O13B -176.1(5) . . . . ? N21A Cd3 C12B O13B -97.5(3) 4_666 . . . ? N1C Cd3 C12B O13B 88.8(14) . . . . ? O13C Cd3 C12B O13B -0.4(3) . . . . ? O17C Cd3 C12B O13B 170.2(3) . . . . ? O42 Cd3 C12B C2B -60(3) . . . . ? O14B Cd3 C12B C2B 37(3) . . . . ? N21A Cd3 C12B C2B 116(3) 4_666 . . . ? N1C Cd3 C12B C2B -58(4) . . . . ? O13C Cd3 C12B C2B -147(3) . . . . ? O17C Cd3 C12B C2B 24(3) . . . . ? O13B Cd3 C12B C2B -146(3) . . . . ? N1C C2C C12C O14C -176.7(5) . . . . ? C3C C2C C12C O14C 3.0(9) . . . . ? N1C C2C C12C O13C 4.6(8) . . . . ? C3C C2C C12C O13C -175.7(6) . . . . ? N1C C2C C12C Cd1 -113(38) . . . . ? C3C C2C C12C Cd1 67(38) . . . . ? O31 Cd1 C12C O14C 94.3(4) . . . . ? N1A Cd1 C12C O14C -19.2(12) . . . . ? O13A Cd1 C12C O14C -167.2(3) . . . . ? O17A Cd1 C12C O14C 13.3(4) . . . . ? N21C Cd1 C12C O14C -77.0(4) 4_565 . . . ? O13C Cd1 C12C O14C -177.9(6) . . . . ? O31 Cd1 C12C O13C -87.8(4) . . . . ? N1A Cd1 C12C O13C 158.7(9) . . . . ? O13A Cd1 C12C O13C 10.7(4) . . . . ? O17A Cd1 C12C O13C -168.8(3) . . . . ? N21C Cd1 C12C O13C 100.8(4) 4_565 . . . ? O14C Cd1 C12C O13C 177.9(6) . . . . ? O31 Cd1 C12C C2C 30(38) . . . . ? N1A Cd1 C12C C2C -83(38) . . . . ? O13A Cd1 C12C C2C 129(38) . . . . ? O17A Cd1 C12C C2C -51(38) . . . . ? N21C Cd1 C12C C2C -141(38) 4_565 . . . ? O14C Cd1 C12C C2C -64(38) . . . . ? O13C Cd1 C12C C2C 118(38) . . . . ? N1D C2D C12D O13D 13.8(16) . . . . ? C3D C2D C12D O13D -167.4(12) . . . . ? N1D C2D C12D O14D -167.5(8) . . . . ? C3D C2D C12D O14D 11.3(13) . . . . ? O14A C12A O13A Cd1 175.7(4) . . . . ? C2A C12A O13A Cd1 -5.3(6) . . . . ? O14A C12A O13A Cd2 -0.6(6) . . . . ? C2A C12A O13A Cd2 178.4(4) . . . . ? O31 Cd1 O13A C12A -99.3(4) . . . . ? N1A Cd1 O13A C12A 3.9(4) . . . . ? O17A Cd1 O13A C12A -2.2(5) . . . . ? N21C Cd1 O13A C12A 89.9(4) 4_565 . . . ? O14C Cd1 O13A C12A 168.5(4) . . . . ? O13C Cd1 O13A C12A -176.6(4) . . . . ? C12C Cd1 O13A C12A 178.5(4) . . . . ? O31 Cd1 O13A Cd2 73.6(4) . . . . ? N1A Cd1 O13A Cd2 176.8(4) . . . . ? O17A Cd1 O13A Cd2 170.7(3) . . . . ? N21C Cd1 O13A Cd2 -97.1(4) 4_565 . . . ? O14C Cd1 O13A Cd2 -18.6(5) . . . . ? O13C Cd1 O13A Cd2 -3.6(4) . . . . ? C12C Cd1 O13A Cd2 -8.5(4) . . . . ? N21D Cd2 O13A C12A 81.2(3) . . . . ? N21B Cd2 O13A C12A -87.6(3) 3_557 . . . ? N1B Cd2 O13A C12A 171.2(4) . . . . ? O13B Cd2 O13A C12A 170.8(3) . . . . ? O17B Cd2 O13A C12A -14.1(4) . . . . ? O14A Cd2 O13A C12A 0.3(3) . . . . ? N21D Cd2 O13A Cd1 -92.6(4) . . . . ? N21B Cd2 O13A Cd1 98.7(4) 3_557 . . . ? N1B Cd2 O13A Cd1 -2.6(6) . . . . ? O13B Cd2 O13A Cd1 -3.0(4) . . . . ? O17B Cd2 O13A Cd1 172.1(3) . . . . ? O14A Cd2 O13A Cd1 -173.5(4) . . . . ? O14B C12B O13B Cd2 176.7(4) . . . . ? C2B C12B O13B Cd2 -4.0(6) . . . . ? Cd3 C12B O13B Cd2 -179.3(3) . . . . ? O14B C12B O13B Cd3 -4.0(5) . . . . ? C2B C12B O13B Cd3 175.3(5) . . . . ? N21D Cd2 O13B C12B -79.6(4) . . . . ? N21B Cd2 O13B C12B 103.7(4) 3_557 . . . ? N1B Cd2 O13B C12B 6.2(4) . . . . ? O13A Cd2 O13B C12B -174.0(4) . . . . ? O17B Cd2 O13B C12B 10.8(5) . . . . ? O14A Cd2 O13B C12B -162.0(4) . . . . ? N21D Cd2 O13B Cd3 102.1(5) . . . . ? N21B Cd2 O13B Cd3 -74.7(5) 3_557 . . . ? N1B Cd2 O13B Cd3 -172.2(5) . . . . ? O13A Cd2 O13B Cd3 7.6(5) . . . . ? O17B Cd2 O13B Cd3 -167.6(4) . . . . ? O14A Cd2 O13B Cd3 19.6(6) . . . . ? O42 Cd3 O13B C12B -89.8(3) . . . . ? O14B Cd3 O13B C12B 2.2(3) . . . . ? N21A Cd3 O13B C12B 86.0(3) 4_666 . . . ? N1C Cd3 O13B C12B -162.4(4) . . . . ? O13C Cd3 O13B C12B 179.6(3) . . . . ? O17C Cd3 O13B C12B -13.7(4) . . . . ? O42 Cd3 O13B Cd2 88.8(5) . . . . ? O14B Cd3 O13B Cd2 -179.2(5) . . . . ? N21A Cd3 O13B Cd2 -95.5(5) 4_666 . . . ? N1C Cd3 O13B Cd2 16.1(7) . . . . ? O13C Cd3 O13B Cd2 -1.9(5) . . . . ? O17C Cd3 O13B Cd2 164.9(4) . . . . ? C12B Cd3 O13B Cd2 178.6(7) . . . . ? O14C C12C O13C Cd3 176.2(4) . . . . ? C2C C12C O13C Cd3 -5.2(7) . . . . ? Cd1 C12C O13C Cd3 174.0(4) . . . . ? O14C C12C O13C Cd1 2.2(6) . . . . ? C2C C12C O13C Cd1 -179.2(5) . . . . ? O42 Cd3 O13C C12C 93.3(4) . . . . ? O14B Cd3 O13C C12C 177.3(4) . . . . ? N21A Cd3 O13C C12C -87.8(4) 4_666 . . . ? N1C Cd3 O13C C12C 3.2(4) . . . . ? O17C Cd3 O13C C12C 7.1(5) . . . . ? O13B Cd3 O13C C12C 174.2(4) . . . . ? C12B Cd3 O13C C12C 174.4(4) . . . . ? O42 Cd3 O13C Cd1 -99.2(4) . . . . ? O14B Cd3 O13C Cd1 -15.3(6) . . . . ? N21A Cd3 O13C Cd1 79.7(4) 4_666 . . . ? N1C Cd3 O13C Cd1 170.7(5) . . . . ? O17C Cd3 O13C Cd1 174.6(3) . . . . ? O13B Cd3 O13C Cd1 -18.4(4) . . . . ? C12B Cd3 O13C Cd1 -18.2(5) . . . . ? O31 Cd1 O13C C12C 85.6(4) . . . . ? N1A Cd1 O13C C12C -169.3(4) . . . . ? O13A Cd1 O13C C12C -170.7(3) . . . . ? O17A Cd1 O13C C12C 14.4(4) . . . . ? N21C Cd1 O13C C12C -79.6(4) 4_565 . . . ? O14C Cd1 O13C C12C -1.2(3) . . . . ? O31 Cd1 O13C Cd3 -83.4(5) . . . . ? N1A Cd1 O13C Cd3 21.7(8) . . . . ? O13A Cd1 O13C Cd3 20.3(4) . . . . ? O17A Cd1 O13C Cd3 -154.6(4) . . . . ? N21C Cd1 O13C Cd3 111.4(4) 4_565 . . . ? O14C Cd1 O13C Cd3 -170.2(5) . . . . ? C12C Cd1 O13C Cd3 -169.0(7) . . . . ? O13A C12A O14A Cd2 0.5(6) . . . . ? C2A C12A O14A Cd2 -178.5(4) . . . . ? N21D Cd2 O14A C12A -99.2(3) . . . . ? N21B Cd2 O14A C12A 85.3(3) 3_557 . . . ? N1B Cd2 O14A C12A -172.9(3) . . . . ? O13B Cd2 O14A C12A -15.1(4) . . . . ? O13A Cd2 O14A C12A -0.3(3) . . . . ? O17B Cd2 O14A C12A 169.9(3) . . . . ? O13B C12B O14B Cd3 4.4(6) . . . . ? C2B C12B O14B Cd3 -174.9(4) . . . . ? O42 Cd3 O14B C12B 79.2(4) . . . . ? N21A Cd3 O14B C12B -102.8(4) 4_666 . . . ? N1C Cd3 O14B C12B 161.7(4) . . . . ? O13C Cd3 O14B C12B -6.1(5) . . . . ? O17C Cd3 O14B C12B 167.2(4) . . . . ? O13B Cd3 O14B C12B -2.2(3) . . . . ? O13C C12C O14C Cd1 -2.3(6) . . . . ? C2C C12C O14C Cd1 179.2(5) . . . . ? O31 Cd1 O14C C12C -80.1(4) . . . . ? N1A Cd1 O14C C12C 174.7(3) . . . . ? O13A Cd1 O14C C12C 19.7(5) . . . . ? O17A Cd1 O14C C12C -166.8(4) . . . . ? N21C Cd1 O14C C12C 100.8(4) 4_565 . . . ? O13C Cd1 O14C C12C 1.2(3) . . . . ? O13D C12D O14D C15D 0.9(17) . . . . ? C2D C12D O14D C15D -177.8(9) . . . . ? N1A C6A C16A O17A 12.3(7) . . . . ? C5A C6A C16A O17A -166.7(6) . . . . ? N1A C6A C16A N18A -168.1(5) . . . . ? C5A C6A C16A N18A 12.9(8) . . . . ? N1B C6B C16B O17B 9.4(8) . . . . ? C5B C6B C16B O17B -170.1(6) . . . . ? N1B C6B C16B N18B -169.8(5) . . . . ? C5B C6B C16B N18B 10.6(9) . . . . ? N1C C6C C16C O17C -10.4(8) . . . . ? C5C C6C C16C O17C 171.9(7) . . . . ? N1C C6C C16C N18C 169.3(5) . . . . ? C5C C6C C16C N18C -8.5(9) . . . . ? N1D C6D C16D O17D -169.8(7) . . . . ? C5D C6D C16D O17D 6.1(11) . . . . ? N1D C6D C16D N18D 7.6(10) . . . . ? C5D C6D C16D N18D -176.5(8) . . . . ? N18A C16A O17A Cd1 160.8(4) . . . . ? C6A C16A O17A Cd1 -19.7(6) . . . . ? O31 Cd1 O17A C16A 125.1(4) . . . . ? N1A Cd1 O17A C16A 14.4(4) . . . . ? O13A Cd1 O17A C16A 20.6(5) . . . . ? N21C Cd1 O17A C16A -71.7(4) 4_565 . . . ? O14C Cd1 O17A C16A -154.0(4) . . . . ? O13C Cd1 O17A C16A -166.9(4) . . . . ? C12C Cd1 O17A C16A -160.1(4) . . . . ? N18B C16B O17B Cd2 172.5(4) . . . . ? C6B C16B O17B Cd2 -6.7(7) . . . . ? N21D Cd2 O17B C16B 87.5(4) . . . . ? N21B Cd2 O17B C16B -102.5(4) 3_557 . . . ? N1B Cd2 O17B C16B 2.0(4) . . . . ? O13B Cd2 O17B C16B -2.6(5) . . . . ? O13A Cd2 O17B C16B -175.6(4) . . . . ? O14A Cd2 O17B C16B 172.7(4) . . . . ? N18C C16C O17C Cd3 -168.5(4) . . . . ? C6C C16C O17C Cd3 11.2(7) . . . . ? O42 Cd3 O17C C16C -97.3(5) . . . . ? O14B Cd3 O17C C16C 176.3(4) . . . . ? N21A Cd3 O17C C16C 86.3(4) 4_666 . . . ? N1C Cd3 O17C C16C -6.4(4) . . . . ? O13C Cd3 O17C C16C -10.4(5) . . . . ? O13B Cd3 O17C C16C -170.9(4) . . . . ? C12B Cd3 O17C C16C -177.5(4) . . . . ? O17A C16A N18A C19A 0.8(8) . . . . ? C6A C16A N18A C19A -178.7(5) . . . . ? O17B C16B N18B C19B -0.6(9) . . . . ? C6B C16B N18B C19B 178.6(5) . . . . ? O17C C16C N18C C19C 1.0(9) . . . . ? C6C C16C N18C C19C -178.7(5) . . . . ? O17D C16D N18D C19D 1.7(13) . . . . ? C6D C16D N18D C19D -175.6(7) . . . . ? C16A N18A C19A C24A -88.4(7) . . . . ? C16B N18B C19B C24B -87.0(8) . . . . ? C16C N18C C19C C24C 83.0(7) . . . . ? C16D N18D C19D C24D -86.2(12) . . . . ? N21B Cd2 N21D C22D 138.4(11) 3_557 . . . ? N1B Cd2 N21D C22D -94.2(7) . . . . ? O13B Cd2 N21D C22D -25.3(7) . . . . ? O13A Cd2 N21D C22D 61.5(7) . . . . ? O17B Cd2 N21D C22D -161.2(7) . . . . ? O14A Cd2 N21D C22D 114.8(7) . . . . ? N21B Cd2 N21D C26D -51.0(13) 3_557 . . . ? N1B Cd2 N21D C26D 76.5(5) . . . . ? O13B Cd2 N21D C26D 145.3(5) . . . . ? O13A Cd2 N21D C26D -127.9(5) . . . . ? O17B Cd2 N21D C26D 9.5(5) . . . . ? O14A Cd2 N21D C26D -74.5(5) . . . . ? C26A N21A C22A C23A -6.6(19) . . . . ? Cd3 N21A C22A C23A 168.4(11) 4_565 . . . ? C26B N21B C22B C23B 1.3(18) . . . . ? Cd2 N21B C22B C23B -173.9(10) 3_557 . . . ? C26C N21C C22C C23C 4.4(17) . . . . ? Cd1 N21C C22C C23C -176.8(9) 4_666 . . . ? C26D N21D C22D C23D -3.4(14) . . . . ? Cd2 N21D C22D C23D 167.3(9) . . . . ? N21A C22A C23A C24A 0(2) . . . . ? N21B C22B C23B C24B -2(2) . . . . ? N21C C22C C23C C24C -0.2(18) . . . . ? N21D C22D C23D C24D 1.5(18) . . . . ? C22A C23A C24A C25A 6.2(17) . . . . ? C22A C23A C24A C19A -178.1(11) . . . . ? N18A C19A C24A C23A 75.2(11) . . . . ? N18A C19A C24A C25A -109.3(8) . . . . ? C22B C23B C24B C25B 1.4(17) . . . . ? C22B C23B C24B C19B -178.1(11) . . . . ? N18B C19B C24B C25B 18.6(10) . . . . ? N18B C19B C24B C23B -162.0(9) . . . . ? C22C C23C C24C C25C -2.9(16) . . . . ? C22C C23C C24C C19C 179.8(9) . . . . ? N18C C19C C24C C23C -105.3(9) . . . . ? N18C C19C C24C C25C 77.4(11) . . . . ? C22D C23D C24D C25D 1.1(18) . . . . ? C22D C23D C24D C19D 179.5(11) . . . . ? N18D C19D C24D C25D -132.2(11) . . . . ? N18D C19D C24D C23D 49.4(16) . . . . ? C23A C24A C25A C26A -6.7(14) . . . . ? C19A C24A C25A C26A 177.4(8) . . . . ? C23B C24B C25B C26B -0.4(13) . . . . ? C19B C24B C25B C26B 179.1(8) . . . . ? C23C C24C C25C C26C 1.7(19) . . . . ? C19C C24C C25C C26C 179.0(11) . . . . ? C23D C24D C25D C26D -1.6(15) . . . . ? C19D C24D C25D C26D 179.9(9) . . . . ? C22A N21A C26A C25A 6.1(14) . . . . ? Cd3 N21A C26A C25A -169.2(7) 4_565 . . . ? C24A C25A C26A N21A 0.6(15) . . . . ? C22B N21B C26B C25B -0.3(14) . . . . ? Cd2 N21B C26B C25B 175.1(7) 3_557 . . . ? C24B C25B C26B N21B -0.2(14) . . . . ? C22C N21C C26C C25C -6(2) . . . . ? Cd1 N21C C26C C25C 175.4(12) 4_666 . . . ? C24C C25C C26C N21C 3(2) . . . . ? C24D C25D C26D N21D -0.4(13) . . . . ? C22D N21D C26D C25D 2.9(12) . . . . ? Cd2 N21D C26D C25D -168.0(6) . . . . ? O33 N30 O31 Cd1 -172.4(8) . . . . ? O32 N30 O31 Cd1 10.2(11) . . . . ? N1A Cd1 O31 N30 -39.0(6) . . . . ? O13A Cd1 O31 N30 33.0(6) . . . . ? O17A Cd1 O31 N30 -104.0(6) . . . . ? N21C Cd1 O31 N30 -179.7(6) 4_565 . . . ? O14C Cd1 O31 N30 177.4(6) . . . . ? O13C Cd1 O31 N30 121.9(6) . . . . ? C12C Cd1 O31 N30 150.1(6) . . . . ? O14B Cd3 O42 C43 -154.1(9) . . . . ? N21A Cd3 O42 C43 178(100) 4_666 . . . ? N1C Cd3 O42 C43 52.9(9) . . . . ? O13C Cd3 O42 C43 -16.6(9) . . . . ? O17C Cd3 O42 C43 120.5(9) . . . . ? O13B Cd3 O42 C43 -100.0(9) . . . . ? C12B Cd3 O42 C43 -127.5(9) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.826 _refine_diff_density_min -1.330 _refine_diff_density_rms 0.153 ######END