# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 1350 _publ_requested_journal CrystEngComm _publ_section_title ; Substituent effect of R-isophthalates (R = CH, CCH3, COCH3, CtBu, COH, and CNO2) on the construction of CdII coordination polymers incorporating a dipyridyl tecton 2,5-bis(3-pyridyl)-1,3,4-oxadiazole ; _publ_contact_author ; Miao Du College of Chemistry, Tianjin Key Laboratory of Structure and Performance for Functional Molecule, Tianjin Normal University, Tianjin 300387, P. R. China ; _publ_contact_author_email dumiao@public.tpt.tj.cn loop_ _publ_author_name 'Chen, Jing' 'Li, Cheng-Peng' 'Du, Miao' data_1 _database_code_depnum_ccdc_archive 'CCDC 790241' #TrackingRef '- CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H32 Cd2 N8 O14' _chemical_formula_weight 1073.54 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.309(4) _cell_length_b 13.977(5) _cell_length_c 15.650(6) _cell_angle_alpha 71.099(6) _cell_angle_beta 84.320(5) _cell_angle_gamma 72.490(6) _cell_volume 2034.6(13) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 884 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 26.36 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 1.752 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1072 _exptl_absorpt_coefficient_mu 1.126 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.799398 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'APEX II CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11838 _diffrn_reflns_av_R_equivalents 0.0214 _diffrn_reflns_av_sigmaI/netI 0.0433 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 26.39 _reflns_number_total 8242 _reflns_number_gt 6226 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX II' _computing_cell_refinement 'Bruker APEX II' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0451P)^2^+0.8547P] 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 8242 _refine_ls_number_parameters 596 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0554 _refine_ls_R_factor_gt 0.0346 _refine_ls_wR_factor_ref 0.0987 _refine_ls_wR_factor_gt 0.0810 _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_restrained_S_all 1.101 _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 0.50433(3) 0.43610(2) 0.331404(19) 0.03075(9) Uani 1 1 d . . . Cd2 Cd 0.03882(3) 0.12126(2) 0.196096(19) 0.03273(9) Uani 1 1 d . . . N1 N 0.5115(3) 0.3124(3) 0.4744(2) 0.0331(7) Uani 1 1 d . . . N2 N 0.4297(4) -0.0220(3) 0.6366(2) 0.0516(10) Uani 1 1 d . . . N3 N 0.3539(4) -0.0780(3) 0.6135(2) 0.0482(9) Uani 1 1 d . . . N4 N 0.0902(3) 0.0053(3) 0.3461(2) 0.0365(8) Uani 1 1 d . . . N5 N 0.4539(3) 0.5477(3) 0.1780(2) 0.0365(8) Uani 1 1 d . . . N6 N 0.2721(4) 0.5912(3) -0.1115(2) 0.0408(8) Uani 1 1 d . . . N7 N 0.1971(4) 0.5348(3) -0.1352(2) 0.0417(8) Uani 1 1 d . . . N8 N 0.0260(3) 0.2464(3) 0.0516(2) 0.0363(8) Uani 1 1 d . . . O1 O 0.3147(3) 0.0783(2) 0.51223(17) 0.0357(6) Uani 1 1 d . . . O2 O 0.2283(3) 0.4742(2) 0.01237(17) 0.0343(6) Uani 1 1 d . . . O3 O 0.6318(3) 0.5279(3) 0.3469(2) 0.0511(8) Uani 1 1 d . . . O4 O 0.7976(3) 0.3792(2) 0.3637(2) 0.0503(8) Uani 1 1 d . . . O5 O 1.2787(3) 0.4246(2) 0.3318(2) 0.0395(7) Uani 1 1 d . . . O6 O 1.3044(3) 0.5547(2) 0.3712(2) 0.0467(8) Uani 1 1 d . . . O7 O 0.2435(3) 0.0238(3) 0.1514(2) 0.0563(9) Uani 1 1 d . . . O8 O 0.2866(3) 0.1494(3) 0.1866(2) 0.0570(9) Uani 1 1 d . . . O9 O 0.7850(3) 0.1506(2) 0.1819(2) 0.0501(8) Uani 1 1 d . . . O10 O 0.9376(3) 0.0085(2) 0.1675(2) 0.0531(9) Uani 1 1 d . . . O11 O 0.5803(3) 0.3007(2) 0.26556(19) 0.0429(7) Uani 1 1 d . . . H11A H 0.6072 0.2369 0.2988 0.064 Uiso 1 1 d R . . H11B H 0.6300 0.3117 0.2188 0.064 Uiso 1 1 d R . . O12 O -0.0098(3) 0.2514(2) 0.2639(2) 0.0493(8) Uani 1 1 d . . . H12A H -0.0824 0.3008 0.2632 0.074 Uiso 1 1 d R . . H12B H 0.0553 0.2610 0.2863 0.074 Uiso 1 1 d R . . C1 C 0.4529(4) 0.2357(3) 0.4864(3) 0.0331(9) Uani 1 1 d . . . H1 H 0.4049 0.2365 0.4387 0.040 Uiso 1 1 calc R . . C2 C 0.4609(4) 0.1553(3) 0.5669(3) 0.0331(9) Uani 1 1 d . . . C3 C 0.5310(4) 0.1552(4) 0.6389(3) 0.0431(10) Uani 1 1 d . . . H3 H 0.5395 0.1016 0.6938 0.052 Uiso 1 1 calc R . . C4 C 0.5870(4) 0.2360(4) 0.6269(3) 0.0452(11) Uani 1 1 d . . . H4 H 0.6314 0.2394 0.6743 0.054 Uiso 1 1 calc R . . C5 C 0.5768(4) 0.3118(4) 0.5443(3) 0.0390(10) Uani 1 1 d . . . H5 H 0.6172 0.3652 0.5365 0.047 Uiso 1 1 calc R . . C6 C 0.4034(4) 0.0687(3) 0.5756(3) 0.0350(9) Uani 1 1 d . . . C7 C 0.2885(4) -0.0170(3) 0.5406(3) 0.0355(9) Uani 1 1 d . . . C8 C 0.1643(4) 0.0255(3) 0.3992(3) 0.0358(9) Uani 1 1 d . . . H8 H 0.1920 0.0865 0.3771 0.043 Uiso 1 1 calc R . . C9 C 0.2024(4) -0.0400(3) 0.4863(3) 0.0337(9) Uani 1 1 d . . . C10 C 0.1591(4) -0.1311(3) 0.5198(3) 0.0428(10) Uani 1 1 d . . . H10 H 0.1818 -0.1767 0.5779 0.051 Uiso 1 1 calc R . . C11 C 0.0819(5) -0.1513(3) 0.4646(3) 0.0461(11) Uani 1 1 d . . . H11 H 0.0514 -0.2111 0.4851 0.055 Uiso 1 1 calc R . . C12 C 0.0502(4) -0.0829(3) 0.3792(3) 0.0410(10) Uani 1 1 d . . . H12 H -0.0012 -0.0983 0.3426 0.049 Uiso 1 1 calc R . . C13 C 0.3863(4) 0.5237(3) 0.1231(3) 0.0338(9) Uani 1 1 d . . . H13 H 0.3555 0.4641 0.1461 0.041 Uiso 1 1 calc R . . C14 C 0.3597(4) 0.5834(3) 0.0333(3) 0.0328(9) Uani 1 1 d . . . C15 C 0.4048(4) 0.6728(3) -0.0007(3) 0.0430(10) Uani 1 1 d . . . H15 H 0.3885 0.7149 -0.0605 0.052 Uiso 1 1 calc R . . C16 C 0.4742(5) 0.6974(3) 0.0563(3) 0.0493(11) Uani 1 1 d . . . H16 H 0.5057 0.7568 0.0353 0.059 Uiso 1 1 calc R . . C17 C 0.4965(4) 0.6342(3) 0.1435(3) 0.0435(10) Uani 1 1 d . . . H17 H 0.5436 0.6520 0.1810 0.052 Uiso 1 1 calc R . . C18 C 0.2881(4) 0.5536(3) -0.0248(3) 0.0327(9) Uani 1 1 d . . . C19 C 0.1728(4) 0.4682(3) -0.0609(3) 0.0322(8) Uani 1 1 d . . . C20 C 0.0905(4) 0.3200(3) 0.0369(3) 0.0337(9) Uani 1 1 d . . . H20 H 0.1309 0.3245 0.0855 0.040 Uiso 1 1 calc R . . C21 C 0.0995(4) 0.3899(3) -0.0480(3) 0.0316(8) Uani 1 1 d . . . C22 C 0.0373(5) 0.3840(4) -0.1199(3) 0.0460(11) Uani 1 1 d . . . H22 H 0.0406 0.4304 -0.1776 0.055 Uiso 1 1 calc R . . C23 C -0.0292(5) 0.3086(4) -0.1044(3) 0.0458(11) Uani 1 1 d . . . H23 H -0.0715 0.3031 -0.1517 0.055 Uiso 1 1 calc R . . C24 C -0.0330(4) 0.2411(3) -0.0183(3) 0.0398(10) Uani 1 1 d . . . H24 H -0.0784 0.1901 -0.0084 0.048 Uiso 1 1 calc R . . C25 C 0.7554(4) 0.4734(3) 0.3585(3) 0.0361(9) Uani 1 1 d . . . C26 C 0.8522(4) 0.5340(3) 0.3640(3) 0.0358(9) Uani 1 1 d . . . C27 C 0.9915(4) 0.4906(3) 0.3637(2) 0.0304(8) Uani 1 1 d . . . H27 H 1.0274 0.4211 0.3638 0.036 Uiso 1 1 calc R . . C28 C 1.0785(4) 0.5498(3) 0.3631(3) 0.0358(9) Uani 1 1 d . . . C29 C 1.0256(5) 0.6517(4) 0.3639(5) 0.0777(19) Uani 1 1 d . . . H29 H 1.0837 0.6911 0.3644 0.093 Uiso 1 1 calc R . . C30 C 0.8873(5) 0.6962(5) 0.3641(6) 0.122(3) Uani 1 1 d . . . H30 H 0.8518 0.7655 0.3645 0.147 Uiso 1 1 calc R . . C31 C 0.8018(5) 0.6377(4) 0.3635(5) 0.081(2) Uani 1 1 d . . . H31 H 0.7082 0.6685 0.3628 0.097 Uiso 1 1 calc R . . C32 C 1.2292(4) 0.5063(3) 0.3567(3) 0.0332(9) Uani 1 1 d . . . C33 C 0.3248(4) 0.0706(3) 0.1601(3) 0.0377(9) Uani 1 1 d . . . C34 C 0.4728(4) 0.0273(3) 0.1406(3) 0.0315(8) Uani 1 1 d . . . C35 C 0.5711(4) 0.0692(3) 0.1564(2) 0.0291(8) Uani 1 1 d . . . H35 H 0.5442 0.1292 0.1750 0.035 Uiso 1 1 calc R . . C36 C 0.7082(4) 0.0237(3) 0.1451(3) 0.0346(9) Uani 1 1 d . . . C37 C 0.7471(4) -0.0650(4) 0.1163(4) 0.0573(14) Uani 1 1 d . . . H37 H 0.8389 -0.0965 0.1084 0.069 Uiso 1 1 calc R . . C38 C 0.6503(5) -0.1067(4) 0.0993(4) 0.0678(16) Uani 1 1 d . . . H38 H 0.6771 -0.1656 0.0793 0.081 Uiso 1 1 calc R . . C39 C 0.5141(4) -0.0612(4) 0.1119(3) 0.0503(12) Uani 1 1 d . . . H39 H 0.4495 -0.0901 0.1010 0.060 Uiso 1 1 calc R . . C40 C 0.8159(4) 0.0646(3) 0.1668(3) 0.0369(9) Uani 1 1 d . . . O13 O 0.1733(8) 0.8386(8) 0.1664(14) 0.092(4) Uani 0.69(3) 1 d PU . . O13' O 0.1652(18) 0.872(2) 0.109(2) 0.080(7) Uani 0.31(3) 1 d PU . . O14 O 0.2049(7) 0.3298(6) 0.2315(5) 0.0557(17) Uani 0.50 1 d PU . . O14' O 0.2285(7) 0.2620(6) 0.3039(6) 0.0650(19) Uani 0.50 1 d PU . . 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 0.02344(15) 0.03161(16) 0.03979(18) -0.01137(13) -0.00214(11) -0.01059(12) Cd2 0.02782(16) 0.03472(17) 0.03907(18) -0.01155(14) -0.00102(12) -0.01340(12) N1 0.0301(17) 0.0387(19) 0.0338(18) -0.0129(15) -0.0026(13) -0.0119(14) N2 0.077(3) 0.038(2) 0.036(2) -0.0049(17) -0.0140(19) -0.014(2) N3 0.076(3) 0.033(2) 0.033(2) -0.0050(17) -0.0072(18) -0.0167(19) N4 0.0404(19) 0.0306(18) 0.0402(19) -0.0106(15) -0.0004(15) -0.0128(15) N5 0.0330(17) 0.0361(19) 0.0412(19) -0.0112(16) -0.0047(14) -0.0104(15) N6 0.045(2) 0.039(2) 0.039(2) -0.0091(17) 0.0008(16) -0.0184(16) N7 0.049(2) 0.041(2) 0.0339(19) -0.0064(16) -0.0032(16) -0.0153(17) N8 0.0353(18) 0.0416(19) 0.0376(19) -0.0145(16) -0.0006(14) -0.0162(15) O1 0.0403(16) 0.0279(14) 0.0342(15) -0.0022(12) -0.0057(12) -0.0093(12) O2 0.0371(15) 0.0374(15) 0.0296(14) -0.0060(12) -0.0015(11) -0.0166(12) O3 0.0269(16) 0.060(2) 0.078(2) -0.0295(18) -0.0041(14) -0.0182(14) O4 0.0453(18) 0.0453(19) 0.068(2) -0.0174(17) 0.0032(15) -0.0252(15) O5 0.0242(13) 0.0441(17) 0.0615(19) -0.0299(15) -0.0003(12) -0.0111(12) O6 0.0252(14) 0.060(2) 0.075(2) -0.0431(18) -0.0006(13) -0.0163(13) O7 0.0285(16) 0.065(2) 0.086(2) -0.0312(19) 0.0093(15) -0.0233(15) O8 0.0340(17) 0.065(2) 0.079(2) -0.042(2) -0.0100(15) 0.0016(15) O9 0.0410(17) 0.0484(19) 0.074(2) -0.0280(17) 0.0019(15) -0.0224(15) O10 0.0206(14) 0.057(2) 0.095(3) -0.0372(19) -0.0061(15) -0.0135(14) O11 0.0543(18) 0.0316(15) 0.0405(16) -0.0106(13) 0.0099(13) -0.0128(13) O12 0.0430(17) 0.0423(17) 0.065(2) -0.0266(16) -0.0064(15) -0.0031(14) C1 0.031(2) 0.038(2) 0.032(2) -0.0124(18) -0.0028(16) -0.0101(17) C2 0.033(2) 0.035(2) 0.028(2) -0.0111(18) -0.0001(16) -0.0050(17) C3 0.048(3) 0.043(3) 0.030(2) -0.008(2) -0.0058(19) -0.005(2) C4 0.041(2) 0.062(3) 0.040(3) -0.026(2) -0.0090(19) -0.011(2) C5 0.032(2) 0.050(3) 0.043(3) -0.024(2) 0.0001(18) -0.0134(19) C6 0.040(2) 0.034(2) 0.028(2) -0.0111(18) -0.0010(17) -0.0041(18) C7 0.042(2) 0.028(2) 0.035(2) -0.0099(18) 0.0089(18) -0.0098(17) C8 0.040(2) 0.026(2) 0.039(2) -0.0075(18) 0.0038(18) -0.0100(17) C9 0.035(2) 0.027(2) 0.038(2) -0.0123(18) 0.0071(17) -0.0079(16) C10 0.050(3) 0.031(2) 0.043(2) -0.010(2) 0.011(2) -0.0109(19) C11 0.052(3) 0.034(2) 0.055(3) -0.010(2) 0.009(2) -0.023(2) C12 0.040(2) 0.035(2) 0.052(3) -0.018(2) 0.005(2) -0.0137(19) C13 0.030(2) 0.032(2) 0.041(2) -0.0086(18) 0.0015(16) -0.0144(17) C14 0.0257(19) 0.031(2) 0.041(2) -0.0115(18) 0.0012(16) -0.0060(16) C15 0.051(3) 0.036(2) 0.041(2) -0.004(2) -0.004(2) -0.017(2) C16 0.059(3) 0.035(2) 0.059(3) -0.010(2) -0.004(2) -0.025(2) C17 0.044(2) 0.038(2) 0.054(3) -0.014(2) -0.006(2) -0.017(2) C18 0.029(2) 0.028(2) 0.039(2) -0.0074(18) 0.0021(16) -0.0087(16) C19 0.032(2) 0.034(2) 0.028(2) -0.0079(17) -0.0039(16) -0.0063(17) C20 0.034(2) 0.036(2) 0.032(2) -0.0091(18) -0.0025(16) -0.0124(17) C21 0.0282(19) 0.036(2) 0.030(2) -0.0108(17) 0.0002(15) -0.0081(16) C22 0.052(3) 0.055(3) 0.032(2) -0.013(2) -0.0023(19) -0.017(2) C23 0.052(3) 0.061(3) 0.036(2) -0.022(2) -0.008(2) -0.022(2) C24 0.033(2) 0.045(2) 0.050(3) -0.024(2) 0.0017(19) -0.0151(19) C25 0.028(2) 0.048(3) 0.038(2) -0.014(2) 0.0003(16) -0.0191(19) C26 0.0208(18) 0.044(2) 0.052(3) -0.023(2) -0.0017(16) -0.0124(17) C27 0.0252(18) 0.034(2) 0.036(2) -0.0129(17) -0.0017(15) -0.0122(16) C28 0.0227(19) 0.046(2) 0.051(2) -0.028(2) 0.0012(17) -0.0129(17) C29 0.029(2) 0.069(3) 0.170(6) -0.081(4) 0.009(3) -0.020(2) C30 0.031(3) 0.085(4) 0.303(11) -0.135(6) 0.017(4) -0.016(3) C31 0.024(2) 0.076(4) 0.175(6) -0.081(4) 0.008(3) -0.016(2) C32 0.0267(19) 0.042(2) 0.038(2) -0.0150(19) -0.0028(16) -0.0153(17) C33 0.028(2) 0.045(3) 0.035(2) -0.0109(19) -0.0031(16) -0.0047(18) C34 0.0263(19) 0.038(2) 0.032(2) -0.0099(18) -0.0011(15) -0.0121(16) C35 0.0305(19) 0.029(2) 0.030(2) -0.0113(16) 0.0006(15) -0.0109(16) C36 0.0265(19) 0.041(2) 0.041(2) -0.0160(19) 0.0019(16) -0.0140(17) C37 0.023(2) 0.069(3) 0.098(4) -0.055(3) 0.006(2) -0.010(2) C38 0.034(2) 0.076(4) 0.125(5) -0.076(4) 0.004(3) -0.014(2) C39 0.031(2) 0.061(3) 0.079(3) -0.044(3) 0.004(2) -0.019(2) C40 0.031(2) 0.044(2) 0.041(2) -0.012(2) 0.0004(17) -0.0188(19) O13 0.092(5) 0.069(5) 0.120(9) -0.032(5) -0.003(5) -0.025(4) O13' 0.082(9) 0.083(10) 0.097(12) -0.055(8) 0.000(7) -0.028(6) O14 0.060(4) 0.063(4) 0.064(4) -0.030(4) -0.006(3) -0.032(3) O14' 0.070(4) 0.064(4) 0.085(5) -0.039(4) 0.003(4) -0.037(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O3 2.170(3) . ? Cd1 N1 2.335(3) . ? Cd1 O11 2.338(3) . ? Cd1 O5 2.378(3) 1_455 ? Cd1 O6 2.397(3) 1_455 ? Cd1 N5 2.408(3) . ? Cd1 C32 2.742(4) 1_455 ? Cd2 O12 2.298(3) . ? Cd2 O10 2.305(3) 1_455 ? Cd2 O7 2.322(3) . ? Cd2 N8 2.355(3) . ? Cd2 N4 2.383(3) . ? Cd2 O9 2.545(3) 1_455 ? N1 C1 1.337(5) . ? N1 C5 1.337(5) . ? N2 C6 1.285(5) . ? N2 N3 1.402(5) . ? N3 C7 1.289(5) . ? N4 C8 1.328(5) . ? N4 C12 1.345(5) . ? N5 C13 1.336(5) . ? N5 C17 1.340(5) . ? N6 C18 1.294(5) . ? N6 N7 1.402(5) . ? N7 C19 1.290(5) . ? N8 C20 1.335(5) . ? N8 C24 1.335(5) . ? O1 C7 1.362(5) . ? O1 C6 1.363(5) . ? O2 C18 1.367(4) . ? O2 C19 1.368(4) . ? O3 C25 1.268(5) . ? O4 C25 1.234(5) . ? O5 C32 1.270(5) . ? O5 Cd1 2.378(3) 1_655 ? O6 C32 1.250(4) . ? O6 Cd1 2.397(3) 1_655 ? O7 C33 1.249(5) . ? O8 C33 1.242(5) . ? O9 C40 1.240(5) . ? O9 Cd2 2.545(3) 1_655 ? O10 C40 1.263(5) . ? O10 Cd2 2.305(3) 1_655 ? O11 H11A 0.8500 . ? O11 H11B 0.8499 . ? O12 H12A 0.8502 . ? O12 H12B 0.8509 . ? C1 C2 1.380(5) . ? C1 H1 0.9300 . ? C2 C3 1.399(6) . ? C2 C6 1.463(6) . ? C3 C4 1.370(6) . ? C3 H3 0.9300 . ? C4 C5 1.370(6) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C7 C9 1.453(6) . ? C8 C9 1.389(5) . ? C8 H8 0.9300 . ? C9 C10 1.399(5) . ? C10 C11 1.374(6) . ? C10 H10 0.9300 . ? C11 C12 1.370(6) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.387(5) . ? C13 H13 0.9300 . ? C14 C15 1.389(5) . ? C14 C18 1.453(5) . ? C15 C16 1.379(6) . ? C15 H15 0.9300 . ? C16 C17 1.362(6) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C19 C21 1.461(5) . ? C20 C21 1.385(5) . ? C20 H20 0.9300 . ? C21 C22 1.386(6) . ? C22 C23 1.369(6) . ? C22 H22 0.9300 . ? C23 C24 1.378(6) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 C26 1.515(5) . ? C26 C27 1.380(5) . ? C26 C31 1.383(6) . ? C27 C28 1.389(5) . ? C27 H27 0.9300 . ? C28 C29 1.367(6) . ? C28 C32 1.495(5) . ? C29 C30 1.373(7) . ? C29 H29 0.9300 . ? C30 C31 1.373(7) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C32 Cd1 2.742(4) 1_655 ? C33 C34 1.502(5) . ? C34 C39 1.385(6) . ? C34 C35 1.390(5) . ? C35 C36 1.384(5) . ? C35 H35 0.9300 . ? C36 C37 1.388(6) . ? C36 C40 1.503(5) . ? C37 C38 1.382(6) . ? C37 H37 0.9300 . ? C38 C39 1.380(6) . ? C38 H38 0.9300 . ? C39 H39 0.9300 . ? O13 O13' 0.86(2) . ? O14 O14' 1.209(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Cd1 N1 103.08(12) . . ? O3 Cd1 O11 123.29(11) . . ? N1 Cd1 O11 90.58(11) . . ? O3 Cd1 O5 146.16(11) . 1_455 ? N1 Cd1 O5 82.85(10) . 1_455 ? O11 Cd1 O5 89.49(10) . 1_455 ? O3 Cd1 O6 91.65(11) . 1_455 ? N1 Cd1 O6 91.16(11) . 1_455 ? O11 Cd1 O6 143.53(10) . 1_455 ? O5 Cd1 O6 54.67(9) 1_455 1_455 ? O3 Cd1 N5 90.52(12) . . ? N1 Cd1 N5 166.16(11) . . ? O11 Cd1 N5 83.92(11) . . ? O5 Cd1 N5 84.41(11) 1_455 . ? O6 Cd1 N5 85.85(11) 1_455 . ? O3 Cd1 C32 118.68(12) . 1_455 ? N1 Cd1 C32 86.94(11) . 1_455 ? O11 Cd1 C32 116.79(11) . 1_455 ? O5 Cd1 C32 27.57(10) 1_455 1_455 ? O6 Cd1 C32 27.10(10) 1_455 1_455 ? N5 Cd1 C32 84.26(11) . 1_455 ? O12 Cd2 O10 139.77(11) . 1_455 ? O12 Cd2 O7 131.59(11) . . ? O10 Cd2 O7 87.65(11) 1_455 . ? O12 Cd2 N8 91.30(11) . . ? O10 Cd2 N8 100.11(12) 1_455 . ? O7 Cd2 N8 87.64(12) . . ? O12 Cd2 N4 83.96(11) . . ? O10 Cd2 N4 90.19(12) 1_455 . ? O7 Cd2 N4 87.71(12) . . ? N8 Cd2 N4 168.51(11) . . ? O12 Cd2 O9 89.28(10) . 1_455 ? O10 Cd2 O9 53.49(10) 1_455 1_455 ? O7 Cd2 O9 138.86(11) . 1_455 ? N8 Cd2 O9 86.80(11) . 1_455 ? N4 Cd2 O9 103.56(11) . 1_455 ? C1 N1 C5 118.1(3) . . ? C1 N1 Cd1 118.9(2) . . ? C5 N1 Cd1 123.0(3) . . ? C6 N2 N3 105.9(3) . . ? C7 N3 N2 107.1(3) . . ? C8 N4 C12 117.7(4) . . ? C8 N4 Cd2 119.7(3) . . ? C12 N4 Cd2 122.6(3) . . ? C13 N5 C17 117.4(4) . . ? C13 N5 Cd1 121.1(3) . . ? C17 N5 Cd1 121.4(3) . . ? C18 N6 N7 106.9(3) . . ? C19 N7 N6 106.3(3) . . ? C20 N8 C24 118.4(4) . . ? C20 N8 Cd2 118.7(3) . . ? C24 N8 Cd2 122.6(3) . . ? C7 O1 C6 103.0(3) . . ? C18 O2 C19 102.9(3) . . ? C25 O3 Cd1 111.4(3) . . ? C32 O5 Cd1 92.4(2) . 1_655 ? C32 O6 Cd1 92.0(2) . 1_655 ? C33 O7 Cd2 102.3(3) . . ? C40 O9 Cd2 86.7(2) . 1_655 ? C40 O10 Cd2 97.4(2) . 1_655 ? Cd1 O11 H11A 119.9 . . ? Cd1 O11 H11B 116.9 . . ? H11A O11 H11B 110.8 . . ? Cd2 O12 H12A 130.1 . . ? Cd2 O12 H12B 118.5 . . ? H12A O12 H12B 110.5 . . ? N1 C1 C2 122.5(4) . . ? N1 C1 H1 118.8 . . ? C2 C1 H1 118.8 . . ? C1 C2 C3 118.6(4) . . ? C1 C2 C6 120.9(3) . . ? C3 C2 C6 120.4(4) . . ? C4 C3 C2 118.5(4) . . ? C4 C3 H3 120.8 . . ? C2 C3 H3 120.8 . . ? C5 C4 C3 119.3(4) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? N1 C5 C4 123.0(4) . . ? N1 C5 H5 118.5 . . ? C4 C5 H5 118.5 . . ? N2 C6 O1 112.5(4) . . ? N2 C6 C2 127.6(4) . . ? O1 C6 C2 119.9(3) . . ? N3 C7 O1 111.5(4) . . ? N3 C7 C9 128.8(4) . . ? O1 C7 C9 119.6(3) . . ? N4 C8 C9 123.2(4) . . ? N4 C8 H8 118.4 . . ? C9 C8 H8 118.4 . . ? C8 C9 C10 118.3(4) . . ? C8 C9 C7 121.3(3) . . ? C10 C9 C7 120.4(4) . . ? C11 C10 C9 118.2(4) . . ? C11 C10 H10 120.9 . . ? C9 C10 H10 120.9 . . ? C12 C11 C10 119.7(4) . . ? C12 C11 H11 120.2 . . ? C10 C11 H11 120.2 . . ? N4 C12 C11 123.0(4) . . ? N4 C12 H12 118.5 . . ? C11 C12 H12 118.5 . . ? N5 C13 C14 123.1(4) . . ? N5 C13 H13 118.5 . . ? C14 C13 H13 118.5 . . ? C13 C14 C15 118.3(4) . . ? C13 C14 C18 121.5(3) . . ? C15 C14 C18 120.1(4) . . ? C16 C15 C14 118.3(4) . . ? C16 C15 H15 120.8 . . ? C14 C15 H15 120.8 . . ? C17 C16 C15 119.6(4) . . ? C17 C16 H16 120.2 . . ? C15 C16 H16 120.2 . . ? N5 C17 C16 123.2(4) . . ? N5 C17 H17 118.4 . . ? C16 C17 H17 118.4 . . ? N6 C18 O2 111.7(3) . . ? N6 C18 C14 129.0(4) . . ? O2 C18 C14 119.3(3) . . ? N7 C19 O2 112.2(3) . . ? N7 C19 C21 128.5(4) . . ? O2 C19 C21 119.2(3) . . ? N8 C20 C21 122.4(4) . . ? N8 C20 H20 118.8 . . ? C21 C20 H20 118.8 . . ? C20 C21 C22 118.6(4) . . ? C20 C21 C19 120.4(3) . . ? C22 C21 C19 121.0(4) . . ? C23 C22 C21 118.7(4) . . ? C23 C22 H22 120.6 . . ? C21 C22 H22 120.6 . . ? C22 C23 C24 119.5(4) . . ? C22 C23 H23 120.3 . . ? C24 C23 H23 120.3 . . ? N8 C24 C23 122.3(4) . . ? N8 C24 H24 118.8 . . ? C23 C24 H24 118.8 . . ? O4 C25 O3 124.6(4) . . ? O4 C25 C26 120.9(4) . . ? O3 C25 C26 114.5(4) . . ? C27 C26 C31 118.4(4) . . ? C27 C26 C25 121.6(4) . . ? C31 C26 C25 119.9(4) . . ? C26 C27 C28 120.7(4) . . ? C26 C27 H27 119.6 . . ? C28 C27 H27 119.6 . . ? C29 C28 C27 119.6(4) . . ? C29 C28 C32 119.0(4) . . ? C27 C28 C32 121.3(4) . . ? C28 C29 C30 120.5(4) . . ? C28 C29 H29 119.8 . . ? C30 C29 H29 119.8 . . ? C31 C30 C29 119.7(5) . . ? C31 C30 H30 120.2 . . ? C29 C30 H30 120.2 . . ? C30 C31 C26 121.2(4) . . ? C30 C31 H31 119.4 . . ? C26 C31 H31 119.4 . . ? O6 C32 O5 120.9(3) . . ? O6 C32 C28 119.0(4) . . ? O5 C32 C28 120.0(3) . . ? O6 C32 Cd1 60.9(2) . 1_655 ? O5 C32 Cd1 60.07(18) . 1_655 ? C28 C32 Cd1 175.6(3) . 1_655 ? O8 C33 O7 121.6(4) . . ? O8 C33 C34 119.9(4) . . ? O7 C33 C34 118.5(4) . . ? C39 C34 C35 118.7(3) . . ? C39 C34 C33 119.3(3) . . ? C35 C34 C33 121.8(4) . . ? C36 C35 C34 121.4(4) . . ? C36 C35 H35 119.3 . . ? C34 C35 H35 119.3 . . ? C35 C36 C37 118.8(4) . . ? C35 C36 C40 121.9(4) . . ? C37 C36 C40 119.2(4) . . ? C38 C37 C36 120.4(4) . . ? C38 C37 H37 119.8 . . ? C36 C37 H37 119.8 . . ? C39 C38 C37 120.2(4) . . ? C39 C38 H38 119.9 . . ? C37 C38 H38 119.9 . . ? C38 C39 C34 120.5(4) . . ? C38 C39 H39 119.7 . . ? C34 C39 H39 119.7 . . ? O9 C40 O10 122.3(4) . . ? O9 C40 C36 120.7(4) . . ? O10 C40 C36 116.9(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Cd1 N1 C1 -173.7(3) . . . . ? O11 Cd1 N1 C1 -49.2(3) . . . . ? O5 Cd1 N1 C1 40.2(3) 1_455 . . . ? O6 Cd1 N1 C1 94.3(3) 1_455 . . . ? N5 Cd1 N1 C1 17.1(6) . . . . ? C32 Cd1 N1 C1 67.6(3) 1_455 . . . ? O3 Cd1 N1 C5 3.3(3) . . . . ? O11 Cd1 N1 C5 127.7(3) . . . . ? O5 Cd1 N1 C5 -142.9(3) 1_455 . . . ? O6 Cd1 N1 C5 -88.7(3) 1_455 . . . ? N5 Cd1 N1 C5 -166.0(4) . . . . ? C32 Cd1 N1 C5 -115.5(3) 1_455 . . . ? C6 N2 N3 C7 0.2(5) . . . . ? O12 Cd2 N4 C8 -45.2(3) . . . . ? O10 Cd2 N4 C8 174.7(3) 1_455 . . . ? O7 Cd2 N4 C8 87.0(3) . . . . ? N8 Cd2 N4 C8 20.8(7) . . . . ? O9 Cd2 N4 C8 -133.0(3) 1_455 . . . ? O12 Cd2 N4 C12 136.7(3) . . . . ? O10 Cd2 N4 C12 -3.4(3) 1_455 . . . ? O7 Cd2 N4 C12 -91.0(3) . . . . ? N8 Cd2 N4 C12 -157.2(5) . . . . ? O9 Cd2 N4 C12 49.0(3) 1_455 . . . ? O3 Cd1 N5 C13 171.8(3) . . . . ? N1 Cd1 N5 C13 -18.6(6) . . . . ? O11 Cd1 N5 C13 48.4(3) . . . . ? O5 Cd1 N5 C13 -41.7(3) 1_455 . . . ? O6 Cd1 N5 C13 -96.6(3) 1_455 . . . ? C32 Cd1 N5 C13 -69.4(3) 1_455 . . . ? O3 Cd1 N5 C17 -5.9(3) . . . . ? N1 Cd1 N5 C17 163.6(4) . . . . ? O11 Cd1 N5 C17 -129.3(3) . . . . ? O5 Cd1 N5 C17 140.6(3) 1_455 . . . ? O6 Cd1 N5 C17 85.7(3) 1_455 . . . ? C32 Cd1 N5 C17 112.9(3) 1_455 . . . ? C18 N6 N7 C19 0.5(4) . . . . ? O12 Cd2 N8 C20 47.0(3) . . . . ? O10 Cd2 N8 C20 -171.8(3) 1_455 . . . ? O7 Cd2 N8 C20 -84.6(3) . . . . ? N4 Cd2 N8 C20 -18.4(7) . . . . ? O9 Cd2 N8 C20 136.2(3) 1_455 . . . ? O12 Cd2 N8 C24 -139.0(3) . . . . ? O10 Cd2 N8 C24 2.2(3) 1_455 . . . ? O7 Cd2 N8 C24 89.4(3) . . . . ? N4 Cd2 N8 C24 155.6(5) . . . . ? O9 Cd2 N8 C24 -49.8(3) 1_455 . . . ? N1 Cd1 O3 C25 67.9(3) . . . . ? O11 Cd1 O3 C25 -31.6(3) . . . . ? O5 Cd1 O3 C25 164.6(2) 1_455 . . . ? O6 Cd1 O3 C25 159.5(3) 1_455 . . . ? N5 Cd1 O3 C25 -114.7(3) . . . . ? C32 Cd1 O3 C25 161.6(3) 1_455 . . . ? O12 Cd2 O7 C33 -10.1(3) . . . . ? O10 Cd2 O7 C33 179.8(3) 1_455 . . . ? N8 Cd2 O7 C33 79.5(3) . . . . ? N4 Cd2 O7 C33 -90.0(3) . . . . ? O9 Cd2 O7 C33 161.9(2) 1_455 . . . ? C5 N1 C1 C2 -1.8(6) . . . . ? Cd1 N1 C1 C2 175.3(3) . . . . ? N1 C1 C2 C3 1.1(6) . . . . ? N1 C1 C2 C6 -175.8(4) . . . . ? C1 C2 C3 C4 1.0(6) . . . . ? C6 C2 C3 C4 177.9(4) . . . . ? C2 C3 C4 C5 -2.3(6) . . . . ? C1 N1 C5 C4 0.5(6) . . . . ? Cd1 N1 C5 C4 -176.5(3) . . . . ? C3 C4 C5 N1 1.6(6) . . . . ? N3 N2 C6 O1 -0.1(5) . . . . ? N3 N2 C6 C2 -177.6(4) . . . . ? C7 O1 C6 N2 0.0(4) . . . . ? C7 O1 C6 C2 177.7(3) . . . . ? C1 C2 C6 N2 162.1(4) . . . . ? C3 C2 C6 N2 -14.8(6) . . . . ? C1 C2 C6 O1 -15.2(5) . . . . ? C3 C2 C6 O1 168.0(4) . . . . ? N2 N3 C7 O1 -0.2(5) . . . . ? N2 N3 C7 C9 175.8(4) . . . . ? C6 O1 C7 N3 0.1(4) . . . . ? C6 O1 C7 C9 -176.3(3) . . . . ? C12 N4 C8 C9 0.4(6) . . . . ? Cd2 N4 C8 C9 -177.8(3) . . . . ? N4 C8 C9 C10 -0.8(6) . . . . ? N4 C8 C9 C7 177.3(4) . . . . ? N3 C7 C9 C8 -165.1(4) . . . . ? O1 C7 C9 C8 10.7(6) . . . . ? N3 C7 C9 C10 13.0(7) . . . . ? O1 C7 C9 C10 -171.2(4) . . . . ? C8 C9 C10 C11 0.5(6) . . . . ? C7 C9 C10 C11 -177.7(4) . . . . ? C9 C10 C11 C12 0.2(6) . . . . ? C8 N4 C12 C11 0.4(6) . . . . ? Cd2 N4 C12 C11 178.5(3) . . . . ? C10 C11 C12 N4 -0.7(7) . . . . ? C17 N5 C13 C14 0.4(6) . . . . ? Cd1 N5 C13 C14 -177.4(3) . . . . ? N5 C13 C14 C15 -0.5(6) . . . . ? N5 C13 C14 C18 178.8(4) . . . . ? C13 C14 C15 C16 0.3(6) . . . . ? C18 C14 C15 C16 -179.0(4) . . . . ? C14 C15 C16 C17 0.0(7) . . . . ? C13 N5 C17 C16 -0.1(6) . . . . ? Cd1 N5 C17 C16 177.7(3) . . . . ? C15 C16 C17 N5 -0.1(7) . . . . ? N7 N6 C18 O2 0.1(4) . . . . ? N7 N6 C18 C14 179.1(4) . . . . ? C19 O2 C18 N6 -0.6(4) . . . . ? C19 O2 C18 C14 -179.7(3) . . . . ? C13 C14 C18 N6 -169.3(4) . . . . ? C15 C14 C18 N6 10.0(6) . . . . ? C13 C14 C18 O2 9.6(5) . . . . ? C15 C14 C18 O2 -171.1(4) . . . . ? N6 N7 C19 O2 -0.9(4) . . . . ? N6 N7 C19 C21 -179.3(4) . . . . ? C18 O2 C19 N7 0.9(4) . . . . ? C18 O2 C19 C21 179.5(3) . . . . ? C24 N8 C20 C21 -0.7(6) . . . . ? Cd2 N8 C20 C21 173.5(3) . . . . ? N8 C20 C21 C22 1.0(6) . . . . ? N8 C20 C21 C19 -179.1(4) . . . . ? N7 C19 C21 C20 176.0(4) . . . . ? O2 C19 C21 C20 -2.4(5) . . . . ? N7 C19 C21 C22 -4.2(6) . . . . ? O2 C19 C21 C22 177.5(4) . . . . ? C20 C21 C22 C23 -0.7(6) . . . . ? C19 C21 C22 C23 179.4(4) . . . . ? C21 C22 C23 C24 0.2(7) . . . . ? C20 N8 C24 C23 0.2(6) . . . . ? Cd2 N8 C24 C23 -173.8(3) . . . . ? C22 C23 C24 N8 0.1(7) . . . . ? Cd1 O3 C25 O4 -2.5(5) . . . . ? Cd1 O3 C25 C26 176.3(3) . . . . ? O4 C25 C26 C27 8.2(6) . . . . ? O3 C25 C26 C27 -170.7(4) . . . . ? O4 C25 C26 C31 -176.1(5) . . . . ? O3 C25 C26 C31 5.0(6) . . . . ? C31 C26 C27 C28 0.2(7) . . . . ? C25 C26 C27 C28 176.0(4) . . . . ? C26 C27 C28 C29 0.7(7) . . . . ? C26 C27 C28 C32 -176.0(4) . . . . ? C27 C28 C29 C30 -0.9(9) . . . . ? C32 C28 C29 C30 175.9(6) . . . . ? C28 C29 C30 C31 0.1(12) . . . . ? C29 C30 C31 C26 0.8(12) . . . . ? C27 C26 C31 C30 -1.0(10) . . . . ? C25 C26 C31 C30 -176.9(6) . . . . ? Cd1 O6 C32 O5 1.0(4) 1_655 . . . ? Cd1 O6 C32 C28 -175.0(3) 1_655 . . . ? Cd1 O5 C32 O6 -1.0(4) 1_655 . . . ? Cd1 O5 C32 C28 175.0(3) 1_655 . . . ? C29 C28 C32 O6 14.9(7) . . . . ? C27 C28 C32 O6 -168.4(4) . . . . ? C29 C28 C32 O5 -161.2(5) . . . . ? C27 C28 C32 O5 15.5(6) . . . . ? Cd2 O7 C33 O8 -0.5(5) . . . . ? Cd2 O7 C33 C34 177.6(3) . . . . ? O8 C33 C34 C39 179.4(4) . . . . ? O7 C33 C34 C39 1.4(6) . . . . ? O8 C33 C34 C35 3.9(6) . . . . ? O7 C33 C34 C35 -174.2(4) . . . . ? C39 C34 C35 C36 -0.8(6) . . . . ? C33 C34 C35 C36 174.8(4) . . . . ? C34 C35 C36 C37 0.8(6) . . . . ? C34 C35 C36 C40 -176.6(4) . . . . ? C35 C36 C37 C38 0.0(8) . . . . ? C40 C36 C37 C38 177.4(5) . . . . ? C36 C37 C38 C39 -0.8(9) . . . . ? C37 C38 C39 C34 0.8(9) . . . . ? C35 C34 C39 C38 0.0(7) . . . . ? C33 C34 C39 C38 -175.7(5) . . . . ? Cd2 O9 C40 O10 1.7(4) 1_655 . . . ? Cd2 O9 C40 C36 -177.1(3) 1_655 . . . ? Cd2 O10 C40 O9 -1.9(5) 1_655 . . . ? Cd2 O10 C40 C36 176.9(3) 1_655 . . . ? C35 C36 C40 O9 -11.6(6) . . . . ? C37 C36 C40 O9 171.0(4) . . . . ? C35 C36 C40 O10 169.5(4) . . . . ? C37 C36 C40 O10 -7.9(6) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 26.39 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.600 _refine_diff_density_min -0.490 _refine_diff_density_rms 0.105 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 790242' #TrackingRef '- CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H14 Cd N4 O5' _chemical_formula_weight 514.76 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 Tetragonal _symmetry_space_group_name_H-M I4(1)/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 29.7088(10) _cell_length_b 29.7088(10) _cell_length_c 10.3135(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9102.8(8) _cell_formula_units_Z 16 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3584 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 24.96 _exptl_crystal_description BLOCK _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 1.502 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4096 _exptl_absorpt_coefficient_mu 0.997 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.806371 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'APEX II CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22269 _diffrn_reflns_av_R_equivalents 0.0628 _diffrn_reflns_av_sigmaI/netI 0.0430 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 25.03 _reflns_number_total 3937 _reflns_number_gt 2976 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX II' _computing_cell_refinement 'Bruker APEX II' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0825P)^2^+18.3674P] 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 3937 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0796 _refine_ls_R_factor_gt 0.0563 _refine_ls_wR_factor_ref 0.1488 _refine_ls_wR_factor_gt 0.1334 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _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 0.287557(15) 0.725732(15) 1.10475(4) 0.03685(19) Uani 1 1 d . . . O1 O 0.19501(16) 0.62696(15) 0.7375(4) 0.0544(12) Uani 1 1 d . . . O2 O 0.28386(15) 0.72775(16) 0.8721(4) 0.0484(11) Uani 1 1 d . . . O3 O 0.34384(16) 0.69858(18) 0.9618(4) 0.0614(14) Uani 1 1 d . . . O4 O 0.32832(19) 0.70026(17) 0.2707(4) 0.0645(14) Uani 1 1 d . . . O5 O 0.28034(17) 0.7401(2) 0.3806(5) 0.0684(15) Uani 1 1 d . . . N1 N 0.24736(18) 0.65657(19) 1.0988(5) 0.0477(13) Uani 1 1 d . . . N2 N 0.1819(3) 0.5560(2) 0.7825(7) 0.089(2) Uani 1 1 d . . . N3 N 0.1700(3) 0.5647(3) 0.6484(6) 0.084(2) Uani 1 1 d . . . N4 N 0.18189(18) 0.7024(2) 0.4004(5) 0.0502(13) Uani 1 1 d . . . C1 C 0.2293(2) 0.6448(2) 0.9803(6) 0.0528(17) Uani 1 1 d . . . H1 H 0.2283 0.6664 0.9150 0.063 Uiso 1 1 calc R . . C2 C 0.2470(2) 0.6251(3) 1.1905(7) 0.061(2) Uani 1 1 d . . . H2 H 0.2585 0.6322 1.2718 0.073 Uiso 1 1 calc R . . C3 C 0.2306(3) 0.5833(3) 1.1711(8) 0.081(3) Uani 1 1 d . . . H3 H 0.2312 0.5625 1.2383 0.098 Uiso 1 1 calc R . . C4 C 0.2131(3) 0.5714(3) 1.0541(9) 0.083(3) Uani 1 1 d . . . H4 H 0.2016 0.5426 1.0406 0.100 Uiso 1 1 calc R . . C5 C 0.2129(3) 0.6033(2) 0.9549(7) 0.0593(19) Uani 1 1 d . . . C6 C 0.1961(3) 0.5929(2) 0.8268(7) 0.0559(18) Uani 1 1 d . . . C7 C 0.1784(2) 0.6059(3) 0.6300(6) 0.0542(18) Uani 1 1 d . . . C8 C 0.1714(2) 0.6330(2) 0.5138(6) 0.0491(16) Uani 1 1 d . . . C9 C 0.1894(2) 0.6755(2) 0.5026(6) 0.0510(17) Uani 1 1 d . . . H9 H 0.2076 0.6861 0.5692 0.061 Uiso 1 1 calc R . . C10 C 0.1556(3) 0.6865(3) 0.3073(7) 0.063(2) Uani 1 1 d . . . H10 H 0.1503 0.7044 0.2351 0.076 Uiso 1 1 calc R . . C11 C 0.1362(3) 0.6450(3) 0.3126(8) 0.087(3) Uani 1 1 d . . . H11 H 0.1180 0.6350 0.2453 0.104 Uiso 1 1 calc R . . C12 C 0.1438(3) 0.6189(3) 0.4168(7) 0.072(2) Uani 1 1 d . . . H12 H 0.1300 0.5908 0.4226 0.086 Uiso 1 1 calc R . . C13 C 0.34061(19) 0.69864(18) 0.7326(5) 0.0329(12) Uani 1 1 d . . . C14 C 0.31803(19) 0.71116(19) 0.6194(5) 0.0325(12) Uani 1 1 d . . . H14 H 0.2899 0.7210 0.6464 0.039 Uiso 1 1 d R . . C15 C 0.33632(19) 0.70094(18) 0.4993(5) 0.0343(13) Uani 1 1 d . . . C16 C 0.3772(2) 0.6795(2) 0.4928(6) 0.0408(14) Uani 1 1 d . . . H16 H 0.3895 0.6732 0.4118 0.049 Uiso 1 1 calc R . . C17 C 0.4008(2) 0.6670(2) 0.6030(6) 0.0449(15) Uani 1 1 d . . . C18 C 0.3819(2) 0.6768(2) 0.7223(5) 0.0418(14) Uani 1 1 d . . . H18 H 0.3971 0.6685 0.7974 0.050 Uiso 1 1 calc R . . C19 C 0.3216(2) 0.7085(2) 0.8628(5) 0.0365(13) Uani 1 1 d . . . C20 C 0.3129(2) 0.7146(2) 0.3770(6) 0.0380(14) Uani 1 1 d . . . C21 C 0.4461(3) 0.6431(3) 0.5939(7) 0.076(3) Uani 1 1 d . . . H21A H 0.4641 0.6571 0.5281 0.114 Uiso 1 1 d R . . H21B H 0.4414 0.6120 0.5721 0.114 Uiso 1 1 d R . . H21C H 0.4613 0.6450 0.6758 0.114 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 0.0402(3) 0.0468(3) 0.0235(3) 0.00103(17) -0.00352(17) 0.00557(19) O1 0.072(3) 0.051(3) 0.041(3) 0.005(2) -0.013(2) -0.017(2) O2 0.046(3) 0.066(3) 0.033(2) -0.001(2) -0.0028(18) 0.009(2) O3 0.065(3) 0.094(4) 0.025(2) 0.010(2) -0.002(2) 0.033(3) O4 0.087(4) 0.082(4) 0.024(2) -0.004(2) -0.012(2) 0.025(3) O5 0.049(3) 0.110(4) 0.047(3) 0.024(3) 0.002(2) 0.031(3) N1 0.046(3) 0.060(3) 0.037(3) 0.004(3) -0.008(2) -0.001(3) N2 0.135(7) 0.059(4) 0.074(5) 0.013(4) -0.040(5) -0.035(4) N3 0.126(7) 0.072(5) 0.053(4) 0.008(3) -0.035(4) -0.035(4) N4 0.047(3) 0.065(4) 0.039(3) 0.004(3) -0.007(2) -0.008(3) C1 0.053(4) 0.063(5) 0.042(4) 0.014(3) -0.007(3) -0.013(3) C2 0.060(5) 0.082(6) 0.040(4) 0.018(4) -0.010(3) -0.016(4) C3 0.100(7) 0.085(6) 0.059(5) 0.031(4) -0.021(5) -0.029(5) C4 0.108(7) 0.070(5) 0.071(6) 0.027(5) -0.031(5) -0.035(5) C5 0.073(5) 0.052(4) 0.053(4) 0.011(3) -0.020(4) -0.017(4) C6 0.066(5) 0.054(4) 0.048(4) 0.001(3) -0.015(3) -0.020(4) C7 0.060(4) 0.057(4) 0.045(4) 0.003(3) -0.011(3) -0.019(3) C8 0.055(4) 0.054(4) 0.039(4) 0.000(3) -0.008(3) -0.017(3) C9 0.052(4) 0.059(4) 0.042(4) 0.001(3) -0.010(3) -0.010(3) C10 0.076(5) 0.074(5) 0.040(4) 0.007(4) -0.018(4) -0.028(4) C11 0.099(7) 0.101(7) 0.060(5) 0.014(5) -0.038(5) -0.055(6) C12 0.081(6) 0.087(6) 0.046(4) 0.010(4) -0.017(4) -0.042(5) C13 0.038(3) 0.030(3) 0.031(3) 0.000(2) -0.002(2) 0.000(2) C14 0.031(3) 0.036(3) 0.031(3) 0.004(2) -0.005(2) 0.001(2) C15 0.041(3) 0.034(3) 0.028(3) 0.004(2) -0.010(2) 0.001(3) C16 0.044(4) 0.050(4) 0.028(3) -0.003(3) -0.002(3) 0.011(3) C17 0.039(3) 0.058(4) 0.038(3) 0.001(3) -0.005(3) 0.010(3) C18 0.051(4) 0.049(4) 0.026(3) 0.003(3) -0.006(3) 0.012(3) C19 0.043(3) 0.040(3) 0.027(3) 0.002(2) -0.003(2) 0.007(3) C20 0.037(3) 0.043(3) 0.034(3) 0.004(3) -0.007(3) -0.005(3) C21 0.061(5) 0.111(7) 0.056(5) 0.005(4) -0.003(4) 0.043(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 O4 2.229(4) 1_556 ? Cd1 O5 2.263(5) 13_566 ? Cd1 N4 2.322(6) 13_566 ? Cd1 O3 2.371(5) . ? Cd1 N1 2.377(6) . ? Cd1 O2 2.403(4) . ? Cd1 C19 2.740(6) . ? O1 C7 1.365(8) . ? O1 C6 1.368(8) . ? O2 C19 1.262(7) . ? O3 C19 1.252(7) . ? O4 C20 1.262(7) . ? O4 Cd1 2.229(4) 1_554 ? O5 C20 1.230(8) . ? O5 Cd1 2.263(5) 13_566 ? N1 C2 1.331(9) . ? N1 C1 1.381(8) . ? N2 C6 1.260(9) . ? N2 N3 1.451(9) . ? N3 C7 1.264(10) . ? N4 C10 1.324(8) . ? N4 C9 1.341(8) . ? N4 Cd1 2.322(6) 13_566 ? C1 C5 1.350(9) . ? C1 H1 0.9300 . ? C2 C3 1.348(11) . ? C2 H2 0.9300 . ? C3 C4 1.361(11) . ? C3 H3 0.9300 . ? C4 C5 1.396(10) . ? C4 H4 0.9300 . ? C5 C6 1.446(9) . ? C7 C8 1.459(9) . ? C8 C12 1.360(9) . ? C8 C9 1.374(9) . ? C9 H9 0.9300 . ? C10 C11 1.360(11) . ? C10 H10 0.9300 . ? C11 C12 1.345(11) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C18 1.392(8) . ? C13 C14 1.397(7) . ? C13 C19 1.486(8) . ? C14 C15 1.386(8) . ? C14 H14 0.9298 . ? C15 C16 1.374(8) . ? C15 C20 1.496(7) . ? C16 C17 1.386(8) . ? C16 H16 0.9300 . ? C17 C18 1.383(8) . ? C17 C21 1.525(9) . ? C18 H18 0.9300 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Cd1 O5 125.82(18) 1_556 13_566 ? O4 Cd1 N4 96.75(19) 1_556 13_566 ? O5 Cd1 N4 86.4(2) 13_566 13_566 ? O4 Cd1 O3 88.78(17) 1_556 . ? O5 Cd1 O3 145.37(16) 13_566 . ? N4 Cd1 O3 91.3(2) 13_566 . ? O4 Cd1 N1 89.95(19) 1_556 . ? O5 Cd1 N1 86.6(2) 13_566 . ? N4 Cd1 N1 172.34(18) 13_566 . ? O3 Cd1 N1 92.54(19) . . ? O4 Cd1 O2 143.14(16) 1_556 . ? O5 Cd1 O2 90.84(16) 13_566 . ? N4 Cd1 O2 88.40(17) 13_566 . ? O3 Cd1 O2 54.54(15) . . ? N1 Cd1 O2 88.45(17) . . ? O4 Cd1 C19 115.81(18) 1_556 . ? O5 Cd1 C19 118.25(17) 13_566 . ? N4 Cd1 C19 90.40(18) 13_566 . ? O3 Cd1 C19 27.14(16) . . ? N1 Cd1 C19 90.02(18) . . ? O2 Cd1 C19 27.41(16) . . ? C7 O1 C6 102.5(5) . . ? C19 O2 Cd1 91.4(3) . . ? C19 O3 Cd1 93.1(4) . . ? C20 O4 Cd1 110.8(4) . 1_554 ? C20 O5 Cd1 168.5(5) . 13_566 ? C2 N1 C1 116.6(6) . . ? C2 N1 Cd1 126.5(5) . . ? C1 N1 Cd1 115.9(4) . . ? C6 N2 N3 105.8(6) . . ? C7 N3 N2 105.5(6) . . ? C10 N4 C9 117.1(6) . . ? C10 N4 Cd1 122.8(5) . 13_566 ? C9 N4 Cd1 120.1(4) . 13_566 ? C5 C1 N1 122.9(6) . . ? C5 C1 H1 118.6 . . ? N1 C1 H1 118.6 . . ? N1 C2 C3 123.0(7) . . ? N1 C2 H2 118.5 . . ? C3 C2 H2 118.5 . . ? C2 C3 C4 120.7(7) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? C3 C4 C5 118.3(8) . . ? C3 C4 H4 120.8 . . ? C5 C4 H4 120.8 . . ? C1 C5 C4 118.5(7) . . ? C1 C5 C6 119.8(6) . . ? C4 C5 C6 121.8(7) . . ? N2 C6 O1 113.1(6) . . ? N2 C6 C5 129.2(7) . . ? O1 C6 C5 117.7(6) . . ? N3 C7 O1 113.1(6) . . ? N3 C7 C8 129.1(6) . . ? O1 C7 C8 117.8(6) . . ? C12 C8 C9 117.1(7) . . ? C12 C8 C7 121.3(6) . . ? C9 C8 C7 121.3(6) . . ? N4 C9 C8 123.2(6) . . ? N4 C9 H9 118.4 . . ? C8 C9 H9 118.4 . . ? N4 C10 C11 122.9(7) . . ? N4 C10 H10 118.5 . . ? C11 C10 H10 118.5 . . ? C12 C11 C10 119.0(7) . . ? C12 C11 H11 120.5 . . ? C10 C11 H11 120.5 . . ? C11 C12 C8 120.6(7) . . ? C11 C12 H12 119.7 . . ? C8 C12 H12 119.7 . . ? C18 C13 C14 118.9(5) . . ? C18 C13 C19 119.8(5) . . ? C14 C13 C19 121.3(5) . . ? C15 C14 C13 120.0(5) . . ? C15 C14 H14 133.6 . . ? C13 C14 H14 105.4 . . ? C16 C15 C14 119.5(5) . . ? C16 C15 C20 119.7(5) . . ? C14 C15 C20 120.8(5) . . ? C15 C16 C17 122.1(5) . . ? C15 C16 H16 119.0 . . ? C17 C16 H16 119.0 . . ? C18 C17 C16 117.9(6) . . ? C18 C17 C21 120.7(6) . . ? C16 C17 C21 121.4(6) . . ? C17 C18 C13 121.6(5) . . ? C17 C18 H18 119.2 . . ? C13 C18 H18 119.2 . . ? O3 C19 O2 120.9(5) . . ? O3 C19 C13 119.3(5) . . ? O2 C19 C13 119.7(5) . . ? O3 C19 Cd1 59.7(3) . . ? O2 C19 Cd1 61.2(3) . . ? C13 C19 Cd1 179.0(4) . . ? O5 C20 O4 121.3(5) . . ? O5 C20 C15 120.5(6) . . ? O4 C20 C15 118.2(5) . . ? C17 C21 H21A 109.5 . . ? C17 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C17 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 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 O4 Cd1 O2 C19 -5.2(5) 1_556 . . . ? O5 Cd1 O2 C19 -179.6(4) 13_566 . . . ? N4 Cd1 O2 C19 94.0(4) 13_566 . . . ? O3 Cd1 O2 C19 1.2(4) . . . . ? N1 Cd1 O2 C19 -93.0(4) . . . . ? O4 Cd1 O3 C19 175.0(4) 1_556 . . . ? O5 Cd1 O3 C19 -2.7(6) 13_566 . . . ? N4 Cd1 O3 C19 -88.3(4) 13_566 . . . ? N1 Cd1 O3 C19 85.1(4) . . . . ? O2 Cd1 O3 C19 -1.2(4) . . . . ? O4 Cd1 N1 C2 14.4(6) 1_556 . . . ? O5 Cd1 N1 C2 -111.5(6) 13_566 . . . ? O3 Cd1 N1 C2 103.1(6) . . . . ? O2 Cd1 N1 C2 157.5(6) . . . . ? C19 Cd1 N1 C2 130.2(6) . . . . ? O4 Cd1 N1 C1 -153.6(5) 1_556 . . . ? O5 Cd1 N1 C1 80.5(5) 13_566 . . . ? O3 Cd1 N1 C1 -64.9(5) . . . . ? O2 Cd1 N1 C1 -10.5(5) . . . . ? C19 Cd1 N1 C1 -37.8(5) . . . . ? C6 N2 N3 C7 -0.4(11) . . . . ? C2 N1 C1 C5 -1.7(10) . . . . ? Cd1 N1 C1 C5 167.5(6) . . . . ? C1 N1 C2 C3 0.9(11) . . . . ? Cd1 N1 C2 C3 -167.0(7) . . . . ? N1 C2 C3 C4 -0.3(14) . . . . ? C2 C3 C4 C5 0.4(15) . . . . ? N1 C1 C5 C4 1.8(12) . . . . ? N1 C1 C5 C6 -177.5(7) . . . . ? C3 C4 C5 C1 -1.1(14) . . . . ? C3 C4 C5 C6 178.2(9) . . . . ? N3 N2 C6 O1 0.5(10) . . . . ? N3 N2 C6 C5 -179.1(8) . . . . ? C7 O1 C6 N2 -0.4(9) . . . . ? C7 O1 C6 C5 179.3(7) . . . . ? C1 C5 C6 N2 175.6(9) . . . . ? C4 C5 C6 N2 -3.7(15) . . . . ? C1 C5 C6 O1 -3.9(11) . . . . ? C4 C5 C6 O1 176.7(8) . . . . ? N2 N3 C7 O1 0.2(10) . . . . ? N2 N3 C7 C8 -177.9(8) . . . . ? C6 O1 C7 N3 0.1(9) . . . . ? C6 O1 C7 C8 178.4(7) . . . . ? N3 C7 C8 C12 17.0(14) . . . . ? O1 C7 C8 C12 -161.0(8) . . . . ? N3 C7 C8 C9 -168.6(9) . . . . ? O1 C7 C8 C9 13.4(11) . . . . ? C10 N4 C9 C8 0.3(10) . . . . ? Cd1 N4 C9 C8 178.2(5) 13_566 . . . ? C12 C8 C9 N4 -1.9(11) . . . . ? C7 C8 C9 N4 -176.5(7) . . . . ? C9 N4 C10 C11 0.7(12) . . . . ? Cd1 N4 C10 C11 -177.2(7) 13_566 . . . ? N4 C10 C11 C12 0.1(16) . . . . ? C10 C11 C12 C8 -1.8(16) . . . . ? C9 C8 C12 C11 2.6(13) . . . . ? C7 C8 C12 C11 177.2(9) . . . . ? C18 C13 C14 C15 1.3(8) . . . . ? C19 C13 C14 C15 -179.1(5) . . . . ? C13 C14 C15 C16 -1.6(8) . . . . ? C13 C14 C15 C20 -179.2(5) . . . . ? C14 C15 C16 C17 1.0(9) . . . . ? C20 C15 C16 C17 178.5(6) . . . . ? C15 C16 C17 C18 0.0(10) . . . . ? C15 C16 C17 C21 179.8(7) . . . . ? C16 C17 C18 C13 -0.3(10) . . . . ? C21 C17 C18 C13 179.9(7) . . . . ? C14 C13 C18 C17 -0.4(9) . . . . ? C19 C13 C18 C17 -180.0(6) . . . . ? Cd1 O3 C19 O2 2.2(6) . . . . ? Cd1 O3 C19 C13 -179.7(5) . . . . ? Cd1 O2 C19 O3 -2.2(6) . . . . ? Cd1 O2 C19 C13 179.8(5) . . . . ? C18 C13 C19 O3 2.9(9) . . . . ? C14 C13 C19 O3 -176.7(6) . . . . ? C18 C13 C19 O2 -179.0(6) . . . . ? C14 C13 C19 O2 1.4(9) . . . . ? O4 Cd1 C19 O3 -5.6(5) 1_556 . . . ? O5 Cd1 C19 O3 178.3(4) 13_566 . . . ? N4 Cd1 C19 O3 92.1(4) 13_566 . . . ? N1 Cd1 C19 O3 -95.6(4) . . . . ? O2 Cd1 C19 O3 177.8(6) . . . . ? O4 Cd1 C19 O2 176.6(3) 1_556 . . . ? O5 Cd1 C19 O2 0.4(4) 13_566 . . . ? N4 Cd1 C19 O2 -85.7(4) 13_566 . . . ? O3 Cd1 C19 O2 -177.8(6) . . . . ? N1 Cd1 C19 O2 86.6(4) . . . . ? Cd1 O4 C20 O5 -1.7(8) 1_554 . . . ? Cd1 O4 C20 C15 -179.8(4) 1_554 . . . ? C16 C15 C20 O5 -168.0(6) . . . . ? C14 C15 C20 O5 9.6(9) . . . . ? C16 C15 C20 O4 10.2(9) . . . . ? C14 C15 C20 O4 -172.3(6) . . . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.548 _refine_diff_density_min -0.542 _refine_diff_density_rms 0.124 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 790243' #TrackingRef '- CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H68 Cd4 N12 O33' _chemical_formula_weight 2078.98 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 C2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 21.225(2) _cell_length_b 17.3202(18) _cell_length_c 21.869(2) _cell_angle_alpha 90.00 _cell_angle_beta 101.709(2) _cell_angle_gamma 90.00 _cell_volume 7872.0(13) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 8496 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 28.03 _exptl_crystal_description BLOCK _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 1.754 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4160 _exptl_absorpt_coefficient_mu 1.164 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.774901 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Apex II CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20385 _diffrn_reflns_av_R_equivalents 0.0246 _diffrn_reflns_av_sigmaI/netI 0.0360 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 25.03 _reflns_number_total 10861 _reflns_number_gt 9702 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex II' _computing_cell_refinement 'Bruker Apex II' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0354P)^2^+3.5765P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(3) _refine_ls_number_reflns 10861 _refine_ls_number_parameters 1096 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0358 _refine_ls_R_factor_gt 0.0294 _refine_ls_wR_factor_ref 0.0714 _refine_ls_wR_factor_gt 0.0679 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _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 -0.20259(2) 0.37308(3) 0.452719(18) 0.04119(11) Uani 1 1 d . . . Cd2 Cd 0.18854(2) 0.41073(3) 0.05830(2) 0.04659(12) Uani 1 1 d . . . Cd3 Cd 0.18938(2) 0.25959(2) 0.293890(18) 0.04197(11) Uani 1 1 d . . . Cd4 Cd 0.306451(19) 0.76244(2) 0.199195(18) 0.03790(10) Uani 1 1 d . . . O1 O -0.1421(2) 0.2684(3) 0.39693(19) 0.0516(11) Uani 1 1 d . . . O2 O -0.2036(2) 0.2449(2) 0.46378(19) 0.0532(11) Uani 1 1 d . . . O3 O -0.2542(3) -0.0192(3) 0.5155(2) 0.0692(15) Uani 1 1 d . . . O4 O -0.2234(2) -0.1180(3) 0.4680(2) 0.0612(12) Uani 1 1 d . . . O5 O -0.0814(3) -0.0023(3) 0.3343(2) 0.0794(18) Uani 1 1 d . . . O6 O 0.1327(2) 0.2904(2) 0.10568(19) 0.0487(11) Uani 1 1 d . . . O7 O 0.2059(2) 0.2858(2) 0.0483(2) 0.0692(14) Uani 1 1 d . . . O8 O 0.2794(2) 0.0380(3) -0.0225(2) 0.0609(13) Uani 1 1 d . . . O9 O 0.2432(2) -0.0688(3) 0.0078(2) 0.0817(16) Uani 1 1 d . . . O10 O 0.1035(2) 0.0042(2) 0.1544(2) 0.0591(12) Uani 1 1 d . . . O11 O -0.00947(16) 0.5102(2) 0.25847(15) 0.0356(8) Uani 1 1 d . . . O12 O 0.1984(2) 0.3886(2) 0.2761(2) 0.0585(13) Uani 1 1 d . . . O13 O 0.14325(19) 0.3687(3) 0.34953(17) 0.0477(10) Uani 1 1 d . . . O14 O 0.2655(2) 0.6504(3) 0.2329(2) 0.0540(11) Uani 1 1 d . . . O15 O 0.2348(2) 0.7501(2) 0.27883(17) 0.0521(10) Uani 1 1 d . . . O16 O 0.0892(3) 0.6406(3) 0.4102(3) 0.100(2) Uani 1 1 d . . . O17 O 0.36026(19) 0.8738(3) 0.14353(18) 0.0504(10) Uani 1 1 d . . . O18 O 0.3022(2) 0.89115(19) 0.21449(18) 0.0486(11) Uani 1 1 d . . . O19 O 0.2313(2) 1.1507(3) 0.2605(2) 0.0517(11) Uani 1 1 d . . . O20 O 0.2646(2) 1.2525(3) 0.21825(18) 0.0564(11) Uani 1 1 d . . . O21 O 0.4176(2) 1.1527(3) 0.0929(2) 0.0658(14) Uani 1 1 d . . . O22 O 0.05017(19) 0.8175(3) 0.1883(2) 0.0619(12) Uani 1 1 d . . . O23 O 0.5000 0.6398(3) 0.0000 0.0372(12) Uani 1 2 d S . . O24 O 0.0000 0.1374(3) 0.5000 0.0396(12) Uani 1 2 d S . . O25 O -0.11149(19) 0.3824(2) 0.53419(17) 0.0527(11) Uani 1 1 d . . . H25A H -0.0805 0.3513 0.5344 0.079 Uiso 1 1 d R . . H25B H -0.1306 0.3810 0.5648 0.079 Uiso 1 1 d R . . O26 O -0.2863(2) 0.3545(3) 0.36706(19) 0.0678(12) Uani 1 1 d . . . H26A H -0.2731 0.3813 0.3396 0.102 Uiso 1 1 d R . . H26B H -0.3269 0.3493 0.3625 0.102 Uiso 1 1 d R . . O27 O 0.1015(2) 0.3997(3) -0.02823(19) 0.0610(12) Uani 1 1 d . . . H27A H 0.0971 0.3962 -0.0676 0.092 Uiso 1 1 d R . . H27B H 0.0781 0.3641 -0.0179 0.092 Uiso 1 1 d R . . O28 O 0.27555(19) 0.2743(2) 0.37650(18) 0.0627(12) Uani 1 1 d . . . H28A H 0.2752 0.2403 0.4044 0.094 Uiso 1 1 d R . . H28B H 0.2647 0.3198 0.3847 0.094 Uiso 1 1 d R . . O29 O 0.09639(17) 0.2600(3) 0.21571(16) 0.0503(9) Uani 1 1 d . . . H29A H 0.1091 0.2650 0.1815 0.075 Uiso 1 1 d R . . H29B H 0.0740 0.2967 0.2259 0.075 Uiso 1 1 d R . . O30 O 0.39419(17) 0.7551(3) 0.28212(16) 0.0484(9) Uani 1 1 d . . . H30A H 0.3815 0.7565 0.3165 0.073 Uiso 1 1 d R . . H30B H 0.4128 0.7951 0.2718 0.073 Uiso 1 1 d R . . O31 O 0.2563(2) 0.3981(3) 0.1628(2) 0.0736(13) Uani 1 1 d . . . H31A H 0.2788 0.4157 0.1966 0.110 Uiso 1 1 d R . . H31B H 0.2759 0.3786 0.1362 0.110 Uiso 1 1 d R . . O32 O 0.3030(4) 0.1879(4) 0.4824(3) 0.129(3) Uani 1 1 d . . . O33 O 0.1973(3) 0.9412(3) 0.2627(2) 0.0930(17) Uani 1 1 d . . . O34 O 0.3976(4) 0.3060(6) 0.5129(4) 0.217(5) Uani 1 1 d . . . N1 N -0.1512(2) 0.4616(3) 0.3980(2) 0.0419(12) Uani 1 1 d . . . N2 N -0.0270(2) 0.3881(3) 0.2779(2) 0.0454(13) Uani 1 1 d . . . N3 N 0.0139(2) 0.3918(2) 0.2346(2) 0.0411(12) Uani 1 1 d . . . N4 N 0.1296(2) 0.4883(3) 0.1129(2) 0.0435(13) Uani 1 1 d . . . N5 N 0.3551(2) 0.6782(3) 0.1388(2) 0.0414(12) Uani 1 1 d . . . N6 N 0.4792(2) 0.7588(3) 0.0213(2) 0.0482(11) Uani 1 1 d . . . N7 N 0.1376(2) 0.1748(3) 0.3528(2) 0.0433(12) Uani 1 1 d . . . N8 N 0.0193(2) 0.2573(3) 0.4778(2) 0.0460(11) Uani 1 1 d . . . N9 N 0.2151(2) 0.7821(2) 0.12137(19) 0.0431(11) Uani 1 1 d . . . N10 N -0.0084(3) 0.8558(4) 0.1003(3) 0.0893(19) Uani 1 1 d . . . N11 N -0.0462(3) 0.8583(4) 0.1465(3) 0.0882(19) Uani 1 1 d . . . C53 C -0.0969(4) 0.8058(5) 0.3255(4) 0.079(2) Uani 1 1 d . . . H53 H -0.1387 0.7992 0.3315 0.095 Uiso 1 1 calc R . . C1 C -0.1098(3) 0.4386(3) 0.3631(2) 0.0413(14) Uani 1 1 d . . . H1 H -0.1009 0.3862 0.3611 0.050 Uiso 1 1 calc R . . C2 C -0.1638(3) 0.5372(4) 0.3994(3) 0.0455(16) Uani 1 1 d . . . H2 H -0.1938 0.5539 0.4220 0.055 Uiso 1 1 calc R . . C3 C -0.1343(3) 0.5909(4) 0.3689(3) 0.0554(16) Uani 1 1 d . . . H3 H -0.1430 0.6432 0.3722 0.067 Uiso 1 1 calc R . . C4 C -0.0923(3) 0.5670(3) 0.3340(3) 0.0496(15) Uani 1 1 d . . . H4 H -0.0720 0.6027 0.3127 0.059 Uiso 1 1 calc R . . C5 C -0.0800(3) 0.4894(3) 0.3303(2) 0.0342(12) Uani 1 1 d . . . C6 C -0.0391(2) 0.4584(3) 0.2899(2) 0.0349(12) Uani 1 1 d . . . C7 C 0.0222(2) 0.4638(3) 0.2248(2) 0.0344(12) Uani 1 1 d . . . C8 C 0.0594(3) 0.5008(3) 0.1843(2) 0.0348(13) Uani 1 1 d . . . C9 C 0.0665(3) 0.5793(3) 0.1848(3) 0.0448(14) Uani 1 1 d . . . H9 H 0.0455 0.6102 0.2091 0.054 Uiso 1 1 calc R . . C10 C 0.1059(3) 0.6119(3) 0.1483(3) 0.0519(15) Uani 1 1 d . . . H10 H 0.1108 0.6652 0.1467 0.062 Uiso 1 1 calc R . . C11 C 0.1376(3) 0.5637(3) 0.1143(2) 0.0440(14) Uani 1 1 d . . . H11 H 0.1657 0.5853 0.0916 0.053 Uiso 1 1 calc R . . C12 C 0.0911(3) 0.4559(3) 0.1477(2) 0.0404(13) Uani 1 1 d . . . H12 H 0.0858 0.4026 0.1472 0.048 Uiso 1 1 calc R . . C13 C 0.1692(2) 0.1669(3) 0.0797(2) 0.0321(11) Uani 1 1 d . . . C14 C 0.2065(3) 0.1259(3) 0.0457(2) 0.0365(12) Uani 1 1 d . . . H14 H 0.2306 0.1522 0.0214 0.044 Uiso 1 1 calc R . . C15 C 0.2082(2) 0.0470(3) 0.0477(2) 0.0324(12) Uani 1 1 d . . . C16 C 0.1720(3) 0.0070(3) 0.0838(2) 0.0387(13) Uani 1 1 d . . . H16 H 0.1728 -0.0466 0.0850 0.046 Uiso 1 1 calc R . . C17 C 0.1349(3) 0.0479(3) 0.1177(3) 0.0399(14) Uani 1 1 d . . . C18 C 0.1330(2) 0.1272(3) 0.1149(2) 0.0351(12) Uani 1 1 d . . . H18 H 0.1070 0.1542 0.1370 0.042 Uiso 1 1 calc R . . C19 C 0.1683(3) 0.2521(3) 0.0775(2) 0.0414(13) Uani 1 1 d . . . C20 C 0.2464(3) 0.0032(4) 0.0089(3) 0.0432(15) Uani 1 1 d . . . C21 C 0.0675(3) 0.0442(4) 0.1915(3) 0.0592(19) Uani 1 1 d . . . H21A H 0.0931 0.0851 0.2134 0.089 Uiso 1 1 calc R . . H21B H 0.0553 0.0092 0.2212 0.089 Uiso 1 1 calc R . . H21C H 0.0296 0.0654 0.1655 0.089 Uiso 1 1 calc R . . C22 C -0.1621(2) 0.1373(3) 0.4192(2) 0.0330(11) Uani 1 1 d . . . C23 C -0.1951(2) 0.0860(3) 0.4494(2) 0.0372(14) Uani 1 1 d . . . H23 H -0.2218 0.1047 0.4748 0.045 Uiso 1 1 calc R . . C24 C -0.1891(3) 0.0077(3) 0.4425(3) 0.0371(13) Uani 1 1 d . . . C25 C -0.1523(3) -0.0207(4) 0.4032(3) 0.0462(16) Uani 1 1 d . . . H25 H -0.1501 -0.0736 0.3965 0.055 Uiso 1 1 calc R . . C26 C -0.1176(3) 0.0314(4) 0.3726(3) 0.0461(15) Uani 1 1 d . . . C27 C -0.1242(2) 0.1080(3) 0.3798(2) 0.0378(12) Uani 1 1 d . . . H27 H -0.1029 0.1419 0.3580 0.045 Uiso 1 1 calc R . . C28 C -0.1693(3) 0.2210(3) 0.4266(2) 0.0387(13) Uani 1 1 d . . . C29 C -0.2238(3) -0.0474(3) 0.4772(3) 0.0422(14) Uani 1 1 d . . . C30 C -0.0637(4) 0.0441(5) 0.2895(4) 0.085(3) Uani 1 1 d . . . H30' H -0.1001 0.0738 0.2692 0.128 Uiso 1 1 calc R . . H30" H -0.0488 0.0125 0.2593 0.128 Uiso 1 1 calc R . . H30C H -0.0299 0.0782 0.3089 0.128 Uiso 1 1 calc R . . C31 C 0.0974(3) 0.2002(3) 0.3885(3) 0.0440(14) Uani 1 1 d . . . H31 H 0.0885 0.2528 0.3884 0.053 Uiso 1 1 calc R . . C32 C 0.1475(3) 0.0988(4) 0.3519(3) 0.0476(16) Uani 1 1 d . . . H32 H 0.1744 0.0797 0.3268 0.057 Uiso 1 1 calc R . . C33 C 0.1197(3) 0.0475(4) 0.3865(3) 0.0533(16) Uani 1 1 d . . . H33 H 0.1282 -0.0050 0.3847 0.064 Uiso 1 1 calc R . . C34 C 0.0794(3) 0.0740(4) 0.4235(3) 0.0523(16) Uani 1 1 d . . . H34 H 0.0598 0.0400 0.4468 0.063 Uiso 1 1 calc R . . C35 C 0.0686(3) 0.1528(4) 0.4253(2) 0.0392(14) Uani 1 1 d . . . C36 C 0.0284(3) 0.1855(4) 0.4667(2) 0.0384(13) Uani 1 1 d . . . C37 C 0.3960(3) 0.7034(3) 0.1049(2) 0.0393(13) Uani 1 1 d . . . H37 H 0.4037 0.7562 0.1039 0.047 Uiso 1 1 calc R . . C38 C 0.3453(3) 0.6012(4) 0.1402(3) 0.0441(15) Uani 1 1 d . . . H38 H 0.3164 0.5824 0.1634 0.053 Uiso 1 1 calc R . . C39 C 0.3754(3) 0.5505(3) 0.1093(3) 0.0485(15) Uani 1 1 d . . . H39 H 0.3685 0.4978 0.1129 0.058 Uiso 1 1 calc R . . C40 C 0.4165(3) 0.5763(3) 0.0726(3) 0.0442(14) Uani 1 1 d . . . H40 H 0.4362 0.5420 0.0496 0.053 Uiso 1 1 calc R . . C41 C 0.4278(2) 0.6555(3) 0.0710(2) 0.0355(13) Uani 1 1 d . . . C42 C 0.4689(3) 0.6877(3) 0.0320(2) 0.0362(13) Uani 1 1 d . . . C43 C 0.1614(3) 0.8009(3) 0.1414(3) 0.0484(14) Uani 1 1 d . . . H43 H 0.1634 0.8044 0.1841 0.058 Uiso 1 1 calc R . . C44 C 0.2124(3) 0.7792(4) 0.0606(3) 0.0584(18) Uani 1 1 d . . . H44 H 0.2499 0.7681 0.0464 0.070 Uiso 1 1 calc R . . C45 C 0.1556(4) 0.7921(4) 0.0165(3) 0.073(2) Uani 1 1 d . . . H45 H 0.1548 0.7876 -0.0261 0.087 Uiso 1 1 calc R . . C46 C 0.1010(3) 0.8116(4) 0.0376(3) 0.0718(19) Uani 1 1 d . . . H46 H 0.0630 0.8220 0.0093 0.086 Uiso 1 1 calc R . . C47 C 0.1026(3) 0.8156(4) 0.1011(3) 0.0512(14) Uani 1 1 d . . . C48 C 0.0461(3) 0.8319(3) 0.1269(3) 0.0526(15) Uani 1 1 d . . . C49 C -0.0102(3) 0.8361(4) 0.1959(4) 0.0649(18) Uani 1 1 d . . . C50 C -0.0237(3) 0.8241(5) 0.2595(4) 0.073(2) Uani 1 1 d . . . C51 C 0.0259(4) 0.8214(6) 0.3104(4) 0.105(3) Uani 1 1 d . . . H51 H 0.0682 0.8263 0.3053 0.126 Uiso 1 1 calc R . . N12 N 0.0131(4) 0.8118(6) 0.3682(4) 0.140(3) Uani 1 1 d . . . C52 C -0.0479(5) 0.8029(6) 0.3743(5) 0.116(4) Uani 1 1 d . . . H52 H -0.0563 0.7944 0.4139 0.139 Uiso 1 1 calc R . . C54 C -0.0863(3) 0.8184(5) 0.2672(4) 0.092(3) Uani 1 1 d . . . H54 H -0.1205 0.8229 0.2333 0.111 Uiso 1 1 calc R . . C55 C 0.1980(2) 0.6270(3) 0.3046(2) 0.0353(12) Uani 1 1 d . . . C56 C 0.2018(2) 0.5480(3) 0.2959(2) 0.0309(12) Uani 1 1 d . . . H56 H 0.2273 0.5282 0.2696 0.037 Uiso 1 1 calc R . . C57 C 0.1671(2) 0.4988(3) 0.3269(2) 0.0344(12) Uani 1 1 d . . . C58 C 0.1283(3) 0.5278(3) 0.3657(2) 0.0405(13) Uani 1 1 d . . . H58 H 0.1048 0.4948 0.3861 0.049 Uiso 1 1 calc R . . C59 C 0.1254(3) 0.6068(4) 0.3732(3) 0.0502(17) Uani 1 1 d . . . C60 C 0.1599(3) 0.6569(4) 0.3430(3) 0.0479(17) Uani 1 1 d . . . H60 H 0.1574 0.7099 0.3485 0.057 Uiso 1 1 calc R . . C61 C 0.2356(3) 0.6796(3) 0.2704(3) 0.0380(13) Uani 1 1 d . . . C62 C 0.1697(2) 0.4131(3) 0.3179(2) 0.0392(12) Uani 1 1 d . . . C63 C 0.0604(4) 0.5977(6) 0.4495(4) 0.096(3) Uani 1 1 d . . . H63A H 0.0308 0.5618 0.4255 0.144 Uiso 1 1 calc R . . H63B H 0.0374 0.6314 0.4722 0.144 Uiso 1 1 calc R . . H63C H 0.0926 0.5700 0.4783 0.144 Uiso 1 1 calc R . . C64 C 0.3376(2) 1.0043(3) 0.1697(2) 0.0338(11) Uani 1 1 d . . . C65 C 0.3028(2) 1.0514(3) 0.2006(2) 0.0338(12) Uani 1 1 d . . . H65 H 0.2770 1.0298 0.2258 0.041 Uiso 1 1 calc R . . C66 C 0.3055(2) 1.1307(3) 0.1947(2) 0.0342(12) Uani 1 1 d . . . C67 C 0.3445(3) 1.1620(4) 0.1580(3) 0.0399(14) Uani 1 1 d . . . H67 H 0.3466 1.2154 0.1539 0.048 Uiso 1 1 calc R . . C68 C 0.3802(3) 1.1155(3) 0.1276(3) 0.0431(14) Uani 1 1 d . . . C69 C 0.3773(2) 1.0358(3) 0.1330(2) 0.0371(12) Uani 1 1 d . . . H69 H 0.4016 1.0041 0.1124 0.045 Uiso 1 1 calc R . . C70 C 0.3335(2) 0.9176(3) 0.1754(2) 0.0360(12) Uani 1 1 d . . . C71 C 0.2648(3) 1.1814(4) 0.2266(3) 0.0401(14) Uani 1 1 d . . . C72 C 0.4388(3) 1.1107(5) 0.0462(3) 0.070(2) Uani 1 1 d . . . H72A H 0.4687 1.0718 0.0651 0.105 Uiso 1 1 calc R . . H72B H 0.4596 1.1449 0.0220 0.105 Uiso 1 1 calc R . . H72C H 0.4026 1.0865 0.0196 0.105 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 0.0609(2) 0.0253(2) 0.0467(2) -0.00112(17) 0.03290(19) 0.0020(2) Cd2 0.0628(3) 0.0279(2) 0.0602(3) 0.0063(2) 0.0387(2) -0.0020(2) Cd3 0.0578(2) 0.0284(2) 0.0490(2) -0.00445(19) 0.03269(19) 0.0004(2) Cd4 0.0482(2) 0.0273(2) 0.0453(2) 0.00281(19) 0.02639(17) -0.00043(19) O1 0.075(3) 0.030(2) 0.054(2) 0.004(2) 0.023(2) -0.011(2) O2 0.077(3) 0.030(3) 0.065(3) -0.0028(19) 0.040(2) -0.0003(19) O3 0.104(4) 0.040(3) 0.086(3) -0.003(2) 0.072(3) -0.011(2) O4 0.094(3) 0.035(3) 0.066(3) 0.003(2) 0.042(2) -0.013(2) O5 0.116(4) 0.045(3) 0.109(4) 0.013(3) 0.096(3) 0.020(3) O6 0.068(3) 0.034(2) 0.052(2) -0.0015(18) 0.030(2) 0.014(2) O7 0.109(4) 0.032(3) 0.090(3) 0.011(2) 0.077(3) 0.006(2) O8 0.081(3) 0.052(3) 0.066(3) -0.004(2) 0.054(2) 0.007(2) O9 0.116(4) 0.034(3) 0.120(4) -0.019(3) 0.084(3) 0.002(2) O10 0.083(3) 0.037(3) 0.073(3) 0.004(2) 0.053(3) -0.006(2) O11 0.046(2) 0.025(2) 0.041(2) 0.0003(15) 0.0223(17) -0.0006(15) O12 0.090(3) 0.026(3) 0.075(3) -0.0070(18) 0.052(2) 0.0014(19) O13 0.075(3) 0.029(2) 0.045(2) 0.0032(19) 0.0275(19) -0.006(2) O14 0.073(3) 0.038(3) 0.065(3) 0.004(2) 0.049(2) -0.008(2) O15 0.076(3) 0.031(3) 0.056(2) 0.0001(19) 0.0271(19) -0.010(2) O16 0.143(5) 0.052(3) 0.144(5) -0.009(3) 0.121(4) 0.008(3) O17 0.069(3) 0.035(2) 0.055(2) -0.001(2) 0.030(2) 0.006(2) O18 0.068(3) 0.029(3) 0.054(2) 0.0013(17) 0.026(2) 0.0026(17) O19 0.068(3) 0.039(3) 0.062(3) -0.006(2) 0.043(2) 0.002(2) O20 0.084(3) 0.031(2) 0.064(2) -0.005(2) 0.036(2) 0.009(2) O21 0.092(3) 0.048(3) 0.076(3) 0.001(2) 0.060(3) -0.012(2) O22 0.048(2) 0.068(3) 0.073(3) 0.002(2) 0.019(2) 0.007(2) O23 0.040(3) 0.043(3) 0.034(3) 0.000 0.021(2) 0.000 O24 0.046(3) 0.043(3) 0.035(3) 0.000 0.021(2) 0.000 O25 0.069(2) 0.044(3) 0.053(2) -0.0005(19) 0.030(2) 0.009(2) O26 0.068(3) 0.065(3) 0.071(3) -0.001(2) 0.017(2) -0.009(2) O27 0.081(3) 0.051(3) 0.059(2) 0.000(2) 0.032(2) -0.014(2) O28 0.074(3) 0.049(3) 0.064(3) -0.009(2) 0.011(2) 0.003(2) O29 0.069(2) 0.040(2) 0.050(2) -0.002(2) 0.0307(18) 0.012(2) O30 0.067(2) 0.034(2) 0.049(2) 0.006(2) 0.0239(18) -0.008(2) O31 0.086(3) 0.065(4) 0.071(3) 0.007(2) 0.018(2) -0.002(2) O32 0.189(7) 0.092(5) 0.135(5) 0.024(4) 0.100(5) 0.029(5) O33 0.108(4) 0.076(4) 0.111(4) 0.029(3) 0.057(3) 0.023(3) O34 0.196(9) 0.250(12) 0.207(9) 0.071(8) 0.047(7) 0.078(9) N1 0.060(3) 0.033(3) 0.040(3) -0.004(2) 0.027(2) 0.001(2) N2 0.053(3) 0.039(4) 0.055(3) 0.000(2) 0.036(2) -0.003(2) N3 0.054(3) 0.030(3) 0.048(3) -0.0009(18) 0.030(2) -0.0014(18) N4 0.052(3) 0.041(3) 0.046(3) 0.004(2) 0.031(2) -0.005(2) N5 0.050(3) 0.038(3) 0.043(3) 0.003(2) 0.024(2) 0.002(2) N6 0.053(3) 0.047(3) 0.055(3) -0.004(3) 0.033(2) 0.005(3) N7 0.055(3) 0.036(3) 0.045(3) -0.004(2) 0.025(2) -0.002(2) N8 0.051(2) 0.046(3) 0.049(3) 0.001(3) 0.030(2) 0.000(3) N9 0.053(3) 0.040(3) 0.039(2) 0.0024(18) 0.017(2) 0.000(2) N10 0.063(4) 0.108(6) 0.087(4) -0.009(4) -0.008(3) 0.012(4) N11 0.060(4) 0.103(5) 0.096(5) -0.015(4) 0.004(4) 0.017(4) C53 0.075(5) 0.058(5) 0.119(7) -0.019(5) 0.056(5) -0.015(4) C1 0.058(3) 0.030(3) 0.043(3) 0.002(2) 0.028(3) 0.000(3) C2 0.064(4) 0.035(4) 0.046(3) -0.003(3) 0.030(3) 0.007(3) C3 0.074(4) 0.034(4) 0.068(4) 0.002(3) 0.035(3) 0.006(3) C4 0.070(4) 0.034(3) 0.056(4) 0.004(3) 0.038(3) 0.004(3) C5 0.040(3) 0.033(3) 0.032(3) -0.003(2) 0.013(2) -0.001(2) C6 0.037(3) 0.038(3) 0.035(3) 0.007(2) 0.017(2) -0.005(2) C7 0.039(3) 0.032(3) 0.038(3) 0.002(2) 0.021(2) 0.002(2) C8 0.039(3) 0.037(3) 0.031(3) 0.004(2) 0.015(2) -0.002(2) C9 0.057(3) 0.034(3) 0.051(3) -0.005(3) 0.029(3) -0.002(3) C10 0.071(4) 0.027(3) 0.065(4) -0.003(3) 0.032(3) -0.010(3) C11 0.057(3) 0.036(3) 0.046(3) 0.009(3) 0.028(3) -0.008(3) C12 0.052(3) 0.027(3) 0.050(3) 0.012(2) 0.029(3) 0.005(2) C13 0.044(3) 0.023(3) 0.032(3) -0.002(2) 0.016(2) 0.006(2) C14 0.046(3) 0.035(3) 0.034(3) 0.001(2) 0.020(2) 0.002(2) C15 0.044(3) 0.026(3) 0.031(3) -0.003(2) 0.017(2) 0.005(2) C16 0.046(3) 0.031(3) 0.044(3) -0.003(2) 0.020(3) 0.003(2) C17 0.046(3) 0.036(3) 0.042(3) 0.002(3) 0.021(3) -0.004(3) C18 0.039(3) 0.031(3) 0.039(3) -0.007(2) 0.018(2) -0.001(2) C19 0.064(4) 0.027(3) 0.037(3) 0.000(3) 0.020(3) 0.008(3) C20 0.048(3) 0.045(4) 0.042(3) -0.008(3) 0.022(3) 0.010(3) C21 0.064(4) 0.062(5) 0.064(4) 0.010(3) 0.042(3) 0.000(3) C22 0.039(3) 0.026(3) 0.036(3) 0.004(2) 0.013(2) -0.002(2) C23 0.046(3) 0.032(3) 0.042(3) 0.003(2) 0.026(3) 0.003(2) C24 0.046(3) 0.033(3) 0.035(3) 0.005(2) 0.015(3) 0.001(2) C25 0.062(4) 0.036(4) 0.050(4) 0.004(3) 0.033(3) 0.000(3) C26 0.060(4) 0.032(3) 0.055(4) 0.009(3) 0.031(3) 0.008(3) C27 0.043(3) 0.037(3) 0.039(3) 0.009(2) 0.022(2) 0.002(2) C28 0.049(3) 0.032(3) 0.038(3) 0.001(2) 0.013(3) -0.002(2) C29 0.058(4) 0.032(4) 0.041(3) 0.001(3) 0.020(3) -0.008(3) C30 0.096(6) 0.103(7) 0.074(5) 0.016(5) 0.056(5) 0.021(5) C31 0.063(4) 0.033(3) 0.045(3) -0.006(3) 0.032(3) 0.001(3) C32 0.062(4) 0.035(4) 0.054(4) -0.006(3) 0.031(3) 0.004(3) C33 0.070(4) 0.033(3) 0.065(4) 0.008(3) 0.033(3) 0.009(3) C34 0.068(4) 0.037(4) 0.058(4) 0.005(3) 0.030(3) 0.003(3) C35 0.038(3) 0.049(4) 0.033(3) -0.005(3) 0.015(2) 0.000(3) C36 0.038(3) 0.047(4) 0.032(3) -0.001(3) 0.012(2) -0.003(3) C37 0.050(3) 0.034(3) 0.040(3) 0.004(2) 0.022(3) 0.001(2) C38 0.052(4) 0.038(4) 0.049(4) 0.003(3) 0.025(3) -0.004(3) C39 0.062(4) 0.033(3) 0.057(4) -0.007(3) 0.027(3) -0.005(3) C40 0.052(3) 0.040(4) 0.048(3) -0.004(3) 0.026(3) 0.010(3) C41 0.031(3) 0.045(4) 0.034(3) 0.003(2) 0.013(2) 0.000(2) C42 0.039(3) 0.037(4) 0.036(3) -0.001(2) 0.016(2) 0.003(2) C43 0.065(4) 0.037(3) 0.046(3) 0.004(3) 0.018(3) -0.006(3) C44 0.073(4) 0.051(5) 0.058(4) -0.004(3) 0.030(3) -0.008(3) C45 0.095(5) 0.075(5) 0.045(4) -0.007(3) 0.010(4) -0.023(4) C46 0.071(4) 0.088(5) 0.053(4) 0.010(4) 0.002(3) -0.011(4) C47 0.056(4) 0.044(4) 0.050(3) -0.004(3) 0.003(3) -0.006(3) C48 0.050(4) 0.047(4) 0.056(4) 0.002(3) -0.001(3) -0.002(3) C49 0.044(4) 0.064(5) 0.085(5) -0.008(4) 0.012(4) 0.004(3) C50 0.059(4) 0.063(5) 0.106(6) -0.012(4) 0.037(4) 0.004(4) C51 0.087(6) 0.144(9) 0.095(6) 0.037(6) 0.045(5) 0.032(6) N12 0.151(8) 0.162(9) 0.123(7) 0.028(6) 0.066(6) 0.052(7) C52 0.131(8) 0.090(7) 0.154(10) 0.013(7) 0.096(8) 0.029(6) C54 0.067(5) 0.073(6) 0.149(8) -0.041(5) 0.049(5) -0.022(4) C55 0.042(3) 0.030(3) 0.037(3) 0.001(2) 0.014(2) 0.000(2) C56 0.041(3) 0.025(3) 0.032(3) -0.002(2) 0.018(2) -0.001(2) C57 0.041(3) 0.028(3) 0.036(3) -0.003(2) 0.012(2) 0.001(2) C58 0.049(3) 0.036(3) 0.043(3) 0.005(2) 0.025(3) -0.005(2) C59 0.060(4) 0.040(4) 0.062(4) 0.000(3) 0.039(3) 0.010(3) C60 0.068(4) 0.025(3) 0.062(4) -0.004(3) 0.040(3) -0.001(3) C61 0.045(3) 0.036(4) 0.036(3) 0.003(2) 0.015(2) -0.008(3) C62 0.049(3) 0.025(3) 0.047(3) 0.003(3) 0.018(3) 0.000(3) C63 0.101(6) 0.107(8) 0.104(7) -0.018(5) 0.074(5) -0.021(5) C64 0.038(3) 0.034(3) 0.031(3) -0.004(2) 0.010(2) -0.002(2) C65 0.047(3) 0.029(3) 0.029(3) 0.001(2) 0.016(2) -0.001(2) C66 0.042(3) 0.031(3) 0.032(3) -0.002(2) 0.015(2) -0.002(2) C67 0.054(3) 0.031(3) 0.040(3) -0.003(2) 0.020(3) -0.002(3) C68 0.053(4) 0.036(4) 0.048(3) 0.000(3) 0.028(3) -0.007(3) C69 0.039(3) 0.036(3) 0.042(3) -0.006(2) 0.021(2) 0.004(2) C70 0.044(3) 0.028(3) 0.038(3) 0.000(2) 0.013(2) 0.001(2) C71 0.049(3) 0.038(4) 0.035(3) -0.002(3) 0.013(3) 0.008(3) C72 0.068(5) 0.090(6) 0.063(5) 0.015(4) 0.040(4) 0.007(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O2 2.234(4) . ? Cd1 O3 2.251(4) 4_456 ? Cd1 O26 2.328(4) . ? Cd1 N1 2.346(5) . ? Cd1 O25 2.354(4) . ? Cd1 O4 2.569(4) 4_456 ? Cd2 O7 2.213(4) . ? Cd2 O9 2.273(4) 4 ? Cd2 N4 2.324(5) . ? Cd2 O27 2.369(4) . ? Cd2 O31 2.451(4) . ? Cd2 O8 2.479(4) 4 ? Cd2 C20 2.729(6) 4 ? Cd3 O19 2.269(4) 1_545 ? Cd3 O12 2.283(4) . ? Cd3 O28 2.309(4) . ? Cd3 O29 2.334(4) . ? Cd3 N7 2.366(5) . ? Cd3 O20 2.524(4) 1_545 ? Cd3 O13 2.548(4) . ? Cd3 C71 2.743(6) 1_545 ? Cd3 C62 2.759(6) . ? Cd4 O18 2.259(3) . ? Cd4 O14 2.308(4) . ? Cd4 O30 2.324(4) . ? Cd4 N9 2.331(4) . ? Cd4 N5 2.342(5) . ? Cd4 O15 2.543(4) . ? O1 C28 1.256(7) . ? O2 C28 1.266(7) . ? O3 C29 1.255(7) . ? O3 Cd1 2.251(4) 4_446 ? O4 C29 1.240(7) . ? O4 Cd1 2.569(4) 4_446 ? O5 C30 1.377(8) . ? O5 C26 1.377(7) . ? O6 C19 1.257(6) . ? O7 C19 1.262(7) . ? O8 C20 1.233(8) . ? O8 Cd2 2.479(4) 4_545 ? O9 C20 1.249(7) . ? O9 Cd2 2.273(4) 4_545 ? O10 C17 1.371(6) . ? O10 C21 1.404(7) . ? O11 C7 1.359(6) . ? O11 C6 1.360(6) . ? O12 C62 1.271(6) . ? O13 C62 1.243(6) . ? O14 C61 1.242(7) . ? O15 C61 1.236(7) . ? O16 C59 1.356(7) . ? O16 C63 1.370(9) . ? O17 C70 1.243(6) . ? O18 C70 1.270(6) . ? O19 C71 1.246(7) . ? O19 Cd3 2.269(4) 1_565 ? O20 C71 1.245(7) . ? O20 Cd3 2.524(4) 1_565 ? O21 C68 1.365(7) . ? O21 C72 1.402(8) . ? O22 C48 1.350(7) . ? O22 C49 1.363(7) . ? O23 C42 1.342(6) . ? O23 C42 1.342(6) 2_655 ? O24 C36 1.330(7) . ? O24 C36 1.330(7) 2_556 ? O25 H25A 0.8500 . ? O25 H25B 0.8499 . ? O26 H26A 0.8504 . ? O26 H26B 0.8519 . ? O27 H27A 0.8501 . ? O27 H27B 0.8500 . ? O28 H28A 0.8501 . ? O28 H28B 0.8500 . ? O29 H29A 0.8500 . ? O29 H29B 0.8498 . ? O30 H30A 0.8500 . ? O30 H30B 0.8503 . ? O31 H31A 0.8502 . ? O31 H31B 0.8519 . ? N1 C1 1.336(6) . ? N1 C2 1.337(7) . ? N2 C6 1.283(7) . ? N2 N3 1.409(5) . ? N3 C7 1.283(7) . ? N4 C11 1.316(7) . ? N4 C12 1.348(6) . ? N5 C37 1.326(7) . ? N5 C38 1.352(8) . ? N6 C42 1.280(8) . ? N6 N6 1.408(8) 2_655 ? N7 C32 1.333(8) . ? N7 C31 1.342(7) . ? N8 C36 1.289(8) . ? N8 N8 1.393(8) 2_556 ? N9 C44 1.320(7) . ? N9 C43 1.341(7) . ? N10 C48 1.255(7) . ? N10 N11 1.411(8) . ? N11 C49 1.251(8) . ? C53 C52 1.332(12) . ? C53 C54 1.356(11) . ? C53 H53 0.9300 . ? C1 C5 1.369(7) . ? C1 H1 0.9300 . ? C2 C3 1.367(8) . ? C2 H2 0.9300 . ? C3 C4 1.351(7) . ? C3 H3 0.9300 . ? C4 C5 1.375(8) . ? C4 H4 0.9300 . ? C5 C6 1.460(7) . ? C7 C8 1.450(7) . ? C8 C9 1.367(8) . ? C8 C12 1.384(7) . ? C9 C10 1.388(8) . ? C9 H9 0.9300 . ? C10 C11 1.380(8) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C18 1.378(7) . ? C13 C14 1.387(7) . ? C13 C19 1.476(8) . ? C14 C15 1.366(7) . ? C14 H14 0.9300 . ? C15 C16 1.393(7) . ? C15 C20 1.495(7) . ? C16 C17 1.380(7) . ? C16 H16 0.9300 . ? C17 C18 1.376(8) . ? C18 H18 0.9300 . ? C20 Cd2 2.729(6) 4_545 ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 C23 1.380(7) . ? C22 C27 1.388(7) . ? C22 C28 1.471(7) . ? C23 C24 1.373(8) . ? C23 H23 0.9300 . ? C24 C25 1.366(8) . ? C24 C29 1.502(8) . ? C25 C26 1.415(8) . ? C25 H25 0.9300 . ? C26 C27 1.347(8) . ? C27 H27 0.9300 . ? C30 H30' 0.9600 . ? C30 H30" 0.9600 . ? C30 H30C 0.9600 . ? C31 C35 1.377(8) . ? C31 H31 0.9300 . ? C32 C33 1.376(9) . ? C32 H32 0.9300 . ? C33 C34 1.371(8) . ? C33 H33 0.9300 . ? C34 C35 1.385(9) . ? C34 H34 0.9300 . ? C35 C36 1.476(8) . ? C37 C41 1.377(7) . ? C37 H37 0.9300 . ? C38 C39 1.346(8) . ? C38 H38 0.9300 . ? C39 C40 1.374(8) . ? C39 H39 0.9300 . ? C40 C41 1.394(8) . ? C40 H40 0.9300 . ? C41 C42 1.450(7) . ? C43 C47 1.397(8) . ? C43 H43 0.9300 . ? C44 C45 1.402(9) . ? C44 H44 0.9300 . ? C45 C46 1.373(9) . ? C45 H45 0.9300 . ? C46 C47 1.384(8) . ? C46 H46 0.9300 . ? C47 C48 1.452(8) . ? C49 C50 1.490(10) . ? C50 C51 1.368(10) . ? C50 C54 1.378(9) . ? C51 N12 1.355(10) . ? C51 H51 0.9300 . ? N12 C52 1.337(12) . ? C52 H52 0.9300 . ? C54 H54 0.9300 . ? C55 C60 1.379(7) . ? C55 C56 1.386(8) . ? C55 C61 1.506(7) . ? C56 C57 1.391(7) . ? C56 H56 0.9300 . ? C57 C58 1.391(7) . ? C57 C62 1.499(8) . ? C58 C59 1.381(8) . ? C58 H58 0.9300 . ? C59 C60 1.386(8) . ? C60 H60 0.9300 . ? C63 H63A 0.9600 . ? C63 H63B 0.9600 . ? C63 H63C 0.9600 . ? C64 C65 1.367(7) . ? C64 C69 1.389(7) . ? C64 C70 1.510(7) . ? C65 C66 1.382(8) . ? C65 H65 0.9300 . ? C66 C67 1.375(7) . ? C66 C71 1.499(7) . ? C67 C68 1.368(8) . ? C67 H67 0.9300 . ? C68 C69 1.388(8) . ? C69 H69 0.9300 . ? C71 Cd3 2.743(6) 1_565 ? C72 H72A 0.9600 . ? C72 H72B 0.9600 . ? C72 H72C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Cd1 O3 140.99(15) . 4_456 ? O2 Cd1 O26 85.83(16) . . ? O3 Cd1 O26 94.06(19) 4_456 . ? O2 Cd1 N1 136.11(15) . . ? O3 Cd1 N1 82.91(16) 4_456 . ? O26 Cd1 N1 92.15(16) . . ? O2 Cd1 O25 90.62(15) . . ? O3 Cd1 O25 91.89(17) 4_456 . ? O26 Cd1 O25 173.82(15) . . ? N1 Cd1 O25 86.91(15) . . ? O2 Cd1 O4 88.05(14) . 4_456 ? O3 Cd1 O4 53.02(15) 4_456 4_456 ? O26 Cd1 O4 94.58(15) . 4_456 ? N1 Cd1 O4 135.74(15) . 4_456 ? O25 Cd1 O4 90.35(14) . 4_456 ? O7 Cd2 O9 87.05(16) . 4 ? O7 Cd2 N4 137.22(16) . . ? O9 Cd2 N4 135.71(16) 4 . ? O7 Cd2 O27 87.77(18) . . ? O9 Cd2 O27 89.95(17) 4 . ? N4 Cd2 O27 92.48(17) . . ? O7 Cd2 O31 85.79(17) . . ? O9 Cd2 O31 106.17(18) 4 . ? N4 Cd2 O31 81.22(17) . . ? O27 Cd2 O31 162.27(14) . . ? O7 Cd2 O8 140.86(16) . 4 ? O9 Cd2 O8 53.82(15) 4 4 ? N4 Cd2 O8 81.90(16) . 4 ? O27 Cd2 O8 92.23(15) . 4 ? O31 Cd2 O8 103.16(15) . 4 ? O7 Cd2 C20 114.03(17) . 4 ? O9 Cd2 C20 26.98(17) 4 4 ? N4 Cd2 C20 108.73(18) . 4 ? O27 Cd2 C20 90.87(16) . 4 ? O31 Cd2 C20 106.83(16) . 4 ? O8 Cd2 C20 26.84(17) 4 4 ? O19 Cd3 O12 134.96(15) 1_545 . ? O19 Cd3 O28 92.49(16) 1_545 . ? O12 Cd3 O28 86.83(16) . . ? O19 Cd3 O29 95.48(16) 1_545 . ? O12 Cd3 O29 87.70(17) . . ? O28 Cd3 O29 172.03(15) . . ? O19 Cd3 N7 85.15(15) 1_545 . ? O12 Cd3 N7 139.88(16) . . ? O28 Cd3 N7 91.39(17) . . ? O29 Cd3 N7 89.06(17) . . ? O19 Cd3 O20 53.63(14) 1_545 1_545 ? O12 Cd3 O20 81.34(14) . 1_545 ? O28 Cd3 O20 90.71(14) . 1_545 ? O29 Cd3 O20 94.20(13) . 1_545 ? N7 Cd3 O20 138.78(16) . 1_545 ? O19 Cd3 O13 169.75(14) 1_545 . ? O12 Cd3 O13 53.81(13) . . ? O28 Cd3 O13 82.21(13) . . ? O29 Cd3 O13 89.88(14) . . ? N7 Cd3 O13 86.22(15) . . ? O20 Cd3 O13 134.78(13) 1_545 . ? O19 Cd3 C71 26.71(17) 1_545 1_545 ? O12 Cd3 C71 108.26(16) . 1_545 ? O28 Cd3 C71 91.05(15) . 1_545 ? O29 Cd3 C71 96.17(15) . 1_545 ? N7 Cd3 C71 111.85(18) . 1_545 ? O20 Cd3 C71 26.95(15) 1_545 1_545 ? O13 Cd3 C71 160.95(15) . 1_545 ? O19 Cd3 C62 161.26(15) 1_545 . ? O12 Cd3 C62 27.15(14) . . ? O28 Cd3 C62 82.58(15) . . ? O29 Cd3 C62 89.92(16) . . ? N7 Cd3 C62 112.93(16) . . ? O20 Cd3 C62 108.16(14) 1_545 . ? O13 Cd3 C62 26.71(13) . . ? C71 Cd3 C62 134.87(17) 1_545 . ? O18 Cd4 O14 138.95(15) . . ? O18 Cd4 O30 89.29(16) . . ? O14 Cd4 O30 89.97(16) . . ? O18 Cd4 N9 84.96(15) . . ? O14 Cd4 N9 92.52(16) . . ? O30 Cd4 N9 173.60(15) . . ? O18 Cd4 N5 137.16(15) . . ? O14 Cd4 N5 83.89(15) . . ? O30 Cd4 N5 91.78(16) . . ? N9 Cd4 N5 94.35(16) . . ? O18 Cd4 O15 86.23(13) . . ? O14 Cd4 O15 52.73(14) . . ? O30 Cd4 O15 87.54(12) . . ? N9 Cd4 O15 89.28(14) . . ? N5 Cd4 O15 136.61(15) . . ? C28 O2 Cd1 103.6(3) . . ? C29 O3 Cd1 100.3(4) . 4_446 ? C29 O4 Cd1 85.7(3) . 4_446 ? C30 O5 C26 116.9(5) . . ? C19 O7 Cd2 105.5(4) . . ? C20 O8 Cd2 88.0(4) . 4_545 ? C20 O9 Cd2 97.3(4) . 4_545 ? C17 O10 C21 117.0(5) . . ? C7 O11 C6 102.4(4) . . ? C62 O12 Cd3 97.8(3) . . ? C62 O13 Cd3 86.1(3) . . ? C61 O14 Cd4 98.3(4) . . ? C61 O15 Cd4 87.3(3) . . ? C59 O16 C63 121.3(6) . . ? C70 O18 Cd4 102.4(3) . . ? C71 O19 Cd3 98.4(4) . 1_565 ? C71 O20 Cd3 86.4(3) . 1_565 ? C68 O21 C72 117.9(5) . . ? C48 O22 C49 101.9(5) . . ? C42 O23 C42 103.7(6) . 2_655 ? C36 O24 C36 102.4(7) . 2_556 ? Cd1 O25 H25A 118.5 . . ? Cd1 O25 H25B 98.3 . . ? H25A O25 H25B 118.0 . . ? Cd1 O26 H26A 100.7 . . ? Cd1 O26 H26B 134.2 . . ? H26A O26 H26B 116.4 . . ? Cd2 O27 H27A 136.3 . . ? Cd2 O27 H27B 104.4 . . ? H27A O27 H27B 105.6 . . ? Cd3 O28 H28A 111.4 . . ? Cd3 O28 H28B 93.6 . . ? H28A O28 H28B 116.6 . . ? Cd3 O29 H29A 105.9 . . ? Cd3 O29 H29B 104.2 . . ? H29A O29 H29B 116.6 . . ? Cd4 O30 H30A 110.0 . . ? Cd4 O30 H30B 95.2 . . ? H30A O30 H30B 117.4 . . ? Cd2 O31 H31A 153.8 . . ? Cd2 O31 H31B 70.9 . . ? H31A O31 H31B 117.9 . . ? C1 N1 C2 117.5(5) . . ? C1 N1 Cd1 121.6(4) . . ? C2 N1 Cd1 120.9(4) . . ? C6 N2 N3 105.6(4) . . ? C7 N3 N2 106.4(4) . . ? C11 N4 C12 119.3(5) . . ? C11 N4 Cd2 120.4(3) . . ? C12 N4 Cd2 120.1(4) . . ? C37 N5 C38 117.3(5) . . ? C37 N5 Cd4 121.6(4) . . ? C38 N5 Cd4 121.0(4) . . ? C42 N6 N6 105.9(3) . 2_655 ? C32 N7 C31 116.9(5) . . ? C32 N7 Cd3 120.8(4) . . ? C31 N7 Cd3 122.3(4) . . ? C36 N8 N8 105.3(3) . 2_556 ? C44 N9 C43 118.2(5) . . ? C44 N9 Cd4 126.1(4) . . ? C43 N9 Cd4 115.7(3) . . ? C48 N10 N11 106.4(6) . . ? C49 N11 N10 105.8(6) . . ? C52 C53 C54 120.5(8) . . ? C52 C53 H53 119.7 . . ? C54 C53 H53 119.7 . . ? N1 C1 C5 122.4(5) . . ? N1 C1 H1 118.8 . . ? C5 C1 H1 118.8 . . ? N1 C2 C3 122.9(5) . . ? N1 C2 H2 118.6 . . ? C3 C2 H2 118.6 . . ? C4 C3 C2 119.1(6) . . ? C4 C3 H3 120.5 . . ? C2 C3 H3 120.5 . . ? C3 C4 C5 119.2(5) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? C1 C5 C4 118.9(5) . . ? C1 C5 C6 118.4(5) . . ? C4 C5 C6 122.6(5) . . ? N2 C6 O11 113.0(4) . . ? N2 C6 C5 129.8(5) . . ? O11 C6 C5 117.1(5) . . ? N3 C7 O11 112.5(4) . . ? N3 C7 C8 130.1(5) . . ? O11 C7 C8 117.4(5) . . ? C9 C8 C12 119.9(5) . . ? C9 C8 C7 120.5(5) . . ? C12 C8 C7 119.5(5) . . ? C8 C9 C10 118.6(5) . . ? C8 C9 H9 120.7 . . ? C10 C9 H9 120.7 . . ? C11 C10 C9 118.6(5) . . ? C11 C10 H10 120.7 . . ? C9 C10 H10 120.7 . . ? N4 C11 C10 122.6(5) . . ? N4 C11 H11 118.7 . . ? C10 C11 H11 118.7 . . ? N4 C12 C8 120.9(5) . . ? N4 C12 H12 119.5 . . ? C8 C12 H12 119.5 . . ? C18 C13 C14 119.2(5) . . ? C18 C13 C19 120.8(4) . . ? C14 C13 C19 120.0(5) . . ? C15 C14 C13 120.6(5) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C14 C15 C16 120.1(5) . . ? C14 C15 C20 120.2(5) . . ? C16 C15 C20 119.6(5) . . ? C17 C16 C15 119.3(5) . . ? C17 C16 H16 120.3 . . ? C15 C16 H16 120.3 . . ? O10 C17 C18 124.2(5) . . ? O10 C17 C16 115.5(5) . . ? C18 C17 C16 120.2(5) . . ? C17 C18 C13 120.5(4) . . ? C17 C18 H18 119.7 . . ? C13 C18 H18 119.7 . . ? O6 C19 O7 120.6(6) . . ? O6 C19 C13 121.0(5) . . ? O7 C19 C13 118.3(5) . . ? O8 C20 O9 120.9(5) . . ? O8 C20 C15 120.2(6) . . ? O9 C20 C15 119.0(5) . . ? O8 C20 Cd2 65.2(3) . 4_545 ? O9 C20 Cd2 55.7(3) . 4_545 ? C15 C20 Cd2 174.6(4) . 4_545 ? O10 C21 H21A 109.5 . . ? O10 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? O10 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 C27 118.4(5) . . ? C23 C22 C28 120.6(5) . . ? C27 C22 C28 121.0(5) . . ? C24 C23 C22 121.1(5) . . ? C24 C23 H23 119.4 . . ? C22 C23 H23 119.4 . . ? C25 C24 C23 120.1(5) . . ? C25 C24 C29 119.4(5) . . ? C23 C24 C29 120.5(5) . . ? C24 C25 C26 119.1(6) . . ? C24 C25 H25 120.5 . . ? C26 C25 H25 120.5 . . ? C27 C26 O5 124.9(5) . . ? C27 C26 C25 119.8(5) . . ? O5 C26 C25 115.2(5) . . ? C26 C27 C22 121.3(5) . . ? C26 C27 H27 119.4 . . ? C22 C27 H27 119.4 . . ? O1 C28 O2 120.2(5) . . ? O1 C28 C22 121.2(5) . . ? O2 C28 C22 118.6(5) . . ? O4 C29 O3 120.9(5) . . ? O4 C29 C24 121.7(5) . . ? O3 C29 C24 117.4(5) . . ? O5 C30 H30' 109.5 . . ? O5 C30 H30" 109.5 . . ? H30' C30 H30" 109.5 . . ? O5 C30 H30C 109.5 . . ? H30' C30 H30C 109.5 . . ? H30" C30 H30C 109.5 . . ? N7 C31 C35 123.7(6) . . ? N7 C31 H31 118.1 . . ? C35 C31 H31 118.1 . . ? N7 C32 C33 122.9(6) . . ? N7 C32 H32 118.5 . . ? C33 C32 H32 118.5 . . ? C34 C33 C32 119.8(6) . . ? C34 C33 H33 120.1 . . ? C32 C33 H33 120.1 . . ? C33 C34 C35 118.2(6) . . ? C33 C34 H34 120.9 . . ? C35 C34 H34 120.9 . . ? C31 C35 C34 118.4(5) . . ? C31 C35 C36 120.6(6) . . ? C34 C35 C36 121.0(5) . . ? N8 C36 O24 113.5(5) . . ? N8 C36 C35 127.8(5) . . ? O24 C36 C35 118.5(6) . . ? N5 C37 C41 123.4(5) . . ? N5 C37 H37 118.3 . . ? C41 C37 H37 118.3 . . ? C39 C38 N5 122.8(5) . . ? C39 C38 H38 118.6 . . ? N5 C38 H38 118.6 . . ? C38 C39 C40 120.3(6) . . ? C38 C39 H39 119.9 . . ? C40 C39 H39 119.9 . . ? C39 C40 C41 117.8(5) . . ? C39 C40 H40 121.1 . . ? C41 C40 H40 121.1 . . ? C37 C41 C40 118.3(5) . . ? C37 C41 C42 120.2(5) . . ? C40 C41 C42 121.3(5) . . ? N6 C42 O23 112.2(5) . . ? N6 C42 C41 128.5(5) . . ? O23 C42 C41 119.2(5) . . ? N9 C43 C47 123.3(5) . . ? N9 C43 H43 118.3 . . ? C47 C43 H43 118.3 . . ? N9 C44 C45 122.8(6) . . ? N9 C44 H44 118.6 . . ? C45 C44 H44 118.6 . . ? C46 C45 C44 118.3(6) . . ? C46 C45 H45 120.9 . . ? C44 C45 H45 120.9 . . ? C45 C46 C47 120.1(6) . . ? C45 C46 H46 120.0 . . ? C47 C46 H46 120.0 . . ? C46 C47 C43 117.3(6) . . ? C46 C47 C48 123.1(6) . . ? C43 C47 C48 119.6(5) . . ? N10 C48 O22 112.9(6) . . ? N10 C48 C47 129.8(6) . . ? O22 C48 C47 117.3(5) . . ? N11 C49 O22 113.1(6) . . ? N11 C49 C50 130.5(6) . . ? O22 C49 C50 116.4(6) . . ? C51 C50 C54 120.0(8) . . ? C51 C50 C49 120.1(6) . . ? C54 C50 C49 119.8(7) . . ? N12 C51 C50 119.8(8) . . ? N12 C51 H51 120.1 . . ? C50 C51 H51 120.1 . . ? C52 N12 C51 119.2(9) . . ? C53 C52 N12 122.0(9) . . ? C53 C52 H52 119.0 . . ? N12 C52 H52 119.0 . . ? C53 C54 C50 118.3(8) . . ? C53 C54 H54 120.8 . . ? C50 C54 H54 120.8 . . ? C60 C55 C56 120.8(5) . . ? C60 C55 C61 120.7(5) . . ? C56 C55 C61 118.5(5) . . ? C55 C56 C57 119.1(4) . . ? C55 C56 H56 120.4 . . ? C57 C56 H56 120.4 . . ? C58 C57 C56 120.9(5) . . ? C58 C57 C62 118.7(4) . . ? C56 C57 C62 120.4(4) . . ? C59 C58 C57 118.5(5) . . ? C59 C58 H58 120.7 . . ? C57 C58 H58 120.7 . . ? O16 C59 C58 122.9(5) . . ? O16 C59 C60 115.7(6) . . ? C58 C59 C60 121.5(5) . . ? C55 C60 C59 119.2(6) . . ? C55 C60 H60 120.4 . . ? C59 C60 H60 120.4 . . ? O15 C61 O14 121.7(5) . . ? O15 C61 C55 119.9(5) . . ? O14 C61 C55 118.3(6) . . ? O13 C62 O12 122.0(5) . . ? O13 C62 C57 120.5(5) . . ? O12 C62 C57 117.5(4) . . ? O13 C62 Cd3 67.1(3) . . ? O12 C62 Cd3 55.1(3) . . ? C57 C62 Cd3 171.9(3) . . ? O16 C63 H63A 109.5 . . ? O16 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? O16 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C65 C64 C69 120.2(5) . . ? C65 C64 C70 120.5(4) . . ? C69 C64 C70 119.4(4) . . ? C64 C65 C66 120.7(5) . . ? C64 C65 H65 119.7 . . ? C66 C65 H65 119.7 . . ? C67 C66 C65 119.2(5) . . ? C67 C66 C71 120.8(5) . . ? C65 C66 C71 120.0(5) . . ? C68 C67 C66 120.6(6) . . ? C68 C67 H67 119.7 . . ? C66 C67 H67 119.7 . . ? O21 C68 C67 115.7(6) . . ? O21 C68 C69 123.9(5) . . ? C67 C68 C69 120.4(5) . . ? C68 C69 C64 118.9(5) . . ? C68 C69 H69 120.5 . . ? C64 C69 H69 120.5 . . ? O17 C70 O18 121.2(5) . . ? O17 C70 C64 121.4(5) . . ? O18 C70 C64 117.4(4) . . ? O20 C71 O19 121.6(6) . . ? O20 C71 C66 119.8(5) . . ? O19 C71 C66 118.6(6) . . ? O20 C71 Cd3 66.7(3) . 1_565 ? O19 C71 Cd3 54.9(3) . 1_565 ? C66 C71 Cd3 173.3(4) . 1_565 ? O21 C72 H72A 109.5 . . ? O21 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? O21 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 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 O3 Cd1 O2 C28 175.4(4) 4_456 . . . ? O26 Cd1 O2 C28 84.1(4) . . . . ? N1 Cd1 O2 C28 -4.7(5) . . . . ? O25 Cd1 O2 C28 -90.9(4) . . . . ? O4 Cd1 O2 C28 178.8(4) 4_456 . . . ? O9 Cd2 O7 C19 -174.5(4) 4 . . . ? N4 Cd2 O7 C19 6.8(6) . . . . ? O27 Cd2 O7 C19 -84.4(4) . . . . ? O31 Cd2 O7 C19 79.1(4) . . . . ? O8 Cd2 O7 C19 -175.2(3) 4 . . . ? C20 Cd2 O7 C19 -174.4(4) 4 . . . ? O19 Cd3 O12 C62 -170.2(3) 1_545 . . . ? O28 Cd3 O12 C62 -79.9(4) . . . . ? O29 Cd3 O12 C62 94.3(4) . . . . ? N7 Cd3 O12 C62 8.5(5) . . . . ? O20 Cd3 O12 C62 -171.1(4) 1_545 . . . ? O13 Cd3 O12 C62 2.8(3) . . . . ? C71 Cd3 O12 C62 -169.9(4) 1_545 . . . ? O19 Cd3 O13 C62 148.2(8) 1_545 . . . ? O12 Cd3 O13 C62 -2.8(3) . . . . ? O28 Cd3 O13 C62 89.0(3) . . . . ? O29 Cd3 O13 C62 -90.1(3) . . . . ? N7 Cd3 O13 C62 -179.1(4) . . . . ? O20 Cd3 O13 C62 5.7(4) 1_545 . . . ? C71 Cd3 O13 C62 18.8(6) 1_545 . . . ? O18 Cd4 O14 C61 -2.2(5) . . . . ? O30 Cd4 O14 C61 86.7(4) . . . . ? N9 Cd4 O14 C61 -87.4(4) . . . . ? N5 Cd4 O14 C61 178.5(4) . . . . ? O15 Cd4 O14 C61 -0.2(3) . . . . ? O18 Cd4 O15 C61 179.0(3) . . . . ? O14 Cd4 O15 C61 0.2(3) . . . . ? O30 Cd4 O15 C61 -91.6(3) . . . . ? N9 Cd4 O15 C61 94.0(3) . . . . ? N5 Cd4 O15 C61 -1.6(4) . . . . ? O14 Cd4 O18 C70 -174.8(3) . . . . ? O30 Cd4 O18 C70 96.0(4) . . . . ? N9 Cd4 O18 C70 -86.8(4) . . . . ? N5 Cd4 O18 C70 4.2(5) . . . . ? O15 Cd4 O18 C70 -176.4(4) . . . . ? O2 Cd1 N1 C1 -1.3(6) . . . . ? O3 Cd1 N1 C1 178.6(5) 4_456 . . . ? O26 Cd1 N1 C1 -87.5(5) . . . . ? O25 Cd1 N1 C1 86.4(5) . . . . ? O4 Cd1 N1 C1 173.7(4) 4_456 . . . ? O2 Cd1 N1 C2 177.0(4) . . . . ? O3 Cd1 N1 C2 -3.1(5) 4_456 . . . ? O26 Cd1 N1 C2 90.8(5) . . . . ? O25 Cd1 N1 C2 -95.3(5) . . . . ? O4 Cd1 N1 C2 -8.0(6) 4_456 . . . ? C6 N2 N3 C7 0.0(6) . . . . ? O7 Cd2 N4 C11 170.4(4) . . . . ? O9 Cd2 N4 C11 -7.7(6) 4 . . . ? O27 Cd2 N4 C11 -100.2(5) . . . . ? O31 Cd2 N4 C11 96.4(5) . . . . ? O8 Cd2 N4 C11 -8.3(5) 4 . . . ? C20 Cd2 N4 C11 -8.4(5) 4 . . . ? O7 Cd2 N4 C12 -3.9(6) . . . . ? O9 Cd2 N4 C12 177.9(4) 4 . . . ? O27 Cd2 N4 C12 85.5(5) . . . . ? O31 Cd2 N4 C12 -77.9(5) . . . . ? O8 Cd2 N4 C12 177.4(5) 4 . . . ? C20 Cd2 N4 C12 177.2(5) 4 . . . ? O18 Cd4 N5 C37 5.8(6) . . . . ? O14 Cd4 N5 C37 -174.8(5) . . . . ? O30 Cd4 N5 C37 -85.0(5) . . . . ? N9 Cd4 N5 C37 93.1(5) . . . . ? O15 Cd4 N5 C37 -173.3(4) . . . . ? O18 Cd4 N5 C38 -178.1(4) . . . . ? O14 Cd4 N5 C38 1.3(5) . . . . ? O30 Cd4 N5 C38 91.1(5) . . . . ? N9 Cd4 N5 C38 -90.8(5) . . . . ? O15 Cd4 N5 C38 2.8(6) . . . . ? O19 Cd3 N7 C32 2.0(5) 1_545 . . . ? O12 Cd3 N7 C32 -177.1(4) . . . . ? O28 Cd3 N7 C32 -90.4(5) . . . . ? O29 Cd3 N7 C32 97.6(5) . . . . ? O20 Cd3 N7 C32 2.3(7) 1_545 . . . ? O13 Cd3 N7 C32 -172.5(5) . . . . ? C71 Cd3 N7 C32 1.3(6) 1_545 . . . ? C62 Cd3 N7 C32 -172.9(5) . . . . ? O19 Cd3 N7 C31 -178.2(5) 1_545 . . . ? O12 Cd3 N7 C31 2.7(6) . . . . ? O28 Cd3 N7 C31 89.4(5) . . . . ? O29 Cd3 N7 C31 -82.6(5) . . . . ? O20 Cd3 N7 C31 -177.9(4) 1_545 . . . ? O13 Cd3 N7 C31 7.3(5) . . . . ? C71 Cd3 N7 C31 -178.9(5) 1_545 . . . ? C62 Cd3 N7 C31 6.9(5) . . . . ? O18 Cd4 N9 C44 107.6(5) . . . . ? O14 Cd4 N9 C44 -113.5(5) . . . . ? N5 Cd4 N9 C44 -29.4(5) . . . . ? O15 Cd4 N9 C44 -166.1(5) . . . . ? O18 Cd4 N9 C43 -69.6(4) . . . . ? O14 Cd4 N9 C43 69.3(4) . . . . ? N5 Cd4 N9 C43 153.3(4) . . . . ? O15 Cd4 N9 C43 16.6(4) . . . . ? C48 N10 N11 C49 0.4(8) . . . . ? C2 N1 C1 C5 0.8(9) . . . . ? Cd1 N1 C1 C5 179.2(4) . . . . ? C1 N1 C2 C3 -2.6(9) . . . . ? Cd1 N1 C2 C3 179.0(5) . . . . ? N1 C2 C3 C4 2.4(10) . . . . ? C2 C3 C4 C5 -0.4(10) . . . . ? N1 C1 C5 C4 1.1(9) . . . . ? N1 C1 C5 C6 -175.6(5) . . . . ? C3 C4 C5 C1 -1.3(9) . . . . ? C3 C4 C5 C6 175.3(6) . . . . ? N3 N2 C6 O11 -0.4(6) . . . . ? N3 N2 C6 C5 178.2(5) . . . . ? C7 O11 C6 N2 0.6(6) . . . . ? C7 O11 C6 C5 -178.2(5) . . . . ? C1 C5 C6 N2 2.2(10) . . . . ? C4 C5 C6 N2 -174.3(6) . . . . ? C1 C5 C6 O11 -179.2(5) . . . . ? C4 C5 C6 O11 4.3(8) . . . . ? N2 N3 C7 O11 0.4(6) . . . . ? N2 N3 C7 C8 -179.6(5) . . . . ? C6 O11 C7 N3 -0.6(6) . . . . ? C6 O11 C7 C8 179.4(5) . . . . ? N3 C7 C8 C9 -174.2(6) . . . . ? O11 C7 C8 C9 5.8(8) . . . . ? N3 C7 C8 C12 1.7(10) . . . . ? O11 C7 C8 C12 -178.3(5) . . . . ? C12 C8 C9 C10 0.0(9) . . . . ? C7 C8 C9 C10 175.9(5) . . . . ? C8 C9 C10 C11 -1.8(9) . . . . ? C12 N4 C11 C10 -2.7(10) . . . . ? Cd2 N4 C11 C10 -177.1(5) . . . . ? C9 C10 C11 N4 3.3(10) . . . . ? C11 N4 C12 C8 0.8(9) . . . . ? Cd2 N4 C12 C8 175.1(4) . . . . ? C9 C8 C12 N4 0.6(9) . . . . ? C7 C8 C12 N4 -175.4(5) . . . . ? C18 C13 C14 C15 -1.0(8) . . . . ? C19 C13 C14 C15 179.5(5) . . . . ? C13 C14 C15 C16 0.4(8) . . . . ? C13 C14 C15 C20 177.4(5) . . . . ? C14 C15 C16 C17 -0.4(8) . . . . ? C20 C15 C16 C17 -177.5(5) . . . . ? C21 O10 C17 C18 -0.4(9) . . . . ? C21 O10 C17 C16 177.3(5) . . . . ? C15 C16 C17 O10 -176.7(5) . . . . ? C15 C16 C17 C18 1.1(9) . . . . ? O10 C17 C18 C13 175.9(5) . . . . ? C16 C17 C18 C13 -1.7(8) . . . . ? C14 C13 C18 C17 1.7(8) . . . . ? C19 C13 C18 C17 -178.8(5) . . . . ? Cd2 O7 C19 O6 -1.9(7) . . . . ? Cd2 O7 C19 C13 -179.5(4) . . . . ? C18 C13 C19 O6 -2.7(8) . . . . ? C14 C13 C19 O6 176.8(5) . . . . ? C18 C13 C19 O7 174.9(5) . . . . ? C14 C13 C19 O7 -5.6(8) . . . . ? Cd2 O8 C20 O9 -1.3(7) 4_545 . . . ? Cd2 O8 C20 C15 -179.9(5) 4_545 . . . ? Cd2 O9 C20 O8 1.5(7) 4_545 . . . ? Cd2 O9 C20 C15 180.0(5) 4_545 . . . ? C14 C15 C20 O8 4.0(9) . . . . ? C16 C15 C20 O8 -178.9(6) . . . . ? C14 C15 C20 O9 -174.5(6) . . . . ? C16 C15 C20 O9 2.6(9) . . . . ? C27 C22 C23 C24 2.2(8) . . . . ? C28 C22 C23 C24 179.5(5) . . . . ? C22 C23 C24 C25 -3.0(9) . . . . ? C22 C23 C24 C29 178.1(5) . . . . ? C23 C24 C25 C26 3.7(9) . . . . ? C29 C24 C25 C26 -177.4(5) . . . . ? C30 O5 C26 C27 -16.5(11) . . . . ? C30 O5 C26 C25 160.0(7) . . . . ? C24 C25 C26 C27 -3.8(10) . . . . ? C24 C25 C26 O5 179.4(6) . . . . ? O5 C26 C27 C22 179.6(6) . . . . ? C25 C26 C27 C22 3.2(9) . . . . ? C23 C22 C27 C26 -2.3(8) . . . . ? C28 C22 C27 C26 -179.7(5) . . . . ? Cd1 O2 C28 O1 3.3(6) . . . . ? Cd1 O2 C28 C22 -176.8(4) . . . . ? C23 C22 C28 O1 -176.4(5) . . . . ? C27 C22 C28 O1 0.9(8) . . . . ? C23 C22 C28 O2 3.8(8) . . . . ? C27 C22 C28 O2 -179.0(5) . . . . ? Cd1 O4 C29 O3 1.2(6) 4_446 . . . ? Cd1 O4 C29 C24 -177.7(5) 4_446 . . . ? Cd1 O3 C29 O4 -1.3(7) 4_446 . . . ? Cd1 O3 C29 C24 177.6(4) 4_446 . . . ? C25 C24 C29 O4 -4.9(9) . . . . ? C23 C24 C29 O4 174.0(6) . . . . ? C25 C24 C29 O3 176.2(6) . . . . ? C23 C24 C29 O3 -4.9(8) . . . . ? C32 N7 C31 C35 2.6(9) . . . . ? Cd3 N7 C31 C35 -177.2(4) . . . . ? C31 N7 C32 C33 -1.4(10) . . . . ? Cd3 N7 C32 C33 178.5(5) . . . . ? N7 C32 C33 C34 0.5(11) . . . . ? C32 C33 C34 C35 -0.7(10) . . . . ? N7 C31 C35 C34 -2.8(9) . . . . ? N7 C31 C35 C36 175.8(5) . . . . ? C33 C34 C35 C31 1.8(9) . . . . ? C33 C34 C35 C36 -176.8(6) . . . . ? N8 N8 C36 O24 -0.6(7) 2_556 . . . ? N8 N8 C36 C35 -176.8(5) 2_556 . . . ? C36 O24 C36 N8 0.3(3) 2_556 . . . ? C36 O24 C36 C35 176.9(6) 2_556 . . . ? C31 C35 C36 N8 -5.9(10) . . . . ? C34 C35 C36 N8 172.7(6) . . . . ? C31 C35 C36 O24 178.0(5) . . . . ? C34 C35 C36 O24 -3.4(8) . . . . ? C38 N5 C37 C41 0.8(9) . . . . ? Cd4 N5 C37 C41 177.0(4) . . . . ? C37 N5 C38 C39 0.6(10) . . . . ? Cd4 N5 C38 C39 -175.7(5) . . . . ? N5 C38 C39 C40 -2.5(10) . . . . ? C38 C39 C40 C41 2.9(9) . . . . ? N5 C37 C41 C40 -0.3(9) . . . . ? N5 C37 C41 C42 176.3(5) . . . . ? C39 C40 C41 C37 -1.6(9) . . . . ? C39 C40 C41 C42 -178.1(5) . . . . ? N6 N6 C42 O23 -0.4(7) 2_655 . . . ? N6 N6 C42 C41 -177.8(6) 2_655 . . . ? C42 O23 C42 N6 0.2(3) 2_655 . . . ? C42 O23 C42 C41 177.9(6) 2_655 . . . ? C37 C41 C42 N6 -3.5(10) . . . . ? C40 C41 C42 N6 173.1(6) . . . . ? C37 C41 C42 O23 179.2(5) . . . . ? C40 C41 C42 O23 -4.3(8) . . . . ? C44 N9 C43 C47 1.7(8) . . . . ? Cd4 N9 C43 C47 179.2(4) . . . . ? C43 N9 C44 C45 -2.4(9) . . . . ? Cd4 N9 C44 C45 -179.6(5) . . . . ? N9 C44 C45 C46 2.6(10) . . . . ? C44 C45 C46 C47 -2.0(10) . . . . ? C45 C46 C47 C43 1.4(10) . . . . ? C45 C46 C47 C48 -176.7(6) . . . . ? N9 C43 C47 C46 -1.2(9) . . . . ? N9 C43 C47 C48 177.0(5) . . . . ? N11 N10 C48 O22 -0.2(8) . . . . ? N11 N10 C48 C47 177.4(6) . . . . ? C49 O22 C48 N10 0.0(7) . . . . ? C49 O22 C48 C47 -177.9(5) . . . . ? C46 C47 C48 N10 -11.9(11) . . . . ? C43 C47 C48 N10 170.0(7) . . . . ? C46 C47 C48 O22 165.5(6) . . . . ? C43 C47 C48 O22 -12.5(8) . . . . ? N10 N11 C49 O22 -0.4(9) . . . . ? N10 N11 C49 C50 -177.7(7) . . . . ? C48 O22 C49 N11 0.3(8) . . . . ? C48 O22 C49 C50 178.0(6) . . . . ? N11 C49 C50 C51 -160.8(9) . . . . ? O22 C49 C50 C51 22.0(11) . . . . ? N11 C49 C50 C54 17.1(13) . . . . ? O22 C49 C50 C54 -160.1(7) . . . . ? C54 C50 C51 N12 1.2(14) . . . . ? C49 C50 C51 N12 179.0(8) . . . . ? C50 C51 N12 C52 1.8(15) . . . . ? C54 C53 C52 N12 -0.2(15) . . . . ? C51 N12 C52 C53 -2.3(15) . . . . ? C52 C53 C54 C50 3.2(13) . . . . ? C51 C50 C54 C53 -3.6(12) . . . . ? C49 C50 C54 C53 178.6(7) . . . . ? C60 C55 C56 C57 -0.7(8) . . . . ? C61 C55 C56 C57 -179.7(5) . . . . ? C55 C56 C57 C58 0.9(8) . . . . ? C55 C56 C57 C62 179.3(5) . . . . ? C56 C57 C58 C59 -0.6(8) . . . . ? C62 C57 C58 C59 -179.1(5) . . . . ? C63 O16 C59 C58 9.4(12) . . . . ? C63 O16 C59 C60 -170.4(8) . . . . ? C57 C58 C59 O16 -179.6(6) . . . . ? C57 C58 C59 C60 0.2(10) . . . . ? C56 C55 C60 C59 0.3(10) . . . . ? C61 C55 C60 C59 179.3(6) . . . . ? O16 C59 C60 C55 179.8(6) . . . . ? C58 C59 C60 C55 0.0(11) . . . . ? Cd4 O15 C61 O14 -0.4(6) . . . . ? Cd4 O15 C61 C55 -178.5(5) . . . . ? Cd4 O14 C61 O15 0.5(7) . . . . ? Cd4 O14 C61 C55 178.6(4) . . . . ? C60 C55 C61 O15 3.3(8) . . . . ? C56 C55 C61 O15 -177.6(5) . . . . ? C60 C55 C61 O14 -174.8(6) . . . . ? C56 C55 C61 O14 4.2(8) . . . . ? Cd3 O13 C62 O12 4.8(6) . . . . ? Cd3 O13 C62 C57 -176.9(5) . . . . ? Cd3 O12 C62 O13 -5.4(6) . . . . ? Cd3 O12 C62 C57 176.2(4) . . . . ? C58 C57 C62 O13 -7.7(8) . . . . ? C56 C57 C62 O13 173.9(5) . . . . ? C58 C57 C62 O12 170.7(5) . . . . ? C56 C57 C62 O12 -7.8(8) . . . . ? O19 Cd3 C62 O13 -163.0(4) 1_545 . . . ? O12 Cd3 C62 O13 175.0(6) . . . . ? O28 Cd3 C62 O13 -87.4(3) . . . . ? O29 Cd3 C62 O13 89.9(3) . . . . ? N7 Cd3 C62 O13 1.0(4) . . . . ? O20 Cd3 C62 O13 -175.7(3) 1_545 . . . ? C71 Cd3 C62 O13 -171.5(3) 1_545 . . . ? O19 Cd3 C62 O12 21.9(7) 1_545 . . . ? O28 Cd3 C62 O12 97.6(4) . . . . ? O29 Cd3 C62 O12 -85.1(4) . . . . ? N7 Cd3 C62 O12 -174.1(4) . . . . ? O20 Cd3 C62 O12 9.3(4) 1_545 . . . ? O13 Cd3 C62 O12 -175.0(6) . . . . ? C71 Cd3 C62 O12 13.5(5) 1_545 . . . ? C69 C64 C65 C66 1.4(8) . . . . ? C70 C64 C65 C66 -178.9(5) . . . . ? C64 C65 C66 C67 -1.0(8) . . . . ? C64 C65 C66 C71 177.3(5) . . . . ? C65 C66 C67 C68 0.1(9) . . . . ? C71 C66 C67 C68 -178.2(6) . . . . ? C72 O21 C68 C67 -160.3(6) . . . . ? C72 O21 C68 C69 20.0(9) . . . . ? C66 C67 C68 O21 -179.4(5) . . . . ? C66 C67 C68 C69 0.3(9) . . . . ? O21 C68 C69 C64 179.9(5) . . . . ? C67 C68 C69 C64 0.1(9) . . . . ? C65 C64 C69 C68 -1.0(8) . . . . ? C70 C64 C69 C68 179.3(5) . . . . ? Cd4 O18 C70 O17 -4.2(6) . . . . ? Cd4 O18 C70 C64 176.6(4) . . . . ? C65 C64 C70 O17 173.6(5) . . . . ? C69 C64 C70 O17 -6.7(8) . . . . ? C65 C64 C70 O18 -7.1(8) . . . . ? C69 C64 C70 O18 172.6(5) . . . . ? Cd3 O20 C71 O19 2.8(6) 1_565 . . . ? Cd3 O20 C71 C66 -178.0(5) 1_565 . . . ? Cd3 O19 C71 O20 -3.2(7) 1_565 . . . ? Cd3 O19 C71 C66 177.7(4) 1_565 . . . ? C67 C66 C71 O20 2.4(8) . . . . ? C65 C66 C71 O20 -175.8(5) . . . . ? C67 C66 C71 O19 -178.4(6) . . . . ? C65 C66 C71 O19 3.4(8) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.898 _refine_diff_density_min -0.391 _refine_diff_density_rms 0.061 #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 790244' #TrackingRef '- CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H40 Cd2 N4 O13' _chemical_formula_weight 961.54 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 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 23.9052(9) _cell_length_b 16.4095(6) _cell_length_c 10.3284(4) _cell_angle_alpha 90.00 _cell_angle_beta 102.3340(10) _cell_angle_gamma 90.00 _cell_volume 3958.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3766 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 26.58 _exptl_crystal_description BLOCK _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 1.614 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1936 _exptl_absorpt_coefficient_mu 1.142 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.821299 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Apex II CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10045 _diffrn_reflns_av_R_equivalents 0.0226 _diffrn_reflns_av_sigmaI/netI 0.0254 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 25.03 _reflns_number_total 3506 _reflns_number_gt 2855 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex II' _computing_cell_refinement 'Bruker Apex II' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0372P)^2^+4.9578P] 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 3506 _refine_ls_number_parameters 252 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0386 _refine_ls_R_factor_gt 0.0282 _refine_ls_wR_factor_ref 0.0749 _refine_ls_wR_factor_gt 0.0688 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _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 0.181038(10) 0.072435(13) 0.85529(2) 0.04108(10) Uani 1 1 d . . . O1 O 0.0000 0.19957(19) 1.2500 0.0425(7) Uani 1 2 d S . . O2 O 0.22676(11) 0.19099(15) 0.7942(3) 0.0605(7) Uani 1 1 d . . . O3 O 0.24504(12) 0.07497(15) 0.7110(3) 0.0650(8) Uani 1 1 d . . . O4 O 0.37163(11) 0.44412(14) 0.5417(2) 0.0542(6) Uani 1 1 d . . . O5 O 0.30970(12) 0.44042(14) 0.6702(3) 0.0647(8) Uani 1 1 d . . . O6 O 0.09580(11) 0.07548(14) 0.6916(2) 0.0552(6) Uani 1 1 d . . . H6A H 0.1083 0.0702 0.6209 0.083 Uiso 1 1 d R . . H6B H 0.0752 0.0369 0.7105 0.083 Uiso 1 1 d R . . O7 O 0.24406(13) 0.06171(16) 1.0674(3) 0.0720(8) Uani 1 1 d . . . H7A H 0.2468 0.0138 1.0992 0.108 Uiso 1 1 d R . . H7B H 0.2364 0.0994 1.1173 0.108 Uiso 1 1 d R . . N1 N 0.13422(11) 0.16094(16) 0.9705(3) 0.0426(6) Uani 1 1 d . . . N2 N 0.01964(12) 0.07244(16) 1.2084(3) 0.0475(7) Uani 1 1 d . . . C1 C 0.09589(13) 0.1332(2) 1.0360(3) 0.0430(8) Uani 1 1 d . . . H1 H 0.0870 0.0780 1.0309 0.052 Uiso 1 1 calc R . . C2 C 0.14632(14) 0.24109(19) 0.9773(3) 0.0451(8) Uani 1 1 d . . . H2 H 0.1736 0.2611 0.9334 0.054 Uiso 1 1 calc R . . C3 C 0.11974(15) 0.2941(2) 1.0470(3) 0.0479(8) Uani 1 1 d . . . H3 H 0.1280 0.3495 1.0472 0.058 Uiso 1 1 calc R . . C4 C 0.08117(14) 0.2658(2) 1.1159(3) 0.0441(8) Uani 1 1 d . . . H4 H 0.0635 0.3012 1.1650 0.053 Uiso 1 1 calc R . . C5 C 0.06861(13) 0.1830(2) 1.1115(3) 0.0387(7) Uani 1 1 d . . . C6 C 0.02985(13) 0.1475(2) 1.1874(3) 0.0414(7) Uani 1 1 d . . . C7 C 0.29221(12) 0.19156(18) 0.6508(3) 0.0346(7) Uani 1 1 d . . . C8 C 0.32537(13) 0.14664(18) 0.5819(3) 0.0375(7) Uani 1 1 d . . . H8 H 0.3220 0.0902 0.5797 0.045 Uiso 1 1 calc R . . C9 C 0.36361(13) 0.18361(19) 0.5159(3) 0.0380(7) Uani 1 1 d . . . C10 C 0.36787(12) 0.26843(19) 0.5230(3) 0.0377(7) Uani 1 1 d . . . H10 H 0.3934 0.2948 0.4806 0.045 Uiso 1 1 calc R . . C11 C 0.33508(12) 0.31442(18) 0.5915(3) 0.0343(7) Uani 1 1 d . . . C12 C 0.29688(13) 0.27522(18) 0.6550(3) 0.0351(7) Uani 1 1 d . . . H12 H 0.2744 0.3056 0.7005 0.042 Uiso 1 1 calc R . . C13 C 0.25186(13) 0.1500(2) 0.7225(3) 0.0410(7) Uani 1 1 d . . . C14 C 0.39865(15) 0.1315(2) 0.4392(4) 0.0531(9) Uani 1 1 d . . . C15 C 0.4370(3) 0.0757(4) 0.5342(7) 0.147(3) Uani 1 1 d . . . H15A H 0.4140 0.0372 0.5700 0.221 Uiso 1 1 calc R . . H15B H 0.4594 0.1072 0.6050 0.221 Uiso 1 1 calc R . . H15C H 0.4619 0.0470 0.4884 0.221 Uiso 1 1 calc R . . C16 C 0.4373(2) 0.1830(3) 0.3722(5) 0.1031(18) Uani 1 1 d . . . H16A H 0.4588 0.1480 0.3264 0.155 Uiso 1 1 calc R . . H16B H 0.4631 0.2139 0.4380 0.155 Uiso 1 1 calc R . . H16C H 0.4143 0.2194 0.3100 0.155 Uiso 1 1 calc R . . C17 C 0.3586(3) 0.0862(4) 0.3323(7) 0.154(3) Uani 1 1 d . . . H17A H 0.3398 0.0439 0.3711 0.231 Uiso 1 1 calc R . . H17B H 0.3797 0.0626 0.2725 0.231 Uiso 1 1 calc R . . H17C H 0.3305 0.1232 0.2846 0.231 Uiso 1 1 calc R . . C18 C 0.33970(15) 0.40547(19) 0.6004(3) 0.0433(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.04963(16) 0.03250(14) 0.04929(16) 0.00055(11) 0.02883(11) -0.00180(10) O1 0.0413(17) 0.0481(18) 0.0445(18) 0.000 0.0236(14) 0.000 O2 0.0734(17) 0.0521(15) 0.0725(17) 0.0008(13) 0.0523(15) -0.0014(13) O3 0.086(2) 0.0475(15) 0.0768(18) -0.0051(13) 0.0529(16) -0.0193(13) O4 0.0702(17) 0.0429(13) 0.0527(15) 0.0039(11) 0.0201(13) -0.0143(12) O5 0.088(2) 0.0326(13) 0.087(2) -0.0054(13) 0.0491(17) 0.0003(12) O6 0.0623(16) 0.0522(14) 0.0558(15) 0.0019(12) 0.0232(12) -0.0070(12) O7 0.083(2) 0.0531(16) 0.0719(19) 0.0058(14) 0.0000(16) 0.0002(14) N1 0.0479(16) 0.0435(15) 0.0433(15) 0.0019(12) 0.0250(13) 0.0038(12) N2 0.0454(16) 0.0503(17) 0.0540(17) 0.0016(14) 0.0267(13) 0.0022(13) C1 0.0455(18) 0.0411(18) 0.0484(19) -0.0003(15) 0.0231(15) 0.0000(15) C2 0.052(2) 0.0419(18) 0.048(2) 0.0036(15) 0.0259(16) -0.0018(15) C3 0.055(2) 0.0403(18) 0.053(2) -0.0019(16) 0.0232(17) -0.0008(16) C4 0.0454(19) 0.049(2) 0.0420(18) -0.0041(15) 0.0173(15) 0.0083(15) C5 0.0344(17) 0.0511(19) 0.0328(16) 0.0022(14) 0.0123(13) 0.0035(14) C6 0.0371(17) 0.054(2) 0.0370(17) -0.0011(15) 0.0163(14) 0.0026(15) C7 0.0335(16) 0.0394(16) 0.0328(16) 0.0031(13) 0.0111(13) -0.0007(13) C8 0.0404(17) 0.0317(16) 0.0429(17) -0.0011(14) 0.0147(14) 0.0012(13) C9 0.0363(17) 0.0423(17) 0.0382(17) -0.0018(14) 0.0140(14) 0.0018(14) C10 0.0330(16) 0.0443(18) 0.0386(17) 0.0047(14) 0.0141(13) -0.0033(13) C11 0.0372(16) 0.0335(15) 0.0330(15) 0.0041(13) 0.0092(13) 0.0022(13) C12 0.0372(16) 0.0369(16) 0.0339(16) -0.0013(13) 0.0137(13) 0.0031(13) C13 0.0399(17) 0.0471(19) 0.0388(17) 0.0022(15) 0.0147(15) -0.0065(15) C14 0.047(2) 0.055(2) 0.064(2) -0.0102(18) 0.0279(18) 0.0057(17) C15 0.156(6) 0.157(6) 0.150(6) 0.037(5) 0.081(5) 0.114(5) C16 0.097(4) 0.116(4) 0.120(4) -0.017(4) 0.079(4) 0.001(3) C17 0.108(5) 0.202(7) 0.173(7) -0.143(6) 0.078(5) -0.052(5) C18 0.052(2) 0.0357(17) 0.0419(18) 0.0023(15) 0.0092(16) -0.0018(15) _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 O5 2.199(2) 4_546 ? Cd1 N1 2.312(2) . ? Cd1 O3 2.353(2) . ? Cd1 O6 2.354(2) . ? Cd1 O2 2.382(2) . ? Cd1 O7 2.385(3) . ? Cd1 C13 2.713(3) . ? O1 C6 1.362(4) . ? O1 C6 1.362(4) 2_557 ? O2 C13 1.245(4) . ? O3 C13 1.244(4) . ? O4 C18 1.245(4) . ? O5 C18 1.258(4) . ? O5 Cd1 2.199(2) 4_556 ? O6 H6A 0.8501 . ? O6 H6B 0.8500 . ? O7 H7A 0.8500 . ? O7 H7B 0.8500 . ? N1 C1 1.330(4) . ? N1 C2 1.345(4) . ? N2 C6 1.284(4) . ? N2 N2 1.402(5) 2_557 ? C1 C5 1.384(4) . ? C1 H1 0.9300 . ? C2 C3 1.368(4) . ? C2 H2 0.9300 . ? C3 C4 1.361(4) . ? C3 H3 0.9300 . ? C4 C5 1.391(4) . ? C4 H4 0.9300 . ? C5 C6 1.456(4) . ? C7 C12 1.377(4) . ? C7 C8 1.385(4) . ? C7 C13 1.500(4) . ? C8 C9 1.391(4) . ? C8 H8 0.9300 . ? C9 C10 1.396(4) . ? C9 C14 1.531(4) . ? C10 C11 1.386(4) . ? C10 H10 0.9300 . ? C11 C12 1.391(4) . ? C11 C18 1.500(4) . ? C12 H12 0.9300 . ? C14 C17 1.495(6) . ? C14 C15 1.502(7) . ? C14 C16 1.523(6) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? 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 O5 Cd1 N1 138.80(9) 4_546 . ? O5 Cd1 O3 81.14(9) 4_546 . ? N1 Cd1 O3 140.03(9) . . ? O5 Cd1 O6 91.65(10) 4_546 . ? N1 Cd1 O6 85.21(9) . . ? O3 Cd1 O6 97.17(10) . . ? O5 Cd1 O2 135.19(9) 4_546 . ? N1 Cd1 O2 85.59(9) . . ? O3 Cd1 O2 54.59(8) . . ? O6 Cd1 O2 99.68(9) . . ? O5 Cd1 O7 88.69(10) 4_546 . ? N1 Cd1 O7 81.61(10) . . ? O3 Cd1 O7 102.37(11) . . ? O6 Cd1 O7 160.27(10) . . ? O2 Cd1 O7 93.89(10) . . ? O5 Cd1 C13 108.19(10) 4_546 . ? N1 Cd1 C13 112.85(10) . . ? O3 Cd1 C13 27.27(9) . . ? O6 Cd1 C13 99.48(9) . . ? O2 Cd1 C13 27.31(9) . . ? O7 Cd1 C13 99.14(10) . . ? C6 O1 C6 102.3(3) . 2_557 ? C13 O2 Cd1 91.3(2) . . ? C13 O3 Cd1 92.7(2) . . ? C18 O5 Cd1 107.2(2) . 4_556 ? Cd1 O6 H6A 101.8 . . ? Cd1 O6 H6B 105.8 . . ? H6A O6 H6B 116.6 . . ? Cd1 O7 H7A 113.9 . . ? Cd1 O7 H7B 109.2 . . ? H7A O7 H7B 116.6 . . ? C1 N1 C2 118.1(3) . . ? C1 N1 Cd1 120.6(2) . . ? C2 N1 Cd1 121.3(2) . . ? C6 N2 N2 106.27(18) . 2_557 ? N1 C1 C5 122.9(3) . . ? N1 C1 H1 118.5 . . ? C5 C1 H1 118.5 . . ? N1 C2 C3 122.0(3) . . ? N1 C2 H2 119.0 . . ? C3 C2 H2 119.0 . . ? C4 C3 C2 120.0(3) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C4 C5 118.8(3) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? C1 C5 C4 118.0(3) . . ? C1 C5 C6 119.9(3) . . ? C4 C5 C6 122.0(3) . . ? N2 C6 O1 112.6(3) . . ? N2 C6 C5 129.8(3) . . ? O1 C6 C5 117.6(3) . . ? C12 C7 C8 119.7(3) . . ? C12 C7 C13 119.6(3) . . ? C8 C7 C13 120.7(3) . . ? C7 C8 C9 121.8(3) . . ? C7 C8 H8 119.1 . . ? C9 C8 H8 119.1 . . ? C8 C9 C10 117.2(3) . . ? C8 C9 C14 119.9(3) . . ? C10 C9 C14 122.8(3) . . ? C11 C10 C9 121.8(3) . . ? C11 C10 H10 119.1 . . ? C9 C10 H10 119.1 . . ? C10 C11 C12 119.3(3) . . ? C10 C11 C18 122.1(3) . . ? C12 C11 C18 118.6(3) . . ? C7 C12 C11 120.2(3) . . ? C7 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? O3 C13 O2 121.4(3) . . ? O3 C13 C7 119.2(3) . . ? O2 C13 C7 119.4(3) . . ? O3 C13 Cd1 60.06(17) . . ? O2 C13 Cd1 61.37(16) . . ? C7 C13 Cd1 178.6(2) . . ? C17 C14 C15 112.6(5) . . ? C17 C14 C16 107.2(4) . . ? C15 C14 C16 106.9(4) . . ? C17 C14 C9 108.9(3) . . ? C15 C14 C9 109.1(3) . . ? C16 C14 C9 112.1(3) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O4 C18 O5 122.0(3) . . ? O4 C18 C11 121.5(3) . . ? O5 C18 C11 116.5(3) . . ? 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 O5 Cd1 O2 C13 10.4(3) 4_546 . . . ? N1 Cd1 O2 C13 -176.3(2) . . . . ? O3 Cd1 O2 C13 0.0(2) . . . . ? O6 Cd1 O2 C13 -91.9(2) . . . . ? O7 Cd1 O2 C13 102.4(2) . . . . ? O5 Cd1 O3 C13 -172.6(2) 4_546 . . . ? N1 Cd1 O3 C13 5.7(3) . . . . ? O6 Cd1 O3 C13 96.8(2) . . . . ? O2 Cd1 O3 C13 0.0(2) . . . . ? O7 Cd1 O3 C13 -86.0(2) . . . . ? O5 Cd1 N1 C1 -8.4(3) 4_546 . . . ? O3 Cd1 N1 C1 174.1(2) . . . . ? O6 Cd1 N1 C1 78.6(3) . . . . ? O2 Cd1 N1 C1 178.8(3) . . . . ? O7 Cd1 N1 C1 -86.7(3) . . . . ? C13 Cd1 N1 C1 176.9(2) . . . . ? O5 Cd1 N1 C2 169.1(2) 4_546 . . . ? O3 Cd1 N1 C2 -8.4(3) . . . . ? O6 Cd1 N1 C2 -103.8(3) . . . . ? O2 Cd1 N1 C2 -3.7(3) . . . . ? O7 Cd1 N1 C2 90.9(3) . . . . ? C13 Cd1 N1 C2 -5.6(3) . . . . ? C2 N1 C1 C5 -0.7(5) . . . . ? Cd1 N1 C1 C5 176.9(2) . . . . ? C1 N1 C2 C3 -1.2(5) . . . . ? Cd1 N1 C2 C3 -178.8(3) . . . . ? N1 C2 C3 C4 2.3(5) . . . . ? C2 C3 C4 C5 -1.4(5) . . . . ? N1 C1 C5 C4 1.5(5) . . . . ? N1 C1 C5 C6 -176.1(3) . . . . ? C3 C4 C5 C1 -0.4(5) . . . . ? C3 C4 C5 C6 177.1(3) . . . . ? N2 N2 C6 O1 -0.3(4) 2_557 . . . ? N2 N2 C6 C5 177.9(3) 2_557 . . . ? C6 O1 C6 N2 0.14(18) 2_557 . . . ? C6 O1 C6 C5 -178.4(3) 2_557 . . . ? C1 C5 C6 N2 7.8(5) . . . . ? C4 C5 C6 N2 -169.7(3) . . . . ? C1 C5 C6 O1 -174.0(3) . . . . ? C4 C5 C6 O1 8.5(4) . . . . ? C12 C7 C8 C9 -0.1(5) . . . . ? C13 C7 C8 C9 -179.2(3) . . . . ? C7 C8 C9 C10 0.7(5) . . . . ? C7 C8 C9 C14 -179.0(3) . . . . ? C8 C9 C10 C11 -0.7(5) . . . . ? C14 C9 C10 C11 179.1(3) . . . . ? C9 C10 C11 C12 0.0(5) . . . . ? C9 C10 C11 C18 179.6(3) . . . . ? C8 C7 C12 C11 -0.6(5) . . . . ? C13 C7 C12 C11 178.5(3) . . . . ? C10 C11 C12 C7 0.6(4) . . . . ? C18 C11 C12 C7 -178.9(3) . . . . ? Cd1 O3 C13 O2 0.0(4) . . . . ? Cd1 O3 C13 C7 178.6(2) . . . . ? Cd1 O2 C13 O3 0.0(4) . . . . ? Cd1 O2 C13 C7 -178.6(3) . . . . ? C12 C7 C13 O3 175.3(3) . . . . ? C8 C7 C13 O3 -5.6(5) . . . . ? C12 C7 C13 O2 -6.1(5) . . . . ? C8 C7 C13 O2 173.0(3) . . . . ? O5 Cd1 C13 O3 7.7(2) 4_546 . . . ? N1 Cd1 C13 O3 -176.0(2) . . . . ? O6 Cd1 C13 O3 -87.2(2) . . . . ? O2 Cd1 C13 O3 180.0(4) . . . . ? O7 Cd1 C13 O3 99.3(2) . . . . ? O5 Cd1 C13 O2 -172.3(2) 4_546 . . . ? N1 Cd1 C13 O2 4.0(2) . . . . ? O3 Cd1 C13 O2 -180.0(4) . . . . ? O6 Cd1 C13 O2 92.8(2) . . . . ? O7 Cd1 C13 O2 -80.7(2) . . . . ? C8 C9 C14 C17 60.7(5) . . . . ? C10 C9 C14 C17 -119.0(5) . . . . ? C8 C9 C14 C15 -62.6(5) . . . . ? C10 C9 C14 C15 117.6(5) . . . . ? C8 C9 C14 C16 179.2(4) . . . . ? C10 C9 C14 C16 -0.6(5) . . . . ? Cd1 O5 C18 O4 6.2(4) 4_556 . . . ? Cd1 O5 C18 C11 -173.9(2) 4_556 . . . ? C10 C11 C18 O4 3.0(5) . . . . ? C12 C11 C18 O4 -177.4(3) . . . . ? C10 C11 C18 O5 -176.9(3) . . . . ? C12 C11 C18 O5 2.7(5) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.647 _refine_diff_density_min -0.282 _refine_diff_density_rms 0.063 #===END data_5 _database_code_depnum_ccdc_archive 'CCDC 790245' #TrackingRef '- CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H52 Cd2 N12 O23' _chemical_formula_weight 1437.86 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.9120(18) _cell_length_b 14.868(2) _cell_length_c 17.797(3) _cell_angle_alpha 99.296(2) _cell_angle_beta 107.664(2) _cell_angle_gamma 100.141(3) _cell_volume 3119.4(8) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3276 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 26.43 _exptl_crystal_description BLOCK _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 1.531 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1456 _exptl_absorpt_coefficient_mu 0.768 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.498799 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Apex II CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15856 _diffrn_reflns_av_R_equivalents 0.0462 _diffrn_reflns_av_sigmaI/netI 0.1035 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 25.03 _reflns_number_total 10948 _reflns_number_gt 6115 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex II' _computing_cell_refinement 'Bruker Apex II' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0924P)^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 10948 _refine_ls_number_parameters 813 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1199 _refine_ls_R_factor_gt 0.0543 _refine_ls_wR_factor_ref 0.1806 _refine_ls_wR_factor_gt 0.1419 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _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 0.30953(5) -0.01533(3) 0.26983(3) 0.03982(18) Uani 1 1 d . . . Cd2 Cd 0.40471(5) 0.69698(4) 0.75126(3) 0.0466(2) Uani 1 1 d . . . O1 O 0.0222(5) -0.1071(4) 0.4430(4) 0.0557(14) Uani 1 1 d . . . O2 O 0.4058(4) 0.3381(3) 0.6059(3) 0.0433(12) Uani 1 1 d . . . O3 O 0.0066(5) 0.6344(4) 0.4667(4) 0.0572(15) Uani 1 1 d . . . O4 O 0.3016(6) -0.0783(4) 0.1396(3) 0.0661(17) Uani 1 1 d . . . O5 O 0.2871(5) 0.0665(4) 0.1505(3) 0.0569(15) Uani 1 1 d . . . O6 O 0.3838(5) 0.1632(4) -0.0835(3) 0.0581(15) Uani 1 1 d . . . H6 H 0.4288 0.1647 -0.1076 0.087 Uiso 1 1 calc R . . O7 O 0.4101(5) -0.1600(4) -0.1868(3) 0.0628(16) Uani 1 1 d . . . O8 O 0.3683(5) -0.2470(4) -0.1064(3) 0.0681(17) Uani 1 1 d . . . O9 O 0.3908(6) 0.6193(4) 0.6194(3) 0.0665(17) Uani 1 1 d . . . O10 O 0.3941(5) 0.7691(4) 0.6399(3) 0.0616(16) Uani 1 1 d . . . O11 O 0.3420(5) 0.9235(3) 0.4008(3) 0.0523(14) Uani 1 1 d . . . O12 O 0.3188(5) 0.8352(3) 0.2826(3) 0.0522(14) Uani 1 1 d . . . O13 O 0.2933(7) 0.5059(4) 0.3219(3) 0.079(2) Uani 1 1 d . . . H13 H 0.2692 0.5089 0.2744 0.118 Uiso 1 1 calc R . . O14 O 0.4991(5) 0.0358(4) 0.3009(4) 0.0733(18) Uani 1 1 d . . . H14A H 0.5134 0.0818 0.3408 0.110 Uiso 1 1 d R . . H14B H 0.5565 0.0182 0.2916 0.110 Uiso 1 1 d R . . O15 O 0.5993(5) 0.7436(4) 0.8129(4) 0.0700(17) Uani 1 1 d . . . H15A H 0.6305 0.8010 0.8359 0.105 Uiso 1 1 d R . . H15B H 0.6401 0.7044 0.8192 0.105 Uiso 1 1 d R . . O16 O 0.6459(5) 0.0107(4) 0.4383(4) 0.0734(18) Uani 1 1 d . . . H16A H 0.6220 -0.0485 0.4211 0.110 Uiso 1 1 d R . . H16B H 0.6548 0.0334 0.4875 0.110 Uiso 1 1 d R . . O17 O 0.4810(6) 0.8276(4) 0.1708(4) 0.088(2) Uani 1 1 d . . . O18 O 0.3130(7) 0.3290(6) 0.9566(5) 0.117(3) Uani 1 1 d . . . O19 O 0.2382(9) 0.3292(7) 0.0852(6) 0.148(4) Uani 1 1 d . . . O20 O 0.2075(9) 0.5018(7) 0.1621(5) 0.138(3) Uani 1 1 d . . . N1 N 0.1149(6) -0.0531(4) 0.2497(4) 0.0512(17) Uani 1 1 d . . . N2 N -0.1593(7) -0.1417(7) 0.3748(5) 0.084(3) Uani 1 1 d . . . N3 N -0.1449(7) -0.1533(7) 0.4546(6) 0.088(3) Uani 1 1 d . . . N4 N 0.0152(8) -0.1590(6) 0.7040(5) 0.078(2) Uani 1 1 d . . . N5 N 0.3137(5) 0.1301(4) 0.3463(4) 0.0437(15) Uani 1 1 d . . . N6 N 0.4113(5) 0.1907(4) 0.6054(4) 0.0427(15) Uani 1 1 d . . . N7 N 0.4394(5) 0.2405(4) 0.6858(4) 0.0446(16) Uani 1 1 d . . . N8 N 0.4377(5) 0.5614(4) 0.7907(3) 0.0426(15) Uani 1 1 d . . . N9 N 0.2028(6) 0.6394(5) 0.7052(4) 0.0593(19) Uani 1 1 d . . . N10 N -0.1519(7) 0.5898(6) 0.4879(5) 0.073(2) Uani 1 1 d . . . N11 N -0.1780(7) 0.5971(6) 0.4076(5) 0.076(2) Uani 1 1 d . . . N12 N -0.1468(8) 0.6512(6) 0.1867(5) 0.083(3) Uani 1 1 d . . . C1 C 0.0806(7) -0.0706(5) 0.3095(5) 0.051(2) Uani 1 1 d . . . H1 H 0.1351 -0.0661 0.3591 0.061 Uiso 1 1 calc R . . C2 C 0.0339(9) -0.0618(7) 0.1782(6) 0.073(3) Uani 1 1 d . . . H2 H 0.0556 -0.0500 0.1348 0.088 Uiso 1 1 calc R . . C3 C -0.0797(9) -0.0874(8) 0.1657(6) 0.081(3) Uani 1 1 d . . . H3 H -0.1325 -0.0948 0.1148 0.097 Uiso 1 1 calc R . . C4 C -0.1116(8) -0.1013(7) 0.2295(6) 0.076(3) Uani 1 1 d . . . H4 H -0.1871 -0.1148 0.2237 0.091 Uiso 1 1 calc R . . C5 C -0.0305(7) -0.0954(6) 0.3044(5) 0.054(2) Uani 1 1 d . . . C6 C -0.0613(8) -0.1153(6) 0.3713(6) 0.055(2) Uani 1 1 d . . . C7 C -0.0365(8) -0.1314(6) 0.4936(6) 0.059(2) Uani 1 1 d . . . C8 C 0.0245(8) -0.1327(6) 0.5759(5) 0.054(2) Uani 1 1 d . . . C9 C -0.0341(8) -0.1567(6) 0.6276(6) 0.065(2) Uani 1 1 d . . . H9 H -0.1119 -0.1719 0.6069 0.077 Uiso 1 1 calc R . . C10 C 0.1252(11) -0.1385(7) 0.7307(6) 0.081(3) Uani 1 1 d . . . H10 H 0.1611 -0.1413 0.7839 0.097 Uiso 1 1 calc R . . C11 C 0.1919(9) -0.1133(8) 0.6860(6) 0.082(3) Uani 1 1 d . . . H11 H 0.2695 -0.0989 0.7086 0.098 Uiso 1 1 calc R . . C12 C 0.1395(9) -0.1102(7) 0.6074(6) 0.071(3) Uani 1 1 d . . . H12 H 0.1815 -0.0931 0.5755 0.085 Uiso 1 1 calc R . . C13 C 0.3288(7) 0.3073(5) 0.4349(5) 0.057(2) Uani 1 1 d . . . H13A H 0.3343 0.3668 0.4642 0.068 Uiso 1 1 calc R . . C14 C 0.2901(8) 0.2860(5) 0.3513(5) 0.058(2) Uani 1 1 d . . . H14 H 0.2699 0.3316 0.3235 0.070 Uiso 1 1 calc R . . C15 C 0.2812(7) 0.1973(5) 0.3090(5) 0.052(2) Uani 1 1 d . . . H15 H 0.2517 0.1833 0.2528 0.062 Uiso 1 1 calc R . . C16 C 0.3509(6) 0.1501(5) 0.4270(4) 0.0419(18) Uani 1 1 d . . . H16 H 0.3723 0.1036 0.4531 0.050 Uiso 1 1 calc R . . C17 C 0.3595(6) 0.2374(5) 0.4743(4) 0.0412(18) Uani 1 1 d . . . C18 C 0.3926(6) 0.2512(5) 0.5608(4) 0.0417(18) Uani 1 1 d . . . C19 C 0.4349(6) 0.3249(5) 0.6826(4) 0.0423(18) Uani 1 1 d . . . C20 C 0.4527(6) 0.4045(5) 0.7491(4) 0.0389(17) Uani 1 1 d . . . C21 C 0.4910(9) 0.3981(6) 0.8281(5) 0.076(3) Uani 1 1 d . . . H21 H 0.5095 0.3434 0.8410 0.091 Uiso 1 1 calc R . . C22 C 0.5021(11) 0.4747(7) 0.8888(5) 0.099(4) Uani 1 1 d . . . H22 H 0.5285 0.4722 0.9430 0.119 Uiso 1 1 calc R . . C23 C 0.4728(9) 0.5551(6) 0.8672(5) 0.070(3) Uani 1 1 d . . . H23 H 0.4782 0.6057 0.9076 0.084 Uiso 1 1 calc R . . C24 C 0.4285(6) 0.4876(5) 0.7324(4) 0.0395(18) Uani 1 1 d . . . H24 H 0.4051 0.4927 0.6787 0.047 Uiso 1 1 calc R . . C25 C 0.1369(8) 0.6371(6) 0.6297(5) 0.059(2) Uani 1 1 d . . . H25 H 0.1717 0.6550 0.5939 0.070 Uiso 1 1 calc R . . C26 C 0.1512(9) 0.6161(6) 0.7551(6) 0.067(3) Uani 1 1 d . . . H26 H 0.1945 0.6197 0.8084 0.081 Uiso 1 1 calc R . . C27 C 0.0364(10) 0.5866(7) 0.7329(6) 0.081(3) Uani 1 1 d . . . H27 H 0.0041 0.5686 0.7699 0.097 Uiso 1 1 calc R . . C28 C -0.0300(9) 0.5840(6) 0.6550(6) 0.071(3) Uani 1 1 d . . . H28 H -0.1076 0.5654 0.6385 0.085 Uiso 1 1 calc R . . C29 C 0.0238(8) 0.6105(5) 0.6020(5) 0.057(2) Uani 1 1 d . . . C30 C -0.0443(8) 0.6096(6) 0.5189(6) 0.056(2) Uani 1 1 d . . . C31 C -0.0831(8) 0.6245(6) 0.3983(6) 0.059(2) Uani 1 1 d . . . C32 C -0.0640(8) 0.6452(6) 0.3247(6) 0.057(2) Uani 1 1 d . . . C33 C -0.1554(9) 0.6358(8) 0.2570(7) 0.085(3) Uani 1 1 d . . . H33 H -0.2265 0.6179 0.2601 0.102 Uiso 1 1 calc R . . C34 C -0.0444(10) 0.6749(8) 0.1832(7) 0.084(3) Uani 1 1 d . . . H34 H -0.0367 0.6827 0.1342 0.101 Uiso 1 1 calc R . . C35 C 0.0500(9) 0.6883(8) 0.2492(7) 0.080(3) Uani 1 1 d . . . H35 H 0.1201 0.7085 0.2453 0.096 Uiso 1 1 calc R . . C36 C 0.0413(9) 0.6717(7) 0.3227(6) 0.071(3) Uani 1 1 d . . . H36 H 0.1044 0.6785 0.3678 0.085 Uiso 1 1 calc R . . C37 C 0.3239(6) -0.0047(5) 0.0349(4) 0.0401(18) Uani 1 1 d . . . C38 C 0.3384(6) 0.0779(5) 0.0082(4) 0.0435(19) Uani 1 1 d . . . H38 H 0.3268 0.1319 0.0357 0.052 Uiso 1 1 calc R . . C39 C 0.3700(6) 0.0800(5) -0.0592(4) 0.0426(18) Uani 1 1 d . . . C40 C 0.3844(6) -0.0008(5) -0.1027(4) 0.0437(19) Uani 1 1 d . . . H40 H 0.4045 0.0011 -0.1485 0.052 Uiso 1 1 calc R . . C41 C 0.3685(6) -0.0844(5) -0.0773(4) 0.0436(18) Uani 1 1 d . . . C42 C 0.3384(6) -0.0857(5) -0.0080(4) 0.0435(18) Uani 1 1 d . . . H42 H 0.3280 -0.1412 0.0094 0.052 Uiso 1 1 calc R . . C43 C 0.3020(7) -0.0055(5) 0.1124(4) 0.0444(19) Uani 1 1 d . . . C44 C 0.3846(7) -0.1698(5) -0.1252(4) 0.048(2) Uani 1 1 d . . . C45 C 0.3600(6) 0.6855(5) 0.5043(4) 0.0376(17) Uani 1 1 d . . . C46 C 0.3553(6) 0.7668(5) 0.4738(4) 0.0373(17) Uani 1 1 d . . . H46 H 0.3644 0.8242 0.5080 0.045 Uiso 1 1 calc R . . C47 C 0.3368(6) 0.7602(5) 0.3924(4) 0.0366(17) Uani 1 1 d . . . C48 C 0.3189(6) 0.6735(5) 0.3408(4) 0.0404(18) Uani 1 1 d . . . H48 H 0.3085 0.6697 0.2862 0.049 Uiso 1 1 calc R . . C49 C 0.3167(7) 0.5927(5) 0.3706(4) 0.046(2) Uani 1 1 d . . . C50 C 0.3388(7) 0.5995(5) 0.4526(5) 0.048(2) Uani 1 1 d . . . H50 H 0.3393 0.5457 0.4731 0.058 Uiso 1 1 calc R . . C51 C 0.3842(7) 0.6917(6) 0.5938(4) 0.0463(19) Uani 1 1 d . . . C52 C 0.3329(6) 0.8449(5) 0.3571(4) 0.0421(18) Uani 1 1 d . . . O21 O 0.3378(15) 0.6699(9) 0.0091(8) 0.226(7) Uani 1 1 d . . . O22 O 0.2291(15) 0.6931(9) 0.1255(9) 0.256(8) Uani 1 1 d . . . O23 O 0.0344(17) 0.2125(15) 0.1542(12) 0.150(8) Uani 0.50 1 d P . . O24 O 0.918(2) 0.887(2) 0.9571(13) 0.205(12) Uani 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 0.0571(4) 0.0352(3) 0.0302(3) 0.0082(2) 0.0187(3) 0.0115(3) Cd2 0.0731(5) 0.0356(3) 0.0301(3) 0.0055(2) 0.0173(3) 0.0130(3) O1 0.044(4) 0.059(3) 0.062(4) 0.015(3) 0.018(3) 0.007(3) O2 0.059(4) 0.034(3) 0.032(3) -0.001(2) 0.014(3) 0.010(2) O3 0.048(4) 0.058(4) 0.062(4) 0.012(3) 0.018(3) 0.010(3) O4 0.119(5) 0.053(3) 0.046(3) 0.023(3) 0.044(3) 0.029(4) O5 0.087(5) 0.047(3) 0.044(3) 0.005(3) 0.036(3) 0.013(3) O6 0.091(5) 0.051(3) 0.054(3) 0.025(3) 0.041(3) 0.030(3) O7 0.086(5) 0.065(4) 0.039(3) -0.001(3) 0.023(3) 0.029(3) O8 0.107(5) 0.045(3) 0.051(4) 0.000(3) 0.029(3) 0.023(3) O9 0.116(5) 0.050(3) 0.041(3) 0.022(3) 0.026(3) 0.027(3) O10 0.098(5) 0.047(3) 0.036(3) 0.006(3) 0.023(3) 0.011(3) O11 0.075(4) 0.037(3) 0.047(3) 0.014(2) 0.020(3) 0.015(3) O12 0.080(4) 0.044(3) 0.040(3) 0.020(2) 0.024(3) 0.017(3) O13 0.152(7) 0.035(3) 0.045(3) 0.004(3) 0.032(4) 0.020(4) O14 0.066(4) 0.060(4) 0.096(5) 0.023(4) 0.029(4) 0.015(3) O15 0.082(5) 0.048(3) 0.075(4) 0.008(3) 0.026(4) 0.009(3) O16 0.112(6) 0.046(3) 0.064(4) 0.013(3) 0.036(4) 0.011(3) O17 0.142(7) 0.087(5) 0.084(5) 0.045(4) 0.076(5) 0.063(5) O18 0.145(8) 0.103(6) 0.084(6) 0.004(5) 0.007(5) 0.055(5) O19 0.169(10) 0.118(7) 0.147(9) 0.030(7) 0.035(7) 0.037(7) O20 0.191(10) 0.144(8) 0.068(5) 0.006(5) 0.038(6) 0.039(7) N1 0.050(5) 0.051(4) 0.047(4) 0.010(3) 0.011(4) 0.006(3) N2 0.045(6) 0.127(8) 0.082(6) 0.042(6) 0.018(5) 0.011(5) N3 0.044(6) 0.135(8) 0.088(7) 0.052(6) 0.023(5) 0.006(5) N4 0.079(7) 0.092(6) 0.059(5) 0.020(5) 0.021(5) 0.014(5) N5 0.057(5) 0.035(3) 0.039(4) 0.007(3) 0.018(3) 0.010(3) N6 0.050(4) 0.034(3) 0.036(3) -0.002(3) 0.012(3) 0.005(3) N7 0.062(5) 0.036(3) 0.039(4) 0.008(3) 0.023(3) 0.012(3) N8 0.060(5) 0.038(3) 0.029(3) 0.006(3) 0.016(3) 0.011(3) N9 0.066(5) 0.053(4) 0.055(5) 0.013(4) 0.017(4) 0.009(4) N10 0.063(6) 0.087(6) 0.069(6) 0.021(5) 0.025(5) 0.011(5) N11 0.061(6) 0.095(6) 0.069(6) 0.022(5) 0.019(5) 0.015(5) N12 0.060(6) 0.109(7) 0.067(6) 0.034(5) 0.005(5) 0.005(5) C1 0.050(6) 0.057(5) 0.045(5) 0.013(4) 0.011(4) 0.017(4) C2 0.082(8) 0.084(7) 0.058(6) 0.025(5) 0.023(6) 0.027(6) C3 0.052(7) 0.116(9) 0.064(7) 0.027(6) 0.004(6) 0.016(6) C4 0.049(7) 0.097(8) 0.073(7) 0.025(6) 0.013(6) 0.005(6) C5 0.043(6) 0.053(5) 0.055(5) 0.009(4) 0.006(5) 0.008(4) C6 0.041(6) 0.057(5) 0.068(6) 0.016(4) 0.017(5) 0.013(4) C7 0.059(7) 0.054(5) 0.069(6) 0.014(5) 0.031(5) 0.009(5) C8 0.051(6) 0.053(5) 0.056(5) 0.009(4) 0.015(5) 0.013(4) C9 0.053(6) 0.064(6) 0.071(7) 0.014(5) 0.024(5) -0.006(5) C10 0.085(9) 0.090(8) 0.058(6) 0.011(6) 0.011(6) 0.029(7) C11 0.063(7) 0.101(8) 0.065(7) 0.001(6) 0.007(6) 0.024(6) C12 0.064(8) 0.076(7) 0.077(7) 0.020(5) 0.026(6) 0.021(6) C13 0.087(7) 0.030(4) 0.060(5) 0.005(4) 0.036(5) 0.013(4) C14 0.097(7) 0.047(5) 0.042(5) 0.019(4) 0.032(5) 0.025(5) C15 0.072(6) 0.052(5) 0.037(4) 0.015(4) 0.022(4) 0.019(4) C16 0.051(5) 0.039(4) 0.036(4) 0.009(3) 0.014(4) 0.010(4) C17 0.047(5) 0.036(4) 0.038(4) -0.001(3) 0.017(4) 0.009(4) C18 0.041(5) 0.040(4) 0.039(4) -0.002(3) 0.013(4) 0.009(4) C19 0.050(5) 0.039(4) 0.034(4) 0.001(3) 0.014(4) 0.009(4) C20 0.048(5) 0.032(4) 0.033(4) 0.003(3) 0.011(4) 0.007(3) C21 0.138(10) 0.050(5) 0.040(5) 0.008(4) 0.021(5) 0.044(6) C22 0.205(13) 0.075(7) 0.034(5) 0.024(5) 0.038(7) 0.068(8) C23 0.124(9) 0.052(5) 0.036(5) 0.009(4) 0.024(5) 0.031(5) C24 0.048(5) 0.036(4) 0.031(4) 0.004(3) 0.011(4) 0.010(4) C25 0.057(7) 0.058(5) 0.062(6) 0.011(4) 0.021(5) 0.017(5) C26 0.082(8) 0.062(6) 0.052(6) 0.014(5) 0.020(6) 0.010(5) C27 0.095(9) 0.078(7) 0.070(7) 0.015(6) 0.038(7) 0.004(6) C28 0.063(7) 0.068(6) 0.076(7) 0.018(5) 0.024(6) 0.000(5) C29 0.062(7) 0.042(5) 0.062(6) 0.007(4) 0.022(5) 0.008(4) C30 0.040(6) 0.053(5) 0.065(6) 0.003(4) 0.013(5) 0.010(4) C31 0.041(6) 0.062(6) 0.065(6) 0.010(5) 0.008(5) 0.010(5) C32 0.038(6) 0.051(5) 0.069(6) 0.006(4) 0.004(5) 0.006(4) C33 0.053(7) 0.124(9) 0.072(7) 0.024(7) 0.018(6) 0.012(6) C34 0.068(8) 0.096(8) 0.074(7) 0.010(6) 0.014(7) 0.011(7) C35 0.050(7) 0.106(8) 0.076(7) 0.026(6) 0.015(6) 0.003(6) C36 0.055(7) 0.081(7) 0.063(6) 0.010(5) 0.007(5) 0.015(5) C37 0.047(5) 0.044(4) 0.029(4) 0.006(3) 0.013(4) 0.012(4) C38 0.055(5) 0.049(4) 0.030(4) 0.007(3) 0.013(4) 0.026(4) C39 0.051(5) 0.043(4) 0.032(4) 0.007(3) 0.009(4) 0.015(4) C40 0.051(5) 0.050(4) 0.028(4) 0.002(3) 0.013(4) 0.013(4) C41 0.049(5) 0.043(4) 0.033(4) 0.003(3) 0.009(4) 0.009(4) C42 0.054(5) 0.047(4) 0.029(4) 0.010(3) 0.012(4) 0.012(4) C43 0.053(5) 0.047(4) 0.032(4) 0.001(3) 0.016(4) 0.013(4) C44 0.062(6) 0.046(5) 0.030(4) -0.005(3) 0.012(4) 0.020(4) C45 0.041(5) 0.041(4) 0.033(4) 0.014(3) 0.014(4) 0.007(3) C46 0.043(5) 0.034(4) 0.036(4) 0.007(3) 0.016(4) 0.009(3) C47 0.041(5) 0.032(4) 0.038(4) 0.010(3) 0.016(4) 0.006(3) C48 0.047(5) 0.043(4) 0.033(4) 0.011(3) 0.017(4) 0.009(4) C49 0.079(6) 0.032(4) 0.038(4) 0.012(3) 0.031(4) 0.014(4) C50 0.066(6) 0.031(4) 0.052(5) 0.017(3) 0.023(4) 0.013(4) C51 0.051(6) 0.053(5) 0.031(4) 0.011(4) 0.012(4) 0.007(4) C52 0.040(5) 0.050(5) 0.035(4) 0.011(4) 0.011(4) 0.007(4) O21 0.44(2) 0.171(11) 0.173(11) 0.115(9) 0.178(13) 0.152(13) O22 0.35(2) 0.183(12) 0.211(14) -0.037(10) 0.182(14) -0.087(12) O23 0.158(18) 0.19(2) 0.135(17) 0.093(15) 0.070(14) 0.046(15) O24 0.18(2) 0.37(4) 0.111(17) 0.08(2) 0.051(15) 0.15(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O12 2.289(5) 1_545 ? Cd1 O14 2.294(6) . ? Cd1 O4 2.320(5) . ? Cd1 N5 2.345(6) . ? Cd1 N1 2.378(7) . ? Cd1 O5 2.580(5) . ? Cd1 O11 2.581(5) 1_545 ? Cd2 O7 2.211(5) 1_566 ? Cd2 N8 2.306(6) . ? Cd2 O15 2.338(6) . ? Cd2 O9 2.381(5) . ? Cd2 O10 2.382(5) . ? Cd2 N9 2.427(8) . ? Cd2 C51 2.720(7) . ? O1 C6 1.369(10) . ? O1 C7 1.392(10) . ? O2 C19 1.358(8) . ? O2 C18 1.360(8) . ? O3 C30 1.350(10) . ? O3 C31 1.368(10) . ? O4 C43 1.254(9) . ? O5 C43 1.249(8) . ? O6 C39 1.374(8) . ? O6 H6 0.8200 . ? O7 C44 1.260(9) . ? O7 Cd2 2.211(5) 1_544 ? O8 C44 1.246(9) . ? O9 C51 1.241(9) . ? O10 C51 1.262(9) . ? O11 C52 1.259(8) . ? O11 Cd1 2.581(5) 1_565 ? O12 C52 1.263(8) . ? O12 Cd1 2.289(5) 1_565 ? O13 C49 1.359(8) . ? O13 H13 0.8200 . ? O14 H14A 0.8515 . ? O14 H14B 0.8803 . ? O15 H15A 0.8501 . ? O15 H15B 0.8501 . ? O16 H16A 0.8500 . ? O16 H16B 0.8511 . ? N1 C1 1.316(10) . ? N1 C2 1.349(11) . ? N2 C6 1.279(10) . ? N2 N3 1.418(11) . ? N3 C7 1.314(11) . ? N4 C10 1.314(12) . ? N4 C9 1.323(11) . ? N5 C16 1.332(9) . ? N5 C15 1.344(9) . ? N6 C18 1.300(9) . ? N6 N7 1.405(8) . ? N7 C19 1.277(8) . ? N8 C23 1.322(9) . ? N8 C24 1.345(8) . ? N9 C26 1.315(11) . ? N9 C25 1.346(10) . ? N10 C30 1.288(10) . ? N10 N11 1.392(10) . ? N11 C31 1.291(11) . ? N12 C34 1.330(12) . ? N12 C33 1.340(12) . ? C1 C5 1.388(11) . ? C1 H1 0.9300 . ? C2 C3 1.387(13) . ? C2 H2 0.9300 . ? C3 C4 1.355(13) . ? C3 H3 0.9300 . ? C4 C5 1.401(12) . ? C4 H4 0.9300 . ? C5 C6 1.424(12) . ? C7 C8 1.442(12) . ? C8 C12 1.376(12) . ? C8 C9 1.407(12) . ? C9 H9 0.9300 . ? C10 C11 1.383(14) . ? C10 H10 0.9300 . ? C11 C12 1.370(13) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.380(11) . ? C13 C17 1.393(10) . ? C13 H13A 0.9300 . ? C14 C15 1.376(10) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.395(9) . ? C16 H16 0.9300 . ? C17 C18 1.436(10) . ? C19 C20 1.463(9) . ? C20 C21 1.367(10) . ? C20 C24 1.382(9) . ? C21 C22 1.392(12) . ? C21 H21 0.9300 . ? C22 C23 1.392(12) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 C29 1.353(11) . ? C25 H25 0.9300 . ? C26 C27 1.381(13) . ? C26 H26 0.9300 . ? C27 C28 1.382(13) . ? C27 H27 0.9300 . ? C28 C29 1.395(12) . ? C28 H28 0.9300 . ? C29 C30 1.471(12) . ? C31 C32 1.472(13) . ? C32 C36 1.361(12) . ? C32 C33 1.375(13) . ? C33 H33 0.9300 . ? C34 C35 1.370(13) . ? C34 H34 0.9300 . ? C35 C36 1.403(13) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C37 C38 1.390(10) . ? C37 C42 1.391(9) . ? C37 C43 1.491(9) . ? C38 C39 1.382(10) . ? C38 H38 0.9300 . ? C39 C40 1.395(9) . ? C40 C41 1.391(10) . ? C40 H40 0.9300 . ? C41 C42 1.403(10) . ? C41 C44 1.494(9) . ? C42 H42 0.9300 . ? C45 C50 1.379(10) . ? C45 C46 1.407(9) . ? C45 C51 1.512(9) . ? C46 C47 1.378(9) . ? C46 H46 0.9300 . ? C47 C48 1.395(9) . ? C47 C52 1.498(9) . ? C48 C49 1.389(9) . ? C48 H48 0.9300 . ? C49 C50 1.384(10) . ? C50 H50 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O12 Cd1 O14 93.8(2) 1_545 . ? O12 Cd1 O4 81.17(18) 1_545 . ? O14 Cd1 O4 87.0(2) . . ? O12 Cd1 N5 140.77(19) 1_545 . ? O14 Cd1 N5 87.8(2) . . ? O4 Cd1 N5 138.00(19) . . ? O12 Cd1 N1 90.3(2) 1_545 . ? O14 Cd1 N1 173.3(2) . . ? O4 Cd1 N1 98.9(2) . . ? N5 Cd1 N1 85.7(2) . . ? O12 Cd1 O5 133.51(17) 1_545 . ? O14 Cd1 O5 86.8(2) . . ? O4 Cd1 O5 52.41(17) . . ? N5 Cd1 O5 85.71(18) . . ? N1 Cd1 O5 94.3(2) . . ? O12 Cd1 O11 53.21(16) 1_545 1_545 ? O14 Cd1 O11 90.5(2) . 1_545 ? O4 Cd1 O11 134.05(17) . 1_545 ? N5 Cd1 O11 87.61(18) . 1_545 ? N1 Cd1 O11 87.7(2) . 1_545 ? O5 Cd1 O11 172.87(16) . 1_545 ? O7 Cd2 N8 135.9(2) 1_566 . ? O7 Cd2 O15 83.9(2) 1_566 . ? N8 Cd2 O15 80.6(2) . . ? O7 Cd2 O9 137.05(19) 1_566 . ? N8 Cd2 O9 86.52(18) . . ? O15 Cd2 O9 100.1(2) . . ? O7 Cd2 O10 82.35(19) 1_566 . ? N8 Cd2 O10 140.27(19) . . ? O15 Cd2 O10 96.7(2) . . ? O9 Cd2 O10 54.70(18) . . ? O7 Cd2 N9 96.4(2) 1_566 . ? N8 Cd2 N9 93.4(2) . . ? O15 Cd2 N9 171.3(2) . . ? O9 Cd2 N9 85.6(2) . . ? O10 Cd2 N9 92.0(2) . . ? O7 Cd2 C51 109.9(2) 1_566 . ? N8 Cd2 C51 113.5(2) . . ? O15 Cd2 C51 100.7(2) . . ? O9 Cd2 C51 27.1(2) . . ? O10 Cd2 C51 27.6(2) . . ? N9 Cd2 C51 87.4(2) . . ? C6 O1 C7 103.0(7) . . ? C19 O2 C18 102.7(5) . . ? C30 O3 C31 101.7(7) . . ? C43 O4 Cd1 98.9(4) . . ? C43 O5 Cd1 86.8(4) . . ? C39 O6 H6 109.5 . . ? C44 O7 Cd2 105.3(5) . 1_544 ? C51 O9 Cd2 91.9(4) . . ? C51 O10 Cd2 91.3(4) . . ? C52 O11 Cd1 86.0(4) . 1_565 ? C52 O12 Cd1 99.6(4) . 1_565 ? C49 O13 H13 109.5 . . ? Cd1 O14 H14A 100.0 . . ? Cd1 O14 H14B 141.5 . . ? H14A O14 H14B 117.2 . . ? Cd2 O15 H15A 119.7 . . ? Cd2 O15 H15B 122.4 . . ? H15A O15 H15B 117.4 . . ? H16A O16 H16B 117.1 . . ? C1 N1 C2 116.1(8) . . ? C1 N1 Cd1 120.0(6) . . ? C2 N1 Cd1 123.9(6) . . ? C6 N2 N3 106.9(8) . . ? C7 N3 N2 106.4(7) . . ? C10 N4 C9 116.4(9) . . ? C16 N5 C15 118.0(6) . . ? C16 N5 Cd1 121.9(5) . . ? C15 N5 Cd1 120.1(5) . . ? C18 N6 N7 106.1(5) . . ? C19 N7 N6 106.2(6) . . ? C23 N8 C24 119.0(6) . . ? C23 N8 Cd2 123.6(5) . . ? C24 N8 Cd2 117.2(4) . . ? C26 N9 C25 116.3(8) . . ? C26 N9 Cd2 121.3(7) . . ? C25 N9 Cd2 122.2(6) . . ? C30 N10 N11 106.8(8) . . ? C31 N11 N10 105.5(8) . . ? C34 N12 C33 117.5(9) . . ? N1 C1 C5 125.1(8) . . ? N1 C1 H1 117.5 . . ? C5 C1 H1 117.5 . . ? N1 C2 C3 123.9(9) . . ? N1 C2 H2 118.1 . . ? C3 C2 H2 118.1 . . ? C4 C3 C2 118.2(9) . . ? C4 C3 H3 120.9 . . ? C2 C3 H3 120.9 . . ? C3 C4 C5 119.8(10) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? C1 C5 C4 116.8(8) . . ? C1 C5 C6 121.9(8) . . ? C4 C5 C6 121.2(9) . . ? N2 C6 O1 112.9(8) . . ? N2 C6 C5 128.9(9) . . ? O1 C6 C5 118.2(8) . . ? N3 C7 O1 110.8(8) . . ? N3 C7 C8 129.7(9) . . ? O1 C7 C8 119.4(8) . . ? C12 C8 C9 117.5(9) . . ? C12 C8 C7 122.7(9) . . ? C9 C8 C7 119.8(8) . . ? N4 C9 C8 123.7(9) . . ? N4 C9 H9 118.1 . . ? C8 C9 H9 118.1 . . ? N4 C10 C11 125.1(10) . . ? N4 C10 H10 117.4 . . ? C11 C10 H10 117.4 . . ? C12 C11 C10 117.7(10) . . ? C12 C11 H11 121.1 . . ? C10 C11 H11 121.1 . . ? C11 C12 C8 119.5(10) . . ? C11 C12 H12 120.3 . . ? C8 C12 H12 120.3 . . ? C14 C13 C17 118.3(7) . . ? C14 C13 H13A 120.9 . . ? C17 C13 H13A 120.9 . . ? C15 C14 C13 120.1(7) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? N5 C15 C14 122.2(7) . . ? N5 C15 H15 118.9 . . ? C14 C15 H15 118.9 . . ? N5 C16 C17 123.3(7) . . ? N5 C16 H16 118.4 . . ? C17 C16 H16 118.4 . . ? C13 C17 C16 118.1(7) . . ? C13 C17 C18 122.0(6) . . ? C16 C17 C18 119.8(7) . . ? N6 C18 O2 112.0(6) . . ? N6 C18 C17 129.3(6) . . ? O2 C18 C17 118.7(6) . . ? N7 C19 O2 113.1(6) . . ? N7 C19 C20 128.5(7) . . ? O2 C19 C20 118.4(6) . . ? C21 C20 C24 118.8(6) . . ? C21 C20 C19 121.3(7) . . ? C24 C20 C19 119.9(6) . . ? C20 C21 C22 118.9(8) . . ? C20 C21 H21 120.6 . . ? C22 C21 H21 120.6 . . ? C21 C22 C23 119.0(8) . . ? C21 C22 H22 120.5 . . ? C23 C22 H22 120.5 . . ? N8 C23 C22 121.7(8) . . ? N8 C23 H23 119.1 . . ? C22 C23 H23 119.1 . . ? N8 C24 C20 122.5(6) . . ? N8 C24 H24 118.7 . . ? C20 C24 H24 118.7 . . ? N9 C25 C29 124.8(9) . . ? N9 C25 H25 117.6 . . ? C29 C25 H25 117.6 . . ? N9 C26 C27 123.7(9) . . ? N9 C26 H26 118.2 . . ? C27 C26 H26 118.2 . . ? C26 C27 C28 119.3(9) . . ? C26 C27 H27 120.4 . . ? C28 C27 H27 120.4 . . ? C27 C28 C29 117.5(10) . . ? C27 C28 H28 121.2 . . ? C29 C28 H28 121.2 . . ? C25 C29 C28 118.5(9) . . ? C25 C29 C30 122.5(8) . . ? C28 C29 C30 119.0(9) . . ? N10 C30 O3 112.9(8) . . ? N10 C30 C29 127.4(9) . . ? O3 C30 C29 119.7(8) . . ? N11 C31 O3 113.0(8) . . ? N11 C31 C32 127.4(9) . . ? O3 C31 C32 119.5(8) . . ? C36 C32 C33 120.2(10) . . ? C36 C32 C31 121.3(8) . . ? C33 C32 C31 118.5(9) . . ? N12 C33 C32 123.0(10) . . ? N12 C33 H33 118.5 . . ? C32 C33 H33 118.5 . . ? N12 C34 C35 122.3(11) . . ? N12 C34 H34 118.9 . . ? C35 C34 H34 118.9 . . ? C34 C35 C36 120.3(10) . . ? C34 C35 H35 119.8 . . ? C36 C35 H35 119.8 . . ? C32 C36 C35 116.6(9) . . ? C32 C36 H36 121.7 . . ? C35 C36 H36 121.7 . . ? C38 C37 C42 119.5(6) . . ? C38 C37 C43 120.6(6) . . ? C42 C37 C43 119.7(6) . . ? C39 C38 C37 120.1(6) . . ? C39 C38 H38 120.0 . . ? C37 C38 H38 120.0 . . ? O6 C39 C38 118.3(6) . . ? O6 C39 C40 120.9(6) . . ? C38 C39 C40 120.8(7) . . ? C41 C40 C39 119.7(7) . . ? C41 C40 H40 120.2 . . ? C39 C40 H40 120.2 . . ? C40 C41 C42 119.2(7) . . ? C40 C41 C44 118.5(7) . . ? C42 C41 C44 122.3(7) . . ? C37 C42 C41 120.7(7) . . ? C37 C42 H42 119.7 . . ? C41 C42 H42 119.7 . . ? O5 C43 O4 120.7(7) . . ? O5 C43 C37 120.1(7) . . ? O4 C43 C37 119.2(6) . . ? O8 C44 O7 122.6(7) . . ? O8 C44 C41 121.1(7) . . ? O7 C44 C41 116.3(7) . . ? C50 C45 C46 120.4(6) . . ? C50 C45 C51 119.7(6) . . ? C46 C45 C51 119.9(6) . . ? C47 C46 C45 119.0(6) . . ? C47 C46 H46 120.5 . . ? C45 C46 H46 120.5 . . ? C46 C47 C48 120.4(6) . . ? C46 C47 C52 121.1(6) . . ? C48 C47 C52 118.5(6) . . ? C49 C48 C47 120.2(6) . . ? C49 C48 H48 119.9 . . ? C47 C48 H48 119.9 . . ? O13 C49 C50 118.0(6) . . ? O13 C49 C48 122.4(6) . . ? C50 C49 C48 119.6(6) . . ? C45 C50 C49 120.3(6) . . ? C45 C50 H50 119.8 . . ? C49 C50 H50 119.8 . . ? O9 C51 O10 121.9(7) . . ? O9 C51 C45 118.5(7) . . ? O10 C51 C45 119.5(7) . . ? O9 C51 Cd2 61.0(4) . . ? O10 C51 Cd2 61.1(4) . . ? C45 C51 Cd2 174.2(6) . . ? O11 C52 O12 121.1(7) . . ? O11 C52 C47 120.4(6) . . ? O12 C52 C47 118.4(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O12 Cd1 O4 C43 -176.3(5) 1_545 . . . ? O14 Cd1 O4 C43 -81.9(5) . . . . ? N5 Cd1 O4 C43 1.4(7) . . . . ? N1 Cd1 O4 C43 94.8(5) . . . . ? O5 Cd1 O4 C43 6.3(5) . . . . ? O11 Cd1 O4 C43 -169.7(4) 1_545 . . . ? O12 Cd1 O5 C43 -9.8(6) 1_545 . . . ? O14 Cd1 O5 C43 82.4(5) . . . . ? O4 Cd1 O5 C43 -6.3(5) . . . . ? N5 Cd1 O5 C43 170.4(5) . . . . ? N1 Cd1 O5 C43 -104.3(5) . . . . ? O7 Cd2 O9 C51 -1.6(7) 1_566 . . . ? N8 Cd2 O9 C51 -173.4(5) . . . . ? O15 Cd2 O9 C51 -93.6(5) . . . . ? O10 Cd2 O9 C51 -2.6(5) . . . . ? N9 Cd2 O9 C51 92.9(5) . . . . ? O7 Cd2 O10 C51 -176.8(5) 1_566 . . . ? N8 Cd2 O10 C51 17.1(7) . . . . ? O15 Cd2 O10 C51 100.3(5) . . . . ? O9 Cd2 O10 C51 2.6(5) . . . . ? N9 Cd2 O10 C51 -80.6(5) . . . . ? O12 Cd1 N1 C1 67.6(6) 1_545 . . . ? O4 Cd1 N1 C1 148.8(6) . . . . ? N5 Cd1 N1 C1 -73.3(6) . . . . ? O5 Cd1 N1 C1 -158.7(6) . . . . ? O11 Cd1 N1 C1 14.5(6) 1_545 . . . ? O12 Cd1 N1 C2 -109.5(7) 1_545 . . . ? O4 Cd1 N1 C2 -28.4(7) . . . . ? N5 Cd1 N1 C2 109.6(7) . . . . ? O5 Cd1 N1 C2 24.2(7) . . . . ? O11 Cd1 N1 C2 -162.6(7) 1_545 . . . ? C6 N2 N3 C7 0.6(11) . . . . ? O12 Cd1 N5 C16 16.5(7) 1_545 . . . ? O14 Cd1 N5 C16 -76.8(6) . . . . ? O4 Cd1 N5 C16 -159.8(5) . . . . ? N1 Cd1 N5 C16 101.7(6) . . . . ? O5 Cd1 N5 C16 -163.7(6) . . . . ? O11 Cd1 N5 C16 13.8(6) 1_545 . . . ? O12 Cd1 N5 C15 -165.6(5) 1_545 . . . ? O14 Cd1 N5 C15 101.1(6) . . . . ? O4 Cd1 N5 C15 18.1(7) . . . . ? N1 Cd1 N5 C15 -80.4(6) . . . . ? O5 Cd1 N5 C15 14.2(6) . . . . ? O11 Cd1 N5 C15 -168.3(6) 1_545 . . . ? C18 N6 N7 C19 0.2(8) . . . . ? O7 Cd2 N8 C23 -3.0(8) 1_566 . . . ? O15 Cd2 N8 C23 68.0(7) . . . . ? O9 Cd2 N8 C23 168.9(7) . . . . ? O10 Cd2 N8 C23 157.1(6) . . . . ? N9 Cd2 N8 C23 -105.7(7) . . . . ? C51 Cd2 N8 C23 165.6(7) . . . . ? O7 Cd2 N8 C24 -177.7(5) 1_566 . . . ? O15 Cd2 N8 C24 -106.7(6) . . . . ? O9 Cd2 N8 C24 -5.8(5) . . . . ? O10 Cd2 N8 C24 -17.6(7) . . . . ? N9 Cd2 N8 C24 79.6(6) . . . . ? C51 Cd2 N8 C24 -9.1(6) . . . . ? O7 Cd2 N9 C26 -76.5(7) 1_566 . . . ? N8 Cd2 N9 C26 60.4(7) . . . . ? O9 Cd2 N9 C26 146.6(7) . . . . ? O10 Cd2 N9 C26 -159.0(7) . . . . ? C51 Cd2 N9 C26 173.8(7) . . . . ? O7 Cd2 N9 C25 97.8(6) 1_566 . . . ? N8 Cd2 N9 C25 -125.3(6) . . . . ? O9 Cd2 N9 C25 -39.1(6) . . . . ? O10 Cd2 N9 C25 15.3(6) . . . . ? C51 Cd2 N9 C25 -12.0(6) . . . . ? C30 N10 N11 C31 -2.5(10) . . . . ? C2 N1 C1 C5 -1.2(12) . . . . ? Cd1 N1 C1 C5 -178.5(6) . . . . ? C1 N1 C2 C3 0.2(13) . . . . ? Cd1 N1 C2 C3 177.4(7) . . . . ? N1 C2 C3 C4 2.4(16) . . . . ? C2 C3 C4 C5 -3.9(16) . . . . ? N1 C1 C5 C4 -0.4(12) . . . . ? N1 C1 C5 C6 178.7(8) . . . . ? C3 C4 C5 C1 3.0(14) . . . . ? C3 C4 C5 C6 -176.0(9) . . . . ? N3 N2 C6 O1 -0.1(11) . . . . ? N3 N2 C6 C5 179.2(9) . . . . ? C7 O1 C6 N2 -0.4(9) . . . . ? C7 O1 C6 C5 -179.8(7) . . . . ? C1 C5 C6 N2 -177.5(9) . . . . ? C4 C5 C6 N2 1.5(15) . . . . ? C1 C5 C6 O1 1.8(12) . . . . ? C4 C5 C6 O1 -179.3(8) . . . . ? N2 N3 C7 O1 -0.9(11) . . . . ? N2 N3 C7 C8 -178.7(9) . . . . ? C6 O1 C7 N3 0.8(9) . . . . ? C6 O1 C7 C8 178.9(7) . . . . ? N3 C7 C8 C12 178.0(9) . . . . ? O1 C7 C8 C12 0.3(12) . . . . ? N3 C7 C8 C9 -2.7(14) . . . . ? O1 C7 C8 C9 179.6(7) . . . . ? C10 N4 C9 C8 -1.0(14) . . . . ? C12 C8 C9 N4 -0.2(14) . . . . ? C7 C8 C9 N4 -179.5(9) . . . . ? C9 N4 C10 C11 1.5(16) . . . . ? N4 C10 C11 C12 -0.8(17) . . . . ? C10 C11 C12 C8 -0.5(15) . . . . ? C9 C8 C12 C11 0.9(13) . . . . ? C7 C8 C12 C11 -179.8(9) . . . . ? C17 C13 C14 C15 0.8(13) . . . . ? C16 N5 C15 C14 3.0(12) . . . . ? Cd1 N5 C15 C14 -175.0(6) . . . . ? C13 C14 C15 N5 -2.9(13) . . . . ? C15 N5 C16 C17 -1.1(11) . . . . ? Cd1 N5 C16 C17 176.8(6) . . . . ? C14 C13 C17 C16 1.0(12) . . . . ? C14 C13 C17 C18 -175.2(8) . . . . ? N5 C16 C17 C13 -0.9(12) . . . . ? N5 C16 C17 C18 175.4(7) . . . . ? N7 N6 C18 O2 -0.3(8) . . . . ? N7 N6 C18 C17 -179.0(7) . . . . ? C19 O2 C18 N6 0.3(8) . . . . ? C19 O2 C18 C17 179.1(7) . . . . ? C13 C17 C18 N6 171.5(8) . . . . ? C16 C17 C18 N6 -4.6(13) . . . . ? C13 C17 C18 O2 -7.1(11) . . . . ? C16 C17 C18 O2 176.7(7) . . . . ? N6 N7 C19 O2 -0.1(9) . . . . ? N6 N7 C19 C20 177.5(7) . . . . ? C18 O2 C19 N7 -0.1(8) . . . . ? C18 O2 C19 C20 -177.9(7) . . . . ? N7 C19 C20 C21 8.1(13) . . . . ? O2 C19 C20 C21 -174.5(8) . . . . ? N7 C19 C20 C24 -170.7(8) . . . . ? O2 C19 C20 C24 6.7(11) . . . . ? C24 C20 C21 C22 1.4(14) . . . . ? C19 C20 C21 C22 -177.4(9) . . . . ? C20 C21 C22 C23 0.5(17) . . . . ? C24 N8 C23 C22 0.9(14) . . . . ? Cd2 N8 C23 C22 -173.7(8) . . . . ? C21 C22 C23 N8 -1.8(18) . . . . ? C23 N8 C24 C20 1.2(12) . . . . ? Cd2 N8 C24 C20 176.1(6) . . . . ? C21 C20 C24 N8 -2.3(12) . . . . ? C19 C20 C24 N8 176.5(7) . . . . ? C26 N9 C25 C29 -1.8(12) . . . . ? Cd2 N9 C25 C29 -176.3(6) . . . . ? C25 N9 C26 C27 2.8(13) . . . . ? Cd2 N9 C26 C27 177.3(7) . . . . ? N9 C26 C27 C28 -2.4(15) . . . . ? C26 C27 C28 C29 1.0(14) . . . . ? N9 C25 C29 C28 0.5(13) . . . . ? N9 C25 C29 C30 179.7(8) . . . . ? C27 C28 C29 C25 -0.1(13) . . . . ? C27 C28 C29 C30 -179.4(8) . . . . ? N11 N10 C30 O3 2.8(10) . . . . ? N11 N10 C30 C29 -179.3(8) . . . . ? C31 O3 C30 N10 -1.9(9) . . . . ? C31 O3 C30 C29 180.0(7) . . . . ? C25 C29 C30 N10 -176.6(8) . . . . ? C28 C29 C30 N10 2.6(13) . . . . ? C25 C29 C30 O3 1.2(12) . . . . ? C28 C29 C30 O3 -179.5(8) . . . . ? N10 N11 C31 O3 1.4(10) . . . . ? N10 N11 C31 C32 -178.5(9) . . . . ? C30 O3 C31 N11 0.2(9) . . . . ? C30 O3 C31 C32 -179.9(7) . . . . ? N11 C31 C32 C36 -178.5(9) . . . . ? O3 C31 C32 C36 1.7(12) . . . . ? N11 C31 C32 C33 0.6(14) . . . . ? O3 C31 C32 C33 -179.2(8) . . . . ? C34 N12 C33 C32 1.3(17) . . . . ? C36 C32 C33 N12 0.3(16) . . . . ? C31 C32 C33 N12 -178.8(10) . . . . ? C33 N12 C34 C35 -3.4(16) . . . . ? N12 C34 C35 C36 3.8(17) . . . . ? C33 C32 C36 C35 0.0(14) . . . . ? C31 C32 C36 C35 179.1(9) . . . . ? C34 C35 C36 C32 -2.0(15) . . . . ? C42 C37 C38 C39 -1.8(11) . . . . ? C43 C37 C38 C39 173.3(7) . . . . ? C37 C38 C39 O6 -179.8(7) . . . . ? C37 C38 C39 C40 2.0(12) . . . . ? O6 C39 C40 C41 -179.2(7) . . . . ? C38 C39 C40 C41 -1.0(12) . . . . ? C39 C40 C41 C42 -0.1(12) . . . . ? C39 C40 C41 C44 -180.0(7) . . . . ? C38 C37 C42 C41 0.7(12) . . . . ? C43 C37 C42 C41 -174.5(7) . . . . ? C40 C41 C42 C37 0.3(12) . . . . ? C44 C41 C42 C37 -179.8(7) . . . . ? Cd1 O5 C43 O4 10.7(8) . . . . ? Cd1 O5 C43 C37 -167.5(7) . . . . ? Cd1 O4 C43 O5 -12.1(9) . . . . ? Cd1 O4 C43 C37 166.1(6) . . . . ? C38 C37 C43 O5 6.1(12) . . . . ? C42 C37 C43 O5 -178.8(7) . . . . ? C38 C37 C43 O4 -172.1(7) . . . . ? C42 C37 C43 O4 3.0(12) . . . . ? Cd2 O7 C44 O8 3.9(10) 1_544 . . . ? Cd2 O7 C44 C41 -172.9(5) 1_544 . . . ? C40 C41 C44 O8 -178.0(8) . . . . ? C42 C41 C44 O8 2.2(12) . . . . ? C40 C41 C44 O7 -1.1(11) . . . . ? C42 C41 C44 O7 179.0(8) . . . . ? C50 C45 C46 C47 -4.5(11) . . . . ? C51 C45 C46 C47 177.9(7) . . . . ? C45 C46 C47 C48 2.4(11) . . . . ? C45 C46 C47 C52 -178.9(7) . . . . ? C46 C47 C48 C49 1.7(11) . . . . ? C52 C47 C48 C49 -177.0(7) . . . . ? C47 C48 C49 O13 176.1(8) . . . . ? C47 C48 C49 C50 -3.7(12) . . . . ? C46 C45 C50 C49 2.5(12) . . . . ? C51 C45 C50 C49 -179.9(7) . . . . ? O13 C49 C50 C45 -178.2(8) . . . . ? C48 C49 C50 C45 1.6(12) . . . . ? Cd2 O9 C51 O10 4.8(9) . . . . ? Cd2 O9 C51 C45 -173.4(6) . . . . ? Cd2 O10 C51 O9 -4.7(9) . . . . ? Cd2 O10 C51 C45 173.3(6) . . . . ? C50 C45 C51 O9 4.2(11) . . . . ? C46 C45 C51 O9 -178.2(7) . . . . ? C50 C45 C51 O10 -173.9(8) . . . . ? C46 C45 C51 O10 3.7(11) . . . . ? O7 Cd2 C51 O9 178.8(5) 1_566 . . . ? N8 Cd2 C51 O9 7.2(6) . . . . ? O15 Cd2 C51 O9 91.5(5) . . . . ? O10 Cd2 C51 O9 175.4(8) . . . . ? N9 Cd2 C51 O9 -85.4(5) . . . . ? O7 Cd2 C51 O10 3.4(5) 1_566 . . . ? N8 Cd2 C51 O10 -168.2(5) . . . . ? O15 Cd2 C51 O10 -83.9(5) . . . . ? O9 Cd2 C51 O10 -175.4(8) . . . . ? N9 Cd2 C51 O10 99.2(5) . . . . ? Cd1 O11 C52 O12 2.4(7) 1_565 . . . ? Cd1 O11 C52 C47 -176.6(6) 1_565 . . . ? Cd1 O12 C52 O11 -2.7(8) 1_565 . . . ? Cd1 O12 C52 C47 176.3(6) 1_565 . . . ? C46 C47 C52 O11 -2.9(11) . . . . ? C48 C47 C52 O11 175.8(7) . . . . ? C46 C47 C52 O12 178.0(7) . . . . ? C48 C47 C52 O12 -3.3(11) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.925 _refine_diff_density_min -0.828 _refine_diff_density_rms 0.116 #===END data_6 _database_code_depnum_ccdc_archive 'CCDC 790246' #TrackingRef '- CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H13 Cd N5 O8' _chemical_formula_weight 563.75 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2623(6) _cell_length_b 10.8870(6) _cell_length_c 10.9849(7) _cell_angle_alpha 70.7110(10) _cell_angle_beta 73.5830(10) _cell_angle_gamma 70.1800(10) _cell_volume 1069.47(11) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3758 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 30.21 _exptl_crystal_description BLOCK _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 1.751 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 560 _exptl_absorpt_coefficient_mu 1.080 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.835376 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Apex II CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5538 _diffrn_reflns_av_R_equivalents 0.0109 _diffrn_reflns_av_sigmaI/netI 0.0215 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 25.03 _reflns_number_total 3751 _reflns_number_gt 3435 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex II' _computing_cell_refinement 'Bruker Apex II' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0436P)^2^+0.6394P] 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 3751 _refine_ls_number_parameters 313 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0298 _refine_ls_R_factor_gt 0.0261 _refine_ls_wR_factor_ref 0.0745 _refine_ls_wR_factor_gt 0.0719 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.098 _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 0.586353(19) 0.56995(2) 0.59449(2) 0.02947(9) Uani 1 1 d . . . O1 O 0.9510(2) 0.8676(2) 0.2604(2) 0.0364(5) Uani 1 1 d . . . O2 O 0.3647(2) 0.6328(3) 0.6981(3) 0.0583(7) Uani 1 1 d . . . O3 O 0.3306(3) 0.5351(3) 0.5709(3) 0.0634(8) Uani 1 1 d . . . O4 O -0.1783(2) 0.5604(2) 0.5900(2) 0.0406(5) Uani 1 1 d . . . O5 O -0.3434(2) 0.6505(3) 0.7375(3) 0.0517(6) Uani 1 1 d . . . O6 O -0.2061(3) 0.7456(3) 1.0813(3) 0.0547(7) Uani 1 1 d . . . O7 O 0.0129(3) 0.6770(3) 1.0976(2) 0.0485(6) Uani 1 1 d . . . N1 N 0.5684(3) 0.7798(3) 0.4377(3) 0.0380(6) Uani 1 1 d . . . N2 N 0.8559(3) 1.0740(3) 0.1496(3) 0.0502(8) Uani 1 1 d . . . N3 N 1.0038(3) 1.0484(3) 0.1176(3) 0.0507(8) Uani 1 1 d . . . N4 N 1.3716(3) 0.6507(3) 0.2664(3) 0.0399(6) Uani 1 1 d . . . N5 N -0.0807(3) 0.6988(3) 1.0399(3) 0.0369(6) Uani 1 1 d . . . C1 C 0.6886(3) 0.8104(3) 0.3736(3) 0.0361(7) Uani 1 1 d . . . H1 H 0.7727 0.7422 0.3800 0.043 Uiso 1 1 calc R . . C2 C 0.4487(3) 0.8776(4) 0.4238(4) 0.0453(8) Uani 1 1 d . . . H2 H 0.3636 0.8572 0.4671 0.054 Uiso 1 1 calc R . . C3 C 0.4454(4) 1.0069(4) 0.3483(4) 0.0510(9) Uani 1 1 d . . . H3 H 0.3594 1.0717 0.3403 0.061 Uiso 1 1 calc R . . C4 C 0.5695(4) 1.0402(3) 0.2849(4) 0.0456(8) Uani 1 1 d . . . H4 H 0.5696 1.1277 0.2350 0.055 Uiso 1 1 calc R . . C5 C 0.6950(3) 0.9387(3) 0.2976(3) 0.0351(7) Uani 1 1 d . . . C6 C 0.8307(3) 0.9664(3) 0.2325(3) 0.0354(7) Uani 1 1 d . . . C7 C 1.0536(3) 0.9272(3) 0.1835(3) 0.0363(7) Uani 1 1 d . . . C8 C 1.2009(3) 0.8515(3) 0.1836(3) 0.0372(7) Uani 1 1 d . . . C9 C 1.3076(4) 0.9075(4) 0.0986(4) 0.0527(10) Uani 1 1 d . . . H9 H 1.2864 0.9932 0.0415 0.063 Uiso 1 1 calc R . . C10 C 1.4448(4) 0.8326(4) 0.1017(4) 0.0605(11) Uani 1 1 d . . . H10 H 1.5185 0.8677 0.0472 0.073 Uiso 1 1 calc R . . C11 C 1.4727(4) 0.7055(4) 0.1859(4) 0.0493(9) Uani 1 1 d . . . H11 H 1.5663 0.6557 0.1867 0.059 Uiso 1 1 calc R . . C12 C 1.2379(3) 0.7240(3) 0.2646(3) 0.0385(7) Uani 1 1 d . . . H12 H 1.1664 0.6867 0.3210 0.046 Uiso 1 1 calc R . . C13 C 0.1364(3) 0.6124(3) 0.7299(3) 0.0274(6) Uani 1 1 d . . . C14 C 0.0985(3) 0.6460(3) 0.8493(3) 0.0292(6) Uani 1 1 d . . . H14 H 0.1659 0.6533 0.8861 0.035 Uiso 1 1 calc R . . C15 C -0.0410(3) 0.6681(3) 0.9118(3) 0.0293(6) Uani 1 1 d . . . C16 C -0.1447(3) 0.6609(3) 0.8588(3) 0.0327(7) Uani 1 1 d . . . H16 H -0.2386 0.6793 0.9016 0.039 Uiso 1 1 calc R . . C17 C -0.1056(3) 0.6257(3) 0.7406(3) 0.0302(6) Uani 1 1 d . . . C18 C 0.0346(3) 0.5992(3) 0.6772(3) 0.0307(6) Uani 1 1 d . . . H18 H 0.0608 0.5726 0.5995 0.037 Uiso 1 1 calc R . . C19 C 0.2876(3) 0.5916(3) 0.6601(3) 0.0334(7) Uani 1 1 d . . . C20 C -0.2170(3) 0.6115(3) 0.6850(3) 0.0350(7) Uani 1 1 d . . . O9 O 0.4280(14) 0.5344(15) 0.9818(14) 0.181(5) Uani 0.50 1 d PU . . O8 O 0.0000 1.0000 0.5000 0.247(6) Uani 1 2 d SU . . 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 0.01677(12) 0.03460(14) 0.03741(14) -0.01089(9) -0.00279(8) -0.00792(9) O1 0.0317(11) 0.0299(11) 0.0419(12) -0.0040(9) -0.0045(9) -0.0086(9) O2 0.0198(11) 0.091(2) 0.0786(18) -0.0467(16) 0.0050(11) -0.0207(12) O3 0.0383(14) 0.097(2) 0.0624(17) -0.0539(17) 0.0082(12) -0.0106(14) O4 0.0305(12) 0.0494(14) 0.0486(13) -0.0160(11) -0.0103(10) -0.0138(10) O5 0.0201(12) 0.0677(17) 0.0752(17) -0.0340(14) -0.0096(11) -0.0065(11) O6 0.0368(14) 0.0712(18) 0.0538(15) -0.0331(14) 0.0133(11) -0.0133(13) O7 0.0537(15) 0.0549(15) 0.0395(13) -0.0166(11) -0.0118(11) -0.0113(12) N1 0.0292(14) 0.0368(15) 0.0442(15) -0.0090(12) -0.0059(11) -0.0068(11) N2 0.0339(15) 0.0355(16) 0.067(2) -0.0027(14) -0.0035(14) -0.0065(12) N3 0.0342(15) 0.0357(16) 0.070(2) -0.0028(14) -0.0047(14) -0.0093(13) N4 0.0285(14) 0.0384(15) 0.0462(16) -0.0046(12) -0.0032(11) -0.0103(12) N5 0.0374(16) 0.0356(14) 0.0352(14) -0.0109(11) 0.0026(12) -0.0131(12) C1 0.0267(16) 0.0357(17) 0.0404(17) -0.0118(14) -0.0040(13) -0.0019(13) C2 0.0255(16) 0.051(2) 0.054(2) -0.0115(17) -0.0069(14) -0.0057(15) C3 0.0312(18) 0.046(2) 0.063(2) -0.0110(18) -0.0115(16) 0.0036(15) C4 0.0393(19) 0.0356(18) 0.052(2) -0.0076(15) -0.0091(15) -0.0022(15) C5 0.0343(17) 0.0357(17) 0.0350(16) -0.0129(13) -0.0050(13) -0.0071(13) C6 0.0307(16) 0.0307(16) 0.0419(17) -0.0126(13) -0.0037(13) -0.0043(13) C7 0.0336(17) 0.0311(17) 0.0422(17) -0.0093(14) -0.0011(13) -0.0114(13) C8 0.0311(17) 0.0360(17) 0.0437(18) -0.0100(14) -0.0058(13) -0.0096(13) C9 0.039(2) 0.041(2) 0.064(2) 0.0070(17) -0.0083(17) -0.0152(16) C10 0.0330(19) 0.055(2) 0.076(3) 0.005(2) -0.0014(18) -0.0203(17) C11 0.0313(18) 0.049(2) 0.061(2) -0.0054(17) -0.0060(16) -0.0130(16) C12 0.0303(17) 0.0365(17) 0.0451(18) -0.0081(14) 0.0000(13) -0.0130(14) C13 0.0189(13) 0.0262(14) 0.0342(15) -0.0081(12) -0.0027(11) -0.0044(11) C14 0.0237(14) 0.0305(15) 0.0341(15) -0.0066(12) -0.0058(12) -0.0096(12) C15 0.0249(14) 0.0276(15) 0.0325(15) -0.0092(12) 0.0008(11) -0.0072(12) C16 0.0194(14) 0.0318(16) 0.0428(17) -0.0086(13) 0.0000(12) -0.0079(12) C17 0.0213(14) 0.0295(15) 0.0401(16) -0.0079(13) -0.0081(12) -0.0064(11) C18 0.0286(15) 0.0320(15) 0.0319(15) -0.0083(12) -0.0053(12) -0.0090(12) C19 0.0217(15) 0.0343(16) 0.0368(16) -0.0062(13) -0.0029(12) -0.0039(12) C20 0.0263(16) 0.0305(16) 0.0488(19) -0.0045(14) -0.0126(13) -0.0094(12) O9 0.175(7) 0.191(7) 0.165(6) -0.040(5) -0.029(5) -0.045(5) O8 0.271(7) 0.250(7) 0.238(7) -0.089(5) -0.049(5) -0.067(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 O2 2.222(2) . ? Cd1 O3 2.274(2) 2_666 ? Cd1 N1 2.348(3) . ? Cd1 N4 2.353(3) 2_766 ? Cd1 O4 2.369(2) 1_655 ? Cd1 O5 2.395(2) 1_655 ? Cd1 C20 2.705(3) 1_655 ? O1 C7 1.357(4) . ? O1 C6 1.368(4) . ? O2 C19 1.246(4) . ? O3 C19 1.227(4) . ? O3 Cd1 2.274(2) 2_666 ? O4 C20 1.247(4) . ? O4 Cd1 2.369(2) 1_455 ? O5 C20 1.249(4) . ? O5 Cd1 2.395(2) 1_455 ? O6 N5 1.225(4) . ? O7 N5 1.213(4) . ? N1 C1 1.328(4) . ? N1 C2 1.333(4) . ? N2 C6 1.279(4) . ? N2 N3 1.408(4) . ? N3 C7 1.284(4) . ? N4 C11 1.329(4) . ? N4 C12 1.335(4) . ? N4 Cd1 2.353(3) 2_766 ? N5 C15 1.467(4) . ? C1 C5 1.383(5) . ? C1 H1 0.9300 . ? C2 C3 1.372(5) . ? C2 H2 0.9300 . ? C3 C4 1.372(5) . ? C3 H3 0.9300 . ? C4 C5 1.391(4) . ? C4 H4 0.9300 . ? C5 C6 1.456(4) . ? C7 C8 1.456(4) . ? C8 C12 1.372(5) . ? C8 C9 1.393(5) . ? C9 C10 1.370(5) . ? C9 H9 0.9300 . ? C10 C11 1.374(5) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.392(4) . ? C13 C18 1.396(4) . ? C13 C19 1.500(4) . ? C14 C15 1.378(4) . ? C14 H14 0.9300 . ? C15 C16 1.383(4) . ? C16 C17 1.388(4) . ? C16 H16 0.9300 . ? C17 C18 1.387(4) . ? C17 C20 1.510(4) . ? C18 H18 0.9300 . ? C20 Cd1 2.705(3) 1_455 ? O9 O9 1.51(2) 2_667 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Cd1 O3 127.98(9) . 2_666 ? O2 Cd1 N1 92.91(10) . . ? O3 Cd1 N1 89.47(11) 2_666 . ? O2 Cd1 N4 93.67(10) . 2_766 ? O3 Cd1 N4 84.76(11) 2_666 2_766 ? N1 Cd1 N4 173.06(9) . 2_766 ? O2 Cd1 O4 143.34(9) . 1_655 ? O3 Cd1 O4 88.64(9) 2_666 1_655 ? N1 Cd1 O4 88.67(9) . 1_655 ? N4 Cd1 O4 87.36(9) 2_766 1_655 ? O2 Cd1 O5 88.41(9) . 1_655 ? O3 Cd1 O5 143.55(9) 2_666 1_655 ? N1 Cd1 O5 90.80(10) . 1_655 ? N4 Cd1 O5 91.56(10) 2_766 1_655 ? O4 Cd1 O5 54.93(8) 1_655 1_655 ? O2 Cd1 C20 115.89(10) . 1_655 ? O3 Cd1 C20 116.04(10) 2_666 1_655 ? N1 Cd1 C20 90.52(9) . 1_655 ? N4 Cd1 C20 88.57(9) 2_766 1_655 ? O4 Cd1 C20 27.45(9) 1_655 1_655 ? O5 Cd1 C20 27.51(9) 1_655 1_655 ? C7 O1 C6 102.2(2) . . ? C19 O2 Cd1 109.6(2) . . ? C19 O3 Cd1 179.2(2) . 2_666 ? C20 O4 Cd1 91.44(18) . 1_455 ? C20 O5 Cd1 90.2(2) . 1_455 ? C1 N1 C2 117.6(3) . . ? C1 N1 Cd1 116.6(2) . . ? C2 N1 Cd1 124.9(2) . . ? C6 N2 N3 106.0(3) . . ? C7 N3 N2 106.3(3) . . ? C11 N4 C12 117.8(3) . . ? C11 N4 Cd1 124.0(2) . 2_766 ? C12 N4 Cd1 118.1(2) . 2_766 ? O7 N5 O6 124.2(3) . . ? O7 N5 C15 117.9(3) . . ? O6 N5 C15 117.9(3) . . ? N1 C1 C5 123.2(3) . . ? N1 C1 H1 118.4 . . ? C5 C1 H1 118.4 . . ? N1 C2 C3 123.0(3) . . ? N1 C2 H2 118.5 . . ? C3 C2 H2 118.5 . . ? C4 C3 C2 119.7(3) . . ? C4 C3 H3 120.2 . . ? C2 C3 H3 120.2 . . ? C3 C4 C5 117.9(3) . . ? C3 C4 H4 121.1 . . ? C5 C4 H4 121.1 . . ? C1 C5 C4 118.6(3) . . ? C1 C5 C6 120.4(3) . . ? C4 C5 C6 120.9(3) . . ? N2 C6 O1 112.8(3) . . ? N2 C6 C5 128.7(3) . . ? O1 C6 C5 118.5(3) . . ? N3 C7 O1 112.6(3) . . ? N3 C7 C8 128.2(3) . . ? O1 C7 C8 119.2(3) . . ? C12 C8 C9 118.6(3) . . ? C12 C8 C7 121.3(3) . . ? C9 C8 C7 120.0(3) . . ? C10 C9 C8 118.1(3) . . ? C10 C9 H9 120.9 . . ? C8 C9 H9 120.9 . . ? C9 C10 C11 119.6(3) . . ? C9 C10 H10 120.2 . . ? C11 C10 H10 120.2 . . ? N4 C11 C10 122.8(3) . . ? N4 C11 H11 118.6 . . ? C10 C11 H11 118.6 . . ? N4 C12 C8 123.1(3) . . ? N4 C12 H12 118.4 . . ? C8 C12 H12 118.4 . . ? C14 C13 C18 120.0(3) . . ? C14 C13 C19 118.7(3) . . ? C18 C13 C19 121.3(3) . . ? C15 C14 C13 118.6(3) . . ? C15 C14 H14 120.7 . . ? C13 C14 H14 120.7 . . ? C14 C15 C16 122.4(3) . . ? C14 C15 N5 118.8(3) . . ? C16 C15 N5 118.8(3) . . ? C15 C16 C17 118.6(3) . . ? C15 C16 H16 120.7 . . ? C17 C16 H16 120.7 . . ? C18 C17 C16 120.3(3) . . ? C18 C17 C20 120.7(3) . . ? C16 C17 C20 119.0(3) . . ? C17 C18 C13 120.0(3) . . ? C17 C18 H18 120.0 . . ? C13 C18 H18 120.0 . . ? O3 C19 O2 122.9(3) . . ? O3 C19 C13 120.1(3) . . ? O2 C19 C13 117.0(3) . . ? O4 C20 O5 123.3(3) . . ? O4 C20 C17 118.5(3) . . ? O5 C20 C17 118.2(3) . . ? O4 C20 Cd1 61.11(16) . 1_455 ? O5 C20 Cd1 62.29(17) . 1_455 ? C17 C20 Cd1 176.4(2) . 1_455 ? 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 O3 Cd1 O2 C19 5.7(3) 2_666 . . . ? N1 Cd1 O2 C19 97.3(2) . . . . ? N4 Cd1 O2 C19 -80.5(3) 2_766 . . . ? O4 Cd1 O2 C19 -171.05(19) 1_655 . . . ? O5 Cd1 O2 C19 -172.0(2) 1_655 . . . ? C20 Cd1 O2 C19 -170.7(2) 1_655 . . . ? O2 Cd1 N1 C1 159.7(2) . . . . ? O3 Cd1 N1 C1 -72.3(2) 2_666 . . . ? O4 Cd1 N1 C1 16.3(2) 1_655 . . . ? O5 Cd1 N1 C1 71.2(2) 1_655 . . . ? C20 Cd1 N1 C1 43.7(2) 1_655 . . . ? O2 Cd1 N1 C2 -9.0(3) . . . . ? O3 Cd1 N1 C2 119.0(3) 2_666 . . . ? O4 Cd1 N1 C2 -152.4(3) 1_655 . . . ? O5 Cd1 N1 C2 -97.5(3) 1_655 . . . ? C20 Cd1 N1 C2 -125.0(3) 1_655 . . . ? C6 N2 N3 C7 0.6(4) . . . . ? C2 N1 C1 C5 2.3(5) . . . . ? Cd1 N1 C1 C5 -167.3(2) . . . . ? C1 N1 C2 C3 -0.9(5) . . . . ? Cd1 N1 C2 C3 167.7(3) . . . . ? N1 C2 C3 C4 -1.0(6) . . . . ? C2 C3 C4 C5 1.5(6) . . . . ? N1 C1 C5 C4 -1.7(5) . . . . ? N1 C1 C5 C6 178.4(3) . . . . ? C3 C4 C5 C1 -0.3(5) . . . . ? C3 C4 C5 C6 179.7(3) . . . . ? N3 N2 C6 O1 0.0(4) . . . . ? N3 N2 C6 C5 179.8(3) . . . . ? C7 O1 C6 N2 -0.5(4) . . . . ? C7 O1 C6 C5 179.6(3) . . . . ? C1 C5 C6 N2 172.6(3) . . . . ? C4 C5 C6 N2 -7.4(6) . . . . ? C1 C5 C6 O1 -7.5(5) . . . . ? C4 C5 C6 O1 172.5(3) . . . . ? N2 N3 C7 O1 -1.0(4) . . . . ? N2 N3 C7 C8 178.9(3) . . . . ? C6 O1 C7 N3 1.0(4) . . . . ? C6 O1 C7 C8 -178.9(3) . . . . ? N3 C7 C8 C12 176.9(4) . . . . ? O1 C7 C8 C12 -3.3(5) . . . . ? N3 C7 C8 C9 -4.3(6) . . . . ? O1 C7 C8 C9 175.6(3) . . . . ? C12 C8 C9 C10 -0.9(6) . . . . ? C7 C8 C9 C10 -179.8(4) . . . . ? C8 C9 C10 C11 1.0(7) . . . . ? C12 N4 C11 C10 -0.4(6) . . . . ? Cd1 N4 C11 C10 177.2(3) 2_766 . . . ? C9 C10 C11 N4 -0.3(7) . . . . ? C11 N4 C12 C8 0.4(5) . . . . ? Cd1 N4 C12 C8 -177.3(3) 2_766 . . . ? C9 C8 C12 N4 0.2(5) . . . . ? C7 C8 C12 N4 179.1(3) . . . . ? C18 C13 C14 C15 -1.3(4) . . . . ? C19 C13 C14 C15 178.5(3) . . . . ? C13 C14 C15 C16 -1.4(4) . . . . ? C13 C14 C15 N5 177.9(3) . . . . ? O7 N5 C15 C14 -14.5(4) . . . . ? O6 N5 C15 C14 165.0(3) . . . . ? O7 N5 C15 C16 164.7(3) . . . . ? O6 N5 C15 C16 -15.7(4) . . . . ? C14 C15 C16 C17 2.2(4) . . . . ? N5 C15 C16 C17 -177.0(3) . . . . ? C15 C16 C17 C18 -0.4(4) . . . . ? C15 C16 C17 C20 177.3(3) . . . . ? C16 C17 C18 C13 -2.2(4) . . . . ? C20 C17 C18 C13 -179.8(3) . . . . ? C14 C13 C18 C17 3.0(4) . . . . ? C19 C13 C18 C17 -176.7(3) . . . . ? Cd1 O2 C19 O3 -5.5(4) . . . . ? Cd1 O2 C19 C13 173.8(2) . . . . ? C14 C13 C19 O3 164.6(3) . . . . ? C18 C13 C19 O3 -15.6(5) . . . . ? C14 C13 C19 O2 -14.7(4) . . . . ? C18 C13 C19 O2 165.1(3) . . . . ? Cd1 O4 C20 O5 -3.3(3) 1_455 . . . ? Cd1 O4 C20 C17 176.0(2) 1_455 . . . ? Cd1 O5 C20 O4 3.3(3) 1_455 . . . ? Cd1 O5 C20 C17 -176.0(2) 1_455 . . . ? C18 C17 C20 O4 8.3(4) . . . . ? C16 C17 C20 O4 -169.4(3) . . . . ? C18 C17 C20 O5 -172.3(3) . . . . ? C16 C17 C20 O5 10.0(4) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.952 _refine_diff_density_min -0.310 _refine_diff_density_rms 0.076 #===END