# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_1 _database_code_depnum_ccdc_archive 'CCDC 862815' #TrackingRef '1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H38 Cd3 N10 O18' _chemical_formula_weight 1380.12 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 11.175(2) _cell_length_b 11.499(2) _cell_length_c 22.243(4) _cell_angle_alpha 83.95(3) _cell_angle_beta 83.06(3) _cell_angle_gamma 76.05(3) _cell_volume 2745.0(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.670 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2310 _exptl_absorpt_coefficient_mu 1.231 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.766 _exptl_absorpt_correction_T_max 0.853 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16678 _diffrn_reflns_av_R_equivalents 0.0463 _diffrn_reflns_av_sigmaI/netI 0.0708 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9516 _reflns_number_gt 7609 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1007P)^2^+80.0000P] 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 9516 _refine_ls_number_parameters 721 _refine_ls_number_restraints 33 _refine_ls_R_factor_all 0.1225 _refine_ls_R_factor_gt 0.1036 _refine_ls_wR_factor_ref 0.2745 _refine_ls_wR_factor_gt 0.2605 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.38996(9) 0.22856(9) 1.01073(4) 0.0364(3) Uani 1 1 d . . . Cd2 Cd 1.34731(10) 0.20042(12) 0.74286(5) 0.0547(4) Uani 1 1 d . . . Cd3 Cd 1.27541(9) 1.11353(9) 0.48717(4) 0.0362(3) Uani 1 1 d . . . C1 C 0.2044(13) 0.1059(13) 1.0105(7) 0.048(3) Uani 1 1 d . . . C2 C 0.0985(12) 0.0511(12) 1.0051(7) 0.042(3) Uani 1 1 d . . . C3 C -0.0053(14) 0.0707(14) 1.0477(7) 0.050(4) Uani 1 1 d . . . C4 C 0.1013(14) -0.0205(14) 0.9570(7) 0.049(4) Uani 1 1 d . . . C5 C 0.6140(13) 0.2317(13) 0.9403(6) 0.045(3) Uani 1 1 d . . . C6 C 0.7326(12) 0.2160(12) 0.9001(6) 0.041(3) Uani 1 1 d . . . C7 C 0.8309(14) 0.2606(14) 0.9136(6) 0.050(4) Uani 1 1 d . . . H7A H 0.8221 0.3016 0.9484 0.060 Uiso 1 1 calc R . . C8 C 0.9386(14) 0.2454(13) 0.8773(7) 0.048(3) Uani 1 1 d . . . H8A H 1.0018 0.2781 0.8868 0.058 Uiso 1 1 calc R . . C9 C 0.9566(13) 0.1808(12) 0.8252(6) 0.043(3) Uani 1 1 d . . . C10 C 0.8590(14) 0.1363(17) 0.8106(7) 0.060(4) Uani 1 1 d . . . H10A H 0.8678 0.0962 0.7756 0.072 Uiso 1 1 calc R . . C11 C 0.7480(14) 0.1517(17) 0.8486(7) 0.060(4) Uani 1 1 d . . . H11A H 0.6843 0.1192 0.8396 0.072 Uiso 1 1 calc R . . C12 C 1.0792(13) 0.1560(13) 0.7857(7) 0.045(3) Uani 1 1 d . . . C13 C 1.3248(13) 0.4423(15) 0.7013(7) 0.050(4) Uani 1 1 d . . . C14 C 1.3092(12) 0.5617(13) 0.6675(6) 0.042(3) Uani 1 1 d . . . C15 C 1.2472(14) 0.5840(14) 0.6142(7) 0.051(4) Uani 1 1 d . . . H15A H 1.2134 0.5247 0.6024 0.061 Uiso 1 1 calc R . . C16 C 1.2361(13) 0.6909(13) 0.5799(6) 0.045(3) Uani 1 1 d . . . H16A H 1.1948 0.7023 0.5450 0.054 Uiso 1 1 calc R . . C17 C 1.2835(12) 0.7817(12) 0.5949(6) 0.038(3) Uani 1 1 d . . . C18 C 1.3455(16) 0.7627(13) 0.6482(7) 0.053(4) Uani 1 1 d . . . H18A H 1.3781 0.8227 0.6602 0.063 Uiso 1 1 calc R . . C19 C 1.3567(14) 0.6524(14) 0.6822(6) 0.049(4) Uani 1 1 d . . . H19A H 1.3989 0.6400 0.7168 0.058 Uiso 1 1 calc R . . C20 C 1.2736(12) 0.8984(13) 0.5572(6) 0.042(3) Uani 1 1 d . . . C21 C 1.3983(18) 1.2969(18) 0.4917(10) 0.071(3) Uani 1 1 d U . . C22 C 1.4520(13) 1.3985(13) 0.4964(7) 0.045(3) Uani 1 1 d . . . C23 C 1.4272(14) 1.4995(16) 0.4526(8) 0.059(4) Uani 1 1 d . . . C24 C 1.5247(13) 1.4030(13) 0.5427(7) 0.047(3) Uani 1 1 d . . . C25 C 0.2841(13) 0.5048(12) 0.9578(6) 0.043(3) Uani 1 1 d . . . H25A H 0.3220 0.5205 0.9901 0.052 Uiso 1 1 calc R . . C26 C 0.2345(13) 0.5998(13) 0.9191(6) 0.044(3) Uani 1 1 d . . . H26A H 0.2384 0.6775 0.9252 0.053 Uiso 1 1 calc R . . C27 C 0.1786(13) 0.5785(13) 0.8707(6) 0.044(3) Uani 1 1 d . . . C28 C 0.1725(13) 0.4628(13) 0.8645(6) 0.046(3) Uani 1 1 d . . . H28A H 0.1338 0.4465 0.8327 0.055 Uiso 1 1 calc R . . C29 C 0.2237(13) 0.3706(14) 0.9052(7) 0.048(4) Uani 1 1 d . . . H29A H 0.2189 0.2925 0.9005 0.058 Uiso 1 1 calc R . . C30 C 0.1307(12) 0.6765(12) 0.8254(6) 0.038(3) Uani 1 1 d . . . C31 C 0.0411(13) 0.7657(13) 0.7510(6) 0.041(3) Uani 1 1 d . . . C32 C -0.0263(13) 0.7978(13) 0.6959(6) 0.041(3) Uani 1 1 d . . . C33 C -0.0493(14) 0.9104(14) 0.6652(6) 0.048(3) Uani 1 1 d . . . H33A H -0.0212 0.9721 0.6785 0.058 Uiso 1 1 calc R . . C34 C -0.1142(15) 0.9308(13) 0.6148(7) 0.050(4) Uani 1 1 d . . . H34A H -0.1281 1.0070 0.5944 0.061 Uiso 1 1 calc R . . C35 C -0.1318(15) 0.7348(14) 0.6239(7) 0.054(4) Uani 1 1 d . . . H35A H -0.1584 0.6739 0.6089 0.065 Uiso 1 1 calc R . . H36A H -0.0551 0.6287 0.6945 0.065 Uiso 1 1 d R . . C36 C -0.0694(15) 0.7078(13) 0.6742(7) 0.050(4) Uani 1 1 d . . . C37 C 1.1222(14) 1.2716(14) 0.5934(7) 0.049(4) Uani 1 1 d . . . H37A H 1.2018 1.2802 0.5966 0.058 Uiso 1 1 calc R . . C38 C 1.0297(14) 1.3229(13) 0.6352(7) 0.048(4) Uani 1 1 d . . . H38A H 1.0463 1.3666 0.6647 0.058 Uiso 1 1 calc R . . C39 C 0.9123(12) 1.3089(12) 0.6327(6) 0.037(3) Uani 1 1 d . . . C40 C 0.8913(13) 1.2468(13) 0.5863(6) 0.046(3) Uani 1 1 d . . . H40A H 0.8123 1.2376 0.5823 0.055 Uiso 1 1 calc R . . C41 C 0.9910(14) 1.1991(13) 0.5463(6) 0.046(3) Uani 1 1 d . . . H41A H 0.9774 1.1563 0.5155 0.056 Uiso 1 1 calc R . . C42 C 0.8118(12) 1.3591(13) 0.6787(6) 0.041(3) Uani 1 1 d . . . C43 C 0.7188(12) 1.4533(13) 0.7532(6) 0.040(3) Uani 1 1 d . . . C44 C 0.6903(12) 1.5213(12) 0.8074(6) 0.038(3) Uani 1 1 d . . . C45 C 0.7844(14) 1.5610(14) 0.8271(7) 0.051(4) Uani 1 1 d . . . H45A H 0.8635 1.5449 0.8066 0.061 Uiso 1 1 calc R . . C46 C 0.7590(13) 1.6251(13) 0.8778(6) 0.042(3) Uani 1 1 d . . . H46A H 0.8231 1.6503 0.8918 0.051 Uiso 1 1 calc R . . C47 C 0.5563(13) 1.6112(15) 0.8881(6) 0.048(4) Uani 1 1 d . . . H47A H 0.4777 1.6298 0.9089 0.058 Uiso 1 1 calc R . . C48 C 0.5735(13) 1.5451(14) 0.8403(7) 0.048(4) Uani 1 1 d . . . H48A H 0.5093 1.5158 0.8294 0.057 Uiso 1 1 calc R . . N1 N 0.2817(10) 0.3922(11) 0.9524(5) 0.043(3) Uani 1 1 d . . . N2 N 0.0914(11) 0.8437(10) 0.7747(5) 0.045(3) Uani 1 1 d . . . N3 N 0.1499(11) 0.7848(11) 0.8241(5) 0.045(3) Uani 1 1 d . . . N4 N 0.0642(10) 0.6619(10) 0.7803(5) 0.040(3) Uani 1 1 d . . . N5 N -0.1574(11) 0.8468(11) 0.5943(5) 0.046(3) Uani 1 1 d . . . N6 N 1.1072(10) 1.2111(10) 0.5493(5) 0.042(3) Uani 1 1 d . . . N7 N 0.6385(11) 1.4028(11) 0.7306(5) 0.043(3) Uani 1 1 d . . . N8 N 0.6971(10) 1.3413(11) 0.6805(5) 0.045(3) Uani 1 1 d . . . N9 N 0.8293(10) 1.4285(10) 0.7220(5) 0.042(3) Uani 1 1 d . . . N10 N 0.6473(10) 1.6524(10) 0.9077(5) 0.040(3) Uani 1 1 d . . . O1 O 0.2000(12) 0.1700(11) 1.0523(6) 0.071(3) Uani 1 1 d . . . O2 O 0.2966(10) 0.0918(10) 0.9708(6) 0.064(3) Uani 1 1 d . . . O3 O 0.5987(10) 0.2881(12) 0.9856(5) 0.067(3) Uani 1 1 d . . . O4 O 0.5306(9) 0.1826(11) 0.9259(5) 0.060(3) Uani 1 1 d . . . O5 O 1.1580(9) 0.2131(11) 0.7951(5) 0.056(3) Uani 1 1 d . . . O6 O 1.0935(10) 0.0798(10) 0.7481(5) 0.054(3) Uani 1 1 d . . . O7 O 1.2783(13) 0.3665(11) 0.6868(7) 0.080(4) Uani 1 1 d . . . O8 O 1.3896(11) 0.4199(11) 0.7447(6) 0.069(3) Uani 1 1 d . . . O9 O 1.3298(9) 0.9729(8) 0.5707(4) 0.044(2) Uani 1 1 d . . . O10 O 1.2149(11) 0.9169(10) 0.5113(5) 0.059(3) Uani 1 1 d . . . O11 O 1.3310(12) 1.2988(12) 0.4505(7) 0.080(3) Uani 1 1 d U . . O12 O 1.4219(12) 1.2059(11) 0.5281(7) 0.078(3) Uani 1 1 d U . . O13 O 0.5038(12) 0.0707(13) 1.0717(5) 0.077(4) Uani 1 1 d . . . O14 O 1.3117(12) 0.0592(12) 0.6866(6) 0.077(4) Uani 1 1 d . . . O15 O 1.5424(14) 0.1620(15) 0.6843(8) 0.102(6) Uani 1 1 d . . . O16 O 1.428(2) 0.149(2) 0.8244(10) 0.151(8) Uani 1 1 d U . . O17 O 1.4350(10) 0.9971(12) 0.4242(5) 0.065(3) Uani 1 1 d . . . O18 O 0.627(4) 0.108(4) 0.1742(18) 0.120(12) Uani 0.50 1 d PU . . O19 O 0.563(5) 0.860(4) 0.743(2) 0.19(2) Uani 0.50 1 d PU . . H13A H 0.5842 0.0649 1.0742 0.224 Uiso 1 1 d R . . H13B H 0.4716 0.0198 1.0928 0.224 Uiso 1 1 d R . . H14A H 1.3699 0.0274 0.6605 0.224 Uiso 1 1 d R . . H14B H 1.2448 0.0401 0.6927 0.224 Uiso 1 1 d R . . H15B H 1.5617 0.1118 0.6582 0.224 Uiso 1 1 d R . . H15C H 1.6003 0.2005 0.6901 0.224 Uiso 1 1 d R . . H16B H 1.5090 0.1223 0.8251 0.224 Uiso 1 1 d R . . H16C H 1.3852 0.1479 0.8590 0.224 Uiso 1 1 d R . . H17A H 1.4424 0.9234 0.4231 0.224 Uiso 1 1 d R . . H17B H 1.4919 1.0304 0.4033 0.224 Uiso 1 1 d R . . H19 H 0.5001 0.8769 0.7686 0.224 Uiso 1 1 d R . . H18 H 0.6111 0.0236 0.1806 0.224 Uiso 1 1 d R . . H2 H 0.0952 0.9207 0.7667 0.224 Uiso 1 1 d R . . H7 H 0.5612 1.4094 0.7356 0.224 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 0.0359(5) 0.0405(5) 0.0356(5) -0.0142(4) -0.0035(4) -0.0096(4) Cd2 0.0459(6) 0.0782(9) 0.0437(6) -0.0118(6) -0.0009(5) -0.0203(6) Cd3 0.0375(5) 0.0399(5) 0.0339(5) -0.0085(4) -0.0072(4) -0.0102(4) C1 0.043(8) 0.045(8) 0.060(9) -0.005(7) -0.006(7) -0.017(6) C2 0.039(7) 0.031(7) 0.055(8) -0.003(6) -0.012(6) -0.005(6) C3 0.044(8) 0.059(9) 0.047(8) -0.020(7) 0.005(6) -0.013(7) C4 0.054(9) 0.053(9) 0.045(8) -0.022(7) 0.013(7) -0.023(7) C5 0.042(8) 0.051(9) 0.043(8) -0.013(7) 0.002(6) -0.012(7) C6 0.041(7) 0.043(8) 0.043(7) -0.016(6) -0.008(6) -0.012(6) C7 0.062(9) 0.061(10) 0.036(7) -0.015(7) -0.006(7) -0.026(8) C8 0.048(8) 0.049(8) 0.057(9) -0.011(7) -0.004(7) -0.025(7) C9 0.045(8) 0.039(7) 0.047(8) -0.002(6) -0.004(6) -0.016(6) C10 0.042(8) 0.090(13) 0.054(9) -0.030(9) -0.005(7) -0.019(8) C11 0.041(8) 0.092(13) 0.058(10) -0.036(9) 0.000(7) -0.027(8) C12 0.044(8) 0.043(8) 0.048(8) -0.002(7) -0.008(6) -0.011(6) C13 0.035(7) 0.071(11) 0.044(8) 0.007(7) -0.001(6) -0.019(7) C14 0.038(7) 0.042(8) 0.045(8) -0.005(6) 0.000(6) -0.009(6) C15 0.055(9) 0.048(9) 0.061(9) -0.017(7) -0.004(7) -0.028(7) C16 0.049(8) 0.050(9) 0.042(8) -0.009(6) -0.020(6) -0.012(7) C17 0.042(7) 0.037(7) 0.034(7) -0.003(6) -0.008(6) -0.007(6) C18 0.082(11) 0.042(8) 0.041(8) -0.004(6) -0.011(7) -0.025(8) C19 0.063(9) 0.054(9) 0.039(7) -0.006(7) -0.015(7) -0.028(8) C20 0.035(7) 0.048(8) 0.041(7) -0.011(6) -0.007(6) 0.001(6) C21 0.064(7) 0.062(7) 0.096(9) -0.013(6) -0.001(6) -0.032(6) C22 0.046(8) 0.040(8) 0.052(8) -0.011(6) 0.003(6) -0.017(6) C23 0.044(8) 0.071(11) 0.063(10) -0.013(9) -0.009(7) -0.011(8) C24 0.046(8) 0.045(8) 0.050(8) 0.009(7) -0.006(6) -0.018(7) C25 0.054(8) 0.040(8) 0.041(7) -0.003(6) -0.015(6) -0.016(6) C26 0.052(8) 0.047(8) 0.040(7) -0.021(6) -0.014(6) -0.012(7) C27 0.045(8) 0.047(8) 0.038(7) -0.008(6) 0.001(6) -0.009(6) C28 0.052(8) 0.052(9) 0.040(7) -0.005(6) -0.025(6) -0.013(7) C29 0.045(8) 0.046(8) 0.061(9) -0.015(7) -0.016(7) -0.016(7) C30 0.042(7) 0.038(7) 0.039(7) -0.010(6) -0.008(6) -0.013(6) C31 0.046(8) 0.050(8) 0.031(7) -0.008(6) -0.008(6) -0.016(6) C32 0.049(8) 0.044(8) 0.031(7) -0.003(6) -0.020(6) -0.004(6) C33 0.061(9) 0.055(9) 0.036(7) -0.006(7) -0.018(7) -0.020(7) C34 0.065(10) 0.039(8) 0.053(9) 0.000(7) -0.025(7) -0.016(7) C35 0.073(11) 0.044(9) 0.056(9) -0.013(7) -0.025(8) -0.022(8) C36 0.065(10) 0.034(7) 0.058(9) -0.002(7) -0.026(8) -0.015(7) C37 0.042(8) 0.059(9) 0.051(8) -0.020(7) -0.005(6) -0.017(7) C38 0.054(9) 0.049(9) 0.047(8) -0.025(7) -0.007(7) -0.012(7) C39 0.044(7) 0.036(7) 0.032(6) -0.013(5) -0.004(5) -0.008(6) C40 0.036(7) 0.056(9) 0.051(8) -0.023(7) -0.006(6) -0.010(6) C41 0.054(9) 0.053(9) 0.040(7) -0.014(7) -0.004(6) -0.023(7) C42 0.042(7) 0.046(8) 0.036(7) -0.012(6) 0.000(6) -0.013(6) C43 0.039(7) 0.048(8) 0.035(7) -0.017(6) 0.001(6) -0.010(6) C44 0.039(7) 0.045(8) 0.036(7) -0.015(6) -0.005(6) -0.014(6) C45 0.044(8) 0.057(9) 0.058(9) -0.026(8) -0.002(7) -0.014(7) C46 0.045(8) 0.057(9) 0.032(7) -0.020(6) -0.005(6) -0.017(7) C47 0.037(7) 0.075(10) 0.036(7) -0.020(7) 0.011(6) -0.020(7) C48 0.041(8) 0.057(9) 0.053(9) -0.026(7) -0.007(6) -0.018(7) N1 0.041(6) 0.054(7) 0.038(6) -0.005(5) -0.008(5) -0.013(5) N2 0.056(7) 0.039(6) 0.046(7) -0.011(5) -0.017(6) -0.013(5) N3 0.059(7) 0.053(7) 0.030(6) -0.006(5) -0.015(5) -0.016(6) N4 0.038(6) 0.047(7) 0.035(6) 0.002(5) -0.009(5) -0.012(5) N5 0.055(7) 0.046(7) 0.040(6) -0.003(5) -0.017(5) -0.010(6) N6 0.044(6) 0.044(7) 0.040(6) -0.015(5) -0.009(5) -0.009(5) N7 0.048(7) 0.050(7) 0.035(6) -0.020(5) 0.001(5) -0.014(5) N8 0.040(6) 0.059(8) 0.041(6) -0.022(6) -0.004(5) -0.013(6) N9 0.039(6) 0.044(7) 0.044(6) -0.015(5) -0.003(5) -0.009(5) N10 0.044(6) 0.047(7) 0.033(6) -0.013(5) -0.007(5) -0.012(5) O1 0.077(8) 0.076(8) 0.078(8) -0.030(7) -0.006(6) -0.043(7) O2 0.047(6) 0.060(7) 0.087(8) -0.014(6) 0.007(6) -0.022(5) O3 0.056(7) 0.098(9) 0.054(7) -0.037(7) 0.004(5) -0.022(6) O4 0.041(6) 0.090(9) 0.055(6) -0.023(6) 0.009(5) -0.025(6) O5 0.041(6) 0.077(8) 0.057(6) -0.014(6) 0.006(5) -0.032(5) O6 0.059(6) 0.059(6) 0.050(6) -0.015(5) 0.008(5) -0.030(5) O7 0.094(10) 0.057(7) 0.098(10) -0.009(7) 0.008(8) -0.040(7) O8 0.050(7) 0.071(8) 0.080(8) 0.022(7) 0.008(6) -0.021(6) O9 0.053(6) 0.037(5) 0.047(5) 0.004(4) -0.013(4) -0.016(4) O10 0.078(8) 0.054(7) 0.046(6) 0.007(5) -0.023(6) -0.015(6) O11 0.076(7) 0.079(7) 0.099(8) -0.016(6) -0.012(6) -0.041(6) O12 0.070(7) 0.057(6) 0.110(9) -0.013(6) 0.002(6) -0.020(6) O13 0.076(8) 0.089(9) 0.056(7) -0.012(7) -0.011(6) 0.010(7) O14 0.074(8) 0.076(8) 0.088(9) -0.041(7) 0.036(7) -0.035(7) O15 0.084(10) 0.119(12) 0.125(12) -0.066(10) 0.044(9) -0.069(9) O16 0.142(11) 0.174(12) 0.137(11) -0.023(9) -0.037(8) -0.022(8) O17 0.041(6) 0.098(9) 0.053(6) -0.016(6) 0.001(5) -0.011(6) O18 0.121(13) 0.122(13) 0.120(13) -0.012(5) -0.016(5) -0.030(6) O19 0.19(2) 0.19(2) 0.19(2) -0.012(5) -0.020(6) -0.041(7) _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 2.325(10) . y Cd1 N10 2.325(10) 2_677 y Cd1 N1 2.335(12) . y Cd1 O13 2.352(13) . y Cd1 O2 2.379(11) . y Cd1 O1 2.429(12) . y Cd1 O3 2.568(12) . y Cd2 O16 2.09(2) . y Cd2 O7 2.195(14) . y Cd2 O5 2.267(10) . y Cd2 O14 2.285(12) . y Cd2 O15 2.370(13) . y Cd3 N5 2.312(11) 2_676 y Cd3 N6 2.320(11) . y Cd3 O17 2.361(11) . y Cd3 O9 2.367(9) . y Cd3 O11 2.396(13) . y Cd3 O12 2.458(14) . y Cd3 O10 2.500(11) . y C1 O1 1.235(18) . ? C1 O2 1.264(18) . ? C1 C2 1.491(19) . ? C2 C3 1.39(2) . ? C2 C4 1.411(19) . ? C3 C4 1.35(2) 2_557 ? C4 C3 1.35(2) 2_557 ? C5 O3 1.229(17) . ? C5 O4 1.286(18) . ? C5 C6 1.490(19) . ? C6 C7 1.395(19) . ? C6 C11 1.398(19) . ? C7 C8 1.35(2) . ? C7 H7A 0.9300 . ? C8 C9 1.41(2) . ? C8 H8A 0.9300 . ? C9 C10 1.39(2) . ? C9 C12 1.52(2) . ? C10 C11 1.40(2) . ? C10 H10A 0.9300 . ? C11 H11A 0.9300 . ? C12 O6 1.243(17) . ? C12 O5 1.267(17) . ? C13 O7 1.21(2) . ? C13 O8 1.244(19) . ? C13 C14 1.48(2) . ? C14 C19 1.363(19) . ? C14 C15 1.41(2) . ? C15 C16 1.36(2) . ? C15 H15A 0.9300 . ? C16 C17 1.367(19) . ? C16 H16A 0.9300 . ? C17 C18 1.42(2) . ? C17 C20 1.49(2) . ? C18 C19 1.39(2) . ? C18 H18A 0.9300 . ? C19 H19A 0.9300 . ? C20 O10 1.252(16) . ? C20 O9 1.256(17) . ? C21 O11 1.25(2) . ? C21 O12 1.25(2) . ? C21 C22 1.45(2) . ? C22 C24 1.40(2) . ? C22 C23 1.43(2) . ? C23 C24 1.37(2) 2_886 ? C24 C23 1.37(2) 2_886 ? C25 N1 1.319(18) . ? C25 C26 1.37(2) . ? C25 H25A 0.9300 . ? C26 C27 1.377(19) . ? C26 H26A 0.9300 . ? C27 C28 1.37(2) . ? C27 C30 1.47(2) . ? C28 C29 1.38(2) . ? C28 H28A 0.9300 . ? C29 N1 1.372(17) . ? C29 H29A 0.9300 . ? C30 N3 1.310(17) . ? C30 N4 1.365(16) . ? C31 N4 1.283(18) . ? C31 N2 1.347(17) . ? C31 C32 1.482(17) . ? C32 C33 1.38(2) . ? C32 C36 1.393(19) . ? C33 C34 1.377(19) . ? C33 H33A 0.9300 . ? C34 N5 1.322(18) . ? C34 H34A 0.9300 . ? C35 C36 1.36(2) . ? C35 N5 1.366(19) . ? C35 H35A 0.9300 . ? C36 H36A 0.9572 . ? C37 N6 1.309(17) . ? C37 C38 1.37(2) . ? C37 H37A 0.9300 . ? C38 C39 1.37(2) . ? C38 H38A 0.9300 . ? C39 C40 1.387(18) . ? C39 C42 1.475(18) . ? C40 C41 1.38(2) . ? C40 H40A 0.9300 . ? C41 N6 1.349(18) . ? C41 H41A 0.9300 . ? C42 N8 1.341(17) . ? C42 N9 1.373(17) . ? C43 N9 1.324(17) . ? C43 N7 1.348(17) . ? C43 C44 1.466(17) . ? C44 C45 1.376(19) . ? C44 C48 1.398(19) . ? C45 C46 1.376(19) . ? C45 H45A 0.9300 . ? C46 N10 1.324(17) . ? C46 H46A 0.9300 . ? C47 C48 1.340(19) . ? C47 N10 1.353(17) . ? C47 H47A 0.9300 . ? C48 H48A 0.9300 . ? N2 N3 1.376(16) . ? N2 H2 0.8952 . ? N5 Cd3 2.312(11) 2_676 ? N7 N8 1.392(15) . ? N7 H7 0.8430 . ? N10 Cd1 2.325(10) 2_677 ? O13 H13A 0.8932 . ? O13 H13B 0.8346 . ? O14 H14A 0.8551 . ? O14 H14B 0.8208 . ? O15 H15B 0.8346 . ? O15 H15C 0.8951 . ? O16 H16B 0.8803 . ? O16 H16C 0.8572 . ? O17 H17A 0.8340 . ? O17 H17B 0.8810 . ? O18 H18 1.0273 . ? O19 H19 0.8500 . ? 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 N10 140.4(4) . 2_677 y O4 Cd1 N1 88.5(4) . . y N10 Cd1 N1 88.8(4) 2_677 . y O4 Cd1 O13 92.1(4) . . y N10 Cd1 O13 88.9(4) 2_677 . y N1 Cd1 O13 177.0(5) . . y O4 Cd1 O2 81.3(4) . . y N10 Cd1 O2 138.3(4) 2_677 . y N1 Cd1 O2 92.3(4) . . y O13 Cd1 O2 90.7(5) . . y O4 Cd1 O1 134.6(4) . . y N10 Cd1 O1 84.9(4) 2_677 . y N1 Cd1 O1 91.9(4) . . y O13 Cd1 O1 89.8(5) . . y O2 Cd1 O1 53.3(4) . . y O4 Cd1 O3 53.2(3) . . y N10 Cd1 O3 87.7(4) 2_677 . y N1 Cd1 O3 94.2(4) . . y O13 Cd1 O3 83.8(5) . . y O2 Cd1 O3 133.7(4) . . y O1 Cd1 O3 170.3(4) . . y O16 Cd2 O7 138.3(8) . . y O16 Cd2 O5 89.3(7) . . y O7 Cd2 O5 91.3(5) . . y O16 Cd2 O14 120.4(8) . . y O7 Cd2 O14 101.2(5) . . y O5 Cd2 O14 89.9(4) . . y O16 Cd2 O15 92.3(8) . . y O7 Cd2 O15 92.5(6) . . y O5 Cd2 O15 172.3(4) . . y O14 Cd2 O15 82.8(4) . . y N5 Cd3 N6 90.3(4) 2_676 . y N5 Cd3 O17 87.7(4) 2_676 . y N6 Cd3 O17 173.7(4) . . y N5 Cd3 O9 142.7(4) 2_676 . y N6 Cd3 O9 88.2(4) . . y O17 Cd3 O9 89.7(4) . . y N5 Cd3 O11 84.1(5) 2_676 . y N6 Cd3 O11 92.1(5) . . y O17 Cd3 O11 93.7(5) . . y O9 Cd3 O11 133.2(4) . . y N5 Cd3 O12 136.9(5) 2_676 . y N6 Cd3 O12 93.4(4) . . y O17 Cd3 O12 92.1(4) . . y O9 Cd3 O12 80.4(4) . . y O11 Cd3 O12 52.8(5) . . y N5 Cd3 O10 89.5(4) 2_676 . y N6 Cd3 O10 91.8(4) . . y O17 Cd3 O10 82.2(4) . . y O9 Cd3 O10 53.4(3) . . y O11 Cd3 O10 172.5(4) . . y O12 Cd3 O10 133.2(4) . . y O1 C1 O2 119.5(13) . . ? O1 C1 C2 120.1(14) . . ? O2 C1 C2 120.3(14) . . ? C3 C2 C4 119.2(13) . . ? C3 C2 C1 120.1(13) . . ? C4 C2 C1 120.7(13) . . ? C4 C3 C2 120.2(13) 2_557 . ? C3 C4 C2 120.7(13) 2_557 . ? O3 C5 O4 122.1(13) . . ? O3 C5 C6 120.6(13) . . ? O4 C5 C6 117.2(12) . . ? C7 C6 C11 118.8(13) . . ? C7 C6 C5 121.4(12) . . ? C11 C6 C5 119.7(12) . . ? C8 C7 C6 121.3(13) . . ? C8 C7 H7A 119.3 . . ? C6 C7 H7A 119.3 . . ? C7 C8 C9 120.9(13) . . ? C7 C8 H8A 119.5 . . ? C9 C8 H8A 119.5 . . ? C10 C9 C8 118.5(13) . . ? C10 C9 C12 119.3(13) . . ? C8 C9 C12 122.1(12) . . ? C9 C10 C11 120.2(14) . . ? C9 C10 H10A 119.9 . . ? C11 C10 H10A 119.9 . . ? C6 C11 C10 120.1(14) . . ? C6 C11 H11A 119.9 . . ? C10 C11 H11A 119.9 . . ? O6 C12 O5 126.4(14) . . ? O6 C12 C9 116.9(12) . . ? O5 C12 C9 116.7(13) . . ? O7 C13 O8 120.1(16) . . ? O7 C13 C14 121.2(15) . . ? O8 C13 C14 118.7(15) . . ? C19 C14 C15 116.3(13) . . ? C19 C14 C13 124.3(14) . . ? C15 C14 C13 119.3(13) . . ? C16 C15 C14 121.3(13) . . ? C16 C15 H15A 119.3 . . ? C14 C15 H15A 119.3 . . ? C15 C16 C17 122.1(13) . . ? C15 C16 H16A 118.9 . . ? C17 C16 H16A 118.9 . . ? C16 C17 C18 118.1(13) . . ? C16 C17 C20 122.7(12) . . ? C18 C17 C20 119.2(12) . . ? C19 C18 C17 118.7(13) . . ? C19 C18 H18A 120.7 . . ? C17 C18 H18A 120.7 . . ? C14 C19 C18 123.4(14) . . ? C14 C19 H19A 118.3 . . ? C18 C19 H19A 118.3 . . ? O10 C20 O9 121.6(14) . . ? O10 C20 C17 119.3(13) . . ? O9 C20 C17 119.0(12) . . ? O11 C21 O12 119.7(17) . . ? O11 C21 C22 120.4(19) . . ? O12 C21 C22 119.9(18) . . ? C24 C22 C23 118.5(13) . . ? C24 C22 C21 122.9(15) . . ? C23 C22 C21 118.6(15) . . ? C24 C23 C22 119.1(14) 2_886 . ? C23 C24 C22 122.4(14) 2_886 . ? N1 C25 C26 124.3(13) . . ? N1 C25 H25A 117.9 . . ? C26 C25 H25A 117.9 . . ? C25 C26 C27 118.8(13) . . ? C25 C26 H26A 120.6 . . ? C27 C26 H26A 120.6 . . ? C28 C27 C26 118.3(13) . . ? C28 C27 C30 120.6(12) . . ? C26 C27 C30 121.0(13) . . ? C27 C28 C29 120.3(12) . . ? C27 C28 H28A 119.9 . . ? C29 C28 H28A 119.9 . . ? N1 C29 C28 121.0(13) . . ? N1 C29 H29A 119.5 . . ? C28 C29 H29A 119.5 . . ? N3 C30 N4 114.0(12) . . ? N3 C30 C27 123.2(12) . . ? N4 C30 C27 122.9(12) . . ? N4 C31 N2 111.4(12) . . ? N4 C31 C32 125.8(12) . . ? N2 C31 C32 122.7(13) . . ? C33 C32 C36 118.3(12) . . ? C33 C32 C31 124.5(13) . . ? C36 C32 C31 117.3(12) . . ? C34 C33 C32 119.7(13) . . ? C34 C33 H33A 120.1 . . ? C32 C33 H33A 120.1 . . ? N5 C34 C33 122.7(14) . . ? N5 C34 H34A 118.6 . . ? C33 C34 H34A 118.6 . . ? C36 C35 N5 123.4(13) . . ? C36 C35 H35A 118.3 . . ? N5 C35 H35A 118.3 . . ? C35 C36 C32 118.5(13) . . ? C35 C36 H36A 121.1 . . ? C32 C36 H36A 120.4 . . ? N6 C37 C38 124.9(14) . . ? N6 C37 H37A 117.6 . . ? C38 C37 H37A 117.6 . . ? C37 C38 C39 118.9(13) . . ? C37 C38 H38A 120.5 . . ? C39 C38 H38A 120.5 . . ? C38 C39 C40 118.4(12) . . ? C38 C39 C42 120.1(11) . . ? C40 C39 C42 121.6(12) . . ? C41 C40 C39 118.1(13) . . ? C41 C40 H40A 120.9 . . ? C39 C40 H40A 120.9 . . ? N6 C41 C40 123.5(12) . . ? N6 C41 H41A 118.2 . . ? C40 C41 H41A 118.2 . . ? N8 C42 N9 115.6(11) . . ? N8 C42 C39 122.3(12) . . ? N9 C42 C39 122.1(12) . . ? N9 C43 N7 111.2(11) . . ? N9 C43 C44 124.0(12) . . ? N7 C43 C44 124.7(12) . . ? C45 C44 C48 118.8(12) . . ? C45 C44 C43 117.9(12) . . ? C48 C44 C43 123.2(12) . . ? C44 C45 C46 118.6(14) . . ? C44 C45 H45A 120.7 . . ? C46 C45 H45A 120.7 . . ? N10 C46 C45 122.8(13) . . ? N10 C46 H46A 118.6 . . ? C45 C46 H46A 118.6 . . ? C48 C47 N10 123.5(13) . . ? C48 C47 H47A 118.3 . . ? N10 C47 H47A 118.3 . . ? C47 C48 C44 118.4(12) . . ? C47 C48 H48A 120.8 . . ? C44 C48 H48A 120.8 . . ? C25 N1 C29 117.2(12) . . ? C25 N1 Cd1 123.7(9) . . ? C29 N1 Cd1 118.7(10) . . ? C31 N2 N3 108.0(11) . . ? C31 N2 H2 136.6 . . ? N3 N2 H2 115.5 . . ? C30 N3 N2 102.9(10) . . ? C31 N4 C30 103.8(11) . . ? C34 N5 C35 117.3(12) . . ? C34 N5 Cd3 122.0(10) . 2_676 ? C35 N5 Cd3 120.6(9) . 2_676 ? C37 N6 C41 116.1(12) . . ? C37 N6 Cd3 121.2(10) . . ? C41 N6 Cd3 122.3(9) . . ? C43 N7 N8 109.7(11) . . ? C43 N7 H7 135.3 . . ? N8 N7 H7 114.0 . . ? C42 N8 N7 101.0(10) . . ? C43 N9 C42 102.4(11) . . ? C46 N10 C47 117.7(11) . . ? C46 N10 Cd1 120.5(8) . 2_677 ? C47 N10 Cd1 121.8(9) . 2_677 ? C1 O1 Cd1 92.7(10) . . ? C1 O2 Cd1 94.3(9) . . ? C5 O3 Cd1 87.3(9) . . ? C5 O4 Cd1 97.2(8) . . ? C12 O5 Cd2 125.6(10) . . ? C13 O7 Cd2 107.2(12) . . ? C20 O9 Cd3 95.6(8) . . ? C20 O10 Cd3 89.4(9) . . ? C21 O11 Cd3 94.9(12) . . ? C21 O12 Cd3 92.0(12) . . ? Cd1 O13 H13A 120.4 . . ? Cd1 O13 H13B 122.8 . . ? H13A O13 H13B 116.8 . . ? Cd2 O14 H14A 118.0 . . ? Cd2 O14 H14B 119.1 . . ? H14A O14 H14B 122.9 . . ? Cd2 O15 H15B 122.9 . . ? Cd2 O15 H15C 120.4 . . ? H15B O15 H15C 116.6 . . ? Cd2 O16 H16B 121.8 . . ? Cd2 O16 H16C 122.3 . . ? H16B O16 H16C 115.8 . . ? Cd3 O17 H17A 121.7 . . ? Cd3 O17 H17B 119.9 . . ? H17A O17 H17B 118.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 -1(2) . . . . ? O2 C1 C2 C3 -177.5(14) . . . . ? O1 C1 C2 C4 178.8(15) . . . . ? O2 C1 C2 C4 2(2) . . . . ? C4 C2 C3 C4 1(3) . . . 2_557 ? C1 C2 C3 C4 -179.7(15) . . . 2_557 ? C3 C2 C4 C3 -1(3) . . . 2_557 ? C1 C2 C4 C3 179.7(15) . . . 2_557 ? O3 C5 C6 C7 2(2) . . . . ? O4 C5 C6 C7 -176.7(15) . . . . ? O3 C5 C6 C11 -179.9(16) . . . . ? O4 C5 C6 C11 1(2) . . . . ? C11 C6 C7 C8 2(2) . . . . ? C5 C6 C7 C8 179.5(14) . . . . ? C6 C7 C8 C9 -2(2) . . . . ? C7 C8 C9 C10 2(2) . . . . ? C7 C8 C9 C12 -176.3(14) . . . . ? C8 C9 C10 C11 -3(3) . . . . ? C12 C9 C10 C11 176.0(16) . . . . ? C7 C6 C11 C10 -2(3) . . . . ? C5 C6 C11 C10 -179.9(16) . . . . ? C9 C10 C11 C6 3(3) . . . . ? C10 C9 C12 O6 -12(2) . . . . ? C8 C9 C12 O6 166.6(14) . . . . ? C10 C9 C12 O5 169.5(15) . . . . ? C8 C9 C12 O5 -12(2) . . . . ? O7 C13 C14 C19 178.4(16) . . . . ? O8 C13 C14 C19 -3(2) . . . . ? O7 C13 C14 C15 -5(2) . . . . ? O8 C13 C14 C15 173.2(14) . . . . ? C19 C14 C15 C16 0(2) . . . . ? C13 C14 C15 C16 -176.7(14) . . . . ? C14 C15 C16 C17 0(2) . . . . ? C15 C16 C17 C18 0(2) . . . . ? C15 C16 C17 C20 179.1(14) . . . . ? C16 C17 C18 C19 1(2) . . . . ? C20 C17 C18 C19 -178.5(13) . . . . ? C15 C14 C19 C18 1(2) . . . . ? C13 C14 C19 C18 177.2(15) . . . . ? C17 C18 C19 C14 -1(2) . . . . ? C16 C17 C20 O10 3(2) . . . . ? C18 C17 C20 O10 -177.5(14) . . . . ? C16 C17 C20 O9 -173.1(13) . . . . ? C18 C17 C20 O9 6(2) . . . . ? O11 C21 C22 C24 177.9(16) . . . . ? O12 C21 C22 C24 -4(3) . . . . ? O11 C21 C22 C23 -1(3) . . . . ? O12 C21 C22 C23 177.6(16) . . . . ? C24 C22 C23 C24 0(2) . . . 2_886 ? C21 C22 C23 C24 178.8(15) . . . 2_886 ? C23 C22 C24 C23 0(3) . . . 2_886 ? C21 C22 C24 C23 -178.7(16) . . . 2_886 ? N1 C25 C26 C27 0(2) . . . . ? C25 C26 C27 C28 2(2) . . . . ? C25 C26 C27 C30 -176.1(13) . . . . ? C26 C27 C28 C29 -1(2) . . . . ? C30 C27 C28 C29 176.3(13) . . . . ? C27 C28 C29 N1 0(2) . . . . ? C28 C27 C30 N3 -169.8(14) . . . . ? C26 C27 C30 N3 8(2) . . . . ? C28 C27 C30 N4 9(2) . . . . ? C26 C27 C30 N4 -173.4(13) . . . . ? N4 C31 C32 C33 -179.8(14) . . . . ? N2 C31 C32 C33 -3(2) . . . . ? N4 C31 C32 C36 1(2) . . . . ? N2 C31 C32 C36 177.2(14) . . . . ? C36 C32 C33 C34 0(2) . . . . ? C31 C32 C33 C34 -179.2(14) . . . . ? C32 C33 C34 N5 1(3) . . . . ? N5 C35 C36 C32 -2(3) . . . . ? C33 C32 C36 C35 0(2) . . . . ? C31 C32 C36 C35 179.8(15) . . . . ? N6 C37 C38 C39 2(3) . . . . ? C37 C38 C39 C40 -2(2) . . . . ? C37 C38 C39 C42 177.5(14) . . . . ? C38 C39 C40 C41 2(2) . . . . ? C42 C39 C40 C41 -177.8(13) . . . . ? C39 C40 C41 N6 -1(2) . . . . ? C38 C39 C42 N8 -175.7(14) . . . . ? C40 C39 C42 N8 4(2) . . . . ? C38 C39 C42 N9 5(2) . . . . ? C40 C39 C42 N9 -174.9(14) . . . . ? N9 C43 C44 C45 0(2) . . . . ? N7 C43 C44 C45 176.0(15) . . . . ? N9 C43 C44 C48 -179.1(14) . . . . ? N7 C43 C44 C48 -3(2) . . . . ? C48 C44 C45 C46 -1(2) . . . . ? C43 C44 C45 C46 179.9(14) . . . . ? C44 C45 C46 N10 -2(2) . . . . ? N10 C47 C48 C44 -3(3) . . . . ? C45 C44 C48 C47 3(2) . . . . ? C43 C44 C48 C47 -178.0(15) . . . . ? C26 C25 N1 C29 -1(2) . . . . ? C26 C25 N1 Cd1 171.3(11) . . . . ? C28 C29 N1 C25 1(2) . . . . ? C28 C29 N1 Cd1 -171.4(11) . . . . ? O4 Cd1 N1 C25 -105.3(11) . . . . ? N10 Cd1 N1 C25 35.2(11) 2_677 . . . ? O13 Cd1 N1 C25 -5(9) . . . . ? O2 Cd1 N1 C25 173.5(11) . . . . ? O1 Cd1 N1 C25 120.1(11) . . . . ? O3 Cd1 N1 C25 -52.4(11) . . . . ? O4 Cd1 N1 C29 66.8(10) . . . . ? N10 Cd1 N1 C29 -152.7(10) 2_677 . . . ? O13 Cd1 N1 C29 167(8) . . . . ? O2 Cd1 N1 C29 -14.4(10) . . . . ? O1 Cd1 N1 C29 -67.8(10) . . . . ? O3 Cd1 N1 C29 119.8(10) . . . . ? N4 C31 N2 N3 -1.0(16) . . . . ? C32 C31 N2 N3 -178.1(12) . . . . ? N4 C30 N3 N2 0.1(15) . . . . ? C27 C30 N3 N2 179.0(12) . . . . ? C31 N2 N3 C30 0.6(15) . . . . ? N2 C31 N4 C30 1.0(15) . . . . ? C32 C31 N4 C30 178.0(13) . . . . ? N3 C30 N4 C31 -0.7(16) . . . . ? C27 C30 N4 C31 -179.6(13) . . . . ? C33 C34 N5 C35 -2(2) . . . . ? C33 C34 N5 Cd3 176.5(12) . . . 2_676 ? C36 C35 N5 C34 3(2) . . . . ? C36 C35 N5 Cd3 -175.9(13) . . . 2_676 ? C38 C37 N6 C41 -1(2) . . . . ? C38 C37 N6 Cd3 -174.2(12) . . . . ? C40 C41 N6 C37 0(2) . . . . ? C40 C41 N6 Cd3 173.7(12) . . . . ? N5 Cd3 N6 C37 -146.3(12) 2_676 . . . ? O17 Cd3 N6 C37 141(3) . . . . ? O9 Cd3 N6 C37 70.9(12) . . . . ? O11 Cd3 N6 C37 -62.2(12) . . . . ? O12 Cd3 N6 C37 -9.3(12) . . . . ? O10 Cd3 N6 C37 124.2(12) . . . . ? N5 Cd3 N6 C41 40.6(11) 2_676 . . . ? O17 Cd3 N6 C41 -32(4) . . . . ? O9 Cd3 N6 C41 -102.2(11) . . . . ? O11 Cd3 N6 C41 124.7(11) . . . . ? O12 Cd3 N6 C41 177.6(11) . . . . ? O10 Cd3 N6 C41 -48.9(11) . . . . ? N9 C43 N7 N8 -0.9(17) . . . . ? C44 C43 N7 N8 -177.7(13) . . . . ? N9 C42 N8 N7 -1.7(16) . . . . ? C39 C42 N8 N7 179.2(13) . . . . ? C43 N7 N8 C42 1.5(15) . . . . ? N7 C43 N9 C42 -0.2(16) . . . . ? C44 C43 N9 C42 176.7(14) . . . . ? N8 C42 N9 C43 1.3(17) . . . . ? C39 C42 N9 C43 -179.6(13) . . . . ? C45 C46 N10 C47 2(2) . . . . ? C45 C46 N10 Cd1 -176.1(12) . . . 2_677 ? C48 C47 N10 C46 0(2) . . . . ? C48 C47 N10 Cd1 178.2(12) . . . 2_677 ? O2 C1 O1 Cd1 4.1(16) . . . . ? C2 C1 O1 Cd1 -172.5(12) . . . . ? O4 Cd1 O1 C1 -0.6(13) . . . . ? N10 Cd1 O1 C1 177.8(10) 2_677 . . . ? N1 Cd1 O1 C1 89.1(10) . . . . ? O13 Cd1 O1 C1 -93.3(10) . . . . ? O2 Cd1 O1 C1 -2.4(9) . . . . ? O3 Cd1 O1 C1 -142(2) . . . . ? O1 C1 O2 Cd1 -4.2(16) . . . . ? C2 C1 O2 Cd1 172.4(12) . . . . ? O4 Cd1 O2 C1 -176.4(10) . . . . ? N10 Cd1 O2 C1 2.5(13) 2_677 . . . ? N1 Cd1 O2 C1 -88.4(10) . . . . ? O13 Cd1 O2 C1 91.6(10) . . . . ? O1 Cd1 O2 C1 2.3(9) . . . . ? O3 Cd1 O2 C1 173.6(9) . . . . ? O4 C5 O3 Cd1 3.7(16) . . . . ? C6 C5 O3 Cd1 -175.3(13) . . . . ? O4 Cd1 O3 C5 -2.1(9) . . . . ? N10 Cd1 O3 C5 -175.7(10) 2_677 . . . ? N1 Cd1 O3 C5 -87.0(10) . . . . ? O13 Cd1 O3 C5 95.2(10) . . . . ? O2 Cd1 O3 C5 10.3(12) . . . . ? O1 Cd1 O3 C5 144(2) . . . . ? O3 C5 O4 Cd1 -4.1(18) . . . . ? C6 C5 O4 Cd1 174.9(11) . . . . ? N10 Cd1 O4 C5 12.2(13) 2_677 . . . ? N1 Cd1 O4 C5 98.5(10) . . . . ? O13 Cd1 O4 C5 -78.6(10) . . . . ? O2 Cd1 O4 C5 -168.9(10) . . . . ? O1 Cd1 O4 C5 -170.3(9) . . . . ? O3 Cd1 O4 C5 2.1(9) . . . . ? O6 C12 O5 Cd2 3(2) . . . . ? C9 C12 O5 Cd2 -178.5(9) . . . . ? O16 Cd2 O5 C12 -122.4(14) . . . . ? O7 Cd2 O5 C12 99.3(13) . . . . ? O14 Cd2 O5 C12 -2.0(13) . . . . ? O15 Cd2 O5 C12 -20(5) . . . . ? O8 C13 O7 Cd2 -5.5(18) . . . . ? C14 C13 O7 Cd2 172.9(11) . . . . ? O16 Cd2 O7 C13 19.8(17) . . . . ? O5 Cd2 O7 C13 110.2(11) . . . . ? O14 Cd2 O7 C13 -159.6(11) . . . . ? O15 Cd2 O7 C13 -76.5(11) . . . . ? O10 C20 O9 Cd3 0.0(14) . . . . ? C17 C20 O9 Cd3 176.2(10) . . . . ? N5 Cd3 O9 C20 5.4(11) 2_676 . . . ? N6 Cd3 O9 C20 93.6(8) . . . . ? O17 Cd3 O9 C20 -80.5(8) . . . . ? O11 Cd3 O9 C20 -175.2(8) . . . . ? O12 Cd3 O9 C20 -172.7(9) . . . . ? O10 Cd3 O9 C20 0.0(8) . . . . ? O9 C20 O10 Cd3 0.0(14) . . . . ? C17 C20 O10 Cd3 -176.2(11) . . . . ? N5 Cd3 O10 C20 -176.8(9) 2_676 . . . ? N6 Cd3 O10 C20 -86.4(9) . . . . ? O17 Cd3 O10 C20 95.5(9) . . . . ? O9 Cd3 O10 C20 0.0(8) . . . . ? O11 Cd3 O10 C20 152(3) . . . . ? O12 Cd3 O10 C20 9.9(11) . . . . ? O12 C21 O11 Cd3 7(2) . . . . ? C22 C21 O11 Cd3 -174.2(15) . . . . ? N5 Cd3 O11 C21 178.7(12) 2_676 . . . ? N6 Cd3 O11 C21 88.5(12) . . . . ? O17 Cd3 O11 C21 -94.0(12) . . . . ? O9 Cd3 O11 C21 -0.9(14) . . . . ? O12 Cd3 O11 C21 -4.1(11) . . . . ? O10 Cd3 O11 C21 -150(3) . . . . ? O11 C21 O12 Cd3 -7(2) . . . . ? C22 C21 O12 Cd3 174.4(15) . . . . ? N5 Cd3 O12 C21 8.2(14) 2_676 . . . ? N6 Cd3 O12 C21 -85.9(12) . . . . ? O17 Cd3 O12 C21 97.1(12) . . . . ? O9 Cd3 O12 C21 -173.5(12) . . . . ? O11 Cd3 O12 C21 4.1(11) . . . . ? O10 Cd3 O12 C21 178.4(11) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 5.860 _refine_diff_density_min -2.622 _refine_diff_density_rms 0.207 data_2 _database_code_depnum_ccdc_archive 'CCDC 862816' #TrackingRef '2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H16 Cd N5 O6' _chemical_formula_weight 582.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M p-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.985(2) _cell_length_b 10.440(2) _cell_length_c 11.511(2) _cell_angle_alpha 93.48(3) _cell_angle_beta 97.29(3) _cell_angle_gamma 100.15(3) _cell_volume 1167.4(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.658 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 516 _exptl_absorpt_coefficient_mu 0.987 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6783 _exptl_absorpt_correction_T_max 0.7960 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8970 _diffrn_reflns_av_R_equivalents 0.0183 _diffrn_reflns_av_sigmaI/netI 0.0289 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5217 _reflns_number_gt 4898 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0445P)^2^+2.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5217 _refine_ls_number_parameters 337 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0358 _refine_ls_R_factor_gt 0.0318 _refine_ls_wR_factor_ref 0.0923 _refine_ls_wR_factor_gt 0.0904 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _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 0.53695(2) 0.88262(2) 0.369059(18) 0.02161(8) Uani 1 1 d . . . C1 C 0.5424(3) 0.6863(3) 0.2030(3) 0.0260(6) Uani 1 1 d . . . C2 C 0.5216(3) 0.5892(3) 0.0983(3) 0.0264(6) Uani 1 1 d . . . C3 C 0.6290(4) 0.5749(3) 0.0362(3) 0.0336(7) Uani 1 1 d . . . C4 C 0.3921(4) 0.5143(3) 0.0618(3) 0.0324(7) Uani 1 1 d . . . C5 C 0.3102(3) 0.8399(3) 0.5645(3) 0.0262(6) Uani 1 1 d . . . C6 C 0.2407(3) 0.7077(3) 0.5921(3) 0.0262(6) Uani 1 1 d . . . C7 C 0.2200(4) 0.6004(3) 0.5105(3) 0.0300(7) Uani 1 1 d . . . H7A H 0.2441 0.6104 0.4357 0.036 Uiso 1 1 calc R . . C8 C 0.1632(4) 0.4779(3) 0.5408(3) 0.0323(7) Uani 1 1 d . . . H8A H 0.1504 0.4057 0.4863 0.039 Uiso 1 1 calc R . . C9 C 0.1256(4) 0.4625(3) 0.6515(3) 0.0328(7) Uani 1 1 d . . . C10 C 0.1448(5) 0.5701(4) 0.7329(4) 0.0466(10) Uani 1 1 d . . . H10A H 0.1195 0.5603 0.8073 0.056 Uiso 1 1 calc R . . C11 C 0.2018(4) 0.6920(4) 0.7027(3) 0.0419(9) Uani 1 1 d . . . H11A H 0.2142 0.7642 0.7571 0.050 Uiso 1 1 calc R . . C12 C 0.0685(4) 0.3325(4) 0.6896(4) 0.0389(8) Uani 1 1 d . . . C13 C 0.2641(4) 0.8582(4) 0.1888(3) 0.0387(8) Uani 1 1 d . . . H13A H 0.2389 0.7957 0.2401 0.046 Uiso 1 1 calc R . . C14 C 0.1754(4) 0.8619(4) 0.0872(3) 0.0364(8) Uani 1 1 d . . . H14A H 0.0930 0.8024 0.0705 0.044 Uiso 1 1 calc R . . C15 C 0.2109(3) 0.9557(3) 0.0103(3) 0.0272(6) Uani 1 1 d . . . C16 C 0.3335(4) 1.0434(4) 0.0399(3) 0.0352(8) Uani 1 1 d . . . H16A H 0.3595 1.1089 -0.0085 0.042 Uiso 1 1 calc R . . C17 C 0.4172(4) 1.0314(4) 0.1438(3) 0.0349(8) Uani 1 1 d . . . H17A H 0.4999 1.0901 0.1632 0.042 Uiso 1 1 calc R . . C18 C 0.1166(3) 0.9548(3) -0.0982(3) 0.0262(6) Uani 1 1 d . . . C19 C -0.0466(3) 0.9033(3) -0.2359(3) 0.0257(6) Uani 1 1 d . . . C20 C -0.1736(3) 0.8301(3) -0.3044(3) 0.0260(6) Uani 1 1 d . . . C21 C -0.2329(3) 0.8743(3) -0.4072(3) 0.0285(7) Uani 1 1 d . . . H21A H -0.1904 0.9522 -0.4325 0.034 Uiso 1 1 calc R . . C22 C -0.2400(4) 0.7140(4) -0.2681(3) 0.0360(8) Uani 1 1 d . . . H22A H -0.2043 0.6827 -0.1991 0.043 Uiso 1 1 calc R . . C23 C -0.3580(4) 0.6454(4) -0.3338(3) 0.0398(9) Uani 1 1 d . . . H23A H -0.4025 0.5670 -0.3107 0.048 Uiso 1 1 calc R . . C24 C -0.4087(4) 0.6950(3) -0.4342(3) 0.0344(8) Uani 1 1 d . . . H24A H -0.4881 0.6484 -0.4792 0.041 Uiso 1 1 calc R . . N1 N 0.3847(3) 0.9402(3) 0.2167(2) 0.0310(6) Uani 1 1 d . . . N2 N 0.0035(3) 0.8671(3) -0.1305(2) 0.0280(6) Uani 1 1 d . . . N3 N 0.1335(3) 1.0405(3) -0.1799(2) 0.0301(6) Uani 1 1 d . . . N4 N 0.0286(3) 1.0086(3) -0.2700(2) 0.0304(6) Uani 1 1 d . . . N5 N -0.3483(3) 0.8085(3) -0.4703(2) 0.0284(6) Uani 1 1 d . . . O1 O 0.4599(3) 0.6703(2) 0.2770(2) 0.0321(5) Uani 1 1 d . . . O2 O 0.6388(3) 0.7839(2) 0.2125(2) 0.0353(6) Uani 1 1 d . . . O3 O 0.3484(3) 0.8527(2) 0.4660(2) 0.0357(6) Uani 1 1 d . . . O4 O 0.3262(3) 0.9308(2) 0.6451(2) 0.0416(6) Uani 1 1 d . . . O5 O 0.0556(3) 0.2339(2) 0.6084(3) 0.0466(7) Uani 1 1 d . . . O6 O 0.0376(4) 0.3181(3) 0.7863(3) 0.0641(10) Uani 1 1 d . . . H3A H 0.212(6) 1.106(5) -0.178(5) 0.072(16) Uiso 1 1 d . . . H4 H 0.322(4) 0.526(4) 0.103(3) 0.028(9) Uiso 1 1 d . . . H3 H 0.712(4) 0.627(4) 0.055(4) 0.040(11) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.02585(12) 0.01928(11) 0.01695(12) 0.00023(7) -0.00136(8) 0.00028(8) C1 0.0320(16) 0.0214(14) 0.0216(15) -0.0031(11) 0.0009(12) 0.0008(12) C2 0.0338(17) 0.0218(14) 0.0203(14) -0.0036(11) 0.0019(12) -0.0005(12) C3 0.0289(17) 0.0324(17) 0.0326(18) -0.0089(14) 0.0026(14) -0.0073(14) C4 0.0313(17) 0.0319(17) 0.0308(17) -0.0074(14) 0.0069(14) -0.0013(14) C5 0.0209(14) 0.0236(14) 0.0326(17) 0.0057(12) 0.0013(12) 0.0005(11) C6 0.0278(16) 0.0217(14) 0.0292(16) 0.0055(12) 0.0075(13) 0.0010(12) C7 0.0349(17) 0.0257(15) 0.0280(16) 0.0032(13) 0.0065(14) 0.0003(13) C8 0.0355(18) 0.0242(15) 0.0348(18) 0.0014(13) 0.0061(14) -0.0012(13) C9 0.0308(17) 0.0275(16) 0.0384(19) 0.0090(14) 0.0061(14) -0.0019(13) C10 0.068(3) 0.037(2) 0.035(2) 0.0048(16) 0.025(2) -0.0020(19) C11 0.060(3) 0.0289(17) 0.036(2) -0.0009(15) 0.0213(18) -0.0013(17) C12 0.0369(19) 0.0320(18) 0.045(2) 0.0130(16) 0.0038(16) -0.0027(15) C13 0.0311(18) 0.047(2) 0.0351(19) 0.0184(16) -0.0011(15) -0.0008(16) C14 0.0272(17) 0.0417(19) 0.0357(19) 0.0122(15) -0.0018(14) -0.0050(14) C15 0.0241(15) 0.0315(16) 0.0262(16) 0.0045(13) 0.0023(12) 0.0056(13) C16 0.0349(18) 0.0340(18) 0.0325(18) 0.0105(14) 0.0000(15) -0.0041(14) C17 0.0312(17) 0.0382(18) 0.0309(18) 0.0088(14) -0.0029(14) -0.0022(14) C18 0.0254(15) 0.0288(15) 0.0246(15) 0.0070(12) 0.0023(12) 0.0047(12) C19 0.0248(15) 0.0254(15) 0.0253(15) 0.0039(12) -0.0014(12) 0.0036(12) C20 0.0245(15) 0.0246(15) 0.0270(16) 0.0021(12) 0.0003(12) 0.0018(12) C21 0.0297(16) 0.0231(15) 0.0302(17) 0.0062(12) -0.0023(13) 0.0018(12) C22 0.0371(19) 0.0341(18) 0.0334(18) 0.0134(15) -0.0018(15) -0.0015(15) C23 0.040(2) 0.0310(18) 0.043(2) 0.0126(15) -0.0018(16) -0.0073(15) C24 0.0298(17) 0.0301(17) 0.0383(19) 0.0044(14) -0.0052(14) -0.0019(13) N1 0.0285(14) 0.0385(15) 0.0252(14) 0.0077(12) -0.0013(11) 0.0057(12) N2 0.0275(14) 0.0309(14) 0.0243(13) 0.0082(11) -0.0009(11) 0.0036(11) N3 0.0286(14) 0.0300(14) 0.0276(14) 0.0080(11) -0.0029(11) -0.0027(11) N4 0.0294(14) 0.0297(14) 0.0271(14) 0.0062(11) -0.0050(11) -0.0033(11) N5 0.0298(14) 0.0266(13) 0.0258(14) 0.0043(11) -0.0040(11) 0.0023(11) O1 0.0415(13) 0.0256(11) 0.0252(12) -0.0041(9) 0.0086(10) -0.0051(10) O2 0.0368(13) 0.0273(12) 0.0349(13) -0.0106(10) 0.0078(11) -0.0104(10) O3 0.0366(13) 0.0353(13) 0.0384(14) 0.0133(11) 0.0160(11) 0.0044(10) O4 0.0541(16) 0.0246(12) 0.0399(15) -0.0006(10) 0.0081(13) -0.0097(11) O5 0.0632(19) 0.0260(12) 0.0456(16) 0.0097(11) 0.0023(14) -0.0037(12) O6 0.092(3) 0.0424(17) 0.058(2) 0.0145(15) 0.0357(19) -0.0110(16) _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 2.201(3) 2_676 Y Cd1 O3 2.293(2) . Y Cd1 N5 2.297(3) 1_656 Y Cd1 N1 2.351(3) . Y Cd1 O1 2.353(2) . Y Cd1 O2 2.440(2) . Y C1 O1 1.257(4) . ? C1 O2 1.261(4) . ? C1 C2 1.496(4) . ? C2 C3 1.386(5) . ? C2 C4 1.388(5) . ? C3 C4 1.388(5) 2_665 ? C3 H3 0.90(4) . ? C4 C3 1.388(5) 2_665 ? C4 H4 0.92(4) . ? C5 O3 1.249(4) . ? C5 O4 1.260(4) . ? C5 C6 1.503(4) . ? C6 C7 1.386(5) . ? C6 C11 1.389(5) . ? C7 C8 1.388(5) . ? C7 H7A 0.9300 . ? C8 C9 1.385(5) . ? C8 H8A 0.9300 . ? C9 C10 1.389(5) . ? C9 C12 1.491(5) . ? C10 C11 1.382(5) . ? C10 H10A 0.9300 . ? C11 H11A 0.9300 . ? C12 O6 1.204(5) . ? C12 O5 1.324(5) . ? C13 N1 1.338(5) . ? C13 C14 1.381(5) . ? C13 H13A 0.9300 . ? C14 C15 1.390(5) . ? C14 H14A 0.9300 . ? C15 C16 1.383(5) . ? C15 C18 1.464(4) . ? C16 C17 1.396(5) . ? C16 H16A 0.9300 . ? C17 N1 1.331(4) . ? C17 H17A 0.9300 . ? C18 N2 1.320(4) . ? C18 N3 1.343(4) . ? C19 N4 1.327(4) . ? C19 N2 1.354(4) . ? C19 C20 1.465(4) . ? C20 C22 1.390(5) . ? C20 C21 1.396(4) . ? C21 N5 1.333(4) . ? C21 H21A 0.9300 . ? C22 C23 1.373(5) . ? C22 H22A 0.9300 . ? C23 C24 1.370(5) . ? C23 H23A 0.9300 . ? C24 N5 1.346(4) . ? C24 H24A 0.9300 . ? N3 N4 1.357(4) . ? N3 H3A 0.94(6) . ? N5 Cd1 2.297(3) 1_454 ? O4 Cd1 2.201(2) 2_676 ? 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 O3 126.59(10) 2_676 . Y O4 Cd1 N5 101.11(11) 2_676 1_656 Y O3 Cd1 N5 86.50(10) . 1_656 Y O4 Cd1 N1 87.30(11) 2_676 . Y O3 Cd1 N1 84.09(10) . . Y N5 Cd1 N1 169.98(10) 1_656 . Y O4 Cd1 O1 142.85(9) 2_676 . Y O3 Cd1 O1 88.23(9) . . Y N5 Cd1 O1 92.64(10) 1_656 . Y N1 Cd1 O1 83.66(10) . . Y O4 Cd1 O2 88.83(9) 2_676 . Y O3 Cd1 O2 142.35(9) . . Y N5 Cd1 O2 99.94(10) 1_656 . Y N1 Cd1 O2 85.55(10) . . Y O1 Cd1 O2 54.65(8) . . Y O1 C1 O2 122.0(3) . . ? O1 C1 C2 118.7(3) . . ? O2 C1 C2 119.3(3) . . ? C3 C2 C4 119.7(3) . . ? C3 C2 C1 121.0(3) . . ? C4 C2 C1 119.3(3) . . ? C2 C3 C4 120.4(3) . 2_665 ? C2 C3 H3 121(3) . . ? C4 C3 H3 118(3) 2_665 . ? C2 C4 C3 119.9(3) . 2_665 ? C2 C4 H4 118(2) . . ? C3 C4 H4 122(2) 2_665 . ? O3 C5 O4 124.7(3) . . ? O3 C5 C6 119.1(3) . . ? O4 C5 C6 116.3(3) . . ? C7 C6 C11 119.6(3) . . ? C7 C6 C5 121.0(3) . . ? C11 C6 C5 119.4(3) . . ? C6 C7 C8 119.8(3) . . ? C6 C7 H7A 120.1 . . ? C8 C7 H7A 120.1 . . ? C9 C8 C7 120.4(3) . . ? C9 C8 H8A 119.8 . . ? C7 C8 H8A 119.8 . . ? C8 C9 C10 119.9(3) . . ? C8 C9 C12 122.4(3) . . ? C10 C9 C12 117.7(3) . . ? C11 C10 C9 119.7(3) . . ? C11 C10 H10A 120.2 . . ? C9 C10 H10A 120.2 . . ? C10 C11 C6 120.7(3) . . ? C10 C11 H11A 119.7 . . ? C6 C11 H11A 119.7 . . ? O6 C12 O5 122.7(3) . . ? O6 C12 C9 122.8(4) . . ? O5 C12 C9 114.4(3) . . ? N1 C13 C14 123.1(3) . . ? N1 C13 H13A 118.5 . . ? C14 C13 H13A 118.5 . . ? C13 C14 C15 119.1(3) . . ? C13 C14 H14A 120.4 . . ? C15 C14 H14A 120.4 . . ? C16 C15 C14 118.3(3) . . ? C16 C15 C18 123.8(3) . . ? C14 C15 C18 117.9(3) . . ? C15 C16 C17 118.6(3) . . ? C15 C16 H16A 120.7 . . ? C17 C16 H16A 120.7 . . ? N1 C17 C16 123.3(3) . . ? N1 C17 H17A 118.4 . . ? C16 C17 H17A 118.4 . . ? N2 C18 N3 110.3(3) . . ? N2 C18 C15 124.3(3) . . ? N3 C18 C15 125.4(3) . . ? N4 C19 N2 114.4(3) . . ? N4 C19 C20 124.1(3) . . ? N2 C19 C20 121.5(3) . . ? C22 C20 C21 117.7(3) . . ? C22 C20 C19 120.7(3) . . ? C21 C20 C19 121.6(3) . . ? N5 C21 C20 122.2(3) . . ? N5 C21 H21A 118.9 . . ? C20 C21 H21A 118.9 . . ? C23 C22 C20 120.2(3) . . ? C23 C22 H22A 119.9 . . ? C20 C22 H22A 119.9 . . ? C24 C23 C22 118.4(3) . . ? C24 C23 H23A 120.8 . . ? C22 C23 H23A 120.8 . . ? N5 C24 C23 122.8(3) . . ? N5 C24 H24A 118.6 . . ? C23 C24 H24A 118.6 . . ? C17 N1 C13 117.7(3) . . ? C17 N1 Cd1 125.4(2) . . ? C13 N1 Cd1 115.7(2) . . ? C18 N2 C19 103.2(3) . . ? C18 N3 N4 109.6(3) . . ? C18 N3 H3A 124(3) . . ? N4 N3 H3A 126(3) . . ? C19 N4 N3 102.6(3) . . ? C21 N5 C24 118.7(3) . . ? C21 N5 Cd1 124.5(2) . 1_454 ? C24 N5 Cd1 116.7(2) . 1_454 ? C1 O1 Cd1 93.19(18) . . ? C1 O2 Cd1 89.09(19) . . ? C5 O3 Cd1 144.0(2) . . ? C5 O4 Cd1 119.7(2) . 2_676 ? 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 O1 C1 C2 C3 -158.3(3) . . . . ? O2 C1 C2 C3 24.2(5) . . . . ? O1 C1 C2 C4 22.9(5) . . . . ? O2 C1 C2 C4 -154.6(3) . . . . ? C4 C2 C3 C4 -0.4(6) . . . 2_665 ? C1 C2 C3 C4 -179.1(3) . . . 2_665 ? C3 C2 C4 C3 0.4(6) . . . 2_665 ? C1 C2 C4 C3 179.2(3) . . . 2_665 ? O3 C5 C6 C7 0.7(5) . . . . ? O4 C5 C6 C7 -178.9(3) . . . . ? O3 C5 C6 C11 178.0(3) . . . . ? O4 C5 C6 C11 -1.5(5) . . . . ? C11 C6 C7 C8 -1.3(5) . . . . ? C5 C6 C7 C8 176.1(3) . . . . ? C6 C7 C8 C9 0.8(5) . . . . ? C7 C8 C9 C10 -0.1(6) . . . . ? C7 C8 C9 C12 -178.0(3) . . . . ? C8 C9 C10 C11 -0.2(7) . . . . ? C12 C9 C10 C11 177.9(4) . . . . ? C9 C10 C11 C6 -0.4(7) . . . . ? C7 C6 C11 C10 1.1(6) . . . . ? C5 C6 C11 C10 -176.3(4) . . . . ? C8 C9 C12 O6 178.8(4) . . . . ? C10 C9 C12 O6 0.8(6) . . . . ? C8 C9 C12 O5 -0.6(5) . . . . ? C10 C9 C12 O5 -178.6(4) . . . . ? N1 C13 C14 C15 -0.8(6) . . . . ? C13 C14 C15 C16 -1.0(6) . . . . ? C13 C14 C15 C18 178.3(3) . . . . ? C14 C15 C16 C17 1.6(5) . . . . ? C18 C15 C16 C17 -177.7(3) . . . . ? C15 C16 C17 N1 -0.5(6) . . . . ? C16 C15 C18 N2 175.9(3) . . . . ? C14 C15 C18 N2 -3.4(5) . . . . ? C16 C15 C18 N3 -2.7(5) . . . . ? C14 C15 C18 N3 178.0(3) . . . . ? N4 C19 C20 C22 174.0(3) . . . . ? N2 C19 C20 C22 -5.9(5) . . . . ? N4 C19 C20 C21 -6.5(5) . . . . ? N2 C19 C20 C21 173.5(3) . . . . ? C22 C20 C21 N5 -0.6(5) . . . . ? C19 C20 C21 N5 179.9(3) . . . . ? C21 C20 C22 C23 1.3(6) . . . . ? C19 C20 C22 C23 -179.2(4) . . . . ? C20 C22 C23 C24 -0.8(6) . . . . ? C22 C23 C24 N5 -0.6(6) . . . . ? C16 C17 N1 C13 -1.3(6) . . . . ? C16 C17 N1 Cd1 165.6(3) . . . . ? C14 C13 N1 C17 1.9(6) . . . . ? C14 C13 N1 Cd1 -166.2(3) . . . . ? O4 Cd1 N1 C17 17.5(3) 2_676 . . . ? O3 Cd1 N1 C17 144.7(3) . . . . ? N5 Cd1 N1 C17 164.8(5) 1_656 . . . ? O1 Cd1 N1 C17 -126.4(3) . . . . ? O2 Cd1 N1 C17 -71.5(3) . . . . ? O4 Cd1 N1 C13 -175.4(3) 2_676 . . . ? O3 Cd1 N1 C13 -48.2(3) . . . . ? N5 Cd1 N1 C13 -28.1(7) 1_656 . . . ? O1 Cd1 N1 C13 40.7(3) . . . . ? O2 Cd1 N1 C13 95.6(3) . . . . ? N3 C18 N2 C19 0.4(4) . . . . ? C15 C18 N2 C19 -178.4(3) . . . . ? N4 C19 N2 C18 -0.4(4) . . . . ? C20 C19 N2 C18 179.6(3) . . . . ? N2 C18 N3 N4 -0.4(4) . . . . ? C15 C18 N3 N4 178.4(3) . . . . ? N2 C19 N4 N3 0.1(4) . . . . ? C20 C19 N4 N3 -179.8(3) . . . . ? C18 N3 N4 C19 0.1(4) . . . . ? C20 C21 N5 C24 -0.7(5) . . . . ? C20 C21 N5 Cd1 174.3(2) . . . 1_454 ? C23 C24 N5 C21 1.3(6) . . . . ? C23 C24 N5 Cd1 -174.1(3) . . . 1_454 ? O2 C1 O1 Cd1 10.9(4) . . . . ? C2 C1 O1 Cd1 -166.5(3) . . . . ? O4 Cd1 O1 C1 6.2(3) 2_676 . . . ? O3 Cd1 O1 C1 167.4(2) . . . . ? N5 Cd1 O1 C1 -106.2(2) 1_656 . . . ? N1 Cd1 O1 C1 83.2(2) . . . . ? O2 Cd1 O1 C1 -5.85(19) . . . . ? O1 C1 O2 Cd1 -10.5(3) . . . . ? C2 C1 O2 Cd1 166.9(3) . . . . ? O4 Cd1 O2 C1 -166.9(2) 2_676 . . . ? O3 Cd1 O2 C1 -5.2(3) . . . . ? N5 Cd1 O2 C1 92.0(2) 1_656 . . . ? N1 Cd1 O2 C1 -79.6(2) . . . . ? O1 Cd1 O2 C1 5.82(19) . . . . ? O4 C5 O3 Cd1 72.7(5) . . . . ? C6 C5 O3 Cd1 -106.8(4) . . . . ? O4 Cd1 O3 C5 -81.9(4) 2_676 . . . ? N5 Cd1 O3 C5 19.3(4) 1_656 . . . ? N1 Cd1 O3 C5 -164.1(4) . . . . ? O1 Cd1 O3 C5 112.1(4) . . . . ? O2 Cd1 O3 C5 121.1(4) . . . . ? O3 C5 O4 Cd1 -12.3(5) . . . 2_676 ? C6 C5 O4 Cd1 167.3(2) . . . 2_676 ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.946 _refine_diff_density_min -0.674 _refine_diff_density_rms 0.180 data_3 _database_code_depnum_ccdc_archive 'CCDC 862817' #TrackingRef '3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C80 H70 Cd4 N20 O25' _chemical_formula_weight 2161.20 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 p21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.495(3) _cell_length_b 16.313(3) _cell_length_c 19.838(4) _cell_angle_alpha 90.00 _cell_angle_beta 107.07(3) _cell_angle_gamma 90.00 _cell_volume 4484.1(16) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.601 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3780 _exptl_absorpt_coefficient_mu 1.021 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6867 _exptl_absorpt_correction_T_max 0.7245 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27604 _diffrn_reflns_av_R_equivalents 0.0596 _diffrn_reflns_av_sigmaI/netI 0.0566 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7875 _reflns_number_gt 6394 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0599P)^2^+21.4902P] 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 7875 _refine_ls_number_parameters 595 _refine_ls_number_restraints 38 _refine_ls_R_factor_all 0.0899 _refine_ls_R_factor_gt 0.0671 _refine_ls_wR_factor_ref 0.1631 _refine_ls_wR_factor_gt 0.1539 _refine_ls_goodness_of_fit_ref 1.181 _refine_ls_restrained_S_all 1.188 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.39563(4) 0.27384(3) 0.18976(3) 0.02829(17) Uani 1 1 d . . . Cd2 Cd 0.11605(4) 0.25444(3) 0.10389(3) 0.02638(16) Uani 1 1 d . . . C1 C 0.3153(6) 0.3078(5) 0.0477(4) 0.0329(18) Uani 1 1 d . . . C2 C 0.2840(5) 0.3078(5) -0.0304(4) 0.0301(17) Uani 1 1 d . . . C3 C 0.3506(6) 0.2949(5) -0.0672(4) 0.041(2) Uani 1 1 d . . . H3 H 0.4158 0.2900 -0.0429 0.050 Uiso 1 1 calc R . . C4 C 0.3202(6) 0.2893(5) -0.1396(4) 0.041(2) Uani 1 1 d . . . H4 H 0.3653 0.2807 -0.1639 0.049 Uiso 1 1 calc R . . C5 C 0.2244(5) 0.2963(4) -0.1766(3) 0.0283(16) Uani 1 1 d . . . C6 C 0.1918(6) 0.2859(4) -0.2547(4) 0.0288(17) Uani 1 1 d . . . C7 C 0.1575(6) 0.3107(6) -0.1407(4) 0.046(2) Uani 1 1 d . . . H7 H 0.0926 0.3166 -0.1654 0.055 Uiso 1 1 calc R . . C8 C 0.1871(6) 0.3163(6) -0.0681(4) 0.044(2) Uani 1 1 d . . . H8 H 0.1418 0.3257 -0.0442 0.052 Uiso 1 1 calc R . . C9 C -0.0635(5) 0.2595(4) 0.0062(4) 0.0279(16) Uani 1 1 d . . . C10 C -0.1581(5) 0.2580(4) -0.0514(4) 0.0259(16) Uani 1 1 d . . . C11 C -0.1581(6) 0.2480(4) -0.1206(4) 0.0312(17) Uani 1 1 d . . . H11 H -0.1003 0.2470 -0.1319 0.037 Uiso 1 1 calc R . . C12 C -0.2451(6) 0.2394(5) -0.1728(4) 0.0337(18) Uani 1 1 d . . . H12 H -0.2454 0.2296 -0.2190 0.040 Uiso 1 1 calc R . . C13 C -0.3323(5) 0.2452(4) -0.1569(4) 0.0278(16) Uani 1 1 d . . . C14 C -0.4266(6) 0.2378(5) -0.2136(4) 0.0324(18) Uani 1 1 d . . . C15 C -0.3310(6) 0.2563(5) -0.0879(4) 0.0333(18) Uani 1 1 d . . . H15 H -0.3888 0.2604 -0.0768 0.040 Uiso 1 1 calc R . . C16 C -0.2448(6) 0.2613(5) -0.0351(4) 0.0368(19) Uani 1 1 d . . . H16 H -0.2447 0.2669 0.0115 0.044 Uiso 1 1 calc R . . C17 C 0.4019(6) 0.0819(5) 0.2074(4) 0.040(2) Uani 1 1 d . . . H17 H 0.4058 0.1007 0.2524 0.048 Uiso 1 1 calc R . . C18 C 0.3988(7) -0.0022(5) 0.1953(5) 0.048(2) Uani 1 1 d . . . H18 H 0.4025 -0.0389 0.2319 0.058 Uiso 1 1 calc R . . C19 C 0.3903(7) -0.0297(5) 0.1295(4) 0.046(2) Uani 1 1 d . . . H19 H 0.3868 -0.0857 0.1205 0.055 Uiso 1 1 calc R . . C20 C 0.3867(5) 0.0248(5) 0.0756(4) 0.0316(17) Uani 1 1 d . . . C21 C 0.3921(6) 0.1081(5) 0.0922(4) 0.0363(19) Uani 1 1 d . . . H21 H 0.3904 0.1459 0.0567 0.044 Uiso 1 1 calc R . . C22 C 0.3761(5) -0.0043(5) 0.0036(4) 0.0316(17) Uani 1 1 d . . . C23 C 0.3631(6) -0.0131(5) -0.1039(4) 0.0328(18) Uani 1 1 d . . . C24 C 0.3592(6) 0.0034(4) -0.1773(4) 0.0319(17) Uani 1 1 d . . . C25 C 0.3415(7) -0.0592(5) -0.2274(4) 0.048(2) Uani 1 1 d . . . H25 H 0.3313 -0.1126 -0.2147 0.058 Uiso 1 1 calc R . . C26 C 0.3393(8) -0.0417(6) -0.2949(5) 0.056(3) Uani 1 1 d . . . H26 H 0.3283 -0.0831 -0.3286 0.067 Uiso 1 1 calc R . . C27 C 0.3532(7) 0.0367(5) -0.3126(4) 0.046(2) Uani 1 1 d . . . H27 H 0.3512 0.0479 -0.3590 0.055 Uiso 1 1 calc R . . C28 C 0.0902(7) 0.4476(5) 0.0894(4) 0.045(2) Uani 1 1 d . . . H28 H 0.0881 0.4325 0.0438 0.054 Uiso 1 1 calc R . . C29 C 0.0807(8) 0.5296(5) 0.1037(5) 0.056(3) Uani 1 1 d . . . H29 H 0.0727 0.5689 0.0685 0.067 Uiso 1 1 calc R . . C30 C 0.0833(7) 0.5522(5) 0.1719(4) 0.050(2) Uani 1 1 d . . . H30 H 0.0760 0.6068 0.1829 0.059 Uiso 1 1 calc R . . C31 C 0.0970(6) 0.4922(5) 0.2233(4) 0.0344(18) Uani 1 1 d . . . C32 C 0.1071(6) 0.4119(5) 0.2047(4) 0.0361(19) Uani 1 1 d . . . H32 H 0.1178 0.3717 0.2394 0.043 Uiso 1 1 calc R . . C33 C 0.1035(6) 0.5141(5) 0.2971(4) 0.0332(18) Uani 1 1 d . . . C34 C 0.1152(5) 0.5073(4) 0.4037(4) 0.0308(17) Uani 1 1 d . . . C35 C 0.1239(5) 0.4837(4) 0.4765(4) 0.0319(17) Uani 1 1 d . . . C36 C 0.1225(6) 0.4024(5) 0.4967(4) 0.0360(19) Uani 1 1 d . . . H36 H 0.1178 0.3619 0.4628 0.043 Uiso 1 1 calc R . . C37 C 0.1344(7) 0.5424(5) 0.5292(4) 0.045(2) Uani 1 1 d . . . H37 H 0.1379 0.5977 0.5186 0.054 Uiso 1 1 calc R . . C38 C 0.1395(7) 0.5193(5) 0.5955(4) 0.046(2) Uani 1 1 d . . . H38 H 0.1444 0.5583 0.6306 0.055 Uiso 1 1 calc R . . C39 C 0.1373(6) 0.4374(5) 0.6103(4) 0.040(2) Uani 1 1 d . . . H39 H 0.1429 0.4220 0.6564 0.048 Uiso 1 1 calc R . . C40 C 0.3724(6) 0.0806(5) -0.2004(4) 0.0333(18) Uani 1 1 d . . . H40 H 0.3841 0.1234 -0.1680 0.040 Uiso 1 1 calc R . . N1 N 0.3995(5) 0.1363(4) 0.1572(3) 0.0362(16) Uani 1 1 d . . . N2 N 0.3638(6) -0.0835(4) -0.0093(3) 0.0448(18) Uani 1 1 d . . . N3 N 0.3560(6) -0.0874(4) -0.0792(3) 0.0452(19) Uani 1 1 d . . . N4 N 0.3765(5) 0.0424(4) -0.0524(3) 0.0342(15) Uani 1 1 d . . . N5 N 0.3694(5) 0.0976(4) -0.2672(3) 0.0339(15) Uani 1 1 d . . . N6 N 0.1023(5) 0.3893(4) 0.1383(3) 0.0353(15) Uani 1 1 d . . . N7 N 0.1126(5) 0.4599(4) 0.3499(3) 0.0373(16) Uani 1 1 d . . . N8 N 0.1090(5) 0.5861(4) 0.3834(3) 0.0411(17) Uani 1 1 d . . . N9 N 0.1024(6) 0.5916(4) 0.3147(3) 0.0421(18) Uani 1 1 d . . . N10 N 0.1277(5) 0.3793(4) 0.5625(3) 0.0353(15) Uani 1 1 d . . . O1 O 0.2526(4) 0.3029(4) 0.0804(3) 0.0439(14) Uani 1 1 d . . . O2 O 0.4028(4) 0.3123(4) 0.0800(3) 0.0427(14) Uani 1 1 d . . . O3 O 0.2523(4) 0.2719(4) -0.2876(3) 0.0398(14) Uani 1 1 d . . . O4 O 0.1031(4) 0.2886(3) -0.2871(3) 0.0385(13) Uani 1 1 d . . . O5 O 0.0095(4) 0.2870(3) -0.0077(3) 0.0367(13) Uani 1 1 d . . . O6 O -0.0597(4) 0.2317(3) 0.0657(3) 0.0371(13) Uani 1 1 d . . . O7 O -0.4286(4) 0.2134(4) -0.2733(3) 0.0493(16) Uani 1 1 d . . . O8 O -0.5021(4) 0.2559(4) -0.1982(3) 0.0458(15) Uani 1 1 d . . . O9 O 0.5934(14) 0.464(4) 0.978(4) 0.46(4) Uani 0.50 1 d PDU . . O10 O 0.9088(12) 0.2321(10) 0.7219(9) 0.198(6) Uani 1 1 d U . . O11 O 0.3248(8) 0.7545(5) 0.8671(5) 0.099(3) Uani 1 1 d U . . H8A H 0.1021 0.6314 0.4062 0.149 Uiso 1 1 d R . . H3A H 0.3569 -0.1309 -0.0952 0.149 Uiso 1 1 d R . . H10A H 0.9632 0.2468 0.7185 0.218 Uiso 1 1 d R . . H11A H 0.3556 0.7419 0.8393 0.218 Uiso 1 1 d R . . H11B H 0.3341 0.8016 0.8833 0.218 Uiso 1 1 d R . . H9A H 0.5333 0.4731 0.9634 0.417 Uiso 1 1 d RD . . H12A H 0.4108 0.5149 0.8987 0.516 Uiso 1 1 d R . . H12B H 0.3234 0.5189 0.8634 0.516 Uiso 1 1 d R . . H10B H 0.8757 0.2126 0.6869 0.218 Uiso 1 1 d R . . H13A H 0.1775 0.5529 0.8074 0.516 Uiso 1 1 d RD . . H14A H 0.5131 0.3458 0.0575 0.317 Uiso 1 1 d R . . O12 O 0.365(3) 0.521(2) 0.8929(19) 0.46(2) Uani 1 1 d U . . O13 O 0.175(6) 0.585(4) 0.841(3) 0.52(5) Uani 0.50 1 d PDU . . O14 O 0.567(2) 0.359(2) 0.0451(17) 0.205(13) 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 0.0284(3) 0.0365(3) 0.0167(3) -0.0025(2) 0.0015(2) 0.0017(2) Cd2 0.0284(3) 0.0315(3) 0.0161(3) -0.0006(2) 0.0018(2) 0.0002(2) C1 0.043(5) 0.030(4) 0.023(4) -0.001(3) 0.007(4) -0.001(3) C2 0.034(5) 0.038(4) 0.017(3) 0.000(3) 0.006(3) 0.001(3) C3 0.035(5) 0.063(6) 0.026(4) -0.001(4) 0.008(4) 0.008(4) C4 0.031(5) 0.070(6) 0.022(4) -0.003(4) 0.010(3) 0.006(4) C5 0.031(4) 0.037(4) 0.015(3) 0.000(3) 0.004(3) 0.001(3) C6 0.036(5) 0.029(4) 0.020(4) -0.002(3) 0.006(3) -0.002(3) C7 0.025(5) 0.087(7) 0.023(4) -0.006(4) 0.003(3) 0.005(4) C8 0.031(5) 0.082(7) 0.020(4) -0.004(4) 0.012(4) 0.006(4) C9 0.028(4) 0.023(4) 0.029(4) 0.003(3) 0.003(3) -0.003(3) C10 0.037(5) 0.019(3) 0.021(4) -0.002(3) 0.007(3) -0.005(3) C11 0.029(4) 0.037(4) 0.027(4) 0.001(3) 0.008(3) 0.000(3) C12 0.035(5) 0.046(5) 0.020(4) 0.001(3) 0.008(3) 0.000(4) C13 0.028(4) 0.025(4) 0.027(4) 0.007(3) 0.003(3) 0.001(3) C14 0.029(5) 0.037(4) 0.026(4) 0.009(3) -0.001(3) -0.006(3) C15 0.023(4) 0.045(5) 0.030(4) 0.002(3) 0.004(3) -0.005(3) C16 0.032(5) 0.053(5) 0.025(4) -0.002(3) 0.007(3) -0.008(4) C17 0.048(6) 0.044(5) 0.023(4) 0.001(3) 0.002(4) 0.004(4) C18 0.057(6) 0.049(5) 0.039(5) 0.011(4) 0.014(4) 0.002(4) C19 0.070(7) 0.035(5) 0.033(5) 0.003(4) 0.017(4) -0.006(4) C20 0.030(5) 0.033(4) 0.029(4) -0.004(3) 0.005(3) 0.002(3) C21 0.041(5) 0.038(5) 0.029(4) 0.006(3) 0.008(4) 0.003(4) C22 0.032(5) 0.037(4) 0.029(4) 0.002(3) 0.014(4) 0.001(3) C23 0.033(5) 0.030(4) 0.037(4) -0.001(3) 0.014(4) -0.001(3) C24 0.041(5) 0.029(4) 0.026(4) -0.002(3) 0.011(4) 0.003(3) C25 0.075(7) 0.032(5) 0.043(5) 0.003(4) 0.028(5) 0.001(4) C26 0.089(8) 0.045(5) 0.036(5) -0.010(4) 0.023(5) -0.005(5) C27 0.069(7) 0.045(5) 0.025(4) 0.003(4) 0.015(4) 0.002(4) C28 0.066(7) 0.041(5) 0.027(4) 0.000(4) 0.011(4) -0.003(4) C29 0.089(8) 0.037(5) 0.038(5) 0.015(4) 0.012(5) 0.005(5) C30 0.081(7) 0.029(4) 0.039(5) -0.001(4) 0.019(5) 0.003(4) C31 0.042(5) 0.033(4) 0.027(4) 0.003(3) 0.009(4) 0.000(4) C32 0.046(5) 0.032(4) 0.028(4) 0.006(3) 0.007(4) 0.005(4) C33 0.037(5) 0.031(4) 0.034(4) 0.002(3) 0.013(4) -0.001(3) C34 0.032(5) 0.029(4) 0.033(4) -0.002(3) 0.011(3) -0.001(3) C35 0.029(4) 0.030(4) 0.038(4) 0.000(3) 0.011(4) 0.000(3) C36 0.043(5) 0.034(4) 0.028(4) -0.005(3) 0.007(4) -0.002(4) C37 0.067(7) 0.030(4) 0.041(5) -0.004(4) 0.019(5) -0.002(4) C38 0.075(7) 0.032(5) 0.031(5) -0.006(3) 0.015(4) -0.003(4) C39 0.044(5) 0.048(5) 0.027(4) 0.001(4) 0.009(4) 0.000(4) C40 0.036(5) 0.031(4) 0.032(4) -0.003(3) 0.009(4) 0.004(3) N1 0.041(4) 0.038(4) 0.026(3) 0.000(3) 0.005(3) 0.004(3) N2 0.079(6) 0.031(4) 0.033(4) -0.002(3) 0.030(4) -0.005(4) N3 0.075(6) 0.035(4) 0.033(4) -0.005(3) 0.028(4) -0.006(4) N4 0.046(4) 0.028(3) 0.028(3) 0.000(3) 0.010(3) 0.000(3) N5 0.041(4) 0.030(3) 0.027(3) 0.002(3) 0.006(3) 0.003(3) N6 0.044(4) 0.030(3) 0.031(4) -0.002(3) 0.009(3) 0.002(3) N7 0.051(5) 0.029(3) 0.031(4) -0.003(3) 0.010(3) 0.001(3) N8 0.061(5) 0.034(4) 0.031(4) -0.002(3) 0.018(3) 0.003(3) N9 0.071(5) 0.026(4) 0.035(4) 0.004(3) 0.024(4) 0.005(3) N10 0.038(4) 0.036(4) 0.030(4) -0.001(3) 0.008(3) -0.004(3) O1 0.047(4) 0.067(4) 0.022(3) -0.005(3) 0.017(3) -0.011(3) O2 0.034(4) 0.069(4) 0.021(3) 0.002(3) 0.002(2) -0.003(3) O3 0.041(3) 0.059(4) 0.021(3) -0.007(2) 0.012(2) 0.005(3) O4 0.033(3) 0.054(4) 0.024(3) -0.005(2) 0.003(2) -0.002(3) O5 0.031(3) 0.048(3) 0.027(3) 0.006(2) 0.004(2) -0.006(3) O6 0.037(3) 0.044(3) 0.023(3) 0.011(2) -0.001(2) -0.007(2) O7 0.033(3) 0.081(5) 0.028(3) -0.011(3) -0.001(3) -0.005(3) O8 0.022(3) 0.077(4) 0.033(3) 0.000(3) -0.001(2) 0.000(3) O9 0.47(4) 0.46(4) 0.46(4) 0.008(10) 0.144(15) -0.005(10) O10 0.197(10) 0.212(10) 0.225(10) 0.020(8) 0.123(8) 0.000(8) O11 0.159(7) 0.070(5) 0.084(5) -0.021(4) 0.060(5) -0.021(5) O12 0.47(2) 0.44(2) 0.47(2) 0.017(10) 0.139(11) -0.017(10) O13 0.51(5) 0.52(5) 0.53(5) 0.012(10) 0.146(17) -0.007(10) O14 0.202(15) 0.213(16) 0.199(15) 0.007(10) 0.058(10) -0.004(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O2 2.298(5) . y Cd1 O8 2.332(6) 4_666 y Cd1 N5 2.337(6) 4_566 y Cd1 N1 2.341(6) . y Cd1 O3 2.371(5) 4_566 y Cd1 O7 2.445(6) 4_666 y Cd1 O1 2.568(6) . y Cd1 C14 2.730(8) 4_666 ? Cd2 O1 2.302(6) . y Cd2 N6 2.329(6) . y Cd2 O4 2.333(5) 4_566 y Cd2 N10 2.354(6) 4_565 y Cd2 O5 2.359(5) . y Cd2 O6 2.463(5) . y Cd2 O3 2.495(5) 4_566 y C1 O2 1.243(9) . ? C1 O1 1.265(9) . ? C1 C2 1.481(9) . ? C2 C3 1.386(11) . ? C2 C8 1.390(11) . ? C3 C4 1.377(10) . ? C3 H3 0.9300 . ? C4 C5 1.372(11) . ? C4 H4 0.9300 . ? C5 C7 1.381(11) . ? C5 C6 1.491(9) . ? C6 O3 1.258(9) . ? C6 O4 1.259(9) . ? C7 C8 1.379(10) . ? C7 H7 0.9300 . ? C8 H8 0.9300 . ? C9 O6 1.251(9) . ? C9 O5 1.252(9) . ? C9 C10 1.505(10) . ? C10 C11 1.381(10) . ? C10 C16 1.387(11) . ? C11 C12 1.384(11) . ? C11 H11 0.9300 . ? C12 C13 1.392(11) . ? C12 H12 0.9300 . ? C13 C15 1.375(10) . ? C13 C14 1.498(10) . ? C14 O7 1.242(9) . ? C14 O8 1.256(10) . ? C14 Cd1 2.730(8) 4_465 ? C15 C16 1.376(11) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 N1 1.326(10) . ? C17 C18 1.391(12) . ? C17 H17 0.9300 . ? C18 C19 1.350(11) . ? C18 H18 0.9300 . ? C19 C20 1.381(11) . ? C19 H19 0.9300 . ? C20 C21 1.395(11) . ? C20 C22 1.468(10) . ? C21 N1 1.343(9) . ? C21 H21 0.9300 . ? C22 N2 1.319(10) . ? C22 N4 1.349(9) . ? C23 N3 1.321(10) . ? C23 N4 1.335(9) . ? C23 C24 1.466(10) . ? C24 C40 1.373(10) . ? C24 C25 1.394(11) . ? C25 C26 1.361(12) . ? C25 H25 0.9300 . ? C26 C27 1.357(12) . ? C26 H26 0.9300 . ? C27 N5 1.314(10) . ? C27 H27 0.9300 . ? C28 N6 1.332(10) . ? C28 C29 1.383(12) . ? C28 H28 0.9300 . ? C29 C30 1.392(12) . ? C29 H29 0.9300 . ? C30 C31 1.384(11) . ? C30 H30 0.9300 . ? C31 C32 1.380(11) . ? C31 C33 1.482(10) . ? C32 N6 1.350(9) . ? C32 H32 0.9300 . ? C33 N9 1.313(10) . ? C33 N7 1.348(9) . ? C34 N7 1.309(9) . ? C34 N8 1.342(10) . ? C34 C35 1.464(10) . ? C35 C36 1.387(11) . ? C35 C37 1.394(11) . ? C36 N10 1.340(9) . ? C36 H36 0.9300 . ? C37 C38 1.350(11) . ? C37 H37 0.9300 . ? C38 C39 1.370(11) . ? C38 H38 0.9300 . ? C39 N10 1.319(10) . ? C39 H39 0.9300 . ? C40 N5 1.343(9) . ? C40 H40 0.9300 . ? N2 N3 1.360(9) . ? N3 H3A 0.7787 . ? N5 Cd1 2.337(6) 4_565 ? N8 N9 1.342(9) . ? N8 H8A 0.8861 . ? N10 Cd2 2.354(6) 4_566 ? O3 Cd1 2.371(5) 4_565 ? O3 Cd2 2.495(5) 4_565 ? O4 Cd2 2.333(5) 4_565 ? O7 Cd1 2.445(6) 4_465 ? O8 Cd1 2.332(5) 4_465 ? O9 H9A 0.8479 . ? O10 H10B 0.7864 . ? O10 H10A 0.8461 . ? O10 H10B 0.7864 . ? O11 H11A 0.8301 . ? O11 H11B 0.8298 . ? O12 H12A 0.6510 . ? O12 H12B 0.7048 . ? O13 H13A 0.8557 . ? O13 H13A 0.8557 . ? O14 H14A 0.9159 . ? 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 O8 140.1(2) . 4_666 y O2 Cd1 N5 99.1(2) . 4_566 y O8 Cd1 N5 88.0(2) 4_666 4_566 y O2 Cd1 N1 89.4(2) . . y O8 Cd1 N1 90.2(2) 4_666 . y N5 Cd1 N1 168.8(2) 4_566 . y O2 Cd1 O3 123.46(19) . 4_566 y O8 Cd1 O3 95.77(19) 4_666 4_566 y N5 Cd1 O3 88.1(2) 4_566 4_566 y N1 Cd1 O3 81.0(2) . 4_566 y O2 Cd1 O7 85.88(19) . 4_666 y O8 Cd1 O7 54.35(19) 4_666 4_666 y N5 Cd1 O7 94.7(2) 4_566 4_666 y N1 Cd1 O7 93.2(2) . 4_666 y O3 Cd1 O7 149.76(18) 4_566 4_666 y O2 Cd1 O1 53.02(18) . . y O8 Cd1 O1 166.80(19) 4_666 . y N5 Cd1 O1 88.0(2) 4_566 . y N1 Cd1 O1 91.3(2) . . y O3 Cd1 O1 71.53(17) 4_566 . y O7 Cd1 O1 138.58(18) 4_666 . y O2 Cd1 C14 112.9(2) . 4_666 ? O8 Cd1 C14 27.3(2) 4_666 4_666 ? N5 Cd1 C14 91.6(2) 4_566 4_666 ? N1 Cd1 C14 91.9(2) . 4_666 ? O3 Cd1 C14 122.9(2) 4_566 4_666 ? O7 Cd1 C14 27.0(2) 4_666 4_666 ? O1 Cd1 C14 165.5(2) . 4_666 ? O1 Cd2 N6 83.5(2) . . y O1 Cd2 O4 126.81(19) . 4_566 y N6 Cd2 O4 88.6(2) . 4_566 y O1 Cd2 N10 95.4(2) . 4_565 y N6 Cd2 N10 176.8(2) . 4_565 y O4 Cd2 N10 94.5(2) 4_566 4_565 y O1 Cd2 O5 95.57(19) . . y N6 Cd2 O5 88.5(2) . . y O4 Cd2 O5 136.83(19) 4_566 . y N10 Cd2 O5 88.6(2) 4_565 . y O1 Cd2 O6 149.54(17) . . y N6 Cd2 O6 93.6(2) . . y O4 Cd2 O6 83.26(18) 4_566 . y N10 Cd2 O6 85.8(2) 4_565 . y O5 Cd2 O6 53.99(17) . . y O1 Cd2 O3 73.99(18) . 4_566 y N6 Cd2 O3 91.4(2) . 4_566 y O4 Cd2 O3 53.64(18) 4_566 4_566 y N10 Cd2 O3 91.3(2) 4_565 4_566 y O5 Cd2 O3 169.50(17) . 4_566 y O6 Cd2 O3 136.47(16) . 4_566 y O2 C1 O1 121.2(7) . . ? O2 C1 C2 119.5(7) . . ? O1 C1 C2 119.3(7) . . ? C3 C2 C8 118.8(7) . . ? C3 C2 C1 120.2(7) . . ? C8 C2 C1 120.9(7) . . ? C4 C3 C2 120.0(8) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C5 C4 C3 121.1(7) . . ? C5 C4 H4 119.5 . . ? C3 C4 H4 119.5 . . ? C4 C5 C7 119.5(7) . . ? C4 C5 C6 120.5(7) . . ? C7 C5 C6 120.0(7) . . ? O3 C6 O4 120.3(6) . . ? O3 C6 C5 120.2(7) . . ? O4 C6 C5 119.4(7) . . ? C5 C7 C8 120.0(8) . . ? C5 C7 H7 120.0 . . ? C8 C7 H7 120.0 . . ? C7 C8 C2 120.7(7) . . ? C7 C8 H8 119.7 . . ? C2 C8 H8 119.7 . . ? O6 C9 O5 122.1(7) . . ? O6 C9 C10 119.2(6) . . ? O5 C9 C10 118.6(6) . . ? C11 C10 C16 120.0(7) . . ? C11 C10 C9 119.3(7) . . ? C16 C10 C9 120.5(6) . . ? C10 C11 C12 119.3(7) . . ? C10 C11 H11 120.4 . . ? C12 C11 H11 120.4 . . ? C11 C12 C13 120.8(7) . . ? C11 C12 H12 119.6 . . ? C13 C12 H12 119.6 . . ? C15 C13 C12 119.0(7) . . ? C15 C13 C14 120.0(7) . . ? C12 C13 C14 120.9(7) . . ? O7 C14 O8 122.0(7) . . ? O7 C14 C13 120.2(7) . . ? O8 C14 C13 117.8(7) . . ? O7 C14 Cd1 63.5(4) . 4_465 ? O8 C14 Cd1 58.4(4) . 4_465 ? C13 C14 Cd1 176.2(6) . 4_465 ? C16 C15 C13 120.6(7) . . ? C16 C15 H15 119.7 . . ? C13 C15 H15 119.7 . . ? C15 C16 C10 120.1(7) . . ? C15 C16 H16 119.9 . . ? C10 C16 H16 119.9 . . ? N1 C17 C18 122.6(7) . . ? N1 C17 H17 118.7 . . ? C18 C17 H17 118.7 . . ? C19 C18 C17 118.9(8) . . ? C19 C18 H18 120.6 . . ? C17 C18 H18 120.6 . . ? C18 C19 C20 120.5(8) . . ? C18 C19 H19 119.8 . . ? C20 C19 H19 119.8 . . ? C19 C20 C21 117.2(7) . . ? C19 C20 C22 120.9(7) . . ? C21 C20 C22 121.9(7) . . ? N1 C21 C20 122.9(7) . . ? N1 C21 H21 118.5 . . ? C20 C21 H21 118.5 . . ? N2 C22 N4 115.2(7) . . ? N2 C22 C20 118.4(7) . . ? N4 C22 C20 126.4(7) . . ? N3 C23 N4 110.4(7) . . ? N3 C23 C24 123.5(7) . . ? N4 C23 C24 126.2(7) . . ? C40 C24 C25 116.7(7) . . ? C40 C24 C23 122.1(7) . . ? C25 C24 C23 121.3(7) . . ? C26 C25 C24 119.6(8) . . ? C26 C25 H25 120.2 . . ? C24 C25 H25 120.2 . . ? C27 C26 C25 119.3(8) . . ? C27 C26 H26 120.4 . . ? C25 C26 H26 120.4 . . ? N5 C27 C26 123.1(8) . . ? N5 C27 H27 118.5 . . ? C26 C27 H27 118.5 . . ? N6 C28 C29 122.8(8) . . ? N6 C28 H28 118.6 . . ? C29 C28 H28 118.6 . . ? C28 C29 C30 118.6(8) . . ? C28 C29 H29 120.7 . . ? C30 C29 H29 120.7 . . ? C31 C30 C29 119.1(8) . . ? C31 C30 H30 120.5 . . ? C29 C30 H30 120.5 . . ? C32 C31 C30 118.5(7) . . ? C32 C31 C33 120.8(7) . . ? C30 C31 C33 120.7(7) . . ? N6 C32 C31 122.8(7) . . ? N6 C32 H32 118.6 . . ? C31 C32 H32 118.6 . . ? N9 C33 N7 115.5(7) . . ? N9 C33 C31 119.5(7) . . ? N7 C33 C31 125.0(7) . . ? N7 C34 N8 109.8(7) . . ? N7 C34 C35 128.4(7) . . ? N8 C34 C35 121.8(7) . . ? C36 C35 C37 116.6(7) . . ? C36 C35 C34 122.2(7) . . ? C37 C35 C34 121.2(7) . . ? N10 C36 C35 123.3(7) . . ? N10 C36 H36 118.3 . . ? C35 C36 H36 118.3 . . ? C38 C37 C35 120.1(8) . . ? C38 C37 H37 119.9 . . ? C35 C37 H37 119.9 . . ? C37 C38 C39 118.9(8) . . ? C37 C38 H38 120.6 . . ? C39 C38 H38 120.6 . . ? N10 C39 C38 123.5(7) . . ? N10 C39 H39 118.2 . . ? C38 C39 H39 118.2 . . ? N5 C40 C24 123.4(7) . . ? N5 C40 H40 118.3 . . ? C24 C40 H40 118.3 . . ? C17 N1 C21 118.0(7) . . ? C17 N1 Cd1 115.6(5) . . ? C21 N1 Cd1 126.2(5) . . ? C22 N2 N3 102.1(6) . . ? C23 N3 N2 110.1(6) . . ? C23 N3 H3A 132.3 . . ? N2 N3 H3A 116.7 . . ? C23 N4 C22 102.3(6) . . ? C27 N5 C40 117.9(7) . . ? C27 N5 Cd1 116.3(5) . 4_565 ? C40 N5 Cd1 125.7(5) . 4_565 ? C28 N6 C32 118.2(7) . . ? C28 N6 Cd2 117.7(5) . . ? C32 N6 Cd2 124.0(5) . . ? C34 N7 C33 102.6(6) . . ? C34 N8 N9 110.2(6) . . ? C34 N8 H8A 130.8 . . ? N9 N8 H8A 118.5 . . ? C33 N9 N8 101.8(6) . . ? C39 N10 C36 117.5(7) . . ? C39 N10 Cd2 114.8(5) . 4_566 ? C36 N10 Cd2 127.7(5) . 4_566 ? C1 O1 Cd2 156.3(5) . . ? C1 O1 Cd1 85.5(5) . . ? Cd2 O1 Cd1 107.1(2) . . ? C1 O2 Cd1 98.6(5) . . ? C6 O3 Cd1 159.8(5) . 4_565 ? C6 O3 Cd2 89.0(4) . 4_565 ? Cd1 O3 Cd2 107.35(19) 4_565 4_565 ? C6 O4 Cd2 96.6(4) . 4_565 ? C9 O5 Cd2 94.3(4) . . ? C9 O6 Cd2 89.5(4) . . ? C14 O7 Cd1 89.4(5) . 4_465 ? C14 O8 Cd1 94.3(5) . 4_465 ? H10B O10 H10A 112.8 . . ? H10B O10 H10B 0.0 . . ? H10A O10 H10B 112.8 . . ? H11A O11 H11B 115.5 . . ? H12A O12 H12B 135.8 . . ? H13A O13 H13A 0.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 C1 C2 C3 14.0(12) . . . . ? O1 C1 C2 C3 -165.7(8) . . . . ? O2 C1 C2 C8 -169.5(8) . . . . ? O1 C1 C2 C8 10.7(12) . . . . ? C8 C2 C3 C4 -1.0(13) . . . . ? C1 C2 C3 C4 175.5(8) . . . . ? C2 C3 C4 C5 -0.1(14) . . . . ? C3 C4 C5 C7 1.2(13) . . . . ? C3 C4 C5 C6 -176.9(8) . . . . ? C4 C5 C6 O3 -1.1(11) . . . . ? C7 C5 C6 O3 -179.1(8) . . . . ? C4 C5 C6 O4 176.5(7) . . . . ? C7 C5 C6 O4 -1.5(11) . . . . ? C4 C5 C7 C8 -1.3(14) . . . . ? C6 C5 C7 C8 176.8(8) . . . . ? C5 C7 C8 C2 0.2(14) . . . . ? C3 C2 C8 C7 0.9(13) . . . . ? C1 C2 C8 C7 -175.6(8) . . . . ? O6 C9 C10 C11 -147.6(7) . . . . ? O5 C9 C10 C11 30.7(10) . . . . ? O6 C9 C10 C16 28.4(10) . . . . ? O5 C9 C10 C16 -153.3(7) . . . . ? C16 C10 C11 C12 -1.5(11) . . . . ? C9 C10 C11 C12 174.4(6) . . . . ? C10 C11 C12 C13 3.5(11) . . . . ? C11 C12 C13 C15 -2.7(11) . . . . ? C11 C12 C13 C14 178.6(7) . . . . ? C15 C13 C14 O7 -167.1(7) . . . . ? C12 C13 C14 O7 11.6(11) . . . . ? C15 C13 C14 O8 11.9(11) . . . . ? C12 C13 C14 O8 -169.4(7) . . . . ? C15 C13 C14 Cd1 3(8) . . . 4_465 ? C12 C13 C14 Cd1 -178(100) . . . 4_465 ? C12 C13 C15 C16 -0.2(11) . . . . ? C14 C13 C15 C16 178.5(7) . . . . ? C13 C15 C16 C10 2.2(12) . . . . ? C11 C10 C16 C15 -1.3(11) . . . . ? C9 C10 C16 C15 -177.2(7) . . . . ? N1 C17 C18 C19 -1.9(14) . . . . ? C17 C18 C19 C20 1.3(14) . . . . ? C18 C19 C20 C21 -0.1(13) . . . . ? C18 C19 C20 C22 -179.1(8) . . . . ? C19 C20 C21 N1 -0.6(12) . . . . ? C22 C20 C21 N1 178.4(7) . . . . ? C19 C20 C22 N2 4.3(12) . . . . ? C21 C20 C22 N2 -174.7(8) . . . . ? C19 C20 C22 N4 -176.5(8) . . . . ? C21 C20 C22 N4 4.6(13) . . . . ? N3 C23 C24 C40 -176.1(8) . . . . ? N4 C23 C24 C40 2.2(13) . . . . ? N3 C23 C24 C25 3.9(13) . . . . ? N4 C23 C24 C25 -177.8(8) . . . . ? C40 C24 C25 C26 0.7(13) . . . . ? C23 C24 C25 C26 -179.3(9) . . . . ? C24 C25 C26 C27 -0.8(15) . . . . ? C25 C26 C27 N5 0.3(16) . . . . ? N6 C28 C29 C30 -0.4(16) . . . . ? C28 C29 C30 C31 1.1(15) . . . . ? C29 C30 C31 C32 -0.3(14) . . . . ? C29 C30 C31 C33 177.9(9) . . . . ? C30 C31 C32 N6 -1.4(13) . . . . ? C33 C31 C32 N6 -179.6(7) . . . . ? C32 C31 C33 N9 173.8(8) . . . . ? C30 C31 C33 N9 -4.3(13) . . . . ? C32 C31 C33 N7 -4.8(13) . . . . ? C30 C31 C33 N7 177.0(8) . . . . ? N7 C34 C35 C36 -5.8(13) . . . . ? N8 C34 C35 C36 174.7(8) . . . . ? N7 C34 C35 C37 174.1(8) . . . . ? N8 C34 C35 C37 -5.4(12) . . . . ? C37 C35 C36 N10 2.1(12) . . . . ? C34 C35 C36 N10 -178.0(7) . . . . ? C36 C35 C37 C38 -2.1(13) . . . . ? C34 C35 C37 C38 178.0(8) . . . . ? C35 C37 C38 C39 2.0(14) . . . . ? C37 C38 C39 N10 -2.0(14) . . . . ? C25 C24 C40 N5 -0.2(12) . . . . ? C23 C24 C40 N5 179.9(7) . . . . ? C18 C17 N1 C21 1.2(13) . . . . ? C18 C17 N1 Cd1 176.2(7) . . . . ? C20 C21 N1 C17 0.1(12) . . . . ? C20 C21 N1 Cd1 -174.3(6) . . . . ? O2 Cd1 N1 C17 176.6(6) . . . . ? O8 Cd1 N1 C17 36.5(6) 4_666 . . . ? N5 Cd1 N1 C17 -44.1(14) 4_566 . . . ? O3 Cd1 N1 C17 -59.3(6) 4_566 . . . ? O7 Cd1 N1 C17 90.8(6) 4_666 . . . ? O1 Cd1 N1 C17 -130.4(6) . . . . ? C14 Cd1 N1 C17 63.7(6) 4_666 . . . ? O2 Cd1 N1 C21 -8.9(7) . . . . ? O8 Cd1 N1 C21 -149.0(7) 4_666 . . . ? N5 Cd1 N1 C21 130.4(11) 4_566 . . . ? O3 Cd1 N1 C21 115.1(7) 4_566 . . . ? O7 Cd1 N1 C21 -94.7(7) 4_666 . . . ? O1 Cd1 N1 C21 44.1(7) . . . . ? C14 Cd1 N1 C21 -121.8(7) 4_666 . . . ? N4 C22 N2 N3 0.1(10) . . . . ? C20 C22 N2 N3 179.4(7) . . . . ? N4 C23 N3 N2 0.5(10) . . . . ? C24 C23 N3 N2 179.0(7) . . . . ? C22 N2 N3 C23 -0.3(9) . . . . ? N3 C23 N4 C22 -0.4(9) . . . . ? C24 C23 N4 C22 -178.8(8) . . . . ? N2 C22 N4 C23 0.1(9) . . . . ? C20 C22 N4 C23 -179.1(7) . . . . ? C26 C27 N5 C40 0.2(14) . . . . ? C26 C27 N5 Cd1 178.2(8) . . . 4_565 ? C24 C40 N5 C27 -0.3(12) . . . . ? C24 C40 N5 Cd1 -178.1(6) . . . 4_565 ? C29 C28 N6 C32 -1.2(14) . . . . ? C29 C28 N6 Cd2 179.7(8) . . . . ? C31 C32 N6 C28 2.2(12) . . . . ? C31 C32 N6 Cd2 -178.8(6) . . . . ? O1 Cd2 N6 C28 62.7(6) . . . . ? O4 Cd2 N6 C28 -170.0(6) 4_566 . . . ? N10 Cd2 N6 C28 -8(4) 4_565 . . . ? O5 Cd2 N6 C28 -33.1(6) . . . . ? O6 Cd2 N6 C28 -86.8(6) . . . . ? O3 Cd2 N6 C28 136.4(6) 4_566 . . . ? O1 Cd2 N6 C32 -116.3(6) . . . . ? O4 Cd2 N6 C32 11.0(6) 4_566 . . . ? N10 Cd2 N6 C32 173(4) 4_565 . . . ? O5 Cd2 N6 C32 147.9(6) . . . . ? O6 Cd2 N6 C32 94.1(6) . . . . ? O3 Cd2 N6 C32 -42.6(6) 4_566 . . . ? N8 C34 N7 C33 -0.8(9) . . . . ? C35 C34 N7 C33 179.7(8) . . . . ? N9 C33 N7 C34 1.5(10) . . . . ? C31 C33 N7 C34 -179.8(8) . . . . ? N7 C34 N8 N9 -0.1(10) . . . . ? C35 C34 N8 N9 179.5(7) . . . . ? N7 C33 N9 N8 -1.5(10) . . . . ? C31 C33 N9 N8 179.7(7) . . . . ? C34 N8 N9 C33 0.9(9) . . . . ? C38 C39 N10 C36 1.9(13) . . . . ? C38 C39 N10 Cd2 -176.0(7) . . . 4_566 ? C35 C36 N10 C39 -2.0(12) . . . . ? C35 C36 N10 Cd2 175.6(6) . . . 4_566 ? O2 C1 O1 Cd2 -136.3(11) . . . . ? C2 C1 O1 Cd2 43.4(17) . . . . ? O2 C1 O1 Cd1 -12.7(7) . . . . ? C2 C1 O1 Cd1 167.0(6) . . . . ? N6 Cd2 O1 C1 -145.7(14) . . . . ? O4 Cd2 O1 C1 131.0(13) 4_566 . . . ? N10 Cd2 O1 C1 31.3(14) 4_565 . . . ? O5 Cd2 O1 C1 -57.8(14) . . . . ? O6 Cd2 O1 C1 -59.6(15) . . . . ? O3 Cd2 O1 C1 121.0(14) 4_566 . . . ? N6 Cd2 O1 Cd1 94.7(2) . . . . ? O4 Cd2 O1 Cd1 11.3(3) 4_566 . . . ? N10 Cd2 O1 Cd1 -88.4(2) 4_565 . . . ? O5 Cd2 O1 Cd1 -177.5(2) . . . . ? O6 Cd2 O1 Cd1 -179.2(3) . . . . ? O3 Cd2 O1 Cd1 1.37(19) 4_566 . . . ? O2 Cd1 O1 C1 7.3(4) . . . . ? O8 Cd1 O1 C1 -177.3(8) 4_666 . . . ? N5 Cd1 O1 C1 110.3(5) 4_566 . . . ? N1 Cd1 O1 C1 -80.9(5) . . . . ? O3 Cd1 O1 C1 -161.0(5) 4_566 . . . ? O7 Cd1 O1 C1 15.5(6) 4_666 . . . ? C14 Cd1 O1 C1 21.8(10) 4_666 . . . ? O2 Cd1 O1 Cd2 166.8(3) . . . . ? O8 Cd1 O1 Cd2 -17.8(10) 4_666 . . . ? N5 Cd1 O1 Cd2 -90.2(3) 4_566 . . . ? N1 Cd1 O1 Cd2 78.6(3) . . . . ? O3 Cd1 O1 Cd2 -1.5(2) 4_566 . . . ? O7 Cd1 O1 Cd2 175.1(2) 4_666 . . . ? C14 Cd1 O1 Cd2 -178.7(7) 4_666 . . . ? O1 C1 O2 Cd1 14.4(8) . . . . ? C2 C1 O2 Cd1 -165.3(6) . . . . ? O8 Cd1 O2 C1 174.1(4) 4_666 . . . ? N5 Cd1 O2 C1 -88.0(5) 4_566 . . . ? N1 Cd1 O2 C1 84.6(5) . . . . ? O3 Cd1 O2 C1 5.8(6) 4_566 . . . ? O7 Cd1 O2 C1 177.9(5) 4_666 . . . ? O1 Cd1 O2 C1 -7.5(4) . . . . ? C14 Cd1 O2 C1 176.4(5) 4_666 . . . ? O4 C6 O3 Cd1 -151.1(11) . . . 4_565 ? C5 C6 O3 Cd1 26.4(19) . . . 4_565 ? O4 C6 O3 Cd2 -6.4(7) . . . 4_565 ? C5 C6 O3 Cd2 171.2(6) . . . 4_565 ? O3 C6 O4 Cd2 6.9(8) . . . 4_565 ? C5 C6 O4 Cd2 -170.7(6) . . . 4_565 ? O6 C9 O5 Cd2 3.1(8) . . . . ? C10 C9 O5 Cd2 -175.2(5) . . . . ? O1 Cd2 O5 C9 179.4(4) . . . . ? N6 Cd2 O5 C9 -97.2(5) . . . . ? O4 Cd2 O5 C9 -10.9(6) 4_566 . . . ? N10 Cd2 O5 C9 84.2(4) 4_565 . . . ? O6 Cd2 O5 C9 -1.7(4) . . . . ? O3 Cd2 O5 C9 173.5(9) 4_566 . . . ? O5 C9 O6 Cd2 -3.0(7) . . . . ? C10 C9 O6 Cd2 175.3(6) . . . . ? O1 Cd2 O6 C9 3.8(6) . . . . ? N6 Cd2 O6 C9 87.2(4) . . . . ? O4 Cd2 O6 C9 175.3(4) 4_566 . . . ? N10 Cd2 O6 C9 -89.7(4) 4_565 . . . ? O5 Cd2 O6 C9 1.7(4) . . . . ? O3 Cd2 O6 C9 -177.1(4) 4_566 . . . ? O8 C14 O7 Cd1 0.3(8) . . . 4_465 ? C13 C14 O7 Cd1 179.3(6) . . . 4_465 ? O7 C14 O8 Cd1 -0.3(8) . . . 4_465 ? C13 C14 O8 Cd1 -179.3(5) . . . 4_465 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.461 _refine_diff_density_min -0.545 _refine_diff_density_rms 0.125 data_4 _database_code_depnum_ccdc_archive 'CCDC 862818' #TrackingRef '4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H19 Cd N5 O7' _chemical_formula_weight 553.80 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.5869(5) _cell_length_b 9.7706(6) _cell_length_c 13.3468(6) _cell_angle_alpha 75.481(4) _cell_angle_beta 81.145(4) _cell_angle_gamma 63.890(5) _cell_volume 1085.39(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour ? _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.695 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 556 _exptl_absorpt_coefficient_mu 1.059 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6530 _exptl_absorpt_correction_T_max 0.8834 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10961 _diffrn_reflns_av_R_equivalents 0.0330 _diffrn_reflns_av_sigmaI/netI 0.0412 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4257 _reflns_number_gt 3798 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0376P)^2^+0.4912P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4257 _refine_ls_number_parameters 316 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0372 _refine_ls_R_factor_gt 0.0313 _refine_ls_wR_factor_ref 0.0807 _refine_ls_wR_factor_gt 0.0763 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd -0.26790(2) 0.38306(2) 0.270487(17) 0.03219(9) Uani 1 1 d D . . C1 C -0.0169(3) 0.1593(3) 0.1856(3) 0.0364(7) Uani 1 1 d . . . C2 C 0.1177(3) 0.0473(4) 0.1313(3) 0.0390(8) Uani 1 1 d . . . C3 C 0.2281(3) -0.0862(3) 0.1871(2) 0.0298(6) Uani 1 1 d . . . H3 H 0.2166 -0.1080 0.2590 0.036 Uiso 1 1 calc R . . C4 C 0.3551(4) -0.1879(4) 0.1381(2) 0.0381(7) Uani 1 1 d . . . C5 C 0.4785(3) -0.3274(3) 0.1994(3) 0.0363(7) Uani 1 1 d . . . C6 C 0.3686(5) -0.1565(5) 0.0311(3) 0.093(2) Uani 1 1 d . . . H6 H 0.4525 -0.2248 -0.0029 0.232 Uiso 1 1 calc R . . C7 C 0.2581(6) -0.0238(6) -0.0262(3) 0.125(3) Uani 1 1 d . . . H7 H 0.2680 -0.0031 -0.0982 0.399 Uiso 1 1 calc R . . C8 C 0.1325(5) 0.0781(5) 0.0250(3) 0.0867(18) Uani 1 1 d . . . H8 H 0.0584 0.1673 -0.0130 0.217 Uiso 1 1 calc R . . C9 C 0.0082(3) 0.4053(3) 0.3621(2) 0.0340(7) Uani 1 1 d . . . H9 H 0.0073 0.3127 0.4020 0.041 Uiso 1 1 calc R . . C10 C 0.1195(3) 0.4482(3) 0.3793(2) 0.0313(6) Uani 1 1 d . . . C11 C 0.1200(4) 0.5869(4) 0.3203(3) 0.0492(9) Uani 1 1 d . . . H11 H 0.1926 0.6210 0.3299 0.108 Uiso 1 1 calc R . . C12 C 0.0102(5) 0.6726(4) 0.2470(3) 0.0588(11) Uani 1 1 d . . . H12 H 0.0087 0.7655 0.2059 0.129 Uiso 1 1 calc R . . C13 C -0.0968(4) 0.6212(4) 0.2346(3) 0.0471(9) Uani 1 1 d . . . H13 H -0.1702 0.6807 0.1848 0.104 Uiso 1 1 calc R . . C14 C 0.2320(3) 0.3496(3) 0.4599(2) 0.0307(6) Uani 1 1 d . . . C15 C 0.3591(3) 0.1587(3) 0.5758(2) 0.0310(6) Uani 1 1 d . . . C16 C 0.4203(3) 0.0094(3) 0.6488(2) 0.0302(6) Uani 1 1 d . . . C17 C 0.3543(3) -0.0937(3) 0.6590(2) 0.0365(7) Uani 1 1 d . . . H17 H 0.2698 -0.0640 0.6196 0.044 Uiso 1 1 calc R . . C18 C 0.5259(3) -0.2756(4) 0.7791(2) 0.0376(7) Uani 1 1 d . . . H18 H 0.5633 -0.3736 0.8225 0.045 Uiso 1 1 calc R . . C19 C 0.5970(4) -0.1797(4) 0.7756(3) 0.0472(9) Uani 1 1 d . . . H19 H 0.6796 -0.2112 0.8172 0.057 Uiso 1 1 calc R . . C20 C 0.5444(4) -0.0359(4) 0.7095(3) 0.0439(8) Uani 1 1 d . . . H20 H 0.5918 0.0304 0.7057 0.053 Uiso 1 1 calc R . . N1 N -0.0991(3) 0.4888(3) 0.2915(2) 0.0367(6) Uani 1 1 d . . . N2 N 0.2519(3) 0.2021(3) 0.5072(2) 0.0336(6) Uani 1 1 d . . . N3 N 0.3996(3) 0.2760(3) 0.5681(2) 0.0350(6) Uani 1 1 d . . . H3A H 0.4672 0.2732 0.6050 0.042 Uiso 1 1 calc R . . N4 N 0.3202(3) 0.3991(3) 0.4946(2) 0.0348(6) Uani 1 1 d . . . N5 N 0.4043(3) -0.2333(3) 0.7221(2) 0.0360(6) Uani 1 1 d . . . O1 O -0.0324(2) 0.1307(3) 0.28238(18) 0.0413(5) Uani 1 1 d . . . O2 O -0.1104(3) 0.2809(3) 0.13090(18) 0.0550(7) Uani 1 1 d . . . O3 O 0.4696(3) -0.3506(2) 0.29591(18) 0.0422(5) Uani 1 1 d . . . O4 O 0.5868(3) -0.4187(3) 0.1498(2) 0.0599(8) Uani 1 1 d . . . O5 O -0.2881(3) 0.3233(2) 0.44988(18) 0.0434(5) Uani 1 1 d D . . O6 O 0.7933(10) 0.5362(8) 0.9616(5) 0.348(7) Uani 1 1 d D . . O7 O 0.8225(4) 0.0263(3) 0.5602(2) 0.0659(8) Uani 1 1 d D . . H5A H -0.242(5) 0.2335(17) 0.4850(18) 0.099 Uiso 1 1 d D . . H5B H -0.302(6) 0.391(2) 0.4842(18) 0.099 Uiso 1 1 d D . . H7A H 0.814(5) -0.046(4) 0.539(4) 0.099 Uiso 1 1 d D . . H7B H 0.895(4) -0.017(5) 0.603(3) 0.099 Uiso 1 1 d D . . H6A H 0.889(2) 0.504(5) 0.939(4) 0.099 Uiso 1 1 d D . . H6B H 0.778(5) 0.616(4) 0.985(4) 0.099 Uiso 1 1 d 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 0.02809(13) 0.02333(13) 0.04001(15) -0.00258(10) -0.00784(9) -0.00633(9) C1 0.0288(15) 0.0288(16) 0.045(2) -0.0076(14) -0.0077(13) -0.0045(13) C2 0.0361(16) 0.0297(16) 0.0369(18) -0.0032(14) -0.0079(13) -0.0008(13) C3 0.0306(14) 0.0265(15) 0.0293(15) -0.0029(12) -0.0084(12) -0.0085(12) C4 0.0367(16) 0.0283(16) 0.0343(17) -0.0028(13) -0.0097(13) 0.0003(13) C5 0.0290(15) 0.0253(15) 0.050(2) -0.0022(14) -0.0132(13) -0.0062(12) C6 0.083(3) 0.076(3) 0.038(2) -0.012(2) -0.007(2) 0.042(3) C7 0.110(4) 0.102(4) 0.036(2) 0.001(2) -0.004(2) 0.061(3) C8 0.075(3) 0.070(3) 0.039(2) 0.001(2) -0.012(2) 0.034(2) C9 0.0310(15) 0.0271(15) 0.0411(18) -0.0011(13) -0.0057(13) -0.0117(12) C10 0.0326(15) 0.0279(15) 0.0333(16) -0.0072(13) 0.0009(12) -0.0130(12) C11 0.053(2) 0.047(2) 0.053(2) 0.0066(17) -0.0126(17) -0.0324(17) C12 0.067(2) 0.047(2) 0.065(3) 0.0183(19) -0.022(2) -0.036(2) C13 0.0485(19) 0.0402(19) 0.051(2) 0.0082(16) -0.0159(16) -0.0219(16) C14 0.0288(14) 0.0296(16) 0.0344(16) -0.0077(13) 0.0005(12) -0.0130(12) C15 0.0293(14) 0.0324(16) 0.0347(16) -0.0103(13) -0.0012(12) -0.0143(12) C16 0.0278(14) 0.0321(16) 0.0325(16) -0.0096(13) -0.0021(12) -0.0124(12) C17 0.0354(15) 0.0336(17) 0.0409(18) -0.0038(14) -0.0130(13) -0.0134(13) C18 0.0367(16) 0.0353(17) 0.0352(17) -0.0044(14) -0.0087(13) -0.0093(14) C19 0.0400(18) 0.052(2) 0.049(2) -0.0032(17) -0.0206(15) -0.0165(16) C20 0.0453(18) 0.045(2) 0.050(2) -0.0049(16) -0.0135(16) -0.0255(16) N1 0.0303(12) 0.0322(14) 0.0432(16) -0.0025(12) -0.0055(11) -0.0108(11) N2 0.0345(13) 0.0325(14) 0.0378(15) -0.0065(11) -0.0066(11) -0.0165(11) N3 0.0331(13) 0.0370(14) 0.0404(15) -0.0092(12) -0.0059(11) -0.0178(11) N4 0.0366(13) 0.0294(13) 0.0402(15) -0.0058(12) -0.0073(11) -0.0147(11) N5 0.0371(13) 0.0302(14) 0.0393(15) -0.0028(12) -0.0097(11) -0.0128(11) O1 0.0339(11) 0.0380(12) 0.0406(13) -0.0069(10) -0.0049(9) -0.0046(10) O2 0.0464(13) 0.0369(13) 0.0469(15) -0.0041(11) -0.0090(11) 0.0133(11) O3 0.0481(13) 0.0330(12) 0.0416(14) 0.0021(10) -0.0229(10) -0.0122(10) O4 0.0432(13) 0.0399(14) 0.0573(16) -0.0014(12) -0.0069(12) 0.0145(11) O5 0.0579(14) 0.0300(12) 0.0420(14) -0.0055(10) -0.0083(11) -0.0174(11) O6 0.397(11) 0.209(7) 0.091(5) 0.027(4) 0.013(6) 0.147(7) O7 0.092(2) 0.0449(16) 0.0592(18) 0.0000(13) -0.0320(15) -0.0241(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 O4 2.245(2) 1_465 y Cd1 O5 2.317(2) . y Cd1 N5 2.331(3) 2_556 y Cd1 O2 2.342(2) . y Cd1 N1 2.350(3) . y Cd1 O1 2.493(2) . y C1 O1 1.251(4) . ? C1 O2 1.256(4) . ? C1 C2 1.502(4) . ? C2 C8 1.374(5) . ? C2 C3 1.384(4) . ? C3 C4 1.383(4) . ? C3 H3 0.9300 . ? C4 C6 1.382(5) . ? C4 C5 1.499(4) . ? C5 O3 1.247(4) . ? C5 O4 1.257(4) . ? C6 C7 1.390(5) . ? C6 H6 0.9300 . ? C7 C8 1.393(5) . ? C7 H7 0.9300 . ? C8 H8 0.9300 . ? C9 N1 1.337(4) . ? C9 C10 1.373(4) . ? C9 H9 0.9300 . ? C10 C11 1.389(4) . ? C10 C14 1.473(4) . ? C11 C12 1.377(5) . ? C11 H11 0.9300 . ? C12 C13 1.371(5) . ? C12 H12 0.9300 . ? C13 N1 1.334(4) . ? C13 H13 0.9300 . ? C14 N4 1.325(4) . ? C14 N2 1.361(4) . ? C15 N2 1.336(4) . ? C15 N3 1.340(4) . ? C15 C16 1.461(4) . ? C16 C17 1.379(4) . ? C16 C20 1.386(4) . ? C17 N5 1.331(4) . ? C17 H17 0.9300 . ? C18 N5 1.341(4) . ? C18 C19 1.369(5) . ? C18 H18 0.9300 . ? C19 C20 1.377(5) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? N3 N4 1.349(3) . ? N3 H3A 0.8600 . ? N5 Cd1 2.331(3) 2_556 ? O4 Cd1 2.245(2) 1_645 ? O5 H5A 0.837(10) . ? O5 H5B 0.848(10) . ? O6 H6A 0.859(10) . ? O6 H6B 0.853(10) . ? O7 H7A 0.859(10) . ? O7 H7B 0.858(10) . ? 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 133.70(8) 1_465 . y O4 Cd1 N5 94.91(10) 1_465 2_556 y O5 Cd1 N5 85.45(9) . 2_556 y O4 Cd1 O2 85.78(8) 1_465 . y O5 Cd1 O2 140.50(8) . . y N5 Cd1 O2 90.41(10) 2_556 . y O4 Cd1 N1 97.63(10) 1_465 . y O5 Cd1 N1 85.61(9) . . y N5 Cd1 N1 167.46(8) 2_556 . y O2 Cd1 N1 90.89(10) . . y O4 Cd1 O1 139.59(8) 1_465 . y O5 Cd1 O1 86.65(8) . . y N5 Cd1 O1 84.86(8) 2_556 . y O2 Cd1 O1 53.85(7) . . y N1 Cd1 O1 85.84(8) . . y O1 C1 O2 122.1(3) . . ? O1 C1 C2 120.0(3) . . ? O2 C1 C2 117.9(3) . . ? C8 C2 C3 119.5(3) . . ? C8 C2 C1 119.7(3) . . ? C3 C2 C1 120.8(3) . . ? C4 C3 C2 121.4(3) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C6 C4 C3 118.8(3) . . ? C6 C4 C5 120.3(3) . . ? C3 C4 C5 121.0(3) . . ? O3 C5 O4 122.6(3) . . ? O3 C5 C4 119.9(3) . . ? O4 C5 C4 117.5(3) . . ? C4 C6 C7 120.6(3) . . ? C4 C6 H6 119.7 . . ? C7 C6 H6 119.7 . . ? C6 C7 C8 119.5(4) . . ? C6 C7 H7 120.2 . . ? C8 C7 H7 120.2 . . ? C2 C8 C7 120.2(3) . . ? C2 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? N1 C9 C10 123.8(3) . . ? N1 C9 H9 118.1 . . ? C10 C9 H9 118.1 . . ? C9 C10 C11 118.0(3) . . ? C9 C10 C14 120.1(3) . . ? C11 C10 C14 121.9(3) . . ? C12 C11 C10 118.2(3) . . ? C12 C11 H11 120.9 . . ? C10 C11 H11 120.9 . . ? C13 C12 C11 120.1(3) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? N1 C13 C12 122.2(3) . . ? N1 C13 H13 118.9 . . ? C12 C13 H13 118.9 . . ? N4 C14 N2 114.0(3) . . ? N4 C14 C10 122.6(3) . . ? N2 C14 C10 123.4(3) . . ? N2 C15 N3 108.8(3) . . ? N2 C15 C16 125.9(3) . . ? N3 C15 C16 125.3(3) . . ? C17 C16 C20 117.3(3) . . ? C17 C16 C15 119.7(3) . . ? C20 C16 C15 123.0(3) . . ? N5 C17 C16 123.8(3) . . ? N5 C17 H17 118.1 . . ? C16 C17 H17 118.1 . . ? N5 C18 C19 122.4(3) . . ? N5 C18 H18 118.8 . . ? C19 C18 H18 118.8 . . ? C18 C19 C20 119.0(3) . . ? C18 C19 H19 120.5 . . ? C20 C19 H19 120.5 . . ? C19 C20 C16 119.6(3) . . ? C19 C20 H20 120.2 . . ? C16 C20 H20 120.2 . . ? C13 N1 C9 117.7(3) . . ? C13 N1 Cd1 125.0(2) . . ? C9 N1 Cd1 117.23(19) . . ? C15 N2 C14 103.6(2) . . ? C15 N3 N4 110.9(2) . . ? C15 N3 H3A 124.5 . . ? N4 N3 H3A 124.5 . . ? C14 N4 N3 102.7(2) . . ? C17 N5 C18 117.9(3) . . ? C17 N5 Cd1 117.27(19) . 2_556 ? C18 N5 Cd1 124.8(2) . 2_556 ? C1 O1 Cd1 88.58(17) . . ? C1 O2 Cd1 95.5(2) . . ? C5 O4 Cd1 105.5(2) . 1_645 ? Cd1 O5 H5A 123.3(19) . . ? Cd1 O5 H5B 120.0(18) . . ? H5A O5 H5B 110(2) . . ? H6A O6 H6B 103(2) . . ? H7A O7 H7B 108(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C8 178.8(4) . . . . ? O2 C1 C2 C8 -1.8(6) . . . . ? O1 C1 C2 C3 -1.7(5) . . . . ? O2 C1 C2 C3 177.7(3) . . . . ? C8 C2 C3 C4 1.4(6) . . . . ? C1 C2 C3 C4 -178.1(3) . . . . ? C2 C3 C4 C6 -1.8(6) . . . . ? C2 C3 C4 C5 176.5(3) . . . . ? C6 C4 C5 O3 176.2(4) . . . . ? C3 C4 C5 O3 -2.1(5) . . . . ? C6 C4 C5 O4 -4.9(6) . . . . ? C3 C4 C5 O4 176.8(3) . . . . ? C3 C4 C6 C7 1.1(8) . . . . ? C5 C4 C6 C7 -177.2(5) . . . . ? C4 C6 C7 C8 -0.2(11) . . . . ? C3 C2 C8 C7 -0.4(8) . . . . ? C1 C2 C8 C7 179.1(5) . . . . ? C6 C7 C8 C2 -0.2(11) . . . . ? N1 C9 C10 C11 0.4(5) . . . . ? N1 C9 C10 C14 179.2(3) . . . . ? C9 C10 C11 C12 -0.8(5) . . . . ? C14 C10 C11 C12 -179.6(3) . . . . ? C10 C11 C12 C13 0.6(6) . . . . ? C11 C12 C13 N1 -0.1(7) . . . . ? C9 C10 C14 N4 -165.8(3) . . . . ? C11 C10 C14 N4 13.0(5) . . . . ? C9 C10 C14 N2 12.4(4) . . . . ? C11 C10 C14 N2 -168.8(3) . . . . ? N2 C15 C16 C17 -7.6(5) . . . . ? N3 C15 C16 C17 171.1(3) . . . . ? N2 C15 C16 C20 172.1(3) . . . . ? N3 C15 C16 C20 -9.1(5) . . . . ? C20 C16 C17 N5 -1.0(5) . . . . ? C15 C16 C17 N5 178.7(3) . . . . ? N5 C18 C19 C20 -1.5(5) . . . . ? C18 C19 C20 C16 0.5(5) . . . . ? C17 C16 C20 C19 0.7(5) . . . . ? C15 C16 C20 C19 -179.1(3) . . . . ? C12 C13 N1 C9 -0.3(5) . . . . ? C12 C13 N1 Cd1 -176.5(3) . . . . ? C10 C9 N1 C13 0.1(5) . . . . ? C10 C9 N1 Cd1 176.6(2) . . . . ? O4 Cd1 N1 C13 -5.7(3) 1_465 . . . ? O5 Cd1 N1 C13 -139.2(3) . . . . ? N5 Cd1 N1 C13 176.1(4) 2_556 . . . ? O2 Cd1 N1 C13 80.1(3) . . . . ? O1 Cd1 N1 C13 133.8(3) . . . . ? O4 Cd1 N1 C9 178.1(2) 1_465 . . . ? O5 Cd1 N1 C9 44.6(2) . . . . ? N5 Cd1 N1 C9 -0.1(5) 2_556 . . . ? O2 Cd1 N1 C9 -96.0(2) . . . . ? O1 Cd1 N1 C9 -42.4(2) . . . . ? N3 C15 N2 C14 -0.3(3) . . . . ? C16 C15 N2 C14 178.7(3) . . . . ? N4 C14 N2 C15 0.3(3) . . . . ? C10 C14 N2 C15 -178.1(3) . . . . ? N2 C15 N3 N4 0.1(3) . . . . ? C16 C15 N3 N4 -178.8(3) . . . . ? N2 C14 N4 N3 -0.2(3) . . . . ? C10 C14 N4 N3 178.1(3) . . . . ? C15 N3 N4 C14 0.1(3) . . . . ? C16 C17 N5 C18 0.1(5) . . . . ? C16 C17 N5 Cd1 178.1(2) . . . 2_556 ? C19 C18 N5 C17 1.2(5) . . . . ? C19 C18 N5 Cd1 -176.6(2) . . . 2_556 ? O2 C1 O1 Cd1 -0.8(3) . . . . ? C2 C1 O1 Cd1 178.6(3) . . . . ? O4 Cd1 O1 C1 3.2(3) 1_465 . . . ? O5 Cd1 O1 C1 -179.5(2) . . . . ? N5 Cd1 O1 C1 94.7(2) 2_556 . . . ? O2 Cd1 O1 C1 0.45(19) . . . . ? N1 Cd1 O1 C1 -93.7(2) . . . . ? O1 C1 O2 Cd1 0.8(4) . . . . ? C2 C1 O2 Cd1 -178.6(3) . . . . ? O4 Cd1 O2 C1 -178.7(2) 1_465 . . . ? O5 Cd1 O2 C1 -0.4(3) . . . . ? N5 Cd1 O2 C1 -83.8(2) 2_556 . . . ? N1 Cd1 O2 C1 83.7(2) . . . . ? O1 Cd1 O2 C1 -0.45(19) . . . . ? O3 C5 O4 Cd1 3.1(4) . . . 1_645 ? C4 C5 O4 Cd1 -175.8(2) . . . 1_645 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.755 _refine_diff_density_min -0.449 _refine_diff_density_rms 0.076 data_5 _database_code_depnum_ccdc_archive 'CCDC 862819' #TrackingRef '5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H32 Cd N10 O9' _chemical_formula_weight 813.09 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 p21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.931(3) _cell_length_b 9.908(2) _cell_length_c 21.471(4) _cell_angle_alpha 90.00 _cell_angle_beta 108.61(3) _cell_angle_gamma 90.00 _cell_volume 3413.5(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.582 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2870 _exptl_absorpt_coefficient_mu 0.710 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.894 _exptl_absorpt_correction_T_max 0.912 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17824 _diffrn_reflns_av_R_equivalents 0.0692 _diffrn_reflns_av_sigmaI/netI 0.0744 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.17 _diffrn_reflns_theta_max 25.25 _reflns_number_total 6148 _reflns_number_gt 4480 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0591P)^2^+15.0000P] 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 6148 _refine_ls_number_parameters 469 _refine_ls_number_restraints 95 _refine_ls_R_factor_all 0.1039 _refine_ls_R_factor_gt 0.0685 _refine_ls_wR_factor_ref 0.1594 _refine_ls_wR_factor_gt 0.1417 _refine_ls_goodness_of_fit_ref 0.984 _refine_ls_restrained_S_all 0.991 _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 0.86538(3) -0.17793(5) 0.81421(2) 0.03712(17) Uani 1 1 d . . . C1 C 0.7565(4) -0.0372(6) 0.8615(3) 0.0383(15) Uani 1 1 d . . . C2 C 0.6882(4) 0.0076(6) 0.8878(3) 0.0366(15) Uani 1 1 d . . . C3 C 0.6832(5) -0.0507(8) 0.9453(3) 0.055(2) Uani 1 1 d . . . H3A H 0.7255 -0.1075 0.9697 0.120 Uiso 1 1 calc R . . C4 C 0.6154(5) -0.0245(9) 0.9666(4) 0.063(2) Uani 1 1 d . . . H4A H 0.6126 -0.0640 1.0051 0.140 Uiso 1 1 calc R . . C5 C 0.5522(5) 0.0596(9) 0.9310(4) 0.060(2) Uani 1 1 d . . . H5 H 0.5070 0.0772 0.9455 0.131 Uiso 1 1 calc R . . C6 C 0.5568(4) 0.1178(8) 0.8734(3) 0.0468(17) Uani 1 1 d . . . H6 H 0.5140 0.1738 0.8491 0.056 Uiso 1 1 calc R . . C7 C 0.6245(4) 0.0938(6) 0.8516(3) 0.0372(15) Uani 1 1 d . . . C8 C 0.6283(4) 0.1660(6) 0.7914(3) 0.0342(14) Uani 1 1 d . . . C9 C 0.8859(4) 0.0500(7) 0.7117(3) 0.0409(16) Uani 1 1 d . . . H9 H 0.8576 -0.0144 0.6812 0.049 Uiso 1 1 calc R . . C10 C 0.9037(4) 0.1712(7) 0.6892(3) 0.0463(17) Uani 1 1 d . . . H10A H 0.8878 0.1885 0.6443 0.102 Uiso 1 1 calc R . . C11 C 0.9456(4) 0.2679(7) 0.7338(3) 0.0422(16) Uani 1 1 d . . . H11A H 0.9586 0.3511 0.7195 0.051 Uiso 1 1 calc R . . C12 C 0.9679(4) 0.2388(6) 0.8001(3) 0.0332(14) Uani 1 1 d . . . C13 C 0.9468(4) 0.1139(6) 0.8184(3) 0.0385(15) Uani 1 1 d . . . H13A H 0.9610 0.0947 0.8630 0.046 Uiso 1 1 calc R . . C14 C 1.0094(4) 0.3374(6) 0.8513(3) 0.0348(14) Uani 1 1 d . . . C15 C 1.0699(4) 0.4313(6) 0.9423(3) 0.0340(14) Uani 1 1 d . . . C16 C 1.1082(4) 0.4535(6) 1.0133(3) 0.0355(15) Uani 1 1 d . . . C17 C 1.1186(4) 0.3476(6) 1.0565(3) 0.0388(16) Uani 1 1 d . . . H17A H 1.1037 0.2617 1.0393 0.047 Uiso 1 1 calc R . . C18 C 1.1325(4) 0.5812(7) 1.0396(3) 0.0431(17) Uani 1 1 d . . . H18A H 1.1270 0.6556 1.0122 0.052 Uiso 1 1 calc R . . C19 C 1.1647(4) 0.5956(7) 1.1065(3) 0.0460(17) Uani 1 1 d . . . H19A H 1.1811 0.6801 1.1249 0.055 Uiso 1 1 calc R . . C20 C 1.1725(4) 0.4840(7) 1.1462(3) 0.0438(17) Uani 1 1 d . . . H20A H 1.1949 0.4948 1.1915 0.053 Uiso 1 1 calc R . . C21 C 0.0656(6) 0.0155(10) 0.6299(5) 0.077(3) Uani 1 1 d U . . H21A H 0.0447 -0.0583 0.6029 0.191 Uiso 1 1 calc R . . C22 C 0.0560(6) 0.1424(10) 0.6021(5) 0.076(3) Uani 1 1 d U . . H22A H 0.0278 0.1536 0.5575 0.191 Uiso 1 1 calc R . . C23 C 0.0888(5) 0.2540(9) 0.6415(4) 0.067(2) Uani 1 1 d U . . H23A H 0.0844 0.3402 0.6236 0.167 Uiso 1 1 calc R . . C24 C 0.1283(5) 0.2325(8) 0.7082(4) 0.0531(19) Uani 1 1 d U . . C25 C 0.1345(5) 0.1016(9) 0.7318(4) 0.067(2) Uani 1 1 d U . . H25A H 0.1616 0.0873 0.7764 0.147 Uiso 1 1 calc R . . C26 C 0.1583(4) 0.3446(8) 0.7533(4) 0.0512(18) Uani 1 1 d . . . C27 C 0.2104(4) 0.4544(8) 0.8416(4) 0.0497(18) Uani 1 1 d U . . C28 C 0.2531(4) 0.4990(8) 0.9091(4) 0.0524(19) Uani 1 1 d U . . C29 C 0.2568(5) 0.6319(9) 0.9277(4) 0.064(2) Uani 1 1 d U . . H29A H 0.2308 0.6978 0.8972 0.141 Uiso 1 1 calc R . . C30 C 0.2994(6) 0.6677(10) 0.9919(4) 0.075(2) Uani 1 1 d U . . H30A H 0.3014 0.7568 1.0059 0.189 Uiso 1 1 calc R . . C31 C 0.3389(6) 0.5661(11) 1.0345(5) 0.082(3) Uani 1 1 d U . . H31A H 0.3695 0.5902 1.0772 0.205 Uiso 1 1 calc R . . C32 C 0.2941(6) 0.4048(9) 0.9566(4) 0.074(2) Uani 1 1 d U . . H32A H 0.2919 0.3145 0.9443 0.184 Uiso 1 1 calc R . . N1 N 0.9075(3) 0.0195(5) 0.7759(2) 0.0402(13) Uani 1 1 d . . . N2 N 1.0465(3) 0.3083(5) 0.9153(2) 0.0355(12) Uani 1 1 d . . . N3 N 1.0129(3) 0.4694(5) 0.8414(2) 0.0362(12) Uani 1 1 d D . . N4 N 1.0502(3) 0.5331(5) 0.9002(2) 0.0373(12) Uani 1 1 d . . . N5 N 1.1490(3) 0.3609(5) 1.1221(2) 0.0397(13) Uani 1 1 d . . . N6 N 0.1035(5) -0.0058(7) 0.6938(4) 0.078(2) Uani 1 1 d . . . N7 N 0.1366(4) 0.4720(6) 0.7367(3) 0.0544(16) Uani 1 1 d . . . N8 N 0.1711(4) 0.5431(6) 0.7928(3) 0.0519(15) Uani 1 1 d D . . N9 N 0.2038(4) 0.3296(6) 0.8181(3) 0.0541(16) Uani 1 1 d . . . N10 N 0.3362(5) 0.4368(9) 1.0186(4) 0.090(3) Uani 1 1 d . . . O1 O 0.7366(3) -0.0783(5) 0.8035(2) 0.0464(12) Uani 1 1 d . . . O2 O 0.8306(3) -0.0419(5) 0.9003(2) 0.0507(12) Uani 1 1 d . . . O3 O 0.6921(3) 0.2291(5) 0.7924(2) 0.0474(12) Uani 1 1 d . . . O4 O 0.5638(3) 0.1671(5) 0.7416(2) 0.0461(11) Uani 1 1 d . . . O5 O 1.0071(3) -0.1816(5) 0.8876(3) 0.0640(15) Uani 1 1 d D . . O6 O 0.0993(5) 0.0234(8) 0.9637(3) 0.116(3) Uani 1 1 d U . . O7 O 0.1552(5) 0.6409(7) 0.6289(3) 0.100(2) Uani 1 1 d U . . O8 O 0.1245(5) 0.8012(7) 0.7914(4) 0.118(3) Uani 1 1 d U . . O9 O 0.2140(9) 0.9487(13) 0.8925(6) 0.319(9) Uani 1 1 d U . . H3 H 0.9951 0.5256 0.8055 0.319 Uiso 1 1 d RD . . H8 H 0.1551 0.6342 0.7979 0.478 Uiso 1 1 d RD . . H9A H 0.1806 0.9704 0.9132 0.383 Uiso 1 1 d R . . H9B H 0.2503 1.0016 0.8863 0.383 Uiso 1 1 d R . . H5A H 1.0198 -0.1442 0.9250 0.383 Uiso 1 1 d RD . . H5B H 1.0448 -0.2256 0.8771 0.383 Uiso 1 1 d RD . . H6B H 0.0844 0.1052 0.9500 0.383 Uiso 1 1 d R . . H6A H 0.1206 0.0306 1.0051 0.383 Uiso 1 1 d R . . H7A H 0.1966 0.6951 0.6445 0.383 Uiso 1 1 d R . . H7B H 0.1506 0.5922 0.6603 0.383 Uiso 1 1 d R . . H8A H 0.1170 0.8608 0.7608 0.383 Uiso 1 1 d R . . H8B H 0.0788 0.7589 0.7892 0.383 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 0.0450(3) 0.0317(3) 0.0304(3) -0.0005(2) 0.0060(2) 0.0009(2) C1 0.046(4) 0.027(3) 0.038(4) 0.003(3) 0.008(3) 0.000(3) C2 0.044(4) 0.035(4) 0.028(3) 0.000(3) 0.009(3) -0.004(3) C3 0.061(5) 0.063(5) 0.038(4) 0.017(4) 0.013(4) 0.006(4) C4 0.073(6) 0.080(6) 0.044(4) 0.013(4) 0.028(4) -0.002(5) C5 0.054(5) 0.080(6) 0.055(5) 0.001(4) 0.032(4) -0.005(4) C6 0.041(4) 0.057(5) 0.042(4) -0.006(3) 0.013(3) -0.002(3) C7 0.043(4) 0.039(4) 0.025(3) -0.003(3) 0.004(3) -0.008(3) C8 0.046(4) 0.022(3) 0.032(3) -0.004(3) 0.008(3) 0.002(3) C9 0.043(4) 0.048(4) 0.027(3) -0.009(3) 0.006(3) -0.002(3) C10 0.059(4) 0.048(4) 0.025(3) 0.003(3) 0.005(3) 0.000(4) C11 0.051(4) 0.037(4) 0.037(4) 0.001(3) 0.011(3) -0.001(3) C12 0.033(3) 0.034(4) 0.029(3) -0.004(3) 0.005(3) 0.000(3) C13 0.051(4) 0.035(4) 0.026(3) 0.001(3) 0.006(3) 0.000(3) C14 0.038(3) 0.031(4) 0.036(3) 0.002(3) 0.012(3) 0.001(3) C15 0.037(4) 0.035(4) 0.032(3) 0.000(3) 0.014(3) -0.002(3) C16 0.035(4) 0.037(4) 0.032(3) 0.003(3) 0.008(3) 0.000(3) C17 0.044(4) 0.037(4) 0.031(3) -0.001(3) 0.005(3) -0.001(3) C18 0.056(4) 0.036(4) 0.033(4) 0.001(3) 0.009(3) -0.011(3) C19 0.053(4) 0.039(4) 0.045(4) -0.001(3) 0.015(4) -0.010(3) C20 0.043(4) 0.048(4) 0.036(4) -0.010(3) 0.007(3) -0.002(3) C21 0.077(4) 0.075(4) 0.081(4) -0.013(4) 0.029(4) -0.003(4) C22 0.078(4) 0.080(5) 0.072(4) -0.005(4) 0.025(4) -0.002(4) C23 0.072(4) 0.066(4) 0.064(4) -0.005(3) 0.024(3) -0.001(3) C24 0.050(4) 0.054(4) 0.058(4) 0.002(3) 0.022(3) 0.007(3) C25 0.065(4) 0.063(4) 0.072(4) -0.001(3) 0.020(3) 0.002(3) C26 0.048(4) 0.050(5) 0.056(5) 0.004(4) 0.017(4) 0.000(4) C27 0.046(3) 0.051(4) 0.053(3) 0.005(3) 0.018(3) 0.006(3) C28 0.048(3) 0.057(4) 0.053(3) 0.004(3) 0.016(3) 0.003(3) C29 0.064(4) 0.063(4) 0.063(4) 0.002(3) 0.016(3) -0.002(3) C30 0.075(4) 0.078(4) 0.072(4) -0.002(4) 0.021(3) -0.004(4) C31 0.082(4) 0.089(5) 0.075(4) -0.002(4) 0.023(4) -0.004(4) C32 0.078(4) 0.071(4) 0.067(4) 0.006(3) 0.017(4) 0.006(4) N1 0.050(3) 0.036(3) 0.030(3) -0.001(2) 0.008(3) -0.002(3) N2 0.046(3) 0.029(3) 0.028(3) 0.001(2) 0.007(2) 0.003(2) N3 0.042(3) 0.033(3) 0.030(3) 0.002(2) 0.006(2) -0.003(2) N4 0.047(3) 0.030(3) 0.031(3) 0.000(2) 0.007(3) 0.001(3) N5 0.045(3) 0.042(3) 0.028(3) 0.000(2) 0.005(3) 0.001(3) N6 0.079(5) 0.056(5) 0.100(6) -0.011(4) 0.027(5) 0.001(4) N7 0.052(4) 0.054(4) 0.055(4) 0.008(3) 0.014(3) -0.001(3) N8 0.050(4) 0.055(4) 0.046(3) 0.007(3) 0.008(3) -0.002(3) N9 0.048(4) 0.058(4) 0.051(4) 0.011(3) 0.010(3) 0.010(3) N10 0.100(6) 0.103(7) 0.052(4) 0.011(4) 0.001(4) 0.020(5) O1 0.053(3) 0.051(3) 0.034(3) -0.005(2) 0.011(2) 0.004(2) O2 0.047(3) 0.058(3) 0.041(3) 0.004(2) 0.006(2) 0.011(2) O3 0.053(3) 0.045(3) 0.036(3) 0.011(2) 0.003(2) -0.014(2) O4 0.053(3) 0.046(3) 0.031(2) 0.000(2) 0.001(2) -0.003(2) O5 0.059(3) 0.047(3) 0.064(3) -0.001(3) -0.011(3) -0.002(3) O6 0.129(5) 0.104(5) 0.086(4) -0.028(4) -0.007(4) 0.009(4) O7 0.119(5) 0.106(5) 0.068(4) 0.001(3) 0.019(4) -0.043(4) O8 0.150(6) 0.067(4) 0.117(5) 0.014(4) 0.014(5) 0.010(4) O9 0.328(12) 0.322(12) 0.309(12) -0.004(9) 0.105(9) 0.001(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N1 2.320(5) . y Cd1 N5 2.330(5) 3_757 y Cd1 O1 2.338(5) . y Cd1 O3 2.368(4) 2_646 y Cd1 O5 2.415(5) . y Cd1 O4 2.478(5) 2_646 y Cd1 O2 2.506(5) . y C1 O1 1.250(7) . ? C1 O2 1.267(7) . ? C1 C2 1.505(9) . ? C2 C3 1.391(9) . ? C2 C7 1.400(9) . ? C3 C4 1.389(10) . ? C3 H3A 0.9300 . ? C4 C5 1.379(11) . ? C4 H4A 0.9300 . ? C5 C6 1.389(10) . ? C5 H5 0.9300 . ? C6 C7 1.391(9) . ? C6 H6 0.9300 . ? C7 C8 1.497(8) . ? C8 O3 1.242(7) . ? C8 O4 1.261(7) . ? C9 N1 1.344(8) . ? C9 C10 1.363(9) . ? C9 H9 0.9300 . ? C10 C11 1.380(9) . ? C10 H10A 0.9300 . ? C11 C12 1.382(8) . ? C11 H11A 0.9300 . ? C12 C13 1.380(9) . ? C12 C14 1.471(8) . ? C13 N1 1.327(8) . ? C13 H13A 0.9300 . ? C14 N3 1.330(8) . ? C14 N2 1.346(7) . ? C15 N4 1.326(8) . ? C15 N2 1.353(8) . ? C15 C16 1.470(8) . ? C16 C17 1.373(8) . ? C16 C18 1.393(9) . ? C17 N5 1.344(8) . ? C17 H17A 0.9300 . ? C18 C19 1.371(9) . ? C18 H18A 0.9300 . ? C19 C20 1.377(9) . ? C19 H19A 0.9300 . ? C20 N5 1.335(8) . ? C20 H20A 0.9300 . ? C21 N6 1.334(11) . ? C21 C22 1.378(12) . ? C21 H21A 0.9300 . ? C22 C23 1.394(12) . ? C22 H22A 0.9300 . ? C23 C24 1.391(11) . ? C23 H23A 0.9300 . ? C24 C25 1.384(11) . ? C24 C26 1.454(10) . ? C25 N6 1.342(10) . ? C25 H25A 0.9300 . ? C26 N7 1.331(9) . ? C26 N9 1.366(9) . ? C27 N9 1.327(9) . ? C27 N8 1.367(9) . ? C27 C28 1.466(10) . ? C28 C29 1.372(11) . ? C28 C32 1.393(11) . ? C29 C30 1.382(12) . ? C29 H29A 0.9300 . ? C30 C31 1.381(12) . ? C30 H30A 0.9300 . ? C31 N10 1.323(12) . ? C31 H31A 0.9300 . ? C32 N10 1.334(11) . ? C32 H32A 0.9300 . ? N3 N4 1.371(7) . ? N3 H3 0.9210 . ? N5 Cd1 2.330(5) 3_757 ? N7 N8 1.356(8) . ? N8 H8 0.9586 . ? O3 Cd1 2.368(4) 2_656 ? O4 Cd1 2.478(5) 2_656 ? O5 H5A 0.8476 . ? O5 H5B 0.8607 . ? O6 H6B 0.8722 . ? O6 H6A 0.8477 . ? O7 H7A 0.8614 . ? O7 H7B 0.8524 . ? O8 H8A 0.8620 . ? O8 H8B 0.8681 . ? O9 H9A 0.8501 . ? O9 H9B 0.8501 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cd1 N5 164.86(18) . 3_757 y N1 Cd1 O1 89.52(18) . . y N5 Cd1 O1 96.76(18) 3_757 . y N1 Cd1 O3 93.65(17) . 2_646 y N5 Cd1 O3 100.18(17) 3_757 2_646 y O1 Cd1 O3 89.22(16) . 2_646 y N1 Cd1 O5 83.67(18) . . y N5 Cd1 O5 82.74(18) 3_757 . y O1 Cd1 O5 140.57(17) . . y O3 Cd1 O5 129.86(17) 2_646 . y N1 Cd1 O4 95.76(18) . 2_646 y N5 Cd1 O4 87.63(17) 3_757 2_646 y O1 Cd1 O4 142.54(15) . 2_646 y O3 Cd1 O4 53.50(15) 2_646 2_646 y O5 Cd1 O4 76.88(16) . 2_646 y N1 Cd1 O2 88.81(17) . . y N5 Cd1 O2 83.81(17) 3_757 . y O1 Cd1 O2 54.13(15) . . y O3 Cd1 O2 143.27(16) 2_646 . y O5 Cd1 O2 86.84(17) . . y O4 Cd1 O2 162.46(14) 2_646 . y O1 C1 O2 122.7(6) . . ? O1 C1 C2 118.3(6) . . ? O2 C1 C2 118.8(6) . . ? C3 C2 C7 119.4(6) . . ? C3 C2 C1 118.9(6) . . ? C7 C2 C1 121.3(5) . . ? C4 C3 C2 120.4(7) . . ? C4 C3 H3A 119.8 . . ? C2 C3 H3A 119.8 . . ? C5 C4 C3 120.5(7) . . ? C5 C4 H4A 119.8 . . ? C3 C4 H4A 119.8 . . ? C4 C5 C6 119.3(7) . . ? C4 C5 H5 120.3 . . ? C6 C5 H5 120.3 . . ? C5 C6 C7 121.0(7) . . ? C5 C6 H6 119.5 . . ? C7 C6 H6 119.5 . . ? C6 C7 C2 119.3(6) . . ? C6 C7 C8 118.4(6) . . ? C2 C7 C8 122.2(6) . . ? O3 C8 O4 121.5(6) . . ? O3 C8 C7 120.2(5) . . ? O4 C8 C7 118.2(6) . . ? N1 C9 C10 122.9(6) . . ? N1 C9 H9 118.6 . . ? C10 C9 H9 118.6 . . ? C9 C10 C11 119.3(6) . . ? C9 C10 H10A 120.3 . . ? C11 C10 H10A 120.3 . . ? C10 C11 C12 118.7(6) . . ? C10 C11 H11A 120.7 . . ? C12 C11 H11A 120.7 . . ? C13 C12 C11 118.1(6) . . ? C13 C12 C14 119.2(5) . . ? C11 C12 C14 122.7(6) . . ? N1 C13 C12 123.7(6) . . ? N1 C13 H13A 118.1 . . ? C12 C13 H13A 118.1 . . ? N3 C14 N2 110.1(5) . . ? N3 C14 C12 124.6(5) . . ? N2 C14 C12 125.2(6) . . ? N4 C15 N2 114.6(5) . . ? N4 C15 C16 121.7(6) . . ? N2 C15 C16 123.5(5) . . ? C17 C16 C18 117.6(6) . . ? C17 C16 C15 120.3(6) . . ? C18 C16 C15 122.1(6) . . ? N5 C17 C16 123.8(6) . . ? N5 C17 H17A 118.1 . . ? C16 C17 H17A 118.1 . . ? C19 C18 C16 119.1(6) . . ? C19 C18 H18A 120.4 . . ? C16 C18 H18A 120.4 . . ? C18 C19 C20 119.5(6) . . ? C18 C19 H19A 120.2 . . ? C20 C19 H19A 120.2 . . ? N5 C20 C19 122.4(6) . . ? N5 C20 H20A 118.8 . . ? C19 C20 H20A 118.8 . . ? N6 C21 C22 122.8(9) . . ? N6 C21 H21A 118.6 . . ? C22 C21 H21A 118.6 . . ? C21 C22 C23 119.4(9) . . ? C21 C22 H22A 120.3 . . ? C23 C22 H22A 120.3 . . ? C22 C23 C24 118.1(8) . . ? C22 C23 H23A 120.9 . . ? C24 C23 H23A 120.9 . . ? C25 C24 C23 118.4(8) . . ? C25 C24 C26 120.2(7) . . ? C23 C24 C26 121.3(7) . . ? N6 C25 C24 123.4(8) . . ? N6 C25 H25A 118.3 . . ? C24 C25 H25A 118.3 . . ? N7 C26 N9 113.2(7) . . ? N7 C26 C24 122.6(7) . . ? N9 C26 C24 123.9(7) . . ? N9 C27 N8 110.3(6) . . ? N9 C27 C28 127.7(7) . . ? N8 C27 C28 122.0(7) . . ? C29 C28 C32 117.6(8) . . ? C29 C28 C27 122.7(7) . . ? C32 C28 C27 119.7(7) . . ? C28 C29 C30 119.9(8) . . ? C28 C29 H29A 120.1 . . ? C30 C29 H29A 120.1 . . ? C29 C30 C31 117.5(9) . . ? C29 C30 H30A 121.3 . . ? C31 C30 H30A 121.3 . . ? N10 C31 C30 124.5(9) . . ? N10 C31 H31A 117.8 . . ? C30 C31 H31A 117.8 . . ? N10 C32 C28 123.7(9) . . ? N10 C32 H32A 118.1 . . ? C28 C32 H32A 118.1 . . ? C13 N1 C9 117.3(6) . . ? C13 N1 Cd1 119.6(4) . . ? C9 N1 Cd1 122.7(4) . . ? C14 N2 C15 102.9(5) . . ? C14 N3 N4 109.7(5) . . ? C14 N3 H3 135.2 . . ? N4 N3 H3 115.1 . . ? C15 N4 N3 102.7(5) . . ? C20 N5 C17 117.6(6) . . ? C20 N5 Cd1 123.9(4) . 3_757 ? C17 N5 Cd1 117.5(4) . 3_757 ? C21 N6 C25 117.8(8) . . ? C26 N7 N8 104.5(6) . . ? N7 N8 C27 108.2(6) . . ? N7 N8 H8 122.2 . . ? C27 N8 H8 127.2 . . ? C27 N9 C26 103.7(6) . . ? C32 N10 C31 116.8(8) . . ? C1 O1 Cd1 95.3(4) . . ? C1 O2 Cd1 87.2(4) . . ? C8 O3 Cd1 95.3(4) . 2_656 ? C8 O4 Cd1 89.7(4) . 2_656 ? Cd1 O5 H5A 120.7 . . ? Cd1 O5 H5B 120.1 . . ? H5A O5 H5B 119.0 . . ? H6B O6 H6A 104.8 . . ? H7A O7 H7B 108.3 . . ? H8A O8 H8B 112.2 . . ? H9A O9 H9B 124.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 125.5(7) . . . . ? O2 C1 C2 C3 -49.0(9) . . . . ? O1 C1 C2 C7 -46.8(9) . . . . ? O2 C1 C2 C7 138.8(6) . . . . ? C7 C2 C3 C4 0.4(11) . . . . ? C1 C2 C3 C4 -172.0(7) . . . . ? C2 C3 C4 C5 0.0(13) . . . . ? C3 C4 C5 C6 0.2(13) . . . . ? C4 C5 C6 C7 -0.7(12) . . . . ? C5 C6 C7 C2 1.1(10) . . . . ? C5 C6 C7 C8 -176.4(7) . . . . ? C3 C2 C7 C6 -0.9(10) . . . . ? C1 C2 C7 C6 171.3(6) . . . . ? C3 C2 C7 C8 176.5(6) . . . . ? C1 C2 C7 C8 -11.3(9) . . . . ? C6 C7 C8 O3 128.6(7) . . . . ? C2 C7 C8 O3 -48.8(9) . . . . ? C6 C7 C8 O4 -47.4(8) . . . . ? C2 C7 C8 O4 135.2(6) . . . . ? N1 C9 C10 C11 -0.1(11) . . . . ? C9 C10 C11 C12 -0.3(10) . . . . ? C10 C11 C12 C13 -0.1(10) . . . . ? C10 C11 C12 C14 -177.3(6) . . . . ? C11 C12 C13 N1 1.0(10) . . . . ? C14 C12 C13 N1 178.4(6) . . . . ? C13 C12 C14 N3 -161.1(6) . . . . ? C11 C12 C14 N3 16.1(10) . . . . ? C13 C12 C14 N2 16.1(10) . . . . ? C11 C12 C14 N2 -166.7(6) . . . . ? N4 C15 C16 C17 172.1(6) . . . . ? N2 C15 C16 C17 -2.9(10) . . . . ? N4 C15 C16 C18 -5.8(10) . . . . ? N2 C15 C16 C18 179.2(6) . . . . ? C18 C16 C17 N5 1.5(10) . . . . ? C15 C16 C17 N5 -176.4(6) . . . . ? C17 C16 C18 C19 -0.5(10) . . . . ? C15 C16 C18 C19 177.4(6) . . . . ? C16 C18 C19 C20 0.1(11) . . . . ? C18 C19 C20 N5 -0.6(11) . . . . ? N6 C21 C22 C23 1.7(15) . . . . ? C21 C22 C23 C24 -1.8(13) . . . . ? C22 C23 C24 C25 1.3(12) . . . . ? C22 C23 C24 C26 -175.1(8) . . . . ? C23 C24 C25 N6 -0.8(13) . . . . ? C26 C24 C25 N6 175.6(8) . . . . ? C25 C24 C26 N7 -163.5(7) . . . . ? C23 C24 C26 N7 12.9(12) . . . . ? C25 C24 C26 N9 9.6(12) . . . . ? C23 C24 C26 N9 -174.1(7) . . . . ? N9 C27 C28 C29 179.2(8) . . . . ? N8 C27 C28 C29 -0.4(12) . . . . ? N9 C27 C28 C32 1.3(12) . . . . ? N8 C27 C28 C32 -178.3(7) . . . . ? C32 C28 C29 C30 -0.8(12) . . . . ? C27 C28 C29 C30 -178.7(7) . . . . ? C28 C29 C30 C31 1.9(13) . . . . ? C29 C30 C31 N10 -2.6(16) . . . . ? C29 C28 C32 N10 0.1(14) . . . . ? C27 C28 C32 N10 178.2(8) . . . . ? C12 C13 N1 C9 -1.4(10) . . . . ? C12 C13 N1 Cd1 -174.3(5) . . . . ? C10 C9 N1 C13 0.9(10) . . . . ? C10 C9 N1 Cd1 173.6(5) . . . . ? N5 Cd1 N1 C13 -23.4(10) 3_757 . . . ? O1 Cd1 N1 C13 91.4(5) . . . . ? O3 Cd1 N1 C13 -179.4(5) 2_646 . . . ? O5 Cd1 N1 C13 -49.7(5) . . . . ? O4 Cd1 N1 C13 -125.7(5) 2_646 . . . ? O2 Cd1 N1 C13 37.3(5) . . . . ? N5 Cd1 N1 C9 164.1(6) 3_757 . . . ? O1 Cd1 N1 C9 -81.0(5) . . . . ? O3 Cd1 N1 C9 8.2(5) 2_646 . . . ? O5 Cd1 N1 C9 137.9(5) . . . . ? O4 Cd1 N1 C9 61.8(5) 2_646 . . . ? O2 Cd1 N1 C9 -135.2(5) . . . . ? N3 C14 N2 C15 1.4(7) . . . . ? C12 C14 N2 C15 -176.1(6) . . . . ? N4 C15 N2 C14 0.0(7) . . . . ? C16 C15 N2 C14 175.4(6) . . . . ? N2 C14 N3 N4 -2.4(7) . . . . ? C12 C14 N3 N4 175.2(6) . . . . ? N2 C15 N4 N3 -1.4(7) . . . . ? C16 C15 N4 N3 -176.8(5) . . . . ? C14 N3 N4 C15 2.2(7) . . . . ? C19 C20 N5 C17 1.5(10) . . . . ? C19 C20 N5 Cd1 -166.8(5) . . . 3_757 ? C16 C17 N5 C20 -2.0(10) . . . . ? C16 C17 N5 Cd1 167.1(5) . . . 3_757 ? C22 C21 N6 C25 -1.2(14) . . . . ? C24 C25 N6 C21 0.7(13) . . . . ? N9 C26 N7 N8 1.4(8) . . . . ? C24 C26 N7 N8 175.1(7) . . . . ? C26 N7 N8 C27 -1.7(8) . . . . ? N9 C27 N8 N7 1.4(8) . . . . ? C28 C27 N8 N7 -178.9(6) . . . . ? N8 C27 N9 C26 -0.6(8) . . . . ? C28 C27 N9 C26 179.8(7) . . . . ? N7 C26 N9 C27 -0.5(8) . . . . ? C24 C26 N9 C27 -174.2(7) . . . . ? C28 C32 N10 C31 -0.6(15) . . . . ? C30 C31 N10 C32 1.9(16) . . . . ? O2 C1 O1 Cd1 9.1(7) . . . . ? C2 C1 O1 Cd1 -165.1(5) . . . . ? N1 Cd1 O1 C1 -93.7(4) . . . . ? N5 Cd1 O1 C1 72.5(4) 3_757 . . . ? O3 Cd1 O1 C1 172.7(4) 2_646 . . . ? O5 Cd1 O1 C1 -14.3(5) . . . . ? O4 Cd1 O1 C1 167.5(4) 2_646 . . . ? O2 Cd1 O1 C1 -4.8(4) . . . . ? O1 C1 O2 Cd1 -8.5(6) . . . . ? C2 C1 O2 Cd1 165.7(5) . . . . ? N1 Cd1 O2 C1 95.0(4) . . . . ? N5 Cd1 O2 C1 -98.3(4) 3_757 . . . ? O1 Cd1 O2 C1 4.7(4) . . . . ? O3 Cd1 O2 C1 0.5(5) 2_646 . . . ? O5 Cd1 O2 C1 178.7(4) . . . . ? O4 Cd1 O2 C1 -159.5(5) 2_646 . . . ? O4 C8 O3 Cd1 1.8(6) . . . 2_656 ? C7 C8 O3 Cd1 -174.1(5) . . . 2_656 ? O3 C8 O4 Cd1 -1.7(6) . . . 2_656 ? C7 C8 O4 Cd1 174.3(5) . . . 2_656 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.707 _refine_diff_density_min -0.520 _refine_diff_density_rms 0.092 data_6 _database_code_depnum_ccdc_archive 'CCDC 862820' #TrackingRef '6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H15 Cd N5 O6' _chemical_formula_weight 533.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M p21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.0410(14) _cell_length_b 23.337(5) _cell_length_c 13.814(4) _cell_angle_alpha 90.00 _cell_angle_beta 116.54(2) _cell_angle_gamma 90.00 _cell_volume 2030.7(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.746 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1064.0 _exptl_absorpt_coefficient_mu 1.125 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11003 _diffrn_reflns_av_R_equivalents 0.0790 _diffrn_reflns_av_sigmaI/netI 0.0841 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3587 _reflns_number_gt 2812 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0437P)^2^+89.5303P] 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 3579 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1529 _refine_ls_R_factor_gt 0.1260 _refine_ls_wR_factor_ref 0.3007 _refine_ls_wR_factor_gt 0.2899 _refine_ls_goodness_of_fit_ref 1.282 _refine_ls_restrained_S_all 1.282 _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 O3 O -0.130(2) 0.2091(6) -0.0340(12) 0.058(4) Uani 1 1 d . . . O4 O 0.153(2) 0.1589(6) -0.0044(12) 0.045(4) Uani 1 1 d . . . C8 C -0.020(3) 0.1649(8) 0.0030(15) 0.038(5) Uani 1 1 d . . . C7 C -0.086(2) 0.1186(7) 0.0544(14) 0.024(4) Uani 1 1 d . . . Cd1 Cd 0.1130(2) 0.26523(5) 0.37211(10) 0.0280(4) Uani 1 1 d . . . N1 N 0.273(2) 0.2001(5) 0.5126(11) 0.022(3) Uani 1 1 d . . . C13 C 0.266(3) 0.1433(7) 0.5053(14) 0.032(4) Uani 1 1 d . . . H13A H 0.1977 0.1271 0.4367 0.038 Uiso 1 1 calc R . . N5 N 0.006(2) -0.1659(6) 0.2631(12) 0.032(4) Uani 1 1 d . . . C18 C 0.109(3) -0.1804(7) 0.3682(17) 0.043(5) Uani 1 1 d . . . H18A H 0.1268 -0.2190 0.3869 0.052 Uiso 1 1 calc R . . C17 C 0.190(3) -0.1398(7) 0.4494(14) 0.026(4) Uani 1 1 d . . . H17A H 0.2547 -0.1513 0.5215 0.032 Uiso 1 1 calc R . . C19 C -0.008(3) -0.1095(8) 0.2403(14) 0.031(4) Uani 1 1 d . . . H19A H -0.0795 -0.0991 0.1678 0.037 Uiso 1 1 calc R . . C20 C 0.072(3) -0.0666(7) 0.3137(16) 0.042(5) Uani 1 1 d . . . H20A H 0.0598 -0.0286 0.2919 0.050 Uiso 1 1 calc R . . N3 N 0.372(2) -0.0426(6) 0.6087(11) 0.030(3) Uani 1 1 d . . . O2 O 0.1372(18) 0.2007(5) 0.2364(10) 0.031(3) Uani 1 1 d . . . C2 C -0.105(2) 0.1245(6) 0.1523(13) 0.022(4) Uani 1 1 d . . . C1 C -0.036(3) 0.1774(7) 0.2215(13) 0.024(4) Uani 1 1 d . . . N4 N 0.229(2) 0.0203(6) 0.4799(11) 0.030(3) Uani 1 1 d . . . C14 C 0.336(3) 0.0452(7) 0.5774(14) 0.028(4) Uani 1 1 d . . . O1 O -0.143(2) 0.1948(5) 0.2654(10) 0.038(3) Uani 1 1 d . . . C15 C 0.262(3) -0.0358(7) 0.5030(14) 0.023(4) Uani 1 1 d . . . C12 C 0.353(3) 0.1071(7) 0.5926(13) 0.026(4) Uani 1 1 d . . . O6 O 0.463(2) 0.3068(7) 0.4403(12) 0.053(4) Uani 1 1 d . . . N2 N 0.425(3) 0.0088(6) 0.6593(12) 0.034(4) Uani 1 1 d . . . C5 C -0.233(3) 0.0235(8) 0.0343(18) 0.048(6) Uani 1 1 d . . . H5A H -0.2764 -0.0104 -0.0052 0.058 Uiso 1 1 calc R . . C4 C -0.252(3) 0.0293(8) 0.1263(16) 0.038(5) Uani 1 1 d . . . H4A H -0.3073 -0.0006 0.1504 0.045 Uiso 1 1 calc R . . C3 C -0.190(3) 0.0795(8) 0.1856(17) 0.039(5) Uani 1 1 d . . . H3A H -0.2062 0.0831 0.2486 0.047 Uiso 1 1 calc R . . C6 C -0.149(3) 0.0672(7) -0.0021(15) 0.031(4) Uani 1 1 d . . . H6A H -0.1350 0.0623 -0.0653 0.037 Uiso 1 1 calc R . . C16 C 0.174(3) -0.0816(7) 0.4237(14) 0.022(3) Uani 1 1 d . . . C10 C 0.478(3) 0.1905(8) 0.7024(15) 0.040(5) Uani 1 1 d . . . H10A H 0.5567 0.2079 0.7692 0.048 Uiso 1 1 calc R . . C11 C 0.462(3) 0.1320(8) 0.6949(14) 0.029(4) Uani 1 1 d . . . H11A H 0.5216 0.1092 0.7566 0.035 Uiso 1 1 calc R . . C9 C 0.378(3) 0.2238(8) 0.6098(14) 0.038(5) Uani 1 1 d . . . H9A H 0.3850 0.2636 0.6160 0.046 Uiso 1 1 calc R . . O5 O 0.513(2) 0.1457(6) 0.2844(12) 0.052(4) Uani 1 1 d . . . H5D H 0.3962 0.1626 0.2695 0.063 Uiso 1 1 d R . . H3 H 0.4091 -0.0763 0.6430 0.063 Uiso 1 1 d R . . H5C H 0.6178 0.1605 0.2787 0.063 Uiso 1 1 d R . . H6B H -0.1302 0.2085 -0.0338 0.063 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 O3 0.059(10) 0.047(9) 0.049(9) 0.016(7) 0.009(8) -0.008(8) O4 0.055(9) 0.043(8) 0.057(9) -0.009(7) 0.043(8) -0.009(7) C8 0.044(12) 0.035(11) 0.026(10) -0.006(8) 0.007(9) -0.002(9) C7 0.020(8) 0.020(8) 0.029(9) 0.002(7) 0.009(7) -0.005(7) Cd1 0.0328(7) 0.0234(6) 0.0236(7) -0.0002(6) 0.0087(5) -0.0002(6) N1 0.021(7) 0.012(6) 0.027(8) -0.004(6) 0.006(6) -0.001(5) C13 0.039(11) 0.027(9) 0.020(9) -0.005(7) 0.004(8) -0.006(8) N5 0.029(8) 0.029(8) 0.028(8) -0.003(6) 0.003(7) -0.008(7) C18 0.067(14) 0.016(8) 0.040(11) 0.001(8) 0.018(10) 0.006(9) C17 0.029(9) 0.021(9) 0.026(9) 0.003(7) 0.009(8) -0.006(7) C19 0.032(10) 0.033(10) 0.020(9) 0.003(8) 0.005(8) 0.000(8) C20 0.057(13) 0.013(8) 0.040(12) 0.004(8) 0.008(10) 0.016(8) N3 0.043(9) 0.017(7) 0.027(9) -0.002(6) 0.014(7) 0.001(6) O2 0.030(7) 0.029(6) 0.034(7) -0.007(5) 0.015(6) -0.011(5) C2 0.022(8) 0.012(7) 0.026(9) -0.004(6) 0.007(7) 0.004(6) C1 0.038(10) 0.015(8) 0.025(9) 0.008(7) 0.018(8) 0.004(7) N4 0.050(10) 0.021(7) 0.022(8) -0.001(6) 0.020(7) 0.000(7) C14 0.043(10) 0.022(9) 0.027(9) 0.001(7) 0.024(8) -0.006(8) O1 0.041(8) 0.036(7) 0.033(7) -0.019(6) 0.015(6) -0.005(6) C15 0.022(8) 0.017(8) 0.029(9) 0.002(7) 0.010(7) 0.002(7) C12 0.038(10) 0.019(8) 0.021(9) -0.002(7) 0.014(8) -0.005(7) O6 0.041(8) 0.067(10) 0.054(10) -0.017(8) 0.025(7) -0.014(7) N2 0.055(10) 0.021(7) 0.026(9) 0.003(6) 0.018(8) -0.003(7) C5 0.039(12) 0.027(10) 0.052(14) -0.021(10) -0.003(10) -0.018(9) C4 0.040(11) 0.027(10) 0.038(12) 0.003(8) 0.010(9) -0.003(8) C3 0.037(11) 0.037(11) 0.046(12) 0.005(9) 0.022(10) -0.002(9) C6 0.033(10) 0.025(9) 0.034(10) -0.016(8) 0.013(8) -0.001(8) C16 0.027(9) 0.018(8) 0.031(9) -0.001(7) 0.023(8) -0.002(7) C10 0.051(12) 0.036(10) 0.025(10) -0.014(8) 0.011(9) -0.006(9) C11 0.031(10) 0.035(10) 0.018(9) -0.001(7) 0.009(8) -0.005(8) C9 0.052(12) 0.025(9) 0.028(10) -0.003(8) 0.009(9) -0.006(9) O5 0.044(8) 0.061(10) 0.059(10) 0.029(8) 0.029(8) 0.009(7) _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 O3 C8 1.25(2) . ? O3 Cd1 2.640(17) 4_565 ? O3 H6B 0.0136 . ? O4 C8 1.28(2) . ? O4 Cd1 2.386(14) 4_565 ? C8 C7 1.48(3) . ? C8 H6B 1.2419 . ? C7 C6 1.39(2) . ? C7 C2 1.42(2) . ? Cd1 N5 2.318(14) 3_555 y Cd1 N1 2.322(13) . y Cd1 O4 2.386(14) 4_566 y Cd1 O1 2.397(12) . y Cd1 O6 2.417(14) . y Cd1 O2 2.470(12) . y Cd1 O3 2.640(17) 4_566 y N1 C13 1.33(2) . ? N1 C9 1.33(2) . ? C13 C12 1.37(2) . ? C13 H13A 0.9300 . ? N5 C18 1.34(2) . ? N5 C19 1.35(2) . ? N5 Cd1 2.318(14) 2_545 ? C18 C17 1.38(2) . ? C18 H18A 0.9300 . ? C17 C16 1.39(2) . ? C17 H17A 0.9300 . ? C19 C20 1.35(3) . ? C19 H19A 0.9300 . ? C20 C16 1.40(2) . ? C20 H20A 0.9300 . ? N3 C15 1.32(2) . ? N3 N2 1.353(19) . ? N3 H3 0.8964 . ? O2 C1 1.27(2) . ? C2 C3 1.39(2) . ? C2 C1 1.50(2) . ? C1 O1 1.22(2) . ? N4 C15 1.34(2) . ? N4 C14 1.35(2) . ? C14 N2 1.33(2) . ? C14 C12 1.46(2) . ? C15 C16 1.46(2) . ? C12 C11 1.40(2) . ? C5 C4 1.34(3) . ? C5 C6 1.38(3) . ? C5 H5A 0.9300 . ? C4 C3 1.38(3) . ? C4 H4A 0.9300 . ? C3 H3A 0.9300 . ? C6 H6A 0.9300 . ? C10 C11 1.37(2) . ? C10 C9 1.39(3) . ? C10 H10A 0.9300 . ? C11 H11A 0.9300 . ? C9 H9A 0.9300 . ? O5 H5D 0.8500 . ? O5 H5C 0.8501 . ? 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 C8 O3 Cd1 88.1(13) . 4_565 ? C8 O3 H6B 27.5 . . ? Cd1 O3 H6B 102.6 4_565 . ? C8 O4 Cd1 99.3(12) . 4_565 ? O3 C8 O4 119.9(19) . . ? O3 C8 C7 121.7(19) . . ? O4 C8 C7 118.4(17) . . ? O3 C8 H6B 0.3 . . ? O4 C8 H6B 120.1 . . ? C7 C8 H6B 121.5 . . ? C6 C7 C2 118.3(15) . . ? C6 C7 C8 116.8(16) . . ? C2 C7 C8 124.7(15) . . ? N5 Cd1 N1 173.1(5) 2 . y N5 Cd1 O4 86.9(5) 2 4_566 y N1 Cd1 O4 91.7(5) . 4_566 y N5 Cd1 O1 94.5(5) 2 . y N1 Cd1 O1 90.9(5) . . y O4 Cd1 O1 140.0(5) 4_566 . y N5 Cd1 O6 88.5(5) 2 . y N1 Cd1 O6 84.7(5) . . y O4 Cd1 O6 69.4(5) 4_566 . y O1 Cd1 O6 150.5(5) . . y N5 Cd1 O2 86.2(5) 2 . y N1 Cd1 O2 93.6(4) . . y O4 Cd1 O2 165.6(4) 4_566 . y O1 Cd1 O2 53.3(4) . . y O6 Cd1 O2 97.8(4) . . y N5 Cd1 O3 99.1(5) 2 4_566 y N1 Cd1 O3 85.2(5) . 4_566 y O4 Cd1 O3 51.4(5) 4_566 4_566 y O1 Cd1 O3 89.1(5) . 4_566 y O6 Cd1 O3 119.4(5) . 4_566 y O2 Cd1 O3 142.4(4) . 4_566 y C13 N1 C9 118.5(15) . . ? C13 N1 Cd1 127.0(11) . . ? C9 N1 Cd1 114.5(11) . . ? N1 C13 C12 124.1(16) . . ? N1 C13 H13A 118.0 . . ? C12 C13 H13A 118.0 . . ? C18 N5 C19 116.4(15) . . ? C18 N5 Cd1 121.5(12) . 2_545 ? C19 N5 Cd1 121.8(12) . 2_545 ? N5 C18 C17 122.2(16) . . ? N5 C18 H18A 118.9 . . ? C17 C18 H18A 118.9 . . ? C18 C17 C16 120.2(16) . . ? C18 C17 H17A 119.9 . . ? C16 C17 H17A 119.9 . . ? N5 C19 C20 125.8(16) . . ? N5 C19 H19A 117.1 . . ? C20 C19 H19A 117.1 . . ? C19 C20 C16 117.8(16) . . ? C19 C20 H20A 121.1 . . ? C16 C20 H20A 121.1 . . ? C15 N3 N2 110.8(13) . . ? C15 N3 H3 125.4 . . ? N2 N3 H3 123.9 . . ? C1 O2 Cd1 89.8(10) . . ? C3 C2 C7 118.6(15) . . ? C3 C2 C1 118.5(16) . . ? C7 C2 C1 122.9(14) . . ? O1 C1 O2 122.4(16) . . ? O1 C1 C2 119.4(15) . . ? O2 C1 C2 118.1(15) . . ? C15 N4 C14 102.9(14) . . ? N2 C14 N4 114.6(15) . . ? N2 C14 C12 122.4(16) . . ? N4 C14 C12 123.1(15) . . ? C1 O1 Cd1 94.3(11) . . ? N3 C15 N4 109.5(14) . . ? N3 C15 C16 125.8(14) . . ? N4 C15 C16 124.6(15) . . ? C13 C12 C11 117.4(15) . . ? C13 C12 C14 120.6(15) . . ? C11 C12 C14 122.0(15) . . ? C14 N2 N3 102.2(14) . . ? C4 C5 C6 120.5(17) . . ? C4 C5 H5A 119.7 . . ? C6 C5 H5A 119.7 . . ? C5 C4 C3 120.5(19) . . ? C5 C4 H4A 119.7 . . ? C3 C4 H4A 119.7 . . ? C4 C3 C2 121.0(19) . . ? C4 C3 H3A 119.5 . . ? C2 C3 H3A 119.5 . . ? C5 C6 C7 121.0(18) . . ? C5 C6 H6A 119.5 . . ? C7 C6 H6A 119.5 . . ? C17 C16 C20 117.5(15) . . ? C17 C16 C15 124.4(15) . . ? C20 C16 C15 118.1(15) . . ? C11 C10 C9 119.8(16) . . ? C11 C10 H10A 120.1 . . ? C9 C10 H10A 120.1 . . ? C10 C11 C12 118.7(16) . . ? C10 C11 H11A 120.7 . . ? C12 C11 H11A 120.7 . . ? N1 C9 C10 121.4(16) . . ? N1 C9 H9A 119.3 . . ? C10 C9 H9A 119.3 . . ? H5D O5 H5C 125.2 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 4.019 _refine_diff_density_min -2.329 _refine_diff_density_rms 0.235