# 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 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C74 H62 N8 O22 Zn5' _chemical_formula_sum 'C74 H62 N8 O22 Zn5' _chemical_formula_weight 1742.17 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 14.9603(11) _cell_length_b 17.1932(13) _cell_length_c 27.477(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7067.5(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7040 _cell_measurement_theta_min 1.61 _cell_measurement_theta_max 26.02 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.637 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3552 _exptl_absorpt_coefficient_mu 1.758 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.790 _exptl_absorpt_correction_T_max 0.818 _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 9.00cm _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 37437 _diffrn_reflns_av_R_equivalents 0.0811 _diffrn_reflns_av_sigmaI/netI 0.0607 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 26.12 _reflns_number_total 7040 _reflns_number_gt 4409 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXP-97 _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0391P)^2^+4.9648P] 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 7040 _refine_ls_number_parameters 493 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0847 _refine_ls_R_factor_gt 0.0406 _refine_ls_wR_factor_ref 0.1031 _refine_ls_wR_factor_gt 0.0863 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _refine_ls_shift/su_max 0.004 _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 C1 C 0.8720(3) 0.1699(2) 1.17974(16) 0.0423(13) Uani 1 1 d . . . H1 H 0.8498 0.2046 1.1568 0.051 Uiso 1 1 calc R . . C2 C 0.8482(3) 0.1681(3) 1.22698(16) 0.0491(14) Uani 1 1 d . . . H2 H 0.8080 0.2011 1.2425 0.059 Uiso 1 1 calc R . . C3 C 0.9452(3) 0.0766(2) 1.21221(13) 0.0241(9) Uani 1 1 d . . . H3 H 0.9832 0.0344 1.2165 0.029 Uiso 1 1 calc R . . C4 C 0.8887(3) 0.0782(2) 1.29676(13) 0.0243(9) Uani 1 1 d . . . C5 C 0.8299(3) 0.1120(3) 1.32913(15) 0.0377(12) Uani 1 1 d . . . H5 H 0.7962 0.1548 1.3197 0.045 Uiso 1 1 calc R . . C6 C 0.8212(3) 0.0821(3) 1.37544(15) 0.0411(12) Uani 1 1 d . . . H6 H 0.7807 0.1040 1.3971 0.049 Uiso 1 1 calc R . . C7 C 0.8731(3) 0.0194(2) 1.38958(14) 0.0280(10) Uani 1 1 d . . . C8 C 0.9317(3) -0.0147(2) 1.35666(14) 0.0243(9) Uani 1 1 d . . . C9 C 0.9396(3) 0.0143(2) 1.31013(14) 0.0277(10) Uani 1 1 d . . . H9 H 0.9786 -0.0086 1.2880 0.033 Uiso 1 1 calc R . . C10 C 0.9785(3) -0.0844(2) 1.37915(15) 0.0293(10) Uani 1 1 d . . . C11 C 0.9423(3) -0.0816(2) 1.43065(14) 0.0245(9) Uani 1 1 d . . . C12 C 0.8787(3) -0.0233(2) 1.43599(14) 0.0282(10) Uani 1 1 d . . . C13 C 0.8329(3) -0.0147(2) 1.47944(15) 0.0361(11) Uani 1 1 d . . . H13 H 0.7895 0.0237 1.4828 0.043 Uiso 1 1 calc R . . C14 C 0.8525(3) -0.0639(2) 1.51798(15) 0.0357(11) Uani 1 1 d . . . H14 H 0.8219 -0.0594 1.5473 0.043 Uiso 1 1 calc R . . C15 C 0.9182(3) -0.1199(2) 1.51213(13) 0.0256(9) Uani 1 1 d . . . C16 C 0.9639(3) -0.1291(2) 1.46919(14) 0.0272(10) Uani 1 1 d . . . H16 H 1.0085 -0.1665 1.4662 0.033 Uiso 1 1 calc R . . C17 C 0.9479(4) -0.1599(2) 1.35408(16) 0.0496(14) Uani 1 1 d . . . H17A H 0.9711 -0.1614 1.3215 0.074 Uiso 1 1 calc R . . H17B H 0.8838 -0.1614 1.3531 0.074 Uiso 1 1 calc R . . H17C H 0.9697 -0.2039 1.3720 0.074 Uiso 1 1 calc R . . C18 C 1.0805(3) -0.0786(3) 1.37723(18) 0.0492(14) Uani 1 1 d . . . H18A H 1.1000 -0.0807 1.3440 0.074 Uiso 1 1 calc R . . H18B H 1.1063 -0.1211 1.3950 0.074 Uiso 1 1 calc R . . H18C H 1.0992 -0.0303 1.3915 0.074 Uiso 1 1 calc R . . C19 C 0.9662(2) -0.2452(2) 1.54742(14) 0.0225(9) Uani 1 1 d . . . H19 H 0.9772 -0.2697 1.5178 0.027 Uiso 1 1 calc R . . C20 C 0.9542(4) -0.2230(2) 1.62365(16) 0.0495(14) Uani 1 1 d . . . H20 H 0.9553 -0.2298 1.6572 0.059 Uiso 1 1 calc R . . C21 C 0.9305(4) -0.1573(3) 1.60062(16) 0.0531(15) Uani 1 1 d . . . H21 H 0.9123 -0.1111 1.6151 0.064 Uiso 1 1 calc R . . C22 C 1.1263(3) -0.0442(2) 1.16602(14) 0.0233(9) Uani 1 1 d . . . C23 C 1.1830(2) -0.0518(2) 1.21081(14) 0.0220(9) Uani 1 1 d . . . C24 C 1.2331(3) -0.1185(2) 1.21913(15) 0.0312(10) Uani 1 1 d . . . H24 H 1.2323 -0.1589 1.1966 0.037 Uiso 1 1 calc R . . C25 C 1.2842(3) -0.1249(2) 1.26088(15) 0.0330(11) Uani 1 1 d . . . H25 H 1.3203 -0.1683 1.2654 0.040 Uiso 1 1 calc R . . C26 C 1.2823(3) -0.0672(2) 1.29603(14) 0.0248(9) Uani 1 1 d . . . C27 C 1.2309(3) -0.0020(2) 1.28849(14) 0.0266(9) Uani 1 1 d . . . H27 H 1.2280 0.0363 1.3123 0.032 Uiso 1 1 calc R . . C28 C 1.1834(3) 0.0067(2) 1.24568(14) 0.0263(9) Uani 1 1 d . . . H28 H 1.1515 0.0523 1.2402 0.032 Uiso 1 1 calc R . . C29 C 1.3381(3) -0.0731(2) 1.34193(15) 0.0266(9) Uani 1 1 d . . . C30 C 0.8861(2) 0.1426(2) 1.02263(14) 0.0195(8) Uani 1 1 d . . . C31 C 0.8212(2) 0.2031(2) 1.00448(13) 0.0185(8) Uani 1 1 d . . . C32 C 0.7929(2) 0.2618(2) 1.03534(14) 0.0220(9) Uani 1 1 d . . . H32 H 0.8146 0.2638 1.0670 0.026 Uiso 1 1 calc R . . C33 C 0.7333(2) 0.3171(2) 1.01978(14) 0.0208(9) Uani 1 1 d . . . H33 H 0.7159 0.3571 1.0405 0.025 Uiso 1 1 calc R . . C34 C 0.6988(2) 0.3129(2) 0.97240(13) 0.0191(8) Uani 1 1 d . . . C35 C 0.7268(2) 0.2536(2) 0.94178(14) 0.0222(9) Uani 1 1 d . . . H35 H 0.7038 0.2504 0.9104 0.027 Uiso 1 1 calc R . . C36 C 0.7886(2) 0.1992(2) 0.95737(14) 0.0228(9) Uani 1 1 d . . . H36 H 0.8080 0.1602 0.9364 0.027 Uiso 1 1 calc R . . C37 C 1.1297(2) 0.1299(2) 1.04456(14) 0.0207(9) Uani 1 1 d . . . N1 N 0.9339(2) 0.11280(17) 1.17047(11) 0.0212(7) Uani 1 1 d . . . N2 N 0.8954(2) 0.10769(17) 1.24788(11) 0.0249(8) Uani 1 1 d . . . N3 N 0.9381(2) -0.17120(18) 1.55176(12) 0.0285(8) Uani 1 1 d . . . N4 N 0.9764(2) -0.27870(18) 1.58987(11) 0.0250(8) Uani 1 1 d . . . O1 O 1.09211(17) 0.02031(15) 1.15636(9) 0.0265(6) Uani 1 1 d . . . O2 O 1.11308(18) -0.10645(15) 1.14161(9) 0.0278(7) Uani 1 1 d . . . O3 O 1.30825(19) -0.04644(18) 1.38027(10) 0.0386(8) Uani 1 1 d . . . O4 O 1.41491(19) -0.10527(15) 1.33672(10) 0.0295(7) Uani 1 1 d . . . O5 O 0.90097(19) 0.14171(15) 1.06742(10) 0.0313(7) Uani 1 1 d . . . O6 O 0.92141(18) 0.09850(13) 0.99140(9) 0.0239(6) Uani 1 1 d . . . O7 O 1.09357(19) 0.14438(15) 1.08518(10) 0.0298(7) Uani 1 1 d . . . O8 O 1.11135(17) 0.07327(15) 1.01778(10) 0.0262(6) Uani 1 1 d . . . O9 O 0.96388(16) -0.01751(13) 1.07229(8) 0.0161(5) Uani 1 1 d . . . OW1 O 0.8701(4) -0.3030(3) 1.2844(2) 0.144(2) Uani 1 1 d . . . OW2 O 1.4996(3) -0.1923(3) 1.26601(17) 0.1119(17) Uani 1 1 d . . . Zn1 Zn 0.99486(3) 0.08018(2) 1.107926(14) 0.01750(11) Uani 1 1 d . . . Zn2 Zn 1.0000 0.0000 1.0000 0.01524(13) Uani 1 2 d S . . Zn3 Zn 1.00096(3) -0.11127(2) 1.106181(15) 0.02038(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.066(4) 0.034(2) 0.027(3) 0.011(2) 0.012(2) 0.024(2) C2 0.075(4) 0.040(3) 0.031(3) 0.005(2) 0.020(3) 0.039(3) C3 0.025(2) 0.029(2) 0.018(2) 0.0021(18) 0.0016(17) 0.0041(18) C4 0.031(2) 0.026(2) 0.017(2) 0.0025(17) 0.0024(17) 0.0033(19) C5 0.049(3) 0.039(3) 0.025(2) 0.009(2) 0.009(2) 0.023(2) C6 0.054(3) 0.044(3) 0.026(2) 0.008(2) 0.012(2) 0.028(2) C7 0.035(3) 0.029(2) 0.020(2) 0.0024(17) 0.0044(18) 0.0073(19) C8 0.022(2) 0.025(2) 0.026(2) 0.0037(18) 0.0009(17) -0.0012(18) C9 0.028(2) 0.029(2) 0.026(2) 0.0024(18) 0.0104(18) 0.0078(19) C10 0.032(3) 0.031(2) 0.025(2) 0.0060(18) 0.0104(18) 0.0103(19) C11 0.026(2) 0.026(2) 0.021(2) 0.0002(18) 0.0038(17) -0.0005(18) C12 0.035(3) 0.029(2) 0.021(2) 0.0016(18) 0.0020(18) 0.0082(19) C13 0.051(3) 0.032(2) 0.025(2) 0.0062(19) 0.007(2) 0.018(2) C14 0.051(3) 0.037(3) 0.020(2) 0.0009(19) 0.007(2) 0.012(2) C15 0.034(3) 0.026(2) 0.017(2) 0.0046(17) -0.0030(17) -0.0012(19) C16 0.030(2) 0.023(2) 0.029(2) 0.0042(18) 0.0032(19) 0.0043(18) C17 0.089(4) 0.030(3) 0.029(3) 0.001(2) 0.016(3) 0.008(3) C18 0.039(3) 0.054(3) 0.054(3) 0.029(3) 0.017(2) 0.019(3) C19 0.024(2) 0.019(2) 0.025(2) 0.0002(17) -0.0013(17) -0.0017(16) C20 0.106(5) 0.027(2) 0.016(2) -0.0022(19) 0.002(3) 0.011(3) C21 0.110(5) 0.027(2) 0.023(3) 0.000(2) 0.008(3) 0.019(3) C22 0.016(2) 0.034(2) 0.020(2) -0.0005(18) 0.0036(16) -0.0014(19) C23 0.018(2) 0.027(2) 0.021(2) 0.0032(17) -0.0033(16) -0.0021(17) C24 0.032(3) 0.027(2) 0.034(3) -0.007(2) -0.012(2) 0.003(2) C25 0.033(3) 0.027(2) 0.039(3) -0.003(2) -0.013(2) 0.007(2) C26 0.020(2) 0.028(2) 0.027(2) 0.0048(18) -0.0042(17) -0.0036(18) C27 0.026(2) 0.029(2) 0.025(2) -0.0031(18) -0.0032(18) -0.0007(18) C28 0.024(2) 0.029(2) 0.027(2) 0.0006(18) -0.0028(17) 0.0044(18) C29 0.023(2) 0.028(2) 0.029(2) 0.0066(19) -0.0069(18) -0.010(2) C30 0.016(2) 0.0164(19) 0.026(2) 0.0015(17) -0.0016(17) -0.0021(16) C31 0.014(2) 0.0203(19) 0.021(2) 0.0039(16) -0.0009(16) 0.0002(16) C32 0.021(2) 0.021(2) 0.024(2) 0.0013(17) -0.0006(17) 0.0013(17) C33 0.019(2) 0.021(2) 0.023(2) -0.0018(17) 0.0034(16) 0.0003(17) C34 0.018(2) 0.0184(19) 0.021(2) 0.0049(16) 0.0007(16) 0.0006(17) C35 0.022(2) 0.027(2) 0.018(2) 0.0006(17) -0.0014(16) 0.0019(17) C36 0.021(2) 0.019(2) 0.029(2) -0.0013(17) 0.0006(17) 0.0037(17) C37 0.016(2) 0.018(2) 0.028(2) 0.0054(17) -0.0037(17) 0.0007(16) N1 0.0209(18) 0.0238(17) 0.0189(17) 0.0012(14) 0.0002(14) 0.0009(15) N2 0.032(2) 0.0226(16) 0.0201(18) 0.0003(14) 0.0051(15) 0.0080(15) N3 0.043(2) 0.0199(17) 0.0223(19) -0.0003(14) 0.0008(16) 0.0019(16) N4 0.038(2) 0.0191(16) 0.0181(17) 0.0016(14) -0.0017(15) -0.0034(14) O1 0.0251(16) 0.0323(16) 0.0222(15) 0.0011(12) -0.0036(12) 0.0040(13) O2 0.0260(17) 0.0332(16) 0.0243(16) -0.0086(13) -0.0072(12) 0.0043(13) O3 0.0280(18) 0.063(2) 0.0247(17) -0.0010(15) -0.0027(13) -0.0041(16) O4 0.0311(18) 0.0268(15) 0.0306(17) -0.0019(12) -0.0136(13) 0.0010(13) O5 0.0375(19) 0.0342(16) 0.0221(16) 0.0006(13) -0.0073(13) 0.0165(14) O6 0.0274(16) 0.0214(14) 0.0230(15) 0.0027(12) 0.0010(12) 0.0090(12) O7 0.0324(18) 0.0283(16) 0.0287(17) -0.0012(13) 0.0100(13) -0.0113(13) O8 0.0215(16) 0.0276(15) 0.0294(16) -0.0026(13) 0.0019(12) -0.0101(13) O9 0.0185(13) 0.0162(13) 0.0135(13) 0.0005(10) 0.0003(10) 0.0011(10) OW1 0.124(5) 0.074(3) 0.234(7) -0.007(4) -0.090(5) 0.003(3) OW2 0.113(4) 0.151(5) 0.071(3) 0.000(3) -0.007(3) 0.001(3) Zn1 0.0191(2) 0.0185(2) 0.0149(2) 0.00057(17) 0.00109(19) -0.0007(2) Zn2 0.0166(3) 0.0152(3) 0.0139(3) 0.0016(2) 0.0001(3) 0.0001(3) Zn3 0.0216(3) 0.0170(2) 0.0226(2) -0.00013(17) -0.0019(2) 0.0013(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.346(6) . ? C1 N1 1.373(5) . ? C1 H1 0.9300 . ? C2 N2 1.381(5) . ? C2 H2 0.9300 . ? C3 N1 1.316(4) . ? C3 N2 1.342(5) . ? C3 H3 0.9300 . ? C4 C5 1.379(5) . ? C4 C9 1.386(5) . ? C4 N2 1.439(4) . ? C5 C6 1.378(5) . ? C5 H5 0.9300 . ? C6 C7 1.384(5) . ? C6 H6 0.9300 . ? C7 C8 1.390(5) . ? C7 C12 1.474(5) . ? C8 C9 1.378(5) . ? C8 C10 1.520(5) . ? C9 H9 0.9300 . ? C10 C11 1.516(5) . ? C10 C18 1.530(6) . ? C10 C17 1.538(6) . ? C11 C16 1.375(5) . ? C11 C12 1.391(5) . ? C12 C13 1.384(5) . ? C13 C14 1.387(5) . ? C13 H13 0.9300 . ? C14 C15 1.386(5) . ? C14 H14 0.9300 . ? C15 C16 1.372(5) . ? C15 N3 1.432(5) . ? C16 H16 0.9300 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 N4 1.310(5) . ? C19 N3 1.346(5) . ? C19 H19 0.9300 . ? C20 C21 1.343(6) . ? C20 N4 1.374(5) . ? C20 H20 0.9300 . ? C21 N3 1.368(5) . ? C21 H21 0.9300 . ? C22 O1 1.250(4) . ? C22 O2 1.278(4) . ? C22 C23 1.500(5) . ? C23 C28 1.389(5) . ? C23 C24 1.389(5) . ? C24 C25 1.383(5) . ? C24 H24 0.9300 . ? C25 C26 1.384(5) . ? C25 H25 0.9300 . ? C26 C27 1.375(5) . ? C26 C29 1.516(5) . ? C27 C28 1.382(5) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? C29 O3 1.233(5) . ? C29 O4 1.283(5) . ? C30 O5 1.251(4) . ? C30 O6 1.262(4) . ? C30 C31 1.507(5) . ? C31 C32 1.385(5) . ? C31 C36 1.385(5) . ? C32 C33 1.372(5) . ? C32 H32 0.9300 . ? C33 C34 1.402(5) . ? C33 H33 0.9300 . ? C34 C35 1.386(5) . ? C34 C37 1.501(5) 3_457 ? C35 C36 1.384(5) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C37 O8 1.251(4) . ? C37 O7 1.265(4) . ? C37 C34 1.501(5) 3_557 ? N1 Zn1 2.025(3) . ? N4 Zn3 1.978(3) 8_556 ? O1 Zn1 2.224(3) . ? O2 Zn3 1.941(3) . ? O4 Zn3 2.032(3) 6_658 ? O5 Zn1 2.081(3) . ? O6 Zn2 2.075(2) . ? O7 Zn1 1.947(3) . ? O8 Zn2 2.145(2) . ? O9 Zn3 1.942(2) . ? O9 Zn1 1.999(2) . ? O9 Zn2 2.081(2) . ? Zn2 O6 2.075(2) 5_757 ? Zn2 O9 2.081(2) 5_757 ? Zn2 O8 2.145(2) 5_757 ? Zn3 N4 1.978(3) 8 ? Zn3 O4 2.032(3) 6_558 ? 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 C2 C1 N1 109.9(4) . . ? C2 C1 H1 125.0 . . ? N1 C1 H1 125.0 . . ? C1 C2 N2 106.4(4) . . ? C1 C2 H2 126.8 . . ? N2 C2 H2 126.8 . . ? N1 C3 N2 112.1(3) . . ? N1 C3 H3 123.9 . . ? N2 C3 H3 123.9 . . ? C5 C4 C9 120.9(4) . . ? C5 C4 N2 119.9(3) . . ? C9 C4 N2 119.2(3) . . ? C6 C5 C4 119.9(4) . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C5 C6 C7 119.8(4) . . ? C5 C6 H6 120.1 . . ? C7 C6 H6 120.1 . . ? C6 C7 C8 120.0(4) . . ? C6 C7 C12 131.5(4) . . ? C8 C7 C12 108.5(3) . . ? C9 C8 C7 120.3(4) . . ? C9 C8 C10 128.6(4) . . ? C7 C8 C10 111.0(3) . . ? C8 C9 C4 119.1(4) . . ? C8 C9 H9 120.5 . . ? C4 C9 H9 120.5 . . ? C11 C10 C8 100.9(3) . . ? C11 C10 C18 112.7(4) . . ? C8 C10 C18 113.2(3) . . ? C11 C10 C17 109.8(3) . . ? C8 C10 C17 110.2(4) . . ? C18 C10 C17 109.7(4) . . ? C16 C11 C12 120.5(4) . . ? C16 C11 C10 128.0(4) . . ? C12 C11 C10 111.5(3) . . ? C13 C12 C11 120.4(4) . . ? C13 C12 C7 131.7(4) . . ? C11 C12 C7 107.8(3) . . ? C12 C13 C14 119.3(4) . . ? C12 C13 H13 120.4 . . ? C14 C13 H13 120.4 . . ? C15 C14 C13 119.0(4) . . ? C15 C14 H14 120.5 . . ? C13 C14 H14 120.5 . . ? C16 C15 C14 122.2(4) . . ? C16 C15 N3 118.7(4) . . ? C14 C15 N3 119.1(4) . . ? C15 C16 C11 118.5(4) . . ? C15 C16 H16 120.8 . . ? C11 C16 H16 120.8 . . ? C10 C17 H17A 109.5 . . ? C10 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C10 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C10 C18 H18A 109.5 . . ? C10 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C10 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N4 C19 N3 111.9(3) . . ? N4 C19 H19 124.0 . . ? N3 C19 H19 124.0 . . ? C21 C20 N4 109.4(4) . . ? C21 C20 H20 125.3 . . ? N4 C20 H20 125.3 . . ? C20 C21 N3 107.1(4) . . ? C20 C21 H21 126.5 . . ? N3 C21 H21 126.5 . . ? O1 C22 O2 124.6(4) . . ? O1 C22 C23 118.8(3) . . ? O2 C22 C23 116.5(3) . . ? C28 C23 C24 118.8(4) . . ? C28 C23 C22 120.4(3) . . ? C24 C23 C22 120.8(3) . . ? C25 C24 C23 120.0(4) . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C24 C25 C26 120.7(4) . . ? C24 C25 H25 119.7 . . ? C26 C25 H25 119.7 . . ? C27 C26 C25 119.4(4) . . ? C27 C26 C29 119.2(4) . . ? C25 C26 C29 121.4(4) . . ? C26 C27 C28 120.3(4) . . ? C26 C27 H27 119.8 . . ? C28 C27 H27 119.8 . . ? C27 C28 C23 120.7(4) . . ? C27 C28 H28 119.7 . . ? C23 C28 H28 119.7 . . ? O3 C29 O4 125.4(4) . . ? O3 C29 C26 119.1(4) . . ? O4 C29 C26 115.4(4) . . ? O5 C30 O6 125.9(3) . . ? O5 C30 C31 116.7(3) . . ? O6 C30 C31 117.4(3) . . ? C32 C31 C36 120.0(3) . . ? C32 C31 C30 119.8(3) . . ? C36 C31 C30 120.2(3) . . ? C33 C32 C31 120.9(4) . . ? C33 C32 H32 119.6 . . ? C31 C32 H32 119.6 . . ? C32 C33 C34 119.5(3) . . ? C32 C33 H33 120.2 . . ? C34 C33 H33 120.2 . . ? C35 C34 C33 119.4(3) . . ? C35 C34 C37 120.1(3) . 3_457 ? C33 C34 C37 120.5(3) . 3_457 ? C36 C35 C34 120.8(4) . . ? C36 C35 H35 119.6 . . ? C34 C35 H35 119.6 . . ? C35 C36 C31 119.4(4) . . ? C35 C36 H36 120.3 . . ? C31 C36 H36 120.3 . . ? O8 C37 O7 125.3(4) . . ? O8 C37 C34 118.6(4) . 3_557 ? O7 C37 C34 116.0(3) . 3_557 ? C3 N1 C1 105.2(3) . . ? C3 N1 Zn1 123.5(3) . . ? C1 N1 Zn1 131.2(3) . . ? C3 N2 C2 106.2(3) . . ? C3 N2 C4 125.4(3) . . ? C2 N2 C4 128.1(3) . . ? C19 N3 C21 106.1(3) . . ? C19 N3 C15 125.4(3) . . ? C21 N3 C15 128.4(3) . . ? C19 N4 C20 105.5(3) . . ? C19 N4 Zn3 130.1(3) . 8_556 ? C20 N4 Zn3 123.9(3) . 8_556 ? C22 O1 Zn1 143.6(3) . . ? C22 O2 Zn3 115.6(2) . . ? C29 O4 Zn3 120.2(2) . 6_658 ? C30 O5 Zn1 130.8(2) . . ? C30 O6 Zn2 130.6(2) . . ? C37 O7 Zn1 119.7(2) . . ? C37 O8 Zn2 139.6(3) . . ? Zn3 O9 Zn1 113.35(11) . . ? Zn3 O9 Zn2 120.24(11) . . ? Zn1 O9 Zn2 106.61(10) . . ? O7 Zn1 O9 119.67(11) . . ? O7 Zn1 N1 117.20(12) . . ? O9 Zn1 N1 122.97(11) . . ? O7 Zn1 O5 92.99(12) . . ? O9 Zn1 O5 90.50(10) . . ? N1 Zn1 O5 90.53(11) . . ? O7 Zn1 O1 87.61(11) . . ? O9 Zn1 O1 93.20(9) . . ? N1 Zn1 O1 85.11(11) . . ? O5 Zn1 O1 175.37(10) . . ? O6 Zn2 O6 180.000(1) 5_757 . ? O6 Zn2 O9 85.43(9) 5_757 . ? O6 Zn2 O9 94.57(9) . . ? O6 Zn2 O9 94.57(9) 5_757 5_757 ? O6 Zn2 O9 85.43(9) . 5_757 ? O9 Zn2 O9 180.000(1) . 5_757 ? O6 Zn2 O8 89.23(10) 5_757 5_757 ? O6 Zn2 O8 90.77(10) . 5_757 ? O9 Zn2 O8 86.03(10) . 5_757 ? O9 Zn2 O8 93.97(10) 5_757 5_757 ? O6 Zn2 O8 90.77(10) 5_757 . ? O6 Zn2 O8 89.23(10) . . ? O9 Zn2 O8 93.97(10) . . ? O9 Zn2 O8 86.03(10) 5_757 . ? O8 Zn2 O8 180.0 5_757 . ? O2 Zn3 O9 116.86(11) . . ? O2 Zn3 N4 108.34(12) . 8 ? O9 Zn3 N4 129.20(12) . 8 ? O2 Zn3 O4 99.10(12) . 6_558 ? O9 Zn3 O4 98.46(10) . 6_558 ? N4 Zn3 O4 96.08(12) 8 6_558 ? 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 N1 C1 C2 N2 -0.8(6) . . . . ? C9 C4 C5 C6 -0.1(7) . . . . ? N2 C4 C5 C6 177.8(4) . . . . ? C4 C5 C6 C7 1.4(7) . . . . ? C5 C6 C7 C8 -1.9(7) . . . . ? C5 C6 C7 C12 179.3(5) . . . . ? C6 C7 C8 C9 0.9(7) . . . . ? C12 C7 C8 C9 -179.9(4) . . . . ? C6 C7 C8 C10 -177.5(4) . . . . ? C12 C7 C8 C10 1.6(5) . . . . ? C7 C8 C9 C4 0.4(6) . . . . ? C10 C8 C9 C4 178.5(4) . . . . ? C5 C4 C9 C8 -0.8(6) . . . . ? N2 C4 C9 C8 -178.7(4) . . . . ? C9 C8 C10 C11 178.2(4) . . . . ? C7 C8 C10 C11 -3.6(4) . . . . ? C9 C8 C10 C18 57.4(6) . . . . ? C7 C8 C10 C18 -124.3(4) . . . . ? C9 C8 C10 C17 -65.8(5) . . . . ? C7 C8 C10 C17 112.5(4) . . . . ? C8 C10 C11 C16 -177.0(4) . . . . ? C18 C10 C11 C16 -55.9(6) . . . . ? C17 C10 C11 C16 66.7(6) . . . . ? C8 C10 C11 C12 4.4(4) . . . . ? C18 C10 C11 C12 125.4(4) . . . . ? C17 C10 C11 C12 -112.0(4) . . . . ? C16 C11 C12 C13 -3.3(6) . . . . ? C10 C11 C12 C13 175.5(4) . . . . ? C16 C11 C12 C7 177.6(4) . . . . ? C10 C11 C12 C7 -3.7(5) . . . . ? C6 C7 C12 C13 1.2(8) . . . . ? C8 C7 C12 C13 -177.8(5) . . . . ? C6 C7 C12 C11 -179.8(5) . . . . ? C8 C7 C12 C11 1.3(5) . . . . ? C11 C12 C13 C14 1.3(7) . . . . ? C7 C12 C13 C14 -179.8(4) . . . . ? C12 C13 C14 C15 0.8(7) . . . . ? C13 C14 C15 C16 -0.9(7) . . . . ? C13 C14 C15 N3 -179.6(4) . . . . ? C14 C15 C16 C11 -1.0(6) . . . . ? N3 C15 C16 C11 177.6(4) . . . . ? C12 C11 C16 C15 3.1(6) . . . . ? C10 C11 C16 C15 -175.4(4) . . . . ? N4 C20 C21 N3 -0.2(7) . . . . ? O1 C22 C23 C28 12.4(6) . . . . ? O2 C22 C23 C28 -164.3(4) . . . . ? O1 C22 C23 C24 -170.2(4) . . . . ? O2 C22 C23 C24 13.1(5) . . . . ? C28 C23 C24 C25 -1.8(6) . . . . ? C22 C23 C24 C25 -179.2(4) . . . . ? C23 C24 C25 C26 3.7(7) . . . . ? C24 C25 C26 C27 -1.9(6) . . . . ? C24 C25 C26 C29 -179.8(4) . . . . ? C25 C26 C27 C28 -1.6(6) . . . . ? C29 C26 C27 C28 176.3(4) . . . . ? C26 C27 C28 C23 3.5(6) . . . . ? C24 C23 C28 C27 -1.7(6) . . . . ? C22 C23 C28 C27 175.7(4) . . . . ? C27 C26 C29 O3 36.2(5) . . . . ? C25 C26 C29 O3 -145.9(4) . . . . ? C27 C26 C29 O4 -142.5(4) . . . . ? C25 C26 C29 O4 35.4(5) . . . . ? O5 C30 C31 C32 10.6(5) . . . . ? O6 C30 C31 C32 -168.3(3) . . . . ? O5 C30 C31 C36 -168.1(4) . . . . ? O6 C30 C31 C36 12.9(5) . . . . ? C36 C31 C32 C33 -0.7(6) . . . . ? C30 C31 C32 C33 -179.4(3) . . . . ? C31 C32 C33 C34 1.7(5) . . . . ? C32 C33 C34 C35 -1.1(5) . . . . ? C32 C33 C34 C37 176.7(3) . . . 3_457 ? C33 C34 C35 C36 -0.4(6) . . . . ? C37 C34 C35 C36 -178.2(3) 3_457 . . . ? C34 C35 C36 C31 1.4(6) . . . . ? C32 C31 C36 C35 -0.9(6) . . . . ? C30 C31 C36 C35 177.8(3) . . . . ? N2 C3 N1 C1 -1.0(5) . . . . ? N2 C3 N1 Zn1 -177.9(2) . . . . ? C2 C1 N1 C3 1.1(5) . . . . ? C2 C1 N1 Zn1 177.7(3) . . . . ? N1 C3 N2 C2 0.5(5) . . . . ? N1 C3 N2 C4 175.9(3) . . . . ? C1 C2 N2 C3 0.2(5) . . . . ? C1 C2 N2 C4 -175.0(4) . . . . ? C5 C4 N2 C3 -175.1(4) . . . . ? C9 C4 N2 C3 2.8(6) . . . . ? C5 C4 N2 C2 -0.7(7) . . . . ? C9 C4 N2 C2 177.2(4) . . . . ? N4 C19 N3 C21 0.3(5) . . . . ? N4 C19 N3 C15 -178.0(4) . . . . ? C20 C21 N3 C19 0.0(6) . . . . ? C20 C21 N3 C15 178.2(4) . . . . ? C16 C15 N3 C19 -30.1(6) . . . . ? C14 C15 N3 C19 148.6(4) . . . . ? C16 C15 N3 C21 151.9(5) . . . . ? C14 C15 N3 C21 -29.4(7) . . . . ? N3 C19 N4 C20 -0.4(5) . . . . ? N3 C19 N4 Zn3 171.3(3) . . . 8_556 ? C21 C20 N4 C19 0.4(6) . . . . ? C21 C20 N4 Zn3 -172.0(4) . . . 8_556 ? O2 C22 O1 Zn1 5.9(7) . . . . ? C23 C22 O1 Zn1 -170.6(3) . . . . ? O1 C22 O2 Zn3 -25.8(5) . . . . ? C23 C22 O2 Zn3 150.7(3) . . . . ? O3 C29 O4 Zn3 -2.6(5) . . . 6_658 ? C26 C29 O4 Zn3 176.0(2) . . . 6_658 ? O6 C30 O5 Zn1 7.5(6) . . . . ? C31 C30 O5 Zn1 -171.3(2) . . . . ? O5 C30 O6 Zn2 10.0(6) . . . . ? C31 C30 O6 Zn2 -171.2(2) . . . . ? O8 C37 O7 Zn1 -4.8(5) . . . . ? C34 C37 O7 Zn1 173.9(2) 3_557 . . . ? O7 C37 O8 Zn2 30.3(6) . . . . ? C34 C37 O8 Zn2 -148.3(3) 3_557 . . . ? C37 O7 Zn1 O9 9.5(3) . . . . ? C37 O7 Zn1 N1 -174.9(3) . . . . ? C37 O7 Zn1 O5 -82.8(3) . . . . ? C37 O7 Zn1 O1 101.8(3) . . . . ? Zn3 O9 Zn1 O7 105.38(14) . . . . ? Zn2 O9 Zn1 O7 -29.15(16) . . . . ? Zn3 O9 Zn1 N1 -69.94(17) . . . . ? Zn2 O9 Zn1 N1 155.53(12) . . . . ? Zn3 O9 Zn1 O5 -160.90(13) . . . . ? Zn2 O9 Zn1 O5 64.57(12) . . . . ? Zn3 O9 Zn1 O1 16.30(13) . . . . ? Zn2 O9 Zn1 O1 -118.22(11) . . . . ? C3 N1 Zn1 O7 -105.6(3) . . . . ? C1 N1 Zn1 O7 78.3(4) . . . . ? C3 N1 Zn1 O9 69.9(3) . . . . ? C1 N1 Zn1 O9 -106.2(4) . . . . ? C3 N1 Zn1 O5 160.8(3) . . . . ? C1 N1 Zn1 O5 -15.3(4) . . . . ? C3 N1 Zn1 O1 -20.8(3) . . . . ? C1 N1 Zn1 O1 163.1(4) . . . . ? C30 O5 Zn1 O7 72.9(3) . . . . ? C30 O5 Zn1 O9 -46.8(3) . . . . ? C30 O5 Zn1 N1 -169.8(3) . . . . ? C30 O5 Zn1 O1 170.2(12) . . . . ? C22 O1 Zn1 O7 -119.8(4) . . . . ? C22 O1 Zn1 O9 -0.2(4) . . . . ? C22 O1 Zn1 N1 122.6(4) . . . . ? C22 O1 Zn1 O5 142.6(12) . . . . ? C30 O6 Zn2 O6 -25(100) . . . 5_757 ? C30 O6 Zn2 O9 17.2(3) . . . . ? C30 O6 Zn2 O9 -162.8(3) . . . 5_757 ? C30 O6 Zn2 O8 103.3(3) . . . 5_757 ? C30 O6 Zn2 O8 -76.7(3) . . . . ? Zn3 O9 Zn2 O6 -7.66(14) . . . 5_757 ? Zn1 O9 Zn2 O6 123.09(12) . . . 5_757 ? Zn3 O9 Zn2 O6 172.34(14) . . . . ? Zn1 O9 Zn2 O6 -56.91(12) . . . . ? Zn3 O9 Zn2 O9 -178.6(2) . . . 5_757 ? Zn1 O9 Zn2 O9 -47.8(4) . . . 5_757 ? Zn3 O9 Zn2 O8 81.89(14) . . . 5_757 ? Zn1 O9 Zn2 O8 -147.36(12) . . . 5_757 ? Zn3 O9 Zn2 O8 -98.11(14) . . . . ? Zn1 O9 Zn2 O8 32.64(12) . . . . ? C37 O8 Zn2 O6 -132.0(4) . . . 5_757 ? C37 O8 Zn2 O6 48.0(4) . . . . ? C37 O8 Zn2 O9 -46.5(4) . . . . ? C37 O8 Zn2 O9 133.5(4) . . . 5_757 ? C37 O8 Zn2 O8 50.9(4) . . . 5_757 ? C22 O2 Zn3 O9 42.4(3) . . . . ? C22 O2 Zn3 N4 -161.5(3) . . . 8 ? C22 O2 Zn3 O4 -62.0(3) . . . 6_558 ? Zn1 O9 Zn3 O2 -36.20(16) . . . . ? Zn2 O9 Zn3 O2 91.54(15) . . . . ? Zn1 O9 Zn3 N4 173.57(13) . . . 8 ? Zn2 O9 Zn3 N4 -58.7(2) . . . 8 ? Zn1 O9 Zn3 O4 68.54(14) . . . 6_558 ? Zn2 O9 Zn3 O4 -163.72(14) . . . 6_558 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.12 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.783 _refine_diff_density_min -0.510 _refine_diff_density_rms 0.088 _database_code_depnum_ccdc_archive 'CCDC 972069' ####################################################################### # # 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_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C29 H26 N4 O6 Zn' _chemical_formula_sum 'C29 H26 N4 O6 Zn' _chemical_formula_weight 591.91 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M c2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 28.3903(12) _cell_length_b 13.8667(6) _cell_length_c 14.3593(6) _cell_angle_alpha 90.00 _cell_angle_beta 107.2540(10) _cell_angle_gamma 90.00 _cell_volume 5398.6(4) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5370 _cell_measurement_theta_min 1.61 _cell_measurement_theta_max 26.02 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.457 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2448 _exptl_absorpt_coefficient_mu 0.961 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.760 _exptl_absorpt_correction_T_max 0.792 _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 9.00cm _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 14786 _diffrn_reflns_av_R_equivalents 0.0230 _diffrn_reflns_av_sigmaI/netI 0.0272 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 26.12 _reflns_number_total 5370 _reflns_number_gt 4623 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXP-97 _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0478P)^2^+9.0991P] 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 5370 _refine_ls_number_parameters 370 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0412 _refine_ls_R_factor_gt 0.0340 _refine_ls_wR_factor_ref 0.0946 _refine_ls_wR_factor_gt 0.0906 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _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 C1 C 0.24795(8) 0.11228(18) 0.52519(17) 0.0295(5) Uani 1 1 d . . . H1 H 0.2734 0.1499 0.5164 0.035 Uiso 1 1 calc R . . C2 C 0.20173(9) 0.10824(19) 0.46345(18) 0.0335(6) Uani 1 1 d . . . H2 H 0.1895 0.1421 0.4053 0.040 Uiso 1 1 calc R . . C3 C 0.20768(8) 0.01153(16) 0.58790(16) 0.0221(5) Uani 1 1 d . . . H3 H 0.1997 -0.0329 0.6293 0.027 Uiso 1 1 calc R . . C4 C 0.12525(8) 0.01665(16) 0.46599(16) 0.0220(5) Uani 1 1 d . . . C5 C 0.11203(8) -0.07815(16) 0.47645(16) 0.0228(5) Uani 1 1 d . . . H5 H 0.1357 -0.1238 0.5061 0.027 Uiso 1 1 calc R . . C6 C 0.06285(8) -0.10308(15) 0.44188(15) 0.0208(4) Uani 1 1 d . . . C7 C 0.02700(8) -0.03386(15) 0.39878(16) 0.0217(5) Uani 1 1 d . . . C8 C 0.04103(8) 0.06059(16) 0.38897(17) 0.0245(5) Uani 1 1 d . . . H8 H 0.0174 0.1066 0.3600 0.029 Uiso 1 1 calc R . . C9 C 0.09043(8) 0.08623(16) 0.42242(17) 0.0254(5) Uani 1 1 d . . . H9 H 0.1001 0.1493 0.4158 0.030 Uiso 1 1 calc R . . C10 C 0.03971(8) -0.20189(15) 0.44230(16) 0.0224(5) Uani 1 1 d . . . C11 C -0.01452(8) -0.17744(16) 0.39946(16) 0.0215(4) Uani 1 1 d . . . C12 C -0.02151(8) -0.08037(16) 0.37230(16) 0.0213(4) Uani 1 1 d . . . C13 C -0.06872(8) -0.04454(16) 0.32878(17) 0.0237(5) Uani 1 1 d . . . H13 H -0.0734 0.0202 0.3116 0.028 Uiso 1 1 calc R . . C14 C -0.10872(8) -0.10654(16) 0.31130(16) 0.0243(5) Uani 1 1 d . . . H14 H -0.1405 -0.0840 0.2812 0.029 Uiso 1 1 calc R . . C15 C -0.10097(8) -0.20256(16) 0.33914(17) 0.0237(5) Uani 1 1 d . . . C16 C -0.05429(8) -0.23916(16) 0.38439(17) 0.0245(5) Uani 1 1 d . . . H16 H -0.0499 -0.3033 0.4040 0.029 Uiso 1 1 calc R . . C17 C 0.05558(8) -0.27152(17) 0.37412(18) 0.0298(5) Uani 1 1 d . . . H17A H 0.0899 -0.2868 0.4014 0.045 Uiso 1 1 calc R . . H17B H 0.0504 -0.2417 0.3115 0.045 Uiso 1 1 calc R . . H17C H 0.0364 -0.3296 0.3668 0.045 Uiso 1 1 calc R . . C18 C 0.05159(9) -0.24522(18) 0.54461(18) 0.0307(5) Uani 1 1 d . . . H18A H 0.0862 -0.2593 0.5684 0.046 Uiso 1 1 calc R . . H18B H 0.0331 -0.3036 0.5421 0.046 Uiso 1 1 calc R . . H18C H 0.0430 -0.2000 0.5875 0.046 Uiso 1 1 calc R . . C19 C -0.18777(8) -0.25455(17) 0.32920(18) 0.0282(5) Uani 1 1 d . . . H19 H -0.1993 -0.1991 0.3516 0.034 Uiso 1 1 calc R . . C20 C -0.21285(8) -0.33782(17) 0.30143(18) 0.0272(5) Uani 1 1 d . . . H20 H -0.2450 -0.3495 0.3020 0.033 Uiso 1 1 calc R . . C21 C -0.14106(8) -0.35782(16) 0.28316(18) 0.0275(5) Uani 1 1 d . . . H21 H -0.1141 -0.3850 0.2687 0.033 Uiso 1 1 calc R . . C22 C 0.26167(8) 0.11814(16) 0.85117(16) 0.0244(5) Uani 1 1 d . . . C23 C 0.25576(8) 0.18598(16) 0.92872(16) 0.0239(5) Uani 1 1 d . . . C24 C 0.20903(8) 0.20960(18) 0.93324(18) 0.0298(5) Uani 1 1 d . . . H24 H 0.1814 0.1828 0.8887 0.036 Uiso 1 1 calc R . . C25 C 0.29659(8) 0.22719(18) 0.99628(18) 0.0303(5) Uani 1 1 d . . . H25 H 0.3281 0.2119 0.9939 0.036 Uiso 1 1 calc R . . C26 C 0.39324(8) 0.13192(16) 0.70358(17) 0.0259(5) Uani 1 1 d . . . C27 C 0.44850(8) 0.12971(16) 0.72667(17) 0.0252(5) Uani 1 1 d . . . C28 C 0.47452(9) 0.04409(18) 0.7390(3) 0.0459(8) Uani 1 1 d . . . H28 H 0.4577 -0.0142 0.7325 0.055 Uiso 1 1 calc R . . C29 C 0.47463(8) 0.21532(16) 0.73822(16) 0.0229(5) Uani 1 1 d . . . H29 H 0.4577 0.2737 0.7300 0.027 Uiso 1 1 calc R . . N1 N 0.25156(6) 0.05201(13) 0.60320(14) 0.0216(4) Uani 1 1 d . . . N2 N 0.17628(7) 0.04388(13) 0.50377(14) 0.0226(4) Uani 1 1 d . . . N3 N -0.14188(7) -0.26826(13) 0.31778(14) 0.0243(4) Uani 1 1 d . . . N8 N -0.18338(7) -0.40251(13) 0.27228(15) 0.0247(4) Uani 1 1 d . . . O1 O 0.22967(6) 0.05985(12) 0.81220(12) 0.0308(4) Uani 1 1 d . . . O2 O 0.30261(6) 0.12800(12) 0.82954(12) 0.0311(4) Uani 1 1 d . . . O3 O 0.37055(6) 0.20796(13) 0.67805(14) 0.0370(4) Uani 1 1 d . . . O4 O 0.37319(6) 0.05172(12) 0.71276(15) 0.0365(4) Uani 1 1 d . . . OW1 O 0.33232(7) 0.32365(14) 0.79916(15) 0.0456(5) Uani 1 1 d . . . OW2 O 0.4570(5) 0.0221(4) 0.4765(7) 0.182(5) Uani 0.50 1 d P . . OW3 O 0.3842(4) -0.0043(7) 0.5005(6) 0.162(4) Uani 0.50 1 d P . . Zn1 Zn 0.306868(9) 0.039819(17) 0.726176(18) 0.02048(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0197(11) 0.0356(13) 0.0332(13) 0.0056(10) 0.0079(10) -0.0066(10) C2 0.0248(12) 0.0423(15) 0.0313(13) 0.0122(11) 0.0049(10) -0.0085(11) C3 0.0184(11) 0.0200(11) 0.0268(11) 0.0005(9) 0.0048(9) -0.0009(8) C4 0.0141(10) 0.0260(11) 0.0237(11) -0.0016(9) 0.0023(8) -0.0043(8) C5 0.0179(11) 0.0221(11) 0.0255(11) 0.0003(9) 0.0022(9) 0.0004(9) C6 0.0184(10) 0.0208(11) 0.0221(11) -0.0020(8) 0.0043(8) -0.0014(8) C7 0.0181(11) 0.0233(11) 0.0222(11) -0.0004(9) 0.0037(9) -0.0031(8) C8 0.0191(11) 0.0217(11) 0.0301(12) 0.0042(9) 0.0031(9) 0.0011(9) C9 0.0228(11) 0.0209(11) 0.0305(12) 0.0035(9) 0.0049(9) -0.0054(9) C10 0.0179(11) 0.0193(11) 0.0277(11) -0.0009(9) 0.0032(9) -0.0016(8) C11 0.0171(10) 0.0215(11) 0.0243(11) -0.0018(9) 0.0038(8) -0.0002(8) C12 0.0183(11) 0.0215(11) 0.0240(11) -0.0013(9) 0.0059(9) -0.0026(9) C13 0.0208(11) 0.0203(11) 0.0280(12) 0.0016(9) 0.0043(9) -0.0007(8) C14 0.0169(10) 0.0258(11) 0.0284(12) -0.0016(9) 0.0041(9) 0.0010(9) C15 0.0168(10) 0.0243(11) 0.0306(12) -0.0054(9) 0.0080(9) -0.0057(9) C16 0.0216(11) 0.0191(11) 0.0317(12) -0.0008(9) 0.0064(9) -0.0024(9) C17 0.0207(12) 0.0293(12) 0.0370(13) -0.0064(10) 0.0047(10) 0.0023(9) C18 0.0265(12) 0.0296(12) 0.0326(13) 0.0055(10) 0.0036(10) -0.0026(10) C19 0.0188(11) 0.0269(12) 0.0398(13) -0.0062(10) 0.0103(10) -0.0003(9) C20 0.0158(10) 0.0288(12) 0.0385(13) -0.0023(10) 0.0102(9) -0.0007(9) C21 0.0195(11) 0.0242(11) 0.0409(14) -0.0067(10) 0.0122(10) -0.0027(9) C22 0.0225(11) 0.0225(11) 0.0270(11) 0.0027(9) 0.0057(9) 0.0042(9) C23 0.0231(11) 0.0243(11) 0.0253(11) 0.0006(9) 0.0086(9) -0.0005(9) C24 0.0193(11) 0.0372(13) 0.0315(13) -0.0088(10) 0.0054(9) -0.0063(10) C25 0.0175(11) 0.0394(14) 0.0346(13) -0.0057(11) 0.0085(10) 0.0000(10) C26 0.0199(11) 0.0258(12) 0.0341(13) -0.0020(10) 0.0113(9) -0.0017(9) C27 0.0192(11) 0.0240(11) 0.0342(12) -0.0005(9) 0.0108(9) -0.0004(9) C28 0.0249(14) 0.0195(12) 0.099(3) -0.0029(13) 0.0277(15) -0.0041(10) C29 0.0209(11) 0.0188(10) 0.0283(12) 0.0023(9) 0.0064(9) 0.0028(9) N1 0.0152(9) 0.0215(9) 0.0274(10) -0.0010(7) 0.0051(7) -0.0012(7) N2 0.0156(9) 0.0250(10) 0.0254(10) 0.0013(8) 0.0031(7) -0.0040(7) N3 0.0165(9) 0.0213(9) 0.0349(11) -0.0039(8) 0.0074(8) -0.0028(7) N8 0.0164(9) 0.0219(10) 0.0354(11) -0.0027(8) 0.0070(8) -0.0027(7) O1 0.0278(9) 0.0295(9) 0.0334(9) -0.0064(7) 0.0063(7) -0.0055(7) O2 0.0238(8) 0.0346(9) 0.0376(10) -0.0117(8) 0.0132(7) -0.0024(7) O3 0.0223(9) 0.0325(9) 0.0559(12) 0.0117(8) 0.0111(8) 0.0043(7) O4 0.0199(8) 0.0258(9) 0.0676(13) -0.0025(8) 0.0188(8) -0.0027(7) OW1 0.0343(10) 0.0443(11) 0.0519(12) -0.0021(9) 0.0033(9) 0.0035(9) OW2 0.358(16) 0.036(3) 0.130(7) -0.017(4) 0.037(9) 0.002(6) OW3 0.215(11) 0.156(8) 0.074(5) -0.032(5) -0.021(6) 0.050(8) Zn1 0.01253(13) 0.01887(14) 0.02892(15) -0.00185(10) 0.00441(10) 0.00074(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 C1 C2 1.349(3) . ? C1 N1 1.377(3) . ? C1 H1 0.9300 . ? C2 N2 1.379(3) . ? C2 H2 0.9300 . ? C3 N1 1.324(3) . ? C3 N2 1.348(3) . ? C3 H3 0.9300 . ? C4 C5 1.387(3) . ? C4 C9 1.390(3) . ? C4 N2 1.438(3) . ? C5 C6 1.380(3) . ? C5 H5 0.9300 . ? C6 C7 1.402(3) . ? C6 C10 1.520(3) . ? C7 C8 1.388(3) . ? C7 C12 1.465(3) . ? C8 C9 1.387(3) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 C11 1.517(3) . ? C10 C18 1.529(3) . ? C10 C17 1.535(3) . ? C11 C16 1.382(3) . ? C11 C12 1.399(3) . ? C12 C13 1.392(3) . ? C13 C14 1.387(3) . ? C13 H13 0.9300 . ? C14 C15 1.389(3) . ? C14 H14 0.9300 . ? C15 C16 1.388(3) . ? C15 N3 1.436(3) . ? C16 H16 0.9300 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C20 1.353(3) . ? C19 N3 1.374(3) . ? C19 H19 0.9300 . ? C20 N8 1.374(3) . ? C20 H20 0.9300 . ? C21 N8 1.319(3) . ? C21 N3 1.340(3) . ? C21 H21 0.9300 . ? C22 O1 1.221(3) . ? C22 O2 1.296(3) . ? C22 C23 1.505(3) . ? C23 C24 1.386(3) . ? C23 C25 1.394(3) . ? C24 C25 1.383(3) 7_557 ? C24 H24 0.9300 . ? C25 C24 1.383(3) 7_557 ? C25 H25 0.9300 . ? C26 O3 1.233(3) . ? C26 O4 1.274(3) . ? C26 C27 1.504(3) . ? C27 C28 1.382(3) . ? C27 C29 1.384(3) . ? C28 C28 1.387(5) 2_656 ? C28 H28 0.9300 . ? C29 C29 1.379(4) 2_656 ? C29 H29 0.9300 . ? N1 Zn1 1.9919(18) . ? N8 Zn1 2.0078(19) 8_445 ? O2 Zn1 1.9543(16) . ? O4 Zn1 1.9557(17) . ? Zn1 N8 2.0078(19) 8_546 ? 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 C2 C1 N1 109.4(2) . . ? C2 C1 H1 125.3 . . ? N1 C1 H1 125.3 . . ? C1 C2 N2 106.2(2) . . ? C1 C2 H2 126.9 . . ? N2 C2 H2 126.9 . . ? N1 C3 N2 110.32(19) . . ? N1 C3 H3 124.8 . . ? N2 C3 H3 124.8 . . ? C5 C4 C9 121.8(2) . . ? C5 C4 N2 118.85(19) . . ? C9 C4 N2 119.32(19) . . ? C6 C5 C4 118.4(2) . . ? C6 C5 H5 120.8 . . ? C4 C5 H5 120.8 . . ? C5 C6 C7 120.8(2) . . ? C5 C6 C10 128.1(2) . . ? C7 C6 C10 111.14(18) . . ? C8 C7 C6 119.9(2) . . ? C8 C7 C12 131.7(2) . . ? C6 C7 C12 108.45(18) . . ? C9 C8 C7 119.8(2) . . ? C9 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? C8 C9 C4 119.3(2) . . ? C8 C9 H9 120.4 . . ? C4 C9 H9 120.4 . . ? C11 C10 C6 100.65(17) . . ? C11 C10 C18 112.68(19) . . ? C6 C10 C18 112.67(18) . . ? C11 C10 C17 109.67(18) . . ? C6 C10 C17 110.82(19) . . ? C18 C10 C17 110.04(19) . . ? C16 C11 C12 120.7(2) . . ? C16 C11 C10 127.5(2) . . ? C12 C11 C10 111.78(18) . . ? C13 C12 C11 120.46(19) . . ? C13 C12 C7 131.7(2) . . ? C11 C12 C7 107.85(18) . . ? C14 C13 C12 119.2(2) . . ? C14 C13 H13 120.4 . . ? C12 C13 H13 120.4 . . ? C13 C14 C15 119.4(2) . . ? C13 C14 H14 120.3 . . ? C15 C14 H14 120.3 . . ? C16 C15 C14 122.2(2) . . ? C16 C15 N3 117.9(2) . . ? C14 C15 N3 119.9(2) . . ? C11 C16 C15 118.0(2) . . ? C11 C16 H16 121.0 . . ? C15 C16 H16 121.0 . . ? C10 C17 H17A 109.5 . . ? C10 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C10 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C10 C18 H18A 109.5 . . ? C10 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C10 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 N3 106.4(2) . . ? C20 C19 H19 126.8 . . ? N3 C19 H19 126.8 . . ? C19 C20 N8 109.4(2) . . ? C19 C20 H20 125.3 . . ? N8 C20 H20 125.3 . . ? N8 C21 N3 111.3(2) . . ? N8 C21 H21 124.3 . . ? N3 C21 H21 124.3 . . ? O1 C22 O2 123.9(2) . . ? O1 C22 C23 121.5(2) . . ? O2 C22 C23 114.59(19) . . ? C24 C23 C25 118.7(2) . . ? C24 C23 C22 120.1(2) . . ? C25 C23 C22 121.2(2) . . ? C25 C24 C23 120.2(2) 7_557 . ? C25 C24 H24 119.9 7_557 . ? C23 C24 H24 119.9 . . ? C24 C25 C23 121.1(2) 7_557 . ? C24 C25 H25 119.5 7_557 . ? C23 C25 H25 119.5 . . ? O3 C26 O4 124.5(2) . . ? O3 C26 C27 120.1(2) . . ? O4 C26 C27 115.4(2) . . ? C28 C27 C29 118.3(2) . . ? C28 C27 C26 121.9(2) . . ? C29 C27 C26 119.7(2) . . ? C27 C28 C28 120.75(14) . 2_656 ? C27 C28 H28 119.6 . . ? C28 C28 H28 119.6 2_656 . ? C29 C29 C27 120.90(13) 2_656 . ? C29 C29 H29 119.6 2_656 . ? C27 C29 H29 119.6 . . ? C3 N1 C1 106.44(18) . . ? C3 N1 Zn1 124.51(15) . . ? C1 N1 Zn1 128.44(15) . . ? C3 N2 C2 107.58(19) . . ? C3 N2 C4 125.11(19) . . ? C2 N2 C4 127.29(19) . . ? C21 N3 C19 107.09(18) . . ? C21 N3 C15 124.41(19) . . ? C19 N3 C15 128.49(19) . . ? C21 N8 C20 105.82(19) . . ? C21 N8 Zn1 121.08(15) . 8_445 ? C20 N8 Zn1 133.05(15) . 8_445 ? C22 O2 Zn1 112.20(14) . . ? C26 O4 Zn1 123.83(15) . . ? O2 Zn1 O4 107.48(7) . . ? O2 Zn1 N1 114.21(7) . . ? O4 Zn1 N1 115.74(8) . . ? O2 Zn1 N8 112.12(8) . 8_546 ? O4 Zn1 N8 94.00(7) . 8_546 ? N1 Zn1 N8 111.60(8) . 8_546 ? 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 N1 C1 C2 N2 -0.3(3) . . . . ? C9 C4 C5 C6 0.3(3) . . . . ? N2 C4 C5 C6 178.6(2) . . . . ? C4 C5 C6 C7 -1.1(3) . . . . ? C4 C5 C6 C10 178.1(2) . . . . ? C5 C6 C7 C8 1.2(3) . . . . ? C10 C6 C7 C8 -178.2(2) . . . . ? C5 C6 C7 C12 -178.2(2) . . . . ? C10 C6 C7 C12 2.4(3) . . . . ? C6 C7 C8 C9 -0.4(3) . . . . ? C12 C7 C8 C9 178.8(2) . . . . ? C7 C8 C9 C4 -0.4(4) . . . . ? C5 C4 C9 C8 0.4(4) . . . . ? N2 C4 C9 C8 -177.8(2) . . . . ? C5 C6 C10 C11 177.2(2) . . . . ? C7 C6 C10 C11 -3.5(2) . . . . ? C5 C6 C10 C18 56.9(3) . . . . ? C7 C6 C10 C18 -123.8(2) . . . . ? C5 C6 C10 C17 -66.9(3) . . . . ? C7 C6 C10 C17 112.5(2) . . . . ? C6 C10 C11 C16 -178.0(2) . . . . ? C18 C10 C11 C16 -57.8(3) . . . . ? C17 C10 C11 C16 65.2(3) . . . . ? C6 C10 C11 C12 3.5(2) . . . . ? C18 C10 C11 C12 123.7(2) . . . . ? C17 C10 C11 C12 -113.4(2) . . . . ? C16 C11 C12 C13 -0.6(3) . . . . ? C10 C11 C12 C13 178.1(2) . . . . ? C16 C11 C12 C7 179.1(2) . . . . ? C10 C11 C12 C7 -2.2(3) . . . . ? C8 C7 C12 C13 0.2(4) . . . . ? C6 C7 C12 C13 179.5(2) . . . . ? C8 C7 C12 C11 -179.4(2) . . . . ? C6 C7 C12 C11 -0.1(2) . . . . ? C11 C12 C13 C14 -0.9(3) . . . . ? C7 C12 C13 C14 179.5(2) . . . . ? C12 C13 C14 C15 1.2(3) . . . . ? C13 C14 C15 C16 0.1(4) . . . . ? C13 C14 C15 N3 -177.4(2) . . . . ? C12 C11 C16 C15 1.8(3) . . . . ? C10 C11 C16 C15 -176.6(2) . . . . ? C14 C15 C16 C11 -1.6(3) . . . . ? N3 C15 C16 C11 176.0(2) . . . . ? N3 C19 C20 N8 -0.5(3) . . . . ? O1 C22 C23 C24 -23.8(3) . . . . ? O2 C22 C23 C24 155.5(2) . . . . ? O1 C22 C23 C25 157.1(2) . . . . ? O2 C22 C23 C25 -23.7(3) . . . . ? C25 C23 C24 C25 0.0(4) . . . 7_557 ? C22 C23 C24 C25 -179.3(2) . . . 7_557 ? C24 C23 C25 C24 0.0(4) . . . 7_557 ? C22 C23 C25 C24 179.2(2) . . . 7_557 ? O3 C26 C27 C28 -168.6(3) . . . . ? O4 C26 C27 C28 11.6(4) . . . . ? O3 C26 C27 C29 12.8(4) . . . . ? O4 C26 C27 C29 -167.0(2) . . . . ? C29 C27 C28 C28 -1.0(6) . . . 2_656 ? C26 C27 C28 C28 -179.5(4) . . . 2_656 ? C28 C27 C29 C29 -0.2(4) . . . 2_656 ? C26 C27 C29 C29 178.4(3) . . . 2_656 ? N2 C3 N1 C1 -0.3(2) . . . . ? N2 C3 N1 Zn1 171.40(14) . . . . ? C2 C1 N1 C3 0.4(3) . . . . ? C2 C1 N1 Zn1 -170.92(18) . . . . ? N1 C3 N2 C2 0.2(3) . . . . ? N1 C3 N2 C4 -178.4(2) . . . . ? C1 C2 N2 C3 0.1(3) . . . . ? C1 C2 N2 C4 178.6(2) . . . . ? C5 C4 N2 C3 -38.4(3) . . . . ? C9 C4 N2 C3 139.9(2) . . . . ? C5 C4 N2 C2 143.3(2) . . . . ? C9 C4 N2 C2 -38.4(3) . . . . ? N8 C21 N3 C19 -0.4(3) . . . . ? N8 C21 N3 C15 178.7(2) . . . . ? C20 C19 N3 C21 0.5(3) . . . . ? C20 C19 N3 C15 -178.5(2) . . . . ? C16 C15 N3 C21 -41.2(3) . . . . ? C14 C15 N3 C21 136.5(2) . . . . ? C16 C15 N3 C19 137.7(2) . . . . ? C14 C15 N3 C19 -44.6(3) . . . . ? N3 C21 N8 C20 0.1(3) . . . . ? N3 C21 N8 Zn1 -177.77(15) . . . 8_445 ? C19 C20 N8 C21 0.2(3) . . . . ? C19 C20 N8 Zn1 177.75(17) . . . 8_445 ? O1 C22 O2 Zn1 0.7(3) . . . . ? C23 C22 O2 Zn1 -178.56(14) . . . . ? O3 C26 O4 Zn1 -18.8(4) . . . . ? C27 C26 O4 Zn1 160.96(16) . . . . ? C22 O2 Zn1 O4 -173.20(15) . . . . ? C22 O2 Zn1 N1 56.94(17) . . . . ? C22 O2 Zn1 N8 -71.26(16) . . . 8_546 ? C26 O4 Zn1 O2 -50.4(2) . . . . ? C26 O4 Zn1 N1 78.5(2) . . . . ? C26 O4 Zn1 N8 -165.1(2) . . . 8_546 ? C3 N1 Zn1 O2 -81.72(19) . . . . ? C1 N1 Zn1 O2 88.1(2) . . . . ? C3 N1 Zn1 O4 152.66(17) . . . . ? C1 N1 Zn1 O4 -37.5(2) . . . . ? C3 N1 Zn1 N8 46.74(19) . . . 8_546 ? C1 N1 Zn1 N8 -143.41(19) . . . 8_546 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.12 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.819 _refine_diff_density_min -0.326 _refine_diff_density_rms 0.064 _database_code_depnum_ccdc_archive 'CCDC 972070' ####################################################################### # # 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_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C29 H28 Cd N4 O7' _chemical_formula_sum 'C29 H28 Cd N4 O7' _chemical_formula_weight 656.95 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 9.9705(6) _cell_length_b 10.7624(7) _cell_length_c 15.0951(14) _cell_angle_alpha 104.6840(10) _cell_angle_beta 95.0970(10) _cell_angle_gamma 111.9480(10) _cell_volume 1422.58(18) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5462 _cell_measurement_theta_min 1.61 _cell_measurement_theta_max 26.02 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.534 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 668 _exptl_absorpt_coefficient_mu 0.821 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.799 _exptl_absorpt_correction_T_max 0.841 _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 9.00cm _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 7841 _diffrn_reflns_av_R_equivalents 0.0223 _diffrn_reflns_av_sigmaI/netI 0.0507 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 25.93 _reflns_number_total 5462 _reflns_number_gt 4599 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXP-97 _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0604P)^2^+0.7302P] 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 5462 _refine_ls_number_parameters 368 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0524 _refine_ls_R_factor_gt 0.0398 _refine_ls_wR_factor_ref 0.1135 _refine_ls_wR_factor_gt 0.1002 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _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 C1 C 0.8288(5) -0.0858(4) 0.2568(3) 0.0295(9) Uani 1 1 d . . . H1 H 0.8261 -0.0525 0.2058 0.035 Uiso 1 1 calc R . . C2 C 0.8469(5) -0.0980(5) 0.3963(3) 0.0326(10) Uani 1 1 d . . . H2 H 0.8599 -0.0731 0.4612 0.039 Uiso 1 1 calc R . . C3 C 0.8220(5) -0.2268(5) 0.3398(3) 0.0371(11) Uani 1 1 d . . . H3 H 0.8137 -0.3055 0.3576 0.045 Uiso 1 1 calc R . . C4 C 0.7784(5) -0.3256(4) 0.1630(3) 0.0309(9) Uani 1 1 d . . . C5 C 0.6683(5) -0.4589(5) 0.1470(3) 0.0326(10) Uani 1 1 d . . . H5 H 0.6227 -0.4819 0.1952 0.039 Uiso 1 1 calc R . . C6 C 0.6262(5) -0.5581(4) 0.0591(3) 0.0313(10) Uani 1 1 d . . . H6 H 0.5524 -0.6477 0.0478 0.038 Uiso 1 1 calc R . . C7 C 0.6962(5) -0.5212(4) -0.0120(3) 0.0274(9) Uani 1 1 d . . . C8 C 0.8097(5) -0.3886(4) 0.0054(3) 0.0276(9) Uani 1 1 d . . . C9 C 0.8532(5) -0.2898(4) 0.0935(3) 0.0324(10) Uani 1 1 d . . . H9 H 0.9304 -0.2018 0.1058 0.039 Uiso 1 1 calc R . . C10 C 0.8710(5) -0.3719(4) -0.0814(3) 0.0322(10) Uani 1 1 d . . . C11 C 0.8587(7) -0.2478(5) -0.1080(4) 0.0531(15) Uani 1 1 d . . . H11A H 0.8985 -0.2405 -0.1630 0.080 Uiso 1 1 calc R . . H11B H 0.9132 -0.1622 -0.0574 0.080 Uiso 1 1 calc R . . H11C H 0.7568 -0.2628 -0.1203 0.080 Uiso 1 1 calc R . . C12 C 1.0322(5) -0.3562(6) -0.0704(4) 0.0489(13) Uani 1 1 d . . . H12A H 1.0670 -0.3458 -0.1265 0.073 Uiso 1 1 calc R . . H12B H 1.0373 -0.4385 -0.0593 0.073 Uiso 1 1 calc R . . H12C H 1.0929 -0.2745 -0.0185 0.073 Uiso 1 1 calc R . . C13 C 0.7680(4) 0.4880(4) 0.8472(3) 0.0267(9) Uani 1 1 d . . . C14 C 0.7657(4) 0.4457(4) 0.7519(3) 0.0288(9) Uani 1 1 d . . . H14 H 0.8328 0.5031 0.7249 0.035 Uiso 1 1 calc R . . C15 C 0.6586(5) 0.3136(5) 0.6987(3) 0.0300(9) Uani 1 1 d . . . C16 C 0.5579(5) 0.2271(5) 0.7387(3) 0.0336(10) Uani 1 1 d . . . H16 H 0.4867 0.1399 0.7014 0.040 Uiso 1 1 calc R . . C17 C 0.5633(5) 0.2702(4) 0.8335(3) 0.0336(10) Uani 1 1 d . . . H17 H 0.4972 0.2122 0.8608 0.040 Uiso 1 1 calc R . . C18 C 0.6690(5) -0.5981(4) -0.1124(3) 0.0289(9) Uani 1 1 d . . . C19 C 0.5318(5) 0.1961(5) 0.5294(3) 0.0353(10) Uani 1 1 d . . . H19 H 0.4336 0.1679 0.5351 0.042 Uiso 1 1 calc R . . C20 C 0.5828(5) 0.1751(5) 0.4491(3) 0.0347(10) Uani 1 1 d . . . H20 H 0.5241 0.1295 0.3893 0.042 Uiso 1 1 calc R . . C21 C 0.7741(5) 0.2870(5) 0.5607(3) 0.0332(10) Uani 1 1 d . . . H21 H 0.8716 0.3338 0.5935 0.040 Uiso 1 1 calc R . . C22 C 0.6658(5) 0.1684(4) 0.1888(3) 0.0284(9) Uani 1 1 d . . . C23 C 0.5796(4) 0.0806(4) 0.0907(3) 0.0260(9) Uani 1 1 d . . . C24 C 0.4418(5) 0.0760(4) 0.0604(3) 0.0292(9) Uani 1 1 d . . . H24 H 0.4023 0.1272 0.1009 0.035 Uiso 1 1 calc R . . C25 C 1.4387(4) 0.4267(5) 0.4061(3) 0.0305(9) Uani 1 1 d . . . H25 H 1.3978 0.3776 0.3431 0.037 Uiso 1 1 calc R . . C26 C 1.3464(4) 0.4311(4) 0.4700(3) 0.0263(9) Uani 1 1 d . . . C27 C 1.4101(4) 0.5055(5) 0.5643(3) 0.0310(10) Uani 1 1 d . . . H27 H 1.3498 0.5093 0.6076 0.037 Uiso 1 1 calc R . . C28 C 0.6372(5) 0.0041(4) 0.0293(3) 0.0292(9) Uani 1 1 d . . . H28 H 0.7297 0.0068 0.0488 0.035 Uiso 1 1 calc R . . C29 C 1.1819(4) 0.3554(4) 0.4368(3) 0.0252(9) Uani 1 1 d . . . N1 N 0.8502(4) -0.0086(4) 0.3447(2) 0.0294(8) Uani 1 1 d . . . N2 N 0.8114(4) -0.2179(4) 0.2503(2) 0.0307(8) Uani 1 1 d . . . N3 N 0.6551(4) 0.2677(4) 0.6009(2) 0.0296(8) Uani 1 1 d . . . N4 N 0.7344(4) 0.2314(4) 0.4695(2) 0.0293(8) Uani 1 1 d . . . O1 O 0.6299(4) 0.2611(4) 0.2334(2) 0.0441(8) Uani 1 1 d . . . O2 O 0.7720(3) 0.1425(3) 0.2178(2) 0.0361(7) Uani 1 1 d . . . O1W O 0.8964(3) 0.4407(3) 0.3482(2) 0.0333(7) Uani 1 1 d . . . O3 O 1.0995(3) 0.3642(3) 0.4947(2) 0.0304(7) Uani 1 1 d . . . O2W O 0.8552(8) 0.9661(8) 0.7939(5) 0.0529(18) Uiso 0.50 1 d P . . O4 O 1.1303(3) 0.2850(3) 0.3519(2) 0.0315(7) Uani 1 1 d . . . O3W O 0.7562(9) 1.0097(9) 0.7606(6) 0.066(2) Uiso 0.50 1 d P . . O4W O 0.7922(9) 1.0383(9) 0.6720(6) 0.065(2) Uiso 0.50 1 d P . . O5W O 0.7815(12) 0.9376(12) 0.6218(8) 0.098(3) Uiso 0.50 1 d P . . Cd1 Cd 0.88592(3) 0.22381(3) 0.367944(19) 0.02373(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.038(2) 0.027(2) 0.021(2) 0.0071(17) 0.0063(18) 0.0113(19) C2 0.032(2) 0.042(3) 0.021(2) 0.0114(19) 0.0056(17) 0.010(2) C3 0.043(3) 0.035(3) 0.030(2) 0.016(2) 0.006(2) 0.009(2) C4 0.039(2) 0.027(2) 0.027(2) 0.0078(18) 0.0086(19) 0.0142(19) C5 0.037(2) 0.033(2) 0.030(2) 0.0117(19) 0.0129(19) 0.014(2) C6 0.036(2) 0.025(2) 0.035(2) 0.0105(19) 0.0154(19) 0.0118(19) C7 0.029(2) 0.025(2) 0.032(2) 0.0083(18) 0.0108(18) 0.0141(18) C8 0.032(2) 0.024(2) 0.030(2) 0.0110(18) 0.0112(18) 0.0115(18) C9 0.039(2) 0.023(2) 0.031(2) 0.0087(18) 0.0101(19) 0.0072(19) C10 0.036(2) 0.027(2) 0.028(2) 0.0088(18) 0.0115(19) 0.0060(19) C11 0.089(4) 0.032(3) 0.041(3) 0.015(2) 0.028(3) 0.021(3) C12 0.032(3) 0.061(3) 0.038(3) 0.009(2) 0.012(2) 0.004(2) C13 0.029(2) 0.026(2) 0.029(2) 0.0094(18) 0.0110(18) 0.0132(18) C14 0.026(2) 0.031(2) 0.032(2) 0.0122(19) 0.0120(18) 0.0108(18) C15 0.029(2) 0.036(2) 0.026(2) 0.0070(19) 0.0095(18) 0.0143(19) C16 0.033(2) 0.031(2) 0.031(2) 0.0021(19) 0.0123(19) 0.0098(19) C17 0.030(2) 0.026(2) 0.038(3) 0.0089(19) 0.0160(19) 0.0042(18) C18 0.028(2) 0.028(2) 0.033(2) 0.0094(19) 0.0108(18) 0.0130(18) C19 0.023(2) 0.040(3) 0.038(3) 0.007(2) 0.0057(18) 0.0105(19) C20 0.029(2) 0.037(2) 0.030(2) 0.007(2) 0.0058(18) 0.0079(19) C21 0.023(2) 0.044(3) 0.028(2) 0.007(2) 0.0072(17) 0.0123(19) C22 0.028(2) 0.028(2) 0.022(2) 0.0068(17) -0.0011(17) 0.0060(18) C23 0.026(2) 0.023(2) 0.023(2) 0.0069(17) 0.0005(16) 0.0055(17) C24 0.029(2) 0.031(2) 0.026(2) 0.0074(18) 0.0026(17) 0.0113(18) C25 0.027(2) 0.036(2) 0.025(2) 0.0098(18) 0.0007(17) 0.0102(19) C26 0.0192(19) 0.031(2) 0.030(2) 0.0154(18) 0.0019(16) 0.0086(17) C27 0.023(2) 0.039(2) 0.028(2) 0.0122(19) 0.0056(17) 0.0074(18) C28 0.025(2) 0.032(2) 0.027(2) 0.0093(18) -0.0021(17) 0.0094(18) C29 0.0189(19) 0.024(2) 0.033(2) 0.0130(18) 0.0012(17) 0.0069(16) N1 0.0304(19) 0.0312(19) 0.0225(18) 0.0082(15) 0.0075(15) 0.0078(16) N2 0.039(2) 0.0283(19) 0.0209(18) 0.0083(15) 0.0064(15) 0.0092(16) N3 0.0257(18) 0.0326(19) 0.0268(19) 0.0053(15) 0.0079(15) 0.0100(15) N4 0.0234(18) 0.0322(19) 0.0276(19) 0.0052(16) 0.0056(14) 0.0089(15) O1 0.0418(19) 0.050(2) 0.0297(17) -0.0067(15) -0.0081(14) 0.0231(16) O2 0.0409(18) 0.0380(18) 0.0248(15) 0.0008(13) -0.0111(13) 0.0209(15) O1W 0.0322(16) 0.0294(16) 0.0330(17) 0.0079(13) 0.0005(13) 0.0097(13) O3 0.0192(14) 0.0360(17) 0.0286(16) 0.0069(13) 0.0010(12) 0.0063(12) O4 0.0202(14) 0.0393(17) 0.0267(16) 0.0063(13) 0.0005(12) 0.0068(13) Cd1 0.01828(16) 0.02790(18) 0.01934(17) 0.00289(12) 0.00145(11) 0.00685(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.325(5) . ? C1 N2 1.343(5) . ? C1 H1 0.9300 . ? C2 C3 1.348(6) . ? C2 N1 1.377(6) . ? C2 H2 0.9300 . ? C3 N2 1.376(5) . ? C3 H3 0.9300 . ? C4 C5 1.386(6) . ? C4 C9 1.391(6) . ? C4 N2 1.432(5) . ? C5 C6 1.387(6) . ? C5 H5 0.9300 . ? C6 C7 1.392(6) . ? C6 H6 0.9300 . ? C7 C8 1.391(6) . ? C7 C18 1.475(6) . ? C8 C9 1.387(6) . ? C8 C10 1.516(6) . ? C9 H9 0.9300 . ? C10 C13 1.521(6) 1_544 ? C10 C11 1.532(7) . ? C10 C12 1.542(6) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C18 1.383(6) 1_566 ? C13 C14 1.389(6) . ? C13 C10 1.521(6) 1_566 ? C14 C15 1.393(6) . ? C14 H14 0.9300 . ? C15 C16 1.392(6) . ? C15 N3 1.426(5) . ? C16 C17 1.376(6) . ? C16 H16 0.9300 . ? C17 C18 1.389(6) 1_566 ? C17 H17 0.9300 . ? C18 C13 1.383(6) 1_544 ? C18 C17 1.389(6) 1_544 ? C19 C20 1.354(6) . ? C19 N3 1.380(5) . ? C19 H19 0.9300 . ? C20 N4 1.373(5) . ? C20 H20 0.9300 . ? C21 N4 1.311(5) . ? C21 N3 1.352(5) . ? C21 H21 0.9300 . ? C22 O1 1.243(5) . ? C22 O2 1.261(5) . ? C22 C23 1.511(5) . ? C23 C28 1.388(6) . ? C23 C24 1.388(6) . ? C24 C28 1.382(6) 2_655 ? C24 H24 0.9300 . ? C25 C27 1.377(6) 2_866 ? C25 C26 1.395(6) . ? C25 H25 0.9300 . ? C26 C27 1.397(6) . ? C26 C29 1.501(5) . ? C27 C25 1.377(6) 2_866 ? C27 H27 0.9300 . ? C28 C24 1.382(6) 2_655 ? C28 H28 0.9300 . ? C29 O4 1.258(5) . ? C29 O3 1.262(5) . ? C29 Cd1 2.717(4) . ? N1 Cd1 2.318(4) . ? N4 Cd1 2.253(3) . ? O2 Cd1 2.233(3) . ? O1W Cd1 2.393(3) . ? O3 Cd1 2.426(3) . ? O2W O3W 1.351(11) . ? O4 Cd1 2.327(3) . ? O3W O4W 1.491(11) . ? O4W O5W 1.115(12) . ? 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 C1 N2 111.8(4) . . ? N1 C1 H1 124.1 . . ? N2 C1 H1 124.1 . . ? C3 C2 N1 110.6(4) . . ? C3 C2 H2 124.7 . . ? N1 C2 H2 124.7 . . ? C2 C3 N2 105.9(4) . . ? C2 C3 H3 127.0 . . ? N2 C3 H3 127.0 . . ? C5 C4 C9 121.3(4) . . ? C5 C4 N2 120.4(4) . . ? C9 C4 N2 118.1(4) . . ? C4 C5 C6 120.1(4) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C5 C6 C7 118.9(4) . . ? C5 C6 H6 120.5 . . ? C7 C6 H6 120.5 . . ? C8 C7 C6 120.6(4) . . ? C8 C7 C18 107.9(4) . . ? C6 C7 C18 131.5(4) . . ? C9 C8 C7 120.5(4) . . ? C9 C8 C10 127.7(4) . . ? C7 C8 C10 111.7(4) . . ? C8 C9 C4 118.4(4) . . ? C8 C9 H9 120.8 . . ? C4 C9 H9 120.8 . . ? C8 C10 C13 100.3(3) . 1_544 ? C8 C10 C11 111.9(4) . . ? C13 C10 C11 111.4(4) 1_544 . ? C8 C10 C12 112.0(4) . . ? C13 C10 C12 110.9(4) 1_544 . ? C11 C10 C12 110.1(4) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C18 C13 C14 121.4(4) 1_566 . ? C18 C13 C10 111.8(4) 1_566 1_566 ? C14 C13 C10 126.8(4) . 1_566 ? C13 C14 C15 117.2(4) . . ? C13 C14 H14 121.4 . . ? C15 C14 H14 121.4 . . ? C16 C15 C14 121.7(4) . . ? C16 C15 N3 120.2(4) . . ? C14 C15 N3 118.1(4) . . ? C17 C16 C15 120.2(4) . . ? C17 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C16 C17 C18 118.9(4) . 1_566 ? C16 C17 H17 120.5 . . ? C18 C17 H17 120.5 1_566 . ? C13 C18 C17 120.6(4) 1_544 1_544 ? C13 C18 C7 108.1(4) 1_544 . ? C17 C18 C7 131.2(4) 1_544 . ? C20 C19 N3 106.1(4) . . ? C20 C19 H19 127.0 . . ? N3 C19 H19 127.0 . . ? C19 C20 N4 109.6(4) . . ? C19 C20 H20 125.2 . . ? N4 C20 H20 125.2 . . ? N4 C21 N3 111.2(4) . . ? N4 C21 H21 124.4 . . ? N3 C21 H21 124.4 . . ? O1 C22 O2 125.4(4) . . ? O1 C22 C23 118.5(4) . . ? O2 C22 C23 116.1(4) . . ? C28 C23 C24 119.0(4) . . ? C28 C23 C22 120.6(4) . . ? C24 C23 C22 120.3(4) . . ? C28 C24 C23 120.4(4) 2_655 . ? C28 C24 H24 119.8 2_655 . ? C23 C24 H24 119.8 . . ? C27 C25 C26 120.4(4) 2_866 . ? C27 C25 H25 119.8 2_866 . ? C26 C25 H25 119.8 . . ? C25 C26 C27 118.8(4) . . ? C25 C26 C29 119.8(4) . . ? C27 C26 C29 121.4(4) . . ? C25 C27 C26 120.7(4) 2_866 . ? C25 C27 H27 119.6 2_866 . ? C26 C27 H27 119.6 . . ? C24 C28 C23 120.5(4) 2_655 . ? C24 C28 H28 119.7 2_655 . ? C23 C28 H28 119.7 . . ? O4 C29 O3 121.9(4) . . ? O4 C29 C26 118.9(4) . . ? O3 C29 C26 119.2(4) . . ? O4 C29 Cd1 58.73(19) . . ? O3 C29 Cd1 63.2(2) . . ? C26 C29 Cd1 176.7(3) . . ? C1 N1 C2 104.7(4) . . ? C1 N1 Cd1 116.0(3) . . ? C2 N1 Cd1 139.3(3) . . ? C1 N2 C3 107.0(4) . . ? C1 N2 C4 123.4(3) . . ? C3 N2 C4 129.5(4) . . ? C21 N3 C19 106.9(4) . . ? C21 N3 C15 125.8(4) . . ? C19 N3 C15 127.3(3) . . ? C21 N4 C20 106.2(3) . . ? C21 N4 Cd1 126.5(3) . . ? C20 N4 Cd1 127.3(3) . . ? C22 O2 Cd1 122.9(3) . . ? C29 O3 Cd1 89.1(2) . . ? C29 O4 Cd1 93.8(2) . . ? O2W O3W O4W 107.7(7) . . ? O5W O4W O3W 107.6(9) . . ? O2 Cd1 N4 114.05(12) . . ? O2 Cd1 N1 83.48(11) . . ? N4 Cd1 N1 96.85(12) . . ? O2 Cd1 O4 100.28(11) . . ? N4 Cd1 O4 145.39(11) . . ? N1 Cd1 O4 90.98(11) . . ? O2 Cd1 O1W 81.34(10) . . ? N4 Cd1 O1W 90.69(12) . . ? N1 Cd1 O1W 164.75(11) . . ? O4 Cd1 O1W 90.28(10) . . ? O2 Cd1 O3 153.00(11) . . ? N4 Cd1 O3 90.33(11) . . ? N1 Cd1 O3 105.92(11) . . ? O4 Cd1 O3 55.17(10) . . ? O1W Cd1 O3 87.21(10) . . ? O2 Cd1 C29 126.86(12) . . ? N4 Cd1 C29 117.99(12) . . ? N1 Cd1 C29 100.07(12) . . ? O4 Cd1 C29 27.52(11) . . ? O1W Cd1 C29 87.94(11) . . ? O3 Cd1 C29 27.67(11) . . ? 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 N1 C2 C3 N2 0.8(5) . . . . ? C9 C4 C5 C6 -2.8(7) . . . . ? N2 C4 C5 C6 173.1(4) . . . . ? C4 C5 C6 C7 0.1(7) . . . . ? C5 C6 C7 C8 1.9(6) . . . . ? C5 C6 C7 C18 -174.9(4) . . . . ? C6 C7 C8 C9 -1.3(6) . . . . ? C18 C7 C8 C9 176.2(4) . . . . ? C6 C7 C8 C10 179.4(4) . . . . ? C18 C7 C8 C10 -3.1(5) . . . . ? C7 C8 C9 C4 -1.4(7) . . . . ? C10 C8 C9 C4 177.8(4) . . . . ? C5 C4 C9 C8 3.5(7) . . . . ? N2 C4 C9 C8 -172.6(4) . . . . ? C9 C8 C10 C13 -175.7(4) . . . 1_544 ? C7 C8 C10 C13 3.6(5) . . . 1_544 ? C9 C8 C10 C11 -57.5(6) . . . . ? C7 C8 C10 C11 121.8(4) . . . . ? C9 C8 C10 C12 66.7(6) . . . . ? C7 C8 C10 C12 -114.0(4) . . . . ? C18 C13 C14 C15 0.7(6) 1_566 . . . ? C10 C13 C14 C15 -178.2(4) 1_566 . . . ? C13 C14 C15 C16 -0.1(6) . . . . ? C13 C14 C15 N3 -179.5(4) . . . . ? C14 C15 C16 C17 -0.8(7) . . . . ? N3 C15 C16 C17 178.6(4) . . . . ? C15 C16 C17 C18 1.0(7) . . . 1_566 ? C8 C7 C18 C13 1.2(5) . . . 1_544 ? C6 C7 C18 C13 178.3(4) . . . 1_544 ? C8 C7 C18 C17 -175.8(5) . . . 1_544 ? C6 C7 C18 C17 1.4(8) . . . 1_544 ? N3 C19 C20 N4 0.3(5) . . . . ? O1 C22 C23 C28 162.4(4) . . . . ? O2 C22 C23 C28 -16.0(6) . . . . ? O1 C22 C23 C24 -17.2(6) . . . . ? O2 C22 C23 C24 164.4(4) . . . . ? C28 C23 C24 C28 0.3(7) . . . 2_655 ? C22 C23 C24 C28 179.9(4) . . . 2_655 ? C27 C25 C26 C27 0.1(7) 2_866 . . . ? C27 C25 C26 C29 -179.4(4) 2_866 . . . ? C25 C26 C27 C25 -0.1(7) . . . 2_866 ? C29 C26 C27 C25 179.4(4) . . . 2_866 ? C24 C23 C28 C24 -0.3(7) . . . 2_655 ? C22 C23 C28 C24 -179.9(4) . . . 2_655 ? C25 C26 C29 O4 2.4(6) . . . . ? C27 C26 C29 O4 -177.0(4) . . . . ? C25 C26 C29 O3 -177.6(4) . . . . ? C27 C26 C29 O3 3.0(6) . . . . ? C25 C26 C29 Cd1 -41(5) . . . . ? C27 C26 C29 Cd1 139(5) . . . . ? N2 C1 N1 C2 0.4(5) . . . . ? N2 C1 N1 Cd1 179.0(3) . . . . ? C3 C2 N1 C1 -0.8(5) . . . . ? C3 C2 N1 Cd1 -178.9(3) . . . . ? N1 C1 N2 C3 0.1(5) . . . . ? N1 C1 N2 C4 176.4(4) . . . . ? C2 C3 N2 C1 -0.6(5) . . . . ? C2 C3 N2 C4 -176.5(4) . . . . ? C5 C4 N2 C1 -133.5(5) . . . . ? C9 C4 N2 C1 42.6(6) . . . . ? C5 C4 N2 C3 41.8(7) . . . . ? C9 C4 N2 C3 -142.1(5) . . . . ? N4 C21 N3 C19 -0.8(5) . . . . ? N4 C21 N3 C15 179.4(4) . . . . ? C20 C19 N3 C21 0.3(5) . . . . ? C20 C19 N3 C15 -179.9(4) . . . . ? C16 C15 N3 C21 -139.4(5) . . . . ? C14 C15 N3 C21 40.1(6) . . . . ? C16 C15 N3 C19 40.8(7) . . . . ? C14 C15 N3 C19 -139.8(4) . . . . ? N3 C21 N4 C20 1.0(5) . . . . ? N3 C21 N4 Cd1 -177.1(3) . . . . ? C19 C20 N4 C21 -0.8(5) . . . . ? C19 C20 N4 Cd1 177.3(3) . . . . ? O1 C22 O2 Cd1 14.8(6) . . . . ? C23 C22 O2 Cd1 -166.9(3) . . . . ? O4 C29 O3 Cd1 -2.5(4) . . . . ? C26 C29 O3 Cd1 177.4(3) . . . . ? O3 C29 O4 Cd1 2.6(4) . . . . ? C26 C29 O4 Cd1 -177.3(3) . . . . ? O2W O3W O4W O5W 61.1(11) . . . . ? C22 O2 Cd1 N4 36.4(4) . . . . ? C22 O2 Cd1 N1 131.0(3) . . . . ? C22 O2 Cd1 O4 -139.2(3) . . . . ? C22 O2 Cd1 O1W -50.5(3) . . . . ? C22 O2 Cd1 O3 -116.5(4) . . . . ? C22 O2 Cd1 C29 -131.3(3) . . . . ? C21 N4 Cd1 O2 -172.8(4) . . . . ? C20 N4 Cd1 O2 9.5(4) . . . . ? C21 N4 Cd1 N1 101.3(4) . . . . ? C20 N4 Cd1 N1 -76.4(4) . . . . ? C21 N4 Cd1 O4 -0.5(5) . . . . ? C20 N4 Cd1 O4 -178.2(3) . . . . ? C21 N4 Cd1 O1W -92.0(4) . . . . ? C20 N4 Cd1 O1W 90.3(4) . . . . ? C21 N4 Cd1 O3 -4.8(4) . . . . ? C20 N4 Cd1 O3 177.5(4) . . . . ? C21 N4 Cd1 C29 -4.0(4) . . . . ? C20 N4 Cd1 C29 178.3(3) . . . . ? C1 N1 Cd1 O2 21.5(3) . . . . ? C2 N1 Cd1 O2 -160.5(4) . . . . ? C1 N1 Cd1 N4 135.0(3) . . . . ? C2 N1 Cd1 N4 -47.0(4) . . . . ? C1 N1 Cd1 O4 -78.8(3) . . . . ? C2 N1 Cd1 O4 99.3(4) . . . . ? C1 N1 Cd1 O1W 15.9(6) . . . . ? C2 N1 Cd1 O1W -166.1(4) . . . . ? C1 N1 Cd1 O3 -132.7(3) . . . . ? C2 N1 Cd1 O3 45.3(4) . . . . ? C1 N1 Cd1 C29 -104.9(3) . . . . ? C2 N1 Cd1 C29 73.1(4) . . . . ? C29 O4 Cd1 O2 166.2(2) . . . . ? C29 O4 Cd1 N4 -6.6(4) . . . . ? C29 O4 Cd1 N1 -110.2(2) . . . . ? C29 O4 Cd1 O1W 85.0(2) . . . . ? C29 O4 Cd1 O3 -1.4(2) . . . . ? C29 O3 Cd1 O2 -26.2(4) . . . . ? C29 O3 Cd1 N4 178.4(2) . . . . ? C29 O3 Cd1 N1 81.2(2) . . . . ? C29 O3 Cd1 O4 1.4(2) . . . . ? C29 O3 Cd1 O1W -90.9(2) . . . . ? O4 C29 Cd1 O2 -17.0(3) . . . . ? O3 C29 Cd1 O2 165.5(2) . . . . ? C26 C29 Cd1 O2 28(5) . . . . ? O4 C29 Cd1 N4 175.7(2) . . . . ? O3 C29 Cd1 N4 -1.8(3) . . . . ? C26 C29 Cd1 N4 -139(5) . . . . ? O4 C29 Cd1 N1 72.4(2) . . . . ? O3 C29 Cd1 N1 -105.1(2) . . . . ? C26 C29 Cd1 N1 117(5) . . . . ? O3 C29 Cd1 O4 -177.5(4) . . . . ? C26 C29 Cd1 O4 45(5) . . . . ? O4 C29 Cd1 O1W -94.6(2) . . . . ? O3 C29 Cd1 O1W 87.9(2) . . . . ? C26 C29 Cd1 O1W -50(5) . . . . ? O4 C29 Cd1 O3 177.5(4) . . . . ? C26 C29 Cd1 O3 -138(5) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.93 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.686 _refine_diff_density_min -0.761 _refine_diff_density_rms 0.120 _database_code_depnum_ccdc_archive 'CCDC 972071' ####################################################################### # # 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_4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C37 H42 Cd2 N4 O10' _chemical_formula_sum 'C37 H42 Cd2 N4 O10' _chemical_formula_weight 927.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 11.774(5) _cell_length_b 11.812(5) _cell_length_c 14.993(5) _cell_angle_alpha 97.373(5) _cell_angle_beta 93.976(5) _cell_angle_gamma 114.192(5) _cell_volume 1869.1(13) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7295 _cell_measurement_theta_min 1.61 _cell_measurement_theta_max 26.02 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.648 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 936 _exptl_absorpt_coefficient_mu 1.200 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.716 _exptl_absorpt_correction_T_max 0.728 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 9.00cm _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 10470 _diffrn_reflns_av_R_equivalents 0.0201 _diffrn_reflns_av_sigmaI/netI 0.0435 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 26.00 _reflns_number_total 7295 _reflns_number_gt 5787 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXP-97 _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0617P)^2^+1.0922P] 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 7295 _refine_ls_number_parameters 473 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0542 _refine_ls_R_factor_gt 0.0380 _refine_ls_wR_factor_ref 0.1128 _refine_ls_wR_factor_gt 0.1011 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _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 C1 C 0.1575(5) -0.0125(5) 0.6419(4) 0.0374(12) Uani 1 1 d . . . C2 C 0.0145(11) -0.0493(12) 0.6309(9) 0.046(3) Uiso 0.50 1 d P . . C2' C 0.0327(8) -0.0258(8) 0.6787(6) 0.0201(18) Uiso 0.50 1 d P . . C3' C -0.0681(10) -0.1681(10) 0.6454(7) 0.0362(17) Uiso 0.50 1 d P . . C3 C -0.0484(10) -0.1317(10) 0.6981(7) 0.0362(17) Uiso 0.50 1 d P . . C4 C -0.1941(5) -0.1776(7) 0.6802(6) 0.072(2) Uani 1 1 d . . . C5' C -0.2427(7) -0.0974(8) 0.6325(6) 0.0137(16) Uiso 0.50 1 d P . . C5 C -0.2294(10) -0.0655(11) 0.6741(8) 0.039(3) Uiso 0.50 1 d P . . C6' C -0.1476(10) 0.0436(10) 0.6659(8) 0.038(2) Uiso 0.50 1 d P . . C6 C -0.1595(10) 0.0183(10) 0.6102(8) 0.040(2) Uiso 0.50 1 d P . . C7 C -0.0169(5) 0.0608(6) 0.6327(6) 0.068(2) Uani 1 1 d . . . C8 C -0.3729(4) -0.1143(5) 0.6540(3) 0.0336(11) Uani 1 1 d . . . C9 C -0.4491(5) 0.0612(5) 0.8198(3) 0.0301(11) Uani 1 1 d . . . C10 C -0.4818(5) 0.0036(5) 0.9048(3) 0.0373(12) Uani 1 1 d . . . H10 H -0.5160 -0.0878 0.8850 0.045 Uiso 1 1 calc R . . C11 C -0.5872(5) 0.0289(6) 0.9431(3) 0.0388(13) Uani 1 1 d . . . H11A H -0.6587 -0.0007 0.8961 0.047 Uiso 1 1 calc R . . H11B H -0.5591 0.1189 0.9615 0.047 Uiso 1 1 calc R . . C12 C -0.6278(5) -0.0366(6) 1.0242(4) 0.0487(15) Uani 1 1 d . . . H12A H -0.6891 -0.0119 1.0502 0.058 Uiso 1 1 calc R . . H12B H -0.6675 -0.1271 1.0039 0.058 Uiso 1 1 calc R . . C13 C -0.2092(4) 0.2974(4) 0.5558(3) 0.0253(10) Uani 1 1 d . . . C14 C -0.1101(4) 0.3844(4) 0.5057(3) 0.0309(11) Uani 1 1 d . . . H14 H -0.1302 0.3464 0.4413 0.037 Uiso 1 1 calc R . . C15 C -0.1167(5) 0.5110(5) 0.5140(5) 0.0492(16) Uani 1 1 d . . . H15A H -0.1010 0.5489 0.5776 0.059 Uiso 1 1 calc R . . H15B H -0.2003 0.4986 0.4900 0.059 Uiso 1 1 calc R . . C16 C -0.0199(5) 0.6002(5) 0.4624(5) 0.0504(16) Uani 1 1 d . . . H16A H -0.0408 0.5666 0.3980 0.060 Uiso 1 1 calc R . . H16B H -0.0227 0.6817 0.4719 0.060 Uiso 1 1 calc R . . C17 C 0.1879(5) -0.2748(5) 0.7618(3) 0.0320(11) Uani 1 1 d . . . H17 H 0.1613 -0.2105 0.7691 0.038 Uiso 1 1 calc R . . C18 C 0.2882(5) -0.3839(5) 0.7226(3) 0.0354(12) Uani 1 1 d . . . H18 H 0.3460 -0.4089 0.6974 0.043 Uiso 1 1 calc R . . C19 C 0.1993(5) -0.4530(5) 0.7707(4) 0.0371(12) Uani 1 1 d . . . H19 H 0.1841 -0.5325 0.7837 0.044 Uiso 1 1 calc R . . C20 C 0.0327(4) -0.4139(5) 0.8475(3) 0.0282(10) Uani 1 1 d . . . C21 C -0.0542(5) -0.5388(5) 0.8365(3) 0.0310(11) Uani 1 1 d . . . H21 H -0.0457 -0.6001 0.7955 0.037 Uiso 1 1 calc R . . C22 C -0.1527(4) -0.5715(4) 0.8867(3) 0.0316(11) Uani 1 1 d . . . H22 H -0.2089 -0.6556 0.8817 0.038 Uiso 1 1 calc R . . C23 C -0.1682(4) -0.4795(4) 0.9443(3) 0.0281(10) Uani 1 1 d . . . C24 C -0.0814(4) -0.3521(4) 0.9536(3) 0.0297(10) Uani 1 1 d . . . C25 C 0.0200(4) -0.3196(5) 0.9064(3) 0.0314(11) Uani 1 1 d . . . H25 H 0.0792 -0.2364 0.9136 0.038 Uiso 1 1 calc R . . C26 C -0.8810(4) 0.2679(4) 0.9816(3) 0.0306(11) Uani 1 1 d . . . C27 C -0.9853(5) 0.1901(5) 0.9029(4) 0.0499(16) Uani 1 1 d . . . H27A H -0.9579 0.1383 0.8636 0.075 Uiso 1 1 calc R . . H27B H -1.0042 0.2456 0.8694 0.075 Uiso 1 1 calc R . . H27C H -1.0592 0.1376 0.9264 0.075 Uiso 1 1 calc R . . C28 C -0.8426(6) 0.1820(5) 1.0325(4) 0.0516(15) Uani 1 1 d . . . H28A H -0.8195 0.1292 0.9906 0.077 Uiso 1 1 calc R . . H28B H -0.9118 0.1305 1.0608 0.077 Uiso 1 1 calc R . . H28C H -0.7723 0.2326 1.0782 0.077 Uiso 1 1 calc R . . C29 C -0.7655(4) 0.3661(4) 0.9499(3) 0.0289(10) Uani 1 1 d . . . C30 C -0.7367(4) 0.4868(4) 0.9963(3) 0.0272(10) Uani 1 1 d . . . C31 C -0.6325(4) 0.5890(5) 0.9798(3) 0.0314(11) Uani 1 1 d . . . H31 H -0.6131 0.6699 1.0099 0.038 Uiso 1 1 calc R . . C32 C -0.5576(5) 0.5691(5) 0.9179(3) 0.0327(11) Uani 1 1 d . . . H32 H -0.4858 0.6366 0.9083 0.039 Uiso 1 1 calc R . . C33 C -0.5885(4) 0.4505(5) 0.8708(3) 0.0300(11) Uani 1 1 d . . . C34 C -0.6932(4) 0.3472(4) 0.8859(3) 0.0296(10) Uani 1 1 d . . . H34 H -0.7140 0.2671 0.8537 0.036 Uiso 1 1 calc R . . C35 C -0.4265(5) 0.5212(5) 0.7628(4) 0.0420(13) Uani 1 1 d . . . H35 H -0.4102 0.6059 0.7675 0.050 Uiso 1 1 calc R . . C36 C -0.3738(5) 0.4591(5) 0.7120(4) 0.0447(14) Uani 1 1 d . . . H36 H -0.3137 0.4957 0.6747 0.054 Uiso 1 1 calc R . . C37 C -0.5022(5) 0.3224(4) 0.7783(3) 0.0322(11) Uani 1 1 d . . . H37 H -0.5498 0.2466 0.7968 0.039 Uiso 1 1 calc R . . N1 N 0.2812(4) -0.2721(4) 0.7162(3) 0.0279(9) Uani 1 1 d . . . N2 N 0.1363(4) -0.3812(4) 0.7964(3) 0.0284(9) Uani 1 1 d . . . N3 N -0.4195(4) 0.3349(4) 0.7217(3) 0.0328(9) Uani 1 1 d . . . N4 N -0.5109(4) 0.4322(4) 0.8071(3) 0.0300(9) Uani 1 1 d . . . O1 O 0.1846(3) -0.1047(3) 0.6381(3) 0.0408(9) Uani 1 1 d . . . O2 O 0.2326(3) 0.0962(4) 0.6337(3) 0.0562(12) Uani 1 1 d . . . O3 O -0.4374(4) -0.1947(4) 0.6941(3) 0.0626(13) Uani 1 1 d . . . O4 O -0.4177(3) -0.0478(3) 0.6127(2) 0.0263(7) Uani 1 1 d . . . O5 O -0.5390(3) 0.0419(3) 0.7604(2) 0.0343(8) Uani 1 1 d . . . O6 O -0.3366(3) 0.1236(3) 0.8090(2) 0.0385(9) Uani 1 1 d . . . O7 O -0.1863(3) 0.3031(3) 0.6392(2) 0.0378(9) Uani 1 1 d . . . O8 O -0.3160(3) 0.2225(3) 0.5140(2) 0.0341(8) Uani 1 1 d . . . OW1 O -0.5766(3) 0.0734(3) 0.5735(2) 0.0256(7) Uani 1 1 d . . . OW2 O 0.2850(9) 0.3428(7) 0.6152(8) 0.196(5) Uani 1 1 d . . . Cd1 Cd -0.38054(3) 0.16845(3) 0.66353(2) 0.02234(10) Uani 1 1 d . . . Cd2 Cd 0.37257(3) -0.12248(3) 0.63391(2) 0.02229(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.024(3) 0.036(3) 0.059(3) 0.018(3) 0.014(2) 0.015(2) C4 0.024(3) 0.068(4) 0.152(7) 0.073(5) 0.034(4) 0.027(3) C7 0.027(3) 0.050(4) 0.149(7) 0.051(4) 0.034(4) 0.023(3) C8 0.023(2) 0.040(3) 0.041(3) 0.010(2) 0.008(2) 0.015(2) C9 0.041(3) 0.030(3) 0.022(2) 0.008(2) 0.011(2) 0.015(2) C10 0.032(3) 0.050(3) 0.031(3) 0.019(2) 0.008(2) 0.014(2) C11 0.031(3) 0.058(4) 0.030(3) 0.019(3) 0.007(2) 0.018(3) C12 0.041(3) 0.071(4) 0.037(3) 0.020(3) 0.011(2) 0.023(3) C13 0.025(2) 0.023(2) 0.024(2) 0.0035(19) 0.0107(19) 0.004(2) C14 0.023(2) 0.028(3) 0.027(2) 0.007(2) 0.0103(19) -0.004(2) C15 0.028(3) 0.041(3) 0.090(5) 0.037(3) 0.034(3) 0.015(3) C16 0.036(3) 0.043(3) 0.083(4) 0.042(3) 0.028(3) 0.015(3) C17 0.034(3) 0.034(3) 0.034(3) 0.014(2) 0.014(2) 0.017(2) C18 0.033(3) 0.043(3) 0.043(3) 0.014(2) 0.017(2) 0.024(2) C19 0.040(3) 0.035(3) 0.048(3) 0.020(2) 0.018(2) 0.022(2) C20 0.029(2) 0.034(3) 0.023(2) 0.011(2) 0.0115(19) 0.012(2) C21 0.032(3) 0.031(3) 0.027(2) 0.003(2) 0.009(2) 0.010(2) C22 0.030(3) 0.022(2) 0.033(3) 0.001(2) 0.009(2) 0.001(2) C23 0.026(2) 0.024(2) 0.026(2) 0.0004(19) 0.0066(19) 0.003(2) C24 0.032(3) 0.025(2) 0.029(2) 0.005(2) 0.012(2) 0.008(2) C25 0.028(3) 0.027(3) 0.034(3) 0.007(2) 0.013(2) 0.005(2) C26 0.031(3) 0.021(2) 0.036(3) 0.004(2) 0.017(2) 0.005(2) C27 0.041(3) 0.040(3) 0.048(3) -0.009(3) 0.017(3) 0.000(3) C28 0.058(4) 0.037(3) 0.070(4) 0.020(3) 0.028(3) 0.023(3) C29 0.027(2) 0.026(3) 0.032(2) 0.005(2) 0.009(2) 0.010(2) C30 0.024(2) 0.025(2) 0.028(2) 0.0015(19) 0.0079(19) 0.006(2) C31 0.028(3) 0.023(2) 0.036(3) 0.000(2) 0.010(2) 0.005(2) C32 0.027(3) 0.026(3) 0.041(3) 0.005(2) 0.014(2) 0.005(2) C33 0.032(3) 0.034(3) 0.028(2) 0.007(2) 0.012(2) 0.017(2) C34 0.032(3) 0.023(2) 0.036(3) 0.006(2) 0.012(2) 0.011(2) C35 0.044(3) 0.028(3) 0.057(3) 0.016(3) 0.029(3) 0.013(2) C36 0.046(3) 0.037(3) 0.053(3) 0.013(3) 0.034(3) 0.014(3) C37 0.034(3) 0.024(2) 0.041(3) 0.009(2) 0.014(2) 0.012(2) N1 0.024(2) 0.032(2) 0.030(2) 0.0115(17) 0.0089(16) 0.0120(17) N2 0.026(2) 0.031(2) 0.029(2) 0.0099(17) 0.0120(16) 0.0102(18) N3 0.031(2) 0.032(2) 0.034(2) 0.0035(18) 0.0130(18) 0.0112(19) N4 0.028(2) 0.026(2) 0.038(2) 0.0080(18) 0.0150(17) 0.0111(17) O1 0.0238(18) 0.037(2) 0.072(3) 0.0229(19) 0.0177(17) 0.0170(16) O2 0.030(2) 0.040(2) 0.110(4) 0.023(2) 0.031(2) 0.0192(18) O3 0.032(2) 0.065(3) 0.111(4) 0.060(3) 0.032(2) 0.024(2) O4 0.0208(16) 0.0347(18) 0.0282(16) 0.0066(14) 0.0045(13) 0.0162(14) O5 0.044(2) 0.037(2) 0.0219(16) 0.0032(15) 0.0008(15) 0.0188(17) O6 0.036(2) 0.039(2) 0.0292(18) 0.0097(16) 0.0108(15) 0.0018(17) O7 0.0259(18) 0.045(2) 0.0257(17) 0.0067(16) 0.0085(14) -0.0021(16) O8 0.0212(17) 0.0344(19) 0.0283(17) -0.0002(15) 0.0076(14) -0.0056(15) OW1 0.0175(15) 0.0327(18) 0.0265(16) 0.0085(14) 0.0042(12) 0.0093(14) OW2 0.163(8) 0.083(5) 0.332(14) 0.006(7) -0.067(8) 0.067(5) Cd1 0.01901(18) 0.02393(19) 0.02156(17) 0.00655(13) 0.00851(13) 0.00494(14) Cd2 0.01483(17) 0.02545(19) 0.02456(18) 0.00578(14) 0.00650(12) 0.00549(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.250(6) . ? C1 O2 1.253(6) . ? C1 C2 1.548(13) . ? C1 C2' 1.560(10) . ? C2 C2' 0.719(12) . ? C2 C3' 1.397(16) . ? C2 C7 1.488(14) . ? C2 C3 1.508(16) . ? C2' C3 1.309(13) . ? C2' C7 1.575(11) . ? C2' C3' 1.597(14) . ? C3' C3 0.817(12) . ? C3' C4 1.572(12) . ? C3 C4 1.564(12) . ? C4 C5' 1.516(10) . ? C4 C5 1.553(13) . ? C5' C5 0.659(11) . ? C5' C6 1.416(13) . ? C5' C8 1.526(9) . ? C5' C6' 1.568(14) . ? C5 C6' 1.282(15) . ? C5 C6 1.504(16) . ? C5 C8 1.538(12) . ? C6' C6 0.832(13) . ? C6' C7 1.592(12) . ? C6 C7 1.540(12) . ? C8 O3 1.208(6) . ? C8 O4 1.303(6) . ? C9 O6 1.258(6) . ? C9 O5 1.260(6) . ? C9 C10 1.519(6) . ? C10 C12 1.497(7) 2_457 ? C10 C11 1.523(7) . ? C10 H10 0.9800 . ? C11 C12 1.524(7) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C10 1.497(7) 2_457 ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 O7 1.248(5) . ? C13 O8 1.262(5) . ? C13 C14 1.522(6) . ? C13 Cd1 2.750(4) . ? C14 C16 1.501(7) 2_566 ? C14 C15 1.519(7) . ? C14 H14 0.9800 . ? C15 C16 1.534(6) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C14 1.501(7) 2_566 ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 N1 1.325(6) . ? C17 N2 1.342(6) . ? C17 H17 0.9300 . ? C18 C19 1.356(7) . ? C18 N1 1.372(6) . ? C18 H18 0.9300 . ? C19 N2 1.374(6) . ? C19 H19 0.9300 . ? C20 C21 1.389(7) . ? C20 C25 1.394(7) . ? C20 N2 1.430(5) . ? C21 C22 1.374(6) . ? C21 H21 0.9300 . ? C22 C23 1.380(7) . ? C22 H22 0.9300 . ? C23 C24 1.412(6) . ? C23 C30 1.460(6) 2_457 ? C24 C25 1.373(6) . ? C24 C26 1.517(6) 2_457 ? C25 H25 0.9300 . ? C26 C24 1.517(6) 2_457 ? C26 C27 1.530(7) . ? C26 C28 1.531(7) . ? C26 C29 1.536(6) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 C34 1.382(6) . ? C29 C30 1.396(6) . ? C30 C31 1.389(6) . ? C30 C23 1.460(6) 2_457 ? C31 C32 1.385(7) . ? C31 H31 0.9300 . ? C32 C33 1.374(7) . ? C32 H32 0.9300 . ? C33 C34 1.392(7) . ? C33 N4 1.422(6) . ? C34 H34 0.9300 . ? C35 C36 1.341(7) . ? C35 N4 1.397(6) . ? C35 H35 0.9300 . ? C36 N3 1.371(7) . ? C36 H36 0.9300 . ? C37 N3 1.312(6) . ? C37 N4 1.360(6) . ? C37 H37 0.9300 . ? N1 Cd2 2.234(4) . ? N3 Cd1 2.278(4) . ? O1 Cd2 2.311(3) . ? O4 Cd2 2.318(3) 1_455 ? O4 Cd1 2.415(3) . ? O5 Cd2 2.362(3) 1_455 ? O5 Cd1 2.544(3) . ? O6 Cd1 2.381(3) . ? O7 Cd1 2.276(3) . ? O8 Cd2 2.288(3) 2_556 ? O8 Cd1 2.494(3) . ? OW1 Cd1 2.339(3) . ? OW1 Cd2 2.452(3) 1_455 ? Cd1 Cd2 3.4204(12) 1_455 ? Cd2 O8 2.288(3) 2_556 ? Cd2 O4 2.318(3) 1_655 ? Cd2 O5 2.362(3) 1_655 ? Cd2 OW1 2.452(3) 1_655 ? Cd2 Cd1 3.4204(12) 1_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 O2 124.4(5) . . ? O1 C1 C2 113.7(6) . . ? O2 C1 C2 119.9(6) . . ? O1 C1 C2' 117.7(5) . . ? O2 C1 C2' 116.7(5) . . ? C2 C1 C2' 26.7(5) . . ? C2' C2 C3' 92.3(15) . . ? C2' C2 C7 83.2(14) . . ? C3' C2 C7 124.5(10) . . ? C2' C2 C3 60.2(13) . . ? C3' C2 C3 32.4(6) . . ? C7 C2 C3 112.4(10) . . ? C2' C2 C1 77.6(13) . . ? C3' C2 C1 119.5(10) . . ? C7 C2 C1 113.3(8) . . ? C3 C2 C1 111.2(9) . . ? C2 C2' C3 91.4(15) . . ? C2 C2' C1 75.7(13) . . ? C3 C2' C1 122.8(8) . . ? C2 C2' C7 69.8(13) . . ? C3 C2' C7 119.2(8) . . ? C1 C2' C7 108.0(6) . . ? C2 C2' C3' 60.9(13) . . ? C3 C2' C3' 30.7(6) . . ? C1 C2' C3' 107.5(7) . . ? C7 C2' C3' 107.3(7) . . ? C3 C3' C2 81.3(13) . . ? C3 C3' C4 74.4(11) . . ? C2 C3' C4 116.2(9) . . ? C3 C3' C2' 54.8(11) . . ? C2 C3' C2' 26.7(5) . . ? C4 C3' C2' 106.4(8) . . ? C3' C3 C2' 94.6(13) . . ? C3' C3 C2 66.3(12) . . ? C2' C3 C2 28.5(5) . . ? C3' C3 C4 75.4(12) . . ? C2' C3 C4 123.9(9) . . ? C2 C3 C4 110.4(8) . . ? C5' C4 C5 24.8(4) . . ? C5' C4 C3 117.3(6) . . ? C5 C4 C3 111.2(7) . . ? C5' C4 C3' 109.4(6) . . ? C5 C4 C3' 117.4(7) . . ? C3 C4 C3' 30.2(5) . . ? C5 C5' C6 84.5(14) . . ? C5 C5' C4 80.7(13) . . ? C6 C5' C4 121.2(7) . . ? C5 C5' C8 78.6(13) . . ? C6 C5' C8 119.6(7) . . ? C4 C5' C8 112.5(6) . . ? C5 C5' C6' 52.8(13) . . ? C6 C5' C6' 31.9(5) . . ? C4 C5' C6' 107.2(7) . . ? C8 C5' C6' 108.9(7) . . ? C5' C5 C6' 103.1(16) . . ? C5' C5 C6 69.6(13) . . ? C6' C5 C6 33.6(6) . . ? C5' C5 C8 76.6(13) . . ? C6' C5 C8 126.2(10) . . ? C6 C5 C8 113.4(9) . . ? C5' C5 C4 74.5(13) . . ? C6' C5 C4 122.0(10) . . ? C6 C5 C4 113.4(9) . . ? C8 C5 C4 109.9(8) . . ? C6 C6' C5 88.0(14) . . ? C6 C6' C5' 63.9(11) . . ? C5 C6' C5' 24.2(6) . . ? C6 C6' C7 71.2(11) . . ? C5 C6' C7 120.8(10) . . ? C5' C6' C7 107.4(8) . . ? C6' C6 C5' 84.2(12) . . ? C6' C6 C5 58.4(11) . . ? C5' C6 C5 25.9(5) . . ? C6' C6 C7 78.1(12) . . ? C5' C6 C7 119.0(8) . . ? C5 C6 C7 110.7(9) . . ? C2 C7 C6 111.2(8) . . ? C2 C7 C2' 27.0(5) . . ? C6 C7 C2' 119.3(6) . . ? C2 C7 C6' 116.0(7) . . ? C6 C7 C6' 30.8(5) . . ? C2' C7 C6' 108.8(7) . . ? O3 C8 O4 121.6(4) . . ? O3 C8 C5' 123.8(5) . . ? O4 C8 C5' 113.8(5) . . ? O3 C8 C5 118.1(6) . . ? O4 C8 C5 118.2(6) . . ? C5' C8 C5 24.8(4) . . ? O6 C9 O5 121.7(4) . . ? O6 C9 C10 121.2(4) . . ? O5 C9 C10 117.2(4) . . ? C12 C10 C9 115.0(4) 2_457 . ? C12 C10 C11 112.2(4) 2_457 . ? C9 C10 C11 111.1(4) . . ? C12 C10 H10 105.9 2_457 . ? C9 C10 H10 105.9 . . ? C11 C10 H10 105.9 . . ? C10 C11 C12 111.7(5) . . ? C10 C11 H11A 109.3 . . ? C12 C11 H11A 109.3 . . ? C10 C11 H11B 109.3 . . ? C12 C11 H11B 109.3 . . ? H11A C11 H11B 107.9 . . ? C10 C12 C11 111.5(5) 2_457 . ? C10 C12 H12A 109.3 2_457 . ? C11 C12 H12A 109.3 . . ? C10 C12 H12B 109.3 2_457 . ? C11 C12 H12B 109.3 . . ? H12A C12 H12B 108.0 . . ? O7 C13 O8 119.8(4) . . ? O7 C13 C14 119.8(4) . . ? O8 C13 C14 120.3(4) . . ? O7 C13 Cd1 55.0(2) . . ? O8 C13 Cd1 65.0(2) . . ? C14 C13 Cd1 172.3(3) . . ? C16 C14 C15 111.2(4) 2_566 . ? C16 C14 C13 112.7(4) 2_566 . ? C15 C14 C13 109.8(4) . . ? C16 C14 H14 107.7 2_566 . ? C15 C14 H14 107.7 . . ? C13 C14 H14 107.7 . . ? C14 C15 C16 111.2(4) . . ? C14 C15 H15A 109.4 . . ? C16 C15 H15A 109.4 . . ? C14 C15 H15B 109.4 . . ? C16 C15 H15B 109.4 . . ? H15A C15 H15B 108.0 . . ? C14 C16 C15 110.8(5) 2_566 . ? C14 C16 H16A 109.5 2_566 . ? C15 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 2_566 . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 108.1 . . ? N1 C17 N2 112.1(4) . . ? N1 C17 H17 124.0 . . ? N2 C17 H17 124.0 . . ? C19 C18 N1 110.7(4) . . ? C19 C18 H18 124.7 . . ? N1 C18 H18 124.7 . . ? C18 C19 N2 105.7(4) . . ? C18 C19 H19 127.1 . . ? N2 C19 H19 127.1 . . ? C21 C20 C25 121.3(4) . . ? C21 C20 N2 119.3(4) . . ? C25 C20 N2 119.4(4) . . ? C22 C21 C20 119.7(4) . . ? C22 C21 H21 120.2 . . ? C20 C21 H21 120.2 . . ? C21 C22 C23 119.9(4) . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C22 C23 C24 120.2(4) . . ? C22 C23 C30 131.5(4) . 2_457 ? C24 C23 C30 108.3(4) . 2_457 ? C25 C24 C23 120.0(4) . . ? C25 C24 C26 129.0(4) . 2_457 ? C23 C24 C26 111.0(4) . 2_457 ? C24 C25 C20 118.7(4) . . ? C24 C25 H25 120.6 . . ? C20 C25 H25 120.6 . . ? C24 C26 C27 112.1(4) 2_457 . ? C24 C26 C28 110.5(4) 2_457 . ? C27 C26 C28 110.7(5) . . ? C24 C26 C29 101.0(4) 2_457 . ? C27 C26 C29 112.2(4) . . ? C28 C26 C29 110.1(4) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C34 C29 C30 120.8(4) . . ? C34 C29 C26 128.5(4) . . ? C30 C29 C26 110.7(4) . . ? C31 C30 C29 119.8(4) . . ? C31 C30 C23 131.3(4) . 2_457 ? C29 C30 C23 108.9(4) . 2_457 ? C32 C31 C30 119.3(5) . . ? C32 C31 H31 120.4 . . ? C30 C31 H31 120.4 . . ? C33 C32 C31 120.5(4) . . ? C33 C32 H32 119.7 . . ? C31 C32 H32 119.7 . . ? C32 C33 C34 121.0(4) . . ? C32 C33 N4 119.7(4) . . ? C34 C33 N4 119.4(4) . . ? C29 C34 C33 118.6(4) . . ? C29 C34 H34 120.7 . . ? C33 C34 H34 120.7 . . ? C36 C35 N4 105.6(5) . . ? C36 C35 H35 127.2 . . ? N4 C35 H35 127.2 . . ? C35 C36 N3 111.7(4) . . ? C35 C36 H36 124.2 . . ? N3 C36 H36 124.2 . . ? N3 C37 N4 112.7(4) . . ? N3 C37 H37 123.7 . . ? N4 C37 H37 123.7 . . ? C17 N1 C18 104.6(4) . . ? C17 N1 Cd2 122.2(3) . . ? C18 N1 Cd2 132.5(3) . . ? C17 N2 C19 107.0(4) . . ? C17 N2 C20 125.9(4) . . ? C19 N2 C20 127.1(4) . . ? C37 N3 C36 104.5(4) . . ? C37 N3 Cd1 121.0(3) . . ? C36 N3 Cd1 134.4(3) . . ? C37 N4 C35 105.6(4) . . ? C37 N4 C33 126.3(4) . . ? C35 N4 C33 128.2(4) . . ? C1 O1 Cd2 132.5(3) . . ? C8 O4 Cd2 105.8(3) . 1_455 ? C8 O4 Cd1 126.9(3) . . ? Cd2 O4 Cd1 92.54(10) 1_455 . ? C9 O5 Cd2 127.5(3) . 1_455 ? C9 O5 Cd1 88.9(3) . . ? Cd2 O5 Cd1 88.32(11) 1_455 . ? C9 O6 Cd1 96.6(3) . . ? C13 O7 Cd1 98.4(3) . . ? C13 O8 Cd2 130.0(3) . 2_556 ? C13 O8 Cd1 87.7(2) . . ? Cd2 O8 Cd1 136.07(14) 2_556 . ? Cd1 OW1 Cd2 91.08(10) . 1_455 ? O7 Cd1 N3 90.21(14) . . ? O7 Cd1 OW1 133.13(11) . . ? N3 Cd1 OW1 91.22(13) . . ? O7 Cd1 O6 101.70(12) . . ? N3 Cd1 O6 93.66(14) . . ? OW1 Cd1 O6 124.92(11) . . ? O7 Cd1 O4 110.91(12) . . ? N3 Cd1 O4 158.86(13) . . ? OW1 Cd1 O4 73.83(11) . . ? O6 Cd1 O4 83.32(12) . . ? O7 Cd1 O8 53.94(11) . . ? N3 Cd1 O8 101.83(13) . . ? OW1 Cd1 O8 80.03(10) . . ? O6 Cd1 O8 150.56(12) . . ? O4 Cd1 O8 90.43(11) . . ? O7 Cd1 O5 153.98(11) . . ? N3 Cd1 O5 86.37(13) . . ? OW1 Cd1 O5 72.79(11) . . ? O6 Cd1 O5 52.91(11) . . ? O4 Cd1 O5 75.09(11) . . ? O8 Cd1 O5 151.80(10) . . ? O7 Cd1 C13 26.67(12) . . ? N3 Cd1 C13 95.61(14) . . ? OW1 Cd1 C13 106.77(12) . . ? O6 Cd1 C13 127.15(13) . . ? O4 Cd1 C13 102.90(12) . . ? O8 Cd1 C13 27.30(11) . . ? O5 Cd1 C13 177.99(12) . . ? O7 Cd1 Cd2 152.61(9) . 1_455 ? N3 Cd1 Cd2 116.33(10) . 1_455 ? OW1 Cd1 Cd2 45.79(8) . 1_455 ? O6 Cd1 Cd2 84.12(8) . 1_455 ? O4 Cd1 Cd2 42.61(7) . 1_455 ? O8 Cd1 Cd2 110.29(7) . 1_455 ? O5 Cd1 Cd2 43.64(7) . 1_455 ? C13 Cd1 Cd2 134.69(9) . 1_455 ? N1 Cd2 O8 105.44(13) . 2_556 ? N1 Cd2 O1 81.62(13) . . ? O8 Cd2 O1 92.10(13) 2_556 . ? N1 Cd2 O4 123.77(12) . 1_655 ? O8 Cd2 O4 89.78(11) 2_556 1_655 ? O1 Cd2 O4 152.91(12) . 1_655 ? N1 Cd2 O5 94.63(13) . 1_655 ? O8 Cd2 O5 159.83(12) 2_556 1_655 ? O1 Cd2 O5 88.80(13) . 1_655 ? O4 Cd2 O5 80.51(12) 1_655 1_655 ? N1 Cd2 OW1 158.29(12) . 1_655 ? O8 Cd2 OW1 86.22(12) 2_556 1_655 ? O1 Cd2 OW1 79.66(11) . 1_655 ? O4 Cd2 OW1 73.50(10) 1_655 1_655 ? O5 Cd2 OW1 74.12(11) 1_655 1_655 ? N1 Cd2 Cd1 138.15(10) . 1_655 ? O8 Cd2 Cd1 113.52(8) 2_556 1_655 ? O1 Cd2 Cd1 110.76(9) . 1_655 ? O4 Cd2 Cd1 44.86(8) 1_655 1_655 ? O5 Cd2 Cd1 48.04(8) 1_655 1_655 ? OW1 Cd2 Cd1 43.13(7) 1_655 1_655 ? 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 C2' 104.8(13) . . . . ? O2 C1 C2 C2' -90.6(14) . . . . ? O1 C1 C2 C3' 19.2(14) . . . . ? O2 C1 C2 C3' -176.2(9) . . . . ? C2' C1 C2 C3' -85.6(16) . . . . ? O1 C1 C2 C7 -178.2(8) . . . . ? O2 C1 C2 C7 -13.7(13) . . . . ? C2' C1 C2 C7 76.9(14) . . . . ? O1 C1 C2 C3 54.0(11) . . . . ? O2 C1 C2 C3 -141.4(8) . . . . ? C2' C1 C2 C3 -50.8(12) . . . . ? C3' C2 C2' C3 -3.8(10) . . . . ? C7 C2 C2' C3 120.7(8) . . . . ? C1 C2 C2' C3 -123.6(7) . . . . ? C3' C2 C2' C1 119.7(9) . . . . ? C7 C2 C2' C1 -115.7(6) . . . . ? C3 C2 C2' C1 123.6(7) . . . . ? C3' C2 C2' C7 -124.5(10) . . . . ? C3 C2 C2' C7 -120.7(8) . . . . ? C1 C2 C2' C7 115.7(6) . . . . ? C7 C2 C2' C3' 124.5(10) . . . . ? C3 C2 C2' C3' 3.8(10) . . . . ? C1 C2 C2' C3' -119.7(9) . . . . ? O1 C1 C2' C2 -88.2(14) . . . . ? O2 C1 C2' C2 104.0(14) . . . . ? O1 C1 C2' C3 -5.9(12) . . . . ? O2 C1 C2' C3 -173.8(9) . . . . ? C2 C1 C2' C3 82.2(16) . . . . ? O1 C1 C2' C7 -150.9(6) . . . . ? O2 C1 C2' C7 41.2(9) . . . . ? C2 C1 C2' C7 -62.8(13) . . . . ? O1 C1 C2' C3' -35.5(9) . . . . ? O2 C1 C2' C3' 156.7(7) . . . . ? C2 C1 C2' C3' 52.7(13) . . . . ? C2' C2 C3' C3 6.2(17) . . . . ? C7 C2 C3' C3 -77.2(16) . . . . ? C1 C2 C3' C3 83.3(15) . . . . ? C2' C2 C3' C4 73.9(16) . . . . ? C7 C2 C3' C4 -9.5(18) . . . . ? C3 C2 C3' C4 67.7(12) . . . . ? C1 C2 C3' C4 151.0(9) . . . . ? C7 C2 C3' C2' -83.4(17) . . . . ? C3 C2 C3' C2' -6.2(17) . . . . ? C1 C2 C3' C2' 77.0(15) . . . . ? C2 C2' C3' C3 -172(2) . . . . ? C1 C2' C3' C3 125.7(13) . . . . ? C7 C2' C3' C3 -118.4(13) . . . . ? C3 C2' C3' C2 172(2) . . . . ? C1 C2' C3' C2 -61.9(14) . . . . ? C7 C2' C3' C2 54.1(14) . . . . ? C2 C2' C3' C4 -116.0(16) . . . . ? C3 C2' C3' C4 56.5(12) . . . . ? C1 C2' C3' C4 -177.9(6) . . . . ? C7 C2' C3' C4 -61.9(9) . . . . ? C2 C3' C3 C2' -3.4(9) . . . . ? C4 C3' C3 C2' -123.9(8) . . . . ? C4 C3' C3 C2 -120.5(8) . . . . ? C2' C3' C3 C2 3.4(9) . . . . ? C2 C3' C3 C4 120.5(8) . . . . ? C2' C3' C3 C4 123.9(8) . . . . ? C2 C2' C3 C3' 6.6(18) . . . . ? C1 C2' C3 C3' -67.2(15) . . . . ? C7 C2' C3 C3' 74.1(15) . . . . ? C1 C2' C3 C2 -73.8(14) . . . . ? C7 C2' C3 C2 67.5(14) . . . . ? C3' C2' C3 C2 -6.6(18) . . . . ? C2 C2' C3 C4 -68.9(17) . . . . ? C1 C2' C3 C4 -142.7(9) . . . . ? C7 C2' C3 C4 -1.4(15) . . . . ? C3' C2' C3 C4 -75.5(14) . . . . ? C2' C2 C3 C3' -173(2) . . . . ? C7 C2 C3 C3' 119.7(14) . . . . ? C1 C2 C3 C3' -112.1(14) . . . . ? C3' C2 C3 C2' 173(2) . . . . ? C7 C2 C3 C2' -67.5(14) . . . . ? C1 C2 C3 C2' 60.8(13) . . . . ? C2' C2 C3 C4 124.3(15) . . . . ? C3' C2 C3 C4 -62.9(12) . . . . ? C7 C2 C3 C4 56.8(13) . . . . ? C1 C2 C3 C4 -174.9(8) . . . . ? C3' C3 C4 C5' -81.9(13) . . . . ? C2' C3 C4 C5' 3.8(15) . . . . ? C2 C3 C4 C5' -24.6(13) . . . . ? C3' C3 C4 C5 -108.3(13) . . . . ? C2' C3 C4 C5 -22.6(14) . . . . ? C2 C3 C4 C5 -50.9(12) . . . . ? C2' C3 C4 C3' 85.7(14) . . . . ? C2 C3 C4 C3' 57.3(12) . . . . ? C3 C3' C4 C5' 111.1(12) . . . . ? C2 C3' C4 C5' 39.3(13) . . . . ? C2' C3' C4 C5' 66.1(9) . . . . ? C3 C3' C4 C5 85.4(14) . . . . ? C2 C3' C4 C5 13.7(14) . . . . ? C2' C3' C4 C5 40.4(11) . . . . ? C2 C3' C4 C3 -71.8(13) . . . . ? C2' C3' C4 C3 -45.0(10) . . . . ? C3 C4 C5' C5 -81.6(15) . . . . ? C3' C4 C5' C5 -113.5(14) . . . . ? C5 C4 C5' C6 77.8(15) . . . . ? C3 C4 C5' C6 -3.8(13) . . . . ? C3' C4 C5' C6 -35.7(12) . . . . ? C5 C4 C5' C8 -73.5(13) . . . . ? C3 C4 C5' C8 -155.1(7) . . . . ? C3' C4 C5' C8 173.0(7) . . . . ? C5 C4 C5' C6' 46.2(13) . . . . ? C3 C4 C5' C6' -35.4(11) . . . . ? C3' C4 C5' C6' -67.3(9) . . . . ? C6 C5' C5 C6' -3.0(11) . . . . ? C4 C5' C5 C6' 120.0(10) . . . . ? C8 C5' C5 C6' -124.7(11) . . . . ? C4 C5' C5 C6 122.9(6) . . . . ? C8 C5' C5 C6 -121.7(6) . . . . ? C6' C5' C5 C6 3.0(11) . . . . ? C6 C5' C5 C8 121.7(6) . . . . ? C4 C5' C5 C8 -115.4(5) . . . . ? C6' C5' C5 C8 124.7(11) . . . . ? C6 C5' C5 C4 -122.9(6) . . . . ? C8 C5' C5 C4 115.4(5) . . . . ? C6' C5' C5 C4 -120.0(10) . . . . ? C3 C4 C5 C5' 109.4(14) . . . . ? C3' C4 C5 C5' 76.9(15) . . . . ? C5' C4 C5 C6' -95.9(18) . . . . ? C3 C4 C5 C6' 13.5(16) . . . . ? C3' C4 C5 C6' -19.1(16) . . . . ? C5' C4 C5 C6 -59.0(13) . . . . ? C3 C4 C5 C6 50.4(12) . . . . ? C3' C4 C5 C6 17.8(13) . . . . ? C5' C4 C5 C8 69.1(13) . . . . ? C3 C4 C5 C8 178.5(7) . . . . ? C3' C4 C5 C8 146.0(8) . . . . ? C5' C5 C6' C6 5.0(19) . . . . ? C8 C5 C6' C6 -77.7(16) . . . . ? C4 C5 C6' C6 84.7(16) . . . . ? C6 C5 C6' C5' -5.0(19) . . . . ? C8 C5 C6' C5' -82.8(17) . . . . ? C4 C5 C6' C5' 79.7(17) . . . . ? C5' C5 C6' C7 -61.6(18) . . . . ? C6 C5 C6' C7 -66.6(13) . . . . ? C8 C5 C6' C7 -144.4(10) . . . . ? C4 C5 C6' C7 18.1(18) . . . . ? C5 C5' C6' C6 -174(2) . . . . ? C4 C5' C6' C6 122.1(13) . . . . ? C8 C5' C6' C6 -115.9(12) . . . . ? C6 C5' C6' C5 174(2) . . . . ? C4 C5' C6' C5 -63.5(15) . . . . ? C8 C5' C6' C5 58.5(15) . . . . ? C5 C5' C6' C7 127.6(17) . . . . ? C6 C5' C6' C7 -58.0(11) . . . . ? C4 C5' C6' C7 64.1(9) . . . . ? C8 C5' C6' C7 -173.9(6) . . . . ? C5 C6' C6 C5' -2.3(9) . . . . ? C7 C6' C6 C5' 121.3(7) . . . . ? C5' C6' C6 C5 2.3(9) . . . . ? C7 C6' C6 C5 123.6(8) . . . . ? C5 C6' C6 C7 -123.6(8) . . . . ? C5' C6' C6 C7 -121.3(7) . . . . ? C5 C5' C6 C6' 4.5(17) . . . . ? C4 C5' C6 C6' -71.2(14) . . . . ? C8 C5' C6 C6' 78.1(13) . . . . ? C4 C5' C6 C5 -75.7(14) . . . . ? C8 C5' C6 C5 73.6(14) . . . . ? C6' C5' C6 C5 -4.5(17) . . . . ? C5 C5' C6 C7 77.4(16) . . . . ? C4 C5' C6 C7 1.7(14) . . . . ? C8 C5' C6 C7 151.0(8) . . . . ? C6' C5' C6 C7 72.9(13) . . . . ? C5' C5 C6 C6' -175(2) . . . . ? C8 C5 C6 C6' 120.8(14) . . . . ? C4 C5 C6 C6' -112.9(14) . . . . ? C6' C5 C6 C5' 175(2) . . . . ? C8 C5 C6 C5' -64.4(13) . . . . ? C4 C5 C6 C5' 61.8(13) . . . . ? C5' C5 C6 C7 -114.1(15) . . . . ? C6' C5 C6 C7 60.6(12) . . . . ? C8 C5 C6 C7 -178.6(8) . . . . ? C4 C5 C6 C7 -52.3(12) . . . . ? C2' C2 C7 C6 -113.4(14) . . . . ? C3' C2 C7 C6 -25.3(16) . . . . ? C3 C2 C7 C6 -59.7(13) . . . . ? C1 C2 C7 C6 173.2(8) . . . . ? C3' C2 C7 C2' 88.2(17) . . . . ? C3 C2 C7 C2' 53.8(12) . . . . ? C1 C2 C7 C2' -73.3(13) . . . . ? C2' C2 C7 C6' -80.2(15) . . . . ? C3' C2 C7 C6' 8.0(17) . . . . ? C3 C2 C7 C6' -26.4(14) . . . . ? C1 C2 C7 C6' -153.5(8) . . . . ? C6' C6 C7 C2 105.7(13) . . . . ? C5' C6 C7 C2 29.2(13) . . . . ? C5 C6 C7 C2 56.3(12) . . . . ? C6' C6 C7 C2' 77.2(14) . . . . ? C5' C6 C7 C2' 0.7(14) . . . . ? C5 C6 C7 C2' 27.8(13) . . . . ? C5' C6 C7 C6' -76.4(13) . . . . ? C5 C6 C7 C6' -49.4(11) . . . . ? C3 C2' C7 C2 -79.9(15) . . . . ? C1 C2' C7 C2 66.6(13) . . . . ? C3' C2' C7 C2 -49.0(13) . . . . ? C2 C2' C7 C6 79.0(16) . . . . ? C3 C2' C7 C6 -0.9(14) . . . . ? C1 C2' C7 C6 145.6(8) . . . . ? C3' C2' C7 C6 30.0(11) . . . . ? C2 C2' C7 C6' 110.7(14) . . . . ? C3 C2' C7 C6' 30.9(12) . . . . ? C1 C2' C7 C6' 177.3(6) . . . . ? C3' C2' C7 C6' 61.8(9) . . . . ? C6 C6' C7 C2 -88.0(14) . . . . ? C5 C6' C7 C2 -12.2(15) . . . . ? C5' C6' C7 C2 -34.4(12) . . . . ? C5 C6' C7 C6 75.7(14) . . . . ? C5' C6' C7 C6 53.6(11) . . . . ? C6 C6' C7 C2' -116.1(12) . . . . ? C5 C6' C7 C2' -40.4(14) . . . . ? C5' C6' C7 C2' -62.6(10) . . . . ? C5 C5' C8 O3 -84.5(14) . . . . ? C6 C5' C8 O3 -161.4(8) . . . . ? C4 C5' C8 O3 -9.6(10) . . . . ? C6' C5' C8 O3 -128.3(7) . . . . ? C5 C5' C8 O4 106.1(13) . . . . ? C6 C5' C8 O4 29.2(10) . . . . ? C4 C5' C8 O4 -179.0(6) . . . . ? C6' C5' C8 O4 62.3(8) . . . . ? C6 C5' C8 C5 -76.9(15) . . . . ? C4 C5' C8 C5 74.9(14) . . . . ? C6' C5' C8 C5 -43.8(13) . . . . ? C5' C5 C8 O3 110.3(13) . . . . ? C6' C5 C8 O3 -153.2(11) . . . . ? C6 C5 C8 O3 170.7(8) . . . . ? C4 C5 C8 O3 42.5(11) . . . . ? C5' C5 C8 O4 -86.0(14) . . . . ? C6' C5 C8 O4 10.5(15) . . . . ? C6 C5 C8 O4 -25.6(12) . . . . ? C4 C5 C8 O4 -153.8(7) . . . . ? C6' C5 C8 C5' 96.5(18) . . . . ? C6 C5 C8 C5' 60.4(13) . . . . ? C4 C5 C8 C5' -67.8(13) . . . . ? O6 C9 C10 C12 5.1(7) . . . 2_457 ? O5 C9 C10 C12 -176.0(5) . . . 2_457 ? O6 C9 C10 C11 134.0(5) . . . . ? O5 C9 C10 C11 -47.2(6) . . . . ? C12 C10 C11 C12 -54.0(7) 2_457 . . . ? C9 C10 C11 C12 175.7(5) . . . . ? C10 C11 C12 C10 53.5(7) . . . 2_457 ? O7 C13 C14 C16 40.2(7) . . . 2_566 ? O8 C13 C14 C16 -142.1(5) . . . 2_566 ? Cd1 C13 C14 C16 86(3) . . . 2_566 ? O7 C13 C14 C15 -84.3(6) . . . . ? O8 C13 C14 C15 93.4(6) . . . . ? Cd1 C13 C14 C15 -39(3) . . . . ? C16 C14 C15 C16 55.9(7) 2_566 . . . ? C13 C14 C15 C16 -178.7(5) . . . . ? C14 C15 C16 C14 -55.7(7) . . . 2_566 ? N1 C18 C19 N2 -1.0(6) . . . . ? C25 C20 C21 C22 -2.0(7) . . . . ? N2 C20 C21 C22 178.7(4) . . . . ? C20 C21 C22 C23 3.0(8) . . . . ? C21 C22 C23 C24 -1.5(8) . . . . ? C21 C22 C23 C30 179.2(5) . . . 2_457 ? C22 C23 C24 C25 -1.2(8) . . . . ? C30 C23 C24 C25 178.3(5) 2_457 . . . ? C22 C23 C24 C26 178.5(5) . . . 2_457 ? C30 C23 C24 C26 -2.0(6) 2_457 . . 2_457 ? C23 C24 C25 C20 2.2(7) . . . . ? C26 C24 C25 C20 -177.5(5) 2_457 . . . ? C21 C20 C25 C24 -0.6(7) . . . . ? N2 C20 C25 C24 178.6(4) . . . . ? C24 C26 C29 C34 -176.3(5) 2_457 . . . ? C27 C26 C29 C34 -56.8(7) . . . . ? C28 C26 C29 C34 66.9(7) . . . . ? C24 C26 C29 C30 4.5(5) 2_457 . . . ? C27 C26 C29 C30 123.9(5) . . . . ? C28 C26 C29 C30 -112.4(5) . . . . ? C34 C29 C30 C31 -1.5(7) . . . . ? C26 C29 C30 C31 177.8(5) . . . . ? C34 C29 C30 C23 177.1(5) . . . 2_457 ? C26 C29 C30 C23 -3.6(6) . . . 2_457 ? C29 C30 C31 C32 -0.7(7) . . . . ? C23 C30 C31 C32 -179.0(5) 2_457 . . . ? C30 C31 C32 C33 2.5(8) . . . . ? C31 C32 C33 C34 -2.0(8) . . . . ? C31 C32 C33 N4 179.6(5) . . . . ? C30 C29 C34 C33 2.0(7) . . . . ? C26 C29 C34 C33 -177.2(5) . . . . ? C32 C33 C34 C29 -0.2(7) . . . . ? N4 C33 C34 C29 178.1(4) . . . . ? N4 C35 C36 N3 -0.3(7) . . . . ? N2 C17 N1 C18 0.1(6) . . . . ? N2 C17 N1 Cd2 171.7(3) . . . . ? C19 C18 N1 C17 0.6(6) . . . . ? C19 C18 N1 Cd2 -169.8(4) . . . . ? N1 C17 N2 C19 -0.7(6) . . . . ? N1 C17 N2 C20 -178.8(4) . . . . ? C18 C19 N2 C17 1.0(6) . . . . ? C18 C19 N2 C20 179.1(4) . . . . ? C21 C20 N2 C17 143.9(5) . . . . ? C25 C20 N2 C17 -35.3(7) . . . . ? C21 C20 N2 C19 -33.9(7) . . . . ? C25 C20 N2 C19 146.9(5) . . . . ? N4 C37 N3 C36 -1.2(6) . . . . ? N4 C37 N3 Cd1 178.8(3) . . . . ? C35 C36 N3 C37 0.9(7) . . . . ? C35 C36 N3 Cd1 -179.1(4) . . . . ? N3 C37 N4 C35 1.0(6) . . . . ? N3 C37 N4 C33 -177.8(4) . . . . ? C36 C35 N4 C37 -0.4(6) . . . . ? C36 C35 N4 C33 178.4(5) . . . . ? C32 C33 N4 C37 156.7(5) . . . . ? C34 C33 N4 C37 -21.7(8) . . . . ? C32 C33 N4 C35 -21.8(8) . . . . ? C34 C33 N4 C35 159.8(5) . . . . ? O2 C1 O1 Cd2 8.8(9) . . . . ? C2 C1 O1 Cd2 172.6(6) . . . . ? C2' C1 O1 Cd2 -158.0(5) . . . . ? O3 C8 O4 Cd2 -1.1(6) . . . 1_455 ? C5' C8 O4 Cd2 168.6(4) . . . 1_455 ? C5 C8 O4 Cd2 -164.1(6) . . . 1_455 ? O3 C8 O4 Cd1 104.6(6) . . . . ? C5' C8 O4 Cd1 -85.7(5) . . . . ? C5 C8 O4 Cd1 -58.5(7) . . . . ? O6 C9 O5 Cd2 86.6(6) . . . 1_455 ? C10 C9 O5 Cd2 -92.3(5) . . . 1_455 ? O6 C9 O5 Cd1 -0.4(5) . . . . ? C10 C9 O5 Cd1 -179.3(4) . . . . ? O5 C9 O6 Cd1 0.5(5) . . . . ? C10 C9 O6 Cd1 179.3(4) . . . . ? O8 C13 O7 Cd1 -4.4(5) . . . . ? C14 C13 O7 Cd1 173.3(4) . . . . ? O7 C13 O8 Cd2 -151.2(4) . . . 2_556 ? C14 C13 O8 Cd2 31.2(7) . . . 2_556 ? Cd1 C13 O8 Cd2 -155.1(4) . . . 2_556 ? O7 C13 O8 Cd1 3.9(5) . . . . ? C14 C13 O8 Cd1 -173.7(4) . . . . ? C13 O7 Cd1 N3 -102.2(3) . . . . ? C13 O7 Cd1 OW1 -10.3(4) . . . . ? C13 O7 Cd1 O6 164.1(3) . . . . ? C13 O7 Cd1 O4 76.8(3) . . . . ? C13 O7 Cd1 O8 2.4(3) . . . . ? C13 O7 Cd1 O5 175.7(3) . . . . ? C13 O7 Cd1 Cd2 64.1(4) . . . 1_455 ? C37 N3 Cd1 O7 -155.8(4) . . . . ? C36 N3 Cd1 O7 24.1(5) . . . . ? C37 N3 Cd1 OW1 71.0(4) . . . . ? C36 N3 Cd1 OW1 -109.1(5) . . . . ? C37 N3 Cd1 O6 -54.1(4) . . . . ? C36 N3 Cd1 O6 125.8(5) . . . . ? C37 N3 Cd1 O4 26.8(6) . . . . ? C36 N3 Cd1 O4 -153.2(4) . . . . ? C37 N3 Cd1 O8 151.1(4) . . . . ? C36 N3 Cd1 O8 -29.0(5) . . . . ? C37 N3 Cd1 O5 -1.7(4) . . . . ? C36 N3 Cd1 O5 178.3(5) . . . . ? C37 N3 Cd1 C13 178.0(4) . . . . ? C36 N3 Cd1 C13 -2.1(5) . . . . ? C37 N3 Cd1 Cd2 31.1(4) . . . 1_455 ? C36 N3 Cd1 Cd2 -148.9(5) . . . 1_455 ? Cd2 OW1 Cd1 O7 141.82(14) 1_455 . . . ? Cd2 OW1 Cd1 N3 -126.74(12) 1_455 . . . ? Cd2 OW1 Cd1 O6 -31.42(17) 1_455 . . . ? Cd2 OW1 Cd1 O4 38.09(10) 1_455 . . . ? Cd2 OW1 Cd1 O8 131.46(12) 1_455 . . . ? Cd2 OW1 Cd1 O5 -40.92(10) 1_455 . . . ? Cd2 OW1 Cd1 C13 137.02(12) 1_455 . . . ? C9 O6 Cd1 O7 173.4(3) . . . . ? C9 O6 Cd1 N3 82.4(3) . . . . ? C9 O6 Cd1 OW1 -11.6(3) . . . . ? C9 O6 Cd1 O4 -76.6(3) . . . . ? C9 O6 Cd1 O8 -155.5(3) . . . . ? C9 O6 Cd1 O5 -0.2(3) . . . . ? C9 O6 Cd1 C13 -177.7(3) . . . . ? C9 O6 Cd1 Cd2 -33.7(3) . . . 1_455 ? C8 O4 Cd1 O7 76.7(4) . . . . ? Cd2 O4 Cd1 O7 -171.41(10) 1_455 . . . ? C8 O4 Cd1 N3 -106.2(5) . . . . ? Cd2 O4 Cd1 N3 5.7(4) 1_455 . . . ? C8 O4 Cd1 OW1 -152.7(4) . . . . ? Cd2 O4 Cd1 OW1 -40.78(10) 1_455 . . . ? C8 O4 Cd1 O6 -23.4(3) . . . . ? Cd2 O4 Cd1 O6 88.57(12) 1_455 . . . ? C8 O4 Cd1 O8 127.8(3) . . . . ? Cd2 O4 Cd1 O8 -120.27(11) 1_455 . . . ? C8 O4 Cd1 O5 -76.7(3) . . . . ? Cd2 O4 Cd1 O5 35.24(10) 1_455 . . . ? C8 O4 Cd1 C13 103.3(4) . . . . ? Cd2 O4 Cd1 C13 -144.77(12) 1_455 . . . ? C8 O4 Cd1 Cd2 -111.9(4) . . . 1_455 ? C13 O8 Cd1 O7 -2.3(3) . . . . ? Cd2 O8 Cd1 O7 150.0(3) 2_556 . . . ? C13 O8 Cd1 N3 79.2(3) . . . . ? Cd2 O8 Cd1 N3 -128.5(2) 2_556 . . . ? C13 O8 Cd1 OW1 168.3(3) . . . . ? Cd2 O8 Cd1 OW1 -39.4(2) 2_556 . . . ? C13 O8 Cd1 O6 -41.1(4) . . . . ? Cd2 O8 Cd1 O6 111.2(3) 2_556 . . . ? C13 O8 Cd1 O4 -118.2(3) . . . . ? Cd2 O8 Cd1 O4 34.1(2) 2_556 . . . ? C13 O8 Cd1 O5 -176.1(3) . . . . ? Cd2 O8 Cd1 O5 -23.8(4) 2_556 . . . ? Cd2 O8 Cd1 C13 152.3(4) 2_556 . . . ? C13 O8 Cd1 Cd2 -156.7(3) . . . 1_455 ? Cd2 O8 Cd1 Cd2 -4.4(3) 2_556 . . 1_455 ? C9 O5 Cd1 O7 -14.1(4) . . . . ? Cd2 O5 Cd1 O7 -141.7(3) 1_455 . . . ? C9 O5 Cd1 N3 -97.1(3) . . . . ? Cd2 O5 Cd1 N3 135.27(14) 1_455 . . . ? C9 O5 Cd1 OW1 170.5(3) . . . . ? Cd2 O5 Cd1 OW1 42.87(11) 1_455 . . . ? C9 O5 Cd1 O6 0.2(3) . . . . ? Cd2 O5 Cd1 O6 -127.36(17) 1_455 . . . ? C9 O5 Cd1 O4 93.1(3) . . . . ? Cd2 O5 Cd1 O4 -34.47(10) 1_455 . . . ? C9 O5 Cd1 O8 154.4(3) . . . . ? Cd2 O5 Cd1 O8 26.8(3) 1_455 . . . ? C9 O5 Cd1 C13 93(3) . . . . ? Cd2 O5 Cd1 C13 -35(3) 1_455 . . . ? C9 O5 Cd1 Cd2 127.6(3) . . . 1_455 ? O8 C13 Cd1 O7 175.8(5) . . . . ? C14 C13 Cd1 O7 -49(2) . . . . ? O7 C13 Cd1 N3 79.2(3) . . . . ? O8 C13 Cd1 N3 -105.0(3) . . . . ? C14 C13 Cd1 N3 30(3) . . . . ? O7 C13 Cd1 OW1 172.2(3) . . . . ? O8 C13 Cd1 OW1 -12.0(3) . . . . ? C14 C13 Cd1 OW1 123(3) . . . . ? O7 C13 Cd1 O6 -19.7(4) . . . . ? O8 C13 Cd1 O6 156.1(3) . . . . ? C14 C13 Cd1 O6 -69(3) . . . . ? O7 C13 Cd1 O4 -111.1(3) . . . . ? O8 C13 Cd1 O4 64.7(3) . . . . ? C14 C13 Cd1 O4 -160(3) . . . . ? O7 C13 Cd1 O8 -175.8(5) . . . . ? C14 C13 Cd1 O8 135(3) . . . . ? O7 C13 Cd1 O5 -111(3) . . . . ? O8 C13 Cd1 O5 65(3) . . . . ? C14 C13 Cd1 O5 -160(3) . . . . ? O7 C13 Cd1 Cd2 -144.4(3) . . . 1_455 ? O8 C13 Cd1 Cd2 31.4(3) . . . 1_455 ? C14 C13 Cd1 Cd2 166(2) . . . 1_455 ? C17 N1 Cd2 O8 -111.3(4) . . . 2_556 ? C18 N1 Cd2 O8 57.6(5) . . . 2_556 ? C17 N1 Cd2 O1 -21.5(4) . . . . ? C18 N1 Cd2 O1 147.5(5) . . . . ? C17 N1 Cd2 O4 148.3(3) . . . 1_655 ? C18 N1 Cd2 O4 -42.7(5) . . . 1_655 ? C17 N1 Cd2 O5 66.6(4) . . . 1_655 ? C18 N1 Cd2 O5 -124.4(4) . . . 1_655 ? C17 N1 Cd2 OW1 9.2(6) . . . 1_655 ? C18 N1 Cd2 OW1 178.2(4) . . . 1_655 ? C17 N1 Cd2 Cd1 90.4(4) . . . 1_655 ? C18 N1 Cd2 Cd1 -100.6(4) . . . 1_655 ? C1 O1 Cd2 N1 144.8(5) . . . . ? C1 O1 Cd2 O8 -109.9(5) . . . 2_556 ? C1 O1 Cd2 O4 -16.2(7) . . . 1_655 ? C1 O1 Cd2 O5 50.0(5) . . . 1_655 ? C1 O1 Cd2 OW1 -24.1(5) . . . 1_655 ? C1 O1 Cd2 Cd1 6.3(5) . . . 1_655 ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.985 _refine_diff_density_min -0.499 _refine_diff_density_rms 0.129 _database_code_depnum_ccdc_archive 'CCDC 972072' ####################################################################### # # 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_5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C29 H30 Cd N4 O5' _chemical_formula_sum 'C29 H30 Cd N4 O5' _chemical_formula_weight 626.97 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M c2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 13.977(5) _cell_length_b 17.017(5) _cell_length_c 24.062(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 93.727(5) _cell_angle_gamma 90.000(5) _cell_volume 5711(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6983 _cell_measurement_theta_min 1.61 _cell_measurement_theta_max 26.02 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.458 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2560 _exptl_absorpt_coefficient_mu 0.809 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.790 _exptl_absorpt_correction_T_max 0.818 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 9.00cm _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 18055 _diffrn_reflns_av_R_equivalents 0.0362 _diffrn_reflns_av_sigmaI/netI 0.0500 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 28.40 _reflns_number_total 6983 _reflns_number_gt 5128 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXP-97 _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0466P)^2^+0.5066P] 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 6983 _refine_ls_number_parameters 349 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0594 _refine_ls_R_factor_gt 0.0360 _refine_ls_wR_factor_ref 0.0971 _refine_ls_wR_factor_gt 0.0884 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _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 C1 C 0.7813(2) 0.4438(2) 0.00968(12) 0.0430(7) Uani 1 1 d . . . H1 H 0.7749 0.4385 -0.0289 0.052 Uiso 1 1 calc R . . C2 C 0.8396(2) 0.4647(3) 0.09199(13) 0.0602(10) Uani 1 1 d . . . H2 H 0.8827 0.4770 0.1218 0.072 Uiso 1 1 calc R . . C3 C 0.7480(2) 0.4453(3) 0.09680(12) 0.0584(10) Uani 1 1 d . . . H3 H 0.7164 0.4417 0.1295 0.070 Uiso 1 1 calc R . . C4 C 0.6130(2) 0.41077(18) 0.02641(11) 0.0372(7) Uani 1 1 d . . . C5 C 0.5397(2) 0.43462(18) 0.05858(12) 0.0393(7) Uani 1 1 d . . . H5 H 0.5535 0.4629 0.0912 0.047 Uiso 1 1 calc R . . C6 C 0.4459(2) 0.41608(18) 0.04181(11) 0.0381(7) Uani 1 1 d . . . H6 H 0.3961 0.4323 0.0629 0.046 Uiso 1 1 calc R . . C7 C 0.4265(2) 0.37340(16) -0.00643(11) 0.0337(6) Uani 1 1 d . . . C8 C 0.5012(2) 0.34938(17) -0.03827(11) 0.0361(6) Uani 1 1 d . . . C9 C 0.5954(2) 0.36730(18) -0.02195(12) 0.0403(7) Uani 1 1 d . . . H9 H 0.6454 0.3507 -0.0428 0.048 Uiso 1 1 calc R . . C10 C 0.4637(2) 0.30243(19) -0.08958(12) 0.0421(7) Uani 1 1 d . . . C11 C 0.3571(2) 0.30281(18) -0.08119(11) 0.0386(7) Uani 1 1 d . . . C12 C 0.3354(2) 0.34428(17) -0.03339(11) 0.0343(6) Uani 1 1 d . . . C13 C 0.2422(2) 0.35097(17) -0.01864(11) 0.0383(7) Uani 1 1 d . . . H13 H 0.2281 0.3792 0.0129 0.046 Uiso 1 1 calc R . . C14 C 0.1702(2) 0.31522(18) -0.05121(12) 0.0401(7) Uani 1 1 d . . . H14 H 0.1070 0.3189 -0.0416 0.048 Uiso 1 1 calc R . . C15 C 0.1917(2) 0.27374(18) -0.09829(12) 0.0379(7) Uani 1 1 d . . . C16 C 0.2847(2) 0.26789(19) -0.11426(12) 0.0423(7) Uani 1 1 d . . . H16 H 0.2981 0.2411 -0.1465 0.051 Uiso 1 1 calc R . . C17 C 0.5042(2) 0.2194(2) -0.08815(17) 0.0634(10) Uani 1 1 d . . . H17A H 0.5716 0.2212 -0.0936 0.095 Uiso 1 1 calc R . . H17B H 0.4721 0.1887 -0.1172 0.095 Uiso 1 1 calc R . . H17C H 0.4944 0.1959 -0.0527 0.095 Uiso 1 1 calc R . . C18 C 0.4847(3) 0.3456(3) -0.14360(13) 0.0653(11) Uani 1 1 d . . . H18A H 0.5524 0.3445 -0.1482 0.098 Uiso 1 1 calc R . . H18B H 0.4635 0.3991 -0.1416 0.098 Uiso 1 1 calc R . . H18C H 0.4514 0.3200 -0.1747 0.098 Uiso 1 1 calc R . . C19 C 0.1218(2) 0.17037(19) -0.16195(12) 0.0417(7) Uani 1 1 d . . . H19 H 0.1787 0.1435 -0.1664 0.050 Uiso 1 1 calc R . . C20 C 0.0199(2) 0.2572(2) -0.13445(14) 0.0522(8) Uani 1 1 d . . . H20 H -0.0074 0.3000 -0.1174 0.063 Uiso 1 1 calc R . . C21 C -0.0257(2) 0.2035(2) -0.16784(14) 0.0531(9) Uani 1 1 d . . . H21 H -0.0912 0.2034 -0.1776 0.064 Uiso 1 1 calc R . . C22 C -0.1690(2) -0.0172(2) -0.24314(13) 0.0434(8) Uani 1 1 d . . . C23 C -0.2618(2) -0.0627(2) -0.23566(13) 0.0583(10) Uani 1 1 d . . . H23 H -0.2572 -0.0840 -0.1977 0.070 Uiso 1 1 calc R . . C24 C -0.3481(2) -0.0085(3) -0.23994(14) 0.0734(14) Uani 1 1 d . . . H24A H -0.3345 0.0376 -0.2171 0.088 Uiso 1 1 calc R . . H24B H -0.4026 -0.0353 -0.2256 0.088 Uiso 1 1 calc R . . C25 C -0.3737(2) 0.0173(2) -0.29987(13) 0.0550(9) Uani 1 1 d . . . H25A H -0.4305 0.0500 -0.3010 0.066 Uiso 1 1 calc R . . H25B H -0.3215 0.0482 -0.3132 0.066 Uiso 1 1 calc R . . C26 C -0.3918(2) -0.0533(2) -0.33735(11) 0.0434(7) Uani 1 1 d . . . H26 H -0.4445 -0.0830 -0.3225 0.052 Uiso 1 1 calc R . . C27 C -0.3044(2) -0.1072(2) -0.33472(13) 0.0501(8) Uani 1 1 d . . . H27A H -0.3186 -0.1536 -0.3572 0.060 Uiso 1 1 calc R . . H27B H -0.2510 -0.0802 -0.3500 0.060 Uiso 1 1 calc R . . C28 C -0.2766(3) -0.1317(2) -0.27488(15) 0.0717(12) Uani 1 1 d . . . H28A H -0.3266 -0.1652 -0.2617 0.086 Uiso 1 1 calc R . . H28B H -0.2180 -0.1623 -0.2742 0.086 Uiso 1 1 calc R . . C29 C 1.07729(19) 0.53230(19) 0.10306(11) 0.0346(6) Uani 1 1 d . . . N1 N 0.86171(18) 0.46413(17) 0.03763(10) 0.0434(6) Uani 1 1 d . . . N2 N 0.70978(17) 0.43166(15) 0.04331(9) 0.0401(6) Uani 1 1 d . . . N3 N 0.11510(17) 0.23558(15) -0.13065(10) 0.0394(6) Uani 1 1 d . . . N4 N 0.03801(17) 0.14924(16) -0.18539(10) 0.0422(6) Uani 1 1 d . . . O1 O 1.03566(15) 0.58494(13) 0.07340(8) 0.0444(5) Uani 1 1 d . . . O2 O 1.09285(16) 0.46550(13) 0.08455(8) 0.0488(6) Uani 1 1 d . . . O3 O -0.1507(2) 0.0408(2) -0.21257(12) 0.0874(11) Uani 1 1 d . . . O4 O -0.11405(18) -0.03692(18) -0.27764(12) 0.0766(9) Uani 1 1 d . . . Cd1 Cd 1.0000 0.5000 0.0000 0.03392(9) Uani 1 2 d S . . Cd2 Cd 0.0000 0.055712(19) -0.2500 0.03316(9) Uani 1 2 d S . . OW1 O -0.2935(13) 0.1810(11) -0.2360(7) 0.598(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 C1 0.0418(17) 0.059(2) 0.0281(14) -0.0052(14) 0.0032(12) -0.0153(16) C2 0.0458(19) 0.104(3) 0.0297(16) -0.0049(18) -0.0040(14) -0.019(2) C3 0.0434(19) 0.105(3) 0.0268(15) -0.0037(17) 0.0017(13) -0.015(2) C4 0.0352(15) 0.0415(17) 0.0346(15) 0.0018(13) -0.0004(12) -0.0106(13) C5 0.0434(17) 0.0433(18) 0.0312(14) -0.0024(13) 0.0020(12) -0.0058(14) C6 0.0381(16) 0.0432(17) 0.0334(15) -0.0010(13) 0.0063(12) -0.0026(14) C7 0.0339(15) 0.0325(15) 0.0344(14) 0.0028(12) 0.0002(11) -0.0029(12) C8 0.0364(15) 0.0367(16) 0.0353(15) -0.0041(12) 0.0037(12) -0.0081(13) C9 0.0373(16) 0.0464(18) 0.0379(15) -0.0059(13) 0.0072(12) -0.0051(14) C10 0.0367(16) 0.0489(19) 0.0411(16) -0.0131(14) 0.0067(12) -0.0112(14) C11 0.0373(16) 0.0399(17) 0.0386(16) -0.0047(13) 0.0026(12) -0.0064(13) C12 0.0366(15) 0.0338(16) 0.0321(14) -0.0012(12) -0.0002(11) -0.0022(13) C13 0.0401(16) 0.0377(17) 0.0366(15) -0.0066(12) -0.0009(12) 0.0027(13) C14 0.0319(15) 0.0421(18) 0.0459(17) -0.0055(14) -0.0002(12) 0.0047(13) C15 0.0338(15) 0.0383(17) 0.0406(16) -0.0024(13) -0.0056(12) -0.0024(13) C16 0.0438(17) 0.0469(18) 0.0364(15) -0.0116(13) 0.0033(13) -0.0080(14) C17 0.045(2) 0.056(2) 0.090(3) -0.029(2) 0.0101(18) -0.0051(18) C18 0.066(2) 0.090(3) 0.0415(19) -0.0089(19) 0.0103(16) -0.027(2) C19 0.0368(16) 0.0454(18) 0.0427(17) -0.0086(14) 0.0012(13) 0.0017(14) C20 0.0401(18) 0.051(2) 0.064(2) -0.0123(17) -0.0090(15) 0.0119(16) C21 0.0356(17) 0.059(2) 0.063(2) -0.0163(17) -0.0124(15) 0.0060(16) C22 0.0305(16) 0.061(2) 0.0375(16) 0.0139(15) -0.0090(13) -0.0077(15) C23 0.0410(18) 0.097(3) 0.0354(17) 0.0246(18) -0.0123(13) -0.0278(19) C24 0.0334(18) 0.152(5) 0.0343(18) -0.001(2) 0.0000(14) -0.018(2) C25 0.0364(17) 0.091(3) 0.0364(17) -0.0093(17) -0.0028(13) 0.0065(18) C26 0.0286(14) 0.070(2) 0.0304(14) 0.0124(15) -0.0057(11) -0.0104(15) C27 0.0464(18) 0.049(2) 0.0519(19) 0.0095(15) -0.0193(14) -0.0077(16) C28 0.065(2) 0.074(3) 0.071(2) 0.037(2) -0.0366(19) -0.032(2) C29 0.0240(13) 0.0471(18) 0.0325(14) -0.0069(13) 0.0002(11) -0.0012(13) N1 0.0380(14) 0.0597(18) 0.0321(13) -0.0044(12) -0.0003(10) -0.0117(13) N2 0.0341(13) 0.0553(17) 0.0311(13) -0.0050(11) 0.0017(10) -0.0098(12) N3 0.0342(13) 0.0407(15) 0.0423(14) -0.0068(11) -0.0059(10) -0.0007(11) N4 0.0343(13) 0.0467(16) 0.0446(14) -0.0093(12) -0.0044(10) 0.0017(12) O1 0.0490(13) 0.0471(13) 0.0352(11) -0.0100(9) -0.0122(9) 0.0108(11) O2 0.0605(15) 0.0467(14) 0.0378(12) -0.0042(10) -0.0083(10) 0.0053(11) O3 0.076(2) 0.119(3) 0.0718(18) -0.0421(18) 0.0402(15) -0.0527(19) O4 0.0467(15) 0.090(2) 0.096(2) -0.0384(17) 0.0239(14) -0.0220(15) Cd1 0.02891(16) 0.04433(19) 0.02780(15) -0.00657(12) -0.00374(11) -0.00498(13) Cd2 0.02449(15) 0.04312(18) 0.03136(16) 0.000 -0.00200(10) 0.000 _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 C1 N1 1.318(4) . ? C1 N2 1.343(4) . ? C1 H1 0.9300 . ? C2 C3 1.334(4) . ? C2 N1 1.363(4) . ? C2 H2 0.9300 . ? C3 N2 1.381(4) . ? C3 H3 0.9300 . ? C4 C5 1.384(4) . ? C4 C9 1.387(4) . ? C4 N2 1.432(4) . ? C5 C6 1.383(4) . ? C5 H5 0.9300 . ? C6 C7 1.381(4) . ? C6 H6 0.9300 . ? C7 C8 1.396(4) . ? C7 C12 1.476(4) . ? C8 C9 1.383(4) . ? C8 C10 1.534(4) . ? C9 H9 0.9300 . ? C10 C11 1.517(4) . ? C10 C17 1.522(5) . ? C10 C18 1.538(4) . ? C11 C16 1.380(4) . ? C11 C12 1.399(4) . ? C12 C13 1.376(4) . ? C13 C14 1.376(4) . ? C13 H13 0.9300 . ? C14 C15 1.384(4) . ? C14 H14 0.9300 . ? C15 C16 1.382(4) . ? C15 N3 1.438(3) . ? C16 H16 0.9300 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 N4 1.316(4) . ? C19 N3 1.348(4) . ? C19 H19 0.9300 . ? C20 C21 1.348(4) . ? C20 N3 1.378(4) . ? C20 H20 0.9300 . ? C21 N4 1.368(4) . ? C21 H21 0.9300 . ? C22 O4 1.214(4) . ? C22 O3 1.247(4) . ? C22 C23 1.532(4) . ? C22 Cd2 2.682(3) . ? C23 C28 1.512(5) . ? C23 C24 1.516(6) . ? C23 H23 0.9800 . ? C24 C25 1.527(5) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.513(5) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C29 1.513(4) 8_355 ? C26 C27 1.526(5) . ? C26 H26 0.9800 . ? C27 C28 1.525(4) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 O2 1.245(4) . ? C29 O1 1.263(3) . ? C29 C26 1.513(4) 8_656 ? C29 Cd1 2.696(3) . ? N1 Cd1 2.271(3) . ? N4 Cd2 2.264(2) . ? O1 Cd1 2.3115(19) . ? O2 Cd1 2.413(2) . ? O3 Cd2 2.357(3) . ? O4 Cd2 2.309(3) . ? Cd1 N1 2.271(3) 5_765 ? Cd1 O1 2.3115(19) 5_765 ? Cd1 O2 2.413(2) 5_765 ? Cd1 C29 2.696(3) 5_765 ? Cd2 N4 2.264(2) 2_554 ? Cd2 O4 2.309(3) 2_554 ? Cd2 O3 2.357(3) 2_554 ? Cd2 C22 2.682(3) 2_554 ? 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 C1 N2 112.1(3) . . ? N1 C1 H1 123.9 . . ? N2 C1 H1 123.9 . . ? C3 C2 N1 111.1(3) . . ? C3 C2 H2 124.5 . . ? N1 C2 H2 124.5 . . ? C2 C3 N2 106.0(3) . . ? C2 C3 H3 127.0 . . ? N2 C3 H3 127.0 . . ? C5 C4 C9 121.9(3) . . ? C5 C4 N2 119.2(3) . . ? C9 C4 N2 118.9(3) . . ? C6 C5 C4 119.5(3) . . ? C6 C5 H5 120.3 . . ? C4 C5 H5 120.3 . . ? C7 C6 C5 119.7(3) . . ? C7 C6 H6 120.1 . . ? C5 C6 H6 120.1 . . ? C6 C7 C8 120.1(3) . . ? C6 C7 C12 131.5(3) . . ? C8 C7 C12 108.4(2) . . ? C9 C8 C7 120.8(3) . . ? C9 C8 C10 127.8(3) . . ? C7 C8 C10 111.4(2) . . ? C8 C9 C4 118.0(3) . . ? C8 C9 H9 121.0 . . ? C4 C9 H9 121.0 . . ? C11 C10 C17 111.6(3) . . ? C11 C10 C8 100.3(2) . . ? C17 C10 C8 111.0(3) . . ? C11 C10 C18 110.7(3) . . ? C17 C10 C18 111.8(3) . . ? C8 C10 C18 110.9(3) . . ? C16 C11 C12 120.1(3) . . ? C16 C11 C10 127.7(3) . . ? C12 C11 C10 112.3(2) . . ? C13 C12 C11 120.8(3) . . ? C13 C12 C7 131.5(3) . . ? C11 C12 C7 107.7(2) . . ? C12 C13 C14 119.0(3) . . ? C12 C13 H13 120.5 . . ? C14 C13 H13 120.5 . . ? C13 C14 C15 120.1(3) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? C16 C15 C14 121.5(3) . . ? C16 C15 N3 119.8(3) . . ? C14 C15 N3 118.7(3) . . ? C11 C16 C15 118.4(3) . . ? C11 C16 H16 120.8 . . ? C15 C16 H16 120.8 . . ? C10 C17 H17A 109.5 . . ? C10 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C10 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C10 C18 H18A 109.5 . . ? C10 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C10 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N4 C19 N3 111.9(3) . . ? N4 C19 H19 124.1 . . ? N3 C19 H19 124.1 . . ? C21 C20 N3 106.0(3) . . ? C21 C20 H20 127.0 . . ? N3 C20 H20 127.0 . . ? C20 C21 N4 110.5(3) . . ? C20 C21 H21 124.8 . . ? N4 C21 H21 124.8 . . ? O4 C22 O3 120.5(3) . . ? O4 C22 C23 121.3(3) . . ? O3 C22 C23 118.2(3) . . ? O4 C22 Cd2 59.16(17) . . ? O3 C22 Cd2 61.49(17) . . ? C23 C22 Cd2 175.6(2) . . ? C28 C23 C24 110.8(3) . . ? C28 C23 C22 113.7(3) . . ? C24 C23 C22 111.1(3) . . ? C28 C23 H23 107.0 . . ? C24 C23 H23 107.0 . . ? C22 C23 H23 107.0 . . ? C23 C24 C25 112.0(3) . . ? C23 C24 H24A 109.2 . . ? C25 C24 H24A 109.2 . . ? C23 C24 H24B 109.2 . . ? C25 C24 H24B 109.2 . . ? H24A C24 H24B 107.9 . . ? C26 C25 C24 110.8(3) . . ? C26 C25 H25A 109.5 . . ? C24 C25 H25A 109.5 . . ? C26 C25 H25B 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 108.1 . . ? C25 C26 C29 113.9(3) . 8_355 ? C25 C26 C27 110.5(2) . . ? C29 C26 C27 111.1(2) 8_355 . ? C25 C26 H26 107.0 . . ? C29 C26 H26 107.0 8_355 . ? C27 C26 H26 107.0 . . ? C28 C27 C26 111.0(3) . . ? C28 C27 H27A 109.4 . . ? C26 C27 H27A 109.4 . . ? C28 C27 H27B 109.4 . . ? C26 C27 H27B 109.4 . . ? H27A C27 H27B 108.0 . . ? C23 C28 C27 113.1(3) . . ? C23 C28 H28A 109.0 . . ? C27 C28 H28A 109.0 . . ? C23 C28 H28B 109.0 . . ? C27 C28 H28B 109.0 . . ? H28A C28 H28B 107.8 . . ? O2 C29 O1 122.0(2) . . ? O2 C29 C26 120.6(3) . 8_656 ? O1 C29 C26 117.4(3) . 8_656 ? O2 C29 Cd1 63.50(14) . . ? O1 C29 Cd1 58.86(14) . . ? C26 C29 Cd1 172.86(19) 8_656 . ? C1 N1 C2 104.6(2) . . ? C1 N1 Cd1 125.9(2) . . ? C2 N1 Cd1 129.2(2) . . ? C1 N2 C3 106.1(2) . . ? C1 N2 C4 126.4(2) . . ? C3 N2 C4 127.4(2) . . ? C19 N3 C20 106.5(2) . . ? C19 N3 C15 126.8(3) . . ? C20 N3 C15 126.7(3) . . ? C19 N4 C21 105.2(3) . . ? C19 N4 Cd2 130.5(2) . . ? C21 N4 Cd2 123.93(19) . . ? C29 O1 Cd1 93.25(17) . . ? C29 O2 Cd1 89.00(17) . . ? C22 O3 Cd2 90.8(2) . . ? C22 O4 Cd2 94.0(2) . . ? N1 Cd1 N1 180.00(11) . 5_765 ? N1 Cd1 O1 90.59(8) . . ? N1 Cd1 O1 89.41(8) 5_765 . ? N1 Cd1 O1 89.41(8) . 5_765 ? N1 Cd1 O1 90.59(8) 5_765 5_765 ? O1 Cd1 O1 180.00(6) . 5_765 ? N1 Cd1 O2 88.65(9) . 5_765 ? N1 Cd1 O2 91.35(9) 5_765 5_765 ? O1 Cd1 O2 124.71(7) . 5_765 ? O1 Cd1 O2 55.29(7) 5_765 5_765 ? N1 Cd1 O2 91.35(9) . . ? N1 Cd1 O2 88.65(9) 5_765 . ? O1 Cd1 O2 55.29(7) . . ? O1 Cd1 O2 124.71(7) 5_765 . ? O2 Cd1 O2 180.00(12) 5_765 . ? N1 Cd1 C29 89.35(9) . . ? N1 Cd1 C29 90.65(9) 5_765 . ? O1 Cd1 C29 27.89(8) . . ? O1 Cd1 C29 152.11(8) 5_765 . ? O2 Cd1 C29 152.50(8) 5_765 . ? O2 Cd1 C29 27.50(8) . . ? N1 Cd1 C29 90.65(9) . 5_765 ? N1 Cd1 C29 89.35(9) 5_765 5_765 ? O1 Cd1 C29 152.11(8) . 5_765 ? O1 Cd1 C29 27.89(8) 5_765 5_765 ? O2 Cd1 C29 27.50(8) 5_765 5_765 ? O2 Cd1 C29 152.50(8) . 5_765 ? C29 Cd1 C29 180.0 . 5_765 ? N4 Cd2 N4 90.66(13) . 2_554 ? N4 Cd2 O4 143.58(9) . . ? N4 Cd2 O4 98.94(11) 2_554 . ? N4 Cd2 O4 98.94(11) . 2_554 ? N4 Cd2 O4 143.58(9) 2_554 2_554 ? O4 Cd2 O4 93.88(16) . 2_554 ? N4 Cd2 O3 89.38(9) . . ? N4 Cd2 O3 99.36(11) 2_554 . ? O4 Cd2 O3 54.49(9) . . ? O4 Cd2 O3 115.69(11) 2_554 . ? N4 Cd2 O3 99.36(11) . 2_554 ? N4 Cd2 O3 89.38(9) 2_554 2_554 ? O4 Cd2 O3 115.69(11) . 2_554 ? O4 Cd2 O3 54.49(9) 2_554 2_554 ? O3 Cd2 O3 167.61(17) . 2_554 ? N4 Cd2 C22 116.83(10) . . ? N4 Cd2 C22 101.49(9) 2_554 . ? O4 Cd2 C22 26.83(9) . . ? O4 Cd2 C22 105.10(10) 2_554 . ? O3 Cd2 C22 27.70(10) . . ? O3 Cd2 C22 141.76(13) 2_554 . ? N4 Cd2 C22 101.49(9) . 2_554 ? N4 Cd2 C22 116.83(10) 2_554 2_554 ? O4 Cd2 C22 105.10(10) . 2_554 ? O4 Cd2 C22 26.83(9) 2_554 2_554 ? O3 Cd2 C22 141.76(13) . 2_554 ? O3 Cd2 C22 27.70(10) 2_554 2_554 ? C22 Cd2 C22 124.88(16) . 2_554 ? 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 N1 C2 C3 N2 0.0(5) . . . . ? C9 C4 C5 C6 -1.2(5) . . . . ? N2 C4 C5 C6 178.6(3) . . . . ? C4 C5 C6 C7 0.6(5) . . . . ? C5 C6 C7 C8 -0.3(4) . . . . ? C5 C6 C7 C12 178.6(3) . . . . ? C6 C7 C8 C9 0.5(4) . . . . ? C12 C7 C8 C9 -178.7(3) . . . . ? C6 C7 C8 C10 179.6(3) . . . . ? C12 C7 C8 C10 0.4(3) . . . . ? C7 C8 C9 C4 -1.0(5) . . . . ? C10 C8 C9 C4 -179.9(3) . . . . ? C5 C4 C9 C8 1.4(5) . . . . ? N2 C4 C9 C8 -178.4(3) . . . . ? C9 C8 C10 C11 178.2(3) . . . . ? C7 C8 C10 C11 -0.8(3) . . . . ? C9 C8 C10 C17 60.2(4) . . . . ? C7 C8 C10 C17 -118.8(3) . . . . ? C9 C8 C10 C18 -64.7(4) . . . . ? C7 C8 C10 C18 116.3(3) . . . . ? C17 C10 C11 C16 -61.2(4) . . . . ? C8 C10 C11 C16 -178.8(3) . . . . ? C18 C10 C11 C16 64.0(4) . . . . ? C17 C10 C11 C12 118.5(3) . . . . ? C8 C10 C11 C12 0.9(3) . . . . ? C18 C10 C11 C12 -116.3(3) . . . . ? C16 C11 C12 C13 -0.1(5) . . . . ? C10 C11 C12 C13 -179.8(3) . . . . ? C16 C11 C12 C7 179.0(3) . . . . ? C10 C11 C12 C7 -0.7(3) . . . . ? C6 C7 C12 C13 0.1(5) . . . . ? C8 C7 C12 C13 179.1(3) . . . . ? C6 C7 C12 C11 -178.8(3) . . . . ? C8 C7 C12 C11 0.2(3) . . . . ? C11 C12 C13 C14 0.9(4) . . . . ? C7 C12 C13 C14 -177.9(3) . . . . ? C12 C13 C14 C15 -0.5(5) . . . . ? C13 C14 C15 C16 -0.9(5) . . . . ? C13 C14 C15 N3 178.6(3) . . . . ? C12 C11 C16 C15 -1.3(5) . . . . ? C10 C11 C16 C15 178.4(3) . . . . ? C14 C15 C16 C11 1.7(5) . . . . ? N3 C15 C16 C11 -177.7(3) . . . . ? N3 C20 C21 N4 -0.4(4) . . . . ? O4 C22 C23 C28 -0.4(5) . . . . ? O3 C22 C23 C28 180.0(3) . . . . ? Cd2 C22 C23 C28 -95(4) . . . . ? O4 C22 C23 C24 -126.1(4) . . . . ? O3 C22 C23 C24 54.2(4) . . . . ? Cd2 C22 C23 C24 140(4) . . . . ? C28 C23 C24 C25 -53.7(4) . . . . ? C22 C23 C24 C25 73.7(4) . . . . ? C23 C24 C25 C26 56.9(4) . . . . ? C24 C25 C26 C29 177.0(2) . . . 8_355 ? C24 C25 C26 C27 -57.3(3) . . . . ? C25 C26 C27 C28 55.7(3) . . . . ? C29 C26 C27 C28 -177.0(3) 8_355 . . . ? C24 C23 C28 C27 52.6(4) . . . . ? C22 C23 C28 C27 -73.3(4) . . . . ? C26 C27 C28 C23 -54.0(4) . . . . ? N2 C1 N1 C2 0.1(4) . . . . ? N2 C1 N1 Cd1 -175.1(2) . . . . ? C3 C2 N1 C1 -0.1(5) . . . . ? C3 C2 N1 Cd1 174.9(3) . . . . ? N1 C1 N2 C3 -0.1(4) . . . . ? N1 C1 N2 C4 178.5(3) . . . . ? C2 C3 N2 C1 0.0(4) . . . . ? C2 C3 N2 C4 -178.5(3) . . . . ? C5 C4 N2 C1 -150.1(3) . . . . ? C9 C4 N2 C1 29.7(5) . . . . ? C5 C4 N2 C3 28.1(5) . . . . ? C9 C4 N2 C3 -152.1(3) . . . . ? N4 C19 N3 C20 0.2(4) . . . . ? N4 C19 N3 C15 178.5(3) . . . . ? C21 C20 N3 C19 0.1(4) . . . . ? C21 C20 N3 C15 -178.2(3) . . . . ? C16 C15 N3 C19 28.1(4) . . . . ? C14 C15 N3 C19 -151.3(3) . . . . ? C16 C15 N3 C20 -153.9(3) . . . . ? C14 C15 N3 C20 26.6(5) . . . . ? N3 C19 N4 C21 -0.4(4) . . . . ? N3 C19 N4 Cd2 171.98(19) . . . . ? C20 C21 N4 C19 0.5(4) . . . . ? C20 C21 N4 Cd2 -172.5(2) . . . . ? O2 C29 O1 Cd1 7.0(3) . . . . ? C26 C29 O1 Cd1 -173.0(2) 8_656 . . . ? O1 C29 O2 Cd1 -6.7(3) . . . . ? C26 C29 O2 Cd1 173.3(2) 8_656 . . . ? O4 C22 O3 Cd2 -4.6(4) . . . . ? C23 C22 O3 Cd2 175.0(2) . . . . ? O3 C22 O4 Cd2 4.7(4) . . . . ? C23 C22 O4 Cd2 -174.9(3) . . . . ? C1 N1 Cd1 N1 -50(45) . . . 5_765 ? C2 N1 Cd1 N1 136(45) . . . 5_765 ? C1 N1 Cd1 O1 147.4(3) . . . . ? C2 N1 Cd1 O1 -26.6(3) . . . . ? C1 N1 Cd1 O1 -32.6(3) . . . 5_765 ? C2 N1 Cd1 O1 153.4(3) . . . 5_765 ? C1 N1 Cd1 O2 22.7(3) . . . 5_765 ? C2 N1 Cd1 O2 -151.3(3) . . . 5_765 ? C1 N1 Cd1 O2 -157.3(3) . . . . ? C2 N1 Cd1 O2 28.7(3) . . . . ? C1 N1 Cd1 C29 175.3(3) . . . . ? C2 N1 Cd1 C29 1.3(3) . . . . ? C1 N1 Cd1 C29 -4.7(3) . . . 5_765 ? C2 N1 Cd1 C29 -178.7(3) . . . 5_765 ? C29 O1 Cd1 N1 87.50(17) . . . . ? C29 O1 Cd1 N1 -92.50(17) . . . 5_765 ? C29 O1 Cd1 O1 41(100) . . . 5_765 ? C29 O1 Cd1 O2 176.26(15) . . . 5_765 ? C29 O1 Cd1 O2 -3.74(15) . . . . ? C29 O1 Cd1 C29 180.0 . . . 5_765 ? C29 O2 Cd1 N1 -85.99(18) . . . . ? C29 O2 Cd1 N1 94.01(18) . . . 5_765 ? C29 O2 Cd1 O1 3.79(16) . . . . ? C29 O2 Cd1 O1 -176.21(16) . . . 5_765 ? C29 O2 Cd1 O2 -109(100) . . . 5_765 ? C29 O2 Cd1 C29 180.0 . . . 5_765 ? O2 C29 Cd1 N1 94.18(18) . . . . ? O1 C29 Cd1 N1 -92.49(17) . . . . ? C26 C29 Cd1 N1 -32.0(19) 8_656 . . . ? O2 C29 Cd1 N1 -85.82(18) . . . 5_765 ? O1 C29 Cd1 N1 87.51(17) . . . 5_765 ? C26 C29 Cd1 N1 148.0(19) 8_656 . . 5_765 ? O2 C29 Cd1 O1 -173.3(3) . . . . ? C26 C29 Cd1 O1 60.5(19) 8_656 . . . ? O2 C29 Cd1 O1 6.7(3) . . . 5_765 ? O1 C29 Cd1 O1 180.0 . . . 5_765 ? C26 C29 Cd1 O1 -119.5(19) 8_656 . . 5_765 ? O2 C29 Cd1 O2 180.000(1) . . . 5_765 ? O1 C29 Cd1 O2 -6.7(3) . . . 5_765 ? C26 C29 Cd1 O2 54(2) 8_656 . . 5_765 ? O1 C29 Cd1 O2 173.3(3) . . . . ? C26 C29 Cd1 O2 -126(2) 8_656 . . . ? O2 C29 Cd1 C29 -99(100) . . . 5_765 ? O1 C29 Cd1 C29 75(100) . . . 5_765 ? C26 C29 Cd1 C29 135(100) 8_656 . . 5_765 ? C19 N4 Cd2 N4 -109.8(3) . . . 2_554 ? C21 N4 Cd2 N4 61.4(2) . . . 2_554 ? C19 N4 Cd2 O4 144.1(3) . . . . ? C21 N4 Cd2 O4 -44.7(3) . . . . ? C19 N4 Cd2 O4 35.0(3) . . . 2_554 ? C21 N4 Cd2 O4 -153.9(3) . . . 2_554 ? C19 N4 Cd2 O3 150.9(3) . . . . ? C21 N4 Cd2 O3 -38.0(3) . . . . ? C19 N4 Cd2 O3 -20.3(3) . . . 2_554 ? C21 N4 Cd2 O3 150.9(3) . . . 2_554 ? C19 N4 Cd2 C22 147.0(3) . . . . ? C21 N4 Cd2 C22 -41.9(3) . . . . ? C19 N4 Cd2 C22 7.8(3) . . . 2_554 ? C21 N4 Cd2 C22 179.0(3) . . . 2_554 ? C22 O4 Cd2 N4 5.6(3) . . . . ? C22 O4 Cd2 N4 -97.8(2) . . . 2_554 ? C22 O4 Cd2 O4 116.4(3) . . . 2_554 ? C22 O4 Cd2 O3 -2.6(2) . . . . ? C22 O4 Cd2 O3 168.6(2) . . . 2_554 ? C22 O4 Cd2 C22 141.1(2) . . . 2_554 ? C22 O3 Cd2 N4 -172.5(2) . . . . ? C22 O3 Cd2 N4 96.9(2) . . . 2_554 ? C22 O3 Cd2 O4 2.6(2) . . . . ? C22 O3 Cd2 O4 -72.9(3) . . . 2_554 ? C22 O3 Cd2 O3 -37.4(2) . . . 2_554 ? C22 O3 Cd2 C22 -64.6(3) . . . 2_554 ? O4 C22 Cd2 N4 -176.2(2) . . . . ? O3 C22 Cd2 N4 8.4(3) . . . . ? C23 C22 Cd2 N4 -79(4) . . . . ? O4 C22 Cd2 N4 87.1(2) . . . 2_554 ? O3 C22 Cd2 N4 -88.3(2) . . . 2_554 ? C23 C22 Cd2 N4 -176(4) . . . 2_554 ? O3 C22 Cd2 O4 -175.4(4) . . . . ? C23 C22 Cd2 O4 97(4) . . . . ? O4 C22 Cd2 O4 -67.8(3) . . . 2_554 ? O3 C22 Cd2 O4 116.9(2) . . . 2_554 ? C23 C22 Cd2 O4 29(4) . . . 2_554 ? O4 C22 Cd2 O3 175.4(4) . . . . ? C23 C22 Cd2 O3 -88(4) . . . . ? O4 C22 Cd2 O3 -16.8(3) . . . 2_554 ? O3 C22 Cd2 O3 167.84(19) . . . 2_554 ? C23 C22 Cd2 O3 80(4) . . . 2_554 ? O4 C22 Cd2 C22 -47.6(2) . . . 2_554 ? O3 C22 Cd2 C22 137.1(3) . . . 2_554 ? C23 C22 Cd2 C22 49(4) . . . 2_554 ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 28.40 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 0.873 _refine_diff_density_min -0.378 _refine_diff_density_rms 0.073 _database_code_depnum_ccdc_archive 'CCDC 972073' ####################################################################### # # 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_6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C60 H44 N8 O13 Zn2' _chemical_formula_sum 'C60 H44 N8 O13 Zn2' _chemical_formula_weight 1215.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 '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 13.0926(5) _cell_length_b 20.9762(8) _cell_length_c 20.0992(8) _cell_angle_alpha 90.00 _cell_angle_beta 94.1230(10) _cell_angle_gamma 90.00 _cell_volume 5505.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 10893 _cell_measurement_theta_min 1.61 _cell_measurement_theta_max 26.02 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.467 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2496 _exptl_absorpt_coefficient_mu 0.946 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.774 _exptl_absorpt_correction_T_max 0.794 _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 9.00cm _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 30329 _diffrn_reflns_av_R_equivalents 0.0561 _diffrn_reflns_av_sigmaI/netI 0.0706 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 26.07 _reflns_number_total 10893 _reflns_number_gt 7536 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXP-97 _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0671P)^2^+5.5604P] 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 10893 _refine_ls_number_parameters 743 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0839 _refine_ls_R_factor_gt 0.0510 _refine_ls_wR_factor_ref 0.1448 _refine_ls_wR_factor_gt 0.1263 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.002 _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 C1 C 0.9541(3) -0.47396(19) 1.0782(2) 0.0259(9) Uani 1 1 d . . . H1 H 1.0165 -0.4635 1.0616 0.031 Uiso 1 1 calc R . . C2 C 0.9108(3) -0.5321(2) 1.0750(2) 0.0287(10) Uani 1 1 d . . . H2 H 0.9365 -0.5685 1.0558 0.034 Uiso 1 1 calc R . . C3 C 0.8123(3) -0.46629(19) 1.1256(2) 0.0233(9) Uani 1 1 d . . . H3 H 0.7576 -0.4502 1.1475 0.028 Uiso 1 1 calc R . . C4 C 0.7459(3) -0.5762(2) 1.1118(2) 0.0331(11) Uani 1 1 d . . . C5 C 0.7399(5) -0.6242(3) 1.0658(3) 0.079(2) Uani 1 1 d . . . H5 H 0.7864 -0.6262 1.0329 0.095 Uiso 1 1 calc R . . C6 C 0.6634(6) -0.6703(3) 1.0684(4) 0.111(4) Uani 1 1 d . . . H6 H 0.6588 -0.7032 1.0373 0.134 Uiso 1 1 calc R . . C7 C 0.5950(4) -0.6671(2) 1.1170(3) 0.0554(17) Uani 1 1 d . . . C8 C 0.6020(3) -0.6180(2) 1.1630(2) 0.0290(10) Uani 1 1 d . . . C9 C 0.6780(3) -0.57246(19) 1.1615(2) 0.0266(9) Uani 1 1 d . . . H9 H 0.6835 -0.5400 1.1931 0.032 Uiso 1 1 calc R . . C10 C 0.5075(4) -0.7076(2) 1.1310(3) 0.0557(16) Uani 1 1 d . . . C11 C 0.4710(5) -0.7630(3) 1.1024(3) 0.085(3) Uani 1 1 d . . . H11 H 0.5042 -0.7816 1.0680 0.102 Uiso 1 1 calc R . . C12 C 0.3838(5) -0.7916(3) 1.1252(3) 0.0637(19) Uani 1 1 d . . . H12 H 0.3574 -0.8287 1.1051 0.076 Uiso 1 1 calc R . . C13 C 0.3371(3) -0.7645(2) 1.1775(2) 0.0314(10) Uani 1 1 d . . . C14 C 0.3743(3) -0.70937(19) 1.2076(2) 0.0256(9) Uani 1 1 d . . . H14 H 0.3421 -0.6914 1.2429 0.031 Uiso 1 1 calc R . . C15 C 0.4603(3) -0.6812(2) 1.1844(2) 0.0270(9) Uani 1 1 d . . . C16 C 0.5163(3) -0.62207(19) 1.2101(2) 0.0249(9) Uani 1 1 d . . . C17 C 0.5572(4) -0.6309(3) 1.2824(2) 0.0524(15) Uani 1 1 d . . . H17A H 0.5923 -0.5929 1.2978 0.079 Uiso 1 1 calc R . . H17B H 0.6038 -0.6663 1.2854 0.079 Uiso 1 1 calc R . . H17C H 0.5012 -0.6391 1.3095 0.079 Uiso 1 1 calc R . . C18 C 0.4486(4) -0.5630(2) 1.2039(3) 0.0503(14) Uani 1 1 d . . . H18A H 0.4867 -0.5266 1.2206 0.075 Uiso 1 1 calc R . . H18B H 0.3899 -0.5689 1.2291 0.075 Uiso 1 1 calc R . . H18C H 0.4266 -0.5562 1.1578 0.075 Uiso 1 1 calc R . . C19 C 0.2270(3) -0.8005(2) 1.2657(2) 0.0274(9) Uani 1 1 d . . . H19 H 0.2689 -0.7856 1.3017 0.033 Uiso 1 1 calc R . . C20 C 0.1030(3) -0.8437(2) 1.2069(2) 0.0329(10) Uani 1 1 d . . . H20 H 0.0417 -0.8647 1.1952 0.040 Uiso 1 1 calc R . . C21 C 0.1694(3) -0.8229(2) 1.1637(2) 0.0361(11) Uani 1 1 d . . . H21 H 0.1630 -0.8267 1.1175 0.043 Uiso 1 1 calc R . . C22 C 0.6602(6) 0.1958(2) 0.9529(4) 0.094(3) Uani 1 1 d . . . H22 H 0.6171 0.2201 0.9777 0.112 Uiso 1 1 calc R . . C23 C 0.7335(6) 0.2196(2) 0.9156(4) 0.092(3) Uani 1 1 d . . . H23 H 0.7514 0.2622 0.9110 0.110 Uiso 1 1 calc R . . C24 C 0.7280(3) 0.11699(19) 0.9073(2) 0.0230(9) Uani 1 1 d . . . H24 H 0.7420 0.0756 0.8940 0.028 Uiso 1 1 calc R . . C25 C 0.8446(3) 0.1697(2) 0.8340(2) 0.0302(10) Uani 1 1 d . . . C26 C 0.8289(4) 0.2151(2) 0.7835(2) 0.0383(12) Uani 1 1 d . . . H26 H 0.7770 0.2451 0.7853 0.046 Uiso 1 1 calc R . . C27 C 0.8911(4) 0.2150(2) 0.7308(2) 0.0355(11) Uani 1 1 d . . . H27 H 0.8834 0.2462 0.6979 0.043 Uiso 1 1 calc R . . C28 C 0.9648(3) 0.16816(19) 0.7273(2) 0.0272(9) Uani 1 1 d . . . C29 C 0.9801(3) 0.12322(19) 0.7783(2) 0.0242(9) Uani 1 1 d . . . C30 C 0.9201(3) 0.1237(2) 0.8325(2) 0.0272(9) Uani 1 1 d . . . H30 H 0.9304 0.0941 0.8668 0.033 Uiso 1 1 calc R . . C31 C 1.0623(3) 0.07595(19) 0.7635(2) 0.0241(9) Uani 1 1 d . . . C32 C 1.0923(3) 0.10054(19) 0.6965(2) 0.0247(9) Uani 1 1 d . . . C33 C 1.1649(3) 0.0751(2) 0.6572(2) 0.0259(9) Uani 1 1 d . . . H33 H 1.2044 0.0402 0.6714 0.031 Uiso 1 1 calc R . . C34 C 1.1767(3) 0.1034(2) 0.5957(2) 0.0287(10) Uani 1 1 d . . . C35 C 1.1177(3) 0.1552(2) 0.5735(2) 0.0331(10) Uani 1 1 d . . . H35 H 1.1255 0.1724 0.5315 0.040 Uiso 1 1 calc R . . C36 C 1.0478(4) 0.1811(2) 0.6137(2) 0.0358(11) Uani 1 1 d . . . H36 H 1.0096 0.2167 0.5997 0.043 Uiso 1 1 calc R . . C37 C 1.0346(3) 0.15344(19) 0.6756(2) 0.0275(9) Uani 1 1 d . . . C38 C 1.0184(3) 0.00859(19) 0.7574(2) 0.0308(10) Uani 1 1 d . . . H38A H 1.0718 -0.0207 0.7480 0.046 Uiso 1 1 calc R . . H38B H 0.9654 0.0073 0.7219 0.046 Uiso 1 1 calc R . . H38C H 0.9905 -0.0032 0.7985 0.046 Uiso 1 1 calc R . . C39 C 1.1536(3) 0.0773(2) 0.8162(2) 0.0381(11) Uani 1 1 d . . . H39A H 1.2038 0.0466 0.8048 0.057 Uiso 1 1 calc R . . H39B H 1.1302 0.0670 0.8592 0.057 Uiso 1 1 calc R . . H39C H 1.1836 0.1191 0.8177 0.057 Uiso 1 1 calc R . . C40 C 1.2832(3) 0.0158(2) 0.5503(2) 0.0386(11) Uani 1 1 d . . . H40 H 1.2576 -0.0191 0.5723 0.046 Uiso 1 1 calc R . . C41 C 1.3584(4) 0.0154(3) 0.5078(2) 0.0437(12) Uani 1 1 d . . . H41 H 1.3944 -0.0205 0.4958 0.052 Uiso 1 1 calc R . . C42 C 1.3085(3) 0.1127(2) 0.5139(2) 0.0371(11) Uani 1 1 d . . . H42 H 1.3023 0.1565 0.5072 0.045 Uiso 1 1 calc R . . C43 C 0.8508(3) -0.25052(18) 1.07502(19) 0.0219(9) Uani 1 1 d . . . C44 C 0.8444(3) -0.18673(18) 1.04047(19) 0.0205(8) Uani 1 1 d . . . C45 C 0.7513(3) -0.15474(17) 1.03526(19) 0.0195(8) Uani 1 1 d . . . H45 H 0.6938 -0.1735 1.0517 0.023 Uiso 1 1 calc R . . C46 C 0.7434(3) -0.09505(17) 1.00567(19) 0.0185(8) Uani 1 1 d . . . C47 C 0.8292(3) -0.06767(18) 0.97974(19) 0.0200(8) Uani 1 1 d . . . H47 H 0.8242 -0.0279 0.9593 0.024 Uiso 1 1 calc R . . C48 C 0.9217(3) -0.09974(18) 0.98448(19) 0.0205(8) Uani 1 1 d . . . C49 C 0.9298(3) -0.15877(18) 1.01570(19) 0.0200(8) Uani 1 1 d . . . H49 H 0.9927 -0.1796 1.0200 0.024 Uiso 1 1 calc R . . C50 C 1.0109(3) -0.0698(2) 0.9533(2) 0.0260(9) Uani 1 1 d . . . C51 C 0.6432(3) -0.06042(18) 1.00193(19) 0.0202(8) Uani 1 1 d . . . C52 C 1.1465(3) -0.37261(18) 1.1579(2) 0.0226(9) Uani 1 1 d . . . C53 C 1.2459(3) -0.38270(18) 1.1981(2) 0.0219(8) Uani 1 1 d . . . C54 C 1.2499(3) -0.39231(18) 1.2669(2) 0.0221(9) Uani 1 1 d . . . H54 H 1.1896 -0.3918 1.2886 0.026 Uiso 1 1 calc R . . C55 C 1.3426(3) -0.40264(18) 1.3034(2) 0.0225(9) Uani 1 1 d . . . C56 C 1.4330(3) -0.40235(19) 1.2706(2) 0.0259(9) Uani 1 1 d . . . H56 H 1.4955 -0.4081 1.2949 0.031 Uiso 1 1 calc R . . C57 C 1.4302(3) -0.39358(19) 1.2019(2) 0.0245(9) Uani 1 1 d . . . C58 C 1.3362(3) -0.38365(18) 1.1660(2) 0.0228(9) Uani 1 1 d . . . H58 H 1.3341 -0.3776 1.1201 0.027 Uiso 1 1 calc R . . C59 C 1.5254(3) -0.3996(2) 1.1650(2) 0.0305(10) Uani 1 1 d . . . C60 C 1.3443(3) -0.41564(19) 1.3768(2) 0.0263(9) Uani 1 1 d . . . N1 N 0.6591(3) 0.13141(16) 0.94882(18) 0.0313(9) Uani 1 1 d . . . N2 N 0.7759(3) 0.16844(16) 0.88608(19) 0.0336(9) Uani 1 1 d . . . N3 N 1.2522(3) 0.07828(18) 0.55454(17) 0.0298(8) Uani 1 1 d . . . N4 N 1.3735(3) 0.0756(2) 0.48495(19) 0.0414(10) Uani 1 1 d . . . N5 N 0.8924(2) -0.43223(15) 1.10970(16) 0.0213(7) Uani 1 1 d . . . N6 N 0.8208(2) -0.52697(16) 1.10586(17) 0.0262(8) Uani 1 1 d . . . N7 N 0.2486(3) -0.79494(16) 1.20157(17) 0.0275(8) Uani 1 1 d . . . N8 N 0.1396(2) -0.82935(16) 1.27085(17) 0.0245(8) Uani 1 1 d . . . O1 O 0.6366(2) -0.00945(12) 0.96871(14) 0.0250(6) Uani 1 1 d . . . O2 O 0.57125(19) -0.08450(13) 1.03205(14) 0.0256(6) Uani 1 1 d . . . O3 O 0.7720(2) -0.27890(13) 1.08735(15) 0.0311(7) Uani 1 1 d . . . O4 O 0.9414(2) -0.27167(13) 1.08894(14) 0.0289(7) Uani 1 1 d . . . O5 O 1.0966(2) -0.10391(16) 0.96225(19) 0.0474(9) Uani 1 1 d . . . O6 O 1.0054(2) -0.02044(14) 0.92311(15) 0.0326(7) Uani 1 1 d . . . O7 O 1.1435(2) -0.37541(15) 1.09636(15) 0.0353(7) Uani 1 1 d . . . O8 O 1.06998(19) -0.36184(13) 1.19226(14) 0.0248(6) Uani 1 1 d . . . O9 O 1.2637(2) -0.42599(17) 1.40307(16) 0.0429(8) Uani 1 1 d . . . O10 O 1.4324(2) -0.41657(14) 1.40827(14) 0.0296(7) Uani 1 1 d . . . O11 O 1.6077(2) -0.41460(15) 1.19282(16) 0.0363(8) Uani 1 1 d . . . O12 O 1.5095(2) -0.38825(18) 1.10142(16) 0.0462(9) Uani 1 1 d . . . OW1 O 1.6932(4) -0.4763(3) 1.3150(3) 0.1065(17) Uiso 1 1 d . . . Zn1 Zn 0.57445(3) 0.07043(2) 0.99654(2) 0.01991(12) Uani 1 1 d . . . Zn2 Zn 0.93563(3) -0.34659(2) 1.14647(2) 0.02013(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.021(2) 0.030(2) 0.028(2) -0.0010(18) 0.0111(18) 0.0018(17) C2 0.025(2) 0.026(2) 0.036(3) -0.0020(19) 0.0163(19) 0.0010(18) C3 0.0184(19) 0.026(2) 0.026(2) -0.0020(17) 0.0063(17) 0.0004(16) C4 0.033(2) 0.029(2) 0.040(3) -0.007(2) 0.018(2) -0.0121(19) C5 0.101(5) 0.057(4) 0.090(5) -0.046(3) 0.081(4) -0.052(4) C6 0.151(7) 0.081(5) 0.118(6) -0.080(5) 0.114(6) -0.092(5) C7 0.063(4) 0.046(3) 0.063(4) -0.032(3) 0.048(3) -0.033(3) C8 0.030(2) 0.029(2) 0.030(2) -0.0020(19) 0.0102(19) -0.0048(18) C9 0.026(2) 0.026(2) 0.028(2) -0.0063(18) 0.0111(18) -0.0030(17) C10 0.069(4) 0.045(3) 0.059(4) -0.025(3) 0.044(3) -0.036(3) C11 0.111(5) 0.071(4) 0.084(5) -0.051(4) 0.078(4) -0.060(4) C12 0.088(4) 0.051(3) 0.058(4) -0.030(3) 0.044(3) -0.049(3) C13 0.033(2) 0.032(2) 0.031(2) -0.0049(19) 0.014(2) -0.0142(19) C14 0.026(2) 0.030(2) 0.022(2) -0.0037(17) 0.0069(17) -0.0049(18) C15 0.030(2) 0.027(2) 0.025(2) -0.0038(18) 0.0079(19) -0.0077(18) C16 0.023(2) 0.027(2) 0.025(2) -0.0049(17) 0.0067(18) -0.0087(17) C17 0.046(3) 0.082(4) 0.029(3) 0.000(3) 0.000(2) -0.033(3) C18 0.035(3) 0.035(3) 0.084(4) -0.007(3) 0.023(3) -0.006(2) C19 0.024(2) 0.034(2) 0.025(2) -0.0039(18) 0.0080(18) -0.0060(18) C20 0.030(2) 0.039(3) 0.031(2) -0.005(2) 0.003(2) -0.013(2) C21 0.042(3) 0.042(3) 0.024(2) -0.006(2) 0.002(2) -0.017(2) C22 0.146(6) 0.024(3) 0.127(6) -0.017(3) 0.123(6) -0.018(3) C23 0.140(6) 0.023(3) 0.127(6) -0.024(3) 0.114(6) -0.023(3) C24 0.023(2) 0.021(2) 0.026(2) 0.0052(17) 0.0064(17) 0.0012(16) C25 0.035(2) 0.026(2) 0.032(2) -0.0061(19) 0.020(2) -0.0095(19) C26 0.048(3) 0.020(2) 0.050(3) 0.001(2) 0.025(2) 0.003(2) C27 0.049(3) 0.022(2) 0.039(3) 0.0062(19) 0.025(2) 0.003(2) C28 0.031(2) 0.020(2) 0.032(2) -0.0008(17) 0.0138(19) -0.0051(17) C29 0.025(2) 0.025(2) 0.023(2) -0.0035(17) 0.0090(18) -0.0067(17) C30 0.033(2) 0.027(2) 0.023(2) -0.0040(17) 0.0127(19) -0.0110(19) C31 0.024(2) 0.030(2) 0.020(2) -0.0006(17) 0.0095(17) -0.0014(17) C32 0.025(2) 0.030(2) 0.019(2) 0.0011(17) 0.0055(17) -0.0056(18) C33 0.025(2) 0.032(2) 0.022(2) 0.0031(18) 0.0070(18) 0.0020(18) C34 0.026(2) 0.036(2) 0.026(2) -0.0033(19) 0.0115(18) -0.0038(19) C35 0.039(3) 0.035(2) 0.028(2) 0.0085(19) 0.017(2) 0.002(2) C36 0.042(3) 0.030(2) 0.038(3) 0.011(2) 0.016(2) 0.002(2) C37 0.029(2) 0.028(2) 0.028(2) -0.0014(18) 0.0165(19) -0.0043(18) C38 0.040(3) 0.029(2) 0.025(2) 0.0032(18) 0.008(2) 0.0001(19) C39 0.032(2) 0.054(3) 0.029(3) -0.003(2) 0.007(2) -0.001(2) C40 0.039(3) 0.046(3) 0.032(3) 0.005(2) 0.014(2) 0.010(2) C41 0.040(3) 0.060(3) 0.033(3) 0.004(2) 0.010(2) 0.016(2) C42 0.031(2) 0.051(3) 0.030(3) 0.005(2) 0.015(2) -0.001(2) C43 0.024(2) 0.023(2) 0.019(2) -0.0013(16) 0.0035(17) 0.0014(17) C44 0.022(2) 0.019(2) 0.020(2) -0.0007(16) -0.0012(16) 0.0024(16) C45 0.0173(18) 0.0201(19) 0.021(2) 0.0011(16) 0.0007(16) -0.0009(15) C46 0.0166(18) 0.0204(19) 0.019(2) -0.0031(16) 0.0033(16) 0.0004(15) C47 0.0211(19) 0.0179(19) 0.021(2) 0.0026(16) 0.0026(16) 0.0009(15) C48 0.0188(19) 0.023(2) 0.020(2) 0.0001(16) 0.0000(16) -0.0002(16) C49 0.0172(19) 0.022(2) 0.021(2) 0.0003(16) 0.0014(16) 0.0040(16) C50 0.022(2) 0.028(2) 0.028(2) -0.0006(19) 0.0032(18) 0.0009(18) C51 0.0191(19) 0.026(2) 0.0156(19) -0.0034(16) 0.0016(16) 0.0021(16) C52 0.0170(19) 0.0180(19) 0.033(2) 0.0039(17) 0.0018(18) -0.0010(16) C53 0.019(2) 0.019(2) 0.028(2) -0.0001(17) 0.0039(17) -0.0002(16) C54 0.0151(19) 0.024(2) 0.029(2) -0.0020(17) 0.0107(17) 0.0012(16) C55 0.0188(19) 0.025(2) 0.024(2) -0.0011(17) 0.0087(17) 0.0007(16) C56 0.017(2) 0.035(2) 0.026(2) -0.0015(18) 0.0033(17) -0.0006(17) C57 0.018(2) 0.024(2) 0.032(2) -0.0010(18) 0.0097(18) 0.0024(16) C58 0.023(2) 0.022(2) 0.024(2) 0.0000(17) 0.0045(17) 0.0003(16) C59 0.024(2) 0.039(3) 0.030(3) -0.001(2) 0.010(2) -0.0021(19) C60 0.019(2) 0.029(2) 0.032(2) -0.0032(18) 0.0050(18) 0.0000(17) N1 0.037(2) 0.0246(18) 0.035(2) -0.0038(16) 0.0221(18) -0.0043(16) N2 0.044(2) 0.0214(18) 0.038(2) -0.0061(16) 0.0258(19) -0.0095(16) N3 0.0234(18) 0.046(2) 0.0211(18) 0.0038(16) 0.0119(15) 0.0029(16) N4 0.027(2) 0.069(3) 0.030(2) 0.001(2) 0.0115(17) 0.008(2) N5 0.0165(16) 0.0237(17) 0.0241(18) 0.0012(14) 0.0040(14) 0.0025(13) N6 0.0218(17) 0.0265(19) 0.032(2) -0.0020(15) 0.0111(15) -0.0038(14) N7 0.0287(19) 0.0304(19) 0.0244(19) -0.0027(15) 0.0079(16) -0.0102(15) N8 0.0224(17) 0.0274(18) 0.0244(19) -0.0020(15) 0.0053(15) -0.0065(14) O1 0.0262(15) 0.0219(15) 0.0275(16) 0.0048(12) 0.0066(13) 0.0073(12) O2 0.0157(14) 0.0340(16) 0.0278(16) 0.0075(13) 0.0060(12) 0.0042(12) O3 0.0319(16) 0.0254(16) 0.0360(18) 0.0083(13) 0.0029(14) -0.0015(13) O4 0.0302(16) 0.0221(15) 0.0350(17) 0.0092(13) 0.0053(14) 0.0076(12) O5 0.0221(16) 0.050(2) 0.072(3) 0.0252(19) 0.0174(17) 0.0083(15) O6 0.0314(16) 0.0334(17) 0.0341(18) 0.0104(14) 0.0086(14) -0.0018(13) O7 0.0253(16) 0.051(2) 0.0288(18) 0.0047(15) -0.0007(14) 0.0018(14) O8 0.0160(13) 0.0271(15) 0.0316(16) 0.0024(12) 0.0045(12) 0.0045(11) O9 0.0224(16) 0.075(2) 0.0326(18) 0.0002(17) 0.0115(14) -0.0006(16) O10 0.0199(14) 0.0452(18) 0.0238(16) 0.0025(13) 0.0031(12) 0.0000(13) O11 0.0171(15) 0.056(2) 0.0374(19) -0.0030(15) 0.0097(14) 0.0020(14) O12 0.0329(18) 0.078(3) 0.0289(18) 0.0063(17) 0.0112(15) 0.0052(17) Zn1 0.0163(2) 0.0202(2) 0.0239(3) 0.00331(19) 0.00710(18) 0.00194(18) Zn2 0.0169(2) 0.0189(2) 0.0249(3) 0.00300(19) 0.00451(19) 0.00279(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.345(6) . ? C1 N5 1.376(5) . ? C1 H1 0.9300 . ? C2 N6 1.374(5) . ? C2 H2 0.9300 . ? C3 N5 1.327(5) . ? C3 N6 1.340(5) . ? C3 H3 0.9300 . ? C4 C5 1.367(6) . ? C4 C9 1.386(5) . ? C4 N6 1.435(5) . ? C5 C6 1.396(7) . ? C5 H5 0.9300 . ? C6 C7 1.374(7) . ? C6 H6 0.9300 . ? C7 C8 1.383(6) . ? C7 C10 1.469(6) . ? C8 C9 1.381(6) . ? C8 C16 1.521(5) . ? C9 H9 0.9300 . ? C10 C11 1.368(7) . ? C10 C15 1.391(6) . ? C11 C12 1.396(7) . ? C11 H11 0.9300 . ? C12 C13 1.376(6) . ? C12 H12 0.9300 . ? C13 C14 1.379(6) . ? C13 N7 1.437(5) . ? C14 C15 1.382(5) . ? C14 H14 0.9300 . ? C15 C16 1.514(5) . ? C16 C17 1.522(6) . ? C16 C18 1.524(6) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 N8 1.306(5) . ? C19 N7 1.344(5) . ? C19 H19 0.9300 . ? C20 C21 1.345(6) . ? C20 N8 1.373(5) . ? C20 H20 0.9300 . ? C21 N7 1.373(5) . ? C21 H21 0.9300 . ? C22 N1 1.354(6) . ? C22 C23 1.356(7) . ? C22 H22 0.9300 . ? C23 N2 1.363(6) . ? C23 H23 0.9300 . ? C24 N1 1.308(5) . ? C24 N2 1.333(5) . ? C24 H24 0.9300 . ? C25 C30 1.383(6) . ? C25 C26 1.395(6) . ? C25 N2 1.429(5) . ? C26 C27 1.381(6) . ? C26 H26 0.9300 . ? C27 C28 1.382(6) . ? C27 H27 0.9300 . ? C28 C29 1.396(6) . ? C28 C37 1.464(5) . ? C29 C30 1.390(5) . ? C29 C31 1.508(5) . ? C30 H30 0.9300 . ? C31 C32 1.519(5) . ? C31 C38 1.527(6) . ? C31 C39 1.539(6) . ? C32 C33 1.386(5) . ? C32 C37 1.390(6) . ? C33 C34 1.390(6) . ? C33 H33 0.9300 . ? C34 C35 1.387(6) . ? C34 N3 1.435(5) . ? C35 C36 1.375(6) . ? C35 H35 0.9300 . ? C36 C37 1.396(6) . ? C36 H36 0.9300 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 C41 1.349(6) . ? C40 N3 1.377(6) . ? C40 H40 0.9300 . ? C41 N4 1.362(6) . ? C41 H41 0.9300 . ? C42 N4 1.320(6) . ? C42 N3 1.348(5) . ? C42 H42 0.9300 . ? C43 O3 1.231(5) . ? C43 O4 1.279(5) . ? C43 C44 1.507(5) . ? C44 C49 1.387(5) . ? C44 C45 1.389(5) . ? C45 C46 1.387(5) . ? C45 H45 0.9300 . ? C46 C47 1.396(5) . ? C46 C51 1.496(5) . ? C47 C48 1.382(5) . ? C47 H47 0.9300 . ? C48 C49 1.389(5) . ? C48 C50 1.502(5) . ? C49 H49 0.9300 . ? C50 O6 1.201(5) . ? C50 O5 1.332(5) . ? C51 O1 1.260(4) . ? C51 O2 1.262(4) . ? C52 O7 1.237(5) . ? C52 O8 1.277(4) . ? C52 C53 1.496(5) . ? C53 C58 1.386(5) . ? C53 C54 1.394(6) . ? C54 C55 1.389(5) . ? C54 H54 0.9300 . ? C55 C56 1.395(5) . ? C55 C60 1.498(6) . ? C56 C57 1.391(6) . ? C56 H56 0.9300 . ? C57 C58 1.397(5) . ? C57 C59 1.502(5) . ? C58 H58 0.9300 . ? C59 O11 1.219(5) . ? C59 O12 1.301(5) . ? C60 O9 1.233(5) . ? C60 O10 1.275(5) . ? N1 Zn1 1.984(3) . ? N5 Zn2 2.008(3) . ? N8 Zn2 2.024(3) 2_647 ? O1 Zn1 1.961(3) . ? O2 Zn1 1.975(3) 3_657 ? O4 Zn2 1.956(3) . ? O8 Zn2 1.952(3) . ? O10 Zn1 1.941(3) 2_747 ? Zn1 O10 1.941(3) 2_757 ? Zn1 O2 1.975(3) 3_657 ? Zn2 N8 2.024(3) 2_657 ? 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 C2 C1 N5 109.8(3) . . ? C2 C1 H1 125.1 . . ? N5 C1 H1 125.1 . . ? C1 C2 N6 106.2(3) . . ? C1 C2 H2 126.9 . . ? N6 C2 H2 126.9 . . ? N5 C3 N6 110.8(3) . . ? N5 C3 H3 124.6 . . ? N6 C3 H3 124.6 . . ? C5 C4 C9 121.4(4) . . ? C5 C4 N6 118.6(4) . . ? C9 C4 N6 119.9(4) . . ? C4 C5 C6 119.4(5) . . ? C4 C5 H5 120.3 . . ? C6 C5 H5 120.3 . . ? C7 C6 C5 120.0(5) . . ? C7 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? C6 C7 C8 119.8(4) . . ? C6 C7 C10 131.7(4) . . ? C8 C7 C10 108.5(4) . . ? C9 C8 C7 120.9(4) . . ? C9 C8 C16 128.1(4) . . ? C7 C8 C16 111.0(4) . . ? C8 C9 C4 118.5(4) . . ? C8 C9 H9 120.7 . . ? C4 C9 H9 120.7 . . ? C11 C10 C15 120.0(4) . . ? C11 C10 C7 131.7(5) . . ? C15 C10 C7 108.3(4) . . ? C10 C11 C12 119.8(5) . . ? C10 C11 H11 120.1 . . ? C12 C11 H11 120.1 . . ? C13 C12 C11 119.4(5) . . ? C13 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? C12 C13 C14 121.4(4) . . ? C12 C13 N7 119.2(4) . . ? C14 C13 N7 119.5(4) . . ? C13 C14 C15 118.7(4) . . ? C13 C14 H14 120.7 . . ? C15 C14 H14 120.7 . . ? C14 C15 C10 120.6(4) . . ? C14 C15 C16 128.4(4) . . ? C10 C15 C16 111.0(4) . . ? C15 C16 C8 101.2(3) . . ? C15 C16 C17 110.8(4) . . ? C8 C16 C17 112.1(4) . . ? C15 C16 C18 112.0(4) . . ? C8 C16 C18 110.7(4) . . ? C17 C16 C18 109.9(4) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N8 C19 N7 111.3(4) . . ? N8 C19 H19 124.4 . . ? N7 C19 H19 124.4 . . ? C21 C20 N8 109.5(4) . . ? C21 C20 H20 125.2 . . ? N8 C20 H20 125.2 . . ? C20 C21 N7 106.2(4) . . ? C20 C21 H21 126.9 . . ? N7 C21 H21 126.9 . . ? N1 C22 C23 109.8(4) . . ? N1 C22 H22 125.1 . . ? C23 C22 H22 125.1 . . ? C22 C23 N2 106.1(4) . . ? C22 C23 H23 127.0 . . ? N2 C23 H23 127.0 . . ? N1 C24 N2 112.2(4) . . ? N1 C24 H24 123.9 . . ? N2 C24 H24 123.9 . . ? C30 C25 C26 121.9(4) . . ? C30 C25 N2 119.4(4) . . ? C26 C25 N2 118.6(4) . . ? C27 C26 C25 119.6(4) . . ? C27 C26 H26 120.2 . . ? C25 C26 H26 120.2 . . ? C26 C27 C28 119.5(4) . . ? C26 C27 H27 120.3 . . ? C28 C27 H27 120.3 . . ? C27 C28 C29 120.4(4) . . ? C27 C28 C37 131.3(4) . . ? C29 C28 C37 108.3(4) . . ? C30 C29 C28 120.8(4) . . ? C30 C29 C31 127.7(4) . . ? C28 C29 C31 111.5(3) . . ? C25 C30 C29 117.9(4) . . ? C25 C30 H30 121.1 . . ? C29 C30 H30 121.1 . . ? C29 C31 C32 100.6(3) . . ? C29 C31 C38 110.8(3) . . ? C32 C31 C38 111.3(3) . . ? C29 C31 C39 112.4(3) . . ? C32 C31 C39 111.5(3) . . ? C38 C31 C39 109.9(4) . . ? C33 C32 C37 121.0(4) . . ? C33 C32 C31 127.3(4) . . ? C37 C32 C31 111.7(3) . . ? C32 C33 C34 117.9(4) . . ? C32 C33 H33 121.1 . . ? C34 C33 H33 121.1 . . ? C35 C34 C33 121.7(4) . . ? C35 C34 N3 119.6(4) . . ? C33 C34 N3 118.7(4) . . ? C36 C35 C34 120.0(4) . . ? C36 C35 H35 120.0 . . ? C34 C35 H35 120.0 . . ? C35 C36 C37 119.3(4) . . ? C35 C36 H36 120.4 . . ? C37 C36 H36 120.4 . . ? C32 C37 C36 120.1(4) . . ? C32 C37 C28 107.9(4) . . ? C36 C37 C28 131.9(4) . . ? C31 C38 H38A 109.5 . . ? C31 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C31 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C31 C39 H39A 109.5 . . ? C31 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C31 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C41 C40 N3 106.0(4) . . ? C41 C40 H40 127.0 . . ? N3 C40 H40 127.0 . . ? C40 C41 N4 109.8(4) . . ? C40 C41 H41 125.1 . . ? N4 C41 H41 125.1 . . ? N4 C42 N3 110.4(4) . . ? N4 C42 H42 124.8 . . ? N3 C42 H42 124.8 . . ? O3 C43 O4 124.4(4) . . ? O3 C43 C44 120.2(3) . . ? O4 C43 C44 115.4(3) . . ? C49 C44 C45 119.7(3) . . ? C49 C44 C43 121.4(3) . . ? C45 C44 C43 118.9(3) . . ? C46 C45 C44 120.4(3) . . ? C46 C45 H45 119.8 . . ? C44 C45 H45 119.8 . . ? C45 C46 C47 119.6(3) . . ? C45 C46 C51 119.9(3) . . ? C47 C46 C51 120.5(3) . . ? C48 C47 C46 119.9(3) . . ? C48 C47 H47 120.0 . . ? C46 C47 H47 120.0 . . ? C47 C48 C49 120.2(3) . . ? C47 C48 C50 118.2(3) . . ? C49 C48 C50 121.6(3) . . ? C44 C49 C48 120.1(3) . . ? C44 C49 H49 120.0 . . ? C48 C49 H49 120.0 . . ? O6 C50 O5 123.4(4) . . ? O6 C50 C48 123.4(4) . . ? O5 C50 C48 113.2(3) . . ? O1 C51 O2 124.6(3) . . ? O1 C51 C46 117.8(3) . . ? O2 C51 C46 117.6(3) . . ? O7 C52 O8 125.4(4) . . ? O7 C52 C53 119.8(4) . . ? O8 C52 C53 114.8(4) . . ? C58 C53 C54 119.1(4) . . ? C58 C53 C52 119.2(4) . . ? C54 C53 C52 121.6(3) . . ? C55 C54 C53 121.1(3) . . ? C55 C54 H54 119.5 . . ? C53 C54 H54 119.5 . . ? C54 C55 C56 119.2(4) . . ? C54 C55 C60 120.0(3) . . ? C56 C55 C60 120.8(4) . . ? C57 C56 C55 120.4(4) . . ? C57 C56 H56 119.8 . . ? C55 C56 H56 119.8 . . ? C56 C57 C58 119.5(4) . . ? C56 C57 C59 121.1(4) . . ? C58 C57 C59 119.3(4) . . ? C53 C58 C57 120.7(4) . . ? C53 C58 H58 119.6 . . ? C57 C58 H58 119.6 . . ? O11 C59 O12 124.9(4) . . ? O11 C59 C57 122.1(4) . . ? O12 C59 C57 112.9(4) . . ? O9 C60 O10 123.8(4) . . ? O9 C60 C55 120.1(4) . . ? O10 C60 C55 116.1(3) . . ? C24 N1 C22 105.4(3) . . ? C24 N1 Zn1 126.5(3) . . ? C22 N1 Zn1 128.2(3) . . ? C24 N2 C23 106.5(4) . . ? C24 N2 C25 125.8(3) . . ? C23 N2 C25 126.9(4) . . ? C42 N3 C40 107.3(4) . . ? C42 N3 C34 125.5(4) . . ? C40 N3 C34 127.2(4) . . ? C42 N4 C41 106.6(4) . . ? C3 N5 C1 105.6(3) . . ? C3 N5 Zn2 126.8(3) . . ? C1 N5 Zn2 125.4(3) . . ? C3 N6 C2 107.5(3) . . ? C3 N6 C4 125.9(3) . . ? C2 N6 C4 126.5(3) . . ? C19 N7 C21 107.0(3) . . ? C19 N7 C13 126.3(4) . . ? C21 N7 C13 126.7(4) . . ? C19 N8 C20 106.0(3) . . ? C19 N8 Zn2 129.0(3) . 2_647 ? C20 N8 Zn2 124.9(3) . 2_647 ? C51 O1 Zn1 126.0(2) . . ? C51 O2 Zn1 122.7(2) . 3_657 ? C43 O4 Zn2 109.5(2) . . ? C52 O8 Zn2 119.3(3) . . ? C60 O10 Zn1 112.8(3) . 2_747 ? O10 Zn1 O1 116.78(12) 2_757 . ? O10 Zn1 O2 98.85(11) 2_757 3_657 ? O1 Zn1 O2 117.15(12) . 3_657 ? O10 Zn1 N1 116.93(14) 2_757 . ? O1 Zn1 N1 98.94(13) . . ? O2 Zn1 N1 108.94(14) 3_657 . ? O8 Zn2 O4 109.81(12) . . ? O8 Zn2 N5 104.33(12) . . ? O4 Zn2 N5 121.53(13) . . ? O8 Zn2 N8 96.73(12) . 2_657 ? O4 Zn2 N8 112.55(12) . 2_657 ? N5 Zn2 N8 108.73(13) . 2_657 ? 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 N5 C1 C2 N6 -0.8(5) . . . . ? C9 C4 C5 C6 0.5(11) . . . . ? N6 C4 C5 C6 -176.1(7) . . . . ? C4 C5 C6 C7 0.1(13) . . . . ? C5 C6 C7 C8 0.2(13) . . . . ? C5 C6 C7 C10 178.9(8) . . . . ? C6 C7 C8 C9 -1.0(10) . . . . ? C10 C7 C8 C9 180.0(5) . . . . ? C6 C7 C8 C16 177.6(7) . . . . ? C10 C7 C8 C16 -1.5(7) . . . . ? C7 C8 C9 C4 1.5(7) . . . . ? C16 C8 C9 C4 -176.8(4) . . . . ? C5 C4 C9 C8 -1.2(8) . . . . ? N6 C4 C9 C8 175.3(4) . . . . ? C6 C7 C10 C11 4.5(14) . . . . ? C8 C7 C10 C11 -176.6(8) . . . . ? C6 C7 C10 C15 -177.0(8) . . . . ? C8 C7 C10 C15 1.9(7) . . . . ? C15 C10 C11 C12 2.6(11) . . . . ? C7 C10 C11 C12 -179.0(7) . . . . ? C10 C11 C12 C13 -1.8(11) . . . . ? C11 C12 C13 C14 0.5(9) . . . . ? C11 C12 C13 N7 -178.7(6) . . . . ? C12 C13 C14 C15 0.0(7) . . . . ? N7 C13 C14 C15 179.1(4) . . . . ? C13 C14 C15 C10 0.9(7) . . . . ? C13 C14 C15 C16 -178.4(4) . . . . ? C11 C10 C15 C14 -2.2(9) . . . . ? C7 C10 C15 C14 179.1(5) . . . . ? C11 C10 C15 C16 177.2(6) . . . . ? C7 C10 C15 C16 -1.5(7) . . . . ? C14 C15 C16 C8 180.0(4) . . . . ? C10 C15 C16 C8 0.7(5) . . . . ? C14 C15 C16 C17 60.9(6) . . . . ? C10 C15 C16 C17 -118.4(5) . . . . ? C14 C15 C16 C18 -62.1(6) . . . . ? C10 C15 C16 C18 118.6(5) . . . . ? C9 C8 C16 C15 178.9(4) . . . . ? C7 C8 C16 C15 0.5(5) . . . . ? C9 C8 C16 C17 -63.0(6) . . . . ? C7 C8 C16 C17 118.6(5) . . . . ? C9 C8 C16 C18 60.1(6) . . . . ? C7 C8 C16 C18 -118.3(5) . . . . ? N8 C20 C21 N7 -0.1(5) . . . . ? N1 C22 C23 N2 2.1(10) . . . . ? C30 C25 C26 C27 -0.9(7) . . . . ? N2 C25 C26 C27 -176.5(4) . . . . ? C25 C26 C27 C28 3.0(7) . . . . ? C26 C27 C28 C29 -3.3(7) . . . . ? C26 C27 C28 C37 174.5(4) . . . . ? C27 C28 C29 C30 1.6(6) . . . . ? C37 C28 C29 C30 -176.7(4) . . . . ? C27 C28 C29 C31 178.7(4) . . . . ? C37 C28 C29 C31 0.4(5) . . . . ? C26 C25 C30 C29 -0.8(6) . . . . ? N2 C25 C30 C29 174.8(4) . . . . ? C28 C29 C30 C25 0.4(6) . . . . ? C31 C29 C30 C25 -176.2(4) . . . . ? C30 C29 C31 C32 177.1(4) . . . . ? C28 C29 C31 C32 0.2(4) . . . . ? C30 C29 C31 C38 59.3(5) . . . . ? C28 C29 C31 C38 -117.6(4) . . . . ? C30 C29 C31 C39 -64.1(5) . . . . ? C28 C29 C31 C39 119.0(4) . . . . ? C29 C31 C32 C33 -179.0(4) . . . . ? C38 C31 C32 C33 -61.6(5) . . . . ? C39 C31 C32 C33 61.6(5) . . . . ? C29 C31 C32 C37 -0.9(4) . . . . ? C38 C31 C32 C37 116.6(4) . . . . ? C39 C31 C32 C37 -120.3(4) . . . . ? C37 C32 C33 C34 -1.2(6) . . . . ? C31 C32 C33 C34 176.8(4) . . . . ? C32 C33 C34 C35 -0.5(6) . . . . ? C32 C33 C34 N3 179.2(4) . . . . ? C33 C34 C35 C36 2.1(7) . . . . ? N3 C34 C35 C36 -177.6(4) . . . . ? C34 C35 C36 C37 -2.1(7) . . . . ? C33 C32 C37 C36 1.2(6) . . . . ? C31 C32 C37 C36 -177.0(4) . . . . ? C33 C32 C37 C28 179.4(4) . . . . ? C31 C32 C37 C28 1.1(5) . . . . ? C35 C36 C37 C32 0.4(7) . . . . ? C35 C36 C37 C28 -177.2(4) . . . . ? C27 C28 C37 C32 -179.0(5) . . . . ? C29 C28 C37 C32 -1.0(5) . . . . ? C27 C28 C37 C36 -1.1(8) . . . . ? C29 C28 C37 C36 176.9(5) . . . . ? N3 C40 C41 N4 -0.9(6) . . . . ? O3 C43 C44 C49 -168.8(4) . . . . ? O4 C43 C44 C49 10.5(5) . . . . ? O3 C43 C44 C45 13.1(6) . . . . ? O4 C43 C44 C45 -167.6(4) . . . . ? C49 C44 C45 C46 -0.2(6) . . . . ? C43 C44 C45 C46 177.9(3) . . . . ? C44 C45 C46 C47 1.4(6) . . . . ? C44 C45 C46 C51 -178.5(3) . . . . ? C45 C46 C47 C48 -0.9(6) . . . . ? C51 C46 C47 C48 179.0(3) . . . . ? C46 C47 C48 C49 -0.8(6) . . . . ? C46 C47 C48 C50 177.4(4) . . . . ? C45 C44 C49 C48 -1.5(6) . . . . ? C43 C44 C49 C48 -179.6(3) . . . . ? C47 C48 C49 C44 2.0(6) . . . . ? C50 C48 C49 C44 -176.2(4) . . . . ? C47 C48 C50 O6 -2.0(6) . . . . ? C49 C48 C50 O6 176.2(4) . . . . ? C47 C48 C50 O5 178.4(4) . . . . ? C49 C48 C50 O5 -3.4(6) . . . . ? C45 C46 C51 O1 -172.9(3) . . . . ? C47 C46 C51 O1 7.3(6) . . . . ? C45 C46 C51 O2 6.8(5) . . . . ? C47 C46 C51 O2 -173.0(3) . . . . ? O7 C52 C53 C58 11.5(6) . . . . ? O8 C52 C53 C58 -168.9(3) . . . . ? O7 C52 C53 C54 -167.3(4) . . . . ? O8 C52 C53 C54 12.3(5) . . . . ? C58 C53 C54 C55 0.1(6) . . . . ? C52 C53 C54 C55 179.0(4) . . . . ? C53 C54 C55 C56 1.0(6) . . . . ? C53 C54 C55 C60 -177.4(4) . . . . ? C54 C55 C56 C57 -1.7(6) . . . . ? C60 C55 C56 C57 176.6(4) . . . . ? C55 C56 C57 C58 1.4(6) . . . . ? C55 C56 C57 C59 -173.9(4) . . . . ? C54 C53 C58 C57 -0.5(6) . . . . ? C52 C53 C58 C57 -179.4(3) . . . . ? C56 C57 C58 C53 -0.2(6) . . . . ? C59 C57 C58 C53 175.1(4) . . . . ? C56 C57 C59 O11 2.8(7) . . . . ? C58 C57 C59 O11 -172.5(4) . . . . ? C56 C57 C59 O12 -178.3(4) . . . . ? C58 C57 C59 O12 6.4(6) . . . . ? C54 C55 C60 O9 10.1(6) . . . . ? C56 C55 C60 O9 -168.2(4) . . . . ? C54 C55 C60 O10 -171.4(4) . . . . ? C56 C55 C60 O10 10.3(6) . . . . ? N2 C24 N1 C22 2.1(6) . . . . ? N2 C24 N1 Zn1 -176.6(3) . . . . ? C23 C22 N1 C24 -2.6(8) . . . . ? C23 C22 N1 Zn1 176.1(5) . . . . ? N1 C24 N2 C23 -0.8(6) . . . . ? N1 C24 N2 C25 -171.0(4) . . . . ? C22 C23 N2 C24 -0.8(8) . . . . ? C22 C23 N2 C25 169.2(6) . . . . ? C30 C25 N2 C24 -45.9(6) . . . . ? C26 C25 N2 C24 129.9(5) . . . . ? C30 C25 N2 C23 146.0(6) . . . . ? C26 C25 N2 C23 -38.3(8) . . . . ? N4 C42 N3 C40 -0.6(5) . . . . ? N4 C42 N3 C34 177.7(4) . . . . ? C41 C40 N3 C42 0.9(5) . . . . ? C41 C40 N3 C34 -177.4(4) . . . . ? C35 C34 N3 C42 34.1(6) . . . . ? C33 C34 N3 C42 -145.6(4) . . . . ? C35 C34 N3 C40 -147.9(5) . . . . ? C33 C34 N3 C40 32.4(6) . . . . ? N3 C42 N4 C41 0.0(5) . . . . ? C40 C41 N4 C42 0.5(6) . . . . ? N6 C3 N5 C1 0.1(5) . . . . ? N6 C3 N5 Zn2 -163.7(3) . . . . ? C2 C1 N5 C3 0.5(5) . . . . ? C2 C1 N5 Zn2 164.5(3) . . . . ? N5 C3 N6 C2 -0.6(5) . . . . ? N5 C3 N6 C4 -176.6(4) . . . . ? C1 C2 N6 C3 0.9(5) . . . . ? C1 C2 N6 C4 176.8(4) . . . . ? C5 C4 N6 C3 150.3(6) . . . . ? C9 C4 N6 C3 -26.3(7) . . . . ? C5 C4 N6 C2 -24.9(8) . . . . ? C9 C4 N6 C2 158.4(4) . . . . ? N8 C19 N7 C21 -0.6(5) . . . . ? N8 C19 N7 C13 178.5(4) . . . . ? C20 C21 N7 C19 0.4(5) . . . . ? C20 C21 N7 C13 -178.6(4) . . . . ? C12 C13 N7 C19 140.6(5) . . . . ? C14 C13 N7 C19 -38.6(7) . . . . ? C12 C13 N7 C21 -40.5(7) . . . . ? C14 C13 N7 C21 140.3(5) . . . . ? N7 C19 N8 C20 0.5(5) . . . . ? N7 C19 N8 Zn2 -176.2(3) . . . 2_647 ? C21 C20 N8 C19 -0.2(5) . . . . ? C21 C20 N8 Zn2 176.7(3) . . . 2_647 ? O2 C51 O1 Zn1 45.3(5) . . . . ? C46 C51 O1 Zn1 -135.0(3) . . . . ? O1 C51 O2 Zn1 27.1(5) . . . 3_657 ? C46 C51 O2 Zn1 -152.5(3) . . . 3_657 ? O3 C43 O4 Zn2 -10.4(5) . . . . ? C44 C43 O4 Zn2 170.3(3) . . . . ? O7 C52 O8 Zn2 -1.2(5) . . . . ? C53 C52 O8 Zn2 179.1(2) . . . . ? O9 C60 O10 Zn1 -4.4(5) . . . 2_747 ? C55 C60 O10 Zn1 177.1(3) . . . 2_747 ? C51 O1 Zn1 O10 23.6(3) . . . 2_757 ? C51 O1 Zn1 O2 -93.3(3) . . . 3_657 ? C51 O1 Zn1 N1 150.0(3) . . . . ? C24 N1 Zn1 O10 131.5(3) . . . 2_757 ? C22 N1 Zn1 O10 -46.9(6) . . . 2_757 ? C24 N1 Zn1 O1 5.3(4) . . . . ? C22 N1 Zn1 O1 -173.2(6) . . . . ? C24 N1 Zn1 O2 -117.6(4) . . . 3_657 ? C22 N1 Zn1 O2 64.0(6) . . . 3_657 ? C52 O8 Zn2 O4 -60.2(3) . . . . ? C52 O8 Zn2 N5 71.6(3) . . . . ? C52 O8 Zn2 N8 -177.1(3) . . . 2_657 ? C43 O4 Zn2 O8 -160.8(3) . . . . ? C43 O4 Zn2 N5 77.3(3) . . . . ? C43 O4 Zn2 N8 -54.2(3) . . . 2_657 ? C3 N5 Zn2 O8 116.9(3) . . . . ? C1 N5 Zn2 O8 -43.8(3) . . . . ? C3 N5 Zn2 O4 -118.6(3) . . . . ? C1 N5 Zn2 O4 80.7(3) . . . . ? C3 N5 Zn2 N8 14.5(4) . . . 2_657 ? C1 N5 Zn2 N8 -146.2(3) . . . 2_657 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.07 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.926 _refine_diff_density_min -0.536 _refine_diff_density_rms 0.091 _database_code_depnum_ccdc_archive 'CCDC 972074' ####################################################################### # # 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_7 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C81 H66 Cd3 N12 O15' _chemical_formula_sum 'C81 H66 Cd3 N12 O15' _chemical_formula_weight 1784.66 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 13.698(5) _cell_length_b 16.879(5) _cell_length_c 18.153(5) _cell_angle_alpha 110.202(5) _cell_angle_beta 91.837(5) _cell_angle_gamma 109.065(5) _cell_volume 3673(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 14318 _cell_measurement_theta_min 1.61 _cell_measurement_theta_max 26.02 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.614 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1800 _exptl_absorpt_coefficient_mu 0.939 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.758 _exptl_absorpt_correction_T_max 0.804 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 9.00cm _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 20509 _diffrn_reflns_av_R_equivalents 0.0213 _diffrn_reflns_av_sigmaI/netI 0.0470 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.21 _diffrn_reflns_theta_max 26.07 _reflns_number_total 14318 _reflns_number_gt 11526 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXP-97 _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0428P)^2^+6.1346P] 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 14318 _refine_ls_number_parameters 980 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0542 _refine_ls_R_factor_gt 0.0408 _refine_ls_wR_factor_ref 0.1032 _refine_ls_wR_factor_gt 0.0942 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.002 _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 C1 C -0.5615(3) 0.1502(3) 0.5325(2) 0.0325(10) Uani 1 1 d . . . H1 H -0.5088 0.1374 0.5051 0.039 Uiso 1 1 calc R . . C2 C -0.6586(3) 0.1350(3) 0.5003(2) 0.0319(10) Uani 1 1 d . . . H2 H -0.6847 0.1091 0.4461 0.038 Uiso 1 1 calc R . . C3 C -0.6490(3) 0.1951(3) 0.6269(2) 0.0262(9) Uani 1 1 d . . . H3 H -0.6658 0.2189 0.6771 0.031 Uiso 1 1 calc R . . C4 C -0.4657(3) 0.2156(3) 0.6727(2) 0.0255(9) Uani 1 1 d . . . C5 C -0.3658(3) 0.2448(3) 0.6547(2) 0.0260(9) Uani 1 1 d . . . H5 H -0.3560 0.2472 0.6049 0.031 Uiso 1 1 calc R . . C6 C -0.2810(3) 0.2702(3) 0.7124(2) 0.0235(8) Uani 1 1 d . . . C7 C -0.2968(3) 0.2695(3) 0.7880(2) 0.0234(8) Uani 1 1 d . . . C8 C -0.3969(3) 0.2412(3) 0.8056(2) 0.0273(9) Uani 1 1 d . . . H8 H -0.4070 0.2408 0.8559 0.033 Uiso 1 1 calc R . . C9 C -0.4817(3) 0.2135(3) 0.7472(2) 0.0278(9) Uani 1 1 d . . . H9 H -0.5494 0.1935 0.7580 0.033 Uiso 1 1 calc R . . C10 C -0.1941(3) 0.2998(3) 0.8364(2) 0.0235(8) Uani 1 1 d . . . C11 C -0.1171(3) 0.3182(3) 0.7898(2) 0.0272(9) Uani 1 1 d . . . C12 C -0.1653(3) 0.3014(3) 0.7066(2) 0.0278(9) Uani 1 1 d . . . C13 C -0.1297(3) 0.3882(3) 0.6897(3) 0.0422(12) Uani 1 1 d . . . H13A H -0.1611 0.3758 0.6370 0.063 Uiso 1 1 calc R . . H13B H -0.0548 0.4105 0.6939 0.063 Uiso 1 1 calc R . . H13C H -0.1507 0.4329 0.7276 0.063 Uiso 1 1 calc R . . C14 C -0.1387(3) 0.2276(3) 0.6428(3) 0.0410(12) Uani 1 1 d . . . H14A H -0.1701 0.2186 0.5912 0.062 Uiso 1 1 calc R . . H14B H -0.1651 0.1721 0.6518 0.062 Uiso 1 1 calc R . . H14C H -0.0641 0.2459 0.6457 0.062 Uiso 1 1 calc R . . C15 C -0.0123(3) 0.3475(3) 0.8211(2) 0.0280(9) Uani 1 1 d . . . H15 H 0.0395 0.3590 0.7903 0.034 Uiso 1 1 calc R . . C16 C 0.0132(3) 0.3592(3) 0.8991(2) 0.0245(9) Uani 1 1 d . . . C17 C -0.0627(3) 0.3412(3) 0.9463(2) 0.0283(9) Uani 1 1 d . . . H17 H -0.0431 0.3496 0.9988 0.034 Uiso 1 1 calc R . . C18 C -0.1679(3) 0.3106(3) 0.9144(2) 0.0291(9) Uani 1 1 d . . . H18 H -0.2197 0.2976 0.9449 0.035 Uiso 1 1 calc R . . C19 C 0.1876(3) 0.4805(3) 0.9721(3) 0.0356(10) Uani 1 1 d . . . H19 H 0.1712 0.5317 0.9795 0.043 Uiso 1 1 calc R . . C20 C 0.2804(3) 0.4783(3) 0.9962(2) 0.0294(9) Uani 1 1 d . . . H20 H 0.3397 0.5290 1.0236 0.035 Uiso 1 1 calc R . . C21 C 0.1781(3) 0.3407(3) 0.9369(3) 0.0309(10) Uani 1 1 d . . . H21 H 0.1522 0.2777 0.9150 0.037 Uiso 1 1 calc R . . C22 C -0.0379(3) 0.0175(3) 0.6072(2) 0.0230(8) Uani 1 1 d . . . C23 C 0.0259(3) 0.0267(3) 0.6816(2) 0.0215(8) Uani 1 1 d . . . C24 C -0.0004(3) -0.0457(3) 0.7063(2) 0.0254(9) Uani 1 1 d . . . H24 H -0.0610 -0.0958 0.6809 0.031 Uiso 1 1 calc R . . C25 C 0.0625(3) -0.0441(3) 0.7683(2) 0.0265(9) Uani 1 1 d . . . C26 C 0.0401(3) -0.1237(3) 0.7921(2) 0.0302(9) Uani 1 1 d . . . C27 C 0.1510(3) 0.0331(3) 0.8084(2) 0.0231(8) Uani 1 1 d . . . H27 H 0.1938 0.0346 0.8500 0.028 Uiso 1 1 calc R . . C28 C 0.1751(3) 0.1071(3) 0.7868(2) 0.0204(8) Uani 1 1 d . . . C29 C 0.1135(3) 0.1039(3) 0.7224(2) 0.0218(8) Uani 1 1 d . . . H29 H 0.1308 0.1531 0.7067 0.026 Uiso 1 1 calc R . . C30 C 0.2694(3) 0.1904(3) 0.8321(2) 0.0239(8) Uani 1 1 d . . . C31 C -0.8163(3) 0.3464(3) 0.6506(2) 0.0339(11) Uani 1 1 d . . . C32 C -0.7830(3) 0.4394(3) 0.7169(2) 0.0247(9) Uani 1 1 d . . . C33 C -0.8347(3) 0.4981(3) 0.7184(2) 0.0281(9) Uani 1 1 d . . . H33 H -0.8859 0.4830 0.6759 0.034 Uiso 1 1 calc R . . C34 C -0.8101(3) 0.5797(3) 0.7834(3) 0.0294(9) Uani 1 1 d . . . C35 C -0.7266(3) 0.6056(3) 0.8418(2) 0.0272(9) Uani 1 1 d . . . H35 H -0.7083 0.6608 0.8843 0.033 Uiso 1 1 calc R . . C36 C -0.6693(3) 0.5501(3) 0.8379(2) 0.0247(9) Uani 1 1 d . . . C37 C -0.7011(3) 0.4653(3) 0.7773(2) 0.0248(8) Uani 1 1 d . . . H37 H -0.6673 0.4255 0.7772 0.030 Uiso 1 1 calc R . . C38 C -0.8746(3) 0.6379(3) 0.7940(3) 0.0351(10) Uani 1 1 d . . . C39 C -0.5753(3) 0.5853(3) 0.9005(2) 0.0251(9) Uani 1 1 d . . . C40 C -0.9952(4) 0.2445(3) 0.4371(3) 0.0469(13) Uani 1 1 d . . . H40 H -0.9347 0.2934 0.4431 0.056 Uiso 1 1 calc R . . C41 C -1.0881(4) 0.2236(3) 0.3929(3) 0.0452(13) Uani 1 1 d . . . H41 H -1.1033 0.2547 0.3634 0.054 Uiso 1 1 calc R . . C42 C -1.1010(3) 0.1250(3) 0.4485(2) 0.0268(9) Uani 1 1 d . . . H42 H -1.1286 0.0756 0.4632 0.032 Uiso 1 1 calc R . . C43 C -1.2641(3) 0.1021(3) 0.3662(2) 0.0285(9) Uani 1 1 d . . . C44 C -1.2961(3) 0.0966(3) 0.2909(3) 0.0310(10) Uani 1 1 d . . . H44 H -1.2476 0.1190 0.2616 0.037 Uiso 1 1 calc R . . C45 C -1.4017(3) 0.0570(3) 0.2603(2) 0.0289(9) Uani 1 1 d . . . C46 C -1.4742(3) 0.0239(3) 0.3050(2) 0.0266(9) Uani 1 1 d . . . C47 C -1.4407(3) 0.0266(3) 0.3783(2) 0.0301(9) Uani 1 1 d . . . H47 H -1.4887 0.0018 0.4067 0.036 Uiso 1 1 calc R . . C48 C -1.3348(3) 0.0666(3) 0.4098(2) 0.0310(10) Uani 1 1 d . . . H48 H -1.3115 0.0696 0.4597 0.037 Uiso 1 1 calc R . . C49 C -1.5797(3) -0.0105(3) 0.2591(2) 0.0274(9) Uani 1 1 d . . . C50 C -1.5694(3) -0.0018(3) 0.1858(2) 0.0293(9) Uani 1 1 d . . . C51 C -1.4555(3) 0.0422(3) 0.1793(2) 0.0320(10) Uani 1 1 d . . . C52 C -1.4203(4) -0.0209(4) 0.1118(3) 0.0464(13) Uani 1 1 d . . . H52A H -1.3483 0.0090 0.1095 0.070 Uiso 1 1 calc R . . H52B H -1.4628 -0.0365 0.0622 0.070 Uiso 1 1 calc R . . H52C H -1.4277 -0.0749 0.1214 0.070 Uiso 1 1 calc R . . C53 C -1.4366(4) 0.1311(4) 0.1684(3) 0.0482(13) Uani 1 1 d . . . H53A H -1.3643 0.1574 0.1646 0.072 Uiso 1 1 calc R . . H53B H -1.4537 0.1719 0.2132 0.072 Uiso 1 1 calc R . . H53C H -1.4798 0.1202 0.1207 0.072 Uiso 1 1 calc R . . C54 C -1.6588(3) -0.0310(3) 0.1301(3) 0.0317(10) Uani 1 1 d . . . H54 H -1.6536 -0.0260 0.0809 0.038 Uiso 1 1 calc R . . C55 C -1.7554(3) -0.0676(3) 0.1499(2) 0.0300(10) Uani 1 1 d . . . C56 C -1.7652(3) -0.0742(3) 0.2237(3) 0.0338(10) Uani 1 1 d . . . H56 H -1.8313 -0.0981 0.2358 0.041 Uiso 1 1 calc R . . C57 C -1.6768(3) -0.0451(3) 0.2792(3) 0.0318(10) Uani 1 1 d . . . H57 H -1.6825 -0.0488 0.3290 0.038 Uiso 1 1 calc R . . C58 C 0.2700(3) 0.1793(3) 1.0761(2) 0.0328(10) Uani 1 1 d . . . H58 H 0.2332 0.1341 1.0278 0.039 Uiso 1 1 calc R . . C59 C 0.2665(3) 0.1705(3) 1.1477(3) 0.0361(11) Uani 1 1 d . . . H59 H 0.2269 0.1200 1.1576 0.043 Uiso 1 1 calc R . . C60 C 0.3715(3) 0.3056(3) 1.1619(2) 0.0312(10) Uani 1 1 d . . . H60 H 0.4179 0.3651 1.1854 0.037 Uiso 1 1 calc R . . C61 C 0.3650(3) 0.2764(3) 1.2863(2) 0.0290(9) Uani 1 1 d . . . C62 C 0.2915(3) 0.2660(3) 1.3357(2) 0.0317(10) Uani 1 1 d . . . H62 H 0.2205 0.2395 1.3148 0.038 Uiso 1 1 calc R . . C63 C 0.3242(3) 0.2953(3) 1.4174(2) 0.0309(10) Uani 1 1 d . . . H63 H 0.2756 0.2894 1.4516 0.037 Uiso 1 1 calc R . . C64 C 0.4307(3) 0.3335(3) 1.4466(2) 0.0265(9) Uani 1 1 d . . . C65 C 0.5043(3) 0.3408(3) 1.3953(2) 0.0266(9) Uani 1 1 d . . . C66 C 0.4718(3) 0.3131(3) 1.3146(2) 0.0275(9) Uani 1 1 d . . . H66 H 0.5202 0.3189 1.2802 0.033 Uiso 1 1 calc R . . C67 C 0.6152(3) 0.3806(3) 1.4395(2) 0.0282(9) Uani 1 1 d . . . C68 C 0.6682(4) 0.3100(4) 1.4169(3) 0.0432(12) Uani 1 1 d . . . H68A H 0.7384 0.3369 1.4456 0.065 Uiso 1 1 calc R . . H68B H 0.6699 0.2896 1.3608 0.065 Uiso 1 1 calc R . . H68C H 0.6295 0.2596 1.4302 0.065 Uiso 1 1 calc R . . C69 C 0.6811(4) 0.4656(3) 1.4257(3) 0.0415(12) Uani 1 1 d . . . H69A H 0.7508 0.4885 1.4546 0.062 Uiso 1 1 calc R . . H69B H 0.6500 0.5108 1.4439 0.062 Uiso 1 1 calc R . . H69C H 0.6839 0.4506 1.3699 0.062 Uiso 1 1 calc R . . C70 C 0.5954(3) 0.4036(3) 1.5246(2) 0.0261(9) Uani 1 1 d . . . C71 C 0.4885(3) 0.3735(3) 1.5284(2) 0.0266(9) Uani 1 1 d . . . C72 C 0.4549(3) 0.3887(3) 1.6017(2) 0.0294(9) Uani 1 1 d . . . H72 H 0.3840 0.3670 1.6045 0.035 Uiso 1 1 calc R . . C73 C 0.5287(3) 0.4369(3) 1.6708(2) 0.0299(9) Uani 1 1 d . . . H73 H 0.5075 0.4483 1.7204 0.036 Uiso 1 1 calc R . . C74 C 0.6347(3) 0.4678(3) 1.6652(2) 0.0254(9) Uani 1 1 d . . . C75 C 0.6697(3) 0.4508(3) 1.5926(2) 0.0272(9) Uani 1 1 d . . . H75 H 0.7408 0.4706 1.5897 0.033 Uiso 1 1 calc R . . C76 C -1.2046(3) 0.5948(3) 0.7429(2) 0.0284(9) Uani 1 1 d . . . H76 H -1.1896 0.6173 0.7029 0.034 Uiso 1 1 calc R . . C77 C -1.2845(3) 0.5097(3) 0.8066(2) 0.0327(10) Uani 1 1 d . . . H77 H -1.3322 0.4651 0.8198 0.039 Uiso 1 1 calc R . . C78 C -1.1962(3) 0.5754(3) 0.8530(2) 0.0336(10) Uani 1 1 d . . . H78 H -1.1722 0.5833 0.9044 0.040 Uiso 1 1 calc R . . C79 C -0.8610(3) 0.8497(3) 1.0144(2) 0.0321(10) Uani 1 1 d . . . H79 H -0.8079 0.8355 0.9885 0.039 Uiso 1 1 calc R . . C80 C -1.0092(3) 0.8599(3) 1.0380(3) 0.0424(12) Uani 1 1 d . . . H80 H -1.0792 0.8538 1.0308 0.051 Uiso 1 1 calc R . . C81 C -0.9432(3) 0.9050(4) 1.1079(3) 0.0449(13) Uani 1 1 d . . . H81 H -0.9589 0.9346 1.1570 0.054 Uiso 1 1 calc R . . N1 N -0.7137(2) 0.1636(2) 0.5597(2) 0.0289(8) Uani 1 1 d . . . N2 N -0.5547(2) 0.1882(2) 0.61368(19) 0.0258(7) Uani 1 1 d . . . N3 N 0.1222(2) 0.3918(2) 0.93420(19) 0.0257(7) Uani 1 1 d . . . N4 N 0.2744(2) 0.3907(2) 0.97457(19) 0.0266(8) Uani 1 1 d . . . N5 N 0.3354(3) 0.2642(2) 1.08522(19) 0.0308(8) Uani 1 1 d . . . N6 N 0.3334(3) 0.2518(2) 1.20241(19) 0.0286(8) Uani 1 1 d . . . N7 N -1.2894(3) 0.5220(2) 0.73618(19) 0.0260(7) Uani 1 1 d . . . N8 N -1.1465(3) 0.6293(2) 0.8130(2) 0.0282(8) Uani 1 1 d . . . N9 N -0.9575(3) 0.8244(3) 0.9790(2) 0.0341(9) Uani 1 1 d . . . N10 N -0.8485(3) 0.8985(2) 1.0924(2) 0.0324(8) Uani 1 1 d . . . N11 N -1.1556(3) 0.1471(2) 0.4004(2) 0.0294(8) Uani 1 1 d . . . N12 N -1.0038(3) 0.1825(2) 0.4718(2) 0.0306(8) Uani 1 1 d . . . O1 O 0.3053(2) 0.24689(19) 0.80145(15) 0.0272(6) Uani 1 1 d . . . O2 O 0.3041(2) 0.19645(18) 0.90051(16) 0.0336(7) Uani 1 1 d . . . O3 O 0.1149(2) -0.1296(2) 0.8292(2) 0.0394(8) Uani 1 1 d . . . O4 O -0.0507(2) -0.1812(2) 0.77595(19) 0.0369(7) Uani 1 1 d . . . O5 O -0.0081(2) 0.0795(2) 0.58081(16) 0.0306(7) Uani 1 1 d . . . O6 O -0.1177(2) -0.05266(19) 0.57624(16) 0.0292(7) Uani 1 1 d . . . O7 O -0.5127(2) 0.54247(18) 0.89184(16) 0.0281(6) Uani 1 1 d . . . O8 O -0.5591(2) 0.65736(19) 0.95861(16) 0.0317(7) Uani 1 1 d . . . O9 O -0.8721(3) 0.6883(2) 0.8644(2) 0.0474(9) Uani 1 1 d . . . O10 O -0.9294(3) 0.6343(2) 0.7358(2) 0.0485(9) Uiso 1 1 d . . . O11 O -0.8114(3) 0.3376(3) 0.5811(3) 0.0701(12) Uiso 1 1 d . . . O12 O -0.8367(3) 0.2802(2) 0.6694(2) 0.0606(11) Uani 1 1 d . . . OW1 O -1.0626(5) 0.5528(4) 0.5938(4) 0.1136(19) Uiso 1 1 d . . . OW2 O -1.0199(18) 0.4266(16) 0.5250(15) 0.498(13) Uiso 1 1 d . . . OW3 O 0.4752(2) 0.38074(18) 0.89585(16) 0.0270(6) Uani 1 1 d . . . Cd1 Cd -0.87661(2) 0.168189(19) 0.543917(16) 0.02180(8) Uani 1 1 d . . . Cd2 Cd 0.39515(2) 0.331154(19) 0.994284(16) 0.02330(8) Uani 1 1 d . . . Cd3 Cd -0.99439(2) 0.74324(2) 0.845044(18) 0.02792(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.026(2) 0.041(3) 0.022(2) 0.0015(18) 0.0025(17) 0.013(2) C2 0.025(2) 0.039(3) 0.020(2) -0.0005(18) -0.0007(16) 0.0090(19) C3 0.0154(19) 0.031(2) 0.025(2) 0.0032(17) 0.0005(15) 0.0070(17) C4 0.0157(19) 0.026(2) 0.027(2) 0.0026(17) -0.0025(15) 0.0071(16) C5 0.0177(19) 0.032(2) 0.023(2) 0.0042(17) 0.0021(15) 0.0086(17) C6 0.0162(19) 0.027(2) 0.025(2) 0.0060(17) 0.0030(15) 0.0085(16) C7 0.0179(19) 0.024(2) 0.025(2) 0.0046(16) -0.0018(15) 0.0088(16) C8 0.0189(19) 0.037(2) 0.023(2) 0.0081(18) 0.0022(16) 0.0104(18) C9 0.0139(18) 0.034(2) 0.033(2) 0.0107(18) 0.0037(16) 0.0073(17) C10 0.0202(19) 0.024(2) 0.024(2) 0.0060(16) 0.0032(16) 0.0084(16) C11 0.019(2) 0.028(2) 0.028(2) 0.0049(17) -0.0004(16) 0.0068(17) C12 0.0120(18) 0.041(3) 0.026(2) 0.0110(18) 0.0011(15) 0.0060(17) C13 0.021(2) 0.061(3) 0.049(3) 0.032(3) 0.001(2) 0.009(2) C14 0.025(2) 0.060(3) 0.032(2) 0.007(2) 0.0063(19) 0.018(2) C15 0.0170(19) 0.035(2) 0.030(2) 0.0119(18) 0.0041(16) 0.0068(18) C16 0.0139(18) 0.027(2) 0.030(2) 0.0089(17) -0.0006(15) 0.0055(16) C17 0.027(2) 0.035(2) 0.022(2) 0.0091(18) -0.0004(16) 0.0117(19) C18 0.021(2) 0.038(2) 0.026(2) 0.0101(18) 0.0062(16) 0.0095(18) C19 0.025(2) 0.031(2) 0.048(3) 0.014(2) -0.0022(19) 0.0071(19) C20 0.021(2) 0.031(2) 0.032(2) 0.0128(18) 0.0003(17) 0.0028(18) C21 0.021(2) 0.029(2) 0.034(2) 0.0046(18) -0.0024(17) 0.0065(18) C22 0.0167(19) 0.028(2) 0.0180(19) 0.0008(16) -0.0014(15) 0.0083(17) C23 0.0172(18) 0.025(2) 0.0182(19) 0.0043(15) 0.0006(15) 0.0062(16) C24 0.0156(18) 0.025(2) 0.024(2) 0.0047(16) -0.0055(15) -0.0016(16) C25 0.024(2) 0.026(2) 0.026(2) 0.0094(17) 0.0032(16) 0.0053(17) C26 0.026(2) 0.032(2) 0.029(2) 0.0119(18) 0.0014(17) 0.0058(19) C27 0.0195(19) 0.026(2) 0.0187(19) 0.0067(16) -0.0009(15) 0.0049(17) C28 0.0157(18) 0.022(2) 0.0152(18) 0.0016(15) 0.0021(14) 0.0027(16) C29 0.0193(19) 0.024(2) 0.0177(18) 0.0059(15) 0.0007(15) 0.0044(16) C30 0.0197(19) 0.023(2) 0.021(2) 0.0016(16) -0.0006(15) 0.0062(17) C31 0.022(2) 0.042(3) 0.0135(19) 0.0072(18) 0.0024(16) -0.0158(19) C32 0.0157(18) 0.027(2) 0.0206(19) 0.0078(16) 0.0019(15) -0.0041(16) C33 0.0157(19) 0.035(2) 0.029(2) 0.0182(19) -0.0034(16) -0.0023(17) C34 0.020(2) 0.034(2) 0.035(2) 0.0177(19) 0.0010(17) 0.0053(18) C35 0.022(2) 0.024(2) 0.028(2) 0.0078(17) -0.0037(16) 0.0020(17) C36 0.0167(19) 0.025(2) 0.024(2) 0.0086(17) -0.0049(15) -0.0015(16) C37 0.0192(19) 0.024(2) 0.025(2) 0.0075(16) -0.0006(15) 0.0022(16) C38 0.022(2) 0.041(3) 0.045(3) 0.023(2) -0.0019(19) 0.007(2) C39 0.0186(19) 0.025(2) 0.026(2) 0.0107(17) -0.0043(16) 0.0010(17) C40 0.033(3) 0.036(3) 0.067(4) 0.027(3) -0.014(2) 0.001(2) C41 0.033(3) 0.036(3) 0.066(3) 0.029(2) -0.014(2) 0.003(2) C42 0.025(2) 0.026(2) 0.024(2) 0.0030(17) -0.0034(16) 0.0103(18) C43 0.022(2) 0.026(2) 0.029(2) 0.0036(17) -0.0050(17) 0.0062(17) C44 0.022(2) 0.038(2) 0.031(2) 0.0118(19) 0.0001(17) 0.0099(19) C45 0.024(2) 0.035(2) 0.027(2) 0.0074(18) -0.0007(17) 0.0139(19) C46 0.022(2) 0.026(2) 0.026(2) 0.0026(17) -0.0027(16) 0.0094(17) C47 0.027(2) 0.032(2) 0.025(2) 0.0047(18) 0.0001(17) 0.0083(19) C48 0.029(2) 0.033(2) 0.023(2) 0.0036(18) -0.0060(17) 0.0094(19) C49 0.024(2) 0.023(2) 0.026(2) 0.0016(17) -0.0039(16) 0.0063(17) C50 0.023(2) 0.028(2) 0.030(2) 0.0035(18) -0.0029(17) 0.0095(18) C51 0.021(2) 0.043(3) 0.026(2) 0.0084(19) -0.0048(17) 0.0087(19) C52 0.035(3) 0.073(4) 0.025(2) 0.007(2) -0.0020(19) 0.025(3) C53 0.036(3) 0.055(3) 0.053(3) 0.031(3) -0.005(2) 0.005(2) C54 0.026(2) 0.034(2) 0.027(2) 0.0039(18) -0.0054(17) 0.0093(19) C55 0.021(2) 0.029(2) 0.029(2) -0.0005(18) -0.0074(17) 0.0088(18) C56 0.023(2) 0.034(2) 0.033(2) 0.0033(19) 0.0010(18) 0.0072(19) C57 0.028(2) 0.033(2) 0.028(2) 0.0069(18) -0.0006(17) 0.0084(19) C58 0.030(2) 0.029(2) 0.025(2) 0.0052(18) -0.0069(17) -0.0004(19) C59 0.035(2) 0.028(2) 0.031(2) 0.0082(19) -0.0073(19) -0.002(2) C60 0.039(2) 0.023(2) 0.024(2) 0.0081(17) -0.0042(18) 0.0029(19) C61 0.036(2) 0.026(2) 0.020(2) 0.0080(17) -0.0026(17) 0.0066(19) C62 0.026(2) 0.035(2) 0.031(2) 0.0170(19) -0.0011(18) 0.0016(19) C63 0.027(2) 0.036(2) 0.027(2) 0.0153(19) 0.0033(17) 0.0047(19) C64 0.028(2) 0.025(2) 0.023(2) 0.0106(17) 0.0036(17) 0.0037(18) C65 0.027(2) 0.028(2) 0.021(2) 0.0095(17) 0.0015(16) 0.0047(18) C66 0.027(2) 0.031(2) 0.021(2) 0.0097(17) 0.0022(16) 0.0062(18) C67 0.024(2) 0.033(2) 0.023(2) 0.0102(18) 0.0014(16) 0.0046(18) C68 0.041(3) 0.056(3) 0.034(3) 0.013(2) 0.005(2) 0.024(2) C69 0.034(2) 0.048(3) 0.031(2) 0.022(2) 0.0009(19) -0.006(2) C70 0.026(2) 0.027(2) 0.023(2) 0.0119(17) 0.0017(16) 0.0047(18) C71 0.023(2) 0.028(2) 0.024(2) 0.0116(17) 0.0008(16) 0.0022(17) C72 0.023(2) 0.032(2) 0.027(2) 0.0126(18) 0.0021(17) 0.0020(18) C73 0.027(2) 0.037(2) 0.023(2) 0.0122(18) 0.0039(17) 0.0063(19) C74 0.024(2) 0.026(2) 0.023(2) 0.0094(17) -0.0034(16) 0.0046(17) C75 0.0186(19) 0.031(2) 0.028(2) 0.0128(18) 0.0019(16) 0.0020(17) C76 0.027(2) 0.030(2) 0.025(2) 0.0116(18) 0.0008(17) 0.0043(18) C77 0.030(2) 0.039(3) 0.023(2) 0.0135(19) 0.0062(17) 0.003(2) C78 0.028(2) 0.041(3) 0.021(2) 0.0102(19) 0.0004(17) 0.001(2) C79 0.023(2) 0.037(2) 0.029(2) 0.0074(19) -0.0025(17) 0.0075(19) C80 0.021(2) 0.054(3) 0.045(3) 0.011(2) 0.000(2) 0.013(2) C81 0.026(2) 0.058(3) 0.039(3) 0.001(2) -0.001(2) 0.020(2) N1 0.0180(16) 0.031(2) 0.0268(18) 0.0006(15) -0.0043(14) 0.0074(15) N2 0.0164(16) 0.0284(19) 0.0242(17) 0.0020(14) -0.0011(13) 0.0064(14) N3 0.0159(16) 0.0316(19) 0.0258(18) 0.0079(15) -0.0009(13) 0.0074(15) N4 0.0176(16) 0.034(2) 0.0226(17) 0.0067(15) -0.0025(13) 0.0061(15) N5 0.034(2) 0.033(2) 0.0204(17) 0.0088(15) -0.0027(14) 0.0080(17) N6 0.0312(19) 0.0288(19) 0.0207(17) 0.0090(15) -0.0037(14) 0.0057(16) N7 0.0231(17) 0.0259(18) 0.0212(17) 0.0069(14) 0.0000(13) 0.0015(14) N8 0.0225(17) 0.0274(19) 0.0252(18) 0.0059(15) -0.0018(14) 0.0016(15) N9 0.0223(18) 0.037(2) 0.034(2) 0.0109(17) -0.0061(15) 0.0039(16) N10 0.0202(17) 0.037(2) 0.0306(19) 0.0030(16) -0.0052(14) 0.0095(16) N11 0.0220(17) 0.0297(19) 0.0326(19) 0.0099(16) -0.0054(14) 0.0074(15) N12 0.0260(18) 0.0240(18) 0.035(2) 0.0076(15) -0.0089(15) 0.0051(15) O1 0.0220(14) 0.0274(15) 0.0211(14) 0.0062(12) -0.0010(11) -0.0012(12) O2 0.0397(17) 0.0234(15) 0.0244(15) 0.0052(12) -0.0141(13) 0.0005(13) O3 0.0253(16) 0.0384(18) 0.055(2) 0.0304(16) -0.0052(14) -0.0005(14) O4 0.0244(15) 0.0349(17) 0.0454(19) 0.0224(15) -0.0067(13) -0.0034(14) O5 0.0237(15) 0.0391(18) 0.0274(15) 0.0156(13) -0.0020(12) 0.0068(13) O6 0.0197(14) 0.0304(16) 0.0229(14) -0.0002(12) -0.0070(11) 0.0027(12) O7 0.0201(14) 0.0225(15) 0.0347(16) 0.0073(12) -0.0078(12) 0.0036(12) O8 0.0265(15) 0.0258(16) 0.0287(16) 0.0001(13) -0.0118(12) 0.0043(13) O9 0.0406(19) 0.050(2) 0.054(2) 0.0159(18) -0.0034(16) 0.0250(17) O12 0.092(3) 0.034(2) 0.041(2) -0.0025(16) -0.019(2) 0.024(2) OW3 0.0220(14) 0.0250(15) 0.0278(15) 0.0070(12) -0.0004(11) 0.0045(12) Cd1 0.01565(14) 0.02202(15) 0.02039(14) 0.00265(11) -0.00427(10) 0.00394(11) Cd2 0.01833(14) 0.02330(15) 0.02082(15) 0.00462(11) -0.00607(11) 0.00298(12) Cd3 0.02066(15) 0.02818(17) 0.03192(17) 0.01398(13) -0.00448(12) 0.00302(13) _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 C1 C2 1.341(6) . ? C1 N2 1.375(5) . ? C1 H1 0.9300 . ? C2 N1 1.377(5) . ? C2 H2 0.9300 . ? C3 N1 1.317(5) . ? C3 N2 1.356(5) . ? C3 H3 0.9300 . ? C4 C5 1.386(5) . ? C4 C9 1.388(6) . ? C4 N2 1.434(5) . ? C5 C6 1.384(5) . ? C5 H5 0.9300 . ? C6 C7 1.400(6) . ? C6 C12 1.518(5) . ? C7 C8 1.384(5) . ? C7 C10 1.467(5) . ? C8 C9 1.383(5) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 C18 1.384(6) . ? C10 C11 1.396(6) . ? C11 C15 1.385(5) . ? C11 C12 1.523(5) . ? C12 C13 1.527(6) . ? C12 C14 1.534(6) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C16 1.376(6) . ? C15 H15 0.9300 . ? C16 C17 1.392(6) . ? C16 N3 1.449(5) . ? C17 C18 1.391(5) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C20 1.346(6) . ? C19 N3 1.375(5) . ? C19 H19 0.9300 . ? C20 N4 1.366(5) . ? C20 H20 0.9300 . ? C21 N4 1.318(5) . ? C21 N3 1.338(5) . ? C21 H21 0.9300 . ? C22 O6 1.252(5) . ? C22 O5 1.253(5) . ? C22 C23 1.519(5) . ? C23 C24 1.387(6) . ? C23 C29 1.394(5) . ? C24 C25 1.383(5) . ? C24 H24 0.9300 . ? C25 C27 1.397(5) . ? C25 C26 1.490(6) . ? C26 O4 1.252(5) . ? C26 O3 1.258(5) . ? C26 Cd3 2.650(4) 1_645 ? C27 C28 1.380(5) . ? C27 H27 0.9300 . ? C28 C29 1.395(5) . ? C28 C30 1.506(5) . ? C29 H29 0.9300 . ? C30 O1 1.241(5) . ? C30 O2 1.273(5) . ? C31 O11 1.225(5) . ? C31 O12 1.228(6) . ? C31 C32 1.520(6) . ? C32 C33 1.387(6) . ? C32 C37 1.387(5) . ? C33 C34 1.398(6) . ? C33 H33 0.9300 . ? C34 C35 1.378(5) . ? C34 C38 1.493(6) . ? C35 C36 1.393(6) . ? C35 H35 0.9300 . ? C36 C37 1.387(5) . ? C36 C39 1.498(5) . ? C37 H37 0.9300 . ? C38 O10 1.249(5) . ? C38 O9 1.259(6) . ? C38 Cd3 2.753(5) . ? C39 O8 1.251(5) . ? C39 O7 1.272(5) . ? C39 Cd2 2.700(4) 2_567 ? C40 C41 1.355(6) . ? C40 N12 1.372(6) . ? C40 H40 0.9300 . ? C41 N11 1.374(6) . ? C41 H41 0.9300 . ? C42 N12 1.315(5) . ? C42 N11 1.350(5) . ? C42 H42 0.9300 . ? C43 C44 1.384(6) . ? C43 C48 1.385(6) . ? C43 N11 1.432(5) . ? C44 C45 1.382(6) . ? C44 H44 0.9300 . ? C45 C46 1.399(6) . ? C45 C51 1.525(5) . ? C46 C47 1.375(6) . ? C46 C49 1.470(5) . ? C47 C48 1.388(6) . ? C47 H47 0.9300 . ? C48 H48 0.9300 . ? C49 C57 1.384(6) . ? C49 C50 1.395(6) . ? C50 C54 1.395(5) . ? C50 C51 1.521(6) . ? C51 C53 1.520(7) . ? C51 C52 1.530(6) . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C53 H53A 0.9600 . ? C53 H53B 0.9600 . ? C53 H53C 0.9600 . ? C54 C55 1.383(6) . ? C54 H54 0.9300 . ? C55 C56 1.388(6) . ? C55 N10 1.440(5) 1_444 ? C56 C57 1.385(6) . ? C56 H56 0.9300 . ? C57 H57 0.9300 . ? C58 C59 1.358(6) . ? C58 N5 1.368(5) . ? C58 H58 0.9300 . ? C59 N6 1.374(5) . ? C59 H59 0.9300 . ? C60 N5 1.315(5) . ? C60 N6 1.347(5) . ? C60 H60 0.9300 . ? C61 C62 1.380(6) . ? C61 C66 1.388(6) . ? C61 N6 1.443(5) . ? C62 C63 1.396(6) . ? C62 H62 0.9300 . ? C63 C64 1.387(6) . ? C63 H63 0.9300 . ? C64 C65 1.400(6) . ? C64 C71 1.473(5) . ? C65 C66 1.383(5) . ? C65 C67 1.511(5) . ? C66 H66 0.9300 . ? C67 C70 1.514(6) . ? C67 C69 1.534(6) . ? C67 C68 1.536(6) . ? C68 H68A 0.9600 . ? C68 H68B 0.9600 . ? C68 H68C 0.9600 . ? C69 H69A 0.9600 . ? C69 H69B 0.9600 . ? C69 H69C 0.9600 . ? C70 C75 1.380(5) . ? C70 C71 1.396(6) . ? C71 C72 1.389(6) . ? C72 C73 1.392(6) . ? C72 H72 0.9300 . ? C73 C74 1.393(6) . ? C73 H73 0.9300 . ? C74 C75 1.386(6) . ? C74 N7 1.435(5) 1_756 ? C75 H75 0.9300 . ? C76 N8 1.309(5) . ? C76 N7 1.352(5) . ? C76 H76 0.9300 . ? C77 C78 1.348(6) . ? C77 N7 1.367(5) . ? C77 H77 0.9300 . ? C78 N8 1.378(5) . ? C78 H78 0.9300 . ? C79 N9 1.315(5) . ? C79 N10 1.341(5) . ? C79 H79 0.9300 . ? C80 C81 1.348(6) . ? C80 N9 1.375(6) . ? C80 H80 0.9300 . ? C81 N10 1.367(5) . ? C81 H81 0.9300 . ? N1 Cd1 2.270(3) . ? N4 Cd2 2.274(3) . ? N5 Cd2 2.333(4) . ? N7 C74 1.435(5) 1_354 ? N8 Cd3 2.216(3) . ? N9 Cd3 2.283(4) . ? N10 C55 1.440(5) 1_666 ? N12 Cd1 2.270(3) . ? O2 Cd2 2.227(3) . ? O3 Cd3 2.299(3) 1_645 ? O4 Cd3 2.340(3) 1_645 ? O5 Cd1 2.223(3) 1_655 ? O6 Cd1 2.349(3) 2_456 ? O7 Cd2 2.432(3) 2_567 ? O8 Cd2 2.301(3) 2_567 ? O9 Cd3 2.234(3) . ? O10 Cd3 2.602(3) . ? O11 Cd1 2.527(4) . ? O12 Cd1 2.309(3) . ? OW3 Cd2 2.378(3) . ? Cd1 O5 2.223(3) 1_455 ? Cd1 O6 2.349(3) 2_456 ? Cd2 O8 2.301(3) 2_567 ? Cd2 O7 2.432(3) 2_567 ? Cd2 C39 2.700(4) 2_567 ? Cd3 O3 2.299(3) 1_465 ? Cd3 O4 2.340(3) 1_465 ? Cd3 C26 2.650(4) 1_465 ? 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 C2 C1 N2 107.0(4) . . ? C2 C1 H1 126.5 . . ? N2 C1 H1 126.5 . . ? C1 C2 N1 109.7(4) . . ? C1 C2 H2 125.2 . . ? N1 C2 H2 125.2 . . ? N1 C3 N2 111.3(3) . . ? N1 C3 H3 124.3 . . ? N2 C3 H3 124.3 . . ? C5 C4 C9 121.5(4) . . ? C5 C4 N2 119.5(4) . . ? C9 C4 N2 119.0(3) . . ? C6 C5 C4 118.5(4) . . ? C6 C5 H5 120.8 . . ? C4 C5 H5 120.8 . . ? C5 C6 C7 120.2(4) . . ? C5 C6 C12 128.6(4) . . ? C7 C6 C12 111.2(3) . . ? C8 C7 C6 120.7(3) . . ? C8 C7 C10 131.0(4) . . ? C6 C7 C10 108.3(3) . . ? C9 C8 C7 119.1(4) . . ? C9 C8 H8 120.5 . . ? C7 C8 H8 120.5 . . ? C8 C9 C4 120.0(4) . . ? C8 C9 H9 120.0 . . ? C4 C9 H9 120.0 . . ? C18 C10 C11 121.1(4) . . ? C18 C10 C7 130.5(4) . . ? C11 C10 C7 108.4(3) . . ? C15 C11 C10 120.3(4) . . ? C15 C11 C12 128.5(4) . . ? C10 C11 C12 111.2(3) . . ? C6 C12 C11 100.9(3) . . ? C6 C12 C13 111.8(3) . . ? C11 C12 C13 111.1(4) . . ? C6 C12 C14 111.5(3) . . ? C11 C12 C14 111.5(3) . . ? C13 C12 C14 109.8(4) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 C11 118.2(4) . . ? C16 C15 H15 120.9 . . ? C11 C15 H15 120.9 . . ? C15 C16 C17 122.2(3) . . ? C15 C16 N3 119.6(4) . . ? C17 C16 N3 118.2(3) . . ? C18 C17 C16 119.4(4) . . ? C18 C17 H17 120.3 . . ? C16 C17 H17 120.3 . . ? C10 C18 C17 118.7(4) . . ? C10 C18 H18 120.6 . . ? C17 C18 H18 120.6 . . ? C20 C19 N3 106.2(4) . . ? C20 C19 H19 126.9 . . ? N3 C19 H19 126.9 . . ? C19 C20 N4 109.9(4) . . ? C19 C20 H20 125.0 . . ? N4 C20 H20 125.0 . . ? N4 C21 N3 111.4(4) . . ? N4 C21 H21 124.3 . . ? N3 C21 H21 124.3 . . ? O6 C22 O5 124.5(4) . . ? O6 C22 C23 116.8(4) . . ? O5 C22 C23 118.7(3) . . ? C24 C23 C29 119.8(3) . . ? C24 C23 C22 118.9(3) . . ? C29 C23 C22 121.2(4) . . ? C25 C24 C23 120.7(3) . . ? C25 C24 H24 119.6 . . ? C23 C24 H24 119.6 . . ? C24 C25 C27 119.2(4) . . ? C24 C25 C26 121.7(4) . . ? C27 C25 C26 119.1(4) . . ? O4 C26 O3 122.1(4) . . ? O4 C26 C25 120.3(4) . . ? O3 C26 C25 117.6(4) . . ? O4 C26 Cd3 62.0(2) . 1_645 ? O3 C26 Cd3 60.2(2) . 1_645 ? C25 C26 Cd3 175.8(3) . 1_645 ? C28 C27 C25 120.5(4) . . ? C28 C27 H27 119.7 . . ? C25 C27 H27 119.7 . . ? C27 C28 C29 120.0(3) . . ? C27 C28 C30 119.5(3) . . ? C29 C28 C30 120.5(4) . . ? C23 C29 C28 119.7(4) . . ? C23 C29 H29 120.2 . . ? C28 C29 H29 120.2 . . ? O1 C30 O2 125.8(4) . . ? O1 C30 C28 118.7(3) . . ? O2 C30 C28 115.4(4) . . ? O11 C31 O12 120.0(5) . . ? O11 C31 C32 121.5(4) . . ? O12 C31 C32 118.0(4) . . ? C33 C32 C37 119.6(4) . . ? C33 C32 C31 120.8(4) . . ? C37 C32 C31 119.6(4) . . ? C32 C33 C34 120.4(4) . . ? C32 C33 H33 119.8 . . ? C34 C33 H33 119.8 . . ? C35 C34 C33 119.1(4) . . ? C35 C34 C38 118.6(4) . . ? C33 C34 C38 122.2(4) . . ? C34 C35 C36 120.8(4) . . ? C34 C35 H35 119.6 . . ? C36 C35 H35 119.6 . . ? C37 C36 C35 119.4(3) . . ? C37 C36 C39 122.8(4) . . ? C35 C36 C39 117.8(3) . . ? C36 C37 C32 120.3(4) . . ? C36 C37 H37 119.9 . . ? C32 C37 H37 119.9 . . ? O10 C38 O9 122.7(4) . . ? O10 C38 C34 121.0(4) . . ? O9 C38 C34 116.2(4) . . ? O10 C38 Cd3 69.9(3) . . ? O9 C38 Cd3 53.0(2) . . ? C34 C38 Cd3 167.8(3) . . ? O8 C39 O7 122.0(3) . . ? O8 C39 C36 119.0(4) . . ? O7 C39 C36 119.0(4) . . ? O8 C39 Cd2 58.17(19) . 2_567 ? O7 C39 Cd2 64.15(19) . 2_567 ? C36 C39 Cd2 171.6(3) . 2_567 ? C41 C40 N12 109.6(4) . . ? C41 C40 H40 125.2 . . ? N12 C40 H40 125.2 . . ? C40 C41 N11 106.2(4) . . ? C40 C41 H41 126.9 . . ? N11 C41 H41 126.9 . . ? N12 C42 N11 111.3(4) . . ? N12 C42 H42 124.4 . . ? N11 C42 H42 124.4 . . ? C44 C43 C48 121.6(4) . . ? C44 C43 N11 119.1(4) . . ? C48 C43 N11 119.3(4) . . ? C45 C44 C43 118.5(4) . . ? C45 C44 H44 120.8 . . ? C43 C44 H44 120.8 . . ? C44 C45 C46 120.4(4) . . ? C44 C45 C51 128.2(4) . . ? C46 C45 C51 111.4(3) . . ? C47 C46 C45 120.3(4) . . ? C47 C46 C49 131.4(4) . . ? C45 C46 C49 108.3(4) . . ? C46 C47 C48 119.7(4) . . ? C46 C47 H47 120.2 . . ? C48 C47 H47 120.2 . . ? C43 C48 C47 119.4(4) . . ? C43 C48 H48 120.3 . . ? C47 C48 H48 120.3 . . ? C57 C49 C50 121.7(4) . . ? C57 C49 C46 130.3(4) . . ? C50 C49 C46 108.0(4) . . ? C49 C50 C54 119.5(4) . . ? C49 C50 C51 111.9(3) . . ? C54 C50 C51 128.6(4) . . ? C53 C51 C50 111.3(4) . . ? C53 C51 C45 111.7(4) . . ? C50 C51 C45 100.4(3) . . ? C53 C51 C52 110.2(4) . . ? C50 C51 C52 111.8(4) . . ? C45 C51 C52 111.1(4) . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C51 C53 H53A 109.5 . . ? C51 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C51 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C55 C54 C50 118.4(4) . . ? C55 C54 H54 120.8 . . ? C50 C54 H54 120.8 . . ? C54 C55 C56 121.8(4) . . ? C54 C55 N10 119.5(4) . 1_444 ? C56 C55 N10 118.7(4) . 1_444 ? C57 C56 C55 120.0(4) . . ? C57 C56 H56 120.0 . . ? C55 C56 H56 120.0 . . ? C49 C57 C56 118.5(4) . . ? C49 C57 H57 120.8 . . ? C56 C57 H57 120.8 . . ? C59 C58 N5 110.4(4) . . ? C59 C58 H58 124.8 . . ? N5 C58 H58 124.8 . . ? C58 C59 N6 105.8(4) . . ? C58 C59 H59 127.1 . . ? N6 C59 H59 127.1 . . ? N5 C60 N6 112.1(4) . . ? N5 C60 H60 123.9 . . ? N6 C60 H60 123.9 . . ? C62 C61 C66 122.2(4) . . ? C62 C61 N6 120.8(4) . . ? C66 C61 N6 117.0(4) . . ? C61 C62 C63 119.6(4) . . ? C61 C62 H62 120.2 . . ? C63 C62 H62 120.2 . . ? C64 C63 C62 118.7(4) . . ? C64 C63 H63 120.6 . . ? C62 C63 H63 120.6 . . ? C63 C64 C65 120.9(4) . . ? C63 C64 C71 131.4(4) . . ? C65 C64 C71 107.7(3) . . ? C66 C65 C64 120.3(4) . . ? C66 C65 C67 127.9(4) . . ? C64 C65 C67 111.8(3) . . ? C65 C66 C61 118.2(4) . . ? C65 C66 H66 120.9 . . ? C61 C66 H66 120.9 . . ? C65 C67 C70 100.6(3) . . ? C65 C67 C69 112.1(4) . . ? C70 C67 C69 111.2(4) . . ? C65 C67 C68 111.0(4) . . ? C70 C67 C68 111.2(4) . . ? C69 C67 C68 110.4(4) . . ? C67 C68 H68A 109.5 . . ? C67 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C67 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C67 C69 H69A 109.5 . . ? C67 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C67 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? C75 C70 C71 121.5(4) . . ? C75 C70 C67 126.8(4) . . ? C71 C70 C67 111.7(3) . . ? C72 C71 C70 120.1(4) . . ? C72 C71 C64 131.9(4) . . ? C70 C71 C64 108.0(3) . . ? C71 C72 C73 119.2(4) . . ? C71 C72 H72 120.4 . . ? C73 C72 H72 120.4 . . ? C72 C73 C74 119.4(4) . . ? C72 C73 H73 120.3 . . ? C74 C73 H73 120.3 . . ? C75 C74 C73 122.1(4) . . ? C75 C74 N7 118.2(3) . 1_756 ? C73 C74 N7 119.6(3) . 1_756 ? C70 C75 C74 117.6(4) . . ? C70 C75 H75 121.2 . . ? C74 C75 H75 121.2 . . ? N8 C76 N7 111.2(4) . . ? N8 C76 H76 124.4 . . ? N7 C76 H76 124.4 . . ? C78 C77 N7 105.9(4) . . ? C78 C77 H77 127.1 . . ? N7 C77 H77 127.1 . . ? C77 C78 N8 110.1(4) . . ? C77 C78 H78 124.9 . . ? N8 C78 H78 124.9 . . ? N9 C79 N10 111.7(4) . . ? N9 C79 H79 124.1 . . ? N10 C79 H79 124.1 . . ? C81 C80 N9 109.8(4) . . ? C81 C80 H80 125.1 . . ? N9 C80 H80 125.1 . . ? C80 C81 N10 106.4(4) . . ? C80 C81 H81 126.8 . . ? N10 C81 H81 126.8 . . ? C3 N1 C2 105.7(3) . . ? C3 N1 Cd1 127.2(3) . . ? C2 N1 Cd1 126.8(3) . . ? C3 N2 C1 106.3(3) . . ? C3 N2 C4 126.7(3) . . ? C1 N2 C4 127.0(3) . . ? C21 N3 C19 106.9(3) . . ? C21 N3 C16 126.2(3) . . ? C19 N3 C16 126.9(3) . . ? C21 N4 C20 105.6(3) . . ? C21 N4 Cd2 123.1(3) . . ? C20 N4 Cd2 131.3(3) . . ? C60 N5 C58 105.0(4) . . ? C60 N5 Cd2 122.1(3) . . ? C58 N5 Cd2 132.6(3) . . ? C60 N6 C59 106.7(3) . . ? C60 N6 C61 124.6(3) . . ? C59 N6 C61 128.6(4) . . ? C76 N7 C77 107.3(3) . . ? C76 N7 C74 124.1(3) . 1_354 ? C77 N7 C74 128.5(3) . 1_354 ? C76 N8 C78 105.4(3) . . ? C76 N8 Cd3 122.6(3) . . ? C78 N8 Cd3 131.7(3) . . ? C79 N9 C80 105.2(4) . . ? C79 N9 Cd3 117.3(3) . . ? C80 N9 Cd3 137.5(3) . . ? C79 N10 C81 106.9(4) . . ? C79 N10 C55 126.7(4) . 1_666 ? C81 N10 C55 126.2(4) . 1_666 ? C42 N11 C41 106.9(3) . . ? C42 N11 C43 126.9(4) . . ? C41 N11 C43 126.1(4) . . ? C42 N12 C40 105.9(4) . . ? C42 N12 Cd1 125.0(3) . . ? C40 N12 Cd1 128.8(3) . . ? C30 O2 Cd2 120.3(3) . . ? C26 O3 Cd3 91.5(2) . 1_645 ? C26 O4 Cd3 89.8(3) . 1_645 ? C22 O5 Cd1 146.9(3) . 1_655 ? C22 O6 Cd1 121.7(2) . 2_456 ? C39 O7 Cd2 87.8(2) . 2_567 ? C39 O8 Cd2 94.3(2) . 2_567 ? C38 O9 Cd3 100.2(3) . . ? C38 O10 Cd3 83.4(3) . . ? C31 O11 Cd1 88.6(3) . . ? C31 O12 Cd1 99.1(3) . . ? O5 Cd1 N12 85.26(12) 1_455 . ? O5 Cd1 N1 120.10(12) 1_455 . ? N12 Cd1 N1 149.67(13) . . ? O5 Cd1 O12 90.58(14) 1_455 . ? N12 Cd1 O12 108.14(13) . . ? N1 Cd1 O12 89.26(13) . . ? O5 Cd1 O6 94.24(10) 1_455 2_456 ? N12 Cd1 O6 83.60(11) . 2_456 ? N1 Cd1 O6 78.50(10) . 2_456 ? O12 Cd1 O6 167.67(12) . 2_456 ? O5 Cd1 O11 130.01(13) 1_455 . ? N12 Cd1 O11 78.78(13) . . ? N1 Cd1 O11 94.15(13) . . ? O12 Cd1 O11 51.86(14) . . ? O6 Cd1 O11 129.84(13) 2_456 . ? O2 Cd2 N4 92.58(12) . . ? O2 Cd2 O8 113.07(10) . 2_567 ? N4 Cd2 O8 152.99(11) . 2_567 ? O2 Cd2 N5 85.98(12) . . ? N4 Cd2 N5 104.72(13) . . ? O8 Cd2 N5 86.15(12) 2_567 . ? O2 Cd2 OW3 89.95(10) . . ? N4 Cd2 OW3 85.74(11) . . ? O8 Cd2 OW3 85.97(10) 2_567 . ? N5 Cd2 OW3 168.92(11) . . ? O2 Cd2 O7 166.41(10) . 2_567 ? N4 Cd2 O7 100.00(11) . 2_567 ? O8 Cd2 O7 55.49(9) 2_567 2_567 ? N5 Cd2 O7 85.87(11) . 2_567 ? OW3 Cd2 O7 96.04(10) . 2_567 ? O2 Cd2 C39 139.72(12) . 2_567 ? N4 Cd2 C39 127.70(12) . 2_567 ? O8 Cd2 C39 27.51(11) 2_567 2_567 ? N5 Cd2 C39 83.73(12) . 2_567 ? OW3 Cd2 C39 92.81(11) . 2_567 ? O7 Cd2 C39 28.08(11) 2_567 2_567 ? N8 Cd3 O9 106.31(13) . . ? N8 Cd3 N9 110.70(13) . . ? O9 Cd3 N9 86.53(13) . . ? N8 Cd3 O3 150.38(12) . 1_465 ? O9 Cd3 O3 97.37(12) . 1_465 ? N9 Cd3 O3 87.88(13) . 1_465 ? N8 Cd3 O4 94.49(12) . 1_465 ? O9 Cd3 O4 145.82(13) . 1_465 ? N9 Cd3 O4 111.46(13) . 1_465 ? O3 Cd3 O4 56.50(10) 1_465 1_465 ? N8 Cd3 O10 86.64(12) . . ? O9 Cd3 O10 53.49(12) . . ? N9 Cd3 O10 139.89(12) . . ? O3 Cd3 O10 93.62(12) 1_465 . ? O4 Cd3 O10 102.43(12) 1_465 . ? N8 Cd3 C26 122.57(13) . 1_465 ? O9 Cd3 C26 123.28(13) . 1_465 ? N9 Cd3 C26 100.07(13) . 1_465 ? O3 Cd3 C26 28.33(11) 1_465 1_465 ? O4 Cd3 C26 28.20(11) 1_465 1_465 ? O10 Cd3 C26 99.89(12) . 1_465 ? N8 Cd3 C38 96.09(13) . . ? O9 Cd3 C38 26.75(12) . . ? N9 Cd3 C38 113.28(13) . . ? O3 Cd3 C38 97.29(13) 1_465 . ? O4 Cd3 C38 126.34(13) 1_465 . ? O10 Cd3 C38 26.78(12) . . ? C26 Cd3 C38 114.81(14) 1_465 . ? 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 N2 C1 C2 N1 0.6(5) . . . . ? C9 C4 C5 C6 1.5(6) . . . . ? N2 C4 C5 C6 -179.5(4) . . . . ? C4 C5 C6 C7 -2.5(6) . . . . ? C4 C5 C6 C12 177.9(4) . . . . ? C5 C6 C7 C8 1.8(6) . . . . ? C12 C6 C7 C8 -178.5(4) . . . . ? C5 C6 C7 C10 -179.6(4) . . . . ? C12 C6 C7 C10 0.1(5) . . . . ? C6 C7 C8 C9 -0.1(6) . . . . ? C10 C7 C8 C9 -178.3(4) . . . . ? C7 C8 C9 C4 -0.9(6) . . . . ? C5 C4 C9 C8 0.2(6) . . . . ? N2 C4 C9 C8 -178.8(4) . . . . ? C8 C7 C10 C18 -1.5(7) . . . . ? C6 C7 C10 C18 -179.9(4) . . . . ? C8 C7 C10 C11 178.1(4) . . . . ? C6 C7 C10 C11 -0.3(5) . . . . ? C18 C10 C11 C15 0.2(6) . . . . ? C7 C10 C11 C15 -179.4(4) . . . . ? C18 C10 C11 C12 -180.0(4) . . . . ? C7 C10 C11 C12 0.4(5) . . . . ? C5 C6 C12 C11 179.8(4) . . . . ? C7 C6 C12 C11 0.1(4) . . . . ? C5 C6 C12 C13 61.6(6) . . . . ? C7 C6 C12 C13 -118.0(4) . . . . ? C5 C6 C12 C14 -61.7(6) . . . . ? C7 C6 C12 C14 118.6(4) . . . . ? C15 C11 C12 C6 179.5(4) . . . . ? C10 C11 C12 C6 -0.3(4) . . . . ? C15 C11 C12 C13 -61.8(6) . . . . ? C10 C11 C12 C13 118.4(4) . . . . ? C15 C11 C12 C14 61.0(6) . . . . ? C10 C11 C12 C14 -118.8(4) . . . . ? C10 C11 C15 C16 -1.1(6) . . . . ? C12 C11 C15 C16 179.1(4) . . . . ? C11 C15 C16 C17 1.0(6) . . . . ? C11 C15 C16 N3 -178.6(4) . . . . ? C15 C16 C17 C18 -0.1(6) . . . . ? N3 C16 C17 C18 179.5(4) . . . . ? C11 C10 C18 C17 0.7(6) . . . . ? C7 C10 C18 C17 -179.7(4) . . . . ? C16 C17 C18 C10 -0.7(6) . . . . ? N3 C19 C20 N4 -0.1(5) . . . . ? O6 C22 C23 C24 6.7(5) . . . . ? O5 C22 C23 C24 -173.3(4) . . . . ? O6 C22 C23 C29 -177.3(3) . . . . ? O5 C22 C23 C29 2.7(5) . . . . ? C29 C23 C24 C25 -3.5(6) . . . . ? C22 C23 C24 C25 172.6(4) . . . . ? C23 C24 C25 C27 2.8(6) . . . . ? C23 C24 C25 C26 -175.5(4) . . . . ? C24 C25 C26 O4 -23.4(6) . . . . ? C27 C25 C26 O4 158.3(4) . . . . ? C24 C25 C26 O3 157.5(4) . . . . ? C27 C25 C26 O3 -20.8(6) . . . . ? C24 C25 C26 Cd3 -146(4) . . . 1_645 ? C27 C25 C26 Cd3 35(4) . . . 1_645 ? C24 C25 C27 C28 0.3(6) . . . . ? C26 C25 C27 C28 178.6(4) . . . . ? C25 C27 C28 C29 -2.6(6) . . . . ? C25 C27 C28 C30 178.5(3) . . . . ? C24 C23 C29 C28 1.2(6) . . . . ? C22 C23 C29 C28 -174.9(3) . . . . ? C27 C28 C29 C23 1.8(6) . . . . ? C30 C28 C29 C23 -179.2(3) . . . . ? C27 C28 C30 O1 162.5(4) . . . . ? C29 C28 C30 O1 -16.4(5) . . . . ? C27 C28 C30 O2 -18.4(5) . . . . ? C29 C28 C30 O2 162.7(4) . . . . ? O11 C31 C32 C33 62.6(6) . . . . ? O12 C31 C32 C33 -125.9(5) . . . . ? O11 C31 C32 C37 -118.5(5) . . . . ? O12 C31 C32 C37 53.1(6) . . . . ? C37 C32 C33 C34 -5.0(6) . . . . ? C31 C32 C33 C34 173.9(4) . . . . ? C32 C33 C34 C35 6.9(6) . . . . ? C32 C33 C34 C38 -170.0(4) . . . . ? C33 C34 C35 C36 -2.2(6) . . . . ? C38 C34 C35 C36 174.8(4) . . . . ? C34 C35 C36 C37 -4.3(6) . . . . ? C34 C35 C36 C39 176.0(4) . . . . ? C35 C36 C37 C32 6.2(6) . . . . ? C39 C36 C37 C32 -174.2(4) . . . . ? C33 C32 C37 C36 -1.5(6) . . . . ? C31 C32 C37 C36 179.5(4) . . . . ? C35 C34 C38 O10 158.6(4) . . . . ? C33 C34 C38 O10 -24.5(7) . . . . ? C35 C34 C38 O9 -23.1(6) . . . . ? C33 C34 C38 O9 153.8(4) . . . . ? C35 C34 C38 Cd3 -49.7(16) . . . . ? C33 C34 C38 Cd3 127.2(13) . . . . ? C37 C36 C39 O8 -171.1(4) . . . . ? C35 C36 C39 O8 8.5(6) . . . . ? C37 C36 C39 O7 10.9(6) . . . . ? C35 C36 C39 O7 -169.5(4) . . . . ? C37 C36 C39 Cd2 121.0(19) . . . 2_567 ? C35 C36 C39 Cd2 -59(2) . . . 2_567 ? N12 C40 C41 N11 0.0(6) . . . . ? C48 C43 C44 C45 2.0(6) . . . . ? N11 C43 C44 C45 -176.8(4) . . . . ? C43 C44 C45 C46 0.4(6) . . . . ? C43 C44 C45 C51 -179.2(4) . . . . ? C44 C45 C46 C47 -3.0(6) . . . . ? C51 C45 C46 C47 176.6(4) . . . . ? C44 C45 C46 C49 177.7(4) . . . . ? C51 C45 C46 C49 -2.7(5) . . . . ? C45 C46 C47 C48 3.3(6) . . . . ? C49 C46 C47 C48 -177.6(4) . . . . ? C44 C43 C48 C47 -1.7(6) . . . . ? N11 C43 C48 C47 177.0(4) . . . . ? C46 C47 C48 C43 -0.9(6) . . . . ? C47 C46 C49 C57 4.7(8) . . . . ? C45 C46 C49 C57 -176.0(4) . . . . ? C47 C46 C49 C50 -176.4(4) . . . . ? C45 C46 C49 C50 2.9(5) . . . . ? C57 C49 C50 C54 -1.9(6) . . . . ? C46 C49 C50 C54 179.2(4) . . . . ? C57 C49 C50 C51 177.1(4) . . . . ? C46 C49 C50 C51 -1.9(5) . . . . ? C49 C50 C51 C53 -118.0(4) . . . . ? C54 C50 C51 C53 60.8(6) . . . . ? C49 C50 C51 C45 0.3(5) . . . . ? C54 C50 C51 C45 179.1(4) . . . . ? C49 C50 C51 C52 118.2(4) . . . . ? C54 C50 C51 C52 -62.9(6) . . . . ? C44 C45 C51 C53 -60.9(6) . . . . ? C46 C45 C51 C53 119.5(4) . . . . ? C44 C45 C51 C50 -178.9(4) . . . . ? C46 C45 C51 C50 1.5(5) . . . . ? C44 C45 C51 C52 62.6(6) . . . . ? C46 C45 C51 C52 -116.9(4) . . . . ? C49 C50 C54 C55 0.2(6) . . . . ? C51 C50 C54 C55 -178.5(4) . . . . ? C50 C54 C55 C56 1.3(6) . . . . ? C50 C54 C55 N10 -177.5(4) . . . 1_444 ? C54 C55 C56 C57 -1.2(7) . . . . ? N10 C55 C56 C57 177.7(4) 1_444 . . . ? C50 C49 C57 C56 2.0(6) . . . . ? C46 C49 C57 C56 -179.3(4) . . . . ? C55 C56 C57 C49 -0.5(6) . . . . ? N5 C58 C59 N6 -1.3(5) . . . . ? C66 C61 C62 C63 1.8(7) . . . . ? N6 C61 C62 C63 -176.1(4) . . . . ? C61 C62 C63 C64 -0.7(7) . . . . ? C62 C63 C64 C65 -1.4(7) . . . . ? C62 C63 C64 C71 177.2(4) . . . . ? C63 C64 C65 C66 2.5(6) . . . . ? C71 C64 C65 C66 -176.3(4) . . . . ? C63 C64 C65 C67 -177.5(4) . . . . ? C71 C64 C65 C67 3.7(5) . . . . ? C64 C65 C66 C61 -1.4(6) . . . . ? C67 C65 C66 C61 178.6(4) . . . . ? C62 C61 C66 C65 -0.7(7) . . . . ? N6 C61 C66 C65 177.3(4) . . . . ? C66 C65 C67 C70 174.8(4) . . . . ? C64 C65 C67 C70 -5.2(5) . . . . ? C66 C65 C67 C69 56.5(6) . . . . ? C64 C65 C67 C69 -123.5(4) . . . . ? C66 C65 C67 C68 -67.5(6) . . . . ? C64 C65 C67 C68 112.5(4) . . . . ? C65 C67 C70 C75 -172.8(4) . . . . ? C69 C67 C70 C75 -53.9(6) . . . . ? C68 C67 C70 C75 69.5(6) . . . . ? C65 C67 C70 C71 5.0(5) . . . . ? C69 C67 C70 C71 124.0(4) . . . . ? C68 C67 C70 C71 -112.6(4) . . . . ? C75 C70 C71 C72 -1.8(7) . . . . ? C67 C70 C71 C72 -179.8(4) . . . . ? C75 C70 C71 C64 174.8(4) . . . . ? C67 C70 C71 C64 -3.2(5) . . . . ? C63 C64 C71 C72 -2.9(8) . . . . ? C65 C64 C71 C72 175.8(5) . . . . ? C63 C64 C71 C70 -179.0(5) . . . . ? C65 C64 C71 C70 -0.3(5) . . . . ? C70 C71 C72 C73 2.2(6) . . . . ? C64 C71 C72 C73 -173.4(4) . . . . ? C71 C72 C73 C74 -0.8(7) . . . . ? C72 C73 C74 C75 -1.3(7) . . . . ? C72 C73 C74 N7 176.4(4) . . . 1_756 ? C71 C70 C75 C74 -0.2(6) . . . . ? C67 C70 C75 C74 177.5(4) . . . . ? C73 C74 C75 C70 1.7(6) . . . . ? N7 C74 C75 C70 -175.9(4) 1_756 . . . ? N7 C77 C78 N8 0.8(5) . . . . ? N9 C80 C81 N10 0.7(6) . . . . ? N2 C3 N1 C2 0.1(5) . . . . ? N2 C3 N1 Cd1 -174.5(3) . . . . ? C1 C2 N1 C3 -0.4(5) . . . . ? C1 C2 N1 Cd1 174.1(3) . . . . ? N1 C3 N2 C1 0.3(5) . . . . ? N1 C3 N2 C4 -180.0(4) . . . . ? C2 C1 N2 C3 -0.5(5) . . . . ? C2 C1 N2 C4 179.7(4) . . . . ? C5 C4 N2 C3 -149.6(4) . . . . ? C9 C4 N2 C3 29.4(6) . . . . ? C5 C4 N2 C1 30.1(6) . . . . ? C9 C4 N2 C1 -150.9(4) . . . . ? N4 C21 N3 C19 0.6(5) . . . . ? N4 C21 N3 C16 -178.5(4) . . . . ? C20 C19 N3 C21 -0.3(5) . . . . ? C20 C19 N3 C16 178.8(4) . . . . ? C15 C16 N3 C21 -92.7(5) . . . . ? C17 C16 N3 C21 87.7(5) . . . . ? C15 C16 N3 C19 88.4(5) . . . . ? C17 C16 N3 C19 -91.2(5) . . . . ? N3 C21 N4 C20 -0.6(5) . . . . ? N3 C21 N4 Cd2 179.1(3) . . . . ? C19 C20 N4 C21 0.4(5) . . . . ? C19 C20 N4 Cd2 -179.3(3) . . . . ? N6 C60 N5 C58 0.4(5) . . . . ? N6 C60 N5 Cd2 -174.3(3) . . . . ? C59 C58 N5 C60 0.6(5) . . . . ? C59 C58 N5 Cd2 174.5(3) . . . . ? N5 C60 N6 C59 -1.2(5) . . . . ? N5 C60 N6 C61 175.1(4) . . . . ? C58 C59 N6 C60 1.5(5) . . . . ? C58 C59 N6 C61 -174.6(4) . . . . ? C62 C61 N6 C60 129.8(5) . . . . ? C66 C61 N6 C60 -48.3(6) . . . . ? C62 C61 N6 C59 -54.7(6) . . . . ? C66 C61 N6 C59 127.2(5) . . . . ? N8 C76 N7 C77 -0.1(5) . . . . ? N8 C76 N7 C74 -177.5(4) . . . 1_354 ? C78 C77 N7 C76 -0.4(5) . . . . ? C78 C77 N7 C74 176.9(4) . . . 1_354 ? N7 C76 N8 C78 0.6(5) . . . . ? N7 C76 N8 Cd3 175.4(3) . . . . ? C77 C78 N8 C76 -0.8(5) . . . . ? C77 C78 N8 Cd3 -175.0(3) . . . . ? N10 C79 N9 C80 0.5(5) . . . . ? N10 C79 N9 Cd3 178.6(3) . . . . ? C81 C80 N9 C79 -0.7(6) . . . . ? C81 C80 N9 Cd3 -178.2(4) . . . . ? N9 C79 N10 C81 -0.1(6) . . . . ? N9 C79 N10 C55 176.0(4) . . . 1_666 ? C80 C81 N10 C79 -0.4(6) . . . . ? C80 C81 N10 C55 -176.5(4) . . . 1_666 ? N12 C42 N11 C41 0.1(5) . . . . ? N12 C42 N11 C43 -177.6(4) . . . . ? C40 C41 N11 C42 0.0(6) . . . . ? C40 C41 N11 C43 177.7(4) . . . . ? C44 C43 N11 C42 -145.2(4) . . . . ? C48 C43 N11 C42 36.0(6) . . . . ? C44 C43 N11 C41 37.5(6) . . . . ? C48 C43 N11 C41 -141.2(5) . . . . ? N11 C42 N12 C40 -0.1(5) . . . . ? N11 C42 N12 Cd1 -174.3(3) . . . . ? C41 C40 N12 C42 0.0(6) . . . . ? C41 C40 N12 Cd1 174.0(3) . . . . ? O1 C30 O2 Cd2 23.8(5) . . . . ? C28 C30 O2 Cd2 -155.2(2) . . . . ? O4 C26 O3 Cd3 -3.1(5) . . . 1_645 ? C25 C26 O3 Cd3 176.0(3) . . . 1_645 ? O3 C26 O4 Cd3 3.0(4) . . . 1_645 ? C25 C26 O4 Cd3 -176.0(4) . . . 1_645 ? O6 C22 O5 Cd1 -129.0(4) . . . 1_655 ? C23 C22 O5 Cd1 51.0(6) . . . 1_655 ? O5 C22 O6 Cd1 72.3(5) . . . 2_456 ? C23 C22 O6 Cd1 -107.7(3) . . . 2_456 ? O8 C39 O7 Cd2 -6.7(4) . . . 2_567 ? C36 C39 O7 Cd2 171.2(3) . . . 2_567 ? O7 C39 O8 Cd2 7.1(4) . . . 2_567 ? C36 C39 O8 Cd2 -170.8(3) . . . 2_567 ? O10 C38 O9 Cd3 5.1(5) . . . . ? C34 C38 O9 Cd3 -173.2(3) . . . . ? O9 C38 O10 Cd3 -4.3(4) . . . . ? C34 C38 O10 Cd3 173.9(4) . . . . ? O12 C31 O11 Cd1 6.7(5) . . . . ? C32 C31 O11 Cd1 178.1(4) . . . . ? O11 C31 O12 Cd1 -7.5(5) . . . . ? C32 C31 O12 Cd1 -179.2(3) . . . . ? C42 N12 Cd1 O5 -21.9(3) . . . 1_455 ? C40 N12 Cd1 O5 165.3(4) . . . 1_455 ? C42 N12 Cd1 N1 126.9(3) . . . . ? C40 N12 Cd1 N1 -46.0(5) . . . . ? C42 N12 Cd1 O12 -110.9(3) . . . . ? C40 N12 Cd1 O12 76.2(4) . . . . ? C42 N12 Cd1 O6 73.0(3) . . . 2_456 ? C40 N12 Cd1 O6 -99.9(4) . . . 2_456 ? C42 N12 Cd1 O11 -154.2(4) . . . . ? C40 N12 Cd1 O11 32.9(4) . . . . ? C3 N1 Cd1 O5 -72.1(4) . . . 1_455 ? C2 N1 Cd1 O5 114.4(4) . . . 1_455 ? C3 N1 Cd1 N12 144.6(3) . . . . ? C2 N1 Cd1 N12 -28.9(5) . . . . ? C3 N1 Cd1 O12 18.1(4) . . . . ? C2 N1 Cd1 O12 -155.3(4) . . . . ? C3 N1 Cd1 O6 -160.4(4) . . . 2_456 ? C2 N1 Cd1 O6 26.2(4) . . . 2_456 ? C3 N1 Cd1 O11 69.8(4) . . . . ? C2 N1 Cd1 O11 -103.6(4) . . . . ? C31 O12 Cd1 O5 -140.1(3) . . . 1_455 ? C31 O12 Cd1 N12 -54.9(4) . . . . ? C31 O12 Cd1 N1 99.8(3) . . . . ? C31 O12 Cd1 O6 106.8(6) . . . 2_456 ? C31 O12 Cd1 O11 4.0(3) . . . . ? C31 O11 Cd1 O5 46.1(4) . . . 1_455 ? C31 O11 Cd1 N12 120.1(3) . . . . ? C31 O11 Cd1 N1 -89.7(3) . . . . ? C31 O11 Cd1 O12 -3.9(3) . . . . ? C31 O11 Cd1 O6 -168.2(3) . . . 2_456 ? C30 O2 Cd2 N4 48.8(3) . . . . ? C30 O2 Cd2 O8 -122.5(3) . . . 2_567 ? C30 O2 Cd2 N5 153.4(3) . . . . ? C30 O2 Cd2 OW3 -36.9(3) . . . . ? C30 O2 Cd2 O7 -153.3(4) . . . 2_567 ? C30 O2 Cd2 C39 -131.2(3) . . . 2_567 ? C21 N4 Cd2 O2 17.4(3) . . . . ? C20 N4 Cd2 O2 -163.0(4) . . . . ? C21 N4 Cd2 O8 179.6(3) . . . 2_567 ? C20 N4 Cd2 O8 -0.7(5) . . . 2_567 ? C21 N4 Cd2 N5 -69.1(3) . . . . ? C20 N4 Cd2 N5 110.5(4) . . . . ? C21 N4 Cd2 OW3 107.1(3) . . . . ? C20 N4 Cd2 OW3 -73.2(4) . . . . ? C21 N4 Cd2 O7 -157.5(3) . . . 2_567 ? C20 N4 Cd2 O7 22.2(4) . . . 2_567 ? C21 N4 Cd2 C39 -162.6(3) . . . 2_567 ? C20 N4 Cd2 C39 17.1(4) . . . 2_567 ? C60 N5 Cd2 O2 171.0(4) . . . . ? C58 N5 Cd2 O2 -2.0(4) . . . . ? C60 N5 Cd2 N4 -97.3(3) . . . . ? C58 N5 Cd2 N4 89.6(4) . . . . ? C60 N5 Cd2 O8 57.6(3) . . . 2_567 ? C58 N5 Cd2 O8 -115.5(4) . . . 2_567 ? C60 N5 Cd2 OW3 102.3(6) . . . . ? C58 N5 Cd2 OW3 -70.7(7) . . . . ? C60 N5 Cd2 O7 1.9(3) . . . 2_567 ? C58 N5 Cd2 O7 -171.1(4) . . . 2_567 ? C60 N5 Cd2 C39 30.1(3) . . . 2_567 ? C58 N5 Cd2 C39 -143.0(4) . . . 2_567 ? C76 N8 Cd3 O9 -114.4(3) . . . . ? C78 N8 Cd3 O9 58.9(4) . . . . ? C76 N8 Cd3 N9 153.1(3) . . . . ? C78 N8 Cd3 N9 -33.5(4) . . . . ? C76 N8 Cd3 O3 27.3(5) . . . 1_465 ? C78 N8 Cd3 O3 -159.3(3) . . . 1_465 ? C76 N8 Cd3 O4 38.1(3) . . . 1_465 ? C78 N8 Cd3 O4 -148.5(4) . . . 1_465 ? C76 N8 Cd3 O10 -64.1(3) . . . . ? C78 N8 Cd3 O10 109.3(4) . . . . ? C76 N8 Cd3 C26 35.5(4) . . . 1_465 ? C78 N8 Cd3 C26 -151.1(4) . . . 1_465 ? C76 N8 Cd3 C38 -89.2(3) . . . . ? C78 N8 Cd3 C38 84.2(4) . . . . ? C38 O9 Cd3 N8 70.5(3) . . . . ? C38 O9 Cd3 N9 -179.0(3) . . . . ? C38 O9 Cd3 O3 -91.6(3) . . . 1_465 ? C38 O9 Cd3 O4 -54.7(4) . . . 1_465 ? C38 O9 Cd3 O10 -2.5(3) . . . . ? C38 O9 Cd3 C26 -79.2(3) . . . 1_465 ? C79 N9 Cd3 N8 137.2(3) . . . . ? C80 N9 Cd3 N8 -45.6(5) . . . . ? C79 N9 Cd3 O9 31.0(3) . . . . ? C80 N9 Cd3 O9 -151.7(5) . . . . ? C79 N9 Cd3 O3 -66.5(3) . . . 1_465 ? C80 N9 Cd3 O3 110.7(5) . . . 1_465 ? C79 N9 Cd3 O4 -119.0(3) . . . 1_465 ? C80 N9 Cd3 O4 58.2(5) . . . 1_465 ? C79 N9 Cd3 O10 26.6(4) . . . . ? C80 N9 Cd3 O10 -156.2(4) . . . . ? C79 N9 Cd3 C26 -92.2(3) . . . 1_465 ? C80 N9 Cd3 C26 85.1(5) . . . 1_465 ? C79 N9 Cd3 C38 30.5(4) . . . . ? C80 N9 Cd3 C38 -152.2(5) . . . . ? C38 O10 Cd3 N8 -110.6(3) . . . . ? C38 O10 Cd3 O9 2.5(3) . . . . ? C38 O10 Cd3 N9 8.0(4) . . . . ? C38 O10 Cd3 O3 99.0(3) . . . 1_465 ? C38 O10 Cd3 O4 155.5(3) . . . 1_465 ? C38 O10 Cd3 C26 126.9(3) . . . 1_465 ? O10 C38 Cd3 N8 70.0(3) . . . . ? O9 C38 Cd3 N8 -114.6(3) . . . . ? C34 C38 Cd3 N8 -84.4(14) . . . . ? O10 C38 Cd3 O9 -175.5(5) . . . . ? C34 C38 Cd3 O9 30.2(13) . . . . ? O10 C38 Cd3 N9 -174.4(2) . . . . ? O9 C38 Cd3 N9 1.1(3) . . . . ? C34 C38 Cd3 N9 31.3(15) . . . . ? O10 C38 Cd3 O3 -83.5(3) . . . 1_465 ? O9 C38 Cd3 O3 91.9(3) . . . 1_465 ? C34 C38 Cd3 O3 122.1(14) . . . 1_465 ? O10 C38 Cd3 O4 -30.2(3) . . . 1_465 ? O9 C38 Cd3 O4 145.3(3) . . . 1_465 ? C34 C38 Cd3 O4 175.5(14) . . . 1_465 ? O9 C38 Cd3 O10 175.5(5) . . . . ? C34 C38 Cd3 O10 -154.3(16) . . . . ? O10 C38 Cd3 C26 -60.3(3) . . . 1_465 ? O9 C38 Cd3 C26 115.2(3) . . . 1_465 ? C34 C38 Cd3 C26 145.4(14) . . . 1_465 ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 26.07 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.890 _refine_diff_density_min -1.089 _refine_diff_density_rms 0.096 _database_code_depnum_ccdc_archive 'CCDC 972075'