# 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 #TrackingRef 'all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H35 N5 O7 Zn' _chemical_formula_weight 630.99 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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 19.6517(17) _cell_length_b 5.9639(5) _cell_length_c 26.919(3) _cell_angle_alpha 90.00 _cell_angle_beta 105.210(7) _cell_angle_gamma 90.00 _cell_volume 3044.4(5) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 46 _cell_measurement_theta_min 3.71 _cell_measurement_theta_max 12.53 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.5 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.377 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1320 _exptl_absorpt_coefficient_mu 0.859 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9184 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details '(XSCANS; Siemens, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7000 _diffrn_reflns_av_R_equivalents 0.0787 _diffrn_reflns_av_sigmaI/netI 0.0469 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5321 _reflns_number_gt 4534 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XSCANS (Siemens, 1995)' _computing_cell_refinement 'XSCANS (Siemens, 1995)' _computing_data_reduction 'SHELXTL (Sheldrick, 2008)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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^)+(0.0393P)^2^+1.6958P] 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 5321 _refine_ls_number_parameters 396 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0480 _refine_ls_R_factor_gt 0.0337 _refine_ls_wR_factor_ref 0.0873 _refine_ls_wR_factor_gt 0.0815 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _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 Zn Zn 0.218650(11) 0.52700(3) 0.092040(8) 0.02704(7) Uani 1 1 d . . . O1 O 0.22996(7) 0.8847(2) 0.10167(5) 0.0352(4) Uani 1 1 d . . . O2 O 0.18144(8) 1.2067(2) 0.06750(6) 0.0390(4) Uani 1 1 d . . . O3 O -0.04942(8) 0.8240(3) -0.12746(6) 0.0443(4) Uani 1 1 d . . . O4 O -0.02104(9) 1.1584(3) -0.09139(7) 0.0503(5) Uani 1 1 d . . . O5 O 0.43846(9) 0.9365(3) 0.20032(6) 0.0524(5) Uani 1 1 d . . . O6 O 0.9541(4) 2.5718(14) 0.4424(3) 0.097(2) Uani 0.50 1 d P . . O6' O 0.9415(4) 2.6433(14) 0.4304(3) 0.092(2) Uani 0.50 1 d P . . O7 O 0.12790(8) 0.5495(3) 0.12139(6) 0.0377(4) Uani 1 1 d . . . N1 N 0.15991(9) 0.6592(3) 0.01906(6) 0.0298(4) Uani 1 1 d . . . N2 N 0.27817(8) 0.4612(3) 0.16765(6) 0.0275(4) Uani 1 1 d . . . N3 N 0.41713(9) 0.7412(3) 0.26689(7) 0.0364(4) Uani 1 1 d . . . H3A H 0.4287 0.7330 0.2999 0.044 Uiso 1 1 calc R . . N4 N 1.03082(11) 2.6161(4) 0.39328(9) 0.0638(7) Uani 1 1 d . . . H4A H 1.0438 2.5530 0.3685 0.077 Uiso 1 1 calc R . . N5 N 1.18530(10) 2.9789(3) 0.43174(7) 0.0388(4) Uani 1 1 d . . . C1 C 0.18784(10) 0.9984(3) 0.06813(7) 0.0280(4) Uani 1 1 d . . . C2 C 0.14161(10) 0.8737(3) 0.02268(7) 0.0259(4) Uani 1 1 d . . . C3 C 0.08611(10) 0.9727(3) -0.01283(7) 0.0282(4) Uani 1 1 d . . . H3B H 0.0738 1.1207 -0.0086 0.034 Uiso 1 1 calc R . . C4 C 0.04888(10) 0.8496(3) -0.05479(7) 0.0287(4) Uani 1 1 d . . . C5 C 0.06991(12) 0.6306(3) -0.05962(8) 0.0354(5) Uani 1 1 d . . . H5B H 0.0468 0.5440 -0.0877 0.042 Uiso 1 1 calc R . . C6 C 0.12538(12) 0.5425(3) -0.02229(8) 0.0364(5) Uani 1 1 d . . . H6A H 0.1394 0.3959 -0.0260 0.044 Uiso 1 1 calc R . . C7 C -0.01282(11) 0.9539(4) -0.09453(8) 0.0316(5) Uani 1 1 d . . . C8 C 0.26773(11) 0.2792(3) 0.19378(8) 0.0314(5) Uani 1 1 d . . . H8A H 0.2345 0.1737 0.1774 0.038 Uiso 1 1 calc R . . C9 C 0.30466(11) 0.2439(3) 0.24413(8) 0.0350(5) Uani 1 1 d . . . H9A H 0.2964 0.1163 0.2615 0.042 Uiso 1 1 calc R . . C10 C 0.35385(11) 0.3987(4) 0.26839(8) 0.0340(5) Uani 1 1 d . . . H10A H 0.3785 0.3787 0.3026 0.041 Uiso 1 1 calc R . . C11 C 0.36648(10) 0.5867(3) 0.24115(8) 0.0294(4) Uani 1 1 d . . . C12 C 0.32691(10) 0.6123(3) 0.19066(8) 0.0303(5) Uani 1 1 d . . . H12A H 0.3343 0.7377 0.1722 0.036 Uiso 1 1 calc R . . C13 C 0.45027(11) 0.9022(4) 0.24638(8) 0.0367(5) Uani 1 1 d . . . C14 C 0.50281(12) 1.0337(4) 0.28693(9) 0.0458(6) Uani 1 1 d . . . H14A H 0.4777 1.1075 0.3089 0.055 Uiso 1 1 calc R . . H14B H 0.5357 0.9290 0.3082 0.055 Uiso 1 1 calc R . . C15 C 0.54420(14) 1.2074(5) 0.26695(11) 0.0576(7) Uani 1 1 d . . . H15A H 0.5119 1.3085 0.2440 0.069 Uiso 1 1 calc R . . H15B H 0.5729 1.1345 0.2474 0.069 Uiso 1 1 calc R . . C16 C 0.59166(15) 1.3416(5) 0.31089(12) 0.0639(8) Uani 1 1 d . . . H16A H 0.5623 1.4267 0.3280 0.077 Uiso 1 1 calc R . . H16B H 0.6196 1.2380 0.3359 0.077 Uiso 1 1 calc R . . C17 C 0.64067(17) 1.5010(5) 0.29367(13) 0.0730(9) Uani 1 1 d . . . H17A H 0.6128 1.6020 0.2680 0.088 Uiso 1 1 calc R . . H17B H 0.6710 1.4155 0.2775 0.088 Uiso 1 1 calc R . . C18 C 0.68668(16) 1.6396(6) 0.33765(13) 0.0727(9) Uani 1 1 d . . . H18A H 0.6566 1.7321 0.3526 0.087 Uiso 1 1 calc R . . H18B H 0.7126 1.5390 0.3642 0.087 Uiso 1 1 calc R . . C19 C 0.73835(18) 1.7887(6) 0.32015(14) 0.0826(10) Uani 1 1 d . . . H19A H 0.7698 1.6948 0.3068 0.099 Uiso 1 1 calc R . . H19B H 0.7123 1.8826 0.2922 0.099 Uiso 1 1 calc R . . C20 C 0.78219(17) 1.9376(6) 0.36204(14) 0.0790(10) Uani 1 1 d . . . H20A H 0.7511 2.0378 0.3741 0.095 Uiso 1 1 calc R . . H20B H 0.8065 1.8448 0.3908 0.095 Uiso 1 1 calc R . . C21 C 0.83587(17) 2.0753(6) 0.34418(13) 0.0798(10) Uani 1 1 d . . . H21A H 0.8689 1.9743 0.3345 0.096 Uiso 1 1 calc R . . H21B H 0.8117 2.1584 0.3137 0.096 Uiso 1 1 calc R . . C22 C 0.87688(16) 2.2384(6) 0.38375(13) 0.0744(9) Uani 1 1 d . . . H22A H 0.8989 2.1576 0.4151 0.089 Uiso 1 1 calc R . . H22B H 0.8446 2.3469 0.3918 0.089 Uiso 1 1 calc R . . C23 C 0.93328(17) 2.3613(6) 0.36538(12) 0.0790(10) Uani 1 1 d . . . H23A H 0.9680 2.2539 0.3605 0.095 Uiso 1 1 calc R . . H23B H 0.9119 2.4299 0.3323 0.095 Uiso 1 1 calc R . . C24 C 0.96996(16) 2.5401(6) 0.40241(13) 0.0703(9) Uani 1 1 d . . . C25 C 1.07481(14) 2.7872(5) 0.42004(10) 0.0526(7) Uani 1 1 d . . . C26 C 1.05650(17) 2.9346(6) 0.45439(14) 0.0833(10) Uani 1 1 d . . . H26A H 1.0136 2.9198 0.4626 0.100 Uiso 1 1 calc R . . C27 C 1.10293(17) 3.1035(6) 0.47619(14) 0.0853(11) Uani 1 1 d . . . H27A H 1.0915 3.2050 0.4990 0.102 Uiso 1 1 calc R . . C28 C 1.16618(14) 3.1194(5) 0.46373(11) 0.0599(7) Uani 1 1 d . . . H28A H 1.1970 3.2340 0.4784 0.072 Uiso 1 1 calc R . . C29 C 1.14005(12) 2.8152(4) 0.41084(9) 0.0424(6) Uani 1 1 d . . . H29A H 1.1535 2.7144 0.3888 0.051 Uiso 1 1 calc R . . H7A H 0.0990(14) 0.648(5) 0.1130(10) 0.048(8) Uiso 1 1 d . . . H7B H 0.1055(16) 0.441(5) 0.1179(12) 0.068(10) 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 Zn 0.02871(12) 0.01811(11) 0.02650(12) -0.00038(9) -0.00660(9) 0.00280(9) O1 0.0393(8) 0.0209(7) 0.0327(8) -0.0009(6) -0.0133(6) 0.0033(6) O2 0.0497(9) 0.0168(7) 0.0394(8) -0.0030(6) -0.0083(7) 0.0008(6) O3 0.0457(9) 0.0403(9) 0.0321(8) 0.0039(7) -0.0158(7) -0.0078(7) O4 0.0449(9) 0.0303(9) 0.0589(10) 0.0018(8) -0.0161(8) 0.0101(7) O5 0.0544(10) 0.0602(11) 0.0390(9) 0.0044(8) 0.0060(8) -0.0244(9) O6 0.115(4) 0.114(5) 0.087(3) -0.051(3) 0.068(3) -0.068(4) O6' 0.076(3) 0.097(5) 0.127(6) -0.061(4) 0.067(3) -0.052(3) O7 0.0293(7) 0.0266(8) 0.0522(9) 0.0011(7) 0.0016(7) 0.0047(7) N1 0.0334(9) 0.0179(8) 0.0303(9) -0.0019(7) -0.0053(7) 0.0027(7) N2 0.0272(8) 0.0240(8) 0.0261(8) -0.0004(7) -0.0023(6) 0.0014(7) N3 0.0380(9) 0.0383(10) 0.0248(8) 0.0038(7) -0.0061(7) -0.0115(8) N4 0.0561(12) 0.0713(15) 0.0730(15) -0.0362(12) 0.0329(11) -0.0342(12) N5 0.0383(9) 0.0396(10) 0.0372(10) -0.0060(8) 0.0078(8) -0.0102(8) C1 0.0299(9) 0.0202(10) 0.0288(10) -0.0030(8) -0.0013(8) 0.0003(8) C2 0.0295(9) 0.0192(9) 0.0245(9) -0.0014(7) -0.0011(8) -0.0005(8) C3 0.0310(10) 0.0179(9) 0.0302(10) 0.0004(8) -0.0015(8) 0.0024(8) C4 0.0289(10) 0.0274(10) 0.0246(9) 0.0015(8) -0.0019(8) 0.0002(8) C5 0.0438(12) 0.0243(10) 0.0285(10) -0.0049(8) -0.0075(9) -0.0009(9) C6 0.0451(12) 0.0178(9) 0.0373(11) -0.0036(8) -0.0051(9) 0.0050(9) C7 0.0302(10) 0.0327(11) 0.0263(10) 0.0046(9) -0.0022(8) -0.0017(9) C8 0.0320(10) 0.0247(10) 0.0330(10) -0.0015(8) 0.0006(9) -0.0032(8) C9 0.0391(11) 0.0259(10) 0.0359(11) 0.0077(9) 0.0027(9) -0.0018(9) C10 0.0335(10) 0.0339(11) 0.0280(10) 0.0057(9) -0.0038(8) 0.0016(9) C11 0.0270(9) 0.0284(10) 0.0282(10) -0.0002(8) -0.0010(8) -0.0013(8) C12 0.0299(10) 0.0263(10) 0.0294(10) 0.0031(8) -0.0016(8) -0.0033(8) C13 0.0290(10) 0.0389(12) 0.0371(12) 0.0002(10) -0.0004(9) -0.0045(9) C14 0.0380(12) 0.0459(14) 0.0468(13) -0.0045(11) -0.0005(10) -0.0130(11) C15 0.0533(14) 0.0585(16) 0.0607(16) -0.0107(13) 0.0142(13) -0.0249(13) C16 0.0589(16) 0.0632(18) 0.0692(18) -0.0155(15) 0.0160(14) -0.0310(14) C17 0.0677(18) 0.071(2) 0.083(2) -0.0172(17) 0.0235(16) -0.0366(16) C18 0.0606(17) 0.073(2) 0.083(2) -0.0161(17) 0.0162(16) -0.0319(16) C19 0.0736(19) 0.080(2) 0.094(2) -0.0220(19) 0.0222(18) -0.0440(18) C20 0.0662(18) 0.086(2) 0.084(2) -0.0202(19) 0.0190(16) -0.0437(18) C21 0.0734(19) 0.085(2) 0.083(2) -0.0230(18) 0.0234(17) -0.0452(18) C22 0.0665(17) 0.079(2) 0.082(2) -0.0224(17) 0.0266(16) -0.0393(17) C23 0.0765(19) 0.095(2) 0.074(2) -0.0350(18) 0.0341(16) -0.0514(18) C24 0.0637(16) 0.082(2) 0.0741(19) -0.0309(17) 0.0340(15) -0.0372(16) C25 0.0517(14) 0.0557(15) 0.0545(15) -0.0179(12) 0.0212(12) -0.0218(12) C26 0.0683(17) 0.100(2) 0.098(2) -0.055(2) 0.0507(16) -0.0387(18) C27 0.0805(19) 0.094(2) 0.098(2) -0.0596(19) 0.0535(18) -0.0408(19) C28 0.0579(15) 0.0642(17) 0.0594(16) -0.0295(14) 0.0189(13) -0.0250(14) C29 0.0427(12) 0.0419(13) 0.0437(12) -0.0112(10) 0.0134(10) -0.0102(11) _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 Zn O2 2.0899(14) 1_545 ? Zn N2 2.1013(15) . ? Zn O7 2.1359(17) . ? Zn N1 2.1503(16) . ? Zn O1 2.1537(14) . ? Zn N5 2.1654(19) 2_625 ? O1 C1 1.252(2) . ? O2 C1 1.248(2) . ? O2 Zn 2.0899(14) 1_565 ? O3 C7 1.252(2) . ? O4 C7 1.236(3) . ? O5 C13 1.217(3) . ? O6 O6' 0.553(13) . ? O6 C24 1.211(9) . ? O6' C24 1.216(9) . ? O7 H7A 0.81(3) . ? O7 H7B 0.77(3) . ? N1 C6 1.337(3) . ? N1 C2 1.339(3) . ? N2 C8 1.338(3) . ? N2 C12 1.342(2) . ? N3 C13 1.356(3) . ? N3 C11 1.399(3) . ? N3 H3A 0.8600 . ? N4 C24 1.360(4) . ? N4 C25 1.407(3) . ? N4 H4A 0.8600 . ? N5 C28 1.325(3) . ? N5 C29 1.341(3) . ? N5 Zn 2.1654(19) 2_675 ? C1 C2 1.514(2) . ? C2 C3 1.380(3) . ? C3 C4 1.384(3) . ? C3 H3B 0.9300 . ? C4 C5 1.386(3) . ? C4 C7 1.523(3) . ? C5 C6 1.378(3) . ? C5 H5B 0.9300 . ? C6 H6A 0.9300 . ? C8 C9 1.376(3) . ? C8 H8A 0.9300 . ? C9 C10 1.372(3) . ? C9 H9A 0.9300 . ? C10 C11 1.397(3) . ? C10 H10A 0.9300 . ? C11 C12 1.386(3) . ? C12 H12A 0.9300 . ? C13 C14 1.510(3) . ? C14 C15 1.501(4) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.527(4) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.510(4) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.530(4) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.515(4) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.514(4) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.512(4) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.510(4) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.516(4) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.508(4) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C25 C29 1.378(3) . ? C25 C26 1.390(4) . ? C26 C27 1.383(4) . ? C26 H26A 0.9300 . ? C27 C28 1.373(4) . ? C27 H27A 0.9300 . ? C28 H28A 0.9300 . ? C29 H29A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Zn N2 101.25(6) 1_545 . ? O2 Zn O7 85.27(6) 1_545 . ? N2 Zn O7 87.71(6) . . ? O2 Zn N1 89.26(6) 1_545 . ? N2 Zn N1 169.23(6) . . ? O7 Zn N1 90.84(7) . . ? O2 Zn O1 163.77(5) 1_545 . ? N2 Zn O1 93.14(6) . . ? O7 Zn O1 87.88(6) . . ? N1 Zn O1 76.14(5) . . ? O2 Zn N5 92.60(7) 1_545 2_625 ? N2 Zn N5 87.40(7) . 2_625 ? O7 Zn N5 174.19(7) . 2_625 ? N1 Zn N5 94.54(7) . 2_625 ? O1 Zn N5 95.53(7) . 2_625 ? C1 O1 Zn 114.95(12) . . ? C1 O2 Zn 151.62(14) . 1_565 ? O6' O6 C24 77.4(17) . . ? O6 O6' C24 76.3(17) . . ? Zn O7 H7A 122.5(19) . . ? Zn O7 H7B 114(2) . . ? H7A O7 H7B 104(3) . . ? C6 N1 C2 118.07(16) . . ? C6 N1 Zn 127.10(13) . . ? C2 N1 Zn 111.95(12) . . ? C8 N2 C12 119.42(17) . . ? C8 N2 Zn 122.52(13) . . ? C12 N2 Zn 118.03(13) . . ? C13 N3 C11 128.30(18) . . ? C13 N3 H3A 115.9 . . ? C11 N3 H3A 115.9 . . ? C24 N4 C25 126.9(2) . . ? C24 N4 H4A 116.6 . . ? C25 N4 H4A 116.6 . . ? C28 N5 C29 117.6(2) . . ? C28 N5 Zn 121.76(16) . 2_675 ? C29 N5 Zn 120.40(16) . 2_675 ? O2 C1 O1 126.44(18) . . ? O2 C1 C2 116.17(17) . . ? O1 C1 C2 117.36(16) . . ? N1 C2 C3 122.46(17) . . ? N1 C2 C1 114.36(16) . . ? C3 C2 C1 123.17(17) . . ? C2 C3 C4 119.39(17) . . ? C2 C3 H3B 120.3 . . ? C4 C3 H3B 120.3 . . ? C3 C4 C5 118.00(17) . . ? C3 C4 C7 120.63(18) . . ? C5 C4 C7 121.37(18) . . ? C6 C5 C4 119.27(18) . . ? C6 C5 H5B 120.4 . . ? C4 C5 H5B 120.4 . . ? N1 C6 C5 122.70(19) . . ? N1 C6 H6A 118.7 . . ? C5 C6 H6A 118.7 . . ? O4 C7 O3 126.69(19) . . ? O4 C7 C4 116.67(18) . . ? O3 C7 C4 116.63(18) . . ? N2 C8 C9 121.90(18) . . ? N2 C8 H8A 119.1 . . ? C9 C8 H8A 119.1 . . ? C10 C9 C8 119.31(19) . . ? C10 C9 H9A 120.3 . . ? C8 C9 H9A 120.3 . . ? C9 C10 C11 119.36(18) . . ? C9 C10 H10A 120.3 . . ? C11 C10 H10A 120.3 . . ? C12 C11 C10 118.17(18) . . ? C12 C11 N3 123.79(19) . . ? C10 C11 N3 118.02(17) . . ? N2 C12 C11 121.82(19) . . ? N2 C12 H12A 119.1 . . ? C11 C12 H12A 119.1 . . ? O5 C13 N3 123.4(2) . . ? O5 C13 C14 124.1(2) . . ? N3 C13 C14 112.56(19) . . ? C15 C14 C13 115.6(2) . . ? C15 C14 H14A 108.4 . . ? C13 C14 H14A 108.4 . . ? C15 C14 H14B 108.4 . . ? C13 C14 H14B 108.4 . . ? H14A C14 H14B 107.5 . . ? C14 C15 C16 111.3(2) . . ? 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 . . ? C17 C16 C15 113.7(3) . . ? C17 C16 H16A 108.8 . . ? C15 C16 H16A 108.8 . . ? C17 C16 H16B 108.8 . . ? C15 C16 H16B 108.8 . . ? H16A C16 H16B 107.7 . . ? C16 C17 C18 113.4(3) . . ? C16 C17 H17A 108.9 . . ? C18 C17 H17A 108.9 . . ? C16 C17 H17B 108.9 . . ? C18 C17 H17B 108.9 . . ? H17A C17 H17B 107.7 . . ? C19 C18 C17 112.6(3) . . ? C19 C18 H18A 109.1 . . ? C17 C18 H18A 109.1 . . ? C19 C18 H18B 109.1 . . ? C17 C18 H18B 109.1 . . ? H18A C18 H18B 107.8 . . ? C20 C19 C18 114.2(3) . . ? C20 C19 H19A 108.7 . . ? C18 C19 H19A 108.7 . . ? C20 C19 H19B 108.7 . . ? C18 C19 H19B 108.7 . . ? H19A C19 H19B 107.6 . . ? C21 C20 C19 113.0(3) . . ? C21 C20 H20A 109.0 . . ? C19 C20 H20A 109.0 . . ? C21 C20 H20B 109.0 . . ? C19 C20 H20B 109.0 . . ? H20A C20 H20B 107.8 . . ? C22 C21 C20 114.4(3) . . ? C22 C21 H21A 108.7 . . ? C20 C21 H21A 108.7 . . ? C22 C21 H21B 108.7 . . ? C20 C21 H21B 108.7 . . ? H21A C21 H21B 107.6 . . ? C21 C22 C23 112.5(3) . . ? C21 C22 H22A 109.1 . . ? C23 C22 H22A 109.1 . . ? C21 C22 H22B 109.1 . . ? C23 C22 H22B 109.1 . . ? H22A C22 H22B 107.8 . . ? C24 C23 C22 113.0(3) . . ? C24 C23 H23A 109.0 . . ? C22 C23 H23A 109.0 . . ? C24 C23 H23B 109.0 . . ? C22 C23 H23B 109.0 . . ? H23A C23 H23B 107.8 . . ? O6 C24 O6' 26.3(6) . . ? O6 C24 N4 123.5(4) . . ? O6' C24 N4 120.8(4) . . ? O6 C24 C23 120.6(4) . . ? O6' C24 C23 123.4(4) . . ? N4 C24 C23 114.0(3) . . ? C29 C25 C26 117.3(2) . . ? C29 C25 N4 118.1(2) . . ? C26 C25 N4 124.6(2) . . ? C27 C26 C25 119.1(3) . . ? C27 C26 H26A 120.5 . . ? C25 C26 H26A 120.5 . . ? C28 C27 C26 119.0(3) . . ? C28 C27 H27A 120.5 . . ? C26 C27 H27A 120.5 . . ? N5 C28 C27 123.0(3) . . ? N5 C28 H28A 118.5 . . ? C27 C28 H28A 118.5 . . ? N5 C29 C25 123.9(2) . . ? N5 C29 H29A 118.0 . . ? C25 C29 H29A 118.0 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.432 _refine_diff_density_min -0.474 _refine_diff_density_rms 0.081 _database_code_depnum_ccdc_archive 'CCDC 917800' ####################################################################### # # 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 #TrackingRef 'all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H38 N4 O10 Zn' _chemical_formula_weight 692.02 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.482(2) _cell_length_b 11.424(3) _cell_length_c 15.607(4) _cell_angle_alpha 89.33(2) _cell_angle_beta 81.068(13) _cell_angle_gamma 78.376(16) _cell_volume 1635.5(7) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 6113 _cell_measurement_theta_min 2.6377 _cell_measurement_theta_max 29.0388 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.405 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 724 _exptl_absorpt_coefficient_mu 0.812 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.97356 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; 'Tue Mar 16 15:42:27 2010' ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'Xcalibur, Sapphire3, Gemini' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.0690 _diffrn_reflns_number 15061 _diffrn_reflns_av_R_equivalents 0.0355 _diffrn_reflns_av_sigmaI/netI 0.1021 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.64 _diffrn_reflns_theta_max 29.10 _reflns_number_total 7509 _reflns_number_gt 4757 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; 'Tue Mar 16 15:42:27 2010' ; _computing_cell_refinement ; 'Tue Mar 16 15:42:27 2010' ; _computing_data_reduction ; 'Tue Mar 16 15:42:27 2010' ; _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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^)+(0.0255P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7509 _refine_ls_number_parameters 418 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0754 _refine_ls_R_factor_gt 0.0405 _refine_ls_wR_factor_ref 0.0773 _refine_ls_wR_factor_gt 0.0740 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _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 Zn Zn -1.08797(3) 0.65330(3) 0.547410(17) 0.01562(7) Uani 1 1 d . . . O1 O -0.70831(17) 0.88148(17) 0.63267(12) 0.0389(5) Uani 1 1 d . . . O2 O 0.55512(17) 0.65245(19) 0.97310(10) 0.0405(6) Uani 1 1 d . . . O3 O -0.90865(13) 0.60156(15) 0.46728(9) 0.0187(4) Uani 1 1 d . . . O4 O -0.78381(14) 0.60970(14) 0.57589(9) 0.0168(4) Uani 1 1 d . . . O5 O -0.27334(13) 0.65392(14) 0.50884(9) 0.0162(4) Uani 1 1 d . . . O6 O -0.17637(15) 0.69132(16) 0.37428(10) 0.0258(4) Uani 1 1 d . . . O7 O -0.45367(15) 0.65516(16) 0.13776(10) 0.0246(4) Uani 1 1 d . . . O8 O -0.69535(15) 0.67065(15) 0.16599(9) 0.0224(4) Uani 1 1 d . . . N1 N -1.09959(18) 0.83467(18) 0.57136(11) 0.0193(5) Uani 1 1 d . . . N2 N -0.90804(19) 1.02626(19) 0.67928(13) 0.0287(5) Uani 1 1 d . . . H2A H -0.9393 1.0889 0.7122 0.034 Uiso 1 1 calc R . . N3 N 0.54214(17) 0.62553(18) 0.83263(11) 0.0190(5) Uani 1 1 d . . . H3A H 0.4844 0.6244 0.7954 0.023 Uiso 1 1 calc R . . N4 N 0.87313(17) 0.60915(17) 0.67446(11) 0.0151(4) Uani 1 1 d . . . C1 C -1.2090(2) 0.9187(2) 0.54929(16) 0.0260(6) Uani 1 1 d . . . H1A H -1.2773 0.8950 0.5201 0.031 Uiso 1 1 calc R . . C2 C -1.2232(3) 1.0373(2) 0.56837(17) 0.0314(7) Uani 1 1 d . . . H2B H -1.3001 1.0931 0.5525 0.038 Uiso 1 1 calc R . . C3 C -1.1218(2) 1.0738(2) 0.61156(16) 0.0304(7) Uani 1 1 d . . . H3B H -1.1297 1.1542 0.6251 0.036 Uiso 1 1 calc R . . C4 C -1.0089(2) 0.9888(2) 0.63417(15) 0.0227(6) Uani 1 1 d . . . C5 C -1.0017(2) 0.8703(2) 0.61329(15) 0.0233(6) Uani 1 1 d . . . H5A H -0.9260 0.8129 0.6289 0.028 Uiso 1 1 calc R . . C6 C -0.7645(3) 0.9721(3) 0.67569(17) 0.0314(7) Uani 1 1 d . . . C7 C -0.6815(3) 1.0384(3) 0.72705(19) 0.0429(8) Uani 1 1 d . . . H7A H -0.7447 1.0712 0.7798 0.051 Uiso 1 1 calc R . . H7B H -0.6550 1.1047 0.6933 0.051 Uiso 1 1 calc R . . C8 C -0.5440(2) 0.9596(2) 0.75084(16) 0.0299(7) Uani 1 1 d . . . H8A H -0.5689 0.8890 0.7793 0.036 Uiso 1 1 calc R . . H8B H -0.4762 0.9338 0.6982 0.036 Uiso 1 1 calc R . . C9 C -0.4706(3) 1.0235(3) 0.81006(18) 0.0392(8) Uani 1 1 d . . . H9A H -0.5430 1.0606 0.8580 0.047 Uiso 1 1 calc R . . H9B H -0.4322 1.0865 0.7781 0.047 Uiso 1 1 calc R . . C10 C -0.3476(3) 0.9418(3) 0.84618(19) 0.0451(8) Uani 1 1 d . . . H10A H -0.2682 0.9149 0.7992 0.054 Uiso 1 1 calc R . . H10B H -0.3820 0.8719 0.8698 0.054 Uiso 1 1 calc R . . C11 C -0.2895(3) 1.0021(3) 0.91755(19) 0.0498(9) Uani 1 1 d . . . H11A H -0.2413 1.0643 0.8918 0.060 Uiso 1 1 calc R . . H11B H -0.3710 1.0398 0.9603 0.060 Uiso 1 1 calc R . . C12 C -0.1835(3) 0.9153(3) 0.96262(19) 0.0513(9) Uani 1 1 d . . . H12A H -0.2223 0.8437 0.9759 0.062 Uiso 1 1 calc R . . H12B H -0.1747 0.9512 1.0171 0.062 Uiso 1 1 calc R . . C13 C -0.0311(3) 0.8800(3) 0.90806(19) 0.0485(9) Uani 1 1 d . . . H13A H -0.0405 0.8505 0.8516 0.058 Uiso 1 1 calc R . . H13B H 0.0117 0.9503 0.8992 0.058 Uiso 1 1 calc R . . C14 C 0.0709(3) 0.7837(3) 0.95120(18) 0.0420(8) Uani 1 1 d . . . H14A H 0.0668 0.8071 1.0112 0.050 Uiso 1 1 calc R . . H14B H 0.0370 0.7091 0.9508 0.050 Uiso 1 1 calc R . . C15 C 0.2276(2) 0.7638(3) 0.90615(17) 0.0374(8) Uani 1 1 d . . . H15A H 0.2692 0.8318 0.9177 0.045 Uiso 1 1 calc R . . H15B H 0.2301 0.7575 0.8440 0.045 Uiso 1 1 calc R . . C16 C 0.3183(2) 0.6509(3) 0.93712(15) 0.0286(7) Uani 1 1 d . . . H16A H 0.2914 0.6464 0.9995 0.034 Uiso 1 1 calc R . . H16B H 0.2942 0.5823 0.9109 0.034 Uiso 1 1 calc R . . C17 C 0.4813(2) 0.6425(2) 0.91641(16) 0.0254(6) Uani 1 1 d . . . C18 C 0.6930(2) 0.6093(2) 0.80034(14) 0.0169(5) Uani 1 1 d . . . C19 C 0.8016(2) 0.5693(2) 0.85021(15) 0.0233(6) Uani 1 1 d . . . H19A H 0.7785 0.5560 0.9091 0.028 Uiso 1 1 calc R . . C20 C 0.9445(2) 0.5499(2) 0.81005(15) 0.0248(6) Uani 1 1 d . . . H20A H 1.0192 0.5235 0.8421 0.030 Uiso 1 1 calc R . . C21 C 0.9771(2) 0.5693(2) 0.72291(14) 0.0207(6) Uani 1 1 d . . . H21A H 1.0742 0.5544 0.6968 0.025 Uiso 1 1 calc R . . C22 C 0.7334(2) 0.6278(2) 0.71283(14) 0.0162(5) Uani 1 1 d . . . H22A H 0.6607 0.6543 0.6793 0.019 Uiso 1 1 calc R . . C23 C -0.7918(2) 0.6088(2) 0.49806(14) 0.0139(5) Uani 1 1 d . . . C24 C -0.6646(2) 0.6234(2) 0.43195(13) 0.0121(5) Uani 1 1 d . . . C25 C -0.5340(2) 0.6351(2) 0.45809(13) 0.0130(5) Uani 1 1 d . . . H25A H -0.5253 0.6306 0.5166 0.016 Uiso 1 1 calc R . . C26 C -0.4171(2) 0.6535(2) 0.39812(13) 0.0133(5) Uani 1 1 d . . . C27 C -0.2756(2) 0.6665(2) 0.42732(15) 0.0163(5) Uani 1 1 d . . . C28 C -0.4285(2) 0.6588(2) 0.31030(14) 0.0149(5) Uani 1 1 d . . . H28A H -0.3491 0.6686 0.2697 0.018 Uiso 1 1 calc R . . C29 C -0.5596(2) 0.6494(2) 0.28336(13) 0.0132(5) Uani 1 1 d . . . C30 C -0.5778(2) 0.6602(2) 0.19042(14) 0.0176(5) Uani 1 1 d . . . C31 C -0.6762(2) 0.6314(2) 0.34433(13) 0.0134(5) Uani 1 1 d . . . H31A H -0.7631 0.6245 0.3262 0.016 Uiso 1 1 calc R . . O9 O -0.99902(16) 1.24565(16) 0.77161(10) 0.0307(5) Uani 1 1 d . . . H9E H -1.0904 1.2731 0.7786 0.037 Uiso 1 1 d R . . H9F H -0.9589 1.2798 0.7286 0.037 Uiso 1 1 d R . . O10 O 0.38964(16) 0.65642(16) 0.69267(10) 0.0305(5) Uani 1 1 d . . . H10D H 0.3463 0.6174 0.6629 0.037 Uiso 1 1 d R . . H10E H 0.3579 0.7306 0.6863 0.037 Uiso 1 1 d R . . H7C H -0.470(2) 0.671(2) 0.0873(16) 0.037 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 Zn 0.00877(11) 0.02496(18) 0.01348(13) -0.00056(12) -0.00103(9) -0.00474(11) O1 0.0298(9) 0.0258(12) 0.0628(13) -0.0129(10) -0.0239(9) 0.0036(9) O2 0.0265(9) 0.0790(17) 0.0123(9) -0.0030(10) -0.0005(7) -0.0038(10) O3 0.0084(7) 0.0338(11) 0.0149(8) -0.0020(7) -0.0015(6) -0.0070(7) O4 0.0136(7) 0.0270(10) 0.0107(8) -0.0015(7) -0.0005(6) -0.0072(7) O5 0.0098(7) 0.0251(10) 0.0145(8) 0.0002(7) -0.0041(6) -0.0043(7) O6 0.0121(7) 0.0465(12) 0.0212(9) 0.0070(8) -0.0025(7) -0.0122(8) O7 0.0204(8) 0.0445(13) 0.0088(8) 0.0011(8) 0.0015(7) -0.0088(8) O8 0.0167(7) 0.0352(12) 0.0162(8) 0.0012(8) -0.0056(7) -0.0045(8) N1 0.0161(9) 0.0235(13) 0.0191(10) -0.0016(9) -0.0032(8) -0.0059(9) N2 0.0262(10) 0.0190(13) 0.0421(13) -0.0093(10) -0.0138(10) -0.0004(10) N3 0.0144(9) 0.0320(14) 0.0114(10) -0.0004(9) -0.0025(7) -0.0063(9) N4 0.0141(9) 0.0166(12) 0.0148(10) -0.0005(9) -0.0018(8) -0.0039(9) C1 0.0219(12) 0.0273(17) 0.0307(14) 0.0026(12) -0.0103(11) -0.0046(12) C2 0.0253(13) 0.0250(18) 0.0442(16) 0.0008(14) -0.0166(12) 0.0032(13) C3 0.0281(13) 0.0198(16) 0.0431(17) -0.0030(13) -0.0105(12) -0.0003(12) C4 0.0219(12) 0.0176(15) 0.0299(14) -0.0015(12) -0.0099(11) -0.0028(11) C5 0.0173(11) 0.0246(17) 0.0278(14) 0.0011(12) -0.0072(10) -0.0013(12) C6 0.0298(13) 0.0242(18) 0.0439(17) 0.0016(14) -0.0198(12) -0.0031(13) C7 0.0427(15) 0.0291(18) 0.067(2) -0.0020(15) -0.0348(15) -0.0099(15) C8 0.0235(12) 0.0296(17) 0.0414(16) 0.0011(13) -0.0137(11) -0.0106(12) C9 0.0329(14) 0.0317(18) 0.0588(19) -0.0014(15) -0.0260(13) -0.0058(14) C10 0.0386(15) 0.035(2) 0.069(2) -0.0012(16) -0.0284(15) -0.0078(15) C11 0.0361(15) 0.044(2) 0.064(2) -0.0134(17) -0.0136(15) 0.0094(16) C12 0.0319(15) 0.067(3) 0.052(2) -0.0162(18) -0.0126(14) 0.0014(17) C13 0.0340(15) 0.057(2) 0.054(2) -0.0005(17) -0.0090(14) -0.0068(16) C14 0.0293(14) 0.049(2) 0.0455(18) 0.0005(16) -0.0076(13) -0.0006(15) C15 0.0229(13) 0.046(2) 0.0396(17) 0.0049(15) -0.0005(12) -0.0012(14) C16 0.0176(11) 0.0435(19) 0.0201(14) 0.0030(13) 0.0046(10) -0.0009(13) C17 0.0230(12) 0.0283(17) 0.0219(14) 0.0027(12) 0.0006(11) -0.0017(12) C18 0.0159(10) 0.0189(15) 0.0158(12) -0.0026(10) -0.0002(9) -0.0046(10) C19 0.0216(12) 0.0334(17) 0.0145(12) 0.0041(12) -0.0014(10) -0.0060(12) C20 0.0185(11) 0.0357(18) 0.0201(13) 0.0054(12) -0.0062(10) -0.0035(12) C21 0.0142(10) 0.0237(16) 0.0247(13) -0.0015(11) -0.0032(10) -0.0043(11) C22 0.0138(10) 0.0187(15) 0.0168(12) -0.0024(10) -0.0024(9) -0.0050(10) C23 0.0107(10) 0.0145(14) 0.0160(12) 0.0000(10) -0.0001(9) -0.0028(10) C24 0.0092(9) 0.0107(13) 0.0157(11) -0.0001(10) -0.0007(8) -0.0017(9) C25 0.0131(10) 0.0139(14) 0.0114(11) -0.0012(10) -0.0035(9) 0.0002(10) C26 0.0105(10) 0.0117(13) 0.0174(12) 0.0006(10) -0.0025(9) -0.0010(10) C27 0.0099(10) 0.0145(14) 0.0243(13) 0.0003(11) -0.0028(9) -0.0019(10) C28 0.0101(10) 0.0167(14) 0.0166(12) 0.0009(10) 0.0029(9) -0.0039(10) C29 0.0139(10) 0.0133(14) 0.0123(11) -0.0011(10) -0.0026(9) -0.0023(10) C30 0.0205(11) 0.0140(14) 0.0181(12) 0.0005(10) -0.0010(10) -0.0044(11) C31 0.0099(10) 0.0139(14) 0.0160(12) 0.0007(10) -0.0035(9) -0.0006(10) O9 0.0259(8) 0.0317(12) 0.0306(10) -0.0001(9) 0.0057(8) -0.0046(9) O10 0.0311(9) 0.0326(12) 0.0309(10) -0.0070(8) -0.0164(8) -0.0045(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 Zn O3 1.9382(14) . ? Zn O5 1.9431(13) 1_455 ? Zn N4 2.0363(18) 1_355 ? Zn N1 2.088(2) . ? O1 C6 1.220(3) . ? O2 C17 1.230(3) . ? O3 C23 1.292(2) . ? O4 C23 1.229(2) . ? O5 C27 1.282(3) . ? O5 Zn 1.9431(13) 1_655 ? O6 C27 1.229(2) . ? O7 C30 1.318(3) . ? O7 H7C 0.84(2) . ? O8 C30 1.217(2) . ? N1 C5 1.343(3) . ? N1 C1 1.348(3) . ? N2 C6 1.370(3) . ? N2 C4 1.405(3) . ? N2 H2A 0.8600 . ? N3 C17 1.344(3) . ? N3 C18 1.416(3) . ? N3 H3A 0.8600 . ? N4 C21 1.339(3) . ? N4 C22 1.343(3) . ? N4 Zn 2.0363(18) 1_755 ? C1 C2 1.367(4) . ? C1 H1A 0.9300 . ? C2 C3 1.386(3) . ? C2 H2B 0.9300 . ? C3 C4 1.380(3) . ? C3 H3B 0.9300 . ? C4 C5 1.382(3) . ? C5 H5A 0.9300 . ? C6 C7 1.512(3) . ? C7 C8 1.522(3) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.513(3) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.517(3) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.543(4) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.513(4) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.538(4) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.535(4) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.515(3) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.518(3) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.513(3) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C18 C22 1.386(3) . ? C18 C19 1.388(3) . ? C19 C20 1.377(3) . ? C19 H19A 0.9300 . ? C20 C21 1.373(3) . ? C20 H20A 0.9300 . ? C21 H21A 0.9300 . ? C22 H22A 0.9300 . ? C23 C24 1.496(3) . ? C24 C31 1.389(3) . ? C24 C25 1.393(3) . ? C25 C26 1.384(3) . ? C25 H25A 0.9300 . ? C26 C28 1.391(3) . ? C26 C27 1.517(3) . ? C28 C29 1.397(3) . ? C28 H28A 0.9300 . ? C29 C31 1.389(3) . ? C29 C30 1.488(3) . ? C31 H31A 0.9300 . ? O9 H9E 0.8500 . ? O9 H9F 0.8499 . ? O10 H10D 0.8498 . ? O10 H10E 0.8502 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Zn O5 119.28(6) . 1_455 ? O3 Zn N4 126.52(7) . 1_355 ? O5 Zn N4 102.76(6) 1_455 1_355 ? O3 Zn N1 105.32(7) . . ? O5 Zn N1 102.19(7) 1_455 . ? N4 Zn N1 95.61(8) 1_355 . ? C23 O3 Zn 114.50(13) . . ? C27 O5 Zn 116.26(13) . 1_655 ? C30 O7 H7C 109.8(16) . . ? C5 N1 C1 118.1(2) . . ? C5 N1 Zn 120.54(16) . . ? C1 N1 Zn 121.27(16) . . ? C6 N2 C4 126.0(2) . . ? C6 N2 H2A 117.0 . . ? C4 N2 H2A 117.0 . . ? C17 N3 C18 125.70(18) . . ? C17 N3 H3A 117.2 . . ? C18 N3 H3A 117.2 . . ? C21 N4 C22 118.29(18) . . ? C21 N4 Zn 124.48(14) . 1_755 ? C22 N4 Zn 117.13(14) . 1_755 ? N1 C1 C2 122.3(2) . . ? N1 C1 H1A 118.8 . . ? C2 C1 H1A 118.8 . . ? C1 C2 C3 119.4(2) . . ? C1 C2 H2B 120.3 . . ? C3 C2 H2B 120.3 . . ? C4 C3 C2 118.8(2) . . ? C4 C3 H3B 120.6 . . ? C2 C3 H3B 120.6 . . ? C3 C4 C5 118.7(2) . . ? C3 C4 N2 118.5(2) . . ? C5 C4 N2 122.8(2) . . ? N1 C5 C4 122.6(2) . . ? N1 C5 H5A 118.7 . . ? C4 C5 H5A 118.7 . . ? O1 C6 N2 123.0(2) . . ? O1 C6 C7 123.5(2) . . ? N2 C6 C7 113.4(2) . . ? C6 C7 C8 113.0(2) . . ? C6 C7 H7A 109.0 . . ? C8 C7 H7A 109.0 . . ? C6 C7 H7B 109.0 . . ? C8 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? C9 C8 C7 112.5(2) . . ? C9 C8 H8A 109.1 . . ? C7 C8 H8A 109.1 . . ? C9 C8 H8B 109.1 . . ? C7 C8 H8B 109.1 . . ? H8A C8 H8B 107.8 . . ? C8 C9 C10 113.5(2) . . ? C8 C9 H9A 108.9 . . ? C10 C9 H9A 108.9 . . ? C8 C9 H9B 108.9 . . ? C10 C9 H9B 108.9 . . ? H9A C9 H9B 107.7 . . ? C9 C10 C11 113.4(2) . . ? C9 C10 H10A 108.9 . . ? C11 C10 H10A 108.9 . . ? C9 C10 H10B 108.9 . . ? C11 C10 H10B 108.9 . . ? H10A C10 H10B 107.7 . . ? C12 C11 C10 112.9(3) . . ? C12 C11 H11A 109.0 . . ? C10 C11 H11A 109.0 . . ? C12 C11 H11B 109.0 . . ? C10 C11 H11B 109.0 . . ? H11A C11 H11B 107.8 . . ? C11 C12 C13 113.1(3) . . ? C11 C12 H12A 109.0 . . ? C13 C12 H12A 109.0 . . ? C11 C12 H12B 109.0 . . ? C13 C12 H12B 109.0 . . ? H12A C12 H12B 107.8 . . ? C14 C13 C12 112.4(2) . . ? C14 C13 H13A 109.1 . . ? C12 C13 H13A 109.1 . . ? C14 C13 H13B 109.1 . . ? C12 C13 H13B 109.1 . . ? H13A C13 H13B 107.9 . . ? C15 C14 C13 112.7(2) . . ? C15 C14 H14A 109.0 . . ? C13 C14 H14A 109.0 . . ? C15 C14 H14B 109.0 . . ? C13 C14 H14B 109.0 . . ? H14A C14 H14B 107.8 . . ? C14 C15 C16 111.2(2) . . ? 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 . . ? C17 C16 C15 114.6(2) . . ? C17 C16 H16A 108.6 . . ? C15 C16 H16A 108.6 . . ? C17 C16 H16B 108.6 . . ? C15 C16 H16B 108.6 . . ? H16A C16 H16B 107.6 . . ? O2 C17 N3 121.2(2) . . ? O2 C17 C16 121.9(2) . . ? N3 C17 C16 116.9(2) . . ? C22 C18 C19 118.57(19) . . ? C22 C18 N3 117.69(18) . . ? C19 C18 N3 123.6(2) . . ? C20 C19 C18 118.2(2) . . ? C20 C19 H19A 120.9 . . ? C18 C19 H19A 120.9 . . ? C21 C20 C19 120.4(2) . . ? C21 C20 H20A 119.8 . . ? C19 C20 H20A 119.8 . . ? N4 C21 C20 121.9(2) . . ? N4 C21 H21A 119.1 . . ? C20 C21 H21A 119.1 . . ? N4 C22 C18 122.72(19) . . ? N4 C22 H22A 118.6 . . ? C18 C22 H22A 118.6 . . ? O4 C23 O3 123.97(19) . . ? O4 C23 C24 120.68(18) . . ? O3 C23 C24 115.25(18) . . ? C31 C24 C25 118.83(19) . . ? C31 C24 C23 120.98(18) . . ? C25 C24 C23 120.11(19) . . ? C26 C25 C24 120.91(19) . . ? C26 C25 H25A 119.5 . . ? C24 C25 H25A 119.5 . . ? C25 C26 C28 119.93(18) . . ? C25 C26 C27 120.48(19) . . ? C28 C26 C27 119.59(18) . . ? O6 C27 O5 125.32(19) . . ? O6 C27 C26 119.8(2) . . ? O5 C27 C26 114.84(18) . . ? C26 C28 C29 119.74(19) . . ? C26 C28 H28A 120.1 . . ? C29 C28 H28A 120.1 . . ? C31 C29 C28 119.65(19) . . ? C31 C29 C30 119.16(18) . . ? C28 C29 C30 121.18(19) . . ? O8 C30 O7 123.8(2) . . ? O8 C30 C29 123.0(2) . . ? O7 C30 C29 113.13(18) . . ? C24 C31 C29 120.91(18) . . ? C24 C31 H31A 119.5 . . ? C29 C31 H31A 119.5 . . ? H9E O9 H9F 108.6 . . ? H10D O10 H10E 108.3 . . ? _diffrn_measured_fraction_theta_max 0.856 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.708 _refine_diff_density_min -0.437 _refine_diff_density_rms 0.070 _database_code_depnum_ccdc_archive 'CCDC 917801' ####################################################################### # # 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 #TrackingRef 'all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H48 N7 O7 Zn' _chemical_formula_weight 804.22 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.7047(8) _cell_length_b 8.9034(11) _cell_length_c 29.447(4) _cell_angle_alpha 89.256(12) _cell_angle_beta 89.387(10) _cell_angle_gamma 71.385(10) _cell_volume 1914.1(4) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 18 _cell_measurement_theta_min 5.38 _cell_measurement_theta_max 12.52 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.4 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.395 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 846 _exptl_absorpt_coefficient_mu 0.702 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8422 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details '(XSCANS; Siemens, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8308 _diffrn_reflns_av_R_equivalents 0.0357 _diffrn_reflns_av_sigmaI/netI 0.0373 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6701 _reflns_number_gt 5722 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XSCANS (Siemens, 1995)' _computing_cell_refinement 'XSCANS (Siemens, 1995)' _computing_data_reduction 'SHELXTL (Sheldrick, 2008)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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^)+(0.0577P)^2^+1.3771P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6701 _refine_ls_number_parameters 496 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0533 _refine_ls_R_factor_gt 0.0433 _refine_ls_wR_factor_ref 0.1179 _refine_ls_wR_factor_gt 0.1110 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn Zn 0.16247(4) 0.37936(4) 0.054538(10) 0.03462(11) Uani 1 1 d . . . O1 O 0.4433(4) 0.2925(3) 0.28417(9) 0.0849(9) Uani 1 1 d . . . O2 O 0.2198(3) 1.2711(3) 0.67647(9) 0.0697(7) Uani 1 1 d . . . O3 O -0.1272(3) 2.0016(3) 0.69922(8) 0.0653(7) Uani 1 1 d . . . O4 O 0.8538(3) 0.3377(3) 0.07854(11) 0.0816(9) Uani 1 1 d . . . O5 O 0.9212(3) 0.5340(3) 0.04772(10) 0.0694(7) Uani 1 1 d . . . O6 O 0.7385(3) 0.7979(2) -0.01485(7) 0.0448(5) Uani 1 1 d . . . O7 O 0.6847(3) 0.9070(3) 0.05306(8) 0.0584(6) Uani 1 1 d . . . N1 N 0.2552(3) 0.2815(3) 0.11635(7) 0.0351(5) Uani 1 1 d . . . N2 N 0.2293(3) 0.4174(3) 0.23278(8) 0.0435(6) Uani 1 1 d . . . H2A H 0.1311 0.4964 0.2290 0.052 Uiso 1 1 calc R . . N3 N 0.4848(3) 1.1764(3) 0.71511(8) 0.0461(6) Uani 1 1 d . . . H3A H 0.5906 1.1048 0.7147 0.055 Uiso 1 1 calc R . . N4 N 0.2743(4) 1.5278(3) 0.78544(11) 0.0696(9) Uani 1 1 d . . . N5 N 0.0160(4) 2.2367(3) 0.80703(10) 0.0552(7) Uani 1 1 d . . . N6 N 0.0874(4) 1.8613(3) 0.74770(9) 0.0603(8) Uani 1 1 d . . . H6A H 0.1690 1.7706 0.7522 0.072 Uiso 1 1 calc R . . N7 N 0.3077(3) 0.5397(3) 0.05225(7) 0.0341(5) Uani 1 1 d . . . C1 C 0.3884(4) 0.1426(3) 0.11862(10) 0.0421(6) Uani 1 1 d . . . H1A H 0.4241 0.0835 0.0923 0.051 Uiso 1 1 calc R . . C2 C 0.4739(4) 0.0846(4) 0.15862(11) 0.0493(7) Uani 1 1 d . . . H2B H 0.5662 -0.0129 0.1591 0.059 Uiso 1 1 calc R . . C3 C 0.4247(4) 0.1688(4) 0.19784(10) 0.0484(7) Uani 1 1 d . . . H3B H 0.4821 0.1295 0.2251 0.058 Uiso 1 1 calc R . . C4 C 0.2871(4) 0.3144(3) 0.19601(9) 0.0365(6) Uani 1 1 d . . . C5 C 0.2053(4) 0.3646(3) 0.15454(9) 0.0361(6) Uani 1 1 d . . . H5B H 0.1111 0.4608 0.1531 0.043 Uiso 1 1 calc R . . C6 C 0.3127(4) 0.4051(4) 0.27382(10) 0.0458(7) Uani 1 1 d . . . C7 C 0.2319(4) 0.5436(4) 0.30483(9) 0.0435(7) Uani 1 1 d . . . H7A H 0.1063 0.5510 0.3119 0.052 Uiso 1 1 calc R . . H7B H 0.2300 0.6403 0.2890 0.052 Uiso 1 1 calc R . . C8 C 0.3362(4) 0.5317(4) 0.34881(10) 0.0476(7) Uani 1 1 d . . . H8A H 0.3435 0.4327 0.3640 0.057 Uiso 1 1 calc R . . H8B H 0.4601 0.5302 0.3419 0.057 Uiso 1 1 calc R . . C9 C 0.2475(4) 0.6676(4) 0.38045(9) 0.0468(7) Uani 1 1 d . . . H9A H 0.1252 0.6666 0.3882 0.056 Uiso 1 1 calc R . . H9B H 0.2359 0.7668 0.3647 0.056 Uiso 1 1 calc R . . C10 C 0.3550(5) 0.6601(4) 0.42396(10) 0.0498(7) Uani 1 1 d . . . H10A H 0.3654 0.5612 0.4397 0.060 Uiso 1 1 calc R . . H10B H 0.4778 0.6593 0.4160 0.060 Uiso 1 1 calc R . . C11 C 0.2709(5) 0.7955(4) 0.45605(10) 0.0496(7) Uani 1 1 d . . . H11A H 0.1483 0.7962 0.4641 0.060 Uiso 1 1 calc R . . H11B H 0.2601 0.8945 0.4404 0.060 Uiso 1 1 calc R . . C12 C 0.3791(5) 0.7876(4) 0.49924(10) 0.0520(8) Uani 1 1 d . . . H12A H 0.3891 0.6888 0.5150 0.062 Uiso 1 1 calc R . . H12B H 0.5020 0.7860 0.4911 0.062 Uiso 1 1 calc R . . C13 C 0.2966(5) 0.9234(4) 0.53143(10) 0.0514(8) Uani 1 1 d . . . H13A H 0.1744 0.9241 0.5401 0.062 Uiso 1 1 calc R . . H13B H 0.2850 1.0224 0.5157 0.062 Uiso 1 1 calc R . . C14 C 0.4083(5) 0.9142(4) 0.57401(10) 0.0504(7) Uani 1 1 d . . . H14A H 0.5309 0.9118 0.5653 0.060 Uiso 1 1 calc R . . H14B H 0.4184 0.8157 0.5899 0.060 Uiso 1 1 calc R . . C15 C 0.3286(4) 1.0507(4) 0.60630(10) 0.0502(7) Uani 1 1 d . . . H15A H 0.2084 1.0505 0.6163 0.060 Uiso 1 1 calc R . . H15B H 0.3137 1.1498 0.5902 0.060 Uiso 1 1 calc R . . C16 C 0.4484(4) 1.0415(4) 0.64748(10) 0.0494(7) Uani 1 1 d . . . H16A H 0.4648 0.9414 0.6631 0.059 Uiso 1 1 calc R . . H16B H 0.5680 1.0429 0.6373 0.059 Uiso 1 1 calc R . . C17 C 0.3709(4) 1.1744(4) 0.68034(10) 0.0437(7) Uani 1 1 d . . . C18 C 0.4490(4) 1.2826(3) 0.75165(9) 0.0397(6) Uani 1 1 d . . . C19 C 0.5596(4) 1.2476(4) 0.78930(10) 0.0464(7) Uani 1 1 d . . . H19A H 0.6574 1.1538 0.7908 0.056 Uiso 1 1 calc R . . C20 C 0.5242(5) 1.3529(4) 0.82477(11) 0.0551(8) Uani 1 1 d . . . H20A H 0.5968 1.3303 0.8506 0.066 Uiso 1 1 calc R . . C21 C 0.3816(5) 1.4907(4) 0.82156(11) 0.0552(8) Uani 1 1 d . . . H21A H 0.3587 1.5612 0.8456 0.066 Uiso 1 1 calc R . . C22 C 0.3073(5) 1.4241(4) 0.75192(12) 0.0654(10) Uani 1 1 d . . . H22A H 0.2299 1.4484 0.7270 0.078 Uiso 1 1 calc R . . C23 C 0.0162(5) 2.1850(4) 0.84985(12) 0.0595(9) Uani 1 1 d . . . H23A H 0.0014 2.2579 0.8731 0.071 Uiso 1 1 calc R . . C24 C 0.0369(5) 2.0312(4) 0.86145(12) 0.0600(9) Uani 1 1 d . . . H24A H 0.0385 2.0004 0.8918 0.072 Uiso 1 1 calc R . . C25 C 0.0553(4) 1.9232(4) 0.82755(11) 0.0527(8) Uani 1 1 d . . . H25A H 0.0657 1.8185 0.8345 0.063 Uiso 1 1 calc R . . C26 C 0.0580(4) 1.9717(3) 0.78317(11) 0.0459(7) Uani 1 1 d . . . C27 C 0.0406(4) 2.1298(4) 0.77448(11) 0.0496(7) Uani 1 1 d . . . H27A H 0.0463 2.1621 0.7445 0.060 Uiso 1 1 calc R . . C28 C 0.0006(4) 1.8831(3) 0.70738(10) 0.0438(7) Uani 1 1 d . . . C29 C 0.0756(5) 1.7512(4) 0.67395(11) 0.0531(8) Uani 1 1 d . . . H29A H 0.0757 1.6526 0.6884 0.064 Uiso 1 1 calc R . . H29B H 0.2020 1.7425 0.6674 0.064 Uiso 1 1 calc R . . C30 C -0.0254(4) 1.7680(4) 0.62937(10) 0.0474(7) Uani 1 1 d . . . H30A H -0.0274 1.8665 0.6146 0.057 Uiso 1 1 calc R . . H30B H -0.1511 1.7728 0.6353 0.057 Uiso 1 1 calc R . . C31 C 0.0637(4) 1.6307(4) 0.59781(10) 0.0487(7) Uani 1 1 d . . . H31A H 0.0721 1.5323 0.6136 0.058 Uiso 1 1 calc R . . H31B H 0.1875 1.6297 0.5909 0.058 Uiso 1 1 calc R . . C32 C -0.0383(4) 1.6368(4) 0.55327(10) 0.0494(7) Uani 1 1 d . . . H32A H -0.1624 1.6387 0.5601 0.059 Uiso 1 1 calc R . . H32B H -0.0457 1.7347 0.5373 0.059 Uiso 1 1 calc R . . C33 C 0.0510(4) 1.4981(4) 0.52205(10) 0.0489(7) Uani 1 1 d . . . H33A H 0.1745 1.4971 0.5149 0.059 Uiso 1 1 calc R . . H33B H 0.0600 1.4002 0.5382 0.059 Uiso 1 1 calc R . . C34 C 0.4886(3) 0.4772(3) 0.06006(8) 0.0348(6) Uani 1 1 d . . . H34A H 0.5331 0.3734 0.0709 0.042 Uiso 1 1 calc R . . C35 C 0.6107(3) 0.5591(3) 0.05288(8) 0.0334(6) Uani 1 1 d . . . C36 C 0.5454(3) 0.7148(3) 0.03647(9) 0.0350(6) Uani 1 1 d . . . C37 C 0.3567(4) 0.7814(3) 0.03030(10) 0.0406(6) Uani 1 1 d . . . H37A H 0.3075 0.8864 0.0208 0.049 Uiso 1 1 calc R . . C38 C 0.2440(3) 0.6910(3) 0.03824(9) 0.0377(6) Uani 1 1 d . . . H38A H 0.1188 0.7367 0.0337 0.045 Uiso 1 1 calc R . . C39 C 0.8089(4) 0.4702(4) 0.06100(9) 0.0412(7) Uani 1 1 d . . . C40 C 0.6688(4) 0.8134(3) 0.02508(9) 0.0381(6) 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 Zn 0.02820(17) 0.03893(19) 0.03511(18) -0.00722(13) -0.00302(12) -0.00807(12) O1 0.103(2) 0.0638(16) 0.0564(15) -0.0148(13) -0.0355(15) 0.0193(15) O2 0.0499(14) 0.0790(17) 0.0631(15) -0.0273(13) -0.0154(11) 0.0049(12) O3 0.0569(14) 0.0623(15) 0.0570(14) -0.0148(12) -0.0204(11) 0.0096(12) O4 0.0467(14) 0.0679(18) 0.124(2) 0.0228(17) -0.0214(15) -0.0093(12) O5 0.0285(11) 0.0628(15) 0.116(2) 0.0209(14) 0.0006(12) -0.0135(10) O6 0.0518(12) 0.0427(11) 0.0433(11) -0.0122(9) 0.0115(9) -0.0199(9) O7 0.0631(14) 0.0656(15) 0.0586(14) -0.0341(12) 0.0162(11) -0.0369(12) N1 0.0355(11) 0.0345(12) 0.0339(12) -0.0058(9) -0.0007(9) -0.0090(9) N2 0.0460(13) 0.0428(13) 0.0325(12) -0.0091(10) -0.0072(10) -0.0008(11) N3 0.0485(14) 0.0413(13) 0.0387(13) -0.0082(11) -0.0098(11) -0.0001(11) N4 0.081(2) 0.0443(16) 0.0657(19) -0.0166(14) -0.0222(16) 0.0058(14) N5 0.0648(17) 0.0360(14) 0.0616(18) -0.0136(12) 0.0042(14) -0.0114(12) N6 0.0742(19) 0.0355(14) 0.0543(16) -0.0133(12) -0.0287(14) 0.0076(13) N7 0.0277(10) 0.0430(13) 0.0330(11) -0.0084(9) -0.0009(9) -0.0130(9) C1 0.0444(15) 0.0351(15) 0.0430(16) -0.0091(12) 0.0060(12) -0.0072(12) C2 0.0471(17) 0.0376(16) 0.0521(18) -0.0034(13) -0.0009(14) 0.0022(13) C3 0.0536(18) 0.0418(16) 0.0405(16) -0.0005(13) -0.0086(13) -0.0020(13) C4 0.0381(14) 0.0353(14) 0.0354(14) -0.0042(11) -0.0016(11) -0.0106(11) C5 0.0376(14) 0.0335(14) 0.0345(14) -0.0060(11) -0.0023(11) -0.0073(11) C6 0.0553(18) 0.0439(17) 0.0336(15) -0.0003(12) -0.0057(13) -0.0094(14) C7 0.0491(16) 0.0476(17) 0.0307(14) -0.0045(12) -0.0042(12) -0.0105(13) C8 0.0554(18) 0.0507(18) 0.0345(15) -0.0019(13) -0.0079(13) -0.0135(14) C9 0.0547(18) 0.0507(18) 0.0334(15) -0.0046(13) -0.0049(13) -0.0141(14) C10 0.0594(19) 0.0508(18) 0.0376(16) -0.0056(13) -0.0084(14) -0.0145(15) C11 0.0585(19) 0.0513(18) 0.0376(16) -0.0043(13) -0.0092(14) -0.0151(15) C12 0.062(2) 0.0554(19) 0.0372(16) -0.0086(14) -0.0089(14) -0.0160(16) C13 0.0594(19) 0.0519(19) 0.0410(17) -0.0080(14) -0.0076(14) -0.0146(15) C14 0.0575(19) 0.0486(18) 0.0422(17) -0.0080(14) -0.0066(14) -0.0124(15) C15 0.0550(18) 0.0519(18) 0.0402(16) -0.0068(14) -0.0076(14) -0.0118(15) C16 0.0553(18) 0.0473(17) 0.0401(16) -0.0072(13) -0.0084(13) -0.0081(14) C17 0.0469(17) 0.0456(16) 0.0353(15) -0.0030(12) -0.0025(12) -0.0100(14) C18 0.0458(15) 0.0365(15) 0.0352(14) -0.0032(11) -0.0022(12) -0.0106(12) C19 0.0429(16) 0.0444(16) 0.0445(16) -0.0046(13) -0.0072(13) -0.0029(13) C20 0.060(2) 0.059(2) 0.0403(17) -0.0079(14) -0.0122(14) -0.0098(16) C21 0.066(2) 0.0462(18) 0.0478(18) -0.0126(14) -0.0015(16) -0.0099(16) C22 0.080(2) 0.0429(18) 0.057(2) -0.0083(15) -0.0311(18) 0.0056(16) C23 0.067(2) 0.0496(19) 0.055(2) -0.0212(16) 0.0037(16) -0.0086(16) C24 0.069(2) 0.057(2) 0.0469(18) -0.0072(15) 0.0018(16) -0.0096(17) C25 0.0567(19) 0.0429(17) 0.056(2) 0.0024(14) -0.0113(15) -0.0126(14) C26 0.0454(16) 0.0352(15) 0.0503(18) -0.0105(13) -0.0123(13) -0.0024(12) C27 0.0556(18) 0.0388(16) 0.0483(17) -0.0069(13) -0.0021(14) -0.0059(13) C28 0.0479(17) 0.0395(16) 0.0408(16) -0.0012(12) -0.0104(13) -0.0093(13) C29 0.061(2) 0.0430(17) 0.0464(18) -0.0098(14) -0.0154(15) -0.0033(14) C30 0.0530(17) 0.0463(17) 0.0388(16) -0.0047(13) -0.0076(13) -0.0098(14) C31 0.0539(18) 0.0504(18) 0.0384(16) -0.0085(13) -0.0043(13) -0.0114(14) C32 0.0575(19) 0.0504(18) 0.0373(16) -0.0065(13) -0.0050(13) -0.0124(15) C33 0.0569(18) 0.0504(18) 0.0380(16) -0.0080(13) -0.0012(14) -0.0146(15) C34 0.0317(13) 0.0428(15) 0.0287(13) -0.0091(11) -0.0040(10) -0.0096(11) C35 0.0275(12) 0.0441(15) 0.0276(13) -0.0122(11) -0.0003(10) -0.0094(11) C36 0.0316(13) 0.0447(15) 0.0298(13) -0.0172(11) 0.0038(10) -0.0132(11) C37 0.0345(14) 0.0369(15) 0.0485(16) -0.0076(12) -0.0016(12) -0.0082(11) C38 0.0265(13) 0.0405(15) 0.0436(15) -0.0089(12) -0.0017(11) -0.0070(11) C39 0.0343(14) 0.0507(18) 0.0360(15) -0.0113(13) -0.0031(11) -0.0092(13) C40 0.0310(13) 0.0407(15) 0.0431(16) -0.0136(12) 0.0029(11) -0.0117(11) _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 Zn O6 1.9236(19) 2_665 ? Zn O5 1.938(2) 1_455 ? Zn N1 2.042(2) . ? Zn N7 2.076(2) . ? Zn C39 2.588(3) 1_455 ? O1 C6 1.210(4) . ? O2 C17 1.213(4) . ? O3 C28 1.215(4) . ? O4 C39 1.227(4) . ? O5 C39 1.235(4) . ? O5 Zn 1.938(2) 1_655 ? O6 C40 1.278(3) . ? O6 Zn 1.9236(19) 2_665 ? O7 C40 1.214(3) . ? N1 C1 1.333(3) . ? N1 C5 1.338(3) . ? N2 C6 1.362(4) . ? N2 C4 1.402(3) . ? N2 H2A 0.8600 . ? N3 C17 1.360(4) . ? N3 C18 1.407(3) . ? N3 H3A 0.8600 . ? N4 C21 1.326(4) . ? N4 C22 1.327(4) . ? N5 C27 1.329(4) . ? N5 C23 1.337(5) . ? N6 C28 1.350(4) . ? N6 C26 1.410(4) . ? N6 H6A 0.8600 . ? N7 C38 1.339(4) . ? N7 C34 1.346(3) . ? C1 C2 1.368(4) . ? C1 H1A 0.9300 . ? C2 C3 1.368(4) . ? C2 H2B 0.9300 . ? C3 C4 1.389(4) . ? C3 H3B 0.9300 . ? C4 C5 1.382(4) . ? C5 H5B 0.9300 . ? C6 C7 1.506(4) . ? C7 C8 1.516(4) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.512(4) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.522(4) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.511(4) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.517(4) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.513(4) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.515(4) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.516(4) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.517(4) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.503(4) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C18 C19 1.376(4) . ? C18 C22 1.379(4) . ? C19 C20 1.379(4) . ? C19 H19A 0.9300 . ? C20 C21 1.364(5) . ? C20 H20A 0.9300 . ? C21 H21A 0.9300 . ? C22 H22A 0.9300 . ? C23 C24 1.367(5) . ? C23 H23A 0.9300 . ? C24 C25 1.369(5) . ? C24 H24A 0.9300 . ? C25 C26 1.373(5) . ? C25 H25A 0.9300 . ? C26 C27 1.391(4) . ? C27 H27A 0.9300 . ? C28 C29 1.506(4) . ? C29 C30 1.514(4) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 C31 1.520(4) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C32 1.528(4) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 C33 1.523(4) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C33 1.519(6) 2_586 ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C35 1.375(4) . ? C34 H34A 0.9300 . ? C35 C36 1.397(4) . ? C35 C39 1.499(4) . ? C36 C37 1.397(4) . ? C36 C40 1.518(4) . ? C37 C38 1.377(4) . ? C37 H37A 0.9300 . ? C38 H38A 0.9300 . ? C39 Zn 2.588(3) 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 O6 Zn O5 123.90(11) 2_665 1_455 ? O6 Zn N1 101.71(9) 2_665 . ? O5 Zn N1 121.43(11) 1_455 . ? O6 Zn N7 113.18(8) 2_665 . ? O5 Zn N7 96.60(9) 1_455 . ? N1 Zn N7 96.73(9) . . ? O6 Zn C39 113.55(9) 2_665 1_455 ? O5 Zn C39 27.12(10) 1_455 1_455 ? N1 Zn C39 105.33(9) . 1_455 ? N7 Zn C39 122.06(9) . 1_455 ? C39 O5 Zn 107.2(2) . 1_655 ? C40 O6 Zn 133.97(19) . 2_665 ? C1 N1 C5 118.3(2) . . ? C1 N1 Zn 119.87(18) . . ? C5 N1 Zn 121.05(18) . . ? C6 N2 C4 126.7(2) . . ? C6 N2 H2A 116.7 . . ? C4 N2 H2A 116.7 . . ? C17 N3 C18 127.3(2) . . ? C17 N3 H3A 116.3 . . ? C18 N3 H3A 116.3 . . ? C21 N4 C22 117.7(3) . . ? C27 N5 C23 117.0(3) . . ? C28 N6 C26 126.7(3) . . ? C28 N6 H6A 116.6 . . ? C26 N6 H6A 116.6 . . ? C38 N7 C34 117.8(2) . . ? C38 N7 Zn 126.29(17) . . ? C34 N7 Zn 115.25(18) . . ? N1 C1 C2 121.7(3) . . ? N1 C1 H1A 119.1 . . ? C2 C1 H1A 119.1 . . ? C1 C2 C3 120.5(3) . . ? C1 C2 H2B 119.7 . . ? C3 C2 H2B 119.7 . . ? C2 C3 C4 118.5(3) . . ? C2 C3 H3B 120.7 . . ? C4 C3 H3B 120.7 . . ? C5 C4 C3 117.8(2) . . ? C5 C4 N2 117.3(2) . . ? C3 C4 N2 124.9(3) . . ? N1 C5 C4 123.2(2) . . ? N1 C5 H5B 118.4 . . ? C4 C5 H5B 118.4 . . ? O1 C6 N2 122.4(3) . . ? O1 C6 C7 122.8(3) . . ? N2 C6 C7 114.8(2) . . ? C6 C7 C8 113.4(2) . . ? C6 C7 H7A 108.9 . . ? C8 C7 H7A 108.9 . . ? C6 C7 H7B 108.9 . . ? C8 C7 H7B 108.9 . . ? H7A C7 H7B 107.7 . . ? C9 C8 C7 112.6(3) . . ? C9 C8 H8A 109.1 . . ? C7 C8 H8A 109.1 . . ? C9 C8 H8B 109.1 . . ? C7 C8 H8B 109.1 . . ? H8A C8 H8B 107.8 . . ? C8 C9 C10 113.0(3) . . ? C8 C9 H9A 109.0 . . ? C10 C9 H9A 109.0 . . ? C8 C9 H9B 109.0 . . ? C10 C9 H9B 109.0 . . ? H9A C9 H9B 107.8 . . ? C11 C10 C9 114.2(3) . . ? C11 C10 H10A 108.7 . . ? C9 C10 H10A 108.7 . . ? C11 C10 H10B 108.7 . . ? C9 C10 H10B 108.7 . . ? H10A C10 H10B 107.6 . . ? C10 C11 C12 113.9(3) . . ? C10 C11 H11A 108.8 . . ? C12 C11 H11A 108.8 . . ? C10 C11 H11B 108.8 . . ? C12 C11 H11B 108.8 . . ? H11A C11 H11B 107.7 . . ? C13 C12 C11 114.3(3) . . ? C13 C12 H12A 108.7 . . ? C11 C12 H12A 108.7 . . ? C13 C12 H12B 108.7 . . ? C11 C12 H12B 108.7 . . ? H12A C12 H12B 107.6 . . ? C12 C13 C14 113.4(3) . . ? C12 C13 H13A 108.9 . . ? C14 C13 H13A 108.9 . . ? C12 C13 H13B 108.9 . . ? C14 C13 H13B 108.9 . . ? H13A C13 H13B 107.7 . . ? C13 C14 C15 114.0(3) . . ? C13 C14 H14A 108.8 . . ? C15 C14 H14A 108.8 . . ? C13 C14 H14B 108.8 . . ? C15 C14 H14B 108.8 . . ? H14A C14 H14B 107.6 . . ? C14 C15 C16 112.5(3) . . ? C14 C15 H15A 109.1 . . ? C16 C15 H15A 109.1 . . ? C14 C15 H15B 109.1 . . ? C16 C15 H15B 109.1 . . ? H15A C15 H15B 107.8 . . ? C17 C16 C15 113.5(3) . . ? C17 C16 H16A 108.9 . . ? C15 C16 H16A 108.9 . . ? C17 C16 H16B 108.9 . . ? C15 C16 H16B 108.9 . . ? H16A C16 H16B 107.7 . . ? O2 C17 N3 122.7(3) . . ? O2 C17 C16 123.2(3) . . ? N3 C17 C16 114.1(2) . . ? C19 C18 C22 116.9(3) . . ? C19 C18 N3 119.8(3) . . ? C22 C18 N3 123.3(3) . . ? C18 C19 C20 119.4(3) . . ? C18 C19 H19A 120.3 . . ? C20 C19 H19A 120.3 . . ? C21 C20 C19 119.3(3) . . ? C21 C20 H20A 120.4 . . ? C19 C20 H20A 120.4 . . ? N4 C21 C20 122.5(3) . . ? N4 C21 H21A 118.8 . . ? C20 C21 H21A 118.8 . . ? N4 C22 C18 124.2(3) . . ? N4 C22 H22A 117.9 . . ? C18 C22 H22A 117.9 . . ? N5 C23 C24 123.8(3) . . ? N5 C23 H23A 118.1 . . ? C24 C23 H23A 118.1 . . ? C23 C24 C25 118.7(3) . . ? C23 C24 H24A 120.6 . . ? C25 C24 H24A 120.6 . . ? C24 C25 C26 119.1(3) . . ? C24 C25 H25A 120.4 . . ? C26 C25 H25A 120.4 . . ? C25 C26 C27 118.3(3) . . ? C25 C26 N6 120.3(3) . . ? C27 C26 N6 121.3(3) . . ? N5 C27 C26 123.0(3) . . ? N5 C27 H27A 118.5 . . ? C26 C27 H27A 118.5 . . ? O3 C28 N6 121.6(3) . . ? O3 C28 C29 123.5(3) . . ? N6 C28 C29 114.9(2) . . ? C28 C29 C30 116.1(3) . . ? C28 C29 H29A 108.3 . . ? C30 C29 H29A 108.3 . . ? C28 C29 H29B 108.3 . . ? C30 C29 H29B 108.3 . . ? H29A C29 H29B 107.4 . . ? C29 C30 C31 111.8(3) . . ? C29 C30 H30A 109.2 . . ? C31 C30 H30A 109.2 . . ? C29 C30 H30B 109.2 . . ? C31 C30 H30B 109.2 . . ? H30A C30 H30B 107.9 . . ? C30 C31 C32 114.1(3) . . ? C30 C31 H31A 108.7 . . ? C32 C31 H31A 108.7 . . ? C30 C31 H31B 108.7 . . ? C32 C31 H31B 108.7 . . ? H31A C31 H31B 107.6 . . ? C33 C32 C31 113.8(3) . . ? C33 C32 H32A 108.8 . . ? C31 C32 H32A 108.8 . . ? C33 C32 H32B 108.8 . . ? C31 C32 H32B 108.8 . . ? H32A C32 H32B 107.7 . . ? C33 C33 C32 114.1(3) 2_586 . ? C33 C33 H33A 108.7 2_586 . ? C32 C33 H33A 108.7 . . ? C33 C33 H33B 108.7 2_586 . ? C32 C33 H33B 108.7 . . ? H33A C33 H33B 107.6 . . ? N7 C34 C35 123.3(3) . . ? N7 C34 H34A 118.3 . . ? C35 C34 H34A 118.3 . . ? C34 C35 C36 118.9(2) . . ? C34 C35 C39 116.8(3) . . ? C36 C35 C39 124.2(2) . . ? C37 C36 C35 117.6(2) . . ? C37 C36 C40 119.0(3) . . ? C35 C36 C40 123.4(2) . . ? C38 C37 C36 119.8(3) . . ? C38 C37 H37A 120.1 . . ? C36 C37 H37A 120.1 . . ? N7 C38 C37 122.5(2) . . ? N7 C38 H38A 118.7 . . ? C37 C38 H38A 118.7 . . ? O4 C39 O5 122.9(3) . . ? O4 C39 C35 120.1(3) . . ? O5 C39 C35 116.9(3) . . ? O4 C39 Zn 77.35(18) . 1_655 ? O5 C39 Zn 45.68(14) . 1_655 ? C35 C39 Zn 161.4(2) . 1_655 ? O7 C40 O6 125.1(3) . . ? O7 C40 C36 118.3(2) . . ? O6 C40 C36 116.5(2) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.816 _refine_diff_density_min -0.416 _refine_diff_density_rms 0.060 _database_code_depnum_ccdc_archive 'CCDC 917802' ####################################################################### # # 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 #TrackingRef 'all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H49 Cd N6 O8' _chemical_formula_weight 866.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.94090(10) _cell_length_b 8.75380(10) _cell_length_c 38.6259(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.2160(10) _cell_angle_gamma 90.00 _cell_volume 4020.78(7) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 6988 _cell_measurement_theta_min 2.227 _cell_measurement_theta_max 26.628 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.431 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1796 _exptl_absorpt_coefficient_mu 0.603 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6227 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_process_details 'SADABS V2008/1 (Bruker AXS, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_reflns_number 37296 _diffrn_reflns_av_R_equivalents 0.0963 _diffrn_reflns_av_sigmaI/netI 0.1015 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -51 _diffrn_reflns_limit_l_max 48 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 28.29 _reflns_number_total 9987 _reflns_number_gt 5963 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2010)' _computing_cell_refinement 'SAINT V7.68A (Bruker AXS, 2010)' _computing_data_reduction 'SAINT V7.68A (Bruker AXS, 2010)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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^)+(0.0359P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9987 _refine_ls_number_parameters 505 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1142 _refine_ls_R_factor_gt 0.0529 _refine_ls_wR_factor_ref 0.1027 _refine_ls_wR_factor_gt 0.0873 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _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 Cd Cd 0.323460(19) -1.05132(3) 0.208640(6) 0.02749(6) Uani 1 1 d . . . N1 N 0.2998(2) -1.1868(3) 0.15638(7) 0.0345(7) Uani 1 1 d . . . N2 N 0.4766(2) -1.3146(3) 0.08996(7) 0.0411(8) Uani 1 1 d . . . H2A H 0.5268 -1.2445 0.0936 0.049 Uiso 1 1 calc R . . N3 N 1.3578(2) -2.2173(3) -0.13154(8) 0.0464(9) Uani 1 1 d . . . H3A H 1.3141 -2.2931 -0.1284 0.056 Uiso 1 1 calc R . . N4 N 1.5899(2) -2.1575(3) -0.18669(7) 0.0327(7) Uani 1 1 d . . . N5 N 1.1991(3) -2.5242(4) -0.13543(9) 0.0622(11) Uani 1 1 d . . . N6 N 0.9370(2) -2.3017(3) -0.13433(8) 0.0437(8) Uani 1 1 d . . . H6A H 0.9011 -2.2451 -0.1498 0.052 Uiso 1 1 calc R . . O1 O 0.4350(2) -1.5324(4) 0.06087(9) 0.0799(10) Uani 1 1 d . . . O2 O 1.3887(2) -1.9680(3) -0.11773(7) 0.0493(7) Uani 1 1 d . . . O3 O 0.14430(18) -1.1016(3) 0.22562(6) 0.0391(6) Uani 1 1 d . . . O4 O 0.14542(18) -0.9060(3) 0.19032(6) 0.0406(7) Uani 1 1 d . . . O5 O 0.12426(17) -0.7777(3) 0.26129(6) 0.0408(7) Uani 1 1 d . . . O6 O -0.01528(19) -0.6512(3) 0.27961(7) 0.0541(8) Uani 1 1 d . . . O7 O 0.9494(2) -2.3636(3) -0.07760(7) 0.0569(8) Uani 1 1 d . . . O8 O 0.32924(18) -0.9140(3) 0.26204(6) 0.0380(6) Uani 1 1 d . . . C1 C 0.2006(3) -1.2494(4) 0.14509(9) 0.0409(10) Uani 1 1 d . . . H1A H 0.1392 -1.2326 0.1578 0.049 Uiso 1 1 calc R . . C2 C 0.1861(3) -1.3366(4) 0.11576(9) 0.0438(10) Uani 1 1 d . . . H2B H 0.1160 -1.3784 0.1089 0.053 Uiso 1 1 calc R . . C3 C 0.2757(3) -1.3630(4) 0.09628(9) 0.0413(10) Uani 1 1 d . . . H3B H 0.2669 -1.4225 0.0763 0.050 Uiso 1 1 calc R . . C4 C 0.3784(3) -1.2992(4) 0.10719(9) 0.0324(8) Uani 1 1 d . . . C5 C 0.3861(3) -1.2141(4) 0.13753(9) 0.0375(9) Uani 1 1 d . . . H5B H 0.4558 -1.1732 0.1453 0.045 Uiso 1 1 calc R . . C6 C 0.4997(3) -1.4304(5) 0.06804(9) 0.0444(10) Uani 1 1 d . . . C7 C 0.6145(3) -1.4194(4) 0.05458(10) 0.0480(11) Uani 1 1 d . . . H7A H 0.6707 -1.4035 0.0740 0.058 Uiso 1 1 calc R . . H7B H 0.6161 -1.3316 0.0393 0.058 Uiso 1 1 calc R . . C8 C 0.6443(3) -1.5616(5) 0.03494(10) 0.0489(10) Uani 1 1 d . . . H8B H 0.5870 -1.5791 0.0159 0.059 Uiso 1 1 calc R . . H8C H 0.6447 -1.6490 0.0504 0.059 Uiso 1 1 calc R . . C9 C 0.7586(3) -1.5494(5) 0.02048(9) 0.0474(10) Uani 1 1 d . . . H9A H 0.7571 -1.4643 0.0044 0.057 Uiso 1 1 calc R . . H9B H 0.8153 -1.5276 0.0394 0.057 Uiso 1 1 calc R . . C10 C 0.7919(3) -1.6922(4) 0.00206(10) 0.0478(11) Uani 1 1 d . . . H10A H 0.7361 -1.7129 -0.0172 0.057 Uiso 1 1 calc R . . H10B H 0.7919 -1.7778 0.0180 0.057 Uiso 1 1 calc R . . C11 C 0.9073(3) -1.6806(5) -0.01166(10) 0.0478(11) Uani 1 1 d . . . H11A H 0.9636 -1.6649 0.0078 0.057 Uiso 1 1 calc R . . H11B H 0.9084 -1.5922 -0.0268 0.057 Uiso 1 1 calc R . . C12 C 0.9381(3) -1.8221(4) -0.03173(10) 0.0461(10) Uani 1 1 d . . . H12A H 0.9383 -1.9101 -0.0164 0.055 Uiso 1 1 calc R . . H12B H 0.8807 -1.8390 -0.0508 0.055 Uiso 1 1 calc R . . C13 C 1.0518(3) -1.8112(5) -0.04628(10) 0.0485(11) Uani 1 1 d . . . H13A H 1.0534 -1.7198 -0.0604 0.058 Uiso 1 1 calc R . . H13B H 1.1098 -1.8011 -0.0272 0.058 Uiso 1 1 calc R . . C14 C 1.0781(3) -1.9481(5) -0.06803(10) 0.0503(10) Uani 1 1 d . . . H14A H 1.0216 -1.9557 -0.0876 0.060 Uiso 1 1 calc R . . H14B H 1.0733 -2.0398 -0.0541 0.060 Uiso 1 1 calc R . . C15 C 1.1939(3) -1.9421(4) -0.08167(10) 0.0499(10) Uani 1 1 d . . . H15A H 1.1973 -1.8549 -0.0970 0.060 Uiso 1 1 calc R . . H15B H 1.2506 -1.9280 -0.0623 0.060 Uiso 1 1 calc R . . C16 C 1.2199(3) -2.0855(4) -0.10108(10) 0.0498(11) Uani 1 1 d . . . H16A H 1.1599 -2.1028 -0.1193 0.060 Uiso 1 1 calc R . . H16B H 1.2206 -2.1713 -0.0852 0.060 Uiso 1 1 calc R . . C17 C 1.3307(3) -2.0815(4) -0.11718(9) 0.0395(10) Uani 1 1 d . . . C18 C 1.4491(3) -2.2468(4) -0.15092(9) 0.0367(9) Uani 1 1 d . . . C19 C 1.4861(3) -2.3948(4) -0.15467(10) 0.0455(10) Uani 1 1 d . . . H19A H 1.4522 -2.4752 -0.1438 0.055 Uiso 1 1 calc R . . C20 C 1.5745(3) -2.4219(4) -0.17482(10) 0.0482(11) Uani 1 1 d . . . H20A H 1.5987 -2.5212 -0.1784 0.058 Uiso 1 1 calc R . . C21 C 1.6260(3) -2.3002(4) -0.18955(9) 0.0394(9) Uani 1 1 d . . . H21A H 1.6880 -2.3186 -0.2019 0.047 Uiso 1 1 calc R . . C22 C 1.5017(3) -2.1319(4) -0.16803(9) 0.0362(9) Uani 1 1 d . . . H22A H 1.4750 -2.0325 -0.1666 0.043 Uiso 1 1 calc R . . C23 C 0.0970(3) -0.9890(4) 0.21066(8) 0.0275(8) Uani 1 1 d . . . C24 C -0.0245(2) -0.9603(4) 0.21616(8) 0.0291(8) Uani 1 1 d . . . C25 C -0.1043(3) -1.0450(4) 0.19598(9) 0.0395(9) Uani 1 1 d . . . H25A H -0.0811 -1.1152 0.1800 0.047 Uiso 1 1 calc R . . C26 C -0.2174(3) -1.0262(4) 0.19935(10) 0.0455(10) Uani 1 1 d . . . H26A H -0.2702 -1.0836 0.1858 0.055 Uiso 1 1 calc R . . C27 C -0.2520(3) -0.9217(5) 0.22298(10) 0.0453(11) Uani 1 1 d . . . H27A H -0.3282 -0.9086 0.2253 0.054 Uiso 1 1 calc R . . C28 C -0.1741(3) -0.8373(4) 0.24293(9) 0.0384(9) Uani 1 1 d . . . H28A H -0.1982 -0.7668 0.2587 0.046 Uiso 1 1 calc R . . C29 C -0.0599(2) -0.8551(4) 0.24005(8) 0.0287(8) Uani 1 1 d . . . C30 C 0.0211(3) -0.7562(4) 0.26188(8) 0.0289(8) Uani 1 1 d . . . C31 C 1.1952(4) -2.5533(5) -0.16953(12) 0.0645(13) Uani 1 1 d . . . H31A H 1.2542 -2.6070 -0.1779 0.077 Uiso 1 1 calc R . . C32 C 1.1079(4) -2.5073(5) -0.19263(12) 0.0612(13) Uani 1 1 d . . . H32A H 1.1072 -2.5313 -0.2161 0.073 Uiso 1 1 calc R . . C33 C 1.0220(3) -2.4258(4) -0.18072(9) 0.0479(11) Uani 1 1 d . . . H33A H 0.9626 -2.3928 -0.1961 0.057 Uiso 1 1 calc R . . C34 C 1.0232(3) -2.3923(4) -0.14575(9) 0.0372(9) Uani 1 1 d . . . C35 C 1.1130(3) -2.4465(5) -0.12409(10) 0.0493(10) Uani 1 1 d . . . H35A H 1.1136 -2.4281 -0.1004 0.059 Uiso 1 1 calc R . . C36 C 0.9033(3) -2.2927(4) -0.10139(10) 0.0419(10) Uani 1 1 d . . . C37 C 0.8025(3) -2.1916(5) -0.09844(10) 0.0502(11) Uani 1 1 d . . . H37A H 0.8209 -2.0886 -0.1052 0.060 Uiso 1 1 calc R . . H37B H 0.7411 -2.2275 -0.1146 0.060 Uiso 1 1 calc R . . C38 C 0.7638(3) -2.1877(4) -0.06242(9) 0.0455(10) Uani 1 1 d . . . H38A H 0.7476 -2.2913 -0.0555 0.055 Uiso 1 1 calc R . . H38B H 0.8248 -2.1497 -0.0464 0.055 Uiso 1 1 calc R . . C39 C 0.6615(3) -2.0906(4) -0.05904(10) 0.0503(11) Uani 1 1 d . . . H39A H 0.6014 -2.1251 -0.0758 0.060 Uiso 1 1 calc R . . H39B H 0.6788 -1.9858 -0.0647 0.060 Uiso 1 1 calc R . . C40 C 0.6208(3) -2.0953(4) -0.02311(10) 0.0498(11) Uani 1 1 d . . . H40A H 0.6822 -2.0642 -0.0064 0.060 Uiso 1 1 calc R . . H40B H 0.6022 -2.2001 -0.0179 0.060 Uiso 1 1 calc R . . C41 C 0.5198(3) -1.9962(5) -0.01797(10) 0.0542(12) Uani 1 1 d . . . H41A H 0.5384 -1.8910 -0.0229 0.065 Uiso 1 1 calc R . . H41B H 0.4584 -2.0265 -0.0347 0.065 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd 0.02694(11) 0.02613(12) 0.03049(12) 0.00044(13) 0.00850(9) 0.00287(12) N1 0.0396(16) 0.0307(17) 0.0344(17) -0.0044(14) 0.0101(13) 0.0040(13) N2 0.0445(17) 0.0396(19) 0.0419(18) -0.0129(15) 0.0181(14) -0.0026(14) N3 0.0457(18) 0.0368(19) 0.061(2) -0.0014(16) 0.0311(16) -0.0036(15) N4 0.0327(15) 0.0304(17) 0.0363(17) -0.0010(14) 0.0106(13) 0.0036(13) N5 0.052(2) 0.069(3) 0.066(3) -0.002(2) 0.0084(18) 0.0115(19) N6 0.0490(18) 0.047(2) 0.0353(18) 0.0080(15) 0.0073(15) 0.0116(15) O1 0.0658(19) 0.068(2) 0.113(3) -0.054(2) 0.0424(17) -0.0183(17) O2 0.0457(14) 0.0458(17) 0.0600(17) -0.0129(15) 0.0235(13) -0.0097(13) O3 0.0337(13) 0.0321(14) 0.0524(16) 0.0075(12) 0.0086(11) 0.0091(11) O4 0.0329(13) 0.0461(17) 0.0443(15) 0.0123(12) 0.0124(11) 0.0050(11) O5 0.0223(12) 0.0421(15) 0.0583(17) -0.0183(13) 0.0051(11) -0.0031(11) O6 0.0355(14) 0.0559(18) 0.0705(19) -0.0349(16) 0.0029(13) 0.0058(13) O7 0.0656(18) 0.071(2) 0.0348(16) 0.0101(15) 0.0064(14) 0.0206(16) O8 0.0406(13) 0.0362(16) 0.0373(14) -0.0068(11) 0.0038(11) 0.0067(11) C1 0.0323(19) 0.044(2) 0.047(2) -0.0064(19) 0.0097(17) 0.0006(17) C2 0.033(2) 0.051(3) 0.047(2) -0.012(2) 0.0017(17) -0.0072(18) C3 0.049(2) 0.040(2) 0.035(2) -0.0112(18) 0.0051(17) -0.0026(18) C4 0.042(2) 0.0253(19) 0.031(2) -0.0040(16) 0.0101(16) 0.0017(15) C5 0.036(2) 0.034(2) 0.043(2) -0.0086(18) 0.0122(17) -0.0016(16) C6 0.052(2) 0.043(3) 0.040(2) -0.007(2) 0.0162(18) 0.004(2) C7 0.049(2) 0.054(3) 0.043(2) -0.009(2) 0.0168(18) 0.0055(19) C8 0.049(2) 0.056(3) 0.044(2) -0.009(2) 0.0148(18) 0.014(2) C9 0.050(2) 0.055(3) 0.038(2) -0.007(2) 0.0086(17) 0.011(2) C10 0.049(2) 0.051(3) 0.047(2) -0.005(2) 0.0175(19) 0.0107(19) C11 0.046(2) 0.052(3) 0.048(2) -0.011(2) 0.0150(18) 0.0048(19) C12 0.048(2) 0.047(3) 0.046(2) -0.003(2) 0.0167(18) 0.0115(19) C13 0.038(2) 0.057(3) 0.052(3) -0.009(2) 0.0124(18) 0.0032(19) C14 0.043(2) 0.053(3) 0.058(3) -0.003(2) 0.0218(18) 0.005(2) C15 0.043(2) 0.052(3) 0.058(2) -0.008(2) 0.0229(18) 0.003(2) C16 0.046(2) 0.051(3) 0.057(3) -0.002(2) 0.0283(19) 0.0003(19) C17 0.039(2) 0.045(3) 0.036(2) 0.0017(18) 0.0134(16) 0.0030(17) C18 0.0357(19) 0.036(2) 0.040(2) -0.0013(17) 0.0141(16) 0.0014(16) C19 0.058(2) 0.033(2) 0.048(2) 0.0112(18) 0.0204(19) 0.0029(18) C20 0.063(2) 0.029(2) 0.055(3) 0.0019(19) 0.023(2) 0.0100(18) C21 0.043(2) 0.038(2) 0.040(2) 0.0008(18) 0.0156(17) 0.0090(17) C22 0.039(2) 0.028(2) 0.043(2) -0.0012(17) 0.0130(17) 0.0028(16) C23 0.0268(17) 0.0264(19) 0.0294(19) -0.0057(15) 0.0026(14) 0.0010(14) C24 0.0256(16) 0.0286(19) 0.0332(18) 0.0061(17) 0.0030(13) -0.0035(15) C25 0.0353(19) 0.041(2) 0.041(2) -0.007(2) 0.0007(16) -0.0011(19) C26 0.0315(19) 0.051(3) 0.053(2) -0.002(2) -0.0032(17) -0.0140(18) C27 0.0236(18) 0.062(3) 0.050(2) 0.005(2) 0.0036(16) -0.0015(18) C28 0.0267(18) 0.047(2) 0.043(2) -0.0040(19) 0.0101(16) -0.0006(17) C29 0.0242(17) 0.0273(19) 0.035(2) 0.0031(16) 0.0052(14) -0.0003(14) C30 0.0277(18) 0.0282(19) 0.0320(19) 0.0002(16) 0.0095(15) -0.0008(15) C31 0.064(3) 0.063(3) 0.069(3) -0.017(3) 0.022(2) 0.005(3) C32 0.072(3) 0.065(3) 0.049(3) -0.012(2) 0.017(2) 0.007(2) C33 0.059(2) 0.052(3) 0.032(2) 0.003(2) 0.0017(18) 0.004(2) C34 0.040(2) 0.034(2) 0.039(2) 0.0027(17) 0.0104(17) -0.0045(16) C35 0.048(2) 0.057(3) 0.043(2) -0.002(2) 0.0069(18) 0.000(2) C36 0.047(2) 0.043(2) 0.037(2) 0.0013(19) 0.0097(18) -0.0018(18) C37 0.049(2) 0.059(3) 0.043(2) -0.002(2) 0.0087(19) 0.010(2) C38 0.053(2) 0.044(2) 0.041(2) -0.0022(19) 0.0129(18) -0.0024(19) C39 0.054(2) 0.052(3) 0.046(2) 0.003(2) 0.0119(19) 0.009(2) C40 0.057(2) 0.050(3) 0.043(2) 0.0020(19) 0.0158(19) 0.012(2) C41 0.053(2) 0.060(3) 0.052(3) 0.004(2) 0.015(2) 0.014(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 Cd N4 2.300(3) 3_725 ? Cd O3 2.336(2) . ? Cd N1 2.336(3) . ? Cd O5 2.352(2) 2_545 ? Cd O8 2.383(2) . ? Cd O6 2.455(2) 2_545 ? Cd O4 2.523(2) . ? Cd C30 2.752(3) 2_545 ? N1 C5 1.336(4) . ? N1 C1 1.342(4) . ? N2 C6 1.365(4) . ? N2 C4 1.407(4) . ? N2 H2A 0.8600 . ? N3 C17 1.363(4) . ? N3 C18 1.401(4) . ? N3 H3A 0.8600 . ? N4 C21 1.330(4) . ? N4 C22 1.347(4) . ? N4 Cd 2.300(3) 3_725 ? N5 C31 1.338(5) . ? N5 C35 1.339(5) . ? N6 C36 1.371(4) . ? N6 C34 1.402(4) . ? N6 H6A 0.8600 . ? O1 C6 1.197(4) . ? O2 C17 1.212(4) . ? O3 C23 1.251(4) . ? O4 C23 1.250(4) . ? O5 C30 1.248(3) . ? O5 Cd 2.352(2) 2 ? O6 C30 1.248(4) . ? O6 Cd 2.455(2) 2 ? O7 C36 1.200(4) . ? C1 C2 1.364(5) . ? C1 H1A 0.9300 . ? C2 C3 1.382(4) . ? C2 H2B 0.9300 . ? C3 C4 1.378(5) . ? C3 H3B 0.9300 . ? C4 C5 1.385(4) . ? C5 H5B 0.9300 . ? C6 C7 1.513(5) . ? C7 C8 1.517(5) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.525(5) . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C9 C10 1.509(5) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.524(4) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.525(5) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.519(4) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.513(5) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.524(4) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.508(5) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.513(4) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C18 C19 1.381(5) . ? C18 C22 1.385(5) . ? C19 C20 1.387(5) . ? C19 H19A 0.9300 . ? C20 C21 1.378(5) . ? C20 H20A 0.9300 . ? C21 H21A 0.9300 . ? C22 H22A 0.9300 . ? C23 C24 1.507(4) . ? C24 C25 1.389(4) . ? C24 C29 1.396(4) . ? C25 C26 1.378(5) . ? C25 H25A 0.9300 . ? C26 C27 1.382(5) . ? C26 H26A 0.9300 . ? C27 C28 1.369(5) . ? C27 H27A 0.9300 . ? C28 C29 1.387(4) . ? C28 H28A 0.9300 . ? C29 C30 1.499(4) . ? C30 Cd 2.752(3) 2 ? C31 C32 1.370(6) . ? C31 H31A 0.9300 . ? C32 C33 1.363(5) . ? C32 H32A 0.9300 . ? C33 C34 1.381(5) . ? C33 H33A 0.9300 . ? C34 C35 1.382(5) . ? C35 H35A 0.9300 . ? C36 C37 1.506(5) . ? C37 C38 1.506(5) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 C39 1.503(5) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 C40 1.512(5) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 C41 1.513(5) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 C41 1.509(7) 3_615 ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? 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 N4 Cd O3 135.04(9) 3_725 . ? N4 Cd N1 96.20(9) 3_725 . ? O3 Cd N1 96.04(9) . . ? N4 Cd O5 138.01(8) 3_725 2_545 ? O3 Cd O5 84.92(8) . 2_545 ? N1 Cd O5 90.27(9) . 2_545 ? N4 Cd O8 86.54(9) 3_725 . ? O3 Cd O8 78.88(8) . . ? N1 Cd O8 174.72(8) . . ? O5 Cd O8 90.69(8) 2_545 . ? N4 Cd O6 84.69(9) 3_725 2_545 ? O3 Cd O6 138.07(8) . 2_545 ? N1 Cd O6 90.94(9) . 2_545 ? O5 Cd O6 53.67(7) 2_545 2_545 ? O8 Cd O6 93.81(9) . 2_545 ? N4 Cd O4 83.80(8) 3_725 . ? O3 Cd O4 53.40(7) . . ? N1 Cd O4 88.92(9) . . ? O5 Cd O4 137.93(7) 2_545 . ? O8 Cd O4 86.89(8) . . ? O6 Cd O4 168.40(8) 2_545 . ? N4 Cd C30 111.17(9) 3_725 2_545 ? O3 Cd C30 111.19(9) . 2_545 ? N1 Cd C30 92.91(10) . 2_545 ? O5 Cd C30 26.88(8) 2_545 2_545 ? O8 Cd C30 90.29(9) . 2_545 ? O6 Cd C30 26.97(8) 2_545 2_545 ? O4 Cd C30 164.59(8) . 2_545 ? C5 N1 C1 116.9(3) . . ? C5 N1 Cd 121.5(2) . . ? C1 N1 Cd 121.5(2) . . ? C6 N2 C4 126.0(3) . . ? C6 N2 H2A 117.0 . . ? C4 N2 H2A 117.0 . . ? C17 N3 C18 127.1(3) . . ? C17 N3 H3A 116.5 . . ? C18 N3 H3A 116.5 . . ? C21 N4 C22 118.4(3) . . ? C21 N4 Cd 123.8(2) . 3_725 ? C22 N4 Cd 117.7(2) . 3_725 ? C31 N5 C35 117.3(4) . . ? C36 N6 C34 127.6(3) . . ? C36 N6 H6A 116.2 . . ? C34 N6 H6A 116.2 . . ? C23 O3 Cd 96.21(19) . . ? C23 O4 Cd 87.50(19) . . ? C30 O5 Cd 94.7(2) . 2 ? C30 O6 Cd 89.88(19) . 2 ? N1 C1 C2 122.7(3) . . ? N1 C1 H1A 118.7 . . ? C2 C1 H1A 118.7 . . ? C1 C2 C3 120.0(3) . . ? C1 C2 H2B 120.0 . . ? C3 C2 H2B 120.0 . . ? C4 C3 C2 118.5(3) . . ? C4 C3 H3B 120.8 . . ? C2 C3 H3B 120.8 . . ? C3 C4 C5 117.8(3) . . ? C3 C4 N2 125.0(3) . . ? C5 C4 N2 117.2(3) . . ? N1 C5 C4 124.2(3) . . ? N1 C5 H5B 117.9 . . ? C4 C5 H5B 117.9 . . ? O1 C6 N2 122.3(3) . . ? O1 C6 C7 123.7(3) . . ? N2 C6 C7 114.0(3) . . ? C6 C7 C8 112.4(3) . . ? C6 C7 H7A 109.1 . . ? C8 C7 H7A 109.1 . . ? C6 C7 H7B 109.1 . . ? C8 C7 H7B 109.1 . . ? H7A C7 H7B 107.9 . . ? C7 C8 C9 112.6(3) . . ? C7 C8 H8B 109.1 . . ? C9 C8 H8B 109.1 . . ? C7 C8 H8C 109.1 . . ? C9 C8 H8C 109.1 . . ? H8B C8 H8C 107.8 . . ? C10 C9 C8 113.4(3) . . ? C10 C9 H9A 108.9 . . ? C8 C9 H9A 108.9 . . ? C10 C9 H9B 108.9 . . ? C8 C9 H9B 108.9 . . ? H9A C9 H9B 107.7 . . ? C9 C10 C11 113.2(3) . . ? C9 C10 H10A 108.9 . . ? C11 C10 H10A 108.9 . . ? C9 C10 H10B 108.9 . . ? C11 C10 H10B 108.9 . . ? H10A C10 H10B 107.8 . . ? C10 C11 C12 112.9(3) . . ? C10 C11 H11A 109.0 . . ? C12 C11 H11A 109.0 . . ? C10 C11 H11B 109.0 . . ? C12 C11 H11B 109.0 . . ? H11A C11 H11B 107.8 . . ? C13 C12 C11 113.7(3) . . ? C13 C12 H12A 108.8 . . ? C11 C12 H12A 108.8 . . ? C13 C12 H12B 108.8 . . ? C11 C12 H12B 108.8 . . ? H12A C12 H12B 107.7 . . ? C14 C13 C12 113.2(3) . . ? C14 C13 H13A 108.9 . . ? C12 C13 H13A 108.9 . . ? C14 C13 H13B 108.9 . . ? C12 C13 H13B 108.9 . . ? H13A C13 H13B 107.8 . . ? C13 C14 C15 113.9(3) . . ? C13 C14 H14A 108.8 . . ? C15 C14 H14A 108.8 . . ? C13 C14 H14B 108.8 . . ? C15 C14 H14B 108.8 . . ? H14A C14 H14B 107.7 . . ? C16 C15 C14 112.1(3) . . ? C16 C15 H15A 109.2 . . ? C14 C15 H15A 109.2 . . ? C16 C15 H15B 109.2 . . ? C14 C15 H15B 109.2 . . ? H15A C15 H15B 107.9 . . ? C15 C16 C17 114.3(3) . . ? C15 C16 H16A 108.7 . . ? C17 C16 H16A 108.7 . . ? C15 C16 H16B 108.7 . . ? C17 C16 H16B 108.7 . . ? H16A C16 H16B 107.6 . . ? O2 C17 N3 123.4(3) . . ? O2 C17 C16 123.3(3) . . ? N3 C17 C16 113.3(3) . . ? C19 C18 C22 117.9(3) . . ? C19 C18 N3 120.0(3) . . ? C22 C18 N3 122.0(3) . . ? C18 C19 C20 119.1(3) . . ? C18 C19 H19A 120.5 . . ? C20 C19 H19A 120.5 . . ? C21 C20 C19 119.4(3) . . ? C21 C20 H20A 120.3 . . ? C19 C20 H20A 120.3 . . ? N4 C21 C20 122.1(3) . . ? N4 C21 H21A 119.0 . . ? C20 C21 H21A 119.0 . . ? N4 C22 C18 123.1(3) . . ? N4 C22 H22A 118.5 . . ? C18 C22 H22A 118.5 . . ? O4 C23 O3 122.3(3) . . ? O4 C23 C24 119.9(3) . . ? O3 C23 C24 117.8(3) . . ? C25 C24 C29 119.4(3) . . ? C25 C24 C23 116.9(3) . . ? C29 C24 C23 123.8(3) . . ? C26 C25 C24 120.7(3) . . ? C26 C25 H25A 119.6 . . ? C24 C25 H25A 119.6 . . ? C25 C26 C27 119.7(3) . . ? C25 C26 H26A 120.1 . . ? C27 C26 H26A 120.1 . . ? C28 C27 C26 120.1(3) . . ? C28 C27 H27A 120.0 . . ? C26 C27 H27A 120.0 . . ? C27 C28 C29 121.1(3) . . ? C27 C28 H28A 119.4 . . ? C29 C28 H28A 119.4 . . ? C28 C29 C24 119.0(3) . . ? C28 C29 C30 118.6(3) . . ? C24 C29 C30 122.3(3) . . ? O6 C30 O5 121.0(3) . . ? O6 C30 C29 119.7(3) . . ? O5 C30 C29 119.3(3) . . ? O6 C30 Cd 63.15(18) . 2 ? O5 C30 Cd 58.43(17) . 2 ? C29 C30 Cd 170.2(2) . 2 ? N5 C31 C32 122.8(4) . . ? N5 C31 H31A 118.6 . . ? C32 C31 H31A 118.6 . . ? C33 C32 C31 119.0(4) . . ? C33 C32 H32A 120.5 . . ? C31 C32 H32A 120.5 . . ? C32 C33 C34 120.0(4) . . ? C32 C33 H33A 120.0 . . ? C34 C33 H33A 120.0 . . ? C33 C34 C35 117.2(3) . . ? C33 C34 N6 119.0(3) . . ? C35 C34 N6 123.7(3) . . ? N5 C35 C34 123.5(4) . . ? N5 C35 H35A 118.2 . . ? C34 C35 H35A 118.2 . . ? O7 C36 N6 121.8(3) . . ? O7 C36 C37 124.1(3) . . ? N6 C36 C37 114.1(3) . . ? C38 C37 C36 113.4(3) . . ? C38 C37 H37A 108.9 . . ? C36 C37 H37A 108.9 . . ? C38 C37 H37B 108.9 . . ? C36 C37 H37B 108.9 . . ? H37A C37 H37B 107.7 . . ? C39 C38 C37 114.4(3) . . ? C39 C38 H38A 108.7 . . ? C37 C38 H38A 108.7 . . ? C39 C38 H38B 108.7 . . ? C37 C38 H38B 108.7 . . ? H38A C38 H38B 107.6 . . ? C38 C39 C40 113.3(3) . . ? C38 C39 H39A 108.9 . . ? C40 C39 H39A 108.9 . . ? C38 C39 H39B 108.9 . . ? C40 C39 H39B 108.9 . . ? H39A C39 H39B 107.7 . . ? C39 C40 C41 115.6(3) . . ? C39 C40 H40A 108.4 . . ? C41 C40 H40A 108.4 . . ? C39 C40 H40B 108.4 . . ? C41 C40 H40B 108.4 . . ? H40A C40 H40B 107.4 . . ? C41 C41 C40 114.6(4) 3_615 . ? C41 C41 H41A 108.6 3_615 . ? C40 C41 H41A 108.6 . . ? C41 C41 H41B 108.6 3_615 . ? C40 C41 H41B 108.6 . . ? H41A C41 H41B 107.6 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.693 _refine_diff_density_min -0.812 _refine_diff_density_rms 0.088 _database_code_depnum_ccdc_archive 'CCDC 917803' ####################################################################### # # 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 #TrackingRef 'all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H53 Cd N6 O11' _chemical_formula_weight 930.30 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 9.7935(4) _cell_length_b 12.1729(6) _cell_length_c 18.9627(9) _cell_angle_alpha 78.802(3) _cell_angle_beta 89.871(3) _cell_angle_gamma 70.511(3) _cell_volume 2085.76(17) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9817 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 28.26 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.481 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 966 _exptl_absorpt_coefficient_mu 0.592 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6346 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_process_details 'SADABS V2008/1 (Bruker AXS, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 34440 _diffrn_reflns_av_R_equivalents 0.0547 _diffrn_reflns_av_sigmaI/netI 0.0618 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 28.34 _reflns_number_total 10282 _reflns_number_gt 8181 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2010)' _computing_cell_refinement 'SAINT V7.68A (Bruker AXS, 2010)' _computing_data_reduction 'SAINT V7.68A (Bruker AXS, 2010)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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^)+(0.0346P)^2^+0.4081P] 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 10282 _refine_ls_number_parameters 561 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0599 _refine_ls_R_factor_gt 0.0404 _refine_ls_wR_factor_ref 0.0857 _refine_ls_wR_factor_gt 0.0783 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _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 Cd Cd 0.81414(2) 0.617738(16) -0.490736(9) 0.01629(6) Uani 1 1 d . . . O1 O 0.3082(2) 0.77615(18) -0.38861(12) 0.0364(5) Uani 1 1 d . . . O2 O -1.0383(2) 0.95411(17) -0.07278(10) 0.0299(4) Uani 1 1 d . . . O3 O 0.7153(2) 0.36542(17) -0.11381(9) 0.0281(4) Uani 1 1 d . . . O4 O 0.9108(2) 0.73490(17) -0.57461(9) 0.0262(4) Uani 1 1 d . . . O5 O 1.07045(19) 0.59161(15) -0.49660(9) 0.0189(4) Uani 1 1 d . . . O6 O 1.3267(2) 0.86901(17) -0.81019(9) 0.0287(4) Uani 1 1 d . . . O7 O 1.0900(2) 0.89955(17) -0.79936(9) 0.0223(4) Uani 1 1 d . . . O8 O 1.66996(19) 0.63266(17) -0.59544(9) 0.0251(4) Uani 1 1 d . . . O9 O 1.57597(19) 0.61142(15) -0.48961(8) 0.0191(4) Uani 1 1 d . . . N1 N 0.6949(2) 0.80478(19) -0.45492(11) 0.0204(4) Uani 1 1 d . . . N2 N 0.3607(2) 0.93430(19) -0.36509(11) 0.0206(4) Uani 1 1 d . . . H2A H 0.3302 0.9936 -0.3439 0.025 Uiso 1 1 calc R . . N3 N -0.9711(2) 0.81137(19) 0.02816(11) 0.0231(5) Uani 1 1 d . . . H3A H -0.8999 0.7565 0.0543 0.028 Uiso 1 1 calc R . . N4 N -1.2583(3) 0.8364(2) 0.15492(12) 0.0304(5) Uani 1 1 d . . . N5 N 0.8557(2) 0.53649(18) -0.36859(10) 0.0174(4) Uani 1 1 d . . . N6 N 0.6285(2) 0.46492(18) -0.22816(10) 0.0183(4) Uani 1 1 d . . . H6A H 0.5503 0.4959 -0.2560 0.022 Uiso 1 1 calc R . . C1 C 0.7495(3) 0.8934(2) -0.46188(13) 0.0213(5) Uani 1 1 d . . . H1A H 0.8361 0.8854 -0.4841 0.026 Uiso 1 1 calc R . . C2 C 0.6808(3) 0.9968(2) -0.43691(14) 0.0248(6) Uani 1 1 d . . . H2B H 0.7211 1.0568 -0.4422 0.030 Uiso 1 1 calc R . . C3 C 0.5526(3) 1.0096(2) -0.40427(13) 0.0223(5) Uani 1 1 d . . . H3B H 0.5057 1.0782 -0.3870 0.027 Uiso 1 1 calc R . . C4 C 0.4935(3) 0.9188(2) -0.39727(12) 0.0189(5) Uani 1 1 d . . . C5 C 0.5692(3) 0.8173(2) -0.42310(13) 0.0204(5) Uani 1 1 d . . . H5A H 0.5314 0.7557 -0.4182 0.025 Uiso 1 1 calc R . . C6 C 0.2748(3) 0.8659(2) -0.36370(13) 0.0228(5) Uani 1 1 d . . . C7 C 0.1310(3) 0.9133(2) -0.33095(14) 0.0252(6) Uani 1 1 d . . . H7A H 0.0671 0.9809 -0.3651 0.030 Uiso 1 1 calc R . . H7B H 0.1473 0.9413 -0.2883 0.030 Uiso 1 1 calc R . . C8 C 0.0561(3) 0.8215(2) -0.31042(14) 0.0253(6) Uani 1 1 d . . . H8A H 0.1214 0.7518 -0.2782 0.030 Uiso 1 1 calc R . . H8B H 0.0334 0.7970 -0.3534 0.030 Uiso 1 1 calc R . . C9 C -0.0835(3) 0.8718(2) -0.27362(14) 0.0235(6) Uani 1 1 d . . . H9A H -0.0588 0.8921 -0.2295 0.028 Uiso 1 1 calc R . . H9B H -0.1445 0.9448 -0.3049 0.028 Uiso 1 1 calc R . . C10 C -0.1707(3) 0.7885(2) -0.25535(14) 0.0245(6) Uani 1 1 d . . . H10A H -0.1101 0.7148 -0.2246 0.029 Uiso 1 1 calc R . . H10B H -0.1984 0.7695 -0.2994 0.029 Uiso 1 1 calc R . . C11 C -0.3072(3) 0.8427(2) -0.21732(14) 0.0244(6) Uani 1 1 d . . . H11A H -0.2786 0.8577 -0.1722 0.029 Uiso 1 1 calc R . . H11B H -0.3646 0.9187 -0.2470 0.029 Uiso 1 1 calc R . . C12 C -0.4010(3) 0.7650(2) -0.20193(14) 0.0236(6) Uani 1 1 d . . . H12A H -0.3440 0.6895 -0.1716 0.028 Uiso 1 1 calc R . . H12B H -0.4281 0.7489 -0.2470 0.028 Uiso 1 1 calc R . . C13 C -0.5381(3) 0.8194(2) -0.16519(14) 0.0252(6) Uani 1 1 d . . . H13A H -0.5970 0.8938 -0.1960 0.030 Uiso 1 1 calc R . . H13B H -0.5117 0.8371 -0.1205 0.030 Uiso 1 1 calc R . . C14 C -0.6273(3) 0.7372(3) -0.14900(16) 0.0310(6) Uani 1 1 d . . . H14A H -0.6353 0.7066 -0.1918 0.037 Uiso 1 1 calc R . . H14B H -0.5745 0.6699 -0.1113 0.037 Uiso 1 1 calc R . . C15 C -0.7790(3) 0.7929(3) -0.12571(16) 0.0330(7) Uani 1 1 d . . . H15A H -0.8292 0.7357 -0.1226 0.040 Uiso 1 1 calc R . . H15B H -0.8313 0.8613 -0.1628 0.040 Uiso 1 1 calc R . . C16 C -0.7861(3) 0.8330(3) -0.05360(14) 0.0266(6) Uani 1 1 d . . . H16A H -0.7271 0.7677 -0.0164 0.032 Uiso 1 1 calc R . . H16B H -0.7486 0.8982 -0.0576 0.032 Uiso 1 1 calc R . . C17 C -0.9416(3) 0.8728(2) -0.03385(13) 0.0240(6) Uani 1 1 d . . . C18 C -1.1127(3) 0.8322(2) 0.05266(13) 0.0220(5) Uani 1 1 d . . . C19 C -1.2352(3) 0.8617(2) 0.00659(14) 0.0279(6) Uani 1 1 d . . . H19A H -1.2284 0.8708 -0.0430 0.033 Uiso 1 1 calc R . . C20 C -1.3671(3) 0.8770(3) 0.03622(16) 0.0329(7) Uani 1 1 d . . . H20A H -1.4505 0.8945 0.0067 0.039 Uiso 1 1 calc R . . C21 C -1.3751(3) 0.8661(3) 0.10996(17) 0.0333(7) Uani 1 1 d . . . H21A H -1.4656 0.8801 0.1289 0.040 Uiso 1 1 calc R . . C22 C -1.1300(3) 0.8197(2) 0.12612(14) 0.0252(6) Uani 1 1 d . . . H22A H -1.0477 0.7984 0.1571 0.030 Uiso 1 1 calc R . . C23 C 0.9842(3) 0.5082(2) -0.33284(13) 0.0205(5) Uani 1 1 d . . . H23A H 1.0628 0.5172 -0.3580 0.025 Uiso 1 1 calc R . . C24 C 1.0025(3) 0.4657(2) -0.25876(13) 0.0243(6) Uani 1 1 d . . . H24A H 1.0926 0.4469 -0.2347 0.029 Uiso 1 1 calc R . . C25 C 0.8868(3) 0.4513(2) -0.22067(13) 0.0233(6) Uani 1 1 d . . . H25A H 0.8975 0.4247 -0.1709 0.028 Uiso 1 1 calc R . . C26 C 0.7541(3) 0.4775(2) -0.25821(12) 0.0174(5) Uani 1 1 d . . . C27 C 0.7441(3) 0.5212(2) -0.33245(12) 0.0171(5) Uani 1 1 d . . . H27A H 0.6554 0.5405 -0.3580 0.020 Uiso 1 1 calc R . . C28 C 0.6142(3) 0.4099(2) -0.16039(13) 0.0206(5) Uani 1 1 d . . . C29 C 0.4628(3) 0.4078(2) -0.14820(13) 0.0238(6) Uani 1 1 d . . . H29A H 0.4545 0.3376 -0.1621 0.029 Uiso 1 1 calc R . . H29B H 0.3943 0.4770 -0.1795 0.029 Uiso 1 1 calc R . . C30 C 0.4207(3) 0.4074(3) -0.07098(13) 0.0249(6) Uani 1 1 d . . . H30A H 0.4490 0.4665 -0.0530 0.030 Uiso 1 1 calc R . . H30B H 0.4728 0.3300 -0.0411 0.030 Uiso 1 1 calc R . . C31 C 0.2578(3) 0.4341(3) -0.06537(14) 0.0265(6) Uani 1 1 d . . . H31A H 0.2061 0.5116 -0.0951 0.032 Uiso 1 1 calc R . . H31B H 0.2297 0.3754 -0.0840 0.032 Uiso 1 1 calc R . . C32 C 0.2129(3) 0.4330(3) 0.01177(15) 0.0328(7) Uani 1 1 d . . . H32A H 0.2305 0.4982 0.0281 0.039 Uiso 1 1 calc R . . H32B H 0.2741 0.3594 0.0424 0.039 Uiso 1 1 calc R . . C33 C 0.0536(3) 0.4442(3) 0.02118(16) 0.0354(7) Uani 1 1 d . . . H33A H 0.0374 0.3767 0.0072 0.053 Uiso 1 1 calc R . . H33B H 0.0360 0.4399 0.0718 0.053 Uiso 1 1 calc R . . C34 C 1.0392(3) 0.6776(2) -0.55113(12) 0.0170(5) Uani 1 1 d . . . C35 C 1.1598(3) 0.7071(2) -0.58925(12) 0.0155(5) Uani 1 1 d . . . C36 C 1.2984(3) 0.6660(2) -0.55590(12) 0.0156(5) Uani 1 1 d . . . H36A H 1.3144 0.6267 -0.5079 0.019 Uiso 1 1 calc R . . C37 C 1.4134(3) 0.6832(2) -0.59388(12) 0.0154(5) Uani 1 1 d . . . C38 C 1.3895(3) 0.7436(2) -0.66550(12) 0.0160(5) Uani 1 1 d . . . H38A H 1.4670 0.7533 -0.6913 0.019 Uiso 1 1 calc R . . C39 C 1.2499(3) 0.7893(2) -0.69835(12) 0.0154(5) Uani 1 1 d . . . C40 C 1.1349(3) 0.7710(2) -0.66015(12) 0.0154(5) Uani 1 1 d . . . H40A H 1.0414 0.8015 -0.6821 0.019 Uiso 1 1 calc R . . C41 C 1.2285(3) 0.8561(2) -0.77472(12) 0.0185(5) Uani 1 1 d . . . C42 C 1.5625(3) 0.6388(2) -0.55711(13) 0.0182(5) Uani 1 1 d . . . O10 O 0.3628(2) 0.5369(2) -0.31909(11) 0.0317(5) Uani 1 1 d . . . O11 O 0.2847(3) 1.1341(2) -0.30037(13) 0.0378(6) Uani 1 1 d . . . H7D H 1.083(4) 0.945(3) -0.841(2) 0.054(11) Uiso 1 1 d . . . H10C H 0.347(4) 0.495(3) -0.3467(17) 0.034(9) Uiso 1 1 d . . . H10D H 0.342(4) 0.601(3) -0.3464(19) 0.049(12) Uiso 1 1 d . . . H11C H 0.250(4) 1.187(3) -0.3276(18) 0.031(10) Uiso 1 1 d . . . H11D H 0.269(5) 1.143(4) -0.260(3) 0.080(15) 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 Cd 0.00988(9) 0.02308(10) 0.01498(8) -0.00089(6) 0.00247(6) -0.00611(7) O1 0.0312(12) 0.0331(12) 0.0567(13) -0.0242(10) 0.0240(10) -0.0182(10) O2 0.0223(11) 0.0335(11) 0.0242(9) 0.0073(8) 0.0009(8) -0.0043(9) O3 0.0229(10) 0.0374(11) 0.0199(8) 0.0052(8) -0.0011(8) -0.0109(9) O4 0.0120(9) 0.0359(11) 0.0256(9) 0.0026(8) 0.0039(7) -0.0064(9) O5 0.0165(9) 0.0214(9) 0.0202(8) -0.0014(7) 0.0050(7) -0.0097(8) O6 0.0182(10) 0.0387(11) 0.0244(9) 0.0036(8) 0.0061(8) -0.0091(9) O7 0.0161(10) 0.0282(10) 0.0191(8) 0.0041(7) -0.0013(7) -0.0080(9) O8 0.0101(9) 0.0414(11) 0.0223(9) -0.0018(8) 0.0011(7) -0.0093(9) O9 0.0154(9) 0.0224(9) 0.0188(8) -0.0034(7) -0.0007(7) -0.0062(8) N1 0.0164(11) 0.0231(11) 0.0197(10) 0.0005(8) 0.0016(9) -0.0067(10) N2 0.0178(11) 0.0213(11) 0.0240(10) -0.0083(8) 0.0060(9) -0.0065(10) N3 0.0167(11) 0.0260(12) 0.0206(10) 0.0020(8) 0.0035(9) -0.0031(10) N4 0.0326(14) 0.0321(13) 0.0302(12) -0.0099(10) 0.0125(11) -0.0140(12) N5 0.0170(11) 0.0194(11) 0.0159(9) -0.0018(8) 0.0024(8) -0.0073(9) N6 0.0136(11) 0.0228(11) 0.0168(9) -0.0016(8) 0.0015(8) -0.0052(9) C1 0.0164(13) 0.0249(14) 0.0213(11) -0.0014(10) 0.0015(10) -0.0074(12) C2 0.0236(15) 0.0266(14) 0.0277(13) -0.0039(11) 0.0012(11) -0.0139(13) C3 0.0246(15) 0.0216(13) 0.0206(11) -0.0048(10) 0.0015(11) -0.0076(12) C4 0.0164(13) 0.0242(13) 0.0160(10) -0.0024(9) 0.0013(10) -0.0076(11) C5 0.0194(13) 0.0226(13) 0.0205(11) -0.0025(10) 0.0043(10) -0.0096(12) C6 0.0199(14) 0.0253(14) 0.0243(12) -0.0045(10) 0.0055(11) -0.0093(12) C7 0.0207(14) 0.0258(14) 0.0304(13) -0.0079(11) 0.0096(11) -0.0084(12) C8 0.0170(14) 0.0289(15) 0.0306(13) -0.0072(11) 0.0071(11) -0.0083(12) C9 0.0181(14) 0.0273(14) 0.0266(12) -0.0082(11) 0.0048(11) -0.0082(12) C10 0.0200(14) 0.0268(14) 0.0268(13) -0.0067(11) 0.0044(11) -0.0076(12) C11 0.0229(14) 0.0283(14) 0.0244(12) -0.0080(11) 0.0051(11) -0.0105(13) C12 0.0187(14) 0.0276(14) 0.0229(12) -0.0028(10) 0.0051(11) -0.0072(12) C13 0.0215(14) 0.0289(15) 0.0257(12) -0.0056(11) 0.0065(11) -0.0091(13) C14 0.0264(16) 0.0334(16) 0.0367(15) -0.0109(12) 0.0133(13) -0.0127(14) C15 0.0259(16) 0.0439(18) 0.0358(15) -0.0133(13) 0.0117(13) -0.0176(15) C16 0.0172(14) 0.0333(15) 0.0255(13) -0.0001(11) 0.0039(11) -0.0071(13) C17 0.0228(15) 0.0264(14) 0.0214(12) -0.0027(10) 0.0050(11) -0.0080(13) C18 0.0195(14) 0.0226(13) 0.0239(12) -0.0041(10) 0.0040(11) -0.0076(12) C19 0.0250(16) 0.0335(16) 0.0228(12) -0.0010(11) 0.0008(11) -0.0095(14) C20 0.0199(15) 0.0360(17) 0.0388(16) -0.0009(13) -0.0023(13) -0.0081(14) C21 0.0222(16) 0.0298(16) 0.0469(17) -0.0087(13) 0.0123(14) -0.0072(14) C22 0.0272(15) 0.0271(14) 0.0234(12) -0.0044(10) 0.0033(11) -0.0126(13) C23 0.0162(13) 0.0241(13) 0.0218(11) -0.0034(10) 0.0050(10) -0.0083(12) C24 0.0177(14) 0.0314(15) 0.0220(12) -0.0007(11) -0.0029(11) -0.0086(12) C25 0.0231(14) 0.0285(14) 0.0169(11) 0.0001(10) 0.0009(10) -0.0098(12) C26 0.0156(13) 0.0174(12) 0.0194(11) -0.0040(9) 0.0035(10) -0.0058(11) C27 0.0132(12) 0.0176(12) 0.0204(11) -0.0037(9) 0.0003(10) -0.0053(11) C28 0.0230(14) 0.0219(13) 0.0188(11) -0.0055(10) 0.0061(11) -0.0093(12) C29 0.0225(14) 0.0301(15) 0.0204(12) -0.0033(10) 0.0046(11) -0.0119(13) C30 0.0235(15) 0.0311(15) 0.0216(12) -0.0035(11) 0.0047(11) -0.0121(13) C31 0.0231(15) 0.0320(15) 0.0253(13) -0.0055(11) 0.0069(11) -0.0106(13) C32 0.0291(17) 0.0440(18) 0.0264(13) -0.0074(12) 0.0070(12) -0.0136(15) C33 0.0331(17) 0.0439(18) 0.0333(15) -0.0106(13) 0.0144(13) -0.0169(15) C34 0.0168(13) 0.0217(13) 0.0160(10) -0.0063(9) 0.0059(10) -0.0100(11) C35 0.0118(12) 0.0170(12) 0.0196(11) -0.0046(9) 0.0031(9) -0.0071(10) C36 0.0147(12) 0.0150(12) 0.0168(10) -0.0015(9) 0.0011(9) -0.0055(10) C37 0.0120(12) 0.0153(12) 0.0196(11) -0.0045(9) 0.0008(9) -0.0050(10) C38 0.0124(12) 0.0177(12) 0.0208(11) -0.0054(9) 0.0055(10) -0.0081(10) C39 0.0132(12) 0.0143(11) 0.0188(11) -0.0030(9) 0.0026(9) -0.0051(10) C40 0.0126(12) 0.0142(11) 0.0195(11) -0.0033(9) 0.0013(9) -0.0046(10) C41 0.0154(13) 0.0208(13) 0.0193(11) -0.0026(9) 0.0020(10) -0.0068(11) C42 0.0142(12) 0.0169(12) 0.0243(12) -0.0034(9) 0.0011(10) -0.0067(11) O10 0.0288(12) 0.0339(12) 0.0298(10) -0.0085(10) -0.0040(9) -0.0060(11) O11 0.0543(17) 0.0266(12) 0.0212(10) -0.0033(9) 0.0025(11) 0.0003(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 Cd N5 2.3140(19) . ? Cd O4 2.3393(18) . ? Cd O9 2.3592(17) 1_455 ? Cd O8 2.3813(17) 1_455 ? Cd N1 2.415(2) . ? Cd O5 2.4278(17) . ? Cd O5 2.4786(17) 2_764 ? Cd C42 2.681(2) 1_455 ? Cd C34 2.728(2) . ? O1 C6 1.218(3) . ? O2 C17 1.231(3) . ? O3 C28 1.230(3) . ? O4 C34 1.250(3) . ? O5 C34 1.275(3) . ? O5 Cd 2.4786(17) 2_764 ? O6 C41 1.208(3) . ? O7 C41 1.329(3) . ? O7 H7D 0.86(4) . ? O8 C42 1.267(3) . ? O8 Cd 2.3813(17) 1_655 ? O9 C42 1.254(3) . ? O9 Cd 2.3592(17) 1_655 ? N1 C1 1.341(3) . ? N1 C5 1.345(3) . ? N2 C6 1.364(3) . ? N2 C4 1.406(3) . ? N2 H2A 0.8600 . ? N3 C17 1.351(3) . ? N3 C18 1.418(3) . ? N3 H3A 0.8600 . ? N4 C21 1.333(4) . ? N4 C22 1.337(4) . ? N5 C27 1.335(3) . ? N5 C23 1.337(3) . ? N6 C28 1.359(3) . ? N6 C26 1.397(3) . ? N6 H6A 0.8600 . ? C1 C2 1.388(4) . ? C1 H1A 0.9300 . ? C2 C3 1.373(4) . ? C2 H2B 0.9300 . ? C3 C4 1.394(3) . ? C3 H3B 0.9300 . ? C4 C5 1.393(4) . ? C5 H5A 0.9300 . ? C6 C7 1.515(4) . ? C7 C8 1.522(4) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.528(4) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.522(4) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.528(4) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.514(4) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.519(4) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.523(4) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.518(4) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.533(4) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.506(4) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C18 C22 1.388(3) . ? C18 C19 1.388(4) . ? C19 C20 1.377(4) . ? C19 H19A 0.9300 . ? C20 C21 1.383(4) . ? C20 H20A 0.9300 . ? C21 H21A 0.9300 . ? C22 H22A 0.9300 . ? C23 C24 1.389(3) . ? C23 H23A 0.9300 . ? C24 C25 1.385(4) . ? C24 H24A 0.9300 . ? C25 C26 1.392(4) . ? C25 H25A 0.9300 . ? C26 C27 1.396(3) . ? C27 H27A 0.9300 . ? C28 C29 1.508(4) . ? C29 C30 1.520(3) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 C31 1.527(4) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C32 1.525(4) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 C33 1.533(4) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C33 1.491(6) 2_565 ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C35 1.491(3) . ? C35 C36 1.386(3) . ? C35 C40 1.393(3) . ? C36 C37 1.388(3) . ? C36 H36A 0.9300 . ? C37 C38 1.392(3) . ? C37 C42 1.497(3) . ? C38 C39 1.389(3) . ? C38 H38A 0.9300 . ? C39 C40 1.394(3) . ? C39 C41 1.494(3) . ? C40 H40A 0.9300 . ? C42 Cd 2.681(2) 1_655 ? O10 H10C 0.85(3) . ? O10 H10D 0.81(4) . ? O11 H11C 0.72(3) . ? O11 H11D 0.80(5) . ? 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 N5 Cd O4 135.75(7) . . ? N5 Cd O9 91.21(7) . 1_455 ? O4 Cd O9 128.66(6) . 1_455 ? N5 Cd O8 143.14(7) . 1_455 ? O4 Cd O8 81.11(6) . 1_455 ? O9 Cd O8 55.61(6) 1_455 1_455 ? N5 Cd N1 85.60(7) . . ? O4 Cd N1 82.73(7) . . ? O9 Cd N1 81.75(7) 1_455 . ? O8 Cd N1 102.86(7) 1_455 . ? N5 Cd O5 89.00(7) . . ? O4 Cd O5 55.08(6) . . ? O9 Cd O5 170.48(6) 1_455 . ? O8 Cd O5 120.93(6) 1_455 . ? N1 Cd O5 107.76(6) . . ? N5 Cd O5 83.89(6) . 2_764 ? O4 Cd O5 107.39(6) . 2_764 ? O9 Cd O5 94.88(6) 1_455 2_764 ? O8 Cd O5 83.61(6) 1_455 2_764 ? N1 Cd O5 168.89(6) . 2_764 ? O5 Cd O5 75.68(6) . 2_764 ? N5 Cd C42 118.71(7) . 1_455 ? O4 Cd C42 103.64(7) . 1_455 ? O9 Cd C42 27.88(6) 1_455 1_455 ? O8 Cd C42 28.21(7) 1_455 1_455 ? N1 Cd C42 89.01(7) . 1_455 ? O5 Cd C42 149.09(6) . 1_455 ? O5 Cd C42 92.89(7) 2_764 1_455 ? N5 Cd C34 113.80(7) . . ? O4 Cd C34 27.21(7) . . ? O9 Cd C34 154.75(6) 1_455 . ? O8 Cd C34 101.04(6) 1_455 . ? N1 Cd C34 96.16(7) . . ? O5 Cd C34 27.88(6) . . ? O5 Cd C34 91.37(6) 2_764 . ? C42 Cd C34 127.48(7) 1_455 . ? C34 O4 Cd 93.96(14) . . ? C34 O5 Cd 89.25(14) . . ? C34 O5 Cd 121.48(14) . 2_764 ? Cd O5 Cd 104.32(6) . 2_764 ? C41 O7 H7D 108(3) . . ? C42 O8 Cd 89.17(14) . 1_655 ? C42 O9 Cd 90.49(14) . 1_655 ? C1 N1 C5 118.7(2) . . ? C1 N1 Cd 124.04(17) . . ? C5 N1 Cd 117.16(16) . . ? C6 N2 C4 127.3(2) . . ? C6 N2 H2A 116.3 . . ? C4 N2 H2A 116.3 . . ? C17 N3 C18 123.7(2) . . ? C17 N3 H3A 118.1 . . ? C18 N3 H3A 118.1 . . ? C21 N4 C22 117.5(2) . . ? C27 N5 C23 119.2(2) . . ? C27 N5 Cd 117.82(16) . . ? C23 N5 Cd 122.96(16) . . ? C28 N6 C26 128.1(2) . . ? C28 N6 H6A 115.9 . . ? C26 N6 H6A 115.9 . . ? N1 C1 C2 122.0(2) . . ? N1 C1 H1A 119.0 . . ? C2 C1 H1A 119.0 . . ? C3 C2 C1 119.4(2) . . ? C3 C2 H2B 120.3 . . ? C1 C2 H2B 120.3 . . ? C2 C3 C4 119.4(2) . . ? C2 C3 H3B 120.3 . . ? C4 C3 H3B 120.3 . . ? C5 C4 C3 118.0(2) . . ? C5 C4 N2 123.3(2) . . ? C3 C4 N2 118.7(2) . . ? N1 C5 C4 122.5(2) . . ? N1 C5 H5A 118.7 . . ? C4 C5 H5A 118.7 . . ? O1 C6 N2 123.2(2) . . ? O1 C6 C7 122.4(2) . . ? N2 C6 C7 114.3(2) . . ? C6 C7 C8 113.6(2) . . ? C6 C7 H7A 108.9 . . ? C8 C7 H7A 108.9 . . ? C6 C7 H7B 108.9 . . ? C8 C7 H7B 108.9 . . ? H7A C7 H7B 107.7 . . ? C7 C8 C9 111.3(2) . . ? C7 C8 H8A 109.4 . . ? C9 C8 H8A 109.4 . . ? C7 C8 H8B 109.4 . . ? C9 C8 H8B 109.4 . . ? H8A C8 H8B 108.0 . . ? C10 C9 C8 114.9(2) . . ? C10 C9 H9A 108.6 . . ? C8 C9 H9A 108.6 . . ? C10 C9 H9B 108.6 . . ? C8 C9 H9B 108.6 . . ? H9A C9 H9B 107.5 . . ? C9 C10 C11 112.4(2) . . ? C9 C10 H10A 109.1 . . ? C11 C10 H10A 109.1 . . ? C9 C10 H10B 109.1 . . ? C11 C10 H10B 109.1 . . ? H10A C10 H10B 107.9 . . ? C12 C11 C10 113.9(2) . . ? C12 C11 H11A 108.8 . . ? C10 C11 H11A 108.8 . . ? C12 C11 H11B 108.8 . . ? C10 C11 H11B 108.8 . . ? H11A C11 H11B 107.7 . . ? C11 C12 C13 114.1(2) . . ? C11 C12 H12A 108.7 . . ? C13 C12 H12A 108.7 . . ? C11 C12 H12B 108.7 . . ? C13 C12 H12B 108.7 . . ? H12A C12 H12B 107.6 . . ? C12 C13 C14 112.4(2) . . ? C12 C13 H13A 109.1 . . ? C14 C13 H13A 109.1 . . ? C12 C13 H13B 109.1 . . ? C14 C13 H13B 109.1 . . ? H13A C13 H13B 107.9 . . ? C15 C14 C13 115.8(2) . . ? C15 C14 H14A 108.3 . . ? C13 C14 H14A 108.3 . . ? C15 C14 H14B 108.3 . . ? C13 C14 H14B 108.3 . . ? H14A C14 H14B 107.4 . . ? C14 C15 C16 115.4(2) . . ? C14 C15 H15A 108.4 . . ? C16 C15 H15A 108.4 . . ? C14 C15 H15B 108.4 . . ? C16 C15 H15B 108.4 . . ? H15A C15 H15B 107.5 . . ? C17 C16 C15 109.1(2) . . ? C17 C16 H16A 109.9 . . ? C15 C16 H16A 109.9 . . ? C17 C16 H16B 109.9 . . ? C15 C16 H16B 109.9 . . ? H16A C16 H16B 108.3 . . ? O2 C17 N3 121.2(3) . . ? O2 C17 C16 122.4(2) . . ? N3 C17 C16 116.3(2) . . ? C22 C18 C19 118.1(3) . . ? C22 C18 N3 118.9(2) . . ? C19 C18 N3 123.0(2) . . ? C20 C19 C18 118.3(2) . . ? C20 C19 H19A 120.9 . . ? C18 C19 H19A 120.9 . . ? C19 C20 C21 119.8(3) . . ? C19 C20 H20A 120.1 . . ? C21 C20 H20A 120.1 . . ? N4 C21 C20 122.6(3) . . ? N4 C21 H21A 118.7 . . ? C20 C21 H21A 118.7 . . ? N4 C22 C18 123.7(3) . . ? N4 C22 H22A 118.1 . . ? C18 C22 H22A 118.1 . . ? N5 C23 C24 121.1(2) . . ? N5 C23 H23A 119.4 . . ? C24 C23 H23A 119.4 . . ? C25 C24 C23 120.1(2) . . ? C25 C24 H24A 120.0 . . ? C23 C24 H24A 120.0 . . ? C24 C25 C26 118.8(2) . . ? C24 C25 H25A 120.6 . . ? C26 C25 H25A 120.6 . . ? C25 C26 C27 117.6(2) . . ? C25 C26 N6 125.8(2) . . ? C27 C26 N6 116.5(2) . . ? N5 C27 C26 123.2(2) . . ? N5 C27 H27A 118.4 . . ? C26 C27 H27A 118.4 . . ? O3 C28 N6 123.2(2) . . ? O3 C28 C29 123.4(2) . . ? N6 C28 C29 113.3(2) . . ? C28 C29 C30 114.3(2) . . ? C28 C29 H29A 108.7 . . ? C30 C29 H29A 108.7 . . ? C28 C29 H29B 108.7 . . ? C30 C29 H29B 108.7 . . ? H29A C29 H29B 107.6 . . ? C29 C30 C31 111.7(2) . . ? C29 C30 H30A 109.3 . . ? C31 C30 H30A 109.3 . . ? C29 C30 H30B 109.3 . . ? C31 C30 H30B 109.3 . . ? H30A C30 H30B 107.9 . . ? C32 C31 C30 112.7(2) . . ? C32 C31 H31A 109.1 . . ? C30 C31 H31A 109.1 . . ? C32 C31 H31B 109.1 . . ? C30 C31 H31B 109.1 . . ? H31A C31 H31B 107.8 . . ? C31 C32 C33 114.3(2) . . ? C31 C32 H32A 108.7 . . ? C33 C32 H32A 108.7 . . ? C31 C32 H32B 108.7 . . ? C33 C32 H32B 108.7 . . ? H32A C32 H32B 107.6 . . ? C33 C33 C32 114.7(3) 2_565 . ? C33 C33 H33A 108.6 2_565 . ? C32 C33 H33A 108.6 . . ? C33 C33 H33B 108.6 2_565 . ? C32 C33 H33B 108.6 . . ? H33A C33 H33B 107.6 . . ? O4 C34 O5 121.7(2) . . ? O4 C34 C35 119.5(2) . . ? O5 C34 C35 118.8(2) . . ? O4 C34 Cd 58.83(13) . . ? O5 C34 Cd 62.88(12) . . ? C35 C34 Cd 175.52(16) . . ? C36 C35 C40 119.7(2) . . ? C36 C35 C34 120.4(2) . . ? C40 C35 C34 119.9(2) . . ? C35 C36 C37 120.3(2) . . ? C35 C36 H36A 119.8 . . ? C37 C36 H36A 119.8 . . ? C36 C37 C38 120.0(2) . . ? C36 C37 C42 119.8(2) . . ? C38 C37 C42 120.2(2) . . ? C39 C38 C37 119.9(2) . . ? C39 C38 H38A 120.0 . . ? C37 C38 H38A 120.0 . . ? C38 C39 C40 119.8(2) . . ? C38 C39 C41 118.2(2) . . ? C40 C39 C41 122.0(2) . . ? C35 C40 C39 120.2(2) . . ? C35 C40 H40A 119.9 . . ? C39 C40 H40A 119.9 . . ? O6 C41 O7 123.7(2) . . ? O6 C41 C39 123.5(2) . . ? O7 C41 C39 112.8(2) . . ? O9 C42 O8 122.6(2) . . ? O9 C42 C37 118.8(2) . . ? O8 C42 C37 118.6(2) . . ? O9 C42 Cd 61.62(13) . 1_655 ? O8 C42 Cd 62.62(13) . 1_655 ? C37 C42 Cd 165.45(16) . 1_655 ? H10C O10 H10D 101(3) . . ? H11C O11 H11D 113(4) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 28.34 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.297 _refine_diff_density_min -1.074 _refine_diff_density_rms 0.094 #===END _database_code_depnum_ccdc_archive 'CCDC 917804'