# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Jiang, Jianzhuang' _publ_contact_author_email jianzhuang@ustb.edu.cn _publ_section_title ; Synthesis, Crystal Structures, and Luminescent Properties of Cd(II) Coordination Polymers Assembled from Asymmetric Semi-rigid V-Shaped Multicarboxylate Ligands ; _publ_author_name 'Jianzhuang Jiang' # Attachment 'complexes.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 746377' #TrackingRef 'complexes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C66 H42 Cd3 N6 O16' _chemical_formula_weight 1512.29 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 'C 2/c ' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 15.159(3) _cell_length_b 18.821(3) _cell_length_c 19.798(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.382(3) _cell_angle_gamma 90.00 _cell_volume 5643.4(16) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 7636 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 27.45 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.780 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3008 _exptl_absorpt_coefficient_mu 1.202 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7950 _exptl_absorpt_correction_T_max 0.8402 _exptl_absorpt_process_details '(SADABS; Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 0 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 13563 _diffrn_reflns_av_R_equivalents 0.0403 _diffrn_reflns_av_sigmaI/netI 0.0469 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4961 _reflns_number_gt 4226 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'SAINT-Plus (Bruker, 2001)' _computing_data_reduction SAINT-Plus _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Sheldrick, 1998)' _computing_publication_material XP _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^)+(0.0830P)^2^+18.8716P] 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 4961 _refine_ls_number_parameters 411 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0609 _refine_ls_R_factor_gt 0.0521 _refine_ls_wR_factor_ref 0.1435 _refine_ls_wR_factor_gt 0.1383 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.233 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 1.2819(5) 0.4166(4) 0.1239(3) 0.0468(15) Uani 1 1 d . . . C2 C 1.3213(4) 0.3845(4) 0.0699(3) 0.0467(15) Uani 1 1 d . . . C3 C 1.3391(6) 0.3136(5) 0.0694(4) 0.074(2) Uani 1 1 d . . . H3 H 1.3644 0.2930 0.0322 0.089 Uiso 1 1 calc R . . C4 C 1.3191(7) 0.2725(5) 0.1248(5) 0.085(3) Uani 1 1 d . . . H4 H 1.3310 0.2240 0.1249 0.102 Uiso 1 1 calc R . . C5 C 1.2815(6) 0.3039(4) 0.1802(4) 0.068(2) Uani 1 1 d . . . H5 H 1.2690 0.2766 0.2178 0.082 Uiso 1 1 calc R . . C6 C 1.2628(5) 0.3746(4) 0.1793(3) 0.0587(18) Uani 1 1 d . . . H6 H 1.2370 0.3952 0.2163 0.070 Uiso 1 1 calc R . . C7 C 1.2564(5) 0.4941(4) 0.1219(4) 0.0550(18) Uani 1 1 d . . . C8 C 1.1636(4) 0.4204(3) -0.1106(3) 0.0363(12) Uani 1 1 d . . . C9 C 1.2110(4) 0.4260(3) -0.1703(3) 0.0375(12) Uani 1 1 d . . . C10 C 1.3028(4) 0.4314(3) -0.1644(3) 0.0453(14) Uani 1 1 d . . . H10 H 1.3347 0.4351 -0.2033 0.054 Uiso 1 1 calc R . . C11 C 1.3469(4) 0.4312(4) -0.1027(3) 0.0469(15) Uani 1 1 d . . . H11 H 1.4080 0.4359 -0.0999 0.056 Uiso 1 1 calc R . . C12 C 1.3006(4) 0.4242(3) -0.0449(3) 0.0425(14) Uani 1 1 d . . . C13 C 1.2099(4) 0.4182(3) -0.0487(3) 0.0417(13) Uani 1 1 d . . . H13 H 1.1794 0.4125 -0.0092 0.050 Uiso 1 1 calc R . . C14 C 1.0648(4) 0.4158(3) -0.1116(3) 0.0420(13) Uani 1 1 d . . . C15 C 1.1686(4) 0.4275(3) -0.2395(3) 0.0402(13) Uani 1 1 d . . . C16 C 1.1766(6) 0.6076(5) -0.0436(4) 0.067(2) Uani 1 1 d . . . H16 H 1.1851 0.5594 -0.0354 0.081 Uiso 1 1 calc R . . C17 C 1.1894(6) 0.6330(6) -0.1080(4) 0.083(3) Uani 1 1 d . . . H17 H 1.2049 0.6021 -0.1422 0.100 Uiso 1 1 calc R . . C18 C 1.1792(6) 0.7027(7) -0.1207(4) 0.082(3) Uani 1 1 d . . . H18 H 1.1897 0.7207 -0.1634 0.098 Uiso 1 1 calc R . . C19 C 1.1527(5) 0.7481(5) -0.0695(5) 0.073(3) Uani 1 1 d . . . C20 C 1.1386(7) 0.8219(6) -0.0787(6) 0.093(3) Uani 1 1 d . . . H20 H 1.1479 0.8423 -0.1206 0.111 Uiso 1 1 calc R . . C21 C 1.1120(7) 0.8628(5) -0.0282(6) 0.096(4) Uani 1 1 d . . . H21 H 1.1032 0.9110 -0.0361 0.115 Uiso 1 1 calc R . . C22 C 1.0960(7) 0.8343(4) 0.0396(5) 0.082(3) Uani 1 1 d . . . C23 C 1.0722(9) 0.8747(5) 0.0946(7) 0.115(5) Uani 1 1 d . . . H23 H 1.0615 0.9231 0.0895 0.138 Uiso 1 1 calc R . . C24 C 1.0645(10) 0.8439(6) 0.1553(7) 0.121(5) Uani 1 1 d . . . H24 H 1.0484 0.8709 0.1922 0.146 Uiso 1 1 calc R . . C25 C 1.0810(7) 0.7709(5) 0.1628(5) 0.084(3) Uani 1 1 d . . . H25 H 1.0770 0.7504 0.2053 0.100 Uiso 1 1 calc R . . C26 C 1.1117(5) 0.7614(4) 0.0501(4) 0.0578(19) Uani 1 1 d . . . C27 C 1.1389(4) 0.7184(4) -0.0048(3) 0.0503(16) Uani 1 1 d . . . C28 C 1.0426(5) 0.6135(4) -0.3813(3) 0.0539(17) Uani 1 1 d . . . H28 H 1.0452 0.5706 -0.4043 0.065 Uiso 1 1 calc R . . C29 C 1.0625(5) 0.6754(4) -0.4156(3) 0.0544(17) Uani 1 1 d . . . H29 H 1.0795 0.6733 -0.4601 0.065 Uiso 1 1 calc R . . C30 C 1.0569(5) 0.7391(4) -0.3836(3) 0.0518(16) Uani 1 1 d . . . H30 H 1.0710 0.7809 -0.4057 0.062 Uiso 1 1 calc R . . C31 C 1.0296(4) 0.7410(3) -0.3164(3) 0.0414(13) Uani 1 1 d . . . C32 C 1.0133(4) 0.6764(3) -0.2846(3) 0.0374(12) Uani 1 1 d . . . C33 C 1.0152(4) 0.8069(3) -0.2819(3) 0.0496(15) Uani 1 1 d . . . H33 H 1.0267 0.8498 -0.3032 0.060 Uiso 1 1 calc R . . N1 N 1.1018(4) 0.7305(3) 0.1118(3) 0.0565(15) Uani 1 1 d . . . N2 N 1.1525(3) 0.6487(3) 0.0079(3) 0.0501(13) Uani 1 1 d . . . N3 N 1.0201(4) 0.6127(3) -0.3173(3) 0.0418(12) Uani 1 1 d . . . O1 O 1.3038(4) 0.5375(3) 0.1533(4) 0.0801(18) Uani 1 1 d . . . O2 O 1.1847(4) 0.5080(3) 0.0896(2) 0.0678(15) Uani 1 1 d . . . O3 O 1.3491(3) 0.4274(3) 0.0166(2) 0.0528(11) Uani 1 1 d . . . O4 O 1.0281(4) 0.3995(4) -0.0593(3) 0.094(2) Uani 1 1 d . . . O5 O 1.0188(3) 0.4276(3) -0.1643(2) 0.0547(12) Uani 1 1 d . . . O6 O 1.1410(3) 0.4868(2) -0.2620(2) 0.0484(11) Uani 1 1 d . . . O7 O 1.1672(3) 0.3714(3) -0.2733(2) 0.0516(11) Uani 1 1 d . . . O9 O 1.4742(6) 0.5092(6) 0.1818(6) 0.149(4) Uani 1 1 d D . . H9A H 1.4367 0.4714 0.1758 0.223 Uiso 1 1 d RD . . H9B H 1.4110 0.5484 0.1599 0.223 Uiso 1 1 d RD . . Cd1 Cd 1.11865(3) 0.60693(2) 0.11765(2) 0.03861(19) Uani 1 1 d . . . Cd2 Cd 1.0000 0.51310(3) -0.2500 0.0400(2) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.063(4) 0.043(3) 0.035(3) -0.002(3) 0.001(3) 0.010(3) C2 0.056(4) 0.053(4) 0.031(3) -0.002(3) -0.008(3) 0.009(3) C3 0.105(6) 0.059(5) 0.058(5) -0.023(4) 0.002(4) 0.019(4) C4 0.121(8) 0.046(5) 0.088(7) 0.004(4) -0.011(6) 0.020(5) C5 0.102(6) 0.051(4) 0.050(4) 0.013(4) -0.010(4) 0.006(4) C6 0.090(5) 0.050(4) 0.036(3) 0.010(3) 0.005(3) 0.008(4) C7 0.078(5) 0.044(4) 0.046(4) 0.006(3) 0.027(4) 0.010(4) C8 0.050(3) 0.032(3) 0.026(3) 0.000(2) 0.003(2) -0.002(2) C9 0.054(3) 0.031(3) 0.028(3) 0.000(2) 0.004(2) 0.003(2) C10 0.057(4) 0.049(4) 0.031(3) -0.001(3) 0.010(3) 0.004(3) C11 0.049(4) 0.058(4) 0.034(3) -0.005(3) 0.005(3) 0.005(3) C12 0.054(4) 0.045(3) 0.029(3) -0.006(3) 0.000(2) 0.000(3) C13 0.055(4) 0.047(3) 0.023(3) -0.001(2) 0.003(2) -0.004(3) C14 0.057(4) 0.038(3) 0.031(3) 0.002(3) 0.003(3) -0.006(3) C15 0.050(3) 0.044(3) 0.026(3) 0.003(3) 0.005(2) 0.000(3) C16 0.079(5) 0.084(6) 0.039(4) 0.007(4) 0.002(4) 0.012(4) C17 0.092(6) 0.112(8) 0.045(4) 0.015(5) 0.010(4) 0.009(6) C18 0.068(5) 0.137(9) 0.041(4) 0.025(5) 0.004(4) -0.017(5) C19 0.056(4) 0.089(6) 0.072(6) 0.043(5) -0.024(4) -0.030(4) C20 0.113(8) 0.080(7) 0.081(7) 0.047(6) -0.035(6) -0.045(6) C21 0.117(8) 0.058(5) 0.107(8) 0.053(6) -0.057(7) -0.035(5) C22 0.107(7) 0.042(4) 0.093(7) 0.012(4) -0.039(5) -0.013(4) C23 0.178(12) 0.047(5) 0.116(10) 0.008(6) -0.054(9) 0.017(6) C24 0.194(13) 0.062(6) 0.107(9) -0.021(6) -0.011(9) 0.042(8) C25 0.130(8) 0.056(5) 0.064(5) -0.014(4) -0.015(5) 0.019(5) C26 0.066(4) 0.043(4) 0.062(5) 0.022(3) -0.024(3) -0.014(3) C27 0.051(4) 0.053(4) 0.046(4) 0.019(3) -0.014(3) -0.014(3) C28 0.072(5) 0.054(4) 0.036(3) -0.005(3) 0.005(3) 0.009(3) C29 0.070(4) 0.061(4) 0.033(3) 0.002(3) 0.009(3) 0.009(3) C30 0.065(4) 0.056(4) 0.035(3) 0.010(3) 0.007(3) 0.003(3) C31 0.052(3) 0.041(3) 0.031(3) 0.003(2) 0.000(2) 0.002(3) C32 0.043(3) 0.040(3) 0.029(3) -0.003(2) -0.002(2) 0.001(2) C33 0.065(4) 0.035(3) 0.049(4) 0.003(3) 0.005(3) -0.003(3) N1 0.074(4) 0.043(3) 0.051(3) 0.002(3) -0.012(3) 0.002(3) N2 0.053(3) 0.057(3) 0.040(3) 0.019(3) 0.000(2) -0.004(3) N3 0.057(3) 0.038(3) 0.031(3) -0.002(2) 0.003(2) 0.004(2) O1 0.094(4) 0.047(3) 0.102(5) -0.001(3) 0.039(4) -0.008(3) O2 0.102(4) 0.065(3) 0.038(3) 0.010(2) 0.009(3) 0.036(3) O3 0.056(3) 0.076(3) 0.025(2) -0.003(2) -0.0057(18) -0.008(2) O4 0.058(3) 0.185(8) 0.039(3) 0.032(4) 0.000(2) -0.030(4) O5 0.055(3) 0.067(3) 0.042(3) 0.023(2) -0.003(2) 0.000(2) O6 0.057(3) 0.051(3) 0.037(2) 0.015(2) 0.0070(19) 0.008(2) O7 0.075(3) 0.048(3) 0.031(2) -0.003(2) -0.004(2) -0.005(2) O9 0.102(6) 0.132(8) 0.215(12) -0.030(7) 0.033(7) 0.007(5) Cd1 0.0526(3) 0.0353(3) 0.0280(3) 0.00479(16) 0.00259(19) -0.00177(17) Cd2 0.0545(4) 0.0328(3) 0.0328(3) 0.000 0.0023(3) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.384(9) . ? C1 C6 1.393(9) . ? C1 C7 1.508(9) . ? C2 C3 1.362(10) . ? C2 O3 1.407(8) . ? C3 C4 1.387(13) . ? C3 H3 0.9300 . ? C4 C5 1.388(13) . ? C4 H4 0.9300 . ? C5 C6 1.361(11) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 O1 1.238(10) . ? C7 O2 1.265(10) . ? C8 C13 1.389(8) . ? C8 C9 1.411(8) . ? C8 C14 1.499(9) . ? C9 C10 1.395(9) . ? C9 C15 1.489(8) . ? C10 C11 1.369(9) . ? C10 H10 0.9300 . ? C11 C12 1.372(8) . ? C11 H11 0.9300 . ? C12 C13 1.378(9) . ? C12 O3 1.397(7) . ? C13 H13 0.9300 . ? C14 O4 1.235(8) . ? C14 O5 1.251(7) . ? C15 O7 1.250(8) . ? C15 O6 1.267(7) . ? C16 N2 1.342(10) . ? C16 C17 1.384(11) . ? C16 H16 0.9300 . ? C17 C18 1.344(15) . ? C17 H17 0.9300 . ? C18 C19 1.396(14) . ? C18 H18 0.9300 . ? C19 C20 1.416(14) . ? C19 C27 1.422(10) . ? C20 C21 1.338(16) . ? C20 H20 0.9300 . ? C21 C22 1.475(14) . ? C21 H21 0.9300 . ? C22 C23 1.388(16) . ? C22 C26 1.407(11) . ? C23 C24 1.343(17) . ? C23 H23 0.9300 . ? C24 C25 1.404(13) . ? C24 H24 0.9300 . ? C25 N1 1.312(10) . ? C25 H25 0.9300 . ? C26 N1 1.366(9) . ? C26 C27 1.429(11) . ? C27 N2 1.349(9) . ? C28 N3 1.326(9) . ? C28 C29 1.387(10) . ? C28 H28 0.9300 . ? C29 C30 1.360(10) . ? C29 H29 0.9300 . ? C30 C31 1.409(9) . ? C30 H30 0.9300 . ? C31 C32 1.396(9) . ? C31 C33 1.438(9) . ? C32 N3 1.368(8) . ? C32 C32 1.445(11) 2_754 ? C33 C33 1.361(13) 2_754 ? C33 H33 0.9300 . ? N1 Cd1 2.342(6) . ? N2 Cd1 2.386(5) . ? N3 Cd2 2.327(5) . ? O2 Cd1 2.197(5) . ? O4 Cd1 2.466(6) 5_765 ? O5 Cd2 2.347(4) . ? O5 Cd1 2.403(4) 5_765 ? O6 Cd2 2.216(4) . ? O7 Cd1 2.289(4) 6_565 ? O9 H9A 0.9151 . ? O9 H9B 1.2716 . ? Cd1 O7 2.289(4) 6_566 ? Cd1 O5 2.403(4) 5_765 ? Cd1 O4 2.466(6) 5_765 ? Cd2 O6 2.216(4) 2_754 ? Cd2 N3 2.327(5) 2_754 ? Cd2 O5 2.347(4) 2_754 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 118.1(6) . . ? C2 C1 C7 121.4(6) . . ? C6 C1 C7 120.5(6) . . ? C3 C2 C1 121.7(7) . . ? C3 C2 O3 119.4(6) . . ? C1 C2 O3 118.8(6) . . ? C2 C3 C4 119.4(8) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C3 C4 C5 119.9(8) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? C6 C5 C4 119.8(7) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C5 C6 C1 121.0(7) . . ? C5 C6 H6 119.5 . . ? C1 C6 H6 119.5 . . ? O1 C7 O2 125.9(7) . . ? O1 C7 C1 118.8(7) . . ? O2 C7 C1 115.3(7) . . ? C13 C8 C9 119.0(5) . . ? C13 C8 C14 118.6(5) . . ? C9 C8 C14 122.4(5) . . ? C10 C9 C8 118.4(5) . . ? C10 C9 C15 117.8(5) . . ? C8 C9 C15 123.8(5) . . ? C11 C10 C9 121.5(6) . . ? C11 C10 H10 119.2 . . ? C9 C10 H10 119.2 . . ? C10 C11 C12 119.8(6) . . ? C10 C11 H11 120.1 . . ? C12 C11 H11 120.1 . . ? C11 C12 C13 120.4(6) . . ? C11 C12 O3 116.9(5) . . ? C13 C12 O3 122.6(5) . . ? C12 C13 C8 120.8(5) . . ? C12 C13 H13 119.6 . . ? C8 C13 H13 119.6 . . ? O4 C14 O5 119.2(6) . . ? O4 C14 C8 119.3(6) . . ? O5 C14 C8 121.5(5) . . ? O7 C15 O6 124.0(6) . . ? O7 C15 C9 118.2(5) . . ? O6 C15 C9 117.6(5) . . ? N2 C16 C17 123.7(9) . . ? N2 C16 H16 118.2 . . ? C17 C16 H16 118.2 . . ? C18 C17 C16 119.3(10) . . ? C18 C17 H17 120.3 . . ? C16 C17 H17 120.3 . . ? C17 C18 C19 119.8(8) . . ? C17 C18 H18 120.1 . . ? C19 C18 H18 120.1 . . ? C18 C19 C20 123.6(9) . . ? C18 C19 C27 118.1(8) . . ? C20 C19 C27 118.3(10) . . ? C21 C20 C19 121.1(9) . . ? C21 C20 H20 119.4 . . ? C19 C20 H20 119.4 . . ? C20 C21 C22 122.6(9) . . ? C20 C21 H21 118.7 . . ? C22 C21 H21 118.7 . . ? C23 C22 C26 117.8(9) . . ? C23 C22 C21 124.9(9) . . ? C26 C22 C21 117.1(10) . . ? C24 C23 C22 120.0(9) . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? C23 C24 C25 119.7(11) . . ? C23 C24 H24 120.2 . . ? C25 C24 H24 120.2 . . ? N1 C25 C24 122.2(10) . . ? N1 C25 H25 118.9 . . ? C24 C25 H25 118.9 . . ? N1 C26 C22 121.5(8) . . ? N1 C26 C27 119.0(6) . . ? C22 C26 C27 119.5(7) . . ? N2 C27 C19 121.5(8) . . ? N2 C27 C26 117.0(6) . . ? C19 C27 C26 121.4(7) . . ? N3 C28 C29 123.1(6) . . ? N3 C28 H28 118.4 . . ? C29 C28 H28 118.4 . . ? C30 C29 C28 119.6(6) . . ? C30 C29 H29 120.2 . . ? C28 C29 H29 120.2 . . ? C29 C30 C31 119.2(6) . . ? C29 C30 H30 120.4 . . ? C31 C30 H30 120.4 . . ? C32 C31 C30 117.9(6) . . ? C32 C31 C33 120.3(5) . . ? C30 C31 C33 121.8(6) . . ? N3 C32 C31 122.2(5) . . ? N3 C32 C32 118.5(3) . 2_754 ? C31 C32 C32 119.3(3) . 2_754 ? C33 C33 C31 120.3(4) 2_754 . ? C33 C33 H33 119.8 2_754 . ? C31 C33 H33 119.8 . . ? C25 N1 C26 118.7(7) . . ? C25 N1 Cd1 124.5(6) . . ? C26 N1 Cd1 116.8(5) . . ? C16 N2 C27 117.6(6) . . ? C16 N2 Cd1 125.2(5) . . ? C27 N2 Cd1 116.9(5) . . ? C28 N3 C32 118.0(5) . . ? C28 N3 Cd2 127.0(4) . . ? C32 N3 Cd2 114.9(4) . . ? C7 O2 Cd1 116.0(5) . . ? C12 O3 C2 117.7(5) . . ? C14 O4 Cd1 92.8(4) . 5_765 ? C14 O5 Cd2 140.4(4) . . ? C14 O5 Cd1 95.4(4) . 5_765 ? Cd2 O5 Cd1 112.45(18) . 5_765 ? C15 O6 Cd2 117.7(4) . . ? C15 O7 Cd1 110.6(4) . 6_565 ? H9A O9 H9B 87.3 . . ? O2 Cd1 O7 104.92(18) . 6_566 ? O2 Cd1 N1 151.6(2) . . ? O7 Cd1 N1 84.22(19) 6_566 . ? O2 Cd1 N2 86.1(2) . . ? O7 Cd1 N2 136.65(19) 6_566 . ? N1 Cd1 N2 69.8(2) . . ? O2 Cd1 O5 106.3(2) . 5_765 ? O7 Cd1 O5 86.30(17) 6_566 5_765 ? N1 Cd1 O5 101.1(2) . 5_765 ? N2 Cd1 O5 131.42(16) . 5_765 ? O2 Cd1 O4 104.6(3) . 5_765 ? O7 Cd1 O4 134.34(18) 6_566 5_765 ? N1 Cd1 O4 86.1(2) . 5_765 ? N2 Cd1 O4 79.26(17) . 5_765 ? O5 Cd1 O4 52.22(16) 5_765 5_765 ? O6 Cd2 O6 154.2(2) 2_754 . ? O6 Cd2 N3 88.22(17) 2_754 2_754 ? O6 Cd2 N3 112.99(18) . 2_754 ? O6 Cd2 N3 112.99(18) 2_754 . ? O6 Cd2 N3 88.22(17) . . ? N3 Cd2 N3 72.7(2) 2_754 . ? O6 Cd2 O5 80.54(15) 2_754 2_754 ? O6 Cd2 O5 81.85(17) . 2_754 ? N3 Cd2 O5 162.06(18) 2_754 2_754 ? N3 Cd2 O5 98.85(18) . 2_754 ? O6 Cd2 O5 81.85(17) 2_754 . ? O6 Cd2 O5 80.54(15) . . ? N3 Cd2 O5 98.85(18) 2_754 . ? N3 Cd2 O5 162.06(18) . . ? O5 Cd2 O5 93.4(3) 2_754 . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 3.185 _refine_diff_density_min -0.860 _refine_diff_density_rms 0.146 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 746378' #TrackingRef 'complexes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H48 Cd3 N6 O19' _chemical_formula_weight 1494.24 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 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.5260(5) _cell_length_b 15.0310(8) _cell_length_c 22.0200(11) _cell_angle_alpha 70.5440(10) _cell_angle_beta 78.3470(10) _cell_angle_gamma 84.9060(10) _cell_volume 2910.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 5265 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 26.56 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.705 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1492 _exptl_absorpt_coefficient_mu 1.168 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8262 _exptl_absorpt_correction_T_max 0.8922 _exptl_absorpt_process_details '(SADABS; Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 0 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 14571 _diffrn_reflns_av_R_equivalents 0.0184 _diffrn_reflns_av_sigmaI/netI 0.0412 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10139 _reflns_number_gt 8174 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'SAINT-Plus (Bruker, 2001)' _computing_data_reduction SAINT-Plus _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Sheldrick, 1998)' _computing_publication_material XP _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^)+(0.0736P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10139 _refine_ls_number_parameters 788 _refine_ls_number_restraints 45 _refine_ls_R_factor_all 0.0547 _refine_ls_R_factor_gt 0.0419 _refine_ls_wR_factor_ref 0.1211 _refine_ls_wR_factor_gt 0.1143 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 11.389 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.071(5) 0.087(3) 0.820(2) 0.038(11) Uani 1 1 d . . . C2 C -0.057(5) 0.279(3) 0.839(2) 0.035(11) Uani 1 1 d . . . C3 C 0.063(5) 0.237(3) 0.800(2) 0.031(10) Uani 1 1 d . . . C4 C 0.184(5) 0.289(3) 0.772(2) 0.038(11) Uani 1 1 d . . . H4 H 0.1889 0.3464 0.7788 0.046 Uiso 1 1 calc R . . C5 C 0.301(5) 0.259(4) 0.734(3) 0.043(12) Uani 1 1 d . . . H5 H 0.3820 0.2950 0.7150 0.052 Uiso 1 1 calc R . . C6 C 0.292(5) 0.174(4) 0.724(2) 0.036(11) Uani 1 1 d . . . C7 C 0.173(5) 0.119(3) 0.752(2) 0.036(11) Uani 1 1 d . . . H7 H 0.1701 0.0613 0.7453 0.043 Uiso 1 1 calc R . . C8 C 0.055(5) 0.151(3) 0.790(2) 0.032(10) Uani 1 1 d . . . C9 C 0.493(5) 0.092(3) 0.593(2) 0.037(11) Uani 1 1 d . . . C10 C 0.418(5) 0.158(3) 0.623(2) 0.038(11) Uani 1 1 d . . . C11 C 0.360(6) 0.240(4) 0.584(3) 0.052(14) Uani 1 1 d . . . H11 H 0.3082 0.2824 0.6037 0.062 Uiso 1 1 calc R . . C12 C 0.378(7) 0.260(4) 0.518(3) 0.064(17) Uani 1 1 d . . . H12 H 0.3418 0.3169 0.4922 0.076 Uiso 1 1 calc R . . C13 C 0.451(7) 0.197(4) 0.488(3) 0.059(16) Uani 1 1 d . . . H13 H 0.4616 0.2104 0.4428 0.071 Uiso 1 1 calc R . . C14 C 0.506(6) 0.116(4) 0.526(3) 0.047(13) Uani 1 1 d . . . H14 H 0.5549 0.0736 0.5059 0.056 Uiso 1 1 calc R . . C15 C 0.558(5) 0.001(4) 0.631(3) 0.042(12) Uani 1 1 d . . . C16 C -0.115(5) 0.605(3) 0.810(2) 0.036(11) Uani 1 1 d . . . C17 C -0.125(5) 0.806(3) 0.818(2) 0.034(11) Uani 1 1 d . . . C18 C 0.009(5) 0.671(3) 0.779(2) 0.034(11) Uani 1 1 d . . . C19 C 0.137(5) 0.640(3) 0.749(2) 0.039(11) Uani 1 1 d . . . H19 H 0.1456 0.5785 0.7474 0.046 Uiso 1 1 calc R . . C20 C 0.251(5) 0.699(4) 0.721(3) 0.040(12) Uani 1 1 d . . . C21 C 0.242(5) 0.790(3) 0.721(3) 0.043(12) Uani 1 1 d . . . H21 H 0.3189 0.8298 0.7010 0.051 Uiso 1 1 calc R . . C22 C 0.117(5) 0.821(3) 0.752(3) 0.041(12) Uani 1 1 d . . . H22 H 0.1102 0.8830 0.7523 0.050 Uiso 1 1 calc R . . C23 C 0.000(5) 0.764(3) 0.782(2) 0.034(10) Uani 1 1 d . . . C24 C 0.486(5) 0.526(3) 0.676(2) 0.038(11) Uani 1 1 d . . . C25 C 0.394(5) 0.604(3) 0.661(2) 0.039(12) Uani 1 1 d . . . C26 C 0.319(6) 0.621(5) 0.611(3) 0.061(16) Uani 1 1 d . . . H26 H 0.2545 0.6721 0.6030 0.074 Uiso 1 1 calc R . . C27 C 0.338(8) 0.563(6) 0.574(3) 0.08(2) Uani 1 1 d . . . H27 H 0.2867 0.5740 0.5403 0.095 Uiso 1 1 calc R . . C28 C 0.433(8) 0.487(5) 0.586(3) 0.071(19) Uani 1 1 d . . . H28 H 0.4480 0.4482 0.5599 0.085 Uiso 1 1 calc R . . C30 C 0.562(6) 0.498(4) 0.734(3) 0.055(15) Uani 1 1 d . . . C31 C -0.610(6) -0.116(5) 0.869(3) 0.059(16) Uani 1 1 d . . . H31 H -0.5817 -0.1028 0.8242 0.071 Uiso 1 1 calc R . . C32 C -0.750(7) -0.144(5) 0.897(3) 0.067(17) Uani 1 1 d . . . H32 H -0.8136 -0.1500 0.8722 0.080 Uiso 1 1 calc R . . C33 C -0.790(6) -0.163(4) 0.964(3) 0.061(17) Uani 1 1 d . . . H33 H -0.8831 -0.1804 0.9843 0.073 Uiso 1 1 calc R . . C34 C -0.692(6) -0.155(4) 1.000(3) 0.050(14) Uani 1 1 d . . . H34 H -0.7190 -0.1686 1.0451 0.060 Uiso 1 1 calc R . . C35 C -0.555(5) -0.126(3) 0.969(2) 0.038(11) Uani 1 1 d . . . C36 C -0.445(6) -0.115(3) 1.004(2) 0.038(11) Uani 1 1 d . . . C37 C -0.470(7) -0.132(4) 1.072(3) 0.059(17) Uani 1 1 d . . . H37 H -0.5600 -0.1518 1.0967 0.071 Uiso 1 1 calc R . . C38 C -0.360(9) -0.120(5) 1.101(3) 0.07(2) Uani 1 1 d . . . H38 H -0.3755 -0.1308 1.1460 0.084 Uiso 1 1 calc R . . C39 C -0.229(8) -0.093(4) 1.063(3) 0.066(18) Uani 1 1 d . . . H39 H -0.1532 -0.0862 1.0821 0.079 Uiso 1 1 calc R . . C40 C -0.210(7) -0.075(4) 0.997(3) 0.052(14) Uani 1 1 d . . . H40 H -0.1212 -0.0552 0.9712 0.063 Uiso 1 1 calc R . . C41 C 0.957(9) 0.017(6) 0.639(4) 0.10(3) Uani 1 1 d . . . H41 H 0.9010 0.0392 0.6714 0.116 Uiso 1 1 calc R . . C42 C 1.078(13) 0.067(8) 0.598(6) 0.13(4) Uani 1 1 d U . . H42 H 1.1007 0.1237 0.6017 0.150 Uiso 1 1 calc R . . C43 C 1.159(11) 0.031(10) 0.554(6) 0.14(6) Uani 1 1 d . . . H43 H 1.2380 0.0636 0.5257 0.173 Uiso 1 1 calc R . . C44 C 1.128(9) -0.052(10) 0.549(5) 0.14(5) Uani 1 1 d . . . H44 H 1.1873 -0.0765 0.5195 0.164 Uiso 1 1 calc R . . C45 C 1.006(6) -0.102(7) 0.589(3) 0.08(3) Uani 1 1 d . . . C46 C 0.960(7) -0.192(6) 0.587(3) 0.066(18) Uani 1 1 d . . . C47 C 1.032(9) -0.236(9) 0.538(4) 0.11(4) Uani 1 1 d . . . H47 H 1.1079 -0.2076 0.5059 0.134 Uiso 1 1 calc R . . C48 C 0.981(12) -0.320(8) 0.544(5) 0.10(3) Uani 1 1 d U . . H48 H 1.0244 -0.3490 0.5134 0.126 Uiso 1 1 calc R . . C49 C 0.872(12) -0.364(7) 0.590(5) 0.11(3) Uani 1 1 d U . . H49 H 0.8390 -0.4216 0.5927 0.133 Uiso 1 1 calc R . . C50 C 0.811(9) -0.315(6) 0.634(4) 0.09(2) Uani 1 1 d . . . H50 H 0.7355 -0.3438 0.6665 0.104 Uiso 1 1 calc R . . C51 C -0.624(6) 0.374(4) 0.884(3) 0.055(15) Uani 1 1 d . . . H51 H -0.6123 0.3849 0.8394 0.067 Uiso 1 1 calc R . . C52 C -0.756(6) 0.345(4) 0.922(3) 0.054(15) Uani 1 1 d . . . H52 H -0.8307 0.3356 0.9038 0.065 Uiso 1 1 calc R . . C53 C -0.775(6) 0.332(4) 0.987(3) 0.052(14) Uani 1 1 d . . . H53 H -0.8624 0.3120 1.0142 0.062 Uiso 1 1 calc R . . C54 C -0.663(5) 0.347(3) 1.014(2) 0.042(12) Uani 1 1 d . . . H54 H -0.6747 0.3378 1.0583 0.051 Uiso 1 1 calc R . . C55 C -0.532(5) 0.375(3) 0.973(2) 0.035(11) Uani 1 1 d . . . C56 C -0.406(5) 0.391(3) 0.998(2) 0.036(11) Uani 1 1 d . . . C57 C -0.412(7) 0.382(4) 1.063(3) 0.053(14) Uani 1 1 d . . . H57 H -0.4975 0.3678 1.0925 0.063 Uiso 1 1 calc R . . C58 C -0.289(7) 0.393(4) 1.083(3) 0.061(16) Uani 1 1 d . . . H58 H -0.2905 0.3868 1.1268 0.074 Uiso 1 1 calc R . . C59 C -0.164(7) 0.414(4) 1.038(3) 0.060(16) Uani 1 1 d . . . H59 H -0.0795 0.4222 1.0504 0.072 Uiso 1 1 calc R . . C60 C -0.165(6) 0.423(4) 0.974(3) 0.049(13) Uani 1 1 d . . . H60 H -0.0800 0.4371 0.9443 0.059 Uiso 1 1 calc R . . C29 C 0.506(7) 0.470(4) 0.637(3) 0.055(15) Uiso 1 1 d . . . H29 H 0.5703 0.4186 0.6446 0.066 Uiso 1 1 calc R . . N1 N -0.514(5) -0.107(3) 0.903(2) 0.044(10) Uani 1 1 d . . . N2 N -0.315(5) -0.085(3) 0.968(2) 0.042(10) Uani 1 1 d . . . N3 N 0.923(6) -0.062(4) 0.633(3) 0.064(14) Uani 1 1 d . . . N4 N 0.853(6) -0.233(4) 0.633(2) 0.059(13) Uani 1 1 d . . . N5 N -0.513(5) 0.388(3) 0.908(2) 0.043(10) Uani 1 1 d . . . N6 N -0.283(4) 0.413(3) 0.953(2) 0.037(9) Uani 1 1 d . . . O1 O -0.068(4) 0.014(3) 0.803(3) 0.078(15) Uani 1 1 d . . . O2 O -0.173(4) 0.107(3) 0.8573(19) 0.059(11) Uani 1 1 d . . . O3 O -0.043(4) 0.279(3) 0.8930(19) 0.058(11) Uani 1 1 d . . . O4 O -0.160(4) 0.319(3) 0.810(2) 0.054(10) Uani 1 1 d . . . O5 O 0.409(4) 0.137(3) 0.6888(16) 0.050(10) Uani 1 1 d . . . O6 O 0.581(5) -0.013(3) 0.688(2) 0.071(13) Uani 1 1 d . . . O7 O 0.590(5) -0.061(3) 0.605(2) 0.071(13) Uani 1 1 d . . . O8 O -0.097(4) 0.525(2) 0.803(2) 0.058(11) Uani 1 1 d . . . O9 O -0.229(4) 0.634(2) 0.8367(17) 0.045(9) Uani 1 1 d . . . O10 O -0.223(3) 0.852(2) 0.7874(16) 0.038(8) Uani 1 1 d . . . O11 O -0.117(4) 0.806(3) 0.8728(17) 0.049(9) Uani 1 1 d . . . O12 O 0.386(4) 0.669(3) 0.694(2) 0.056(11) Uani 1 1 d . . . O13 O 0.573(7) 0.551(3) 0.765(2) 0.093(18) Uani 1 1 d . . . O14 O 0.604(6) 0.415(4) 0.753(2) 0.099(19) Uani 1 1 d . . . O15 O -0.395(5) 0.061(3) 0.7826(19) 0.062(11) Uani 1 1 d D . . H15B H -0.4342 0.0462 0.7555 0.093 Uiso 1 1 d RD . . H15C H -0.3767 0.1213 0.7668 0.093 Uiso 1 1 d RD . . O16 O 0.579(4) -0.266(3) 0.7622(19) 0.054(10) Uani 1 1 d D . . H16A H 0.5232 -0.3077 0.7628 0.081 Uiso 1 1 d RD . . H16B H 0.6048 -0.2821 0.7996 0.081 Uiso 1 1 d RD . . O17 O -0.308(7) 0.242(3) 0.744(3) 0.11(2) Uani 1 1 d D . . H17A H -0.2836 0.2982 0.7193 0.169 Uiso 1 1 d RD . . H17B H -0.3781 0.2437 0.7756 0.169 Uiso 1 1 d RD . . O18 O -0.037(11) 0.451(7) 0.681(5) 0.20(4) Uani 1 1 d DU . . H18A H -0.1408 0.3794 0.7087 0.294 Uiso 1 1 d RD . . H18B H 0.0037 0.4402 0.6295 0.294 Uiso 1 1 d RD . . Cd1 Cd -0.2817(4) -0.0512(2) 0.85640(17) 0.0354(12) Uani 1 1 d . . . Cd2 Cd 0.7195(4) -0.1459(3) 0.69288(19) 0.0424(13) Uani 1 1 d . . . Cd3 Cd -0.2878(4) 0.4320(2) 0.84272(17) 0.0354(12) Uani 1 1 d . . . O19 O -0.236(18) 0.255(10) 0.604(7) 0.32(7) Uani 1 1 d DU . . H19A H -0.1255 0.2704 0.6263 0.473 Uiso 1 1 d RD . . H19B H -0.2970 0.2236 0.6355 0.473 Uiso 1 1 d RD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.04(3) 0.03(3) 0.04(3) -0.01(2) -0.01(2) 0.00(2) C2 0.03(3) 0.03(2) 0.04(3) -0.02(2) 0.00(2) 0.00(2) C3 0.03(2) 0.03(2) 0.03(2) -0.01(2) -0.008(19) 0.003(19) C4 0.03(3) 0.04(3) 0.05(3) -0.02(2) 0.00(2) 0.00(2) C5 0.03(3) 0.05(3) 0.05(3) -0.02(2) 0.00(2) -0.01(2) C6 0.03(2) 0.05(3) 0.03(3) -0.02(2) -0.01(2) 0.01(2) C7 0.04(3) 0.04(3) 0.04(3) -0.02(2) -0.01(2) 0.01(2) C8 0.03(2) 0.03(2) 0.04(3) -0.01(2) -0.01(2) 0.003(19) C9 0.03(2) 0.04(3) 0.04(3) -0.02(2) 0.00(2) 0.00(2) C10 0.03(3) 0.05(3) 0.03(3) -0.01(2) 0.00(2) 0.00(2) C11 0.06(4) 0.05(3) 0.05(3) -0.02(3) -0.01(3) 0.01(3) C12 0.08(5) 0.05(4) 0.04(3) 0.00(3) -0.02(3) 0.00(3) C13 0.08(4) 0.06(4) 0.04(3) -0.01(3) -0.01(3) -0.02(3) C14 0.05(3) 0.05(3) 0.04(3) -0.02(3) 0.00(2) -0.01(3) C15 0.04(3) 0.05(3) 0.04(3) -0.02(3) -0.01(2) 0.01(2) C16 0.03(3) 0.03(3) 0.04(3) -0.01(2) 0.00(2) -0.01(2) C17 0.03(3) 0.03(2) 0.04(3) -0.01(2) 0.00(2) -0.01(2) C18 0.03(3) 0.03(2) 0.04(3) -0.01(2) -0.01(2) 0.00(2) C19 0.03(3) 0.03(3) 0.05(3) -0.01(2) -0.01(2) 0.00(2) C20 0.03(2) 0.04(3) 0.05(3) -0.02(2) 0.00(2) 0.00(2) C21 0.03(3) 0.04(3) 0.06(3) -0.01(2) 0.00(2) -0.01(2) C22 0.04(3) 0.03(3) 0.05(3) -0.02(2) 0.00(2) -0.01(2) C23 0.03(3) 0.03(3) 0.04(3) -0.01(2) -0.01(2) 0.00(2) C24 0.03(3) 0.04(3) 0.04(3) -0.01(2) 0.00(2) 0.00(2) C25 0.03(3) 0.04(3) 0.04(3) -0.02(2) 0.00(2) -0.01(2) C26 0.05(4) 0.07(4) 0.06(4) -0.02(3) -0.02(3) 0.01(3) C27 0.08(5) 0.11(6) 0.06(4) -0.03(4) -0.03(4) 0.00(5) C28 0.09(5) 0.07(4) 0.06(4) -0.04(3) 0.00(4) -0.01(4) C30 0.05(3) 0.06(4) 0.05(4) 0.00(3) 0.00(3) 0.00(3) C31 0.05(3) 0.08(4) 0.05(4) -0.03(3) -0.01(3) -0.01(3) C32 0.06(4) 0.07(4) 0.07(5) -0.02(4) -0.02(3) -0.02(3) C33 0.04(3) 0.05(3) 0.09(5) -0.01(3) 0.00(3) -0.01(3) C34 0.05(3) 0.04(3) 0.05(3) -0.01(3) 0.01(3) 0.00(2) C35 0.04(3) 0.03(2) 0.04(3) -0.01(2) 0.00(2) 0.01(2) C36 0.05(3) 0.03(2) 0.03(3) -0.01(2) 0.00(2) 0.01(2) C37 0.07(4) 0.06(4) 0.04(3) -0.01(3) 0.00(3) 0.02(3) C38 0.10(6) 0.07(4) 0.04(4) -0.02(3) -0.03(4) 0.03(4) C39 0.09(5) 0.06(4) 0.06(4) -0.02(3) -0.04(4) 0.02(4) C40 0.06(4) 0.05(3) 0.05(3) -0.02(3) -0.02(3) 0.00(3) C41 0.10(6) 0.09(6) 0.09(6) 0.01(4) -0.04(5) -0.05(5) C42 0.12(7) 0.12(7) 0.13(8) 0.01(6) -0.07(6) -0.05(6) C43 0.07(6) 0.16(12) 0.14(10) 0.06(9) -0.04(6) -0.06(7) C44 0.05(5) 0.20(12) 0.09(7) 0.04(7) 0.00(5) -0.03(6) C45 0.03(3) 0.14(7) 0.04(4) 0.02(4) 0.00(3) 0.00(4) C46 0.05(4) 0.09(5) 0.05(4) -0.01(3) -0.01(3) 0.02(4) C47 0.06(5) 0.20(11) 0.05(4) -0.02(6) -0.01(4) 0.05(6) C48 0.12(7) 0.12(7) 0.10(6) -0.06(5) -0.03(5) 0.04(6) C49 0.13(7) 0.11(6) 0.12(7) -0.07(5) -0.05(6) 0.03(5) C50 0.10(6) 0.08(5) 0.09(6) -0.06(5) -0.02(5) 0.02(5) C51 0.05(3) 0.08(4) 0.05(3) -0.02(3) 0.00(3) -0.02(3) C52 0.04(3) 0.06(4) 0.06(4) -0.02(3) -0.01(3) -0.01(3) C53 0.03(3) 0.05(3) 0.07(4) -0.01(3) 0.00(3) -0.01(2) C54 0.04(3) 0.04(3) 0.04(3) -0.01(2) 0.01(2) 0.00(2) C55 0.03(3) 0.03(2) 0.04(3) -0.01(2) 0.00(2) 0.003(19) C56 0.04(3) 0.03(2) 0.04(3) -0.01(2) 0.00(2) 0.00(2) C57 0.06(4) 0.06(3) 0.04(3) -0.01(3) 0.00(3) -0.01(3) C58 0.07(4) 0.07(4) 0.05(4) -0.02(3) -0.02(3) -0.01(3) C59 0.06(4) 0.06(4) 0.08(4) -0.03(3) -0.03(3) 0.00(3) C60 0.04(3) 0.06(3) 0.06(4) -0.03(3) -0.01(3) 0.00(2) N1 0.05(3) 0.05(3) 0.03(2) -0.02(2) -0.003(19) 0.00(2) N2 0.05(3) 0.04(2) 0.04(2) -0.011(19) -0.01(2) 0.00(2) N3 0.06(3) 0.07(3) 0.06(3) 0.00(3) -0.02(3) -0.02(3) N4 0.06(3) 0.07(3) 0.05(3) -0.03(3) -0.01(3) 0.01(3) N5 0.04(2) 0.05(3) 0.04(2) -0.02(2) 0.000(19) -0.01(2) N6 0.03(2) 0.04(2) 0.04(2) -0.020(19) -0.002(18) -0.002(17) O1 0.05(3) 0.06(3) 0.14(4) -0.06(3) 0.02(3) -0.02(2) O2 0.05(2) 0.07(3) 0.06(3) -0.03(2) 0.02(2) -0.02(2) O3 0.05(2) 0.09(3) 0.05(2) -0.04(2) 0.000(18) 0.00(2) O4 0.05(2) 0.05(2) 0.08(3) -0.04(2) -0.02(2) 0.020(19) O5 0.04(2) 0.07(2) 0.03(2) -0.019(18) -0.006(16) 0.023(18) O6 0.10(4) 0.07(3) 0.06(3) -0.03(2) -0.03(2) 0.04(3) O7 0.10(4) 0.06(3) 0.07(3) -0.04(2) -0.04(3) 0.03(3) O8 0.05(2) 0.04(2) 0.08(3) -0.03(2) 0.01(2) -0.013(17) O9 0.034(19) 0.05(2) 0.05(2) -0.016(17) 0.003(16) -0.008(16) O10 0.035(18) 0.038(18) 0.05(2) -0.021(16) -0.007(15) 0.005(15) O11 0.06(2) 0.05(2) 0.04(2) -0.023(18) -0.007(17) 0.005(18) O12 0.029(19) 0.07(3) 0.09(3) -0.05(2) -0.001(19) -0.001(17) O13 0.16(5) 0.06(3) 0.08(3) -0.01(2) -0.06(3) -0.03(3) O14 0.12(5) 0.10(4) 0.07(3) -0.03(3) -0.03(3) 0.07(4) O15 0.08(3) 0.05(2) 0.06(3) -0.012(19) -0.03(2) 0.00(2) O16 0.05(2) 0.05(2) 0.06(2) -0.017(19) -0.011(19) -0.012(18) O17 0.17(6) 0.04(3) 0.16(5) -0.03(3) -0.11(5) 0.01(3) O18 0.20(4) 0.20(4) 0.20(4) -0.062(16) -0.035(13) -0.004(11) Cd1 0.034(2) 0.038(2) 0.034(2) -0.0156(16) 0.0000(15) -0.0016(15) Cd2 0.042(2) 0.042(2) 0.045(2) -0.0194(18) -0.0059(17) 0.0037(17) Cd3 0.032(2) 0.032(2) 0.041(2) -0.0153(16) 0.0027(15) -0.0022(14) O19 0.32(7) 0.32(7) 0.32(7) -0.10(3) -0.057(17) -0.007(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 C1 O2 1.23(6) . ? C1 O1 1.25(6) . ? C1 C8 1.51(7) . ? C2 O3 1.22(6) . ? C2 O4 1.27(6) . ? C2 C3 1.52(6) . ? C3 C4 1.38(6) . ? C3 C8 1.39(6) . ? C4 C5 1.39(7) . ? C4 H4 0.9300 . ? C5 C6 1.38(7) . ? C5 H5 0.9300 . ? C6 C7 1.37(7) . ? C6 O5 1.40(5) . ? C7 C8 1.40(6) . ? C7 H7 0.9300 . ? C9 C14 1.38(7) . ? C9 C10 1.42(7) . ? C9 C15 1.50(7) . ? C10 O5 1.36(6) . ? C10 C11 1.39(7) . ? C11 C12 1.37(8) . ? C11 H11 0.9300 . ? C12 C13 1.38(8) . ? C12 H12 0.9300 . ? C13 C14 1.37(8) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 O7 1.22(6) . ? C15 O6 1.27(6) . ? C15 Cd2 2.71(5) . ? C16 O9 1.24(5) . ? C16 O8 1.26(6) . ? C16 C18 1.51(6) . ? C17 O11 1.23(6) . ? C17 O10 1.27(6) . ? C17 C23 1.51(6) . ? C18 C19 1.39(6) . ? C18 C23 1.41(6) . ? C19 C20 1.38(7) . ? C19 H19 0.9300 . ? C20 C21 1.36(7) . ? C20 O12 1.40(6) . ? C21 C22 1.37(7) . ? C21 H21 0.9300 . ? C22 C23 1.38(6) . ? C22 H22 0.9300 . ? C24 C25 1.38(7) . ? C24 C29 1.39(7) . ? C24 C30 1.51(8) . ? C25 C26 1.37(8) . ? C25 O12 1.38(6) . ? C26 C27 1.37(9) . ? C26 H26 0.9300 . ? C27 C28 1.38(9) . ? C27 H27 0.9300 . ? C28 C29 1.37(9) . ? C28 H28 0.9300 . ? C30 O13 1.22(7) . ? C30 O14 1.23(7) . ? C31 N1 1.33(7) . ? C31 C32 1.39(8) . ? C31 H31 0.9300 . ? C32 C33 1.37(9) . ? C32 H32 0.9300 . ? C33 C34 1.38(9) . ? C33 H33 0.9300 . ? C34 C35 1.38(7) . ? C34 H34 0.9300 . ? C35 N1 1.36(6) . ? C35 C36 1.47(7) . ? C36 N2 1.36(6) . ? C36 C37 1.39(7) . ? C37 C38 1.40(9) . ? C37 H37 0.9300 . ? C38 C39 1.37(10) . ? C38 H38 0.9300 . ? C39 C40 1.37(8) . ? C39 H39 0.9300 . ? C40 N2 1.34(7) . ? C40 H40 0.9300 . ? C41 N3 1.31(9) . ? C41 C42 1.41(13) . ? C41 H41 0.9300 . ? C42 C43 1.36(16) . ? C42 H42 0.9300 . ? C43 C44 1.34(18) . ? C43 H43 0.9300 . ? C44 C45 1.40(11) . ? C44 H44 0.9300 . ? C45 N3 1.39(9) . ? C45 C46 1.49(11) . ? C46 N4 1.30(8) . ? C46 C47 1.46(11) . ? C47 C48 1.35(14) . ? C47 H47 0.9300 . ? C48 C49 1.34(13) . ? C48 H48 0.9300 . ? C49 C50 1.39(10) . ? C49 H49 0.9300 . ? C50 N4 1.33(9) . ? C50 H50 0.9300 . ? C51 N5 1.34(7) . ? C51 C52 1.38(8) . ? C51 H51 0.9300 . ? C52 C53 1.35(8) . ? C52 H52 0.9300 . ? C53 C54 1.38(8) . ? C53 H53 0.9300 . ? C54 C55 1.39(7) . ? C54 H54 0.9300 . ? C55 N5 1.35(6) . ? C55 C56 1.49(7) . ? C56 N6 1.35(6) . ? C56 C57 1.39(7) . ? C57 C58 1.38(8) . ? C57 H57 0.9300 . ? C58 C59 1.38(9) . ? C58 H58 0.9300 . ? C59 C60 1.36(8) . ? C59 H59 0.9300 . ? C60 N6 1.33(7) . ? C60 H60 0.9300 . ? C29 H29 0.9300 . ? N1 Cd1 2.35(4) . ? N2 Cd1 2.29(4) . ? N3 Cd2 2.32(5) . ? N4 Cd2 2.29(5) . ? N5 Cd3 2.34(4) . ? N6 Cd3 2.37(4) . ? O1 Cd1 2.26(4) . ? O4 Cd3 2.23(3) . ? O6 Cd2 2.28(4) . ? O7 Cd2 2.44(4) . ? O8 Cd3 2.24(4) . ? O10 Cd2 2.25(3) 1_465 ? O10 Cd1 2.39(3) 1_565 ? O11 Cd1 2.51(4) 1_565 ? O13 Cd3 2.52(5) 1_655 ? O14 Cd3 2.50(5) 1_655 ? O15 Cd1 2.28(4) . ? O15 H15B 0.8621 . ? O15 H15C 0.8727 . ? O16 Cd2 2.27(4) . ? O16 H16A 0.8522 . ? O16 H16B 0.8584 . ? Cd1 O10 2.39(3) 1_545 ? Cd1 O11 2.51(4) 1_545 ? Cd2 O10 2.25(3) 1_645 ? Cd3 O14 2.50(5) 1_455 ? Cd3 O13 2.52(5) 1_455 ? 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 C1 O1 122(5) . . ? O2 C1 C8 121(4) . . ? O1 C1 C8 117(4) . . ? O3 C2 O4 125(5) . . ? O3 C2 C3 119(4) . . ? O4 C2 C3 116(4) . . ? C4 C3 C8 119(4) . . ? C4 C3 C2 116(4) . . ? C8 C3 C2 124(4) . . ? C3 C4 C5 122(4) . . ? C3 C4 H4 119.1 . . ? C5 C4 H4 119.1 . . ? C6 C5 C4 118(5) . . ? C6 C5 H5 120.8 . . ? C4 C5 H5 120.8 . . ? C7 C6 C5 121(4) . . ? C7 C6 O5 118(4) . . ? C5 C6 O5 121(5) . . ? C6 C7 C8 120(4) . . ? C6 C7 H7 119.9 . . ? C8 C7 H7 119.9 . . ? C3 C8 C7 119(4) . . ? C3 C8 C1 123(4) . . ? C7 C8 C1 118(4) . . ? C14 C9 C10 117(5) . . ? C14 C9 C15 119(4) . . ? C10 C9 C15 124(4) . . ? O5 C10 C11 123(5) . . ? O5 C10 C9 118(4) . . ? C11 C10 C9 119(5) . . ? C12 C11 C10 121(5) . . ? C12 C11 H11 119.7 . . ? C10 C11 H11 119.7 . . ? C11 C12 C13 121(6) . . ? C11 C12 H12 119.6 . . ? C13 C12 H12 119.6 . . ? C14 C13 C12 119(5) . . ? C14 C13 H13 120.7 . . ? C12 C13 H13 120.7 . . ? C13 C14 C9 123(5) . . ? C13 C14 H14 118.3 . . ? C9 C14 H14 118.3 . . ? O7 C15 O6 120(5) . . ? O7 C15 C9 119(5) . . ? O6 C15 C9 121(4) . . ? O7 C15 Cd2 64(3) . . ? O6 C15 Cd2 57(3) . . ? C9 C15 Cd2 169(4) . . ? O9 C16 O8 124(4) . . ? O9 C16 C18 119(4) . . ? O8 C16 C18 116(4) . . ? O11 C17 O10 123(4) . . ? O11 C17 C23 117(5) . . ? O10 C17 C23 119(4) . . ? C19 C18 C23 118(4) . . ? C19 C18 C16 120(4) . . ? C23 C18 C16 122(4) . . ? C20 C19 C18 121(4) . . ? C20 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? C21 C20 C19 121(4) . . ? C21 C20 O12 116(4) . . ? C19 C20 O12 122(4) . . ? C20 C21 C22 119(5) . . ? C20 C21 H21 120.6 . . ? C22 C21 H21 120.6 . . ? C21 C22 C23 122(4) . . ? C21 C22 H22 118.9 . . ? C23 C22 H22 118.9 . . ? C22 C23 C18 119(4) . . ? C22 C23 C17 116(4) . . ? C18 C23 C17 126(4) . . ? C25 C24 C29 117(5) . . ? C25 C24 C30 125(5) . . ? C29 C24 C30 118(5) . . ? C26 C25 O12 119(5) . . ? C26 C25 C24 122(5) . . ? O12 C25 C24 119(5) . . ? C25 C26 C27 120(6) . . ? C25 C26 H26 120.2 . . ? C27 C26 H26 120.2 . . ? C26 C27 C28 120(6) . . ? C26 C27 H27 119.8 . . ? C28 C27 H27 119.8 . . ? C29 C28 C27 119(6) . . ? C29 C28 H28 120.3 . . ? C27 C28 H28 120.3 . . ? O13 C30 O14 121(6) . . ? O13 C30 C24 123(6) . . ? O14 C30 C24 116(6) . . ? N1 C31 C32 123(6) . . ? N1 C31 H31 118.3 . . ? C32 C31 H31 118.3 . . ? C33 C32 C31 117(6) . . ? C33 C32 H32 121.3 . . ? C31 C32 H32 121.3 . . ? C32 C33 C34 120(5) . . ? C32 C33 H33 120.0 . . ? C34 C33 H33 120.0 . . ? C33 C34 C35 120(5) . . ? C33 C34 H34 120.1 . . ? C35 C34 H34 120.1 . . ? N1 C35 C34 121(5) . . ? N1 C35 C36 117(4) . . ? C34 C35 C36 123(5) . . ? N2 C36 C37 120(5) . . ? N2 C36 C35 117(4) . . ? C37 C36 C35 123(5) . . ? C36 C37 C38 119(6) . . ? C36 C37 H37 120.3 . . ? C38 C37 H37 120.3 . . ? C39 C38 C37 119(6) . . ? C39 C38 H38 120.5 . . ? C37 C38 H38 120.5 . . ? C38 C39 C40 119(6) . . ? C38 C39 H39 120.3 . . ? C40 C39 H39 120.3 . . ? N2 C40 C39 122(6) . . ? N2 C40 H40 118.9 . . ? C39 C40 H40 118.9 . . ? N3 C41 C42 120(10) . . ? N3 C41 H41 119.9 . . ? C42 C41 H41 119.9 . . ? C43 C42 C41 119(10) . . ? C43 C42 H42 120.7 . . ? C41 C42 H42 120.7 . . ? C44 C43 C42 121(10) . . ? C44 C43 H43 119.5 . . ? C42 C43 H43 119.5 . . ? C43 C44 C45 121(10) . . ? C43 C44 H44 119.4 . . ? C45 C44 H44 119.4 . . ? N3 C45 C44 117(10) . . ? N3 C45 C46 118(5) . . ? C44 C45 C46 126(9) . . ? N4 C46 C47 121(9) . . ? N4 C46 C45 116(6) . . ? C47 C46 C45 122(8) . . ? C48 C47 C46 116(9) . . ? C48 C47 H47 122.0 . . ? C46 C47 H47 122.0 . . ? C49 C48 C47 124(9) . . ? C49 C48 H48 117.8 . . ? C47 C48 H48 117.8 . . ? C48 C49 C50 115(10) . . ? C48 C49 H49 122.7 . . ? C50 C49 H49 122.7 . . ? N4 C50 C49 126(9) . . ? N4 C50 H50 117.1 . . ? C49 C50 H50 117.1 . . ? N5 C51 C52 124(5) . . ? N5 C51 H51 118.1 . . ? C52 C51 H51 118.1 . . ? C53 C52 C51 118(5) . . ? C53 C52 H52 120.9 . . ? C51 C52 H52 120.9 . . ? C52 C53 C54 120(5) . . ? C52 C53 H53 120.0 . . ? C54 C53 H53 120.0 . . ? C53 C54 C55 119(5) . . ? C53 C54 H54 120.5 . . ? C55 C54 H54 120.5 . . ? N5 C55 C54 121(5) . . ? N5 C55 C56 116(4) . . ? C54 C55 C56 122(5) . . ? N6 C56 C57 121(5) . . ? N6 C56 C55 116(4) . . ? C57 C56 C55 122(5) . . ? C58 C57 C56 119(5) . . ? C58 C57 H57 120.3 . . ? C56 C57 H57 120.3 . . ? C59 C58 C57 119(6) . . ? C59 C58 H58 120.6 . . ? C57 C58 H58 120.6 . . ? C60 C59 C58 119(6) . . ? C60 C59 H59 120.4 . . ? C58 C59 H59 120.4 . . ? N6 C60 C59 123(5) . . ? N6 C60 H60 118.3 . . ? C59 C60 H60 118.3 . . ? C28 C29 C24 122(6) . . ? C28 C29 H29 119.1 . . ? C24 C29 H29 119.1 . . ? C31 N1 C35 119(5) . . ? C31 N1 Cd1 124(4) . . ? C35 N1 Cd1 117(3) . . ? C40 N2 C36 120(5) . . ? C40 N2 Cd1 121(4) . . ? C36 N2 Cd1 119(3) . . ? C41 N3 C45 122(7) . . ? C41 N3 Cd2 124(6) . . ? C45 N3 Cd2 114(5) . . ? C46 N4 C50 118(6) . . ? C46 N4 Cd2 118(5) . . ? C50 N4 Cd2 123(5) . . ? C51 N5 C55 118(4) . . ? C51 N5 Cd3 123(4) . . ? C55 N5 Cd3 119(3) . . ? C60 N6 C56 118(5) . . ? C60 N6 Cd3 124(3) . . ? C56 N6 Cd3 118(3) . . ? C1 O1 Cd1 103(3) . . ? C2 O4 Cd3 118(3) . . ? C10 O5 C6 118(4) . . ? C15 O6 Cd2 95(3) . . ? C15 O7 Cd2 89(3) . . ? C16 O8 Cd3 116(3) . . ? C17 O10 Cd2 131(3) . 1_465 ? C17 O10 Cd1 93(3) . 1_565 ? Cd2 O10 Cd1 135.1(14) 1_465 1_565 ? C17 O11 Cd1 89(3) . 1_565 ? C25 O12 C20 120(4) . . ? C30 O13 Cd3 94(4) . 1_655 ? C30 O14 Cd3 95(5) . 1_655 ? Cd1 O15 H15B 120.5 . . ? Cd1 O15 H15C 126.2 . . ? H15B O15 H15C 108.9 . . ? Cd2 O16 H16A 142.3 . . ? Cd2 O16 H16B 107.6 . . ? H16A O16 H16B 108.4 . . ? H17A O17 H17B 110.5 . . ? H18A O18 H18B 99.8 . . ? O1 Cd1 O15 90.3(18) . . ? O1 Cd1 N2 113.4(18) . . ? O15 Cd1 N2 128.6(15) . . ? O1 Cd1 N1 174.1(17) . . ? O15 Cd1 N1 83.9(15) . . ? N2 Cd1 N1 70.9(15) . . ? O1 Cd1 O10 83.7(13) . 1_545 ? O15 Cd1 O10 93.0(13) . 1_545 ? N2 Cd1 O10 132.7(13) . 1_545 ? N1 Cd1 O10 96.3(13) . 1_545 ? O1 Cd1 O11 78.3(14) . 1_545 ? O15 Cd1 O11 144.9(13) . 1_545 ? N2 Cd1 O11 86.1(13) . 1_545 ? N1 Cd1 O11 106.5(14) . 1_545 ? O10 Cd1 O11 53.1(11) 1_545 1_545 ? O10 Cd2 O16 81.5(13) 1_645 . ? O10 Cd2 O6 91.1(13) 1_645 . ? O16 Cd2 O6 104.9(16) . . ? O10 Cd2 N4 120.3(15) 1_645 . ? O16 Cd2 N4 95.9(17) . . ? O6 Cd2 N4 144.7(16) . . ? O10 Cd2 N3 91.2(16) 1_645 . ? O16 Cd2 N3 160.5(17) . . ? O6 Cd2 N3 93(2) . . ? N4 Cd2 N3 72(2) . . ? O10 Cd2 O7 145.4(12) 1_645 . ? O16 Cd2 O7 107.0(16) . . ? O6 Cd2 O7 54.3(13) . . ? N4 Cd2 O7 92.7(16) . . ? N3 Cd2 O7 89.3(17) . . ? O10 Cd2 C15 118.6(13) 1_645 . ? O16 Cd2 C15 110.8(15) . . ? O6 Cd2 C15 27.7(14) . . ? N4 Cd2 C15 117.8(17) . . ? N3 Cd2 C15 88.6(17) . . ? O7 Cd2 C15 26.8(13) . . ? O4 Cd3 O8 89.6(14) . . ? O4 Cd3 N5 115.9(15) . . ? O8 Cd3 N5 153.1(14) . . ? O4 Cd3 N6 111.8(14) . . ? O8 Cd3 N6 93.8(15) . . ? N5 Cd3 N6 69.6(14) . . ? O4 Cd3 O14 73.7(14) . 1_455 ? O8 Cd3 O14 111.9(18) . 1_455 ? N5 Cd3 O14 85.0(17) . 1_455 ? N6 Cd3 O14 154.0(18) . 1_455 ? O4 Cd3 O13 118.7(17) . 1_455 ? O8 Cd3 O13 90.3(17) . 1_455 ? N5 Cd3 O13 84.9(18) . 1_455 ? N6 Cd3 O13 129.3(16) . 1_455 ? O14 Cd3 O13 50.2(15) 1_455 1_455 ? H19A O19 H19B 109.6 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.540 _refine_diff_density_min -0.775 _refine_diff_density_rms 0.099 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 746379' #TrackingRef 'complexes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H38 Cd3 N4 O18' _chemical_formula_weight 1320.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M c2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.8380(15) _cell_length_b 10.485(2) _cell_length_c 22.5800(10) _cell_angle_alpha 90.00 _cell_angle_beta 102.9680(10) _cell_angle_gamma 90.00 _cell_volume 4807.6(10) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 7929 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 27.58 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.824 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2616 _exptl_absorpt_coefficient_mu 1.398 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7870 _exptl_absorpt_correction_T_max 0.8502 _exptl_absorpt_process_details '(SADABS; Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 0 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 11619 _diffrn_reflns_av_R_equivalents 0.0191 _diffrn_reflns_av_sigmaI/netI 0.0227 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4246 _reflns_number_gt 3850 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'SAINT-Plus (Bruker, 2001)' _computing_data_reduction SAINT-Plus _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Sheldrick, 1998)' _computing_publication_material XP _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^)+(0.0335P)^2^+5.8955P] 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 4246 _refine_ls_number_parameters 339 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0264 _refine_ls_R_factor_gt 0.0234 _refine_ls_wR_factor_ref 0.0635 _refine_ls_wR_factor_gt 0.0619 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.02154(12) 0.1970(2) -0.02796(11) 0.0290(6) Uani 1 1 d . . . C2 C 0.02178(13) 0.1598(3) -0.16233(11) 0.0296(6) Uani 1 1 d . . . C3 C -0.01040(12) 0.2888(2) -0.07665(11) 0.0275(5) Uani 1 1 d . . . C5 C -0.04683(12) 0.3530(2) -0.18161(11) 0.0290(5) Uani 1 1 d . . . H5 H -0.0482 0.3398 -0.2226 0.035 Uiso 1 1 calc R . . C6 C -0.07944(13) 0.4556(2) -0.16385(12) 0.0308(6) Uani 1 1 d . . . C7 C -0.07705(15) 0.4789(3) -0.10331(13) 0.0403(7) Uani 1 1 d . . . H7 H -0.0982 0.5495 -0.0915 0.048 Uiso 1 1 calc R . . C8 C -0.04265(15) 0.3952(3) -0.06046(12) 0.0370(6) Uani 1 1 d . . . H8 H -0.0410 0.4104 -0.0196 0.044 Uiso 1 1 calc R . . C9 C -0.16464(13) 0.6056(2) -0.20137(12) 0.0292(6) Uani 1 1 d . . . C10 C -0.21998(15) 0.5467(3) -0.19058(13) 0.0399(7) Uani 1 1 d . . . H10 H -0.2199 0.4591 -0.1841 0.048 Uiso 1 1 calc R . . C11 C -0.27561(15) 0.6175(3) -0.18937(14) 0.0447(7) Uani 1 1 d . . . H11 H -0.3131 0.5775 -0.1824 0.054 Uiso 1 1 calc R . . C12 C -0.27547(14) 0.7475(3) -0.19856(14) 0.0421(7) Uani 1 1 d . . . H12 H -0.3127 0.7956 -0.1976 0.051 Uiso 1 1 calc R . . C13 C -0.21980(13) 0.8062(3) -0.20918(12) 0.0336(6) Uani 1 1 d . . . H13 H -0.2199 0.8939 -0.2153 0.040 Uiso 1 1 calc R . . C14 C -0.16357(12) 0.7358(2) -0.21090(11) 0.0260(5) Uani 1 1 d . . . C15 C -0.10328(12) 0.7998(2) -0.22218(11) 0.0278(5) Uani 1 1 d . . . C16 C 0.16416(13) 0.0352(3) 0.06309(13) 0.0390(7) Uani 1 1 d . . . H16 H 0.1491 0.1022 0.0367 0.047 Uiso 1 1 calc R . . C17 C 0.22370(13) -0.0203(3) 0.06098(13) 0.0413(7) Uani 1 1 d . . . H17 H 0.2486 0.0111 0.0348 0.050 Uiso 1 1 calc R . . C18 C 0.24591(12) -0.1233(3) 0.09837(12) 0.0319(6) Uani 1 1 d . . . C19 C 0.20849(13) -0.1597(3) 0.13889(13) 0.0362(6) Uani 1 1 d . . . H19 H 0.2225 -0.2261 0.1660 0.043 Uiso 1 1 calc R . . C20 C 0.15037(13) -0.0972(3) 0.13901(13) 0.0348(6) Uani 1 1 d . . . H20 H 0.1262 -0.1224 0.1670 0.042 Uiso 1 1 calc R . . C21 C -0.07726(13) 0.3057(3) 0.09864(15) 0.0433(7) Uani 1 1 d . . . H21 H -0.0379 0.3500 0.1025 0.052 Uiso 1 1 calc R . . C22 C -0.13342(14) 0.3739(3) 0.09986(15) 0.0434(7) Uani 1 1 d . . . H22 H -0.1320 0.4623 0.1033 0.052 Uiso 1 1 calc R . . C23 C -0.19235(12) 0.3088(3) 0.09593(12) 0.0333(6) Uani 1 1 d . . . C24 C -0.19133(13) 0.1780(3) 0.08930(13) 0.0385(6) Uani 1 1 d . . . H24 H -0.2298 0.1309 0.0862 0.046 Uiso 1 1 calc R . . C25 C -0.13303(13) 0.1172(3) 0.08735(13) 0.0365(6) Uani 1 1 d . . . H25 H -0.1333 0.0292 0.0824 0.044 Uiso 1 1 calc R . . N1 N 0.12726(10) -0.0024(2) 0.10093(9) 0.0292(5) Uani 1 1 d . . . N2 N -0.07656(10) 0.1796(2) 0.09219(10) 0.0328(5) Uani 1 1 d . . . O1 O -0.01264(8) 0.05817(17) -0.17523(7) 0.0315(4) Uani 1 1 d . . . O2 O 0.07646(10) 0.1758(2) -0.17209(12) 0.0572(6) Uani 1 1 d . . . O3 O 0.03389(10) 0.08576(17) -0.04233(9) 0.0373(5) Uani 1 1 d . . . O4 O 0.03403(10) 0.23652(18) 0.02619(8) 0.0374(4) Uani 1 1 d . . . O5 O -0.11150(10) 0.53432(18) -0.21025(8) 0.0380(5) Uani 1 1 d . . . O6 O -0.05029(8) 0.79112(17) -0.18200(8) 0.0334(4) Uani 1 1 d . . . O7 O -0.10712(10) 0.8610(2) -0.27007(9) 0.0435(5) Uani 1 1 d . . . O8 O 0.1994(4) 0.3696(6) 0.0395(3) 0.211(3) Uani 1 1 d D . . H8A H 0.1754 0.3049 0.0416 0.317 Uiso 1 1 d RD . . H8B H 0.2249 0.3800 0.0742 0.317 Uiso 1 1 d RD . . O9 O 0.1751(2) 0.2441(6) -0.0634(2) 0.170(2) Uani 1 1 d D . . H9A H 0.1483 0.2166 -0.0950 0.254 Uiso 1 1 d RD . . H9B H 0.1555 0.3006 -0.0474 0.254 Uiso 1 1 d RD . . Cd1 Cd 0.0000 -0.07003(2) -0.2500 0.02788(8) Uani 1 2 d S . . Cd2 Cd 0.023590(8) 0.080798(17) 0.093132(8) 0.02637(7) Uani 1 1 d . . . C4 C -0.01194(12) 0.2694(2) -0.13840(11) 0.0261(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0242(12) 0.0338(15) 0.0289(14) 0.0019(11) 0.0059(10) 0.0033(11) C2 0.0320(14) 0.0294(14) 0.0296(13) 0.0047(11) 0.0116(11) 0.0077(11) C3 0.0285(13) 0.0255(13) 0.0284(13) 0.0005(10) 0.0058(10) 0.0035(10) C5 0.0329(14) 0.0272(13) 0.0282(13) 0.0012(10) 0.0099(11) 0.0031(11) C6 0.0319(14) 0.0254(13) 0.0348(14) 0.0048(11) 0.0065(11) 0.0039(11) C7 0.0525(18) 0.0300(15) 0.0385(16) -0.0038(12) 0.0103(13) 0.0167(13) C8 0.0469(16) 0.0366(15) 0.0265(14) -0.0047(11) 0.0063(12) 0.0110(13) C9 0.0328(14) 0.0247(13) 0.0305(13) 0.0038(10) 0.0075(11) 0.0051(11) C10 0.0463(17) 0.0290(15) 0.0451(17) 0.0048(12) 0.0119(13) -0.0070(13) C11 0.0333(15) 0.0525(19) 0.0500(18) 0.0056(15) 0.0129(13) -0.0105(14) C12 0.0257(14) 0.0518(19) 0.0496(18) -0.0011(14) 0.0101(13) 0.0054(13) C13 0.0304(14) 0.0295(14) 0.0399(15) 0.0023(11) 0.0060(11) 0.0039(11) C14 0.0244(12) 0.0264(13) 0.0263(12) 0.0014(10) 0.0040(10) 0.0006(10) C15 0.0272(13) 0.0270(13) 0.0304(14) -0.0024(11) 0.0090(11) 0.0010(10) C16 0.0285(14) 0.0487(17) 0.0414(16) 0.0153(13) 0.0113(12) 0.0169(13) C17 0.0299(14) 0.0546(19) 0.0439(16) 0.0149(14) 0.0177(12) 0.0134(13) C18 0.0228(12) 0.0359(15) 0.0365(14) -0.0003(12) 0.0055(11) 0.0078(11) C19 0.0287(14) 0.0339(15) 0.0477(16) 0.0123(13) 0.0123(12) 0.0096(12) C20 0.0263(13) 0.0374(15) 0.0429(16) 0.0058(12) 0.0124(12) 0.0052(11) C21 0.0249(14) 0.0370(17) 0.070(2) -0.0006(14) 0.0143(14) 0.0027(12) C22 0.0339(15) 0.0304(15) 0.068(2) -0.0001(14) 0.0158(14) 0.0082(12) C23 0.0229(13) 0.0402(16) 0.0372(15) 0.0027(12) 0.0075(11) 0.0105(11) C24 0.0254(13) 0.0375(16) 0.0525(17) -0.0026(13) 0.0086(12) 0.0026(12) C25 0.0287(14) 0.0325(15) 0.0476(17) -0.0026(12) 0.0073(12) 0.0065(12) N1 0.0209(10) 0.0339(12) 0.0335(12) 0.0030(9) 0.0073(9) 0.0084(9) N2 0.0231(11) 0.0348(13) 0.0407(13) 0.0010(10) 0.0076(9) 0.0091(9) O1 0.0401(11) 0.0255(10) 0.0331(10) -0.0035(7) 0.0168(9) 0.0025(8) O2 0.0385(12) 0.0526(14) 0.0927(18) -0.0056(12) 0.0403(12) 0.0035(10) O3 0.0377(11) 0.0291(10) 0.0400(11) -0.0013(8) -0.0021(9) 0.0089(8) O4 0.0450(11) 0.0399(11) 0.0270(10) 0.0010(8) 0.0076(8) 0.0079(9) O5 0.0476(11) 0.0308(10) 0.0383(11) 0.0105(8) 0.0155(9) 0.0160(9) O6 0.0255(9) 0.0349(10) 0.0379(10) -0.0019(8) 0.0027(8) 0.0017(8) O7 0.0409(11) 0.0527(13) 0.0364(11) 0.0122(10) 0.0076(9) -0.0110(10) O8 0.280(8) 0.194(6) 0.192(6) -0.022(5) 0.121(6) -0.021(6) O9 0.138(4) 0.251(6) 0.126(4) -0.054(4) 0.042(3) -0.081(4) Cd1 0.03100(15) 0.02747(15) 0.02982(15) 0.000 0.01667(11) 0.000 Cd2 0.02058(11) 0.03063(12) 0.02863(12) 0.00204(7) 0.00708(8) 0.00887(7) C4 0.0242(12) 0.0232(12) 0.0323(13) -0.0003(10) 0.0094(10) 0.0006(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O3 1.253(3) . ? C1 O4 1.261(3) . ? C1 C3 1.500(3) . ? C2 O2 1.220(3) . ? C2 O1 1.281(3) . ? C2 C4 1.509(3) . ? C3 C8 1.393(4) . ? C3 C4 1.402(3) . ? C5 C6 1.379(4) . ? C5 C4 1.389(3) . ? C5 H5 0.9300 . ? C6 C7 1.378(4) . ? C6 O5 1.382(3) . ? C7 C8 1.381(4) . ? C7 H7 0.9300 . ? C8 H8 0.9300 . ? C9 C10 1.377(4) . ? C9 C14 1.382(4) . ? C9 O5 1.388(3) . ? C10 C11 1.382(4) . ? C10 H10 0.9300 . ? C11 C12 1.379(4) . ? C11 H11 0.9300 . ? C12 C13 1.380(4) . ? C12 H12 0.9300 . ? C13 C14 1.393(4) . ? C13 H13 0.9300 . ? C14 C15 1.496(3) . ? C15 O7 1.244(3) . ? C15 O6 1.265(3) . ? C15 Cd1 2.738(3) 1_565 ? C16 N1 1.331(3) . ? C16 C17 1.381(4) . ? C16 H16 0.9300 . ? C17 C18 1.385(4) . ? C17 H17 0.9300 . ? C18 C19 1.382(4) . ? C18 C23 1.482(3) 3_545 ? C19 C20 1.377(4) . ? C19 H19 0.9300 . ? C20 N1 1.332(3) . ? C20 H20 0.9300 . ? C21 N2 1.331(4) . ? C21 C22 1.377(4) . ? C21 H21 0.9300 . ? C22 C23 1.390(4) . ? C22 H22 0.9300 . ? C23 C24 1.381(4) . ? C23 C18 1.482(3) 3_455 ? C24 C25 1.381(4) . ? C24 H24 0.9300 . ? C25 N2 1.329(3) . ? C25 H25 0.9300 . ? N1 Cd2 2.2993(19) . ? N2 Cd2 2.326(2) . ? O1 Cd1 2.2195(17) . ? O1 Cd2 2.4086(17) 5 ? O3 Cd2 2.2768(19) 5 ? O4 Cd2 2.2685(19) . ? O6 Cd2 2.3745(18) 5_565 ? O6 Cd1 2.5095(19) 1_565 ? O7 Cd1 2.2928(19) 1_565 ? O8 H8A 0.8501 . ? O8 H8B 0.8501 . ? O9 H9A 0.8516 . ? O9 H9B 0.8471 . ? Cd1 O1 2.2195(17) 2_554 ? Cd1 O7 2.2928(19) 2_544 ? Cd1 O7 2.2928(19) 1_545 ? Cd1 O6 2.5095(19) 2_544 ? Cd1 O6 2.5095(19) 1_545 ? Cd1 C15 2.738(3) 2_544 ? Cd1 C15 2.738(3) 1_545 ? Cd2 O3 2.2768(19) 5 ? Cd2 O6 2.3745(18) 5_565 ? Cd2 O1 2.4086(17) 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 O3 C1 O4 123.1(2) . . ? O3 C1 C3 119.4(2) . . ? O4 C1 C3 117.4(2) . . ? O2 C2 O1 124.8(2) . . ? O2 C2 C4 119.3(2) . . ? O1 C2 C4 115.7(2) . . ? C8 C3 C4 118.2(2) . . ? C8 C3 C1 118.9(2) . . ? C4 C3 C1 122.9(2) . . ? C6 C5 C4 120.2(2) . . ? C6 C5 H5 119.9 . . ? C4 C5 H5 119.9 . . ? C7 C6 C5 121.0(2) . . ? C7 C6 O5 123.4(2) . . ? C5 C6 O5 115.5(2) . . ? C6 C7 C8 118.7(2) . . ? C6 C7 H7 120.7 . . ? C8 C7 H7 120.7 . . ? C7 C8 C3 122.0(3) . . ? C7 C8 H8 119.0 . . ? C3 C8 H8 119.0 . . ? C10 C9 C14 120.9(2) . . ? C10 C9 O5 120.7(2) . . ? C14 C9 O5 117.9(2) . . ? C9 C10 C11 120.1(3) . . ? C9 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? C12 C11 C10 119.8(3) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? C11 C12 C13 119.8(3) . . ? C11 C12 H12 120.1 . . ? C13 C12 H12 120.1 . . ? C12 C13 C14 120.9(3) . . ? C12 C13 H13 119.5 . . ? C14 C13 H13 119.5 . . ? C9 C14 C13 118.4(2) . . ? C9 C14 C15 120.9(2) . . ? C13 C14 C15 120.8(2) . . ? O7 C15 O6 122.4(2) . . ? O7 C15 C14 119.1(2) . . ? O6 C15 C14 118.5(2) . . ? O7 C15 Cd1 56.23(13) . 1_565 ? O6 C15 Cd1 66.16(14) . 1_565 ? C14 C15 Cd1 175.05(18) . 1_565 ? N1 C16 C17 123.4(3) . . ? N1 C16 H16 118.3 . . ? C17 C16 H16 118.3 . . ? C16 C17 C18 119.2(3) . . ? C16 C17 H17 120.4 . . ? C18 C17 H17 120.4 . . ? C19 C18 C17 117.2(2) . . ? C19 C18 C23 121.0(2) . 3_545 ? C17 C18 C23 121.7(2) . 3_545 ? C20 C19 C18 119.8(2) . . ? C20 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? N1 C20 C19 123.0(3) . . ? N1 C20 H20 118.5 . . ? C19 C20 H20 118.5 . . ? N2 C21 C22 123.2(3) . . ? N2 C21 H21 118.4 . . ? C22 C21 H21 118.4 . . ? C21 C22 C23 119.1(3) . . ? C21 C22 H22 120.4 . . ? C23 C22 H22 120.4 . . ? C24 C23 C22 117.4(2) . . ? C24 C23 C18 121.1(2) . 3_455 ? C22 C23 C18 121.6(3) . 3_455 ? C23 C24 C25 119.8(3) . . ? C23 C24 H24 120.1 . . ? C25 C24 H24 120.1 . . ? N2 C25 C24 122.7(3) . . ? N2 C25 H25 118.7 . . ? C24 C25 H25 118.7 . . ? C16 N1 C20 117.2(2) . . ? C16 N1 Cd2 120.48(17) . . ? C20 N1 Cd2 121.99(17) . . ? C25 N2 C21 117.8(2) . . ? C25 N2 Cd2 123.92(18) . . ? C21 N2 Cd2 118.24(17) . . ? C2 O1 Cd1 121.38(15) . . ? C2 O1 Cd2 118.24(15) . 5 ? Cd1 O1 Cd2 105.48(7) . 5 ? C1 O3 Cd2 136.82(17) . 5 ? C1 O4 Cd2 112.33(17) . . ? C6 O5 C9 118.5(2) . . ? C15 O6 Cd2 124.51(16) . 5_565 ? C15 O6 Cd1 86.37(15) . 1_565 ? Cd2 O6 Cd1 97.94(6) 5_565 1_565 ? C15 O7 Cd1 96.96(16) . 1_565 ? H8A O8 H8B 107.7 . . ? H9A O9 H9B 107.8 . . ? O1 Cd1 O1 105.45(9) . 2_554 ? O1 Cd1 O7 108.49(6) . 2_544 ? O1 Cd1 O7 93.73(7) 2_554 2_544 ? O1 Cd1 O7 93.73(7) . 1_545 ? O1 Cd1 O7 108.49(6) 2_554 1_545 ? O7 Cd1 O7 143.21(11) 2_544 1_545 ? O1 Cd1 O6 162.54(6) . 2_544 ? O1 Cd1 O6 75.45(6) 2_554 2_544 ? O7 Cd1 O6 54.28(6) 2_544 2_544 ? O7 Cd1 O6 102.57(7) 1_545 2_544 ? O1 Cd1 O6 75.45(6) . 1_545 ? O1 Cd1 O6 162.54(6) 2_554 1_545 ? O7 Cd1 O6 102.57(7) 2_544 1_545 ? O7 Cd1 O6 54.28(6) 1_545 1_545 ? O6 Cd1 O6 109.08(8) 2_544 1_545 ? O1 Cd1 C15 135.24(7) . 2_544 ? O1 Cd1 C15 83.90(7) 2_554 2_544 ? O7 Cd1 C15 26.82(7) 2_544 2_544 ? O7 Cd1 C15 125.30(8) 1_545 2_544 ? O6 Cd1 C15 27.47(6) 2_544 2_544 ? O6 Cd1 C15 107.99(6) 1_545 2_544 ? O1 Cd1 C15 83.90(7) . 1_545 ? O1 Cd1 C15 135.24(7) 2_554 1_545 ? O7 Cd1 C15 125.30(8) 2_544 1_545 ? O7 Cd1 C15 26.82(7) 1_545 1_545 ? O6 Cd1 C15 107.99(7) 2_544 1_545 ? O6 Cd1 C15 27.47(6) 1_545 1_545 ? C15 Cd1 C15 120.19(10) 2_544 1_545 ? O4 Cd2 O3 109.55(7) . 5 ? O4 Cd2 N1 95.45(7) . . ? O3 Cd2 N1 97.28(7) 5 . ? O4 Cd2 N2 83.89(7) . . ? O3 Cd2 N2 88.13(7) 5 . ? N1 Cd2 N2 174.44(8) . . ? O4 Cd2 O6 96.70(7) . 5_565 ? O3 Cd2 O6 148.94(7) 5 5_565 ? N1 Cd2 O6 96.42(7) . 5_565 ? N2 Cd2 O6 78.20(7) . 5_565 ? O4 Cd2 O1 171.15(6) . 5 ? O3 Cd2 O1 78.10(7) 5 5 ? N1 Cd2 O1 87.78(7) . 5 ? N2 Cd2 O1 92.10(7) . 5 ? O6 Cd2 O1 74.72(6) 5_565 5 ? C5 C4 C3 119.9(2) . . ? C5 C4 C2 116.2(2) . . ? C3 C4 C2 123.9(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.555 _refine_diff_density_min -0.559 _refine_diff_density_rms 0.068 #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 746380' #TrackingRef 'complexes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H30 Cd3 N4 O14' _chemical_formula_weight 1296.02 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' 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 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.6201(5) _cell_length_b 11.9085(5) _cell_length_c 18.7329(8) _cell_angle_alpha 84.3870(10) _cell_angle_beta 86.8870(10) _cell_angle_gamma 66.2650(10) _cell_volume 2361.27(17) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 6368 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.823 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1276 _exptl_absorpt_coefficient_mu 1.416 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7459 _exptl_absorpt_correction_T_max 0.8157 _exptl_absorpt_process_details '(SADABS; Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 0 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 11838 _diffrn_reflns_av_R_equivalents 0.0147 _diffrn_reflns_av_sigmaI/netI 0.0319 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.09 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8241 _reflns_number_gt 7164 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'SAINT-Plus (Bruker, 2001)' _computing_data_reduction SAINT-Plus _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Sheldrick, 1998)' _computing_publication_material XP _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^)+(0.0716P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8241 _refine_ls_number_parameters 676 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0380 _refine_ls_R_factor_gt 0.0305 _refine_ls_wR_factor_ref 0.1120 _refine_ls_wR_factor_gt 0.0962 _refine_ls_goodness_of_fit_ref 1.134 _refine_ls_restrained_S_all 1.134 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd -0.03663(3) 0.31499(3) 0.616478(15) 0.03280(10) Uani 1 1 d . . . Cd2 Cd 0.06714(3) 0.44172(3) 0.741731(15) 0.02945(10) Uani 1 1 d . . . Cd3 Cd 0.25910(3) 0.26035(3) 0.880613(15) 0.03190(10) Uani 1 1 d . . . C1 C 0.4121(4) 0.2790(3) 0.6720(2) 0.0312(9) Uani 1 1 d . . . C53 C 0.3365(4) 0.0232(4) 0.9880(3) 0.0399(10) Uani 1 1 d . . . C6 C 0.5244(4) 0.2968(5) 0.6637(2) 0.0435(11) Uani 1 1 d . . . H6 H 0.5719 0.2892 0.7037 0.052 Uiso 1 1 calc R . . N1 N -0.0494(3) 0.1248(3) 0.62853(19) 0.0365(8) Uani 1 1 d . . . O10 O 0.0460(3) 0.3860(3) 0.86241(15) 0.0348(6) Uani 1 1 d . . . O5 O 0.3111(3) 0.3301(3) 0.48645(15) 0.0430(8) Uani 1 1 d . . . O2 O 0.2546(2) 0.2627(3) 0.75499(15) 0.0347(6) Uani 1 1 d . . . O3 O 0.1228(2) 0.3812(2) 0.62665(14) 0.0325(6) Uani 1 1 d . . . O11 O 0.0542(3) 0.2014(3) 0.89624(18) 0.0477(8) Uani 1 1 d . . . C14 C 0.2807(4) 0.2809(4) 0.3705(2) 0.0321(9) Uani 1 1 d . . . O9 O -0.0458(2) 0.3199(3) 0.74008(14) 0.0336(6) Uani 1 1 d . . . C43 C 0.1600(4) 0.3307(5) 1.0415(2) 0.0452(11) Uani 1 1 d . . . H43 H 0.1347 0.4109 1.0208 0.054 Uiso 1 1 calc R . . C4 C 0.4973(4) 0.3314(5) 0.5364(2) 0.0488(12) Uani 1 1 d . . . H4 H 0.5260 0.3478 0.4909 0.059 Uiso 1 1 calc R . . C45 C 0.1611(6) 0.1950(7) 1.1423(3) 0.0662(17) Uani 1 1 d . . . H45 H 0.1379 0.1812 1.1895 0.079 Uiso 1 1 calc R . . O1 O 0.4387(3) 0.2311(4) 0.79778(16) 0.0554(9) Uani 1 1 d . . . N4 N 0.3641(3) 0.0521(3) 0.9205(2) 0.0398(9) Uani 1 1 d . . . C32 C -0.0290(5) -0.0656(5) 0.6905(3) 0.0542(13) Uani 1 1 d . . . H32 H -0.0012 -0.1214 0.7306 0.065 Uiso 1 1 calc R . . O4 O 0.2048(3) 0.1875(3) 0.60235(19) 0.0511(8) Uani 1 1 d . . . C2 C 0.3427(3) 0.2884(3) 0.6116(2) 0.0273(8) Uani 1 1 d . . . N3 N 0.2267(3) 0.2388(3) 1.00245(18) 0.0353(8) Uani 1 1 d . . . N2 N -0.1191(3) 0.2941(3) 0.51287(18) 0.0331(8) Uani 1 1 d . . . C9 C 0.3514(4) 0.2488(4) 0.4328(2) 0.0308(9) Uani 1 1 d . . . C37 C -0.2022(4) 0.1699(4) 0.4562(2) 0.0366(10) Uani 1 1 d . . . C46 C 0.2318(5) 0.0948(5) 1.1031(3) 0.0499(12) Uani 1 1 d . . . C10 C 0.4559(4) 0.1412(4) 0.4408(2) 0.0419(11) Uani 1 1 d . . . H10 H 0.5031 0.1224 0.4821 0.050 Uiso 1 1 calc R . . C18 C -0.4096(4) 0.4775(5) 0.8930(3) 0.0497(12) Uani 1 1 d . . . H18 H -0.4966 0.5174 0.8964 0.060 Uiso 1 1 calc R . . C54 C 0.2626(4) 0.1217(4) 1.0320(2) 0.0347(9) Uani 1 1 d . . . O8 O -0.2333(3) 0.3576(4) 0.69953(19) 0.0694(12) Uani 1 1 d . . . C34 C -0.1253(4) -0.0071(4) 0.5749(3) 0.0387(10) Uani 1 1 d . . . C3 C 0.3878(4) 0.3126(4) 0.5441(2) 0.0340(9) Uani 1 1 d . . . C11 C 0.4917(5) 0.0604(4) 0.3878(3) 0.0551(13) Uani 1 1 d . . . H11 H 0.5618 -0.0136 0.3940 0.066 Uiso 1 1 calc R . . C13 C 0.3206(4) 0.1985(4) 0.3176(2) 0.0496(12) Uani 1 1 d . . . H13 H 0.2758 0.2181 0.2753 0.060 Uiso 1 1 calc R . . C8 C 0.2161(4) 0.2819(4) 0.6151(2) 0.0314(9) Uani 1 1 d . . . C49 C 0.3798(5) -0.0985(4) 1.0198(3) 0.0569(14) Uani 1 1 d . . . C21 C -0.1485(4) 0.3647(3) 0.8813(2) 0.0304(9) Uani 1 1 d . . . C7 C 0.3678(4) 0.2554(4) 0.7465(2) 0.0338(9) Uani 1 1 d . . . C16 C -0.2213(4) 0.3869(4) 0.8216(2) 0.0330(9) Uani 1 1 d . . . C42 C -0.1036(3) 0.1021(4) 0.5740(2) 0.0316(9) Uani 1 1 d . . . C23 C -0.1656(4) 0.3535(4) 0.7485(2) 0.0392(10) Uani 1 1 d . . . C40 C -0.1561(4) 0.3761(4) 0.4574(2) 0.0424(10) Uani 1 1 d . . . H40 H -0.1399 0.4465 0.4573 0.051 Uiso 1 1 calc R . . C41 C -0.1415(3) 0.1903(3) 0.5125(2) 0.0289(8) Uani 1 1 d . . . C22 C -0.0052(4) 0.3085(4) 0.8793(2) 0.0326(9) Uani 1 1 d . . . C5 C 0.5649(4) 0.3258(5) 0.5963(3) 0.0547(13) Uani 1 1 d . . . H5 H 0.6373 0.3415 0.5912 0.066 Uiso 1 1 calc R . . C48 C 0.3438(6) -0.1206(6) 1.0928(4) 0.0704(18) Uani 1 1 d . . . H48 H 0.3714 -0.2012 1.1132 0.084 Uiso 1 1 calc R . . C44 C 0.1263(5) 0.3116(6) 1.1126(3) 0.0607(14) Uani 1 1 d . . . H44 H 0.0805 0.3779 1.1392 0.073 Uiso 1 1 calc R . . C36 C -0.2210(4) 0.0577(4) 0.4584(3) 0.0458(12) Uani 1 1 d . . . H36 H -0.2588 0.0428 0.4199 0.055 Uiso 1 1 calc R . . C33 C -0.0842(5) -0.0907(5) 0.6362(3) 0.0574(14) Uani 1 1 d . . . H33 H -0.0953 -0.1642 0.6393 0.069 Uiso 1 1 calc R . . C35 C -0.1846(4) -0.0267(5) 0.5154(3) 0.0518(13) Uani 1 1 d . . . H35 H -0.1984 -0.0985 0.5159 0.062 Uiso 1 1 calc R . . C17 C -0.3527(4) 0.4417(4) 0.8276(2) 0.0426(10) Uani 1 1 d . . . H17 H -0.4015 0.4539 0.7876 0.051 Uiso 1 1 calc R . . C51 C 0.4830(5) -0.1616(5) 0.9083(4) 0.0691(17) Uani 1 1 d . . . H51 H 0.5328 -0.2227 0.8792 0.083 Uiso 1 1 calc R . . C15 C 0.1643(4) 0.3979(4) 0.3577(2) 0.0360(10) Uani 1 1 d . . . C31 C -0.0144(5) 0.0452(5) 0.6856(3) 0.0495(12) Uani 1 1 d . . . H31 H 0.0211 0.0639 0.7237 0.059 Uiso 1 1 calc R . . C38 C -0.2417(4) 0.2608(5) 0.3983(2) 0.0476(11) Uani 1 1 d . . . H38 H -0.2834 0.2505 0.3601 0.057 Uiso 1 1 calc R . . C12 C 0.4235(5) 0.0895(5) 0.3259(3) 0.0564(14) Uani 1 1 d . . . H12 H 0.4473 0.0355 0.2899 0.068 Uiso 1 1 calc R . . C39 C -0.2181(5) 0.3642(5) 0.3988(3) 0.0527(13) Uani 1 1 d . . . H39 H -0.2428 0.4252 0.3610 0.063 Uiso 1 1 calc R . . C52 C 0.4357(5) -0.0368(5) 0.8816(3) 0.0573(14) Uani 1 1 d . . . H52 H 0.4559 -0.0168 0.8347 0.069 Uiso 1 1 calc R . . C47 C 0.2741(6) -0.0319(6) 1.1309(3) 0.0684(17) Uani 1 1 d . . . H47 H 0.2509 -0.0507 1.1773 0.082 Uiso 1 1 calc R . . C50 C 0.4556(5) -0.1910(5) 0.9758(4) 0.074(2) Uani 1 1 d . . . H50 H 0.4867 -0.2731 0.9939 0.089 Uiso 1 1 calc R . . O7 O 0.0992(3) 0.4016(3) 0.30436(17) 0.0465(8) Uani 1 1 d . . . O6 O 0.1413(3) 0.4799(3) 0.39831(19) 0.0597(10) Uani 1 1 d . . . C19 C -0.3374(4) 0.4542(4) 0.9533(3) 0.0444(11) Uani 1 1 d . . . H19 H -0.3758 0.4766 0.9976 0.053 Uiso 1 1 calc R . . O12 O -0.1349(3) 0.3763(3) 1.00761(15) 0.0374(7) Uani 1 1 d . . . C24 C -0.1566(4) 0.2963(4) 1.0623(2) 0.0354(9) Uani 1 1 d . . . C29 C -0.1944(4) 0.3376(4) 1.1303(2) 0.0348(9) Uani 1 1 d . . . C20 C -0.2090(4) 0.3980(4) 0.9476(2) 0.0334(9) Uani 1 1 d . . . C25 C -0.1318(5) 0.1789(4) 1.0482(3) 0.0515(12) Uani 1 1 d . . . H25 H -0.1022 0.1533 1.0029 0.062 Uiso 1 1 calc R . . C30 C -0.2110(4) 0.4614(4) 1.1512(2) 0.0316(9) Uani 1 1 d . . . C28 C -0.2109(5) 0.2511(5) 1.1819(3) 0.0548(13) Uani 1 1 d . . . H28 H -0.2356 0.2739 1.2282 0.066 Uiso 1 1 calc R . . C27 C -0.1924(6) 0.1367(5) 1.1671(3) 0.0692(18) Uani 1 1 d . . . H27 H -0.2084 0.0839 1.2023 0.083 Uiso 1 1 calc R . . C26 C -0.1502(6) 0.0972(5) 1.1005(3) 0.0649(16) Uani 1 1 d . . . H26 H -0.1342 0.0172 1.0907 0.078 Uiso 1 1 calc R . . O14 O -0.2653(3) 0.5524(3) 1.10877(16) 0.0407(7) Uani 1 1 d . . . O13 O -0.1701(3) 0.4597(3) 1.21250(15) 0.0436(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.03098(17) 0.04044(19) 0.03132(18) -0.01441(13) -0.00360(13) -0.01583(14) Cd2 0.02763(17) 0.03129(17) 0.02872(17) -0.00723(12) -0.00691(12) -0.00920(13) Cd3 0.03382(18) 0.03318(18) 0.02494(17) 0.00137(12) -0.00469(12) -0.00982(13) C1 0.0278(19) 0.031(2) 0.028(2) -0.0049(16) -0.0029(16) -0.0038(16) C53 0.034(2) 0.039(2) 0.048(3) 0.009(2) -0.019(2) -0.0162(19) C6 0.027(2) 0.073(3) 0.032(2) -0.015(2) -0.0027(18) -0.019(2) N1 0.0380(19) 0.042(2) 0.035(2) -0.0052(16) -0.0022(16) -0.0209(16) O10 0.0339(15) 0.0448(17) 0.0313(15) -0.0093(13) 0.0009(12) -0.0205(13) O5 0.0301(15) 0.0564(19) 0.0271(15) -0.0136(14) -0.0056(12) 0.0017(14) O2 0.0290(15) 0.0389(16) 0.0315(16) -0.0024(12) -0.0011(12) -0.0086(12) O3 0.0248(13) 0.0378(15) 0.0290(15) -0.0036(12) -0.0020(11) -0.0060(12) O11 0.0384(17) 0.0366(18) 0.061(2) -0.0096(15) -0.0043(15) -0.0061(14) C14 0.029(2) 0.030(2) 0.033(2) -0.0086(17) -0.0027(17) -0.0061(17) O9 0.0308(15) 0.0455(16) 0.0306(15) -0.0142(13) 0.0014(12) -0.0195(13) C43 0.050(3) 0.048(3) 0.039(3) -0.012(2) -0.001(2) -0.020(2) C4 0.035(2) 0.075(3) 0.031(2) -0.012(2) 0.0121(19) -0.017(2) C45 0.073(4) 0.118(5) 0.029(3) -0.005(3) 0.008(3) -0.060(4) O1 0.0371(17) 0.094(3) 0.0289(17) 0.0042(17) -0.0138(14) -0.0197(18) N4 0.0299(18) 0.040(2) 0.046(2) -0.0049(17) -0.0052(16) -0.0093(16) C32 0.057(3) 0.048(3) 0.054(3) 0.007(2) 0.002(3) -0.020(2) O4 0.0500(19) 0.0447(18) 0.071(2) -0.0286(17) -0.0034(17) -0.0257(16) C2 0.0232(18) 0.0259(19) 0.029(2) -0.0096(16) -0.0025(15) -0.0042(15) N3 0.0380(19) 0.0368(19) 0.0311(19) 0.0012(15) -0.0066(15) -0.0152(16) N2 0.0371(18) 0.0312(17) 0.0340(19) -0.0098(15) -0.0033(15) -0.0149(15) C9 0.0262(19) 0.039(2) 0.024(2) -0.0061(17) 0.0006(16) -0.0094(17) C37 0.026(2) 0.052(3) 0.033(2) -0.019(2) 0.0011(17) -0.0127(18) C46 0.059(3) 0.065(3) 0.037(3) 0.009(2) -0.016(2) -0.038(3) C10 0.031(2) 0.044(2) 0.040(3) -0.006(2) -0.0107(19) -0.0025(19) C18 0.027(2) 0.066(3) 0.045(3) -0.002(2) 0.006(2) -0.008(2) C54 0.040(2) 0.036(2) 0.033(2) 0.0015(18) -0.0098(18) -0.0198(19) O8 0.0401(19) 0.134(4) 0.043(2) -0.036(2) -0.0018(16) -0.037(2) C34 0.033(2) 0.035(2) 0.051(3) -0.013(2) 0.0104(19) -0.0154(18) C3 0.028(2) 0.039(2) 0.029(2) -0.0115(18) -0.0006(17) -0.0050(17) C11 0.047(3) 0.037(3) 0.064(3) -0.017(2) -0.013(2) 0.005(2) C13 0.046(3) 0.057(3) 0.035(2) -0.016(2) -0.015(2) -0.003(2) C8 0.0253(19) 0.041(2) 0.026(2) -0.0073(17) -0.0038(16) -0.0103(17) C49 0.047(3) 0.040(3) 0.086(4) 0.013(3) -0.028(3) -0.020(2) C21 0.032(2) 0.030(2) 0.033(2) -0.0063(17) 0.0007(17) -0.0161(17) C7 0.032(2) 0.036(2) 0.028(2) -0.0067(17) -0.0004(17) -0.0070(17) C16 0.032(2) 0.034(2) 0.034(2) -0.0055(18) 0.0015(17) -0.0141(17) C42 0.0256(19) 0.036(2) 0.036(2) -0.0123(18) 0.0050(17) -0.0132(17) C23 0.035(2) 0.054(3) 0.033(2) -0.015(2) 0.0024(19) -0.020(2) C40 0.049(3) 0.041(2) 0.040(3) -0.001(2) -0.009(2) -0.021(2) C41 0.0244(19) 0.031(2) 0.033(2) -0.0121(16) 0.0036(16) -0.0108(16) C22 0.032(2) 0.041(2) 0.028(2) -0.0123(18) -0.0009(17) -0.0154(19) C5 0.033(2) 0.092(4) 0.046(3) -0.013(3) 0.007(2) -0.032(3) C48 0.079(4) 0.062(4) 0.077(4) 0.045(3) -0.039(3) -0.042(3) C44 0.062(3) 0.083(4) 0.045(3) -0.023(3) 0.010(3) -0.034(3) C36 0.035(2) 0.058(3) 0.056(3) -0.034(3) 0.002(2) -0.024(2) C33 0.049(3) 0.051(3) 0.075(4) 0.001(3) 0.021(3) -0.027(2) C35 0.042(3) 0.051(3) 0.073(4) -0.028(3) 0.012(3) -0.026(2) C17 0.032(2) 0.060(3) 0.036(2) -0.003(2) -0.0036(19) -0.019(2) C51 0.047(3) 0.039(3) 0.115(6) -0.025(3) 0.001(3) -0.007(2) C15 0.025(2) 0.042(2) 0.033(2) -0.0050(19) -0.0069(17) -0.0050(18) C31 0.058(3) 0.059(3) 0.033(3) -0.001(2) -0.003(2) -0.026(2) C38 0.045(3) 0.062(3) 0.037(3) -0.015(2) -0.008(2) -0.019(2) C12 0.053(3) 0.049(3) 0.055(3) -0.028(2) -0.005(2) -0.001(2) C39 0.057(3) 0.055(3) 0.035(3) 0.001(2) -0.012(2) -0.011(2) C52 0.041(3) 0.054(3) 0.076(4) -0.024(3) 0.007(3) -0.014(2) C47 0.093(5) 0.083(4) 0.046(3) 0.023(3) -0.020(3) -0.056(4) C50 0.057(3) 0.029(3) 0.134(6) 0.004(3) -0.030(4) -0.013(3) O7 0.0407(17) 0.0441(17) 0.0440(18) -0.0081(14) -0.0217(14) -0.0024(14) O6 0.055(2) 0.0445(19) 0.058(2) -0.0230(17) -0.0300(17) 0.0104(16) C19 0.040(2) 0.051(3) 0.039(3) -0.012(2) 0.014(2) -0.015(2) O12 0.0425(16) 0.0483(17) 0.0301(15) -0.0070(13) -0.0009(13) -0.0261(14) C24 0.037(2) 0.038(2) 0.035(2) -0.0029(18) -0.0102(18) -0.0172(18) C29 0.040(2) 0.040(2) 0.032(2) 0.0049(18) -0.0125(18) -0.0242(19) C20 0.036(2) 0.038(2) 0.030(2) -0.0049(17) 0.0009(17) -0.0183(18) C25 0.056(3) 0.041(3) 0.057(3) -0.009(2) -0.016(2) -0.015(2) C30 0.035(2) 0.040(2) 0.029(2) -0.0026(18) -0.0013(17) -0.0251(19) C28 0.080(4) 0.062(3) 0.037(3) 0.015(2) -0.021(2) -0.046(3) C27 0.099(5) 0.064(4) 0.062(4) 0.030(3) -0.044(3) -0.052(3) C26 0.080(4) 0.033(3) 0.084(4) 0.008(3) -0.042(3) -0.024(3) O14 0.0494(18) 0.0375(16) 0.0405(17) -0.0018(14) -0.0071(14) -0.0225(14) O13 0.067(2) 0.0489(18) 0.0327(16) -0.0049(14) -0.0089(15) -0.0400(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O6 2.244(3) 2_566 ? Cd1 N2 2.288(3) . ? Cd1 O3 2.310(3) . ? Cd1 O9 2.317(3) . ? Cd1 N1 2.318(3) . ? Cd1 O8 2.595(3) . ? Cd1 O4 2.610(3) . ? Cd1 Cd2 3.4208(4) . ? Cd2 O7 2.220(3) 2_566 ? Cd2 O13 2.232(3) 2_567 ? Cd2 O3 2.316(3) . ? Cd2 O9 2.318(3) . ? Cd2 O10 2.321(3) . ? Cd2 O2 2.360(3) . ? Cd2 Cd3 3.4730(4) . ? Cd3 O14 2.288(3) 2_567 ? Cd3 N3 2.299(3) . ? Cd3 O10 2.344(3) . ? Cd3 N4 2.345(4) . ? Cd3 O2 2.354(3) . ? Cd3 O1 2.460(3) . ? Cd3 C7 2.744(4) . ? C1 C2 1.394(5) . ? C1 C6 1.403(6) . ? C1 C7 1.502(5) . ? C53 N4 1.334(6) . ? C53 C49 1.409(6) . ? C53 C54 1.448(6) . ? C6 C5 1.384(6) . ? C6 H6 0.9300 . ? N1 C31 1.322(6) . ? N1 C42 1.332(5) . ? O10 C22 1.293(5) . ? O5 C3 1.384(5) . ? O5 C9 1.393(5) . ? O2 C7 1.285(5) . ? O3 C8 1.270(5) . ? O11 C22 1.199(5) . ? C14 C13 1.391(6) . ? C14 C9 1.395(5) . ? C14 C15 1.511(5) . ? O9 C23 1.290(5) . ? C43 N3 1.321(6) . ? C43 C44 1.391(7) . ? C43 H43 0.9300 . ? C4 C3 1.376(6) . ? C4 C5 1.386(7) . ? C4 H4 0.9300 . ? C45 C44 1.349(8) . ? C45 C46 1.398(8) . ? C45 H45 0.9300 . ? O1 C7 1.234(5) . ? N4 C52 1.311(6) . ? C32 C33 1.349(8) . ? C32 C31 1.390(7) . ? C32 H32 0.9300 . ? O4 C8 1.231(5) . ? C2 C3 1.391(6) . ? C2 C8 1.501(5) . ? N3 C54 1.353(5) . ? N2 C40 1.315(5) . ? N2 C41 1.362(5) . ? C9 C10 1.366(5) . ? C37 C41 1.392(5) . ? C37 C38 1.408(6) . ? C37 C36 1.434(6) . ? C46 C54 1.399(6) . ? C46 C47 1.438(8) . ? C10 C11 1.379(6) . ? C10 H10 0.9300 . ? C18 C17 1.380(6) . ? C18 C19 1.383(7) . ? C18 H18 0.9300 . ? O8 C23 1.226(5) . ? C34 C33 1.411(7) . ? C34 C42 1.420(6) . ? C34 C35 1.426(7) . ? C11 C12 1.377(7) . ? C11 H11 0.9300 . ? C13 C12 1.368(7) . ? C13 H13 0.9300 . ? C49 C50 1.409(9) . ? C49 C48 1.438(8) . ? C21 C16 1.379(6) . ? C21 C20 1.404(6) . ? C21 C22 1.525(5) . ? C16 C17 1.401(6) . ? C16 C23 1.501(6) . ? C42 C41 1.439(6) . ? C40 C39 1.395(6) . ? C40 H40 0.9300 . ? C5 H5 0.9300 . ? C48 C47 1.295(9) . ? C48 H48 0.9300 . ? C44 H44 0.9300 . ? C36 C35 1.353(7) . ? C36 H36 0.9300 . ? C33 H33 0.9300 . ? C35 H35 0.9300 . ? C17 H17 0.9300 . ? C51 C50 1.337(9) . ? C51 C52 1.410(8) . ? C51 H51 0.9300 . ? C15 O6 1.231(5) . ? C15 O7 1.273(5) . ? C31 H31 0.9300 . ? C38 C39 1.366(7) . ? C38 H38 0.9300 . ? C12 H12 0.9300 . ? C39 H39 0.9300 . ? C52 H52 0.9300 . ? C47 H47 0.9300 . ? C50 H50 0.9300 . ? O7 Cd2 2.220(3) 2_566 ? O6 Cd1 2.244(3) 2_566 ? C19 C20 1.370(6) . ? C19 H19 0.9300 . ? O12 C20 1.393(5) . ? O12 C24 1.412(5) . ? C24 C25 1.359(6) . ? C24 C29 1.396(6) . ? C29 C28 1.405(6) . ? C29 C30 1.497(6) . ? C25 C26 1.381(8) . ? C25 H25 0.9300 . ? C30 O14 1.241(5) . ? C30 O13 1.262(5) . ? C28 C27 1.346(8) . ? C28 H28 0.9300 . ? C27 C26 1.371(9) . ? C27 H27 0.9300 . ? C26 H26 0.9300 . ? O14 Cd3 2.288(3) 2_567 ? O13 Cd2 2.232(3) 2_567 ? 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 Cd1 N2 90.44(11) 2_566 . ? O6 Cd1 O3 78.43(12) 2_566 . ? N2 Cd1 O3 127.15(11) . . ? O6 Cd1 O9 91.12(11) 2_566 . ? N2 Cd1 O9 150.06(11) . . ? O3 Cd1 O9 82.36(9) . . ? O6 Cd1 N1 146.74(13) 2_566 . ? N2 Cd1 N1 72.60(12) . . ? O3 Cd1 N1 134.61(11) . . ? O9 Cd1 N1 90.35(11) . . ? O6 Cd1 O8 76.26(15) 2_566 . ? N2 Cd1 O8 98.68(11) . . ? O3 Cd1 O8 127.17(11) . . ? O9 Cd1 O8 52.91(10) . . ? N1 Cd1 O8 78.29(13) . . ? O6 Cd1 O4 127.85(13) 2_566 . ? N2 Cd1 O4 104.34(11) . . ? O3 Cd1 O4 52.62(9) . . ? O9 Cd1 O4 98.17(10) . . ? N1 Cd1 O4 84.70(11) . . ? O8 Cd1 O4 145.72(12) . . ? O6 Cd1 Cd2 72.08(8) 2_566 . ? N2 Cd1 Cd2 160.56(8) . . ? O3 Cd1 Cd2 42.37(7) . . ? O9 Cd1 Cd2 42.44(7) . . ? N1 Cd1 Cd2 126.79(9) . . ? O8 Cd1 Cd2 85.64(8) . . ? O4 Cd1 Cd2 81.05(7) . . ? O7 Cd2 O13 101.24(12) 2_566 2_567 ? O7 Cd2 O3 88.03(10) 2_566 . ? O13 Cd2 O3 117.41(10) 2_567 . ? O7 Cd2 O9 87.98(11) 2_566 . ? O13 Cd2 O9 158.25(10) 2_567 . ? O3 Cd2 O9 82.23(10) . . ? O7 Cd2 O10 114.55(11) 2_566 . ? O13 Cd2 O10 81.44(10) 2_567 . ? O3 Cd2 O10 148.19(10) . . ? O9 Cd2 O10 76.81(10) . . ? O7 Cd2 O2 163.10(11) 2_566 . ? O13 Cd2 O2 86.87(11) 2_567 . ? O3 Cd2 O2 75.07(9) . . ? O9 Cd2 O2 89.69(10) . . ? O10 Cd2 O2 81.12(10) . . ? O7 Cd2 Cd1 76.20(8) 2_566 . ? O13 Cd2 Cd1 158.96(8) 2_567 . ? O3 Cd2 Cd1 42.24(7) . . ? O9 Cd2 Cd1 42.44(7) . . ? O10 Cd2 Cd1 118.88(7) . . ? O2 Cd2 Cd1 90.87(7) . . ? O7 Cd2 Cd3 154.42(8) 2_566 . ? O13 Cd2 Cd3 69.08(8) 2_567 . ? O3 Cd2 Cd3 117.53(6) . . ? O9 Cd2 Cd3 94.19(7) . . ? O10 Cd2 Cd3 42.15(7) . . ? O2 Cd2 Cd3 42.47(7) . . ? Cd1 Cd2 Cd3 121.368(11) . . ? O14 Cd3 N3 89.94(12) 2_567 . ? O14 Cd3 O10 81.00(10) 2_567 . ? N3 Cd3 O10 91.68(11) . . ? O14 Cd3 N4 140.50(12) 2_567 . ? N3 Cd3 N4 71.68(12) . . ? O10 Cd3 N4 132.49(11) . . ? O14 Cd3 O2 100.45(10) 2_567 . ? N3 Cd3 O2 165.95(11) . . ? O10 Cd3 O2 80.76(9) . . ? N4 Cd3 O2 104.80(11) . . ? O14 Cd3 O1 83.88(12) 2_567 . ? N3 Cd3 O1 137.18(11) . . ? O10 Cd3 O1 128.63(10) . . ? N4 Cd3 O1 86.71(12) . . ? O2 Cd3 O1 54.33(10) . . ? O14 Cd3 C7 89.58(12) 2_567 . ? N3 Cd3 C7 163.71(12) . . ? O10 Cd3 C7 104.33(11) . . ? N4 Cd3 C7 98.81(13) . . ? O2 Cd3 C7 27.87(11) . . ? O1 Cd3 C7 26.72(11) . . ? O14 Cd3 Cd2 78.10(8) 2_567 . ? N3 Cd3 Cd2 132.79(9) . . ? O10 Cd3 Cd2 41.64(7) . . ? N4 Cd3 Cd2 139.67(9) . . ? O2 Cd3 Cd2 42.60(6) . . ? O1 Cd3 Cd2 87.25(7) . . ? C7 Cd3 Cd2 62.85(8) . . ? C2 C1 C6 119.5(4) . . ? C2 C1 C7 122.0(4) . . ? C6 C1 C7 118.5(4) . . ? N4 C53 C49 123.4(5) . . ? N4 C53 C54 118.7(4) . . ? C49 C53 C54 117.9(4) . . ? C5 C6 C1 120.4(4) . . ? C5 C6 H6 119.8 . . ? C1 C6 H6 119.8 . . ? C31 N1 C42 120.4(4) . . ? C31 N1 Cd1 124.9(3) . . ? C42 N1 Cd1 114.6(3) . . ? C22 O10 Cd2 118.3(2) . . ? C22 O10 Cd3 101.2(2) . . ? Cd2 O10 Cd3 96.21(10) . . ? C3 O5 C9 119.7(3) . . ? C7 O2 Cd3 93.2(2) . . ? C7 O2 Cd2 127.3(3) . . ? Cd3 O2 Cd2 94.92(10) . . ? C8 O3 Cd1 98.8(2) . . ? C8 O3 Cd2 121.3(2) . . ? Cd1 O3 Cd2 95.39(10) . . ? C13 C14 C9 117.2(4) . . ? C13 C14 C15 118.7(4) . . ? C9 C14 C15 124.1(4) . . ? C23 O9 Cd1 97.8(2) . . ? C23 O9 Cd2 127.3(3) . . ? Cd1 O9 Cd2 95.12(10) . . ? N3 C43 C44 122.3(5) . . ? N3 C43 H43 118.8 . . ? C44 C43 H43 118.8 . . ? C3 C4 C5 120.1(4) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? C44 C45 C46 121.0(5) . . ? C44 C45 H45 119.5 . . ? C46 C45 H45 119.5 . . ? C7 O1 Cd3 89.6(2) . . ? C52 N4 C53 118.7(4) . . ? C52 N4 Cd3 126.5(4) . . ? C53 N4 Cd3 114.5(3) . . ? C33 C32 C31 118.9(5) . . ? C33 C32 H32 120.5 . . ? C31 C32 H32 120.5 . . ? C8 O4 Cd1 85.7(2) . . ? C3 C2 C1 119.2(4) . . ? C3 C2 C8 117.0(3) . . ? C1 C2 C8 123.7(3) . . ? C43 N3 C54 119.2(4) . . ? C43 N3 Cd3 124.3(3) . . ? C54 N3 Cd3 115.7(3) . . ? C40 N2 C41 117.8(4) . . ? C40 N2 Cd1 126.5(3) . . ? C41 N2 Cd1 115.4(3) . . ? C10 C9 O5 121.5(4) . . ? C10 C9 C14 121.0(4) . . ? O5 C9 C14 117.5(3) . . ? C41 C37 C38 118.1(4) . . ? C41 C37 C36 119.5(4) . . ? C38 C37 C36 122.3(4) . . ? C45 C46 C54 116.8(5) . . ? C45 C46 C47 124.5(5) . . ? C54 C46 C47 118.7(5) . . ? C9 C10 C11 120.4(4) . . ? C9 C10 H10 119.8 . . ? C11 C10 H10 119.8 . . ? C17 C18 C19 120.1(4) . . ? C17 C18 H18 119.9 . . ? C19 C18 H18 119.9 . . ? N3 C54 C46 122.0(4) . . ? N3 C54 C53 117.8(4) . . ? C46 C54 C53 120.2(4) . . ? C23 O8 Cd1 86.4(3) . . ? C33 C34 C42 116.1(4) . . ? C33 C34 C35 124.3(5) . . ? C42 C34 C35 119.5(4) . . ? C4 C3 O5 121.6(4) . . ? C4 C3 C2 121.1(4) . . ? O5 C3 C2 117.0(4) . . ? C12 C11 C10 119.8(4) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? C12 C13 C14 122.1(4) . . ? C12 C13 H13 119.0 . . ? C14 C13 H13 119.0 . . ? O4 C8 O3 122.9(4) . . ? O4 C8 C2 120.9(4) . . ? O3 C8 C2 116.0(3) . . ? C53 C49 C50 116.0(5) . . ? C53 C49 C48 119.3(5) . . ? C50 C49 C48 124.7(5) . . ? C16 C21 C20 118.6(4) . . ? C16 C21 C22 123.7(4) . . ? C20 C21 C22 117.7(4) . . ? O1 C7 O2 121.7(4) . . ? O1 C7 C1 120.3(4) . . ? O2 C7 C1 118.1(3) . . ? O1 C7 Cd3 63.7(2) . . ? O2 C7 Cd3 58.9(2) . . ? C1 C7 Cd3 168.9(3) . . ? C21 C16 C17 120.2(4) . . ? C21 C16 C23 122.6(4) . . ? C17 C16 C23 117.2(4) . . ? N1 C42 C34 121.6(4) . . ? N1 C42 C41 119.4(4) . . ? C34 C42 C41 118.9(4) . . ? O8 C23 O9 122.2(4) . . ? O8 C23 C16 120.1(4) . . ? O9 C23 C16 117.7(4) . . ? N2 C40 C39 124.2(4) . . ? N2 C40 H40 117.9 . . ? C39 C40 H40 117.9 . . ? N2 C41 C37 122.2(4) . . ? N2 C41 C42 117.7(3) . . ? C37 C41 C42 120.1(4) . . ? O11 C22 O10 123.2(4) . . ? O11 C22 C21 121.7(4) . . ? O10 C22 C21 114.9(3) . . ? C6 C5 C4 119.8(4) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C47 C48 C49 122.1(5) . . ? C47 C48 H48 118.9 . . ? C49 C48 H48 118.9 . . ? C45 C44 C43 118.8(5) . . ? C45 C44 H44 120.6 . . ? C43 C44 H44 120.6 . . ? C35 C36 C37 121.0(4) . . ? C35 C36 H36 119.5 . . ? C37 C36 H36 119.5 . . ? C32 C33 C34 120.9(5) . . ? C32 C33 H33 119.5 . . ? C34 C33 H33 119.5 . . ? C36 C35 C34 120.9(4) . . ? C36 C35 H35 119.6 . . ? C34 C35 H35 119.6 . . ? C18 C17 C16 120.1(4) . . ? C18 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? C50 C51 C52 119.2(5) . . ? C50 C51 H51 120.4 . . ? C52 C51 H51 120.4 . . ? O6 C15 O7 126.3(4) . . ? O6 C15 C14 118.5(4) . . ? O7 C15 C14 115.3(4) . . ? N1 C31 C32 122.0(5) . . ? N1 C31 H31 119.0 . . ? C32 C31 H31 119.0 . . ? C39 C38 C37 119.4(4) . . ? C39 C38 H38 120.3 . . ? C37 C38 H38 120.3 . . ? C13 C12 C11 119.5(4) . . ? C13 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? C38 C39 C40 118.3(4) . . ? C38 C39 H39 120.9 . . ? C40 C39 H39 120.9 . . ? N4 C52 C51 122.3(6) . . ? N4 C52 H52 118.8 . . ? C51 C52 H52 118.8 . . ? C48 C47 C46 121.6(5) . . ? C48 C47 H47 119.2 . . ? C46 C47 H47 119.2 . . ? C51 C50 C49 120.4(5) . . ? C51 C50 H50 119.8 . . ? C49 C50 H50 119.8 . . ? C15 O7 Cd2 128.5(3) . 2_566 ? C15 O6 Cd1 132.5(3) . 2_566 ? C20 C19 C18 119.7(4) . . ? C20 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? C20 O12 C24 113.2(3) . . ? C25 C24 C29 122.0(4) . . ? C25 C24 O12 118.8(4) . . ? C29 C24 O12 119.0(4) . . ? C24 C29 C28 115.2(4) . . ? C24 C29 C30 124.7(4) . . ? C28 C29 C30 120.0(4) . . ? C19 C20 O12 120.4(4) . . ? C19 C20 C21 121.3(4) . . ? O12 C20 C21 118.2(3) . . ? C24 C25 C26 120.7(5) . . ? C24 C25 H25 119.7 . . ? C26 C25 H25 119.7 . . ? O14 C30 O13 127.7(4) . . ? O14 C30 C29 118.0(4) . . ? O13 C30 C29 114.3(4) . . ? C27 C28 C29 122.7(5) . . ? C27 C28 H28 118.6 . . ? C29 C28 H28 118.6 . . ? C28 C27 C26 120.6(5) . . ? C28 C27 H27 119.7 . . ? C26 C27 H27 119.7 . . ? C27 C26 C25 118.6(5) . . ? C27 C26 H26 120.7 . . ? C25 C26 H26 120.7 . . ? C30 O14 Cd3 122.3(3) . 2_567 ? C30 O13 Cd2 134.5(3) . 2_567 ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.202 _refine_diff_density_min -0.637 _refine_diff_density_rms 0.162 #===END data_5 _database_code_depnum_ccdc_archive 'CCDC 746381' #TrackingRef 'complexes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H30 Cd3 N4 O14' _chemical_formula_weight 1247.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.2000(9) _cell_length_b 11.5369(9) _cell_length_c 18.3362(14) _cell_angle_alpha 88.2210(10) _cell_angle_beta 81.4750(10) _cell_angle_gamma 70.8300(10) _cell_volume 2212.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 6378 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.873 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1228 _exptl_absorpt_coefficient_mu 1.506 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7138 _exptl_absorpt_correction_T_max 0.7732 _exptl_absorpt_process_details '(SADABS; Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 0 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 11015 _diffrn_reflns_av_R_equivalents 0.0155 _diffrn_reflns_av_sigmaI/netI 0.0324 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7681 _reflns_number_gt 6767 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'SAINT-Plus (Bruker, 2001)' _computing_data_reduction SAINT-Plus _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Sheldrick, 1998)' _computing_publication_material XP _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^)+(0.0259P)^2^+1.3056P] 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 7681 _refine_ls_number_parameters 640 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0300 _refine_ls_R_factor_gt 0.0246 _refine_ls_wR_factor_ref 0.0629 _refine_ls_wR_factor_gt 0.0607 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2154(3) 1.1698(3) 0.23495(17) 0.0358(7) Uani 1 1 d . . . C2 C 0.2340(3) 1.0137(3) 0.10026(16) 0.0308(7) Uani 1 1 d . . . C3 C 0.1707(3) 1.1518(3) 0.10447(16) 0.0257(6) Uani 1 1 d . . . C4 C 0.1579(3) 1.2235(3) 0.16751(16) 0.0303(7) Uani 1 1 d . . . C5 C 0.0898(3) 1.3483(3) 0.16864(18) 0.0372(8) Uani 1 1 d . . . H5 H 0.0820 1.3958 0.2103 0.045 Uiso 1 1 calc R . . C6 C 0.0336(3) 1.4024(3) 0.10814(19) 0.0429(8) Uani 1 1 d . . . H6 H -0.0153 1.4852 0.1101 0.051 Uiso 1 1 calc R . . C7 C 0.0501(3) 1.3332(3) 0.04476(18) 0.0391(8) Uani 1 1 d . . . H7 H 0.0149 1.3696 0.0035 0.047 Uiso 1 1 calc R . . C8 C 0.1193(3) 1.2097(3) 0.04345(16) 0.0287(6) Uani 1 1 d . . . C9 C 0.2053(3) 1.1677(3) -0.08132(16) 0.0289(6) Uani 1 1 d . . . C10 C 0.3338(3) 1.1480(3) -0.08097(19) 0.0396(8) Uani 1 1 d . . . H10 H 0.3709 1.1172 -0.0392 0.048 Uiso 1 1 calc R . . C11 C 0.4069(3) 1.1740(3) -0.1425(2) 0.0433(8) Uani 1 1 d . . . H11 H 0.4933 1.1609 -0.1422 0.052 Uiso 1 1 calc R . . C12 C 0.3523(3) 1.2194(3) -0.20442(19) 0.0450(9) Uani 1 1 d . . . H12 H 0.4003 1.2411 -0.2450 0.054 Uiso 1 1 calc R . . C13 C 0.2259(3) 1.2323(3) -0.20568(17) 0.0397(8) Uani 1 1 d . . . H13 H 0.1909 1.2593 -0.2486 0.048 Uiso 1 1 calc R . . C14 C 0.1491(3) 1.2065(3) -0.14516(16) 0.0276(6) Uani 1 1 d . . . C15 C 0.0160(3) 1.2140(3) -0.15362(16) 0.0282(6) Uani 1 1 d . . . C16 C 0.2606(3) 0.8088(3) 0.37817(15) 0.0305(7) Uani 1 1 d . . . C17 C 0.2769(3) 0.6547(3) 0.24254(16) 0.0271(6) Uani 1 1 d . . . C18 C 0.2386(3) 0.6861(2) 0.38180(15) 0.0240(6) Uani 1 1 d . . . C19 C 0.2466(3) 0.6143(3) 0.31979(15) 0.0268(6) Uani 1 1 d . . . C20 C 0.2240(3) 0.5030(3) 0.32838(18) 0.0377(8) Uani 1 1 d . . . H20 H 0.2331 0.4542 0.2872 0.045 Uiso 1 1 calc R . . C21 C 0.1880(4) 0.4643(3) 0.39767(19) 0.0473(9) Uani 1 1 d . . . H21 H 0.1707 0.3908 0.4029 0.057 Uiso 1 1 calc R . . C22 C 0.1777(3) 0.5350(3) 0.45935(18) 0.0418(8) Uani 1 1 d . . . H22 H 0.1520 0.5100 0.5060 0.050 Uiso 1 1 calc R . . C23 C 0.2060(3) 0.6431(3) 0.45121(16) 0.0305(7) Uani 1 1 d . . . C24 C 0.2414(3) 0.6622(3) 0.57397(16) 0.0297(7) Uani 1 1 d . . . C25 C 0.3542(3) 0.5653(3) 0.56756(19) 0.0463(9) Uani 1 1 d . . . H25 H 0.3954 0.5330 0.5212 0.056 Uiso 1 1 calc R . . C26 C 0.4065(4) 0.5157(4) 0.6298(2) 0.0635(12) Uani 1 1 d . . . H26 H 0.4838 0.4516 0.6252 0.076 Uiso 1 1 calc R . . C27 C 0.3442(4) 0.5612(4) 0.6983(2) 0.0688(13) Uani 1 1 d . . . H27 H 0.3764 0.5254 0.7405 0.083 Uiso 1 1 calc R . . C28 C 0.2338(4) 0.6602(3) 0.70405(19) 0.0495(10) Uani 1 1 d . . . H28 H 0.1944 0.6933 0.7505 0.059 Uiso 1 1 calc R . . C29 C 0.1794(3) 0.7122(3) 0.64253(16) 0.0301(7) Uani 1 1 d . . . C30 C 0.0571(3) 0.8201(3) 0.65381(16) 0.0308(7) Uani 1 1 d . . . C31 C 0.1247(3) 1.2044(3) 0.53194(19) 0.0458(9) Uani 1 1 d . . . H31 H 0.0519 1.1873 0.5243 0.055 Uiso 1 1 calc R . . C32 C 0.1177(4) 1.2760(3) 0.59207(19) 0.0505(9) Uani 1 1 d . . . H32 H 0.0423 1.3055 0.6249 0.061 Uiso 1 1 calc R . . C33 C 0.2245(4) 1.3028(3) 0.60249(18) 0.0483(9) Uani 1 1 d . . . H33 H 0.2215 1.3538 0.6415 0.058 Uiso 1 1 calc R . . C34 C 0.3370(4) 1.2531(3) 0.55452(17) 0.0407(8) Uani 1 1 d . . . H34 H 0.4111 1.2681 0.5619 0.049 Uiso 1 1 calc R . . C35 C 0.3377(3) 1.1809(3) 0.49541(16) 0.0308(7) Uani 1 1 d . . . C36 C 0.4541(3) 1.1253(3) 0.44166(16) 0.0294(7) Uani 1 1 d . . . C37 C 0.5739(3) 1.1265(3) 0.45231(19) 0.0418(8) Uani 1 1 d . . . H37 H 0.5834 1.1648 0.4939 0.050 Uiso 1 1 calc R . . C38 C 0.6780(4) 1.0707(3) 0.4010(2) 0.0472(9) Uani 1 1 d . . . H38 H 0.7588 1.0706 0.4077 0.057 Uiso 1 1 calc R . . C39 C 0.6626(4) 1.0153(3) 0.3402(2) 0.0506(9) Uani 1 1 d . . . H39 H 0.7323 0.9767 0.3050 0.061 Uiso 1 1 calc R . . C40 C 0.5424(4) 1.0177(3) 0.3321(2) 0.0474(9) Uani 1 1 d . . . H40 H 0.5318 0.9811 0.2901 0.057 Uiso 1 1 calc R . . C41 C 0.5620(3) 0.5769(3) 0.0938(2) 0.0483(9) Uani 1 1 d . . . H41 H 0.5373 0.5705 0.1441 0.058 Uiso 1 1 calc R . . C42 C 0.6848(4) 0.5132(3) 0.0636(3) 0.0645(13) Uani 1 1 d . . . H42 H 0.7423 0.4639 0.0927 0.077 Uiso 1 1 calc R . . C43 C 0.7212(4) 0.5235(4) -0.0100(3) 0.0735(15) Uani 1 1 d . . . H43 H 0.8039 0.4805 -0.0318 0.088 Uiso 1 1 calc R . . C44 C 0.6352(4) 0.5974(4) -0.0515(3) 0.0629(12) Uani 1 1 d . . . H44 H 0.6595 0.6059 -0.1016 0.075 Uiso 1 1 calc R . . C45 C 0.5119(3) 0.6597(3) -0.01859(19) 0.0396(8) Uani 1 1 d . . . C46 C 0.4104(4) 0.7354(3) -0.06073(18) 0.0419(8) Uani 1 1 d . . . C47 C 0.4354(5) 0.7595(5) -0.1351(2) 0.0784(14) Uani 1 1 d . . . H47 H 0.5180 0.7322 -0.1607 0.094 Uiso 1 1 calc R . . C48 C 0.3331(8) 0.8254(6) -0.1699(3) 0.103(2) Uani 1 1 d . . . H48 H 0.3470 0.8411 -0.2200 0.124 Uiso 1 1 calc R . . C49 C 0.2137(6) 0.8673(5) -0.1327(3) 0.0830(17) Uani 1 1 d . . . H49 H 0.1458 0.9134 -0.1562 0.100 Uiso 1 1 calc R . . C50 C 0.1944(4) 0.8405(3) -0.0591(2) 0.0538(10) Uani 1 1 d . . . H50 H 0.1121 0.8679 -0.0330 0.065 Uiso 1 1 calc R . . N1 N 0.2317(2) 1.1585(2) 0.48407(14) 0.0340(6) Uani 1 1 d . . . N2 N 0.4392(3) 1.0702(2) 0.38186(14) 0.0339(6) Uani 1 1 d . . . N3 N 0.4760(2) 0.6481(2) 0.05360(15) 0.0354(6) Uani 1 1 d . . . N4 N 0.2917(3) 0.7758(2) -0.02421(14) 0.0369(6) Uani 1 1 d . . . O1 O 0.2299(3) 1.2382(2) 0.28034(15) 0.0712(9) Uani 1 1 d . . . O2 O 0.2434(2) 1.05406(18) 0.24544(11) 0.0311(5) Uani 1 1 d . . . O3 O 0.1572(2) 0.95426(18) 0.12553(11) 0.0358(5) Uani 1 1 d . . . O4 O 0.3437(2) 0.9666(2) 0.07191(13) 0.0461(6) Uani 1 1 d . . . O5 O 0.1328(2) 1.13835(19) -0.01925(11) 0.0334(5) Uani 1 1 d . . . O6 O -0.0727(2) 1.2631(2) -0.10343(12) 0.0369(5) Uani 1 1 d . . . O7 O 0.0060(2) 1.1707(2) -0.21421(12) 0.0411(5) Uani 1 1 d . . . O8 O 0.1631(2) 0.90178(18) 0.36930(11) 0.0366(5) Uani 1 1 d . . . O9 O 0.3641(2) 0.8156(2) 0.38690(13) 0.0500(6) Uani 1 1 d . . . O10 O 0.28270(19) 0.76332(18) 0.23234(11) 0.0296(5) Uani 1 1 d . . . O11 O 0.2930(3) 0.5842(2) 0.18988(12) 0.0460(6) Uani 1 1 d . . . O12 O 0.1937(2) 0.71785(18) 0.51142(11) 0.0385(5) Uani 1 1 d . . . O13 O 0.0512(2) 0.89506(19) 0.70434(12) 0.0402(5) Uani 1 1 d . . . O14 O -0.0258(2) 0.8254(2) 0.61507(14) 0.0515(7) Uani 1 1 d . . . Cd1 Cd 0.23907(2) 1.06418(2) 0.372967(12) 0.03126(7) Uani 1 1 d . . . Cd2 Cd 0.10542(2) 0.940489(18) 0.250642(11) 0.02652(6) Uani 1 1 d . . . Cd3 Cd 0.26896(2) 0.751604(19) 0.101938(11) 0.02762(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 C1 0.051(2) 0.0319(17) 0.0303(17) 0.0014(14) -0.0133(15) -0.0175(15) C2 0.0420(19) 0.0308(16) 0.0221(15) 0.0014(13) -0.0147(14) -0.0111(15) C3 0.0272(15) 0.0273(15) 0.0262(15) 0.0014(12) -0.0065(12) -0.0126(12) C4 0.0374(18) 0.0311(16) 0.0271(16) 0.0046(13) -0.0079(13) -0.0166(14) C5 0.048(2) 0.0298(16) 0.0325(18) -0.0039(14) -0.0049(15) -0.0118(15) C6 0.049(2) 0.0253(16) 0.048(2) 0.0041(15) -0.0095(17) -0.0037(15) C7 0.047(2) 0.0340(17) 0.0344(19) 0.0109(14) -0.0161(15) -0.0075(15) C8 0.0327(17) 0.0300(16) 0.0253(16) 0.0033(12) -0.0071(13) -0.0120(13) C9 0.0349(17) 0.0290(15) 0.0254(16) -0.0015(12) -0.0066(13) -0.0128(13) C10 0.0383(19) 0.0424(19) 0.041(2) 0.0024(15) -0.0204(16) -0.0111(15) C11 0.0287(18) 0.052(2) 0.050(2) -0.0104(17) -0.0058(16) -0.0138(16) C12 0.042(2) 0.065(2) 0.0347(19) -0.0066(17) 0.0043(15) -0.0295(18) C13 0.045(2) 0.058(2) 0.0221(16) 0.0019(15) -0.0075(14) -0.0237(17) C14 0.0320(16) 0.0291(15) 0.0235(15) -0.0026(12) -0.0076(12) -0.0108(13) C15 0.0345(17) 0.0263(15) 0.0279(16) 0.0041(13) -0.0095(13) -0.0137(13) C16 0.048(2) 0.0318(16) 0.0131(14) 0.0000(12) -0.0078(13) -0.0135(15) C17 0.0260(15) 0.0284(16) 0.0234(15) -0.0022(12) -0.0078(12) -0.0020(12) C18 0.0231(15) 0.0237(14) 0.0221(15) -0.0007(11) -0.0053(11) -0.0026(11) C19 0.0313(16) 0.0248(14) 0.0210(15) -0.0003(12) -0.0076(12) -0.0031(12) C20 0.059(2) 0.0275(16) 0.0297(17) -0.0007(13) -0.0144(15) -0.0144(15) C21 0.074(3) 0.0318(18) 0.041(2) 0.0073(15) -0.0161(18) -0.0222(18) C22 0.061(2) 0.0368(18) 0.0275(17) 0.0102(14) -0.0034(16) -0.0188(17) C23 0.0364(17) 0.0284(16) 0.0218(15) -0.0015(12) -0.0043(13) -0.0039(13) C24 0.0309(16) 0.0320(16) 0.0229(15) -0.0002(12) -0.0053(12) -0.0051(13) C25 0.0376(19) 0.053(2) 0.0343(19) -0.0137(16) -0.0013(15) 0.0031(16) C26 0.042(2) 0.065(3) 0.062(3) -0.023(2) -0.025(2) 0.0220(19) C27 0.075(3) 0.064(3) 0.045(2) -0.003(2) -0.036(2) 0.018(2) C28 0.056(2) 0.050(2) 0.0261(18) -0.0066(15) -0.0150(16) 0.0096(18) C29 0.0315(16) 0.0299(15) 0.0240(15) -0.0019(12) -0.0083(12) -0.0015(13) C30 0.0331(17) 0.0298(16) 0.0239(16) -0.0012(13) -0.0018(13) -0.0033(13) C31 0.038(2) 0.061(2) 0.037(2) -0.0016(17) -0.0127(16) -0.0114(17) C32 0.050(2) 0.058(2) 0.0316(19) -0.0029(17) -0.0031(16) -0.0034(19) C33 0.075(3) 0.043(2) 0.0254(18) -0.0040(15) -0.0106(18) -0.0157(19) C34 0.059(2) 0.0406(19) 0.0295(18) 0.0010(15) -0.0155(16) -0.0221(17) C35 0.0434(19) 0.0274(15) 0.0241(16) 0.0060(12) -0.0145(13) -0.0116(14) C36 0.0383(18) 0.0283(15) 0.0273(16) 0.0082(13) -0.0138(13) -0.0153(13) C37 0.048(2) 0.045(2) 0.042(2) 0.0029(16) -0.0168(17) -0.0239(17) C38 0.042(2) 0.048(2) 0.060(2) 0.0167(18) -0.0130(18) -0.0242(17) C39 0.046(2) 0.051(2) 0.052(2) 0.0073(18) 0.0008(18) -0.0142(18) C40 0.053(2) 0.052(2) 0.037(2) -0.0028(17) -0.0045(17) -0.0181(18) C41 0.037(2) 0.0390(19) 0.069(3) 0.0026(18) -0.0155(18) -0.0096(16) C42 0.033(2) 0.039(2) 0.122(4) -0.007(2) -0.019(2) -0.0075(17) C43 0.032(2) 0.051(3) 0.129(5) -0.034(3) 0.018(3) -0.012(2) C44 0.052(3) 0.062(3) 0.074(3) -0.034(2) 0.028(2) -0.031(2) C45 0.0380(19) 0.0364(18) 0.046(2) -0.0151(15) 0.0089(15) -0.0201(15) C46 0.062(2) 0.044(2) 0.0267(17) -0.0079(15) 0.0034(16) -0.0306(18) C47 0.102(4) 0.105(4) 0.036(2) 0.004(2) 0.009(2) -0.053(3) C48 0.172(7) 0.124(5) 0.038(3) 0.030(3) -0.023(4) -0.081(5) C49 0.142(5) 0.070(3) 0.057(3) 0.023(3) -0.055(3) -0.046(3) C50 0.080(3) 0.042(2) 0.045(2) 0.0022(17) -0.030(2) -0.018(2) N1 0.0367(15) 0.0377(14) 0.0274(14) -0.0020(11) -0.0124(12) -0.0082(12) N2 0.0395(16) 0.0380(15) 0.0281(14) -0.0020(12) -0.0091(12) -0.0159(12) N3 0.0313(15) 0.0354(14) 0.0378(16) -0.0060(12) -0.0018(12) -0.0095(12) N4 0.0501(18) 0.0356(15) 0.0286(14) -0.0023(12) -0.0102(13) -0.0166(13) O1 0.137(3) 0.0385(14) 0.0553(17) 0.0039(13) -0.0586(18) -0.0325(16) O2 0.0409(13) 0.0289(11) 0.0272(11) 0.0020(9) -0.0104(9) -0.0140(9) O3 0.0579(15) 0.0291(11) 0.0255(11) 0.0014(9) -0.0113(10) -0.0192(11) O4 0.0410(15) 0.0411(13) 0.0485(15) -0.0030(11) -0.0129(12) -0.0001(11) O5 0.0471(13) 0.0369(12) 0.0234(11) 0.0040(9) -0.0123(9) -0.0209(10) O6 0.0287(12) 0.0430(13) 0.0395(13) -0.0043(10) -0.0059(10) -0.0117(10) O7 0.0435(14) 0.0594(15) 0.0307(12) -0.0040(11) -0.0119(10) -0.0276(12) O8 0.0548(14) 0.0226(11) 0.0250(11) -0.0009(9) -0.0057(10) -0.0029(10) O9 0.0594(17) 0.0621(16) 0.0465(15) 0.0037(12) -0.0238(13) -0.0373(14) O10 0.0317(11) 0.0299(11) 0.0233(11) 0.0022(9) -0.0032(8) -0.0055(9) O11 0.0732(18) 0.0390(13) 0.0231(12) -0.0073(10) -0.0043(11) -0.0152(12) O12 0.0600(15) 0.0287(11) 0.0177(11) -0.0007(9) -0.0049(10) -0.0024(10) O13 0.0374(13) 0.0369(12) 0.0390(13) -0.0145(10) -0.0094(10) 0.0005(10) O14 0.0403(14) 0.0526(15) 0.0497(15) -0.0204(12) -0.0236(12) 0.0100(11) Cd1 0.03857(14) 0.03159(12) 0.02725(13) -0.00192(9) -0.01570(10) -0.01146(10) Cd2 0.02919(12) 0.02542(11) 0.02440(12) -0.00515(9) -0.00797(9) -0.00595(9) Cd3 0.02779(12) 0.03134(12) 0.02018(11) -0.00234(9) -0.00345(8) -0.00466(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.227(4) . ? C1 O2 1.283(4) . ? C1 C4 1.501(4) . ? C2 O4 1.210(4) . ? C2 O3 1.294(4) . ? C2 C3 1.516(4) . ? C3 C8 1.386(4) . ? C3 C4 1.405(4) . ? C4 C5 1.389(4) . ? C5 C6 1.387(4) . ? C5 H5 0.9300 . ? C6 C7 1.385(5) . ? C6 H6 0.9300 . ? C7 C8 1.380(4) . ? C7 H7 0.9300 . ? C8 O5 1.396(3) . ? C9 C10 1.382(4) . ? C9 O5 1.397(4) . ? C9 C14 1.403(4) . ? C10 C11 1.379(5) . ? C10 H10 0.9300 . ? C11 C12 1.376(5) . ? C11 H11 0.9300 . ? C12 C13 1.377(5) . ? C12 H12 0.9300 . ? C13 C14 1.387(4) . ? C13 H13 0.9300 . ? C14 C15 1.496(4) . ? C15 O6 1.244(4) . ? C15 O7 1.267(3) . ? C16 O9 1.221(4) . ? C16 O8 1.281(4) . ? C16 C18 1.513(4) . ? C17 O11 1.236(3) . ? C17 O10 1.282(3) . ? C17 C19 1.503(4) . ? C18 C23 1.394(4) . ? C18 C19 1.402(4) . ? C19 C20 1.389(4) . ? C20 C21 1.381(5) . ? C20 H20 0.9300 . ? C21 C22 1.384(5) . ? C21 H21 0.9300 . ? C22 C23 1.382(4) . ? C22 H22 0.9300 . ? C23 O12 1.385(3) . ? C24 C25 1.377(4) . ? C24 C29 1.385(4) . ? C24 O12 1.387(3) . ? C25 C26 1.382(5) . ? C25 H25 0.9300 . ? C26 C27 1.371(5) . ? C26 H26 0.9300 . ? C27 C28 1.373(5) . ? C27 H27 0.9300 . ? C28 C29 1.388(4) . ? C28 H28 0.9300 . ? C29 C30 1.510(4) . ? C30 O14 1.235(4) . ? C30 O13 1.267(3) . ? C31 N1 1.337(4) . ? C31 C32 1.376(5) . ? C31 H31 0.9300 . ? C32 C33 1.369(5) . ? C32 H32 0.9300 . ? C33 C34 1.385(5) . ? C33 H33 0.9300 . ? C34 C35 1.385(4) . ? C34 H34 0.9300 . ? C35 N1 1.341(4) . ? C35 C36 1.481(4) . ? C36 N2 1.342(4) . ? C36 C37 1.388(4) . ? C37 C38 1.370(5) . ? C37 H37 0.9300 . ? C38 C39 1.362(5) . ? C38 H38 0.9300 . ? C39 C40 1.368(5) . ? C39 H39 0.9300 . ? C40 N2 1.341(4) . ? C40 H40 0.9300 . ? C41 N3 1.342(4) . ? C41 C42 1.369(5) . ? C41 H41 0.9300 . ? C42 C43 1.365(7) . ? C42 H42 0.9300 . ? C43 C44 1.368(7) . ? C43 H43 0.9300 . ? C44 C45 1.384(5) . ? C44 H44 0.9300 . ? C45 N3 1.341(4) . ? C45 C46 1.489(5) . ? C46 N4 1.335(4) . ? C46 C47 1.390(5) . ? C47 C48 1.383(8) . ? C47 H47 0.9300 . ? C48 C49 1.346(8) . ? C48 H48 0.9300 . ? C49 C50 1.376(6) . ? C49 H49 0.9300 . ? C50 N4 1.341(4) . ? C50 H50 0.9300 . ? N1 Cd1 2.317(2) . ? N2 Cd1 2.295(3) . ? N3 Cd3 2.286(3) . ? N4 Cd3 2.307(3) . ? O1 Cd1 2.575(3) . ? O2 Cd2 2.322(2) . ? O2 Cd1 2.337(2) . ? O3 Cd3 2.280(2) . ? O3 Cd2 2.295(2) . ? O6 Cd3 2.256(2) 2_575 ? O7 Cd2 2.236(2) 2_575 ? O8 Cd1 2.304(2) . ? O8 Cd2 2.349(2) . ? O10 Cd2 2.326(2) . ? O10 Cd3 2.4294(19) . ? O11 Cd3 2.448(2) . ? O13 Cd2 2.200(2) 2_576 ? O14 Cd1 2.289(2) 2_576 ? Cd1 O14 2.289(2) 2_576 ? Cd1 Cd2 3.4504(3) . ? Cd2 O13 2.200(2) 2_576 ? Cd2 O7 2.236(2) 2_575 ? Cd2 Cd3 3.4359(3) . ? Cd3 O6 2.256(2) 2_575 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 O2 121.3(3) . . ? O1 C1 C4 119.3(3) . . ? O2 C1 C4 119.3(3) . . ? O4 C2 O3 124.8(3) . . ? O4 C2 C3 121.8(3) . . ? O3 C2 C3 113.3(3) . . ? C8 C3 C4 118.4(3) . . ? C8 C3 C2 118.0(2) . . ? C4 C3 C2 123.6(2) . . ? C5 C4 C3 119.8(3) . . ? C5 C4 C1 118.0(3) . . ? C3 C4 C1 122.2(3) . . ? C6 C5 C4 120.5(3) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? C7 C6 C5 119.9(3) . . ? C7 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? C8 C7 C6 119.4(3) . . ? C8 C7 H7 120.3 . . ? C6 C7 H7 120.3 . . ? C7 C8 C3 121.8(3) . . ? C7 C8 O5 119.8(3) . . ? C3 C8 O5 118.3(2) . . ? C10 C9 O5 119.5(3) . . ? C10 C9 C14 121.0(3) . . ? O5 C9 C14 119.3(3) . . ? C11 C10 C9 119.9(3) . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C12 C11 C10 120.2(3) . . ? C12 C11 H11 119.9 . . ? C10 C11 H11 119.9 . . ? C11 C12 C13 119.4(3) . . ? C11 C12 H12 120.3 . . ? C13 C12 H12 120.3 . . ? C12 C13 C14 122.2(3) . . ? C12 C13 H13 118.9 . . ? C14 C13 H13 118.9 . . ? C13 C14 C9 117.0(3) . . ? C13 C14 C15 118.3(3) . . ? C9 C14 C15 124.5(3) . . ? O6 C15 O7 126.5(3) . . ? O6 C15 C14 119.0(3) . . ? O7 C15 C14 114.5(3) . . ? O9 C16 O8 124.1(3) . . ? O9 C16 C18 120.3(3) . . ? O8 C16 C18 115.5(3) . . ? O11 C17 O10 121.0(3) . . ? O11 C17 C19 119.8(3) . . ? O10 C17 C19 119.2(2) . . ? C23 C18 C19 118.1(3) . . ? C23 C18 C16 117.7(2) . . ? C19 C18 C16 124.1(2) . . ? C20 C19 C18 120.2(3) . . ? C20 C19 C17 117.7(3) . . ? C18 C19 C17 122.1(3) . . ? C21 C20 C19 120.5(3) . . ? C21 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C20 C21 C22 120.0(3) . . ? C20 C21 H21 120.0 . . ? C22 C21 H21 120.0 . . ? C23 C22 C21 119.6(3) . . ? C23 C22 H22 120.2 . . ? C21 C22 H22 120.2 . . ? C22 C23 O12 121.3(3) . . ? C22 C23 C18 121.5(3) . . ? O12 C23 C18 117.0(3) . . ? C25 C24 C29 120.7(3) . . ? C25 C24 O12 120.3(3) . . ? C29 C24 O12 118.7(3) . . ? C24 C25 C26 120.2(3) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? C27 C26 C25 119.8(3) . . ? C27 C26 H26 120.1 . . ? C25 C26 H26 120.1 . . ? C26 C27 C28 119.5(3) . . ? C26 C27 H27 120.3 . . ? C28 C27 H27 120.3 . . ? C27 C28 C29 121.9(3) . . ? C27 C28 H28 119.1 . . ? C29 C28 H28 119.1 . . ? C24 C29 C28 117.7(3) . . ? C24 C29 C30 123.8(3) . . ? C28 C29 C30 118.5(3) . . ? O14 C30 O13 127.2(3) . . ? O14 C30 C29 118.2(3) . . ? O13 C30 C29 114.5(3) . . ? N1 C31 C32 122.8(3) . . ? N1 C31 H31 118.6 . . ? C32 C31 H31 118.6 . . ? C33 C32 C31 118.4(3) . . ? C33 C32 H32 120.8 . . ? C31 C32 H32 120.8 . . ? C32 C33 C34 119.5(3) . . ? C32 C33 H33 120.3 . . ? C34 C33 H33 120.3 . . ? C33 C34 C35 119.1(3) . . ? C33 C34 H34 120.5 . . ? C35 C34 H34 120.5 . . ? N1 C35 C34 121.1(3) . . ? N1 C35 C36 116.7(3) . . ? C34 C35 C36 122.1(3) . . ? N2 C36 C37 120.8(3) . . ? N2 C36 C35 116.5(3) . . ? C37 C36 C35 122.7(3) . . ? C38 C37 C36 119.5(3) . . ? C38 C37 H37 120.3 . . ? C36 C37 H37 120.3 . . ? C39 C38 C37 119.6(3) . . ? C39 C38 H38 120.2 . . ? C37 C38 H38 120.2 . . ? C38 C39 C40 118.6(4) . . ? C38 C39 H39 120.7 . . ? C40 C39 H39 120.7 . . ? N2 C40 C39 123.0(3) . . ? N2 C40 H40 118.5 . . ? C39 C40 H40 118.5 . . ? N3 C41 C42 122.4(4) . . ? N3 C41 H41 118.8 . . ? C42 C41 H41 118.8 . . ? C43 C42 C41 118.7(4) . . ? C43 C42 H42 120.7 . . ? C41 C42 H42 120.7 . . ? C42 C43 C44 119.6(4) . . ? C42 C43 H43 120.2 . . ? C44 C43 H43 120.2 . . ? C43 C44 C45 119.7(4) . . ? C43 C44 H44 120.2 . . ? C45 C44 H44 120.2 . . ? N3 C45 C44 120.6(4) . . ? N3 C45 C46 116.3(3) . . ? C44 C45 C46 123.0(4) . . ? N4 C46 C47 120.8(4) . . ? N4 C46 C45 116.7(3) . . ? C47 C46 C45 122.5(4) . . ? C48 C47 C46 117.8(5) . . ? C48 C47 H47 121.1 . . ? C46 C47 H47 121.1 . . ? C49 C48 C47 121.2(5) . . ? C49 C48 H48 119.4 . . ? C47 C48 H48 119.4 . . ? C48 C49 C50 118.6(5) . . ? C48 C49 H49 120.7 . . ? C50 C49 H49 120.7 . . ? N4 C50 C49 121.4(5) . . ? N4 C50 H50 119.3 . . ? C49 C50 H50 119.3 . . ? C31 N1 C35 119.0(3) . . ? C31 N1 Cd1 123.6(2) . . ? C35 N1 Cd1 116.8(2) . . ? C40 N2 C36 118.5(3) . . ? C40 N2 Cd1 123.5(2) . . ? C36 N2 Cd1 117.9(2) . . ? C45 N3 C41 119.0(3) . . ? C45 N3 Cd3 117.8(2) . . ? C41 N3 Cd3 123.2(2) . . ? C46 N4 C50 120.2(3) . . ? C46 N4 Cd3 116.7(2) . . ? C50 N4 Cd3 122.5(3) . . ? C1 O1 Cd1 86.6(2) . . ? C1 O2 Cd2 126.6(2) . . ? C1 O2 Cd1 96.18(18) . . ? Cd2 O2 Cd1 95.54(7) . . ? C2 O3 Cd3 106.18(19) . . ? C2 O3 Cd2 119.51(17) . . ? Cd3 O3 Cd2 97.34(8) . . ? C8 O5 C9 114.3(2) . . ? C15 O6 Cd3 121.15(19) . 2_575 ? C15 O7 Cd2 136.2(2) . 2_575 ? C16 O8 Cd1 102.91(19) . . ? C16 O8 Cd2 118.67(17) . . ? Cd1 O8 Cd2 95.71(7) . . ? C17 O10 Cd2 123.70(18) . . ? C17 O10 Cd3 91.67(16) . . ? Cd2 O10 Cd3 92.49(7) . . ? C17 O11 Cd3 91.94(18) . . ? C23 O12 C24 117.7(2) . . ? C30 O13 Cd2 130.47(19) . 2_576 ? C30 O14 Cd1 132.1(2) . 2_576 ? O14 Cd1 N2 145.39(9) 2_576 . ? O14 Cd1 O8 82.12(9) 2_576 . ? N2 Cd1 O8 131.43(8) . . ? O14 Cd1 N1 84.52(8) 2_576 . ? N2 Cd1 N1 71.28(9) . . ? O8 Cd1 N1 120.80(8) . . ? O14 Cd1 O2 89.25(8) 2_576 . ? N2 Cd1 O2 102.34(8) . . ? O8 Cd1 O2 81.80(7) . . ? N1 Cd1 O2 155.22(8) . . ? O14 Cd1 O1 76.68(11) 2_576 . ? N2 Cd1 O1 84.69(10) . . ? O8 Cd1 O1 129.16(7) . . ? N1 Cd1 O1 102.59(8) . . ? O2 Cd1 O1 52.64(7) . . ? O14 Cd1 Cd2 72.27(6) 2_576 . ? N2 Cd1 Cd2 136.03(6) . . ? O8 Cd1 Cd2 42.64(5) . . ? N1 Cd1 Cd2 152.39(7) . . ? O2 Cd1 Cd2 42.06(5) . . ? O1 Cd1 Cd2 86.73(5) . . ? O13 Cd2 O7 100.36(9) 2_576 2_575 ? O13 Cd2 O3 110.93(8) 2_576 . ? O7 Cd2 O3 81.60(8) 2_575 . ? O13 Cd2 O2 88.37(8) 2_576 . ? O7 Cd2 O2 160.40(8) 2_575 . ? O3 Cd2 O2 78.89(7) . . ? O13 Cd2 O10 165.96(7) 2_576 . ? O7 Cd2 O10 86.80(8) 2_575 . ? O3 Cd2 O10 81.91(7) . . ? O2 Cd2 O10 88.65(7) . . ? O13 Cd2 O8 88.84(8) 2_576 . ? O7 Cd2 O8 116.22(8) 2_575 . ? O3 Cd2 O8 151.29(8) . . ? O2 Cd2 O8 81.18(7) . . ? O10 Cd2 O8 77.14(7) . . ? O13 Cd2 Cd3 149.08(6) 2_576 . ? O7 Cd2 Cd3 67.59(6) 2_575 . ? O3 Cd2 Cd3 41.17(5) . . ? O2 Cd2 Cd3 96.02(5) . . ? O10 Cd2 Cd3 44.94(5) . . ? O8 Cd2 Cd3 122.08(5) . . ? O13 Cd2 Cd1 76.19(6) 2_576 . ? O7 Cd2 Cd1 156.85(6) 2_575 . ? O3 Cd2 Cd1 121.24(5) . . ? O2 Cd2 Cd1 42.40(5) . . ? O10 Cd2 Cd1 92.45(5) . . ? O8 Cd2 Cd1 41.65(5) . . ? Cd3 Cd2 Cd1 125.982(9) . . ? O6 Cd3 O3 83.28(8) 2_575 . ? O6 Cd3 N3 138.87(8) 2_575 . ? O3 Cd3 N3 133.26(9) . . ? O6 Cd3 N4 91.30(9) 2_575 . ? O3 Cd3 N4 93.33(8) . . ? N3 Cd3 N4 71.55(10) . . ? O6 Cd3 O10 102.57(7) 2_575 . ? O3 Cd3 O10 80.00(7) . . ? N3 Cd3 O10 102.18(8) . . ? N4 Cd3 O10 163.68(8) . . ? O6 Cd3 O11 83.50(8) 2_575 . ? O3 Cd3 O11 126.79(7) . . ? N3 Cd3 O11 85.53(9) . . ? N4 Cd3 O11 138.25(8) . . ? O10 Cd3 O11 53.41(7) . . ? O6 Cd3 Cd2 79.96(6) 2_575 . ? O3 Cd3 Cd2 41.49(5) . . ? N3 Cd3 Cd2 138.38(6) . . ? N4 Cd3 Cd2 134.46(7) . . ? O10 Cd3 Cd2 42.57(5) . . ? O11 Cd3 Cd2 85.45(5) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.663 _refine_diff_density_min -0.485 _refine_diff_density_rms 0.069 #===END data_6 _database_code_depnum_ccdc_archive 'CCDC 746382' #TrackingRef 'complexes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H36 Cd3 N4 O17' _chemical_formula_weight 1350.07 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 Cc _symmetry_space_group_name_Hall 'C -2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 14.0039(5) _cell_length_b 28.8677(11) _cell_length_c 13.6293(5) _cell_angle_alpha 90.00 _cell_angle_beta 118.5460(10) _cell_angle_gamma 90.00 _cell_volume 4840.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 8368 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.853 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2672 _exptl_absorpt_coefficient_mu 1.390 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7880 _exptl_absorpt_correction_T_max 0.8510 _exptl_absorpt_process_details '(SADABS; Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 0 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 12013 _diffrn_reflns_av_R_equivalents 0.0169 _diffrn_reflns_av_sigmaI/netI 0.0226 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5519 _reflns_number_gt 5369 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'SAINT-Plus (Bruker, 2001)' _computing_data_reduction SAINT-Plus _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Sheldrick, 1998)' _computing_publication_material XP _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^)+(0.0352P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.41(2) _refine_ls_number_reflns 5519 _refine_ls_number_parameters 699 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.0184 _refine_ls_R_factor_gt 0.0172 _refine_ls_wR_factor_ref 0.0555 _refine_ls_wR_factor_gt 0.0462 _refine_ls_goodness_of_fit_ref 1.150 _refine_ls_restrained_S_all 1.149 _refine_ls_shift/su_max 0.025 _refine_ls_shift/su_mean 0.003 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 1.3252(3) 0.12627(15) 0.9805(4) 0.0273(9) Uani 1 1 d . . . C2 C 1.2278(3) 0.11631(16) 0.8839(4) 0.0329(10) Uani 1 1 d . . . C3 C 1.2121(4) 0.1317(2) 0.7816(4) 0.0465(13) Uani 1 1 d . . . H3 H 1.1477 0.1248 0.7174 0.056 Uiso 1 1 calc R . . C4 C 1.2924(5) 0.1576(2) 0.7737(5) 0.0562(15) Uani 1 1 d . . . H4 H 1.2827 0.1669 0.7042 0.067 Uiso 1 1 calc R . . C5 C 1.3862(4) 0.16930(18) 0.8695(5) 0.0450(13) Uani 1 1 d . . . H5 H 1.4381 0.1881 0.8655 0.054 Uiso 1 1 calc R . . C6 C 1.4019(3) 0.15295(16) 0.9706(4) 0.0313(10) Uani 1 1 d . . . C7 C 1.3473(3) 0.10818(16) 1.0935(4) 0.0295(10) Uani 1 1 d . . . C8 C 1.1322(4) 0.09526(16) 0.8915(4) 0.0354(11) Uani 1 1 d . . . C9 C 1.5065(4) 0.20042(15) 1.1310(4) 0.0297(10) Uani 1 1 d . . . C10 C 1.6079(4) 0.21097(17) 1.2165(4) 0.0363(11) Uani 1 1 d . . . H10 H 1.6689 0.1955 1.2227 0.044 Uiso 1 1 calc R . . C11 C 1.6187(4) 0.24449(17) 1.2928(4) 0.0350(10) Uani 1 1 d . . . H11 H 1.6871 0.2514 1.3513 0.042 Uiso 1 1 calc R . . C12 C 1.5276(4) 0.26818(15) 1.2831(4) 0.0310(10) Uani 1 1 d . . . C13 C 1.4285(4) 0.25868(15) 1.1952(4) 0.0314(10) Uani 1 1 d . . . H13 H 1.3680 0.2748 1.1878 0.038 Uiso 1 1 calc R . . C14 C 1.4158(3) 0.22565(15) 1.1165(4) 0.0317(10) Uani 1 1 d . . . H14 H 1.3480 0.2203 1.0551 0.038 Uiso 1 1 calc R . . C15 C 1.5383(4) 0.30100(15) 1.3740(4) 0.0318(10) Uani 1 1 d . . . C16 C 1.1248(3) 0.13222(14) 1.3548(4) 0.0282(9) Uani 1 1 d . . . C17 C 1.0212(3) 0.13947(14) 1.2636(4) 0.0277(9) Uani 1 1 d . . . C18 C 0.9470(4) 0.16595(15) 1.2811(4) 0.0332(11) Uani 1 1 d . . . C19 C 0.9747(4) 0.18459(17) 1.3845(4) 0.0405(11) Uani 1 1 d . . . H19 H 0.9243 0.2023 1.3943 0.049 Uiso 1 1 calc R . . C20 C 1.0768(5) 0.17707(18) 1.4735(4) 0.0434(12) Uani 1 1 d . . . H20 H 1.0954 0.1896 1.5432 0.052 Uiso 1 1 calc R . . C21 C 1.1507(4) 0.15090(18) 1.4583(4) 0.0406(11) Uani 1 1 d . . . H21 H 1.2192 0.1456 1.5185 0.049 Uiso 1 1 calc R . . C22 C 1.2103(4) 0.10557(15) 1.3411(4) 0.0331(11) Uani 1 1 d . . . C23 C 0.9851(3) 0.11836(15) 1.1497(4) 0.0293(10) Uani 1 1 d . . . C24 C 0.8173(4) 0.19851(15) 1.1054(4) 0.0307(10) Uani 1 1 d . . . C25 C 0.7132(4) 0.19363(15) 1.0161(4) 0.0326(10) Uani 1 1 d . . . H25 H 0.6630 0.1740 1.0212 0.039 Uiso 1 1 calc R . . C26 C 0.6858(4) 0.21843(16) 0.9199(4) 0.0338(10) Uani 1 1 d . . . H26 H 0.6163 0.2155 0.8596 0.041 Uiso 1 1 calc R . . C27 C 0.7595(4) 0.24751(16) 0.9112(4) 0.0313(10) Uani 1 1 d . . . C28 C 0.8610(4) 0.25316(15) 1.0037(4) 0.0339(10) Uani 1 1 d . . . H28 H 0.9103 0.2736 0.9996 0.041 Uiso 1 1 calc R . . C29 C 0.8907(4) 0.22916(17) 1.1018(4) 0.0360(11) Uani 1 1 d . . . H29 H 0.9586 0.2336 1.1637 0.043 Uiso 1 1 calc R . . C31 C 1.5393(4) 0.15086(17) 1.4143(5) 0.0432(12) Uani 1 1 d . . . H31 H 1.4794 0.1699 1.3746 0.052 Uiso 1 1 calc R . . C32 C 1.6411(5) 0.17150(17) 1.4834(5) 0.0489(14) Uani 1 1 d . . . H32 H 1.6471 0.2035 1.4920 0.059 Uiso 1 1 calc R . . C33 C 1.7291(4) 0.14440(18) 1.5366(5) 0.0462(13) Uani 1 1 d . . . H33 H 1.7970 0.1578 1.5799 0.055 Uiso 1 1 calc R . . C34 C 1.7193(4) 0.09557(16) 1.5273(4) 0.0334(11) Uani 1 1 d . . . C35 C 1.8091(4) 0.06491(18) 1.5836(4) 0.0402(12) Uani 1 1 d . . . H35 H 1.8784 0.0771 1.6267 0.048 Uiso 1 1 calc R . . C36 C 1.7956(4) 0.01901(19) 1.5754(4) 0.0410(12) Uani 1 1 d . . . H36 H 1.8557 -0.0002 1.6118 0.049 Uiso 1 1 calc R . . C37 C 1.6895(4) -0.00109(16) 1.5112(4) 0.0347(10) Uani 1 1 d . . . C38 C 1.6717(4) -0.04901(17) 1.5031(5) 0.0428(12) Uani 1 1 d . . . H38 H 1.7299 -0.0694 1.5377 0.051 Uiso 1 1 calc R . . C39 C 1.5683(5) -0.06553(17) 1.4439(5) 0.0455(12) Uani 1 1 d . . . H39 H 1.5552 -0.0972 1.4393 0.055 Uiso 1 1 calc R . . C40 C 1.4829(4) -0.03469(17) 1.3909(5) 0.0429(12) Uani 1 1 d . . . H40 H 1.4128 -0.0464 1.3506 0.052 Uiso 1 1 calc R . . C41 C 1.5987(3) 0.02797(15) 1.4537(4) 0.0271(9) Uani 1 1 d . . . C42 C 1.6140(3) 0.07769(15) 1.4606(4) 0.0273(9) Uani 1 1 d . . . C43 C 0.9655(5) -0.01126(17) 0.9253(5) 0.0478(13) Uani 1 1 d . . . H43 H 1.0396 -0.0063 0.9700 0.057 Uiso 1 1 calc R . . C44 C 0.9279(5) -0.05675(18) 0.8987(5) 0.0546(15) Uani 1 1 d . . . H44 H 0.9763 -0.0814 0.9257 0.065 Uiso 1 1 calc R . . C45 C 0.8203(5) -0.06464(19) 0.8334(5) 0.0548(15) Uani 1 1 d . . . H45 H 0.7946 -0.0948 0.8146 0.066 Uiso 1 1 calc R . . C46 C 0.7475(4) -0.02712(17) 0.7942(4) 0.0400(12) Uani 1 1 d . . . C47 C 0.6333(5) -0.0322(2) 0.7254(5) 0.0501(15) Uani 1 1 d . . . H47 H 0.6035 -0.0617 0.7070 0.060 Uiso 1 1 calc R . . C48 C 0.5675(5) 0.0049(2) 0.6865(5) 0.0510(15) Uani 1 1 d . . . H48 H 0.4930 0.0006 0.6428 0.061 Uiso 1 1 calc R . . C49 C 0.6100(4) 0.0505(2) 0.7110(4) 0.0416(12) Uani 1 1 d . . . C50 C 0.5450(4) 0.0916(2) 0.6691(5) 0.0544(15) Uani 1 1 d . . . H50 H 0.4703 0.0891 0.6236 0.065 Uiso 1 1 calc R . . C51 C 0.5921(5) 0.1338(2) 0.6956(5) 0.0564(15) Uani 1 1 d . . . H51 H 0.5505 0.1605 0.6680 0.068 Uiso 1 1 calc R . . C52 C 0.7030(5) 0.13671(19) 0.7644(5) 0.0460(13) Uani 1 1 d . . . H52 H 0.7346 0.1660 0.7822 0.055 Uiso 1 1 calc R . . C53 C 0.7222(4) 0.05763(16) 0.7813(4) 0.0305(10) Uani 1 1 d . . . C54 C 0.7922(4) 0.01776(16) 0.8231(4) 0.0327(10) Uani 1 1 d . . . C30 C 0.7308(4) 0.27280(16) 0.8044(4) 0.0340(10) Uiso 1 1 d . . . N1 N 1.5258(3) 0.10519(12) 1.4036(3) 0.0327(8) Uani 1 1 d . . . N2 N 1.4971(3) 0.01143(12) 1.3952(3) 0.0334(9) Uani 1 1 d . . . N3 N 0.8997(3) 0.02507(13) 0.8892(3) 0.0338(9) Uani 1 1 d . . . N4 N 0.7671(3) 0.09992(13) 0.8066(3) 0.0333(9) Uani 1 1 d . . . O1 O 1.3765(3) 0.06661(11) 1.1178(3) 0.0442(9) Uani 1 1 d . . . O2 O 1.3381(2) 0.13481(11) 1.1609(3) 0.0322(7) Uani 1 1 d . . . O3 O 1.1352(3) 0.09600(11) 0.9852(3) 0.0384(8) Uani 1 1 d . . . O4 O 1.0523(3) 0.08170(14) 0.8052(3) 0.0536(10) Uani 1 1 d . . . O5 O 1.5009(3) 0.16299(11) 1.0656(3) 0.0367(8) Uani 1 1 d . . . O6 O 1.6245(3) 0.29763(11) 1.4664(3) 0.0379(8) Uani 1 1 d . . . O7 O 1.4606(3) 0.32814(11) 1.3510(3) 0.0441(9) Uani 1 1 d . . . O8 O 1.2916(3) 0.08951(13) 1.4247(3) 0.0463(9) Uani 1 1 d . . . O9 O 1.1983(3) 0.10132(10) 1.2432(3) 0.0329(7) Uani 1 1 d . . . O10 O 1.0024(3) 0.14168(11) 1.0812(3) 0.0325(7) Uani 1 1 d . . . O11 O 0.9385(3) 0.08034(13) 1.1269(3) 0.0473(9) Uani 1 1 d . . . O12 O 0.8402(3) 0.17040(12) 1.1971(3) 0.0409(8) Uani 1 1 d . . . O13 O 0.6465(3) 0.26221(14) 0.7172(3) 0.0522(10) Uani 1 1 d . . . O14 O 0.7921(3) 0.30462(12) 0.8052(3) 0.0469(9) Uani 1 1 d . . . O15 O 1.2612(3) 0.00135(14) 1.2233(4) 0.0725(14) Uani 1 1 d D . . H15B H 1.1982 -0.0013 1.2171 0.109 Uiso 1 1 d RD . . H15A H 1.2595 0.0205 1.1741 0.109 Uiso 1 1 d RD . . Cd1 Cd 1.36399(2) 0.067416(11) 1.28883(3) 0.03289(9) Uani 1 1 d . . . Cd2 Cd 0.95173(2) 0.101566(11) 0.92261(2) 0.03106(8) Uani 1 1 d . . . Cd3 Cd 0.67527(2) 0.331389(10) 0.62831(2) 0.02688(8) Uani 1 1 d . . . O16 O 1.2464(6) -0.0145(2) 1.0218(7) 0.133(3) Uani 1 1 d D . . H16B H 1.2761 -0.0395 1.0171 0.200 Uiso 1 1 d RD . . H16A H 1.2930 0.0073 1.0440 0.200 Uiso 1 1 d RD . . O17 O 1.0758(5) 0.0035(2) 1.2281(8) 0.149(4) Uani 1 1 d D . . H17A H 1.0712 -0.0183 1.2684 0.223 Uiso 1 1 d RD . . H17B H 1.0782 -0.0087 1.1732 0.223 Uiso 1 1 d RD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.023(2) 0.032(2) 0.024(2) -0.0076(18) 0.0089(19) 0.0030(17) C2 0.025(2) 0.037(2) 0.032(3) -0.010(2) 0.010(2) -0.0014(19) C3 0.034(3) 0.074(4) 0.022(2) -0.013(2) 0.005(2) -0.009(2) C4 0.048(3) 0.089(4) 0.032(3) 0.003(3) 0.019(3) -0.006(3) C5 0.038(3) 0.060(3) 0.040(3) -0.005(2) 0.022(3) -0.010(2) C6 0.025(2) 0.040(2) 0.027(2) -0.013(2) 0.011(2) -0.0020(18) C7 0.015(2) 0.040(3) 0.028(2) -0.004(2) 0.0056(18) 0.0028(17) C8 0.024(2) 0.034(2) 0.041(3) -0.006(2) 0.009(2) 0.0005(19) C9 0.024(2) 0.038(2) 0.025(2) -0.0065(19) 0.0103(19) -0.0069(18) C10 0.028(2) 0.050(3) 0.032(3) -0.013(2) 0.015(2) -0.002(2) C11 0.026(2) 0.045(3) 0.030(2) -0.009(2) 0.0104(19) -0.0049(19) C12 0.039(2) 0.030(2) 0.025(2) -0.0003(19) 0.015(2) -0.0039(19) C13 0.032(2) 0.027(2) 0.032(3) 0.0015(19) 0.013(2) 0.0034(18) C14 0.025(2) 0.037(2) 0.026(2) -0.0031(19) 0.0069(19) 0.0002(18) C15 0.035(2) 0.030(2) 0.029(2) -0.0049(19) 0.014(2) -0.0072(19) C16 0.029(2) 0.030(2) 0.024(2) 0.0064(18) 0.0111(19) -0.0023(18) C17 0.028(2) 0.033(2) 0.026(2) 0.0052(18) 0.017(2) -0.0038(18) C18 0.029(2) 0.037(3) 0.033(3) 0.013(2) 0.014(2) 0.0043(19) C19 0.048(3) 0.042(3) 0.042(3) 0.002(2) 0.029(3) 0.008(2) C20 0.052(3) 0.051(3) 0.026(3) -0.004(2) 0.018(2) -0.001(2) C21 0.039(3) 0.054(3) 0.023(2) 0.004(2) 0.009(2) 0.002(2) C22 0.028(2) 0.031(2) 0.040(3) 0.005(2) 0.016(2) -0.0014(18) C23 0.021(2) 0.036(2) 0.026(2) 0.005(2) 0.0073(19) 0.0024(18) C24 0.030(2) 0.033(2) 0.031(3) 0.006(2) 0.017(2) 0.0063(18) C25 0.028(2) 0.036(2) 0.037(3) 0.003(2) 0.017(2) -0.0028(18) C26 0.023(2) 0.043(3) 0.031(2) 0.002(2) 0.008(2) 0.0024(18) C27 0.031(2) 0.032(2) 0.030(2) 0.0042(19) 0.015(2) 0.0046(18) C28 0.031(2) 0.031(2) 0.038(3) 0.009(2) 0.015(2) -0.0014(19) C29 0.023(2) 0.043(3) 0.032(3) 0.007(2) 0.005(2) 0.0006(19) C31 0.043(3) 0.032(2) 0.040(3) 0.004(2) 0.009(2) 0.005(2) C32 0.053(3) 0.037(3) 0.044(3) 0.002(2) 0.013(3) -0.006(2) C33 0.042(3) 0.049(3) 0.039(3) -0.006(2) 0.012(3) -0.014(2) C34 0.029(2) 0.040(3) 0.025(2) 0.000(2) 0.008(2) -0.0032(19) C35 0.022(2) 0.061(3) 0.030(3) -0.002(2) 0.007(2) 0.000(2) C36 0.026(2) 0.057(3) 0.033(3) 0.002(2) 0.009(2) 0.010(2) C37 0.036(2) 0.042(3) 0.029(2) 0.007(2) 0.018(2) 0.009(2) C38 0.051(3) 0.042(3) 0.040(3) 0.011(2) 0.026(3) 0.015(2) C39 0.052(3) 0.033(2) 0.052(3) 0.005(2) 0.025(3) 0.003(2) C40 0.041(3) 0.041(3) 0.043(3) 0.001(2) 0.017(2) -0.007(2) C41 0.022(2) 0.039(2) 0.020(2) 0.0034(18) 0.0097(18) 0.0025(17) C42 0.029(2) 0.032(2) 0.022(2) 0.0045(18) 0.0131(19) 0.0038(18) C43 0.043(3) 0.050(3) 0.052(3) -0.004(3) 0.024(3) 0.003(2) C44 0.068(4) 0.041(3) 0.062(4) -0.002(3) 0.038(4) 0.012(3) C45 0.084(5) 0.040(3) 0.057(4) -0.015(3) 0.046(4) -0.014(3) C46 0.053(3) 0.042(3) 0.034(3) -0.011(2) 0.028(2) -0.017(2) C47 0.058(4) 0.061(4) 0.037(3) -0.020(3) 0.027(3) -0.037(3) C48 0.039(3) 0.080(4) 0.031(3) -0.010(3) 0.014(2) -0.032(3) C49 0.028(2) 0.069(3) 0.026(3) -0.006(2) 0.011(2) -0.007(2) C50 0.028(3) 0.095(5) 0.034(3) 0.004(3) 0.010(2) 0.009(3) C51 0.045(3) 0.070(4) 0.045(3) 0.002(3) 0.014(3) 0.018(3) C52 0.050(3) 0.047(3) 0.042(3) -0.003(2) 0.023(3) 0.004(2) C53 0.029(2) 0.043(3) 0.018(2) -0.0080(19) 0.0094(19) -0.0041(19) C54 0.034(3) 0.043(3) 0.027(2) -0.010(2) 0.020(2) -0.009(2) N1 0.028(2) 0.036(2) 0.028(2) 0.0050(17) 0.0088(17) 0.0032(15) N2 0.032(2) 0.0319(19) 0.037(2) 0.0025(17) 0.0175(19) 0.0025(16) N3 0.032(2) 0.035(2) 0.032(2) -0.0037(17) 0.0129(18) -0.0036(16) N4 0.031(2) 0.035(2) 0.031(2) -0.0030(17) 0.0122(18) -0.0012(16) O1 0.043(2) 0.040(2) 0.039(2) 0.0014(16) 0.0123(17) 0.0131(15) O2 0.0330(17) 0.0371(17) 0.0282(17) -0.0043(14) 0.0158(15) 0.0024(13) O3 0.0268(17) 0.0457(19) 0.038(2) 0.0006(15) 0.0113(16) -0.0051(13) O4 0.031(2) 0.065(2) 0.052(3) -0.019(2) 0.0098(19) -0.0136(18) O5 0.0245(16) 0.0463(19) 0.0364(19) -0.0158(16) 0.0123(15) -0.0032(14) O6 0.0421(19) 0.0394(18) 0.0262(17) -0.0048(14) 0.0114(16) 0.0026(14) O7 0.041(2) 0.0399(18) 0.045(2) -0.0094(16) 0.0155(18) 0.0059(15) O8 0.0297(18) 0.059(2) 0.039(2) 0.0131(18) 0.0069(17) 0.0128(16) O9 0.0349(18) 0.0330(16) 0.0329(19) 0.0030(14) 0.0179(16) 0.0044(13) O10 0.0302(17) 0.0411(18) 0.0241(17) -0.0010(14) 0.0112(14) -0.0029(14) O11 0.044(2) 0.046(2) 0.044(2) -0.0067(17) 0.0146(18) -0.0191(18) O12 0.0278(17) 0.056(2) 0.037(2) 0.0216(16) 0.0141(16) 0.0088(14) O13 0.042(2) 0.068(2) 0.036(2) 0.0177(19) 0.0099(17) 0.0013(18) O14 0.053(2) 0.045(2) 0.041(2) 0.0126(16) 0.0216(18) -0.0008(16) O15 0.037(2) 0.051(2) 0.099(4) -0.011(2) 0.008(2) -0.0035(18) Cd1 0.02266(15) 0.03821(18) 0.03054(18) 0.00277(14) 0.00685(13) 0.00405(13) Cd2 0.02651(16) 0.03275(16) 0.02862(17) -0.00504(13) 0.00890(14) -0.00830(13) Cd3 0.02591(15) 0.02847(15) 0.02176(15) -0.00182(13) 0.00774(12) -0.00082(12) O16 0.116(5) 0.120(5) 0.171(7) -0.088(5) 0.074(5) -0.022(4) O17 0.066(4) 0.121(5) 0.247(10) 0.107(6) 0.065(5) 0.016(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C6 1.380(6) . ? C1 C2 1.401(6) . ? C1 C7 1.511(6) . ? C2 C3 1.377(7) . ? C2 C8 1.519(6) . ? C3 C4 1.396(8) . ? C3 H3 0.9300 . ? C4 C5 1.380(8) . ? C4 H4 0.9300 . ? C5 C6 1.371(7) . ? C5 H5 0.9300 . ? C6 O5 1.402(5) . ? C7 O2 1.251(6) . ? C7 O1 1.260(5) . ? C8 O4 1.237(6) . ? C8 O3 1.257(6) . ? C9 C10 1.373(6) . ? C9 O5 1.379(5) . ? C9 C14 1.395(6) . ? C10 C11 1.375(7) . ? C10 H10 0.9300 . ? C11 C12 1.397(7) . ? C11 H11 0.9300 . ? C12 C13 1.359(6) . ? C12 C15 1.509(6) . ? C13 C14 1.381(6) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 O7 1.253(6) . ? C15 O6 1.265(5) . ? C16 C21 1.387(7) . ? C16 C17 1.404(6) . ? C16 C22 1.509(6) . ? C17 C18 1.399(6) . ? C17 C23 1.512(6) . ? C18 C19 1.380(7) . ? C18 O12 1.388(6) . ? C19 C20 1.380(8) . ? C19 H19 0.9300 . ? C20 C21 1.374(7) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 O8 1.253(6) . ? C22 O9 1.267(6) . ? C23 O11 1.238(6) . ? C23 O10 1.265(5) . ? C24 C29 1.376(6) . ? C24 C25 1.389(7) . ? C24 O12 1.393(6) . ? C25 C26 1.379(6) . ? C25 H25 0.9300 . ? C26 C27 1.378(7) . ? C26 H26 0.9300 . ? C27 C28 1.387(7) . ? C27 C30 1.503(7) . ? C28 C29 1.381(7) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C31 N1 1.330(6) . ? C31 C32 1.410(8) . ? C31 H31 0.9300 . ? C32 C33 1.343(8) . ? C32 H32 0.9300 . ? C33 C34 1.416(7) . ? C33 H33 0.9300 . ? C34 C42 1.410(6) . ? C34 C35 1.425(7) . ? C35 C36 1.335(7) . ? C35 H35 0.9300 . ? C36 C37 1.438(7) . ? C36 H36 0.9300 . ? C37 C38 1.400(7) . ? C37 C41 1.408(6) . ? C38 C39 1.364(8) . ? C38 H38 0.9300 . ? C39 C40 1.385(7) . ? C39 H39 0.9300 . ? C40 N2 1.344(6) . ? C40 H40 0.9300 . ? C41 N2 1.343(6) . ? C41 C42 1.448(6) . ? C42 N1 1.357(5) . ? C43 N3 1.326(6) . ? C43 C44 1.397(8) . ? C43 H43 0.9300 . ? C44 C45 1.354(9) . ? C44 H44 0.9300 . ? C45 C46 1.406(8) . ? C45 H45 0.9300 . ? C46 C54 1.410(7) . ? C46 C47 1.423(8) . ? C47 C48 1.345(9) . ? C47 H47 0.9300 . ? C48 C49 1.417(8) . ? C48 H48 0.9300 . ? C49 C53 1.410(7) . ? C49 C50 1.437(8) . ? C50 C51 1.350(9) . ? C50 H50 0.9300 . ? C51 C52 1.381(8) . ? C51 H51 0.9300 . ? C52 N4 1.331(6) . ? C52 H52 0.9300 . ? C53 N4 1.341(6) . ? C53 C54 1.441(7) . ? C54 N3 1.352(6) . ? C30 O13 1.248(6) . ? C30 O14 1.253(6) . ? C30 Cd3 2.727(5) . ? N1 Cd1 2.321(4) . ? N2 Cd1 2.368(4) . ? N3 Cd2 2.301(4) . ? N4 Cd2 2.298(4) . ? O1 Cd1 2.420(4) . ? O2 Cd3 2.320(3) 4 ? O2 Cd1 2.520(3) . ? O3 Cd2 2.294(3) . ? O6 Cd3 2.197(3) 1_656 ? O7 Cd2 2.280(3) 4 ? O8 Cd1 2.581(4) . ? O9 Cd1 2.313(3) . ? O9 Cd3 2.418(3) 4 ? O10 Cd2 2.247(3) . ? O10 Cd3 2.322(3) 4 ? O13 Cd3 2.467(4) . ? O14 Cd3 2.306(4) . ? O15 Cd1 2.297(4) . ? O15 H15A 0.8598 . ? Cd1 H15A 2.0580 . ? Cd2 O7 2.280(3) 4_454 ? Cd3 O6 2.197(3) 1_454 ? Cd3 O2 2.320(3) 4_454 ? Cd3 O10 2.322(3) 4_454 ? Cd3 O9 2.418(3) 4_454 ? O16 H16B 0.8522 . ? O16 H16A 0.8517 . ? O17 H17A 0.8563 . ? O17 H17B 0.8423 . ? 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 C6 C1 C2 118.5(4) . . ? C6 C1 C7 120.2(4) . . ? C2 C1 C7 121.4(4) . . ? C3 C2 C1 119.9(4) . . ? C3 C2 C8 118.6(4) . . ? C1 C2 C8 120.8(4) . . ? C2 C3 C4 120.4(5) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? C5 C4 C3 119.7(5) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.2 . . ? C6 C5 C4 119.3(5) . . ? C6 C5 H5 120.3 . . ? C4 C5 H5 120.3 . . ? C5 C6 C1 122.1(4) . . ? C5 C6 O5 118.1(4) . . ? C1 C6 O5 119.8(4) . . ? O2 C7 O1 121.8(5) . . ? O2 C7 C1 119.5(4) . . ? O1 C7 C1 118.7(4) . . ? O4 C8 O3 123.2(5) . . ? O4 C8 C2 119.2(5) . . ? O3 C8 C2 117.4(4) . . ? C10 C9 O5 116.0(4) . . ? C10 C9 C14 120.5(4) . . ? O5 C9 C14 123.4(4) . . ? C9 C10 C11 119.5(4) . . ? C9 C10 H10 120.2 . . ? C11 C10 H10 120.2 . . ? C10 C11 C12 120.5(4) . . ? C10 C11 H11 119.7 . . ? C12 C11 H11 119.7 . . ? C13 C12 C11 119.0(4) . . ? C13 C12 C15 120.6(4) . . ? C11 C12 C15 120.1(4) . . ? C12 C13 C14 121.5(4) . . ? C12 C13 H13 119.2 . . ? C14 C13 H13 119.2 . . ? C13 C14 C9 118.6(4) . . ? C13 C14 H14 120.7 . . ? C9 C14 H14 120.7 . . ? O7 C15 O6 126.7(4) . . ? O7 C15 C12 117.0(4) . . ? O6 C15 C12 116.2(4) . . ? C21 C16 C17 120.0(4) . . ? C21 C16 C22 119.2(4) . . ? C17 C16 C22 120.8(4) . . ? C18 C17 C16 117.9(4) . . ? C18 C17 C23 118.9(4) . . ? C16 C17 C23 123.1(4) . . ? C19 C18 O12 118.2(4) . . ? C19 C18 C17 121.2(4) . . ? O12 C18 C17 120.3(4) . . ? C18 C19 C20 120.2(4) . . ? C18 C19 H19 119.9 . . ? C20 C19 H19 119.9 . . ? C21 C20 C19 119.5(5) . . ? C21 C20 H20 120.2 . . ? C19 C20 H20 120.2 . . ? C20 C21 C16 121.1(5) . . ? C20 C21 H21 119.4 . . ? C16 C21 H21 119.4 . . ? O8 C22 O9 121.9(4) . . ? O8 C22 C16 120.3(5) . . ? O9 C22 C16 117.8(4) . . ? O11 C23 O10 123.4(5) . . ? O11 C23 C17 119.5(4) . . ? O10 C23 C17 117.1(4) . . ? C29 C24 C25 121.6(4) . . ? C29 C24 O12 123.4(4) . . ? C25 C24 O12 115.0(4) . . ? C26 C25 C24 118.7(4) . . ? C26 C25 H25 120.7 . . ? C24 C25 H25 120.7 . . ? C27 C26 C25 121.2(4) . . ? C27 C26 H26 119.4 . . ? C25 C26 H26 119.4 . . ? C26 C27 C28 118.6(4) . . ? C26 C27 C30 121.0(4) . . ? C28 C27 C30 120.4(4) . . ? C29 C28 C27 121.6(4) . . ? C29 C28 H28 119.2 . . ? C27 C28 H28 119.2 . . ? C24 C29 C28 118.2(4) . . ? C24 C29 H29 120.9 . . ? C28 C29 H29 120.9 . . ? N1 C31 C32 122.5(5) . . ? N1 C31 H31 118.8 . . ? C32 C31 H31 118.8 . . ? C33 C32 C31 119.2(5) . . ? C33 C32 H32 120.4 . . ? C31 C32 H32 120.4 . . ? C32 C33 C34 120.5(5) . . ? C32 C33 H33 119.8 . . ? C34 C33 H33 119.8 . . ? C42 C34 C33 116.7(4) . . ? C42 C34 C35 120.1(4) . . ? C33 C34 C35 123.2(5) . . ? C36 C35 C34 121.2(5) . . ? C36 C35 H35 119.4 . . ? C34 C35 H35 119.4 . . ? C35 C36 C37 121.0(4) . . ? C35 C36 H36 119.5 . . ? C37 C36 H36 119.5 . . ? C38 C37 C41 117.7(5) . . ? C38 C37 C36 122.7(4) . . ? C41 C37 C36 119.6(4) . . ? C39 C38 C37 119.4(5) . . ? C39 C38 H38 120.3 . . ? C37 C38 H38 120.3 . . ? C38 C39 C40 119.5(5) . . ? C38 C39 H39 120.3 . . ? C40 C39 H39 120.3 . . ? N2 C40 C39 122.7(5) . . ? N2 C40 H40 118.6 . . ? C39 C40 H40 118.6 . . ? N2 C41 C37 122.5(4) . . ? N2 C41 C42 118.2(4) . . ? C37 C41 C42 119.2(4) . . ? N1 C42 C34 122.7(4) . . ? N1 C42 C41 118.5(4) . . ? C34 C42 C41 118.8(4) . . ? N3 C43 C44 122.6(5) . . ? N3 C43 H43 118.7 . . ? C44 C43 H43 118.7 . . ? C45 C44 C43 119.5(5) . . ? C45 C44 H44 120.3 . . ? C43 C44 H44 120.3 . . ? C44 C45 C46 119.8(5) . . ? C44 C45 H45 120.1 . . ? C46 C45 H45 120.1 . . ? C45 C46 C54 117.2(5) . . ? C45 C46 C47 123.6(5) . . ? C54 C46 C47 119.2(5) . . ? C48 C47 C46 121.3(5) . . ? C48 C47 H47 119.3 . . ? C46 C47 H47 119.3 . . ? C47 C48 C49 121.0(5) . . ? C47 C48 H48 119.5 . . ? C49 C48 H48 119.5 . . ? C53 C49 C48 120.1(5) . . ? C53 C49 C50 116.0(5) . . ? C48 C49 C50 123.9(5) . . ? C51 C50 C49 120.2(5) . . ? C51 C50 H50 119.9 . . ? C49 C50 H50 119.9 . . ? C50 C51 C52 118.9(6) . . ? C50 C51 H51 120.5 . . ? C52 C51 H51 120.5 . . ? N4 C52 C51 123.5(5) . . ? N4 C52 H52 118.2 . . ? C51 C52 H52 118.2 . . ? N4 C53 C49 122.7(5) . . ? N4 C53 C54 118.6(4) . . ? C49 C53 C54 118.6(4) . . ? N3 C54 C46 122.3(5) . . ? N3 C54 C53 118.0(4) . . ? C46 C54 C53 119.7(4) . . ? O13 C30 O14 121.4(5) . . ? O13 C30 C27 119.7(4) . . ? O14 C30 C27 118.9(4) . . ? O13 C30 Cd3 64.7(3) . . ? O14 C30 Cd3 57.3(3) . . ? C27 C30 Cd3 170.4(3) . . ? C31 N1 C42 118.3(4) . . ? C31 N1 Cd1 125.6(3) . . ? C42 N1 Cd1 116.1(3) . . ? C41 N2 C40 118.1(4) . . ? C41 N2 Cd1 115.0(3) . . ? C40 N2 Cd1 126.3(3) . . ? C43 N3 C54 118.6(4) . . ? C43 N3 Cd2 126.0(3) . . ? C54 N3 Cd2 115.3(3) . . ? C52 N4 C53 118.6(4) . . ? C52 N4 Cd2 125.9(3) . . ? C53 N4 Cd2 115.5(3) . . ? C7 O1 Cd1 94.6(3) . . ? C7 O2 Cd3 123.7(3) . 4 ? C7 O2 Cd1 90.1(3) . . ? Cd3 O2 Cd1 105.09(12) 4 . ? C8 O3 Cd2 97.8(3) . . ? C9 O5 C6 119.0(3) . . ? C15 O6 Cd3 131.5(3) . 1_656 ? C15 O7 Cd2 131.9(3) . 4 ? C22 O8 Cd1 86.3(3) . . ? C22 O9 Cd1 98.4(3) . . ? C22 O9 Cd3 120.9(3) . 4 ? Cd1 O9 Cd3 108.67(13) . 4 ? C23 O10 Cd2 110.6(3) . . ? C23 O10 Cd3 121.1(3) . 4 ? Cd2 O10 Cd3 104.30(13) . 4 ? C18 O12 C24 119.3(3) . . ? C30 O13 Cd3 88.1(3) . . ? C30 O14 Cd3 95.5(3) . . ? Cd1 O15 H15A 63.2 . . ? O15 Cd1 O9 83.41(13) . . ? O15 Cd1 N1 151.74(14) . . ? O9 Cd1 N1 120.90(12) . . ? O15 Cd1 N2 80.52(14) . . ? O9 Cd1 N2 148.08(12) . . ? N1 Cd1 N2 71.23(12) . . ? O15 Cd1 O1 86.42(17) . . ? O9 Cd1 O1 105.68(12) . . ? N1 Cd1 O1 99.04(13) . . ? N2 Cd1 O1 100.65(12) . . ? O15 Cd1 O2 121.04(15) . . ? O9 Cd1 O2 72.14(10) . . ? N1 Cd1 O2 82.81(12) . . ? N2 Cd1 O2 139.56(12) . . ? O1 Cd1 O2 52.68(10) . . ? O15 Cd1 O8 95.53(17) . . ? O9 Cd1 O8 53.17(11) . . ? N1 Cd1 O8 89.54(13) . . ? N2 Cd1 O8 101.19(12) . . ? O1 Cd1 O8 158.10(11) . . ? O2 Cd1 O8 109.25(11) . . ? O15 Cd1 H15A 21.9 . . ? O9 Cd1 H15A 79.4 . . ? N1 Cd1 H15A 158.8 . . ? N2 Cd1 H15A 94.7 . . ? O1 Cd1 H15A 67.3 . . ? O2 Cd1 H15A 99.7 . . ? O8 Cd1 H15A 109.1 . . ? O10 Cd2 O7 84.04(13) . 4_454 ? O10 Cd2 O3 84.01(12) . . ? O7 Cd2 O3 86.62(13) 4_454 . ? O10 Cd2 N4 114.01(13) . . ? O7 Cd2 N4 89.85(13) 4_454 . ? O3 Cd2 N4 161.19(13) . . ? O10 Cd2 N3 127.53(13) . . ? O7 Cd2 N3 147.78(14) 4_454 . ? O3 Cd2 N3 101.46(13) . . ? N4 Cd2 N3 72.45(13) . . ? O6 Cd3 O14 128.99(13) 1_454 . ? O6 Cd3 O2 101.29(12) 1_454 4_454 ? O14 Cd3 O2 78.41(12) . 4_454 ? O6 Cd3 O10 94.38(12) 1_454 4_454 ? O14 Cd3 O10 121.77(12) . 4_454 ? O2 Cd3 O10 135.38(11) 4_454 4_454 ? O6 Cd3 O9 152.37(12) 1_454 4_454 ? O14 Cd3 O9 77.49(12) . 4_454 ? O2 Cd3 O9 73.94(11) 4_454 4_454 ? O10 Cd3 O9 73.09(11) 4_454 4_454 ? O6 Cd3 O13 94.82(13) 1_454 . ? O14 Cd3 O13 54.26(12) . . ? O2 Cd3 O13 128.50(11) 4_454 . ? O10 Cd3 O13 90.79(12) 4_454 . ? O9 Cd3 O13 109.55(13) 4_454 . ? O6 Cd3 C30 115.35(14) 1_454 . ? O14 Cd3 C30 27.22(13) . . ? O2 Cd3 C30 104.54(12) 4_454 . ? O10 Cd3 C30 105.82(13) 4_454 . ? O9 Cd3 C30 91.98(13) 4_454 . ? O13 Cd3 C30 27.22(13) . . ? H16B O16 H16A 109.6 . . ? H17A O17 H17B 108.2 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.356 _refine_diff_density_min -0.397 _refine_diff_density_rms 0.103 #===END data_7 _database_code_depnum_ccdc_archive 'CCDC 746383' #TrackingRef 'complexes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C66 H47 Cd3 N6 O19' _chemical_formula_weight 1565.30 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 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.511(3) _cell_length_b 14.864(3) _cell_length_c 17.527(3) _cell_angle_alpha 66.948(2) _cell_angle_beta 86.831(2) _cell_angle_gamma 67.297(3) _cell_volume 2968.8(10) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 5999 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.751 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1562 _exptl_absorpt_coefficient_mu 1.150 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8027 _exptl_absorpt_correction_T_max 0.8937 _exptl_absorpt_process_details '(SADABS; Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 0 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 14304 _diffrn_reflns_av_R_equivalents 0.0215 _diffrn_reflns_av_sigmaI/netI 0.0473 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10205 _reflns_number_gt 7825 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'SAINT-Plus (Bruker, 2001)' _computing_data_reduction SAINT-Plus _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Sheldrick, 1998)' _computing_publication_material XP _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^)+(0.0668P)^2^+2.1076P] 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 10205 _refine_ls_number_parameters 847 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0626 _refine_ls_R_factor_gt 0.0439 _refine_ls_wR_factor_ref 0.1296 _refine_ls_wR_factor_gt 0.1175 _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_restrained_S_all 1.843 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1399(6) 0.3656(6) 0.3728(5) 0.0277(17) Uani 1 1 d . . . C2 C 0.0686(6) 0.4419(6) 0.3010(5) 0.0296(18) Uani 1 1 d . . . C3 C 0.1066(7) 0.4568(7) 0.2236(5) 0.037(2) Uani 1 1 d . . . H3 H 0.0606 0.5082 0.1756 0.044 Uiso 1 1 calc R . . C4 C 0.2120(7) 0.3963(7) 0.2167(6) 0.036(2) Uani 1 1 d . . . H4 H 0.2359 0.4060 0.1644 0.043 Uiso 1 1 calc R . . C5 C 0.2801(6) 0.3227(7) 0.2870(6) 0.035(2) Uani 1 1 d . . . C6 C 0.2456(7) 0.3060(7) 0.3659(6) 0.036(2) Uani 1 1 d . . . H6 H 0.2929 0.2555 0.4134 0.043 Uiso 1 1 calc R . . C7 C 0.0979(6) 0.3393(7) 0.4566(5) 0.0320(19) Uani 1 1 d . . . C8 C -0.0444(7) 0.5127(7) 0.3058(6) 0.036(2) Uani 1 1 d . . . C9 C 0.4760(6) 0.2447(7) 0.3098(5) 0.0320(19) Uani 1 1 d . . . C10 C 0.4853(6) 0.3242(7) 0.3281(5) 0.035(2) Uani 1 1 d . . . H10 H 0.4244 0.3841 0.3238 0.042 Uiso 1 1 calc R . . C11 C 0.5863(6) 0.3127(7) 0.3528(5) 0.0322(19) Uani 1 1 d . . . H11 H 0.5933 0.3660 0.3644 0.039 Uiso 1 1 calc R . . C12 C 0.6775(6) 0.2230(7) 0.3605(5) 0.0303(18) Uani 1 1 d . . . C13 C 0.6652(6) 0.1448(7) 0.3430(5) 0.0335(19) Uani 1 1 d . . . H13 H 0.7253 0.0833 0.3493 0.040 Uiso 1 1 calc R . . C14 C 0.5647(7) 0.1568(7) 0.3165(6) 0.038(2) Uani 1 1 d . . . H14 H 0.5578 0.1046 0.3031 0.046 Uiso 1 1 calc R . . C15 C -0.2119(6) 0.2120(7) 0.3839(5) 0.0328(19) Uani 1 1 d . . . C16 C 0.3112(6) -0.0372(7) 0.8303(5) 0.0305(18) Uani 1 1 d . . . C17 C 0.3549(7) -0.1414(7) 0.8921(5) 0.0335(19) Uani 1 1 d . . . H17 H 0.4193 -0.1654 0.9246 0.040 Uiso 1 1 calc R . . C18 C 0.3021(7) -0.2079(7) 0.9042(5) 0.0348(19) Uani 1 1 d . . . C19 C 0.2076(7) -0.1753(7) 0.8559(6) 0.038(2) Uani 1 1 d . . . H19 H 0.1732 -0.2214 0.8647 0.046 Uiso 1 1 calc R . . C20 C 0.1652(7) -0.0744(7) 0.7950(6) 0.036(2) Uani 1 1 d . . . H20 H 0.1021 -0.0527 0.7619 0.044 Uiso 1 1 calc R . . C21 C 0.2143(6) -0.0036(6) 0.7815(5) 0.0283(17) Uani 1 1 d . . . C22 C 0.1605(6) 0.1084(7) 0.7179(5) 0.0301(18) Uani 1 1 d . . . C23 C 0.3740(7) 0.0319(7) 0.8172(6) 0.036(2) Uani 1 1 d . . . C24 C 0.3596(7) -0.3955(6) 0.9502(5) 0.0323(18) Uani 1 1 d . . . C25 C 0.3830(7) -0.3958(7) 0.8729(6) 0.039(2) Uani 1 1 d . . . H25 H 0.3881 -0.3364 0.8304 0.047 Uiso 1 1 calc R . . C26 C 0.3990(7) -0.4856(7) 0.8591(6) 0.039(2) Uani 1 1 d . . . H26 H 0.4133 -0.4854 0.8065 0.047 Uiso 1 1 calc R . . C27 C 0.3942(6) -0.5763(7) 0.9222(6) 0.035(2) Uani 1 1 d . . . C28 C 0.3714(7) -0.5750(7) 0.9994(6) 0.042(2) Uani 1 1 d . . . H28 H 0.3672 -0.6347 1.0420 0.050 Uiso 1 1 calc R . . C29 C 0.3547(7) -0.4850(7) 1.0145(6) 0.040(2) Uani 1 1 d . . . H29 H 0.3404 -0.4849 1.0670 0.048 Uiso 1 1 calc R . . C30 C 0.4118(7) -0.6707(8) 0.9028(7) 0.045(2) Uani 1 1 d . . . C31 C -0.0887(8) 0.3452(9) 0.2086(7) 0.053(3) Uani 1 1 d . . . H31 H -0.1540 0.3797 0.2252 0.063 Uiso 1 1 calc R . . C32 C -0.0779(9) 0.3755(10) 0.1230(7) 0.059(3) Uani 1 1 d . . . H32 H -0.1361 0.4274 0.0836 0.071 Uiso 1 1 calc R . . C33 C 0.0174(10) 0.3288(10) 0.0987(7) 0.061(3) Uani 1 1 d . . . H33 H 0.0258 0.3501 0.0421 0.073 Uiso 1 1 calc R . . C34 C 0.1049(8) 0.2480(8) 0.1580(6) 0.045(2) Uani 1 1 d . . . C35 C 0.2112(9) 0.1945(10) 0.1370(7) 0.059(3) Uani 1 1 d . . . H35 H 0.2229 0.2113 0.0812 0.071 Uiso 1 1 calc R . . C36 C 0.2924(9) 0.1215(9) 0.1966(7) 0.056(3) Uani 1 1 d . . . H36 H 0.3596 0.0886 0.1816 0.068 Uiso 1 1 calc R . . C37 C 0.2776(7) 0.0933(8) 0.2829(6) 0.042(2) Uani 1 1 d . . . C38 C 0.3628(8) 0.0230(8) 0.3457(7) 0.053(3) Uani 1 1 d . . . H38 H 0.4313 -0.0087 0.3319 0.063 Uiso 1 1 calc R . . C39 C 0.3461(8) 0.0009(9) 0.4268(8) 0.058(3) Uani 1 1 d . . . H39 H 0.4024 -0.0460 0.4692 0.070 Uiso 1 1 calc R . . C40 C 0.2414(7) 0.0505(9) 0.4451(7) 0.053(3) Uani 1 1 d . . . H40 H 0.2300 0.0355 0.5008 0.064 Uiso 1 1 calc R . . C41 C 0.1753(7) 0.1420(7) 0.3059(6) 0.0346(19) Uani 1 1 d . . . C42 C 0.0868(7) 0.2211(7) 0.2419(6) 0.036(2) Uani 1 1 d . . . C43 C 0.0236(9) 0.2543(8) 0.8314(6) 0.052(3) Uani 1 1 d . . . H43 H 0.0983 0.2323 0.8354 0.062 Uiso 1 1 calc R . . C44 C -0.0267(10) 0.2417(9) 0.9041(7) 0.061(3) Uani 1 1 d . . . H44 H 0.0135 0.2138 0.9555 0.074 Uiso 1 1 calc R . . C45 C -0.1354(10) 0.2708(9) 0.8988(7) 0.065(3) Uani 1 1 d . . . H45 H -0.1696 0.2604 0.9472 0.078 Uiso 1 1 calc R . . C46 C -0.1959(8) 0.3157(8) 0.8222(7) 0.053(3) Uani 1 1 d . . . C47 C -0.3100(9) 0.3490(9) 0.8110(9) 0.063(3) Uani 1 1 d . . . H47 H -0.3472 0.3388 0.8578 0.075 Uiso 1 1 calc R . . C48 C -0.3646(9) 0.3936(9) 0.7368(9) 0.062(3) Uani 1 1 d . . . H48 H -0.4390 0.4139 0.7323 0.075 Uiso 1 1 calc R . . C49 C -0.3105(8) 0.4118(8) 0.6615(7) 0.050(3) Uani 1 1 d . . . C50 C -0.3653(9) 0.4616(9) 0.5822(9) 0.064(3) Uani 1 1 d . . . H50 H -0.4399 0.4835 0.5756 0.077 Uiso 1 1 calc R . . C51 C -0.3109(9) 0.4789(9) 0.5138(8) 0.061(3) Uani 1 1 d . . . H51 H -0.3480 0.5143 0.4605 0.074 Uiso 1 1 calc R . . C52 C -0.1973(8) 0.4422(8) 0.5249(7) 0.052(3) Uani 1 1 d . . . C53 C -0.1985(7) 0.3787(7) 0.6689(6) 0.041(2) Uani 1 1 d . . . C54 C -0.1397(7) 0.3282(7) 0.7502(6) 0.040(2) Uani 1 1 d . . . C55 C 0.4959(12) 0.2535(10) 0.6292(8) 0.075(4) Uani 1 1 d . . . H55 H 0.4212 0.2809 0.6183 0.090 Uiso 1 1 calc R . . C56 C 0.5559(19) 0.2644(12) 0.5631(9) 0.103(6) Uani 1 1 d . . . H56 H 0.5223 0.2965 0.5088 0.123 Uiso 1 1 calc R . . C57 C 0.6645(19) 0.2282(12) 0.5775(10) 0.103(7) Uani 1 1 d . . . H57 H 0.7054 0.2378 0.5329 0.124 Uiso 1 1 calc R . . C58 C 0.7161(12) 0.1754(10) 0.6608(9) 0.071(4) Uani 1 1 d . . . C59 C 0.8263(14) 0.1352(13) 0.6823(13) 0.099(6) Uani 1 1 d . . . H59 H 0.8712 0.1413 0.6401 0.119 Uiso 1 1 calc R . . C60 C 0.8704(11) 0.0881(13) 0.7612(14) 0.096(6) Uani 1 1 d . . . H60 H 0.9443 0.0660 0.7728 0.115 Uiso 1 1 calc R . . C61 C 0.8066(9) 0.0715(10) 0.8269(10) 0.070(4) Uani 1 1 d . . . C62 C 0.8478(10) 0.0181(12) 0.9134(13) 0.096(5) Uani 1 1 d . . . H62 H 0.9213 -0.0068 0.9291 0.115 Uiso 1 1 calc R . . C63 C 0.7813(13) 0.0043(13) 0.9712(11) 0.104(5) Uani 1 1 d . . . H63 H 0.8086 -0.0323 1.0273 0.125 Uiso 1 1 calc R . . C64 C 0.6705(11) 0.0441(10) 0.9485(8) 0.074(4) Uani 1 1 d . . . H64 H 0.6249 0.0335 0.9898 0.089 Uiso 1 1 calc R . . C65 C 0.6947(7) 0.1096(7) 0.8096(6) 0.042(2) Uani 1 1 d . . . C66 C 0.6484(9) 0.1645(8) 0.7249(7) 0.047(3) Uani 1 1 d . . . N1 N -0.0087(6) 0.2689(6) 0.2664(5) 0.0375(17) Uani 1 1 d . . . N2 N 0.1574(6) 0.1182(6) 0.3868(5) 0.0377(17) Uani 1 1 d . . . N3 N -0.1434(6) 0.3921(6) 0.6011(5) 0.0406(18) Uani 1 1 d . . . N4 N -0.0303(6) 0.2962(6) 0.7567(5) 0.0400(18) Uani 1 1 d . . . N5 N 0.5400(7) 0.2054(6) 0.7086(5) 0.046(2) Uani 1 1 d . . . N6 N 0.6295(6) 0.0960(6) 0.8704(5) 0.0425(18) Uani 1 1 d . . . O1 O 0.1405(5) 0.3487(6) 0.5130(4) 0.0459(16) Uani 1 1 d . . . O2 O 0.0232(4) 0.3055(5) 0.4688(4) 0.0349(13) Uani 1 1 d . . . O3 O -0.0599(5) 0.5383(5) 0.3675(4) 0.0397(14) Uani 1 1 d . . . O4 O -0.1159(5) 0.5421(6) 0.2491(4) 0.0555(19) Uani 1 1 d . . . O5 O 0.3803(4) 0.2538(6) 0.2771(4) 0.0477(18) Uani 1 1 d . . . O6 O -0.2022(4) 0.2876(5) 0.3946(4) 0.0442(16) Uani 1 1 d . . . O7 O -0.1310(5) 0.1299(5) 0.3916(4) 0.0427(15) Uani 1 1 d . . . O8 O 0.1924(5) 0.1779(5) 0.7149(4) 0.0390(14) Uani 1 1 d . . . O9 O 0.0805(5) 0.1329(5) 0.6688(4) 0.0425(15) Uani 1 1 d . . . O10 O 0.4257(5) 0.0458(6) 0.7566(4) 0.0535(18) Uani 1 1 d . . . O11 O 0.3702(6) 0.0682(6) 0.8710(4) 0.0571(19) Uani 1 1 d . . . O12 O 0.3459(5) -0.3095(5) 0.9689(4) 0.0407(15) Uani 1 1 d . . . O13 O 0.3987(7) -0.7507(6) 0.9553(6) 0.071(2) Uani 1 1 d . . . O14 O 0.4380(6) 0.3346(6) 0.8318(5) 0.063(2) Uani 1 1 d . . . O15 O 0.0208(5) 0.0858(5) 0.5477(4) 0.0455(16) Uani 1 1 d D . . H15A H 0.0475 0.1083 0.5754 0.068 Uiso 1 1 d RD . . H15B H 0.0575 0.0203 0.5603 0.068 Uiso 1 1 d RD . . O16 O 0.2908(6) 0.2995(6) 0.7310(6) 0.081(3) Uani 1 1 d D . . H16A H 0.2286 0.3402 0.7035 0.121 Uiso 1 1 d RD . . H16B H 0.2825 0.2720 0.7827 0.121 Uiso 1 1 d RD . . O17 O 0.8408(7) 0.6610(10) 0.0745(6) 0.113(4) Uani 1 1 d D . . H17A H 0.8564 0.6066 0.1207 0.170 Uiso 1 1 d RD . . H17B H 0.8739 0.6415 0.0371 0.170 Uiso 1 1 d RD . . O18 O 0.3458(8) 0.1364(10) 0.5775(6) 0.118(4) Uani 1 1 d D . . H18C H 0.3177 0.2336 0.5885 0.177 Uiso 1 1 d RD . . H18D H 0.3778 0.0808 0.6212 0.177 Uiso 1 1 d RD . . O19 O 0.6442(10) 0.5115(10) 0.3318(8) 0.125(4) Uani 1 1 d . . . H19A H 0.6958 0.4504 0.3482 0.188 Uiso 1 1 d R . . H19B H 0.6701 0.5575 0.3056 0.188 Uiso 1 1 d R . . Cd1 Cd 0.04181(5) 0.32279(5) 0.62212(4) 0.0333(2) Uani 1 1 d . . . Cd2 Cd -0.01472(5) 0.20952(5) 0.41115(4) 0.0351(2) Uani 1 1 d . . . Cd3 Cd 0.44447(5) 0.18595(6) 0.82518(5) 0.0425(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.026(4) 0.031(4) 0.032(4) -0.015(4) 0.006(3) -0.015(3) C2 0.027(4) 0.030(4) 0.034(5) -0.016(4) 0.002(3) -0.010(3) C3 0.038(5) 0.036(5) 0.032(5) -0.011(4) 0.006(4) -0.015(4) C4 0.041(5) 0.037(5) 0.032(5) -0.013(4) 0.012(4) -0.020(4) C5 0.023(4) 0.043(5) 0.052(6) -0.030(5) 0.010(4) -0.016(4) C6 0.028(4) 0.042(5) 0.039(5) -0.019(4) -0.001(4) -0.012(4) C7 0.030(4) 0.030(5) 0.035(5) -0.016(4) 0.003(4) -0.007(4) C8 0.035(5) 0.029(5) 0.038(5) -0.010(4) 0.008(4) -0.012(4) C9 0.021(4) 0.046(5) 0.037(5) -0.023(4) 0.012(3) -0.016(4) C10 0.026(4) 0.037(5) 0.044(5) -0.022(4) 0.007(4) -0.008(4) C11 0.034(4) 0.033(5) 0.034(5) -0.016(4) 0.007(4) -0.015(4) C12 0.024(4) 0.042(5) 0.029(4) -0.017(4) 0.007(3) -0.015(4) C13 0.025(4) 0.034(5) 0.038(5) -0.014(4) 0.005(3) -0.008(4) C14 0.035(5) 0.041(5) 0.044(5) -0.023(5) 0.007(4) -0.015(4) C15 0.029(4) 0.043(5) 0.030(5) -0.014(4) 0.008(3) -0.018(4) C16 0.027(4) 0.034(5) 0.029(4) -0.014(4) 0.003(3) -0.010(4) C17 0.033(4) 0.034(5) 0.033(5) -0.014(4) -0.001(4) -0.010(4) C18 0.040(5) 0.030(5) 0.029(5) -0.012(4) 0.007(4) -0.010(4) C19 0.037(5) 0.033(5) 0.042(5) -0.011(4) 0.005(4) -0.017(4) C20 0.026(4) 0.037(5) 0.048(6) -0.021(5) 0.002(4) -0.010(4) C21 0.024(4) 0.029(4) 0.030(4) -0.012(4) 0.007(3) -0.010(3) C22 0.025(4) 0.035(5) 0.034(5) -0.018(4) 0.005(3) -0.010(4) C23 0.031(4) 0.032(5) 0.042(5) -0.012(4) -0.005(4) -0.011(4) C24 0.038(5) 0.024(4) 0.031(5) -0.007(4) 0.002(4) -0.012(4) C25 0.042(5) 0.030(5) 0.039(5) -0.009(4) 0.010(4) -0.014(4) C26 0.045(5) 0.035(5) 0.040(5) -0.018(4) 0.010(4) -0.015(4) C27 0.027(4) 0.034(5) 0.048(6) -0.022(4) 0.003(4) -0.010(4) C28 0.044(5) 0.026(5) 0.045(6) -0.006(4) 0.002(4) -0.012(4) C29 0.046(5) 0.041(5) 0.030(5) -0.010(4) 0.005(4) -0.017(4) C30 0.028(5) 0.035(5) 0.071(7) -0.023(5) -0.008(4) -0.008(4) C31 0.045(6) 0.053(6) 0.054(7) -0.015(5) -0.005(5) -0.018(5) C32 0.057(7) 0.064(7) 0.051(7) -0.016(6) -0.007(5) -0.025(6) C33 0.077(8) 0.072(8) 0.043(6) -0.021(6) 0.008(6) -0.040(7) C34 0.054(6) 0.052(6) 0.042(6) -0.024(5) 0.011(5) -0.029(5) C35 0.070(8) 0.075(8) 0.049(7) -0.037(6) 0.027(6) -0.034(7) C36 0.051(6) 0.067(8) 0.067(8) -0.042(7) 0.027(6) -0.027(6) C37 0.040(5) 0.040(5) 0.054(6) -0.025(5) 0.019(4) -0.019(4) C38 0.038(5) 0.045(6) 0.078(8) -0.032(6) 0.020(5) -0.013(5) C39 0.029(5) 0.049(6) 0.073(8) -0.014(6) 0.000(5) -0.002(5) C40 0.034(5) 0.059(7) 0.049(6) -0.009(5) 0.004(4) -0.014(5) C41 0.033(5) 0.033(5) 0.043(5) -0.016(4) 0.010(4) -0.018(4) C42 0.038(5) 0.036(5) 0.043(5) -0.021(4) 0.008(4) -0.020(4) C43 0.058(6) 0.045(6) 0.045(6) -0.017(5) 0.011(5) -0.015(5) C44 0.072(8) 0.060(7) 0.041(6) -0.016(6) 0.010(5) -0.020(6) C45 0.081(9) 0.057(7) 0.055(7) -0.020(6) 0.036(6) -0.031(6) C46 0.054(6) 0.044(6) 0.068(8) -0.028(6) 0.029(6) -0.024(5) C47 0.052(7) 0.057(7) 0.085(9) -0.035(7) 0.041(7) -0.025(6) C48 0.035(6) 0.052(7) 0.109(11) -0.040(7) 0.036(6) -0.023(5) C49 0.035(5) 0.035(5) 0.080(8) -0.027(6) 0.007(5) -0.011(4) C50 0.036(6) 0.050(7) 0.111(11) -0.041(7) 0.004(6) -0.010(5) C51 0.043(6) 0.054(7) 0.072(8) -0.023(6) -0.009(6) -0.004(5) C52 0.041(6) 0.045(6) 0.060(7) -0.015(5) -0.004(5) -0.011(5) C53 0.037(5) 0.027(5) 0.060(6) -0.022(5) 0.014(4) -0.011(4) C54 0.043(5) 0.032(5) 0.047(6) -0.020(4) 0.017(4) -0.012(4) C55 0.108(11) 0.055(8) 0.053(8) -0.017(6) -0.004(7) -0.026(7) C56 0.20(2) 0.065(10) 0.044(8) -0.024(7) 0.033(11) -0.053(12) C57 0.199(19) 0.069(10) 0.069(11) -0.046(9) 0.084(13) -0.072(12) C58 0.103(11) 0.052(7) 0.084(10) -0.042(7) 0.057(8) -0.048(7) C59 0.092(12) 0.089(12) 0.150(16) -0.075(12) 0.089(12) -0.052(10) C60 0.043(7) 0.088(12) 0.186(18) -0.081(13) 0.050(10) -0.033(8) C61 0.036(6) 0.057(7) 0.125(12) -0.052(8) 0.014(7) -0.012(5) C62 0.036(7) 0.082(11) 0.160(17) -0.061(11) -0.020(9) 0.001(7) C63 0.077(11) 0.099(12) 0.089(12) -0.026(10) -0.036(9) 0.006(9) C64 0.073(8) 0.069(8) 0.051(7) -0.012(7) -0.003(6) -0.010(7) C65 0.033(5) 0.039(5) 0.065(7) -0.030(5) 0.021(4) -0.017(4) C66 0.062(7) 0.041(6) 0.055(7) -0.032(5) 0.030(5) -0.027(5) N1 0.035(4) 0.037(4) 0.042(4) -0.016(4) 0.003(3) -0.016(3) N2 0.031(4) 0.038(4) 0.040(4) -0.012(4) 0.010(3) -0.014(3) N3 0.031(4) 0.032(4) 0.049(5) -0.012(4) 0.002(3) -0.006(3) N4 0.042(4) 0.035(4) 0.037(5) -0.013(4) 0.010(3) -0.012(3) N5 0.063(6) 0.041(5) 0.038(5) -0.018(4) 0.007(4) -0.021(4) N6 0.040(4) 0.039(4) 0.040(5) -0.014(4) 0.006(3) -0.009(3) O1 0.053(4) 0.063(5) 0.038(4) -0.028(3) 0.011(3) -0.031(3) O2 0.036(3) 0.033(3) 0.035(3) -0.013(3) 0.009(3) -0.015(3) O3 0.044(4) 0.037(4) 0.036(3) -0.015(3) 0.013(3) -0.014(3) O4 0.034(4) 0.062(5) 0.053(4) -0.023(4) -0.008(3) 0.001(3) O5 0.022(3) 0.072(5) 0.073(5) -0.054(4) 0.013(3) -0.017(3) O6 0.027(3) 0.051(4) 0.064(4) -0.034(4) 0.005(3) -0.014(3) O7 0.025(3) 0.042(4) 0.059(4) -0.021(3) 0.001(3) -0.010(3) O8 0.034(3) 0.031(3) 0.047(4) -0.009(3) -0.006(3) -0.012(3) O9 0.040(4) 0.037(4) 0.045(4) -0.014(3) -0.010(3) -0.011(3) O10 0.039(4) 0.061(5) 0.062(5) -0.023(4) 0.019(3) -0.026(3) O11 0.084(5) 0.071(5) 0.043(4) -0.026(4) 0.009(4) -0.055(4) O12 0.057(4) 0.028(3) 0.033(3) -0.010(3) 0.001(3) -0.015(3) O13 0.086(6) 0.044(5) 0.095(6) -0.033(5) 0.012(5) -0.031(4) O14 0.074(5) 0.053(5) 0.077(6) -0.042(4) 0.013(4) -0.025(4) O15 0.053(4) 0.043(4) 0.043(4) -0.020(3) 0.005(3) -0.020(3) O16 0.041(4) 0.054(5) 0.138(8) -0.040(5) -0.023(4) -0.003(4) O17 0.072(6) 0.188(12) 0.057(6) -0.016(7) 0.015(5) -0.065(7) O18 0.091(7) 0.157(11) 0.073(7) -0.055(7) 0.006(5) -0.006(7) O19 0.122(9) 0.105(9) 0.144(11) -0.041(8) 0.001(8) -0.047(7) Cd1 0.0286(3) 0.0320(4) 0.0327(4) -0.0098(3) 0.0042(3) -0.0086(3) Cd2 0.0253(3) 0.0436(4) 0.0405(4) -0.0205(3) 0.0066(3) -0.0145(3) Cd3 0.0314(4) 0.0405(4) 0.0656(5) -0.0300(4) 0.0142(3) -0.0167(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C6 1.389(11) . ? C1 C2 1.404(11) . ? C1 C7 1.503(11) . ? C2 C3 1.388(11) . ? C2 C8 1.503(11) . ? C3 C4 1.390(12) . ? C3 H3 0.9300 . ? C4 C5 1.362(13) . ? C4 H4 0.9300 . ? C5 C6 1.393(12) . ? C5 O5 1.399(9) . ? C6 H6 0.9300 . ? C7 O1 1.250(10) . ? C7 O2 1.265(10) . ? C8 O4 1.246(11) . ? C8 O3 1.263(10) . ? C9 C14 1.359(12) . ? C9 O5 1.380(10) . ? C9 C10 1.389(12) . ? C10 C11 1.381(11) . ? C10 H10 0.9300 . ? C11 C12 1.387(11) . ? C11 H11 0.9300 . ? C12 C13 1.381(12) . ? C12 C15 1.502(11) 1_655 ? C13 C14 1.382(11) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 O7 1.249(10) . ? C15 O6 1.262(10) . ? C15 C12 1.502(11) 1_455 ? C15 Cd2 2.716(8) . ? C16 C17 1.404(12) . ? C16 C21 1.407(11) . ? C16 C23 1.516(11) . ? C17 C18 1.376(12) . ? C17 H17 0.9300 . ? C18 C19 1.379(12) . ? C18 O12 1.400(10) . ? C19 C20 1.367(12) . ? C19 H19 0.9300 . ? C20 C21 1.389(11) . ? C20 H20 0.9300 . ? C21 C22 1.498(12) . ? C22 O8 1.246(10) . ? C22 O9 1.263(10) . ? C23 O10 1.230(11) . ? C23 O11 1.247(10) . ? C24 C25 1.376(12) . ? C24 O12 1.384(10) . ? C24 C29 1.389(12) . ? C25 C26 1.382(12) . ? C25 H25 0.9300 . ? C26 C27 1.392(12) . ? C26 H26 0.9300 . ? C27 C28 1.378(12) . ? C27 C30 1.498(12) . ? C28 C29 1.395(12) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C30 O14 1.257(12) 1_545 ? C30 O13 1.258(12) . ? C31 N1 1.326(12) . ? C31 C32 1.403(15) . ? C31 H31 0.9300 . ? C32 C33 1.343(15) . ? C32 H32 0.9300 . ? C33 C34 1.408(15) . ? C33 H33 0.9300 . ? C34 C42 1.398(12) . ? C34 C35 1.456(14) . ? C35 C36 1.339(16) . ? C35 H35 0.9300 . ? C36 C37 1.426(14) . ? C36 H36 0.9300 . ? C37 C38 1.393(15) . ? C37 C41 1.412(11) . ? C38 C39 1.355(15) . ? C38 H38 0.9300 . ? C39 C40 1.407(13) . ? C39 H39 0.9300 . ? C40 N2 1.337(12) . ? C40 H40 0.9300 . ? C41 N2 1.352(11) . ? C41 C42 1.450(13) . ? C42 N1 1.350(10) . ? C43 N4 1.323(12) . ? C43 C44 1.392(14) . ? C43 H43 0.9300 . ? C44 C45 1.360(16) . ? C44 H44 0.9300 . ? C45 C46 1.383(16) . ? C45 H45 0.9300 . ? C46 C54 1.422(13) . ? C46 C47 1.425(15) . ? C47 C48 1.314(17) . ? C47 H47 0.9300 . ? C48 C49 1.453(16) . ? C48 H48 0.9300 . ? C49 C50 1.383(16) . ? C49 C53 1.395(13) . ? C50 C51 1.361(16) . ? C50 H50 0.9300 . ? C51 C52 1.412(14) . ? C51 H51 0.9300 . ? C52 N3 1.334(13) . ? C53 N3 1.356(12) . ? C53 C54 1.433(14) . ? C54 N4 1.362(11) . ? C55 N5 1.337(14) . ? C55 C56 1.37(2) . ? C55 H55 0.9300 . ? C56 C57 1.35(2) . ? C56 H56 0.9300 . ? C57 C58 1.42(2) . ? C57 H57 0.9300 . ? C58 C59 1.38(2) . ? C58 C66 1.409(14) . ? C59 C60 1.33(2) . ? C59 H59 0.9300 . ? C60 C61 1.40(2) . ? C60 H60 0.9300 . ? C61 C65 1.398(14) . ? C61 C62 1.43(2) . ? C62 C63 1.32(2) . ? C62 H62 0.9300 . ? C63 C64 1.396(19) . ? C63 H63 0.9300 . ? C64 N6 1.305(13) . ? C64 H64 0.9300 . ? C65 N6 1.347(11) . ? C65 C66 1.422(14) . ? C66 N5 1.349(13) . ? N1 Cd2 2.345(7) . ? N2 Cd2 2.310(7) . ? N3 Cd1 2.296(7) . ? N4 Cd1 2.446(7) . ? N5 Cd3 2.336(8) . ? N6 Cd3 2.340(8) . ? O1 Cd1 2.263(6) . ? O2 Cd2 2.251(6) . ? O3 Cd1 2.245(6) 2_566 ? O6 Cd2 2.323(6) . ? O7 Cd2 2.407(6) . ? O8 Cd1 2.380(6) . ? O9 Cd1 2.451(6) . ? O11 Cd3 2.210(7) . ? O14 C30 1.257(12) 1_565 ? O14 Cd3 2.226(7) . ? O15 Cd2 2.310(6) . ? O15 H15A 0.8459 . ? O15 H15B 0.8454 . ? O16 Cd3 2.319(8) . ? Cd1 O3 2.245(6) 2_566 ? 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 C6 C1 C2 120.3(7) . . ? C6 C1 C7 119.7(7) . . ? C2 C1 C7 119.6(7) . . ? C3 C2 C1 118.6(7) . . ? C3 C2 C8 119.3(8) . . ? C1 C2 C8 122.0(7) . . ? C2 C3 C4 121.1(8) . . ? C2 C3 H3 119.4 . . ? C4 C3 H3 119.4 . . ? C5 C4 C3 119.5(8) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? C4 C5 C6 121.2(8) . . ? C4 C5 O5 117.5(8) . . ? C6 C5 O5 120.6(8) . . ? C1 C6 C5 119.3(8) . . ? C1 C6 H6 120.4 . . ? C5 C6 H6 120.4 . . ? O1 C7 O2 122.0(8) . . ? O1 C7 C1 118.5(7) . . ? O2 C7 C1 119.4(7) . . ? O4 C8 O3 124.5(8) . . ? O4 C8 C2 118.3(8) . . ? O3 C8 C2 117.2(8) . . ? C14 C9 O5 116.1(7) . . ? C14 C9 C10 120.6(8) . . ? O5 C9 C10 123.0(7) . . ? C11 C10 C9 119.0(8) . . ? C11 C10 H10 120.5 . . ? C9 C10 H10 120.5 . . ? C10 C11 C12 121.1(8) . . ? C10 C11 H11 119.4 . . ? C12 C11 H11 119.4 . . ? C13 C12 C11 118.4(7) . . ? C13 C12 C15 120.1(7) . 1_655 ? C11 C12 C15 121.4(8) . 1_655 ? C12 C13 C14 120.8(8) . . ? C12 C13 H13 119.6 . . ? C14 C13 H13 119.6 . . ? C9 C14 C13 120.1(8) . . ? C9 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? O7 C15 O6 120.9(7) . . ? O7 C15 C12 120.3(8) . 1_455 ? O6 C15 C12 118.8(7) . 1_455 ? O7 C15 Cd2 62.4(4) . . ? O6 C15 Cd2 58.6(4) . . ? C12 C15 Cd2 174.1(6) 1_455 . ? C17 C16 C21 118.9(7) . . ? C17 C16 C23 117.8(7) . . ? C21 C16 C23 123.3(7) . . ? C18 C17 C16 119.7(8) . . ? C18 C17 H17 120.2 . . ? C16 C17 H17 120.2 . . ? C17 C18 C19 121.5(8) . . ? C17 C18 O12 117.9(8) . . ? C19 C18 O12 120.6(8) . . ? C20 C19 C18 119.1(8) . . ? C20 C19 H19 120.4 . . ? C18 C19 H19 120.4 . . ? C19 C20 C21 121.5(8) . . ? C19 C20 H20 119.2 . . ? C21 C20 H20 119.2 . . ? C20 C21 C16 119.3(8) . . ? C20 C21 C22 119.4(7) . . ? C16 C21 C22 121.3(7) . . ? O8 C22 O9 120.0(8) . . ? O8 C22 C21 120.3(7) . . ? O9 C22 C21 119.6(7) . . ? O10 C23 O11 125.6(8) . . ? O10 C23 C16 118.5(8) . . ? O11 C23 C16 115.9(8) . . ? C25 C24 O12 122.2(8) . . ? C25 C24 C29 120.6(8) . . ? O12 C24 C29 117.1(7) . . ? C24 C25 C26 119.2(8) . . ? C24 C25 H25 120.4 . . ? C26 C25 H25 120.4 . . ? C25 C26 C27 121.4(8) . . ? C25 C26 H26 119.3 . . ? C27 C26 H26 119.3 . . ? C28 C27 C26 118.6(8) . . ? C28 C27 C30 122.7(9) . . ? C26 C27 C30 118.7(8) . . ? C27 C28 C29 120.8(8) . . ? C27 C28 H28 119.6 . . ? C29 C28 H28 119.6 . . ? C24 C29 C28 119.3(8) . . ? C24 C29 H29 120.4 . . ? C28 C29 H29 120.4 . . ? O14 C30 O13 121.7(9) 1_545 . ? O14 C30 C27 117.3(9) 1_545 . ? O13 C30 C27 121.0(10) . . ? N1 C31 C32 122.0(10) . . ? N1 C31 H31 119.0 . . ? C32 C31 H31 119.0 . . ? C33 C32 C31 119.3(10) . . ? C33 C32 H32 120.4 . . ? C31 C32 H32 120.4 . . ? C32 C33 C34 120.6(10) . . ? C32 C33 H33 119.7 . . ? C34 C33 H33 119.7 . . ? C42 C34 C33 116.5(9) . . ? C42 C34 C35 119.4(9) . . ? C33 C34 C35 124.1(9) . . ? C36 C35 C34 121.1(9) . . ? C36 C35 H35 119.4 . . ? C34 C35 H35 119.4 . . ? C35 C36 C37 121.1(9) . . ? C35 C36 H36 119.4 . . ? C37 C36 H36 119.4 . . ? C38 C37 C41 118.4(9) . . ? C38 C37 C36 121.9(9) . . ? C41 C37 C36 119.6(9) . . ? C39 C38 C37 120.1(9) . . ? C39 C38 H38 119.9 . . ? C37 C38 H38 119.9 . . ? C38 C39 C40 118.3(10) . . ? C38 C39 H39 120.9 . . ? C40 C39 H39 120.9 . . ? N2 C40 C39 123.5(10) . . ? N2 C40 H40 118.2 . . ? C39 C40 H40 118.2 . . ? N2 C41 C37 121.7(8) . . ? N2 C41 C42 118.5(7) . . ? C37 C41 C42 119.8(8) . . ? N1 C42 C34 122.9(8) . . ? N1 C42 C41 118.0(8) . . ? C34 C42 C41 119.0(8) . . ? N4 C43 C44 122.8(10) . . ? N4 C43 H43 118.6 . . ? C44 C43 H43 118.6 . . ? C45 C44 C43 118.9(11) . . ? C45 C44 H44 120.5 . . ? C43 C44 H44 120.5 . . ? C44 C45 C46 120.7(10) . . ? C44 C45 H45 119.7 . . ? C46 C45 H45 119.7 . . ? C45 C46 C54 117.5(10) . . ? C45 C46 C47 124.4(10) . . ? C54 C46 C47 118.1(11) . . ? C48 C47 C46 122.4(10) . . ? C48 C47 H47 118.8 . . ? C46 C47 H47 118.8 . . ? C47 C48 C49 121.1(10) . . ? C47 C48 H48 119.5 . . ? C49 C48 H48 119.5 . . ? C50 C49 C53 118.1(10) . . ? C50 C49 C48 122.9(10) . . ? C53 C49 C48 119.0(10) . . ? C51 C50 C49 120.4(10) . . ? C51 C50 H50 119.8 . . ? C49 C50 H50 119.8 . . ? C50 C51 C52 119.1(11) . . ? C50 C51 H51 120.4 . . ? C52 C51 H51 120.4 . . ? N3 C52 C51 121.0(10) . . ? N3 C53 C49 121.7(9) . . ? N3 C53 C54 118.9(8) . . ? C49 C53 C54 119.3(9) . . ? N4 C54 C46 121.2(9) . . ? N4 C54 C53 118.8(8) . . ? C46 C54 C53 120.0(9) . . ? N5 C55 C56 122.9(15) . . ? N5 C55 H55 118.5 . . ? C56 C55 H55 118.5 . . ? C57 C56 C55 119.5(16) . . ? C57 C56 H56 120.3 . . ? C55 C56 H56 120.3 . . ? C56 C57 C58 120.2(13) . . ? C56 C57 H57 119.9 . . ? C58 C57 H57 119.9 . . ? C59 C58 C66 118.7(14) . . ? C59 C58 C57 124.8(14) . . ? C66 C58 C57 116.5(14) . . ? C60 C59 C58 122.4(13) . . ? C60 C59 H59 118.8 . . ? C58 C59 H59 118.8 . . ? C59 C60 C61 120.7(14) . . ? C59 C60 H60 119.6 . . ? C61 C60 H60 119.6 . . ? C65 C61 C60 119.8(14) . . ? C65 C61 C62 115.9(12) . . ? C60 C61 C62 124.4(13) . . ? C63 C62 C61 120.0(12) . . ? C63 C62 H62 120.0 . . ? C61 C62 H62 120.0 . . ? C62 C63 C64 120.5(14) . . ? C62 C63 H63 119.8 . . ? C64 C63 H63 119.8 . . ? N6 C64 C63 121.3(13) . . ? N6 C64 H64 119.3 . . ? C63 C64 H64 119.3 . . ? N6 C65 C61 122.3(11) . . ? N6 C65 C66 119.1(8) . . ? C61 C65 C66 118.6(10) . . ? N5 C66 C58 122.0(11) . . ? N5 C66 C65 118.4(8) . . ? C58 C66 C65 119.6(11) . . ? C31 N1 C42 118.6(8) . . ? C31 N1 Cd2 125.9(7) . . ? C42 N1 Cd2 115.4(6) . . ? C40 N2 C41 117.9(8) . . ? C40 N2 Cd2 125.6(6) . . ? C41 N2 Cd2 116.3(6) . . ? C52 N3 C53 119.6(8) . . ? C52 N3 Cd1 122.1(6) . . ? C53 N3 Cd1 118.3(6) . . ? C43 N4 C54 118.9(8) . . ? C43 N4 Cd1 128.0(6) . . ? C54 N4 Cd1 113.0(6) . . ? C55 N5 C66 118.9(10) . . ? C55 N5 Cd3 125.4(8) . . ? C66 N5 Cd3 115.7(6) . . ? C64 N6 C65 120.1(9) . . ? C64 N6 Cd3 124.4(7) . . ? C65 N6 Cd3 115.2(6) . . ? C7 O1 Cd1 107.6(5) . . ? C7 O2 Cd2 129.3(5) . . ? C8 O3 Cd1 127.2(6) . 2_566 ? C9 O5 C5 121.9(6) . . ? C15 O6 Cd2 93.7(5) . . ? C15 O7 Cd2 90.2(5) . . ? C22 O8 Cd1 94.7(5) . . ? C22 O9 Cd1 91.0(5) . . ? C23 O11 Cd3 107.8(6) . . ? C24 O12 C18 117.5(6) . . ? C30 O14 Cd3 105.9(6) 1_565 . ? Cd2 O15 H15A 106.4 . . ? Cd2 O15 H15B 121.6 . . ? H15A O15 H15B 110.4 . . ? Cd3 O16 H16A 170.5 . . ? Cd3 O16 H16B 62.1 . . ? H16A O16 H16B 108.4 . . ? H17A O17 H17B 109.0 . . ? H19A O19 H19B 107.7 . . ? O3 Cd1 O1 86.1(2) 2_566 . ? O3 Cd1 N3 97.8(2) 2_566 . ? O1 Cd1 N3 120.9(3) . . ? O3 Cd1 O8 101.2(2) 2_566 . ? O1 Cd1 O8 92.9(2) . . ? N3 Cd1 O8 142.2(2) . . ? O3 Cd1 N4 85.2(2) 2_566 . ? O1 Cd1 N4 166.5(2) . . ? N3 Cd1 N4 70.7(3) . . ? O8 Cd1 N4 78.7(2) . . ? O3 Cd1 O9 153.4(2) 2_566 . ? O1 Cd1 O9 101.3(2) . . ? N3 Cd1 O9 99.9(2) . . ? O8 Cd1 O9 53.4(2) . . ? N4 Cd1 O9 82.2(2) . . ? O2 Cd2 O15 82.9(2) . . ? O2 Cd2 N2 99.1(2) . . ? O15 Cd2 N2 89.8(2) . . ? O2 Cd2 O6 100.5(2) . . ? O15 Cd2 O6 101.6(2) . . ? N2 Cd2 O6 158.4(2) . . ? O2 Cd2 N1 114.4(2) . . ? O15 Cd2 N1 156.0(2) . . ? N2 Cd2 N1 71.8(3) . . ? O6 Cd2 N1 91.8(2) . . ? O2 Cd2 O7 150.0(2) . . ? O15 Cd2 O7 85.7(2) . . ? N2 Cd2 O7 108.5(2) . . ? O6 Cd2 O7 55.0(2) . . ? N1 Cd2 O7 85.9(2) . . ? O2 Cd2 C15 126.9(2) . . ? O15 Cd2 C15 95.3(2) . . ? N2 Cd2 C15 134.0(3) . . ? O6 Cd2 C15 27.6(2) . . ? N1 Cd2 C15 87.4(2) . . ? O7 Cd2 C15 27.4(2) . . ? O11 Cd3 O14 142.1(3) . . ? O11 Cd3 O16 87.6(3) . . ? O14 Cd3 O16 84.1(3) . . ? O11 Cd3 N5 122.3(3) . . ? O14 Cd3 N5 93.9(3) . . ? O16 Cd3 N5 86.1(3) . . ? O11 Cd3 N6 108.0(3) . . ? O14 Cd3 N6 92.9(3) . . ? O16 Cd3 N6 156.8(3) . . ? N5 Cd3 N6 71.1(3) . . ? O11 Cd3 H16B 74.7 . . ? O14 Cd3 H16B 84.7 . . ? O16 Cd3 H16B 21.6 . . ? N5 Cd3 H16B 107.6 . . ? N6 Cd3 H16B 177.3 . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 2.846 _refine_diff_density_min -1.320 _refine_diff_density_rms 0.105 #===END