# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2011 data_global #TrackingRef '- Cifs.txt' _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Wei-Shan Li' _publ_contact_author_email liwsh@scnu.edu.cn _publ_section_title ; Synthesis, Crystal Structures, and Properties of Ln(III)-Cu(I)-Na(I) and Ln(III)-Ag(I) Heterometallic Coordination Polymers ; loop_ _publ_author_name 'Rong-Hua Zeng.' 'Guo Peng.' 'Yong-Cai Qiu.' 'Wei-Xiong Zhang.' ; Wei-Shan Li ; 'Matthias Zeller.' 'Sheng-Run Zheng.' 'Hong Deng.' 'Yue-Peng Cai.' ###################################################################### data_4 #TrackingRef '- Cifs.txt' _database_code_depnum_ccdc_archive 'CCDC 718833' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H32 Cu6 I5 N6 Na O20 Tb2, 0.5(H4 O2)' _chemical_formula_sum 'C38 H34 Cu6 I5 N6 Na O21 Tb2' _chemical_formula_weight 2267.28 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 '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 '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.1322(15) _cell_length_b 11.260(3) _cell_length_c 18.161(4) _cell_angle_alpha 86.072(3) _cell_angle_beta 79.964(3) _cell_angle_gamma 72.880(2) _cell_volume 1372.3(6) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2360 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 26.32 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.744 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1052 _exptl_absorpt_coefficient_mu 7.718 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.252 _exptl_absorpt_correction_T_max 0.295 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II area-detector diffractometer' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6878 _diffrn_reflns_av_R_equivalents 0.0273 _diffrn_reflns_av_sigmaI/netI 0.0558 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 25.20 _reflns_number_total 4868 _reflns_number_gt 3945 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0743P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4868 _refine_ls_number_parameters 386 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0580 _refine_ls_R_factor_gt 0.0459 _refine_ls_wR_factor_ref 0.1209 _refine_ls_wR_factor_gt 0.1113 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.004 _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 0.6230(12) 0.6509(8) 0.3782(4) 0.0235(18) Uani 1 1 d . . . C2 C 0.6089(12) 0.6195(8) 0.3012(5) 0.0250(19) Uani 1 1 d . . . C3 C 0.6840(14) 0.4982(9) 0.2764(5) 0.033(2) Uani 1 1 d . . . H3 H 0.7403 0.4342 0.3081 0.040 Uiso 1 1 calc R . . C4 C 0.6737(15) 0.4743(10) 0.2041(6) 0.039(2) Uani 1 1 d . . . H4 H 0.7231 0.3925 0.1882 0.047 Uiso 1 1 calc R . . C5 C 0.5241(13) 0.6806(8) 0.1792(5) 0.0273(19) Uani 1 1 d . . . H5 H 0.4679 0.7431 0.1467 0.033 Uiso 1 1 calc R . . C6 C 0.5313(14) 0.7109(9) 0.2504(5) 0.034(2) Uani 1 1 d . . . H6 H 0.4838 0.7935 0.2648 0.041 Uiso 1 1 calc R . . C7 C 0.8372(16) 0.7889(9) 0.6461(5) 0.036(2) Uani 1 1 d . . . C8 C 0.8929(13) 0.8218(9) 0.7168(5) 0.030(2) Uani 1 1 d . . . C9 C 1.0660(16) 0.8513(10) 0.7177(5) 0.042(3) Uani 1 1 d . . . H9 H 1.1550 0.8514 0.6737 0.050 Uiso 1 1 calc R . . C10 C 1.1060(15) 0.8805(10) 0.7841(6) 0.040(2) Uani 1 1 d . . . H10 H 1.2218 0.9029 0.7836 0.048 Uiso 1 1 calc R . . C11 C 0.8245(17) 0.8483(13) 0.8478(6) 0.057(3) Uani 1 1 d . . . H11 H 0.7402 0.8464 0.8929 0.068 Uiso 1 1 calc R . . C12 C 0.7700(16) 0.8196(11) 0.7847(6) 0.049(3) Uani 1 1 d . . . H12 H 0.6521 0.7989 0.7870 0.059 Uiso 1 1 calc R . . C13 C 0.8951(11) 0.4240(8) 0.6007(4) 0.0196(17) Uani 1 1 d . . . C14 C 0.9036(11) 0.3927(8) 0.6822(4) 0.0209(18) Uani 1 1 d . . . C15 C 0.8287(12) 0.4851(8) 0.7355(4) 0.0252(19) Uani 1 1 d . . . H15 H 0.7676 0.5665 0.7216 0.030 Uiso 1 1 calc R . . C16 C 0.8466(14) 0.4539(9) 0.8087(5) 0.034(2) Uani 1 1 d . . . H16 H 0.7990 0.5171 0.8434 0.041 Uiso 1 1 calc R . . C17 C 0.9971(13) 0.2509(9) 0.7822(5) 0.030(2) Uani 1 1 d . . . H17 H 1.0540 0.1699 0.7979 0.036 Uiso 1 1 calc R . . C18 C 0.9890(13) 0.2738(8) 0.7065(5) 0.028(2) Uani 1 1 d . . . H18 H 1.0408 0.2094 0.6726 0.034 Uiso 1 1 calc R . . C19 C 0.3995(12) 0.9941(7) 0.5171(5) 0.0210(17) Uani 1 1 d . . . N1 N 0.5966(11) 0.5621(7) 0.1552(4) 0.0314(18) Uani 1 1 d . . . N2 N 0.9885(12) 0.8786(8) 0.8495(4) 0.040(2) Uani 1 1 d . . . N3 N 0.9272(11) 0.3395(7) 0.8334(4) 0.0278(17) Uani 1 1 d . . . O1 O 0.5738(9) 0.7628(5) 0.3973(3) 0.0285(14) Uani 1 1 d . . . O2 O 0.6889(9) 0.5645(6) 0.4229(3) 0.0280(14) Uani 1 1 d . . . O3 O 0.6607(11) 0.7853(6) 0.6466(4) 0.0408(17) Uani 1 1 d . . . O4 O 0.9685(10) 0.7639(7) 0.5882(4) 0.049(2) Uani 1 1 d . . . O5 O 0.7928(10) 0.5292(6) 0.5842(3) 0.0341(15) Uani 1 1 d . . . O6 O 0.9951(8) 0.3399(5) 0.5545(3) 0.0278(14) Uani 1 1 d . . . O7 O 0.3893(8) 0.8886(5) 0.5399(4) 0.0288(14) Uani 1 1 d . . . O8 O 0.2513(8) 1.0902(5) 0.5194(4) 0.0292(14) Uani 1 1 d . . . O9 O 0.3928(9) 0.6556(6) 0.5551(4) 0.0325(15) Uani 1 1 d D . . H9A H 0.286(7) 0.702(7) 0.548(5) 0.049 Uiso 1 1 d D . . H9B H 0.380(13) 0.595(6) 0.581(5) 0.049 Uiso 1 1 d D . . O10 O 0.1727(14) 0.8940(11) 0.4007(6) 0.079(3) Uani 1 1 d D . . H10A H 0.17(2) 0.824(7) 0.391(9) 0.119 Uiso 1 1 d D . . H10B H 0.265(18) 0.913(13) 0.374(8) 0.119 Uiso 1 1 d D . . O11 O 0.597(3) 0.9798(17) 0.3016(13) 0.079(6) Uani 0.50 1 d PD . . H11A H 0.52(3) 1.045(13) 0.320(18) 0.119 Uiso 0.50 1 d PD . . H11B H 0.55(4) 0.921(15) 0.315(17) 0.119 Uiso 0.50 1 d PD . . I3 I 1.23578(9) 0.08767(6) 0.94419(4) 0.03535(18) Uani 1 1 d . . . Cu3 Cu 0.9386(2) 0.29459(14) 0.94323(7) 0.0489(4) Uani 1 1 d . . . Cu2 Cu 1.0512(2) 0.91923(17) 0.94668(8) 0.0614(5) Uani 1 1 d . . . Cu1 Cu 0.6084(2) 0.52014(13) 0.04766(7) 0.0430(3) Uani 1 1 d . . . Na1 Na -0.0196(17) 1.0393(9) 0.4901(7) 0.052(3) Uani 0.50 1 d P . . I2 I 1.0000 0.5000 1.0000 0.0462(3) Uani 1 2 d S . . I1 I 0.59603(9) 0.29302(6) 0.02894(4) 0.03255(17) Uani 1 1 d . . . Tb1 Tb 0.69288(6) 0.71462(3) 0.52064(2) 0.01951(14) 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 0.023(4) 0.034(5) 0.015(4) 0.000(4) -0.008(3) -0.008(4) C2 0.022(4) 0.029(5) 0.024(5) -0.001(4) 0.001(4) -0.010(4) C3 0.038(5) 0.036(6) 0.026(5) -0.002(4) -0.011(4) -0.007(4) C4 0.043(6) 0.039(6) 0.032(5) -0.007(5) -0.012(5) -0.001(5) C5 0.035(5) 0.028(5) 0.021(4) 0.005(4) -0.006(4) -0.013(4) C6 0.041(5) 0.029(5) 0.036(6) -0.003(4) -0.009(5) -0.015(4) C7 0.057(7) 0.025(5) 0.023(5) -0.008(4) -0.016(5) 0.001(5) C8 0.036(5) 0.034(5) 0.020(4) -0.009(4) -0.009(4) -0.003(4) C9 0.048(6) 0.060(7) 0.023(5) -0.003(5) -0.004(4) -0.024(5) C10 0.036(5) 0.052(7) 0.037(6) -0.001(5) -0.010(5) -0.018(5) C11 0.055(7) 0.101(10) 0.030(6) -0.008(6) 0.002(5) -0.051(7) C12 0.046(6) 0.071(9) 0.036(6) -0.015(6) -0.002(5) -0.025(6) C13 0.019(4) 0.021(5) 0.021(4) 0.011(4) -0.003(3) -0.012(3) C14 0.015(4) 0.028(5) 0.017(4) 0.006(3) 0.002(3) -0.007(3) C15 0.025(4) 0.028(5) 0.018(4) 0.005(4) -0.001(4) -0.003(4) C16 0.037(5) 0.031(6) 0.031(5) -0.017(4) 0.002(4) -0.005(4) C17 0.030(5) 0.030(5) 0.028(5) 0.003(4) -0.010(4) -0.003(4) C18 0.026(4) 0.026(5) 0.031(5) -0.001(4) -0.002(4) -0.006(4) C19 0.023(4) 0.018(5) 0.019(4) -0.005(3) -0.005(3) 0.000(3) N1 0.032(4) 0.043(5) 0.021(4) -0.001(4) -0.006(3) -0.013(4) N2 0.041(5) 0.059(6) 0.026(4) -0.015(4) 0.000(4) -0.023(4) N3 0.032(4) 0.035(5) 0.016(4) 0.003(3) -0.001(3) -0.012(3) O1 0.030(3) 0.026(4) 0.029(3) -0.002(3) -0.008(3) -0.005(3) O2 0.043(4) 0.030(4) 0.015(3) -0.003(3) -0.007(3) -0.013(3) O3 0.049(4) 0.041(4) 0.036(4) -0.009(3) -0.015(3) -0.011(3) O4 0.047(4) 0.063(5) 0.022(4) -0.017(4) -0.008(3) 0.013(4) O5 0.045(4) 0.032(4) 0.019(3) 0.005(3) -0.005(3) -0.003(3) O6 0.025(3) 0.030(4) 0.025(3) -0.007(3) 0.003(3) -0.005(3) O7 0.022(3) 0.016(3) 0.044(4) 0.004(3) -0.001(3) -0.004(2) O8 0.014(3) 0.024(3) 0.047(4) 0.000(3) 0.000(3) -0.004(2) O9 0.025(3) 0.022(4) 0.048(4) 0.004(3) 0.000(3) -0.008(3) O10 0.063(6) 0.093(8) 0.078(7) -0.035(6) -0.026(5) -0.002(5) O11 0.107(16) 0.042(11) 0.085(14) -0.010(11) 0.014(12) -0.032(11) I3 0.0370(4) 0.0364(4) 0.0332(4) 0.0032(3) -0.0065(3) -0.0117(3) Cu3 0.0531(8) 0.0632(10) 0.0273(7) 0.0072(6) -0.0053(6) -0.0144(7) Cu2 0.0655(10) 0.0999(13) 0.0354(8) -0.0224(8) -0.0021(7) -0.0482(9) Cu1 0.0523(8) 0.0523(8) 0.0267(7) -0.0043(6) -0.0096(6) -0.0159(6) Na1 0.031(5) 0.085(11) 0.046(7) -0.007(7) 0.004(4) -0.030(8) I2 0.0284(5) 0.0576(7) 0.0538(6) -0.0285(5) 0.0071(4) -0.0161(4) I1 0.0302(3) 0.0308(4) 0.0352(4) 0.0016(3) -0.0031(3) -0.0084(3) Tb1 0.0223(2) 0.0163(2) 0.0180(2) -0.00080(16) -0.00184(16) -0.00336(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 C1 O2 1.259(10) . ? C1 O1 1.259(10) . ? C1 C2 1.493(11) . ? C2 C3 1.387(12) . ? C2 C6 1.389(13) . ? C3 C4 1.378(12) . ? C3 H3 0.9300 . ? C4 N1 1.341(13) . ? C4 H4 0.9300 . ? C5 N1 1.353(11) . ? C5 C6 1.373(12) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 O4 1.266(12) . ? C7 O3 1.270(12) . ? C7 C8 1.509(11) . ? C8 C9 1.373(13) . ? C8 C12 1.385(14) . ? C9 C10 1.370(13) . ? C9 H9 0.9300 . ? C10 N2 1.331(13) . ? C10 H10 0.9300 . ? C11 N2 1.317(13) . ? C11 C12 1.360(14) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 O5 1.242(10) . ? C13 O6 1.270(9) . ? C13 C14 1.505(11) . ? C14 C18 1.375(12) . ? C14 C15 1.391(11) . ? C15 C16 1.369(13) . ? C15 H15 0.9300 . ? C16 N3 1.329(12) . ? C16 H16 0.9300 . ? C17 N3 1.335(11) . ? C17 C18 1.389(13) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 O7 1.250(10) . ? C19 O8 1.267(9) . ? C19 C19 1.499(16) 2_676 ? C19 Na1 2.869(14) 2_576 ? N1 Cu1 2.023(7) . ? N2 Cu2 2.008(8) . ? N3 Cu3 2.034(7) . ? O1 Tb1 2.502(6) . ? O2 Tb1 2.543(5) . ? O3 Tb1 2.424(6) . ? O4 Na1 2.632(13) 2_676 ? O4 Tb1 2.694(7) . ? O5 Tb1 2.298(6) . ? O6 Tb1 2.333(5) 2_766 ? O7 Tb1 2.445(6) . ? O7 Na1 2.663(13) 2_576 ? O8 Na1 2.323(13) . ? O8 Tb1 2.390(6) 2_676 ? O8 Na1 2.539(12) 2_576 ? O9 Tb1 2.393(6) . ? O9 H9A 0.81(7) . ? O9 H9B 0.82(8) . ? O10 Na1 2.157(15) 2_576 ? O10 Na1 2.336(14) . ? O10 H10A 0.83(8) . ? O10 H10B 0.82(14) . ? O11 H11A 0.82(2) . ? O11 H11B 0.82(2) . ? I3 Cu2 2.6019(16) 1_545 ? I3 Cu2 2.6042(16) 2_767 ? I3 Cu3 2.6499(16) . ? Cu3 I1 2.6623(15) 1_556 ? Cu3 I2 2.7722(15) . ? Cu3 Cu2 3.014(2) 2_767 ? Cu2 I3 2.6019(16) 1_565 ? Cu2 I3 2.6042(16) 2_767 ? Cu2 Cu2 2.608(3) 2_777 ? Cu2 I1 2.990(2) 2_766 ? Cu2 Cu3 3.014(2) 2_767 ? Cu1 I1 2.6316(15) . ? Cu1 I1 2.6433(16) 2_665 ? Cu1 Cu1 2.655(2) 2_665 ? Cu1 I2 2.7225(15) 1_554 ? Na1 Na1 0.916(18) 2_576 ? Na1 O10 2.157(15) 2_576 ? Na1 O8 2.539(12) 2_576 ? Na1 O4 2.632(13) 2_676 ? Na1 O7 2.663(13) 2_576 ? Na1 C19 2.869(14) 2_576 ? Na1 Tb1 4.088(11) 2_676 ? I2 Cu1 2.7225(15) 1_556 ? I2 Cu1 2.7225(15) 2_766 ? I2 Cu3 2.7722(15) 2_767 ? I1 Cu1 2.6433(16) 2_665 ? I1 Cu3 2.6623(15) 1_554 ? I1 Cu2 2.990(2) 2_766 ? Tb1 O6 2.333(5) 2_766 ? Tb1 O8 2.390(6) 2_676 ? Tb1 Na1 4.088(11) 2_676 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 C1 O1 120.7(7) . . ? O2 C1 C2 119.1(7) . . ? O1 C1 C2 120.2(8) . . ? C3 C2 C6 117.5(8) . . ? C3 C2 C1 120.9(8) . . ? C6 C2 C1 121.5(8) . . ? C4 C3 C2 118.8(9) . . ? C4 C3 H3 120.6 . . ? C2 C3 H3 120.6 . . ? N1 C4 C3 123.8(9) . . ? N1 C4 H4 118.1 . . ? C3 C4 H4 118.1 . . ? N1 C5 C6 121.7(9) . . ? N1 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? C5 C6 C2 120.7(8) . . ? C5 C6 H6 119.7 . . ? C2 C6 H6 119.7 . . ? O4 C7 O3 121.9(8) . . ? O4 C7 C8 119.1(9) . . ? O3 C7 C8 119.0(8) . . ? C9 C8 C12 117.4(8) . . ? C9 C8 C7 122.5(9) . . ? C12 C8 C7 120.0(9) . . ? C10 C9 C8 119.2(9) . . ? C10 C9 H9 120.4 . . ? C8 C9 H9 120.4 . . ? N2 C10 C9 123.6(9) . . ? N2 C10 H10 118.2 . . ? C9 C10 H10 118.2 . . ? N2 C11 C12 124.4(10) . . ? N2 C11 H11 117.8 . . ? C12 C11 H11 117.8 . . ? C11 C12 C8 119.0(10) . . ? C11 C12 H12 120.5 . . ? C8 C12 H12 120.5 . . ? O5 C13 O6 125.6(8) . . ? O5 C13 C14 117.8(7) . . ? O6 C13 C14 116.6(8) . . ? C18 C14 C15 117.7(8) . . ? C18 C14 C13 121.8(7) . . ? C15 C14 C13 120.4(8) . . ? C16 C15 C14 118.8(9) . . ? C16 C15 H15 120.6 . . ? C14 C15 H15 120.6 . . ? N3 C16 C15 124.4(8) . . ? N3 C16 H16 117.8 . . ? C15 C16 H16 117.8 . . ? N3 C17 C18 123.1(9) . . ? N3 C17 H17 118.4 . . ? C18 C17 H17 118.4 . . ? C14 C18 C17 119.3(8) . . ? C14 C18 H18 120.3 . . ? C17 C18 H18 120.3 . . ? O7 C19 O8 124.4(8) . . ? O7 C19 C19 117.2(9) . 2_676 ? O8 C19 C19 118.4(9) . 2_676 ? O7 C19 Na1 67.8(5) . 2_576 ? O8 C19 Na1 62.2(5) . 2_576 ? C19 C19 Na1 153.3(8) 2_676 2_576 ? C4 N1 C5 117.5(8) . . ? C4 N1 Cu1 120.8(6) . . ? C5 N1 Cu1 121.5(6) . . ? C11 N2 C10 116.4(8) . . ? C11 N2 Cu2 120.4(7) . . ? C10 N2 Cu2 123.2(7) . . ? C16 N3 C17 116.6(8) . . ? C16 N3 Cu3 123.5(6) . . ? C17 N3 Cu3 119.9(6) . . ? C1 O1 Tb1 94.8(5) . . ? C1 O2 Tb1 92.9(5) . . ? C7 O3 Tb1 99.8(5) . . ? C7 O4 Na1 114.1(7) . 2_676 ? C7 O4 Tb1 87.3(6) . . ? Na1 O4 Tb1 100.3(4) 2_676 . ? C13 O5 Tb1 160.4(6) . . ? C13 O6 Tb1 137.7(5) . 2_766 ? C19 O7 Tb1 118.2(5) . . ? C19 O7 Na1 86.4(5) . 2_576 ? Tb1 O7 Na1 141.0(3) . 2_576 ? C19 O8 Na1 109.9(5) . . ? C19 O8 Tb1 118.8(5) . 2_676 ? Na1 O8 Tb1 120.3(3) . 2_676 ? C19 O8 Na1 91.6(5) . 2_576 ? Tb1 O8 Na1 141.3(3) 2_676 2_576 ? Tb1 O9 H9A 121(6) . . ? Tb1 O9 H9B 126(6) . . ? H9A O9 H9B 112(9) . . ? Na1 O10 H10A 115(10) 2_576 . ? Na1 O10 H10A 133(10) . . ? Na1 O10 H10B 130(10) 2_576 . ? Na1 O10 H10B 117(10) . . ? H10A O10 H10B 111(15) . . ? H11A O11 H11B 111(4) . . ? Cu2 I3 Cu2 60.12(5) 1_545 2_767 ? Cu2 I3 Cu3 101.31(6) 1_545 . ? Cu2 I3 Cu3 70.02(5) 2_767 . ? N3 Cu3 I3 105.4(2) . . ? N3 Cu3 I1 116.3(2) . 1_556 ? I3 Cu3 I1 116.31(6) . 1_556 ? N3 Cu3 I2 104.0(2) . . ? I3 Cu3 I2 114.77(5) . . ? I1 Cu3 I2 99.73(5) 1_556 . ? N3 Cu3 Cu2 141.5(2) . 2_767 ? I3 Cu3 Cu2 54.28(4) . 2_767 ? I1 Cu3 Cu2 63.21(5) 1_556 2_767 ? I2 Cu3 Cu2 114.18(5) . 2_767 ? N2 Cu2 I3 117.7(3) . 1_565 ? N2 Cu2 I3 110.6(2) . 2_767 ? I3 Cu2 I3 119.88(5) 1_565 2_767 ? N2 Cu2 Cu2 144.7(3) . 2_777 ? I3 Cu2 Cu2 59.99(6) 1_565 2_777 ? I3 Cu2 Cu2 59.90(6) 2_767 2_777 ? N2 Cu2 I1 103.2(3) . 2_766 ? I3 Cu2 I1 94.54(5) 1_565 2_766 ? I3 Cu2 I1 107.34(6) 2_767 2_766 ? Cu2 Cu2 I1 112.12(9) 2_777 2_766 ? N2 Cu2 Cu3 110.3(3) . 2_767 ? I3 Cu2 Cu3 127.07(6) 1_565 2_767 ? I3 Cu2 Cu3 55.70(4) 2_767 2_767 ? Cu2 Cu2 Cu3 92.22(9) 2_777 2_767 ? I1 Cu2 Cu3 52.64(4) 2_766 2_767 ? N1 Cu1 I1 114.3(2) . . ? N1 Cu1 I1 113.1(2) . 2_665 ? I1 Cu1 I1 119.57(5) . 2_665 ? N1 Cu1 Cu1 143.0(2) . 2_665 ? I1 Cu1 Cu1 60.00(5) . 2_665 ? I1 Cu1 Cu1 59.57(5) 2_665 2_665 ? N1 Cu1 I2 97.7(2) . 1_554 ? I1 Cu1 I2 101.79(5) . 1_554 ? I1 Cu1 I2 106.79(5) 2_665 1_554 ? Cu1 Cu1 I2 119.36(7) 2_665 1_554 ? Na1 Na1 O10 89.5(16) 2_576 2_576 ? Na1 Na1 O8 92.8(15) 2_576 . ? O10 Na1 O8 86.7(5) 2_576 . ? Na1 Na1 O10 67.4(15) 2_576 . ? O10 Na1 O10 156.9(5) 2_576 . ? O8 Na1 O10 94.2(5) . . ? Na1 Na1 O8 66.1(14) 2_576 2_576 ? O10 Na1 O8 92.9(5) 2_576 2_576 ? O8 Na1 O8 158.9(4) . 2_576 ? O10 Na1 O8 78.2(5) . 2_576 ? Na1 Na1 O4 155.4(17) 2_576 2_676 ? O10 Na1 O4 106.0(5) 2_576 2_676 ? O8 Na1 O4 69.8(4) . 2_676 ? O10 Na1 O4 95.9(5) . 2_676 ? O8 Na1 O4 130.1(5) 2_576 2_676 ? Na1 Na1 O7 115.2(16) 2_576 2_576 ? O10 Na1 O7 81.6(5) 2_576 2_576 ? O8 Na1 O7 149.4(5) . 2_576 ? O10 Na1 O7 107.6(5) . 2_576 ? O8 Na1 O7 50.6(3) 2_576 2_576 ? O4 Na1 O7 86.4(4) 2_676 2_576 ? Na1 Na1 C19 89.4(14) 2_576 2_576 ? O10 Na1 C19 81.0(5) 2_576 2_576 ? O8 Na1 C19 167.4(6) . 2_576 ? O10 Na1 C19 98.1(5) . 2_576 ? O8 Na1 C19 26.2(2) 2_576 2_576 ? O4 Na1 C19 111.5(4) 2_676 2_576 ? O7 Na1 C19 25.8(2) 2_576 2_576 ? Na1 Na1 Tb1 123.0(16) 2_576 2_676 ? O10 Na1 Tb1 90.1(5) 2_576 2_676 ? O8 Na1 Tb1 30.3(2) . 2_676 ? O10 Na1 Tb1 102.2(5) . 2_676 ? O8 Na1 Tb1 170.5(4) 2_576 2_676 ? O4 Na1 Tb1 40.4(2) 2_676 2_676 ? O7 Na1 Tb1 121.1(3) 2_576 2_676 ? C19 Na1 Tb1 146.5(4) 2_576 2_676 ? Cu1 I2 Cu1 180.00(5) 1_556 2_766 ? Cu1 I2 Cu3 105.07(4) 1_556 2_767 ? Cu1 I2 Cu3 74.93(4) 2_766 2_767 ? Cu1 I2 Cu3 74.93(4) 1_556 . ? Cu1 I2 Cu3 105.07(4) 2_766 . ? Cu3 I2 Cu3 180.0 2_767 . ? Cu1 I1 Cu1 60.43(5) . 2_665 ? Cu1 I1 Cu3 78.31(5) . 1_554 ? Cu1 I1 Cu3 92.26(5) 2_665 1_554 ? Cu1 I1 Cu2 118.29(5) . 2_766 ? Cu1 I1 Cu2 154.93(5) 2_665 2_766 ? Cu3 I1 Cu2 64.15(5) 1_554 2_766 ? O5 Tb1 O6 87.6(2) . 2_766 ? O5 Tb1 O8 148.1(2) . 2_676 ? O6 Tb1 O8 76.0(2) 2_766 2_676 ? O5 Tb1 O9 76.7(2) . . ? O6 Tb1 O9 143.2(2) 2_766 . ? O8 Tb1 O9 131.5(2) 2_676 . ? O5 Tb1 O3 78.6(2) . . ? O6 Tb1 O3 119.5(2) 2_766 . ? O8 Tb1 O3 85.8(2) 2_676 . ? O9 Tb1 O3 90.1(2) . . ? O5 Tb1 O7 132.2(2) . . ? O6 Tb1 O7 140.0(2) 2_766 . ? O8 Tb1 O7 67.14(18) 2_676 . ? O9 Tb1 O7 65.3(2) . . ? O3 Tb1 O7 73.7(2) . . ? O5 Tb1 O1 131.0(2) . . ? O6 Tb1 O1 82.9(2) 2_766 . ? O8 Tb1 O1 74.6(2) 2_676 . ? O9 Tb1 O1 82.8(2) . . ? O3 Tb1 O1 145.9(2) . . ? O7 Tb1 O1 73.0(2) . . ? O5 Tb1 O2 80.0(2) . . ? O6 Tb1 O2 71.87(19) 2_766 . ? O8 Tb1 O2 119.1(2) 2_676 . ? O9 Tb1 O2 72.7(2) . . ? O3 Tb1 O2 155.1(2) . . ? O7 Tb1 O2 112.9(2) . . ? O1 Tb1 O2 51.39(19) . . ? O5 Tb1 O4 80.9(2) . . ? O6 Tb1 O4 68.8(2) 2_766 . ? O8 Tb1 O4 67.7(2) 2_676 . ? O9 Tb1 O4 138.4(2) . . ? O3 Tb1 O4 51.0(2) . . ? O7 Tb1 O4 108.8(2) . . ? O1 Tb1 O4 137.0(2) . . ? O2 Tb1 O4 136.63(19) . . ? O5 Tb1 Na1 118.7(2) . 2_676 ? O6 Tb1 Na1 63.4(2) 2_766 2_676 ? O8 Tb1 Na1 29.4(2) 2_676 2_676 ? O9 Tb1 Na1 152.7(2) . 2_676 ? O3 Tb1 Na1 72.7(2) . 2_676 ? O7 Tb1 Na1 89.2(2) . 2_676 ? O1 Tb1 Na1 99.4(2) . 2_676 ? O2 Tb1 Na1 129.6(2) . 2_676 ? O4 Tb1 Na1 39.3(2) . 2_676 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 C1 C2 C3 -6.0(12) . . . . ? O1 C1 C2 C3 172.4(8) . . . . ? O2 C1 C2 C6 177.9(8) . . . . ? O1 C1 C2 C6 -3.7(13) . . . . ? C6 C2 C3 C4 -1.5(13) . . . . ? C1 C2 C3 C4 -177.8(8) . . . . ? C2 C3 C4 N1 0.7(15) . . . . ? N1 C5 C6 C2 -1.9(14) . . . . ? C3 C2 C6 C5 2.1(13) . . . . ? C1 C2 C6 C5 178.4(8) . . . . ? O4 C7 C8 C9 14.0(15) . . . . ? O3 C7 C8 C9 -167.0(10) . . . . ? O4 C7 C8 C12 -164.2(10) . . . . ? O3 C7 C8 C12 14.8(14) . . . . ? C12 C8 C9 C10 -2.0(16) . . . . ? C7 C8 C9 C10 179.8(9) . . . . ? C8 C9 C10 N2 2.1(17) . . . . ? N2 C11 C12 C8 0(2) . . . . ? C9 C8 C12 C11 1.0(17) . . . . ? C7 C8 C12 C11 179.3(11) . . . . ? O5 C13 C14 C18 170.6(8) . . . . ? O6 C13 C14 C18 -9.8(11) . . . . ? O5 C13 C14 C15 -11.1(11) . . . . ? O6 C13 C14 C15 168.6(7) . . . . ? C18 C14 C15 C16 1.1(12) . . . . ? C13 C14 C15 C16 -177.3(8) . . . . ? C14 C15 C16 N3 -1.7(14) . . . . ? C15 C14 C18 C17 0.0(12) . . . . ? C13 C14 C18 C17 178.4(8) . . . . ? N3 C17 C18 C14 -0.7(14) . . . . ? C3 C4 N1 C5 -0.4(15) . . . . ? C3 C4 N1 Cu1 175.0(8) . . . . ? C6 C5 N1 C4 1.0(13) . . . . ? C6 C5 N1 Cu1 -174.3(7) . . . . ? C12 C11 N2 C10 0.0(19) . . . . ? C12 C11 N2 Cu2 179.9(10) . . . . ? C9 C10 N2 C11 -1.0(17) . . . . ? C9 C10 N2 Cu2 179.0(8) . . . . ? C15 C16 N3 C17 1.0(14) . . . . ? C15 C16 N3 Cu3 -176.7(7) . . . . ? C18 C17 N3 C16 0.2(13) . . . . ? C18 C17 N3 Cu3 178.0(7) . . . . ? O2 C1 O1 Tb1 5.6(8) . . . . ? C2 C1 O1 Tb1 -172.7(7) . . . . ? O1 C1 O2 Tb1 -5.5(8) . . . . ? C2 C1 O2 Tb1 172.9(7) . . . . ? O4 C7 O3 Tb1 2.6(10) . . . . ? C8 C7 O3 Tb1 -176.3(7) . . . . ? O3 C7 O4 Na1 97.7(10) . . . 2_676 ? C8 C7 O4 Na1 -83.4(9) . . . 2_676 ? O3 C7 O4 Tb1 -2.3(9) . . . . ? C8 C7 O4 Tb1 176.6(8) . . . . ? O6 C13 O5 Tb1 -37(2) . . . . ? C14 C13 O5 Tb1 142.3(14) . . . . ? O5 C13 O6 Tb1 83.8(11) . . . 2_766 ? C14 C13 O6 Tb1 -95.9(9) . . . 2_766 ? O8 C19 O7 Tb1 175.5(6) . . . . ? C19 C19 O7 Tb1 -2.9(11) 2_676 . . . ? Na1 C19 O7 Tb1 148.2(5) 2_576 . . . ? O8 C19 O7 Na1 27.3(8) . . . 2_576 ? C19 C19 O7 Na1 -151.1(9) 2_676 . . 2_576 ? O7 C19 O8 Na1 -39.4(10) . . . . ? C19 C19 O8 Na1 138.9(8) 2_676 . . . ? Na1 C19 O8 Na1 -10.7(6) 2_576 . . . ? O7 C19 O8 Tb1 176.4(6) . . . 2_676 ? C19 C19 O8 Tb1 -5.3(12) 2_676 . . 2_676 ? Na1 C19 O8 Tb1 -154.9(6) 2_576 . . 2_676 ? O7 C19 O8 Na1 -28.7(9) . . . 2_576 ? C19 C19 O8 Na1 149.7(9) 2_676 . . 2_576 ? C16 N3 Cu3 I3 -157.1(7) . . . . ? C17 N3 Cu3 I3 25.3(7) . . . . ? C16 N3 Cu3 I1 72.5(7) . . . 1_556 ? C17 N3 Cu3 I1 -105.2(6) . . . 1_556 ? C16 N3 Cu3 I2 -36.0(7) . . . . ? C17 N3 Cu3 I2 146.3(6) . . . . ? C16 N3 Cu3 Cu2 151.7(6) . . . 2_767 ? C17 N3 Cu3 Cu2 -26.0(8) . . . 2_767 ? Cu2 I3 Cu3 N3 -91.1(2) 1_545 . . . ? Cu2 I3 Cu3 N3 -143.3(2) 2_767 . . . ? Cu2 I3 Cu3 I1 39.27(7) 1_545 . . 1_556 ? Cu2 I3 Cu3 I1 -12.90(5) 2_767 . . 1_556 ? Cu2 I3 Cu3 I2 155.10(5) 1_545 . . . ? Cu2 I3 Cu3 I2 102.93(6) 2_767 . . . ? Cu2 I3 Cu3 Cu2 52.17(6) 1_545 . . 2_767 ? C11 N2 Cu2 I3 -145.8(9) . . . 1_565 ? C10 N2 Cu2 I3 34.1(10) . . . 1_565 ? C11 N2 Cu2 I3 -2.8(10) . . . 2_767 ? C10 N2 Cu2 I3 177.1(8) . . . 2_767 ? C11 N2 Cu2 Cu2 -69.5(11) . . . 2_777 ? C10 N2 Cu2 Cu2 110.5(8) . . . 2_777 ? C11 N2 Cu2 I1 111.7(9) . . . 2_766 ? C10 N2 Cu2 I1 -68.3(9) . . . 2_766 ? C11 N2 Cu2 Cu3 57.0(10) . . . 2_767 ? C10 N2 Cu2 Cu3 -123.0(8) . . . 2_767 ? C4 N1 Cu1 I1 31.4(8) . . . . ? C5 N1 Cu1 I1 -153.5(6) . . . . ? C4 N1 Cu1 I1 172.7(7) . . . 2_665 ? C5 N1 Cu1 I1 -12.1(7) . . . 2_665 ? C4 N1 Cu1 Cu1 103.2(8) . . . 2_665 ? C5 N1 Cu1 Cu1 -81.7(8) . . . 2_665 ? C4 N1 Cu1 I2 -75.3(7) . . . 1_554 ? C5 N1 Cu1 I2 99.8(7) . . . 1_554 ? C19 O8 Na1 Na1 31.1(17) . . . 2_576 ? Tb1 O8 Na1 Na1 174.7(14) 2_676 . . 2_576 ? C19 O8 Na1 O10 120.4(7) . . . 2_576 ? Tb1 O8 Na1 O10 -96.0(5) 2_676 . . 2_576 ? Na1 O8 Na1 O10 89.4(16) 2_576 . . 2_576 ? C19 O8 Na1 O10 -36.5(7) . . . . ? Tb1 O8 Na1 O10 107.2(5) 2_676 . . . ? Na1 O8 Na1 O10 -67.5(15) 2_576 . . . ? C19 O8 Na1 O8 31.1(17) . . . 2_576 ? Tb1 O8 Na1 O8 174.7(14) 2_676 . . 2_576 ? Na1 O8 Na1 O8 0.000(4) 2_576 . . 2_576 ? C19 O8 Na1 O4 -131.2(6) . . . 2_676 ? Tb1 O8 Na1 O4 12.4(4) 2_676 . . 2_676 ? Na1 O8 Na1 O4 -162.3(17) 2_576 . . 2_676 ? C19 O8 Na1 O7 -172.2(10) . . . 2_576 ? Tb1 O8 Na1 O7 -28.6(13) 2_676 . . 2_576 ? Na1 O8 Na1 O7 157(2) 2_576 . . 2_576 ? C19 O8 Na1 C19 130.9(19) . . . 2_576 ? Tb1 O8 Na1 C19 -86(2) 2_676 . . 2_576 ? Na1 O8 Na1 C19 100(3) 2_576 . . 2_576 ? C19 O8 Na1 Tb1 -143.6(8) . . . 2_676 ? Na1 O8 Na1 Tb1 -174.7(14) 2_576 . . 2_676 ? Na1 O10 Na1 O10 0.000(3) 2_576 . . 2_576 ? Na1 O10 Na1 O8 91.3(15) 2_576 . . . ? Na1 O10 Na1 O8 -68.8(14) 2_576 . . 2_576 ? Na1 O10 Na1 O4 161.3(17) 2_576 . . 2_676 ? Na1 O10 Na1 O7 -110.6(16) 2_576 . . 2_576 ? Na1 O10 Na1 C19 -85.9(14) 2_576 . . 2_576 ? Na1 O10 Na1 Tb1 120.9(16) 2_576 . . 2_676 ? N3 Cu3 I2 Cu1 103.3(2) . . . 1_556 ? I3 Cu3 I2 Cu1 -142.07(6) . . . 1_556 ? I1 Cu3 I2 Cu1 -17.02(4) 1_556 . . 1_556 ? Cu2 Cu3 I2 Cu1 -81.91(6) 2_767 . . 1_556 ? N3 Cu3 I2 Cu1 -76.7(2) . . . 2_766 ? I3 Cu3 I2 Cu1 37.93(6) . . . 2_766 ? I1 Cu3 I2 Cu1 162.98(4) 1_556 . . 2_766 ? Cu2 Cu3 I2 Cu1 98.09(6) 2_767 . . 2_766 ? N1 Cu1 I1 Cu1 138.6(3) . . . 2_665 ? I1 Cu1 I1 Cu1 0.0 2_665 . . 2_665 ? I2 Cu1 I1 Cu1 -117.24(7) 1_554 . . 2_665 ? N1 Cu1 I1 Cu3 -121.9(2) . . . 1_554 ? I1 Cu1 I1 Cu3 99.42(6) 2_665 . . 1_554 ? Cu1 Cu1 I1 Cu3 99.42(6) 2_665 . . 1_554 ? I2 Cu1 I1 Cu3 -17.82(4) 1_554 . . 1_554 ? N1 Cu1 I1 Cu2 -70.0(2) . . . 2_766 ? I1 Cu1 I1 Cu2 151.32(6) 2_665 . . 2_766 ? Cu1 Cu1 I1 Cu2 151.32(6) 2_665 . . 2_766 ? I2 Cu1 I1 Cu2 34.08(6) 1_554 . . 2_766 ? C13 O5 Tb1 O6 -8.1(17) . . . 2_766 ? C13 O5 Tb1 O8 -66.6(18) . . . 2_676 ? C13 O5 Tb1 O9 138.3(17) . . . . ? C13 O5 Tb1 O3 -128.8(17) . . . . ? C13 O5 Tb1 O7 175.8(16) . . . . ? C13 O5 Tb1 O1 70.4(17) . . . . ? C13 O5 Tb1 O2 63.9(17) . . . . ? C13 O5 Tb1 O4 -77.0(17) . . . . ? C13 O5 Tb1 Na1 -65.9(17) . . . 2_676 ? C7 O3 Tb1 O5 86.0(6) . . . . ? C7 O3 Tb1 O6 5.4(7) . . . 2_766 ? C7 O3 Tb1 O8 -66.0(6) . . . 2_676 ? C7 O3 Tb1 O9 162.4(6) . . . . ? C7 O3 Tb1 O7 -133.4(6) . . . . ? C7 O3 Tb1 O1 -120.3(6) . . . . ? C7 O3 Tb1 O2 117.2(7) . . . . ? C7 O3 Tb1 O4 -1.3(5) . . . . ? C7 O3 Tb1 Na1 -39.1(6) . . . 2_676 ? C19 O7 Tb1 O5 153.3(5) . . . . ? Na1 O7 Tb1 O5 -83.4(6) 2_576 . . . ? C19 O7 Tb1 O6 -20.6(7) . . . 2_766 ? Na1 O7 Tb1 O6 102.7(6) 2_576 . . 2_766 ? C19 O7 Tb1 O8 3.9(6) . . . 2_676 ? Na1 O7 Tb1 O8 127.1(6) 2_576 . . 2_676 ? C19 O7 Tb1 O9 -166.0(7) . . . . ? Na1 O7 Tb1 O9 -42.7(5) 2_576 . . . ? C19 O7 Tb1 O3 96.2(6) . . . . ? Na1 O7 Tb1 O3 -140.6(6) 2_576 . . . ? C19 O7 Tb1 O1 -76.2(6) . . . . ? Na1 O7 Tb1 O1 47.1(5) 2_576 . . . ? C19 O7 Tb1 O2 -109.3(6) . . . . ? Na1 O7 Tb1 O2 13.9(6) 2_576 . . . ? C19 O7 Tb1 O4 58.6(6) . . . . ? Na1 O7 Tb1 O4 -178.2(5) 2_576 . . . ? C19 O7 Tb1 Na1 23.9(6) . . . 2_676 ? Na1 O7 Tb1 Na1 147.2(6) 2_576 . . 2_676 ? C1 O1 Tb1 O5 -11.2(6) . . . . ? C1 O1 Tb1 O6 69.4(5) . . . 2_766 ? C1 O1 Tb1 O8 146.8(5) . . . 2_676 ? C1 O1 Tb1 O9 -76.6(5) . . . . ? C1 O1 Tb1 O3 -156.1(5) . . . . ? C1 O1 Tb1 O7 -142.9(5) . . . . ? C1 O1 Tb1 O2 -3.0(5) . . . . ? C1 O1 Tb1 O4 117.5(5) . . . . ? C1 O1 Tb1 Na1 130.9(5) . . . 2_676 ? C1 O2 Tb1 O5 176.7(5) . . . . ? C1 O2 Tb1 O6 -92.5(5) . . . 2_766 ? C1 O2 Tb1 O8 -30.7(5) . . . 2_676 ? C1 O2 Tb1 O9 97.7(5) . . . . ? C1 O2 Tb1 O3 145.8(6) . . . . ? C1 O2 Tb1 O7 45.0(5) . . . . ? C1 O2 Tb1 O1 3.0(5) . . . . ? C1 O2 Tb1 O4 -118.2(5) . . . . ? C1 O2 Tb1 Na1 -64.2(6) . . . 2_676 ? C7 O4 Tb1 O5 -81.4(6) . . . . ? Na1 O4 Tb1 O5 164.6(4) 2_676 . . . ? C7 O4 Tb1 O6 -172.4(6) . . . 2_766 ? Na1 O4 Tb1 O6 73.6(4) 2_676 . . 2_766 ? C7 O4 Tb1 O8 104.5(6) . . . 2_676 ? Na1 O4 Tb1 O8 -9.5(3) 2_676 . . 2_676 ? C7 O4 Tb1 O9 -23.5(7) . . . . ? Na1 O4 Tb1 O9 -137.6(4) 2_676 . . . ? C7 O4 Tb1 O3 1.3(5) . . . . ? Na1 O4 Tb1 O3 -112.7(4) 2_676 . . . ? C7 O4 Tb1 O7 50.2(6) . . . . ? Na1 O4 Tb1 O7 -63.9(4) 2_676 . . . ? C7 O4 Tb1 O1 135.2(5) . . . . ? Na1 O4 Tb1 O1 21.2(4) 2_676 . . . ? C7 O4 Tb1 O2 -146.1(5) . . . . ? Na1 O4 Tb1 O2 99.8(4) 2_676 . . . ? C7 O4 Tb1 Na1 114.0(7) . . . 2_676 ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.20 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.860 _refine_diff_density_min -2.193 _refine_diff_density_rms 0.234 ########################################################################## data_6 #TrackingRef '- Cifs.txt' _database_code_depnum_ccdc_archive 'CCDC 718834' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H24 Ag4 Ho2 N6 O23, 2(H O0.50), 2(H2 O)' _chemical_formula_sum 'C34 H30 Ag4 Ho2 N6 O26' _chemical_formula_weight 1699.98 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ho Ho -0.2175 4.6783 '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 '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.7650(13) _cell_length_b 11.6593(17) _cell_length_c 11.9268(18) _cell_angle_alpha 77.744(2) _cell_angle_beta 76.470(2) _cell_angle_gamma 76.133(2) _cell_volume 1134.6(3) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2442 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 28.05 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.488 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 806 _exptl_absorpt_coefficient_mu 5.236 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3026 _exptl_absorpt_correction_T_max 0.4060 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite __diffrn_measurement_device_type 'Bruker APEX-II area-detector diffractometer' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5885 _diffrn_reflns_av_R_equivalents 0.0255 _diffrn_reflns_av_sigmaI/netI 0.0509 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 25.20 _reflns_number_total 4018 _reflns_number_gt 3555 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0157P)^2^+10.8876P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4018 _refine_ls_number_parameters 386 _refine_ls_number_restraints 83 _refine_ls_R_factor_all 0.0521 _refine_ls_R_factor_gt 0.0449 _refine_ls_wR_factor_ref 0.1012 _refine_ls_wR_factor_gt 0.0983 _refine_ls_goodness_of_fit_ref 1.197 _refine_ls_restrained_S_all 1.188 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ho1 Ho 0.75652(4) 0.84370(3) 0.13657(3) 0.02207(10) Uani 1 1 d . . . Ag1 Ag 1.02931(9) 0.73628(7) -0.16814(6) 0.0459(2) Uani 1 1 d . . . Ag2 Ag 0.34737(9) 0.20896(7) 0.22725(6) 0.0442(2) Uani 1 1 d . . . C1 C 1.0258(9) 0.9606(7) -0.0480(7) 0.0246(19) Uani 1 1 d . . . C2 C 0.4811(10) 1.0458(7) 0.0427(7) 0.0262(19) Uani 1 1 d . . . C3 C 1.5451(10) 0.8124(7) -0.6556(7) 0.0274(19) Uani 1 1 d . . . C4 C 1.4282(11) 0.7906(8) -0.5410(7) 0.032(2) Uani 1 1 d . . . C5 C 1.4158(11) 0.8520(7) -0.4525(7) 0.031(2) Uani 1 1 d . . . H5 H 1.4842 0.9044 -0.4611 0.037 Uiso 1 1 calc R . . C6 C 1.3038(11) 0.8375(8) -0.3508(7) 0.034(2) Uani 1 1 d . . . H6 H 1.2918 0.8847 -0.2943 0.041 Uiso 1 1 calc R . . C7 C 1.2248(12) 0.6909(9) -0.4139(8) 0.045(3) Uani 1 1 d . . . H7 H 1.1613 0.6341 -0.4014 0.053 Uiso 1 1 calc R . . C8 C 1.3340(11) 0.7056(8) -0.5206(8) 0.041(2) Uani 1 1 d . . . H8 H 1.3428 0.6588 -0.5768 0.049 Uiso 1 1 calc R . . C9 C 0.8096(9) 0.5930(7) 0.0175(8) 0.0271(19) Uani 1 1 d . . . C10 C 0.7064(10) 0.5010(7) 0.0685(8) 0.029(2) Uani 1 1 d . . . C11 C 0.5931(11) 0.5113(8) 0.1691(9) 0.042(3) Uani 1 1 d . E . H11 H 0.5831 0.5737 0.2093 0.051 Uiso 1 1 calc R . . C12 C 0.4951(11) 0.4302(8) 0.2104(8) 0.038(2) Uani 1 1 d . . . H12 H 0.4165 0.4409 0.2769 0.046 Uiso 1 1 calc R E . C13 C 0.6209(11) 0.3227(8) 0.0638(8) 0.038(2) Uani 1 1 d . . . H13 H 0.6327 0.2571 0.0276 0.045 Uiso 1 1 calc R E . C14 C 0.7217(11) 0.4020(7) 0.0165(7) 0.031(2) Uani 1 1 d . E . H14 H 0.7997 0.3894 -0.0499 0.037 Uiso 1 1 calc R . . N1 N 1.2091(9) 0.7534(6) -0.3321(6) 0.0327(18) Uani 1 1 d . . . N2 N 0.5080(9) 0.3352(6) 0.1583(6) 0.0315(17) Uani 1 1 d . E . O1 O 0.9562(7) 0.8752(5) -0.0338(5) 0.0301(14) Uani 1 1 d . . . O2 O 1.1230(7) 0.9947(5) -0.1367(5) 0.0292(14) Uani 1 1 d . . . O3 O 0.5561(7) 1.0211(5) 0.1232(5) 0.0303(14) Uani 1 1 d . . . O4 O 0.3755(7) 1.1380(5) 0.0207(5) 0.0305(14) Uani 1 1 d . . . O5 O 1.5296(7) 0.7699(5) -0.7417(5) 0.0327(14) Uani 1 1 d D . . O6 O 1.6479(7) 0.8725(6) -0.6626(5) 0.0383(16) Uani 1 1 d D . . O7 O 0.8181(7) 0.6609(5) 0.0842(5) 0.0332(15) Uani 1 1 d D . . O8 O 0.8780(7) 0.5978(5) -0.0870(5) 0.0374(16) Uani 1 1 d D . . O11 O 0.9849(9) 0.7544(6) 0.2168(7) 0.0536(19) Uani 1 1 d . . . H11A H 1.0296 0.7793 0.2586 0.080 Uiso 0.50 1 d PR A 2 H11B H 0.9961 0.6760 0.2448 0.080 Uiso 0.50 1 d PR A 2 N3 N 0.996(3) 0.6515(19) 0.2785(17) 0.064(6) Uani 0.50 1 d P B 1 O12 O 0.866(3) 0.615(2) 0.316(2) 0.109(7) Uani 0.50 1 d P B 1 O13 O 1.117(3) 0.592(3) 0.315(2) 0.137(11) Uani 0.50 1 d P B 1 O14 O 0.210(2) 0.3847(13) 0.4581(14) 0.065(5) Uani 0.50 1 d P C 1 H14A H 0.1265 0.3627 0.4585 0.098 Uiso 0.50 1 d PR C 1 H14B H 0.1881 0.4280 0.5098 0.098 Uiso 0.50 1 d PR C 1 O15 O 1.038(2) 0.5174(14) 0.2890(15) 0.066(5) Uani 0.50 1 d P D 2 H15A H 1.0205 0.4958 0.2315 0.098 Uiso 0.50 1 d PR D 2 H15B H 1.1267 0.4769 0.3017 0.098 Uiso 0.50 1 d PR D 2 O16 O 0.7507(10) 0.1442(7) 0.8432(9) 0.081(3) Uani 1 1 d D . . H16A H 0.819(4) 0.185(4) 0.841(9) 0.122 Uiso 0.50 1 d PD . . H16B H 0.679(5) 0.190(4) 0.810(5) 0.122 Uiso 1 1 d D . . H16C H 0.784(10) 0.085(3) 0.805(5) 0.122 Uiso 0.50 1 d PD . . N5 N 0.1890(11) 0.1157(9) 0.3550(7) 0.030(3) Uani 0.50 1 d PGU E -1 C15 C 0.1295(14) 0.0292(10) 0.3236(7) 0.035(4) Uani 0.50 1 d PGU E -1 H15 H 0.1598 0.0131 0.2475 0.042 Uiso 0.50 1 calc PR E -1 C16 C 0.0246(16) -0.0331(11) 0.4059(10) 0.039(4) Uani 0.50 1 d PGU E -1 H16 H -0.0153 -0.0909 0.3849 0.047 Uiso 0.50 1 calc PR E -1 C17 C -0.0208(16) -0.0090(11) 0.5196(9) 0.031(3) Uani 0.50 1 d PGU E -1 C18 C 0.0388(15) 0.0775(11) 0.5510(7) 0.033(4) Uani 0.50 1 d PGU E -1 H18 H 0.0085 0.0936 0.6270 0.040 Uiso 0.50 1 calc PR E -1 C19 C 0.1437(14) 0.1398(9) 0.4687(8) 0.033(4) Uani 0.50 1 d PGU E -1 H19 H 0.1836 0.1976 0.4897 0.039 Uiso 0.50 1 calc PR E -1 C20 C -0.136(2) -0.0843(19) 0.6084(19) 0.044(4) Uani 0.50 1 d PU E -1 O9 O -0.178(2) -0.1633(18) 0.5752(14) 0.083(5) Uani 0.50 1 d PDU . -1 O10 O -0.178(2) -0.0548(15) 0.7069(13) 0.068(5) Uani 0.50 1 d PDU . -1 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 Ho1 0.02101(19) 0.02679(19) 0.01924(18) -0.00575(14) 0.00409(14) -0.01240(15) Ag1 0.0460(4) 0.0595(5) 0.0296(4) -0.0109(3) 0.0166(3) -0.0258(4) Ag2 0.0477(4) 0.0469(4) 0.0385(4) -0.0095(3) 0.0141(3) -0.0304(4) C1 0.017(4) 0.032(4) 0.023(4) -0.007(3) 0.008(3) -0.012(3) C2 0.030(5) 0.024(4) 0.023(4) -0.004(3) 0.003(4) -0.012(4) C3 0.031(5) 0.028(4) 0.021(4) -0.002(3) 0.000(3) -0.010(4) C4 0.036(5) 0.031(5) 0.026(4) -0.010(4) 0.005(4) -0.007(4) C5 0.041(5) 0.027(4) 0.026(4) -0.003(3) 0.005(4) -0.019(4) C6 0.048(6) 0.026(4) 0.027(4) 0.000(4) -0.003(4) -0.014(4) C7 0.055(6) 0.048(6) 0.033(5) -0.011(4) 0.014(4) -0.031(5) C8 0.044(6) 0.042(5) 0.038(5) -0.013(4) 0.013(4) -0.027(4) C9 0.016(4) 0.025(4) 0.040(5) -0.002(4) -0.005(4) -0.007(3) C10 0.029(5) 0.023(4) 0.036(5) -0.002(4) 0.000(4) -0.014(4) C11 0.041(5) 0.033(5) 0.056(6) -0.029(4) 0.013(5) -0.016(4) C12 0.031(5) 0.044(5) 0.036(5) -0.015(4) 0.016(4) -0.015(4) C13 0.047(6) 0.028(5) 0.043(5) -0.012(4) -0.002(4) -0.019(4) C14 0.040(5) 0.025(4) 0.029(4) -0.010(3) 0.002(4) -0.016(4) N1 0.036(4) 0.036(4) 0.023(4) -0.005(3) 0.009(3) -0.017(3) N2 0.039(4) 0.017(3) 0.040(4) -0.005(3) -0.008(3) -0.007(3) O1 0.035(3) 0.028(3) 0.028(3) -0.010(2) 0.013(3) -0.021(3) O2 0.031(3) 0.032(3) 0.028(3) -0.014(2) 0.010(2) -0.021(3) O3 0.035(3) 0.025(3) 0.034(3) -0.011(3) -0.010(3) -0.003(3) O4 0.035(3) 0.031(3) 0.028(3) -0.009(3) -0.008(3) -0.008(3) O5 0.036(3) 0.036(3) 0.026(3) -0.005(3) 0.008(3) -0.021(3) O6 0.036(3) 0.066(4) 0.019(3) -0.009(3) 0.002(3) -0.027(3) O7 0.034(3) 0.020(3) 0.046(4) -0.006(3) -0.004(3) -0.010(3) O8 0.043(4) 0.039(4) 0.031(3) -0.004(3) 0.003(3) -0.022(3) O11 0.060(5) 0.044(4) 0.065(5) -0.004(4) -0.032(4) -0.011(4) N3 0.084(15) 0.066(13) 0.054(12) -0.015(10) -0.006(11) -0.042(12) O12 0.102(16) 0.140(19) 0.107(17) -0.031(15) -0.014(13) -0.061(15) O13 0.090(17) 0.19(3) 0.107(18) 0.031(18) -0.057(14) 0.011(18) O14 0.069(11) 0.043(9) 0.070(11) 0.013(8) -0.009(9) -0.009(8) O15 0.081(12) 0.055(10) 0.071(11) -0.004(8) -0.037(9) -0.017(9) O16 0.072(6) 0.063(5) 0.116(8) 0.008(5) -0.042(5) -0.023(5) N5 0.032(8) 0.027(7) 0.029(6) -0.003(6) 0.010(6) -0.020(6) C15 0.029(10) 0.040(9) 0.037(8) -0.022(7) 0.012(7) -0.012(7) C16 0.052(10) 0.034(9) 0.036(7) 0.001(6) -0.004(7) -0.027(7) C17 0.029(9) 0.019(7) 0.036(7) 0.006(6) 0.001(6) -0.003(5) C18 0.035(9) 0.038(9) 0.021(7) 0.001(6) 0.004(6) -0.014(7) C19 0.047(10) 0.031(9) 0.024(7) 0.005(6) -0.003(7) -0.026(7) C20 0.032(10) 0.036(9) 0.047(8) 0.025(7) -0.003(7) -0.007(7) O9 0.077(11) 0.127(12) 0.063(11) 0.002(9) -0.002(9) -0.077(10) O10 0.056(10) 0.077(11) 0.056(8) 0.000(8) 0.026(8) -0.030(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 Ho1 O7 2.254(5) . ? Ho1 O11 2.341(7) . ? Ho1 O2 2.371(5) 2_775 ? Ho1 O4 2.372(6) 2_675 ? Ho1 O3 2.375(6) . ? Ho1 O1 2.378(5) . ? Ho1 O5 2.397(5) 1_456 ? Ho1 O6 2.425(5) 1_456 ? Ho1 C3 2.739(8) 1_456 ? Ag1 N1 2.212(6) . ? Ag1 O8 2.250(6) . ? Ag1 O1 2.393(5) . ? Ag2 N5 2.112(7) . ? Ag2 N2 2.182(7) . ? Ag2 O10 2.484(15) 2_556 ? Ag2 O9 2.501(16) 2_556 ? C1 O2 1.251(9) . ? C1 O1 1.251(9) . ? C1 C1 1.539(15) 2_775 ? C2 O3 1.235(10) . ? C2 O4 1.265(10) . ? C2 C2 1.555(15) 2_675 ? C3 O6 1.246(10) . ? C3 O5 1.278(10) . ? C3 C4 1.519(11) . ? C3 Ho1 2.739(8) 1_654 ? C4 C5 1.367(11) . ? C4 C8 1.385(12) . ? C5 C6 1.378(11) . ? C5 H5 0.9300 . ? C6 N1 1.382(11) . ? C6 H6 0.9300 . ? C7 N1 1.302(11) . ? C7 C8 1.407(12) . ? C7 H7 0.9300 . ? C8 H8 0.9300 . ? C9 O8 1.246(10) . ? C9 O7 1.260(10) . ? C9 C10 1.507(11) . ? C10 C11 1.373(12) . ? C10 C14 1.388(11) . ? C11 C12 1.367(12) . ? C11 H11 0.9300 . ? C12 N2 1.351(11) . ? C12 H12 0.9300 . ? C13 N2 1.322(11) . ? C13 C14 1.374(12) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? O2 Ho1 2.371(5) 2_775 ? O4 Ho1 2.372(6) 2_675 ? O5 Ho1 2.397(5) 1_654 ? O6 Ho1 2.425(5) 1_654 ? O11 N3 1.26(2) . ? O11 H11A 0.8328 . ? O11 H11B 0.8940 . ? N3 O13 1.24(3) . ? N3 O12 1.27(3) . ? O14 H14A 0.8310 . ? O14 H14B 0.8376 . ? O15 H15A 0.8354 . ? O15 H15B 0.8365 . ? O16 H16A 0.84(2) . ? O16 H16B 0.841(19) . ? O16 H16C 0.862(17) . ? N5 C15 1.3900 . ? N5 C19 1.3900 . ? C15 C16 1.3900 . ? C15 H15 0.9300 . ? C16 C17 1.3900 . ? C16 H16 0.9300 . ? C17 C18 1.3900 . ? C17 C20 1.56(2) . ? C18 C19 1.3900 . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 O9 1.23(3) . ? C20 O10 1.24(3) . ? O9 Ag2 2.501(16) 2_556 ? O10 Ag2 2.484(15) 2_556 ? 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 O7 Ho1 O11 78.2(2) . . ? O7 Ho1 O2 140.9(2) . 2_775 ? O11 Ho1 O2 75.3(2) . 2_775 ? O7 Ho1 O4 74.1(2) . 2_675 ? O11 Ho1 O4 146.3(2) . 2_675 ? O2 Ho1 O4 116.4(2) 2_775 2_675 ? O7 Ho1 O3 139.3(2) . . ? O11 Ho1 O3 142.4(2) . . ? O2 Ho1 O3 72.8(2) 2_775 . ? O4 Ho1 O3 68.2(2) 2_675 . ? O7 Ho1 O1 79.86(19) . . ? O11 Ho1 O1 80.9(2) . . ? O2 Ho1 O1 68.07(18) 2_775 . ? O4 Ho1 O1 75.7(2) 2_675 . ? O3 Ho1 O1 104.5(2) . . ? O7 Ho1 O5 82.7(2) . 1_456 ? O11 Ho1 O5 109.5(2) . 1_456 ? O2 Ho1 O5 133.31(18) 2_775 1_456 ? O4 Ho1 O5 85.8(2) 2_675 1_456 ? O3 Ho1 O5 79.8(2) . 1_456 ? O1 Ho1 O5 157.33(19) . 1_456 ? O7 Ho1 O6 121.8(2) . 1_456 ? O11 Ho1 O6 81.0(2) . 1_456 ? O2 Ho1 O6 81.63(19) 2_775 1_456 ? O4 Ho1 O6 130.3(2) 2_675 1_456 ? O3 Ho1 O6 75.3(2) . 1_456 ? O1 Ho1 O6 147.79(19) . 1_456 ? O5 Ho1 O6 54.85(19) 1_456 1_456 ? O7 Ho1 C3 102.7(2) . 1_456 ? O11 Ho1 C3 94.9(3) . 1_456 ? O2 Ho1 C3 107.6(2) 2_775 1_456 ? O4 Ho1 C3 109.6(2) 2_675 1_456 ? O3 Ho1 C3 76.7(2) . 1_456 ? O1 Ho1 C3 174.6(2) . 1_456 ? O5 Ho1 C3 27.8(2) 1_456 1_456 ? O6 Ho1 C3 27.1(2) 1_456 1_456 ? N1 Ag1 O8 131.6(2) . . ? N1 Ag1 O1 124.0(2) . . ? O8 Ag1 O1 104.40(19) . . ? N5 Ag2 N2 156.6(3) . . ? N5 Ag2 O10 27.7(4) . 2_556 ? N2 Ag2 O10 175.1(4) . 2_556 ? N5 Ag2 O9 25.0(5) . 2_556 ? N2 Ag2 O9 131.7(4) . 2_556 ? O10 Ag2 O9 52.7(4) 2_556 2_556 ? O2 C1 O1 126.7(7) . . ? O2 C1 C1 116.5(8) . 2_775 ? O1 C1 C1 116.6(8) . 2_775 ? O3 C2 O4 127.5(7) . . ? O3 C2 C2 117.3(9) . 2_675 ? O4 C2 C2 115.2(9) . 2_675 ? O6 C3 O5 123.2(7) . . ? O6 C3 C4 119.3(7) . . ? O5 C3 C4 117.4(7) . . ? O6 C3 Ho1 62.3(4) . 1_654 ? O5 C3 Ho1 61.0(4) . 1_654 ? C4 C3 Ho1 178.0(6) . 1_654 ? C5 C4 C8 117.4(8) . . ? C5 C4 C3 120.9(8) . . ? C8 C4 C3 121.6(8) . . ? C4 C5 C6 121.2(8) . . ? C4 C5 H5 119.4 . . ? C6 C5 H5 119.4 . . ? C5 C6 N1 120.5(8) . . ? C5 C6 H6 119.7 . . ? N1 C6 H6 119.7 . . ? N1 C7 C8 122.6(9) . . ? N1 C7 H7 118.7 . . ? C8 C7 H7 118.7 . . ? C4 C8 C7 119.4(9) . . ? C4 C8 H8 120.3 . . ? C7 C8 H8 120.3 . . ? O8 C9 O7 124.9(7) . . ? O8 C9 C10 118.2(8) . . ? O7 C9 C10 116.9(7) . . ? C11 C10 C14 117.0(7) . . ? C11 C10 C9 121.3(8) . . ? C14 C10 C9 121.7(7) . . ? C12 C11 C10 120.3(8) . . ? C12 C11 H11 119.9 . . ? C10 C11 H11 119.9 . . ? N2 C12 C11 122.5(8) . . ? N2 C12 H12 118.7 . . ? C11 C12 H12 118.7 . . ? N2 C13 C14 123.3(8) . . ? N2 C13 H13 118.4 . . ? C14 C13 H13 118.4 . . ? C13 C14 C10 119.6(8) . . ? C13 C14 H14 120.2 . . ? C10 C14 H14 120.2 . . ? C7 N1 C6 118.6(7) . . ? C7 N1 Ag1 122.5(6) . . ? C6 N1 Ag1 118.8(5) . . ? C13 N2 C12 117.2(7) . . ? C13 N2 Ag2 121.7(6) . . ? C12 N2 Ag2 121.1(6) . . ? C1 O1 Ho1 119.1(5) . . ? C1 O1 Ag1 121.6(5) . . ? Ho1 O1 Ag1 119.2(2) . . ? C1 O2 Ho1 119.2(5) . 2_775 ? C2 O3 Ho1 119.5(5) . . ? C2 O4 Ho1 119.7(5) . 2_675 ? C3 O5 Ho1 91.2(5) . 1_654 ? C3 O6 Ho1 90.6(5) . 1_654 ? C9 O7 Ho1 149.8(6) . . ? C9 O8 Ag1 119.5(5) . . ? N3 O11 Ho1 120.8(11) . . ? N3 O11 H11A 92.8 . . ? Ho1 O11 H11A 130.6 . . ? N3 O11 H11B 13.2 . . ? Ho1 O11 H11B 116.2 . . ? H11A O11 H11B 103.5 . . ? O13 N3 O11 126(2) . . ? O13 N3 O12 119(2) . . ? O11 N3 O12 115(2) . . ? O13 N3 H11B 125.7 . . ? O11 N3 H11B 27.5 . . ? O12 N3 H11B 111.6 . . ? N3 O13 H15B 106.0 . . ? H14A O14 H14B 106.8 . . ? H15A O15 H15B 106.9 . . ? H16A O16 H16B 107(3) . . ? H16A O16 H16C 115(8) . . ? H16B O16 H16C 104(3) . . ? C15 N5 C19 120.0 . . ? C15 N5 Ag2 118.9(5) . . ? C19 N5 Ag2 121.1(5) . . ? N5 C15 C16 120.0 . . ? N5 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C15 C16 C17 120.0 . . ? C15 C16 H16 120.0 . . ? C17 C16 H16 120.0 . . ? C18 C17 C16 120.0 . . ? C18 C17 C20 122.7(12) . . ? C16 C17 C20 117.3(12) . . ? C19 C18 C17 120.0 . . ? C19 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? C18 C19 N5 120.0 . . ? C18 C19 H19 120.0 . . ? N5 C19 H19 120.0 . . ? O9 C20 O10 126.9(19) . . ? O9 C20 C17 118.7(19) . . ? O10 C20 C17 114.3(19) . . ? C20 O9 Ag2 89.9(13) . 2_556 ? C20 O10 Ag2 90.5(12) . 2_556 ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.20 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.237 _refine_diff_density_min -1.092 _refine_diff_density_rms 0.173 #################################################################### data_7 #TrackingRef '- Cifs.txt' _database_code_depnum_ccdc_archive 'CCDC 725532' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H8 Ag N2 O8 La, H2 O' _chemical_formula_sum 'C14 H10 Ag La N2 O9' _chemical_formula_weight 597.02 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 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 21.6736(11) _cell_length_b 9.4185(5) _cell_length_c 17.5251(9) _cell_angle_alpha 90.00 _cell_angle_beta 109.3790(10) _cell_angle_gamma 90.00 _cell_volume 3374.8(3) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2928 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 27.02 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.350 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2272 _exptl_absorpt_coefficient_mu 3.712 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5095 _exptl_absorpt_correction_T_max 0.5547 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8470 _diffrn_reflns_av_R_equivalents 0.0294 _diffrn_reflns_av_sigmaI/netI 0.0347 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 25.20 _reflns_number_total 3037 _reflns_number_gt 2571 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0229P)^2^+7.1392P] 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 3037 _refine_ls_number_parameters 244 _refine_ls_number_restraints 192 _refine_ls_R_factor_all 0.0352 _refine_ls_R_factor_gt 0.0266 _refine_ls_wR_factor_ref 0.0581 _refine_ls_wR_factor_gt 0.0544 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.470 _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 La1 La 0.986054(17) 0.31571(4) 0.426334(19) 0.02136(12) Uani 1 1 d U . . Ag1 Ag 0.82607(3) 0.06855(8) 0.85733(4) 0.0630(2) Uani 1 1 d U . . O1 O 0.9620(2) 0.2797(5) 0.5565(3) 0.0369(11) Uani 1 1 d U . . O2 O 0.9821(2) 0.4730(5) 0.6345(3) 0.0339(11) Uani 1 1 d U . . O7 O 0.9289(2) 0.2683(4) 0.2750(2) 0.0287(10) Uani 1 1 d U . . O5 O 0.9359(2) 0.0716(4) 0.4202(2) 0.0313(10) Uani 1 1 d U . . N1 N 0.8603(3) 0.1636(6) 0.7654(3) 0.0414(15) Uani 1 1 d U . . C1 C 0.9593(3) 0.3504(7) 0.6152(4) 0.0269(14) Uani 1 1 d U . . C2 C 0.9243(3) 0.2846(6) 0.6679(3) 0.0255(14) Uani 1 1 d U . . C6 C 0.9179(4) 0.1390(7) 0.6720(4) 0.0426(18) Uani 1 1 d U . . H6 H 0.9349 0.0792 0.6416 0.051 Uiso 1 1 calc R . . C5 C 0.8863(4) 0.0841(8) 0.7215(5) 0.054(2) Uani 1 1 d U . . H5 H 0.8829 -0.0141 0.7243 0.065 Uiso 1 1 calc R . . C3 C 0.8970(3) 0.3680(7) 0.7122(4) 0.0367(17) Uani 1 1 d U . . H3 H 0.8999 0.4664 0.7106 0.044 Uiso 1 1 calc R . . C4 C 0.8650(4) 0.3036(8) 0.7596(4) 0.0427(18) Uani 1 1 d U . . H4 H 0.8459 0.3611 0.7886 0.051 Uiso 1 1 calc R . . C14 C 0.9626(3) 0.2517(6) 0.2295(4) 0.0247(13) Uani 1 1 d U . . C13 C 0.9638(3) -0.0155(6) 0.4749(4) 0.0251(14) Uani 1 1 d U . . N2 N 0.7680(3) 0.0469(7) 0.9364(3) 0.0434(15) Uani 1 1 d U . . C7 C 0.7164(3) 0.1320(8) 0.9254(4) 0.047(2) Uani 1 1 d U . . H7 H 0.7092 0.2037 0.8870 0.057 Uiso 1 1 calc R . . C12 C 0.7775(4) -0.0502(9) 0.9934(5) 0.061(2) Uani 1 1 d U . . H12 H 0.8146 -0.1069 1.0049 0.074 Uiso 1 1 calc R . . C8 C 0.6733(3) 0.1195(8) 0.9678(4) 0.0429(18) Uani 1 1 d U . . H8 H 0.6392 0.1837 0.9596 0.051 Uiso 1 1 calc R . . C11 C 0.7359(4) -0.0726(9) 1.0368(5) 0.058(2) Uani 1 1 d U . . H11 H 0.7446 -0.1439 1.0756 0.070 Uiso 1 1 calc R . . C9 C 0.6816(3) 0.0110(7) 1.0222(4) 0.0285(14) Uani 1 1 d U . . O8 O 0.9417(2) 0.2309(5) 0.1550(2) 0.0317(10) Uani 1 1 d U . . O6 O 0.9387(2) -0.1246(4) 0.4923(3) 0.0309(10) Uani 1 1 d U . . C10 C 0.6291(3) -0.0224(7) 1.0588(4) 0.0269(14) Uani 1 1 d U . . O4 O 0.6373(2) -0.1221(5) 1.1074(3) 0.0368(11) Uani 1 1 d U . . O3 O 0.5758(2) 0.0470(4) 1.0341(2) 0.0294(10) Uani 1 1 d U . . O1W O 0.7962(3) 0.1933(7) 0.2574(4) 0.0768(19) Uani 1 1 d U . . H1W H 0.7949 0.2412 0.2422 0.115 Uiso 1 1 d R . . H2W H 0.7762 0.2241 0.2663 0.115 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 La1 0.0296(2) 0.01918(19) 0.02176(19) -0.00020(15) 0.01718(15) -0.00138(15) Ag1 0.0458(4) 0.1008(6) 0.0566(4) 0.0364(4) 0.0359(3) 0.0078(3) O1 0.060(3) 0.031(3) 0.033(3) 0.001(2) 0.033(2) -0.002(2) O2 0.047(3) 0.029(3) 0.033(2) 0.001(2) 0.023(2) -0.009(2) O7 0.0293(14) 0.0316(15) 0.0282(14) -0.0006(12) 0.0137(12) 0.0000(11) O5 0.039(3) 0.024(2) 0.028(2) 0.0041(19) 0.007(2) -0.005(2) N1 0.048(4) 0.046(4) 0.042(3) 0.014(3) 0.030(3) 0.006(3) C1 0.035(4) 0.027(4) 0.025(3) 0.007(3) 0.018(3) 0.004(3) C2 0.030(3) 0.027(4) 0.022(3) 0.002(3) 0.012(3) -0.005(3) C6 0.058(5) 0.028(4) 0.062(5) 0.005(3) 0.047(4) 0.008(3) C5 0.070(5) 0.037(4) 0.076(5) 0.017(4) 0.051(4) 0.005(4) C3 0.051(4) 0.029(4) 0.041(4) -0.006(3) 0.029(3) -0.008(3) C4 0.053(4) 0.045(4) 0.043(4) -0.010(3) 0.033(4) -0.010(4) C14 0.036(3) 0.018(3) 0.026(3) 0.001(3) 0.018(3) 0.000(3) C13 0.032(3) 0.023(3) 0.027(3) -0.003(3) 0.017(3) -0.002(3) N2 0.037(3) 0.061(4) 0.042(3) 0.016(3) 0.026(3) 0.005(3) C7 0.036(4) 0.060(5) 0.050(4) 0.027(4) 0.020(4) 0.000(4) C12 0.056(5) 0.073(6) 0.072(5) 0.036(5) 0.045(4) 0.030(4) C8 0.028(4) 0.046(4) 0.058(5) 0.019(4) 0.020(3) 0.005(3) C11 0.052(5) 0.072(6) 0.062(5) 0.039(4) 0.036(4) 0.027(4) C9 0.026(3) 0.034(4) 0.027(3) 0.006(3) 0.011(3) 0.001(3) O8 0.037(3) 0.040(3) 0.022(2) 0.0001(19) 0.015(2) -0.004(2) O6 0.031(2) 0.026(2) 0.038(3) 0.008(2) 0.014(2) -0.0021(19) C10 0.028(3) 0.033(4) 0.023(3) -0.006(3) 0.013(3) -0.005(3) O4 0.037(3) 0.043(3) 0.037(3) 0.016(2) 0.020(2) 0.002(2) O3 0.029(2) 0.031(3) 0.031(2) -0.0015(19) 0.014(2) 0.000(2) O1W 0.059(4) 0.085(5) 0.089(5) -0.014(4) 0.028(4) -0.002(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 La1 O2 2.463(4) 5_766 ? La1 O1 2.526(4) . ? La1 O6 2.528(4) 5_756 ? La1 O5 2.530(4) . ? La1 O3 2.566(4) 8 ? La1 O7 2.566(4) . ? La1 O8 2.569(4) 2_755 ? La1 O4 2.606(4) 4_656 ? La1 O3 2.765(4) 4_656 ? La1 C10 3.008(6) 4_656 ? Ag1 N2 2.169(5) . ? Ag1 N1 2.176(5) . ? O1 C1 1.243(7) . ? O2 C1 1.258(7) . ? O2 La1 2.463(4) 5_766 ? O7 C14 1.257(7) . ? O5 C13 1.254(7) . ? N1 C5 1.327(9) . ? N1 C4 1.329(9) . ? C1 C2 1.510(8) . ? C2 C3 1.369(8) . ? C2 C6 1.382(9) . ? C6 C5 1.373(9) . ? C6 H6 0.9300 . ? C5 H5 0.9300 . ? C3 C4 1.385(9) . ? C3 H3 0.9300 . ? C4 H4 0.9300 . ? C14 O8 1.247(7) . ? C14 C14 1.540(12) 2_755 ? C13 O6 1.247(7) . ? C13 C13 1.550(12) 5_756 ? N2 C12 1.318(9) . ? N2 C7 1.337(9) . ? C7 C8 1.378(9) . ? C7 H7 0.9300 . ? C12 C11 1.376(9) . ? C12 H12 0.9300 . ? C8 C9 1.368(9) . ? C8 H8 0.9300 . ? C11 C9 1.367(9) . ? C11 H11 0.9300 . ? C9 C10 1.515(8) . ? O8 La1 2.569(4) 2_755 ? O6 La1 2.528(4) 5_756 ? C10 O4 1.241(7) . ? C10 O3 1.270(7) . ? C10 La1 3.008(6) 4_646 ? O4 La1 2.606(4) 4_646 ? O3 La1 2.566(4) 8_456 ? O3 La1 2.765(4) 4_646 ? O1W H1W 0.5197 . ? O1W H2W 0.5835 . ? 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 La1 O1 132.18(14) 5_766 . ? O2 La1 O6 126.78(14) 5_766 5_756 ? O1 La1 O6 71.48(14) . 5_756 ? O2 La1 O5 153.42(14) 5_766 . ? O1 La1 O5 72.64(14) . . ? O6 La1 O5 64.18(13) 5_756 . ? O2 La1 O3 70.03(13) 5_766 8 ? O1 La1 O3 74.72(14) . 8 ? O6 La1 O3 75.75(14) 5_756 8 ? O5 La1 O3 134.36(13) . 8 ? O2 La1 O7 78.56(14) 5_766 . ? O1 La1 O7 137.41(14) . . ? O6 La1 O7 117.34(14) 5_756 . ? O5 La1 O7 75.22(13) . . ? O3 La1 O7 146.74(13) 8 . ? O2 La1 O8 72.58(14) 5_766 2_755 ? O1 La1 O8 143.68(14) . 2_755 ? O6 La1 O8 72.20(13) 5_756 2_755 ? O5 La1 O8 91.51(14) . 2_755 ? O3 La1 O8 96.43(13) 8 2_755 ? O7 La1 O8 63.05(13) . 2_755 ? O2 La1 O4 97.71(15) 5_766 4_656 ? O1 La1 O4 74.44(14) . 4_656 ? O6 La1 O4 135.17(14) 5_756 4_656 ? O5 La1 O4 78.50(14) . 4_656 ? O3 La1 O4 121.62(13) 8 4_656 ? O7 La1 O4 72.37(13) . 4_656 ? O8 La1 O4 135.39(13) 2_755 4_656 ? O2 La1 O3 72.61(13) 5_766 4_656 ? O1 La1 O3 67.45(13) . 4_656 ? O6 La1 O3 134.04(13) 5_756 4_656 ? O5 La1 O3 119.30(13) . 4_656 ? O3 La1 O3 74.38(14) 8 4_656 ? O7 La1 O3 106.76(12) . 4_656 ? O8 La1 O3 145.06(13) 2_755 4_656 ? O4 La1 O3 48.20(13) 4_656 4_656 ? O2 La1 C10 89.29(16) 5_766 4_656 ? O1 La1 C10 64.18(15) . 4_656 ? O6 La1 C10 135.27(14) 5_756 4_656 ? O5 La1 C10 96.17(16) . 4_656 ? O3 La1 C10 97.41(16) 8 4_656 ? O7 La1 C10 92.73(15) . 4_656 ? O8 La1 C10 151.76(15) 2_755 4_656 ? O4 La1 C10 24.20(15) 4_656 4_656 ? O3 La1 C10 24.97(15) 4_656 4_656 ? N2 Ag1 N1 157.5(2) . . ? C1 O1 La1 139.1(4) . . ? C1 O2 La1 140.0(4) . 5_766 ? C14 O7 La1 119.6(4) . . ? C13 O5 La1 118.1(4) . . ? C5 N1 C4 117.1(6) . . ? C5 N1 Ag1 120.8(5) . . ? C4 N1 Ag1 121.3(5) . . ? O1 C1 O2 126.4(5) . . ? O1 C1 C2 117.3(6) . . ? O2 C1 C2 116.3(5) . . ? C3 C2 C6 118.1(6) . . ? C3 C2 C1 120.7(6) . . ? C6 C2 C1 121.1(5) . . ? C5 C6 C2 119.0(6) . . ? C5 C6 H6 120.5 . . ? C2 C6 H6 120.5 . . ? N1 C5 C6 123.5(7) . . ? N1 C5 H5 118.3 . . ? C6 C5 H5 118.3 . . ? C2 C3 C4 119.0(6) . . ? C2 C3 H3 120.5 . . ? C4 C3 H3 120.5 . . ? N1 C4 C3 123.3(6) . . ? N1 C4 H4 118.4 . . ? C3 C4 H4 118.4 . . ? O8 C14 O7 126.7(6) . . ? O8 C14 C14 116.6(6) . 2_755 ? O7 C14 C14 116.6(6) . 2_755 ? O6 C13 O5 125.9(6) . . ? O6 C13 C13 117.3(7) . 5_756 ? O5 C13 C13 116.8(7) . 5_756 ? C12 N2 C7 116.0(6) . . ? C12 N2 Ag1 124.8(5) . . ? C7 N2 Ag1 119.1(4) . . ? N2 C7 C8 123.7(6) . . ? N2 C7 H7 118.1 . . ? C8 C7 H7 118.1 . . ? N2 C12 C11 124.0(7) . . ? N2 C12 H12 118.0 . . ? C11 C12 H12 118.0 . . ? C9 C8 C7 118.9(7) . . ? C9 C8 H8 120.5 . . ? C7 C8 H8 120.5 . . ? C9 C11 C12 119.3(7) . . ? C9 C11 H11 120.4 . . ? C12 C11 H11 120.4 . . ? C11 C9 C8 117.8(6) . . ? C11 C9 C10 121.5(6) . . ? C8 C9 C10 120.4(6) . . ? C14 O8 La1 117.1(4) . 2_755 ? C13 O6 La1 118.2(4) . 5_756 ? O4 C10 O3 122.1(5) . . ? O4 C10 C9 119.4(6) . . ? O3 C10 C9 118.3(5) . . ? O4 C10 La1 59.4(3) . 4_646 ? O3 C10 La1 66.7(3) . 4_646 ? C9 C10 La1 154.7(4) . 4_646 ? C10 O4 La1 96.4(4) . 4_646 ? C10 O3 La1 153.0(4) . 8_456 ? C10 O3 La1 88.3(4) . 4_646 ? La1 O3 La1 105.62(14) 8_456 4_646 ? H1W O1W H2W 77.6 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.20 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.225 _refine_diff_density_min -0.858 _refine_diff_density_rms 0.103 ###################################################################### data_5 #TrackingRef '- Cifs.txt' _database_code_depnum_ccdc_archive 'CCDC 727504' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H24 Ag4 Dy2 N6 O23, 2(H O0.50), 2(H2 O)' _chemical_formula_sum 'C34 H30 Ag4 Dy2 N6 O26' _chemical_formula_weight 1695.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 '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 '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.7942(15) _cell_length_b 11.6555(19) _cell_length_c 11.946(2) _cell_angle_alpha 77.532(2) _cell_angle_beta 76.519(2) _cell_angle_gamma 76.058(2) _cell_volume 1139.0(3) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2699 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 27.71 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.471 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 804 _exptl_absorpt_coefficient_mu 5.023 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3141 _exptl_absorpt_correction_T_max 0.4185 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II area-detector diffractometer' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5895 _diffrn_reflns_av_R_equivalents 0.0289 _diffrn_reflns_av_sigmaI/netI 0.0570 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 25.20 _reflns_number_total 4036 _reflns_number_gt 3602 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0472P)^2^+15.9189P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4036 _refine_ls_number_parameters 386 _refine_ls_number_restraints 100 _refine_ls_R_factor_all 0.0626 _refine_ls_R_factor_gt 0.0563 _refine_ls_wR_factor_ref 0.1366 _refine_ls_wR_factor_gt 0.1334 _refine_ls_goodness_of_fit_ref 1.146 _refine_ls_restrained_S_all 1.132 _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 Dy1 Dy 0.75670(5) 0.84245(4) 1.13785(4) 0.02134(12) Uani 1 1 d . . 4 Ag1 Ag 1.02859(10) 0.73647(9) 0.83265(7) 0.0451(2) Uani 1 1 d . . 4 Ag2 Ag 0.34758(10) 0.20814(8) 1.22683(8) 0.0431(2) Uani 1 1 d . . 4 C1 C 1.0246(11) 0.9619(9) 0.9517(8) 0.025(2) Uani 1 1 d . . 4 C2 C 0.4808(11) 1.0446(8) 1.0421(8) 0.024(2) Uani 1 1 d . . 4 C3 C 1.5422(11) 0.8105(9) 0.3476(8) 0.025(2) Uani 1 1 d . . 4 C4 C 1.4275(11) 0.7891(10) 0.4618(8) 0.030(2) Uani 1 1 d . . 4 C5 C 1.4153(12) 0.8515(9) 0.5485(8) 0.030(2) Uani 1 1 d . . 4 H5 H 1.4836 0.9039 0.5399 0.036 Uiso 1 1 calc R . 4 C6 C 1.3019(12) 0.8373(9) 0.6491(8) 0.030(2) Uani 1 1 d . . 4 H6 H 1.2896 0.8850 0.7051 0.037 Uiso 1 1 calc R . 4 C7 C 1.2256(14) 0.6930(11) 0.5860(9) 0.042(3) Uani 1 1 d . . 4 H7 H 1.1618 0.6366 0.5988 0.050 Uiso 1 1 calc R . 4 C8 C 1.3322(13) 0.7044(10) 0.4813(9) 0.035(2) Uani 1 1 d . . 4 H8 H 1.3402 0.6573 0.4258 0.042 Uiso 1 1 calc R . 4 C9 C 0.8093(10) 0.5920(9) 1.0187(9) 0.029(2) Uani 1 1 d . . 4 C10 C 0.7075(11) 0.5007(9) 1.0675(9) 0.029(2) Uani 1 1 d . . 4 C11 C 0.5932(13) 0.5113(10) 1.1692(10) 0.039(3) Uani 1 1 d . . 4 H11 H 0.5832 0.5732 1.2098 0.047 Uiso 1 1 calc R . 4 C12 C 0.4940(12) 0.4286(10) 1.2097(10) 0.039(3) Uani 1 1 d . . 4 H12 H 0.4143 0.4390 1.2753 0.046 Uiso 1 1 calc R . 4 C13 C 0.6208(13) 0.3237(10) 1.0621(9) 0.037(3) Uani 1 1 d . . 4 H13 H 0.6298 0.2600 1.0239 0.044 Uiso 1 1 calc R . 4 C14 C 0.7229(12) 0.4007(9) 1.0169(9) 0.033(2) Uani 1 1 d . . 4 H14 H 0.8028 0.3864 0.9523 0.039 Uiso 1 1 calc R . 4 N1 N 1.2076(10) 0.7554(8) 0.6686(7) 0.033(2) Uani 1 1 d . . 4 N2 N 0.5091(10) 0.3347(8) 1.1577(7) 0.031(2) Uani 1 1 d . . 4 O1 O 0.9576(8) 0.8744(6) 0.9672(6) 0.0275(15) Uani 1 1 d . . 4 O2 O 1.1226(7) 0.9940(6) 0.8633(5) 0.0275(15) Uani 1 1 d . . 4 O3 O 0.5554(8) 1.0204(6) 1.1236(6) 0.0283(15) Uani 1 1 d . A 4 O4 O 0.3761(8) 1.1372(6) 1.0204(6) 0.0284(15) Uani 1 1 d . . 4 O5 O 1.5285(8) 0.7691(6) 0.2602(6) 0.0307(16) Uani 1 1 d D . 4 O6 O 1.6461(8) 0.8708(7) 0.3389(6) 0.0368(18) Uani 1 1 d D . 4 O7 O 0.8191(8) 0.6597(6) 1.0840(6) 0.0323(17) Uani 1 1 d D . 4 O8 O 0.8777(9) 0.5979(7) 0.9137(6) 0.0393(19) Uani 1 1 d D . 4 O11 O 0.9886(10) 0.7540(9) 1.2173(8) 0.055(2) Uani 1 1 d U B 4 H11A H 1.0333 0.7790 1.2591 0.082 Uiso 0.50 1 d PR B 2 H11B H 0.9998 0.6756 1.2453 0.082 Uiso 0.50 1 d PR B 2 N3 N 0.994(3) 0.652(3) 1.279(2) 0.066(7) Uani 0.50 1 d PU C 1 O12 O 0.861(3) 0.622(3) 1.312(2) 0.095(8) Uani 0.50 1 d PU C 1 O13 O 1.113(3) 0.590(3) 1.318(3) 0.127(12) Uani 0.50 1 d P C 1 O14 O 0.212(2) 0.3835(17) 0.4553(16) 0.059(5) Uani 0.50 1 d P D 1 H14A H 0.1282 0.3615 0.4557 0.088 Uiso 0.50 1 d PR D 1 H14B H 0.1899 0.4267 0.5070 0.088 Uiso 0.50 1 d PR D 1 O15 O 1.042(3) 0.5157(19) 1.2913(17) 0.070(6) Uani 0.50 1 d P E 2 H15A H 1.0243 0.4941 1.2338 0.105 Uiso 0.50 1 d PR E 2 H15B H 1.1305 0.4752 1.3040 0.105 Uiso 0.50 1 d PR E 2 O16 O 0.7484(13) 0.1448(10) 0.8427(11) 0.088(4) Uani 1 1 d D . . H16A H 0.820(4) 0.185(4) 0.831(8) 0.132 Uiso 0.50 1 d PD . . H16B H 0.687(6) 0.180(5) 0.797(5) 0.132 Uiso 1 1 d D . . H16C H 0.716(9) 0.083(6) 0.880(9) 0.132 Uiso 0.50 1 d PD . . N5 N 0.1885(14) 0.1148(10) 1.3536(9) 0.031(4) Uani 0.50 1 d PGU F -1 C15 C 0.1314(16) 0.0268(12) 1.3231(9) 0.038(5) Uani 0.50 1 d PGU F -1 H15 H 0.1632 0.0096 1.2476 0.045 Uiso 0.50 1 calc PR F -1 C16 C 0.0269(18) -0.0355(12) 1.4054(13) 0.035(4) Uani 0.50 1 d PGU F -1 H16 H -0.0113 -0.0944 1.3850 0.043 Uiso 0.50 1 calc PR F -1 C17 C -0.0206(17) -0.0098(14) 1.5182(11) 0.031(3) Uani 0.50 1 d PGU F -1 C18 C 0.0365(18) 0.0782(14) 1.5487(9) 0.036(4) Uani 0.50 1 d PGU F -1 H18 H 0.0047 0.0954 1.6242 0.043 Uiso 0.50 1 calc PR F -1 C19 C 0.1410(16) 0.1405(11) 1.4664(11) 0.036(5) Uani 0.50 1 d PGU F -1 H19 H 0.1792 0.1994 1.4868 0.043 Uiso 0.50 1 calc PR F -1 C20 C -0.138(3) -0.084(2) 1.605(2) 0.046(5) Uani 0.50 1 d PU F -1 O9 O -0.182(3) -0.161(2) 1.5754(18) 0.092(7) Uani 0.50 1 d PDU F -1 O10 O -0.173(2) -0.0589(17) 1.7075(15) 0.057(5) Uani 0.50 1 d PDU F -1 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 Dy1 0.0180(2) 0.0271(2) 0.0194(2) -0.00854(18) 0.00133(15) -0.00596(17) Ag1 0.0427(5) 0.0599(6) 0.0303(4) -0.0144(4) 0.0153(4) -0.0214(4) Ag2 0.0440(5) 0.0482(5) 0.0382(5) -0.0127(4) 0.0124(4) -0.0257(4) C1 0.023(4) 0.029(5) 0.021(4) -0.011(4) -0.003(4) 0.001(4) C2 0.024(4) 0.019(5) 0.026(5) -0.005(4) 0.003(4) -0.008(4) C3 0.028(5) 0.022(5) 0.021(5) 0.001(4) -0.003(4) -0.004(4) C4 0.017(4) 0.040(6) 0.027(5) -0.006(5) 0.002(4) -0.003(4) C5 0.035(5) 0.028(5) 0.028(5) -0.009(4) 0.003(4) -0.010(4) C6 0.039(5) 0.027(5) 0.023(5) -0.006(4) -0.001(4) -0.005(5) C7 0.047(6) 0.047(7) 0.034(6) -0.019(5) 0.012(5) -0.023(5) C8 0.043(6) 0.033(6) 0.033(5) -0.013(5) 0.001(5) -0.017(5) C9 0.017(4) 0.027(5) 0.039(6) -0.002(5) -0.009(4) 0.002(4) C10 0.023(4) 0.033(6) 0.031(5) -0.002(4) -0.004(4) -0.007(4) C11 0.045(6) 0.031(6) 0.042(6) -0.017(5) 0.005(5) -0.013(5) C12 0.030(5) 0.043(6) 0.041(6) -0.026(5) 0.012(4) -0.007(5) C13 0.043(6) 0.038(6) 0.031(5) -0.007(5) -0.001(5) -0.016(5) C14 0.033(5) 0.030(5) 0.033(5) -0.013(5) 0.004(4) -0.006(4) N1 0.030(4) 0.044(5) 0.025(4) -0.012(4) 0.008(3) -0.015(4) N2 0.032(4) 0.026(4) 0.033(5) -0.005(4) -0.003(4) -0.009(4) O1 0.029(3) 0.027(4) 0.028(3) -0.014(3) 0.007(3) -0.012(3) O2 0.027(3) 0.035(4) 0.024(3) -0.015(3) 0.008(3) -0.016(3) O3 0.031(3) 0.030(4) 0.026(3) -0.011(3) -0.008(3) -0.001(3) O4 0.029(3) 0.029(4) 0.028(3) -0.009(3) -0.007(3) -0.001(3) O5 0.033(3) 0.037(4) 0.026(3) -0.013(3) 0.003(3) -0.016(3) O6 0.032(4) 0.063(5) 0.022(3) -0.016(3) 0.002(3) -0.022(4) O7 0.029(3) 0.018(3) 0.052(4) -0.011(3) -0.006(3) -0.005(3) O8 0.041(4) 0.036(4) 0.041(4) -0.009(4) 0.000(3) -0.014(4) O11 0.057(5) 0.055(6) 0.060(5) -0.008(5) -0.040(4) -0.001(4) N3 0.052(13) 0.086(19) 0.061(15) -0.020(14) -0.007(11) -0.011(13) O12 0.077(14) 0.14(2) 0.086(16) -0.035(15) -0.002(12) -0.057(15) O13 0.086(16) 0.16(3) 0.12(2) 0.04(2) -0.069(16) -0.003(19) O14 0.064(11) 0.050(11) 0.055(11) 0.008(9) -0.014(9) -0.010(9) O15 0.092(15) 0.060(13) 0.055(12) 0.000(10) -0.028(11) -0.003(12) O16 0.081(7) 0.071(7) 0.123(10) 0.011(7) -0.055(7) -0.027(6) N5 0.038(9) 0.024(8) 0.031(7) 0.007(7) 0.000(7) -0.020(7) C15 0.044(11) 0.028(10) 0.042(9) -0.009(8) 0.003(8) -0.015(8) C16 0.035(9) 0.035(10) 0.043(8) -0.011(7) -0.003(7) -0.021(8) C17 0.023(8) 0.027(8) 0.038(7) -0.007(7) -0.001(6) -0.002(6) C18 0.027(9) 0.050(10) 0.031(8) -0.015(7) 0.009(7) -0.015(7) C19 0.050(11) 0.035(10) 0.025(8) 0.008(8) -0.010(8) -0.022(8) C20 0.030(10) 0.046(11) 0.052(9) 0.016(9) -0.005(8) -0.013(8) O9 0.101(15) 0.118(16) 0.076(14) 0.002(12) -0.008(13) -0.083(13) O10 0.056(11) 0.047(11) 0.051(8) 0.016(8) 0.009(8) -0.018(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 Dy1 O7 2.261(6) . ? Dy1 O11 2.364(8) . ? Dy1 O3 2.384(6) . ? Dy1 O4 2.387(7) 2_677 ? Dy1 O2 2.391(7) 2_777 ? Dy1 O1 2.393(6) . ? Dy1 O5 2.411(6) 1_456 ? Dy1 O6 2.433(6) 1_456 ? Dy1 C3 2.776(9) 1_456 ? Ag1 N1 2.215(8) . ? Ag1 O8 2.251(8) . ? Ag1 O1 2.392(6) . ? Ag2 N2 2.193(9) . ? C1 O2 1.249(11) . ? C1 O1 1.257(12) . ? C1 C1 1.527(18) 2_777 ? C2 O3 1.245(12) . ? C2 O4 1.262(11) . ? C2 C2 1.525(18) 2_677 ? C3 O6 1.254(12) . ? C3 O5 1.282(12) . ? C3 C4 1.508(13) . ? C3 Dy1 2.776(9) 1_654 ? C4 C5 1.361(14) . ? C4 C8 1.392(15) . ? C5 C6 1.379(13) . ? C5 H5 0.9300 . ? C6 N1 1.361(14) . ? C6 H6 0.9300 . ? C7 N1 1.307(14) . ? C7 C8 1.379(15) . ? C7 H7 0.9300 . ? C8 H8 0.9300 . ? C9 O8 1.253(12) . ? C9 O7 1.253(13) . ? C9 C10 1.490(14) . ? C10 C14 1.390(15) . ? C10 C11 1.392(14) . ? C11 C12 1.389(16) . ? C11 H11 0.9300 . ? C12 N2 1.337(14) . ? C12 H12 0.9300 . ? C13 N2 1.329(13) . ? C13 C14 1.362(15) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? O2 Dy1 2.391(7) 2_777 ? O4 Dy1 2.387(7) 2_677 ? O5 Dy1 2.411(6) 1_654 ? O6 Dy1 2.433(6) 1_654 ? O11 H11A 0.8349 . ? O11 H11B 0.8924 . ? N3 O12 1.24(3) . ? N3 O13 1.25(3) . ? N3 H11B 0.4391 . ? O14 H14A 0.8336 . ? O14 H14B 0.8396 . ? O15 H15A 0.8373 . ? O15 H15B 0.8377 . ? O16 H16A 0.84(2) . ? O16 H16B 0.84(2) . ? O16 H16C 0.84(2) . ? N5 C15 1.3900 . ? N5 C19 1.3900 . ? C15 C16 1.3900 . ? C15 H15 0.9300 . ? C16 C17 1.3900 . ? C16 H16 0.9300 . ? C17 C18 1.3900 . ? C17 C20 1.56(3) . ? C18 C19 1.3900 . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 O9 1.20(3) . ? C20 O10 1.28(3) . ? 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 O7 Dy1 O11 78.7(3) . . ? O7 Dy1 O3 138.9(2) . . ? O11 Dy1 O3 142.3(3) . . ? O7 Dy1 O4 74.2(2) . 2_677 ? O11 Dy1 O4 146.4(3) . 2_677 ? O3 Dy1 O4 67.6(2) . 2_677 ? O7 Dy1 O2 140.6(2) . 2_777 ? O11 Dy1 O2 74.8(3) . 2_777 ? O3 Dy1 O2 72.8(2) . 2_777 ? O4 Dy1 O2 115.8(2) 2_677 2_777 ? O7 Dy1 O1 79.5(2) . . ? O11 Dy1 O1 80.0(3) . . ? O3 Dy1 O1 104.6(2) . . ? O4 Dy1 O1 75.9(2) 2_677 . ? O2 Dy1 O1 67.7(2) 2_777 . ? O7 Dy1 O5 83.3(2) . 1_456 ? O11 Dy1 O5 110.5(3) . 1_456 ? O3 Dy1 O5 79.4(2) . 1_456 ? O4 Dy1 O5 85.9(2) 2_677 1_456 ? O2 Dy1 O5 133.2(2) 2_777 1_456 ? O1 Dy1 O5 157.7(2) . 1_456 ? O7 Dy1 O6 122.3(3) . 1_456 ? O11 Dy1 O6 81.8(3) . 1_456 ? O3 Dy1 O6 75.2(2) . 1_456 ? O4 Dy1 O6 129.7(2) 2_677 1_456 ? O2 Dy1 O6 82.2(2) 2_777 1_456 ? O1 Dy1 O6 148.0(2) . 1_456 ? O5 Dy1 O6 54.3(2) 1_456 1_456 ? O7 Dy1 C3 103.2(3) . 1_456 ? O11 Dy1 C3 95.8(3) . 1_456 ? O3 Dy1 C3 76.6(2) . 1_456 ? O4 Dy1 C3 109.4(3) 2_677 1_456 ? O2 Dy1 C3 108.0(3) 2_777 1_456 ? O1 Dy1 C3 174.6(3) . 1_456 ? O5 Dy1 C3 27.5(3) 1_456 1_456 ? O6 Dy1 C3 26.8(3) 1_456 1_456 ? N1 Ag1 O8 132.0(3) . . ? N1 Ag1 O1 123.6(3) . . ? O8 Ag1 O1 104.5(2) . . ? O2 C1 O1 125.9(8) . . ? O2 C1 C1 117.7(11) . 2_777 ? O1 C1 C1 116.4(10) . 2_777 ? O3 C2 O4 126.4(9) . . ? O3 C2 C2 117.9(10) . 2_677 ? O4 C2 C2 115.7(11) . 2_677 ? O6 C3 O5 121.3(8) . . ? O6 C3 C4 119.7(9) . . ? O5 C3 C4 119.0(9) . . ? O6 C3 Dy1 61.2(5) . 1_654 ? O5 C3 Dy1 60.2(5) . 1_654 ? C4 C3 Dy1 178.2(7) . 1_654 ? C5 C4 C8 118.4(9) . . ? C5 C4 C3 120.8(10) . . ? C8 C4 C3 120.9(9) . . ? C4 C5 C6 120.1(10) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? N1 C6 C5 121.7(9) . . ? N1 C6 H6 119.2 . . ? C5 C6 H6 119.2 . . ? N1 C7 C8 125.0(11) . . ? N1 C7 H7 117.5 . . ? C8 C7 H7 117.5 . . ? C7 C8 C4 117.6(10) . . ? C7 C8 H8 121.2 . . ? C4 C8 H8 121.2 . . ? O8 C9 O7 123.8(10) . . ? O8 C9 C10 117.9(10) . . ? O7 C9 C10 118.3(9) . . ? C14 C10 C11 116.7(10) . . ? C14 C10 C9 122.7(9) . . ? C11 C10 C9 120.6(10) . . ? C12 C11 C10 119.5(10) . . ? C12 C11 H11 120.2 . . ? C10 C11 H11 120.2 . . ? N2 C12 C11 122.4(9) . . ? N2 C12 H12 118.8 . . ? C11 C12 H12 118.8 . . ? N2 C13 C14 123.5(10) . . ? N2 C13 H13 118.3 . . ? C14 C13 H13 118.3 . . ? C13 C14 C10 120.0(9) . . ? C13 C14 H14 120.0 . . ? C10 C14 H14 120.0 . . ? C7 N1 C6 117.0(9) . . ? C7 N1 Ag1 123.1(7) . . ? C6 N1 Ag1 119.8(6) . . ? C13 N2 C12 117.7(9) . . ? C13 N2 Ag2 122.1(7) . . ? C12 N2 Ag2 120.2(7) . . ? C1 O1 Ag1 121.8(5) . . ? C1 O1 Dy1 119.2(5) . . ? Ag1 O1 Dy1 119.0(3) . . ? C1 O2 Dy1 118.7(6) . 2_777 ? C2 O3 Dy1 119.1(6) . . ? C2 O4 Dy1 119.6(6) . 2_677 ? C3 O5 Dy1 92.3(5) . 1_654 ? C3 O6 Dy1 92.0(5) . 1_654 ? C9 O7 Dy1 150.1(6) . . ? C9 O8 Ag1 119.9(7) . . ? Dy1 O11 H11A 130.9 . . ? Dy1 O11 H11B 115.4 . . ? H11A O11 H11B 103.6 . . ? O12 N3 O13 121(3) . . ? O12 N3 H11B 115.0 . . ? O13 N3 H11B 120.0 . . ? N3 O13 H15B 109.2 . . ? H14A O14 H14B 106.7 . . ? H15A O15 H15B 106.9 . . ? H16A O16 H16B 107(3) . . ? H16A O16 H16C 145(5) . . ? H16B O16 H16C 108(3) . . ? C15 N5 C19 120.0 . . ? C16 C15 N5 120.0 . . ? C16 C15 H15 120.0 . . ? N5 C15 H15 120.0 . . ? C15 C16 C17 120.0 . . ? C15 C16 H16 120.0 . . ? C17 C16 H16 120.0 . . ? C18 C17 C16 120.0 . . ? C18 C17 C20 123.6(14) . . ? C16 C17 C20 116.4(14) . . ? C17 C18 C19 120.0 . . ? C17 C18 H18 120.0 . . ? C19 C18 H18 120.0 . . ? C18 C19 N5 120.0 . . ? C18 C19 H19 120.0 . . ? N5 C19 H19 120.0 . . ? O9 C20 O10 125(2) . . ? O9 C20 C17 121(2) . . ? O10 C20 C17 113(2) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.20 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.794 _refine_diff_density_min -3.412 _refine_diff_density_rms 0.214 # Attachment 'Cifs.cif' data_1 #TrackingRef '- Cifs.txt' _database_code_depnum_ccdc_archive 'CCDC 727506' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H32 Cu6 La2 I5 N6 Na O20, 0.5(H4 O2)' _chemical_formula_sum 'C38 H34 Cu6 I5 La2 N6 Na O21' _chemical_formula_weight 2227.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' La La -0.2871 2.4523 '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' Na Na 0.0362 0.0249 '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 '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.1755(7) _cell_length_b 11.4346(12) _cell_length_c 18.3179(19) _cell_angle_alpha 86.1880(10) _cell_angle_beta 78.8800(10) _cell_angle_gamma 73.5730(10) _cell_volume 1414.4(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2012 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 24.82 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.615 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1036 _exptl_absorpt_coefficient_mu 6.498 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.3423 _exptl_absorpt_correction_T_max 0.3876 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II area-detector diffractometer' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7378 _diffrn_reflns_av_R_equivalents 0.0253 _diffrn_reflns_av_sigmaI/netI 0.0566 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 25.20 _reflns_number_total 5013 _reflns_number_gt 3797 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0193P)^2^+5.2846P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5013 _refine_ls_number_parameters 375 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0588 _refine_ls_R_factor_gt 0.0388 _refine_ls_wR_factor_ref 0.0768 _refine_ls_wR_factor_gt 0.0681 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.014 _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 La1 La 0.30407(6) 0.28845(4) 0.47693(2) 0.01837(11) Uani 1 1 d . . . I2 I 0.0000 0.5000 1.0000 0.0478(3) Uani 1 2 d S . . I1 I 0.59342(8) 0.29599(5) 1.02793(3) 0.03313(15) Uani 1 1 d . . . I3 I 0.23380(8) 0.08774(5) 0.94352(3) 0.03682(15) Uani 1 1 d . . . Cu2 Cu 0.39340(17) 0.47979(11) 0.95270(6) 0.0436(3) Uani 1 1 d . . . Cu3 Cu -0.05864(18) 0.29204(12) 0.94480(6) 0.0549(3) Uani 1 1 d . . . Cu1 Cu 0.9436(2) 0.08193(14) 1.05292(7) 0.0676(4) Uani 1 1 d . . . O3 O 0.3019(8) 0.4355(4) 0.5828(3) 0.0278(12) Uani 1 1 d . . . O9 O 0.6241(7) 0.3454(5) 0.4432(3) 0.0353(14) Uani 1 1 d D . . H9B H 0.6431 0.4142 0.4459 0.053 Uiso 1 1 d RD . . H9A H 0.7375 0.2968 0.4288 0.053 Uiso 1 1 d RD . . O4 O 0.4251(8) 0.2403(4) 0.6067(3) 0.0292(13) Uani 1 1 d . . . O1 O 0.3420(8) 0.2166(5) 0.3429(3) 0.0387(15) Uani 1 1 d . . . O2 O 0.0423(8) 0.2332(6) 0.4061(3) 0.0428(16) Uani 1 1 d . . . O5 O -0.0214(7) 0.3341(4) 0.5605(3) 0.0280(12) Uani 1 1 d . . . O7 O 0.6106(7) 0.1102(4) 0.4568(3) 0.0315(13) Uani 1 1 d . . . N2 N 0.4065(9) 0.4379(6) 0.8464(3) 0.0286(16) Uani 1 1 d . . . N1 N 0.0024(11) 0.1269(7) 0.1477(4) 0.0432(19) Uani 1 1 d . . . N3 N -0.0682(9) 0.3347(6) 0.8359(4) 0.0314(16) Uani 1 1 d . . . C9 C 0.4626(12) 0.2911(7) 0.7512(4) 0.0310(19) Uani 1 1 d . . . H9 H 0.5072 0.2100 0.7369 0.037 Uiso 1 1 calc R . . C10 C 0.4707(11) 0.3233(7) 0.8212(4) 0.0302(19) Uani 1 1 d . . . H10 H 0.5240 0.2617 0.8532 0.036 Uiso 1 1 calc R . . C11 C 0.3327(12) 0.5238(7) 0.7979(5) 0.036(2) Uani 1 1 d . . . H11 H 0.2870 0.6043 0.8136 0.043 Uiso 1 1 calc R . . C12 C 0.3207(12) 0.5005(7) 0.7272(4) 0.0320(19) Uani 1 1 d . . . H12 H 0.2686 0.5638 0.6959 0.038 Uiso 1 1 calc R . . C8 C 0.3871(10) 0.3815(7) 0.7025(4) 0.0248(17) Uani 1 1 d . . . C7 C 0.3722(11) 0.3505(7) 0.6259(4) 0.0247(18) Uani 1 1 d . . . C1 C 0.1667(13) 0.2099(7) 0.3484(5) 0.033(2) Uani 1 1 d . . . C2 C 0.1068(12) 0.1800(8) 0.2786(4) 0.033(2) Uani 1 1 d . . . C3 C -0.0671(12) 0.1500(8) 0.2805(5) 0.041(2) Uani 1 1 d . . . H3 H -0.1535 0.1484 0.3252 0.050 Uiso 1 1 calc R . . C4 C -0.1104(13) 0.1224(8) 0.2144(5) 0.042(2) Uani 1 1 d . . . H4 H -0.2256 0.0993 0.2166 0.051 Uiso 1 1 calc R . . C5 C 0.1700(15) 0.1569(10) 0.1479(5) 0.060(3) Uani 1 1 d . . . H5 H 0.2530 0.1600 0.1025 0.072 Uiso 1 1 calc R . . C6 C 0.2262(14) 0.1832(10) 0.2104(5) 0.056(3) Uani 1 1 d . . . H6 H 0.3445 0.2032 0.2070 0.067 Uiso 1 1 calc R . . C15 C -0.0175(11) 0.2688(7) 0.7110(4) 0.0283(18) Uani 1 1 d . . . H15 H 0.0310 0.2050 0.6774 0.034 Uiso 1 1 calc R . . C16 C -0.0087(12) 0.2482(8) 0.7849(5) 0.035(2) Uani 1 1 d . . . H16 H 0.0423 0.1684 0.8004 0.042 Uiso 1 1 calc R . . C17 C -0.1452(11) 0.4492(7) 0.8119(4) 0.0312(19) Uani 1 1 d . . . H17 H -0.1864 0.5117 0.8463 0.037 Uiso 1 1 calc R . . C18 C -0.1661(11) 0.4784(7) 0.7395(4) 0.0309(19) Uani 1 1 d . . . H18 H -0.2236 0.5584 0.7259 0.037 Uiso 1 1 calc R . . C14 C -0.1003(10) 0.3869(7) 0.6870(4) 0.0222(17) Uani 1 1 d . . . C13 C -0.1138(10) 0.4170(7) 0.6068(4) 0.0224(17) Uani 1 1 d . . . C19 C 0.6031(10) 0.0069(7) 0.4821(4) 0.0228(17) Uani 1 1 d . . . O10 O 1.1743(10) -0.1054(7) 0.4031(4) 0.077(2) Uani 1 1 d D . . H10A H 1.3011 -0.1388 0.4058 0.115 Uiso 1 1 d RD . . H10B H 1.1734 -0.0978 0.3546 0.115 Uiso 1 1 d RD . . Na1 Na 1.0220(13) -0.0389(7) 0.5121(6) 0.057(2) Uani 0.50 1 d P . . O11 O 0.394(3) 0.0256(15) 0.7012(12) 0.106(7) Uani 0.50 1 d PD . . O8 O 0.7470(7) -0.0842(4) 0.4808(3) 0.0289(13) Uani 1 1 d . . . O6 O -0.2134(8) 0.5194(5) 0.5910(3) 0.0356(14) Uani 1 1 d . . . H11B H 0.488(13) 0.055(12) 0.695(12) 0.053 Uiso 0.50 1 d PD . . H11A H 0.431(19) -0.046(5) 0.688(10) 0.053 Uiso 0.50 1 d PD . . 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 La1 0.0218(2) 0.0155(2) 0.0186(2) -0.00074(17) -0.00612(19) -0.00445(18) I2 0.0315(5) 0.0610(6) 0.0540(6) -0.0267(5) 0.0026(4) -0.0190(4) I1 0.0327(3) 0.0322(3) 0.0353(3) 0.0021(2) -0.0073(3) -0.0100(2) I3 0.0402(3) 0.0387(3) 0.0344(3) 0.0043(3) -0.0102(3) -0.0142(3) Cu2 0.0544(7) 0.0533(7) 0.0279(6) -0.0063(5) -0.0135(6) -0.0171(6) Cu3 0.0564(8) 0.0765(9) 0.0286(6) 0.0101(6) -0.0088(6) -0.0148(7) Cu1 0.0742(10) 0.1144(12) 0.0363(7) -0.0234(8) -0.0042(7) -0.0602(9) O3 0.039(3) 0.026(3) 0.023(3) 0.002(2) -0.011(3) -0.012(2) O9 0.025(3) 0.022(3) 0.060(4) -0.001(3) -0.001(3) -0.011(2) O4 0.043(3) 0.025(3) 0.022(3) 0.000(2) -0.016(3) -0.007(3) O1 0.029(3) 0.054(4) 0.036(3) -0.016(3) -0.004(3) -0.015(3) O2 0.036(4) 0.065(4) 0.028(3) -0.015(3) -0.006(3) -0.011(3) O5 0.027(3) 0.028(3) 0.027(3) -0.005(3) -0.002(3) -0.005(2) O7 0.025(3) 0.017(3) 0.047(4) 0.006(3) 0.001(3) -0.002(2) N2 0.029(4) 0.045(4) 0.017(3) 0.000(3) -0.007(3) -0.018(3) N1 0.044(5) 0.067(5) 0.028(4) -0.008(4) -0.003(4) -0.030(4) N3 0.030(4) 0.038(4) 0.027(4) -0.001(3) -0.007(3) -0.010(3) C9 0.038(5) 0.030(4) 0.030(5) -0.006(4) -0.010(4) -0.013(4) C10 0.033(5) 0.035(5) 0.029(5) 0.000(4) -0.008(4) -0.017(4) C11 0.040(5) 0.033(5) 0.031(5) -0.010(4) -0.011(4) 0.001(4) C12 0.039(5) 0.032(4) 0.024(4) -0.006(4) -0.009(4) -0.005(4) C8 0.018(4) 0.027(4) 0.031(5) -0.002(4) -0.008(4) -0.007(3) C7 0.027(4) 0.031(5) 0.020(4) -0.006(4) -0.004(4) -0.013(4) C1 0.040(5) 0.031(5) 0.027(5) -0.007(4) -0.007(4) -0.009(4) C2 0.034(5) 0.045(5) 0.026(5) -0.009(4) -0.014(4) -0.011(4) C3 0.036(5) 0.059(6) 0.033(5) -0.013(5) -0.012(4) -0.012(5) C4 0.042(6) 0.060(6) 0.042(6) 0.004(5) -0.019(5) -0.036(5) C5 0.066(7) 0.104(9) 0.027(5) -0.012(6) -0.007(5) -0.049(7) C6 0.056(7) 0.097(9) 0.029(5) -0.015(5) -0.001(5) -0.046(6) C15 0.027(5) 0.023(4) 0.033(5) -0.002(4) -0.005(4) -0.005(3) C16 0.038(5) 0.034(5) 0.034(5) 0.013(4) -0.011(4) -0.012(4) C17 0.028(5) 0.038(5) 0.026(5) -0.012(4) 0.007(4) -0.011(4) C18 0.034(5) 0.031(5) 0.026(5) 0.000(4) 0.001(4) -0.009(4) C14 0.015(4) 0.029(4) 0.021(4) 0.002(3) -0.002(3) -0.005(3) C13 0.014(4) 0.023(4) 0.028(4) 0.007(4) -0.001(3) -0.004(3) C19 0.022(4) 0.025(4) 0.022(4) -0.006(3) -0.004(3) -0.005(4) O10 0.055(5) 0.092(6) 0.082(6) -0.038(5) -0.028(4) 0.000(4) Na1 0.033(5) 0.073(8) 0.074(7) 0.002(6) -0.013(4) -0.028(6) O11 0.162(19) 0.049(11) 0.106(15) -0.016(11) -0.001(15) -0.038(11) O8 0.016(3) 0.018(3) 0.052(4) 0.002(3) -0.006(3) -0.004(2) O6 0.049(4) 0.027(3) 0.027(3) 0.007(2) -0.011(3) -0.001(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 La1 O6 2.438(5) 2_566 ? La1 O5 2.472(5) . ? La1 O8 2.514(5) 2_656 ? La1 O9 2.515(5) . ? La1 O7 2.526(5) . ? La1 O1 2.580(5) . ? La1 O3 2.646(5) . ? La1 O4 2.657(5) . ? La1 O2 2.707(5) . ? La1 Na1 4.144(9) 2_656 ? I2 Cu2 2.7362(12) . ? I2 Cu2 2.7362(12) 2_567 ? I2 Cu3 2.8114(14) . ? I2 Cu3 2.8114(14) 2_567 ? I1 Cu2 2.6419(13) 2_667 ? I1 Cu3 2.6520(14) 1_655 ? I1 Cu2 2.6547(13) . ? I1 Cu1 3.0547(17) . ? I3 Cu1 2.5956(14) 2_657 ? I3 Cu1 2.6091(14) 1_455 ? I3 Cu3 2.6602(14) . ? Cu2 N2 2.015(6) . ? Cu2 I1 2.6419(13) 2_667 ? Cu2 Cu2 2.662(2) 2_667 ? Cu3 N3 2.031(7) . ? Cu3 I1 2.6520(14) 1_455 ? Cu3 Cu1 3.009(2) 1_455 ? Cu1 N1 1.996(7) 1_656 ? Cu1 I3 2.5956(14) 2_657 ? Cu1 I3 2.6091(14) 1_655 ? Cu1 Cu1 2.635(2) 2_757 ? Cu1 Cu3 3.009(2) 1_655 ? O3 C7 1.264(9) . ? O9 H9B 0.8413 . ? O9 H9A 0.8493 . ? O4 C7 1.262(8) . ? O1 C1 1.266(9) . ? O2 C1 1.234(9) . ? O2 Na1 2.696(10) 2_656 ? O5 C13 1.262(8) . ? O7 C19 1.252(8) . ? O7 Na1 2.691(10) 2_756 ? N2 C10 1.341(9) . ? N2 C11 1.344(10) . ? N1 C4 1.336(11) . ? N1 C5 1.341(11) . ? N1 Cu1 1.996(7) 1_454 ? N3 C16 1.328(10) . ? N3 C17 1.349(10) . ? C9 C10 1.374(10) . ? C9 C8 1.380(10) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.363(10) . ? C11 H11 0.9300 . ? C12 C8 1.384(10) . ? C12 H12 0.9300 . ? C8 C7 1.501(10) . ? C1 C2 1.513(10) . ? C2 C6 1.377(11) . ? C2 C3 1.378(11) . ? C3 C4 1.382(11) . ? C3 H3 0.9300 . ? C4 H4 0.9300 . ? C5 C6 1.362(11) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C15 C16 1.369(11) . ? C15 C14 1.392(10) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 C18 1.371(10) . ? C17 H17 0.9300 . ? C18 C14 1.386(10) . ? C18 H18 0.9300 . ? C14 C13 1.501(10) . ? C13 O6 1.236(8) . ? C19 O8 1.240(8) . ? C19 C19 1.545(14) 2_656 ? C19 Na1 2.839(11) 2_756 ? O10 Na1 2.155(13) . ? O10 Na1 2.302(12) 2_756 ? O10 H10A 0.8909 . ? O10 H10B 0.8881 . ? Na1 Na1 0.963(14) 2_756 ? Na1 O10 2.302(12) 2_756 ? Na1 O8 2.354(10) . ? Na1 O8 2.485(10) 2_756 ? Na1 O7 2.691(10) 2_756 ? Na1 O2 2.696(10) 2_656 ? Na1 C19 2.839(11) 2_756 ? Na1 La1 4.144(9) 2_656 ? Na1 H10A 2.5704 . ? O11 H11B 0.822(11) . ? O11 H11A 0.822(11) . ? O8 Na1 2.485(10) 2_756 ? O8 La1 2.514(5) 2_656 ? O6 La1 2.438(5) 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 O6 La1 O5 92.27(17) 2_566 . ? O6 La1 O8 150.95(17) 2_566 2_656 ? O5 La1 O8 74.68(16) . 2_656 ? O6 La1 O9 76.84(18) 2_566 . ? O5 La1 O9 144.49(17) . . ? O8 La1 O9 128.18(16) 2_656 . ? O6 La1 O7 131.44(18) 2_566 . ? O5 La1 O7 136.12(17) . . ? O8 La1 O7 64.51(15) 2_656 . ? O9 La1 O7 65.07(16) . . ? O6 La1 O1 77.63(18) 2_566 . ? O5 La1 O1 120.36(17) . . ? O8 La1 O1 86.67(18) 2_656 . ? O9 La1 O1 90.59(18) . . ? O7 La1 O1 73.96(18) . . ? O6 La1 O3 82.19(17) 2_566 . ? O5 La1 O3 70.97(16) . . ? O8 La1 O3 116.22(17) 2_656 . ? O9 La1 O3 74.08(17) . . ? O7 La1 O3 112.91(17) . . ? O1 La1 O3 157.03(17) . . ? O6 La1 O4 130.51(16) 2_566 . ? O5 La1 O4 80.98(16) . . ? O8 La1 O4 73.88(16) 2_656 . ? O9 La1 O4 81.02(17) . . ? O7 La1 O4 73.10(17) . . ? O1 La1 O4 146.50(17) . . ? O3 La1 O4 49.13(15) . . ? O6 La1 O2 82.38(19) 2_566 . ? O5 La1 O2 71.44(17) . . ? O8 La1 O2 68.95(18) 2_656 . ? O9 La1 O2 137.99(18) . . ? O7 La1 O2 106.16(17) . . ? O1 La1 O2 49.09(17) . . ? O3 La1 O2 138.51(17) . . ? O4 La1 O2 138.18(17) . . ? O6 La1 Na1 120.50(17) 2_566 2_656 ? O5 La1 Na1 62.33(18) . 2_656 ? O8 La1 Na1 30.51(15) 2_656 2_656 ? O9 La1 Na1 151.33(17) . 2_656 ? O7 La1 Na1 87.47(16) . 2_656 ? O1 La1 Na1 73.1(2) . 2_656 ? O3 La1 Na1 127.63(19) . 2_656 ? O4 La1 Na1 99.48(17) . 2_656 ? O2 La1 Na1 39.82(18) . 2_656 ? Cu2 I2 Cu2 180.0 . 2_567 ? Cu2 I2 Cu3 104.77(3) . . ? Cu2 I2 Cu3 75.23(3) 2_567 . ? Cu2 I2 Cu3 75.23(3) . 2_567 ? Cu2 I2 Cu3 104.77(3) 2_567 2_567 ? Cu3 I2 Cu3 180.000(1) . 2_567 ? Cu2 I1 Cu3 79.54(4) 2_667 1_655 ? Cu2 I1 Cu2 60.34(4) 2_667 . ? Cu3 I1 Cu2 94.30(4) 1_655 . ? Cu2 I1 Cu1 119.05(4) 2_667 . ? Cu3 I1 Cu1 63.17(4) 1_655 . ? Cu2 I1 Cu1 155.87(4) . . ? Cu1 I3 Cu1 60.84(5) 2_657 1_455 ? Cu1 I3 Cu3 103.18(5) 2_657 . ? Cu1 I3 Cu3 69.63(5) 1_455 . ? N2 Cu2 I1 114.74(19) . 2_667 ? N2 Cu2 I1 112.9(2) . . ? I1 Cu2 I1 119.66(4) 2_667 . ? N2 Cu2 Cu2 143.39(19) . 2_667 ? I1 Cu2 Cu2 60.07(4) 2_667 2_667 ? I1 Cu2 Cu2 59.59(4) . 2_667 ? N2 Cu2 I2 96.85(18) . . ? I1 Cu2 I2 101.42(4) 2_667 . ? I1 Cu2 I2 107.48(4) . . ? Cu2 Cu2 I2 119.75(6) 2_667 . ? N3 Cu3 I1 114.17(19) . 1_455 ? N3 Cu3 I3 105.02(19) . . ? I1 Cu3 I3 118.01(5) 1_455 . ? N3 Cu3 I2 103.48(19) . . ? I1 Cu3 I2 99.24(4) 1_455 . ? I3 Cu3 I2 116.32(5) . . ? N3 Cu3 Cu1 140.6(2) . 1_455 ? I1 Cu3 Cu1 64.96(4) 1_455 1_455 ? I3 Cu3 Cu1 54.38(4) . 1_455 ? I2 Cu3 Cu1 115.66(4) . 1_455 ? N1 Cu1 I3 118.6(2) 1_656 2_657 ? N1 Cu1 I3 110.0(2) 1_656 1_655 ? I3 Cu1 I3 119.16(5) 2_657 1_655 ? N1 Cu1 Cu1 144.2(2) 1_656 2_757 ? I3 Cu1 Cu1 59.83(5) 2_657 2_757 ? I3 Cu1 Cu1 59.33(5) 1_655 2_757 ? N1 Cu1 Cu3 108.3(2) 1_656 1_655 ? I3 Cu1 Cu3 128.62(5) 2_657 1_655 ? I3 Cu1 Cu3 55.98(4) 1_655 1_655 ? Cu1 Cu1 Cu3 93.49(7) 2_757 1_655 ? N1 Cu1 I1 102.1(2) 1_656 . ? I3 Cu1 I1 96.75(4) 2_657 . ? I3 Cu1 I1 106.77(5) 1_655 . ? Cu1 Cu1 I1 113.66(8) 2_757 . ? Cu3 Cu1 I1 51.87(4) 1_655 . ? C7 O3 La1 94.8(4) . . ? La1 O9 H9B 128.1 . . ? La1 O9 H9A 126.0 . . ? H9B O9 H9A 105.8 . . ? C7 O4 La1 94.3(4) . . ? C1 O1 La1 96.5(5) . . ? C1 O2 Na1 115.7(6) . 2_656 ? C1 O2 La1 91.2(5) . . ? Na1 O2 La1 100.2(3) 2_656 . ? C13 O5 La1 134.0(5) . . ? C19 O7 La1 120.0(4) . . ? C19 O7 Na1 83.6(4) . 2_756 ? La1 O7 Na1 140.2(3) . 2_756 ? C10 N2 C11 115.7(7) . . ? C10 N2 Cu2 123.1(5) . . ? C11 N2 Cu2 120.9(5) . . ? C4 N1 C5 115.5(7) . . ? C4 N1 Cu1 124.1(6) . 1_454 ? C5 N1 Cu1 120.3(6) . 1_454 ? C16 N3 C17 116.3(7) . . ? C16 N3 Cu3 120.7(6) . . ? C17 N3 Cu3 122.8(5) . . ? C10 C9 C8 118.8(7) . . ? C10 C9 H9 120.6 . . ? C8 C9 H9 120.6 . . ? N2 C10 C9 124.2(8) . . ? N2 C10 H10 117.9 . . ? C9 C10 H10 117.9 . . ? N2 C11 C12 124.2(7) . . ? N2 C11 H11 117.9 . . ? C12 C11 H11 117.9 . . ? C11 C12 C8 119.1(8) . . ? C11 C12 H12 120.4 . . ? C8 C12 H12 120.4 . . ? C9 C8 C12 118.1(7) . . ? C9 C8 C7 120.6(7) . . ? C12 C8 C7 121.2(7) . . ? O3 C7 O4 121.6(6) . . ? O3 C7 C8 118.9(6) . . ? O4 C7 C8 119.5(7) . . ? O2 C1 O1 123.2(8) . . ? O2 C1 C2 119.5(8) . . ? O1 C1 C2 117.2(7) . . ? C6 C2 C3 117.8(8) . . ? C6 C2 C1 120.2(8) . . ? C3 C2 C1 122.0(8) . . ? C2 C3 C4 118.6(8) . . ? C2 C3 H3 120.7 . . ? C4 C3 H3 120.7 . . ? N1 C4 C3 124.3(8) . . ? N1 C4 H4 117.9 . . ? C3 C4 H4 117.9 . . ? N1 C5 C6 124.2(9) . . ? N1 C5 H5 117.9 . . ? C6 C5 H5 117.9 . . ? C5 C6 C2 119.6(8) . . ? C5 C6 H6 120.2 . . ? C2 C6 H6 120.2 . . ? C16 C15 C14 118.8(7) . . ? C16 C15 H15 120.6 . . ? C14 C15 H15 120.6 . . ? N3 C16 C15 124.4(8) . . ? N3 C16 H16 117.8 . . ? C15 C16 H16 117.8 . . ? N3 C17 C18 123.7(7) . . ? N3 C17 H17 118.2 . . ? C18 C17 H17 118.2 . . ? C17 C18 C14 119.0(7) . . ? C17 C18 H18 120.5 . . ? C14 C18 H18 120.5 . . ? C18 C14 C15 117.8(7) . . ? C18 C14 C13 120.1(7) . . ? C15 C14 C13 122.0(7) . . ? O6 C13 O5 125.0(7) . . ? O6 C13 C14 118.4(7) . . ? O5 C13 C14 116.5(6) . . ? O8 C19 O7 125.3(7) . . ? O8 C19 C19 117.9(8) . 2_656 ? O7 C19 C19 116.8(8) . 2_656 ? O8 C19 Na1 60.9(4) . 2_756 ? O7 C19 Na1 70.4(4) . 2_756 ? C19 C19 Na1 153.2(7) 2_656 2_756 ? Na1 O10 Na1 24.7(4) . 2_756 ? Na1 O10 H10A 107.7 . . ? Na1 O10 H10A 120.3 2_756 . ? Na1 O10 H10B 145.5 . . ? Na1 O10 H10B 123.1 2_756 . ? H10A O10 H10B 104.0 . . ? Na1 Na1 O10 86.2(13) 2_756 . ? Na1 Na1 O10 69.1(12) 2_756 2_756 ? O10 Na1 O10 155.3(4) . 2_756 ? Na1 Na1 O8 86.2(11) 2_756 . ? O10 Na1 O8 85.7(4) . . ? O10 Na1 O8 92.4(4) 2_756 . ? Na1 Na1 O8 71.0(10) 2_756 2_756 ? O10 Na1 O8 92.6(4) . 2_756 ? O10 Na1 O8 79.7(4) 2_756 2_756 ? O8 Na1 O8 157.2(3) . 2_756 ? Na1 Na1 O7 119.5(12) 2_756 2_756 ? O10 Na1 O7 82.8(4) . 2_756 ? O10 Na1 O7 108.9(4) 2_756 2_756 ? O8 Na1 O7 150.8(4) . 2_756 ? O8 Na1 O7 50.4(2) 2_756 2_756 ? Na1 Na1 O2 152.7(13) 2_756 2_656 ? O10 Na1 O2 106.8(4) . 2_656 ? O10 Na1 O2 95.8(4) 2_756 2_656 ? O8 Na1 O2 71.4(3) . 2_656 ? O8 Na1 O2 130.3(4) 2_756 2_656 ? O7 Na1 O2 86.4(3) 2_756 2_656 ? Na1 Na1 C19 93.5(11) 2_756 2_756 ? O10 Na1 C19 81.4(4) . 2_756 ? O10 Na1 C19 99.5(4) 2_756 2_756 ? O8 Na1 C19 167.1(5) . 2_756 ? O8 Na1 C19 25.9(2) 2_756 2_756 ? O7 Na1 C19 26.00(19) 2_756 2_756 ? O2 Na1 C19 111.8(3) 2_656 2_756 ? Na1 Na1 La1 119.1(12) 2_756 2_656 ? O10 Na1 La1 89.1(3) . 2_656 ? O10 Na1 La1 102.6(3) 2_756 2_656 ? O8 Na1 La1 32.83(17) . 2_656 ? O8 Na1 La1 169.9(3) 2_756 2_656 ? O7 Na1 La1 120.0(2) 2_756 2_656 ? O2 Na1 La1 40.02(17) 2_656 2_656 ? C19 Na1 La1 145.4(3) 2_756 2_656 ? Na1 Na1 H10A 97.3 2_756 . ? O10 Na1 H10A 19.3 . . ? O10 Na1 H10A 159.5 2_756 . ? O8 Na1 H10A 102.1 . . ? O8 Na1 H10A 81.4 2_756 . ? O7 Na1 H10A 63.6 2_756 . ? O2 Na1 H10A 102.4 2_656 . ? C19 Na1 H10A 65.1 2_756 . ? La1 Na1 H10A 97.4 2_656 . ? H11B O11 H11A 110(2) . . ? C19 O8 Na1 112.6(5) . . ? C19 O8 Na1 93.2(5) . 2_756 ? Na1 O8 Na1 22.8(3) . 2_756 ? C19 O8 La1 120.2(5) . 2_656 ? Na1 O8 La1 116.7(3) . 2_656 ? Na1 O8 La1 139.4(3) 2_756 2_656 ? C13 O6 La1 158.8(5) . 2_566 ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.20 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.105 _refine_diff_density_min -1.489 _refine_diff_density_rms 0.169 ########################################################################### data_9 #TrackingRef '- Cifs.txt' _database_code_depnum_ccdc_archive 'CCDC 727507' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H8 Ag N2 O8 Tm, H2 O' _chemical_formula_sum 'C14 H10 Ag N2 O9 Tm' _chemical_formula_weight 627.04 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tm Tm -0.3139 5.2483 '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 21.893(4) _cell_length_b 9.2903(17) _cell_length_c 17.243(3) _cell_angle_alpha 90.00 _cell_angle_beta 108.622(2) _cell_angle_gamma 90.00 _cell_volume 3323.5(10) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3299 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 27.89 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.506 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2368 _exptl_absorpt_coefficient_mu 6.538 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3406 _exptl_absorpt_correction_T_max 0.3858 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8250 _diffrn_reflns_av_R_equivalents 0.0348 _diffrn_reflns_av_sigmaI/netI 0.0396 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 25.19 _reflns_number_total 3003 _reflns_number_gt 2510 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0587P)^2^+180.7559P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3003 _refine_ls_number_parameters 252 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0590 _refine_ls_R_factor_gt 0.0499 _refine_ls_wR_factor_ref 0.1394 _refine_ls_wR_factor_gt 0.1334 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.065 _refine_ls_shift/su_mean 0.006 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 Tm1 Tm 0.01308(2) -0.18533(5) 1.07338(3) 0.02684(19) Uani 1 1 d . . . Ag1 Ag 0.32773(5) 0.06516(15) 0.86140(7) 0.0554(4) Uani 1 1 d . . . O5 O 0.0631(3) -0.4263(7) 1.0791(4) 0.0222(15) Uani 1 1 d . . . C13 C 0.0354(5) -0.5149(10) 1.0249(6) 0.018(2) Uani 1 1 d . . . O7 O -0.0573(4) -0.2675(8) 1.1545(4) 0.0222(15) Uani 1 1 d . . . O1 O 0.0729(3) 0.0495(8) 1.0311(4) 0.0216(15) Uani 1 1 d . . . O2 O 0.1317(4) -0.1228(9) 1.1058(5) 0.0285(17) Uani 1 1 d . . . C1 C 0.1245(5) -0.0218(11) 1.0568(6) 0.021(2) Uani 1 1 d . . . C2 C 0.1782(5) 0.0110(12) 1.0218(6) 0.023(2) Uani 1 1 d . . . C3 C 0.1718(6) 0.1187(14) 0.9662(8) 0.039(3) Uani 1 1 d . . . H3 H 0.1378 0.1837 0.9559 0.047 Uiso 1 1 calc R . . N2 N 0.3605(5) 0.1626(11) 0.7668(6) 0.033(2) Uani 1 1 d . . . C7 C 0.3650(6) 0.3063(14) 0.7609(7) 0.036(3) Uani 1 1 d . . . H7 H 0.3455 0.3646 0.7900 0.043 Uiso 1 1 calc R . . C12 C 0.3874(7) 0.0838(14) 0.7217(10) 0.051(4) Uani 1 1 d . . . H12 H 0.3844 -0.0158 0.7245 0.061 Uiso 1 1 calc R . . N1 N 0.2667(5) 0.0463(13) 0.9398(6) 0.039(3) Uani 1 1 d . . . C14 C -0.0368(5) -0.2474(10) 1.2300(6) 0.019(2) Uani 1 1 d . . . O8 O -0.0696(3) -0.2317(8) 1.2771(4) 0.0207(15) Uani 1 1 d . . . C11 C 0.4186(7) 0.1377(13) 0.6726(9) 0.040(3) Uani 1 1 d . . . H11 H 0.4351 0.0767 0.6415 0.048 Uiso 1 1 calc R . . C4 C 0.2168(6) 0.1299(16) 0.9252(8) 0.043(3) Uani 1 1 d . . . H4 H 0.2110 0.2006 0.8853 0.052 Uiso 1 1 calc R . . C5 C 0.2753(7) -0.053(2) 0.9968(10) 0.064(5) Uani 1 1 d . . . H5 H 0.3113 -0.1119 1.0081 0.077 Uiso 1 1 calc R . . C6 C 0.2333(7) -0.0728(19) 1.0403(10) 0.062(5) Uani 1 1 d . . . H6 H 0.2417 -0.1416 1.0815 0.074 Uiso 1 1 calc R . . C9 C 0.4259(5) 0.2860(11) 0.6690(6) 0.020(2) Uani 1 1 d . . . C8 C 0.3973(6) 0.3702(13) 0.7134(7) 0.032(3) Uani 1 1 d . . . H8 H 0.3999 0.4700 0.7114 0.039 Uiso 1 1 calc R . . C10 C 0.4620(5) 0.3525(11) 0.6168(6) 0.020(2) Uani 1 1 d . . . O4 O 0.4843(4) 0.4752(8) 0.6358(4) 0.0244(16) Uani 1 1 d . . . O3 O 0.4641(4) 0.2807(8) 0.5566(4) 0.0267(17) Uani 1 1 d . . . O6 O 0.0604(3) -0.6261(8) 1.0074(4) 0.0237(16) Uani 1 1 d . . . O1W O 0.2036(5) 0.6977(14) 0.2419(8) 0.059(3) Uani 1 1 d D . . H1W H 0.234(5) 0.712(18) 0.222(8) 0.05(5) Uiso 1 1 d D . . H2W H 0.221(7) 0.68(3) 0.291(5) 0.17(13) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tm1 0.0347(3) 0.0237(3) 0.0289(3) 0.0006(2) 0.0196(2) 0.0022(2) Ag1 0.0378(6) 0.0908(9) 0.0522(6) 0.0362(6) 0.0349(5) 0.0096(6) O5 0.029(4) 0.013(3) 0.025(4) -0.003(3) 0.009(3) 0.003(3) C13 0.029(5) 0.012(5) 0.021(5) 0.009(4) 0.021(4) 0.006(4) O7 0.030(4) 0.028(4) 0.011(3) -0.002(3) 0.011(3) -0.002(3) O1 0.020(4) 0.021(4) 0.027(4) -0.002(3) 0.014(3) 0.002(3) O2 0.031(4) 0.032(4) 0.029(4) 0.011(3) 0.018(3) 0.001(3) C1 0.023(5) 0.027(6) 0.018(5) -0.003(4) 0.012(4) -0.005(4) C2 0.022(5) 0.029(6) 0.023(5) 0.002(4) 0.016(4) -0.002(4) C3 0.024(6) 0.042(7) 0.056(8) 0.025(6) 0.018(6) 0.006(5) N2 0.034(5) 0.038(6) 0.037(5) 0.017(5) 0.025(5) 0.006(4) C7 0.048(7) 0.040(7) 0.033(6) -0.012(5) 0.031(6) -0.013(6) C12 0.067(9) 0.026(7) 0.087(11) 0.020(7) 0.065(9) 0.009(6) N1 0.033(6) 0.052(7) 0.041(6) 0.019(5) 0.023(5) 0.000(5) C14 0.027(6) 0.006(4) 0.029(6) 0.004(4) 0.018(5) -0.002(4) O8 0.022(4) 0.026(4) 0.021(3) 0.002(3) 0.017(3) -0.001(3) C11 0.053(8) 0.020(6) 0.063(9) 0.007(6) 0.043(7) 0.007(5) C4 0.029(6) 0.059(9) 0.047(8) 0.033(7) 0.018(6) 0.007(6) C5 0.043(8) 0.087(12) 0.083(11) 0.050(10) 0.049(8) 0.039(8) C6 0.041(8) 0.081(11) 0.079(11) 0.058(9) 0.041(8) 0.033(8) C9 0.032(6) 0.017(5) 0.019(5) 0.001(4) 0.018(4) -0.004(4) C8 0.050(7) 0.020(6) 0.040(7) -0.013(5) 0.033(6) -0.011(5) C10 0.023(5) 0.026(6) 0.016(5) 0.007(4) 0.013(4) 0.002(4) O4 0.038(4) 0.020(4) 0.021(4) 0.002(3) 0.017(3) -0.009(3) O3 0.044(5) 0.019(4) 0.028(4) 0.000(3) 0.027(4) 0.000(3) O6 0.024(4) 0.020(4) 0.028(4) -0.003(3) 0.010(3) 0.004(3) O1W 0.038(6) 0.067(8) 0.070(8) 0.019(6) 0.015(5) 0.001(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tm1 O4 2.407(7) 8_456 ? Tm1 O6 2.483(7) 5_547 ? Tm1 O5 2.480(7) . ? Tm1 O3 2.467(7) 4_546 ? Tm1 O1 2.493(7) 5_557 ? Tm1 O7 2.509(7) . ? Tm1 O8 2.515(7) 2_557 ? Tm1 O2 2.543(8) . ? Tm1 O1 2.760(7) . ? Ag1 N2 2.178(9) . ? Ag1 N1 2.190(9) . ? O5 C13 1.248(12) . ? C13 O6 1.250(12) . ? C13 C13 1.54(2) 5_547 ? O7 C14 1.247(12) . ? O1 C1 1.261(13) . ? O1 Tm1 2.493(7) 5_557 ? O2 C1 1.239(13) . ? C1 C2 1.514(13) . ? C2 C3 1.361(16) . ? C2 C6 1.384(17) . ? C3 C4 1.390(16) . ? C3 H3 0.9300 . ? N2 C7 1.344(16) . ? N2 C12 1.334(16) . ? C7 C8 1.377(15) . ? C7 H7 0.9300 . ? C12 C11 1.343(16) . ? C12 H12 0.9300 . ? N1 C4 1.297(17) . ? N1 C5 1.316(17) . ? C14 O8 1.253(11) . ? C14 C14 1.54(2) 2_557 ? O8 Tm1 2.515(7) 2_557 ? C11 C9 1.391(16) . ? C11 H11 0.9300 . ? C4 H4 0.9300 . ? C5 C6 1.372(17) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C9 C8 1.378(14) . ? C9 C10 1.507(12) . ? C8 H8 0.9300 . ? C10 O4 1.242(13) . ? C10 O3 1.246(12) . ? O4 Tm1 2.407(7) 8 ? O3 Tm1 2.467(7) 4_556 ? O6 Tm1 2.483(7) 5_547 ? O1W H1W 0.85(12) . ? O1W H2W 0.83(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Tm1 O6 127.4(2) 8_456 5_547 ? O4 Tm1 O5 152.8(2) 8_456 . ? O6 Tm1 O5 65.4(2) 5_547 . ? O4 Tm1 O3 131.8(2) 8_456 4_546 ? O6 Tm1 O3 71.5(2) 5_547 4_546 ? O5 Tm1 O3 72.9(2) . 4_546 ? O4 Tm1 O1 70.6(2) 8_456 5_557 ? O6 Tm1 O1 75.4(2) 5_547 5_557 ? O5 Tm1 O1 135.0(2) . 5_557 ? O3 Tm1 O1 74.5(2) 4_546 5_557 ? O4 Tm1 O7 72.7(2) 8_456 . ? O6 Tm1 O7 72.2(2) 5_547 . ? O5 Tm1 O7 92.6(2) . . ? O3 Tm1 O7 143.7(2) 4_546 . ? O1 Tm1 O7 95.8(2) 5_557 . ? O4 Tm1 O8 78.1(2) 8_456 2_557 ? O6 Tm1 O8 118.2(2) 5_547 2_557 ? O5 Tm1 O8 74.8(2) . 2_557 ? O3 Tm1 O8 137.2(2) 4_546 2_557 ? O1 Tm1 O8 146.9(2) 5_557 2_557 ? O7 Tm1 O8 64.2(2) . 2_557 ? O4 Tm1 O2 96.4(3) 8_456 . ? O6 Tm1 O2 135.8(2) 5_547 . ? O5 Tm1 O2 77.9(2) . . ? O3 Tm1 O2 74.9(3) 4_546 . ? O1 Tm1 O2 121.7(2) 5_557 . ? O7 Tm1 O2 135.5(2) . . ? O8 Tm1 O2 71.4(2) 2_557 . ? O4 Tm1 O1 72.0(2) 8_456 . ? O6 Tm1 O1 133.4(2) 5_547 . ? O5 Tm1 O1 118.9(2) . . ? O3 Tm1 O1 67.1(2) 4_546 . ? O1 Tm1 O1 73.8(2) 5_557 . ? O7 Tm1 O1 144.7(2) . . ? O8 Tm1 O1 106.6(2) 2_557 . ? O2 Tm1 O1 48.7(2) . . ? N2 Ag1 N1 155.2(4) . . ? C13 O5 Tm1 117.6(6) . . ? O5 C13 O6 125.5(10) . . ? O5 C13 C13 117.4(10) . 5_547 ? O6 C13 C13 117.1(11) . 5_547 ? C14 O7 Tm1 117.1(6) . . ? C1 O1 Tm1 154.8(6) . 5_557 ? C1 O1 Tm1 86.5(6) . . ? Tm1 O1 Tm1 106.2(2) 5_557 . ? C1 O2 Tm1 97.1(6) . . ? O2 C1 O1 122.8(9) . . ? O2 C1 C2 118.6(9) . . ? O1 C1 C2 118.5(9) . . ? C3 C2 C6 117.6(10) . . ? C3 C2 C1 120.6(10) . . ? C6 C2 C1 121.7(10) . . ? C2 C3 C4 118.8(11) . . ? C2 C3 H3 120.6 . . ? C4 C3 H3 120.6 . . ? C7 N2 C12 116.4(10) . . ? C7 N2 Ag1 121.2(8) . . ? C12 N2 Ag1 121.4(8) . . ? N2 C7 C8 122.5(11) . . ? N2 C7 H7 118.8 . . ? C8 C7 H7 118.8 . . ? N2 C12 C11 124.8(12) . . ? N2 C12 H12 117.6 . . ? C11 C12 H12 117.6 . . ? C4 N1 C5 118.3(10) . . ? C4 N1 Ag1 118.3(8) . . ? C5 N1 Ag1 123.2(9) . . ? O7 C14 O8 127.1(10) . . ? O7 C14 C14 116.4(10) . 2_557 ? O8 C14 C14 116.4(11) . 2_557 ? C14 O8 Tm1 119.3(6) . 2_557 ? C12 C11 C9 119.2(11) . . ? C12 C11 H11 120.4 . . ? C9 C11 H11 120.4 . . ? N1 C4 C3 123.1(11) . . ? N1 C4 H4 118.4 . . ? C3 C4 H4 118.4 . . ? N1 C5 C6 122.9(12) . . ? N1 C5 H5 118.6 . . ? C6 C5 H5 118.6 . . ? C5 C6 C2 119.0(12) . . ? C5 C6 H6 120.5 . . ? C2 C6 H6 120.5 . . ? C8 C9 C11 117.2(10) . . ? C8 C9 C10 121.2(9) . . ? C11 C9 C10 121.6(9) . . ? C9 C8 C7 119.8(11) . . ? C9 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? O4 C10 O3 126.5(9) . . ? O4 C10 C9 117.1(9) . . ? O3 C10 C9 116.3(9) . . ? C10 O4 Tm1 139.7(6) . 8 ? C10 O3 Tm1 139.4(7) . 4_556 ? C13 O6 Tm1 117.6(6) . 5_547 ? H1W O1W H2W 107.0(18) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.19 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 3.264 _refine_diff_density_min -1.863 _refine_diff_density_rms 0.261 ######################################################################## data_8 #TrackingRef '- Cifs.txt' _database_code_depnum_ccdc_archive 'CCDC 727508' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H8 Ag N2 O8 Pr, H2 O' _chemical_formula_sum 'C14 H10 Ag N2 O9 Pr' _chemical_formula_weight 599.02 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pr Pr -0.2180 2.8214 '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 21.814(2) _cell_length_b 9.3193(8) _cell_length_c 17.3133(16) _cell_angle_alpha 90.00 _cell_angle_beta 108.9000(10) _cell_angle_gamma 90.00 _cell_volume 3329.8(5) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2621 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 27.03 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.390 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2288 _exptl_absorpt_coefficient_mu 4.122 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4507 _exptl_absorpt_correction_T_max 0.5080 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10230 _diffrn_reflns_av_R_equivalents 0.0366 _diffrn_reflns_av_sigmaI/netI 0.0467 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 28.19 _reflns_number_total 3911 _reflns_number_gt 3036 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0187P)^2^+12.7951P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3911 _refine_ls_number_parameters 252 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0491 _refine_ls_R_factor_gt 0.0328 _refine_ls_wR_factor_ref 0.0660 _refine_ls_wR_factor_gt 0.0599 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _refine_ls_shift/su_max 0.026 _refine_ls_shift/su_mean 0.002 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 Pr1 Pr 0.013335(12) 0.68501(3) 1.073498(15) 0.02114(7) Uani 1 1 d . . . Ag2 Ag 0.17288(2) 0.93339(6) 0.64002(3) 0.06422(17) Uani 1 1 d . . . O2 O 0.03654(17) 0.7199(3) 0.9438(2) 0.0354(8) Uani 1 1 d . . . N2 N 0.2330(2) 0.9534(5) 0.5616(3) 0.0437(12) Uani 1 1 d . . . C1 C 0.0391(2) 0.6474(5) 0.8842(3) 0.0259(10) Uani 1 1 d . . . C2 C 0.0750(2) 0.7150(5) 0.8321(3) 0.0231(10) Uani 1 1 d . . . C6 C 0.1028(3) 0.6311(6) 0.7867(3) 0.0389(13) Uani 1 1 d . . . H6 H 0.0995 0.5317 0.7875 0.047 Uiso 1 1 calc R . . C3 C 0.0814(3) 0.8613(5) 0.8277(4) 0.0465(15) Uani 1 1 d . . . H3 H 0.0640 0.9222 0.8578 0.056 Uiso 1 1 calc R . . C11 C 0.3274(3) 0.8817(6) 0.5324(4) 0.0457(15) Uani 1 1 d . . . H11 H 0.3617 0.8175 0.5421 0.055 Uiso 1 1 calc R . . C8 C 0.2661(3) 1.0714(8) 0.4602(4) 0.067(2) Uani 1 1 d . . . H8 H 0.2579 1.1412 0.4197 0.081 Uiso 1 1 calc R . . C12 C 0.2835(3) 0.8677(7) 0.5740(4) 0.0519(16) Uani 1 1 d . . . H12 H 0.2896 0.7947 0.6124 0.062 Uiso 1 1 calc R . . C7 C 0.2231(3) 1.0507(8) 0.5032(4) 0.072(2) Uani 1 1 d . . . H7 H 0.1860 1.1073 0.4906 0.087 Uiso 1 1 calc R . . N1 N 0.1400(2) 0.8372(5) 0.7342(3) 0.0415(11) Uani 1 1 d . . . C5 C 0.1353(3) 0.6955(6) 0.7408(3) 0.0408(13) Uani 1 1 d . . . H5 H 0.1552 0.6372 0.7124 0.049 Uiso 1 1 calc R . . C4 C 0.1135(3) 0.9162(6) 0.7785(4) 0.0592(19) Uani 1 1 d . . . H4 H 0.1170 1.0154 0.7760 0.071 Uiso 1 1 calc R . . C10 C 0.3739(2) 1.0220(5) 0.4429(3) 0.0270(10) Uani 1 1 d . . . C9 C 0.3206(2) 0.9887(5) 0.4776(3) 0.0298(11) Uani 1 1 d . . . O1 O 0.01644(16) 0.5248(3) 0.8646(2) 0.0330(8) Uani 1 1 d . . . O3 O 0.42595(14) 0.9513(3) 0.46775(19) 0.0294(7) Uani 1 1 d . . . O4 O 0.36679(16) 1.1236(4) 0.3936(2) 0.0378(9) Uani 1 1 d . . . O7 O -0.05787(15) 0.7679(3) 1.15447(19) 0.0300(8) Uani 1 1 d . . . C14 C -0.0364(2) 0.7490(5) 1.2303(3) 0.0245(10) Uani 1 1 d . . . O8 O -0.07005(15) 0.7317(3) 1.27666(19) 0.0284(7) Uani 1 1 d . . . O5 O -0.06059(15) 0.8738(3) 0.9928(2) 0.0294(7) Uani 1 1 d . . . O1W O 0.7963(2) 0.8035(6) 0.2568(3) 0.0690(13) Uani 1 1 d D . . C13 C -0.0356(2) 0.9844(5) 0.9752(3) 0.0258(10) Uani 1 1 d . . . O6 O -0.06326(15) 1.0736(3) 0.92023(19) 0.0295(7) Uani 1 1 d . . . H1W H 0.826(6) 0.751(13) 0.252(8) 0.37(11) Uiso 1 1 d D . . H2W H 0.788(4) 0.775(9) 0.298(3) 0.12(4) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pr1 0.02908(13) 0.01848(12) 0.02278(12) -0.00046(11) 0.01797(10) -0.00176(11) Ag2 0.0461(3) 0.1014(4) 0.0611(3) 0.0385(3) 0.0394(3) 0.0102(3) O2 0.059(2) 0.0280(19) 0.0329(19) 0.0006(15) 0.0335(18) -0.0027(16) N2 0.039(3) 0.060(3) 0.044(3) 0.016(2) 0.030(2) 0.004(2) C1 0.031(3) 0.027(3) 0.025(2) 0.0056(19) 0.017(2) 0.001(2) C2 0.031(2) 0.022(2) 0.021(2) 0.0006(18) 0.0149(19) -0.0047(19) C6 0.053(3) 0.027(3) 0.051(3) -0.009(2) 0.037(3) -0.013(2) C3 0.067(4) 0.023(3) 0.076(4) 0.004(3) 0.060(4) 0.004(3) C11 0.030(3) 0.052(3) 0.061(4) 0.026(3) 0.024(3) 0.010(3) C8 0.059(4) 0.089(5) 0.076(5) 0.059(4) 0.053(4) 0.040(4) C12 0.035(3) 0.067(4) 0.062(4) 0.034(3) 0.026(3) 0.008(3) C7 0.062(4) 0.089(5) 0.088(5) 0.050(4) 0.054(4) 0.039(4) N1 0.047(3) 0.039(3) 0.051(3) 0.015(2) 0.034(2) 0.004(2) C5 0.052(3) 0.045(3) 0.040(3) -0.009(3) 0.034(3) -0.006(3) C4 0.088(5) 0.029(3) 0.095(5) 0.017(3) 0.076(4) 0.010(3) C10 0.031(3) 0.028(3) 0.026(2) -0.003(2) 0.016(2) -0.002(2) C9 0.026(2) 0.035(3) 0.033(3) 0.006(2) 0.015(2) 0.001(2) O1 0.047(2) 0.0263(19) 0.0333(19) 0.0000(15) 0.0241(16) -0.0102(16) O3 0.0256(17) 0.0302(18) 0.0372(19) -0.0025(15) 0.0167(15) -0.0008(15) O4 0.0330(19) 0.047(2) 0.039(2) 0.0150(17) 0.0196(17) 0.0037(16) O7 0.0339(18) 0.0361(19) 0.0249(17) 0.0015(14) 0.0165(15) 0.0060(15) C14 0.037(3) 0.015(2) 0.027(3) -0.0025(18) 0.017(2) 0.0028(19) O8 0.0306(17) 0.0328(19) 0.0304(18) -0.0001(14) 0.0216(15) 0.0020(14) O5 0.0300(18) 0.0247(17) 0.0373(19) 0.0068(15) 0.0162(16) -0.0041(14) O1W 0.056(3) 0.082(4) 0.070(3) 0.017(3) 0.022(3) 0.006(3) C13 0.035(3) 0.022(2) 0.025(2) -0.0056(19) 0.016(2) -0.003(2) O6 0.0342(18) 0.0222(17) 0.0304(18) 0.0028(14) 0.0082(15) -0.0039(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pr1 O1 2.417(3) 5_567 ? Pr1 O2 2.478(3) . ? Pr1 O6 2.486(3) 5_577 ? Pr1 O5 2.488(3) . ? Pr1 O3 2.518(3) 8_466 ? Pr1 O8 2.524(3) 2_557 ? Pr1 O7 2.527(3) . ? Pr1 O4 2.555(3) 4_546 ? Pr1 O3 2.760(3) 4_546 ? Pr1 C10 2.983(5) 4_546 ? Ag2 N2 2.179(4) . ? Ag2 N1 2.176(4) . ? O2 C1 1.250(5) . ? N2 C7 1.322(7) . ? N2 C12 1.321(7) . ? C1 O1 1.248(5) . ? C1 C2 1.509(6) . ? C2 C3 1.376(6) . ? C2 C6 1.380(6) . ? C6 C5 1.363(7) . ? C6 H6 0.9300 . ? C3 C4 1.366(7) . ? C3 H3 0.9300 . ? C11 C9 1.352(7) . ? C11 C12 1.378(7) . ? C11 H11 0.9300 . ? C8 C9 1.365(7) . ? C8 C7 1.389(8) . ? C8 H8 0.9300 . ? C12 H12 0.9300 . ? C7 H7 0.9300 . ? N1 C4 1.323(7) . ? N1 C5 1.332(6) . ? C5 H5 0.9300 . ? C4 H4 0.9300 . ? C10 O4 1.250(5) . ? C10 O3 1.262(5) . ? C10 C9 1.503(6) . ? C10 Pr1 2.983(5) 4_556 ? O1 Pr1 2.417(3) 5_567 ? O3 Pr1 2.518(3) 8_565 ? O3 Pr1 2.760(3) 4_556 ? O4 Pr1 2.555(3) 4_556 ? O7 C14 1.256(5) . ? C14 O8 1.262(5) . ? C14 C14 1.510(9) 2_557 ? O8 Pr1 2.524(3) 2_557 ? O5 C13 1.250(5) . ? O1W H1W 0.84(13) . ? O1W H2W 0.839(10) . ? C13 O6 1.260(5) . ? C13 C13 1.538(9) 5_577 ? O6 Pr1 2.486(3) 5_577 ? 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 Pr1 O2 132.15(11) 5_567 . ? O1 Pr1 O6 152.76(11) 5_567 5_577 ? O2 Pr1 O6 72.88(11) . 5_577 ? O1 Pr1 O5 127.06(11) 5_567 . ? O2 Pr1 O5 71.55(11) . . ? O6 Pr1 O5 65.15(10) 5_577 . ? O1 Pr1 O3 70.46(11) 5_567 8_466 ? O2 Pr1 O3 74.70(11) . 8_466 ? O6 Pr1 O3 134.92(10) 5_577 8_466 ? O5 Pr1 O3 75.40(11) . 8_466 ? O1 Pr1 O8 78.24(10) 5_567 2_557 ? O2 Pr1 O8 137.12(11) . 2_557 ? O6 Pr1 O8 74.77(10) 5_577 2_557 ? O5 Pr1 O8 117.93(11) . 2_557 ? O3 Pr1 O8 146.92(10) 8_466 2_557 ? O1 Pr1 O7 72.51(11) 5_567 . ? O2 Pr1 O7 143.63(11) . . ? O6 Pr1 O7 92.20(11) 5_577 . ? O5 Pr1 O7 72.09(10) . . ? O3 Pr1 O7 95.80(10) 8_466 . ? O8 Pr1 O7 64.01(10) 2_557 . ? O1 Pr1 O4 97.04(12) 5_567 4_546 ? O2 Pr1 O4 74.73(12) . 4_546 ? O6 Pr1 O4 77.92(11) 5_577 4_546 ? O5 Pr1 O4 135.58(11) . 4_546 ? O3 Pr1 O4 121.88(10) 8_466 4_546 ? O8 Pr1 O4 71.58(10) 2_557 4_546 ? O7 Pr1 O4 135.54(11) . 4_546 ? O1 Pr1 O3 72.37(10) 5_567 4_546 ? O2 Pr1 O3 67.25(10) . 4_546 ? O6 Pr1 O3 119.01(10) 5_577 4_546 ? O5 Pr1 O3 133.67(10) . 4_546 ? O3 Pr1 O3 74.18(10) 8_466 4_546 ? O8 Pr1 O3 106.58(10) 2_557 4_546 ? O7 Pr1 O3 144.83(10) . 4_546 ? O4 Pr1 O3 48.59(10) 4_546 4_546 ? O1 Pr1 C10 88.79(12) 5_567 4_546 ? O2 Pr1 C10 64.12(12) . 4_546 ? O6 Pr1 C10 95.83(12) 5_577 4_546 ? O5 Pr1 C10 135.33(11) . 4_546 ? O3 Pr1 C10 97.31(12) 8_466 4_546 ? O8 Pr1 C10 92.35(11) 2_557 4_546 ? O7 Pr1 C10 152.00(11) . 4_546 ? O4 Pr1 C10 24.57(11) 4_546 4_546 ? O3 Pr1 C10 25.01(11) 4_546 4_546 ? N2 Ag2 N1 155.89(17) . . ? C1 O2 Pr1 139.0(3) . . ? C7 N2 C12 117.4(5) . . ? C7 N2 Ag2 123.5(4) . . ? C12 N2 Ag2 119.0(4) . . ? O2 C1 O1 126.8(4) . . ? O2 C1 C2 116.0(4) . . ? O1 C1 C2 117.1(4) . . ? C3 C2 C6 117.3(4) . . ? C3 C2 C1 121.9(4) . . ? C6 C2 C1 120.8(4) . . ? C5 C6 C2 119.4(5) . . ? C5 C6 H6 120.3 . . ? C2 C6 H6 120.3 . . ? C4 C3 C2 119.2(5) . . ? C4 C3 H3 120.4 . . ? C2 C3 H3 120.4 . . ? C9 C11 C12 120.0(5) . . ? C9 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? C9 C8 C7 119.7(5) . . ? C9 C8 H8 120.2 . . ? C7 C8 H8 120.2 . . ? N2 C12 C11 122.8(5) . . ? N2 C12 H12 118.6 . . ? C11 C12 H12 118.6 . . ? N2 C7 C8 122.2(5) . . ? N2 C7 H7 118.9 . . ? C8 C7 H7 118.9 . . ? C4 N1 C5 116.2(4) . . ? C4 N1 Ag2 121.1(4) . . ? C5 N1 Ag2 121.7(3) . . ? N1 C5 C6 123.8(5) . . ? N1 C5 H5 118.1 . . ? C6 C5 H5 118.1 . . ? N1 C4 C3 124.2(5) . . ? N1 C4 H4 117.9 . . ? C3 C4 H4 117.9 . . ? O4 C10 O3 121.7(4) . . ? O4 C10 C9 119.2(4) . . ? O3 C10 C9 118.9(4) . . ? O4 C10 Pr1 58.2(2) . 4_556 ? O3 C10 Pr1 67.6(2) . 4_556 ? C9 C10 Pr1 155.8(3) . 4_556 ? C11 C9 C8 117.4(5) . . ? C11 C9 C10 120.6(4) . . ? C8 C9 C10 121.7(4) . . ? C1 O1 Pr1 139.4(3) . 5_567 ? C10 O3 Pr1 153.8(3) . 8_565 ? C10 O3 Pr1 87.4(3) . 4_556 ? Pr1 O3 Pr1 105.82(10) 8_565 4_556 ? C10 O4 Pr1 97.3(3) . 4_556 ? C14 O7 Pr1 116.7(3) . . ? O7 C14 O8 125.9(4) . . ? O7 C14 C14 117.0(5) . 2_557 ? O8 C14 C14 117.2(5) . 2_557 ? C14 O8 Pr1 118.9(3) . 2_557 ? C13 O5 Pr1 117.8(3) . . ? H1W O1W H2W 107.1(18) . . ? O5 C13 O6 126.0(4) . . ? O5 C13 C13 117.4(5) . 5_577 ? O6 C13 C13 116.6(5) . 5_577 ? C13 O6 Pr1 117.9(3) . 5_577 ? _diffrn_measured_fraction_theta_max 0.951 _diffrn_reflns_theta_full 28.19 _diffrn_measured_fraction_theta_full 0.951 _refine_diff_density_max 1.331 _refine_diff_density_min -1.117 _refine_diff_density_rms 0.139 ################################################################## data_2 _database_code_depnum_ccdc_archive 'CCDC 804308' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H32 Cu6 Eu2 I5 N6 Na O20, 0.5(H4 O2)' _chemical_formula_sum 'C38 H34 Cu6 Eu2 I5 N6 Na O21' _chemical_formula_weight 2253.36 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 '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 '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.1322(15) _cell_length_b 11.260(3) _cell_length_c 18.161(4) _cell_angle_alpha 86.072(3) _cell_angle_beta 79.964(3) _cell_angle_gamma 72.880(2) _cell_volume 1372.3(6) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2183 _cell_measurement_theta_min 2.62 _cell_measurement_theta_max 27.99 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.727 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1048 _exptl_absorpt_coefficient_mu 7.426 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.259 _exptl_absorpt_correction_T_max 0.298 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II area-detector diffractometer' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7187 _diffrn_reflns_av_R_equivalents 0.0489 _diffrn_reflns_av_sigmaI/netI 0.1072 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 25.20 _reflns_number_total 4881 _reflns_number_gt 3146 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0469P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4881 _refine_ls_number_parameters 386 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0925 _refine_ls_R_factor_gt 0.0558 _refine_ls_wR_factor_ref 0.1290 _refine_ls_wR_factor_gt 0.1107 _refine_ls_goodness_of_fit_ref 0.972 _refine_ls_restrained_S_all 0.971 _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 0.6236(18) 0.6508(13) 0.3777(7) 0.029(3) Uani 1 1 d . . . C2 C 0.6098(17) 0.6211(12) 0.3009(7) 0.027(3) Uani 1 1 d . . . C3 C 0.6808(19) 0.5000(12) 0.2746(7) 0.036(4) Uani 1 1 d . . . H3 H 0.7341 0.4352 0.3064 0.044 Uiso 1 1 calc R . . C4 C 0.674(2) 0.4750(11) 0.2034(7) 0.038(4) Uani 1 1 d . . . H4 H 0.7267 0.3933 0.1877 0.045 Uiso 1 1 calc R . . C5 C 0.5273(19) 0.6790(12) 0.1785(7) 0.030(3) Uani 1 1 d . . . H5 H 0.4765 0.7418 0.1452 0.036 Uiso 1 1 calc R . . C6 C 0.5306(18) 0.7105(13) 0.2506(7) 0.030(3) Uani 1 1 d . . . H6 H 0.4789 0.7929 0.2650 0.036 Uiso 1 1 calc R . . C7 C 0.832(2) 0.7868(11) 0.6475(7) 0.029(3) Uani 1 1 d . . . C8 C 0.891(2) 0.8208(12) 0.7189(7) 0.032(3) Uani 1 1 d . . . C9 C 1.062(2) 0.8499(14) 0.7178(8) 0.042(4) Uani 1 1 d . . . H9 H 1.1493 0.8507 0.6733 0.050 Uiso 1 1 calc R . . C10 C 1.104(2) 0.8784(15) 0.7850(8) 0.048(4) Uani 1 1 d . . . H10 H 1.2206 0.8995 0.7842 0.057 Uiso 1 1 calc R . . C11 C 0.821(2) 0.8434(16) 0.8508(8) 0.055(5) Uani 1 1 d . . . H11 H 0.7418 0.8358 0.8962 0.066 Uiso 1 1 calc R . . C12 C 0.766(2) 0.8193(13) 0.7856(7) 0.039(4) Uani 1 1 d . . . H12 H 0.6452 0.8023 0.7867 0.047 Uiso 1 1 calc R . . C13 C 0.8952(18) 0.4211(11) 0.6021(7) 0.025(3) Uani 1 1 d . . . C14 C 0.9018(17) 0.3931(11) 0.6826(6) 0.021(3) Uani 1 1 d . . . C15 C 0.8295(17) 0.4838(11) 0.7361(7) 0.025(3) Uani 1 1 d . . . H15 H 0.7689 0.5655 0.7226 0.030 Uiso 1 1 calc R . . C16 C 0.8479(19) 0.4528(12) 0.8095(7) 0.033(3) Uani 1 1 d . . . H16 H 0.8015 0.5161 0.8442 0.039 Uiso 1 1 calc R . . C17 C 0.9958(18) 0.2505(12) 0.7827(7) 0.032(3) Uani 1 1 d . . . H17 H 1.0523 0.1693 0.7982 0.038 Uiso 1 1 calc R . . C18 C 0.9877(18) 0.2726(10) 0.7074(6) 0.025(3) Uani 1 1 d . . . H18 H 1.0390 0.2080 0.6737 0.029 Uiso 1 1 calc R . . C19 C 0.3985(17) 0.9945(11) 0.5182(7) 0.023(3) Uani 1 1 d . . . N1 N 0.5948(15) 0.5608(10) 0.1549(6) 0.030(3) Uani 1 1 d . . . N2 N 0.9876(19) 0.8775(11) 0.8503(6) 0.043(3) Uani 1 1 d . . . N3 N 0.9278(16) 0.3377(10) 0.8343(5) 0.030(3) Uani 1 1 d . . . O1 O 0.5746(13) 0.7628(7) 0.3956(4) 0.028(2) Uani 1 1 d . . . O2 O 0.6937(13) 0.5651(8) 0.4219(5) 0.031(2) Uani 1 1 d . . . O3 O 0.6562(14) 0.7857(9) 0.6492(5) 0.041(2) Uani 1 1 d . . . O4 O 0.9633(14) 0.7621(9) 0.5898(5) 0.047(3) Uani 1 1 d . . . O5 O 0.7938(13) 0.5275(7) 0.5853(4) 0.031(2) Uani 1 1 d . . . O6 O 0.9919(12) 0.3391(8) 0.5555(5) 0.031(2) Uani 1 1 d . . . O7 O 0.3873(12) 0.8886(7) 0.5407(5) 0.029(2) Uani 1 1 d . . . O8 O 0.2529(11) 1.0864(7) 0.5187(5) 0.024(2) Uani 1 1 d . . . O9 O 0.3864(12) 0.6559(8) 0.5555(6) 0.035(2) Uani 1 1 d D . . H9A H 0.271(7) 0.692(9) 0.549(8) 0.053 Uiso 1 1 d D . . H9B H 0.401(16) 0.581(3) 0.561(8) 0.053 Uiso 1 1 d D . . O10 O 0.172(2) 0.8931(14) 0.4028(7) 0.080(4) Uani 1 1 d D . . H10A H 0.09(2) 0.878(17) 0.382(8) 0.120 Uiso 1 1 d D . . H10B H 0.24(3) 0.932(19) 0.375(8) 0.120 Uiso 1 1 d D . . O11 O 0.600(4) 0.9784(19) 0.2991(11) 0.059(6) Uani 0.50 1 d PD . . H11A H 0.60(5) 1.045(15) 0.316(14) 0.089 Uiso 0.50 1 d PD . . H11B H 0.59(6) 0.93(2) 0.333(11) 0.089 Uiso 0.50 1 d PD . . I3 I 1.23556(14) 0.08747(8) 0.94392(5) 0.0364(3) Uani 1 1 d . . . Cu3 Cu 0.9403(3) 0.29354(19) 0.94328(10) 0.0517(6) Uani 1 1 d . . . Cu2 Cu 1.0522(3) 0.9184(2) 0.94695(11) 0.0618(6) Uani 1 1 d . . . Cu1 Cu 0.6081(3) 0.52008(17) 0.04794(9) 0.0427(5) Uani 1 1 d . . . Na1 Na -0.022(2) 1.0409(11) 0.4898(8) 0.049(4) Uani 0.50 1 d P . . I2 I 1.0000 0.5000 1.0000 0.0457(4) Uani 1 2 d S . . I1 I 0.59572(13) 0.29357(8) 0.02846(5) 0.0335(2) Uani 1 1 d . . . Eu3 Eu 0.69374(9) 0.71402(6) 0.52114(3) 0.02095(18) 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 0.017(7) 0.038(8) 0.033(8) -0.005(7) -0.007(6) -0.008(6) C2 0.013(6) 0.041(8) 0.023(7) -0.014(6) -0.003(5) 0.003(6) C3 0.040(9) 0.017(7) 0.042(9) -0.006(6) -0.016(7) 0.012(6) C4 0.059(10) 0.012(7) 0.036(8) -0.006(6) -0.024(7) 0.009(6) C5 0.032(8) 0.033(8) 0.030(8) 0.005(6) -0.016(6) -0.009(6) C6 0.025(7) 0.036(8) 0.029(7) 0.003(6) -0.010(6) -0.006(6) C7 0.037(9) 0.023(7) 0.030(8) -0.006(6) -0.008(7) -0.011(6) C8 0.032(8) 0.035(8) 0.032(8) -0.009(6) -0.007(7) -0.009(6) C9 0.041(9) 0.059(10) 0.030(8) -0.003(7) -0.015(7) -0.016(8) C10 0.020(8) 0.075(12) 0.051(10) -0.012(9) -0.014(7) -0.011(8) C11 0.058(11) 0.090(13) 0.027(8) -0.030(9) 0.001(8) -0.034(10) C12 0.030(8) 0.059(10) 0.032(8) -0.012(7) 0.003(7) -0.020(7) C13 0.024(7) 0.018(7) 0.028(7) 0.006(6) -0.012(6) 0.004(6) C14 0.019(7) 0.029(7) 0.021(7) 0.003(6) -0.012(5) -0.011(6) C15 0.026(7) 0.023(7) 0.031(7) 0.005(6) -0.009(6) -0.014(6) C16 0.032(8) 0.032(8) 0.032(8) -0.007(7) -0.002(6) -0.005(6) C17 0.024(7) 0.031(8) 0.039(8) 0.009(7) -0.011(6) -0.004(6) C18 0.035(8) 0.008(6) 0.021(7) -0.004(5) 0.002(6) 0.005(5) C19 0.016(6) 0.020(7) 0.036(8) -0.015(6) -0.006(6) -0.004(6) N1 0.032(6) 0.030(7) 0.030(6) 0.003(5) -0.006(5) -0.013(5) N2 0.056(8) 0.056(8) 0.032(7) -0.007(6) -0.003(6) -0.040(7) N3 0.037(7) 0.039(7) 0.015(6) -0.003(5) -0.005(5) -0.013(6) O1 0.040(5) 0.015(5) 0.028(5) -0.006(4) -0.004(4) -0.003(4) O2 0.050(6) 0.023(5) 0.024(5) -0.006(4) -0.011(4) -0.013(4) O3 0.044(6) 0.045(6) 0.038(6) -0.011(5) -0.005(5) -0.018(5) O4 0.042(6) 0.064(7) 0.028(5) -0.022(5) -0.004(5) -0.001(5) O5 0.047(6) 0.020(5) 0.020(5) 0.004(4) -0.008(4) 0.003(4) O6 0.025(5) 0.031(5) 0.032(5) -0.009(4) -0.003(4) -0.001(4) O7 0.030(5) 0.022(5) 0.041(6) -0.009(4) -0.011(4) -0.011(4) O8 0.013(4) 0.014(4) 0.044(5) 0.000(4) -0.006(4) -0.002(4) O9 0.019(5) 0.023(5) 0.065(7) 0.008(5) -0.008(5) -0.009(4) O10 0.059(9) 0.103(12) 0.084(9) -0.043(8) -0.045(8) -0.003(7) O11 0.089(18) 0.029(12) 0.050(13) -0.009(11) 0.002(14) -0.007(13) I3 0.0409(6) 0.0341(5) 0.0358(5) 0.0021(4) -0.0095(4) -0.0119(4) Cu3 0.0604(14) 0.0625(14) 0.0290(10) 0.0059(10) -0.0105(9) -0.0123(11) Cu2 0.0698(15) 0.0979(18) 0.0359(11) -0.0224(12) -0.0051(10) -0.0495(13) Cu1 0.0532(12) 0.0485(12) 0.0294(10) -0.0068(9) -0.0130(9) -0.0143(10) Na1 0.039(8) 0.063(11) 0.059(9) 0.018(8) -0.011(6) -0.038(9) I2 0.0307(8) 0.0542(9) 0.0552(9) -0.0276(8) 0.0014(7) -0.0155(7) I1 0.0343(5) 0.0288(5) 0.0381(5) 0.0009(4) -0.0071(4) -0.0094(4) Eu3 0.0253(4) 0.0158(3) 0.0217(3) -0.0013(3) -0.0069(3) -0.0038(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 O1 1.255(15) . ? C1 O2 1.256(14) . ? C1 C2 1.481(17) . ? C2 C6 1.374(16) . ? C2 C3 1.394(16) . ? C3 C4 1.354(17) . ? C3 H3 0.9300 . ? C4 N1 1.327(15) . ? C4 H4 0.9300 . ? C5 N1 1.347(15) . ? C5 C6 1.385(17) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 O3 1.253(15) . ? C7 O4 1.264(15) . ? C7 C8 1.535(17) . ? C8 C9 1.353(18) . ? C8 C12 1.374(17) . ? C9 C10 1.384(18) . ? C9 H9 0.9300 . ? C10 N2 1.323(17) . ? C10 H10 0.9300 . ? C11 N2 1.350(18) . ? C11 C12 1.380(18) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 O5 1.252(13) . ? C13 O6 1.255(14) . ? C13 C14 1.480(16) . ? C14 C15 1.381(16) . ? C14 C18 1.394(15) . ? C15 C16 1.373(16) . ? C15 H15 0.9300 . ? C16 N3 1.334(15) . ? C16 H16 0.9300 . ? C17 N3 1.329(16) . ? C17 C18 1.380(17) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 O8 1.231(13) . ? C19 O7 1.254(13) . ? C19 C19 1.52(2) 2_676 ? C19 Na1 2.855(17) 2_576 ? C19 Eu3 3.207(12) 2_676 ? N1 Cu1 2.006(11) . ? N2 Cu2 2.006(12) . ? N3 Cu3 2.019(10) . ? O1 Eu3 2.540(8) . ? O2 Eu3 2.545(8) . ? O3 Eu3 2.459(9) . ? O4 Na1 2.661(15) 2_676 ? O4 Eu3 2.662(10) . ? O5 Eu3 2.313(8) . ? O6 Eu3 2.357(8) 2_766 ? O7 Eu3 2.462(8) . ? O7 Na1 2.635(15) 2_576 ? O8 Na1 2.319(16) . ? O8 Eu3 2.430(8) 2_676 ? O8 Na1 2.507(15) 2_576 ? O9 Eu3 2.436(8) . ? O9 H9A 0.83(7) . ? O9 H9B 0.82(5) . ? O10 Na1 2.12(2) 2_576 ? O10 Na1 2.33(2) . ? O10 H10A 0.81(14) . ? O10 H10B 0.8(2) . ? O11 H11A 0.82(2) . ? O11 H11B 0.82(2) . ? I3 Cu2 2.601(2) 1_545 ? I3 Cu2 2.605(2) 2_767 ? I3 Cu3 2.636(2) . ? Cu3 I1 2.666(2) 1_556 ? Cu3 I2 2.777(2) . ? Cu3 Cu2 2.997(3) 2_767 ? Cu2 I3 2.601(2) 1_565 ? Cu2 I3 2.605(2) 2_767 ? Cu2 Cu2 2.612(4) 2_777 ? Cu2 I1 2.987(3) 2_766 ? Cu2 Cu3 2.997(3) 2_767 ? Cu1 I1 2.628(2) . ? Cu1 I1 2.636(2) 2_665 ? Cu1 Cu1 2.659(4) 2_665 ? Cu1 I2 2.726(2) 1_554 ? Na1 Na1 0.95(2) 2_576 ? Na1 O10 2.12(2) 2_576 ? Na1 O8 2.507(15) 2_576 ? Na1 O7 2.635(15) 2_576 ? Na1 O4 2.661(15) 2_676 ? Na1 C19 2.855(17) 2_576 ? Na1 Eu3 4.089(12) 2_676 ? Na1 H10A 2.64(17) . ? Na1 H10B 2.6(2) . ? I2 Cu1 2.726(2) 1_556 ? I2 Cu1 2.726(2) 2_766 ? I2 Cu3 2.777(2) 2_767 ? I1 Cu1 2.636(2) 2_665 ? I1 Cu3 2.666(2) 1_554 ? I1 Cu2 2.987(3) 2_766 ? Eu3 O6 2.357(8) 2_766 ? Eu3 O8 2.430(8) 2_676 ? Eu3 C19 3.207(12) 2_676 ? Eu3 Na1 4.089(12) 2_676 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 O2 121.3(12) . . ? O1 C1 C2 118.7(12) . . ? O2 C1 C2 119.9(12) . . ? C6 C2 C3 115.5(12) . . ? C6 C2 C1 122.6(12) . . ? C3 C2 C1 121.9(12) . . ? C4 C3 C2 121.1(12) . . ? C4 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? N1 C4 C3 123.6(12) . . ? N1 C4 H4 118.2 . . ? C3 C4 H4 118.2 . . ? N1 C5 C6 122.5(12) . . ? N1 C5 H5 118.8 . . ? C6 C5 H5 118.8 . . ? C2 C6 C5 120.7(13) . . ? C2 C6 H6 119.7 . . ? C5 C6 H6 119.7 . . ? O3 C7 O4 123.3(12) . . ? O3 C7 C8 118.3(12) . . ? O4 C7 C8 118.3(12) . . ? C9 C8 C12 119.8(13) . . ? C9 C8 C7 121.7(12) . . ? C12 C8 C7 118.4(12) . . ? C8 C9 C10 117.7(14) . . ? C8 C9 H9 121.1 . . ? C10 C9 H9 121.1 . . ? N2 C10 C9 124.2(14) . . ? N2 C10 H10 117.9 . . ? C9 C10 H10 117.9 . . ? N2 C11 C12 121.7(14) . . ? N2 C11 H11 119.2 . . ? C12 C11 H11 119.2 . . ? C8 C12 C11 119.1(13) . . ? C8 C12 H12 120.4 . . ? C11 C12 H12 120.4 . . ? O5 C13 O6 124.3(11) . . ? O5 C13 C14 116.8(11) . . ? O6 C13 C14 118.9(10) . . ? C15 C14 C18 116.8(11) . . ? C15 C14 C13 122.4(11) . . ? C18 C14 C13 120.7(11) . . ? C16 C15 C14 119.6(12) . . ? C16 C15 H15 120.2 . . ? C14 C15 H15 120.2 . . ? N3 C16 C15 124.3(12) . . ? N3 C16 H16 117.8 . . ? C15 C16 H16 117.8 . . ? N3 C17 C18 124.1(12) . . ? N3 C17 H17 117.9 . . ? C18 C17 H17 117.9 . . ? C17 C18 C14 119.2(11) . . ? C17 C18 H18 120.4 . . ? C14 C18 H18 120.4 . . ? O8 C19 O7 123.5(11) . . ? O8 C19 C19 118.9(14) . 2_676 ? O7 C19 C19 117.3(13) . 2_676 ? O8 C19 Na1 61.3(6) . 2_576 ? O7 C19 Na1 67.1(6) . 2_576 ? C19 C19 Na1 151.6(12) 2_676 2_576 ? O7 C19 Eu3 165.0(8) . 2_676 ? C19 C19 Eu3 77.6(9) 2_676 2_676 ? Na1 C19 Eu3 100.2(4) 2_576 2_676 ? C4 N1 C5 116.6(11) . . ? C4 N1 Cu1 121.5(9) . . ? C5 N1 Cu1 121.4(8) . . ? C10 N2 C11 117.2(13) . . ? C10 N2 Cu2 123.4(10) . . ? C11 N2 Cu2 119.4(10) . . ? C17 N3 C16 115.9(11) . . ? C17 N3 Cu3 120.7(9) . . ? C16 N3 Cu3 123.4(9) . . ? C1 O1 Eu3 93.9(7) . . ? C1 O2 Eu3 93.7(7) . . ? C7 O3 Eu3 97.6(8) . . ? C7 O4 Na1 115.1(9) . 2_676 ? C7 O4 Eu3 87.9(8) . . ? Na1 O4 Eu3 100.4(4) 2_676 . ? C13 O5 Eu3 160.7(8) . . ? C13 O6 Eu3 137.2(9) . 2_766 ? C19 O7 Eu3 117.7(7) . . ? C19 O7 Na1 86.8(7) . 2_576 ? Eu3 O7 Na1 140.8(5) . 2_576 ? C19 O8 Na1 113.0(8) . . ? C19 O8 Eu3 118.6(7) . 2_676 ? Na1 O8 Eu3 118.8(4) . 2_676 ? C19 O8 Na1 93.2(7) . 2_576 ? Eu3 O8 Na1 141.1(4) 2_676 2_576 ? Eu3 O9 H9A 132(8) . . ? Eu3 O9 H9B 115(8) . . ? H9A O9 H9B 110(10) . . ? Na1 O10 H10A 107(10) 2_576 . ? Na1 O10 H10A 103(10) . . ? Na1 O10 H10B 122(10) 2_576 . ? Na1 O10 H10B 103(10) . . ? H10A O10 H10B 112(17) . . ? H11A O11 H11B 110(4) . . ? Cu2 I3 Cu2 60.22(8) 1_545 2_767 ? Cu2 I3 Cu3 101.64(8) 1_545 . ? Cu2 I3 Cu3 69.75(7) 2_767 . ? N3 Cu3 I3 105.3(3) . . ? N3 Cu3 I1 115.6(3) . 1_556 ? I3 Cu3 I1 116.75(8) . 1_556 ? N3 Cu3 I2 104.1(3) . . ? I3 Cu3 I2 115.21(8) . . ? I1 Cu3 I2 99.44(7) 1_556 . ? N3 Cu3 Cu2 141.4(3) . 2_767 ? I3 Cu3 Cu2 54.65(6) . 2_767 ? I1 Cu3 Cu2 63.34(6) 1_556 2_767 ? I2 Cu3 Cu2 114.32(7) . 2_767 ? N2 Cu2 I3 117.9(3) . 1_565 ? N2 Cu2 I3 110.2(4) . 2_767 ? I3 Cu2 I3 119.78(8) 1_565 2_767 ? N2 Cu2 Cu2 144.1(4) . 2_777 ? I3 Cu2 Cu2 59.97(8) 1_565 2_777 ? I3 Cu2 Cu2 59.80(8) 2_767 2_777 ? N2 Cu2 I1 103.4(4) . 2_766 ? I3 Cu2 I1 94.80(7) 1_565 2_766 ? I3 Cu2 I1 107.47(8) 2_767 2_766 ? Cu2 Cu2 I1 112.51(12) 2_777 2_766 ? N2 Cu2 Cu3 110.1(4) . 2_767 ? I3 Cu2 Cu3 127.53(9) 1_565 2_767 ? I3 Cu2 Cu3 55.60(6) 2_767 2_767 ? Cu2 Cu2 Cu3 92.47(11) 2_777 2_767 ? I1 Cu2 Cu3 52.91(6) 2_766 2_767 ? N1 Cu1 I1 114.2(3) . . ? N1 Cu1 I1 113.2(3) . 2_665 ? I1 Cu1 I1 119.33(7) . 2_665 ? N1 Cu1 Cu1 142.8(3) . 2_665 ? I1 Cu1 Cu1 59.82(7) . 2_665 ? I1 Cu1 Cu1 59.50(7) 2_665 2_665 ? N1 Cu1 I2 98.1(3) . 1_554 ? I1 Cu1 I2 101.73(6) . 1_554 ? I1 Cu1 I2 106.70(7) 2_665 1_554 ? Cu1 Cu1 I2 119.07(10) 2_665 1_554 ? Na1 Na1 O10 90.2(19) 2_576 2_576 ? Na1 Na1 O8 90.0(16) 2_576 . ? O10 Na1 O8 87.3(7) 2_576 . ? Na1 Na1 O10 65.6(18) 2_576 . ? O10 Na1 O10 155.8(5) 2_576 . ? O8 Na1 O10 92.5(6) . . ? Na1 Na1 O8 67.7(15) 2_576 2_576 ? O10 Na1 O8 92.6(6) 2_576 2_576 ? O8 Na1 O8 157.7(5) . 2_576 ? O10 Na1 O8 78.6(6) . 2_576 ? Na1 Na1 O7 116.7(17) 2_576 2_576 ? O10 Na1 O7 82.1(6) 2_576 2_576 ? O8 Na1 O7 151.1(6) . 2_576 ? O10 Na1 O7 108.0(6) . 2_576 ? O8 Na1 O7 50.3(3) 2_576 2_576 ? Na1 Na1 O4 153(2) 2_576 2_676 ? O10 Na1 O4 106.4(7) 2_576 2_676 ? O8 Na1 O4 69.9(4) . 2_676 ? O10 Na1 O4 96.1(6) . 2_676 ? O8 Na1 O4 131.0(6) 2_576 2_676 ? O7 Na1 O4 87.4(4) 2_576 2_676 ? Na1 Na1 C19 90.7(16) 2_576 2_576 ? O10 Na1 C19 81.6(6) 2_576 2_576 ? O8 Na1 C19 168.8(8) . 2_576 ? O10 Na1 C19 97.9(6) . 2_576 ? O8 Na1 C19 25.5(3) 2_576 2_576 ? O7 Na1 C19 26.0(3) 2_576 2_576 ? O4 Na1 C19 112.6(5) 2_676 2_576 ? Na1 Na1 Eu3 121.3(17) 2_576 2_676 ? O10 Na1 Eu3 90.1(6) 2_576 2_676 ? O8 Na1 Eu3 31.4(2) . 2_676 ? O10 Na1 Eu3 102.2(6) . 2_676 ? O8 Na1 Eu3 170.7(4) 2_576 2_676 ? O7 Na1 Eu3 121.4(4) 2_576 2_676 ? O4 Na1 Eu3 39.8(3) 2_676 2_676 ? C19 Na1 Eu3 147.1(4) 2_576 2_676 ? Na1 Na1 H10A 70(4) 2_576 . ? O10 Na1 H10A 153(4) 2_576 . ? O8 Na1 H10A 110(2) . . ? O10 Na1 H10A 18(2) . . ? O8 Na1 H10A 64(3) 2_576 . ? O7 Na1 H10A 91(2) 2_576 . ? O4 Na1 H10A 99(4) 2_676 . ? C19 Na1 H10A 81(2) 2_576 . ? Eu3 Na1 H10A 115(3) 2_676 . ? Na1 Na1 H10B 80(4) 2_576 . ? O10 Na1 H10B 166(4) 2_576 . ? O8 Na1 H10B 82(3) . . ? O10 Na1 H10B 18(3) . . ? O8 Na1 H10B 93(3) 2_576 . ? O7 Na1 H10B 112(4) 2_576 . ? O4 Na1 H10B 79(3) 2_676 . ? C19 Na1 H10B 109(3) 2_576 . ? Eu3 Na1 H10B 86(2) 2_676 . ? H10A Na1 H10B 29.6(13) . . ? Cu1 I2 Cu1 180.000(1) 1_556 2_766 ? Cu1 I2 Cu3 75.18(6) 1_556 . ? Cu1 I2 Cu3 104.82(6) 2_766 . ? Cu1 I2 Cu3 104.82(6) 1_556 2_767 ? Cu1 I2 Cu3 75.18(6) 2_766 2_767 ? Cu3 I2 Cu3 180.000(1) . 2_767 ? Cu1 I1 Cu1 60.67(7) . 2_665 ? Cu1 I1 Cu3 78.71(7) . 1_554 ? Cu1 I1 Cu3 92.72(6) 2_665 1_554 ? Cu1 I1 Cu2 118.15(7) . 2_766 ? Cu1 I1 Cu2 155.00(7) 2_665 2_766 ? Cu3 I1 Cu2 63.74(6) 1_554 2_766 ? O5 Eu3 O6 88.3(3) . 2_766 ? O5 Eu3 O8 148.4(3) . 2_676 ? O6 Eu3 O8 76.1(3) 2_766 2_676 ? O5 Eu3 O9 77.2(3) . . ? O6 Eu3 O9 143.7(3) 2_766 . ? O8 Eu3 O9 130.4(3) 2_676 . ? O5 Eu3 O3 78.6(3) . . ? O6 Eu3 O3 120.5(3) 2_766 . ? O8 Eu3 O3 85.7(3) 2_676 . ? O9 Eu3 O3 89.5(3) . . ? O5 Eu3 O7 131.9(3) . . ? O6 Eu3 O7 139.6(3) 2_766 . ? O8 Eu3 O7 66.8(3) 2_676 . ? O9 Eu3 O7 64.6(3) . . ? O3 Eu3 O7 73.1(3) . . ? O5 Eu3 O1 131.1(3) . . ? O6 Eu3 O1 82.3(3) 2_766 . ? O8 Eu3 O1 74.6(3) 2_676 . ? O9 Eu3 O1 82.6(3) . . ? O3 Eu3 O1 145.6(3) . . ? O7 Eu3 O1 73.2(3) . . ? O5 Eu3 O2 80.5(3) . . ? O6 Eu3 O2 71.2(3) 2_766 . ? O8 Eu3 O2 118.7(3) 2_676 . ? O9 Eu3 O2 73.6(3) . . ? O3 Eu3 O2 155.5(3) . . ? O7 Eu3 O2 113.1(3) . . ? O1 Eu3 O2 51.0(3) . . ? O5 Eu3 O4 80.5(3) . . ? O6 Eu3 O4 69.6(3) 2_766 . ? O8 Eu3 O4 68.4(3) 2_676 . ? O9 Eu3 O4 137.9(3) . . ? O3 Eu3 O4 51.1(3) . . ? O7 Eu3 O4 108.7(3) . . ? O1 Eu3 O4 137.6(3) . . ? O2 Eu3 O4 136.6(3) . . ? O5 Eu3 C19 159.7(3) . 2_676 ? O6 Eu3 C19 94.3(3) 2_766 2_676 ? O8 Eu3 C19 19.7(3) 2_676 2_676 ? O9 Eu3 C19 110.8(3) . 2_676 ? O3 Eu3 C19 82.7(3) . 2_676 ? O7 Eu3 C19 47.3(3) . 2_676 ? O1 Eu3 C19 69.2(3) . 2_676 ? O2 Eu3 C19 119.4(3) . 2_676 ? O4 Eu3 C19 81.6(3) . 2_676 ? O5 Eu3 Na1 118.6(3) . 2_676 ? O6 Eu3 Na1 62.9(3) 2_766 2_676 ? O8 Eu3 Na1 29.8(2) 2_676 2_676 ? O9 Eu3 Na1 152.6(3) . 2_676 ? O3 Eu3 Na1 73.5(3) . 2_676 ? O7 Eu3 Na1 89.6(3) . 2_676 ? O1 Eu3 Na1 99.3(3) . 2_676 ? O2 Eu3 Na1 128.5(3) . 2_676 ? O4 Eu3 Na1 39.8(3) . 2_676 ? C19 Eu3 Na1 47.0(3) 2_676 2_676 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C6 -5.3(19) . . . . ? O2 C1 C2 C6 178.6(12) . . . . ? O1 C1 C2 C3 173.2(12) . . . . ? O2 C1 C2 C3 -2.9(19) . . . . ? C6 C2 C3 C4 1(2) . . . . ? C1 C2 C3 C4 -177.6(13) . . . . ? C2 C3 C4 N1 -2(2) . . . . ? C3 C2 C6 C5 -1.0(19) . . . . ? C1 C2 C6 C5 177.6(12) . . . . ? N1 C5 C6 C2 2(2) . . . . ? O3 C7 C8 C9 -165.7(13) . . . . ? O4 C7 C8 C9 14(2) . . . . ? O3 C7 C8 C12 15.4(19) . . . . ? O4 C7 C8 C12 -165.1(13) . . . . ? C12 C8 C9 C10 -1(2) . . . . ? C7 C8 C9 C10 -179.4(13) . . . . ? C8 C9 C10 N2 1(2) . . . . ? C9 C8 C12 C11 -2(2) . . . . ? C7 C8 C12 C11 176.6(13) . . . . ? N2 C11 C12 C8 5(2) . . . . ? O5 C13 C14 C15 -10.7(18) . . . . ? O6 C13 C14 C15 168.3(11) . . . . ? O5 C13 C14 C18 171.2(12) . . . . ? O6 C13 C14 C18 -9.8(19) . . . . ? C18 C14 C15 C16 1.0(17) . . . . ? C13 C14 C15 C16 -177.2(12) . . . . ? C14 C15 C16 N3 -2(2) . . . . ? N3 C17 C18 C14 -1(2) . . . . ? C15 C14 C18 C17 0.1(18) . . . . ? C13 C14 C18 C17 178.4(12) . . . . ? C3 C4 N1 C5 3(2) . . . . ? C3 C4 N1 Cu1 175.1(11) . . . . ? C6 C5 N1 C4 -2.7(19) . . . . ? C6 C5 N1 Cu1 -175.0(10) . . . . ? C9 C10 N2 C11 2(2) . . . . ? C9 C10 N2 Cu2 179.7(12) . . . . ? C12 C11 N2 C10 -5(2) . . . . ? C12 C11 N2 Cu2 177.2(12) . . . . ? C18 C17 N3 C16 0.0(19) . . . . ? C18 C17 N3 Cu3 178.2(10) . . . . ? C15 C16 N3 C17 1.3(19) . . . . ? C15 C16 N3 Cu3 -176.8(10) . . . . ? O2 C1 O1 Eu3 3.4(13) . . . . ? C2 C1 O1 Eu3 -172.6(10) . . . . ? O1 C1 O2 Eu3 -3.4(13) . . . . ? C2 C1 O2 Eu3 172.6(10) . . . . ? O4 C7 O3 Eu3 3.5(14) . . . . ? C8 C7 O3 Eu3 -177.1(10) . . . . ? O3 C7 O4 Na1 97.3(14) . . . 2_676 ? C8 C7 O4 Na1 -82.2(13) . . . 2_676 ? O3 C7 O4 Eu3 -3.2(13) . . . . ? C8 C7 O4 Eu3 177.4(10) . . . . ? O6 C13 O5 Eu3 -36(4) . . . . ? C14 C13 O5 Eu3 143(2) . . . . ? O5 C13 O6 Eu3 83.7(16) . . . 2_766 ? C14 C13 O6 Eu3 -95.2(14) . . . 2_766 ? O8 C19 O7 Eu3 173.2(9) . . . . ? C19 C19 O7 Eu3 -0.9(17) 2_676 . . . ? Na1 C19 O7 Eu3 148.0(7) 2_576 . . . ? Eu3 C19 O7 Eu3 -179(3) 2_676 . . . ? O8 C19 O7 Na1 25.1(13) . . . 2_576 ? C19 C19 O7 Na1 -148.9(14) 2_676 . . 2_576 ? Eu3 C19 O7 Na1 33(3) 2_676 . . 2_576 ? O7 C19 O8 Na1 -37.2(15) . . . . ? C19 C19 O8 Na1 136.8(12) 2_676 . . . ? Na1 C19 O8 Na1 -10.7(8) 2_576 . . . ? Eu3 C19 O8 Na1 146.0(10) 2_676 . . . ? O7 C19 O8 Eu3 176.8(9) . . . 2_676 ? C19 C19 O8 Eu3 -9.3(18) 2_676 . . 2_676 ? Na1 C19 O8 Eu3 -156.7(8) 2_576 . . 2_676 ? O7 C19 O8 Na1 -26.5(13) . . . 2_576 ? C19 C19 O8 Na1 147.5(13) 2_676 . . 2_576 ? Eu3 C19 O8 Na1 156.7(8) 2_676 . . 2_576 ? C17 N3 Cu3 I3 25.3(10) . . . . ? C16 N3 Cu3 I3 -156.7(10) . . . . ? C17 N3 Cu3 I1 -105.2(9) . . . 1_556 ? C16 N3 Cu3 I1 72.8(11) . . . 1_556 ? C17 N3 Cu3 I2 146.9(9) . . . . ? C16 N3 Cu3 I2 -35.1(11) . . . . ? C17 N3 Cu3 Cu2 -26.6(13) . . . 2_767 ? C16 N3 Cu3 Cu2 151.5(8) . . . 2_767 ? Cu2 I3 Cu3 N3 -91.0(3) 1_545 . . . ? Cu2 I3 Cu3 N3 -143.0(3) 2_767 . . . ? Cu2 I3 Cu3 I1 38.77(9) 1_545 . . 1_556 ? Cu2 I3 Cu3 I1 -13.18(8) 2_767 . . 1_556 ? Cu2 I3 Cu3 I2 154.90(7) 1_545 . . . ? Cu2 I3 Cu3 I2 102.95(8) 2_767 . . . ? Cu2 I3 Cu3 Cu2 51.95(8) 1_545 . . 2_767 ? C10 N2 Cu2 I3 34.8(14) . . . 1_565 ? C11 N2 Cu2 I3 -147.4(11) . . . 1_565 ? C10 N2 Cu2 I3 177.3(11) . . . 2_767 ? C11 N2 Cu2 I3 -4.9(13) . . . 2_767 ? C10 N2 Cu2 Cu2 111.2(12) . . . 2_777 ? C11 N2 Cu2 Cu2 -70.9(14) . . . 2_777 ? C10 N2 Cu2 I1 -68.1(13) . . . 2_766 ? C11 N2 Cu2 I1 109.7(12) . . . 2_766 ? C10 N2 Cu2 Cu3 -123.2(12) . . . 2_767 ? C11 N2 Cu2 Cu3 54.7(13) . . . 2_767 ? C4 N1 Cu1 I1 32.9(12) . . . . ? C5 N1 Cu1 I1 -155.3(9) . . . . ? C4 N1 Cu1 I1 173.9(10) . . . 2_665 ? C5 N1 Cu1 I1 -14.2(10) . . . 2_665 ? C4 N1 Cu1 Cu1 104.3(11) . . . 2_665 ? C5 N1 Cu1 Cu1 -83.8(11) . . . 2_665 ? C4 N1 Cu1 I2 -73.9(11) . . . 1_554 ? C5 N1 Cu1 I2 97.9(9) . . . 1_554 ? C19 O8 Na1 Na1 29(2) . . . 2_576 ? Eu3 O8 Na1 Na1 175.1(17) 2_676 . . 2_576 ? C19 O8 Na1 O10 119.4(10) . . . 2_576 ? Eu3 O8 Na1 O10 -94.6(6) 2_676 . . 2_576 ? Na1 O8 Na1 O10 90.2(19) 2_576 . . 2_576 ? C19 O8 Na1 O10 -36.4(10) . . . . ? Eu3 O8 Na1 O10 109.5(5) 2_676 . . . ? Na1 O8 Na1 O10 -65.6(18) 2_576 . . . ? C19 O8 Na1 O8 29(2) . . . 2_576 ? Eu3 O8 Na1 O8 175.1(17) 2_676 . . 2_576 ? Na1 O8 Na1 O8 0.000(4) 2_576 . . 2_576 ? C19 O8 Na1 O7 -172.4(14) . . . 2_576 ? Eu3 O8 Na1 O7 -26.5(17) 2_676 . . 2_576 ? Na1 O8 Na1 O7 158(3) 2_576 . . 2_576 ? C19 O8 Na1 O4 -132.0(9) . . . 2_676 ? Eu3 O8 Na1 O4 13.9(6) 2_676 . . 2_676 ? Na1 O8 Na1 O4 -161(2) 2_576 . . 2_676 ? C19 O8 Na1 C19 123(3) . . . 2_576 ? Eu3 O8 Na1 C19 -91(3) 2_676 . . 2_576 ? Na1 O8 Na1 C19 94(3) 2_576 . . 2_576 ? C19 O8 Na1 Eu3 -146.0(11) . . . 2_676 ? Na1 O8 Na1 Eu3 -175.1(17) 2_576 . . 2_676 ? Na1 O10 Na1 O10 0.000(3) 2_576 . . 2_576 ? Na1 O10 Na1 O8 88.9(17) 2_576 . . . ? Na1 O10 Na1 O8 -70.5(15) 2_576 . . 2_576 ? Na1 O10 Na1 O7 -111.8(18) 2_576 . . 2_576 ? Na1 O10 Na1 O4 158.9(19) 2_576 . . 2_676 ? Na1 O10 Na1 C19 -87.2(16) 2_576 . . 2_576 ? Na1 O10 Na1 Eu3 119.0(18) 2_576 . . 2_676 ? N3 Cu3 I2 Cu1 103.1(3) . . . 1_556 ? I3 Cu3 I2 Cu1 -142.11(8) . . . 1_556 ? I1 Cu3 I2 Cu1 -16.47(6) 1_556 . . 1_556 ? Cu2 Cu3 I2 Cu1 -81.38(9) 2_767 . . 1_556 ? N3 Cu3 I2 Cu1 -76.9(3) . . . 2_766 ? I3 Cu3 I2 Cu1 37.89(8) . . . 2_766 ? I1 Cu3 I2 Cu1 163.53(6) 1_556 . . 2_766 ? Cu2 Cu3 I2 Cu1 98.62(9) 2_767 . . 2_766 ? N1 Cu1 I1 Cu1 138.4(4) . . . 2_665 ? I1 Cu1 I1 Cu1 0.0 2_665 . . 2_665 ? I2 Cu1 I1 Cu1 -116.96(9) 1_554 . . 2_665 ? N1 Cu1 I1 Cu3 -121.9(3) . . . 1_554 ? I1 Cu1 I1 Cu3 99.65(8) 2_665 . . 1_554 ? Cu1 Cu1 I1 Cu3 99.65(8) 2_665 . . 1_554 ? I2 Cu1 I1 Cu3 -17.31(6) 1_554 . . 1_554 ? N1 Cu1 I1 Cu2 -70.1(3) . . . 2_766 ? I1 Cu1 I1 Cu2 151.45(8) 2_665 . . 2_766 ? Cu1 Cu1 I1 Cu2 151.45(8) 2_665 . . 2_766 ? I2 Cu1 I1 Cu2 34.49(8) 1_554 . . 2_766 ? C13 O5 Eu3 O6 -9(3) . . . 2_766 ? C13 O5 Eu3 O8 -69(3) . . . 2_676 ? C13 O5 Eu3 O9 137(3) . . . . ? C13 O5 Eu3 O3 -131(3) . . . . ? C13 O5 Eu3 O7 174(3) . . . . ? C13 O5 Eu3 O1 69(3) . . . . ? C13 O5 Eu3 O2 62(3) . . . . ? C13 O5 Eu3 O4 -79(3) . . . . ? C13 O5 Eu3 C19 -107(3) . . . 2_676 ? C13 O5 Eu3 Na1 -67(3) . . . 2_676 ? C7 O3 Eu3 O5 85.1(8) . . . . ? C7 O3 Eu3 O6 3.9(9) . . . 2_766 ? C7 O3 Eu3 O8 -67.3(8) . . . 2_676 ? C7 O3 Eu3 O9 162.2(8) . . . . ? C7 O3 Eu3 O7 -134.3(8) . . . . ? C7 O3 Eu3 O1 -121.7(8) . . . . ? C7 O3 Eu3 O2 116.9(9) . . . . ? C7 O3 Eu3 O4 -1.8(7) . . . . ? C7 O3 Eu3 C19 -86.8(8) . . . 2_676 ? C7 O3 Eu3 Na1 -39.6(7) . . . 2_676 ? C19 O7 Eu3 O5 152.9(8) . . . . ? Na1 O7 Eu3 O5 -83.9(8) 2_576 . . . ? C19 O7 Eu3 O6 -21.2(10) . . . 2_766 ? Na1 O7 Eu3 O6 102.0(8) 2_576 . . 2_766 ? C19 O7 Eu3 O8 3.7(8) . . . 2_676 ? Na1 O7 Eu3 O8 126.9(8) 2_576 . . 2_676 ? C19 O7 Eu3 O9 -166.1(9) . . . . ? Na1 O7 Eu3 O9 -42.9(7) 2_576 . . . ? C19 O7 Eu3 O3 96.3(9) . . . . ? Na1 O7 Eu3 O3 -140.6(8) 2_576 . . . ? C19 O7 Eu3 O1 -76.4(8) . . . . ? Na1 O7 Eu3 O1 46.8(7) 2_576 . . . ? C19 O7 Eu3 O2 -108.9(8) . . . . ? Na1 O7 Eu3 O2 14.2(8) 2_576 . . . ? C19 O7 Eu3 O4 59.0(9) . . . . ? Na1 O7 Eu3 O4 -177.8(7) 2_576 . . . ? C19 O7 Eu3 C19 0.5(10) . . . 2_676 ? Na1 O7 Eu3 C19 123.7(9) 2_576 . . 2_676 ? C19 O7 Eu3 Na1 23.4(8) . . . 2_676 ? Na1 O7 Eu3 Na1 146.6(8) 2_576 . . 2_676 ? C1 O1 Eu3 O5 -10.8(9) . . . . ? C1 O1 Eu3 O6 70.2(7) . . . 2_766 ? C1 O1 Eu3 O8 147.9(8) . . . 2_676 ? C1 O1 Eu3 O9 -76.7(7) . . . . ? C1 O1 Eu3 O3 -154.8(7) . . . . ? C1 O1 Eu3 O7 -142.3(8) . . . . ? C1 O1 Eu3 O2 -1.9(7) . . . . ? C1 O1 Eu3 O4 118.1(8) . . . . ? C1 O1 Eu3 C19 167.8(8) . . . 2_676 ? C1 O1 Eu3 Na1 131.0(7) . . . 2_676 ? C1 O2 Eu3 O5 175.0(8) . . . . ? C1 O2 Eu3 O6 -93.5(8) . . . 2_766 ? C1 O2 Eu3 O8 -31.8(8) . . . 2_676 ? C1 O2 Eu3 O9 95.7(8) . . . . ? C1 O2 Eu3 O3 143.5(8) . . . . ? C1 O2 Eu3 O7 43.4(8) . . . . ? C1 O2 Eu3 O1 1.8(7) . . . . ? C1 O2 Eu3 O4 -119.9(8) . . . . ? C1 O2 Eu3 C19 -9.3(8) . . . 2_676 ? C1 O2 Eu3 Na1 -65.8(8) . . . 2_676 ? C7 O4 Eu3 O5 -81.3(8) . . . . ? Na1 O4 Eu3 O5 163.6(5) 2_676 . . . ? C7 O4 Eu3 O6 -173.0(8) . . . 2_766 ? Na1 O4 Eu3 O6 71.8(5) 2_676 . . 2_766 ? C7 O4 Eu3 O8 104.3(8) . . . 2_676 ? Na1 O4 Eu3 O8 -10.9(4) 2_676 . . 2_676 ? C7 O4 Eu3 O9 -22.6(10) . . . . ? Na1 O4 Eu3 O9 -137.7(5) 2_676 . . . ? C7 O4 Eu3 O3 1.7(7) . . . . ? Na1 O4 Eu3 O3 -113.4(6) 2_676 . . . ? C7 O4 Eu3 O7 49.9(8) . . . . ? Na1 O4 Eu3 O7 -65.3(5) 2_676 . . . ? C7 O4 Eu3 O1 135.3(7) . . . . ? Na1 O4 Eu3 O1 20.1(6) 2_676 . . . ? C7 O4 Eu3 O2 -146.4(7) . . . . ? Na1 O4 Eu3 O2 98.5(5) 2_676 . . . ? C7 O4 Eu3 C19 89.2(8) . . . 2_676 ? Na1 O4 Eu3 C19 -26.0(4) 2_676 . . 2_676 ? C7 O4 Eu3 Na1 115.1(9) . . . 2_676 ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.20 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.100 _refine_diff_density_min -1.423 _refine_diff_density_rms 0.268 ################################################################################ data_3 #TrackingRef '- Cifs.txt' _database_code_depnum_ccdc_archive 'CCDC 804309' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H32 Cu6 Gd2 I5 N6 Na O20, 0.5(H4 O2)' _chemical_formula_sum 'C38 H34 Cu6 Gd2 I5 N6 Na O21' _chemical_formula_weight 2263.94 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 '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 '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.1322(15) _cell_length_b 11.260(3) _cell_length_c 18.161(4) _cell_angle_alpha 86.072(3) _cell_angle_beta 79.964(3) _cell_angle_gamma 72.880(2) _cell_volume 1372.2(5) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1912 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 26.19 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.740 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1050 _exptl_absorpt_coefficient_mu 7.557 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.189 _exptl_absorpt_correction_T_max 0.230 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II area-detector diffractometer' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7184 _diffrn_reflns_av_R_equivalents 0.0279 _diffrn_reflns_av_sigmaI/netI 0.0599 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 25.20 _reflns_number_total 4876 _reflns_number_gt 3773 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0346P)^2^+3.2376P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4876 _refine_ls_number_parameters 386 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0581 _refine_ls_R_factor_gt 0.0405 _refine_ls_wR_factor_ref 0.0906 _refine_ls_wR_factor_gt 0.0812 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6222(12) 0.6497(7) 0.3780(4) 0.0193(18) Uani 1 1 d . . . C2 C 0.6086(12) 0.6195(7) 0.3001(5) 0.0201(19) Uani 1 1 d . . . C3 C 0.6843(13) 0.4985(8) 0.2758(5) 0.031(2) Uani 1 1 d . . . H3 H 0.7410 0.4341 0.3072 0.038 Uiso 1 1 calc R . . C4 C 0.6724(14) 0.4768(8) 0.2024(5) 0.035(2) Uani 1 1 d . . . H4 H 0.7209 0.3952 0.1861 0.042 Uiso 1 1 calc R . . C5 C 0.5272(14) 0.6781(8) 0.1789(5) 0.031(2) Uani 1 1 d . . . H5 H 0.4711 0.7410 0.1466 0.037 Uiso 1 1 calc R . . C6 C 0.5331(13) 0.7091(8) 0.2499(5) 0.028(2) Uani 1 1 d . . . H6 H 0.4854 0.7918 0.2640 0.033 Uiso 1 1 calc R . . C7 C 0.8360(15) 0.7871(8) 0.6472(5) 0.031(2) Uani 1 1 d . . . C8 C 0.8915(13) 0.8197(8) 0.7185(5) 0.025(2) Uani 1 1 d . . . C9 C 1.0631(15) 0.8508(9) 0.7180(5) 0.035(2) Uani 1 1 d . . . H9 H 1.1487 0.8538 0.6735 0.042 Uiso 1 1 calc R . . C10 C 1.1068(15) 0.8777(10) 0.7852(5) 0.040(3) Uani 1 1 d . . . H10 H 1.2254 0.8966 0.7847 0.048 Uiso 1 1 calc R . . C11 C 0.8234(17) 0.8460(11) 0.8493(6) 0.055(3) Uani 1 1 d . . . H11 H 0.7412 0.8422 0.8947 0.066 Uiso 1 1 calc R . . C12 C 0.7685(16) 0.8187(10) 0.7850(5) 0.047(3) Uani 1 1 d . . . H12 H 0.6493 0.7998 0.7868 0.056 Uiso 1 1 calc R . . C13 C 0.8948(11) 0.4216(7) 0.6019(4) 0.0178(18) Uani 1 1 d . . . C14 C 0.9013(12) 0.3922(7) 0.6827(4) 0.0188(18) Uani 1 1 d . . . C15 C 0.8279(12) 0.4848(8) 0.7363(5) 0.026(2) Uani 1 1 d . . . H15 H 0.7661 0.5662 0.7225 0.032 Uiso 1 1 calc R . . C16 C 0.8481(14) 0.4543(8) 0.8101(5) 0.033(2) Uani 1 1 d . . . H16 H 0.8047 0.5174 0.8450 0.039 Uiso 1 1 calc R . . C17 C 0.9970(14) 0.2487(8) 0.7818(5) 0.031(2) Uani 1 1 d . . . H17 H 1.0536 0.1676 0.7974 0.037 Uiso 1 1 calc R . . C18 C 0.9880(12) 0.2726(8) 0.7067(5) 0.025(2) Uani 1 1 d . . . H18 H 1.0399 0.2086 0.6726 0.030 Uiso 1 1 calc R . . C19 C 0.3972(12) 0.9940(7) 0.5174(4) 0.0181(18) Uani 1 1 d . . . N1 N 0.5973(10) 0.5632(7) 0.1542(4) 0.0275(17) Uani 1 1 d . . . N2 N 0.9898(12) 0.8778(7) 0.8496(4) 0.035(2) Uani 1 1 d . . . N3 N 0.9271(11) 0.3384(7) 0.8332(4) 0.0280(17) Uani 1 1 d . . . O1 O 0.5752(9) 0.7626(5) 0.3965(3) 0.0266(14) Uani 1 1 d . . . O2 O 0.6910(9) 0.5636(5) 0.4224(3) 0.0252(14) Uani 1 1 d . . . O3 O 0.6580(10) 0.7856(6) 0.6484(3) 0.0364(16) Uani 1 1 d . . . O4 O 0.9648(10) 0.7633(6) 0.5896(4) 0.0439(18) Uani 1 1 d . . . O5 O 0.7935(9) 0.5278(5) 0.5855(3) 0.0300(15) Uani 1 1 d . . . O6 O 0.9923(8) 0.3395(5) 0.5556(3) 0.0251(13) Uani 1 1 d . . . O7 O 0.3875(8) 0.8885(5) 0.5404(3) 0.0258(14) Uani 1 1 d . . . O8 O 0.2523(8) 1.0892(5) 0.5186(3) 0.0242(13) Uani 1 1 d . . . O9 O 0.3903(9) 0.6560(5) 0.5551(4) 0.0312(15) Uani 1 1 d D . . H9A H 0.318(11) 0.713(5) 0.581(4) 0.047 Uiso 1 1 d D . . H9B H 0.358(13) 0.592(4) 0.563(5) 0.047 Uiso 1 1 d D . . O10 O 0.1708(12) 0.8942(9) 0.4018(6) 0.078(3) Uani 1 1 d D . . H10A H 0.278(9) 0.840(8) 0.400(8) 0.117 Uiso 1 1 d D . . H10B H 0.185(18) 0.957(7) 0.379(8) 0.117 Uiso 1 1 d D . . O11 O 0.603(2) 0.9785(15) 0.3001(10) 0.061(4) Uani 0.50 1 d PD . . H11A H 0.494(16) 1.01(2) 0.288(13) 0.092 Uiso 0.50 1 d PD . . H11B H 0.59(3) 0.929(19) 0.335(10) 0.092 Uiso 0.50 1 d PD . . I3 I 1.23588(9) 0.08750(5) 0.94402(3) 0.03278(17) Uani 1 1 d . . . Cu3 Cu 0.9395(2) 0.29410(13) 0.94325(7) 0.0480(4) Uani 1 1 d . . . Cu2 Cu 1.0520(2) 0.91860(15) 0.94705(7) 0.0591(4) Uani 1 1 d . . . Cu1 Cu 0.60857(19) 0.51998(11) 0.04763(6) 0.0401(3) Uani 1 1 d . . . Na1 Na -0.0219(14) 1.0406(8) 0.4889(5) 0.048(3) Uani 0.50 1 d P . . I2 I 1.0000 0.5000 1.0000 0.0429(3) Uani 1 2 d S . . I1 I 0.59591(9) 0.29345(5) 0.02858(3) 0.03030(16) Uani 1 1 d . . . Gd1 Gd 0.69348(6) 0.71416(3) 0.52090(2) 0.01679(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.019(4) 0.025(5) 0.016(4) -0.001(4) -0.007(4) -0.008(4) C2 0.016(4) 0.027(4) 0.022(5) -0.002(4) -0.014(4) -0.006(4) C3 0.043(6) 0.023(5) 0.021(5) -0.006(4) -0.009(4) 0.005(4) C4 0.045(6) 0.031(5) 0.032(6) -0.008(4) -0.013(5) -0.009(5) C5 0.038(6) 0.037(5) 0.027(5) 0.003(4) -0.015(5) -0.021(5) C6 0.031(5) 0.024(5) 0.034(5) 0.000(4) -0.010(4) -0.014(4) C7 0.038(6) 0.030(5) 0.024(5) -0.006(4) -0.007(5) -0.006(4) C8 0.024(5) 0.032(5) 0.020(5) -0.004(4) -0.008(4) -0.005(4) C9 0.042(6) 0.047(6) 0.019(5) -0.003(4) -0.002(5) -0.018(5) C10 0.029(6) 0.066(7) 0.034(6) -0.018(5) 0.000(5) -0.025(5) C11 0.055(7) 0.098(10) 0.026(6) -0.014(6) -0.001(5) -0.042(7) C12 0.050(7) 0.071(8) 0.032(6) -0.012(5) -0.013(6) -0.030(6) C13 0.014(4) 0.023(4) 0.018(5) 0.000(4) -0.003(4) -0.007(3) C14 0.018(4) 0.019(4) 0.018(4) 0.002(3) -0.002(4) -0.004(3) C15 0.027(5) 0.022(5) 0.028(5) 0.009(4) -0.006(4) -0.007(4) C16 0.037(6) 0.033(5) 0.028(5) -0.003(4) -0.004(5) -0.008(4) C17 0.035(5) 0.019(5) 0.037(6) 0.002(4) -0.009(5) -0.005(4) C18 0.021(5) 0.031(5) 0.021(5) 0.002(4) -0.002(4) -0.007(4) C19 0.019(4) 0.018(4) 0.017(4) -0.005(3) 0.000(4) -0.006(3) N1 0.025(4) 0.036(4) 0.020(4) -0.001(3) -0.006(3) -0.007(3) N2 0.044(5) 0.049(5) 0.022(4) -0.011(4) -0.006(4) -0.025(4) N3 0.027(4) 0.037(5) 0.021(4) 0.008(3) -0.009(3) -0.010(4) O1 0.036(4) 0.019(3) 0.022(3) -0.003(2) -0.010(3) -0.002(3) O2 0.037(4) 0.024(3) 0.019(3) 0.002(3) -0.008(3) -0.014(3) O3 0.043(4) 0.039(4) 0.031(4) -0.015(3) -0.015(3) -0.008(3) O4 0.039(4) 0.056(5) 0.025(4) -0.011(3) -0.010(3) 0.009(3) O5 0.040(4) 0.018(3) 0.024(3) 0.004(3) -0.005(3) 0.003(3) O6 0.023(3) 0.028(3) 0.019(3) -0.004(3) 0.004(3) -0.003(3) O7 0.022(3) 0.010(3) 0.041(4) 0.005(3) -0.004(3) -0.001(2) O8 0.019(3) 0.013(3) 0.039(4) -0.001(3) -0.004(3) -0.004(2) O9 0.028(4) 0.021(3) 0.042(4) -0.002(3) 0.003(3) -0.007(3) O10 0.052(5) 0.088(7) 0.083(7) -0.033(6) -0.032(5) 0.014(5) O11 0.078(12) 0.037(10) 0.061(12) 0.005(8) -0.005(10) -0.009(9) I3 0.0375(4) 0.0325(3) 0.0310(4) 0.0038(3) -0.0100(3) -0.0125(3) Cu3 0.0551(9) 0.0621(9) 0.0248(7) 0.0080(6) -0.0103(6) -0.0137(7) Cu2 0.0675(10) 0.0959(12) 0.0320(8) -0.0221(8) -0.0038(7) -0.0490(9) Cu1 0.0507(8) 0.0483(8) 0.0257(7) -0.0047(6) -0.0132(6) -0.0162(6) Na1 0.035(5) 0.085(9) 0.033(6) 0.007(5) -0.003(4) -0.034(6) I2 0.0282(5) 0.0525(6) 0.0515(6) -0.0268(5) 0.0033(5) -0.0167(4) I1 0.0309(3) 0.0273(3) 0.0333(4) 0.0021(3) -0.0064(3) -0.0092(3) Gd1 0.0214(2) 0.0133(2) 0.0158(2) -0.00033(15) -0.00482(17) -0.00413(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 C1 O2 1.258(9) . ? C1 O1 1.268(9) . ? C1 C2 1.504(10) . ? C2 C6 1.365(11) . ? C2 C3 1.381(11) . ? C3 C4 1.394(11) . ? C3 H3 0.9300 . ? C4 N1 1.319(11) . ? C4 H4 0.9300 . ? C5 N1 1.321(11) . ? C5 C6 1.368(12) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 O4 1.253(11) . ? C7 O3 1.271(11) . ? C7 C8 1.515(11) . ? C8 C12 1.365(13) . ? C8 C9 1.367(12) . ? C9 C10 1.384(12) . ? C9 H9 0.9300 . ? C10 N2 1.312(12) . ? C10 H10 0.9300 . ? C11 N2 1.337(12) . ? C11 C12 1.375(13) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 O5 1.248(9) . ? C13 O6 1.252(9) . ? C13 C14 1.489(11) . ? C14 C18 1.382(11) . ? C14 C15 1.396(11) . ? C15 C16 1.381(12) . ? C15 H15 0.9300 . ? C16 N3 1.332(11) . ? C16 H16 0.9300 . ? C17 N3 1.346(11) . ? C17 C18 1.380(12) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 O7 1.248(9) . ? C19 O8 1.250(9) . ? C19 C19 1.533(16) 2_676 ? C19 Na1 2.838(12) 2_576 ? N1 Cu1 2.010(7) . ? N2 Cu2 2.012(7) . ? N3 Cu3 2.036(7) . ? O1 Gd1 2.517(5) . ? O2 Gd1 2.552(5) . ? O3 Gd1 2.451(6) . ? O4 Na1 2.640(10) 2_676 ? O4 Gd1 2.678(6) . ? O5 Gd1 2.315(5) . ? O6 Gd1 2.356(6) 2_766 ? O7 Gd1 2.459(5) . ? O7 Na1 2.630(11) 2_576 ? O8 Na1 2.335(11) . ? O8 Gd1 2.399(5) 2_676 ? O8 Na1 2.524(11) 2_576 ? O9 Gd1 2.409(6) . ? O9 H9A 0.81(2) . ? O9 H9B 0.81(2) . ? O10 Na1 2.148(14) 2_576 ? O10 Na1 2.318(14) . ? O10 H10A 0.822(10) . ? O10 H10B 0.82(10) . ? O11 H11A 0.82(2) . ? O11 H11B 0.82(2) . ? I3 Cu2 2.6015(15) 1_545 ? I3 Cu2 2.6044(17) 2_767 ? I3 Cu3 2.6439(15) . ? Cu3 I1 2.6633(16) 1_556 ? Cu3 I2 2.7738(15) . ? Cu3 Cu2 3.002(2) 2_767 ? Cu2 I3 2.6015(15) 1_565 ? Cu2 I3 2.6044(17) 2_767 ? Cu2 Cu2 2.606(3) 2_777 ? Cu2 I1 2.9858(18) 2_766 ? Cu2 Cu3 3.002(2) 2_767 ? Cu1 I1 2.6270(14) . ? Cu1 I1 2.6376(14) 2_665 ? Cu1 Cu1 2.654(2) 2_665 ? Cu1 I2 2.7218(14) 1_554 ? Na1 Na1 0.959(15) 2_576 ? Na1 O10 2.148(14) 2_576 ? Na1 O8 2.524(11) 2_576 ? Na1 O7 2.630(11) 2_576 ? Na1 O4 2.640(10) 2_676 ? Na1 C19 2.838(12) 2_576 ? Na1 Gd1 4.091(9) 2_676 ? Na1 H10B 2.33(15) . ? I2 Cu1 2.7218(14) 1_556 ? I2 Cu1 2.7218(14) 2_766 ? I2 Cu3 2.7739(15) 2_767 ? I1 Cu1 2.6376(14) 2_665 ? I1 Cu3 2.6633(16) 1_554 ? I1 Cu2 2.9858(19) 2_766 ? Gd1 O6 2.356(6) 2_766 ? Gd1 O8 2.399(5) 2_676 ? Gd1 Na1 4.091(9) 2_676 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 C1 O1 120.8(7) . . ? O2 C1 C2 119.8(7) . . ? O1 C1 C2 119.3(7) . . ? C6 C2 C3 117.7(8) . . ? C6 C2 C1 122.3(7) . . ? C3 C2 C1 119.9(7) . . ? C2 C3 C4 117.3(8) . . ? C2 C3 H3 121.4 . . ? C4 C3 H3 121.4 . . ? N1 C4 C3 124.9(8) . . ? N1 C4 H4 117.5 . . ? C3 C4 H4 117.5 . . ? N1 C5 C6 123.2(8) . . ? N1 C5 H5 118.4 . . ? C6 C5 H5 118.4 . . ? C2 C6 C5 120.5(8) . . ? C2 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? O4 C7 O3 122.3(8) . . ? O4 C7 C8 119.6(8) . . ? O3 C7 C8 118.0(8) . . ? C12 C8 C9 118.7(8) . . ? C12 C8 C7 119.9(8) . . ? C9 C8 C7 121.4(8) . . ? C8 C9 C10 118.6(9) . . ? C8 C9 H9 120.7 . . ? C10 C9 H9 120.7 . . ? N2 C10 C9 123.5(9) . . ? N2 C10 H10 118.3 . . ? C9 C10 H10 118.3 . . ? N2 C11 C12 122.9(10) . . ? N2 C11 H11 118.6 . . ? C12 C11 H11 118.6 . . ? C8 C12 C11 119.0(10) . . ? C8 C12 H12 120.5 . . ? C11 C12 H12 120.5 . . ? O5 C13 O6 125.0(7) . . ? O5 C13 C14 116.9(7) . . ? O6 C13 C14 118.1(7) . . ? C18 C14 C15 117.8(7) . . ? C18 C14 C13 120.8(7) . . ? C15 C14 C13 121.4(7) . . ? C16 C15 C14 119.3(8) . . ? C16 C15 H15 120.4 . . ? C14 C15 H15 120.4 . . ? N3 C16 C15 122.7(8) . . ? N3 C16 H16 118.7 . . ? C15 C16 H16 118.7 . . ? N3 C17 C18 122.5(8) . . ? N3 C17 H17 118.7 . . ? C18 C17 H17 118.7 . . ? C17 C18 C14 119.5(8) . . ? C17 C18 H18 120.2 . . ? C14 C18 H18 120.2 . . ? O7 C19 O8 125.2(7) . . ? O7 C19 C19 117.1(9) . 2_676 ? O8 C19 C19 117.6(8) . 2_676 ? O7 C19 Na1 67.6(4) . 2_576 ? O8 C19 Na1 62.8(4) . 2_576 ? C19 C19 Na1 153.6(7) 2_676 2_576 ? C4 N1 C5 116.3(8) . . ? C4 N1 Cu1 120.5(6) . . ? C5 N1 Cu1 123.1(6) . . ? C10 N2 C11 117.2(8) . . ? C10 N2 Cu2 123.5(6) . . ? C11 N2 Cu2 119.3(7) . . ? C16 N3 C17 118.2(8) . . ? C16 N3 Cu3 121.9(6) . . ? C17 N3 Cu3 119.9(6) . . ? C1 O1 Gd1 94.6(4) . . ? C1 O2 Gd1 93.2(5) . . ? C7 O3 Gd1 98.4(5) . . ? C7 O4 Na1 115.1(6) . 2_676 ? C7 O4 Gd1 88.2(5) . . ? Na1 O4 Gd1 100.6(3) 2_676 . ? C13 O5 Gd1 160.4(6) . . ? C13 O6 Gd1 137.6(5) . 2_766 ? C19 O7 Gd1 118.1(5) . . ? C19 O7 Na1 86.3(5) . 2_576 ? Gd1 O7 Na1 141.2(3) . 2_576 ? C19 O8 Na1 110.5(5) . . ? C19 O8 Gd1 119.8(5) . 2_676 ? Na1 O8 Gd1 119.6(3) . 2_676 ? C19 O8 Na1 91.1(5) . 2_576 ? Na1 O8 Na1 22.3(4) . 2_576 ? Gd1 O8 Na1 141.9(3) 2_676 2_576 ? Gd1 O9 H9A 103(6) . . ? Gd1 O9 H9B 137(6) . . ? H9A O9 H9B 113(4) . . ? Na1 O10 Na1 24.4(4) 2_576 . ? Na1 O10 H10A 117(10) 2_576 . ? Na1 O10 H10A 135(10) . . ? Na1 O10 H10B 104(10) 2_576 . ? Na1 O10 H10B 81(10) . . ? H10A O10 H10B 110(2) . . ? H11A O11 H11B 110(4) . . ? Cu2 I3 Cu2 60.09(5) 1_545 2_767 ? Cu2 I3 Cu3 101.52(6) 1_545 . ? Cu2 I3 Cu3 69.77(5) 2_767 . ? N3 Cu3 I3 105.3(2) . . ? N3 Cu3 I1 115.8(2) . 1_556 ? I3 Cu3 I1 116.57(5) . 1_556 ? N3 Cu3 I2 104.2(2) . . ? I3 Cu3 I2 115.01(5) . . ? I1 Cu3 I2 99.57(5) 1_556 . ? N3 Cu3 Cu2 141.2(2) . 2_767 ? I3 Cu3 Cu2 54.50(4) . 2_767 ? I1 Cu3 Cu2 63.28(4) 1_556 2_767 ? I2 Cu3 Cu2 114.31(5) . 2_767 ? N2 Cu2 I3 117.5(2) . 1_565 ? N2 Cu2 I3 110.6(2) . 2_767 ? I3 Cu2 I3 119.91(5) 1_565 2_767 ? N2 Cu2 Cu2 144.3(3) . 2_777 ? I3 Cu2 Cu2 60.01(6) 1_565 2_777 ? I3 Cu2 Cu2 59.90(6) 2_767 2_777 ? N2 Cu2 I1 103.1(2) . 2_766 ? I3 Cu2 I1 94.76(5) 1_565 2_766 ? I3 Cu2 I1 107.53(6) 2_767 2_766 ? Cu2 Cu2 I1 112.57(8) 2_777 2_766 ? N2 Cu2 Cu3 110.3(2) . 2_767 ? I3 Cu2 Cu3 127.49(6) 1_565 2_767 ? I3 Cu2 Cu3 55.73(4) 2_767 2_767 ? Cu2 Cu2 Cu3 92.57(8) 2_777 2_767 ? I1 Cu2 Cu3 52.82(4) 2_766 2_767 ? N1 Cu1 I1 115.0(2) . . ? N1 Cu1 I1 112.6(2) . 2_665 ? I1 Cu1 I1 119.45(5) . 2_665 ? N1 Cu1 Cu1 143.2(2) . 2_665 ? I1 Cu1 Cu1 59.92(5) . 2_665 ? I1 Cu1 Cu1 59.53(5) 2_665 2_665 ? N1 Cu1 I2 97.4(2) . 1_554 ? I1 Cu1 I2 101.84(4) . 1_554 ? I1 Cu1 I2 106.85(5) 2_665 1_554 ? Cu1 Cu1 I2 119.41(7) 2_665 1_554 ? Na1 Na1 O10 87.8(13) 2_576 2_576 ? Na1 Na1 O10 67.8(13) 2_576 . ? O10 Na1 O10 155.6(4) 2_576 . ? Na1 Na1 O8 90.0(11) 2_576 . ? O10 Na1 O8 86.3(4) 2_576 . ? O10 Na1 O8 93.4(4) . . ? Na1 Na1 O8 67.7(11) 2_576 2_576 ? O10 Na1 O8 92.6(4) 2_576 2_576 ? O10 Na1 O8 78.5(4) . 2_576 ? O8 Na1 O8 157.7(4) . 2_576 ? Na1 Na1 O7 116.9(12) 2_576 2_576 ? O10 Na1 O7 82.2(4) 2_576 2_576 ? O10 Na1 O7 108.2(4) . 2_576 ? O8 Na1 O7 150.1(4) . 2_576 ? O8 Na1 O7 50.9(2) 2_576 2_576 ? Na1 Na1 O4 153.7(14) 2_576 2_676 ? O10 Na1 O4 106.5(5) 2_576 2_676 ? O10 Na1 O4 96.2(4) . 2_676 ? O8 Na1 O4 69.5(3) . 2_676 ? O8 Na1 O4 131.6(4) 2_576 2_676 ? O7 Na1 O4 87.4(3) 2_576 2_676 ? Na1 Na1 C19 90.9(11) 2_576 2_576 ? O10 Na1 C19 81.4(4) 2_576 2_576 ? O10 Na1 C19 98.3(4) . 2_576 ? O8 Na1 C19 167.6(5) . 2_576 ? O8 Na1 C19 26.1(2) 2_576 2_576 ? O7 Na1 C19 26.0(2) 2_576 2_576 ? O4 Na1 C19 112.7(3) 2_676 2_576 ? Na1 Na1 Gd1 120.6(12) 2_576 2_676 ? O10 Na1 Gd1 89.7(4) 2_576 2_676 ? O10 Na1 Gd1 102.4(4) . 2_676 ? O8 Na1 Gd1 30.66(17) . 2_676 ? O8 Na1 Gd1 171.5(3) 2_576 2_676 ? O7 Na1 Gd1 121.5(3) 2_576 2_676 ? O4 Na1 Gd1 40.04(19) 2_676 2_676 ? C19 Na1 Gd1 147.1(3) 2_576 2_676 ? Na1 Na1 H10B 86.8(18) 2_576 . ? O10 Na1 H10B 171(3) 2_576 . ? O10 Na1 H10B 20.3(7) . . ? O8 Na1 H10B 86(3) . . ? O8 Na1 H10B 92(3) 2_576 . ? O7 Na1 H10B 107(4) 2_576 . ? O4 Na1 H10B 75.9(8) 2_676 . ? C19 Na1 H10B 106(3) 2_576 . ? Gd1 Na1 H10B 87(3) 2_676 . ? Cu1 I2 Cu1 180.00(5) 1_556 2_766 ? Cu1 I2 Cu3 104.97(4) 1_556 2_767 ? Cu1 I2 Cu3 75.03(4) 2_766 2_767 ? Cu1 I2 Cu3 75.03(4) 1_556 . ? Cu1 I2 Cu3 104.97(4) 2_766 . ? Cu3 I2 Cu3 180.0 2_767 . ? Cu1 I1 Cu1 60.55(5) . 2_665 ? Cu1 I1 Cu3 78.48(4) . 1_554 ? Cu1 I1 Cu3 92.63(5) 2_665 1_554 ? Cu1 I1 Cu2 118.22(4) . 2_766 ? Cu1 I1 Cu2 155.05(5) 2_665 2_766 ? Cu3 I1 Cu2 63.90(4) 1_554 2_766 ? O5 Gd1 O6 88.3(2) . 2_766 ? O5 Gd1 O8 148.1(2) . 2_676 ? O6 Gd1 O8 76.05(19) 2_766 2_676 ? O5 Gd1 O9 77.0(2) . . ? O6 Gd1 O9 143.4(2) 2_766 . ? O8 Gd1 O9 130.82(19) 2_676 . ? O5 Gd1 O3 78.4(2) . . ? O6 Gd1 O3 120.2(2) 2_766 . ? O8 Gd1 O3 85.6(2) 2_676 . ? O9 Gd1 O3 89.8(2) . . ? O5 Gd1 O7 131.8(2) . . ? O6 Gd1 O7 139.74(19) 2_766 . ? O8 Gd1 O7 67.02(18) 2_676 . ? O9 Gd1 O7 64.79(19) . . ? O3 Gd1 O7 73.4(2) . . ? O5 Gd1 O1 131.26(19) . . ? O6 Gd1 O1 82.33(19) 2_766 . ? O8 Gd1 O1 74.66(18) 2_676 . ? O9 Gd1 O1 82.8(2) . . ? O3 Gd1 O1 145.75(19) . . ? O7 Gd1 O1 73.19(19) . . ? O5 Gd1 O2 80.29(19) . . ? O6 Gd1 O2 71.63(19) 2_766 . ? O8 Gd1 O2 119.19(18) 2_676 . ? O9 Gd1 O2 73.0(2) . . ? O3 Gd1 O2 155.1(2) . . ? O7 Gd1 O2 112.94(19) . . ? O1 Gd1 O2 51.33(17) . . ? O5 Gd1 O4 80.5(2) . . ? O6 Gd1 O4 69.5(2) 2_766 . ? O8 Gd1 O4 68.0(2) 2_676 . ? O9 Gd1 O4 138.0(2) . . ? O3 Gd1 O4 50.9(2) . . ? O7 Gd1 O4 108.66(19) . . ? O1 Gd1 O4 137.4(2) . . ? O2 Gd1 O4 136.89(19) . . ? O5 Gd1 Na1 118.33(19) . 2_676 ? O6 Gd1 Na1 63.2(2) 2_766 2_676 ? O8 Gd1 Na1 29.76(17) 2_676 2_676 ? O9 Gd1 Na1 152.6(2) . 2_676 ? O3 Gd1 Na1 72.9(2) . 2_676 ? O7 Gd1 Na1 89.54(19) . 2_676 ? O1 Gd1 Na1 99.55(17) . 2_676 ? O2 Gd1 Na1 129.4(2) . 2_676 ? O4 Gd1 Na1 39.37(19) . 2_676 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 C1 C2 C6 179.2(8) . . . . ? O1 C1 C2 C6 -5.1(12) . . . . ? O2 C1 C2 C3 -4.5(12) . . . . ? O1 C1 C2 C3 171.2(8) . . . . ? C6 C2 C3 C4 -1.8(13) . . . . ? C1 C2 C3 C4 -178.3(8) . . . . ? C2 C3 C4 N1 1.2(15) . . . . ? C3 C2 C6 C5 2.3(13) . . . . ? C1 C2 C6 C5 178.6(8) . . . . ? N1 C5 C6 C2 -2.0(14) . . . . ? O4 C7 C8 C12 -165.5(9) . . . . ? O3 C7 C8 C12 14.9(13) . . . . ? O4 C7 C8 C9 14.7(13) . . . . ? O3 C7 C8 C9 -165.0(8) . . . . ? C12 C8 C9 C10 1.2(14) . . . . ? C7 C8 C9 C10 -179.0(8) . . . . ? C8 C9 C10 N2 -1.6(16) . . . . ? C9 C8 C12 C11 -1.5(15) . . . . ? C7 C8 C12 C11 178.6(9) . . . . ? N2 C11 C12 C8 2.3(18) . . . . ? O5 C13 C14 C18 171.6(7) . . . . ? O6 C13 C14 C18 -9.3(12) . . . . ? O5 C13 C14 C15 -11.0(12) . . . . ? O6 C13 C14 C15 168.0(7) . . . . ? C18 C14 C15 C16 1.3(12) . . . . ? C13 C14 C15 C16 -176.1(8) . . . . ? C14 C15 C16 N3 -3.1(14) . . . . ? N3 C17 C18 C14 -1.1(14) . . . . ? C15 C14 C18 C17 0.7(12) . . . . ? C13 C14 C18 C17 178.1(8) . . . . ? C3 C4 N1 C5 -0.8(14) . . . . ? C3 C4 N1 Cu1 175.4(8) . . . . ? C6 C5 N1 C4 1.2(13) . . . . ? C6 C5 N1 Cu1 -174.9(7) . . . . ? C9 C10 N2 C11 2.3(16) . . . . ? C9 C10 N2 Cu2 -179.3(8) . . . . ? C12 C11 N2 C10 -2.6(17) . . . . ? C12 C11 N2 Cu2 178.9(9) . . . . ? C15 C16 N3 C17 2.7(14) . . . . ? C15 C16 N3 Cu3 -176.1(7) . . . . ? C18 C17 N3 C16 -0.6(13) . . . . ? C18 C17 N3 Cu3 178.3(7) . . . . ? O2 C1 O1 Gd1 3.6(8) . . . . ? C2 C1 O1 Gd1 -172.1(6) . . . . ? O1 C1 O2 Gd1 -3.5(8) . . . . ? C2 C1 O2 Gd1 172.1(6) . . . . ? O4 C7 O3 Gd1 3.9(10) . . . . ? C8 C7 O3 Gd1 -176.5(6) . . . . ? O3 C7 O4 Na1 97.4(9) . . . 2_676 ? C8 C7 O4 Na1 -82.3(9) . . . 2_676 ? O3 C7 O4 Gd1 -3.5(9) . . . . ? C8 C7 O4 Gd1 176.8(7) . . . . ? O6 C13 O5 Gd1 -35(2) . . . . ? C14 C13 O5 Gd1 144.3(13) . . . . ? O5 C13 O6 Gd1 83.2(10) . . . 2_766 ? C14 C13 O6 Gd1 -95.7(9) . . . 2_766 ? O8 C19 O7 Gd1 174.7(6) . . . . ? C19 C19 O7 Gd1 -3.0(11) 2_676 . . . ? Na1 C19 O7 Gd1 148.3(5) 2_576 . . . ? O8 C19 O7 Na1 26.4(8) . . . 2_576 ? C19 C19 O7 Na1 -151.3(9) 2_676 . . 2_576 ? O7 C19 O8 Na1 -38.9(10) . . . . ? C19 C19 O8 Na1 138.8(8) 2_676 . . . ? Na1 C19 O8 Na1 -11.3(5) 2_576 . . . ? O7 C19 O8 Gd1 175.9(6) . . . 2_676 ? C19 C19 O8 Gd1 -6.4(11) 2_676 . . 2_676 ? Na1 C19 O8 Gd1 -156.5(5) 2_576 . . 2_676 ? O7 C19 O8 Na1 -27.5(9) . . . 2_576 ? C19 C19 O8 Na1 150.1(8) 2_676 . . 2_576 ? C16 N3 Cu3 I3 -156.0(7) . . . . ? C17 N3 Cu3 I3 25.2(7) . . . . ? C16 N3 Cu3 I1 73.7(7) . . . 1_556 ? C17 N3 Cu3 I1 -105.2(6) . . . 1_556 ? C16 N3 Cu3 I2 -34.5(7) . . . . ? C17 N3 Cu3 I2 146.6(6) . . . . ? C16 N3 Cu3 Cu2 152.4(6) . . . 2_767 ? C17 N3 Cu3 Cu2 -26.5(8) . . . 2_767 ? Cu2 I3 Cu3 N3 -91.0(2) 1_545 . . . ? Cu2 I3 Cu3 N3 -142.9(2) 2_767 . . . ? Cu2 I3 Cu3 I1 38.87(6) 1_545 . . 1_556 ? Cu2 I3 Cu3 I1 -13.00(5) 2_767 . . 1_556 ? Cu2 I3 Cu3 I2 154.88(5) 1_545 . . . ? Cu2 I3 Cu3 I2 103.01(5) 2_767 . . . ? Cu2 I3 Cu3 Cu2 51.87(5) 1_545 . . 2_767 ? C10 N2 Cu2 I3 35.2(9) . . . 1_565 ? C11 N2 Cu2 I3 -146.4(8) . . . 1_565 ? C10 N2 Cu2 I3 178.0(7) . . . 2_767 ? C11 N2 Cu2 I3 -3.7(9) . . . 2_767 ? C10 N2 Cu2 Cu2 111.2(8) . . . 2_777 ? C11 N2 Cu2 Cu2 -70.4(10) . . . 2_777 ? C10 N2 Cu2 I1 -67.3(8) . . . 2_766 ? C11 N2 Cu2 I1 111.1(8) . . . 2_766 ? C10 N2 Cu2 Cu3 -122.2(8) . . . 2_767 ? C11 N2 Cu2 Cu3 56.2(9) . . . 2_767 ? C4 N1 Cu1 I1 30.9(8) . . . . ? C5 N1 Cu1 I1 -153.3(6) . . . . ? C4 N1 Cu1 I1 172.3(6) . . . 2_665 ? C5 N1 Cu1 I1 -11.8(7) . . . 2_665 ? C4 N1 Cu1 Cu1 103.4(7) . . . 2_665 ? C5 N1 Cu1 Cu1 -80.7(8) . . . 2_665 ? C4 N1 Cu1 I2 -75.9(7) . . . 1_554 ? C5 N1 Cu1 I2 99.9(7) . . . 1_554 ? Na1 O10 Na1 O10 0.000(2) 2_576 . . 2_576 ? Na1 O10 Na1 O8 88.6(11) 2_576 . . . ? Na1 O10 Na1 O8 -70.4(11) 2_576 . . 2_576 ? Na1 O10 Na1 O7 -112.3(13) 2_576 . . 2_576 ? Na1 O10 Na1 O4 158.4(13) 2_576 . . 2_676 ? Na1 O10 Na1 C19 -87.5(11) 2_576 . . 2_576 ? Na1 O10 Na1 Gd1 118.2(12) 2_576 . . 2_676 ? C19 O8 Na1 Na1 31.2(15) . . . 2_576 ? Gd1 O8 Na1 Na1 176.4(12) 2_676 . . 2_576 ? C19 O8 Na1 O10 119.0(6) . . . 2_576 ? Gd1 O8 Na1 O10 -95.8(4) 2_676 . . 2_576 ? Na1 O8 Na1 O10 87.8(13) 2_576 . . 2_576 ? C19 O8 Na1 O10 -36.6(6) . . . . ? Gd1 O8 Na1 O10 108.7(4) 2_676 . . . ? Na1 O8 Na1 O10 -67.7(13) 2_576 . . . ? C19 O8 Na1 O8 31.2(15) . . . 2_576 ? Gd1 O8 Na1 O8 176.4(12) 2_676 . . 2_576 ? Na1 O8 Na1 O8 0.000(3) 2_576 . . 2_576 ? C19 O8 Na1 O7 -173.7(9) . . . 2_576 ? Gd1 O8 Na1 O7 -28.5(11) 2_676 . . 2_576 ? Na1 O8 Na1 O7 155(2) 2_576 . . 2_576 ? C19 O8 Na1 O4 -131.9(6) . . . 2_676 ? Gd1 O8 Na1 O4 13.3(4) 2_676 . . 2_676 ? Na1 O8 Na1 O4 -163.1(14) 2_576 . . 2_676 ? C19 O8 Na1 C19 125.2(17) . . . 2_576 ? Gd1 O8 Na1 C19 -89.6(18) 2_676 . . 2_576 ? Na1 O8 Na1 C19 94(2) 2_576 . . 2_576 ? C19 O8 Na1 Gd1 -145.2(7) . . . 2_676 ? Na1 O8 Na1 Gd1 -176.4(12) 2_576 . . 2_676 ? N3 Cu3 I2 Cu1 103.1(2) . . . 1_556 ? I3 Cu3 I2 Cu1 -142.12(6) . . . 1_556 ? I1 Cu3 I2 Cu1 -16.72(4) 1_556 . . 1_556 ? Cu2 Cu3 I2 Cu1 -81.62(6) 2_767 . . 1_556 ? N3 Cu3 I2 Cu1 -76.9(2) . . . 2_766 ? I3 Cu3 I2 Cu1 37.88(6) . . . 2_766 ? I1 Cu3 I2 Cu1 163.28(4) 1_556 . . 2_766 ? Cu2 Cu3 I2 Cu1 98.38(6) 2_767 . . 2_766 ? N3 Cu3 I2 Cu3 -75(100) . . . 2_767 ? I3 Cu3 I2 Cu3 40(100) . . . 2_767 ? I1 Cu3 I2 Cu3 165(100) 1_556 . . 2_767 ? Cu2 Cu3 I2 Cu3 100(100) 2_767 . . 2_767 ? N1 Cu1 I1 Cu1 138.6(2) . . . 2_665 ? I1 Cu1 I1 Cu1 0.0 2_665 . . 2_665 ? I2 Cu1 I1 Cu1 -117.28(7) 1_554 . . 2_665 ? N1 Cu1 I1 Cu3 -121.7(2) . . . 1_554 ? I1 Cu1 I1 Cu3 99.72(6) 2_665 . . 1_554 ? Cu1 Cu1 I1 Cu3 99.72(6) 2_665 . . 1_554 ? I2 Cu1 I1 Cu3 -17.57(4) 1_554 . . 1_554 ? N1 Cu1 I1 Cu2 -69.9(2) . . . 2_766 ? I1 Cu1 I1 Cu2 151.48(6) 2_665 . . 2_766 ? Cu1 Cu1 I1 Cu2 151.48(6) 2_665 . . 2_766 ? I2 Cu1 I1 Cu2 34.20(6) 1_554 . . 2_766 ? C13 O5 Gd1 O6 -10.5(16) . . . 2_766 ? C13 O5 Gd1 O8 -70.2(17) . . . 2_676 ? C13 O5 Gd1 O9 135.8(16) . . . . ? C13 O5 Gd1 O3 -131.8(16) . . . . ? C13 O5 Gd1 O7 173.4(15) . . . . ? C13 O5 Gd1 O1 67.8(17) . . . . ? C13 O5 Gd1 O2 61.2(16) . . . . ? C13 O5 Gd1 O4 -80.0(16) . . . . ? C13 O5 Gd1 Na1 -68.6(17) . . . 2_676 ? C7 O3 Gd1 O5 85.2(5) . . . . ? C7 O3 Gd1 O6 4.1(6) . . . 2_766 ? C7 O3 Gd1 O8 -67.0(5) . . . 2_676 ? C7 O3 Gd1 O9 162.0(5) . . . . ? C7 O3 Gd1 O7 -134.3(6) . . . . ? C7 O3 Gd1 O1 -121.3(6) . . . . ? C7 O3 Gd1 O2 116.8(6) . . . . ? C7 O3 Gd1 O4 -2.0(5) . . . . ? C7 O3 Gd1 Na1 -39.5(5) . . . 2_676 ? C19 O7 Gd1 O5 153.4(5) . . . . ? Na1 O7 Gd1 O5 -83.5(5) 2_576 . . . ? C19 O7 Gd1 O6 -20.7(7) . . . 2_766 ? Na1 O7 Gd1 O6 102.5(5) 2_576 . . 2_766 ? C19 O7 Gd1 O8 4.3(5) . . . 2_676 ? Na1 O7 Gd1 O8 127.5(5) 2_576 . . 2_676 ? C19 O7 Gd1 O9 -165.6(6) . . . . ? Na1 O7 Gd1 O9 -42.4(5) 2_576 . . . ? C19 O7 Gd1 O3 96.7(6) . . . . ? Na1 O7 Gd1 O3 -140.2(5) 2_576 . . . ? C19 O7 Gd1 O1 -75.7(6) . . . . ? Na1 O7 Gd1 O1 47.4(5) 2_576 . . . ? C19 O7 Gd1 O2 -109.0(6) . . . . ? Na1 O7 Gd1 O2 14.2(5) 2_576 . . . ? C19 O7 Gd1 O4 59.4(6) . . . . ? Na1 O7 Gd1 O4 -177.4(5) 2_576 . . . ? C19 O7 Gd1 Na1 24.4(6) . . . 2_676 ? Na1 O7 Gd1 Na1 147.5(5) 2_576 . . 2_676 ? C1 O1 Gd1 O5 -10.2(6) . . . . ? C1 O1 Gd1 O6 70.6(5) . . . 2_766 ? C1 O1 Gd1 O8 148.2(5) . . . 2_676 ? C1 O1 Gd1 O9 -75.9(5) . . . . ? C1 O1 Gd1 O3 -154.7(5) . . . . ? C1 O1 Gd1 O7 -141.7(5) . . . . ? C1 O1 Gd1 O2 -1.9(4) . . . . ? C1 O1 Gd1 O4 118.8(5) . . . . ? C1 O1 Gd1 Na1 131.7(5) . . . 2_676 ? C1 O2 Gd1 O5 175.6(5) . . . . ? C1 O2 Gd1 O6 -93.0(5) . . . 2_766 ? C1 O2 Gd1 O8 -31.4(5) . . . 2_676 ? C1 O2 Gd1 O9 96.3(5) . . . . ? C1 O2 Gd1 O3 144.2(5) . . . . ? C1 O2 Gd1 O7 44.1(5) . . . . ? C1 O2 Gd1 O1 1.9(4) . . . . ? C1 O2 Gd1 O4 -119.7(5) . . . . ? C1 O2 Gd1 Na1 -65.5(5) . . . 2_676 ? C7 O4 Gd1 O5 -80.7(5) . . . . ? Na1 O4 Gd1 O5 164.0(3) 2_676 . . . ? C7 O4 Gd1 O6 -172.4(6) . . . 2_766 ? Na1 O4 Gd1 O6 72.4(3) 2_676 . . 2_766 ? C7 O4 Gd1 O8 104.9(5) . . . 2_676 ? Na1 O4 Gd1 O8 -10.4(3) 2_676 . . 2_676 ? C7 O4 Gd1 O9 -22.3(6) . . . . ? Na1 O4 Gd1 O9 -137.6(3) 2_676 . . . ? C7 O4 Gd1 O3 2.0(5) . . . . ? Na1 O4 Gd1 O3 -113.2(4) 2_676 . . . ? C7 O4 Gd1 O7 50.4(6) . . . . ? Na1 O4 Gd1 O7 -64.9(3) 2_676 . . . ? C7 O4 Gd1 O1 135.6(5) . . . . ? Na1 O4 Gd1 O1 20.3(4) 2_676 . . . ? C7 O4 Gd1 O2 -145.4(5) . . . . ? Na1 O4 Gd1 O2 99.4(4) 2_676 . . . ? C7 O4 Gd1 Na1 115.2(6) . . . 2_676 ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.20 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 1.257 _refine_diff_density_min -1.565 _refine_diff_density_rms 0.206