# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_coden_ASTM ? _journal_coeditor_code ? _journal_coeditor_name ? _journal_coeditor_notes ? _journal_date_accepted ? _journal_date_from_coeditor ? _journal_date_printers_final ? _journal_date_printers_first ? _journal_date_proofs_in ? _journal_date_proofs_out ? #================================================================= # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? _journal_techeditor_code ? _journal_techeditor_notes ? _journal_volume ? _journal_year ? loop_ _publ_author_address ; School of Chemistry and Environment South China Normal University Guangzhou 510006 P.R. China ; #TrackingRef 'cifs.cif' #==================================================================== # 1. SUBMISSION DETAILS _publ_contact_author # Name and address of author for correspondence ; Hong Deng School of Chemistry and Environment South China Nomal University Guangzhou 510006 P. R. China ; _publ_contact_author_email dh@scnu.edu.cn _publ_contact_author_fax '86 20 33381880' _publ_contact_author_phone '86 20 33381880' _publ_contact_letter ;xx Dear Sir or Madam: Please consider this CIF as supplmentary data for a manuscript submitted to ' CrystEngComm '. Deng Hong ; _publ_requested_coeditor_name ? #======================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; ? ; _publ_contact_author_name 'Hong Deng' _publ_author_name 'Hong Deng' data_1 _database_code_depnum_ccdc_archive 'CCDC 752715' _publ_requested_joiurnal ' CrystEngComm ' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H18 Ag3 N8 O8 Tb, 4(H2 O)' _chemical_formula_sum 'C32 H26 Ag3 N8 O12 Tb' _chemical_formula_weight 1197.14 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' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.0731(6) _cell_length_b 5.4794(2) _cell_length_c 21.8203(8) _cell_angle_alpha 90.00 _cell_angle_beta 108.287(2) _cell_angle_gamma 90.00 _cell_volume 1824.68(12) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 5379 _cell_measurement_theta_min 2.669 _cell_measurement_theta_max 27.000 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.179 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1152 _exptl_absorpt_coefficient_mu 3.574 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.481052 _exptl_absorpt_correction_T_max 0.745620 _exptl_absorpt_process_details 'TWINABS (Sheldrick, 2007)' _exptl_special_details ; The crystal under investigation was found to be non-merohedrally twinned. The orientation matrices for the two components were identified using the program Cell_Now, and the two components were integrated using Saint, resulting in a total of 36985 reflections. 12243 reflections (2822 unique ones) involved component 1 only (mean I/sigma = 6.8), 12154 reflections (2826 unique ones) involved component 2 only (mean I/sigma = 3.6), and 12588 reflections (3073 unique ones) involved both components (mean I/sigma = 7.1). The exact twin matrix identified by the integration program was found to be -0.41575 0.01122 0.58084, -0.00157 -0.99973 0.00021, 1.42419 -0.01652 0.41523, which represents a 180 degree rotation around the real axis 1 0 1. The data were corrected for absorption using twinabs, and the structure was solved using direct methods with only the non-overlapping reflections of component 1. The structure was refined using the hklf 5 routine with all reflections of component 1 (including the overlapping ones) below a d-spacing threshold of 0.75, resulting in a BASF value of 0.242(1). The Rint value given is for all reflections before the cutoff at d = 0.75 and is based on agreement between observed single and composite intensities and those calculated from refined unique intensities and twin fractions (TWINABS (Sheldrick, 2007)). The water H atoms were placed in position suggested by possible hydrogen bonding interactions. O-H distances were fixed at 0.84 Angstroms and the H atoms were set to ride on their parent atoms in the final refinement cycles. ; _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 36985 _diffrn_reflns_av_R_equivalents 0.0468 _diffrn_reflns_av_sigmaI/netI 0.0341 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 27.89 _reflns_number_total 4357 _reflns_number_gt 3725 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Apex2 v2.1-4 (Bruker, 2007)' _computing_cell_refinement 'Apex2 v2.1-4' _computing_data_reduction 'Apex2 v2.1-4' _computing_structure_solution 'SHELXTL 6.14 (Bruker, 2000-2003)' _computing_structure_refinement 'SHELXTL 6.14' _computing_molecular_graphics 'SHELXTL 6.14' _computing_publication_material 'SHELXTL 6.14' _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^)+(0.0380P)^2^+8.0723P] 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 4357 _refine_ls_number_parameters 259 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0496 _refine_ls_R_factor_gt 0.0388 _refine_ls_wR_factor_ref 0.0913 _refine_ls_wR_factor_gt 0.0863 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _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 Tb1 Tb 0.5000 0.5000 0.5000 0.02548(10) Uani 1 2 d S . . O4 O 0.4282(3) 0.1923(8) 0.4344(2) 0.0374(10) Uani 1 1 d . . . C7 C 0.2351(3) -0.1678(10) 0.3651(3) 0.0258(11) Uani 1 1 d . . . H7 H 0.2470 -0.3002 0.3932 0.031 Uiso 1 1 calc R . . C1 C 0.3816(3) 0.0006(10) 0.4205(3) 0.0243(11) Uani 1 1 d . . . C3 C 0.2758(4) 0.2184(11) 0.3273(3) 0.0283(12) Uani 1 1 d . . . H3A H 0.3169 0.3427 0.3327 0.034 Uiso 1 1 calc R . . C5 C 0.1384(4) 0.0481(11) 0.2731(3) 0.0283(12) Uani 1 1 d . . . C6 C 0.1563(4) -0.1476(10) 0.3162(3) 0.0271(12) Uani 1 1 d . . . C4 C 0.1982(4) 0.2354(12) 0.2780(3) 0.0319(13) Uani 1 1 d . . . H4A H 0.1863 0.3659 0.2493 0.038 Uiso 1 1 calc R . . C2 C 0.2954(3) 0.0164(10) 0.3704(3) 0.0244(11) Uani 1 1 d . . . N2 N 0.0552(3) 0.0064(10) 0.2303(3) 0.0373(12) Uani 1 1 d . . . H2 H 0.0275 0.0960 0.1980 0.045 Uiso 1 1 calc R . . N3 N 0.0831(3) -0.3027(10) 0.3006(2) 0.0346(12) Uani 1 1 d . . . C14 C 0.0268(4) -0.2020(13) 0.2494(3) 0.0398(15) Uani 1 1 d . . . H14A H -0.0279 -0.2692 0.2283 0.048 Uiso 1 1 calc R . . C15 C 0.3900(4) 0.2561(13) 0.5954(3) 0.0366(14) Uani 1 1 d . . . O1 O 0.4315(3) 0.2068(11) 0.6531(2) 0.0534(14) Uani 1 1 d . . . O3 O 0.4159(3) 0.4067(9) 0.5615(2) 0.0415(11) Uani 1 1 d . . . O2 O 0.4059(3) -0.2048(8) 0.4458(2) 0.0407(11) Uani 1 1 d . . . Ag1 Ag 0.07690(3) 0.41043(10) 0.36233(2) 0.03847(13) Uani 1 1 d . . . N1 N 0.0940(3) 0.1343(10) 0.4307(2) 0.0348(12) Uani 1 1 d . . . C12 C 0.2856(4) -0.0863(13) 0.5957(3) 0.0446(16) Uani 1 1 d . . . H12 H 0.3267 -0.1429 0.6333 0.053 Uiso 1 1 calc R . . C8 C 0.1650(4) 0.0928(12) 0.4842(3) 0.0295(12) Uani 1 1 d . . . C10 C 0.1480(4) -0.1212(12) 0.5144(3) 0.0331(13) Uani 1 1 d . . . C9 C 0.2447(4) 0.2158(12) 0.5095(3) 0.0329(13) Uani 1 1 d . . . H9 H 0.2572 0.3535 0.4890 0.039 Uiso 1 1 calc R . . C11 C 0.2087(4) -0.2106(14) 0.5707(3) 0.0464(17) Uani 1 1 d . . . H11 H 0.1970 -0.3507 0.5907 0.056 Uiso 1 1 calc R . . N4 N 0.0671(3) -0.2078(11) 0.4782(3) 0.0381(12) Uani 1 1 d . . . C13 C 0.0384(4) -0.0476(11) 0.4304(3) 0.0359(14) Uani 1 1 d . . . H13 H -0.0162 -0.0610 0.3991 0.043 Uiso 1 1 calc R . . C16 C 0.3044(4) 0.1290(12) 0.5653(3) 0.0352(14) Uani 1 1 d . . . O6 O 0.3416(7) 0.693(3) 0.7991(6) 0.170(5) Uani 1 1 d . . . H6A H 0.3351 0.8451 0.7989 0.256 Uiso 1 1 d R . . H6B H 0.3070 0.5738 0.7922 0.256 Uiso 1 1 d R . . O5 O 0.3716(8) 0.186(2) 0.7599(6) 0.163(5) Uani 1 1 d . . . H5A H 0.3714 0.2246 0.7226 0.245 Uiso 1 1 d R . . H5B H 0.3912 0.2909 0.7888 0.245 Uiso 1 1 d R . . Ag2 Ag 0.0000 -0.5000 0.5000 0.04192(18) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tb1 0.02135(18) 0.01633(17) 0.0321(2) 0.00371(15) -0.00121(13) -0.00516(14) O4 0.040(2) 0.025(2) 0.037(2) -0.0018(18) -0.0030(17) -0.0122(19) C7 0.028(3) 0.019(3) 0.026(3) 0.002(2) 0.002(2) 0.000(2) C1 0.010(2) 0.023(3) 0.040(3) -0.002(2) 0.0074(19) -0.003(2) C3 0.033(3) 0.021(3) 0.030(3) 0.004(2) 0.009(2) -0.003(2) C5 0.028(3) 0.026(3) 0.027(3) 0.000(2) 0.003(2) 0.004(2) C6 0.028(3) 0.022(3) 0.029(3) -0.002(2) 0.006(2) -0.002(2) C4 0.038(3) 0.027(3) 0.027(3) 0.006(2) 0.006(2) 0.007(3) C2 0.026(2) 0.018(3) 0.026(2) -0.001(2) 0.004(2) 0.002(2) N2 0.030(3) 0.039(3) 0.035(3) 0.004(2) -0.002(2) 0.006(2) N3 0.023(2) 0.035(3) 0.040(3) 0.001(2) 0.002(2) -0.005(2) C14 0.023(3) 0.044(4) 0.042(3) -0.006(3) -0.006(2) 0.000(3) C15 0.034(3) 0.034(3) 0.039(3) -0.002(3) 0.008(3) -0.006(3) O1 0.053(3) 0.060(4) 0.037(2) -0.003(2) -0.001(2) -0.026(3) O3 0.034(2) 0.040(3) 0.051(3) 0.002(2) 0.014(2) -0.012(2) O2 0.030(2) 0.025(2) 0.054(3) 0.010(2) -0.0054(19) -0.0001(18) Ag1 0.0364(3) 0.0334(3) 0.0428(3) 0.0031(2) 0.00836(19) -0.0061(2) N1 0.035(3) 0.034(3) 0.035(3) -0.001(2) 0.010(2) -0.007(2) C12 0.042(4) 0.038(4) 0.045(4) 0.007(3) 0.002(3) -0.012(3) C8 0.035(3) 0.025(3) 0.029(3) -0.006(2) 0.011(2) -0.007(3) C10 0.035(3) 0.029(3) 0.038(3) 0.001(3) 0.017(3) -0.009(3) C9 0.034(3) 0.033(3) 0.034(3) -0.003(3) 0.013(2) -0.010(3) C11 0.050(4) 0.035(4) 0.050(4) 0.008(3) 0.011(3) -0.015(3) N4 0.035(3) 0.033(3) 0.046(3) -0.004(3) 0.012(2) -0.014(2) C13 0.033(3) 0.028(3) 0.047(4) -0.008(3) 0.012(3) -0.010(3) C16 0.033(3) 0.034(4) 0.038(3) -0.003(3) 0.010(3) -0.011(3) O6 0.132(8) 0.179(12) 0.232(14) 0.016(11) 0.104(9) 0.009(9) O5 0.239(13) 0.129(9) 0.174(10) -0.016(8) 0.139(10) -0.035(9) Ag2 0.0391(4) 0.0330(4) 0.0544(4) -0.0043(3) 0.0159(3) -0.0173(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 Tb1 O3 2.243(4) . ? Tb1 O3 2.243(4) 3_666 ? Tb1 O2 2.275(4) 3_656 ? Tb1 O2 2.275(4) 1_565 ? Tb1 O4 2.277(4) . ? Tb1 O4 2.277(4) 3_666 ? O4 C1 1.270(7) . ? C7 C2 1.378(8) . ? C7 C6 1.381(7) . ? C7 H7 0.9300 . ? C1 O2 1.261(7) . ? C1 C2 1.474(7) . ? C3 C4 1.371(8) . ? C3 C2 1.423(8) . ? C3 H3A 0.9300 . ? C5 C4 1.388(9) . ? C5 N2 1.388(7) . ? C5 C6 1.396(8) . ? C6 N3 1.404(7) . ? C4 H4A 0.9300 . ? N2 C14 1.344(9) . ? N2 H2 0.8600 . ? N3 C14 1.319(8) . ? N3 Ag1 2.092(5) 1_545 ? C14 H14A 0.9300 . ? C15 O1 1.254(8) . ? C15 O3 1.263(8) . ? C15 C16 1.499(8) . ? O2 Tb1 2.275(4) 1_545 ? Ag1 N1 2.082(5) . ? Ag1 N3 2.092(5) 1_565 ? N1 C13 1.338(8) . ? N1 C8 1.370(8) . ? C12 C11 1.366(9) . ? C12 C16 1.431(9) . ? C12 H12 0.9300 . ? C8 C9 1.400(8) . ? C8 C10 1.413(9) . ? C10 N4 1.376(7) . ? C10 C11 1.397(9) . ? C9 C16 1.377(9) . ? C9 H9 0.9300 . ? C11 H11 0.9300 . ? N4 C13 1.331(8) . ? N4 Ag2 2.068(5) . ? C13 H13 0.9300 . ? O6 H6A 0.8400 . ? O6 H6B 0.8400 . ? O5 H5A 0.8400 . ? O5 H5B 0.8400 . ? Ag2 N4 2.068(5) 3_546 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Tb1 O3 180.00(15) . 3_666 ? O3 Tb1 O2 87.38(17) . 3_656 ? O3 Tb1 O2 92.62(17) 3_666 3_656 ? O3 Tb1 O2 92.62(17) . 1_565 ? O3 Tb1 O2 87.38(17) 3_666 1_565 ? O2 Tb1 O2 179.999(1) 3_656 1_565 ? O3 Tb1 O4 85.70(17) . . ? O3 Tb1 O4 94.30(17) 3_666 . ? O2 Tb1 O4 85.60(16) 3_656 . ? O2 Tb1 O4 94.40(16) 1_565 . ? O3 Tb1 O4 94.30(17) . 3_666 ? O3 Tb1 O4 85.70(17) 3_666 3_666 ? O2 Tb1 O4 94.40(16) 3_656 3_666 ? O2 Tb1 O4 85.60(16) 1_565 3_666 ? O4 Tb1 O4 180.00(19) . 3_666 ? C1 O4 Tb1 155.1(4) . . ? C2 C7 C6 117.2(5) . . ? C2 C7 H7 121.4 . . ? C6 C7 H7 121.4 . . ? O2 C1 O4 123.7(5) . . ? O2 C1 C2 117.9(5) . . ? O4 C1 C2 118.4(5) . . ? C4 C3 C2 122.0(6) . . ? C4 C3 H3A 119.0 . . ? C2 C3 H3A 119.0 . . ? C4 C5 N2 132.2(5) . . ? C4 C5 C6 121.7(5) . . ? N2 C5 C6 106.2(5) . . ? C7 C6 C5 121.8(5) . . ? C7 C6 N3 129.3(5) . . ? C5 C6 N3 108.8(5) . . ? C3 C4 C5 116.6(6) . . ? C3 C4 H4A 121.7 . . ? C5 C4 H4A 121.7 . . ? C7 C2 C3 120.7(5) . . ? C7 C2 C1 119.5(5) . . ? C3 C2 C1 119.8(5) . . ? C14 N2 C5 106.3(5) . . ? C14 N2 H2 126.9 . . ? C5 N2 H2 126.9 . . ? C14 N3 C6 104.6(5) . . ? C14 N3 Ag1 134.5(4) . 1_545 ? C6 N3 Ag1 120.3(4) . 1_545 ? N3 C14 N2 114.1(5) . . ? N3 C14 H14A 122.9 . . ? N2 C14 H14A 122.9 . . ? O1 C15 O3 124.0(6) . . ? O1 C15 C16 117.7(6) . . ? O3 C15 C16 118.2(6) . . ? C15 O3 Tb1 150.5(5) . . ? C1 O2 Tb1 157.9(4) . 1_545 ? N1 Ag1 N3 170.05(19) . 1_565 ? C13 N1 C8 104.9(5) . . ? C13 N1 Ag1 126.8(4) . . ? C8 N1 Ag1 128.2(4) . . ? C11 C12 C16 121.4(6) . . ? C11 C12 H12 119.3 . . ? C16 C12 H12 119.3 . . ? N1 C8 C9 132.1(6) . . ? N1 C8 C10 107.7(5) . . ? C9 C8 C10 120.1(6) . . ? N4 C10 C11 131.0(6) . . ? N4 C10 C8 107.7(5) . . ? C11 C10 C8 121.2(5) . . ? C16 C9 C8 118.7(6) . . ? C16 C9 H9 120.7 . . ? C8 C9 H9 120.7 . . ? C12 C11 C10 118.1(6) . . ? C12 C11 H11 120.9 . . ? C10 C11 H11 120.9 . . ? C13 N4 C10 104.8(5) . . ? C13 N4 Ag2 127.8(4) . . ? C10 N4 Ag2 127.1(4) . . ? N4 C13 N1 114.8(6) . . ? N4 C13 H13 122.6 . . ? N1 C13 H13 122.6 . . ? C9 C16 C12 120.4(5) . . ? C9 C16 C15 121.1(6) . . ? C12 C16 C15 118.6(6) . . ? H6A O6 H6B 134.2 . . ? H5A O5 H5B 116.0 . . ? N4 Ag2 N4 180.0(3) 3_546 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Tb1 O4 C1 -18.4(9) . . . . ? O3 Tb1 O4 C1 161.6(9) 3_666 . . . ? O2 Tb1 O4 C1 69.3(9) 3_656 . . . ? O2 Tb1 O4 C1 -110.7(9) 1_565 . . . ? Tb1 O4 C1 O2 -65.7(12) . . . . ? Tb1 O4 C1 C2 116.4(9) . . . . ? C2 C7 C6 C5 1.1(9) . . . . ? C2 C7 C6 N3 -178.3(6) . . . . ? C4 C5 C6 C7 -1.4(9) . . . . ? N2 C5 C6 C7 178.7(5) . . . . ? C4 C5 C6 N3 178.1(5) . . . . ? N2 C5 C6 N3 -1.8(7) . . . . ? C2 C3 C4 C5 1.5(9) . . . . ? N2 C5 C4 C3 179.9(6) . . . . ? C6 C5 C4 C3 0.1(9) . . . . ? C6 C7 C2 C3 0.5(8) . . . . ? C6 C7 C2 C1 -178.3(5) . . . . ? C4 C3 C2 C7 -1.8(9) . . . . ? C4 C3 C2 C1 176.9(5) . . . . ? O2 C1 C2 C7 17.6(8) . . . . ? O4 C1 C2 C7 -164.4(5) . . . . ? O2 C1 C2 C3 -161.1(5) . . . . ? O4 C1 C2 C3 16.9(8) . . . . ? C4 C5 N2 C14 -178.7(7) . . . . ? C6 C5 N2 C14 1.2(7) . . . . ? C7 C6 N3 C14 -178.9(6) . . . . ? C5 C6 N3 C14 1.7(7) . . . . ? C7 C6 N3 Ag1 8.5(8) . . . 1_545 ? C5 C6 N3 Ag1 -170.9(4) . . . 1_545 ? C6 N3 C14 N2 -0.9(8) . . . . ? Ag1 N3 C14 N2 170.1(5) 1_545 . . . ? C5 N2 C14 N3 -0.2(8) . . . . ? O1 C15 O3 Tb1 80.3(11) . . . . ? C16 C15 O3 Tb1 -100.1(9) . . . . ? O2 Tb1 O3 C15 -25.8(9) 3_656 . . . ? O2 Tb1 O3 C15 154.2(9) 1_565 . . . ? O4 Tb1 O3 C15 60.0(9) . . . . ? O4 Tb1 O3 C15 -120.0(9) 3_666 . . . ? O4 C1 O2 Tb1 -18.9(16) . . . 1_545 ? C2 C1 O2 Tb1 159.0(9) . . . 1_545 ? C13 N1 C8 C9 178.4(7) . . . . ? Ag1 N1 C8 C9 0.5(10) . . . . ? C13 N1 C8 C10 0.3(7) . . . . ? Ag1 N1 C8 C10 -177.6(4) . . . . ? N1 C8 C10 N4 0.6(7) . . . . ? C9 C8 C10 N4 -177.7(6) . . . . ? N1 C8 C10 C11 -179.8(6) . . . . ? C9 C8 C10 C11 1.9(10) . . . . ? N1 C8 C9 C16 179.8(6) . . . . ? C10 C8 C9 C16 -2.3(9) . . . . ? C16 C12 C11 C10 -0.2(12) . . . . ? N4 C10 C11 C12 178.9(7) . . . . ? C8 C10 C11 C12 -0.6(11) . . . . ? C11 C10 N4 C13 179.1(7) . . . . ? C8 C10 N4 C13 -1.3(7) . . . . ? C11 C10 N4 Ag2 5.5(11) . . . . ? C8 C10 N4 Ag2 -175.0(4) . . . . ? C10 N4 C13 N1 1.6(8) . . . . ? Ag2 N4 C13 N1 175.2(4) . . . . ? C8 N1 C13 N4 -1.2(8) . . . . ? Ag1 N1 C13 N4 176.7(4) . . . . ? C8 C9 C16 C12 1.5(10) . . . . ? C8 C9 C16 C15 -178.7(6) . . . . ? C11 C12 C16 C9 -0.2(11) . . . . ? C11 C12 C16 C15 180.0(7) . . . . ? O1 C15 C16 C9 162.9(6) . . . . ? O3 C15 C16 C9 -16.7(10) . . . . ? O1 C15 C16 C12 -17.3(10) . . . . ? O3 C15 C16 C12 163.1(6) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O6 H6B O5 0.84 2.80 3.261(16) 116.0 2_556 O6 H6A O5 0.84 2.20 2.917(17) 142.7 1_565 O5 H5B O6 0.84 2.38 2.993(17) 130.5 . O5 H5A O1 0.84 2.04 2.790(11) 148.0 . N2 H2 O1 0.86 1.89 2.676(7) 151.9 4_565 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.89 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.678 _refine_diff_density_min -1.090 _refine_diff_density_rms 0.135 data_4 _database_code_depnum_ccdc_archive 'CCDC 782273' #TrackingRef 'cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H19 Ag2 Eu N6 O9' _chemical_formula_sum 'C26 H19 Ag2 Eu N6 O9' _chemical_formula_weight 927.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M p-1 _symmetry_space_group_name_Hall '-p 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.8964(9) _cell_length_b 12.3459(13) _cell_length_c 13.8600(14) _cell_angle_alpha 72.9500(10) _cell_angle_beta 84.2720(10) _cell_angle_gamma 71.6480(10) _cell_volume 1381.3(2) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4875 _cell_measurement_theta_min 1.81 _cell_measurement_theta_max 25.20 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.229 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 892 _exptl_absorpt_coefficient_mu 3.713 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.420 _exptl_absorpt_correction_T_max 0.481 _exptl_absorpt_process_details 'Apex2 (Bruker, 2005)' _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_reflns_number 7066 _diffrn_reflns_av_R_equivalents 0.0133 _diffrn_reflns_av_sigmaI/netI 0.0281 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 25.20 _reflns_number_total 4873 _reflns_number_gt 4275 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (Bruker, 2005)' _computing_cell_refinement 'Apex2 (Bruker, 2005)' _computing_data_reduction 'Apex2 (Bruker, 2005)' _computing_structure_solution 'SHELXTL 6.12 (Bruker, 2000-2003)' _computing_structure_refinement 'SHELXTL 6.12' _computing_molecular_graphics 'SHELXTL 6.12' _computing_publication_material 'SHELXTL 6.12' _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^)+(0.0287P)^2^+8.2069P] 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 4873 _refine_ls_number_parameters 398 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0418 _refine_ls_R_factor_gt 0.0352 _refine_ls_wR_factor_ref 0.0832 _refine_ls_wR_factor_gt 0.0790 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _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 Eu1 Eu 0.42219(4) 0.08080(2) 0.86133(2) 0.02696(10) Uani 1 1 d . . . Ag1 Ag -0.29675(7) 0.50127(5) 0.87347(3) 0.04278(15) Uani 1 1 d . . . Ag2 Ag -0.04235(7) -0.26594(5) 0.45749(4) 0.04973(16) Uani 1 1 d . . . C1 C 0.2599(7) 0.1679(5) 1.0692(4) 0.0290(13) Uani 1 1 d . . . C2 C 0.1321(7) 0.2634(5) 1.1026(4) 0.0265(12) Uani 1 1 d . . . C3 C 0.1423(8) 0.2866(5) 1.1953(4) 0.0347(14) Uani 1 1 d . . . H3 H 0.2286 0.2406 1.2368 0.042 Uiso 1 1 calc R . . C4 C 0.0275(8) 0.3759(5) 1.2261(4) 0.0346(14) Uani 1 1 d . . . H4 H 0.0369 0.3926 1.2860 0.042 Uiso 1 1 calc R . . C5 C -0.1021(7) 0.4391(5) 1.1637(4) 0.0296(13) Uani 1 1 d . . . C6 C -0.1151(7) 0.4149(5) 1.0726(4) 0.0266(12) Uani 1 1 d . . . C7 C 0.0043(7) 0.3285(5) 1.0405(4) 0.0274(12) Uani 1 1 d . . . H7 H -0.0020 0.3151 0.9786 0.033 Uiso 1 1 calc R . . C8 C -0.3209(8) 0.5595(5) 1.0848(5) 0.0370(15) Uani 1 1 d . . . H8 H -0.4161 0.6203 1.0706 0.044 Uiso 1 1 calc R . . C9 C 0.2149(8) 0.0050(6) 0.7678(5) 0.0415(16) Uani 1 1 d . . . C10 C 0.1210(7) -0.0322(5) 0.7056(5) 0.0334(14) Uani 1 1 d . . . C11 C -0.0418(8) 0.0134(6) 0.6992(5) 0.0398(16) Uani 1 1 d . . . H11 H -0.0983 0.0708 0.7311 0.048 Uiso 1 1 calc R . . C12 C -0.1184(8) -0.0307(5) 0.6424(4) 0.0342(14) Uani 1 1 d . . . C13 C -0.0321(7) -0.1165(6) 0.5946(5) 0.0343(14) Uani 1 1 d . . . C14 C 0.1323(8) -0.1632(6) 0.6017(5) 0.0447(17) Uani 1 1 d . . . H14 H 0.1895 -0.2205 0.5699 0.054 Uiso 1 1 calc R . . C15 C 0.2040(8) -0.1203(6) 0.6576(5) 0.0442(17) Uani 1 1 d . . . H15 H 0.3134 -0.1504 0.6646 0.053 Uiso 1 1 calc R . . C16 C -0.2759(8) -0.0808(6) 0.5623(5) 0.0386(15) Uani 1 1 d . . . H16 H -0.3678 -0.0838 0.5379 0.046 Uiso 1 1 calc R . . C17 C 0.3849(7) 0.2528(5) 0.6645(4) 0.0309(13) Uani 1 1 d . . . C18 C 0.3629(8) 0.3307(5) 0.5587(4) 0.0320(14) Uani 1 1 d . . . C19 C 0.2485(8) 0.4408(5) 0.5353(4) 0.0381(15) Uani 1 1 d . . . H19 H 0.1906 0.4711 0.5863 0.046 Uiso 1 1 calc R . . C20 C 0.2219(8) 0.5050(5) 0.4348(5) 0.0368(15) Uani 1 1 d . . . C21 C 0.3123(8) 0.4606(5) 0.3576(4) 0.0368(15) Uani 1 1 d . . . C22 C 0.4283(8) 0.3512(6) 0.3808(5) 0.0428(17) Uani 1 1 d . . . H22 H 0.4879 0.3212 0.3302 0.051 Uiso 1 1 calc R . . C23 C 0.4525(8) 0.2890(6) 0.4801(4) 0.0377(15) Uani 1 1 d . . . H23 H 0.5313 0.2162 0.4965 0.045 Uiso 1 1 calc R . . C24 C 0.1423(9) 0.6265(6) 0.2904(5) 0.0488(19) Uani 1 1 d . . . H24 H 0.0846 0.6925 0.2419 0.059 Uiso 1 1 calc R . . C25 C 0.6807(8) 0.1326(5) 0.9310(5) 0.0379(15) Uani 1 1 d . . . C26 C 0.8250(9) 0.1506(8) 0.9627(6) 0.062(2) Uani 1 1 d . . . H26A H 0.9089 0.1351 0.9147 0.092 Uiso 1 1 calc R . . H26B H 0.8575 0.0971 1.0281 0.092 Uiso 1 1 calc R . . H26C H 0.8012 0.2310 0.9656 0.092 Uiso 1 1 calc R . . N1 N -0.2552(6) 0.4914(4) 1.0251(4) 0.0318(11) Uani 1 1 d . . . N2 N -0.2367(6) 0.5324(4) 1.1682(4) 0.0372(13) Uani 1 1 d . . . H2 H -0.2615 0.5666 1.2159 0.045 Uiso 1 1 calc R . . N3 N -0.2744(6) -0.0098(5) 0.6190(4) 0.0394(13) Uani 1 1 d . . . H3A H -0.3558 0.0397 0.6375 0.047 Uiso 1 1 calc R . . N4 N -0.1332(6) -0.1456(5) 0.5449(4) 0.0374(12) Uani 1 1 d . . . N5 N 0.1140(8) 0.6124(5) 0.3886(4) 0.0489(16) Uani 1 1 d . . . N6 N 0.2588(7) 0.5400(5) 0.2660(4) 0.0418(14) Uani 1 1 d . . . O1 O 0.2698(5) 0.1806(4) 0.9750(3) 0.0377(11) Uani 1 1 d . . . O2 O 0.3459(5) 0.0850(4) 1.1351(3) 0.0345(10) Uani 1 1 d . . . O3 O 0.1534(6) 0.0979(5) 0.7950(4) 0.0551(13) Uani 1 1 d . . . O4 O 0.3543(6) -0.0560(4) 0.7879(4) 0.0501(12) Uani 1 1 d . . . O5 O 0.3155(5) 0.2901(3) 0.7371(3) 0.0356(10) Uani 1 1 d . . . O6 O 0.4697(5) 0.1457(4) 0.6796(3) 0.0410(11) Uani 1 1 d . . . O7 O 0.6302(7) 0.1803(5) 0.8435(4) 0.0628(16) Uani 1 1 d . . . O8 O 0.6097(5) 0.0687(4) 0.9951(3) 0.0360(10) Uani 1 1 d . . . O1W O -0.5377(7) 0.6954(5) 0.8748(5) 0.0688(17) Uani 1 1 d . . . H1W H -0.6240 0.6821 0.8701 0.103 Uiso 1 1 d R . . H2W H -0.5502 0.7698 0.8514 0.103 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 Eu1 0.03328(17) 0.02140(15) 0.01944(15) -0.00592(11) 0.00269(11) 0.00044(12) Ag1 0.0552(3) 0.0406(3) 0.0241(2) -0.0093(2) -0.0010(2) -0.0022(2) Ag2 0.0610(4) 0.0366(3) 0.0395(3) -0.0171(2) 0.0009(2) 0.0078(3) C1 0.030(3) 0.023(3) 0.031(3) -0.010(2) 0.000(2) -0.001(2) C2 0.030(3) 0.018(3) 0.024(3) -0.003(2) 0.002(2) 0.000(2) C3 0.043(4) 0.027(3) 0.025(3) -0.005(2) -0.002(3) -0.001(3) C4 0.047(4) 0.031(3) 0.023(3) -0.012(2) 0.002(3) -0.003(3) C5 0.038(3) 0.024(3) 0.025(3) -0.009(2) 0.008(2) -0.006(3) C6 0.032(3) 0.020(3) 0.022(3) -0.003(2) 0.005(2) -0.004(2) C7 0.038(3) 0.020(3) 0.024(3) -0.011(2) 0.006(2) -0.006(2) C8 0.036(4) 0.028(3) 0.038(4) -0.011(3) 0.002(3) 0.005(3) C9 0.049(4) 0.029(3) 0.037(4) -0.006(3) 0.005(3) -0.002(3) C10 0.033(3) 0.032(3) 0.032(3) -0.010(3) 0.000(3) -0.004(3) C11 0.043(4) 0.035(3) 0.030(3) -0.010(3) 0.010(3) 0.002(3) C12 0.038(4) 0.033(3) 0.027(3) -0.003(3) 0.000(3) -0.010(3) C13 0.028(3) 0.037(3) 0.031(3) -0.005(3) 0.003(3) -0.005(3) C14 0.043(4) 0.039(4) 0.046(4) -0.017(3) 0.004(3) -0.001(3) C15 0.037(4) 0.043(4) 0.049(4) -0.020(3) 0.007(3) -0.003(3) C16 0.036(4) 0.038(4) 0.036(3) -0.012(3) -0.004(3) -0.001(3) C17 0.041(4) 0.025(3) 0.020(3) -0.007(2) 0.002(2) -0.001(3) C18 0.043(4) 0.025(3) 0.021(3) -0.006(2) 0.003(3) -0.001(3) C19 0.053(4) 0.030(3) 0.022(3) -0.010(3) 0.003(3) 0.003(3) C20 0.048(4) 0.024(3) 0.027(3) -0.007(2) 0.000(3) 0.005(3) C21 0.053(4) 0.030(3) 0.022(3) -0.008(2) 0.000(3) -0.005(3) C22 0.057(4) 0.032(3) 0.024(3) -0.010(3) 0.009(3) 0.007(3) C23 0.039(4) 0.032(3) 0.027(3) -0.007(3) -0.001(3) 0.009(3) C24 0.072(5) 0.030(4) 0.027(3) -0.006(3) -0.005(3) 0.007(3) C25 0.044(4) 0.029(3) 0.038(4) -0.007(3) 0.008(3) -0.011(3) C26 0.052(5) 0.087(6) 0.053(5) -0.013(4) 0.001(4) -0.036(5) N1 0.035(3) 0.026(3) 0.028(3) -0.010(2) 0.002(2) 0.000(2) N2 0.043(3) 0.029(3) 0.032(3) -0.017(2) 0.004(2) 0.006(2) N3 0.036(3) 0.034(3) 0.036(3) -0.012(2) 0.008(2) 0.006(2) N4 0.035(3) 0.039(3) 0.032(3) -0.014(2) -0.001(2) 0.001(2) N5 0.070(4) 0.031(3) 0.026(3) -0.010(2) 0.000(3) 0.014(3) N6 0.060(4) 0.029(3) 0.022(3) -0.005(2) -0.001(2) 0.004(3) O1 0.044(3) 0.032(2) 0.024(2) -0.0121(18) 0.0031(18) 0.0089(19) O2 0.036(2) 0.030(2) 0.028(2) -0.0086(18) 0.0016(18) 0.0034(18) O3 0.057(3) 0.049(3) 0.059(3) -0.028(3) -0.001(3) -0.004(3) O4 0.048(3) 0.043(3) 0.055(3) -0.016(2) -0.011(2) -0.002(2) O5 0.050(3) 0.027(2) 0.022(2) -0.0087(17) 0.0035(18) 0.0011(19) O6 0.054(3) 0.025(2) 0.025(2) -0.0045(17) 0.0059(19) 0.010(2) O7 0.077(4) 0.070(4) 0.041(3) 0.014(3) -0.011(3) -0.046(3) O8 0.045(3) 0.032(2) 0.030(2) -0.0069(18) 0.0061(19) -0.013(2) O1W 0.059(4) 0.038(3) 0.091(4) -0.009(3) 0.008(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 Eu1 O1 2.345(4) . ? Eu1 O8 2.347(4) 2_657 ? Eu1 O2 2.398(4) 2_657 ? Eu1 O6 2.445(4) . ? Eu1 O4 2.454(5) . ? Eu1 O7 2.481(5) . ? Eu1 O8 2.558(4) . ? Eu1 O3 2.572(5) . ? Eu1 O5 2.591(4) . ? Eu1 Eu1 3.9368(6) 2_657 ? Ag1 N6 2.110(5) 2_566 ? Ag1 N1 2.131(5) . ? Ag2 N5 2.089(5) 1_545 ? Ag2 N4 2.106(5) . ? C1 O2 1.251(7) . ? C1 O1 1.266(7) . ? C1 C2 1.506(7) . ? C2 C7 1.376(8) . ? C2 C3 1.412(8) . ? C3 C4 1.386(8) . ? C3 H3 0.9300 . ? C4 C5 1.387(9) . ? C4 H4 0.9300 . ? C5 N2 1.387(7) . ? C5 C6 1.404(8) . ? C6 C7 1.391(7) . ? C6 N1 1.391(7) . ? C7 H7 0.9300 . ? C8 N1 1.318(7) . ? C8 N2 1.341(8) . ? C8 H8 0.9300 . ? C9 O4 1.241(8) . ? C9 O3 1.255(8) . ? C9 C10 1.506(10) . ? C10 C11 1.380(9) . ? C10 C15 1.411(9) . ? C11 C12 1.405(9) . ? C11 H11 0.9300 . ? C12 N3 1.383(8) . ? C12 C13 1.396(9) . ? C13 N4 1.373(8) . ? C13 C14 1.395(9) . ? C14 C15 1.357(10) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 N4 1.312(8) . ? C16 N3 1.341(8) . ? C16 H16 0.9300 . ? C17 O5 1.254(7) . ? C17 O6 1.266(7) . ? C17 C18 1.492(8) . ? C18 C19 1.388(8) . ? C18 C23 1.408(8) . ? C19 C20 1.388(8) . ? C19 H19 0.9300 . ? C20 N5 1.382(8) . ? C20 C21 1.410(8) . ? C21 N6 1.377(8) . ? C21 C22 1.388(9) . ? C22 C23 1.366(8) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 N5 1.329(8) . ? C24 N6 1.332(8) . ? C24 H24 0.9300 . ? C25 O7 1.242(8) . ? C25 O8 1.266(7) . ? C25 C26 1.497(10) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? N2 H2 0.8600 . ? N3 H3A 0.8600 . ? N5 Ag2 2.089(5) 1_565 ? N6 Ag1 2.110(5) 2_566 ? O2 Eu1 2.398(4) 2_657 ? O8 Eu1 2.347(4) 2_657 ? O1W H1W 0.8455 . ? O1W H2W 0.8543 . ? 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 Eu1 O8 74.44(14) . 2_657 ? O1 Eu1 O2 137.98(14) . 2_657 ? O8 Eu1 O2 74.95(14) 2_657 2_657 ? O1 Eu1 O6 132.36(13) . . ? O8 Eu1 O6 149.42(15) 2_657 . ? O2 Eu1 O6 86.46(13) 2_657 . ? O1 Eu1 O4 127.24(17) . . ? O8 Eu1 O4 77.58(16) 2_657 . ? O2 Eu1 O4 71.92(16) 2_657 . ? O6 Eu1 O4 73.61(17) . . ? O1 Eu1 O7 93.85(19) . . ? O8 Eu1 O7 123.85(16) 2_657 . ? O2 Eu1 O7 80.11(18) 2_657 . ? O6 Eu1 O7 74.92(17) . . ? O4 Eu1 O7 138.69(19) . . ? O1 Eu1 O8 72.56(14) . . ? O8 Eu1 O8 73.31(16) 2_657 . ? O2 Eu1 O8 71.54(14) 2_657 . ? O6 Eu1 O8 123.79(15) . . ? O4 Eu1 O8 137.86(14) . . ? O7 Eu1 O8 51.12(15) . . ? O1 Eu1 O3 84.76(16) . . ? O8 Eu1 O3 89.99(17) 2_657 . ? O2 Eu1 O3 123.22(15) 2_657 . ? O6 Eu1 O3 80.02(17) . . ? O4 Eu1 O3 51.33(16) . . ? O7 Eu1 O3 144.53(17) . . ? O8 Eu1 O3 154.61(15) . . ? O1 Eu1 O5 81.11(13) . . ? O8 Eu1 O5 150.73(14) 2_657 . ? O2 Eu1 O5 134.16(13) 2_657 . ? O6 Eu1 O5 51.26(12) . . ? O4 Eu1 O5 105.89(15) . . ? O7 Eu1 O5 73.01(16) . . ? O8 Eu1 O5 114.46(14) . . ? O3 Eu1 O5 71.75(16) . . ? O1 Eu1 Eu1 69.22(10) . 2_657 ? O8 Eu1 Eu1 38.49(11) 2_657 2_657 ? O2 Eu1 Eu1 68.87(10) 2_657 2_657 ? O6 Eu1 Eu1 151.00(11) . 2_657 ? O4 Eu1 Eu1 110.70(12) . 2_657 ? O7 Eu1 Eu1 85.66(11) . 2_657 ? O8 Eu1 Eu1 34.83(9) . 2_657 ? O3 Eu1 Eu1 125.93(12) . 2_657 ? O5 Eu1 Eu1 142.10(9) . 2_657 ? N6 Ag1 N1 158.8(2) 2_566 . ? N5 Ag2 N4 162.1(2) 1_545 . ? O2 C1 O1 126.2(5) . . ? O2 C1 C2 118.3(5) . . ? O1 C1 C2 115.5(5) . . ? C7 C2 C3 120.3(5) . . ? C7 C2 C1 118.5(5) . . ? C3 C2 C1 121.2(5) . . ? C4 C3 C2 121.9(6) . . ? C4 C3 H3 119.1 . . ? C2 C3 H3 119.1 . . ? C3 C4 C5 117.1(5) . . ? C3 C4 H4 121.5 . . ? C5 C4 H4 121.5 . . ? N2 C5 C4 133.8(5) . . ? N2 C5 C6 104.8(5) . . ? C4 C5 C6 121.4(5) . . ? C7 C6 N1 129.7(5) . . ? C7 C6 C5 120.9(5) . . ? N1 C6 C5 109.4(5) . . ? C2 C7 C6 118.3(5) . . ? C2 C7 H7 120.8 . . ? C6 C7 H7 120.8 . . ? N1 C8 N2 113.2(5) . . ? N1 C8 H8 123.4 . . ? N2 C8 H8 123.4 . . ? O4 C9 O3 121.6(7) . . ? O4 C9 C10 118.4(6) . . ? O3 C9 C10 119.9(6) . . ? C11 C10 C15 120.5(6) . . ? C11 C10 C9 121.7(6) . . ? C15 C10 C9 117.8(6) . . ? C10 C11 C12 117.0(6) . . ? C10 C11 H11 121.5 . . ? C12 C11 H11 121.5 . . ? N3 C12 C13 104.4(5) . . ? N3 C12 C11 134.7(6) . . ? C13 C12 C11 120.8(6) . . ? N4 C13 C14 128.1(6) . . ? N4 C13 C12 109.8(5) . . ? C14 C13 C12 122.1(6) . . ? C15 C14 C13 116.1(6) . . ? C15 C14 H14 121.9 . . ? C13 C14 H14 121.9 . . ? C14 C15 C10 123.3(6) . . ? C14 C15 H15 118.3 . . ? C10 C15 H15 118.3 . . ? N4 C16 N3 112.5(6) . . ? N4 C16 H16 123.8 . . ? N3 C16 H16 123.8 . . ? O5 C17 O6 120.1(5) . . ? O5 C17 C18 121.3(5) . . ? O6 C17 C18 118.6(5) . . ? C19 C18 C23 119.2(5) . . ? C19 C18 C17 121.0(5) . . ? C23 C18 C17 119.6(5) . . ? C18 C19 C20 118.9(5) . . ? C18 C19 H19 120.5 . . ? C20 C19 H19 120.5 . . ? N5 C20 C19 132.2(6) . . ? N5 C20 C21 107.2(5) . . ? C19 C20 C21 120.6(5) . . ? N6 C21 C22 131.0(6) . . ? N6 C21 C20 108.4(5) . . ? C22 C21 C20 120.5(5) . . ? C23 C22 C21 118.1(5) . . ? C23 C22 H22 120.9 . . ? C21 C22 H22 120.9 . . ? C22 C23 C18 122.5(6) . . ? C22 C23 H23 118.7 . . ? C18 C23 H23 118.7 . . ? N5 C24 N6 115.7(6) . . ? N5 C24 H24 122.2 . . ? N6 C24 H24 122.2 . . ? O7 C25 O8 120.3(6) . . ? O7 C25 C26 120.8(6) . . ? O8 C25 C26 118.9(6) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C8 N1 C6 105.0(5) . . ? C8 N1 Ag1 133.6(4) . . ? C6 N1 Ag1 120.0(4) . . ? C8 N2 C5 107.5(5) . . ? C8 N2 H2 126.2 . . ? C5 N2 H2 126.2 . . ? C16 N3 C12 107.6(5) . . ? C16 N3 H3A 126.2 . . ? C12 N3 H3A 126.2 . . ? C16 N4 C13 105.6(5) . . ? C16 N4 Ag2 134.1(5) . . ? C13 N4 Ag2 120.2(4) . . ? C24 N5 C20 104.7(5) . . ? C24 N5 Ag2 127.3(4) . 1_565 ? C20 N5 Ag2 127.7(4) . 1_565 ? C24 N6 C21 104.1(5) . . ? C24 N6 Ag1 127.5(4) . 2_566 ? C21 N6 Ag1 124.8(4) . 2_566 ? C1 O1 Eu1 138.5(4) . . ? C1 O2 Eu1 136.8(4) . 2_657 ? C9 O3 Eu1 90.4(4) . . ? C9 O4 Eu1 96.3(4) . . ? C17 O5 Eu1 91.0(3) . . ? C17 O6 Eu1 97.6(3) . . ? C25 O7 Eu1 96.2(4) . . ? C25 O8 Eu1 157.8(4) . 2_657 ? C25 O8 Eu1 91.9(4) . . ? Eu1 O8 Eu1 106.69(16) 2_657 . ? H1W O1W H2W 109.2 . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 25.20 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 2.130 _refine_diff_density_min -1.946 _refine_diff_density_rms 0.124 data_2 _database_code_depnum_ccdc_archive 'CCDC 782274' #TrackingRef 'cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H20 Br Cu2 Er N8 O8' _chemical_formula_sum 'C32 H20 Br Cu2 Er N8 O8' _chemical_formula_weight 1018.81 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' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21 _symmetry_space_group_name_Hall P2yb loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 15.993(2) _cell_length_b 5.3401(7) _cell_length_c 18.709(2) _cell_angle_alpha 90.00 _cell_angle_beta 101.289(2) _cell_angle_gamma 90.00 _cell_volume 1566.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4826 _cell_measurement_theta_min 1.87 _cell_measurement_theta_max 25.19 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.159 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 986 _exptl_absorpt_coefficient_mu 5.343 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.397 _exptl_absorpt_correction_T_max 0.448 _exptl_absorpt_process_details 'Apex2 (Bruker, 2005)' _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 7042 _diffrn_reflns_av_R_equivalents 0.0230 _diffrn_reflns_av_sigmaI/netI 0.0540 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 25.19 _reflns_number_total 4826 _reflns_number_gt 4393 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (Bruker, 2005)' _computing_cell_refinement 'Apex2 (Bruker, 2005)' _computing_data_reduction 'Apex2 (Bruker, 2005)' _computing_structure_solution 'SHELXTL 6.12 (Bruker, 2000-2003)' _computing_structure_refinement 'SHELXTL 6.12' _computing_molecular_graphics 'SHELXTL 6.12' _computing_publication_material 'SHELXTL 6.12' _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^)+(0.0231P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.013(12) _refine_ls_number_reflns 4826 _refine_ls_number_parameters 469 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0342 _refine_ls_R_factor_gt 0.0295 _refine_ls_wR_factor_ref 0.0655 _refine_ls_wR_factor_gt 0.0634 _refine_ls_goodness_of_fit_ref 0.991 _refine_ls_restrained_S_all 0.991 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.76294(5) 0.09182(16) 0.60942(4) 0.0358(3) Uani 1 1 d . . . Cu2 Cu 0.71236(5) 0.1977(2) -0.11371(4) 0.0360(3) Uani 1 1 d . . . Er1 Er 0.776105(16) 0.15581(6) 0.253347(13) 0.02325(8) Uani 1 1 d . . . Br1 Br 0.71887(5) 0.1449(3) -0.25802(4) 0.0568(2) Uani 1 1 d . . . C1 C 0.8845(5) 0.4584(16) 0.6781(4) 0.0380(19) Uani 1 1 d . . . H1 H 0.8834 0.3926 0.7239 0.046 Uiso 1 1 calc R . . C2 C 0.8613(4) 0.5106(12) 0.5615(3) 0.0235(15) Uani 1 1 d . . . C3 C 0.9133(4) 0.7068(13) 0.5931(4) 0.0274(17) Uani 1 1 d . . . C4 C 0.9400(4) 0.8992(13) 0.5522(4) 0.0297(17) Uani 1 1 d . . . H4 H 0.9739 1.0310 0.5737 0.036 Uiso 1 1 calc R . . C5 C 0.9127(4) 0.8800(12) 0.4780(4) 0.0266(15) Uani 1 1 d . . . H5 H 0.9277 1.0058 0.4485 0.032 Uiso 1 1 calc R . . C6 C 0.8634(3) 0.6803(15) 0.4448(3) 0.0216(14) Uani 1 1 d . . . C7 C 0.8371(4) 0.4934(11) 0.4867(3) 0.0216(14) Uani 1 1 d . . . H7 H 0.8042 0.3601 0.4651 0.026 Uiso 1 1 calc R . . C8 C 0.8413(3) 0.662(2) 0.3635(3) 0.0235(12) Uani 1 1 d . . . C9 C 0.9340(5) 0.4000(14) 0.1769(4) 0.0311(17) Uani 1 1 d . . . C10 C 0.9102(4) 0.5293(14) 0.1046(4) 0.0270(16) Uani 1 1 d . . . C11 C 0.9517(4) 0.7535(12) 0.0930(4) 0.0285(16) Uani 1 1 d . . . H11 H 0.9888 0.8263 0.1320 0.034 Uiso 1 1 calc R . . C12 C 0.9392(4) 0.8685(13) 0.0262(4) 0.0303(17) Uani 1 1 d . . . H12 H 0.9657 1.0193 0.0195 0.036 Uiso 1 1 calc R . . C13 C 0.8852(4) 0.7499(13) -0.0310(4) 0.0270(16) Uani 1 1 d . . . C14 C 0.8103(4) 0.6224(19) -0.1360(3) 0.0347(19) Uani 1 1 d . . . H14 H 0.7877 0.6148 -0.1857 0.042 Uiso 1 1 calc R . . C15 C 0.8420(4) 0.5324(14) -0.0206(4) 0.0252(16) Uani 1 1 d . . . C16 C 0.8522(4) 0.4187(12) 0.0473(3) 0.0228(14) Uani 1 1 d . . . H16 H 0.8219 0.2753 0.0545 0.027 Uiso 1 1 calc R . . C17 C 0.5815(5) -0.1712(15) -0.1644(4) 0.0363(19) Uani 1 1 d . . . H17 H 0.5712 -0.1092 -0.2118 0.044 Uiso 1 1 calc R . . C18 C 0.6292(4) -0.2113(12) -0.0499(3) 0.0213(14) Uani 1 1 d . . . C19 C 0.5752(4) -0.4106(13) -0.0711(3) 0.0279(18) Uani 1 1 d . . . C20 C 0.5612(4) -0.5999(12) -0.0234(4) 0.0261(15) Uani 1 1 d . . . H20 H 0.5255 -0.7353 -0.0387 0.031 Uiso 1 1 calc R . . C21 C 0.6037(4) -0.5732(12) 0.0480(4) 0.0265(15) Uani 1 1 d . . . H21 H 0.5969 -0.6952 0.0819 0.032 Uiso 1 1 calc R . . C22 C 0.6569(3) -0.3673(15) 0.0710(3) 0.0200(13) Uani 1 1 d . . . C23 C 0.6706(4) -0.1855(12) 0.0222(3) 0.0233(15) Uani 1 1 d . . . H23 H 0.7063 -0.0501 0.0372 0.028 Uiso 1 1 calc R . . C24 C 0.7011(3) -0.349(2) 0.1494(3) 0.0236(12) Uani 1 1 d . . . C25 C 0.6059(5) -0.1017(14) 0.3013(4) 0.0336(17) Uani 1 1 d . . . C26 C 0.6067(4) -0.2250(13) 0.3741(4) 0.0292(17) Uani 1 1 d . . . C27 C 0.6527(4) -0.1211(12) 0.4377(4) 0.0272(16) Uani 1 1 d . . . H27 H 0.6855 0.0221 0.4365 0.033 Uiso 1 1 calc R . . C28 C 0.6483(4) -0.2370(12) 0.5032(4) 0.0241(15) Uani 1 1 d . . . C29 C 0.6005(4) -0.4528(14) 0.5040(4) 0.0291(16) Uani 1 1 d . . . C30 C 0.5554(5) -0.5631(14) 0.4426(4) 0.0377(18) Uani 1 1 d . . . H30 H 0.5246 -0.7099 0.4442 0.045 Uiso 1 1 calc R . . C31 C 0.5586(4) -0.4429(14) 0.3778(4) 0.0375(19) Uani 1 1 d . . . H31 H 0.5275 -0.5093 0.3347 0.045 Uiso 1 1 calc R . . C32 C 0.6606(4) -0.344(2) 0.6167(3) 0.0377(15) Uani 1 1 d . . . H32 H 0.6761 -0.3444 0.6673 0.045 Uiso 1 1 calc R . . N1 N 0.8445(3) 0.3556(10) 0.6172(3) 0.0282(13) Uani 1 1 d . . . N2 N 0.9268(3) 0.6663(17) 0.6679(2) 0.0362(13) Uani 1 1 d . . . H2 H 0.9567 0.7578 0.7012 0.043 Uiso 1 1 calc R . . N3 N 0.8633(4) 0.8010(11) -0.1055(3) 0.0404(16) Uani 1 1 d . . . H3 H 0.8809 0.9257 -0.1276 0.048 Uiso 1 1 calc R . . N4 N 0.7932(4) 0.4575(11) -0.0888(3) 0.0304(14) Uani 1 1 d . . . N5 N 0.6336(3) -0.0610(11) -0.1102(3) 0.0298(13) Uani 1 1 d . . . N6 N 0.5449(3) -0.3788(14) -0.1456(3) 0.0312(14) Uani 1 1 d . . . H6 H 0.5096 -0.4742 -0.1738 0.037 Uiso 1 1 calc R . . N7 N 0.6103(4) -0.5186(11) 0.5781(3) 0.0354(15) Uani 1 1 d . . . H7A H 0.5883 -0.6464 0.5954 0.042 Uiso 1 1 calc R . . N8 N 0.6855(4) -0.1706(11) 0.5749(3) 0.0293(14) Uani 1 1 d . . . O1 O 0.7043(4) -0.5392(10) 0.1880(3) 0.0344(14) Uani 1 1 d . . . O2 O 0.7335(4) -0.1384(10) 0.1703(3) 0.0359(14) Uani 1 1 d . . . O3 O 0.8813(3) 0.2507(9) 0.1969(2) 0.0354(12) Uani 1 1 d . . . O4 O 1.0064(3) 0.4430(11) 0.2129(3) 0.0517(15) Uani 1 1 d . . . O5 O 0.8209(4) 0.4535(10) 0.3370(3) 0.0358(14) Uani 1 1 d . . . O6 O 0.8458(4) 0.8596(11) 0.3266(3) 0.0369(15) Uani 1 1 d . . . O7 O 0.6631(3) 0.0610(9) 0.2990(2) 0.0382(12) Uani 1 1 d . . . O8 O 0.5497(3) -0.1630(10) 0.2501(3) 0.0485(15) 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 Cu1 0.0414(5) 0.0350(7) 0.0301(5) 0.0036(4) 0.0050(4) -0.0040(4) Cu2 0.0402(5) 0.0365(7) 0.0303(4) 0.0055(4) 0.0046(3) -0.0072(4) Er1 0.03843(16) 0.01539(13) 0.01501(12) 0.00249(14) 0.00295(10) -0.00366(17) Br1 0.0956(6) 0.0538(5) 0.0267(3) 0.0008(5) 0.0257(4) -0.0192(6) C1 0.042(5) 0.056(6) 0.015(4) 0.000(3) 0.003(3) -0.005(4) C2 0.020(4) 0.023(4) 0.026(4) 0.001(3) 0.003(3) -0.001(3) C3 0.028(3) 0.026(5) 0.029(3) -0.010(3) 0.010(3) 0.000(3) C4 0.027(4) 0.031(4) 0.032(4) -0.016(3) 0.006(3) -0.008(3) C5 0.037(4) 0.017(4) 0.027(4) -0.002(3) 0.009(3) 0.003(3) C6 0.025(3) 0.015(4) 0.026(3) -0.002(3) 0.006(2) 0.006(3) C7 0.024(4) 0.015(3) 0.024(3) -0.002(3) 0.001(3) -0.002(3) C8 0.027(3) 0.017(3) 0.026(3) 0.010(5) 0.004(2) 0.006(4) C9 0.042(4) 0.026(4) 0.025(4) 0.001(3) 0.006(3) 0.002(3) C10 0.025(4) 0.033(4) 0.023(4) 0.005(3) 0.007(3) 0.000(3) C11 0.032(4) 0.028(4) 0.023(4) -0.003(3) 0.001(3) -0.001(3) C12 0.029(4) 0.021(4) 0.042(5) 0.005(3) 0.011(3) 0.000(3) C13 0.028(4) 0.025(4) 0.027(4) 0.005(3) 0.005(3) 0.004(3) C14 0.044(4) 0.037(5) 0.023(3) 0.004(4) 0.005(3) -0.007(4) C15 0.019(4) 0.029(4) 0.028(4) 0.002(3) 0.007(3) 0.002(3) C16 0.025(4) 0.022(4) 0.024(4) 0.001(3) 0.009(3) -0.005(3) C17 0.042(5) 0.040(5) 0.027(4) -0.002(3) 0.006(3) -0.013(4) C18 0.023(4) 0.020(4) 0.022(4) -0.002(3) 0.007(3) -0.001(3) C19 0.022(3) 0.043(5) 0.019(3) -0.003(3) 0.003(3) 0.004(3) C20 0.027(4) 0.023(4) 0.028(4) -0.004(3) 0.005(3) -0.008(3) C21 0.035(4) 0.016(3) 0.030(4) 0.002(3) 0.009(3) 0.000(3) C22 0.021(3) 0.016(3) 0.022(3) 0.000(3) 0.002(2) 0.007(3) C23 0.025(4) 0.018(4) 0.026(4) 0.001(3) 0.002(3) -0.004(3) C24 0.029(3) 0.019(3) 0.023(3) -0.002(5) 0.006(2) 0.003(5) C25 0.036(4) 0.033(4) 0.035(4) 0.005(3) 0.014(4) 0.008(4) C26 0.029(4) 0.032(4) 0.026(4) 0.001(3) 0.004(3) 0.000(3) C27 0.029(4) 0.016(4) 0.038(4) 0.005(3) 0.009(3) -0.005(3) C28 0.021(4) 0.023(3) 0.028(4) 0.001(3) 0.004(3) 0.002(3) C29 0.029(4) 0.028(4) 0.033(4) 0.004(3) 0.014(3) 0.009(3) C30 0.040(5) 0.028(4) 0.046(5) 0.004(4) 0.012(4) -0.003(3) C31 0.036(4) 0.038(4) 0.036(4) -0.004(3) 0.000(4) -0.009(4) C32 0.044(4) 0.041(4) 0.031(3) 0.010(5) 0.013(3) 0.006(5) N1 0.031(3) 0.031(3) 0.024(3) -0.001(3) 0.009(3) -0.004(3) N2 0.038(3) 0.050(4) 0.019(2) -0.007(4) 0.003(2) -0.005(4) N3 0.054(4) 0.033(4) 0.034(4) 0.013(3) 0.007(3) -0.009(3) N4 0.028(3) 0.032(3) 0.031(3) -0.002(3) 0.002(3) 0.001(3) N5 0.031(3) 0.036(4) 0.023(3) 0.003(3) 0.007(3) -0.004(3) N6 0.035(3) 0.038(4) 0.018(2) -0.001(3) -0.004(2) -0.008(3) N7 0.049(4) 0.024(3) 0.039(4) 0.005(3) 0.022(3) -0.003(3) N8 0.029(3) 0.031(3) 0.026(3) 0.002(3) 0.001(3) -0.001(3) O1 0.049(3) 0.025(3) 0.025(3) 0.008(2) -0.004(2) 0.001(2) O2 0.060(4) 0.022(3) 0.022(3) -0.001(2) 0.000(3) -0.005(3) O3 0.041(3) 0.037(3) 0.031(3) 0.004(2) 0.015(2) -0.005(2) O4 0.044(3) 0.061(4) 0.042(3) 0.017(3) -0.012(3) -0.011(3) O5 0.063(4) 0.021(3) 0.019(3) -0.002(2) -0.002(3) -0.006(3) O6 0.053(4) 0.025(3) 0.031(3) 0.010(2) 0.001(3) -0.005(3) O7 0.045(3) 0.041(3) 0.030(3) 0.001(2) 0.011(2) -0.011(2) O8 0.046(3) 0.058(4) 0.034(3) 0.015(3) -0.012(3) -0.008(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 Cu1 N8 1.898(6) . ? Cu1 N1 1.906(5) . ? Cu1 Br1 2.7225(11) 1_556 ? Cu2 N5 1.879(5) . ? Cu2 N4 1.891(6) . ? Cu2 Br1 2.7366(11) . ? Er1 O7 2.204(4) . ? Er1 O3 2.214(4) . ? Er1 O1 2.217(5) 1_565 ? Er1 O2 2.221(5) . ? Er1 O6 2.241(6) 1_545 ? Er1 O5 2.247(6) . ? Br1 Cu1 2.7225(11) 1_554 ? C1 N1 1.311(9) . ? C1 N2 1.333(11) . ? C1 H1 0.9300 . ? C2 C7 1.379(8) . ? C2 C3 1.395(9) . ? C2 N1 1.398(8) . ? C3 N2 1.390(8) . ? C3 C4 1.397(10) . ? C4 C5 1.376(9) . ? C4 H4 0.9300 . ? C5 C6 1.398(9) . ? C5 H5 0.9300 . ? C6 C7 1.385(9) . ? C6 C8 1.495(7) . ? C7 H7 0.9300 . ? C8 O5 1.238(10) . ? C8 O6 1.269(10) . ? C9 O4 1.241(8) . ? C9 O3 1.268(8) . ? C9 C10 1.501(9) . ? C10 C16 1.403(9) . ? C10 C11 1.406(9) . ? C11 C12 1.371(9) . ? C11 H11 0.9300 . ? C12 C13 1.389(10) . ? C12 H12 0.9300 . ? C13 C15 1.384(9) . ? C13 N3 1.396(9) . ? C14 N4 1.314(10) . ? C14 N3 1.328(10) . ? C14 H14 0.9300 . ? C15 C16 1.388(9) . ? C15 N4 1.418(8) . ? C16 H16 0.9300 . ? C17 N5 1.318(9) . ? C17 N6 1.333(10) . ? C17 H17 0.9300 . ? C18 C19 1.379(9) . ? C18 C23 1.389(9) . ? C18 N5 1.397(8) . ? C19 N6 1.393(7) . ? C19 C20 1.396(9) . ? C20 C21 1.384(9) . ? C20 H20 0.9300 . ? C21 C22 1.405(9) . ? C21 H21 0.9300 . ? C22 C23 1.378(9) . ? C22 C24 1.502(7) . ? C23 H23 0.9300 . ? C24 O1 1.240(10) . ? C24 O2 1.269(11) . ? C25 O8 1.223(9) . ? C25 O7 1.269(8) . ? C25 C26 1.511(10) . ? C26 C27 1.387(10) . ? C26 C31 1.404(9) . ? C27 C28 1.386(9) . ? C27 H27 0.9300 . ? C28 C29 1.384(9) . ? C28 N8 1.402(9) . ? C29 C30 1.365(10) . ? C29 N7 1.408(9) . ? C30 C31 1.381(10) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C32 N8 1.322(10) . ? C32 N7 1.348(11) . ? C32 H32 0.9300 . ? N2 H2 0.8600 . ? N3 H3 0.8600 . ? N6 H6 0.8600 . ? N7 H7A 0.8600 . ? O1 Er1 2.217(5) 1_545 ? O6 Er1 2.241(6) 1_565 ? 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 N8 Cu1 N1 164.4(2) . . ? N8 Cu1 Br1 96.85(18) . 1_556 ? N1 Cu1 Br1 98.53(17) . 1_556 ? N5 Cu2 N4 164.0(2) . . ? N5 Cu2 Br1 96.54(17) . . ? N4 Cu2 Br1 99.35(18) . . ? O7 Er1 O3 174.39(17) . . ? O7 Er1 O1 90.42(19) . 1_565 ? O3 Er1 O1 85.89(18) . 1_565 ? O7 Er1 O2 86.89(19) . . ? O3 Er1 O2 89.19(19) . . ? O1 Er1 O2 94.51(16) 1_565 . ? O7 Er1 O6 87.03(19) . 1_545 ? O3 Er1 O6 96.90(19) . 1_545 ? O1 Er1 O6 175.8(2) 1_565 1_545 ? O2 Er1 O6 88.6(2) . 1_545 ? O7 Er1 O5 93.81(19) . . ? O3 Er1 O5 90.12(19) . . ? O1 Er1 O5 85.7(2) 1_565 . ? O2 Er1 O5 179.3(2) . . ? O6 Er1 O5 91.21(16) 1_545 . ? Cu1 Br1 Cu2 167.43(4) 1_554 . ? N1 C1 N2 113.6(6) . . ? N1 C1 H1 123.2 . . ? N2 C1 H1 123.2 . . ? C7 C2 C3 120.4(6) . . ? C7 C2 N1 131.3(6) . . ? C3 C2 N1 108.3(6) . . ? N2 C3 C2 105.8(6) . . ? N2 C3 C4 131.4(7) . . ? C2 C3 C4 122.8(6) . . ? C5 C4 C3 115.2(6) . . ? C5 C4 H4 122.4 . . ? C3 C4 H4 122.4 . . ? C4 C5 C6 123.1(6) . . ? C4 C5 H5 118.5 . . ? C6 C5 H5 118.5 . . ? C7 C6 C5 120.3(6) . . ? C7 C6 C8 119.5(7) . . ? C5 C6 C8 120.1(7) . . ? C2 C7 C6 118.1(6) . . ? C2 C7 H7 121.0 . . ? C6 C7 H7 121.0 . . ? O5 C8 O6 124.6(5) . . ? O5 C8 C6 117.2(7) . . ? O6 C8 C6 118.2(8) . . ? O4 C9 O3 124.0(7) . . ? O4 C9 C10 116.7(7) . . ? O3 C9 C10 119.2(6) . . ? C16 C10 C11 120.1(6) . . ? C16 C10 C9 120.6(6) . . ? C11 C10 C9 119.1(6) . . ? C12 C11 C10 122.2(7) . . ? C12 C11 H11 118.9 . . ? C10 C11 H11 118.9 . . ? C11 C12 C13 117.1(6) . . ? C11 C12 H12 121.4 . . ? C13 C12 H12 121.4 . . ? C15 C13 C12 121.7(6) . . ? C15 C13 N3 105.7(6) . . ? C12 C13 N3 132.6(6) . . ? N4 C14 N3 113.1(6) . . ? N4 C14 H14 123.5 . . ? N3 C14 H14 123.5 . . ? C13 C15 C16 121.6(6) . . ? C13 C15 N4 108.2(6) . . ? C16 C15 N4 130.2(6) . . ? C15 C16 C10 117.2(6) . . ? C15 C16 H16 121.4 . . ? C10 C16 H16 121.4 . . ? N5 C17 N6 114.3(6) . . ? N5 C17 H17 122.8 . . ? N6 C17 H17 122.8 . . ? C19 C18 C23 120.6(6) . . ? C19 C18 N5 109.8(6) . . ? C23 C18 N5 129.6(6) . . ? C18 C19 N6 105.6(6) . . ? C18 C19 C20 123.1(6) . . ? N6 C19 C20 131.3(6) . . ? C21 C20 C19 115.6(6) . . ? C21 C20 H20 122.2 . . ? C19 C20 H20 122.2 . . ? C20 C21 C22 122.0(6) . . ? C20 C21 H21 119.0 . . ? C22 C21 H21 119.0 . . ? C23 C22 C21 121.0(5) . . ? C23 C22 C24 119.7(7) . . ? C21 C22 C24 119.3(7) . . ? C22 C23 C18 117.8(6) . . ? C22 C23 H23 121.1 . . ? C18 C23 H23 121.1 . . ? O1 C24 O2 125.4(5) . . ? O1 C24 C22 118.3(8) . . ? O2 C24 C22 116.3(8) . . ? O8 C25 O7 125.5(7) . . ? O8 C25 C26 117.7(7) . . ? O7 C25 C26 116.7(6) . . ? C27 C26 C31 119.6(7) . . ? C27 C26 C25 120.6(6) . . ? C31 C26 C25 119.8(7) . . ? C26 C27 C28 118.0(6) . . ? C26 C27 H27 121.0 . . ? C28 C27 H27 121.0 . . ? C29 C28 C27 120.3(7) . . ? C29 C28 N8 109.4(6) . . ? C27 C28 N8 130.3(6) . . ? C30 C29 C28 123.4(7) . . ? C30 C29 N7 131.3(7) . . ? C28 C29 N7 105.3(6) . . ? C29 C30 C31 115.8(7) . . ? C29 C30 H30 122.1 . . ? C31 C30 H30 122.1 . . ? C30 C31 C26 122.8(7) . . ? C30 C31 H31 118.6 . . ? C26 C31 H31 118.6 . . ? N8 C32 N7 112.6(6) . . ? N8 C32 H32 123.7 . . ? N7 C32 H32 123.7 . . ? C1 N1 C2 105.5(6) . . ? C1 N1 Cu1 125.9(5) . . ? C2 N1 Cu1 127.5(4) . . ? C1 N2 C3 106.8(6) . . ? C1 N2 H2 126.6 . . ? C3 N2 H2 126.6 . . ? C14 N3 C13 107.7(6) . . ? C14 N3 H3 126.2 . . ? C13 N3 H3 126.2 . . ? C14 N4 C15 105.4(6) . . ? C14 N4 Cu2 123.3(5) . . ? C15 N4 Cu2 131.2(5) . . ? C17 N5 C18 103.9(6) . . ? C17 N5 Cu2 128.9(5) . . ? C18 N5 Cu2 126.2(4) . . ? C17 N6 C19 106.3(6) . . ? C17 N6 H6 126.9 . . ? C19 N6 H6 126.9 . . ? C32 N7 C29 107.1(6) . . ? C32 N7 H7A 126.4 . . ? C29 N7 H7A 126.4 . . ? C32 N8 C28 105.6(6) . . ? C32 N8 Cu1 124.5(5) . . ? C28 N8 Cu1 129.7(5) . . ? C24 O1 Er1 151.7(5) . 1_545 ? C24 O2 Er1 153.4(4) . . ? C9 O3 Er1 153.5(5) . . ? C8 O5 Er1 160.0(5) . . ? C8 O6 Er1 147.6(5) . 1_565 ? C25 O7 Er1 145.3(5) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.19 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.136 _refine_diff_density_min -0.628 _refine_diff_density_rms 0.100 data_3 _database_code_depnum_ccdc_archive 'CCDC 782275' #TrackingRef 'cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H20 Br Cu2 N8 O8 Yb' _chemical_formula_sum 'C32 H20 Br Cu2 N8 O8 Yb' _chemical_formula_weight 1024.59 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' Br Br -0.2901 2.4595 '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' 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' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21 _symmetry_space_group_name_Hall P2yb loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 16.1117(14) _cell_length_b 5.3028(5) _cell_length_c 18.7099(17) _cell_angle_alpha 90.00 _cell_angle_beta 101.1110(10) _cell_angle_gamma 90.00 _cell_volume 1568.6(2) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3165 _cell_measurement_theta_min 1.85 _cell_measurement_theta_max 25.20 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.169 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 990 _exptl_absorpt_coefficient_mu 5.643 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.270 _exptl_absorpt_correction_T_max 0.325 _exptl_absorpt_process_details 'Apex2 (Bruker, 2005)' _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 8120 _diffrn_reflns_av_R_equivalents 0.0255 _diffrn_reflns_av_sigmaI/netI 0.0405 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -4 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 25.20 _reflns_number_total 4349 _reflns_number_gt 4092 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (Bruker, 2005)' _computing_cell_refinement 'Apex2 (Bruker, 2005)' _computing_data_reduction 'Apex2 (Bruker, 2005)' _computing_structure_solution 'SHELXTL 6.12 (Bruker, 2000-2003)' _computing_structure_refinement 'SHELXTL 6.12' _computing_molecular_graphics 'SHELXTL 6.12' _computing_publication_material 'SHELXTL 6.12' _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^)+(0.0242P)^2^+3.7719P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.180(13) _refine_ls_number_reflns 4349 _refine_ls_number_parameters 469 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0335 _refine_ls_R_factor_gt 0.0307 _refine_ls_wR_factor_ref 0.0692 _refine_ls_wR_factor_gt 0.0679 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _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 Cu1 Cu 0.23534(6) 0.90441(19) 0.39104(5) 0.0379(3) Uani 1 1 d . . . Cu2 Cu 0.28547(6) 0.8012(2) 1.11315(5) 0.0375(3) Uani 1 1 d . . . Yb1 Yb 0.227620(18) 0.84428(8) 0.747959(13) 0.02537(9) Uani 1 1 d . . . Br1 Br 0.27681(7) 0.8520(4) 1.25719(4) 0.0692(3) Uani 1 1 d . . . C1 C 0.1132(5) 0.5375(19) 0.3240(4) 0.039(2) Uani 1 1 d . . . H1 H 0.1136 0.6017 0.2778 0.047 Uiso 1 1 calc R . . C2 C 0.1386(4) 0.4866(15) 0.4407(4) 0.0226(16) Uani 1 1 d . . . C3 C 0.0862(4) 0.2876(14) 0.4111(4) 0.0280(19) Uani 1 1 d . . . C4 C 0.0601(5) 0.1004(17) 0.4522(4) 0.035(2) Uani 1 1 d . . . H4 H 0.0250 -0.0299 0.4314 0.041 Uiso 1 1 calc R . . C5 C 0.0893(5) 0.1170(14) 0.5270(4) 0.0287(17) Uani 1 1 d . . . H5 H 0.0751 -0.0097 0.5568 0.034 Uiso 1 1 calc R . . C6 C 0.1389(4) 0.3159(17) 0.5586(3) 0.0203(16) Uani 1 1 d . . . C7 C 0.1641(4) 0.5070(13) 0.5149(4) 0.0209(15) Uani 1 1 d . . . H7 H 0.1968 0.6423 0.5356 0.025 Uiso 1 1 calc R . . C8 C 0.1633(4) 0.342(3) 0.6397(3) 0.0262(14) Uani 1 1 d . . . C9 C 0.0709(5) 0.6041(17) 0.8205(4) 0.036(2) Uani 1 1 d . . . C10 C 0.0918(5) 0.4745(16) 0.8944(4) 0.0290(18) Uani 1 1 d . . . C11 C 0.0492(5) 0.2481(16) 0.9050(4) 0.0337(19) Uani 1 1 d . . . H11 H 0.0128 0.1769 0.8656 0.040 Uiso 1 1 calc R . . C12 C 0.0597(5) 0.1307(16) 0.9709(4) 0.036(2) Uani 1 1 d . . . H12 H 0.0324 -0.0199 0.9773 0.043 Uiso 1 1 calc R . . C13 C 0.1133(5) 0.2489(16) 1.0280(4) 0.0333(19) Uani 1 1 d . . . C14 C 0.1866(5) 0.378(3) 1.1342(4) 0.038(2) Uani 1 1 d . . . H14 H 0.2082 0.3856 1.1840 0.046 Uiso 1 1 calc R . . C15 C 0.1579(5) 0.4676(16) 1.0191(4) 0.0261(17) Uani 1 1 d . . . C16 C 0.1486(4) 0.5811(15) 0.9511(4) 0.0281(17) Uani 1 1 d . . . H16 H 0.1795 0.7239 0.9440 0.034 Uiso 1 1 calc R . . C17 C 0.4169(5) 1.171(2) 1.1655(4) 0.041(2) Uani 1 1 d . . . H17 H 0.4272 1.1080 1.2128 0.050 Uiso 1 1 calc R . . C18 C 0.3697(4) 1.2122(15) 1.0506(4) 0.0249(17) Uani 1 1 d . . . C19 C 0.4250(4) 1.4126(15) 1.0723(4) 0.029(2) Uani 1 1 d . . . C20 C 0.4397(5) 1.6014(15) 1.0243(4) 0.0285(18) Uani 1 1 d . . . H20 H 0.4756 1.7366 1.0393 0.034 Uiso 1 1 calc R . . C21 C 0.3971(4) 1.5741(15) 0.9524(4) 0.0254(16) Uani 1 1 d . . . H21 H 0.4037 1.6969 0.9184 0.031 Uiso 1 1 calc R . . C22 C 0.3447(4) 1.367(2) 0.9299(3) 0.0224(15) Uani 1 1 d . . . C23 C 0.3294(4) 1.1850(14) 0.9782(4) 0.0217(16) Uani 1 1 d . . . H23 H 0.2936 1.0496 0.9631 0.026 Uiso 1 1 calc R . . C24 C 0.3009(4) 1.350(3) 0.8517(3) 0.0246(13) Uani 1 1 d . . . C25 C 0.3944(5) 1.1025(17) 0.6972(4) 0.036(2) Uani 1 1 d . . . C26 C 0.3929(5) 1.2219(16) 0.6249(4) 0.0293(18) Uani 1 1 d . . . C27 C 0.3465(5) 1.1200(15) 0.5620(4) 0.0311(18) Uani 1 1 d . . . H27 H 0.3129 0.9784 0.5635 0.037 Uiso 1 1 calc R . . C28 C 0.3516(5) 1.2359(16) 0.4957(4) 0.0291(18) Uani 1 1 d . . . C29 C 0.3988(5) 1.4511(16) 0.4943(4) 0.0322(18) Uani 1 1 d . . . C30 C 0.4455(6) 1.5613(18) 0.5564(5) 0.042(2) Uani 1 1 d . . . H30 H 0.4773 1.7067 0.5543 0.051 Uiso 1 1 calc R . . C31 C 0.4422(5) 1.4416(17) 0.6224(4) 0.039(2) Uani 1 1 d . . . H31 H 0.4730 1.5076 0.6655 0.046 Uiso 1 1 calc R . . C32 C 0.3384(4) 1.342(3) 0.3833(4) 0.0416(18) Uani 1 1 d . . . H32 H 0.3223 1.3443 0.3329 0.050 Uiso 1 1 calc R . . N1 N 0.1553(4) 0.6426(14) 0.3847(3) 0.0328(16) Uani 1 1 d . . . N2 N 0.0707(4) 0.333(2) 0.3355(3) 0.0426(17) Uani 1 1 d . . . H2 H 0.0392 0.2430 0.3027 0.051 Uiso 1 1 calc R . . N3 N 0.1341(5) 0.1988(14) 1.1027(4) 0.0410(18) Uani 1 1 d . . . H3 H 0.1160 0.0735 1.1246 0.049 Uiso 1 1 calc R . . N4 N 0.2044(4) 0.5416(14) 1.0866(3) 0.0329(16) Uani 1 1 d . . . N5 N 0.3640(4) 1.0604(14) 1.1107(3) 0.0337(16) Uani 1 1 d . . . N6 N 0.4540(4) 1.3816(18) 1.1459(3) 0.0338(17) Uani 1 1 d . . . H6 H 0.4889 1.4778 1.1741 0.041 Uiso 1 1 calc R . . N7 N 0.3886(5) 1.5140(14) 0.4208(4) 0.0398(18) Uani 1 1 d . . . H7A H 0.4108 1.6412 0.4030 0.048 Uiso 1 1 calc R . . N8 N 0.3135(4) 1.1662(13) 0.4248(3) 0.0311(16) Uani 1 1 d . . . O1 O 0.2985(4) 1.5436(13) 0.8130(3) 0.0362(16) Uani 1 1 d . . . O2 O 0.2698(4) 1.1405(13) 0.8307(3) 0.0371(16) Uani 1 1 d . . . O3 O 0.1235(3) 0.7538(11) 0.8029(3) 0.0389(14) Uani 1 1 d . . . O4 O -0.0011(4) 0.5599(14) 0.7840(4) 0.065(2) Uani 1 1 d . . . O5 O 0.1843(4) 0.5528(13) 0.6653(3) 0.0365(17) Uani 1 1 d . . . O6 O 0.1588(4) 0.1455(14) 0.6768(3) 0.0380(17) Uani 1 1 d . . . O7 O 0.3376(4) 0.9405(11) 0.7010(3) 0.0421(15) Uani 1 1 d . . . O8 O 0.4514(4) 1.1607(14) 0.7486(3) 0.0568(19) 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 Cu1 0.0421(5) 0.0398(10) 0.0303(5) 0.0045(4) 0.0034(4) -0.0029(5) Cu2 0.0401(5) 0.0401(9) 0.0310(4) 0.0056(5) 0.0036(4) -0.0083(5) Yb1 0.04342(16) 0.01574(14) 0.01524(13) 0.00251(15) 0.00142(10) -0.0039(2) Br1 0.1241(8) 0.0600(6) 0.0311(4) 0.0000(6) 0.0341(4) -0.0266(9) C1 0.044(5) 0.046(6) 0.026(4) 0.003(4) 0.003(4) -0.003(5) C2 0.022(4) 0.025(4) 0.020(3) -0.006(3) 0.001(3) -0.003(3) C3 0.031(4) 0.027(6) 0.024(3) -0.010(3) 0.002(3) 0.001(3) C4 0.028(4) 0.032(5) 0.039(5) -0.013(4) -0.002(4) -0.005(4) C5 0.034(4) 0.019(4) 0.036(4) -0.002(3) 0.011(3) 0.003(3) C6 0.020(3) 0.014(5) 0.025(3) -0.002(3) 0.000(2) 0.005(3) C7 0.020(3) 0.017(4) 0.023(4) 0.000(3) -0.002(3) 0.001(3) C8 0.030(3) 0.023(4) 0.023(3) 0.001(6) -0.002(2) -0.002(5) C9 0.044(5) 0.035(5) 0.028(4) 0.001(4) 0.004(4) 0.009(4) C10 0.025(4) 0.029(5) 0.032(4) 0.005(4) 0.005(3) 0.002(4) C11 0.033(4) 0.029(4) 0.036(4) -0.005(4) 0.000(4) 0.000(4) C12 0.035(4) 0.026(5) 0.047(5) 0.008(4) 0.006(4) -0.006(4) C13 0.031(4) 0.032(5) 0.035(4) 0.011(4) 0.002(4) 0.005(4) C14 0.043(4) 0.038(7) 0.035(4) 0.008(5) 0.009(3) 0.000(5) C15 0.023(4) 0.027(4) 0.028(4) 0.001(3) 0.004(3) 0.001(4) C16 0.024(4) 0.024(4) 0.038(4) 0.000(4) 0.009(3) -0.001(3) C17 0.048(5) 0.050(6) 0.024(4) 0.003(4) 0.002(4) 0.001(5) C18 0.023(4) 0.030(5) 0.022(4) 0.001(3) 0.005(3) -0.003(3) C19 0.027(3) 0.041(6) 0.020(3) -0.006(3) 0.006(3) 0.010(4) C20 0.032(4) 0.024(4) 0.030(4) -0.008(3) 0.007(3) -0.007(3) C21 0.028(4) 0.019(4) 0.031(4) -0.001(3) 0.008(3) 0.000(3) C22 0.022(3) 0.021(4) 0.023(3) -0.001(4) 0.003(2) 0.013(4) C23 0.022(3) 0.020(4) 0.024(4) -0.002(3) 0.006(3) -0.005(3) C24 0.029(3) 0.020(3) 0.025(3) 0.004(6) 0.006(2) 0.007(6) C25 0.039(5) 0.031(5) 0.036(5) 0.008(4) 0.005(4) 0.009(4) C26 0.020(4) 0.034(5) 0.031(4) 0.007(4) -0.001(3) 0.000(4) C27 0.038(4) 0.024(4) 0.034(4) 0.005(4) 0.012(4) -0.007(4) C28 0.021(4) 0.035(5) 0.031(4) -0.001(4) 0.007(3) -0.002(4) C29 0.031(4) 0.030(4) 0.037(4) 0.004(4) 0.009(4) 0.005(4) C30 0.046(5) 0.039(6) 0.042(5) 0.001(4) 0.009(4) -0.010(4) C31 0.042(5) 0.036(5) 0.037(5) 0.002(4) 0.003(4) -0.010(4) C32 0.046(4) 0.046(5) 0.032(4) 0.010(7) 0.008(3) 0.014(7) N1 0.037(4) 0.037(4) 0.025(3) -0.005(3) 0.009(3) -0.004(3) N2 0.039(3) 0.061(5) 0.023(3) -0.005(5) -0.005(2) -0.011(5) N3 0.056(5) 0.031(4) 0.034(4) 0.017(3) 0.003(3) -0.008(4) N4 0.030(3) 0.038(4) 0.030(3) 0.001(3) 0.005(3) -0.003(3) N5 0.038(4) 0.044(4) 0.018(3) 0.004(3) 0.001(3) -0.006(3) N6 0.038(3) 0.040(5) 0.021(3) -0.005(4) -0.003(2) -0.007(4) N7 0.052(4) 0.035(4) 0.036(4) 0.012(3) 0.015(3) 0.001(4) N8 0.030(3) 0.036(4) 0.026(3) 0.003(3) 0.003(3) 0.002(3) O1 0.050(4) 0.029(4) 0.027(3) 0.009(3) 0.000(3) -0.006(3) O2 0.059(4) 0.027(4) 0.022(3) -0.002(3) -0.001(3) -0.006(3) O3 0.050(3) 0.038(4) 0.032(3) 0.008(3) 0.015(2) -0.005(3) O4 0.058(4) 0.066(5) 0.055(4) 0.031(4) -0.027(3) -0.016(4) O5 0.062(4) 0.021(3) 0.024(3) -0.001(3) 0.001(3) -0.009(3) O6 0.052(4) 0.026(4) 0.031(3) 0.007(3) -0.005(3) 0.001(3) O7 0.056(3) 0.039(4) 0.034(3) 0.003(3) 0.016(3) -0.007(3) O8 0.052(4) 0.064(5) 0.043(4) 0.021(3) -0.020(3) -0.006(4) _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 Cu1 N1 1.883(7) . ? Cu1 N8 1.899(7) . ? Cu1 Br1 2.7276(12) 1_554 ? Cu2 N5 1.875(7) . ? Cu2 N4 1.897(7) . ? Cu2 Br1 2.7386(12) . ? Yb1 O3 2.182(5) . ? Yb1 O7 2.184(5) . ? Yb1 O1 2.189(7) 1_545 ? Yb1 O5 2.203(7) . ? Yb1 O2 2.218(7) . ? Yb1 O6 2.233(7) 1_565 ? Br1 Cu1 2.7276(12) 1_556 ? C1 N2 1.324(13) . ? C1 N1 1.329(10) . ? C1 H1 0.9300 . ? C2 C7 1.375(9) . ? C2 C3 1.397(10) . ? C2 N1 1.401(9) . ? C3 C4 1.370(11) . ? C3 N2 1.409(9) . ? C4 C5 1.390(10) . ? C4 H4 0.9300 . ? C5 C6 1.385(11) . ? C5 H5 0.9300 . ? C6 C7 1.410(10) . ? C6 C8 1.497(8) . ? C7 H7 0.9300 . ? C8 O5 1.238(13) . ? C8 O6 1.261(13) . ? C9 O4 1.249(10) . ? C9 O3 1.252(10) . ? C9 C10 1.523(11) . ? C10 C16 1.381(11) . ? C10 C11 1.416(11) . ? C11 C12 1.362(11) . ? C11 H11 0.9300 . ? C12 C13 1.387(11) . ? C12 H12 0.9300 . ? C13 C15 1.391(11) . ? C13 N3 1.399(10) . ? C14 N4 1.316(12) . ? C14 N3 1.330(13) . ? C14 H14 0.9300 . ? C15 C16 1.390(10) . ? C15 N4 1.394(9) . ? C16 H16 0.9300 . ? C17 N5 1.334(10) . ? C17 N6 1.351(13) . ? C17 H17 0.9300 . ? C18 C23 1.393(9) . ? C18 C19 1.396(10) . ? C18 N5 1.400(9) . ? C19 N6 1.376(8) . ? C19 C20 1.396(11) . ? C20 C21 1.396(10) . ? C20 H20 0.9300 . ? C21 C22 1.401(12) . ? C21 H21 0.9300 . ? C22 C23 1.375(11) . ? C22 C24 1.500(8) . ? C23 H23 0.9300 . ? C24 O2 1.250(13) . ? C24 O1 1.253(13) . ? C25 O8 1.235(10) . ? C25 O7 1.268(10) . ? C25 C26 1.490(11) . ? C26 C27 1.377(11) . ? C26 C31 1.416(11) . ? C27 C28 1.399(10) . ? C27 H27 0.9300 . ? C28 C29 1.374(11) . ? C28 N8 1.400(10) . ? C29 C30 1.386(11) . ? C29 N7 1.393(10) . ? C30 C31 1.398(11) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C32 N8 1.323(13) . ? C32 N7 1.327(14) . ? C32 H32 0.9300 . ? N2 H2 0.8600 . ? N3 H3 0.8600 . ? N6 H6 0.8600 . ? N7 H7A 0.8600 . ? O1 Yb1 2.189(7) 1_565 ? O6 Yb1 2.233(7) 1_545 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 N8 164.2(3) . . ? N1 Cu1 Br1 98.83(19) . 1_554 ? N8 Cu1 Br1 96.66(19) . 1_554 ? N5 Cu2 N4 163.6(3) . . ? N5 Cu2 Br1 96.58(19) . . ? N4 Cu2 Br1 99.6(2) . . ? O3 Yb1 O7 175.7(2) . . ? O3 Yb1 O1 86.8(2) . 1_545 ? O7 Yb1 O1 91.0(2) . 1_545 ? O3 Yb1 O5 90.5(2) . . ? O7 Yb1 O5 93.0(2) . . ? O1 Yb1 O5 86.6(3) 1_545 . ? O3 Yb1 O2 89.3(2) . . ? O7 Yb1 O2 87.3(2) . . ? O1 Yb1 O2 94.09(19) 1_545 . ? O5 Yb1 O2 179.3(3) . . ? O3 Yb1 O6 95.7(2) . 1_565 ? O7 Yb1 O6 86.6(2) . 1_565 ? O1 Yb1 O6 176.9(3) 1_545 1_565 ? O5 Yb1 O6 91.67(19) . 1_565 ? O2 Yb1 O6 87.7(3) . 1_565 ? Cu1 Br1 Cu2 168.95(5) 1_556 . ? N2 C1 N1 113.6(7) . . ? N2 C1 H1 123.2 . . ? N1 C1 H1 123.2 . . ? C7 C2 C3 120.0(7) . . ? C7 C2 N1 130.2(7) . . ? C3 C2 N1 109.8(6) . . ? C4 C3 C2 123.5(7) . . ? C4 C3 N2 132.2(8) . . ? C2 C3 N2 104.3(7) . . ? C3 C4 C5 116.0(7) . . ? C3 C4 H4 122.0 . . ? C5 C4 H4 122.0 . . ? C6 C5 C4 122.3(7) . . ? C6 C5 H5 118.9 . . ? C4 C5 H5 118.9 . . ? C5 C6 C7 120.4(6) . . ? C5 C6 C8 121.3(8) . . ? C7 C6 C8 118.2(8) . . ? C2 C7 C6 117.8(7) . . ? C2 C7 H7 121.1 . . ? C6 C7 H7 121.1 . . ? O5 C8 O6 125.0(6) . . ? O5 C8 C6 118.3(9) . . ? O6 C8 C6 116.7(10) . . ? O4 C9 O3 125.5(8) . . ? O4 C9 C10 115.6(8) . . ? O3 C9 C10 118.8(7) . . ? C16 C10 C11 120.5(8) . . ? C16 C10 C9 120.7(8) . . ? C11 C10 C9 118.7(7) . . ? C12 C11 C10 122.4(8) . . ? C12 C11 H11 118.8 . . ? C10 C11 H11 118.8 . . ? C11 C12 C13 116.1(8) . . ? C11 C12 H12 121.9 . . ? C13 C12 H12 121.9 . . ? C12 C13 C15 123.0(8) . . ? C12 C13 N3 132.6(8) . . ? C15 C13 N3 104.3(7) . . ? N4 C14 N3 111.9(7) . . ? N4 C14 H14 124.0 . . ? N3 C14 H14 124.0 . . ? C16 C15 C13 120.2(7) . . ? C16 C15 N4 130.7(8) . . ? C13 C15 N4 109.1(7) . . ? C10 C16 C15 117.7(7) . . ? C10 C16 H16 121.2 . . ? C15 C16 H16 121.2 . . ? N5 C17 N6 113.9(7) . . ? N5 C17 H17 123.0 . . ? N6 C17 H17 123.0 . . ? C23 C18 C19 120.9(7) . . ? C23 C18 N5 129.1(7) . . ? C19 C18 N5 109.9(6) . . ? N6 C19 C20 131.5(8) . . ? N6 C19 C18 105.9(7) . . ? C20 C19 C18 122.5(6) . . ? C19 C20 C21 115.7(7) . . ? C19 C20 H20 122.2 . . ? C21 C20 H20 122.2 . . ? C20 C21 C22 121.8(7) . . ? C20 C21 H21 119.1 . . ? C22 C21 H21 119.1 . . ? C23 C22 C21 121.8(6) . . ? C23 C22 C24 119.3(9) . . ? C21 C22 C24 118.8(8) . . ? C22 C23 C18 117.2(7) . . ? C22 C23 H23 121.4 . . ? C18 C23 H23 121.4 . . ? O2 C24 O1 125.5(6) . . ? O2 C24 C22 116.4(9) . . ? O1 C24 C22 118.1(10) . . ? O8 C25 O7 124.2(8) . . ? O8 C25 C26 118.7(8) . . ? O7 C25 C26 117.0(7) . . ? C27 C26 C31 120.7(8) . . ? C27 C26 C25 121.3(8) . . ? C31 C26 C25 118.0(7) . . ? C26 C27 C28 118.0(7) . . ? C26 C27 H27 121.0 . . ? C28 C27 H27 121.0 . . ? C29 C28 C27 120.6(7) . . ? C29 C28 N8 110.1(7) . . ? C27 C28 N8 129.3(7) . . ? C28 C29 C30 123.1(8) . . ? C28 C29 N7 105.0(7) . . ? C30 C29 N7 131.9(8) . . ? C29 C30 C31 116.2(8) . . ? C29 C30 H30 121.9 . . ? C31 C30 H30 121.9 . . ? C30 C31 C26 121.3(8) . . ? C30 C31 H31 119.3 . . ? C26 C31 H31 119.3 . . ? N8 C32 N7 113.4(6) . . ? N8 C32 H32 123.3 . . ? N7 C32 H32 123.3 . . ? C1 N1 C2 104.6(7) . . ? C1 N1 Cu1 126.4(6) . . ? C2 N1 Cu1 128.1(5) . . ? C1 N2 C3 107.8(7) . . ? C1 N2 H2 126.1 . . ? C3 N2 H2 126.1 . . ? C14 N3 C13 108.5(7) . . ? C14 N3 H3 125.8 . . ? C13 N3 H3 125.8 . . ? C14 N4 C15 106.1(7) . . ? C14 N4 Cu2 122.1(6) . . ? C15 N4 Cu2 131.6(5) . . ? C17 N5 C18 103.5(7) . . ? C17 N5 Cu2 129.5(6) . . ? C18 N5 Cu2 126.2(5) . . ? C17 N6 C19 106.7(7) . . ? C17 N6 H6 126.7 . . ? C19 N6 H6 126.7 . . ? C32 N7 C29 107.5(7) . . ? C32 N7 H7A 126.3 . . ? C29 N7 H7A 126.3 . . ? C32 N8 C28 104.1(7) . . ? C32 N8 Cu1 125.2(6) . . ? C28 N8 Cu1 130.5(5) . . ? C24 O1 Yb1 150.9(5) . 1_565 ? C24 O2 Yb1 154.0(5) . . ? C9 O3 Yb1 152.2(6) . . ? C8 O5 Yb1 158.7(6) . . ? C8 O6 Yb1 147.6(6) . 1_545 ? C25 O7 Yb1 146.3(6) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.20 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.491 _refine_diff_density_min -1.105 _refine_diff_density_rms 0.097 data_5 _database_code_depnum_ccdc_archive 'CCDC 782276' #TrackingRef 'cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H15 Ag N6 O8 Tb' _chemical_formula_sum 'C25 H15 Ag N6 O8 Tb' _chemical_formula_weight 794.22 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 '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' _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 9.742(3) _cell_length_b 12.158(3) _cell_length_c 12.383(3) _cell_angle_alpha 61.150(3) _cell_angle_beta 76.851(3) _cell_angle_gamma 82.676(4) _cell_volume 1250.7(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4395 _cell_measurement_theta_min 1.91 _cell_measurement_theta_max 25.20 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.109 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 766 _exptl_absorpt_coefficient_mu 3.651 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.421 _exptl_absorpt_correction_T_max 0.482 _exptl_absorpt_process_details 'Apex2 (Bruker, 2005)' _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 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 6342 _diffrn_reflns_av_R_equivalents 0.0284 _diffrn_reflns_av_sigmaI/netI 0.0607 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 25.20 _reflns_number_total 4395 _reflns_number_gt 3573 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (Bruker, 2005)' _computing_cell_refinement 'Apex2 (Bruker, 2005)' _computing_data_reduction 'Apex2 (Bruker, 2005)' _computing_structure_solution 'SHELXTL 6.12 (Bruker, 2000-2003)' _computing_structure_refinement 'SHELXTL 6.12' _computing_molecular_graphics 'SHELXTL 6.12' _computing_publication_material 'SHELXTL 6.12' _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^)+(0.0856P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4395 _refine_ls_number_parameters 370 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0669 _refine_ls_R_factor_gt 0.0524 _refine_ls_wR_factor_ref 0.1338 _refine_ls_wR_factor_gt 0.1244 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _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 Ag1 Ag 0.52007(9) 1.34253(7) 0.37099(6) 0.0455(2) Uani 1 1 d . . . Tb1 Tb 0.17390(4) 0.97951(4) 0.07203(3) 0.02494(16) Uani 1 1 d . . . C1 C 0.2202(8) 0.7562(8) 0.0471(7) 0.0273(18) Uani 1 1 d . . . C2 C 0.2455(9) 0.6398(8) 0.0321(8) 0.0305(19) Uani 1 1 d . . . C3 C 0.1842(10) 0.5266(9) 0.1302(9) 0.040(2) Uani 1 1 d . . . H3 H 0.1229 0.5275 0.1994 0.048 Uiso 1 1 calc R . . C4 C 0.2129(10) 0.4152(9) 0.1258(8) 0.043(2) Uani 1 1 d . . . H4 H 0.1723 0.3407 0.1904 0.051 Uiso 1 1 calc R . . C5 C 0.3055(10) 0.4187(8) 0.0201(8) 0.034(2) Uani 1 1 d . . . C6 C 0.3613(9) 0.5316(8) -0.0811(8) 0.033(2) Uani 1 1 d . . . C7 C 0.3326(9) 0.6449(9) -0.0757(8) 0.034(2) Uani 1 1 d . . . H7 H 0.3703 0.7201 -0.1415 0.041 Uiso 1 1 calc R . . C8 C 0.4433(10) 0.3856(9) -0.1292(9) 0.038(2) Uani 1 1 d . . . H8 H 0.4929 0.3426 -0.1714 0.046 Uiso 1 1 calc R . . C9 C 0.0993(9) 1.1918(8) -0.1404(8) 0.0320(19) Uani 1 1 d . . . C10 C 0.1367(8) 1.2953(8) -0.2711(8) 0.0310(19) Uani 1 1 d . . . C11 C 0.1040(9) 1.2908(9) -0.3727(8) 0.035(2) Uani 1 1 d . . . H11 H 0.0586 1.2210 -0.3586 0.042 Uiso 1 1 calc R . . C12 C 0.1374(10) 1.3875(9) -0.4941(8) 0.040(2) Uani 1 1 d . . . H12 H 0.1133 1.3850 -0.5613 0.048 Uiso 1 1 calc R . . C13 C 0.2079(9) 1.4878(9) -0.5111(8) 0.035(2) Uani 1 1 d . . . C14 C 0.2469(9) 1.4928(8) -0.4104(8) 0.035(2) Uani 1 1 d . . . C15 C 0.2070(10) 1.3974(8) -0.2895(8) 0.037(2) Uani 1 1 d . . . H15 H 0.2268 1.4014 -0.2215 0.044 Uiso 1 1 calc R . . C16 C 0.3186(12) 1.6626(10) -0.5779(9) 0.052(3) Uani 1 1 d . . . H16 H 0.3578 1.7410 -0.6324 0.063 Uiso 1 1 calc R . . C17 C 0.1998(9) 1.0105(8) 0.2759(8) 0.033(2) Uani 1 1 d . . . C18 C 0.2288(9) 1.0072(8) 0.3918(7) 0.031(2) Uani 1 1 d . . . C19 C 0.1677(10) 0.9121(9) 0.5096(8) 0.042(2) Uani 1 1 d . . . H19 H 0.1108 0.8535 0.5142 0.051 Uiso 1 1 calc R . . C20 C 0.1915(10) 0.9046(9) 0.6202(8) 0.041(2) Uani 1 1 d . . . H20 H 0.1515 0.8425 0.6990 0.049 Uiso 1 1 calc R . . C21 C 0.2780(10) 0.9949(8) 0.6061(8) 0.033(2) Uani 1 1 d . . . C22 C 0.3369(9) 1.0898(8) 0.4898(7) 0.0301(19) Uani 1 1 d . . . C23 C 0.3135(9) 1.0959(8) 0.3795(7) 0.0313(19) Uani 1 1 d . . . H23 H 0.3540 1.1579 0.3008 0.038 Uiso 1 1 calc R . . C24 C 0.4001(10) 1.1176(9) 0.6307(8) 0.037(2) Uani 1 1 d . . . H24 H 0.4399 1.1518 0.6691 0.045 Uiso 1 1 calc R . . C25 C 0.5072(9) 0.9412(8) 0.0631(7) 0.0267(18) Uani 1 1 d . . . N1 N 0.3597(8) 0.3278(7) -0.0152(7) 0.0377(18) Uani 1 1 d . . . H1 H 0.3432 0.2488 0.0277 0.045 Uiso 1 1 calc R . . N2 N 0.4486(8) 0.5081(7) -0.1756(6) 0.0347(17) Uani 1 1 d . . . N3 N 0.2554(8) 1.5993(7) -0.6151(7) 0.043(2) Uani 1 1 d . . . H3A H 0.2458 1.6236 -0.6908 0.051 Uiso 1 1 calc R . . N4 N 0.3204(9) 1.6030(8) -0.4555(7) 0.052(2) Uani 1 1 d . . . N5 N 0.4152(8) 1.1662(7) 0.5074(6) 0.0350(17) Uani 1 1 d . . . N6 N 0.3221(8) 1.0144(7) 0.6948(6) 0.0366(18) Uani 1 1 d . . . H6 H 0.3029 0.9690 0.7750 0.044 Uiso 1 1 calc R . . O1 O 0.1750(6) 0.7458(5) 0.1552(5) 0.0286(13) Uani 1 1 d . . . O2 O 0.2478(7) 0.8633(5) -0.0472(5) 0.0365(14) Uani 1 1 d . . . O3 O 0.0650(6) 1.0839(5) -0.1261(5) 0.0287(13) Uani 1 1 d . . . O4 O 0.1090(6) 1.2009(5) -0.0476(5) 0.0308(13) Uani 1 1 d . . . O5 O 0.2535(7) 1.0931(6) 0.1679(5) 0.0426(17) Uani 1 1 d . . . O6 O 0.1273(7) 0.9228(6) 0.2892(5) 0.0391(15) Uani 1 1 d . . . O7 O 0.3971(6) 0.8868(6) 0.1339(5) 0.0363(14) Uani 1 1 d . . . O8 O 0.6294(6) 0.9088(6) 0.0854(5) 0.0336(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 Ag1 0.0698(5) 0.0333(4) 0.0306(4) -0.0130(3) 0.0010(3) -0.0196(4) Tb1 0.0338(2) 0.0212(2) 0.0180(2) -0.00548(17) -0.00499(15) -0.01019(16) C1 0.028(4) 0.030(5) 0.023(4) -0.011(4) -0.007(3) -0.002(4) C2 0.046(5) 0.021(4) 0.026(4) -0.010(4) -0.008(4) -0.006(4) C3 0.049(6) 0.032(5) 0.036(5) -0.017(4) 0.003(4) -0.007(4) C4 0.062(6) 0.026(5) 0.029(5) -0.008(4) 0.005(4) -0.016(5) C5 0.050(5) 0.018(4) 0.035(5) -0.010(4) -0.007(4) -0.014(4) C6 0.046(5) 0.024(5) 0.028(5) -0.008(4) -0.010(4) -0.008(4) C7 0.046(5) 0.033(5) 0.026(4) -0.013(4) -0.006(4) -0.009(4) C8 0.054(6) 0.026(5) 0.040(5) -0.020(4) -0.004(4) -0.006(4) C9 0.036(5) 0.025(5) 0.031(5) -0.007(4) -0.010(4) -0.002(4) C10 0.031(4) 0.023(5) 0.026(4) 0.001(4) -0.005(3) -0.013(4) C11 0.040(5) 0.029(5) 0.034(5) -0.014(4) 0.000(4) -0.011(4) C12 0.052(6) 0.042(6) 0.025(5) -0.009(4) -0.012(4) -0.013(5) C13 0.043(5) 0.035(5) 0.021(4) -0.007(4) -0.005(4) -0.012(4) C14 0.046(5) 0.023(5) 0.026(4) 0.000(4) -0.006(4) -0.018(4) C15 0.055(6) 0.030(5) 0.030(5) -0.012(4) -0.013(4) -0.009(4) C16 0.078(7) 0.034(6) 0.034(5) 0.001(5) -0.018(5) -0.026(5) C17 0.046(5) 0.031(5) 0.024(4) -0.013(4) -0.006(4) -0.007(4) C18 0.044(5) 0.032(5) 0.018(4) -0.011(4) -0.005(3) -0.006(4) C19 0.056(6) 0.040(6) 0.030(5) -0.014(5) -0.006(4) -0.017(5) C20 0.057(6) 0.042(6) 0.019(4) -0.010(4) 0.003(4) -0.028(5) C21 0.052(5) 0.030(5) 0.024(4) -0.017(4) -0.007(4) -0.004(4) C22 0.040(5) 0.028(5) 0.023(4) -0.011(4) -0.005(4) -0.005(4) C23 0.050(5) 0.023(5) 0.019(4) -0.007(4) -0.003(4) -0.016(4) C24 0.054(6) 0.034(5) 0.025(4) -0.011(4) -0.010(4) -0.014(5) C25 0.035(5) 0.025(5) 0.021(4) -0.010(4) -0.001(3) -0.013(4) N1 0.054(5) 0.019(4) 0.041(4) -0.013(4) -0.011(4) -0.005(4) N2 0.052(5) 0.028(4) 0.028(4) -0.015(3) -0.006(3) -0.011(4) N3 0.054(5) 0.037(5) 0.026(4) -0.001(4) -0.012(3) -0.018(4) N4 0.076(6) 0.037(5) 0.033(4) 0.003(4) -0.021(4) -0.034(4) N5 0.053(5) 0.032(4) 0.022(4) -0.012(3) -0.006(3) -0.011(4) N6 0.053(5) 0.041(5) 0.015(3) -0.010(3) -0.005(3) -0.018(4) O1 0.041(3) 0.024(3) 0.017(3) -0.005(2) -0.003(2) -0.011(3) O2 0.062(4) 0.023(3) 0.020(3) -0.008(3) -0.002(3) -0.005(3) O3 0.040(3) 0.019(3) 0.023(3) -0.004(2) -0.005(2) -0.013(3) O4 0.045(3) 0.023(3) 0.021(3) -0.006(3) -0.007(2) -0.007(3) O5 0.083(5) 0.026(3) 0.019(3) -0.003(3) -0.013(3) -0.029(3) O6 0.057(4) 0.039(4) 0.028(3) -0.017(3) -0.004(3) -0.025(3) O7 0.044(4) 0.031(4) 0.028(3) -0.006(3) -0.009(3) -0.009(3) O8 0.038(3) 0.032(3) 0.023(3) -0.005(3) -0.009(2) -0.004(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 Ag1 N5 2.184(7) . ? Ag1 N2 2.193(7) 2_675 ? Ag1 N4 2.371(7) 2_685 ? Tb1 O6 2.377(6) . ? Tb1 O3 2.390(5) 2_575 ? Tb1 O8 2.393(6) 2_675 ? Tb1 O7 2.425(6) . ? Tb1 O2 2.442(6) . ? Tb1 O4 2.446(6) . ? Tb1 O5 2.488(5) . ? Tb1 O1 2.511(6) . ? Tb1 O3 2.567(5) . ? C1 O1 1.259(9) . ? C1 O2 1.270(10) . ? C1 C2 1.497(11) . ? C2 C7 1.387(12) . ? C2 C3 1.412(12) . ? C3 C4 1.372(13) . ? C3 H3 0.9300 . ? C4 C5 1.395(12) . ? C4 H4 0.9300 . ? C5 N1 1.380(11) . ? C5 C6 1.404(12) . ? C6 C7 1.400(12) . ? C6 N2 1.409(11) . ? C7 H7 0.9300 . ? C8 N2 1.316(11) . ? C8 N1 1.348(11) . ? C8 H8 0.9300 . ? C9 O4 1.231(10) . ? C9 O3 1.312(10) . ? C9 C10 1.490(11) . ? C10 C15 1.391(12) . ? C10 C11 1.391(12) . ? C11 C12 1.385(12) . ? C11 H11 0.9300 . ? C12 C13 1.380(13) . ? C12 H12 0.9300 . ? C13 N3 1.384(11) . ? C13 C14 1.413(12) . ? C14 C15 1.383(12) . ? C14 N4 1.399(11) . ? C15 H15 0.9300 . ? C16 N4 1.332(12) . ? C16 N3 1.332(12) . ? C16 H16 0.9300 . ? C17 O5 1.261(10) . ? C17 O6 1.277(10) . ? C17 C18 1.506(11) . ? C18 C23 1.371(11) . ? C18 C19 1.405(12) . ? C19 C20 1.398(12) . ? C19 H19 0.9300 . ? C20 C21 1.388(12) . ? C20 H20 0.9300 . ? C21 C22 1.387(12) . ? C21 N6 1.393(10) . ? C22 N5 1.394(11) . ? C22 C23 1.401(11) . ? C23 H23 0.9300 . ? C24 N5 1.324(10) . ? C24 N6 1.338(11) . ? C24 H24 0.9300 . ? C25 O7 1.245(9) . ? C25 O8 1.254(10) . ? C25 C25 1.549(15) 2_675 ? N1 H1 0.8600 . ? N2 Ag1 2.193(7) 2_675 ? N3 H3A 0.8600 . ? N4 Ag1 2.371(7) 2_685 ? N6 H6 0.8600 . ? O3 Tb1 2.390(5) 2_575 ? O8 Tb1 2.393(6) 2_675 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Ag1 N2 145.5(3) . 2_675 ? N5 Ag1 N4 112.0(3) . 2_685 ? N2 Ag1 N4 102.3(3) 2_675 2_685 ? O6 Tb1 O3 80.68(19) . 2_575 ? O6 Tb1 O8 128.11(19) . 2_675 ? O3 Tb1 O8 149.29(19) 2_575 2_675 ? O6 Tb1 O7 77.4(2) . . ? O3 Tb1 O7 137.60(19) 2_575 . ? O8 Tb1 O7 67.99(19) 2_675 . ? O6 Tb1 O2 134.3(2) . . ? O3 Tb1 O2 92.4(2) 2_575 . ? O8 Tb1 O2 75.0(2) 2_675 . ? O7 Tb1 O2 78.2(2) . . ? O6 Tb1 O4 109.1(2) . . ? O3 Tb1 O4 92.19(19) 2_575 . ? O8 Tb1 O4 69.9(2) 2_675 . ? O7 Tb1 O4 129.19(19) . . ? O2 Tb1 O4 116.29(18) . . ? O6 Tb1 O5 53.84(19) . . ? O3 Tb1 O5 121.1(2) 2_575 . ? O8 Tb1 O5 78.6(2) 2_675 . ? O7 Tb1 O5 71.7(2) . . ? O2 Tb1 O5 145.6(2) . . ? O4 Tb1 O5 73.34(19) . . ? O6 Tb1 O1 82.72(19) . . ? O3 Tb1 O1 72.02(18) 2_575 . ? O8 Tb1 O1 117.19(19) 2_675 . ? O7 Tb1 O1 69.56(19) . . ? O2 Tb1 O1 52.60(18) . . ? O4 Tb1 O1 158.88(18) . . ? O5 Tb1 O1 126.64(18) . . ? O6 Tb1 O3 143.5(2) . . ? O3 Tb1 O3 70.6(2) 2_575 . ? O8 Tb1 O3 78.75(17) 2_675 . ? O7 Tb1 O3 139.10(18) . . ? O2 Tb1 O3 70.48(19) . . ? O4 Tb1 O3 51.92(17) . . ? O5 Tb1 O3 125.06(19) . . ? O1 Tb1 O3 108.25(17) . . ? O1 C1 O2 120.5(8) . . ? O1 C1 C2 119.0(7) . . ? O2 C1 C2 120.5(7) . . ? C7 C2 C3 121.7(8) . . ? C7 C2 C1 119.3(8) . . ? C3 C2 C1 119.1(7) . . ? C4 C3 C2 121.5(8) . . ? C4 C3 H3 119.2 . . ? C2 C3 H3 119.2 . . ? C3 C4 C5 117.1(8) . . ? C3 C4 H4 121.5 . . ? C5 C4 H4 121.5 . . ? N1 C5 C4 133.3(8) . . ? N1 C5 C6 104.7(8) . . ? C4 C5 C6 122.0(8) . . ? C7 C6 C5 120.6(8) . . ? C7 C6 N2 129.3(8) . . ? C5 C6 N2 110.0(8) . . ? C2 C7 C6 117.0(8) . . ? C2 C7 H7 121.5 . . ? C6 C7 H7 121.5 . . ? N2 C8 N1 114.2(8) . . ? N2 C8 H8 122.9 . . ? N1 C8 H8 122.9 . . ? O4 C9 O3 119.4(8) . . ? O4 C9 C10 122.8(8) . . ? O3 C9 C10 117.5(7) . . ? C15 C10 C11 120.4(8) . . ? C15 C10 C9 117.9(7) . . ? C11 C10 C9 121.7(8) . . ? C12 C11 C10 121.8(8) . . ? C12 C11 H11 119.1 . . ? C10 C11 H11 119.1 . . ? C13 C12 C11 117.1(8) . . ? C13 C12 H12 121.4 . . ? C11 C12 H12 121.4 . . ? C12 C13 N3 133.5(8) . . ? C12 C13 C14 122.3(8) . . ? N3 C13 C14 104.2(7) . . ? C15 C14 N4 130.9(8) . . ? C15 C14 C13 119.2(8) . . ? N4 C14 C13 109.9(7) . . ? C14 C15 C10 119.0(8) . . ? C14 C15 H15 120.5 . . ? C10 C15 H15 120.5 . . ? N4 C16 N3 113.7(9) . . ? N4 C16 H16 123.2 . . ? N3 C16 H16 123.2 . . ? O5 C17 O6 120.6(7) . . ? O5 C17 C18 120.8(8) . . ? O6 C17 C18 118.5(7) . . ? C23 C18 C19 122.2(7) . . ? C23 C18 C17 119.5(7) . . ? C19 C18 C17 118.3(8) . . ? C20 C19 C18 120.7(9) . . ? C20 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? C21 C20 C19 116.4(8) . . ? C21 C20 H20 121.8 . . ? C19 C20 H20 121.8 . . ? C22 C21 C20 123.0(7) . . ? C22 C21 N6 105.9(7) . . ? C20 C21 N6 131.1(8) . . ? C21 C22 N5 109.1(7) . . ? C21 C22 C23 120.2(8) . . ? N5 C22 C23 130.8(8) . . ? C18 C23 C22 117.6(8) . . ? C18 C23 H23 121.2 . . ? C22 C23 H23 121.2 . . ? N5 C24 N6 113.4(8) . . ? N5 C24 H24 123.3 . . ? N6 C24 H24 123.3 . . ? O7 C25 O8 125.5(7) . . ? O7 C25 C25 117.6(9) . 2_675 ? O8 C25 C25 117.0(8) . 2_675 ? C8 N1 C5 107.5(7) . . ? C8 N1 H1 126.3 . . ? C5 N1 H1 126.3 . . ? C8 N2 C6 103.7(7) . . ? C8 N2 Ag1 130.4(6) . 2_675 ? C6 N2 Ag1 119.4(6) . 2_675 ? C16 N3 C13 108.3(7) . . ? C16 N3 H3A 125.9 . . ? C13 N3 H3A 125.9 . . ? C16 N4 C14 103.9(7) . . ? C16 N4 Ag1 121.5(6) . 2_685 ? C14 N4 Ag1 131.8(6) . 2_685 ? C24 N5 C22 105.0(7) . . ? C24 N5 Ag1 124.6(6) . . ? C22 N5 Ag1 130.0(5) . . ? C24 N6 C21 106.6(7) . . ? C24 N6 H6 126.7 . . ? C21 N6 H6 126.7 . . ? C1 O1 Tb1 92.0(5) . . ? C1 O2 Tb1 94.9(5) . . ? C9 O3 Tb1 122.7(5) . 2_575 ? C9 O3 Tb1 86.9(4) . . ? Tb1 O3 Tb1 109.4(2) 2_575 . ? C9 O4 Tb1 94.3(5) . . ? C17 O5 Tb1 90.3(5) . . ? C17 O6 Tb1 95.0(5) . . ? C25 O7 Tb1 118.0(5) . . ? C25 O8 Tb1 119.2(5) . 2_675 ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 25.20 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 1.416 _refine_diff_density_min -1.404 _refine_diff_density_rms 0.211