# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Mei Pan' _publ_contact_author_email panm@mail.sysu.edu.cn loop_ _publ_author_name 'Kang Li' 'Yu Liu' 'Cheng Yan' 'Lei Fu' 'Shi-Chao Wei' 'Hai-Ping Wang' 'Mei Pan' 'Cheng-Yong Su' #===============================# data_2 _database_code_depnum_ccdc_archive 'CCDC 856044' #TrackingRef 'Compounds.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H46 N19 O23 Tb' _chemical_formula_weight 1560.08 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' 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 P21/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 12.9555(2) _cell_length_b 22.6337(4) _cell_length_c 20.6389(4) _cell_angle_alpha 90.00 _cell_angle_beta 94.147(2) _cell_angle_gamma 90.00 _cell_volume 6036.12(18) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 17093 _cell_measurement_theta_min 2.8697 _cell_measurement_theta_max 29.8758 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.717 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3152 _exptl_absorpt_coefficient_mu 1.275 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6295 _exptl_absorpt_correction_T_max 0.7411 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 16.0855 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34688 _diffrn_reflns_av_R_equivalents 0.0327 _diffrn_reflns_av_sigmaI/netI 0.0407 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.88 _diffrn_reflns_theta_max 27.00 _reflns_number_total 13169 _reflns_number_gt 11666 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0369P)^2^+7.9489P] 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 geom _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13169 _refine_ls_number_parameters 928 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0421 _refine_ls_R_factor_gt 0.0352 _refine_ls_wR_factor_ref 0.0855 _refine_ls_wR_factor_gt 0.0816 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tb1 Tb 0.739176(10) 0.240967(6) 0.754994(7) 0.01581(5) Uani 1 1 d . . . N1 N 0.72913(17) 0.12216(11) 0.75817(12) 0.0188(5) Uani 1 1 d . . . N2 N 0.86585(18) 0.19021(11) 0.83341(12) 0.0195(5) Uani 1 1 d . . . N3 N 0.97678(18) 0.11688(11) 0.85944(12) 0.0213(5) Uani 1 1 d . . . N4 N 1.1772(3) 0.05741(19) 0.71666(19) 0.0594(10) Uani 1 1 d . . . N5 N 0.77625(18) 0.18824(11) 0.65317(12) 0.0202(5) Uani 1 1 d . . . N6 N 0.7552(2) 0.11387(12) 0.58230(13) 0.0241(6) Uani 1 1 d . . . N7 N 0.5286(3) 0.05876(19) 0.40477(17) 0.0573(10) Uani 1 1 d . . . N8 N 0.57202(18) 0.19833(11) 0.78186(12) 0.0210(5) Uani 1 1 d . . . N9 N 0.4748(2) 0.13061(12) 0.82701(14) 0.0272(6) Uani 1 1 d . . . N10 N 0.3366(3) 0.0591(3) 1.0169(2) 0.0793(15) Uani 1 1 d . . . N11 N 0.90256(19) 0.41012(12) 0.76881(14) 0.0272(6) Uani 1 1 d . . . N12 N 1.2222(2) 0.41395(14) 0.66088(17) 0.0411(8) Uani 1 1 d . . . N13 N 1.0591(2) 0.22393(13) 0.69043(14) 0.0285(6) Uani 1 1 d . . . N14 N 0.6640(2) 0.24655(12) 0.96285(14) 0.0288(6) Uani 1 1 d . . . N15 N 0.5745(2) 0.44190(14) 1.03870(14) 0.0337(7) Uani 1 1 d . . . N16 N 0.64234(19) 0.41992(12) 0.81264(13) 0.0242(6) Uani 1 1 d . . . N17 N 0.4612(2) 0.23311(12) 0.61907(14) 0.0302(6) Uani 1 1 d . . . N18 N 0.3793(2) 0.41432(13) 0.50161(14) 0.0296(6) Uani 1 1 d . . . N19 N 0.6992(2) 0.40665(12) 0.63987(12) 0.0234(6) Uani 1 1 d . . . C1 C 0.8332(2) 0.09641(13) 0.77424(15) 0.0210(6) Uani 1 1 d . . . H1A H 0.8264 0.0559 0.7915 0.025 Uiso 1 1 calc R . . H1B H 0.8719 0.0942 0.7347 0.025 Uiso 1 1 calc R . . C2 C 0.8900(2) 0.13453(13) 0.82376(14) 0.0184(6) Uani 1 1 d . . . C3 C 0.9433(2) 0.21137(13) 0.87801(14) 0.0197(6) Uani 1 1 d . . . C4 C 0.9582(2) 0.26740(14) 0.90478(16) 0.0264(7) Uani 1 1 d . . . H4A H 0.9112 0.2988 0.8942 0.032 Uiso 1 1 calc R . . C5 C 1.0446(3) 0.27548(16) 0.94750(17) 0.0304(7) Uani 1 1 d . . . H5A H 1.0568 0.3134 0.9663 0.036 Uiso 1 1 calc R . . C6 C 1.1143(2) 0.22991(16) 0.96386(16) 0.0286(7) Uani 1 1 d . . . H6A H 1.1724 0.2374 0.9935 0.034 Uiso 1 1 calc R . . C7 C 1.1000(2) 0.17413(15) 0.93773(15) 0.0246(7) Uani 1 1 d . . . H7A H 1.1469 0.1429 0.9488 0.030 Uiso 1 1 calc R . . C8 C 1.0138(2) 0.16576(14) 0.89438(15) 0.0207(6) Uani 1 1 d . . . C9 C 1.0191(3) 0.05668(15) 0.86248(17) 0.0310(8) Uani 1 1 d . . . H9A H 0.9626 0.0288 0.8708 0.037 Uiso 1 1 calc R . . H9B H 1.0715 0.0541 0.8997 0.037 Uiso 1 1 calc R . . C10 C 1.0676(3) 0.03751(16) 0.80246(17) 0.0315(8) Uani 1 1 d . . . C11 C 1.1292(3) 0.07468(18) 0.76866(19) 0.0397(9) Uani 1 1 d . . . H11A H 1.1379 0.1143 0.7831 0.048 Uiso 1 1 calc R . . C12 C 1.1619(4) -0.0001(2) 0.6971(2) 0.0567(12) Uani 1 1 d . . . H12A H 1.1965 -0.0138 0.6609 0.068 Uiso 1 1 calc R . . C13 C 1.1012(3) -0.0376(2) 0.7260(2) 0.0520(11) Uani 1 1 d . . . H13A H 1.0914 -0.0766 0.7098 0.062 Uiso 1 1 calc R . . C14 C 1.0525(3) -0.01918(19) 0.7798(2) 0.0442(10) Uani 1 1 d . . . H14A H 1.0089 -0.0455 0.8011 0.053 Uiso 1 1 calc R . . C15 C 0.6882(2) 0.10048(14) 0.69316(14) 0.0219(6) Uani 1 1 d . . . H15A H 0.7022 0.0577 0.6891 0.026 Uiso 1 1 calc R . . H15B H 0.6125 0.1068 0.6875 0.026 Uiso 1 1 calc R . . C16 C 0.7406(2) 0.13401(14) 0.64295(15) 0.0216(6) Uani 1 1 d . . . C17 C 0.8164(2) 0.20517(14) 0.59492(15) 0.0218(6) Uani 1 1 d . . . C18 C 0.8627(2) 0.25809(15) 0.57734(16) 0.0258(7) Uani 1 1 d . . . H18A H 0.8699 0.2906 0.6065 0.031 Uiso 1 1 calc R . . C19 C 0.8978(2) 0.26101(16) 0.51556(16) 0.0296(7) Uani 1 1 d . . . H19A H 0.9307 0.2961 0.5025 0.036 Uiso 1 1 calc R . . C20 C 0.8863(2) 0.21420(17) 0.47211(16) 0.0323(8) Uani 1 1 d . . . H20A H 0.9120 0.2181 0.4304 0.039 Uiso 1 1 calc R . . C21 C 0.8386(3) 0.16233(17) 0.48786(16) 0.0323(8) Uani 1 1 d . . . H21A H 0.8299 0.1306 0.4579 0.039 Uiso 1 1 calc R . . C22 C 0.8036(2) 0.15882(14) 0.55038(15) 0.0243(7) Uani 1 1 d . . . C23 C 0.7197(3) 0.05799(16) 0.55276(18) 0.0351(8) Uani 1 1 d . . . H23A H 0.7100 0.0288 0.5875 0.042 Uiso 1 1 calc R . . H23B H 0.7735 0.0426 0.5256 0.042 Uiso 1 1 calc R . . C24 C 0.6185(3) 0.06475(16) 0.51097(18) 0.0360(8) Uani 1 1 d . . . C25 C 0.6148(3) 0.05608(19) 0.4444(2) 0.0466(10) Uani 1 1 d . . . H25A H 0.6780 0.0477 0.4256 0.056 Uiso 1 1 calc R . . C26 C 0.4410(4) 0.07240(19) 0.4332(2) 0.0499(11) Uani 1 1 d . . . H26A H 0.3786 0.0754 0.4062 0.060 Uiso 1 1 calc R . . C27 C 0.4363(3) 0.08219(18) 0.4986(2) 0.0462(10) Uani 1 1 d . . . H27A H 0.3727 0.0917 0.5163 0.055 Uiso 1 1 calc R . . C28 C 0.5275(3) 0.07783(17) 0.5380(2) 0.0416(9) Uani 1 1 d . . . H28A H 0.5270 0.0839 0.5835 0.050 Uiso 1 1 calc R . . C29 C 0.6591(2) 0.10367(13) 0.80741(15) 0.0223(6) Uani 1 1 d . . . H29A H 0.6957 0.1054 0.8512 0.027 Uiso 1 1 calc R . . H29B H 0.6362 0.0625 0.7991 0.027 Uiso 1 1 calc R . . C30 C 0.5674(2) 0.14402(14) 0.80440(15) 0.0228(6) Uani 1 1 d . . . C31 C 0.4754(2) 0.22352(15) 0.79096(15) 0.0242(7) Uani 1 1 d . . . C32 C 0.4364(2) 0.27979(16) 0.77704(16) 0.0279(7) Uani 1 1 d . . . H32A H 0.4774 0.3093 0.7585 0.033 Uiso 1 1 calc R . . C33 C 0.3360(3) 0.29092(18) 0.79136(17) 0.0341(8) Uani 1 1 d . . . H33A H 0.3074 0.3289 0.7821 0.041 Uiso 1 1 calc R . . C34 C 0.2748(3) 0.24837(18) 0.81896(18) 0.0364(9) Uani 1 1 d . . . H34A H 0.2058 0.2579 0.8278 0.044 Uiso 1 1 calc R . . C35 C 0.3127(2) 0.19295(17) 0.83361(18) 0.0346(8) Uani 1 1 d . . . H35A H 0.2716 0.1640 0.8529 0.042 Uiso 1 1 calc R . . C36 C 0.4139(2) 0.18102(15) 0.81904(16) 0.0259(7) Uani 1 1 d . . . C37 C 0.4407(3) 0.07406(16) 0.85206(18) 0.0348(8) Uani 1 1 d . . . H37A H 0.4890 0.0427 0.8399 0.042 Uiso 1 1 calc R . . H37B H 0.3714 0.0646 0.8313 0.042 Uiso 1 1 calc R . . C38 C 0.4353(3) 0.07383(15) 0.92509(18) 0.0308(7) Uani 1 1 d . . . C39 C 0.3441(3) 0.0605(2) 0.9523(2) 0.0489(11) Uani 1 1 d . . . H39A H 0.2844 0.0519 0.9244 0.059 Uiso 1 1 calc R . . C40 C 0.4252(3) 0.0697(2) 1.0554(2) 0.0502(11) Uani 1 1 d . . . H40A H 0.4217 0.0671 1.1012 0.060 Uiso 1 1 calc R . . C41 C 0.5157(3) 0.08327(18) 1.03284(19) 0.0411(9) Uani 1 1 d . . . H41A H 0.5748 0.0913 1.0615 0.049 Uiso 1 1 calc R . . C42 C 0.5209(3) 0.08529(19) 0.9677(2) 0.0463(10) Uani 1 1 d . . . H42A H 0.5849 0.0948 0.9506 0.056 Uiso 1 1 calc R . . C43 C 0.9691(2) 0.31470(14) 0.72773(14) 0.0214(6) Uani 1 1 d . . . C44 C 0.9817(2) 0.37693(14) 0.73743(15) 0.0229(6) Uani 1 1 d . . . C45 C 1.0629(2) 0.40891(14) 0.71668(16) 0.0268(7) Uani 1 1 d . . . H45A H 1.0667 0.4504 0.7234 0.032 Uiso 1 1 calc R . . C46 C 1.1389(2) 0.37978(15) 0.68584(17) 0.0284(7) Uani 1 1 d . . . C47 C 1.1370(2) 0.31952(15) 0.67693(16) 0.0268(7) Uani 1 1 d . . . H47A H 1.1906 0.3001 0.6561 0.032 Uiso 1 1 calc R . . C48 C 1.0556(2) 0.28804(14) 0.69887(15) 0.0236(6) Uani 1 1 d . . . C49 C 0.6631(2) 0.33008(14) 0.88297(15) 0.0208(6) Uani 1 1 d . . . C50 C 0.6496(2) 0.30942(14) 0.94783(15) 0.0227(6) Uani 1 1 d . . . C51 C 0.6214(2) 0.34417(15) 0.99799(16) 0.0256(7) Uani 1 1 d . . . H51A H 0.6133 0.3277 1.0396 0.031 Uiso 1 1 calc R . . C52 C 0.6050(2) 0.40386(15) 0.98666(16) 0.0260(7) Uani 1 1 d . . . C53 C 0.6139(2) 0.42819(14) 0.92557(15) 0.0237(6) Uani 1 1 d . . . H53A H 0.6022 0.4692 0.9183 0.028 Uiso 1 1 calc R . . C54 C 0.6400(2) 0.39185(14) 0.87565(15) 0.0217(6) Uani 1 1 d . . . C55 C 0.5858(2) 0.31697(14) 0.63500(14) 0.0220(6) Uani 1 1 d . . . C56 C 0.4916(2) 0.29327(14) 0.60430(16) 0.0243(7) Uani 1 1 d . . . C57 C 0.4247(2) 0.32394(15) 0.56144(15) 0.0244(7) Uani 1 1 d . . . H57A H 0.3627 0.3062 0.5433 0.029 Uiso 1 1 calc R . . C58 C 0.4501(2) 0.38072(14) 0.54571(15) 0.0236(6) Uani 1 1 d . . . C59 C 0.5398(2) 0.40746(14) 0.57117(14) 0.0227(6) Uani 1 1 d . . . H59A H 0.5563 0.4467 0.5594 0.027 Uiso 1 1 calc R . . C60 C 0.6052(2) 0.37578(14) 0.61421(15) 0.0218(6) Uani 1 1 d . . . O1 O 0.88830(15) 0.28658(10) 0.73941(11) 0.0250(5) Uani 1 1 d . . . O2 O 0.84873(17) 0.38358(11) 0.80567(12) 0.0346(6) Uani 1 1 d . . . O3 O 0.89357(19) 0.46288(11) 0.75695(14) 0.0395(6) Uani 1 1 d . . . O4 O 1.2139(2) 0.46800(12) 0.66042(15) 0.0477(7) Uani 1 1 d . . . O5 O 1.2954(2) 0.38798(14) 0.6414(2) 0.0768(12) Uani 1 1 d . . . O6 O 1.1140(2) 0.20455(12) 0.64970(14) 0.0504(7) Uani 1 1 d . . . O7 O 1.0112(2) 0.19289(11) 0.72537(15) 0.0489(7) Uani 1 1 d . . . O8 O 0.69603(16) 0.29792(10) 0.83875(10) 0.0238(5) Uani 1 1 d . . . O9 O 0.6383(3) 0.21045(12) 0.92111(13) 0.0520(8) Uani 1 1 d . . . O10 O 0.6956(2) 0.23345(12) 1.01815(13) 0.0468(7) Uani 1 1 d . . . O11 O 0.5262(2) 0.41983(12) 1.08169(13) 0.0431(6) Uani 1 1 d . . . O12 O 0.5986(2) 0.49468(11) 1.03652(13) 0.0408(6) Uani 1 1 d . . . O13 O 0.66365(18) 0.47295(10) 0.81097(12) 0.0320(5) Uani 1 1 d . . . O14 O 0.62101(18) 0.38995(11) 0.76399(11) 0.0314(5) Uani 1 1 d . . . O15 O 0.64079(16) 0.28933(9) 0.67859(10) 0.0239(5) Uani 1 1 d . . . O16 O 0.5286(2) 0.19524(11) 0.62594(14) 0.0435(7) Uani 1 1 d . . . O17 O 0.3689(2) 0.22330(13) 0.62336(16) 0.0519(8) Uani 1 1 d . . . O18 O 0.30907(19) 0.38801(13) 0.47098(13) 0.0429(7) Uani 1 1 d . . . O19 O 0.39333(19) 0.46767(12) 0.49760(14) 0.0456(7) Uani 1 1 d . . . O20 O 0.69648(17) 0.46073(10) 0.64331(11) 0.0295(5) Uani 1 1 d . . . O21 O 0.77563(16) 0.37686(11) 0.65596(12) 0.0315(5) Uani 1 1 d . . . O1W O 1.4480(3) 0.0449(2) 0.69595(17) 0.0790(11) Uani 1 1 d . . . O2W O 1.2925(3) 0.10365(18) 0.6208(2) 0.0888(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tb1 0.01713(7) 0.01294(7) 0.01733(8) 0.00038(6) 0.00113(5) 0.00052(5) N1 0.0189(12) 0.0172(12) 0.0200(13) -0.0017(11) 0.0003(10) 0.0004(9) N2 0.0222(12) 0.0162(13) 0.0198(13) 0.0017(10) -0.0009(10) 0.0003(9) N3 0.0213(12) 0.0204(14) 0.0221(13) 0.0023(11) 0.0011(10) 0.0035(9) N4 0.065(2) 0.058(3) 0.057(2) 0.013(2) 0.019(2) 0.0145(19) N5 0.0230(12) 0.0189(13) 0.0187(13) -0.0010(11) 0.0013(10) 0.0008(9) N6 0.0294(14) 0.0208(14) 0.0220(13) -0.0053(11) 0.0005(11) 0.0045(10) N7 0.067(3) 0.065(3) 0.038(2) 0.0082(19) -0.0097(18) -0.016(2) N8 0.0220(12) 0.0178(13) 0.0233(13) -0.0003(11) 0.0018(10) -0.0004(9) N9 0.0298(14) 0.0202(14) 0.0329(15) -0.0041(12) 0.0109(12) -0.0069(10) N10 0.060(3) 0.130(5) 0.050(2) -0.020(3) 0.021(2) -0.008(3) N11 0.0223(13) 0.0259(15) 0.0334(16) -0.0005(13) 0.0013(11) -0.0001(10) N12 0.0405(18) 0.0325(18) 0.053(2) -0.0045(16) 0.0204(15) -0.0086(13) N13 0.0307(14) 0.0229(15) 0.0324(16) -0.0022(13) 0.0047(12) -0.0002(11) N14 0.0356(15) 0.0260(15) 0.0245(14) 0.0029(12) 0.0009(12) 0.0068(11) N15 0.0408(16) 0.0349(18) 0.0260(15) -0.0069(14) 0.0066(13) 0.0023(13) N16 0.0264(13) 0.0211(14) 0.0259(14) -0.0010(12) 0.0072(11) 0.0008(10) N17 0.0348(15) 0.0225(15) 0.0322(16) 0.0028(13) -0.0059(12) 0.0009(11) N18 0.0258(14) 0.0349(17) 0.0282(15) 0.0076(13) 0.0010(12) 0.0043(11) N19 0.0293(14) 0.0239(15) 0.0168(13) 0.0009(11) 0.0002(10) 0.0015(10) C1 0.0239(15) 0.0157(15) 0.0231(15) 0.0007(12) 0.0002(12) 0.0036(11) C2 0.0202(14) 0.0174(15) 0.0179(14) 0.0036(12) 0.0031(11) 0.0009(10) C3 0.0217(14) 0.0190(15) 0.0180(14) 0.0027(12) -0.0004(11) -0.0017(11) C4 0.0302(16) 0.0190(16) 0.0293(17) 0.0008(14) -0.0026(13) 0.0000(12) C5 0.0339(17) 0.0242(17) 0.0324(18) -0.0048(15) -0.0029(14) -0.0053(13) C6 0.0222(15) 0.035(2) 0.0275(17) 0.0005(15) -0.0029(13) -0.0060(13) C7 0.0200(14) 0.0291(18) 0.0248(16) 0.0061(14) 0.0011(12) 0.0029(12) C8 0.0212(14) 0.0207(15) 0.0205(15) 0.0027(13) 0.0039(12) -0.0002(11) C9 0.0338(17) 0.0213(17) 0.037(2) 0.0050(15) -0.0024(15) 0.0049(13) C10 0.0286(17) 0.0285(19) 0.0364(19) -0.0011(16) -0.0034(14) 0.0071(13) C11 0.041(2) 0.037(2) 0.041(2) 0.0011(18) 0.0079(17) 0.0108(16) C12 0.064(3) 0.066(3) 0.040(2) -0.006(2) 0.011(2) 0.023(2) C13 0.062(3) 0.039(2) 0.056(3) -0.014(2) 0.005(2) 0.006(2) C14 0.043(2) 0.038(2) 0.050(2) -0.008(2) -0.0010(18) 0.0037(17) C15 0.0264(15) 0.0169(15) 0.0218(15) -0.0040(13) -0.0015(12) 0.0003(11) C16 0.0197(14) 0.0211(16) 0.0239(16) 0.0000(13) -0.0006(12) 0.0033(11) C17 0.0199(14) 0.0259(17) 0.0195(15) 0.0011(13) -0.0003(11) 0.0047(11) C18 0.0242(15) 0.0266(17) 0.0262(16) 0.0008(14) -0.0013(13) -0.0014(12) C19 0.0254(16) 0.037(2) 0.0264(17) 0.0052(15) 0.0012(13) -0.0038(13) C20 0.0280(17) 0.048(2) 0.0218(17) 0.0039(16) 0.0050(13) 0.0064(15) C21 0.0347(18) 0.040(2) 0.0226(17) -0.0051(16) 0.0025(14) 0.0091(15) C22 0.0284(16) 0.0225(16) 0.0217(16) -0.0010(13) 0.0007(12) 0.0061(12) C23 0.051(2) 0.0226(18) 0.0306(19) -0.0065(15) -0.0005(16) 0.0066(15) C24 0.052(2) 0.0202(17) 0.034(2) -0.0030(16) -0.0078(17) -0.0023(15) C25 0.062(3) 0.041(2) 0.036(2) 0.0020(19) -0.0008(19) -0.0045(19) C26 0.059(3) 0.043(3) 0.045(2) 0.016(2) -0.015(2) -0.0114(19) C27 0.044(2) 0.039(2) 0.054(3) 0.004(2) -0.0047(19) -0.0058(17) C28 0.054(2) 0.030(2) 0.039(2) -0.0044(18) -0.0037(18) -0.0067(17) C29 0.0267(15) 0.0170(15) 0.0236(16) 0.0008(13) 0.0049(12) -0.0019(11) C30 0.0226(14) 0.0217(16) 0.0246(16) -0.0006(13) 0.0048(12) -0.0031(11) C31 0.0212(14) 0.0280(17) 0.0233(16) -0.0039(14) 0.0018(12) -0.0026(12) C32 0.0252(16) 0.0318(18) 0.0263(17) 0.0003(15) 0.0002(13) 0.0000(13) C33 0.0291(17) 0.042(2) 0.0306(18) 0.0011(17) -0.0001(14) 0.0090(14) C34 0.0214(16) 0.052(2) 0.036(2) -0.0056(18) 0.0025(14) 0.0041(14) C35 0.0246(16) 0.045(2) 0.035(2) -0.0031(17) 0.0084(14) -0.0079(14) C36 0.0236(15) 0.0273(17) 0.0272(17) -0.0031(14) 0.0053(13) -0.0046(12) C37 0.0370(19) 0.0282(19) 0.041(2) -0.0029(16) 0.0150(16) -0.0102(14) C38 0.0344(18) 0.0201(17) 0.039(2) -0.0034(15) 0.0067(15) -0.0013(13) C39 0.036(2) 0.075(3) 0.036(2) -0.008(2) 0.0113(17) -0.0039(19) C40 0.059(3) 0.054(3) 0.038(2) -0.003(2) 0.010(2) 0.011(2) C41 0.040(2) 0.044(2) 0.039(2) 0.0074(19) -0.0076(17) 0.0003(16) C42 0.038(2) 0.045(2) 0.055(3) 0.013(2) 0.0006(18) -0.0068(17) C43 0.0213(14) 0.0237(16) 0.0186(15) 0.0040(13) -0.0020(11) -0.0003(11) C44 0.0214(14) 0.0229(16) 0.0242(16) 0.0009(13) 0.0012(12) 0.0017(11) C45 0.0293(16) 0.0186(16) 0.0322(18) 0.0032(14) 0.0011(14) -0.0014(12) C46 0.0223(15) 0.0301(18) 0.0335(19) 0.0036(15) 0.0063(13) -0.0052(12) C47 0.0264(16) 0.0261(17) 0.0287(17) -0.0013(14) 0.0067(13) 0.0010(12) C48 0.0241(15) 0.0213(17) 0.0250(16) 0.0024(13) -0.0010(12) -0.0015(11) C49 0.0161(13) 0.0233(16) 0.0232(15) -0.0042(13) 0.0020(11) -0.0026(11) C50 0.0222(14) 0.0216(16) 0.0242(16) 0.0004(13) 0.0013(12) -0.0004(11) C51 0.0259(15) 0.0284(18) 0.0228(16) 0.0004(14) 0.0029(12) -0.0013(12) C52 0.0296(16) 0.0265(18) 0.0224(16) -0.0076(14) 0.0063(13) 0.0000(12) C53 0.0265(15) 0.0209(16) 0.0241(16) -0.0037(13) 0.0050(12) -0.0006(12) C54 0.0234(14) 0.0207(16) 0.0215(15) -0.0026(13) 0.0045(12) -0.0023(11) C55 0.0248(15) 0.0238(16) 0.0173(15) -0.0023(13) 0.0009(12) 0.0075(12) C56 0.0287(16) 0.0171(15) 0.0273(17) 0.0006(13) 0.0038(13) 0.0027(12) C57 0.0222(15) 0.0307(18) 0.0204(15) -0.0010(14) 0.0027(12) 0.0024(12) C58 0.0248(15) 0.0287(17) 0.0171(15) 0.0019(13) 0.0008(12) 0.0060(12) C59 0.0292(16) 0.0212(16) 0.0182(15) 0.0001(13) 0.0046(12) 0.0028(12) C60 0.0241(15) 0.0219(16) 0.0189(15) -0.0018(13) -0.0005(12) 0.0032(11) O1 0.0202(10) 0.0255(12) 0.0294(12) 0.0054(10) 0.0021(9) -0.0035(8) O2 0.0285(12) 0.0387(15) 0.0376(14) 0.0003(12) 0.0092(10) 0.0015(10) O3 0.0395(14) 0.0228(13) 0.0571(17) 0.0000(13) 0.0100(12) 0.0081(10) O4 0.0418(15) 0.0281(15) 0.075(2) 0.0090(15) 0.0158(14) -0.0074(11) O5 0.064(2) 0.0427(18) 0.133(3) -0.022(2) 0.072(2) -0.0149(15) O6 0.0708(19) 0.0325(15) 0.0522(18) -0.0106(14) 0.0333(15) -0.0016(13) O7 0.0580(17) 0.0227(14) 0.070(2) 0.0113(14) 0.0333(15) 0.0024(12) O8 0.0261(11) 0.0218(11) 0.0241(11) -0.0044(9) 0.0065(9) -0.0001(8) O9 0.096(2) 0.0219(14) 0.0358(15) -0.0013(13) -0.0098(15) -0.0054(14) O10 0.0715(19) 0.0386(16) 0.0284(14) 0.0027(12) -0.0080(13) 0.0232(13) O11 0.0576(17) 0.0438(17) 0.0303(14) -0.0061(13) 0.0201(12) 0.0004(13) O12 0.0594(17) 0.0273(14) 0.0364(15) -0.0109(12) 0.0095(13) -0.0010(11) O13 0.0428(13) 0.0192(12) 0.0346(13) 0.0019(11) 0.0075(11) -0.0049(10) O14 0.0454(14) 0.0291(13) 0.0198(12) -0.0029(10) 0.0018(10) 0.0003(10) O15 0.0304(11) 0.0185(11) 0.0221(11) 0.0021(9) -0.0030(9) 0.0047(8) O16 0.0482(15) 0.0184(13) 0.0616(18) -0.0008(13) -0.0121(13) 0.0042(11) O17 0.0375(15) 0.0410(16) 0.077(2) 0.0179(16) -0.0007(14) -0.0102(12) O18 0.0359(14) 0.0487(17) 0.0417(15) 0.0056(14) -0.0136(12) 0.0006(12) O19 0.0379(14) 0.0361(16) 0.0610(19) 0.0239(14) -0.0097(13) 0.0015(11) O20 0.0358(12) 0.0205(12) 0.0319(13) -0.0025(10) 0.0000(10) 0.0001(9) O21 0.0249(11) 0.0326(14) 0.0359(13) 0.0044(11) -0.0054(10) 0.0039(9) O1W 0.078(2) 0.106(3) 0.053(2) -0.006(2) 0.0021(18) -0.014(2) O2W 0.084(3) 0.066(3) 0.116(3) 0.007(3) 0.000(2) 0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tb1 O1 2.234(2) . ? Tb1 O15 2.240(2) . ? Tb1 O8 2.259(2) . ? Tb1 N8 2.470(2) . ? Tb1 N5 2.494(2) . ? Tb1 N2 2.500(2) . ? Tb1 N1 2.693(2) . ? N1 C29 1.471(4) . ? N1 C1 1.484(3) . ? N1 C15 1.490(4) . ? N2 C2 1.317(4) . ? N2 C3 1.396(4) . ? N3 C2 1.359(4) . ? N3 C8 1.387(4) . ? N3 C9 1.468(4) . ? N4 C11 1.337(5) . ? N4 C12 1.374(6) . ? N5 C16 1.323(4) . ? N5 C17 1.397(4) . ? N6 C16 1.358(4) . ? N6 C22 1.387(4) . ? N6 C23 1.464(4) . ? N7 C25 1.338(5) . ? N7 C26 1.350(6) . ? N8 C30 1.317(4) . ? N8 C31 1.400(4) . ? N9 C30 1.353(4) . ? N9 C36 1.390(4) . ? N9 C37 1.461(4) . ? N10 C39 1.345(6) . ? N10 C40 1.369(6) . ? N11 O3 1.223(4) . ? N11 O2 1.226(4) . ? N11 C44 1.460(4) . ? N12 O5 1.209(4) . ? N12 O4 1.228(4) . ? N12 C46 1.452(4) . ? N13 O7 1.210(4) . ? N13 O6 1.221(4) . ? N13 C48 1.463(4) . ? N14 O10 1.221(4) . ? N14 O9 1.216(4) . ? N14 C50 1.465(4) . ? N15 O11 1.228(4) . ? N15 O12 1.236(4) . ? N15 C52 1.453(4) . ? N16 O14 1.227(3) . ? N16 O13 1.232(3) . ? N16 C54 1.450(4) . ? N17 O17 1.225(4) . ? N17 O16 1.225(4) . ? N17 C56 1.456(4) . ? N18 O19 1.225(4) . ? N18 O18 1.225(4) . ? N18 C58 1.459(4) . ? N19 O21 1.224(3) . ? N19 O20 1.227(3) . ? N19 C60 1.469(4) . ? C1 C2 1.491(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C3 C4 1.391(4) . ? C3 C8 1.404(4) . ? C4 C5 1.386(4) . ? C4 H4A 0.9500 . ? C5 C6 1.396(5) . ? C5 H5A 0.9500 . ? C6 C7 1.380(5) . ? C6 H6A 0.9500 . ? C7 C8 1.393(4) . ? C7 H7A 0.9500 . ? C9 C10 1.494(5) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C14 1.375(5) . ? C10 C11 1.383(5) . ? C11 H11A 0.9500 . ? C12 C13 1.326(7) . ? C12 H12A 0.9500 . ? C13 C14 1.382(6) . ? C13 H13A 0.9500 . ? C14 H14A 0.9500 . ? C15 C16 1.488(4) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C17 C22 1.397(4) . ? C17 C18 1.400(4) . ? C18 C19 1.386(5) . ? C18 H18A 0.9500 . ? C19 C20 1.389(5) . ? C19 H19A 0.9500 . ? C20 C21 1.376(5) . ? C20 H20A 0.9500 . ? C21 C22 1.400(5) . ? C21 H21A 0.9500 . ? C23 C24 1.524(5) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C28 1.372(6) . ? C24 C25 1.386(5) . ? C25 H25A 0.9500 . ? C26 C27 1.374(6) . ? C26 H26A 0.9500 . ? C27 C28 1.390(5) . ? C27 H27A 0.9500 . ? C28 H28A 0.9500 . ? C29 C30 1.496(4) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C31 C32 1.392(5) . ? C31 C36 1.401(4) . ? C32 C33 1.378(5) . ? C32 H32A 0.9500 . ? C33 C34 1.395(5) . ? C33 H33A 0.9500 . ? C34 C35 1.373(5) . ? C34 H34A 0.9500 . ? C35 C36 1.392(4) . ? C35 H35A 0.9500 . ? C37 C38 1.514(5) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.378(5) . ? C38 C42 1.389(5) . ? C39 H39A 0.9500 . ? C40 C41 1.329(6) . ? C40 H40A 0.9500 . ? C41 C42 1.351(6) . ? C41 H41A 0.9500 . ? C42 H42A 0.9500 . ? C43 O1 1.263(4) . ? C43 C44 1.430(4) . ? C43 C48 1.439(4) . ? C44 C45 1.371(4) . ? C45 C46 1.378(5) . ? C45 H45A 0.9500 . ? C46 C47 1.376(5) . ? C47 C48 1.377(4) . ? C47 H47A 0.9500 . ? C49 O8 1.265(4) . ? C49 C54 1.436(4) . ? C49 C50 1.440(4) . ? C50 C51 1.371(4) . ? C51 C52 1.385(5) . ? C51 H51A 0.9500 . ? C52 C53 1.388(4) . ? C53 C54 1.379(4) . ? C53 H53A 0.9500 . ? C55 O15 1.271(3) . ? C55 C56 1.437(4) . ? C55 C60 1.427(4) . ? C56 C57 1.381(4) . ? C57 C58 1.372(5) . ? C57 H57A 0.9500 . ? C58 C59 1.380(4) . ? C59 C60 1.383(4) . ? C59 H59A 0.9500 . ? 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 Tb1 O15 97.29(8) . . ? O1 Tb1 O8 96.37(8) . . ? O15 Tb1 O8 95.75(8) . . ? O1 Tb1 N8 173.76(8) . . ? O15 Tb1 N8 83.42(8) . . ? O8 Tb1 N8 77.39(8) . . ? O1 Tb1 N5 83.03(8) . . ? O15 Tb1 N5 77.00(8) . . ? O8 Tb1 N5 172.55(8) . . ? N8 Tb1 N5 103.16(8) . . ? O1 Tb1 N2 76.79(8) . . ? O15 Tb1 N2 173.62(8) . . ? O8 Tb1 N2 87.36(8) . . ? N8 Tb1 N2 102.73(8) . . ? N5 Tb1 N2 99.69(8) . . ? O1 Tb1 N1 120.57(8) . . ? O15 Tb1 N1 118.62(7) . . ? O8 Tb1 N1 122.42(8) . . ? N8 Tb1 N1 63.88(8) . . ? N5 Tb1 N1 63.59(8) . . ? N2 Tb1 N1 63.64(7) . . ? C29 N1 C1 109.2(2) . . ? C29 N1 C15 109.3(2) . . ? C1 N1 C15 109.3(2) . . ? C29 N1 Tb1 109.52(17) . . ? C1 N1 Tb1 110.66(17) . . ? C15 N1 Tb1 108.77(17) . . ? C2 N2 C3 105.1(2) . . ? C2 N2 Tb1 119.58(19) . . ? C3 N2 Tb1 132.53(19) . . ? C2 N3 C8 106.8(2) . . ? C2 N3 C9 126.0(3) . . ? C8 N3 C9 127.2(3) . . ? C11 N4 C12 116.6(4) . . ? C16 N5 C17 105.3(3) . . ? C16 N5 Tb1 119.5(2) . . ? C17 N5 Tb1 134.4(2) . . ? C16 N6 C22 106.8(3) . . ? C16 N6 C23 127.9(3) . . ? C22 N6 C23 125.1(3) . . ? C25 N7 C26 115.9(4) . . ? C30 N8 C31 105.6(3) . . ? C30 N8 Tb1 120.43(19) . . ? C31 N8 Tb1 132.7(2) . . ? C30 N9 C36 106.6(3) . . ? C30 N9 C37 128.1(3) . . ? C36 N9 C37 125.2(3) . . ? C39 N10 C40 117.1(4) . . ? O3 N11 O2 123.5(3) . . ? O3 N11 C44 118.3(3) . . ? O2 N11 C44 118.2(3) . . ? O5 N12 O4 123.5(3) . . ? O5 N12 C46 118.7(3) . . ? O4 N12 C46 117.8(3) . . ? O7 N13 O6 123.4(3) . . ? O7 N13 C48 118.9(3) . . ? O6 N13 C48 117.6(3) . . ? O10 N14 O9 123.7(3) . . ? O10 N14 C50 117.6(3) . . ? O9 N14 C50 118.6(3) . . ? O11 N15 O12 124.2(3) . . ? O11 N15 C52 118.2(3) . . ? O12 N15 C52 117.6(3) . . ? O14 N16 O13 123.6(3) . . ? O14 N16 C54 118.3(3) . . ? O13 N16 C54 118.1(3) . . ? O17 N17 O16 123.8(3) . . ? O17 N17 C56 117.7(3) . . ? O16 N17 C56 118.5(3) . . ? O19 N18 O18 123.5(3) . . ? O19 N18 C58 117.8(3) . . ? O18 N18 C58 118.6(3) . . ? O21 N19 O20 124.0(3) . . ? O21 N19 C60 118.0(3) . . ? O20 N19 C60 118.0(2) . . ? C2 C1 N1 108.7(2) . . ? C2 C1 H1A 109.9 . . ? N1 C1 H1A 109.9 . . ? C2 C1 H1B 109.9 . . ? N1 C1 H1B 109.9 . . ? H1A C1 H1B 108.3 . . ? N2 C2 N3 113.3(3) . . ? N2 C2 C1 123.2(3) . . ? N3 C2 C1 123.3(3) . . ? C4 C3 N2 130.3(3) . . ? C4 C3 C8 120.3(3) . . ? N2 C3 C8 109.3(3) . . ? C5 C4 C3 117.1(3) . . ? C5 C4 H4A 121.4 . . ? C3 C4 H4A 121.4 . . ? C4 C5 C6 122.3(3) . . ? C4 C5 H5A 118.8 . . ? C6 C5 H5A 118.8 . . ? C7 C6 C5 121.1(3) . . ? C7 C6 H6A 119.5 . . ? C5 C6 H6A 119.5 . . ? C6 C7 C8 117.0(3) . . ? C6 C7 H7A 121.5 . . ? C8 C7 H7A 121.5 . . ? N3 C8 C7 132.4(3) . . ? N3 C8 C3 105.5(2) . . ? C7 C8 C3 122.2(3) . . ? N3 C9 C10 114.3(3) . . ? N3 C9 H9A 108.7 . . ? C10 C9 H9A 108.7 . . ? N3 C9 H9B 108.7 . . ? C10 C9 H9B 108.7 . . ? H9A C9 H9B 107.6 . . ? C14 C10 C11 118.0(4) . . ? C14 C10 C9 119.6(4) . . ? C11 C10 C9 122.3(3) . . ? N4 C11 C10 123.1(4) . . ? N4 C11 H11A 118.5 . . ? C10 C11 H11A 118.5 . . ? C13 C12 N4 123.5(4) . . ? C13 C12 H12A 118.3 . . ? N4 C12 H12A 118.3 . . ? C12 C13 C14 119.3(4) . . ? C12 C13 H13A 120.4 . . ? C14 C13 H13A 120.4 . . ? C10 C14 C13 119.5(4) . . ? C10 C14 H14A 120.2 . . ? C13 C14 H14A 120.2 . . ? C16 C15 N1 108.0(2) . . ? C16 C15 H15A 110.1 . . ? N1 C15 H15A 110.1 . . ? C16 C15 H15B 110.1 . . ? N1 C15 H15B 110.1 . . ? H15A C15 H15B 108.4 . . ? N5 C16 N6 112.9(3) . . ? N5 C16 C15 122.3(3) . . ? N6 C16 C15 124.9(3) . . ? C22 C17 C18 120.3(3) . . ? C22 C17 N5 109.1(3) . . ? C18 C17 N5 130.6(3) . . ? C19 C18 C17 117.0(3) . . ? C19 C18 H18A 121.5 . . ? C17 C18 H18A 121.5 . . ? C18 C19 C20 122.1(3) . . ? C18 C19 H19A 119.0 . . ? C20 C19 H19A 119.0 . . ? C21 C20 C19 121.8(3) . . ? C21 C20 H20A 119.1 . . ? C19 C20 H20A 119.1 . . ? C20 C21 C22 116.5(3) . . ? C20 C21 H21A 121.7 . . ? C22 C21 H21A 121.7 . . ? N6 C22 C17 105.9(3) . . ? N6 C22 C21 131.8(3) . . ? C17 C22 C21 122.2(3) . . ? N6 C23 C24 112.4(3) . . ? N6 C23 H23A 109.1 . . ? C24 C23 H23A 109.1 . . ? N6 C23 H23B 109.1 . . ? C24 C23 H23B 109.1 . . ? H23A C23 H23B 107.9 . . ? C28 C24 C25 117.8(4) . . ? C28 C24 C23 121.3(3) . . ? C25 C24 C23 120.9(4) . . ? N7 C25 C24 124.5(4) . . ? N7 C25 H25A 117.7 . . ? C24 C25 H25A 117.7 . . ? N7 C26 C27 124.2(4) . . ? N7 C26 H26A 117.9 . . ? C27 C26 H26A 117.9 . . ? C26 C27 C28 117.9(4) . . ? C26 C27 H27A 121.0 . . ? C28 C27 H27A 121.0 . . ? C24 C28 C27 119.7(4) . . ? C24 C28 H28A 120.1 . . ? C27 C28 H28A 120.1 . . ? N1 C29 C30 109.0(2) . . ? N1 C29 H29A 109.9 . . ? C30 C29 H29A 109.9 . . ? N1 C29 H29B 109.9 . . ? C30 C29 H29B 109.9 . . ? H29A C29 H29B 108.3 . . ? N8 C30 N9 113.3(3) . . ? N8 C30 C29 121.9(3) . . ? N9 C30 C29 124.8(3) . . ? C32 C31 N8 131.2(3) . . ? C32 C31 C36 120.3(3) . . ? N8 C31 C36 108.5(3) . . ? C33 C32 C31 117.2(3) . . ? C33 C32 H32A 121.4 . . ? C31 C32 H32A 121.4 . . ? C32 C33 C34 122.3(3) . . ? C32 C33 H33A 118.8 . . ? C34 C33 H33A 118.8 . . ? C35 C34 C33 121.1(3) . . ? C35 C34 H34A 119.5 . . ? C33 C34 H34A 119.5 . . ? C34 C35 C36 117.2(3) . . ? C34 C35 H35A 121.4 . . ? C36 C35 H35A 121.4 . . ? C35 C36 N9 132.0(3) . . ? C35 C36 C31 121.9(3) . . ? N9 C36 C31 106.1(3) . . ? N9 C37 C38 113.1(3) . . ? N9 C37 H37A 109.0 . . ? C38 C37 H37A 109.0 . . ? N9 C37 H37B 109.0 . . ? C38 C37 H37B 109.0 . . ? H37A C37 H37B 107.8 . . ? C39 C38 C42 116.9(4) . . ? C39 C38 C37 120.6(3) . . ? C42 C38 C37 122.6(3) . . ? N10 C39 C38 122.3(4) . . ? N10 C39 H39A 118.9 . . ? C38 C39 H39A 118.9 . . ? C41 C40 N10 124.1(4) . . ? C41 C40 H40A 118.0 . . ? N10 C40 H40A 118.0 . . ? C40 C41 C42 117.7(4) . . ? C40 C41 H41A 121.1 . . ? C42 C41 H41A 121.1 . . ? C41 C42 C38 122.0(4) . . ? C41 C42 H42A 119.0 . . ? C38 C42 H42A 119.0 . . ? O1 C43 C44 123.8(3) . . ? O1 C43 C48 123.3(3) . . ? C44 C43 C48 112.8(3) . . ? C45 C44 C43 123.9(3) . . ? C45 C44 N11 116.5(3) . . ? C43 C44 N11 119.5(3) . . ? C44 C45 C46 118.8(3) . . ? C44 C45 H45A 120.6 . . ? C46 C45 H45A 120.6 . . ? C47 C46 C45 122.0(3) . . ? C47 C46 N12 119.1(3) . . ? C45 C46 N12 118.9(3) . . ? C46 C47 C48 118.4(3) . . ? C46 C47 H47A 120.8 . . ? C48 C47 H47A 120.8 . . ? C47 C48 C43 123.9(3) . . ? C47 C48 N13 116.3(3) . . ? C43 C48 N13 119.8(3) . . ? O8 C49 C54 124.3(3) . . ? O8 C49 C50 123.6(3) . . ? C54 C49 C50 112.1(3) . . ? C51 C50 C49 124.9(3) . . ? C51 C50 N14 115.7(3) . . ? C49 C50 N14 119.3(3) . . ? C50 C51 C52 118.6(3) . . ? C50 C51 H51A 120.7 . . ? C52 C51 H51A 120.7 . . ? C53 C52 C51 121.2(3) . . ? C53 C52 N15 118.8(3) . . ? C51 C52 N15 120.0(3) . . ? C54 C53 C52 118.9(3) . . ? C54 C53 H53A 120.6 . . ? C52 C53 H53A 120.6 . . ? C53 C54 C49 124.2(3) . . ? C53 C54 N16 115.5(3) . . ? C49 C54 N16 120.2(3) . . ? O15 C55 C56 122.9(3) . . ? O15 C55 C60 124.7(3) . . ? C56 C55 C60 112.2(3) . . ? C57 C56 C55 124.7(3) . . ? C57 C56 N17 115.9(3) . . ? C55 C56 N17 119.4(3) . . ? C58 C57 C56 118.2(3) . . ? C58 C57 H57A 120.9 . . ? C56 C57 H57A 120.9 . . ? C57 C58 C59 122.1(3) . . ? C57 C58 N18 119.0(3) . . ? C59 C58 N18 118.9(3) . . ? C60 C59 C58 118.5(3) . . ? C60 C59 H59A 120.8 . . ? C58 C59 H59A 120.8 . . ? C59 C60 C55 124.3(3) . . ? C59 C60 N19 116.0(3) . . ? C55 C60 N19 119.7(3) . . ? C43 O1 Tb1 175.9(2) . . ? C49 O8 Tb1 174.45(19) . . ? C55 O15 Tb1 179.4(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Tb1 N1 C29 142.50(17) . . . . ? O15 Tb1 N1 C29 -98.15(18) . . . . ? O8 Tb1 N1 C29 20.6(2) . . . . ? N8 Tb1 N1 C29 -32.53(17) . . . . ? N5 Tb1 N1 C29 -154.30(19) . . . . ? N2 Tb1 N1 C29 88.58(19) . . . . ? O1 Tb1 N1 C1 22.0(2) . . . . ? O15 Tb1 N1 C1 141.37(17) . . . . ? O8 Tb1 N1 C1 -99.84(19) . . . . ? N8 Tb1 N1 C1 -153.0(2) . . . . ? N5 Tb1 N1 C1 85.22(19) . . . . ? N2 Tb1 N1 C1 -31.90(17) . . . . ? O1 Tb1 N1 C15 -98.05(18) . . . . ? O15 Tb1 N1 C15 21.3(2) . . . . ? O8 Tb1 N1 C15 140.09(17) . . . . ? N8 Tb1 N1 C15 86.92(18) . . . . ? N5 Tb1 N1 C15 -34.85(17) . . . . ? N2 Tb1 N1 C15 -151.97(19) . . . . ? O1 Tb1 N2 C2 -111.9(2) . . . . ? O15 Tb1 N2 C2 -89.8(7) . . . . ? O8 Tb1 N2 C2 150.9(2) . . . . ? N8 Tb1 N2 C2 74.5(2) . . . . ? N5 Tb1 N2 C2 -31.5(2) . . . . ? N1 Tb1 N2 C2 22.5(2) . . . . ? O1 Tb1 N2 C3 46.2(3) . . . . ? O15 Tb1 N2 C3 68.3(8) . . . . ? O8 Tb1 N2 C3 -51.0(3) . . . . ? N8 Tb1 N2 C3 -127.4(3) . . . . ? N5 Tb1 N2 C3 126.6(3) . . . . ? N1 Tb1 N2 C3 -179.4(3) . . . . ? O1 Tb1 N5 C16 151.7(2) . . . . ? O15 Tb1 N5 C16 -109.1(2) . . . . ? O8 Tb1 N5 C16 -122.5(6) . . . . ? N8 Tb1 N5 C16 -29.2(2) . . . . ? N2 Tb1 N5 C16 76.4(2) . . . . ? N1 Tb1 N5 C16 22.4(2) . . . . ? O1 Tb1 N5 C17 -39.7(3) . . . . ? O15 Tb1 N5 C17 59.4(3) . . . . ? O8 Tb1 N5 C17 46.0(7) . . . . ? N8 Tb1 N5 C17 139.4(2) . . . . ? N2 Tb1 N5 C17 -115.0(3) . . . . ? N1 Tb1 N5 C17 -169.0(3) . . . . ? O1 Tb1 N8 C30 -115.3(7) . . . . ? O15 Tb1 N8 C30 147.8(2) . . . . ? O8 Tb1 N8 C30 -114.8(2) . . . . ? N5 Tb1 N8 C30 72.8(2) . . . . ? N2 Tb1 N8 C30 -30.5(2) . . . . ? N1 Tb1 N8 C30 21.4(2) . . . . ? O1 Tb1 N8 C31 49.6(9) . . . . ? O15 Tb1 N8 C31 -47.3(3) . . . . ? O8 Tb1 N8 C31 50.1(3) . . . . ? N5 Tb1 N8 C31 -122.3(3) . . . . ? N2 Tb1 N8 C31 134.4(3) . . . . ? N1 Tb1 N8 C31 -173.7(3) . . . . ? C29 N1 C1 C2 -82.5(3) . . . . ? C15 N1 C1 C2 157.9(2) . . . . ? Tb1 N1 C1 C2 38.1(3) . . . . ? C3 N2 C2 N3 1.0(3) . . . . ? Tb1 N2 C2 N3 164.46(19) . . . . ? C3 N2 C2 C1 -173.8(3) . . . . ? Tb1 N2 C2 C1 -10.3(4) . . . . ? C8 N3 C2 N2 -1.4(3) . . . . ? C9 N3 C2 N2 175.7(3) . . . . ? C8 N3 C2 C1 173.3(3) . . . . ? C9 N3 C2 C1 -9.6(5) . . . . ? N1 C1 C2 N2 -21.2(4) . . . . ? N1 C1 C2 N3 164.6(3) . . . . ? C2 N2 C3 C4 178.7(3) . . . . ? Tb1 N2 C3 C4 18.3(5) . . . . ? C2 N2 C3 C8 -0.2(3) . . . . ? Tb1 N2 C3 C8 -160.6(2) . . . . ? N2 C3 C4 C5 -178.8(3) . . . . ? C8 C3 C4 C5 0.0(5) . . . . ? C3 C4 C5 C6 -0.3(5) . . . . ? C4 C5 C6 C7 0.1(5) . . . . ? C5 C6 C7 C8 0.3(5) . . . . ? C2 N3 C8 C7 -179.0(3) . . . . ? C9 N3 C8 C7 4.0(5) . . . . ? C2 N3 C8 C3 1.2(3) . . . . ? C9 N3 C8 C3 -175.8(3) . . . . ? C6 C7 C8 N3 179.5(3) . . . . ? C6 C7 C8 C3 -0.6(5) . . . . ? C4 C3 C8 N3 -179.6(3) . . . . ? N2 C3 C8 N3 -0.6(3) . . . . ? C4 C3 C8 C7 0.5(5) . . . . ? N2 C3 C8 C7 179.5(3) . . . . ? C2 N3 C9 C10 72.3(4) . . . . ? C8 N3 C9 C10 -111.2(4) . . . . ? N3 C9 C10 C14 -139.8(3) . . . . ? N3 C9 C10 C11 41.2(5) . . . . ? C12 N4 C11 C10 0.6(6) . . . . ? C14 C10 C11 N4 -2.3(6) . . . . ? C9 C10 C11 N4 176.7(3) . . . . ? C11 N4 C12 C13 1.6(7) . . . . ? N4 C12 C13 C14 -1.9(7) . . . . ? C11 C10 C14 C13 2.0(6) . . . . ? C9 C10 C14 C13 -177.1(3) . . . . ? C12 C13 C14 C10 0.0(6) . . . . ? C29 N1 C15 C16 163.3(2) . . . . ? C1 N1 C15 C16 -77.2(3) . . . . ? Tb1 N1 C15 C16 43.7(3) . . . . ? C17 N5 C16 N6 0.5(3) . . . . ? Tb1 N5 C16 N6 172.00(17) . . . . ? C17 N5 C16 C15 -178.1(3) . . . . ? Tb1 N5 C16 C15 -6.5(4) . . . . ? C22 N6 C16 N5 -0.4(3) . . . . ? C23 N6 C16 N5 -175.5(3) . . . . ? C22 N6 C16 C15 178.1(3) . . . . ? C23 N6 C16 C15 3.0(5) . . . . ? N1 C15 C16 N5 -27.8(4) . . . . ? N1 C15 C16 N6 153.8(3) . . . . ? C16 N5 C17 C22 -0.4(3) . . . . ? Tb1 N5 C17 C22 -170.1(2) . . . . ? C16 N5 C17 C18 179.2(3) . . . . ? Tb1 N5 C17 C18 9.5(5) . . . . ? C22 C17 C18 C19 -2.2(4) . . . . ? N5 C17 C18 C19 178.3(3) . . . . ? C17 C18 C19 C20 1.1(5) . . . . ? C18 C19 C20 C21 0.5(5) . . . . ? C19 C20 C21 C22 -0.9(5) . . . . ? C16 N6 C22 C17 0.1(3) . . . . ? C23 N6 C22 C17 175.4(3) . . . . ? C16 N6 C22 C21 178.7(3) . . . . ? C23 N6 C22 C21 -6.0(5) . . . . ? C18 C17 C22 N6 -179.4(3) . . . . ? N5 C17 C22 N6 0.2(3) . . . . ? C18 C17 C22 C21 1.8(5) . . . . ? N5 C17 C22 C21 -178.6(3) . . . . ? C20 C21 C22 N6 -178.6(3) . . . . ? C20 C21 C22 C17 -0.2(5) . . . . ? C16 N6 C23 C24 96.6(4) . . . . ? C22 N6 C23 C24 -77.7(4) . . . . ? N6 C23 C24 C28 -67.6(5) . . . . ? N6 C23 C24 C25 114.4(4) . . . . ? C26 N7 C25 C24 1.7(6) . . . . ? C28 C24 C25 N7 -1.0(6) . . . . ? C23 C24 C25 N7 177.1(4) . . . . ? C25 N7 C26 C27 -1.2(7) . . . . ? N7 C26 C27 C28 0.1(7) . . . . ? C25 C24 C28 C27 -0.3(6) . . . . ? C23 C24 C28 C27 -178.4(3) . . . . ? C26 C27 C28 C24 0.7(6) . . . . ? C1 N1 C29 C30 161.7(2) . . . . ? C15 N1 C29 C30 -78.8(3) . . . . ? Tb1 N1 C29 C30 40.3(3) . . . . ? C31 N8 C30 N9 0.9(4) . . . . ? Tb1 N8 C30 N9 169.5(2) . . . . ? C31 N8 C30 C29 -175.8(3) . . . . ? Tb1 N8 C30 C29 -7.3(4) . . . . ? C36 N9 C30 N8 -0.6(4) . . . . ? C37 N9 C30 N8 176.4(3) . . . . ? C36 N9 C30 C29 176.0(3) . . . . ? C37 N9 C30 C29 -6.9(5) . . . . ? N1 C29 C30 N8 -25.1(4) . . . . ? N1 C29 C30 N9 158.6(3) . . . . ? C30 N8 C31 C32 179.2(3) . . . . ? Tb1 N8 C31 C32 12.7(5) . . . . ? C30 N8 C31 C36 -0.8(3) . . . . ? Tb1 N8 C31 C36 -167.3(2) . . . . ? N8 C31 C32 C33 179.2(3) . . . . ? C36 C31 C32 C33 -0.7(5) . . . . ? C31 C32 C33 C34 0.3(5) . . . . ? C32 C33 C34 C35 0.4(6) . . . . ? C33 C34 C35 C36 -0.7(5) . . . . ? C34 C35 C36 N9 -179.7(4) . . . . ? C34 C35 C36 C31 0.4(5) . . . . ? C30 N9 C36 C35 -179.9(4) . . . . ? C37 N9 C36 C35 2.9(6) . . . . ? C30 N9 C36 C31 0.1(4) . . . . ? C37 N9 C36 C31 -177.1(3) . . . . ? C32 C31 C36 C35 0.4(5) . . . . ? N8 C31 C36 C35 -179.6(3) . . . . ? C32 C31 C36 N9 -179.6(3) . . . . ? N8 C31 C36 N9 0.5(4) . . . . ? C30 N9 C37 C38 106.7(4) . . . . ? C36 N9 C37 C38 -76.7(4) . . . . ? N9 C37 C38 C39 122.6(4) . . . . ? N9 C37 C38 C42 -59.1(5) . . . . ? C40 N10 C39 C38 -2.2(8) . . . . ? C42 C38 C39 N10 0.8(7) . . . . ? C37 C38 C39 N10 179.2(5) . . . . ? C39 N10 C40 C41 2.7(8) . . . . ? N10 C40 C41 C42 -1.7(7) . . . . ? C40 C41 C42 C38 0.1(7) . . . . ? C39 C38 C42 C41 0.3(6) . . . . ? C37 C38 C42 C41 -178.0(4) . . . . ? O1 C43 C44 C45 -170.7(3) . . . . ? C48 C43 C44 C45 5.1(4) . . . . ? O1 C43 C44 N11 6.7(5) . . . . ? C48 C43 C44 N11 -177.4(3) . . . . ? O3 N11 C44 C45 23.1(4) . . . . ? O2 N11 C44 C45 -156.9(3) . . . . ? O3 N11 C44 C43 -154.6(3) . . . . ? O2 N11 C44 C43 25.5(4) . . . . ? C43 C44 C45 C46 -1.5(5) . . . . ? N11 C44 C45 C46 -179.0(3) . . . . ? C44 C45 C46 C47 -1.8(5) . . . . ? C44 C45 C46 N12 176.9(3) . . . . ? O5 N12 C46 C47 -10.5(6) . . . . ? O4 N12 C46 C47 169.0(3) . . . . ? O5 N12 C46 C45 170.7(4) . . . . ? O4 N12 C46 C45 -9.8(5) . . . . ? C45 C46 C47 C48 1.0(5) . . . . ? N12 C46 C47 C48 -177.8(3) . . . . ? C46 C47 C48 C43 3.3(5) . . . . ? C46 C47 C48 N13 -177.8(3) . . . . ? O1 C43 C48 C47 169.8(3) . . . . ? C44 C43 C48 C47 -6.1(4) . . . . ? O1 C43 C48 N13 -9.0(5) . . . . ? C44 C43 C48 N13 175.1(3) . . . . ? O7 N13 C48 C47 156.7(3) . . . . ? O6 N13 C48 C47 -20.6(4) . . . . ? O7 N13 C48 C43 -24.3(4) . . . . ? O6 N13 C48 C43 158.4(3) . . . . ? O8 C49 C50 C51 175.0(3) . . . . ? C54 C49 C50 C51 -2.0(4) . . . . ? O8 C49 C50 N14 -6.6(4) . . . . ? C54 C49 C50 N14 176.4(3) . . . . ? O10 N14 C50 C51 -32.0(4) . . . . ? O9 N14 C50 C51 143.8(3) . . . . ? O10 N14 C50 C49 149.5(3) . . . . ? O9 N14 C50 C49 -34.8(4) . . . . ? C49 C50 C51 C52 -0.5(5) . . . . ? N14 C50 C51 C52 -178.9(3) . . . . ? C50 C51 C52 C53 1.7(5) . . . . ? C50 C51 C52 N15 179.7(3) . . . . ? O11 N15 C52 C53 150.2(3) . . . . ? O12 N15 C52 C53 -29.4(4) . . . . ? O11 N15 C52 C51 -27.9(5) . . . . ? O12 N15 C52 C51 152.5(3) . . . . ? C51 C52 C53 C54 -0.2(5) . . . . ? N15 C52 C53 C54 -178.2(3) . . . . ? C52 C53 C54 C49 -2.7(5) . . . . ? C52 C53 C54 N16 176.8(3) . . . . ? O8 C49 C54 C53 -173.4(3) . . . . ? C50 C49 C54 C53 3.6(4) . . . . ? O8 C49 C54 N16 7.2(4) . . . . ? C50 C49 C54 N16 -175.9(2) . . . . ? O14 N16 C54 C53 -149.4(3) . . . . ? O13 N16 C54 C53 29.2(4) . . . . ? O14 N16 C54 C49 30.1(4) . . . . ? O13 N16 C54 C49 -151.3(3) . . . . ? O15 C55 C56 C57 173.5(3) . . . . ? C60 C55 C56 C57 -2.4(4) . . . . ? O15 C55 C56 N17 -5.4(5) . . . . ? C60 C55 C56 N17 178.7(3) . . . . ? O17 N17 C56 C57 -36.8(4) . . . . ? O16 N17 C56 C57 142.5(3) . . . . ? O17 N17 C56 C55 142.1(3) . . . . ? O16 N17 C56 C55 -38.5(4) . . . . ? C55 C56 C57 C58 1.4(5) . . . . ? N17 C56 C57 C58 -179.7(3) . . . . ? C56 C57 C58 C59 0.2(5) . . . . ? C56 C57 C58 N18 -178.7(3) . . . . ? O19 N18 C58 C57 166.7(3) . . . . ? O18 N18 C58 C57 -12.9(4) . . . . ? O19 N18 C58 C59 -12.2(4) . . . . ? O18 N18 C58 C59 168.2(3) . . . . ? C57 C58 C59 C60 -0.5(5) . . . . ? N18 C58 C59 C60 178.4(3) . . . . ? C58 C59 C60 C55 -0.8(5) . . . . ? C58 C59 C60 N19 -179.7(3) . . . . ? O15 C55 C60 C59 -173.7(3) . . . . ? C56 C55 C60 C59 2.0(4) . . . . ? O15 C55 C60 N19 5.2(5) . . . . ? C56 C55 C60 N19 -179.0(3) . . . . ? O21 N19 C60 C59 -151.9(3) . . . . ? O20 N19 C60 C59 27.4(4) . . . . ? O21 N19 C60 C55 29.1(4) . . . . ? O20 N19 C60 C55 -151.6(3) . . . . ? C44 C43 O1 Tb1 59(3) . . . . ? C48 C43 O1 Tb1 -116(3) . . . . ? O15 Tb1 O1 C43 5(3) . . . . ? O8 Tb1 O1 C43 -92(3) . . . . ? N8 Tb1 O1 C43 -91(3) . . . . ? N5 Tb1 O1 C43 81(3) . . . . ? N2 Tb1 O1 C43 -178(100) . . . . ? N1 Tb1 O1 C43 134(3) . . . . ? C54 C49 O8 Tb1 -73(2) . . . . ? C50 C49 O8 Tb1 111(2) . . . . ? O1 Tb1 O8 C49 135(2) . . . . ? O15 Tb1 O8 C49 37(2) . . . . ? N8 Tb1 O8 C49 -45(2) . . . . ? N5 Tb1 O8 C49 50(2) . . . . ? N2 Tb1 O8 C49 -149(2) . . . . ? N1 Tb1 O8 C49 -93(2) . . . . ? C56 C55 O15 Tb1 142(24) . . . . ? C60 C55 O15 Tb1 -43(24) . . . . ? O1 Tb1 O15 C55 14(24) . . . . ? O8 Tb1 O15 C55 111(24) . . . . ? N8 Tb1 O15 C55 -172(100) . . . . ? N5 Tb1 O15 C55 -67(24) . . . . ? N2 Tb1 O15 C55 -8(24) . . . . ? N1 Tb1 O15 C55 -117(24) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.844 _refine_diff_density_min -0.875 _refine_diff_density_rms 0.084 #===============================# data_4 _database_code_depnum_ccdc_archive 'CCDC 856045' #TrackingRef 'Compounds.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H16.33 N5.83 O5.17 Tb0.50' _chemical_formula_weight 452.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -9.1472 9.1891 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M P31c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, z+1/2' 'x-y, -y, z+1/2' '-x, -x+y, z+1/2' _cell_length_a 19.5224(3) _cell_length_b 19.5224(3) _cell_length_c 8.4283(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2781.87(9) _cell_formula_units_Z 6 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.621 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1362 _exptl_absorpt_coefficient_mu 10.003 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.346 _exptl_absorpt_correction_T_max 0.368 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13568 _diffrn_reflns_av_R_equivalents 0.0480 _diffrn_reflns_av_sigmaI/netI 0.0381 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 62.61 _reflns_number_total 2502 _reflns_number_gt 2082 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1000P)^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 geom _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 0.016(9) _refine_ls_number_reflns 2502 _refine_ls_number_parameters 275 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0491 _refine_ls_R_factor_gt 0.0425 _refine_ls_wR_factor_ref 0.1180 _refine_ls_wR_factor_gt 0.1140 _refine_ls_goodness_of_fit_ref 0.914 _refine_ls_restrained_S_all 0.913 _refine_ls_shift/su_max 0.090 _refine_ls_shift/su_mean 0.009 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 0.6667 0.3333 -0.23333(6) 0.02908(19) Uani 1 3 d S . . N1 N 0.6667 0.3333 0.0879(13) 0.037(2) Uani 1 3 d S . . N2 N 0.5358(3) 0.2920(3) -0.1034(8) 0.0390(13) Uani 1 1 d . . . N3 N 0.4474(3) 0.2372(3) 0.0909(7) 0.0428(14) Uani 1 1 d . . . C1 C 0.5897(5) 0.2715(5) 0.1448(9) 0.0449(17) Uani 1 1 d . . . H1A H 0.5824 0.2826 0.2562 0.054 Uiso 1 1 calc R . . H1B H 0.5878 0.2199 0.1418 0.054 Uiso 1 1 calc R . . C2 C 0.5244(4) 0.2671(4) 0.0458(9) 0.0375(15) Uani 1 1 d . . . C3 C 0.4624(4) 0.2803(4) -0.1550(9) 0.0404(16) Uani 1 1 d . . . C4 C 0.4390(4) 0.2963(5) -0.2989(10) 0.0467(17) Uani 1 1 d . . . H4A H 0.4762 0.3193 -0.3829 0.056 Uiso 1 1 calc R . . C5 C 0.3634(5) 0.2794(5) -0.3201(12) 0.058(2) Uani 1 1 d . . . H5A H 0.3477 0.2918 -0.4175 0.069 Uiso 1 1 calc R . . C6 C 0.3083(6) 0.2432(6) -0.1966(13) 0.066(3) Uani 1 1 d . . . H6A H 0.2552 0.2304 -0.2147 0.079 Uiso 1 1 calc R . . C7 C 0.3270(4) 0.2256(5) -0.0539(12) 0.052(2) Uani 1 1 d . . . H7A H 0.2891 0.2014 0.0284 0.062 Uiso 1 1 calc R . . C8 C 0.4075(4) 0.2458(4) -0.0355(9) 0.0441(17) Uani 1 1 d . . . C9 C 0.4142(4) 0.2087(6) 0.2469(12) 0.0529(19) Uani 1 1 d . . . H9A H 0.3842 0.2346 0.2815 0.063 Uiso 1 1 calc R . . H9B H 0.4573 0.2222 0.3241 0.063 Uiso 1 1 calc R . . C10 C 0.3586(5) 0.1181(6) 0.2432(11) 0.062(2) Uani 1 1 d . . . C11 C 0.2828(7) 0.0899(10) 0.3054(19) 0.126(5) Uani 1 1 d . . . H11A H 0.2710 0.1280 0.3474 0.151 Uiso 1 1 calc R . . N4 N 0.2274(9) 0.0169(10) 0.311(3) 0.171(8) Uani 1 1 d . . . C12 C 0.2547(11) -0.0343(11) 0.259(2) 0.155(9) Uani 1 1 d . . . H12A H 0.2188 -0.0896 0.2666 0.186 Uiso 1 1 calc R . . C13 C 0.3303(11) -0.0104(11) 0.197(3) 0.152(10) Uani 1 1 d . . . H13A H 0.3440 -0.0478 0.1584 0.183 Uiso 1 1 calc R . . C14 C 0.3837(9) 0.0700(8) 0.194(2) 0.116(6) Uani 1 1 d . . . H14A H 0.4364 0.0899 0.1573 0.140 Uiso 1 1 calc R . . N5 N 0.5416(4) 0.2037(4) -0.4135(8) 0.0463(15) Uani 1 1 d . . . O1 O 0.5699(3) 0.2756(3) -0.4511(6) 0.0392(11) Uani 1 1 d . . . O2 O 0.5697(3) 0.1892(3) -0.2905(6) 0.0466(12) Uani 1 1 d . . . O3 O 0.4904(4) 0.1487(4) -0.4931(9) 0.0713(19) Uani 1 1 d . . . Tb2 Tb 0.0000 0.0000 0.7430(3) 0.0702(9) Uani 0.50 3 d SP . . N6 N 0.1414(9) 0.1118(9) 0.576(3) 0.090(6) Uani 0.50 1 d P . . O4 O 0.1151(7) 0.1350(7) 0.6795(17) 0.069(3) Uani 0.50 1 d P . . O5 O 0.1041(8) 0.0314(9) 0.549(2) 0.085(4) Uani 0.50 1 d P . . O6 O 0.1974(8) 0.1511(8) 0.497(2) 0.083(4) Uani 0.50 1 d P . . O7 O -0.0114(8) 0.0894(7) 0.918(2) 0.077(4) Uani 0.50 1 d P . . C15 C 0.5607(6) 0.0537(5) -0.6625(11) 0.062(2) Uani 1 1 d . . . C16 C 0.5037(9) -0.0150(6) -0.5774(17) 0.103(4) Uani 1 1 d . . . H16A H 0.4924 0.0011 -0.4751 0.155 Uiso 1 1 calc R . . H16B H 0.5250 -0.0504 -0.5595 0.155 Uiso 1 1 calc R . . H16C H 0.4549 -0.0426 -0.6395 0.155 Uiso 1 1 calc R . . N7 N 0.6051(5) 0.1061(6) -0.7259(14) 0.094(3) Uani 1 1 d . . . O8 O 0.0000 0.0000 1.066(2) 0.052(5) Uani 0.50 3 d SP . . 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 0.0312(2) 0.0312(2) 0.0248(3) 0.000 0.000 0.01561(11) N1 0.037(3) 0.037(3) 0.036(6) 0.000 0.000 0.0186(16) N2 0.033(3) 0.038(3) 0.046(4) 0.002(3) 0.004(3) 0.018(3) N3 0.041(3) 0.038(3) 0.043(4) -0.003(3) 0.011(3) 0.015(3) C1 0.063(5) 0.053(4) 0.028(4) 0.006(3) 0.007(3) 0.035(4) C2 0.034(4) 0.043(4) 0.038(4) -0.002(3) 0.004(3) 0.021(3) C3 0.035(3) 0.034(3) 0.049(4) -0.006(3) 0.005(3) 0.014(3) C4 0.042(4) 0.050(4) 0.052(5) -0.007(4) -0.012(3) 0.025(3) C5 0.049(4) 0.065(5) 0.064(6) -0.011(4) -0.011(4) 0.033(4) C6 0.057(5) 0.077(6) 0.078(7) -0.011(5) -0.020(5) 0.044(5) C7 0.043(4) 0.047(4) 0.071(6) -0.008(4) 0.011(4) 0.027(3) C8 0.042(4) 0.042(4) 0.048(4) -0.012(3) -0.007(3) 0.021(3) C9 0.049(4) 0.063(5) 0.046(5) -0.003(4) 0.002(4) 0.028(4) C10 0.054(5) 0.064(5) 0.056(6) 0.005(4) 0.007(4) 0.021(4) C11 0.063(7) 0.122(11) 0.127(12) 0.024(10) 0.026(8) -0.003(8) N4 0.102(10) 0.127(12) 0.26(2) 0.100(13) -0.008(11) 0.040(10) C12 0.105(12) 0.095(12) 0.157(18) 0.078(13) -0.010(11) -0.030(10) C13 0.18(2) 0.074(9) 0.17(2) -0.011(11) 0.033(14) 0.036(11) C14 0.094(9) 0.067(7) 0.165(16) 0.003(8) 0.049(10) 0.023(7) N5 0.043(3) 0.057(4) 0.042(4) -0.008(3) -0.004(3) 0.027(3) O1 0.049(3) 0.036(2) 0.033(3) -0.007(2) -0.011(2) 0.022(2) O2 0.051(3) 0.033(2) 0.049(3) 0.000(2) 0.002(2) 0.016(2) O3 0.066(4) 0.056(3) 0.076(5) -0.028(3) -0.025(3) 0.019(3) Tb2 0.0510(6) 0.0510(6) 0.109(3) 0.000 0.000 0.0255(3) N6 0.043(8) 0.040(8) 0.151(18) 0.015(10) 0.031(11) -0.006(7) O4 0.051(6) 0.059(8) 0.077(9) -0.022(7) 0.004(6) 0.011(6) O5 0.055(7) 0.077(9) 0.122(13) -0.010(9) 0.005(8) 0.032(7) O6 0.064(8) 0.060(8) 0.118(12) 0.005(8) 0.004(8) 0.026(7) O7 0.069(8) 0.045(6) 0.116(12) 0.003(7) 0.009(8) 0.027(6) C15 0.079(6) 0.046(5) 0.055(5) -0.001(4) 0.002(5) 0.025(5) C16 0.154(12) 0.054(5) 0.092(9) 0.016(6) 0.040(8) 0.045(7) N7 0.064(5) 0.068(6) 0.136(9) 0.020(6) 0.015(6) 0.023(5) O8 0.043(6) 0.043(6) 0.071(14) 0.000 0.000 0.021(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 O1 2.466(5) 2_655 ? Tb1 O1 2.466(5) . ? Tb1 O1 2.466(5) 3_665 ? Tb1 N2 2.513(6) 2_655 ? Tb1 N2 2.513(6) 3_665 ? Tb1 N2 2.513(6) . ? Tb1 O2 2.532(5) 2_655 ? Tb1 O2 2.532(5) . ? Tb1 O2 2.532(5) 3_665 ? Tb1 N1 2.708(11) . ? Tb1 N5 2.914(7) 2_655 ? Tb1 N5 2.914(7) . ? N1 C1 1.460(9) 2_655 ? N1 C1 1.460(9) . ? N1 C1 1.460(9) 3_665 ? N2 C2 1.327(9) . ? N2 C3 1.402(9) . ? N3 C2 1.367(9) . ? N3 C8 1.378(10) . ? N3 C9 1.449(11) . ? C1 C2 1.488(10) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C3 C4 1.386(11) . ? C3 C8 1.377(10) . ? C4 C5 1.353(11) . ? C4 H4A 0.9500 . ? C5 C6 1.407(15) . ? C5 H5A 0.9500 . ? C6 C7 1.350(14) . ? C6 H6A 0.9500 . ? C7 C8 1.425(10) . ? C7 H7A 0.9500 . ? C9 C10 1.545(14) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C14 1.325(17) . ? C10 C11 1.398(15) . ? C11 N4 1.29(2) . ? C11 H11A 0.9500 . ? N4 C12 1.42(3) . ? C12 C13 1.41(3) . ? C12 H12A 0.9500 . ? C13 C14 1.38(2) . ? C13 H13A 0.9500 . ? C14 H14A 0.9500 . ? N5 O1 1.264(8) . ? N5 O3 1.237(9) . ? N5 O2 1.270(8) . ? Tb2 O8 1.49(2) 4_554 ? Tb2 O7 2.382(14) . ? Tb2 O7 2.382(14) 3 ? Tb2 O7 2.382(14) 2 ? Tb2 O5 2.434(15) 3 ? Tb2 O5 2.434(15) 2 ? Tb2 O5 2.434(15) . ? Tb2 O4 2.521(12) 2 ? Tb2 O4 2.521(12) . ? Tb2 O4 2.521(12) 3 ? Tb2 O8 2.72(2) . ? N6 O6 1.18(2) . ? N6 O5 1.38(2) . ? N6 O4 1.21(2) . ? O5 O7 1.33(2) 4_554 ? O7 O5 1.33(2) 4 ? C15 N7 1.093(12) . ? C15 C16 1.436(14) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? O8 Tb2 1.49(2) 4 ? 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 Tb1 O1 70.7(2) 2_655 . ? O1 Tb1 O1 70.7(2) 2_655 3_665 ? O1 Tb1 O1 70.7(2) . 3_665 ? O1 Tb1 N2 75.7(2) 2_655 2_655 ? O1 Tb1 N2 116.45(18) . 2_655 ? O1 Tb1 N2 140.68(17) 3_665 2_655 ? O1 Tb1 N2 116.45(18) 2_655 3_665 ? O1 Tb1 N2 140.68(17) . 3_665 ? O1 Tb1 N2 75.7(2) 3_665 3_665 ? N2 Tb1 N2 102.43(18) 2_655 3_665 ? O1 Tb1 N2 140.68(17) 2_655 . ? O1 Tb1 N2 75.7(2) . . ? O1 Tb1 N2 116.45(18) 3_665 . ? N2 Tb1 N2 102.43(18) 2_655 . ? N2 Tb1 N2 102.43(18) 3_665 . ? O1 Tb1 O2 51.23(17) 2_655 2_655 ? O1 Tb1 O2 118.89(18) . 2_655 ? O1 Tb1 O2 73.63(16) 3_665 2_655 ? N2 Tb1 O2 69.56(19) 2_655 2_655 ? N2 Tb1 O2 68.38(19) 3_665 2_655 ? N2 Tb1 O2 165.12(19) . 2_655 ? O1 Tb1 O2 73.63(16) 2_655 . ? O1 Tb1 O2 51.23(17) . . ? O1 Tb1 O2 118.89(18) 3_665 . ? N2 Tb1 O2 68.38(19) 2_655 . ? N2 Tb1 O2 165.12(19) 3_665 . ? N2 Tb1 O2 69.56(19) . . ? O2 Tb1 O2 116.47(8) 2_655 . ? O1 Tb1 O2 118.89(18) 2_655 3_665 ? O1 Tb1 O2 73.63(16) . 3_665 ? O1 Tb1 O2 51.23(17) 3_665 3_665 ? N2 Tb1 O2 165.12(19) 2_655 3_665 ? N2 Tb1 O2 69.56(19) 3_665 3_665 ? N2 Tb1 O2 68.38(19) . 3_665 ? O2 Tb1 O2 116.47(8) 2_655 3_665 ? O2 Tb1 O2 116.47(8) . 3_665 ? O1 Tb1 N1 138.10(13) 2_655 . ? O1 Tb1 N1 138.10(13) . . ? O1 Tb1 N1 138.10(13) 3_665 . ? N2 Tb1 N1 64.17(15) 2_655 . ? N2 Tb1 N1 64.17(15) 3_665 . ? N2 Tb1 N1 64.17(15) . . ? O2 Tb1 N1 100.97(12) 2_655 . ? O2 Tb1 N1 100.97(12) . . ? O2 Tb1 N1 100.97(12) 3_665 . ? O1 Tb1 N5 25.47(18) 2_655 2_655 ? O1 Tb1 N5 94.66(18) . 2_655 ? O1 Tb1 N5 69.99(16) 3_665 2_655 ? N2 Tb1 N5 70.88(19) 2_655 2_655 ? N2 Tb1 N5 92.54(18) 3_665 2_655 ? N2 Tb1 N5 164.72(18) . 2_655 ? O2 Tb1 N5 25.76(18) 2_655 2_655 ? O2 Tb1 N5 95.16(17) . 2_655 ? O2 Tb1 N5 120.87(17) 3_665 2_655 ? N1 Tb1 N5 121.42(14) . 2_655 ? O1 Tb1 N5 69.99(16) 2_655 . ? O1 Tb1 N5 25.47(18) . . ? O1 Tb1 N5 94.66(18) 3_665 . ? N2 Tb1 N5 92.54(18) 2_655 . ? N2 Tb1 N5 164.72(18) 3_665 . ? N2 Tb1 N5 70.88(19) . . ? O2 Tb1 N5 120.87(17) 2_655 . ? O2 Tb1 N5 25.76(18) . . ? O2 Tb1 N5 95.16(17) 3_665 . ? N1 Tb1 N5 121.42(14) . . ? N5 Tb1 N5 95.31(19) 2_655 . ? C1 N1 C1 109.8(5) 2_655 . ? C1 N1 C1 109.8(5) 2_655 3_665 ? C1 N1 C1 109.8(5) . 3_665 ? C1 N1 Tb1 109.1(5) 2_655 . ? C1 N1 Tb1 109.1(5) . . ? C1 N1 Tb1 109.1(5) 3_665 . ? C2 N2 C3 105.3(6) . . ? C2 N2 Tb1 119.2(4) . . ? C3 N2 Tb1 135.1(5) . . ? C2 N3 C8 107.5(6) . . ? C2 N3 C9 127.0(6) . . ? C8 N3 C9 125.2(6) . . ? N1 C1 C2 111.2(6) . . ? N1 C1 H1A 109.4 . . ? C2 C1 H1A 109.4 . . ? N1 C1 H1B 109.4 . . ? C2 C1 H1B 109.4 . . ? H1A C1 H1B 108.0 . . ? N2 C2 N3 111.5(6) . . ? N2 C2 C1 121.9(6) . . ? N3 C2 C1 126.6(7) . . ? C4 C3 C8 119.1(7) . . ? C4 C3 N2 131.3(7) . . ? C8 C3 N2 109.6(7) . . ? C5 C4 C3 120.2(8) . . ? C5 C4 H4A 119.9 . . ? C3 C4 H4A 119.9 . . ? C4 C5 C6 119.4(9) . . ? C4 C5 H5A 120.3 . . ? C6 C5 H5A 120.3 . . ? C7 C6 C5 123.4(8) . . ? C7 C6 H6A 118.3 . . ? C5 C6 H6A 118.3 . . ? C6 C7 C8 115.3(8) . . ? C6 C7 H7A 122.4 . . ? C8 C7 H7A 122.4 . . ? C3 C8 N3 106.0(6) . . ? C3 C8 C7 122.5(8) . . ? N3 C8 C7 131.5(8) . . ? N3 C9 C10 110.2(8) . . ? N3 C9 H9A 109.6 . . ? C10 C9 H9A 109.6 . . ? N3 C9 H9B 109.6 . . ? C10 C9 H9B 109.6 . . ? H9A C9 H9B 108.1 . . ? C14 C10 C11 122.2(12) . . ? C14 C10 C9 121.4(9) . . ? C11 C10 C9 116.2(11) . . ? C10 C11 N4 125.9(18) . . ? C10 C11 H11A 117.0 . . ? N4 C11 H11A 117.0 . . ? C12 N4 C11 111.4(16) . . ? C13 C12 N4 125.7(14) . . ? C13 C12 H12A 117.1 . . ? N4 C12 H12A 117.2 . . ? C12 C13 C14 117.0(18) . . ? C12 C13 H13A 121.5 . . ? C14 C13 H13A 121.5 . . ? C10 C14 C13 117.5(14) . . ? C10 C14 H14A 121.3 . . ? C13 C14 H14A 121.3 . . ? O1 N5 O3 122.9(7) . . ? O1 N5 O2 117.1(6) . . ? O3 N5 O2 120.0(7) . . ? O1 N5 Tb1 57.0(3) . . ? O3 N5 Tb1 177.9(5) . . ? O2 N5 Tb1 60.1(3) . . ? N5 O1 Tb1 97.5(4) . . ? N5 O2 Tb1 94.2(4) . . ? O8 Tb2 O7 128.4(4) 4_554 . ? O8 Tb2 O7 128.4(4) 4_554 3 ? O7 Tb2 O7 85.5(6) . 3 ? O8 Tb2 O7 128.4(4) 4_554 2 ? O7 Tb2 O7 85.5(6) . 2 ? O7 Tb2 O7 85.5(6) 3 2 ? O8 Tb2 O5 47.9(4) 4_554 3 ? O7 Tb2 O5 143.0(5) . 3 ? O7 Tb2 O5 127.2(5) 3 3 ? O7 Tb2 O5 81.1(5) 2 3 ? O8 Tb2 O5 47.9(4) 4_554 2 ? O7 Tb2 O5 81.1(5) . 2 ? O7 Tb2 O5 143.0(5) 3 2 ? O7 Tb2 O5 127.2(5) 2 2 ? O5 Tb2 O5 80.0(6) 3 2 ? O8 Tb2 O5 47.9(4) 4_554 . ? O7 Tb2 O5 127.2(5) . . ? O7 Tb2 O5 81.1(5) 3 . ? O7 Tb2 O5 143.0(5) 2 . ? O5 Tb2 O5 80.0(6) 3 . ? O5 Tb2 O5 80.0(6) 2 . ? O8 Tb2 O4 77.7(3) 4_554 2 ? O7 Tb2 O4 76.7(5) . 2 ? O7 Tb2 O4 153.8(5) 3 2 ? O7 Tb2 O4 74.2(5) 2 2 ? O5 Tb2 O4 66.5(5) 3 2 ? O5 Tb2 O4 53.1(5) 2 2 ? O5 Tb2 O4 125.0(5) . 2 ? O8 Tb2 O4 77.7(3) 4_554 . ? O7 Tb2 O4 74.2(5) . . ? O7 Tb2 O4 76.7(5) 3 . ? O7 Tb2 O4 153.8(5) 2 . ? O5 Tb2 O4 125.0(5) 3 . ? O5 Tb2 O4 66.5(5) 2 . ? O5 Tb2 O4 53.1(5) . . ? O4 Tb2 O4 115.6(2) 2 . ? O8 Tb2 O4 77.7(3) 4_554 3 ? O7 Tb2 O4 153.8(5) . 3 ? O7 Tb2 O4 74.2(5) 3 3 ? O7 Tb2 O4 76.7(5) 2 3 ? O5 Tb2 O4 53.1(5) 3 3 ? O5 Tb2 O4 125.0(5) 2 3 ? O5 Tb2 O4 66.5(5) . 3 ? O4 Tb2 O4 115.6(2) 2 3 ? O4 Tb2 O4 115.6(2) . 3 ? O8 Tb2 O8 180.000(9) 4_554 . ? O7 Tb2 O8 51.6(4) . . ? O7 Tb2 O8 51.6(4) 3 . ? O7 Tb2 O8 51.6(4) 2 . ? O5 Tb2 O8 132.1(4) 3 . ? O5 Tb2 O8 132.1(4) 2 . ? O5 Tb2 O8 132.1(4) . . ? O4 Tb2 O8 102.3(3) 2 . ? O4 Tb2 O8 102.3(3) . . ? O4 Tb2 O8 102.3(3) 3 . ? O6 N6 O5 116.1(19) . . ? O6 N6 O4 126.4(16) . . ? O5 N6 O4 117.5(15) . . ? N6 O4 Tb2 94.9(9) . . ? N6 O5 O7 132.6(18) . 4_554 ? N6 O5 Tb2 94.4(11) . . ? O7 O5 Tb2 120.6(10) 4_554 . ? O5 O7 Tb2 113.3(10) 4 . ? N7 C15 C16 178.8(13) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.4 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Tb2 O8 Tb2 180.000(2) 4 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Tb1 N1 C1 12.9(3) 2_655 . . 2_655 ? O1 Tb1 N1 C1 132.9(3) . . . 2_655 ? O1 Tb1 N1 C1 -107.1(3) 3_665 . . 2_655 ? N2 Tb1 N1 C1 31.3(3) 2_655 . . 2_655 ? N2 Tb1 N1 C1 -88.7(3) 3_665 . . 2_655 ? N2 Tb1 N1 C1 151.3(3) . . . 2_655 ? O2 Tb1 N1 C1 -29.4(3) 2_655 . . 2_655 ? O2 Tb1 N1 C1 90.6(3) . . . 2_655 ? O2 Tb1 N1 C1 -149.4(3) 3_665 . . 2_655 ? N5 Tb1 N1 C1 -12.5(3) 2_655 . . 2_655 ? N5 Tb1 N1 C1 107.5(3) . . . 2_655 ? O1 Tb1 N1 C1 -107.1(3) 2_655 . . . ? O1 Tb1 N1 C1 12.9(3) . . . . ? O1 Tb1 N1 C1 132.9(3) 3_665 . . . ? N2 Tb1 N1 C1 -88.7(3) 2_655 . . . ? N2 Tb1 N1 C1 151.3(3) 3_665 . . . ? N2 Tb1 N1 C1 31.3(3) . . . . ? O2 Tb1 N1 C1 -149.4(3) 2_655 . . . ? O2 Tb1 N1 C1 -29.4(3) . . . . ? O2 Tb1 N1 C1 90.6(3) 3_665 . . . ? N5 Tb1 N1 C1 -132.5(3) 2_655 . . . ? N5 Tb1 N1 C1 -12.5(3) . . . . ? O1 Tb1 N1 C1 132.9(3) 2_655 . . 3_665 ? O1 Tb1 N1 C1 -107.1(3) . . . 3_665 ? O1 Tb1 N1 C1 12.9(3) 3_665 . . 3_665 ? N2 Tb1 N1 C1 151.3(3) 2_655 . . 3_665 ? N2 Tb1 N1 C1 31.3(3) 3_665 . . 3_665 ? N2 Tb1 N1 C1 -88.7(3) . . . 3_665 ? O2 Tb1 N1 C1 90.6(3) 2_655 . . 3_665 ? O2 Tb1 N1 C1 -149.4(3) . . . 3_665 ? O2 Tb1 N1 C1 -29.4(3) 3_665 . . 3_665 ? N5 Tb1 N1 C1 107.5(3) 2_655 . . 3_665 ? N5 Tb1 N1 C1 -132.5(3) . . . 3_665 ? O1 Tb1 N2 C2 115.0(5) 2_655 . . . ? O1 Tb1 N2 C2 146.9(5) . . . . ? O1 Tb1 N2 C2 -153.6(5) 3_665 . . . ? N2 Tb1 N2 C2 32.4(5) 2_655 . . . ? N2 Tb1 N2 C2 -73.5(4) 3_665 . . . ? O2 Tb1 N2 C2 -23.3(11) 2_655 . . . ? O2 Tb1 N2 C2 93.4(5) . . . . ? O2 Tb1 N2 C2 -135.3(6) 3_665 . . . ? N1 Tb1 N2 C2 -20.5(5) . . . . ? N5 Tb1 N2 C2 94.6(9) 2_655 . . . ? N5 Tb1 N2 C2 120.8(5) . . . . ? O1 Tb1 N2 C3 -57.3(7) 2_655 . . . ? O1 Tb1 N2 C3 -25.4(6) . . . . ? O1 Tb1 N2 C3 34.1(7) 3_665 . . . ? N2 Tb1 N2 C3 -139.9(6) 2_655 . . . ? N2 Tb1 N2 C3 114.2(7) 3_665 . . . ? O2 Tb1 N2 C3 164.4(6) 2_655 . . . ? O2 Tb1 N2 C3 -78.9(6) . . . . ? O2 Tb1 N2 C3 52.4(6) 3_665 . . . ? N1 Tb1 N2 C3 167.2(7) . . . . ? N5 Tb1 N2 C3 -77.6(10) 2_655 . . . ? N5 Tb1 N2 C3 -51.5(6) . . . . ? C1 N1 C1 C2 -159.2(7) 2_655 . . . ? C1 N1 C1 C2 80.0(10) 3_665 . . . ? Tb1 N1 C1 C2 -39.6(6) . . . . ? C3 N2 C2 N3 2.5(8) . . . . ? Tb1 N2 C2 N3 -171.9(4) . . . . ? C3 N2 C2 C1 -178.5(6) . . . . ? Tb1 N2 C2 C1 7.1(9) . . . . ? C8 N3 C2 N2 -2.0(8) . . . . ? C9 N3 C2 N2 -176.5(7) . . . . ? C8 N3 C2 C1 179.0(7) . . . . ? C9 N3 C2 C1 4.6(12) . . . . ? N1 C1 C2 N2 24.6(10) . . . . ? N1 C1 C2 N3 -156.5(7) . . . . ? C2 N2 C3 C4 178.9(7) . . . . ? Tb1 N2 C3 C4 -8.1(11) . . . . ? C2 N2 C3 C8 -2.0(8) . . . . ? Tb1 N2 C3 C8 171.0(5) . . . . ? C8 C3 C4 C5 1.1(11) . . . . ? N2 C3 C4 C5 -180.0(7) . . . . ? C3 C4 C5 C6 -1.9(12) . . . . ? C4 C5 C6 C7 1.6(14) . . . . ? C5 C6 C7 C8 -0.4(13) . . . . ? C4 C3 C8 N3 180.0(6) . . . . ? N2 C3 C8 N3 0.8(7) . . . . ? C4 C3 C8 C7 0.2(10) . . . . ? N2 C3 C8 C7 -179.0(6) . . . . ? C2 N3 C8 C3 0.7(7) . . . . ? C9 N3 C8 C3 175.2(7) . . . . ? C2 N3 C8 C7 -179.5(7) . . . . ? C9 N3 C8 C7 -5.0(12) . . . . ? C6 C7 C8 C3 -0.5(11) . . . . ? C6 C7 C8 N3 179.8(8) . . . . ? C2 N3 C9 C10 -111.0(8) . . . . ? C8 N3 C9 C10 75.6(10) . . . . ? N3 C9 C10 C14 56.1(14) . . . . ? N3 C9 C10 C11 -128.3(11) . . . . ? C14 C10 C11 N4 -6(3) . . . . ? C9 C10 C11 N4 178.8(15) . . . . ? C10 C11 N4 C12 6(3) . . . . ? C11 N4 C12 C13 -5(3) . . . . ? N4 C12 C13 C14 3(4) . . . . ? C11 C10 C14 C13 4(3) . . . . ? C9 C10 C14 C13 179.0(17) . . . . ? C12 C13 C14 C10 -3(3) . . . . ? O1 Tb1 N5 O1 -86.9(5) 2_655 . . . ? O1 Tb1 N5 O1 -19.4(4) 3_665 . . . ? N2 Tb1 N5 O1 -160.7(4) 2_655 . . . ? N2 Tb1 N5 O1 30.9(10) 3_665 . . . ? N2 Tb1 N5 O1 97.0(4) . . . . ? O2 Tb1 N5 O1 -93.1(4) 2_655 . . . ? O2 Tb1 N5 O1 179.4(7) . . . . ? O2 Tb1 N5 O1 32.0(4) 3_665 . . . ? N1 Tb1 N5 O1 138.2(4) . . . . ? N5 Tb1 N5 O1 -89.7(3) 2_655 . . . ? O1 Tb1 N5 O3 2(16) 2_655 . . . ? O1 Tb1 N5 O3 89(16) . . . . ? O1 Tb1 N5 O3 69(16) 3_665 . . . ? N2 Tb1 N5 O3 -72(16) 2_655 . . . ? N2 Tb1 N5 O3 120(16) 3_665 . . . ? N2 Tb1 N5 O3 -174(100) . . . . ? O2 Tb1 N5 O3 -4(16) 2_655 . . . ? O2 Tb1 N5 O3 -92(16) . . . . ? O2 Tb1 N5 O3 121(16) 3_665 . . . ? N1 Tb1 N5 O3 -133(16) . . . . ? N5 Tb1 N5 O3 -1(16) 2_655 . . . ? O1 Tb1 N5 O2 93.7(4) 2_655 . . . ? O1 Tb1 N5 O2 -179.4(7) . . . . ? O1 Tb1 N5 O2 161.2(4) 3_665 . . . ? N2 Tb1 N5 O2 19.9(4) 2_655 . . . ? N2 Tb1 N5 O2 -148.5(7) 3_665 . . . ? N2 Tb1 N5 O2 -82.4(4) . . . . ? O2 Tb1 N5 O2 87.5(3) 2_655 . . . ? O2 Tb1 N5 O2 -147.4(4) 3_665 . . . ? N1 Tb1 N5 O2 -41.2(4) . . . . ? N5 Tb1 N5 O2 90.9(5) 2_655 . . . ? O3 N5 O1 Tb1 -177.5(6) . . . . ? O2 N5 O1 Tb1 0.6(6) . . . . ? O1 Tb1 O1 N5 83.9(5) 2_655 . . . ? O1 Tb1 O1 N5 159.5(4) 3_665 . . . ? N2 Tb1 O1 N5 21.6(5) 2_655 . . . ? N2 Tb1 O1 N5 -167.7(4) 3_665 . . . ? N2 Tb1 O1 N5 -75.4(4) . . . . ? O2 Tb1 O1 N5 101.8(4) 2_655 . . . ? O2 Tb1 O1 N5 -0.3(4) . . . . ? O2 Tb1 O1 N5 -146.6(4) 3_665 . . . ? N1 Tb1 O1 N5 -58.3(4) . . . . ? N5 Tb1 O1 N5 92.6(3) 2_655 . . . ? O1 N5 O2 Tb1 -0.6(6) . . . . ? O3 N5 O2 Tb1 177.6(6) . . . . ? O1 Tb1 O2 N5 -77.8(4) 2_655 . . . ? O1 Tb1 O2 N5 0.3(4) . . . . ? O1 Tb1 O2 N5 -21.5(4) 3_665 . . . ? N2 Tb1 O2 N5 -158.6(4) 2_655 . . . ? N2 Tb1 O2 N5 147.6(7) 3_665 . . . ? N2 Tb1 O2 N5 88.2(4) . . . . ? O2 Tb1 O2 N5 -106.7(3) 2_655 . . . ? O2 Tb1 O2 N5 36.8(5) 3_665 . . . ? N1 Tb1 O2 N5 145.1(4) . . . . ? N5 Tb1 O2 N5 -91.5(5) 2_655 . . . ? O6 N6 O4 Tb2 178(2) . . . . ? O5 N6 O4 Tb2 -4(2) . . . . ? O8 Tb2 O4 N6 -43.7(12) 4_554 . . . ? O7 Tb2 O4 N6 -179.9(14) . . . . ? O7 Tb2 O4 N6 91.1(14) 3 . . . ? O7 Tb2 O4 N6 139.6(13) 2 . . . ? O5 Tb2 O4 N6 -35.3(14) 3 . . . ? O5 Tb2 O4 N6 -92.9(13) 2 . . . ? O5 Tb2 O4 N6 2.3(13) . . . . ? O4 Tb2 O4 N6 -113.5(11) 2 . . . ? O4 Tb2 O4 N6 26.1(15) 3 . . . ? O8 Tb2 O4 N6 136.3(12) . . . . ? O6 N6 O5 O7 -38(3) . . . 4_554 ? O4 N6 O5 O7 143.6(19) . . . 4_554 ? O6 N6 O5 Tb2 -178.0(18) . . . . ? O4 N6 O5 Tb2 4(2) . . . . ? O8 Tb2 O5 N6 106.8(13) 4_554 . . . ? O7 Tb2 O5 N6 -4.7(16) . . . . ? O7 Tb2 O5 N6 -82.0(13) 3 . . . ? O7 Tb2 O5 N6 -152.2(11) 2 . . . ? O5 Tb2 O5 N6 147.5(12) 3 . . . ? O5 Tb2 O5 N6 66.0(14) 2 . . . ? O4 Tb2 O5 N6 95.7(13) 2 . . . ? O4 Tb2 O5 N6 -2.0(11) . . . . ? O4 Tb2 O5 N6 -158.6(14) 3 . . . ? O8 Tb2 O5 N6 -73.2(13) . . . . ? O8 Tb2 O5 O7 -39.7(11) 4_554 . . 4_554 ? O7 Tb2 O5 O7 -151.2(12) . . . 4_554 ? O7 Tb2 O5 O7 131.5(13) 3 . . 4_554 ? O7 Tb2 O5 O7 61.3(16) 2 . . 4_554 ? O5 Tb2 O5 O7 1.0(13) 3 . . 4_554 ? O5 Tb2 O5 O7 -80.5(10) 2 . . 4_554 ? O4 Tb2 O5 O7 -50.8(15) 2 . . 4_554 ? O4 Tb2 O5 O7 -148.5(16) . . . 4_554 ? O4 Tb2 O5 O7 54.9(12) 3 . . 4_554 ? O8 Tb2 O5 O7 140.3(11) . . . 4_554 ? O8 Tb2 O7 O5 -144.5(10) 4_554 . . 4 ? O7 Tb2 O7 O5 -7.4(11) 3 . . 4 ? O7 Tb2 O7 O5 78.4(9) 2 . . 4 ? O5 Tb2 O7 O5 147.1(11) 3 . . 4 ? O5 Tb2 O7 O5 -152.9(10) 2 . . 4 ? O5 Tb2 O7 O5 -82.7(12) . . . 4 ? O4 Tb2 O7 O5 153.2(12) 2 . . 4 ? O4 Tb2 O7 O5 -84.9(11) . . . 4 ? O4 Tb2 O7 O5 31.3(17) 3 . . 4 ? O8 Tb2 O7 O5 35.5(10) . . . 4 ? O8 Tb2 O8 Tb2 0(100) 4_554 . . 4 ? O7 Tb2 O8 Tb2 0(100) . . . 4 ? O7 Tb2 O8 Tb2 0(100) 3 . . 4 ? O7 Tb2 O8 Tb2 0(100) 2 . . 4 ? O5 Tb2 O8 Tb2 0(100) 3 . . 4 ? O5 Tb2 O8 Tb2 0(100) 2 . . 4 ? O5 Tb2 O8 Tb2 0(100) . . . 4 ? O4 Tb2 O8 Tb2 0(100) 2 . . 4 ? O4 Tb2 O8 Tb2 0(100) . . . 4 ? O4 Tb2 O8 Tb2 0(100) 3 . . 4 ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 62.61 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.603 _refine_diff_density_min -1.000 _refine_diff_density_rms 0.096 #===============================# data_5 _database_code_depnum_ccdc_archive 'CCDC 856046' #TrackingRef 'Compounds.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H52 Eu2 N19 O21.50' _chemical_formula_weight 1543.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -8.9294 11.1857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 17.3716(6) _cell_length_b 17.3716(6) _cell_length_c 39.5287(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 10330.5(7) _cell_formula_units_Z 6 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6957 _cell_measurement_theta_min 3.1308 _cell_measurement_theta_max 62.3954 _exptl_crystal_description block _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.488 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4626 _exptl_absorpt_coefficient_mu 13.601 _exptl_absorpt_correction_T_min 0.0739 _exptl_absorpt_correction_T_max 0.1057 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9993 _diffrn_reflns_av_R_equivalents 0.0783 _diffrn_reflns_av_sigmaI/netI 0.0584 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_theta_min 5.09 _diffrn_reflns_theta_max 62.56 _reflns_number_total 3499 _reflns_number_gt 2929 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1100P)^2^+240.0000P] 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 3499 _refine_ls_number_parameters 269 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0948 _refine_ls_R_factor_gt 0.0838 _refine_ls_wR_factor_ref 0.2139 _refine_ls_wR_factor_gt 0.2070 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Eu1 Eu 1.0000 1.0000 0.125791(19) 0.0237(3) Uani 1 3 d S . . Eu2 Eu 1.3333 0.6667 0.00089(3) 0.0543(4) Uani 1 3 d S . . N1 N 1.0000 1.0000 0.1958(3) 0.024(3) Uani 1 3 d S . . N2 N 1.1466(5) 1.0341(5) 0.15559(17) 0.0264(16) Uani 1 1 d . . . N3 N 1.2340(5) 1.0629(5) 0.20037(18) 0.0302(17) Uani 1 1 d . . . N4 N 1.2334(9) 0.8350(10) 0.2808(4) 0.094(5) Uani 1 1 d . . . N5 N 0.8593(7) 1.0047(6) 0.0864(2) 0.043(2) Uani 1 1 d . . . N6 N 1.1845(9) 0.6463(9) -0.0381(3) 0.071(3) Uani 1 1 d . . . C1 C 1.0888(6) 1.0621(7) 0.2084(2) 0.032(2) Uani 1 1 d . . . H1A H 1.0932 1.0502 0.2326 0.039 Uiso 1 1 calc R . . H1B H 1.1004 1.1238 0.2062 0.039 Uiso 1 1 calc R . . C2 C 1.1566(6) 1.0513(6) 0.1882(2) 0.0268(19) Uani 1 1 d . . . C3 C 1.2253(6) 1.0373(6) 0.1454(2) 0.031(2) Uani 1 1 d . . . C4 C 1.2513(7) 1.0208(7) 0.1138(3) 0.043(2) Uani 1 1 d . . . H4A H 1.2137 1.0056 0.0946 0.052 Uiso 1 1 calc R . . C5 C 1.3336(7) 1.0276(8) 0.1120(3) 0.053(3) Uani 1 1 d . . . H5A H 1.3540 1.0199 0.0907 0.064 Uiso 1 1 calc R . . C6 C 1.3890(7) 1.0458(7) 0.1406(3) 0.050(3) Uani 1 1 d . . . H6A H 1.4444 1.0477 0.1384 0.060 Uiso 1 1 calc R . . C7 C 1.3632(7) 1.0607(7) 0.1716(3) 0.045(3) Uani 1 1 d . . . H7A H 1.4003 1.0743 0.1909 0.053 Uiso 1 1 calc R . . C8 C 1.2803(6) 1.0549(6) 0.1735(2) 0.033(2) Uani 1 1 d . . . C9 C 1.2628(7) 1.0722(7) 0.2359(2) 0.043(3) Uani 1 1 d . . . H9A H 1.2296 1.0940 0.2494 0.052 Uiso 1 1 calc R . . H9B H 1.3267 1.1173 0.2373 0.052 Uiso 1 1 calc R . . C10 C 1.2486(7) 0.9864(8) 0.2512(3) 0.048(3) Uani 1 1 d . . . C11 C 1.2269(9) 0.9103(8) 0.2330(3) 0.061(3) Uani 1 1 d . . . H11A H 1.2180 0.9094 0.2093 0.073 Uiso 1 1 calc R . . C12 C 1.2180(10) 0.8359(10) 0.2488(4) 0.083(5) Uani 1 1 d . . . H12A H 1.2000 0.7835 0.2359 0.099 Uiso 1 1 calc R . . C13 C 1.2545(11) 0.9085(11) 0.3002(4) 0.086(5) Uani 1 1 d . . . H13A H 1.2639 0.9074 0.3238 0.103 Uiso 1 1 calc R . . C14 C 1.2620(9) 0.9834(10) 0.2857(3) 0.069(4) Uani 1 1 d . . . H14A H 1.2765 1.0339 0.2993 0.082 Uiso 1 1 calc R . . O1 O 0.9409(5) 1.0511(5) 0.07881(16) 0.0439(17) Uani 1 1 d . . . O2 O 0.8418(4) 0.9569(4) 0.11278(16) 0.0349(15) Uani 1 1 d . . . O3 O 0.8027(6) 1.0079(6) 0.0701(2) 0.065(2) Uani 1 1 d . . . O4 O 1.2054(6) 0.6904(6) -0.0128(3) 0.072(3) Uani 1 1 d . . . O5 O 1.2240(6) 0.6033(7) -0.0463(2) 0.074(3) Uani 1 1 d . . . O6 O 1.1224(8) 0.6384(9) -0.0564(3) 0.109(4) Uani 1 1 d . . . O7 O 1.3488(8) 0.7889(10) 0.0325(4) 0.141(6) Uani 1 1 d . . . N7 N 1.320(2) 1.086(2) 0.3649(8) 0.104(9) Uiso 0.50 1 d P . . C15 C 1.391(3) 1.088(3) 0.3580(10) 0.100(11) Uiso 0.50 1 d P . . C16 C 1.460(2) 1.063(2) 0.3493(9) 0.090(9) Uiso 0.50 1 d P . . H16A H 1.5176 1.1166 0.3456 0.135 Uiso 0.50 1 calc PR . . H16B H 1.4423 1.0266 0.3286 0.135 Uiso 0.50 1 calc PR . . H16C H 1.4653 1.0283 0.3679 0.135 Uiso 0.50 1 calc PR . . N8 N 1.236(2) 0.802(2) 0.1628(9) 0.114(10) Uiso 0.50 1 d P . . C17 C 1.210(2) 0.794(2) 0.1382(8) 0.073(8) Uiso 0.50 1 d P . . C18 C 1.1944(19) 0.7860(18) 0.1016(6) 0.079(8) Uiso 0.50 1 d P . . H18A H 1.1418 0.7908 0.0964 0.119 Uiso 0.50 1 calc PR . . H18B H 1.1848 0.7281 0.0941 0.119 Uiso 0.50 1 calc PR . . H18C H 1.2463 0.8335 0.0900 0.119 Uiso 0.50 1 calc PR . . O8 O 1.3300(19) 0.6964(18) 0.1137(6) 0.076(17) Uiso 0.17 1 d PR . . 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 0.0302(4) 0.0302(4) 0.0106(4) 0.000 0.000 0.01509(19) Eu2 0.0625(6) 0.0625(6) 0.0378(7) 0.000 0.000 0.0312(3) N1 0.028(4) 0.028(4) 0.015(6) 0.000 0.000 0.014(2) N2 0.023(4) 0.036(4) 0.019(3) 0.000(3) -0.004(3) 0.014(3) N3 0.035(4) 0.025(4) 0.031(4) -0.001(3) -0.010(3) 0.016(3) N4 0.071(8) 0.086(9) 0.108(11) 0.048(9) -0.019(8) 0.027(7) N5 0.066(6) 0.052(5) 0.026(4) -0.019(4) -0.023(4) 0.040(5) N6 0.103(10) 0.085(8) 0.046(6) 0.007(6) 0.007(6) 0.063(8) C1 0.035(5) 0.048(6) 0.014(4) -0.014(4) -0.006(4) 0.021(5) C2 0.034(5) 0.032(5) 0.015(4) -0.004(3) -0.011(4) 0.017(4) C3 0.034(5) 0.022(4) 0.029(5) -0.002(4) 0.000(4) 0.009(4) C4 0.048(6) 0.049(6) 0.040(6) -0.001(5) 0.003(5) 0.029(5) C5 0.043(6) 0.056(7) 0.061(7) 0.007(6) 0.025(6) 0.025(6) C6 0.031(6) 0.040(6) 0.077(8) 0.006(6) 0.007(6) 0.016(5) C7 0.037(6) 0.043(6) 0.056(7) 0.004(5) -0.003(5) 0.021(5) C8 0.033(5) 0.031(5) 0.040(5) 0.005(4) 0.000(4) 0.019(4) C9 0.044(6) 0.052(6) 0.037(5) -0.006(5) -0.020(5) 0.027(5) C10 0.038(6) 0.058(7) 0.037(6) 0.009(5) -0.016(5) 0.015(5) C11 0.071(8) 0.042(7) 0.062(8) 0.000(6) -0.018(7) 0.022(6) C12 0.088(11) 0.063(9) 0.092(11) 0.017(8) -0.028(9) 0.034(8) C13 0.092(11) 0.076(10) 0.069(9) 0.029(9) -0.024(9) 0.027(9) C14 0.060(8) 0.081(9) 0.058(8) 0.016(7) -0.006(6) 0.030(7) O1 0.060(5) 0.053(4) 0.027(3) 0.002(3) -0.008(3) 0.034(4) O2 0.034(4) 0.040(4) 0.033(3) -0.010(3) -0.008(3) 0.020(3) O3 0.081(6) 0.095(7) 0.051(5) -0.015(4) -0.035(4) 0.068(6) O4 0.066(6) 0.073(6) 0.074(6) -0.007(5) 0.002(5) 0.033(5) O5 0.082(6) 0.090(7) 0.049(5) -0.004(5) -0.009(5) 0.042(6) O6 0.100(9) 0.153(12) 0.100(9) 0.011(8) -0.025(7) 0.082(9) O7 0.076(8) 0.151(12) 0.167(13) -0.116(11) -0.015(8) 0.036(8) _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 2.490(6) 2_765 ? Eu1 O1 2.490(6) . ? Eu1 O1 2.490(6) 3_675 ? Eu1 O2 2.514(6) 3_675 ? Eu1 O2 2.514(6) . ? Eu1 O2 2.514(6) 2_765 ? Eu1 N2 2.591(7) . ? Eu1 N2 2.591(7) 2_765 ? Eu1 N2 2.591(7) 3_675 ? Eu1 N1 2.769(11) . ? Eu1 N5 2.934(8) . ? Eu1 N5 2.934(8) 2_765 ? Eu2 O7 2.360(11) . ? Eu2 O7 2.360(11) 2_755 ? Eu2 O7 2.360(11) 3_775 ? Eu2 O5 2.492(9) . ? Eu2 O5 2.492(9) 3_775 ? Eu2 O5 2.492(9) 2_755 ? Eu2 O4 2.514(9) . ? Eu2 O4 2.514(10) 3_775 ? Eu2 O4 2.514(9) 2_755 ? Eu2 N6 2.875(13) . ? Eu2 N6 2.875(13) 3_775 ? Eu2 N6 2.875(13) 2_755 ? N1 C1 1.457(9) . ? N1 C1 1.457(9) 2_765 ? N1 C1 1.457(9) 3_675 ? N2 C2 1.316(10) . ? N2 C3 1.399(12) . ? N3 C2 1.345(11) . ? N3 C8 1.380(12) . ? N3 C9 1.473(11) . ? N4 C12 1.295(19) . ? N4 C13 1.37(2) . ? N5 O3 1.199(11) . ? N5 O1 1.267(12) . ? N5 O2 1.273(11) . ? N6 O4 1.198(14) . ? N6 O6 1.248(15) . ? N6 O5 1.285(14) . ? C1 C2 1.510(12) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C3 C8 1.396(13) . ? C3 C4 1.407(13) . ? C4 C5 1.375(15) . ? C4 H4A 0.9500 . ? C5 C6 1.416(17) . ? C5 H5A 0.9500 . ? C6 C7 1.371(16) . ? C6 H6A 0.9500 . ? C7 C8 1.395(14) . ? C7 H7A 0.9500 . ? C9 C10 1.509(15) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.381(17) . ? C10 C14 1.389(16) . ? C11 C12 1.372(18) . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? C13 C14 1.366(19) . ? C13 H13A 0.9500 . ? C14 H14A 0.9500 . ? N7 C15 1.25(4) . ? C15 C16 1.51(5) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? N8 C17 1.06(4) . ? C17 C18 1.46(4) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? O8 O8 0.95(4) 3_775 ? O8 O8 0.95(4) 2_755 ? 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 O1 70.5(3) 2_765 . ? O1 Eu1 O1 70.5(3) 2_765 3_675 ? O1 Eu1 O1 70.5(3) . 3_675 ? O1 Eu1 O2 118.1(2) 2_765 3_675 ? O1 Eu1 O2 72.7(2) . 3_675 ? O1 Eu1 O2 50.9(2) 3_675 3_675 ? O1 Eu1 O2 72.7(2) 2_765 . ? O1 Eu1 O2 50.9(2) . . ? O1 Eu1 O2 118.1(2) 3_675 . ? O2 Eu1 O2 115.93(10) 3_675 . ? O1 Eu1 O2 50.9(2) 2_765 2_765 ? O1 Eu1 O2 118.1(2) . 2_765 ? O1 Eu1 O2 72.7(2) 3_675 2_765 ? O2 Eu1 O2 115.93(10) 3_675 2_765 ? O2 Eu1 O2 115.93(10) . 2_765 ? O1 Eu1 N2 116.5(2) 2_765 . ? O1 Eu1 N2 142.2(2) . . ? O1 Eu1 N2 77.3(2) 3_675 . ? O2 Eu1 N2 71.9(2) 3_675 . ? O2 Eu1 N2 164.6(2) . . ? O2 Eu1 N2 68.0(2) 2_765 . ? O1 Eu1 N2 142.2(2) 2_765 2_765 ? O1 Eu1 N2 77.3(2) . 2_765 ? O1 Eu1 N2 116.5(2) 3_675 2_765 ? O2 Eu1 N2 68.0(2) 3_675 2_765 ? O2 Eu1 N2 71.9(2) . 2_765 ? O2 Eu1 N2 164.6(2) 2_765 2_765 ? N2 Eu1 N2 100.95(19) . 2_765 ? O1 Eu1 N2 77.3(2) 2_765 3_675 ? O1 Eu1 N2 116.5(2) . 3_675 ? O1 Eu1 N2 142.2(2) 3_675 3_675 ? O2 Eu1 N2 164.6(2) 3_675 3_675 ? O2 Eu1 N2 68.0(2) . 3_675 ? O2 Eu1 N2 71.9(2) 2_765 3_675 ? N2 Eu1 N2 100.95(19) . 3_675 ? N2 Eu1 N2 100.95(19) 2_765 3_675 ? O1 Eu1 N1 138.22(16) 2_765 . ? O1 Eu1 N1 138.22(16) . . ? O1 Eu1 N1 138.22(17) 3_675 . ? O2 Eu1 N1 101.80(14) 3_675 . ? O2 Eu1 N1 101.80(14) . . ? O2 Eu1 N1 101.80(14) 2_765 . ? N2 Eu1 N1 62.96(15) . . ? N2 Eu1 N1 62.96(15) 2_765 . ? N2 Eu1 N1 62.96(15) 3_675 . ? O1 Eu1 N5 69.1(2) 2_765 . ? O1 Eu1 N5 25.4(2) . . ? O1 Eu1 N5 94.1(2) 3_675 . ? O2 Eu1 N5 94.6(2) 3_675 . ? O2 Eu1 N5 25.6(2) . . ? O2 Eu1 N5 119.8(2) 2_765 . ? N2 Eu1 N5 166.4(3) . . ? N2 Eu1 N5 73.3(2) 2_765 . ? N2 Eu1 N5 92.3(3) 3_675 . ? N1 Eu1 N5 122.09(18) . . ? O1 Eu1 N5 25.4(2) 2_765 2_765 ? O1 Eu1 N5 94.1(2) . 2_765 ? O1 Eu1 N5 69.1(2) 3_675 2_765 ? O2 Eu1 N5 119.8(2) 3_675 2_765 ? O2 Eu1 N5 94.6(2) . 2_765 ? O2 Eu1 N5 25.6(2) 2_765 2_765 ? N2 Eu1 N5 92.3(3) . 2_765 ? N2 Eu1 N5 166.4(3) 2_765 2_765 ? N2 Eu1 N5 73.3(2) 3_675 2_765 ? N1 Eu1 N5 122.09(17) . 2_765 ? N5 Eu1 N5 94.4(2) . 2_765 ? O7 Eu2 O7 94.6(6) . 2_755 ? O7 Eu2 O7 94.6(6) . 3_775 ? O7 Eu2 O7 94.6(6) 2_755 3_775 ? O7 Eu2 O5 120.9(4) . . ? O7 Eu2 O5 82.0(5) 2_755 . ? O7 Eu2 O5 144.5(4) 3_775 . ? O7 Eu2 O5 82.0(5) . 3_775 ? O7 Eu2 O5 144.5(4) 2_755 3_775 ? O7 Eu2 O5 120.9(4) 3_775 3_775 ? O5 Eu2 O5 70.0(4) . 3_775 ? O7 Eu2 O5 144.5(4) . 2_755 ? O7 Eu2 O5 120.9(4) 2_755 2_755 ? O7 Eu2 O5 82.0(5) 3_775 2_755 ? O5 Eu2 O5 70.0(4) . 2_755 ? O5 Eu2 O5 70.0(4) 3_775 2_755 ? O7 Eu2 O4 71.3(4) . . ? O7 Eu2 O4 73.8(4) 2_755 . ? O7 Eu2 O4 160.5(5) 3_775 . ? O5 Eu2 O4 51.0(3) . . ? O5 Eu2 O4 71.7(3) 3_775 . ? O5 Eu2 O4 117.3(3) 2_755 . ? O7 Eu2 O4 73.8(4) . 3_775 ? O7 Eu2 O4 160.5(5) 2_755 3_775 ? O7 Eu2 O4 71.3(4) 3_775 3_775 ? O5 Eu2 O4 117.3(3) . 3_775 ? O5 Eu2 O4 51.0(3) 3_775 3_775 ? O5 Eu2 O4 71.7(3) 2_755 3_775 ? O4 Eu2 O4 115.48(16) . 3_775 ? O7 Eu2 O4 160.5(5) . 2_755 ? O7 Eu2 O4 71.3(4) 2_755 2_755 ? O7 Eu2 O4 73.8(4) 3_775 2_755 ? O5 Eu2 O4 71.7(3) . 2_755 ? O5 Eu2 O4 117.3(3) 3_775 2_755 ? O5 Eu2 O4 51.0(3) 2_755 2_755 ? O4 Eu2 O4 115.48(16) . 2_755 ? O4 Eu2 O4 115.48(16) 3_775 2_755 ? O7 Eu2 N6 94.9(4) . . ? O7 Eu2 N6 77.6(4) 2_755 . ? O7 Eu2 N6 168.2(4) 3_775 . ? O5 Eu2 N6 26.5(3) . . ? O5 Eu2 N6 67.5(3) 3_775 . ? O5 Eu2 N6 94.2(3) 2_755 . ? O4 Eu2 N6 24.5(3) . . ? O4 Eu2 N6 118.3(3) 3_775 . ? O4 Eu2 N6 95.1(3) 2_755 . ? O7 Eu2 N6 77.6(4) . 3_775 ? O7 Eu2 N6 168.2(4) 2_755 3_775 ? O7 Eu2 N6 94.9(4) 3_775 3_775 ? O5 Eu2 N6 94.2(3) . 3_775 ? O5 Eu2 N6 26.5(3) 3_775 3_775 ? O5 Eu2 N6 67.5(3) 2_755 3_775 ? O4 Eu2 N6 95.1(3) . 3_775 ? O4 Eu2 N6 24.5(3) 3_775 3_775 ? O4 Eu2 N6 118.3(3) 2_755 3_775 ? N6 Eu2 N6 94.0(3) . 3_775 ? O7 Eu2 N6 168.2(4) . 2_755 ? O7 Eu2 N6 94.9(4) 2_755 2_755 ? O7 Eu2 N6 77.6(4) 3_775 2_755 ? O5 Eu2 N6 67.5(3) . 2_755 ? O5 Eu2 N6 94.2(3) 3_775 2_755 ? O5 Eu2 N6 26.5(3) 2_755 2_755 ? O4 Eu2 N6 118.3(3) . 2_755 ? O4 Eu2 N6 95.1(3) 3_775 2_755 ? O4 Eu2 N6 24.5(3) 2_755 2_755 ? N6 Eu2 N6 94.0(3) . 2_755 ? N6 Eu2 N6 94.0(3) 3_775 2_755 ? C1 N1 C1 109.0(5) . 2_765 ? C1 N1 C1 109.0(5) . 3_675 ? C1 N1 C1 109.0(5) 2_765 3_675 ? C1 N1 Eu1 109.9(5) . . ? C1 N1 Eu1 109.9(5) 2_765 . ? C1 N1 Eu1 109.9(5) 3_675 . ? C2 N2 C3 104.8(7) . . ? C2 N2 Eu1 120.1(6) . . ? C3 N2 Eu1 135.0(5) . . ? C2 N3 C8 107.5(7) . . ? C2 N3 C9 128.1(8) . . ? C8 N3 C9 124.1(8) . . ? C12 N4 C13 119.5(13) . . ? O3 N5 O1 121.8(9) . . ? O3 N5 O2 122.4(10) . . ? O1 N5 O2 115.8(8) . . ? O3 N5 Eu1 179.0(9) . . ? O1 N5 Eu1 57.3(4) . . ? O2 N5 Eu1 58.5(4) . . ? O4 N6 O6 121.4(13) . . ? O4 N6 O5 120.3(12) . . ? O6 N6 O5 118.3(12) . . ? O4 N6 Eu2 60.6(7) . . ? O6 N6 Eu2 176.9(10) . . ? O5 N6 Eu2 59.9(6) . . ? N1 C1 C2 109.3(7) . . ? N1 C1 H1A 109.8 . . ? C2 C1 H1A 109.8 . . ? N1 C1 H1B 109.8 . . ? C2 C1 H1B 109.8 . . ? H1A C1 H1B 108.3 . . ? N2 C2 N3 113.2(8) . . ? N2 C2 C1 121.5(7) . . ? N3 C2 C1 125.2(7) . . ? C8 C3 N2 109.2(8) . . ? C8 C3 C4 119.8(9) . . ? N2 C3 C4 130.9(9) . . ? C5 C4 C3 117.1(10) . . ? C5 C4 H4A 121.4 . . ? C3 C4 H4A 121.4 . . ? C4 C5 C6 122.6(11) . . ? C4 C5 H5A 118.7 . . ? C6 C5 H5A 118.7 . . ? C7 C6 C5 120.4(10) . . ? C7 C6 H6A 119.8 . . ? C5 C6 H6A 119.8 . . ? C6 C7 C8 117.3(10) . . ? C6 C7 H7A 121.3 . . ? C8 C7 H7A 121.3 . . ? N3 C8 C7 132.0(9) . . ? N3 C8 C3 105.3(8) . . ? C7 C8 C3 122.7(9) . . ? N3 C9 C10 113.3(8) . . ? N3 C9 H9A 108.9 . . ? C10 C9 H9A 108.9 . . ? N3 C9 H9B 108.9 . . ? C10 C9 H9B 108.9 . . ? H9A C9 H9B 107.7 . . ? C11 C10 C14 116.4(12) . . ? C11 C10 C9 124.7(9) . . ? C14 C10 C9 118.8(11) . . ? C12 C11 C10 120.8(13) . . ? C12 C11 H11A 119.6 . . ? C10 C11 H11A 119.6 . . ? N4 C12 C11 122.1(16) . . ? N4 C12 H12A 119.0 . . ? C11 C12 H12A 119.0 . . ? C14 C13 N4 120.5(13) . . ? C14 C13 H13A 119.8 . . ? N4 C13 H13A 119.8 . . ? C13 C14 C10 120.6(15) . . ? C13 C14 H14A 119.7 . . ? C10 C14 H14A 119.7 . . ? N5 O1 Eu1 97.3(5) . . ? N5 O2 Eu1 96.0(6) . . ? N6 O4 Eu2 94.9(8) . . ? N6 O5 Eu2 93.6(8) . . ? N7 C15 C16 164(4) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N8 C17 C18 166(4) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O8 O8 O8 60.0 3_775 2_755 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Eu1 N1 C1 130.6(5) 2_765 . . . ? O1 Eu1 N1 C1 -109.4(5) . . . . ? O1 Eu1 N1 C1 10.6(5) 3_675 . . . ? O2 Eu1 N1 C1 -32.3(4) 3_675 . . . ? O2 Eu1 N1 C1 -152.3(4) . . . . ? O2 Eu1 N1 C1 87.7(4) 2_765 . . . ? N2 Eu1 N1 C1 30.1(5) . . . . ? N2 Eu1 N1 C1 -89.9(5) 2_765 . . . ? N2 Eu1 N1 C1 150.1(5) 3_675 . . . ? N5 Eu1 N1 C1 -135.4(5) . . . . ? N5 Eu1 N1 C1 104.6(5) 2_765 . . . ? O1 Eu1 N1 C1 -109.4(5) 2_765 . . 2_765 ? O1 Eu1 N1 C1 10.6(5) . . . 2_765 ? O1 Eu1 N1 C1 130.6(5) 3_675 . . 2_765 ? O2 Eu1 N1 C1 87.7(4) 3_675 . . 2_765 ? O2 Eu1 N1 C1 -32.3(4) . . . 2_765 ? O2 Eu1 N1 C1 -152.3(4) 2_765 . . 2_765 ? N2 Eu1 N1 C1 150.1(5) . . . 2_765 ? N2 Eu1 N1 C1 30.1(5) 2_765 . . 2_765 ? N2 Eu1 N1 C1 -89.9(5) 3_675 . . 2_765 ? N5 Eu1 N1 C1 -15.4(5) . . . 2_765 ? N5 Eu1 N1 C1 -135.4(5) 2_765 . . 2_765 ? O1 Eu1 N1 C1 10.6(5) 2_765 . . 3_675 ? O1 Eu1 N1 C1 130.6(5) . . . 3_675 ? O1 Eu1 N1 C1 -109.4(5) 3_675 . . 3_675 ? O2 Eu1 N1 C1 -152.3(4) 3_675 . . 3_675 ? O2 Eu1 N1 C1 87.7(4) . . . 3_675 ? O2 Eu1 N1 C1 -32.3(4) 2_765 . . 3_675 ? N2 Eu1 N1 C1 -89.9(5) . . . 3_675 ? N2 Eu1 N1 C1 150.1(5) 2_765 . . 3_675 ? N2 Eu1 N1 C1 30.1(5) 3_675 . . 3_675 ? N5 Eu1 N1 C1 104.6(5) . . . 3_675 ? N5 Eu1 N1 C1 -15.4(5) 2_765 . . 3_675 ? O1 Eu1 N2 C2 -145.4(6) 2_765 . . . ? O1 Eu1 N2 C2 122.6(6) . . . . ? O1 Eu1 N2 C2 154.3(7) 3_675 . . . ? O2 Eu1 N2 C2 101.6(7) 3_675 . . . ? O2 Eu1 N2 C2 -21.4(13) . . . . ? O2 Eu1 N2 C2 -129.5(7) 2_765 . . . ? N2 Eu1 N2 C2 39.3(6) 2_765 . . . ? N2 Eu1 N2 C2 -64.3(6) 3_675 . . . ? N1 Eu1 N2 C2 -12.5(6) . . . . ? N5 Eu1 N2 C2 102.8(11) . . . . ? N5 Eu1 N2 C2 -137.7(7) 2_765 . . . ? O1 Eu1 N2 C3 32.3(8) 2_765 . . . ? O1 Eu1 N2 C3 -59.7(9) . . . . ? O1 Eu1 N2 C3 -28.0(8) 3_675 . . . ? O2 Eu1 N2 C3 -80.7(8) 3_675 . . . ? O2 Eu1 N2 C3 156.3(8) . . . . ? O2 Eu1 N2 C3 48.2(7) 2_765 . . . ? N2 Eu1 N2 C3 -143.0(8) 2_765 . . . ? N2 Eu1 N2 C3 113.4(9) 3_675 . . . ? N1 Eu1 N2 C3 165.2(8) . . . . ? N5 Eu1 N2 C3 -79.5(13) . . . . ? N5 Eu1 N2 C3 40.0(8) 2_765 . . . ? O1 Eu1 N5 O3 -119(43) 2_765 . . . ? O1 Eu1 N5 O3 -30(42) . . . . ? O1 Eu1 N5 O3 -51(43) 3_675 . . . ? O2 Eu1 N5 O3 0(43) 3_675 . . . ? O2 Eu1 N5 O3 148(43) . . . . ? O2 Eu1 N5 O3 -124(43) 2_765 . . . ? N2 Eu1 N5 O3 -1(43) . . . . ? N2 Eu1 N5 O3 65(43) 2_765 . . . ? N2 Eu1 N5 O3 166(100) 3_675 . . . ? N1 Eu1 N5 O3 107(43) . . . . ? N5 Eu1 N5 O3 -121(43) 2_765 . . . ? O1 Eu1 N5 O1 -88.3(6) 2_765 . . . ? O1 Eu1 N5 O1 -21.0(5) 3_675 . . . ? O2 Eu1 N5 O1 30.1(5) 3_675 . . . ? O2 Eu1 N5 O1 178.3(8) . . . . ? O2 Eu1 N5 O1 -93.4(5) 2_765 . . . ? N2 Eu1 N5 O1 28.9(12) . . . . ? N2 Eu1 N5 O1 95.5(5) 2_765 . . . ? N2 Eu1 N5 O1 -163.8(5) 3_675 . . . ? N1 Eu1 N5 O1 137.0(5) . . . . ? N5 Eu1 N5 O1 -90.3(4) 2_765 . . . ? O1 Eu1 N5 O2 93.4(5) 2_765 . . . ? O1 Eu1 N5 O2 -178.3(8) . . . . ? O1 Eu1 N5 O2 160.7(5) 3_675 . . . ? O2 Eu1 N5 O2 -148.2(5) 3_675 . . . ? O2 Eu1 N5 O2 88.3(4) 2_765 . . . ? N2 Eu1 N5 O2 -149.4(9) . . . . ? N2 Eu1 N5 O2 -82.8(5) 2_765 . . . ? N2 Eu1 N5 O2 18.0(5) 3_675 . . . ? N1 Eu1 N5 O2 -41.2(5) . . . . ? N5 Eu1 N5 O2 91.4(6) 2_765 . . . ? O7 Eu2 N6 O4 -15.6(9) . . . . ? O7 Eu2 N6 O4 78.0(8) 2_755 . . . ? O7 Eu2 N6 O4 128(2) 3_775 . . . ? O5 Eu2 N6 O4 175.0(13) . . . . ? O5 Eu2 N6 O4 -94.9(8) 3_775 . . . ? O5 Eu2 N6 O4 -161.3(8) 2_755 . . . ? O4 Eu2 N6 O4 -89.9(6) 3_775 . . . ? O4 Eu2 N6 O4 147.6(8) 2_755 . . . ? N6 Eu2 N6 O4 -93.6(9) 3_775 . . . ? N6 Eu2 N6 O4 172.2(8) 2_755 . . . ? O7 Eu2 N6 O6 116(20) . . . . ? O7 Eu2 N6 O6 -151(20) 2_755 . . . ? O7 Eu2 N6 O6 -101(20) 3_775 . . . ? O5 Eu2 N6 O6 -54(20) . . . . ? O5 Eu2 N6 O6 36(20) 3_775 . . . ? O5 Eu2 N6 O6 -30(20) 2_755 . . . ? O4 Eu2 N6 O6 131(20) . . . . ? O4 Eu2 N6 O6 41(20) 3_775 . . . ? O4 Eu2 N6 O6 -81(20) 2_755 . . . ? N6 Eu2 N6 O6 38(20) 3_775 . . . ? N6 Eu2 N6 O6 -57(20) 2_755 . . . ? O7 Eu2 N6 O5 169.3(8) . . . . ? O7 Eu2 N6 O5 -97.0(8) 2_755 . . . ? O7 Eu2 N6 O5 -47(3) 3_775 . . . ? O5 Eu2 N6 O5 90.0(9) 3_775 . . . ? O5 Eu2 N6 O5 23.7(8) 2_755 . . . ? O4 Eu2 N6 O5 -175.0(13) . . . . ? O4 Eu2 N6 O5 95.1(8) 3_775 . . . ? O4 Eu2 N6 O5 -27.5(8) 2_755 . . . ? N6 Eu2 N6 O5 91.4(6) 3_775 . . . ? N6 Eu2 N6 O5 -2.9(7) 2_755 . . . ? C1 N1 C1 C2 -164.3(7) 2_765 . . . ? C1 N1 C1 C2 76.8(12) 3_675 . . . ? Eu1 N1 C1 C2 -43.7(8) . . . . ? C3 N2 C2 N3 -1.7(10) . . . . ? Eu1 N2 C2 N3 176.6(5) . . . . ? C3 N2 C2 C1 174.6(8) . . . . ? Eu1 N2 C2 C1 -7.0(11) . . . . ? C8 N3 C2 N2 1.5(10) . . . . ? C9 N3 C2 N2 -171.9(8) . . . . ? C8 N3 C2 C1 -174.7(8) . . . . ? C9 N3 C2 C1 11.9(14) . . . . ? N1 C1 C2 N2 36.5(12) . . . . ? N1 C1 C2 N3 -147.5(8) . . . . ? C2 N2 C3 C8 1.4(10) . . . . ? Eu1 N2 C3 C8 -176.6(6) . . . . ? C2 N2 C3 C4 177.1(10) . . . . ? Eu1 N2 C3 C4 -0.9(15) . . . . ? C8 C3 C4 C5 -3.3(15) . . . . ? N2 C3 C4 C5 -178.6(10) . . . . ? C3 C4 C5 C6 3.2(17) . . . . ? C4 C5 C6 C7 -2.4(17) . . . . ? C5 C6 C7 C8 1.6(16) . . . . ? C2 N3 C8 C7 -179.9(10) . . . . ? C9 N3 C8 C7 -6.3(15) . . . . ? C2 N3 C8 C3 -0.5(9) . . . . ? C9 N3 C8 C3 173.1(8) . . . . ? C6 C7 C8 N3 177.6(10) . . . . ? C6 C7 C8 C3 -1.8(15) . . . . ? N2 C3 C8 N3 -0.5(10) . . . . ? C4 C3 C8 N3 -176.8(8) . . . . ? N2 C3 C8 C7 179.0(8) . . . . ? C4 C3 C8 C7 2.7(14) . . . . ? C2 N3 C9 C10 97.4(11) . . . . ? C8 N3 C9 C10 -74.9(12) . . . . ? N3 C9 C10 C11 11.6(16) . . . . ? N3 C9 C10 C14 -171.6(10) . . . . ? C14 C10 C11 C12 1.0(19) . . . . ? C9 C10 C11 C12 177.9(12) . . . . ? C13 N4 C12 C11 4(3) . . . . ? C10 C11 C12 N4 -3(2) . . . . ? C12 N4 C13 C14 -2(2) . . . . ? N4 C13 C14 C10 0(2) . . . . ? C11 C10 C14 C13 1(2) . . . . ? C9 C10 C14 C13 -176.5(13) . . . . ? O3 N5 O1 Eu1 179.4(8) . . . . ? O2 N5 O1 Eu1 1.6(8) . . . . ? O1 Eu1 O1 N5 82.2(6) 2_765 . . . ? O1 Eu1 O1 N5 157.7(6) 3_675 . . . ? O2 Eu1 O1 N5 -148.5(6) 3_675 . . . ? O2 Eu1 O1 N5 -1.0(5) . . . . ? O2 Eu1 O1 N5 100.9(5) 2_765 . . . ? N2 Eu1 O1 N5 -169.3(5) . . . . ? N2 Eu1 O1 N5 -77.8(5) 2_765 . . . ? N2 Eu1 O1 N5 18.2(6) 3_675 . . . ? N1 Eu1 O1 N5 -60.0(6) . . . . ? N5 Eu1 O1 N5 91.6(4) 2_765 . . . ? O3 N5 O2 Eu1 -179.4(8) . . . . ? O1 N5 O2 Eu1 -1.6(8) . . . . ? O1 Eu1 O2 N5 -77.7(5) 2_765 . . . ? O1 Eu1 O2 N5 0.9(5) . . . . ? O1 Eu1 O2 N5 -21.9(5) 3_675 . . . ? O2 Eu1 O2 N5 35.7(6) 3_675 . . . ? O2 Eu1 O2 N5 -105.3(4) 2_765 . . . ? N2 Eu1 O2 N5 153.3(8) . . . . ? N2 Eu1 O2 N5 89.1(5) 2_765 . . . ? N2 Eu1 O2 N5 -160.6(5) 3_675 . . . ? N1 Eu1 O2 N5 145.2(4) . . . . ? N5 Eu1 O2 N5 -90.7(6) 2_765 . . . ? O6 N6 O4 Eu2 -177.3(12) . . . . ? O5 N6 O4 Eu2 5.0(13) . . . . ? O7 Eu2 O4 N6 163.5(9) . . . . ? O7 Eu2 O4 N6 -95.7(9) 2_755 . . . ? O7 Eu2 O4 N6 -151.0(11) 3_775 . . . ? O5 Eu2 O4 N6 -2.9(7) . . . . ? O5 Eu2 O4 N6 75.9(8) 3_775 . . . ? O5 Eu2 O4 N6 21.1(9) 2_755 . . . ? O4 Eu2 O4 N6 102.7(7) 3_775 . . . ? O4 Eu2 O4 N6 -36.3(9) 2_755 . . . ? N6 Eu2 O4 N6 88.4(9) 3_775 . . . ? N6 Eu2 O4 N6 -8.9(9) 2_755 . . . ? O4 N6 O5 Eu2 -5.0(13) . . . . ? O6 N6 O5 Eu2 177.2(12) . . . . ? O7 Eu2 O5 N6 -12.4(9) . . . . ? O7 Eu2 O5 N6 78.2(8) 2_755 . . . ? O7 Eu2 O5 N6 165.0(9) 3_775 . . . ? O5 Eu2 O5 N6 -79.5(9) 3_775 . . . ? O5 Eu2 O5 N6 -154.8(8) 2_755 . . . ? O4 Eu2 O5 N6 2.7(7) . . . . ? O4 Eu2 O5 N6 -99.1(8) 3_775 . . . ? O4 Eu2 O5 N6 151.1(8) 2_755 . . . ? N6 Eu2 O5 N6 -90.5(6) 3_775 . . . ? N6 Eu2 O5 N6 176.9(8) 2_755 . . . ? _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 62.56 _diffrn_measured_fraction_theta_full 0.954 _refine_diff_density_max 1.561 _refine_diff_density_min -2.389 _refine_diff_density_rms 0.159 data_1 _database_code_depnum_ccdc_archive 'CCDC 867185' #TrackingRef 'Compounds.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H46 Eu N19 O23' _chemical_formula_weight 1553.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 '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/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 12.9860(2) _cell_length_b 22.6333(4) _cell_length_c 20.6359(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.335(2) _cell_angle_gamma 90.00 _cell_volume 6047.87(17) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 16502 _cell_measurement_theta_min 3.0971 _cell_measurement_theta_max 29.7082 _exptl_crystal_description block _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.50 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.706 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3144 _exptl_absorpt_coefficient_mu 1.140 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5025 _exptl_absorpt_correction_T_max 0.5995 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 16.0855 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30606 _diffrn_reflns_av_R_equivalents 0.0320 _diffrn_reflns_av_sigmaI/netI 0.0438 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 27.00 _reflns_number_total 13173 _reflns_number_gt 11615 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0334P)^2^+8.5273P] 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 geom _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13173 _refine_ls_number_parameters 928 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0441 _refine_ls_R_factor_gt 0.0361 _refine_ls_wR_factor_ref 0.0857 _refine_ls_wR_factor_gt 0.0814 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Eu1 Eu 0.739533(10) 0.241337(6) 0.755005(7) 0.01357(5) Uani 1 1 d . . . N1 N 0.72926(18) 0.12150(11) 0.75822(11) 0.0158(5) Uani 1 1 d . . . N2 N 0.86722(18) 0.18938(11) 0.83367(12) 0.0177(5) Uani 1 1 d . . . N3 N 0.97726(18) 0.11564(11) 0.85914(12) 0.0181(5) Uani 1 1 d . . . N4 N 1.1771(3) 0.05559(18) 0.71634(18) 0.0521(10) Uani 1 1 d . . . N5 N 0.77649(18) 0.18737(11) 0.65263(12) 0.0177(5) Uani 1 1 d . . . N6 N 0.75387(19) 0.11285(11) 0.58208(12) 0.0210(5) Uani 1 1 d . . . N7 N 0.5264(3) 0.05900(17) 0.40446(16) 0.0493(9) Uani 1 1 d . . . N8 N 0.57181(18) 0.19753(11) 0.78193(12) 0.0185(5) Uani 1 1 d . . . N9 N 0.47639(19) 0.12960(12) 0.82750(13) 0.0236(6) Uani 1 1 d . . . N10 N 0.3374(3) 0.0586(2) 1.0167(2) 0.0752(14) Uani 1 1 d . . . N11 N 0.90330(19) 0.40920(12) 0.76698(13) 0.0244(6) Uani 1 1 d . . . N12 N 1.2228(2) 0.41367(14) 0.66058(16) 0.0364(7) Uani 1 1 d . . . N13 N 1.0615(2) 0.22335(12) 0.69072(14) 0.0261(6) Uani 1 1 d . . . N14 N 0.6620(2) 0.24679(12) 0.96402(13) 0.0254(6) Uani 1 1 d . . . N15 N 0.5745(2) 0.44268(14) 1.03874(14) 0.0303(6) Uani 1 1 d . . . N16 N 0.64381(19) 0.41955(12) 0.81314(13) 0.0218(6) Uani 1 1 d . . . N17 N 0.4598(2) 0.23302(13) 0.61789(14) 0.0289(6) Uani 1 1 d . . . N18 N 0.3784(2) 0.41431(13) 0.50066(13) 0.0264(6) Uani 1 1 d . . . N19 N 0.69768(19) 0.40590(12) 0.63910(12) 0.0208(5) Uani 1 1 d . . . C1 C 0.8336(2) 0.09578(13) 0.77417(15) 0.0186(6) Uani 1 1 d . . . H1A H 0.8719 0.0937 0.7345 0.022 Uiso 1 1 calc R . . H1B H 0.8271 0.0552 0.7914 0.022 Uiso 1 1 calc R . . C2 C 0.8906(2) 0.13386(13) 0.82377(14) 0.0159(6) Uani 1 1 d . . . C3 C 0.9450(2) 0.21025(13) 0.87822(14) 0.0177(6) Uani 1 1 d . . . C4 C 0.9604(2) 0.26619(14) 0.90503(16) 0.0237(7) Uani 1 1 d . . . H4A H 0.9135 0.2976 0.8947 0.028 Uiso 1 1 calc R . . C5 C 1.0474(2) 0.27419(15) 0.94760(17) 0.0278(7) Uani 1 1 d . . . H5A H 1.0603 0.3120 0.9664 0.033 Uiso 1 1 calc R . . C6 C 1.1160(2) 0.22825(15) 0.96348(16) 0.0259(7) Uani 1 1 d . . . H6A H 1.1744 0.2355 0.9930 0.031 Uiso 1 1 calc R . . C7 C 1.1015(2) 0.17256(15) 0.93750(15) 0.0220(6) Uani 1 1 d . . . H7A H 1.1480 0.1411 0.9485 0.026 Uiso 1 1 calc R . . C8 C 1.0149(2) 0.16476(13) 0.89415(14) 0.0185(6) Uani 1 1 d . . . C9 C 1.0188(2) 0.05539(14) 0.86244(16) 0.0262(7) Uani 1 1 d . . . H9A H 0.9623 0.0277 0.8708 0.031 Uiso 1 1 calc R . . H9B H 1.0714 0.0528 0.8997 0.031 Uiso 1 1 calc R . . C10 C 1.0670(2) 0.03607(15) 0.80183(17) 0.0273(7) Uani 1 1 d . . . C11 C 1.1290(3) 0.07304(18) 0.76825(19) 0.0372(9) Uani 1 1 d . . . H11A H 1.1380 0.1127 0.7827 0.045 Uiso 1 1 calc R . . C12 C 1.1603(4) -0.0009(2) 0.6963(2) 0.0498(11) Uani 1 1 d . . . H12A H 1.1936 -0.0143 0.6596 0.060 Uiso 1 1 calc R . . C13 C 1.0998(3) -0.03892(19) 0.7252(2) 0.0456(10) Uani 1 1 d . . . H13A H 1.0900 -0.0779 0.7088 0.055 Uiso 1 1 calc R . . C14 C 1.0517(3) -0.02074(18) 0.7791(2) 0.0377(9) Uani 1 1 d . . . H14A H 1.0084 -0.0471 0.8004 0.045 Uiso 1 1 calc R . . C15 C 0.6885(2) 0.10010(13) 0.69322(14) 0.0188(6) Uani 1 1 d . . . H15A H 0.7023 0.0573 0.6892 0.023 Uiso 1 1 calc R . . H15B H 0.6129 0.1064 0.6876 0.023 Uiso 1 1 calc R . . C16 C 0.7401(2) 0.13327(13) 0.64263(14) 0.0183(6) Uani 1 1 d . . . C17 C 0.8164(2) 0.20398(14) 0.59436(14) 0.0202(6) Uani 1 1 d . . . C18 C 0.8636(2) 0.25610(15) 0.57665(16) 0.0238(7) Uani 1 1 d . . . H18A H 0.8718 0.2885 0.6059 0.029 Uiso 1 1 calc R . . C19 C 0.8981(2) 0.25906(16) 0.51492(16) 0.0274(7) Uani 1 1 d . . . H19A H 0.9315 0.2940 0.5019 0.033 Uiso 1 1 calc R . . C20 C 0.8850(2) 0.21213(17) 0.47130(16) 0.0301(8) Uani 1 1 d . . . H20A H 0.9098 0.2158 0.4293 0.036 Uiso 1 1 calc R . . C21 C 0.8367(3) 0.16041(16) 0.48773(16) 0.0287(7) Uani 1 1 d . . . H21A H 0.8275 0.1285 0.4580 0.034 Uiso 1 1 calc R . . C22 C 0.8024(2) 0.15732(14) 0.54974(15) 0.0217(6) Uani 1 1 d . . . C23 C 0.7171(3) 0.05709(15) 0.55271(17) 0.0295(8) Uani 1 1 d . . . H23A H 0.7065 0.0282 0.5876 0.035 Uiso 1 1 calc R . . H23B H 0.7705 0.0410 0.5258 0.035 Uiso 1 1 calc R . . C24 C 0.6167(3) 0.06454(15) 0.51066(17) 0.0304(8) Uani 1 1 d . . . C25 C 0.6128(3) 0.05531(18) 0.44421(18) 0.0391(9) Uani 1 1 d . . . H25A H 0.6753 0.0458 0.4256 0.047 Uiso 1 1 calc R . . C26 C 0.4402(3) 0.07274(19) 0.4322(2) 0.0441(10) Uani 1 1 d . . . H26A H 0.3778 0.0753 0.4052 0.053 Uiso 1 1 calc R . . C27 C 0.4359(3) 0.08342(17) 0.4975(2) 0.0401(9) Uani 1 1 d . . . H27A H 0.3727 0.0940 0.5149 0.048 Uiso 1 1 calc R . . C28 C 0.5257(3) 0.07841(16) 0.53726(18) 0.0343(8) Uani 1 1 d . . . H28A H 0.5248 0.0845 0.5828 0.041 Uiso 1 1 calc R . . C29 C 0.6596(2) 0.10315(13) 0.80755(15) 0.0194(6) Uani 1 1 d . . . H29A H 0.6963 0.1051 0.8513 0.023 Uiso 1 1 calc R . . H29B H 0.6369 0.0619 0.7994 0.023 Uiso 1 1 calc R . . C30 C 0.5679(2) 0.14317(14) 0.80447(15) 0.0197(6) Uani 1 1 d . . . C31 C 0.4752(2) 0.22202(15) 0.79081(15) 0.0216(6) Uani 1 1 d . . . C32 C 0.4361(2) 0.27810(15) 0.77642(15) 0.0249(7) Uani 1 1 d . . . H32A H 0.4765 0.3075 0.7574 0.030 Uiso 1 1 calc R . . C33 C 0.3351(2) 0.28915(17) 0.79109(17) 0.0300(8) Uani 1 1 d . . . H33A H 0.3061 0.3271 0.7821 0.036 Uiso 1 1 calc R . . C34 C 0.2755(2) 0.24624(17) 0.81862(17) 0.0324(8) Uani 1 1 d . . . H34A H 0.2064 0.2554 0.8272 0.039 Uiso 1 1 calc R . . C35 C 0.3138(2) 0.19101(17) 0.83377(18) 0.0321(8) Uani 1 1 d . . . H35A H 0.2732 0.1619 0.8532 0.039 Uiso 1 1 calc R . . C36 C 0.4146(2) 0.17970(14) 0.81940(15) 0.0230(7) Uani 1 1 d . . . C37 C 0.4431(3) 0.07294(15) 0.85253(17) 0.0311(8) Uani 1 1 d . . . H37A H 0.4925 0.0419 0.8413 0.037 Uiso 1 1 calc R . . H37B H 0.3747 0.0627 0.8310 0.037 Uiso 1 1 calc R . . C38 C 0.4359(2) 0.07340(15) 0.92548(17) 0.0269(7) Uani 1 1 d . . . C39 C 0.3455(3) 0.0597(2) 0.9517(2) 0.0464(11) Uani 1 1 d . . . H39A H 0.2864 0.0506 0.9234 0.056 Uiso 1 1 calc R . . C40 C 0.4250(3) 0.0703(2) 1.0563(2) 0.0472(10) Uani 1 1 d . . . H40A H 0.4209 0.0684 1.1020 0.057 Uiso 1 1 calc R . . C41 C 0.5147(3) 0.08418(18) 1.03379(19) 0.0372(9) Uani 1 1 d . . . H41A H 0.5732 0.0930 1.0626 0.045 Uiso 1 1 calc R . . C42 C 0.5207(3) 0.08547(18) 0.9691(2) 0.0428(10) Uani 1 1 d . . . H42A H 0.5849 0.0949 0.9525 0.051 Uiso 1 1 calc R . . C43 C 0.9713(2) 0.31386(14) 0.72687(14) 0.0198(6) Uani 1 1 d . . . C44 C 0.9828(2) 0.37640(14) 0.73642(15) 0.0203(6) Uani 1 1 d . . . C45 C 1.0638(2) 0.40849(14) 0.71597(15) 0.0227(7) Uani 1 1 d . . . H45A H 1.0674 0.4500 0.7229 0.027 Uiso 1 1 calc R . . C46 C 1.1400(2) 0.37959(15) 0.68516(16) 0.0244(7) Uani 1 1 d . . . C47 C 1.1386(2) 0.31901(15) 0.67670(15) 0.0241(7) Uani 1 1 d . . . H47A H 1.1923 0.2996 0.6563 0.029 Uiso 1 1 calc R . . C48 C 1.0577(2) 0.28761(14) 0.69849(15) 0.0210(6) Uani 1 1 d . . . C49 C 0.6631(2) 0.33012(13) 0.88422(14) 0.0170(6) Uani 1 1 d . . . C50 C 0.6485(2) 0.30959(13) 0.94896(15) 0.0196(6) Uani 1 1 d . . . C51 C 0.6206(2) 0.34476(14) 0.99881(15) 0.0225(6) Uani 1 1 d . . . H51A H 0.6125 0.3287 1.0406 0.027 Uiso 1 1 calc R . . C52 C 0.6045(2) 0.40435(14) 0.98669(15) 0.0226(7) Uani 1 1 d . . . C53 C 0.6146(2) 0.42861(14) 0.92622(15) 0.0214(6) Uani 1 1 d . . . H53A H 0.6038 0.4697 0.9189 0.026 Uiso 1 1 calc R . . C54 C 0.6408(2) 0.39185(13) 0.87655(14) 0.0185(6) Uani 1 1 d . . . C55 C 0.5838(2) 0.31659(13) 0.63386(14) 0.0192(6) Uani 1 1 d . . . C56 C 0.4899(2) 0.29296(14) 0.60300(15) 0.0211(6) Uani 1 1 d . . . C57 C 0.4233(2) 0.32365(14) 0.56033(14) 0.0213(6) Uani 1 1 d . . . H57A H 0.3615 0.3059 0.5420 0.026 Uiso 1 1 calc R . . C58 C 0.4484(2) 0.38055(14) 0.54485(14) 0.0202(6) Uani 1 1 d . . . C59 C 0.5391(2) 0.40723(14) 0.57043(14) 0.0193(6) Uani 1 1 d . . . H59A H 0.5559 0.4464 0.5586 0.023 Uiso 1 1 calc R . . C60 C 0.6038(2) 0.37543(14) 0.61319(14) 0.0193(6) Uani 1 1 d . . . O1 O 0.89060(15) 0.28590(10) 0.73864(11) 0.0233(5) Uani 1 1 d . . . O2 O 0.84939(17) 0.38285(11) 0.80358(12) 0.0327(6) Uani 1 1 d . . . O3 O 0.89409(19) 0.46194(11) 0.75500(14) 0.0368(6) Uani 1 1 d . . . O4 O 1.2152(2) 0.46755(12) 0.66068(15) 0.0439(7) Uani 1 1 d . . . O5 O 1.2959(2) 0.38755(14) 0.6415(2) 0.0713(11) Uani 1 1 d . . . O6 O 1.1162(2) 0.20379(12) 0.65014(14) 0.0466(7) Uani 1 1 d . . . O7 O 1.0140(2) 0.19285(12) 0.72602(15) 0.0480(7) Uani 1 1 d . . . O8 O 0.69675(16) 0.29770(9) 0.84041(10) 0.0220(5) Uani 1 1 d . . . O9 O 0.6353(3) 0.21100(11) 0.92220(13) 0.0486(8) Uani 1 1 d . . . O10 O 0.6932(2) 0.23333(12) 1.01933(12) 0.0432(7) Uani 1 1 d . . . O11 O 0.5261(2) 0.42095(12) 1.08175(12) 0.0388(6) Uani 1 1 d . . . O12 O 0.5987(2) 0.49555(11) 1.03645(12) 0.0357(6) Uani 1 1 d . . . O13 O 0.66514(18) 0.47237(10) 0.81116(12) 0.0300(5) Uani 1 1 d . . . O14 O 0.62224(18) 0.38928(10) 0.76482(11) 0.0288(5) Uani 1 1 d . . . O15 O 0.63866(16) 0.28890(9) 0.67752(10) 0.0222(5) Uani 1 1 d . . . O16 O 0.5266(2) 0.19492(11) 0.62506(14) 0.0410(7) Uani 1 1 d . . . O17 O 0.3676(2) 0.22299(13) 0.62165(16) 0.0503(8) Uani 1 1 d . . . O18 O 0.30772(19) 0.38823(12) 0.46997(13) 0.0396(6) Uani 1 1 d . . . O19 O 0.39269(19) 0.46778(12) 0.49663(14) 0.0416(7) Uani 1 1 d . . . O20 O 0.69568(17) 0.45984(10) 0.64259(11) 0.0263(5) Uani 1 1 d . . . O21 O 0.77397(16) 0.37577(11) 0.65511(11) 0.0293(5) Uani 1 1 d . . . O1W O 1.4495(3) 0.04409(18) 0.69642(16) 0.0708(10) Uani 1 1 d . . . O2W O 1.2921(3) 0.10275(16) 0.6217(2) 0.0719(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu1 0.01426(7) 0.01222(8) 0.01421(7) 0.00047(5) 0.00091(5) 0.00060(5) N1 0.0176(12) 0.0142(12) 0.0156(12) -0.0010(10) 0.0012(9) 0.0008(9) N2 0.0199(12) 0.0162(13) 0.0167(12) 0.0002(10) -0.0009(10) 0.0002(9) N3 0.0182(12) 0.0165(13) 0.0193(12) 0.0019(10) -0.0003(10) 0.0027(9) N4 0.058(2) 0.053(2) 0.048(2) 0.0121(19) 0.0220(18) 0.0137(18) N5 0.0166(12) 0.0185(13) 0.0179(12) -0.0020(10) 0.0003(10) 0.0006(9) N6 0.0245(13) 0.0188(14) 0.0196(13) -0.0027(10) 0.0014(10) 0.0036(10) N7 0.052(2) 0.062(3) 0.0327(18) 0.0080(17) -0.0089(16) -0.0106(18) N8 0.0179(12) 0.0175(13) 0.0202(13) -0.0009(10) 0.0017(10) 0.0001(9) N9 0.0243(13) 0.0183(14) 0.0296(14) -0.0026(11) 0.0106(11) -0.0067(10) N10 0.053(2) 0.126(4) 0.049(2) -0.022(3) 0.023(2) -0.009(3) N11 0.0185(13) 0.0270(16) 0.0272(14) -0.0001(12) -0.0002(11) 0.0020(11) N12 0.0346(17) 0.0317(18) 0.0453(19) -0.0052(15) 0.0190(14) -0.0096(13) N13 0.0284(14) 0.0218(15) 0.0283(15) -0.0002(12) 0.0033(12) -0.0005(11) N14 0.0305(14) 0.0253(15) 0.0203(13) 0.0016(11) 0.0005(11) 0.0060(11) N15 0.0353(16) 0.0337(18) 0.0228(14) -0.0054(13) 0.0080(12) 0.0030(13) N16 0.0244(13) 0.0207(15) 0.0211(13) -0.0006(11) 0.0066(11) -0.0002(10) N17 0.0314(15) 0.0243(16) 0.0296(15) 0.0030(12) -0.0074(12) -0.0015(12) N18 0.0219(13) 0.0351(17) 0.0224(14) 0.0080(12) 0.0033(11) 0.0058(12) N19 0.0242(13) 0.0219(15) 0.0159(12) 0.0000(11) -0.0004(10) 0.0007(10) C1 0.0209(14) 0.0135(15) 0.0214(15) -0.0006(12) 0.0017(12) 0.0038(11) C2 0.0174(13) 0.0158(15) 0.0148(13) 0.0018(11) 0.0027(11) 0.0019(11) C3 0.0197(14) 0.0139(15) 0.0192(14) 0.0014(12) -0.0002(12) -0.0014(11) C4 0.0261(15) 0.0169(16) 0.0277(16) -0.0006(13) -0.0009(13) 0.0008(12) C5 0.0299(17) 0.0230(18) 0.0298(18) -0.0035(14) -0.0030(14) -0.0050(13) C6 0.0191(15) 0.035(2) 0.0235(16) 0.0007(14) -0.0017(12) -0.0071(13) C7 0.0163(14) 0.0282(18) 0.0216(15) 0.0043(13) 0.0022(12) 0.0000(12) C8 0.0173(14) 0.0192(16) 0.0194(14) 0.0022(12) 0.0039(11) -0.0006(11) C9 0.0255(16) 0.0214(17) 0.0315(18) 0.0054(14) 0.0009(14) 0.0045(12) C10 0.0228(16) 0.0265(19) 0.0318(18) -0.0012(14) -0.0033(14) 0.0064(13) C11 0.037(2) 0.034(2) 0.041(2) 0.0009(17) 0.0077(17) 0.0059(16) C12 0.059(3) 0.057(3) 0.035(2) -0.004(2) 0.012(2) 0.019(2) C13 0.051(2) 0.036(2) 0.050(3) -0.010(2) 0.004(2) 0.0065(18) C14 0.0352(19) 0.034(2) 0.044(2) -0.0052(18) 0.0015(17) 0.0002(16) C15 0.0218(14) 0.0169(15) 0.0175(14) -0.0038(12) -0.0003(12) -0.0015(11) C16 0.0196(14) 0.0182(16) 0.0169(14) -0.0008(12) 0.0003(11) 0.0034(11) C17 0.0178(14) 0.0253(17) 0.0174(14) 0.0004(12) 0.0008(11) 0.0051(12) C18 0.0193(14) 0.0299(18) 0.0216(15) 0.0016(13) -0.0027(12) -0.0027(12) C19 0.0201(15) 0.036(2) 0.0262(17) 0.0069(15) 0.0014(13) -0.0018(13) C20 0.0262(17) 0.045(2) 0.0193(16) 0.0024(15) 0.0048(13) 0.0073(15) C21 0.0329(18) 0.033(2) 0.0206(16) -0.0053(14) 0.0045(14) 0.0071(14) C22 0.0220(15) 0.0235(17) 0.0192(15) -0.0013(13) -0.0005(12) 0.0060(12) C23 0.0412(19) 0.0208(18) 0.0261(17) -0.0063(14) -0.0012(15) 0.0045(14) C24 0.043(2) 0.0179(17) 0.0294(18) -0.0010(14) -0.0046(15) -0.0029(14) C25 0.049(2) 0.039(2) 0.0283(19) 0.0013(17) -0.0017(17) -0.0020(17) C26 0.045(2) 0.044(3) 0.041(2) 0.0115(19) -0.0107(19) -0.0113(18) C27 0.038(2) 0.033(2) 0.048(2) 0.0040(18) -0.0029(18) -0.0053(16) C28 0.043(2) 0.028(2) 0.0315(19) -0.0067(16) -0.0012(16) -0.0047(15) C29 0.0239(15) 0.0143(15) 0.0205(15) 0.0016(12) 0.0039(12) -0.0024(11) C30 0.0205(14) 0.0192(16) 0.0198(15) -0.0048(12) 0.0042(12) -0.0037(11) C31 0.0193(14) 0.0254(17) 0.0201(15) -0.0032(13) 0.0016(12) -0.0015(12) C32 0.0226(15) 0.0290(18) 0.0232(16) 0.0029(14) 0.0017(13) 0.0018(13) C33 0.0232(16) 0.037(2) 0.0297(18) 0.0011(15) -0.0013(14) 0.0090(14) C34 0.0169(15) 0.048(2) 0.0325(18) -0.0066(17) 0.0028(13) 0.0039(14) C35 0.0213(16) 0.042(2) 0.0343(19) -0.0052(16) 0.0085(14) -0.0072(14) C36 0.0219(15) 0.0244(17) 0.0230(16) -0.0052(13) 0.0034(12) -0.0046(12) C37 0.0361(19) 0.0238(19) 0.0355(19) -0.0032(15) 0.0163(15) -0.0106(14) C38 0.0275(17) 0.0203(17) 0.0336(18) -0.0034(14) 0.0074(14) -0.0010(13) C39 0.033(2) 0.074(3) 0.034(2) -0.010(2) 0.0122(17) -0.0077(19) C40 0.057(3) 0.054(3) 0.031(2) -0.0056(19) 0.0086(19) 0.011(2) C41 0.035(2) 0.042(2) 0.034(2) 0.0065(17) -0.0026(16) 0.0027(16) C42 0.034(2) 0.040(2) 0.054(3) 0.013(2) -0.0002(18) -0.0037(16) C43 0.0181(14) 0.0234(17) 0.0174(14) 0.0053(12) -0.0025(11) -0.0014(11) C44 0.0158(14) 0.0238(17) 0.0213(15) 0.0008(13) 0.0019(12) 0.0031(11) C45 0.0232(15) 0.0185(16) 0.0260(16) 0.0032(13) 0.0002(13) -0.0013(12) C46 0.0205(15) 0.0256(18) 0.0280(17) 0.0012(14) 0.0084(13) -0.0054(12) C47 0.0215(15) 0.0273(18) 0.0242(16) -0.0023(14) 0.0058(13) 0.0005(12) C48 0.0217(15) 0.0209(17) 0.0200(15) 0.0000(12) 0.0000(12) -0.0018(12) C49 0.0141(13) 0.0200(16) 0.0170(14) -0.0046(12) 0.0016(11) -0.0017(11) C50 0.0191(14) 0.0187(16) 0.0209(15) -0.0002(12) 0.0017(12) 0.0001(11) C51 0.0252(15) 0.0262(18) 0.0163(14) -0.0006(13) 0.0024(12) -0.0008(12) C52 0.0240(15) 0.0245(17) 0.0200(15) -0.0078(13) 0.0059(12) 0.0018(12) C53 0.0211(15) 0.0196(16) 0.0240(16) -0.0044(13) 0.0050(12) -0.0009(12) C54 0.0207(14) 0.0180(16) 0.0169(14) 0.0015(12) 0.0023(11) -0.0023(11) C55 0.0222(14) 0.0191(16) 0.0161(14) -0.0031(12) 0.0001(12) 0.0068(11) C56 0.0255(15) 0.0173(16) 0.0205(15) 0.0002(12) 0.0022(12) 0.0018(12) C57 0.0214(15) 0.0240(17) 0.0183(15) -0.0011(13) 0.0008(12) 0.0024(12) C58 0.0210(14) 0.0256(17) 0.0140(14) 0.0021(12) 0.0016(12) 0.0064(12) C59 0.0242(15) 0.0206(16) 0.0135(14) 0.0005(12) 0.0034(12) 0.0029(12) C60 0.0201(14) 0.0211(16) 0.0163(14) -0.0031(12) -0.0009(11) 0.0020(11) O1 0.0180(10) 0.0229(12) 0.0289(12) 0.0049(10) 0.0013(9) -0.0033(8) O2 0.0266(12) 0.0400(15) 0.0334(13) 0.0013(11) 0.0137(10) 0.0027(10) O3 0.0358(14) 0.0228(14) 0.0528(16) -0.0002(12) 0.0092(12) 0.0064(10) O4 0.0385(15) 0.0249(15) 0.070(2) 0.0092(14) 0.0131(14) -0.0070(11) O5 0.0588(19) 0.0391(18) 0.126(3) -0.025(2) 0.070(2) -0.0153(14) O6 0.0659(19) 0.0286(15) 0.0492(17) -0.0094(13) 0.0303(15) -0.0011(13) O7 0.0578(17) 0.0236(15) 0.067(2) 0.0123(14) 0.0356(15) 0.0008(12) O8 0.0229(11) 0.0201(12) 0.0234(11) -0.0059(9) 0.0049(9) -0.0006(8) O9 0.094(2) 0.0205(14) 0.0296(14) 0.0011(11) -0.0098(15) -0.0060(14) O10 0.0662(18) 0.0378(16) 0.0244(13) 0.0036(12) -0.0058(13) 0.0195(13) O11 0.0518(16) 0.0417(16) 0.0253(13) -0.0051(12) 0.0181(12) 0.0009(12) O12 0.0506(15) 0.0257(14) 0.0318(13) -0.0107(11) 0.0098(12) -0.0014(11) O13 0.0395(13) 0.0189(12) 0.0326(13) 0.0026(10) 0.0094(11) -0.0040(10) O14 0.0421(14) 0.0274(13) 0.0171(11) -0.0026(10) 0.0026(10) -0.0014(10) O15 0.0272(11) 0.0187(12) 0.0201(11) 0.0029(9) -0.0029(9) 0.0045(9) O16 0.0442(15) 0.0166(13) 0.0599(18) -0.0008(12) -0.0104(13) 0.0039(11) O17 0.0346(15) 0.0384(17) 0.077(2) 0.0189(16) -0.0015(14) -0.0089(12) O18 0.0325(13) 0.0468(17) 0.0372(14) 0.0086(13) -0.0135(12) -0.0018(12) O19 0.0348(14) 0.0330(16) 0.0551(17) 0.0250(13) -0.0101(13) -0.0001(11) O20 0.0328(12) 0.0180(12) 0.0277(12) -0.0008(9) -0.0013(10) -0.0007(9) O21 0.0215(11) 0.0323(14) 0.0330(13) 0.0009(11) -0.0045(10) 0.0047(9) O1W 0.068(2) 0.091(3) 0.052(2) -0.003(2) 0.0017(17) -0.007(2) O2W 0.065(2) 0.060(2) 0.091(3) 0.009(2) 0.009(2) 0.0024(17) _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 2.254(2) . ? Eu1 O15 2.2617(19) . ? Eu1 O8 2.278(2) . ? Eu1 N8 2.494(2) . ? Eu1 N5 2.518(2) . ? Eu1 N2 2.522(2) . ? Eu1 N1 2.717(2) . ? N1 C29 1.472(4) . ? N1 C1 1.489(3) . ? N1 C15 1.485(3) . ? N2 C2 1.312(4) . ? N2 C3 1.396(4) . ? N3 C2 1.358(3) . ? N3 C8 1.394(4) . ? N3 C9 1.466(4) . ? N4 C11 1.339(5) . ? N4 C12 1.357(6) . ? N5 C16 1.323(4) . ? N5 C17 1.396(4) . ? N6 C16 1.357(4) . ? N6 C22 1.385(4) . ? N6 C23 1.465(4) . ? N7 C25 1.341(5) . ? N7 C26 1.333(6) . ? N8 C30 1.318(4) . ? N8 C31 1.397(4) . ? N9 C30 1.348(4) . ? N9 C36 1.392(4) . ? N9 C37 1.460(4) . ? N10 C39 1.355(6) . ? N10 C40 1.375(6) . ? N11 O3 1.223(4) . ? N11 O2 1.223(4) . ? N11 C44 1.454(4) . ? N12 O5 1.209(4) . ? N12 O4 1.224(4) . ? N12 C46 1.445(4) . ? N13 O7 1.206(4) . ? N13 O6 1.221(4) . ? N13 C48 1.464(4) . ? N14 O10 1.221(3) . ? N14 O9 1.215(4) . ? N14 C50 1.463(4) . ? N15 O11 1.228(4) . ? N15 O12 1.239(4) . ? N15 C52 1.457(4) . ? N16 O14 1.225(3) . ? N16 O13 1.228(3) . ? N16 C54 1.454(4) . ? N17 O16 1.224(4) . ? N17 O17 1.227(4) . ? N17 C56 1.451(4) . ? N18 O19 1.228(4) . ? N18 O18 1.227(4) . ? N18 C58 1.455(4) . ? N19 O20 1.223(3) . ? N19 O21 1.227(3) . ? N19 C60 1.466(4) . ? C1 C2 1.491(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C3 C4 1.390(4) . ? C3 C8 1.395(4) . ? C4 C5 1.389(4) . ? C4 H4A 0.9500 . ? C5 C6 1.392(5) . ? C5 H5A 0.9500 . ? C6 C7 1.377(5) . ? C6 H6A 0.9500 . ? C7 C8 1.394(4) . ? C7 H7A 0.9500 . ? C9 C10 1.505(5) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C14 1.378(5) . ? C10 C11 1.384(5) . ? C11 H11A 0.9500 . ? C12 C13 1.335(6) . ? C12 H12A 0.9500 . ? C13 C14 1.380(6) . ? C13 H13A 0.9500 . ? C14 H14A 0.9500 . ? C15 C16 1.486(4) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C17 C18 1.391(4) . ? C17 C22 1.404(4) . ? C18 C19 1.383(5) . ? C18 H18A 0.9500 . ? C19 C20 1.394(5) . ? C19 H19A 0.9500 . ? C20 C21 1.382(5) . ? C20 H20A 0.9500 . ? C21 C22 1.388(4) . ? C21 H21A 0.9500 . ? C23 C24 1.520(5) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C28 1.376(5) . ? C24 C25 1.384(5) . ? C25 H25A 0.9500 . ? C26 C27 1.374(6) . ? C26 H26A 0.9500 . ? C27 C28 1.379(5) . ? C27 H27A 0.9500 . ? C28 H28A 0.9500 . ? C29 C30 1.494(4) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C31 C32 1.391(5) . ? C31 C36 1.398(4) . ? C32 C33 1.390(4) . ? C32 H32A 0.9500 . ? C33 C34 1.390(5) . ? C33 H33A 0.9500 . ? C34 C35 1.373(5) . ? C34 H34A 0.9500 . ? C35 C36 1.388(4) . ? C35 H35A 0.9500 . ? C37 C38 1.515(5) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.366(5) . ? C38 C42 1.395(5) . ? C39 H39A 0.9500 . ? C40 C41 1.324(6) . ? C40 H40A 0.9500 . ? C41 C42 1.343(6) . ? C41 H41A 0.9500 . ? C42 H42A 0.9500 . ? C43 O1 1.263(4) . ? C43 C48 1.434(4) . ? C43 C44 1.435(4) . ? C44 C45 1.370(4) . ? C45 C46 1.381(4) . ? C45 H45A 0.9500 . ? C46 C47 1.382(5) . ? C47 C48 1.372(4) . ? C47 H47A 0.9500 . ? C49 O8 1.268(3) . ? C49 C54 1.433(4) . ? C49 C50 1.440(4) . ? C50 C51 1.371(4) . ? C51 C52 1.385(5) . ? C51 H51A 0.9500 . ? C52 C53 1.378(4) . ? C53 C54 1.382(4) . ? C53 H53A 0.9500 . ? C55 O15 1.270(3) . ? C55 C60 1.428(4) . ? C55 C56 1.436(4) . ? C56 C57 1.375(4) . ? C57 C58 1.372(4) . ? C57 H57A 0.9500 . ? C58 C59 1.392(4) . ? C59 C60 1.375(4) . ? C59 H59A 0.9500 . ? 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 O15 98.35(8) . . ? O1 Eu1 O8 97.54(8) . . ? O15 Eu1 O8 96.80(8) . . ? O1 Eu1 N8 174.92(8) . . ? O15 Eu1 N8 82.99(8) . . ? O8 Eu1 N8 77.41(8) . . ? O1 Eu1 N5 82.42(8) . . ? O15 Eu1 N5 76.98(8) . . ? O8 Eu1 N5 173.67(8) . . ? N8 Eu1 N5 102.66(8) . . ? O1 Eu1 N2 76.57(8) . . ? O15 Eu1 N2 173.99(8) . . ? O8 Eu1 N2 87.14(8) . . ? N8 Eu1 N2 102.36(8) . . ? N5 Eu1 N2 98.98(8) . . ? O1 Eu1 N1 119.69(7) . . ? O15 Eu1 N1 117.75(7) . . ? O8 Eu1 N1 121.66(8) . . ? N8 Eu1 N1 63.40(8) . . ? N5 Eu1 N1 63.19(8) . . ? N2 Eu1 N1 63.25(7) . . ? C29 N1 C1 109.5(2) . . ? C29 N1 C15 109.7(2) . . ? C1 N1 C15 109.2(2) . . ? C29 N1 Eu1 109.42(17) . . ? C1 N1 Eu1 110.50(17) . . ? C15 N1 Eu1 108.56(17) . . ? C2 N2 C3 105.2(2) . . ? C2 N2 Eu1 119.66(18) . . ? C3 N2 Eu1 132.39(19) . . ? C2 N3 C8 106.3(2) . . ? C2 N3 C9 126.5(3) . . ? C8 N3 C9 127.2(2) . . ? C11 N4 C12 116.6(4) . . ? C16 N5 C17 105.4(2) . . ? C16 N5 Eu1 119.4(2) . . ? C17 N5 Eu1 134.3(2) . . ? C16 N6 C22 107.0(3) . . ? C16 N6 C23 127.8(3) . . ? C22 N6 C23 124.9(3) . . ? C25 N7 C26 116.3(4) . . ? C30 N8 C31 105.4(3) . . ? C30 N8 Eu1 120.52(19) . . ? C31 N8 Eu1 132.8(2) . . ? C30 N9 C36 106.7(3) . . ? C30 N9 C37 128.1(3) . . ? C36 N9 C37 125.1(3) . . ? C39 N10 C40 117.6(4) . . ? O3 N11 O2 123.3(3) . . ? O3 N11 C44 118.2(3) . . ? O2 N11 C44 118.5(3) . . ? O5 N12 O4 123.6(3) . . ? O5 N12 C46 118.4(3) . . ? O4 N12 C46 118.0(3) . . ? O7 N13 O6 123.8(3) . . ? O7 N13 C48 118.6(3) . . ? O6 N13 C48 117.5(3) . . ? O10 N14 O9 123.7(3) . . ? O10 N14 C50 117.9(3) . . ? O9 N14 C50 118.3(3) . . ? O11 N15 O12 124.0(3) . . ? O11 N15 C52 118.3(3) . . ? O12 N15 C52 117.7(3) . . ? O14 N16 O13 123.8(3) . . ? O14 N16 C54 118.1(3) . . ? O13 N16 C54 118.1(3) . . ? O16 N17 O17 123.2(3) . . ? O16 N17 C56 119.0(3) . . ? O17 N17 C56 117.8(3) . . ? O19 N18 O18 123.4(3) . . ? O19 N18 C58 118.0(3) . . ? O18 N18 C58 118.6(3) . . ? O20 N19 O21 124.0(3) . . ? O20 N19 C60 118.0(2) . . ? O21 N19 C60 118.0(3) . . ? N1 C1 C2 108.8(2) . . ? N1 C1 H1A 109.9 . . ? C2 C1 H1A 109.9 . . ? N1 C1 H1B 109.9 . . ? C2 C1 H1B 109.9 . . ? H1A C1 H1B 108.3 . . ? N2 C2 N3 113.5(3) . . ? N2 C2 C1 123.5(2) . . ? N3 C2 C1 122.8(3) . . ? C4 C3 N2 130.2(3) . . ? C4 C3 C8 120.5(3) . . ? N2 C3 C8 109.3(3) . . ? C5 C4 C3 117.1(3) . . ? C5 C4 H4A 121.4 . . ? C3 C4 H4A 121.4 . . ? C4 C5 C6 121.8(3) . . ? C4 C5 H5A 119.1 . . ? C6 C5 H5A 119.1 . . ? C7 C6 C5 121.7(3) . . ? C7 C6 H6A 119.2 . . ? C5 C6 H6A 119.2 . . ? C6 C7 C8 116.5(3) . . ? C6 C7 H7A 121.8 . . ? C8 C7 H7A 121.8 . . ? N3 C8 C7 131.9(3) . . ? N3 C8 C3 105.7(2) . . ? C7 C8 C3 122.4(3) . . ? N3 C9 C10 114.0(3) . . ? N3 C9 H9A 108.8 . . ? C10 C9 H9A 108.8 . . ? N3 C9 H9B 108.8 . . ? C10 C9 H9B 108.8 . . ? H9A C9 H9B 107.7 . . ? C14 C10 C11 117.9(4) . . ? C14 C10 C9 119.7(3) . . ? C11 C10 C9 122.3(3) . . ? N4 C11 C10 123.1(4) . . ? N4 C11 H11A 118.4 . . ? C10 C11 H11A 118.4 . . ? C13 C12 N4 123.9(4) . . ? C13 C12 H12A 118.1 . . ? N4 C12 H12A 118.1 . . ? C12 C13 C14 119.1(4) . . ? C12 C13 H13A 120.5 . . ? C14 C13 H13A 120.5 . . ? C10 C14 C13 119.4(4) . . ? C10 C14 H14A 120.3 . . ? C13 C14 H14A 120.3 . . ? C16 C15 N1 108.7(2) . . ? C16 C15 H15A 109.9 . . ? N1 C15 H15A 109.9 . . ? C16 C15 H15B 109.9 . . ? N1 C15 H15B 109.9 . . ? H15A C15 H15B 108.3 . . ? N5 C16 N6 112.9(3) . . ? N5 C16 C15 122.2(3) . . ? N6 C16 C15 124.9(3) . . ? C18 C17 N5 130.9(3) . . ? C18 C17 C22 120.2(3) . . ? N5 C17 C22 108.9(3) . . ? C19 C18 C17 117.6(3) . . ? C19 C18 H18A 121.2 . . ? C17 C18 H18A 121.2 . . ? C18 C19 C20 121.7(3) . . ? C18 C19 H19A 119.1 . . ? C20 C19 H19A 119.1 . . ? C21 C20 C19 121.5(3) . . ? C21 C20 H20A 119.3 . . ? C19 C20 H20A 119.3 . . ? C20 C21 C22 116.9(3) . . ? C20 C21 H21A 121.6 . . ? C22 C21 H21A 121.6 . . ? N6 C22 C21 132.1(3) . . ? N6 C22 C17 105.8(3) . . ? C21 C22 C17 122.1(3) . . ? N6 C23 C24 112.3(3) . . ? N6 C23 H23A 109.1 . . ? C24 C23 H23A 109.1 . . ? N6 C23 H23B 109.1 . . ? C24 C23 H23B 109.1 . . ? H23A C23 H23B 107.9 . . ? C28 C24 C25 117.5(3) . . ? C28 C24 C23 121.5(3) . . ? C25 C24 C23 120.9(3) . . ? N7 C25 C24 124.2(4) . . ? N7 C25 H25A 117.9 . . ? C24 C25 H25A 117.9 . . ? N7 C26 C27 124.1(4) . . ? N7 C26 H26A 118.0 . . ? C27 C26 H26A 118.0 . . ? C26 C27 C28 118.2(4) . . ? C26 C27 H27A 120.9 . . ? C28 C27 H27A 120.9 . . ? C24 C28 C27 119.7(4) . . ? C24 C28 H28A 120.2 . . ? C27 C28 H28A 120.2 . . ? N1 C29 C30 109.2(2) . . ? N1 C29 H29A 109.8 . . ? C30 C29 H29A 109.8 . . ? N1 C29 H29B 109.8 . . ? C30 C29 H29B 109.8 . . ? H29A C29 H29B 108.3 . . ? N8 C30 N9 113.3(3) . . ? N8 C30 C29 121.9(3) . . ? N9 C30 C29 124.6(3) . . ? C32 C31 N8 130.6(3) . . ? C32 C31 C36 120.5(3) . . ? N8 C31 C36 108.8(3) . . ? C31 C32 C33 116.9(3) . . ? C31 C32 H32A 121.5 . . ? C33 C32 H32A 121.5 . . ? C34 C33 C32 121.8(3) . . ? C34 C33 H33A 119.1 . . ? C32 C33 H33A 119.1 . . ? C35 C34 C33 121.7(3) . . ? C35 C34 H34A 119.1 . . ? C33 C34 H34A 119.1 . . ? C34 C35 C36 116.8(3) . . ? C34 C35 H35A 121.6 . . ? C36 C35 H35A 121.6 . . ? C35 C36 N9 132.0(3) . . ? C35 C36 C31 122.2(3) . . ? N9 C36 C31 105.8(3) . . ? N9 C37 C38 112.8(3) . . ? N9 C37 H37A 109.0 . . ? C38 C37 H37A 109.0 . . ? N9 C37 H37B 109.0 . . ? C38 C37 H37B 109.0 . . ? H37A C37 H37B 107.8 . . ? C39 C38 C42 116.7(4) . . ? C39 C38 C37 120.7(3) . . ? C42 C38 C37 122.5(3) . . ? N10 C39 C38 122.0(4) . . ? N10 C39 H39A 119.0 . . ? C38 C39 H39A 119.0 . . ? C41 C40 N10 123.2(4) . . ? C41 C40 H40A 118.4 . . ? N10 C40 H40A 118.4 . . ? C40 C41 C42 118.2(4) . . ? C40 C41 H41A 120.9 . . ? C42 C41 H41A 120.9 . . ? C41 C42 C38 122.3(4) . . ? C41 C42 H42A 118.8 . . ? C38 C42 H42A 118.8 . . ? O1 C43 C48 123.9(3) . . ? O1 C43 C44 123.2(3) . . ? C48 C43 C44 112.8(3) . . ? C45 C44 C43 123.7(3) . . ? C45 C44 N11 116.7(3) . . ? C43 C44 N11 119.5(3) . . ? C44 C45 C46 118.9(3) . . ? C44 C45 H45A 120.5 . . ? C46 C45 H45A 120.5 . . ? C47 C46 C45 121.6(3) . . ? C47 C46 N12 119.2(3) . . ? C45 C46 N12 119.1(3) . . ? C48 C47 C46 118.4(3) . . ? C48 C47 H47A 120.8 . . ? C46 C47 H47A 120.8 . . ? C47 C48 C43 124.2(3) . . ? C47 C48 N13 116.5(3) . . ? C43 C48 N13 119.3(3) . . ? O8 C49 C54 124.3(3) . . ? O8 C49 C50 123.5(3) . . ? C54 C49 C50 112.2(3) . . ? C51 C50 C49 124.7(3) . . ? C51 C50 N14 116.0(3) . . ? C49 C50 N14 119.2(3) . . ? C50 C51 C52 118.3(3) . . ? C50 C51 H51A 120.8 . . ? C52 C51 H51A 120.8 . . ? C53 C52 C51 121.9(3) . . ? C53 C52 N15 118.6(3) . . ? C51 C52 N15 119.5(3) . . ? C52 C53 C54 118.5(3) . . ? C52 C53 H53A 120.8 . . ? C54 C53 H53A 120.8 . . ? C53 C54 C49 124.3(3) . . ? C53 C54 N16 115.6(3) . . ? C49 C54 N16 120.0(3) . . ? O15 C55 C60 124.6(3) . . ? O15 C55 C56 122.9(3) . . ? C60 C55 C56 112.5(3) . . ? C57 C56 C55 124.6(3) . . ? C57 C56 N17 116.2(3) . . ? C55 C56 N17 119.2(3) . . ? C58 C57 C56 118.3(3) . . ? C58 C57 H57A 120.8 . . ? C56 C57 H57A 120.8 . . ? C57 C58 C59 121.9(3) . . ? C57 C58 N18 119.4(3) . . ? C59 C58 N18 118.7(3) . . ? C60 C59 C58 118.4(3) . . ? C60 C59 H59A 120.8 . . ? C58 C59 H59A 120.8 . . ? C59 C60 C55 124.3(3) . . ? C59 C60 N19 116.0(3) . . ? C55 C60 N19 119.6(3) . . ? C43 O1 Eu1 175.5(2) . . ? C49 O8 Eu1 173.40(19) . . ? C55 O15 Eu1 178.5(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Eu1 N1 C29 142.82(16) . . . . ? O15 Eu1 N1 C29 -97.91(18) . . . . ? O8 Eu1 N1 C29 20.87(19) . . . . ? N8 Eu1 N1 C29 -32.61(16) . . . . ? N5 Eu1 N1 C29 -154.46(19) . . . . ? N2 Eu1 N1 C29 88.75(18) . . . . ? O1 Eu1 N1 C1 22.2(2) . . . . ? O15 Eu1 N1 C1 141.45(17) . . . . ? O8 Eu1 N1 C1 -99.76(18) . . . . ? N8 Eu1 N1 C1 -153.2(2) . . . . ? N5 Eu1 N1 C1 84.91(18) . . . . ? N2 Eu1 N1 C1 -31.88(17) . . . . ? O1 Eu1 N1 C15 -97.51(18) . . . . ? O15 Eu1 N1 C15 21.76(19) . . . . ? O8 Eu1 N1 C15 140.55(16) . . . . ? N8 Eu1 N1 C15 87.07(18) . . . . ? N5 Eu1 N1 C15 -34.79(16) . . . . ? N2 Eu1 N1 C15 -151.58(19) . . . . ? O1 Eu1 N2 C2 -111.2(2) . . . . ? O15 Eu1 N2 C2 -78.6(8) . . . . ? O8 Eu1 N2 C2 150.3(2) . . . . ? N8 Eu1 N2 C2 73.9(2) . . . . ? N5 Eu1 N2 C2 -31.3(2) . . . . ? N1 Eu1 N2 C2 22.5(2) . . . . ? O1 Eu1 N2 C3 46.9(3) . . . . ? O15 Eu1 N2 C3 79.5(8) . . . . ? O8 Eu1 N2 C3 -51.6(3) . . . . ? N8 Eu1 N2 C3 -128.0(3) . . . . ? N5 Eu1 N2 C3 126.8(3) . . . . ? N1 Eu1 N2 C3 -179.4(3) . . . . ? O1 Eu1 N5 C16 151.7(2) . . . . ? O15 Eu1 N5 C16 -107.9(2) . . . . ? O8 Eu1 N5 C16 -118.2(7) . . . . ? N8 Eu1 N5 C16 -28.2(2) . . . . ? N2 Eu1 N5 C16 76.7(2) . . . . ? N1 Eu1 N5 C16 22.87(19) . . . . ? O1 Eu1 N5 C17 -40.3(2) . . . . ? O15 Eu1 N5 C17 60.2(2) . . . . ? O8 Eu1 N5 C17 49.8(8) . . . . ? N8 Eu1 N5 C17 139.8(2) . . . . ? N2 Eu1 N5 C17 -115.3(2) . . . . ? N1 Eu1 N5 C17 -169.1(3) . . . . ? O1 Eu1 N8 C30 -107.1(9) . . . . ? O15 Eu1 N8 C30 147.4(2) . . . . ? O8 Eu1 N8 C30 -114.0(2) . . . . ? N5 Eu1 N8 C30 72.5(2) . . . . ? N2 Eu1 N8 C30 -29.8(2) . . . . ? N1 Eu1 N8 C30 21.5(2) . . . . ? O1 Eu1 N8 C31 58.0(10) . . . . ? O15 Eu1 N8 C31 -47.5(3) . . . . ? O8 Eu1 N8 C31 51.1(3) . . . . ? N5 Eu1 N8 C31 -122.4(3) . . . . ? N2 Eu1 N8 C31 135.3(3) . . . . ? N1 Eu1 N8 C31 -173.4(3) . . . . ? C29 N1 C1 C2 -82.3(3) . . . . ? C15 N1 C1 C2 157.6(2) . . . . ? Eu1 N1 C1 C2 38.3(3) . . . . ? C3 N2 C2 N3 1.1(3) . . . . ? Eu1 N2 C2 N3 164.47(19) . . . . ? C3 N2 C2 C1 -173.7(3) . . . . ? Eu1 N2 C2 C1 -10.3(4) . . . . ? C8 N3 C2 N2 -1.6(3) . . . . ? C9 N3 C2 N2 175.1(3) . . . . ? C8 N3 C2 C1 173.2(3) . . . . ? C9 N3 C2 C1 -10.1(5) . . . . ? N1 C1 C2 N2 -21.4(4) . . . . ? N1 C1 C2 N3 164.3(3) . . . . ? C2 N2 C3 C4 178.6(3) . . . . ? Eu1 N2 C3 C4 18.3(5) . . . . ? C2 N2 C3 C8 -0.1(3) . . . . ? Eu1 N2 C3 C8 -160.5(2) . . . . ? N2 C3 C4 C5 -178.6(3) . . . . ? C8 C3 C4 C5 0.1(5) . . . . ? C3 C4 C5 C6 -0.6(5) . . . . ? C4 C5 C6 C7 0.3(5) . . . . ? C5 C6 C7 C8 0.5(5) . . . . ? C2 N3 C8 C7 -179.1(3) . . . . ? C9 N3 C8 C7 4.2(5) . . . . ? C2 N3 C8 C3 1.4(3) . . . . ? C9 N3 C8 C3 -175.3(3) . . . . ? C6 C7 C8 N3 179.6(3) . . . . ? C6 C7 C8 C3 -1.0(5) . . . . ? C4 C3 C8 N3 -179.7(3) . . . . ? N2 C3 C8 N3 -0.8(3) . . . . ? C4 C3 C8 C7 0.8(5) . . . . ? N2 C3 C8 C7 179.7(3) . . . . ? C2 N3 C9 C10 72.5(4) . . . . ? C8 N3 C9 C10 -111.4(3) . . . . ? N3 C9 C10 C14 -140.0(3) . . . . ? N3 C9 C10 C11 41.7(4) . . . . ? C12 N4 C11 C10 1.5(6) . . . . ? C14 C10 C11 N4 -2.2(5) . . . . ? C9 C10 C11 N4 176.2(3) . . . . ? C11 N4 C12 C13 0.0(6) . . . . ? N4 C12 C13 C14 -0.8(7) . . . . ? C11 C10 C14 C13 1.3(5) . . . . ? C9 C10 C14 C13 -177.2(3) . . . . ? C12 C13 C14 C10 0.1(6) . . . . ? C29 N1 C15 C16 163.2(2) . . . . ? C1 N1 C15 C16 -76.8(3) . . . . ? Eu1 N1 C15 C16 43.7(3) . . . . ? C17 N5 C16 N6 0.5(3) . . . . ? Eu1 N5 C16 N6 171.60(17) . . . . ? C17 N5 C16 C15 -178.6(3) . . . . ? Eu1 N5 C16 C15 -7.5(4) . . . . ? C22 N6 C16 N5 -0.5(3) . . . . ? C23 N6 C16 N5 -175.2(3) . . . . ? C22 N6 C16 C15 178.5(3) . . . . ? C23 N6 C16 C15 3.8(5) . . . . ? N1 C15 C16 N5 -27.3(4) . . . . ? N1 C15 C16 N6 153.7(3) . . . . ? C16 N5 C17 C18 179.6(3) . . . . ? Eu1 N5 C17 C18 10.4(5) . . . . ? C16 N5 C17 C22 -0.3(3) . . . . ? Eu1 N5 C17 C22 -169.44(19) . . . . ? N5 C17 C18 C19 178.3(3) . . . . ? C22 C17 C18 C19 -1.8(4) . . . . ? C17 C18 C19 C20 0.9(5) . . . . ? C18 C19 C20 C21 0.1(5) . . . . ? C19 C20 C21 C22 -0.3(5) . . . . ? C16 N6 C22 C21 178.5(3) . . . . ? C23 N6 C22 C21 -6.6(5) . . . . ? C16 N6 C22 C17 0.3(3) . . . . ? C23 N6 C22 C17 175.2(3) . . . . ? C20 C21 C22 N6 -178.5(3) . . . . ? C20 C21 C22 C17 -0.6(5) . . . . ? C18 C17 C22 N6 -179.9(3) . . . . ? N5 C17 C22 N6 0.0(3) . . . . ? C18 C17 C22 C21 1.7(4) . . . . ? N5 C17 C22 C21 -178.4(3) . . . . ? C16 N6 C23 C24 96.9(4) . . . . ? C22 N6 C23 C24 -76.9(4) . . . . ? N6 C23 C24 C28 -67.9(4) . . . . ? N6 C23 C24 C25 114.7(4) . . . . ? C26 N7 C25 C24 0.3(6) . . . . ? C28 C24 C25 N7 -0.1(6) . . . . ? C23 C24 C25 N7 177.5(4) . . . . ? C25 N7 C26 C27 0.5(6) . . . . ? N7 C26 C27 C28 -1.5(6) . . . . ? C25 C24 C28 C27 -0.9(5) . . . . ? C23 C24 C28 C27 -178.5(3) . . . . ? C26 C27 C28 C24 1.6(6) . . . . ? C1 N1 C29 C30 161.9(2) . . . . ? C15 N1 C29 C30 -78.3(3) . . . . ? Eu1 N1 C29 C30 40.7(3) . . . . ? C31 N8 C30 N9 0.1(3) . . . . ? Eu1 N8 C30 N9 168.80(19) . . . . ? C31 N8 C30 C29 -176.1(3) . . . . ? Eu1 N8 C30 C29 -7.3(4) . . . . ? C36 N9 C30 N8 -0.1(4) . . . . ? C37 N9 C30 N8 176.3(3) . . . . ? C36 N9 C30 C29 175.9(3) . . . . ? C37 N9 C30 C29 -7.7(5) . . . . ? N1 C29 C30 N8 -25.3(4) . . . . ? N1 C29 C30 N9 159.0(3) . . . . ? C30 N8 C31 C32 179.5(3) . . . . ? Eu1 N8 C31 C32 12.8(5) . . . . ? C30 N8 C31 C36 -0.1(3) . . . . ? Eu1 N8 C31 C36 -166.8(2) . . . . ? N8 C31 C32 C33 179.8(3) . . . . ? C36 C31 C32 C33 -0.7(5) . . . . ? C31 C32 C33 C34 -0.3(5) . . . . ? C32 C33 C34 C35 1.1(5) . . . . ? C33 C34 C35 C36 -0.9(5) . . . . ? C34 C35 C36 N9 -179.4(3) . . . . ? C34 C35 C36 C31 -0.1(5) . . . . ? C30 N9 C36 C35 179.5(3) . . . . ? C37 N9 C36 C35 3.0(6) . . . . ? C30 N9 C36 C31 0.0(3) . . . . ? C37 N9 C36 C31 -176.5(3) . . . . ? C32 C31 C36 C35 0.9(5) . . . . ? N8 C31 C36 C35 -179.5(3) . . . . ? C32 C31 C36 N9 -179.6(3) . . . . ? N8 C31 C36 N9 0.0(3) . . . . ? C30 N9 C37 C38 108.6(4) . . . . ? C36 N9 C37 C38 -75.6(4) . . . . ? N9 C37 C38 C39 122.7(4) . . . . ? N9 C37 C38 C42 -59.7(5) . . . . ? C40 N10 C39 C38 -1.8(8) . . . . ? C42 C38 C39 N10 1.0(7) . . . . ? C37 C38 C39 N10 178.7(4) . . . . ? C39 N10 C40 C41 2.1(8) . . . . ? N10 C40 C41 C42 -1.6(7) . . . . ? C40 C41 C42 C38 0.7(6) . . . . ? C39 C38 C42 C41 -0.4(6) . . . . ? C37 C38 C42 C41 -178.1(4) . . . . ? O1 C43 C44 C45 -171.1(3) . . . . ? C48 C43 C44 C45 4.9(4) . . . . ? O1 C43 C44 N11 6.3(4) . . . . ? C48 C43 C44 N11 -177.8(3) . . . . ? O3 N11 C44 C45 22.7(4) . . . . ? O2 N11 C44 C45 -156.9(3) . . . . ? O3 N11 C44 C43 -154.9(3) . . . . ? O2 N11 C44 C43 25.5(4) . . . . ? C43 C44 C45 C46 -1.0(5) . . . . ? N11 C44 C45 C46 -178.4(3) . . . . ? C44 C45 C46 C47 -2.5(5) . . . . ? C44 C45 C46 N12 176.9(3) . . . . ? O5 N12 C46 C47 -10.2(5) . . . . ? O4 N12 C46 C47 170.3(3) . . . . ? O5 N12 C46 C45 170.4(4) . . . . ? O4 N12 C46 C45 -9.1(5) . . . . ? C45 C46 C47 C48 1.4(5) . . . . ? N12 C46 C47 C48 -177.9(3) . . . . ? C46 C47 C48 C43 3.2(5) . . . . ? C46 C47 C48 N13 -177.7(3) . . . . ? O1 C43 C48 C47 169.9(3) . . . . ? C44 C43 C48 C47 -6.0(4) . . . . ? O1 C43 C48 N13 -9.2(4) . . . . ? C44 C43 C48 N13 174.9(3) . . . . ? O7 N13 C48 C47 156.3(3) . . . . ? O6 N13 C48 C47 -20.9(4) . . . . ? O7 N13 C48 C43 -24.5(4) . . . . ? O6 N13 C48 C43 158.2(3) . . . . ? O8 C49 C50 C51 174.2(3) . . . . ? C54 C49 C50 C51 -2.5(4) . . . . ? O8 C49 C50 N14 -6.9(4) . . . . ? C54 C49 C50 N14 176.4(2) . . . . ? O10 N14 C50 C51 -32.0(4) . . . . ? O9 N14 C50 C51 143.4(3) . . . . ? O10 N14 C50 C49 149.1(3) . . . . ? O9 N14 C50 C49 -35.6(4) . . . . ? C49 C50 C51 C52 0.4(5) . . . . ? N14 C50 C51 C52 -178.6(3) . . . . ? C50 C51 C52 C53 0.8(5) . . . . ? C50 C51 C52 N15 179.8(3) . . . . ? O11 N15 C52 C53 150.9(3) . . . . ? O12 N15 C52 C53 -28.5(4) . . . . ? O11 N15 C52 C51 -28.2(4) . . . . ? O12 N15 C52 C51 152.5(3) . . . . ? C51 C52 C53 C54 0.5(5) . . . . ? N15 C52 C53 C54 -178.5(3) . . . . ? C52 C53 C54 C49 -3.1(5) . . . . ? C52 C53 C54 N16 176.3(3) . . . . ? O8 C49 C54 C53 -172.8(3) . . . . ? C50 C49 C54 C53 3.9(4) . . . . ? O8 C49 C54 N16 7.8(4) . . . . ? C50 C49 C54 N16 -175.5(2) . . . . ? O14 N16 C54 C53 -149.2(3) . . . . ? O13 N16 C54 C53 28.9(4) . . . . ? O14 N16 C54 C49 30.3(4) . . . . ? O13 N16 C54 C49 -151.7(3) . . . . ? O15 C55 C56 C57 173.3(3) . . . . ? C60 C55 C56 C57 -2.6(4) . . . . ? O15 C55 C56 N17 -5.3(5) . . . . ? C60 C55 C56 N17 178.7(3) . . . . ? O16 N17 C56 C57 142.8(3) . . . . ? O17 N17 C56 C57 -36.1(4) . . . . ? O16 N17 C56 C55 -38.5(4) . . . . ? O17 N17 C56 C55 142.6(3) . . . . ? C55 C56 C57 C58 1.2(5) . . . . ? N17 C56 C57 C58 179.9(3) . . . . ? C56 C57 C58 C59 0.8(5) . . . . ? C56 C57 C58 N18 -179.0(3) . . . . ? O19 N18 C58 C57 167.2(3) . . . . ? O18 N18 C58 C57 -12.1(4) . . . . ? O19 N18 C58 C59 -12.6(4) . . . . ? O18 N18 C58 C59 168.2(3) . . . . ? C57 C58 C59 C60 -1.1(5) . . . . ? N18 C58 C59 C60 178.7(3) . . . . ? C58 C59 C60 C55 -0.6(5) . . . . ? C58 C59 C60 N19 -179.4(3) . . . . ? O15 C55 C60 C59 -173.6(3) . . . . ? C56 C55 C60 C59 2.3(4) . . . . ? O15 C55 C60 N19 5.2(5) . . . . ? C56 C55 C60 N19 -178.9(3) . . . . ? O20 N19 C60 C59 27.2(4) . . . . ? O21 N19 C60 C59 -151.8(3) . . . . ? O20 N19 C60 C55 -151.7(3) . . . . ? O21 N19 C60 C55 29.3(4) . . . . ? C48 C43 O1 Eu1 -125(3) . . . . ? C44 C43 O1 Eu1 50(3) . . . . ? O15 Eu1 O1 C43 14(3) . . . . ? O8 Eu1 O1 C43 -84(3) . . . . ? N8 Eu1 O1 C43 -91(3) . . . . ? N5 Eu1 O1 C43 90(3) . . . . ? N2 Eu1 O1 C43 -169(3) . . . . ? N1 Eu1 O1 C43 143(3) . . . . ? C54 C49 O8 Eu1 -65.0(19) . . . . ? C50 C49 O8 Eu1 118.6(17) . . . . ? O1 Eu1 O8 C49 126.8(18) . . . . ? O15 Eu1 O8 C49 27.5(18) . . . . ? N8 Eu1 O8 C49 -53.8(18) . . . . ? N5 Eu1 O8 C49 38(2) . . . . ? N2 Eu1 O8 C49 -157.1(18) . . . . ? N1 Eu1 O8 C49 -101.2(18) . . . . ? C60 C55 O15 Eu1 -16(9) . . . . ? C56 C55 O15 Eu1 169(8) . . . . ? O1 Eu1 O15 C55 -14(8) . . . . ? O8 Eu1 O15 C55 85(8) . . . . ? N8 Eu1 O15 C55 161(8) . . . . ? N5 Eu1 O15 C55 -94(8) . . . . ? N2 Eu1 O15 C55 -46(9) . . . . ? N1 Eu1 O15 C55 -144(8) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.833 _refine_diff_density_min -0.746 _refine_diff_density_rms 0.087 #===============================# data_3 _database_code_depnum_ccdc_archive 'CCDC 867186' #TrackingRef 'Compounds.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H16.33 Eu0.50 N5.83 O5.17' _chemical_formula_weight 449.00 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -8.9294 11.1857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M P31c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, z+1/2' 'x-y, -y, z+1/2' '-x, -x+y, z+1/2' _cell_length_a 19.5543(4) _cell_length_b 19.5543(4) _cell_length_c 8.4847(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2809.65(13) _cell_formula_units_Z 6 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5696 _cell_measurement_theta_min 2.6071 _cell_measurement_theta_max 62.4500 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.592 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1356 _exptl_absorpt_coefficient_mu 12.606 _exptl_absorpt_correction_T_min 0.2911 _exptl_absorpt_correction_T_max 0.3654 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9628 _diffrn_reflns_av_R_equivalents 0.0423 _diffrn_reflns_av_sigmaI/netI 0.0496 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 4.52 _diffrn_reflns_theta_max 62.54 _reflns_number_total 2648 _reflns_number_gt 2490 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. Due to the poor crystal data quality, the restrained refinement was applied which causes relatively high R values. All C, N and O atoms are refined with ISOR/SIMU combination to simulate isotropically to give 168/180 restraints. The inorganic moiety [Eu(NO~3~)~3~(H~2~O)~4~] shows disorder over two half positions, of which the nitrate anions are modeled to resembling those on the coordination moiety by SAME/SADI (6 restraints), DFIX (1 restraints), and FLAT (1 restraints). ; _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^)+(0.0610P)^2^+100.0000P] 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 0.314(14) _refine_ls_number_reflns 2648 _refine_ls_number_parameters 249 _refine_ls_number_restraints 357 _refine_ls_R_factor_all 0.1286 _refine_ls_R_factor_gt 0.1237 _refine_ls_wR_factor_ref 0.2821 _refine_ls_wR_factor_gt 0.2792 _refine_ls_goodness_of_fit_ref 1.103 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.032 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Eu1 Eu 0.6667 0.3333 -0.2344(3) 0.0250(2) Uani 1 3 d S . . Eu2 Eu 0.0000 0.0000 0.7742(11) 0.0958(13) Uani 0.50 3 d SP . . C1 C 0.5872(8) 0.2758(10) 0.1552(19) 0.061(4) Uani 1 1 d U . . H1A H 0.5839 0.2243 0.1745 0.073 Uiso 1 1 calc R . . H1B H 0.5814 0.2969 0.2574 0.073 Uiso 1 1 calc R . . C2 C 0.5239(7) 0.2655(8) 0.0466(17) 0.048(3) Uani 1 1 d U . . C3 C 0.4632(4) 0.2795(5) -0.1475(11) 0.067(4) Uani 1 1 d GU . . C4 C 0.4395(6) 0.2954(7) -0.2907(11) 0.082(5) Uani 1 1 d GU . . H4A H 0.4763 0.3179 -0.3747 0.099 Uiso 1 1 calc R . . C5 C 0.3620(6) 0.2783(8) -0.3110(13) 0.077(4) Uani 1 1 d GU . . H5A H 0.3458 0.2892 -0.4089 0.092 Uiso 1 1 calc R . . C6 C 0.3082(5) 0.2453(7) -0.1881(16) 0.079(4) Uani 1 1 d GU . . H6A H 0.2552 0.2337 -0.2019 0.095 Uiso 1 1 calc R . . C7 C 0.3319(5) 0.2295(7) -0.0448(15) 0.076(4) Uani 1 1 d GU . . H7A H 0.2952 0.2069 0.0392 0.091 Uiso 1 1 calc R . . C8 C 0.4095(5) 0.2466(6) -0.0246(11) 0.070(4) Uani 1 1 d GU . . C9 C 0.4132(6) 0.2080(10) 0.252(2) 0.053(3) Uani 1 1 d U . . H9A H 0.3836 0.2358 0.2720 0.064 Uiso 1 1 calc R . . H9B H 0.4541 0.2226 0.3342 0.064 Uiso 1 1 calc R . . C10 C 0.3594(6) 0.1210(6) 0.2457(14) 0.077(4) Uani 1 1 d GU . . C11 C 0.2863(7) 0.0959(8) 0.3152(18) 0.127(5) Uani 1 1 d GU . . H11A H 0.2733 0.1336 0.3537 0.152 Uiso 1 1 calc R . . N4 N 0.2322(7) 0.0157(9) 0.328(2) 0.138(5) Uani 1 1 d GU . . C12 C 0.2512(10) -0.0394(6) 0.272(2) 0.126(5) Uani 1 1 d GU . . H12A H 0.2142 -0.0942 0.2809 0.151 Uiso 1 1 calc R . . C13 C 0.3244(11) -0.0144(7) 0.202(2) 0.130(5) Uani 1 1 d GU . . H13A H 0.3374 -0.0521 0.1639 0.156 Uiso 1 1 calc R . . C14 C 0.3785(8) 0.0658(8) 0.1894(18) 0.110(5) Uani 1 1 d GU . . H14A H 0.4285 0.0829 0.1419 0.133 Uiso 1 1 calc R . . N1 N 0.6667 0.3333 0.0807(19) 0.025(3) Uani 1 3 d SU . . N2 N 0.5365(6) 0.2943(7) -0.0956(16) 0.059(3) Uani 1 1 d U . . N3 N 0.4483(7) 0.2258(8) 0.0946(14) 0.062(3) Uani 1 1 d U . . C15 C 0.5660(12) 0.0545(13) -0.648(3) 0.098(5) Uani 1 1 d U . . C16 C 0.5138(12) -0.0146(12) -0.592(3) 0.099(5) Uani 1 1 d U . . H16A H 0.4793 -0.0082 -0.5172 0.149 Uiso 1 1 calc R . . H16B H 0.5410 -0.0386 -0.5383 0.149 Uiso 1 1 calc R . . H16C H 0.4821 -0.0488 -0.6789 0.149 Uiso 1 1 calc R . . N7 N 0.6051(8) 0.1084(9) -0.727(2) 0.085(4) Uani 1 1 d U . . N5 N 0.5429(6) 0.1966(5) -0.4098(12) 0.071(3) Uani 1 1 d DU . . O1 O 0.5687(5) 0.2788(4) -0.4515(10) 0.044(2) Uani 1 1 d DU . . O2 O 0.5654(6) 0.1862(6) -0.2705(12) 0.076(3) Uani 1 1 d DU . . O3 O 0.4928(7) 0.1458(7) -0.4948(15) 0.101(4) Uani 1 1 d DU . . N6 N 0.1234(7) 0.1183(7) 0.5558(16) 0.133(5) Uani 0.50 1 d PDU A 1 O4 O 0.1059(13) 0.1443(13) 0.704(2) 0.138(7) Uani 0.50 1 d PDU A 1 O5 O 0.1046(4) 0.0440(8) 0.552(3) 0.155(7) Uani 0.50 1 d PDU A 1 O6 O 0.1551(14) 0.1690(11) 0.455(2) 0.136(7) Uani 0.50 1 d PDU A 1 O7 O -0.0190(13) 0.0889(13) 0.926(3) 0.078(7) Uani 0.50 1 d PU A 1 O8 O 0.0000 0.0000 1.078(3) 0.025 Uiso 0.50 3 d SP . 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu1 0.0263(2) 0.0263(2) 0.0225(4) 0.000 0.000 0.01314(12) Eu2 0.0659(11) 0.0659(11) 0.156(4) 0.000 0.000 0.0329(6) C1 0.043(5) 0.075(6) 0.054(6) 0.001(5) 0.010(5) 0.020(4) C2 0.031(4) 0.063(5) 0.051(5) -0.001(4) 0.009(4) 0.024(3) C3 0.059(5) 0.068(5) 0.060(6) 0.001(5) 0.008(5) 0.021(4) C4 0.066(6) 0.079(6) 0.069(6) 0.013(6) -0.010(6) 0.011(5) C5 0.063(6) 0.083(6) 0.071(7) -0.004(6) -0.007(6) 0.027(5) C6 0.076(6) 0.079(6) 0.089(7) -0.012(6) -0.005(6) 0.045(5) C7 0.070(5) 0.086(6) 0.083(7) -0.012(6) 0.002(6) 0.048(4) C8 0.065(5) 0.073(5) 0.073(6) 0.007(5) 0.002(5) 0.034(4) C9 0.050(4) 0.067(4) 0.059(6) 0.011(4) 0.018(5) 0.042(4) C10 0.070(5) 0.083(5) 0.093(6) 0.003(5) 0.010(5) 0.049(4) C11 0.110(7) 0.113(7) 0.132(7) 0.009(7) 0.015(7) 0.037(6) N4 0.120(7) 0.122(7) 0.146(7) 0.019(7) 0.013(7) 0.040(6) C12 0.118(7) 0.114(7) 0.134(8) -0.002(7) 0.020(7) 0.049(6) C13 0.124(7) 0.119(7) 0.143(8) 0.003(7) 0.005(7) 0.058(6) C14 0.106(7) 0.095(7) 0.127(7) -0.002(7) 0.007(7) 0.048(5) N1 0.021(4) 0.021(4) 0.034(7) 0.000 0.000 0.0106(18) N2 0.041(4) 0.074(5) 0.063(6) 0.002(5) -0.005(4) 0.029(4) N3 0.048(4) 0.075(5) 0.046(5) 0.007(4) 0.011(4) 0.017(4) C15 0.097(7) 0.092(6) 0.099(7) 0.006(6) 0.000(6) 0.042(5) C16 0.101(8) 0.091(7) 0.100(8) 0.016(7) -0.012(7) 0.044(6) N7 0.075(6) 0.085(6) 0.106(8) 0.003(6) 0.009(6) 0.049(4) N5 0.061(4) 0.071(5) 0.081(5) -0.012(5) 0.017(4) 0.034(4) O1 0.043(4) 0.047(4) 0.034(4) -0.008(3) 0.008(3) 0.016(3) O2 0.065(5) 0.052(4) 0.103(7) 0.003(5) 0.001(5) 0.022(4) O3 0.103(6) 0.079(6) 0.100(7) -0.008(6) -0.002(6) 0.030(5) N6 0.129(7) 0.139(7) 0.138(7) 0.011(6) 0.001(6) 0.072(5) O4 0.127(9) 0.145(9) 0.134(10) 0.007(8) -0.001(8) 0.063(7) O5 0.147(9) 0.159(9) 0.146(10) 0.007(9) 0.007(9) 0.065(7) O6 0.133(9) 0.141(9) 0.147(10) 0.020(8) -0.006(8) 0.077(7) O7 0.076(9) 0.058(8) 0.096(11) 0.005(9) 0.006(9) 0.031(7) _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 2.482(8) 2_655 ? Eu1 O1 2.482(8) . ? Eu1 O1 2.482(8) 3_665 ? Eu1 N2 2.551(12) 2_655 ? Eu1 N2 2.551(12) 3_665 ? Eu1 N2 2.551(12) . ? Eu1 O2 2.568(9) 2_655 ? Eu1 O2 2.568(9) . ? Eu1 O2 2.568(9) 3_665 ? Eu1 N1 2.674(16) . ? Eu1 N5 2.958(9) 2_655 ? Eu1 N5 2.958(9) . ? Eu2 O7 2.34(3) 3 ? Eu2 O7 2.34(3) . ? Eu2 O7 2.34(3) 2 ? Eu2 O8 2.57(3) . ? Eu2 O5 2.59(2) 3 ? Eu2 O5 2.59(2) 2 ? Eu2 O5 2.59(2) . ? Eu2 O4 2.60(2) 2 ? Eu2 O4 2.60(2) . ? Eu2 O4 2.60(2) 3 ? C1 C2 1.47(2) . ? C1 N1 1.527(15) . ? C2 N2 1.301(19) . ? C2 N3 1.344(16) . ? C3 N2 1.383(14) . ? C3 C4 1.3900 . ? C3 C8 1.3900 . ? C4 C5 1.3900 . ? C5 C6 1.3900 . ? C6 C7 1.3900 . ? C7 C8 1.3900 . ? C8 N3 1.440(17) . ? C9 N3 1.46(2) . ? C9 C10 1.488(19) . ? C10 C11 1.3900 . ? C10 C14 1.3900 . ? C11 N4 1.3900 . ? N4 C12 1.3900 . ? C12 C13 1.3900 . ? C13 C14 1.3900 . ? N1 C1 1.527(15) 2_655 ? N1 C1 1.527(15) 3_665 ? C15 N7 1.16(2) . ? C15 C16 1.31(3) . ? N5 O3 1.222(13) . ? N5 O2 1.312(14) . ? N5 O1 1.467(12) . ? N6 O6 1.220(17) . ? N6 O5 1.310(17) . ? N6 O4 1.458(18) . ? O5 O7 1.54(3) 4_554 ? O5 O8 1.792(8) 4_554 ? O5 Eu2 2.95(2) 4_554 ? O7 O5 1.54(3) 4 ? O8 Eu2 1.67(3) 4 ? O8 O5 1.792(9) 4 ? O8 O5 1.792(8) 5 ? O8 O5 1.792(9) 6 ? 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 O1 70.9(3) 2_655 . ? O1 Eu1 O1 70.9(3) 2_655 3_665 ? O1 Eu1 O1 70.9(3) . 3_665 ? O1 Eu1 N2 76.9(3) 2_655 2_655 ? O1 Eu1 N2 118.6(4) . 2_655 ? O1 Eu1 N2 140.8(3) 3_665 2_655 ? O1 Eu1 N2 118.6(4) 2_655 3_665 ? O1 Eu1 N2 140.8(3) . 3_665 ? O1 Eu1 N2 76.9(3) 3_665 3_665 ? N2 Eu1 N2 100.4(4) 2_655 3_665 ? O1 Eu1 N2 140.8(3) 2_655 . ? O1 Eu1 N2 76.9(3) . . ? O1 Eu1 N2 118.6(4) 3_665 . ? N2 Eu1 N2 100.4(4) 2_655 . ? N2 Eu1 N2 100.4(4) 3_665 . ? O1 Eu1 O2 55.4(3) 2_655 2_655 ? O1 Eu1 O2 123.4(3) . 2_655 ? O1 Eu1 O2 75.6(3) 3_665 2_655 ? N2 Eu1 O2 67.9(4) 2_655 2_655 ? N2 Eu1 O2 66.8(4) 3_665 2_655 ? N2 Eu1 O2 159.4(4) . 2_655 ? O1 Eu1 O2 75.6(3) 2_655 . ? O1 Eu1 O2 55.4(3) . . ? O1 Eu1 O2 123.4(3) 3_665 . ? N2 Eu1 O2 66.8(4) 2_655 . ? N2 Eu1 O2 159.4(4) 3_665 . ? N2 Eu1 O2 67.9(4) . . ? O2 Eu1 O2 118.60(10) 2_655 . ? O1 Eu1 O2 123.4(3) 2_655 3_665 ? O1 Eu1 O2 75.6(3) . 3_665 ? O1 Eu1 O2 55.4(3) 3_665 3_665 ? N2 Eu1 O2 159.4(4) 2_655 3_665 ? N2 Eu1 O2 67.9(4) 3_665 3_665 ? N2 Eu1 O2 66.8(4) . 3_665 ? O2 Eu1 O2 118.60(10) 2_655 3_665 ? O2 Eu1 O2 118.60(10) . 3_665 ? O1 Eu1 N1 137.93(18) 2_655 . ? O1 Eu1 N1 137.93(18) . . ? O1 Eu1 N1 137.93(18) 3_665 . ? N2 Eu1 N1 62.5(3) 2_655 . ? N2 Eu1 N1 62.5(3) 3_665 . ? N2 Eu1 N1 62.5(3) . . ? O2 Eu1 N1 96.9(2) 2_655 . ? O2 Eu1 N1 96.9(2) . . ? O2 Eu1 N1 96.9(2) 3_665 . ? O1 Eu1 N5 29.7(3) 2_655 2_655 ? O1 Eu1 N5 97.7(3) . 2_655 ? O1 Eu1 N5 67.3(3) 3_665 2_655 ? N2 Eu1 N5 73.6(4) 2_655 2_655 ? N2 Eu1 N5 89.8(4) 3_665 2_655 ? N2 Eu1 N5 169.1(4) . 2_655 ? O2 Eu1 N5 26.3(3) 2_655 2_655 ? O2 Eu1 N5 101.2(4) . 2_655 ? O2 Eu1 N5 121.5(3) 3_665 2_655 ? N1 Eu1 N5 120.21(19) . 2_655 ? O1 Eu1 N5 67.3(3) 2_655 . ? O1 Eu1 N5 29.7(3) . . ? O1 Eu1 N5 97.7(3) 3_665 . ? N2 Eu1 N5 89.8(4) 2_655 . ? N2 Eu1 N5 169.1(4) 3_665 . ? N2 Eu1 N5 73.6(4) . . ? O2 Eu1 N5 121.5(3) 2_655 . ? O2 Eu1 N5 26.3(3) . . ? O2 Eu1 N5 101.2(4) 3_665 . ? N1 Eu1 N5 120.21(19) . . ? N5 Eu1 N5 96.9(3) 2_655 . ? O8 Eu2 O7 123.5(7) 4_554 3 ? O8 Eu2 O7 123.5(7) 4_554 . ? O7 Eu2 O7 92.5(10) 3 . ? O8 Eu2 O7 123.5(7) 4_554 2 ? O7 Eu2 O7 92.5(10) 3 2 ? O7 Eu2 O7 92.5(10) . 2 ? O8 Eu2 O8 180.000(10) 4_554 . ? O7 Eu2 O8 56.5(7) 3 . ? O7 Eu2 O8 56.5(7) . . ? O7 Eu2 O8 56.5(7) 2 . ? O8 Eu2 O5 43.3(5) 4_554 3 ? O7 Eu2 O5 123.2(6) 3 3 ? O7 Eu2 O5 143.9(7) . 3 ? O7 Eu2 O5 81.3(8) 2 3 ? O8 Eu2 O5 136.7(5) . 3 ? O8 Eu2 O5 43.3(5) 4_554 2 ? O7 Eu2 O5 143.9(7) 3 2 ? O7 Eu2 O5 81.3(8) . 2 ? O7 Eu2 O5 123.2(6) 2 2 ? O8 Eu2 O5 136.7(5) . 2 ? O5 Eu2 O5 72.9(7) 3 2 ? O8 Eu2 O5 43.3(5) 4_554 . ? O7 Eu2 O5 81.3(8) 3 . ? O7 Eu2 O5 123.2(6) . . ? O7 Eu2 O5 143.9(7) 2 . ? O8 Eu2 O5 136.7(5) . . ? O5 Eu2 O5 72.9(7) 3 . ? O5 Eu2 O5 72.9(7) 2 . ? O8 Eu2 O4 76.7(4) 4_554 2 ? O7 Eu2 O4 159.2(9) 3 2 ? O7 Eu2 O4 77.8(8) . 2 ? O7 Eu2 O4 69.9(7) 2 2 ? O8 Eu2 O4 103.3(4) . 2 ? O5 Eu2 O4 66.6(7) 3 2 ? O5 Eu2 O4 53.5(5) 2 2 ? O5 Eu2 O4 119.4(7) . 2 ? O8 Eu2 O4 76.7(4) 4_554 . ? O7 Eu2 O4 77.8(8) 3 . ? O7 Eu2 O4 69.9(7) . . ? O7 Eu2 O4 159.2(9) 2 . ? O8 Eu2 O4 103.3(4) . . ? O5 Eu2 O4 119.4(7) 3 . ? O5 Eu2 O4 66.6(7) 2 . ? O5 Eu2 O4 53.5(5) . . ? O4 Eu2 O4 114.9(3) 2 . ? O8 Eu2 O4 76.7(4) 4_554 3 ? O7 Eu2 O4 69.9(7) 3 3 ? O7 Eu2 O4 159.2(9) . 3 ? O7 Eu2 O4 77.8(8) 2 3 ? O8 Eu2 O4 103.3(4) . 3 ? O5 Eu2 O4 53.5(5) 3 3 ? O5 Eu2 O4 119.4(7) 2 3 ? O5 Eu2 O4 66.6(7) . 3 ? O4 Eu2 O4 114.9(3) 2 3 ? O4 Eu2 O4 114.9(3) . 3 ? O8 Eu2 O5 142.9(4) 4_554 4 ? O7 Eu2 O5 61.5(7) 3 4 ? O7 Eu2 O5 31.2(7) . 4 ? O7 Eu2 O5 90.7(8) 2 4 ? O8 Eu2 O5 37.1(4) . 4 ? O5 Eu2 O5 170.8(7) 3 4 ? O5 Eu2 O5 108.2(4) 2 4 ? O5 Eu2 O5 116.3(4) . 4 ? O4 Eu2 O5 106.4(6) 2 4 ? O4 Eu2 O5 68.5(5) . 4 ? O4 Eu2 O5 129.4(6) 3 4 ? C2 C1 N1 108.5(12) . . ? N2 C2 N3 116.5(13) . . ? N2 C2 C1 123.8(11) . . ? N3 C2 C1 119.7(13) . . ? N2 C3 C4 131.1(7) . . ? N2 C3 C8 108.8(7) . . ? C4 C3 C8 120.0 . . ? C5 C4 C3 120.0 . . ? C4 C5 C6 120.0 . . ? C5 C6 C7 120.0 . . ? C6 C7 C8 120.0 . . ? C7 C8 C3 120.0 . . ? C7 C8 N3 133.2(7) . . ? C3 C8 N3 105.9(7) . . ? N3 C9 C10 102.8(14) . . ? C11 C10 C14 120.0 . . ? C11 C10 C9 113.8(10) . . ? C14 C10 C9 126.1(10) . . ? N4 C11 C10 120.0 . . ? C11 N4 C12 120.0 . . ? C13 C12 N4 120.0 . . ? C12 C13 C14 120.0 . . ? C13 C14 C10 120.0 . . ? C1 N1 C1 104.1(9) 2_655 . ? C1 N1 C1 104.1(9) 2_655 3_665 ? C1 N1 C1 104.1(9) . 3_665 ? C1 N1 Eu1 114.4(8) 2_655 . ? C1 N1 Eu1 114.4(8) . . ? C1 N1 Eu1 114.4(8) 3_665 . ? C2 N2 C3 104.7(10) . . ? C2 N2 Eu1 120.1(10) . . ? C3 N2 Eu1 133.6(9) . . ? C2 N3 C8 102.0(11) . . ? C2 N3 C9 131.7(12) . . ? C8 N3 C9 117.2(12) . . ? N7 C15 C16 166(3) . . ? O3 N5 O2 126.9(10) . . ? O3 N5 O1 116.4(11) . . ? O2 N5 O1 115.4(8) . . ? O3 N5 Eu1 173.1(9) . . ? O2 N5 Eu1 60.0(5) . . ? O1 N5 Eu1 56.9(4) . . ? N5 O1 Eu1 93.4(6) . . ? N5 O2 Eu1 93.7(6) . . ? O6 N6 O5 129.1(19) . . ? O6 N6 O4 115.7(16) . . ? O5 N6 O4 115.1(16) . . ? O6 N6 Eu2 161.0(15) . . ? O5 N6 Eu2 59.3(10) . . ? O4 N6 Eu2 60.0(9) . . ? N6 O4 Eu2 91.0(10) . . ? N6 O5 O7 138(2) . 4_554 ? N6 O5 O8 98.6(9) . 4_554 ? O7 O5 O8 88.7(12) 4_554 4_554 ? N6 O5 Eu2 95.0(12) . . ? O7 O5 Eu2 115.5(10) 4_554 . ? O8 O5 Eu2 39.7(9) 4_554 . ? N6 O5 Eu2 96.5(12) . 4_554 ? O7 O5 Eu2 51.8(12) 4_554 4_554 ? O8 O5 Eu2 60.0(10) 4_554 4_554 ? Eu2 O5 Eu2 99.6(2) . 4_554 ? O5 O7 Eu2 97.0(15) 4 . ? Eu2 O8 O5 97.0(12) 4 4 ? Eu2 O8 O5 97.0(12) 4 5 ? O5 O8 O5 118.5(5) 4 5 ? Eu2 O8 O5 97.0(12) 4 6 ? O5 O8 O5 118.5(5) 4 6 ? O5 O8 O5 118.5(5) 5 6 ? Eu2 O8 Eu2 180.000(6) 4 . ? O5 O8 Eu2 83.0(12) 4 . ? O5 O8 Eu2 83.0(12) 5 . ? O5 O8 Eu2 83.0(12) 6 . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 62.54 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 2.674 _refine_diff_density_min -1.271 _refine_diff_density_rms 0.215 #===============================# data_6 _database_code_depnum_ccdc_archive 'CCDC 867187' #TrackingRef 'Compounds.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H52 N19 O21.50 Tb2' _chemical_formula_weight 1556.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -9.1472 9.1891 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 17.3754(7) _cell_length_b 17.3754(7) _cell_length_c 39.4344(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 10310.4(8) _cell_formula_units_Z 6 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.505 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4650 _exptl_absorpt_coefficient_mu 10.683 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.0999 _exptl_absorpt_correction_T_max 0.1418 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10639 _diffrn_reflns_av_R_equivalents 0.0744 _diffrn_reflns_av_sigmaI/netI 0.0676 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_theta_min 5.09 _diffrn_reflns_theta_max 62.46 _reflns_number_total 3566 _reflns_number_gt 2692 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1000P)^2^+120.0000P] 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 3566 _refine_ls_number_parameters 272 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0948 _refine_ls_R_factor_gt 0.0732 _refine_ls_wR_factor_ref 0.1936 _refine_ls_wR_factor_gt 0.1825 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.087 _refine_ls_shift/su_max 0.025 _refine_ls_shift/su_mean 0.003 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tb1 Tb 0.0000 0.0000 0.126319(13) 0.02585(14) Uani 1 3 d S . . Tb2 Tb 0.3333 0.6667 0.000364(18) 0.0549(2) Uani 1 3 d S . . N1 N 0.0000 0.0000 0.19538(19) 0.0285(19) Uani 1 3 d S . . N2 N 0.1459(3) 0.0347(3) 0.15548(11) 0.0278(11) Uani 1 1 d . . . N3 N 0.2343(3) 0.0639(3) 0.20062(12) 0.0333(13) Uani 1 1 d . . . N4 N 0.2337(5) -0.1634(5) 0.2818(2) 0.092(3) Uani 1 1 d . . . N5 N 0.1439(3) 0.1381(4) 0.08732(12) 0.0405(14) Uani 1 1 d . . . N6 N 0.1842(4) 0.6439(4) -0.03795(16) 0.0669(19) Uani 1 1 d . . . C1 C 0.0896(3) 0.0611(4) 0.20865(13) 0.0319(14) Uani 1 1 d . . . H1A H 0.1015 0.1230 0.2076 0.038 Uiso 1 1 calc R . . H1B H 0.0937 0.0465 0.2326 0.038 Uiso 1 1 calc R . . C2 C 0.1557(3) 0.0525(3) 0.18817(14) 0.0297(14) Uani 1 1 d . . . C3 C 0.2232(3) 0.0367(4) 0.14531(14) 0.0312(15) Uani 1 1 d . . . C4 C 0.2504(4) 0.0215(4) 0.11360(16) 0.0400(16) Uani 1 1 d . . . H4A H 0.2130 0.0072 0.0943 0.048 Uiso 1 1 calc R . . C5 C 0.3319(4) 0.0279(4) 0.11127(19) 0.0490(19) Uani 1 1 d . . . H5A H 0.3520 0.0200 0.0899 0.059 Uiso 1 1 calc R . . C6 C 0.3871(4) 0.0461(4) 0.1402(2) 0.052(2) Uani 1 1 d . . . H6A H 0.4422 0.0475 0.1381 0.062 Uiso 1 1 calc R . . C7 C 0.3616(4) 0.0616(4) 0.17129(19) 0.0456(18) Uani 1 1 d . . . H7A H 0.3992 0.0762 0.1905 0.055 Uiso 1 1 calc R . . C8 C 0.2797(3) 0.0551(3) 0.17343(15) 0.0331(15) Uani 1 1 d . . . C9 C 0.2629(4) 0.0729(4) 0.23614(16) 0.0470(19) Uani 1 1 d . . . H9A H 0.2291 0.0939 0.2497 0.056 Uiso 1 1 calc R . . H9B H 0.3266 0.1186 0.2376 0.056 Uiso 1 1 calc R . . C10 C 0.2500(4) -0.0125(5) 0.25136(17) 0.050(2) Uani 1 1 d . . . C11 C 0.2635(6) -0.0152(6) 0.2863(2) 0.074(3) Uani 1 1 d . . . H11A H 0.2767 0.0346 0.3002 0.089 Uiso 1 1 calc R . . C12 C 0.2576(6) -0.0899(6) 0.3002(2) 0.083(3) Uani 1 1 d . . . H12A H 0.2708 -0.0899 0.3235 0.099 Uiso 1 1 calc R . . C13 C 0.2189(5) -0.1631(6) 0.2489(2) 0.074(3) Uani 1 1 d . . . H13A H 0.2029 -0.2150 0.2360 0.089 Uiso 1 1 calc R . . C14 C 0.2261(5) -0.0893(5) 0.2331(2) 0.061(2) Uani 1 1 d . . . H14A H 0.2145 -0.0911 0.2095 0.073 Uiso 1 1 calc R . . O1 O 0.1144(2) 0.1577(3) 0.11361(10) 0.0382(11) Uani 1 1 d . . . O2 O 0.1083(3) 0.0580(3) 0.07966(10) 0.0429(12) Uani 1 1 d . . . O3 O 0.2052(3) 0.1974(4) 0.07118(12) 0.0651(17) Uani 1 1 d . . . O4 O 0.2237(3) 0.6026(4) -0.04590(13) 0.0662(16) Uani 1 1 d . . . O5 O 0.2061(3) 0.6901(4) -0.01248(15) 0.0723(18) Uani 1 1 d . . . O6 O 0.1201(4) 0.6361(5) -0.05582(17) 0.099(2) Uani 1 1 d . . . O1W O 0.3494(5) 0.7862(5) 0.0334(2) 0.134(3) Uani 1 1 d . . . O2W O 0.3333 0.6667 0.2234(17) 0.13(2) Uiso 0.25 3 d SP A 1 O3W O 0.3333 0.6667 0.1867(13) 0.108(17) Uiso 0.25 3 d SP . 2 N7 N 0.2370(11) 0.7985(13) 0.1659(4) 0.114(6) Uiso 0.50 1 d PD . . C15 C 0.2070(11) 0.7941(11) 0.1370(3) 0.074(5) Uiso 0.50 1 d PD . . C16 C 0.1993(11) 0.7869(11) 0.1014(3) 0.075(5) Uiso 0.50 1 d PD . . H16A H 0.1463 0.7890 0.0942 0.112 Uiso 0.50 1 calc PR . . H16B H 0.1940 0.7305 0.0942 0.112 Uiso 0.50 1 calc PR . . H16C H 0.2521 0.8363 0.0910 0.112 Uiso 0.50 1 calc PR . . N8 N 0.2463(12) -0.0966(10) 0.0309(6) 0.126(7) Uiso 0.50 1 d PD . . C17 C 0.2367(14) -0.0304(10) 0.0238(7) 0.125(9) Uiso 0.50 1 d PD . . C18 C 0.2680(13) 0.0602(10) 0.0159(6) 0.097(7) Uiso 0.50 1 d PD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tb1 0.03246(19) 0.03246(19) 0.0126(2) 0.000 0.000 0.01623(10) Tb2 0.0643(3) 0.0643(3) 0.0360(4) 0.000 0.000 0.03217(15) N1 0.029(3) 0.029(3) 0.028(4) 0.000 0.000 0.0145(13) N2 0.0244(18) 0.042(2) 0.022(2) 0.0005(17) -0.0032(17) 0.0202(16) N3 0.036(2) 0.032(2) 0.029(2) 0.0018(19) -0.002(2) 0.0145(18) N4 0.084(4) 0.079(4) 0.100(6) 0.040(4) -0.007(4) 0.030(4) N5 0.029(2) 0.062(3) 0.029(2) 0.013(2) 0.005(2) 0.023(2) N6 0.089(4) 0.079(4) 0.048(4) 0.000(3) 0.003(3) 0.054(3) C1 0.036(2) 0.044(3) 0.017(3) -0.008(2) -0.004(2) 0.021(2) C2 0.029(2) 0.025(2) 0.029(3) 0.004(2) -0.008(2) 0.009(2) C3 0.030(2) 0.031(3) 0.028(3) 0.001(2) -0.001(2) 0.012(2) C4 0.044(3) 0.041(3) 0.037(3) 0.006(2) 0.008(3) 0.023(2) C5 0.041(3) 0.050(3) 0.057(4) 0.004(3) 0.018(3) 0.023(3) C6 0.033(3) 0.047(3) 0.081(5) 0.016(3) 0.013(3) 0.024(2) C7 0.032(3) 0.040(3) 0.062(4) 0.004(3) -0.003(3) 0.015(2) C8 0.030(2) 0.027(2) 0.044(3) 0.006(2) 0.002(2) 0.015(2) C9 0.041(3) 0.050(3) 0.043(4) -0.007(3) -0.018(3) 0.018(3) C10 0.047(3) 0.060(4) 0.040(4) 0.010(3) -0.007(3) 0.024(3) C11 0.075(5) 0.079(5) 0.056(5) 0.013(4) -0.001(4) 0.029(4) C12 0.091(6) 0.073(5) 0.065(5) 0.027(4) -0.014(5) 0.027(4) C13 0.077(5) 0.066(4) 0.072(5) 0.020(4) -0.012(4) 0.030(4) C14 0.071(4) 0.050(4) 0.064(5) 0.000(3) -0.014(4) 0.032(3) O1 0.0355(18) 0.0387(19) 0.036(2) 0.0102(17) 0.0006(17) 0.0154(15) O2 0.046(2) 0.061(2) 0.0220(19) 0.0114(17) 0.0126(17) 0.0267(18) O3 0.044(2) 0.077(3) 0.054(3) 0.031(2) 0.022(2) 0.015(2) O4 0.073(3) 0.076(3) 0.051(3) -0.008(2) -0.006(2) 0.038(2) O5 0.065(3) 0.073(3) 0.070(4) -0.009(3) 0.001(3) 0.028(2) O6 0.093(3) 0.145(5) 0.086(4) 0.006(4) -0.017(3) 0.079(3) O1W 0.080(4) 0.158(5) 0.137(5) -0.105(4) -0.015(4) 0.040(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. Two CH~3~CN solvents molecules are disordered over two partial positions, One is modelled as the other with better geometry by SAME command to give 3 restraints. ; 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 O2 2.459(4) 3 ? Tb1 O2 2.459(4) 2 ? Tb1 O2 2.459(4) . ? Tb1 O1 2.503(4) 2 ? Tb1 O1 2.503(4) . ? Tb1 O1 2.503(4) 3 ? Tb1 N2 2.566(4) . ? Tb1 N2 2.566(4) 2 ? Tb1 N2 2.566(4) 3 ? Tb1 N1 2.723(8) . ? Tb1 N5 2.894(4) 2 ? Tb1 N5 2.894(4) 3 ? Tb2 O1W 2.348(7) . ? Tb2 O1W 2.348(7) 2_665 ? Tb2 O1W 2.348(7) 3_565 ? Tb2 O4 2.465(5) . ? Tb2 O4 2.465(5) 3_565 ? Tb2 O4 2.465(5) 2_665 ? Tb2 O5 2.492(6) . ? Tb2 O5 2.492(6) 3_565 ? Tb2 O5 2.492(6) 2_665 ? Tb2 N6 2.852(7) . ? Tb2 N6 2.852(7) 3_565 ? Tb2 N6 2.852(7) 2_665 ? N1 C1 1.474(6) . ? N1 C1 1.474(6) 2 ? N1 C1 1.474(6) 3 ? N2 C2 1.317(7) . ? N2 C3 1.385(7) . ? N3 C2 1.370(7) . ? N3 C8 1.383(8) . ? N3 C9 1.468(8) . ? N4 C13 1.321(11) . ? N4 C12 1.341(13) . ? N5 O3 1.226(6) . ? N5 O2 1.244(7) . ? N5 O1 1.275(7) . ? N6 O5 1.222(8) . ? N6 O4 1.257(9) . ? N6 O6 1.266(9) . ? C1 C2 1.471(8) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C3 C8 1.408(8) . ? C3 C4 1.408(8) . ? C4 C5 1.368(9) . ? C4 H4A 0.9500 . ? C5 C6 1.421(10) . ? C5 H5A 0.9500 . ? C6 C7 1.375(11) . ? C6 H6A 0.9500 . ? C7 C8 1.373(9) . ? C7 H7A 0.9500 . ? C9 C10 1.510(10) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C14 1.385(11) . ? C10 C11 1.404(11) . ? C11 C12 1.364(13) . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? C13 C14 1.374(12) . ? C13 H13A 0.9500 . ? C14 H14A 0.9500 . ? O3W O3W 1.58(10) 13_565 ? N7 C15 1.240(17) . ? C15 C16 1.410(16) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? N8 C17 1.27(2) . ? C17 C18 1.420(19) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Tb1 O2 70.14(15) 3 2 ? O2 Tb1 O2 70.14(15) 3 . ? O2 Tb1 O2 70.14(15) 2 . ? O2 Tb1 O1 72.76(15) 3 2 ? O2 Tb1 O1 51.32(14) 2 2 ? O2 Tb1 O1 118.16(14) . 2 ? O2 Tb1 O1 118.16(14) 3 . ? O2 Tb1 O1 72.76(15) 2 . ? O2 Tb1 O1 51.32(14) . . ? O1 Tb1 O1 116.09(6) 2 . ? O2 Tb1 O1 51.32(14) 3 3 ? O2 Tb1 O1 118.16(14) 2 3 ? O2 Tb1 O1 72.76(15) . 3 ? O1 Tb1 O1 116.09(6) 2 3 ? O1 Tb1 O1 116.09(6) . 3 ? O2 Tb1 N2 116.52(15) 3 . ? O2 Tb1 N2 141.66(14) 2 . ? O2 Tb1 N2 77.02(13) . . ? O1 Tb1 N2 164.78(13) 2 . ? O1 Tb1 N2 71.45(14) . . ? O1 Tb1 N2 67.83(15) 3 . ? O2 Tb1 N2 141.66(14) 3 2 ? O2 Tb1 N2 77.02(13) 2 2 ? O2 Tb1 N2 116.52(15) . 2 ? O1 Tb1 N2 71.45(14) 2 2 ? O1 Tb1 N2 67.83(15) . 2 ? O1 Tb1 N2 164.78(13) 3 2 ? N2 Tb1 N2 101.46(12) . 2 ? O2 Tb1 N2 77.01(14) 3 3 ? O2 Tb1 N2 116.52(15) 2 3 ? O2 Tb1 N2 141.66(14) . 3 ? O1 Tb1 N2 67.83(15) 2 3 ? O1 Tb1 N2 164.78(13) . 3 ? O1 Tb1 N2 71.45(14) 3 3 ? N2 Tb1 N2 101.46(12) . 3 ? N2 Tb1 N2 101.46(12) 2 3 ? O2 Tb1 N1 138.43(9) 3 . ? O2 Tb1 N1 138.43(9) 2 . ? O2 Tb1 N1 138.43(9) . . ? O1 Tb1 N1 101.55(9) 2 . ? O1 Tb1 N1 101.55(9) . . ? O1 Tb1 N1 101.55(9) 3 . ? N2 Tb1 N1 63.37(10) . . ? N2 Tb1 N1 63.37(10) 2 . ? N2 Tb1 N1 63.37(10) 3 . ? O2 Tb1 N5 69.24(15) 3 2 ? O2 Tb1 N5 25.25(15) 2 2 ? O2 Tb1 N5 93.79(15) . 2 ? O1 Tb1 N5 26.07(15) 2 2 ? O1 Tb1 N5 94.26(15) . 2 ? O1 Tb1 N5 120.31(15) 3 2 ? N2 Tb1 N5 165.69(15) . 2 ? N2 Tb1 N5 72.60(14) 2 2 ? N2 Tb1 N5 92.56(16) 3 2 ? N1 Tb1 N5 122.10(10) . 2 ? O2 Tb1 N5 25.25(15) 3 3 ? O2 Tb1 N5 93.79(15) 2 3 ? O2 Tb1 N5 69.24(15) . 3 ? O1 Tb1 N5 94.26(15) 2 3 ? O1 Tb1 N5 120.31(15) . 3 ? O1 Tb1 N5 26.07(15) 3 3 ? N2 Tb1 N5 92.56(16) . 3 ? N2 Tb1 N5 165.69(15) 2 3 ? N2 Tb1 N5 72.60(14) 3 3 ? N1 Tb1 N5 122.10(10) . 3 ? N5 Tb1 N5 94.38(13) 2 3 ? O1W Tb2 O1W 92.1(3) . 2_665 ? O1W Tb2 O1W 92.1(3) . 3_565 ? O1W Tb2 O1W 92.1(3) 2_665 3_565 ? O1W Tb2 O4 122.3(3) . . ? O1W Tb2 O4 82.9(2) 2_665 . ? O1W Tb2 O4 145.3(2) 3_565 . ? O1W Tb2 O4 82.9(2) . 3_565 ? O1W Tb2 O4 145.3(2) 2_665 3_565 ? O1W Tb2 O4 122.3(3) 3_565 3_565 ? O4 Tb2 O4 71.25(19) . 3_565 ? O1W Tb2 O4 145.3(2) . 2_665 ? O1W Tb2 O4 122.3(3) 2_665 2_665 ? O1W Tb2 O4 82.9(2) 3_565 2_665 ? O4 Tb2 O4 71.25(19) . 2_665 ? O4 Tb2 O4 71.25(19) 3_565 2_665 ? O1W Tb2 O5 72.0(2) . . ? O1W Tb2 O5 73.8(2) 2_665 . ? O1W Tb2 O5 158.0(3) 3_565 . ? O4 Tb2 O5 51.3(2) . . ? O4 Tb2 O5 72.02(19) 3_565 . ? O4 Tb2 O5 118.84(18) 2_665 . ? O1W Tb2 O5 73.8(2) . 3_565 ? O1W Tb2 O5 158.0(3) 2_665 3_565 ? O1W Tb2 O5 72.0(2) 3_565 3_565 ? O4 Tb2 O5 118.84(18) . 3_565 ? O4 Tb2 O5 51.3(2) 3_565 3_565 ? O4 Tb2 O5 72.02(19) 2_665 3_565 ? O5 Tb2 O5 115.98(9) . 3_565 ? O1W Tb2 O5 158.0(3) . 2_665 ? O1W Tb2 O5 72.0(2) 2_665 2_665 ? O1W Tb2 O5 73.8(2) 3_565 2_665 ? O4 Tb2 O5 72.02(19) . 2_665 ? O4 Tb2 O5 118.84(18) 3_565 2_665 ? O4 Tb2 O5 51.3(2) 2_665 2_665 ? O5 Tb2 O5 115.98(9) . 2_665 ? O5 Tb2 O5 115.98(9) 3_565 2_665 ? O1W Tb2 N6 96.6(3) . . ? O1W Tb2 N6 78.1(2) 2_665 . ? O1W Tb2 N6 167.1(2) 3_565 . ? O4 Tb2 N6 26.1(2) . . ? O4 Tb2 N6 68.49(19) 3_565 . ? O4 Tb2 N6 95.09(18) 2_665 . ? O5 Tb2 N6 25.30(19) . . ? O5 Tb2 N6 119.62(18) 3_565 . ? O5 Tb2 N6 94.98(19) 2_665 . ? O1W Tb2 N6 78.1(2) . 3_565 ? O1W Tb2 N6 167.1(2) 2_665 3_565 ? O1W Tb2 N6 96.6(3) 3_565 3_565 ? O4 Tb2 N6 95.09(18) . 3_565 ? O4 Tb2 N6 26.1(2) 3_565 3_565 ? O4 Tb2 N6 68.49(19) 2_665 3_565 ? O5 Tb2 N6 94.98(19) . 3_565 ? O5 Tb2 N6 25.30(19) 3_565 3_565 ? O5 Tb2 N6 119.62(18) 2_665 3_565 ? N6 Tb2 N6 94.53(18) . 3_565 ? O1W Tb2 N6 167.1(2) . 2_665 ? O1W Tb2 N6 96.6(3) 2_665 2_665 ? O1W Tb2 N6 78.1(2) 3_565 2_665 ? O4 Tb2 N6 68.49(19) . 2_665 ? O4 Tb2 N6 95.09(18) 3_565 2_665 ? O4 Tb2 N6 26.1(2) 2_665 2_665 ? O5 Tb2 N6 119.62(18) . 2_665 ? O5 Tb2 N6 94.98(19) 3_565 2_665 ? O5 Tb2 N6 25.30(19) 2_665 2_665 ? N6 Tb2 N6 94.53(18) . 2_665 ? N6 Tb2 N6 94.53(18) 3_565 2_665 ? C1 N1 C1 108.1(4) . 2 ? C1 N1 C1 108.1(4) . 3 ? C1 N1 C1 108.1(4) 2 3 ? C1 N1 Tb1 110.8(3) . . ? C1 N1 Tb1 110.8(3) 2 . ? C1 N1 Tb1 110.8(3) 3 . ? C2 N2 C3 105.5(4) . . ? C2 N2 Tb1 119.4(4) . . ? C3 N2 Tb1 135.0(3) . . ? C2 N3 C8 106.7(5) . . ? C2 N3 C9 128.2(5) . . ? C8 N3 C9 124.7(5) . . ? C13 N4 C12 119.6(8) . . ? O3 N5 O2 123.4(6) . . ? O3 N5 O1 119.6(5) . . ? O2 N5 O1 117.0(4) . . ? O3 N5 Tb1 179.1(5) . . ? O2 N5 Tb1 57.5(3) . . ? O1 N5 Tb1 59.6(2) . . ? O5 N6 O4 120.0(7) . . ? O5 N6 O6 119.8(8) . . ? O4 N6 O6 120.1(7) . . ? O5 N6 Tb2 60.6(4) . . ? O4 N6 Tb2 59.5(4) . . ? O6 N6 Tb2 177.7(5) . . ? C2 C1 N1 109.2(4) . . ? C2 C1 H1A 109.8 . . ? N1 C1 H1A 109.8 . . ? C2 C1 H1B 109.8 . . ? N1 C1 H1B 109.8 . . ? H1A C1 H1B 108.3 . . ? N2 C2 N3 112.8(5) . . ? N2 C2 C1 123.0(5) . . ? N3 C2 C1 124.1(5) . . ? N2 C3 C8 109.6(5) . . ? N2 C3 C4 131.6(5) . . ? C8 C3 C4 118.8(6) . . ? C5 C4 C3 118.4(6) . . ? C5 C4 H4A 120.8 . . ? C3 C4 H4A 120.8 . . ? C4 C5 C6 121.4(7) . . ? C4 C5 H5A 119.3 . . ? C6 C5 H5A 119.3 . . ? C7 C6 C5 120.8(6) . . ? C7 C6 H6A 119.6 . . ? C5 C6 H6A 119.6 . . ? C8 C7 C6 117.5(6) . . ? C8 C7 H7A 121.3 . . ? C6 C7 H7A 121.3 . . ? C7 C8 N3 131.5(6) . . ? C7 C8 C3 123.1(6) . . ? N3 C8 C3 105.4(5) . . ? N3 C9 C10 113.5(5) . . ? N3 C9 H9A 108.9 . . ? C10 C9 H9A 108.9 . . ? N3 C9 H9B 108.9 . . ? C10 C9 H9B 108.9 . . ? H9A C9 H9B 107.7 . . ? C14 C10 C11 117.0(7) . . ? C14 C10 C9 124.5(6) . . ? C11 C10 C9 118.5(7) . . ? C12 C11 C10 119.3(9) . . ? C12 C11 H11A 120.3 . . ? C10 C11 H11A 120.3 . . ? N4 C12 C11 122.1(8) . . ? N4 C12 H12A 119.0 . . ? C11 C12 H12A 119.0 . . ? N4 C13 C14 121.5(9) . . ? N4 C13 H13A 119.2 . . ? C14 C13 H13A 119.2 . . ? C13 C14 C10 120.4(8) . . ? C13 C14 H14A 119.8 . . ? C10 C14 H14A 119.8 . . ? N5 O1 Tb1 94.3(3) . . ? N5 O2 Tb1 97.3(3) . . ? N6 O4 Tb2 94.4(4) . . ? N6 O5 Tb2 94.1(5) . . ? N7 C15 C16 160(2) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N8 C17 C18 154(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Tb1 N1 C1 129.5(3) 3 . . . ? O2 Tb1 N1 C1 -110.5(3) 2 . . . ? O2 Tb1 N1 C1 9.5(3) . . . . ? O1 Tb1 N1 C1 -153.6(3) 2 . . . ? O1 Tb1 N1 C1 -33.6(3) . . . . ? O1 Tb1 N1 C1 86.4(3) 3 . . . ? N2 Tb1 N1 C1 28.7(3) . . . . ? N2 Tb1 N1 C1 -91.3(3) 2 . . . ? N2 Tb1 N1 C1 148.7(3) 3 . . . ? N5 Tb1 N1 C1 -136.1(3) 2 . . . ? N5 Tb1 N1 C1 103.9(3) 3 . . . ? O2 Tb1 N1 C1 -110.5(3) 3 . . 2 ? O2 Tb1 N1 C1 9.5(3) 2 . . 2 ? O2 Tb1 N1 C1 129.5(3) . . . 2 ? O1 Tb1 N1 C1 -33.6(3) 2 . . 2 ? O1 Tb1 N1 C1 86.4(3) . . . 2 ? O1 Tb1 N1 C1 -153.6(3) 3 . . 2 ? N2 Tb1 N1 C1 148.7(3) . . . 2 ? N2 Tb1 N1 C1 28.7(3) 2 . . 2 ? N2 Tb1 N1 C1 -91.3(3) 3 . . 2 ? N5 Tb1 N1 C1 -16.1(3) 2 . . 2 ? N5 Tb1 N1 C1 -136.1(3) 3 . . 2 ? O2 Tb1 N1 C1 9.5(3) 3 . . 3 ? O2 Tb1 N1 C1 129.5(3) 2 . . 3 ? O2 Tb1 N1 C1 -110.5(3) . . . 3 ? O1 Tb1 N1 C1 86.4(3) 2 . . 3 ? O1 Tb1 N1 C1 -153.6(3) . . . 3 ? O1 Tb1 N1 C1 -33.6(3) 3 . . 3 ? N2 Tb1 N1 C1 -91.3(3) . . . 3 ? N2 Tb1 N1 C1 148.7(3) 2 . . 3 ? N2 Tb1 N1 C1 28.7(3) 3 . . 3 ? N5 Tb1 N1 C1 103.9(3) 2 . . 3 ? N5 Tb1 N1 C1 -16.1(3) 3 . . 3 ? O2 Tb1 N2 C2 -146.2(4) 3 . . . ? O2 Tb1 N2 C2 122.7(4) 2 . . . ? O2 Tb1 N2 C2 154.1(4) . . . . ? O1 Tb1 N2 C2 -21.3(8) 2 . . . ? O1 Tb1 N2 C2 100.9(4) . . . . ? O1 Tb1 N2 C2 -129.5(4) 3 . . . ? N2 Tb1 N2 C2 39.2(4) 2 . . . ? N2 Tb1 N2 C2 -65.1(4) 3 . . . ? N1 Tb1 N2 C2 -13.0(4) . . . . ? N5 Tb1 N2 C2 103.1(6) 2 . . . ? N5 Tb1 N2 C2 -137.9(4) 3 . . . ? O2 Tb1 N2 C3 30.6(5) 3 . . . ? O2 Tb1 N2 C3 -60.5(6) 2 . . . ? O2 Tb1 N2 C3 -29.1(5) . . . . ? O1 Tb1 N2 C3 155.5(5) 2 . . . ? O1 Tb1 N2 C3 -82.3(5) . . . . ? O1 Tb1 N2 C3 47.3(5) 3 . . . ? N2 Tb1 N2 C3 -144.0(5) 2 . . . ? N2 Tb1 N2 C3 111.7(5) 3 . . . ? N1 Tb1 N2 C3 163.8(5) . . . . ? N5 Tb1 N2 C3 -80.1(8) 2 . . . ? N5 Tb1 N2 C3 38.9(5) 3 . . . ? O2 Tb1 N5 O3 -180(100) 3 . . . ? O2 Tb1 N5 O3 113(35) 2 . . . ? O2 Tb1 N5 O3 -160(100) . . . . ? O1 Tb1 N5 O3 108(35) 2 . . . ? O1 Tb1 N5 O3 20(35) . . . . ? O1 Tb1 N5 O3 -129(35) 3 . . . ? N2 Tb1 N5 O3 -63(35) . . . . ? N2 Tb1 N5 O3 38(35) 2 . . . ? N2 Tb1 N5 O3 -131(35) 3 . . . ? N1 Tb1 N5 O3 -22(35) . . . . ? N5 Tb1 N5 O3 111(35) 2 . . . ? N5 Tb1 N5 O3 -155(100) 3 . . . ? O2 Tb1 N5 O2 -20.2(4) 3 . . . ? O2 Tb1 N5 O2 -87.3(4) 2 . . . ? O1 Tb1 N5 O2 -92.4(4) 2 . . . ? O1 Tb1 N5 O2 179.7(5) . . . . ? O1 Tb1 N5 O2 31.3(3) 3 . . . ? N2 Tb1 N5 O2 96.5(4) . . . . ? N2 Tb1 N5 O2 -162.3(3) 2 . . . ? N2 Tb1 N5 O2 29.2(7) 3 . . . ? N1 Tb1 N5 O2 137.8(3) . . . . ? N5 Tb1 N5 O2 -89.6(3) 2 . . . ? N5 Tb1 N5 O2 5.1(3) 3 . . . ? O2 Tb1 N5 O1 160.2(3) 3 . . . ? O2 Tb1 N5 O1 93.1(3) 2 . . . ? O2 Tb1 N5 O1 -179.7(5) . . . . ? O1 Tb1 N5 O1 87.9(2) 2 . . . ? O1 Tb1 N5 O1 -148.4(3) 3 . . . ? N2 Tb1 N5 O1 -83.2(3) . . . . ? N2 Tb1 N5 O1 18.0(3) 2 . . . ? N2 Tb1 N5 O1 -150.5(5) 3 . . . ? N1 Tb1 N5 O1 -41.9(4) . . . . ? N5 Tb1 N5 O1 90.7(4) 2 . . . ? N5 Tb1 N5 O1 -174.5(3) 3 . . . ? O1W Tb2 N6 O5 -13.6(4) . . . . ? O1W Tb2 N6 O5 77.2(4) 2_665 . . . ? O1W Tb2 N6 O5 118.6(12) 3_565 . . . ? O4 Tb2 N6 O5 175.6(7) . . . . ? O4 Tb2 N6 O5 -93.3(4) 3_565 . . . ? O4 Tb2 N6 O5 -160.8(4) 2_665 . . . ? O5 Tb2 N6 O5 -88.6(3) 3_565 . . . ? O5 Tb2 N6 O5 147.6(4) 2_665 . . . ? N6 Tb2 N6 O5 -92.1(5) 3_565 . . . ? N6 Tb2 N6 O5 173.0(4) 2_665 . . . ? O1W Tb2 N6 O4 170.8(4) . . . . ? O1W Tb2 N6 O4 -98.4(4) 2_665 . . . ? O1W Tb2 N6 O4 -57.0(13) 3_565 . . . ? O4 Tb2 N6 O4 91.1(5) 3_565 . . . ? O4 Tb2 N6 O4 23.6(4) 2_665 . . . ? O5 Tb2 N6 O4 -175.6(7) . . . . ? O5 Tb2 N6 O4 95.8(4) 3_565 . . . ? O5 Tb2 N6 O4 -28.0(4) 2_665 . . . ? N6 Tb2 N6 O4 92.3(3) 3_565 . . . ? N6 Tb2 N6 O4 -2.6(4) 2_665 . . . ? O1W Tb2 N6 O6 88(16) . . . . ? O1W Tb2 N6 O6 179(100) 2_665 . . . ? O1W Tb2 N6 O6 -140(15) 3_565 . . . ? O4 Tb2 N6 O6 -83(16) . . . . ? O4 Tb2 N6 O6 9(16) 3_565 . . . ? O4 Tb2 N6 O6 -59(16) 2_665 . . . ? O5 Tb2 N6 O6 102(16) . . . . ? O5 Tb2 N6 O6 13(16) 3_565 . . . ? O5 Tb2 N6 O6 -111(16) 2_665 . . . ? N6 Tb2 N6 O6 10(16) 3_565 . . . ? N6 Tb2 N6 O6 -85(16) 2_665 . . . ? C1 N1 C1 C2 -162.6(5) 2 . . . ? C1 N1 C1 C2 80.5(7) 3 . . . ? Tb1 N1 C1 C2 -41.0(5) . . . . ? C3 N2 C2 N3 -1.7(6) . . . . ? Tb1 N2 C2 N3 176.0(3) . . . . ? C3 N2 C2 C1 177.0(5) . . . . ? Tb1 N2 C2 C1 -5.4(7) . . . . ? C8 N3 C2 N2 1.7(6) . . . . ? C9 N3 C2 N2 -171.3(5) . . . . ? C8 N3 C2 C1 -176.9(5) . . . . ? C9 N3 C2 C1 10.1(9) . . . . ? N1 C1 C2 N2 33.2(7) . . . . ? N1 C1 C2 N3 -148.3(5) . . . . ? C2 N2 C3 C8 0.9(6) . . . . ? Tb1 N2 C3 C8 -176.2(4) . . . . ? C2 N2 C3 C4 178.9(6) . . . . ? Tb1 N2 C3 C4 1.8(9) . . . . ? N2 C3 C4 C5 -179.6(6) . . . . ? C8 C3 C4 C5 -1.9(8) . . . . ? C3 C4 C5 C6 2.3(10) . . . . ? C4 C5 C6 C7 -2.8(10) . . . . ? C5 C6 C7 C8 2.6(9) . . . . ? C6 C7 C8 N3 177.8(6) . . . . ? C6 C7 C8 C3 -2.3(9) . . . . ? C2 N3 C8 C7 178.9(6) . . . . ? C9 N3 C8 C7 -7.8(9) . . . . ? C2 N3 C8 C3 -1.0(6) . . . . ? C9 N3 C8 C3 172.3(5) . . . . ? N2 C3 C8 C7 -179.8(5) . . . . ? C4 C3 C8 C7 1.9(9) . . . . ? N2 C3 C8 N3 0.1(6) . . . . ? C4 C3 C8 N3 -178.1(5) . . . . ? C2 N3 C9 C10 98.4(8) . . . . ? C8 N3 C9 C10 -73.5(7) . . . . ? N3 C9 C10 C14 9.1(10) . . . . ? N3 C9 C10 C11 -171.5(6) . . . . ? C14 C10 C11 C12 3.6(12) . . . . ? C9 C10 C11 C12 -175.9(8) . . . . ? C13 N4 C12 C11 2.9(15) . . . . ? C10 C11 C12 N4 -4.2(14) . . . . ? C12 N4 C13 C14 -1.0(14) . . . . ? N4 C13 C14 C10 0.5(13) . . . . ? C11 C10 C14 C13 -1.8(11) . . . . ? C9 C10 C14 C13 177.6(7) . . . . ? O3 N5 O1 Tb1 -179.7(5) . . . . ? O2 N5 O1 Tb1 -0.3(5) . . . . ? O2 Tb1 O1 N5 -22.6(4) 3 . . . ? O2 Tb1 O1 N5 -77.9(3) 2 . . . ? O2 Tb1 O1 N5 0.2(3) . . . . ? O1 Tb1 O1 N5 -106.1(3) 2 . . . ? O1 Tb1 O1 N5 35.6(4) 3 . . . ? N2 Tb1 O1 N5 88.2(3) . . . . ? N2 Tb1 O1 N5 -160.5(3) 2 . . . ? N2 Tb1 O1 N5 152.4(5) 3 . . . ? N1 Tb1 O1 N5 144.7(3) . . . . ? N5 Tb1 O1 N5 -91.3(4) 2 . . . ? N5 Tb1 O1 N5 6.3(4) 3 . . . ? O3 N5 O2 Tb1 179.6(5) . . . . ? O1 N5 O2 Tb1 0.3(5) . . . . ? O2 Tb1 O2 N5 158.5(4) 3 . . . ? O2 Tb1 O2 N5 83.2(4) 2 . . . ? O1 Tb1 O2 N5 102.0(3) 2 . . . ? O1 Tb1 O2 N5 -0.2(3) . . . . ? O1 Tb1 O2 N5 -147.2(4) 3 . . . ? N2 Tb1 O2 N5 -76.7(3) . . . . ? N2 Tb1 O2 N5 19.8(4) 2 . . . ? N2 Tb1 O2 N5 -168.8(3) 3 . . . ? N1 Tb1 O2 N5 -59.1(4) . . . . ? N5 Tb1 O2 N5 92.2(3) 2 . . . ? N5 Tb1 O2 N5 -174.5(4) 3 . . . ? O5 N6 O4 Tb2 -4.4(7) . . . . ? O6 N6 O4 Tb2 177.3(6) . . . . ? O1W Tb2 O4 N6 -10.8(5) . . . . ? O1W Tb2 O4 N6 77.3(4) 2_665 . . . ? O1W Tb2 O4 N6 160.8(5) 3_565 . . . ? O4 Tb2 O4 N6 -79.2(5) 3_565 . . . ? O4 Tb2 O4 N6 -155.1(4) 2_665 . . . ? O5 Tb2 O4 N6 2.4(4) . . . . ? O5 Tb2 O4 N6 -99.1(4) 3_565 . . . ? O5 Tb2 O4 N6 150.6(4) 2_665 . . . ? N6 Tb2 O4 N6 -89.9(3) 3_565 . . . ? N6 Tb2 O4 N6 177.2(4) 2_665 . . . ? O4 N6 O5 Tb2 4.4(6) . . . . ? O6 N6 O5 Tb2 -177.4(6) . . . . ? O1W Tb2 O5 N6 165.8(5) . . . . ? O1W Tb2 O5 N6 -96.4(5) 2_665 . . . ? O1W Tb2 O5 N6 -148.5(6) 3_565 . . . ? O4 Tb2 O5 N6 -2.5(4) . . . . ? O4 Tb2 O5 N6 77.5(4) 3_565 . . . ? O4 Tb2 O5 N6 21.9(5) 2_665 . . . ? O5 Tb2 O5 N6 104.8(4) 3_565 . . . ? O5 Tb2 O5 N6 -36.4(5) 2_665 . . . ? N6 Tb2 O5 N6 90.1(5) 3_565 . . . ? N6 Tb2 O5 N6 -8.0(5) 2_665 . . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 62.46 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 1.088 _refine_diff_density_min -1.962 _refine_diff_density_rms 0.156 #============================END