# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_shelxl _database_code_depnum_ccdc_archive 'CCDC 908244' #TrackingRef '17900_web_deposit_cif_file_0_HeatherLouisaBuckley_1361293565.hb035squeeze.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common HB035 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H67 La N4 O7' _chemical_formula_weight 1047.05 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' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.9588(9) _cell_length_b 15.2867(13) _cell_length_c 19.8423(15) _cell_angle_alpha 68.450(3) _cell_angle_beta 88.921(3) _cell_angle_gamma 83.803(3) _cell_volume 3072.9(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9893 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 25.25 _exptl_crystal_description plate _exptl_crystal_colour purple _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.132 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1088 _exptl_absorpt_coefficient_mu 0.741 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9431 _exptl_absorpt_correction_T_max 0.9853 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_reflns_number 35604 _diffrn_reflns_av_R_equivalents 0.0673 _diffrn_reflns_av_sigmaI/netI 0.0955 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 25.46 _reflns_number_total 11189 _reflns_number_gt 8333 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution SIR-2004 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ORTEP-32 _computing_publication_material WinGX _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^)+(0.0635P)^2^+7.3819P] 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 11189 _refine_ls_number_parameters 626 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0707 _refine_ls_R_factor_gt 0.0477 _refine_ls_wR_factor_ref 0.1159 _refine_ls_wR_factor_gt 0.1059 _refine_ls_goodness_of_fit_ref 0.799 _refine_ls_restrained_S_all 0.799 _refine_ls_shift/su_max 0.031 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2171(3) 0.1931(3) 0.8898(2) 0.0194(9) Uani 1 1 d . . . C2 C 0.2676(4) 0.1336(3) 0.9593(2) 0.0268(10) Uani 1 1 d . . . H2 H 0.2883 0.1534 0.9973 0.032 Uiso 1 1 calc R . . C3 C 0.2807(4) 0.0426(3) 0.9611(2) 0.0248(10) Uani 1 1 d . . . H3 H 0.3130 -0.0123 1.0003 0.030 Uiso 1 1 calc R . . C4 C 0.2362(3) 0.0460(3) 0.8926(2) 0.0215(9) Uani 1 1 d . . . C5 C 0.2513(3) -0.0238(3) 0.8611(2) 0.0220(9) Uani 1 1 d . . . C6 C 0.2418(4) -0.0042(3) 0.7858(2) 0.0229(9) Uani 1 1 d . . . C7 C 0.2713(4) -0.0698(3) 0.7504(2) 0.0261(10) Uani 1 1 d . . . H7 H 0.2916 -0.1361 0.7735 0.031 Uiso 1 1 calc R . . C8 C 0.2650(4) -0.0200(3) 0.6780(2) 0.0271(10) Uani 1 1 d . . . H8 H 0.2791 -0.0458 0.6413 0.033 Uiso 1 1 calc R . . C9 C 0.2335(3) 0.0780(3) 0.6660(2) 0.0199(9) Uani 1 1 d . . . C10 C 0.2313(3) 0.1563(3) 0.5992(2) 0.0213(9) Uani 1 1 d . . . C11 C 0.2260(3) 0.2524(3) 0.5908(2) 0.0208(9) Uani 1 1 d . . . C12 C 0.2559(4) 0.3299(3) 0.5271(2) 0.0238(10) Uani 1 1 d . . . H12 H 0.2734 0.3268 0.4809 0.029 Uiso 1 1 calc R . . C13 C 0.2548(4) 0.4084(3) 0.5444(2) 0.0236(10) Uani 1 1 d . . . H13 H 0.2723 0.4693 0.5127 0.028 Uiso 1 1 calc R . . C14 C 0.2224(3) 0.3826(3) 0.6191(2) 0.0196(9) Uani 1 1 d . . . C15 C 0.2231(3) 0.4387(3) 0.6613(2) 0.0210(9) Uani 1 1 d . . . C16 C 0.2131(4) 0.4036(3) 0.7381(2) 0.0217(9) Uani 1 1 d . . . C17 C 0.2525(4) 0.4420(3) 0.7886(2) 0.0272(10) Uani 1 1 d . . . H17 H 0.2750 0.5040 0.7775 0.033 Uiso 1 1 calc R . . C18 C 0.2520(4) 0.3724(3) 0.8562(2) 0.0292(10) Uani 1 1 d . . . H18 H 0.2745 0.3771 0.9007 0.035 Uiso 1 1 calc R . . C19 C 0.2112(4) 0.2917(3) 0.8473(2) 0.0232(10) Uani 1 1 d . . . C20 C 0.2949(4) -0.1236(3) 0.9088(2) 0.0244(10) Uani 1 1 d . . . C21 C 0.4213(4) -0.1532(3) 0.9183(2) 0.0302(11) Uani 1 1 d . . . C22 C 0.4617(4) -0.2460(3) 0.9614(2) 0.0373(12) Uani 1 1 d . . . H22 H 0.5474 -0.2656 0.9671 0.045 Uiso 1 1 calc R . . C23 C 0.3801(5) -0.3108(3) 0.9965(3) 0.0395(12) Uani 1 1 d . . . C24 C 0.2552(5) -0.2805(3) 0.9865(2) 0.0365(12) Uani 1 1 d . . . H24 H 0.1980 -0.3241 1.0097 0.044 Uiso 1 1 calc R . . C25 C 0.2116(4) -0.1881(3) 0.9433(2) 0.0289(10) Uani 1 1 d . . . C26 C 0.5134(4) -0.0842(4) 0.8832(2) 0.0383(12) Uani 1 1 d . . . H26A H 0.5234 -0.0455 0.9122 0.057 Uiso 1 1 calc R . . H26B H 0.4840 -0.0432 0.8343 0.057 Uiso 1 1 calc R . . H26C H 0.5925 -0.1191 0.8804 0.057 Uiso 1 1 calc R . . C27 C 0.4274(6) -0.4114(4) 1.0453(3) 0.0576(16) Uani 1 1 d . . . H27A H 0.5051 -0.4308 1.0268 0.086 Uiso 1 1 calc R . . H27B H 0.3669 -0.4543 1.0458 0.086 Uiso 1 1 calc R . . H27C H 0.4406 -0.4136 1.0946 0.086 Uiso 1 1 calc R . . C28 C 0.0753(4) -0.1598(3) 0.9324(3) 0.0385(12) Uani 1 1 d . . . H28A H 0.0558 -0.0966 0.9340 0.058 Uiso 1 1 calc R . . H28B H 0.0318 -0.2053 0.9708 0.058 Uiso 1 1 calc R . . H28C H 0.0495 -0.1592 0.8852 0.058 Uiso 1 1 calc R . . C29 C 0.2492(4) 0.1345(3) 0.5319(2) 0.0223(9) Uani 1 1 d . . . C30 C 0.3626(4) 0.1109(4) 0.5090(3) 0.0406(13) Uani 1 1 d . . . H30 H 0.4328 0.1067 0.5378 0.049 Uiso 1 1 calc R . . C31 C 0.3793(4) 0.0930(4) 0.4458(3) 0.0399(13) Uani 1 1 d . . . H31 H 0.4596 0.0772 0.4320 0.048 Uiso 1 1 calc R . . C32 C 0.2807(4) 0.0981(3) 0.4037(2) 0.0302(11) Uani 1 1 d . . . C33 C 0.1665(5) 0.1186(5) 0.4258(3) 0.069(2) Uani 1 1 d . . . H33 H 0.0964 0.1200 0.3978 0.083 Uiso 1 1 calc R . . C34 C 0.1516(4) 0.1371(5) 0.4883(3) 0.0575(18) Uani 1 1 d . . . H34 H 0.0709 0.1524 0.5019 0.069 Uiso 1 1 calc R . . C35 C 0.4050(5) 0.0690(4) 0.3129(3) 0.0481(14) Uani 1 1 d . . . H35A H 0.4498 0.1225 0.3095 0.072 Uiso 1 1 calc R . . H35B H 0.3968 0.0662 0.2646 0.072 Uiso 1 1 calc R . . H35C H 0.4501 0.0100 0.3453 0.072 Uiso 1 1 calc R . . C36 C 0.2440(4) 0.5413(3) 0.6253(2) 0.0211(9) Uani 1 1 d . . . C37 C 0.3632(4) 0.5684(3) 0.6080(2) 0.0289(10) Uani 1 1 d . . . C38 C 0.3772(4) 0.6651(3) 0.5789(2) 0.0317(11) Uani 1 1 d . . . H38 H 0.4571 0.6834 0.5660 0.038 Uiso 1 1 calc R . . C39 C 0.2808(4) 0.7354(3) 0.5679(2) 0.0279(10) Uani 1 1 d . . . C40 C 0.1655(4) 0.7069(3) 0.5853(2) 0.0314(11) Uani 1 1 d . . . H40 H 0.0972 0.7537 0.5775 0.038 Uiso 1 1 calc R . . C41 C 0.1455(4) 0.6111(3) 0.6143(2) 0.0254(10) Uani 1 1 d . . . C42 C 0.4722(4) 0.4958(4) 0.6199(3) 0.0453(13) Uani 1 1 d . . . H42A H 0.4696 0.4472 0.6685 0.068 Uiso 1 1 calc R . . H42B H 0.5477 0.5263 0.6154 0.068 Uiso 1 1 calc R . . H42C H 0.4707 0.4664 0.5836 0.068 Uiso 1 1 calc R . . C43 C 0.3003(5) 0.8386(3) 0.5399(3) 0.0398(12) Uani 1 1 d . . . H43A H 0.2206 0.8771 0.5317 0.060 Uiso 1 1 calc R . . H43B H 0.3443 0.8544 0.4942 0.060 Uiso 1 1 calc R . . H43C H 0.3488 0.8514 0.5756 0.060 Uiso 1 1 calc R . . C44 C 0.0161(4) 0.5857(3) 0.6323(3) 0.0366(12) Uani 1 1 d . . . H44A H 0.0011 0.5350 0.6154 0.055 Uiso 1 1 calc R . . H44B H -0.0425 0.6415 0.6083 0.055 Uiso 1 1 calc R . . H44C H 0.0059 0.5643 0.6849 0.055 Uiso 1 1 calc R . . C45 C -0.0830(4) 0.0962(4) 0.9096(3) 0.0425(13) Uani 1 1 d . . . H45A H -0.1573 0.1399 0.9055 0.064 Uiso 1 1 calc R . . H45B H -0.0128 0.1213 0.9231 0.064 Uiso 1 1 calc R . . H45C H -0.0940 0.0344 0.9467 0.064 Uiso 1 1 calc R . . C46 C -0.1513(4) 0.0374(4) 0.8223(3) 0.0419(13) Uani 1 1 d . . . H46A H -0.2320 0.0761 0.8130 0.050 Uiso 1 1 calc R . . H46B H -0.1597 -0.0237 0.8622 0.050 Uiso 1 1 calc R . . C47 C -0.1087(5) 0.0208(3) 0.7551(3) 0.0433(13) Uani 1 1 d . . . H47A H -0.0298 -0.0204 0.7650 0.052 Uiso 1 1 calc R . . H47B H -0.1701 -0.0104 0.7386 0.052 Uiso 1 1 calc R . . C48 C -0.0854(5) 0.1061(4) 0.6301(3) 0.0445(13) Uani 1 1 d . . . H48A H -0.0150 0.0613 0.6291 0.067 Uiso 1 1 calc R . . H48B H -0.0746 0.1689 0.5943 0.067 Uiso 1 1 calc R . . H48C H -0.1608 0.0850 0.6184 0.067 Uiso 1 1 calc R . . C49 C -0.1015(5) 0.3823(4) 0.8151(3) 0.0438(13) Uani 1 1 d . . . H49A H -0.0966 0.4427 0.7749 0.066 Uiso 1 1 calc R . . H49B H -0.0274 0.3665 0.8460 0.066 Uiso 1 1 calc R . . H49C H -0.1739 0.3874 0.8438 0.066 Uiso 1 1 calc R . . C50 C -0.2194(4) 0.3238(4) 0.7431(3) 0.0383(12) Uani 1 1 d . . . H50A H -0.2880 0.3564 0.7611 0.046 Uiso 1 1 calc R . . H50B H -0.2429 0.2613 0.7472 0.046 Uiso 1 1 calc R . . C51 C -0.1987(4) 0.3806(3) 0.6655(2) 0.0321(11) Uani 1 1 d . . . H51A H -0.2718 0.3846 0.6355 0.039 Uiso 1 1 calc R . . H51B H -0.1837 0.4456 0.6599 0.039 Uiso 1 1 calc R . . C53 C 0.5651(4) 0.2038(4) 0.8872(3) 0.0435(13) Uani 1 1 d . . . H53A H 0.5271 0.2693 0.8723 0.065 Uiso 1 1 calc R . . H53B H 0.6433 0.1974 0.9126 0.065 Uiso 1 1 calc R . . H53C H 0.5102 0.1614 0.9196 0.065 Uiso 1 1 calc R . . C54 C 0.4766(4) 0.1968(4) 0.7832(3) 0.0353(12) Uani 1 1 d . . . H54A H 0.4407 0.2632 0.7707 0.042 Uiso 1 1 calc R . . H54B H 0.4159 0.1550 0.8114 0.042 Uiso 1 1 calc R . . C55 C 0.5044(4) 0.1785(4) 0.7167(3) 0.0447(13) Uani 1 1 d . . . H55A H 0.5498 0.1148 0.7289 0.054 Uiso 1 1 calc R . . H55B H 0.4271 0.1805 0.6908 0.054 Uiso 1 1 calc R . . C56 C 0.5926(6) 0.2430(6) 0.6038(3) 0.084(3) Uani 1 1 d . . . H56A H 0.6376 0.1818 0.6091 0.126 Uiso 1 1 calc R . . H56B H 0.6391 0.2941 0.5735 0.126 Uiso 1 1 calc R . . H56C H 0.5120 0.2489 0.5809 0.126 Uiso 1 1 calc R . . N1 N 0.1937(3) 0.1381(2) 0.85223(17) 0.0201(8) Uani 1 1 d . . . N2 N 0.2151(3) 0.0858(2) 0.73299(17) 0.0198(7) Uani 1 1 d . . . N3 N 0.2026(3) 0.2873(2) 0.64547(17) 0.0197(8) Uani 1 1 d . . . N4 N 0.1833(3) 0.3142(2) 0.77565(17) 0.0202(8) Uani 1 1 d . . . O1 O 0.2870(3) 0.0807(3) 0.34055(17) 0.0433(9) Uani 1 1 d . . . O2 O -0.0610(3) 0.0859(2) 0.84142(16) 0.0331(8) Uani 1 1 d . . . O3 O -0.0938(3) 0.1107(2) 0.70098(17) 0.0345(8) Uani 1 1 d . . . O4 O -0.1113(3) 0.3104(2) 0.78722(16) 0.0328(8) Uani 1 1 d . . . O5 O -0.0946(2) 0.3349(2) 0.64311(15) 0.0318(7) Uani 1 1 d . . . O6 O 0.5861(3) 0.1799(2) 0.82548(17) 0.0363(8) Uani 1 1 d . . . O7 O 0.5770(3) 0.2489(3) 0.67150(19) 0.0582(11) Uani 1 1 d . . . La1 La 0.06510(2) 0.209750(18) 0.742400(13) 0.02021(9) Uani 1 1 d . . . C52 C -0.0774(4) 0.3761(3) 0.5664(2) 0.0353(12) Uani 1 1 d . . . H52A H -0.0712 0.4439 0.5523 0.053 Uiso 1 1 calc R . . H52B H -0.1474 0.3668 0.5407 0.053 Uiso 1 1 calc R . . H52C H -0.0018 0.3456 0.5538 0.053 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0136(19) 0.029(2) 0.017(2) -0.0096(19) 0.0022(16) -0.0037(18) C2 0.029(2) 0.034(3) 0.017(2) -0.008(2) 0.0034(18) -0.008(2) C3 0.021(2) 0.029(3) 0.017(2) -0.0004(19) 0.0012(17) -0.0027(19) C4 0.0147(19) 0.026(2) 0.023(2) -0.007(2) 0.0003(17) -0.0050(18) C5 0.016(2) 0.024(2) 0.019(2) -0.0010(19) 0.0042(17) -0.0002(18) C6 0.019(2) 0.022(2) 0.025(2) -0.008(2) 0.0035(18) 0.0027(18) C7 0.033(2) 0.016(2) 0.024(2) -0.0023(19) 0.0019(19) 0.0030(19) C8 0.030(2) 0.025(3) 0.028(2) -0.013(2) 0.0002(19) 0.001(2) C9 0.0132(19) 0.026(2) 0.020(2) -0.0085(19) 0.0026(16) -0.0039(18) C10 0.017(2) 0.026(2) 0.021(2) -0.0103(19) -0.0013(17) -0.0012(18) C11 0.0158(19) 0.027(3) 0.019(2) -0.0078(19) -0.0003(16) 0.0007(18) C12 0.023(2) 0.028(3) 0.015(2) -0.0026(19) 0.0003(17) -0.0015(19) C13 0.023(2) 0.022(2) 0.018(2) 0.0000(19) 0.0021(17) 0.0003(18) C14 0.0148(19) 0.021(2) 0.021(2) -0.0066(19) -0.0007(16) 0.0003(17) C15 0.018(2) 0.019(2) 0.021(2) -0.0021(18) 0.0035(17) -0.0009(17) C16 0.021(2) 0.021(2) 0.023(2) -0.0086(19) 0.0024(17) -0.0028(18) C17 0.029(2) 0.025(3) 0.031(2) -0.012(2) 0.004(2) -0.008(2) C18 0.033(2) 0.031(3) 0.025(2) -0.013(2) 0.003(2) -0.006(2) C19 0.020(2) 0.030(3) 0.019(2) -0.010(2) 0.0030(17) -0.0006(19) C20 0.027(2) 0.024(2) 0.019(2) -0.0062(19) -0.0003(18) 0.0045(19) C21 0.035(3) 0.036(3) 0.018(2) -0.010(2) -0.0010(19) 0.005(2) C22 0.036(3) 0.039(3) 0.032(3) -0.012(2) -0.005(2) 0.013(2) C23 0.055(3) 0.029(3) 0.033(3) -0.012(2) -0.006(2) 0.006(3) C24 0.054(3) 0.023(3) 0.029(3) -0.006(2) 0.003(2) -0.005(2) C25 0.035(2) 0.024(3) 0.028(2) -0.011(2) 0.000(2) 0.000(2) C26 0.023(2) 0.052(3) 0.028(3) -0.004(2) 0.007(2) 0.007(2) C27 0.081(4) 0.032(3) 0.050(3) -0.009(3) -0.014(3) 0.015(3) C28 0.035(3) 0.034(3) 0.042(3) -0.007(2) 0.006(2) -0.010(2) C29 0.022(2) 0.025(2) 0.019(2) -0.0074(19) 0.0016(17) -0.0029(18) C30 0.020(2) 0.075(4) 0.039(3) -0.034(3) 0.002(2) -0.012(2) C31 0.022(2) 0.069(4) 0.045(3) -0.039(3) 0.011(2) -0.014(2) C32 0.028(2) 0.041(3) 0.028(2) -0.020(2) 0.0021(19) -0.003(2) C33 0.027(3) 0.141(7) 0.069(4) -0.079(5) -0.012(3) 0.014(3) C34 0.024(3) 0.118(5) 0.049(3) -0.060(4) -0.007(2) 0.022(3) C35 0.053(3) 0.066(4) 0.041(3) -0.034(3) 0.013(3) -0.017(3) C36 0.028(2) 0.020(2) 0.015(2) -0.0061(18) 0.0000(17) -0.0031(19) C37 0.030(2) 0.025(3) 0.029(2) -0.005(2) 0.005(2) -0.004(2) C38 0.027(2) 0.039(3) 0.029(2) -0.010(2) 0.007(2) -0.011(2) C39 0.037(3) 0.028(3) 0.023(2) -0.011(2) 0.010(2) -0.015(2) C40 0.037(3) 0.025(3) 0.032(3) -0.010(2) 0.002(2) -0.005(2) C41 0.027(2) 0.026(3) 0.025(2) -0.010(2) 0.0034(19) -0.007(2) C42 0.025(2) 0.037(3) 0.069(4) -0.015(3) 0.008(2) -0.006(2) C43 0.047(3) 0.029(3) 0.046(3) -0.016(2) 0.012(2) -0.012(2) C44 0.024(2) 0.027(3) 0.057(3) -0.013(2) 0.008(2) -0.006(2) C45 0.032(3) 0.045(3) 0.038(3) -0.002(3) 0.016(2) -0.002(2) C46 0.023(2) 0.035(3) 0.056(3) 0.000(3) 0.002(2) -0.011(2) C47 0.034(3) 0.028(3) 0.060(4) -0.005(3) -0.014(3) -0.007(2) C48 0.040(3) 0.043(3) 0.053(3) -0.021(3) -0.005(3) -0.002(3) C49 0.038(3) 0.051(4) 0.050(3) -0.028(3) 0.009(2) -0.006(3) C50 0.022(2) 0.049(3) 0.042(3) -0.018(3) 0.004(2) 0.003(2) C51 0.017(2) 0.035(3) 0.036(3) -0.007(2) -0.0020(19) 0.008(2) C53 0.028(3) 0.062(4) 0.043(3) -0.024(3) 0.003(2) 0.004(3) C54 0.018(2) 0.044(3) 0.043(3) -0.015(2) 0.001(2) -0.005(2) C55 0.029(3) 0.057(4) 0.049(3) -0.018(3) -0.007(2) -0.011(3) C56 0.056(4) 0.173(8) 0.047(4) -0.059(5) 0.009(3) -0.048(5) N1 0.0162(16) 0.025(2) 0.0165(17) -0.0052(16) 0.0019(14) 0.0005(15) N2 0.0206(17) 0.0187(19) 0.0171(17) -0.0037(15) 0.0005(14) -0.0005(15) N3 0.0187(17) 0.0191(19) 0.0196(18) -0.0056(15) 0.0010(14) 0.0005(15) N4 0.0198(17) 0.021(2) 0.0181(18) -0.0060(15) 0.0046(14) -0.0008(15) O1 0.0333(18) 0.072(3) 0.041(2) -0.041(2) 0.0038(15) -0.0040(18) O2 0.0213(15) 0.040(2) 0.0329(18) -0.0056(15) 0.0032(13) -0.0090(14) O3 0.0312(17) 0.0306(19) 0.044(2) -0.0154(16) -0.0007(15) -0.0085(15) O4 0.0218(15) 0.038(2) 0.0376(18) -0.0150(16) -0.0021(14) 0.0048(14) O5 0.0187(15) 0.039(2) 0.0272(17) -0.0021(15) 0.0001(13) 0.0067(14) O6 0.0191(15) 0.053(2) 0.0399(19) -0.0208(17) 0.0027(14) -0.0017(15) O7 0.044(2) 0.103(3) 0.042(2) -0.036(2) 0.0136(17) -0.036(2) La1 0.01533(12) 0.02161(15) 0.02100(14) -0.00477(10) 0.00092(9) -0.00179(9) C52 0.032(3) 0.038(3) 0.026(2) -0.002(2) -0.002(2) 0.002(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 C1 N1 1.357(5) . ? C1 C2 1.426(6) . ? C1 C19 1.426(6) . ? C2 C3 1.370(6) . ? C2 H2 0.9500 . ? C3 C4 1.433(6) . ? C3 H3 0.9500 . ? C4 N1 1.372(5) . ? C4 C5 1.417(6) . ? C5 C6 1.415(6) . ? C5 C20 1.500(6) . ? C6 N2 1.395(5) . ? C6 C7 1.427(6) . ? C7 C8 1.356(6) . ? C7 H7 0.9500 . ? C8 C9 1.432(6) . ? C8 H8 0.9500 . ? C9 N2 1.387(5) . ? C9 C10 1.421(6) . ? C10 C11 1.412(6) . ? C10 C29 1.494(6) . ? C11 N3 1.383(5) . ? C11 C12 1.442(6) . ? C12 C13 1.362(6) . ? C12 H12 0.9500 . ? C13 C14 1.436(5) . ? C13 H13 0.9500 . ? C14 N3 1.395(5) . ? C14 C15 1.401(6) . ? C15 C16 1.424(6) . ? C15 C36 1.507(6) . ? C16 N4 1.367(5) . ? C16 C17 1.429(6) . ? C17 C18 1.373(6) . ? C17 H17 0.9500 . ? C18 C19 1.427(6) . ? C18 H18 0.9500 . ? C19 N4 1.366(5) . ? C20 C21 1.404(6) . ? C20 C25 1.397(6) . ? C21 C22 1.388(6) . ? C21 C26 1.510(7) . ? C22 C23 1.389(7) . ? C22 H22 0.9500 . ? C23 C24 1.391(7) . ? C23 C27 1.524(7) . ? C24 C25 1.392(6) . ? C24 H24 0.9500 . ? C25 C28 1.507(6) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.372(6) . ? C29 C34 1.377(6) . ? C30 C31 1.382(6) . ? C30 H30 0.9500 . ? C31 C32 1.357(6) . ? C31 H31 0.9500 . ? C32 C33 1.362(6) . ? C32 O1 1.372(5) . ? C33 C34 1.372(7) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? C35 O1 1.415(6) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 C41 1.393(6) . ? C36 C37 1.411(6) . ? C37 C38 1.401(6) . ? C37 C42 1.499(6) . ? C38 C39 1.382(6) . ? C38 H38 0.9500 . ? C39 C40 1.378(6) . ? C39 C43 1.505(6) . ? C40 C41 1.403(6) . ? C40 H40 0.9500 . ? C41 C44 1.512(6) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 O2 1.430(6) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 O2 1.433(6) . ? C46 C47 1.503(7) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 O3 1.423(6) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 O3 1.435(6) . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 O4 1.413(6) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 O4 1.438(5) . ? C50 C51 1.491(6) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 O5 1.424(5) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C53 O6 1.409(6) . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 O6 1.421(5) . ? C54 C55 1.466(7) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 O7 1.431(6) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 O7 1.385(6) . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? N1 La1 2.442(3) . ? N2 La1 2.429(3) . ? N3 La1 2.445(3) . ? N4 La1 2.433(3) . ? O2 La1 2.662(3) . ? O3 La1 2.745(3) . ? O4 La1 2.683(3) . ? O5 C52 1.435(5) . ? O5 La1 2.691(3) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 108.7(4) . . ? N1 C1 C19 114.6(3) . . ? C2 C1 C19 135.0(4) . . ? C3 C2 C1 107.4(4) . . ? C3 C2 H2 126.3 . . ? C1 C2 H2 126.3 . . ? C2 C3 C4 107.0(4) . . ? C2 C3 H3 126.5 . . ? C4 C3 H3 126.5 . . ? N1 C4 C5 121.2(4) . . ? N1 C4 C3 108.2(4) . . ? C5 C4 C3 129.5(4) . . ? C6 C5 C4 124.2(4) . . ? C6 C5 C20 116.9(4) . . ? C4 C5 C20 118.4(3) . . ? N2 C6 C5 124.7(4) . . ? N2 C6 C7 108.5(3) . . ? C5 C6 C7 126.5(4) . . ? C8 C7 C6 107.5(4) . . ? C8 C7 H7 126.2 . . ? C6 C7 H7 126.2 . . ? C7 C8 C9 108.6(4) . . ? C7 C8 H8 125.7 . . ? C9 C8 H8 125.7 . . ? N2 C9 C10 124.3(4) . . ? N2 C9 C8 107.9(3) . . ? C10 C9 C8 127.6(4) . . ? C11 C10 C9 126.0(4) . . ? C11 C10 C29 116.6(4) . . ? C9 C10 C29 117.0(4) . . ? N3 C11 C10 125.3(4) . . ? N3 C11 C12 107.5(4) . . ? C10 C11 C12 126.9(4) . . ? C13 C12 C11 108.4(4) . . ? C13 C12 H12 125.8 . . ? C11 C12 H12 125.8 . . ? C12 C13 C14 107.7(4) . . ? C12 C13 H13 126.1 . . ? C14 C13 H13 126.1 . . ? N3 C14 C15 125.0(4) . . ? N3 C14 C13 107.9(3) . . ? C15 C14 C13 126.8(4) . . ? C14 C15 C16 124.0(4) . . ? C14 C15 C36 119.3(3) . . ? C16 C15 C36 116.5(4) . . ? N4 C16 C17 108.6(4) . . ? N4 C16 C15 121.5(4) . . ? C17 C16 C15 128.9(4) . . ? C18 C17 C16 107.1(4) . . ? C18 C17 H17 126.4 . . ? C16 C17 H17 126.4 . . ? C17 C18 C19 107.2(4) . . ? C17 C18 H18 126.4 . . ? C19 C18 H18 126.4 . . ? N4 C19 C18 108.7(4) . . ? N4 C19 C1 114.2(4) . . ? C18 C19 C1 135.6(4) . . ? C21 C20 C25 119.3(4) . . ? C21 C20 C5 119.7(4) . . ? C25 C20 C5 121.0(4) . . ? C22 C21 C20 119.7(4) . . ? C22 C21 C26 119.9(4) . . ? C20 C21 C26 120.4(4) . . ? C23 C22 C21 121.7(4) . . ? C23 C22 H22 119.2 . . ? C21 C22 H22 119.2 . . ? C22 C23 C24 118.0(4) . . ? C22 C23 C27 120.4(5) . . ? C24 C23 C27 121.6(5) . . ? C25 C24 C23 121.8(5) . . ? C25 C24 H24 119.1 . . ? C23 C24 H24 119.1 . . ? C24 C25 C20 119.5(4) . . ? C24 C25 C28 119.6(4) . . ? C20 C25 C28 120.8(4) . . ? C21 C26 H26A 109.5 . . ? C21 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C21 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C27 H27A 109.5 . . ? C23 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C23 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 C34 115.2(4) . . ? C30 C29 C10 123.0(4) . . ? C34 C29 C10 121.7(4) . . ? C29 C30 C31 123.0(4) . . ? C29 C30 H30 118.5 . . ? C31 C30 H30 118.5 . . ? C32 C31 C30 119.8(4) . . ? C32 C31 H31 120.1 . . ? C30 C31 H31 120.1 . . ? C31 C32 C33 118.8(4) . . ? C31 C32 O1 124.5(4) . . ? C33 C32 O1 116.7(4) . . ? C32 C33 C34 120.6(5) . . ? C32 C33 H33 119.7 . . ? C34 C33 H33 119.7 . . ? C33 C34 C29 122.5(4) . . ? C33 C34 H34 118.7 . . ? C29 C34 H34 118.7 . . ? O1 C35 H35A 109.5 . . ? O1 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? O1 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C41 C36 C37 119.2(4) . . ? C41 C36 C15 119.5(4) . . ? C37 C36 C15 121.2(4) . . ? C38 C37 C36 118.3(4) . . ? C38 C37 C42 120.7(4) . . ? C36 C37 C42 121.1(4) . . ? C39 C38 C37 123.5(4) . . ? C39 C38 H38 118.3 . . ? C37 C38 H38 118.3 . . ? C40 C39 C38 117.0(4) . . ? C40 C39 C43 121.1(4) . . ? C38 C39 C43 121.9(4) . . ? C39 C40 C41 122.3(4) . . ? C39 C40 H40 118.9 . . ? C41 C40 H40 118.9 . . ? C36 C41 C40 119.9(4) . . ? C36 C41 C44 121.2(4) . . ? C40 C41 C44 119.0(4) . . ? C37 C42 H42A 109.5 . . ? C37 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C37 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C39 C43 H43A 109.5 . . ? C39 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C39 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? O2 C45 H45A 109.5 . . ? O2 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? O2 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? O2 C46 C47 107.3(4) . . ? O2 C46 H46A 110.2 . . ? C47 C46 H46A 110.2 . . ? O2 C46 H46B 110.2 . . ? C47 C46 H46B 110.2 . . ? H46A C46 H46B 108.5 . . ? O3 C47 C46 107.4(4) . . ? O3 C47 H47A 110.2 . . ? C46 C47 H47A 110.2 . . ? O3 C47 H47B 110.2 . . ? C46 C47 H47B 110.2 . . ? H47A C47 H47B 108.5 . . ? O3 C48 H48A 109.5 . . ? O3 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? O3 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? O4 C49 H49A 109.5 . . ? O4 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? O4 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? O4 C50 C51 111.5(4) . . ? O4 C50 H50A 109.3 . . ? C51 C50 H50A 109.3 . . ? O4 C50 H50B 109.3 . . ? C51 C50 H50B 109.3 . . ? H50A C50 H50B 108.0 . . ? O5 C51 C50 107.6(3) . . ? O5 C51 H51A 110.2 . . ? C50 C51 H51A 110.2 . . ? O5 C51 H51B 110.2 . . ? C50 C51 H51B 110.2 . . ? H51A C51 H51B 108.5 . . ? O6 C53 H53A 109.5 . . ? O6 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? O6 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? O6 C54 C55 109.7(4) . . ? O6 C54 H54A 109.7 . . ? C55 C54 H54A 109.7 . . ? O6 C54 H54B 109.7 . . ? C55 C54 H54B 109.7 . . ? H54A C54 H54B 108.2 . . ? O7 C55 C54 108.9(4) . . ? O7 C55 H55A 109.9 . . ? C54 C55 H55A 109.9 . . ? O7 C55 H55B 109.9 . . ? C54 C55 H55B 109.9 . . ? H55A C55 H55B 108.3 . . ? O7 C56 H56A 109.5 . . ? O7 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? O7 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C1 N1 C4 108.5(3) . . ? C1 N1 La1 118.2(3) . . ? C4 N1 La1 132.5(3) . . ? C9 N2 C6 107.5(3) . . ? C9 N2 La1 119.0(2) . . ? C6 N2 La1 125.9(2) . . ? C11 N3 C14 108.5(3) . . ? C11 N3 La1 119.2(3) . . ? C14 N3 La1 126.9(2) . . ? C16 N4 C19 108.3(3) . . ? C16 N4 La1 132.3(3) . . ? C19 N4 La1 118.3(3) . . ? C32 O1 C35 117.3(3) . . ? C46 O2 C45 113.1(3) . . ? C46 O2 La1 122.4(3) . . ? C45 O2 La1 119.0(3) . . ? C47 O3 C48 111.6(4) . . ? C47 O3 La1 113.4(3) . . ? C48 O3 La1 119.6(3) . . ? C49 O4 C50 114.8(4) . . ? C49 O4 La1 129.6(3) . . ? C50 O4 La1 107.7(2) . . ? C51 O5 C52 112.1(3) . . ? C51 O5 La1 120.2(2) . . ? C52 O5 La1 126.8(2) . . ? C53 O6 C54 111.4(3) . . ? C56 O7 C55 111.6(5) . . ? N2 La1 N4 105.23(11) . . ? N2 La1 N1 69.02(11) . . ? N4 La1 N1 63.10(11) . . ? N2 La1 N3 73.53(11) . . ? N4 La1 N3 68.97(11) . . ? N1 La1 N3 105.85(10) . . ? N2 La1 O2 92.47(10) . . ? N4 La1 O2 120.60(10) . . ? N1 La1 O2 72.34(10) . . ? N3 La1 O2 165.24(10) . . ? N2 La1 O4 164.56(10) . . ? N4 La1 O4 78.37(10) . . ? N1 La1 O4 100.48(10) . . ? N3 La1 O4 121.22(10) . . ? O2 La1 O4 73.15(10) . . ? N2 La1 O5 130.56(10) . . ? N4 La1 O5 101.53(10) . . ? N1 La1 O5 159.55(10) . . ? N3 La1 O5 78.55(9) . . ? O2 La1 O5 108.42(9) . . ? O4 La1 O5 61.55(9) . . ? N2 La1 O3 82.23(10) . . ? N4 La1 O3 172.35(10) . . ? N1 La1 O3 122.33(10) . . ? N3 La1 O3 112.39(10) . . ? O2 La1 O3 59.80(9) . . ? O4 La1 O3 94.88(9) . . ? O5 La1 O3 71.80(10) . . ? O5 C52 H52A 109.5 . . ? O5 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? O5 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.147 _refine_diff_density_min -0.584 _refine_diff_density_rms 0.093 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.038 0.500 0.000 714 159 ' ' _platon_squeeze_details ; 1.5 Molecules 1,2-Dimethoxyethane (C4H10O2) removed per formula unit ; data_shelxl3 _database_code_depnum_ccdc_archive 'CCDC 908245' #TrackingRef '16816_web_deposit_cif_file_2_HeatherLouisaBuckley_1357921663.hb041.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common HB041 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H66 Gd N7 O' _chemical_formula_weight 1058.45 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' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.4694(10) _cell_length_b 13.2999(7) _cell_length_c 21.7953(12) _cell_angle_alpha 90.00 _cell_angle_beta 114.652(2) _cell_angle_gamma 90.00 _cell_volume 5129.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9824 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 25.35 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.371 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2188 _exptl_absorpt_coefficient_mu 1.341 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9238 _exptl_absorpt_correction_T_max 0.9737 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_reflns_number 15792 _diffrn_reflns_av_R_equivalents 0.0676 _diffrn_reflns_av_sigmaI/netI 0.0961 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 25.37 _reflns_number_total 15792 _reflns_number_gt 11004 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution SIR-2004 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ORTEP-32 _computing_publication_material WinGX _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^)+(0.0513P)^2^+35.1697P] 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 15792 _refine_ls_number_parameters 634 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1067 _refine_ls_R_factor_gt 0.0587 _refine_ls_wR_factor_ref 0.1628 _refine_ls_wR_factor_gt 0.1322 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.099 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.8717(3) 0.1787(4) 0.6167(3) 0.0173(13) Uani 1 1 d . . . C2 C 0.9282(3) 0.1160(4) 0.6117(3) 0.0171(12) Uani 1 1 d . . . H2 H 0.9650 0.1352 0.5960 0.021 Uiso 1 1 calc R . . C3 C 0.9195(3) 0.0225(5) 0.6340(3) 0.0187(13) Uani 1 1 d . . . H3 H 0.9496 -0.0350 0.6369 0.022 Uiso 1 1 calc R . . C4 C 0.8572(3) 0.0272(4) 0.6520(3) 0.0163(12) Uani 1 1 d . . . C5 C 0.8134(3) -0.0518(4) 0.6605(3) 0.0154(12) Uani 1 1 d . . . C6 C 0.7392(3) -0.0426(4) 0.6546(3) 0.0152(12) Uani 1 1 d . . . C7 C 0.6897(3) -0.1213(4) 0.6543(3) 0.0206(13) Uani 1 1 d . . . H7 H 0.7031 -0.1902 0.6630 0.025 Uiso 1 1 calc R . . C8 C 0.6201(3) -0.0818(5) 0.6396(3) 0.0217(13) Uani 1 1 d . . . H8 H 0.5767 -0.1175 0.6371 0.026 Uiso 1 1 calc R . . C9 C 0.6246(3) 0.0236(4) 0.6285(3) 0.0175(13) Uani 1 1 d . . . C10 C 0.5638(3) 0.0939(4) 0.6045(3) 0.0164(12) Uani 1 1 d . . . C11 C 0.5650(3) 0.1887(4) 0.5759(3) 0.0173(13) Uani 1 1 d . . . C12 C 0.4994(3) 0.2460(4) 0.5326(3) 0.0188(13) Uani 1 1 d . . . H12 H 0.4485 0.2325 0.5246 0.023 Uiso 1 1 calc R . . C13 C 0.5238(3) 0.3225(4) 0.5055(3) 0.0218(14) Uani 1 1 d . . . H13 H 0.4928 0.3717 0.4749 0.026 Uiso 1 1 calc R . . C14 C 0.6054(3) 0.3158(4) 0.5316(3) 0.0188(13) Uani 1 1 d . . . C15 C 0.6525(3) 0.3739(4) 0.5114(3) 0.0175(12) Uani 1 1 d . . . C16 C 0.7314(3) 0.3580(4) 0.5353(3) 0.0161(12) Uani 1 1 d . . . C17 C 0.7806(3) 0.3876(4) 0.5057(3) 0.0205(13) Uani 1 1 d . . . H17 H 0.7703 0.4370 0.4714 0.025 Uiso 1 1 calc R . . C18 C 0.8467(3) 0.3320(4) 0.5353(3) 0.0198(13) Uani 1 1 d . . . H18 H 0.8891 0.3340 0.5245 0.024 Uiso 1 1 calc R . . C19 C 0.8378(3) 0.2714(4) 0.5851(3) 0.0159(12) Uani 1 1 d . . . C20 C 0.8436(3) -0.1571(4) 0.6641(3) 0.0163(12) Uani 1 1 d . . . C21 C 0.8871(3) -0.2021(5) 0.7254(3) 0.0218(13) Uani 1 1 d . . . C22 C 0.9153(3) -0.2992(5) 0.7265(3) 0.0223(13) Uani 1 1 d . . . H22 H 0.9443 -0.3302 0.7687 0.027 Uiso 1 1 calc R . . C23 C 0.9019(3) -0.3508(5) 0.6678(3) 0.0260(14) Uani 1 1 d . . . C24 C 0.8579(3) -0.3035(5) 0.6064(3) 0.0248(14) Uani 1 1 d . . . H24 H 0.8491 -0.3371 0.5653 0.030 Uiso 1 1 calc R . . C25 C 0.8274(3) -0.2102(5) 0.6040(3) 0.0207(13) Uani 1 1 d . . . C26 C 0.9060(4) -0.1483(5) 0.7918(3) 0.0317(16) Uani 1 1 d . . . H26A H 0.8601 -0.1410 0.7994 0.048 Uiso 1 1 calc R . . H26B H 0.9267 -0.0817 0.7903 0.048 Uiso 1 1 calc R . . H26C H 0.9435 -0.1875 0.8287 0.048 Uiso 1 1 calc R . . C27 C 0.9366(4) -0.4523(5) 0.6683(4) 0.0396(18) Uani 1 1 d . . . H27A H 0.9734 -0.4465 0.6486 0.059 Uiso 1 1 calc R . . H27B H 0.8969 -0.4999 0.6418 0.059 Uiso 1 1 calc R . . H27C H 0.9622 -0.4764 0.7149 0.059 Uiso 1 1 calc R . . C28 C 0.7778(4) -0.1630(5) 0.5365(3) 0.0329(16) Uani 1 1 d . . . H28A H 0.8040 -0.1053 0.5282 0.049 Uiso 1 1 calc R . . H28B H 0.7302 -0.1406 0.5372 0.049 Uiso 1 1 calc R . . H28C H 0.7672 -0.2128 0.5005 0.049 Uiso 1 1 calc R . . C29 C 0.4890(3) 0.0570(4) 0.5998(3) 0.0157(12) Uani 1 1 d . . . C30 C 0.4484(3) -0.0169(5) 0.5539(3) 0.0222(13) Uani 1 1 d . . . H30 H 0.4695 -0.0466 0.5260 0.027 Uiso 1 1 calc R . . C31 C 0.3777(3) -0.0487(5) 0.5477(3) 0.0215(13) Uani 1 1 d . . . H31 H 0.3505 -0.0979 0.5149 0.026 Uiso 1 1 calc R . . C32 C 0.2346(3) -0.1025(5) 0.5346(3) 0.0210(13) Uani 1 1 d . . . H32A H 0.2600 -0.1677 0.5408 0.032 Uiso 1 1 calc R . . H32B H 0.2281 -0.0736 0.4912 0.032 Uiso 1 1 calc R . . H32C H 0.1849 -0.1116 0.5353 0.032 Uiso 1 1 calc R . . C33 C 0.3868(3) 0.0655(5) 0.6352(3) 0.0207(13) Uani 1 1 d . . . H33 H 0.3657 0.0942 0.6634 0.025 Uiso 1 1 calc R . . C34 C 0.4566(3) 0.0978(4) 0.6403(3) 0.0195(13) Uani 1 1 d . . . H34 H 0.4829 0.1487 0.6720 0.023 Uiso 1 1 calc R . . C35 C 0.3474(3) -0.0087(5) 0.5890(3) 0.0193(13) Uani 1 1 d . . . C36 C 0.6189(3) 0.4453(4) 0.4529(3) 0.0182(13) Uani 1 1 d . . . C37 C 0.5790(3) 0.4079(5) 0.3868(3) 0.0213(14) Uani 1 1 d . . . C38 C 0.5598(3) 0.4742(5) 0.3332(3) 0.0243(14) Uani 1 1 d . . . H38 H 0.5331 0.4490 0.2887 0.029 Uiso 1 1 calc R . . C39 C 0.5776(3) 0.5746(5) 0.3413(3) 0.0259(15) Uani 1 1 d . . . C40 C 0.6140(3) 0.6109(5) 0.4068(3) 0.0236(14) Uani 1 1 d . . . H40 H 0.6255 0.6806 0.4138 0.028 Uiso 1 1 calc R . . C41 C 0.6339(3) 0.5479(4) 0.4622(3) 0.0173(13) Uani 1 1 d . . . C42 C 0.5603(3) 0.2984(5) 0.3735(3) 0.0245(13) Uani 1 1 d . . . H42A H 0.6046 0.2580 0.4009 0.037 Uiso 1 1 calc R . . H42B H 0.5458 0.2841 0.3255 0.037 Uiso 1 1 calc R . . H42C H 0.5183 0.2816 0.3852 0.037 Uiso 1 1 calc R . . C43 C 0.5585(4) 0.6414(6) 0.2808(3) 0.0391(18) Uani 1 1 d . . . H43A H 0.6013 0.6435 0.2683 0.059 Uiso 1 1 calc R . . H43B H 0.5479 0.7095 0.2918 0.059 Uiso 1 1 calc R . . H43C H 0.5139 0.6150 0.2430 0.059 Uiso 1 1 calc R . . C44 C 0.6723(4) 0.5909(5) 0.5324(3) 0.0280(15) Uani 1 1 d . . . H44A H 0.6430 0.5738 0.5582 0.042 Uiso 1 1 calc R . . H44B H 0.6756 0.6642 0.5297 0.042 Uiso 1 1 calc R . . H44C H 0.7233 0.5627 0.5550 0.042 Uiso 1 1 calc R . . C45 C 0.8706(4) 0.2656(5) 0.8351(3) 0.0342(17) Uani 1 1 d . . . H45A H 0.8512 0.3123 0.8596 0.041 Uiso 1 1 calc R . . H45B H 0.9261 0.2613 0.8605 0.041 Uiso 1 1 calc R . . C46 C 0.8366(4) 0.1628(6) 0.8327(3) 0.0370(17) Uani 1 1 d . . . H46A H 0.8611 0.1143 0.8136 0.044 Uiso 1 1 calc R . . H46B H 0.8478 0.1411 0.8793 0.044 Uiso 1 1 calc R . . C47 C 0.7134(4) 0.2304(5) 0.8186(3) 0.0304(16) Uani 1 1 d . . . H47A H 0.7512 0.2728 0.8539 0.037 Uiso 1 1 calc R . . H47B H 0.6859 0.1914 0.8400 0.037 Uiso 1 1 calc R . . C48 C 0.6579(3) 0.2977(5) 0.7645(3) 0.0298(15) Uani 1 1 d . . . H48A H 0.6164 0.2557 0.7326 0.036 Uiso 1 1 calc R . . H48B H 0.6356 0.3453 0.7861 0.036 Uiso 1 1 calc R . . C49 C 0.7527(4) 0.4247(5) 0.7694(3) 0.0324(16) Uani 1 1 d . . . H49A H 0.7637 0.4111 0.8172 0.039 Uiso 1 1 calc R . . H49B H 0.7355 0.4953 0.7595 0.039 Uiso 1 1 calc R . . C50 C 0.8243(4) 0.4112(5) 0.7588(4) 0.0336(17) Uani 1 1 d . . . H50A H 0.8147 0.4346 0.7128 0.040 Uiso 1 1 calc R . . H50B H 0.8642 0.4547 0.7913 0.040 Uiso 1 1 calc R . . C51 C 0.9226(3) 0.3050(5) 0.7553(3) 0.0316(16) Uani 1 1 d . . . H51A H 0.9624 0.3430 0.7911 0.047 Uiso 1 1 calc R . . H51B H 0.9124 0.3356 0.7115 0.047 Uiso 1 1 calc R . . H51C H 0.9391 0.2353 0.7557 0.047 Uiso 1 1 calc R . . C52 C 0.7264(4) 0.0574(5) 0.7933(3) 0.0350(17) Uani 1 1 d . . . H52A H 0.7536 0.0103 0.7768 0.053 Uiso 1 1 calc R . . H52B H 0.6721 0.0536 0.7644 0.053 Uiso 1 1 calc R . . H52C H 0.7355 0.0399 0.8397 0.053 Uiso 1 1 calc R . . C53 C 0.6297(4) 0.4152(5) 0.6738(3) 0.0326(16) Uani 1 1 d . . . H53A H 0.5873 0.3704 0.6485 0.049 Uiso 1 1 calc R . . H53B H 0.6481 0.4463 0.6427 0.049 Uiso 1 1 calc R . . H53C H 0.6129 0.4677 0.6960 0.049 Uiso 1 1 calc R . . C54 C 0.8302(7) 0.7412(11) 0.9083(6) 0.087(3) Uani 1 1 d . . . H54 H 0.7875 0.7040 0.8789 0.104 Uiso 1 1 calc R . . C55 C 0.8268(7) 0.8467(11) 0.9180(6) 0.085(3) Uani 1 1 d . . . H55 H 0.7799 0.8808 0.8962 0.103 Uiso 1 1 calc R . . C56 C 0.8920(8) 0.9017(9) 0.9595(7) 0.090(4) Uani 1 1 d . . . H56 H 0.8893 0.9725 0.9640 0.109 Uiso 1 1 calc R . . C57 C 0.9591(6) 0.8524(9) 0.9932(5) 0.071(3) Uani 1 1 d . . . H57 H 1.0032 0.8880 1.0217 0.085 Uiso 1 1 calc R . . C58 C 0.9613(6) 0.7482(7) 0.9847(5) 0.060(2) Uani 1 1 d . . . H58 H 1.0076 0.7134 1.0078 0.072 Uiso 1 1 calc R . . C59 C 0.8996(6) 0.6962(10) 0.9446(5) 0.077(3) Uani 1 1 d . . . C60 C 0.9009(9) 0.5810(11) 0.9383(9) 0.135(6) Uani 1 1 d . . . H60A H 0.8532 0.5529 0.9357 0.202 Uiso 1 1 calc R . . H60B H 0.9430 0.5534 0.9779 0.202 Uiso 1 1 calc R . . H60C H 0.9074 0.5633 0.8974 0.202 Uiso 1 1 calc R . . N1 N 0.8323(2) 0.1253(4) 0.6451(2) 0.0166(10) Uani 1 1 d . . . N2 N 0.6983(2) 0.0483(4) 0.6399(2) 0.0156(10) Uani 1 1 d . . . N3 N 0.6282(2) 0.2339(4) 0.5757(2) 0.0168(11) Uani 1 1 d . . . N4 N 0.7696(2) 0.2917(4) 0.5867(2) 0.0152(10) Uani 1 1 d . . . N5 N 0.8528(3) 0.3067(4) 0.7669(3) 0.0253(12) Uani 1 1 d . . . N6 N 0.7532(3) 0.1594(4) 0.7917(2) 0.0255(12) Uani 1 1 d . . . N7 N 0.6915(3) 0.3565(4) 0.7254(2) 0.0224(11) Uani 1 1 d . . . O1 O 0.2789(2) -0.0367(3) 0.5875(2) 0.0222(9) Uani 1 1 d . . . Gd1 Gd 0.740509(15) 0.21003(2) 0.668592(14) 0.01590(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 C1 0.011(3) 0.030(4) 0.012(3) -0.002(2) 0.006(2) -0.003(2) C2 0.009(3) 0.027(4) 0.017(3) -0.002(3) 0.007(2) -0.002(2) C3 0.014(3) 0.026(4) 0.018(3) -0.001(3) 0.008(2) 0.005(2) C4 0.020(3) 0.015(3) 0.013(3) -0.005(2) 0.005(2) -0.001(2) C5 0.018(3) 0.018(3) 0.010(3) 0.001(2) 0.005(2) 0.005(2) C6 0.022(3) 0.009(3) 0.015(3) -0.002(2) 0.009(2) 0.004(2) C7 0.025(3) 0.015(3) 0.025(3) 0.001(3) 0.013(3) 0.002(2) C8 0.023(3) 0.027(4) 0.022(3) -0.002(3) 0.016(3) -0.002(3) C9 0.019(3) 0.026(4) 0.013(3) -0.001(2) 0.013(2) -0.001(2) C10 0.016(3) 0.024(3) 0.014(3) -0.006(2) 0.010(2) -0.004(2) C11 0.016(3) 0.023(4) 0.017(3) -0.004(2) 0.010(2) 0.001(2) C12 0.016(3) 0.022(3) 0.019(3) 0.000(2) 0.008(2) 0.003(2) C13 0.020(3) 0.026(4) 0.024(3) 0.005(3) 0.013(3) 0.006(2) C14 0.021(3) 0.017(3) 0.024(3) -0.001(3) 0.015(3) 0.002(2) C15 0.021(3) 0.022(3) 0.011(3) -0.008(2) 0.007(2) -0.002(2) C16 0.023(3) 0.009(3) 0.019(3) 0.001(2) 0.011(2) 0.000(2) C17 0.029(3) 0.009(3) 0.027(3) -0.005(3) 0.015(3) -0.001(2) C18 0.015(3) 0.024(3) 0.026(3) 0.004(3) 0.014(3) -0.007(2) C19 0.017(3) 0.015(3) 0.016(3) -0.003(2) 0.007(2) -0.005(2) C20 0.013(3) 0.018(3) 0.022(3) -0.002(3) 0.012(2) -0.002(2) C21 0.015(3) 0.026(4) 0.026(3) 0.005(3) 0.011(2) -0.005(3) C22 0.018(3) 0.024(4) 0.025(3) 0.010(3) 0.009(2) 0.000(3) C23 0.019(3) 0.023(4) 0.038(4) 0.000(3) 0.014(3) 0.000(3) C24 0.027(3) 0.027(4) 0.022(3) -0.006(3) 0.012(3) 0.000(3) C25 0.018(3) 0.023(3) 0.022(3) 0.002(3) 0.009(2) 0.001(3) C26 0.034(4) 0.033(4) 0.028(4) 0.002(3) 0.013(3) 0.003(3) C27 0.045(4) 0.030(4) 0.046(4) 0.008(3) 0.022(4) 0.014(3) C28 0.042(4) 0.034(4) 0.021(3) 0.004(3) 0.012(3) 0.007(3) C29 0.014(3) 0.021(3) 0.014(3) 0.000(2) 0.009(2) 0.002(2) C30 0.023(3) 0.028(4) 0.024(3) -0.006(3) 0.017(3) -0.004(3) C31 0.021(3) 0.030(4) 0.014(3) -0.005(3) 0.009(2) -0.007(3) C32 0.016(3) 0.032(4) 0.013(3) -0.004(3) 0.003(2) -0.003(2) C33 0.020(3) 0.027(4) 0.020(3) -0.005(3) 0.013(3) 0.001(3) C34 0.019(3) 0.019(3) 0.021(3) -0.006(3) 0.008(2) -0.001(2) C35 0.014(3) 0.026(4) 0.018(3) 0.011(3) 0.007(2) 0.004(2) C36 0.010(3) 0.025(4) 0.022(3) 0.003(3) 0.010(2) 0.004(2) C37 0.013(3) 0.032(4) 0.023(3) 0.005(3) 0.011(2) 0.006(2) C38 0.024(3) 0.027(4) 0.024(3) 0.007(3) 0.012(3) 0.007(3) C39 0.026(3) 0.034(4) 0.021(3) 0.010(3) 0.013(3) 0.017(3) C40 0.026(3) 0.017(3) 0.032(4) 0.001(3) 0.016(3) 0.004(3) C41 0.014(3) 0.020(4) 0.021(3) 0.005(3) 0.010(2) 0.003(2) C42 0.024(3) 0.031(4) 0.020(3) 0.000(3) 0.011(2) -0.001(3) C43 0.054(5) 0.039(4) 0.030(4) 0.016(3) 0.023(3) 0.022(4) C44 0.027(3) 0.022(4) 0.034(4) 0.002(3) 0.011(3) 0.002(3) C45 0.030(4) 0.050(5) 0.020(3) -0.005(3) 0.008(3) -0.002(3) C46 0.044(4) 0.044(5) 0.023(3) 0.008(3) 0.014(3) 0.012(3) C47 0.028(3) 0.043(5) 0.029(3) -0.003(3) 0.021(3) 0.001(3) C48 0.023(3) 0.042(4) 0.031(3) -0.004(3) 0.018(3) 0.002(3) C49 0.036(4) 0.039(4) 0.031(4) -0.011(3) 0.023(3) -0.002(3) C50 0.034(4) 0.036(4) 0.040(4) -0.019(3) 0.023(3) -0.015(3) C51 0.018(3) 0.045(4) 0.032(4) -0.015(3) 0.011(3) -0.006(3) C52 0.060(5) 0.033(4) 0.022(3) -0.001(3) 0.027(3) -0.003(3) C53 0.040(4) 0.030(4) 0.034(4) -0.007(3) 0.021(3) 0.011(3) C54 0.084(8) 0.114(11) 0.076(8) 0.014(7) 0.048(7) 0.008(7) C55 0.090(9) 0.107(10) 0.074(8) 0.037(7) 0.049(7) 0.017(8) C56 0.121(11) 0.073(8) 0.112(10) 0.034(7) 0.083(9) 0.025(8) C57 0.067(7) 0.093(9) 0.076(7) 0.004(6) 0.053(6) 0.011(6) C58 0.068(6) 0.065(7) 0.060(6) -0.002(5) 0.038(5) 0.017(5) C59 0.072(7) 0.123(10) 0.048(5) 0.005(6) 0.035(5) 0.014(7) C60 0.187(16) 0.117(12) 0.180(16) -0.065(11) 0.155(14) -0.058(10) N1 0.017(2) 0.019(3) 0.016(2) 0.002(2) 0.008(2) -0.003(2) N2 0.009(2) 0.027(3) 0.012(2) -0.001(2) 0.0056(19) -0.0015(19) N3 0.008(2) 0.026(3) 0.018(2) 0.002(2) 0.0064(19) -0.0008(19) N4 0.009(2) 0.017(2) 0.020(2) 0.002(2) 0.0056(18) 0.001(2) N5 0.026(3) 0.032(3) 0.025(3) -0.006(2) 0.017(2) -0.009(2) N6 0.037(3) 0.026(3) 0.018(3) 0.002(2) 0.017(2) 0.004(2) N7 0.022(3) 0.027(3) 0.020(3) -0.007(2) 0.010(2) 0.001(2) O1 0.015(2) 0.033(3) 0.022(2) -0.0050(19) 0.0114(17) -0.0077(17) Gd1 0.01437(14) 0.02176(18) 0.01424(14) -0.00103(14) 0.00861(10) 0.00023(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.366(7) . ? C1 C2 1.421(8) . ? C1 C19 1.432(8) . ? C2 C3 1.370(8) . ? C2 H2 0.9500 . ? C3 C4 1.423(8) . ? C3 H3 0.9500 . ? C4 N1 1.377(7) . ? C4 C5 1.413(8) . ? C5 C6 1.402(8) . ? C5 C20 1.508(8) . ? C6 N2 1.409(7) . ? C6 C7 1.419(8) . ? C7 C8 1.362(8) . ? C7 H7 0.9500 . ? C8 C9 1.431(9) . ? C8 H8 0.9500 . ? C9 N2 1.389(7) . ? C9 C10 1.426(8) . ? C10 C11 1.411(8) . ? C10 C29 1.500(7) . ? C11 N3 1.370(7) . ? C11 C12 1.448(8) . ? C12 C13 1.356(8) . ? C12 H12 0.9500 . ? C13 C14 1.450(8) . ? C13 H13 0.9500 . ? C14 N3 1.396(7) . ? C14 C15 1.403(8) . ? C15 C16 1.416(8) . ? C15 C36 1.503(8) . ? C16 N4 1.376(7) . ? C16 C17 1.418(8) . ? C17 C18 1.388(8) . ? C17 H17 0.9500 . ? C18 C19 1.418(8) . ? C18 H18 0.9500 . ? C19 N4 1.371(7) . ? C20 C21 1.384(8) . ? C20 C25 1.403(8) . ? C21 C22 1.399(9) . ? C21 C26 1.517(9) . ? C22 C23 1.378(9) . ? C22 H22 0.9500 . ? C23 C24 1.401(9) . ? C23 C27 1.508(9) . ? C24 C25 1.367(9) . ? C24 H24 0.9500 . ? C25 C28 1.519(8) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C34 1.390(8) . ? C29 C30 1.391(8) . ? C30 C31 1.390(8) . ? C30 H30 0.9500 . ? C31 C35 1.374(8) . ? C31 H31 0.9500 . ? C32 O1 1.418(7) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.386(8) . ? C33 C35 1.390(8) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? C35 O1 1.373(7) . ? C36 C41 1.393(9) . ? C36 C37 1.412(8) . ? C37 C38 1.385(8) . ? C37 C42 1.500(9) . ? C38 C39 1.372(9) . ? C38 H38 0.9500 . ? C39 C40 1.390(9) . ? C39 C43 1.502(9) . ? C40 C41 1.385(8) . ? C40 H40 0.9500 . ? C41 C44 1.509(9) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 N5 1.482(8) . ? C45 C46 1.510(10) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 N6 1.493(9) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 N6 1.488(8) . ? C47 C48 1.516(9) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 N7 1.493(8) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 N7 1.487(8) . ? C49 C50 1.514(9) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 N5 1.480(9) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 N5 1.481(8) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 N6 1.459(9) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 N7 1.481(8) . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 C59 1.384(15) . ? C54 C55 1.425(17) . ? C54 H54 0.9500 . ? C55 C56 1.418(17) . ? C55 H55 0.9500 . ? C56 C57 1.370(15) . ? C56 H56 0.9500 . ? C57 C58 1.400(14) . ? C57 H57 0.9500 . ? C58 C59 1.346(14) . ? C58 H58 0.9500 . ? C59 C60 1.539(17) . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? N1 Gd1 2.344(5) . ? N2 Gd1 2.294(5) . ? N3 Gd1 2.300(4) . ? N4 Gd1 2.350(4) . ? N5 Gd1 2.668(5) . ? N6 Gd1 2.676(5) . ? N7 Gd1 2.688(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 109.1(5) . . ? N1 C1 C19 115.6(5) . . ? C2 C1 C19 133.2(5) . . ? C3 C2 C1 106.9(5) . . ? C3 C2 H2 126.5 . . ? C1 C2 H2 126.5 . . ? C2 C3 C4 107.7(5) . . ? C2 C3 H3 126.2 . . ? C4 C3 H3 126.2 . . ? N1 C4 C5 121.0(5) . . ? N1 C4 C3 108.2(5) . . ? C5 C4 C3 129.3(5) . . ? C6 C5 C4 125.4(5) . . ? C6 C5 C20 116.8(5) . . ? C4 C5 C20 117.0(5) . . ? C5 C6 N2 123.9(5) . . ? C5 C6 C7 127.4(5) . . ? N2 C6 C7 108.3(5) . . ? C8 C7 C6 108.9(5) . . ? C8 C7 H7 125.6 . . ? C6 C7 H7 125.6 . . ? C7 C8 C9 107.0(5) . . ? C7 C8 H8 126.5 . . ? C9 C8 H8 126.5 . . ? N2 C9 C10 123.1(5) . . ? N2 C9 C8 109.5(5) . . ? C10 C9 C8 127.2(5) . . ? C11 C10 C9 125.8(5) . . ? C11 C10 C29 117.2(5) . . ? C9 C10 C29 116.4(5) . . ? N3 C11 C10 125.0(5) . . ? N3 C11 C12 108.4(5) . . ? C10 C11 C12 125.9(5) . . ? C13 C12 C11 107.7(5) . . ? C13 C12 H12 126.1 . . ? C11 C12 H12 126.1 . . ? C12 C13 C14 107.9(5) . . ? C12 C13 H13 126.0 . . ? C14 C13 H13 126.0 . . ? N3 C14 C15 125.7(5) . . ? N3 C14 C13 107.4(5) . . ? C15 C14 C13 126.6(5) . . ? C14 C15 C16 123.6(5) . . ? C14 C15 C36 120.3(5) . . ? C16 C15 C36 115.3(5) . . ? N4 C16 C15 122.0(5) . . ? N4 C16 C17 108.1(5) . . ? C15 C16 C17 128.9(5) . . ? C18 C17 C16 108.1(5) . . ? C18 C17 H17 125.9 . . ? C16 C17 H17 125.9 . . ? C17 C18 C19 105.9(5) . . ? C17 C18 H18 127.0 . . ? C19 C18 H18 127.0 . . ? N4 C19 C18 109.7(5) . . ? N4 C19 C1 114.4(5) . . ? C18 C19 C1 132.8(5) . . ? C21 C20 C25 119.4(5) . . ? C21 C20 C5 121.3(5) . . ? C25 C20 C5 119.2(5) . . ? C20 C21 C22 119.6(6) . . ? C20 C21 C26 121.6(6) . . ? C22 C21 C26 118.7(5) . . ? C23 C22 C21 121.5(6) . . ? C23 C22 H22 119.3 . . ? C21 C22 H22 119.3 . . ? C22 C23 C24 117.8(6) . . ? C22 C23 C27 121.9(6) . . ? C24 C23 C27 120.2(6) . . ? C25 C24 C23 121.8(6) . . ? C25 C24 H24 119.1 . . ? C23 C24 H24 119.1 . . ? C24 C25 C20 119.8(5) . . ? C24 C25 C28 120.1(5) . . ? C20 C25 C28 120.1(5) . . ? C21 C26 H26A 109.5 . . ? C21 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C21 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C27 H27A 109.5 . . ? C23 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C23 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C34 C29 C30 117.4(5) . . ? C34 C29 C10 120.9(5) . . ? C30 C29 C10 121.7(5) . . ? C31 C30 C29 121.8(5) . . ? C31 C30 H30 119.1 . . ? C29 C30 H30 119.1 . . ? C35 C31 C30 119.8(5) . . ? C35 C31 H31 120.1 . . ? C30 C31 H31 120.1 . . ? O1 C32 H32A 109.5 . . ? O1 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? O1 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34 C33 C35 120.2(5) . . ? C34 C33 H33 119.9 . . ? C35 C33 H33 119.9 . . ? C33 C34 C29 121.2(5) . . ? C33 C34 H34 119.4 . . ? C29 C34 H34 119.4 . . ? O1 C35 C31 123.9(5) . . ? O1 C35 C33 116.5(5) . . ? C31 C35 C33 119.5(5) . . ? C41 C36 C37 119.0(5) . . ? C41 C36 C15 120.4(5) . . ? C37 C36 C15 120.2(5) . . ? C38 C37 C36 118.5(6) . . ? C38 C37 C42 119.8(6) . . ? C36 C37 C42 121.7(5) . . ? C39 C38 C37 123.1(6) . . ? C39 C38 H38 118.5 . . ? C37 C38 H38 118.5 . . ? C38 C39 C40 117.7(6) . . ? C38 C39 C43 120.4(6) . . ? C40 C39 C43 121.9(6) . . ? C41 C40 C39 121.4(6) . . ? C41 C40 H40 119.3 . . ? C39 C40 H40 119.3 . . ? C40 C41 C36 120.1(6) . . ? C40 C41 C44 119.7(5) . . ? C36 C41 C44 120.2(5) . . ? C37 C42 H42A 109.5 . . ? C37 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C37 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C39 C43 H43A 109.5 . . ? C39 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C39 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? N5 C45 C46 112.6(5) . . ? N5 C45 H45A 109.1 . . ? C46 C45 H45A 109.1 . . ? N5 C45 H45B 109.1 . . ? C46 C45 H45B 109.1 . . ? H45A C45 H45B 107.8 . . ? N6 C46 C45 113.5(5) . . ? N6 C46 H46A 108.9 . . ? C45 C46 H46A 108.9 . . ? N6 C46 H46B 108.9 . . ? C45 C46 H46B 108.9 . . ? H46A C46 H46B 107.7 . . ? N6 C47 C48 112.8(5) . . ? N6 C47 H47A 109.0 . . ? C48 C47 H47A 109.0 . . ? N6 C47 H47B 109.0 . . ? C48 C47 H47B 109.0 . . ? H47A C47 H47B 107.8 . . ? N7 C48 C47 114.4(5) . . ? N7 C48 H48A 108.7 . . ? C47 C48 H48A 108.7 . . ? N7 C48 H48B 108.7 . . ? C47 C48 H48B 108.7 . . ? H48A C48 H48B 107.6 . . ? N7 C49 C50 111.8(5) . . ? N7 C49 H49A 109.3 . . ? C50 C49 H49A 109.3 . . ? N7 C49 H49B 109.3 . . ? C50 C49 H49B 109.3 . . ? H49A C49 H49B 107.9 . . ? N5 C50 C49 114.6(5) . . ? N5 C50 H50A 108.6 . . ? C49 C50 H50A 108.6 . . ? N5 C50 H50B 108.6 . . ? C49 C50 H50B 108.6 . . ? H50A C50 H50B 107.6 . . ? N5 C51 H51A 109.5 . . ? N5 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? N5 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? N6 C52 H52A 109.5 . . ? N6 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? N6 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? N7 C53 H53A 109.5 . . ? N7 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? N7 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C59 C54 C55 115.9(13) . . ? C59 C54 H54 122.1 . . ? C55 C54 H54 122.1 . . ? C56 C55 C54 121.2(12) . . ? C56 C55 H55 119.4 . . ? C54 C55 H55 119.4 . . ? C57 C56 C55 119.7(12) . . ? C57 C56 H56 120.2 . . ? C55 C56 H56 120.2 . . ? C56 C57 C58 118.5(11) . . ? C56 C57 H57 120.7 . . ? C58 C57 H57 120.7 . . ? C59 C58 C57 121.8(10) . . ? C59 C58 H58 119.1 . . ? C57 C58 H58 119.1 . . ? C58 C59 C54 122.9(12) . . ? C58 C59 C60 121.7(11) . . ? C54 C59 C60 115.4(13) . . ? C59 C60 H60A 109.5 . . ? C59 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C59 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C1 N1 C4 107.8(5) . . ? C1 N1 Gd1 118.1(4) . . ? C4 N1 Gd1 134.1(4) . . ? C9 N2 C6 106.3(4) . . ? C9 N2 Gd1 119.8(4) . . ? C6 N2 Gd1 129.7(3) . . ? C11 N3 C14 108.4(4) . . ? C11 N3 Gd1 117.5(4) . . ? C14 N3 Gd1 128.7(3) . . ? C19 N4 C16 107.8(4) . . ? C19 N4 Gd1 118.2(3) . . ? C16 N4 Gd1 134.0(3) . . ? C50 N5 C51 108.6(5) . . ? C50 N5 C45 112.7(5) . . ? C51 N5 C45 108.6(5) . . ? C50 N5 Gd1 102.5(4) . . ? C51 N5 Gd1 111.0(4) . . ? C45 N5 Gd1 113.4(4) . . ? C52 N6 C47 109.3(5) . . ? C52 N6 C46 108.9(5) . . ? C47 N6 C46 111.1(5) . . ? C52 N6 Gd1 111.9(4) . . ? C47 N6 Gd1 113.0(4) . . ? C46 N6 Gd1 102.4(4) . . ? C53 N7 C49 110.3(5) . . ? C53 N7 C48 107.4(5) . . ? C49 N7 C48 112.1(5) . . ? C53 N7 Gd1 111.3(3) . . ? C49 N7 Gd1 113.3(3) . . ? C48 N7 Gd1 102.0(4) . . ? C35 O1 C32 116.3(4) . . ? N2 Gd1 N3 77.78(16) . . ? N2 Gd1 N1 73.09(15) . . ? N3 Gd1 N1 113.92(16) . . ? N2 Gd1 N4 113.49(16) . . ? N3 Gd1 N4 73.11(15) . . ? N1 Gd1 N4 66.97(15) . . ? N2 Gd1 N5 138.69(16) . . ? N3 Gd1 N5 143.18(17) . . ? N1 Gd1 N5 87.89(16) . . ? N4 Gd1 N5 90.62(15) . . ? N2 Gd1 N6 84.84(16) . . ? N3 Gd1 N6 125.02(16) . . ? N1 Gd1 N6 109.80(15) . . ? N4 Gd1 N6 157.91(16) . . ? N5 Gd1 N6 67.29(16) . . ? N2 Gd1 N7 130.47(15) . . ? N3 Gd1 N7 85.17(15) . . ? N1 Gd1 N7 154.03(15) . . ? N4 Gd1 N7 105.03(16) . . ? N5 Gd1 N7 67.06(15) . . ? N6 Gd1 N7 67.81(15) . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 2.159 _refine_diff_density_min -1.313 _refine_diff_density_rms 0.153 data_shelxl2 _database_code_depnum_ccdc_archive 'CCDC 908246' #TrackingRef '16815_web_deposit_cif_file_1_HeatherLouisaBuckley_1357921663.hb051.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common HB051 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H77 N4 O9 Tb' _chemical_formula_weight 1157.9 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.6378(8) _cell_length_b 15.7546(10) _cell_length_c 15.8507(11) _cell_angle_alpha 95.090(3) _cell_angle_beta 101.785(3) _cell_angle_gamma 100.993(3) _cell_volume 2768.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9331 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 25.46 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.388 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1204 _exptl_absorpt_coefficient_mu 1.337 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9006 _exptl_absorpt_correction_T_max 0.9737 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_reflns_number 101764 _diffrn_reflns_av_R_equivalents 0.0498 _diffrn_reflns_av_sigmaI/netI 0.0282 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 25.52 _reflns_number_total 10139 _reflns_number_gt 8931 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution SIR-2004 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ORTEP-32 _computing_publication_material WinGX _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^)+(0.0783P)^2^+25.7994P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10139 _refine_ls_number_parameters 640 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0759 _refine_ls_R_factor_gt 0.0643 _refine_ls_wR_factor_ref 0.1720 _refine_ls_wR_factor_gt 0.1580 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1799(6) 0.6179(4) 0.7785(4) 0.0235(12) Uani 1 1 d . . . C2 C 0.1078(6) 0.5838(4) 0.8352(4) 0.0281(13) Uani 1 1 d . . . H2 H 0.0629 0.5257 0.8296 0.034 Uiso 1 1 calc R . . C3 C 0.1151(6) 0.6502(4) 0.8992(4) 0.0320(15) Uani 1 1 d . . . H3 H 0.0771 0.6465 0.9468 0.038 Uiso 1 1 calc R . . C4 C 0.1912(6) 0.7268(4) 0.8810(4) 0.0281(14) Uani 1 1 d . . . C5 C 0.2047(6) 0.8153(4) 0.9138(4) 0.0294(14) Uani 1 1 d . . . C6 C 0.2496(6) 0.8852(4) 0.8715(4) 0.0301(14) Uani 1 1 d . . . C7 C 0.2493(7) 0.9752(4) 0.8936(5) 0.0335(15) Uani 1 1 d . . . H7 H 0.2277 0.9994 0.9436 0.040 Uiso 1 1 calc R . . C8 C 0.2849(6) 1.0199(4) 0.8311(4) 0.0309(14) Uani 1 1 d . . . H8 H 0.2938 1.0810 0.8300 0.037 Uiso 1 1 calc R . . C9 C 0.3072(6) 0.9578(4) 0.7660(4) 0.0248(13) Uani 1 1 d . . . C10 C 0.3334(5) 0.9749(4) 0.6860(4) 0.0238(12) Uani 1 1 d . . . C11 C 0.3317(5) 0.9123(4) 0.6168(4) 0.0227(12) Uani 1 1 d . . . C12 C 0.3328(5) 0.9265(4) 0.5280(4) 0.0226(12) Uani 1 1 d . . . H12 H 0.3472 0.9816 0.5076 0.027 Uiso 1 1 calc R . . C13 C 0.3098(6) 0.8477(4) 0.4789(4) 0.0237(12) Uani 1 1 d . . . H13 H 0.3051 0.8380 0.4181 0.028 Uiso 1 1 calc R . . C14 C 0.2938(5) 0.7813(4) 0.5348(4) 0.0208(12) Uani 1 1 d . . . C15 C 0.2529(5) 0.6908(4) 0.5093(4) 0.0202(12) Uani 1 1 d . . . C16 C 0.2255(5) 0.6311(4) 0.5682(4) 0.0202(12) Uani 1 1 d . . . C17 C 0.1490(5) 0.5454(4) 0.5485(4) 0.0223(12) Uani 1 1 d . . . H17 H 0.1199 0.5116 0.4928 0.027 Uiso 1 1 calc R . . C18 C 0.1258(6) 0.5215(4) 0.6262(4) 0.0232(12) Uani 1 1 d . . . H18 H 0.0772 0.4685 0.6344 0.028 Uiso 1 1 calc R . . C19 C 0.1893(5) 0.5923(4) 0.6917(4) 0.0212(12) Uani 1 1 d . . . C20 C 0.1536(6) 0.8355(4) 0.9908(4) 0.0284(14) Uani 1 1 d . . . C21 C 0.2163(7) 0.8290(5) 1.0751(5) 0.0345(15) Uani 1 1 d . . . C22 C 0.1649(8) 0.8451(5) 1.1450(5) 0.0440(18) Uani 1 1 d . . . H22 H 0.2067 0.8395 1.2016 0.053 Uiso 1 1 calc R . . C23 C 0.0554(8) 0.8688(5) 1.1352(5) 0.0422(18) Uani 1 1 d . . . C24 C -0.0051(7) 0.8751(5) 1.0518(5) 0.0420(18) Uani 1 1 d . . . H24 H -0.0806 0.8915 1.0439 0.050 Uiso 1 1 calc R . . C25 C 0.0414(7) 0.8581(5) 0.9793(5) 0.0385(16) Uani 1 1 d . . . C26 C 0.3367(8) 0.8054(7) 1.0896(6) 0.057(2) Uani 1 1 d . . . H26A H 0.3572 0.7891 1.1482 0.086 Uiso 1 1 calc R . . H26B H 0.3974 0.8555 1.0837 0.086 Uiso 1 1 calc R . . H26C H 0.3343 0.7561 1.0466 0.086 Uiso 1 1 calc R . . C27 C -0.0003(10) 0.8857(7) 1.2119(6) 0.062(3) Uani 1 1 d . . . H27A H 0.0456 0.8673 1.2635 0.093 Uiso 1 1 calc R . . H27B H -0.0836 0.8526 1.1988 0.093 Uiso 1 1 calc R . . H27C H 0.0010 0.9481 1.2230 0.093 Uiso 1 1 calc R . . C28 C -0.0318(8) 0.8632(6) 0.8899(5) 0.052(2) Uani 1 1 d . . . H28A H 0.0056 0.9149 0.8674 0.077 Uiso 1 1 calc R . . H28B H -0.1136 0.8673 0.8940 0.077 Uiso 1 1 calc R . . H28C H -0.0350 0.8108 0.8506 0.077 Uiso 1 1 calc R . . C29 C 0.3464(6) 1.0679(4) 0.6670(4) 0.0244(13) Uani 1 1 d . . . C30 C 0.2486(6) 1.1058(4) 0.6545(5) 0.0299(14) Uani 1 1 d . . . H30 H 0.1735 1.0734 0.6601 0.036 Uiso 1 1 calc R . . C31 C 0.2563(6) 1.1907(4) 0.6339(5) 0.0322(15) Uani 1 1 d . . . H31 H 0.1873 1.2156 0.6252 0.039 Uiso 1 1 calc R . . C32 C 0.3659(6) 1.2378(4) 0.6264(5) 0.0293(14) Uani 1 1 d . . . C33 C 0.4661(6) 1.2017(4) 0.6401(5) 0.0351(16) Uani 1 1 d . . . H33 H 0.5418 1.2347 0.6361 0.042 Uiso 1 1 calc R . . C34 C 0.4555(6) 1.1171(4) 0.6595(5) 0.0317(15) Uani 1 1 d . . . H34 H 0.5244 1.0921 0.6679 0.038 Uiso 1 1 calc R . . C35 C 0.2816(8) 1.3587(5) 0.5843(6) 0.049(2) Uani 1 1 d . . . H35A H 0.2251 1.3217 0.5342 0.073 Uiso 1 1 calc R . . H35B H 0.3062 1.4173 0.5689 0.073 Uiso 1 1 calc R . . H35C H 0.2427 1.3623 0.6334 0.073 Uiso 1 1 calc R . . C36 C 0.2246(5) 0.6578(4) 0.4141(4) 0.0216(12) Uani 1 1 d . . . C37 C 0.2935(6) 0.6044(4) 0.3807(4) 0.0283(14) Uani 1 1 d . . . C38 C 0.2706(7) 0.5808(4) 0.2905(5) 0.0353(16) Uani 1 1 d . . . H38 H 0.3180 0.5455 0.2680 0.042 Uiso 1 1 calc R . . C39 C 0.1819(7) 0.6067(4) 0.2332(5) 0.0381(17) Uani 1 1 d . . . C40 C 0.1106(7) 0.6551(4) 0.2682(4) 0.0335(15) Uani 1 1 d . . . H40 H 0.0469 0.6716 0.2299 0.040 Uiso 1 1 calc R . . C41 C 0.1288(6) 0.6803(4) 0.3570(4) 0.0255(13) Uani 1 1 d . . . C42 C 0.3890(7) 0.5714(4) 0.4401(5) 0.0367(16) Uani 1 1 d . . . H42A H 0.4344 0.6183 0.4864 0.055 Uiso 1 1 calc R . . H42B H 0.4437 0.5521 0.4066 0.055 Uiso 1 1 calc R . . H42C H 0.3511 0.5222 0.4658 0.055 Uiso 1 1 calc R . . C43 C 0.1617(10) 0.5832(6) 0.1361(5) 0.058(2) Uani 1 1 d . . . H43A H 0.1956 0.6341 0.1107 0.086 Uiso 1 1 calc R . . H43B H 0.0753 0.5650 0.1105 0.086 Uiso 1 1 calc R . . H43C H 0.2011 0.5353 0.1239 0.086 Uiso 1 1 calc R . . C44 C 0.0431(6) 0.7277(4) 0.3902(4) 0.0298(14) Uani 1 1 d . . . H44A H 0.0798 0.7901 0.4042 0.045 Uiso 1 1 calc R . . H44B H 0.0250 0.7047 0.4426 0.045 Uiso 1 1 calc R . . H44C H -0.0313 0.7192 0.3454 0.045 Uiso 1 1 calc R . . C45 C 0.575(2) 0.9260(16) 0.9079(15) 0.162(8) Uiso 1 1 d . . . H45A H 0.6456 0.9735 0.9350 0.195 Uiso 1 1 calc R . . H45B H 0.5014 0.9459 0.9142 0.195 Uiso 1 1 calc R . . C46 C 0.584(2) 0.8389(16) 0.9547(17) 0.175(9) Uiso 1 1 d . . . H46A H 0.6596 0.8193 0.9529 0.210 Uiso 1 1 calc R . . H46B H 0.5750 0.8467 1.0155 0.210 Uiso 1 1 calc R . . C47 C 0.495(2) 0.6906(16) 0.9320(16) 0.178(9) Uiso 1 1 d . . . H47A H 0.5326 0.6591 0.8930 0.266 Uiso 1 1 calc R . . H47B H 0.4119 0.6593 0.9264 0.266 Uiso 1 1 calc R . . H47C H 0.5399 0.6946 0.9921 0.266 Uiso 1 1 calc R . . C48 C 0.4654(14) 0.5645(10) 0.7560(10) 0.104(4) Uiso 1 1 d . . . H48A H 0.4693 0.5533 0.6949 0.156 Uiso 1 1 calc R . . H48B H 0.3837 0.5411 0.7621 0.156 Uiso 1 1 calc R . . H48C H 0.5220 0.5361 0.7918 0.156 Uiso 1 1 calc R . . C49 C 0.630(18) 0.691(13) 0.799(8) 1.4(2) Uiso 1 1 d D . . H49A H 0.6514 0.7392 0.8477 1.621 Uiso 1 1 calc R . . H49B H 0.6778 0.6469 0.8150 1.621 Uiso 1 1 calc R . . C50 C 0.654(6) 0.724(4) 0.719(4) 0.45(4) Uiso 1 1 d D . . H50A H 0.6601 0.6740 0.6790 0.536 Uiso 1 1 calc R . . H50B H 0.7349 0.7637 0.7347 0.536 Uiso 1 1 calc R . . C51 C 0.5887(13) 0.7978(10) 0.5916(9) 0.093(4) Uiso 1 1 d . . . H51A H 0.6497 0.8522 0.6029 0.140 Uiso 1 1 calc R . . H51B H 0.5130 0.8074 0.5576 0.140 Uiso 1 1 calc R . . H51C H 0.6157 0.7526 0.5589 0.140 Uiso 1 1 calc R . . C52 C 0.6482(19) 0.9260(14) 0.7443(14) 0.146(7) Uiso 1 1 d . . . H52A H 0.6431 0.9851 0.7316 0.220 Uiso 1 1 calc R . . H52B H 0.6210 0.8853 0.6902 0.220 Uiso 1 1 calc R . . H52C H 0.7316 0.9249 0.7708 0.220 Uiso 1 1 calc R . . C53 C 0.870(2) 0.6360(10) 0.6673(13) 0.187(13) Uani 1 1 d . . . H53A H 0.7941 0.5980 0.6359 0.280 Uiso 1 1 calc R . . H53B H 0.8737 0.6416 0.7298 0.280 Uiso 1 1 calc R . . H53C H 0.9372 0.6107 0.6555 0.280 Uiso 1 1 calc R . . C54 C 0.9999(9) 0.7824(9) 0.6484(6) 0.135(8) Uani 1 1 d D . . H54A H 1.0340 0.8087 0.7097 0.162 Uiso 1 1 calc R . . H54B H 1.0583 0.7523 0.6277 0.162 Uiso 1 1 calc R . . C55 C 0.9691(15) 0.8491(8) 0.5927(10) 0.098(5) Uani 1 1 d D . . H55A H 1.0419 0.8823 0.5780 0.117 Uiso 1 1 calc R . . H55B H 0.9107 0.8215 0.5382 0.117 Uiso 1 1 calc R . . C56 C 0.904(3) 0.9598(19) 0.5819(18) 0.47(4) Uani 1 1 d . . . H56A H 0.8683 1.0074 0.6010 0.704 Uiso 1 1 calc R . . H56B H 0.8518 0.9263 0.5281 0.704 Uiso 1 1 calc R . . H56C H 0.9831 0.9839 0.5713 0.704 Uiso 1 1 calc R . . C57 C 0.576(4) 0.6531(12) 0.1683(13) 0.241(19) Uani 1 1 d . . . H57A H 0.5902 0.6231 0.2198 0.362 Uiso 1 1 calc R . . H57B H 0.4980 0.6696 0.1613 0.362 Uiso 1 1 calc R . . H57C H 0.6397 0.7057 0.1754 0.362 Uiso 1 1 calc R . . C58 C 0.716(2) 0.606(2) 0.1174(12) 0.210(15) Uani 1 1 d D . . H58A H 0.7632 0.6655 0.1190 0.252 Uiso 1 1 calc R . . H58B H 0.7465 0.5816 0.1711 0.252 Uiso 1 1 calc R . . C59 C 0.714(3) 0.5479(18) 0.0377(17) 0.72(8) Uani 1 1 d D . . H59A H 0.7781 0.5145 0.0456 0.859 Uiso 1 1 calc R . . H59B H 0.6344 0.5081 0.0137 0.859 Uiso 1 1 calc R . . C60 C 0.8441(17) 0.6496(12) -0.0041(18) 0.180(12) Uani 1 1 d . . . H60A H 0.8519 0.7054 -0.0276 0.271 Uiso 1 1 calc R . . H60B H 0.8788 0.6095 -0.0371 0.271 Uiso 1 1 calc R . . H60C H 0.8867 0.6593 0.0571 0.271 Uiso 1 1 calc R . . N1 N 0.2344(5) 0.7031(3) 0.8101(3) 0.0277(12) Uani 1 1 d . . . N2 N 0.2894(5) 0.8768(3) 0.7942(3) 0.0256(11) Uani 1 1 d . . . N3 N 0.3132(5) 0.8232(3) 0.6195(3) 0.0213(10) Uani 1 1 d . . . N4 N 0.2524(4) 0.6553(3) 0.6553(3) 0.0211(10) Uani 1 1 d . . . O1 O 0.3838(5) 1.3224(3) 0.6077(4) 0.0433(13) Uani 1 1 d . . . O2 O 0.5714(6) 0.7717(5) 0.6681(5) 0.0684(19) Uani 1 1 d . . . O3 O 0.4941(6) 0.6492(4) 0.7816(5) 0.070(2) Uani 1 1 d . . . O4 O 0.5725(7) 0.9003(5) 0.8038(6) 0.081(2) Uani 1 1 d . . . O5 O 0.4955(6) 0.7896(7) 0.9057(5) 0.091(3) Uani 1 1 d . . . O6 O 0.8799(8) 0.7201(5) 0.6390(10) 0.149(6) Uani 1 1 d . . . O7 O 0.9164(10) 0.9067(7) 0.6443(7) 0.109(3) Uani 1 1 d . . . O8 O 0.5768(11) 0.6020(9) 0.1006(8) 0.126(5) Uani 1 1 d . . . O9 O 0.7361(14) 0.6176(17) -0.010(2) 0.39(2) Uani 1 1 d . . . Tb1 Tb 0.38517(3) 0.771553(17) 0.747337(19) 0.02570(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.031(3) 0.014(3) 0.025(3) 0.005(2) 0.007(3) 0.002(2) C2 0.034(3) 0.019(3) 0.032(3) 0.010(3) 0.008(3) 0.004(3) C3 0.044(4) 0.024(3) 0.033(4) 0.014(3) 0.013(3) 0.010(3) C4 0.039(4) 0.021(3) 0.027(3) 0.009(2) 0.011(3) 0.005(3) C5 0.039(4) 0.026(3) 0.024(3) 0.005(3) 0.011(3) 0.005(3) C6 0.039(4) 0.021(3) 0.031(3) 0.002(3) 0.011(3) 0.005(3) C7 0.047(4) 0.021(3) 0.035(4) -0.002(3) 0.017(3) 0.007(3) C8 0.044(4) 0.014(3) 0.033(3) -0.003(2) 0.010(3) 0.002(3) C9 0.029(3) 0.013(3) 0.030(3) 0.002(2) 0.006(3) -0.001(2) C10 0.025(3) 0.016(3) 0.031(3) 0.004(2) 0.008(3) 0.002(2) C11 0.022(3) 0.013(3) 0.034(3) 0.006(2) 0.008(2) 0.002(2) C12 0.028(3) 0.013(3) 0.031(3) 0.007(2) 0.014(3) 0.005(2) C13 0.031(3) 0.016(3) 0.029(3) 0.011(2) 0.018(3) 0.005(2) C14 0.026(3) 0.016(3) 0.025(3) 0.006(2) 0.012(2) 0.007(2) C15 0.025(3) 0.012(3) 0.027(3) 0.006(2) 0.010(2) 0.004(2) C16 0.022(3) 0.014(3) 0.026(3) 0.002(2) 0.007(2) 0.007(2) C17 0.028(3) 0.012(3) 0.026(3) 0.002(2) 0.006(2) 0.003(2) C18 0.030(3) 0.012(3) 0.029(3) 0.006(2) 0.008(3) 0.004(2) C19 0.027(3) 0.013(3) 0.026(3) 0.006(2) 0.008(2) 0.005(2) C20 0.038(4) 0.019(3) 0.030(3) 0.002(2) 0.013(3) 0.003(3) C21 0.047(4) 0.032(4) 0.033(4) 0.007(3) 0.021(3) 0.014(3) C22 0.064(5) 0.046(4) 0.030(4) 0.014(3) 0.018(4) 0.021(4) C23 0.066(5) 0.032(4) 0.042(4) 0.011(3) 0.033(4) 0.018(4) C24 0.045(4) 0.037(4) 0.055(5) 0.013(3) 0.027(4) 0.016(3) C25 0.048(4) 0.029(4) 0.043(4) 0.009(3) 0.020(3) 0.008(3) C26 0.061(5) 0.084(7) 0.038(4) 0.008(4) 0.019(4) 0.034(5) C27 0.085(7) 0.065(6) 0.056(6) 0.023(5) 0.043(5) 0.032(5) C28 0.050(5) 0.065(6) 0.042(5) 0.011(4) 0.008(4) 0.021(4) C29 0.031(3) 0.013(3) 0.028(3) 0.000(2) 0.009(3) 0.000(2) C30 0.027(3) 0.018(3) 0.045(4) 0.004(3) 0.010(3) 0.002(2) C31 0.027(3) 0.020(3) 0.053(4) 0.006(3) 0.012(3) 0.009(3) C32 0.037(4) 0.011(3) 0.045(4) 0.009(3) 0.020(3) 0.003(2) C33 0.029(3) 0.020(3) 0.059(5) 0.015(3) 0.015(3) 0.003(3) C34 0.028(3) 0.019(3) 0.052(4) 0.012(3) 0.014(3) 0.007(3) C35 0.051(5) 0.023(4) 0.082(6) 0.028(4) 0.022(4) 0.015(3) C36 0.027(3) 0.011(3) 0.030(3) 0.006(2) 0.014(3) 0.001(2) C37 0.037(3) 0.013(3) 0.039(4) 0.005(3) 0.022(3) 0.001(2) C38 0.057(5) 0.016(3) 0.039(4) 0.000(3) 0.033(4) 0.003(3) C39 0.061(5) 0.022(3) 0.028(4) 0.000(3) 0.019(3) -0.007(3) C40 0.044(4) 0.029(3) 0.026(3) 0.010(3) 0.010(3) -0.002(3) C41 0.034(3) 0.018(3) 0.025(3) 0.006(2) 0.010(3) 0.000(2) C42 0.041(4) 0.023(3) 0.057(5) 0.011(3) 0.027(4) 0.017(3) C43 0.088(7) 0.047(5) 0.034(4) -0.001(4) 0.033(4) -0.010(5) C44 0.029(3) 0.030(3) 0.029(3) 0.006(3) 0.003(3) 0.009(3) C53 0.26(2) 0.068(9) 0.172(18) -0.026(10) -0.119(18) 0.081(13) C54 0.039(5) 0.31(2) 0.048(6) -0.065(10) -0.018(5) 0.086(10) C55 0.142(12) 0.084(8) 0.128(11) 0.055(8) 0.106(11) 0.071(9) C56 0.57(6) 0.27(3) 0.26(3) 0.23(3) -0.32(4) -0.33(4) C57 0.53(6) 0.084(12) 0.084(12) 0.017(10) -0.01(2) 0.09(2) C58 0.24(3) 0.40(4) 0.104(13) 0.12(2) 0.084(16) 0.24(3) C59 0.76(10) 1.05(14) 1.02(13) 0.99(13) 0.80(11) 0.84(11) C60 0.130(15) 0.104(13) 0.34(3) -0.006(17) 0.15(2) 0.010(11) N1 0.043(3) 0.018(3) 0.024(3) 0.005(2) 0.012(2) 0.006(2) N2 0.039(3) 0.016(2) 0.023(3) 0.000(2) 0.013(2) 0.004(2) N3 0.031(3) 0.009(2) 0.025(3) 0.0017(19) 0.012(2) 0.0030(19) N4 0.028(3) 0.014(2) 0.021(2) 0.0055(19) 0.005(2) 0.0032(19) O1 0.042(3) 0.021(2) 0.079(4) 0.024(2) 0.028(3) 0.012(2) O2 0.058(4) 0.075(5) 0.075(5) 0.033(4) 0.006(3) 0.021(3) O3 0.063(4) 0.049(4) 0.089(5) 0.040(4) -0.010(4) 0.009(3) O4 0.064(4) 0.073(5) 0.099(6) -0.006(4) 0.021(4) 0.001(4) O5 0.051(4) 0.143(8) 0.051(4) -0.038(5) -0.006(3) -0.001(4) O6 0.067(5) 0.048(5) 0.284(16) -0.020(7) -0.058(7) 0.021(4) O7 0.111(7) 0.118(8) 0.093(7) -0.006(6) 0.017(6) 0.030(6) O8 0.160(10) 0.170(11) 0.119(8) 0.092(8) 0.083(8) 0.119(9) O9 0.149(12) 0.55(4) 0.71(5) 0.58(4) 0.27(2) 0.238(19) Tb1 0.0355(2) 0.01445(17) 0.02494(18) 0.00270(11) 0.00543(13) 0.00132(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.372(8) . ? C1 C2 1.422(9) . ? C1 C19 1.432(9) . ? C2 C3 1.369(10) . ? C2 H2 0.9500 . ? C3 C4 1.443(9) . ? C3 H3 0.9500 . ? C4 N1 1.372(8) . ? C4 C5 1.412(9) . ? C5 C6 1.411(9) . ? C5 C20 1.498(9) . ? C6 N2 1.399(8) . ? C6 C7 1.430(9) . ? C7 C8 1.352(10) . ? C7 H7 0.9500 . ? C8 C9 1.455(9) . ? C8 H8 0.9500 . ? C9 N2 1.382(8) . ? C9 C10 1.400(9) . ? C10 C11 1.402(9) . ? C10 C29 1.508(8) . ? C11 N3 1.385(7) . ? C11 C12 1.448(9) . ? C12 C13 1.355(8) . ? C12 H12 0.9500 . ? C13 C14 1.440(8) . ? C13 H13 0.9500 . ? C14 N3 1.397(8) . ? C14 C15 1.408(8) . ? C15 C16 1.421(8) . ? C15 C36 1.499(8) . ? C16 N4 1.355(8) . ? C16 C17 1.438(8) . ? C17 C18 1.383(9) . ? C17 H17 0.9500 . ? C18 C19 1.426(8) . ? C18 H18 0.9500 . ? C19 N4 1.362(8) . ? C20 C25 1.399(10) . ? C20 C21 1.408(10) . ? C21 C22 1.389(10) . ? C21 C26 1.494(11) . ? C22 C23 1.378(12) . ? C22 H22 0.9500 . ? C23 C24 1.386(12) . ? C23 C27 1.517(11) . ? C24 C25 1.393(11) . ? C24 H24 0.9500 . ? C25 C28 1.514(11) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.371(9) . ? C29 C34 1.389(9) . ? C30 C31 1.395(9) . ? C30 H30 0.9500 . ? C31 C32 1.382(9) . ? C31 H31 0.9500 . ? C32 O1 1.378(7) . ? C32 C33 1.379(10) . ? C33 C34 1.382(9) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? C35 O1 1.413(9) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 C41 1.408(9) . ? C36 C37 1.409(9) . ? C37 C38 1.403(10) . ? C37 C42 1.507(10) . ? C38 C39 1.379(11) . ? C38 H38 0.9500 . ? C39 C40 1.390(11) . ? C39 C43 1.510(10) . ? C40 C41 1.390(9) . ? C40 H40 0.9500 . ? C41 C44 1.502(9) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C46 1.63(3) . ? C45 O4 1.66(2) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 O5 1.24(2) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 O5 1.65(2) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 O3 1.318(16) . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 C50 1.481(5) . ? C49 O3 1.55(19) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 O2 1.48(6) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 O2 1.356(15) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 O4 1.45(2) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 O6 1.428(19) . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 C55 1.481(5) . ? C54 O6 1.517(16) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 O7 1.467(14) . ? C55 C56 2.04(4) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 O7 1.353(19) . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 O8 1.29(2) . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 C59 1.482(5) . ? C58 O8 1.58(2) . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 O9 1.40(3) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 O9 1.24(2) . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? N1 Tb1 2.327(5) . ? N2 Tb1 2.317(5) . ? N3 Tb1 2.309(5) . ? N4 Tb1 2.322(5) . ? O2 Tb1 2.718(7) . ? O3 Tb1 2.540(6) . ? O4 Tb1 2.620(7) . ? O5 Tb1 2.540(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 109.1(5) . . ? N1 C1 C19 113.8(5) . . ? C2 C1 C19 135.6(6) . . ? C3 C2 C1 107.2(6) . . ? C3 C2 H2 126.4 . . ? C1 C2 H2 126.4 . . ? C2 C3 C4 107.3(6) . . ? C2 C3 H3 126.3 . . ? C4 C3 H3 126.3 . . ? N1 C4 C5 121.4(6) . . ? N1 C4 C3 108.0(6) . . ? C5 C4 C3 129.5(6) . . ? C6 C5 C4 123.3(6) . . ? C6 C5 C20 118.2(6) . . ? C4 C5 C20 117.9(6) . . ? N2 C6 C5 125.2(6) . . ? N2 C6 C7 108.1(6) . . ? C5 C6 C7 126.3(6) . . ? C8 C7 C6 108.4(6) . . ? C8 C7 H7 125.8 . . ? C6 C7 H7 125.8 . . ? C7 C8 C9 107.7(5) . . ? C7 C8 H8 126.1 . . ? C9 C8 H8 126.1 . . ? N2 C9 C10 125.6(5) . . ? N2 C9 C8 107.8(5) . . ? C10 C9 C8 126.5(6) . . ? C9 C10 C11 126.0(5) . . ? C9 C10 C29 117.1(5) . . ? C11 C10 C29 116.2(5) . . ? N3 C11 C10 125.1(6) . . ? N3 C11 C12 107.5(5) . . ? C10 C11 C12 127.0(5) . . ? C13 C12 C11 108.3(5) . . ? C13 C12 H12 125.9 . . ? C11 C12 H12 125.9 . . ? C12 C13 C14 108.1(5) . . ? C12 C13 H13 126.0 . . ? C14 C13 H13 126.0 . . ? N3 C14 C15 125.0(5) . . ? N3 C14 C13 107.6(5) . . ? C15 C14 C13 127.0(6) . . ? C14 C15 C16 123.1(5) . . ? C14 C15 C36 117.9(5) . . ? C16 C15 C36 118.7(5) . . ? N4 C16 C15 122.1(5) . . ? N4 C16 C17 108.9(5) . . ? C15 C16 C17 127.9(5) . . ? C18 C17 C16 106.8(5) . . ? C18 C17 H17 126.6 . . ? C16 C17 H17 126.6 . . ? C17 C18 C19 106.3(5) . . ? C17 C18 H18 126.9 . . ? C19 C18 H18 126.9 . . ? N4 C19 C18 109.7(5) . . ? N4 C19 C1 115.1(5) . . ? C18 C19 C1 133.5(6) . . ? C25 C20 C21 119.5(6) . . ? C25 C20 C5 120.3(6) . . ? C21 C20 C5 120.2(6) . . ? C22 C21 C20 119.0(7) . . ? C22 C21 C26 120.2(7) . . ? C20 C21 C26 120.8(6) . . ? C23 C22 C21 122.4(7) . . ? C23 C22 H22 118.8 . . ? C21 C22 H22 118.8 . . ? C22 C23 C24 117.8(7) . . ? C22 C23 C27 122.0(8) . . ? C24 C23 C27 120.1(8) . . ? C23 C24 C25 122.1(7) . . ? C23 C24 H24 119.0 . . ? C25 C24 H24 119.0 . . ? C24 C25 C20 119.2(7) . . ? C24 C25 C28 119.1(7) . . ? C20 C25 C28 121.7(7) . . ? C21 C26 H26A 109.5 . . ? C21 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C21 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C27 H27A 109.5 . . ? C23 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C23 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 C34 117.9(6) . . ? C30 C29 C10 120.2(6) . . ? C34 C29 C10 121.9(6) . . ? C29 C30 C31 121.9(6) . . ? C29 C30 H30 119.1 . . ? C31 C30 H30 119.1 . . ? C32 C31 C30 118.8(6) . . ? C32 C31 H31 120.6 . . ? C30 C31 H31 120.6 . . ? O1 C32 C33 116.0(6) . . ? O1 C32 C31 123.6(6) . . ? C33 C32 C31 120.4(6) . . ? C32 C33 C34 119.4(6) . . ? C32 C33 H33 120.3 . . ? C34 C33 H33 120.3 . . ? C33 C34 C29 121.5(6) . . ? C33 C34 H34 119.3 . . ? C29 C34 H34 119.3 . . ? O1 C35 H35A 109.5 . . ? O1 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? O1 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C41 C36 C37 119.3(6) . . ? C41 C36 C15 120.2(5) . . ? C37 C36 C15 120.5(6) . . ? C38 C37 C36 118.8(6) . . ? C38 C37 C42 119.9(6) . . ? C36 C37 C42 121.3(6) . . ? C39 C38 C37 122.5(6) . . ? C39 C38 H38 118.7 . . ? C37 C38 H38 118.7 . . ? C38 C39 C40 117.5(6) . . ? C38 C39 C43 121.6(7) . . ? C40 C39 C43 120.9(8) . . ? C39 C40 C41 122.6(7) . . ? C39 C40 H40 118.7 . . ? C41 C40 H40 118.7 . . ? C40 C41 C36 119.1(6) . . ? C40 C41 C44 119.3(6) . . ? C36 C41 C44 121.5(5) . . ? C37 C42 H42A 109.5 . . ? C37 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C37 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C39 C43 H43A 109.5 . . ? C39 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C39 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C46 C45 O4 107.4(17) . . ? C46 C45 H45A 110.2 . . ? O4 C45 H45A 110.2 . . ? C46 C45 H45B 110.2 . . ? O4 C45 H45B 110.2 . . ? H45A C45 H45B 108.5 . . ? O5 C46 C45 97(2) . . ? O5 C46 H46A 112.3 . . ? C45 C46 H46A 112.3 . . ? O5 C46 H46B 112.3 . . ? C45 C46 H46B 112.3 . . ? H46A C46 H46B 109.9 . . ? O5 C47 H47A 109.5 . . ? O5 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? O5 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? O3 C48 H48A 109.5 . . ? O3 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? O3 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C50 C49 O3 108(10) . . ? C50 C49 H49A 110.1 . . ? O3 C49 H49A 110.1 . . ? C50 C49 H49B 110.1 . . ? O3 C49 H49B 110.1 . . ? H49A C49 H49B 108.4 . . ? C49 C50 O2 120(10) . . ? C49 C50 H50A 107.2 . . ? O2 C50 H50A 107.2 . . ? C49 C50 H50B 107.2 . . ? O2 C50 H50B 107.2 . . ? H50A C50 H50B 106.9 . . ? O2 C51 H51A 109.5 . . ? O2 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? O2 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? O4 C52 H52A 109.5 . . ? O4 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? O4 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? O6 C53 H53A 109.5 . . ? O6 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? O6 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C55 C54 O6 103.2(9) . . ? C55 C54 H54A 111.1 . . ? O6 C54 H54A 111.1 . . ? C55 C54 H54B 111.1 . . ? O6 C54 H54B 111.1 . . ? H54A C54 H54B 109.1 . . ? O7 C55 C54 105.5(10) . . ? O7 C55 C56 41.6(12) . . ? C54 C55 C56 147.1(14) . . ? O7 C55 H55A 110.6 . . ? C54 C55 H55A 110.6 . . ? C56 C55 H55A 86.0 . . ? O7 C55 H55B 110.6 . . ? C54 C55 H55B 110.6 . . ? C56 C55 H55B 88.9 . . ? H55A C55 H55B 108.8 . . ? O7 C56 C55 46.1(14) . . ? O7 C56 H56A 109.5 . . ? C55 C56 H56A 155.6 . . ? O7 C56 H56B 109.5 . . ? C55 C56 H56B 83.8 . . ? H56A C56 H56B 109.5 . . ? O7 C56 H56C 109.5 . . ? C55 C56 H56C 83.7 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? O8 C57 H57A 109.5 . . ? O8 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? O8 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C59 C58 O8 97.2(17) . . ? C59 C58 H58A 112.3 . . ? O8 C58 H58A 112.3 . . ? C59 C58 H58B 112.3 . . ? O8 C58 H58B 112.3 . . ? H58A C58 H58B 109.9 . . ? O9 C59 C58 93(2) . . ? O9 C59 H59A 113.0 . . ? C58 C59 H59A 113.0 . . ? O9 C59 H59B 113.0 . . ? C58 C59 H59B 113.0 . . ? H59A C59 H59B 110.4 . . ? O9 C60 H60A 109.5 . . ? O9 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? O9 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C4 N1 C1 108.1(5) . . ? C4 N1 Tb1 133.6(4) . . ? C1 N1 Tb1 118.1(4) . . ? C9 N2 C6 107.9(5) . . ? C9 N2 Tb1 120.1(4) . . ? C6 N2 Tb1 127.7(4) . . ? C11 N3 C14 108.4(5) . . ? C11 N3 Tb1 119.5(4) . . ? C14 N3 Tb1 127.3(4) . . ? C16 N4 C19 108.1(5) . . ? C16 N4 Tb1 133.7(4) . . ? C19 N4 Tb1 118.1(4) . . ? C32 O1 C35 117.8(6) . . ? C51 O2 C50 121(3) . . ? C51 O2 Tb1 131.1(7) . . ? C50 O2 Tb1 107(3) . . ? C48 O3 C49 115(8) . . ? C48 O3 Tb1 132.6(8) . . ? C49 O3 Tb1 106(7) . . ? C52 O4 C45 136.8(13) . . ? C52 O4 Tb1 118.0(10) . . ? C45 O4 Tb1 104.9(9) . . ? C46 O5 C47 107.0(16) . . ? C46 O5 Tb1 137.7(14) . . ? C47 O5 Tb1 106.8(9) . . ? C53 O6 C54 122.3(11) . . ? C56 O7 C55 92(2) . . ? C57 O8 C58 99(2) . . ? C60 O9 C59 115(2) . . ? N3 Tb1 N2 77.84(17) . . ? N3 Tb1 N4 72.71(17) . . ? N2 Tb1 N4 112.51(18) . . ? N3 Tb1 N1 113.55(19) . . ? N2 Tb1 N1 72.16(18) . . ? N4 Tb1 N1 66.95(18) . . ? N3 Tb1 O3 133.1(2) . . ? N2 Tb1 O3 148.9(2) . . ? N4 Tb1 O3 79.8(2) . . ? N1 Tb1 O3 88.4(2) . . ? N3 Tb1 O5 153.7(3) . . ? N2 Tb1 O5 84.7(2) . . ? N4 Tb1 O5 132.9(3) . . ? N1 Tb1 O5 78.7(2) . . ? O3 Tb1 O5 67.5(3) . . ? N3 Tb1 O4 96.2(2) . . ? N2 Tb1 O4 81.0(2) . . ? N4 Tb1 O4 159.2(2) . . ? N1 Tb1 O4 133.7(2) . . ? O3 Tb1 O4 96.6(2) . . ? O5 Tb1 O4 61.4(3) . . ? N3 Tb1 O2 79.28(18) . . ? N2 Tb1 O2 135.1(2) . . ? N4 Tb1 O2 96.5(2) . . ? N1 Tb1 O2 152.7(2) . . ? O3 Tb1 O2 66.7(2) . . ? O5 Tb1 O2 100.3(2) . . ? O4 Tb1 O2 63.7(2) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 3.073 _refine_diff_density_min -2.057 _refine_diff_density_rms 0.162