# Electronic Supplementary Material (ESI) for CrystEngComm # 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_TbLi _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H50 Li N10 O7 Tb' _chemical_formula_weight 1188.96 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' 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 22.7180(13) _cell_length_b 11.7263(4) _cell_length_c 22.8679(12) _cell_angle_alpha 90.00 _cell_angle_beta 118.173(7) _cell_angle_gamma 90.00 _cell_volume 5370.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8850 _cell_measurement_theta_min 3.0454 _cell_measurement_theta_max 28.5066 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.471 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2416 _exptl_absorpt_coefficient_mu 1.381 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8742 _exptl_absorpt_correction_T_max 0.9217 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _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, Eos, Gemini' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.2141 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 30727 _diffrn_reflns_av_R_equivalents 0.0511 _diffrn_reflns_av_sigmaI/netI 0.0597 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9434 _reflns_number_gt 6997 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker FRAMBO' _computing_cell_refinement 'Bruker FRAMBO' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0842P)^2^+2.2895P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9434 _refine_ls_number_parameters 775 _refine_ls_number_restraints 3295 _refine_ls_R_factor_all 0.0745 _refine_ls_R_factor_gt 0.0487 _refine_ls_wR_factor_ref 0.1393 _refine_ls_wR_factor_gt 0.1280 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.201 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3096(3) 0.0609(5) -0.0843(3) 0.0249(13) Uani 1 1 d U . . C2 C 0.3122(3) -0.0321(5) -0.1254(3) 0.0254(13) Uani 1 1 d U . . C3 C 0.3662(4) -0.0881(6) -0.1266(4) 0.0359(16) Uani 1 1 d U . . H3 H 0.4101 -0.0697 -0.0966 0.043 Uiso 1 1 calc R . . C4 C 0.3517(4) -0.1723(7) -0.1745(4) 0.046(2) Uani 1 1 d U . . H4 H 0.3864 -0.2115 -0.1763 0.055 Uiso 1 1 calc R . . C5 C 0.2857(4) -0.1986(6) -0.2198(4) 0.0435(19) Uani 1 1 d U . . H5 H 0.2775 -0.2546 -0.2516 0.052 Uiso 1 1 calc R . . C6 C 0.2319(4) -0.1437(5) -0.2189(4) 0.0316(15) Uani 1 1 d U . . H6 H 0.1881 -0.1610 -0.2496 0.038 Uiso 1 1 calc R . . C7 C 0.2467(3) -0.0612(5) -0.1697(3) 0.0240(13) Uani 1 1 d U . . C8 C 0.2040(3) 0.0157(5) -0.1550(3) 0.0224(13) Uani 1 1 d U . . C9 C 0.0666(3) 0.2428(5) -0.1432(3) 0.0209(13) Uani 1 1 d U . . C10 C 0.0084(3) 0.2061(5) -0.2040(3) 0.0208(13) Uani 1 1 d U . . C11 C -0.0573(3) 0.2440(5) -0.2366(3) 0.0251(14) Uani 1 1 d U . . H11 H -0.0713 0.3055 -0.2206 0.030 Uiso 1 1 calc R . . C12 C -0.1007(4) 0.1878(6) -0.2929(3) 0.0276(15) Uani 1 1 d U . . H12 H -0.1451 0.2109 -0.3145 0.033 Uiso 1 1 calc R . . C13 C -0.0812(4) 0.0973(6) -0.3193(3) 0.0308(16) Uani 1 1 d U . . H13 H -0.1124 0.0614 -0.3578 0.037 Uiso 1 1 calc R . . C14 C -0.0135(3) 0.0595(5) -0.2875(3) 0.0270(14) Uani 1 1 d U . . H14 H 0.0009 0.0006 -0.3049 0.032 Uiso 1 1 calc R . . C15 C 0.0296(3) 0.1147(5) -0.2297(3) 0.0222(13) Uani 1 1 d U . . C16 C 0.1003(3) 0.0988(5) -0.1833(3) 0.0221(13) Uani 1 1 d U . . C17 C 0.1175(3) 0.3751(5) -0.0565(3) 0.0220(13) Uani 1 1 d U . . C18 C 0.1145(3) 0.4776(5) -0.0214(3) 0.0248(14) Uani 1 1 d U . . C19 C 0.0609(4) 0.5410(5) -0.0254(4) 0.0304(15) Uani 1 1 d U . . H19 H 0.0172 0.5224 -0.0557 0.036 Uiso 1 1 calc R . . C20 C 0.0752(4) 0.6333(6) 0.0174(4) 0.0407(18) Uani 1 1 d U . . H20 H 0.0404 0.6759 0.0169 0.049 Uiso 1 1 calc R . . C21 C 0.1415(4) 0.6630(7) 0.0614(4) 0.048(2) Uani 1 1 d U . . H21 H 0.1500 0.7261 0.0888 0.058 Uiso 1 1 calc R . . C22 C 0.1938(4) 0.6009(6) 0.0646(4) 0.0396(17) Uani 1 1 d U . . H22 H 0.2376 0.6213 0.0937 0.048 Uiso 1 1 calc R . . C23 C 0.1800(4) 0.5060(5) 0.0232(3) 0.0279(14) Uani 1 1 d U . . C24 C 0.2224(3) 0.4215(5) 0.0135(3) 0.0253(13) Uani 1 1 d U . . C25 C 0.3266(4) 0.3532(5) 0.0304(4) 0.0308(15) Uani 1 1 d U . . C26 C 0.3967(4) 0.3759(6) 0.0496(4) 0.0375(17) Uani 1 1 d U . . C27 C 0.4396(4) 0.4649(6) 0.0841(5) 0.049(2) Uani 1 1 d U . . H27 H 0.4253 0.5252 0.1006 0.059 Uiso 1 1 calc R . . C28 C 0.5046(4) 0.4609(7) 0.0930(5) 0.063(2) Uani 1 1 d U . . H28 H 0.5345 0.5185 0.1167 0.075 Uiso 1 1 calc R . . C29 C 0.5255(4) 0.3716(7) 0.0668(5) 0.059(2) Uani 1 1 d U . . H29 H 0.5689 0.3716 0.0728 0.070 Uiso 1 1 calc R . . C30 C 0.4825(4) 0.2824(7) 0.0320(4) 0.0460(19) Uani 1 1 d U . . H30 H 0.4962 0.2234 0.0140 0.055 Uiso 1 1 calc R . . C31 C 0.4187(4) 0.2853(6) 0.0253(4) 0.0353(16) Uani 1 1 d U . . C32 C 0.3610(3) 0.2095(5) -0.0089(3) 0.0278(14) Uani 1 1 d U . . C33 C 0.4803(5) -0.0599(10) 0.0969(6) 0.081(3) Uani 1 1 d U . . H33A H 0.5077 -0.0005 0.1260 0.122 Uiso 1 1 calc R . . H33B H 0.4801 -0.0537 0.0550 0.122 Uiso 1 1 calc R . . H33C H 0.4980 -0.1328 0.1164 0.122 Uiso 1 1 calc R . . C34 C 0.3841(4) -0.2320(6) 0.0293(4) 0.0418(18) Uani 1 1 d U . . H34 H 0.4287 -0.2510 0.0441 0.050 Uiso 1 1 calc R . . C35 C 0.3678(4) -0.1287(6) 0.0464(4) 0.0338(16) Uani 1 1 d U . . C36 C 0.3011(3) -0.0941(6) 0.0242(3) 0.0260(14) Uani 1 1 d U . . C37 C 0.2504(3) -0.1717(5) -0.0160(3) 0.0252(14) Uani 1 1 d U . . C38 C 0.2689(4) -0.2786(6) -0.0316(4) 0.0341(16) Uani 1 1 d U . . H38 H 0.2357 -0.3304 -0.0574 0.041 Uiso 1 1 calc R . . C39 C 0.3346(4) -0.3071(6) -0.0096(4) 0.0415(18) Uani 1 1 d U . . H39 H 0.3456 -0.3771 -0.0210 0.050 Uiso 1 1 calc R . . C40 C 0.1801(4) -0.1506(5) -0.0419(3) 0.0265(14) Uani 1 1 d U . . H40 H 0.1517 -0.2133 -0.0565 0.032 Uiso 1 1 calc R . . C41 C 0.0821(3) -0.0440(5) -0.0736(3) 0.0231(13) Uani 1 1 d U . . C42 C 0.0367(4) -0.1144(5) -0.1231(4) 0.0288(15) Uani 1 1 d U . . H42 H 0.0518 -0.1756 -0.1382 0.035 Uiso 1 1 calc R . . C43 C -0.0310(4) -0.0937(6) -0.1502(4) 0.0346(16) Uani 1 1 d U . . H43 H -0.0612 -0.1413 -0.1832 0.042 Uiso 1 1 calc R . . C44 C -0.0541(4) -0.0027(6) -0.1285(4) 0.0360(17) Uani 1 1 d U . . H44 H -0.0998 0.0106 -0.1469 0.043 Uiso 1 1 calc R . . C45 C -0.0092(4) 0.0692(6) -0.0790(4) 0.0327(15) Uani 1 1 d U . . H45 H -0.0251 0.1306 -0.0648 0.039 Uiso 1 1 calc R . . C46 C 0.0592(3) 0.0497(5) -0.0506(3) 0.0249(13) Uani 1 1 d U . . C47 C 0.0974(4) 0.1781(5) 0.0393(3) 0.0274(14) Uani 1 1 d U . . H47 H 0.0551 0.1708 0.0356 0.033 Uiso 1 1 calc R . . C48 C 0.1440(4) 0.2506(5) 0.0910(3) 0.0281(14) Uani 1 1 d U . . C49 C 0.1174(4) 0.3237(6) 0.1215(4) 0.0342(16) Uani 1 1 d U . . H49 H 0.0717 0.3231 0.1072 0.041 Uiso 1 1 calc R . . C50 C 0.1573(4) 0.3955(7) 0.1717(4) 0.0452(19) Uani 1 1 d U . . H50 H 0.1387 0.4460 0.1898 0.054 Uiso 1 1 calc R . . C51 C 0.2253(5) 0.3921(8) 0.1952(5) 0.061(2) Uani 1 1 d U . . H51 H 0.2530 0.4394 0.2300 0.073 Uiso 1 1 calc R . . C52 C 0.2527(5) 0.3191(8) 0.1673(4) 0.052(2) Uani 1 1 d U A . C53 C 0.2130(4) 0.2476(6) 0.1135(3) 0.0309(14) Uani 1 1 d U . . C55 C 0.2323(6) -0.0658(13) 0.1478(7) 0.117(5) Uani 1 1 d DU . . H55A H 0.2046 -0.0075 0.1181 0.175 Uiso 1 1 calc R . . H55B H 0.2140 -0.0892 0.1761 0.175 Uiso 1 1 calc R . . H55C H 0.2341 -0.1300 0.1227 0.175 Uiso 1 1 calc R . . O1 O 0.4148(3) -0.0490(4) 0.0875(3) 0.0491(14) Uani 1 1 d U . . O2 O 0.2884(2) 0.0058(4) 0.0424(2) 0.0285(10) Uani 1 1 d U A . O3 O 0.2427(2) 0.1822(4) 0.0888(2) 0.0322(11) Uani 1 1 d U A . O4 O 0.3213(4) 0.3107(7) 0.1896(3) 0.083(2) Uani 1 1 d DU . . O5 O 0.3007(4) -0.0203(6) 0.1889(4) 0.089(2) Uani 1 1 d DU A . H5A H 0.3373 -0.0568 0.1985 0.134 Uiso 1 1 d RD . . O6 O 0.4031(7) 0.1464(10) 0.1447(7) 0.087(3) Uani 0.591(7) 1 d PDU A 1 H6A H 0.3794 0.1368 0.0942 0.131 Uiso 1 1 d RD A 1 C56 C 0.4633(10) 0.195(2) 0.1928(11) 0.120(6) Uani 0.591(7) 1 d PDU A 1 H56A H 0.4793 0.1592 0.2352 0.179 Uiso 0.591(7) 1 d PR A 1 H56B H 0.4589 0.2760 0.1974 0.179 Uiso 0.591(7) 1 d PR A 1 H56C H 0.4943 0.1826 0.1761 0.179 Uiso 0.591(7) 1 d PR A 1 O6A O 0.4092(10) 0.1251(16) 0.1925(10) 0.087(3) Uani 0.409(7) 1 d PDU A 2 H6B H 0.3956 0.0642 0.2036 0.131 Uiso 0.409(7) 1 d PRD A 2 C56A C 0.4756(12) 0.164(3) 0.222(2) 0.120(6) Uani 0.409(7) 1 d PDU A 2 H56D H 0.5059 0.1268 0.2100 0.179 Uiso 0.409(7) 1 d PR A 2 H56E H 0.4910 0.1546 0.2688 0.179 Uiso 0.409(7) 1 d PR A 2 H56F H 0.4734 0.2438 0.2118 0.179 Uiso 0.409(7) 1 d PR A 2 Tb01 Tb 0.210674(15) 0.13982(2) -0.019905(15) 0.01971(12) Uani 1 1 d U A . N1 N 0.3071(3) 0.2527(4) -0.0040(3) 0.0257(12) Uani 1 1 d U . . N2 N 0.3639(3) 0.1175(5) -0.0420(3) 0.0300(12) Uani 1 1 d U . . N3 N 0.2441(3) 0.0821(4) -0.1016(3) 0.0218(11) Uani 1 1 d U . . N4 N 0.1375(3) 0.0210(4) -0.1925(3) 0.0217(11) Uani 1 1 d U . . N5 N 0.1204(3) 0.1753(4) -0.1311(3) 0.0197(11) Uani 1 1 d U . . N6 N 0.0636(3) 0.3306(4) -0.1076(3) 0.0224(11) Uani 1 1 d U . . N7 N 0.1825(3) 0.3421(4) -0.0325(3) 0.0226(11) Uani 1 1 d U . . N8 N 0.2886(3) 0.4275(5) 0.0428(3) 0.0310(13) Uani 1 1 d U . . N9 N 0.1530(3) -0.0513(4) -0.0465(3) 0.0218(11) Uani 1 1 d U . . N10 N 0.1095(3) 0.1214(4) -0.0033(3) 0.0225(11) Uani 1 1 d U . . O7 O 0.3184(7) 0.0419(12) 0.3094(7) 0.088(3) Uani 0.591(7) 1 d PDU A 1 C59 C 0.2303(10) 0.0695(15) 0.3339(11) 0.085(4) Uani 0.591(7) 1 d PDU A 1 H59A H 0.2340 0.0916 0.3764 0.102 Uiso 0.591(7) 1 calc PR A 1 H59B H 0.1877 0.0321 0.3080 0.102 Uiso 0.591(7) 1 calc PR A 1 C58 C 0.2368(8) 0.1720(13) 0.2976(9) 0.073(4) Uani 0.591(7) 1 d PDU A 1 H58A H 0.2045 0.1694 0.2509 0.088 Uiso 0.591(7) 1 calc PR A 1 H58B H 0.2309 0.2423 0.3166 0.088 Uiso 0.591(7) 1 calc PR A 1 C60 C 0.2865(10) -0.0079(15) 0.3434(12) 0.106(5) Uani 0.591(7) 1 d PDU A 1 H60A H 0.3178 -0.0156 0.3902 0.128 Uiso 0.591(7) 1 calc PR A 1 H60B H 0.2696 -0.0829 0.3255 0.128 Uiso 0.591(7) 1 calc PR A 1 C57 C 0.3066(8) 0.1615(12) 0.3077(11) 0.093(4) Uani 0.591(7) 1 d PDU A 1 H57A H 0.3107 0.1970 0.2714 0.111 Uiso 0.591(7) 1 calc PR A 1 H57B H 0.3381 0.1971 0.3490 0.111 Uiso 0.591(7) 1 calc PR A 1 O7A O 0.2056(10) 0.070(2) 0.2598(8) 0.122(5) Uani 0.409(7) 1 d PDU A 2 C58A C 0.3121(9) 0.049(3) 0.3557(10) 0.086(5) Uani 0.409(7) 1 d PDU A 2 H58C H 0.3383 0.1185 0.3719 0.103 Uiso 0.409(7) 1 calc PR A 2 H58D H 0.3410 -0.0164 0.3734 0.103 Uiso 0.409(7) 1 calc PR A 2 C59A C 0.2552(12) 0.046(3) 0.3724(10) 0.089(5) Uani 0.409(7) 1 d PDU A 2 H59C H 0.2676 0.0826 0.4148 0.107 Uiso 0.409(7) 1 calc PR A 2 H59D H 0.2411 -0.0313 0.3736 0.107 Uiso 0.409(7) 1 calc PR A 2 C60A C 0.2011(12) 0.113(3) 0.3159(11) 0.094(5) Uani 0.409(7) 1 d PDU A 2 H60C H 0.1575 0.0984 0.3123 0.113 Uiso 0.409(7) 1 calc PR A 2 H60D H 0.2100 0.1944 0.3212 0.113 Uiso 0.409(7) 1 calc PR A 2 C57A C 0.2747(11) 0.047(3) 0.2813(10) 0.082(4) Uani 0.409(7) 1 d PDU A 2 H57C H 0.2928 0.1037 0.2634 0.098 Uiso 0.409(7) 1 calc PR A 2 H57D H 0.2795 -0.0275 0.2654 0.098 Uiso 0.409(7) 1 calc PR A 2 Li1 Li 0.3250(9) 0.0863(15) 0.1325(8) 0.063(3) Uani 1 1 d U . . C54 C 0.3573(9) 0.4180(13) 0.2179(11) 0.090(5) Uani 0.591(7) 1 d PDU A 1 H54A H 0.4041 0.4073 0.2322 0.135 Uiso 0.591(7) 1 calc PR A 1 H54B H 0.3512 0.4396 0.2552 0.135 Uiso 0.591(7) 1 calc PR A 1 H54C H 0.3402 0.4769 0.1849 0.135 Uiso 0.591(7) 1 calc PR A 1 C54A C 0.3627(12) 0.332(3) 0.2593(7) 0.083(7) Uani 0.409(7) 1 d PDU A 2 H54D H 0.4088 0.3239 0.2702 0.125 Uiso 0.409(7) 1 calc PR A 2 H54E H 0.3522 0.2773 0.2844 0.125 Uiso 0.409(7) 1 calc PR A 2 H54F H 0.3548 0.4074 0.2698 0.125 Uiso 0.409(7) 1 calc PR A 2 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 0.024(3) 0.024(3) 0.028(3) 0.006(2) 0.013(3) 0.004(2) C2 0.030(3) 0.026(3) 0.026(3) 0.001(2) 0.018(3) 0.003(3) C3 0.025(4) 0.038(4) 0.046(4) -0.003(3) 0.019(3) 0.004(3) C4 0.035(4) 0.050(4) 0.061(5) -0.013(4) 0.029(4) 0.012(3) C5 0.042(4) 0.038(4) 0.056(5) -0.016(3) 0.027(4) 0.005(3) C6 0.032(4) 0.028(3) 0.040(4) -0.001(3) 0.022(3) 0.004(3) C7 0.026(3) 0.017(3) 0.030(3) 0.005(2) 0.014(3) 0.001(2) C8 0.024(3) 0.026(3) 0.019(3) 0.006(2) 0.012(3) 0.002(2) C9 0.020(3) 0.020(3) 0.024(3) 0.005(2) 0.011(2) 0.000(2) C10 0.020(3) 0.023(3) 0.020(3) 0.000(2) 0.010(2) -0.001(2) C11 0.023(3) 0.026(3) 0.027(3) 0.001(3) 0.012(3) 0.001(3) C12 0.021(3) 0.031(3) 0.026(4) -0.001(3) 0.007(3) -0.004(3) C13 0.025(4) 0.032(3) 0.024(4) -0.004(3) 0.002(3) -0.005(3) C14 0.026(3) 0.032(3) 0.022(3) -0.001(3) 0.011(3) 0.000(3) C15 0.023(3) 0.022(3) 0.022(3) 0.003(2) 0.011(3) -0.004(2) C16 0.024(3) 0.019(3) 0.026(3) 0.003(2) 0.014(3) 0.001(2) C17 0.022(3) 0.020(3) 0.024(3) 0.003(2) 0.011(3) 0.002(2) C18 0.027(3) 0.022(3) 0.026(3) 0.002(2) 0.012(3) 0.002(3) C19 0.022(3) 0.028(3) 0.035(4) -0.006(3) 0.009(3) 0.007(3) C20 0.032(4) 0.036(4) 0.047(4) -0.012(3) 0.014(4) 0.012(3) C21 0.043(5) 0.042(4) 0.046(5) -0.021(3) 0.011(4) 0.010(3) C22 0.031(4) 0.034(3) 0.043(4) -0.013(3) 0.009(3) 0.001(3) C23 0.032(3) 0.024(3) 0.029(3) -0.001(2) 0.015(3) 0.001(3) C24 0.023(3) 0.023(3) 0.027(3) -0.002(2) 0.010(3) 0.001(3) C25 0.021(3) 0.027(3) 0.037(3) -0.002(3) 0.008(3) -0.003(3) C26 0.023(3) 0.033(3) 0.047(4) -0.006(3) 0.009(3) -0.002(3) C27 0.028(4) 0.033(4) 0.069(5) -0.011(3) 0.009(4) -0.001(3) C28 0.024(4) 0.046(5) 0.099(6) -0.016(4) 0.013(4) -0.008(4) C29 0.025(4) 0.054(5) 0.089(6) -0.011(4) 0.021(4) -0.005(4) C30 0.024(4) 0.045(4) 0.063(5) -0.009(3) 0.015(3) -0.003(3) C31 0.021(3) 0.031(3) 0.048(4) 0.000(3) 0.011(3) 0.001(3) C32 0.019(3) 0.027(3) 0.033(3) 0.001(3) 0.009(3) 0.002(2) C33 0.027(5) 0.095(8) 0.103(8) -0.012(6) 0.014(5) -0.012(5) C34 0.025(4) 0.038(4) 0.054(4) 0.005(3) 0.012(3) 0.010(3) C35 0.028(3) 0.032(3) 0.036(4) 0.003(3) 0.010(3) 0.004(3) C36 0.029(3) 0.026(3) 0.024(3) 0.007(2) 0.014(3) 0.007(3) C37 0.025(3) 0.021(3) 0.031(3) 0.006(2) 0.015(3) 0.008(2) C38 0.036(4) 0.024(3) 0.040(4) 0.002(3) 0.015(3) 0.004(3) C39 0.039(4) 0.031(4) 0.053(4) -0.001(3) 0.020(4) 0.014(3) C40 0.028(3) 0.024(3) 0.027(3) 0.002(2) 0.012(3) 0.001(3) C41 0.024(3) 0.022(3) 0.027(3) 0.005(2) 0.016(3) 0.001(2) C42 0.029(3) 0.025(3) 0.031(3) 0.003(3) 0.013(3) -0.001(3) C43 0.030(4) 0.031(3) 0.038(4) -0.002(3) 0.011(3) -0.008(3) C44 0.022(4) 0.037(4) 0.043(4) 0.004(3) 0.010(3) -0.005(3) C45 0.026(3) 0.034(3) 0.044(4) 0.002(3) 0.020(3) 0.002(3) C46 0.025(3) 0.025(3) 0.027(3) 0.008(2) 0.015(3) 0.002(2) C47 0.028(3) 0.029(3) 0.027(3) 0.006(3) 0.015(3) 0.009(3) C48 0.036(3) 0.029(3) 0.025(3) 0.001(2) 0.018(3) 0.007(3) C49 0.040(4) 0.038(4) 0.028(4) 0.002(3) 0.019(3) 0.006(3) C50 0.048(4) 0.053(4) 0.037(4) -0.011(3) 0.022(4) 0.010(4) C51 0.050(5) 0.077(5) 0.048(4) -0.029(4) 0.016(4) 0.004(4) C52 0.042(4) 0.070(4) 0.037(4) -0.020(3) 0.014(3) 0.011(4) C53 0.035(3) 0.032(3) 0.027(3) 0.002(3) 0.016(3) 0.008(3) C55 0.094(9) 0.130(10) 0.100(9) 0.051(8) 0.024(8) -0.008(8) O1 0.029(3) 0.045(3) 0.052(3) -0.001(2) 0.002(3) -0.002(2) O2 0.026(2) 0.029(2) 0.029(2) 0.0011(18) 0.011(2) 0.0052(18) O3 0.035(3) 0.034(2) 0.027(2) -0.0006(19) 0.015(2) 0.011(2) O4 0.053(4) 0.119(4) 0.051(4) -0.047(3) 0.004(3) 0.010(3) O5 0.100(5) 0.098(4) 0.066(4) 0.021(4) 0.036(4) 0.024(4) O6 0.064(4) 0.095(4) 0.066(4) 0.001(4) 0.000(4) -0.004(4) C56 0.082(9) 0.130(10) 0.092(11) -0.001(9) -0.004(9) 0.015(9) O6A 0.064(4) 0.095(4) 0.066(4) 0.001(4) 0.000(4) -0.004(4) C56A 0.082(9) 0.130(10) 0.092(11) -0.001(9) -0.004(9) 0.015(9) Tb01 0.01811(19) 0.01997(19) 0.01986(19) -0.00020(12) 0.00799(14) 0.00171(13) N1 0.021(3) 0.026(3) 0.031(3) -0.001(2) 0.012(2) 0.003(2) N2 0.024(3) 0.032(3) 0.035(3) 0.002(2) 0.014(2) 0.003(2) N3 0.017(3) 0.022(2) 0.026(3) 0.000(2) 0.010(2) 0.005(2) N4 0.022(3) 0.023(2) 0.021(3) 0.002(2) 0.010(2) 0.000(2) N5 0.022(3) 0.018(2) 0.019(3) 0.0008(19) 0.009(2) 0.001(2) N6 0.021(3) 0.022(2) 0.024(3) 0.002(2) 0.010(2) 0.005(2) N7 0.022(3) 0.018(2) 0.027(3) -0.002(2) 0.011(2) 0.000(2) N8 0.024(3) 0.027(3) 0.035(3) -0.008(2) 0.008(2) 0.000(2) N9 0.025(3) 0.021(2) 0.021(3) 0.001(2) 0.013(2) 0.002(2) N10 0.023(3) 0.024(3) 0.022(3) 0.001(2) 0.013(2) 0.001(2) O7 0.080(7) 0.129(7) 0.063(6) 0.018(6) 0.041(5) 0.038(6) C59 0.081(8) 0.119(8) 0.072(7) 0.008(7) 0.050(6) 0.019(7) C58 0.072(7) 0.087(7) 0.070(6) 0.004(6) 0.041(6) 0.026(6) C60 0.106(8) 0.117(8) 0.080(7) 0.028(7) 0.031(7) 0.027(7) C57 0.083(7) 0.119(7) 0.069(6) 0.007(6) 0.030(6) 0.017(6) O7A 0.102(8) 0.138(8) 0.094(7) 0.023(7) 0.020(7) 0.009(7) C58A 0.078(8) 0.118(8) 0.069(8) 0.017(7) 0.040(7) 0.021(7) C59A 0.084(8) 0.115(9) 0.072(8) 0.017(8) 0.040(7) 0.026(8) C60A 0.086(9) 0.117(9) 0.077(8) 0.018(8) 0.037(8) 0.030(8) C57A 0.081(8) 0.125(8) 0.063(7) 0.013(7) 0.053(7) 0.037(7) Li1 0.059(5) 0.073(5) 0.040(5) 0.007(5) 0.008(5) 0.020(5) C54 0.052(10) 0.124(12) 0.073(11) -0.033(10) 0.012(9) 0.004(10) C54A 0.047(11) 0.120(13) 0.059(12) -0.032(11) 0.006(10) 0.024(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N2 1.331(9) . ? C1 N3 1.369(8) . ? C1 C2 1.459(9) . ? C2 C7 1.390(9) . ? C2 C3 1.402(9) . ? C3 C4 1.393(11) . ? C3 H3 0.9300 . ? C4 C5 1.396(11) . ? C4 H4 0.9300 . ? C5 C6 1.390(10) . ? C5 H5 0.9300 . ? C6 C7 1.399(9) . ? C6 H6 0.9300 . ? C7 C8 1.475(9) . ? C8 N4 1.341(8) . ? C8 N3 1.371(8) . ? C9 N6 1.335(8) . ? C9 N5 1.370(8) . ? C9 C10 1.459(9) . ? C10 C11 1.389(9) . ? C10 C15 1.412(9) . ? C11 C12 1.365(9) . ? C11 H11 0.9300 . ? C12 C13 1.392(9) . ? C12 H12 0.9300 . ? C13 C14 1.427(9) . ? C13 H13 0.9300 . ? C14 C15 1.380(9) . ? C14 H14 0.9300 . ? C15 C16 1.460(9) . ? C16 N4 1.326(8) . ? C16 N5 1.388(8) . ? C17 N6 1.336(9) . ? C17 N7 1.366(9) . ? C17 C18 1.465(8) . ? C18 C23 1.389(10) . ? C18 C19 1.392(9) . ? C19 C20 1.392(9) . ? C19 H19 0.9300 . ? C20 C21 1.404(11) . ? C20 H20 0.9300 . ? C21 C22 1.364(11) . ? C21 H21 0.9300 . ? C22 C23 1.397(9) . ? C22 H22 0.9300 . ? C23 C24 1.471(9) . ? C24 N8 1.329(8) . ? C24 N7 1.377(8) . ? C25 N8 1.348(9) . ? C25 N1 1.369(8) . ? C25 C26 1.463(10) . ? C26 C27 1.391(10) . ? C26 C31 1.395(10) . ? C27 C28 1.392(11) . ? C27 H27 0.9300 . ? C28 C29 1.395(12) . ? C28 H28 0.9300 . ? C29 C30 1.396(11) . ? C29 H29 0.9300 . ? C30 C31 1.386(10) . ? C30 H30 0.9300 . ? C31 C32 1.466(10) . ? C32 N2 1.338(8) . ? C32 N1 1.377(8) . ? C33 O1 1.405(10) . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 C39 1.375(11) . ? C34 C35 1.376(10) . ? C34 H34 0.9300 . ? C35 O1 1.396(9) . ? C35 C36 1.412(10) . ? C36 O2 1.320(8) . ? C36 C37 1.413(10) . ? C37 C38 1.420(9) . ? C37 C40 1.439(10) . ? C38 C39 1.372(10) . ? C38 H38 0.9300 . ? C39 H39 0.9300 . ? C40 N9 1.298(8) . ? C40 H40 0.9300 . ? C41 C42 1.388(9) . ? C41 C46 1.419(9) . ? C41 N9 1.429(8) . ? C42 C43 1.380(10) . ? C42 H42 0.9300 . ? C43 C44 1.381(10) . ? C43 H43 0.9300 . ? C44 C45 1.394(10) . ? C44 H44 0.9300 . ? C45 C46 1.391(9) . ? C45 H45 0.9300 . ? C46 N10 1.420(8) . ? C47 N10 1.310(8) . ? C47 C48 1.435(10) . ? C47 H47 0.9300 . ? C48 C53 1.400(10) . ? C48 C49 1.411(9) . ? C49 C50 1.365(11) . ? C49 H49 0.9300 . ? C50 C51 1.378(12) . ? C50 H50 0.9300 . ? C51 C52 1.380(11) . ? C51 H51 0.9300 . ? C52 O4 1.396(11) . ? C52 C53 1.408(11) . ? C53 O3 1.312(8) . ? C55 O5 1.484(13) . ? C55 H55A 0.9600 . ? C55 H55B 0.9600 . ? C55 H55C 0.9600 . ? O2 Li1 2.052(17) . ? O2 Tb01 2.289(4) . ? O3 Li1 2.000(16) . ? O3 Tb01 2.290(5) . ? O4 C54A 1.440(11) . ? O4 C54 1.474(10) . ? O5 Li1 2.050(19) . ? O5 H5A 0.8650 . ? O6 H6A 1.0259 . ? O6 C56 1.411(10) . ? O6 Li1 1.80(2) . ? O6 H6A 1.0259 . ? C56 H56A 0.9600 . ? C56 H56B 0.9600 . ? C56 H56C 0.9600 . ? C56 H56D 1.1753 . ? C56 H56F 0.6852 . ? O6A C56A 1.407(11) . ? O6A Li1 1.81(2) . ? O6A H6B 0.8622 . ? C56A H56A 0.2765 . ? C56A H56D 0.9600 . ? C56A H56E 0.9600 . ? C56A H56F 0.9600 . ? Tb01 N3 2.421(5) . ? Tb01 N5 2.433(5) . ? Tb01 N1 2.436(5) . ? Tb01 N7 2.438(5) . ? Tb01 N10 2.509(5) . ? Tb01 N9 2.522(5) . ? Tb01 Li1 3.278(15) . ? O7 C60 1.415(10) . ? O7 C57 1.424(10) . ? C59 C60 1.496(11) . ? C59 C58 1.508(11) . ? C59 H59A 0.9700 . ? C59 H59B 0.9700 . ? C58 C57 1.496(11) . ? C58 H58A 0.9700 . ? C58 H58B 0.9700 . ? C60 H60A 0.9700 . ? C60 H60B 0.9700 . ? C57 H57A 0.9700 . ? C57 H57B 0.9700 . ? O7A C60A 1.427(11) . ? O7A C57A 1.432(11) . ? C58A C57A 1.500(11) . ? C58A C59A 1.511(11) . ? C58A H58C 0.9700 . ? C58A H58D 0.9700 . ? C59A C60A 1.515(11) . ? C59A H59C 0.9700 . ? C59A H59D 0.9700 . ? C60A H60C 0.9700 . ? C60A H60D 0.9700 . ? C57A H57C 0.9700 . ? C57A H57D 0.9700 . ? Li1 H5A 2.1839 . ? Li1 H6A 1.9160 . ? Li1 H6B 1.6787 . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C54A H54D 0.9600 . ? C54A H54E 0.9600 . ? C54A H54F 0.9600 . ? 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 N2 C1 N3 128.8(6) . . ? N2 C1 C2 122.3(6) . . ? N3 C1 C2 108.7(6) . . ? C7 C2 C3 121.1(6) . . ? C7 C2 C1 107.3(6) . . ? C3 C2 C1 131.7(7) . . ? C4 C3 C2 117.6(7) . . ? C4 C3 H3 121.2 . . ? C2 C3 H3 121.2 . . ? C3 C4 C5 120.8(7) . . ? C3 C4 H4 119.6 . . ? C5 C4 H4 119.6 . . ? C6 C5 C4 122.0(7) . . ? C6 C5 H5 119.0 . . ? C4 C5 H5 119.0 . . ? C5 C6 C7 116.9(7) . . ? C5 C6 H6 121.5 . . ? C7 C6 H6 121.5 . . ? C2 C7 C6 121.6(6) . . ? C2 C7 C8 106.1(5) . . ? C6 C7 C8 132.2(6) . . ? N4 C8 N3 128.2(6) . . ? N4 C8 C7 123.1(6) . . ? N3 C8 C7 108.6(5) . . ? N6 C9 N5 128.3(6) . . ? N6 C9 C10 121.6(6) . . ? N5 C9 C10 110.1(5) . . ? C11 C10 C15 120.7(6) . . ? C11 C10 C9 132.7(6) . . ? C15 C10 C9 106.6(6) . . ? C12 C11 C10 117.8(6) . . ? C12 C11 H11 121.1 . . ? C10 C11 H11 121.1 . . ? C11 C12 C13 122.8(7) . . ? C11 C12 H12 118.6 . . ? C13 C12 H12 118.6 . . ? C12 C13 C14 120.2(6) . . ? C12 C13 H13 119.9 . . ? C14 C13 H13 119.9 . . ? C15 C14 C13 116.7(6) . . ? C15 C14 H14 121.7 . . ? C13 C14 H14 121.7 . . ? C14 C15 C10 121.9(6) . . ? C14 C15 C16 132.5(6) . . ? C10 C15 C16 105.7(6) . . ? N4 C16 N5 127.3(6) . . ? N4 C16 C15 122.6(6) . . ? N5 C16 C15 110.1(5) . . ? N6 C17 N7 127.7(6) . . ? N6 C17 C18 122.6(6) . . ? N7 C17 C18 109.5(6) . . ? C23 C18 C19 121.3(6) . . ? C23 C18 C17 106.8(6) . . ? C19 C18 C17 131.9(6) . . ? C20 C19 C18 117.6(7) . . ? C20 C19 H19 121.2 . . ? C18 C19 H19 121.2 . . ? C19 C20 C21 120.7(7) . . ? C19 C20 H20 119.6 . . ? C21 C20 H20 119.6 . . ? C22 C21 C20 121.3(7) . . ? C22 C21 H21 119.4 . . ? C20 C21 H21 119.4 . . ? C21 C22 C23 118.5(7) . . ? C21 C22 H22 120.8 . . ? C23 C22 H22 120.8 . . ? C18 C23 C22 120.6(6) . . ? C18 C23 C24 106.1(6) . . ? C22 C23 C24 133.3(7) . . ? N8 C24 N7 126.9(6) . . ? N8 C24 C23 123.7(6) . . ? N7 C24 C23 109.3(6) . . ? N8 C25 N1 127.7(6) . . ? N8 C25 C26 122.3(6) . . ? N1 C25 C26 109.9(6) . . ? C27 C26 C31 120.7(7) . . ? C27 C26 C25 132.7(7) . . ? C31 C26 C25 106.6(6) . . ? C26 C27 C28 117.9(8) . . ? C26 C27 H27 121.1 . . ? C28 C27 H27 121.1 . . ? C27 C28 C29 121.0(8) . . ? C27 C28 H28 119.5 . . ? C29 C28 H28 119.5 . . ? C28 C29 C30 121.3(8) . . ? C28 C29 H29 119.4 . . ? C30 C29 H29 119.4 . . ? C31 C30 C29 117.2(7) . . ? C31 C30 H30 121.4 . . ? C29 C30 H30 121.4 . . ? C30 C31 C26 121.8(7) . . ? C30 C31 C32 132.0(7) . . ? C26 C31 C32 106.0(6) . . ? N2 C32 N1 128.8(6) . . ? N2 C32 C31 121.3(6) . . ? N1 C32 C31 109.8(6) . . ? O1 C33 H33A 109.5 . . ? O1 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? O1 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C39 C34 C35 120.0(7) . . ? C39 C34 H34 120.0 . . ? C35 C34 H34 120.0 . . ? C34 C35 O1 123.8(7) . . ? C34 C35 C36 122.6(7) . . ? O1 C35 C36 113.6(6) . . ? O2 C36 C35 119.9(6) . . ? O2 C36 C37 123.0(6) . . ? C35 C36 C37 117.1(6) . . ? C36 C37 C38 119.0(6) . . ? C36 C37 C40 124.1(6) . . ? C38 C37 C40 116.8(6) . . ? C39 C38 C37 121.5(7) . . ? C39 C38 H38 119.2 . . ? C37 C38 H38 119.2 . . ? C38 C39 C34 119.8(7) . . ? C38 C39 H39 120.1 . . ? C34 C39 H39 120.1 . . ? N9 C40 C37 125.5(6) . . ? N9 C40 H40 117.3 . . ? C37 C40 H40 117.3 . . ? C42 C41 C46 120.1(6) . . ? C42 C41 N9 124.7(6) . . ? C46 C41 N9 114.9(6) . . ? C43 C42 C41 120.2(6) . . ? C43 C42 H42 119.9 . . ? C41 C42 H42 119.9 . . ? C42 C43 C44 120.5(7) . . ? C42 C43 H43 119.8 . . ? C44 C43 H43 119.8 . . ? C43 C44 C45 120.1(7) . . ? C43 C44 H44 120.0 . . ? C45 C44 H44 120.0 . . ? C46 C45 C44 120.6(6) . . ? C46 C45 H45 119.7 . . ? C44 C45 H45 119.7 . . ? C45 C46 C41 118.6(6) . . ? C45 C46 N10 125.4(6) . . ? C41 C46 N10 115.9(6) . . ? N10 C47 C48 125.5(6) . . ? N10 C47 H47 117.3 . . ? C48 C47 H47 117.3 . . ? C53 C48 C49 120.0(7) . . ? C53 C48 C47 123.4(6) . . ? C49 C48 C47 116.5(6) . . ? C50 C49 C48 121.5(7) . . ? C50 C49 H49 119.3 . . ? C48 C49 H49 119.3 . . ? C49 C50 C51 119.1(7) . . ? C49 C50 H50 120.4 . . ? C51 C50 H50 120.4 . . ? C50 C51 C52 120.4(8) . . ? C50 C51 H51 119.8 . . ? C52 C51 H51 119.8 . . ? C51 C52 O4 123.0(8) . . ? C51 C52 C53 122.1(8) . . ? O4 C52 C53 114.9(7) . . ? O3 C53 C48 124.7(6) . . ? O3 C53 C52 118.5(7) . . ? C48 C53 C52 116.8(6) . . ? O5 C55 H55A 109.5 . . ? O5 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? O5 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C35 O1 C33 117.5(7) . . ? C36 O2 Li1 132.8(6) . . ? C36 O2 Tb01 129.2(4) . . ? Li1 O2 Tb01 97.9(5) . . ? C53 O3 Li1 131.5(6) . . ? C53 O3 Tb01 129.0(4) . . ? Li1 O3 Tb01 99.4(5) . . ? C52 O4 C54A 115.2(12) . . ? C52 O4 C54 113.1(10) . . ? C54A O4 C54 55.3(14) . . ? C55 O5 Li1 109.5(8) . . ? C55 O5 H5A 125.1 . . ? Li1 O5 H5A 87.1 . . ? H6A O6 C56 136.3 . . ? H6A O6 Li1 80.1 . . ? C56 O6 Li1 143.2(16) . . ? H6A O6 H6A 0.0 . . ? C56 O6 H6A 136.3 . . ? Li1 O6 H6A 80.1 . . ? O6 C56 H56A 111.8 . . ? O6 C56 H56B 112.0 . . ? H56A C56 H56B 109.5 . . ? O6 C56 H56C 104.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? O6 C56 H56D 108.9 . . ? H56A C56 H56D 59.9 . . ? H56B C56 H56D 138.4 . . ? H56C C56 H56D 51.7 . . ? O6 C56 H56F 138.1 . . ? H56A C56 H56F 82.6 . . ? H56B C56 H56F 30.4 . . ? H56C C56 H56F 107.1 . . ? H56D C56 H56F 112.1 . . ? C56A O6A Li1 163(2) . . ? C56A O6A H56A 10.6 . . ? Li1 O6A H56A 173.7 . . ? C56A O6A H6B 125.4 . . ? Li1 O6A H6B 67.5 . . ? H56A O6A H6B 117.0 . . ? O6A C56A H56A 99.4 . . ? O6A C56A H56B 94.9 . . ? H56A C56A H56B 120.9 . . ? O6A C56A H56C 110.1 . . ? H56A C56A H56C 147.9 . . ? H56B C56A H56C 69.9 . . ? O6A C56A H56D 117.8 . . ? H56A C56A H56D 109.1 . . ? H56B C56A H56D 113.7 . . ? H56C C56A H56D 45.8 . . ? O6A C56A H56E 104.1 . . ? H56A C56A H56E 6.1 . . ? H56B C56A H56E 116.1 . . ? H56C C56A H56E 144.7 . . ? H56D C56A H56E 109.5 . . ? O6A C56A H56F 106.2 . . ? H56A C56A H56F 114.9 . . ? H56B C56A H56F 11.7 . . ? H56C C56A H56F 69.2 . . ? H56D C56A H56F 109.5 . . ? H56E C56A H56F 109.5 . . ? O2 Tb01 O3 73.57(16) . . ? O2 Tb01 N3 81.82(17) . . ? O3 Tb01 N3 147.47(17) . . ? O2 Tb01 N5 142.15(16) . . ? O3 Tb01 N5 140.89(17) . . ? N3 Tb01 N5 70.02(17) . . ? O2 Tb01 N1 84.56(17) . . ? O3 Tb01 N1 85.28(18) . . ? N3 Tb01 N1 71.30(17) . . ? N5 Tb01 N1 108.55(18) . . ? O2 Tb01 N7 145.44(18) . . ? O3 Tb01 N7 81.27(17) . . ? N3 Tb01 N7 109.94(17) . . ? N5 Tb01 N7 70.46(17) . . ? N1 Tb01 N7 69.90(18) . . ? O2 Tb01 N10 109.79(16) . . ? O3 Tb01 N10 72.45(17) . . ? N3 Tb01 N10 137.40(18) . . ? N5 Tb01 N10 78.05(17) . . ? N1 Tb01 N10 147.97(16) . . ? N7 Tb01 N10 83.91(17) . . ? O2 Tb01 N9 72.55(17) . . ? O3 Tb01 N9 108.49(17) . . ? N3 Tb01 N9 83.24(16) . . ? N5 Tb01 N9 79.30(16) . . ? N1 Tb01 N9 147.94(17) . . ? N7 Tb01 N9 139.35(18) . . ? N10 Tb01 N9 63.32(16) . . ? O2 Tb01 Li1 38.3(3) . . ? O3 Tb01 Li1 37.0(3) . . ? N3 Tb01 Li1 112.8(3) . . ? N5 Tb01 Li1 176.3(3) . . ? N1 Tb01 Li1 74.9(4) . . ? N7 Tb01 Li1 110.1(3) . . ? N10 Tb01 Li1 98.3(3) . . ? N9 Tb01 Li1 98.4(3) . . ? C25 N1 C32 107.7(6) . . ? C25 N1 Tb01 125.3(4) . . ? C32 N1 Tb01 124.0(4) . . ? C1 N2 C32 122.5(6) . . ? C1 N3 C8 109.1(5) . . ? C1 N3 Tb01 121.5(4) . . ? C8 N3 Tb01 121.9(4) . . ? C16 N4 C8 122.7(6) . . ? C9 N5 C16 107.4(5) . . ? C9 N5 Tb01 122.8(4) . . ? C16 N5 Tb01 124.2(4) . . ? C9 N6 C17 123.0(6) . . ? C17 N7 C24 108.2(5) . . ? C17 N7 Tb01 119.8(4) . . ? C24 N7 Tb01 121.8(4) . . ? C24 N8 C25 123.0(6) . . ? C40 N9 C41 118.9(5) . . ? C40 N9 Tb01 127.2(5) . . ? C41 N9 Tb01 113.7(4) . . ? C47 N10 C46 119.4(6) . . ? C47 N10 Tb01 126.6(5) . . ? C46 N10 Tb01 113.6(4) . . ? C60 O7 C57 106.4(10) . . ? C60 C59 C58 105.4(9) . . ? C60 C59 H59A 110.7 . . ? C58 C59 H59A 110.7 . . ? C60 C59 H59B 110.7 . . ? C58 C59 H59B 110.7 . . ? H59A C59 H59B 108.8 . . ? C57 C58 C59 102.8(9) . . ? C57 C58 H58A 111.2 . . ? C59 C58 H58A 111.2 . . ? C57 C58 H58B 111.2 . . ? C59 C58 H58B 111.2 . . ? H58A C58 H58B 109.1 . . ? O7 C60 C59 107.1(9) . . ? O7 C60 H60A 110.3 . . ? C59 C60 H60A 110.3 . . ? O7 C60 H60B 110.3 . . ? C59 C60 H60B 110.3 . . ? H60A C60 H60B 108.6 . . ? O7 C57 C58 104.9(10) . . ? O7 C57 H57A 110.8 . . ? C58 C57 H57A 110.8 . . ? O7 C57 H57B 110.8 . . ? C58 C57 H57B 110.8 . . ? H57A C57 H57B 108.8 . . ? C60A O7A C57A 106.9(11) . . ? C57A C58A C59A 101.1(11) . . ? C57A C58A H58C 111.5 . . ? C59A C58A H58C 111.5 . . ? C57A C58A H58D 111.5 . . ? C59A C58A H58D 111.5 . . ? H58C C58A H58D 109.4 . . ? C58A C59A C60A 102.5(12) . . ? C58A C59A H59C 111.3 . . ? C60A C59A H59C 111.3 . . ? C58A C59A H59D 111.3 . . ? C60A C59A H59D 111.3 . . ? H59C C59A H59D 109.2 . . ? O7A C60A C59A 102.1(12) . . ? O7A C60A H60C 111.3 . . ? C59A C60A H60C 111.3 . . ? O7A C60A H60D 111.3 . . ? C59A C60A H60D 111.3 . . ? H60C C60A H60D 109.2 . . ? O7A C57A C58A 109.1(10) . . ? O7A C57A H57C 109.9 . . ? C58A C57A H57C 109.9 . . ? O7A C57A H57D 109.9 . . ? C58A C57A H57D 109.9 . . ? H57C C57A H57D 108.3 . . ? O6 Li1 O6A 34.2(8) . . ? O6 Li1 O3 118.5(10) . . ? O6A Li1 O3 130.0(11) . . ? O6 Li1 O5 132.7(10) . . ? O6A Li1 O5 100.3(10) . . ? O3 Li1 O5 101.1(8) . . ? O6 Li1 O2 103.8(9) . . ? O6A Li1 O2 131.3(12) . . ? O3 Li1 O2 85.2(6) . . ? O5 Li1 O2 104.5(8) . . ? O6 Li1 Tb01 108.5(8) . . ? O6A Li1 Tb01 141.4(11) . . ? O3 Li1 Tb01 43.6(3) . . ? O5 Li1 Tb01 118.2(8) . . ? O2 Li1 Tb01 43.8(3) . . ? O6 Li1 H5A 113.5 . . ? O6A Li1 H5A 85.7 . . ? O3 Li1 H5A 124.2 . . ? O5 Li1 H5A 23.3 . . ? O2 Li1 H5A 101.5 . . ? Tb01 Li1 H5A 131.3 . . ? O6 Li1 H6A 31.8 . . ? O6A Li1 H6A 65.8 . . ? O3 Li1 H6A 104.5 . . ? O5 Li1 H6A 154.2 . . ? O2 Li1 H6A 74.1 . . ? Tb01 Li1 H6A 79.2 . . ? H5A Li1 H6A 130.9 . . ? O6 Li1 H6B 59.4 . . ? O6A Li1 H6B 28.3 . . ? O3 Li1 H6B 144.2 . . ? O5 Li1 H6B 73.4 . . ? O2 Li1 H6B 130.6 . . ? Tb01 Li1 H6B 166.9 . . ? H5A Li1 H6B 57.4 . . ? H6A Li1 H6B 87.9 . . ? O4 C54 H54A 109.5 . . ? O4 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? O4 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? O4 C54A H54D 109.5 . . ? O4 C54A H54E 109.5 . . ? H54D C54A H54E 109.5 . . ? O4 C54A H54F 109.5 . . ? H54D C54A H54F 109.5 . . ? H54E C54A H54F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.738 _refine_diff_density_min -1.099 _refine_diff_density_rms 0.126 _database_code_depnum_ccdc_archive 'CCDC 955768' ####################################################################### # # 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_TbNa1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C55 H38 N10 Na O5 Tb' _chemical_formula_weight 1100.86 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' Na Na 0.0362 0.0249 '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 Orthorhombic _symmetry_space_group_name_H-M Pbcm _symmetry_space_group_name_Hall '-P 2c 2b' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z-1/2' '-x, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 8.3000(7) _cell_length_b 28.4450(3) _cell_length_c 18.8690(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4454.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 149.95(10) _cell_measurement_reflns_used 10884 _cell_measurement_theta_min 2.8586 _cell_measurement_theta_max 28.5316 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.641 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2216 _exptl_absorpt_coefficient_mu 1.664 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4351 _exptl_absorpt_correction_T_max 0.9068 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 149.95(10) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.2141 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 30918 _diffrn_reflns_av_R_equivalents 0.0449 _diffrn_reflns_av_sigmaI/netI 0.0257 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.86 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4038 _reflns_number_gt 3473 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker FRAMBO' _computing_cell_refinement 'Bruker FRAMBO' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0239P)^2^+8.4154P] 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 4038 _refine_ls_number_parameters 335 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0372 _refine_ls_R_factor_gt 0.0273 _refine_ls_wR_factor_ref 0.0651 _refine_ls_wR_factor_gt 0.0615 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.106 _refine_ls_shift/su_max 0.184 _refine_ls_shift/su_mean 0.004 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 -0.5562(4) -0.03608(12) -0.2128(2) 0.0288(8) Uani 1 1 d . . . H1 H -0.6203 -0.0576 -0.1886 0.035 Uiso 1 1 calc R . . C2 C -0.4629(4) -0.00481(11) -0.17493(19) 0.0243(7) Uani 1 1 d . . . H2 H -0.4643 -0.0045 -0.1256 0.029 Uiso 1 1 calc R . . C3 C -0.3666(4) 0.02628(11) -0.21275(17) 0.0199(7) Uani 1 1 d . . . C4 C -0.2521(4) 0.06235(11) -0.19108(17) 0.0189(7) Uani 1 1 d . . . C5 C -0.1297(3) 0.10897(11) -0.10339(17) 0.0176(7) Uani 1 1 d . . . C6 C -0.1202(4) 0.12484(11) -0.02987(17) 0.0198(7) Uani 1 1 d . . . C7 C -0.1951(4) 0.10955(12) 0.03171(17) 0.0236(7) Uani 1 1 d . . . H7 H -0.2637 0.0837 0.0315 0.028 Uiso 1 1 calc R . . C8 C -0.1639(4) 0.13417(13) 0.09348(18) 0.0289(8) Uani 1 1 d . . . H8 H -0.2130 0.1247 0.1354 0.035 Uiso 1 1 calc R . . C9 C -0.0603(4) 0.17298(13) 0.09423(18) 0.0295(8) Uani 1 1 d . . . H9 H -0.0411 0.1887 0.1366 0.035 Uiso 1 1 calc R . . C10 C 0.0138(4) 0.18816(12) 0.03256(17) 0.0244(7) Uani 1 1 d . . . H10 H 0.0824 0.2140 0.0328 0.029 Uiso 1 1 calc R . . C11 C -0.0170(4) 0.16378(11) -0.02959(17) 0.0198(7) Uani 1 1 d . . . C12 C 0.0340(4) 0.17044(11) -0.10321(16) 0.0176(7) Uani 1 1 d . . . C13 C 0.1643(4) 0.21515(11) -0.19119(17) 0.0184(7) Uani 1 1 d . . . C14 C 0.2563(4) 0.25654(11) -0.21285(16) 0.0182(7) Uani 1 1 d . . . C15 C 0.3316(4) 0.29224(11) -0.17490(18) 0.0220(7) Uani 1 1 d . . . H15 H 0.3295 0.2927 -0.1256 0.026 Uiso 1 1 calc R . . C16 C 0.4100(4) 0.32718(11) -0.21292(18) 0.0248(7) Uani 1 1 d . . . H16 H 0.4634 0.3510 -0.1887 0.030 Uiso 1 1 calc R . . C17 C 0.5562(5) 0.20710(13) -0.0667(2) 0.0472(12) Uani 1 1 d . . . H17A H 0.6084 0.2284 -0.0987 0.071 Uiso 1 1 calc R . . H17B H 0.6320 0.1967 -0.0315 0.071 Uiso 1 1 calc R . . H17C H 0.4679 0.2228 -0.0438 0.071 Uiso 1 1 calc R . . C18 C 0.4189(4) 0.13346(12) -0.06652(18) 0.0260(8) Uani 1 1 d . . . C19 C 0.4221(4) 0.12853(14) 0.00567(19) 0.0322(9) Uani 1 1 d . . . H19 H 0.4751 0.1508 0.0332 0.039 Uiso 1 1 calc R . . C20 C 0.3468(5) 0.09043(14) 0.03831(19) 0.0343(9) Uani 1 1 d . . . H20 H 0.3496 0.0874 0.0874 0.041 Uiso 1 1 calc R . . C21 C 0.2689(4) 0.05755(13) -0.00164(18) 0.0303(8) Uani 1 1 d . . . H21 H 0.2253 0.0311 0.0202 0.036 Uiso 1 1 calc R . . C22 C 0.2534(4) 0.06313(12) -0.07611(17) 0.0231(7) Uani 1 1 d . . . C23 C 0.3292(4) 0.10200(11) -0.10970(17) 0.0200(7) Uani 1 1 d . . . C24 C 0.1693(4) 0.02729(11) -0.11518(17) 0.0226(7) Uani 1 1 d . . . H24 H 0.1531 -0.0013 -0.0923 0.027 Uiso 1 1 calc R . . C25 C 0.0393(4) -0.00851(10) -0.21243(17) 0.0187(7) Uani 1 1 d . . . C26 C -0.0341(4) -0.04550(11) -0.17685(19) 0.0249(7) Uani 1 1 d . . . H26 H -0.0352 -0.0457 -0.1276 0.030 Uiso 1 1 calc R . . C27 C -0.1052(4) -0.08188(12) -0.21353(19) 0.0293(8) Uani 1 1 d . . . H27 H -0.1533 -0.1065 -0.1889 0.035 Uiso 1 1 calc R . . C28 C 0.7655(10) 0.2444(3) -0.2500 0.091(3) Uani 1 2 d SDU . . H28A H 0.6736 0.2625 -0.2352 0.136 Uiso 0.50 1 calc PR . . H28B H 0.7966 0.2538 -0.2969 0.136 Uiso 0.50 1 calc PR . . H28C H 0.8532 0.2498 -0.2179 0.136 Uiso 0.50 1 calc PR . . N1 N -0.1823(5) 0.08253(13) -0.2500 0.0191(8) Uani 1 2 d S . . N2 N -0.2269(3) 0.07364(9) -0.12321(14) 0.0197(6) Uani 1 1 d . . . N3 N -0.0332(3) 0.13617(9) -0.14540(14) 0.0189(6) Uani 1 1 d . . . N4 N 0.1287(3) 0.20609(9) -0.12318(13) 0.0184(6) Uani 1 1 d . . . N5 N 0.1147(4) 0.19064(13) -0.2500 0.0180(8) Uani 1 2 d S . . N6 N 0.1140(3) 0.03092(9) -0.17916(13) 0.0172(6) Uani 1 1 d . . . O1 O 0.4975(3) 0.16759(8) -0.10505(13) 0.0311(6) Uani 1 1 d . . . O2 O 0.3208(3) 0.10986(7) -0.17814(11) 0.0207(5) Uani 1 1 d . . . O3 O 0.7259(6) 0.19647(17) -0.2500 0.0694(14) Uani 1 2 d SDU . . H3A H 0.7947 0.1733 -0.2500 0.104 Uiso 1 2 d SRD . . Na1 Na 0.5099(3) 0.14947(8) -0.2500 0.0446(6) Uani 1 2 d S . . Tb1 Tb 0.10318(3) 0.104459(7) -0.2500 0.01580(8) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0187(18) 0.0213(18) 0.046(2) 0.0052(16) 0.0045(15) -0.0009(14) C2 0.0207(17) 0.0206(18) 0.0317(19) 0.0025(15) 0.0042(15) 0.0016(14) C3 0.0162(17) 0.0144(16) 0.0290(17) -0.0001(14) 0.0010(13) 0.0017(12) C4 0.0169(16) 0.0152(16) 0.0247(17) 0.0003(13) -0.0001(13) 0.0024(13) C5 0.0146(16) 0.0161(16) 0.0222(16) 0.0001(13) 0.0022(13) 0.0028(12) C6 0.0217(17) 0.0172(16) 0.0205(16) -0.0004(13) 0.0013(14) 0.0050(13) C7 0.0225(18) 0.0247(18) 0.0236(17) 0.0033(14) 0.0023(14) -0.0005(14) C8 0.0301(19) 0.036(2) 0.0208(18) 0.0050(16) 0.0058(15) 0.0013(16) C9 0.035(2) 0.035(2) 0.0188(17) -0.0023(15) -0.0008(15) -0.0020(16) C10 0.0278(19) 0.0227(18) 0.0226(17) 0.0009(15) -0.0016(15) -0.0022(15) C11 0.0209(17) 0.0185(17) 0.0200(17) 0.0013(14) 0.0016(14) 0.0048(13) C12 0.0180(16) 0.0154(17) 0.0193(16) -0.0009(13) -0.0008(13) 0.0036(13) C13 0.0215(16) 0.0136(16) 0.0201(16) -0.0020(13) 0.0006(13) 0.0037(13) C14 0.0185(16) 0.0135(16) 0.0228(16) -0.0003(13) 0.0007(13) 0.0021(13) C15 0.0259(17) 0.0175(17) 0.0227(17) -0.0037(14) -0.0014(14) -0.0004(14) C16 0.0234(18) 0.0171(17) 0.0340(18) -0.0047(14) -0.0038(15) -0.0025(14) C17 0.060(3) 0.024(2) 0.058(3) -0.009(2) -0.027(2) -0.0011(19) C18 0.0217(18) 0.0260(19) 0.0302(19) -0.0053(15) -0.0053(15) 0.0042(14) C19 0.033(2) 0.036(2) 0.0277(19) -0.0143(17) -0.0122(16) 0.0101(17) C20 0.038(2) 0.048(2) 0.0174(17) -0.0030(17) -0.0052(16) 0.0091(18) C21 0.033(2) 0.037(2) 0.0205(18) 0.0033(16) 0.0030(16) 0.0066(17) C22 0.0249(18) 0.0273(19) 0.0169(16) -0.0009(14) 0.0004(14) 0.0048(14) C23 0.0165(15) 0.0220(17) 0.0215(16) -0.0036(14) -0.0003(13) 0.0057(13) C24 0.0258(18) 0.0208(18) 0.0213(17) 0.0038(14) 0.0054(14) 0.0026(14) C25 0.0181(16) 0.0127(16) 0.0253(17) -0.0003(13) -0.0017(14) 0.0038(13) C26 0.0273(18) 0.0207(18) 0.0268(18) 0.0045(15) 0.0021(15) -0.0005(15) C27 0.0251(18) 0.0194(17) 0.043(2) 0.0040(16) 0.0011(16) -0.0019(15) C28 0.071(4) 0.077(4) 0.124(5) 0.000 0.000 0.010(4) N1 0.022(2) 0.0155(19) 0.020(2) 0.000 0.000 0.0022(16) N2 0.0188(14) 0.0175(14) 0.0228(14) -0.0004(12) 0.0024(11) 0.0014(11) N3 0.0216(14) 0.0153(14) 0.0198(14) 0.0013(11) 0.0018(11) 0.0001(11) N4 0.0248(15) 0.0143(13) 0.0160(13) -0.0022(11) 0.0015(11) -0.0001(11) N5 0.024(2) 0.0150(19) 0.0147(18) 0.000 0.000 -0.0013(16) N6 0.0188(13) 0.0154(13) 0.0173(13) -0.0012(11) 0.0020(11) 0.0016(11) O1 0.0309(14) 0.0250(13) 0.0372(15) -0.0069(11) -0.0067(12) -0.0060(10) O2 0.0216(11) 0.0228(12) 0.0177(11) -0.0003(9) -0.0032(9) -0.0023(10) O3 0.055(3) 0.058(3) 0.094(3) 0.000 0.000 0.009(2) Na1 0.0482(14) 0.0488(14) 0.0369(12) 0.000 0.000 -0.0032(11) Tb1 0.01994(12) 0.01276(12) 0.01471(11) 0.000 0.000 -0.00019(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.379(5) . ? C1 C1 1.405(7) 6 ? C1 H1 0.9300 . ? C2 C3 1.389(4) . ? C2 H2 0.9300 . ? C3 C3 1.406(7) 6 ? C3 C4 1.457(4) . ? C4 N2 1.337(4) . ? C4 N1 1.379(4) . ? C5 N2 1.342(4) . ? C5 N3 1.367(4) . ? C5 C6 1.461(4) . ? C6 C7 1.388(4) . ? C6 C11 1.400(5) . ? C7 C8 1.384(5) . ? C7 H7 0.9300 . ? C8 C9 1.399(5) . ? C8 H8 0.9300 . ? C9 C10 1.385(5) . ? C9 H9 0.9300 . ? C10 C11 1.386(4) . ? C10 H10 0.9300 . ? C11 C12 1.465(4) . ? C12 N4 1.337(4) . ? C12 N3 1.376(4) . ? C13 N4 1.342(4) . ? C13 N5 1.374(4) . ? C13 C14 1.462(4) . ? C14 C15 1.391(4) . ? C14 C14 1.402(6) 6 ? C15 C16 1.388(5) . ? C15 H15 0.9300 . ? C16 C16 1.399(7) 6 ? C16 H16 0.9300 . ? C17 O1 1.423(4) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C19 1.370(5) . ? C18 O1 1.377(4) . ? C18 C23 1.421(5) . ? C19 C20 1.395(6) . ? C19 H19 0.9300 . ? C20 C21 1.364(5) . ? C20 H20 0.9300 . ? C21 C22 1.420(5) . ? C21 H21 0.9300 . ? C22 C23 1.421(5) . ? C22 C24 1.439(5) . ? C23 O2 1.312(4) . ? C24 N6 1.296(4) . ? C24 H24 0.9300 . ? C25 C26 1.389(4) . ? C25 C25 1.418(6) 6 ? C25 N6 1.427(4) . ? C26 C27 1.378(5) . ? C26 H26 0.9300 . ? C27 C27 1.376(7) 6 ? C27 H27 0.9300 . ? C28 O3 1.403(9) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? N1 C4 1.379(4) 6 ? N1 Tb1 2.450(4) . ? N3 Tb1 2.447(3) . ? N5 C13 1.374(4) 6 ? N5 Tb1 2.453(4) . ? N6 Tb1 2.484(2) . ? O1 Na1 2.785(3) . ? O2 Tb1 2.264(2) . ? O2 Na1 2.360(3) . ? O3 Na1 2.236(5) . ? O3 H3A 0.8718 . ? Na1 O2 2.360(3) 6 ? Na1 O1 2.785(3) 6 ? Na1 Tb1 3.611(2) . ? Na1 H3A 2.4595 . ? Tb1 O2 2.264(2) 6 ? Tb1 N3 2.447(3) 6 ? Tb1 N6 2.484(2) 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 C2 C1 C1 121.2(2) . 6 ? C2 C1 H1 119.4 . . ? C1 C1 H1 119.4 6 . ? C1 C2 C3 117.9(3) . . ? C1 C2 H2 121.1 . . ? C3 C2 H2 121.1 . . ? C2 C3 C3 120.9(2) . 6 ? C2 C3 C4 132.8(3) . . ? C3 C3 C4 106.29(18) 6 . ? N2 C4 N1 127.3(3) . . ? N2 C4 C3 122.7(3) . . ? N1 C4 C3 109.9(3) . . ? N2 C5 N3 127.9(3) . . ? N2 C5 C6 121.9(3) . . ? N3 C5 C6 110.1(3) . . ? C7 C6 C11 121.2(3) . . ? C7 C6 C5 132.4(3) . . ? C11 C6 C5 106.3(3) . . ? C8 C7 C6 117.6(3) . . ? C8 C7 H7 121.2 . . ? C6 C7 H7 121.2 . . ? C7 C8 C9 121.5(3) . . ? C7 C8 H8 119.3 . . ? C9 C8 H8 119.3 . . ? C10 C9 C8 120.7(3) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? C9 C10 C11 118.2(3) . . ? C9 C10 H10 120.9 . . ? C11 C10 H10 120.9 . . ? C10 C11 C6 120.8(3) . . ? C10 C11 C12 133.2(3) . . ? C6 C11 C12 106.0(3) . . ? N4 C12 N3 127.7(3) . . ? N4 C12 C11 122.4(3) . . ? N3 C12 C11 109.9(3) . . ? N4 C13 N5 127.5(3) . . ? N4 C13 C14 122.5(3) . . ? N5 C13 C14 109.8(3) . . ? C15 C14 C14 120.99(19) . 6 ? C15 C14 C13 132.8(3) . . ? C14 C14 C13 106.24(17) 6 . ? C16 C15 C14 117.9(3) . . ? C16 C15 H15 121.1 . . ? C14 C15 H15 121.1 . . ? C15 C16 C16 121.14(19) . 6 ? C15 C16 H16 119.4 . . ? C16 C16 H16 119.4 6 . ? O1 C17 H17A 109.5 . . ? O1 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? O1 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 O1 126.0(3) . . ? C19 C18 C23 121.1(3) . . ? O1 C18 C23 112.9(3) . . ? C18 C19 C20 120.7(3) . . ? C18 C19 H19 119.7 . . ? C20 C19 H19 119.7 . . ? C21 C20 C19 120.1(3) . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C20 C21 C22 120.9(4) . . ? C20 C21 H21 119.6 . . ? C22 C21 H21 119.6 . . ? C21 C22 C23 119.2(3) . . ? C21 C22 C24 118.1(3) . . ? C23 C22 C24 122.5(3) . . ? O2 C23 C18 119.0(3) . . ? O2 C23 C22 123.2(3) . . ? C18 C23 C22 117.8(3) . . ? N6 C24 C22 126.4(3) . . ? N6 C24 H24 116.8 . . ? C22 C24 H24 116.8 . . ? C26 C25 C25 118.9(2) . 6 ? C26 C25 N6 125.0(3) . . ? C25 C25 N6 116.10(16) 6 . ? C27 C26 C25 120.9(3) . . ? C27 C26 H26 119.5 . . ? C25 C26 H26 119.5 . . ? C27 C27 C26 120.2(2) 6 . ? C27 C27 H27 119.9 6 . ? C26 C27 H27 119.9 . . ? O3 C28 H28A 109.5 . . ? O3 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? O3 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C4 N1 C4 107.5(4) 6 . ? C4 N1 Tb1 120.8(2) 6 . ? C4 N1 Tb1 120.8(2) . . ? C4 N2 C5 122.8(3) . . ? C5 N3 C12 107.6(3) . . ? C5 N3 Tb1 122.01(19) . . ? C12 N3 Tb1 122.7(2) . . ? C12 N4 C13 123.0(3) . . ? C13 N5 C13 107.8(4) 6 . ? C13 N5 Tb1 121.24(19) 6 . ? C13 N5 Tb1 121.24(19) . . ? C24 N6 C25 120.1(3) . . ? C24 N6 Tb1 125.5(2) . . ? C25 N6 Tb1 114.16(18) . . ? C18 O1 C17 116.8(3) . . ? C18 O1 Na1 113.91(19) . . ? C17 O1 Na1 129.3(2) . . ? C23 O2 Tb1 128.3(2) . . ? C23 O2 Na1 127.7(2) . . ? Tb1 O2 Na1 102.64(9) . . ? C28 O3 Na1 140.3(5) . . ? C28 O3 H3A 125.5 . . ? Na1 O3 H3A 94.2 . . ? O3 Na1 O2 144.93(6) . . ? O3 Na1 O2 144.93(6) . 6 ? O2 Na1 O2 70.12(12) . 6 ? O3 Na1 O1 85.35(7) . 6 ? O2 Na1 O1 128.89(11) . 6 ? O2 Na1 O1 59.98(7) 6 6 ? O3 Na1 O1 85.35(7) . . ? O2 Na1 O1 59.98(7) . . ? O2 Na1 O1 128.89(11) 6 . ? O1 Na1 O1 158.23(14) 6 . ? O3 Na1 Tb1 164.05(16) . . ? O2 Na1 Tb1 37.72(6) . . ? O2 Na1 Tb1 37.72(6) 6 . ? O1 Na1 Tb1 91.78(7) 6 . ? O1 Na1 Tb1 91.78(7) . . ? O3 Na1 H3A 20.7 . . ? O2 Na1 H3A 140.4 . . ? O2 Na1 H3A 140.4 6 . ? O1 Na1 H3A 89.1 6 . ? O1 Na1 H3A 89.1 . . ? Tb1 Na1 H3A 175.2 . . ? O2 Tb1 O2 73.59(11) . 6 ? O2 Tb1 N3 145.79(8) . 6 ? O2 Tb1 N3 82.01(8) 6 6 ? O2 Tb1 N3 82.01(8) . . ? O2 Tb1 N3 145.79(8) 6 . ? N3 Tb1 N3 107.51(12) 6 . ? O2 Tb1 N1 142.08(6) . . ? O2 Tb1 N1 142.08(6) 6 . ? N3 Tb1 N1 69.31(7) 6 . ? N3 Tb1 N1 69.31(7) . . ? O2 Tb1 N5 84.33(9) . . ? O2 Tb1 N5 84.33(9) 6 . ? N3 Tb1 N5 69.49(7) 6 . ? N3 Tb1 N5 69.49(7) . . ? N1 Tb1 N5 106.98(12) . . ? O2 Tb1 N6 110.52(8) . 6 ? O2 Tb1 N6 72.90(8) 6 6 ? N3 Tb1 N6 83.87(8) 6 6 ? N3 Tb1 N6 139.56(8) . 6 ? N1 Tb1 N6 79.67(9) . 6 ? N5 Tb1 N6 147.15(6) . 6 ? O2 Tb1 N6 72.90(8) . . ? O2 Tb1 N6 110.52(8) 6 . ? N3 Tb1 N6 139.56(8) 6 . ? N3 Tb1 N6 83.87(8) . . ? N1 Tb1 N6 79.67(9) . . ? N5 Tb1 N6 147.15(6) . . ? N6 Tb1 N6 65.11(11) 6 . ? O2 Tb1 Na1 39.64(6) . . ? O2 Tb1 Na1 39.64(6) 6 . ? N3 Tb1 Na1 107.56(6) 6 . ? N3 Tb1 Na1 107.56(6) . . ? N1 Tb1 Na1 173.98(9) . . ? N5 Tb1 Na1 67.01(9) . . ? N6 Tb1 Na1 105.35(7) 6 . ? N6 Tb1 Na1 105.35(7) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.986 _refine_diff_density_min -0.620 _refine_diff_density_rms 0.084 _database_code_depnum_ccdc_archive 'CCDC 955769' ####################################################################### # # 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_TbK _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C55 H38 K N10 O5 Tb' _chemical_formula_weight 1116.97 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' K K 0.2009 0.2494 '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 Orthorhombic _symmetry_space_group_name_H-M Pbcm _symmetry_space_group_name_Hall '-P 2c 2b' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z-1/2' '-x, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 8.4313(3) _cell_length_b 28.1513(10) _cell_length_c 18.9773(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4504.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 149.95(10) _cell_measurement_reflns_used 3768 _cell_measurement_theta_min 2.8885 _cell_measurement_theta_max 28.5808 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.647 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2248 _exptl_absorpt_coefficient_mu 1.729 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7815 _exptl_absorpt_correction_T_max 0.8741 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 149.95(10) _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, Eos, Gemini' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.2141 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 23572 _diffrn_reflns_av_R_equivalents 0.0964 _diffrn_reflns_av_sigmaI/netI 0.0724 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.89 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4084 _reflns_number_gt 3107 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker FRAMBO' _computing_cell_refinement 'Bruker FRAMBO' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0248P)^2^+3.3965P] 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 4084 _refine_ls_number_parameters 338 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0730 _refine_ls_R_factor_gt 0.0451 _refine_ls_wR_factor_ref 0.0798 _refine_ls_wR_factor_gt 0.0736 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.5590(5) -0.03429(17) -0.2131(3) 0.0334(15) Uani 1 1 d . . . H1 H -0.6244 -0.0554 -0.1891 0.040 Uiso 1 1 calc R . . C2 C -0.4641(6) -0.00356(16) -0.1751(3) 0.0266(13) Uani 1 1 d . . . H2 H -0.4656 -0.0033 -0.1261 0.032 Uiso 1 1 calc R . . C3 C -0.3659(5) 0.02704(15) -0.2131(3) 0.0208(12) Uani 1 1 d . . . C4 C -0.2497(5) 0.06269(16) -0.1913(3) 0.0203(12) Uani 1 1 d . . . C5 C -0.1281(5) 0.10932(16) -0.1044(3) 0.0195(11) Uani 1 1 d . . . C6 C -0.1178(6) 0.12506(16) -0.0310(2) 0.0200(11) Uani 1 1 d . . . C7 C -0.1923(6) 0.11020(18) 0.0300(3) 0.0272(12) Uani 1 1 d . . . H7 H -0.2621 0.0846 0.0295 0.033 Uiso 1 1 calc R . . C8 C -0.1600(6) 0.13442(19) 0.0917(3) 0.0356(14) Uani 1 1 d . . . H8 H -0.2089 0.1251 0.1334 0.043 Uiso 1 1 calc R . . C9 C -0.0547(6) 0.1727(2) 0.0920(3) 0.0386(15) Uani 1 1 d . . . H9 H -0.0337 0.1884 0.1342 0.046 Uiso 1 1 calc R . . C10 C 0.0190(6) 0.18783(19) 0.0310(3) 0.0311(14) Uani 1 1 d . . . H10 H 0.0886 0.2135 0.0315 0.037 Uiso 1 1 calc R . . C11 C -0.0136(6) 0.16386(17) -0.0305(3) 0.0224(12) Uani 1 1 d . . . C12 C 0.0376(5) 0.17038(17) -0.1037(3) 0.0182(11) Uani 1 1 d . . . C13 C 0.1682(5) 0.21477(16) -0.1917(3) 0.0185(11) Uani 1 1 d . . . C14 C 0.2636(5) 0.25590(15) -0.2130(2) 0.0186(11) Uani 1 1 d . . . C15 C 0.3398(5) 0.29162(16) -0.1754(3) 0.0238(12) Uani 1 1 d . . . H15 H 0.3385 0.2920 -0.1264 0.029 Uiso 1 1 calc R . . C16 C 0.4177(5) 0.32655(16) -0.2132(3) 0.0252(12) Uani 1 1 d . . . H16 H 0.4710 0.3505 -0.1891 0.030 Uiso 1 1 calc R . . C17 C 0.5515(7) 0.20493(18) -0.0637(3) 0.0416(16) Uani 1 1 d . . . H17A H 0.6040 0.2266 -0.0950 0.062 Uiso 1 1 calc R . . H17B H 0.6252 0.1940 -0.0288 0.062 Uiso 1 1 calc R . . H17C H 0.4646 0.2208 -0.0411 0.062 Uiso 1 1 calc R . . C18 C 0.4126(6) 0.13038(17) -0.0651(3) 0.0244(12) Uani 1 1 d . . . C19 C 0.4168(6) 0.12503(19) 0.0062(3) 0.0314(13) Uani 1 1 d . . . H19 H 0.4697 0.1472 0.0338 0.038 Uiso 1 1 calc R . . C20 C 0.3419(6) 0.08626(19) 0.0380(3) 0.0326(14) Uani 1 1 d . . . H20 H 0.3469 0.0824 0.0866 0.039 Uiso 1 1 calc R . . C21 C 0.2613(6) 0.05403(19) -0.0022(3) 0.0296(13) Uani 1 1 d . . . H21 H 0.2156 0.0276 0.0191 0.035 Uiso 1 1 calc R . . C22 C 0.2465(6) 0.06034(16) -0.0761(3) 0.0214(12) Uani 1 1 d . . . C23 C 0.3223(6) 0.09975(17) -0.1090(2) 0.0207(11) Uani 1 1 d . . . C24 C 0.1610(6) 0.02495(17) -0.1155(3) 0.0234(12) Uani 1 1 d . . . H24 H 0.1412 -0.0037 -0.0928 0.028 Uiso 1 1 calc R . . C25 C 0.0329(5) -0.01066(15) -0.2125(2) 0.0206(12) Uani 1 1 d . . . C26 C -0.0417(6) -0.04744(16) -0.1774(3) 0.0247(12) Uani 1 1 d . . . H26 H -0.0444 -0.0473 -0.1284 0.030 Uiso 1 1 calc R . . C27 C -0.1120(6) -0.08419(17) -0.2136(3) 0.0304(13) Uani 1 1 d . . . H27 H -0.1594 -0.1090 -0.1891 0.036 Uiso 1 1 calc R . . N1 N -0.1787(6) 0.08236(18) -0.2500 0.0183(13) Uani 1 2 d S . . N2 N -0.2252(4) 0.07381(13) -0.1239(2) 0.0199(10) Uani 1 1 d . . . N3 N -0.0310(4) 0.13629(13) -0.1462(2) 0.0210(10) Uani 1 1 d . . . N4 N 0.1334(4) 0.20561(13) -0.1237(2) 0.0185(9) Uani 1 1 d . . . N5 N 0.1189(6) 0.19024(18) -0.2500 0.0183(13) Uani 1 2 d S . . N6 N 0.1090(5) 0.02898(13) -0.1792(2) 0.0193(9) Uani 1 1 d . . . O1 O 0.4930(4) 0.16531(12) -0.10301(18) 0.0281(9) Uani 1 1 d . . . O2 O 0.3134(4) 0.10832(10) -0.17660(16) 0.0199(7) Uani 1 1 d . . . O3 O 0.7681(7) 0.2140(2) -0.2715(4) 0.042(2) Uani 0.50 1 d PDU . . H3A H 0.8119 0.1855 -0.2792 0.063 Uiso 0.50 1 d PRD . . C28 C 0.7965(14) 0.2555(4) -0.2500 0.100(4) Uani 1 2 d SDU . . H28A H 0.7141 0.2765 -0.2656 0.149 Uiso 0.50 1 calc PR . . H28B H 0.8965 0.2660 -0.2686 0.149 Uiso 0.50 1 calc PR . . H28C H 0.8007 0.2556 -0.1994 0.149 Uiso 0.50 1 calc PR . . K1 K 0.53082(19) 0.15344(6) -0.2500 0.0327(4) Uani 1 2 d S . . Tb1 Tb 0.10272(4) 0.103216(11) -0.2500 0.01708(11) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.022(3) 0.028(3) 0.051(4) 0.005(3) 0.007(3) -0.003(2) C2 0.023(3) 0.020(3) 0.037(3) -0.001(3) 0.000(3) 0.001(2) C3 0.015(3) 0.015(2) 0.033(3) 0.000(2) 0.001(2) 0.003(2) C4 0.022(3) 0.015(3) 0.025(3) 0.000(2) -0.001(2) 0.000(2) C5 0.018(3) 0.016(3) 0.024(3) 0.000(2) 0.005(2) 0.003(2) C6 0.022(3) 0.021(2) 0.017(3) -0.001(2) 0.000(2) 0.006(2) C7 0.026(3) 0.032(3) 0.024(3) 0.004(3) 0.001(2) 0.000(3) C8 0.039(3) 0.046(4) 0.022(3) 0.005(3) 0.005(3) -0.003(3) C9 0.047(4) 0.049(4) 0.020(3) -0.007(3) 0.001(3) -0.002(3) C10 0.035(3) 0.029(3) 0.029(3) -0.005(3) -0.002(3) -0.003(3) C11 0.020(3) 0.022(3) 0.025(3) -0.001(2) 0.003(2) 0.001(2) C12 0.020(3) 0.016(3) 0.018(3) -0.005(2) -0.004(2) 0.006(2) C13 0.017(3) 0.014(2) 0.024(3) 0.002(2) 0.002(2) 0.001(2) C14 0.016(3) 0.013(2) 0.027(3) -0.001(2) 0.003(2) 0.002(2) C15 0.027(3) 0.020(3) 0.024(3) -0.002(2) 0.003(2) 0.000(2) C16 0.022(3) 0.020(2) 0.034(3) -0.005(2) -0.002(2) 0.000(2) C17 0.062(4) 0.025(3) 0.038(4) -0.003(3) -0.013(3) -0.008(3) C18 0.023(3) 0.029(3) 0.021(3) -0.003(2) -0.001(3) 0.004(3) C19 0.034(3) 0.036(3) 0.024(3) -0.011(3) -0.006(3) 0.003(3) C20 0.041(3) 0.042(3) 0.015(3) -0.004(3) -0.006(3) 0.009(3) C21 0.038(3) 0.032(3) 0.019(3) 0.009(3) 0.001(3) 0.002(3) C22 0.026(3) 0.022(3) 0.016(3) -0.001(2) 0.002(2) 0.007(2) C23 0.024(3) 0.022(3) 0.017(3) -0.002(3) 0.002(2) 0.008(2) C24 0.027(3) 0.017(3) 0.026(3) 0.002(2) 0.007(2) 0.001(2) C25 0.019(3) 0.014(2) 0.029(3) -0.002(2) -0.002(2) 0.004(2) C26 0.028(3) 0.017(3) 0.029(3) 0.006(3) 0.002(2) -0.001(2) C27 0.032(3) 0.021(2) 0.038(3) 0.004(2) 0.004(3) -0.006(2) N1 0.020(3) 0.016(3) 0.019(3) 0.000 0.000 -0.001(3) N2 0.021(2) 0.017(2) 0.022(2) 0.002(2) 0.006(2) 0.0017(18) N3 0.024(2) 0.017(2) 0.022(2) -0.001(2) 0.003(2) 0.0005(19) N4 0.024(2) 0.013(2) 0.018(2) -0.0019(18) -0.0008(19) -0.0006(18) N5 0.024(3) 0.014(3) 0.017(3) 0.000 0.000 0.001(3) N6 0.017(2) 0.023(2) 0.018(2) 0.0003(18) 0.002(2) 0.000(2) O1 0.032(2) 0.026(2) 0.027(2) -0.0052(17) -0.0031(18) -0.0051(17) O2 0.0229(17) 0.0201(18) 0.0166(17) -0.0033(16) -0.0038(15) 0.0010(16) O3 0.040(3) 0.036(3) 0.051(5) -0.010(3) -0.005(3) 0.002(3) C28 0.088(5) 0.092(5) 0.119(6) 0.000 0.000 0.003(4) K1 0.0313(10) 0.0367(10) 0.0301(10) 0.000 0.000 -0.0076(8) Tb1 0.02069(18) 0.01496(17) 0.01558(17) 0.000 0.000 0.00024(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 C1 C2 1.381(7) . ? C1 C1 1.401(11) 6 ? C1 H1 0.9300 . ? C2 C3 1.395(6) . ? C2 H2 0.9300 . ? C3 C3 1.402(10) 6 ? C3 C4 1.462(6) . ? C4 N2 1.333(6) . ? C4 N1 1.381(5) . ? C4 K1 3.345(5) 1_455 ? C5 N2 1.344(6) . ? C5 N3 1.369(6) . ? C5 C6 1.465(6) . ? C6 C7 1.381(6) . ? C6 C11 1.402(6) . ? C7 C8 1.383(7) . ? C7 H7 0.9300 . ? C8 C9 1.397(7) . ? C8 H8 0.9300 . ? C9 C10 1.380(7) . ? C9 H9 0.9300 . ? C10 C11 1.376(7) . ? C10 H10 0.9300 . ? C11 C12 1.467(7) . ? C12 N4 1.334(6) . ? C12 N3 1.380(6) . ? C13 N4 1.349(6) . ? C13 N5 1.368(5) . ? C13 C14 1.467(6) . ? C14 C15 1.391(6) . ? C14 C14 1.403(9) 6 ? C15 C16 1.383(6) . ? C15 H15 0.9300 . ? C16 C16 1.397(10) 6 ? C16 H16 0.9300 . ? C17 O1 1.429(6) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C19 1.362(7) . ? C18 O1 1.394(6) . ? C18 C23 1.420(7) . ? C19 C20 1.398(7) . ? C19 H19 0.9300 . ? C20 C21 1.367(7) . ? C20 H20 0.9300 . ? C21 C22 1.418(7) . ? C21 H21 0.9300 . ? C22 C23 1.425(6) . ? C22 C24 1.440(6) . ? C23 O2 1.307(5) . ? C23 K1 3.540(5) . ? C24 N6 1.291(6) . ? C24 H24 0.9300 . ? C25 C26 1.383(6) . ? C25 C25 1.421(9) 6 ? C25 N6 1.434(6) . ? C26 C27 1.376(6) . ? C26 H26 0.9300 . ? C27 C27 1.380(10) 6 ? C27 H27 0.9300 . ? N1 C4 1.381(5) 6 ? N1 Tb1 2.445(5) . ? N1 K1 3.162(5) 1_455 ? N3 Tb1 2.453(4) . ? N5 C13 1.368(5) 6 ? N5 Tb1 2.454(5) . ? N6 Tb1 2.485(4) . ? O1 K1 2.828(3) . ? O2 Tb1 2.262(3) . ? O2 K1 2.630(3) . ? O3 O3 0.817(14) 6 ? O3 C28 1.260(10) . ? O3 K1 2.660(7) . ? O3 H3A 0.8946 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? K1 O2 2.630(3) 6 ? K1 O3 2.660(7) 6 ? K1 O1 2.828(3) 6 ? K1 N1 3.162(5) 1_655 ? K1 C4 3.345(5) 6_655 ? K1 C4 3.345(5) 1_655 ? K1 C23 3.540(5) 6 ? K1 Tb1 3.8764(16) . ? K1 H3A 2.5961 . ? Tb1 O2 2.262(3) 6 ? Tb1 N3 2.453(4) 6 ? Tb1 N6 2.485(4) 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 C2 C1 C1 121.4(3) . 6 ? C2 C1 H1 119.3 . . ? C1 C1 H1 119.3 6 . ? C1 C2 C3 117.5(5) . . ? C1 C2 H2 121.3 . . ? C3 C2 H2 121.3 . . ? C2 C3 C3 121.1(3) . 6 ? C2 C3 C4 132.5(5) . . ? C3 C3 C4 106.4(3) 6 . ? N2 C4 N1 127.8(4) . . ? N2 C4 C3 122.4(4) . . ? N1 C4 C3 109.7(4) . . ? N2 C4 K1 103.1(3) . 1_455 ? N1 C4 K1 70.4(3) . 1_455 ? C3 C4 K1 93.4(3) . 1_455 ? N2 C5 N3 128.1(4) . . ? N2 C5 C6 121.5(4) . . ? N3 C5 C6 110.4(4) . . ? C7 C6 C11 121.0(5) . . ? C7 C6 C5 132.7(4) . . ? C11 C6 C5 106.2(4) . . ? C6 C7 C8 118.1(5) . . ? C6 C7 H7 120.9 . . ? C8 C7 H7 120.9 . . ? C7 C8 C9 120.6(5) . . ? C7 C8 H8 119.7 . . ? C9 C8 H8 119.7 . . ? C10 C9 C8 121.3(5) . . ? C10 C9 H9 119.3 . . ? C8 C9 H9 119.3 . . ? C11 C10 C9 118.1(5) . . ? C11 C10 H10 121.0 . . ? C9 C10 H10 121.0 . . ? C10 C11 C6 120.9(5) . . ? C10 C11 C12 133.1(5) . . ? C6 C11 C12 106.0(4) . . ? N4 C12 N3 127.2(4) . . ? N4 C12 C11 122.7(4) . . ? N3 C12 C11 110.1(4) . . ? N4 C13 N5 127.7(4) . . ? N4 C13 C14 122.3(4) . . ? N5 C13 C14 110.0(4) . . ? C15 C14 C14 120.9(3) . 6 ? C15 C14 C13 133.1(5) . . ? C14 C14 C13 106.0(3) 6 . ? C16 C15 C14 117.9(5) . . ? C16 C15 H15 121.1 . . ? C14 C15 H15 121.1 . . ? C15 C16 C16 121.2(3) . 6 ? C15 C16 H16 119.4 . . ? C16 C16 H16 119.4 6 . ? O1 C17 H17A 109.5 . . ? O1 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? O1 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 O1 125.3(5) . . ? C19 C18 C23 122.0(5) . . ? O1 C18 C23 112.7(4) . . ? C18 C19 C20 120.2(5) . . ? C18 C19 H19 119.9 . . ? C20 C19 H19 119.9 . . ? C21 C20 C19 120.1(5) . . ? C21 C20 H20 119.9 . . ? C19 C20 H20 119.9 . . ? C20 C21 C22 120.8(5) . . ? C20 C21 H21 119.6 . . ? C22 C21 H21 119.6 . . ? C21 C22 C23 119.5(5) . . ? C21 C22 C24 118.1(5) . . ? C23 C22 C24 122.4(4) . . ? O2 C23 C18 119.7(4) . . ? O2 C23 C22 123.2(4) . . ? C18 C23 C22 117.1(4) . . ? O2 C23 K1 37.7(2) . . ? C18 C23 K1 85.3(3) . . ? C22 C23 K1 152.5(3) . . ? N6 C24 C22 126.6(5) . . ? N6 C24 H24 116.7 . . ? C22 C24 H24 116.7 . . ? C26 C25 C25 118.8(3) . 6 ? C26 C25 N6 125.0(4) . . ? C25 C25 N6 116.2(2) 6 . ? C27 C26 C25 121.1(5) . . ? C27 C26 H26 119.4 . . ? C25 C26 H26 119.4 . . ? C26 C27 C27 120.0(3) . 6 ? C26 C27 H27 120.0 . . ? C27 C27 H27 120.0 6 . ? C4 N1 C4 107.6(5) 6 . ? C4 N1 Tb1 121.1(3) 6 . ? C4 N1 Tb1 121.1(3) . . ? C4 N1 K1 85.3(3) 6 1_455 ? C4 N1 K1 85.3(3) . 1_455 ? Tb1 N1 K1 126.85(19) . 1_455 ? C4 N2 C5 122.2(4) . . ? C5 N3 C12 107.3(4) . . ? C5 N3 Tb1 122.0(3) . . ? C12 N3 Tb1 122.7(3) . . ? C12 N4 C13 123.1(4) . . ? C13 N5 C13 107.8(5) . 6 ? C13 N5 Tb1 121.4(3) . . ? C13 N5 Tb1 121.4(3) 6 . ? C24 N6 C25 119.8(4) . . ? C24 N6 Tb1 126.0(3) . . ? C25 N6 Tb1 114.0(3) . . ? C18 O1 C17 116.7(4) . . ? C18 O1 K1 118.7(3) . . ? C17 O1 K1 124.6(3) . . ? C23 O2 Tb1 129.7(3) . . ? C23 O2 K1 124.6(3) . . ? Tb1 O2 K1 104.59(11) . . ? O3 O3 C28 71.1(4) 6 . ? O3 O3 K1 81.17(16) 6 . ? C28 O3 K1 133.4(7) . . ? O3 O3 H3A 99.4 6 . ? C28 O3 H3A 143.6 . . ? K1 O3 H3A 76.2 . . ? O3 C28 H28A 109.5 . . ? O3 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? O3 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O2 K1 O2 63.97(13) 6 . ? O2 K1 O3 156.24(17) 6 6 ? O2 K1 O3 138.82(17) . 6 ? O2 K1 O3 138.82(17) 6 . ? O2 K1 O3 156.24(17) . . ? O3 K1 O3 17.7(3) 6 . ? O2 K1 O1 120.07(10) 6 . ? O2 K1 O1 57.04(9) . . ? O3 K1 O1 81.81(17) 6 . ? O3 K1 O1 99.24(17) . . ? O2 K1 O1 57.04(9) 6 6 ? O2 K1 O1 120.07(10) . 6 ? O3 K1 O1 99.24(17) 6 6 ? O3 K1 O1 81.81(17) . 6 ? O1 K1 O1 161.20(15) . 6 ? O2 K1 N1 103.55(11) 6 1_655 ? O2 K1 N1 103.55(11) . 1_655 ? O3 K1 N1 79.82(17) 6 1_655 ? O3 K1 N1 79.82(17) . 1_655 ? O1 K1 N1 99.33(7) . 1_655 ? O1 K1 N1 99.33(7) 6 1_655 ? O2 K1 C4 80.81(11) 6 6_655 ? O2 K1 C4 101.14(12) . 6_655 ? O3 K1 C4 97.16(17) 6 6_655 ? O3 K1 C4 91.29(17) . 6_655 ? O1 K1 C4 118.76(12) . 6_655 ? O1 K1 C4 79.86(11) 6 6_655 ? N1 K1 C4 24.29(9) 1_655 6_655 ? O2 K1 C4 101.14(12) 6 1_655 ? O2 K1 C4 80.81(11) . 1_655 ? O3 K1 C4 91.29(17) 6 1_655 ? O3 K1 C4 97.16(17) . 1_655 ? O1 K1 C4 79.86(11) . 1_655 ? O1 K1 C4 118.76(12) 6 1_655 ? N1 K1 C4 24.29(9) 1_655 1_655 ? C4 K1 C4 38.91(17) 6_655 1_655 ? O2 K1 C23 17.68(10) 6 6 ? O2 K1 C23 81.25(11) . 6 ? O3 K1 C23 139.74(18) 6 6 ? O3 K1 C23 122.08(17) . 6 ? O1 K1 C23 137.73(11) . 6 ? O1 K1 C23 41.32(10) 6 6 ? N1 K1 C23 96.56(10) 1_655 6 ? C4 K1 C23 72.35(11) 6_655 6 ? C4 K1 C23 101.55(12) 1_655 6 ? O2 K1 C23 81.25(11) 6 . ? O2 K1 C23 17.68(10) . . ? O3 K1 C23 122.08(17) 6 . ? O3 K1 C23 139.74(18) . . ? O1 K1 C23 41.32(10) . . ? O1 K1 C23 137.73(11) 6 . ? N1 K1 C23 96.56(10) 1_655 . ? C4 K1 C23 101.55(12) 6_655 . ? C4 K1 C23 72.35(11) 1_655 . ? C23 K1 C23 98.17(16) 6 . ? O2 K1 Tb1 34.37(7) 6 . ? O2 K1 Tb1 34.37(7) . . ? O3 K1 Tb1 159.07(15) 6 . ? O3 K1 Tb1 159.07(15) . . ? O1 K1 Tb1 86.45(7) . . ? O1 K1 Tb1 86.45(7) 6 . ? N1 K1 Tb1 119.35(11) 1_655 . ? C4 K1 Tb1 103.67(9) 6_655 . ? C4 K1 Tb1 103.67(9) 1_655 . ? C23 K1 Tb1 51.82(8) 6 . ? C23 K1 Tb1 51.82(8) . . ? O2 K1 H3A 133.8 6 . ? O2 K1 H3A 156.6 . . ? O3 K1 H3A 28.7 6 . ? O3 K1 H3A 19.6 . . ? O1 K1 H3A 105.8 . . ? O1 K1 H3A 81.4 6 . ? N1 K1 H3A 60.9 1_655 . ? C4 K1 H3A 71.9 6_655 . ? C4 K1 H3A 80.3 1_655 . ? C23 K1 H3A 116.1 6 . ? C23 K1 H3A 139.7 . . ? Tb1 K1 H3A 167.7 . . ? O2 Tb1 O2 76.04(15) . 6 ? O2 Tb1 N1 141.03(8) . . ? O2 Tb1 N1 141.03(8) 6 . ? O2 Tb1 N3 146.24(12) . 6 ? O2 Tb1 N3 80.92(12) 6 6 ? N1 Tb1 N3 69.21(11) . 6 ? O2 Tb1 N3 80.92(12) . . ? O2 Tb1 N3 146.24(12) 6 . ? N1 Tb1 N3 69.21(11) . . ? N3 Tb1 N3 106.82(18) 6 . ? O2 Tb1 N5 83.85(13) . . ? O2 Tb1 N5 83.85(13) 6 . ? N1 Tb1 N5 107.09(17) . . ? N3 Tb1 N5 69.31(11) 6 . ? N3 Tb1 N5 69.31(11) . . ? O2 Tb1 N6 111.69(12) . 6 ? O2 Tb1 N6 72.77(12) 6 6 ? N1 Tb1 N6 79.55(13) . 6 ? N3 Tb1 N6 83.98(12) 6 6 ? N3 Tb1 N6 139.73(13) . 6 ? N5 Tb1 N6 146.99(9) . 6 ? O2 Tb1 N6 72.77(12) . . ? O2 Tb1 N6 111.69(12) 6 . ? N1 Tb1 N6 79.55(13) . . ? N3 Tb1 N6 139.73(13) 6 . ? N3 Tb1 N6 83.98(12) . . ? N5 Tb1 N6 146.99(9) . . ? N6 Tb1 N6 65.43(17) 6 . ? O2 Tb1 K1 41.03(8) . . ? O2 Tb1 K1 41.03(8) 6 . ? N1 Tb1 K1 172.51(12) . . ? N3 Tb1 K1 106.83(9) 6 . ? N3 Tb1 K1 106.83(9) . . ? N5 Tb1 K1 65.41(13) . . ? N6 Tb1 K1 106.68(9) 6 . ? N6 Tb1 K1 106.68(9) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.983 _refine_diff_density_min -0.744 _refine_diff_density_rms 0.114 _database_code_depnum_ccdc_archive 'CCDC 955770' ####################################################################### # # 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_TbRb _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C55 H38 N10 O5 Rb Tb' _chemical_formula_weight 1163.34 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' Rb Rb -0.9393 2.9676 '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 Orthorhombic _symmetry_space_group_name_H-M Pbcm _symmetry_space_group_name_Hall '-P 2c 2b' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z-1/2' '-x, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 8.4628(5) _cell_length_b 28.0868(9) _cell_length_c 19.0589(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4530.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 2326 _cell_measurement_theta_min 2.8951 _cell_measurement_theta_max 28.0170 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.706 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2320 _exptl_absorpt_coefficient_mu 2.694 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6724 _exptl_absorpt_correction_T_max 0.8133 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(1) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.2141 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 10689 _diffrn_reflns_av_R_equivalents 0.0911 _diffrn_reflns_av_sigmaI/netI 0.1397 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.90 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4110 _reflns_number_gt 2661 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker FRAMBO' _computing_cell_refinement 'Bruker FRAMBO' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0032P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4110 _refine_ls_number_parameters 337 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.1025 _refine_ls_R_factor_gt 0.0543 _refine_ls_wR_factor_ref 0.0906 _refine_ls_wR_factor_gt 0.0788 _refine_ls_goodness_of_fit_ref 0.944 _refine_ls_restrained_S_all 0.962 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.5586(8) -0.0337(3) -0.2133(3) 0.036(2) Uani 1 1 d . . . H1 H -0.6244 -0.0547 -0.1894 0.043 Uiso 1 1 calc R . . C2 C -0.4633(9) -0.0034(3) -0.1761(4) 0.0316(19) Uani 1 1 d . . . H2 H -0.4651 -0.0032 -0.1273 0.038 Uiso 1 1 calc R . . C3 C -0.3656(9) 0.0266(2) -0.2123(3) 0.0283(19) Uani 1 1 d . . . C4 C -0.2461(8) 0.0621(2) -0.1920(3) 0.0225(17) Uani 1 1 d . . . C5 C -0.1273(9) 0.1090(2) -0.1060(3) 0.0248(18) Uani 1 1 d . . . C6 C -0.1188(9) 0.1252(2) -0.0325(3) 0.0248(18) Uani 1 1 d . . . C7 C -0.1959(9) 0.1104(3) 0.0283(3) 0.0304(19) Uani 1 1 d . . . H7 H -0.2677 0.0854 0.0278 0.036 Uiso 1 1 calc R . . C8 C -0.1605(10) 0.1347(3) 0.0895(3) 0.040(2) Uani 1 1 d . . . H8 H -0.2091 0.1255 0.1311 0.048 Uiso 1 1 calc R . . C9 C -0.0548(10) 0.1724(3) 0.0904(3) 0.042(2) Uani 1 1 d . . . H9 H -0.0342 0.1879 0.1325 0.050 Uiso 1 1 calc R . . C10 C 0.0205(10) 0.1873(3) 0.0301(3) 0.035(2) Uani 1 1 d . . . H10 H 0.0920 0.2125 0.0308 0.042 Uiso 1 1 calc R . . C11 C -0.0145(10) 0.1633(3) -0.0318(3) 0.031(2) Uani 1 1 d . . . C12 C 0.0406(9) 0.1701(3) -0.1047(3) 0.0275(19) Uani 1 1 d . . . C13 C 0.1683(9) 0.2144(2) -0.1914(3) 0.0264(18) Uani 1 1 d . . . C14 C 0.2656(9) 0.2558(2) -0.2133(3) 0.0247(18) Uani 1 1 d . . . C15 C 0.3431(9) 0.2915(2) -0.1768(4) 0.0285(19) Uani 1 1 d . . . H15 H 0.3430 0.2916 -0.1280 0.034 Uiso 1 1 calc R . . C16 C 0.4194(10) 0.3264(2) -0.2132(3) 0.033(2) Uani 1 1 d . . . H16 H 0.4719 0.3504 -0.1890 0.040 Uiso 1 1 calc R . . C17 C 0.5467(11) 0.2036(3) -0.0597(4) 0.052(3) Uani 1 1 d . . . H17A H 0.5995 0.2255 -0.0904 0.078 Uiso 1 1 calc R . . H17B H 0.6196 0.1924 -0.0248 0.078 Uiso 1 1 calc R . . H17C H 0.4597 0.2193 -0.0372 0.078 Uiso 1 1 calc R . . C18 C 0.4091(10) 0.1288(3) -0.0634(3) 0.0325(19) Uani 1 1 d . . . C19 C 0.4138(9) 0.1237(3) 0.0076(3) 0.031(2) Uani 1 1 d . . . H19 H 0.4671 0.1457 0.0353 0.038 Uiso 1 1 calc R . . C20 C 0.3376(10) 0.0851(3) 0.0379(3) 0.035(2) Uani 1 1 d . . . H20 H 0.3414 0.0812 0.0863 0.042 Uiso 1 1 calc R . . C21 C 0.2564(10) 0.0522(3) -0.0020(3) 0.034(2) Uani 1 1 d . . . H21 H 0.2103 0.0258 0.0191 0.041 Uiso 1 1 calc R . . C22 C 0.2439(9) 0.0591(2) -0.0754(3) 0.0282(19) Uani 1 1 d . . . C23 C 0.3186(8) 0.0986(2) -0.1077(3) 0.0226(17) Uani 1 1 d . . . C24 C 0.1594(9) 0.0240(3) -0.1150(3) 0.0292(19) Uani 1 1 d . . . H24 H 0.1384 -0.0046 -0.0922 0.035 Uiso 1 1 calc R . . C25 C 0.0337(8) -0.0121(2) -0.2134(3) 0.0231(17) Uani 1 1 d . . . C26 C -0.0409(9) -0.0488(2) -0.1778(4) 0.033(2) Uani 1 1 d . . . H26 H -0.0428 -0.0486 -0.1291 0.039 Uiso 1 1 calc R . . C27 C -0.1122(10) -0.0857(2) -0.2136(3) 0.034(2) Uani 1 1 d . . . H27 H -0.1601 -0.1104 -0.1891 0.041 Uiso 1 1 calc R . . C28 C 0.809(2) 0.2622(5) -0.2500 0.115(6) Uani 1 2 d SDU . . H28A H 0.8035 0.2567 -0.2003 0.172 Uiso 0.50 1 d PR . . H28B H 0.7298 0.2851 -0.2632 0.172 Uiso 0.50 1 d PR . . H28C H 0.9115 0.2743 -0.2620 0.172 Uiso 0.50 1 d PR . . N1 N -0.1758(10) 0.0816(3) -0.2500 0.025(2) Uani 1 2 d S . . N2 N -0.2238(7) 0.0735(2) -0.1246(3) 0.0271(15) Uani 1 1 d . . . N3 N -0.0287(7) 0.13568(19) -0.1464(2) 0.0256(15) Uani 1 1 d . . . N4 N 0.1336(7) 0.20550(19) -0.1241(3) 0.0244(15) Uani 1 1 d . . . N5 N 0.1214(11) 0.1901(3) -0.2500 0.025(2) Uani 1 2 d S . . N6 N 0.1081(7) 0.02751(18) -0.1799(2) 0.0200(13) Uani 1 1 d . . . O1 O 0.4892(6) 0.16408(17) -0.0994(2) 0.0334(14) Uani 1 1 d . . . O2 O 0.3113(5) 0.10750(15) -0.17568(19) 0.0240(11) Uani 1 1 d . . . O3 O 0.7824(13) 0.2216(4) -0.2825(4) 0.058(4) Uani 0.50 1 d PDU . . H3A H 0.7738 0.1964 -0.2500 0.088 Uiso 1 2 d SRD . . Rb1 Rb 0.54036(14) 0.15652(4) -0.2500 0.0388(3) Uani 1 2 d S . . Tb1 Tb 0.10427(7) 0.102611(17) -0.2500 0.02311(15) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.014(5) 0.025(5) 0.069(5) 0.008(4) 0.005(4) 0.003(4) C2 0.021(5) 0.030(5) 0.044(4) -0.004(4) -0.001(4) 0.006(4) C3 0.023(5) 0.018(4) 0.044(4) -0.004(3) -0.002(3) 0.004(4) C4 0.024(4) 0.013(4) 0.031(4) 0.001(4) 0.002(3) 0.004(4) C5 0.032(5) 0.018(4) 0.024(4) 0.003(4) 0.004(3) 0.007(4) C6 0.026(5) 0.023(4) 0.026(4) 0.004(3) 0.004(3) 0.002(4) C7 0.029(5) 0.026(5) 0.036(4) -0.001(4) 0.006(4) 0.008(4) C8 0.049(6) 0.049(6) 0.022(4) 0.004(4) 0.007(4) 0.000(5) C9 0.053(6) 0.051(6) 0.021(4) -0.006(4) 0.007(4) -0.002(5) C10 0.044(6) 0.026(5) 0.034(4) -0.004(4) -0.001(4) -0.001(4) C11 0.044(6) 0.031(5) 0.019(4) -0.004(4) 0.006(4) 0.008(5) C12 0.035(5) 0.018(4) 0.029(4) -0.003(4) 0.003(4) 0.013(4) C13 0.035(5) 0.016(4) 0.028(4) -0.002(4) 0.001(4) 0.007(4) C14 0.031(5) 0.015(4) 0.028(4) -0.001(3) 0.006(3) 0.002(4) C15 0.035(5) 0.020(4) 0.030(4) -0.006(4) -0.001(4) 0.008(4) C16 0.048(6) 0.014(4) 0.037(4) -0.002(3) -0.003(4) -0.003(4) C17 0.078(8) 0.026(5) 0.052(5) -0.009(4) -0.022(5) -0.003(5) C18 0.043(5) 0.025(4) 0.030(4) -0.003(4) -0.001(4) 0.005(5) C19 0.031(5) 0.037(5) 0.026(4) -0.013(4) -0.004(4) 0.010(4) C20 0.049(6) 0.039(5) 0.017(4) -0.001(4) -0.004(4) 0.013(5) C21 0.051(6) 0.033(5) 0.018(4) 0.001(4) 0.005(4) 0.006(5) C22 0.042(5) 0.019(4) 0.024(4) 0.001(3) -0.002(4) 0.004(4) C23 0.023(4) 0.022(4) 0.024(4) -0.003(4) 0.001(3) 0.010(4) C24 0.033(5) 0.025(5) 0.030(4) 0.005(4) 0.010(4) 0.011(4) C25 0.013(4) 0.015(4) 0.042(4) -0.008(3) 0.009(3) 0.004(4) C26 0.043(5) 0.020(4) 0.036(4) 0.000(4) 0.006(4) -0.001(4) C27 0.041(5) 0.022(4) 0.039(4) 0.003(3) 0.007(4) 0.004(5) C28 0.113(8) 0.110(8) 0.121(7) 0.000 0.000 -0.001(5) N1 0.032(6) 0.016(5) 0.028(4) 0.000 0.000 0.003(5) N2 0.029(4) 0.025(4) 0.027(3) 0.002(3) 0.003(3) 0.003(3) N3 0.039(4) 0.014(3) 0.024(3) 0.002(3) 0.010(3) 0.004(3) N4 0.035(4) 0.019(3) 0.019(3) -0.008(3) 0.007(3) 0.004(3) N5 0.049(6) 0.019(5) 0.007(4) 0.000 0.000 0.000(5) N6 0.021(3) 0.024(3) 0.015(3) -0.003(3) 0.000(3) 0.007(3) O1 0.041(4) 0.024(3) 0.035(3) -0.007(3) -0.010(3) -0.003(3) O2 0.030(3) 0.022(3) 0.020(2) -0.001(2) -0.001(2) 0.002(3) O3 0.056(5) 0.054(5) 0.065(5) -0.001(4) 0.006(4) -0.004(4) Rb1 0.0409(8) 0.0362(7) 0.0392(6) 0.000 0.000 -0.0048(6) Tb1 0.0313(3) 0.0161(3) 0.0219(3) 0.000 0.000 0.0002(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.371(9) . ? C1 C1 1.398(12) 6 ? C1 H1 0.9300 . ? C2 C3 1.368(9) . ? C2 H2 0.9300 . ? C3 C3 1.435(12) 6 ? C3 C4 1.473(9) . ? C4 N2 1.336(7) . ? C4 N1 1.369(8) . ? C4 Rb1 3.394(6) 1_455 ? C5 N2 1.337(8) . ? C5 N3 1.361(8) . ? C5 C6 1.476(8) . ? C6 C11 1.388(9) . ? C6 C7 1.394(8) . ? C7 C8 1.384(9) . ? C7 H7 0.9300 . ? C8 C9 1.386(10) . ? C8 H8 0.9300 . ? C9 C10 1.380(9) . ? C9 H9 0.9300 . ? C10 C11 1.390(8) . ? C10 H10 0.9300 . ? C11 C12 1.477(9) . ? C12 N4 1.321(8) . ? C12 N3 1.382(8) . ? C13 N4 1.340(7) . ? C13 N5 1.368(8) . ? C13 C14 1.483(9) . ? C13 Rb1 3.715(7) . ? C14 C15 1.385(9) . ? C14 C14 1.399(11) 6 ? C14 Rb1 3.697(7) . ? C15 C16 1.365(9) . ? C15 H15 0.9300 . ? C16 C16 1.404(11) 6 ? C16 H16 0.9300 . ? C17 O1 1.428(7) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C19 1.361(8) . ? C18 O1 1.382(8) . ? C18 C23 1.422(9) . ? C19 C20 1.388(9) . ? C19 H19 0.9300 . ? C20 C21 1.378(9) . ? C20 H20 0.9300 . ? C21 C22 1.416(8) . ? C21 H21 0.9300 . ? C22 C23 1.418(9) . ? C22 C24 1.433(9) . ? C23 O2 1.320(6) . ? C23 Rb1 3.677(7) . ? C24 N6 1.315(7) . ? C24 H24 0.9300 . ? C25 C26 1.387(8) . ? C25 C25 1.397(11) 6 ? C25 N6 1.427(7) . ? C26 C27 1.378(9) . ? C26 H26 0.9300 . ? C27 C27 1.387(11) 6 ? C27 H27 0.9300 . ? C28 O3 1.317(11) . ? C28 Rb1 3.739(16) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? N1 C4 1.369(8) 6 ? N1 Tb1 2.442(9) . ? N1 Rb1 3.194(8) 1_455 ? N3 Tb1 2.454(5) . ? N5 C13 1.368(8) 6 ? N5 Tb1 2.462(7) . ? N5 Rb1 3.669(9) . ? N6 Tb1 2.497(5) . ? O1 Rb1 2.910(4) . ? O2 Tb1 2.257(4) . ? O2 Rb1 2.768(4) . ? O3 O3 1.238(17) 6 ? O3 Rb1 2.815(11) . ? O3 H3A 0.9432 . ? Rb1 O2 2.768(4) 6 ? Rb1 O3 2.815(11) 6 ? Rb1 O1 2.910(4) 6 ? Rb1 N1 3.194(8) 1_655 ? Rb1 C4 3.394(6) 6_655 ? Rb1 C4 3.394(6) 1_655 ? Rb1 C23 3.677(7) 6 ? Rb1 H3A 2.2714 . ? Tb1 O2 2.257(4) 6 ? Tb1 N3 2.454(5) 6 ? Tb1 N6 2.497(5) 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 C2 C1 C1 121.2(4) . 6 ? C2 C1 H1 119.4 . . ? C1 C1 H1 119.4 6 . ? C3 C2 C1 118.4(7) . . ? C3 C2 H2 120.8 . . ? C1 C2 H2 120.8 . . ? C2 C3 C3 120.4(4) . 6 ? C2 C3 C4 134.4(6) . . ? C3 C3 C4 105.3(4) 6 . ? N2 C4 N1 128.2(6) . . ? N2 C4 C3 120.8(6) . . ? N1 C4 C3 110.9(6) . . ? N2 C4 Rb1 101.6(4) . 1_455 ? N1 C4 Rb1 69.9(4) . 1_455 ? C3 C4 Rb1 94.5(4) . 1_455 ? N2 C5 N3 129.5(6) . . ? N2 C5 C6 120.9(6) . . ? N3 C5 C6 109.7(6) . . ? C11 C6 C7 121.4(6) . . ? C11 C6 C5 106.2(6) . . ? C7 C6 C5 132.4(7) . . ? C8 C7 C6 116.8(7) . . ? C8 C7 H7 121.6 . . ? C6 C7 H7 121.6 . . ? C7 C8 C9 121.8(7) . . ? C7 C8 H8 119.1 . . ? C9 C8 H8 119.1 . . ? C10 C9 C8 121.3(7) . . ? C10 C9 H9 119.4 . . ? C8 C9 H9 119.4 . . ? C9 C10 C11 117.5(7) . . ? C9 C10 H10 121.3 . . ? C11 C10 H10 121.3 . . ? C6 C11 C10 121.2(6) . . ? C6 C11 C12 106.9(6) . . ? C10 C11 C12 131.9(7) . . ? N4 C12 N3 128.1(6) . . ? N4 C12 C11 123.2(6) . . ? N3 C12 C11 108.6(6) . . ? N4 C13 N5 128.7(7) . . ? N4 C13 C14 122.5(6) . . ? N5 C13 C14 108.8(6) . . ? N4 C13 Rb1 113.1(4) . . ? N5 C13 Rb1 77.4(5) . . ? C14 C13 Rb1 77.7(4) . . ? C15 C14 C14 120.1(4) . 6 ? C15 C14 C13 133.5(6) . . ? C14 C14 C13 106.4(3) 6 . ? C15 C14 Rb1 110.1(5) . . ? C14 C14 Rb1 79.09(9) 6 . ? C13 C14 Rb1 79.2(4) . . ? C16 C15 C14 119.4(6) . . ? C16 C15 H15 120.3 . . ? C14 C15 H15 120.3 . . ? C15 C16 C16 120.5(4) . 6 ? C15 C16 H16 119.7 . . ? C16 C16 H16 119.7 6 . ? O1 C17 H17A 109.5 . . ? O1 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? O1 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 O1 123.7(7) . . ? C19 C18 C23 122.9(7) . . ? O1 C18 C23 113.4(6) . . ? C18 C19 C20 118.9(7) . . ? C18 C19 H19 120.6 . . ? C20 C19 H19 120.6 . . ? C21 C20 C19 121.7(6) . . ? C21 C20 H20 119.2 . . ? C19 C20 H20 119.2 . . ? C20 C21 C22 119.5(7) . . ? C20 C21 H21 120.3 . . ? C22 C21 H21 120.3 . . ? C21 C22 C23 120.1(7) . . ? C21 C22 C24 117.7(7) . . ? C23 C22 C24 122.1(6) . . ? O2 C23 C22 123.6(6) . . ? O2 C23 C18 119.7(6) . . ? C22 C23 C18 116.7(6) . . ? O2 C23 Rb1 38.5(3) . . ? C22 C23 Rb1 153.4(4) . . ? C18 C23 Rb1 84.2(4) . . ? N6 C24 C22 127.5(6) . . ? N6 C24 H24 116.3 . . ? C22 C24 H24 116.3 . . ? C26 C25 C25 119.2(4) . 6 ? C26 C25 N6 124.3(6) . . ? C25 C25 N6 116.5(3) 6 . ? C27 C26 C25 121.1(6) . . ? C27 C26 H26 119.4 . . ? C25 C26 H26 119.4 . . ? C26 C27 C27 119.6(4) . 6 ? C26 C27 H27 120.2 . . ? C27 C27 H27 120.2 6 . ? O3 C28 Rb1 37.7(7) . . ? O3 C28 H28A 108.4 . . ? Rb1 C28 H28A 81.0 . . ? O3 C28 H28B 109.8 . . ? Rb1 C28 H28B 96.2 . . ? H28A C28 H28B 109.5 . . ? O3 C28 H28C 110.2 . . ? Rb1 C28 H28C 146.0 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C4 N1 C4 107.6(8) 6 . ? C4 N1 Tb1 121.2(4) 6 . ? C4 N1 Tb1 121.2(4) . . ? C4 N1 Rb1 86.3(4) 6 1_455 ? C4 N1 Rb1 86.3(4) . 1_455 ? Tb1 N1 Rb1 124.8(3) . 1_455 ? C4 N2 C5 121.3(6) . . ? C5 N3 C12 108.6(5) . . ? C5 N3 Tb1 121.9(4) . . ? C12 N3 Tb1 122.2(5) . . ? C12 N4 C13 122.6(6) . . ? C13 N5 C13 109.5(8) 6 . ? C13 N5 Tb1 121.0(4) 6 . ? C13 N5 Tb1 121.0(4) . . ? C13 N5 Rb1 81.2(5) 6 . ? C13 N5 Rb1 81.2(5) . . ? Tb1 N5 Rb1 78.5(2) . . ? C24 N6 C25 120.4(5) . . ? C24 N6 Tb1 124.8(5) . . ? C25 N6 Tb1 114.4(4) . . ? C18 O1 C17 117.4(5) . . ? C18 O1 Rb1 120.7(4) . . ? C17 O1 Rb1 121.9(4) . . ? C23 O2 Tb1 129.8(4) . . ? C23 O2 Rb1 124.3(4) . . ? Tb1 O2 Rb1 104.64(14) . . ? O3 O3 C28 62.0(4) 6 . ? O3 O3 Rb1 77.29(18) 6 . ? C28 O3 Rb1 125.6(9) . . ? O3 O3 H3A 49.0 6 . ? C28 O3 H3A 110.8 . . ? Rb1 O3 H3A 46.5 . . ? O2 Rb1 O2 61.57(16) 6 . ? O2 Rb1 O3 161.0(2) 6 6 ? O2 Rb1 O3 136.1(2) . 6 ? O2 Rb1 O3 136.1(2) 6 . ? O2 Rb1 O3 161.0(2) . . ? O3 Rb1 O3 25.4(4) 6 . ? O2 Rb1 O1 55.06(13) 6 6 ? O2 Rb1 O1 115.90(13) . 6 ? O3 Rb1 O1 106.1(2) 6 6 ? O3 Rb1 O1 81.0(2) . 6 ? O2 Rb1 O1 115.90(13) 6 . ? O2 Rb1 O1 55.06(13) . . ? O3 Rb1 O1 81.0(2) 6 . ? O3 Rb1 O1 106.1(2) . . ? O1 Rb1 O1 160.9(2) 6 . ? O2 Rb1 N1 101.48(16) 6 1_655 ? O2 Rb1 N1 101.48(16) . 1_655 ? O3 Rb1 N1 83.1(3) 6 1_655 ? O3 Rb1 N1 83.1(3) . 1_655 ? O1 Rb1 N1 99.21(10) 6 1_655 ? O1 Rb1 N1 99.21(10) . 1_655 ? O2 Rb1 C4 79.49(15) 6 6_655 ? O2 Rb1 C4 98.68(15) . 6_655 ? O3 Rb1 C4 101.0(3) 6 6_655 ? O3 Rb1 C4 92.8(3) . 6_655 ? O1 Rb1 C4 79.34(14) 6 6_655 ? O1 Rb1 C4 117.22(15) . 6_655 ? N1 Rb1 C4 23.74(13) 1_655 6_655 ? O2 Rb1 C4 98.68(15) 6 1_655 ? O2 Rb1 C4 79.49(15) . 1_655 ? O3 Rb1 C4 92.8(3) 6 1_655 ? O3 Rb1 C4 101.0(3) . 1_655 ? O1 Rb1 C4 117.22(15) 6 1_655 ? O1 Rb1 C4 79.35(14) . 1_655 ? N1 Rb1 C4 23.74(13) 1_655 1_655 ? C4 Rb1 C4 38.0(2) 6_655 1_655 ? O2 Rb1 N5 56.71(13) 6 . ? O2 Rb1 N5 56.71(13) . . ? O3 Rb1 N5 122.4(3) 6 . ? O3 Rb1 N5 122.4(3) . . ? O1 Rb1 N5 80.64(10) 6 . ? O1 Rb1 N5 80.64(10) . . ? N1 Rb1 N5 153.69(19) 1_655 . ? C4 Rb1 N5 135.69(16) 6_655 . ? C4 Rb1 N5 135.69(16) 1_655 . ? O2 Rb1 C23 17.25(13) 6 6 ? O2 Rb1 C23 78.45(14) . 6 ? O3 Rb1 C23 145.2(2) 6 6 ? O3 Rb1 C23 119.8(2) . 6 ? O1 Rb1 C23 39.57(14) 6 6 ? O1 Rb1 C23 133.11(15) . 6 ? N1 Rb1 C23 95.30(15) 1_655 6 ? C4 Rb1 C23 71.70(16) 6_655 6 ? C4 Rb1 C23 99.57(15) 1_655 6 ? N5 Rb1 C23 67.70(13) . 6 ? O2 Rb1 C23 78.45(14) 6 . ? O2 Rb1 C23 17.25(13) . . ? O3 Rb1 C23 119.8(2) 6 . ? O3 Rb1 C23 145.2(2) . . ? O1 Rb1 C23 133.11(15) 6 . ? O1 Rb1 C23 39.57(14) . . ? N1 Rb1 C23 95.30(15) 1_655 . ? C4 Rb1 C23 99.57(15) 6_655 . ? C4 Rb1 C23 71.70(16) 1_655 . ? N5 Rb1 C23 67.70(13) . . ? C23 Rb1 C23 95.0(2) 6 . ? O2 Rb1 H3A 148.7 6 . ? O2 Rb1 H3A 148.7 . . ? O3 Rb1 H3A 17.5 6 . ? O3 Rb1 H3A 17.5 . . ? O1 Rb1 H3A 95.4 6 . ? O1 Rb1 H3A 95.4 . . ? N1 Rb1 H3A 70.8 1_655 . ? C4 Rb1 H3A 85.5 6_655 . ? C4 Rb1 H3A 85.5 1_655 . ? N5 Rb1 H3A 135.5 . . ? C23 Rb1 H3A 131.5 6 . ? C23 Rb1 H3A 131.5 . . ? O2 Tb1 O2 77.7(2) . 6 ? O2 Tb1 N1 140.16(11) . . ? O2 Tb1 N1 140.16(11) 6 . ? O2 Tb1 N3 146.87(18) . 6 ? O2 Tb1 N3 80.10(17) 6 6 ? N1 Tb1 N3 69.31(17) . 6 ? O2 Tb1 N3 80.10(17) . . ? O2 Tb1 N3 146.87(18) 6 . ? N1 Tb1 N3 69.31(17) . . ? N3 Tb1 N3 107.1(3) 6 . ? O2 Tb1 N5 83.89(19) . . ? O2 Tb1 N5 83.89(19) 6 . ? N1 Tb1 N5 107.4(3) . . ? N3 Tb1 N5 69.47(17) 6 . ? N3 Tb1 N5 69.47(17) . . ? O2 Tb1 N6 112.14(16) . 6 ? O2 Tb1 N6 72.88(17) 6 6 ? N1 Tb1 N6 79.0(2) . 6 ? N3 Tb1 N6 84.01(17) 6 6 ? N3 Tb1 N6 139.09(18) . 6 ? N5 Tb1 N6 147.42(11) . 6 ? O2 Tb1 N6 72.88(17) . . ? O2 Tb1 N6 112.14(16) 6 . ? N1 Tb1 N6 79.0(2) . . ? N3 Tb1 N6 139.09(18) 6 . ? N3 Tb1 N6 84.01(17) . . ? N5 Tb1 N6 147.42(11) . . ? N6 Tb1 N6 64.7(2) 6 . ? O2 Tb1 Rb1 42.17(11) . . ? O2 Tb1 Rb1 42.17(11) 6 . ? N1 Tb1 Rb1 171.68(17) . . ? N3 Tb1 Rb1 106.28(14) 6 . ? N3 Tb1 Rb1 106.28(14) . . ? N5 Tb1 Rb1 64.3(2) . . ? N6 Tb1 Rb1 107.98(13) 6 . ? N6 Tb1 Rb1 107.98(13) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.779 _refine_diff_density_min -1.298 _refine_diff_density_rms 0.148 _database_code_depnum_ccdc_archive 'CCDC 955771' ####################################################################### # # 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_TbCs _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C55 H34 Cs N10 O5 Tb' _chemical_formula_weight 1206.75 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' Cs Cs -0.3680 2.1192 '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 Orthorhombic _symmetry_space_group_name_H-M Pbcm _symmetry_space_group_name_Hall '-P 2c 2b' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z-1/2' '-x, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 8.0865(2) _cell_length_b 28.9520(12) _cell_length_c 19.3040(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4519.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 149.95(10) _cell_measurement_reflns_used 4030 _cell_measurement_theta_min 2.9788 _cell_measurement_theta_max 28.3694 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.774 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2376 _exptl_absorpt_coefficient_mu 2.424 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6977 _exptl_absorpt_correction_T_max 0.7936 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 149.95(10) _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, Eos, Gemini' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.2141 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 12898 _diffrn_reflns_av_R_equivalents 0.0380 _diffrn_reflns_av_sigmaI/netI 0.0430 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4099 _reflns_number_gt 3283 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker FRAMBO' _computing_cell_refinement 'Bruker FRAMBO' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0557P)^2^+19.1313P] 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 4099 _refine_ls_number_parameters 338 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0588 _refine_ls_R_factor_gt 0.0417 _refine_ls_wR_factor_ref 0.1154 _refine_ls_wR_factor_gt 0.1086 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.5512(8) -0.0402(2) -0.2141(4) 0.0412(18) Uani 1 1 d . . . H1 H -0.6155 -0.0618 -0.1907 0.049 Uiso 1 1 calc R . . C2 C -0.4583(7) -0.0091(2) -0.1765(4) 0.0335(16) Uani 1 1 d . . . H2 H -0.4594 -0.0091 -0.1283 0.040 Uiso 1 1 calc R . . C3 C -0.3634(7) 0.0222(2) -0.2136(3) 0.0294(14) Uani 1 1 d . . . C4 C -0.2484(7) 0.0588(2) -0.1923(3) 0.0273(14) Uani 1 1 d . . . C5 C -0.1326(7) 0.1064(2) -0.1069(3) 0.0261(13) Uani 1 1 d . . . C6 C -0.1259(7) 0.1225(2) -0.0354(3) 0.0273(13) Uani 1 1 d . . . C7 C -0.1993(8) 0.1068(2) 0.0252(3) 0.0325(15) Uani 1 1 d . . . H7 H -0.2662 0.0807 0.0254 0.039 Uiso 1 1 calc R . . C8 C -0.1696(8) 0.1313(2) 0.0851(3) 0.0388(17) Uani 1 1 d . . . H8 H -0.2189 0.1215 0.1261 0.047 Uiso 1 1 calc R . . C9 C -0.0670(8) 0.1707(3) 0.0866(4) 0.0401(17) Uani 1 1 d . . . H9 H -0.0483 0.1863 0.1280 0.048 Uiso 1 1 calc R . . C10 C 0.0062(8) 0.1861(2) 0.0252(3) 0.0318(15) Uani 1 1 d . . . H10 H 0.0736 0.2122 0.0250 0.038 Uiso 1 1 calc R . . C11 C -0.0238(7) 0.1617(2) -0.0352(3) 0.0268(14) Uani 1 1 d . . . C12 C 0.0296(7) 0.1687(2) -0.1069(3) 0.0230(13) Uani 1 1 d . . . C13 C 0.1578(7) 0.21337(19) -0.1925(3) 0.0230(13) Uani 1 1 d . . . C14 C 0.2469(7) 0.2547(2) -0.2137(3) 0.0236(13) Uani 1 1 d . . . C15 C 0.3193(7) 0.2912(2) -0.1763(3) 0.0266(13) Uani 1 1 d . . . H15 H 0.3178 0.2917 -0.1282 0.032 Uiso 1 1 calc R . . C16 C 0.3924(8) 0.3261(2) -0.2135(3) 0.0345(15) Uani 1 1 d . . . H16 H 0.4430 0.3503 -0.1900 0.041 Uiso 1 1 calc R . . C17 C 0.5442(10) 0.2071(2) -0.0574(4) 0.0469(19) Uani 1 1 d . . . H17A H 0.5968 0.2294 -0.0869 0.070 Uiso 1 1 calc R . . H17B H 0.6203 0.1974 -0.0222 0.070 Uiso 1 1 calc R . . H17C H 0.4486 0.2207 -0.0362 0.070 Uiso 1 1 calc R . . C18 C 0.4151(7) 0.1330(2) -0.0628(3) 0.0277(14) Uani 1 1 d . . . C19 C 0.4098(8) 0.1275(2) 0.0069(3) 0.0349(16) Uani 1 1 d . . . H19 H 0.4580 0.1498 0.0352 0.042 Uiso 1 1 calc R . . C20 C 0.3337(8) 0.0893(2) 0.0371(3) 0.0359(16) Uani 1 1 d . . . H20 H 0.3315 0.0859 0.0850 0.043 Uiso 1 1 calc R . . C21 C 0.2625(8) 0.0570(2) -0.0048(3) 0.0327(15) Uani 1 1 d . . . H21 H 0.2176 0.0304 0.0148 0.039 Uiso 1 1 calc R . . C22 C 0.2557(7) 0.0631(2) -0.0772(3) 0.0259(13) Uani 1 1 d . . . C23 C 0.3313(7) 0.1019(2) -0.1082(3) 0.0238(12) Uani 1 1 d . . . C24 C 0.1769(7) 0.0273(2) -0.1176(3) 0.0250(13) Uani 1 1 d . . . H24 H 0.1630 -0.0012 -0.0961 0.030 Uiso 1 1 calc R . . C25 C 0.0514(7) -0.0086(2) -0.2136(3) 0.0223(13) Uani 1 1 d . . . C26 C -0.0213(7) -0.0451(2) -0.1789(3) 0.0272(14) Uani 1 1 d . . . H26 H -0.0250 -0.0447 -0.1307 0.033 Uiso 1 1 calc R . . C27 C -0.0888(8) -0.0821(2) -0.2145(3) 0.0338(15) Uani 1 1 d . . . H27 H -0.1339 -0.1069 -0.1903 0.041 Uiso 1 1 calc R . . N1 N -0.1765(8) 0.0783(2) -0.2500 0.0226(15) Uani 1 2 d S . . N2 N -0.2260(6) 0.07077(16) -0.1263(3) 0.0258(11) Uani 1 1 d . . . N3 N -0.0363(6) 0.13401(16) -0.1483(2) 0.0235(11) Uani 1 1 d . . . N4 N 0.1209(6) 0.20422(16) -0.1267(2) 0.0232(11) Uani 1 1 d . . . N5 N 0.1150(8) 0.1891(2) -0.2500 0.0208(14) Uani 1 2 d S . . N6 N 0.1237(6) 0.03079(16) -0.1806(2) 0.0210(10) Uani 1 1 d . . . O1 O 0.4952(6) 0.16825(15) -0.0975(2) 0.0329(10) Uani 1 1 d . . . O2 O 0.3272(5) 0.11036(13) -0.1751(2) 0.0244(9) Uani 1 1 d . . . Cs1 Cs 0.58353(8) 0.16591(2) -0.2500 0.0425(2) Uani 1 2 d S . . Tb1 Tb 0.11217(5) 0.103690(13) -0.2500 0.01996(14) Uani 1 2 d S . . O3 O 0.759(2) 0.2502(6) -0.1927(8) 0.126(6) Uani 0.50 1 d PDU . . C28 C 0.803(2) 0.2788(5) -0.2500 0.086(4) Uani 1 2 d SDU . . 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 0.021(3) 0.026(4) 0.076(5) 0.006(3) 0.008(3) -0.002(3) C2 0.019(3) 0.025(4) 0.056(4) 0.004(3) 0.008(3) 0.005(3) C3 0.019(3) 0.028(3) 0.042(4) -0.002(3) 0.004(3) 0.008(3) C4 0.023(3) 0.020(3) 0.038(4) 0.002(3) -0.001(3) 0.010(3) C5 0.022(3) 0.025(3) 0.031(3) -0.001(3) 0.002(3) 0.009(3) C6 0.024(3) 0.029(3) 0.029(3) 0.001(3) 0.006(3) 0.009(3) C7 0.026(3) 0.035(4) 0.037(4) 0.007(3) 0.004(3) 0.004(3) C8 0.038(4) 0.052(5) 0.026(4) 0.012(3) 0.006(3) 0.003(4) C9 0.041(4) 0.053(5) 0.027(4) 0.002(3) 0.002(3) -0.002(3) C10 0.035(3) 0.038(4) 0.022(3) 0.000(3) 0.000(3) -0.003(3) C11 0.025(3) 0.028(3) 0.027(3) 0.003(3) 0.002(3) 0.007(3) C12 0.022(3) 0.023(3) 0.024(3) 0.000(2) 0.002(2) 0.007(3) C13 0.027(3) 0.015(3) 0.027(3) -0.003(2) -0.001(3) 0.001(3) C14 0.025(3) 0.021(3) 0.024(3) 0.005(2) 0.002(2) 0.008(3) C15 0.030(3) 0.022(3) 0.027(3) -0.003(2) 0.000(3) 0.005(3) C16 0.041(4) 0.023(3) 0.039(4) -0.007(3) 0.002(3) -0.008(3) C17 0.063(5) 0.029(4) 0.048(5) -0.013(3) -0.011(4) -0.002(4) C18 0.025(3) 0.029(3) 0.030(3) -0.006(3) -0.002(3) 0.006(3) C19 0.036(4) 0.038(4) 0.030(4) -0.013(3) -0.008(3) 0.010(3) C20 0.036(4) 0.052(4) 0.020(3) -0.005(3) -0.004(3) 0.011(3) C21 0.035(3) 0.042(4) 0.021(3) 0.005(3) 0.002(3) 0.009(3) C22 0.027(3) 0.029(3) 0.022(3) -0.001(2) 0.001(3) 0.007(3) C23 0.025(3) 0.024(3) 0.023(3) -0.003(2) -0.001(2) 0.009(3) C24 0.028(3) 0.025(3) 0.022(3) 0.005(2) 0.005(3) 0.004(3) C25 0.018(3) 0.019(3) 0.029(3) 0.001(2) 0.002(2) 0.003(2) C26 0.032(3) 0.027(3) 0.023(3) 0.006(3) 0.003(3) 0.006(3) C27 0.037(4) 0.022(3) 0.042(4) 0.007(3) 0.001(3) -0.005(3) N1 0.021(3) 0.018(4) 0.029(4) 0.000 0.000 0.000(3) N2 0.021(2) 0.022(3) 0.035(3) 0.003(2) 0.004(2) 0.004(2) N3 0.027(3) 0.019(3) 0.024(3) 0.001(2) 0.007(2) 0.001(2) N4 0.028(3) 0.018(2) 0.023(3) -0.001(2) 0.002(2) 0.002(2) N5 0.031(4) 0.015(3) 0.015(3) 0.000 0.000 -0.004(3) N6 0.022(2) 0.019(2) 0.022(3) -0.0011(19) 0.002(2) 0.004(2) O1 0.038(2) 0.031(2) 0.030(2) -0.0115(19) -0.006(2) -0.001(2) O2 0.029(2) 0.024(2) 0.020(2) -0.0021(16) -0.0037(18) 0.0004(18) Cs1 0.0457(4) 0.0352(4) 0.0466(4) 0.000 0.000 0.0016(3) Tb1 0.0231(2) 0.0174(2) 0.0193(2) 0.000 0.000 0.00218(17) O3 0.127(7) 0.126(7) 0.126(7) 0.002(5) 0.004(5) -0.009(5) C28 0.083(6) 0.089(6) 0.085(6) 0.000 0.000 -0.003(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.380(9) . ? C1 C1 1.385(15) 6 ? C1 H1 0.9300 . ? C2 C3 1.386(9) . ? C2 H2 0.9300 . ? C3 C3 1.407(13) 6 ? C3 C4 1.468(9) . ? C4 N2 1.334(8) . ? C4 N1 1.377(7) . ? C4 Cs1 3.564(6) 1_455 ? C5 N2 1.333(8) . ? C5 N3 1.372(8) . ? C5 C6 1.459(9) . ? C6 C7 1.388(8) . ? C6 C11 1.402(9) . ? C7 C8 1.378(9) . ? C7 H7 0.9300 . ? C8 C9 1.410(10) . ? C8 H8 0.9300 . ? C9 C10 1.397(9) . ? C9 H9 0.9300 . ? C10 C11 1.386(8) . ? C10 H10 0.9300 . ? C11 C12 1.464(8) . ? C12 N4 1.323(8) . ? C12 N3 1.389(8) . ? C13 N4 1.332(8) . ? C13 N5 1.357(7) . ? C13 C14 1.454(8) . ? C14 C14 1.400(11) 6 ? C14 C15 1.409(8) . ? C15 C16 1.373(9) . ? C15 H15 0.9300 . ? C16 C16 1.408(13) 6 ? C16 H16 0.9300 . ? C17 O1 1.421(7) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C19 1.357(9) . ? C18 O1 1.381(8) . ? C18 C23 1.427(8) . ? C19 C20 1.395(10) . ? C19 H19 0.9300 . ? C20 C21 1.364(9) . ? C20 H20 0.9300 . ? C21 C22 1.410(8) . ? C21 H21 0.9300 . ? C22 C23 1.413(8) . ? C22 C24 1.445(8) . ? C23 O2 1.314(7) . ? C24 N6 1.294(7) . ? C24 H24 0.9300 . ? C25 C26 1.382(8) . ? C25 C25 1.404(12) 6 ? C25 N6 1.432(7) . ? C26 C27 1.386(9) . ? C26 H26 0.9300 . ? C27 C27 1.371(13) 6 ? C27 H27 0.9300 . ? N1 C4 1.377(7) 6 ? N1 Tb1 2.447(7) . ? N1 Cs1 3.194(7) 1_455 ? N3 Tb1 2.463(5) . ? N3 Cs1 3.763(5) 1_455 ? N5 C13 1.357(7) 6 ? N5 Tb1 2.474(6) . ? N5 Cs1 3.848(7) . ? N6 Tb1 2.502(5) . ? O1 Cs1 3.030(4) . ? O2 Tb1 2.270(4) . ? O2 Cs1 2.996(4) . ? Cs1 O2 2.996(4) 6 ? Cs1 O1 3.030(4) 6 ? Cs1 O3 3.031(19) . ? Cs1 O3 3.031(19) 6 ? Cs1 N1 3.194(7) 1_655 ? Cs1 C4 3.564(6) 1_655 ? Cs1 C4 3.564(6) 6_655 ? Cs1 N3 3.763(5) 1_655 ? Cs1 N3 3.763(5) 6_655 ? Cs1 C14 3.808(6) 6 ? Tb1 O2 2.270(4) 6 ? Tb1 N3 2.463(5) 6 ? Tb1 N6 2.502(5) 6 ? Tb1 Cs1 4.6389(7) 1_455 ? O3 C28 1.426(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C1 121.7(4) . 6 ? C2 C1 H1 119.1 . . ? C1 C1 H1 119.1 6 . ? C1 C2 C3 117.2(7) . . ? C1 C2 H2 121.4 . . ? C3 C2 H2 121.4 . . ? C2 C3 C3 121.1(4) . 6 ? C2 C3 C4 132.7(6) . . ? C3 C3 C4 106.2(4) 6 . ? N2 C4 N1 127.5(6) . . ? N2 C4 C3 122.7(6) . . ? N1 C4 C3 109.7(6) . . ? N2 C4 Cs1 97.1(3) . 1_455 ? N1 C4 Cs1 63.4(3) . 1_455 ? C3 C4 Cs1 107.4(4) . 1_455 ? N2 C5 N3 127.6(6) . . ? N2 C5 C6 122.3(6) . . ? N3 C5 C6 110.1(5) . . ? C7 C6 C11 121.0(6) . . ? C7 C6 C5 132.6(6) . . ? C11 C6 C5 106.4(5) . . ? C8 C7 C6 117.7(6) . . ? C8 C7 H7 121.2 . . ? C6 C7 H7 121.2 . . ? C7 C8 C9 122.4(6) . . ? C7 C8 H8 118.8 . . ? C9 C8 H8 118.8 . . ? C10 C9 C8 119.4(6) . . ? C10 C9 H9 120.3 . . ? C8 C9 H9 120.3 . . ? C11 C10 C9 118.4(6) . . ? C11 C10 H10 120.8 . . ? C9 C10 H10 120.8 . . ? C10 C11 C6 121.2(6) . . ? C10 C11 C12 132.4(6) . . ? C6 C11 C12 106.4(5) . . ? N4 C12 N3 127.6(5) . . ? N4 C12 C11 123.0(5) . . ? N3 C12 C11 109.3(5) . . ? N4 C13 N5 128.3(5) . . ? N4 C13 C14 122.9(5) . . ? N5 C13 C14 108.7(5) . . ? C14 C14 C15 120.8(3) 6 . ? C14 C14 C13 106.4(3) 6 . ? C15 C14 C13 132.8(5) . . ? C16 C15 C14 117.6(6) . . ? C16 C15 H15 121.2 . . ? C14 C15 H15 121.2 . . ? C15 C16 C16 121.5(4) . 6 ? C15 C16 H16 119.2 . . ? C16 C16 H16 119.2 6 . ? O1 C17 H17A 109.5 . . ? O1 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? O1 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 O1 125.5(6) . . ? C19 C18 C23 121.4(6) . . ? O1 C18 C23 113.0(5) . . ? C18 C19 C20 121.4(6) . . ? C18 C19 H19 119.3 . . ? C20 C19 H19 119.3 . . ? C21 C20 C19 118.9(6) . . ? C21 C20 H20 120.5 . . ? C19 C20 H20 120.5 . . ? C20 C21 C22 121.2(6) . . ? C20 C21 H21 119.4 . . ? C22 C21 H21 119.4 . . ? C21 C22 C23 120.2(6) . . ? C21 C22 C24 117.5(6) . . ? C23 C22 C24 122.2(5) . . ? O2 C23 C22 123.6(5) . . ? O2 C23 C18 119.9(5) . . ? C22 C23 C18 116.6(5) . . ? N6 C24 C22 126.7(5) . . ? N6 C24 H24 116.7 . . ? C22 C24 H24 116.7 . . ? C26 C25 C25 119.1(4) . 6 ? C26 C25 N6 124.4(5) . . ? C25 C25 N6 116.5(3) 6 . ? C25 C26 C27 121.1(6) . . ? C25 C26 H26 119.4 . . ? C27 C26 H26 119.4 . . ? C27 C27 C26 119.8(4) 6 . ? C27 C27 H27 120.1 6 . ? C26 C27 H27 120.1 . . ? C4 N1 C4 107.9(7) . 6 ? C4 N1 Tb1 121.7(4) . . ? C4 N1 Tb1 121.7(4) 6 . ? C4 N1 Cs1 94.0(4) . 1_455 ? C4 N1 Cs1 94.0(4) 6 1_455 ? Tb1 N1 Cs1 109.9(2) . 1_455 ? C5 N2 C4 123.1(5) . . ? C5 N3 C12 107.7(5) . . ? C5 N3 Tb1 122.2(4) . . ? C12 N3 Tb1 121.9(4) . . ? C5 N3 Cs1 89.0(3) . 1_455 ? C12 N3 Cs1 115.8(3) . 1_455 ? Tb1 N3 Cs1 94.00(14) . 1_455 ? C12 N4 C13 123.7(5) . . ? C13 N5 C13 109.6(7) . 6 ? C13 N5 Tb1 121.3(4) . . ? C13 N5 Tb1 121.3(4) 6 . ? C13 N5 Cs1 80.7(4) . . ? C13 N5 Cs1 80.7(4) 6 . ? Tb1 N5 Cs1 80.46(17) . . ? C24 N6 C25 119.5(5) . . ? C24 N6 Tb1 125.6(4) . . ? C25 N6 Tb1 114.7(3) . . ? C18 O1 C17 116.9(5) . . ? C18 O1 Cs1 124.3(3) . . ? C17 O1 Cs1 118.7(4) . . ? C23 O2 Tb1 129.0(4) . . ? C23 O2 Cs1 123.8(4) . . ? Tb1 O2 Cs1 105.56(14) . . ? O2 Cs1 O2 57.72(15) 6 . ? O2 Cs1 O1 108.53(11) 6 . ? O2 Cs1 O1 51.68(11) . . ? O2 Cs1 O1 51.68(11) 6 6 ? O2 Cs1 O1 108.53(11) . 6 ? O1 Cs1 O1 152.60(17) . 6 ? O2 Cs1 O3 158.7(4) 6 . ? O2 Cs1 O3 125.4(3) . . ? O1 Cs1 O3 74.8(3) . . ? O1 Cs1 O3 116.5(3) 6 . ? O2 Cs1 O3 125.4(3) 6 6 ? O2 Cs1 O3 158.7(4) . 6 ? O1 Cs1 O3 116.5(3) . 6 ? O1 Cs1 O3 74.8(3) 6 6 ? O3 Cs1 O3 42.8(5) . 6 ? O2 Cs1 N1 89.67(13) 6 1_655 ? O2 Cs1 N1 89.67(13) . 1_655 ? O1 Cs1 N1 99.27(9) . 1_655 ? O1 Cs1 N1 99.27(9) 6 1_655 ? O3 Cs1 N1 110.8(4) . 1_655 ? O3 Cs1 N1 110.8(4) 6 1_655 ? O2 Cs1 C4 87.00(13) 6 1_655 ? O2 Cs1 C4 69.27(13) . 1_655 ? O1 Cs1 C4 78.81(13) . 1_655 ? O1 Cs1 C4 114.39(13) 6 1_655 ? O3 Cs1 C4 114.1(4) . 1_655 ? O3 Cs1 C4 129.5(4) 6 1_655 ? N1 Cs1 C4 22.67(12) 1_655 1_655 ? O2 Cs1 C4 69.27(13) 6 6_655 ? O2 Cs1 C4 87.00(13) . 6_655 ? O1 Cs1 C4 114.39(13) . 6_655 ? O1 Cs1 C4 78.81(13) 6 6_655 ? O3 Cs1 C4 129.5(4) . 6_655 ? O3 Cs1 C4 114.1(4) 6 6_655 ? N1 Cs1 C4 22.67(12) 1_655 6_655 ? C4 Cs1 C4 36.4(2) 1_655 6_655 ? O2 Cs1 N3 133.27(10) 6 1_655 ? O2 Cs1 N3 100.48(10) . 1_655 ? O1 Cs1 N3 72.02(11) . 1_655 ? O1 Cs1 N3 134.83(11) 6 1_655 ? O3 Cs1 N3 68.0(4) . 1_655 ? O3 Cs1 N3 90.4(4) 6 1_655 ? N1 Cs1 N3 46.26(11) 1_655 1_655 ? C4 Cs1 N3 46.52(12) 1_655 1_655 ? C4 Cs1 N3 68.77(12) 6_655 1_655 ? O2 Cs1 N3 100.48(10) 6 6_655 ? O2 Cs1 N3 133.27(10) . 6_655 ? O1 Cs1 N3 134.83(11) . 6_655 ? O1 Cs1 N3 72.02(11) 6 6_655 ? O3 Cs1 N3 90.4(4) . 6_655 ? O3 Cs1 N3 68.0(4) 6 6_655 ? N1 Cs1 N3 46.26(11) 1_655 6_655 ? C4 Cs1 N3 68.77(12) 1_655 6_655 ? C4 Cs1 N3 46.52(12) 6_655 6_655 ? N3 Cs1 N3 62.89(14) 1_655 6_655 ? O2 Cs1 C14 77.23(11) 6 6 ? O2 Cs1 C14 87.50(12) . 6 ? O1 Cs1 C14 89.71(12) . 6 ? O1 Cs1 C14 68.76(12) 6 6 ? O3 Cs1 C14 81.8(4) . 6 ? O3 Cs1 C14 74.0(4) 6 6 ? N1 Cs1 C14 165.99(11) 1_655 6 ? C4 Cs1 C14 156.50(13) 1_655 6 ? C4 Cs1 C14 143.35(13) 6_655 6 ? N3 Cs1 C14 147.73(11) 1_655 6 ? N3 Cs1 C14 130.82(11) 6_655 6 ? O2 Tb1 O2 79.2(2) . 6 ? O2 Tb1 N1 139.13(11) . . ? O2 Tb1 N1 139.13(11) 6 . ? O2 Tb1 N3 148.31(15) . 6 ? O2 Tb1 N3 80.51(15) 6 6 ? N1 Tb1 N3 69.03(14) . 6 ? O2 Tb1 N3 80.51(15) . . ? O2 Tb1 N3 148.31(15) 6 . ? N1 Tb1 N3 69.03(14) . . ? N3 Tb1 N3 105.7(2) 6 . ? O2 Tb1 N5 84.72(16) . . ? O2 Tb1 N5 84.72(16) 6 . ? N1 Tb1 N5 108.0(2) . . ? N3 Tb1 N5 69.39(14) 6 . ? N3 Tb1 N5 69.39(14) . . ? O2 Tb1 N6 112.61(14) . 6 ? O2 Tb1 N6 72.66(14) 6 6 ? N1 Tb1 N6 77.42(17) . 6 ? N3 Tb1 N6 83.79(15) 6 6 ? N3 Tb1 N6 138.23(15) . 6 ? N5 Tb1 N6 147.49(11) . 6 ? O2 Tb1 N6 72.66(14) . . ? O2 Tb1 N6 112.61(14) 6 . ? N1 Tb1 N6 77.42(17) . . ? N3 Tb1 N6 138.23(15) 6 . ? N3 Tb1 N6 83.79(15) . . ? N5 Tb1 N6 147.49(11) . . ? N6 Tb1 N6 64.8(2) 6 . ? O2 Tb1 Cs1 43.20(10) . . ? O2 Tb1 Cs1 43.20(10) 6 . ? N1 Tb1 Cs1 172.18(15) . . ? N3 Tb1 Cs1 106.76(11) 6 . ? N3 Tb1 Cs1 106.76(11) . . ? N5 Tb1 Cs1 64.18(16) . . ? N6 Tb1 Cs1 109.08(11) 6 . ? N6 Tb1 Cs1 109.08(11) . . ? O2 Tb1 Cs1 132.29(10) . 1_455 ? O2 Tb1 Cs1 132.29(10) 6 1_455 ? N1 Tb1 Cs1 40.33(15) . 1_455 ? N3 Tb1 Cs1 54.02(11) 6 1_455 ? N3 Tb1 Cs1 54.02(11) . 1_455 ? N5 Tb1 Cs1 67.67(16) . 1_455 ? N6 Tb1 Cs1 111.21(10) 6 1_455 ? N6 Tb1 Cs1 111.21(10) . 1_455 ? Cs1 Tb1 Cs1 131.856(18) . 1_455 ? C28 O3 Cs1 107.6(11) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.129 _refine_diff_density_min -1.986 _refine_diff_density_rms 0.133 _database_code_depnum_ccdc_archive 'CCDC 955772' ####################################################################### # # 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_TbZn _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C70 H60 N13 O10 Tb Zn' _chemical_formula_weight 1467.60 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' Zn Zn 0.2839 1.4301 '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 P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' 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 13.1038(3) _cell_length_b 32.3516(6) _cell_length_c 15.5736(4) _cell_angle_alpha 90.00 _cell_angle_beta 105.086(2) _cell_angle_gamma 90.00 _cell_volume 6374.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 149.95(10) _cell_measurement_reflns_used 5751 _cell_measurement_theta_min 2.8539 _cell_measurement_theta_max 27.9853 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.529 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2984 _exptl_absorpt_coefficient_mu 1.549 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7897 _exptl_absorpt_correction_T_max 0.8732 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 149.95(10) _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, Eos, Gemini' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.2141 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 24066 _diffrn_reflns_av_R_equivalents 0.0783 _diffrn_reflns_av_sigmaI/netI 0.1320 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.86 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11197 _reflns_number_gt 7288 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker FRAMBO' _computing_cell_refinement 'Bruker FRAMBO' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0705P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11197 _refine_ls_number_parameters 836 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.1119 _refine_ls_R_factor_gt 0.0666 _refine_ls_wR_factor_ref 0.1619 _refine_ls_wR_factor_gt 0.1450 _refine_ls_goodness_of_fit_ref 0.977 _refine_ls_restrained_S_all 0.978 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.5942(6) 0.0756(2) 0.3831(4) 0.0213(17) Uani 1 1 d . . . H053 H 0.5361 0.0629 0.3451 0.026 Uiso 1 1 calc R . . C2 C 0.6958(6) 0.0686(2) 0.3760(5) 0.0241(18) Uani 1 1 d . . . H070 H 0.7062 0.0507 0.3322 0.029 Uiso 1 1 calc R . . C3 C 0.7830(6) 0.0877(2) 0.4330(5) 0.0282(19) Uani 1 1 d . . . H037 H 0.8506 0.0814 0.4283 0.034 Uiso 1 1 calc R . . C4 C 0.7702(6) 0.1161(2) 0.4972(5) 0.0251(18) Uani 1 1 d . . . H033 H 0.8280 0.1299 0.5331 0.030 Uiso 1 1 calc R . . C5 C 0.6698(6) 0.1230(2) 0.5056(4) 0.0182(17) Uani 1 1 d . . . C6 C 0.5827(6) 0.1027(2) 0.4497(5) 0.0198(17) Uani 1 1 d U . . C7 C 0.8178(6) 0.2456(3) 0.7421(5) 0.029(2) Uani 1 1 d . . . H1 H 0.8647 0.2297 0.7202 0.035 Uiso 1 1 calc R . . C8 C 0.8522(7) 0.2795(3) 0.7965(5) 0.036(2) Uani 1 1 d . . . H073 H 0.9235 0.2865 0.8115 0.043 Uiso 1 1 calc R . . C9 C 0.7825(7) 0.3031(3) 0.8289(5) 0.037(2) Uani 1 1 d . . . H444 H 0.8086 0.3254 0.8658 0.044 Uiso 1 1 calc R . . C10 C 0.6754(7) 0.2947(3) 0.8083(5) 0.031(2) Uani 1 1 d . . . H062 H 0.6290 0.3110 0.8297 0.038 Uiso 1 1 calc R . . C11 C 0.6401(6) 0.2602(3) 0.7536(5) 0.0256(19) Uani 1 1 d . . . C12 C 0.7108(6) 0.2362(2) 0.7217(5) 0.0254(19) Uani 1 1 d . . . C13 C 0.1351(7) 0.3209(3) 0.7168(5) 0.037(2) Uani 1 1 d . . . H045 H 0.1220 0.3456 0.7426 0.045 Uiso 1 1 calc R . . C14 C 0.2382(7) 0.3084(3) 0.7276(5) 0.031(2) Uani 1 1 d . . . H058 H 0.2946 0.3245 0.7586 0.037 Uiso 1 1 calc R . . C15 C 0.2547(6) 0.2701(2) 0.6896(5) 0.0227(18) Uani 1 1 d . . . C16 C 0.1684(6) 0.2475(2) 0.6415(5) 0.0259(19) Uani 1 1 d . . . C17 C 0.0660(6) 0.2601(3) 0.6303(5) 0.0288(19) Uani 1 1 d . . . H079 H 0.0095 0.2443 0.5985 0.035 Uiso 1 1 calc R . . C18 C 0.0502(7) 0.2977(3) 0.6687(5) 0.032(2) Uani 1 1 d . . . H069 H -0.0182 0.3074 0.6619 0.039 Uiso 1 1 calc R . . C19 C 0.0223(6) 0.1302(3) 0.3968(5) 0.0265(19) Uani 1 1 d . . . H125 H -0.0241 0.1469 0.4174 0.032 Uiso 1 1 calc R . . C20 C 0.1301(6) 0.1308(2) 0.4360(4) 0.0192(17) Uani 1 1 d . . . C21 C 0.1999(6) 0.1067(2) 0.4038(4) 0.0215(18) Uani 1 1 d . . . C22 C 0.1629(6) 0.0797(2) 0.3322(5) 0.0258(18) Uani 1 1 d . . . H076 H 0.2094 0.0633 0.3111 0.031 Uiso 1 1 calc R . . C23 C 0.0553(6) 0.0782(2) 0.2937(5) 0.0273(19) Uani 1 1 d . . . H063 H 0.0286 0.0602 0.2467 0.033 Uiso 1 1 calc R . . C24 C -0.0134(7) 0.1036(3) 0.3249(5) 0.032(2) Uani 1 1 d . . . H051 H -0.0853 0.1026 0.2969 0.038 Uiso 1 1 calc R . . C25 C 0.4911(5) 0.1155(2) 0.4781(4) 0.0171(16) Uani 1 1 d U . . C26 C 0.3060(6) 0.1168(2) 0.4562(5) 0.0236(18) Uani 1 1 d . . . C27 C 0.1953(6) 0.1554(2) 0.5088(4) 0.0184(17) Uani 1 1 d . . . C28 C 0.2147(6) 0.2113(2) 0.6080(4) 0.0213(18) Uani 1 1 d . . . C29 C 0.3521(6) 0.2477(2) 0.6882(5) 0.0227(18) Uani 1 1 d . . . C30 C 0.5344(6) 0.2433(2) 0.7174(5) 0.0209(17) Uani 1 1 d . . . C31 C 0.6477(6) 0.2032(2) 0.6703(4) 0.0224(18) Uani 1 1 d . . . C32 C 0.6268(6) 0.1491(2) 0.5650(5) 0.0238(18) Uani 1 1 d . . . C33 C 0.6531(6) 0.0086(3) 0.6077(5) 0.0285(19) Uani 1 1 d . . . H336 H 0.6640 -0.0143 0.5751 0.034 Uiso 1 1 calc R . . C34 C 0.7398(7) 0.0306(3) 0.6585(5) 0.033(2) Uani 1 1 d . . . H047 H 0.8082 0.0223 0.6601 0.040 Uiso 1 1 calc R . . C35 C 0.7233(6) 0.0651(2) 0.7068(5) 0.029(2) Uani 1 1 d . . . H227 H 0.7809 0.0797 0.7409 0.035 Uiso 1 1 calc R . . C36 C 0.6226(6) 0.0776(2) 0.7044(5) 0.0215(18) Uani 1 1 d . . . C37 C 0.5335(6) 0.0558(2) 0.6511(5) 0.0236(18) Uani 1 1 d . . . C38 C 0.5524(6) 0.0207(2) 0.6057(5) 0.0266(19) Uani 1 1 d . . . H038 H 0.4956 0.0051 0.5735 0.032 Uiso 1 1 calc R . . C39 C 0.5368(7) 0.2128(3) 0.9222(5) 0.034(2) Uani 1 1 d . . . C40 C 0.6278(8) 0.2289(3) 0.9768(5) 0.042(2) Uani 1 1 d . . . H043 H 0.6224 0.2518 1.0114 0.050 Uiso 1 1 calc R . . C41 C 0.7266(8) 0.2127(3) 0.9826(6) 0.046(3) Uani 1 1 d . . . H987 H 0.7860 0.2247 1.0205 0.055 Uiso 1 1 calc R . . C42 C 0.7375(7) 0.1781(3) 0.9311(5) 0.040(2) Uani 1 1 d . . . H057 H 0.8034 0.1666 0.9343 0.048 Uiso 1 1 calc R . . C43 C 0.6443(6) 0.1614(2) 0.8743(5) 0.0269(19) Uani 1 1 d . . . C44 C 0.5457(6) 0.1772(2) 0.8682(5) 0.0253(19) Uani 1 1 d . . . C45 C 0.2438(6) 0.0592(2) 0.6297(5) 0.0247(18) Uani 1 1 d . . . C46 C 0.2190(6) 0.0953(2) 0.6743(5) 0.0231(18) Uani 1 1 d . . . C47 C 0.1131(6) 0.1018(2) 0.6719(5) 0.0256(18) Uani 1 1 d . . . C48 C 0.0339(6) 0.0766(3) 0.6270(5) 0.031(2) Uani 1 1 d . . . H559 H -0.0360 0.0826 0.6251 0.038 Uiso 1 1 calc R . . C49 C 0.0587(7) 0.0413(3) 0.5835(6) 0.040(2) Uani 1 1 d . . . H066 H 0.0051 0.0237 0.5535 0.048 Uiso 1 1 calc R . . C50 C 0.1604(7) 0.0329(3) 0.5851(5) 0.035(2) Uani 1 1 d . . . H044 H 0.1758 0.0094 0.5564 0.042 Uiso 1 1 calc R . . C51 C 0.4529(9) 0.1459(3) 1.0467(7) 0.061(3) Uani 1 1 d . . . H565 H 0.3996 0.1657 1.0341 0.074 Uiso 1 1 calc R . . C52 C 0.5237(10) 0.1472(4) 1.1294(7) 0.080(4) Uani 1 1 d . . . H36 H 0.5189 0.1671 1.1712 0.095 Uiso 1 1 calc R . . C53 C 0.6006(12) 0.1179(4) 1.1469(8) 0.089(5) Uani 1 1 d . . . H049 H 0.6490 0.1173 1.2024 0.106 Uiso 1 1 calc R . . C54 C 0.6078(10) 0.0900(5) 1.0853(9) 0.082(4) Uani 1 1 d . . . H56 H 0.6616 0.0705 1.0964 0.098 Uiso 1 1 calc R . . C55 C 0.5302(9) 0.0913(4) 1.0023(7) 0.069(3) Uani 1 1 d . . . H669 H 0.5338 0.0717 0.9597 0.083 Uiso 1 1 calc R . . C56 C 0.2184(7) 0.1989(3) 0.8531(5) 0.035(2) Uani 1 1 d . . . H046 H 0.2578 0.2082 0.8151 0.042 Uiso 1 1 calc R . . C57 C 0.1417(8) 0.2244(3) 0.8703(6) 0.046(3) Uani 1 1 d . . . H035 H 0.1299 0.2503 0.8438 0.055 Uiso 1 1 calc R . . C58 C 0.0838(9) 0.2118(4) 0.9258(6) 0.061(3) Uani 1 1 d . . . H121 H 0.0329 0.2290 0.9388 0.073 Uiso 1 1 calc R . . C59 C 0.1019(10) 0.1730(4) 0.9623(7) 0.073(4) Uani 1 1 d . . . H232 H 0.0626 0.1633 0.9999 0.088 Uiso 1 1 calc R . . C61 C 0.6626(6) 0.1257(3) 0.8222(5) 0.031(2) Uani 1 1 d . . . H080 H 0.7251 0.1109 0.8428 0.037 Uiso 1 1 calc R . . C62 C 0.3505(6) 0.0484(3) 0.6321(4) 0.0222(18) Uani 1 1 d . . . H059 H 0.3621 0.0207 0.6214 0.027 Uiso 1 1 calc R . . C63 C 0.9256(16) 0.0901(6) 1.0396(11) 0.179(10) Uani 1 1 d . . . H99A H 0.9775 0.1092 1.0721 0.268 Uiso 1 1 calc R . . H99B H 0.9511 0.0624 1.0521 0.268 Uiso 1 1 calc R . . H99C H 0.8611 0.0934 1.0571 0.268 Uiso 1 1 calc R . . C64 C 0.3886(14) 0.0268(6) 0.1575(11) 0.137(6) Uiso 1 1 d . . . H66A H 0.4021 0.0111 0.2123 0.164 Uiso 1 1 calc R . . H66B H 0.4557 0.0329 0.1448 0.164 Uiso 1 1 calc R . . C65 C 0.3190(13) 0.0031(6) 0.0830(11) 0.136(6) Uiso 1 1 d . . . H55A H 0.3175 -0.0261 0.0976 0.163 Uiso 1 1 calc R . . H55B H 0.3413 0.0061 0.0286 0.163 Uiso 1 1 calc R . . C67 C 0.2118(13) 0.0236(6) 0.0752(10) 0.121(6) Uiso 1 1 d . . . H36A H 0.1781 0.0297 0.0134 0.145 Uiso 1 1 calc R . . H36B H 0.1663 0.0050 0.0972 0.145 Uiso 1 1 calc R . . C68 C 0.2261(11) 0.0588(5) 0.1232(9) 0.102(5) Uiso 1 1 d . . . H96A H 0.1859 0.0576 0.1673 0.122 Uiso 1 1 calc R . . H96B H 0.2004 0.0821 0.0842 0.122 Uiso 1 1 calc R . . C69 C 0.4242(9) 0.2659(3) 0.9502(7) 0.061(3) Uani 1 1 d . . . H45A H 0.3503 0.2721 0.9396 0.091 Uiso 1 1 calc R . . H45B H 0.4575 0.2867 0.9228 0.091 Uiso 1 1 calc R . . H45C H 0.4564 0.2655 1.0130 0.091 Uiso 1 1 calc R . . C71 C -0.0080(7) 0.1472(3) 0.7156(7) 0.063(3) Uani 1 1 d . . . H65A H -0.0469 0.1518 0.6551 0.095 Uiso 1 1 calc R . . H65B H -0.0084 0.1720 0.7495 0.095 Uiso 1 1 calc R . . H65C H -0.0402 0.1252 0.7405 0.095 Uiso 1 1 calc R . . C363 C 0.1789(8) 0.1488(3) 0.9424(6) 0.049(3) Uani 1 1 d . . . H363 H 0.1903 0.1225 0.9674 0.059 Uiso 1 1 calc R . . N1 N 0.1553(5) 0.18487(18) 0.5492(4) 0.0198(14) Uani 1 1 d . . . N2 N 0.3922(5) 0.10243(19) 0.4380(4) 0.0200(14) Uani 1 1 d . . . N3 N 0.6878(5) 0.17572(19) 0.6220(4) 0.0209(14) Uani 1 1 d . . . N4 N 0.4475(5) 0.2609(2) 0.7265(4) 0.0238(15) Uani 1 1 d . . . N5 N 0.5206(5) 0.14303(18) 0.5489(4) 0.0183(14) Uani 1 1 d . . . N6 N 0.2986(5) 0.14521(19) 0.5217(4) 0.0211(14) Uani 1 1 d . . . N7 N 0.3219(5) 0.21201(19) 0.6401(4) 0.0200(14) Uani 1 1 d . . . N8 N 0.5447(5) 0.20710(19) 0.6709(4) 0.0189(14) Uani 1 1 d . . . N9 N 0.4321(5) 0.07187(18) 0.6470(3) 0.0188(14) Uani 1 1 d . . . N10 N 0.5957(5) 0.11318(19) 0.7475(4) 0.0221(15) Uani 1 1 d . . . N11 N 0.2382(6) 0.1610(2) 0.8891(4) 0.0332(18) Uani 1 1 d . . . N12 N 0.4554(6) 0.1181(3) 0.9828(5) 0.042(2) Uani 1 1 d . . . N13 N 0.3152(10) 0.0391(3) 0.8457(6) 0.067(3) Uani 1 1 d . . . O1 O 0.4017(7) 0.0476(3) 0.8328(4) 0.083(3) Uani 1 1 d . . . O2 O 0.2762(10) 0.0043(2) 0.8402(6) 0.125(4) Uani 1 1 d . . . O3 O 0.2625(5) 0.0690(2) 0.8689(4) 0.0470(17) Uani 1 1 d . . . O4 O 0.2939(4) 0.12096(16) 0.7177(3) 0.0238(12) Uani 1 1 d . . . O5 O 0.0970(4) 0.13649(17) 0.7185(3) 0.0298(13) Uani 1 1 d . . . O6 O 0.4556(4) 0.16240(16) 0.8151(3) 0.0234(12) Uani 1 1 d . . . O7 O 0.4367(5) 0.22645(18) 0.9131(3) 0.0360(15) Uani 1 1 d . . . O8 O 0.3337(15) 0.0647(6) 0.1659(10) 0.218(7) Uiso 1 1 d . . . O10 O 0.9068(9) 0.0979(3) 0.9480(7) 0.117(4) Uani 1 1 d . . . H555 H 0.9230 0.0775 0.9233 0.176 Uiso 1 1 calc R . . Zn1 Zn 0.34876(8) 0.12401(3) 0.85606(6) 0.0301(3) Uani 1 1 d . . . Tb1 Tb 0.42780(3) 0.149009(11) 0.66462(2) 0.01909(13) Uani 1 1 d . . . O99 O 1.0427(10) 0.0578(5) 0.8692(14) 0.212(8) Uani 1 1 d D . . H99 H 1.1049 0.0623 0.8714 0.318 Uiso 1 1 calc R . . C99 C 1.0149(13) 0.0198(5) 0.8329(10) 0.137(7) Uani 1 1 d D . . H99D H 1.0280 -0.0006 0.8791 0.205 Uiso 1 1 calc R . . H99E H 1.0559 0.0135 0.7917 0.205 Uiso 1 1 calc R . . H99F H 0.9411 0.0198 0.8022 0.205 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 0.034(5) 0.009(4) 0.018(4) 0.000(3) 0.001(3) -0.002(4) C2 0.040(5) 0.013(4) 0.022(4) 0.002(3) 0.012(3) 0.002(4) C3 0.032(5) 0.020(5) 0.037(5) -0.003(4) 0.018(4) -0.001(4) C4 0.034(5) 0.015(4) 0.029(4) 0.004(4) 0.012(3) 0.001(4) C5 0.029(4) 0.009(4) 0.016(4) 0.007(3) 0.005(3) -0.003(4) C6 0.031(4) 0.006(4) 0.023(4) 0.006(3) 0.008(3) 0.004(3) C7 0.028(5) 0.025(5) 0.033(5) -0.010(4) 0.005(4) 0.006(4) C8 0.030(5) 0.027(5) 0.051(6) -0.007(4) 0.012(4) -0.008(4) C9 0.039(5) 0.023(5) 0.044(5) -0.022(4) 0.001(4) -0.014(5) C10 0.037(5) 0.015(5) 0.041(5) -0.012(4) 0.009(4) -0.004(4) C11 0.028(4) 0.021(5) 0.023(4) 0.000(4) 0.001(3) 0.003(4) C12 0.038(5) 0.010(4) 0.025(4) -0.004(3) 0.002(3) -0.003(4) C13 0.044(6) 0.020(5) 0.049(5) -0.007(4) 0.016(4) 0.011(5) C14 0.039(5) 0.019(5) 0.034(5) -0.002(4) 0.010(4) 0.000(4) C15 0.027(4) 0.015(4) 0.023(4) 0.000(3) 0.002(3) 0.004(4) C16 0.037(5) 0.014(4) 0.024(4) 0.007(4) 0.005(3) 0.002(4) C17 0.029(5) 0.021(5) 0.036(5) -0.001(4) 0.008(4) 0.001(4) C18 0.040(5) 0.023(5) 0.034(5) -0.001(4) 0.011(4) 0.010(4) C19 0.025(4) 0.021(5) 0.034(5) 0.004(4) 0.006(3) -0.003(4) C20 0.031(5) 0.009(4) 0.019(4) 0.006(3) 0.009(3) 0.000(4) C21 0.029(4) 0.016(4) 0.019(4) 0.004(3) 0.004(3) -0.003(4) C22 0.025(5) 0.015(4) 0.039(5) -0.003(4) 0.011(4) -0.003(4) C23 0.038(5) 0.017(4) 0.025(4) -0.004(4) 0.004(3) -0.005(4) C24 0.033(5) 0.024(5) 0.037(5) 0.008(4) 0.005(4) -0.005(4) C25 0.0175(18) 0.0169(18) 0.0166(18) 0.0010(10) 0.0037(10) 0.0007(10) C26 0.041(5) 0.010(4) 0.020(4) 0.001(3) 0.007(3) 0.001(4) C27 0.024(4) 0.013(4) 0.018(4) 0.001(3) 0.005(3) 0.002(4) C28 0.033(5) 0.015(4) 0.016(4) 0.003(3) 0.006(3) 0.005(4) C29 0.036(5) 0.007(4) 0.027(4) -0.004(3) 0.010(3) -0.004(4) C30 0.029(4) 0.010(4) 0.025(4) 0.002(3) 0.009(3) -0.003(4) C31 0.040(5) 0.013(4) 0.012(4) 0.005(3) 0.002(3) -0.004(4) C32 0.027(4) 0.015(4) 0.025(4) 0.010(4) 0.000(3) 0.009(4) C33 0.029(5) 0.024(5) 0.032(5) -0.001(4) 0.007(4) 0.005(4) C34 0.034(5) 0.025(5) 0.040(5) 0.004(4) 0.009(4) 0.003(4) C35 0.026(5) 0.016(5) 0.040(5) 0.008(4) 0.002(4) 0.005(4) C36 0.033(5) 0.007(4) 0.022(4) 0.003(3) 0.003(3) -0.004(4) C37 0.037(5) 0.008(4) 0.026(4) 0.002(3) 0.008(3) 0.004(4) C38 0.034(5) 0.018(5) 0.027(4) -0.002(4) 0.005(3) -0.006(4) C39 0.055(6) 0.021(5) 0.026(5) -0.003(4) 0.010(4) -0.007(5) C40 0.063(7) 0.022(5) 0.035(5) -0.013(4) 0.003(4) -0.009(5) C41 0.044(6) 0.041(6) 0.040(6) -0.017(5) -0.011(4) -0.014(5) C42 0.038(5) 0.038(6) 0.038(5) 0.000(5) -0.001(4) 0.007(5) C43 0.034(5) 0.016(4) 0.026(4) -0.005(3) 0.000(3) -0.009(4) C44 0.038(5) 0.016(4) 0.019(4) 0.006(3) 0.003(3) -0.005(4) C45 0.028(5) 0.016(4) 0.030(4) -0.003(4) 0.007(3) -0.006(4) C46 0.031(5) 0.013(4) 0.023(4) 0.000(3) 0.002(3) -0.005(4) C47 0.034(5) 0.016(4) 0.027(4) -0.002(4) 0.008(3) -0.002(4) C48 0.025(5) 0.027(5) 0.039(5) -0.005(4) 0.002(4) -0.003(4) C49 0.027(5) 0.033(6) 0.054(6) -0.016(5) -0.001(4) -0.005(5) C50 0.043(6) 0.016(5) 0.044(5) -0.008(4) 0.006(4) 0.004(4) C51 0.083(8) 0.028(6) 0.056(7) 0.013(5) -0.013(6) -0.010(6) C52 0.109(10) 0.042(7) 0.056(7) 0.018(6) -0.037(7) -0.009(8) C53 0.123(12) 0.057(9) 0.061(9) 0.025(7) -0.021(8) -0.014(9) C54 0.070(8) 0.081(11) 0.084(9) 0.039(8) 0.001(7) 0.031(8) C55 0.057(7) 0.082(10) 0.068(8) 0.014(7) 0.014(6) 0.004(7) C56 0.040(5) 0.034(6) 0.032(5) -0.002(4) 0.009(4) 0.002(5) C57 0.063(7) 0.038(6) 0.033(5) -0.004(5) 0.006(5) 0.012(6) C58 0.076(8) 0.069(9) 0.042(6) -0.001(6) 0.021(5) 0.024(7) C59 0.103(10) 0.070(9) 0.067(8) 0.022(7) 0.060(7) 0.024(8) C61 0.029(5) 0.026(5) 0.035(5) 0.004(4) 0.004(4) -0.003(4) C62 0.030(5) 0.017(4) 0.021(4) -0.004(3) 0.010(3) 0.009(4) C63 0.25(2) 0.118(17) 0.117(14) 0.059(13) -0.046(14) -0.002(17) C69 0.078(8) 0.039(7) 0.064(7) -0.035(6) 0.017(6) -0.001(6) C71 0.035(6) 0.060(8) 0.092(8) -0.044(7) 0.010(5) 0.010(6) C363 0.068(7) 0.049(7) 0.041(5) 0.013(5) 0.032(5) 0.017(6) N1 0.030(4) 0.010(3) 0.019(3) -0.002(3) 0.007(3) 0.001(3) N2 0.027(4) 0.008(3) 0.026(3) 0.001(3) 0.008(3) -0.003(3) N3 0.028(4) 0.011(3) 0.023(3) 0.000(3) 0.006(3) 0.002(3) N4 0.024(4) 0.012(4) 0.032(4) -0.005(3) 0.002(3) 0.000(3) N5 0.025(4) 0.004(3) 0.026(3) 0.000(3) 0.005(3) -0.001(3) N6 0.028(4) 0.011(3) 0.025(3) -0.002(3) 0.007(3) 0.001(3) N7 0.025(4) 0.012(3) 0.020(3) -0.004(3) 0.001(3) 0.001(3) N8 0.021(3) 0.012(3) 0.021(3) -0.003(3) 0.001(3) 0.001(3) N9 0.032(4) 0.006(3) 0.015(3) -0.006(2) -0.001(3) 0.002(3) N10 0.030(4) 0.007(3) 0.026(4) 0.003(3) 0.001(3) -0.002(3) N11 0.051(5) 0.026(4) 0.024(4) -0.005(3) 0.011(3) -0.009(4) N12 0.051(5) 0.033(5) 0.037(5) 0.013(4) 0.001(4) -0.005(4) N13 0.111(9) 0.039(6) 0.051(6) 0.018(5) 0.019(6) 0.016(7) O1 0.093(6) 0.120(9) 0.038(4) 0.020(5) 0.020(4) 0.051(7) O2 0.269(14) 0.018(5) 0.084(6) 0.006(4) 0.039(7) 0.003(7) O3 0.070(5) 0.028(4) 0.043(4) 0.005(3) 0.015(3) -0.006(4) O4 0.027(3) 0.022(3) 0.023(3) 0.001(2) 0.007(2) 0.000(3) O5 0.031(3) 0.025(3) 0.034(3) -0.010(3) 0.009(2) 0.004(3) O6 0.030(3) 0.021(3) 0.018(3) -0.015(2) 0.005(2) -0.004(3) O7 0.049(4) 0.022(3) 0.038(3) -0.015(3) 0.014(3) 0.002(3) O10 0.110(8) 0.080(8) 0.131(8) -0.002(6) -0.024(7) 0.043(7) Zn1 0.0433(6) 0.0220(6) 0.0253(5) -0.0002(4) 0.0097(4) -0.0010(5) Tb1 0.0261(2) 0.00821(19) 0.0220(2) -0.00122(17) 0.00456(14) 0.00018(19) O99 0.101(9) 0.146(13) 0.36(2) -0.155(14) 0.004(12) 0.017(10) C99 0.107(13) 0.18(2) 0.112(13) 0.010(13) 0.010(10) -0.024(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.383(10) . ? C1 C6 1.396(10) . ? C1 H053 0.9300 . ? C2 C3 1.396(10) . ? C2 H070 0.9300 . ? C3 C4 1.400(10) . ? C3 H037 0.9300 . ? C4 C5 1.374(10) . ? C4 H033 0.9300 . ? C5 C6 1.406(10) . ? C5 C32 1.469(10) . ? C6 C25 1.444(10) . ? C7 C12 1.388(11) . ? C7 C8 1.389(11) . ? C7 H1 0.9300 . ? C8 C9 1.382(11) . ? C8 H073 0.9300 . ? C9 C10 1.383(11) . ? C9 H444 0.9300 . ? C10 C11 1.405(10) . ? C10 H062 0.9300 . ? C11 C12 1.397(11) . ? C11 C30 1.460(10) . ? C12 C31 1.455(10) . ? C13 C14 1.378(11) . ? C13 C18 1.388(11) . ? C13 H045 0.9300 . ? C14 C15 1.413(11) . ? C14 H058 0.9300 . ? C15 C16 1.391(10) . ? C15 C29 1.473(10) . ? C16 C17 1.370(11) . ? C16 C28 1.476(11) . ? C17 C18 1.394(11) . ? C17 H079 0.9300 . ? C18 H069 0.9300 . ? C19 C20 1.386(10) . ? C19 C24 1.394(11) . ? C19 H125 0.9300 . ? C20 C21 1.391(10) . ? C20 C27 1.464(10) . ? C21 C22 1.399(10) . ? C21 C26 1.455(10) . ? C22 C23 1.381(10) . ? C22 H076 0.9300 . ? C23 C24 1.395(11) . ? C23 H063 0.9300 . ? C24 H051 0.9300 . ? C25 N2 1.352(9) . ? C25 N5 1.391(9) . ? C26 N2 1.318(9) . ? C26 N6 1.395(9) . ? C27 N1 1.323(9) . ? C27 N6 1.357(9) . ? C28 N1 1.343(9) . ? C28 N7 1.364(9) . ? C29 N4 1.309(9) . ? C29 N7 1.377(9) . ? C30 N4 1.314(9) . ? C30 N8 1.401(9) . ? C31 N3 1.355(9) . ? C31 N8 1.358(9) . ? C32 N3 1.341(9) . ? C32 N5 1.362(9) . ? C33 C38 1.368(10) . ? C33 C34 1.398(11) . ? C33 H336 0.9300 . ? C34 C35 1.392(11) . ? C34 H047 0.9300 . ? C35 C36 1.372(10) . ? C35 H227 0.9300 . ? C36 N10 1.422(9) . ? C36 C37 1.431(10) . ? C37 C38 1.394(10) . ? C37 N9 1.412(9) . ? C38 H038 0.9300 . ? C39 O7 1.355(10) . ? C39 C40 1.373(11) . ? C39 C44 1.449(11) . ? C40 C41 1.377(12) . ? C40 H043 0.9300 . ? C41 C42 1.405(12) . ? C41 H987 0.9300 . ? C42 C43 1.415(11) . ? C42 H057 0.9300 . ? C43 C44 1.370(11) . ? C43 C61 1.468(11) . ? C44 O6 1.341(8) . ? C45 C50 1.418(11) . ? C45 C62 1.433(10) . ? C45 C46 1.439(11) . ? C46 O4 1.328(8) . ? C46 C47 1.395(11) . ? C47 C48 1.361(10) . ? C47 O5 1.383(9) . ? C48 C49 1.409(12) . ? C48 H559 0.9300 . ? C49 C50 1.354(11) . ? C49 H066 0.9300 . ? C50 H044 0.9300 . ? C51 N12 1.347(12) . ? C51 C52 1.377(13) . ? C51 H565 0.9300 . ? C52 C53 1.357(18) . ? C52 H36 0.9300 . ? C53 C54 1.337(17) . ? C53 H049 0.9300 . ? C54 C55 1.422(15) . ? C54 H56 0.9300 . ? C55 N12 1.284(13) . ? C55 H669 0.9300 . ? C56 N11 1.345(11) . ? C56 C57 1.379(12) . ? C56 H046 0.9300 . ? C57 C58 1.353(13) . ? C57 H035 0.9300 . ? C58 C59 1.372(15) . ? C58 H121 0.9300 . ? C59 C363 1.376(13) . ? C59 H232 0.9300 . ? C61 N10 1.324(9) . ? C61 H080 0.9300 . ? C62 N9 1.283(9) . ? C62 H059 0.9300 . ? C63 O10 1.405(16) . ? C63 H99A 0.9600 . ? C63 H99B 0.9600 . ? C63 H99C 0.9600 . ? C64 O8 1.44(2) . ? C64 C65 1.49(2) . ? C64 H66A 0.9700 . ? C64 H66B 0.9700 . ? C65 C67 1.530(19) . ? C65 H55A 0.9700 . ? C65 H55B 0.9700 . ? C67 C68 1.348(19) . ? C67 H36A 0.9700 . ? C67 H36B 0.9700 . ? C68 O8 1.406(19) . ? C68 H96A 0.9700 . ? C68 H96B 0.9700 . ? C69 O7 1.428(10) . ? C69 H45A 0.9600 . ? C69 H45B 0.9600 . ? C69 H45C 0.9600 . ? C71 O5 1.408(10) . ? C71 H65A 0.9600 . ? C71 H65B 0.9600 . ? C71 H65C 0.9600 . ? C363 N11 1.335(10) . ? C363 H363 0.9300 . ? N5 Tb1 2.431(6) . ? N6 Tb1 2.424(6) . ? N7 Tb1 2.439(6) . ? N8 Tb1 2.410(6) . ? N9 Tb1 2.513(6) . ? N10 Tb1 2.524(6) . ? N11 Zn1 2.046(7) . ? N12 Zn1 2.109(7) . ? N13 O1 1.232(12) . ? N13 O2 1.233(12) . ? N13 O3 1.292(11) . ? O3 Zn1 2.145(6) . ? O4 Zn1 2.089(5) . ? O4 Tb1 2.311(5) . ? O6 Zn1 2.091(5) . ? O6 Tb1 2.317(4) . ? O10 H555 0.8200 . ? Zn1 Tb1 3.4962(10) . ? O99 C99 1.362(9) . ? O99 H99 0.8200 . ? C99 H99D 0.9600 . ? C99 H99E 0.9600 . ? C99 H99F 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 117.1(7) . . ? C2 C1 H053 121.4 . . ? C6 C1 H053 121.4 . . ? C1 C2 C3 121.4(7) . . ? C1 C2 H070 119.3 . . ? C3 C2 H070 119.3 . . ? C2 C3 C4 121.0(7) . . ? C2 C3 H037 119.5 . . ? C4 C3 H037 119.5 . . ? C5 C4 C3 118.1(7) . . ? C5 C4 H033 121.0 . . ? C3 C4 H033 121.0 . . ? C4 C5 C6 120.5(7) . . ? C4 C5 C32 133.4(7) . . ? C6 C5 C32 106.0(6) . . ? C1 C6 C5 121.8(7) . . ? C1 C6 C25 131.8(7) . . ? C5 C6 C25 106.4(6) . . ? C12 C7 C8 117.5(7) . . ? C12 C7 H1 121.3 . . ? C8 C7 H1 121.3 . . ? C9 C8 C7 121.3(8) . . ? C9 C8 H073 119.4 . . ? C7 C8 H073 119.4 . . ? C8 C9 C10 122.2(8) . . ? C8 C9 H444 118.9 . . ? C10 C9 H444 118.9 . . ? C9 C10 C11 116.8(8) . . ? C9 C10 H062 121.6 . . ? C11 C10 H062 121.6 . . ? C12 C11 C10 120.9(7) . . ? C12 C11 C30 107.7(7) . . ? C10 C11 C30 131.4(7) . . ? C7 C12 C11 121.3(7) . . ? C7 C12 C31 133.0(8) . . ? C11 C12 C31 105.6(7) . . ? C14 C13 C18 122.1(8) . . ? C14 C13 H045 119.0 . . ? C18 C13 H045 119.0 . . ? C13 C14 C15 117.2(8) . . ? C13 C14 H058 121.4 . . ? C15 C14 H058 121.4 . . ? C16 C15 C14 119.7(7) . . ? C16 C15 C29 108.6(7) . . ? C14 C15 C29 131.7(7) . . ? C17 C16 C15 123.0(8) . . ? C17 C16 C28 132.1(7) . . ? C15 C16 C28 104.9(7) . . ? C16 C17 C18 117.0(8) . . ? C16 C17 H079 121.5 . . ? C18 C17 H079 121.5 . . ? C13 C18 C17 121.0(8) . . ? C13 C18 H069 119.5 . . ? C17 C18 H069 119.5 . . ? C20 C19 C24 116.9(8) . . ? C20 C19 H125 121.5 . . ? C24 C19 H125 121.5 . . ? C19 C20 C21 121.5(7) . . ? C19 C20 C27 132.2(7) . . ? C21 C20 C27 106.2(6) . . ? C20 C21 C22 120.9(7) . . ? C20 C21 C26 107.0(6) . . ? C22 C21 C26 132.0(7) . . ? C23 C22 C21 118.1(7) . . ? C23 C22 H076 121.0 . . ? C21 C22 H076 121.0 . . ? C22 C23 C24 120.4(7) . . ? C22 C23 H063 119.8 . . ? C24 C23 H063 119.8 . . ? C19 C24 C23 122.1(7) . . ? C19 C24 H051 119.0 . . ? C23 C24 H051 119.0 . . ? N2 C25 N5 127.0(6) . . ? N2 C25 C6 122.9(6) . . ? N5 C25 C6 110.1(6) . . ? N2 C26 N6 128.0(7) . . ? N2 C26 C21 123.2(7) . . ? N6 C26 C21 108.7(7) . . ? N1 C27 N6 127.5(7) . . ? N1 C27 C20 122.4(7) . . ? N6 C27 C20 109.9(6) . . ? N1 C28 N7 128.4(7) . . ? N1 C28 C16 121.9(7) . . ? N7 C28 C16 109.6(6) . . ? N4 C29 N7 128.8(7) . . ? N4 C29 C15 124.1(7) . . ? N7 C29 C15 107.1(6) . . ? N4 C30 N8 128.4(7) . . ? N4 C30 C11 123.8(7) . . ? N8 C30 C11 107.7(6) . . ? N3 C31 N8 126.4(7) . . ? N3 C31 C12 122.6(7) . . ? N8 C31 C12 110.6(7) . . ? N3 C32 N5 128.3(7) . . ? N3 C32 C5 121.7(7) . . ? N5 C32 C5 109.9(6) . . ? C38 C33 C34 120.3(8) . . ? C38 C33 H336 119.9 . . ? C34 C33 H336 119.9 . . ? C35 C34 C33 119.8(8) . . ? C35 C34 H047 120.1 . . ? C33 C34 H047 120.1 . . ? C36 C35 C34 120.3(8) . . ? C36 C35 H227 119.8 . . ? C34 C35 H227 119.8 . . ? C35 C36 N10 125.5(7) . . ? C35 C36 C37 120.3(7) . . ? N10 C36 C37 114.1(7) . . ? C38 C37 N9 124.5(7) . . ? C38 C37 C36 118.0(7) . . ? N9 C37 C36 117.4(6) . . ? C33 C38 C37 121.3(8) . . ? C33 C38 H038 119.4 . . ? C37 C38 H038 119.4 . . ? O7 C39 C40 127.0(8) . . ? O7 C39 C44 114.8(7) . . ? C40 C39 C44 118.1(9) . . ? C39 C40 C41 123.2(8) . . ? C39 C40 H043 118.4 . . ? C41 C40 H043 118.4 . . ? C40 C41 C42 119.9(8) . . ? C40 C41 H987 120.1 . . ? C42 C41 H987 120.1 . . ? C41 C42 C43 117.5(8) . . ? C41 C42 H057 121.3 . . ? C43 C42 H057 121.3 . . ? C44 C43 C42 123.1(8) . . ? C44 C43 C61 122.8(7) . . ? C42 C43 C61 114.1(8) . . ? O6 C44 C43 125.0(7) . . ? O6 C44 C39 116.8(7) . . ? C43 C44 C39 118.2(7) . . ? C50 C45 C62 119.2(7) . . ? C50 C45 C46 118.9(7) . . ? C62 C45 C46 121.9(7) . . ? O4 C46 C47 121.3(7) . . ? O4 C46 C45 121.5(7) . . ? C47 C46 C45 117.2(7) . . ? C48 C47 O5 123.8(7) . . ? C48 C47 C46 123.0(8) . . ? O5 C47 C46 113.2(7) . . ? C47 C48 C49 119.5(8) . . ? C47 C48 H559 120.2 . . ? C49 C48 H559 120.2 . . ? C50 C49 C48 120.2(8) . . ? C50 C49 H066 119.9 . . ? C48 C49 H066 119.9 . . ? C49 C50 C45 121.2(8) . . ? C49 C50 H044 119.4 . . ? C45 C50 H044 119.4 . . ? N12 C51 C52 124.8(11) . . ? N12 C51 H565 117.6 . . ? C52 C51 H565 117.6 . . ? C53 C52 C51 116.8(13) . . ? C53 C52 H36 121.6 . . ? C51 C52 H36 121.6 . . ? C54 C53 C52 120.8(12) . . ? C54 C53 H049 119.6 . . ? C52 C53 H049 119.6 . . ? C53 C54 C55 117.7(12) . . ? C53 C54 H56 121.2 . . ? C55 C54 H56 121.2 . . ? N12 C55 C54 123.8(12) . . ? N12 C55 H669 118.1 . . ? C54 C55 H669 118.1 . . ? N11 C56 C57 122.4(9) . . ? N11 C56 H046 118.8 . . ? C57 C56 H046 118.8 . . ? C58 C57 C56 120.1(10) . . ? C58 C57 H035 119.9 . . ? C56 C57 H035 119.9 . . ? C57 C58 C59 118.3(10) . . ? C57 C58 H121 120.8 . . ? C59 C58 H121 120.8 . . ? C58 C59 C363 119.1(10) . . ? C58 C59 H232 120.5 . . ? C363 C59 H232 120.5 . . ? N10 C61 C43 124.1(7) . . ? N10 C61 H080 118.0 . . ? C43 C61 H080 118.0 . . ? N9 C62 C45 128.4(7) . . ? N9 C62 H059 115.8 . . ? C45 C62 H059 115.8 . . ? O10 C63 H99A 109.5 . . ? O10 C63 H99B 109.5 . . ? H99A C63 H99B 109.5 . . ? O10 C63 H99C 109.5 . . ? H99A C63 H99C 109.5 . . ? H99B C63 H99C 109.5 . . ? O8 C64 C65 106.8(15) . . ? O8 C64 H66A 110.4 . . ? C65 C64 H66A 110.4 . . ? O8 C64 H66B 110.4 . . ? C65 C64 H66B 110.4 . . ? H66A C64 H66B 108.6 . . ? C64 C65 C67 101.6(15) . . ? C64 C65 H55A 111.5 . . ? C67 C65 H55A 111.5 . . ? C64 C65 H55B 111.5 . . ? C67 C65 H55B 111.5 . . ? H55A C65 H55B 109.3 . . ? C68 C67 C65 109.3(15) . . ? C68 C67 H36A 109.8 . . ? C65 C67 H36A 109.8 . . ? C68 C67 H36B 109.8 . . ? C65 C67 H36B 109.8 . . ? H36A C67 H36B 108.3 . . ? C67 C68 O8 110.8(16) . . ? C67 C68 H96A 109.5 . . ? O8 C68 H96A 109.5 . . ? C67 C68 H96B 109.5 . . ? O8 C68 H96B 109.5 . . ? H96A C68 H96B 108.1 . . ? O7 C69 H45A 109.5 . . ? O7 C69 H45B 109.5 . . ? H45A C69 H45B 109.5 . . ? O7 C69 H45C 109.5 . . ? H45A C69 H45C 109.5 . . ? H45B C69 H45C 109.5 . . ? O5 C71 H65A 109.5 . . ? O5 C71 H65B 109.5 . . ? H65A C71 H65B 109.5 . . ? O5 C71 H65C 109.5 . . ? H65A C71 H65C 109.5 . . ? H65B C71 H65C 109.5 . . ? N11 C363 C59 123.4(10) . . ? N11 C363 H363 118.3 . . ? C59 C363 H363 118.3 . . ? C27 N1 C28 123.5(6) . . ? C26 N2 C25 124.2(6) . . ? C32 N3 C31 122.6(7) . . ? C29 N4 C30 124.1(6) . . ? C32 N5 C25 107.4(6) . . ? C32 N5 Tb1 122.4(4) . . ? C25 N5 Tb1 123.3(4) . . ? C27 N6 C26 108.0(6) . . ? C27 N6 Tb1 123.7(4) . . ? C26 N6 Tb1 122.7(5) . . ? C28 N7 C29 109.7(6) . . ? C28 N7 Tb1 122.2(5) . . ? C29 N7 Tb1 123.0(5) . . ? C31 N8 C30 108.1(6) . . ? C31 N8 Tb1 123.3(5) . . ? C30 N8 Tb1 121.8(5) . . ? C62 N9 C37 121.3(6) . . ? C62 N9 Tb1 124.5(5) . . ? C37 N9 Tb1 114.1(5) . . ? C61 N10 C36 118.2(7) . . ? C61 N10 Tb1 126.8(5) . . ? C36 N10 Tb1 114.8(4) . . ? C363 N11 C56 116.7(8) . . ? C363 N11 Zn1 123.2(6) . . ? C56 N11 Zn1 120.0(6) . . ? C55 N12 C51 116.0(9) . . ? C55 N12 Zn1 124.2(8) . . ? C51 N12 Zn1 119.6(7) . . ? O1 N13 O2 125.1(13) . . ? O1 N13 O3 117.4(10) . . ? O2 N13 O3 117.5(12) . . ? N13 O3 Zn1 105.1(6) . . ? C46 O4 Zn1 124.4(4) . . ? C46 O4 Tb1 126.4(4) . . ? Zn1 O4 Tb1 105.1(2) . . ? C47 O5 C71 117.6(6) . . ? C44 O6 Zn1 125.2(4) . . ? C44 O6 Tb1 124.8(4) . . ? Zn1 O6 Tb1 104.84(19) . . ? C39 O7 C69 117.3(7) . . ? C68 O8 C64 107.7(17) . . ? C63 O10 H555 109.5 . . ? N11 Zn1 O4 102.2(2) . . ? N11 Zn1 O6 107.7(2) . . ? O4 Zn1 O6 77.96(19) . . ? N11 Zn1 N12 99.1(3) . . ? O4 Zn1 N12 158.0(3) . . ? O6 Zn1 N12 90.4(2) . . ? N11 Zn1 O3 92.1(3) . . ? O4 Zn1 O3 90.5(2) . . ? O6 Zn1 O3 158.7(2) . . ? N12 Zn1 O3 94.3(3) . . ? N11 Zn1 Tb1 117.77(19) . . ? O4 Zn1 Tb1 39.64(14) . . ? O6 Zn1 Tb1 39.85(12) . . ? N12 Zn1 Tb1 123.2(2) . . ? O3 Zn1 Tb1 123.47(16) . . ? O4 Tb1 O6 69.23(17) . . ? O4 Tb1 N8 145.63(19) . . ? O6 Tb1 N8 83.26(18) . . ? O4 Tb1 N6 83.97(18) . . ? O6 Tb1 N6 145.77(19) . . ? N8 Tb1 N6 111.16(19) . . ? O4 Tb1 N5 143.81(18) . . ? O6 Tb1 N5 141.99(18) . . ? N8 Tb1 N5 69.92(19) . . ? N6 Tb1 N5 71.3(2) . . ? O4 Tb1 N7 86.00(19) . . ? O6 Tb1 N7 86.28(18) . . ? N8 Tb1 N7 71.6(2) . . ? N6 Tb1 N7 70.49(19) . . ? N5 Tb1 N7 108.95(19) . . ? O4 Tb1 N9 71.94(19) . . ? O6 Tb1 N9 107.11(18) . . ? N8 Tb1 N9 138.3(2) . . ? N6 Tb1 N9 83.07(19) . . ? N5 Tb1 N9 79.03(19) . . ? N7 Tb1 N9 147.2(2) . . ? O4 Tb1 N10 106.16(18) . . ? O6 Tb1 N10 71.45(18) . . ? N8 Tb1 N10 82.96(19) . . ? N6 Tb1 N10 138.9(2) . . ? N5 Tb1 N10 78.76(19) . . ? N7 Tb1 N10 148.02(19) . . ? N9 Tb1 N10 63.79(19) . . ? O4 Tb1 Zn1 35.22(12) . . ? O6 Tb1 Zn1 35.32(13) . . ? N8 Tb1 Zn1 118.17(13) . . ? N6 Tb1 Zn1 118.71(14) . . ? N5 Tb1 Zn1 158.52(14) . . ? N7 Tb1 Zn1 92.51(14) . . ? N9 Tb1 Zn1 83.33(13) . . ? N10 Tb1 Zn1 82.52(14) . . ? C99 O99 H99 109.5 . . ? O99 C99 H99D 109.5 . . ? O99 C99 H99E 109.5 . . ? H99D C99 H99E 109.5 . . ? O99 C99 H99F 109.5 . . ? H99D C99 H99F 109.5 . . ? H99E C99 H99F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.573 _refine_diff_density_min -2.235 _refine_diff_density_rms 0.155 #===END _database_code_depnum_ccdc_archive 'CCDC 955773'