# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_address ; Department of chemistry, Moscow State University, 119899, Moscow, Vorobjevy Gory, Russia. Tel: +74959394549 ; _publ_contact_author_email semenov@inorg.chem.msu.ru _publ_contact_author_name 'Sergey Semenov' _publ_section_title ; First direct assembly of molecular helical complexes to coordination polymer ; loop_ _publ_author_name S.Semenov A.Drozdov S.V.Eliseeva F.Marchetti C.Pettinari ; A.Yu.Rogachev ; S.Troyanov data_TbQ2Q _database_code_depnum_ccdc_archive 'CCDC 670980' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Tb2(Q2Q)3(H2O)2 _chemical_melting_point ? _chemical_formula_moiety '[Tb2(C24H20N4O4)3(H2O)2]*7/3(H2O)*1/3(C2H5OH)' _chemical_formula_sum 'C72.67 H70.67 N12 O16.67 Tb2' _chemical_formula_weight 1695.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 17.257(4) _cell_length_b 27.225(5) _cell_length_c 28.140(6) _cell_angle_alpha 115.55(3) _cell_angle_beta 104.56(3) _cell_angle_gamma 97.14(3) _cell_volume 11126(4) _cell_formula_units_Z 6 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2270 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 60.0 _exptl_crystal_description nidles _exptl_crystal_colour colorless _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.513 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5084 _exptl_absorpt_coefficient_mu 1.966 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type IPDS(Stoe) _diffrn_measurement_method '\f oscillation scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 103098 _diffrn_reflns_av_R_equivalents 0.1279 _diffrn_reflns_av_sigmaI/netI 0.1340 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 3.31 _diffrn_reflns_theta_max 28.70 _reflns_number_total 52881 _reflns_number_gt 40004 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The 17 restraints (DELU commands included in SHELXL-97) were used to correct the thermal parameters of the two benzene rings and C145 carbon atom.Hydrogen atoms of the crystal water molecules O43--O50 were not observed nor calculated. Occupancy of water molecule oxygen atom O43 was refined. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0743P)^2^+101.7092P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _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 52881 _refine_ls_number_parameters 2745 _refine_ls_number_restraints 17 _refine_ls_R_factor_all 0.1081 _refine_ls_R_factor_gt 0.0816 _refine_ls_wR_factor_ref 0.2108 _refine_ls_wR_factor_gt 0.2000 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.094 _refine_ls_shift/su_max 0.155 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tb1 Tb -0.00304(2) 0.349232(15) 1.041010(16) 0.01136(8) Uani 1 1 d . . . O1 O 0.0758(4) 0.4305(2) 1.0548(3) 0.0171(13) Uani 1 1 d . . . N1 N 0.1145(5) 0.5270(3) 1.0868(3) 0.0180(16) Uani 1 1 d . . . C1 C 0.0548(6) 0.4762(3) 1.0649(3) 0.0153(17) Uani 1 1 d . . . Tb2 Tb -0.29939(2) 0.382958(16) 1.126659(17) 0.01305(8) Uani 1 1 d . . . O2 O -0.1013(4) 0.3967(2) 1.0227(3) 0.0162(12) Uani 1 1 d . . . N2 N 0.0784(5) 0.5715(3) 1.0950(3) 0.0193(16) Uani 1 1 d . . . C2 C -0.0216(5) 0.4891(3) 1.0578(3) 0.0143(16) Uani 1 1 d . . . Tb3 Tb 0.36898(2) 0.746985(16) 0.620980(16) 0.01226(8) Uani 1 1 d . . . O3 O -0.3982(4) 0.3168(3) 1.0450(3) 0.0191(13) Uani 1 1 d . . . C3 C -0.0998(6) 0.4468(3) 1.0343(3) 0.0153(17) Uani 1 1 d . . . N3 N -0.4444(5) 0.2471(3) 0.9500(3) 0.0163(15) Uani 1 1 d . . . Tb4 Tb 0.70588(2) 0.695505(16) 0.650825(16) 0.01114(8) Uani 1 1 d . . . O4 O -0.2774(4) 0.4052(3) 1.0591(3) 0.0189(13) Uani 1 1 d . . . C4 C -0.0026(6) 0.5489(3) 1.0769(4) 0.0183(18) Uani 1 1 d . . . N4 N -0.4292(5) 0.2395(3) 0.9015(3) 0.0168(15) Uani 1 1 d . . . Tb5 Tb -0.02549(2) 0.053928(16) 0.693374(16) 0.01214(8) Uani 1 1 d . . . O5 O 0.0615(4) 0.3187(3) 1.1006(3) 0.0168(12) Uani 1 1 d . . . N5 N 0.1008(4) 0.3047(3) 1.1784(3) 0.0106(13) Uani 1 1 d . . . C5 C -0.0584(6) 0.5864(4) 1.0793(4) 0.025(2) Uani 1 1 d . . . H5A H -0.0260 0.6251 1.1006 0.038 Uiso 1 1 calc R . . H5B H -0.0968 0.5800 1.0968 0.038 Uiso 1 1 calc R . . H5C H -0.0887 0.5785 1.0420 0.038 Uiso 1 1 calc R . . Tb6 Tb 0.34510(2) 0.135188(16) 0.750464(16) 0.01132(8) Uani 1 1 d . . . O6 O -0.0040(4) 0.4124(3) 1.1294(2) 0.0157(12) Uani 1 1 d . . . N6 N 0.0997(4) 0.3291(3) 1.2328(3) 0.0138(14) Uani 1 1 d . . . C6 C 0.2014(6) 0.5373(4) 1.1066(4) 0.0189(18) Uani 1 1 d . . . O7 O -0.3116(4) 0.4724(3) 1.1752(3) 0.0194(13) Uani 1 1 d . . . N7 N -0.2744(5) 0.5707(3) 1.2277(4) 0.0221(17) Uani 1 1 d . . . C7 C 0.2493(6) 0.5898(4) 1.1526(4) 0.025(2) Uani 1 1 d . . . H7A H 0.2240 0.6180 1.1686 0.030 Uiso 1 1 calc R . . O8 O -0.1638(4) 0.4407(2) 1.1671(3) 0.0174(13) Uani 1 1 d . . . N8 N -0.2064(5) 0.6165(3) 1.2506(4) 0.0248(18) Uani 1 1 d . . . C8 C 0.3340(7) 0.5992(4) 1.1739(4) 0.029(2) Uani 1 1 d . . . H8B H 0.3656 0.6335 1.2050 0.035 Uiso 1 1 calc R . . O9 O -0.0704(4) 0.2938(2) 0.9460(3) 0.0168(13) Uani 1 1 d . . . N9 N -0.1747(4) 0.2276(3) 0.8623(3) 0.0150(14) Uani 1 1 d . . . C9 C 0.3731(6) 0.5583(5) 1.1495(5) 0.033(3) Uani 1 1 d . . . H9A H 0.4303 0.5648 1.1644 0.039 Uiso 1 1 calc R . . O10 O -0.1133(4) 0.2846(3) 1.0332(3) 0.0174(13) Uani 1 1 d . . . N10 N -0.2437(4) 0.1839(3) 0.8434(3) 0.0177(15) Uani 1 1 d . . . C10 C 0.3259(6) 0.5080(5) 1.1032(5) 0.026(2) Uani 1 1 d . . . H10B H 0.3521 0.4812 1.0857 0.031 Uiso 1 1 calc R . . O11 O -0.2499(4) 0.3706(3) 1.2027(3) 0.0171(12) Uani 1 1 d . . . N11 N -0.1647(4) 0.3462(3) 1.2621(3) 0.0153(14) Uani 1 1 d . . . C11 C 0.2399(6) 0.4961(4) 1.0816(4) 0.0207(19) Uani 1 1 d . . . H11A H 0.2087 0.4612 1.0511 0.025 Uiso 1 1 calc R . . O12 O -0.2420(4) 0.3063(3) 1.0941(3) 0.0192(13) Uani 1 1 d . . . N12 N -0.1178(5) 0.3074(3) 1.2581(3) 0.0181(15) Uani 1 1 d . . . C12 C -0.1810(5) 0.4615(3) 1.0227(4) 0.0138(16) Uani 1 1 d . . . H12B H -0.1771 0.4876 1.0080 0.017 Uiso 1 1 calc R . . H12C H -0.1915 0.4804 1.0577 0.017 Uiso 1 1 calc R . . O13 O 0.1050(4) 0.3208(3) 1.0093(3) 0.0217(14) Uani 1 1 d . . . N13 N 0.3735(4) 0.7060(3) 0.7587(3) 0.0122(13) Uani 1 1 d . . . C13 C -0.2536(5) 0.4100(4) 0.9814(4) 0.0178(18) Uani 1 1 d . . . H13B H -0.2957 0.4217 0.9618 0.021 Uiso 1 1 calc R . . H13C H -0.2344 0.3833 0.9539 0.021 Uiso 1 1 calc R . . O14 O -0.4181(4) 0.3660(3) 1.1508(3) 0.0202(13) Uani 1 1 d . . . N14 N 0.4072(4) 0.6655(3) 0.7687(3) 0.0133(14) Uani 1 1 d . . . C14 C -0.2931(5) 0.3802(3) 1.0074(3) 0.0125(15) Uani 1 1 d . . . O15 O 0.3405(4) 0.7299(3) 0.6878(3) 0.0171(13) Uani 1 1 d . . . N15 N 0.6486(5) 0.5836(3) 0.4673(3) 0.0203(16) Uani 1 1 d U . . C15 C -0.3485(5) 0.3250(4) 0.9735(4) 0.0158(17) Uani 1 1 d . . . O16 O 0.3912(4) 0.6594(3) 0.6019(3) 0.0160(12) Uani 1 1 d . . . N16 N 0.5716(5) 0.5563(3) 0.4257(3) 0.0201(16) Uani 1 1 d . . . C16 C -0.3957(5) 0.2983(3) 0.9951(4) 0.0137(16) Uani 1 1 d . . . O17 O 0.7071(4) 0.6312(3) 0.5652(3) 0.0184(13) Uani 1 1 d . . . N17 N 0.2268(5) 0.6356(3) 0.4329(3) 0.0198(16) Uani 1 1 d . . . C17 C -0.3735(5) 0.2852(4) 0.9148(4) 0.0169(17) Uani 1 1 d . . . O18 O 0.5739(4) 0.6296(2) 0.6067(2) 0.0157(12) Uani 1 1 d . . . N18 N 0.2563(5) 0.6227(3) 0.3887(3) 0.0213(16) Uani 1 1 d . . . C18 C -0.3474(6) 0.2903(4) 0.8701(4) 0.022(2) Uani 1 1 d . . . H18B H -0.3719 0.2554 0.8356 0.033 Uiso 1 1 calc R . . H18C H -0.2879 0.2985 0.8808 0.033 Uiso 1 1 calc R . . H18D H -0.3654 0.3202 0.8651 0.033 Uiso 1 1 calc R . . O19 O 0.2741(4) 0.6911(3) 0.5304(3) 0.0185(13) Uani 1 1 d . . . N19 N 0.8190(4) 0.8798(3) 0.7012(3) 0.0142(14) Uani 1 1 d . . . C19 C -0.4976(5) 0.2022(4) 0.9502(4) 0.0162(17) Uani 1 1 d . . . O20 O 0.4485(4) 0.7366(2) 0.5631(2) 0.0164(12) Uani 1 1 d . . . N20 N 0.7879(4) 0.9123(3) 0.6771(3) 0.0151(14) Uani 1 1 d . . . C20 C -0.5199(5) 0.1478(3) 0.9053(4) 0.0149(16) Uani 1 1 d . . . H20B H -0.5019 0.1408 0.8750 0.018 Uiso 1 1 calc R . . O21 O 0.6359(4) 0.7272(2) 0.5924(2) 0.0154(12) Uani 1 1 d . . . N21 N 0.5058(5) 0.9212(3) 0.6608(3) 0.0161(15) Uani 1 1 d . . . C21 C -0.5691(5) 0.1040(4) 0.9061(4) 0.0197(18) Uani 1 1 d . . . H21A H -0.5857 0.0678 0.8758 0.024 Uiso 1 1 calc R . . O22 O 0.7830(4) 0.7873(3) 0.6866(3) 0.0158(12) Uani 1 1 d . . . N22 N 0.5836(5) 0.9555(3) 0.7005(3) 0.0183(15) Uani 1 1 d . . . C22 C -0.5941(6) 0.1141(4) 0.9525(4) 0.024(2) Uani 1 1 d . . . H22B H -0.6260 0.0845 0.9534 0.029 Uiso 1 1 calc R . . O23 O 0.4138(4) 0.8363(2) 0.6349(3) 0.0166(13) Uani 1 1 d . . . N23 N 0.6884(4) 0.6340(3) 0.7762(3) 0.0142(14) Uani 1 1 d . . . C23 C -0.5711(6) 0.1677(4) 0.9964(4) 0.0206(19) Uani 1 1 d . . . H23A H -0.5870 0.1743 1.0274 0.025 Uiso 1 1 calc R . . O24 O 0.4930(4) 0.7888(2) 0.6974(3) 0.0168(13) Uani 1 1 d . . . N24 N 0.6594(5) 0.6569(3) 0.8209(3) 0.0178(15) Uani 1 1 d . . . C24 C -0.5241(5) 0.2128(4) 0.9955(4) 0.0173(17) Uani 1 1 d . . . H24B H -0.5109 0.2494 1.0249 0.021 Uiso 1 1 calc R . . O25 O 0.7095(3) 0.6538(2) 0.7071(2) 0.0131(11) Uani 1 1 d . . . N25 N 0.0168(5) 0.1826(3) 0.8731(3) 0.0163(15) Uani 1 1 d . . . C25 C 0.0676(5) 0.3324(3) 1.1500(3) 0.0124(16) Uani 1 1 d . . . O26 O 0.6497(4) 0.7478(3) 0.7172(2) 0.0140(12) Uani 1 1 d . . . N26 N 0.0709(5) 0.2372(3) 0.9052(3) 0.0169(15) Uani 1 1 d . . . C26 C 0.0460(5) 0.3766(3) 1.1897(3) 0.0120(15) Uani 1 1 d . . . O27 O 0.2625(4) 0.7908(3) 0.6385(3) 0.0195(13) Uani 1 1 d . . . N27 N 0.3535(5) 0.1952(3) 0.6236(3) 0.0167(15) Uani 1 1 d . . . C27 C 0.0130(5) 0.4175(4) 1.1777(3) 0.0129(16) Uani 1 1 d . . . O28 O 0.8401(4) 0.6873(3) 0.6771(3) 0.0203(14) Uani 1 1 d . . . N28 N 0.3018(5) 0.2237(3) 0.6045(4) 0.0201(16) Uani 1 1 d . . . C28 C 0.0685(5) 0.3719(3) 1.2400(3) 0.0113(15) Uani 1 1 d . . . O29 O -0.0290(4) 0.1094(2) 0.7808(2) 0.0148(12) Uani 1 1 d U . . N29 N -0.0836(5) 0.1294(3) 0.5794(3) 0.0190(16) Uani 1 1 d . . . C29 C 0.0616(5) 0.4081(4) 1.2957(4) 0.0178(17) Uani 1 1 d . . . H29A H 0.0841 0.3947 1.3213 0.027 Uiso 1 1 calc R . . H29B H 0.0043 0.4065 1.2916 0.027 Uiso 1 1 calc R . . H29C H 0.0922 0.4465 1.3101 0.027 Uiso 1 1 calc R . . O30 O 0.0570(4) 0.1438(2) 0.7217(3) 0.0153(12) Uani 1 1 d . . . C30 C 0.1296(5) 0.2553(4) 1.1561(3) 0.0136(16) Uani 1 1 d . . . N30 N -0.0357(5) 0.1378(3) 0.5487(4) 0.0237(17) Uani 1 1 d . . . O31 O 0.3741(4) 0.1622(3) 0.6882(3) 0.0164(12) Uani 1 1 d . . . N31 N 0.3433(5) -0.0451(3) 0.7153(3) 0.0145(14) Uani 1 1 d . . . C31 C 0.1325(5) 0.2221(4) 1.1827(4) 0.0168(17) Uani 1 1 d . . . H31A H 0.1167 0.2323 1.2142 0.020 Uiso 1 1 calc R . . O32 O 0.2455(3) 0.1824(2) 0.7367(2) 0.0121(11) Uani 1 1 d . . . N32 N 0.2839(4) -0.0948(3) 0.6743(3) 0.0147(14) Uani 1 1 d . . . C32 C 0.1596(6) 0.1734(4) 1.1610(4) 0.023(2) Uani 1 1 d . . . H32B H 0.1629 0.1515 1.1788 0.028 Uiso 1 1 calc R . . O33 O -0.0916(4) 0.0801(3) 0.6291(3) 0.0201(13) Uani 1 1 d . . . N33 N -0.0140(4) -0.1261(3) 0.6496(3) 0.0155(14) Uani 1 1 d . . . C33 C 0.1815(6) 0.1573(4) 1.1138(4) 0.0206(19) Uani 1 1 d . . . H33A H 0.1982 0.1243 1.0992 0.025 Uiso 1 1 calc R . . O34 O 0.0451(4) 0.0306(2) 0.6289(2) 0.0140(12) Uani 1 1 d . . . N34 N 0.0469(5) -0.1446(3) 0.6747(3) 0.0189(16) Uani 1 1 d . . . C34 C 0.1784(5) 0.1913(4) 1.0881(4) 0.0212(19) Uani 1 1 d . . . H34B H 0.1933 0.1806 1.0562 0.025 Uiso 1 1 calc R . . O35 O 0.3735(4) 0.0518(2) 0.7410(2) 0.0136(12) Uani 1 1 d . . . C35 C 0.1539(5) 0.2398(4) 1.1086(4) 0.0167(17) Uani 1 1 d . . . H35A H 0.1532 0.2623 1.0914 0.020 Uiso 1 1 calc R . . N35 N 0.3667(5) 0.2761(3) 0.9217(3) 0.0173(15) Uani 1 1 d . . . O36 O 0.2471(4) 0.0653(2) 0.6656(3) 0.0148(8) Uani 1 1 d . . . C36 C 0.0043(5) 0.4687(4) 1.2242(4) 0.0177(17) Uani 1 1 d . . . H36A H 0.0590 0.4901 1.2519 0.021 Uiso 1 1 calc R . . H36B H -0.0287 0.4562 1.2422 0.021 Uiso 1 1 calc R . . N36 N 0.3274(5) 0.2736(3) 0.9587(3) 0.0208(16) Uani 1 1 d . . . O37 O -0.0435(3) -0.0411(2) 0.6617(2) 0.0113(11) Uani 1 1 d . . . C37 C -0.0348(6) 0.5077(4) 1.2070(4) 0.0197(18) Uani 1 1 d . . . H37A H -0.0208 0.5065 1.1753 0.024 Uiso 1 1 calc R . . H37B H -0.0119 0.5461 1.2377 0.024 Uiso 1 1 calc R . . O38 O 0.0868(4) 0.0475(2) 0.7532(3) 0.0163(13) Uani 1 1 d . . . C38 C -0.1288(6) 0.4921(3) 1.1912(3) 0.0159(17) Uani 1 1 d . . . O39 O 0.3772(4) 0.2144(2) 0.8362(3) 0.0148(8) Uani 1 1 d . . . C39 C -0.1712(5) 0.5345(3) 1.2077(4) 0.0161(17) Uani 1 1 d . . . O40 O 0.2702(4) 0.1082(2) 0.7970(3) 0.0156(12) Uani 1 1 d . . . C40 C -0.2577(6) 0.5203(4) 1.2007(4) 0.0178(17) Uani 1 1 d . . . O41 O -0.1611(4) 0.0171(3) 0.6860(3) 0.0206(14) Uani 1 1 d . . . C41 C -0.1457(6) 0.5946(4) 1.2391(4) 0.023(2) Uani 1 1 d . . . O42 O 0.4898(4) 0.1627(3) 0.7892(3) 0.0211(13) Uani 1 1 d . . . C42 C -0.0613(7) 0.6347(4) 1.2581(5) 0.034(3) Uani 1 1 d . . . H42B H -0.0650 0.6729 1.2753 0.050 Uiso 1 1 calc R . . H42C H -0.0441 0.6273 1.2264 0.050 Uiso 1 1 calc R . . H42D H -0.0215 0.6291 1.2847 0.050 Uiso 1 1 calc R . . C43 C -0.3467(6) 0.5812(4) 1.2416(4) 0.026(2) Uani 1 1 d . . . O43 O 0.0041(10) 0.7649(9) 0.4850(9) 0.078(9) Uani 0.63(4) 1 d P . . O44 O 0.0949(7) 0.7035(4) 0.5207(4) 0.052(2) Uani 1 1 d . . . C44 C -0.3982(7) 0.5408(5) 1.2465(5) 0.031(2) Uani 1 1 d . . . H44A H -0.3879 0.5058 1.2379 0.037 Uiso 1 1 calc R . . O45 O 0.0972(4) 0.7549(3) 0.6271(4) 0.0305(17) Uani 1 1 d . . . C45 C -0.4657(7) 0.5536(6) 1.2644(5) 0.039(3) Uani 1 1 d . . . H45A H -0.5015 0.5267 1.2664 0.047 Uiso 1 1 calc R . . O46 O 0.2958(5) 0.9536(3) 1.2878(4) 0.041(2) Uani 1 1 d . . . C46 C -0.4785(7) 0.6072(6) 1.2791(5) 0.036(3) Uani 1 1 d . . . H46A H -0.5217 0.6164 1.2924 0.043 Uiso 1 1 calc R . . O47 O -0.6200(4) 0.8610(3) 1.2531(3) 0.0249(15) Uani 1 1 d . . . H47A H -0.5806 0.8529 1.2430 0.037 Uiso 1 1 calc R . . C47 C -0.4278(7) 0.6461(5) 1.2741(5) 0.0377(19) Uani 1 1 d . . . H47B H -0.4364 0.6819 1.2847 0.045 Uiso 1 1 calc R . . O48 O -0.2767(4) 0.6424(3) 0.9613(3) 0.0306(17) Uani 1 1 d . . . C48 C -0.3638(7) 0.6331(5) 1.2535(5) 0.0377(19) Uani 1 1 d . . . H48A H -0.3324 0.6589 1.2476 0.045 Uiso 1 1 calc R . . O49 O 0.9877(5) 0.6967(4) 0.6592(4) 0.042(2) Uani 1 1 d . . . C49 C -0.1380(5) 0.2550(3) 0.9190(4) 0.0144(16) Uani 1 1 d . . . O50 O 0.5708(4) 0.5975(3) 0.8595(3) 0.0250(15) Uani 1 1 d . . . C50 C -0.1889(5) 0.2271(4) 0.9378(4) 0.0156(16) Uani 1 1 d . . . C51 C -0.1721(5) 0.2431(3) 0.9951(4) 0.0139(16) Uani 1 1 d . . . C52 C -0.2522(5) 0.1832(3) 0.8883(4) 0.0137(16) Uani 1 1 d . . . C53 C -0.3229(6) 0.1392(4) 0.8812(4) 0.023(2) Uani 1 1 d . . . H53A H -0.3577 0.1182 0.8425 0.035 Uiso 1 1 calc R . . H53B H -0.3550 0.1574 0.9035 0.035 Uiso 1 1 calc R . . H53C H -0.3011 0.1140 0.8930 0.035 Uiso 1 1 calc R . . C54 C -0.1484(5) 0.2364(4) 0.8219(4) 0.0175(17) Uani 1 1 d . . . C55 C -0.1465(5) 0.1912(4) 0.7751(4) 0.0168(17) Uani 1 1 d . . . H55A H -0.1613 0.1549 0.7704 0.020 Uiso 1 1 calc R . . C56 C -0.1225(6) 0.1991(4) 0.7346(4) 0.025(2) Uani 1 1 d . . . H56A H -0.1232 0.1683 0.7023 0.030 Uiso 1 1 calc R . . C57 C -0.0974(6) 0.2541(4) 0.7434(4) 0.026(2) Uani 1 1 d . . . H57A H -0.0795 0.2600 0.7173 0.032 Uiso 1 1 calc R . . C58 C -0.0989(7) 0.3002(4) 0.7914(4) 0.025(2) Uani 1 1 d . . . H58A H -0.0831 0.3366 0.7965 0.031 Uiso 1 1 calc R . . C59 C -0.1244(6) 0.2920(4) 0.8320(4) 0.0213(19) Uani 1 1 d . . . H59A H -0.1251 0.3223 0.8641 0.026 Uiso 1 1 calc R . . C60 C -0.2231(6) 0.2102(4) 1.0139(4) 0.0201(19) Uani 1 1 d . . . H60A H -0.2785 0.2156 1.0065 0.024 Uiso 1 1 calc R . . H60B H -0.2281 0.1703 0.9919 0.024 Uiso 1 1 calc R . . C61 C -0.1860(6) 0.2276(4) 1.0748(4) 0.0175(17) Uani 1 1 d . . . H61A H -0.2078 0.1969 1.0807 0.021 Uiso 1 1 calc R . . H61B H -0.1265 0.2328 1.0841 0.021 Uiso 1 1 calc R . . C62 C -0.2016(5) 0.2802(4) 1.1142(4) 0.0169(17) Uani 1 1 d . . . C63 C -0.1728(5) 0.2993(4) 1.1729(4) 0.0161(17) Uani 1 1 d . . . C64 C -0.2000(5) 0.3415(4) 1.2102(4) 0.0183(18) Uani 1 1 d . . . C65 C -0.1238(5) 0.2793(4) 1.2051(4) 0.0172(17) Uani 1 1 d . . . C66 C -0.0803(6) 0.2341(4) 1.1891(4) 0.0228(19) Uani 1 1 d . . . H66A H -0.0531 0.2310 1.2215 0.034 Uiso 1 1 calc R . . H66B H -0.0398 0.2432 1.1742 0.034 Uiso 1 1 calc R . . H66C H -0.1199 0.1988 1.1613 0.034 Uiso 1 1 calc R . . C67 C -0.1777(5) 0.3789(3) 1.3134(3) 0.0149(16) Uani 1 1 d . . . C68 C -0.2061(5) 0.4265(4) 1.3230(4) 0.0173(17) Uani 1 1 d . . . H68A H -0.2179 0.4373 1.2954 0.021 Uiso 1 1 calc R . . C69 C -0.2170(5) 0.4581(4) 1.3739(4) 0.0212(19) Uani 1 1 d . . . H69A H -0.2371 0.4897 1.3802 0.025 Uiso 1 1 calc R . . C70 C -0.1977(6) 0.4420(4) 1.4152(4) 0.027(2) Uani 1 1 d . . . H70A H -0.2028 0.4637 1.4498 0.032 Uiso 1 1 calc R . . C71 C -0.1713(6) 0.3948(5) 1.4050(4) 0.026(2) Uani 1 1 d . . . H71A H -0.1607 0.3837 1.4324 0.032 Uiso 1 1 calc R . . C72 C -0.1598(6) 0.3623(5) 1.3543(4) 0.026(2) Uani 1 1 d . . . H72A H -0.1406 0.3303 1.3481 0.031 Uiso 1 1 calc R . . C73 C 0.3702(5) 0.6984(3) 0.7073(4) 0.0163(17) Uani 1 1 d . . . C74 C 0.4023(5) 0.6526(3) 0.6822(4) 0.0142(16) Uani 1 1 d U . . C75 C 0.4060(5) 0.6309(4) 0.6277(4) 0.0155(16) Uani 1 1 d U . . C76 C 0.4223(5) 0.6335(3) 0.7231(4) 0.0142(16) Uani 1 1 d U . . C77 C 0.4569(6) 0.5844(4) 0.7188(4) 0.0222(19) Uani 1 1 d U . . H77A H 0.4588 0.5796 0.7509 0.033 Uiso 1 1 calc R . . H77B H 0.5119 0.5914 0.7174 0.033 Uiso 1 1 calc R . . H77C H 0.4220 0.5507 0.6854 0.033 Uiso 1 1 calc R . . C78 C 0.3575(5) 0.7502(4) 0.8020(4) 0.0154(16) Uani 1 1 d U . . C79 C 0.3070(6) 0.7820(4) 0.7890(4) 0.0188(18) Uani 1 1 d U . . H79A H 0.2816 0.7734 0.7521 0.023 Uiso 1 1 calc R . . C80 C 0.2954(6) 0.8276(4) 0.8334(4) 0.0213(19) Uani 1 1 d . . . H80A H 0.2614 0.8488 0.8252 0.026 Uiso 1 1 calc R . . C81 C 0.3327(6) 0.8414(4) 0.8883(4) 0.0222(19) Uani 1 1 d . . . H81A H 0.3271 0.8731 0.9171 0.027 Uiso 1 1 calc R . . C82 C 0.3791(6) 0.8071(4) 0.9002(4) 0.024(2) Uani 1 1 d . . . H82A H 0.4012 0.8144 0.9371 0.029 Uiso 1 1 calc R . . C83 C 0.3927(6) 0.7626(4) 0.8580(4) 0.0206(18) Uani 1 1 d . . . H83A H 0.4251 0.7407 0.8666 0.025 Uiso 1 1 calc R . . C84 C 0.4229(5) 0.5755(4) 0.5977(4) 0.0184(18) Uani 1 1 d . . . H84A H 0.3752 0.5456 0.5879 0.022 Uiso 1 1 calc R . . H84B H 0.4700 0.5727 0.6229 0.022 Uiso 1 1 calc R . . C85 C 0.4411(5) 0.5659(3) 0.5450(4) 0.0148(16) Uani 1 1 d . . . H85A H 0.4329 0.5258 0.5216 0.018 Uiso 1 1 calc R . . H85B H 0.4021 0.5784 0.5242 0.018 Uiso 1 1 calc R . . C86 C 0.5279(5) 0.5967(3) 0.5571(4) 0.0160(17) Uani 1 1 d . . . C87 C 0.5584(5) 0.5866(3) 0.5115(4) 0.0161(17) Uani 1 1 d . . . C88 C 0.6448(6) 0.6039(3) 0.5206(3) 0.0157(17) Uani 1 1 d . . . C89 C 0.5188(6) 0.5573(3) 0.4526(4) 0.0195(19) Uani 1 1 d . . . C90 C 0.4278(6) 0.5292(4) 0.4176(4) 0.028(2) Uani 1 1 d . . . H90A H 0.4217 0.5116 0.3786 0.043 Uiso 1 1 calc R . . H90B H 0.3970 0.5571 0.4255 0.043 Uiso 1 1 calc R . . H90C H 0.4071 0.5011 0.4266 0.043 Uiso 1 1 calc R . . C91 C 0.7206(8) 0.5916(4) 0.4527(5) 0.0332(16) Uani 1 1 d U . . C92 C 0.7994(7) 0.5955(4) 0.4852(5) 0.032(2) Uani 1 1 d U . . H92A H 0.8061 0.5914 0.5170 0.038 Uiso 1 1 calc R . . C93 C 0.8668(8) 0.6055(5) 0.4700(6) 0.037(3) Uani 1 1 d U . . H93A H 0.9191 0.6076 0.4914 0.045 Uiso 1 1 calc R . . C94 C 0.8574(8) 0.6125(4) 0.4216(5) 0.0332(16) Uani 1 1 d . . . H94A H 0.9034 0.6212 0.4123 0.040 Uiso 1 1 calc R . . C95 C 0.7805(9) 0.6063(5) 0.3899(5) 0.039(3) Uani 1 1 d U . . H95A H 0.7736 0.6092 0.3575 0.047 Uiso 1 1 calc R . . C96 C 0.7106(8) 0.5955(4) 0.4038(5) 0.031(2) Uani 1 1 d U . . H96A H 0.6581 0.5910 0.3808 0.037 Uiso 1 1 calc R . . C97 C 0.2869(5) 0.6710(4) 0.4834(4) 0.0162(17) Uani 1 1 d . . . C98 C 0.3602(5) 0.6795(3) 0.4705(4) 0.0143(12) Uani 1 1 d . . . C99 C 0.4408(5) 0.7118(3) 0.5129(4) 0.0143(12) Uani 1 1 d . . . C100 C 0.3352(6) 0.6492(4) 0.4112(4) 0.0202(18) Uani 1 1 d . . . C101 C 0.3827(6) 0.6420(4) 0.3720(4) 0.027(2) Uani 1 1 d . . . H10C H 0.3452 0.6208 0.3341 0.040 Uiso 1 1 calc R . . H10D H 0.4232 0.6222 0.3781 0.040 Uiso 1 1 calc R . . H10E H 0.4103 0.6785 0.3788 0.040 Uiso 1 1 calc R . . C102 C 0.1484(5) 0.6009(4) 0.4213(4) 0.0213(19) Uani 1 1 d . . . C103 C 0.0810(6) 0.5894(5) 0.3770(4) 0.030(2) Uani 1 1 d . . . H10F H 0.0851 0.6063 0.3549 0.036 Uiso 1 1 calc R . . C104 C 0.0065(7) 0.5530(6) 0.3644(5) 0.043(3) Uani 1 1 d . . . H10G H -0.0389 0.5455 0.3338 0.052 Uiso 1 1 calc R . . C105 C -0.0011(7) 0.5278(6) 0.3967(5) 0.048(4) Uani 1 1 d . . . H10H H -0.0520 0.5046 0.3891 0.058 Uiso 1 1 calc R . . C106 C 0.0688(7) 0.5373(6) 0.4416(5) 0.046(4) Uani 1 1 d . . . H10I H 0.0653 0.5186 0.4623 0.055 Uiso 1 1 calc R . . C107 C 0.1429(7) 0.5746(5) 0.4546(5) 0.032(2) Uani 1 1 d . . . H10J H 0.1887 0.5824 0.4851 0.038 Uiso 1 1 calc R . . C108 C 0.5176(5) 0.7144(4) 0.4976(4) 0.0174(18) Uani 1 1 d . . . H10K H 0.5034 0.7095 0.4600 0.021 Uiso 1 1 calc R . . H10L H 0.5406 0.6838 0.4980 0.021 Uiso 1 1 calc R . . C109 C 0.5822(5) 0.7705(4) 0.5381(4) 0.0165(17) Uani 1 1 d . . . H10M H 0.6142 0.7798 0.5179 0.020 Uiso 1 1 calc R . . H10N H 0.5536 0.7996 0.5510 0.020 Uiso 1 1 calc R . . C110 C 0.6418(5) 0.7722(3) 0.5888(4) 0.0136(16) Uani 1 1 d . . . C111 C 0.7033(5) 0.8225(3) 0.6297(4) 0.0143(16) Uani 1 1 d . . . C112 C 0.7687(5) 0.8250(4) 0.6729(4) 0.0130(16) Uani 1 1 d . . . C113 C 0.7208(5) 0.8784(4) 0.6353(4) 0.0172(12) Uani 1 1 d . . . C114 C 0.6735(5) 0.8998(4) 0.5993(4) 0.0172(12) Uani 1 1 d . . . H11B H 0.7000 0.9389 0.6136 0.026 Uiso 1 1 calc R . . H11C H 0.6177 0.8958 0.5996 0.026 Uiso 1 1 calc R . . H11D H 0.6727 0.8783 0.5616 0.026 Uiso 1 1 calc R . . C115 C 0.8908(5) 0.9062(4) 0.7496(4) 0.0167(17) Uani 1 1 d . . . C116 C 0.9130(5) 0.9643(4) 0.7835(4) 0.0191(18) Uani 1 1 d . . . H11E H 0.8819 0.9861 0.7736 0.023 Uiso 1 1 calc R . . C117 C 0.9825(6) 0.9903(4) 0.8329(4) 0.0214(19) Uani 1 1 d . . . H11F H 0.9976 1.0292 0.8558 0.026 Uiso 1 1 calc R . . C118 C 1.0286(6) 0.9570(4) 0.8472(4) 0.024(2) Uani 1 1 d . . . H11G H 1.0739 0.9738 0.8803 0.029 Uiso 1 1 calc R . . C119 C 1.0073(6) 0.8992(4) 0.8124(4) 0.0215(19) Uani 1 1 d . . . H11H H 1.0388 0.8774 0.8218 0.026 Uiso 1 1 calc R . . C120 C 0.9392(5) 0.8740(4) 0.7635(4) 0.0164(17) Uani 1 1 d . . . H12D H 0.9257 0.8353 0.7399 0.020 Uiso 1 1 calc R . . C121 C 0.4838(5) 0.8722(3) 0.6642(4) 0.0143(16) Uani 1 1 d . . . C122 C 0.5524(5) 0.8762(3) 0.7070(4) 0.0156(17) Uani 1 1 d . . . C123 C 0.5512(5) 0.8331(3) 0.7244(4) 0.0139(16) Uani 1 1 d . . . C124 C 0.6103(5) 0.9282(4) 0.7276(4) 0.0156(16) Uani 1 1 d . . . C125 C 0.6925(6) 0.9551(4) 0.7727(4) 0.0210(19) Uani 1 1 d . . . H12E H 0.7163 0.9906 0.7758 0.032 Uiso 1 1 calc R . . H12F H 0.7285 0.9308 0.7640 0.032 Uiso 1 1 calc R . . H12G H 0.6860 0.9613 0.8076 0.032 Uiso 1 1 calc R . . C126 C 0.4558(5) 0.9412(4) 0.6289(4) 0.0146(16) Uani 1 1 d . . . C127 C 0.3925(5) 0.9037(4) 0.5791(4) 0.0185(17) Uani 1 1 d . . . H12H H 0.3826 0.8650 0.5661 0.022 Uiso 1 1 calc R . . C128 C 0.3446(6) 0.9244(4) 0.5491(4) 0.024(2) Uani 1 1 d . . . H12I H 0.3017 0.8996 0.5158 0.029 Uiso 1 1 calc R . . C129 C 0.3599(6) 0.9822(4) 0.5684(4) 0.0214(19) Uani 1 1 d . . . H12J H 0.3277 0.9960 0.5477 0.026 Uiso 1 1 calc R . . C130 C 0.4235(6) 1.0195(4) 0.6186(5) 0.027(2) Uani 1 1 d . . . H13D H 0.4335 1.0582 0.6315 0.033 Uiso 1 1 calc R . . C131 C 0.4714(6) 0.9995(4) 0.6492(4) 0.022(2) Uani 1 1 d . . . H13E H 0.5136 1.0244 0.6830 0.027 Uiso 1 1 calc R . . C132 C 0.6154(6) 0.8446(4) 0.7766(4) 0.0181(17) Uani 1 1 d . . . H13F H 0.6145 0.8793 0.8071 0.022 Uiso 1 1 calc R . . H13G H 0.6695 0.8503 0.7726 0.022 Uiso 1 1 calc R . . C133 C 0.6044(5) 0.7980(4) 0.7920(4) 0.0162(17) Uani 1 1 d . . . H13H H 0.6345 0.8132 0.8316 0.019 Uiso 1 1 calc R . . H13I H 0.5461 0.7845 0.7855 0.019 Uiso 1 1 calc R . . C134 C 0.6349(5) 0.7494(3) 0.7590(3) 0.0125(9) Uani 1 1 d . . . C135 C 0.6479(5) 0.7078(3) 0.7753(3) 0.0125(9) Uani 1 1 d . . . C136 C 0.6839(5) 0.6642(3) 0.7477(3) 0.0125(9) Uani 1 1 d . . . C137 C 0.6360(5) 0.7007(4) 0.8210(3) 0.0142(16) Uani 1 1 d . . . C138 C 0.6047(6) 0.7352(4) 0.8653(4) 0.0218(19) Uani 1 1 d . . . H13J H 0.5908 0.7144 0.8836 0.033 Uiso 1 1 calc R . . H13K H 0.5562 0.7439 0.8489 0.033 Uiso 1 1 calc R . . H13L H 0.6469 0.7696 0.8922 0.033 Uiso 1 1 calc R . . C139 C 0.7222(5) 0.5868(4) 0.7678(4) 0.0173(18) Uani 1 1 d . . . C140 C 0.7282(5) 0.5519(4) 0.7160(4) 0.0191(18) Uani 1 1 d . . . H14C H 0.7128 0.5602 0.6868 0.023 Uiso 1 1 calc R . . C141 C 0.7567(6) 0.5055(4) 0.7084(4) 0.025(2) Uani 1 1 d . . . H14D H 0.7607 0.4823 0.6738 0.030 Uiso 1 1 calc R . . C142 C 0.7802(6) 0.4922(4) 0.7524(5) 0.030(2) Uani 1 1 d . . . H14E H 0.7980 0.4599 0.7468 0.036 Uiso 1 1 calc R . . C143 C 0.7761(6) 0.5282(5) 0.8036(5) 0.028(2) Uani 1 1 d . . . H14F H 0.7928 0.5205 0.8332 0.034 Uiso 1 1 calc R . . C144 C 0.7480(6) 0.5752(4) 0.8119(4) 0.024(2) Uani 1 1 d . . . H14G H 0.7461 0.5992 0.8469 0.029 Uiso 1 1 calc R . . C145 C 0.0158(5) 0.1584(3) 0.8188(3) 0.0126(15) Uani 1 1 d U . . C146 C 0.0726(5) 0.1989(3) 0.8159(3) 0.0121(11) Uani 1 1 d . . . C147 C 0.0872(5) 0.1902(3) 0.7659(3) 0.0121(11) Uani 1 1 d . . . C148 C 0.1025(5) 0.2468(3) 0.8707(4) 0.0149(16) Uani 1 1 d . . . C149 C 0.1616(6) 0.3033(4) 0.8930(4) 0.0176(17) Uani 1 1 d . . . H14H H 0.1720 0.3253 0.9324 0.026 Uiso 1 1 calc R . . H14I H 0.1377 0.3226 0.8740 0.026 Uiso 1 1 calc R . . H14J H 0.2130 0.2980 0.8869 0.026 Uiso 1 1 calc R . . C150 C -0.0250(5) 0.1585(4) 0.8980(4) 0.0141(16) Uani 1 1 d . . . C151 C 0.0064(6) 0.1808(4) 0.9569(4) 0.0178(17) Uani 1 1 d . . . H15A H 0.0535 0.2112 0.9785 0.021 Uiso 1 1 calc R . . C152 C -0.0327(6) 0.1574(4) 0.9820(4) 0.023(2) Uani 1 1 d . . . H15B H -0.0121 0.1725 1.0207 0.027 Uiso 1 1 calc R . . C153 C -0.1021(6) 0.1120(4) 0.9509(4) 0.024(2) Uani 1 1 d . . . H15C H -0.1278 0.0961 0.9683 0.028 Uiso 1 1 calc R . . C154 C -0.1331(6) 0.0902(4) 0.8930(4) 0.024(2) Uani 1 1 d . . . H15D H -0.1792 0.0590 0.8717 0.029 Uiso 1 1 calc R . . C155 C -0.0968(5) 0.1141(4) 0.8665(4) 0.0177(18) Uani 1 1 d . . . H15E H -0.1202 0.1005 0.8281 0.021 Uiso 1 1 calc R . . C156 C 0.1336(6) 0.2401(3) 0.7647(4) 0.0156(16) Uani 1 1 d . . . H15F H 0.1869 0.2563 0.7947 0.019 Uiso 1 1 calc R . . H15G H 0.1028 0.2684 0.7727 0.019 Uiso 1 1 calc R . . C157 C 0.1489(5) 0.2284(3) 0.7108(4) 0.0147(16) Uani 1 1 d . . . H15H H 0.0996 0.2022 0.6794 0.018 Uiso 1 1 calc R . . H15I H 0.1586 0.2633 0.7090 0.018 Uiso 1 1 calc R . . C158 C 0.2213(5) 0.2044(3) 0.7055(3) 0.0132(11) Uani 1 1 d . . . C159 C 0.2634(5) 0.2067(3) 0.6692(3) 0.0132(11) Uani 1 1 d . . . C160 C 0.3325(5) 0.1854(4) 0.6635(3) 0.0151(17) Uani 1 1 d . . . C161 C 0.2487(5) 0.2302(3) 0.6315(3) 0.0135(16) Uani 1 1 d . . . C162 C 0.1846(6) 0.2589(4) 0.6199(4) 0.0212(19) Uani 1 1 d . . . H16B H 0.1863 0.2647 0.5888 0.032 Uiso 1 1 calc R . . H16C H 0.1954 0.2948 0.6523 0.032 Uiso 1 1 calc R . . H16D H 0.1308 0.2360 0.6110 0.032 Uiso 1 1 calc R . . C163 C 0.4076(6) 0.1741(4) 0.5950(4) 0.0211(19) Uani 1 1 d . . . C164 C 0.4032(7) 0.1166(5) 0.5724(5) 0.029(2) Uani 1 1 d . . . H16E H 0.3665 0.0932 0.5779 0.035 Uiso 1 1 calc R . . C165 C 0.4539(7) 0.0940(5) 0.5413(5) 0.0294(16) Uani 1 1 d . . . H16F H 0.4517 0.0558 0.5266 0.035 Uiso 1 1 calc R . . C166 C 0.5076(7) 0.1294(5) 0.5327(5) 0.030(2) Uani 1 1 d . . . H16G H 0.5421 0.1149 0.5127 0.037 Uiso 1 1 calc R . . C167 C 0.5098(6) 0.1859(5) 0.5537(5) 0.030(2) Uani 1 1 d . . . H16H H 0.5454 0.2091 0.5474 0.036 Uiso 1 1 calc R . . C168 C 0.4594(7) 0.2083(5) 0.5843(5) 0.0294(16) Uani 1 1 d . . . H16I H 0.4603 0.2462 0.5975 0.035 Uiso 1 1 calc R . . C169 C -0.0567(5) 0.0947(4) 0.6006(4) 0.0156(17) Uani 1 1 d . . . C170 C 0.0109(5) 0.0812(3) 0.5821(3) 0.0135(16) Uani 1 1 d . . . C171 C 0.0569(5) 0.0458(3) 0.5943(4) 0.0156(17) Uani 1 1 d . . . C172 C 0.0193(6) 0.1082(4) 0.5492(4) 0.0209(19) Uani 1 1 d . . . C173 C 0.0776(7) 0.1083(4) 0.5192(4) 0.029(2) Uani 1 1 d . . . H17A H 0.0706 0.1343 0.5048 0.043 Uiso 1 1 calc R . . H17B H 0.0669 0.0711 0.4887 0.043 Uiso 1 1 calc R . . H17C H 0.1335 0.1197 0.5444 0.043 Uiso 1 1 calc R . . C174 C -0.1454(8) 0.1584(5) 0.5875(6) 0.041(2) Uani 1 1 d . . . C175 C -0.2144(6) 0.1373(5) 0.5959(4) 0.029(2) Uani 1 1 d . . . H17D H -0.2210 0.1030 0.5960 0.035 Uiso 1 1 calc R . . C176 C -0.2744(8) 0.1668(6) 0.6042(4) 0.044(3) Uani 1 1 d . . . H17E H -0.3213 0.1527 0.6098 0.053 Uiso 1 1 calc R . . C177 C -0.2621(9) 0.2175(6) 0.6039(6) 0.050(4) Uani 1 1 d . . . H17F H -0.3011 0.2380 0.6103 0.060 Uiso 1 1 calc R . . C178 C -0.1961(8) 0.2388(5) 0.5949(5) 0.041(2) Uani 1 1 d . . . H17G H -0.1903 0.2732 0.5947 0.049 Uiso 1 1 calc R . . C179 C -0.1358(8) 0.2087(5) 0.5857(5) 0.037(3) Uani 1 1 d . . . H17H H -0.0904 0.2223 0.5785 0.045 Uiso 1 1 calc R . . C180 C 0.1200(5) 0.0256(4) 0.5676(4) 0.0138(16) Uani 1 1 d . . . H18E H 0.1654 0.0579 0.5795 0.017 Uiso 1 1 calc R . . H18F H 0.0944 0.0084 0.5272 0.017 Uiso 1 1 calc R . . C181 C 0.1545(5) -0.0165(3) 0.5819(4) 0.0160(16) Uani 1 1 d . . . H18G H 0.1778 -0.0379 0.5539 0.019 Uiso 1 1 calc R . . H18H H 0.1095 -0.0429 0.5805 0.019 Uiso 1 1 calc R . . C182 C 0.2209(5) 0.0113(3) 0.6394(4) 0.0146(16) Uani 1 1 d . . . C183 C 0.2551(5) -0.0215(3) 0.6618(4) 0.0137(16) Uani 1 1 d . . . C184 C 0.3276(5) 0.0015(4) 0.7088(4) 0.0159(17) Uani 1 1 d . . . C185 C 0.2330(5) -0.0812(4) 0.6416(4) 0.0143(16) Uani 1 1 d . . . C186 C 0.1626(6) -0.1269(4) 0.5921(4) 0.0190(18) Uani 1 1 d . . . H18I H 0.1639 -0.1625 0.5911 0.029 Uiso 1 1 calc R . . H18J H 0.1679 -0.1285 0.5584 0.029 Uiso 1 1 calc R . . H18K H 0.1109 -0.1190 0.5952 0.029 Uiso 1 1 calc R . . C187 C 0.4055(5) -0.0443(3) 0.7595(4) 0.0136(16) Uani 1 1 d . . . C188 C 0.3939(5) -0.0905(4) 0.7703(4) 0.0170(17) Uani 1 1 d . . . H18L H 0.3475 -0.1213 0.7478 0.020 Uiso 1 1 calc R . . C189 C 0.4523(6) -0.0889(4) 0.8147(4) 0.024(2) Uani 1 1 d . . . H18M H 0.4443 -0.1186 0.8224 0.029 Uiso 1 1 calc R . . C190 C 0.5231(6) -0.0440(4) 0.8482(4) 0.0226(19) Uani 1 1 d . . . H19A H 0.5621 -0.0435 0.8782 0.027 Uiso 1 1 calc R . . C191 C 0.5343(5) 0.0002(4) 0.8359(4) 0.0179(17) Uani 1 1 d . . . H19B H 0.5808 0.0309 0.8583 0.021 Uiso 1 1 calc R . . C192 C 0.4779(6) -0.0007(4) 0.7914(4) 0.0179(17) Uani 1 1 d . . . H19C H 0.4881 0.0280 0.7825 0.021 Uiso 1 1 calc R . . C193 C 0.0023(5) -0.0680(4) 0.6763(4) 0.0159(17) Uani 1 1 d . . . C194 C 0.0791(5) -0.0488(3) 0.7204(4) 0.0139(16) Uani 1 1 d . . . C195 C 0.1158(5) 0.0094(4) 0.7594(4) 0.0170(17) Uani 1 1 d . . . C196 C 0.1009(6) -0.0990(4) 0.7172(4) 0.0190(18) Uani 1 1 d . . . C197 C 0.1730(6) -0.1042(4) 0.7546(4) 0.0209(19) Uani 1 1 d . . . H19D H 0.1744 -0.1430 0.7392 0.031 Uiso 1 1 calc R . . H19E H 0.1679 -0.0915 0.7909 0.031 Uiso 1 1 calc R . . H19F H 0.2232 -0.0816 0.7578 0.031 Uiso 1 1 calc R . . C198 C -0.0865(6) -0.1665(3) 0.6062(4) 0.0180(17) Uani 1 1 d . . . C199 C -0.1361(5) -0.1545(4) 0.5675(4) 0.0192(18) Uani 1 1 d . . . H19G H -0.1234 -0.1185 0.5712 0.023 Uiso 1 1 calc R . . C200 C -0.2041(6) -0.1955(4) 0.5236(4) 0.023(2) Uani 1 1 d . . . H20C H -0.2371 -0.1873 0.4978 0.028 Uiso 1 1 calc R . . C201 C -0.2229(6) -0.2497(4) 0.5183(4) 0.028(2) Uani 1 1 d . . . H20D H -0.2671 -0.2780 0.4879 0.033 Uiso 1 1 calc R . . C202 C -0.1759(6) -0.2608(4) 0.5580(5) 0.028(2) Uani 1 1 d . . . H20E H -0.1909 -0.2961 0.5555 0.033 Uiso 1 1 calc R . . C203 C -0.1069(6) -0.2205(4) 0.6015(4) 0.0206(18) Uani 1 1 d . . . H20F H -0.0742 -0.2289 0.6273 0.025 Uiso 1 1 calc R . . C204 C 0.1867(6) 0.0272(4) 0.8116(4) 0.0192(18) Uani 1 1 d . . . H20G H 0.2357 0.0201 0.8018 0.023 Uiso 1 1 calc R . . H20H H 0.1740 0.0041 0.8284 0.023 Uiso 1 1 calc R . . C205 C 0.2066(5) 0.0900(4) 0.8553(4) 0.0191(18) Uani 1 1 d . . . H20I H 0.1549 0.1000 0.8568 0.023 Uiso 1 1 calc R . . H20J H 0.2371 0.0953 0.8919 0.023 Uiso 1 1 calc R . . C206 C 0.2567(5) 0.1290(4) 0.8424(4) 0.0147(16) Uani 1 1 d . . . C207 C 0.2901(5) 0.1868(3) 0.8813(4) 0.0117(15) Uani 1 1 d . . . C208 C 0.3469(5) 0.2246(3) 0.8752(3) 0.0110(14) Uani 1 1 d . . . C209 C 0.2841(6) 0.2204(4) 0.9353(4) 0.0185(18) Uani 1 1 d . . . C210 C 0.2362(6) 0.2057(4) 0.9669(4) 0.023(2) Uani 1 1 d . . . H21B H 0.2418 0.2392 1.0004 0.035 Uiso 1 1 calc R . . H21C H 0.2574 0.1790 0.9767 0.035 Uiso 1 1 calc R . . H21D H 0.1786 0.1893 0.9440 0.035 Uiso 1 1 calc R . . C211 C 0.4211(6) 0.3283(4) 0.9371(4) 0.0221(19) Uani 1 1 d . . . C212 C 0.4601(6) 0.3671(4) 0.9930(5) 0.028(2) Uani 1 1 d . . . H21E H 0.4523 0.3585 1.0203 0.034 Uiso 1 1 calc R . . C213 C 0.5120(7) 0.4200(5) 1.0087(6) 0.039(3) Uani 1 1 d . . . H21F H 0.5361 0.4472 1.0462 0.047 Uiso 1 1 calc R . . C214 C 0.5260(7) 0.4303(4) 0.9680(6) 0.040(3) Uani 1 1 d . . . H21G H 0.5606 0.4649 0.9783 0.048 Uiso 1 1 calc R . . C215 C 0.4906(9) 0.3914(5) 0.9126(6) 0.046(3) Uani 1 1 d . . . H21H H 0.5016 0.3994 0.8856 0.055 Uiso 1 1 calc R . . C216 C 0.4370(7) 0.3388(4) 0.8964(5) 0.030(2) Uani 1 1 d . . . H21I H 0.4129 0.3119 0.8588 0.036 Uiso 1 1 calc R . . C217 C -0.6226(8) 0.8456(6) 1.2967(5) 0.040(3) Uani 1 1 d . . . H21J H -0.6753 0.8479 1.3028 0.049 Uiso 1 1 calc R . . H21K H -0.5789 0.8730 1.3315 0.049 Uiso 1 1 calc R . . C218 C -0.6126(16) 0.7874(7) 1.2830(7) 0.091(8) Uani 1 1 d . . . H21L H -0.6229 0.7780 1.3104 0.136 Uiso 1 1 calc R . . H21M H -0.5571 0.7866 1.2832 0.136 Uiso 1 1 calc R . . H21N H -0.6515 0.7605 1.2465 0.136 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 Tb1 0.01534(17) 0.00913(16) 0.01305(17) 0.00794(14) 0.00562(14) 0.00298(14) O1 0.019(3) 0.010(3) 0.025(3) 0.011(2) 0.009(3) 0.005(2) N1 0.023(4) 0.010(3) 0.025(4) 0.013(3) 0.005(3) 0.005(3) C1 0.027(4) 0.013(4) 0.009(3) 0.008(3) 0.007(3) 0.000(3) Tb2 0.01682(17) 0.01092(17) 0.01441(18) 0.00813(14) 0.00663(15) 0.00298(14) O2 0.022(3) 0.011(3) 0.019(3) 0.009(2) 0.010(3) 0.006(2) N2 0.026(4) 0.014(3) 0.024(4) 0.016(3) 0.006(3) 0.007(3) C2 0.024(4) 0.013(4) 0.013(4) 0.009(3) 0.010(3) 0.009(3) Tb3 0.01603(17) 0.01039(16) 0.01383(18) 0.00847(14) 0.00535(15) 0.00420(14) O3 0.019(3) 0.017(3) 0.021(3) 0.009(3) 0.009(3) 0.000(2) C3 0.030(4) 0.010(3) 0.010(4) 0.007(3) 0.007(3) 0.007(3) N3 0.020(3) 0.015(3) 0.021(4) 0.014(3) 0.009(3) 0.006(3) Tb4 0.01420(16) 0.01015(16) 0.01320(17) 0.00875(14) 0.00533(14) 0.00341(13) O4 0.028(3) 0.012(3) 0.014(3) 0.007(2) 0.006(3) 0.000(3) C4 0.025(4) 0.008(3) 0.024(4) 0.012(3) 0.005(4) 0.005(3) N4 0.022(3) 0.015(3) 0.017(3) 0.010(3) 0.009(3) 0.003(3) Tb5 0.01514(17) 0.00951(16) 0.01403(18) 0.00736(14) 0.00585(15) 0.00234(14) O5 0.023(3) 0.019(3) 0.017(3) 0.013(3) 0.010(3) 0.012(3) N5 0.017(3) 0.010(3) 0.014(3) 0.010(3) 0.010(3) 0.006(3) C5 0.021(4) 0.013(4) 0.032(5) 0.010(4) 0.000(4) 0.001(3) Tb6 0.01500(17) 0.00987(16) 0.01364(17) 0.00904(14) 0.00583(14) 0.00333(14) O6 0.020(3) 0.016(3) 0.008(3) 0.005(2) 0.004(2) 0.002(2) N6 0.021(3) 0.013(3) 0.014(3) 0.009(3) 0.010(3) 0.010(3) C6 0.024(4) 0.020(4) 0.021(4) 0.017(4) 0.009(4) 0.002(3) O7 0.021(3) 0.012(3) 0.027(3) 0.010(3) 0.009(3) 0.003(2) N7 0.024(4) 0.015(3) 0.030(4) 0.010(3) 0.013(4) 0.010(3) C7 0.029(5) 0.024(5) 0.027(5) 0.019(4) 0.007(4) 0.000(4) O8 0.023(3) 0.009(3) 0.025(3) 0.009(2) 0.012(3) 0.005(2) N8 0.025(4) 0.012(3) 0.036(5) 0.009(3) 0.012(4) 0.004(3) C8 0.031(5) 0.021(4) 0.027(5) 0.013(4) -0.001(4) -0.006(4) O9 0.018(3) 0.013(3) 0.023(3) 0.012(2) 0.008(3) 0.000(2) N9 0.016(3) 0.011(3) 0.021(4) 0.009(3) 0.009(3) 0.002(3) C9 0.018(4) 0.040(6) 0.049(7) 0.035(6) 0.002(4) 0.004(4) O10 0.024(3) 0.014(3) 0.020(3) 0.012(2) 0.011(3) 0.002(2) N10 0.017(3) 0.017(3) 0.020(4) 0.011(3) 0.006(3) -0.002(3) C10 0.024(4) 0.037(5) 0.038(6) 0.032(5) 0.016(4) 0.011(4) O11 0.022(3) 0.020(3) 0.021(3) 0.016(3) 0.012(3) 0.010(3) N11 0.018(3) 0.019(3) 0.014(3) 0.011(3) 0.005(3) 0.008(3) C11 0.021(4) 0.020(4) 0.032(5) 0.021(4) 0.011(4) 0.003(3) O12 0.026(3) 0.018(3) 0.023(3) 0.014(3) 0.013(3) 0.009(3) N12 0.021(3) 0.017(3) 0.022(4) 0.013(3) 0.009(3) 0.008(3) C12 0.020(4) 0.013(4) 0.019(4) 0.011(3) 0.015(3) 0.008(3) O13 0.023(3) 0.018(3) 0.024(3) 0.010(3) 0.008(3) 0.005(3) N13 0.018(3) 0.010(3) 0.018(3) 0.011(3) 0.011(3) 0.009(3) C13 0.018(4) 0.019(4) 0.028(5) 0.021(4) 0.008(4) 0.003(3) O14 0.029(3) 0.020(3) 0.024(3) 0.016(3) 0.015(3) 0.013(3) N14 0.017(3) 0.011(3) 0.023(4) 0.014(3) 0.012(3) 0.010(3) C14 0.016(3) 0.009(3) 0.013(4) 0.006(3) 0.005(3) 0.004(3) O15 0.027(3) 0.019(3) 0.015(3) 0.016(2) 0.007(3) 0.009(3) N15 0.036(4) 0.012(3) 0.019(4) 0.009(3) 0.017(3) 0.006(3) C15 0.014(3) 0.017(4) 0.017(4) 0.012(3) 0.000(3) 0.003(3) O16 0.027(3) 0.016(3) 0.016(3) 0.013(2) 0.012(3) 0.009(2) N16 0.033(4) 0.013(3) 0.013(3) 0.006(3) 0.008(3) 0.004(3) C16 0.012(3) 0.012(4) 0.019(4) 0.008(3) 0.009(3) 0.003(3) O17 0.023(3) 0.017(3) 0.014(3) 0.007(2) 0.007(3) 0.004(3) N17 0.019(3) 0.018(4) 0.024(4) 0.010(3) 0.009(3) 0.004(3) C17 0.018(4) 0.018(4) 0.020(4) 0.011(3) 0.008(3) 0.007(3) O18 0.022(3) 0.012(3) 0.013(3) 0.007(2) 0.004(2) 0.004(2) N18 0.024(4) 0.021(4) 0.014(3) 0.005(3) 0.009(3) 0.003(3) C18 0.026(4) 0.018(4) 0.021(4) 0.012(4) 0.006(4) -0.002(4) O19 0.015(3) 0.023(3) 0.021(3) 0.012(3) 0.008(3) 0.007(2) N19 0.018(3) 0.013(3) 0.020(4) 0.013(3) 0.009(3) 0.005(3) C19 0.008(3) 0.019(4) 0.027(4) 0.017(4) 0.005(3) 0.000(3) O20 0.024(3) 0.015(3) 0.012(3) 0.008(2) 0.005(2) 0.006(2) N20 0.021(3) 0.013(3) 0.021(4) 0.015(3) 0.009(3) 0.005(3) C20 0.017(4) 0.013(4) 0.020(4) 0.010(3) 0.011(3) 0.006(3) O21 0.023(3) 0.010(3) 0.015(3) 0.009(2) 0.004(2) 0.001(2) N21 0.020(3) 0.014(3) 0.022(4) 0.014(3) 0.008(3) 0.005(3) C21 0.020(4) 0.014(4) 0.023(4) 0.010(3) 0.005(4) 0.000(3) O22 0.016(3) 0.015(3) 0.018(3) 0.010(2) 0.004(2) 0.002(2) N22 0.020(3) 0.015(3) 0.026(4) 0.012(3) 0.013(3) 0.006(3) C22 0.024(4) 0.025(5) 0.030(5) 0.020(4) 0.011(4) 0.006(4) O23 0.017(3) 0.011(3) 0.023(3) 0.012(2) 0.003(2) -0.001(2) N23 0.019(3) 0.014(3) 0.016(3) 0.012(3) 0.008(3) 0.003(3) C23 0.021(4) 0.025(4) 0.022(4) 0.016(4) 0.009(4) 0.005(4) O24 0.017(3) 0.007(2) 0.025(3) 0.008(2) 0.004(3) 0.004(2) N24 0.021(3) 0.020(4) 0.025(4) 0.019(3) 0.014(3) 0.006(3) C24 0.017(4) 0.018(4) 0.020(4) 0.014(3) 0.004(3) 0.001(3) O25 0.016(3) 0.018(3) 0.015(3) 0.013(2) 0.008(2) 0.006(2) N25 0.021(3) 0.011(3) 0.018(4) 0.006(3) 0.011(3) 0.002(3) C25 0.012(3) 0.013(4) 0.013(4) 0.008(3) 0.006(3) -0.003(3) O26 0.019(3) 0.017(3) 0.012(3) 0.009(2) 0.011(2) 0.008(2) N26 0.021(3) 0.016(3) 0.016(3) 0.011(3) 0.009(3) 0.001(3) C26 0.015(3) 0.016(4) 0.011(4) 0.011(3) 0.004(3) 0.006(3) O27 0.015(3) 0.020(3) 0.033(4) 0.020(3) 0.007(3) 0.007(2) N27 0.020(3) 0.017(3) 0.027(4) 0.019(3) 0.014(3) 0.010(3) C27 0.010(3) 0.019(4) 0.013(4) 0.010(3) 0.004(3) 0.002(3) O28 0.019(3) 0.028(3) 0.033(4) 0.027(3) 0.011(3) 0.011(3) N28 0.022(3) 0.024(4) 0.031(4) 0.023(4) 0.016(3) 0.013(3) C28 0.013(3) 0.017(4) 0.008(3) 0.008(3) 0.006(3) 0.007(3) O29 0.027(3) 0.013(3) 0.013(3) 0.009(2) 0.014(3) 0.005(2) N29 0.027(4) 0.024(4) 0.020(4) 0.019(3) 0.009(3) 0.017(3) C29 0.020(4) 0.019(4) 0.019(4) 0.014(3) 0.006(3) 0.005(3) O30 0.019(3) 0.013(3) 0.017(3) 0.008(2) 0.009(2) 0.003(2) C30 0.013(3) 0.017(4) 0.014(4) 0.011(3) 0.003(3) 0.005(3) N30 0.037(4) 0.022(4) 0.026(4) 0.018(3) 0.018(4) 0.014(4) O31 0.019(3) 0.026(3) 0.019(3) 0.017(3) 0.014(3) 0.014(3) N31 0.022(3) 0.006(3) 0.019(4) 0.005(3) 0.012(3) 0.007(3) C31 0.018(4) 0.020(4) 0.021(4) 0.015(4) 0.008(3) 0.010(3) O32 0.017(3) 0.015(3) 0.017(3) 0.013(2) 0.012(2) 0.010(2) N32 0.014(3) 0.016(3) 0.016(3) 0.008(3) 0.008(3) 0.005(3) C32 0.026(4) 0.018(4) 0.037(5) 0.021(4) 0.015(4) 0.004(4) O33 0.024(3) 0.017(3) 0.019(3) 0.008(3) 0.009(3) 0.004(3) N33 0.017(3) 0.013(3) 0.022(4) 0.009(3) 0.012(3) 0.009(3) C33 0.021(4) 0.014(4) 0.027(5) 0.010(4) 0.007(4) 0.004(3) O34 0.026(3) 0.010(3) 0.014(3) 0.009(2) 0.012(3) 0.008(2) N34 0.021(3) 0.021(4) 0.030(4) 0.020(3) 0.013(3) 0.015(3) C34 0.018(4) 0.025(4) 0.024(5) 0.017(4) 0.002(4) 0.008(4) O35 0.021(3) 0.007(2) 0.015(3) 0.006(2) 0.008(2) 0.006(2) C35 0.024(4) 0.017(4) 0.018(4) 0.010(3) 0.015(4) 0.011(3) N35 0.020(3) 0.015(3) 0.023(4) 0.010(3) 0.015(3) 0.006(3) O36 0.020(2) 0.0146(19) 0.017(2) 0.0104(17) 0.0116(18) 0.0080(17) C36 0.013(3) 0.015(4) 0.022(4) 0.007(3) 0.004(3) 0.003(3) N36 0.027(4) 0.021(4) 0.020(4) 0.011(3) 0.013(3) 0.009(3) O37 0.014(2) 0.015(3) 0.014(3) 0.009(2) 0.013(2) 0.010(2) C37 0.025(4) 0.011(4) 0.023(4) 0.007(3) 0.008(4) 0.009(3) O38 0.016(3) 0.013(3) 0.019(3) 0.011(2) 0.000(2) 0.000(2) C38 0.025(4) 0.013(4) 0.010(4) 0.006(3) 0.006(3) 0.002(3) O39 0.020(2) 0.0146(19) 0.017(2) 0.0104(17) 0.0116(18) 0.0080(17) C39 0.021(4) 0.012(4) 0.017(4) 0.008(3) 0.008(3) 0.007(3) O40 0.021(3) 0.015(3) 0.017(3) 0.010(2) 0.012(3) 0.004(2) C40 0.025(4) 0.016(4) 0.017(4) 0.011(3) 0.006(4) 0.011(3) O41 0.018(3) 0.016(3) 0.029(3) 0.014(3) 0.005(3) 0.004(2) C41 0.025(4) 0.011(4) 0.033(5) 0.008(4) 0.014(4) 0.008(4) O42 0.022(3) 0.021(3) 0.027(3) 0.015(3) 0.011(3) 0.008(3) C42 0.033(5) 0.014(4) 0.054(7) 0.014(5) 0.017(5) 0.009(4) C43 0.019(4) 0.027(5) 0.028(5) 0.009(4) 0.010(4) 0.012(4) O43 0.034(9) 0.083(16) 0.081(15) 0.015(12) 0.015(9) 0.003(9) O44 0.076(7) 0.039(5) 0.040(5) 0.019(4) 0.021(5) 0.014(5) C44 0.029(5) 0.037(6) 0.031(5) 0.017(5) 0.017(5) 0.012(5) O45 0.022(3) 0.014(3) 0.061(5) 0.017(3) 0.025(4) 0.007(3) C45 0.036(6) 0.056(8) 0.040(7) 0.028(6) 0.023(5) 0.021(6) O46 0.036(4) 0.017(3) 0.086(7) 0.026(4) 0.041(5) 0.012(3) C46 0.031(5) 0.056(7) 0.022(5) 0.013(5) 0.013(4) 0.029(5) O47 0.020(3) 0.031(4) 0.025(3) 0.015(3) 0.010(3) 0.002(3) C47 0.030(4) 0.029(4) 0.043(5) 0.008(4) 0.009(4) 0.016(3) O48 0.019(3) 0.031(4) 0.031(4) 0.007(3) 0.007(3) 0.004(3) C48 0.030(4) 0.029(4) 0.043(5) 0.008(4) 0.009(4) 0.016(3) O49 0.028(4) 0.077(6) 0.071(6) 0.068(6) 0.030(4) 0.028(4) C49 0.018(4) 0.005(3) 0.017(4) 0.004(3) 0.005(3) 0.003(3) O50 0.029(3) 0.028(3) 0.027(4) 0.019(3) 0.012(3) 0.008(3) C50 0.019(4) 0.016(4) 0.020(4) 0.012(3) 0.014(4) 0.007(3) C51 0.022(4) 0.008(3) 0.023(4) 0.010(3) 0.017(4) 0.009(3) C52 0.014(3) 0.014(4) 0.016(4) 0.009(3) 0.007(3) 0.003(3) C53 0.021(4) 0.025(4) 0.028(5) 0.018(4) 0.005(4) 0.006(4) C54 0.016(4) 0.016(4) 0.015(4) 0.004(3) 0.005(3) 0.001(3) C55 0.019(4) 0.017(4) 0.018(4) 0.011(3) 0.005(3) 0.010(3) C56 0.024(4) 0.024(5) 0.029(5) 0.012(4) 0.013(4) 0.014(4) C57 0.030(5) 0.035(5) 0.021(5) 0.019(4) 0.009(4) 0.004(4) C58 0.038(5) 0.024(5) 0.021(5) 0.014(4) 0.016(4) 0.005(4) C59 0.030(5) 0.015(4) 0.019(4) 0.010(3) 0.009(4) -0.001(4) C60 0.027(4) 0.018(4) 0.021(4) 0.013(4) 0.013(4) 0.003(4) C61 0.025(4) 0.015(4) 0.024(4) 0.014(3) 0.018(4) 0.005(3) C62 0.016(4) 0.017(4) 0.023(4) 0.012(4) 0.012(3) 0.004(3) C63 0.018(4) 0.014(4) 0.025(4) 0.012(3) 0.015(4) 0.009(3) C64 0.019(4) 0.018(4) 0.018(4) 0.009(3) 0.010(3) -0.002(3) C65 0.015(4) 0.019(4) 0.022(4) 0.011(4) 0.010(3) 0.006(3) C66 0.022(4) 0.022(4) 0.024(5) 0.009(4) 0.007(4) 0.012(4) C67 0.018(4) 0.015(4) 0.015(4) 0.009(3) 0.008(3) 0.002(3) C68 0.016(4) 0.013(4) 0.022(4) 0.007(3) 0.007(3) 0.001(3) C69 0.016(4) 0.018(4) 0.026(5) 0.010(4) 0.007(4) -0.003(3) C70 0.032(5) 0.030(5) 0.021(5) 0.011(4) 0.012(4) 0.011(4) C71 0.031(5) 0.037(5) 0.023(5) 0.021(4) 0.013(4) 0.012(4) C72 0.029(5) 0.035(5) 0.019(5) 0.015(4) 0.012(4) 0.013(4) C73 0.019(4) 0.012(4) 0.020(4) 0.010(3) 0.004(3) 0.006(3) C74 0.015(3) 0.014(4) 0.020(4) 0.014(3) 0.005(3) 0.003(3) C75 0.011(3) 0.015(4) 0.028(4) 0.016(4) 0.010(3) 0.003(3) C76 0.017(4) 0.015(4) 0.018(4) 0.011(3) 0.009(3) 0.006(3) C77 0.031(5) 0.015(4) 0.024(5) 0.012(4) 0.009(4) 0.008(4) C78 0.020(4) 0.021(4) 0.015(4) 0.013(3) 0.011(3) 0.007(3) C79 0.022(4) 0.017(4) 0.024(4) 0.013(4) 0.011(4) 0.008(3) C80 0.026(4) 0.019(4) 0.034(5) 0.020(4) 0.018(4) 0.014(4) C81 0.022(4) 0.022(4) 0.028(5) 0.013(4) 0.016(4) 0.005(4) C82 0.022(4) 0.030(5) 0.019(4) 0.012(4) 0.007(4) 0.002(4) C83 0.020(4) 0.022(4) 0.020(4) 0.012(4) 0.007(4) 0.005(4) C84 0.019(4) 0.013(4) 0.024(4) 0.010(3) 0.008(4) 0.003(3) C85 0.017(4) 0.010(3) 0.017(4) 0.008(3) 0.006(3) 0.002(3) C86 0.018(4) 0.008(3) 0.023(4) 0.012(3) 0.001(3) 0.001(3) C87 0.019(4) 0.013(4) 0.017(4) 0.011(3) 0.002(3) 0.003(3) C88 0.030(4) 0.011(3) 0.009(4) 0.005(3) 0.008(3) 0.009(3) C89 0.032(5) 0.011(4) 0.015(4) 0.008(3) 0.003(4) 0.006(3) C90 0.032(5) 0.025(5) 0.024(5) 0.012(4) 0.003(4) 0.004(4) C91 0.050(4) 0.020(3) 0.038(4) 0.013(3) 0.030(4) 0.011(3) C92 0.042(5) 0.018(4) 0.038(6) 0.011(4) 0.020(5) 0.011(4) C93 0.040(5) 0.035(6) 0.048(7) 0.020(6) 0.029(6) 0.020(5) C94 0.050(4) 0.020(3) 0.038(4) 0.013(3) 0.030(4) 0.011(3) C95 0.071(8) 0.029(5) 0.044(7) 0.026(5) 0.041(7) 0.021(6) C96 0.053(6) 0.018(4) 0.029(5) 0.013(4) 0.026(5) 0.005(5) C97 0.021(4) 0.014(4) 0.021(4) 0.013(3) 0.007(4) 0.011(3) C98 0.014(3) 0.011(2) 0.020(3) 0.012(2) 0.004(2) 0.000(2) C99 0.014(3) 0.011(2) 0.020(3) 0.012(2) 0.004(2) 0.000(2) C100 0.022(4) 0.017(4) 0.021(4) 0.009(4) 0.007(4) 0.006(3) C101 0.025(4) 0.029(5) 0.021(5) 0.011(4) 0.009(4) -0.002(4) C102 0.016(4) 0.018(4) 0.025(5) 0.005(4) 0.007(4) 0.008(3) C103 0.018(4) 0.037(6) 0.024(5) 0.008(4) 0.002(4) 0.005(4) C104 0.021(5) 0.062(8) 0.017(5) 0.001(5) -0.001(4) 0.002(5) C105 0.031(6) 0.047(7) 0.038(6) -0.002(6) 0.020(5) -0.017(6) C106 0.033(6) 0.057(8) 0.036(6) 0.012(6) 0.021(5) -0.009(6) C107 0.026(5) 0.034(6) 0.026(5) 0.011(4) 0.007(4) -0.002(4) C108 0.022(4) 0.015(4) 0.015(4) 0.010(3) 0.003(3) -0.002(3) C109 0.020(4) 0.016(4) 0.020(4) 0.013(3) 0.010(3) 0.003(3) C110 0.014(3) 0.014(4) 0.017(4) 0.011(3) 0.006(3) 0.006(3) C111 0.019(4) 0.013(4) 0.015(4) 0.007(3) 0.012(3) 0.005(3) C112 0.010(3) 0.017(4) 0.017(4) 0.011(3) 0.009(3) 0.001(3) C113 0.021(3) 0.015(3) 0.023(3) 0.017(3) 0.007(3) 0.005(2) C114 0.021(3) 0.015(3) 0.023(3) 0.017(3) 0.007(3) 0.005(2) C115 0.019(4) 0.022(4) 0.018(4) 0.015(4) 0.008(3) 0.008(3) C116 0.020(4) 0.012(4) 0.028(5) 0.011(4) 0.010(4) 0.004(3) C117 0.020(4) 0.017(4) 0.020(4) 0.007(4) 0.004(4) -0.001(3) C118 0.018(4) 0.022(4) 0.023(5) 0.010(4) -0.002(4) -0.004(4) C119 0.020(4) 0.028(5) 0.025(5) 0.020(4) 0.007(4) 0.008(4) C120 0.016(4) 0.017(4) 0.022(4) 0.012(3) 0.011(3) 0.004(3) C121 0.010(3) 0.015(4) 0.025(4) 0.014(3) 0.008(3) 0.006(3) C122 0.017(4) 0.012(4) 0.022(4) 0.011(3) 0.008(3) 0.003(3) C123 0.014(3) 0.011(3) 0.021(4) 0.013(3) 0.005(3) 0.004(3) C124 0.016(4) 0.020(4) 0.019(4) 0.011(3) 0.012(3) 0.010(3) C125 0.023(4) 0.015(4) 0.022(4) 0.007(3) 0.008(4) -0.002(3) C126 0.020(4) 0.017(4) 0.018(4) 0.013(3) 0.014(3) 0.010(3) C127 0.023(4) 0.026(4) 0.020(4) 0.016(4) 0.016(4) 0.014(4) C128 0.029(5) 0.027(5) 0.028(5) 0.021(4) 0.016(4) 0.010(4) C129 0.023(4) 0.031(5) 0.033(5) 0.027(4) 0.018(4) 0.019(4) C130 0.034(5) 0.018(4) 0.047(6) 0.022(5) 0.024(5) 0.016(4) C131 0.021(4) 0.022(4) 0.034(5) 0.022(4) 0.011(4) 0.003(4) C132 0.023(4) 0.013(4) 0.019(4) 0.008(3) 0.009(4) 0.007(3) C133 0.019(4) 0.018(4) 0.019(4) 0.013(3) 0.007(3) 0.013(3) C134 0.0130(19) 0.014(2) 0.016(2) 0.0108(18) 0.0077(18) 0.0044(17) C135 0.0130(19) 0.014(2) 0.016(2) 0.0108(18) 0.0077(18) 0.0044(17) C136 0.0130(19) 0.014(2) 0.016(2) 0.0108(18) 0.0077(18) 0.0044(17) C137 0.013(3) 0.020(4) 0.015(4) 0.012(3) 0.007(3) 0.002(3) C138 0.026(4) 0.024(4) 0.021(4) 0.015(4) 0.011(4) 0.006(4) C139 0.013(3) 0.017(4) 0.027(5) 0.017(4) 0.005(3) 0.001(3) C140 0.021(4) 0.015(4) 0.023(4) 0.011(4) 0.006(4) 0.005(3) C141 0.025(4) 0.015(4) 0.028(5) 0.008(4) 0.005(4) 0.003(4) C142 0.026(5) 0.026(5) 0.058(7) 0.034(5) 0.016(5) 0.014(4) C143 0.028(5) 0.033(5) 0.037(6) 0.029(5) 0.010(4) 0.009(4) C144 0.024(4) 0.034(5) 0.031(5) 0.029(5) 0.009(4) 0.011(4) C145 0.011(3) 0.016(4) 0.014(4) 0.007(3) 0.007(3) 0.004(3) C146 0.013(2) 0.014(3) 0.014(3) 0.009(2) 0.005(2) 0.007(2) C147 0.013(2) 0.014(3) 0.014(3) 0.009(2) 0.005(2) 0.007(2) C148 0.021(4) 0.011(3) 0.016(4) 0.008(3) 0.011(3) 0.003(3) C149 0.023(4) 0.014(4) 0.017(4) 0.008(3) 0.010(4) 0.006(3) C150 0.019(4) 0.018(4) 0.016(4) 0.011(3) 0.014(3) 0.011(3) C151 0.021(4) 0.018(4) 0.019(4) 0.011(3) 0.009(4) 0.005(3) C152 0.024(4) 0.028(5) 0.012(4) 0.009(4) 0.007(4) 0.000(4) C153 0.027(4) 0.027(5) 0.036(5) 0.024(4) 0.022(4) 0.009(4) C154 0.030(5) 0.018(4) 0.024(5) 0.013(4) 0.009(4) -0.002(4) C155 0.018(4) 0.019(4) 0.024(4) 0.017(4) 0.008(4) 0.004(3) C156 0.026(4) 0.009(3) 0.016(4) 0.005(3) 0.014(4) 0.009(3) C157 0.016(4) 0.011(3) 0.016(4) 0.008(3) 0.001(3) 0.000(3) C158 0.022(3) 0.011(2) 0.010(3) 0.007(2) 0.006(2) 0.007(2) C159 0.022(3) 0.011(2) 0.010(3) 0.007(2) 0.006(2) 0.007(2) C160 0.019(4) 0.017(4) 0.014(4) 0.011(3) 0.008(3) 0.000(3) C161 0.022(4) 0.012(3) 0.015(4) 0.011(3) 0.008(3) 0.007(3) C162 0.024(4) 0.027(5) 0.023(5) 0.018(4) 0.012(4) 0.012(4) C163 0.024(4) 0.035(5) 0.015(4) 0.019(4) 0.008(4) 0.008(4) C164 0.037(5) 0.041(6) 0.034(6) 0.031(5) 0.021(5) 0.018(5) C165 0.037(4) 0.032(4) 0.042(4) 0.029(4) 0.026(4) 0.016(3) C166 0.044(6) 0.049(6) 0.034(6) 0.035(5) 0.030(5) 0.034(5) C167 0.029(5) 0.052(7) 0.038(6) 0.039(6) 0.021(5) 0.018(5) C168 0.037(4) 0.032(4) 0.042(4) 0.029(4) 0.026(4) 0.016(3) C169 0.013(3) 0.020(4) 0.013(4) 0.010(3) 0.001(3) 0.002(3) C170 0.019(4) 0.009(3) 0.016(4) 0.009(3) 0.006(3) 0.005(3) C171 0.023(4) 0.009(3) 0.014(4) 0.006(3) 0.006(3) 0.003(3) C172 0.029(5) 0.015(4) 0.016(4) 0.010(3) 0.002(4) 0.002(4) C173 0.049(6) 0.022(5) 0.026(5) 0.016(4) 0.022(5) 0.009(5) C174 0.051(5) 0.042(4) 0.042(5) 0.028(4) 0.012(4) 0.033(4) C175 0.030(5) 0.044(6) 0.018(5) 0.020(5) 0.005(4) 0.013(5) C176 0.039(6) 0.078(9) 0.010(5) 0.014(5) 0.004(4) 0.028(7) C177 0.059(8) 0.066(9) 0.038(7) 0.026(7) 0.017(6) 0.049(8) C178 0.051(5) 0.042(4) 0.042(5) 0.028(4) 0.012(4) 0.033(4) C179 0.049(7) 0.039(6) 0.049(7) 0.034(6) 0.025(6) 0.031(6) C180 0.015(3) 0.017(4) 0.016(4) 0.013(3) 0.004(3) 0.005(3) C181 0.023(4) 0.011(4) 0.024(4) 0.012(3) 0.014(4) 0.011(3) C182 0.020(4) 0.010(3) 0.016(4) 0.005(3) 0.011(3) 0.005(3) C183 0.015(3) 0.015(4) 0.017(4) 0.011(3) 0.007(3) 0.007(3) C184 0.018(4) 0.023(4) 0.019(4) 0.018(4) 0.011(3) 0.006(3) C185 0.015(3) 0.017(4) 0.023(4) 0.013(3) 0.016(3) 0.009(3) C186 0.029(4) 0.012(4) 0.020(4) 0.009(3) 0.011(4) 0.007(3) C187 0.021(4) 0.011(3) 0.016(4) 0.010(3) 0.009(3) 0.007(3) C188 0.019(4) 0.015(4) 0.028(5) 0.015(4) 0.013(4) 0.008(3) C189 0.025(4) 0.025(5) 0.036(5) 0.024(4) 0.016(4) 0.008(4) C190 0.021(4) 0.032(5) 0.026(5) 0.019(4) 0.012(4) 0.014(4) C191 0.014(4) 0.016(4) 0.024(4) 0.010(4) 0.006(3) 0.004(3) C192 0.026(4) 0.014(4) 0.023(4) 0.013(3) 0.014(4) 0.010(3) C193 0.015(4) 0.018(4) 0.014(4) 0.009(3) 0.007(3) -0.004(3) C194 0.009(3) 0.015(4) 0.027(4) 0.016(4) 0.008(3) 0.004(3) C195 0.020(4) 0.020(4) 0.023(4) 0.015(4) 0.017(4) 0.008(3) C196 0.025(4) 0.022(4) 0.021(4) 0.016(4) 0.011(4) 0.009(4) C197 0.022(4) 0.021(4) 0.023(5) 0.014(4) 0.006(4) 0.007(4) C198 0.022(4) 0.009(4) 0.018(4) -0.001(3) 0.013(4) 0.003(3) C199 0.019(4) 0.019(4) 0.023(4) 0.013(4) 0.009(4) 0.003(3) C200 0.029(5) 0.022(4) 0.020(4) 0.009(4) 0.013(4) 0.005(4) C201 0.028(5) 0.014(4) 0.029(5) 0.001(4) 0.012(4) -0.002(4) C202 0.033(5) 0.013(4) 0.035(5) 0.007(4) 0.021(5) 0.002(4) C203 0.027(4) 0.011(4) 0.029(5) 0.011(4) 0.014(4) 0.009(3) C204 0.024(4) 0.018(4) 0.020(4) 0.013(4) 0.010(4) 0.001(3) C205 0.014(4) 0.022(4) 0.021(4) 0.013(4) 0.006(3) -0.004(3) C206 0.013(3) 0.016(4) 0.019(4) 0.012(3) 0.007(3) 0.000(3) C207 0.009(3) 0.016(4) 0.020(4) 0.015(3) 0.008(3) 0.005(3) C208 0.013(3) 0.013(3) 0.013(4) 0.007(3) 0.010(3) 0.009(3) C209 0.021(4) 0.015(4) 0.024(4) 0.012(4) 0.012(4) 0.005(3) C210 0.025(4) 0.025(5) 0.030(5) 0.018(4) 0.018(4) 0.005(4) C211 0.022(4) 0.016(4) 0.030(5) 0.010(4) 0.013(4) 0.008(4) C212 0.026(5) 0.017(4) 0.038(6) 0.008(4) 0.016(5) 0.004(4) C213 0.034(6) 0.018(5) 0.048(7) 0.002(5) 0.016(5) 0.001(4) C214 0.039(6) 0.011(4) 0.068(9) 0.015(5) 0.022(6) 0.002(4) C215 0.061(8) 0.019(5) 0.064(8) 0.022(6) 0.034(7) 0.001(5) C216 0.045(6) 0.017(4) 0.037(6) 0.015(4) 0.027(5) 0.007(4) C217 0.046(7) 0.048(7) 0.023(5) 0.017(5) 0.009(5) 0.006(6) C218 0.22(3) 0.064(10) 0.058(10) 0.052(9) 0.088(14) 0.092(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tb1 O1 2.266(6) . ? Tb1 O5 2.289(6) . ? Tb1 O9 2.302(6) . ? Tb1 O10 2.321(6) . ? Tb1 O13 2.340(7) . ? Tb1 O6 2.343(6) . ? Tb1 O2 2.343(6) . ? O1 C1 1.272(11) . ? N1 C1 1.395(10) . ? N1 N2 1.389(10) . ? N1 C6 1.406(12) . ? C1 C2 1.396(13) . ? Tb2 O3 2.265(6) . ? Tb2 O11 2.280(6) . ? Tb2 O7 2.291(7) . ? Tb2 O4 2.330(6) . ? Tb2 O8 2.333(6) . ? Tb2 O12 2.344(7) . ? Tb2 O14 2.369(7) . ? O2 C3 1.253(10) . ? N2 C4 1.322(12) . ? C2 C3 1.445(12) . ? C2 C4 1.439(11) . ? Tb3 O15 2.272(6) . ? Tb3 O23 2.286(5) . ? Tb3 O16 2.312(6) . ? Tb3 O19 2.330(6) . ? Tb3 O20 2.333(7) . ? Tb3 O24 2.338(6) . ? Tb3 O27 2.353(7) . ? O3 C16 1.283(11) . ? C3 C12 1.500(13) . ? N3 C16 1.381(11) . ? N3 N4 1.387(10) . ? N3 C19 1.436(10) . ? Tb4 O17 2.294(7) . ? Tb4 O25 2.306(5) . ? Tb4 O22 2.314(6) . ? Tb4 O28 2.316(6) . ? Tb4 O21 2.322(6) . ? Tb4 O26 2.327(6) . ? Tb4 O18 2.364(6) . ? O4 C14 1.247(10) . ? C4 C5 1.482(13) . ? N4 C17 1.316(11) . ? Tb5 O29 2.286(6) . ? Tb5 O37 2.292(6) . ? Tb5 O38 2.307(6) . ? Tb5 O33 2.315(7) . ? Tb5 O34 2.344(6) . ? Tb5 O30 2.351(6) . ? Tb5 O41 2.349(6) . ? O5 C25 1.247(10) . ? N5 N6 1.389(10) . ? N5 C25 1.390(10) . ? N5 C30 1.429(11) . ? Tb6 O35 2.299(6) . ? Tb6 O39 2.308(6) . ? Tb6 O31 2.307(6) . ? Tb6 O40 2.317(6) . ? Tb6 O32 2.323(6) . ? Tb6 O36 2.332(6) . ? Tb6 O42 2.333(6) . ? O6 C27 1.256(10) . ? N6 C28 1.303(11) . ? C6 C11 1.390(14) . ? C6 C7 1.405(13) . ? O7 C40 1.277(10) . ? N7 C40 1.362(12) . ? N7 N8 1.382(10) . ? N7 C43 1.425(13) . ? C7 C8 1.378(14) . ? O8 C38 1.245(10) . ? N8 C41 1.311(13) . ? C8 C9 1.387(17) . ? O9 C49 1.268(9) . ? N9 C49 1.361(11) . ? N9 N10 1.378(9) . ? N9 C54 1.424(11) . ? C9 C10 1.375(16) . ? O10 C51 1.255(10) . ? N10 C52 1.317(11) . ? C10 C11 1.390(13) . ? O11 C64 1.280(12) . ? N11 C64 1.374(11) . ? N11 N12 1.393(10) . ? N11 C67 1.425(12) . ? O12 C62 1.259(11) . ? N12 C65 1.319(12) . ? C12 C13 1.519(11) . ? N13 C73 1.355(11) . ? N13 N14 1.406(9) . ? N13 C78 1.412(12) . ? C13 C14 1.511(11) . ? N14 C76 1.317(12) . ? C14 C15 1.423(11) . ? O15 C73 1.292(10) . ? N15 C88 1.379(11) . ? N15 N16 1.383(11) . ? N15 C91 1.424(14) . ? C15 C16 1.432(11) . ? C15 C17 1.438(13) . ? O16 C75 1.279(9) . ? N16 C89 1.318(13) . ? O17 C88 1.267(10) . ? N17 C97 1.361(11) . ? N17 N18 1.386(11) . ? N17 C102 1.422(11) . ? C17 C18 1.493(12) . ? O18 C86 1.253(10) . ? N18 C100 1.305(12) . ? O19 C97 1.285(11) . ? N19 C112 1.386(10) . ? N19 C115 1.411(11) . ? N19 N20 1.407(9) . ? C19 C24 1.389(13) . ? C19 C20 1.393(12) . ? O20 C99 1.235(11) . ? N20 C113 1.300(11) . ? C20 C21 1.388(11) . ? O21 C110 1.265(9) . ? N21 C121 1.390(10) . ? N21 N22 1.399(10) . ? N21 C126 1.413(10) . ? C21 C22 1.402(14) . ? O22 C112 1.272(10) . ? N22 C124 1.322(11) . ? C22 C23 1.367(14) . ? O23 C121 1.267(10) . ? N23 C136 1.367(9) . ? N23 N24 1.393(11) . ? N23 C139 1.428(11) . ? C23 C24 1.397(11) . ? O24 C123 1.251(9) . ? N24 C137 1.305(11) . ? O25 C136 1.261(10) . ? N25 C145 1.372(11) . ? N25 C150 1.407(10) . ? N25 N26 1.404(10) . ? C25 C26 1.413(13) . ? O26 C134 1.246(10) . ? N26 C148 1.326(10) . ? C26 C27 1.435(11) . ? C26 C28 1.436(10) . ? N27 C160 1.380(10) . ? N27 N28 1.406(10) . ? N27 C163 1.402(13) . ? C27 C36 1.503(13) . ? N28 C161 1.313(12) . ? C28 C29 1.496(12) . ? O29 C145 1.272(10) . ? N29 C169 1.384(10) . ? N29 N30 1.401(11) . ? N29 C174 1.411(14) . ? O30 C147 1.253(10) . ? C30 C31 1.399(11) . ? C30 C35 1.408(12) . ? N30 C172 1.322(13) . ? O31 C160 1.279(10) . ? N31 N32 1.389(9) . ? N31 C184 1.405(10) . ? N31 C187 1.413(11) . ? C31 C32 1.395(13) . ? O32 C158 1.279(9) . ? N32 C185 1.312(11) . ? C32 C33 1.376(14) . ? O33 C169 1.274(10) . ? N33 C193 1.380(11) . ? N33 N34 1.386(10) . ? N33 C198 1.413(11) . ? C33 C34 1.397(12) . ? O34 C171 1.257(10) . ? N34 C196 1.308(12) . ? C34 C35 1.363(13) . ? O35 C184 1.275(10) . ? N35 C208 1.367(11) . ? N35 N36 1.400(10) . ? N35 C211 1.421(11) . ? O36 C182 1.281(10) . ? C36 C37 1.507(12) . ? N36 C209 1.322(11) . ? O37 C193 1.255(11) . ? C37 C38 1.520(13) . ? O38 C195 1.262(11) . ? C38 C39 1.415(13) . ? O39 C208 1.270(10) . ? C39 C41 1.423(12) . ? C39 C40 1.436(13) . ? O40 C206 1.251(11) . ? C41 C42 1.519(13) . ? C43 C44 1.400(15) . ? C43 C48 1.394(15) . ? C44 C45 1.406(16) . ? C45 C46 1.397(18) . ? C46 C47 1.366(18) . ? O47 C217 1.468(13) . ? C47 C48 1.388(18) . ? C49 C50 1.430(11) . ? C50 C51 1.414(12) . ? C50 C52 1.428(11) . ? C51 C60 1.518(11) . ? C52 C53 1.508(11) . ? C54 C55 1.372(13) . ? C54 C59 1.398(12) . ? C55 C56 1.393(13) . ? C56 C57 1.398(14) . ? C57 C58 1.402(15) . ? C58 C59 1.413(12) . ? C60 C61 1.498(12) . ? C61 C62 1.494(13) . ? C62 C63 1.423(13) . ? C63 C64 1.408(14) . ? C63 C65 1.411(12) . ? C65 C66 1.484(13) . ? C67 C68 1.383(12) . ? C67 C72 1.390(12) . ? C68 C69 1.393(14) . ? C69 C70 1.390(13) . ? C70 C71 1.355(15) . ? C71 C72 1.398(15) . ? C73 C74 1.404(13) . ? C74 C75 1.409(13) . ? C74 C76 1.438(10) . ? C75 C84 1.487(13) . ? C76 C77 1.501(12) . ? C78 C79 1.393(12) . ? C78 C83 1.405(12) . ? C79 C80 1.411(14) . ? C80 C81 1.371(14) . ? C81 C82 1.395(14) . ? C82 C83 1.381(15) . ? C84 C85 1.514(12) . ? C85 C86 1.498(11) . ? C86 C87 1.437(13) . ? C87 C89 1.417(12) . ? C87 C88 1.429(12) . ? C89 C90 1.515(13) . ? C91 C96 1.395(15) . ? C91 C92 1.397(17) . ? C92 C93 1.372(16) . ? C93 C94 1.427(17) . ? C94 C95 1.344(18) . ? C95 C96 1.392(16) . ? C97 C98 1.418(12) . ? C98 C100 1.419(13) . ? C98 C99 1.446(11) . ? C99 C108 1.494(12) . ? C100 C101 1.494(14) . ? C102 C103 1.359(13) . ? C102 C107 1.417(15) . ? C103 C104 1.384(15) . ? C104 C105 1.38(2) . ? C105 C106 1.412(19) . ? C106 C107 1.386(14) . ? C108 C109 1.520(11) . ? C109 C110 1.512(11) . ? C110 C111 1.412(11) . ? C111 C112 1.407(12) . ? C111 C113 1.443(11) . ? C113 C114 1.497(11) . ? C115 C116 1.386(12) . ? C115 C120 1.392(12) . ? C116 C117 1.405(12) . ? C117 C118 1.396(14) . ? C118 C119 1.384(14) . ? C119 C120 1.383(12) . ? C121 C122 1.414(12) . ? C122 C124 1.409(11) . ? C122 C123 1.453(10) . ? C123 C132 1.477(12) . ? C124 C125 1.482(12) . ? C126 C127 1.385(12) . ? C126 C131 1.397(12) . ? C127 C128 1.375(13) . ? C128 C129 1.387(13) . ? C129 C130 1.392(15) . ? C130 C131 1.371(13) . ? C132 C133 1.511(11) . ? C133 C134 1.501(12) . ? C134 C135 1.418(10) . ? C135 C136 1.424(12) . ? C135 C137 1.437(11) . ? C137 C138 1.477(13) . ? C139 C144 1.392(11) . ? C139 C140 1.394(14) . ? C140 C141 1.361(13) . ? C141 C142 1.415(14) . ? C142 C143 1.375(17) . ? C143 C144 1.372(14) . ? C145 C146 1.425(10) . ? C146 C147 1.417(11) . ? C146 C148 1.428(12) . ? C147 C156 1.507(11) . ? C148 C149 1.503(11) . ? C150 C155 1.392(12) . ? C150 C151 1.417(12) . ? C151 C152 1.371(12) . ? C152 C153 1.379(13) . ? C153 C154 1.393(14) . ? C154 C155 1.387(11) . ? C156 C157 1.509(12) . ? C157 C158 1.491(12) . ? C158 C159 1.413(12) . ? C159 C160 1.403(13) . ? C159 C161 1.444(10) . ? C161 C162 1.483(12) . ? C163 C168 1.388(12) . ? C163 C164 1.394(15) . ? C164 C165 1.401(16) . ? C165 C166 1.391(13) . ? C166 C167 1.381(16) . ? C167 C168 1.387(16) . ? C169 C170 1.419(13) . ? C170 C171 1.419(11) . ? C170 C172 1.430(11) . ? C171 C180 1.503(13) . ? C172 C173 1.468(14) . ? C174 C175 1.373(17) . ? C174 C179 1.384(15) . ? C175 C176 1.392(17) . ? C176 C177 1.37(2) . ? C177 C178 1.34(2) . ? C178 C179 1.411(17) . ? C180 C181 1.510(11) . ? C181 C182 1.517(12) . ? C182 C183 1.405(11) . ? C183 C184 1.401(11) . ? C183 C185 1.431(11) . ? C185 C186 1.498(12) . ? C187 C192 1.385(12) . ? C187 C188 1.420(10) . ? C188 C189 1.373(13) . ? C189 C190 1.389(13) . ? C190 C191 1.395(12) . ? C191 C192 1.367(12) . ? C193 C194 1.417(11) . ? C194 C195 1.420(12) . ? C194 C196 1.434(12) . ? C195 C204 1.492(12) . ? C196 C197 1.480(12) . ? C198 C199 1.390(13) . ? C198 C203 1.407(11) . ? C199 C200 1.379(12) . ? C200 C201 1.402(13) . ? C201 C202 1.379(16) . ? C202 C203 1.379(13) . ? C204 C205 1.543(13) . ? C205 C206 1.508(10) . ? C206 C207 1.406(12) . ? C207 C208 1.427(10) . ? C207 C209 1.435(13) . ? C209 C210 1.495(12) . ? C211 C216 1.373(14) . ? C211 C212 1.379(14) . ? C212 C213 1.414(14) . ? C213 C214 1.360(19) . ? C214 C215 1.365(19) . ? C215 C216 1.418(13) . ? C217 C218 1.504(19) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Tb1 O5 112.4(2) . . ? O1 Tb1 O9 107.3(2) . . ? O5 Tb1 O9 125.6(2) . . ? O1 Tb1 O10 161.1(2) . . ? O5 Tb1 O10 78.3(2) . . ? O9 Tb1 O10 75.6(2) . . ? O1 Tb1 O13 76.9(2) . . ? O5 Tb1 O13 76.7(2) . . ? O9 Tb1 O13 77.7(2) . . ? O10 Tb1 O13 121.5(2) . . ? O1 Tb1 O6 79.7(2) . . ? O5 Tb1 O6 74.4(2) . . ? O9 Tb1 O6 149.9(2) . . ? O10 Tb1 O6 88.9(2) . . ? O13 Tb1 O6 132.0(2) . . ? O1 Tb1 O2 76.8(2) . . ? O5 Tb1 O2 145.9(2) . . ? O9 Tb1 O2 77.9(2) . . ? O10 Tb1 O2 85.9(2) . . ? O13 Tb1 O2 136.5(2) . . ? O6 Tb1 O2 75.3(2) . . ? C1 O1 Tb1 126.6(6) . . ? C1 N1 N2 111.3(7) . . ? C1 N1 C6 127.7(7) . . ? N2 N1 C6 120.4(7) . . ? O1 C1 C2 133.3(8) . . ? O1 C1 N1 120.8(8) . . ? C2 C1 N1 105.9(7) . . ? O3 Tb2 O11 124.3(2) . . ? O3 Tb2 O7 122.1(2) . . ? O11 Tb2 O7 96.3(2) . . ? O3 Tb2 O4 74.9(2) . . ? O11 Tb2 O4 150.7(2) . . ? O7 Tb2 O4 88.8(2) . . ? O3 Tb2 O8 144.4(2) . . ? O11 Tb2 O8 78.6(2) . . ? O7 Tb2 O8 75.3(2) . . ? O4 Tb2 O8 74.8(2) . . ? O3 Tb2 O12 75.2(2) . . ? O11 Tb2 O12 75.9(2) . . ? O7 Tb2 O12 161.6(2) . . ? O4 Tb2 O12 90.3(2) . . ? O8 Tb2 O12 86.8(2) . . ? O3 Tb2 O14 75.1(2) . . ? O11 Tb2 O14 76.0(2) . . ? O7 Tb2 O14 77.9(2) . . ? O4 Tb2 O14 133.2(2) . . ? O8 Tb2 O14 140.4(2) . . ? O12 Tb2 O14 115.3(2) . . ? C3 O2 Tb1 135.6(6) . . ? C4 N2 N1 105.8(7) . . ? C1 C2 C3 122.7(7) . . ? C1 C2 C4 105.5(7) . . ? C3 C2 C4 131.7(8) . . ? O15 Tb3 O23 122.5(2) . . ? O15 Tb3 O16 74.9(2) . . ? O23 Tb3 O16 149.8(2) . . ? O15 Tb3 O19 115.6(2) . . ? O23 Tb3 O19 109.0(2) . . ? O16 Tb3 O19 79.2(2) . . ? O15 Tb3 O20 148.0(2) . . ? O23 Tb3 O20 76.1(2) . . ? O16 Tb3 O20 78.2(2) . . ? O19 Tb3 O20 75.4(2) . . ? O15 Tb3 O24 74.5(2) . . ? O23 Tb3 O24 74.4(2) . . ? O16 Tb3 O24 89.1(2) . . ? O19 Tb3 O24 161.3(2) . . ? O20 Tb3 O24 88.0(2) . . ? O15 Tb3 O27 75.9(2) . . ? O23 Tb3 O27 74.0(2) . . ? O16 Tb3 O27 136.2(2) . . ? O19 Tb3 O27 84.8(2) . . ? O20 Tb3 O27 136.1(2) . . ? O24 Tb3 O27 113.5(2) . . ? C16 O3 Tb2 128.1(5) . . ? O2 C3 C2 120.6(8) . . ? O2 C3 C12 118.2(7) . . ? C2 C3 C12 121.2(7) . . ? C16 N3 N4 111.0(6) . . ? C16 N3 C19 128.1(7) . . ? N4 N3 C19 120.6(7) . . ? O17 Tb4 O25 109.5(2) . . ? O17 Tb4 O22 116.0(2) . . ? O25 Tb4 O22 121.0(2) . . ? O17 Tb4 O28 80.4(2) . . ? O25 Tb4 O28 74.0(2) . . ? O22 Tb4 O28 78.7(2) . . ? O17 Tb4 O21 78.2(2) . . ? O25 Tb4 O21 151.9(2) . . ? O22 Tb4 O21 75.1(2) . . ? O28 Tb4 O21 134.0(2) . . ? O17 Tb4 O26 157.6(2) . . ? O25 Tb4 O26 74.5(2) . . ? O22 Tb4 O26 77.1(2) . . ? O28 Tb4 O26 121.2(2) . . ? O21 Tb4 O26 88.7(2) . . ? O17 Tb4 O18 74.8(2) . . ? O25 Tb4 O18 77.6(2) . . ? O22 Tb4 O18 148.2(2) . . ? O28 Tb4 O18 133.1(2) . . ? O21 Tb4 O18 78.5(2) . . ? O26 Tb4 O18 84.8(2) . . ? C14 O4 Tb2 137.3(5) . . ? N2 C4 C2 111.5(8) . . ? N2 C4 C5 118.3(7) . . ? C2 C4 C5 130.2(8) . . ? C17 N4 N3 107.2(7) . . ? O29 Tb5 O37 118.92(19) . . ? O29 Tb5 O38 75.6(2) . . ? O37 Tb5 O38 75.3(2) . . ? O29 Tb5 O33 112.0(2) . . ? O37 Tb5 O33 116.4(2) . . ? O38 Tb5 O33 155.7(2) . . ? O29 Tb5 O34 150.3(2) . . ? O37 Tb5 O34 78.10(19) . . ? O38 Tb5 O34 86.9(2) . . ? O33 Tb5 O34 75.7(2) . . ? O29 Tb5 O30 75.6(2) . . ? O37 Tb5 O30 151.1(2) . . ? O38 Tb5 O30 85.7(2) . . ? O33 Tb5 O30 74.6(2) . . ? O34 Tb5 O30 79.4(2) . . ? O29 Tb5 O41 77.2(2) . . ? O37 Tb5 O41 73.2(2) . . ? O38 Tb5 O41 120.1(2) . . ? O33 Tb5 O41 84.2(2) . . ? O34 Tb5 O41 132.4(2) . . ? O30 Tb5 O41 135.7(2) . . ? C25 O5 Tb1 131.5(6) . . ? N6 N5 C25 111.8(7) . . ? N6 N5 C30 121.4(6) . . ? C25 N5 C30 126.8(7) . . ? O35 Tb6 O39 123.0(2) . . ? O35 Tb6 O31 115.0(2) . . ? O39 Tb6 O31 109.1(2) . . ? O35 Tb6 O40 75.7(2) . . ? O39 Tb6 O40 74.8(2) . . ? O31 Tb6 O40 160.0(2) . . ? O35 Tb6 O32 147.8(2) . . ? O39 Tb6 O32 75.1(2) . . ? O31 Tb6 O32 76.8(2) . . ? O40 Tb6 O32 85.6(2) . . ? O35 Tb6 O36 75.0(2) . . ? O39 Tb6 O36 150.0(2) . . ? O31 Tb6 O36 78.3(2) . . ? O40 Tb6 O36 89.0(2) . . ? O32 Tb6 O36 78.7(2) . . ? O35 Tb6 O42 78.4(2) . . ? O39 Tb6 O42 74.4(2) . . ? O31 Tb6 O42 81.5(2) . . ? O40 Tb6 O42 118.1(2) . . ? O32 Tb6 O42 133.8(2) . . ? O36 Tb6 O42 135.4(2) . . ? C27 O6 Tb1 138.8(6) . . ? C28 N6 N5 106.7(6) . . ? C11 C6 N1 120.8(8) . . ? C11 C6 C7 120.0(9) . . ? N1 C6 C7 119.2(9) . . ? C40 O7 Tb2 130.6(6) . . ? C40 N7 N8 113.2(8) . . ? C40 N7 C43 128.6(8) . . ? N8 N7 C43 117.5(8) . . ? C8 C7 C6 119.4(10) . . ? C38 O8 Tb2 137.5(6) . . ? C41 N8 N7 104.9(8) . . ? C7 C8 C9 121.1(10) . . ? C49 O9 Tb1 130.3(6) . . ? C49 N9 N10 113.1(7) . . ? C49 N9 C54 128.7(7) . . ? N10 N9 C54 118.1(7) . . ? C10 C9 C8 118.8(9) . . ? C51 O10 Tb1 138.3(6) . . ? C52 N10 N9 106.1(7) . . ? C9 C10 C11 121.8(11) . . ? C64 O11 Tb2 128.7(6) . . ? C64 N11 N12 110.0(8) . . ? C64 N11 C67 129.3(8) . . ? N12 N11 C67 120.3(7) . . ? C6 C11 C10 118.7(9) . . ? C62 O12 Tb2 137.3(6) . . ? C65 N12 N11 107.0(7) . . ? C3 C12 C13 112.8(7) . . ? C73 N13 N14 110.1(7) . . ? C73 N13 C78 129.4(7) . . ? N14 N13 C78 120.1(7) . . ? C14 C13 C12 114.8(7) . . ? C76 N14 N13 106.1(7) . . ? O4 C14 C15 120.5(7) . . ? O4 C14 C13 118.6(7) . . ? C15 C14 C13 120.8(8) . . ? C73 O15 Tb3 127.5(6) . . ? C88 N15 N16 113.2(8) . . ? C88 N15 C91 127.0(9) . . ? N16 N15 C91 119.7(8) . . ? C14 C15 C16 122.6(8) . . ? C14 C15 C17 132.8(8) . . ? C16 C15 C17 104.6(7) . . ? C75 O16 Tb3 138.1(6) . . ? C89 N16 N15 104.8(7) . . ? O3 C16 N3 124.3(7) . . ? O3 C16 C15 129.6(8) . . ? N3 C16 C15 106.0(7) . . ? C88 O17 Tb4 126.0(6) . . ? C97 N17 N18 112.3(7) . . ? C97 N17 C102 128.9(8) . . ? N18 N17 C102 116.8(7) . . ? N4 C17 C15 111.3(8) . . ? N4 C17 C18 119.4(8) . . ? C15 C17 C18 129.3(8) . . ? C86 O18 Tb4 135.4(6) . . ? C100 N18 N17 105.9(7) . . ? C97 O19 Tb3 129.4(5) . . ? C112 N19 C115 129.9(7) . . ? C112 N19 N20 111.3(7) . . ? C115 N19 N20 118.7(7) . . ? C24 C19 C20 120.5(7) . . ? C24 C19 N3 120.3(8) . . ? C20 C19 N3 119.2(8) . . ? C99 O20 Tb3 139.9(6) . . ? C113 N20 N19 105.6(6) . . ? C21 C20 C19 119.4(8) . . ? C110 O21 Tb4 138.2(5) . . ? C121 N21 N22 111.2(7) . . ? C121 N21 C126 127.9(7) . . ? N22 N21 C126 120.2(7) . . ? C20 C21 C22 120.4(8) . . ? C112 O22 Tb4 130.6(5) . . ? C124 N22 N21 105.9(7) . . ? C23 C22 C21 119.4(8) . . ? C121 O23 Tb3 130.1(5) . . ? C136 N23 N24 111.8(7) . . ? C136 N23 C139 129.1(8) . . ? N24 N23 C139 119.1(7) . . ? C22 C23 C24 121.2(9) . . ? C123 O24 Tb3 140.4(5) . . ? C137 N24 N23 107.1(7) . . ? C19 C24 C23 119.0(8) . . ? C136 O25 Tb4 131.5(5) . . ? C145 N25 C150 128.2(7) . . ? C145 N25 N26 111.4(6) . . ? C150 N25 N26 120.3(7) . . ? O5 C25 N5 124.3(8) . . ? O5 C25 C26 131.4(8) . . ? N5 C25 C26 104.4(7) . . ? C134 O26 Tb4 139.4(6) . . ? C148 N26 N25 105.9(7) . . ? C25 C26 C27 122.2(7) . . ? C25 C26 C28 106.2(7) . . ? C27 C26 C28 131.5(8) . . ? C160 N27 N28 111.7(7) . . ? C160 N27 C163 129.8(8) . . ? N28 N27 C163 117.8(7) . . ? O6 C27 C26 120.5(8) . . ? O6 C27 C36 119.7(8) . . ? C26 C27 C36 119.7(7) . . ? C161 N28 N27 105.3(7) . . ? N6 C28 C26 110.9(7) . . ? N6 C28 C29 119.4(7) . . ? C26 C28 C29 129.7(8) . . ? C145 O29 Tb5 130.5(5) . . ? C169 N29 N30 111.1(7) . . ? C169 N29 C174 129.9(9) . . ? N30 N29 C174 118.9(8) . . ? C147 O30 Tb5 136.7(5) . . ? C31 C30 C35 120.4(8) . . ? C31 C30 N5 118.0(8) . . ? C35 C30 N5 121.6(7) . . ? C172 N30 N29 107.1(7) . . ? C160 O31 Tb6 128.0(5) . . ? N32 N31 C184 111.3(7) . . ? N32 N31 C187 121.2(6) . . ? C184 N31 C187 127.3(7) . . ? C32 C31 C30 118.6(9) . . ? C158 O32 Tb6 137.4(6) . . ? C185 N32 N31 106.5(7) . . ? C33 C32 C31 121.2(8) . . ? C169 O33 Tb5 124.0(6) . . ? C193 N33 N34 112.2(7) . . ? C193 N33 C198 128.5(8) . . ? N34 N33 C198 118.9(7) . . ? C32 C33 C34 119.1(9) . . ? C171 O34 Tb5 136.9(6) . . ? C196 N34 N33 105.9(7) . . ? C35 C34 C33 121.6(10) . . ? C184 O35 Tb6 128.8(5) . . ? C34 C35 C30 119.1(8) . . ? C208 N35 N36 111.4(7) . . ? C208 N35 C211 129.9(8) . . ? N36 N35 C211 118.6(8) . . ? C182 O36 Tb6 137.5(6) . . ? C27 C36 C37 115.7(8) . . ? C209 N36 N35 105.8(8) . . ? C193 O37 Tb5 131.3(5) . . ? C36 C37 C38 112.6(7) . . ? C195 O38 Tb5 138.3(6) . . ? O8 C38 C39 123.2(8) . . ? O8 C38 C37 115.8(8) . . ? C39 C38 C37 120.7(7) . . ? C208 O39 Tb6 131.2(5) . . ? C38 C39 C41 134.2(8) . . ? C38 C39 C40 121.0(8) . . ? C41 C39 C40 104.2(8) . . ? C206 O40 Tb6 139.4(5) . . ? O7 C40 N7 124.2(9) . . ? O7 C40 C39 131.0(9) . . ? N7 C40 C39 104.9(7) . . ? N8 C41 C39 112.8(8) . . ? N8 C41 C42 117.9(8) . . ? C39 C41 C42 129.2(9) . . ? C44 C43 C48 119.7(10) . . ? C44 C43 N7 120.5(9) . . ? C48 C43 N7 119.7(10) . . ? C43 C44 C45 119.6(11) . . ? C46 C45 C44 119.4(11) . . ? C47 C46 C45 120.4(11) . . ? C46 C47 C48 120.9(11) . . ? C43 C48 C47 119.7(12) . . ? O9 C49 N9 124.8(8) . . ? O9 C49 C50 130.7(8) . . ? N9 C49 C50 104.4(7) . . ? C51 C50 C49 122.5(8) . . ? C51 C50 C52 131.9(7) . . ? C49 C50 C52 105.6(7) . . ? O10 C51 C50 122.1(7) . . ? O10 C51 C60 116.3(8) . . ? C50 C51 C60 121.6(7) . . ? N10 C52 C50 110.8(7) . . ? N10 C52 C53 118.9(7) . . ? C50 C52 C53 130.3(8) . . ? C55 C54 C59 122.2(9) . . ? C55 C54 N9 120.0(8) . . ? C59 C54 N9 117.8(8) . . ? C54 C55 C56 120.6(8) . . ? C55 C56 C57 119.0(10) . . ? C58 C57 C56 120.3(9) . . ? C57 C58 C59 120.6(9) . . ? C54 C59 C58 117.4(9) . . ? C61 C60 C51 113.0(7) . . ? C62 C61 C60 115.5(8) . . ? O12 C62 C63 121.3(9) . . ? O12 C62 C61 118.2(8) . . ? C63 C62 C61 120.4(8) . . ? C64 C63 C65 105.8(8) . . ? C64 C63 C62 122.2(8) . . ? C65 C63 C62 131.6(9) . . ? O11 C64 N11 121.4(9) . . ? O11 C64 C63 132.1(8) . . ? N11 C64 C63 106.4(8) . . ? N12 C65 C63 110.8(8) . . ? N12 C65 C66 118.1(8) . . ? C63 C65 C66 131.2(9) . . ? C68 C67 C72 120.4(9) . . ? C68 C67 N11 121.4(7) . . ? C72 C67 N11 118.2(8) . . ? C67 C68 C69 120.2(8) . . ? C68 C69 C70 119.4(10) . . ? C71 C70 C69 120.0(10) . . ? C70 C71 C72 121.8(9) . . ? C67 C72 C71 118.2(10) . . ? O15 C73 N13 122.1(8) . . ? O15 C73 C74 129.5(8) . . ? N13 C73 C74 108.4(7) . . ? C73 C74 C75 124.6(7) . . ? C73 C74 C76 103.7(8) . . ? C75 C74 C76 131.5(8) . . ? O16 C75 C74 118.5(8) . . ? O16 C75 C84 118.2(8) . . ? C74 C75 C84 123.2(7) . . ? N14 C76 C74 111.7(8) . . ? N14 C76 C77 120.3(7) . . ? C74 C76 C77 128.1(8) . . ? C79 C78 C83 119.8(9) . . ? C79 C78 N13 119.7(8) . . ? C83 C78 N13 120.5(8) . . ? C78 C79 C80 118.4(9) . . ? C81 C80 C79 122.0(9) . . ? C80 C81 C82 118.8(10) . . ? C83 C82 C81 120.7(9) . . ? C82 C83 C78 120.1(9) . . ? C75 C84 C85 114.1(7) . . ? C86 C85 C84 112.5(7) . . ? O18 C86 C87 120.7(8) . . ? O18 C86 C85 119.9(8) . . ? C87 C86 C85 119.4(7) . . ? C89 C87 C88 105.4(8) . . ? C89 C87 C86 132.5(8) . . ? C88 C87 C86 121.9(7) . . ? O17 C88 N15 124.5(8) . . ? O17 C88 C87 131.4(8) . . ? N15 C88 C87 104.0(7) . . ? N16 C89 C87 112.5(8) . . ? N16 C89 C90 117.4(8) . . ? C87 C89 C90 130.2(9) . . ? C96 C91 C92 119.7(11) . . ? C96 C91 N15 117.7(11) . . ? C92 C91 N15 122.5(10) . . ? C93 C92 C91 119.7(11) . . ? C92 C93 C94 120.7(12) . . ? C95 C94 C93 118.3(11) . . ? C94 C95 C96 122.4(11) . . ? C95 C96 C91 119.1(12) . . ? O19 C97 N17 124.1(8) . . ? O19 C97 C98 131.1(8) . . ? N17 C97 C98 104.8(8) . . ? C97 C98 C100 105.6(7) . . ? C97 C98 C99 123.0(8) . . ? C100 C98 C99 131.4(8) . . ? O20 C99 C98 120.8(8) . . ? O20 C99 C108 118.1(7) . . ? C98 C99 C108 121.0(8) . . ? N18 C100 C98 111.4(8) . . ? N18 C100 C101 116.8(8) . . ? C98 C100 C101 131.8(8) . . ? C103 C102 N17 121.7(9) . . ? C103 C102 C107 119.8(9) . . ? N17 C102 C107 118.3(8) . . ? C102 C103 C104 120.9(11) . . ? C103 C104 C105 120.6(11) . . ? C104 C105 C106 119.5(10) . . ? C107 C106 C105 119.5(12) . . ? C106 C107 C102 119.6(11) . . ? C99 C108 C109 111.3(8) . . ? C110 C109 C108 115.4(7) . . ? O21 C110 C111 121.8(7) . . ? O21 C110 C109 118.1(7) . . ? C111 C110 C109 120.1(7) . . ? C112 C111 C110 123.0(7) . . ? C112 C111 C113 104.9(7) . . ? C110 C111 C113 131.8(8) . . ? O22 C112 N19 123.6(7) . . ? O22 C112 C111 130.6(7) . . ? N19 C112 C111 105.8(7) . . ? N20 C113 C111 112.4(7) . . ? N20 C113 C114 119.1(7) . . ? C111 C113 C114 128.5(8) . . ? C116 C115 C120 119.7(8) . . ? C116 C115 N19 120.2(8) . . ? C120 C115 N19 120.1(8) . . ? C115 C116 C117 120.1(9) . . ? C118 C117 C116 119.3(9) . . ? C119 C118 C117 120.3(8) . . ? C120 C119 C118 120.1(9) . . ? C119 C120 C115 120.4(9) . . ? O23 C121 N21 122.7(7) . . ? O23 C121 C122 132.5(7) . . ? N21 C121 C122 104.7(7) . . ? C121 C122 C124 106.7(7) . . ? C121 C122 C123 121.0(7) . . ? C124 C122 C123 132.1(8) . . ? O24 C123 C122 119.7(7) . . ? O24 C123 C132 121.0(7) . . ? C122 C123 C132 119.0(7) . . ? N22 C124 C122 111.4(7) . . ? N22 C124 C125 117.8(8) . . ? C122 C124 C125 130.8(8) . . ? C127 C126 C131 121.3(8) . . ? C127 C126 N21 120.4(8) . . ? C131 C126 N21 118.4(8) . . ? C128 C127 C126 119.1(9) . . ? C127 C128 C129 120.4(9) . . ? C128 C129 C130 120.0(9) . . ? C131 C130 C129 120.4(9) . . ? C130 C131 C126 118.9(9) . . ? C123 C132 C133 114.0(7) . . ? C134 C133 C132 112.4(8) . . ? O26 C134 C135 121.6(8) . . ? O26 C134 C133 117.3(7) . . ? C135 C134 C133 121.1(7) . . ? C134 C135 C136 122.1(8) . . ? C134 C135 C137 131.9(8) . . ? C136 C135 C137 105.9(7) . . ? O25 C136 N23 124.4(8) . . ? O25 C136 C135 130.6(7) . . ? N23 C136 C135 104.9(7) . . ? N24 C137 C135 110.4(8) . . ? N24 C137 C138 119.6(7) . . ? C135 C137 C138 130.0(8) . . ? C144 C139 C140 119.8(9) . . ? C144 C139 N23 119.1(9) . . ? C140 C139 N23 121.1(8) . . ? C141 C140 C139 119.8(9) . . ? C140 C141 C142 120.8(10) . . ? C143 C142 C141 118.4(9) . . ? C144 C143 C142 121.3(9) . . ? C143 C144 C139 119.8(10) . . ? O29 C145 N25 124.0(7) . . ? O29 C145 C146 130.0(8) . . ? N25 C145 C146 106.0(7) . . ? C145 C146 C147 123.2(7) . . ? C145 C146 C148 105.2(7) . . ? C147 C146 C148 131.5(7) . . ? O30 C147 C146 122.1(7) . . ? O30 C147 C156 119.2(7) . . ? C146 C147 C156 118.4(7) . . ? N26 C148 C146 111.5(7) . . ? N26 C148 C149 118.3(8) . . ? C146 C148 C149 130.1(7) . . ? C155 C150 N25 121.7(8) . . ? C155 C150 C151 119.4(8) . . ? N25 C150 C151 118.9(7) . . ? C152 C151 C150 119.8(8) . . ? C151 C152 C153 121.2(9) . . ? C152 C153 C154 118.9(8) . . ? C155 C154 C153 121.4(8) . . ? C154 C155 C150 119.2(8) . . ? C147 C156 C157 116.3(7) . . ? C158 C157 C156 112.8(7) . . ? O32 C158 C159 120.7(8) . . ? O32 C158 C157 116.8(7) . . ? C159 C158 C157 122.5(7) . . ? C160 C159 C158 124.3(7) . . ? C160 C159 C161 105.2(7) . . ? C158 C159 C161 130.4(8) . . ? O31 C160 N27 121.8(8) . . ? O31 C160 C159 132.3(7) . . ? N27 C160 C159 105.9(7) . . ? N28 C161 C159 111.9(8) . . ? N28 C161 C162 118.2(7) . . ? C159 C161 C162 130.0(8) . . ? C168 C163 C164 119.8(10) . . ? C168 C163 N27 120.8(9) . . ? C164 C163 N27 119.1(8) . . ? C163 C164 C165 120.1(9) . . ? C164 C165 C166 119.3(10) . . ? C167 C166 C165 120.3(10) . . ? C166 C167 C168 120.6(9) . . ? C163 C168 C167 119.9(10) . . ? O33 C169 N29 122.6(8) . . ? O33 C169 C170 132.4(8) . . ? N29 C169 C170 104.9(7) . . ? C169 C170 C171 123.8(8) . . ? C169 C170 C172 106.8(8) . . ? C171 C170 C172 129.4(9) . . ? O34 C171 C170 119.4(9) . . ? O34 C171 C180 118.1(8) . . ? C170 C171 C180 122.4(7) . . ? N30 C172 C170 110.0(9) . . ? N30 C172 C173 119.2(8) . . ? C170 C172 C173 130.8(9) . . ? C175 C174 C179 120.3(12) . . ? C175 C174 N29 121.7(10) . . ? C179 C174 N29 117.9(12) . . ? C174 C175 C176 120.9(12) . . ? C177 C176 C175 117.7(13) . . ? C178 C177 C176 123.0(13) . . ? C177 C178 C179 119.4(12) . . ? C174 C179 C178 118.7(12) . . ? C171 C180 C181 113.3(7) . . ? C180 C181 C182 112.7(7) . . ? O36 C182 C183 121.3(8) . . ? O36 C182 C181 117.9(7) . . ? C183 C182 C181 120.7(7) . . ? C182 C183 C184 122.3(8) . . ? C182 C183 C185 130.7(8) . . ? C184 C183 C185 106.7(7) . . ? O35 C184 C183 132.0(8) . . ? O35 C184 N31 123.5(7) . . ? C183 C184 N31 104.5(7) . . ? N32 C185 C183 110.9(7) . . ? N32 C185 C186 118.8(7) . . ? C183 C185 C186 130.3(8) . . ? C192 C187 N31 122.2(7) . . ? C192 C187 C188 119.3(8) . . ? N31 C187 C188 118.5(7) . . ? C189 C188 C187 118.7(8) . . ? C188 C189 C190 121.9(8) . . ? C191 C190 C189 118.3(9) . . ? C192 C191 C190 121.1(8) . . ? C191 C192 C187 120.4(7) . . ? O37 C193 N33 124.4(8) . . ? O37 C193 C194 130.7(8) . . ? N33 C193 C194 104.9(8) . . ? C195 C194 C193 122.1(8) . . ? C195 C194 C196 132.4(8) . . ? C193 C194 C196 105.3(7) . . ? O38 C195 C194 121.9(8) . . ? O38 C195 C204 117.7(8) . . ? C194 C195 C204 120.3(8) . . ? N34 C196 C194 111.7(8) . . ? N34 C196 C197 119.5(8) . . ? C194 C196 C197 128.8(8) . . ? C199 C198 C203 119.9(8) . . ? C199 C198 N33 121.5(8) . . ? C203 C198 N33 118.6(8) . . ? C198 C199 C200 120.5(8) . . ? C199 C200 C201 119.5(9) . . ? C202 C201 C200 120.0(9) . . ? C203 C202 C201 121.0(9) . . ? C202 C203 C198 119.1(9) . . ? C195 C204 C205 113.8(8) . . ? C206 C205 C204 112.9(8) . . ? O40 C206 C207 121.1(7) . . ? O40 C206 C205 118.1(8) . . ? C207 C206 C205 120.8(8) . . ? C206 C207 C208 123.8(8) . . ? C206 C207 C209 131.8(7) . . ? C208 C207 C209 104.2(7) . . ? O39 C208 N35 124.4(7) . . ? O39 C208 C207 129.0(8) . . ? N35 C208 C207 106.6(7) . . ? N36 C209 C207 111.9(8) . . ? N36 C209 C210 116.9(9) . . ? C207 C209 C210 131.1(8) . . ? C216 C211 C212 120.4(9) . . ? C216 C211 N35 120.0(9) . . ? C212 C211 N35 119.6(9) . . ? C211 C212 C213 120.0(11) . . ? C214 C213 C212 118.9(11) . . ? C215 C214 C213 121.8(10) . . ? C214 C215 C216 119.6(11) . . ? C211 C216 C215 119.1(11) . . ? O47 C217 C218 113.8(11) . . ? _diffrn_measured_fraction_theta_max 0.920 _diffrn_reflns_theta_full 28.70 _diffrn_measured_fraction_theta_full 0.920 _refine_diff_density_max 4.167 _refine_diff_density_min -4.524 _refine_diff_density_rms 0.238 # Attachment 'Structure2.CIF' data_Tb2q2qDMF _database_code_depnum_ccdc_archive 'CCDC 670981' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Tb2(Q2Q)3(DMF)2) _chemical_melting_point ? _chemical_formula_moiety '[Tb2(C24H20N4O4)3(C3H7NO)2]' _chemical_formula_sum 'C78 H74 N14 O14 Tb2' _chemical_formula_weight 1749.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.807(3) _cell_length_b 14.379(3) _cell_length_c 21.830(4) _cell_angle_alpha 96.03(3) _cell_angle_beta 90.17(3) _cell_angle_gamma 111.71(3) _cell_volume 3710.4(13) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 32278 _cell_measurement_theta_min 2.2813 _cell_measurement_theta_max 32.7980 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.566 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1764 _exptl_absorpt_coefficient_mu 1.966 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.748 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(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 IPDS(Stoe) _diffrn_measurement_method '\f oscillation scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 101982 _diffrn_reflns_av_R_equivalents 0.0877 _diffrn_reflns_av_sigmaI/netI 0.0799 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 27.10 _reflns_number_total 16377 _reflns_number_gt 12763 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Two phenyl rings have been found to be disordered over two positions. They were anisotropically refined with the same occupancy with help of AFIX and EADP procedures in the frame of SHELXL-97 program. ; _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^)+(0.0877P)^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 16377 _refine_ls_number_parameters 893 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1187 _refine_ls_R_factor_gt 0.0785 _refine_ls_wR_factor_ref 0.1774 _refine_ls_wR_factor_gt 0.1610 _refine_ls_goodness_of_fit_ref 1.203 _refine_ls_restrained_S_all 1.203 _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 Tb1 Tb 0.48133(3) 0.08451(3) 0.256264(16) 0.02336(11) Uani 1 1 d . . . O1 O 0.4059(4) 0.1238(4) 0.3460(2) 0.0256(11) Uani 1 1 d . . . N1 N 0.2955(5) 0.1014(5) 0.4312(3) 0.0284(15) Uani 1 1 d . . . C1 C 0.3250(6) 0.0679(6) 0.3754(3) 0.0251(16) Uani 1 1 d . . . Tb2 Tb 0.40996(3) -0.36906(3) 0.247544(15) 0.02246(11) Uani 1 1 d . . . O2 O 0.3222(4) -0.0589(4) 0.2659(2) 0.0298(12) Uani 1 1 d . . . C2 C 0.2464(6) -0.0314(6) 0.3597(3) 0.0249(17) Uani 1 1 d . . . N2 N 0.1990(6) 0.0280(5) 0.4522(3) 0.0368(17) Uani 1 1 d . . . O3 O 0.3286(4) -0.4260(4) 0.1507(2) 0.0311(13) Uani 1 1 d . . . N3 N 0.2380(6) -0.4272(6) 0.0581(3) 0.0396(18) Uani 1 1 d . . . C3 C 0.1706(7) -0.0499(7) 0.4101(4) 0.0342(19) Uani 1 1 d . . . O4 O 0.2778(4) -0.2940(4) 0.2386(2) 0.0299(12) Uani 1 1 d . . . N4 N 0.1682(6) -0.3817(5) 0.0349(3) 0.0393(18) Uani 1 1 d . A . C4 C 0.0725(7) -0.1423(7) 0.4202(4) 0.046(2) Uani 1 1 d . . . H4B H 0.0384 -0.1301 0.4577 0.069 Uiso 1 1 calc R . . H4C H 0.0975 -0.1970 0.4231 0.069 Uiso 1 1 calc R . . H4D H 0.0185 -0.1593 0.3862 0.069 Uiso 1 1 calc R . . O5 O 0.3749(4) 0.0669(4) 0.1675(2) 0.0334(13) Uani 1 1 d . . . N5 N 0.2889(5) 0.0049(5) 0.0699(3) 0.0316(16) Uani 1 1 d . . . C5 C 0.3393(7) 0.1989(6) 0.4656(3) 0.0291(18) Uani 1 1 d . . . O6 O 0.5338(4) -0.0216(4) 0.1855(2) 0.0279(12) Uani 1 1 d . . . N6 N 0.2997(6) -0.0550(6) 0.0178(3) 0.0383(18) Uani 1 1 d . B . C6 C 0.4522(7) 0.2591(6) 0.4634(3) 0.0320(19) Uani 1 1 d . . . H6B H 0.4997 0.2369 0.4391 0.038 Uiso 1 1 calc R . . O7 O 0.5788(4) -0.3841(4) 0.2554(2) 0.0304(13) Uani 1 1 d . B . N7 N 0.7737(5) -0.3326(5) 0.2647(3) 0.0266(14) Uani 1 1 d . B . C7 C 0.4927(8) 0.3515(7) 0.4976(4) 0.042(2) Uani 1 1 d . . . H7A H 0.5680 0.3928 0.4959 0.050 Uiso 1 1 calc R . . O8 O 0.5290(4) -0.2457(4) 0.1891(2) 0.0268(12) Uani 1 1 d . B . N8 N 0.8701(5) -0.2573(5) 0.2459(3) 0.0337(16) Uani 1 1 d . B . C8 C 0.4231(10) 0.3840(8) 0.5346(5) 0.063(3) Uani 1 1 d . . . H8B H 0.4520 0.4463 0.5583 0.076 Uiso 1 1 calc R . . O9 O 0.6711(4) 0.1678(4) 0.2498(2) 0.0271(12) Uani 1 1 d . . . N9 N 0.8562(5) 0.1781(5) 0.2431(3) 0.0272(14) Uani 1 1 d . . . C9 C 0.3105(10) 0.3243(10) 0.5365(6) 0.081(4) Uani 1 1 d . . . H9A H 0.2629 0.3464 0.5608 0.097 Uiso 1 1 calc R . . O10 O 0.5628(4) 0.0153(4) 0.3241(2) 0.0267(12) Uani 1 1 d . . . N10 N 0.9287(5) 0.1383(5) 0.2688(3) 0.0273(14) Uani 1 1 d . . . C10 C 0.2699(9) 0.2311(8) 0.5015(5) 0.053(3) Uani 1 1 d . . . H10B H 0.1943 0.1901 0.5025 0.064 Uiso 1 1 calc R . . O11 O 0.3149(4) -0.4148(4) 0.3347(2) 0.0286(12) Uani 1 1 d . . . C11 C 0.2452(6) -0.0896(6) 0.3022(4) 0.0268(17) Uani 1 1 d . . . N11 N 0.2307(5) -0.3930(5) 0.4266(3) 0.0302(15) Uani 1 1 d . . . O12 O 0.4957(4) -0.2316(4) 0.3236(2) 0.0322(13) Uani 1 1 d . . . N12 N 0.2401(5) -0.3175(5) 0.4742(3) 0.0341(16) Uani 1 1 d . . . C12 C 0.1501(6) -0.1882(6) 0.2839(4) 0.0291(18) Uani 1 1 d . . . H12B H 0.0797 -0.1814 0.2948 0.035 Uiso 1 1 calc R . . H12C H 0.1589 -0.2392 0.3070 0.035 Uiso 1 1 calc R . . O13 O 0.4975(5) 0.2481(4) 0.2441(3) 0.0396(14) Uani 1 1 d . . . C13 C 0.1448(6) -0.2229(6) 0.2154(4) 0.0304(18) Uani 1 1 d . . . H13A H 0.0677 -0.2652 0.2027 0.037 Uiso 1 1 calc R . . H13B H 0.1662 -0.1643 0.1930 0.037 Uiso 1 1 calc R . . N13 N 0.5479(10) 0.3480(7) 0.1678(4) 0.0729(17) Uani 1 1 d . . . O14 O 0.3603(5) -0.5429(4) 0.2406(3) 0.0397(14) Uani 1 1 d . . . C14 C 0.2190(6) -0.2805(6) 0.1975(4) 0.0254(17) Uani 1 1 d . A . N14 N 0.2940(5) -0.6749(5) 0.2962(3) 0.0372(17) Uani 1 1 d . . . C15 C 0.2685(7) -0.3925(6) 0.1188(3) 0.0286(18) Uani 1 1 d . A . C16 C 0.2160(6) -0.3241(6) 0.1355(3) 0.0276(17) Uani 1 1 d . . . C17 C 0.1560(7) -0.3205(6) 0.0807(4) 0.0327(19) Uani 1 1 d . A . C18 C 0.0875(8) -0.2598(7) 0.0695(4) 0.045(2) Uani 1 1 d . . . H18A H 0.0640 -0.2710 0.0267 0.067 Uiso 1 1 calc R A . H18B H 0.1318 -0.1896 0.0805 0.067 Uiso 1 1 calc R . . H18C H 0.0225 -0.2793 0.0941 0.067 Uiso 1 1 calc R . . C19 C 0.2784(13) -0.4939(10) 0.0194(6) 0.0624(18) Uani 0.50 1 d PG A 1 C20 C 0.3847(12) -0.4969(10) 0.0278(5) 0.0624(18) Uani 0.50 1 d PG A 1 H20 H 0.4341 -0.4538 0.0590 0.075 Uiso 0.50 1 calc PR A 1 C21 C 0.4172(10) -0.5642(11) -0.0103(6) 0.0624(18) Uani 0.50 1 d PG A 1 H21 H 0.4883 -0.5662 -0.0046 0.075 Uiso 0.50 1 calc PR A 1 C22 C 0.3434(13) -0.6285(10) -0.0568(5) 0.0624(18) Uani 0.50 1 d PG A 1 H22 H 0.3651 -0.6736 -0.0823 0.075 Uiso 0.50 1 calc PR A 1 C23 C 0.2371(12) -0.6256(10) -0.0653(6) 0.0624(18) Uani 0.50 1 d PG A 1 H23 H 0.1877 -0.6686 -0.0964 0.075 Uiso 0.50 1 calc PR A 1 C24 C 0.2046(11) -0.5583(12) -0.0271(7) 0.0624(18) Uani 0.50 1 d PG A 1 H24 H 0.1335 -0.5563 -0.0328 0.075 Uiso 0.50 1 calc PR A 1 C19A C 0.2379(15) -0.5114(10) 0.0199(6) 0.0624(18) Uani 0.50 1 d PG A 2 C20A C 0.2912(13) -0.5708(11) 0.0415(5) 0.0624(18) Uani 0.50 1 d PG A 2 H20A H 0.3192 -0.5583 0.0821 0.075 Uiso 0.50 1 calc PR A 2 C21A C 0.3027(13) -0.6488(11) 0.0023(6) 0.0624(18) Uani 0.50 1 d PG A 2 H21A H 0.3384 -0.6885 0.0168 0.075 Uiso 0.50 1 calc PR A 2 C22A C 0.2608(14) -0.6674(10) -0.0584(5) 0.0624(18) Uani 0.50 1 d PG A 2 H22A H 0.2685 -0.7196 -0.0846 0.075 Uiso 0.50 1 calc PR A 2 C23A C 0.2075(14) -0.6080(11) -0.0800(5) 0.0624(18) Uani 0.50 1 d PG A 2 H23A H 0.1795 -0.6204 -0.1206 0.075 Uiso 0.50 1 calc PR A 2 C24A C 0.1960(14) -0.5300(11) -0.0408(6) 0.0624(18) Uani 0.50 1 d PG A 2 H24A H 0.1604 -0.4902 -0.0552 0.075 Uiso 0.50 1 calc PR A 2 C25 C 0.3635(6) 0.0105(6) 0.1177(3) 0.0246(17) Uani 1 1 d . B . C26 C 0.4210(6) -0.0519(6) 0.0949(3) 0.0242(16) Uani 1 1 d . . . C27 C 0.3781(6) -0.0894(6) 0.0330(3) 0.0305(18) Uani 1 1 d . B . C28 C 0.4064(7) -0.1593(7) -0.0132(4) 0.039(2) Uani 1 1 d . . . H28A H 0.3628 -0.1690 -0.0508 0.059 Uiso 1 1 calc R B . H28B H 0.3896 -0.2229 0.0025 0.059 Uiso 1 1 calc R . . H28C H 0.4850 -0.1310 -0.0210 0.059 Uiso 1 1 calc R . . C29 C 0.2146(14) 0.0587(13) 0.0732(8) 0.0441(16) Uani 0.50 1 d PG B 1 C30 C 0.1982(10) 0.1036(11) 0.0225(6) 0.0441(16) Uani 0.50 1 d PG B 1 H30 H 0.2352 0.0983 -0.0135 0.053 Uiso 0.50 1 calc PR B 1 C31 C 0.1264(10) 0.1564(11) 0.0257(5) 0.0441(16) Uani 0.50 1 d PG B 1 H31 H 0.1155 0.1864 -0.0082 0.053 Uiso 0.50 1 calc PR B 1 C32 C 0.0711(10) 0.1643(10) 0.0795(5) 0.0441(16) Uani 0.50 1 d PG B 1 H32 H 0.0231 0.1996 0.0817 0.053 Uiso 0.50 1 calc PR B 1 C33 C 0.0875(14) 0.1194(15) 0.1302(5) 0.0441(16) Uani 0.50 1 d PG B 1 H33 H 0.0504 0.1246 0.1662 0.053 Uiso 0.50 1 calc PR B 1 C34 C 0.1593(17) 0.0665(17) 0.1270(7) 0.0441(16) Uani 0.50 1 d PG B 1 H34 H 0.1702 0.0365 0.1608 0.053 Uiso 0.50 1 calc PR B 1 C29A C 0.2052(12) 0.0453(12) 0.0658(7) 0.0441(16) Uani 0.50 1 d PG B 2 C30A C 0.1592(10) 0.0473(10) 0.0084(6) 0.0441(16) Uani 0.50 1 d PG B 2 H30A H 0.1855 0.0236 -0.0273 0.053 Uiso 0.50 1 calc PR B 2 C31A C 0.0740(9) 0.0847(11) 0.0043(5) 0.0441(16) Uani 0.50 1 d PG B 2 H31A H 0.0432 0.0860 -0.0341 0.053 Uiso 0.50 1 calc PR B 2 C32A C 0.0347(10) 0.1200(11) 0.0575(5) 0.0441(16) Uani 0.50 1 d PG B 2 H32A H -0.0223 0.1450 0.0548 0.053 Uiso 0.50 1 calc PR B 2 C33A C 0.0807(13) 0.1181(13) 0.1149(5) 0.0441(16) Uani 0.50 1 d PG B 2 H33A H 0.0544 0.1417 0.1506 0.053 Uiso 0.50 1 calc PR B 2 C34A C 0.1660(15) 0.0807(14) 0.1190(6) 0.038(5) Uani 0.50 1 d PG B 2 H34A H 0.1967 0.0794 0.1574 0.046 Uiso 0.50 1 calc PR B 2 C35 C 0.5109(6) -0.0607(6) 0.1308(3) 0.0233(16) Uani 1 1 d . B . C36 C 0.5818(6) -0.1145(6) 0.1018(3) 0.0267(17) Uani 1 1 d . . . H36A H 0.6168 -0.0815 0.0665 0.032 Uiso 1 1 calc R B . H36B H 0.5334 -0.1830 0.0868 0.032 Uiso 1 1 calc R . . C37 C 0.6738(6) -0.1176(6) 0.1455(3) 0.0254(17) Uani 1 1 d . B . H37A H 0.7343 -0.1249 0.1214 0.030 Uiso 1 1 calc R . . H37B H 0.7042 -0.0541 0.1718 0.030 Uiso 1 1 calc R . . C38 C 0.6329(6) -0.2023(5) 0.1857(3) 0.0210(15) Uani 1 1 d . . . C39 C 0.6775(6) -0.3207(6) 0.2460(3) 0.0232(11) Uani 1 1 d . . . C40 C 0.7122(6) -0.2341(6) 0.2154(3) 0.0232(11) Uani 1 1 d . B . C41 C 0.8321(6) -0.1996(6) 0.2160(4) 0.0277(17) Uani 1 1 d . . . C42 C 0.9167(7) -0.1111(7) 0.1895(4) 0.043(2) Uani 1 1 d . B . H42A H 0.9909 -0.1012 0.2046 0.064 Uiso 1 1 calc R . . H42B H 0.9009 -0.0517 0.2017 0.064 Uiso 1 1 calc R . . H42C H 0.9121 -0.1240 0.1453 0.064 Uiso 1 1 calc R . . C43 C 0.7867(6) -0.4123(6) 0.2929(4) 0.0315(18) Uani 1 1 d . . . C44 C 0.7035(7) -0.4725(7) 0.3261(4) 0.042(2) Uani 1 1 d . B . H44A H 0.6373 -0.4605 0.3308 0.051 Uiso 1 1 calc R . . C45 C 0.7159(9) -0.5515(8) 0.3529(4) 0.052(3) Uani 1 1 d . . . H45A H 0.6586 -0.5916 0.3756 0.062 Uiso 1 1 calc R B . C46 C 0.8131(9) -0.5698(8) 0.3457(5) 0.054(3) Uani 1 1 d . B . H46A H 0.8229 -0.6219 0.3639 0.065 Uiso 1 1 calc R . . C47 C 0.8959(11) -0.5102(11) 0.3115(7) 0.092(5) Uani 1 1 d . . . H47A H 0.9617 -0.5227 0.3063 0.110 Uiso 1 1 calc R B . C48 C 0.8832(9) -0.4319(9) 0.2846(6) 0.072(4) Uani 1 1 d . B . H48A H 0.9396 -0.3928 0.2611 0.086 Uiso 1 1 calc R . . C49 C 0.7504(6) 0.1389(6) 0.2639(3) 0.0225(16) Uani 1 1 d . . . C50 C 0.7540(6) 0.0688(6) 0.3044(3) 0.0226(16) Uani 1 1 d . . . C51 C 0.8667(6) 0.0746(6) 0.3053(3) 0.0276(17) Uani 1 1 d . . . C52 C 0.9207(7) 0.0174(7) 0.3407(4) 0.041(2) Uani 1 1 d . . . H52A H 0.9975 0.0347 0.3297 0.062 Uiso 1 1 calc R . . H52B H 0.8805 -0.0537 0.3306 0.062 Uiso 1 1 calc R . . H52C H 0.9182 0.0351 0.3841 0.062 Uiso 1 1 calc R . . C53 C 0.8972(6) 0.2523(6) 0.2021(3) 0.0281(18) Uani 1 1 d . . . C54 C 0.8346(7) 0.2516(7) 0.1510(4) 0.042(2) Uani 1 1 d . . . H54A H 0.7634 0.2018 0.1428 0.050 Uiso 1 1 calc R . . C55 C 0.8774(8) 0.3252(9) 0.1113(4) 0.057(3) Uani 1 1 d . . . H55A H 0.8345 0.3246 0.0767 0.068 Uiso 1 1 calc R . . C56 C 0.9821(7) 0.3985(7) 0.1230(4) 0.046(2) Uani 1 1 d . . . H56A H 1.0096 0.4490 0.0972 0.056 Uiso 1 1 calc R . . C57 C 1.0457(8) 0.3969(7) 0.1726(5) 0.051(3) Uani 1 1 d . . . H57A H 1.1189 0.4439 0.1792 0.061 Uiso 1 1 calc R . . C58 C 1.0027(7) 0.3261(7) 0.2132(4) 0.041(2) Uani 1 1 d . . . H58A H 1.0452 0.3284 0.2484 0.049 Uiso 1 1 calc R . . C59 C 0.6569(6) 0.0098(5) 0.3347(3) 0.0231(16) Uani 1 1 d . . . C60 C 0.6637(6) -0.0599(6) 0.3794(3) 0.0271(17) Uani 1 1 d . . . H60A H 0.7223 -0.0228 0.4108 0.033 Uiso 1 1 calc R . . H60B H 0.6844 -0.1127 0.3579 0.033 Uiso 1 1 calc R . . C61 C 0.5526(6) -0.1079(6) 0.4104(3) 0.0305(18) Uani 1 1 d . . . H61A H 0.5688 -0.1247 0.4503 0.037 Uiso 1 1 calc R . . H61B H 0.5179 -0.0583 0.4175 0.037 Uiso 1 1 calc R . . C62 C 0.4698(6) -0.2008(6) 0.3747(3) 0.0246(16) Uani 1 1 d . . . C63 C 0.3052(6) -0.3575(6) 0.3820(3) 0.0254(17) Uani 1 1 d . . . C64 C 0.3682(6) -0.2562(6) 0.4021(3) 0.0231(16) Uani 1 1 d . . . C65 C 0.3222(6) -0.2364(6) 0.4594(4) 0.0316(18) Uani 1 1 d . . . C66 C 0.3486(7) -0.1415(7) 0.5012(4) 0.044(2) Uani 1 1 d . . . H66A H 0.2974 -0.1529 0.5342 0.065 Uiso 1 1 calc R . . H66B H 0.3410 -0.0904 0.4785 0.065 Uiso 1 1 calc R . . H66C H 0.4243 -0.1197 0.5180 0.065 Uiso 1 1 calc R . . C67 C 0.1580(6) -0.4950(6) 0.4329(4) 0.0300(18) Uani 1 1 d . . . C68 C 0.1185(7) -0.5653(7) 0.3834(4) 0.041(2) Uani 1 1 d . . . H68A H 0.1400 -0.5485 0.3441 0.050 Uiso 1 1 calc R . . C69 C 0.0454(8) -0.6630(7) 0.3912(4) 0.048(2) Uani 1 1 d . . . H69A H 0.0194 -0.7114 0.3572 0.057 Uiso 1 1 calc R . . C70 C 0.0125(8) -0.6871(8) 0.4486(5) 0.050(3) Uani 1 1 d . . . H70A H -0.0368 -0.7517 0.4541 0.060 Uiso 1 1 calc R . . C71 C 0.0527(9) -0.6155(9) 0.4980(5) 0.068(3) Uani 1 1 d . . . H71A H 0.0315 -0.6316 0.5374 0.081 Uiso 1 1 calc R . . C72 C 0.1246(8) -0.5192(8) 0.4899(4) 0.054(3) Uani 1 1 d . . . H72A H 0.1504 -0.4707 0.5238 0.065 Uiso 1 1 calc R . . C73 C 0.5682(12) 0.3159(9) 0.2184(5) 0.0729(17) Uani 1 1 d . . . H73 H 0.6404 0.3457 0.2365 0.087 Uiso 1 1 calc R . . C74 C 0.4403(11) 0.3079(9) 0.1346(5) 0.0729(17) Uani 1 1 d . . . H74A H 0.3881 0.2565 0.1561 0.109 Uiso 1 1 calc R . . H74B H 0.4484 0.2796 0.0939 0.109 Uiso 1 1 calc R . . H74C H 0.4126 0.3610 0.1318 0.109 Uiso 1 1 calc R . . C75 C 0.6337(11) 0.4330(9) 0.1443(5) 0.0729(17) Uani 1 1 d . . . H75A H 0.7017 0.4534 0.1696 0.109 Uiso 1 1 calc R . . H75B H 0.6082 0.4880 0.1452 0.109 Uiso 1 1 calc R . . H75C H 0.6480 0.4138 0.1027 0.109 Uiso 1 1 calc R . . C76 C 0.2951(7) -0.6288(7) 0.2476(4) 0.036(2) Uani 1 1 d . . . H76 H 0.2423 -0.6635 0.2157 0.043 Uiso 1 1 calc R . . C77 C 0.3762(8) -0.6249(9) 0.3479(4) 0.058(3) Uani 1 1 d . . . H77A H 0.4248 -0.5595 0.3385 0.086 Uiso 1 1 calc R . . H77B H 0.4202 -0.6647 0.3544 0.086 Uiso 1 1 calc R . . H77C H 0.3372 -0.6178 0.3845 0.086 Uiso 1 1 calc R . . C78 C 0.2199(8) -0.7790(7) 0.2996(6) 0.061(3) Uani 1 1 d . . . H78A H 0.1638 -0.8002 0.2664 0.092 Uiso 1 1 calc R . . H78B H 0.1839 -0.7842 0.3383 0.092 Uiso 1 1 calc R . . H78C H 0.2630 -0.8214 0.2963 0.092 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 Tb1 0.02072(19) 0.0284(2) 0.0235(2) 0.00783(16) 0.00206(14) 0.01080(16) O1 0.028(3) 0.021(3) 0.026(3) 0.007(2) 0.004(2) 0.007(2) N1 0.032(3) 0.028(4) 0.027(3) 0.006(3) 0.003(3) 0.013(3) C1 0.025(4) 0.030(4) 0.025(4) 0.006(3) 0.001(3) 0.014(3) Tb2 0.02125(19) 0.0272(2) 0.02184(19) 0.00956(15) 0.00162(14) 0.01051(15) O2 0.026(3) 0.033(3) 0.030(3) 0.001(2) 0.004(2) 0.011(2) C2 0.024(4) 0.026(4) 0.029(4) 0.015(3) 0.006(3) 0.012(3) N2 0.042(4) 0.037(4) 0.033(4) 0.012(3) 0.017(3) 0.013(3) O3 0.041(3) 0.040(3) 0.022(3) 0.010(2) 0.001(2) 0.024(3) N3 0.067(5) 0.041(4) 0.019(3) 0.009(3) -0.007(3) 0.028(4) C3 0.036(4) 0.036(5) 0.035(5) 0.015(4) 0.009(4) 0.015(4) O4 0.028(3) 0.040(3) 0.026(3) 0.003(2) 0.001(2) 0.017(2) N4 0.057(5) 0.033(4) 0.029(4) 0.008(3) -0.010(3) 0.017(4) C4 0.048(5) 0.045(6) 0.040(5) 0.007(4) 0.015(4) 0.011(4) O5 0.034(3) 0.042(4) 0.033(3) 0.004(3) -0.003(2) 0.023(3) N5 0.024(3) 0.049(5) 0.025(3) 0.009(3) -0.003(3) 0.016(3) C5 0.036(4) 0.036(5) 0.019(4) 0.003(3) -0.005(3) 0.018(4) O6 0.026(3) 0.035(3) 0.029(3) 0.009(2) -0.004(2) 0.018(2) N6 0.033(4) 0.049(5) 0.032(4) 0.007(3) -0.005(3) 0.013(3) C6 0.045(5) 0.039(5) 0.022(4) 0.009(4) -0.002(3) 0.025(4) O7 0.022(3) 0.035(3) 0.037(3) 0.014(3) -0.002(2) 0.011(2) N7 0.030(3) 0.024(4) 0.034(4) 0.016(3) 0.000(3) 0.016(3) C7 0.057(6) 0.035(5) 0.034(5) 0.004(4) -0.013(4) 0.018(4) O8 0.020(3) 0.030(3) 0.035(3) 0.013(2) 0.002(2) 0.013(2) N8 0.022(3) 0.036(4) 0.044(4) 0.010(3) -0.005(3) 0.010(3) C8 0.077(8) 0.042(6) 0.061(7) -0.025(5) -0.003(6) 0.019(6) O9 0.033(3) 0.026(3) 0.027(3) 0.016(2) 0.005(2) 0.013(2) N9 0.023(3) 0.032(4) 0.028(3) 0.012(3) 0.000(3) 0.009(3) C9 0.069(8) 0.067(9) 0.097(10) -0.033(7) 0.017(7) 0.024(7) O10 0.020(3) 0.032(3) 0.028(3) 0.017(2) 0.002(2) 0.006(2) N10 0.022(3) 0.031(4) 0.030(3) 0.012(3) -0.004(3) 0.010(3) C10 0.052(6) 0.054(7) 0.053(6) -0.012(5) 0.003(5) 0.024(5) O11 0.026(3) 0.029(3) 0.028(3) 0.009(2) 0.001(2) 0.005(2) C11 0.019(4) 0.027(4) 0.037(4) 0.010(4) -0.002(3) 0.010(3) N11 0.027(3) 0.035(4) 0.028(3) 0.006(3) 0.008(3) 0.010(3) O12 0.027(3) 0.031(3) 0.036(3) 0.013(3) 0.002(2) 0.005(2) N12 0.029(3) 0.031(4) 0.038(4) -0.002(3) 0.008(3) 0.007(3) C12 0.018(4) 0.034(5) 0.039(5) 0.004(4) 0.000(3) 0.014(3) O13 0.037(3) 0.031(3) 0.050(4) 0.011(3) 0.000(3) 0.010(3) C13 0.019(4) 0.032(5) 0.040(5) 0.005(4) -0.001(3) 0.008(3) N13 0.115(5) 0.060(4) 0.048(3) 0.013(3) 0.006(3) 0.035(3) O14 0.050(4) 0.036(4) 0.036(3) 0.011(3) 0.008(3) 0.017(3) C14 0.017(3) 0.027(4) 0.033(4) 0.007(3) -0.005(3) 0.008(3) N14 0.028(3) 0.030(4) 0.059(5) 0.022(4) 0.000(3) 0.012(3) C15 0.038(4) 0.030(5) 0.017(4) 0.006(3) 0.002(3) 0.010(4) C16 0.029(4) 0.030(4) 0.025(4) 0.009(3) -0.003(3) 0.012(3) C17 0.038(4) 0.032(5) 0.029(4) 0.013(4) -0.003(3) 0.011(4) C18 0.048(5) 0.052(6) 0.041(5) 0.016(4) -0.011(4) 0.023(5) C19 0.103(5) 0.068(5) 0.035(3) -0.003(3) -0.007(3) 0.056(4) C20 0.103(5) 0.068(5) 0.035(3) -0.003(3) -0.007(3) 0.056(4) C21 0.103(5) 0.068(5) 0.035(3) -0.003(3) -0.007(3) 0.056(4) C22 0.103(5) 0.068(5) 0.035(3) -0.003(3) -0.007(3) 0.056(4) C23 0.103(5) 0.068(5) 0.035(3) -0.003(3) -0.007(3) 0.056(4) C24 0.103(5) 0.068(5) 0.035(3) -0.003(3) -0.007(3) 0.056(4) C19A 0.103(5) 0.068(5) 0.035(3) -0.003(3) -0.007(3) 0.056(4) C20A 0.103(5) 0.068(5) 0.035(3) -0.003(3) -0.007(3) 0.056(4) C21A 0.103(5) 0.068(5) 0.035(3) -0.003(3) -0.007(3) 0.056(4) C22A 0.103(5) 0.068(5) 0.035(3) -0.003(3) -0.007(3) 0.056(4) C23A 0.103(5) 0.068(5) 0.035(3) -0.003(3) -0.007(3) 0.056(4) C24A 0.103(5) 0.068(5) 0.035(3) -0.003(3) -0.007(3) 0.056(4) C25 0.022(4) 0.027(4) 0.029(4) 0.013(3) 0.002(3) 0.011(3) C26 0.022(4) 0.027(4) 0.021(4) 0.010(3) -0.001(3) 0.004(3) C27 0.025(4) 0.039(5) 0.025(4) 0.013(4) 0.002(3) 0.007(3) C28 0.038(5) 0.048(6) 0.027(4) 0.002(4) -0.007(4) 0.011(4) C29 0.033(3) 0.068(4) 0.044(4) 0.021(3) 0.005(3) 0.029(3) C30 0.033(3) 0.068(4) 0.044(4) 0.021(3) 0.005(3) 0.029(3) C31 0.033(3) 0.068(4) 0.044(4) 0.021(3) 0.005(3) 0.029(3) C32 0.033(3) 0.068(4) 0.044(4) 0.021(3) 0.005(3) 0.029(3) C33 0.033(3) 0.068(4) 0.044(4) 0.021(3) 0.005(3) 0.029(3) C34 0.033(3) 0.068(4) 0.044(4) 0.021(3) 0.005(3) 0.029(3) C29A 0.033(3) 0.068(4) 0.044(4) 0.021(3) 0.005(3) 0.029(3) C30A 0.033(3) 0.068(4) 0.044(4) 0.021(3) 0.005(3) 0.029(3) C31A 0.033(3) 0.068(4) 0.044(4) 0.021(3) 0.005(3) 0.029(3) C32A 0.033(3) 0.068(4) 0.044(4) 0.021(3) 0.005(3) 0.029(3) C33A 0.033(3) 0.068(4) 0.044(4) 0.021(3) 0.005(3) 0.029(3) C34A 0.045(11) 0.031(11) 0.038(10) -0.005(8) -0.027(9) 0.017(9) C35 0.024(4) 0.024(4) 0.024(4) 0.010(3) 0.002(3) 0.009(3) C36 0.034(4) 0.030(4) 0.022(4) 0.013(3) 0.006(3) 0.016(3) C37 0.024(4) 0.028(4) 0.032(4) 0.012(3) 0.010(3) 0.017(3) C38 0.024(4) 0.023(4) 0.016(3) 0.001(3) 0.001(3) 0.010(3) C39 0.025(3) 0.031(3) 0.023(3) 0.006(2) -0.002(2) 0.020(2) C40 0.025(3) 0.031(3) 0.023(3) 0.006(2) -0.002(2) 0.020(2) C41 0.023(4) 0.023(4) 0.037(4) 0.007(3) -0.001(3) 0.008(3) C42 0.027(4) 0.038(5) 0.063(6) 0.011(5) 0.004(4) 0.011(4) C43 0.030(4) 0.025(4) 0.042(5) -0.003(4) -0.006(4) 0.015(3) C44 0.040(5) 0.064(7) 0.036(5) 0.025(5) 0.002(4) 0.030(5) C45 0.060(6) 0.071(7) 0.037(5) 0.023(5) -0.004(5) 0.033(6) C46 0.078(7) 0.052(7) 0.054(6) 0.018(5) -0.002(5) 0.046(6) C47 0.073(8) 0.099(11) 0.149(13) 0.058(10) 0.034(9) 0.072(8) C48 0.048(6) 0.097(9) 0.106(9) 0.075(8) 0.031(6) 0.053(6) C49 0.018(3) 0.030(4) 0.016(3) -0.001(3) -0.009(3) 0.005(3) C50 0.020(3) 0.025(4) 0.022(4) 0.007(3) -0.005(3) 0.006(3) C51 0.024(4) 0.029(4) 0.028(4) 0.004(3) -0.008(3) 0.007(3) C52 0.029(4) 0.043(5) 0.057(6) 0.028(5) -0.002(4) 0.014(4) C53 0.022(4) 0.039(5) 0.026(4) 0.014(4) 0.003(3) 0.013(3) C54 0.028(4) 0.058(6) 0.035(5) 0.024(4) -0.001(4) 0.005(4) C55 0.048(6) 0.085(8) 0.043(6) 0.041(6) 0.006(5) 0.023(6) C56 0.041(5) 0.056(6) 0.048(6) 0.034(5) 0.021(4) 0.016(5) C57 0.038(5) 0.047(6) 0.059(6) 0.031(5) 0.003(4) -0.001(4) C58 0.029(4) 0.049(6) 0.041(5) 0.020(4) -0.005(4) 0.006(4) C59 0.030(4) 0.015(4) 0.022(4) -0.002(3) -0.004(3) 0.006(3) C60 0.028(4) 0.025(4) 0.022(4) 0.010(3) -0.004(3) 0.002(3) C61 0.036(4) 0.028(4) 0.023(4) 0.014(3) 0.002(3) 0.005(3) C62 0.030(4) 0.025(4) 0.024(4) 0.008(3) -0.002(3) 0.014(3) C63 0.025(4) 0.035(5) 0.023(4) 0.010(3) 0.004(3) 0.017(3) C64 0.022(4) 0.030(4) 0.020(4) 0.008(3) -0.002(3) 0.012(3) C65 0.031(4) 0.033(5) 0.035(4) 0.004(4) 0.003(3) 0.016(4) C66 0.040(5) 0.040(6) 0.048(5) 0.001(4) 0.007(4) 0.013(4) C67 0.020(4) 0.038(5) 0.034(4) 0.012(4) 0.008(3) 0.011(3) C68 0.038(5) 0.040(5) 0.041(5) 0.018(4) 0.018(4) 0.005(4) C69 0.052(6) 0.041(6) 0.042(5) 0.002(4) 0.008(4) 0.009(5) C70 0.042(5) 0.047(6) 0.057(6) 0.025(5) 0.015(5) 0.006(5) C71 0.078(8) 0.060(7) 0.048(6) 0.026(6) 0.019(6) -0.001(6) C72 0.059(6) 0.053(7) 0.029(5) 0.005(4) 0.005(4) -0.003(5) C73 0.115(5) 0.060(4) 0.048(3) 0.013(3) 0.006(3) 0.035(3) C74 0.115(5) 0.060(4) 0.048(3) 0.013(3) 0.006(3) 0.035(3) C75 0.115(5) 0.060(4) 0.048(3) 0.013(3) 0.006(3) 0.035(3) C76 0.028(4) 0.035(5) 0.050(5) 0.005(4) -0.002(4) 0.017(4) C77 0.055(6) 0.079(8) 0.043(6) 0.028(5) -0.009(5) 0.025(6) C78 0.037(5) 0.041(6) 0.109(9) 0.030(6) 0.010(6) 0.014(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 Tb1 O9 2.291(5) . ? Tb1 O1 2.295(5) . ? Tb1 O5 2.302(5) . ? Tb1 O10 2.311(5) . ? Tb1 O13 2.328(6) . ? Tb1 O6 2.331(5) . ? Tb1 O2 2.331(5) . ? O1 C1 1.277(8) . ? N1 C1 1.368(9) . ? N1 N2 1.410(9) . ? N1 C5 1.427(10) . ? C1 C2 1.415(10) . ? Tb2 O7 2.259(5) . ? Tb2 O11 2.284(5) . ? Tb2 O3 2.284(5) . ? Tb2 O14 2.329(6) . ? Tb2 O4 2.337(5) . ? Tb2 O12 2.359(6) . ? Tb2 O8 2.364(5) . ? O2 C11 1.246(8) . ? C2 C11 1.431(11) . ? C2 C3 1.448(10) . ? N2 C3 1.308(11) . ? O3 C15 1.285(9) . ? N3 C15 1.367(10) . ? N3 C19A 1.395(12) . ? N3 N4 1.409(10) . ? N3 C19 1.450(12) . ? C3 C4 1.490(11) . ? O4 C14 1.244(9) . ? N4 C17 1.310(11) . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C4 H4D 0.9600 . ? O5 C25 1.261(9) . ? N5 C25 1.387(9) . ? N5 N6 1.393(9) . ? N5 C29A 1.403(12) . ? N5 C29 1.429(13) . ? C5 C10 1.361(12) . ? C5 C6 1.387(11) . ? O6 C35 1.251(9) . ? N6 C27 1.328(10) . ? C6 C7 1.368(12) . ? C6 H6B 0.9300 . ? O7 C39 1.289(9) . ? N7 C39 1.372(9) . ? N7 N8 1.404(9) . ? N7 C43 1.417(10) . ? C7 C8 1.376(14) . ? C7 H7A 0.9300 . ? O8 C38 1.249(8) . ? N8 C41 1.328(10) . ? C8 C9 1.382(15) . ? C8 H8B 0.9300 . ? O9 C49 1.279(9) . ? N9 C49 1.361(9) . ? N9 N10 1.402(8) . ? N9 C53 1.414(9) . ? C9 C10 1.385(14) . ? C9 H9A 0.9300 . ? O10 C59 1.258(9) . ? N10 C51 1.312(9) . ? C10 H10B 0.9300 . ? O11 C63 1.287(9) . ? C11 C12 1.501(10) . ? N11 C63 1.369(9) . ? N11 N12 1.391(9) . ? N11 C67 1.438(10) . ? O12 C62 1.248(9) . ? N12 C65 1.320(10) . ? C12 C13 1.520(11) . ? C12 H12B 0.9700 . ? C12 H12C 0.9700 . ? O13 C73 1.246(13) . ? C13 C14 1.502(11) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? N13 C73 1.301(14) . ? N13 C74 1.441(15) . ? N13 C75 1.451(14) . ? O14 C76 1.234(10) . ? C14 C16 1.425(11) . ? N14 C76 1.305(11) . ? N14 C78 1.456(11) . ? N14 C77 1.470(11) . ? C15 C16 1.402(11) . ? C16 C17 1.436(10) . ? C17 C18 1.483(12) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C20 1.3900 . ? C19 C24 1.3900 . ? C20 C21 1.3900 . ? C20 H20 0.9300 . ? C21 C22 1.3900 . ? C21 H21 0.9300 . ? C22 C23 1.3900 . ? C22 H22 0.9300 . ? C23 C24 1.3900 . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C19A C20A 1.3900 . ? C19A C24A 1.3900 . ? C20A C21A 1.3900 . ? C20A H20A 0.9300 . ? C21A C22A 1.3900 . ? C21A H21A 0.9300 . ? C22A C23A 1.3900 . ? C22A H22A 0.9300 . ? C23A C24A 1.3900 . ? C23A H23A 0.9300 . ? C24A H24A 0.9300 . ? C25 C26 1.410(11) . ? C26 C27 1.429(10) . ? C26 C35 1.441(10) . ? C27 C28 1.489(12) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 C30 1.3900 . ? C29 C34 1.3900 . ? C30 C31 1.3900 . ? C30 H30 0.9300 . ? C31 C32 1.3900 . ? C31 H31 0.9300 . ? C32 C33 1.3900 . ? C32 H32 0.9300 . ? C33 C34 1.3900 . ? C33 H33 0.9300 . ? C34 H34 0.9300 . ? C29A C30A 1.3900 . ? C29A C34A 1.3900 . ? C30A C31A 1.3900 . ? C30A H30A 0.9300 . ? C31A C32A 1.3900 . ? C31A H31A 0.9300 . ? C32A C33A 1.3900 . ? C32A H32A 0.9300 . ? C33A C34A 1.3900 . ? C33A H33A 0.9300 . ? C34A H34A 0.9300 . ? C35 C36 1.498(10) . ? C36 C37 1.530(10) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 C38 1.509(10) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 C40 1.437(10) . ? C39 C40 1.400(10) . ? C40 C41 1.428(10) . ? C41 C42 1.505(11) . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 C44 1.365(11) . ? C43 C48 1.374(12) . ? C44 C45 1.389(13) . ? C44 H44A 0.9300 . ? C45 C46 1.371(14) . ? C45 H45A 0.9300 . ? C46 C47 1.373(15) . ? C46 H46A 0.9300 . ? C47 C48 1.382(15) . ? C47 H47A 0.9300 . ? C48 H48A 0.9300 . ? C49 C50 1.420(10) . ? C50 C51 1.414(10) . ? C50 C59 1.431(10) . ? C51 C52 1.517(11) . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C53 C54 1.369(11) . ? C53 C58 1.376(11) . ? C54 C55 1.393(12) . ? C54 H54A 0.9300 . ? C55 C56 1.368(13) . ? C55 H55A 0.9300 . ? C56 C57 1.361(13) . ? C56 H56A 0.9300 . ? C57 C58 1.380(11) . ? C57 H57A 0.9300 . ? C58 H58A 0.9300 . ? C59 C60 1.495(10) . ? C60 C61 1.528(10) . ? C60 H60A 0.9700 . ? C60 H60B 0.9700 . ? C61 C62 1.498(10) . ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? C62 C64 1.422(10) . ? C63 C64 1.399(11) . ? C64 C65 1.432(10) . ? C65 C66 1.486(12) . ? C66 H66A 0.9600 . ? C66 H66B 0.9600 . ? C66 H66C 0.9600 . ? C67 C68 1.355(12) . ? C67 C72 1.355(11) . ? C68 C69 1.399(12) . ? C68 H68A 0.9300 . ? C69 C70 1.363(12) . ? C69 H69A 0.9300 . ? C70 C71 1.363(14) . ? C70 H70A 0.9300 . ? C71 C72 1.379(13) . ? C71 H71A 0.9300 . ? C72 H72A 0.9300 . ? C73 H73 0.9300 . ? C74 H74A 0.9600 . ? C74 H74B 0.9600 . ? C74 H74C 0.9600 . ? C75 H75A 0.9600 . ? C75 H75B 0.9600 . ? C75 H75C 0.9600 . ? C76 H76 0.9300 . ? C77 H77A 0.9600 . ? C77 H77B 0.9600 . ? C77 H77C 0.9600 . ? C78 H78A 0.9600 . ? C78 H78B 0.9600 . ? C78 H78C 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 O9 Tb1 O1 115.72(18) . . ? O9 Tb1 O5 115.34(18) . . ? O1 Tb1 O5 115.28(18) . . ? O9 Tb1 O10 75.14(17) . . ? O1 Tb1 O10 80.54(18) . . ? O5 Tb1 O10 149.7(2) . . ? O9 Tb1 O13 76.77(19) . . ? O1 Tb1 O13 79.9(2) . . ? O5 Tb1 O13 75.8(2) . . ? O10 Tb1 O13 134.1(2) . . ? O9 Tb1 O6 76.09(18) . . ? O1 Tb1 O6 154.35(18) . . ? O5 Tb1 O6 74.85(18) . . ? O10 Tb1 O6 80.97(18) . . ? O13 Tb1 O6 125.71(19) . . ? O9 Tb1 O2 152.94(19) . . ? O1 Tb1 O2 75.62(18) . . ? O5 Tb1 O2 76.68(19) . . ? O10 Tb1 O2 83.26(18) . . ? O13 Tb1 O2 130.28(19) . . ? O6 Tb1 O2 84.69(18) . . ? C1 O1 Tb1 129.7(5) . . ? C1 N1 N2 111.4(6) . . ? C1 N1 C5 129.9(6) . . ? N2 N1 C5 118.3(6) . . ? O1 C1 N1 122.4(7) . . ? O1 C1 C2 131.2(7) . . ? N1 C1 C2 106.3(6) . . ? O7 Tb2 O11 109.14(18) . . ? O7 Tb2 O3 111.44(19) . . ? O11 Tb2 O3 122.74(18) . . ? O7 Tb2 O14 77.6(2) . . ? O11 Tb2 O14 75.4(2) . . ? O3 Tb2 O14 75.9(2) . . ? O7 Tb2 O4 159.58(19) . . ? O11 Tb2 O4 81.02(18) . . ? O3 Tb2 O4 74.69(19) . . ? O14 Tb2 O4 122.7(2) . . ? O7 Tb2 O12 82.14(19) . . ? O11 Tb2 O12 74.94(18) . . ? O3 Tb2 O12 148.30(19) . . ? O14 Tb2 O12 135.82(19) . . ? O4 Tb2 O12 83.65(19) . . ? O7 Tb2 O8 75.43(18) . . ? O11 Tb2 O8 151.33(19) . . ? O3 Tb2 O8 78.30(18) . . ? O14 Tb2 O8 132.14(19) . . ? O4 Tb2 O8 87.30(18) . . ? O12 Tb2 O8 77.82(18) . . ? C11 O2 Tb1 138.9(5) . . ? C1 C2 C11 122.9(6) . . ? C1 C2 C3 104.9(7) . . ? C11 C2 C3 132.0(7) . . ? C3 N2 N1 105.9(6) . . ? C15 O3 Tb2 129.7(5) . . ? C15 N3 C19A 133.8(8) . . ? C15 N3 N4 110.8(7) . . ? C19A N3 N4 113.3(8) . . ? C15 N3 C19 126.4(8) . . ? C19A N3 C19 19.6(11) . . ? N4 N3 C19 122.5(8) . . ? N2 C3 C2 111.5(7) . . ? N2 C3 C4 118.8(7) . . ? C2 C3 C4 129.7(8) . . ? C14 O4 Tb2 138.6(5) . . ? C17 N4 N3 106.3(6) . . ? C3 C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C4 H4D 109.5 . . ? H4B C4 H4D 109.5 . . ? H4C C4 H4D 109.5 . . ? C25 O5 Tb1 130.6(5) . . ? C25 N5 N6 111.8(6) . . ? C25 N5 C29A 132.1(9) . . ? N6 N5 C29A 116.1(8) . . ? C25 N5 C29 123.7(9) . . ? N6 N5 C29 124.4(9) . . ? C29A N5 C29 9.3(13) . . ? C10 C5 C6 120.5(8) . . ? C10 C5 N1 119.3(8) . . ? C6 C5 N1 120.2(7) . . ? C35 O6 Tb1 138.9(5) . . ? C27 N6 N5 105.8(6) . . ? C7 C6 C5 119.1(8) . . ? C7 C6 H6B 120.4 . . ? C5 C6 H6B 120.4 . . ? C39 O7 Tb2 129.5(5) . . ? C39 N7 N8 111.2(6) . . ? C39 N7 C43 129.8(6) . . ? N8 N7 C43 118.6(6) . . ? C6 C7 C8 120.7(9) . . ? C6 C7 H7A 119.7 . . ? C8 C7 H7A 119.7 . . ? C38 O8 Tb2 135.6(5) . . ? C41 N8 N7 105.3(6) . . ? C7 C8 C9 120.3(10) . . ? C7 C8 H8B 119.9 . . ? C9 C8 H8B 119.9 . . ? C49 O9 Tb1 128.0(4) . . ? C49 N9 N10 111.8(6) . . ? C49 N9 C53 128.0(6) . . ? N10 N9 C53 120.1(6) . . ? C8 C9 C10 118.8(10) . . ? C8 C9 H9A 120.6 . . ? C10 C9 H9A 120.6 . . ? C59 O10 Tb1 138.6(4) . . ? C51 N10 N9 105.2(6) . . ? C5 C10 C9 120.7(10) . . ? C5 C10 H10B 119.7 . . ? C9 C10 H10B 119.7 . . ? C63 O11 Tb2 128.4(5) . . ? O2 C11 C2 120.7(7) . . ? O2 C11 C12 118.6(7) . . ? C2 C11 C12 120.6(6) . . ? C63 N11 N12 111.5(6) . . ? C63 N11 C67 129.0(7) . . ? N12 N11 C67 119.1(6) . . ? C62 O12 Tb2 135.9(5) . . ? C65 N12 N11 105.4(6) . . ? C11 C12 C13 112.6(6) . . ? C11 C12 H12B 109.1 . . ? C13 C12 H12B 109.1 . . ? C11 C12 H12C 109.1 . . ? C13 C12 H12C 109.1 . . ? H12B C12 H12C 107.8 . . ? C73 O13 Tb1 131.9(7) . . ? C14 C13 C12 114.3(6) . . ? C14 C13 H13A 108.7 . . ? C12 C13 H13A 108.7 . . ? C14 C13 H13B 108.7 . . ? C12 C13 H13B 108.7 . . ? H13A C13 H13B 107.6 . . ? C73 N13 C74 123.5(11) . . ? C73 N13 C75 120.0(12) . . ? C74 N13 C75 116.3(9) . . ? C76 O14 Tb2 152.6(6) . . ? O4 C14 C16 121.0(7) . . ? O4 C14 C13 118.6(7) . . ? C16 C14 C13 120.3(7) . . ? C76 N14 C78 122.4(8) . . ? C76 N14 C77 120.1(7) . . ? C78 N14 C77 117.3(8) . . ? O3 C15 N3 122.3(7) . . ? O3 C15 C16 131.3(7) . . ? N3 C15 C16 106.3(7) . . ? C15 C16 C14 122.2(7) . . ? C15 C16 C17 105.7(7) . . ? C14 C16 C17 131.8(8) . . ? N4 C17 C16 110.9(7) . . ? N4 C17 C18 118.6(7) . . ? C16 C17 C18 130.5(8) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C24 120.0 . . ? C20 C19 N3 123.1(10) . . ? C24 C19 N3 116.9(10) . . ? C19 C20 C21 120.0 . . ? C19 C20 H20 120.0 . . ? C21 C20 H20 120.0 . . ? C20 C21 C22 120.0 . . ? C20 C21 H21 120.0 . . ? C22 C21 H21 120.0 . . ? C23 C22 C21 120.0 . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C22 C23 C24 120.0 . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C23 C24 C19 120.0 . . ? C23 C24 H24 120.0 . . ? C19 C24 H24 120.0 . . ? C20A C19A C24A 120.0 . . ? C20A C19A N3 118.7(9) . . ? C24A C19A N3 120.9(9) . . ? C19A C20A C21A 120.0 . . ? C19A C20A H20A 120.0 . . ? C21A C20A H20A 120.0 . . ? C22A C21A C20A 120.0 . . ? C22A C21A H21A 120.0 . . ? C20A C21A H21A 120.0 . . ? C21A C22A C23A 120.0 . . ? C21A C22A H22A 120.0 . . ? C23A C22A H22A 120.0 . . ? C22A C23A C24A 120.0 . . ? C22A C23A H23A 120.0 . . ? C24A C23A H23A 120.0 . . ? C23A C24A C19A 120.0 . . ? C23A C24A H24A 120.0 . . ? C19A C24A H24A 120.0 . . ? O5 C25 N5 122.8(7) . . ? O5 C25 C26 132.0(7) . . ? N5 C25 C26 105.1(7) . . ? C25 C26 C27 106.2(7) . . ? C25 C26 C35 121.3(7) . . ? C27 C26 C35 132.2(7) . . ? N6 C27 C26 111.0(7) . . ? N6 C27 C28 118.7(7) . . ? C26 C27 C28 130.3(7) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 C34 120.0 . . ? C30 C29 N5 119.9(10) . . ? C34 C29 N5 120.1(10) . . ? C29 C30 C31 120.0 . . ? C29 C30 H30 120.0 . . ? C31 C30 H30 120.0 . . ? C30 C31 C32 120.0 . . ? C30 C31 H31 120.0 . . ? C32 C31 H31 120.0 . . ? C33 C32 C31 120.0 . . ? C33 C32 H32 120.0 . . ? C31 C32 H32 120.0 . . ? C32 C33 C34 120.0 . . ? C32 C33 H33 120.0 . . ? C34 C33 H33 120.0 . . ? C33 C34 C29 120.0 . . ? C33 C34 H34 120.0 . . ? C29 C34 H34 120.0 . . ? C30A C29A C34A 120.0 . . ? C30A C29A N5 119.9(10) . . ? C34A C29A N5 120.1(10) . . ? C31A C30A C29A 120.0 . . ? C31A C30A H30A 120.0 . . ? C29A C30A H30A 120.0 . . ? C30A C31A C32A 120.0 . . ? C30A C31A H31A 120.0 . . ? C32A C31A H31A 120.0 . . ? C33A C32A C31A 120.0 . . ? C33A C32A H32A 120.0 . . ? C31A C32A H32A 120.0 . . ? C34A C33A C32A 120.0 . . ? C34A C33A H33A 120.0 . . ? C32A C33A H33A 120.0 . . ? C33A C34A C29A 120.0 . . ? C33A C34A H34A 120.0 . . ? C29A C34A H34A 120.0 . . ? O6 C35 C26 121.5(7) . . ? O6 C35 C36 118.6(6) . . ? C26 C35 C36 119.9(6) . . ? C35 C36 C37 113.9(6) . . ? C35 C36 H36A 108.8 . . ? C37 C36 H36A 108.8 . . ? C35 C36 H36B 108.8 . . ? C37 C36 H36B 108.8 . . ? H36A C36 H36B 107.7 . . ? C38 C37 C36 113.5(6) . . ? C38 C37 H37A 108.9 . . ? C36 C37 H37A 108.9 . . ? C38 C37 H37B 108.9 . . ? C36 C37 H37B 108.9 . . ? H37A C37 H37B 107.7 . . ? O8 C38 C40 122.3(6) . . ? O8 C38 C37 117.6(6) . . ? C40 C38 C37 120.0(6) . . ? O7 C39 N7 122.0(7) . . ? O7 C39 C40 131.5(7) . . ? N7 C39 C40 106.4(6) . . ? C39 C40 C41 105.6(6) . . ? C39 C40 C38 121.8(6) . . ? C41 C40 C38 132.2(7) . . ? N8 C41 C40 111.4(6) . . ? N8 C41 C42 118.1(7) . . ? C40 C41 C42 130.5(7) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C44 C43 C48 119.3(8) . . ? C44 C43 N7 121.4(7) . . ? C48 C43 N7 119.3(8) . . ? C43 C44 C45 121.2(8) . . ? C43 C44 H44A 119.4 . . ? C45 C44 H44A 119.4 . . ? C46 C45 C44 119.5(9) . . ? C46 C45 H45A 120.2 . . ? C44 C45 H45A 120.2 . . ? C45 C46 C47 119.2(9) . . ? C45 C46 H46A 120.4 . . ? C47 C46 H46A 120.4 . . ? C46 C47 C48 121.3(10) . . ? C46 C47 H47A 119.4 . . ? C48 C47 H47A 119.4 . . ? C43 C48 C47 119.5(10) . . ? C43 C48 H48A 120.2 . . ? C47 C48 H48A 120.2 . . ? O9 C49 N9 123.4(7) . . ? O9 C49 C50 131.0(6) . . ? N9 C49 C50 105.5(6) . . ? C51 C50 C49 105.2(6) . . ? C51 C50 C59 132.5(7) . . ? C49 C50 C59 122.2(7) . . ? N10 C51 C50 112.2(7) . . ? N10 C51 C52 118.6(7) . . ? C50 C51 C52 129.2(7) . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C54 C53 C58 119.0(7) . . ? C54 C53 N9 121.4(7) . . ? C58 C53 N9 119.6(7) . . ? C53 C54 C55 120.1(8) . . ? C53 C54 H54A 119.9 . . ? C55 C54 H54A 119.9 . . ? C56 C55 C54 120.3(9) . . ? C56 C55 H55A 119.8 . . ? C54 C55 H55A 119.8 . . ? C57 C56 C55 119.4(8) . . ? C57 C56 H56A 120.3 . . ? C55 C56 H56A 120.3 . . ? C56 C57 C58 120.6(8) . . ? C56 C57 H57A 119.7 . . ? C58 C57 H57A 119.7 . . ? C53 C58 C57 120.4(8) . . ? C53 C58 H58A 119.8 . . ? C57 C58 H58A 119.8 . . ? O10 C59 C50 120.4(7) . . ? O10 C59 C60 118.2(6) . . ? C50 C59 C60 121.4(7) . . ? C59 C60 C61 112.3(7) . . ? C59 C60 H60A 109.1 . . ? C61 C60 H60A 109.1 . . ? C59 C60 H60B 109.1 . . ? C61 C60 H60B 109.1 . . ? H60A C60 H60B 107.9 . . ? C62 C61 C60 115.0(6) . . ? C62 C61 H61A 108.5 . . ? C60 C61 H61A 108.5 . . ? C62 C61 H61B 108.5 . . ? C60 C61 H61B 108.5 . . ? H61A C61 H61B 107.5 . . ? O12 C62 C64 121.6(7) . . ? O12 C62 C61 118.9(7) . . ? C64 C62 C61 119.3(7) . . ? O11 C63 N11 122.5(7) . . ? O11 C63 C64 130.7(6) . . ? N11 C63 C64 106.6(6) . . ? C63 C64 C62 122.4(7) . . ? C63 C64 C65 104.8(6) . . ? C62 C64 C65 131.3(7) . . ? N12 C65 C64 111.6(7) . . ? N12 C65 C66 117.6(7) . . ? C64 C65 C66 130.7(7) . . ? C65 C66 H66A 109.5 . . ? C65 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C65 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C68 C67 C72 119.6(8) . . ? C68 C67 N11 121.8(7) . . ? C72 C67 N11 118.5(8) . . ? C67 C68 C69 120.2(8) . . ? C67 C68 H68A 119.9 . . ? C69 C68 H68A 119.9 . . ? C70 C69 C68 119.9(9) . . ? C70 C69 H69A 120.1 . . ? C68 C69 H69A 120.1 . . ? C69 C70 C71 119.2(9) . . ? C69 C70 H70A 120.4 . . ? C71 C70 H70A 120.4 . . ? C70 C71 C72 120.5(9) . . ? C70 C71 H71A 119.7 . . ? C72 C71 H71A 119.7 . . ? C67 C72 C71 120.5(9) . . ? C67 C72 H72A 119.7 . . ? C71 C72 H72A 119.7 . . ? O13 C73 N13 124.5(13) . . ? O13 C73 H73 117.8 . . ? N13 C73 H73 117.8 . . ? N13 C74 H74A 109.5 . . ? N13 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? N13 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? N13 C75 H75A 109.5 . . ? N13 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? N13 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? O14 C76 N14 125.3(8) . . ? O14 C76 H76 117.3 . . ? N14 C76 H76 117.3 . . ? N14 C77 H77A 109.5 . . ? N14 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? N14 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? N14 C78 H78A 109.5 . . ? N14 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? N14 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 3.308 _refine_diff_density_min -1.247 _refine_diff_density_rms 0.181 # Attachment 'Structure3.CIF' data_TbQ2Qdpppe _database_code_depnum_ccdc_archive 'CCDC 670982' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Tb2(Q2Q)3(dppeO2))n _chemical_melting_point ? _chemical_formula_moiety '[Tb2(C24H20N4O4)3(C26H24P2)]n' _chemical_formula_sum 'C98 H84 N12 O14 P2 Tb2' _chemical_formula_weight 2033.57 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.674(3) _cell_length_b 16.276(3) _cell_length_c 18.847(4) _cell_angle_alpha 83.63(3) _cell_angle_beta 82.24(3) _cell_angle_gamma 76.43(3) _cell_volume 4320.9(15) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 8796 _cell_measurement_theta_min 2.415 _cell_measurement_theta_max 29.363 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.565 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2060 _exptl_absorpt_coefficient_mu 1.735 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.857 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(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 IPDS(Stoe) _diffrn_measurement_method '\f oscillation scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 58840 _diffrn_reflns_av_R_equivalents 0.1061 _diffrn_reflns_av_sigmaI/netI 0.2466 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.43 _diffrn_reflns_theta_max 26.37 _reflns_number_total 17652 _reflns_number_gt 6137 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0610P)^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 17652 _refine_ls_number_parameters 1159 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1637 _refine_ls_R_factor_gt 0.0560 _refine_ls_wR_factor_ref 0.1476 _refine_ls_wR_factor_gt 0.1125 _refine_ls_goodness_of_fit_ref 0.808 _refine_ls_restrained_S_all 0.808 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tb1 Tb 0.75728(3) 0.29787(3) 0.29505(2) 0.03812(14) Uani 1 1 d . . . P1 P 0.67549(17) 0.09097(17) 0.32283(14) 0.0485(7) Uani 1 1 d . . . O1 O 0.7185(4) 0.2775(4) 0.4165(3) 0.0445(16) Uani 1 1 d . . . N1 N 0.6992(5) 0.3015(5) 0.5379(4) 0.0415(19) Uani 1 1 d . . . C1 C 0.7366(5) 0.3100(6) 0.4683(5) 0.038(2) Uani 1 1 d . . . Tb2 Tb 0.80936(3) 0.67624(3) 0.25135(2) 0.03737(14) Uani 1 1 d . . . P2 P 0.86802(17) -0.11539(16) 0.20812(14) 0.0460(7) Uani 1 1 d . . . O2 O 0.8569(4) 0.3624(4) 0.3468(3) 0.0386(15) Uani 1 1 d . . . N2 N 0.7347(5) 0.3447(5) 0.5834(4) 0.0424(19) Uani 1 1 d . . . C2 C 0.8035(6) 0.3630(5) 0.4696(4) 0.035(2) Uani 1 1 d . . . O3 O 0.9558(4) 0.6647(4) 0.1879(3) 0.0373(14) Uani 1 1 d . . . N3 N 1.1035(4) 0.5940(5) 0.1369(4) 0.0397(19) Uani 1 1 d . . . C3 C 0.7957(6) 0.3814(6) 0.5434(5) 0.041(2) Uani 1 1 d . . . O4 O 0.9026(4) 0.5592(3) 0.3095(3) 0.0392(15) Uani 1 1 d . . . N4 N 1.1707(5) 0.5199(5) 0.1512(4) 0.051(2) Uani 1 1 d . . . C4 C 0.8461(6) 0.4321(6) 0.5783(5) 0.057(3) Uani 1 1 d . . . H4B H 0.8244 0.4318 0.6287 0.085 Uiso 1 1 calc R . . H4C H 0.8338 0.4894 0.5569 0.085 Uiso 1 1 calc R . . H4D H 0.9126 0.4080 0.5718 0.085 Uiso 1 1 calc R . . O5 O 0.8992(4) 0.2108(4) 0.2597(3) 0.0468(16) Uani 1 1 d . . . N5 N 1.0560(4) 0.1722(5) 0.2123(4) 0.0405(19) Uani 1 1 d . . . C5 C 0.6278(6) 0.2562(6) 0.5666(5) 0.041(2) Uani 1 1 d . . . N6 N 1.1201(5) 0.2072(5) 0.1620(4) 0.048(2) Uani 1 1 d . . . C6 C 0.6142(7) 0.2398(6) 0.6407(5) 0.057(3) Uani 1 1 d . . . H6B H 0.6524 0.2548 0.6704 0.069 Uiso 1 1 calc R . . O6 O 0.8211(4) 0.3702(4) 0.1941(3) 0.0413(15) Uani 1 1 d . . . N7 N 0.5577(5) 0.7228(5) 0.1307(4) 0.0390(18) Uani 1 1 d . . . C7 C 0.5411(7) 0.2000(7) 0.6691(6) 0.064(3) Uani 1 1 d . . . H7A H 0.5300 0.1889 0.7186 0.077 Uiso 1 1 calc R . . O7 O 0.6896(3) 0.7304(3) 0.1771(3) 0.0298(14) Uani 1 1 d . . . N8 N 0.5283(5) 0.6630(5) 0.0952(4) 0.048(2) Uani 1 1 d . . . C8 C 0.4862(8) 0.1772(7) 0.6263(7) 0.074(3) Uani 1 1 d . . . H8B H 0.4387 0.1499 0.6465 0.089 Uiso 1 1 calc R . . O8 O 0.8218(4) 0.5742(4) 0.1701(3) 0.0427(15) Uani 1 1 d . . . N9 N 0.5023(5) 0.3557(5) 0.1701(4) 0.0386(18) Uani 1 1 d . . . C9 C 0.4995(7) 0.1937(6) 0.5549(6) 0.057(3) Uani 1 1 d . . . H9A H 0.4602 0.1790 0.5260 0.068 Uiso 1 1 calc R . . O9 O 0.6397(4) 0.3112(4) 0.2210(3) 0.0435(17) Uani 1 1 d . . . O10 O 0.6504(4) 0.4265(4) 0.3176(3) 0.0405(15) Uani 1 1 d . . . N10 N 0.4256(5) 0.4278(5) 0.1719(4) 0.048(2) Uani 1 1 d . . . C10 C 0.5718(6) 0.2326(6) 0.5236(5) 0.049(3) Uani 1 1 d . . . H10B H 0.5820 0.2426 0.4739 0.059 Uiso 1 1 calc R . . O11 O 0.8039(4) 0.7129(3) 0.3657(3) 0.0404(15) Uani 1 1 d . . . C11 C 0.8622(6) 0.3845(5) 0.4075(5) 0.034(2) Uani 1 1 d . . . N11 N 0.7862(5) 0.6910(5) 0.4923(4) 0.046(2) Uani 1 1 d . . . O12 O 0.6874(4) 0.6219(4) 0.3146(3) 0.0425(16) Uani 1 1 d . . . N12 N 0.7315(5) 0.6527(5) 0.5457(4) 0.044(2) Uani 1 1 d . . . C12 C 0.9401(5) 0.4299(5) 0.4154(4) 0.040(2) Uani 1 1 d . . . H12B H 0.9112 0.4872 0.4279 0.048 Uiso 1 1 calc R . . H12C H 0.9747 0.4008 0.4547 0.048 Uiso 1 1 calc R . . O13 O 0.7264(4) 0.1625(3) 0.3075(3) 0.0437(15) Uani 1 1 d . . . C13 C 1.0096(5) 0.4342(6) 0.3477(5) 0.045(2) Uani 1 1 d . . . H13A H 1.0709 0.4334 0.3620 0.054 Uiso 1 1 calc R . . H13B H 1.0159 0.3837 0.3229 0.054 Uiso 1 1 calc R . . O14 O 0.8125(4) -0.1808(3) 0.2342(3) 0.0408(15) Uani 1 1 d . . . C14 C 0.9824(5) 0.5116(5) 0.2955(5) 0.032(2) Uani 1 1 d . . . C15 C 1.0246(5) 0.6030(6) 0.1870(5) 0.034(2) Uani 1 1 d . . . C16 C 1.0456(6) 0.5284(5) 0.2353(5) 0.039(2) Uani 1 1 d . . . C17 C 1.1364(6) 0.4828(6) 0.2097(5) 0.039(2) Uani 1 1 d . . . C18 C 1.1963(6) 0.4001(6) 0.2383(5) 0.056(3) Uani 1 1 d . . . H18A H 1.2545 0.3867 0.2074 0.085 Uiso 1 1 calc R . . H18B H 1.1630 0.3556 0.2397 0.085 Uiso 1 1 calc R . . H18C H 1.2095 0.4055 0.2858 0.085 Uiso 1 1 calc R . . C19 C 1.1230(6) 0.6507(6) 0.0781(5) 0.043(2) Uani 1 1 d . . . C20 C 1.0535(6) 0.7118(6) 0.0456(5) 0.045(2) Uani 1 1 d . . . H20A H 0.9904 0.7169 0.0636 0.054 Uiso 1 1 calc R . . C21 C 1.0775(7) 0.7646(6) -0.0128(5) 0.054(3) Uani 1 1 d . . . H21A H 1.0302 0.8046 -0.0335 0.065 Uiso 1 1 calc R . . C22 C 1.1685(8) 0.7595(7) -0.0405(6) 0.064(3) Uani 1 1 d . . . H22A H 1.1833 0.7950 -0.0805 0.077 Uiso 1 1 calc R . . C23 C 1.2403(7) 0.7001(7) -0.0084(6) 0.066(3) Uani 1 1 d . . . H23A H 1.3030 0.6967 -0.0269 0.079 Uiso 1 1 calc R . . C24 C 1.2186(6) 0.6469(6) 0.0504(5) 0.045(2) Uani 1 1 d . . . H24A H 1.2666 0.6085 0.0719 0.054 Uiso 1 1 calc R . . C25 C 0.9694(6) 0.2283(5) 0.2202(4) 0.032(2) Uani 1 1 d . . . C26 C 0.9773(6) 0.2985(6) 0.1713(5) 0.041(2) Uani 1 1 d . . . C27 C 1.0739(5) 0.2820(6) 0.1363(5) 0.041(2) Uani 1 1 d . . . C28 C 1.1228(6) 0.3334(6) 0.0820(5) 0.060(3) Uani 1 1 d . . . H28A H 1.1875 0.3044 0.0722 0.090 Uiso 1 1 calc R . . H28B H 1.1200 0.3871 0.0998 0.090 Uiso 1 1 calc R . . H28C H 1.0928 0.3425 0.0387 0.090 Uiso 1 1 calc R . . C29 C 1.0877(6) 0.0924(6) 0.2504(5) 0.038(2) Uani 1 1 d . . . C30 C 1.1807(6) 0.0519(7) 0.2373(6) 0.062(3) Uani 1 1 d . . . H30A H 1.2214 0.0763 0.2039 0.075 Uiso 1 1 calc R . . C31 C 1.2139(7) -0.0260(7) 0.2741(6) 0.063(3) Uani 1 1 d . . . H31A H 1.2763 -0.0549 0.2644 0.076 Uiso 1 1 calc R . . C32 C 1.1529(8) -0.0602(7) 0.3257(6) 0.064(3) Uani 1 1 d . . . H32A H 1.1753 -0.1104 0.3530 0.077 Uiso 1 1 calc R . . C33 C 1.0608(7) -0.0201(6) 0.3361(6) 0.060(3) Uani 1 1 d . . . H33A H 1.0195 -0.0445 0.3690 0.073 Uiso 1 1 calc R . . C34 C 1.0278(6) 0.0549(6) 0.2992(5) 0.051(3) Uani 1 1 d . . . H34A H 0.9642 0.0813 0.3068 0.061 Uiso 1 1 calc R . . C35 C 0.9013(6) 0.3662(6) 0.1574(4) 0.036(2) Uani 1 1 d . . . C36 C 0.9057(6) 0.4341(6) 0.0952(5) 0.050(3) Uani 1 1 d . . . H36A H 0.9361 0.4068 0.0523 0.060 Uiso 1 1 calc R . . H36B H 0.9446 0.4708 0.1059 0.060 Uiso 1 1 calc R . . C37 C 0.8092(6) 0.4885(6) 0.0799(5) 0.045(2) Uani 1 1 d . . . H37A H 0.8145 0.5143 0.0310 0.054 Uiso 1 1 calc R . . H37B H 0.7651 0.4519 0.0830 0.054 Uiso 1 1 calc R . . C38 C 0.7701(7) 0.5563(6) 0.1289(5) 0.043(2) Uani 1 1 d . . . C39 C 0.6483(7) 0.6879(7) 0.1472(5) 0.050(3) Uani 1 1 d . . . C40 C 0.6773(6) 0.6056(6) 0.1244(4) 0.035(2) Uani 1 1 d . . . C41 C 0.5990(6) 0.5953(6) 0.0912(5) 0.043(2) Uani 1 1 d . . . C42 C 0.5859(6) 0.5233(6) 0.0528(5) 0.059(3) Uani 1 1 d . . . H42A H 0.5206 0.5208 0.0595 0.088 Uiso 1 1 calc R . . H42B H 0.6231 0.4709 0.0719 0.088 Uiso 1 1 calc R . . H42C H 0.6058 0.5322 0.0024 0.088 Uiso 1 1 calc R . . C43 C 0.5025(6) 0.8061(6) 0.1297(5) 0.038(2) Uani 1 1 d . . . C44 C 0.5434(6) 0.8720(7) 0.1410(5) 0.049(3) Uani 1 1 d . . . H44A H 0.6045 0.8608 0.1536 0.059 Uiso 1 1 calc R . . C45 C 0.4916(7) 0.9539(7) 0.1330(5) 0.057(3) Uani 1 1 d . . . H45A H 0.5199 0.9987 0.1362 0.068 Uiso 1 1 calc R . . C46 C 0.3996(7) 0.9704(7) 0.1207(6) 0.066(3) Uani 1 1 d . . . H46A H 0.3636 1.0257 0.1182 0.079 Uiso 1 1 calc R . . C47 C 0.3616(7) 0.9043(8) 0.1122(6) 0.077(4) Uani 1 1 d . . . H47A H 0.2988 0.9153 0.1036 0.092 Uiso 1 1 calc R . . C48 C 0.4120(6) 0.8219(7) 0.1157(5) 0.061(3) Uani 1 1 d . . . H48A H 0.3845 0.7779 0.1085 0.073 Uiso 1 1 calc R . . C49 C 0.5670(8) 0.3648(6) 0.2139(5) 0.048(3) Uani 1 1 d . . . C50 C 0.5301(6) 0.4419(6) 0.2444(5) 0.039(2) Uani 1 1 d . . . C51 C 0.4440(6) 0.4775(6) 0.2159(5) 0.042(2) Uani 1 1 d . . . C52 C 0.3738(6) 0.5587(6) 0.2263(5) 0.055(3) Uani 1 1 d . . . H52A H 0.3224 0.5621 0.1988 0.083 Uiso 1 1 calc R . . H52B H 0.4034 0.6053 0.2107 0.083 Uiso 1 1 calc R . . H52C H 0.3504 0.5612 0.2763 0.083 Uiso 1 1 calc R . . C53 C 0.4992(6) 0.2880(6) 0.1307(5) 0.042(2) Uani 1 1 d . . . C54 C 0.4198(6) 0.2925(7) 0.0968(5) 0.054(3) Uani 1 1 d . . . H54A H 0.3691 0.3390 0.1005 0.064 Uiso 1 1 calc R . . C55 C 0.4177(9) 0.2260(8) 0.0571(5) 0.068(3) Uani 1 1 d . . . H55A H 0.3650 0.2294 0.0336 0.081 Uiso 1 1 calc R . . C56 C 0.4879(7) 0.1579(7) 0.0514(5) 0.056(3) Uani 1 1 d . . . H56A H 0.4836 0.1136 0.0258 0.067 Uiso 1 1 calc R . . C57 C 0.5682(7) 0.1544(7) 0.0846(5) 0.055(3) Uani 1 1 d . . . H57A H 0.6189 0.1080 0.0798 0.065 Uiso 1 1 calc R . . C58 C 0.5733(7) 0.2195(6) 0.1248(5) 0.050(3) Uani 1 1 d . . . H58A H 0.6267 0.2165 0.1475 0.061 Uiso 1 1 calc R . . C59 C 0.5755(6) 0.4699(6) 0.2959(5) 0.043(2) Uani 1 1 d . . . C60 C 0.5318(5) 0.5521(5) 0.3303(5) 0.037(2) Uani 1 1 d . . . H60A H 0.4651 0.5544 0.3438 0.045 Uiso 1 1 calc R . . H60B H 0.5369 0.5989 0.2945 0.045 Uiso 1 1 calc R . . C61 C 0.5745(5) 0.5653(5) 0.3959(5) 0.041(2) Uani 1 1 d . . . H61A H 0.5260 0.5996 0.4272 0.049 Uiso 1 1 calc R . . H61B H 0.5951 0.5106 0.4219 0.049 Uiso 1 1 calc R . . C62 C 0.6570(6) 0.6075(5) 0.3793(6) 0.042(2) Uani 1 1 d . . . C63 C 0.7674(5) 0.6810(5) 0.4246(5) 0.034(2) Uani 1 1 d . . . C64 C 0.6974(5) 0.6300(5) 0.4370(4) 0.033(2) Uani 1 1 d . . . C65 C 0.6778(6) 0.6187(6) 0.5122(5) 0.038(2) Uani 1 1 d . . . C66 C 0.6104(6) 0.5712(7) 0.5578(5) 0.059(3) Uani 1 1 d . . . H66A H 0.6165 0.5728 0.6077 0.088 Uiso 1 1 calc R . . H66B H 0.6252 0.5134 0.5460 0.088 Uiso 1 1 calc R . . H66C H 0.5468 0.5974 0.5487 0.088 Uiso 1 1 calc R . . C67 C 0.8536(6) 0.7316(5) 0.5115(5) 0.039(2) Uani 1 1 d . . . C68 C 0.9279(7) 0.7489(6) 0.4615(5) 0.060(3) Uani 1 1 d . . . H68A H 0.9339 0.7335 0.4148 0.072 Uiso 1 1 calc R . . C69 C 0.9915(7) 0.7886(6) 0.4820(5) 0.056(3) Uani 1 1 d . . . H69A H 1.0397 0.8020 0.4486 0.067 Uiso 1 1 calc R . . C70 C 0.9841(7) 0.8089(6) 0.5527(6) 0.058(3) Uani 1 1 d . . . H70A H 1.0287 0.8338 0.5672 0.070 Uiso 1 1 calc R . . C71 C 0.9112(8) 0.7919(7) 0.6006(6) 0.071(3) Uani 1 1 d . . . H71A H 0.9056 0.8073 0.6473 0.085 Uiso 1 1 calc R . . C72 C 0.8460(7) 0.7529(6) 0.5819(5) 0.052(3) Uani 1 1 d . . . H72A H 0.7975 0.7408 0.6156 0.062 Uiso 1 1 calc R . . C73 C 0.7213(6) 0.0082(6) 0.2612(5) 0.048(2) Uani 1 1 d . . . H73A H 0.6899 -0.0383 0.2752 0.058 Uiso 1 1 calc R . . H73B H 0.7073 0.0308 0.2130 0.058 Uiso 1 1 calc R . . C74 C 0.8300(6) -0.0258(6) 0.2607(5) 0.050(3) Uani 1 1 d . . . H74A H 0.8454 -0.0423 0.3094 0.060 Uiso 1 1 calc R . . H74B H 0.8625 0.0184 0.2405 0.060 Uiso 1 1 calc R . . C75 C 0.5527(6) 0.1248(7) 0.3138(5) 0.053(3) Uani 1 1 d . . . C76 C 0.5024(6) 0.0738(7) 0.2876(5) 0.061(3) Uani 1 1 d . . . H76A H 0.5305 0.0175 0.2800 0.073 Uiso 1 1 calc R . . C77 C 0.4100(7) 0.1076(8) 0.2728(6) 0.078(4) Uani 1 1 d . . . H77A H 0.3785 0.0731 0.2540 0.094 Uiso 1 1 calc R . . C78 C 0.3641(7) 0.1869(8) 0.2843(6) 0.068(3) Uani 1 1 d . . . H78A H 0.3032 0.2082 0.2719 0.081 Uiso 1 1 calc R . . C79 C 0.4107(7) 0.2361(8) 0.3152(6) 0.072(3) Uani 1 1 d . . . H79A H 0.3796 0.2907 0.3261 0.086 Uiso 1 1 calc R . . C80 C 0.5022(7) 0.2054(7) 0.3299(5) 0.061(3) Uani 1 1 d . . . H80A H 0.5313 0.2396 0.3514 0.073 Uiso 1 1 calc R . . C81 C 0.6913(7) 0.0407(7) 0.4123(5) 0.059(3) Uani 1 1 d . . . C82 C 0.6327(9) -0.0087(8) 0.4478(7) 0.091(4) Uani 1 1 d . . . H82A H 0.5818 -0.0167 0.4269 0.110 Uiso 1 1 calc R . . C83 C 0.6513(11) -0.0469(9) 0.5162(8) 0.106(5) Uani 1 1 d . . . H83A H 0.6141 -0.0827 0.5401 0.127 Uiso 1 1 calc R . . C84 C 0.7200(11) -0.0327(10) 0.5468(8) 0.113(5) Uani 1 1 d . . . H84A H 0.7307 -0.0576 0.5926 0.135 Uiso 1 1 calc R . . C85 C 0.7779(10) 0.0199(10) 0.5112(7) 0.105(5) Uani 1 1 d . . . H85A H 0.8254 0.0310 0.5341 0.127 Uiso 1 1 calc R . . C86 C 0.7655(9) 0.0528(9) 0.4469(7) 0.102(5) Uani 1 1 d . . . H86A H 0.8064 0.0852 0.4230 0.122 Uiso 1 1 calc R . . C87 C 0.9922(6) -0.1548(6) 0.2135(6) 0.052(3) Uani 1 1 d . . . C88 C 1.0189(8) -0.2082(7) 0.2747(6) 0.064(3) Uani 1 1 d . . . H88A H 0.9739 -0.2178 0.3125 0.077 Uiso 1 1 calc R . . C89 C 1.1100(9) -0.2449(8) 0.2778(7) 0.078(4) Uani 1 1 d . . . H89A H 1.1274 -0.2763 0.3201 0.094 Uiso 1 1 calc R . . C90 C 1.1762(8) -0.2389(8) 0.2244(7) 0.073(3) Uani 1 1 d . . . H90A H 1.2376 -0.2702 0.2271 0.087 Uiso 1 1 calc R . . C91 C 1.1532(8) -0.1853(9) 0.1640(7) 0.081(4) Uani 1 1 d . . . H91A H 1.1999 -0.1786 0.1267 0.097 Uiso 1 1 calc R . . C92 C 1.0595(6) -0.1409(6) 0.1590(5) 0.052(3) Uani 1 1 d . . . H92A H 1.0437 -0.1029 0.1196 0.062 Uiso 1 1 calc R . . C93 C 0.8512(6) -0.0800(6) 0.1163(5) 0.056(3) Uani 1 1 d . . . C94 C 0.8209(7) -0.1315(7) 0.0737(6) 0.060(3) Uani 1 1 d . . . H94A H 0.8028 -0.1806 0.0944 0.072 Uiso 1 1 calc R . . C95 C 0.8181(7) -0.1091(8) 0.0011(6) 0.067(3) Uani 1 1 d . . . H95A H 0.7995 -0.1440 -0.0274 0.080 Uiso 1 1 calc R . . C96 C 0.8427(8) -0.0357(8) -0.0294(6) 0.071(3) Uani 1 1 d . . . H96A H 0.8397 -0.0206 -0.0782 0.085 Uiso 1 1 calc R . . C97 C 0.8719(8) 0.0155(7) 0.0121(6) 0.071(3) Uani 1 1 d . . . H97A H 0.8884 0.0653 -0.0087 0.086 Uiso 1 1 calc R . . C98 C 0.8764(7) -0.0062(7) 0.0826(6) 0.067(3) Uani 1 1 d . . . H98A H 0.8970 0.0287 0.1098 0.081 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 Tb1 0.0355(2) 0.0353(3) 0.0442(3) -0.0063(2) -0.0033(2) -0.0083(2) P1 0.0503(15) 0.0388(17) 0.0557(17) -0.0094(13) -0.0015(13) -0.0084(13) O1 0.040(3) 0.062(5) 0.035(4) -0.015(3) 0.001(3) -0.014(3) N1 0.052(5) 0.040(5) 0.039(5) -0.013(4) 0.002(4) -0.021(4) C1 0.029(5) 0.035(6) 0.043(6) -0.006(5) -0.003(4) 0.008(4) Tb2 0.0372(3) 0.0336(3) 0.0427(3) -0.0070(2) -0.0050(2) -0.0087(2) P2 0.0508(15) 0.0382(17) 0.0479(16) -0.0044(13) -0.0023(13) -0.0094(13) O2 0.042(3) 0.040(4) 0.034(4) 0.002(3) -0.002(3) -0.014(3) N2 0.049(4) 0.043(5) 0.040(5) -0.004(4) -0.011(4) -0.017(4) C2 0.041(5) 0.023(5) 0.040(6) -0.006(4) -0.013(4) -0.001(4) O3 0.042(3) 0.037(4) 0.029(3) -0.001(3) -0.006(3) -0.001(3) N3 0.031(4) 0.042(5) 0.045(5) -0.004(4) 0.010(4) -0.014(4) C3 0.047(5) 0.052(7) 0.032(5) -0.015(5) -0.008(4) -0.017(5) O4 0.046(4) 0.026(4) 0.042(4) -0.001(3) -0.001(3) -0.003(3) N4 0.045(5) 0.034(5) 0.069(6) -0.003(4) 0.000(4) 0.000(4) C4 0.059(6) 0.051(7) 0.065(7) -0.008(6) -0.008(5) -0.018(5) O5 0.035(3) 0.046(4) 0.054(4) -0.003(3) 0.005(3) -0.004(3) N5 0.027(4) 0.042(5) 0.051(5) -0.010(4) 0.003(4) -0.006(4) C5 0.048(6) 0.040(6) 0.034(6) -0.003(5) -0.001(5) -0.010(5) N6 0.034(4) 0.047(6) 0.068(6) -0.020(4) 0.003(4) -0.017(4) C6 0.061(7) 0.042(7) 0.061(7) -0.001(5) 0.011(6) -0.007(5) O6 0.052(4) 0.033(4) 0.037(4) -0.002(3) -0.004(3) -0.007(3) N7 0.037(4) 0.050(6) 0.035(4) -0.006(4) -0.013(3) -0.015(4) C7 0.081(8) 0.054(8) 0.050(7) 0.005(6) 0.010(6) -0.016(6) O7 0.020(3) 0.015(3) 0.049(4) 0.000(3) 0.008(3) 0.000(2) N8 0.058(5) 0.047(6) 0.046(5) -0.012(4) -0.018(4) -0.015(4) C8 0.095(9) 0.060(9) 0.074(9) 0.005(7) -0.006(8) -0.037(7) O8 0.047(4) 0.039(4) 0.045(4) -0.016(3) -0.004(3) -0.008(3) N9 0.039(4) 0.043(5) 0.036(4) -0.005(4) -0.009(4) -0.010(4) C9 0.057(6) 0.061(8) 0.057(7) -0.005(6) -0.004(6) -0.020(6) O9 0.030(3) 0.075(5) 0.037(4) -0.040(3) 0.002(3) -0.021(3) O10 0.042(3) 0.034(4) 0.046(4) -0.004(3) -0.008(3) -0.006(3) N10 0.049(5) 0.054(6) 0.044(5) -0.012(4) -0.006(4) -0.013(4) C10 0.059(6) 0.057(7) 0.032(6) -0.008(5) 0.015(5) -0.025(5) O11 0.045(3) 0.031(4) 0.048(4) -0.002(3) -0.007(3) -0.013(3) C11 0.040(5) 0.029(6) 0.029(5) -0.005(4) 0.001(4) -0.001(4) N11 0.063(5) 0.053(6) 0.028(4) -0.004(4) -0.011(4) -0.022(4) O12 0.042(4) 0.047(4) 0.044(4) -0.009(3) -0.002(3) -0.018(3) N12 0.057(5) 0.053(6) 0.027(4) -0.002(4) 0.009(4) -0.030(4) C12 0.044(5) 0.031(6) 0.047(6) 0.007(4) -0.013(5) -0.013(4) O13 0.050(4) 0.020(4) 0.063(4) -0.005(3) -0.011(3) -0.010(3) C13 0.033(5) 0.054(7) 0.060(6) -0.012(5) -0.012(5) -0.026(5) O14 0.056(4) 0.032(4) 0.039(4) -0.002(3) -0.007(3) -0.018(3) C14 0.027(4) 0.015(5) 0.054(6) -0.011(4) -0.014(4) 0.002(4) C15 0.027(5) 0.024(6) 0.056(6) -0.015(5) 0.000(4) -0.011(4) C16 0.038(5) 0.026(6) 0.049(6) 0.000(5) 0.000(5) -0.007(4) C17 0.044(5) 0.038(6) 0.040(6) -0.004(5) -0.009(5) -0.015(5) C18 0.054(6) 0.048(7) 0.061(7) 0.001(5) -0.003(5) -0.003(5) C19 0.054(6) 0.032(6) 0.051(6) -0.021(5) 0.000(5) -0.022(5) C20 0.047(6) 0.033(6) 0.049(6) -0.011(5) -0.001(5) 0.003(5) C21 0.066(7) 0.053(7) 0.042(6) 0.009(5) -0.003(5) -0.016(6) C22 0.078(8) 0.045(7) 0.060(7) 0.005(6) 0.009(6) -0.010(6) C23 0.067(7) 0.063(8) 0.073(8) -0.027(7) 0.030(6) -0.038(7) C24 0.054(6) 0.043(6) 0.047(6) -0.014(5) 0.008(5) -0.031(5) C25 0.040(5) 0.021(5) 0.035(5) -0.003(4) -0.013(4) -0.001(4) C26 0.034(5) 0.051(7) 0.036(5) -0.012(5) -0.005(4) 0.000(5) C27 0.026(5) 0.041(7) 0.054(6) -0.011(5) 0.003(4) -0.007(5) C28 0.043(6) 0.065(8) 0.078(8) -0.014(6) 0.004(5) -0.027(5) C29 0.032(5) 0.029(6) 0.053(6) -0.019(5) -0.014(5) 0.003(4) C30 0.040(6) 0.056(8) 0.090(8) -0.018(7) -0.014(6) 0.002(5) C31 0.047(6) 0.055(8) 0.080(8) -0.020(6) 0.001(6) 0.008(6) C32 0.072(8) 0.051(8) 0.071(8) -0.005(6) -0.025(6) -0.006(6) C33 0.053(7) 0.030(7) 0.094(9) -0.003(6) -0.013(6) 0.000(5) C34 0.039(5) 0.037(7) 0.080(8) -0.008(6) -0.015(5) -0.006(5) C35 0.053(6) 0.033(6) 0.029(5) -0.010(4) -0.002(5) -0.024(5) C36 0.064(6) 0.042(7) 0.046(6) -0.010(5) 0.004(5) -0.018(5) C37 0.063(6) 0.032(6) 0.043(6) -0.004(5) -0.009(5) -0.014(5) C38 0.057(6) 0.033(6) 0.040(6) -0.002(5) 0.004(5) -0.016(5) C39 0.053(6) 0.057(8) 0.040(6) 0.010(5) 0.000(5) -0.020(6) C40 0.049(6) 0.026(6) 0.033(5) -0.007(4) 0.000(4) -0.014(5) C41 0.052(6) 0.040(7) 0.040(6) -0.008(5) -0.006(5) -0.018(5) C42 0.070(7) 0.045(7) 0.069(7) -0.016(6) -0.026(6) -0.012(5) C43 0.036(5) 0.027(6) 0.046(6) 0.003(4) -0.011(4) 0.005(4) C44 0.039(5) 0.063(8) 0.047(6) -0.001(5) -0.020(5) -0.011(5) C45 0.070(7) 0.041(7) 0.052(7) -0.008(5) -0.009(6) 0.003(6) C46 0.049(7) 0.045(8) 0.094(9) -0.005(6) -0.008(6) 0.006(6) C47 0.035(6) 0.079(10) 0.106(10) 0.002(8) -0.009(6) 0.007(6) C48 0.041(6) 0.063(8) 0.076(8) 0.000(6) -0.016(5) -0.003(6) C49 0.087(8) 0.038(7) 0.030(5) 0.008(5) -0.034(6) -0.023(6) C50 0.033(5) 0.034(6) 0.050(6) -0.005(5) -0.011(4) -0.004(4) C51 0.038(5) 0.044(7) 0.042(6) 0.003(5) -0.003(4) -0.007(5) C52 0.040(5) 0.053(7) 0.074(7) -0.015(6) -0.022(5) 0.003(5) C53 0.048(6) 0.028(6) 0.056(6) -0.010(5) -0.003(5) -0.021(5) C54 0.049(6) 0.066(8) 0.053(6) -0.020(6) -0.010(5) -0.016(5) C55 0.095(9) 0.072(9) 0.051(7) -0.006(7) -0.020(6) -0.043(8) C56 0.075(7) 0.061(8) 0.043(6) -0.009(6) -0.016(6) -0.031(7) C57 0.072(7) 0.051(7) 0.043(6) 0.002(5) -0.019(5) -0.012(6) C58 0.069(7) 0.052(7) 0.040(6) -0.022(5) -0.011(5) -0.022(6) C59 0.045(6) 0.028(6) 0.048(6) 0.008(5) -0.008(5) 0.000(5) C60 0.031(5) 0.031(6) 0.051(6) -0.004(4) -0.008(4) -0.008(4) C61 0.038(5) 0.026(6) 0.063(6) -0.014(5) 0.000(5) -0.014(4) C62 0.034(5) 0.017(5) 0.077(8) -0.010(5) -0.013(5) -0.003(4) C63 0.040(5) 0.020(5) 0.035(6) 0.000(4) 0.007(4) -0.002(4) C64 0.032(5) 0.027(5) 0.042(6) -0.001(4) 0.004(4) -0.015(4) C65 0.044(5) 0.037(6) 0.039(6) -0.014(4) -0.005(4) -0.016(5) C66 0.053(6) 0.087(9) 0.045(6) -0.002(6) 0.000(5) -0.038(6) C67 0.039(5) 0.032(6) 0.050(6) -0.012(5) -0.002(5) -0.013(4) C68 0.077(7) 0.069(8) 0.053(7) -0.006(6) -0.020(6) -0.047(6) C69 0.071(7) 0.048(7) 0.060(7) 0.003(6) -0.014(6) -0.032(6) C70 0.063(7) 0.062(8) 0.060(7) -0.017(6) -0.029(6) -0.019(6) C71 0.087(8) 0.066(9) 0.071(8) -0.031(7) -0.022(7) -0.023(7) C72 0.066(6) 0.062(7) 0.033(6) -0.026(5) 0.000(5) -0.017(6) C73 0.058(6) 0.037(6) 0.053(6) -0.012(5) -0.014(5) -0.009(5) C74 0.052(6) 0.033(6) 0.057(6) -0.006(5) 0.009(5) 0.000(5) C75 0.043(6) 0.054(7) 0.059(7) -0.018(6) 0.002(5) -0.006(5) C76 0.046(6) 0.068(8) 0.071(8) -0.024(6) -0.011(5) -0.007(6) C77 0.045(7) 0.078(10) 0.112(10) -0.029(8) -0.013(7) -0.004(6) C78 0.049(6) 0.071(9) 0.077(8) -0.028(7) 0.018(6) -0.004(6) C79 0.044(6) 0.087(10) 0.076(8) -0.011(7) 0.004(6) -0.001(6) C80 0.067(7) 0.048(7) 0.066(7) -0.028(6) -0.001(6) -0.006(6) C81 0.073(7) 0.062(8) 0.043(6) -0.002(6) -0.011(6) -0.016(6) C82 0.114(10) 0.081(10) 0.089(10) 0.014(8) -0.013(8) -0.050(9) C83 0.143(14) 0.091(12) 0.085(11) 0.035(9) -0.002(10) -0.056(11) C84 0.128(13) 0.118(15) 0.091(12) 0.021(10) -0.036(11) -0.023(11) C85 0.124(12) 0.137(14) 0.067(9) 0.024(9) -0.070(9) -0.035(11) C86 0.115(11) 0.116(13) 0.085(10) -0.008(9) -0.052(9) -0.023(9) C87 0.044(6) 0.050(7) 0.064(7) -0.012(6) -0.008(5) -0.012(5) C88 0.068(8) 0.061(8) 0.061(8) 0.000(6) -0.001(6) -0.016(6) C89 0.072(8) 0.074(9) 0.087(10) -0.002(7) -0.037(8) -0.001(7) C90 0.071(8) 0.075(10) 0.072(9) -0.019(7) -0.023(7) 0.000(7) C91 0.066(8) 0.111(11) 0.075(9) -0.042(8) 0.011(7) -0.034(8) C92 0.039(6) 0.057(7) 0.058(7) -0.002(5) 0.000(5) -0.013(5) C93 0.053(6) 0.040(7) 0.064(7) -0.002(6) 0.015(6) -0.002(5) C94 0.069(7) 0.046(7) 0.076(8) 0.000(6) -0.032(6) -0.024(6) C95 0.079(8) 0.066(9) 0.046(7) -0.010(6) -0.021(6) 0.013(6) C96 0.088(8) 0.063(9) 0.052(7) 0.008(7) -0.028(6) 0.011(7) C97 0.087(8) 0.058(9) 0.064(8) 0.007(7) -0.003(7) -0.015(7) C98 0.096(8) 0.051(8) 0.059(8) -0.004(6) -0.017(7) -0.021(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tb1 O1 2.289(6) . ? Tb1 O5 2.289(6) . ? Tb1 O9 2.319(6) . ? Tb1 O6 2.328(5) . ? Tb1 O13 2.332(5) . ? Tb1 O10 2.345(6) . ? Tb1 O2 2.350(6) . ? P1 O13 1.508(5) . ? P1 C75 1.782(9) . ? P1 C81 1.810(10) . ? P1 C73 1.824(9) . ? O1 C1 1.246(10) . ? N1 C1 1.357(10) . ? N1 N2 1.390(9) . ? N1 C5 1.435(10) . ? C1 C2 1.456(11) . ? Tb2 O11 2.286(6) . ? Tb2 O3 2.291(5) . ? Tb2 O12 2.310(5) . ? Tb2 O14 2.324(5) 1_565 ? Tb2 O4 2.328(6) . ? Tb2 O8 2.342(6) . ? Tb2 O7 2.342(5) . ? P2 O14 1.491(5) . ? P2 C74 1.790(9) . ? P2 C93 1.794(11) . ? P2 C87 1.797(9) . ? O2 C11 1.255(9) . ? N2 C3 1.302(10) . ? C2 C11 1.419(11) . ? C2 C3 1.438(11) . ? O3 C15 1.245(9) . ? N3 C15 1.382(9) . ? N3 N4 1.392(9) . ? N3 C19 1.406(11) . ? C3 C4 1.483(11) . ? O4 C14 1.254(8) . ? N4 C17 1.296(10) . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C4 H4D 0.9600 . ? O5 C25 1.257(9) . ? N5 C25 1.381(10) . ? N5 N6 1.413(9) . ? N5 C29 1.420(11) . ? C5 C10 1.370(11) . ? C5 C6 1.388(12) . ? N6 C27 1.322(11) . ? C6 C7 1.397(12) . ? C6 H6B 0.9300 . ? O6 C35 1.274(9) . ? N7 C39 1.380(11) . ? N7 C43 1.406(10) . ? N7 N8 1.414(9) . ? C7 C8 1.348(13) . ? C7 H7A 0.9300 . ? O7 C39 1.241(10) . ? N8 C41 1.325(11) . ? C8 C9 1.339(13) . ? C8 H8B 0.9300 . ? O8 C38 1.255(10) . ? N9 C49 1.381(10) . ? N9 C53 1.409(10) . ? N9 N10 1.423(10) . ? C9 C10 1.393(11) . ? C9 H9A 0.9300 . ? O9 C49 1.222(11) . ? O10 C59 1.251(9) . ? N10 C51 1.313(11) . ? C10 H10B 0.9300 . ? O11 C63 1.277(9) . ? C11 C12 1.530(11) . ? N11 C63 1.376(10) . ? N11 N12 1.386(9) . ? N11 C67 1.415(10) . ? O12 C62 1.256(10) . ? N12 C65 1.321(10) . ? C12 C13 1.527(10) . ? C12 H12B 0.9700 . ? C12 H12C 0.9700 . ? C13 C14 1.521(11) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? O14 Tb2 2.324(5) 1_545 ? C14 C16 1.411(11) . ? C15 C16 1.432(12) . ? C16 C17 1.414(11) . ? C17 C18 1.512(12) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C20 1.401(12) . ? C19 C24 1.418(11) . ? C20 C21 1.378(11) . ? C20 H20A 0.9300 . ? C21 C22 1.354(12) . ? C21 H21A 0.9300 . ? C22 C23 1.406(14) . ? C22 H22A 0.9300 . ? C23 C24 1.379(12) . ? C23 H23A 0.9300 . ? C24 H24A 0.9300 . ? C25 C26 1.403(11) . ? C26 C35 1.402(12) . ? C26 C27 1.458(11) . ? C27 C28 1.467(11) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 C30 1.372(11) . ? C29 C34 1.379(11) . ? C30 C31 1.390(13) . ? C30 H30A 0.9300 . ? C31 C32 1.391(13) . ? C31 H31A 0.9300 . ? C32 C33 1.355(12) . ? C32 H32A 0.9300 . ? C33 C34 1.355(12) . ? C33 H33A 0.9300 . ? C34 H34A 0.9300 . ? C35 C36 1.525(11) . ? C36 C37 1.529(12) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 C38 1.478(12) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 C40 1.418(12) . ? C39 C40 1.404(13) . ? C40 C41 1.430(11) . ? C41 C42 1.506(12) . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 C48 1.350(11) . ? C43 C44 1.394(12) . ? C44 C45 1.374(12) . ? C44 H44A 0.9300 . ? C45 C46 1.360(12) . ? C45 H45A 0.9300 . ? C46 C47 1.356(14) . ? C46 H46A 0.9300 . ? C47 C48 1.370(14) . ? C47 H47A 0.9300 . ? C48 H48A 0.9300 . ? C49 C50 1.398(12) . ? C50 C51 1.412(11) . ? C50 C59 1.417(12) . ? C51 C52 1.487(12) . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C53 C58 1.365(12) . ? C53 C54 1.386(11) . ? C54 C55 1.391(13) . ? C54 H54A 0.9300 . ? C55 C56 1.327(14) . ? C55 H55A 0.9300 . ? C56 C57 1.393(12) . ? C56 H56A 0.9300 . ? C57 C58 1.392(12) . ? C57 H57A 0.9300 . ? C58 H58A 0.9300 . ? C59 C60 1.516(11) . ? C60 C61 1.517(11) . ? C60 H60A 0.9700 . ? C60 H60B 0.9700 . ? C61 C62 1.508(10) . ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? C62 C64 1.425(12) . ? C63 C64 1.445(10) . ? C64 C65 1.409(11) . ? C65 C66 1.515(11) . ? C66 H66A 0.9600 . ? C66 H66B 0.9600 . ? C66 H66C 0.9600 . ? C67 C72 1.392(11) . ? C67 C68 1.401(11) . ? C68 C69 1.368(11) . ? C68 H68A 0.9300 . ? C69 C70 1.392(13) . ? C69 H69A 0.9300 . ? C70 C71 1.364(13) . ? C70 H70A 0.9300 . ? C71 C72 1.366(12) . ? C71 H71A 0.9300 . ? C72 H72A 0.9300 . ? C73 C74 1.561(11) . ? C73 H73A 0.9700 . ? C73 H73B 0.9700 . ? C74 H74A 0.9700 . ? C74 H74B 0.9700 . ? C75 C80 1.391(12) . ? C75 C76 1.399(12) . ? C76 C77 1.391(13) . ? C76 H76A 0.9300 . ? C77 C78 1.333(13) . ? C77 H77A 0.9300 . ? C78 C79 1.385(14) . ? C78 H78A 0.9300 . ? C79 C80 1.372(13) . ? C79 H79A 0.9300 . ? C80 H80A 0.9300 . ? C81 C82 1.373(13) . ? C81 C86 1.404(14) . ? C82 C83 1.400(16) . ? C82 H82A 0.9300 . ? C83 C84 1.304(16) . ? C83 H83A 0.9300 . ? C84 C85 1.401(17) . ? C84 H84A 0.9300 . ? C85 C86 1.287(15) . ? C85 H85A 0.9300 . ? C86 H86A 0.9300 . ? C87 C92 1.364(12) . ? C87 C88 1.407(13) . ? C88 C89 1.335(13) . ? C88 H88A 0.9300 . ? C89 C90 1.314(14) . ? C89 H89A 0.9300 . ? C90 C91 1.384(15) . ? C90 H90A 0.9300 . ? C91 C92 1.406(14) . ? C91 H91A 0.9300 . ? C92 H92A 0.9300 . ? C93 C94 1.400(13) . ? C93 C98 1.400(13) . ? C94 C95 1.381(13) . ? C94 H94A 0.9300 . ? C95 C96 1.371(14) . ? C95 H95A 0.9300 . ? C96 C97 1.376(14) . ? C96 H96A 0.9300 . ? C97 C98 1.342(13) . ? C97 H97A 0.9300 . ? C98 H98A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Tb1 O5 110.7(2) . . ? O1 Tb1 O9 118.09(18) . . ? O5 Tb1 O9 115.9(2) . . ? O1 Tb1 O6 151.9(2) . . ? O5 Tb1 O6 74.7(2) . . ? O9 Tb1 O6 80.4(2) . . ? O1 Tb1 O13 77.8(2) . . ? O5 Tb1 O13 75.6(2) . . ? O9 Tb1 O13 76.9(2) . . ? O6 Tb1 O13 129.2(2) . . ? O1 Tb1 O10 79.1(2) . . ? O5 Tb1 O10 156.77(19) . . ? O9 Tb1 O10 73.8(2) . . ? O6 Tb1 O10 86.99(19) . . ? O13 Tb1 O10 127.63(18) . . ? O1 Tb1 O2 74.87(19) . . ? O5 Tb1 O2 81.0(2) . . ? O9 Tb1 O2 148.5(2) . . ? O6 Tb1 O2 79.02(19) . . ? O13 Tb1 O2 134.48(19) . . ? O10 Tb1 O2 81.59(19) . . ? O13 P1 C75 112.7(4) . . ? O13 P1 C81 110.2(4) . . ? C75 P1 C81 109.5(5) . . ? O13 P1 C73 112.1(4) . . ? C75 P1 C73 105.6(4) . . ? C81 P1 C73 106.4(5) . . ? C1 O1 Tb1 132.4(6) . . ? C1 N1 N2 113.6(7) . . ? C1 N1 C5 127.2(7) . . ? N2 N1 C5 119.2(7) . . ? O1 C1 N1 127.2(8) . . ? O1 C1 C2 129.0(8) . . ? N1 C1 C2 103.8(8) . . ? O11 Tb2 O3 112.96(18) . . ? O11 Tb2 O12 75.92(19) . . ? O3 Tb2 O12 153.7(2) . . ? O11 Tb2 O14 76.90(19) . 1_565 ? O3 Tb2 O14 81.18(19) . 1_565 ? O12 Tb2 O14 125.1(2) . 1_565 ? O11 Tb2 O4 75.4(2) . . ? O3 Tb2 O4 75.95(19) . . ? O12 Tb2 O4 83.00(19) . . ? O14 Tb2 O4 133.14(19) 1_565 . ? O11 Tb2 O8 150.9(2) . . ? O3 Tb2 O8 74.14(19) . . ? O12 Tb2 O8 86.73(19) . . ? O14 Tb2 O8 131.88(19) 1_565 . ? O4 Tb2 O8 79.6(2) . . ? O11 Tb2 O7 123.94(18) . . ? O3 Tb2 O7 111.40(17) . . ? O12 Tb2 O7 79.34(19) . . ? O14 Tb2 O7 77.85(19) 1_565 . ? O4 Tb2 O7 148.77(19) . . ? O8 Tb2 O7 73.9(2) . . ? O14 P2 C74 110.5(4) . . ? O14 P2 C93 109.7(4) . . ? C74 P2 C93 108.5(5) . . ? O14 P2 C87 112.4(4) . . ? C74 P2 C87 107.4(4) . . ? C93 P2 C87 108.3(5) . . ? C11 O2 Tb1 137.1(5) . . ? C3 N2 N1 106.3(7) . . ? C11 C2 C3 132.4(8) . . ? C11 C2 C1 122.5(8) . . ? C3 C2 C1 105.1(7) . . ? C15 O3 Tb2 128.9(5) . . ? C15 N3 N4 112.7(7) . . ? C15 N3 C19 128.0(8) . . ? N4 N3 C19 119.3(7) . . ? N2 C3 C2 111.3(7) . . ? N2 C3 C4 118.3(8) . . ? C2 C3 C4 130.4(8) . . ? C14 O4 Tb2 136.0(5) . . ? C17 N4 N3 105.9(7) . . ? C3 C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C4 H4D 109.5 . . ? H4B C4 H4D 109.5 . . ? H4C C4 H4D 109.5 . . ? C25 O5 Tb1 129.4(5) . . ? C25 N5 N6 110.7(7) . . ? C25 N5 C29 129.4(7) . . ? N6 N5 C29 119.7(7) . . ? C10 C5 C6 120.6(8) . . ? C10 C5 N1 121.9(8) . . ? C6 C5 N1 117.5(8) . . ? C27 N6 N5 107.4(7) . . ? C5 C6 C7 117.6(10) . . ? C5 C6 H6B 121.2 . . ? C7 C6 H6B 121.2 . . ? C35 O6 Tb1 137.5(5) . . ? C39 N7 C43 132.5(8) . . ? C39 N7 N8 108.0(8) . . ? C43 N7 N8 118.0(7) . . ? C8 C7 C6 121.4(10) . . ? C8 C7 H7A 119.3 . . ? C6 C7 H7A 119.3 . . ? C39 O7 Tb2 125.9(6) . . ? C41 N8 N7 107.1(7) . . ? C9 C8 C7 120.6(10) . . ? C9 C8 H8B 119.7 . . ? C7 C8 H8B 119.7 . . ? C38 O8 Tb2 137.0(6) . . ? C49 N9 C53 131.2(8) . . ? C49 N9 N10 109.6(8) . . ? C53 N9 N10 119.1(7) . . ? C8 C9 C10 120.5(10) . . ? C8 C9 H9A 119.7 . . ? C10 C9 H9A 119.7 . . ? C49 O9 Tb1 132.1(6) . . ? C59 O10 Tb1 138.3(6) . . ? C51 N10 N9 106.2(7) . . ? C5 C10 C9 119.3(8) . . ? C5 C10 H10B 120.3 . . ? C9 C10 H10B 120.3 . . ? C63 O11 Tb2 129.1(5) . . ? O2 C11 C2 122.2(8) . . ? O2 C11 C12 118.4(7) . . ? C2 C11 C12 119.2(8) . . ? C63 N11 N12 112.1(7) . . ? C63 N11 C67 128.3(7) . . ? N12 N11 C67 119.6(7) . . ? C62 O12 Tb2 137.3(5) . . ? C65 N12 N11 106.0(7) . . ? C13 C12 C11 113.8(7) . . ? C13 C12 H12B 108.8 . . ? C11 C12 H12B 108.8 . . ? C13 C12 H12C 108.8 . . ? C11 C12 H12C 108.8 . . ? H12B C12 H12C 107.7 . . ? P1 O13 Tb1 161.8(3) . . ? C14 C13 C12 114.9(7) . . ? C14 C13 H13A 108.5 . . ? C12 C13 H13A 108.5 . . ? C14 C13 H13B 108.5 . . ? C12 C13 H13B 108.5 . . ? H13A C13 H13B 107.5 . . ? P2 O14 Tb2 147.7(3) . 1_545 ? O4 C14 C16 122.7(8) . . ? O4 C14 C13 116.8(7) . . ? C16 C14 C13 120.5(7) . . ? O3 C15 N3 125.5(8) . . ? O3 C15 C16 131.4(8) . . ? N3 C15 C16 103.1(7) . . ? C14 C16 C17 131.4(8) . . ? C14 C16 C15 122.1(8) . . ? C17 C16 C15 106.5(7) . . ? N4 C17 C16 111.9(8) . . ? N4 C17 C18 117.1(8) . . ? C16 C17 C18 131.1(8) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 N3 123.8(8) . . ? C20 C19 C24 117.9(9) . . ? N3 C19 C24 118.3(9) . . ? C21 C20 C19 120.7(8) . . ? C21 C20 H20A 119.6 . . ? C19 C20 H20A 119.6 . . ? C22 C21 C20 121.5(10) . . ? C22 C21 H21A 119.2 . . ? C20 C21 H21A 119.2 . . ? C21 C22 C23 119.3(9) . . ? C21 C22 H22A 120.3 . . ? C23 C22 H22A 120.3 . . ? C24 C23 C22 120.5(9) . . ? C24 C23 H23A 119.7 . . ? C22 C23 H23A 119.7 . . ? C23 C24 C19 120.0(10) . . ? C23 C24 H24A 120.0 . . ? C19 C24 H24A 120.0 . . ? O5 C25 N5 123.1(8) . . ? O5 C25 C26 130.8(8) . . ? N5 C25 C26 105.8(7) . . ? C25 C26 C35 123.7(7) . . ? C25 C26 C27 106.9(8) . . ? C35 C26 C27 129.2(9) . . ? N6 C27 C26 109.0(8) . . ? N6 C27 C28 119.8(8) . . ? C26 C27 C28 131.2(9) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 C34 119.6(9) . . ? C30 C29 N5 118.4(9) . . ? C34 C29 N5 122.0(8) . . ? C29 C30 C31 119.7(10) . . ? C29 C30 H30A 120.2 . . ? C31 C30 H30A 120.2 . . ? C30 C31 C32 119.4(10) . . ? C30 C31 H31A 120.3 . . ? C32 C31 H31A 120.3 . . ? C33 C32 C31 119.7(10) . . ? C33 C32 H32A 120.2 . . ? C31 C32 H32A 120.2 . . ? C32 C33 C34 120.9(10) . . ? C32 C33 H33A 119.5 . . ? C34 C33 H33A 119.5 . . ? C33 C34 C29 120.5(9) . . ? C33 C34 H34A 119.7 . . ? C29 C34 H34A 119.7 . . ? O6 C35 C26 120.4(8) . . ? O6 C35 C36 116.0(8) . . ? C26 C35 C36 123.5(8) . . ? C35 C36 C37 113.9(7) . . ? C35 C36 H36A 108.8 . . ? C37 C36 H36A 108.8 . . ? C35 C36 H36B 108.8 . . ? C37 C36 H36B 108.8 . . ? H36A C36 H36B 107.7 . . ? C38 C37 C36 114.5(8) . . ? C38 C37 H37A 108.6 . . ? C36 C37 H37A 108.6 . . ? C38 C37 H37B 108.6 . . ? C36 C37 H37B 108.6 . . ? H37A C37 H37B 107.6 . . ? O8 C38 C40 120.4(9) . . ? O8 C38 C37 119.7(8) . . ? C40 C38 C37 119.7(9) . . ? O7 C39 N7 119.3(9) . . ? O7 C39 C40 131.4(9) . . ? N7 C39 C40 109.3(9) . . ? C39 C40 C38 122.2(8) . . ? C39 C40 C41 103.8(8) . . ? C38 C40 C41 133.5(9) . . ? N8 C41 C40 111.7(8) . . ? N8 C41 C42 117.2(8) . . ? C40 C41 C42 131.1(9) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C48 C43 C44 120.7(9) . . ? C48 C43 N7 120.0(9) . . ? C44 C43 N7 119.3(8) . . ? C45 C44 C43 118.7(9) . . ? C45 C44 H44A 120.7 . . ? C43 C44 H44A 120.7 . . ? C46 C45 C44 120.9(10) . . ? C46 C45 H45A 119.5 . . ? C44 C45 H45A 119.5 . . ? C47 C46 C45 118.4(10) . . ? C47 C46 H46A 120.8 . . ? C45 C46 H46A 120.8 . . ? C46 C47 C48 122.7(10) . . ? C46 C47 H47A 118.6 . . ? C48 C47 H47A 118.6 . . ? C43 C48 C47 118.3(10) . . ? C43 C48 H48A 120.8 . . ? C47 C48 H48A 120.8 . . ? O9 C49 N9 122.0(9) . . ? O9 C49 C50 131.7(8) . . ? N9 C49 C50 106.4(9) . . ? C49 C50 C51 106.5(8) . . ? C49 C50 C59 122.1(8) . . ? C51 C50 C59 131.4(9) . . ? N10 C51 C50 111.4(9) . . ? N10 C51 C52 116.7(8) . . ? C50 C51 C52 131.9(9) . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C58 C53 C54 120.3(9) . . ? C58 C53 N9 120.9(8) . . ? C54 C53 N9 118.8(9) . . ? C53 C54 C55 118.5(10) . . ? C53 C54 H54A 120.8 . . ? C55 C54 H54A 120.8 . . ? C56 C55 C54 122.7(11) . . ? C56 C55 H55A 118.6 . . ? C54 C55 H55A 118.6 . . ? C55 C56 C57 118.6(10) . . ? C55 C56 H56A 120.7 . . ? C57 C56 H56A 120.7 . . ? C58 C57 C56 120.7(10) . . ? C58 C57 H57A 119.7 . . ? C56 C57 H57A 119.7 . . ? C53 C58 C57 119.3(9) . . ? C53 C58 H58A 120.4 . . ? C57 C58 H58A 120.4 . . ? O10 C59 C50 122.0(9) . . ? O10 C59 C60 117.0(8) . . ? C50 C59 C60 120.9(8) . . ? C59 C60 C61 115.7(7) . . ? C59 C60 H60A 108.4 . . ? C61 C60 H60A 108.4 . . ? C59 C60 H60B 108.4 . . ? C61 C60 H60B 108.4 . . ? H60A C60 H60B 107.4 . . ? C62 C61 C60 114.4(7) . . ? C62 C61 H61A 108.7 . . ? C60 C61 H61A 108.7 . . ? C62 C61 H61B 108.7 . . ? C60 C61 H61B 108.7 . . ? H61A C61 H61B 107.6 . . ? O12 C62 C64 122.3(7) . . ? O12 C62 C61 118.4(8) . . ? C64 C62 C61 119.3(8) . . ? O11 C63 N11 125.7(8) . . ? O11 C63 C64 129.8(8) . . ? N11 C63 C64 104.5(7) . . ? C65 C64 C62 132.6(7) . . ? C65 C64 C63 105.3(7) . . ? C62 C64 C63 121.8(7) . . ? N12 C65 C64 111.9(7) . . ? N12 C65 C66 117.7(8) . . ? C64 C65 C66 130.3(7) . . ? C65 C66 H66A 109.5 . . ? C65 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C65 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C72 C67 C68 120.1(8) . . ? C72 C67 N11 118.6(8) . . ? C68 C67 N11 121.3(8) . . ? C69 C68 C67 119.6(9) . . ? C69 C68 H68A 120.2 . . ? C67 C68 H68A 120.2 . . ? C68 C69 C70 120.0(9) . . ? C68 C69 H69A 120.0 . . ? C70 C69 H69A 120.0 . . ? C71 C70 C69 119.6(9) . . ? C71 C70 H70A 120.2 . . ? C69 C70 H70A 120.2 . . ? C70 C71 C72 121.9(10) . . ? C70 C71 H71A 119.0 . . ? C72 C71 H71A 119.0 . . ? C71 C72 C67 118.7(9) . . ? C71 C72 H72A 120.6 . . ? C67 C72 H72A 120.6 . . ? C74 C73 P1 111.9(6) . . ? C74 C73 H73A 109.2 . . ? P1 C73 H73A 109.2 . . ? C74 C73 H73B 109.2 . . ? P1 C73 H73B 109.2 . . ? H73A C73 H73B 107.9 . . ? C73 C74 P2 109.6(6) . . ? C73 C74 H74A 109.8 . . ? P2 C74 H74A 109.8 . . ? C73 C74 H74B 109.8 . . ? P2 C74 H74B 109.8 . . ? H74A C74 H74B 108.2 . . ? C80 C75 C76 116.1(9) . . ? C80 C75 P1 121.5(8) . . ? C76 C75 P1 122.4(8) . . ? C77 C76 C75 119.6(10) . . ? C77 C76 H76A 120.2 . . ? C75 C76 H76A 120.2 . . ? C78 C77 C76 123.6(11) . . ? C78 C77 H77A 118.2 . . ? C76 C77 H77A 118.2 . . ? C77 C78 C79 117.3(11) . . ? C77 C78 H78A 121.3 . . ? C79 C78 H78A 121.3 . . ? C80 C79 C78 120.9(11) . . ? C80 C79 H79A 119.6 . . ? C78 C79 H79A 119.6 . . ? C79 C80 C75 122.1(10) . . ? C79 C80 H80A 118.9 . . ? C75 C80 H80A 118.9 . . ? C82 C81 C86 118.6(11) . . ? C82 C81 P1 122.1(9) . . ? C86 C81 P1 119.2(9) . . ? C81 C82 C83 118.4(12) . . ? C81 C82 H82A 120.8 . . ? C83 C82 H82A 120.8 . . ? C84 C83 C82 120.8(13) . . ? C84 C83 H83A 119.6 . . ? C82 C83 H83A 119.6 . . ? C83 C84 C85 120.5(14) . . ? C83 C84 H84A 119.7 . . ? C85 C84 H84A 119.7 . . ? C86 C85 C84 120.3(13) . . ? C86 C85 H85A 119.8 . . ? C84 C85 H85A 119.8 . . ? C85 C86 C81 121.2(14) . . ? C85 C86 H86A 119.4 . . ? C81 C86 H86A 119.4 . . ? C92 C87 C88 119.6(9) . . ? C92 C87 P2 122.9(8) . . ? C88 C87 P2 117.2(8) . . ? C89 C88 C87 119.0(10) . . ? C89 C88 H88A 120.5 . . ? C87 C88 H88A 120.5 . . ? C90 C89 C88 123.5(12) . . ? C90 C89 H89A 118.2 . . ? C88 C89 H89A 118.2 . . ? C89 C90 C91 119.0(11) . . ? C89 C90 H90A 120.5 . . ? C91 C90 H90A 120.5 . . ? C90 C91 C92 120.2(11) . . ? C90 C91 H91A 119.9 . . ? C92 C91 H91A 119.9 . . ? C87 C92 C91 118.3(10) . . ? C87 C92 H92A 120.9 . . ? C91 C92 H92A 120.9 . . ? C94 C93 C98 117.6(10) . . ? C94 C93 P2 119.7(8) . . ? C98 C93 P2 122.3(9) . . ? C95 C94 C93 119.8(10) . . ? C95 C94 H94A 120.1 . . ? C93 C94 H94A 120.1 . . ? C96 C95 C94 120.4(11) . . ? C96 C95 H95A 119.8 . . ? C94 C95 H95A 119.8 . . ? C95 C96 C97 120.1(11) . . ? C95 C96 H96A 119.9 . . ? C97 C96 H96A 119.9 . . ? C98 C97 C96 120.0(11) . . ? C98 C97 H97A 120.0 . . ? C96 C97 H97A 120.0 . . ? C97 C98 C93 121.9(11) . . ? C97 C98 H98A 119.0 . . ? C93 C98 H98A 119.0 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.812 _refine_diff_density_min -1.379 _refine_diff_density_rms 0.140