# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Yu Tang' _publ_contact_author_email tangyu@lzu.edu.cn loop_ _publ_author_name 'Xuhuan Yan' 'Zhenzhong Yan' 'Ye Zhang' 'Weisheng Liu' 'Yu Tang' 'Min-Yu Tan' #===END data_666992 _database_code_depnum_ccdc_archive 'CCDC 666992' #TrackingRef '- cif_Revision.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84 H92 N14 O28 Sm2' _chemical_formula_weight 2046.44 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' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.6358(13) _cell_length_b 14.0938(11) _cell_length_c 19.7424(17) _cell_angle_alpha 90.00 _cell_angle_beta 101.880(3) _cell_angle_gamma 90.00 _cell_volume 4529.7(6) _cell_formula_units_Z 2 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.37 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.500 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2084 _exptl_absorpt_coefficient_mu 1.369 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5778 _exptl_absorpt_correction_T_max 0.9224 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 27307 _diffrn_reflns_av_R_equivalents 0.0391 _diffrn_reflns_av_sigmaI/netI 0.0456 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 27.57 _reflns_number_total 10212 _reflns_number_gt 7889 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.Standard DFIX restraint was used for the distance of the disordered atoms C46 and C47. #============================================================================== The Following Model and Quality ALERTS were generated - (Acta-Mode) <<< #============================================================================== Format: alert-number_ALERT_alert-type_alert-level text PLAT241_ALERT_2_A Check High Ueq as Compared to Neighbors for C46 The larger than normal range of thermal motion is mostly due to the difference between the disordered ethyl group and the other atoms which are not disordered. ; _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^)+(0.0357P)^2^+1.8146P] 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 SHELXL _refine_ls_extinction_coef 0.00059(11) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 10212 _refine_ls_number_parameters 580 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0505 _refine_ls_R_factor_gt 0.0352 _refine_ls_wR_factor_ref 0.0852 _refine_ls_wR_factor_gt 0.0777 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O13 O 0.33586(13) 0.91172(15) 0.46923(13) 0.0544(6) Uani 1 1 d . . . C50 C -0.0204(4) 0.9540(4) 0.3146(4) 0.123(2) Uani 1 1 d . . . H50 H -0.0647 0.9210 0.2887 0.148 Uiso 1 1 calc R . . C52 C 0.0469(4) 0.9727(4) 0.2869(3) 0.1084(18) Uani 1 1 d . . . H52 H 0.0487 0.9506 0.2428 0.130 Uiso 1 1 calc R . . C51 C -0.0229(3) 0.9831(4) 0.3794(4) 0.122(2) Uani 1 1 d . . . H51 H -0.0681 0.9687 0.3985 0.147 Uiso 1 1 calc R . . C39 C 0.53179(18) 0.9298(2) 0.41378(17) 0.0499(8) Uani 1 1 d . . . H39 H 0.5801 0.8956 0.4163 0.060 Uiso 1 1 calc R . . C33 C 0.0422(2) 1.0343(3) 0.4172(3) 0.0889(14) Uani 1 1 d . . . H33 H 0.0406 1.0542 0.4618 0.107 Uiso 1 1 calc R . . C22 C 0.1116(3) 1.0239(3) 0.3236(3) 0.0790(12) Uani 1 1 d . . . H22 H 0.1568 1.0369 0.3042 0.095 Uiso 1 1 calc R . . C20 C 0.17742(18) 1.1187(2) 0.42815(19) 0.0534(8) Uani 1 1 d . . . H20A H 0.1778 1.1782 0.4035 0.064 Uiso 1 1 calc R . . H20B H 0.1668 1.1327 0.4736 0.064 Uiso 1 1 calc R . . C21 C 0.1096(2) 1.0561(3) 0.3893(2) 0.0585(9) Uani 1 1 d . . . C25 C 0.47131(18) 0.8945(2) 0.44469(17) 0.0473(8) Uani 1 1 d . . . H25 H 0.4790 0.8370 0.4682 0.057 Uiso 1 1 calc R . . C18 C 0.31092(17) 1.0909(2) 0.39631(15) 0.0390(7) Uani 1 1 d . . . C17 C 0.38704(16) 1.0321(2) 0.40525(15) 0.0384(6) Uani 1 1 d . . . N6 N 0.25752(15) 1.0734(2) 0.43573(14) 0.0497(7) Uani 1 1 d . . . H6 H 0.2710 1.0322 0.4683 0.060 Uiso 1 1 calc R . . C24 C 0.39857(17) 0.9448(2) 0.44077(16) 0.0417(7) Uani 1 1 d . . . O10 O 0.29895(12) 1.15576(16) 0.35265(12) 0.0523(6) Uani 1 1 d . . . Sm1 Sm 0.725666(8) 0.724199(11) 0.731078(8) 0.03698(7) Uani 1 1 d . . . N3 N 0.79428(15) 0.5738(2) 0.65761(17) 0.0542(7) Uani 1 1 d . . . O6 O 0.77243(14) 0.65145(18) 0.62791(12) 0.0585(6) Uani 1 1 d . . . O2 O 0.63183(15) 0.82627(19) 0.78286(13) 0.0611(6) Uani 1 1 d . . . O7 O 0.77980(15) 0.56236(17) 0.71758(14) 0.0616(6) Uani 1 1 d . . . O5 O 0.67438(13) 0.61126(19) 0.81142(13) 0.0613(7) Uani 1 1 d . . . O4 O 0.79410(14) 0.6703(2) 0.85138(12) 0.0661(7) Uani 1 1 d . . . O1 O 0.75641(16) 0.87633(19) 0.79827(16) 0.0752(8) Uani 1 1 d . . . O3 O 0.6632(2) 0.9657(2) 0.82776(19) 0.0997(11) Uani 1 1 d . . . O8 O 0.82779(18) 0.5120(2) 0.63004(16) 0.0844(9) Uani 1 1 d . . . N1 N 0.6830(2) 0.8918(2) 0.80410(16) 0.0636(8) Uani 1 1 d . . . N2 N 0.73872(18) 0.6108(2) 0.85838(15) 0.0583(8) Uani 1 1 d . . . O9 O 0.74798(19) 0.5557(3) 0.90662(15) 0.0943(10) Uani 1 1 d . . . N5 N 0.26152(18) 0.70305(19) 0.54770(15) 0.0517(7) Uani 1 1 d . . . N7 N 0.46761(15) 0.6412(2) 0.65917(14) 0.0583(8) Uani 1 1 d . . . H7 H 0.4210 0.6304 0.6321 0.070 Uiso 1 1 calc R . . C5 C 0.40207(19) 0.7067(3) 0.74930(17) 0.0490(8) Uani 1 1 d . . . C3 C 0.2801(2) 0.7274(3) 0.7951(2) 0.0730(12) Uani 1 1 d . . . H3 H 0.2394 0.7018 0.8157 0.088 Uiso 1 1 calc R . . C4 C 0.3408(2) 0.6687(3) 0.77909(18) 0.0564(9) Uani 1 1 d . . . H4 H 0.3402 0.6041 0.7883 0.068 Uiso 1 1 calc R . . C6 C 0.46934(19) 0.6445(3) 0.73332(18) 0.0604(10) Uani 1 1 d . . . H6A H 0.5221 0.6686 0.7574 0.072 Uiso 1 1 calc R . . H6B H 0.4631 0.5808 0.7501 0.072 Uiso 1 1 calc R . . C2 C 0.2798(3) 0.8226(4) 0.7809(2) 0.0767(12) Uani 1 1 d . . . H2 H 0.2388 0.8614 0.7915 0.092 Uiso 1 1 calc R . . C1 C 0.3393(3) 0.8598(3) 0.7514(2) 0.0756(11) Uani 1 1 d . . . H1 H 0.3389 0.9243 0.7414 0.091 Uiso 1 1 calc R . . C9 C 0.0857(4) 0.5953(4) 0.5906(3) 0.119(2) Uani 1 1 d . . . H9 H 0.1180 0.5484 0.6160 0.143 Uiso 1 1 calc R . . C10 C 0.1221(3) 0.6785(4) 0.5761(2) 0.0798(13) Uani 1 1 d . . . C11 C 0.2122(3) 0.6951(3) 0.6005(2) 0.0793(13) Uani 1 1 d . . . H11A H 0.2193 0.7529 0.6277 0.095 Uiso 1 1 calc R . . H11B H 0.2343 0.6434 0.6313 0.095 Uiso 1 1 calc R . . C8 C 0.0705(3) 0.7451(4) 0.5387(3) 0.1030(18) Uani 1 1 d . . . H8A H 0.0923 0.8028 0.5285 0.124 Uiso 1 1 calc R . . O11 O 0.60018(12) 0.67276(17) 0.66692(11) 0.0508(5) Uani 1 1 d . . . O12 O 0.86751(13) 0.75757(17) 0.74093(14) 0.0569(6) Uani 1 1 d . . . C14 C 0.53118(17) 0.6532(2) 0.63047(15) 0.0403(7) Uani 1 1 d . . . C15 C 0.5216(2) 0.6450(2) 0.55395(16) 0.0498(8) Uani 1 1 d . . . C16 C 0.5878(2) 0.6740(3) 0.52550(19) 0.0616(9) Uani 1 1 d . . . H16 H 0.6348 0.6975 0.5544 0.074 Uiso 1 1 calc R . . N4 N 1.00022(16) 0.7911(2) 0.78420(19) 0.0645(9) Uani 1 1 d . . . C30 C 0.9229(2) 0.7808(3) 0.7889(3) 0.0715(11) Uani 1 1 d . . . H30 H 0.9095 0.7921 0.8317 0.086 Uiso 1 1 calc R . . C36 C -0.0135(4) 0.7287(5) 0.5156(4) 0.127(2) Uani 1 1 d . . . H36 H -0.0463 0.7740 0.4888 0.153 Uiso 1 1 calc R . . C37 C -0.0471(4) 0.6461(7) 0.5324(5) 0.147(4) Uani 1 1 d . . . H37 H -0.1033 0.6356 0.5194 0.177 Uiso 1 1 calc R . . C38 C 0.0030(5) 0.5798(6) 0.5684(5) 0.153(3) Uani 1 1 d . . . H38 H -0.0192 0.5222 0.5785 0.184 Uiso 1 1 calc R . . C41 C 0.4518(3) 0.6092(3) 0.5090(2) 0.0697(12) Uani 1 1 d . . . C43 C 0.5171(5) 0.6337(4) 0.4119(3) 0.111(2) Uani 1 1 d . . . H43 H 0.5156 0.6299 0.3646 0.134 Uiso 1 1 calc R . . C42 C 0.4510(4) 0.6041(4) 0.4377(2) 0.101(2) Uani 1 1 d . . . H42 H 0.4049 0.5803 0.4076 0.122 Uiso 1 1 calc R . . C44 C 0.5846(4) 0.6685(3) 0.4552(2) 0.0893(15) Uani 1 1 d . . . H44 H 0.6292 0.6889 0.4373 0.107 Uiso 1 1 calc R . . O14 O 0.38911(15) 0.5798(2) 0.53791(16) 0.0933(11) Uani 1 1 d . . . C46 C 0.3091(3) 0.5620(5) 0.4982(4) 0.176(4) Uani 1 1 d D . . H46A H 0.3132 0.5575 0.4500 0.211 Uiso 1 1 calc R . . H46B H 0.2917 0.5003 0.5117 0.211 Uiso 1 1 calc R . . C47 C 0.2515(2) 0.6225(3) 0.5024(3) 0.107(2) Uani 1 1 d D . . H47A H 0.2064 0.5859 0.5132 0.128 Uiso 1 1 calc R . . H47B H 0.2324 0.6472 0.4560 0.128 Uiso 1 1 calc R . . C48 C 0.2589(2) 0.7942(3) 0.5136(2) 0.0600(10) Uani 1 1 d . . . H48A H 0.2414 0.8426 0.5424 0.072 Uiso 1 1 calc R . . H48B H 0.2194 0.7921 0.4700 0.072 Uiso 1 1 calc R . . C54 C 0.3427(2) 0.8194(2) 0.5004(2) 0.0562(9) Uani 1 1 d . . . H54A H 0.3831 0.8201 0.5435 0.067 Uiso 1 1 calc R . . H54B H 0.3596 0.7733 0.4696 0.067 Uiso 1 1 calc R . . C55 C 0.4003(2) 0.8027(3) 0.7361(2) 0.0680(11) Uani 1 1 d . . . H55 H 0.4413 0.8296 0.7165 0.082 Uiso 1 1 calc R . . C56 C 1.0282(3) 0.7754(4) 0.7218(3) 0.0906(15) Uani 1 1 d . . . H56A H 1.0621 0.7198 0.7266 0.136 Uiso 1 1 calc R . . H56B H 1.0594 0.8293 0.7123 0.136 Uiso 1 1 calc R . . H56C H 0.9818 0.7667 0.6844 0.136 Uiso 1 1 calc R . . C57 C 1.0620(3) 0.8162(5) 0.8454(3) 0.129(2) Uani 1 1 d . . . H57A H 1.0354 0.8407 0.8805 0.193 Uiso 1 1 calc R . . H57B H 1.0981 0.8637 0.8334 0.193 Uiso 1 1 calc R . . H57C H 1.0933 0.7609 0.8626 0.193 Uiso 1 1 calc R . . C58 C 0.45015(18) 1.0654(2) 0.37495(16) 0.0457(7) Uani 1 1 d . . . H58 H 0.4437 1.1229 0.3514 0.055 Uiso 1 1 calc R . . C59 C 0.52195(19) 1.0149(3) 0.37920(17) 0.0521(8) Uani 1 1 d . . . H59 H 0.5635 1.0383 0.3587 0.063 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 O13 0.0462(12) 0.0475(13) 0.0748(16) 0.0208(12) 0.0247(11) 0.0105(10) C50 0.082(4) 0.075(4) 0.188(7) 0.004(4) -0.028(4) -0.025(3) C52 0.118(4) 0.073(3) 0.118(5) -0.010(3) -0.012(4) -0.010(3) C51 0.070(3) 0.107(5) 0.191(7) 0.014(5) 0.028(4) -0.031(3) C39 0.0380(16) 0.059(2) 0.053(2) 0.0001(17) 0.0115(14) 0.0118(15) C33 0.058(2) 0.087(3) 0.127(4) 0.013(3) 0.032(3) -0.009(2) C22 0.079(3) 0.062(3) 0.093(3) -0.001(2) 0.010(2) -0.008(2) C20 0.0390(16) 0.057(2) 0.067(2) 0.0044(18) 0.0156(16) 0.0100(15) C21 0.0447(18) 0.050(2) 0.081(3) 0.0132(19) 0.0139(18) 0.0016(15) C25 0.0455(17) 0.0464(19) 0.0501(19) 0.0053(15) 0.0101(15) 0.0084(14) C18 0.0374(15) 0.0385(17) 0.0411(17) 0.0025(13) 0.0075(13) 0.0016(12) C17 0.0365(14) 0.0438(17) 0.0353(16) 0.0008(13) 0.0081(12) 0.0041(12) N6 0.0403(13) 0.0567(17) 0.0552(17) 0.0162(14) 0.0171(12) 0.0115(12) C24 0.0386(15) 0.0432(17) 0.0444(17) -0.0006(14) 0.0111(13) 0.0024(13) O10 0.0452(12) 0.0514(14) 0.0630(15) 0.0207(12) 0.0174(11) 0.0110(10) Sm1 0.02823(8) 0.04231(11) 0.04088(10) 0.00261(7) 0.00826(6) 0.00126(6) N3 0.0363(14) 0.0566(19) 0.069(2) -0.0175(16) 0.0085(13) 0.0004(13) O6 0.0551(14) 0.0650(17) 0.0574(15) 0.0020(13) 0.0165(12) 0.0128(12) O2 0.0587(14) 0.0627(16) 0.0685(16) -0.0089(14) 0.0281(12) 0.0014(13) O7 0.0728(16) 0.0474(14) 0.0682(17) 0.0040(12) 0.0227(13) 0.0049(12) O5 0.0409(12) 0.0859(19) 0.0570(15) 0.0198(13) 0.0098(11) -0.0041(12) O4 0.0546(14) 0.0869(19) 0.0519(15) 0.0055(14) -0.0001(11) -0.0158(14) O1 0.0627(16) 0.0659(18) 0.096(2) -0.0210(16) 0.0143(15) -0.0038(13) O3 0.134(3) 0.0633(19) 0.115(3) -0.0230(18) 0.055(2) 0.0141(19) O8 0.0815(19) 0.078(2) 0.095(2) -0.0342(17) 0.0221(16) 0.0182(16) N1 0.082(2) 0.056(2) 0.0573(19) -0.0061(16) 0.0240(17) 0.0080(18) N2 0.0538(17) 0.080(2) 0.0430(17) 0.0095(16) 0.0149(14) 0.0049(16) O9 0.094(2) 0.130(3) 0.0585(18) 0.0483(19) 0.0132(15) 0.001(2) N5 0.0568(16) 0.0424(16) 0.0554(17) -0.0023(13) 0.0105(14) -0.0078(12) N7 0.0322(13) 0.091(2) 0.0498(17) -0.0074(15) 0.0040(12) -0.0028(13) C5 0.0385(16) 0.066(2) 0.0408(18) 0.0076(16) 0.0041(13) -0.0010(14) C3 0.061(2) 0.103(4) 0.062(2) 0.001(2) 0.0306(19) -0.001(2) C4 0.0501(19) 0.068(2) 0.053(2) 0.0103(18) 0.0150(16) -0.0024(17) C6 0.0418(18) 0.089(3) 0.051(2) 0.0109(19) 0.0112(15) 0.0035(17) C2 0.076(3) 0.089(3) 0.065(3) -0.012(2) 0.015(2) 0.018(2) C1 0.087(3) 0.061(3) 0.077(3) -0.002(2) 0.012(2) 0.004(2) C9 0.124(4) 0.104(4) 0.147(5) -0.011(4) 0.069(4) -0.052(4) C10 0.093(3) 0.085(3) 0.074(3) -0.015(3) 0.045(3) -0.031(3) C11 0.099(3) 0.084(3) 0.057(2) 0.007(2) 0.022(2) -0.032(3) C8 0.084(4) 0.113(4) 0.127(5) -0.022(4) 0.058(4) -0.022(3) O11 0.0365(11) 0.0730(16) 0.0414(12) -0.0002(11) 0.0047(9) -0.0077(11) O12 0.0310(11) 0.0667(16) 0.0705(17) 0.0033(13) 0.0050(11) -0.0058(10) C14 0.0356(15) 0.0376(17) 0.0445(17) -0.0003(13) 0.0005(13) 0.0066(12) C15 0.0571(19) 0.048(2) 0.0395(17) -0.0020(15) -0.0024(15) 0.0200(15) C16 0.079(2) 0.057(2) 0.050(2) 0.0028(18) 0.0152(18) 0.0198(19) N4 0.0319(14) 0.069(2) 0.091(2) 0.0017(17) 0.0072(15) -0.0072(13) C30 0.052(2) 0.076(3) 0.089(3) 0.005(2) 0.019(2) -0.0030(19) C36 0.073(4) 0.155(6) 0.166(7) -0.040(5) 0.053(4) -0.001(4) C37 0.087(4) 0.171(8) 0.205(9) -0.094(7) 0.079(5) -0.046(5) C38 0.130(6) 0.132(6) 0.226(9) -0.056(6) 0.103(7) -0.077(5) C41 0.072(3) 0.060(2) 0.062(2) -0.021(2) -0.021(2) 0.038(2) C43 0.182(6) 0.100(4) 0.045(3) -0.001(3) 0.008(4) 0.071(4) C42 0.137(5) 0.085(4) 0.056(3) -0.031(3) -0.040(3) 0.058(3) C44 0.141(4) 0.084(3) 0.047(2) 0.008(2) 0.030(3) 0.044(3) O14 0.0418(14) 0.122(3) 0.101(2) -0.058(2) -0.0207(15) 0.0139(15) C46 0.055(3) 0.186(6) 0.244(8) -0.162(6) -0.068(4) 0.043(3) C47 0.049(2) 0.089(3) 0.166(5) -0.076(3) -0.016(3) 0.006(2) C48 0.0512(19) 0.064(2) 0.068(2) 0.0191(19) 0.0214(18) 0.0073(17) C54 0.0490(18) 0.048(2) 0.071(2) 0.0163(18) 0.0105(17) 0.0028(16) C55 0.063(2) 0.076(3) 0.066(3) 0.012(2) 0.017(2) -0.012(2) C56 0.071(3) 0.112(4) 0.093(4) 0.008(3) 0.028(3) 0.010(3) C57 0.081(3) 0.181(6) 0.117(5) -0.034(5) 0.004(3) -0.039(4) C58 0.0426(16) 0.0490(19) 0.0463(18) 0.0071(15) 0.0108(14) 0.0036(14) C59 0.0412(17) 0.067(2) 0.052(2) 0.0076(17) 0.0191(15) 0.0048(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O13 C24 1.365(3) . ? O13 C54 1.434(4) . ? C50 C51 1.353(8) . ? C50 C52 1.368(8) . ? C50 H50 0.9300 . ? C52 C22 1.373(6) . ? C52 H52 0.9300 . ? C51 C33 1.385(7) . ? C51 H51 0.9300 . ? C39 C59 1.372(5) . ? C39 C25 1.373(4) . ? C39 H39 0.9300 . ? C33 C21 1.382(5) . ? C33 H33 0.9300 . ? C22 C21 1.381(6) . ? C22 H22 0.9300 . ? C20 N6 1.457(4) . ? C20 C21 1.510(5) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C25 C24 1.391(4) . ? C25 H25 0.9300 . ? C18 O10 1.244(3) . ? C18 N6 1.319(4) . ? C18 C17 1.494(4) . ? C17 C58 1.392(4) . ? C17 C24 1.409(4) . ? N6 H6 0.8600 . ? O10 Sm1 2.342(2) 3_676 ? Sm1 O11 2.324(2) . ? Sm1 O10 2.342(2) 3_676 ? Sm1 O12 2.375(2) . ? Sm1 O7 2.487(2) . ? Sm1 O2 2.492(2) . ? Sm1 O5 2.517(2) . ? Sm1 O1 2.518(3) . ? Sm1 O4 2.530(2) . ? Sm1 O6 2.541(2) . ? N3 O8 1.221(3) . ? N3 O6 1.260(4) . ? N3 O7 1.266(4) . ? O2 N1 1.267(4) . ? O5 N2 1.264(4) . ? O4 N2 1.274(4) . ? O1 N1 1.269(4) . ? O3 N1 1.215(4) . ? N2 O9 1.214(4) . ? N5 C47 1.434(5) . ? N5 C48 1.447(4) . ? N5 C11 1.458(5) . ? N7 C14 1.309(4) . ? N7 C6 1.459(4) . ? N7 H7 0.8600 . ? C5 C55 1.378(5) . ? C5 C4 1.385(4) . ? C5 C6 1.505(5) . ? C3 C2 1.370(6) . ? C3 C4 1.391(5) . ? C3 H3 0.9300 . ? C4 H4 0.9300 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C2 C1 1.354(6) . ? C2 H2 0.9300 . ? C1 C55 1.377(6) . ? C1 H1 0.9300 . ? C9 C38 1.374(9) . ? C9 C10 1.376(6) . ? C9 H9 0.9300 . ? C10 C8 1.379(7) . ? C10 C11 1.496(6) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C8 C36 1.396(8) . ? C8 H8A 0.9300 . ? O11 C14 1.254(3) . ? O12 C30 1.222(5) . ? C14 C15 1.491(4) . ? C15 C16 1.397(5) . ? C15 C41 1.402(5) . ? C16 C44 1.380(5) . ? C16 H16 0.9300 . ? N4 C30 1.317(5) . ? N4 C56 1.420(6) . ? N4 C57 1.460(6) . ? C30 H30 0.9300 . ? C36 C37 1.362(9) . ? C36 H36 0.9300 . ? C37 C38 1.353(11) . ? C37 H37 0.9300 . ? C38 H38 0.9300 . ? C41 O14 1.353(5) . ? C41 C42 1.407(6) . ? C43 C44 1.355(8) . ? C43 C42 1.367(8) . ? C43 H43 0.9300 . ? C42 H42 0.9300 . ? C44 H44 0.9300 . ? O14 C46 1.420(5) . ? C46 C47 1.298(6) . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C48 C54 1.512(4) . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C54 H54A 0.9700 . ? C54 H54B 0.9700 . ? C55 H55 0.9300 . ? C56 H56A 0.9600 . ? C56 H56B 0.9600 . ? C56 H56C 0.9600 . ? C57 H57A 0.9600 . ? C57 H57B 0.9600 . ? C57 H57C 0.9600 . ? C58 C59 1.378(4) . ? C58 H58 0.9300 . ? C59 H59 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 C24 O13 C54 119.1(2) . . ? C51 C50 C52 120.5(6) . . ? C51 C50 H50 119.8 . . ? C52 C50 H50 119.8 . . ? C50 C52 C22 120.5(6) . . ? C50 C52 H52 119.8 . . ? C22 C52 H52 119.8 . . ? C50 C51 C33 119.6(5) . . ? C50 C51 H51 120.2 . . ? C33 C51 H51 120.2 . . ? C59 C39 C25 121.0(3) . . ? C59 C39 H39 119.5 . . ? C25 C39 H39 119.5 . . ? C21 C33 C51 120.7(5) . . ? C21 C33 H33 119.6 . . ? C51 C33 H33 119.6 . . ? C52 C22 C21 120.1(5) . . ? C52 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? N6 C20 C21 111.6(3) . . ? N6 C20 H20A 109.3 . . ? C21 C20 H20A 109.3 . . ? N6 C20 H20B 109.3 . . ? C21 C20 H20B 109.3 . . ? H20A C20 H20B 108.0 . . ? C22 C21 C33 118.6(4) . . ? C22 C21 C20 120.7(3) . . ? C33 C21 C20 120.6(4) . . ? C39 C25 C24 119.9(3) . . ? C39 C25 H25 120.0 . . ? C24 C25 H25 120.0 . . ? O10 C18 N6 121.0(3) . . ? O10 C18 C17 120.1(3) . . ? N6 C18 C17 118.9(3) . . ? C58 C17 C24 118.1(3) . . ? C58 C17 C18 117.2(3) . . ? C24 C17 C18 124.7(2) . . ? C18 N6 C20 124.7(3) . . ? C18 N6 H6 117.6 . . ? C20 N6 H6 117.6 . . ? O13 C24 C25 122.2(3) . . ? O13 C24 C17 117.8(2) . . ? C25 C24 C17 120.0(3) . . ? C18 O10 Sm1 178.8(2) . 3_676 ? O11 Sm1 O10 80.42(8) . 3_676 ? O11 Sm1 O12 150.76(8) . . ? O10 Sm1 O12 86.63(8) 3_676 . ? O11 Sm1 O7 87.70(9) . . ? O10 Sm1 O7 126.98(8) 3_676 . ? O12 Sm1 O7 79.32(8) . . ? O11 Sm1 O2 80.52(8) . . ? O10 Sm1 O2 80.75(8) 3_676 . ? O12 Sm1 O2 123.23(9) . . ? O7 Sm1 O2 147.66(8) . . ? O11 Sm1 O5 76.30(8) . . ? O10 Sm1 O5 150.35(7) 3_676 . ? O12 Sm1 O5 122.26(8) . . ? O7 Sm1 O5 70.41(8) . . ? O2 Sm1 O5 77.54(9) . . ? O11 Sm1 O1 127.97(8) . . ? O10 Sm1 O1 75.15(9) 3_676 . ? O12 Sm1 O1 72.39(9) . . ? O7 Sm1 O1 143.02(9) . . ? O2 Sm1 O1 50.85(8) . . ? O5 Sm1 O1 105.37(10) . . ? O11 Sm1 O4 126.75(8) . . ? O10 Sm1 O4 149.20(9) 3_676 . ? O12 Sm1 O4 74.63(8) . . ? O7 Sm1 O4 73.89(9) . . ? O2 Sm1 O4 89.25(9) . . ? O5 Sm1 O4 50.50(8) . . ? O1 Sm1 O4 75.97(9) . . ? O11 Sm1 O6 79.98(7) . . ? O10 Sm1 O6 76.32(8) 3_676 . ? O12 Sm1 O6 71.49(8) . . ? O7 Sm1 O6 50.70(8) . . ? O2 Sm1 O6 151.98(8) . . ? O5 Sm1 O6 116.70(9) . . ? O1 Sm1 O6 134.70(9) . . ? O4 Sm1 O6 118.59(8) . . ? O8 N3 O6 121.8(3) . . ? O8 N3 O7 121.2(3) . . ? O6 N3 O7 117.0(3) . . ? N3 O6 Sm1 94.84(19) . . ? N1 O2 Sm1 97.00(18) . . ? N3 O7 Sm1 97.27(19) . . ? N2 O5 Sm1 96.86(18) . . ? N2 O4 Sm1 95.95(18) . . ? N1 O1 Sm1 95.7(2) . . ? O3 N1 O2 122.4(3) . . ? O3 N1 O1 121.7(4) . . ? O2 N1 O1 116.0(3) . . ? O9 N2 O5 122.0(3) . . ? O9 N2 O4 121.9(3) . . ? O5 N2 O4 116.1(3) . . ? C47 N5 C48 115.1(4) . . ? C47 N5 C11 112.0(3) . . ? C48 N5 C11 115.7(3) . . ? C14 N7 C6 125.4(3) . . ? C14 N7 H7 117.3 . . ? C6 N7 H7 117.3 . . ? C55 C5 C4 118.1(3) . . ? C55 C5 C6 121.3(3) . . ? C4 C5 C6 120.6(3) . . ? C2 C3 C4 120.5(4) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? C5 C4 C3 120.0(4) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? N7 C6 C5 111.5(3) . . ? N7 C6 H6A 109.3 . . ? C5 C6 H6A 109.3 . . ? N7 C6 H6B 109.3 . . ? C5 C6 H6B 109.3 . . ? H6A C6 H6B 108.0 . . ? C1 C2 C3 119.7(4) . . ? C1 C2 H2 120.2 . . ? C3 C2 H2 120.2 . . ? C2 C1 C55 120.4(4) . . ? C2 C1 H1 119.8 . . ? C55 C1 H1 119.8 . . ? C38 C9 C10 121.6(7) . . ? C38 C9 H9 119.2 . . ? C10 C9 H9 119.2 . . ? C9 C10 C8 116.1(5) . . ? C9 C10 C11 121.3(5) . . ? C8 C10 C11 122.6(4) . . ? N5 C11 C10 117.1(3) . . ? N5 C11 H11A 108.0 . . ? C10 C11 H11A 108.0 . . ? N5 C11 H11B 108.0 . . ? C10 C11 H11B 108.0 . . ? H11A C11 H11B 107.3 . . ? C10 C8 C36 122.2(6) . . ? C10 C8 H8A 118.9 . . ? C36 C8 H8A 118.9 . . ? C14 O11 Sm1 174.4(2) . . ? C30 O12 Sm1 134.0(3) . . ? O11 C14 N7 120.4(3) . . ? O11 C14 C15 119.6(3) . . ? N7 C14 C15 120.1(3) . . ? C16 C15 C41 118.0(3) . . ? C16 C15 C14 117.1(3) . . ? C41 C15 C14 124.9(3) . . ? C44 C16 C15 121.2(4) . . ? C44 C16 H16 119.4 . . ? C15 C16 H16 119.4 . . ? C30 N4 C56 122.9(4) . . ? C30 N4 C57 120.0(4) . . ? C56 N4 C57 117.1(4) . . ? O12 C30 N4 124.5(4) . . ? O12 C30 H30 117.8 . . ? N4 C30 H30 117.8 . . ? C37 C36 C8 119.6(7) . . ? C37 C36 H36 120.2 . . ? C8 C36 H36 120.2 . . ? C38 C37 C36 118.7(7) . . ? C38 C37 H37 120.6 . . ? C36 C37 H37 120.6 . . ? C37 C38 C9 121.7(7) . . ? C37 C38 H38 119.2 . . ? C9 C38 H38 119.2 . . ? O14 C41 C15 116.9(3) . . ? O14 C41 C42 123.9(4) . . ? C15 C41 C42 119.2(5) . . ? C44 C43 C42 120.0(5) . . ? C44 C43 H43 120.0 . . ? C42 C43 H43 120.0 . . ? C43 C42 C41 121.0(5) . . ? C43 C42 H42 119.5 . . ? C41 C42 H42 119.5 . . ? C43 C44 C16 120.6(5) . . ? C43 C44 H44 119.7 . . ? C16 C44 H44 119.7 . . ? C41 O14 C46 122.5(5) . . ? C47 C46 O14 118.0(4) . . ? C47 C46 H46A 107.8 . . ? O14 C46 H46A 107.8 . . ? C47 C46 H46B 107.8 . . ? O14 C46 H46B 107.8 . . ? H46A C46 H46B 107.1 . . ? C46 C47 N5 124.5(4) . . ? C46 C47 H47A 106.2 . . ? N5 C47 H47A 106.2 . . ? C46 C47 H47B 106.2 . . ? N5 C47 H47B 106.2 . . ? H47A C47 H47B 106.4 . . ? N5 C48 C54 110.4(3) . . ? N5 C48 H48A 109.6 . . ? C54 C48 H48A 109.6 . . ? N5 C48 H48B 109.6 . . ? C54 C48 H48B 109.6 . . ? H48A C48 H48B 108.1 . . ? O13 C54 C48 107.0(3) . . ? O13 C54 H54A 110.3 . . ? C48 C54 H54A 110.3 . . ? O13 C54 H54B 110.3 . . ? C48 C54 H54B 110.3 . . ? H54A C54 H54B 108.6 . . ? C1 C55 C5 121.4(4) . . ? C1 C55 H55 119.3 . . ? C5 C55 H55 119.3 . . ? N4 C56 H56A 109.5 . . ? N4 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? N4 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? N4 C57 H57A 109.5 . . ? N4 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? N4 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C59 C58 C17 121.3(3) . . ? C59 C58 H58 119.3 . . ? C17 C58 H58 119.3 . . ? C39 C59 C58 119.6(3) . . ? C39 C59 H59 120.2 . . ? C58 C59 H59 120.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C51 C50 C52 C22 -2.1(9) . . . . ? C52 C50 C51 C33 1.7(10) . . . . ? C50 C51 C33 C21 0.1(9) . . . . ? C50 C52 C22 C21 0.7(8) . . . . ? C52 C22 C21 C33 1.1(6) . . . . ? C52 C22 C21 C20 -175.4(4) . . . . ? C51 C33 C21 C22 -1.5(7) . . . . ? C51 C33 C21 C20 175.0(4) . . . . ? N6 C20 C21 C22 -57.2(5) . . . . ? N6 C20 C21 C33 126.3(4) . . . . ? C59 C39 C25 C24 0.4(5) . . . . ? O10 C18 C17 C58 13.8(4) . . . . ? N6 C18 C17 C58 -165.7(3) . . . . ? O10 C18 C17 C24 -164.9(3) . . . . ? N6 C18 C17 C24 15.7(5) . . . . ? O10 C18 N6 C20 6.8(5) . . . . ? C17 C18 N6 C20 -173.7(3) . . . . ? C21 C20 N6 C18 99.2(4) . . . . ? C54 O13 C24 C25 -4.1(5) . . . . ? C54 O13 C24 C17 174.6(3) . . . . ? C39 C25 C24 O13 178.5(3) . . . . ? C39 C25 C24 C17 -0.2(5) . . . . ? C58 C17 C24 O13 -178.8(3) . . . . ? C18 C17 C24 O13 -0.2(5) . . . . ? C58 C17 C24 C25 -0.1(5) . . . . ? C18 C17 C24 C25 178.5(3) . . . . ? N6 C18 O10 Sm1 -76(10) . . . 3_676 ? C17 C18 O10 Sm1 105(10) . . . 3_676 ? O8 N3 O6 Sm1 -175.3(3) . . . . ? O7 N3 O6 Sm1 4.8(3) . . . . ? O11 Sm1 O6 N3 -98.08(18) . . . . ? O10 Sm1 O6 N3 179.44(19) 3_676 . . . ? O12 Sm1 O6 N3 88.43(18) . . . . ? O7 Sm1 O6 N3 -2.80(16) . . . . ? O2 Sm1 O6 N3 -144.62(19) . . . . ? O5 Sm1 O6 N3 -29.1(2) . . . . ? O1 Sm1 O6 N3 127.16(18) . . . . ? O4 Sm1 O6 N3 28.5(2) . . . . ? O11 Sm1 O2 N1 -156.0(2) . . . . ? O10 Sm1 O2 N1 -74.3(2) 3_676 . . . ? O12 Sm1 O2 N1 5.5(2) . . . . ? O7 Sm1 O2 N1 133.8(2) . . . . ? O5 Sm1 O2 N1 126.0(2) . . . . ? O1 Sm1 O2 N1 4.05(19) . . . . ? O4 Sm1 O2 N1 76.5(2) . . . . ? O6 Sm1 O2 N1 -109.6(2) . . . . ? O8 N3 O7 Sm1 175.2(3) . . . . ? O6 N3 O7 Sm1 -4.9(3) . . . . ? O11 Sm1 O7 N3 81.73(18) . . . . ? O10 Sm1 O7 N3 5.5(2) 3_676 . . . ? O12 Sm1 O7 N3 -71.94(18) . . . . ? O2 Sm1 O7 N3 149.93(18) . . . . ? O5 Sm1 O7 N3 158.0(2) . . . . ? O1 Sm1 O7 N3 -112.3(2) . . . . ? O4 Sm1 O7 N3 -148.86(19) . . . . ? O6 Sm1 O7 N3 2.80(16) . . . . ? O11 Sm1 O5 N2 172.8(2) . . . . ? O10 Sm1 O5 N2 -147.9(2) 3_676 . . . ? O12 Sm1 O5 N2 17.6(2) . . . . ? O7 Sm1 O5 N2 80.4(2) . . . . ? O2 Sm1 O5 N2 -104.0(2) . . . . ? O1 Sm1 O5 N2 -61.0(2) . . . . ? O4 Sm1 O5 N2 -4.55(19) . . . . ? O6 Sm1 O5 N2 101.7(2) . . . . ? O11 Sm1 O4 N2 1.4(2) . . . . ? O10 Sm1 O4 N2 149.28(18) 3_676 . . . ? O12 Sm1 O4 N2 -156.2(2) . . . . ? O7 Sm1 O4 N2 -73.1(2) . . . . ? O2 Sm1 O4 N2 78.9(2) . . . . ? O5 Sm1 O4 N2 4.51(18) . . . . ? O1 Sm1 O4 N2 128.6(2) . . . . ? O6 Sm1 O4 N2 -97.8(2) . . . . ? O11 Sm1 O1 N1 21.2(3) . . . . ? O10 Sm1 O1 N1 86.0(2) 3_676 . . . ? O12 Sm1 O1 N1 177.2(2) . . . . ? O7 Sm1 O1 N1 -140.9(2) . . . . ? O2 Sm1 O1 N1 -4.04(19) . . . . ? O5 Sm1 O1 N1 -63.2(2) . . . . ? O4 Sm1 O1 N1 -104.8(2) . . . . ? O6 Sm1 O1 N1 138.7(2) . . . . ? Sm1 O2 N1 O3 172.0(3) . . . . ? Sm1 O2 N1 O1 -6.9(3) . . . . ? Sm1 O1 N1 O3 -172.1(3) . . . . ? Sm1 O1 N1 O2 6.9(3) . . . . ? Sm1 O5 N2 O9 -170.8(3) . . . . ? Sm1 O5 N2 O4 7.8(3) . . . . ? Sm1 O4 N2 O9 170.8(3) . . . . ? Sm1 O4 N2 O5 -7.7(3) . . . . ? C55 C5 C4 C3 -0.3(5) . . . . ? C6 C5 C4 C3 178.4(3) . . . . ? C2 C3 C4 C5 0.8(6) . . . . ? C14 N7 C6 C5 131.7(3) . . . . ? C55 C5 C6 N7 -64.3(4) . . . . ? C4 C5 C6 N7 116.9(4) . . . . ? C4 C3 C2 C1 -0.4(7) . . . . ? C3 C2 C1 C55 -0.5(7) . . . . ? C38 C9 C10 C8 0.5(8) . . . . ? C38 C9 C10 C11 179.8(5) . . . . ? C47 N5 C11 C10 -54.8(5) . . . . ? C48 N5 C11 C10 79.9(5) . . . . ? C9 C10 C11 N5 114.4(5) . . . . ? C8 C10 C11 N5 -66.3(6) . . . . ? C9 C10 C8 C36 -1.2(8) . . . . ? C11 C10 C8 C36 179.4(5) . . . . ? O10 Sm1 O11 C14 -24(2) 3_676 . . . ? O12 Sm1 O11 C14 -89(2) . . . . ? O7 Sm1 O11 C14 -152(2) . . . . ? O2 Sm1 O11 C14 58(2) . . . . ? O5 Sm1 O11 C14 137(2) . . . . ? O1 Sm1 O11 C14 38(2) . . . . ? O4 Sm1 O11 C14 140(2) . . . . ? O6 Sm1 O11 C14 -102(2) . . . . ? O11 Sm1 O12 C30 -173.8(3) . . . . ? O10 Sm1 O12 C30 122.7(4) 3_676 . . . ? O7 Sm1 O12 C30 -108.6(4) . . . . ? O2 Sm1 O12 C30 46.1(4) . . . . ? O5 Sm1 O12 C30 -50.1(4) . . . . ? O1 Sm1 O12 C30 47.2(4) . . . . ? O4 Sm1 O12 C30 -32.6(3) . . . . ? O6 Sm1 O12 C30 -160.6(4) . . . . ? Sm1 O11 C14 N7 -101(2) . . . . ? Sm1 O11 C14 C15 78(2) . . . . ? C6 N7 C14 O11 -2.8(5) . . . . ? C6 N7 C14 C15 178.0(3) . . . . ? O11 C14 C15 C16 -9.7(4) . . . . ? N7 C14 C15 C16 169.5(3) . . . . ? O11 C14 C15 C41 169.4(3) . . . . ? N7 C14 C15 C41 -11.4(5) . . . . ? C41 C15 C16 C44 0.5(5) . . . . ? C14 C15 C16 C44 179.7(3) . . . . ? Sm1 O12 C30 N4 176.0(3) . . . . ? C56 N4 C30 O12 -0.4(6) . . . . ? C57 N4 C30 O12 -178.0(5) . . . . ? C10 C8 C36 C37 2.6(9) . . . . ? C8 C36 C37 C38 -3.2(11) . . . . ? C36 C37 C38 C9 2.6(13) . . . . ? C10 C9 C38 C37 -1.2(11) . . . . ? C16 C15 C41 O14 178.8(3) . . . . ? C14 C15 C41 O14 -0.3(5) . . . . ? C16 C15 C41 C42 -0.1(5) . . . . ? C14 C15 C41 C42 -179.2(3) . . . . ? C44 C43 C42 C41 0.0(8) . . . . ? O14 C41 C42 C43 -178.9(4) . . . . ? C15 C41 C42 C43 -0.1(6) . . . . ? C42 C43 C44 C16 0.4(7) . . . . ? C15 C16 C44 C43 -0.6(6) . . . . ? C15 C41 O14 C46 165.7(4) . . . . ? C42 C41 O14 C46 -15.4(6) . . . . ? C41 O14 C46 C47 -106.9(7) . . . . ? O14 C46 C47 N5 -4.3(12) . . . . ? C48 N5 C47 C46 110.9(7) . . . . ? C11 N5 C47 C46 -114.2(7) . . . . ? C47 N5 C48 C54 -84.8(4) . . . . ? C11 N5 C48 C54 141.9(3) . . . . ? C24 O13 C54 C48 -168.5(3) . . . . ? N5 C48 C54 O13 -177.7(3) . . . . ? C2 C1 C55 C5 1.0(7) . . . . ? C4 C5 C55 C1 -0.6(6) . . . . ? C6 C5 C55 C1 -179.3(4) . . . . ? C24 C17 C58 C59 0.1(5) . . . . ? C18 C17 C58 C59 -178.6(3) . . . . ? C25 C39 C59 C58 -0.4(5) . . . . ? C17 C58 C59 C39 0.1(5) . . . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 27.57 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 0.785 _refine_diff_density_min -0.775 _refine_diff_density_rms 0.072 #===END data_666993 _database_code_depnum_ccdc_archive 'CCDC 666993' #TrackingRef '- cif_Revision.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84 H92 Eu2 N14 O28' _chemical_formula_weight 2049.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.6144(3) _cell_length_b 14.0677(2) _cell_length_c 19.7534(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.0960(10) _cell_angle_gamma 90.00 _cell_volume 4514.39(12) _cell_formula_units_Z 2 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 5350 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 22.19 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.508 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2088 _exptl_absorpt_coefficient_mu 1.462 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6935 _exptl_absorpt_correction_T_max 0.9046 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27499 _diffrn_reflns_av_R_equivalents 0.0483 _diffrn_reflns_av_sigmaI/netI 0.0625 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 27.56 _reflns_number_total 10188 _reflns_number_gt 6675 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Standard DFIX restraint was used for the distance of the disordered atoms C35 and C10. #============================================================================== The Following Model and Quality ALERTS were generated - (Acta-Mode) <<< #============================================================================== Format: alert-number_ALERT_alert-type_alert-level text PLAT241_ALERT_2_A Check High Ueq as Compared to Neighbors for C35 The larger than normal range of thermal motion is mostly due to the difference between the disordered ethyl group and the other atoms which are not disordered. ; _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^)+(0.0339P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10188 _refine_ls_number_parameters 595 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0798 _refine_ls_R_factor_gt 0.0417 _refine_ls_wR_factor_ref 0.0881 _refine_ls_wR_factor_gt 0.0759 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3872(2) 1.0324(3) 0.40527(18) 0.0390(9) Uani 1 1 d . . . C2 C 0.4500(2) 1.0651(3) 0.3745(2) 0.0464(10) Uani 1 1 d . . . C3 C 0.5221(3) 1.0146(3) 0.3795(2) 0.0540(11) Uani 1 1 d . . . C4 C 0.5322(3) 0.9289(3) 0.4143(2) 0.0527(11) Uani 1 1 d . . . C5 C 0.4709(2) 0.8942(3) 0.4446(2) 0.0470(10) Uani 1 1 d . . . H5 H 0.4782 0.8366 0.4681 0.056 Uiso 1 1 calc R . . C6 C 0.3982(2) 0.9446(3) 0.4402(2) 0.0431(9) Uani 1 1 d . . . C7 C 0.3116(2) 1.0910(3) 0.39608(19) 0.0415(9) Uani 1 1 d . . . C8 C 0.3420(3) 0.8199(3) 0.4996(2) 0.0580(12) Uani 1 1 d . . . H8A H 0.3826 0.8203 0.5427 0.070 Uiso 1 1 calc R . . H8B H 0.3587 0.7738 0.4687 0.070 Uiso 1 1 calc R . . C9 C 0.2579(3) 0.7945(3) 0.5128(2) 0.0626(13) Uani 1 1 d . . . H9A H 0.2404 0.8429 0.5415 0.075 Uiso 1 1 calc R . . H9B H 0.2182 0.7923 0.4691 0.075 Uiso 1 1 calc R . . C10 C 0.2506(3) 0.6233(4) 0.5013(3) 0.108(2) Uani 1 1 d D . . H10A H 0.2053 0.5866 0.5117 0.129 Uiso 1 1 calc R . . H10B H 0.2318 0.6486 0.4550 0.129 Uiso 1 1 calc R . . C11 C 0.3411(3) 0.6694(3) 0.7788(2) 0.0582(11) Uani 1 1 d . . . H11 H 0.3410 0.6047 0.7884 0.070 Uiso 1 1 calc R . . C12 C 0.2800(3) 0.7272(4) 0.7944(3) 0.0768(15) Uani 1 1 d . . . H12 H 0.2393 0.7010 0.8146 0.092 Uiso 1 1 calc R . . C13 C 0.2788(3) 0.8221(5) 0.7803(3) 0.0770(15) Uani 1 1 d . . . H13 H 0.2375 0.8606 0.7906 0.092 Uiso 1 1 calc R . . C14 C 0.3388(4) 0.8597(4) 0.7511(3) 0.0807(15) Uani 1 1 d . . . H14 H 0.3385 0.9244 0.7414 0.097 Uiso 1 1 calc R . . C15 C 0.4000(3) 0.8027(4) 0.7358(3) 0.0711(14) Uani 1 1 d . . . H15 H 0.4407 0.8296 0.7159 0.085 Uiso 1 1 calc R . . C16 C 0.4020(2) 0.7073(3) 0.7491(2) 0.0494(11) Uani 1 1 d . . . C17 C 0.1201(4) 0.6790(4) 0.5744(3) 0.0832(17) Uani 1 1 d . . . C18 C 0.2107(3) 0.6961(4) 0.5993(3) 0.0803(16) Uani 1 1 d . . . H18A H 0.2175 0.7545 0.6260 0.096 Uiso 1 1 calc R . . H18B H 0.2327 0.6450 0.6307 0.096 Uiso 1 1 calc R . . C19 C 0.0686(4) 0.7437(5) 0.5364(4) 0.107(2) Uani 1 1 d . . . H19 H 0.0905 0.8014 0.5258 0.129 Uiso 1 1 calc R . . C20 C 0.0845(5) 0.5955(5) 0.5905(4) 0.126(3) Uani 1 1 d . . . H20 H 0.1172 0.5496 0.6168 0.151 Uiso 1 1 calc R . . C21 C 0.1111(4) 1.0237(4) 0.3249(3) 0.0862(17) Uani 1 1 d . . . H21 H 0.1566 1.0360 0.3058 0.103 Uiso 1 1 calc R . . C22 C 0.1092(3) 1.0578(3) 0.3903(3) 0.0613(12) Uani 1 1 d . . . C23 C 0.0426(3) 1.0352(4) 0.4176(3) 0.0979(19) Uani 1 1 d . . . H23 H 0.0413 1.0553 0.4622 0.117 Uiso 1 1 calc R . . C24 C 0.0458(5) 0.9711(4) 0.2874(4) 0.119(2) Uani 1 1 d . . . H24 H 0.0471 0.9483 0.2435 0.143 Uiso 1 1 calc R . . C25 C 0.1774(2) 1.1199(3) 0.4283(2) 0.0556(11) Uani 1 1 d . . . H25A H 0.1775 1.1793 0.4034 0.067 Uiso 1 1 calc R . . H25B H 0.1673 1.1344 0.4739 0.067 Uiso 1 1 calc R . . C26 C 0.0000(6) 0.5791(7) 0.5678(5) 0.154(4) Uani 1 1 d . . . H26 H -0.0227 0.5219 0.5783 0.185 Uiso 1 1 calc R . . C27 C -0.0483(6) 0.6457(8) 0.5308(6) 0.154(4) Uani 1 1 d . . . H27 H -0.1047 0.6354 0.5178 0.184 Uiso 1 1 calc R . . C28 C -0.0159(5) 0.7275(6) 0.5123(4) 0.131(3) Uani 1 1 d . . . H28 H -0.0488 0.7718 0.4844 0.157 Uiso 1 1 calc R . . C29 C -0.0228(4) 0.9833(6) 0.3809(5) 0.131(3) Uani 1 1 d . . . H29 H -0.0676 0.9694 0.4005 0.157 Uiso 1 1 calc R . . C30 C -0.0213(5) 0.9535(5) 0.3173(5) 0.136(3) Uani 1 1 d . . . H30 H -0.0662 0.9201 0.2923 0.163 Uiso 1 1 calc R . . C31 C 0.0781(3) 1.2180(4) 0.2121(3) 0.0817(16) Uani 1 1 d . . . H31 H 0.0912 1.2044 0.1696 0.098 Uiso 1 1 calc R . . C32 C 0.5310(2) 0.6536(3) 0.6305(2) 0.0432(9) Uani 1 1 d . . . C33 C 0.5208(3) 0.6441(3) 0.5540(2) 0.0503(11) Uani 1 1 d . . . C34 C 0.5866(4) 0.6733(4) 0.5254(3) 0.0637(13) Uani 1 1 d . . . C35 C 0.3086(3) 0.5627(5) 0.4974(4) 0.174(4) Uani 1 1 d D . . H35A H 0.3134 0.5590 0.4494 0.209 Uiso 1 1 calc R . . H35B H 0.2909 0.5007 0.5101 0.209 Uiso 1 1 calc R . . C36 C 0.4696(3) 0.6451(3) 0.7332(2) 0.0639(13) Uani 1 1 d . . . H36A H 0.5225 0.6694 0.7573 0.077 Uiso 1 1 calc R . . H36B H 0.4635 0.5812 0.7498 0.077 Uiso 1 1 calc R . . C37 C 0.5839(4) 0.6681(4) 0.4554(3) 0.0920(19) Uani 1 1 d . . . H37 H 0.6283 0.6887 0.4374 0.110 Uiso 1 1 calc R . . C38 C 0.4507(3) 0.6090(3) 0.5093(3) 0.0690(15) Uani 1 1 d . . . C39 C 0.4487(4) 0.6037(4) 0.4380(3) 0.104(2) Uani 1 1 d . . . H39 H 0.4022 0.5807 0.4079 0.124 Uiso 1 1 calc R . . C40 C 0.5155(5) 0.6326(5) 0.4132(3) 0.112(3) Uani 1 1 d . . . H40 H 0.5140 0.6278 0.3660 0.134 Uiso 1 1 calc R . . C41 C -0.0289(4) 1.2261(4) 0.2794(3) 0.112(2) Uani 1 1 d . . . H41A H 0.0160 1.2479 0.3149 0.168 Uiso 1 1 calc R . . H41B H -0.0505 1.1681 0.2942 0.168 Uiso 1 1 calc R . . H41C H -0.0713 1.2735 0.2711 0.168 Uiso 1 1 calc R . . C42 C -0.0608(4) 1.1826(6) 0.1560(3) 0.147(3) Uani 1 1 d . . . H42A H -0.0334 1.1646 0.1198 0.220 Uiso 1 1 calc R . . H42B H -0.0965 1.2356 0.1410 0.220 Uiso 1 1 calc R . . H42C H -0.0927 1.1300 0.1668 0.220 Uiso 1 1 calc R . . N7 N -0.0001(2) 1.2091(3) 0.2172(2) 0.0728(12) Uani 1 1 d . . . Eu1 Eu 0.274569(11) 1.275193(14) 0.268680(10) 0.03985(7) Uani 1 1 d . . . N1 N 0.2063(2) 1.4262(3) 0.3413(2) 0.0557(9) Uani 1 1 d . . . N2 N 0.2612(2) 1.3870(3) 0.1417(2) 0.0618(10) Uani 1 1 d . . . N3 N 0.3171(3) 1.1088(3) 0.1960(2) 0.0682(11) Uani 1 1 d . . . N4 N 0.2608(2) 0.7031(2) 0.54692(18) 0.0531(9) Uani 1 1 d . . . N5 N 0.25806(19) 1.0745(2) 0.43589(17) 0.0522(9) Uani 1 1 d . . . H5A H 0.2718 1.0338 0.4688 0.063 Uiso 1 1 calc R . . N6 N 0.4680(2) 0.6419(3) 0.65915(18) 0.0608(10) Uani 1 1 d . . . H6 H 0.4212 0.6313 0.6320 0.073 Uiso 1 1 calc R . . O1 O 0.22797(17) 1.3484(2) 0.37091(15) 0.0610(8) Uani 1 1 d . . . O2 O 0.22071(19) 1.4368(2) 0.28130(17) 0.0648(8) Uani 1 1 d . . . O3 O 0.1728(2) 1.4882(2) 0.36817(18) 0.0867(11) Uani 1 1 d . . . O4 O 0.32608(17) 1.3870(2) 0.18856(15) 0.0606(8) Uani 1 1 d . . . O5 O 0.20662(19) 1.3270(3) 0.14905(15) 0.0700(9) Uani 1 1 d . . . O6 O 0.2440(2) 1.1233(2) 0.20211(18) 0.0775(10) Uani 1 1 d . . . O7 O 0.36861(19) 1.1742(2) 0.21746(15) 0.0633(8) Uani 1 1 d . . . O8 O 0.3367(3) 1.0350(3) 0.1719(2) 0.1034(13) Uani 1 1 d . . . O9 O 0.29878(16) 1.1563(2) 0.35196(14) 0.0544(7) Uani 1 1 d . . . O10 O 0.60070(15) 0.6734(2) 0.66707(13) 0.0519(7) Uani 1 1 d . . . O11 O 0.13311(18) 1.2423(2) 0.25894(17) 0.0633(9) Uani 1 1 d . . . O12 O 0.2518(2) 1.4418(3) 0.09271(18) 0.0951(12) Uani 1 1 d . . . O13 O 0.33537(16) 0.91225(19) 0.46879(15) 0.0560(8) Uani 1 1 d . . . O14 O 0.3884(2) 0.5801(3) 0.5383(2) 0.0960(13) Uani 1 1 d . . . H2 H 0.4444(19) 1.126(2) 0.3523(16) 0.036(10) Uiso 1 1 d . . . H3 H 0.565(2) 1.041(2) 0.3595(17) 0.041(10) Uiso 1 1 d . . . H4 H 0.579(2) 0.894(3) 0.4140(19) 0.058(13) Uiso 1 1 d . . . H34 H 0.631(2) 0.695(2) 0.5527(18) 0.033(11) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.037(2) 0.042(2) 0.038(2) 0.0017(17) 0.0056(17) 0.0040(17) C2 0.046(3) 0.047(3) 0.047(2) 0.010(2) 0.0122(19) 0.004(2) C3 0.043(3) 0.068(3) 0.055(3) 0.008(2) 0.020(2) 0.004(2) C4 0.040(3) 0.063(3) 0.056(3) 0.000(2) 0.012(2) 0.011(2) C5 0.047(3) 0.044(2) 0.049(3) 0.0071(19) 0.007(2) 0.010(2) C6 0.040(2) 0.042(2) 0.047(2) -0.0012(18) 0.0107(18) 0.0035(19) C7 0.042(2) 0.039(2) 0.042(2) -0.0030(18) 0.0061(18) 0.0019(18) C8 0.051(3) 0.047(3) 0.076(3) 0.015(2) 0.013(2) 0.001(2) C9 0.054(3) 0.063(3) 0.075(3) 0.016(2) 0.023(2) 0.004(2) C10 0.052(3) 0.095(4) 0.163(6) -0.074(4) -0.010(3) 0.002(3) C11 0.053(3) 0.066(3) 0.057(3) 0.010(2) 0.016(2) 0.001(2) C12 0.067(4) 0.102(4) 0.069(3) 0.005(3) 0.030(3) -0.004(3) C13 0.065(4) 0.093(4) 0.072(4) -0.012(3) 0.011(3) 0.017(3) C14 0.094(4) 0.059(3) 0.085(4) -0.002(3) 0.009(3) 0.002(3) C15 0.071(4) 0.072(4) 0.071(3) 0.005(3) 0.018(3) -0.010(3) C16 0.038(2) 0.069(3) 0.039(2) 0.004(2) 0.0017(17) -0.003(2) C17 0.094(5) 0.086(4) 0.084(4) -0.015(3) 0.049(4) -0.030(4) C18 0.097(4) 0.084(4) 0.064(3) 0.006(3) 0.026(3) -0.029(3) C19 0.087(5) 0.118(6) 0.131(6) -0.021(4) 0.056(4) -0.017(4) C20 0.119(6) 0.114(6) 0.164(7) -0.013(5) 0.071(5) -0.049(5) C21 0.087(4) 0.062(4) 0.106(5) -0.002(3) 0.012(4) -0.008(3) C22 0.047(3) 0.054(3) 0.082(4) 0.015(3) 0.012(3) 0.002(2) C23 0.069(4) 0.095(5) 0.134(5) 0.002(4) 0.032(4) -0.021(3) C24 0.130(7) 0.086(5) 0.124(6) -0.015(4) -0.011(5) -0.024(5) C25 0.039(3) 0.057(3) 0.072(3) 0.009(2) 0.014(2) 0.013(2) C26 0.136(9) 0.129(8) 0.224(11) -0.051(7) 0.100(8) -0.069(6) C27 0.105(8) 0.159(10) 0.223(12) -0.084(8) 0.093(8) -0.050(7) C28 0.077(5) 0.151(7) 0.177(8) -0.039(6) 0.057(5) 0.001(5) C29 0.078(5) 0.124(7) 0.191(9) -0.005(6) 0.027(6) -0.044(4) C30 0.090(6) 0.082(5) 0.208(10) 0.012(6) -0.030(6) -0.026(4) C31 0.061(4) 0.079(4) 0.108(5) 0.012(3) 0.024(3) 0.001(3) C32 0.039(2) 0.038(2) 0.050(3) 0.0020(18) 0.002(2) 0.0055(18) C33 0.057(3) 0.046(3) 0.041(2) -0.0009(19) -0.005(2) 0.023(2) C34 0.079(4) 0.058(3) 0.051(3) 0.002(2) 0.007(3) 0.017(3) C35 0.058(4) 0.181(7) 0.239(9) -0.157(7) -0.071(5) 0.041(4) C36 0.043(3) 0.089(4) 0.059(3) 0.011(3) 0.008(2) 0.001(2) C37 0.143(6) 0.082(4) 0.057(4) 0.006(3) 0.036(4) 0.039(4) C38 0.071(4) 0.055(3) 0.066(3) -0.021(2) -0.021(3) 0.037(3) C39 0.127(6) 0.081(4) 0.073(5) -0.032(3) -0.049(4) 0.056(4) C40 0.175(8) 0.095(5) 0.054(4) -0.011(3) -0.002(5) 0.071(5) C41 0.111(5) 0.134(6) 0.102(5) 0.021(4) 0.048(4) 0.033(4) C42 0.102(6) 0.192(8) 0.136(6) -0.047(6) 0.003(5) -0.048(5) N7 0.036(2) 0.074(3) 0.104(3) 0.004(2) 0.006(2) -0.011(2) Eu1 0.03070(11) 0.04360(12) 0.04505(12) 0.00338(10) 0.00751(8) 0.00167(10) N1 0.042(2) 0.053(2) 0.071(3) -0.016(2) 0.0077(19) 0.0005(18) N2 0.056(3) 0.081(3) 0.050(2) 0.011(2) 0.014(2) 0.008(2) N3 0.087(4) 0.061(3) 0.061(3) -0.007(2) 0.025(2) 0.007(3) N4 0.059(2) 0.043(2) 0.058(2) -0.0050(17) 0.0142(18) -0.0071(17) N5 0.040(2) 0.060(2) 0.060(2) 0.0167(18) 0.0173(17) 0.0129(17) N6 0.032(2) 0.097(3) 0.051(2) -0.008(2) 0.0027(16) -0.0037(19) O1 0.057(2) 0.067(2) 0.061(2) 0.0052(16) 0.0177(15) 0.0118(16) O2 0.075(2) 0.0508(19) 0.071(2) 0.0040(16) 0.0202(18) 0.0053(16) O3 0.089(3) 0.075(2) 0.097(3) -0.032(2) 0.021(2) 0.021(2) O4 0.0397(18) 0.083(2) 0.0569(19) 0.0183(16) 0.0058(15) -0.0022(15) O5 0.058(2) 0.094(3) 0.054(2) 0.0077(18) 0.0011(15) -0.0156(19) O6 0.065(2) 0.067(2) 0.099(3) -0.0267(19) 0.013(2) -0.0061(18) O7 0.061(2) 0.069(2) 0.066(2) -0.0086(17) 0.0269(16) 0.0015(18) O8 0.137(4) 0.069(3) 0.116(3) -0.026(2) 0.053(3) 0.015(2) O9 0.0483(18) 0.0522(18) 0.0643(19) 0.0187(15) 0.0157(14) 0.0106(14) O10 0.0343(16) 0.076(2) 0.0434(16) 0.0006(14) 0.0032(12) -0.0073(14) O11 0.0343(17) 0.074(2) 0.077(2) 0.0064(17) -0.0001(15) -0.0049(15) O12 0.091(3) 0.128(3) 0.063(2) 0.044(2) 0.0105(19) 0.002(2) O13 0.0478(18) 0.0469(17) 0.079(2) 0.0201(15) 0.0261(15) 0.0090(14) O14 0.044(2) 0.120(3) 0.107(3) -0.058(2) -0.022(2) 0.012(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.391(5) . ? C1 C6 1.409(5) . ? C1 C7 1.481(5) . ? C2 C3 1.379(5) . ? C2 H2 0.96(3) . ? C3 C4 1.380(6) . ? C3 H3 0.95(3) . ? C4 C5 1.374(5) . ? C4 H4 0.92(4) . ? C5 C6 1.387(5) . ? C5 H5 0.9300 . ? C6 O13 1.365(4) . ? C7 O9 1.253(4) . ? C7 N5 1.326(4) . ? C8 O13 1.429(4) . ? C8 C9 1.516(5) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 N4 1.448(5) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C35 1.301(6) . ? C10 N4 1.427(5) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C16 1.379(5) . ? C11 C12 1.385(6) . ? C11 H11 0.9300 . ? C12 C13 1.363(7) . ? C12 H12 0.9300 . ? C13 C14 1.359(6) . ? C13 H13 0.9300 . ? C14 C15 1.378(6) . ? C14 H14 0.9300 . ? C15 C16 1.368(6) . ? C15 H15 0.9300 . ? C16 C36 1.508(5) . ? C17 C19 1.362(8) . ? C17 C20 1.382(7) . ? C17 C18 1.502(7) . ? C18 N4 1.462(5) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C28 1.404(9) . ? C19 H19 0.9300 . ? C20 C26 1.400(10) . ? C20 H20 0.9300 . ? C21 C22 1.385(7) . ? C21 C24 1.391(8) . ? C21 H21 0.9300 . ? C22 C23 1.366(6) . ? C22 C25 1.501(6) . ? C23 C29 1.382(8) . ? C23 H23 0.9300 . ? C24 C30 1.389(9) . ? C24 H24 0.9300 . ? C25 N5 1.464(4) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C27 1.346(12) . ? C26 H26 0.9300 . ? C27 C28 1.352(10) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? C29 C30 1.329(9) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 O11 1.206(6) . ? C31 N7 1.330(6) . ? C31 H31 0.9300 . ? C32 O10 1.261(4) . ? C32 N6 1.301(5) . ? C32 C33 1.490(5) . ? C33 C34 1.393(6) . ? C33 C38 1.396(6) . ? C34 C37 1.375(6) . ? C34 H34 0.87(3) . ? C35 O14 1.422(5) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 N6 1.457(5) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 C40 1.357(9) . ? C37 H37 0.9300 . ? C38 O14 1.347(6) . ? C38 C39 1.404(7) . ? C39 C40 1.366(9) . ? C39 H39 0.9300 . ? C40 H40 0.9300 . ? C41 N7 1.430(6) . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 N7 1.451(7) . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? Eu1 O10 2.308(3) 3_676 ? Eu1 O9 2.321(3) . ? Eu1 O11 2.363(3) . ? Eu1 O2 2.475(3) . ? Eu1 O7 2.479(3) . ? Eu1 O6 2.504(3) . ? Eu1 O5 2.505(3) . ? Eu1 O4 2.506(3) . ? Eu1 O1 2.529(3) . ? N1 O3 1.215(4) . ? N1 O1 1.257(4) . ? N1 O2 1.266(4) . ? N2 O12 1.221(4) . ? N2 O4 1.265(4) . ? N2 O5 1.269(4) . ? N3 O8 1.215(4) . ? N3 O6 1.263(5) . ? N3 O7 1.267(5) . ? N5 H5A 0.8600 . ? N6 H6 0.8600 . ? O10 Eu1 2.308(3) 3_676 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 118.1(3) . . ? C2 C1 C7 117.2(4) . . ? C6 C1 C7 124.6(3) . . ? C3 C2 C1 121.3(4) . . ? C3 C2 H2 119.5(19) . . ? C1 C2 H2 119.0(19) . . ? C2 C3 C4 119.8(4) . . ? C2 C3 H3 119(2) . . ? C4 C3 H3 121(2) . . ? C5 C4 C3 120.3(4) . . ? C5 C4 H4 121(2) . . ? C3 C4 H4 119(2) . . ? C4 C5 C6 120.4(4) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? O13 C6 C5 122.4(4) . . ? O13 C6 C1 117.6(3) . . ? C5 C6 C1 120.0(3) . . ? O9 C7 N5 120.3(4) . . ? O9 C7 C1 120.6(3) . . ? N5 C7 C1 119.1(4) . . ? O13 C8 C9 107.2(3) . . ? O13 C8 H8A 110.3 . . ? C9 C8 H8A 110.3 . . ? O13 C8 H8B 110.3 . . ? C9 C8 H8B 110.3 . . ? H8A C8 H8B 108.5 . . ? N4 C9 C8 110.4(3) . . ? N4 C9 H9A 109.6 . . ? C8 C9 H9A 109.6 . . ? N4 C9 H9B 109.6 . . ? C8 C9 H9B 109.6 . . ? H9A C9 H9B 108.1 . . ? C35 C10 N4 124.2(5) . . ? C35 C10 H10A 106.3 . . ? N4 C10 H10A 106.3 . . ? C35 C10 H10B 106.3 . . ? N4 C10 H10B 106.3 . . ? H10A C10 H10B 106.4 . . ? C16 C11 C12 120.4(5) . . ? C16 C11 H11 119.8 . . ? C12 C11 H11 119.8 . . ? C13 C12 C11 120.6(5) . . ? C13 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C14 C13 C12 119.2(5) . . ? C14 C13 H13 120.4 . . ? C12 C13 H13 120.4 . . ? C13 C14 C15 120.5(5) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C16 C15 C14 121.2(5) . . ? C16 C15 H15 119.4 . . ? C14 C15 H15 119.4 . . ? C15 C16 C11 118.1(4) . . ? C15 C16 C36 121.2(4) . . ? C11 C16 C36 120.7(4) . . ? C19 C17 C20 116.4(7) . . ? C19 C17 C18 123.0(6) . . ? C20 C17 C18 120.6(7) . . ? N4 C18 C17 117.3(4) . . ? N4 C18 H18A 108.0 . . ? C17 C18 H18A 108.0 . . ? N4 C18 H18B 108.0 . . ? C17 C18 H18B 108.0 . . ? H18A C18 H18B 107.2 . . ? C17 C19 C28 123.1(7) . . ? C17 C19 H19 118.5 . . ? C28 C19 H19 118.5 . . ? C17 C20 C26 121.1(8) . . ? C17 C20 H20 119.5 . . ? C26 C20 H20 119.5 . . ? C22 C21 C24 120.9(6) . . ? C22 C21 H21 119.6 . . ? C24 C21 H21 119.6 . . ? C23 C22 C21 117.7(5) . . ? C23 C22 C25 121.8(5) . . ? C21 C22 C25 120.5(4) . . ? C22 C23 C29 122.0(7) . . ? C22 C23 H23 119.0 . . ? C29 C23 H23 119.0 . . ? C30 C24 C21 118.4(7) . . ? C30 C24 H24 120.8 . . ? C21 C24 H24 120.8 . . ? N5 C25 C22 112.1(3) . . ? N5 C25 H25A 109.2 . . ? C22 C25 H25A 109.2 . . ? N5 C25 H25B 109.2 . . ? C22 C25 H25B 109.2 . . ? H25A C25 H25B 107.9 . . ? C27 C26 C20 120.1(9) . . ? C27 C26 H26 119.9 . . ? C20 C26 H26 119.9 . . ? C26 C27 C28 120.9(10) . . ? C26 C27 H27 119.5 . . ? C28 C27 H27 119.5 . . ? C27 C28 C19 118.3(9) . . ? C27 C28 H28 120.9 . . ? C19 C28 H28 120.9 . . ? C30 C29 C23 119.6(8) . . ? C30 C29 H29 120.2 . . ? C23 C29 H29 120.2 . . ? C29 C30 C24 121.3(8) . . ? C29 C30 H30 119.3 . . ? C24 C30 H30 119.3 . . ? O11 C31 N7 124.3(5) . . ? O11 C31 H31 117.8 . . ? N7 C31 H31 117.8 . . ? O10 C32 N6 120.3(4) . . ? O10 C32 C33 119.8(4) . . ? N6 C32 C33 119.9(4) . . ? C34 C33 C38 117.9(5) . . ? C34 C33 C32 116.9(4) . . ? C38 C33 C32 125.1(4) . . ? C37 C34 C33 122.0(6) . . ? C37 C34 H34 119(3) . . ? C33 C34 H34 119(2) . . ? C10 C35 O14 117.9(5) . . ? C10 C35 H35A 107.8 . . ? O14 C35 H35A 107.8 . . ? C10 C35 H35B 107.8 . . ? O14 C35 H35B 107.8 . . ? H35A C35 H35B 107.2 . . ? N6 C36 C16 111.7(3) . . ? N6 C36 H36A 109.3 . . ? C16 C36 H36A 109.3 . . ? N6 C36 H36B 109.3 . . ? C16 C36 H36B 109.3 . . ? H36A C36 H36B 107.9 . . ? C40 C37 C34 118.9(6) . . ? C40 C37 H37 120.5 . . ? C34 C37 H37 120.5 . . ? O14 C38 C33 116.8(5) . . ? O14 C38 C39 123.5(5) . . ? C33 C38 C39 119.7(6) . . ? C40 C39 C38 119.7(6) . . ? C40 C39 H39 120.2 . . ? C38 C39 H39 120.2 . . ? C37 C40 C39 121.8(6) . . ? C37 C40 H40 119.1 . . ? C39 C40 H40 119.1 . . ? N7 C41 H41A 109.5 . . ? N7 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? N7 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? N7 C42 H42A 109.5 . . ? N7 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? N7 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C31 N7 C41 123.9(5) . . ? C31 N7 C42 118.7(5) . . ? C41 N7 C42 117.4(5) . . ? O10 Eu1 O9 80.41(10) 3_676 . ? O10 Eu1 O11 150.36(10) 3_676 . ? O9 Eu1 O11 86.47(10) . . ? O10 Eu1 O2 87.65(10) 3_676 . ? O9 Eu1 O2 127.09(10) . . ? O11 Eu1 O2 79.25(10) . . ? O10 Eu1 O7 80.43(10) 3_676 . ? O9 Eu1 O7 81.14(10) . . ? O11 Eu1 O7 123.76(11) . . ? O2 Eu1 O7 147.11(10) . . ? O10 Eu1 O6 128.01(11) 3_676 . ? O9 Eu1 O6 75.14(11) . . ? O11 Eu1 O6 72.64(11) . . ? O2 Eu1 O6 143.01(11) . . ? O7 Eu1 O6 51.14(11) . . ? O10 Eu1 O5 127.09(10) 3_676 . ? O9 Eu1 O5 148.82(11) . . ? O11 Eu1 O5 74.71(11) . . ? O2 Eu1 O5 74.13(11) . . ? O7 Eu1 O5 88.85(11) . . ? O6 Eu1 O5 75.60(11) . . ? O10 Eu1 O4 76.39(9) 3_676 . ? O9 Eu1 O4 150.29(9) . . ? O11 Eu1 O4 122.47(10) . . ? O2 Eu1 O4 70.46(10) . . ? O7 Eu1 O4 76.95(10) . . ? O6 Eu1 O4 105.21(11) . . ? O5 Eu1 O4 50.75(10) . . ? O10 Eu1 O1 79.81(9) 3_676 . ? O9 Eu1 O1 76.35(10) . . ? O11 Eu1 O1 71.27(10) . . ? O2 Eu1 O1 50.78(10) . . ? O7 Eu1 O1 152.13(10) . . ? O6 Eu1 O1 134.79(11) . . ? O5 Eu1 O1 118.81(10) . . ? O4 Eu1 O1 116.80(10) . . ? O3 N1 O1 122.3(4) . . ? O3 N1 O2 121.2(4) . . ? O1 N1 O2 116.5(3) . . ? O12 N2 O4 121.8(4) . . ? O12 N2 O5 122.3(4) . . ? O4 N2 O5 115.9(4) . . ? O8 N3 O6 121.2(5) . . ? O8 N3 O7 122.3(5) . . ? O6 N3 O7 116.5(4) . . ? C10 N4 C9 114.6(4) . . ? C10 N4 C18 112.6(4) . . ? C9 N4 C18 114.9(4) . . ? C7 N5 C25 125.2(3) . . ? C7 N5 H5A 117.4 . . ? C25 N5 H5A 117.4 . . ? C32 N6 C36 125.8(4) . . ? C32 N6 H6 117.1 . . ? C36 N6 H6 117.1 . . ? N1 O1 Eu1 95.1(2) . . ? N1 O2 Eu1 97.4(2) . . ? N2 O4 Eu1 96.3(2) . . ? N2 O5 Eu1 96.3(2) . . ? N3 O6 Eu1 95.5(3) . . ? N3 O7 Eu1 96.5(3) . . ? C7 O9 Eu1 179.0(3) . . ? C32 O10 Eu1 174.5(3) . 3_676 ? C31 O11 Eu1 134.3(4) . . ? C6 O13 C8 118.8(3) . . ? C38 O14 C35 121.3(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -1.8(6) . . . . ? C7 C1 C2 C3 -179.1(4) . . . . ? C1 C2 C3 C4 1.4(7) . . . . ? C2 C3 C4 C5 -0.6(7) . . . . ? C3 C4 C5 C6 0.4(6) . . . . ? C4 C5 C6 O13 179.2(4) . . . . ? C4 C5 C6 C1 -0.8(6) . . . . ? C2 C1 C6 O13 -178.5(3) . . . . ? C7 C1 C6 O13 -1.4(6) . . . . ? C2 C1 C6 C5 1.5(6) . . . . ? C7 C1 C6 C5 178.6(3) . . . . ? C2 C1 C7 O9 13.3(5) . . . . ? C6 C1 C7 O9 -163.8(4) . . . . ? C2 C1 C7 N5 -165.7(4) . . . . ? C6 C1 C7 N5 17.2(6) . . . . ? O13 C8 C9 N4 -177.5(4) . . . . ? C16 C11 C12 C13 0.3(8) . . . . ? C11 C12 C13 C14 -0.4(8) . . . . ? C12 C13 C14 C15 0.1(8) . . . . ? C13 C14 C15 C16 0.2(8) . . . . ? C14 C15 C16 C11 -0.3(7) . . . . ? C14 C15 C16 C36 -179.2(5) . . . . ? C12 C11 C16 C15 0.0(6) . . . . ? C12 C11 C16 C36 178.9(4) . . . . ? C19 C17 C18 N4 -66.2(7) . . . . ? C20 C17 C18 N4 114.9(6) . . . . ? C20 C17 C19 C28 -1.8(10) . . . . ? C18 C17 C19 C28 179.3(5) . . . . ? C19 C17 C20 C26 0.7(10) . . . . ? C18 C17 C20 C26 179.7(6) . . . . ? C24 C21 C22 C23 2.4(8) . . . . ? C24 C21 C22 C25 -175.9(5) . . . . ? C21 C22 C23 C29 -2.6(9) . . . . ? C25 C22 C23 C29 175.6(6) . . . . ? C22 C21 C24 C30 -0.2(10) . . . . ? C23 C22 C25 N5 125.7(5) . . . . ? C21 C22 C25 N5 -56.0(6) . . . . ? C17 C20 C26 C27 -1.3(13) . . . . ? C20 C26 C27 C28 3.0(16) . . . . ? C26 C27 C28 C19 -3.9(14) . . . . ? C17 C19 C28 C27 3.4(11) . . . . ? C22 C23 C29 C30 0.6(12) . . . . ? C23 C29 C30 C24 1.8(13) . . . . ? C21 C24 C30 C29 -2.0(12) . . . . ? O10 C32 C33 C34 -10.3(5) . . . . ? N6 C32 C33 C34 169.3(4) . . . . ? O10 C32 C33 C38 170.0(4) . . . . ? N6 C32 C33 C38 -10.4(6) . . . . ? C38 C33 C34 C37 0.0(7) . . . . ? C32 C33 C34 C37 -179.8(4) . . . . ? N4 C10 C35 O14 -3.9(13) . . . . ? C15 C16 C36 N6 -64.0(5) . . . . ? C11 C16 C36 N6 117.1(4) . . . . ? C33 C34 C37 C40 -0.7(8) . . . . ? C34 C33 C38 O14 179.1(4) . . . . ? C32 C33 C38 O14 -1.2(6) . . . . ? C34 C33 C38 C39 0.2(6) . . . . ? C32 C33 C38 C39 179.9(4) . . . . ? O14 C38 C39 C40 -178.5(5) . . . . ? C33 C38 C39 C40 0.3(8) . . . . ? C34 C37 C40 C39 1.4(9) . . . . ? C38 C39 C40 C37 -1.2(9) . . . . ? O11 C31 N7 C41 -1.1(8) . . . . ? O11 C31 N7 C42 177.7(6) . . . . ? C35 C10 N4 C9 111.3(8) . . . . ? C35 C10 N4 C18 -114.8(8) . . . . ? C8 C9 N4 C10 -84.9(5) . . . . ? C8 C9 N4 C18 142.3(4) . . . . ? C17 C18 N4 C10 -53.5(6) . . . . ? C17 C18 N4 C9 80.2(6) . . . . ? O9 C7 N5 C25 7.3(6) . . . . ? C1 C7 N5 C25 -173.7(4) . . . . ? C22 C25 N5 C7 99.0(5) . . . . ? O10 C32 N6 C36 -3.0(6) . . . . ? C33 C32 N6 C36 177.3(4) . . . . ? C16 C36 N6 C32 132.0(4) . . . . ? O3 N1 O1 Eu1 175.1(4) . . . . ? O2 N1 O1 Eu1 -4.4(4) . . . . ? O10 Eu1 O1 N1 97.9(2) 3_676 . . . ? O9 Eu1 O1 N1 -179.6(2) . . . . ? O11 Eu1 O1 N1 -88.7(2) . . . . ? O2 Eu1 O1 N1 2.6(2) . . . . ? O7 Eu1 O1 N1 143.4(3) . . . . ? O6 Eu1 O1 N1 -127.4(2) . . . . ? O5 Eu1 O1 N1 -29.0(3) . . . . ? O4 Eu1 O1 N1 29.0(3) . . . . ? O3 N1 O2 Eu1 -175.0(3) . . . . ? O1 N1 O2 Eu1 4.5(4) . . . . ? O10 Eu1 O2 N1 -81.4(2) 3_676 . . . ? O9 Eu1 O2 N1 -5.3(3) . . . . ? O11 Eu1 O2 N1 71.9(2) . . . . ? O7 Eu1 O2 N1 -149.7(2) . . . . ? O6 Eu1 O2 N1 112.7(3) . . . . ? O5 Eu1 O2 N1 148.9(2) . . . . ? O4 Eu1 O2 N1 -157.8(2) . . . . ? O1 Eu1 O2 N1 -2.6(2) . . . . ? O12 N2 O4 Eu1 171.2(4) . . . . ? O5 N2 O4 Eu1 -8.5(4) . . . . ? O10 Eu1 O4 N2 -172.5(3) 3_676 . . . ? O9 Eu1 O4 N2 147.9(2) . . . . ? O11 Eu1 O4 N2 -17.6(3) . . . . ? O2 Eu1 O4 N2 -80.1(3) . . . . ? O7 Eu1 O4 N2 104.4(3) . . . . ? O6 Eu1 O4 N2 61.3(3) . . . . ? O5 Eu1 O4 N2 5.0(2) . . . . ? O1 Eu1 O4 N2 -101.5(3) . . . . ? O12 N2 O5 Eu1 -171.2(4) . . . . ? O4 N2 O5 Eu1 8.5(4) . . . . ? O10 Eu1 O5 N2 -1.9(3) 3_676 . . . ? O9 Eu1 O5 N2 -149.7(2) . . . . ? O11 Eu1 O5 N2 155.4(3) . . . . ? O2 Eu1 O5 N2 72.5(3) . . . . ? O7 Eu1 O5 N2 -79.0(3) . . . . ? O6 Eu1 O5 N2 -129.0(3) . . . . ? O4 Eu1 O5 N2 -5.0(2) . . . . ? O1 Eu1 O5 N2 97.4(3) . . . . ? O8 N3 O6 Eu1 172.5(4) . . . . ? O7 N3 O6 Eu1 -6.1(4) . . . . ? O10 Eu1 O6 N3 -22.2(3) 3_676 . . . ? O9 Eu1 O6 N3 -87.0(3) . . . . ? O11 Eu1 O6 N3 -177.9(3) . . . . ? O2 Eu1 O6 N3 139.8(2) . . . . ? O7 Eu1 O6 N3 3.6(2) . . . . ? O5 Eu1 O6 N3 103.9(3) . . . . ? O4 Eu1 O6 N3 62.3(3) . . . . ? O1 Eu1 O6 N3 -139.5(2) . . . . ? O8 N3 O7 Eu1 -172.4(4) . . . . ? O6 N3 O7 Eu1 6.2(4) . . . . ? O10 Eu1 O7 N3 156.1(3) 3_676 . . . ? O9 Eu1 O7 N3 74.4(3) . . . . ? O11 Eu1 O7 N3 -5.2(3) . . . . ? O2 Eu1 O7 N3 -133.6(3) . . . . ? O6 Eu1 O7 N3 -3.6(2) . . . . ? O5 Eu1 O7 N3 -75.9(3) . . . . ? O4 Eu1 O7 N3 -125.8(3) . . . . ? O1 Eu1 O7 N3 110.7(3) . . . . ? N5 C7 O9 Eu1 -109(14) . . . . ? C1 C7 O9 Eu1 72(14) . . . . ? O10 Eu1 O9 C7 -130(14) 3_676 . . . ? O11 Eu1 O9 C7 77(14) . . . . ? O2 Eu1 O9 C7 151(14) . . . . ? O7 Eu1 O9 C7 -48(14) . . . . ? O6 Eu1 O9 C7 4(14) . . . . ? O5 Eu1 O9 C7 25(14) . . . . ? O4 Eu1 O9 C7 -91(14) . . . . ? O1 Eu1 O9 C7 148(14) . . . . ? N6 C32 O10 Eu1 -97(3) . . . 3_676 ? C33 C32 O10 Eu1 83(3) . . . 3_676 ? N7 C31 O11 Eu1 -175.4(3) . . . . ? O10 Eu1 O11 C31 175.0(4) 3_676 . . . ? O9 Eu1 O11 C31 -121.5(5) . . . . ? O2 Eu1 O11 C31 109.7(5) . . . . ? O7 Eu1 O11 C31 -44.6(5) . . . . ? O6 Eu1 O11 C31 -46.0(5) . . . . ? O5 Eu1 O11 C31 33.4(5) . . . . ? O4 Eu1 O11 C31 51.3(5) . . . . ? O1 Eu1 O11 C31 161.7(5) . . . . ? C5 C6 O13 C8 -5.0(6) . . . . ? C1 C6 O13 C8 175.0(4) . . . . ? C9 C8 O13 C6 -168.1(3) . . . . ? C33 C38 O14 C35 166.2(4) . . . . ? C39 C38 O14 C35 -14.9(7) . . . . ? C10 C35 O14 C38 -107.6(8) . . . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.652 _refine_diff_density_min -0.481 _refine_diff_density_rms 0.080 #===END data_666994 _database_code_depnum_ccdc_archive 'CCDC 666994' #TrackingRef '- cif_Revision.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84 H92 N14 O28 Tb2' _chemical_formula_weight 2063.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.5638(2) _cell_length_b 14.0683(2) _cell_length_c 19.7449(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.2270(10) _cell_angle_gamma 90.00 _cell_volume 4496.68(11) _cell_formula_units_Z 2 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.524 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2096 _exptl_absorpt_coefficient_mu 1.646 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6209 _exptl_absorpt_correction_T_max 0.9222 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26591 _diffrn_reflns_av_R_equivalents 0.0398 _diffrn_reflns_av_sigmaI/netI 0.0511 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 27.11 _reflns_number_total 9804 _reflns_number_gt 6890 _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 Following Model and Quality ALERTS were generated - (Acta-Mode) <<< #============================================================================== Format: alert-number_ALERT_alert-type_alert-level text PLAT241_ALERT_2_A Check High Ueq as Compared to Neighbors for C14 The larger than normal range of thermal motion is mostly due to the difference between the disordered ethyl group and the other atoms which are not disordered. ; _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^)+(0.0315P)^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 9804 _refine_ls_number_parameters 579 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0638 _refine_ls_R_factor_gt 0.0374 _refine_ls_wR_factor_ref 0.0821 _refine_ls_wR_factor_gt 0.0724 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.0794(3) 0.7173(3) 0.7133(3) 0.0747(14) Uani 1 1 d . . . H1 H 0.0927 0.7037 0.6709 0.090 Uiso 1 1 calc R . . C2 C 0.5315(2) 0.1544(3) 1.13103(18) 0.0428(9) Uani 1 1 d . . . C3 C 0.5207(2) 0.1449(3) 1.05455(18) 0.0487(10) Uani 1 1 d . . . C4 C 0.3114(2) 0.5917(3) 0.89559(17) 0.0397(8) Uani 1 1 d . . . C5 C 0.3875(2) 0.5321(3) 0.90466(16) 0.0385(8) Uani 1 1 d . . . C6 C 0.4509(2) 0.5653(3) 0.87433(17) 0.0443(9) Uani 1 1 d . . . H6 H 0.4444 0.6225 0.8502 0.053 Uiso 1 1 calc R . . C7 C 0.3981(2) 0.4445(3) 0.94020(17) 0.0416(9) Uani 1 1 d . . . C8 C 0.4712(2) 0.3940(3) 0.94429(19) 0.0486(10) Uani 1 1 d . . . H8 H 0.4785 0.3360 0.9675 0.058 Uiso 1 1 calc R . . C9 C 0.5326(2) 0.4290(3) 0.91439(19) 0.0533(10) Uani 1 1 d . . . H9 H 0.5812 0.3946 0.9177 0.064 Uiso 1 1 calc R . . C10 C 0.5232(2) 0.5145(3) 0.87949(19) 0.0541(11) Uani 1 1 d . . . H10 H 0.5653 0.5378 0.8596 0.065 Uiso 1 1 calc R . . C11 C 0.3413(2) 0.3197(3) 0.9992(2) 0.0577(11) Uani 1 1 d . . . H11A H 0.3821 0.3199 1.0424 0.069 Uiso 1 1 calc R . . H11B H 0.3578 0.2733 0.9684 0.069 Uiso 1 1 calc R . . C12 C 0.2571(3) 0.2953(3) 1.0122(2) 0.0647(12) Uani 1 1 d . . . H12A H 0.2401 0.3437 1.0413 0.078 Uiso 1 1 calc R . . H12B H 0.2171 0.2938 0.9686 0.078 Uiso 1 1 calc R . . C13 C 0.2504(3) 0.1237(4) 0.9992(3) 0.108(2) Uani 1 1 d . . . H13A H 0.2014 0.0899 1.0053 0.130 Uiso 1 1 calc R . . H13B H 0.2376 0.1499 0.9527 0.130 Uiso 1 1 calc R . . C14 C 0.3061(3) 0.0609(5) 0.9996(4) 0.179(4) Uani 1 1 d . . . H14A H 0.3103 0.0499 0.9520 0.214 Uiso 1 1 calc R . . H14B H 0.2870 0.0021 1.0166 0.214 Uiso 1 1 calc R . . C15 C 0.1771(2) 0.6208(3) 0.9277(2) 0.0558(11) Uani 1 1 d . . . H15A H 0.1770 0.6799 0.9024 0.067 Uiso 1 1 calc R . . H15B H 0.1672 0.6358 0.9732 0.067 Uiso 1 1 calc R . . C16 C 0.1087(2) 0.5573(3) 0.8898(2) 0.0607(11) Uani 1 1 d . . . C17 C 0.1103(3) 0.5233(4) 0.8249(3) 0.0829(15) Uani 1 1 d . . . H17 H 0.1558 0.5357 0.8057 0.099 Uiso 1 1 calc R . . C18 C 0.0418(3) 0.5360(4) 0.9177(3) 0.0938(17) Uani 1 1 d . . . H18 H 0.0402 0.5565 0.9622 0.113 Uiso 1 1 calc R . . C19 C 0.0453(4) 0.4708(4) 0.7879(4) 0.118(2) Uani 1 1 d . . . H19 H 0.0471 0.4475 0.7441 0.141 Uiso 1 1 calc R . . C20 C 0.4695(2) 0.1470(3) 1.23375(19) 0.0640(12) Uani 1 1 d . . . H20A H 0.5223 0.1721 1.2580 0.077 Uiso 1 1 calc R . . H20B H 0.4639 0.0832 1.2509 0.077 Uiso 1 1 calc R . . C21 C 0.4011(2) 0.2084(3) 1.24910(18) 0.0476(10) Uani 1 1 d . . . C22 C 0.3994(3) 0.3045(4) 1.2357(2) 0.0688(13) Uani 1 1 d . . . H22 H 0.4406 0.3314 1.2165 0.083 Uiso 1 1 calc R . . C23 C 0.3396(2) 0.1697(3) 1.27846(19) 0.0578(11) Uani 1 1 d . . . H23 H 0.3396 0.1049 1.2881 0.069 Uiso 1 1 calc R . . C24 C -0.0231(4) 0.4844(5) 0.8799(4) 0.125(3) Uani 1 1 d . . . H24 H -0.0684 0.4709 0.8992 0.150 Uiso 1 1 calc R . . C25 C -0.0221(4) 0.4534(5) 0.8164(5) 0.132(3) Uani 1 1 d . . . H25 H -0.0670 0.4200 0.7912 0.158 Uiso 1 1 calc R . . C26 C 0.3376(3) 0.3615(4) 1.2504(2) 0.0796(14) Uani 1 1 d . . . H26 H 0.3370 0.4262 1.2405 0.096 Uiso 1 1 calc R . . C27 C 0.2780(3) 0.2276(4) 1.2935(2) 0.0750(14) Uani 1 1 d . . . H27 H 0.2370 0.2014 1.3133 0.090 Uiso 1 1 calc R . . C28 C 0.2769(3) 0.3227(5) 1.2794(2) 0.0745(14) Uani 1 1 d . . . H28 H 0.2352 0.3610 1.2895 0.089 Uiso 1 1 calc R . . C29 C -0.0618(3) 0.6824(5) 0.6566(3) 0.139(3) Uani 1 1 d . . . H29A H -0.0358 0.6687 0.6187 0.209 Uiso 1 1 calc R . . H29B H -0.0996 0.7344 0.6444 0.209 Uiso 1 1 calc R . . H29C H -0.0913 0.6273 0.6668 0.209 Uiso 1 1 calc R . . C30 C -0.0273(3) 0.7269(4) 0.7811(3) 0.0991(18) Uani 1 1 d . . . H30A H 0.0172 0.7528 0.8153 0.149 Uiso 1 1 calc R . . H30B H -0.0459 0.6687 0.7981 0.149 Uiso 1 1 calc R . . H30C H -0.0721 0.7716 0.7718 0.149 Uiso 1 1 calc R . . C31 C 0.0670(4) 0.2433(5) 1.0344(3) 0.103(2) Uani 1 1 d . . . H31 H 0.0892 0.3003 1.0229 0.123 Uiso 1 1 calc R . . C32 C 0.0824(4) 0.0954(5) 1.0895(3) 0.119(2) Uani 1 1 d . . . H32 H 0.1148 0.0489 1.1157 0.143 Uiso 1 1 calc R . . C33 C 0.1186(4) 0.1781(4) 1.0735(3) 0.0825(15) Uani 1 1 d . . . C34 C 0.2100(3) 0.1958(4) 1.0983(2) 0.0799(15) Uani 1 1 d . . . H34A H 0.2168 0.2540 1.1253 0.096 Uiso 1 1 calc R . . H34B H 0.2325 0.1444 1.1294 0.096 Uiso 1 1 calc R . . C35 C -0.0170(4) 0.2272(6) 1.0115(4) 0.130(3) Uani 1 1 d . . . H35 H -0.0502 0.2720 0.9842 0.156 Uiso 1 1 calc R . . C36 C -0.0502(5) 0.1454(8) 1.0295(5) 0.153(4) Uani 1 1 d . . . H36 H -0.1067 0.1344 1.0155 0.183 Uiso 1 1 calc R . . C37 C -0.0015(6) 0.0806(7) 1.0672(5) 0.159(4) Uani 1 1 d . . . H37 H -0.0246 0.0242 1.0788 0.191 Uiso 1 1 calc R . . C38 C 0.4497(3) 0.1085(3) 1.0102(2) 0.0702(14) Uani 1 1 d . . . C39 C 0.4488(4) 0.1027(4) 0.9396(3) 0.100(2) Uani 1 1 d . . . H39 H 0.4024 0.0778 0.9100 0.121 Uiso 1 1 calc R . . C40 C 0.5127(5) 0.1319(5) 0.9125(3) 0.116(3) Uani 1 1 d . . . H40 H 0.5096 0.1282 0.8650 0.139 Uiso 1 1 calc R . . C41 C 0.5826(4) 0.1671(4) 0.9554(2) 0.0948(19) Uani 1 1 d . . . H41 H 0.6272 0.1866 0.9370 0.114 Uiso 1 1 calc R . . C42 C 0.5865(3) 0.1735(3) 1.0259(2) 0.0663(12) Uani 1 1 d . . . H42 H 0.6340 0.1974 1.0546 0.080 Uiso 1 1 calc R . . Tb1 Tb 0.275185(9) 0.774215(13) 0.769023(8) 0.03930(7) Uani 1 1 d . . . N1 N 0.3175(3) 0.6088(3) 0.69676(18) 0.0649(10) Uani 1 1 d . . . N2 N 0.2619(2) 0.8838(3) 0.64211(17) 0.0599(9) Uani 1 1 d . . . N3 N 0.20810(19) 0.9248(3) 0.84037(19) 0.0552(9) Uani 1 1 d . . . N4 N 0.0012(2) 0.7081(3) 0.7176(2) 0.0720(11) Uani 1 1 d . . . N5 N 0.25780(17) 0.5753(2) 0.93529(15) 0.0505(8) Uani 1 1 d . . . H5 H 0.2716 0.5345 0.9682 0.061 Uiso 1 1 calc R . . N6 N 0.25956(19) 0.2037(2) 1.04587(16) 0.0519(8) Uani 1 1 d . . . N7 N 0.46814(17) 0.1428(3) 1.15970(16) 0.0590(9) Uani 1 1 d . . . H7 H 0.4213 0.1316 1.1325 0.071 Uiso 1 1 calc R . . O1 O 0.36864(17) 0.6757(2) 0.71834(14) 0.0619(7) Uani 1 1 d . . . O2 O 0.24393(18) 0.6232(2) 0.70330(16) 0.0748(9) Uani 1 1 d . . . O3 O 0.3372(2) 0.5352(2) 0.67241(18) 0.0984(12) Uani 1 1 d . . . O4 O 0.32678(15) 0.8849(2) 0.68943(13) 0.0609(8) Uani 1 1 d . . . O5 O 0.20703(17) 0.8238(2) 0.65015(13) 0.0669(8) Uani 1 1 d . . . O6 O 0.22954(16) 0.8476(2) 0.87095(13) 0.0598(7) Uani 1 1 d . . . O7 O 0.22229(17) 0.9343(2) 0.78052(15) 0.0619(7) Uani 1 1 d . . . O8 O 0.17417(19) 0.9868(2) 0.86726(16) 0.0829(10) Uani 1 1 d . . . O9 O 0.60097(14) 0.1746(2) 1.16723(11) 0.0512(7) Uani 1 1 d . . . O11 O 0.29936(14) 0.65664(19) 0.85152(13) 0.0539(7) Uani 1 1 d . . . O12 O 0.13487(16) 0.7421(2) 0.76013(15) 0.0605(8) Uani 1 1 d . . . O13 O 0.25269(19) 0.9372(3) 0.59301(15) 0.0944(12) Uani 1 1 d . . . O14 O 0.33520(15) 0.41249(19) 0.96809(13) 0.0550(7) Uani 1 1 d . . . O15 O 0.38804(18) 0.0795(3) 1.03948(17) 0.0937(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.053(3) 0.079(4) 0.095(4) 0.011(3) 0.022(3) -0.002(3) C2 0.036(2) 0.040(2) 0.048(2) 0.0021(17) 0.0002(17) 0.0064(17) C3 0.055(2) 0.044(2) 0.041(2) -0.0021(18) -0.0018(18) 0.020(2) C4 0.0378(19) 0.042(2) 0.039(2) 0.0001(17) 0.0070(16) 0.0006(17) C5 0.0388(19) 0.042(2) 0.0345(18) 0.0004(16) 0.0066(15) 0.0042(17) C6 0.045(2) 0.046(2) 0.041(2) 0.0065(17) 0.0069(16) 0.0012(18) C7 0.0376(19) 0.044(2) 0.043(2) -0.0010(17) 0.0081(16) 0.0013(18) C8 0.045(2) 0.043(2) 0.057(2) 0.0061(19) 0.0086(18) 0.0069(19) C9 0.040(2) 0.064(3) 0.057(2) -0.001(2) 0.0129(18) 0.010(2) C10 0.043(2) 0.069(3) 0.054(2) 0.010(2) 0.0194(18) 0.009(2) C11 0.054(2) 0.045(3) 0.074(3) 0.018(2) 0.015(2) 0.002(2) C12 0.054(2) 0.070(3) 0.073(3) 0.016(2) 0.019(2) 0.006(2) C13 0.047(3) 0.097(4) 0.163(5) -0.084(4) -0.017(3) 0.009(3) C14 0.057(3) 0.167(7) 0.261(8) -0.162(6) -0.081(4) 0.049(4) C15 0.041(2) 0.058(3) 0.070(3) 0.010(2) 0.0156(19) 0.011(2) C16 0.044(2) 0.060(3) 0.078(3) 0.013(2) 0.012(2) -0.001(2) C17 0.076(3) 0.068(4) 0.100(4) -0.002(3) 0.008(3) -0.010(3) C18 0.062(3) 0.096(4) 0.127(5) 0.008(4) 0.029(3) -0.016(3) C19 0.112(5) 0.090(5) 0.135(6) -0.010(4) -0.012(5) -0.017(4) C20 0.044(2) 0.095(4) 0.054(3) 0.007(2) 0.0112(19) 0.005(2) C21 0.037(2) 0.064(3) 0.040(2) 0.0051(18) 0.0046(16) -0.0023(19) C22 0.066(3) 0.066(3) 0.076(3) 0.012(3) 0.018(2) -0.009(3) C23 0.049(2) 0.070(3) 0.056(2) 0.012(2) 0.0147(19) -0.003(2) C24 0.075(4) 0.112(6) 0.183(8) 0.009(5) 0.020(5) -0.039(4) C25 0.091(5) 0.086(5) 0.190(8) 0.000(5) -0.033(6) -0.028(4) C26 0.092(4) 0.059(3) 0.086(4) -0.002(3) 0.014(3) 0.007(3) C27 0.059(3) 0.106(5) 0.065(3) 0.002(3) 0.024(2) -0.006(3) C28 0.066(3) 0.093(4) 0.065(3) -0.017(3) 0.016(2) 0.014(3) C29 0.084(4) 0.209(8) 0.114(5) -0.026(5) -0.004(4) -0.050(5) C30 0.083(4) 0.124(5) 0.099(4) 0.008(4) 0.039(3) 0.021(4) C31 0.079(4) 0.115(6) 0.127(5) -0.017(4) 0.052(4) -0.024(4) C32 0.133(6) 0.092(5) 0.154(6) -0.012(4) 0.077(5) -0.046(4) C33 0.095(4) 0.089(4) 0.075(3) -0.018(3) 0.043(3) -0.032(4) C34 0.098(4) 0.081(4) 0.064(3) 0.007(3) 0.022(3) -0.031(3) C35 0.077(4) 0.154(7) 0.172(7) -0.043(6) 0.057(4) -0.005(5) C36 0.089(6) 0.165(10) 0.223(11) -0.093(8) 0.078(6) -0.042(6) C37 0.134(8) 0.133(8) 0.242(11) -0.067(7) 0.107(8) -0.077(6) C38 0.074(3) 0.059(3) 0.061(3) -0.019(2) -0.021(2) 0.038(3) C39 0.135(6) 0.084(4) 0.059(4) -0.027(3) -0.032(3) 0.059(4) C40 0.201(8) 0.097(5) 0.039(3) -0.006(3) 0.001(4) 0.078(5) C41 0.157(6) 0.082(4) 0.052(3) 0.013(3) 0.037(3) 0.050(4) C42 0.085(3) 0.061(3) 0.051(3) 0.008(2) 0.011(2) 0.024(3) Tb1 0.03025(9) 0.04363(12) 0.04362(11) 0.00343(9) 0.00692(7) 0.00154(9) N1 0.081(3) 0.061(3) 0.056(2) -0.0035(19) 0.022(2) 0.009(2) N2 0.053(2) 0.082(3) 0.048(2) 0.009(2) 0.0176(18) 0.005(2) N3 0.0428(19) 0.051(2) 0.068(2) -0.009(2) 0.0047(17) 0.0037(17) N4 0.0372(19) 0.080(3) 0.095(3) 0.003(2) 0.0039(19) -0.0094(19) N5 0.0425(17) 0.055(2) 0.0555(19) 0.0148(16) 0.0144(15) 0.0121(16) N6 0.056(2) 0.044(2) 0.057(2) 0.0010(16) 0.0141(16) -0.0053(16) N7 0.0300(16) 0.089(3) 0.054(2) -0.0137(18) -0.0001(14) -0.0035(17) O1 0.0602(18) 0.065(2) 0.0658(18) -0.0068(16) 0.0261(14) 0.0005(17) O2 0.0618(19) 0.066(2) 0.095(2) -0.0222(18) 0.0122(17) -0.0022(17) O3 0.129(3) 0.064(2) 0.112(3) -0.026(2) 0.050(2) 0.015(2) O4 0.0416(15) 0.085(2) 0.0554(17) 0.0191(15) 0.0081(13) 0.0007(15) O5 0.0544(17) 0.090(2) 0.0511(17) 0.0067(16) 0.0005(13) -0.0161(17) O6 0.0591(17) 0.064(2) 0.0594(17) 0.0026(15) 0.0186(14) 0.0116(16) O7 0.0723(19) 0.0508(19) 0.0647(19) 0.0046(14) 0.0191(15) 0.0026(15) O8 0.084(2) 0.071(2) 0.095(2) -0.0255(19) 0.0218(19) 0.0174(19) O9 0.0354(13) 0.075(2) 0.0408(14) 0.0019(13) 0.0033(11) -0.0074(14) O11 0.0465(15) 0.0517(18) 0.0655(17) 0.0204(14) 0.0159(13) 0.0110(13) O12 0.0332(14) 0.072(2) 0.0732(19) 0.0012(15) 0.0036(14) -0.0076(14) O13 0.089(2) 0.133(3) 0.060(2) 0.049(2) 0.0123(17) 0.002(2) O14 0.0460(15) 0.0475(17) 0.0766(18) 0.0207(14) 0.0243(13) 0.0079(13) O15 0.0450(17) 0.116(3) 0.103(3) -0.056(2) -0.0219(18) 0.0154(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O12 1.209(5) . ? C1 N4 1.321(5) . ? C1 H1 0.9300 . ? C2 O9 1.252(4) . ? C2 N7 1.304(4) . ? C2 C3 1.489(5) . ? C3 C42 1.390(5) . ? C3 C38 1.406(6) . ? C4 O11 1.249(4) . ? C4 N5 1.324(4) . ? C4 C5 1.492(4) . ? C5 C6 1.396(4) . ? C5 C7 1.411(5) . ? C6 C10 1.378(5) . ? C6 H6 0.9300 . ? C7 O14 1.355(4) . ? C7 C8 1.392(5) . ? C8 C9 1.371(5) . ? C8 H8 0.9300 . ? C9 C10 1.379(5) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 O14 1.437(4) . ? C11 C12 1.511(5) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 N6 1.446(5) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.276(6) . ? C13 N6 1.441(5) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 O15 1.442(5) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 N5 1.461(4) . ? C15 C16 1.511(6) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C18 1.371(6) . ? C16 C17 1.372(6) . ? C17 C19 1.381(7) . ? C17 H17 0.9300 . ? C18 C24 1.378(8) . ? C18 H18 0.9300 . ? C19 C25 1.373(9) . ? C19 H19 0.9300 . ? C20 N7 1.459(4) . ? C20 C21 1.505(5) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.377(6) . ? C21 C23 1.386(5) . ? C22 C26 1.379(6) . ? C22 H22 0.9300 . ? C23 C27 1.386(6) . ? C23 H23 0.9300 . ? C24 C25 1.332(9) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 C28 1.372(6) . ? C26 H26 0.9300 . ? C27 C28 1.366(7) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? C29 N4 1.462(6) . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 N4 1.454(6) . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 C33 1.373(8) . ? C31 C35 1.389(8) . ? C31 H31 0.9300 . ? C32 C33 1.376(7) . ? C32 C37 1.382(9) . ? C32 H32 0.9300 . ? C33 C34 1.510(7) . ? C34 N6 1.456(5) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.354(10) . ? C35 H35 0.9300 . ? C36 C37 1.335(11) . ? C36 H36 0.9300 . ? C37 H37 0.9300 . ? C38 O15 1.340(6) . ? C38 C39 1.394(6) . ? C39 C40 1.347(8) . ? C39 H39 0.9300 . ? C40 C41 1.374(8) . ? C40 H40 0.9300 . ? C41 C42 1.382(6) . ? C41 H41 0.9300 . ? C42 H42 0.9300 . ? Tb1 O9 2.284(2) 3_667 ? Tb1 O11 2.296(2) . ? Tb1 O12 2.338(3) . ? Tb1 O7 2.444(3) . ? Tb1 O1 2.444(3) . ? Tb1 O5 2.480(3) . ? Tb1 O2 2.486(3) . ? Tb1 O4 2.489(3) . ? Tb1 O6 2.516(3) . ? N1 O3 1.215(4) . ? N1 O2 1.268(4) . ? N1 O1 1.279(4) . ? N2 O13 1.211(4) . ? N2 O4 1.266(4) . ? N2 O5 1.274(4) . ? N3 O8 1.219(4) . ? N3 O6 1.257(4) . ? N3 O7 1.260(4) . ? N5 H5 0.8600 . ? N7 H7 0.8600 . ? O9 Tb1 2.284(2) 3_667 ? 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 O12 C1 N4 125.1(5) . . ? O12 C1 H1 117.4 . . ? N4 C1 H1 117.4 . . ? O9 C2 N7 120.5(3) . . ? O9 C2 C3 119.9(3) . . ? N7 C2 C3 119.6(3) . . ? C42 C3 C38 118.4(4) . . ? C42 C3 C2 116.8(4) . . ? C38 C3 C2 124.7(4) . . ? O11 C4 N5 120.8(3) . . ? O11 C4 C5 120.1(3) . . ? N5 C4 C5 119.1(3) . . ? C6 C5 C7 118.6(3) . . ? C6 C5 C4 117.0(3) . . ? C7 C5 C4 124.3(3) . . ? C10 C6 C5 121.1(3) . . ? C10 C6 H6 119.5 . . ? C5 C6 H6 119.5 . . ? O14 C7 C8 122.8(3) . . ? O14 C7 C5 117.8(3) . . ? C8 C7 C5 119.4(3) . . ? C9 C8 C7 120.5(4) . . ? C9 C8 H8 119.8 . . ? C7 C8 H8 119.8 . . ? C8 C9 C10 120.9(4) . . ? C8 C9 H9 119.6 . . ? C10 C9 H9 119.6 . . ? C6 C10 C9 119.6(4) . . ? C6 C10 H10 120.2 . . ? C9 C10 H10 120.2 . . ? O14 C11 C12 107.1(3) . . ? O14 C11 H11A 110.3 . . ? C12 C11 H11A 110.3 . . ? O14 C11 H11B 110.3 . . ? C12 C11 H11B 110.3 . . ? H11A C11 H11B 108.5 . . ? N6 C12 C11 110.1(3) . . ? N6 C12 H12A 109.6 . . ? C11 C12 H12A 109.6 . . ? N6 C12 H12B 109.6 . . ? C11 C12 H12B 109.6 . . ? H12A C12 H12B 108.2 . . ? C14 C13 N6 124.0(4) . . ? C14 C13 H13A 106.3 . . ? N6 C13 H13A 106.3 . . ? C14 C13 H13B 106.3 . . ? N6 C13 H13B 106.3 . . ? H13A C13 H13B 106.4 . . ? C13 C14 O15 118.3(5) . . ? C13 C14 H14A 107.7 . . ? O15 C14 H14A 107.7 . . ? C13 C14 H14B 107.7 . . ? O15 C14 H14B 107.7 . . ? H14A C14 H14B 107.1 . . ? N5 C15 C16 111.4(3) . . ? N5 C15 H15A 109.3 . . ? C16 C15 H15A 109.3 . . ? N5 C15 H15B 109.3 . . ? C16 C15 H15B 109.3 . . ? H15A C15 H15B 108.0 . . ? C18 C16 C17 118.4(5) . . ? C18 C16 C15 121.0(5) . . ? C17 C16 C15 120.6(4) . . ? C16 C17 C19 120.9(5) . . ? C16 C17 H17 119.5 . . ? C19 C17 H17 119.5 . . ? C16 C18 C24 120.1(6) . . ? C16 C18 H18 119.9 . . ? C24 C18 H18 119.9 . . ? C25 C19 C17 119.2(7) . . ? C25 C19 H19 120.4 . . ? C17 C19 H19 120.4 . . ? N7 C20 C21 111.9(3) . . ? N7 C20 H20A 109.2 . . ? C21 C20 H20A 109.2 . . ? N7 C20 H20B 109.2 . . ? C21 C20 H20B 109.2 . . ? H20A C20 H20B 107.9 . . ? C22 C21 C23 118.6(4) . . ? C22 C21 C20 120.7(4) . . ? C23 C21 C20 120.7(4) . . ? C21 C22 C26 121.2(4) . . ? C21 C22 H22 119.4 . . ? C26 C22 H22 119.4 . . ? C27 C23 C21 119.8(4) . . ? C27 C23 H23 120.1 . . ? C21 C23 H23 120.1 . . ? C25 C24 C18 121.2(7) . . ? C25 C24 H24 119.4 . . ? C18 C24 H24 119.4 . . ? C24 C25 C19 120.1(7) . . ? C24 C25 H25 120.0 . . ? C19 C25 H25 120.0 . . ? C28 C26 C22 119.9(5) . . ? C28 C26 H26 120.0 . . ? C22 C26 H26 120.0 . . ? C28 C27 C23 120.8(5) . . ? C28 C27 H27 119.6 . . ? C23 C27 H27 119.6 . . ? C27 C28 C26 119.7(5) . . ? C27 C28 H28 120.2 . . ? C26 C28 H28 120.2 . . ? N4 C29 H29A 109.5 . . ? N4 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? N4 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N4 C30 H30A 109.5 . . ? N4 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? N4 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C33 C31 C35 122.3(7) . . ? C33 C31 H31 118.8 . . ? C35 C31 H31 118.8 . . ? C33 C32 C37 120.7(8) . . ? C33 C32 H32 119.6 . . ? C37 C32 H32 119.6 . . ? C31 C33 C32 116.4(6) . . ? C31 C33 C34 122.2(5) . . ? C32 C33 C34 121.3(6) . . ? N6 C34 C33 117.4(4) . . ? N6 C34 H34A 107.9 . . ? C33 C34 H34A 107.9 . . ? N6 C34 H34B 107.9 . . ? C33 C34 H34B 107.9 . . ? H34A C34 H34B 107.2 . . ? C36 C35 C31 119.3(8) . . ? C36 C35 H35 120.4 . . ? C31 C35 H35 120.4 . . ? C37 C36 C35 119.7(9) . . ? C37 C36 H36 120.2 . . ? C35 C36 H36 120.2 . . ? C36 C37 C32 121.5(9) . . ? C36 C37 H37 119.2 . . ? C32 C37 H37 119.2 . . ? O15 C38 C39 124.5(5) . . ? O15 C38 C3 117.1(4) . . ? C39 C38 C3 118.3(5) . . ? C40 C39 C38 122.5(6) . . ? C40 C39 H39 118.8 . . ? C38 C39 H39 118.8 . . ? C39 C40 C41 119.7(6) . . ? C39 C40 H40 120.2 . . ? C41 C40 H40 120.2 . . ? C40 C41 C42 119.8(6) . . ? C40 C41 H41 120.1 . . ? C42 C41 H41 120.1 . . ? C41 C42 C3 121.2(5) . . ? C41 C42 H42 119.4 . . ? C3 C42 H42 119.4 . . ? O9 Tb1 O11 80.51(9) 3_667 . ? O9 Tb1 O12 149.88(9) 3_667 . ? O11 Tb1 O12 86.28(9) . . ? O9 Tb1 O7 87.47(10) 3_667 . ? O11 Tb1 O7 127.58(9) . . ? O12 Tb1 O7 79.34(9) . . ? O9 Tb1 O1 80.31(10) 3_667 . ? O11 Tb1 O1 81.47(9) . . ? O12 Tb1 O1 124.43(10) . . ? O7 Tb1 O1 146.19(10) . . ? O9 Tb1 O5 127.48(9) 3_667 . ? O11 Tb1 O5 148.24(10) . . ? O12 Tb1 O5 74.77(10) . . ? O7 Tb1 O5 74.23(10) . . ? O1 Tb1 O5 88.45(10) . . ? O9 Tb1 O2 128.36(10) 3_667 . ? O11 Tb1 O2 74.96(10) . . ? O12 Tb1 O2 72.64(10) . . ? O7 Tb1 O2 142.81(10) . . ? O1 Tb1 O2 51.82(10) . . ? O5 Tb1 O2 75.16(10) . . ? O9 Tb1 O4 76.24(9) 3_667 . ? O11 Tb1 O4 150.11(8) . . ? O12 Tb1 O4 122.86(9) . . ? O7 Tb1 O4 70.12(9) . . ? O1 Tb1 O4 76.36(10) . . ? O5 Tb1 O4 51.28(9) . . ? O2 Tb1 O4 105.46(10) . . ? O9 Tb1 O6 79.44(8) 3_667 . ? O11 Tb1 O6 76.40(9) . . ? O12 Tb1 O6 71.16(9) . . ? O7 Tb1 O6 51.21(9) . . ? O1 Tb1 O6 152.08(9) . . ? O5 Tb1 O6 119.21(10) . . ? O2 Tb1 O6 134.69(10) . . ? O4 Tb1 O6 116.74(10) . . ? O3 N1 O2 121.5(4) . . ? O3 N1 O1 123.0(4) . . ? O2 N1 O1 115.5(4) . . ? O13 N2 O4 121.8(4) . . ? O13 N2 O5 122.6(4) . . ? O4 N2 O5 115.7(3) . . ? O8 N3 O6 121.3(4) . . ? O8 N3 O7 121.8(4) . . ? O6 N3 O7 116.9(3) . . ? C1 N4 C30 122.7(4) . . ? C1 N4 C29 120.6(5) . . ? C30 N4 C29 116.7(4) . . ? C4 N5 C15 125.3(3) . . ? C4 N5 H5 117.4 . . ? C15 N5 H5 117.4 . . ? C13 N6 C12 114.4(4) . . ? C13 N6 C34 113.3(4) . . ? C12 N6 C34 115.4(3) . . ? C2 N7 C20 126.0(3) . . ? C2 N7 H7 117.0 . . ? C20 N7 H7 117.0 . . ? N1 O1 Tb1 97.0(2) . . ? N1 O2 Tb1 95.3(3) . . ? N2 O4 Tb1 96.1(2) . . ? N2 O5 Tb1 96.3(2) . . ? N3 O6 Tb1 94.2(2) . . ? N3 O7 Tb1 97.6(2) . . ? C2 O9 Tb1 174.7(3) . 3_667 ? C4 O11 Tb1 178.8(3) . . ? C1 O12 Tb1 134.1(3) . . ? C7 O14 C11 119.0(3) . . ? C38 O15 C14 122.4(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O9 C2 C3 C42 -9.7(5) . . . . ? N7 C2 C3 C42 169.5(4) . . . . ? O9 C2 C3 C38 169.7(4) . . . . ? N7 C2 C3 C38 -11.2(6) . . . . ? O11 C4 C5 C6 14.1(5) . . . . ? N5 C4 C5 C6 -165.2(3) . . . . ? O11 C4 C5 C7 -164.4(3) . . . . ? N5 C4 C5 C7 16.3(5) . . . . ? C7 C5 C6 C10 -0.8(5) . . . . ? C4 C5 C6 C10 -179.4(3) . . . . ? C6 C5 C7 O14 -178.7(3) . . . . ? C4 C5 C7 O14 -0.2(5) . . . . ? C6 C5 C7 C8 0.3(5) . . . . ? C4 C5 C7 C8 178.7(3) . . . . ? O14 C7 C8 C9 179.2(3) . . . . ? C5 C7 C8 C9 0.3(5) . . . . ? C7 C8 C9 C10 -0.3(6) . . . . ? C5 C6 C10 C9 0.9(6) . . . . ? C8 C9 C10 C6 -0.3(6) . . . . ? O14 C11 C12 N6 -178.0(3) . . . . ? N6 C13 C14 O15 -12.2(12) . . . . ? N5 C15 C16 C18 126.5(4) . . . . ? N5 C15 C16 C17 -56.6(5) . . . . ? C18 C16 C17 C19 1.6(8) . . . . ? C15 C16 C17 C19 -175.4(5) . . . . ? C17 C16 C18 C24 -2.2(8) . . . . ? C15 C16 C18 C24 174.8(5) . . . . ? C16 C17 C19 C25 0.6(9) . . . . ? N7 C20 C21 C22 -64.9(5) . . . . ? N7 C20 C21 C23 116.5(4) . . . . ? C23 C21 C22 C26 -0.7(6) . . . . ? C20 C21 C22 C26 -179.2(4) . . . . ? C22 C21 C23 C27 0.2(6) . . . . ? C20 C21 C23 C27 178.8(4) . . . . ? C16 C18 C24 C25 0.7(11) . . . . ? C18 C24 C25 C19 1.6(12) . . . . ? C17 C19 C25 C24 -2.2(11) . . . . ? C21 C22 C26 C28 0.7(7) . . . . ? C21 C23 C27 C28 0.3(7) . . . . ? C23 C27 C28 C26 -0.3(7) . . . . ? C22 C26 C28 C27 -0.2(7) . . . . ? C35 C31 C33 C32 -0.4(9) . . . . ? C35 C31 C33 C34 179.9(5) . . . . ? C37 C32 C33 C31 -0.4(9) . . . . ? C37 C32 C33 C34 179.3(6) . . . . ? C31 C33 C34 N6 -64.8(7) . . . . ? C32 C33 C34 N6 115.6(5) . . . . ? C33 C31 C35 C36 1.5(10) . . . . ? C31 C35 C36 C37 -1.7(13) . . . . ? C35 C36 C37 C32 0.9(16) . . . . ? C33 C32 C37 C36 0.2(13) . . . . ? C42 C3 C38 O15 178.6(4) . . . . ? C2 C3 C38 O15 -0.8(6) . . . . ? C42 C3 C38 C39 0.1(6) . . . . ? C2 C3 C38 C39 -179.2(4) . . . . ? O15 C38 C39 C40 -179.3(5) . . . . ? C3 C38 C39 C40 -1.0(8) . . . . ? C38 C39 C40 C41 1.3(9) . . . . ? C39 C40 C41 C42 -0.8(9) . . . . ? C40 C41 C42 C3 0.0(7) . . . . ? C38 C3 C42 C41 0.3(6) . . . . ? C2 C3 C42 C41 179.7(4) . . . . ? O12 C1 N4 C30 -0.3(8) . . . . ? O12 C1 N4 C29 176.8(5) . . . . ? O11 C4 N5 C15 7.4(6) . . . . ? C5 C4 N5 C15 -173.4(3) . . . . ? C16 C15 N5 C4 99.5(4) . . . . ? C14 C13 N6 C12 116.7(8) . . . . ? C14 C13 N6 C34 -108.1(8) . . . . ? C11 C12 N6 C13 -83.5(5) . . . . ? C11 C12 N6 C34 142.4(4) . . . . ? C33 C34 N6 C13 -53.9(6) . . . . ? C33 C34 N6 C12 80.7(6) . . . . ? O9 C2 N7 C20 -2.8(6) . . . . ? C3 C2 N7 C20 178.1(4) . . . . ? C21 C20 N7 C2 132.3(4) . . . . ? O3 N1 O1 Tb1 -172.7(4) . . . . ? O2 N1 O1 Tb1 6.3(4) . . . . ? O9 Tb1 O1 N1 155.6(2) 3_667 . . . ? O11 Tb1 O1 N1 73.9(2) . . . . ? O12 Tb1 O1 N1 -5.6(3) . . . . ? O7 Tb1 O1 N1 -134.0(2) . . . . ? O5 Tb1 O1 N1 -75.9(2) . . . . ? O2 Tb1 O1 N1 -3.7(2) . . . . ? O4 Tb1 O1 N1 -126.3(2) . . . . ? O6 Tb1 O1 N1 111.6(3) . . . . ? O3 N1 O2 Tb1 172.9(4) . . . . ? O1 N1 O2 Tb1 -6.1(4) . . . . ? O9 Tb1 O2 N1 -22.7(3) 3_667 . . . ? O11 Tb1 O2 N1 -87.2(2) . . . . ? O12 Tb1 O2 N1 -178.0(3) . . . . ? O7 Tb1 O2 N1 139.1(2) . . . . ? O1 Tb1 O2 N1 3.7(2) . . . . ? O5 Tb1 O2 N1 103.6(2) . . . . ? O4 Tb1 O2 N1 61.8(2) . . . . ? O6 Tb1 O2 N1 -139.8(2) . . . . ? O13 N2 O4 Tb1 171.5(3) . . . . ? O5 N2 O4 Tb1 -7.6(3) . . . . ? O9 Tb1 O4 N2 -173.2(2) 3_667 . . . ? O11 Tb1 O4 N2 146.9(2) . . . . ? O12 Tb1 O4 N2 -18.8(3) . . . . ? O7 Tb1 O4 N2 -80.9(2) . . . . ? O1 Tb1 O4 N2 103.6(2) . . . . ? O5 Tb1 O4 N2 4.5(2) . . . . ? O2 Tb1 O4 N2 60.3(2) . . . . ? O6 Tb1 O4 N2 -102.7(2) . . . . ? O13 N2 O5 Tb1 -171.5(4) . . . . ? O4 N2 O5 Tb1 7.6(3) . . . . ? O9 Tb1 O5 N2 -1.6(3) 3_667 . . . ? O11 Tb1 O5 N2 -149.2(2) . . . . ? O12 Tb1 O5 N2 155.4(2) . . . . ? O7 Tb1 O5 N2 72.4(2) . . . . ? O1 Tb1 O5 N2 -78.2(2) . . . . ? O2 Tb1 O5 N2 -128.9(2) . . . . ? O4 Tb1 O5 N2 -4.5(2) . . . . ? O6 Tb1 O5 N2 97.8(2) . . . . ? O8 N3 O6 Tb1 174.6(3) . . . . ? O7 N3 O6 Tb1 -4.4(3) . . . . ? O9 Tb1 O6 N3 97.9(2) 3_667 . . . ? O11 Tb1 O6 N3 -179.4(2) . . . . ? O12 Tb1 O6 N3 -88.7(2) . . . . ? O7 Tb1 O6 N3 2.60(19) . . . . ? O1 Tb1 O6 N3 142.1(2) . . . . ? O5 Tb1 O6 N3 -29.3(2) . . . . ? O2 Tb1 O6 N3 -127.4(2) . . . . ? O4 Tb1 O6 N3 29.3(2) . . . . ? O8 N3 O7 Tb1 -174.4(3) . . . . ? O6 N3 O7 Tb1 4.6(3) . . . . ? O9 Tb1 O7 N3 -81.1(2) 3_667 . . . ? O11 Tb1 O7 N3 -5.1(3) . . . . ? O12 Tb1 O7 N3 71.7(2) . . . . ? O1 Tb1 O7 N3 -149.4(2) . . . . ? O5 Tb1 O7 N3 148.7(2) . . . . ? O2 Tb1 O7 N3 113.1(2) . . . . ? O4 Tb1 O7 N3 -157.4(2) . . . . ? O6 Tb1 O7 N3 -2.61(19) . . . . ? N7 C2 O9 Tb1 -95(3) . . . 3_667 ? C3 C2 O9 Tb1 84(3) . . . 3_667 ? N5 C4 O11 Tb1 -76(13) . . . . ? C5 C4 O11 Tb1 105(13) . . . . ? O9 Tb1 O11 C4 -163(13) 3_667 . . . ? O12 Tb1 O11 C4 44(13) . . . . ? O7 Tb1 O11 C4 118(13) . . . . ? O1 Tb1 O11 C4 -81(13) . . . . ? O5 Tb1 O11 C4 -9(13) . . . . ? O2 Tb1 O11 C4 -29(13) . . . . ? O4 Tb1 O11 C4 -124(13) . . . . ? O6 Tb1 O11 C4 116(13) . . . . ? N4 C1 O12 Tb1 -175.6(3) . . . . ? O9 Tb1 O12 C1 175.1(4) 3_667 . . . ? O11 Tb1 O12 C1 -121.1(4) . . . . ? O7 Tb1 O12 C1 109.5(4) . . . . ? O1 Tb1 O12 C1 -44.1(4) . . . . ? O5 Tb1 O12 C1 33.1(4) . . . . ? O2 Tb1 O12 C1 -45.7(4) . . . . ? O4 Tb1 O12 C1 51.8(4) . . . . ? O6 Tb1 O12 C1 162.0(4) . . . . ? C8 C7 O14 C11 -4.4(5) . . . . ? C5 C7 O14 C11 174.5(3) . . . . ? C12 C11 O14 C7 -168.7(3) . . . . ? C39 C38 O15 C14 -15.8(7) . . . . ? C3 C38 O15 C14 165.9(4) . . . . ? C13 C14 O15 C38 -101.5(8) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.11 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.765 _refine_diff_density_min -0.612 _refine_diff_density_rms 0.079 #===END data_666995 _database_code_depnum_ccdc_archive 'CCDC 666995' #TrackingRef '- cif_Revision.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84 H92 Dy2 N14 O28' _chemical_formula_weight 2070.72 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' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.5259(5) _cell_length_b 14.0911(4) _cell_length_c 19.6787(6) _cell_angle_alpha 90.00 _cell_angle_beta 102.0430(10) _cell_angle_gamma 90.00 _cell_volume 4481.7(2) _cell_formula_units_Z 2 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 8596 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 26.93 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.39 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.534 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2100 _exptl_absorpt_coefficient_mu 1.741 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5080 _exptl_absorpt_correction_T_max 0.8053 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23720 _diffrn_reflns_av_R_equivalents 0.0311 _diffrn_reflns_av_sigmaI/netI 0.0430 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 27.50 _reflns_number_total 10111 _reflns_number_gt 7958 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. #============================================================================== The Following Model and Quality ALERTS were generated - (Acta-Mode) <<< #============================================================================== Format: alert-number_ALERT_alert-type_alert-level text PLAT241_ALERT_2_A Check High Ueq as Compared to Neighbors for C9 The larger than normal range of thermal motion is mostly due to the difference between the disordered ethyl group and the other atoms which are not disordered. ; _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^)+(0.0263P)^2^+2.9463P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10111 _refine_ls_number_parameters 583 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0465 _refine_ls_R_factor_gt 0.0319 _refine_ls_wR_factor_ref 0.0739 _refine_ls_wR_factor_gt 0.0666 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.000 _refine_ls_shift/su_max 0.019 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.0803(2) 0.7828(3) 0.2130(2) 0.0554(9) Uani 1 1 d . . . H1 H 0.0945 0.7957 0.1707 0.066 Uiso 1 1 calc R . . C2 C -0.0258(2) 0.7741(3) 0.2800(2) 0.0737(12) Uani 1 1 d . . . H2A H 0.0181 0.7453 0.3133 0.110 Uiso 1 1 calc R . . H2B H -0.0724 0.7320 0.2705 0.110 Uiso 1 1 calc R . . H2C H -0.0417 0.8326 0.2985 0.110 Uiso 1 1 calc R . . C3 C 0.46893(17) 0.6546(2) 0.36863(15) 0.0380(7) Uani 1 1 d . . . C4 C 0.4791(2) 0.6451(2) 0.44519(16) 0.0469(8) Uani 1 1 d . . . C5 C 0.53058(19) 0.6472(3) 0.26522(17) 0.0560(10) Uani 1 1 d . . . H5A H 0.4777 0.6722 0.2410 0.067 Uiso 1 1 calc R . . H5B H 0.5364 0.5836 0.2481 0.067 Uiso 1 1 calc R . . C6 C 0.4176(4) 0.6682(4) 0.5451(2) 0.0878(16) Uani 1 1 d . . . H6 H 0.3735 0.6888 0.5638 0.105 Uiso 1 1 calc R . . C7 C 0.4136(2) 0.6745(3) 0.47446(18) 0.0604(10) Uani 1 1 d . . . H7 H 0.3661 0.6988 0.4459 0.072 Uiso 1 1 calc R . . C8 C 0.5507(3) 0.6076(3) 0.4893(2) 0.0668(12) Uani 1 1 d . . . C9 C 0.6943(3) 0.5576(5) 0.4975(4) 0.158(4) Uani 1 1 d . . . H9A H 0.6904 0.5400 0.5444 0.190 Uiso 1 1 calc R . . H9B H 0.7149 0.5027 0.4767 0.190 Uiso 1 1 calc R . . C10 C 0.7489(2) 0.6255(4) 0.5016(3) 0.0975(19) Uani 1 1 d . . . H10A H 0.8011 0.5951 0.4997 0.117 Uiso 1 1 calc R . . H10B H 0.7553 0.6525 0.5477 0.117 Uiso 1 1 calc R . . C11 C 0.7900(3) 0.6953(4) 0.4015(2) 0.0760(13) Uani 1 1 d . . . H11A H 0.7829 0.7528 0.3738 0.091 Uiso 1 1 calc R . . H11B H 0.7679 0.6433 0.3710 0.091 Uiso 1 1 calc R . . C12 C 0.8812(3) 0.6788(4) 0.4267(2) 0.0755(13) Uani 1 1 d . . . C13 C 0.7426(2) 0.7958(3) 0.4874(2) 0.0583(10) Uani 1 1 d . . . H13A H 0.7589 0.8439 0.4576 0.070 Uiso 1 1 calc R . . H13B H 0.7833 0.7950 0.5307 0.070 Uiso 1 1 calc R . . C14 C 0.65822(19) 0.8199(3) 0.5015(2) 0.0532(9) Uani 1 1 d . . . H14A H 0.6168 0.8195 0.4586 0.064 Uiso 1 1 calc R . . H14B H 0.6425 0.7738 0.5330 0.064 Uiso 1 1 calc R . . C15 C 0.60120(17) 0.9453(2) 0.56038(16) 0.0400(7) Uani 1 1 d . . . C16 C 0.46642(19) 0.9296(3) 0.58605(17) 0.0500(9) Uani 1 1 d . . . H16 H 0.4177 0.8954 0.5831 0.060 Uiso 1 1 calc R . . C17 C 0.52811(18) 0.8942(3) 0.55589(17) 0.0458(8) Uani 1 1 d . . . H17 H 0.5210 0.8365 0.5326 0.055 Uiso 1 1 calc R . . C18 C 0.47617(19) 1.0149(3) 0.62052(18) 0.0510(9) Uani 1 1 d . . . H18 H 0.4340 1.0383 0.6406 0.061 Uiso 1 1 calc R . . C19 C 0.54844(18) 1.0659(3) 0.62536(16) 0.0431(7) Uani 1 1 d . . . H19 H 0.5547 1.1234 0.6490 0.052 Uiso 1 1 calc R . . C20 C 0.61220(16) 1.0323(2) 0.59531(15) 0.0360(7) Uani 1 1 d . . . C21 C 0.68819(17) 1.0919(2) 0.60445(15) 0.0365(7) Uani 1 1 d . . . C22 C 0.82319(18) 1.1196(3) 0.57289(19) 0.0490(8) Uani 1 1 d . . . H22A H 0.8233 1.1789 0.5979 0.059 Uiso 1 1 calc R . . H22B H 0.8335 1.1339 0.5272 0.059 Uiso 1 1 calc R . . C23 C 0.9177(4) 0.5962(4) 0.4114(3) 0.116(2) Uani 1 1 d . . . H23 H 0.8854 0.5497 0.3851 0.139 Uiso 1 1 calc R . . C24 C 1.0172(3) 0.7292(5) 0.4887(4) 0.125(2) Uani 1 1 d . . . H24 H 1.0502 0.7740 0.5163 0.150 Uiso 1 1 calc R . . C25 C 0.9328(3) 0.7452(4) 0.4651(3) 0.0959(17) Uani 1 1 d . . . H25 H 0.9104 0.8026 0.4757 0.115 Uiso 1 1 calc R . . C26 C 1.0017(5) 0.5809(6) 0.4342(5) 0.149(3) Uani 1 1 d . . . H26 H 1.0247 0.5237 0.4240 0.179 Uiso 1 1 calc R . . C27 C 1.0507(4) 0.6473(7) 0.4708(5) 0.146(4) Uani 1 1 d . . . H27 H 1.1074 0.6372 0.4839 0.175 Uiso 1 1 calc R . . C28 C 0.6614(2) 0.6709(3) 0.22133(18) 0.0554(9) Uani 1 1 d . . . H28 H 0.6617 0.6062 0.2120 0.067 Uiso 1 1 calc R . . C29 C 0.59957(18) 0.7092(3) 0.25013(16) 0.0454(8) Uani 1 1 d . . . C30 C 0.6013(2) 0.8048(3) 0.2634(2) 0.0630(10) Uani 1 1 d . . . H30 H 0.5597 0.8316 0.2825 0.076 Uiso 1 1 calc R . . C31 C 0.6632(3) 0.8621(3) 0.2492(2) 0.0733(12) Uani 1 1 d . . . H31 H 0.6635 0.9266 0.2590 0.088 Uiso 1 1 calc R . . C32 C 0.7239(2) 0.8236(4) 0.2206(2) 0.0729(12) Uani 1 1 d . . . H32 H 0.7659 0.8619 0.2109 0.088 Uiso 1 1 calc R . . C33 C 0.7233(2) 0.7288(4) 0.2062(2) 0.0688(12) Uani 1 1 d . . . H33 H 0.7645 0.7029 0.1861 0.083 Uiso 1 1 calc R . . C34 C 0.4872(5) 0.6314(4) 0.5876(2) 0.111(2) Uani 1 1 d . . . H34 H 0.4897 0.6262 0.6351 0.133 Uiso 1 1 calc R . . C35 C 0.5523(4) 0.6023(4) 0.5605(2) 0.098(2) Uani 1 1 d . . . H35 H 0.5991 0.5783 0.5902 0.118 Uiso 1 1 calc R . . C36 C 0.8897(3) 1.0233(3) 0.6769(2) 0.0701(11) Uani 1 1 d . . . H36 H 0.8442 1.0361 0.6963 0.084 Uiso 1 1 calc R . . C37 C 0.8913(2) 1.0563(3) 0.6115(2) 0.0522(9) Uani 1 1 d . . . C38 C 0.9587(2) 1.0346(3) 0.5829(3) 0.0807(14) Uani 1 1 d . . . H38 H 0.9603 1.0551 0.5382 0.097 Uiso 1 1 calc R . . C39 C 0.9546(4) 0.9716(4) 0.7139(3) 0.1008(17) Uani 1 1 d . . . H39 H 0.9525 0.9491 0.7580 0.121 Uiso 1 1 calc R . . C40 C 1.0242(3) 0.9821(5) 0.6209(4) 0.112(2) Uani 1 1 d . . . H40 H 1.0693 0.9671 0.6015 0.134 Uiso 1 1 calc R . . C41 C 1.0224(4) 0.9529(4) 0.6862(4) 0.115(2) Uani 1 1 d . . . H41 H 1.0672 0.9202 0.7122 0.138 Uiso 1 1 calc R . . C42 C -0.0597(3) 0.8197(5) 0.1565(3) 0.1059(19) Uani 1 1 d . . . H42A H -0.0330 0.8357 0.1191 0.159 Uiso 1 1 calc R . . H42B H -0.0900 0.8736 0.1676 0.159 Uiso 1 1 calc R . . H42C H -0.0970 0.7677 0.1427 0.159 Uiso 1 1 calc R . . Dy1 Dy 0.275647(7) 0.726126(11) 0.269829(7) 0.03406(5) Uani 1 1 d . . . H6' H 0.735(2) 1.034(3) 0.5386(18) 0.048(11) Uiso 1 1 d . . . N1 N 0.3177(2) 0.8914(3) 0.19775(16) 0.0599(8) Uani 1 1 d . . . N2 N 0.20842(15) 0.5769(2) 0.34157(16) 0.0473(7) Uani 1 1 d . . . N3 N 0.26210(17) 0.6175(2) 0.14302(15) 0.0549(8) Uani 1 1 d . . . N4 N 0.74028(17) 0.7040(2) 0.45404(15) 0.0500(7) Uani 1 1 d . . . N5 N 0.53232(15) 0.6434(2) 0.33933(14) 0.0545(8) Uani 1 1 d . . . H5 H 0.5795 0.6329 0.3664 0.065 Uiso 1 1 calc R . . N6 N 0.74232(16) 1.0745(2) 0.56533(16) 0.0464(7) Uani 1 1 d . . . N7 N 0.00209(16) 0.7926(2) 0.21697(16) 0.0549(8) Uani 1 1 d . . . O1 O 0.36857(14) 0.8243(2) 0.21867(13) 0.0565(6) Uani 1 1 d . . . O2 O 0.3384(2) 0.9642(2) 0.17370(18) 0.0932(10) Uani 1 1 d . . . O3 O 0.24416(15) 0.8764(2) 0.20423(15) 0.0682(7) Uani 1 1 d . . . O4 O 0.22278(14) 0.56749(18) 0.28135(13) 0.0551(6) Uani 1 1 d . . . O5 O 0.23073(13) 0.65426(18) 0.37214(12) 0.0520(6) Uani 1 1 d . . . O6 O 0.17535(17) 0.5146(2) 0.36882(15) 0.0758(8) Uani 1 1 d . . . O7 O 0.32663(13) 0.6161(2) 0.19000(12) 0.0567(7) Uani 1 1 d . . . O8 O 0.20750(14) 0.6775(2) 0.15119(12) 0.0610(7) Uani 1 1 d . . . O9 O 0.25237(18) 0.5642(3) 0.09340(14) 0.0897(10) Uani 1 1 d . . . O10 O 0.13558(12) 0.75775(17) 0.26159(13) 0.0503(6) Uani 1 1 d . . . O11 O 0.39918(11) 0.67487(18) 0.33253(10) 0.0464(5) Uani 1 1 d . . . O12 O 0.70000(12) 1.15710(17) 0.64798(12) 0.0485(6) Uani 1 1 d . . . O13 O 0.61236(15) 0.5776(2) 0.45899(16) 0.0880(11) Uani 1 1 d . . . O14 O 0.66474(13) 0.91241(17) 0.53206(13) 0.0526(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0405(17) 0.060(3) 0.066(2) 0.0011(19) 0.0131(17) 0.0043(16) C2 0.050(2) 0.093(4) 0.080(3) -0.012(3) 0.019(2) -0.005(2) C3 0.0333(14) 0.0378(18) 0.0394(16) -0.0003(14) -0.0007(12) -0.0079(12) C4 0.0508(18) 0.045(2) 0.0383(17) 0.0056(15) -0.0051(14) -0.0213(15) C5 0.0388(17) 0.080(3) 0.049(2) -0.0115(19) 0.0088(15) -0.0022(17) C6 0.136(4) 0.086(4) 0.045(2) -0.011(2) 0.027(3) -0.044(3) C7 0.075(2) 0.063(3) 0.044(2) -0.0041(18) 0.0117(18) -0.025(2) C8 0.067(2) 0.057(3) 0.060(2) 0.023(2) -0.023(2) -0.034(2) C9 0.055(3) 0.154(6) 0.224(7) 0.134(6) -0.068(3) -0.038(3) C10 0.046(2) 0.083(3) 0.149(5) 0.065(3) -0.015(3) -0.007(2) C11 0.094(3) 0.084(3) 0.052(2) -0.006(2) 0.020(2) 0.031(3) C12 0.089(3) 0.079(3) 0.069(3) 0.014(3) 0.043(2) 0.030(3) C13 0.0508(19) 0.059(3) 0.068(2) -0.017(2) 0.0210(18) -0.0052(17) C14 0.0440(17) 0.045(2) 0.070(2) -0.0183(19) 0.0104(16) -0.0046(16) C15 0.0354(15) 0.044(2) 0.0406(17) -0.0042(14) 0.0077(13) -0.0033(13) C16 0.0389(16) 0.062(2) 0.050(2) -0.0012(18) 0.0103(14) -0.0120(16) C17 0.0427(16) 0.047(2) 0.0488(19) -0.0054(16) 0.0117(14) -0.0103(14) C18 0.0388(16) 0.067(3) 0.051(2) -0.0083(18) 0.0182(15) -0.0059(16) C19 0.0409(16) 0.048(2) 0.0404(17) -0.0072(15) 0.0090(13) -0.0026(14) C20 0.0341(14) 0.0398(18) 0.0339(15) -0.0013(13) 0.0064(12) -0.0052(13) C21 0.0337(14) 0.0363(18) 0.0384(16) -0.0021(14) 0.0050(12) -0.0011(12) C22 0.0371(16) 0.050(2) 0.062(2) -0.0058(17) 0.0158(15) -0.0085(14) C23 0.126(5) 0.101(5) 0.139(5) 0.013(4) 0.072(4) 0.052(4) C24 0.072(3) 0.150(6) 0.168(7) 0.053(5) 0.059(4) 0.006(4) C25 0.077(3) 0.107(5) 0.116(5) 0.018(4) 0.047(3) 0.019(3) C26 0.130(6) 0.132(7) 0.214(9) 0.057(7) 0.105(7) 0.072(5) C27 0.087(5) 0.161(8) 0.215(9) 0.099(7) 0.088(5) 0.052(5) C28 0.0463(18) 0.068(3) 0.054(2) -0.0095(19) 0.0146(16) 0.0006(18) C29 0.0367(15) 0.063(3) 0.0349(16) -0.0061(15) 0.0043(13) 0.0002(15) C30 0.058(2) 0.068(3) 0.065(2) -0.008(2) 0.0173(19) 0.008(2) C31 0.080(3) 0.062(3) 0.075(3) 0.005(2) 0.010(2) -0.006(2) C32 0.064(2) 0.093(4) 0.062(3) 0.015(3) 0.015(2) -0.012(2) C33 0.054(2) 0.099(4) 0.059(2) -0.004(2) 0.0249(18) 0.004(2) C34 0.184(6) 0.100(4) 0.037(2) 0.008(3) -0.002(3) -0.079(5) C35 0.130(4) 0.085(4) 0.054(3) 0.029(3) -0.041(3) -0.058(3) C36 0.068(3) 0.054(3) 0.085(3) -0.001(2) 0.009(2) 0.006(2) C37 0.0426(17) 0.044(2) 0.069(2) -0.0126(18) 0.0106(16) -0.0018(15) C38 0.058(2) 0.080(3) 0.108(4) -0.013(3) 0.027(2) 0.011(2) C39 0.118(4) 0.067(4) 0.105(4) 0.010(3) -0.004(4) 0.014(3) C40 0.060(3) 0.105(5) 0.169(6) -0.030(5) 0.019(4) 0.024(3) C41 0.083(4) 0.072(4) 0.164(6) -0.011(4) -0.031(4) 0.024(3) C42 0.060(3) 0.154(6) 0.096(4) 0.031(4) 0.001(2) 0.031(3) Dy1 0.02614(7) 0.03955(9) 0.03634(8) -0.00210(7) 0.00620(5) -0.00122(6) N1 0.073(2) 0.057(2) 0.0530(19) 0.0050(16) 0.0224(16) -0.0068(18) N2 0.0363(13) 0.0459(19) 0.0571(18) 0.0129(15) 0.0041(12) -0.0007(12) N3 0.0468(16) 0.080(2) 0.0400(16) -0.0094(15) 0.0126(13) -0.0036(15) N4 0.0539(16) 0.0423(18) 0.0530(17) 0.0012(14) 0.0093(13) 0.0070(13) N5 0.0287(12) 0.085(2) 0.0476(16) 0.0114(16) 0.0019(11) 0.0021(13) N6 0.0415(14) 0.0474(19) 0.0528(18) -0.0156(15) 0.0158(13) -0.0125(13) N7 0.0325(13) 0.064(2) 0.0666(19) -0.0004(16) 0.0069(13) 0.0071(13) O1 0.0524(13) 0.0632(18) 0.0590(15) 0.0091(14) 0.0232(12) -0.0011(13) O2 0.121(3) 0.064(2) 0.106(3) 0.0253(19) 0.051(2) -0.0146(19) O3 0.0541(15) 0.0645(19) 0.0855(19) 0.0218(16) 0.0133(14) 0.0051(13) O4 0.0634(15) 0.0472(16) 0.0560(15) -0.0033(12) 0.0156(12) -0.0042(12) O5 0.0503(13) 0.0565(17) 0.0505(14) -0.0022(12) 0.0134(11) -0.0092(11) O6 0.0767(18) 0.067(2) 0.085(2) 0.0258(16) 0.0197(15) -0.0202(15) O7 0.0357(11) 0.082(2) 0.0512(14) -0.0170(13) 0.0071(10) 0.0034(12) O8 0.0490(13) 0.084(2) 0.0463(14) -0.0058(14) 0.0020(11) 0.0158(13) O9 0.0808(19) 0.131(3) 0.0556(17) -0.0470(19) 0.0095(14) 0.0011(19) O10 0.0302(11) 0.0575(16) 0.0613(15) -0.0019(12) 0.0049(10) 0.0045(10) O11 0.0313(10) 0.0682(17) 0.0376(11) -0.0015(11) 0.0023(9) 0.0061(10) O12 0.0435(12) 0.0470(15) 0.0573(14) -0.0175(12) 0.0160(10) -0.0103(10) O13 0.0400(14) 0.107(3) 0.102(2) 0.055(2) -0.0208(14) -0.0116(15) O14 0.0455(12) 0.0446(15) 0.0729(16) -0.0222(12) 0.0238(11) -0.0091(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O10 1.228(4) . ? C1 N7 1.317(4) . ? C1 H1 0.9300 . ? C2 N7 1.434(5) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 O11 1.254(3) . ? C3 N5 1.307(4) . ? C3 C4 1.487(4) . ? C4 C7 1.392(5) . ? C4 C8 1.415(5) . ? C5 N5 1.454(4) . ? C5 C29 1.514(5) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C34 1.374(8) . ? C6 C7 1.380(5) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 O13 1.352(5) . ? C8 C35 1.398(6) . ? C9 C10 1.307(6) . ? C9 O13 1.434(4) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N4 1.437(5) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 N4 1.453(5) . ? C11 C12 1.503(6) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C23 1.374(7) . ? C12 C25 1.380(7) . ? C13 N4 1.447(5) . ? C13 C14 1.517(4) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 O14 1.431(4) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 O14 1.368(3) . ? C15 C17 1.393(4) . ? C15 C20 1.398(4) . ? C16 C18 1.373(5) . ? C16 C17 1.376(4) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.380(4) . ? C18 H18 0.9300 . ? C19 C20 1.394(4) . ? C19 H19 0.9300 . ? C20 C21 1.490(4) . ? C21 O12 1.244(4) . ? C21 N6 1.319(4) . ? C22 N6 1.459(4) . ? C22 C37 1.510(5) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C26 1.384(9) . ? C23 H23 0.9300 . ? C24 C27 1.357(10) . ? C24 C25 1.395(7) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 C27 1.344(11) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 C29 1.378(4) . ? C28 C33 1.388(5) . ? C28 H28 0.9300 . ? C29 C30 1.372(5) . ? C30 C31 1.377(6) . ? C30 H30 0.9300 . ? C31 C32 1.361(6) . ? C31 H31 0.9300 . ? C32 C33 1.366(7) . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? C34 C35 1.359(8) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C36 C39 1.374(6) . ? C36 C37 1.374(6) . ? C36 H36 0.9300 . ? C37 C38 1.382(5) . ? C38 C40 1.394(7) . ? C38 H38 0.9300 . ? C39 C41 1.371(8) . ? C39 H39 0.9300 . ? C40 C41 1.355(8) . ? C40 H40 0.9300 . ? C41 H41 0.9300 . ? C42 N7 1.448(5) . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? Dy1 O11 2.2718(19) . ? Dy1 O12 2.283(2) 3_676 ? Dy1 O10 2.329(2) . ? Dy1 O4 2.428(2) . ? Dy1 O1 2.435(2) . ? Dy1 O8 2.468(2) . ? Dy1 O7 2.477(2) . ? Dy1 O3 2.479(3) . ? Dy1 O5 2.501(2) . ? N1 O2 1.209(4) . ? N1 O3 1.265(4) . ? N1 O1 1.275(4) . ? N2 O6 1.216(3) . ? N2 O5 1.263(4) . ? N2 O4 1.263(4) . ? N3 O9 1.216(4) . ? N3 O7 1.257(3) . ? N3 O8 1.271(4) . ? N5 H5 0.8600 . ? N6 H6' 0.77(3) . ? O12 Dy1 2.283(2) 3_676 ? 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 O10 C1 N7 124.3(4) . . ? O10 C1 H1 117.8 . . ? N7 C1 H1 117.8 . . ? N7 C2 H2A 109.5 . . ? N7 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N7 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? O11 C3 N5 120.3(3) . . ? O11 C3 C4 119.4(3) . . ? N5 C3 C4 120.3(3) . . ? C7 C4 C8 118.7(3) . . ? C7 C4 C3 117.3(3) . . ? C8 C4 C3 124.0(3) . . ? N5 C5 C29 111.1(3) . . ? N5 C5 H5A 109.4 . . ? C29 C5 H5A 109.4 . . ? N5 C5 H5B 109.4 . . ? C29 C5 H5B 109.4 . . ? H5A C5 H5B 108.0 . . ? C34 C6 C7 119.7(5) . . ? C34 C6 H6 120.2 . . ? C7 C6 H6 120.2 . . ? C6 C7 C4 121.3(4) . . ? C6 C7 H7 119.4 . . ? C4 C7 H7 119.4 . . ? O13 C8 C35 124.6(4) . . ? O13 C8 C4 117.1(3) . . ? C35 C8 C4 118.3(5) . . ? C10 C9 O13 116.9(4) . . ? C10 C9 H9A 108.1 . . ? O13 C9 H9A 108.1 . . ? C10 C9 H9B 108.1 . . ? O13 C9 H9B 108.1 . . ? H9A C9 H9B 107.3 . . ? C9 C10 N4 123.4(4) . . ? C9 C10 H10A 106.5 . . ? N4 C10 H10A 106.5 . . ? C9 C10 H10B 106.5 . . ? N4 C10 H10B 106.5 . . ? H10A C10 H10B 106.5 . . ? N4 C11 C12 117.1(3) . . ? N4 C11 H11A 108.0 . . ? C12 C11 H11A 108.0 . . ? N4 C11 H11B 108.0 . . ? C12 C11 H11B 108.0 . . ? H11A C11 H11B 107.3 . . ? C23 C12 C25 116.4(5) . . ? C23 C12 C11 121.0(5) . . ? C25 C12 C11 122.6(4) . . ? N4 C13 C14 110.1(3) . . ? N4 C13 H13A 109.6 . . ? C14 C13 H13A 109.6 . . ? N4 C13 H13B 109.6 . . ? C14 C13 H13B 109.6 . . ? H13A C13 H13B 108.1 . . ? O14 C14 C13 106.8(3) . . ? O14 C14 H14A 110.4 . . ? C13 C14 H14A 110.4 . . ? O14 C14 H14B 110.4 . . ? C13 C14 H14B 110.4 . . ? H14A C14 H14B 108.6 . . ? O14 C15 C17 121.9(3) . . ? O14 C15 C20 117.7(3) . . ? C17 C15 C20 120.4(3) . . ? C18 C16 C17 120.6(3) . . ? C18 C16 H16 119.7 . . ? C17 C16 H16 119.7 . . ? C16 C17 C15 119.8(3) . . ? C16 C17 H17 120.1 . . ? C15 C17 H17 120.1 . . ? C16 C18 C19 120.0(3) . . ? C16 C18 H18 120.0 . . ? C19 C18 H18 120.0 . . ? C18 C19 C20 120.9(3) . . ? C18 C19 H19 119.5 . . ? C20 C19 H19 119.5 . . ? C19 C20 C15 118.3(3) . . ? C19 C20 C21 116.7(3) . . ? C15 C20 C21 125.0(3) . . ? O12 C21 N6 120.7(3) . . ? O12 C21 C20 120.5(3) . . ? N6 C21 C20 118.8(3) . . ? N6 C22 C37 111.5(3) . . ? N6 C22 H22A 109.3 . . ? C37 C22 H22A 109.3 . . ? N6 C22 H22B 109.3 . . ? C37 C22 H22B 109.3 . . ? H22A C22 H22B 108.0 . . ? C12 C23 C26 121.2(7) . . ? C12 C23 H23 119.4 . . ? C26 C23 H23 119.4 . . ? C27 C24 C25 119.0(7) . . ? C27 C24 H24 120.5 . . ? C25 C24 H24 120.5 . . ? C12 C25 C24 122.3(6) . . ? C12 C25 H25 118.9 . . ? C24 C25 H25 118.9 . . ? C27 C26 C23 121.1(8) . . ? C27 C26 H26 119.4 . . ? C23 C26 H26 119.4 . . ? C26 C27 C24 119.9(7) . . ? C26 C27 H27 120.0 . . ? C24 C27 H27 120.0 . . ? C29 C28 C33 120.1(4) . . ? C29 C28 H28 119.9 . . ? C33 C28 H28 119.9 . . ? C30 C29 C28 118.3(3) . . ? C30 C29 C5 121.1(3) . . ? C28 C29 C5 120.6(3) . . ? C29 C30 C31 121.6(4) . . ? C29 C30 H30 119.2 . . ? C31 C30 H30 119.2 . . ? C32 C31 C30 119.5(4) . . ? C32 C31 H31 120.2 . . ? C30 C31 H31 120.2 . . ? C31 C32 C33 120.1(4) . . ? C31 C32 H32 119.9 . . ? C33 C32 H32 119.9 . . ? C32 C33 C28 120.2(4) . . ? C32 C33 H33 119.9 . . ? C28 C33 H33 119.9 . . ? C35 C34 C6 120.4(5) . . ? C35 C34 H34 119.8 . . ? C6 C34 H34 119.8 . . ? C34 C35 C8 121.7(5) . . ? C34 C35 H35 119.2 . . ? C8 C35 H35 119.2 . . ? C39 C36 C37 120.8(5) . . ? C39 C36 H36 119.6 . . ? C37 C36 H36 119.6 . . ? C36 C37 C38 118.8(4) . . ? C36 C37 C22 120.8(3) . . ? C38 C37 C22 120.3(4) . . ? C37 C38 C40 120.0(5) . . ? C37 C38 H38 120.0 . . ? C40 C38 H38 120.0 . . ? C41 C39 C36 120.2(6) . . ? C41 C39 H39 119.9 . . ? C36 C39 H39 119.9 . . ? C41 C40 C38 120.1(5) . . ? C41 C40 H40 119.9 . . ? C38 C40 H40 119.9 . . ? C40 C41 C39 120.1(5) . . ? C40 C41 H41 120.0 . . ? C39 C41 H41 120.0 . . ? N7 C42 H42A 109.5 . . ? N7 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? N7 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? O11 Dy1 O12 80.72(8) . 3_676 ? O11 Dy1 O10 149.99(8) . . ? O12 Dy1 O10 86.39(8) 3_676 . ? O11 Dy1 O4 87.52(9) . . ? O12 Dy1 O4 127.66(8) 3_676 . ? O10 Dy1 O4 79.10(8) . . ? O11 Dy1 O1 80.35(8) . . ? O12 Dy1 O1 81.40(8) 3_676 . ? O10 Dy1 O1 124.45(9) . . ? O4 Dy1 O1 146.29(9) . . ? O11 Dy1 O8 127.34(8) . . ? O12 Dy1 O8 148.03(9) 3_676 . ? O10 Dy1 O8 74.73(8) . . ? O4 Dy1 O8 74.37(9) . . ? O1 Dy1 O8 88.24(9) . . ? O11 Dy1 O7 76.08(8) . . ? O12 Dy1 O7 150.16(7) 3_676 . ? O10 Dy1 O7 122.70(8) . . ? O4 Dy1 O7 70.10(8) . . ? O1 Dy1 O7 76.46(9) . . ? O8 Dy1 O7 51.29(8) . . ? O11 Dy1 O3 128.45(9) . . ? O12 Dy1 O3 74.92(9) 3_676 . ? O10 Dy1 O3 72.70(8) . . ? O4 Dy1 O3 142.65(8) . . ? O1 Dy1 O3 51.77(8) . . ? O8 Dy1 O3 74.92(10) . . ? O7 Dy1 O3 105.47(9) . . ? O11 Dy1 O5 79.52(7) . . ? O12 Dy1 O5 76.09(8) 3_676 . ? O10 Dy1 O5 71.09(8) . . ? O4 Dy1 O5 51.60(8) . . ? O1 Dy1 O5 151.83(8) . . ? O8 Dy1 O5 119.71(8) . . ? O7 Dy1 O5 117.04(9) . . ? O3 Dy1 O5 134.43(9) . . ? O2 N1 O3 122.4(4) . . ? O2 N1 O1 122.3(3) . . ? O3 N1 O1 115.3(3) . . ? O6 N2 O5 121.8(3) . . ? O6 N2 O4 121.9(3) . . ? O5 N2 O4 116.3(3) . . ? O9 N3 O7 122.0(3) . . ? O9 N3 O8 122.3(3) . . ? O7 N3 O8 115.7(3) . . ? C10 N4 C13 113.8(4) . . ? C10 N4 C11 113.8(4) . . ? C13 N4 C11 115.6(3) . . ? C3 N5 C5 126.1(3) . . ? C3 N5 H5 117.0 . . ? C5 N5 H5 117.0 . . ? C21 N6 C22 125.3(3) . . ? C21 N6 H6' 120(3) . . ? C22 N6 H6' 114(3) . . ? C1 N7 C2 121.8(3) . . ? C1 N7 C42 120.7(4) . . ? C2 N7 C42 117.4(3) . . ? N1 O1 Dy1 97.13(19) . . ? N1 O3 Dy1 95.3(2) . . ? N2 O4 Dy1 97.65(19) . . ? N2 O5 Dy1 94.16(18) . . ? N3 O7 Dy1 96.20(18) . . ? N3 O8 Dy1 96.23(18) . . ? C1 O10 Dy1 132.6(2) . . ? C3 O11 Dy1 174.6(2) . . ? C21 O12 Dy1 178.3(2) . 3_676 ? C8 O13 C9 122.9(4) . . ? C15 O14 C14 118.9(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O11 C3 C4 C7 -10.3(5) . . . . ? N5 C3 C4 C7 168.6(3) . . . . ? O11 C3 C4 C8 169.1(3) . . . . ? N5 C3 C4 C8 -11.9(5) . . . . ? C34 C6 C7 C4 -0.7(7) . . . . ? C8 C4 C7 C6 0.4(6) . . . . ? C3 C4 C7 C6 180.0(4) . . . . ? C7 C4 C8 O13 178.4(3) . . . . ? C3 C4 C8 O13 -1.1(5) . . . . ? C7 C4 C8 C35 -0.4(5) . . . . ? C3 C4 C8 C35 -179.8(3) . . . . ? O13 C9 C10 N4 -20.1(11) . . . . ? N4 C11 C12 C23 115.9(5) . . . . ? N4 C11 C12 C25 -65.1(6) . . . . ? N4 C13 C14 O14 -178.0(3) . . . . ? C18 C16 C17 C15 0.1(5) . . . . ? O14 C15 C17 C16 179.1(3) . . . . ? C20 C15 C17 C16 0.0(5) . . . . ? C17 C16 C18 C19 -0.2(5) . . . . ? C16 C18 C19 C20 0.4(5) . . . . ? C18 C19 C20 C15 -0.3(5) . . . . ? C18 C19 C20 C21 -179.1(3) . . . . ? O14 C15 C20 C19 -179.0(3) . . . . ? C17 C15 C20 C19 0.1(5) . . . . ? O14 C15 C20 C21 -0.3(5) . . . . ? C17 C15 C20 C21 178.8(3) . . . . ? C19 C20 C21 O12 14.0(4) . . . . ? C15 C20 C21 O12 -164.7(3) . . . . ? C19 C20 C21 N6 -165.7(3) . . . . ? C15 C20 C21 N6 15.6(5) . . . . ? C25 C12 C23 C26 0.7(8) . . . . ? C11 C12 C23 C26 179.7(5) . . . . ? C23 C12 C25 C24 -1.4(8) . . . . ? C11 C12 C25 C24 179.6(5) . . . . ? C27 C24 C25 C12 2.9(9) . . . . ? C12 C23 C26 C27 -1.5(11) . . . . ? C23 C26 C27 C24 3.0(13) . . . . ? C25 C24 C27 C26 -3.6(11) . . . . ? C33 C28 C29 C30 -0.3(5) . . . . ? C33 C28 C29 C5 178.5(3) . . . . ? N5 C5 C29 C30 -65.1(4) . . . . ? N5 C5 C29 C28 116.2(4) . . . . ? C28 C29 C30 C31 -0.5(6) . . . . ? C5 C29 C30 C31 -179.2(4) . . . . ? C29 C30 C31 C32 0.6(6) . . . . ? C30 C31 C32 C33 0.0(6) . . . . ? C31 C32 C33 C28 -0.8(6) . . . . ? C29 C28 C33 C32 0.9(6) . . . . ? C7 C6 C34 C35 0.9(8) . . . . ? C6 C34 C35 C8 -0.8(8) . . . . ? O13 C8 C35 C34 -178.1(4) . . . . ? C4 C8 C35 C34 0.6(7) . . . . ? C39 C36 C37 C38 1.5(6) . . . . ? C39 C36 C37 C22 -175.2(4) . . . . ? N6 C22 C37 C36 -57.0(5) . . . . ? N6 C22 C37 C38 126.3(4) . . . . ? C36 C37 C38 C40 -1.5(7) . . . . ? C22 C37 C38 C40 175.2(4) . . . . ? C37 C36 C39 C41 0.6(8) . . . . ? C37 C38 C40 C41 -0.6(9) . . . . ? C38 C40 C41 C39 2.7(10) . . . . ? C36 C39 C41 C40 -2.7(9) . . . . ? C9 C10 N4 C13 122.7(7) . . . . ? C9 C10 N4 C11 -102.0(7) . . . . ? C14 C13 N4 C10 -82.2(4) . . . . ? C14 C13 N4 C11 143.3(3) . . . . ? C12 C11 N4 C10 -54.4(5) . . . . ? C12 C11 N4 C13 80.1(5) . . . . ? O11 C3 N5 C5 -3.5(6) . . . . ? C4 C3 N5 C5 177.5(3) . . . . ? C29 C5 N5 C3 132.7(4) . . . . ? O12 C21 N6 C22 7.1(5) . . . . ? C20 C21 N6 C22 -173.2(3) . . . . ? C37 C22 N6 C21 99.9(4) . . . . ? O10 C1 N7 C2 -0.2(6) . . . . ? O10 C1 N7 C42 -178.1(4) . . . . ? O2 N1 O1 Dy1 172.7(3) . . . . ? O3 N1 O1 Dy1 -7.0(3) . . . . ? O11 Dy1 O1 N1 -155.4(2) . . . . ? O12 Dy1 O1 N1 -73.4(2) 3_676 . . . ? O10 Dy1 O1 N1 6.2(2) . . . . ? O4 Dy1 O1 N1 134.1(2) . . . . ? O8 Dy1 O1 N1 76.2(2) . . . . ? O7 Dy1 O1 N1 126.7(2) . . . . ? O3 Dy1 O1 N1 4.13(19) . . . . ? O5 Dy1 O1 N1 -110.5(2) . . . . ? O2 N1 O3 Dy1 -172.8(3) . . . . ? O1 N1 O3 Dy1 6.9(3) . . . . ? O11 Dy1 O3 N1 22.0(3) . . . . ? O12 Dy1 O3 N1 86.7(2) 3_676 . . . ? O10 Dy1 O3 N1 177.6(2) . . . . ? O4 Dy1 O3 N1 -139.7(2) . . . . ? O1 Dy1 O3 N1 -4.15(19) . . . . ? O8 Dy1 O3 N1 -104.0(2) . . . . ? O7 Dy1 O3 N1 -62.3(2) . . . . ? O5 Dy1 O3 N1 138.92(19) . . . . ? O6 N2 O4 Dy1 175.4(3) . . . . ? O5 N2 O4 Dy1 -5.0(3) . . . . ? O11 Dy1 O4 N2 81.45(17) . . . . ? O12 Dy1 O4 N2 5.2(2) 3_676 . . . ? O10 Dy1 O4 N2 -71.55(18) . . . . ? O1 Dy1 O4 N2 149.90(17) . . . . ? O8 Dy1 O4 N2 -148.57(19) . . . . ? O7 Dy1 O4 N2 157.54(19) . . . . ? O3 Dy1 O4 N2 -112.8(2) . . . . ? O5 Dy1 O4 N2 2.87(16) . . . . ? O6 N2 O5 Dy1 -175.6(3) . . . . ? O4 N2 O5 Dy1 4.8(3) . . . . ? O11 Dy1 O5 N2 -98.05(17) . . . . ? O12 Dy1 O5 N2 179.02(18) 3_676 . . . ? O10 Dy1 O5 N2 88.09(17) . . . . ? O4 Dy1 O5 N2 -2.86(16) . . . . ? O1 Dy1 O5 N2 -143.07(19) . . . . ? O8 Dy1 O5 N2 29.2(2) . . . . ? O7 Dy1 O5 N2 -29.71(19) . . . . ? O3 Dy1 O5 N2 127.20(18) . . . . ? O9 N3 O7 Dy1 -171.5(3) . . . . ? O8 N3 O7 Dy1 7.8(3) . . . . ? O11 Dy1 O7 N3 173.4(2) . . . . ? O12 Dy1 O7 N3 -146.6(2) 3_676 . . . ? O10 Dy1 O7 N3 19.1(2) . . . . ? O4 Dy1 O7 N3 81.0(2) . . . . ? O1 Dy1 O7 N3 -103.4(2) . . . . ? O8 Dy1 O7 N3 -4.61(19) . . . . ? O3 Dy1 O7 N3 -60.0(2) . . . . ? O5 Dy1 O7 N3 103.1(2) . . . . ? O9 N3 O8 Dy1 171.5(3) . . . . ? O7 N3 O8 Dy1 -7.8(3) . . . . ? O11 Dy1 O8 N3 2.1(2) . . . . ? O12 Dy1 O8 N3 149.19(19) 3_676 . . . ? O10 Dy1 O8 N3 -154.9(2) . . . . ? O4 Dy1 O8 N3 -72.2(2) . . . . ? O1 Dy1 O8 N3 78.6(2) . . . . ? O7 Dy1 O8 N3 4.56(18) . . . . ? O3 Dy1 O8 N3 129.3(2) . . . . ? O5 Dy1 O8 N3 -97.8(2) . . . . ? N7 C1 O10 Dy1 176.1(3) . . . . ? O11 Dy1 O10 C1 -174.6(3) . . . . ? O12 Dy1 O10 C1 121.0(3) 3_676 . . . ? O4 Dy1 O10 C1 -109.5(3) . . . . ? O1 Dy1 O10 C1 44.0(4) . . . . ? O8 Dy1 O10 C1 -32.9(3) . . . . ? O7 Dy1 O10 C1 -51.9(4) . . . . ? O3 Dy1 O10 C1 45.7(3) . . . . ? O5 Dy1 O10 C1 -162.4(3) . . . . ? N5 C3 O11 Dy1 -96(2) . . . . ? C4 C3 O11 Dy1 83(2) . . . . ? O12 Dy1 O11 C3 -28(2) 3_676 . . . ? O10 Dy1 O11 C3 -94(2) . . . . ? O4 Dy1 O11 C3 -157(2) . . . . ? O1 Dy1 O11 C3 54(2) . . . . ? O8 Dy1 O11 C3 135(2) . . . . ? O7 Dy1 O11 C3 133(2) . . . . ? O3 Dy1 O11 C3 34(2) . . . . ? O5 Dy1 O11 C3 -106(2) . . . . ? N6 C21 O12 Dy1 -80(7) . . . 3_676 ? C20 C21 O12 Dy1 100(7) . . . 3_676 ? C35 C8 O13 C9 -15.2(6) . . . . ? C4 C8 O13 C9 166.1(4) . . . . ? C10 C9 O13 C8 -95.6(7) . . . . ? C17 C15 O14 C14 -4.7(5) . . . . ? C20 C15 O14 C14 174.4(3) . . . . ? C13 C14 O14 C15 -169.5(3) . . . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.734 _refine_diff_density_min -0.778 _refine_diff_density_rms 0.090 data_788729 _database_code_depnum_ccdc_archive 'CCDC 788729' #TrackingRef '- cif_Revision.cif' __audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84 H92 N14 O28 Pr2' _chemical_formula_weight 2027.54 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' Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.7358(3) _cell_length_b 14.0425(3) _cell_length_c 19.7825(4) _cell_angle_alpha 90.00 _cell_angle_beta 101.8230(10) _cell_angle_gamma 90.00 _cell_volume 4550.50(16) _cell_formula_units_Z 2 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.480 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2072 _exptl_absorpt_coefficient_mu 1.143 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7255 _exptl_absorpt_correction_T_max 0.8564 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 23902 _diffrn_reflns_av_R_equivalents 0.0264 _diffrn_reflns_av_sigmaI/netI 0.0317 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 25.50 _reflns_number_total 8430 _reflns_number_gt 6685 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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 Following Model and Quality ALERTS were generated - (Acta-Mode) <<< #============================================================================== Format: alert-number_ALERT_alert-type_alert-level text PLAT241_ALERT_2_A Check High Ueq as Compared to Neighbors for C51 The larger than normal range of thermal motion is mostly due to the difference between the disordered ethyl group and the other atoms which are not disordered. ; _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^)+(0.0426P)^2^+2.8197P] 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 8430 _refine_ls_number_parameters 579 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0469 _refine_ls_R_factor_gt 0.0335 _refine_ls_wR_factor_ref 0.0882 _refine_ls_wR_factor_gt 0.0799 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pr1 Pr 0.727152(9) 0.777811(13) 0.231722(9) 0.03995(7) Uani 1 1 d . . . C1 C 0.68935(19) 0.5905(2) 0.10255(17) 0.0418(7) Uani 1 1 d . . . C2 C 0.61359(18) 0.5323(2) 0.09371(16) 0.0406(7) Uani 1 1 d . . . C3 C 0.55184(19) 0.5655(2) 0.12478(17) 0.0464(8) Uani 1 1 d . . . H3 H 0.5590 0.6229 0.1488 0.056 Uiso 1 1 calc R . . C4 C 0.60195(19) 0.4442(2) 0.05847(17) 0.0436(8) Uani 1 1 d . . . C5 C 0.5292(2) 0.3946(2) 0.05487(19) 0.0484(8) Uani 1 1 d . . . H5A H 0.5210 0.3372 0.0310 0.058 Uiso 1 1 calc R . . C7 C 0.6570(2) 0.3187(3) -0.0012(2) 0.0585(10) Uani 1 1 d . . . H7A H 0.6170 0.3195 -0.0443 0.070 Uiso 1 1 calc R . . H7B H 0.6398 0.2725 0.0294 0.070 Uiso 1 1 calc R . . C8 C 0.82191(19) 0.6185(3) 0.0697(2) 0.0573(10) Uani 1 1 d . . . H8A H 0.8215 0.6790 0.0932 0.069 Uiso 1 1 calc R . . H8B H 0.8324 0.6309 0.0241 0.069 Uiso 1 1 calc R . . C9 C 0.8896(2) 0.5564(3) 0.1097(2) 0.0619(11) Uani 1 1 d . . . C11 C 0.46814(18) 0.1512(2) -0.12957(17) 0.0423(7) Uani 1 1 d . . . C12 C 0.4768(2) 0.1445(2) -0.05295(18) 0.0497(9) Uani 1 1 d . . . C13 C 0.4102(3) 0.1735(3) -0.0257(2) 0.0656(11) Uani 1 1 d . . . H13 H 0.3637 0.1961 -0.0555 0.079 Uiso 1 1 calc R . . C17 C 0.5304(2) 0.1415(3) -0.2316(2) 0.0659(11) Uani 1 1 d . . . H17A H 0.4777 0.1647 -0.2558 0.079 Uiso 1 1 calc R . . H17B H 0.5373 0.0773 -0.2476 0.079 Uiso 1 1 calc R . . C18 C 0.4696(2) 0.4299(3) 0.08624(19) 0.0525(9) Uani 1 1 d . . . H18 H 0.4216 0.3957 0.0841 0.063 Uiso 1 1 calc R . . C19 C 0.4802(2) 0.5156(3) 0.12103(19) 0.0531(9) Uani 1 1 d . . . H19 H 0.4393 0.5395 0.1418 0.064 Uiso 1 1 calc R . . C20 C 0.8873(3) 0.5242(3) 0.1748(3) 0.0845(14) Uani 1 1 d . . . H20 H 0.8421 0.5373 0.1938 0.101 Uiso 1 1 calc R . . C21 C 0.9513(4) 0.4728(4) 0.2118(4) 0.117(2) Uani 1 1 d . . . H21 H 0.9488 0.4497 0.2553 0.141 Uiso 1 1 calc R . . C22 C 1.0194(4) 0.4555(5) 0.1843(5) 0.138(3) Uani 1 1 d . . . H22 H 1.0640 0.4238 0.2104 0.165 Uiso 1 1 calc R . . C23 C 1.0212(4) 0.4842(5) 0.1202(5) 0.134(3) Uani 1 1 d . . . H23 H 1.0660 0.4698 0.1011 0.161 Uiso 1 1 calc R . . C24 C 0.9570(3) 0.5350(4) 0.0825(3) 0.0961(17) Uani 1 1 d . . . H24 H 0.9591 0.5551 0.0381 0.115 Uiso 1 1 calc R . . C25 C 0.4115(4) 0.1696(4) 0.0440(3) 0.0929(16) Uani 1 1 d . . . H25 H 0.3665 0.1901 0.0608 0.112 Uiso 1 1 calc R . . C26 C 0.4785(5) 0.1359(4) 0.0881(3) 0.110(2) Uani 1 1 d . . . H26 H 0.4790 0.1330 0.1352 0.132 Uiso 1 1 calc R . . C27 C 0.5454(4) 0.1063(4) 0.0641(3) 0.0958(19) Uani 1 1 d . . . H27 H 0.5909 0.0834 0.0949 0.115 Uiso 1 1 calc R . . C28 C 0.9256(3) 0.7222(4) 0.2890(4) 0.108(2) Uani 1 1 d . . . H28 H 0.9134 0.7135 0.3324 0.129 Uiso 1 1 calc R . . C29 C 1.0332(5) 0.7233(5) 0.2246(4) 0.134(3) Uani 1 1 d . . . H29A H 0.9886 0.7325 0.1860 0.201 Uiso 1 1 calc R . . H29B H 1.0640 0.6683 0.2167 0.201 Uiso 1 1 calc R . . H29C H 1.0679 0.7784 0.2299 0.201 Uiso 1 1 calc R . . C31 C 0.6560(2) 0.1665(3) -0.2797(2) 0.0592(10) Uani 1 1 d . . . H31 H 0.6560 0.1016 -0.2893 0.071 Uiso 1 1 calc R . . C32 C 0.5966(2) 0.2044(3) -0.24877(18) 0.0528(9) Uani 1 1 d . . . C33 C 0.5977(3) 0.3007(3) -0.2354(2) 0.0725(12) Uani 1 1 d . . . H33 H 0.5572 0.3274 -0.2154 0.087 Uiso 1 1 calc R . . C34 C 0.7158(3) 0.2249(4) -0.2965(2) 0.0748(12) Uani 1 1 d . . . H34 H 0.7559 0.1991 -0.3173 0.090 Uiso 1 1 calc R . . C35 C 0.6574(3) 0.3575(3) -0.2513(2) 0.0809(13) Uani 1 1 d . . . H35 H 0.6581 0.4221 -0.2409 0.097 Uiso 1 1 calc R . . C36 C 0.7162(3) 0.3205(4) -0.2824(2) 0.0779(13) Uani 1 1 d . . . H36 H 0.7561 0.3597 -0.2940 0.093 Uiso 1 1 calc R . . C37 C 1.0624(5) 0.6887(6) 0.3465(4) 0.170(3) Uani 1 1 d . . . H37A H 1.0927 0.7453 0.3625 0.255 Uiso 1 1 calc R . . H37B H 1.0991 0.6404 0.3369 0.255 Uiso 1 1 calc R . . H37C H 1.0347 0.6663 0.3814 0.255 Uiso 1 1 calc R . . C46 C 0.5460(3) 0.1101(3) -0.0072(2) 0.0699(13) Uani 1 1 d . . . C48 C 0.7467(3) 0.1199(4) -0.0055(3) 0.115(2) Uani 1 1 d . . . H48A H 0.7833 0.0775 -0.0232 0.138 Uiso 1 1 calc R . . H48B H 0.7764 0.1418 0.0391 0.138 Uiso 1 1 calc R . . C49 C 0.7853(3) 0.1949(3) -0.1029(2) 0.0794(13) Uani 1 1 d . . . H49A H 0.7783 0.2536 -0.1293 0.095 Uiso 1 1 calc R . . H49B H 0.7632 0.1437 -0.1341 0.095 Uiso 1 1 calc R . . C50 C 0.7398(2) 0.2926(3) -0.0143(2) 0.0619(10) Uani 1 1 d . . . H50A H 0.7580 0.3415 -0.0423 0.074 Uiso 1 1 calc R . . H50B H 0.7788 0.2892 0.0293 0.074 Uiso 1 1 calc R . . C51 C 0.6895(3) 0.0677(5) 0.0070(4) 0.175(4) Uani 1 1 d . . . H51A H 0.6860 0.0774 0.0549 0.210 Uiso 1 1 calc R . . H51B H 0.7049 0.0018 0.0024 0.210 Uiso 1 1 calc R . . C52 C 0.8753(3) 0.1777(4) -0.0784(3) 0.0790(13) Uani 1 1 d . . . C53 C 0.9272(4) 0.2441(5) -0.0413(4) 0.1046(19) Uani 1 1 d . . . H53 H 0.9061 0.3022 -0.0307 0.126 Uiso 1 1 calc R . . C54 C 0.9114(4) 0.0949(4) -0.0924(4) 0.121(2) Uani 1 1 d . . . H54 H 0.8788 0.0476 -0.1169 0.145 Uiso 1 1 calc R . . C55 C 0.9934(5) 0.0783(6) -0.0719(5) 0.153(3) Uani 1 1 d . . . H55 H 1.0151 0.0211 -0.0835 0.183 Uiso 1 1 calc R . . C56 C 1.0434(5) 0.1439(7) -0.0351(5) 0.145(3) Uani 1 1 d . . . H56 H 1.0990 0.1322 -0.0211 0.174 Uiso 1 1 calc R . . C57 C 1.0107(4) 0.2266(6) -0.0191(4) 0.130(3) Uani 1 1 d . . . H57 H 1.0439 0.2722 0.0067 0.156 Uiso 1 1 calc R . . N1 N 0.79722(17) 0.9306(2) 0.1572(2) 0.0579(8) Uani 1 1 d . . . N2 N 0.6841(2) 0.6072(3) 0.30527(18) 0.0679(9) Uani 1 1 d . . . N3 N 0.7395(2) 0.8955(3) 0.35936(17) 0.0612(8) Uani 1 1 d . . . N4 N 1.00293(18) 0.7102(3) 0.2839(3) 0.0798(12) Uani 1 1 d . . . N5 N 0.74220(16) 0.5730(2) 0.06302(16) 0.0519(7) Uani 1 1 d . . . H5 H 0.7287 0.5315 0.0307 0.062 Uiso 1 1 calc R . . N6 N 0.73693(19) 0.2016(2) -0.04954(17) 0.0543(8) Uani 1 1 d . . . N7 N 0.53176(17) 0.1392(2) -0.15761(16) 0.0606(8) Uani 1 1 d . . . H7 H 0.5780 0.1290 -0.1303 0.073 Uiso 1 1 calc R . . O1 O 0.78251(18) 0.94283(18) 0.21653(16) 0.0679(7) Uani 1 1 d . . . O2 O 0.77575(16) 0.8524(2) 0.12780(14) 0.0668(7) Uani 1 1 d . . . O3 O 0.87045(15) 0.7431(2) 0.24326(16) 0.0660(8) Uani 1 1 d . . . O4 O 0.75669(18) 0.6230(2) 0.30000(17) 0.0808(9) Uani 1 1 d . . . O5 O 0.6650(2) 0.5335(2) 0.3296(2) 0.1055(12) Uani 1 1 d . . . O6 O 0.79459(16) 0.8362(2) 0.35336(14) 0.0701(8) Uani 1 1 d . . . O7 O 0.67544(15) 0.8941(2) 0.31300(14) 0.0645(7) Uani 1 1 d . . . O9 O 0.39981(13) 0.17015(19) -0.16630(12) 0.0541(6) Uani 1 1 d . . . O10 O 0.70204(14) 0.65568(17) 0.14638(13) 0.0555(6) Uani 1 1 d . . . O12 O 0.63293(16) 0.6726(2) 0.28419(15) 0.0666(7) Uani 1 1 d . . . O13 O 0.8311(2) 0.9917(2) 0.12945(18) 0.0920(10) Uani 1 1 d . . . O14 O 0.66374(14) 0.41134(16) 0.02986(14) 0.0554(6) Uani 1 1 d . . . O15 O 0.7479(2) 0.9524(3) 0.40683(17) 0.0988(11) Uani 1 1 d . . . O16 O 0.60903(17) 0.0816(2) -0.03515(18) 0.0921(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pr1 0.02946(10) 0.04631(12) 0.04304(12) -0.00304(9) 0.00501(7) -0.00140(7) C1 0.0397(17) 0.0397(17) 0.044(2) -0.0009(15) 0.0045(15) -0.0021(13) C2 0.0362(16) 0.0469(18) 0.0371(18) 0.0005(15) 0.0037(14) -0.0024(13) C3 0.0452(18) 0.0517(19) 0.042(2) -0.0073(16) 0.0071(15) -0.0041(15) C4 0.0381(17) 0.0488(19) 0.043(2) -0.0013(16) 0.0068(14) -0.0028(14) C5 0.0447(18) 0.0474(19) 0.053(2) -0.0045(17) 0.0090(16) -0.0071(15) C7 0.050(2) 0.050(2) 0.074(3) -0.015(2) 0.0084(19) -0.0023(17) C8 0.0396(18) 0.062(2) 0.073(3) -0.006(2) 0.0161(18) -0.0133(16) C9 0.047(2) 0.050(2) 0.088(3) -0.014(2) 0.013(2) -0.0021(17) C11 0.0367(17) 0.0412(17) 0.046(2) -0.0002(15) 0.0012(15) -0.0069(13) C12 0.054(2) 0.0485(19) 0.041(2) 0.0018(16) -0.0029(16) -0.0200(16) C13 0.082(3) 0.064(2) 0.052(2) -0.005(2) 0.016(2) -0.019(2) C17 0.044(2) 0.099(3) 0.055(3) -0.014(2) 0.0102(17) -0.006(2) C18 0.0410(18) 0.061(2) 0.056(2) 0.0002(19) 0.0099(17) -0.0109(16) C19 0.0397(18) 0.071(2) 0.051(2) -0.0048(19) 0.0141(16) -0.0010(17) C20 0.080(3) 0.071(3) 0.099(4) 0.006(3) 0.009(3) 0.013(2) C21 0.123(5) 0.083(4) 0.127(5) 0.014(4) -0.020(4) 0.010(4) C22 0.088(5) 0.081(4) 0.218(10) 0.005(5) -0.028(6) 0.023(3) C23 0.066(4) 0.113(5) 0.220(10) -0.001(6) 0.022(5) 0.032(3) C24 0.065(3) 0.094(4) 0.135(5) -0.012(3) 0.035(3) 0.011(3) C25 0.144(5) 0.090(3) 0.049(3) -0.006(3) 0.030(3) -0.037(3) C26 0.174(6) 0.100(4) 0.047(3) 0.002(3) 0.006(4) -0.061(5) C27 0.121(4) 0.081(3) 0.060(3) 0.028(3) -0.039(3) -0.053(3) C28 0.071(3) 0.086(4) 0.165(6) -0.022(4) 0.022(4) 0.000(3) C29 0.161(7) 0.131(6) 0.121(6) -0.027(4) 0.055(5) -0.045(5) C31 0.055(2) 0.070(2) 0.053(2) -0.009(2) 0.0131(18) -0.0007(19) C32 0.0446(19) 0.074(3) 0.037(2) -0.0066(18) 0.0009(15) 0.0003(17) C33 0.072(3) 0.075(3) 0.070(3) -0.013(2) 0.012(2) 0.013(2) C34 0.064(3) 0.103(4) 0.063(3) -0.002(3) 0.026(2) 0.001(2) C35 0.097(4) 0.065(3) 0.075(3) 0.002(2) 0.006(3) -0.003(3) C36 0.078(3) 0.086(3) 0.068(3) 0.014(3) 0.012(2) -0.017(3) C37 0.140(6) 0.221(9) 0.136(7) 0.053(6) 0.000(5) 0.054(6) C46 0.068(3) 0.063(2) 0.065(3) 0.020(2) -0.019(2) -0.037(2) C48 0.044(2) 0.104(4) 0.179(6) 0.090(4) -0.019(3) -0.005(2) C49 0.093(3) 0.086(3) 0.061(3) -0.011(2) 0.019(2) 0.029(3) C50 0.054(2) 0.064(2) 0.071(3) -0.018(2) 0.020(2) -0.0066(18) C51 0.050(3) 0.203(7) 0.232(8) 0.169(7) -0.068(4) -0.044(4) C52 0.085(3) 0.086(3) 0.075(3) 0.009(3) 0.036(3) 0.025(3) C53 0.084(4) 0.117(4) 0.127(5) 0.020(4) 0.054(4) 0.020(3) C54 0.119(5) 0.104(4) 0.156(6) 0.012(4) 0.068(4) 0.049(4) C55 0.124(6) 0.134(7) 0.223(10) 0.049(7) 0.090(7) 0.068(5) C56 0.089(5) 0.168(8) 0.197(9) 0.075(7) 0.073(6) 0.046(5) C57 0.074(4) 0.154(7) 0.172(7) 0.030(5) 0.049(4) -0.005(4) N1 0.0391(16) 0.060(2) 0.073(2) 0.0171(19) 0.0056(16) 0.0013(14) N2 0.088(3) 0.063(2) 0.057(2) 0.0057(18) 0.0244(19) -0.006(2) N3 0.057(2) 0.083(2) 0.0438(19) -0.0100(18) 0.0111(16) -0.0064(18) N4 0.0301(16) 0.073(2) 0.130(4) 0.003(2) 0.002(2) 0.0094(15) N5 0.0422(15) 0.0594(18) 0.0563(19) -0.0165(15) 0.0151(14) -0.0120(13) N6 0.0579(18) 0.0459(16) 0.057(2) 0.0036(14) 0.0076(15) 0.0057(13) N7 0.0369(15) 0.095(2) 0.0468(19) 0.0071(17) 0.0009(13) 0.0015(15) O1 0.0805(19) 0.0531(15) 0.073(2) -0.0039(15) 0.0231(16) -0.0056(14) O2 0.0628(16) 0.079(2) 0.0604(18) -0.0031(15) 0.0176(13) -0.0151(15) O3 0.0314(13) 0.0789(18) 0.083(2) -0.0051(15) 0.0000(14) 0.0073(12) O4 0.0642(18) 0.0752(19) 0.100(2) 0.0259(18) 0.0092(17) 0.0065(15) O5 0.141(3) 0.069(2) 0.118(3) 0.028(2) 0.053(3) -0.014(2) O6 0.0555(15) 0.093(2) 0.0562(17) -0.0070(16) -0.0010(13) 0.0150(15) O7 0.0449(14) 0.090(2) 0.0573(17) -0.0199(15) 0.0078(13) 0.0058(13) O9 0.0368(12) 0.0785(17) 0.0438(14) 0.0006(13) 0.0008(10) 0.0074(12) O10 0.0479(13) 0.0544(14) 0.0651(17) -0.0194(13) 0.0136(12) -0.0092(11) O12 0.0623(16) 0.0733(18) 0.0698(19) 0.0095(16) 0.0269(14) -0.0001(15) O13 0.084(2) 0.089(2) 0.104(3) 0.041(2) 0.0201(19) -0.0173(18) O14 0.0495(13) 0.0496(14) 0.0712(17) -0.0191(13) 0.0220(12) -0.0100(11) O15 0.102(2) 0.131(3) 0.063(2) -0.047(2) 0.0140(18) -0.004(2) O16 0.0437(15) 0.117(3) 0.100(3) 0.055(2) -0.0216(16) -0.0150(16) _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 Pr1 O9 2.366(2) 3_665 ? Pr1 O10 2.383(2) . ? Pr1 O3 2.412(2) . ? Pr1 O12 2.533(3) . ? Pr1 O1 2.536(3) . ? Pr1 O4 2.553(3) . ? Pr1 O7 2.563(3) . ? Pr1 O6 2.574(3) . ? Pr1 O2 2.582(3) . ? C1 O10 1.249(4) . ? C1 N5 1.318(4) . ? C1 C2 1.488(4) . ? C2 C3 1.387(4) . ? C2 C4 1.413(4) . ? C3 C19 1.377(4) . ? C3 H3 0.9300 . ? C4 O14 1.357(4) . ? C4 C5 1.391(4) . ? C5 C18 1.370(5) . ? C5 H5A 0.9300 . ? C7 O14 1.434(4) . ? C7 C50 1.507(5) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 N5 1.461(4) . ? C8 C9 1.518(5) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C20 1.372(7) . ? C9 C24 1.379(6) . ? C11 O9 1.251(4) . ? C11 N7 1.308(4) . ? C11 C12 1.496(5) . ? C12 C13 1.396(5) . ? C12 C46 1.401(5) . ? C13 C25 1.375(6) . ? C13 H13 0.9300 . ? C17 N7 1.460(5) . ? C17 C32 1.509(5) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.380(5) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 C21 1.372(7) . ? C20 H20 0.9300 . ? C21 C22 1.381(10) . ? C21 H21 0.9300 . ? C22 C23 1.336(10) . ? C22 H22 0.9300 . ? C23 C24 1.375(8) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 C26 1.358(8) . ? C25 H25 0.9300 . ? C26 C27 1.368(8) . ? C26 H26 0.9300 . ? C27 C46 1.413(7) . ? C27 H27 0.9300 . ? C28 O3 1.189(7) . ? C28 N4 1.330(6) . ? C28 H28 0.9300 . ? C29 N4 1.382(7) . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C31 C32 1.377(5) . ? C31 C34 1.385(6) . ? C31 H31 0.9300 . ? C32 C33 1.378(5) . ? C33 C35 1.365(6) . ? C33 H33 0.9300 . ? C34 C36 1.371(7) . ? C34 H34 0.9300 . ? C35 C36 1.365(6) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C37 N4 1.452(8) . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C46 O16 1.348(6) . ? C48 C51 1.269(6) . ? C48 N6 1.430(5) . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C49 N6 1.459(5) . ? C49 C52 1.505(7) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 N6 1.451(5) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C51 O16 1.445(5) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C52 C54 1.364(7) . ? C52 C53 1.379(8) . ? C53 C57 1.398(8) . ? C53 H53 0.9300 . ? C54 C55 1.370(9) . ? C54 H54 0.9300 . ? C55 C56 1.351(11) . ? C55 H55 0.9300 . ? C56 C57 1.348(10) . ? C56 H56 0.9300 . ? C57 H57 0.9300 . ? N1 O13 1.220(4) . ? N1 O1 1.259(4) . ? N1 O2 1.261(4) . ? N2 O5 1.212(4) . ? N2 O4 1.260(4) . ? N2 O12 1.267(4) . ? N3 O15 1.219(4) . ? N3 O7 1.260(4) . ? N3 O6 1.266(4) . ? N5 H5 0.8600 . ? N7 H7 0.8600 . ? O9 Pr1 2.366(2) 3_665 ? 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 Pr1 O10 80.00(9) 3_665 . ? O9 Pr1 O3 151.45(10) 3_665 . ? O10 Pr1 O3 87.10(9) . . ? O9 Pr1 O12 80.77(9) 3_665 . ? O10 Pr1 O12 80.58(9) . . ? O3 Pr1 O12 122.27(10) . . ? O9 Pr1 O1 87.82(9) 3_665 . ? O10 Pr1 O1 126.11(9) . . ? O3 Pr1 O1 79.36(10) . . ? O12 Pr1 O1 148.71(9) . . ? O9 Pr1 O4 127.38(9) 3_665 . ? O10 Pr1 O4 75.46(10) . . ? O3 Pr1 O4 72.36(10) . . ? O12 Pr1 O4 49.92(9) . . ? O1 Pr1 O4 143.57(10) . . ? O9 Pr1 O7 76.44(8) 3_665 . ? O10 Pr1 O7 150.42(8) . . ? O3 Pr1 O7 121.76(9) . . ? O12 Pr1 O7 78.22(9) . . ? O1 Pr1 O7 70.78(9) . . ? O4 Pr1 O7 105.32(11) . . ? O9 Pr1 O6 125.86(9) 3_665 . ? O10 Pr1 O6 150.66(9) . . ? O3 Pr1 O6 74.86(10) . . ? O12 Pr1 O6 89.61(9) . . ? O1 Pr1 O6 73.67(10) . . ? O4 Pr1 O6 77.08(10) . . ? O7 Pr1 O6 49.48(8) . . ? O9 Pr1 O2 80.41(8) 3_665 . ? O10 Pr1 O2 76.48(9) . . ? O3 Pr1 O2 71.82(10) . . ? O12 Pr1 O2 152.45(9) . . ? O1 Pr1 O2 49.69(9) . . ? O4 Pr1 O2 135.05(10) . . ? O7 Pr1 O2 116.30(10) . . ? O6 Pr1 O2 117.77(9) . . ? O10 C1 N5 120.6(3) . . ? O10 C1 C2 120.3(3) . . ? N5 C1 C2 119.1(3) . . ? C3 C2 C4 118.2(3) . . ? C3 C2 C1 117.2(3) . . ? C4 C2 C1 124.5(3) . . ? C19 C3 C2 121.6(3) . . ? C19 C3 H3 119.2 . . ? C2 C3 H3 119.2 . . ? O14 C4 C5 122.8(3) . . ? O14 C4 C2 117.6(3) . . ? C5 C4 C2 119.6(3) . . ? C18 C5 C4 120.4(3) . . ? C18 C5 H5A 119.8 . . ? C4 C5 H5A 119.8 . . ? O14 C7 C50 107.5(3) . . ? O14 C7 H7A 110.2 . . ? C50 C7 H7A 110.2 . . ? O14 C7 H7B 110.2 . . ? C50 C7 H7B 110.2 . . ? H7A C7 H7B 108.5 . . ? N5 C8 C9 111.5(3) . . ? N5 C8 H8A 109.3 . . ? C9 C8 H8A 109.3 . . ? N5 C8 H8B 109.3 . . ? C9 C8 H8B 109.3 . . ? H8A C8 H8B 108.0 . . ? C20 C9 C24 118.6(5) . . ? C20 C9 C8 121.1(4) . . ? C24 C9 C8 120.3(5) . . ? O9 C11 N7 120.5(3) . . ? O9 C11 C12 119.3(3) . . ? N7 C11 C12 120.2(3) . . ? C13 C12 C46 118.2(4) . . ? C13 C12 C11 116.9(3) . . ? C46 C12 C11 124.9(4) . . ? C25 C13 C12 121.7(5) . . ? C25 C13 H13 119.2 . . ? C12 C13 H13 119.2 . . ? N7 C17 C32 112.2(3) . . ? N7 C17 H17A 109.2 . . ? C32 C17 H17A 109.2 . . ? N7 C17 H17B 109.2 . . ? C32 C17 H17B 109.2 . . ? H17A C17 H17B 107.9 . . ? C5 C18 C19 120.7(3) . . ? C5 C18 H18 119.7 . . ? C19 C18 H18 119.7 . . ? C3 C19 C18 119.4(3) . . ? C3 C19 H19 120.3 . . ? C18 C19 H19 120.3 . . ? C9 C20 C21 120.3(6) . . ? C9 C20 H20 119.9 . . ? C21 C20 H20 119.9 . . ? C20 C21 C22 120.0(7) . . ? C20 C21 H21 120.0 . . ? C22 C21 H21 120.0 . . ? C23 C22 C21 120.1(6) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C22 C23 C24 120.3(7) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? C23 C24 C9 120.7(7) . . ? C23 C24 H24 119.6 . . ? C9 C24 H24 119.6 . . ? C26 C25 C13 120.0(6) . . ? C26 C25 H25 120.0 . . ? C13 C25 H25 120.0 . . ? C25 C26 C27 120.6(5) . . ? C25 C26 H26 119.7 . . ? C27 C26 H26 119.7 . . ? C26 C27 C46 120.6(5) . . ? C26 C27 H27 119.7 . . ? C46 C27 H27 119.7 . . ? O3 C28 N4 126.1(7) . . ? O3 C28 H28 117.0 . . ? N4 C28 H28 117.0 . . ? N4 C29 H29A 109.5 . . ? N4 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? N4 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C32 C31 C34 120.0(4) . . ? C32 C31 H31 120.0 . . ? C34 C31 H31 120.0 . . ? C31 C32 C33 118.8(4) . . ? C31 C32 C17 120.3(4) . . ? C33 C32 C17 120.9(4) . . ? C35 C33 C32 120.7(4) . . ? C35 C33 H33 119.6 . . ? C32 C33 H33 119.6 . . ? C36 C34 C31 120.3(4) . . ? C36 C34 H34 119.8 . . ? C31 C34 H34 119.8 . . ? C36 C35 C33 120.7(5) . . ? C36 C35 H35 119.6 . . ? C33 C35 H35 119.6 . . ? C35 C36 C34 119.4(4) . . ? C35 C36 H36 120.3 . . ? C34 C36 H36 120.3 . . ? N4 C37 H37A 109.5 . . ? N4 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? N4 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? O16 C46 C12 116.8(4) . . ? O16 C46 C27 124.3(4) . . ? C12 C46 C27 118.9(5) . . ? C51 C48 N6 125.9(4) . . ? C51 C48 H48A 105.9 . . ? N6 C48 H48A 105.9 . . ? C51 C48 H48B 105.9 . . ? N6 C48 H48B 105.9 . . ? H48A C48 H48B 106.2 . . ? N6 C49 C52 116.4(4) . . ? N6 C49 H49A 108.2 . . ? C52 C49 H49A 108.2 . . ? N6 C49 H49B 108.2 . . ? C52 C49 H49B 108.2 . . ? H49A C49 H49B 107.3 . . ? N6 C50 C7 110.8(3) . . ? N6 C50 H50A 109.5 . . ? C7 C50 H50A 109.5 . . ? N6 C50 H50B 109.5 . . ? C7 C50 H50B 109.5 . . ? H50A C50 H50B 108.1 . . ? C48 C51 O16 117.4(4) . . ? C48 C51 H51A 108.0 . . ? O16 C51 H51A 108.0 . . ? C48 C51 H51B 108.0 . . ? O16 C51 H51B 108.0 . . ? H51A C51 H51B 107.2 . . ? C54 C52 C53 115.4(5) . . ? C54 C52 C49 121.8(6) . . ? C53 C52 C49 122.8(4) . . ? C52 C53 C57 121.8(6) . . ? C52 C53 H53 119.1 . . ? C57 C53 H53 119.1 . . ? C52 C54 C55 122.9(8) . . ? C52 C54 H54 118.6 . . ? C55 C54 H54 118.6 . . ? C56 C55 C54 121.0(8) . . ? C56 C55 H55 119.5 . . ? C54 C55 H55 119.5 . . ? C57 C56 C55 118.5(7) . . ? C57 C56 H56 120.8 . . ? C55 C56 H56 120.8 . . ? C56 C57 C53 120.4(8) . . ? C56 C57 H57 119.8 . . ? C53 C57 H57 119.8 . . ? O13 N1 O1 121.4(4) . . ? O13 N1 O2 121.3(4) . . ? O1 N1 O2 117.2(3) . . ? O5 N2 O4 121.3(4) . . ? O5 N2 O12 122.3(4) . . ? O4 N2 O12 116.3(3) . . ? O15 N3 O7 121.2(4) . . ? O15 N3 O6 122.1(3) . . ? O7 N3 O6 116.7(3) . . ? C28 N4 C29 125.4(6) . . ? C28 N4 C37 118.0(6) . . ? C29 N4 C37 116.4(5) . . ? C1 N5 C8 125.2(3) . . ? C1 N5 H5 117.4 . . ? C8 N5 H5 117.4 . . ? C48 N6 C50 115.2(4) . . ? C48 N6 C49 112.2(4) . . ? C50 N6 C49 115.8(3) . . ? C11 N7 C17 125.1(3) . . ? C11 N7 H7 117.4 . . ? C17 N7 H7 117.4 . . ? N1 O1 Pr1 97.6(2) . . ? N1 O2 Pr1 95.3(2) . . ? C28 O3 Pr1 136.3(4) . . ? N2 O4 Pr1 96.2(2) . . ? N3 O6 Pr1 96.2(2) . . ? N3 O7 Pr1 96.9(2) . . ? C11 O9 Pr1 174.1(2) . 3_665 ? C1 O10 Pr1 178.9(2) . . ? N2 O12 Pr1 97.0(2) . . ? C4 O14 C7 119.2(3) . . ? C46 O16 C51 121.3(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O10 C1 C2 C3 13.0(5) . . . . ? N5 C1 C2 C3 -166.2(3) . . . . ? O10 C1 C2 C4 -164.3(3) . . . . ? N5 C1 C2 C4 16.5(5) . . . . ? C4 C2 C3 C19 -1.0(5) . . . . ? C1 C2 C3 C19 -178.4(3) . . . . ? C3 C2 C4 O14 -178.3(3) . . . . ? C1 C2 C4 O14 -1.1(5) . . . . ? C3 C2 C4 C5 1.1(5) . . . . ? C1 C2 C4 C5 178.4(3) . . . . ? O14 C4 C5 C18 178.3(3) . . . . ? C2 C4 C5 C18 -1.1(5) . . . . ? N5 C8 C9 C20 -55.6(5) . . . . ? N5 C8 C9 C24 127.5(4) . . . . ? O9 C11 C12 C13 -9.2(5) . . . . ? N7 C11 C12 C13 169.6(3) . . . . ? O9 C11 C12 C46 169.9(3) . . . . ? N7 C11 C12 C46 -11.3(5) . . . . ? C46 C12 C13 C25 0.4(6) . . . . ? C11 C12 C13 C25 179.5(4) . . . . ? C4 C5 C18 C19 0.9(6) . . . . ? C2 C3 C19 C18 0.8(5) . . . . ? C5 C18 C19 C3 -0.7(6) . . . . ? C24 C9 C20 C21 0.8(7) . . . . ? C8 C9 C20 C21 -176.2(4) . . . . ? C9 C20 C21 C22 1.7(9) . . . . ? C20 C21 C22 C23 -3.6(11) . . . . ? C21 C22 C23 C24 3.0(12) . . . . ? C22 C23 C24 C9 -0.5(11) . . . . ? C20 C9 C24 C23 -1.4(8) . . . . ? C8 C9 C24 C23 175.6(5) . . . . ? C12 C13 C25 C26 -0.7(7) . . . . ? C13 C25 C26 C27 0.5(8) . . . . ? C25 C26 C27 C46 -0.1(8) . . . . ? C34 C31 C32 C33 0.4(6) . . . . ? C34 C31 C32 C17 178.8(4) . . . . ? N7 C17 C32 C31 118.5(4) . . . . ? N7 C17 C32 C33 -63.0(5) . . . . ? C31 C32 C33 C35 -1.2(6) . . . . ? C17 C32 C33 C35 -179.7(4) . . . . ? C32 C31 C34 C36 0.0(7) . . . . ? C32 C33 C35 C36 1.7(7) . . . . ? C33 C35 C36 C34 -1.3(7) . . . . ? C31 C34 C36 C35 0.5(7) . . . . ? C13 C12 C46 O16 179.3(3) . . . . ? C11 C12 C46 O16 0.3(5) . . . . ? C13 C12 C46 C27 0.0(5) . . . . ? C11 C12 C46 C27 -179.0(3) . . . . ? C26 C27 C46 O16 -179.4(4) . . . . ? C26 C27 C46 C12 -0.2(7) . . . . ? O14 C7 C50 N6 -176.7(3) . . . . ? N6 C48 C51 O16 11.0(13) . . . . ? N6 C49 C52 C54 113.3(5) . . . . ? N6 C49 C52 C53 -67.5(7) . . . . ? C54 C52 C53 C57 -0.7(9) . . . . ? C49 C52 C53 C57 -179.9(5) . . . . ? C53 C52 C54 C55 -0.7(9) . . . . ? C49 C52 C54 C55 178.6(6) . . . . ? C52 C54 C55 C56 1.2(13) . . . . ? C54 C55 C56 C57 -0.3(14) . . . . ? C55 C56 C57 C53 -1.0(12) . . . . ? C52 C53 C57 C56 1.5(11) . . . . ? O3 C28 N4 C29 2.5(8) . . . . ? O3 C28 N4 C37 177.3(6) . . . . ? O10 C1 N5 C8 6.3(5) . . . . ? C2 C1 N5 C8 -174.5(3) . . . . ? C9 C8 N5 C1 98.1(4) . . . . ? C51 C48 N6 C50 99.3(9) . . . . ? C51 C48 N6 C49 -125.4(8) . . . . ? C7 C50 N6 C48 -85.5(4) . . . . ? C7 C50 N6 C49 140.8(4) . . . . ? C52 C49 N6 C48 -55.0(6) . . . . ? C52 C49 N6 C50 80.0(5) . . . . ? O9 C11 N7 C17 -3.0(6) . . . . ? C12 C11 N7 C17 178.2(4) . . . . ? C32 C17 N7 C11 131.4(4) . . . . ? O13 N1 O1 Pr1 -174.9(3) . . . . ? O2 N1 O1 Pr1 4.9(3) . . . . ? O9 Pr1 O1 N1 -82.0(2) 3_665 . . . ? O10 Pr1 O1 N1 -6.1(2) . . . . ? O3 Pr1 O1 N1 72.3(2) . . . . ? O12 Pr1 O1 N1 -150.2(2) . . . . ? O4 Pr1 O1 N1 111.7(2) . . . . ? O7 Pr1 O1 N1 -158.4(2) . . . . ? O6 Pr1 O1 N1 149.5(2) . . . . ? O2 Pr1 O1 N1 -2.76(18) . . . . ? O13 N1 O2 Pr1 175.0(3) . . . . ? O1 N1 O2 Pr1 -4.7(3) . . . . ? O9 Pr1 O2 N1 98.1(2) 3_665 . . . ? O10 Pr1 O2 N1 180.0(2) . . . . ? O3 Pr1 O2 N1 -88.6(2) . . . . ? O12 Pr1 O2 N1 145.6(2) . . . . ? O1 Pr1 O2 N1 2.75(18) . . . . ? O4 Pr1 O2 N1 -127.3(2) . . . . ? O7 Pr1 O2 N1 28.5(2) . . . . ? O6 Pr1 O2 N1 -27.5(2) . . . . ? N4 C28 O3 Pr1 -176.7(3) . . . . ? O9 Pr1 O3 C28 172.2(4) 3_665 . . . ? O10 Pr1 O3 C28 -124.9(5) . . . . ? O12 Pr1 O3 C28 -48.0(5) . . . . ? O1 Pr1 O3 C28 107.5(5) . . . . ? O4 Pr1 O3 C28 -49.3(5) . . . . ? O7 Pr1 O3 C28 48.1(5) . . . . ? O6 Pr1 O3 C28 31.7(5) . . . . ? O2 Pr1 O3 C28 158.3(5) . . . . ? O5 N2 O4 Pr1 173.2(4) . . . . ? O12 N2 O4 Pr1 -7.3(4) . . . . ? O9 Pr1 O4 N2 -20.7(3) 3_665 . . . ? O10 Pr1 O4 N2 -85.6(2) . . . . ? O3 Pr1 O4 N2 -177.2(3) . . . . ? O12 Pr1 O4 N2 4.3(2) . . . . ? O1 Pr1 O4 N2 142.0(2) . . . . ? O7 Pr1 O4 N2 63.8(3) . . . . ? O6 Pr1 O4 N2 104.9(3) . . . . ? O2 Pr1 O4 N2 -138.6(2) . . . . ? O15 N3 O6 Pr1 -170.6(3) . . . . ? O7 N3 O6 Pr1 8.2(3) . . . . ? O9 Pr1 O6 N3 -1.2(3) 3_665 . . . ? O10 Pr1 O6 N3 -149.3(2) . . . . ? O3 Pr1 O6 N3 156.8(2) . . . . ? O12 Pr1 O6 N3 -79.5(2) . . . . ? O1 Pr1 O6 N3 73.7(2) . . . . ? O4 Pr1 O6 N3 -128.3(2) . . . . ? O7 Pr1 O6 N3 -4.7(2) . . . . ? O2 Pr1 O6 N3 97.3(2) . . . . ? O15 N3 O7 Pr1 170.6(3) . . . . ? O6 N3 O7 Pr1 -8.3(3) . . . . ? O9 Pr1 O7 N3 -172.3(2) 3_665 . . . ? O10 Pr1 O7 N3 149.6(2) . . . . ? O3 Pr1 O7 N3 -16.3(3) . . . . ? O12 Pr1 O7 N3 104.5(2) . . . . ? O1 Pr1 O7 N3 -79.9(2) . . . . ? O4 Pr1 O7 N3 62.1(2) . . . . ? O6 Pr1 O7 N3 4.8(2) . . . . ? O2 Pr1 O7 N3 -100.4(2) . . . . ? N7 C11 O9 Pr1 -104(2) . . . 3_665 ? C12 C11 O9 Pr1 75(2) . . . 3_665 ? N5 C1 O10 Pr1 -100(11) . . . . ? C2 C1 O10 Pr1 81(11) . . . . ? O9 Pr1 O10 C1 -138(11) 3_665 . . . ? O3 Pr1 O10 C1 68(11) . . . . ? O12 Pr1 O10 C1 -55(11) . . . . ? O1 Pr1 O10 C1 143(11) . . . . ? O4 Pr1 O10 C1 -5(11) . . . . ? O7 Pr1 O10 C1 -100(11) . . . . ? O6 Pr1 O10 C1 17(11) . . . . ? O2 Pr1 O10 C1 140(11) . . . . ? O5 N2 O12 Pr1 -173.1(4) . . . . ? O4 N2 O12 Pr1 7.3(4) . . . . ? O9 Pr1 O12 N2 155.9(2) 3_665 . . . ? O10 Pr1 O12 N2 74.6(2) . . . . ? O3 Pr1 O12 N2 -5.8(3) . . . . ? O1 Pr1 O12 N2 -134.0(2) . . . . ? O4 Pr1 O12 N2 -4.2(2) . . . . ? O7 Pr1 O12 N2 -126.1(2) . . . . ? O6 Pr1 O12 N2 -77.6(2) . . . . ? O2 Pr1 O12 N2 108.5(3) . . . . ? C5 C4 O14 C7 -4.6(5) . . . . ? C2 C4 O14 C7 174.8(3) . . . . ? C50 C7 O14 C4 -167.9(3) . . . . ? C12 C46 O16 C51 164.3(4) . . . . ? C27 C46 O16 C51 -16.4(6) . . . . ? C48 C51 O16 C46 -117.8(8) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.296 _refine_diff_density_min -0.753 _refine_diff_density_rms 0.062 #===END data_852907 _database_code_depnum_ccdc_archive 'CCDC 852907' #TrackingRef '- cif_Revision.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C59 H51 N12 Nd O26' _chemical_formula_weight 1488.36 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' Nd Nd -0.1943 3.0179 '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 13.6963(9) _cell_length_b 15.9834(14) _cell_length_c 17.5498(12) _cell_angle_alpha 96.547(2) _cell_angle_beta 109.7240(10) _cell_angle_gamma 114.2660(10) _cell_volume 3150.7(4) _cell_formula_units_Z 2 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.569 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1514 _exptl_absorpt_coefficient_mu 0.920 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7959 _exptl_absorpt_correction_T_max 0.8094 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 16585 _diffrn_reflns_av_R_equivalents 0.0361 _diffrn_reflns_av_sigmaI/netI 0.0909 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 25.50 _reflns_number_total 11545 _reflns_number_gt 6986 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0543P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11545 _refine_ls_number_parameters 888 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1047 _refine_ls_R_factor_gt 0.0580 _refine_ls_wR_factor_ref 0.1397 _refine_ls_wR_factor_gt 0.1147 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _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 C2 C 0.7463(5) 1.3667(4) 0.6614(4) 0.0555(15) Uani 1 1 d . . . C3 C 0.5613(6) 1.2247(5) 0.6249(6) 0.087(2) Uani 1 1 d . . . H3 H 0.5156 1.1719 0.6380 0.105 Uiso 1 1 calc R . . C4 C 0.5773(9) 1.3199(7) 0.5297(6) 0.122(4) Uani 1 1 d . . . H4 H 0.5436 1.3312 0.4790 0.147 Uiso 1 1 calc R . . C5 C 0.5130(8) 1.2427(7) 0.5504(7) 0.120(4) Uani 1 1 d . . . H5 H 0.4344 1.2012 0.5132 0.144 Uiso 1 1 calc R . . C6 C 0.6928(7) 1.3803(5) 0.5854(4) 0.086(2) Uani 1 1 d . . . H6 H 0.7371 1.4328 0.5713 0.104 Uiso 1 1 calc R . . C7 C 1.1841(5) 1.0425(4) 0.6366(4) 0.0599(16) Uani 1 1 d . . . H7 H 1.2556 1.0837 0.6364 0.072 Uiso 1 1 calc R . . C8 C 1.1711(5) 0.9621(4) 0.6605(4) 0.0548(15) Uani 1 1 d . . . C9 C 0.9726(5) 0.9214(4) 0.6364(4) 0.0518(14) Uani 1 1 d . . . C10 C 1.0649(5) 0.8941(4) 0.6624(3) 0.0523(14) Uani 1 1 d . . . C11 C 1.0923(6) 1.0632(4) 0.6127(4) 0.0651(17) Uani 1 1 d . . . C12 C 0.9853(5) 1.0022(4) 0.6116(4) 0.0608(16) Uani 1 1 d . . . H12 H 0.9227 1.0157 0.5944 0.073 Uiso 1 1 calc R . . C13 C 1.2081(6) 0.9577(5) 0.8793(4) 0.080(2) Uani 1 1 d . . . H13 H 1.1959 0.8956 0.8772 0.097 Uiso 1 1 calc R . . C14 C 1.3168(7) 1.0268(7) 0.8894(5) 0.104(3) Uani 1 1 d . . . H14 H 1.3786 1.0134 0.8963 0.125 Uiso 1 1 calc R . . C15 C 1.2468(8) 1.1418(5) 0.8847(5) 0.098(3) Uani 1 1 d . . . H15 H 1.2612 1.2042 0.8859 0.117 Uiso 1 1 calc R . . C16 C 1.1358(7) 1.0694(6) 0.8783(4) 0.087(2) Uani 1 1 d . . . C17 C 1.3294(8) 1.1139(7) 0.8887(5) 0.108(3) Uani 1 1 d . . . H17 H 1.4007 1.1595 0.8912 0.129 Uiso 1 1 calc R . . C18 C 1.1159(5) 0.9771(4) 0.8723(4) 0.0655(17) Uani 1 1 d . . . C19 C 1.2570(5) 0.6791(4) 0.7528(4) 0.0501(14) Uani 1 1 d . . . C20 C 1.3497(5) 0.6605(4) 0.7623(4) 0.0579(16) Uani 1 1 d . . . H20 H 1.3610 0.6411 0.7154 0.070 Uiso 1 1 calc R . . C21 C 1.4247(5) 0.6711(4) 0.8420(4) 0.0594(16) Uani 1 1 d . . . C22 C 1.2361(5) 0.7093(4) 0.8213(4) 0.0487(14) Uani 1 1 d . . . C23 C 1.3217(5) 0.7219(4) 0.9021(4) 0.0578(16) Uani 1 1 d . . . C24 C 1.4133(5) 0.7030(4) 0.9138(4) 0.0659(17) Uani 1 1 d . . . H24 H 1.4659 0.7111 0.9676 0.079 Uiso 1 1 calc R . . C25 C 0.5810(5) 0.4861(4) 0.6924(4) 0.0559(15) Uani 1 1 d . . . C26 C 0.6826(5) 0.4460(4) 0.8373(4) 0.0555(15) Uani 1 1 d . . . H26 H 0.7157 0.4324 0.8868 0.067 Uiso 1 1 calc R . . C27 C 0.5140(5) 0.4096(4) 0.7121(4) 0.0593(16) Uani 1 1 d . . . H27 H 0.4338 0.3712 0.6771 0.071 Uiso 1 1 calc R . . C28 C 0.7508(5) 0.5224(4) 0.8175(4) 0.0501(14) Uani 1 1 d . . . C29 C 0.7062(5) 0.5477(4) 0.7419(4) 0.0515(14) Uani 1 1 d . . . C30 C 0.5654(5) 0.3895(4) 0.7839(4) 0.0570(16) Uani 1 1 d . . . C32 C 0.8551(6) 1.1908(5) 0.6499(5) 0.077(2) Uani 1 1 d . . . H32 H 0.9246 1.2379 0.6950 0.092 Uiso 1 1 calc R . . C33 C 0.8239(9) 1.2074(7) 0.5715(7) 0.102(3) Uani 1 1 d . . . H33 H 0.8719 1.2645 0.5646 0.123 Uiso 1 1 calc R . . C34 C 0.6869(6) 1.0395(5) 0.5956(5) 0.087(2) Uani 1 1 d . . . H34 H 0.6395 0.9824 0.6028 0.105 Uiso 1 1 calc R . . C35 C 0.7228(11) 1.1398(9) 0.5051(6) 0.112(3) Uani 1 1 d . . . H35 H 0.6994 1.1504 0.4525 0.135 Uiso 1 1 calc R . . C36 C 0.6555(8) 1.0548(8) 0.5171(6) 0.114(3) Uani 1 1 d . . . H36 H 0.5876 1.0069 0.4714 0.136 Uiso 1 1 calc R . . C37 C 1.1449(5) 1.4546(4) 0.8438(4) 0.0567(15) Uani 1 1 d . . . C38 C 1.2278(6) 1.4649(5) 0.9194(5) 0.087(2) Uani 1 1 d . . . H38 H 1.2239 1.4866 0.9692 0.104 Uiso 1 1 calc R . . C39 C 1.1510(6) 1.4218(5) 0.7717(5) 0.085(2) Uani 1 1 d . . . H39 H 1.0957 1.4146 0.7194 0.103 Uiso 1 1 calc R . . C40 C 1.3224(9) 1.4113(7) 0.8525(10) 0.137(5) Uani 1 1 d . . . H40 H 1.3824 1.3968 0.8550 0.165 Uiso 1 1 calc R . . C41 C 1.3169(8) 1.4441(7) 0.9239(7) 0.117(3) Uani 1 1 d . . . H41 H 1.3733 1.4527 0.9762 0.141 Uiso 1 1 calc R . . C42 C 1.2390(9) 1.3993(7) 0.7760(7) 0.128(4) Uani 1 1 d . . . H42 H 1.2419 1.3757 0.7263 0.153 Uiso 1 1 calc R . . C43 C 1.0525(5) 1.4845(5) 0.8432(4) 0.0725(19) Uani 1 1 d . . . H43A H 1.0516 1.4915 0.8986 0.087 Uiso 1 1 calc R . . H43B H 1.0746 1.5466 0.8328 0.087 Uiso 1 1 calc R . . C46 C 1.0037(5) 0.8926(5) 0.8566(4) 0.0636(17) Uani 1 1 d . . . C47 C 1.0675(8) 1.1851(5) 0.8903(6) 0.123(3) Uani 1 1 d . . . H47A H 1.0769 1.2082 0.8431 0.148 Uiso 1 1 calc R . . H47B H 1.1395 1.2259 0.9412 0.148 Uiso 1 1 calc R . . C48 C 0.9660(9) 1.1882(6) 0.8998(5) 0.115(3) Uani 1 1 d . . . H48A H 0.9948 1.2487 0.9407 0.138 Uiso 1 1 calc R . . H48B H 0.9315 1.1371 0.9227 0.138 Uiso 1 1 calc R . . C50 C 0.8017(6) 0.8233(5) 0.8499(6) 0.109(3) Uani 1 1 d . . . H50A H 0.7812 0.7700 0.8043 0.131 Uiso 1 1 calc R . . H50B H 0.8080 0.8023 0.9002 0.131 Uiso 1 1 calc R . . C51 C 0.7073(6) 0.8511(4) 0.8268(5) 0.0657(17) Uani 1 1 d . . . C52 C 0.6296(9) 0.8271(6) 0.7436(6) 0.113(3) Uani 1 1 d . . . H52 H 0.6353 0.7927 0.7004 0.135 Uiso 1 1 calc R . . C53 C 0.6939(6) 0.9005(5) 0.8879(5) 0.080(2) Uani 1 1 d . . . H53 H 0.7446 0.9165 0.9445 0.096 Uiso 1 1 calc R . . C55 C 0.7796(8) 1.1795(5) 0.8419(5) 0.096(3) Uani 1 1 d . . . H55A H 0.8151 1.2352 0.8902 0.116 Uiso 1 1 calc R . . H55B H 0.7462 1.1229 0.8594 0.116 Uiso 1 1 calc R . . C56 C 0.6081(10) 0.9269(7) 0.8678(9) 0.126(4) Uani 1 1 d . . . H56 H 0.5997 0.9611 0.9094 0.151 Uiso 1 1 calc R . . C57 C 0.5378(12) 0.9022(10) 0.7875(12) 0.171(9) Uani 1 1 d . . . H57 H 0.4793 0.9206 0.7745 0.205 Uiso 1 1 calc R . . C58 C 0.5411(14) 0.8552(12) 0.7247(9) 0.183(10) Uani 1 1 d . . . H58 H 0.4874 0.8403 0.6692 0.219 Uiso 1 1 calc R . . C59 C 0.6806(6) 1.1820(5) 0.7727(5) 0.086(2) Uani 1 1 d . . . H59A H 0.6460 1.1292 0.7222 0.103 Uiso 1 1 calc R . . H59B H 0.6193 1.1770 0.7907 0.103 Uiso 1 1 calc R . . C60 C 0.6790(5) 1.2861(4) 0.6805(4) 0.0593(17) Uani 1 1 d . . . C61 C 0.7895(6) 1.1096(5) 0.6639(4) 0.0634(17) Uani 1 1 d . . . C62 C 0.8704(5) 1.4388(4) 0.7184(4) 0.0547(15) Uani 1 1 d . . . C63 C 0.8262(6) 1.0935(5) 0.7497(5) 0.085(2) Uani 1 1 d . . . H63A H 0.7586 1.0410 0.7509 0.102 Uiso 1 1 calc R . . H63B H 0.8868 1.0744 0.7578 0.102 Uiso 1 1 calc R . . C64 C 0.8604(8) 0.6359(7) 0.5012(7) 0.136(4) Uani 1 1 d . . . H64A H 0.8088 0.6557 0.4642 0.163 Uiso 1 1 calc R . . H64B H 0.9413 0.6869 0.5226 0.163 Uiso 1 1 calc R . . C65 C 0.8482(9) 0.5520(8) 0.4568(7) 0.180(6) Uani 1 1 d . . . H65A H 0.8835 0.5244 0.4960 0.270 Uiso 1 1 calc R . . H65B H 0.8869 0.5662 0.4198 0.270 Uiso 1 1 calc R . . H65C H 0.7658 0.5073 0.4239 0.270 Uiso 1 1 calc R . . N1 N 1.5218(5) 0.6481(4) 0.8534(5) 0.0802(17) Uani 1 1 d . . . N2 N 0.9172(5) 0.9047(4) 0.8661(4) 0.0914(19) Uani 1 1 d . . . H2A H 0.9014 0.9405 0.8327 0.110 Uiso 1 1 calc R . . H2B H 0.9478 0.9409 0.9199 0.110 Uiso 1 1 calc R . . N3 N 0.9326(4) 1.4146(3) 0.7784(3) 0.0633(14) Uani 1 1 d . . . N4 N 1.1047(7) 1.1466(4) 0.5836(4) 0.0912(19) Uani 1 1 d . . . N5 N 0.4953(6) 0.3076(4) 0.8053(5) 0.0812(17) Uani 1 1 d . . . N6 N 0.5189(6) 0.5069(5) 0.6176(4) 0.0843(18) Uani 1 1 d . . . N7 N 1.1785(5) 0.6648(3) 0.6670(3) 0.0613(13) Uani 1 1 d . . . N8 N 0.8744(4) 0.5789(4) 0.8781(4) 0.0660(14) Uani 1 1 d . . . N9 N 0.8583(5) 0.8601(4) 0.6349(4) 0.0700(15) Uani 1 1 d . . . N10 N 0.8717(6) 1.1785(4) 0.8202(4) 0.0799(17) Uani 1 1 d . . . N11 N 1.3060(5) 0.7548(5) 0.9772(4) 0.0800(17) Uani 1 1 d . . . N12 N 1.2743(5) 0.9477(4) 0.6867(4) 0.0691(15) Uani 1 1 d . . . Nd1 Nd 0.95840(3) 0.68753(2) 0.72554(2) 0.05516(13) Uani 1 1 d . . . O1 O 1.0455(5) 1.0877(3) 0.8754(3) 0.1008(17) Uani 1 1 d . . . O2 O 0.7319(4) 1.2730(3) 0.7559(3) 0.0682(11) Uani 1 1 d . . . O3 O 1.2391(5) 0.6935(5) 0.9961(4) 0.130(2) Uani 1 1 d . . . O4 O 1.3580(6) 0.8370(5) 1.0124(4) 0.140(3) Uani 1 1 d . . . O5 O 1.3690(4) 1.0133(3) 0.6976(4) 0.0976(17) Uani 1 1 d . . . O6 O 1.2634(4) 0.8709(4) 0.6926(4) 0.124(2) Uani 1 1 d . . . O7 O 1.1973(5) 1.1954(4) 0.5797(4) 0.120(2) Uani 1 1 d . . . O8 O 1.0211(6) 1.1616(4) 0.5607(5) 0.139(3) Uani 1 1 d . . . O9 O 0.5403(5) 0.2998(5) 0.8754(5) 0.143(3) Uani 1 1 d . . . O10 O 0.3945(5) 0.2530(4) 0.7555(4) 0.114(2) Uani 1 1 d . . . O11 O 0.4172(5) 0.4574(6) 0.5793(5) 0.188(4) Uani 1 1 d . . . O12 O 0.5700(6) 0.5700(5) 0.5952(5) 0.189(4) Uani 1 1 d . . . O13 O 1.0774(4) 0.6505(3) 0.6504(3) 0.0690(12) Uani 1 1 d . . . O14 O 1.1500(3) 0.7257(3) 0.8167(2) 0.0571(10) Uani 1 1 d . . . O15 O 0.9885(3) 0.8101(3) 0.8355(3) 0.0728(13) Uani 1 1 d . . . O16 O 1.0531(3) 0.8194(3) 0.6835(3) 0.0669(11) Uani 1 1 d . . . O17 O 0.7676(3) 0.6161(3) 0.7210(3) 0.0686(12) Uani 1 1 d . . . O18 O 0.9484(3) 0.6367(3) 0.8609(3) 0.0711(12) Uani 1 1 d . . . O19 O 0.9137(4) 1.5200(3) 0.7075(2) 0.0679(11) Uani 1 1 d . . . O20 O 0.8285(5) 0.6173(4) 0.5725(3) 0.0810(16) Uani 1 1 d . . . O21 O 0.9029(4) 0.5646(4) 0.9473(3) 0.118(2) Uani 1 1 d . . . O22 O 1.2157(4) 0.6653(4) 0.6120(3) 0.0937(16) Uani 1 1 d . . . O23 O 0.8404(4) 0.7895(4) 0.6599(4) 0.0994(17) Uani 1 1 d . . . O24 O 0.7804(4) 0.8799(4) 0.6067(4) 0.124(2) Uani 1 1 d . . . O25 O 1.5271(4) 0.6152(4) 0.7899(4) 0.1035(18) Uani 1 1 d . . . O26 O 1.5909(5) 0.6639(4) 0.9257(4) 0.1048(18) Uani 1 1 d . . . H20A H 0.765(5) 0.595(5) 0.561(4) 0.07(3) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C2 0.059(4) 0.046(4) 0.063(4) 0.012(3) 0.017(3) 0.035(3) C3 0.061(5) 0.064(5) 0.126(7) 0.005(5) 0.034(5) 0.030(4) C4 0.134(9) 0.108(7) 0.089(7) -0.005(6) -0.014(7) 0.085(7) C5 0.079(6) 0.100(7) 0.125(9) -0.023(7) -0.016(6) 0.055(6) C6 0.114(6) 0.080(5) 0.059(5) 0.017(4) 0.016(5) 0.060(5) C7 0.067(4) 0.043(4) 0.070(4) 0.025(3) 0.033(3) 0.022(3) C8 0.056(4) 0.052(4) 0.070(4) 0.025(3) 0.033(3) 0.031(3) C9 0.052(4) 0.053(4) 0.061(4) 0.028(3) 0.033(3) 0.025(3) C10 0.059(4) 0.056(4) 0.053(4) 0.027(3) 0.030(3) 0.029(3) C11 0.078(5) 0.048(4) 0.085(5) 0.031(3) 0.040(4) 0.037(3) C12 0.060(4) 0.061(4) 0.070(4) 0.024(3) 0.027(3) 0.037(3) C13 0.049(4) 0.084(5) 0.085(5) 0.012(4) 0.031(4) 0.013(4) C14 0.070(6) 0.124(8) 0.095(6) 0.027(6) 0.031(5) 0.030(5) C15 0.095(6) 0.069(5) 0.089(6) 0.044(4) 0.017(5) 0.017(5) C16 0.080(5) 0.085(6) 0.066(5) 0.035(4) 0.006(4) 0.029(5) C17 0.082(6) 0.112(8) 0.100(7) 0.050(6) 0.025(5) 0.026(6) C18 0.052(4) 0.054(4) 0.063(4) 0.020(3) 0.011(3) 0.011(3) C19 0.053(4) 0.055(4) 0.051(4) 0.022(3) 0.024(3) 0.031(3) C20 0.059(4) 0.053(4) 0.071(4) 0.017(3) 0.036(4) 0.028(3) C21 0.053(4) 0.055(4) 0.079(5) 0.020(3) 0.028(4) 0.034(3) C22 0.043(3) 0.045(3) 0.060(4) 0.017(3) 0.023(3) 0.021(3) C23 0.063(4) 0.057(4) 0.057(4) 0.014(3) 0.029(3) 0.029(3) C24 0.059(4) 0.071(4) 0.066(4) 0.018(3) 0.023(3) 0.035(3) C25 0.059(4) 0.063(4) 0.063(4) 0.029(3) 0.030(3) 0.039(3) C26 0.061(4) 0.058(4) 0.058(4) 0.025(3) 0.031(3) 0.032(3) C27 0.049(4) 0.052(4) 0.075(5) 0.017(3) 0.025(3) 0.024(3) C28 0.045(3) 0.051(3) 0.056(4) 0.015(3) 0.022(3) 0.025(3) C29 0.048(4) 0.048(3) 0.070(4) 0.018(3) 0.031(3) 0.028(3) C30 0.054(4) 0.045(3) 0.074(4) 0.020(3) 0.033(4) 0.019(3) C32 0.079(5) 0.062(5) 0.097(6) 0.013(4) 0.043(4) 0.039(4) C33 0.143(8) 0.106(7) 0.116(8) 0.054(6) 0.086(7) 0.080(7) C34 0.077(5) 0.086(6) 0.088(6) 0.016(5) 0.025(5) 0.040(4) C35 0.161(10) 0.137(9) 0.095(7) 0.044(7) 0.068(7) 0.107(8) C36 0.121(8) 0.119(8) 0.087(7) 0.003(6) 0.023(6) 0.069(7) C37 0.045(3) 0.051(4) 0.072(4) 0.031(3) 0.022(3) 0.020(3) C38 0.074(5) 0.114(6) 0.081(5) 0.037(5) 0.029(4) 0.053(5) C39 0.085(5) 0.097(6) 0.079(5) 0.025(4) 0.043(4) 0.042(4) C40 0.097(8) 0.105(8) 0.234(15) 0.047(9) 0.071(10) 0.070(6) C41 0.085(7) 0.141(9) 0.133(9) 0.067(7) 0.030(6) 0.066(6) C42 0.119(8) 0.142(9) 0.150(10) 0.024(7) 0.086(8) 0.069(7) C43 0.061(4) 0.071(4) 0.071(5) 0.012(4) 0.015(4) 0.031(4) C46 0.051(4) 0.066(4) 0.084(5) 0.029(4) 0.030(4) 0.033(3) C47 0.130(8) 0.061(5) 0.121(8) 0.008(5) -0.004(6) 0.045(5) C48 0.176(10) 0.095(6) 0.087(6) 0.011(5) 0.041(7) 0.093(7) C50 0.079(5) 0.065(5) 0.224(10) 0.062(6) 0.096(6) 0.041(4) C51 0.057(4) 0.059(4) 0.088(5) 0.025(4) 0.038(4) 0.027(3) C52 0.113(8) 0.085(6) 0.083(7) 0.019(5) 0.046(6) -0.003(6) C53 0.089(5) 0.089(5) 0.079(5) 0.028(4) 0.041(4) 0.050(4) C55 0.157(8) 0.067(5) 0.112(7) 0.055(5) 0.084(6) 0.067(5) C56 0.145(10) 0.116(8) 0.227(13) 0.095(9) 0.137(10) 0.101(8) C57 0.073(8) 0.158(14) 0.30(2) 0.167(17) 0.056(14) 0.064(10) C58 0.108(11) 0.175(17) 0.128(11) 0.089(11) -0.013(10) -0.013(10) C59 0.089(5) 0.064(5) 0.132(7) 0.042(5) 0.073(5) 0.037(4) C60 0.054(4) 0.051(4) 0.082(5) 0.008(4) 0.030(4) 0.034(3) C61 0.068(4) 0.060(4) 0.069(5) 0.016(4) 0.027(4) 0.039(4) C62 0.064(4) 0.045(4) 0.074(4) 0.025(3) 0.036(4) 0.035(3) C63 0.102(6) 0.059(4) 0.099(6) 0.017(4) 0.036(5) 0.048(4) C64 0.099(7) 0.136(9) 0.134(9) 0.085(7) 0.018(6) 0.038(6) C65 0.165(11) 0.152(10) 0.164(11) -0.046(9) 0.022(8) 0.087(9) N1 0.073(4) 0.081(4) 0.110(6) 0.039(4) 0.038(4) 0.056(4) N2 0.077(4) 0.060(4) 0.146(6) 0.033(4) 0.050(4) 0.038(3) N3 0.048(3) 0.061(3) 0.079(4) 0.027(3) 0.016(3) 0.032(3) N4 0.100(5) 0.077(5) 0.124(6) 0.060(4) 0.057(5) 0.050(4) N5 0.075(4) 0.066(4) 0.095(5) 0.035(4) 0.041(4) 0.021(3) N6 0.071(4) 0.094(5) 0.076(4) 0.037(4) 0.019(4) 0.036(4) N7 0.071(4) 0.059(3) 0.063(4) 0.020(3) 0.034(3) 0.034(3) N8 0.052(3) 0.073(4) 0.067(4) 0.025(3) 0.025(3) 0.024(3) N9 0.062(4) 0.067(4) 0.098(4) 0.035(3) 0.041(3) 0.038(3) N10 0.123(5) 0.064(4) 0.073(4) 0.017(3) 0.043(4) 0.062(4) N11 0.071(4) 0.100(5) 0.067(4) 0.016(4) 0.030(3) 0.041(4) N12 0.057(4) 0.069(4) 0.096(4) 0.040(3) 0.039(3) 0.034(3) Nd1 0.0545(2) 0.0522(2) 0.0754(3) 0.03236(17) 0.03546(18) 0.03047(16) O1 0.099(4) 0.040(3) 0.126(4) 0.025(3) 0.014(3) 0.028(3) O2 0.071(3) 0.054(3) 0.083(3) 0.027(2) 0.037(3) 0.028(2) O3 0.128(5) 0.155(6) 0.098(4) 0.017(4) 0.071(4) 0.046(4) O4 0.179(6) 0.090(4) 0.135(6) -0.011(4) 0.078(5) 0.052(4) O5 0.059(3) 0.085(4) 0.159(5) 0.059(3) 0.052(3) 0.034(3) O6 0.087(4) 0.094(4) 0.246(7) 0.103(5) 0.089(4) 0.064(3) O7 0.098(4) 0.094(4) 0.169(6) 0.088(4) 0.048(4) 0.041(3) O8 0.159(6) 0.129(5) 0.237(8) 0.129(5) 0.125(6) 0.113(5) O9 0.102(4) 0.141(6) 0.145(6) 0.098(5) 0.046(4) 0.015(4) O10 0.082(4) 0.074(4) 0.121(5) 0.026(3) 0.031(3) -0.009(3) O11 0.058(4) 0.300(10) 0.174(7) 0.156(7) 0.018(4) 0.061(5) O12 0.139(6) 0.131(6) 0.154(6) 0.098(5) -0.035(5) 0.001(4) O13 0.061(3) 0.086(3) 0.068(3) 0.027(2) 0.026(2) 0.043(2) O14 0.054(2) 0.062(3) 0.063(3) 0.020(2) 0.027(2) 0.032(2) O15 0.062(3) 0.051(3) 0.112(4) 0.016(2) 0.044(3) 0.029(2) O16 0.061(3) 0.062(3) 0.097(3) 0.047(2) 0.041(2) 0.033(2) O17 0.058(3) 0.070(3) 0.093(3) 0.047(3) 0.039(2) 0.033(2) O18 0.059(3) 0.065(3) 0.080(3) 0.026(2) 0.034(2) 0.016(2) O19 0.090(3) 0.055(3) 0.063(3) 0.028(2) 0.034(2) 0.035(2) O20 0.068(4) 0.097(4) 0.092(4) 0.054(3) 0.038(3) 0.043(3) O21 0.073(3) 0.160(5) 0.072(4) 0.056(4) 0.018(3) 0.017(3) O22 0.108(4) 0.140(5) 0.070(3) 0.042(3) 0.055(3) 0.075(3) O23 0.075(3) 0.099(4) 0.168(5) 0.085(4) 0.074(3) 0.050(3) O24 0.070(3) 0.133(5) 0.214(7) 0.105(5) 0.072(4) 0.066(3) O25 0.102(4) 0.120(5) 0.128(5) 0.029(4) 0.059(4) 0.081(3) O26 0.091(4) 0.132(5) 0.119(5) 0.045(4) 0.034(4) 0.084(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C2 C6 1.379(8) . ? C2 C60 1.397(8) . ? C2 C62 1.482(8) . ? C3 C5 1.374(12) . ? C3 C60 1.391(9) . ? C3 H3 0.9300 . ? C4 C5 1.362(13) . ? C4 C6 1.370(10) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C8 1.358(7) . ? C7 C11 1.373(8) . ? C7 H7 0.9300 . ? C8 C10 1.429(7) . ? C8 N12 1.454(7) . ? C9 C12 1.371(8) . ? C9 C10 1.452(8) . ? C9 N9 1.455(7) . ? C10 O16 1.253(6) . ? C11 C12 1.378(8) . ? C11 N4 1.447(8) . ? C12 H12 0.9300 . ? C13 C14 1.376(9) . ? C13 C18 1.389(9) . ? C13 H13 0.9300 . ? C14 C17 1.332(11) . ? C14 H14 0.9300 . ? C15 C17 1.362(11) . ? C15 C16 1.439(10) . ? C15 H15 0.9300 . ? C16 O1 1.369(9) . ? C16 C18 1.370(9) . ? C17 H17 0.9300 . ? C18 C46 1.478(8) . ? C19 C20 1.381(7) . ? C19 C22 1.405(7) . ? C19 N7 1.451(7) . ? C20 C21 1.367(8) . ? C20 H20 0.9300 . ? C21 C24 1.387(8) . ? C21 N1 1.478(7) . ? C22 O14 1.287(6) . ? C22 C23 1.430(8) . ? C23 C24 1.363(8) . ? C23 N11 1.480(8) . ? C24 H24 0.9300 . ? C25 C27 1.358(8) . ? C25 C29 1.441(7) . ? C25 N6 1.461(8) . ? C26 C28 1.364(7) . ? C26 C30 1.367(7) . ? C26 H26 0.9300 . ? C27 C30 1.366(8) . ? C27 H27 0.9300 . ? C28 C29 1.441(8) . ? C28 N8 1.457(7) . ? C29 O17 1.257(6) . ? C30 N5 1.448(8) . ? C32 C61 1.346(9) . ? C32 C33 1.388(10) . ? C32 H32 0.9300 . ? C33 C35 1.355(11) . ? C33 H33 0.9300 . ? C34 C36 1.381(11) . ? C34 C61 1.388(9) . ? C34 H34 0.9300 . ? C35 C36 1.382(12) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C37 C39 1.356(9) . ? C37 C38 1.363(9) . ? C37 C43 1.523(8) . ? C38 C41 1.372(11) . ? C38 H38 0.9300 . ? C39 C42 1.375(11) . ? C39 H39 0.9300 . ? C40 C41 1.339(13) . ? C40 C42 1.368(13) . ? C40 H40 0.9300 . ? C41 H41 0.9300 . ? C42 H42 0.9300 . ? C43 N3 1.477(7) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C46 O15 1.236(7) . ? C46 N2 1.336(7) . ? C47 O1 1.433(8) . ? C47 C48 1.474(11) . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C48 N10 1.487(9) . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C50 C51 1.480(9) . ? C50 N2 1.482(7) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C51 C53 1.368(9) . ? C51 C52 1.378(11) . ? C52 C58 1.411(17) . ? C52 H52 0.9300 . ? C53 C56 1.357(10) . ? C53 H53 0.9300 . ? C55 N10 1.441(9) . ? C55 C59 1.503(10) . ? C55 H55A 0.9700 . ? C55 H55B 0.9700 . ? C56 C57 1.309(15) . ? C56 H56 0.9300 . ? C57 C58 1.29(2) . ? C57 H57 0.9300 . ? C58 H58 0.9300 . ? C59 O2 1.447(7) . ? C59 H59A 0.9700 . ? C59 H59B 0.9700 . ? C60 O2 1.364(7) . ? C61 C63 1.507(9) . ? C62 O19 1.255(6) . ? C62 N3 1.320(7) . ? C63 N10 1.472(8) . ? C63 H63A 0.9700 . ? C63 H63B 0.9700 . ? C64 C65 1.387(12) . ? C64 O20 1.482(10) . ? C64 H64A 0.9700 . ? C64 H64B 0.9700 . ? C65 H65A 0.9600 . ? C65 H65B 0.9600 . ? C65 H65C 0.9600 . ? N1 O25 1.215(7) . ? N1 O26 1.221(7) . ? N2 H2A 0.9000 . ? N2 H2B 0.9000 . ? N4 O8 1.210(7) . ? N4 O7 1.216(7) . ? N5 O10 1.205(7) . ? N5 O9 1.222(7) . ? N6 O11 1.165(7) . ? N6 O12 1.166(7) . ? N7 O13 1.226(5) . ? N7 O22 1.233(6) . ? N8 O18 1.214(6) . ? N8 O21 1.224(6) . ? N9 O24 1.201(6) . ? N9 O23 1.218(6) . ? N11 O4 1.168(7) . ? N11 O3 1.205(7) . ? N12 O6 1.195(6) . ? N12 O5 1.219(6) . ? Nd1 O16 2.329(4) . ? Nd1 O14 2.334(4) . ? Nd1 O17 2.351(4) . ? Nd1 O15 2.381(4) . ? Nd1 O19 2.443(4) 1_545 ? Nd1 O20 2.466(5) . ? Nd1 O13 2.611(4) . ? Nd1 O18 2.624(4) . ? Nd1 O23 2.816(5) . ? O19 Nd1 2.443(4) 1_565 ? O20 H20A 0.73(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 C2 C60 117.6(6) . . ? C6 C2 C62 118.4(6) . . ? C60 C2 C62 124.0(6) . . ? C5 C3 C60 119.5(8) . . ? C5 C3 H3 120.3 . . ? C60 C3 H3 120.3 . . ? C5 C4 C6 118.3(9) . . ? C5 C4 H4 120.9 . . ? C6 C4 H4 120.9 . . ? C4 C5 C3 121.7(9) . . ? C4 C5 H5 119.2 . . ? C3 C5 H5 119.2 . . ? C4 C6 C2 122.9(8) . . ? C4 C6 H6 118.5 . . ? C2 C6 H6 118.5 . . ? C8 C7 C11 120.3(6) . . ? C8 C7 H7 119.9 . . ? C11 C7 H7 119.9 . . ? C7 C8 C10 124.1(6) . . ? C7 C8 N12 116.2(5) . . ? C10 C8 N12 119.7(5) . . ? C12 C9 C10 124.0(5) . . ? C12 C9 N9 116.8(5) . . ? C10 C9 N9 119.2(5) . . ? O16 C10 C8 123.7(5) . . ? O16 C10 C9 124.3(5) . . ? C8 C10 C9 112.0(5) . . ? C7 C11 C12 120.6(6) . . ? C7 C11 N4 120.1(6) . . ? C12 C11 N4 119.2(6) . . ? C9 C12 C11 119.0(6) . . ? C9 C12 H12 120.5 . . ? C11 C12 H12 120.5 . . ? C14 C13 C18 122.5(8) . . ? C14 C13 H13 118.7 . . ? C18 C13 H13 118.7 . . ? C17 C14 C13 117.0(9) . . ? C17 C14 H14 121.5 . . ? C13 C14 H14 121.5 . . ? C17 C15 C16 116.4(8) . . ? C17 C15 H15 121.8 . . ? C16 C15 H15 121.8 . . ? O1 C16 C18 117.3(7) . . ? O1 C16 C15 122.7(8) . . ? C18 C16 C15 120.0(8) . . ? C14 C17 C15 125.5(9) . . ? C14 C17 H17 117.3 . . ? C15 C17 H17 117.3 . . ? C16 C18 C13 118.4(6) . . ? C16 C18 C46 126.9(7) . . ? C13 C18 C46 114.8(6) . . ? C20 C19 C22 123.2(5) . . ? C20 C19 N7 116.8(5) . . ? C22 C19 N7 120.0(5) . . ? C21 C20 C19 118.8(6) . . ? C21 C20 H20 120.6 . . ? C19 C20 H20 120.6 . . ? C20 C21 C24 122.4(6) . . ? C20 C21 N1 119.8(6) . . ? C24 C21 N1 117.8(6) . . ? O14 C22 C19 126.3(5) . . ? O14 C22 C23 120.0(5) . . ? C19 C22 C23 113.7(5) . . ? C24 C23 C22 124.6(6) . . ? C24 C23 N11 118.7(6) . . ? C22 C23 N11 116.7(5) . . ? C23 C24 C21 117.1(6) . . ? C23 C24 H24 121.4 . . ? C21 C24 H24 121.4 . . ? C27 C25 C29 123.9(6) . . ? C27 C25 N6 116.5(6) . . ? C29 C25 N6 119.5(6) . . ? C28 C26 C30 119.6(6) . . ? C28 C26 H26 120.2 . . ? C30 C26 H26 120.2 . . ? C25 C27 C30 119.4(6) . . ? C25 C27 H27 120.3 . . ? C30 C27 H27 120.3 . . ? C26 C28 C29 123.4(5) . . ? C26 C28 N8 115.9(5) . . ? C29 C28 N8 120.6(5) . . ? O17 C29 C28 124.8(5) . . ? O17 C29 C25 123.1(6) . . ? C28 C29 C25 112.1(5) . . ? C27 C30 C26 121.3(6) . . ? C27 C30 N5 120.0(6) . . ? C26 C30 N5 118.7(6) . . ? C61 C32 C33 123.1(8) . . ? C61 C32 H32 118.5 . . ? C33 C32 H32 118.5 . . ? C35 C33 C32 119.5(9) . . ? C35 C33 H33 120.3 . . ? C32 C33 H33 120.3 . . ? C36 C34 C61 119.9(8) . . ? C36 C34 H34 120.1 . . ? C61 C34 H34 120.1 . . ? C33 C35 C36 118.6(9) . . ? C33 C35 H35 120.7 . . ? C36 C35 H35 120.7 . . ? C34 C36 C35 121.3(9) . . ? C34 C36 H36 119.4 . . ? C35 C36 H36 119.4 . . ? C39 C37 C38 118.4(7) . . ? C39 C37 C43 122.4(6) . . ? C38 C37 C43 119.1(6) . . ? C37 C38 C41 121.6(8) . . ? C37 C38 H38 119.2 . . ? C41 C38 H38 119.2 . . ? C37 C39 C42 120.0(8) . . ? C37 C39 H39 120.0 . . ? C42 C39 H39 120.0 . . ? C41 C40 C42 119.4(10) . . ? C41 C40 H40 120.3 . . ? C42 C40 H40 120.3 . . ? C40 C41 C38 119.7(10) . . ? C40 C41 H41 120.1 . . ? C38 C41 H41 120.1 . . ? C40 C42 C39 120.7(10) . . ? C40 C42 H42 119.6 . . ? C39 C42 H42 119.6 . . ? N3 C43 C37 112.6(5) . . ? N3 C43 H43A 109.1 . . ? C37 C43 H43A 109.1 . . ? N3 C43 H43B 109.1 . . ? C37 C43 H43B 109.1 . . ? H43A C43 H43B 107.8 . . ? O15 C46 N2 118.9(5) . . ? O15 C46 C18 121.1(6) . . ? N2 C46 C18 120.0(6) . . ? O1 C47 C48 108.2(7) . . ? O1 C47 H47A 110.1 . . ? C48 C47 H47A 110.1 . . ? O1 C47 H47B 110.1 . . ? C48 C47 H47B 110.1 . . ? H47A C47 H47B 108.4 . . ? C47 C48 N10 114.8(7) . . ? C47 C48 H48A 108.6 . . ? N10 C48 H48A 108.6 . . ? C47 C48 H48B 108.6 . . ? N10 C48 H48B 108.6 . . ? H48A C48 H48B 107.5 . . ? C51 C50 N2 111.2(6) . . ? C51 C50 H50A 109.4 . . ? N2 C50 H50A 109.4 . . ? C51 C50 H50B 109.4 . . ? N2 C50 H50B 109.4 . . ? H50A C50 H50B 108.0 . . ? C53 C51 C52 117.9(7) . . ? C53 C51 C50 120.7(7) . . ? C52 C51 C50 121.5(8) . . ? C51 C52 C58 119.4(11) . . ? C51 C52 H52 120.3 . . ? C58 C52 H52 120.3 . . ? C56 C53 C51 121.5(8) . . ? C56 C53 H53 119.3 . . ? C51 C53 H53 119.3 . . ? N10 C55 C59 115.6(6) . . ? N10 C55 H55A 108.4 . . ? C59 C55 H55A 108.4 . . ? N10 C55 H55B 108.4 . . ? C59 C55 H55B 108.4 . . ? H55A C55 H55B 107.4 . . ? C57 C56 C53 117.4(11) . . ? C57 C56 H56 121.3 . . ? C53 C56 H56 121.3 . . ? C58 C57 C56 126.8(17) . . ? C58 C57 H57 116.6 . . ? C56 C57 H57 116.6 . . ? C57 C58 C52 117.1(15) . . ? C57 C58 H58 121.5 . . ? C52 C58 H58 121.5 . . ? O2 C59 C55 106.5(5) . . ? O2 C59 H59A 110.4 . . ? C55 C59 H59A 110.4 . . ? O2 C59 H59B 110.4 . . ? C55 C59 H59B 110.4 . . ? H59A C59 H59B 108.6 . . ? O2 C60 C3 122.4(7) . . ? O2 C60 C2 117.6(5) . . ? C3 C60 C2 120.0(7) . . ? C32 C61 C34 117.6(7) . . ? C32 C61 C63 121.8(7) . . ? C34 C61 C63 120.6(7) . . ? O19 C62 N3 122.0(6) . . ? O19 C62 C2 119.3(5) . . ? N3 C62 C2 118.6(5) . . ? N10 C63 C61 113.6(6) . . ? N10 C63 H63A 108.8 . . ? C61 C63 H63A 108.8 . . ? N10 C63 H63B 108.8 . . ? C61 C63 H63B 108.8 . . ? H63A C63 H63B 107.7 . . ? C65 C64 O20 108.3(9) . . ? C65 C64 H64A 110.0 . . ? O20 C64 H64A 110.0 . . ? C65 C64 H64B 110.0 . . ? O20 C64 H64B 110.0 . . ? H64A C64 H64B 108.4 . . ? C64 C65 H65A 109.5 . . ? C64 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C64 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? O25 N1 O26 124.9(6) . . ? O25 N1 C21 117.4(7) . . ? O26 N1 C21 117.8(7) . . ? C46 N2 C50 122.8(5) . . ? C46 N2 H2A 106.6 . . ? C50 N2 H2A 106.6 . . ? C46 N2 H2B 106.6 . . ? C50 N2 H2B 106.6 . . ? H2A N2 H2B 106.6 . . ? C62 N3 C43 122.3(5) . . ? O8 N4 O7 123.5(7) . . ? O8 N4 C11 118.7(6) . . ? O7 N4 C11 117.7(7) . . ? O10 N5 O9 123.0(7) . . ? O10 N5 C30 119.2(7) . . ? O9 N5 C30 117.7(6) . . ? O11 N6 O12 120.3(7) . . ? O11 N6 C25 118.6(7) . . ? O12 N6 C25 121.0(7) . . ? O13 N7 O22 121.9(5) . . ? O13 N7 C19 120.1(5) . . ? O22 N7 C19 118.0(5) . . ? O18 N8 O21 120.2(5) . . ? O18 N8 C28 122.1(5) . . ? O21 N8 C28 117.7(5) . . ? O24 N9 O23 120.4(6) . . ? O24 N9 C9 118.0(6) . . ? O23 N9 C9 121.6(5) . . ? C55 N10 C63 112.0(6) . . ? C55 N10 C48 106.4(6) . . ? C63 N10 C48 114.6(5) . . ? O4 N11 O3 125.8(7) . . ? O4 N11 C23 118.0(7) . . ? O3 N11 C23 116.3(7) . . ? O6 N12 O5 121.6(6) . . ? O6 N12 C8 119.6(5) . . ? O5 N12 C8 118.7(6) . . ? O16 Nd1 O14 84.40(13) . . ? O16 Nd1 O17 130.52(14) . . ? O14 Nd1 O17 138.37(14) . . ? O16 Nd1 O15 81.71(15) . . ? O14 Nd1 O15 82.53(13) . . ? O17 Nd1 O15 81.65(14) . . ? O16 Nd1 O19 140.82(14) . 1_545 ? O14 Nd1 O19 85.82(13) . 1_545 ? O17 Nd1 O19 78.35(14) . 1_545 ? O15 Nd1 O19 134.23(15) . 1_545 ? O16 Nd1 O20 82.69(16) . . ? O14 Nd1 O20 137.77(16) . . ? O17 Nd1 O20 76.75(17) . . ? O15 Nd1 O20 134.44(17) . . ? O19 Nd1 O20 79.49(15) 1_545 . ? O16 Nd1 O13 70.88(14) . . ? O14 Nd1 O13 65.49(13) . . ? O17 Nd1 O13 139.23(14) . . ? O15 Nd1 O13 139.11(13) . . ? O19 Nd1 O13 70.53(14) 1_545 . ? O20 Nd1 O13 72.29(16) . . ? O16 Nd1 O18 141.81(14) . . ? O14 Nd1 O18 72.83(13) . . ? O17 Nd1 O18 65.56(13) . . ? O15 Nd1 O18 65.52(14) . . ? O19 Nd1 O18 68.75(13) 1_545 . ? O20 Nd1 O18 134.32(15) . . ? O13 Nd1 O18 122.61(13) . . ? O16 Nd1 O23 60.42(13) . . ? O14 Nd1 O23 136.50(14) . . ? O17 Nd1 O23 70.11(13) . . ? O15 Nd1 O23 68.64(16) . . ? O19 Nd1 O23 137.58(14) 1_545 . ? O20 Nd1 O23 66.40(17) . . ? O13 Nd1 O23 118.30(14) . . ? O18 Nd1 O23 119.08(14) . . ? C16 O1 C47 118.6(6) . . ? C60 O2 C59 121.4(5) . . ? N7 O13 Nd1 139.3(4) . . ? C22 O14 Nd1 142.5(4) . . ? C46 O15 Nd1 145.7(5) . . ? C10 O16 Nd1 153.6(4) . . ? C29 O17 Nd1 137.7(4) . . ? N8 O18 Nd1 136.8(4) . . ? C62 O19 Nd1 155.4(4) . 1_565 ? C64 O20 Nd1 127.9(5) . . ? C64 O20 H20A 114(6) . . ? Nd1 O20 H20A 116(6) . . ? N9 O23 Nd1 139.8(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C4 C5 C3 -0.1(14) . . . . ? C60 C3 C5 C4 -0.5(13) . . . . ? C5 C4 C6 C2 -0.4(13) . . . . ? C60 C2 C6 C4 1.5(10) . . . . ? C62 C2 C6 C4 -177.5(7) . . . . ? C11 C7 C8 C10 0.5(10) . . . . ? C11 C7 C8 N12 -178.5(5) . . . . ? C7 C8 C10 O16 179.0(6) . . . . ? N12 C8 C10 O16 -2.1(9) . . . . ? C7 C8 C10 C9 -0.5(8) . . . . ? N12 C8 C10 C9 178.4(5) . . . . ? C12 C9 C10 O16 -178.5(6) . . . . ? N9 C9 C10 O16 0.7(9) . . . . ? C12 C9 C10 C8 1.0(8) . . . . ? N9 C9 C10 C8 -179.8(5) . . . . ? C8 C7 C11 C12 -0.8(10) . . . . ? C8 C7 C11 N4 -177.2(6) . . . . ? C10 C9 C12 C11 -1.4(9) . . . . ? N9 C9 C12 C11 179.4(5) . . . . ? C7 C11 C12 C9 1.3(10) . . . . ? N4 C11 C12 C9 177.7(6) . . . . ? C18 C13 C14 C17 -2.7(12) . . . . ? C17 C15 C16 O1 178.8(7) . . . . ? C17 C15 C16 C18 -3.4(11) . . . . ? C13 C14 C17 C15 4.7(14) . . . . ? C16 C15 C17 C14 -1.8(14) . . . . ? O1 C16 C18 C13 -176.9(6) . . . . ? C15 C16 C18 C13 5.2(10) . . . . ? O1 C16 C18 C46 4.8(11) . . . . ? C15 C16 C18 C46 -173.2(7) . . . . ? C14 C13 C18 C16 -2.2(11) . . . . ? C14 C13 C18 C46 176.4(7) . . . . ? C22 C19 C20 C21 0.5(8) . . . . ? N7 C19 C20 C21 -178.8(5) . . . . ? C19 C20 C21 C24 -2.2(9) . . . . ? C19 C20 C21 N1 177.7(5) . . . . ? C20 C19 C22 O14 -178.3(5) . . . . ? N7 C19 C22 O14 1.0(8) . . . . ? C20 C19 C22 C23 1.7(8) . . . . ? N7 C19 C22 C23 -179.0(5) . . . . ? O14 C22 C23 C24 177.3(5) . . . . ? C19 C22 C23 C24 -2.7(8) . . . . ? O14 C22 C23 N11 -0.7(8) . . . . ? C19 C22 C23 N11 179.3(5) . . . . ? C22 C23 C24 C21 1.3(9) . . . . ? N11 C23 C24 C21 179.3(6) . . . . ? C20 C21 C24 C23 1.3(9) . . . . ? N1 C21 C24 C23 -178.6(5) . . . . ? C29 C25 C27 C30 1.6(9) . . . . ? N6 C25 C27 C30 -176.4(6) . . . . ? C30 C26 C28 C29 -0.4(9) . . . . ? C30 C26 C28 N8 179.7(5) . . . . ? C26 C28 C29 O17 -178.0(5) . . . . ? N8 C28 C29 O17 2.0(9) . . . . ? C26 C28 C29 C25 2.9(8) . . . . ? N8 C28 C29 C25 -177.2(5) . . . . ? C27 C25 C29 O17 177.3(6) . . . . ? N6 C25 C29 O17 -4.8(9) . . . . ? C27 C25 C29 C28 -3.5(8) . . . . ? N6 C25 C29 C28 174.4(5) . . . . ? C25 C27 C30 C26 1.3(9) . . . . ? C25 C27 C30 N5 -179.4(5) . . . . ? C28 C26 C30 C27 -1.9(9) . . . . ? C28 C26 C30 N5 178.8(5) . . . . ? C61 C32 C33 C35 0.2(12) . . . . ? C32 C33 C35 C36 -1.8(13) . . . . ? C61 C34 C36 C35 -1.4(13) . . . . ? C33 C35 C36 C34 2.5(14) . . . . ? C39 C37 C38 C41 0.8(11) . . . . ? C43 C37 C38 C41 -176.4(7) . . . . ? C38 C37 C39 C42 0.4(11) . . . . ? C43 C37 C39 C42 177.5(7) . . . . ? C42 C40 C41 C38 0.2(17) . . . . ? C37 C38 C41 C40 -1.1(14) . . . . ? C41 C40 C42 C39 0.9(17) . . . . ? C37 C39 C42 C40 -1.2(14) . . . . ? C39 C37 C43 N3 45.9(8) . . . . ? C38 C37 C43 N3 -137.0(6) . . . . ? C16 C18 C46 O15 165.3(7) . . . . ? C13 C18 C46 O15 -13.1(9) . . . . ? C16 C18 C46 N2 -15.5(11) . . . . ? C13 C18 C46 N2 166.0(6) . . . . ? O1 C47 C48 N10 -92.4(8) . . . . ? N2 C50 C51 C53 -80.7(9) . . . . ? N2 C50 C51 C52 100.1(8) . . . . ? C53 C51 C52 C58 0.8(13) . . . . ? C50 C51 C52 C58 -180.0(9) . . . . ? C52 C51 C53 C56 -1.1(11) . . . . ? C50 C51 C53 C56 179.8(7) . . . . ? C51 C53 C56 C57 0.7(14) . . . . ? C53 C56 C57 C58 0(2) . . . . ? C56 C57 C58 C52 0(3) . . . . ? C51 C52 C58 C57 0(2) . . . . ? N10 C55 C59 O2 -65.0(8) . . . . ? C5 C3 C60 O2 179.2(6) . . . . ? C5 C3 C60 C2 1.6(10) . . . . ? C6 C2 C60 O2 -179.7(5) . . . . ? C62 C2 C60 O2 -0.8(8) . . . . ? C6 C2 C60 C3 -2.1(9) . . . . ? C62 C2 C60 C3 176.9(5) . . . . ? C33 C32 C61 C34 0.9(10) . . . . ? C33 C32 C61 C63 179.7(6) . . . . ? C36 C34 C61 C32 -0.2(10) . . . . ? C36 C34 C61 C63 -179.0(7) . . . . ? C6 C2 C62 O19 17.5(8) . . . . ? C60 C2 C62 O19 -161.5(5) . . . . ? C6 C2 C62 N3 -161.4(6) . . . . ? C60 C2 C62 N3 19.7(9) . . . . ? C32 C61 C63 N10 42.6(9) . . . . ? C34 C61 C63 N10 -138.7(7) . . . . ? C20 C21 N1 O25 -3.9(9) . . . . ? C24 C21 N1 O25 176.0(6) . . . . ? C20 C21 N1 O26 175.8(6) . . . . ? C24 C21 N1 O26 -4.4(9) . . . . ? O15 C46 N2 C50 -2.0(11) . . . . ? C18 C46 N2 C50 178.8(7) . . . . ? C51 C50 N2 C46 -154.0(7) . . . . ? O19 C62 N3 C43 7.4(9) . . . . ? C2 C62 N3 C43 -173.8(5) . . . . ? C37 C43 N3 C62 -122.1(6) . . . . ? C7 C11 N4 O8 178.0(7) . . . . ? C12 C11 N4 O8 1.5(11) . . . . ? C7 C11 N4 O7 1.4(11) . . . . ? C12 C11 N4 O7 -175.0(7) . . . . ? C27 C30 N5 O10 6.6(10) . . . . ? C26 C30 N5 O10 -174.1(6) . . . . ? C27 C30 N5 O9 -170.1(7) . . . . ? C26 C30 N5 O9 9.2(10) . . . . ? C27 C25 N6 O11 -0.4(10) . . . . ? C29 C25 N6 O11 -178.4(8) . . . . ? C27 C25 N6 O12 -178.5(8) . . . . ? C29 C25 N6 O12 3.5(11) . . . . ? C20 C19 N7 O13 157.3(5) . . . . ? C22 C19 N7 O13 -22.0(8) . . . . ? C20 C19 N7 O22 -20.9(8) . . . . ? C22 C19 N7 O22 159.8(5) . . . . ? C26 C28 N8 O18 165.9(5) . . . . ? C29 C28 N8 O18 -14.1(8) . . . . ? C26 C28 N8 O21 -12.1(8) . . . . ? C29 C28 N8 O21 167.9(6) . . . . ? C12 C9 N9 O24 5.2(9) . . . . ? C10 C9 N9 O24 -174.0(6) . . . . ? C12 C9 N9 O23 -176.1(6) . . . . ? C10 C9 N9 O23 4.6(9) . . . . ? C59 C55 N10 C63 -60.9(8) . . . . ? C59 C55 N10 C48 173.2(6) . . . . ? C61 C63 N10 C55 91.8(7) . . . . ? C61 C63 N10 C48 -146.9(7) . . . . ? C47 C48 N10 C55 177.9(6) . . . . ? C47 C48 N10 C63 53.6(10) . . . . ? C24 C23 N11 O4 86.7(9) . . . . ? C22 C23 N11 O4 -95.2(8) . . . . ? C24 C23 N11 O3 -93.9(8) . . . . ? C22 C23 N11 O3 84.3(8) . . . . ? C7 C8 N12 O6 -165.5(7) . . . . ? C10 C8 N12 O6 15.5(9) . . . . ? C7 C8 N12 O5 10.5(9) . . . . ? C10 C8 N12 O5 -168.5(6) . . . . ? C18 C16 O1 C47 173.7(7) . . . . ? C15 C16 O1 C47 -8.4(11) . . . . ? C48 C47 O1 C16 -169.4(7) . . . . ? C3 C60 O2 C59 17.0(8) . . . . ? C2 C60 O2 C59 -165.4(5) . . . . ? C55 C59 O2 C60 158.0(5) . . . . ? O22 N7 O13 Nd1 -155.5(4) . . . . ? C19 N7 O13 Nd1 26.3(8) . . . . ? O16 Nd1 O13 N7 83.5(6) . . . . ? O14 Nd1 O13 N7 -9.1(5) . . . . ? O17 Nd1 O13 N7 -145.9(5) . . . . ? O15 Nd1 O13 N7 32.8(6) . . . . ? O19 Nd1 O13 N7 -103.4(6) 1_545 . . . ? O20 Nd1 O13 N7 171.8(6) . . . . ? O18 Nd1 O13 N7 -56.5(6) . . . . ? O23 Nd1 O13 N7 122.2(5) . . . . ? C19 C22 O14 Nd1 23.7(9) . . . . ? C23 C22 O14 Nd1 -156.3(4) . . . . ? O16 Nd1 O14 C22 -89.4(6) . . . . ? O17 Nd1 O14 C22 119.8(5) . . . . ? O15 Nd1 O14 C22 -171.7(6) . . . . ? O19 Nd1 O14 C22 52.6(6) 1_545 . . . ? O20 Nd1 O14 C22 -16.7(6) . . . . ? O13 Nd1 O14 C22 -17.9(5) . . . . ? O18 Nd1 O14 C22 121.6(6) . . . . ? O23 Nd1 O14 C22 -123.9(5) . . . . ? N2 C46 O15 Nd1 109.9(7) . . . . ? C18 C46 O15 Nd1 -70.9(9) . . . . ? O16 Nd1 O15 C46 24.4(7) . . . . ? O14 Nd1 O15 C46 109.8(7) . . . . ? O17 Nd1 O15 C46 -108.8(7) . . . . ? O19 Nd1 O15 C46 -173.5(6) 1_545 . . . ? O20 Nd1 O15 C46 -46.7(7) . . . . ? O13 Nd1 O15 C46 72.1(7) . . . . ? O18 Nd1 O15 C46 -175.7(7) . . . . ? O23 Nd1 O15 C46 -37.0(7) . . . . ? C8 C10 O16 Nd1 164.6(6) . . . . ? C9 C10 O16 Nd1 -16.0(13) . . . . ? O14 Nd1 O16 C10 -138.9(9) . . . . ? O17 Nd1 O16 C10 15.9(10) . . . . ? O15 Nd1 O16 C10 -55.6(9) . . . . ? O19 Nd1 O16 C10 144.8(9) 1_545 . . . ? O20 Nd1 O16 C10 81.4(9) . . . . ? O13 Nd1 O16 C10 155.2(9) . . . . ? O18 Nd1 O16 C10 -86.0(9) . . . . ? O23 Nd1 O16 C10 14.5(9) . . . . ? C28 C29 O17 Nd1 38.7(9) . . . . ? C25 C29 O17 Nd1 -142.2(5) . . . . ? O16 Nd1 O17 C29 -178.6(5) . . . . ? O14 Nd1 O17 C29 -38.4(7) . . . . ? O15 Nd1 O17 C29 -107.1(6) . . . . ? O19 Nd1 O17 C29 31.5(6) 1_545 . . . ? O20 Nd1 O17 C29 113.3(6) . . . . ? O13 Nd1 O17 C29 72.1(6) . . . . ? O18 Nd1 O17 C29 -40.2(6) . . . . ? O23 Nd1 O17 C29 -177.3(6) . . . . ? O21 N8 O18 Nd1 170.7(5) . . . . ? C28 N8 O18 Nd1 -7.3(9) . . . . ? O16 Nd1 O18 N8 149.4(5) . . . . ? O14 Nd1 O18 N8 -154.5(6) . . . . ? O17 Nd1 O18 N8 24.2(6) . . . . ? O15 Nd1 O18 N8 116.0(6) . . . . ? O19 Nd1 O18 N8 -62.3(6) 1_545 . . . ? O20 Nd1 O18 N8 -13.1(7) . . . . ? O13 Nd1 O18 N8 -110.0(6) . . . . ? O23 Nd1 O18 N8 71.3(6) . . . . ? N3 C62 O19 Nd1 -94.1(10) . . . 1_565 ? C2 C62 O19 Nd1 87.1(11) . . . 1_565 ? C65 C64 O20 Nd1 114.1(8) . . . . ? O16 Nd1 O20 C64 31.9(7) . . . . ? O14 Nd1 O20 C64 -41.4(7) . . . . ? O17 Nd1 O20 C64 166.5(7) . . . . ? O15 Nd1 O20 C64 102.6(7) . . . . ? O19 Nd1 O20 C64 -113.1(7) 1_545 . . . ? O13 Nd1 O20 C64 -40.3(6) . . . . ? O18 Nd1 O20 C64 -159.0(6) . . . . ? O23 Nd1 O20 C64 92.7(7) . . . . ? O24 N9 O23 Nd1 176.6(5) . . . . ? C9 N9 O23 Nd1 -1.9(11) . . . . ? O16 Nd1 O23 N9 -3.2(7) . . . . ? O14 Nd1 O23 N9 37.2(8) . . . . ? O17 Nd1 O23 N9 177.9(8) . . . . ? O15 Nd1 O23 N9 89.3(8) . . . . ? O19 Nd1 O23 N9 -137.7(7) 1_545 . . . ? O20 Nd1 O23 N9 -98.3(8) . . . . ? O13 Nd1 O23 N9 -46.1(8) . . . . ? O18 Nd1 O23 N9 132.7(7) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.486 _refine_diff_density_min -0.606 _refine_diff_density_rms 0.080 #===END data_852908 _database_code_depnum_ccdc_archive 'CCDC 852908' #TrackingRef '- cif_Revision.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C59 H51 Eu N12 O26' _chemical_formula_weight 1496.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 '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 13.6916(11) _cell_length_b 15.9050(12) _cell_length_c 17.5187(13) _cell_angle_alpha 96.5600(10) _cell_angle_beta 109.3340(10) _cell_angle_gamma 114.1270(10) _cell_volume 3144.3(4) _cell_formula_units_Z 2 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.580 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1520 _exptl_absorpt_coefficient_mu 1.093 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7008 _exptl_absorpt_correction_T_max 0.8192 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 16559 _diffrn_reflns_av_R_equivalents 0.0284 _diffrn_reflns_av_sigmaI/netI 0.0665 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 25.50 _reflns_number_total 11520 _reflns_number_gt 8184 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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.Standard DFIX restraint was used for the distance of the disordered atoms H5O and O5. ; _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^)+(0.0487P)^2^+0.8839P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11520 _refine_ls_number_parameters 876 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0776 _refine_ls_R_factor_gt 0.0498 _refine_ls_wR_factor_ref 0.1184 _refine_ls_wR_factor_gt 0.1025 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Eu1 Eu 0.96297(2) 0.690071(18) 0.729834(17) 0.05094(10) Uani 1 1 d . . . C1 C 1.0614(4) 0.8947(3) 0.6636(3) 0.0511(12) Uani 1 1 d . . . C2 C 1.1699(4) 0.9637(3) 0.6636(3) 0.0515(12) Uani 1 1 d . . . C3 C 1.1847(4) 1.0442(3) 0.6395(3) 0.0563(13) Uani 1 1 d . . . H3 H 1.2571 1.0861 0.6411 0.068 Uiso 1 1 calc R . . C4 C 1.0910(5) 1.0637(4) 0.6124(3) 0.0600(14) Uani 1 1 d . . . C5 C 0.9845(5) 1.0034(4) 0.6116(3) 0.0597(13) Uani 1 1 d . . . H5 H 0.9223 1.0172 0.5940 0.072 Uiso 1 1 calc R . . C6 C 0.9711(4) 0.9220(3) 0.6372(3) 0.0533(12) Uani 1 1 d . . . C7 C 1.2074(5) -0.0401(5) 0.8804(4) 0.0811(19) Uani 1 1 d . . . H7 H 1.1966 -0.1022 0.8777 0.097 Uiso 1 1 calc R . . C8 C 1.1152(5) -0.0210(4) 0.8738(3) 0.0652(15) Uani 1 1 d . . . C9 C 1.1311(6) 0.0717(5) 0.8796(4) 0.088(2) Uani 1 1 d . . . C10 C 1.3148(6) 0.0317(7) 0.8907(4) 0.111(3) Uani 1 1 d . . . H10 H 1.3773 0.0192 0.8971 0.134 Uiso 1 1 calc R . . C11 C 1.3273(7) 0.1207(7) 0.8914(5) 0.121(4) Uani 1 1 d . . . H11 H 1.3988 0.1682 0.8959 0.145 Uiso 1 1 calc R . . C12 C 1.2419(8) 0.1443(5) 0.8858(5) 0.114(3) Uani 1 1 d . . . H12 H 1.2542 0.2063 0.8860 0.136 Uiso 1 1 calc R . . C13 C 0.5888(4) 0.4900(4) 0.6942(3) 0.0539(12) Uani 1 1 d . . . C14 C 0.7123(4) 0.5507(3) 0.7439(3) 0.0489(12) Uani 1 1 d . . . C15 C 0.7562(4) 0.5242(3) 0.8191(3) 0.0494(12) Uani 1 1 d . . . C16 C 0.6867(4) 0.4469(3) 0.8387(3) 0.0546(13) Uani 1 1 d . . . H16 H 0.7187 0.4328 0.8881 0.065 Uiso 1 1 calc R . . C17 C 0.5713(4) 0.3914(3) 0.7856(3) 0.0530(12) Uani 1 1 d . . . C18 C 0.5195(4) 0.4119(3) 0.7125(3) 0.0543(13) Uani 1 1 d . . . H18 H 0.4401 0.3736 0.6770 0.065 Uiso 1 1 calc R . . C19 C 1.2331(4) 0.7094(3) 0.8215(3) 0.0469(11) Uani 1 1 d . . . C20 C 1.3462(5) 0.6586(3) 0.7615(3) 0.0574(13) Uani 1 1 d . . . H20 H 1.3566 0.6384 0.7143 0.069 Uiso 1 1 calc R . . C21 C 1.3200(4) 0.7213(4) 0.9017(3) 0.0566(13) Uani 1 1 d . . . C22 C 1.4219(5) 0.6692(4) 0.8408(4) 0.0603(14) Uani 1 1 d . . . C23 C 1.4100(5) 0.7016(4) 0.9119(4) 0.0640(14) Uani 1 1 d . . . H23 H 1.4626 0.7097 0.9655 0.077 Uiso 1 1 calc R . . C24 C 1.2541(4) 0.6782(3) 0.7525(3) 0.0486(12) Uani 1 1 d . . . C25 C 0.7030(6) 0.3876(4) 0.5846(4) 0.0820(18) Uani 1 1 d . . . H25 H 0.7490 0.4411 0.5720 0.098 Uiso 1 1 calc R . . C26 C 0.7522(4) 0.3704(3) 0.6603(3) 0.0544(13) Uani 1 1 d . . . C27 C 0.6809(5) 0.2893(4) 0.6776(4) 0.0576(13) Uani 1 1 d . . . C28 C 0.5646(5) 0.2292(4) 0.6205(5) 0.0836(19) Uani 1 1 d . . . H28 H 0.5171 0.1751 0.6316 0.100 Uiso 1 1 calc R . . C29 C 0.6756(6) 0.1822(4) 0.7668(5) 0.085(2) Uani 1 1 d . . . H29A H 0.6439 0.1308 0.7158 0.102 Uiso 1 1 calc R . . H29B H 0.6120 0.1761 0.7826 0.102 Uiso 1 1 calc R . . C30 C 0.8748(4) 0.4417(3) 0.7189(3) 0.0507(12) Uani 1 1 d . . . C31 C 1.0528(4) 0.4815(4) 0.8452(3) 0.0653(15) Uani 1 1 d . . . H31A H 1.0498 0.4839 0.8999 0.078 Uiso 1 1 calc R . . H31B H 1.0763 0.5457 0.8387 0.078 Uiso 1 1 calc R . . C32 C 1.1448(4) 0.4530(3) 0.8438(3) 0.0550(13) Uani 1 1 d . . . C33 C 1.1502(6) 0.4202(4) 0.7700(4) 0.0800(18) Uani 1 1 d . . . H33 H 1.0947 0.4136 0.7184 0.096 Uiso 1 1 calc R . . C34 C 1.2298(5) 0.4628(4) 0.9190(4) 0.0788(17) Uani 1 1 d . . . H34 H 1.2273 0.4842 0.9697 0.095 Uiso 1 1 calc R . . C35 C 0.7706(7) 0.1766(5) 0.8373(5) 0.101(2) Uani 1 1 d . . . H35A H 0.8033 0.2304 0.8866 0.122 Uiso 1 1 calc R . . H35B H 0.7351 0.1179 0.8520 0.122 Uiso 1 1 calc R . . C36 C 0.8243(6) 0.0927(4) 0.7471(4) 0.0805(18) Uani 1 1 d . . . H36A H 0.7582 0.0388 0.7485 0.097 Uiso 1 1 calc R . . H36B H 0.8870 0.0759 0.7559 0.097 Uiso 1 1 calc R . . C37 C 0.7873(5) 0.1084(4) 0.6611(4) 0.0680(15) Uani 1 1 d . . . C38 C 0.8545(6) 0.1905(5) 0.6472(4) 0.0785(17) Uani 1 1 d . . . H38 H 0.9239 0.2373 0.6918 0.094 Uiso 1 1 calc R . . C39 C 0.6872(6) 0.0385(5) 0.5934(5) 0.094(2) Uani 1 1 d . . . H39 H 0.6412 -0.0194 0.6006 0.113 Uiso 1 1 calc R . . C40 C 0.8230(8) 0.2062(6) 0.5696(6) 0.101(2) Uani 1 1 d . . . H40 H 0.8700 0.2635 0.5622 0.121 Uiso 1 1 calc R . . C41 C 0.7244(10) 0.1388(9) 0.5043(6) 0.118(3) Uani 1 1 d . . . H41 H 0.7034 0.1499 0.4518 0.142 Uiso 1 1 calc R . . C42 C 0.6544(8) 0.0542(7) 0.5137(5) 0.118(3) Uani 1 1 d . . . H42 H 0.5860 0.0078 0.4681 0.142 Uiso 1 1 calc R . . C43 C 0.8018(5) -0.1775(4) 0.8509(5) 0.099(2) Uani 1 1 d . . . H43A H 0.7836 -0.2302 0.8056 0.119 Uiso 1 1 calc R . . H43B H 0.8072 -0.1992 0.9010 0.119 Uiso 1 1 calc R . . C44 C 1.0008(5) -0.1068(4) 0.8578(3) 0.0602(14) Uani 1 1 d . . . C46 C 1.2375(8) 0.3970(6) 0.7722(6) 0.116(3) Uani 1 1 d . . . H46 H 1.2387 0.3724 0.7220 0.140 Uiso 1 1 calc R . . C47 C 1.3227(8) 0.4099(6) 0.8483(8) 0.124(3) Uani 1 1 d . . . H47 H 1.3834 0.3968 0.8496 0.149 Uiso 1 1 calc R . . C48 C 1.3178(6) 0.4416(6) 0.9206(6) 0.103(2) Uani 1 1 d . . . H48 H 1.3745 0.4493 0.9721 0.124 Uiso 1 1 calc R . . C49 C 0.5882(8) 0.3279(6) 0.5276(5) 0.110(3) Uani 1 1 d . . . H49 H 0.5574 0.3399 0.4768 0.132 Uiso 1 1 calc R . . C50 C 0.5207(7) 0.2513(6) 0.5469(5) 0.113(3) Uani 1 1 d . . . H50 H 0.4423 0.2122 0.5093 0.136 Uiso 1 1 calc R . . C51 C 0.6940(4) -0.0998(3) 0.8893(2) 0.0771(17) Uani 1 1 d G . . H51 H 0.7447 -0.0828 0.9458 0.093 Uiso 1 1 calc R . . C52 C 0.7068(3) -0.1511(3) 0.8269(3) 0.0624(14) Uani 1 1 d G . . C53 C 0.6309(5) -0.1764(3) 0.7425(3) 0.107(3) Uani 1 1 d G . . H53 H 0.6395 -0.2107 0.7008 0.128 Uiso 1 1 calc R . . C59 C 0.5422(4) -0.1505(4) 0.7205(3) 0.162(6) Uani 1 1 d G . . H59 H 0.4914 -0.1674 0.6641 0.194 Uiso 1 1 calc R . . C58 C 0.5293(4) -0.0992(4) 0.7829(5) 0.167(6) Uani 1 1 d G . . H58 H 0.4699 -0.0818 0.7682 0.200 Uiso 1 1 calc R . . C60 C 0.6052(5) -0.0738(3) 0.8673(4) 0.128(3) Uani 1 1 d G . . H60 H 0.5966 -0.0395 0.9090 0.154 Uiso 1 1 calc R . . C54 C 0.9582(9) 0.1870(6) 0.8975(5) 0.121(3) Uani 1 1 d . . . H54A H 0.9847 0.2468 0.9385 0.145 Uiso 1 1 calc R . . H54B H 0.9228 0.1347 0.9194 0.145 Uiso 1 1 calc R . . C55 C 0.8564(6) 0.6432(5) 0.5087(4) 0.101(2) Uani 1 1 d . . . H55A H 0.9350 0.6968 0.5284 0.121 Uiso 1 1 calc R . . H55B H 0.8010 0.6616 0.4744 0.121 Uiso 1 1 calc R . . C56 C 0.8478(8) 0.5597(7) 0.4579(5) 0.139(3) Uani 1 1 d . . . H56A H 0.9021 0.5412 0.4921 0.208 Uiso 1 1 calc R . . H56B H 0.8664 0.5751 0.4114 0.208 Uiso 1 1 calc R . . H56C H 0.7691 0.5074 0.4367 0.208 Uiso 1 1 calc R . . C57 C 1.0606(8) 0.1856(5) 0.8902(5) 0.131(4) Uani 1 1 d . . . H57A H 1.0715 0.2091 0.8434 0.157 Uiso 1 1 calc R . . H57B H 1.1307 0.2269 0.9416 0.157 Uiso 1 1 calc R . . N1 N 1.1770(4) 0.6645(3) 0.6671(3) 0.0580(11) Uani 1 1 d . . . N2 N 1.3046(5) 0.7542(5) 0.9766(3) 0.0793(15) Uani 1 1 d . . . N3 N 0.5293(5) 0.5127(4) 0.6201(3) 0.0794(14) Uani 1 1 d . . . N4 N 0.8783(4) 0.5799(3) 0.8806(3) 0.0606(11) Uani 1 1 d . . . N5 N 0.4998(5) 0.3084(4) 0.8064(4) 0.0772(14) Uani 1 1 d . . . N6 N 1.2728(4) 0.9484(4) 0.6901(3) 0.0699(13) Uani 1 1 d . . . N7 N 1.1063(6) 1.1490(4) 0.5848(4) 0.0862(16) Uani 1 1 d . . . N8 N 0.8551(4) 0.8605(3) 0.6341(3) 0.0675(12) Uani 1 1 d . . . N9 N 1.5171(5) 0.6455(4) 0.8507(4) 0.0788(14) Uani 1 1 d . . . N10 N 0.8655(5) 0.1780(3) 0.8170(3) 0.0789(14) Uani 1 1 d . . . N11 N 0.9353(3) 0.4163(3) 0.7796(3) 0.0583(11) Uani 1 1 d . . . H11A H 0.9028 0.3574 0.7801 0.070 Uiso 1 1 calc R . . N12 N 0.9158(4) -0.0951(3) 0.8680(3) 0.0807(15) Uani 1 1 d . . . H12' H 0.9271 -0.0377 0.8851 0.097 Uiso 1 1 calc R . . O1 O 0.7755(3) 0.6205(2) 0.7247(2) 0.0616(9) Uani 1 1 d . . . O2 O 1.0765(3) 0.6530(3) 0.6516(2) 0.0640(9) Uani 1 1 d . . . O3 O 1.1504(3) 0.7271(2) 0.8187(2) 0.0533(8) Uani 1 1 d . . . O4 O 0.9202(3) 0.5243(2) 0.7112(2) 0.0651(10) Uani 1 1 d . . . O5 O 0.8314(3) 0.6225(3) 0.5805(2) 0.0713(10) Uani 1 1 d D . . O6 O 1.0498(3) 0.8197(2) 0.6858(2) 0.0651(10) Uani 1 1 d . . . O7 O 0.9523(3) 0.6387(2) 0.8633(2) 0.0646(10) Uani 1 1 d . . . O8 O 0.9898(3) -0.1886(2) 0.8366(2) 0.0660(10) Uani 1 1 d . . . O9 O 1.2126(4) 0.6638(3) 0.6123(2) 0.0899(13) Uani 1 1 d . . . O10 O 1.3587(6) 0.8365(4) 1.0134(4) 0.138(2) Uani 1 1 d . . . O11 O 1.2362(5) 0.6922(4) 0.9964(3) 0.125(2) Uani 1 1 d . . . O12 O 0.9052(4) 0.5650(4) 0.9493(3) 0.1125(19) Uani 1 1 d . . . O13 O 0.4012(4) 0.2537(3) 0.7549(3) 0.1123(17) Uani 1 1 d . . . O14 O 0.5848(5) 0.5681(4) 0.5908(3) 0.142(2) Uani 1 1 d . . . O15 O 1.2620(4) 0.8710(4) 0.6984(4) 0.127(2) Uani 1 1 d . . . O16 O 1.3673(3) 1.0126(3) 0.7008(3) 0.0972(14) Uani 1 1 d . . . O17 O 1.2011(4) 1.1990(4) 0.5842(4) 0.128(2) Uani 1 1 d . . . O18 O 1.0214(5) 1.1619(4) 0.5582(4) 0.135(2) Uani 1 1 d . . . O19 O 0.7774(4) 0.8770(4) 0.6009(4) 0.142(2) Uani 1 1 d . . . O20 O 0.8396(4) 0.7929(3) 0.6636(3) 0.0996(15) Uani 1 1 d . . . O21 O 0.4253(4) 0.4729(5) 0.5886(4) 0.161(3) Uani 1 1 d . . . O22 O 1.5233(4) 0.6134(4) 0.7875(4) 0.1078(16) Uani 1 1 d . . . O23 O 1.5864(4) 0.6604(4) 0.9221(4) 0.1080(16) Uani 1 1 d . . . O24 O 0.5429(4) 0.2999(4) 0.8760(4) 0.136(2) Uani 1 1 d . . . O25 O 0.7297(3) 0.2746(2) 0.7531(2) 0.0668(10) Uani 1 1 d . . . O26 O 1.0411(4) 0.0887(3) 0.8764(3) 0.1080(17) Uani 1 1 d . . . H5O H 0.762(3) 0.583(3) 0.586(3) 0.050(13) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu1 0.05198(16) 0.04650(16) 0.06623(18) 0.02844(12) 0.03152(13) 0.02549(12) C1 0.056(3) 0.047(3) 0.052(3) 0.021(2) 0.026(3) 0.022(2) C2 0.051(3) 0.053(3) 0.060(3) 0.026(2) 0.025(3) 0.029(2) C3 0.058(3) 0.038(3) 0.065(3) 0.022(2) 0.026(3) 0.013(2) C4 0.073(4) 0.043(3) 0.069(4) 0.027(3) 0.030(3) 0.029(3) C5 0.066(4) 0.061(4) 0.063(3) 0.025(3) 0.028(3) 0.038(3) C6 0.051(3) 0.052(3) 0.065(3) 0.022(3) 0.032(3) 0.024(2) C7 0.053(4) 0.076(4) 0.083(4) 0.004(3) 0.028(3) 0.009(3) C8 0.059(4) 0.056(4) 0.051(3) 0.011(3) 0.012(3) 0.011(3) C9 0.087(5) 0.063(4) 0.070(4) 0.033(3) 0.002(4) 0.017(4) C10 0.062(4) 0.131(7) 0.086(5) 0.010(5) 0.032(4) 0.002(5) C11 0.074(5) 0.117(7) 0.084(5) 0.035(5) 0.007(4) -0.014(5) C12 0.099(6) 0.075(5) 0.096(5) 0.047(4) 0.004(5) 0.002(5) C13 0.057(3) 0.054(3) 0.059(3) 0.020(3) 0.025(3) 0.032(3) C14 0.044(3) 0.044(3) 0.060(3) 0.013(2) 0.024(2) 0.020(2) C15 0.048(3) 0.052(3) 0.050(3) 0.014(2) 0.023(2) 0.024(2) C16 0.062(3) 0.056(3) 0.054(3) 0.020(2) 0.032(3) 0.028(3) C17 0.051(3) 0.050(3) 0.064(3) 0.019(3) 0.032(3) 0.022(3) C18 0.043(3) 0.047(3) 0.066(3) 0.005(3) 0.025(3) 0.017(2) C19 0.050(3) 0.038(3) 0.059(3) 0.018(2) 0.030(3) 0.020(2) C20 0.067(3) 0.055(3) 0.067(4) 0.023(3) 0.042(3) 0.033(3) C21 0.054(3) 0.061(3) 0.052(3) 0.011(2) 0.021(3) 0.026(3) C22 0.057(3) 0.055(3) 0.082(4) 0.020(3) 0.037(3) 0.032(3) C23 0.052(3) 0.069(4) 0.067(4) 0.016(3) 0.018(3) 0.032(3) C24 0.050(3) 0.044(3) 0.055(3) 0.018(2) 0.025(3) 0.022(2) C25 0.099(5) 0.071(4) 0.066(4) 0.015(3) 0.012(4) 0.050(4) C26 0.058(3) 0.045(3) 0.061(3) 0.008(2) 0.016(3) 0.033(3) C27 0.056(3) 0.045(3) 0.076(4) 0.009(3) 0.026(3) 0.031(3) C28 0.059(4) 0.057(4) 0.118(6) 0.003(4) 0.029(4) 0.025(3) C29 0.100(5) 0.049(4) 0.140(6) 0.041(4) 0.088(5) 0.033(3) C30 0.063(3) 0.043(3) 0.057(3) 0.020(2) 0.030(3) 0.029(3) C31 0.060(3) 0.065(4) 0.064(3) 0.014(3) 0.019(3) 0.030(3) C32 0.052(3) 0.050(3) 0.062(3) 0.022(3) 0.025(3) 0.021(2) C33 0.082(4) 0.091(5) 0.070(4) 0.021(3) 0.040(4) 0.038(4) C34 0.072(4) 0.100(5) 0.071(4) 0.036(3) 0.029(3) 0.044(4) C35 0.176(8) 0.067(4) 0.126(6) 0.063(4) 0.104(6) 0.075(5) C36 0.109(5) 0.058(4) 0.078(4) 0.015(3) 0.028(4) 0.051(4) C37 0.079(4) 0.053(4) 0.081(4) 0.016(3) 0.033(4) 0.041(3) C38 0.082(4) 0.080(5) 0.090(5) 0.021(4) 0.047(4) 0.046(4) C39 0.089(5) 0.076(5) 0.088(5) -0.001(4) 0.025(4) 0.029(4) C40 0.127(7) 0.097(6) 0.117(7) 0.038(5) 0.076(6) 0.065(5) C41 0.168(9) 0.155(9) 0.095(6) 0.048(7) 0.071(7) 0.116(8) C42 0.114(7) 0.124(8) 0.085(6) -0.003(5) 0.014(5) 0.060(6) C43 0.075(4) 0.060(4) 0.190(8) 0.044(4) 0.076(5) 0.037(3) C44 0.050(3) 0.057(4) 0.072(4) 0.022(3) 0.025(3) 0.023(3) C46 0.108(6) 0.125(7) 0.139(8) 0.021(6) 0.072(6) 0.064(6) C47 0.095(6) 0.114(7) 0.201(11) 0.048(7) 0.077(7) 0.072(5) C48 0.072(5) 0.117(6) 0.138(7) 0.065(5) 0.037(5) 0.060(5) C49 0.123(7) 0.090(6) 0.076(5) -0.005(4) -0.013(5) 0.066(5) C50 0.075(5) 0.099(6) 0.114(7) -0.017(5) -0.010(5) 0.048(5) C51 0.083(4) 0.081(4) 0.087(4) 0.031(3) 0.044(4) 0.048(4) C52 0.059(3) 0.052(3) 0.086(4) 0.022(3) 0.043(3) 0.025(3) C53 0.111(6) 0.092(5) 0.087(5) 0.030(4) 0.051(5) 0.012(5) C59 0.075(6) 0.152(10) 0.177(10) 0.105(8) -0.001(6) 0.008(6) C58 0.071(6) 0.139(9) 0.308(17) 0.149(11) 0.068(9) 0.054(6) C60 0.123(7) 0.103(6) 0.239(11) 0.073(7) 0.127(8) 0.079(6) C54 0.194(10) 0.092(6) 0.091(6) 0.014(4) 0.044(6) 0.094(6) C55 0.093(5) 0.097(5) 0.081(5) 0.051(4) 0.016(4) 0.028(4) C56 0.131(7) 0.165(9) 0.089(6) -0.007(6) 0.025(5) 0.070(7) C57 0.155(8) 0.049(4) 0.122(7) 0.003(4) -0.009(6) 0.047(5) N1 0.064(3) 0.065(3) 0.059(3) 0.022(2) 0.035(2) 0.035(2) N2 0.068(3) 0.096(5) 0.062(3) 0.008(3) 0.022(3) 0.037(3) N3 0.068(4) 0.085(4) 0.076(4) 0.033(3) 0.021(3) 0.032(3) N4 0.054(3) 0.069(3) 0.055(3) 0.022(2) 0.025(2) 0.023(2) N5 0.066(3) 0.064(3) 0.098(4) 0.033(3) 0.042(3) 0.019(3) N6 0.056(3) 0.067(3) 0.089(3) 0.037(3) 0.032(3) 0.027(3) N7 0.095(4) 0.064(3) 0.119(5) 0.054(3) 0.050(4) 0.043(3) N8 0.058(3) 0.065(3) 0.092(4) 0.031(3) 0.039(3) 0.032(3) N9 0.070(4) 0.078(4) 0.105(5) 0.034(3) 0.039(3) 0.047(3) N10 0.120(4) 0.062(3) 0.072(3) 0.020(3) 0.043(3) 0.057(3) N11 0.051(2) 0.048(3) 0.067(3) 0.025(2) 0.015(2) 0.021(2) N12 0.065(3) 0.042(3) 0.141(5) 0.022(3) 0.050(3) 0.027(2) O1 0.053(2) 0.062(2) 0.085(3) 0.0418(19) 0.0382(19) 0.0274(18) O2 0.063(2) 0.076(3) 0.057(2) 0.0221(18) 0.0240(19) 0.036(2) O3 0.054(2) 0.059(2) 0.062(2) 0.0207(17) 0.0307(17) 0.0343(17) O4 0.084(3) 0.047(2) 0.066(2) 0.0285(18) 0.032(2) 0.0293(19) O5 0.069(3) 0.074(3) 0.071(3) 0.039(2) 0.027(2) 0.031(2) O6 0.060(2) 0.053(2) 0.093(3) 0.041(2) 0.037(2) 0.0276(18) O7 0.057(2) 0.061(2) 0.066(2) 0.0255(18) 0.0269(19) 0.0156(18) O8 0.061(2) 0.050(2) 0.095(3) 0.0162(19) 0.040(2) 0.0279(18) O9 0.101(3) 0.137(4) 0.067(3) 0.039(2) 0.053(3) 0.072(3) O10 0.171(6) 0.096(4) 0.124(4) -0.014(3) 0.074(4) 0.045(4) O11 0.119(4) 0.140(5) 0.098(4) 0.010(3) 0.069(3) 0.033(4) O12 0.074(3) 0.150(5) 0.062(3) 0.052(3) 0.017(2) 0.011(3) O13 0.085(3) 0.072(3) 0.119(4) 0.024(3) 0.034(3) -0.008(3) O14 0.105(4) 0.118(4) 0.119(4) 0.079(4) -0.006(3) 0.009(3) O15 0.080(3) 0.091(4) 0.247(7) 0.104(4) 0.074(4) 0.055(3) O16 0.057(3) 0.081(3) 0.156(4) 0.053(3) 0.045(3) 0.030(2) O17 0.093(4) 0.098(4) 0.186(5) 0.102(4) 0.045(4) 0.034(3) O18 0.154(5) 0.134(5) 0.235(7) 0.137(5) 0.129(5) 0.114(4) O19 0.069(3) 0.137(5) 0.259(7) 0.122(5) 0.072(4) 0.064(3) O20 0.076(3) 0.102(4) 0.151(4) 0.079(3) 0.068(3) 0.042(3) O21 0.057(3) 0.276(8) 0.148(5) 0.135(5) 0.030(3) 0.069(4) O22 0.111(4) 0.122(4) 0.132(4) 0.028(3) 0.067(3) 0.082(3) O23 0.087(3) 0.136(4) 0.128(4) 0.052(3) 0.037(3) 0.079(3) O24 0.091(4) 0.141(5) 0.145(5) 0.100(4) 0.044(4) 0.018(3) O25 0.070(2) 0.048(2) 0.087(3) 0.0273(19) 0.040(2) 0.0256(19) O26 0.102(4) 0.040(2) 0.132(4) 0.022(2) 0.003(3) 0.027(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu1 O6 2.287(3) . ? Eu1 O3 2.295(3) . ? Eu1 O1 2.308(3) . ? Eu1 O8 2.344(4) 1_565 ? Eu1 O4 2.411(3) . ? Eu1 O5 2.428(4) . ? Eu1 O2 2.572(4) . ? Eu1 O7 2.593(3) . ? Eu1 O20 2.875(5) . ? Eu1 H5O 2.72(4) . ? C1 O6 1.260(5) . ? C1 C6 1.428(7) . ? C1 C2 1.442(6) . ? C2 C3 1.351(6) . ? C2 N6 1.460(6) . ? C3 C4 1.386(7) . ? C3 H3 0.9300 . ? C4 C5 1.374(7) . ? C4 N7 1.449(6) . ? C5 C6 1.379(7) . ? C5 H5 0.9300 . ? C6 N8 1.465(6) . ? C7 C10 1.379(8) . ? C7 C8 1.386(8) . ? C7 H7 0.9300 . ? C8 C9 1.386(8) . ? C8 C44 1.506(7) . ? C9 O26 1.351(8) . ? C9 C12 1.441(10) . ? C10 C11 1.353(11) . ? C10 H10 0.9300 . ? C11 C12 1.345(12) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C18 1.369(6) . ? C13 C14 1.431(7) . ? C13 N3 1.458(7) . ? C14 O1 1.260(5) . ? C14 C15 1.443(7) . ? C15 C16 1.375(6) . ? C15 N4 1.455(6) . ? C16 C17 1.357(7) . ? C16 H16 0.9300 . ? C17 C18 1.390(7) . ? C17 N5 1.457(6) . ? C18 H18 0.9300 . ? C19 O3 1.262(5) . ? C19 C24 1.414(6) . ? C19 C21 1.440(7) . ? C20 C22 1.372(7) . ? C20 C24 1.382(7) . ? C20 H20 0.9300 . ? C21 C23 1.354(7) . ? C21 N2 1.469(7) . ? C22 C23 1.378(7) . ? C22 N9 1.462(7) . ? C23 H23 0.9300 . ? C24 N1 1.446(6) . ? C25 C49 1.376(9) . ? C25 C26 1.389(7) . ? C25 H25 0.9300 . ? C26 C27 1.402(7) . ? C26 C30 1.482(7) . ? C27 O25 1.365(6) . ? C27 C28 1.391(8) . ? C28 C50 1.381(10) . ? C28 H28 0.9300 . ? C29 O25 1.440(6) . ? C29 C35 1.509(9) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 O4 1.248(5) . ? C30 N11 1.329(6) . ? C31 N11 1.457(6) . ? C31 C32 1.509(7) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 C33 1.374(7) . ? C32 C34 1.380(7) . ? C33 C46 1.378(9) . ? C33 H33 0.9300 . ? C34 C48 1.370(9) . ? C34 H34 0.9300 . ? C35 N10 1.450(8) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 N10 1.482(7) . ? C36 C37 1.508(8) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 C38 1.360(8) . ? C37 C39 1.377(8) . ? C38 C40 1.370(9) . ? C38 H38 0.9300 . ? C39 C42 1.405(10) . ? C39 H39 0.9300 . ? C40 C41 1.339(10) . ? C40 H40 0.9300 . ? C41 C42 1.362(11) . ? C41 H41 0.9300 . ? C42 H42 0.9300 . ? C43 C52 1.473(7) . ? C43 N12 1.474(7) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 O8 1.244(6) . ? C44 N12 1.314(6) . ? C46 C47 1.375(11) . ? C46 H46 0.9300 . ? C47 C48 1.342(11) . ? C47 H47 0.9300 . ? C48 H48 0.9300 . ? C49 C50 1.353(11) . ? C49 H49 0.9300 . ? C50 H50 0.9300 . ? C51 C52 1.3900 . ? C51 C60 1.3900 . ? C51 H51 0.9300 . ? C52 C53 1.3900 . ? C53 C59 1.3900 . ? C53 H53 0.9300 . ? C59 C58 1.3900 . ? C59 H59 0.9300 . ? C58 C60 1.3900 . ? C58 H58 0.9300 . ? C60 H60 0.9300 . ? C54 C57 1.457(11) . ? C54 N10 1.497(9) . ? C54 H54A 0.9700 . ? C54 H54B 0.9700 . ? C55 O5 1.448(7) . ? C55 C56 1.450(10) . ? C55 H55A 0.9700 . ? C55 H55B 0.9700 . ? C56 H56A 0.9600 . ? C56 H56B 0.9600 . ? C56 H56C 0.9600 . ? C57 O26 1.429(7) . ? C57 H57A 0.9700 . ? C57 H57B 0.9700 . ? N1 O9 1.213(5) . ? N1 O2 1.239(5) . ? N2 O10 1.173(6) . ? N2 O11 1.228(7) . ? N3 O21 1.181(6) . ? N3 O14 1.198(6) . ? N4 O12 1.219(5) . ? N4 O7 1.219(5) . ? N5 O13 1.202(6) . ? N5 O24 1.216(6) . ? N6 O15 1.210(6) . ? N6 O16 1.212(5) . ? N7 O18 1.213(7) . ? N7 O17 1.218(6) . ? N8 O19 1.178(6) . ? N8 O20 1.218(5) . ? N9 O22 1.208(6) . ? N9 O23 1.218(6) . ? N11 H11A 0.8600 . ? N12 H12' 0.8600 . ? O5 H5O 0.948(19) . ? O8 Eu1 2.344(4) 1_545 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Eu1 O3 86.26(12) . . ? O6 Eu1 O1 128.16(12) . . ? O3 Eu1 O1 139.02(12) . . ? O6 Eu1 O8 81.29(13) . 1_565 ? O3 Eu1 O8 83.28(12) . 1_565 ? O1 Eu1 O8 81.47(12) . 1_565 ? O6 Eu1 O4 140.96(13) . . ? O3 Eu1 O4 85.70(12) . . ? O1 Eu1 O4 79.08(12) . . ? O8 Eu1 O4 135.28(12) 1_565 . ? O6 Eu1 O5 81.82(13) . . ? O3 Eu1 O5 139.69(13) . . ? O1 Eu1 O5 74.59(13) . . ? O8 Eu1 O5 131.95(14) 1_565 . ? O4 Eu1 O5 80.02(12) . . ? O6 Eu1 O2 71.43(12) . . ? O3 Eu1 O2 66.93(11) . . ? O1 Eu1 O2 138.25(12) . . ? O8 Eu1 O2 140.23(12) 1_565 . ? O4 Eu1 O2 70.27(12) . . ? O5 Eu1 O2 72.77(12) . . ? O6 Eu1 O7 142.81(12) . . ? O3 Eu1 O7 72.84(11) . . ? O1 Eu1 O7 66.20(11) . . ? O8 Eu1 O7 66.26(12) 1_565 . ? O4 Eu1 O7 69.06(11) . . ? O5 Eu1 O7 133.45(12) . . ? O2 Eu1 O7 123.75(12) . . ? O6 Eu1 O20 59.57(12) . . ? O3 Eu1 O20 137.24(12) . . ? O1 Eu1 O20 68.63(11) . . ? O8 Eu1 O20 67.82(14) 1_565 . ? O4 Eu1 O20 136.97(13) . . ? O5 Eu1 O20 64.80(14) . . ? O2 Eu1 O20 117.70(12) . . ? O7 Eu1 O20 118.55(12) . . ? O6 Eu1 H5O 98.9(7) . . ? O3 Eu1 H5O 151.9(9) . . ? O1 Eu1 H5O 55.1(6) . . ? O8 Eu1 H5O 124.7(9) 1_565 . ? O4 Eu1 H5O 72.9(9) . . ? O5 Eu1 H5O 20.2(5) . . ? O2 Eu1 H5O 88.4(7) . . ? O7 Eu1 H5O 114.1(6) . . ? O20 Eu1 H5O 65.5(10) . . ? O6 C1 C6 124.7(4) . . ? O6 C1 C2 123.0(5) . . ? C6 C1 C2 112.3(4) . . ? C3 C2 C1 124.4(5) . . ? C3 C2 N6 115.6(4) . . ? C1 C2 N6 120.0(4) . . ? C2 C3 C4 119.4(5) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C5 C4 C3 120.8(5) . . ? C5 C4 N7 119.9(5) . . ? C3 C4 N7 119.4(5) . . ? C4 C5 C6 119.1(5) . . ? C4 C5 H5 120.4 . . ? C6 C5 H5 120.4 . . ? C5 C6 C1 124.0(4) . . ? C5 C6 N8 116.2(5) . . ? C1 C6 N8 119.8(4) . . ? C10 C7 C8 121.0(7) . . ? C10 C7 H7 119.5 . . ? C8 C7 H7 119.5 . . ? C9 C8 C7 120.0(6) . . ? C9 C8 C44 124.4(6) . . ? C7 C8 C44 115.6(5) . . ? O26 C9 C8 118.6(6) . . ? O26 C9 C12 123.5(7) . . ? C8 C9 C12 117.9(8) . . ? C11 C10 C7 118.5(9) . . ? C11 C10 H10 120.7 . . ? C7 C10 H10 120.7 . . ? C12 C11 C10 123.5(8) . . ? C12 C11 H11 118.2 . . ? C10 C11 H11 118.2 . . ? C11 C12 C9 118.8(8) . . ? C11 C12 H12 120.6 . . ? C9 C12 H12 120.6 . . ? C18 C13 C14 124.5(5) . . ? C18 C13 N3 116.3(5) . . ? C14 C13 N3 119.2(5) . . ? O1 C14 C13 123.6(5) . . ? O1 C14 C15 123.7(4) . . ? C13 C14 C15 112.7(4) . . ? C16 C15 C14 123.1(4) . . ? C16 C15 N4 115.4(4) . . ? C14 C15 N4 121.4(4) . . ? C17 C16 C15 119.7(5) . . ? C17 C16 H16 120.2 . . ? C15 C16 H16 120.2 . . ? C16 C17 C18 121.8(5) . . ? C16 C17 N5 118.9(5) . . ? C18 C17 N5 119.3(5) . . ? C13 C18 C17 118.2(5) . . ? C13 C18 H18 120.9 . . ? C17 C18 H18 120.9 . . ? O3 C19 C24 127.3(5) . . ? O3 C19 C21 120.0(4) . . ? C24 C19 C21 112.7(4) . . ? C22 C20 C24 119.5(5) . . ? C22 C20 H20 120.3 . . ? C24 C20 H20 120.3 . . ? C23 C21 C19 124.9(5) . . ? C23 C21 N2 119.2(5) . . ? C19 C21 N2 115.9(5) . . ? C20 C22 C23 121.3(5) . . ? C20 C22 N9 119.8(5) . . ? C23 C22 N9 118.9(6) . . ? C21 C23 C22 118.3(5) . . ? C21 C23 H23 120.8 . . ? C22 C23 H23 120.8 . . ? C20 C24 C19 123.3(5) . . ? C20 C24 N1 116.5(4) . . ? C19 C24 N1 120.2(4) . . ? C49 C25 C26 121.9(7) . . ? C49 C25 H25 119.0 . . ? C26 C25 H25 119.0 . . ? C25 C26 C27 117.9(5) . . ? C25 C26 C30 117.5(5) . . ? C27 C26 C30 124.6(5) . . ? O25 C27 C28 122.5(6) . . ? O25 C27 C26 117.1(4) . . ? C28 C27 C26 120.3(6) . . ? C50 C28 C27 118.8(7) . . ? C50 C28 H28 120.6 . . ? C27 C28 H28 120.6 . . ? O25 C29 C35 106.7(5) . . ? O25 C29 H29A 110.4 . . ? C35 C29 H29A 110.4 . . ? O25 C29 H29B 110.4 . . ? C35 C29 H29B 110.4 . . ? H29A C29 H29B 108.6 . . ? O4 C30 N11 120.8(5) . . ? O4 C30 C26 120.3(5) . . ? N11 C30 C26 118.9(4) . . ? N11 C31 C32 113.9(4) . . ? N11 C31 H31A 108.8 . . ? C32 C31 H31A 108.8 . . ? N11 C31 H31B 108.8 . . ? C32 C31 H31B 108.8 . . ? H31A C31 H31B 107.7 . . ? C33 C32 C34 117.9(6) . . ? C33 C32 C31 122.5(5) . . ? C34 C32 C31 119.5(5) . . ? C32 C33 C46 120.3(7) . . ? C32 C33 H33 119.9 . . ? C46 C33 H33 119.9 . . ? C48 C34 C32 121.3(6) . . ? C48 C34 H34 119.3 . . ? C32 C34 H34 119.3 . . ? N10 C35 C29 114.3(5) . . ? N10 C35 H35A 108.7 . . ? C29 C35 H35A 108.7 . . ? N10 C35 H35B 108.7 . . ? C29 C35 H35B 108.7 . . ? H35A C35 H35B 107.6 . . ? N10 C36 C37 113.3(5) . . ? N10 C36 H36A 108.9 . . ? C37 C36 H36A 108.9 . . ? N10 C36 H36B 108.9 . . ? C37 C36 H36B 108.9 . . ? H36A C36 H36B 107.7 . . ? C38 C37 C39 118.0(6) . . ? C38 C37 C36 120.8(6) . . ? C39 C37 C36 121.1(6) . . ? C37 C38 C40 121.9(7) . . ? C37 C38 H38 119.0 . . ? C40 C38 H38 119.0 . . ? C37 C39 C42 120.3(7) . . ? C37 C39 H39 119.9 . . ? C42 C39 H39 119.9 . . ? C41 C40 C38 119.8(8) . . ? C41 C40 H40 120.1 . . ? C38 C40 H40 120.1 . . ? C40 C41 C42 121.1(9) . . ? C40 C41 H41 119.5 . . ? C42 C41 H41 119.5 . . ? C41 C42 C39 118.8(8) . . ? C41 C42 H42 120.6 . . ? C39 C42 H42 120.6 . . ? C52 C43 N12 111.1(5) . . ? C52 C43 H43A 109.4 . . ? N12 C43 H43A 109.4 . . ? C52 C43 H43B 109.4 . . ? N12 C43 H43B 109.4 . . ? H43A C43 H43B 108.0 . . ? O8 C44 N12 120.9(5) . . ? O8 C44 C8 118.5(5) . . ? N12 C44 C8 120.6(5) . . ? C47 C46 C33 120.4(8) . . ? C47 C46 H46 119.8 . . ? C33 C46 H46 119.8 . . ? C48 C47 C46 119.6(8) . . ? C48 C47 H47 120.2 . . ? C46 C47 H47 120.2 . . ? C47 C48 C34 120.4(8) . . ? C47 C48 H48 119.8 . . ? C34 C48 H48 119.8 . . ? C50 C49 C25 118.9(7) . . ? C50 C49 H49 120.5 . . ? C25 C49 H49 120.5 . . ? C49 C50 C28 122.1(7) . . ? C49 C50 H50 118.9 . . ? C28 C50 H50 118.9 . . ? C52 C51 C60 120.0 . . ? C52 C51 H51 120.0 . . ? C60 C51 H51 120.0 . . ? C53 C52 C51 120.0 . . ? C53 C52 C43 120.5(5) . . ? C51 C52 C43 119.5(5) . . ? C52 C53 C59 120.0 . . ? C52 C53 H53 120.0 . . ? C59 C53 H53 120.0 . . ? C58 C59 C53 120.0 . . ? C58 C59 H59 120.0 . . ? C53 C59 H59 120.0 . . ? C60 C58 C59 120.0 . . ? C60 C58 H58 120.0 . . ? C59 C58 H58 120.0 . . ? C58 C60 C51 120.0 . . ? C58 C60 H60 120.0 . . ? C51 C60 H60 120.0 . . ? C57 C54 N10 115.2(7) . . ? C57 C54 H54A 108.5 . . ? N10 C54 H54A 108.5 . . ? C57 C54 H54B 108.5 . . ? N10 C54 H54B 108.5 . . ? H54A C54 H54B 107.5 . . ? O5 C55 C56 110.5(6) . . ? O5 C55 H55A 109.5 . . ? C56 C55 H55A 109.5 . . ? O5 C55 H55B 109.5 . . ? C56 C55 H55B 109.5 . . ? H55A C55 H55B 108.1 . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? O26 C57 C54 108.2(7) . . ? O26 C57 H57A 110.1 . . ? C54 C57 H57A 110.1 . . ? O26 C57 H57B 110.1 . . ? C54 C57 H57B 110.1 . . ? H57A C57 H57B 108.4 . . ? O9 N1 O2 121.8(5) . . ? O9 N1 C24 118.7(5) . . ? O2 N1 C24 119.5(4) . . ? O10 N2 O11 125.0(6) . . ? O10 N2 C21 118.3(6) . . ? O11 N2 C21 116.6(6) . . ? O21 N3 O14 121.2(6) . . ? O21 N3 C13 118.3(5) . . ? O14 N3 C13 120.5(5) . . ? O12 N4 O7 120.7(4) . . ? O12 N4 C15 118.3(4) . . ? O7 N4 C15 121.0(4) . . ? O13 N5 O24 123.9(6) . . ? O13 N5 C17 118.5(6) . . ? O24 N5 C17 117.6(5) . . ? O15 N6 O16 120.8(5) . . ? O15 N6 C2 119.8(5) . . ? O16 N6 C2 119.4(5) . . ? O18 N7 O17 124.2(5) . . ? O18 N7 C4 117.8(5) . . ? O17 N7 C4 117.8(6) . . ? O19 N8 O20 121.4(5) . . ? O19 N8 C6 118.4(5) . . ? O20 N8 C6 120.1(5) . . ? O22 N9 O23 123.8(6) . . ? O22 N9 C22 118.1(6) . . ? O23 N9 C22 118.1(6) . . ? C35 N10 C36 112.0(5) . . ? C35 N10 C54 106.3(6) . . ? C36 N10 C54 113.5(5) . . ? C30 N11 C31 124.5(4) . . ? C30 N11 H11A 117.8 . . ? C31 N11 H11A 117.8 . . ? C44 N12 C43 122.0(5) . . ? C44 N12 H12' 119.0 . . ? C43 N12 H12' 119.0 . . ? C14 O1 Eu1 137.8(3) . . ? N1 O2 Eu1 139.0(3) . . ? C19 O3 Eu1 141.3(3) . . ? C30 O4 Eu1 156.0(3) . . ? C55 O5 Eu1 128.8(4) . . ? C55 O5 H5O 134(3) . . ? Eu1 O5 H5O 98(3) . . ? C1 O6 Eu1 155.5(3) . . ? N4 O7 Eu1 136.7(3) . . ? C44 O8 Eu1 147.1(4) . 1_545 ? N8 O20 Eu1 138.8(3) . . ? C27 O25 C29 120.4(5) . . ? C9 O26 C57 118.7(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O6 C1 C2 C3 179.4(5) . . . . ? C6 C1 C2 C3 -1.5(7) . . . . ? O6 C1 C2 N6 0.0(8) . . . . ? C6 C1 C2 N6 179.1(4) . . . . ? C1 C2 C3 C4 -0.2(8) . . . . ? N6 C2 C3 C4 179.2(5) . . . . ? C2 C3 C4 C5 1.5(8) . . . . ? C2 C3 C4 N7 -178.7(5) . . . . ? C3 C4 C5 C6 -0.9(8) . . . . ? N7 C4 C5 C6 179.4(5) . . . . ? C4 C5 C6 C1 -1.1(8) . . . . ? C4 C5 C6 N8 -179.5(5) . . . . ? O6 C1 C6 C5 -178.7(5) . . . . ? C2 C1 C6 C5 2.2(7) . . . . ? O6 C1 C6 N8 -0.4(8) . . . . ? C2 C1 C6 N8 -179.5(4) . . . . ? C10 C7 C8 C9 -1.5(9) . . . . ? C10 C7 C8 C44 176.7(5) . . . . ? C7 C8 C9 O26 -177.4(6) . . . . ? C44 C8 C9 O26 4.6(9) . . . . ? C7 C8 C9 C12 4.8(9) . . . . ? C44 C8 C9 C12 -173.2(5) . . . . ? C8 C7 C10 C11 -2.3(10) . . . . ? C7 C10 C11 C12 2.8(13) . . . . ? C10 C11 C12 C9 0.6(13) . . . . ? O26 C9 C12 C11 177.9(7) . . . . ? C8 C9 C12 C11 -4.4(11) . . . . ? C18 C13 C14 O1 177.7(5) . . . . ? N3 C13 C14 O1 -4.3(7) . . . . ? C18 C13 C14 C15 -3.3(7) . . . . ? N3 C13 C14 C15 174.7(4) . . . . ? O1 C14 C15 C16 -178.9(5) . . . . ? C13 C14 C15 C16 2.0(7) . . . . ? O1 C14 C15 N4 2.2(7) . . . . ? C13 C14 C15 N4 -176.8(4) . . . . ? C14 C15 C16 C17 0.4(8) . . . . ? N4 C15 C16 C17 179.3(4) . . . . ? C15 C16 C17 C18 -1.9(8) . . . . ? C15 C16 C17 N5 178.5(4) . . . . ? C14 C13 C18 C17 2.1(7) . . . . ? N3 C13 C18 C17 -176.0(4) . . . . ? C16 C17 C18 C13 0.7(7) . . . . ? N5 C17 C18 C13 -179.7(4) . . . . ? O3 C19 C21 C23 177.8(5) . . . . ? C24 C19 C21 C23 -2.6(7) . . . . ? O3 C19 C21 N2 0.0(7) . . . . ? C24 C19 C21 N2 179.6(5) . . . . ? C24 C20 C22 C23 -1.8(8) . . . . ? C24 C20 C22 N9 177.9(4) . . . . ? C19 C21 C23 C22 1.2(8) . . . . ? N2 C21 C23 C22 178.9(5) . . . . ? C20 C22 C23 C21 1.2(8) . . . . ? N9 C22 C23 C21 -178.6(5) . . . . ? C22 C20 C24 C19 0.1(7) . . . . ? C22 C20 C24 N1 -179.4(4) . . . . ? O3 C19 C24 C20 -178.6(4) . . . . ? C21 C19 C24 C20 1.9(6) . . . . ? O3 C19 C24 N1 0.9(7) . . . . ? C21 C19 C24 N1 -178.6(4) . . . . ? C49 C25 C26 C27 0.0(9) . . . . ? C49 C25 C26 C30 -177.2(6) . . . . ? C25 C26 C27 O25 -178.6(5) . . . . ? C30 C26 C27 O25 -1.6(7) . . . . ? C25 C26 C27 C28 -0.5(8) . . . . ? C30 C26 C27 C28 176.5(5) . . . . ? O25 C27 C28 C50 177.6(6) . . . . ? C26 C27 C28 C50 -0.4(9) . . . . ? C25 C26 C30 O4 18.1(7) . . . . ? C27 C26 C30 O4 -158.9(5) . . . . ? C25 C26 C30 N11 -161.9(5) . . . . ? C27 C26 C30 N11 21.1(7) . . . . ? N11 C31 C32 C33 41.8(7) . . . . ? N11 C31 C32 C34 -140.3(5) . . . . ? C34 C32 C33 C46 0.8(9) . . . . ? C31 C32 C33 C46 178.7(6) . . . . ? C33 C32 C34 C48 0.8(9) . . . . ? C31 C32 C34 C48 -177.2(6) . . . . ? O25 C29 C35 N10 -64.3(6) . . . . ? N10 C36 C37 C38 45.3(8) . . . . ? N10 C36 C37 C39 -137.5(6) . . . . ? C39 C37 C38 C40 2.4(9) . . . . ? C36 C37 C38 C40 179.7(6) . . . . ? C38 C37 C39 C42 -2.5(10) . . . . ? C36 C37 C39 C42 -179.8(6) . . . . ? C37 C38 C40 C41 -1.2(11) . . . . ? C38 C40 C41 C42 -0.1(12) . . . . ? C40 C41 C42 C39 0.0(13) . . . . ? C37 C39 C42 C41 1.3(12) . . . . ? C9 C8 C44 O8 165.3(5) . . . . ? C7 C8 C44 O8 -12.7(7) . . . . ? C9 C8 C44 N12 -16.3(9) . . . . ? C7 C8 C44 N12 165.6(5) . . . . ? C32 C33 C46 C47 -2.6(11) . . . . ? C33 C46 C47 C48 2.8(13) . . . . ? C46 C47 C48 C34 -1.2(13) . . . . ? C32 C34 C48 C47 -0.6(11) . . . . ? C26 C25 C49 C50 1.3(11) . . . . ? C25 C49 C50 C28 -2.3(12) . . . . ? C27 C28 C50 C49 1.8(11) . . . . ? C60 C51 C52 C53 0.0 . . . . ? C60 C51 C52 C43 179.5(4) . . . . ? N12 C43 C52 C53 100.6(5) . . . . ? N12 C43 C52 C51 -78.9(6) . . . . ? C51 C52 C53 C59 0.0 . . . . ? C43 C52 C53 C59 -179.5(4) . . . . ? C52 C53 C59 C58 0.0 . . . . ? C53 C59 C58 C60 0.0 . . . . ? C59 C58 C60 C51 0.0 . . . . ? C52 C51 C60 C58 0.0 . . . . ? N10 C54 C57 O26 -93.4(8) . . . . ? C20 C24 N1 O9 -20.4(6) . . . . ? C19 C24 N1 O9 160.1(5) . . . . ? C20 C24 N1 O2 158.9(4) . . . . ? C19 C24 N1 O2 -20.6(6) . . . . ? C23 C21 N2 O10 84.8(8) . . . . ? C19 C21 N2 O10 -97.3(7) . . . . ? C23 C21 N2 O11 -94.3(7) . . . . ? C19 C21 N2 O11 83.7(7) . . . . ? C18 C13 N3 O21 11.3(9) . . . . ? C14 C13 N3 O21 -166.9(6) . . . . ? C18 C13 N3 O14 -166.6(6) . . . . ? C14 C13 N3 O14 15.2(9) . . . . ? C16 C15 N4 O12 -11.8(7) . . . . ? C14 C15 N4 O12 167.1(5) . . . . ? C16 C15 N4 O7 166.8(5) . . . . ? C14 C15 N4 O7 -14.2(7) . . . . ? C16 C17 N5 O13 -172.1(5) . . . . ? C18 C17 N5 O13 8.3(8) . . . . ? C16 C17 N5 O24 9.4(8) . . . . ? C18 C17 N5 O24 -170.2(6) . . . . ? C3 C2 N6 O15 -167.1(6) . . . . ? C1 C2 N6 O15 12.3(8) . . . . ? C3 C2 N6 O16 10.4(8) . . . . ? C1 C2 N6 O16 -170.2(5) . . . . ? C5 C4 N7 O18 -3.2(9) . . . . ? C3 C4 N7 O18 177.0(6) . . . . ? C5 C4 N7 O17 -177.9(6) . . . . ? C3 C4 N7 O17 2.3(9) . . . . ? C5 C6 N8 O19 9.1(8) . . . . ? C1 C6 N8 O19 -169.4(6) . . . . ? C5 C6 N8 O20 -172.5(5) . . . . ? C1 C6 N8 O20 9.0(8) . . . . ? C20 C22 N9 O22 -2.8(8) . . . . ? C23 C22 N9 O22 176.9(5) . . . . ? C20 C22 N9 O23 176.3(5) . . . . ? C23 C22 N9 O23 -3.9(8) . . . . ? C29 C35 N10 C36 -63.9(6) . . . . ? C29 C35 N10 C54 171.7(5) . . . . ? C37 C36 N10 C35 91.0(6) . . . . ? C37 C36 N10 C54 -148.6(6) . . . . ? C57 C54 N10 C35 177.5(6) . . . . ? C57 C54 N10 C36 53.9(9) . . . . ? O4 C30 N11 C31 5.0(8) . . . . ? C26 C30 N11 C31 -175.0(4) . . . . ? C32 C31 N11 C30 -118.4(5) . . . . ? O8 C44 N12 C43 -3.1(9) . . . . ? C8 C44 N12 C43 178.6(6) . . . . ? C52 C43 N12 C44 -152.7(6) . . . . ? C13 C14 O1 Eu1 -141.5(4) . . . . ? C15 C14 O1 Eu1 39.6(7) . . . . ? O6 Eu1 O1 C14 178.9(4) . . . . ? O3 Eu1 O1 C14 -40.0(6) . . . . ? O8 Eu1 O1 C14 -109.3(5) 1_565 . . . ? O4 Eu1 O1 C14 30.2(5) . . . . ? O5 Eu1 O1 C14 112.8(5) . . . . ? O2 Eu1 O1 C14 73.1(5) . . . . ? O7 Eu1 O1 C14 -41.5(5) . . . . ? O20 Eu1 O1 C14 -178.7(5) . . . . ? O9 N1 O2 Eu1 -157.9(4) . . . . ? C24 N1 O2 Eu1 22.8(7) . . . . ? O6 Eu1 O2 N1 87.6(5) . . . . ? O3 Eu1 O2 N1 -6.3(4) . . . . ? O1 Eu1 O2 N1 -145.4(4) . . . . ? O8 Eu1 O2 N1 38.4(5) 1_565 . . . ? O4 Eu1 O2 N1 -100.1(5) . . . . ? O5 Eu1 O2 N1 174.6(5) . . . . ? O7 Eu1 O2 N1 -54.2(5) . . . . ? O20 Eu1 O2 N1 126.3(4) . . . . ? C24 C19 O3 Eu1 23.9(8) . . . . ? C21 C19 O3 Eu1 -156.6(4) . . . . ? O6 Eu1 O3 C19 -90.0(5) . . . . ? O1 Eu1 O3 C19 119.6(5) . . . . ? O8 Eu1 O3 C19 -171.7(5) 1_565 . . . ? O4 Eu1 O3 C19 51.7(5) . . . . ? O5 Eu1 O3 C19 -17.3(5) . . . . ? O2 Eu1 O3 C19 -18.6(4) . . . . ? O7 Eu1 O3 C19 121.1(5) . . . . ? O20 Eu1 O3 C19 -125.1(5) . . . . ? N11 C30 O4 Eu1 -96.8(9) . . . . ? C26 C30 O4 Eu1 83.2(9) . . . . ? O6 Eu1 O4 C30 -171.4(8) . . . . ? O3 Eu1 O4 C30 109.9(8) . . . . ? O1 Eu1 O4 C30 -31.9(8) . . . . ? O8 Eu1 O4 C30 33.9(9) 1_565 . . . ? O5 Eu1 O4 C30 -108.0(8) . . . . ? O2 Eu1 O4 C30 176.9(8) . . . . ? O7 Eu1 O4 C30 36.6(8) . . . . ? O20 Eu1 O4 C30 -73.3(8) . . . . ? C56 C55 O5 Eu1 113.5(6) . . . . ? O6 Eu1 O5 C55 29.5(5) . . . . ? O3 Eu1 O5 C55 -44.7(6) . . . . ? O1 Eu1 O5 C55 162.9(5) . . . . ? O8 Eu1 O5 C55 100.0(5) 1_565 . . . ? O4 Eu1 O5 C55 -115.7(5) . . . . ? O2 Eu1 O5 C55 -43.5(5) . . . . ? O7 Eu1 O5 C55 -163.9(5) . . . . ? O20 Eu1 O5 C55 89.7(5) . . . . ? C6 C1 O6 Eu1 -17.3(12) . . . . ? C2 C1 O6 Eu1 161.7(6) . . . . ? O3 Eu1 O6 C1 -138.4(8) . . . . ? O1 Eu1 O6 C1 17.2(9) . . . . ? O8 Eu1 O6 C1 -54.6(8) 1_565 . . . ? O4 Eu1 O6 C1 143.1(8) . . . . ? O5 Eu1 O6 C1 80.2(8) . . . . ? O2 Eu1 O6 C1 154.7(9) . . . . ? O7 Eu1 O6 C1 -83.5(9) . . . . ? O20 Eu1 O6 C1 14.7(8) . . . . ? O12 N4 O7 Eu1 170.9(4) . . . . ? C15 N4 O7 Eu1 -7.7(8) . . . . ? O6 Eu1 O7 N4 147.4(4) . . . . ? O3 Eu1 O7 N4 -153.9(5) . . . . ? O1 Eu1 O7 N4 25.0(5) . . . . ? O8 Eu1 O7 N4 116.0(5) 1_565 . . . ? O4 Eu1 O7 N4 -61.9(5) . . . . ? O5 Eu1 O7 N4 -10.1(6) . . . . ? O2 Eu1 O7 N4 -108.3(5) . . . . ? O20 Eu1 O7 N4 71.1(5) . . . . ? N12 C44 O8 Eu1 108.1(7) . . . 1_545 ? C8 C44 O8 Eu1 -73.5(8) . . . 1_545 ? O19 N8 O20 Eu1 169.0(5) . . . . ? C6 N8 O20 Eu1 -9.3(9) . . . . ? O6 Eu1 O20 N8 1.7(6) . . . . ? O3 Eu1 O20 N8 43.4(7) . . . . ? O1 Eu1 O20 N8 -176.2(7) . . . . ? O8 Eu1 O20 N8 94.5(6) 1_565 . . . ? O4 Eu1 O20 N8 -132.0(6) . . . . ? O5 Eu1 O20 N8 -93.7(6) . . . . ? O2 Eu1 O20 N8 -41.8(7) . . . . ? O7 Eu1 O20 N8 138.8(6) . . . . ? C28 C27 O25 C29 18.3(7) . . . . ? C26 C27 O25 C29 -163.6(4) . . . . ? C35 C29 O25 C27 157.7(5) . . . . ? C8 C9 O26 C57 174.2(6) . . . . ? C12 C9 O26 C57 -8.1(10) . . . . ? C54 C57 O26 C9 -170.7(6) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.655 _refine_diff_density_min -0.806 _refine_diff_density_rms 0.076 #===END data_852909 _database_code_depnum_ccdc_archive 'CCDC 852909' #TrackingRef '- cif_Revision.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C59 H51 N12 O26 Tb' _chemical_formula_weight 1503.04 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 13.6842(15) _cell_length_b 15.8378(17) _cell_length_c 17.4990(18) _cell_angle_alpha 96.651(2) _cell_angle_beta 109.062(2) _cell_angle_gamma 114.164(2) _cell_volume 3130.6(6) _cell_formula_units_Z 2 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description yellow _exptl_crystal_colour block _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.595 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1524 _exptl_absorpt_coefficient_mu 1.226 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7657 _exptl_absorpt_correction_T_max 0.7916 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 15456 _diffrn_reflns_av_R_equivalents 0.0301 _diffrn_reflns_av_sigmaI/netI 0.0768 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 25.50 _reflns_number_total 11380 _reflns_number_gt 8077 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0735P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11380 _refine_ls_number_parameters 888 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0879 _refine_ls_R_factor_gt 0.0562 _refine_ls_wR_factor_ref 0.1463 _refine_ls_wR_factor_gt 0.1247 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O26 O 1.1477(3) 0.7279(3) 0.8190(3) 0.0532(10) Uani 1 1 d . . . C2 C 1.1835(6) 1.0445(4) 0.6411(4) 0.0556(16) Uani 1 1 d . . . H2 H 1.2560 1.0867 0.6428 0.067 Uiso 1 1 calc R . . C3 C 1.1687(5) 0.9635(4) 0.6657(4) 0.0488(15) Uani 1 1 d . . . C4 C 1.0595(5) 0.8957(4) 0.6652(4) 0.0478(14) Uani 1 1 d . . . C5 C 0.5728(5) 0.3921(4) 0.7855(4) 0.0500(15) Uani 1 1 d . . . C6 C 0.8768(5) 1.4429(4) 0.7207(4) 0.0474(14) Uani 1 1 d . . . C7 C 0.5899(5) 0.4895(4) 0.6942(4) 0.0498(15) Uani 1 1 d . . . C8 C 0.7536(6) 1.3719(4) 0.6598(4) 0.0511(15) Uani 1 1 d . . . C9 C 1.1430(5) 1.4519(4) 0.8435(4) 0.0524(15) Uani 1 1 d . . . C10 C 1.3165(5) 0.7214(4) 0.9012(4) 0.0539(16) Uani 1 1 d . . . C11 C 0.7142(5) 0.5508(4) 0.7450(4) 0.0481(15) Uani 1 1 d . . . C12 C 0.9987(5) 0.8925(5) 0.8581(4) 0.0557(16) Uani 1 1 d . . . C13 C 1.2512(5) 0.6774(4) 0.7523(4) 0.0462(14) Uani 1 1 d . . . C14 C 1.3427(5) 0.6564(4) 0.7609(4) 0.0567(16) Uani 1 1 d . . . H14 H 1.3525 0.6350 0.7136 0.068 Uiso 1 1 calc R . . C15 C 0.5218(5) 0.4121(4) 0.7135(4) 0.0536(16) Uani 1 1 d . . . H15 H 0.4424 0.3737 0.6786 0.064 Uiso 1 1 calc R . . C16 C 1.0524(6) 1.4803(5) 0.8458(4) 0.0608(17) Uani 1 1 d . . . H16A H 1.0484 1.4812 0.9002 0.073 Uiso 1 1 calc R . . H16B H 1.0766 1.5453 0.8406 0.073 Uiso 1 1 calc R . . C17 C 1.1103(6) 0.9795(5) 0.8743(4) 0.0612(18) Uani 1 1 d . . . C18 C 1.2304(5) 0.7090(4) 0.8217(4) 0.0450(14) Uani 1 1 d . . . C19 C 0.6801(5) 1.2905(5) 0.6760(4) 0.0576(17) Uani 1 1 d . . . C20 C 0.9689(5) 0.9215(4) 0.6368(4) 0.0514(15) Uani 1 1 d . . . C21 C 0.6886(5) 0.4471(4) 0.8392(4) 0.0542(16) Uani 1 1 d . . . H21 H 0.7202 0.4324 0.8883 0.065 Uiso 1 1 calc R . . C22 C 0.7077(7) 1.3901(5) 0.5848(4) 0.075(2) Uani 1 1 d . . . H22 H 0.7554 1.4436 0.5729 0.090 Uiso 1 1 calc R . . C23 C 0.7580(5) 0.5251(4) 0.8193(4) 0.0488(15) Uani 1 1 d . . . C24 C 1.4183(5) 0.6679(5) 0.8402(4) 0.0568(16) Uani 1 1 d . . . C25 C 0.7025(6) 0.8466(5) 0.8261(5) 0.0614(18) Uani 1 1 d . . . C26 C 0.9835(6) 1.0031(5) 0.6117(4) 0.0576(16) Uani 1 1 d . . . H26 H 0.9215 1.0171 0.5935 0.069 Uiso 1 1 calc R . . C27 C 0.7872(7) 1.1078(5) 0.6592(5) 0.0676(19) Uani 1 1 d . . . C28 C 1.0907(6) 1.0639(4) 0.6137(4) 0.0592(17) Uani 1 1 d . . . C29 C 1.4054(6) 0.6996(5) 0.9104(4) 0.0640(18) Uani 1 1 d . . . H29 H 1.4566 0.7062 0.9638 0.077 Uiso 1 1 calc R . . C30 C 0.8228(7) 1.0916(5) 0.7452(5) 0.081(2) Uani 1 1 d . . . H30A H 0.7571 1.0362 0.7459 0.097 Uiso 1 1 calc R . . H30B H 0.8871 1.0766 0.7552 0.097 Uiso 1 1 calc R . . C31 C 1.1499(7) 1.4205(6) 0.7715(5) 0.075(2) Uani 1 1 d . . . H31 H 1.0954 1.4150 0.7200 0.090 Uiso 1 1 calc R . . C32 C 0.8530(7) 1.1890(6) 0.6444(5) 0.072(2) Uani 1 1 d . . . H32 H 0.9224 1.2358 0.6889 0.087 Uiso 1 1 calc R . . C33 C 1.2040(6) 0.9622(6) 0.8813(5) 0.080(2) Uani 1 1 d . . . H33 H 1.1947 0.9001 0.8778 0.096 Uiso 1 1 calc R . . C34 C 0.6868(7) 1.0381(6) 0.5920(6) 0.090(2) Uani 1 1 d . . . H34 H 0.6400 0.9807 0.5999 0.108 Uiso 1 1 calc R . . C35 C 0.7638(10) 1.1746(6) 0.8330(6) 0.106(3) Uani 1 1 d . . . H35A H 0.7961 1.2283 0.8826 0.128 Uiso 1 1 calc R . . H35B H 0.7270 1.1154 0.8470 0.128 Uiso 1 1 calc R . . C36 C 0.5669(7) 1.2330(6) 0.6179(6) 0.083(2) Uani 1 1 d . . . H36 H 0.5183 1.1786 0.6282 0.100 Uiso 1 1 calc R . . C37 C 1.2265(7) 1.4608(6) 0.9189(5) 0.078(2) Uani 1 1 d . . . H37 H 1.2230 1.4812 0.9695 0.093 Uiso 1 1 calc R . . C38 C 0.7979(6) 0.8196(6) 0.8503(6) 0.092(3) Uani 1 1 d . . . H38A H 0.7799 0.7669 0.8049 0.111 Uiso 1 1 calc R . . H38B H 0.8021 0.7973 0.9001 0.111 Uiso 1 1 calc R . . C39 C 1.3116(8) 1.0372(9) 0.8933(5) 0.116(4) Uani 1 1 d . . . H39 H 1.3756 1.0264 0.9006 0.139 Uiso 1 1 calc R . . C40 C 1.3220(10) 1.1264(10) 0.8944(6) 0.132(5) Uani 1 1 d . . . H40 H 1.3931 1.1757 0.8998 0.158 Uiso 1 1 calc R . . C41 C 1.2338(9) 1.1462(7) 0.8879(6) 0.123(5) Uani 1 1 d . . . H41 H 1.2436 1.2079 0.8880 0.148 Uiso 1 1 calc R . . C42 C 1.1248(8) 1.0720(6) 0.8807(5) 0.092(3) Uani 1 1 d . . . C43 C 0.8238(11) 1.2064(8) 0.5684(8) 0.103(3) Uani 1 1 d . . . H43 H 0.8709 1.2644 0.5616 0.123 Uiso 1 1 calc R . . C44 C 0.7253(13) 1.1382(12) 0.5028(7) 0.121(4) Uani 1 1 d . . . H44 H 0.7054 1.1496 0.4504 0.145 Uiso 1 1 calc R . . C45 C 0.6538(10) 1.0526(10) 0.5111(7) 0.118(4) Uani 1 1 d . . . H45 H 0.5860 1.0057 0.4654 0.142 Uiso 1 1 calc R . . C46 C 0.9509(11) 1.1853(7) 0.8941(6) 0.126(4) Uani 1 1 d . . . H46A H 0.9760 1.2455 0.9343 0.151 Uiso 1 1 calc R . . H46B H 0.9142 1.1333 0.9162 0.151 Uiso 1 1 calc R . . C47 C 1.3152(8) 1.4396(7) 0.9201(7) 0.099(3) Uani 1 1 d . . . H47 H 1.3714 1.4470 0.9715 0.119 Uiso 1 1 calc R . . C48 C 1.3213(9) 1.4085(8) 0.8482(9) 0.118(4) Uani 1 1 d . . . H48 H 1.3821 1.3955 0.8497 0.142 Uiso 1 1 calc R . . C49 C 1.2378(9) 1.3961(7) 0.7730(7) 0.108(3) Uani 1 1 d . . . H49 H 1.2391 1.3714 0.7227 0.130 Uiso 1 1 calc R . . C50 C 0.5938(9) 1.3318(7) 0.5275(6) 0.103(3) Uani 1 1 d . . . H50 H 0.5654 1.3457 0.4772 0.124 Uiso 1 1 calc R . . C51 C 0.5234(8) 1.2547(8) 0.5436(7) 0.107(3) Uani 1 1 d . . . H51 H 0.4455 1.2159 0.5052 0.128 Uiso 1 1 calc R . . C52 C 1.0515(10) 1.1840(6) 0.8914(7) 0.141(5) Uani 1 1 d . . . H52A H 1.1189 1.2248 0.9443 0.169 Uiso 1 1 calc R . . H52B H 1.0672 1.2092 0.8463 0.169 Uiso 1 1 calc R . . C53 C 0.6711(7) 1.1815(5) 0.7627(6) 0.086(3) Uani 1 1 d . . . H53A H 0.6401 1.1305 0.7114 0.103 Uiso 1 1 calc R . . H53B H 0.6069 1.1755 0.7778 0.103 Uiso 1 1 calc R . . C54 C 0.6855(7) 0.8965(5) 0.8861(5) 0.074(2) Uani 1 1 d . . . H54 H 0.7337 0.9125 0.9429 0.088 Uiso 1 1 calc R . . C55 C 0.6013(10) 0.9223(7) 0.8642(9) 0.118(4) Uani 1 1 d . . . H55 H 0.5947 0.9591 0.9058 0.141 Uiso 1 1 calc R . . C56 C 0.5395(12) 0.8496(12) 0.7245(10) 0.162(8) Uani 1 1 d . . . H56 H 0.4884 0.8346 0.6686 0.195 Uiso 1 1 calc R . . C57 C 0.6283(9) 0.8215(7) 0.7431(6) 0.103(3) Uani 1 1 d . . . H57 H 0.6360 0.7872 0.7005 0.123 Uiso 1 1 calc R . . C58 C 0.8552(8) 0.6457(7) 0.5121(6) 0.102(3) Uani 1 1 d . . . H58A H 0.9335 0.6998 0.5311 0.123 Uiso 1 1 calc R . . H58B H 0.7993 0.6645 0.4794 0.123 Uiso 1 1 calc R . . C59 C 0.8460(10) 0.5623(9) 0.4580(6) 0.134(4) Uani 1 1 d . . . H59A H 0.8968 0.5404 0.4912 0.201 Uiso 1 1 calc R . . H59B H 0.8689 0.5809 0.4137 0.201 Uiso 1 1 calc R . . H59C H 0.7663 0.5111 0.4338 0.201 Uiso 1 1 calc R . . C60 C 0.5280(12) 0.8971(12) 0.7857(13) 0.161(9) Uani 1 1 d . . . H60 H 0.4671 0.9126 0.7725 0.193 Uiso 1 1 calc R . . N1 N 1.2707(5) 0.9473(4) 0.6937(4) 0.0642(15) Uani 1 1 d . . . N2 N 0.8531(5) 0.8604(4) 0.6335(4) 0.0687(16) Uani 1 1 d . . . N3 N 1.5125(6) 0.6423(5) 0.8493(5) 0.0762(18) Uani 1 1 d . . . N4 N 1.3031(6) 0.7551(6) 0.9762(4) 0.0775(18) Uani 1 1 d . . . N5 N 1.1724(5) 0.6637(4) 0.6663(3) 0.0535(13) Uani 1 1 d . . . N6 N 0.5306(6) 0.5122(5) 0.6211(4) 0.0771(18) Uani 1 1 d . . . N7 N 0.5025(6) 0.3085(4) 0.8073(5) 0.0747(18) Uani 1 1 d . . . N8 N 0.8803(5) 0.5807(4) 0.8816(4) 0.0621(15) Uani 1 1 d . . . N9 N 1.1066(7) 1.1498(5) 0.5853(5) 0.085(2) Uani 1 1 d . . . N10 N 0.8594(6) 1.1756(4) 0.8138(4) 0.0752(17) Uani 1 1 d . . . N11 N 0.9352(4) 1.4158(3) 0.7793(3) 0.0542(13) Uani 1 1 d . . . H11 H 0.9024 1.3561 0.7785 0.065 Uiso 1 1 calc R . . N12 N 0.9134(5) 0.9027(4) 0.8683(4) 0.0750(18) Uani 1 1 d . . . H12 H 0.9246 0.9602 0.8862 0.090 Uiso 1 1 calc R . . O1 O 0.7759(5) 0.8756(5) 0.5974(6) 0.148(3) Uani 1 1 d . . . O2 O 0.8371(5) 0.7950(5) 0.6654(4) 0.103(2) Uani 1 1 d . . . O3 O 1.0465(4) 0.8200(3) 0.6878(3) 0.0627(12) Uani 1 1 d . . . O4 O 1.2592(5) 0.8709(4) 0.7022(5) 0.132(3) Uani 1 1 d . . . O5 O 1.3653(4) 1.0125(4) 0.7039(4) 0.0940(18) Uani 1 1 d . . . O6 O 1.5176(5) 0.6101(5) 0.7858(5) 0.107(2) Uani 1 1 d . . . O7 O 1.5801(5) 0.6563(5) 0.9202(4) 0.108(2) Uani 1 1 d . . . O8 O 1.2091(5) 0.6612(4) 0.6113(3) 0.0907(17) Uani 1 1 d . . . O9 O 1.0743(4) 0.6538(3) 0.6519(3) 0.0602(11) Uani 1 1 d . . . O10 O 1.2336(6) 0.6953(6) 0.9963(4) 0.130(3) Uani 1 1 d . . . O11 O 1.3570(8) 0.8379(6) 1.0129(5) 0.142(3) Uani 1 1 d . . . O12 O 0.5860(6) 0.5674(5) 0.5909(4) 0.133(3) Uani 1 1 d . . . O13 O 0.4270(5) 0.4722(7) 0.5897(5) 0.158(4) Uani 1 1 d . . . O14 O 0.4034(5) 0.2530(4) 0.7566(4) 0.111(2) Uani 1 1 d . . . O15 O 0.5459(5) 0.3009(5) 0.8773(5) 0.127(3) Uani 1 1 d . . . O16 O 0.9082(5) 0.5657(5) 0.9506(3) 0.116(2) Uani 1 1 d . . . O17 O 0.9531(4) 0.6390(3) 0.8644(3) 0.0658(12) Uani 1 1 d . . . O18 O 0.7764(4) 0.6198(3) 0.7238(3) 0.0603(11) Uani 1 1 d . . . O19 O 0.8330(4) 0.6252(3) 0.5839(3) 0.0660(13) Uani 1 1 d . . . O20 O 0.9224(4) 1.5262(3) 0.7130(3) 0.0589(11) Uani 1 1 d . . . O21 O 0.9878(4) 0.8107(3) 0.8362(3) 0.0599(11) Uani 1 1 d . . . O22 O 1.0232(7) 1.1631(5) 0.5575(5) 0.129(3) Uani 1 1 d . . . O23 O 1.2023(6) 1.2017(5) 0.5882(5) 0.127(3) Uani 1 1 d . . . O24 O 0.7274(4) 1.2745(3) 0.7506(3) 0.0624(12) Uani 1 1 d . . . O25 O 1.0341(6) 1.0875(3) 0.8773(4) 0.112(2) Uani 1 1 d . . . Tb1 Tb 0.96315(3) 0.69043(2) 0.73114(2) 0.04792(12) Uani 1 1 d . . . H19 H 0.762(5) 0.608(4) 0.603(3) 0.050(16) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O26 0.050(2) 0.054(3) 0.063(3) 0.017(2) 0.027(2) 0.027(2) C2 0.057(4) 0.045(4) 0.061(4) 0.020(3) 0.026(3) 0.017(3) C3 0.046(4) 0.045(3) 0.059(4) 0.021(3) 0.021(3) 0.024(3) C4 0.051(4) 0.048(4) 0.050(4) 0.022(3) 0.025(3) 0.024(3) C5 0.046(4) 0.044(3) 0.064(4) 0.021(3) 0.029(3) 0.019(3) C6 0.057(4) 0.040(3) 0.048(3) 0.011(3) 0.021(3) 0.027(3) C7 0.048(4) 0.054(4) 0.059(4) 0.026(3) 0.023(3) 0.032(3) C8 0.064(4) 0.042(3) 0.051(4) 0.009(3) 0.016(3) 0.035(3) C9 0.050(4) 0.047(4) 0.058(4) 0.021(3) 0.021(3) 0.019(3) C10 0.051(4) 0.052(4) 0.049(4) 0.008(3) 0.018(3) 0.020(3) C11 0.048(4) 0.037(3) 0.066(4) 0.012(3) 0.033(3) 0.019(3) C12 0.048(4) 0.048(4) 0.066(4) 0.019(3) 0.022(3) 0.020(3) C13 0.046(3) 0.046(3) 0.049(4) 0.020(3) 0.021(3) 0.021(3) C14 0.056(4) 0.049(4) 0.071(5) 0.016(3) 0.035(4) 0.023(3) C15 0.043(4) 0.051(4) 0.063(4) 0.010(3) 0.022(3) 0.020(3) C16 0.058(4) 0.064(4) 0.057(4) 0.015(3) 0.015(3) 0.033(4) C17 0.053(4) 0.055(4) 0.056(4) 0.019(3) 0.016(3) 0.012(3) C18 0.045(3) 0.040(3) 0.053(4) 0.014(3) 0.023(3) 0.020(3) C19 0.046(4) 0.047(4) 0.074(5) -0.001(3) 0.019(4) 0.027(3) C20 0.050(4) 0.044(3) 0.063(4) 0.021(3) 0.029(3) 0.019(3) C21 0.058(4) 0.054(4) 0.059(4) 0.020(3) 0.035(3) 0.025(3) C22 0.093(6) 0.058(4) 0.060(4) 0.006(4) 0.008(4) 0.043(4) C23 0.041(3) 0.047(4) 0.053(4) 0.009(3) 0.019(3) 0.018(3) C24 0.047(4) 0.052(4) 0.071(5) 0.013(3) 0.022(4) 0.027(3) C25 0.054(4) 0.055(4) 0.086(5) 0.029(4) 0.037(4) 0.026(3) C26 0.061(4) 0.066(4) 0.065(4) 0.026(4) 0.030(4) 0.042(4) C27 0.074(5) 0.056(4) 0.078(5) 0.011(4) 0.027(4) 0.041(4) C28 0.071(5) 0.043(4) 0.074(5) 0.027(3) 0.034(4) 0.031(3) C29 0.054(4) 0.062(4) 0.064(4) 0.013(4) 0.011(4) 0.029(4) C30 0.106(6) 0.061(5) 0.077(5) 0.009(4) 0.025(5) 0.053(5) C31 0.077(5) 0.085(6) 0.072(5) 0.028(4) 0.036(4) 0.041(5) C32 0.079(5) 0.065(5) 0.088(6) 0.018(4) 0.046(5) 0.039(4) C33 0.055(5) 0.081(5) 0.080(5) 0.008(4) 0.030(4) 0.012(4) C34 0.082(6) 0.075(6) 0.092(6) 0.006(5) 0.023(5) 0.035(5) C35 0.184(10) 0.073(6) 0.129(8) 0.069(6) 0.107(8) 0.079(7) C36 0.057(5) 0.063(5) 0.115(7) 0.003(5) 0.025(5) 0.029(4) C37 0.072(5) 0.098(6) 0.078(5) 0.042(5) 0.031(4) 0.049(5) C38 0.065(5) 0.067(5) 0.166(9) 0.042(5) 0.064(6) 0.036(4) C39 0.055(5) 0.157(10) 0.074(6) 0.012(7) 0.030(5) -0.001(6) C40 0.085(8) 0.133(10) 0.079(7) 0.054(7) 0.008(6) -0.023(8) C41 0.087(7) 0.082(7) 0.104(7) 0.049(6) -0.011(6) -0.012(6) C42 0.077(6) 0.059(5) 0.075(5) 0.029(4) -0.010(4) 0.005(4) C43 0.138(9) 0.095(7) 0.114(8) 0.039(7) 0.082(8) 0.065(7) C44 0.167(12) 0.174(13) 0.094(8) 0.056(9) 0.075(9) 0.126(11) C45 0.102(8) 0.143(10) 0.076(7) -0.010(7) 0.009(6) 0.061(8) C46 0.205(13) 0.092(7) 0.085(7) 0.004(5) 0.027(8) 0.105(8) C47 0.080(6) 0.106(7) 0.130(9) 0.063(7) 0.038(6) 0.058(6) C48 0.094(8) 0.109(8) 0.182(12) 0.045(9) 0.070(9) 0.065(7) C49 0.103(8) 0.101(7) 0.129(9) 0.014(7) 0.065(7) 0.048(6) C50 0.108(8) 0.083(6) 0.079(6) 0.001(5) -0.016(6) 0.058(6) C51 0.059(5) 0.095(7) 0.109(8) -0.026(6) -0.015(5) 0.038(5) C52 0.139(10) 0.053(5) 0.146(10) 0.002(6) -0.028(8) 0.043(6) C53 0.089(6) 0.063(5) 0.140(8) 0.050(5) 0.079(6) 0.036(4) C54 0.075(5) 0.076(5) 0.081(5) 0.022(4) 0.038(4) 0.041(4) C55 0.099(8) 0.083(7) 0.223(14) 0.060(8) 0.091(9) 0.067(6) C56 0.067(9) 0.168(16) 0.161(14) 0.115(13) -0.005(8) -0.003(9) C57 0.096(7) 0.087(6) 0.083(6) 0.022(5) 0.041(6) 0.003(6) C58 0.090(6) 0.094(7) 0.088(6) 0.054(6) 0.015(5) 0.022(5) C59 0.137(10) 0.168(11) 0.081(7) 0.004(7) 0.031(7) 0.079(9) C60 0.058(7) 0.155(15) 0.29(3) 0.139(17) 0.066(13) 0.057(9) N1 0.052(4) 0.062(4) 0.081(4) 0.038(3) 0.029(3) 0.024(3) N2 0.055(4) 0.067(4) 0.095(5) 0.032(4) 0.033(3) 0.034(3) N3 0.066(4) 0.069(4) 0.117(6) 0.036(4) 0.042(4) 0.047(4) N4 0.077(5) 0.102(6) 0.056(4) 0.011(4) 0.024(4) 0.050(4) N5 0.061(4) 0.052(3) 0.055(3) 0.019(3) 0.027(3) 0.031(3) N6 0.065(4) 0.086(5) 0.075(4) 0.034(4) 0.020(4) 0.036(4) N7 0.062(4) 0.062(4) 0.098(5) 0.036(4) 0.043(4) 0.017(3) N8 0.059(4) 0.066(4) 0.060(4) 0.021(3) 0.029(3) 0.023(3) N9 0.087(5) 0.076(5) 0.118(6) 0.057(4) 0.049(5) 0.049(4) N10 0.112(5) 0.055(4) 0.069(4) 0.016(3) 0.033(4) 0.053(4) N11 0.048(3) 0.041(3) 0.064(3) 0.023(3) 0.014(3) 0.019(2) N12 0.063(4) 0.038(3) 0.132(6) 0.021(3) 0.047(4) 0.027(3) O1 0.065(4) 0.138(6) 0.264(10) 0.119(7) 0.063(5) 0.055(4) O2 0.072(4) 0.112(5) 0.149(6) 0.082(4) 0.065(4) 0.039(3) O3 0.059(3) 0.055(3) 0.082(3) 0.038(2) 0.033(2) 0.027(2) O4 0.077(4) 0.092(4) 0.268(9) 0.113(5) 0.078(5) 0.057(3) O5 0.054(3) 0.076(4) 0.151(5) 0.050(4) 0.042(3) 0.026(3) O6 0.109(5) 0.122(5) 0.142(6) 0.035(4) 0.070(4) 0.087(4) O7 0.078(4) 0.130(5) 0.125(5) 0.045(4) 0.022(4) 0.070(4) O8 0.103(4) 0.141(5) 0.063(3) 0.038(3) 0.052(3) 0.074(4) O9 0.056(3) 0.077(3) 0.054(3) 0.026(2) 0.021(2) 0.037(2) O10 0.118(5) 0.159(7) 0.083(4) 0.007(4) 0.061(4) 0.031(5) O11 0.195(8) 0.099(5) 0.118(6) -0.011(5) 0.074(5) 0.060(5) O12 0.094(5) 0.118(5) 0.114(5) 0.070(4) -0.005(4) 0.015(4) O13 0.053(4) 0.264(10) 0.151(6) 0.131(7) 0.026(4) 0.065(5) O14 0.082(4) 0.069(4) 0.126(5) 0.027(4) 0.037(4) -0.009(3) O15 0.093(5) 0.138(6) 0.132(6) 0.094(5) 0.049(4) 0.021(4) O16 0.072(4) 0.157(6) 0.060(3) 0.050(4) 0.011(3) 0.011(4) O17 0.063(3) 0.059(3) 0.068(3) 0.023(2) 0.027(3) 0.021(2) O18 0.051(3) 0.057(3) 0.081(3) 0.034(2) 0.033(2) 0.024(2) O19 0.059(3) 0.078(3) 0.062(3) 0.042(3) 0.023(2) 0.030(3) O20 0.071(3) 0.045(3) 0.065(3) 0.026(2) 0.028(2) 0.029(2) O21 0.053(3) 0.045(3) 0.083(3) 0.015(2) 0.031(2) 0.023(2) O22 0.148(6) 0.136(6) 0.213(8) 0.124(6) 0.114(6) 0.116(5) O23 0.085(4) 0.093(5) 0.191(7) 0.095(5) 0.041(5) 0.030(4) O24 0.068(3) 0.045(3) 0.081(3) 0.026(2) 0.037(3) 0.026(2) O25 0.099(5) 0.042(3) 0.148(6) 0.029(3) 0.001(4) 0.030(3) Tb1 0.0484(2) 0.04295(18) 0.0620(2) 0.02548(14) 0.02780(15) 0.02363(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 O26 C18 1.272(7) . ? O26 Tb1 2.263(4) . ? C2 C3 1.359(8) . ? C2 C28 1.375(9) . ? C2 H2 0.9300 . ? C3 C4 1.436(8) . ? C3 N1 1.459(8) . ? C4 O3 1.267(7) . ? C4 C20 1.417(8) . ? C5 C21 1.364(8) . ? C5 C15 1.369(8) . ? C5 N7 1.463(8) . ? C6 O20 1.253(7) . ? C6 N11 1.313(7) . ? C6 C8 1.497(8) . ? C7 C15 1.360(8) . ? C7 C11 1.445(8) . ? C7 N6 1.447(8) . ? C8 C22 1.378(9) . ? C8 C19 1.401(9) . ? C9 C31 1.346(9) . ? C9 C37 1.382(9) . ? C9 C16 1.492(9) . ? C10 C29 1.362(9) . ? C10 C18 1.428(8) . ? C10 N4 1.455(8) . ? C11 O18 1.262(6) . ? C11 C23 1.425(8) . ? C12 O21 1.240(7) . ? C12 N12 1.306(8) . ? C12 C17 1.488(9) . ? C13 C14 1.388(8) . ? C13 C18 1.417(8) . ? C13 N5 1.465(7) . ? C14 C24 1.371(9) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 N11 1.461(8) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C42 1.380(10) . ? C17 C33 1.389(10) . ? C19 O24 1.360(8) . ? C19 C36 1.365(9) . ? C20 C26 1.372(8) . ? C20 N2 1.457(8) . ? C21 C23 1.379(8) . ? C21 H21 0.9300 . ? C22 C50 1.369(11) . ? C22 H22 0.9300 . ? C23 N8 1.465(8) . ? C24 C29 1.365(9) . ? C24 N3 1.470(8) . ? C25 C57 1.368(11) . ? C25 C54 1.379(10) . ? C25 C38 1.484(9) . ? C26 C28 1.371(9) . ? C26 H26 0.9300 . ? C27 C32 1.347(10) . ? C27 C34 1.375(10) . ? C27 C30 1.511(10) . ? C28 N9 1.460(8) . ? C29 H29 0.9300 . ? C30 N10 1.466(9) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C49 1.400(12) . ? C31 H31 0.9300 . ? C32 C43 1.354(12) . ? C32 H32 0.9300 . ? C33 C39 1.389(11) . ? C33 H33 0.9300 . ? C34 C45 1.415(13) . ? C34 H34 0.9300 . ? C35 N10 1.448(10) . ? C35 C53 1.503(12) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 C51 1.389(12) . ? C36 H36 0.9300 . ? C37 C47 1.380(11) . ? C37 H37 0.9300 . ? C38 N12 1.486(8) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 C40 1.359(16) . ? C39 H39 0.9300 . ? C40 C41 1.341(16) . ? C40 H40 0.9300 . ? C41 C42 1.424(12) . ? C41 H41 0.9300 . ? C42 O25 1.346(11) . ? C43 C44 1.345(14) . ? C43 H43 0.9300 . ? C44 C45 1.367(14) . ? C44 H44 0.9300 . ? C45 H45 0.9300 . ? C46 C52 1.402(15) . ? C46 N10 1.486(11) . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C47 C48 1.337(13) . ? C47 H47 0.9300 . ? C48 C49 1.360(14) . ? C48 H48 0.9300 . ? C49 H49 0.9300 . ? C50 C51 1.339(13) . ? C50 H50 0.9300 . ? C51 H51 0.9300 . ? C52 O25 1.425(10) . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C53 O24 1.434(7) . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C54 C55 1.332(11) . ? C54 H54 0.9300 . ? C55 C60 1.302(18) . ? C55 H55 0.9300 . ? C56 C60 1.33(2) . ? C56 C57 1.414(17) . ? C56 H56 0.9300 . ? C57 H57 0.9300 . ? C58 O19 1.427(9) . ? C58 C59 1.467(13) . ? C58 H58A 0.9700 . ? C58 H58B 0.9700 . ? C59 H59A 0.9600 . ? C59 H59B 0.9600 . ? C59 H59C 0.9600 . ? C60 H60 0.9300 . ? N1 O4 1.188(7) . ? N1 O5 1.219(6) . ? N2 O1 1.175(7) . ? N2 O2 1.208(7) . ? N3 O6 1.204(8) . ? N3 O7 1.210(8) . ? N4 O11 1.174(8) . ? N4 O10 1.217(8) . ? N5 O9 1.220(6) . ? N5 O8 1.225(6) . ? N6 O13 1.178(7) . ? N6 O12 1.202(8) . ? N7 O14 1.207(7) . ? N7 O15 1.218(8) . ? N8 O17 1.202(6) . ? N8 O16 1.224(7) . ? N9 O22 1.201(8) . ? N9 O23 1.208(8) . ? N11 H11 0.8600 . ? N12 H12 0.8600 . ? O3 Tb1 2.258(4) . ? O9 Tb1 2.548(5) . ? O17 Tb1 2.584(5) . ? O18 Tb1 2.283(4) . ? O19 Tb1 2.400(4) . ? O19 H19 1.08(6) . ? O20 Tb1 2.384(4) 1_565 ? O21 Tb1 2.319(4) . ? Tb1 O20 2.384(4) 1_545 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C18 O26 Tb1 140.8(4) . . ? C3 C2 C28 119.7(6) . . ? C3 C2 H2 120.2 . . ? C28 C2 H2 120.2 . . ? C2 C3 C4 123.0(6) . . ? C2 C3 N1 116.7(5) . . ? C4 C3 N1 120.3(5) . . ? O3 C4 C20 123.8(5) . . ? O3 C4 C3 122.5(6) . . ? C20 C4 C3 113.7(5) . . ? C21 C5 C15 122.8(6) . . ? C21 C5 N7 117.3(6) . . ? C15 C5 N7 120.0(6) . . ? O20 C6 N11 121.8(6) . . ? O20 C6 C8 118.9(5) . . ? N11 C6 C8 119.3(5) . . ? C15 C7 C11 123.4(6) . . ? C15 C7 N6 116.7(6) . . ? C11 C7 N6 119.9(6) . . ? C22 C8 C19 117.9(6) . . ? C22 C8 C6 117.9(6) . . ? C19 C8 C6 124.1(6) . . ? C31 C9 C37 117.9(7) . . ? C31 C9 C16 123.4(6) . . ? C37 C9 C16 118.7(6) . . ? C29 C10 C18 124.3(6) . . ? C29 C10 N4 118.9(6) . . ? C18 C10 N4 116.8(6) . . ? O18 C11 C23 124.3(6) . . ? O18 C11 C7 122.1(6) . . ? C23 C11 C7 113.6(5) . . ? O21 C12 N12 120.3(6) . . ? O21 C12 C17 119.9(6) . . ? N12 C12 C17 119.8(6) . . ? C14 C13 C18 123.2(6) . . ? C14 C13 N5 117.1(5) . . ? C18 C13 N5 119.7(5) . . ? C24 C14 C13 119.1(6) . . ? C24 C14 H14 120.4 . . ? C13 C14 H14 120.4 . . ? C7 C15 C5 118.6(6) . . ? C7 C15 H15 120.7 . . ? C5 C15 H15 120.7 . . ? N11 C16 C9 113.6(5) . . ? N11 C16 H16A 108.8 . . ? C9 C16 H16A 108.8 . . ? N11 C16 H16B 108.8 . . ? C9 C16 H16B 108.8 . . ? H16A C16 H16B 107.7 . . ? C42 C17 C33 119.7(7) . . ? C42 C17 C12 125.3(7) . . ? C33 C17 C12 115.0(7) . . ? O26 C18 C13 127.1(6) . . ? O26 C18 C10 120.0(5) . . ? C13 C18 C10 112.9(5) . . ? O24 C19 C36 123.9(7) . . ? O24 C19 C8 116.7(6) . . ? C36 C19 C8 119.4(7) . . ? C26 C20 C4 123.4(6) . . ? C26 C20 N2 116.4(6) . . ? C4 C20 N2 120.2(5) . . ? C5 C21 C23 118.7(6) . . ? C5 C21 H21 120.6 . . ? C23 C21 H21 120.6 . . ? C50 C22 C8 121.8(8) . . ? C50 C22 H22 119.1 . . ? C8 C22 H22 119.1 . . ? C21 C23 C11 123.0(6) . . ? C21 C23 N8 114.6(6) . . ? C11 C23 N8 122.5(5) . . ? C29 C24 C14 121.2(6) . . ? C29 C24 N3 119.6(7) . . ? C14 C24 N3 119.2(7) . . ? C57 C25 C54 118.2(8) . . ? C57 C25 C38 120.5(8) . . ? C54 C25 C38 121.3(8) . . ? C28 C26 C20 119.3(6) . . ? C28 C26 H26 120.4 . . ? C20 C26 H26 120.4 . . ? C32 C27 C34 117.4(8) . . ? C32 C27 C30 121.9(7) . . ? C34 C27 C30 120.7(8) . . ? C26 C28 C2 121.0(6) . . ? C26 C28 N9 119.8(6) . . ? C2 C28 N9 119.2(6) . . ? C10 C29 C24 119.2(6) . . ? C10 C29 H29 120.4 . . ? C24 C29 H29 120.4 . . ? N10 C30 C27 112.9(6) . . ? N10 C30 H30A 109.0 . . ? C27 C30 H30A 109.0 . . ? N10 C30 H30B 109.0 . . ? C27 C30 H30B 109.0 . . ? H30A C30 H30B 107.8 . . ? C9 C31 C49 121.1(8) . . ? C9 C31 H31 119.5 . . ? C49 C31 H31 119.5 . . ? C27 C32 C43 123.6(9) . . ? C27 C32 H32 118.2 . . ? C43 C32 H32 118.2 . . ? C17 C33 C39 120.3(9) . . ? C17 C33 H33 119.9 . . ? C39 C33 H33 119.9 . . ? C27 C34 C45 120.9(9) . . ? C27 C34 H34 119.6 . . ? C45 C34 H34 119.6 . . ? N10 C35 C53 114.5(7) . . ? N10 C35 H35A 108.6 . . ? C53 C35 H35A 108.6 . . ? N10 C35 H35B 108.6 . . ? C53 C35 H35B 108.6 . . ? H35A C35 H35B 107.6 . . ? C19 C36 C51 121.0(8) . . ? C19 C36 H36 119.5 . . ? C51 C36 H36 119.5 . . ? C47 C37 C9 120.7(8) . . ? C47 C37 H37 119.6 . . ? C9 C37 H37 119.6 . . ? C25 C38 N12 111.4(6) . . ? C25 C38 H38A 109.4 . . ? N12 C38 H38A 109.4 . . ? C25 C38 H38B 109.4 . . ? N12 C38 H38B 109.4 . . ? H38A C38 H38B 108.0 . . ? C40 C39 C33 119.0(11) . . ? C40 C39 H39 120.5 . . ? C33 C39 H39 120.5 . . ? C41 C40 C39 122.5(10) . . ? C41 C40 H40 118.7 . . ? C39 C40 H40 118.7 . . ? C40 C41 C42 119.5(11) . . ? C40 C41 H41 120.2 . . ? C42 C41 H41 120.2 . . ? O25 C42 C17 118.5(7) . . ? O25 C42 C41 122.8(9) . . ? C17 C42 C41 118.7(10) . . ? C44 C43 C32 118.8(10) . . ? C44 C43 H43 120.6 . . ? C32 C43 H43 120.6 . . ? C43 C44 C45 121.9(11) . . ? C43 C44 H44 119.1 . . ? C45 C44 H44 119.1 . . ? C44 C45 C34 117.4(10) . . ? C44 C45 H45 121.3 . . ? C34 C45 H45 121.3 . . ? C52 C46 N10 117.7(9) . . ? C52 C46 H46A 107.9 . . ? N10 C46 H46A 107.9 . . ? C52 C46 H46B 107.9 . . ? N10 C46 H46B 107.9 . . ? H46A C46 H46B 107.2 . . ? C48 C47 C37 120.8(9) . . ? C48 C47 H47 119.6 . . ? C37 C47 H47 119.6 . . ? C47 C48 C49 119.6(10) . . ? C47 C48 H48 120.2 . . ? C49 C48 H48 120.2 . . ? C48 C49 C31 119.8(10) . . ? C48 C49 H49 120.1 . . ? C31 C49 H49 120.1 . . ? C51 C50 C22 120.1(9) . . ? C51 C50 H50 120.0 . . ? C22 C50 H50 120.0 . . ? C50 C51 C36 119.8(8) . . ? C50 C51 H51 120.1 . . ? C36 C51 H51 120.1 . . ? C46 C52 O25 109.6(9) . . ? C46 C52 H52A 109.7 . . ? O25 C52 H52A 109.7 . . ? C46 C52 H52B 109.7 . . ? O25 C52 H52B 109.7 . . ? H52A C52 H52B 108.2 . . ? O24 C53 C35 106.4(6) . . ? O24 C53 H53A 110.5 . . ? C35 C53 H53A 110.5 . . ? O24 C53 H53B 110.5 . . ? C35 C53 H53B 110.5 . . ? H53A C53 H53B 108.6 . . ? C55 C54 C25 121.3(9) . . ? C55 C54 H54 119.4 . . ? C25 C54 H54 119.4 . . ? C60 C55 C54 121.4(13) . . ? C60 C55 H55 119.3 . . ? C54 C55 H55 119.3 . . ? C60 C56 C57 120.8(15) . . ? C60 C56 H56 119.6 . . ? C57 C56 H56 119.6 . . ? C25 C57 C56 117.5(11) . . ? C25 C57 H57 121.2 . . ? C56 C57 H57 121.2 . . ? O19 C58 C59 112.1(7) . . ? O19 C58 H58A 109.2 . . ? C59 C58 H58A 109.2 . . ? O19 C58 H58B 109.2 . . ? C59 C58 H58B 109.2 . . ? H58A C58 H58B 107.9 . . ? C58 C59 H59A 109.5 . . ? C58 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C58 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C55 C60 C56 120.7(16) . . ? C55 C60 H60 119.6 . . ? C56 C60 H60 119.6 . . ? O4 N1 O5 121.9(6) . . ? O4 N1 C3 120.0(5) . . ? O5 N1 C3 117.9(6) . . ? O1 N2 O2 121.4(7) . . ? O1 N2 C20 117.8(6) . . ? O2 N2 C20 120.7(6) . . ? O6 N3 O7 124.8(7) . . ? O6 N3 C24 117.7(7) . . ? O7 N3 C24 117.5(7) . . ? O11 N4 O10 123.6(7) . . ? O11 N4 C10 118.9(8) . . ? O10 N4 C10 117.5(7) . . ? O9 N5 O8 122.9(5) . . ? O9 N5 C13 119.9(5) . . ? O8 N5 C13 117.2(5) . . ? O13 N6 O12 120.8(7) . . ? O13 N6 C7 118.5(7) . . ? O12 N6 C7 120.5(6) . . ? O14 N7 O15 123.6(7) . . ? O14 N7 C5 118.4(7) . . ? O15 N7 C5 117.9(6) . . ? O17 N8 O16 120.3(6) . . ? O17 N8 C23 120.2(6) . . ? O16 N8 C23 119.5(6) . . ? O22 N9 O23 123.6(7) . . ? O22 N9 C28 118.4(7) . . ? O23 N9 C28 117.9(7) . . ? C35 N10 C30 113.6(7) . . ? C35 N10 C46 106.6(7) . . ? C30 N10 C46 112.8(6) . . ? C6 N11 C16 124.3(5) . . ? C6 N11 H11 117.9 . . ? C16 N11 H11 117.9 . . ? C12 N12 C38 123.0(6) . . ? C12 N12 H12 118.5 . . ? C38 N12 H12 118.5 . . ? C4 O3 Tb1 157.5(4) . . ? N5 O9 Tb1 139.0(4) . . ? N8 O17 Tb1 136.7(4) . . ? C11 O18 Tb1 137.4(4) . . ? C58 O19 Tb1 129.9(4) . . ? C58 O19 H19 137(3) . . ? Tb1 O19 H19 87(3) . . ? C6 O20 Tb1 155.8(4) . 1_565 ? C12 O21 Tb1 147.9(4) . . ? C19 O24 C53 120.0(6) . . ? C42 O25 C52 118.9(8) . . ? O3 Tb1 O26 86.96(15) . . ? O3 Tb1 O18 126.94(15) . . ? O26 Tb1 O18 139.71(15) . . ? O3 Tb1 O21 80.59(16) . . ? O26 Tb1 O21 83.37(15) . . ? O18 Tb1 O21 82.04(15) . . ? O3 Tb1 O20 141.69(16) . 1_545 ? O26 Tb1 O20 85.61(15) . 1_545 ? O18 Tb1 O20 79.08(15) . 1_545 ? O21 Tb1 O20 135.44(15) . 1_545 ? O3 Tb1 O19 81.25(16) . . ? O26 Tb1 O19 140.53(16) . . ? O18 Tb1 O19 73.39(16) . . ? O21 Tb1 O19 130.73(16) . . ? O20 Tb1 O19 80.98(15) 1_545 . ? O3 Tb1 O9 72.16(15) . . ? O26 Tb1 O9 67.84(14) . . ? O18 Tb1 O9 137.01(16) . . ? O21 Tb1 O9 140.80(15) . . ? O20 Tb1 O9 70.22(14) 1_545 . ? O19 Tb1 O9 72.69(15) . . ? O3 Tb1 O17 142.54(16) . . ? O26 Tb1 O17 72.45(14) . . ? O18 Tb1 O17 67.28(15) . . ? O21 Tb1 O17 66.50(15) . . ? O20 Tb1 O17 68.99(14) 1_545 . ? O19 Tb1 O17 133.88(15) . . ? O9 Tb1 O17 124.08(14) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C28 C2 C3 C4 -0.4(10) . . . . ? C28 C2 C3 N1 179.7(6) . . . . ? C2 C3 C4 O3 179.5(6) . . . . ? N1 C3 C4 O3 -0.6(9) . . . . ? C2 C3 C4 C20 -0.1(9) . . . . ? N1 C3 C4 C20 179.7(5) . . . . ? O20 C6 C8 C22 18.5(9) . . . . ? N11 C6 C8 C22 -160.0(6) . . . . ? O20 C6 C8 C19 -158.4(6) . . . . ? N11 C6 C8 C19 23.1(9) . . . . ? C15 C7 C11 O18 177.0(6) . . . . ? N6 C7 C11 O18 -6.3(9) . . . . ? C15 C7 C11 C23 -2.5(8) . . . . ? N6 C7 C11 C23 174.2(6) . . . . ? C18 C13 C14 C24 -1.0(9) . . . . ? N5 C13 C14 C24 -179.8(5) . . . . ? C11 C7 C15 C5 1.3(9) . . . . ? N6 C7 C15 C5 -175.5(6) . . . . ? C21 C5 C15 C7 0.9(9) . . . . ? N7 C5 C15 C7 -179.0(6) . . . . ? C31 C9 C16 N11 41.3(9) . . . . ? C37 C9 C16 N11 -140.6(6) . . . . ? O21 C12 C17 C42 165.0(7) . . . . ? N12 C12 C17 C42 -16.1(11) . . . . ? O21 C12 C17 C33 -13.5(9) . . . . ? N12 C12 C17 C33 165.4(7) . . . . ? Tb1 O26 C18 C13 25.2(10) . . . . ? Tb1 O26 C18 C10 -156.5(4) . . . . ? C14 C13 C18 O26 -178.6(5) . . . . ? N5 C13 C18 O26 0.1(9) . . . . ? C14 C13 C18 C10 2.9(8) . . . . ? N5 C13 C18 C10 -178.3(5) . . . . ? C29 C10 C18 O26 177.3(6) . . . . ? N4 C10 C18 O26 0.6(9) . . . . ? C29 C10 C18 C13 -4.1(9) . . . . ? N4 C10 C18 C13 179.2(6) . . . . ? C22 C8 C19 O24 -179.7(6) . . . . ? C6 C8 C19 O24 -2.8(9) . . . . ? C22 C8 C19 C36 -0.3(9) . . . . ? C6 C8 C19 C36 176.6(6) . . . . ? O3 C4 C20 C26 -179.3(6) . . . . ? C3 C4 C20 C26 0.3(9) . . . . ? O3 C4 C20 N2 1.0(10) . . . . ? C3 C4 C20 N2 -179.3(6) . . . . ? C15 C5 C21 C23 -1.5(9) . . . . ? N7 C5 C21 C23 178.4(5) . . . . ? C19 C8 C22 C50 0.5(11) . . . . ? C6 C8 C22 C50 -176.6(7) . . . . ? C5 C21 C23 C11 -0.1(9) . . . . ? C5 C21 C23 N8 178.9(5) . . . . ? O18 C11 C23 C21 -177.7(6) . . . . ? C7 C11 C23 C21 1.9(8) . . . . ? O18 C11 C23 N8 3.5(9) . . . . ? C7 C11 C23 N8 -176.9(5) . . . . ? C13 C14 C24 C29 -0.2(10) . . . . ? C13 C14 C24 N3 177.7(5) . . . . ? C4 C20 C26 C28 0.0(10) . . . . ? N2 C20 C26 C28 179.7(6) . . . . ? C20 C26 C28 C2 -0.5(10) . . . . ? C20 C26 C28 N9 178.6(6) . . . . ? C3 C2 C28 C26 0.7(10) . . . . ? C3 C2 C28 N9 -178.4(6) . . . . ? C18 C10 C29 C24 3.2(10) . . . . ? N4 C10 C29 C24 179.9(7) . . . . ? C14 C24 C29 C10 -0.9(10) . . . . ? N3 C24 C29 C10 -178.8(6) . . . . ? C32 C27 C30 N10 46.8(10) . . . . ? C34 C27 C30 N10 -134.8(8) . . . . ? C37 C9 C31 C49 1.0(11) . . . . ? C16 C9 C31 C49 179.1(7) . . . . ? C34 C27 C32 C43 2.0(11) . . . . ? C30 C27 C32 C43 -179.6(7) . . . . ? C42 C17 C33 C39 -1.0(11) . . . . ? C12 C17 C33 C39 177.6(7) . . . . ? C32 C27 C34 C45 -0.9(12) . . . . ? C30 C27 C34 C45 -179.4(8) . . . . ? O24 C19 C36 C51 178.6(7) . . . . ? C8 C19 C36 C51 -0.7(11) . . . . ? C31 C9 C37 C47 1.1(11) . . . . ? C16 C9 C37 C47 -177.1(7) . . . . ? C57 C25 C38 N12 101.1(9) . . . . ? C54 C25 C38 N12 -79.5(9) . . . . ? C17 C33 C39 C40 -3.0(13) . . . . ? C33 C39 C40 C41 3.0(17) . . . . ? C39 C40 C41 C42 0.9(18) . . . . ? C33 C17 C42 O25 -177.3(7) . . . . ? C12 C17 C42 O25 4.3(12) . . . . ? C33 C17 C42 C41 4.8(12) . . . . ? C12 C17 C42 C41 -173.7(7) . . . . ? C40 C41 C42 O25 177.3(9) . . . . ? C40 C41 C42 C17 -4.8(15) . . . . ? C27 C32 C43 C44 -1.9(14) . . . . ? C32 C43 C44 C45 0.7(16) . . . . ? C43 C44 C45 C34 0.3(16) . . . . ? C27 C34 C45 C44 -0.1(14) . . . . ? C9 C37 C47 C48 -1.1(14) . . . . ? C37 C47 C48 C49 -1.2(16) . . . . ? C47 C48 C49 C31 3.3(16) . . . . ? C9 C31 C49 C48 -3.2(14) . . . . ? C8 C22 C50 C51 0.4(14) . . . . ? C22 C50 C51 C36 -1.4(15) . . . . ? C19 C36 C51 C50 1.6(13) . . . . ? N10 C46 C52 O25 -91.6(11) . . . . ? N10 C35 C53 O24 -64.4(9) . . . . ? C57 C25 C54 C55 -1.9(11) . . . . ? C38 C25 C54 C55 178.7(7) . . . . ? C25 C54 C55 C60 3.6(15) . . . . ? C54 C25 C57 C56 0.7(12) . . . . ? C38 C25 C57 C56 -179.9(8) . . . . ? C60 C56 C57 C25 -1.1(19) . . . . ? C54 C55 C60 C56 -4(2) . . . . ? C57 C56 C60 C55 3(2) . . . . ? C2 C3 N1 O4 -167.1(8) . . . . ? C4 C3 N1 O4 13.0(10) . . . . ? C2 C3 N1 O5 9.5(9) . . . . ? C4 C3 N1 O5 -170.4(6) . . . . ? C26 C20 N2 O1 12.2(11) . . . . ? C4 C20 N2 O1 -168.1(8) . . . . ? C26 C20 N2 O2 -169.5(7) . . . . ? C4 C20 N2 O2 10.2(10) . . . . ? C29 C24 N3 O6 176.4(7) . . . . ? C14 C24 N3 O6 -1.5(10) . . . . ? C29 C24 N3 O7 -4.5(10) . . . . ? C14 C24 N3 O7 177.6(7) . . . . ? C29 C10 N4 O11 86.2(10) . . . . ? C18 C10 N4 O11 -96.8(9) . . . . ? C29 C10 N4 O10 -95.5(9) . . . . ? C18 C10 N4 O10 81.4(9) . . . . ? C14 C13 N5 O9 159.2(5) . . . . ? C18 C13 N5 O9 -19.7(8) . . . . ? C14 C13 N5 O8 -19.7(8) . . . . ? C18 C13 N5 O8 161.5(6) . . . . ? C15 C7 N6 O13 10.2(11) . . . . ? C11 C7 N6 O13 -166.7(8) . . . . ? C15 C7 N6 O12 -166.4(8) . . . . ? C11 C7 N6 O12 16.7(11) . . . . ? C21 C5 N7 O14 -172.3(7) . . . . ? C15 C5 N7 O14 7.6(10) . . . . ? C21 C5 N7 O15 10.6(10) . . . . ? C15 C5 N7 O15 -169.5(7) . . . . ? C21 C23 N8 O17 166.8(6) . . . . ? C11 C23 N8 O17 -14.3(9) . . . . ? C21 C23 N8 O16 -11.4(9) . . . . ? C11 C23 N8 O16 167.6(7) . . . . ? C26 C28 N9 O22 -2.9(12) . . . . ? C2 C28 N9 O22 176.2(8) . . . . ? C26 C28 N9 O23 179.8(8) . . . . ? C2 C28 N9 O23 -1.1(11) . . . . ? C53 C35 N10 C30 -64.5(8) . . . . ? C53 C35 N10 C46 170.5(7) . . . . ? C27 C30 N10 C35 90.0(8) . . . . ? C27 C30 N10 C46 -148.4(8) . . . . ? C52 C46 N10 C35 177.5(8) . . . . ? C52 C46 N10 C30 52.0(12) . . . . ? O20 C6 N11 C16 6.3(10) . . . . ? C8 C6 N11 C16 -175.3(5) . . . . ? C9 C16 N11 C6 -118.7(7) . . . . ? O21 C12 N12 C38 -3.4(11) . . . . ? C17 C12 N12 C38 177.7(7) . . . . ? C25 C38 N12 C12 -152.0(7) . . . . ? C20 C4 O3 Tb1 -18.4(15) . . . . ? C3 C4 O3 Tb1 162.0(8) . . . . ? O8 N5 O9 Tb1 -160.3(5) . . . . ? C13 N5 O9 Tb1 21.0(8) . . . . ? O16 N8 O17 Tb1 170.7(5) . . . . ? C23 N8 O17 Tb1 -7.5(9) . . . . ? C23 C11 O18 Tb1 36.0(9) . . . . ? C7 C11 O18 Tb1 -143.5(5) . . . . ? C59 C58 O19 Tb1 113.5(7) . . . . ? N11 C6 O20 Tb1 -98.5(10) . . . 1_565 ? C8 C6 O20 Tb1 83.1(11) . . . 1_565 ? N12 C12 O21 Tb1 108.6(8) . . . . ? C17 C12 O21 Tb1 -72.5(10) . . . . ? C36 C19 O24 C53 17.3(9) . . . . ? C8 C19 O24 C53 -163.4(6) . . . . ? C35 C53 O24 C19 158.5(6) . . . . ? C17 C42 O25 C52 174.5(8) . . . . ? C41 C42 O25 C52 -7.7(14) . . . . ? C46 C52 O25 C42 -173.6(9) . . . . ? C4 O3 Tb1 O26 -138.6(11) . . . . ? C4 O3 Tb1 O18 17.7(12) . . . . ? C4 O3 Tb1 O21 -54.8(11) . . . . ? C4 O3 Tb1 O20 142.4(11) . . . 1_545 ? C4 O3 Tb1 O19 79.2(11) . . . . ? C4 O3 Tb1 O9 153.7(12) . . . . ? C4 O3 Tb1 O17 -83.1(11) . . . . ? C18 O26 Tb1 O3 -92.0(6) . . . . ? C18 O26 Tb1 O18 117.8(6) . . . . ? C18 O26 Tb1 O21 -172.9(6) . . . . ? C18 O26 Tb1 O20 50.4(6) . . . 1_545 ? C18 O26 Tb1 O19 -19.7(7) . . . . ? C18 O26 Tb1 O9 -20.0(6) . . . . ? C18 O26 Tb1 O17 119.7(6) . . . . ? C11 O18 Tb1 O3 -178.2(5) . . . . ? C11 O18 Tb1 O26 -36.5(7) . . . . ? C11 O18 Tb1 O21 -106.4(6) . . . . ? C11 O18 Tb1 O20 33.1(6) . . . 1_545 ? C11 O18 Tb1 O19 116.8(6) . . . . ? C11 O18 Tb1 O9 77.7(6) . . . . ? C11 O18 Tb1 O17 -38.6(6) . . . . ? C12 O21 Tb1 O3 24.4(8) . . . . ? C12 O21 Tb1 O26 112.4(8) . . . . ? C12 O21 Tb1 O18 -105.3(8) . . . . ? C12 O21 Tb1 O20 -170.8(7) . . . 1_545 ? C12 O21 Tb1 O19 -45.4(8) . . . . ? C12 O21 Tb1 O9 70.4(8) . . . . ? C12 O21 Tb1 O17 -173.9(8) . . . . ? C58 O19 Tb1 O3 30.1(7) . . . . ? C58 O19 Tb1 O26 -44.2(7) . . . . ? C58 O19 Tb1 O18 163.0(7) . . . . ? C58 O19 Tb1 O21 99.6(7) . . . . ? C58 O19 Tb1 O20 -115.8(7) . . . 1_545 ? C58 O19 Tb1 O9 -43.8(6) . . . . ? C58 O19 Tb1 O17 -164.8(6) . . . . ? N5 O9 Tb1 O3 89.5(6) . . . . ? N5 O9 Tb1 O26 -4.6(5) . . . . ? N5 O9 Tb1 O18 -145.0(5) . . . . ? N5 O9 Tb1 O21 41.3(7) . . . . ? N5 O9 Tb1 O20 -97.9(6) . . . 1_545 ? N5 O9 Tb1 O19 175.6(6) . . . . ? N5 O9 Tb1 O17 -52.6(6) . . . . ? N8 O17 Tb1 O3 145.8(6) . . . . ? N8 O17 Tb1 O26 -154.5(6) . . . . ? N8 O17 Tb1 O18 24.1(6) . . . . ? N8 O17 Tb1 O21 115.2(6) . . . . ? N8 O17 Tb1 O20 -62.5(6) . . . 1_545 ? N8 O17 Tb1 O19 -9.5(7) . . . . ? N8 O17 Tb1 O9 -108.2(6) . . . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.712 _refine_diff_density_min -0.708 _refine_diff_density_rms 0.086 #===END data_852910 _database_code_depnum_ccdc_archive 'CCDC 852910' #TrackingRef '- cif_Revision.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C59 H51 Er N12 O26' _chemical_formula_weight 1511.38 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' Er Er -0.2586 4.9576 '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 13.7022(10) _cell_length_b 15.7923(11) _cell_length_c 17.4802(12) _cell_angle_alpha 96.6430(10) _cell_angle_beta 108.9350(10) _cell_angle_gamma 114.1490(10) _cell_volume 3126.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 4017 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 21.24 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.605 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1530 _exptl_absorpt_coefficient_mu 1.439 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7150 _exptl_absorpt_correction_T_max 0.7240 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16763 _diffrn_reflns_av_R_equivalents 0.0277 _diffrn_reflns_av_sigmaI/netI 0.0654 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 25.93 _reflns_number_total 11806 _reflns_number_gt 9117 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11806 _refine_ls_number_parameters 888 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0643 _refine_ls_R_factor_gt 0.0449 _refine_ls_wR_factor_ref 0.0676 _refine_ls_wR_factor_gt 0.0630 _refine_ls_goodness_of_fit_ref 1.197 _refine_ls_restrained_S_all 1.197 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 1.1449(3) 0.4502(3) 0.8443(3) 0.0471(11) Uani 1 1 d . . . C2 C 1.1509(4) 0.4183(3) 0.7702(3) 0.0701(14) Uani 1 1 d . . . H2 H 1.0956 0.4117 0.7188 0.084 Uiso 1 1 calc R . . C3 C 1.2289(4) 0.4598(3) 0.9186(3) 0.0731(14) Uani 1 1 d . . . H3 H 1.2261 0.4813 0.9692 0.088 Uiso 1 1 calc R . . C4 C 1.2389(5) 0.3961(4) 0.7720(4) 0.097(2) Uani 1 1 d . . . H4 H 1.2420 0.3736 0.7218 0.117 Uiso 1 1 calc R . . C5 C 1.3177(4) 0.4384(4) 0.9206(4) 0.0915(18) Uani 1 1 d . . . H5 H 1.3739 0.4455 0.9718 0.110 Uiso 1 1 calc R . . C6 C 1.3212(5) 0.4070(4) 0.8471(5) 0.105(2) Uani 1 1 d . . . H6 H 1.3808 0.3926 0.8476 0.126 Uiso 1 1 calc R . . C7 C 1.1662(3) 0.9637(3) 0.6675(2) 0.0436(10) Uani 1 1 d . . . C8 C 1.0566(3) 0.8952(3) 0.6669(2) 0.0428(10) Uani 1 1 d . . . C9 C 0.9669(3) 0.9231(3) 0.6367(2) 0.0449(10) Uani 1 1 d . . . C10 C 0.9820(4) 1.0044(3) 0.6106(2) 0.0522(11) Uani 1 1 d . . . H10 H 0.9201 1.0180 0.5905 0.063 Uiso 1 1 calc R . . C11 C 1.0910(4) 1.0655(3) 0.6148(3) 0.0530(11) Uani 1 1 d . . . C12 C 0.8533(4) 0.6498(3) 0.5153(3) 0.0763(15) Uani 1 1 d . . . H12A H 0.9293 0.7056 0.5316 0.092 Uiso 1 1 calc R . . H12B H 0.7936 0.6660 0.4846 0.092 Uiso 1 1 calc R . . C13 C 1.1821(4) 1.0445(3) 0.6425(2) 0.0507(11) Uani 1 1 d . . . H13 H 1.2547 1.0859 0.6440 0.061 Uiso 1 1 calc R . . C14 C 1.1082(4) -0.0212(3) 0.8754(3) 0.0545(12) Uani 1 1 d . . . C15 C 1.2033(4) -0.0354(3) 0.8826(3) 0.0685(14) Uani 1 1 d . . . H15 H 1.1956 -0.0972 0.8795 0.082 Uiso 1 1 calc R . . C16 C 1.1231(5) 0.0722(4) 0.8820(3) 0.0802(16) Uani 1 1 d . . . C17 C 1.3204(6) 0.1292(5) 0.8966(4) 0.118(3) Uani 1 1 d . . . H17 H 1.3911 0.1792 0.9022 0.142 Uiso 1 1 calc R . . C18 C 1.3095(4) 0.0394(5) 0.8943(3) 0.100(2) Uani 1 1 d . . . H18 H 1.3731 0.0286 0.9006 0.120 Uiso 1 1 calc R . . C19 C 1.2300(5) 0.1473(4) 0.8906(4) 0.114(3) Uani 1 1 d . . . H19 H 1.2389 0.2092 0.8923 0.137 Uiso 1 1 calc R . . C20 C 0.7581(3) 0.3749(3) 0.6588(3) 0.0440(10) Uani 1 1 d . . . C21 C 0.6833(4) 0.2930(3) 0.6732(3) 0.0521(11) Uani 1 1 d . . . C22 C 0.7158(4) 0.3949(3) 0.5839(3) 0.0663(13) Uani 1 1 d . . . H22 H 0.7652 0.4488 0.5733 0.080 Uiso 1 1 calc R . . C23 C 0.5672(4) 0.2361(3) 0.6142(4) 0.0734(15) Uani 1 1 d . . . H23 H 0.5161 0.1828 0.6244 0.088 Uiso 1 1 calc R . . C24 C 0.5294(5) 0.2599(4) 0.5408(4) 0.0925(19) Uani 1 1 d . . . H24 H 0.4522 0.2219 0.5014 0.111 Uiso 1 1 calc R . . C25 C 0.6024(5) 0.3375(4) 0.5246(3) 0.0877(17) Uani 1 1 d . . . H25 H 0.5762 0.3517 0.4741 0.105 Uiso 1 1 calc R . . C26 C 0.5959(3) 0.4908(3) 0.6963(2) 0.0425(10) Uani 1 1 d . . . C27 C 0.7199(3) 0.5516(3) 0.7470(2) 0.0402(10) Uani 1 1 d . . . C28 C 0.5767(4) 0.3916(3) 0.7870(3) 0.0481(11) Uani 1 1 d . . . C29 C 0.7620(3) 0.5250(3) 0.8209(2) 0.0415(10) Uani 1 1 d . . . C30 C 0.5272(3) 0.4128(3) 0.7155(3) 0.0468(11) Uani 1 1 d . . . H30 H 0.4479 0.3747 0.6805 0.056 Uiso 1 1 calc R . . C31 C 0.6928(3) 0.4471(3) 0.8402(2) 0.0460(10) Uani 1 1 d . . . H31 H 0.7244 0.4321 0.8891 0.055 Uiso 1 1 calc R . . C32 C 0.5393(6) -0.1555(6) 0.7215(5) 0.133(3) Uani 1 1 d . . . H32 H 0.4873 -0.1747 0.6653 0.159 Uiso 1 1 calc R . . C33 C 0.6260(5) -0.1805(4) 0.7418(4) 0.0864(17) Uani 1 1 d . . . H33 H 0.6349 -0.2146 0.6998 0.104 Uiso 1 1 calc R . . C34 C 0.7005(4) -0.1550(3) 0.8248(3) 0.0551(12) Uani 1 1 d . . . C35 C 0.6858(4) -0.1049(3) 0.8849(3) 0.0677(13) Uani 1 1 d . . . H35 H 0.7350 -0.0883 0.9416 0.081 Uiso 1 1 calc R . . C36 C 0.5978(6) -0.0784(4) 0.8624(5) 0.103(2) Uani 1 1 d . . . H36 H 0.5883 -0.0434 0.9034 0.124 Uiso 1 1 calc R . . C37 C 0.5264(7) -0.1040(6) 0.7801(7) 0.142(5) Uani 1 1 d . . . H37 H 0.4679 -0.0858 0.7641 0.170 Uiso 1 1 calc R . . C38 C 1.2292(3) 0.7092(3) 0.8217(2) 0.0400(10) Uani 1 1 d . . . C39 C 1.2475(3) 0.6759(3) 0.7506(3) 0.0422(10) Uani 1 1 d . . . C40 C 1.3388(4) 0.6553(3) 0.7588(3) 0.0520(11) Uani 1 1 d . . . H40 H 1.3490 0.6350 0.7111 0.062 Uiso 1 1 calc R . . C41 C 1.4133(3) 0.6649(3) 0.8366(3) 0.0514(11) Uani 1 1 d . . . C42 C 1.3151(3) 0.7205(3) 0.8996(3) 0.0497(11) Uani 1 1 d . . . C43 C 1.4042(3) 0.6990(3) 0.9091(3) 0.0562(12) Uani 1 1 d . . . H43 H 1.4569 0.7070 0.9623 0.067 Uiso 1 1 calc R . . C44 C 0.8803(3) 0.4450(3) 0.7196(3) 0.0433(10) Uani 1 1 d . . . C46 C 1.0525(3) 0.4786(3) 0.8466(3) 0.0556(12) Uani 1 1 d . . . H46A H 1.0469 0.4775 0.9004 0.067 Uiso 1 1 calc R . . H46B H 1.0778 0.5445 0.8433 0.067 Uiso 1 1 calc R . . C48 C 0.9974(3) -0.1086(3) 0.8575(3) 0.0486(11) Uani 1 1 d . . . C50 C 0.7971(4) -0.1822(3) 0.8502(3) 0.0788(16) Uani 1 1 d . . . H50A H 0.8013 -0.2040 0.9003 0.095 Uiso 1 1 calc R . . H50B H 0.7800 -0.2352 0.8053 0.095 Uiso 1 1 calc R . . C67 C 0.7842(4) 0.1055(3) 0.6568(3) 0.0594(12) Uani 1 1 d . . . C68 C 0.8197(4) 0.0898(3) 0.7433(3) 0.0756(15) Uani 1 1 d . . . H68A H 0.7544 0.0342 0.7442 0.091 Uiso 1 1 calc R . . H68B H 0.8843 0.0752 0.7537 0.091 Uiso 1 1 calc R . . C69 C 0.8521(4) 0.1878(4) 0.6424(4) 0.0726(15) Uani 1 1 d . . . H69 H 0.9212 0.2349 0.6868 0.087 Uiso 1 1 calc R . . C70 C 0.8224(6) 0.2035(5) 0.5655(5) 0.097(2) Uani 1 1 d . . . H70 H 0.8705 0.2610 0.5582 0.117 Uiso 1 1 calc R . . C71 C 0.7226(8) 0.1357(6) 0.4988(5) 0.115(2) Uani 1 1 d . . . H71 H 0.7014 0.1467 0.4462 0.138 Uiso 1 1 calc R . . C72 C 0.6543(6) 0.0513(6) 0.5105(4) 0.114(2) Uani 1 1 d . . . H72 H 0.5867 0.0038 0.4653 0.137 Uiso 1 1 calc R . . C73 C 0.6848(5) 0.0358(4) 0.5893(4) 0.0890(17) Uani 1 1 d . . . H73 H 0.6377 -0.0221 0.5966 0.107 Uiso 1 1 calc R . . C74 C 0.7558(5) 0.1725(4) 0.8282(4) 0.099(2) Uani 1 1 d . . . H74A H 0.7856 0.2250 0.8782 0.118 Uiso 1 1 calc R . . H74B H 0.7170 0.1122 0.8404 0.118 Uiso 1 1 calc R . . C75 C 0.6679(4) 0.1811(3) 0.7579(4) 0.0825(17) Uani 1 1 d . . . H75A H 0.6389 0.1310 0.7064 0.099 Uiso 1 1 calc R . . H75B H 0.6022 0.1747 0.7711 0.099 Uiso 1 1 calc R . . C76 C 0.8446(4) 0.5666(4) 0.4592(3) 0.105(2) Uani 1 1 d . . . H76A H 0.8963 0.5448 0.4913 0.158 Uiso 1 1 calc R . . H76B H 0.8665 0.5864 0.4148 0.158 Uiso 1 1 calc R . . H76C H 0.7654 0.5148 0.4352 0.158 Uiso 1 1 calc R . . C77 C 0.9422(7) 0.1829(4) 0.8936(4) 0.132(3) Uani 1 1 d . . . H77A H 0.9646 0.2419 0.9345 0.158 Uiso 1 1 calc R . . H77B H 0.9042 0.1289 0.9135 0.158 Uiso 1 1 calc R . . C78 C 1.0460(6) 0.1841(4) 0.8920(4) 0.137(3) Uani 1 1 d . . . H78A H 1.1122 0.2253 0.9452 0.164 Uiso 1 1 calc R . . H78B H 1.0620 0.2099 0.8471 0.164 Uiso 1 1 calc R . . Er1 Er 0.966324(16) 0.691347(13) 0.733535(13) 0.04212(7) Uani 1 1 d . . . N1 N 1.3032(4) 0.7555(4) 0.9761(3) 0.0715(12) Uani 1 1 d . . . N2 N 1.1701(3) 0.6629(2) 0.6662(2) 0.0535(9) Uani 1 1 d . . . N3 N 0.8493(3) 0.8618(3) 0.6308(3) 0.0648(11) Uani 1 1 d . . . N4 N 1.2678(3) 0.9465(3) 0.6952(2) 0.0613(10) Uani 1 1 d . . . N5 N 1.1090(4) 1.1526(3) 0.5877(3) 0.0767(12) Uani 1 1 d . . . N6 N 0.8843(3) 0.5812(3) 0.8823(2) 0.0541(10) Uani 1 1 d . . . N7 N 0.5054(4) 0.3083(3) 0.8082(3) 0.0675(11) Uani 1 1 d . . . N8 N 0.5373(3) 0.5142(3) 0.6223(3) 0.0678(11) Uani 1 1 d . . . N9 N 1.5093(4) 0.6408(3) 0.8456(3) 0.0726(13) Uani 1 1 d . . . N10 N 0.9371(3) 0.4162(2) 0.7792(2) 0.0507(9) Uani 1 1 d . . . H10A H 0.9028 0.3563 0.7777 0.061 Uiso 1 1 calc R . . N11 N 0.8555(4) 0.1748(3) 0.8118(3) 0.0734(12) Uani 1 1 d . . . N12 N 0.9105(3) -0.0991(2) 0.8677(2) 0.0653(11) Uani 1 1 d . . . H12 H 0.9208 -0.0417 0.8853 0.078 Uiso 1 1 calc R . . O1 O 1.0728(2) 0.65680(19) 0.65234(17) 0.0539(7) Uani 1 1 d . . . O2 O 1.1467(2) 0.72862(17) 0.81944(16) 0.0435(7) Uani 1 1 d . . . O3 O 1.0417(2) 0.82008(18) 0.68961(17) 0.0563(8) Uani 1 1 d . . . O4 O 0.7825(2) 0.62140(18) 0.72620(16) 0.0500(7) Uani 1 1 d . . . O5 O 0.8389(3) 0.6288(2) 0.5898(2) 0.0585(9) Uani 1 1 d . . . O6 O 0.9287(2) 0.52962(18) 0.71478(16) 0.0522(7) Uani 1 1 d . . . O7 O 0.9874(2) -0.19060(19) 0.83548(17) 0.0520(7) Uani 1 1 d . . . O9 O 0.9577(2) 0.64087(19) 0.86510(17) 0.0558(8) Uani 1 1 d . . . O10 O 1.3624(3) 1.0119(2) 0.7065(2) 0.0930(12) Uani 1 1 d . . . O11 O 1.2032(3) 0.6583(2) 0.6094(2) 0.0841(11) Uani 1 1 d . . . O12 O 1.2344(3) 0.6953(3) 0.9961(2) 0.1167(16) Uani 1 1 d . . . O13 O 1.3575(4) 0.8384(3) 1.0123(3) 0.1352(18) Uani 1 1 d . . . O14 O 1.2557(3) 0.8692(3) 0.7050(3) 0.1202(16) Uani 1 1 d . . . O15 O 0.7714(3) 0.8719(3) 0.5888(4) 0.159(2) Uani 1 1 d . . . O16 O 0.8329(3) 0.7998(3) 0.6665(3) 0.1033(13) Uani 1 1 d . . . O17 O 1.2055(3) 1.2049(3) 0.5919(3) 0.1248(16) Uani 1 1 d . . . O18 O 0.4076(3) 0.2527(2) 0.7565(2) 0.1016(13) Uani 1 1 d . . . O19 O 0.9105(3) 0.5658(3) 0.9511(2) 0.0996(13) Uani 1 1 d . . . O20 O 0.5942(3) 0.5684(3) 0.5914(2) 0.1022(13) Uani 1 1 d . . . O21 O 0.4326(3) 0.4773(3) 0.5934(2) 0.1227(16) Uani 1 1 d . . . O22 O 0.5462(3) 0.3000(3) 0.8780(3) 0.1176(15) Uani 1 1 d . . . O23 O 1.0257(4) 1.1658(3) 0.5573(3) 0.1224(16) Uani 1 1 d . . . O24 O 1.5776(3) 0.6552(3) 0.9169(3) 0.0998(13) Uani 1 1 d . . . O25 O 1.5122(3) 0.6067(3) 0.7813(3) 0.1023(14) Uani 1 1 d . . . O26 O 0.7267(2) 0.27552(19) 0.7478(2) 0.0592(8) Uani 1 1 d . . . O27 O 1.0298(3) 0.0864(2) 0.8780(2) 0.1012(13) Uani 1 1 d . . . H5A H 0.777(3) 0.610(2) 0.588(2) 0.031(12) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.043(3) 0.046(3) 0.057(3) 0.025(2) 0.022(2) 0.022(2) C2 0.065(3) 0.078(4) 0.069(4) 0.020(3) 0.032(3) 0.033(3) C3 0.064(3) 0.098(4) 0.072(4) 0.039(3) 0.028(3) 0.047(3) C4 0.098(5) 0.099(5) 0.122(6) 0.023(4) 0.068(5) 0.055(4) C5 0.066(4) 0.105(5) 0.120(5) 0.059(4) 0.030(4) 0.054(3) C6 0.088(5) 0.096(5) 0.171(8) 0.048(5) 0.069(6) 0.065(4) C7 0.044(2) 0.041(2) 0.051(3) 0.021(2) 0.020(2) 0.022(2) C8 0.047(3) 0.037(2) 0.041(3) 0.011(2) 0.021(2) 0.016(2) C9 0.043(3) 0.045(3) 0.050(3) 0.017(2) 0.022(2) 0.022(2) C10 0.053(3) 0.052(3) 0.056(3) 0.017(2) 0.019(2) 0.032(2) C11 0.068(3) 0.041(3) 0.058(3) 0.024(2) 0.026(3) 0.030(2) C12 0.073(3) 0.078(4) 0.059(3) 0.039(3) 0.016(3) 0.023(3) C13 0.051(3) 0.045(3) 0.053(3) 0.023(2) 0.024(2) 0.016(2) C14 0.042(3) 0.050(3) 0.050(3) 0.014(2) 0.012(2) 0.008(2) C15 0.043(3) 0.073(3) 0.063(3) 0.002(3) 0.024(3) 0.007(3) C16 0.067(4) 0.057(3) 0.070(4) 0.026(3) -0.002(3) 0.008(3) C17 0.071(4) 0.106(5) 0.072(4) 0.035(4) -0.001(4) -0.031(4) C18 0.046(3) 0.127(5) 0.070(4) 0.004(4) 0.023(3) -0.002(4) C19 0.082(4) 0.070(4) 0.098(5) 0.047(3) -0.015(4) -0.012(4) C20 0.046(3) 0.036(2) 0.050(3) 0.012(2) 0.015(2) 0.023(2) C21 0.050(3) 0.040(3) 0.071(3) 0.008(2) 0.025(3) 0.026(2) C22 0.074(3) 0.053(3) 0.053(3) 0.010(2) 0.005(3) 0.031(3) C23 0.052(3) 0.057(3) 0.100(4) 0.005(3) 0.028(3) 0.023(3) C24 0.057(4) 0.077(4) 0.095(5) -0.016(4) -0.004(4) 0.027(3) C25 0.094(4) 0.075(4) 0.066(4) 0.006(3) -0.005(4) 0.048(4) C26 0.043(2) 0.043(2) 0.048(3) 0.017(2) 0.017(2) 0.026(2) C27 0.040(2) 0.038(2) 0.047(3) 0.013(2) 0.019(2) 0.021(2) C28 0.044(3) 0.044(3) 0.064(3) 0.023(2) 0.031(3) 0.019(2) C29 0.037(2) 0.041(2) 0.046(3) 0.012(2) 0.021(2) 0.015(2) C30 0.034(2) 0.040(2) 0.060(3) 0.009(2) 0.019(2) 0.013(2) C31 0.047(3) 0.053(3) 0.045(3) 0.020(2) 0.025(2) 0.025(2) C32 0.061(5) 0.130(8) 0.139(8) 0.086(6) -0.002(5) 0.006(5) C33 0.077(4) 0.081(4) 0.076(4) 0.022(3) 0.035(4) 0.012(3) C34 0.051(3) 0.049(3) 0.080(4) 0.027(3) 0.037(3) 0.026(2) C35 0.069(3) 0.074(3) 0.074(4) 0.024(3) 0.035(3) 0.041(3) C36 0.098(5) 0.080(4) 0.192(8) 0.057(5) 0.100(6) 0.061(4) C37 0.062(5) 0.124(8) 0.269(15) 0.124(9) 0.064(7) 0.055(5) C38 0.038(2) 0.034(2) 0.042(3) 0.0105(19) 0.017(2) 0.0108(19) C39 0.045(3) 0.039(2) 0.043(3) 0.016(2) 0.019(2) 0.019(2) C40 0.056(3) 0.049(3) 0.065(3) 0.019(2) 0.034(3) 0.030(2) C41 0.043(3) 0.051(3) 0.074(3) 0.024(3) 0.030(3) 0.028(2) C42 0.044(3) 0.057(3) 0.046(3) 0.010(2) 0.019(2) 0.023(2) C43 0.043(3) 0.063(3) 0.058(3) 0.019(2) 0.011(2) 0.027(2) C44 0.052(3) 0.044(3) 0.048(3) 0.019(2) 0.025(2) 0.029(2) C46 0.048(3) 0.055(3) 0.051(3) 0.012(2) 0.011(2) 0.021(2) C48 0.040(2) 0.046(3) 0.052(3) 0.010(2) 0.015(2) 0.017(2) C50 0.061(3) 0.052(3) 0.143(5) 0.035(3) 0.057(3) 0.031(3) C67 0.063(3) 0.054(3) 0.065(3) 0.013(3) 0.024(3) 0.034(3) C68 0.093(4) 0.053(3) 0.076(4) 0.011(3) 0.020(3) 0.043(3) C69 0.074(4) 0.070(4) 0.085(4) 0.018(3) 0.041(3) 0.040(3) C70 0.141(6) 0.095(5) 0.107(5) 0.043(4) 0.088(5) 0.069(5) C71 0.165(8) 0.153(7) 0.085(5) 0.041(6) 0.066(6) 0.114(6) C72 0.105(5) 0.132(7) 0.074(5) -0.008(5) 0.011(4) 0.057(5) C73 0.074(4) 0.075(4) 0.091(5) 0.007(4) 0.028(4) 0.021(3) C74 0.173(6) 0.063(3) 0.120(5) 0.061(4) 0.102(5) 0.069(4) C75 0.091(4) 0.058(3) 0.137(5) 0.049(3) 0.081(4) 0.038(3) C76 0.114(5) 0.143(6) 0.051(3) 0.016(4) 0.032(4) 0.060(4) C77 0.216(8) 0.103(5) 0.097(5) 0.006(4) 0.043(6) 0.116(6) C78 0.158(7) 0.045(4) 0.131(6) 0.002(4) -0.017(5) 0.045(4) Er1 0.04048(11) 0.03829(11) 0.05176(13) 0.02032(9) 0.02117(9) 0.01881(9) N1 0.065(3) 0.092(4) 0.057(3) 0.013(3) 0.021(3) 0.043(3) N2 0.060(3) 0.056(2) 0.053(3) 0.017(2) 0.028(2) 0.031(2) N3 0.050(3) 0.055(3) 0.091(3) 0.026(2) 0.032(3) 0.024(2) N4 0.052(3) 0.060(3) 0.081(3) 0.032(2) 0.029(2) 0.030(2) N5 0.088(3) 0.062(3) 0.103(4) 0.051(3) 0.047(3) 0.043(3) N6 0.047(2) 0.064(3) 0.047(2) 0.019(2) 0.021(2) 0.020(2) N7 0.056(3) 0.063(3) 0.087(4) 0.034(3) 0.039(3) 0.020(2) N8 0.046(3) 0.076(3) 0.068(3) 0.027(2) 0.015(2) 0.022(2) N9 0.063(3) 0.066(3) 0.107(4) 0.033(3) 0.038(3) 0.041(2) N10 0.049(2) 0.039(2) 0.061(2) 0.0241(18) 0.016(2) 0.0208(18) N11 0.114(4) 0.059(3) 0.064(3) 0.019(2) 0.032(3) 0.059(3) N12 0.054(2) 0.034(2) 0.112(3) 0.016(2) 0.040(2) 0.0218(19) O1 0.0532(18) 0.0624(19) 0.0503(19) 0.0210(15) 0.0222(16) 0.0294(16) O2 0.0377(15) 0.0484(16) 0.0501(17) 0.0129(13) 0.0200(14) 0.0242(13) O3 0.0587(19) 0.0408(17) 0.076(2) 0.0315(16) 0.0338(17) 0.0213(15) O4 0.0428(16) 0.0447(16) 0.0607(19) 0.0264(15) 0.0206(15) 0.0169(14) O5 0.052(2) 0.063(2) 0.062(2) 0.0343(17) 0.0259(19) 0.0231(18) O6 0.0632(19) 0.0331(16) 0.0553(18) 0.0181(14) 0.0190(16) 0.0212(14) O7 0.0417(16) 0.0431(17) 0.069(2) 0.0083(15) 0.0238(15) 0.0197(14) O9 0.0412(17) 0.0544(18) 0.058(2) 0.0201(16) 0.0196(16) 0.0102(15) O10 0.045(2) 0.074(2) 0.154(4) 0.051(2) 0.038(2) 0.0213(18) O11 0.099(3) 0.129(3) 0.057(2) 0.032(2) 0.046(2) 0.071(2) O12 0.101(3) 0.145(4) 0.081(3) 0.004(3) 0.055(3) 0.033(3) O13 0.189(5) 0.088(3) 0.114(4) -0.013(3) 0.073(3) 0.055(3) O14 0.069(2) 0.082(3) 0.240(5) 0.099(3) 0.063(3) 0.049(2) O15 0.052(2) 0.140(4) 0.299(7) 0.136(4) 0.058(3) 0.050(3) O16 0.068(2) 0.113(3) 0.139(4) 0.070(3) 0.062(3) 0.029(2) O17 0.092(3) 0.085(3) 0.185(4) 0.097(3) 0.043(3) 0.026(2) O18 0.069(2) 0.067(2) 0.115(3) 0.024(2) 0.029(2) -0.007(2) O19 0.067(2) 0.132(3) 0.056(2) 0.047(2) 0.015(2) 0.011(2) O20 0.071(2) 0.100(3) 0.095(3) 0.062(2) 0.007(2) 0.017(2) O21 0.044(2) 0.189(4) 0.116(3) 0.085(3) 0.015(2) 0.042(3) O22 0.078(3) 0.126(3) 0.131(4) 0.092(3) 0.042(3) 0.019(2) O23 0.133(4) 0.128(3) 0.206(5) 0.122(3) 0.105(4) 0.105(3) O24 0.079(3) 0.124(3) 0.124(3) 0.049(3) 0.036(3) 0.073(3) O25 0.114(3) 0.110(3) 0.137(4) 0.033(3) 0.074(3) 0.085(3) O26 0.063(2) 0.0417(17) 0.082(2) 0.0285(17) 0.0411(19) 0.0222(15) O27 0.091(3) 0.0331(19) 0.132(3) 0.020(2) -0.003(3) 0.0258(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C3 1.369(6) . ? C1 C2 1.375(5) . ? C1 C46 1.516(5) . ? C2 C4 1.378(6) . ? C2 H2 0.9300 . ? C3 C5 1.380(6) . ? C3 H3 0.9300 . ? C4 C6 1.361(7) . ? C4 H4 0.9300 . ? C5 C6 1.346(7) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C13 1.353(5) . ? C7 C8 1.444(5) . ? C7 N4 1.465(5) . ? C8 O3 1.252(4) . ? C8 C9 1.436(5) . ? C9 C10 1.370(5) . ? C9 N3 1.462(5) . ? C10 C11 1.378(5) . ? C10 H10 0.9300 . ? C11 C13 1.372(5) . ? C11 N5 1.459(5) . ? C12 O5 1.435(5) . ? C12 C76 1.482(6) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 H13 0.9300 . ? C14 C15 1.380(5) . ? C14 C16 1.389(6) . ? C14 C48 1.478(5) . ? C15 C18 1.378(6) . ? C15 H15 0.9300 . ? C16 O27 1.368(6) . ? C16 C19 1.404(6) . ? C17 C19 1.356(8) . ? C17 C18 1.358(8) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 C22 1.379(5) . ? C20 C21 1.395(5) . ? C20 C44 1.489(5) . ? C21 O26 1.358(5) . ? C21 C23 1.397(6) . ? C22 C25 1.377(6) . ? C22 H22 0.9300 . ? C23 C24 1.376(7) . ? C23 H23 0.9300 . ? C24 C25 1.358(7) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 C30 1.368(5) . ? C26 C27 1.444(5) . ? C26 N8 1.461(5) . ? C27 O4 1.267(4) . ? C27 C29 1.420(5) . ? C28 C30 1.366(5) . ? C28 C31 1.368(5) . ? C28 N7 1.455(5) . ? C29 C31 1.369(5) . ? C29 N6 1.464(5) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C32 C37 1.336(10) . ? C32 C33 1.356(8) . ? C32 H32 0.9300 . ? C33 C34 1.370(6) . ? C33 H33 0.9300 . ? C34 C35 1.359(5) . ? C34 C50 1.504(5) . ? C35 C36 1.388(7) . ? C35 H35 0.9300 . ? C36 C37 1.348(9) . ? C36 H36 0.9300 . ? C37 H37 0.9300 . ? C38 O2 1.276(4) . ? C38 C42 1.417(5) . ? C38 C39 1.429(5) . ? C39 C40 1.386(5) . ? C39 N2 1.442(5) . ? C40 C41 1.357(5) . ? C40 H40 0.9300 . ? C41 C43 1.384(5) . ? C41 N9 1.478(5) . ? C42 C43 1.362(5) . ? C42 N1 1.471(5) . ? C43 H43 0.9300 . ? C44 O6 1.253(4) . ? C44 N10 1.330(5) . ? C46 N10 1.452(4) . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C48 O7 1.245(4) . ? C48 N12 1.322(4) . ? C50 N12 1.469(4) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C67 C69 1.362(6) . ? C67 C73 1.374(6) . ? C67 C68 1.515(6) . ? C68 N11 1.479(5) . ? C68 H68A 0.9700 . ? C68 H68B 0.9700 . ? C69 C70 1.356(7) . ? C69 H69 0.9300 . ? C70 C71 1.362(8) . ? C70 H70 0.9300 . ? C71 C72 1.364(8) . ? C71 H71 0.9300 . ? C72 C73 1.386(8) . ? C72 H72 0.9300 . ? C73 H73 0.9300 . ? C74 N11 1.472(6) . ? C74 C75 1.480(7) . ? C74 H74A 0.9700 . ? C74 H74B 0.9700 . ? C75 O26 1.439(5) . ? C75 H75A 0.9700 . ? C75 H75B 0.9700 . ? C76 H76A 0.9600 . ? C76 H76B 0.9600 . ? C76 H76C 0.9600 . ? C77 C78 1.424(7) . ? C77 N11 1.485(7) . ? C77 H77A 0.9700 . ? C77 H77B 0.9700 . ? C78 O27 1.445(6) . ? C78 H78A 0.9700 . ? C78 H78B 0.9700 . ? Er1 O2 2.215(2) . ? Er1 O3 2.224(3) . ? Er1 O4 2.250(2) . ? Er1 O7 2.279(3) 1_565 ? Er1 O5 2.346(3) . ? Er1 O6 2.348(3) . ? Er1 O1 2.501(3) . ? Er1 O9 2.542(3) . ? N1 O13 1.171(5) . ? N1 O12 1.214(5) . ? N2 O11 1.225(4) . ? N2 O1 1.236(4) . ? N3 O15 1.167(5) . ? N3 O16 1.205(5) . ? N4 O14 1.203(4) . ? N4 O10 1.216(4) . ? N5 O23 1.207(5) . ? N5 O17 1.210(4) . ? N6 O9 1.215(4) . ? N6 O19 1.222(4) . ? N7 O18 1.206(4) . ? N7 O22 1.213(5) . ? N8 O21 1.196(4) . ? N8 O20 1.212(4) . ? N9 O25 1.210(5) . ? N9 O24 1.218(5) . ? N10 H10A 0.8600 . ? N12 H12 0.8600 . ? O5 H5A 0.77(3) . ? O7 Er1 2.279(3) 1_545 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 C1 C2 118.0(4) . . ? C3 C1 C46 119.4(4) . . ? C2 C1 C46 122.6(4) . . ? C1 C2 C4 120.1(5) . . ? C1 C2 H2 119.9 . . ? C4 C2 H2 119.9 . . ? C1 C3 C5 122.1(5) . . ? C1 C3 H3 119.0 . . ? C5 C3 H3 119.0 . . ? C6 C4 C2 120.3(6) . . ? C6 C4 H4 119.9 . . ? C2 C4 H4 119.9 . . ? C6 C5 C3 118.7(6) . . ? C6 C5 H5 120.6 . . ? C3 C5 H5 120.6 . . ? C5 C6 C4 120.9(6) . . ? C5 C6 H6 119.6 . . ? C4 C6 H6 119.6 . . ? C13 C7 C8 123.9(4) . . ? C13 C7 N4 116.4(4) . . ? C8 C7 N4 119.8(4) . . ? O3 C8 C9 124.2(4) . . ? O3 C8 C7 123.9(4) . . ? C9 C8 C7 111.9(4) . . ? C10 C9 C8 124.5(4) . . ? C10 C9 N3 115.7(4) . . ? C8 C9 N3 119.7(4) . . ? C9 C10 C11 118.7(4) . . ? C9 C10 H10 120.7 . . ? C11 C10 H10 120.7 . . ? C13 C11 C10 121.0(4) . . ? C13 C11 N5 119.5(4) . . ? C10 C11 N5 119.5(4) . . ? O5 C12 C76 111.9(4) . . ? O5 C12 H12A 109.2 . . ? C76 C12 H12A 109.2 . . ? O5 C12 H12B 109.2 . . ? C76 C12 H12B 109.2 . . ? H12A C12 H12B 107.9 . . ? C7 C13 C11 120.0(4) . . ? C7 C13 H13 120.0 . . ? C11 C13 H13 120.0 . . ? C15 C14 C16 117.8(4) . . ? C15 C14 C48 116.4(4) . . ? C16 C14 C48 125.8(4) . . ? C18 C15 C14 121.8(5) . . ? C18 C15 H15 119.1 . . ? C14 C15 H15 119.1 . . ? O27 C16 C14 117.5(4) . . ? O27 C16 C19 122.4(6) . . ? C14 C16 C19 120.1(6) . . ? C19 C17 C18 121.2(6) . . ? C19 C17 H17 119.4 . . ? C18 C17 H17 119.4 . . ? C17 C18 C15 119.4(6) . . ? C17 C18 H18 120.3 . . ? C15 C18 H18 120.3 . . ? C17 C19 C16 119.6(6) . . ? C17 C19 H19 120.2 . . ? C16 C19 H19 120.2 . . ? C22 C20 C21 118.3(4) . . ? C22 C20 C44 116.8(4) . . ? C21 C20 C44 124.8(4) . . ? O26 C21 C20 117.1(4) . . ? O26 C21 C23 122.9(4) . . ? C20 C21 C23 119.9(5) . . ? C25 C22 C20 121.9(5) . . ? C25 C22 H22 119.1 . . ? C20 C22 H22 119.1 . . ? C24 C23 C21 119.3(5) . . ? C24 C23 H23 120.3 . . ? C21 C23 H23 120.3 . . ? C25 C24 C23 121.4(5) . . ? C25 C24 H24 119.3 . . ? C23 C24 H24 119.3 . . ? C24 C25 C22 119.2(5) . . ? C24 C25 H25 120.4 . . ? C22 C25 H25 120.4 . . ? C30 C26 C27 123.3(4) . . ? C30 C26 N8 116.8(4) . . ? C27 C26 N8 119.8(4) . . ? O4 C27 C29 124.7(4) . . ? O4 C27 C26 122.0(4) . . ? C29 C27 C26 113.2(3) . . ? C30 C28 C31 121.7(4) . . ? C30 C28 N7 119.9(4) . . ? C31 C28 N7 118.5(4) . . ? C31 C29 C27 123.3(4) . . ? C31 C29 N6 115.6(4) . . ? C27 C29 N6 121.1(3) . . ? C28 C30 C26 119.0(4) . . ? C28 C30 H30 120.5 . . ? C26 C30 H30 120.5 . . ? C28 C31 C29 119.5(4) . . ? C28 C31 H31 120.2 . . ? C29 C31 H31 120.2 . . ? C37 C32 C33 121.7(9) . . ? C37 C32 H32 119.1 . . ? C33 C32 H32 119.1 . . ? C32 C33 C34 119.3(6) . . ? C32 C33 H33 120.3 . . ? C34 C33 H33 120.3 . . ? C35 C34 C33 119.2(5) . . ? C35 C34 C50 119.7(5) . . ? C33 C34 C50 121.1(5) . . ? C34 C35 C36 120.4(5) . . ? C34 C35 H35 119.8 . . ? C36 C35 H35 119.8 . . ? C37 C36 C35 119.1(7) . . ? C37 C36 H36 120.5 . . ? C35 C36 H36 120.5 . . ? C32 C37 C36 120.3(9) . . ? C32 C37 H37 119.9 . . ? C36 C37 H37 119.9 . . ? O2 C38 C42 120.8(4) . . ? O2 C38 C39 126.4(4) . . ? C42 C38 C39 112.8(3) . . ? C40 C39 C38 122.6(4) . . ? C40 C39 N2 117.1(4) . . ? C38 C39 N2 120.3(4) . . ? C41 C40 C39 119.6(4) . . ? C41 C40 H40 120.2 . . ? C39 C40 H40 120.2 . . ? C40 C41 C43 121.8(4) . . ? C40 C41 N9 119.9(4) . . ? C43 C41 N9 118.2(4) . . ? C43 C42 C38 125.7(4) . . ? C43 C42 N1 118.1(4) . . ? C38 C42 N1 116.2(3) . . ? C42 C43 C41 117.4(4) . . ? C42 C43 H43 121.3 . . ? C41 C43 H43 121.3 . . ? O6 C44 N10 120.7(4) . . ? O6 C44 C20 120.5(4) . . ? N10 C44 C20 118.8(4) . . ? N10 C46 C1 114.0(3) . . ? N10 C46 H46A 108.7 . . ? C1 C46 H46A 108.7 . . ? N10 C46 H46B 108.7 . . ? C1 C46 H46B 108.7 . . ? H46A C46 H46B 107.6 . . ? O7 C48 N12 120.2(4) . . ? O7 C48 C14 120.0(4) . . ? N12 C48 C14 119.7(4) . . ? N12 C50 C34 110.8(4) . . ? N12 C50 H50A 109.5 . . ? C34 C50 H50A 109.5 . . ? N12 C50 H50B 109.5 . . ? C34 C50 H50B 109.5 . . ? H50A C50 H50B 108.1 . . ? C69 C67 C73 117.7(5) . . ? C69 C67 C68 121.1(5) . . ? C73 C67 C68 121.2(5) . . ? N11 C68 C67 112.8(4) . . ? N11 C68 H68A 109.0 . . ? C67 C68 H68A 109.0 . . ? N11 C68 H68B 109.0 . . ? C67 C68 H68B 109.0 . . ? H68A C68 H68B 107.8 . . ? C70 C69 C67 122.2(6) . . ? C70 C69 H69 118.9 . . ? C67 C69 H69 118.9 . . ? C69 C70 C71 120.4(6) . . ? C69 C70 H70 119.8 . . ? C71 C70 H70 119.8 . . ? C70 C71 C72 118.9(7) . . ? C70 C71 H71 120.6 . . ? C72 C71 H71 120.6 . . ? C71 C72 C73 120.5(7) . . ? C71 C72 H72 119.7 . . ? C73 C72 H72 119.7 . . ? C67 C73 C72 120.3(6) . . ? C67 C73 H73 119.9 . . ? C72 C73 H73 119.9 . . ? N11 C74 C75 114.5(4) . . ? N11 C74 H74A 108.6 . . ? C75 C74 H74A 108.6 . . ? N11 C74 H74B 108.6 . . ? C75 C74 H74B 108.6 . . ? H74A C74 H74B 107.6 . . ? O26 C75 C74 106.6(4) . . ? O26 C75 H75A 110.4 . . ? C74 C75 H75A 110.4 . . ? O26 C75 H75B 110.4 . . ? C74 C75 H75B 110.4 . . ? H75A C75 H75B 108.6 . . ? C12 C76 H76A 109.5 . . ? C12 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C12 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? C78 C77 N11 115.7(6) . . ? C78 C77 H77A 108.4 . . ? N11 C77 H77A 108.4 . . ? C78 C77 H77B 108.4 . . ? N11 C77 H77B 108.4 . . ? H77A C77 H77B 107.4 . . ? C77 C78 O27 108.9(5) . . ? C77 C78 H78A 109.9 . . ? O27 C78 H78A 109.9 . . ? C77 C78 H78B 109.9 . . ? O27 C78 H78B 109.9 . . ? H78A C78 H78B 108.3 . . ? O2 Er1 O3 88.80(9) . . ? O2 Er1 O4 139.93(9) . . ? O3 Er1 O4 124.56(9) . . ? O2 Er1 O7 84.13(9) . 1_565 ? O3 Er1 O7 79.61(10) . 1_565 ? O4 Er1 O7 81.46(9) . 1_565 ? O2 Er1 O5 141.07(10) . . ? O3 Er1 O5 80.10(10) . . ? O4 Er1 O5 73.00(10) . . ? O7 Er1 O5 129.25(10) 1_565 . ? O2 Er1 O6 85.41(9) . . ? O3 Er1 O6 142.33(9) . . ? O4 Er1 O6 79.88(9) . . ? O7 Er1 O6 136.38(10) 1_565 . ? O5 Er1 O6 81.36(10) . . ? O2 Er1 O1 69.14(9) . . ? O3 Er1 O1 72.99(9) . . ? O4 Er1 O1 136.49(9) . . ? O7 Er1 O1 141.59(9) 1_565 . ? O5 Er1 O1 71.92(10) . . ? O6 Er1 O1 70.17(9) . . ? O2 Er1 O9 72.21(8) . . ? O3 Er1 O9 142.49(9) . . ? O4 Er1 O9 67.75(9) . . ? O7 Er1 O9 66.78(9) 1_565 . ? O5 Er1 O9 134.27(10) . . ? O6 Er1 O9 69.68(9) . . ? O1 Er1 O9 125.38(9) . . ? O13 N1 O12 124.5(5) . . ? O13 N1 C42 119.0(5) . . ? O12 N1 C42 116.5(5) . . ? O11 N2 O1 121.3(4) . . ? O11 N2 C39 118.6(4) . . ? O1 N2 C39 120.1(4) . . ? O15 N3 O16 120.8(4) . . ? O15 N3 C9 118.9(4) . . ? O16 N3 C9 120.3(4) . . ? O14 N4 O10 122.1(4) . . ? O14 N4 C7 120.1(4) . . ? O10 N4 C7 117.8(4) . . ? O23 N5 O17 123.2(4) . . ? O23 N5 C11 118.5(4) . . ? O17 N5 C11 118.1(4) . . ? O9 N6 O19 121.0(4) . . ? O9 N6 C29 121.0(4) . . ? O19 N6 C29 118.0(4) . . ? O18 N7 O22 123.3(4) . . ? O18 N7 C28 118.3(4) . . ? O22 N7 C28 118.3(4) . . ? O21 N8 O20 121.9(4) . . ? O21 N8 C26 117.9(4) . . ? O20 N8 C26 120.2(4) . . ? O25 N9 O24 125.3(5) . . ? O25 N9 C41 117.1(5) . . ? O24 N9 C41 117.6(5) . . ? C44 N10 C46 124.8(3) . . ? C44 N10 H10A 117.6 . . ? C46 N10 H10A 117.6 . . ? C74 N11 C68 112.4(4) . . ? C74 N11 C77 106.0(4) . . ? C68 N11 C77 113.0(4) . . ? C48 N12 C50 123.1(3) . . ? C48 N12 H12 118.5 . . ? C50 N12 H12 118.5 . . ? N2 O1 Er1 138.6(3) . . ? C38 O2 Er1 140.4(2) . . ? C8 O3 Er1 161.3(3) . . ? C27 O4 Er1 137.4(2) . . ? C12 O5 Er1 132.8(3) . . ? C12 O5 H5A 117(3) . . ? Er1 O5 H5A 106(3) . . ? C44 O6 Er1 155.2(2) . . ? C48 O7 Er1 148.5(3) . 1_545 ? N6 O9 Er1 136.2(3) . . ? C21 O26 C75 119.8(4) . . ? C16 O27 C78 118.6(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C3 C1 C2 C4 0.6(7) . . . . ? C46 C1 C2 C4 178.1(4) . . . . ? C2 C1 C3 C5 0.0(7) . . . . ? C46 C1 C3 C5 -177.6(4) . . . . ? C1 C2 C4 C6 -1.0(9) . . . . ? C1 C3 C5 C6 -0.1(8) . . . . ? C3 C5 C6 C4 -0.3(9) . . . . ? C2 C4 C6 C5 0.8(10) . . . . ? C13 C7 C8 O3 179.5(4) . . . . ? N4 C7 C8 O3 0.5(6) . . . . ? C13 C7 C8 C9 0.0(6) . . . . ? N4 C7 C8 C9 -179.1(3) . . . . ? O3 C8 C9 C10 -179.0(4) . . . . ? C7 C8 C9 C10 0.6(6) . . . . ? O3 C8 C9 N3 -0.2(6) . . . . ? C7 C8 C9 N3 179.3(3) . . . . ? C8 C9 C10 C11 -1.4(6) . . . . ? N3 C9 C10 C11 179.8(4) . . . . ? C9 C10 C11 C13 1.7(6) . . . . ? C9 C10 C11 N5 -179.7(4) . . . . ? C8 C7 C13 C11 0.3(6) . . . . ? N4 C7 C13 C11 179.4(4) . . . . ? C10 C11 C13 C7 -1.1(6) . . . . ? N5 C11 C13 C7 -179.8(4) . . . . ? C16 C14 C15 C18 -1.3(7) . . . . ? C48 C14 C15 C18 176.2(4) . . . . ? C15 C14 C16 O27 -177.6(4) . . . . ? C48 C14 C16 O27 5.3(7) . . . . ? C15 C14 C16 C19 3.7(7) . . . . ? C48 C14 C16 C19 -173.4(5) . . . . ? C19 C17 C18 C15 2.5(10) . . . . ? C14 C15 C18 C17 -1.8(8) . . . . ? C18 C17 C19 C16 0.0(10) . . . . ? O27 C16 C19 C17 178.2(6) . . . . ? C14 C16 C19 C17 -3.1(9) . . . . ? C22 C20 C21 O26 -179.3(4) . . . . ? C44 C20 C21 O26 -1.4(6) . . . . ? C22 C20 C21 C23 -2.7(6) . . . . ? C44 C20 C21 C23 175.2(4) . . . . ? C21 C20 C22 C25 0.9(7) . . . . ? C44 C20 C22 C25 -177.1(4) . . . . ? O26 C21 C23 C24 178.7(4) . . . . ? C20 C21 C23 C24 2.3(6) . . . . ? C21 C23 C24 C25 -0.2(8) . . . . ? C23 C24 C25 C22 -1.6(8) . . . . ? C20 C22 C25 C24 1.2(7) . . . . ? C30 C26 C27 O4 177.4(4) . . . . ? N8 C26 C27 O4 -5.2(6) . . . . ? C30 C26 C27 C29 -2.9(5) . . . . ? N8 C26 C27 C29 174.5(3) . . . . ? O4 C27 C29 C31 -177.8(3) . . . . ? C26 C27 C29 C31 2.5(5) . . . . ? O4 C27 C29 N6 2.8(6) . . . . ? C26 C27 C29 N6 -176.9(3) . . . . ? C31 C28 C30 C26 0.8(6) . . . . ? N7 C28 C30 C26 -179.3(3) . . . . ? C27 C26 C30 C28 1.3(6) . . . . ? N8 C26 C30 C28 -176.1(4) . . . . ? C30 C28 C31 C29 -1.2(6) . . . . ? N7 C28 C31 C29 179.0(3) . . . . ? C27 C29 C31 C28 -0.6(6) . . . . ? N6 C29 C31 C28 178.8(3) . . . . ? C37 C32 C33 C34 2.0(11) . . . . ? C32 C33 C34 C35 -0.2(8) . . . . ? C32 C33 C34 C50 179.3(5) . . . . ? C33 C34 C35 C36 -1.2(7) . . . . ? C50 C34 C35 C36 179.3(4) . . . . ? C34 C35 C36 C37 0.8(9) . . . . ? C33 C32 C37 C36 -2.4(13) . . . . ? C35 C36 C37 C32 1.0(12) . . . . ? O2 C38 C39 C40 -179.1(4) . . . . ? C42 C38 C39 C40 1.3(5) . . . . ? O2 C38 C39 N2 1.4(6) . . . . ? C42 C38 C39 N2 -178.3(3) . . . . ? C38 C39 C40 C41 1.4(6) . . . . ? N2 C39 C40 C41 -179.1(4) . . . . ? C39 C40 C41 C43 -3.0(6) . . . . ? C39 C40 C41 N9 178.6(4) . . . . ? O2 C38 C42 C43 177.8(4) . . . . ? C39 C38 C42 C43 -2.6(6) . . . . ? O2 C38 C42 N1 -0.2(6) . . . . ? C39 C38 C42 N1 179.5(4) . . . . ? C38 C42 C43 C41 1.2(7) . . . . ? N1 C42 C43 C41 179.1(4) . . . . ? C40 C41 C43 C42 1.8(6) . . . . ? N9 C41 C43 C42 -179.8(4) . . . . ? C22 C20 C44 O6 20.1(5) . . . . ? C21 C20 C44 O6 -157.8(4) . . . . ? C22 C20 C44 N10 -160.0(4) . . . . ? C21 C20 C44 N10 22.1(6) . . . . ? C3 C1 C46 N10 -143.1(4) . . . . ? C2 C1 C46 N10 39.4(6) . . . . ? C15 C14 C48 O7 -12.4(6) . . . . ? C16 C14 C48 O7 164.8(4) . . . . ? C15 C14 C48 N12 165.5(4) . . . . ? C16 C14 C48 N12 -17.3(7) . . . . ? C35 C34 C50 N12 -79.2(5) . . . . ? C33 C34 C50 N12 101.3(5) . . . . ? C69 C67 C68 N11 47.7(6) . . . . ? C73 C67 C68 N11 -134.7(5) . . . . ? C73 C67 C69 C70 2.2(7) . . . . ? C68 C67 C69 C70 179.8(5) . . . . ? C67 C69 C70 C71 -0.7(9) . . . . ? C69 C70 C71 C72 -1.0(10) . . . . ? C70 C71 C72 C73 1.3(10) . . . . ? C69 C67 C73 C72 -1.9(8) . . . . ? C68 C67 C73 C72 -179.5(5) . . . . ? C71 C72 C73 C67 0.2(10) . . . . ? N11 C74 C75 O26 -63.9(5) . . . . ? N11 C77 C78 O27 -93.3(7) . . . . ? C43 C42 N1 O13 85.6(6) . . . . ? C38 C42 N1 O13 -96.3(5) . . . . ? C43 C42 N1 O12 -95.9(5) . . . . ? C38 C42 N1 O12 82.2(5) . . . . ? C40 C39 N2 O11 -17.7(5) . . . . ? C38 C39 N2 O11 161.9(3) . . . . ? C40 C39 N2 O1 162.4(3) . . . . ? C38 C39 N2 O1 -18.1(5) . . . . ? C10 C9 N3 O15 16.6(7) . . . . ? C8 C9 N3 O15 -162.2(5) . . . . ? C10 C9 N3 O16 -166.0(4) . . . . ? C8 C9 N3 O16 15.2(6) . . . . ? C13 C7 N4 O14 -167.7(4) . . . . ? C8 C7 N4 O14 11.5(6) . . . . ? C13 C7 N4 O10 11.3(6) . . . . ? C8 C7 N4 O10 -169.6(4) . . . . ? C13 C11 N5 O23 174.2(5) . . . . ? C10 C11 N5 O23 -4.5(7) . . . . ? C13 C11 N5 O17 -1.2(7) . . . . ? C10 C11 N5 O17 -179.9(4) . . . . ? C31 C29 N6 O9 167.2(4) . . . . ? C27 C29 N6 O9 -13.3(6) . . . . ? C31 C29 N6 O19 -12.2(6) . . . . ? C27 C29 N6 O19 167.3(4) . . . . ? C30 C28 N7 O18 9.3(6) . . . . ? C31 C28 N7 O18 -170.9(4) . . . . ? C30 C28 N7 O22 -168.4(5) . . . . ? C31 C28 N7 O22 11.4(6) . . . . ? C30 C26 N8 O21 14.4(6) . . . . ? C27 C26 N8 O21 -163.1(4) . . . . ? C30 C26 N8 O20 -164.7(4) . . . . ? C27 C26 N8 O20 17.7(6) . . . . ? C40 C41 N9 O25 -5.0(6) . . . . ? C43 C41 N9 O25 176.6(4) . . . . ? C40 C41 N9 O24 176.3(4) . . . . ? C43 C41 N9 O24 -2.2(6) . . . . ? O6 C44 N10 C46 5.0(6) . . . . ? C20 C44 N10 C46 -174.8(3) . . . . ? C1 C46 N10 C44 -117.1(4) . . . . ? C75 C74 N11 C68 -65.8(5) . . . . ? C75 C74 N11 C77 170.2(4) . . . . ? C67 C68 N11 C74 88.7(5) . . . . ? C67 C68 N11 C77 -151.3(5) . . . . ? C78 C77 N11 C74 178.6(5) . . . . ? C78 C77 N11 C68 55.1(7) . . . . ? O7 C48 N12 C50 -2.9(7) . . . . ? C14 C48 N12 C50 179.2(4) . . . . ? C34 C50 N12 C48 -151.6(4) . . . . ? O11 N2 O1 Er1 -164.4(3) . . . . ? C39 N2 O1 Er1 15.6(6) . . . . ? O2 Er1 O1 N2 0.1(4) . . . . ? O3 Er1 O1 N2 95.4(4) . . . . ? O4 Er1 O1 N2 -141.9(3) . . . . ? O7 Er1 O1 N2 49.0(4) 1_565 . . . ? O5 Er1 O1 N2 -179.7(4) . . . . ? O6 Er1 O1 N2 -92.6(4) . . . . ? O9 Er1 O1 N2 -47.7(4) . . . . ? C42 C38 O2 Er1 -155.9(3) . . . . ? C39 C38 O2 Er1 24.5(6) . . . . ? O3 Er1 O2 C38 -93.5(4) . . . . ? O4 Er1 O2 C38 117.6(4) . . . . ? O7 Er1 O2 C38 -173.2(4) 1_565 . . . ? O5 Er1 O2 C38 -20.9(5) . . . . ? O6 Er1 O2 C38 49.3(4) . . . . ? O1 Er1 O2 C38 -21.2(4) . . . . ? O9 Er1 O2 C38 119.4(4) . . . . ? C9 C8 O3 Er1 -20.3(11) . . . . ? C7 C8 O3 Er1 160.2(6) . . . . ? O2 Er1 O3 C8 -137.4(8) . . . . ? O4 Er1 O3 C8 18.8(9) . . . . ? O7 Er1 O3 C8 -53.2(8) 1_565 . . . ? O5 Er1 O3 C8 80.1(8) . . . . ? O6 Er1 O3 C8 141.7(8) . . . . ? O1 Er1 O3 C8 154.1(9) . . . . ? O9 Er1 O3 C8 -79.4(9) . . . . ? C29 C27 O4 Er1 36.5(6) . . . . ? C26 C27 O4 Er1 -143.9(3) . . . . ? O2 Er1 O4 C27 -37.1(4) . . . . ? O3 Er1 O4 C27 -178.4(3) . . . . ? O7 Er1 O4 C27 -107.3(4) 1_565 . . . ? O5 Er1 O4 C27 117.1(4) . . . . ? O6 Er1 O4 C27 33.1(4) . . . . ? O1 Er1 O4 C27 79.6(4) . . . . ? O9 Er1 O4 C27 -39.0(4) . . . . ? C76 C12 O5 Er1 113.8(4) . . . . ? O2 Er1 O5 C12 -46.7(4) . . . . ? O3 Er1 O5 C12 28.8(4) . . . . ? O4 Er1 O5 C12 159.8(4) . . . . ? O7 Er1 O5 C12 96.5(4) 1_565 . . . ? O6 Er1 O5 C12 -118.2(4) . . . . ? O1 Er1 O5 C12 -46.4(4) . . . . ? O9 Er1 O5 C12 -168.5(3) . . . . ? N10 C44 O6 Er1 -102.0(6) . . . . ? C20 C44 O6 Er1 77.9(7) . . . . ? O2 Er1 O6 C44 115.8(6) . . . . ? O3 Er1 O6 C44 -162.1(6) . . . . ? O4 Er1 O6 C44 -26.8(6) . . . . ? O7 Er1 O6 C44 39.3(7) 1_565 . . . ? O5 Er1 O6 C44 -100.9(6) . . . . ? O1 Er1 O6 C44 -174.7(7) . . . . ? O9 Er1 O6 C44 43.1(6) . . . . ? N12 C48 O7 Er1 109.3(5) . . . 1_545 ? C14 C48 O7 Er1 -72.8(6) . . . 1_545 ? O19 N6 O9 Er1 171.1(3) . . . . ? C29 N6 O9 Er1 -8.2(6) . . . . ? O2 Er1 O9 N6 -154.1(4) . . . . ? O3 Er1 O9 N6 142.9(3) . . . . ? O4 Er1 O9 N6 24.7(4) . . . . ? O7 Er1 O9 N6 114.7(4) 1_565 . . . ? O5 Er1 O9 N6 -8.2(4) . . . . ? O6 Er1 O9 N6 -62.4(4) . . . . ? O1 Er1 O9 N6 -107.4(4) . . . . ? C20 C21 O26 C75 -163.3(3) . . . . ? C23 C21 O26 C75 20.2(6) . . . . ? C74 C75 O26 C21 158.4(4) . . . . ? C14 C16 O27 C78 174.7(5) . . . . ? C19 C16 O27 C78 -6.6(8) . . . . ? C77 C78 O27 C16 -174.0(6) . . . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 25.93 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 0.874 _refine_diff_density_min -0.519 _refine_diff_density_rms 0.082 #===END