# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Yan Zhou' _publ_contact_author_email 'zhouxy 07@lzu.edu.cn' _publ_section_title ; Diverse lanthanide coordination polymers tuned by the flexility of ligands and the lanthanide contraction effect: syntheses, structures and luminescence ; _publ_author_name 'Yan Zhou' # Attachment '- 1-12.cif' data_compound1 _database_code_depnum_ccdc_archive 'CCDC 817219' #TrackingRef '- 1-12.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C96 H96 La2 N12 O33' _chemical_formula_weight 2223.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.9319(10) _cell_length_b 22.7781(19) _cell_length_c 21.1246(17) _cell_angle_alpha 90.00 _cell_angle_beta 104.303(4) _cell_angle_gamma 90.00 _cell_volume 5563.4(8) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 5188 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 20.09 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.327 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2460 _exptl_absorpt_coefficient_mu 0.845 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.816 _exptl_absorpt_correction_T_max 0.845 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29677 _diffrn_reflns_av_R_equivalents 0.0438 _diffrn_reflns_av_sigmaI/netI 0.1075 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 25.50 _reflns_number_total 17682 _reflns_number_gt 10410 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _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 ; Restraints to thermal parameters were applied on the disordered phenyl groups. The distance restrains were applied to the phenyl group (C65, C66, C67, C68, C69, C70). 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. Diffuse electron densities resulting from residual disorder solvent moleculeswere removed from the data set using the SQUEEZE routine of PLATON andrefined further using the data generated. ; # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.015 0.123 0.422 208.4 49.3 2 -0.015 0.623 0.578 208.2 49.4 3 0.445 0.199 0.951 178.2 44.2 4 0.555 0.699 0.048 178.2 44.4 _platon_squeeze_details ; ; _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^+0.0200P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.000(8) _refine_ls_number_reflns 17682 _refine_ls_number_parameters 1300 _refine_ls_number_restraints 391 _refine_ls_R_factor_all 0.0999 _refine_ls_R_factor_gt 0.0462 _refine_ls_wR_factor_ref 0.0767 _refine_ls_wR_factor_gt 0.0695 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _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 La1 La 0.92242(3) 1.056031(15) 0.950443(18) 0.06773(11) Uani 1 1 d . . . La2 La 0.61430(3) 0.443961(13) 0.531346(16) 0.06527(11) Uani 1 1 d . . . C1 C 0.4356(6) 1.3657(4) 1.0935(3) 0.088(2) Uani 1 1 d . . . H1 H 0.4485 1.3639 1.0519 0.106 Uiso 1 1 calc R . . C2 C 0.4286(7) 1.3142(3) 1.1289(4) 0.104(3) Uani 1 1 d . . . H2 H 0.4400 1.2780 1.1111 0.125 Uiso 1 1 calc R . . C3 C 0.4054(7) 1.3162(4) 1.1887(4) 0.100(3) Uani 1 1 d . . . H3 H 0.3997 1.2817 1.2114 0.119 Uiso 1 1 calc R . . C4 C 0.3907(6) 1.3696(4) 1.2151(4) 0.097(2) Uani 1 1 d . . . H4 H 0.3757 1.3717 1.2563 0.117 Uiso 1 1 calc R . . C5 C 0.3981(6) 1.4199(3) 1.1812(3) 0.081(2) Uani 1 1 d . . . H5 H 0.3860 1.4560 1.1989 0.097 Uiso 1 1 calc R . . C6 C 0.4231(6) 1.4177(3) 1.1212(3) 0.0721(19) Uani 1 1 d . . . C7 C 0.4321(6) 1.4751(3) 1.0865(3) 0.0753(19) Uani 1 1 d . . . H7A H 0.3813 1.5036 1.0993 0.090 Uiso 1 1 calc R . . H7B H 0.5106 1.4897 1.1012 0.090 Uiso 1 1 calc R . . C8 C 0.2994(6) 1.4872(3) 0.9774(3) 0.0653(17) Uani 1 1 d . . . C9 C 0.2742(6) 1.4726(2) 0.9053(3) 0.0663(17) Uani 1 1 d . . . C10 C 0.1606(7) 1.4716(3) 0.8733(4) 0.095(3) Uani 1 1 d . . . H10 H 0.1043 1.4818 0.8949 0.114 Uiso 1 1 calc R . . C11 C 0.1287(7) 1.4551(4) 0.8070(4) 0.114(3) Uani 1 1 d . . . H11 H 0.0512 1.4541 0.7844 0.137 Uiso 1 1 calc R . . C12 C 0.2138(8) 1.4403(4) 0.7761(4) 0.109(2) Uani 1 1 d . . . H12 H 0.1927 1.4293 0.7323 0.131 Uiso 1 1 calc R . . C13 C 0.3271(7) 1.4415(4) 0.8075(4) 0.090(2) Uani 1 1 d . . . H13 H 0.3829 1.4307 0.7858 0.109 Uiso 1 1 calc R . . C14 C 0.3600(7) 1.4590(2) 0.8729(3) 0.0671(18) Uani 1 1 d . . . C15 C 0.5575(6) 1.4437(4) 0.8766(3) 0.0884(19) Uani 1 1 d . . . H15A H 0.5583 1.4692 0.8400 0.106 Uiso 1 1 calc R . . H15B H 0.5435 1.4038 0.8605 0.106 Uiso 1 1 calc R . . C16 C 0.6681(6) 1.4472(4) 0.9257(3) 0.094(2) Uani 1 1 d . . . H16A H 0.7309 1.4374 0.9061 0.113 Uiso 1 1 calc R . . H16B H 0.6802 1.4869 0.9427 0.113 Uiso 1 1 calc R . . C17 C 0.7736(6) 1.4077(3) 1.0252(3) 0.085(2) Uani 1 1 d . . . H17A H 0.7877 1.4461 1.0454 0.102 Uiso 1 1 calc R . . H17B H 0.8364 1.3988 1.0051 0.102 Uiso 1 1 calc R . . C18 C 0.7696(6) 1.3632(3) 1.0754(3) 0.084(2) Uani 1 1 d . . . H18A H 0.8341 1.3688 1.1132 0.101 Uiso 1 1 calc R . . H18B H 0.6984 1.3672 1.0894 0.101 Uiso 1 1 calc R . . C19 C 0.7864(6) 1.2575(3) 1.0861(3) 0.0745(19) Uani 1 1 d . . . C20 C 0.7790(6) 1.2592(4) 1.1527(4) 0.097(2) Uani 1 1 d . . . H20 H 0.7626 1.2945 1.1706 0.116 Uiso 1 1 calc R . . C21 C 0.7961(7) 1.2087(5) 1.1910(4) 0.110(3) Uani 1 1 d . . . H21 H 0.7962 1.2106 1.2350 0.132 Uiso 1 1 calc R . . C22 C 0.8123(8) 1.1582(5) 1.1640(6) 0.127(3) Uani 1 1 d . . . H22 H 0.8225 1.1240 1.1888 0.152 Uiso 1 1 calc R . . C23 C 0.8139(7) 1.1563(3) 1.0984(5) 0.099(2) Uani 1 1 d . . . H23 H 0.8228 1.1199 1.0803 0.118 Uiso 1 1 calc R . . C24 C 0.8031(6) 1.2052(4) 1.0581(4) 0.0778(19) Uani 1 1 d . . . C25 C 0.8109(6) 1.1945(4) 0.9925(4) 0.0757(19) Uani 1 1 d . . . C26 C 0.8148(9) 1.2334(4) 0.8851(4) 0.157(5) Uani 1 1 d . . . H26A H 0.8970 1.2349 0.8874 0.189 Uiso 1 1 calc R A 1 H26B H 0.7857 1.1958 0.8665 0.189 Uiso 1 1 calc R A 1 C27 C 0.7616(7) 1.2761(4) 0.8466(3) 0.142(6) Uani 0.50 1 d PGU B 1 C28 C 0.6521(7) 1.2606(3) 0.8099(3) 0.166(6) Uani 0.50 1 d PGU B 1 H28 H 0.6222 1.2237 0.8149 0.199 Uiso 0.50 1 calc PR B 1 C29 C 0.5873(6) 1.3004(3) 0.7657(3) 0.166(6) Uani 0.50 1 d PGU B 1 H29 H 0.5140 1.2900 0.7411 0.199 Uiso 0.50 1 calc PR B 1 C30 C 0.6319(9) 1.3556(3) 0.7582(3) 0.166(6) Uani 0.50 1 d PGU B 1 H30 H 0.5885 1.3822 0.7286 0.199 Uiso 0.50 1 calc PR B 1 C31 C 0.7414(10) 1.3711(3) 0.7949(5) 0.156(6) Uani 0.50 1 d PGU B 1 H31 H 0.7713 1.4080 0.7899 0.188 Uiso 0.50 1 calc PR B 1 C32 C 0.8063(7) 1.3313(5) 0.8391(4) 0.166(6) Uani 0.50 1 d PGU B 1 H32 H 0.8795 1.3417 0.8636 0.199 Uiso 0.50 1 calc PR B 1 C27' C 0.7200(7) 1.2612(3) 0.8340(3) 0.091(4) Uani 0.50 1 d PGU B 2 C28' C 0.6213(9) 1.2274(3) 0.8113(4) 0.110(4) Uani 0.50 1 d PGU B 2 H28' H 0.6178 1.1895 0.8271 0.132 Uiso 0.50 1 calc PR B 2 C29' C 0.5277(8) 1.2502(4) 0.7651(5) 0.119(4) Uani 0.50 1 d PGU B 2 H29' H 0.4616 1.2276 0.7499 0.143 Uiso 0.50 1 calc PR B 2 C30' C 0.5328(7) 1.3069(5) 0.7416(3) 0.112(4) Uani 0.50 1 d PGU B 2 H30' H 0.4702 1.3222 0.7107 0.134 Uiso 0.50 1 calc PR B 2 C31' C 0.6315(8) 1.3407(3) 0.7643(3) 0.112(4) Uani 0.50 1 d PGU B 2 H31' H 0.6350 1.3787 0.7485 0.135 Uiso 0.50 1 calc PR B 2 C32' C 0.7251(6) 1.3179(3) 0.8105(3) 0.107(4) Uani 0.50 1 d PGU B 2 H32' H 0.7912 1.3405 0.8257 0.128 Uiso 0.50 1 calc PR B 2 C33 C 1.0615(8) 0.8874(4) 0.7187(3) 0.097(2) Uani 1 1 d . . . H33 H 0.9999 0.8666 0.6930 0.116 Uiso 1 1 calc R . . C34 C 1.1741(9) 0.8764(5) 0.7122(4) 0.122(3) Uani 1 1 d . . . H34 H 1.1874 0.8468 0.6846 0.146 Uiso 1 1 calc R . . C35 C 1.2611(10) 0.9087(5) 0.7458(5) 0.121(3) Uani 1 1 d . . . H35 H 1.3348 0.9014 0.7403 0.145 Uiso 1 1 calc R . . C36 C 1.2493(9) 0.9496(5) 0.7853(5) 0.116(3) Uani 1 1 d . . . H36 H 1.3130 0.9714 0.8071 0.139 Uiso 1 1 calc R . . C37 C 1.1368(9) 0.9612(3) 0.7955(3) 0.094(2) Uani 1 1 d . . . H37 H 1.1281 0.9907 0.8244 0.113 Uiso 1 1 calc R . . C38 C 1.0401(7) 0.9290(3) 0.7629(3) 0.073(2) Uani 1 1 d . . . C39 C 0.9208(6) 0.9358(3) 0.7748(3) 0.078(2) Uani 1 1 d . . . H39A H 0.9113 0.9753 0.7899 0.094 Uiso 1 1 calc R . . H39B H 0.8622 0.9292 0.7345 0.094 Uiso 1 1 calc R . . C40 C 0.9086(5) 0.9071(3) 0.8852(3) 0.0532(15) Uani 1 1 d . . . C41 C 0.9020(5) 0.8585(3) 0.9327(3) 0.0538(16) Uani 1 1 d . . . C42 C 0.8942(6) 0.8735(3) 0.9935(3) 0.0724(19) Uani 1 1 d . . . H42 H 0.8946 0.9133 1.0034 0.087 Uiso 1 1 calc R . . C43 C 0.8860(6) 0.8353(3) 1.0410(3) 0.090(2) Uani 1 1 d . . . H43 H 0.8829 0.8478 1.0824 0.108 Uiso 1 1 calc R . . C44 C 0.8825(7) 0.7761(4) 1.0241(4) 0.093(2) Uani 1 1 d . . . H44 H 0.8767 0.7484 1.0554 0.111 Uiso 1 1 calc R . . C45 C 0.8871(6) 0.7575(3) 0.9644(4) 0.076(2) Uani 1 1 d . . . H45 H 0.8842 0.7175 0.9552 0.091 Uiso 1 1 calc R . . C46 C 0.8963(5) 0.7979(3) 0.9164(3) 0.0614(16) Uani 1 1 d . . . C47 C 0.8873(6) 0.7216(3) 0.8357(3) 0.088(2) Uani 1 1 d . . . H47A H 0.8136 0.7074 0.8412 0.106 Uiso 1 1 calc R . . H47B H 0.9484 0.6971 0.8613 0.106 Uiso 1 1 calc R . . C48 C 0.8892(7) 0.7201(3) 0.7660(3) 0.090(2) Uani 1 1 d . . . H48A H 0.9530 0.7436 0.7591 0.108 Uiso 1 1 calc R . . H48B H 0.8995 0.6801 0.7528 0.108 Uiso 1 1 calc R . . C49 C 0.7885(7) 0.7704(3) 0.6710(4) 0.098(2) Uani 1 1 d . . . H49A H 0.8365 0.7474 0.6493 0.118 Uiso 1 1 calc R . . H49B H 0.8236 0.8088 0.6807 0.118 Uiso 1 1 calc R . . C50 C 0.6724(7) 0.7766(2) 0.6279(3) 0.085(2) Uani 1 1 d . . . H50A H 0.6227 0.7964 0.6512 0.102 Uiso 1 1 calc R . . H50B H 0.6763 0.8006 0.5906 0.102 Uiso 1 1 calc R . . C51 C 0.5961(5) 0.7072(3) 0.5424(3) 0.0536(16) Uani 1 1 d . . . C52 C 0.5664(6) 0.7482(3) 0.4928(3) 0.0703(18) Uani 1 1 d . . . H52 H 0.5683 0.7880 0.5032 0.084 Uiso 1 1 calc R . . C53 C 0.5341(7) 0.7314(3) 0.4282(3) 0.091(2) Uani 1 1 d . . . H53 H 0.5145 0.7595 0.3953 0.109 Uiso 1 1 calc R . . C54 C 0.5311(8) 0.6724(3) 0.4129(3) 0.104(3) Uani 1 1 d . . . H54 H 0.5094 0.6604 0.3695 0.124 Uiso 1 1 calc R . . C55 C 0.5608(7) 0.6306(3) 0.4631(3) 0.088(2) Uani 1 1 d . . . H55 H 0.5590 0.5909 0.4526 0.105 Uiso 1 1 calc R . . C56 C 0.5921(6) 0.6473(3) 0.5265(3) 0.066(2) Uani 1 1 d . . . C57 C 0.6180(6) 0.6001(3) 0.5755(3) 0.0643(18) Uani 1 1 d . . . C58 C 0.6560(7) 0.5670(3) 0.6896(3) 0.092(2) Uani 1 1 d . . . H58A H 0.7383 0.5650 0.7098 0.110 Uiso 1 1 calc R . . H58B H 0.6312 0.5286 0.6715 0.110 Uiso 1 1 calc R . . C59 C 0.5922(8) 0.5824(3) 0.7405(3) 0.073(2) Uani 1 1 d . . . C60 C 0.4816(8) 0.5651(4) 0.7340(4) 0.088(2) Uani 1 1 d . . . H60 H 0.4455 0.5422 0.6984 0.106 Uiso 1 1 calc R . . C61 C 0.4236(7) 0.5802(3) 0.7778(5) 0.093(2) Uani 1 1 d . . . H61 H 0.3472 0.5682 0.7715 0.112 Uiso 1 1 calc R . . C62 C 0.4713(9) 0.6118(4) 0.8298(5) 0.109(3) Uani 1 1 d . . . H62 H 0.4268 0.6254 0.8573 0.131 Uiso 1 1 calc R . . C63 C 0.5858(10) 0.6243(4) 0.8428(4) 0.122(3) Uani 1 1 d . . . H63 H 0.6238 0.6408 0.8826 0.147 Uiso 1 1 calc R . . C64 C 0.6457(8) 0.6118(3) 0.7952(4) 0.104(3) Uani 1 1 d . . . H64 H 0.7221 0.6237 0.8011 0.124 Uiso 1 1 calc R . . C65 C 0.9519(9) 0.2536(4) 0.7333(4) 0.150(3) Uani 1 1 d DU . . H65 H 0.8931 0.2391 0.7508 0.179 Uiso 1 1 calc R . . C66 C 1.0724(11) 0.2442(5) 0.7698(5) 0.175(4) Uani 1 1 d DU . . H66 H 1.0940 0.2237 0.8090 0.209 Uiso 1 1 calc R . . C67 C 1.1504(11) 0.2695(5) 0.7385(6) 0.180(4) Uani 1 1 d DU . . H67 H 1.2291 0.2678 0.7582 0.216 Uiso 1 1 calc R . . C68 C 1.1137(12) 0.2970(5) 0.6793(6) 0.190(4) Uani 1 1 d DU . . H68 H 1.1710 0.3124 0.6613 0.227 Uiso 1 1 calc R . . C69 C 0.9990(11) 0.3043(5) 0.6426(5) 0.171(4) Uani 1 1 d DU . . H69 H 0.9779 0.3218 0.6015 0.205 Uiso 1 1 calc R . . C70 C 0.9221(11) 0.2823(4) 0.6755(4) 0.127(3) Uani 1 1 d DU . . C71 C 0.7935(9) 0.2893(4) 0.6403(4) 0.158(4) Uani 1 1 d . . . H71A H 0.7461 0.2705 0.6657 0.190 Uiso 1 1 calc R . . H71B H 0.7736 0.3307 0.6365 0.190 Uiso 1 1 calc R . . C72 C 0.7226(6) 0.2918(3) 0.5256(3) 0.0700(18) Uani 1 1 d . . . C73 C 0.6914(5) 0.2617(3) 0.4584(3) 0.0625(16) Uani 1 1 d . . . C74 C 0.6580(5) 0.2952(3) 0.4041(3) 0.0716(18) Uani 1 1 d . . . H74 H 0.6549 0.3358 0.4078 0.086 Uiso 1 1 calc R . . C75 C 0.6288(6) 0.2692(4) 0.3435(3) 0.085(2) Uani 1 1 d . . . H75 H 0.6051 0.2928 0.3067 0.102 Uiso 1 1 calc R . . C76 C 0.6335(6) 0.2095(3) 0.3359(4) 0.083(2) Uani 1 1 d . . . H76 H 0.6139 0.1925 0.2946 0.100 Uiso 1 1 calc R . . C77 C 0.6677(6) 0.1755(3) 0.3904(4) 0.086(2) Uani 1 1 d . . . H77 H 0.6715 0.1351 0.3855 0.103 Uiso 1 1 calc R . . C78 C 0.6972(5) 0.1992(3) 0.4532(3) 0.0675(17) Uani 1 1 d . . . C79 C 0.7354(7) 0.1045(3) 0.5052(4) 0.099(3) Uani 1 1 d . . . H79A H 0.7910 0.0918 0.4814 0.119 Uiso 1 1 calc R . . H79B H 0.6599 0.0892 0.4834 0.119 Uiso 1 1 calc R . . C80 C 0.7692(7) 0.0840(3) 0.5723(5) 0.111(3) Uani 1 1 d . . . H80A H 0.7181 0.1006 0.5969 0.133 Uiso 1 1 calc R . . H80B H 0.7628 0.0416 0.5734 0.133 Uiso 1 1 calc R . . C81 C 0.9167(8) 0.0851(4) 0.6678(4) 0.124(3) Uani 1 1 d . . . H81A H 0.9049 0.0434 0.6726 0.149 Uiso 1 1 calc R . . H81B H 0.8695 0.1061 0.6917 0.149 Uiso 1 1 calc R . . C82 C 1.0431(9) 0.1001(4) 0.6958(4) 0.120(3) Uani 1 1 d . . . H82A H 1.0574 0.1410 0.6875 0.144 Uiso 1 1 calc R . . H82B H 1.0646 0.0935 0.7426 0.144 Uiso 1 1 calc R . . C83 C 1.2271(7) 0.0638(4) 0.6815(4) 0.083(2) Uani 1 1 d . . . C84 C 1.2877(10) 0.0963(4) 0.7354(4) 0.108(3) Uani 1 1 d . . . H84 H 1.2475 0.1194 0.7587 0.130 Uiso 1 1 calc R . . C85 C 1.4004(13) 0.0943(5) 0.7530(5) 0.138(4) Uani 1 1 d . . . H85 H 1.4409 0.1155 0.7890 0.166 Uiso 1 1 calc R . . C86 C 1.4578(8) 0.0608(6) 0.7180(5) 0.132(4) Uani 1 1 d . . . H86 H 1.5382 0.0597 0.7298 0.158 Uiso 1 1 calc R . . C87 C 1.3987(9) 0.0287(4) 0.6658(5) 0.105(3) Uani 1 1 d . . . H87 H 1.4395 0.0051 0.6433 0.126 Uiso 1 1 calc R . . C88 C 1.2835(8) 0.0306(3) 0.6465(3) 0.0713(19) Uani 1 1 d . . . C89 C 1.2285(8) -0.0035(3) 0.5865(4) 0.088(2) Uani 1 1 d . . . C90 C 1.0373(9) -0.0244(4) 0.5033(4) 0.146(4) Uani 1 1 d . . . H90A H 0.9827 0.0065 0.4853 0.175 Uiso 1 1 calc R . . H90B H 1.0836 -0.0322 0.4724 0.175 Uiso 1 1 calc R . . C91 C 0.9718(6) -0.0791(2) 0.5118(3) 0.120(3) Uani 1 1 d GU . . C92 C 1.0410(4) -0.1267(3) 0.5376(3) 0.147(3) Uani 1 1 d GU . . H92 H 1.1206 -0.1221 0.5523 0.177 Uiso 1 1 calc R . . C93 C 0.9911(6) -0.1814(3) 0.5414(3) 0.145(3) Uani 1 1 d GU . . H93 H 1.0374 -0.2132 0.5586 0.174 Uiso 1 1 calc R . . C94 C 0.8721(6) -0.1884(2) 0.5195(3) 0.133(3) Uani 1 1 d GU . . H94 H 0.8387 -0.2249 0.5220 0.160 Uiso 1 1 calc R . . C95 C 0.8029(4) -0.1407(3) 0.4937(3) 0.157(3) Uani 1 1 d GU . . H95 H 0.7233 -0.1454 0.4790 0.189 Uiso 1 1 calc R . . C96 C 0.8528(5) -0.0861(2) 0.4899(3) 0.149(3) Uani 1 1 d GU . . H96 H 0.8065 -0.0542 0.4726 0.179 Uiso 1 1 calc R . . N1 N 0.4020(5) 1.4713(2) 1.0138(2) 0.0730(15) Uani 1 1 d . . . H1A H 0.4530 1.4583 0.9949 0.088 Uiso 1 1 calc R . . N2 N 0.7973(6) 1.2381(3) 0.9517(3) 0.100(2) Uani 1 1 d . B . H2A H 0.7770 1.2716 0.9642 0.119 Uiso 1 1 calc R . . N3 N 0.9082(4) 0.8935(2) 0.8236(2) 0.0661(14) Uani 1 1 d . . . H3A H 0.8998 0.8572 0.8123 0.079 Uiso 1 1 calc R . . N4 N 0.6348(5) 0.6103(2) 0.6374(2) 0.0740(16) Uani 1 1 d . . . H4A H 0.6332 0.6465 0.6488 0.089 Uiso 1 1 calc R . . N5 N 0.7706(5) 0.2635(3) 0.5768(3) 0.094(2) Uani 1 1 d . . . H5A H 0.7900 0.2276 0.5732 0.112 Uiso 1 1 calc R . . N6 N 1.1161(7) -0.0036(3) 0.5680(4) 0.137(3) Uani 1 1 d . . . H6 H 1.0813 0.0098 0.5961 0.164 Uiso 1 1 calc R . . N7 N 1.0763(7) 1.0398(5) 1.0863(4) 0.120(3) Uani 1 1 d . . . N8 N 1.1312(7) 1.1067(4) 0.9158(4) 0.113(2) Uani 1 1 d . . . N9 N 0.7844(6) 1.0836(3) 0.8123(4) 0.092(2) Uani 1 1 d . . . N10 N 0.8040(8) 0.4480(5) 0.6525(5) 0.134(4) Uani 1 1 d . . . N11 N 0.4371(7) 0.4180(4) 0.6108(3) 0.094(2) Uani 1 1 d . . . N12 N 0.4044(6) 0.4377(3) 0.4137(3) 0.0886(17) Uani 1 1 d . . . O1 O 0.2244(4) 1.5112(2) 1.0013(2) 0.0787(13) Uani 1 1 d . . . O2 O 0.4708(4) 1.46150(18) 0.90727(18) 0.0808(13) Uani 1 1 d . . . O3 O 0.6666(4) 1.40798(19) 0.9768(2) 0.0803(13) Uani 1 1 d . . . O4 O 0.7755(4) 1.3064(2) 1.0483(2) 0.0813(13) Uani 1 1 d . . . O5 O 0.8309(4) 1.1447(2) 0.9737(2) 0.0956(16) Uani 1 1 d . . . O6 O 0.9221(4) 0.95848(15) 0.90566(18) 0.0692(12) Uani 1 1 d . . . O7 O 0.9048(4) 0.78246(18) 0.8560(2) 0.0751(13) Uani 1 1 d . . . O8 O 0.7824(4) 0.7430(2) 0.7285(2) 0.0979(15) Uani 1 1 d . . . O9 O 0.6253(5) 0.72214(17) 0.6063(2) 0.0946(17) Uani 1 1 d . . . O10 O 0.6246(4) 0.54767(19) 0.55697(18) 0.0884(13) Uani 1 1 d . . . O11 O 0.6947(4) 0.34526(18) 0.5263(2) 0.0831(14) Uani 1 1 d . . . O12 O 0.7324(4) 0.16788(18) 0.5085(2) 0.0848(14) Uani 1 1 d . . . O13 O 0.8828(5) 0.1008(2) 0.6007(3) 0.0951(15) Uani 1 1 d . . . O14 O 1.1086(5) 0.0625(3) 0.6638(2) 0.0972(14) Uani 1 1 d . . . O15 O 1.2829(5) -0.0270(2) 0.5504(2) 0.1044(17) Uani 1 1 d . . . O16 O 1.0371(6) 1.0894(3) 1.0664(3) 0.123(2) Uani 1 1 d . . . O17 O 1.1324(6) 1.0299(3) 1.1405(3) 0.175(4) Uani 1 1 d . . . O18 O 1.0531(4) 0.9982(3) 1.0447(3) 0.0968(16) Uani 1 1 d . . . O19 O 1.1197(4) 1.0531(3) 0.9221(3) 0.1096(16) Uani 1 1 d . . . O20 O 1.2052(6) 1.1282(3) 0.8919(4) 0.170(3) Uani 1 1 d . . . O21 O 1.0609(5) 1.1385(2) 0.9364(3) 0.1173(19) Uani 1 1 d . . . O22 O 0.7381(4) 1.0653(2) 0.8549(2) 0.0862(15) Uani 1 1 d . . . O23 O 0.7304(5) 1.0996(3) 0.7588(3) 0.157(3) Uani 1 1 d . . . O24 O 0.8914(5) 1.0863(2) 0.8290(2) 0.1043(17) Uani 1 1 d . . . O25 O 0.7058(6) 0.4322(3) 0.6531(3) 0.104(2) Uani 1 1 d . . . O26 O 0.8795(6) 0.4521(4) 0.7030(4) 0.230(5) Uani 1 1 d . . . O27 O 0.8263(6) 0.4592(3) 0.5992(3) 0.139(3) Uani 1 1 d . . . O28 O 0.4854(5) 0.3785(2) 0.5854(2) 0.0969(16) Uani 1 1 d . . . O29 O 0.3781(6) 0.4085(3) 0.6469(3) 0.134(2) Uani 1 1 d . . . O30 O 0.4571(5) 0.4700(2) 0.5928(2) 0.0935(16) Uani 1 1 d . . . O31 O 0.4708(5) 0.3948(2) 0.4326(2) 0.1012(18) Uani 1 1 d . . . O32 O 0.3238(5) 0.4362(3) 0.3669(3) 0.135(2) Uani 1 1 d . . . O33 O 0.4344(4) 0.4851(2) 0.4468(2) 0.0934(16) 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 La1 0.0605(2) 0.0565(2) 0.0875(3) -0.0170(2) 0.0207(2) -0.0038(2) La2 0.0838(3) 0.04208(19) 0.0648(2) -0.0094(2) 0.0087(2) -0.0028(2) C1 0.112(6) 0.087(5) 0.062(4) 0.006(4) 0.012(4) 0.019(5) C2 0.131(7) 0.072(5) 0.096(6) -0.015(5) 0.002(6) 0.006(5) C3 0.098(6) 0.107(7) 0.084(6) 0.014(5) 0.005(5) -0.035(5) C4 0.089(6) 0.126(7) 0.076(5) 0.027(6) 0.018(4) 0.000(5) C5 0.086(5) 0.094(6) 0.058(4) 0.000(4) 0.009(4) 0.006(4) C6 0.065(5) 0.081(5) 0.059(5) 0.008(4) -0.007(4) 0.006(4) C7 0.072(5) 0.079(5) 0.069(5) -0.017(4) 0.005(4) 0.006(4) C8 0.061(5) 0.051(4) 0.080(5) 0.022(3) 0.010(4) -0.008(3) C9 0.066(5) 0.062(4) 0.060(5) 0.016(3) -0.005(4) -0.012(3) C10 0.067(6) 0.141(7) 0.072(5) 0.009(5) 0.007(5) -0.004(5) C11 0.068(6) 0.154(9) 0.104(7) 0.003(6) -0.009(5) -0.010(6) C12 0.111(7) 0.128(7) 0.077(5) 0.006(6) 0.000(6) -0.019(7) C13 0.089(6) 0.104(5) 0.078(5) 0.011(5) 0.020(5) 0.000(6) C14 0.077(5) 0.063(5) 0.063(5) 0.002(3) 0.020(4) 0.003(4) C15 0.087(5) 0.103(5) 0.081(5) 0.013(5) 0.031(4) 0.031(5) C16 0.085(5) 0.092(5) 0.115(6) 0.028(5) 0.043(5) 0.027(5) C17 0.087(6) 0.069(5) 0.089(5) -0.020(4) 0.003(5) 0.006(4) C18 0.081(5) 0.068(4) 0.091(5) -0.036(4) -0.001(4) 0.006(4) C19 0.064(5) 0.078(5) 0.078(5) -0.010(4) 0.010(4) 0.005(4) C20 0.087(6) 0.109(7) 0.104(6) -0.025(5) 0.041(5) 0.013(5) C21 0.106(7) 0.146(9) 0.084(6) 0.028(6) 0.033(5) -0.002(7) C22 0.122(8) 0.117(8) 0.159(10) 0.034(7) 0.067(7) 0.013(6) C23 0.093(6) 0.085(6) 0.126(7) -0.004(5) 0.042(6) -0.007(5) C24 0.057(4) 0.085(6) 0.092(6) -0.003(5) 0.018(4) 0.013(4) C25 0.063(5) 0.087(6) 0.071(5) -0.005(5) 0.006(4) 0.018(4) C26 0.196(11) 0.176(10) 0.087(7) -0.010(6) 0.009(7) 0.118(8) C27 0.201(13) 0.167(12) 0.095(10) 0.021(9) 0.106(9) 0.082(11) C28 0.216(14) 0.180(12) 0.128(11) 0.027(10) 0.095(10) 0.067(11) C29 0.213(14) 0.185(12) 0.121(11) 0.010(10) 0.084(10) 0.063(11) C30 0.218(14) 0.185(12) 0.118(11) 0.022(10) 0.088(10) 0.081(11) C31 0.215(14) 0.165(11) 0.119(11) 0.018(8) 0.096(9) 0.075(11) C32 0.208(14) 0.173(12) 0.136(11) -0.002(9) 0.079(10) 0.071(11) C27' 0.122(9) 0.090(8) 0.080(9) 0.017(6) 0.060(8) 0.028(7) C28' 0.143(10) 0.088(8) 0.095(9) 0.006(7) 0.023(8) 0.022(7) C29' 0.152(10) 0.114(8) 0.093(8) 0.011(7) 0.036(8) 0.031(8) C30' 0.161(10) 0.102(8) 0.079(8) 0.018(6) 0.041(8) 0.063(7) C31' 0.164(11) 0.105(8) 0.084(9) 0.020(7) 0.061(8) 0.046(7) C32' 0.146(10) 0.094(7) 0.097(8) 0.002(7) 0.064(7) 0.035(7) C33 0.104(7) 0.100(6) 0.091(6) -0.019(5) 0.033(5) -0.022(5) C34 0.105(8) 0.158(9) 0.114(8) -0.004(6) 0.049(7) 0.008(7) C35 0.104(8) 0.147(10) 0.103(9) 0.041(6) 0.012(7) -0.010(8) C36 0.092(7) 0.126(9) 0.114(8) 0.051(6) -0.005(6) -0.049(7) C37 0.139(7) 0.071(5) 0.056(5) 0.013(3) -0.008(5) -0.030(5) C38 0.098(6) 0.060(5) 0.051(4) 0.011(3) 0.002(4) -0.007(4) C39 0.102(6) 0.068(5) 0.064(4) 0.022(4) 0.020(4) 0.011(5) C40 0.049(4) 0.046(4) 0.064(4) 0.003(3) 0.012(3) 0.004(3) C41 0.049(4) 0.045(4) 0.063(4) -0.002(3) 0.006(3) 0.000(3) C42 0.070(5) 0.075(5) 0.075(5) 0.007(4) 0.023(4) 0.014(4) C43 0.115(6) 0.076(5) 0.086(5) -0.001(4) 0.039(5) 0.011(5) C44 0.118(7) 0.089(6) 0.074(5) 0.011(4) 0.030(5) -0.001(5) C45 0.075(5) 0.054(4) 0.091(6) 0.013(4) 0.008(4) 0.003(4) C46 0.053(4) 0.059(4) 0.068(5) 0.000(4) 0.008(4) 0.006(3) C47 0.110(6) 0.044(4) 0.091(5) -0.017(3) -0.010(5) 0.009(4) C48 0.112(7) 0.078(5) 0.072(5) -0.021(4) 0.009(5) 0.018(4) C49 0.100(6) 0.089(5) 0.095(6) -0.002(5) 0.002(5) -0.017(5) C50 0.132(6) 0.034(3) 0.074(5) -0.011(3) -0.007(5) -0.005(4) C51 0.067(4) 0.038(3) 0.053(4) -0.005(3) 0.009(3) -0.002(3) C52 0.080(5) 0.057(4) 0.075(5) -0.003(4) 0.021(4) -0.006(4) C53 0.133(7) 0.069(5) 0.063(5) -0.003(4) 0.011(5) -0.009(5) C54 0.161(8) 0.096(6) 0.049(5) -0.022(4) 0.019(5) -0.021(6) C55 0.146(7) 0.066(5) 0.057(5) -0.015(4) 0.038(5) -0.026(5) C56 0.085(5) 0.061(5) 0.061(5) -0.007(4) 0.040(4) -0.012(4) C57 0.094(5) 0.045(4) 0.061(5) -0.020(3) 0.032(4) -0.013(3) C58 0.154(7) 0.045(4) 0.079(4) 0.003(3) 0.034(5) -0.003(4) C59 0.124(7) 0.054(4) 0.045(4) 0.008(3) 0.028(5) -0.003(4) C60 0.097(6) 0.082(6) 0.085(6) 0.007(5) 0.021(5) 0.002(6) C61 0.095(6) 0.082(6) 0.101(7) 0.011(5) 0.022(6) -0.007(5) C62 0.114(8) 0.119(7) 0.100(7) -0.005(6) 0.037(6) 0.008(6) C63 0.148(9) 0.133(7) 0.082(6) -0.042(5) 0.023(7) -0.020(7) C64 0.139(8) 0.092(5) 0.089(6) -0.034(5) 0.047(6) -0.026(5) C65 0.202(8) 0.159(7) 0.075(6) -0.025(5) 0.010(6) 0.088(6) C66 0.229(9) 0.180(8) 0.091(6) -0.024(6) -0.004(6) 0.078(7) C67 0.208(9) 0.170(8) 0.119(7) -0.036(6) -0.039(7) 0.027(7) C68 0.243(9) 0.171(7) 0.129(7) -0.022(6) -0.003(7) 0.013(7) C69 0.224(9) 0.151(7) 0.112(7) -0.017(6) -0.009(7) 0.047(7) C70 0.198(8) 0.116(6) 0.059(5) -0.021(4) 0.017(5) 0.047(6) C71 0.220(11) 0.156(8) 0.070(6) -0.023(5) -0.018(7) 0.121(8) C72 0.070(5) 0.064(5) 0.074(5) -0.008(4) 0.013(4) 0.014(4) C73 0.054(4) 0.066(4) 0.066(4) -0.011(4) 0.014(3) 0.006(3) C74 0.082(5) 0.057(4) 0.070(5) -0.008(4) 0.008(4) 0.002(4) C75 0.077(5) 0.099(6) 0.075(5) 0.016(4) 0.015(4) -0.012(4) C76 0.100(6) 0.072(5) 0.084(5) -0.016(4) 0.033(5) -0.004(4) C77 0.087(5) 0.071(5) 0.096(6) -0.027(5) 0.016(5) 0.007(4) C78 0.066(4) 0.067(5) 0.071(5) -0.011(4) 0.020(4) 0.009(4) C79 0.088(6) 0.061(5) 0.154(8) 0.017(5) 0.039(6) 0.014(4) C80 0.082(6) 0.076(5) 0.189(9) 0.034(6) 0.061(7) 0.016(5) C81 0.122(8) 0.150(8) 0.113(7) 0.045(6) 0.053(6) 0.051(6) C82 0.153(9) 0.126(7) 0.089(6) 0.022(5) 0.047(7) 0.049(7) C83 0.082(6) 0.086(6) 0.070(5) 0.019(5) -0.001(5) 0.010(5) C84 0.141(9) 0.102(6) 0.069(6) -0.003(5) 0.002(6) -0.019(6) C85 0.167(13) 0.130(9) 0.091(8) -0.006(6) -0.019(9) -0.038(9) C86 0.096(7) 0.159(10) 0.112(8) 0.055(7) -0.026(7) -0.052(8) C87 0.098(7) 0.114(7) 0.106(7) 0.032(5) 0.027(6) -0.014(6) C88 0.086(6) 0.058(4) 0.071(5) 0.020(4) 0.022(5) -0.011(4) C89 0.085(6) 0.083(5) 0.098(7) 0.003(5) 0.027(6) -0.041(5) C90 0.183(10) 0.114(7) 0.126(7) -0.011(5) 0.013(7) -0.056(7) C91 0.116(6) 0.119(6) 0.128(6) -0.002(4) 0.036(5) -0.052(5) C92 0.141(7) 0.137(7) 0.163(6) 0.023(6) 0.039(5) -0.034(6) C93 0.138(6) 0.134(6) 0.164(6) 0.010(5) 0.040(6) -0.037(6) C94 0.112(6) 0.131(6) 0.152(6) 0.017(5) 0.023(5) -0.060(5) C95 0.133(6) 0.130(6) 0.191(7) 0.011(6) 0.008(6) -0.066(6) C96 0.126(6) 0.135(6) 0.171(6) 0.031(5) 0.008(6) -0.046(5) N1 0.068(4) 0.094(4) 0.053(3) 0.004(3) 0.009(3) 0.013(3) N2 0.139(6) 0.094(5) 0.063(4) -0.026(4) 0.019(4) 0.039(4) N3 0.086(4) 0.048(3) 0.059(3) -0.003(3) 0.007(3) -0.004(3) N4 0.118(5) 0.042(3) 0.070(4) -0.014(3) 0.038(4) -0.009(3) N5 0.127(5) 0.085(4) 0.064(4) 0.007(3) 0.013(4) 0.056(4) N6 0.133(7) 0.156(7) 0.125(6) -0.035(5) 0.036(6) -0.076(6) N7 0.089(6) 0.154(9) 0.104(7) -0.051(7) 0.000(5) -0.009(6) N8 0.076(6) 0.130(8) 0.134(6) -0.014(6) 0.027(5) -0.040(5) N9 0.075(5) 0.116(6) 0.091(6) -0.004(4) 0.033(5) -0.004(4) N10 0.103(7) 0.140(7) 0.126(8) -0.057(8) -0.032(8) 0.017(7) N11 0.110(6) 0.100(6) 0.070(5) -0.005(4) 0.016(4) -0.007(5) N12 0.100(5) 0.068(4) 0.091(5) -0.005(5) 0.013(4) -0.007(5) O1 0.051(3) 0.102(3) 0.084(3) 0.006(3) 0.020(3) 0.005(3) O2 0.058(3) 0.112(4) 0.072(3) -0.016(2) 0.013(3) 0.017(2) O3 0.076(3) 0.076(3) 0.087(3) -0.004(3) 0.017(3) 0.000(2) O4 0.092(3) 0.073(3) 0.072(3) -0.017(3) 0.007(3) 0.010(3) O5 0.097(4) 0.069(3) 0.118(4) -0.030(3) 0.022(3) 0.024(3) O6 0.093(3) 0.039(3) 0.078(3) -0.0077(19) 0.025(2) -0.010(2) O7 0.095(4) 0.059(3) 0.060(3) -0.014(2) -0.001(3) -0.001(2) O8 0.082(4) 0.130(4) 0.070(3) -0.010(3) -0.004(3) 0.015(3) O9 0.167(5) 0.039(3) 0.067(3) -0.010(2) 0.008(3) -0.018(3) O10 0.147(4) 0.051(3) 0.074(3) -0.011(2) 0.038(3) -0.010(3) O11 0.096(4) 0.056(3) 0.088(3) -0.017(2) 0.003(3) 0.012(3) O12 0.108(4) 0.055(3) 0.089(3) 0.006(2) 0.018(3) 0.018(3) O13 0.100(4) 0.091(3) 0.104(4) 0.024(3) 0.044(3) 0.020(3) O14 0.096(4) 0.100(4) 0.091(3) 0.000(3) 0.014(3) 0.005(4) O15 0.145(5) 0.086(4) 0.095(4) 0.006(3) 0.054(4) -0.002(3) O16 0.103(5) 0.112(5) 0.135(5) -0.052(4) -0.006(4) -0.002(4) O17 0.149(6) 0.237(9) 0.099(5) -0.047(5) -0.045(5) 0.003(5) O18 0.068(3) 0.110(4) 0.101(4) -0.015(3) 0.000(3) 0.011(3) O19 0.078(3) 0.080(3) 0.179(5) -0.021(4) 0.046(3) -0.008(3) O20 0.134(6) 0.163(6) 0.240(8) 0.013(5) 0.096(6) -0.039(5) O21 0.105(5) 0.076(4) 0.176(6) -0.031(3) 0.044(4) -0.026(3) O22 0.067(3) 0.111(4) 0.086(3) 0.006(3) 0.029(3) -0.006(3) O23 0.099(5) 0.279(9) 0.091(4) 0.051(5) 0.016(4) -0.008(5) O24 0.067(3) 0.144(5) 0.107(4) 0.009(3) 0.032(3) -0.011(3) O25 0.118(5) 0.082(4) 0.091(4) -0.019(3) -0.017(4) 0.023(4) O26 0.143(6) 0.312(11) 0.171(6) -0.101(7) -0.086(5) 0.041(7) O27 0.100(5) 0.179(7) 0.132(5) -0.038(5) 0.018(5) -0.022(4) O28 0.123(5) 0.065(3) 0.096(4) -0.002(3) 0.015(3) -0.012(3) O29 0.124(5) 0.198(7) 0.093(4) 0.013(4) 0.050(4) -0.021(4) O30 0.111(4) 0.070(3) 0.105(4) -0.005(3) 0.038(3) 0.014(3) O31 0.115(4) 0.056(3) 0.109(4) -0.015(3) -0.017(3) 0.004(3) O32 0.117(4) 0.135(5) 0.115(4) -0.020(4) -0.046(4) -0.002(5) O33 0.102(4) 0.055(3) 0.104(4) -0.014(3) -0.010(3) 0.016(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag La1 O5 2.403(5) . ? La1 O6 2.415(4) . ? La1 O1 2.456(5) 2_647 ? La1 O21 2.568(6) . ? La1 O18 2.569(5) . ? La1 O19 2.569(5) . ? La1 O24 2.593(5) . ? La1 O22 2.600(4) . ? La1 O16 2.607(6) . ? La2 O10 2.420(4) . ? La2 O15 2.443(6) 2_756 ? La2 O11 2.457(4) . ? La2 O25 2.547(5) . ? La2 O28 2.599(5) . ? La2 O30 2.600(5) . ? La2 O31 2.602(5) . ? La2 O33 2.603(5) . ? La2 O27 2.604(7) . ? C1 C6 1.346(8) . ? C1 C2 1.405(9) . ? C1 H1 0.9300 . ? C2 C3 1.360(9) . ? C2 H2 0.9300 . ? C3 C4 1.368(10) . ? C3 H3 0.9300 . ? C4 C5 1.366(8) . ? C4 H4 0.9300 . ? C5 C6 1.373(8) . ? C5 H5 0.9300 . ? C6 C7 1.517(8) . ? C7 N1 1.490(7) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 O1 1.256(7) . ? C8 N1 1.325(7) . ? C8 C9 1.516(8) . ? C9 C10 1.357(9) . ? C9 C14 1.398(8) . ? C10 C11 1.408(9) . ? C10 H10 0.9300 . ? C11 C12 1.379(10) . ? C11 H11 0.9300 . ? C12 C13 1.351(9) . ? C12 H12 0.9300 . ? C13 C14 1.398(8) . ? C13 H13 0.9300 . ? C14 O2 1.343(7) . ? C15 O2 1.410(6) . ? C15 C16 1.466(8) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 O3 1.404(7) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 O3 1.426(7) . ? C17 C18 1.475(8) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 O4 1.424(6) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 O4 1.358(7) . ? C19 C24 1.365(9) . ? C19 C20 1.431(9) . ? C20 C21 1.392(10) . ? C20 H20 0.9300 . ? C21 C22 1.318(11) . ? C21 H21 0.9300 . ? C22 C23 1.392(10) . ? C22 H22 0.9300 . ? C23 C24 1.388(9) . ? C23 H23 0.9300 . ? C24 C25 1.433(9) . ? C25 O5 1.245(7) . ? C25 N2 1.300(8) . ? C26 C27 1.326(9) . ? C26 N2 1.476(8) . ? C26 C27' 1.498(9) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.3900 . ? C27 C32 1.3900 . ? C28 C29 1.3900 . ? C28 H28 0.9300 . ? C29 C30 1.3900 . ? C29 H29 0.9300 . ? C30 C31 1.3900 . ? C30 H30 0.9300 . ? C31 C32 1.3900 . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C27' C28' 1.3899 . ? C27' C32' 1.3901 . ? C28' C29' 1.3900 . ? C28' H28' 0.9300 . ? C29' C30' 1.3900 . ? C29' H29' 0.9300 . ? C30' C31' 1.3900 . ? C30' H30' 0.9300 . ? C31' C32' 1.3900 . ? C31' H31' 0.9300 . ? C32' H32' 0.9300 . ? C33 C38 1.396(9) . ? C33 C34 1.407(10) . ? C33 H33 0.9300 . ? C34 C35 1.327(11) . ? C34 H34 0.9300 . ? C35 C36 1.279(11) . ? C35 H35 0.9300 . ? C36 C37 1.438(11) . ? C36 H36 0.9300 . ? C37 C38 1.398(9) . ? C37 H37 0.9300 . ? C38 C39 1.513(9) . ? C39 N3 1.447(7) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 O6 1.244(6) . ? C40 N3 1.335(6) . ? C40 C41 1.510(8) . ? C41 C42 1.354(8) . ? C41 C46 1.421(8) . ? C42 C43 1.348(8) . ? C42 H42 0.9300 . ? C43 C44 1.393(9) . ? C43 H43 0.9300 . ? C44 C45 1.344(8) . ? C44 H44 0.9300 . ? C45 C46 1.395(8) . ? C45 H45 0.9300 . ? C46 O7 1.351(7) . ? C47 O7 1.452(7) . ? C47 C48 1.477(8) . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C48 O8 1.423(7) . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C49 O8 1.384(8) . ? C49 C50 1.465(9) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 O9 1.392(6) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C51 O9 1.351(6) . ? C51 C52 1.384(7) . ? C51 C56 1.405(8) . ? C52 C53 1.377(8) . ? C52 H52 0.9300 . ? C53 C54 1.381(8) . ? C53 H53 0.9300 . ? C54 C55 1.404(9) . ? C54 H54 0.9300 . ? C55 C56 1.352(8) . ? C55 H55 0.9300 . ? C56 C57 1.472(8) . ? C57 O10 1.265(6) . ? C57 N4 1.294(6) . ? C58 N4 1.455(7) . ? C58 C59 1.505(8) . ? C58 H58A 0.9700 . ? C58 H58B 0.9700 . ? C59 C64 1.351(9) . ? C59 C60 1.351(9) . ? C60 C61 1.330(9) . ? C60 H60 0.9300 . ? C61 C62 1.320(9) . ? C61 H61 0.9300 . ? C62 C63 1.355(11) . ? C62 H62 0.9300 . ? C63 C64 1.400(10) . ? C63 H63 0.9300 . ? C64 H64 0.9300 . ? C65 C70 1.353(9) . ? C65 C66 1.470(11) . ? C65 H65 0.9300 . ? C66 C67 1.393(12) . ? C66 H66 0.9300 . ? C67 C68 1.370(11) . ? C67 H67 0.9300 . ? C68 C69 1.406(12) . ? C68 H68 0.9300 . ? C69 C70 1.377(12) . ? C69 H69 0.9300 . ? C70 C71 1.539(13) . ? C71 N5 1.428(8) . ? C71 H71A 0.9700 . ? C71 H71B 0.9700 . ? C72 O11 1.264(7) . ? C72 N5 1.267(7) . ? C72 C73 1.537(8) . ? C73 C74 1.354(7) . ? C73 C78 1.430(8) . ? C74 C75 1.374(8) . ? C74 H74 0.9300 . ? C75 C76 1.374(9) . ? C75 H75 0.9300 . ? C76 C77 1.362(8) . ? C76 H76 0.9300 . ? C77 C78 1.394(8) . ? C77 H77 0.9300 . ? C78 O12 1.344(7) . ? C79 O12 1.446(7) . ? C79 C80 1.452(9) . ? C79 H79A 0.9700 . ? C79 H79B 0.9700 . ? C80 O13 1.393(8) . ? C80 H80A 0.9700 . ? C80 H80B 0.9700 . ? C81 O13 1.421(8) . ? C81 C82 1.516(11) . ? C81 H81A 0.9700 . ? C81 H81B 0.9700 . ? C82 O14 1.436(9) . ? C82 H82A 0.9700 . ? C82 H82B 0.9700 . ? C83 C88 1.348(9) . ? C83 O14 1.371(8) . ? C83 C84 1.400(10) . ? C84 C85 1.304(12) . ? C84 H84 0.9300 . ? C85 C86 1.359(13) . ? C85 H85 0.9300 . ? C86 C87 1.365(11) . ? C86 H86 0.9300 . ? C87 C88 1.335(10) . ? C87 H87 0.9300 . ? C88 C89 1.494(10) . ? C89 O15 1.238(8) . ? C89 N6 1.301(9) . ? C90 C91 1.504(8) . ? C90 N6 1.531(9) . ? C90 H90A 0.9700 . ? C90 H90B 0.9700 . ? C91 C92 1.3900 . ? C91 C96 1.3900 . ? C92 C93 1.3900 . ? C92 H92 0.9300 . ? C93 C94 1.3900 . ? C93 H93 0.9300 . ? C94 C95 1.3900 . ? C94 H94 0.9300 . ? C95 C96 1.3900 . ? C95 H95 0.9300 . ? C96 H96 0.9300 . ? N1 H1A 0.8600 . ? N2 H2A 0.8600 . ? N3 H3A 0.8600 . ? N4 H4A 0.8600 . ? N5 H5A 0.8600 . ? N6 H6 0.8600 . ? N7 O17 1.197(9) . ? N7 O16 1.255(9) . ? N7 O18 1.275(8) . ? N8 O20 1.221(8) . ? N8 O19 1.240(9) . ? N8 O21 1.264(8) . ? N9 O23 1.212(7) . ? N9 O24 1.239(7) . ? N9 O22 1.240(7) . ? N10 O26 1.217(9) . ? N10 O25 1.228(10) . ? N10 O27 1.246(10) . ? N11 O29 1.178(8) . ? N11 O28 1.257(7) . ? N11 O30 1.286(7) . ? N12 O32 1.198(6) . ? N12 O31 1.259(8) . ? N12 O33 1.288(7) . ? O1 La1 2.456(5) 2_657 ? O15 La2 2.443(6) 2_746 ? 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 O5 La1 O6 153.67(15) . . ? O5 La1 O1 81.82(18) . 2_647 ? O6 La1 O1 81.23(14) . 2_647 ? O5 La1 O21 75.3(2) . . ? O6 La1 O21 124.54(18) . . ? O1 La1 O21 153.87(17) 2_647 . ? O5 La1 O18 119.48(17) . . ? O6 La1 O18 76.93(16) . . ? O1 La1 O18 79.86(15) 2_647 . ? O21 La1 O18 100.38(18) . . ? O5 La1 O19 123.95(19) . . ? O6 La1 O19 78.32(17) . . ? O1 La1 O19 150.96(17) 2_647 . ? O21 La1 O19 48.65(19) . . ? O18 La1 O19 75.59(17) . . ? O5 La1 O24 91.00(17) . . ? O6 La1 O24 82.61(14) . . ? O1 La1 O24 125.37(15) 2_647 . ? O21 La1 O24 68.24(18) . . ? O18 La1 O24 144.51(17) . . ? O19 La1 O24 72.04(17) . . ? O5 La1 O22 75.51(16) . . ? O6 La1 O22 81.48(16) . . ? O1 La1 O22 78.60(15) 2_647 . ? O21 La1 O22 107.20(18) . . ? O18 La1 O22 151.47(17) . . ? O19 La1 O22 118.01(16) . . ? O24 La1 O22 47.48(15) . . ? O5 La1 O16 73.9(2) . . ? O6 La1 O16 125.90(19) . . ? O1 La1 O16 89.67(19) 2_647 . ? O21 La1 O16 72.0(2) . . ? O18 La1 O16 49.00(19) . . ? O19 La1 O16 85.87(19) . . ? O24 La1 O16 139.9(2) . . ? O22 La1 O16 148.47(19) . . ? O10 La2 O15 83.51(14) . 2_756 ? O10 La2 O11 154.71(15) . . ? O15 La2 O11 86.99(16) 2_756 . ? O10 La2 O25 83.76(16) . . ? O15 La2 O25 125.2(2) 2_756 . ? O11 La2 O25 82.71(16) . . ? O10 La2 O28 117.67(16) . . ? O15 La2 O28 156.99(16) 2_756 . ? O11 La2 O28 76.95(17) . . ? O25 La2 O28 69.43(19) . . ? O10 La2 O30 70.65(16) . . ? O15 La2 O30 147.27(17) 2_756 . ? O11 La2 O30 124.62(17) . . ? O25 La2 O30 72.66(19) . . ? O28 La2 O30 48.19(17) . . ? O10 La2 O31 125.89(16) . . ? O15 La2 O31 84.01(18) 2_756 . ? O11 La2 O31 76.01(15) . . ? O25 La2 O31 142.86(19) . . ? O28 La2 O31 76.26(17) . . ? O30 La2 O31 94.92(17) . . ? O10 La2 O33 77.88(15) . . ? O15 La2 O33 83.74(18) 2_756 . ? O11 La2 O33 124.33(14) . . ? O25 La2 O33 143.62(18) . . ? O28 La2 O33 91.75(16) . . ? O30 La2 O33 71.70(17) . . ? O31 La2 O33 48.49(14) . . ? O10 La2 O27 76.0(2) . . ? O15 La2 O27 76.4(2) 2_756 . ? O11 La2 O27 79.0(2) . . ? O25 La2 O27 48.9(2) . . ? O28 La2 O27 115.7(2) . . ? O30 La2 O27 114.63(19) . . ? O31 La2 O27 148.9(2) . . ? O33 La2 O27 148.6(2) . . ? C6 C1 C2 118.4(7) . . ? C6 C1 H1 120.8 . . ? C2 C1 H1 120.8 . . ? C3 C2 C1 121.3(7) . . ? C3 C2 H2 119.3 . . ? C1 C2 H2 119.3 . . ? C2 C3 C4 119.0(7) . . ? C2 C3 H3 120.5 . . ? C4 C3 H3 120.5 . . ? C5 C4 C3 120.0(7) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 120.7(7) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C1 C6 C5 120.5(7) . . ? C1 C6 C7 121.4(7) . . ? C5 C6 C7 118.1(6) . . ? N1 C7 C6 114.8(5) . . ? N1 C7 H7A 108.6 . . ? C6 C7 H7A 108.6 . . ? N1 C7 H7B 108.6 . . ? C6 C7 H7B 108.6 . . ? H7A C7 H7B 107.5 . . ? O1 C8 N1 122.2(6) . . ? O1 C8 C9 121.1(6) . . ? N1 C8 C9 116.7(7) . . ? C10 C9 C14 121.0(7) . . ? C10 C9 C8 115.4(7) . . ? C14 C9 C8 123.6(6) . . ? C9 C10 C11 119.4(7) . . ? C9 C10 H10 120.3 . . ? C11 C10 H10 120.3 . . ? C12 C11 C10 119.1(7) . . ? C12 C11 H11 120.4 . . ? C10 C11 H11 120.4 . . ? C13 C12 C11 121.8(7) . . ? C13 C12 H12 119.1 . . ? C11 C12 H12 119.1 . . ? C12 C13 C14 119.6(8) . . ? C12 C13 H13 120.2 . . ? C14 C13 H13 120.2 . . ? O2 C14 C13 123.0(6) . . ? O2 C14 C9 117.9(6) . . ? C13 C14 C9 119.1(6) . . ? O2 C15 C16 107.0(5) . . ? O2 C15 H15A 110.3 . . ? C16 C15 H15A 110.3 . . ? O2 C15 H15B 110.3 . . ? C16 C15 H15B 110.3 . . ? H15A C15 H15B 108.6 . . ? O3 C16 C15 109.2(6) . . ? O3 C16 H16A 109.8 . . ? C15 C16 H16A 109.8 . . ? O3 C16 H16B 109.8 . . ? C15 C16 H16B 109.8 . . ? H16A C16 H16B 108.3 . . ? O3 C17 C18 109.7(6) . . ? O3 C17 H17A 109.7 . . ? C18 C17 H17A 109.7 . . ? O3 C17 H17B 109.7 . . ? C18 C17 H17B 109.7 . . ? H17A C17 H17B 108.2 . . ? O4 C18 C17 108.8(5) . . ? O4 C18 H18A 109.9 . . ? C17 C18 H18A 109.9 . . ? O4 C18 H18B 109.9 . . ? C17 C18 H18B 109.9 . . ? H18A C18 H18B 108.3 . . ? O4 C19 C24 117.6(7) . . ? O4 C19 C20 122.3(7) . . ? C24 C19 C20 120.1(7) . . ? C21 C20 C19 120.8(7) . . ? C21 C20 H20 119.6 . . ? C19 C20 H20 119.6 . . ? C22 C21 C20 119.1(8) . . ? C22 C21 H21 120.4 . . ? C20 C21 H21 120.4 . . ? C21 C22 C23 119.8(9) . . ? C21 C22 H22 120.1 . . ? C23 C22 H22 120.1 . . ? C24 C23 C22 124.3(8) . . ? C24 C23 H23 117.9 . . ? C22 C23 H23 117.9 . . ? C19 C24 C23 115.8(7) . . ? C19 C24 C25 128.3(8) . . ? C23 C24 C25 115.9(8) . . ? O5 C25 N2 119.2(7) . . ? O5 C25 C24 121.9(7) . . ? N2 C25 C24 118.9(7) . . ? C27 C26 N2 111.9(7) . . ? C27 C26 C27' 23.78(17) . . ? N2 C26 C27' 113.3(7) . . ? C27 C26 H26A 109.2 . . ? N2 C26 H26A 109.2 . . ? C27' C26 H26A 126.5 . . ? C27 C26 H26B 109.2 . . ? N2 C26 H26B 109.2 . . ? C27' C26 H26B 87.1 . . ? H26A C26 H26B 107.9 . . ? C26 C27 C28 113.5(9) . . ? C26 C27 C32 126.5(9) . . ? C28 C27 C32 120.0 . . ? C29 C28 C27 120.0 . . ? C29 C28 H28 120.0 . . ? C27 C28 H28 120.0 . . ? C28 C29 C30 120.0 . . ? C28 C29 H29 120.0 . . ? C30 C29 H29 120.0 . . ? C31 C30 C29 120.0 . . ? C31 C30 H30 120.0 . . ? C29 C30 H30 120.0 . . ? C32 C31 C30 120.0 . . ? C32 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? C31 C32 C27 120.0 . . ? C31 C32 H32 120.0 . . ? C27 C32 H32 120.0 . . ? C28' C27' C32' 120.0 . . ? C28' C27' C26 116.0(8) . . ? C32' C27' C26 123.9(8) . . ? C27' C28' C29' 120.0 . . ? C27' C28' H28' 120.0 . . ? C29' C28' H28' 120.0 . . ? C28' C29' C30' 120.0 . . ? C28' C29' H29' 120.0 . . ? C30' C29' H29' 120.0 . . ? C31' C30' C29' 120.0 . . ? C31' C30' H30' 120.0 . . ? C29' C30' H30' 120.0 . . ? C30' C31' C32' 120.0 . . ? C30' C31' H31' 120.0 . . ? C32' C31' H31' 120.0 . . ? C31' C32' C27' 120.0 . . ? C31' C32' H32' 120.0 . . ? C27' C32' H32' 120.0 . . ? C38 C33 C34 121.6(8) . . ? C38 C33 H33 119.2 . . ? C34 C33 H33 119.2 . . ? C35 C34 C33 119.2(9) . . ? C35 C34 H34 120.4 . . ? C33 C34 H34 120.4 . . ? C36 C35 C34 123.7(12) . . ? C36 C35 H35 118.1 . . ? C34 C35 H35 118.1 . . ? C35 C36 C37 119.3(10) . . ? C35 C36 H36 120.3 . . ? C37 C36 H36 120.3 . . ? C38 C37 C36 121.1(8) . . ? C38 C37 H37 119.5 . . ? C36 C37 H37 119.5 . . ? C33 C38 C37 114.9(8) . . ? C33 C38 C39 121.1(7) . . ? C37 C38 C39 124.0(7) . . ? N3 C39 C38 108.6(5) . . ? N3 C39 H39A 110.0 . . ? C38 C39 H39A 110.0 . . ? N3 C39 H39B 110.0 . . ? C38 C39 H39B 110.0 . . ? H39A C39 H39B 108.4 . . ? O6 C40 N3 121.7(5) . . ? O6 C40 C41 118.8(5) . . ? N3 C40 C41 119.3(5) . . ? C42 C41 C46 117.6(6) . . ? C42 C41 C40 118.3(6) . . ? C46 C41 C40 123.9(6) . . ? C43 C42 C41 125.3(7) . . ? C43 C42 H42 117.3 . . ? C41 C42 H42 117.3 . . ? C42 C43 C44 115.9(7) . . ? C42 C43 H43 122.0 . . ? C44 C43 H43 122.0 . . ? C45 C44 C43 122.6(7) . . ? C45 C44 H44 118.7 . . ? C43 C44 H44 118.7 . . ? C44 C45 C46 120.2(7) . . ? C44 C45 H45 119.9 . . ? C46 C45 H45 119.9 . . ? O7 C46 C45 123.5(6) . . ? O7 C46 C41 118.2(6) . . ? C45 C46 C41 118.2(6) . . ? O7 C47 C48 106.3(5) . . ? O7 C47 H47A 110.5 . . ? C48 C47 H47A 110.5 . . ? O7 C47 H47B 110.5 . . ? C48 C47 H47B 110.5 . . ? H47A C47 H47B 108.7 . . ? O8 C48 C47 108.3(6) . . ? O8 C48 H48A 110.0 . . ? C47 C48 H48A 110.0 . . ? O8 C48 H48B 110.0 . . ? C47 C48 H48B 110.0 . . ? H48A C48 H48B 108.4 . . ? O8 C49 C50 110.0(7) . . ? O8 C49 H49A 109.7 . . ? C50 C49 H49A 109.7 . . ? O8 C49 H49B 109.7 . . ? C50 C49 H49B 109.7 . . ? H49A C49 H49B 108.2 . . ? O9 C50 C49 111.1(5) . . ? O9 C50 H50A 109.4 . . ? C49 C50 H50A 109.4 . . ? O9 C50 H50B 109.4 . . ? C49 C50 H50B 109.4 . . ? H50A C50 H50B 108.0 . . ? O9 C51 C52 122.8(6) . . ? O9 C51 C56 118.0(5) . . ? C52 C51 C56 119.2(6) . . ? C53 C52 C51 121.3(6) . . ? C53 C52 H52 119.3 . . ? C51 C52 H52 119.3 . . ? C52 C53 C54 119.1(6) . . ? C52 C53 H53 120.4 . . ? C54 C53 H53 120.4 . . ? C53 C54 C55 119.8(6) . . ? C53 C54 H54 120.1 . . ? C55 C54 H54 120.1 . . ? C56 C55 C54 121.0(6) . . ? C56 C55 H55 119.5 . . ? C54 C55 H55 119.5 . . ? C55 C56 C51 119.6(6) . . ? C55 C56 C57 116.8(6) . . ? C51 C56 C57 123.5(6) . . ? O10 C57 N4 118.5(6) . . ? O10 C57 C56 119.3(6) . . ? N4 C57 C56 122.2(6) . . ? N4 C58 C59 111.1(5) . . ? N4 C58 H58A 109.4 . . ? C59 C58 H58A 109.4 . . ? N4 C58 H58B 109.4 . . ? C59 C58 H58B 109.4 . . ? H58A C58 H58B 108.0 . . ? C64 C59 C60 118.3(7) . . ? C64 C59 C58 120.7(8) . . ? C60 C59 C58 120.9(8) . . ? C61 C60 C59 121.1(8) . . ? C61 C60 H60 119.4 . . ? C59 C60 H60 119.4 . . ? C62 C61 C60 122.0(9) . . ? C62 C61 H61 119.0 . . ? C60 C61 H61 119.0 . . ? C61 C62 C63 119.2(9) . . ? C61 C62 H62 120.4 . . ? C63 C62 H62 120.4 . . ? C62 C63 C64 118.7(8) . . ? C62 C63 H63 120.6 . . ? C64 C63 H63 120.6 . . ? C59 C64 C63 119.9(8) . . ? C59 C64 H64 120.1 . . ? C63 C64 H64 120.1 . . ? C70 C65 C66 123.3(11) . . ? C70 C65 H65 118.4 . . ? C66 C65 H65 118.4 . . ? C67 C66 C65 111.9(11) . . ? C67 C66 H66 124.1 . . ? C65 C66 H66 124.1 . . ? C68 C67 C66 121.5(12) . . ? C68 C67 H67 119.3 . . ? C66 C67 H67 119.3 . . ? C67 C68 C69 127.3(13) . . ? C67 C68 H68 116.4 . . ? C69 C68 H68 116.4 . . ? C70 C69 C68 110.9(11) . . ? C70 C69 H69 124.5 . . ? C68 C69 H69 124.5 . . ? C65 C70 C69 125.0(12) . . ? C65 C70 C71 119.6(11) . . ? C69 C70 C71 115.3(9) . . ? N5 C71 C70 110.4(7) . . ? N5 C71 H71A 109.6 . . ? C70 C71 H71A 109.6 . . ? N5 C71 H71B 109.6 . . ? C70 C71 H71B 109.6 . . ? H71A C71 H71B 108.1 . . ? O11 C72 N5 123.0(6) . . ? O11 C72 C73 115.9(6) . . ? N5 C72 C73 121.1(6) . . ? C74 C73 C78 120.3(6) . . ? C74 C73 C72 119.0(6) . . ? C78 C73 C72 120.7(6) . . ? C73 C74 C75 120.1(6) . . ? C73 C74 H74 120.0 . . ? C75 C74 H74 120.0 . . ? C74 C75 C76 121.8(6) . . ? C74 C75 H75 119.1 . . ? C76 C75 H75 119.1 . . ? C77 C76 C75 118.4(7) . . ? C77 C76 H76 120.8 . . ? C75 C76 H76 120.8 . . ? C76 C77 C78 122.5(7) . . ? C76 C77 H77 118.8 . . ? C78 C77 H77 118.8 . . ? O12 C78 C77 124.9(6) . . ? O12 C78 C73 118.1(6) . . ? C77 C78 C73 116.9(6) . . ? O12 C79 C80 106.2(6) . . ? O12 C79 H79A 110.5 . . ? C80 C79 H79A 110.5 . . ? O12 C79 H79B 110.5 . . ? C80 C79 H79B 110.5 . . ? H79A C79 H79B 108.7 . . ? O13 C80 C79 109.7(7) . . ? O13 C80 H80A 109.7 . . ? C79 C80 H80A 109.7 . . ? O13 C80 H80B 109.7 . . ? C79 C80 H80B 109.7 . . ? H80A C80 H80B 108.2 . . ? O13 C81 C82 110.0(7) . . ? O13 C81 H81A 109.7 . . ? C82 C81 H81A 109.7 . . ? O13 C81 H81B 109.7 . . ? C82 C81 H81B 109.7 . . ? H81A C81 H81B 108.2 . . ? O14 C82 C81 106.7(7) . . ? O14 C82 H82A 110.4 . . ? C81 C82 H82A 110.4 . . ? O14 C82 H82B 110.4 . . ? C81 C82 H82B 110.4 . . ? H82A C82 H82B 108.6 . . ? C88 C83 O14 117.3(8) . . ? C88 C83 C84 121.0(8) . . ? O14 C83 C84 121.6(9) . . ? C85 C84 C83 120.1(10) . . ? C85 C84 H84 119.9 . . ? C83 C84 H84 120.0 . . ? C84 C85 C86 119.2(11) . . ? C84 C85 H85 120.4 . . ? C86 C85 H85 120.4 . . ? C85 C86 C87 120.7(10) . . ? C85 C86 H86 119.6 . . ? C87 C86 H86 119.6 . . ? C88 C87 C86 121.1(9) . . ? C88 C87 H87 119.4 . . ? C86 C87 H87 119.4 . . ? C87 C88 C83 117.8(8) . . ? C87 C88 C89 116.5(9) . . ? C83 C88 C89 125.7(8) . . ? O15 C89 N6 118.2(8) . . ? O15 C89 C88 124.1(8) . . ? N6 C89 C88 117.4(8) . . ? C91 C90 N6 111.8(7) . . ? C91 C90 H90A 109.3 . . ? N6 C90 H90A 109.3 . . ? C91 C90 H90B 109.3 . . ? N6 C90 H90B 109.3 . . ? H90A C90 H90B 107.9 . . ? C92 C91 C96 120.0 . . ? C92 C91 C90 114.7(6) . . ? C96 C91 C90 124.9(6) . . ? C93 C92 C91 120.0 . . ? C93 C92 H92 120.0 . . ? C91 C92 H92 120.0 . . ? C92 C93 C94 120.0 . . ? C92 C93 H93 120.0 . . ? C94 C93 H93 120.0 . . ? C95 C94 C93 120.0 . . ? C95 C94 H94 120.0 . . ? C93 C94 H94 120.0 . . ? C94 C95 C96 120.0 . . ? C94 C95 H95 120.0 . . ? C96 C95 H95 120.0 . . ? C95 C96 C91 120.0 . . ? C95 C96 H96 120.0 . . ? C91 C96 H96 120.0 . . ? C8 N1 C7 122.3(6) . . ? C8 N1 H1A 118.8 . . ? C7 N1 H1A 118.8 . . ? C25 N2 C26 123.5(6) . . ? C25 N2 H2A 118.3 . . ? C26 N2 H2A 118.3 . . ? C40 N3 C39 124.3(5) . . ? C40 N3 H3A 117.8 . . ? C39 N3 H3A 117.8 . . ? C57 N4 C58 126.8(5) . . ? C57 N4 H4A 116.6 . . ? C58 N4 H4A 116.6 . . ? C72 N5 C71 122.3(6) . . ? C72 N5 H5A 118.8 . . ? C71 N5 H5A 118.8 . . ? C89 N6 C90 129.0(8) . . ? C89 N6 H6 115.5 . . ? C90 N6 H6 115.5 . . ? O17 N7 O16 124.4(9) . . ? O17 N7 O18 119.6(10) . . ? O16 N7 O18 116.1(9) . . ? O20 N8 O19 123.3(10) . . ? O20 N8 O21 121.4(9) . . ? O19 N8 O21 115.3(8) . . ? O23 N9 O24 121.6(7) . . ? O23 N9 O22 123.3(7) . . ? O24 N9 O22 115.0(7) . . ? O26 N10 O25 121.1(12) . . ? O26 N10 O27 119.9(12) . . ? O25 N10 O27 119.0(10) . . ? O29 N11 O28 123.8(8) . . ? O29 N11 O30 123.0(8) . . ? O28 N11 O30 113.2(7) . . ? O32 N12 O31 123.6(7) . . ? O32 N12 O33 122.2(8) . . ? O31 N12 O33 114.1(6) . . ? C8 O1 La1 178.7(4) . 2_657 ? C14 O2 C15 118.4(5) . . ? C16 O3 C17 112.1(6) . . ? C19 O4 C18 121.1(5) . . ? C25 O5 La1 164.5(5) . . ? C40 O6 La1 171.6(4) . . ? C46 O7 C47 119.4(5) . . ? C49 O8 C48 114.9(6) . . ? C51 O9 C50 122.3(5) . . ? C57 O10 La2 170.7(4) . . ? C72 O11 La2 171.6(5) . . ? C78 O12 C79 119.6(5) . . ? C80 O13 C81 111.5(7) . . ? C83 O14 C82 120.2(7) . . ? C89 O15 La2 169.4(5) . 2_746 ? N7 O16 La1 96.7(5) . . ? N7 O18 La1 98.0(6) . . ? N8 O19 La1 97.6(5) . . ? N8 O21 La1 96.9(5) . . ? N9 O22 La1 98.5(5) . . ? N9 O24 La1 98.8(5) . . ? N10 O25 La2 97.6(7) . . ? N10 O27 La2 94.3(6) . . ? N11 O28 La2 99.3(5) . . ? N11 O30 La2 98.4(5) . . ? N12 O31 La2 99.1(4) . . ? N12 O33 La2 98.2(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 2.5(12) . . . . ? C1 C2 C3 C4 -1.1(13) . . . . ? C2 C3 C4 C5 0.7(12) . . . . ? C3 C4 C5 C6 -1.7(11) . . . . ? C2 C1 C6 C5 -3.4(11) . . . . ? C2 C1 C6 C7 178.7(6) . . . . ? C4 C5 C6 C1 3.1(11) . . . . ? C4 C5 C6 C7 -178.9(6) . . . . ? C1 C6 C7 N1 26.5(10) . . . . ? C5 C6 C7 N1 -151.5(6) . . . . ? O1 C8 C9 C10 -17.6(8) . . . . ? N1 C8 C9 C10 159.8(6) . . . . ? O1 C8 C9 C14 164.5(6) . . . . ? N1 C8 C9 C14 -18.1(8) . . . . ? C14 C9 C10 C11 1.7(11) . . . . ? C8 C9 C10 C11 -176.3(7) . . . . ? C9 C10 C11 C12 -0.1(13) . . . . ? C10 C11 C12 C13 -0.2(16) . . . . ? C11 C12 C13 C14 -1.1(15) . . . . ? C12 C13 C14 O2 -179.7(7) . . . . ? C12 C13 C14 C9 2.6(11) . . . . ? C10 C9 C14 O2 179.2(6) . . . . ? C8 C9 C14 O2 -3.0(8) . . . . ? C10 C9 C14 C13 -3.0(9) . . . . ? C8 C9 C14 C13 174.8(6) . . . . ? O2 C15 C16 O3 62.6(8) . . . . ? O3 C17 C18 O4 72.5(7) . . . . ? O4 C19 C20 C21 -176.9(7) . . . . ? C24 C19 C20 C21 4.2(11) . . . . ? C19 C20 C21 C22 -4.1(13) . . . . ? C20 C21 C22 C23 1.1(15) . . . . ? C21 C22 C23 C24 2.2(15) . . . . ? O4 C19 C24 C23 180.0(6) . . . . ? C20 C19 C24 C23 -1.1(10) . . . . ? O4 C19 C24 C25 0.0(11) . . . . ? C20 C19 C24 C25 178.9(7) . . . . ? C22 C23 C24 C19 -2.1(12) . . . . ? C22 C23 C24 C25 177.9(8) . . . . ? C19 C24 C25 O5 177.2(7) . . . . ? C23 C24 C25 O5 -2.8(11) . . . . ? C19 C24 C25 N2 -2.5(12) . . . . ? C23 C24 C25 N2 177.5(7) . . . . ? N2 C26 C27 C28 -94.5(8) . . . . ? C27' C26 C27 C28 3.9(2) . . . . ? N2 C26 C27 C32 87.6(10) . . . . ? C27' C26 C27 C32 -174.0(5) . . . . ? C26 C27 C28 C29 -178.1(6) . . . . ? C32 C27 C28 C29 0.0 . . . . ? C27 C28 C29 C30 0.0 . . . . ? C28 C29 C30 C31 0.0 . . . . ? C29 C30 C31 C32 0.0 . . . . ? C30 C31 C32 C27 0.0 . . . . ? C26 C27 C32 C31 177.8(7) . . . . ? C28 C27 C32 C31 0.0 . . . . ? C27 C26 C27' C28' -173.81(5) . . . . ? N2 C26 C27' C28' -82.2(8) . . . . ? C27 C26 C27' C32' 4.5(6) . . . . ? N2 C26 C27' C32' 96.1(9) . . . . ? C32' C27' C28' C29' 0.0 . . . . ? C26 C27' C28' C29' 178.3(5) . . . . ? C27' C28' C29' C30' 0.0 . . . . ? C28' C29' C30' C31' 0.0 . . . . ? C29' C30' C31' C32' 0.0 . . . . ? C30' C31' C32' C27' 0.0 . . . . ? C28' C27' C32' C31' 0.0 . . . . ? C26 C27' C32' C31' -178.2(6) . . . . ? C38 C33 C34 C35 -4.3(13) . . . . ? C33 C34 C35 C36 1.1(15) . . . . ? C34 C35 C36 C37 1.1(15) . . . . ? C35 C36 C37 C38 -0.4(12) . . . . ? C34 C33 C38 C37 4.7(10) . . . . ? C34 C33 C38 C39 -173.3(7) . . . . ? C36 C37 C38 C33 -2.5(9) . . . . ? C36 C37 C38 C39 175.5(6) . . . . ? C33 C38 C39 N3 85.0(7) . . . . ? C37 C38 C39 N3 -92.8(8) . . . . ? O6 C40 C41 C42 9.4(9) . . . . ? N3 C40 C41 C42 -175.3(6) . . . . ? O6 C40 C41 C46 -174.7(6) . . . . ? N3 C40 C41 C46 0.6(9) . . . . ? C46 C41 C42 C43 2.8(11) . . . . ? C40 C41 C42 C43 179.0(6) . . . . ? C41 C42 C43 C44 -1.7(11) . . . . ? C42 C43 C44 C45 0.1(12) . . . . ? C43 C44 C45 C46 0.2(12) . . . . ? C44 C45 C46 O7 178.0(7) . . . . ? C44 C45 C46 C41 0.8(10) . . . . ? C42 C41 C46 O7 -179.6(6) . . . . ? C40 C41 C46 O7 4.5(9) . . . . ? C42 C41 C46 C45 -2.2(9) . . . . ? C40 C41 C46 C45 -178.2(6) . . . . ? O7 C47 C48 O8 -75.4(7) . . . . ? O8 C49 C50 O9 -66.9(8) . . . . ? O9 C51 C52 C53 -178.2(6) . . . . ? C56 C51 C52 C53 -0.6(10) . . . . ? C51 C52 C53 C54 0.2(11) . . . . ? C52 C53 C54 C55 0.0(12) . . . . ? C53 C54 C55 C56 0.3(12) . . . . ? C54 C55 C56 C51 -0.7(11) . . . . ? C54 C55 C56 C57 178.1(7) . . . . ? O9 C51 C56 C55 178.6(6) . . . . ? C52 C51 C56 C55 0.8(10) . . . . ? O9 C51 C56 C57 -0.1(10) . . . . ? C52 C51 C56 C57 -177.8(6) . . . . ? C55 C56 C57 O10 9.0(10) . . . . ? C51 C56 C57 O10 -172.4(6) . . . . ? C55 C56 C57 N4 -171.2(7) . . . . ? C51 C56 C57 N4 7.4(11) . . . . ? N4 C58 C59 C64 -96.1(8) . . . . ? N4 C58 C59 C60 86.7(8) . . . . ? C64 C59 C60 C61 4.9(11) . . . . ? C58 C59 C60 C61 -177.7(6) . . . . ? C59 C60 C61 C62 -1.1(12) . . . . ? C60 C61 C62 C63 -6.9(13) . . . . ? C61 C62 C63 C64 10.6(14) . . . . ? C60 C59 C64 C63 -0.9(11) . . . . ? C58 C59 C64 C63 -178.2(7) . . . . ? C62 C63 C64 C59 -6.8(13) . . . . ? C70 C65 C66 C67 1.5(14) . . . . ? C65 C66 C67 C68 -2.8(16) . . . . ? C66 C67 C68 C69 0.6(19) . . . . ? C67 C68 C69 C70 3.0(16) . . . . ? C66 C65 C70 C69 2.4(15) . . . . ? C66 C65 C70 C71 179.2(8) . . . . ? C68 C69 C70 C65 -4.4(15) . . . . ? C68 C69 C70 C71 178.7(8) . . . . ? C65 C70 C71 N5 -121.4(9) . . . . ? C69 C70 C71 N5 55.7(11) . . . . ? O11 C72 C73 C74 12.4(9) . . . . ? N5 C72 C73 C74 -169.3(6) . . . . ? O11 C72 C73 C78 -167.4(6) . . . . ? N5 C72 C73 C78 10.9(9) . . . . ? C78 C73 C74 C75 0.4(9) . . . . ? C72 C73 C74 C75 -179.4(5) . . . . ? C73 C74 C75 C76 -0.8(10) . . . . ? C74 C75 C76 C77 0.4(11) . . . . ? C75 C76 C77 C78 0.4(11) . . . . ? C76 C77 C78 O12 -179.4(7) . . . . ? C76 C77 C78 C73 -0.7(10) . . . . ? C74 C73 C78 O12 179.1(6) . . . . ? C72 C73 C78 O12 -1.1(9) . . . . ? C74 C73 C78 C77 0.3(9) . . . . ? C72 C73 C78 C77 -179.9(6) . . . . ? O12 C79 C80 O13 -66.9(7) . . . . ? O13 C81 C82 O14 -66.2(8) . . . . ? C88 C83 C84 C85 -0.8(13) . . . . ? O14 C83 C84 C85 176.6(8) . . . . ? C83 C84 C85 C86 0.6(15) . . . . ? C84 C85 C86 C87 -1.2(16) . . . . ? C85 C86 C87 C88 1.9(13) . . . . ? C86 C87 C88 C83 -2.1(11) . . . . ? C86 C87 C88 C89 176.5(7) . . . . ? O14 C83 C88 C87 -176.0(6) . . . . ? C84 C83 C88 C87 1.5(10) . . . . ? O14 C83 C88 C89 5.6(10) . . . . ? C84 C83 C88 C89 -176.9(7) . . . . ? C87 C88 C89 O15 -8.7(10) . . . . ? C83 C88 C89 O15 169.7(7) . . . . ? C87 C88 C89 N6 178.0(7) . . . . ? C83 C88 C89 N6 -3.6(11) . . . . ? N6 C90 C91 C92 -58.7(8) . . . . ? N6 C90 C91 C96 128.4(7) . . . . ? C96 C91 C92 C93 0.0 . . . . ? C90 C91 C92 C93 -173.3(6) . . . . ? C91 C92 C93 C94 0.0 . . . . ? C92 C93 C94 C95 0.0 . . . . ? C93 C94 C95 C96 0.0 . . . . ? C94 C95 C96 C91 0.0 . . . . ? C92 C91 C96 C95 0.0 . . . . ? C90 C91 C96 C95 172.5(6) . . . . ? O1 C8 N1 C7 6.2(9) . . . . ? C9 C8 N1 C7 -171.1(5) . . . . ? C6 C7 N1 C8 99.5(7) . . . . ? O5 C25 N2 C26 -5.9(12) . . . . ? C24 C25 N2 C26 173.8(8) . . . . ? C27 C26 N2 C25 159.7(9) . . . . ? C27' C26 N2 C25 134.0(9) . . . . ? O6 C40 N3 C39 -1.1(10) . . . . ? C41 C40 N3 C39 -176.2(6) . . . . ? C38 C39 N3 C40 107.0(7) . . . . ? O10 C57 N4 C58 -3.0(11) . . . . ? C56 C57 N4 C58 177.3(6) . . . . ? C59 C58 N4 C57 -139.7(7) . . . . ? O11 C72 N5 C71 2.4(12) . . . . ? C73 C72 N5 C71 -175.8(7) . . . . ? C70 C71 N5 C72 -126.0(8) . . . . ? O15 C89 N6 C90 -6.1(13) . . . . ? C88 C89 N6 C90 167.6(7) . . . . ? C91 C90 N6 C89 111.1(10) . . . . ? N1 C8 O1 La1 -63(21) . . . 2_657 ? C9 C8 O1 La1 114(20) . . . 2_657 ? C13 C14 O2 C15 -2.3(9) . . . . ? C9 C14 O2 C15 175.4(6) . . . . ? C16 C15 O2 C14 -176.5(6) . . . . ? C15 C16 O3 C17 177.8(5) . . . . ? C18 C17 O3 C16 -176.6(5) . . . . ? C24 C19 O4 C18 -173.6(6) . . . . ? C20 C19 O4 C18 7.5(10) . . . . ? C17 C18 O4 C19 172.6(6) . . . . ? N2 C25 O5 La1 96.3(19) . . . . ? C24 C25 O5 La1 -83(2) . . . . ? O6 La1 O5 C25 -179.3(18) . . . . ? O1 La1 O5 C25 130(2) 2_647 . . . ? O21 La1 O5 C25 -36.8(19) . . . . ? O18 La1 O5 C25 57(2) . . . . ? O19 La1 O5 C25 -35(2) . . . . ? O24 La1 O5 C25 -104(2) . . . . ? O22 La1 O5 C25 -149(2) . . . . ? O16 La1 O5 C25 38.3(19) . . . . ? N3 C40 O6 La1 127(2) . . . . ? C41 C40 O6 La1 -58(3) . . . . ? O5 La1 O6 C40 -37(3) . . . . ? O1 La1 O6 C40 14(3) 2_647 . . . ? O21 La1 O6 C40 -171(3) . . . . ? O18 La1 O6 C40 95(3) . . . . ? O19 La1 O6 C40 173(3) . . . . ? O24 La1 O6 C40 -114(3) . . . . ? O22 La1 O6 C40 -66(3) . . . . ? O16 La1 O6 C40 97(3) . . . . ? C45 C46 O7 C47 9.1(9) . . . . ? C41 C46 O7 C47 -173.7(5) . . . . ? C48 C47 O7 C46 173.9(6) . . . . ? C50 C49 O8 C48 163.5(5) . . . . ? C47 C48 O8 C49 150.4(6) . . . . ? C52 C51 O9 C50 -26.3(9) . . . . ? C56 C51 O9 C50 156.0(7) . . . . ? C49 C50 O9 C51 -118.4(7) . . . . ? N4 C57 O10 La2 54(3) . . . . ? C56 C57 O10 La2 -126(3) . . . . ? O15 La2 O10 C57 166(3) 2_756 . . . ? O11 La2 O10 C57 -125(3) . . . . ? O25 La2 O10 C57 -67(3) . . . . ? O28 La2 O10 C57 -4(3) . . . . ? O30 La2 O10 C57 7(3) . . . . ? O31 La2 O10 C57 88(3) . . . . ? O33 La2 O10 C57 81(3) . . . . ? O27 La2 O10 C57 -116(3) . . . . ? N5 C72 O11 La2 -84(3) . . . . ? C73 C72 O11 La2 94(3) . . . . ? O10 La2 O11 C72 143(3) . . . . ? O15 La2 O11 C72 -149(3) 2_756 . . . ? O25 La2 O11 C72 85(3) . . . . ? O28 La2 O11 C72 14(3) . . . . ? O30 La2 O11 C72 22(3) . . . . ? O31 La2 O11 C72 -64(3) . . . . ? O33 La2 O11 C72 -69(3) . . . . ? O27 La2 O11 C72 134(3) . . . . ? C77 C78 O12 C79 -3.5(9) . . . . ? C73 C78 O12 C79 177.9(6) . . . . ? C80 C79 O12 C78 -176.3(6) . . . . ? C79 C80 O13 C81 176.0(6) . . . . ? C82 C81 O13 C80 176.0(7) . . . . ? C88 C83 O14 C82 -175.3(6) . . . . ? C84 C83 O14 C82 7.2(10) . . . . ? C81 C82 O14 C83 -176.6(6) . . . . ? N6 C89 O15 La2 84(3) . . . 2_746 ? C88 C89 O15 La2 -89(3) . . . 2_746 ? O17 N7 O16 La1 -175.8(8) . . . . ? O18 N7 O16 La1 4.2(8) . . . . ? O5 La1 O16 N7 155.9(6) . . . . ? O6 La1 O16 N7 -4.6(7) . . . . ? O1 La1 O16 N7 74.4(6) 2_647 . . . ? O21 La1 O16 N7 -124.6(6) . . . . ? O18 La1 O16 N7 -2.5(5) . . . . ? O19 La1 O16 N7 -76.9(6) . . . . ? O24 La1 O16 N7 -132.4(6) . . . . ? O22 La1 O16 N7 141.6(5) . . . . ? O17 N7 O18 La1 175.8(7) . . . . ? O16 N7 O18 La1 -4.2(9) . . . . ? O5 La1 O18 N7 -21.6(5) . . . . ? O6 La1 O18 N7 -179.3(5) . . . . ? O1 La1 O18 N7 -96.1(5) 2_647 . . . ? O21 La1 O18 N7 57.4(5) . . . . ? O19 La1 O18 N7 99.6(5) . . . . ? O24 La1 O18 N7 124.3(5) . . . . ? O22 La1 O18 N7 -137.5(5) . . . . ? O16 La1 O18 N7 2.4(5) . . . . ? O20 N8 O19 La1 -168.1(7) . . . . ? O21 N8 O19 La1 12.4(7) . . . . ? O5 La1 O19 N8 -9.5(5) . . . . ? O6 La1 O19 N8 155.1(5) . . . . ? O1 La1 O19 N8 -158.8(4) 2_647 . . . ? O21 La1 O19 N8 -7.3(4) . . . . ? O18 La1 O19 N8 -125.6(5) . . . . ? O24 La1 O19 N8 69.1(5) . . . . ? O22 La1 O19 N8 81.4(5) . . . . ? O16 La1 O19 N8 -77.0(5) . . . . ? O20 N8 O21 La1 168.1(7) . . . . ? O19 N8 O21 La1 -12.4(7) . . . . ? O5 La1 O21 N8 -174.7(5) . . . . ? O6 La1 O21 N8 -13.9(5) . . . . ? O1 La1 O21 N8 155.4(4) 2_647 . . . ? O18 La1 O21 N8 67.3(5) . . . . ? O19 La1 O21 N8 7.2(4) . . . . ? O24 La1 O21 N8 -77.6(5) . . . . ? O22 La1 O21 N8 -105.3(5) . . . . ? O16 La1 O21 N8 107.8(5) . . . . ? O23 N9 O22 La1 -173.4(7) . . . . ? O24 N9 O22 La1 4.1(6) . . . . ? O5 La1 O22 N9 102.7(4) . . . . ? O6 La1 O22 N9 -90.2(4) . . . . ? O1 La1 O22 N9 -172.9(4) 2_647 . . . ? O21 La1 O22 N9 33.4(5) . . . . ? O18 La1 O22 N9 -131.2(4) . . . . ? O19 La1 O22 N9 -18.3(5) . . . . ? O24 La1 O22 N9 -2.4(4) . . . . ? O16 La1 O22 N9 117.0(5) . . . . ? O23 N9 O24 La1 173.4(7) . . . . ? O22 N9 O24 La1 -4.2(7) . . . . ? O5 La1 O24 N9 -66.7(4) . . . . ? O6 La1 O24 N9 87.6(4) . . . . ? O1 La1 O24 N9 13.9(5) 2_647 . . . ? O21 La1 O24 N9 -140.5(5) . . . . ? O18 La1 O24 N9 142.5(4) . . . . ? O19 La1 O24 N9 167.7(5) . . . . ? O22 La1 O24 N9 2.4(4) . . . . ? O16 La1 O24 N9 -132.5(4) . . . . ? O26 N10 O25 La2 176.4(9) . . . . ? O27 N10 O25 La2 -4.3(12) . . . . ? O10 La2 O25 N10 -74.4(6) . . . . ? O15 La2 O25 N10 3.1(7) 2_756 . . . ? O11 La2 O25 N10 84.2(6) . . . . ? O28 La2 O25 N10 162.9(7) . . . . ? O30 La2 O25 N10 -146.1(7) . . . . ? O31 La2 O25 N10 139.2(6) . . . . ? O33 La2 O25 N10 -134.1(6) . . . . ? O27 La2 O25 N10 2.4(6) . . . . ? O26 N10 O27 La2 -176.5(9) . . . . ? O25 N10 O27 La2 4.2(11) . . . . ? O10 La2 O27 N10 91.6(7) . . . . ? O15 La2 O27 N10 178.3(7) 2_756 . . . ? O11 La2 O27 N10 -92.2(7) . . . . ? O25 La2 O27 N10 -2.3(6) . . . . ? O28 La2 O27 N10 -22.6(8) . . . . ? O30 La2 O27 N10 31.0(8) . . . . ? O31 La2 O27 N10 -129.3(6) . . . . ? O33 La2 O27 N10 126.1(6) . . . . ? O29 N11 O28 La2 -172.0(7) . . . . ? O30 N11 O28 La2 9.0(7) . . . . ? O10 La2 O28 N11 8.4(5) . . . . ? O15 La2 O28 N11 -146.9(5) 2_756 . . . ? O11 La2 O28 N11 166.3(4) . . . . ? O25 La2 O28 N11 79.3(4) . . . . ? O30 La2 O28 N11 -5.5(4) . . . . ? O31 La2 O28 N11 -115.2(4) . . . . ? O33 La2 O28 N11 -68.8(4) . . . . ? O27 La2 O28 N11 95.5(4) . . . . ? O29 N11 O30 La2 172.0(7) . . . . ? O28 N11 O30 La2 -9.0(7) . . . . ? O10 La2 O30 N11 -161.6(5) . . . . ? O15 La2 O30 N11 158.5(4) 2_756 . . . ? O11 La2 O30 N11 -4.4(5) . . . . ? O25 La2 O30 N11 -72.3(4) . . . . ? O28 La2 O30 N11 5.4(4) . . . . ? O31 La2 O30 N11 72.0(4) . . . . ? O33 La2 O30 N11 115.2(4) . . . . ? O27 La2 O30 N11 -98.0(5) . . . . ? O32 N12 O31 La2 178.1(6) . . . . ? O33 N12 O31 La2 2.2(6) . . . . ? O10 La2 O31 N12 -10.7(5) . . . . ? O15 La2 O31 N12 -88.2(4) 2_756 . . . ? O11 La2 O31 N12 -176.6(5) . . . . ? O25 La2 O31 N12 126.5(4) . . . . ? O28 La2 O31 N12 103.7(5) . . . . ? O30 La2 O31 N12 58.9(5) . . . . ? O33 La2 O31 N12 -1.3(4) . . . . ? O27 La2 O31 N12 -139.0(5) . . . . ? O32 N12 O33 La2 -178.2(6) . . . . ? O31 N12 O33 La2 -2.1(6) . . . . ? O10 La2 O33 N12 173.5(4) . . . . ? O15 La2 O33 N12 88.8(4) 2_756 . . . ? O11 La2 O33 N12 6.8(5) . . . . ? O25 La2 O33 N12 -125.1(4) . . . . ? O28 La2 O33 N12 -68.6(4) . . . . ? O30 La2 O33 N12 -113.1(4) . . . . ? O31 La2 O33 N12 1.3(4) . . . . ? O27 La2 O33 N12 139.4(4) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.422 _refine_diff_density_min -0.378 _refine_diff_density_rms 0.053 #===END data_compound12 _database_code_depnum_ccdc_archive 'CCDC 817220' #TrackingRef '- 1-12.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H54 Er N6 O18' _chemical_formula_weight 1206.26 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' Er Er -0.2586 4.9576 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.3947(5) _cell_length_b 15.8766(6) _cell_length_c 17.5415(7) _cell_angle_alpha 78.8930(10) _cell_angle_beta 87.493(2) _cell_angle_gamma 76.8540(10) _cell_volume 3032.4(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5924 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 22.87 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.321 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1228 _exptl_absorpt_coefficient_mu 1.453 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.730 _exptl_absorpt_correction_T_max 0.746 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 15968 _diffrn_reflns_av_R_equivalents 0.0192 _diffrn_reflns_av_sigmaI/netI 0.0460 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 25.50 _reflns_number_total 11152 _reflns_number_gt 8828 _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. Diffuse electron densities resulting from residual disorder solvent moleculeswere removed from the data set using the SQUEEZE routine of PLATON andrefined further using the data generated. ; # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.500 0.158 0.000 673.4 67.7 _platon_squeeze_details ; ; _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^)+(0.0372P)^2^+1.6801P] 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 11152 _refine_ls_number_parameters 607 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0554 _refine_ls_R_factor_gt 0.0393 _refine_ls_wR_factor_ref 0.0928 _refine_ls_wR_factor_gt 0.0877 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _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 Er1 Er 0.159313(18) 0.701401(13) 0.251316(11) 0.05143(8) Uani 1 1 d . . . C1 C 0.0708(5) 0.5620(2) -0.0686(2) 0.110(2) Uani 1 1 d G . . H1 H 0.1472 0.5252 -0.0617 0.132 Uiso 1 1 calc R . . C2 C -0.0130(6) 0.5446(3) -0.1152(2) 0.149(4) Uani 1 1 d G . . H2 H 0.0073 0.4961 -0.1394 0.179 Uiso 1 1 calc R . . C3 C -0.1272(6) 0.5997(5) -0.1254(3) 0.164(5) Uani 1 1 d G . . H3 H -0.1833 0.5880 -0.1566 0.197 Uiso 1 1 calc R . . C4 C -0.1576(4) 0.6722(4) -0.0891(3) 0.168(4) Uani 1 1 d G . . H4 H -0.2340 0.7090 -0.0959 0.201 Uiso 1 1 calc R . . C5 C -0.0737(5) 0.6896(3) -0.0425(3) 0.120(2) Uani 1 1 d G . . H5 H -0.0940 0.7381 -0.0182 0.145 Uiso 1 1 calc R . . C6 C 0.0405(4) 0.6345(3) -0.03226(19) 0.0795(16) Uani 1 1 d G . . C7 C 0.1268(5) 0.6518(3) 0.0207(3) 0.0818(15) Uani 1 1 d . . . H7A H 0.0990 0.6395 0.0739 0.098 Uiso 1 1 calc R . . H7B H 0.2050 0.6128 0.0168 0.098 Uiso 1 1 calc R . . C8 C 0.1534(4) 0.7905(3) 0.0526(2) 0.0531(10) Uani 1 1 d . . . C9 C 0.1584(3) 0.88483(14) 0.02590(15) 0.0514(10) Uani 1 1 d G . . C10 C 0.1855(3) 0.92715(19) 0.08303(12) 0.0668(12) Uani 1 1 d G . . H10 H 0.1984 0.8968 0.1339 0.080 Uiso 1 1 calc R . . C11 C 0.1933(3) 1.01484(19) 0.06407(18) 0.0779(14) Uani 1 1 d G . . H11 H 0.2114 1.0432 0.1023 0.093 Uiso 1 1 calc R . . C12 C 0.1740(3) 1.06021(14) -0.0120(2) 0.0834(15) Uani 1 1 d G . . H12 H 0.1792 1.1189 -0.0247 0.100 Uiso 1 1 calc R . . C13 C 0.1469(3) 1.01788(18) -0.06916(14) 0.0762(14) Uani 1 1 d G . . H13 H 0.1340 1.0482 -0.1201 0.091 Uiso 1 1 calc R . . C14 C 0.1391(3) 0.93019(18) -0.05020(13) 0.0580(11) Uani 1 1 d G . . C15 C 0.0952(5) 0.9294(3) -0.1829(3) 0.0807(15) Uani 1 1 d . . . H15A H 0.1713 0.9403 -0.2046 0.097 Uiso 1 1 calc R . . H15B H 0.0370 0.9853 -0.1878 0.097 Uiso 1 1 calc R . . C16 C 0.0518(5) 0.8685(3) -0.2238(3) 0.0811(15) Uani 1 1 d . . . H16A H -0.0218 0.8554 -0.1997 0.097 Uiso 1 1 calc R . . H16B H 0.0342 0.8963 -0.2776 0.097 Uiso 1 1 calc R . . C17 C 0.1005(5) 0.7269(4) -0.2540(3) 0.0819(15) Uani 1 1 d . . . H17A H 0.0848 0.7494 -0.3089 0.098 Uiso 1 1 calc R . . H17B H 0.0261 0.7161 -0.2293 0.098 Uiso 1 1 calc R . . C18 C 0.5469(7) 0.9583(5) 0.5003(5) 0.132(3) Uani 1 1 d . . . H18A H 0.6181 0.9596 0.5280 0.158 Uiso 1 1 calc R . . H18B H 0.5160 0.9079 0.5258 0.158 Uiso 1 1 calc R . . C19 C 0.6593(7) 0.8739(5) 0.4190(5) 0.139(3) Uani 1 1 d . . . H19A H 0.6253 0.8244 0.4428 0.167 Uiso 1 1 calc R . . H19B H 0.7309 0.8718 0.4479 0.167 Uiso 1 1 calc R . . C20 C 0.6919(6) 0.8681(5) 0.3364(5) 0.125(3) Uani 1 1 d . . . H20A H 0.7208 0.9194 0.3110 0.150 Uiso 1 1 calc R . . H20B H 0.7544 0.8158 0.3338 0.150 Uiso 1 1 calc R . . C21 C 0.5899(3) 0.8264(2) 0.23685(19) 0.0764(14) Uani 1 1 d G . . C22 C 0.6965(2) 0.8000(3) 0.1975(2) 0.0894(16) Uani 1 1 d G . . H22 H 0.7675 0.8122 0.2120 0.107 Uiso 1 1 calc R . . C23 C 0.6969(3) 0.7554(3) 0.1367(2) 0.109(2) Uani 1 1 d G . . H23 H 0.7683 0.7377 0.1104 0.130 Uiso 1 1 calc R . . C24 C 0.5908(4) 0.7371(3) 0.1151(2) 0.116(2) Uani 1 1 d G . . H24 H 0.5911 0.7072 0.0744 0.139 Uiso 1 1 calc R . . C25 C 0.4842(3) 0.7635(3) 0.1544(2) 0.0927(17) Uani 1 1 d G . . H25 H 0.4132 0.7512 0.1400 0.111 Uiso 1 1 calc R . . C26 C 0.4838(2) 0.8081(2) 0.21528(19) 0.0662(12) Uani 1 1 d G . . C27 C 0.3657(4) 0.8341(3) 0.2543(3) 0.0648(12) Uani 1 1 d . . . C28 C 0.2371(5) 0.9443(4) 0.3211(4) 0.0899(16) Uani 1 1 d . . . H28A H 0.1713 0.9254 0.3012 0.108 Uiso 1 1 calc R . . H28B H 0.2234 1.0077 0.3049 0.108 Uiso 1 1 calc R . . C29 C 0.2362(3) 0.9220(2) 0.4086(2) 0.0856(16) Uani 1 1 d G . . C30 C 0.1569(3) 0.97912(17) 0.4480(2) 0.140(3) Uani 1 1 d G . . H30 H 0.1083 1.0301 0.4204 0.168 Uiso 1 1 calc R . . C31 C 0.1502(3) 0.9600(2) 0.5286(2) 0.168(4) Uani 1 1 d G . . H31 H 0.0971 0.9983 0.5549 0.202 Uiso 1 1 calc R . . C32 C 0.2228(3) 0.8838(2) 0.56975(19) 0.135(3) Uani 1 1 d G . . H32 H 0.2184 0.8710 0.6237 0.162 Uiso 1 1 calc R . . C33 C 0.3022(2) 0.8266(2) 0.5303(2) 0.149(3) Uani 1 1 d G . . H33 H 0.3508 0.7756 0.5579 0.178 Uiso 1 1 calc R . . C34 C 0.3089(3) 0.8457(2) 0.4498(2) 0.119(2) Uani 1 1 d G . . H34 H 0.3619 0.8075 0.4234 0.142 Uiso 1 1 calc R . . C35 C -0.0146(2) 0.72868(17) 0.52926(13) 0.0984(19) Uani 1 1 d G . . H35 H 0.0206 0.7620 0.4891 0.118 Uiso 1 1 calc R . . C36 C -0.1032(2) 0.7702(2) 0.57520(19) 0.134(3) Uani 1 1 d G . . H36 H -0.1272 0.8313 0.5658 0.161 Uiso 1 1 calc R . . C37 C -0.1558(3) 0.7203(3) 0.6352(2) 0.151(4) Uani 1 1 d G . . H37 H -0.2150 0.7481 0.6659 0.181 Uiso 1 1 calc R . . C38 C -0.1199(3) 0.6290(3) 0.64919(16) 0.158(4) Uani 1 1 d G . . H38 H -0.1551 0.5957 0.6893 0.190 Uiso 1 1 calc R . . C39 C -0.0314(3) 0.5875(2) 0.60325(17) 0.101(2) Uani 1 1 d G . . H39 H -0.0074 0.5264 0.6126 0.121 Uiso 1 1 calc R . . C40 C 0.0212(3) 0.63734(17) 0.54328(16) 0.0644(12) Uani 1 1 d G . . C41 C 0.1075(5) 0.5947(4) 0.4899(3) 0.0852(16) Uani 1 1 d . . . H41A H 0.1120 0.5318 0.5022 0.102 Uiso 1 1 calc R . . H41B H 0.0765 0.6158 0.4374 0.102 Uiso 1 1 calc R . . C42 C 0.2987(4) 0.6211(3) 0.4305(2) 0.0536(10) Uani 1 1 d . . . C43 C 0.4282(2) 0.62221(18) 0.44018(16) 0.0520(10) Uani 1 1 d G . . C44 C 0.4930(3) 0.63393(19) 0.37141(13) 0.0626(11) Uani 1 1 d G . . H44 H 0.4553 0.6404 0.3240 0.075 Uiso 1 1 calc R . . C45 C 0.6140(3) 0.6360(2) 0.37348(17) 0.0738(13) Uani 1 1 d G . . H45 H 0.6574 0.6439 0.3275 0.089 Uiso 1 1 calc R . . C46 C 0.6704(2) 0.6264(2) 0.4443(2) 0.0825(15) Uani 1 1 d G . . H46 H 0.7514 0.6278 0.4457 0.099 Uiso 1 1 calc R . . C47 C 0.6057(3) 0.6147(2) 0.51309(16) 0.0738(13) Uani 1 1 d G . . H47 H 0.6434 0.6083 0.5605 0.089 Uiso 1 1 calc R . . C48 C 0.4846(3) 0.61260(19) 0.51102(13) 0.0590(11) Uani 1 1 d G . . C49 C 0.4736(5) 0.5878(4) 0.6507(3) 0.0786(15) Uani 1 1 d . . . H49A H 0.5025 0.6397 0.6549 0.094 Uiso 1 1 calc R . . H49B H 0.5413 0.5373 0.6578 0.094 Uiso 1 1 calc R . . C50 C 0.3795(5) 0.5740(4) 0.7099(3) 0.0834(16) Uani 1 1 d . . . H50A H 0.3441 0.5264 0.7014 0.100 Uiso 1 1 calc R . . H50B H 0.4148 0.5581 0.7615 0.100 Uiso 1 1 calc R . . C51 C 0.1939(5) 0.6430(4) 0.7562(3) 0.0880(16) Uani 1 1 d . . . H51A H 0.2239 0.6277 0.8091 0.106 Uiso 1 1 calc R . . H51B H 0.1588 0.5958 0.7465 0.106 Uiso 1 1 calc R . . N1 N 0.1385(4) 0.7435(2) 0.0011(2) 0.0704(11) Uani 1 1 d . . . H1A H 0.1354 0.7682 -0.0472 0.084 Uiso 1 1 calc R . . N2 N 0.3482(4) 0.9040(3) 0.2879(3) 0.0873(13) Uani 1 1 d . . . H2A H 0.4089 0.9273 0.2900 0.105 Uiso 1 1 calc R . . N3 N 0.2302(3) 0.6093(3) 0.4916(2) 0.0699(10) Uani 1 1 d . . . H3A H 0.2589 0.6102 0.5359 0.084 Uiso 1 1 calc R . . N4 N 0.3033(4) 0.5460(3) 0.2082(2) 0.0771(12) Uani 1 1 d . . . N5 N -0.0547(4) 0.6350(3) 0.2536(3) 0.0680(10) Uani 1 1 d . . . N6 N 0.0064(4) 0.8449(3) 0.3084(3) 0.0665(10) Uani 1 1 d . . . O1 O 0.1639(3) 0.7570(2) 0.12286(16) 0.0665(8) Uani 1 1 d . . . O2 O 0.1097(3) 0.88730(19) -0.10358(16) 0.0726(9) Uani 1 1 d . . . O3 O 0.1405(3) 0.7903(2) -0.22034(18) 0.0751(9) Uani 1 1 d . . . O4 O 0.5761(4) 0.9520(3) 0.4214(3) 0.1155(14) Uani 1 1 d . . . O5 O 0.5846(3) 0.8640(3) 0.3005(3) 0.1144(15) Uani 1 1 d . . . O6 O 0.2853(3) 0.7946(2) 0.25129(16) 0.0641(8) Uani 1 1 d . . . O7 O 0.2579(3) 0.62836(19) 0.36409(16) 0.0644(8) Uani 1 1 d . . . O8 O 0.4192(3) 0.5989(2) 0.57681(17) 0.0704(9) Uani 1 1 d . . . O9 O 0.2900(3) 0.6526(2) 0.70381(18) 0.0779(9) Uani 1 1 d . . . O10 O 0.3462(3) 0.6125(2) 0.20642(19) 0.0768(9) Uani 1 1 d . . . O11 O 0.1966(4) 0.5536(2) 0.2299(2) 0.0888(11) Uani 1 1 d . . . O12 O 0.3617(4) 0.4784(3) 0.1917(3) 0.1281(18) Uani 1 1 d . . . O13 O -0.0026(3) 0.6391(2) 0.3145(2) 0.0787(9) Uani 1 1 d . . . O14 O -0.1345(3) 0.5958(3) 0.2566(2) 0.0984(12) Uani 1 1 d . . . O15 O -0.0176(3) 0.6737(2) 0.1912(2) 0.0736(9) Uani 1 1 d . . . O16 O 0.0774(3) 0.7845(2) 0.35230(17) 0.0721(9) Uani 1 1 d . . . O17 O -0.0553(3) 0.9076(2) 0.3323(2) 0.0899(11) Uani 1 1 d . . . O18 O 0.0049(3) 0.8377(2) 0.23790(18) 0.0708(9) 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 Er1 0.05551(13) 0.05489(12) 0.04715(12) -0.01161(8) -0.00875(8) -0.01567(9) C1 0.210(8) 0.086(4) 0.060(3) -0.026(3) 0.030(4) -0.081(5) C2 0.285(13) 0.139(7) 0.076(5) -0.031(4) 0.023(6) -0.148(9) C3 0.243(12) 0.208(11) 0.095(6) -0.025(6) -0.011(7) -0.157(10) C4 0.122(7) 0.218(11) 0.177(9) -0.028(8) -0.026(6) -0.069(7) C5 0.113(6) 0.146(6) 0.121(6) -0.046(5) -0.004(5) -0.049(5) C6 0.125(5) 0.080(4) 0.052(3) -0.023(3) 0.014(3) -0.054(3) C7 0.121(5) 0.059(3) 0.071(3) -0.011(3) -0.011(3) -0.031(3) C8 0.053(3) 0.062(3) 0.049(2) -0.015(2) -0.007(2) -0.017(2) C9 0.052(2) 0.053(2) 0.053(2) -0.016(2) -0.0010(19) -0.013(2) C10 0.071(3) 0.071(3) 0.065(3) -0.019(2) -0.006(2) -0.025(3) C11 0.088(4) 0.069(3) 0.093(4) -0.037(3) 0.004(3) -0.032(3) C12 0.096(4) 0.058(3) 0.100(4) -0.016(3) 0.009(3) -0.025(3) C13 0.100(4) 0.057(3) 0.068(3) -0.006(2) 0.012(3) -0.017(3) C14 0.062(3) 0.057(3) 0.054(3) -0.012(2) 0.002(2) -0.011(2) C15 0.121(5) 0.062(3) 0.047(3) -0.002(2) 0.000(3) -0.004(3) C16 0.094(4) 0.087(4) 0.050(3) -0.010(3) -0.011(3) 0.004(3) C17 0.081(4) 0.107(4) 0.070(3) -0.036(3) 0.004(3) -0.030(3) C18 0.132(7) 0.132(6) 0.149(7) -0.061(6) -0.036(6) -0.029(5) C19 0.130(6) 0.137(7) 0.160(8) -0.074(6) -0.052(6) -0.002(5) C20 0.080(4) 0.137(6) 0.177(7) -0.059(5) -0.045(5) -0.028(4) C21 0.062(3) 0.077(3) 0.091(4) -0.012(3) -0.007(3) -0.017(3) C22 0.069(4) 0.092(4) 0.105(5) -0.011(3) 0.001(3) -0.020(3) C23 0.085(5) 0.133(6) 0.101(5) -0.008(4) 0.022(4) -0.026(4) C24 0.101(5) 0.171(7) 0.092(4) -0.052(4) 0.025(4) -0.043(5) C25 0.080(4) 0.136(5) 0.076(4) -0.040(4) 0.014(3) -0.038(4) C26 0.063(3) 0.071(3) 0.068(3) -0.008(2) -0.006(2) -0.023(2) C27 0.069(3) 0.066(3) 0.062(3) -0.010(2) -0.012(2) -0.019(3) C28 0.080(4) 0.081(4) 0.113(5) -0.033(3) 0.003(3) -0.016(3) C29 0.076(4) 0.078(4) 0.119(5) -0.044(4) 0.008(3) -0.031(3) C30 0.121(6) 0.153(7) 0.156(7) -0.096(6) 0.004(5) 0.003(5) C31 0.152(8) 0.225(11) 0.151(8) -0.111(8) 0.017(7) -0.028(7) C32 0.142(7) 0.170(8) 0.117(6) -0.040(6) 0.018(5) -0.076(6) C33 0.235(10) 0.106(6) 0.105(6) -0.030(5) 0.015(6) -0.033(6) C34 0.165(7) 0.073(4) 0.114(5) -0.026(4) 0.001(5) -0.011(4) C35 0.133(6) 0.085(4) 0.064(3) -0.002(3) -0.002(3) -0.007(4) C36 0.140(7) 0.138(6) 0.104(5) -0.035(5) -0.036(5) 0.026(5) C37 0.087(5) 0.260(12) 0.133(7) -0.103(8) 0.004(5) -0.042(7) C38 0.188(9) 0.279(12) 0.075(4) -0.068(6) 0.061(5) -0.171(9) C39 0.149(6) 0.114(5) 0.058(3) -0.006(3) -0.001(4) -0.074(4) C40 0.063(3) 0.087(4) 0.046(2) -0.003(2) -0.008(2) -0.031(3) C41 0.072(4) 0.106(4) 0.088(4) -0.029(3) -0.003(3) -0.032(3) C42 0.066(3) 0.047(2) 0.044(2) -0.0088(19) -0.006(2) -0.004(2) C43 0.057(3) 0.043(2) 0.053(2) -0.0111(19) -0.010(2) -0.0013(19) C44 0.066(3) 0.058(3) 0.056(3) -0.005(2) -0.002(2) -0.004(2) C45 0.065(3) 0.070(3) 0.076(3) -0.005(3) 0.009(3) -0.003(3) C46 0.055(3) 0.075(3) 0.113(5) -0.011(3) -0.003(3) -0.009(3) C47 0.065(3) 0.075(3) 0.080(3) -0.017(3) -0.018(3) -0.008(3) C48 0.063(3) 0.052(3) 0.060(3) -0.012(2) -0.012(2) -0.005(2) C49 0.081(4) 0.096(4) 0.056(3) -0.023(3) -0.018(3) -0.004(3) C50 0.105(4) 0.082(4) 0.055(3) -0.017(3) -0.016(3) 0.001(3) C51 0.108(5) 0.094(4) 0.072(3) -0.033(3) 0.015(3) -0.032(4) N1 0.112(3) 0.058(2) 0.047(2) -0.0090(18) -0.015(2) -0.028(2) N2 0.071(3) 0.085(3) 0.123(4) -0.047(3) 0.010(3) -0.032(2) N3 0.063(3) 0.092(3) 0.058(2) -0.017(2) -0.009(2) -0.020(2) N4 0.077(3) 0.076(3) 0.082(3) -0.038(2) -0.030(2) 0.003(3) N5 0.054(2) 0.068(3) 0.087(3) -0.022(2) -0.010(2) -0.016(2) N6 0.062(3) 0.064(3) 0.077(3) -0.024(2) 0.009(2) -0.015(2) O1 0.089(2) 0.075(2) 0.0450(17) -0.0104(15) -0.0127(15) -0.0350(17) O2 0.115(3) 0.0602(19) 0.0429(16) -0.0064(14) -0.0081(17) -0.0207(18) O3 0.082(2) 0.082(2) 0.0619(19) -0.0243(17) -0.0089(17) -0.0094(19) O4 0.119(4) 0.107(3) 0.135(4) -0.049(3) -0.026(3) -0.026(3) O5 0.073(3) 0.150(4) 0.144(4) -0.079(3) -0.022(2) -0.029(2) O6 0.066(2) 0.076(2) 0.0629(19) -0.0201(16) -0.0058(15) -0.0334(17) O7 0.069(2) 0.071(2) 0.0510(17) -0.0116(15) -0.0133(15) -0.0086(16) O8 0.067(2) 0.097(2) 0.0485(17) -0.0200(16) -0.0100(15) -0.0136(18) O9 0.091(3) 0.078(2) 0.063(2) -0.0196(17) 0.0033(19) -0.011(2) O10 0.079(2) 0.083(2) 0.075(2) -0.0297(19) 0.0019(18) -0.0193(19) O11 0.072(3) 0.070(2) 0.134(3) -0.040(2) -0.011(2) -0.0149(19) O12 0.093(3) 0.105(3) 0.195(5) -0.094(3) -0.038(3) 0.022(3) O13 0.073(2) 0.097(3) 0.073(2) -0.0141(19) -0.0037(18) -0.0359(19) O14 0.071(2) 0.101(3) 0.137(3) -0.027(2) -0.006(2) -0.042(2) O15 0.066(2) 0.089(2) 0.071(2) -0.0143(19) -0.0105(17) -0.0259(18) O16 0.094(3) 0.065(2) 0.0520(18) -0.0099(16) 0.0005(17) -0.0075(19) O17 0.088(3) 0.082(2) 0.099(3) -0.038(2) 0.007(2) -0.004(2) O18 0.080(2) 0.070(2) 0.061(2) -0.0207(16) -0.0156(17) -0.0023(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Er1 O1 2.259(3) . ? Er1 O6 2.284(3) . ? Er1 O7 2.288(3) . ? Er1 O11 2.387(3) . ? Er1 O13 2.417(3) . ? Er1 O18 2.438(3) . ? Er1 O16 2.438(3) . ? Er1 O10 2.462(3) . ? Er1 O15 2.477(3) . ? C1 C2 1.3900 . ? C1 C6 1.3900 . ? C1 H1 0.9300 . ? C2 C3 1.3900 . ? C2 H2 0.9300 . ? C3 C4 1.3900 . ? C3 H3 0.9300 . ? C4 C5 1.3900 . ? C4 H4 0.9300 . ? C5 C6 1.3900 . ? C5 H5 0.9300 . ? C6 C7 1.486(6) . ? C7 N1 1.465(5) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 O1 1.243(5) . ? C8 N1 1.317(5) . ? C8 C9 1.495(5) . ? C9 C10 1.3900 . ? C9 C14 1.3900 . ? C10 C11 1.3900 . ? C10 H10 0.9300 . ? C11 C12 1.3900 . ? C11 H11 0.9300 . ? C12 C13 1.3900 . ? C12 H12 0.9300 . ? C13 C14 1.3900 . ? C13 H13 0.9300 . ? C14 O2 1.352(3) . ? C15 O2 1.422(5) . ? C15 C16 1.487(7) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 O3 1.406(6) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 O3 1.425(5) . ? C17 C51 1.490(8) 1_554 ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 O4 1.425(9) . ? C18 C18 1.501(13) 2_676 ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 O4 1.386(8) . ? C19 C20 1.495(10) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 O5 1.420(6) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 O5 1.357(5) . ? C21 C22 1.3900 . ? C21 C26 1.3900 . ? C22 C23 1.3900 . ? C22 H22 0.9300 . ? C23 C24 1.3900 . ? C23 H23 0.9300 . ? C24 C25 1.3900 . ? C24 H24 0.9300 . ? C25 C26 1.3900 . ? C25 H25 0.9300 . ? C26 C27 1.491(6) . ? C27 O6 1.230(5) . ? C27 N2 1.326(6) . ? C28 N2 1.436(6) . ? C28 C29 1.507(7) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C30 1.3900 . ? C29 C34 1.3900 . ? C30 C31 1.3900 . ? C30 H30 0.9300 . ? C31 C32 1.3900 . ? C31 H31 0.9300 . ? C32 C33 1.3900 . ? C32 H32 0.9300 . ? C33 C34 1.3900 . ? C33 H33 0.9300 . ? C34 H34 0.9300 . ? C35 C36 1.3900 . ? C35 C40 1.3900 . ? C35 H35 0.9300 . ? C36 C37 1.3900 . ? C36 H36 0.9300 . ? C37 C38 1.3900 . ? C37 H37 0.9300 . ? C38 C39 1.3900 . ? C38 H38 0.9300 . ? C39 C40 1.3900 . ? C39 H39 0.9300 . ? C40 C41 1.470(6) . ? C41 N3 1.470(6) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 O7 1.248(4) . ? C42 N3 1.308(5) . ? C42 C43 1.498(5) . ? C43 C44 1.3900 . ? C43 C48 1.3900 . ? C44 C45 1.3900 . ? C44 H44 0.9300 . ? C45 C46 1.3900 . ? C45 H45 0.9300 . ? C46 C47 1.3900 . ? C46 H46 0.9300 . ? C47 C48 1.3900 . ? C47 H47 0.9300 . ? C48 O8 1.355(4) . ? C49 O8 1.424(5) . ? C49 C50 1.484(7) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 O9 1.411(6) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C51 O9 1.414(6) . ? C51 C17 1.490(8) 1_556 ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? N1 H1A 0.8600 . ? N2 H2A 0.8600 . ? N3 H3A 0.8600 . ? N4 O12 1.207(5) . ? N4 O11 1.245(5) . ? N4 O10 1.254(5) . ? N5 O14 1.207(5) . ? N5 O15 1.253(5) . ? N5 O13 1.266(5) . ? N6 O17 1.216(5) . ? N6 O16 1.259(5) . ? N6 O18 1.265(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Er1 O6 79.90(10) . . ? O1 Er1 O7 149.99(12) . . ? O6 Er1 O7 83.60(11) . . ? O1 Er1 O11 92.49(13) . . ? O6 Er1 O11 131.54(13) . . ? O7 Er1 O11 79.95(12) . . ? O1 Er1 O13 123.95(11) . . ? O6 Er1 O13 147.80(11) . . ? O7 Er1 O13 81.95(11) . . ? O11 Er1 O13 73.57(13) . . ? O1 Er1 O18 77.27(11) . . ? O6 Er1 O18 82.70(11) . . ? O7 Er1 O18 125.26(10) . . ? O11 Er1 O18 142.46(12) . . ? O13 Er1 O18 82.45(12) . . ? O1 Er1 O16 125.81(11) . . ? O6 Er1 O16 76.02(11) . . ? O7 Er1 O16 73.10(11) . . ? O11 Er1 O16 138.79(13) . . ? O13 Er1 O16 72.29(11) . . ? O18 Er1 O16 52.17(10) . . ? O1 Er1 O10 76.29(12) . . ? O6 Er1 O10 80.27(12) . . ? O7 Er1 O10 76.33(11) . . ? O11 Er1 O10 51.63(12) . . ? O13 Er1 O10 123.41(12) . . ? O18 Er1 O10 150.61(12) . . ? O16 Er1 O10 142.94(12) . . ? O1 Er1 O15 72.54(11) . . ? O6 Er1 O15 146.78(11) . . ? O7 Er1 O15 129.13(11) . . ? O11 Er1 O15 68.92(12) . . ? O13 Er1 O15 51.62(11) . . ? O18 Er1 O15 73.56(11) . . ? O16 Er1 O15 105.46(12) . . ? O10 Er1 O15 109.96(11) . . ? C2 C1 C6 120.0 . . ? C2 C1 H1 120.0 . . ? C6 C1 H1 120.0 . . ? C1 C2 C3 120.0 . . ? C1 C2 H2 120.0 . . ? C3 C2 H2 120.0 . . ? C4 C3 C2 120.0 . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C4 C5 120.0 . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C6 C5 C4 120.0 . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C5 C6 C1 120.0 . . ? C5 C6 C7 119.2(4) . . ? C1 C6 C7 120.7(4) . . ? N1 C7 C6 110.9(4) . . ? N1 C7 H7A 109.5 . . ? C6 C7 H7A 109.5 . . ? N1 C7 H7B 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 108.1 . . ? O1 C8 N1 120.7(4) . . ? O1 C8 C9 120.0(3) . . ? N1 C8 C9 119.3(3) . . ? C10 C9 C14 120.0 . . ? C10 C9 C8 115.5(2) . . ? C14 C9 C8 124.5(2) . . ? C11 C10 C9 120.0 . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C10 C11 C12 120.0 . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? C13 C12 C11 120.0 . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C12 C13 C14 120.0 . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? O2 C14 C13 121.9(2) . . ? O2 C14 C9 118.1(2) . . ? C13 C14 C9 120.0 . . ? O2 C15 C16 106.4(4) . . ? O2 C15 H15A 110.4 . . ? C16 C15 H15A 110.4 . . ? O2 C15 H15B 110.4 . . ? C16 C15 H15B 110.4 . . ? H15A C15 H15B 108.6 . . ? O3 C16 C15 109.6(4) . . ? O3 C16 H16A 109.7 . . ? C15 C16 H16A 109.7 . . ? O3 C16 H16B 109.7 . . ? C15 C16 H16B 109.7 . . ? H16A C16 H16B 108.2 . . ? O3 C17 C51 110.2(5) . 1_554 ? O3 C17 H17A 109.6 . . ? C51 C17 H17A 109.6 1_554 . ? O3 C17 H17B 109.6 . . ? C51 C17 H17B 109.6 1_554 . ? H17A C17 H17B 108.1 . . ? O4 C18 C18 107.3(9) . 2_676 ? O4 C18 H18A 110.2 . . ? C18 C18 H18A 110.2 2_676 . ? O4 C18 H18B 110.2 . . ? C18 C18 H18B 110.2 2_676 . ? H18A C18 H18B 108.5 . . ? O4 C19 C20 109.4(7) . . ? O4 C19 H19A 109.8 . . ? C20 C19 H19A 109.8 . . ? O4 C19 H19B 109.8 . . ? C20 C19 H19B 109.8 . . ? H19A C19 H19B 108.2 . . ? O5 C20 C19 105.9(6) . . ? O5 C20 H20A 110.6 . . ? C19 C20 H20A 110.6 . . ? O5 C20 H20B 110.6 . . ? C19 C20 H20B 110.6 . . ? H20A C20 H20B 108.7 . . ? O5 C21 C22 123.1(3) . . ? O5 C21 C26 116.7(3) . . ? C22 C21 C26 120.0 . . ? C23 C22 C21 120.0 . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C22 C23 C24 120.0 . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C23 C24 C25 120.0 . . ? C23 C24 H24 120.0 . . ? C25 C24 H24 120.0 . . ? C26 C25 C24 120.0 . . ? C26 C25 H25 120.0 . . ? C24 C25 H25 120.0 . . ? C25 C26 C21 120.0 . . ? C25 C26 C27 116.6(3) . . ? C21 C26 C27 123.4(3) . . ? O6 C27 N2 121.5(5) . . ? O6 C27 C26 120.5(4) . . ? N2 C27 C26 117.9(4) . . ? N2 C28 C29 113.0(5) . . ? N2 C28 H28A 109.0 . . ? C29 C28 H28A 109.0 . . ? N2 C28 H28B 109.0 . . ? C29 C28 H28B 109.0 . . ? H28A C28 H28B 107.8 . . ? C30 C29 C34 120.0 . . ? C30 C29 C28 117.9(3) . . ? C34 C29 C28 122.1(3) . . ? C31 C30 C29 120.0 . . ? C31 C30 H30 120.0 . . ? C29 C30 H30 120.0 . . ? C30 C31 C32 120.0 . . ? C30 C31 H31 120.0 . . ? C32 C31 H31 120.0 . . ? C33 C32 C31 120.0 . . ? C33 C32 H32 120.0 . . ? C31 C32 H32 120.0 . . ? C32 C33 C34 120.0 . . ? C32 C33 H33 120.0 . . ? C34 C33 H33 120.0 . . ? C33 C34 C29 120.0 . . ? C33 C34 H34 120.0 . . ? C29 C34 H34 120.0 . . ? C36 C35 C40 120.0 . . ? C36 C35 H35 120.0 . . ? C40 C35 H35 120.0 . . ? C35 C36 C37 120.0 . . ? C35 C36 H36 120.0 . . ? C37 C36 H36 120.0 . . ? C38 C37 C36 120.0 . . ? C38 C37 H37 120.0 . . ? C36 C37 H37 120.0 . . ? C37 C38 C39 120.0 . . ? C37 C38 H38 120.0 . . ? C39 C38 H38 120.0 . . ? C38 C39 C40 120.0 . . ? C38 C39 H39 120.0 . . ? C40 C39 H39 120.0 . . ? C39 C40 C35 120.0 . . ? C39 C40 C41 120.9(3) . . ? C35 C40 C41 119.0(3) . . ? N3 C41 C40 115.3(4) . . ? N3 C41 H41A 108.4 . . ? C40 C41 H41A 108.4 . . ? N3 C41 H41B 108.4 . . ? C40 C41 H41B 108.4 . . ? H41A C41 H41B 107.5 . . ? O7 C42 N3 120.3(4) . . ? O7 C42 C43 119.7(4) . . ? N3 C42 C43 119.9(3) . . ? C44 C43 C48 120.0 . . ? C44 C43 C42 115.0(2) . . ? C48 C43 C42 125.0(2) . . ? C45 C44 C43 120.0 . . ? C45 C44 H44 120.0 . . ? C43 C44 H44 120.0 . . ? C44 C45 C46 120.0 . . ? C44 C45 H45 120.0 . . ? C46 C45 H45 120.0 . . ? C47 C46 C45 120.0 . . ? C47 C46 H46 120.0 . . ? C45 C46 H46 120.0 . . ? C48 C47 C46 120.0 . . ? C48 C47 H47 120.0 . . ? C46 C47 H47 120.0 . . ? O8 C48 C47 121.8(2) . . ? O8 C48 C43 118.1(2) . . ? C47 C48 C43 120.0 . . ? O8 C49 C50 106.7(4) . . ? O8 C49 H49A 110.4 . . ? C50 C49 H49A 110.4 . . ? O8 C49 H49B 110.4 . . ? C50 C49 H49B 110.4 . . ? H49A C49 H49B 108.6 . . ? O9 C50 C49 108.6(4) . . ? O9 C50 H50A 110.0 . . ? C49 C50 H50A 110.0 . . ? O9 C50 H50B 110.0 . . ? C49 C50 H50B 110.0 . . ? H50A C50 H50B 108.4 . . ? O9 C51 C17 109.7(5) . 1_556 ? O9 C51 H51A 109.7 . . ? C17 C51 H51A 109.7 1_556 . ? O9 C51 H51B 109.7 . . ? C17 C51 H51B 109.7 1_556 . ? H51A C51 H51B 108.2 . . ? C8 N1 C7 124.1(4) . . ? C8 N1 H1A 117.9 . . ? C7 N1 H1A 117.9 . . ? C27 N2 C28 125.9(4) . . ? C27 N2 H2A 117.0 . . ? C28 N2 H2A 117.0 . . ? C42 N3 C41 124.6(4) . . ? C42 N3 H3A 117.7 . . ? C41 N3 H3A 117.7 . . ? O12 N4 O11 121.8(5) . . ? O12 N4 O10 122.7(5) . . ? O11 N4 O10 115.5(4) . . ? O14 N5 O15 123.3(4) . . ? O14 N5 O13 121.1(5) . . ? O15 N5 O13 115.6(4) . . ? O17 N6 O16 121.6(4) . . ? O17 N6 O18 122.1(4) . . ? O16 N6 O18 116.3(4) . . ? C8 O1 Er1 173.2(3) . . ? C14 O2 C15 120.2(3) . . ? C16 O3 C17 112.1(4) . . ? C19 O4 C18 109.3(6) . . ? C21 O5 C20 120.5(5) . . ? C27 O6 Er1 170.9(3) . . ? C42 O7 Er1 155.6(3) . . ? C48 O8 C49 120.0(3) . . ? C50 O9 C51 111.7(4) . . ? N4 O10 Er1 94.5(3) . . ? N4 O11 Er1 98.4(3) . . ? N5 O13 Er1 97.2(3) . . ? N5 O15 Er1 94.6(2) . . ? N6 O16 Er1 95.8(3) . . ? N6 O18 Er1 95.7(3) . . ? 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 0.0 . . . . ? C1 C2 C3 C4 0.0 . . . . ? C2 C3 C4 C5 0.0 . . . . ? C3 C4 C5 C6 0.0 . . . . ? C4 C5 C6 C1 0.0 . . . . ? C4 C5 C6 C7 -177.1(4) . . . . ? C2 C1 C6 C5 0.0 . . . . ? C2 C1 C6 C7 177.0(4) . . . . ? C5 C6 C7 N1 -52.1(5) . . . . ? C1 C6 C7 N1 130.9(4) . . . . ? O1 C8 C9 C10 5.3(5) . . . . ? N1 C8 C9 C10 -174.2(3) . . . . ? O1 C8 C9 C14 -175.2(3) . . . . ? N1 C8 C9 C14 5.2(5) . . . . ? C14 C9 C10 C11 0.0 . . . . ? C8 C9 C10 C11 179.5(3) . . . . ? C9 C10 C11 C12 0.0 . . . . ? C10 C11 C12 C13 0.0 . . . . ? C11 C12 C13 C14 0.0 . . . . ? C12 C13 C14 O2 178.2(3) . . . . ? C12 C13 C14 C9 0.0 . . . . ? C10 C9 C14 O2 -178.2(3) . . . . ? C8 C9 C14 O2 2.3(4) . . . . ? C10 C9 C14 C13 0.0 . . . . ? C8 C9 C14 C13 -179.4(3) . . . . ? O2 C15 C16 O3 -63.9(5) . . . . ? O4 C19 C20 O5 -64.3(8) . . . . ? O5 C21 C22 C23 174.7(4) . . . . ? C26 C21 C22 C23 0.0 . . . . ? C21 C22 C23 C24 0.0 . . . . ? C22 C23 C24 C25 0.0 . . . . ? C23 C24 C25 C26 0.0 . . . . ? C24 C25 C26 C21 0.0 . . . . ? C24 C25 C26 C27 179.9(3) . . . . ? O5 C21 C26 C25 -175.0(4) . . . . ? C22 C21 C26 C25 0.0 . . . . ? O5 C21 C26 C27 5.0(4) . . . . ? C22 C21 C26 C27 -179.9(4) . . . . ? C25 C26 C27 O6 23.2(5) . . . . ? C21 C26 C27 O6 -156.9(3) . . . . ? C25 C26 C27 N2 -152.9(4) . . . . ? C21 C26 C27 N2 27.1(5) . . . . ? N2 C28 C29 C30 157.1(3) . . . . ? N2 C28 C29 C34 -24.8(5) . . . . ? C34 C29 C30 C31 0.0 . . . . ? C28 C29 C30 C31 178.1(3) . . . . ? C29 C30 C31 C32 0.0 . . . . ? C30 C31 C32 C33 0.0 . . . . ? C31 C32 C33 C34 0.0 . . . . ? C32 C33 C34 C29 0.0 . . . . ? C30 C29 C34 C33 0.0 . . . . ? C28 C29 C34 C33 -178.0(3) . . . . ? C40 C35 C36 C37 0.0 . . . . ? C35 C36 C37 C38 0.0 . . . . ? C36 C37 C38 C39 0.0 . . . . ? C37 C38 C39 C40 0.0 . . . . ? C38 C39 C40 C35 0.0 . . . . ? C38 C39 C40 C41 -174.8(3) . . . . ? C36 C35 C40 C39 0.0 . . . . ? C36 C35 C40 C41 174.9(3) . . . . ? C39 C40 C41 N3 -117.0(4) . . . . ? C35 C40 C41 N3 68.2(5) . . . . ? O7 C42 C43 C44 1.6(4) . . . . ? N3 C42 C43 C44 179.1(3) . . . . ? O7 C42 C43 C48 -178.4(3) . . . . ? N3 C42 C43 C48 -0.9(5) . . . . ? C48 C43 C44 C45 0.0 . . . . ? C42 C43 C44 C45 180.0(3) . . . . ? C43 C44 C45 C46 0.0 . . . . ? C44 C45 C46 C47 0.0 . . . . ? C45 C46 C47 C48 0.0 . . . . ? C46 C47 C48 O8 178.1(3) . . . . ? C46 C47 C48 C43 0.0 . . . . ? C44 C43 C48 O8 -178.2(3) . . . . ? C42 C43 C48 O8 1.8(3) . . . . ? C44 C43 C48 C47 0.0 . . . . ? C42 C43 C48 C47 -180.0(3) . . . . ? O8 C49 C50 O9 -67.3(5) . . . . ? O1 C8 N1 C7 3.3(7) . . . . ? C9 C8 N1 C7 -177.2(4) . . . . ? C6 C7 N1 C8 144.0(5) . . . . ? O6 C27 N2 C28 -2.8(8) . . . . ? C26 C27 N2 C28 173.2(5) . . . . ? C29 C28 N2 C27 103.3(6) . . . . ? O7 C42 N3 C41 6.5(7) . . . . ? C43 C42 N3 C41 -171.0(4) . . . . ? C40 C41 N3 C42 -142.0(4) . . . . ? N1 C8 O1 Er1 -91(2) . . . . ? C9 C8 O1 Er1 90(2) . . . . ? O6 Er1 O1 C8 -122(2) . . . . ? O7 Er1 O1 C8 180(100) . . . . ? O11 Er1 O1 C8 106(2) . . . . ? O13 Er1 O1 C8 34(2) . . . . ? O18 Er1 O1 C8 -38(2) . . . . ? O16 Er1 O1 C8 -58(2) . . . . ? O10 Er1 O1 C8 155(2) . . . . ? O15 Er1 O1 C8 39(2) . . . . ? C13 C14 O2 C15 5.0(5) . . . . ? C9 C14 O2 C15 -176.8(4) . . . . ? C16 C15 O2 C14 -174.5(4) . . . . ? C15 C16 O3 C17 175.9(4) . . . . ? C51 C17 O3 C16 -175.9(4) 1_554 . . . ? C20 C19 O4 C18 -178.9(6) . . . . ? C18 C18 O4 C19 -177.7(7) 2_676 . . . ? C22 C21 O5 C20 -8.2(7) . . . . ? C26 C21 O5 C20 166.7(5) . . . . ? C19 C20 O5 C21 -155.2(5) . . . . ? N2 C27 O6 Er1 -135.6(18) . . . . ? C26 C27 O6 Er1 48(2) . . . . ? O1 Er1 O6 C27 -112(2) . . . . ? O7 Er1 O6 C27 43(2) . . . . ? O11 Er1 O6 C27 -27(2) . . . . ? O13 Er1 O6 C27 107(2) . . . . ? O18 Er1 O6 C27 170(2) . . . . ? O16 Er1 O6 C27 117(2) . . . . ? O10 Er1 O6 C27 -34(2) . . . . ? O15 Er1 O6 C27 -145.8(19) . . . . ? N3 C42 O7 Er1 85.6(8) . . . . ? C43 C42 O7 Er1 -96.9(7) . . . . ? O1 Er1 O7 C42 108.1(7) . . . . ? O6 Er1 O7 C42 51.2(7) . . . . ? O11 Er1 O7 C42 -174.5(7) . . . . ? O13 Er1 O7 C42 -99.9(7) . . . . ? O18 Er1 O7 C42 -25.1(8) . . . . ? O16 Er1 O7 C42 -26.1(7) . . . . ? O10 Er1 O7 C42 132.7(7) . . . . ? O15 Er1 O7 C42 -122.5(7) . . . . ? C47 C48 O8 C49 1.2(5) . . . . ? C43 C48 O8 C49 179.4(3) . . . . ? C50 C49 O8 C48 -179.8(4) . . . . ? C49 C50 O9 C51 177.1(4) . . . . ? C17 C51 O9 C50 -178.5(4) 1_556 . . . ? O12 N4 O10 Er1 -178.8(4) . . . . ? O11 N4 O10 Er1 -0.2(4) . . . . ? O1 Er1 O10 N4 -104.4(3) . . . . ? O6 Er1 O10 N4 173.8(3) . . . . ? O7 Er1 O10 N4 88.0(3) . . . . ? O11 Er1 O10 N4 0.1(3) . . . . ? O13 Er1 O10 N4 17.5(3) . . . . ? O18 Er1 O10 N4 -130.8(3) . . . . ? O16 Er1 O10 N4 123.1(3) . . . . ? O15 Er1 O10 N4 -39.0(3) . . . . ? O12 N4 O11 Er1 178.8(4) . . . . ? O10 N4 O11 Er1 0.2(4) . . . . ? O1 Er1 O11 N4 70.2(3) . . . . ? O6 Er1 O11 N4 -8.5(4) . . . . ? O7 Er1 O11 N4 -80.6(3) . . . . ? O13 Er1 O11 N4 -165.1(3) . . . . ? O18 Er1 O11 N4 142.4(3) . . . . ? O16 Er1 O11 N4 -130.0(3) . . . . ? O10 Er1 O11 N4 -0.1(3) . . . . ? O15 Er1 O11 N4 140.4(3) . . . . ? O14 N5 O13 Er1 169.7(4) . . . . ? O15 N5 O13 Er1 -10.1(4) . . . . ? O1 Er1 O13 N5 11.7(3) . . . . ? O6 Er1 O13 N5 144.0(3) . . . . ? O7 Er1 O13 N5 -151.8(3) . . . . ? O11 Er1 O13 N5 -70.0(3) . . . . ? O18 Er1 O13 N5 80.8(3) . . . . ? O16 Er1 O13 N5 133.4(3) . . . . ? O10 Er1 O13 N5 -84.1(3) . . . . ? O15 Er1 O13 N5 5.8(2) . . . . ? O14 N5 O15 Er1 -170.0(4) . . . . ? O13 N5 O15 Er1 9.8(4) . . . . ? O1 Er1 O15 N5 179.2(3) . . . . ? O6 Er1 O15 N5 -145.4(2) . . . . ? O7 Er1 O15 N5 23.1(3) . . . . ? O11 Er1 O15 N5 79.4(3) . . . . ? O13 Er1 O15 N5 -5.9(2) . . . . ? O18 Er1 O15 N5 -99.3(3) . . . . ? O16 Er1 O15 N5 -57.4(3) . . . . ? O10 Er1 O15 N5 111.5(3) . . . . ? O17 N6 O16 Er1 -177.3(4) . . . . ? O18 N6 O16 Er1 1.3(4) . . . . ? O1 Er1 O16 N6 24.5(3) . . . . ? O6 Er1 O16 N6 90.8(3) . . . . ? O7 Er1 O16 N6 178.3(3) . . . . ? O11 Er1 O16 N6 -130.3(3) . . . . ? O13 Er1 O16 N6 -95.0(3) . . . . ? O18 Er1 O16 N6 -0.8(2) . . . . ? O10 Er1 O16 N6 142.6(3) . . . . ? O15 Er1 O16 N6 -54.8(3) . . . . ? O17 N6 O18 Er1 177.3(4) . . . . ? O16 N6 O18 Er1 -1.3(4) . . . . ? O1 Er1 O18 N6 -158.4(3) . . . . ? O6 Er1 O18 N6 -77.2(2) . . . . ? O7 Er1 O18 N6 -0.4(3) . . . . ? O11 Er1 O18 N6 124.3(3) . . . . ? O13 Er1 O18 N6 74.1(2) . . . . ? O16 Er1 O18 N6 0.8(2) . . . . ? O10 Er1 O18 N6 -132.1(3) . . . . ? O15 Er1 O18 N6 126.3(3) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.874 _refine_diff_density_min -0.598 _refine_diff_density_rms 0.071 #===END #===END data_compound2 _database_code_depnum_ccdc_archive 'CCDC 817221' #TrackingRef '- 1-12.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C96 H96 N12 O33 Pr2' _chemical_formula_weight 2227.67 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) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.961(2) _cell_length_b 22.678(3) _cell_length_c 21.079(3) _cell_angle_alpha 90.00 _cell_angle_beta 104.390(7) _cell_angle_gamma 90.00 _cell_volume 5538.2(15) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2684 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 15.38 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.336 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2276 _exptl_absorpt_coefficient_mu 0.949 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.827 _exptl_absorpt_correction_T_max 0.827 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30333 _diffrn_reflns_av_R_equivalents 0.0686 _diffrn_reflns_av_sigmaI/netI 0.1318 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.00 _diffrn_reflns_theta_max 25.41 _reflns_number_total 17856 _reflns_number_gt 8597 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _refine_special_details ; Restraints to thermal parameters were applied on the disordered phenyl groups. 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. Diffuse electron densities resulting from residual disorder solvent moleculeswere removed from the data set using the SQUEEZE routine of PLATON andrefined further using the data generated. ; # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.061 0.057 0.443 213 52 ' ' 2 0.061 0.557 0.557 212 52 ' ' 3 0.486 0.623 1.077 254 53 ' ' 4 0.514 0.123 0.923 253 53 ' ' _platon_squeeze_details ; ; _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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.003(11) _refine_ls_number_reflns 17856 _refine_ls_number_parameters 1234 _refine_ls_number_restraints 535 _refine_ls_R_factor_all 0.1297 _refine_ls_R_factor_gt 0.0555 _refine_ls_wR_factor_ref 0.0988 _refine_ls_wR_factor_gt 0.0854 _refine_ls_goodness_of_fit_ref 0.982 _refine_ls_restrained_S_all 0.989 _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 C27 C 0.1018(9) 0.6689(3) 0.2412(4) 0.073(3) Uani 1 1 d G . . C28 C -0.0143(9) 0.6838(3) 0.2297(3) 0.088(4) Uani 1 1 d G . . H28 H -0.0507 0.7034 0.1914 0.106 Uiso 1 1 calc R . . C29 C -0.0759(6) 0.6694(3) 0.2754(6) 0.101(4) Uani 1 1 d G . . H29 H -0.1535 0.6794 0.2677 0.121 Uiso 1 1 calc R . . C30 C -0.0215(9) 0.6401(4) 0.3327(4) 0.112(4) Uani 1 1 d G . . H30 H -0.0627 0.6304 0.3633 0.134 Uiso 1 1 calc R . . C31 C 0.0946(9) 0.6252(3) 0.3442(3) 0.150(6) Uani 1 1 d G . . H31 H 0.1310 0.6055 0.3825 0.180 Uiso 1 1 calc R . . C32 C 0.1562(6) 0.6396(3) 0.2985(5) 0.114(4) Uani 1 1 d G . . H32 H 0.2339 0.6296 0.3062 0.137 Uiso 1 1 calc R . . C1 C 0.6336(8) 0.2871(3) 0.2964(3) 0.106(3) Uani 1 1 d GU . . H1 H 0.6229 0.2576 0.3250 0.127 Uiso 1 1 calc R . . C2 C 0.7433(7) 0.2983(3) 0.2880(3) 0.108(3) Uani 1 1 d GU . . H2 H 0.8060 0.2763 0.3111 0.130 Uiso 1 1 calc R . . C3 C 0.7593(6) 0.3423(4) 0.2453(4) 0.106(3) Uani 1 1 d GU . . H3 H 0.8327 0.3498 0.2397 0.127 Uiso 1 1 calc R . . C4 C 0.6656(8) 0.3751(3) 0.2109(3) 0.117(3) Uani 1 1 d GU . . H4 H 0.6763 0.4046 0.1823 0.141 Uiso 1 1 calc R . . C5 C 0.5559(7) 0.3639(3) 0.2193(3) 0.116(3) Uani 1 1 d GU . . H5 H 0.4933 0.3859 0.1962 0.140 Uiso 1 1 calc R . . C6 C 0.5399(6) 0.3199(4) 0.2620(4) 0.087(3) Uani 1 1 d GU . . Pr1 Pr 0.11697(5) 0.80485(2) 0.03138(3) 0.06956(18) Uani 1 1 d . . . Pr2 Pr 0.42027(5) 0.19556(2) 0.45059(3) 0.06934(18) Uani 1 1 d . . . C7 C 0.4229(8) 0.3149(5) 0.2748(4) 0.076(3) Uani 1 1 d . . . H7A H 0.3646 0.3218 0.2345 0.092 Uiso 1 1 calc R . . H7B H 0.4124 0.2752 0.2896 0.092 Uiso 1 1 calc R . . C8 C 0.4091(8) 0.3455(4) 0.3846(5) 0.058(3) Uani 1 1 d . . . C9 C 0.3995(8) 0.3937(5) 0.4320(6) 0.059(3) Uani 1 1 d . . . C10 C 0.3913(8) 0.3791(5) 0.4929(6) 0.070(3) Uani 1 1 d . . . H10 H 0.3939 0.3393 0.5038 0.084 Uiso 1 1 calc R . . C11 C 0.3794(10) 0.4192(5) 0.5399(6) 0.100(4) Uani 1 1 d . . . H11 H 0.3722 0.4083 0.5812 0.120 Uiso 1 1 calc R . . C12 C 0.3794(9) 0.4761(6) 0.5201(7) 0.092(4) Uani 1 1 d . . . H12 H 0.3732 0.5050 0.5503 0.110 Uiso 1 1 calc R . . C13 C 0.3874(9) 0.4945(5) 0.4609(6) 0.079(4) Uani 1 1 d . . . H13 H 0.3863 0.5345 0.4510 0.095 Uiso 1 1 calc R . . C14 C 0.3973(8) 0.4528(5) 0.4152(5) 0.057(3) Uani 1 1 d . . . C15 C 0.3910(9) 0.5270(4) 0.3341(5) 0.088(4) Uani 1 1 d . . . H15A H 0.4539 0.5509 0.3592 0.106 Uiso 1 1 calc R . . H15B H 0.3190 0.5426 0.3404 0.106 Uiso 1 1 calc R . . C16 C 0.3903(11) 0.5283(4) 0.2620(5) 0.100(4) Uani 1 1 d . . . H16A H 0.4013 0.5683 0.2484 0.120 Uiso 1 1 calc R . . H16B H 0.4522 0.5040 0.2541 0.120 Uiso 1 1 calc R . . C17 C 0.2878(10) 0.4787(5) 0.1676(6) 0.107(4) Uani 1 1 d . . . H17A H 0.3227 0.4401 0.1769 0.129 Uiso 1 1 calc R . . H17B H 0.3352 0.5016 0.1454 0.129 Uiso 1 1 calc R . . C18 C 0.1719(9) 0.4724(4) 0.1244(5) 0.090(3) Uani 1 1 d . . . H18A H 0.1767 0.4494 0.0864 0.108 Uiso 1 1 calc R . . H18B H 0.1239 0.4508 0.1474 0.108 Uiso 1 1 calc R . . C19 C 0.0943(8) 0.5419(4) 0.0406(5) 0.054(3) Uani 1 1 d . . . C20 C 0.0652(9) 0.5017(4) -0.0081(5) 0.069(3) Uani 1 1 d . . . H20 H 0.0672 0.4620 0.0028 0.083 Uiso 1 1 calc R . . C21 C 0.0332(10) 0.5170(5) -0.0721(5) 0.091(4) Uani 1 1 d . . . H21 H 0.0129 0.4887 -0.1048 0.109 Uiso 1 1 calc R . . C22 C 0.0318(11) 0.5790(6) -0.0877(5) 0.117(5) Uani 1 1 d . . . H22 H 0.0117 0.5916 -0.1310 0.140 Uiso 1 1 calc R . . C23 C 0.0607(10) 0.6187(4) -0.0375(5) 0.086(3) Uani 1 1 d . . . H23 H 0.0576 0.6587 -0.0475 0.103 Uiso 1 1 calc R . . C24 C 0.0924(10) 0.6029(5) 0.0240(5) 0.070(3) Uani 1 1 d . . . C25 C 0.1183(9) 0.6516(4) 0.0741(5) 0.064(3) Uani 1 1 d . . . C26 C 0.1567(10) 0.6824(4) 0.1878(5) 0.094(3) Uani 1 1 d . . . H26A H 0.1303 0.7208 0.1700 0.112 Uiso 1 1 calc R . . H26B H 0.2395 0.6850 0.2060 0.112 Uiso 1 1 calc R . . C33 C 0.0603(10) 0.3860(6) 0.4043(6) 0.110(5) Uani 1 1 d . . . H33 H 0.0418 0.3879 0.4446 0.132 Uiso 1 1 calc R . . C34 C 0.0683(10) 0.4369(5) 0.3679(7) 0.110(4) Uani 1 1 d . . . H34 H 0.0538 0.4734 0.3844 0.132 Uiso 1 1 calc R . . C35 C 0.0964(11) 0.4350(7) 0.3093(6) 0.107(5) Uani 1 1 d . . . H35 H 0.1076 0.4694 0.2876 0.129 Uiso 1 1 calc R . . C36 C 0.1073(11) 0.3820(7) 0.2843(6) 0.112(4) Uani 1 1 d . . . H36 H 0.1188 0.3794 0.2423 0.134 Uiso 1 1 calc R . . C37 C 0.1020(8) 0.3323(5) 0.3181(5) 0.086(4) Uani 1 1 d . . . H37 H 0.1131 0.2959 0.3004 0.103 Uiso 1 1 calc R . . C38 C 0.0802(9) 0.3357(6) 0.3788(6) 0.086(4) Uani 1 1 d . . . C39 C 0.0691(8) 0.2759(4) 0.4120(5) 0.077(3) Uani 1 1 d . . . H39A H -0.0095 0.2617 0.3966 0.092 Uiso 1 1 calc R . . H39B H 0.1197 0.2475 0.3989 0.092 Uiso 1 1 calc R . . C40 C 0.1986(10) 0.2635(4) 0.5212(4) 0.057(3) Uani 1 1 d . . . C41 C 0.2234(10) 0.2781(3) 0.5940(5) 0.067(3) Uani 1 1 d . . . C42 C 0.3366(10) 0.2789(4) 0.6275(6) 0.090(4) Uani 1 1 d . . . H42 H 0.3938 0.2690 0.6064 0.108 Uiso 1 1 calc R . . C43 C 0.3666(12) 0.2948(7) 0.6942(6) 0.122(5) Uani 1 1 d . . . H43 H 0.4437 0.2951 0.7175 0.147 Uiso 1 1 calc R . . C44 C 0.2835(12) 0.3097(6) 0.7243(5) 0.102(4) Uani 1 1 d . . . H44 H 0.3028 0.3228 0.7674 0.122 Uiso 1 1 calc R . . C45 C 0.1690(11) 0.3052(6) 0.6900(6) 0.102(3) Uani 1 1 d . . . H45 H 0.1119 0.3121 0.7120 0.122 Uiso 1 1 calc R . . C46 C 0.1370(12) 0.2911(4) 0.6258(6) 0.074(3) Uani 1 1 d . . . C47 C -0.0613(8) 0.3049(5) 0.6231(5) 0.084(3) Uani 1 1 d . . . H47A H -0.0475 0.3445 0.6406 0.100 Uiso 1 1 calc R . . H47B H -0.0642 0.2780 0.6584 0.100 Uiso 1 1 calc R . . C48 C -0.1664(9) 0.3024(5) 0.5723(5) 0.097(3) Uani 1 1 d . . . H48A H -0.1769 0.2627 0.5545 0.117 Uiso 1 1 calc R . . H48B H -0.2311 0.3112 0.5909 0.117 Uiso 1 1 calc R . . C49 C -0.2735(9) 0.3449(5) 0.4730(6) 0.088(3) Uani 1 1 d . . . H49A H -0.3348 0.3544 0.4939 0.106 Uiso 1 1 calc R . . H49B H -0.2898 0.3065 0.4524 0.106 Uiso 1 1 calc R . . C50 C -0.2693(9) 0.3894(4) 0.4231(5) 0.082(3) Uani 1 1 d . . . H50A H -0.1986 0.3855 0.4089 0.099 Uiso 1 1 calc R . . H50B H -0.3343 0.3846 0.3854 0.099 Uiso 1 1 calc R . . C51 C -0.2833(8) 0.4957(5) 0.4131(6) 0.076(3) Uani 1 1 d . . . C52 C -0.2810(9) 0.4951(6) 0.3437(6) 0.105(4) Uani 1 1 d . . . H52 H -0.2703 0.4598 0.3236 0.126 Uiso 1 1 calc R . . C53 C -0.2948(11) 0.5471(8) 0.3086(7) 0.123(5) Uani 1 1 d . . . H53 H -0.2913 0.5463 0.2650 0.148 Uiso 1 1 calc R . . C54 C -0.3123(13) 0.5970(7) 0.3346(9) 0.138(6) Uani 1 1 d . . . H54 H -0.3238 0.6316 0.3101 0.166 Uiso 1 1 calc R . . C55 C -0.3136(10) 0.5972(5) 0.4000(7) 0.095(4) Uani 1 1 d . . . H55 H -0.3252 0.6334 0.4180 0.114 Uiso 1 1 calc R . . C56 C -0.2991(8) 0.5485(5) 0.4418(6) 0.076(3) Uani 1 1 d . . . C57 C -0.3094(8) 0.5574(5) 0.5092(5) 0.069(3) Uani 1 1 d . . . C58 C -0.3132(14) 0.5191(6) 0.6137(6) 0.167(7) Uani 1 1 d . . . H58A H -0.3056 0.5602 0.6269 0.200 Uiso 1 1 calc R . . H58B H -0.3909 0.5064 0.6132 0.200 Uiso 1 1 calc R . . C59 C -0.2322(6) 0.4845(3) 0.6601(3) 0.146(4) Uani 1 1 d GU . . C60 C -0.1217(7) 0.4936(3) 0.6995(3) 0.201(5) Uani 1 1 d GU . . H60 H -0.0842 0.5292 0.6976 0.242 Uiso 1 1 calc R . . C61 C -0.0674(7) 0.4495(4) 0.7418(3) 0.180(5) Uani 1 1 d GU . . H61 H 0.0065 0.4555 0.7682 0.216 Uiso 1 1 calc R . . C62 C -0.1236(7) 0.3962(3) 0.7447(3) 0.181(5) Uani 1 1 d GU . . H62 H -0.0872 0.3667 0.7731 0.217 Uiso 1 1 calc R . . C63 C -0.2340(7) 0.3871(3) 0.7053(3) 0.199(5) Uani 1 1 d GU . . H63 H -0.2715 0.3515 0.7073 0.239 Uiso 1 1 calc R . . C64 C -0.2883(6) 0.4313(3) 0.6630(3) 0.185(5) Uani 1 1 d GU . . H64 H -0.3622 0.4252 0.6366 0.222 Uiso 1 1 calc R . . C65 C 0.6494(6) 0.8334(3) 0.0119(3) 0.170(4) Uani 1 1 d GU . . H65 H 0.6929 0.8008 0.0298 0.204 Uiso 1 1 calc R . . C66 C 0.7031(6) 0.8876(3) 0.0099(3) 0.160(4) Uani 1 1 d GU . . H66 H 0.7824 0.8911 0.0265 0.192 Uiso 1 1 calc R . . C67 C 0.6380(7) 0.9364(3) -0.0168(3) 0.138(4) Uani 1 1 d GU . . H67 H 0.6739 0.9726 -0.0181 0.166 Uiso 1 1 calc R . . C68 C 0.5194(6) 0.9312(3) -0.0416(3) 0.166(4) Uani 1 1 d GU . . H68 H 0.4759 0.9639 -0.0595 0.199 Uiso 1 1 calc R . . C69 C 0.4658(6) 0.8771(3) -0.0396(2) 0.168(4) Uani 1 1 d GU . . H69 H 0.3864 0.8735 -0.0562 0.201 Uiso 1 1 calc R . . C70 C 0.5308(6) 0.8282(3) -0.0129(2) 0.137(4) Uani 1 1 d GU . . C71 C 0.4608(13) 0.7737(6) -0.0049(7) 0.167(4) Uani 1 1 d U . . H71A H 0.4164 0.7812 0.0270 0.200 Uiso 1 1 calc R . . H71B H 0.5120 0.7407 0.0104 0.200 Uiso 1 1 calc R . . C72 C 0.2708(13) 0.7540(5) -0.0854(7) 0.095(4) Uani 1 1 d . . . C73 C 0.2149(12) 0.7195(4) -0.1468(5) 0.073(3) Uani 1 1 d . . . C74 C 0.0945(14) 0.7196(5) -0.1681(7) 0.109(5) Uani 1 1 d . . . H74 H 0.0508 0.7434 -0.1476 0.131 Uiso 1 1 calc R . . C75 C 0.0400(13) 0.6833(9) -0.2212(9) 0.147(8) Uani 1 1 d . . . H75 H -0.0400 0.6806 -0.2342 0.177 Uiso 1 1 calc R . . C76 C 0.1031(17) 0.6544(8) -0.2508(8) 0.143(7) Uani 1 1 d . . . H76 H 0.0658 0.6323 -0.2871 0.172 Uiso 1 1 calc R . . C77 C 0.2109(15) 0.6533(5) -0.2351(6) 0.108(4) Uani 1 1 d . . . H77 H 0.2498 0.6302 -0.2591 0.129 Uiso 1 1 calc R . . C78 C 0.2753(12) 0.6867(5) -0.1811(5) 0.080(3) Uani 1 1 d . . . C79 C 0.4570(14) 0.6511(6) -0.1929(7) 0.137(6) Uani 1 1 d . . . H79A H 0.4332 0.6563 -0.2400 0.165 Uiso 1 1 calc R . . H79B H 0.4450 0.6101 -0.1831 0.165 Uiso 1 1 calc R . . C80 C 0.5812(13) 0.6665(6) -0.1686(7) 0.142(6) Uani 1 1 d . . . H80A H 0.6269 0.6457 -0.1936 0.171 Uiso 1 1 calc R . . H80B H 0.5925 0.7085 -0.1728 0.171 Uiso 1 1 calc R . . C81 C 0.7325(11) 0.6660(5) -0.0733(7) 0.114(5) Uani 1 1 d . . . H81A H 0.7394 0.7087 -0.0736 0.137 Uiso 1 1 calc R . . H81B H 0.7820 0.6496 -0.0989 0.137 Uiso 1 1 calc R . . C82 C 0.7674(10) 0.6444(5) -0.0068(7) 0.109(4) Uani 1 1 d . . . H82A H 0.8439 0.6589 0.0143 0.130 Uiso 1 1 calc R . . H82B H 0.7141 0.6581 0.0179 0.130 Uiso 1 1 calc R . . C83 C 0.8037(8) 0.5484(4) 0.0460(5) 0.061(3) Uani 1 1 d . . . C84 C 0.8105(8) 0.4863(4) 0.0415(5) 0.064(3) Uani 1 1 d . . . C85 C 0.8417(8) 0.4531(4) 0.0955(5) 0.076(3) Uani 1 1 d . . . H85 H 0.8421 0.4123 0.0916 0.091 Uiso 1 1 calc R . . C86 C 0.8735(9) 0.4789(5) 0.1575(6) 0.089(3) Uani 1 1 d . . . H86 H 0.9012 0.4561 0.1947 0.106 Uiso 1 1 calc R . . C87 C 0.8626(10) 0.5390(6) 0.1619(5) 0.092(4) Uani 1 1 d . . . H87 H 0.8771 0.5565 0.2030 0.110 Uiso 1 1 calc R . . C88 C 0.8308(10) 0.5738(5) 0.1070(7) 0.098(4) Uani 1 1 d . . . H88 H 0.8277 0.6145 0.1112 0.118 Uiso 1 1 calc R . . C89 C 0.7764(9) 0.4562(5) -0.0265(5) 0.066(3) Uani 1 1 d . . . C90 C 0.7009(14) 0.4605(5) -0.1437(6) 0.147(6) Uani 1 1 d . . . H90A H 0.7220 0.4191 -0.1416 0.176 Uiso 1 1 calc R . . H90B H 0.7469 0.4808 -0.1688 0.176 Uiso 1 1 calc R . . C91 C 0.5798(16) 0.4665(7) -0.1764(9) 0.139(4) Uani 1 1 d U . . C92 C 0.5407(15) 0.4950(6) -0.2377(8) 0.160(4) Uani 1 1 d U . . H92 H 0.5943 0.5099 -0.2587 0.192 Uiso 1 1 calc R . . C93 C 0.4222(17) 0.5011(7) -0.2672(8) 0.170(5) Uani 1 1 d U . . H93 H 0.3980 0.5210 -0.3068 0.204 Uiso 1 1 calc R . . C94 C 0.3498(15) 0.4799(7) -0.2402(9) 0.175(5) Uani 1 1 d U . . H94 H 0.2713 0.4828 -0.2601 0.211 Uiso 1 1 calc R . . C95 C 0.3895(16) 0.4503(7) -0.1772(9) 0.184(5) Uani 1 1 d U . . H95 H 0.3374 0.4326 -0.1569 0.221 Uiso 1 1 calc R . . C96 C 0.5046(16) 0.4494(6) -0.1488(8) 0.167(5) Uani 1 1 d U . . H96 H 0.5289 0.4353 -0.1062 0.201 Uiso 1 1 calc R . . N1 N 0.4084(6) 0.3559(3) 0.3229(4) 0.062(2) Uani 1 1 d . . . H1A H 0.3978 0.3920 0.3103 0.075 Uiso 1 1 calc R . . N2 N 0.1349(8) 0.6406(3) 0.1353(4) 0.082(3) Uani 1 1 d . . . H2A H 0.1327 0.6041 0.1460 0.098 Uiso 1 1 calc R . . N3 N 0.0980(7) 0.2792(3) 0.4836(4) 0.078(3) Uani 1 1 d . . . H3A H 0.0463 0.2920 0.5021 0.094 Uiso 1 1 calc R . . N4 N -0.2952(8) 0.5135(4) 0.5485(4) 0.104(3) Uani 1 1 d . . . H4A H -0.2746 0.4800 0.5359 0.125 Uiso 1 1 calc R . . N5 N 0.3789(11) 0.7591(6) -0.0722(6) 0.174(6) Uani 1 1 d . . . H5A H 0.4108 0.7538 -0.1041 0.209 Uiso 1 1 calc R . . N6 N 0.7259(8) 0.4845(4) -0.0782(4) 0.097(3) Uani 1 1 d . . . H6 H 0.7054 0.5203 -0.0737 0.116 Uiso 1 1 calc R . . N7 N -0.0932(11) 0.8116(5) -0.0849(5) 0.097(3) Uani 1 1 d . . . N8 N -0.0531(11) 0.8306(6) 0.1121(6) 0.107(4) Uani 1 1 d . . . N9 N 0.3131(15) 0.7972(8) 0.1460(9) 0.168(10) Uani 1 1 d . . . N10 N 0.2869(11) 0.1680(5) 0.3127(6) 0.103(4) Uani 1 1 d . . . N11 N 0.6309(10) 0.1456(6) 0.4184(6) 0.113(4) Uani 1 1 d . . . N12 N 0.5749(11) 0.2134(6) 0.5855(7) 0.119(5) Uani 1 1 d . . . O1 O 0.4181(5) 0.2919(3) 0.4047(3) 0.0720(19) Uani 1 1 d . . . O2 O 0.4052(6) 0.4675(3) 0.3548(3) 0.075(2) Uani 1 1 d . . . O3 O 0.2854(7) 0.5070(4) 0.2274(4) 0.110(3) Uani 1 1 d . . . O4 O 0.1200(7) 0.5261(3) 0.1037(3) 0.103(3) Uani 1 1 d . . . O5 O 0.1277(6) 0.7037(3) 0.0557(3) 0.089(2) Uani 1 1 d . . . O6 O 0.2742(6) 0.2390(3) 0.4982(3) 0.074(2) Uani 1 1 d . . . O7 O 0.0264(6) 0.2876(3) 0.5916(3) 0.087(2) Uani 1 1 d . . . O8 O -0.1655(6) 0.3430(3) 0.5210(4) 0.080(2) Uani 1 1 d . . . O9 O -0.2739(6) 0.4454(3) 0.4523(3) 0.082(2) Uani 1 1 d . . . O10 O -0.3302(6) 0.6083(4) 0.5258(3) 0.089(2) Uani 1 1 d . . . O11 O 0.2122(8) 0.7780(3) -0.0513(4) 0.112(3) Uani 1 1 d . . . O12 O 0.3913(7) 0.6874(4) -0.1628(3) 0.099(2) Uani 1 1 d . . . O13 O 0.6149(7) 0.6492(3) -0.1012(4) 0.093(2) Uani 1 1 d . . . O14 O 0.7679(6) 0.5814(3) -0.0086(4) 0.088(2) Uani 1 1 d . . . O15 O 0.8022(6) 0.4008(3) -0.0261(3) 0.083(2) Uani 1 1 d . . . O16 O -0.0619(7) 0.7638(3) -0.0516(4) 0.090(2) Uani 1 1 d . . . O17 O -0.1714(8) 0.8127(4) -0.1299(4) 0.136(3) Uani 1 1 d . . . O18 O -0.0252(7) 0.8539(3) -0.0647(4) 0.098(3) Uani 1 1 d . . . O19 O -0.0339(8) 0.7781(4) 0.0933(4) 0.104(3) Uani 1 1 d . . . O20 O -0.1166(9) 0.8398(4) 0.1480(5) 0.134(4) Uani 1 1 d . . . O21 O -0.0061(7) 0.8716(3) 0.0850(4) 0.101(3) Uani 1 1 d . . . O22 O 0.2137(9) 0.8170(4) 0.1510(5) 0.115(4) Uani 1 1 d . . . O23 O 0.3905(9) 0.7944(6) 0.1975(6) 0.231(6) Uani 1 1 d . . . O24 O 0.3246(12) 0.7882(7) 0.0922(5) 0.158(5) Uani 1 1 d . . . O25 O 0.2393(6) 0.1872(4) 0.3568(4) 0.090(2) Uani 1 1 d . . . O26 O 0.2318(8) 0.1541(5) 0.2587(4) 0.159(5) Uani 1 1 d . . . O27 O 0.3953(7) 0.1654(3) 0.3319(4) 0.103(3) Uani 1 1 d . . . O28 O 0.6141(6) 0.1998(4) 0.4238(4) 0.106(2) Uani 1 1 d . . . O29 O 0.7044(10) 0.1237(5) 0.3950(6) 0.191(6) Uani 1 1 d . . . O30 O 0.5569(8) 0.1138(3) 0.4343(4) 0.117(3) Uani 1 1 d . . . O31 O 0.5502(6) 0.2536(4) 0.5440(4) 0.092(2) Uani 1 1 d . . . O32 O 0.6293(8) 0.2234(5) 0.6402(5) 0.162(5) Uani 1 1 d . . . O33 O 0.5328(8) 0.1630(5) 0.5656(5) 0.123(4) 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 C27 0.123(11) 0.050(6) 0.060(8) 0.002(5) 0.050(8) -0.015(6) C28 0.104(10) 0.081(9) 0.084(9) 0.019(7) 0.031(8) -0.007(8) C29 0.118(11) 0.071(8) 0.096(10) -0.005(7) -0.007(10) -0.003(7) C30 0.155(15) 0.083(9) 0.103(12) -0.030(8) 0.045(10) -0.019(8) C31 0.212(19) 0.121(11) 0.133(13) 0.062(9) 0.074(13) 0.036(12) C32 0.142(12) 0.120(10) 0.105(10) 0.050(8) 0.075(10) 0.031(8) C1 0.115(6) 0.107(6) 0.094(5) -0.008(5) 0.022(5) 0.006(5) C2 0.117(6) 0.109(6) 0.092(5) -0.029(5) 0.012(5) 0.019(6) C3 0.104(6) 0.117(6) 0.103(6) -0.029(5) 0.035(5) -0.001(5) C4 0.116(6) 0.125(6) 0.115(6) -0.013(5) 0.036(5) 0.008(5) C5 0.118(6) 0.121(6) 0.112(6) 0.002(5) 0.032(5) 0.006(5) C6 0.101(6) 0.080(6) 0.079(5) -0.020(5) 0.021(5) 0.002(5) Pr1 0.0945(5) 0.0441(3) 0.0672(4) 0.0072(4) 0.0147(3) 0.0034(4) Pr2 0.0641(4) 0.0584(4) 0.0871(4) 0.0133(4) 0.0218(3) 0.0017(4) C7 0.099(9) 0.078(8) 0.053(6) -0.041(6) 0.021(6) -0.002(7) C8 0.057(7) 0.046(7) 0.072(8) 0.005(6) 0.016(6) -0.013(5) C9 0.039(6) 0.059(8) 0.080(8) 0.006(7) 0.018(6) 0.011(5) C10 0.066(8) 0.061(7) 0.092(9) -0.004(7) 0.036(7) -0.015(5) C11 0.146(12) 0.072(8) 0.091(9) -0.016(8) 0.049(8) 0.007(8) C12 0.097(10) 0.075(9) 0.106(11) -0.031(8) 0.030(8) -0.005(7) C13 0.107(10) 0.054(7) 0.071(8) 0.002(7) 0.010(8) -0.009(6) C14 0.058(7) 0.050(7) 0.058(7) 0.003(6) 0.007(6) 0.000(5) C15 0.111(9) 0.045(7) 0.087(8) -0.001(6) -0.016(7) -0.014(6) C16 0.151(13) 0.073(8) 0.073(9) 0.021(6) 0.022(9) -0.015(7) C17 0.120(11) 0.093(9) 0.088(9) -0.030(7) -0.014(8) 0.018(7) C18 0.114(9) 0.047(7) 0.092(8) 0.019(6) -0.008(8) -0.008(6) C19 0.076(7) 0.035(6) 0.051(7) 0.007(5) 0.013(6) 0.001(5) C20 0.098(9) 0.052(6) 0.055(7) 0.007(6) 0.014(6) 0.008(6) C21 0.137(11) 0.066(8) 0.069(9) 0.007(6) 0.023(8) 0.012(7) C22 0.182(14) 0.123(11) 0.041(7) 0.021(8) 0.021(8) 0.028(10) C23 0.144(11) 0.059(7) 0.052(7) 0.004(6) 0.023(7) 0.003(7) C24 0.105(10) 0.069(8) 0.043(7) 0.012(6) 0.033(7) 0.031(6) C25 0.103(9) 0.062(8) 0.035(6) 0.018(6) 0.033(6) 0.015(6) C26 0.162(10) 0.046(7) 0.082(7) 0.002(6) 0.048(7) -0.017(7) C33 0.143(12) 0.108(10) 0.074(9) 0.012(9) 0.020(8) 0.083(9) C34 0.129(12) 0.082(9) 0.112(11) 0.006(8) 0.018(9) 0.023(7) C35 0.129(12) 0.121(12) 0.063(9) 0.015(8) 0.007(8) -0.047(9) C36 0.135(12) 0.121(12) 0.070(9) 0.016(10) 0.007(8) -0.008(10) C37 0.080(8) 0.130(11) 0.047(7) 0.002(7) 0.014(6) -0.001(6) C38 0.060(8) 0.117(11) 0.077(10) 0.046(8) 0.006(7) 0.007(7) C39 0.071(8) 0.086(8) 0.068(8) -0.014(6) 0.007(6) -0.002(5) C40 0.088(9) 0.040(5) 0.045(7) 0.007(5) 0.020(6) 0.005(5) C41 0.070(8) 0.050(6) 0.067(8) 0.006(5) -0.008(7) -0.014(5) C42 0.062(9) 0.107(10) 0.101(10) 0.010(7) 0.021(8) 0.005(6) C43 0.095(11) 0.172(14) 0.084(10) -0.016(10) -0.010(9) -0.032(11) C44 0.094(11) 0.131(10) 0.072(8) 0.003(9) 0.005(8) -0.013(10) C45 0.094(10) 0.111(9) 0.105(10) 0.022(10) 0.035(9) 0.007(9) C46 0.116(11) 0.057(7) 0.060(8) -0.004(6) 0.040(8) 0.019(7) C47 0.060(7) 0.103(8) 0.088(8) -0.005(8) 0.020(7) 0.019(7) C48 0.111(10) 0.090(8) 0.104(9) 0.003(9) 0.052(8) 0.003(9) C49 0.079(9) 0.078(8) 0.109(10) -0.009(7) 0.024(8) -0.005(6) C50 0.102(9) 0.069(7) 0.068(7) -0.018(6) 0.007(6) 0.026(6) C51 0.061(7) 0.062(8) 0.104(10) -0.011(7) 0.019(7) 0.019(6) C52 0.104(10) 0.129(12) 0.096(10) -0.064(9) 0.052(8) -0.011(8) C53 0.118(12) 0.144(14) 0.120(13) 0.058(12) 0.051(10) 0.005(11) C54 0.165(16) 0.115(13) 0.157(16) 0.012(12) 0.082(13) 0.024(11) C55 0.091(10) 0.075(9) 0.124(12) 0.001(9) 0.039(9) 0.022(7) C56 0.063(7) 0.064(8) 0.091(9) -0.016(7) 0.004(6) 0.006(6) C57 0.064(7) 0.076(9) 0.059(8) -0.013(7) -0.002(6) 0.017(6) C58 0.28(2) 0.153(13) 0.064(9) 0.025(8) 0.028(11) 0.136(13) C59 0.156(7) 0.174(7) 0.138(7) -0.013(6) 0.092(6) 0.029(6) C60 0.213(8) 0.229(8) 0.179(7) -0.012(6) 0.082(6) 0.044(7) C61 0.204(7) 0.198(8) 0.157(7) -0.010(6) 0.082(6) 0.047(6) C62 0.193(7) 0.206(7) 0.158(7) -0.013(6) 0.071(6) 0.043(6) C63 0.214(8) 0.223(7) 0.178(7) -0.008(6) 0.081(6) 0.050(6) C64 0.202(7) 0.202(8) 0.174(7) -0.023(6) 0.094(6) 0.062(6) C65 0.167(7) 0.160(7) 0.174(6) 0.021(6) 0.028(6) -0.026(6) C66 0.157(7) 0.151(7) 0.165(7) 0.002(6) 0.024(6) -0.034(6) C67 0.133(7) 0.140(6) 0.142(6) 0.016(6) 0.032(6) -0.028(6) C68 0.168(7) 0.158(6) 0.171(6) 0.006(6) 0.041(6) -0.030(6) C69 0.167(7) 0.174(7) 0.162(6) 0.004(6) 0.041(6) -0.010(6) C70 0.136(6) 0.137(6) 0.140(6) -0.001(5) 0.041(5) -0.041(5) C71 0.173(7) 0.155(7) 0.171(7) 0.016(6) 0.041(6) -0.020(6) C72 0.117(12) 0.067(8) 0.113(12) 0.006(8) 0.049(10) -0.052(8) C73 0.096(11) 0.058(7) 0.060(8) 0.023(6) 0.009(8) -0.008(7) C74 0.099(12) 0.135(12) 0.099(11) 0.075(9) 0.036(9) 0.005(8) C75 0.071(11) 0.24(2) 0.113(15) 0.083(15) -0.014(10) -0.044(13) C76 0.111(17) 0.222(19) 0.094(13) 0.011(11) 0.018(12) -0.066(14) C77 0.135(13) 0.108(9) 0.088(10) -0.022(8) 0.044(10) -0.030(10) C78 0.113(11) 0.064(8) 0.050(7) 0.008(6) -0.007(8) 0.010(8) C79 0.161(16) 0.144(12) 0.123(12) 0.031(9) 0.067(13) 0.072(12) C80 0.131(13) 0.173(14) 0.142(14) 0.059(11) 0.070(12) 0.064(11) C81 0.082(10) 0.067(8) 0.213(16) 0.051(9) 0.073(11) 0.025(7) C82 0.082(9) 0.059(8) 0.182(14) 0.020(8) 0.027(10) 0.020(6) C83 0.057(7) 0.049(7) 0.082(8) -0.014(6) 0.025(6) 0.005(5) C84 0.077(7) 0.053(7) 0.064(7) 0.005(6) 0.019(6) 0.002(5) C85 0.089(8) 0.058(7) 0.071(8) -0.005(6) 0.000(7) -0.005(6) C86 0.097(9) 0.071(8) 0.100(10) 0.007(7) 0.030(8) -0.002(7) C87 0.117(10) 0.099(10) 0.066(8) -0.015(7) 0.035(8) 0.003(8) C88 0.103(10) 0.078(8) 0.114(11) -0.033(8) 0.029(9) 0.012(7) C89 0.079(8) 0.062(7) 0.055(7) -0.008(6) 0.013(6) 0.005(6) C90 0.214(17) 0.133(11) 0.071(9) -0.024(8) -0.008(10) 0.093(11) C91 0.162(7) 0.129(6) 0.134(7) -0.015(6) 0.050(6) 0.020(6) C92 0.167(7) 0.162(7) 0.151(7) -0.038(6) 0.038(6) 0.032(6) C93 0.179(7) 0.173(7) 0.155(7) -0.022(6) 0.036(6) 0.009(6) C94 0.177(7) 0.170(7) 0.166(7) -0.021(6) 0.017(6) 0.006(6) C95 0.192(7) 0.177(7) 0.180(7) -0.015(6) 0.041(6) 0.002(6) C96 0.164(7) 0.155(7) 0.171(7) -0.017(6) 0.018(6) 0.016(6) N1 0.084(6) 0.051(5) 0.054(5) 0.016(4) 0.023(5) 0.006(4) N2 0.138(8) 0.031(5) 0.082(7) -0.011(5) 0.036(7) -0.004(5) N3 0.079(7) 0.104(7) 0.048(5) 0.009(4) 0.008(5) 0.026(5) N4 0.167(10) 0.083(7) 0.057(7) -0.008(5) 0.018(7) 0.049(7) N5 0.124(11) 0.269(15) 0.140(11) -0.084(10) 0.054(9) -0.107(11) N6 0.132(8) 0.082(6) 0.065(6) 0.014(6) 0.004(6) 0.060(6) N7 0.156(11) 0.059(7) 0.069(7) 0.005(7) 0.013(7) 0.020(9) N8 0.106(10) 0.132(12) 0.075(9) 0.001(8) 0.006(7) -0.012(9) N9 0.124(15) 0.142(14) 0.184(18) 0.095(17) -0.062(18) -0.048(12) N10 0.103(10) 0.142(10) 0.081(9) 0.028(7) 0.055(8) 0.032(8) N11 0.072(9) 0.111(11) 0.160(11) 0.038(9) 0.033(8) 0.002(8) N12 0.091(10) 0.135(13) 0.116(11) 0.059(10) -0.003(8) 0.003(8) O1 0.086(5) 0.049(5) 0.087(5) 0.010(4) 0.032(4) 0.006(3) O2 0.101(6) 0.045(4) 0.065(5) 0.010(4) -0.005(4) -0.004(4) O3 0.091(6) 0.146(7) 0.078(6) 0.007(5) -0.005(5) -0.032(5) O4 0.181(9) 0.045(5) 0.061(5) 0.010(4) -0.011(5) 0.018(5) O5 0.155(7) 0.040(4) 0.081(5) 0.016(4) 0.049(4) 0.017(4) O6 0.054(5) 0.094(5) 0.075(5) 0.007(4) 0.016(4) -0.002(4) O7 0.053(5) 0.132(7) 0.073(5) -0.006(4) 0.007(4) 0.009(4) O8 0.067(5) 0.077(5) 0.096(6) 0.001(4) 0.019(5) 0.007(4) O9 0.086(5) 0.073(5) 0.081(5) -0.016(4) 0.010(4) 0.016(4) O10 0.092(6) 0.093(6) 0.086(6) -0.013(5) 0.031(5) 0.024(4) O11 0.173(9) 0.073(5) 0.114(7) 0.000(4) 0.078(6) -0.025(5) O12 0.090(6) 0.101(6) 0.102(6) 0.014(5) 0.019(5) 0.029(6) O13 0.094(7) 0.088(5) 0.104(6) 0.031(5) 0.040(5) 0.019(4) O14 0.115(6) 0.058(5) 0.086(5) 0.007(4) 0.013(5) 0.022(4) O15 0.104(6) 0.049(5) 0.088(5) -0.004(4) 0.008(4) 0.004(4) O16 0.120(7) 0.064(5) 0.078(5) 0.009(4) 0.011(5) -0.018(5) O17 0.140(8) 0.127(7) 0.102(6) 0.027(6) -0.045(6) 0.018(7) O18 0.110(7) 0.057(5) 0.105(6) 0.005(5) -0.015(5) -0.005(4) O19 0.145(8) 0.077(5) 0.099(7) -0.001(5) 0.046(6) -0.035(5) O20 0.145(10) 0.157(8) 0.118(8) -0.007(6) 0.067(7) 0.012(6) O21 0.117(7) 0.084(6) 0.105(6) 0.008(5) 0.032(5) 0.027(5) O22 0.160(9) 0.091(7) 0.077(6) 0.012(5) -0.004(8) -0.021(7) O23 0.147(10) 0.273(14) 0.206(11) 0.118(11) -0.086(8) -0.043(10) O24 0.122(9) 0.185(11) 0.174(11) 0.081(11) 0.049(10) 0.034(7) O25 0.069(5) 0.103(6) 0.095(5) -0.008(6) 0.015(4) -0.002(5) O26 0.108(8) 0.280(12) 0.084(7) -0.057(7) 0.013(6) 0.000(7) O27 0.077(6) 0.130(7) 0.114(7) -0.013(5) 0.046(6) 0.010(5) O28 0.082(5) 0.077(5) 0.165(7) 0.026(6) 0.042(5) -0.006(5) O29 0.158(11) 0.165(9) 0.298(15) 0.014(9) 0.147(11) 0.041(8) O30 0.119(8) 0.065(6) 0.177(9) 0.021(5) 0.053(7) 0.039(5) O31 0.057(5) 0.114(6) 0.098(6) 0.016(5) 0.009(5) -0.015(4) O32 0.113(8) 0.234(13) 0.096(7) 0.026(7) -0.052(6) -0.013(7) O33 0.088(7) 0.127(8) 0.147(9) 0.062(7) 0.017(6) 0.016(6) _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 C27 C28 1.3900 . ? C27 C32 1.3900 . ? C27 C26 1.470(10) . ? C28 C29 1.3900 . ? C28 H28 0.9300 . ? C29 C30 1.3900 . ? C29 H29 0.9300 . ? C30 C31 1.3900 . ? C30 H30 0.9300 . ? C31 C32 1.3900 . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C1 C2 1.3900 . ? C1 C6 1.3900 . ? C1 H1 0.9300 . ? C2 C3 1.3900 . ? C2 H2 0.9300 . ? C3 C4 1.3900 . ? C3 H3 0.9300 . ? C4 C5 1.3900 . ? C4 H4 0.9300 . ? C5 C6 1.3900 . ? C5 H5 0.9300 . ? C6 C7 1.494(10) . ? Pr1 O5 2.347(7) . ? Pr1 O11 2.385(9) . ? Pr1 O15 2.395(7) 2_655 ? Pr1 O22 2.514(10) . ? Pr1 O24 2.525(13) . ? Pr1 O19 2.548(8) . ? Pr1 O18 2.554(7) . ? Pr1 O21 2.562(8) . ? Pr1 O16 2.577(7) . ? Pr2 O10 2.365(8) 2_546 ? Pr2 O1 2.388(6) . ? Pr2 O6 2.430(7) . ? Pr2 O28 2.521(6) . ? Pr2 O27 2.539(8) . ? Pr2 O25 2.550(7) . ? Pr2 O30 2.551(7) . ? Pr2 O31 2.551(7) . ? Pr2 O33 2.571(10) . ? C7 N1 1.419(10) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 O1 1.282(9) . ? C8 N1 1.320(10) . ? C8 C9 1.505(13) . ? C9 C10 1.353(13) . ? C9 C14 1.384(12) . ? C10 C11 1.377(12) . ? C10 H10 0.9300 . ? C11 C12 1.357(13) . ? C11 H11 0.9300 . ? C12 C13 1.341(13) . ? C12 H12 0.9300 . ? C13 C14 1.377(12) . ? C13 H13 0.9300 . ? C14 O2 1.343(10) . ? C15 O2 1.416(10) . ? C15 C16 1.518(12) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 O3 1.372(11) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 O3 1.423(11) . ? C17 C18 1.464(12) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 O4 1.389(10) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 O4 1.336(10) . ? C19 C20 1.353(11) . ? C19 C24 1.425(12) . ? C20 C21 1.353(12) . ? C20 H20 0.9300 . ? C21 C22 1.441(13) . ? C21 H21 0.9300 . ? C22 C23 1.367(13) . ? C22 H22 0.9300 . ? C23 C24 1.307(12) . ? C23 H23 0.9300 . ? C24 C25 1.505(13) . ? C25 O5 1.258(10) . ? C25 N2 1.280(10) . ? C26 N2 1.432(10) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C33 C38 1.308(13) . ? C33 C34 1.404(14) . ? C33 H33 0.9300 . ? C34 C35 1.358(14) . ? C34 H34 0.9300 . ? C35 C36 1.333(14) . ? C35 H35 0.9300 . ? C36 C37 1.343(13) . ? C36 H36 0.9300 . ? C37 C38 1.370(13) . ? C37 H37 0.9300 . ? C38 C39 1.547(12) . ? C39 N3 1.463(10) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 O6 1.256(10) . ? C40 N3 1.314(10) . ? C40 C41 1.525(12) . ? C41 C42 1.363(13) . ? C41 C46 1.395(12) . ? C42 C43 1.409(14) . ? C42 H42 0.9300 . ? C43 C44 1.348(14) . ? C43 H43 0.9300 . ? C44 C45 1.384(13) . ? C44 H44 0.9300 . ? C45 C46 1.350(13) . ? C45 H45 0.9300 . ? C46 O7 1.342(12) . ? C47 O7 1.429(9) . ? C47 C48 1.435(11) . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C48 O8 1.424(11) . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C49 O8 1.430(11) . ? C49 C50 1.467(11) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 O9 1.418(9) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C51 C56 1.376(12) . ? C51 O9 1.396(11) . ? C51 C52 1.470(14) . ? C52 C53 1.379(14) . ? C52 H52 0.9300 . ? C53 C54 1.299(16) . ? C53 H53 0.9300 . ? C54 C55 1.382(16) . ? C54 H54 0.9300 . ? C55 C56 1.396(13) . ? C55 H55 0.9300 . ? C56 C57 1.469(13) . ? C57 O10 1.248(11) . ? C57 N4 1.281(11) . ? C58 C59 1.428(11) . ? C58 N4 1.449(12) . ? C58 H58A 0.9700 . ? C58 H58B 0.9700 . ? C59 C60 1.3900 . ? C59 C64 1.3900 . ? C60 C61 1.3900 . ? C60 H60 0.9300 . ? C61 C62 1.3900 . ? C61 H61 0.9300 . ? C62 C63 1.3900 . ? C62 H62 0.9300 . ? C63 C64 1.3900 . ? C63 H63 0.9300 . ? C64 H64 0.9300 . ? C65 C66 1.3900 . ? C65 C70 1.3900 . ? C65 H65 0.9300 . ? C66 C67 1.3900 . ? C66 H66 0.9300 . ? C67 C68 1.3900 . ? C67 H67 0.9300 . ? C68 C69 1.3900 . ? C68 H68 0.9300 . ? C69 C70 1.3900 . ? C69 H69 0.9300 . ? C70 C71 1.526(13) . ? C71 N5 1.547(16) . ? C71 H71A 0.9700 . ? C71 H71B 0.9700 . ? C72 O11 1.248(13) . ? C72 N5 1.258(14) . ? C72 C73 1.517(15) . ? C73 C78 1.364(13) . ? C73 C74 1.397(15) . ? C74 C75 1.410(18) . ? C74 H74 0.9300 . ? C75 C76 1.275(19) . ? C75 H75 0.9300 . ? C76 C77 1.249(17) . ? C76 H76 0.9300 . ? C77 C78 1.423(15) . ? C77 H77 0.9300 . ? C78 O12 1.345(12) . ? C79 O12 1.394(12) . ? C79 C80 1.487(16) . ? C79 H79A 0.9700 . ? C79 H79B 0.9700 . ? C80 O13 1.432(13) . ? C80 H80A 0.9700 . ? C80 H80B 0.9700 . ? C81 O13 1.435(12) . ? C81 C82 1.445(14) . ? C81 H81A 0.9700 . ? C81 H81B 0.9700 . ? C82 O14 1.429(11) . ? C82 H82A 0.9700 . ? C82 H82B 0.9700 . ? C83 O14 1.350(10) . ? C83 C88 1.371(12) . ? C83 C84 1.415(11) . ? C84 C85 1.337(11) . ? C84 C89 1.547(12) . ? C85 C86 1.396(12) . ? C85 H85 0.9300 . ? C86 C87 1.374(13) . ? C86 H86 0.9300 . ? C87 C88 1.374(13) . ? C87 H87 0.9300 . ? C88 H88 0.9300 . ? C89 N6 1.281(11) . ? C89 O15 1.292(10) . ? C90 N6 1.444(12) . ? C90 C91 1.448(18) . ? C90 H90A 0.9700 . ? C90 H90B 0.9700 . ? C91 C96 1.248(18) . ? C91 C92 1.416(17) . ? C92 C93 1.406(17) . ? C92 H92 0.9300 . ? C93 C94 1.246(18) . ? C93 H93 0.9300 . ? C94 C95 1.459(18) . ? C94 H94 0.9300 . ? C95 C96 1.358(18) . ? C95 H95 0.9300 . ? C96 H96 0.9300 . ? N1 H1A 0.8600 . ? N2 H2A 0.8600 . ? N3 H3A 0.8600 . ? N4 H4A 0.8600 . ? N5 H5A 0.8600 . ? N6 H6 0.8600 . ? N7 O17 1.155(10) . ? N7 O18 1.261(12) . ? N7 O16 1.295(10) . ? N8 O20 1.217(12) . ? N8 O21 1.289(12) . ? N8 O19 1.294(12) . ? N9 O24 1.193(19) . ? N9 O23 1.242(17) . ? N9 O22 1.300(19) . ? N10 O26 1.207(12) . ? N10 O27 1.260(12) . ? N10 O25 1.281(10) . ? N11 O29 1.216(13) . ? N11 O30 1.252(11) . ? N11 O28 1.254(12) . ? N12 O32 1.197(14) . ? N12 O31 1.247(12) . ? N12 O33 1.277(13) . ? O10 Pr2 2.365(8) 2_556 ? O15 Pr1 2.395(7) 2_645 ? 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 C28 C27 C32 120.0 . . ? C28 C27 C26 115.7(9) . . ? C32 C27 C26 124.2(9) . . ? C27 C28 C29 120.0 . . ? C27 C28 H28 120.0 . . ? C29 C28 H28 120.0 . . ? C30 C29 C28 120.0 . . ? C30 C29 H29 120.0 . . ? C28 C29 H29 120.0 . . ? C29 C30 C31 120.0 . . ? C29 C30 H30 120.0 . . ? C31 C30 H30 120.0 . . ? C32 C31 C30 120.0 . . ? C32 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? C31 C32 C27 120.0 . . ? C31 C32 H32 120.0 . . ? C27 C32 H32 120.0 . . ? C2 C1 C6 120.0 . . ? C2 C1 H1 120.0 . . ? C6 C1 H1 120.0 . . ? C1 C2 C3 120.0 . . ? C1 C2 H2 120.0 . . ? C3 C2 H2 120.0 . . ? C2 C3 C4 120.0 . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C5 C4 C3 120.0 . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C6 C5 C4 120.0 . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C5 C6 C1 120.0 . . ? C5 C6 C7 117.3(8) . . ? C1 C6 C7 122.3(8) . . ? O5 Pr1 O11 84.2(2) . . ? O5 Pr1 O15 153.8(2) . 2_655 ? O11 Pr1 O15 85.8(2) . 2_655 ? O5 Pr1 O22 84.4(3) . . ? O11 Pr1 O22 125.2(3) . . ? O15 Pr1 O22 81.8(3) 2_655 . ? O5 Pr1 O24 75.5(4) . . ? O11 Pr1 O24 75.2(3) . . ? O15 Pr1 O24 78.6(4) 2_655 . ? O22 Pr1 O24 50.0(4) . . ? O5 Pr1 O19 70.3(3) . . ? O11 Pr1 O19 147.2(3) . . ? O15 Pr1 O19 125.8(3) 2_655 . ? O22 Pr1 O19 73.8(3) . . ? O24 Pr1 O19 115.9(3) . . ? O5 Pr1 O18 126.1(2) . . ? O11 Pr1 O18 82.9(3) . . ? O15 Pr1 O18 76.4(2) 2_655 . ? O22 Pr1 O18 142.9(3) . . ? O24 Pr1 O18 147.7(3) . . ? O19 Pr1 O18 95.3(3) . . ? O5 Pr1 O21 119.2(3) . . ? O11 Pr1 O21 154.7(3) . . ? O15 Pr1 O21 76.5(3) 2_655 . ? O22 Pr1 O21 70.4(3) . . ? O24 Pr1 O21 117.7(4) . . ? O19 Pr1 O21 50.0(3) . . ? O18 Pr1 O21 75.5(3) . . ? O5 Pr1 O16 77.7(2) . . ? O11 Pr1 O16 83.0(3) . . ? O15 Pr1 O16 125.0(2) 2_655 . ? O22 Pr1 O16 144.8(3) . . ? O24 Pr1 O16 146.8(4) . . ? O19 Pr1 O16 71.8(3) . . ? O18 Pr1 O16 48.9(2) . . ? O21 Pr1 O16 92.4(3) . . ? O10 Pr2 O1 153.1(2) 2_546 . ? O10 Pr2 O6 80.8(3) 2_546 . ? O1 Pr2 O6 82.0(2) . . ? O10 Pr2 O28 124.8(3) 2_546 . ? O1 Pr2 O28 78.0(2) . . ? O6 Pr2 O28 150.8(2) . . ? O10 Pr2 O27 92.0(2) 2_546 . ? O1 Pr2 O27 81.9(2) . . ? O6 Pr2 O27 126.6(2) . . ? O28 Pr2 O27 71.2(3) . . ? O10 Pr2 O25 76.0(3) 2_546 . ? O1 Pr2 O25 80.3(2) . . ? O6 Pr2 O25 78.0(2) . . ? O28 Pr2 O25 118.7(3) . . ? O27 Pr2 O25 49.2(2) . . ? O10 Pr2 O30 76.1(3) 2_546 . ? O1 Pr2 O30 123.6(3) . . ? O6 Pr2 O30 154.3(3) . . ? O28 Pr2 O30 48.9(3) . . ? O27 Pr2 O30 66.1(3) . . ? O25 Pr2 O30 106.9(3) . . ? O10 Pr2 O31 119.4(2) 2_546 . ? O1 Pr2 O31 77.5(2) . . ? O6 Pr2 O31 80.5(2) . . ? O28 Pr2 O31 74.7(2) . . ? O27 Pr2 O31 143.1(2) . . ? O25 Pr2 O31 150.9(3) . . ? O30 Pr2 O31 101.0(3) . . ? O10 Pr2 O33 73.8(3) 2_546 . ? O1 Pr2 O33 126.5(3) . . ? O6 Pr2 O33 89.4(3) . . ? O28 Pr2 O33 85.8(3) . . ? O27 Pr2 O33 139.3(3) . . ? O25 Pr2 O33 148.7(3) . . ? O30 Pr2 O33 73.4(3) . . ? O31 Pr2 O33 49.0(3) . . ? N1 C7 C6 111.4(8) . . ? N1 C7 H7A 109.3 . . ? C6 C7 H7A 109.3 . . ? N1 C7 H7B 109.3 . . ? C6 C7 H7B 109.3 . . ? H7A C7 H7B 108.0 . . ? O1 C8 N1 118.3(9) . . ? O1 C8 C9 118.9(9) . . ? N1 C8 C9 122.7(9) . . ? C10 C9 C14 118.6(10) . . ? C10 C9 C8 119.2(10) . . ? C14 C9 C8 122.2(10) . . ? C9 C10 C11 124.4(11) . . ? C9 C10 H10 117.8 . . ? C11 C10 H10 117.8 . . ? C12 C11 C10 113.6(11) . . ? C12 C11 H11 123.2 . . ? C10 C11 H11 123.2 . . ? C13 C12 C11 126.0(11) . . ? C13 C12 H12 117.0 . . ? C11 C12 H12 117.0 . . ? C12 C13 C14 118.4(11) . . ? C12 C13 H13 120.8 . . ? C14 C13 H13 120.8 . . ? O2 C14 C13 122.1(10) . . ? O2 C14 C9 118.8(10) . . ? C13 C14 C9 119.1(10) . . ? O2 C15 C16 107.3(8) . . ? O2 C15 H15A 110.3 . . ? C16 C15 H15A 110.3 . . ? O2 C15 H15B 110.3 . . ? C16 C15 H15B 110.3 . . ? H15A C15 H15B 108.5 . . ? O3 C16 C15 107.5(10) . . ? O3 C16 H16A 110.2 . . ? C15 C16 H16A 110.2 . . ? O3 C16 H16B 110.2 . . ? C15 C16 H16B 110.2 . . ? H16A C16 H16B 108.5 . . ? O3 C17 C18 111.8(10) . . ? O3 C17 H17A 109.3 . . ? C18 C17 H17A 109.3 . . ? O3 C17 H17B 109.3 . . ? C18 C17 H17B 109.3 . . ? H17A C17 H17B 107.9 . . ? O4 C18 C17 112.9(8) . . ? O4 C18 H18A 109.0 . . ? C17 C18 H18A 109.0 . . ? O4 C18 H18B 109.0 . . ? C17 C18 H18B 109.0 . . ? H18A C18 H18B 107.8 . . ? O4 C19 C20 121.9(9) . . ? O4 C19 C24 119.3(9) . . ? C20 C19 C24 118.8(9) . . ? C21 C20 C19 122.7(10) . . ? C21 C20 H20 118.6 . . ? C19 C20 H20 118.6 . . ? C20 C21 C22 117.5(10) . . ? C20 C21 H21 121.3 . . ? C22 C21 H21 121.3 . . ? C23 C22 C21 118.6(10) . . ? C23 C22 H22 120.7 . . ? C21 C22 H22 120.7 . . ? C24 C23 C22 122.9(10) . . ? C24 C23 H23 118.6 . . ? C22 C23 H23 118.6 . . ? C23 C24 C19 119.5(10) . . ? C23 C24 C25 116.9(10) . . ? C19 C24 C25 123.5(9) . . ? O5 C25 N2 119.4(10) . . ? O5 C25 C24 119.5(9) . . ? N2 C25 C24 121.1(9) . . ? N2 C26 C27 115.1(7) . . ? N2 C26 H26A 108.5 . . ? C27 C26 H26A 108.5 . . ? N2 C26 H26B 108.5 . . ? C27 C26 H26B 108.5 . . ? H26A C26 H26B 107.5 . . ? C38 C33 C34 116.7(12) . . ? C38 C33 H33 121.7 . . ? C34 C33 H33 121.7 . . ? C35 C34 C33 122.4(12) . . ? C35 C34 H34 118.8 . . ? C33 C34 H34 118.8 . . ? C36 C35 C34 117.4(13) . . ? C36 C35 H35 121.3 . . ? C34 C35 H35 121.3 . . ? C35 C36 C37 121.6(13) . . ? C35 C36 H36 119.2 . . ? C37 C36 H36 119.2 . . ? C36 C37 C38 119.6(12) . . ? C36 C37 H37 120.2 . . ? C38 C37 H37 120.2 . . ? C33 C38 C37 121.9(11) . . ? C33 C38 C39 122.2(13) . . ? C37 C38 C39 115.6(13) . . ? N3 C39 C38 113.4(8) . . ? N3 C39 H39A 108.9 . . ? C38 C39 H39A 108.9 . . ? N3 C39 H39B 108.9 . . ? C38 C39 H39B 108.9 . . ? H39A C39 H39B 107.7 . . ? O6 C40 N3 121.7(9) . . ? O6 C40 C41 120.3(10) . . ? N3 C40 C41 118.0(10) . . ? C42 C41 C46 120.5(11) . . ? C42 C41 C40 116.4(12) . . ? C46 C41 C40 123.1(10) . . ? C41 C42 C43 119.6(11) . . ? C41 C42 H42 120.2 . . ? C43 C42 H42 120.2 . . ? C44 C43 C42 119.9(12) . . ? C44 C43 H43 120.0 . . ? C42 C43 H43 120.0 . . ? C43 C44 C45 119.1(12) . . ? C43 C44 H44 120.5 . . ? C45 C44 H44 120.5 . . ? C46 C45 C44 122.6(12) . . ? C46 C45 H45 118.7 . . ? C44 C45 H45 118.7 . . ? O7 C46 C45 123.3(11) . . ? O7 C46 C41 118.5(10) . . ? C45 C46 C41 118.2(12) . . ? O7 C47 C48 104.6(8) . . ? O7 C47 H47A 110.8 . . ? C48 C47 H47A 110.8 . . ? O7 C47 H47B 110.8 . . ? C48 C47 H47B 110.8 . . ? H47A C47 H47B 108.9 . . ? O8 C48 C47 111.7(10) . . ? O8 C48 H48A 109.3 . . ? C47 C48 H48A 109.3 . . ? O8 C48 H48B 109.3 . . ? C47 C48 H48B 109.3 . . ? H48A C48 H48B 107.9 . . ? O8 C49 C50 110.0(9) . . ? O8 C49 H49A 109.7 . . ? C50 C49 H49A 109.7 . . ? O8 C49 H49B 109.7 . . ? C50 C49 H49B 109.7 . . ? H49A C49 H49B 108.2 . . ? O9 C50 C49 107.2(8) . . ? O9 C50 H50A 110.3 . . ? C49 C50 H50A 110.3 . . ? O9 C50 H50B 110.3 . . ? C49 C50 H50B 110.3 . . ? H50A C50 H50B 108.5 . . ? C56 C51 O9 116.8(11) . . ? C56 C51 C52 119.0(11) . . ? O9 C51 C52 124.2(10) . . ? C53 C52 C51 119.8(11) . . ? C53 C52 H52 120.1 . . ? C51 C52 H52 120.1 . . ? C54 C53 C52 121.9(16) . . ? C54 C53 H53 119.1 . . ? C52 C53 H53 119.1 . . ? C53 C54 C55 117.8(16) . . ? C53 C54 H54 121.1 . . ? C55 C54 H54 121.1 . . ? C54 C55 C56 126.6(12) . . ? C54 C55 H55 116.7 . . ? C56 C55 H55 116.7 . . ? C51 C56 C55 114.8(11) . . ? C51 C56 C57 126.7(12) . . ? C55 C56 C57 118.3(11) . . ? O10 C57 N4 122.8(11) . . ? O10 C57 C56 117.9(11) . . ? N4 C57 C56 119.3(11) . . ? C59 C58 N4 111.5(9) . . ? C59 C58 H58A 109.3 . . ? N4 C58 H58A 109.3 . . ? C59 C58 H58B 109.3 . . ? N4 C58 H58B 109.3 . . ? H58A C58 H58B 108.0 . . ? C60 C59 C64 120.0 . . ? C60 C59 C58 135.3(8) . . ? C64 C59 C58 104.7(8) . . ? C59 C60 C61 120.0 . . ? C59 C60 H60 120.0 . . ? C61 C60 H60 120.0 . . ? C62 C61 C60 120.0 . . ? C62 C61 H61 120.0 . . ? C60 C61 H61 120.0 . . ? C61 C62 C63 120.0 . . ? C61 C62 H62 120.0 . . ? C63 C62 H62 120.0 . . ? C62 C63 C64 120.0 . . ? C62 C63 H63 120.0 . . ? C64 C63 H63 120.0 . . ? C63 C64 C59 120.0 . . ? C63 C64 H64 120.0 . . ? C59 C64 H64 120.0 . . ? C66 C65 C70 120.0 . . ? C66 C65 H65 120.0 . . ? C70 C65 H65 120.0 . . ? C65 C66 C67 120.0 . . ? C65 C66 H66 120.0 . . ? C67 C66 H66 120.0 . . ? C68 C67 C66 120.0 . . ? C68 C67 H67 120.0 . . ? C66 C67 H67 120.0 . . ? C67 C68 C69 120.0 . . ? C67 C68 H68 120.0 . . ? C69 C68 H68 120.0 . . ? C70 C69 C68 120.0 . . ? C70 C69 H69 120.0 . . ? C68 C69 H69 120.0 . . ? C69 C70 C65 120.0 . . ? C69 C70 C71 115.1(7) . . ? C65 C70 C71 124.4(7) . . ? C70 C71 N5 108.1(10) . . ? C70 C71 H71A 110.1 . . ? N5 C71 H71A 110.1 . . ? C70 C71 H71B 110.1 . . ? N5 C71 H71B 110.1 . . ? H71A C71 H71B 108.4 . . ? O11 C72 N5 121.8(14) . . ? O11 C72 C73 121.6(13) . . ? N5 C72 C73 116.6(14) . . ? C78 C73 C74 118.0(12) . . ? C78 C73 C72 123.6(13) . . ? C74 C73 C72 118.4(14) . . ? C73 C74 C75 119.4(14) . . ? C73 C74 H74 120.3 . . ? C75 C74 H74 120.3 . . ? C76 C75 C74 118.4(18) . . ? C76 C75 H75 120.8 . . ? C74 C75 H75 120.8 . . ? C77 C76 C75 125(2) . . ? C77 C76 H76 117.4 . . ? C75 C76 H76 117.4 . . ? C76 C77 C78 121.3(16) . . ? C76 C77 H77 119.3 . . ? C78 C77 H77 119.3 . . ? O12 C78 C73 119.1(12) . . ? O12 C78 C77 123.4(14) . . ? C73 C78 C77 117.5(13) . . ? O12 C79 C80 109.4(13) . . ? O12 C79 H79A 109.8 . . ? C80 C79 H79A 109.8 . . ? O12 C79 H79B 109.8 . . ? C80 C79 H79B 109.8 . . ? H79A C79 H79B 108.2 . . ? O13 C80 C79 106.8(11) . . ? O13 C80 H80A 110.4 . . ? C79 C80 H80A 110.4 . . ? O13 C80 H80B 110.4 . . ? C79 C80 H80B 110.4 . . ? H80A C80 H80B 108.6 . . ? O13 C81 C82 109.0(10) . . ? O13 C81 H81A 109.9 . . ? C82 C81 H81A 109.9 . . ? O13 C81 H81B 109.9 . . ? C82 C81 H81B 109.9 . . ? H81A C81 H81B 108.3 . . ? O14 C82 C81 108.5(10) . . ? O14 C82 H82A 110.0 . . ? C81 C82 H82A 110.0 . . ? O14 C82 H82B 110.0 . . ? C81 C82 H82B 110.0 . . ? H82A C82 H82B 108.4 . . ? O14 C83 C88 121.2(9) . . ? O14 C83 C84 120.3(9) . . ? C88 C83 C84 118.5(10) . . ? C85 C84 C83 120.7(10) . . ? C85 C84 C89 119.5(9) . . ? C83 C84 C89 119.7(9) . . ? C84 C85 C86 121.0(10) . . ? C84 C85 H85 119.5 . . ? C86 C85 H85 119.5 . . ? C87 C86 C85 118.0(10) . . ? C87 C86 H86 121.0 . . ? C85 C86 H86 121.0 . . ? C88 C87 C86 121.6(11) . . ? C88 C87 H87 119.2 . . ? C86 C87 H87 119.2 . . ? C83 C88 C87 120.0(10) . . ? C83 C88 H88 120.0 . . ? C87 C88 H88 120.0 . . ? N6 C89 O15 123.6(9) . . ? N6 C89 C84 121.8(9) . . ? O15 C89 C84 114.6(9) . . ? N6 C90 C91 111.3(12) . . ? N6 C90 H90A 109.4 . . ? C91 C90 H90A 109.4 . . ? N6 C90 H90B 109.4 . . ? C91 C90 H90B 109.4 . . ? H90A C90 H90B 108.0 . . ? C96 C91 C92 117(2) . . ? C96 C91 C90 120.0(19) . . ? C92 C91 C90 122.8(17) . . ? C93 C92 C91 121.2(17) . . ? C93 C92 H92 119.4 . . ? C91 C92 H92 119.4 . . ? C94 C93 C92 119.9(19) . . ? C94 C93 H93 120.0 . . ? C92 C93 H93 120.0 . . ? C93 C94 C95 119.2(18) . . ? C93 C94 H94 120.4 . . ? C95 C94 H94 120.4 . . ? C96 C95 C94 118.3(17) . . ? C96 C95 H95 120.9 . . ? C94 C95 H95 120.9 . . ? C91 C96 C95 124(2) . . ? C91 C96 H96 118.0 . . ? C95 C96 H96 118.0 . . ? C8 N1 C7 127.9(8) . . ? C8 N1 H1A 116.1 . . ? C7 N1 H1A 116.1 . . ? C25 N2 C26 127.1(8) . . ? C25 N2 H2A 116.5 . . ? C26 N2 H2A 116.5 . . ? C40 N3 C39 123.7(8) . . ? C40 N3 H3A 118.2 . . ? C39 N3 H3A 118.2 . . ? C57 N4 C58 121.2(9) . . ? C57 N4 H4A 119.4 . . ? C58 N4 H4A 119.4 . . ? C72 N5 C71 127.2(13) . . ? C72 N5 H5A 116.4 . . ? C71 N5 H5A 116.4 . . ? C89 N6 C90 124.5(9) . . ? C89 N6 H6 117.8 . . ? C90 N6 H6 117.8 . . ? O17 N7 O18 125.7(12) . . ? O17 N7 O16 122.0(13) . . ? O18 N7 O16 112.2(10) . . ? O20 N8 O21 124.1(14) . . ? O20 N8 O19 122.2(13) . . ? O21 N8 O19 113.4(13) . . ? O24 N9 O23 126(2) . . ? O24 N9 O22 117.5(19) . . ? O23 N9 O22 116(2) . . ? O26 N10 O27 124.6(12) . . ? O26 N10 O25 122.4(12) . . ? O27 N10 O25 113.0(11) . . ? O29 N11 O30 120.2(14) . . ? O29 N11 O28 125.9(12) . . ? O30 N11 O28 113.6(12) . . ? O32 N12 O31 120.9(15) . . ? O32 N12 O33 124.2(13) . . ? O31 N12 O33 114.8(13) . . ? C8 O1 Pr2 173.0(6) . . ? C14 O2 C15 119.9(8) . . ? C16 O3 C17 114.3(9) . . ? C19 O4 C18 121.5(8) . . ? C25 O5 Pr1 169.0(6) . . ? C40 O6 Pr2 177.3(6) . . ? C46 O7 C47 118.3(8) . . ? C48 O8 C49 112.4(8) . . ? C51 O9 C50 118.8(8) . . ? C57 O10 Pr2 164.9(7) . 2_556 ? C72 O11 Pr1 166.2(8) . . ? C78 O12 C79 121.4(11) . . ? C80 O13 C81 109.9(10) . . ? C83 O14 C82 122.3(9) . . ? C89 O15 Pr1 168.8(6) . 2_645 ? N7 O16 Pr1 98.4(7) . . ? N7 O18 Pr1 100.5(7) . . ? N8 O19 Pr1 98.0(8) . . ? N8 O21 Pr1 97.5(8) . . ? N9 O22 Pr1 94.7(11) . . ? N9 O24 Pr1 97.2(14) . . ? N10 O25 Pr2 98.2(7) . . ? N10 O27 Pr2 99.4(7) . . ? N11 O28 Pr2 99.3(7) . . ? N11 O30 Pr2 97.8(8) . . ? N12 O31 Pr2 99.0(9) . . ? N12 O33 Pr2 97.2(8) . . ? 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 C32 C27 C28 C29 0.0 . . . . ? C26 C27 C28 C29 175.8(6) . . . . ? C27 C28 C29 C30 0.0 . . . . ? C28 C29 C30 C31 0.0 . . . . ? C29 C30 C31 C32 0.0 . . . . ? C30 C31 C32 C27 0.0 . . . . ? C28 C27 C32 C31 0.0 . . . . ? C26 C27 C32 C31 -175.4(7) . . . . ? C6 C1 C2 C3 0.0 . . . . ? C1 C2 C3 C4 0.0 . . . . ? C2 C3 C4 C5 0.0 . . . . ? C3 C4 C5 C6 0.0 . . . . ? C4 C5 C6 C1 0.0 . . . . ? C4 C5 C6 C7 172.9(7) . . . . ? C2 C1 C6 C5 0.0 . . . . ? C2 C1 C6 C7 -172.6(7) . . . . ? C5 C6 C7 N1 -82.0(8) . . . . ? C1 C6 C7 N1 90.7(9) . . . . ? O1 C8 C9 C10 -5.2(14) . . . . ? N1 C8 C9 C10 174.6(9) . . . . ? O1 C8 C9 C14 175.6(8) . . . . ? N1 C8 C9 C14 -4.6(14) . . . . ? C14 C9 C10 C11 0.8(16) . . . . ? C8 C9 C10 C11 -178.4(9) . . . . ? C9 C10 C11 C12 -1.5(17) . . . . ? C10 C11 C12 C13 1.3(18) . . . . ? C11 C12 C13 C14 -0.3(19) . . . . ? C12 C13 C14 O2 179.7(10) . . . . ? C12 C13 C14 C9 -0.5(15) . . . . ? C10 C9 C14 O2 -179.9(9) . . . . ? C8 C9 C14 O2 -0.7(14) . . . . ? C10 C9 C14 C13 0.3(14) . . . . ? C8 C9 C14 C13 179.5(9) . . . . ? O2 C15 C16 O3 74.9(11) . . . . ? O3 C17 C18 O4 64.6(12) . . . . ? O4 C19 C20 C21 176.5(10) . . . . ? C24 C19 C20 C21 -0.6(16) . . . . ? C19 C20 C21 C22 0.5(18) . . . . ? C20 C21 C22 C23 -1.1(18) . . . . ? C21 C22 C23 C24 2(2) . . . . ? C22 C23 C24 C19 -2.0(19) . . . . ? C22 C23 C24 C25 -178.3(11) . . . . ? O4 C19 C24 C23 -175.9(11) . . . . ? C20 C19 C24 C23 1.3(16) . . . . ? O4 C19 C24 C25 0.2(15) . . . . ? C20 C19 C24 C25 177.4(10) . . . . ? C23 C24 C25 O5 -11.9(16) . . . . ? C19 C24 C25 O5 172.0(9) . . . . ? C23 C24 C25 N2 170.6(11) . . . . ? C19 C24 C25 N2 -5.6(17) . . . . ? C28 C27 C26 N2 -80.1(9) . . . . ? C32 C27 C26 N2 95.5(9) . . . . ? C38 C33 C34 C35 -0.7(19) . . . . ? C33 C34 C35 C36 5(2) . . . . ? C34 C35 C36 C37 -6(2) . . . . ? C35 C36 C37 C38 2.7(19) . . . . ? C34 C33 C38 C37 -3.2(18) . . . . ? C34 C33 C38 C39 -177.2(10) . . . . ? C36 C37 C38 C33 2.4(18) . . . . ? C36 C37 C38 C39 176.7(10) . . . . ? C33 C38 C39 N3 -31.8(15) . . . . ? C37 C38 C39 N3 153.9(9) . . . . ? O6 C40 C41 C42 18.0(12) . . . . ? N3 C40 C41 C42 -159.9(9) . . . . ? O6 C40 C41 C46 -163.3(9) . . . . ? N3 C40 C41 C46 18.9(12) . . . . ? C46 C41 C42 C43 -1.9(15) . . . . ? C40 C41 C42 C43 176.9(10) . . . . ? C41 C42 C43 C44 -1(2) . . . . ? C42 C43 C44 C45 4(2) . . . . ? C43 C44 C45 C46 -6(2) . . . . ? C44 C45 C46 O7 -178.8(11) . . . . ? C44 C45 C46 C41 3.0(19) . . . . ? C42 C41 C46 O7 -177.5(9) . . . . ? C40 C41 C46 O7 3.8(13) . . . . ? C42 C41 C46 C45 0.8(15) . . . . ? C40 C41 C46 C45 -177.9(10) . . . . ? O7 C47 C48 O8 -62.6(12) . . . . ? O8 C49 C50 O9 -73.4(10) . . . . ? C56 C51 C52 C53 -0.1(16) . . . . ? O9 C51 C52 C53 177.9(10) . . . . ? C51 C52 C53 C54 -1(2) . . . . ? C52 C53 C54 C55 2(2) . . . . ? C53 C54 C55 C56 -1(2) . . . . ? O9 C51 C56 C55 -177.1(9) . . . . ? C52 C51 C56 C55 1.1(14) . . . . ? O9 C51 C56 C57 -1.3(15) . . . . ? C52 C51 C56 C57 176.8(10) . . . . ? C54 C55 C56 C51 -0.7(18) . . . . ? C54 C55 C56 C57 -176.8(13) . . . . ? C51 C56 C57 O10 -175.9(10) . . . . ? C55 C56 C57 O10 -0.3(15) . . . . ? C51 C56 C57 N4 5.1(17) . . . . ? C55 C56 C57 N4 -179.3(10) . . . . ? N4 C58 C59 C60 88.0(12) . . . . ? N4 C58 C59 C64 -93.8(11) . . . . ? C64 C59 C60 C61 0.0 . . . . ? C58 C59 C60 C61 178.0(8) . . . . ? C59 C60 C61 C62 0.0 . . . . ? C60 C61 C62 C63 0.0 . . . . ? C61 C62 C63 C64 0.0 . . . . ? C62 C63 C64 C59 0.0 . . . . ? C60 C59 C64 C63 0.0 . . . . ? C58 C59 C64 C63 -178.5(6) . . . . ? C70 C65 C66 C67 0.0 . . . . ? C65 C66 C67 C68 0.0 . . . . ? C66 C67 C68 C69 0.0 . . . . ? C67 C68 C69 C70 0.0 . . . . ? C68 C69 C70 C65 0.0 . . . . ? C68 C69 C70 C71 171.9(6) . . . . ? C66 C65 C70 C69 0.0 . . . . ? C66 C65 C70 C71 -171.1(7) . . . . ? C69 C70 C71 N5 54.8(11) . . . . ? C65 C70 C71 N5 -133.7(8) . . . . ? O11 C72 C73 C78 -171.8(10) . . . . ? N5 C72 C73 C78 10.9(16) . . . . ? O11 C72 C73 C74 5.8(15) . . . . ? N5 C72 C73 C74 -171.4(11) . . . . ? C78 C73 C74 C75 4.0(15) . . . . ? C72 C73 C74 C75 -173.8(10) . . . . ? C73 C74 C75 C76 -5(2) . . . . ? C74 C75 C76 C77 3(3) . . . . ? C75 C76 C77 C78 -1(3) . . . . ? C74 C73 C78 O12 177.9(9) . . . . ? C72 C73 C78 O12 -4.4(15) . . . . ? C74 C73 C78 C77 -2.1(14) . . . . ? C72 C73 C78 C77 175.6(9) . . . . ? C76 C77 C78 O12 -179.3(13) . . . . ? C76 C77 C78 C73 0.7(18) . . . . ? O12 C79 C80 O13 68.3(13) . . . . ? O13 C81 C82 O14 65.6(11) . . . . ? O14 C83 C84 C85 -177.5(9) . . . . ? C88 C83 C84 C85 0.6(14) . . . . ? O14 C83 C84 C89 -0.2(13) . . . . ? C88 C83 C84 C89 177.9(9) . . . . ? C83 C84 C85 C86 -3.0(15) . . . . ? C89 C84 C85 C86 179.7(9) . . . . ? C84 C85 C86 C87 5.3(16) . . . . ? C85 C86 C87 C88 -5.4(17) . . . . ? O14 C83 C88 C87 177.4(10) . . . . ? C84 C83 C88 C87 -0.7(16) . . . . ? C86 C87 C88 C83 3.2(18) . . . . ? C85 C84 C89 N6 166.8(10) . . . . ? C83 C84 C89 N6 -10.6(14) . . . . ? C85 C84 C89 O15 -12.7(14) . . . . ? C83 C84 C89 O15 170.0(8) . . . . ? N6 C90 C91 C96 -51(2) . . . . ? N6 C90 C91 C92 124.7(14) . . . . ? C96 C91 C92 C93 -3(2) . . . . ? C90 C91 C92 C93 -178.6(13) . . . . ? C91 C92 C93 C94 -2(2) . . . . ? C92 C93 C94 C95 2(3) . . . . ? C93 C94 C95 C96 3(2) . . . . ? C92 C91 C96 C95 8(3) . . . . ? C90 C91 C96 C95 -176.2(13) . . . . ? C94 C95 C96 C91 -8(3) . . . . ? O1 C8 N1 C7 -3.9(15) . . . . ? C9 C8 N1 C7 176.4(9) . . . . ? C6 C7 N1 C8 -105.0(11) . . . . ? O5 C25 N2 C26 4.4(17) . . . . ? C24 C25 N2 C26 -178.0(10) . . . . ? C27 C26 N2 C25 142.0(11) . . . . ? O6 C40 N3 C39 -7.1(14) . . . . ? C41 C40 N3 C39 170.8(8) . . . . ? C38 C39 N3 C40 -99.1(11) . . . . ? O10 C57 N4 C58 5.8(18) . . . . ? C56 C57 N4 C58 -175.2(11) . . . . ? C59 C58 N4 C57 -143.4(11) . . . . ? O11 C72 N5 C71 23(2) . . . . ? C73 C72 N5 C71 -159.4(11) . . . . ? C70 C71 N5 C72 -124.0(14) . . . . ? O15 C89 N6 C90 -6.3(19) . . . . ? C84 C89 N6 C90 174.3(11) . . . . ? C91 C90 N6 C89 126.0(13) . . . . ? N1 C8 O1 Pr2 -147(5) . . . . ? C9 C8 O1 Pr2 33(5) . . . . ? O10 Pr2 O1 C8 60(5) 2_546 . . . ? O6 Pr2 O1 C8 9(5) . . . . ? O28 Pr2 O1 C8 -150(5) . . . . ? O27 Pr2 O1 C8 138(5) . . . . ? O25 Pr2 O1 C8 88(5) . . . . ? O30 Pr2 O1 C8 -168(5) . . . . ? O31 Pr2 O1 C8 -73(5) . . . . ? O33 Pr2 O1 C8 -74(5) . . . . ? C13 C14 O2 C15 -6.8(14) . . . . ? C9 C14 O2 C15 173.4(8) . . . . ? C16 C15 O2 C14 -173.3(9) . . . . ? C15 C16 O3 C17 -150.9(8) . . . . ? C18 C17 O3 C16 -163.5(9) . . . . ? C20 C19 O4 C18 31.6(15) . . . . ? C24 C19 O4 C18 -151.3(9) . . . . ? C17 C18 O4 C19 115.3(11) . . . . ? N2 C25 O5 Pr1 -59(4) . . . . ? C24 C25 O5 Pr1 123(3) . . . . ? O11 Pr1 O5 C25 -161(4) . . . . ? O15 Pr1 O5 C25 131(4) 2_655 . . . ? O22 Pr1 O5 C25 73(4) . . . . ? O24 Pr1 O5 C25 123(4) . . . . ? O19 Pr1 O5 C25 -2(4) . . . . ? O18 Pr1 O5 C25 -84(4) . . . . ? O21 Pr1 O5 C25 9(4) . . . . ? O16 Pr1 O5 C25 -77(4) . . . . ? N3 C40 O6 Pr2 58(15) . . . . ? C41 C40 O6 Pr2 -119(15) . . . . ? O10 Pr2 O6 C40 -150(15) 2_546 . . . ? O1 Pr2 O6 C40 10(15) . . . . ? O28 Pr2 O6 C40 57(15) . . . . ? O27 Pr2 O6 C40 -64(15) . . . . ? O25 Pr2 O6 C40 -72(15) . . . . ? O30 Pr2 O6 C40 -176(100) . . . . ? O31 Pr2 O6 C40 88(15) . . . . ? O33 Pr2 O6 C40 137(15) . . . . ? C45 C46 O7 C47 6.0(15) . . . . ? C41 C46 O7 C47 -175.8(8) . . . . ? C48 C47 O7 C46 173.8(9) . . . . ? C47 C48 O8 C49 -174.8(9) . . . . ? C50 C49 O8 C48 177.3(8) . . . . ? C56 C51 O9 C50 173.7(8) . . . . ? C52 C51 O9 C50 -4.4(14) . . . . ? C49 C50 O9 C51 -173.4(8) . . . . ? N4 C57 O10 Pr2 -87(3) . . . 2_556 ? C56 C57 O10 Pr2 94(3) . . . 2_556 ? N5 C72 O11 Pr1 -77(4) . . . . ? C73 C72 O11 Pr1 106(4) . . . . ? O5 Pr1 O11 C72 -26(4) . . . . ? O15 Pr1 O11 C72 129(4) 2_655 . . . ? O22 Pr1 O11 C72 52(4) . . . . ? O24 Pr1 O11 C72 50(4) . . . . ? O19 Pr1 O11 C72 -65(4) . . . . ? O18 Pr1 O11 C72 -154(4) . . . . ? O21 Pr1 O11 C72 175(4) . . . . ? O16 Pr1 O11 C72 -105(4) . . . . ? C73 C78 O12 C79 174.8(10) . . . . ? C77 C78 O12 C79 -5.2(16) . . . . ? C80 C79 O12 C78 173.1(10) . . . . ? C79 C80 O13 C81 -176.4(10) . . . . ? C82 C81 O13 C80 -175.8(10) . . . . ? C88 C83 O14 C82 6.5(14) . . . . ? C84 C83 O14 C82 -175.4(9) . . . . ? C81 C82 O14 C83 176.0(9) . . . . ? N6 C89 O15 Pr1 84(4) . . . 2_645 ? C84 C89 O15 Pr1 -96(3) . . . 2_645 ? O17 N7 O16 Pr1 177.8(10) . . . . ? O18 N7 O16 Pr1 1.7(9) . . . . ? O5 Pr1 O16 N7 -173.3(6) . . . . ? O11 Pr1 O16 N7 -87.7(6) . . . . ? O15 Pr1 O16 N7 -7.9(7) 2_655 . . . ? O22 Pr1 O16 N7 125.7(7) . . . . ? O24 Pr1 O16 N7 -136.7(7) . . . . ? O19 Pr1 O16 N7 113.6(6) . . . . ? O18 Pr1 O16 N7 -1.0(6) . . . . ? O21 Pr1 O16 N7 67.3(6) . . . . ? O17 N7 O18 Pr1 -177.7(11) . . . . ? O16 N7 O18 Pr1 -1.7(10) . . . . ? O5 Pr1 O18 N7 10.4(8) . . . . ? O11 Pr1 O18 N7 88.0(7) . . . . ? O15 Pr1 O18 N7 175.3(7) 2_655 . . . ? O22 Pr1 O18 N7 -129.1(7) . . . . ? O24 Pr1 O18 N7 135.3(8) . . . . ? O19 Pr1 O18 N7 -59.0(7) . . . . ? O21 Pr1 O18 N7 -105.3(7) . . . . ? O16 Pr1 O18 N7 1.1(6) . . . . ? O20 N8 O19 Pr1 -175.3(11) . . . . ? O21 N8 O19 Pr1 9.9(11) . . . . ? O5 Pr1 O19 N8 161.6(8) . . . . ? O11 Pr1 O19 N8 -157.1(7) . . . . ? O15 Pr1 O19 N8 5.1(8) 2_655 . . . ? O22 Pr1 O19 N8 71.8(7) . . . . ? O24 Pr1 O19 N8 99.6(8) . . . . ? O18 Pr1 O19 N8 -71.9(7) . . . . ? O21 Pr1 O19 N8 -5.9(7) . . . . ? O16 Pr1 O19 N8 -115.4(7) . . . . ? O20 N8 O21 Pr1 175.4(11) . . . . ? O19 N8 O21 Pr1 -9.8(11) . . . . ? O5 Pr1 O21 N8 -7.5(7) . . . . ? O11 Pr1 O21 N8 148.3(7) . . . . ? O15 Pr1 O21 N8 -164.9(7) 2_655 . . . ? O22 Pr1 O21 N8 -79.0(7) . . . . ? O24 Pr1 O21 N8 -95.8(7) . . . . ? O19 Pr1 O21 N8 6.0(7) . . . . ? O18 Pr1 O21 N8 116.0(7) . . . . ? O16 Pr1 O21 N8 69.7(7) . . . . ? O24 N9 O22 Pr1 8(2) . . . . ? O23 N9 O22 Pr1 -178.6(13) . . . . ? O5 Pr1 O22 N9 71.6(10) . . . . ? O11 Pr1 O22 N9 -7.3(11) . . . . ? O15 Pr1 O22 N9 -86.2(10) 2_655 . . . ? O24 Pr1 O22 N9 -4.2(11) . . . . ? O19 Pr1 O22 N9 142.7(10) . . . . ? O18 Pr1 O22 N9 -140.3(9) . . . . ? O21 Pr1 O22 N9 -164.7(10) . . . . ? O16 Pr1 O22 N9 130.7(9) . . . . ? O23 N9 O24 Pr1 179.3(17) . . . . ? O22 N9 O24 Pr1 -8(2) . . . . ? O5 Pr1 O24 N9 -90.2(14) . . . . ? O11 Pr1 O24 N9 -178.0(14) . . . . ? O15 Pr1 O24 N9 93.4(14) 2_655 . . . ? O22 Pr1 O24 N9 4.6(12) . . . . ? O19 Pr1 O24 N9 -31.0(15) . . . . ? O18 Pr1 O24 N9 133.0(11) . . . . ? O21 Pr1 O24 N9 25.5(15) . . . . ? O16 Pr1 O24 N9 -127.2(12) . . . . ? O26 N10 O25 Pr2 175.9(11) . . . . ? O27 N10 O25 Pr2 -4.1(10) . . . . ? O10 Pr2 O25 N10 -102.7(7) 2_546 . . . ? O1 Pr2 O25 N10 90.1(6) . . . . ? O6 Pr2 O25 N10 173.9(7) . . . . ? O28 Pr2 O25 N10 19.6(7) . . . . ? O27 Pr2 O25 N10 2.5(6) . . . . ? O30 Pr2 O25 N10 -32.2(7) . . . . ? O31 Pr2 O25 N10 130.9(6) . . . . ? O33 Pr2 O25 N10 -118.0(8) . . . . ? O26 N10 O27 Pr2 -175.8(11) . . . . ? O25 N10 O27 Pr2 4.2(10) . . . . ? O10 Pr2 O27 N10 67.0(7) 2_546 . . . ? O1 Pr2 O27 N10 -86.7(6) . . . . ? O6 Pr2 O27 N10 -13.0(7) . . . . ? O28 Pr2 O27 N10 -166.7(7) . . . . ? O25 Pr2 O27 N10 -2.5(6) . . . . ? O30 Pr2 O27 N10 140.9(7) . . . . ? O31 Pr2 O27 N10 -143.2(6) . . . . ? O33 Pr2 O27 N10 134.1(7) . . . . ? O29 N11 O28 Pr2 166.9(14) . . . . ? O30 N11 O28 Pr2 -7.0(12) . . . . ? O10 Pr2 O28 N11 8.9(8) 2_546 . . . ? O1 Pr2 O28 N11 -155.5(8) . . . . ? O6 Pr2 O28 N11 156.9(7) . . . . ? O27 Pr2 O28 N11 -70.0(7) . . . . ? O25 Pr2 O28 N11 -83.7(8) . . . . ? O30 Pr2 O28 N11 4.2(7) . . . . ? O31 Pr2 O28 N11 124.4(8) . . . . ? O33 Pr2 O28 N11 75.8(8) . . . . ? O29 N11 O30 Pr2 -167.4(12) . . . . ? O28 N11 O30 Pr2 6.9(12) . . . . ? O10 Pr2 O30 N11 179.8(8) 2_546 . . . ? O1 Pr2 O30 N11 19.9(9) . . . . ? O6 Pr2 O30 N11 -153.2(7) . . . . ? O28 Pr2 O30 N11 -4.2(7) . . . . ? O27 Pr2 O30 N11 81.3(8) . . . . ? O25 Pr2 O30 N11 109.4(8) . . . . ? O31 Pr2 O30 N11 -62.3(8) . . . . ? O33 Pr2 O30 N11 -103.3(8) . . . . ? O32 N12 O31 Pr2 -174.1(12) . . . . ? O33 N12 O31 Pr2 2.5(13) . . . . ? O10 Pr2 O31 N12 22.3(8) 2_546 . . . ? O1 Pr2 O31 N12 179.8(7) . . . . ? O6 Pr2 O31 N12 96.0(7) . . . . ? O28 Pr2 O31 N12 -99.4(7) . . . . ? O27 Pr2 O31 N12 -122.5(7) . . . . ? O25 Pr2 O31 N12 138.5(7) . . . . ? O30 Pr2 O31 N12 -57.9(7) . . . . ? O33 Pr2 O31 N12 -1.5(8) . . . . ? O32 N12 O33 Pr2 174.0(13) . . . . ? O31 N12 O33 Pr2 -2.5(13) . . . . ? O10 Pr2 O33 N12 -157.1(9) 2_546 . . . ? O1 Pr2 O33 N12 3.1(10) . . . . ? O6 Pr2 O33 N12 -76.4(9) . . . . ? O28 Pr2 O33 N12 74.8(9) . . . . ? O27 Pr2 O33 N12 129.4(8) . . . . ? O25 Pr2 O33 N12 -141.6(7) . . . . ? O30 Pr2 O33 N12 123.0(9) . . . . ? O31 Pr2 O33 N12 1.5(8) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.41 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.443 _refine_diff_density_min -0.352 _refine_diff_density_rms 0.066 #===END data_compoud3 _database_code_depnum_ccdc_archive 'CCDC 817222' #TrackingRef '- 1-12.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C96 H96 N12 Nd2 O33' _chemical_formula_weight 2234.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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' O O 0.0106 0.0060 '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' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 19.755(3) _cell_length_b 19.755(3) _cell_length_c 53.209(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 17983(5) _cell_formula_units_Z 6 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5536 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 19.88 _exptl_crystal_description block _exptl_crystal_colour lilac _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.238 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6840 _exptl_absorpt_coefficient_mu 0.930 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.830 _exptl_absorpt_correction_T_max 0.846 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 27977 _diffrn_reflns_av_R_equivalents 0.0425 _diffrn_reflns_av_sigmaI/netI 0.0342 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -59 _diffrn_reflns_limit_l_max 58 _diffrn_reflns_theta_min 1.15 _diffrn_reflns_theta_max 23.57 _reflns_number_total 5953 _reflns_number_gt 4277 _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 ; Restraints to thermal parameters were applied on the disordered phenyl groups. The distance restrains were applied to C12, C13, C18. 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. Diffuse electron densities resulting from residual disorder solvent moleculeswere removed from the data set using the SQUEEZE routine of PLATON andrefined further using the data generated. ; # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.333 0.667 0.167 1451 328 ' ' 2 0.000 0.000 0.236 9 0 ' ' 3 0.000 0.000 0.500 1444 328 ' ' 4 -0.333 0.333 0.833 1451 328 ' ' 5 0.000 0.000 0.764 9 0 ' ' 6 0.333 0.667 0.431 9 0 ' ' 7 0.333 0.667 0.902 10 0 ' ' 8 0.667 0.333 0.098 10 0 ' ' 9 0.667 0.333 0.569 9 0 ' ' _platon_squeeze_details ; ; _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^)+(0.0929P)^2^+1.0000P] 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 5953 _refine_ls_number_parameters 394 _refine_ls_number_restraints 291 _refine_ls_R_factor_all 0.0642 _refine_ls_R_factor_gt 0.0473 _refine_ls_wR_factor_ref 0.1507 _refine_ls_wR_factor_gt 0.1411 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.107 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2466(2) 0.42501(18) 0.36253(7) 0.0626(13) Uani 1 1 d G . . C2 C 0.30929(19) 0.43492(19) 0.34797(7) 0.0762(15) Uani 1 1 d G . . H2 H 0.3472 0.4847 0.3429 0.091 Uiso 1 1 calc R . . C3 C 0.3153(2) 0.3704(3) 0.34094(7) 0.0923(18) Uani 1 1 d G . . H3 H 0.3573 0.3770 0.3312 0.111 Uiso 1 1 calc R . . C4 C 0.2586(3) 0.2959(2) 0.34849(8) 0.0917(19) Uani 1 1 d G . . H4 H 0.2627 0.2527 0.3438 0.110 Uiso 1 1 calc R . . C5 C 0.1959(2) 0.28598(16) 0.36305(8) 0.0932(19) Uani 1 1 d G . . H5 H 0.1580 0.2362 0.3681 0.112 Uiso 1 1 calc R . . C6 C 0.1899(2) 0.3505(2) 0.37007(7) 0.0766(16) Uani 1 1 d G . . C7 C 0.0728(4) 0.2740(4) 0.39490(16) 0.119(3) Uani 1 1 d . . . H7A H 0.0971 0.2619 0.4087 0.143 Uiso 1 1 calc R . . H7B H 0.0523 0.2309 0.3831 0.143 Uiso 1 1 calc R . . C8 C 0.0092(5) 0.2848(5) 0.40442(17) 0.153(4) Uani 1 1 d . . . H8A H -0.0223 0.2838 0.3903 0.183 Uiso 1 1 calc R . . H8B H -0.0239 0.2408 0.4152 0.183 Uiso 1 1 calc R . . C9 C 0.0561(5) 0.3554(4) 0.44274(16) 0.112(2) Uani 1 1 d . . . H9A H 0.1050 0.3549 0.4433 0.134 Uiso 1 1 calc R . . H9B H 0.0169 0.3103 0.4519 0.134 Uiso 1 1 calc R . . C10 C 0.0662(4) 0.4283(4) 0.45400(12) 0.0951(19) Uani 1 1 d . . . H10A H 0.0882 0.4353 0.4707 0.114 Uiso 1 1 calc R . . H10B H 0.1014 0.4729 0.4438 0.114 Uiso 1 1 calc R . . C11 C 0.2473(3) 0.4985(3) 0.36962(10) 0.0667(14) Uani 1 1 d . . . C12 C 0.1969(4) 0.5611(4) 0.39803(13) 0.108(2) Uani 1 1 d D . . H12A H 0.2337 0.6078 0.3890 0.130 Uiso 1 1 calc R . . H12B H 0.2117 0.5689 0.4156 0.130 Uiso 1 1 calc R . . C13 C 0.1174(3) 0.5505(4) 0.39543(11) 0.110(2) Uani 1 1 d GDU . . C14 C 0.0612(4) 0.4936(3) 0.37989(10) 0.143(3) Uani 1 1 d GDU . . H14 H 0.0727 0.4603 0.3709 0.172 Uiso 1 1 calc R . . C15 C -0.0123(4) 0.4864(4) 0.37784(12) 0.172(3) Uani 1 1 d GU . . H15 H -0.0499 0.4483 0.3674 0.206 Uiso 1 1 calc R . . C16 C -0.0295(3) 0.5362(4) 0.39132(14) 0.159(3) Uani 1 1 d GU . . H16 H -0.0787 0.5314 0.3899 0.190 Uiso 1 1 calc R . . C17 C 0.0267(4) 0.5931(4) 0.40686(12) 0.146(3) Uani 1 1 d GU . . H17 H 0.0152 0.6264 0.4159 0.175 Uiso 1 1 calc R . . C18 C 0.1001(4) 0.6002(3) 0.40892(10) 0.135(3) Uani 1 1 d GDU . . H18 H 0.1377 0.6383 0.4193 0.162 Uiso 1 1 calc R . . C19 C -0.0895(3) 0.4754(3) 0.46388(9) 0.0682(14) Uani 1 1 d . . . C20 C -0.0965(3) 0.5375(4) 0.47279(11) 0.0775(15) Uani 1 1 d . . . H20 H -0.1458 0.5324 0.4737 0.093 Uiso 1 1 calc R . . C21 C -0.0330(4) 0.6062(4) 0.48030(12) 0.0884(18) Uani 1 1 d . . . H21 H -0.0394 0.6475 0.4856 0.106 Uiso 1 1 calc R . . C22 C 0.0386(4) 0.6141(4) 0.48002(12) 0.0898(18) Uani 1 1 d . . . H22 H 0.0815 0.6606 0.4854 0.108 Uiso 1 1 calc R . . C23 C 0.0487(3) 0.5530(4) 0.47175(11) 0.0817(17) Uani 1 1 d . . . H23 H 0.0983 0.5585 0.4716 0.098 Uiso 1 1 calc R . . C24 C -0.0150(3) 0.4840(4) 0.46375(9) 0.0705(15) Uani 1 1 d . . . C25 C -0.1614(3) 0.4032(4) 0.45587(11) 0.0766(16) Uani 1 1 d . . . C26 C -0.2201(5) 0.2794(5) 0.43172(17) 0.153(3) Uani 1 1 d U . . H26A H -0.2182 0.2375 0.4406 0.184 Uiso 1 1 calc R . . H26B H -0.2694 0.2765 0.4357 0.184 Uiso 1 1 calc R . . C27 C -0.2164(3) 0.2685(4) 0.40478(9) 0.106(2) Uani 1 1 d GU . . C28 C -0.2250(3) 0.3211(3) 0.38967(15) 0.175(3) Uani 1 1 d GU . . H28 H -0.2334 0.3591 0.3970 0.210 Uiso 1 1 calc R . . C29 C -0.2211(4) 0.3170(4) 0.36367(14) 0.190(4) Uani 1 1 d GU . . H29 H -0.2268 0.3522 0.3536 0.228 Uiso 1 1 calc R . . C30 C -0.2086(4) 0.2602(5) 0.35279(9) 0.179(4) Uani 1 1 d GU . . H30 H -0.2060 0.2574 0.3354 0.215 Uiso 1 1 calc R . . C31 C -0.2000(4) 0.2075(4) 0.36790(14) 0.161(3) Uani 1 1 d GU . . H31 H -0.1917 0.1696 0.3606 0.193 Uiso 1 1 calc R . . C32 C -0.2039(3) 0.2117(4) 0.39389(13) 0.165(3) Uani 1 1 d GU . . H32 H -0.1982 0.1765 0.4040 0.198 Uiso 1 1 calc R . . N1 N 0.4132(3) 0.8133(3) 0.30203(11) 0.0854(15) Uani 1 1 d . . . N2 N -0.4770(3) 0.2648(4) 0.52214(14) 0.0987(17) Uani 1 1 d . . . N3 N 0.2024(3) 0.4945(3) 0.38853(10) 0.0939(16) Uani 1 1 d . . . H3A H 0.1746 0.4500 0.3957 0.113 Uiso 1 1 calc R . . N4 N -0.1544(3) 0.3561(3) 0.44047(11) 0.122(2) Uani 1 1 d . . . H4A H -0.1084 0.3701 0.4349 0.146 Uiso 1 1 calc R . . Nd2 Nd -0.3333 0.3333 0.491749(10) 0.0646(2) Uani 1 3 d S . . Nd1 Nd 0.3333 0.6667 0.330600(8) 0.05493(19) Uani 1 3 d S . . O1 O 0.3737(2) 0.8068(2) 0.32073(9) 0.0807(11) Uani 1 1 d . . . O2 O 0.4230(2) 0.7558(3) 0.29647(8) 0.0907(12) Uani 1 1 d . . . O3 O 0.4457(3) 0.8738(3) 0.28967(13) 0.146(2) Uani 1 1 d . . . O4 O -0.4209(3) 0.3324(3) 0.52690(9) 0.1031(14) Uani 1 1 d . . . O5 O -0.4738(2) 0.2352(3) 0.50187(10) 0.0953(12) Uani 1 1 d . . . O6 O -0.5307(3) 0.2315(3) 0.53672(13) 0.143(2) Uani 1 1 d . . . O7 O 0.2909(2) 0.5593(2) 0.35874(7) 0.0690(9) Uani 1 1 d . . . O8 O -0.2274(2) 0.3899(2) 0.46299(7) 0.0821(11) Uani 1 1 d . . . O9 O 0.1280(3) 0.3428(2) 0.38301(9) 0.1131(16) Uani 1 1 d . . . O10 O 0.0324(3) 0.3527(3) 0.41775(11) 0.1282(18) Uani 1 1 d . . . O11 O -0.0097(2) 0.4221(2) 0.45517(8) 0.0898(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 0.064(3) 0.059(3) 0.057(3) -0.003(2) -0.005(2) 0.025(3) C2 0.087(4) 0.062(4) 0.081(4) -0.002(3) -0.011(3) 0.038(3) C3 0.104(5) 0.105(5) 0.082(4) -0.014(4) -0.002(4) 0.064(5) C4 0.117(6) 0.076(4) 0.093(5) -0.015(3) -0.012(4) 0.056(4) C5 0.110(5) 0.071(4) 0.084(4) -0.004(3) -0.003(4) 0.034(4) C6 0.098(5) 0.060(4) 0.066(4) -0.010(3) -0.004(3) 0.035(3) C7 0.121(6) 0.061(4) 0.137(6) -0.012(4) 0.042(5) 0.017(4) C8 0.145(8) 0.100(6) 0.146(8) -0.030(5) 0.059(6) 0.011(5) C9 0.106(6) 0.115(6) 0.119(7) 0.019(5) 0.017(5) 0.059(5) C10 0.106(5) 0.128(6) 0.071(4) 0.000(4) 0.016(3) 0.073(5) C11 0.062(3) 0.058(3) 0.069(4) -0.001(3) -0.008(3) 0.021(3) C12 0.139(6) 0.079(4) 0.101(5) 0.006(4) 0.048(4) 0.050(5) C13 0.144(5) 0.112(5) 0.096(4) 0.034(3) 0.051(4) 0.082(4) C14 0.136(5) 0.167(6) 0.128(5) 0.027(5) 0.022(4) 0.077(5) C15 0.173(6) 0.187(6) 0.149(6) 0.028(5) 0.008(5) 0.085(5) C16 0.164(6) 0.172(6) 0.147(6) 0.043(5) 0.015(5) 0.089(5) C17 0.160(6) 0.166(6) 0.135(5) 0.037(4) 0.039(5) 0.098(5) C18 0.159(5) 0.149(5) 0.118(5) 0.044(4) 0.044(4) 0.093(4) C19 0.064(4) 0.081(4) 0.054(3) -0.001(3) 0.009(2) 0.032(3) C20 0.068(4) 0.092(4) 0.077(4) 0.001(3) 0.008(3) 0.043(4) C21 0.094(5) 0.083(5) 0.092(5) -0.004(3) 0.006(4) 0.047(4) C22 0.074(4) 0.093(5) 0.084(4) -0.006(3) 0.003(3) 0.028(4) C23 0.056(4) 0.108(5) 0.070(4) 0.007(3) 0.003(3) 0.032(4) C24 0.068(4) 0.087(4) 0.054(3) 0.000(3) 0.004(3) 0.037(3) C25 0.068(4) 0.084(4) 0.067(4) -0.005(3) -0.001(3) 0.031(3) C26 0.132(5) 0.147(5) 0.128(5) -0.033(4) 0.012(4) 0.030(4) C27 0.091(4) 0.118(4) 0.111(4) -0.036(4) 0.001(3) 0.054(3) C28 0.167(6) 0.170(6) 0.160(6) -0.023(5) -0.020(5) 0.063(5) C29 0.177(6) 0.190(6) 0.173(6) -0.011(5) -0.005(5) 0.069(5) C30 0.172(6) 0.192(6) 0.153(6) -0.036(5) 0.009(5) 0.075(5) C31 0.150(5) 0.175(6) 0.156(6) -0.048(5) -0.007(5) 0.080(4) C32 0.153(5) 0.178(6) 0.162(6) -0.020(5) -0.018(5) 0.081(4) N1 0.071(3) 0.078(4) 0.103(4) 0.033(3) 0.003(3) 0.034(3) N2 0.076(4) 0.078(4) 0.136(5) 0.004(4) 0.034(4) 0.034(3) N3 0.111(4) 0.057(3) 0.096(4) 0.012(2) 0.043(3) 0.029(3) N4 0.073(4) 0.124(5) 0.119(5) -0.059(4) 0.012(3) 0.012(3) Nd2 0.0566(2) 0.0566(2) 0.0806(4) 0.000 0.000 0.02832(12) Nd1 0.0502(2) 0.0502(2) 0.0644(3) 0.000 0.000 0.02510(11) O1 0.076(3) 0.071(3) 0.100(3) 0.012(2) 0.008(2) 0.039(2) O2 0.084(3) 0.086(3) 0.108(3) 0.024(2) 0.030(2) 0.047(3) O3 0.136(5) 0.120(4) 0.192(6) 0.085(4) 0.054(4) 0.071(4) O4 0.092(3) 0.093(3) 0.119(4) -0.008(3) 0.026(3) 0.041(3) O5 0.075(3) 0.088(3) 0.110(4) 0.004(3) 0.011(2) 0.031(2) O6 0.109(4) 0.102(4) 0.201(6) 0.021(4) 0.077(4) 0.041(3) O7 0.068(2) 0.057(2) 0.081(2) 0.0155(18) 0.0133(18) 0.030(2) O8 0.062(2) 0.091(3) 0.091(3) 0.008(2) 0.010(2) 0.036(2) O9 0.111(4) 0.062(3) 0.133(4) 0.003(2) 0.052(3) 0.018(3) O10 0.147(4) 0.094(4) 0.100(4) -0.025(3) 0.020(3) 0.027(3) O11 0.074(3) 0.103(3) 0.094(3) -0.016(2) 0.012(2) 0.045(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 1.3900 . ? C1 C6 1.3900 . ? C1 C11 1.492(6) . ? C2 C3 1.3900 . ? C2 H2 0.9300 . ? C3 C4 1.3900 . ? C3 H3 0.9300 . ? C4 C5 1.3900 . ? C4 H4 0.9300 . ? C5 C6 1.3900 . ? C5 H5 0.9300 . ? C6 O9 1.343(5) . ? C7 O9 1.399(7) . ? C7 C8 1.465(10) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 O10 1.379(8) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 O10 1.402(9) . ? C9 C10 1.479(9) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 O11 1.444(7) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 O7 1.220(6) . ? C11 N3 1.317(7) . ? C12 N3 1.463(7) . ? C12 C13 1.484(7) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.3900 . ? C13 C18 1.3900 . ? C14 C15 1.3900 . ? C14 H14 0.9300 . ? C15 C16 1.3900 . ? C15 H15 0.9300 . ? C16 C17 1.3900 . ? C16 H16 0.9300 . ? C17 C18 1.3900 . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C20 1.385(7) . ? C19 C24 1.395(7) . ? C19 C25 1.485(8) . ? C20 C21 1.368(8) . ? C20 H20 0.9300 . ? C21 C22 1.343(8) . ? C21 H21 0.9300 . ? C22 C23 1.390(8) . ? C22 H22 0.9300 . ? C23 C24 1.381(8) . ? C23 H23 0.9300 . ? C24 O11 1.359(6) . ? C25 O8 1.252(6) . ? C25 N4 1.299(7) . ? C26 C27 1.457(9) . ? C26 N4 1.493(9) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.3900 . ? C27 C32 1.3900 . ? C28 C29 1.3900 . ? C28 H28 0.9300 . ? C29 C30 1.3900 . ? C29 H29 0.9300 . ? C30 C31 1.3900 . ? C30 H30 0.9300 . ? C31 C32 1.3900 . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? N1 O3 1.227(6) . ? N1 O1 1.232(6) . ? N1 O2 1.277(6) . ? N2 O6 1.210(7) . ? N2 O5 1.244(7) . ? N2 O4 1.263(6) . ? N3 H3A 0.8600 . ? N4 H4A 0.8600 . ? Nd2 O8 2.373(4) . ? Nd2 O8 2.373(4) 3_455 ? Nd2 O8 2.373(4) 2_565 ? Nd2 O5 2.524(4) 2_565 ? Nd2 O5 2.524(4) . ? Nd2 O5 2.524(4) 3_455 ? Nd2 O4 2.541(4) 2_565 ? Nd2 O4 2.541(4) 3_455 ? Nd2 O4 2.541(4) . ? Nd2 N2 2.942(6) 2_565 ? Nd2 N2 2.942(6) 3_455 ? Nd1 O7 2.380(3) 3_565 ? Nd1 O7 2.380(3) 2_665 ? Nd1 O7 2.380(3) . ? Nd1 O1 2.523(4) . ? Nd1 O1 2.523(4) 2_665 ? Nd1 O1 2.523(4) 3_565 ? Nd1 O2 2.533(4) 2_665 ? Nd1 O2 2.533(4) . ? Nd1 O2 2.533(4) 3_565 ? Nd1 N1 2.936(5) 2_665 ? Nd1 N1 2.936(5) 3_565 ? 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 120.0 . . ? C2 C1 C11 115.4(3) . . ? C6 C1 C11 124.5(3) . . ? C1 C2 C3 120.0 . . ? C1 C2 H2 120.0 . . ? C3 C2 H2 120.0 . . ? C4 C3 C2 120.0 . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C5 C4 C3 120.0 . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C6 C5 C4 120.0 . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? O9 C6 C5 121.6(3) . . ? O9 C6 C1 118.3(3) . . ? C5 C6 C1 120.0 . . ? O9 C7 C8 109.0(6) . . ? O9 C7 H7A 109.9 . . ? C8 C7 H7A 109.9 . . ? O9 C7 H7B 109.9 . . ? C8 C7 H7B 109.9 . . ? H7A C7 H7B 108.3 . . ? O10 C8 C7 115.3(7) . . ? O10 C8 H8A 108.5 . . ? C7 C8 H8A 108.5 . . ? O10 C8 H8B 108.5 . . ? C7 C8 H8B 108.5 . . ? H8A C8 H8B 107.5 . . ? O10 C9 C10 107.5(6) . . ? O10 C9 H9A 110.2 . . ? C10 C9 H9A 110.2 . . ? O10 C9 H9B 110.2 . . ? C10 C9 H9B 110.2 . . ? H9A C9 H9B 108.5 . . ? O11 C10 C9 107.8(6) . . ? O11 C10 H10A 110.1 . . ? C9 C10 H10A 110.1 . . ? O11 C10 H10B 110.1 . . ? C9 C10 H10B 110.1 . . ? H10A C10 H10B 108.5 . . ? O7 C11 N3 123.0(5) . . ? O7 C11 C1 119.8(5) . . ? N3 C11 C1 117.2(5) . . ? N3 C12 C13 113.0(6) . . ? N3 C12 H12A 109.0 . . ? C13 C12 H12A 109.0 . . ? N3 C12 H12B 109.0 . . ? C13 C12 H12B 109.0 . . ? H12A C12 H12B 107.8 . . ? C14 C13 C18 120.0 . . ? C14 C13 C12 122.1(5) . . ? C18 C13 C12 117.9(5) . . ? C15 C14 C13 120.0 . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C14 C15 C16 120.0 . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C17 C16 C15 120.0 . . ? C17 C16 H16 120.0 . . ? C15 C16 H16 120.0 . . ? C16 C17 C18 120.0 . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C17 C18 C13 120.0 . . ? C17 C18 H18 120.0 . . ? C13 C18 H18 120.0 . . ? C20 C19 C24 117.4(5) . . ? C20 C19 C25 118.6(5) . . ? C24 C19 C25 124.0(5) . . ? C21 C20 C19 122.1(6) . . ? C21 C20 H20 119.0 . . ? C19 C20 H20 119.0 . . ? C22 C21 C20 120.1(6) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C21 C22 C23 120.2(6) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? C24 C23 C22 119.9(6) . . ? C24 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? O11 C24 C23 123.3(6) . . ? O11 C24 C19 116.4(5) . . ? C23 C24 C19 120.3(6) . . ? O8 C25 N4 120.9(6) . . ? O8 C25 C19 120.7(5) . . ? N4 C25 C19 118.4(5) . . ? C27 C26 N4 112.0(7) . . ? C27 C26 H26A 109.2 . . ? N4 C26 H26A 109.2 . . ? C27 C26 H26B 109.2 . . ? N4 C26 H26B 109.2 . . ? H26A C26 H26B 107.9 . . ? C28 C27 C32 120.0 . . ? C28 C27 C26 115.2(7) . . ? C32 C27 C26 124.8(7) . . ? C27 C28 C29 120.0 . . ? C27 C28 H28 120.0 . . ? C29 C28 H28 120.0 . . ? C30 C29 C28 120.0 . . ? C30 C29 H29 120.0 . . ? C28 C29 H29 120.0 . . ? C31 C30 C29 120.0 . . ? C31 C30 H30 120.0 . . ? C29 C30 H30 120.0 . . ? C30 C31 C32 120.0 . . ? C30 C31 H31 120.0 . . ? C32 C31 H31 120.0 . . ? C31 C32 C27 120.0 . . ? C31 C32 H32 120.0 . . ? C27 C32 H32 120.0 . . ? O3 N1 O1 122.0(6) . . ? O3 N1 O2 120.3(6) . . ? O1 N1 O2 117.7(5) . . ? O6 N2 O5 122.5(6) . . ? O6 N2 O4 120.9(7) . . ? O5 N2 O4 116.6(5) . . ? C11 N3 C12 124.1(5) . . ? C11 N3 H3A 117.9 . . ? C12 N3 H3A 117.9 . . ? C25 N4 C26 125.0(6) . . ? C25 N4 H4A 117.5 . . ? C26 N4 H4A 117.5 . . ? O8 Nd2 O8 82.90(14) . 3_455 ? O8 Nd2 O8 82.90(14) . 2_565 ? O8 Nd2 O8 82.90(14) 3_455 2_565 ? O8 Nd2 O5 69.57(15) . 2_565 ? O8 Nd2 O5 83.71(15) 3_455 2_565 ? O8 Nd2 O5 150.62(16) 2_565 2_565 ? O8 Nd2 O5 150.62(16) . . ? O8 Nd2 O5 69.57(15) 3_455 . ? O8 Nd2 O5 83.71(15) 2_565 . ? O5 Nd2 O5 115.58(8) 2_565 . ? O8 Nd2 O5 83.71(15) . 3_455 ? O8 Nd2 O5 150.62(16) 3_455 3_455 ? O8 Nd2 O5 69.57(15) 2_565 3_455 ? O5 Nd2 O5 115.58(8) 2_565 3_455 ? O5 Nd2 O5 115.58(8) . 3_455 ? O8 Nd2 O4 119.35(15) . 2_565 ? O8 Nd2 O4 91.08(16) 3_455 2_565 ? O8 Nd2 O4 156.16(16) 2_565 2_565 ? O5 Nd2 O4 49.80(16) 2_565 2_565 ? O5 Nd2 O4 72.60(16) . 2_565 ? O5 Nd2 O4 118.26(17) 3_455 2_565 ? O8 Nd2 O4 91.08(16) . 3_455 ? O8 Nd2 O4 156.16(16) 3_455 3_455 ? O8 Nd2 O4 119.35(15) 2_565 3_455 ? O5 Nd2 O4 72.60(16) 2_565 3_455 ? O5 Nd2 O4 118.26(17) . 3_455 ? O5 Nd2 O4 49.80(16) 3_455 3_455 ? O4 Nd2 O4 71.79(18) 2_565 3_455 ? O8 Nd2 O4 156.16(16) . . ? O8 Nd2 O4 119.35(15) 3_455 . ? O8 Nd2 O4 91.08(16) 2_565 . ? O5 Nd2 O4 118.26(17) 2_565 . ? O5 Nd2 O4 49.80(16) . . ? O5 Nd2 O4 72.60(15) 3_455 . ? O4 Nd2 O4 71.79(18) 2_565 . ? O4 Nd2 O4 71.79(18) 3_455 . ? O8 Nd2 N2 94.13(17) . 2_565 ? O8 Nd2 N2 89.96(16) 3_455 2_565 ? O8 Nd2 N2 172.55(16) 2_565 2_565 ? O5 Nd2 N2 24.81(15) 2_565 2_565 ? O5 Nd2 N2 95.83(16) . 2_565 ? O5 Nd2 N2 117.02(18) 3_455 2_565 ? O4 Nd2 N2 25.30(14) 2_565 2_565 ? O4 Nd2 N2 67.40(17) 3_455 2_565 ? O4 Nd2 N2 94.30(18) . 2_565 ? O8 Nd2 N2 89.96(16) . 3_455 ? O8 Nd2 N2 172.55(17) 3_455 3_455 ? O8 Nd2 N2 94.14(17) 2_565 3_455 ? O5 Nd2 N2 95.83(16) 2_565 3_455 ? O5 Nd2 N2 117.02(18) . 3_455 ? O5 Nd2 N2 24.81(15) 3_455 3_455 ? O4 Nd2 N2 94.30(18) 2_565 3_455 ? O4 Nd2 N2 25.30(14) 3_455 3_455 ? O4 Nd2 N2 67.40(17) . 3_455 ? N2 Nd2 N2 92.7(2) 2_565 3_455 ? O7 Nd1 O7 84.62(13) 3_565 2_665 ? O7 Nd1 O7 84.62(13) 3_565 . ? O7 Nd1 O7 84.62(13) 2_665 . ? O7 Nd1 O1 71.02(13) 3_565 . ? O7 Nd1 O1 80.36(12) 2_665 . ? O7 Nd1 O1 152.35(14) . . ? O7 Nd1 O1 80.36(13) 3_565 2_665 ? O7 Nd1 O1 152.35(14) 2_665 2_665 ? O7 Nd1 O1 71.02(13) . 2_665 ? O1 Nd1 O1 115.78(7) . 2_665 ? O7 Nd1 O1 152.35(14) 3_565 3_565 ? O7 Nd1 O1 71.02(13) 2_665 3_565 ? O7 Nd1 O1 80.36(12) . 3_565 ? O1 Nd1 O1 115.78(7) . 3_565 ? O1 Nd1 O1 115.78(7) 2_665 3_565 ? O7 Nd1 O2 87.22(14) 3_565 2_665 ? O7 Nd1 O2 151.99(14) 2_665 2_665 ? O7 Nd1 O2 121.24(14) . 2_665 ? O1 Nd1 O2 71.66(14) . 2_665 ? O1 Nd1 O2 50.25(14) 2_665 2_665 ? O1 Nd1 O2 120.43(15) 3_565 2_665 ? O7 Nd1 O2 121.24(14) 3_565 . ? O7 Nd1 O2 87.22(14) 2_665 . ? O7 Nd1 O2 151.99(14) . . ? O1 Nd1 O2 50.25(14) . . ? O1 Nd1 O2 120.43(15) 2_665 . ? O1 Nd1 O2 71.66(14) 3_565 . ? O2 Nd1 O2 74.29(17) 2_665 . ? O7 Nd1 O2 151.99(14) 3_565 3_565 ? O7 Nd1 O2 121.24(14) 2_665 3_565 ? O7 Nd1 O2 87.22(14) . 3_565 ? O1 Nd1 O2 120.43(15) . 3_565 ? O1 Nd1 O2 71.66(14) 2_665 3_565 ? O1 Nd1 O2 50.25(14) 3_565 3_565 ? O2 Nd1 O2 74.29(17) 2_665 3_565 ? O2 Nd1 O2 74.29(17) . 3_565 ? O7 Nd1 N1 84.24(13) 3_565 2_665 ? O7 Nd1 N1 168.79(13) 2_665 2_665 ? O7 Nd1 N1 95.56(16) . 2_665 ? O1 Nd1 N1 94.82(15) . 2_665 ? O1 Nd1 N1 24.62(14) 2_665 2_665 ? O1 Nd1 N1 120.10(14) 3_565 2_665 ? O2 Nd1 N1 25.68(13) 2_665 2_665 ? O2 Nd1 N1 97.51(16) . 2_665 ? O2 Nd1 N1 69.93(14) 3_565 2_665 ? O7 Nd1 N1 168.79(13) 3_565 3_565 ? O7 Nd1 N1 95.56(16) 2_665 3_565 ? O7 Nd1 N1 84.24(13) . 3_565 ? O1 Nd1 N1 120.10(14) . 3_565 ? O1 Nd1 N1 94.82(15) 2_665 3_565 ? O1 Nd1 N1 24.62(14) 3_565 3_565 ? O2 Nd1 N1 97.51(16) 2_665 3_565 ? O2 Nd1 N1 69.93(14) . 3_565 ? O2 Nd1 N1 25.68(13) 3_565 3_565 ? N1 Nd1 N1 95.61(16) 2_665 3_565 ? N1 O1 Nd1 96.8(3) . . ? N1 O2 Nd1 95.1(3) . . ? N2 O4 Nd2 95.4(4) . . ? N2 O5 Nd2 96.8(4) . . ? C11 O7 Nd1 159.7(3) . . ? C25 O8 Nd2 150.9(4) . . ? C6 O9 C7 124.5(5) . . ? C8 O10 C9 117.8(7) . . ? C24 O11 C10 118.9(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 0.0 . . . . ? C11 C1 C2 C3 178.2(3) . . . . ? C1 C2 C3 C4 0.0 . . . . ? C2 C3 C4 C5 0.0 . . . . ? C3 C4 C5 C6 0.0 . . . . ? C4 C5 C6 O9 176.4(4) . . . . ? C4 C5 C6 C1 0.0 . . . . ? C2 C1 C6 O9 -176.6(4) . . . . ? C11 C1 C6 O9 5.4(5) . . . . ? C2 C1 C6 C5 0.0 . . . . ? C11 C1 C6 C5 -178.0(4) . . . . ? O9 C7 C8 O10 -48.2(11) . . . . ? O10 C9 C10 O11 66.1(7) . . . . ? C2 C1 C11 O7 14.7(6) . . . . ? C6 C1 C11 O7 -167.2(4) . . . . ? C2 C1 C11 N3 -162.0(4) . . . . ? C6 C1 C11 N3 16.1(6) . . . . ? N3 C12 C13 C14 -15.6(7) . . . . ? N3 C12 C13 C18 165.1(4) . . . . ? C18 C13 C14 C15 0.0 . . . . ? C12 C13 C14 C15 -179.3(5) . . . . ? C13 C14 C15 C16 0.0 . . . . ? C14 C15 C16 C17 0.0 . . . . ? C15 C16 C17 C18 0.0 . . . . ? C16 C17 C18 C13 0.0 . . . . ? C14 C13 C18 C17 0.0 . . . . ? C12 C13 C18 C17 179.3(5) . . . . ? C24 C19 C20 C21 2.6(8) . . . . ? C25 C19 C20 C21 -179.4(5) . . . . ? C19 C20 C21 C22 -2.4(9) . . . . ? C20 C21 C22 C23 1.0(9) . . . . ? C21 C22 C23 C24 0.1(9) . . . . ? C22 C23 C24 O11 179.3(5) . . . . ? C22 C23 C24 C19 0.1(8) . . . . ? C20 C19 C24 O11 179.3(5) . . . . ? C25 C19 C24 O11 1.4(8) . . . . ? C20 C19 C24 C23 -1.4(8) . . . . ? C25 C19 C24 C23 -179.4(5) . . . . ? C20 C19 C25 O8 -18.9(8) . . . . ? C24 C19 C25 O8 159.0(5) . . . . ? C20 C19 C25 N4 158.2(6) . . . . ? C24 C19 C25 N4 -23.9(9) . . . . ? N4 C26 C27 C28 -63.9(8) . . . . ? N4 C26 C27 C32 114.8(7) . . . . ? C32 C27 C28 C29 0.0 . . . . ? C26 C27 C28 C29 178.8(6) . . . . ? C27 C28 C29 C30 0.0 . . . . ? C28 C29 C30 C31 0.0 . . . . ? C29 C30 C31 C32 0.0 . . . . ? C30 C31 C32 C27 0.0 . . . . ? C28 C27 C32 C31 0.0 . . . . ? C26 C27 C32 C31 -178.7(6) . . . . ? O7 C11 N3 C12 2.7(10) . . . . ? C1 C11 N3 C12 179.3(5) . . . . ? C13 C12 N3 C11 117.5(7) . . . . ? O8 C25 N4 C26 -6.3(12) . . . . ? C19 C25 N4 C26 176.6(7) . . . . ? C27 C26 N4 C25 135.6(8) . . . . ? O3 N1 O1 Nd1 178.6(5) . . . . ? O2 N1 O1 Nd1 -4.9(5) . . . . ? O7 Nd1 O1 N1 -175.1(3) 3_565 . . . ? O7 Nd1 O1 N1 97.3(3) 2_665 . . . ? O7 Nd1 O1 N1 155.3(3) . . . . ? O1 Nd1 O1 N1 -106.4(3) 2_665 . . . ? O1 Nd1 O1 N1 33.9(4) 3_565 . . . ? O2 Nd1 O1 N1 -81.7(3) 2_665 . . . ? O2 Nd1 O1 N1 2.8(3) . . . . ? O2 Nd1 O1 N1 -23.4(4) 3_565 . . . ? N1 Nd1 O1 N1 -92.9(4) 2_665 . . . ? N1 Nd1 O1 N1 6.4(4) 3_565 . . . ? O3 N1 O2 Nd1 -178.6(5) . . . . ? O1 N1 O2 Nd1 4.8(5) . . . . ? O7 Nd1 O2 N1 -0.5(4) 3_565 . . . ? O7 Nd1 O2 N1 -82.5(3) 2_665 . . . ? O7 Nd1 O2 N1 -155.6(3) . . . . ? O1 Nd1 O2 N1 -2.7(3) . . . . ? O1 Nd1 O2 N1 96.9(3) 2_665 . . . ? O1 Nd1 O2 N1 -153.4(4) 3_565 . . . ? O2 Nd1 O2 N1 76.3(4) 2_665 . . . ? O2 Nd1 O2 N1 154.0(3) 3_565 . . . ? N1 Nd1 O2 N1 87.3(3) 2_665 . . . ? N1 Nd1 O2 N1 -179.4(4) 3_565 . . . ? O6 N2 O4 Nd2 168.4(6) . . . . ? O5 N2 O4 Nd2 -11.9(6) . . . . ? O8 Nd2 O4 N2 162.4(4) . . . . ? O8 Nd2 O4 N2 5.2(4) 3_455 . . . ? O8 Nd2 O4 N2 87.6(4) 2_565 . . . ? O5 Nd2 O4 N2 -94.0(4) 2_565 . . . ? O5 Nd2 O4 N2 6.8(4) . . . . ? O5 Nd2 O4 N2 155.8(4) 3_455 . . . ? O4 Nd2 O4 N2 -75.5(5) 2_565 . . . ? O4 Nd2 O4 N2 -151.7(4) 3_455 . . . ? N2 Nd2 O4 N2 -87.2(3) 2_565 . . . ? N2 Nd2 O4 N2 -178.3(5) 3_455 . . . ? O6 N2 O5 Nd2 -168.3(6) . . . . ? O4 N2 O5 Nd2 12.0(6) . . . . ? O8 Nd2 O5 N2 -167.0(3) . . . . ? O8 Nd2 O5 N2 171.5(4) 3_455 . . . ? O8 Nd2 O5 N2 -103.7(4) 2_565 . . . ? O5 Nd2 O5 N2 99.5(4) 2_565 . . . ? O5 Nd2 O5 N2 -40.0(5) 3_455 . . . ? O4 Nd2 O5 N2 73.6(4) 2_565 . . . ? O4 Nd2 O5 N2 16.3(4) 3_455 . . . ? O4 Nd2 O5 N2 -6.9(4) . . . . ? N2 Nd2 O5 N2 83.8(5) 2_565 . . . ? N2 Nd2 O5 N2 -12.3(4) 3_455 . . . ? N3 C11 O7 Nd1 -80.2(12) . . . . ? C1 C11 O7 Nd1 103.2(10) . . . . ? O7 Nd1 O7 C11 72.7(11) 3_565 . . . ? O7 Nd1 O7 C11 157.8(10) 2_665 . . . ? O1 Nd1 O7 C11 100.6(11) . . . . ? O1 Nd1 O7 C11 -8.9(10) 2_665 . . . ? O1 Nd1 O7 C11 -130.6(11) 3_565 . . . ? O2 Nd1 O7 C11 -10.7(11) 2_665 . . . ? O2 Nd1 O7 C11 -128.5(10) . . . . ? O2 Nd1 O7 C11 -80.5(11) 3_565 . . . ? N1 Nd1 O7 C11 -11.0(11) 2_665 . . . ? N1 Nd1 O7 C11 -106.0(11) 3_565 . . . ? N4 C25 O8 Nd2 90.8(9) . . . . ? C19 C25 O8 Nd2 -92.2(9) . . . . ? O8 Nd2 O8 C25 -92.8(9) 3_455 . . . ? O8 Nd2 O8 C25 -176.5(8) 2_565 . . . ? O5 Nd2 O8 C25 -6.9(8) 2_565 . . . ? O5 Nd2 O8 C25 -113.0(8) . . . . ? O5 Nd2 O8 C25 113.4(8) 3_455 . . . ? O4 Nd2 O8 C25 -5.6(9) 2_565 . . . ? O4 Nd2 O8 C25 64.0(8) 3_455 . . . ? O4 Nd2 O8 C25 107.1(9) . . . . ? N2 Nd2 O8 C25 -3.4(8) 2_565 . . . ? N2 Nd2 O8 C25 89.3(8) 3_455 . . . ? C5 C6 O9 C7 13.3(8) . . . . ? C1 C6 O9 C7 -170.2(5) . . . . ? C8 C7 O9 C6 -173.2(6) . . . . ? C7 C8 O10 C9 -78.4(10) . . . . ? C10 C9 O10 C8 -171.4(6) . . . . ? C23 C24 O11 C10 -0.8(8) . . . . ? C19 C24 O11 C10 178.5(5) . . . . ? C9 C10 O11 C24 -176.7(5) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 23.57 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.264 _refine_diff_density_min -0.421 _refine_diff_density_rms 0.068 #===END data_compound4 _database_code_depnum_ccdc_archive 'CCDC 817223' #TrackingRef '- 1-12.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C96 H96 Eu2 N12 O33' _chemical_formula_weight 2249.77 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 Hexagonal _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 19.682(5) _cell_length_b 19.682(5) _cell_length_c 53.28(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 17876(12) _cell_formula_units_Z 6 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 6738 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 20.60 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.254 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6876 _exptl_absorpt_coefficient_mu 1.117 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7164 _exptl_absorpt_correction_T_max 0.7677 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38376 _diffrn_reflns_av_R_equivalents 0.0683 _diffrn_reflns_av_sigmaI/netI 0.0584 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -64 _diffrn_reflns_limit_l_max 64 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 25.50 _reflns_number_total 7408 _reflns_number_gt 4331 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Restraints to thermal parameters were applied on the disordered phenyl groups. 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. Diffuse electron densities resulting from residual disorder solvent moleculeswere removed from the data set using the SQUEEZE routine of PLATON andrefined further using the data generated. ; # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.333 0.667 0.167 1319 152 ' ' 2 0.000 0.000 0.500 1316 152 ' ' 3 -0.333 0.333 0.833 1319 152 ' ' _platon_squeeze_details ; ; _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^)+(0.1200P)^2^+297.0487P] 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 7408 _refine_ls_number_parameters 418 _refine_ls_number_restraints 72 _refine_ls_R_factor_all 0.1317 _refine_ls_R_factor_gt 0.0712 _refine_ls_wR_factor_ref 0.2666 _refine_ls_wR_factor_gt 0.2049 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.0980(12) 0.8232(13) 0.7139(3) 0.142(5) Uani 1 1 d U . . H1 H 0.0521 0.7884 0.7055 0.171 Uiso 1 1 calc R . . C2 C 0.1653(13) 0.8158(14) 0.7116(4) 0.156(5) Uani 1 1 d U . . H2 H 0.1642 0.7766 0.7015 0.187 Uiso 1 1 calc R . . C3 C 0.2320(14) 0.8665(15) 0.7241(4) 0.162(6) Uani 1 1 d U . . H3 H 0.2763 0.8615 0.7221 0.194 Uiso 1 1 calc R . . C4 C 0.2366(12) 0.9229(14) 0.7390(4) 0.150(5) Uani 1 1 d U . . H4 H 0.2836 0.9566 0.7471 0.180 Uiso 1 1 calc R . . C5 C 0.1664(10) 0.9320(11) 0.7429(3) 0.139(5) Uani 1 1 d U . . H5 H 0.1677 0.9685 0.7542 0.166 Uiso 1 1 calc R . . C6 C 0.1004(10) 0.8850(12) 0.7293(3) 0.122(4) Uani 1 1 d U . . C7 C 0.0280(8) 0.8952(7) 0.7319(2) 0.093(4) Uani 1 1 d . . . H7A H 0.0204 0.9025 0.7495 0.111 Uiso 1 1 calc R . . H7B H 0.0375 0.9420 0.7230 0.111 Uiso 1 1 calc R . . C8 C -0.0829(6) 0.8322(6) 0.70306(18) 0.059(2) Uani 1 1 d . . . C9 C -0.1555(6) 0.7595(5) 0.69567(17) 0.057(2) Uani 1 1 d . . . C10 C -0.2082(6) 0.7680(6) 0.6811(2) 0.071(3) Uani 1 1 d . . . H10 H -0.1961 0.8178 0.6757 0.085 Uiso 1 1 calc R . . C11 C -0.2784(7) 0.7045(8) 0.6744(2) 0.084(3) Uani 1 1 d . . . H11 H -0.3142 0.7114 0.6649 0.101 Uiso 1 1 calc R . . C12 C -0.2958(7) 0.6310(7) 0.6817(2) 0.085(4) Uani 1 1 d . . . H12 H -0.3437 0.5881 0.6772 0.102 Uiso 1 1 calc R . . C13 C -0.2434(8) 0.6191(7) 0.6958(2) 0.087(4) Uani 1 1 d . . . H13 H -0.2553 0.5686 0.7002 0.104 Uiso 1 1 calc R . . C14 C -0.1732(7) 0.6832(6) 0.7032(2) 0.073(3) Uani 1 1 d . . . C15 C -0.1300(11) 0.6090(8) 0.7271(3) 0.124(6) Uani 1 1 d . . . H15A H -0.1509 0.5671 0.7148 0.149 Uiso 1 1 calc R . . H15B H -0.1683 0.5945 0.7404 0.149 Uiso 1 1 calc R . . C16 C -0.0582(14) 0.6181(10) 0.7372(4) 0.166(9) Uani 1 1 d . . . H16A H -0.0712 0.5735 0.7480 0.199 Uiso 1 1 calc R . . H16B H -0.0273 0.6158 0.7234 0.199 Uiso 1 1 calc R . . C17 C -0.0317(9) 0.6898(9) 0.7752(3) 0.111(5) Uani 1 1 d . . . H17A H -0.0379 0.6446 0.7845 0.133 Uiso 1 1 calc R . . H17B H -0.0813 0.6892 0.7756 0.133 Uiso 1 1 calc R . . C18 C 0.0296(7) 0.7618(9) 0.7867(2) 0.090(4) Uani 1 1 d . . . H18A H 0.0401 0.8066 0.7764 0.108 Uiso 1 1 calc R . . H18B H 0.0131 0.7688 0.8032 0.108 Uiso 1 1 calc R . . C19 C 0.1666(7) 0.8175(7) 0.79722(18) 0.066(3) Uani 1 1 d . . . C20 C 0.1726(8) 0.8880(8) 0.8053(2) 0.079(3) Uani 1 1 d . . . H20 H 0.1284 0.8936 0.8051 0.095 Uiso 1 1 calc R . . C21 C 0.2413(8) 0.9479(8) 0.8136(2) 0.085(3) Uani 1 1 d . . . H21 H 0.2443 0.9941 0.8192 0.102 Uiso 1 1 calc R . . C22 C 0.3063(8) 0.9403(7) 0.8136(2) 0.086(3) Uani 1 1 d . . . H22 H 0.3540 0.9823 0.8188 0.103 Uiso 1 1 calc R . . C23 C 0.3028(7) 0.8704(7) 0.8060(2) 0.077(3) Uani 1 1 d . . . H23 H 0.3474 0.8655 0.8069 0.092 Uiso 1 1 calc R . . C24 C 0.2326(6) 0.8085(7) 0.79723(17) 0.064(3) Uani 1 1 d . . . C25 C 0.2344(7) 0.7380(7) 0.78893(19) 0.070(3) Uani 1 1 d . . . C26 C 0.1682(13) 0.6146(10) 0.7644(3) 0.154(8) Uani 1 1 d . . . H26A H 0.2158 0.6134 0.7680 0.185 Uiso 1 1 calc R . . H26B H 0.1259 0.5723 0.7737 0.185 Uiso 1 1 calc R . . C27 C 0.1517(8) 0.6008(8) 0.73849(19) 0.126(4) Uani 1 1 d GU . . C28 C 0.2110(7) 0.6543(7) 0.7229(3) 0.168(6) Uani 1 1 d GU . . H28 H 0.2570 0.6945 0.7298 0.201 Uiso 1 1 calc R . . C29 C 0.2014(9) 0.6478(8) 0.6970(3) 0.192(6) Uani 1 1 d GU . . H29 H 0.2410 0.6837 0.6866 0.230 Uiso 1 1 calc R . . C30 C 0.1326(10) 0.5878(10) 0.68669(19) 0.185(6) Uani 1 1 d GU . . H30 H 0.1262 0.5834 0.6694 0.222 Uiso 1 1 calc R . . C31 C 0.0733(7) 0.5342(8) 0.7023(3) 0.178(6) Uani 1 1 d GU . . H31 H 0.0273 0.4940 0.6954 0.213 Uiso 1 1 calc R . . C32 C 0.0829(7) 0.5407(8) 0.7282(3) 0.161(5) Uani 1 1 d GU . . H32 H 0.0433 0.5049 0.7386 0.193 Uiso 1 1 calc R . . Eu1 Eu 0.0000 1.0000 0.664703(16) 0.0523(3) Uani 1 3 d S . . Eu2 Eu 0.3333 0.6667 0.824717(18) 0.0625(3) Uani 1 3 d S . . N1 N -0.0428(6) 0.8286(5) 0.72233(18) 0.086(3) Uani 1 1 d . . . H1A H -0.0597 0.7840 0.7296 0.103 Uiso 1 1 calc R . . N2 N 0.1778(8) 0.6891(7) 0.7734(2) 0.116(4) Uani 1 1 d . . . H2A H 0.1445 0.7024 0.7683 0.139 Uiso 1 1 calc R . . N3 N 0.0666(6) 1.1456(6) 0.6365(2) 0.078(3) Uani 1 1 d . . . N4 N 0.4100(6) 0.6001(6) 0.8545(2) 0.090(3) Uani 1 1 d . . . O1 O -0.0648(4) 0.8945(4) 0.69251(12) 0.0616(17) Uani 1 1 d . . . O2 O -0.1174(6) 0.6767(5) 0.71619(18) 0.107(3) Uani 1 1 d . . . O3 O -0.0108(7) 0.6866(6) 0.7509(2) 0.123(4) Uani 1 1 d . . . O4 O 0.0991(5) 0.7552(5) 0.78873(15) 0.088(2) Uani 1 1 d . . . O5 O 0.2858(4) 0.7243(4) 0.79660(14) 0.0734(19) Uani 1 1 d . . . O6 O -0.0015(5) 1.0881(5) 0.63121(15) 0.080(2) Uani 1 1 d . . . O7 O 0.0939(6) 1.2045(6) 0.6233(2) 0.133(4) Uani 1 1 d . . . O8 O -0.1388(4) 0.9608(4) 0.65528(15) 0.0701(19) Uani 1 1 d . . . O9 O 0.4200(5) 0.6680(5) 0.85892(16) 0.090(2) Uani 1 1 d . . . O10 O 0.4324(6) 0.5684(6) 0.8689(2) 0.136(4) Uani 1 1 d . . . O11 O 0.3768(5) 0.5702(5) 0.83469(18) 0.090(2) 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 0.133(9) 0.182(11) 0.110(8) 0.050(8) 0.009(8) 0.078(9) C2 0.143(9) 0.195(11) 0.127(9) 0.038(8) 0.014(8) 0.083(9) C3 0.141(9) 0.198(12) 0.125(9) 0.045(8) 0.007(8) 0.069(9) C4 0.128(8) 0.189(11) 0.109(8) 0.061(8) -0.006(8) 0.060(9) C5 0.120(8) 0.176(10) 0.095(7) 0.064(7) -0.007(7) 0.055(8) C6 0.119(8) 0.158(10) 0.083(7) 0.061(7) -0.004(6) 0.065(8) C7 0.104(10) 0.067(8) 0.088(8) 0.007(6) -0.031(7) 0.028(7) C8 0.062(6) 0.058(6) 0.064(6) -0.003(5) 0.004(5) 0.036(5) C9 0.068(6) 0.051(5) 0.053(5) -0.002(4) 0.008(4) 0.030(5) C10 0.064(7) 0.059(6) 0.084(7) 0.002(5) 0.006(6) 0.028(6) C11 0.080(8) 0.083(9) 0.086(8) -0.008(6) -0.008(6) 0.038(7) C12 0.074(8) 0.060(7) 0.091(9) -0.018(6) 0.008(7) 0.011(6) C13 0.096(9) 0.059(7) 0.081(8) -0.005(6) -0.007(7) 0.021(7) C14 0.084(8) 0.054(6) 0.066(7) 0.000(5) 0.007(6) 0.025(6) C15 0.166(16) 0.065(8) 0.135(13) -0.016(8) -0.065(12) 0.053(10) C16 0.26(3) 0.092(12) 0.160(17) -0.036(11) -0.101(18) 0.101(15) C17 0.101(11) 0.102(11) 0.119(13) 0.026(9) 0.003(9) 0.044(10) C18 0.078(8) 0.120(11) 0.077(8) 0.002(7) -0.016(6) 0.053(8) C19 0.076(7) 0.077(7) 0.051(6) 0.001(5) -0.009(5) 0.043(6) C20 0.104(10) 0.098(9) 0.065(7) 0.009(6) 0.004(6) 0.073(8) C21 0.098(10) 0.076(8) 0.085(8) -0.005(6) -0.008(7) 0.048(8) C22 0.097(10) 0.068(8) 0.087(8) -0.003(6) -0.015(7) 0.037(7) C23 0.077(8) 0.094(9) 0.066(7) 0.008(6) 0.002(6) 0.048(7) C24 0.075(7) 0.080(7) 0.045(5) 0.003(5) -0.008(5) 0.045(6) C25 0.086(8) 0.080(8) 0.059(6) -0.004(5) -0.005(5) 0.052(7) C26 0.27(3) 0.132(14) 0.110(12) -0.052(11) -0.082(14) 0.138(17) C27 0.139(10) 0.157(11) 0.142(10) -0.062(8) -0.055(7) 0.118(8) C28 0.170(11) 0.183(12) 0.162(11) -0.058(9) -0.042(9) 0.098(9) C29 0.187(11) 0.201(12) 0.179(11) -0.052(10) -0.031(9) 0.090(10) C30 0.180(11) 0.206(12) 0.168(11) -0.065(9) -0.037(9) 0.096(10) C31 0.165(11) 0.200(12) 0.170(11) -0.083(9) -0.039(9) 0.093(10) C32 0.155(10) 0.186(11) 0.164(10) -0.072(9) -0.035(8) 0.102(9) Eu1 0.0465(3) 0.0465(3) 0.0639(5) 0.000 0.000 0.02326(17) Eu2 0.0559(4) 0.0559(4) 0.0758(6) 0.000 0.000 0.0279(2) N1 0.102(8) 0.051(5) 0.085(6) 0.014(4) -0.029(6) 0.023(5) N2 0.167(12) 0.117(9) 0.114(9) -0.050(7) -0.067(8) 0.110(9) N3 0.062(6) 0.069(6) 0.102(8) 0.023(6) 0.018(5) 0.032(5) N4 0.079(7) 0.067(7) 0.114(9) -0.006(6) -0.032(6) 0.029(6) O1 0.054(4) 0.050(4) 0.074(4) 0.013(3) 0.002(3) 0.021(3) O2 0.133(8) 0.056(5) 0.127(7) 0.007(5) -0.043(6) 0.044(5) O3 0.170(11) 0.096(7) 0.098(7) -0.026(6) -0.041(7) 0.063(8) O4 0.087(6) 0.098(6) 0.088(5) -0.016(5) -0.028(4) 0.053(5) O5 0.075(5) 0.075(5) 0.082(5) 0.004(4) -0.004(4) 0.046(4) O6 0.069(5) 0.077(5) 0.093(5) 0.020(4) -0.006(4) 0.035(4) O7 0.106(7) 0.111(8) 0.166(10) 0.080(8) 0.025(7) 0.042(6) O8 0.055(4) 0.067(5) 0.093(5) -0.011(4) -0.013(4) 0.034(4) O9 0.089(6) 0.075(6) 0.104(6) -0.008(5) -0.026(5) 0.040(5) O10 0.124(9) 0.096(7) 0.198(12) 0.021(7) -0.058(8) 0.062(7) O11 0.098(6) 0.082(6) 0.106(6) 0.006(5) 0.003(5) 0.058(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.41(3) . ? C1 C6 1.45(3) . ? C1 H1 0.9300 . ? C2 C3 1.36(3) . ? C2 H2 0.9300 . ? C3 C4 1.33(3) . ? C3 H3 0.9300 . ? C4 C5 1.49(3) . ? C4 H4 0.9300 . ? C5 C6 1.37(2) . ? C5 H5 0.9300 . ? C6 C7 1.54(2) . ? C7 N1 1.447(14) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 O1 1.229(11) . ? C8 N1 1.318(13) . ? C8 C9 1.484(14) . ? C9 C10 1.371(14) . ? C9 C14 1.420(14) . ? C10 C11 1.368(15) . ? C10 H10 0.9300 . ? C11 C12 1.368(17) . ? C11 H11 0.9300 . ? C12 C13 1.387(18) . ? C12 H12 0.9300 . ? C13 C14 1.382(16) . ? C13 H13 0.9300 . ? C14 O2 1.357(14) . ? C15 O2 1.359(15) . ? C15 C16 1.44(2) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 O3 1.401(18) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 O3 1.370(18) . ? C17 C18 1.458(19) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 O4 1.442(14) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 O4 1.357(13) . ? C19 C24 1.397(14) . ? C19 C20 1.401(15) . ? C20 C21 1.349(17) . ? C20 H20 0.9300 . ? C21 C22 1.359(17) . ? C21 H21 0.9300 . ? C22 C23 1.403(16) . ? C22 H22 0.9300 . ? C23 C24 1.389(15) . ? C23 H23 0.9300 . ? C24 C25 1.473(15) . ? C25 O5 1.238(12) . ? C25 N2 1.335(15) . ? C26 C27 1.413(16) . ? C26 N2 1.462(17) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.3900 . ? C27 C32 1.3900 . ? C28 C29 1.3900 . ? C28 H28 0.9300 . ? C29 C30 1.3900 . ? C29 H29 0.9300 . ? C30 C31 1.3900 . ? C30 H30 0.9300 . ? C31 C32 1.3900 . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? Eu1 O1 2.342(6) 2_675 ? Eu1 O1 2.342(6) . ? Eu1 O1 2.342(6) 3_465 ? Eu1 O8 2.490(7) 3_465 ? Eu1 O8 2.490(7) . ? Eu1 O8 2.490(7) 2_675 ? Eu1 O6 2.499(7) 2_675 ? Eu1 O6 2.499(7) 3_465 ? Eu1 O6 2.499(7) . ? Eu1 N3 2.905(10) 2_675 ? Eu1 N3 2.905(10) 3_465 ? Eu2 O5 2.339(7) . ? Eu2 O5 2.339(7) 2_665 ? Eu2 O5 2.339(7) 3_565 ? Eu2 O9 2.488(8) 2_665 ? Eu2 O9 2.488(8) 3_565 ? Eu2 O9 2.488(8) . ? Eu2 O11 2.498(8) 2_665 ? Eu2 O11 2.498(8) 3_565 ? Eu2 O11 2.498(8) . ? Eu2 N4 2.914(11) 2_665 ? Eu2 N4 2.914(11) 3_565 ? N1 H1A 0.8600 . ? N2 H2A 0.8600 . ? N3 O7 1.225(12) . ? N3 O8 1.237(11) 3_465 ? N3 O6 1.280(11) . ? N4 O10 1.201(13) . ? N4 O11 1.226(12) . ? N4 O9 1.271(12) . ? O8 N3 1.237(11) 2_675 ? 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 120(2) . . ? C2 C1 H1 120.0 . . ? C6 C1 H1 120.0 . . ? C3 C2 C1 120(3) . . ? C3 C2 H2 120.2 . . ? C1 C2 H2 120.2 . . ? C4 C3 C2 123(3) . . ? C4 C3 H3 118.6 . . ? C2 C3 H3 118.6 . . ? C3 C4 C5 120(2) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? C6 C5 C4 118(2) . . ? C6 C5 H5 121.0 . . ? C4 C5 H5 121.0 . . ? C5 C6 C1 119(2) . . ? C5 C6 C7 120(2) . . ? C1 C6 C7 121.1(17) . . ? N1 C7 C6 112.6(13) . . ? N1 C7 H7A 109.1 . . ? C6 C7 H7A 109.1 . . ? N1 C7 H7B 109.1 . . ? C6 C7 H7B 109.1 . . ? H7A C7 H7B 107.8 . . ? O1 C8 N1 121.9(10) . . ? O1 C8 C9 120.0(9) . . ? N1 C8 C9 117.9(9) . . ? C10 C9 C14 119.3(10) . . ? C10 C9 C8 117.1(9) . . ? C14 C9 C8 123.6(10) . . ? C11 C10 C9 121.0(11) . . ? C11 C10 H10 119.5 . . ? C9 C10 H10 119.5 . . ? C12 C11 C10 119.8(12) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? C11 C12 C13 121.3(12) . . ? C11 C12 H12 119.4 . . ? C13 C12 H12 119.4 . . ? C14 C13 C12 119.2(12) . . ? C14 C13 H13 120.4 . . ? C12 C13 H13 120.4 . . ? O2 C14 C13 123.1(11) . . ? O2 C14 C9 117.5(10) . . ? C13 C14 C9 119.3(12) . . ? O2 C15 C16 110.6(15) . . ? O2 C15 H15A 109.5 . . ? C16 C15 H15A 109.5 . . ? O2 C15 H15B 109.5 . . ? C16 C15 H15B 109.5 . . ? H15A C15 H15B 108.1 . . ? O3 C16 C15 117.1(15) . . ? O3 C16 H16A 108.0 . . ? C15 C16 H16A 108.0 . . ? O3 C16 H16B 108.0 . . ? C15 C16 H16B 108.0 . . ? H16A C16 H16B 107.3 . . ? O3 C17 C18 108.5(12) . . ? O3 C17 H17A 110.0 . . ? C18 C17 H17A 110.0 . . ? O3 C17 H17B 110.0 . . ? C18 C17 H17B 110.0 . . ? H17A C17 H17B 108.4 . . ? O4 C18 C17 107.8(12) . . ? O4 C18 H18A 110.1 . . ? C17 C18 H18A 110.1 . . ? O4 C18 H18B 110.1 . . ? C17 C18 H18B 110.1 . . ? H18A C18 H18B 108.5 . . ? O4 C19 C24 115.9(10) . . ? O4 C19 C20 123.9(11) . . ? C24 C19 C20 120.2(11) . . ? C21 C20 C19 121.2(12) . . ? C21 C20 H20 119.4 . . ? C19 C20 H20 119.4 . . ? C20 C21 C22 119.5(12) . . ? C20 C21 H21 120.3 . . ? C22 C21 H21 120.3 . . ? C21 C22 C23 121.4(12) . . ? C21 C22 H22 119.3 . . ? C23 C22 H22 119.3 . . ? C24 C23 C22 119.8(11) . . ? C24 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? C23 C24 C19 118.0(11) . . ? C23 C24 C25 116.5(10) . . ? C19 C24 C25 125.5(10) . . ? O5 C25 N2 121.8(10) . . ? O5 C25 C24 120.8(10) . . ? N2 C25 C24 117.4(10) . . ? C27 C26 N2 114.6(13) . . ? C27 C26 H26A 108.6 . . ? N2 C26 H26A 108.6 . . ? C27 C26 H26B 108.6 . . ? N2 C26 H26B 108.6 . . ? H26A C26 H26B 107.6 . . ? C28 C27 C32 120.0 . . ? C28 C27 C26 114.4(15) . . ? C32 C27 C26 125.6(15) . . ? C29 C28 C27 120.0 . . ? C29 C28 H28 120.0 . . ? C27 C28 H28 120.0 . . ? C28 C29 C30 120.0 . . ? C28 C29 H29 120.0 . . ? C30 C29 H29 120.0 . . ? C31 C30 C29 120.0 . . ? C31 C30 H30 120.0 . . ? C29 C30 H30 120.0 . . ? C32 C31 C30 120.0 . . ? C32 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? C31 C32 C27 120.0 . . ? C31 C32 H32 120.0 . . ? C27 C32 H32 120.0 . . ? O1 Eu1 O1 84.2(2) 2_675 . ? O1 Eu1 O1 84.2(2) 2_675 3_465 ? O1 Eu1 O1 84.2(2) . 3_465 ? O1 Eu1 O8 71.1(2) 2_675 3_465 ? O1 Eu1 O8 151.8(3) . 3_465 ? O1 Eu1 O8 80.0(2) 3_465 3_465 ? O1 Eu1 O8 151.8(3) 2_675 . ? O1 Eu1 O8 80.0(2) . . ? O1 Eu1 O8 71.1(2) 3_465 . ? O8 Eu1 O8 116.04(12) 3_465 . ? O1 Eu1 O8 80.0(2) 2_675 2_675 ? O1 Eu1 O8 71.1(2) . 2_675 ? O1 Eu1 O8 151.8(3) 3_465 2_675 ? O8 Eu1 O8 116.04(12) 3_465 2_675 ? O8 Eu1 O8 116.04(12) . 2_675 ? O1 Eu1 O6 151.3(2) 2_675 2_675 ? O1 Eu1 O6 87.0(3) . 2_675 ? O1 Eu1 O6 122.0(3) 3_465 2_675 ? O8 Eu1 O6 121.2(3) 3_465 2_675 ? O8 Eu1 O6 51.0(3) . 2_675 ? O8 Eu1 O6 71.3(3) 2_675 2_675 ? O1 Eu1 O6 87.0(3) 2_675 3_465 ? O1 Eu1 O6 122.0(3) . 3_465 ? O1 Eu1 O6 151.3(3) 3_465 3_465 ? O8 Eu1 O6 71.3(3) 3_465 3_465 ? O8 Eu1 O6 121.2(3) . 3_465 ? O8 Eu1 O6 51.0(3) 2_675 3_465 ? O6 Eu1 O6 74.6(3) 2_675 3_465 ? O1 Eu1 O6 122.0(3) 2_675 . ? O1 Eu1 O6 151.3(3) . . ? O1 Eu1 O6 87.0(3) 3_465 . ? O8 Eu1 O6 51.0(3) 3_465 . ? O8 Eu1 O6 71.3(3) . . ? O8 Eu1 O6 121.2(3) 2_675 . ? O6 Eu1 O6 74.6(3) 2_675 . ? O6 Eu1 O6 74.6(3) 3_465 . ? O1 Eu1 N3 168.3(3) 2_675 2_675 ? O1 Eu1 N3 84.2(3) . 2_675 ? O1 Eu1 N3 96.0(3) 3_465 2_675 ? O8 Eu1 N3 120.5(3) 3_465 2_675 ? O8 Eu1 N3 25.0(2) . 2_675 ? O8 Eu1 N3 94.9(3) 2_675 2_675 ? O6 Eu1 N3 26.0(3) 2_675 2_675 ? O6 Eu1 N3 97.9(3) 3_465 2_675 ? O6 Eu1 N3 69.6(3) . 2_675 ? O1 Eu1 N3 84.2(3) 2_675 3_465 ? O1 Eu1 N3 96.0(3) . 3_465 ? O1 Eu1 N3 168.3(3) 3_465 3_465 ? O8 Eu1 N3 94.9(3) 3_465 3_465 ? O8 Eu1 N3 120.5(3) . 3_465 ? O8 Eu1 N3 25.0(2) 2_675 3_465 ? O6 Eu1 N3 69.6(3) 2_675 3_465 ? O6 Eu1 N3 26.0(3) 3_465 3_465 ? O6 Eu1 N3 97.9(3) . 3_465 ? N3 Eu1 N3 95.6(3) 2_675 3_465 ? O5 Eu2 O5 83.4(3) . 2_665 ? O5 Eu2 O5 83.4(3) . 3_565 ? O5 Eu2 O5 83.4(3) 2_665 3_565 ? O5 Eu2 O9 90.0(3) . 2_665 ? O5 Eu2 O9 154.5(3) 2_665 2_665 ? O5 Eu2 O9 120.3(3) 3_565 2_665 ? O5 Eu2 O9 120.3(3) . 3_565 ? O5 Eu2 O9 90.0(3) 2_665 3_565 ? O5 Eu2 O9 154.5(3) 3_565 3_565 ? O9 Eu2 O9 72.2(3) 2_665 3_565 ? O5 Eu2 O9 154.5(3) . . ? O5 Eu2 O9 120.3(3) 2_665 . ? O5 Eu2 O9 90.0(3) 3_565 . ? O9 Eu2 O9 72.2(3) 2_665 . ? O9 Eu2 O9 72.2(3) 3_565 . ? O5 Eu2 O11 82.5(3) . 2_665 ? O5 Eu2 O11 151.3(3) 2_665 2_665 ? O5 Eu2 O11 70.3(3) 3_565 2_665 ? O9 Eu2 O11 50.1(3) 2_665 2_665 ? O9 Eu2 O11 118.7(3) 3_565 2_665 ? O9 Eu2 O11 72.1(3) . 2_665 ? O5 Eu2 O11 70.3(3) . 3_565 ? O5 Eu2 O11 82.5(3) 2_665 3_565 ? O5 Eu2 O11 151.3(3) 3_565 3_565 ? O9 Eu2 O11 72.1(3) 2_665 3_565 ? O9 Eu2 O11 50.1(3) 3_565 3_565 ? O9 Eu2 O11 118.7(3) . 3_565 ? O11 Eu2 O11 115.60(15) 2_665 3_565 ? O5 Eu2 O11 151.3(3) . . ? O5 Eu2 O11 70.3(3) 2_665 . ? O5 Eu2 O11 82.5(3) 3_565 . ? O9 Eu2 O11 118.7(3) 2_665 . ? O9 Eu2 O11 72.1(3) 3_565 . ? O9 Eu2 O11 50.1(3) . . ? O11 Eu2 O11 115.60(16) 2_665 . ? O11 Eu2 O11 115.60(15) 3_565 . ? O5 Eu2 N4 88.6(3) . 2_665 ? O5 Eu2 N4 171.9(3) 2_665 2_665 ? O5 Eu2 N4 94.7(3) 3_565 2_665 ? O9 Eu2 N4 25.7(3) 2_665 2_665 ? O9 Eu2 N4 95.0(3) 3_565 2_665 ? O9 Eu2 N4 67.5(3) . 2_665 ? O11 Eu2 N4 24.7(3) 2_665 2_665 ? O11 Eu2 N4 95.8(3) 3_565 2_665 ? O11 Eu2 N4 117.4(3) . 2_665 ? O5 Eu2 N4 94.7(3) . 3_565 ? O5 Eu2 N4 88.6(3) 2_665 3_565 ? O5 Eu2 N4 171.9(3) 3_565 3_565 ? O9 Eu2 N4 67.5(3) 2_665 3_565 ? O9 Eu2 N4 25.7(3) 3_565 3_565 ? O9 Eu2 N4 95.0(3) . 3_565 ? O11 Eu2 N4 117.4(3) 2_665 3_565 ? O11 Eu2 N4 24.7(3) 3_565 3_565 ? O11 Eu2 N4 95.8(3) . 3_565 ? N4 Eu2 N4 93.2(4) 2_665 3_565 ? C8 N1 C7 123.9(9) . . ? C8 N1 H1A 118.1 . . ? C7 N1 H1A 118.1 . . ? C25 N2 C26 124.7(12) . . ? C25 N2 H2A 117.7 . . ? C26 N2 H2A 117.7 . . ? O7 N3 O8 124.2(11) . 3_465 ? O7 N3 O6 118.7(11) . . ? O8 N3 O6 117.1(9) 3_465 . ? O10 N4 O11 123.1(12) . . ? O10 N4 O9 121.6(12) . . ? O11 N4 O9 115.4(10) . . ? C8 O1 Eu1 158.7(6) . . ? C14 O2 C15 123.4(11) . . ? C17 O3 C16 117.8(16) . . ? C19 O4 C18 119.2(10) . . ? C25 O5 Eu2 152.3(8) . . ? N3 O6 Eu1 95.0(6) . . ? N3 O8 Eu1 96.6(6) 2_675 . ? N4 O9 Eu2 96.2(7) . . ? N4 O11 Eu2 97.0(7) . . ? 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(3) . . . . ? C1 C2 C3 C4 1(3) . . . . ? C2 C3 C4 C5 1(3) . . . . ? C3 C4 C5 C6 -5(2) . . . . ? C4 C5 C6 C1 7(2) . . . . ? C4 C5 C6 C7 -177.3(12) . . . . ? C2 C1 C6 C5 -5(2) . . . . ? C2 C1 C6 C7 179.2(14) . . . . ? C5 C6 C7 N1 -163.5(12) . . . . ? C1 C6 C7 N1 12.6(18) . . . . ? O1 C8 C9 C10 -13.7(13) . . . . ? N1 C8 C9 C10 161.0(10) . . . . ? O1 C8 C9 C14 167.4(9) . . . . ? N1 C8 C9 C14 -17.9(14) . . . . ? C14 C9 C10 C11 2.1(16) . . . . ? C8 C9 C10 C11 -176.9(10) . . . . ? C9 C10 C11 C12 -1.8(18) . . . . ? C10 C11 C12 C13 -0.2(19) . . . . ? C11 C12 C13 C14 1.9(19) . . . . ? C12 C13 C14 O2 -177.5(11) . . . . ? C12 C13 C14 C9 -1.6(17) . . . . ? C10 C9 C14 O2 175.7(10) . . . . ? C8 C9 C14 O2 -5.4(15) . . . . ? C10 C9 C14 C13 -0.3(15) . . . . ? C8 C9 C14 C13 178.5(10) . . . . ? O2 C15 C16 O3 45(3) . . . . ? O3 C17 C18 O4 -67.2(14) . . . . ? O4 C19 C20 C21 -180.0(11) . . . . ? C24 C19 C20 C21 -0.8(16) . . . . ? C19 C20 C21 C22 1.1(18) . . . . ? C20 C21 C22 C23 -2.2(19) . . . . ? C21 C22 C23 C24 2.9(18) . . . . ? C22 C23 C24 C19 -2.5(15) . . . . ? C22 C23 C24 C25 178.2(10) . . . . ? O4 C19 C24 C23 -179.3(9) . . . . ? C20 C19 C24 C23 1.5(15) . . . . ? O4 C19 C24 C25 -0.1(15) . . . . ? C20 C19 C24 C25 -179.3(10) . . . . ? C23 C24 C25 O5 22.4(15) . . . . ? C19 C24 C25 O5 -156.8(10) . . . . ? C23 C24 C25 N2 -159.1(11) . . . . ? C19 C24 C25 N2 21.6(17) . . . . ? N2 C26 C27 C28 63(2) . . . . ? N2 C26 C27 C32 -115.8(16) . . . . ? C32 C27 C28 C29 0.0 . . . . ? C26 C27 C28 C29 -178.9(12) . . . . ? C27 C28 C29 C30 0.0 . . . . ? C28 C29 C30 C31 0.0 . . . . ? C29 C30 C31 C32 0.0 . . . . ? C30 C31 C32 C27 0.0 . . . . ? C28 C27 C32 C31 0.0 . . . . ? C26 C27 C32 C31 178.8(13) . . . . ? O1 C8 N1 C7 -3.9(18) . . . . ? C9 C8 N1 C7 -178.5(11) . . . . ? C6 C7 N1 C8 -116.3(13) . . . . ? O5 C25 N2 C26 2(2) . . . . ? C24 C25 N2 C26 -176.6(15) . . . . ? C27 C26 N2 C25 -135.8(17) . . . . ? N1 C8 O1 Eu1 85(2) . . . . ? C9 C8 O1 Eu1 -100.4(18) . . . . ? O1 Eu1 O1 C8 -76(2) 2_675 . . . ? O1 Eu1 O1 C8 -160.4(18) 3_465 . . . ? O8 Eu1 O1 C8 -104.3(19) 3_465 . . . ? O8 Eu1 O1 C8 127.9(19) . . . . ? O8 Eu1 O1 C8 5.8(18) 2_675 . . . ? O6 Eu1 O1 C8 77.0(19) 2_675 . . . ? O6 Eu1 O1 C8 7.2(19) 3_465 . . . ? O6 Eu1 O1 C8 126.7(18) . . . . ? N3 Eu1 O1 C8 103.0(19) 2_675 . . . ? N3 Eu1 O1 C8 7.9(19) 3_465 . . . ? C13 C14 O2 C15 -12(2) . . . . ? C9 C14 O2 C15 171.7(13) . . . . ? C16 C15 O2 C14 174.1(14) . . . . ? C18 C17 O3 C16 173.9(13) . . . . ? C15 C16 O3 C17 79(2) . . . . ? C24 C19 O4 C18 -176.2(9) . . . . ? C20 C19 O4 C18 3.0(15) . . . . ? C17 C18 O4 C19 175.3(10) . . . . ? N2 C25 O5 Eu2 -86.2(19) . . . . ? C24 C25 O5 Eu2 92.2(18) . . . . ? O5 Eu2 O5 C25 89.4(17) 2_665 . . . ? O5 Eu2 O5 C25 173.5(16) 3_565 . . . ? O9 Eu2 O5 C25 -65.9(16) 2_665 . . . ? O9 Eu2 O5 C25 3.4(17) 3_565 . . . ? O9 Eu2 O5 C25 -110.7(17) . . . . ? O11 Eu2 O5 C25 -115.6(16) 2_665 . . . ? O11 Eu2 O5 C25 5.1(16) 3_565 . . . ? O11 Eu2 O5 C25 112.6(16) . . . . ? N4 Eu2 O5 C25 -91.6(16) 2_665 . . . ? N4 Eu2 O5 C25 1.5(16) 3_565 . . . ? O7 N3 O6 Eu1 176.5(10) . . . . ? O8 N3 O6 Eu1 -5.9(10) 3_465 . . . ? O1 Eu1 O6 N3 1.6(7) 2_675 . . . ? O1 Eu1 O6 N3 155.2(6) . . . . ? O1 Eu1 O6 N3 82.9(6) 3_465 . . . ? O8 Eu1 O6 N3 3.4(6) 3_465 . . . ? O8 Eu1 O6 N3 153.9(7) . . . . ? O8 Eu1 O6 N3 -96.4(7) 2_675 . . . ? O6 Eu1 O6 N3 -152.7(6) 2_675 . . . ? O6 Eu1 O6 N3 -74.8(7) 3_465 . . . ? N3 Eu1 O6 N3 -179.6(7) 2_675 . . . ? N3 Eu1 O6 N3 -86.5(5) 3_465 . . . ? O1 Eu1 O8 N3 -154.8(6) 2_675 . . 2_675 ? O1 Eu1 O8 N3 -97.8(6) . . . 2_675 ? O1 Eu1 O8 N3 174.9(7) 3_465 . . 2_675 ? O8 Eu1 O8 N3 106.8(5) 3_465 . . 2_675 ? O8 Eu1 O8 N3 -34.7(7) 2_675 . . 2_675 ? O6 Eu1 O8 N3 -3.5(6) 2_675 . . 2_675 ? O6 Eu1 O8 N3 23.7(7) 3_465 . . 2_675 ? O6 Eu1 O8 N3 81.6(6) . . . 2_675 ? N3 Eu1 O8 N3 -6.7(7) 3_465 . . 2_675 ? O10 N4 O9 Eu2 -169.2(12) . . . . ? O11 N4 O9 Eu2 11.3(12) . . . . ? O5 Eu2 O9 N4 -161.1(7) . . . . ? O5 Eu2 O9 N4 -4.4(8) 2_665 . . . ? O5 Eu2 O9 N4 -86.7(7) 3_565 . . . ? O9 Eu2 O9 N4 151.3(8) 2_665 . . . ? O9 Eu2 O9 N4 74.8(9) 3_565 . . . ? O11 Eu2 O9 N4 -155.9(8) 2_665 . . . ? O11 Eu2 O9 N4 94.1(8) 3_565 . . . ? O11 Eu2 O9 N4 -6.5(7) . . . . ? N4 Eu2 O9 N4 178.2(9) 2_665 . . . ? N4 Eu2 O9 N4 86.9(6) 3_565 . . . ? O10 N4 O11 Eu2 169.3(12) . . . . ? O9 N4 O11 Eu2 -11.2(12) . . . . ? O5 Eu2 O11 N4 164.2(7) . . . . ? O5 Eu2 O11 N4 -171.3(8) 2_665 . . . ? O5 Eu2 O11 N4 103.0(8) 3_565 . . . ? O9 Eu2 O11 N4 -17.5(9) 2_665 . . . ? O9 Eu2 O11 N4 -74.7(8) 3_565 . . . ? O9 Eu2 O11 N4 6.7(7) . . . . ? O11 Eu2 O11 N4 39.2(9) 2_665 . . . ? O11 Eu2 O11 N4 -100.3(7) 3_565 . . . ? N4 Eu2 O11 N4 11.6(8) 2_665 . . . ? N4 Eu2 O11 N4 -85.0(9) 3_565 . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.410 _refine_diff_density_min -0.825 _refine_diff_density_rms 0.151 #===END data_compound7 _database_code_depnum_ccdc_archive 'CCDC 817224' #TrackingRef '- 1-12.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H54 La N6 O18' _chemical_formula_weight 1177.91 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.721(7) _cell_length_b 14.110(9) _cell_length_c 19.522(12) _cell_angle_alpha 81.873(7) _cell_angle_beta 88.382(8) _cell_angle_gamma 66.118(7) _cell_volume 2921(3) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 1944 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 19.21 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.339 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1206 _exptl_absorpt_coefficient_mu 0.803 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8065 _exptl_absorpt_correction_T_max 0.8495 _exptl_absorpt_process_details SADABS _exptl_special_details ; Problem: diffrn_measured_fraction_theta_full Low 0.96 Response: The limited quality of the crystals gives rise to the weak diffraction,leading to the relatively low data completeness ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 14041 _diffrn_reflns_av_R_equivalents 0.0490 _diffrn_reflns_av_sigmaI/netI 0.1243 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 25.25 _reflns_number_total 9690 _reflns_number_gt 6153 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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. Diffuse electron densities resulting from residual disorder solvent moleculeswere removed from the data set using the SQUEEZE routine of PLATON andrefined further using the data generated. ; _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^)+(0.0320P)^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 9690 _refine_ls_number_parameters 685 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0996 _refine_ls_R_factor_gt 0.0580 _refine_ls_wR_factor_ref 0.1173 _refine_ls_wR_factor_gt 0.1077 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.500 0.000 445 70 ' ' _platon_squeeze_details ; ; 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 La1 La -0.12068(3) 0.75386(3) 0.738424(19) 0.03937(13) Uani 1 1 d . . . C1 C 0.2632(7) 0.7483(7) 0.5785(4) 0.073(2) Uani 1 1 d . . . H1A H 0.1846 0.7680 0.5582 0.087 Uiso 1 1 calc R . . C2 C 0.3326(8) 0.8076(7) 0.5600(5) 0.096(3) Uani 1 1 d . . . H2A H 0.2983 0.8671 0.5273 0.115 Uiso 1 1 calc R . . C3 C 0.4496(10) 0.7823(9) 0.5879(6) 0.110(3) Uani 1 1 d . . . H3A H 0.4946 0.8225 0.5739 0.132 Uiso 1 1 calc R . . C4 C 0.4962(8) 0.6971(10) 0.6361(5) 0.107(4) Uani 1 1 d . . . H4 H 0.5741 0.6793 0.6568 0.128 Uiso 1 1 calc R . . C5 C 0.4277(7) 0.6321(8) 0.6567(4) 0.095(3) Uani 1 1 d . . . H5 H 0.4612 0.5724 0.6893 0.113 Uiso 1 1 calc R . . C6 C 0.3111(6) 0.6624(7) 0.6258(4) 0.061(2) Uani 1 1 d . . . C7 C 0.2392(6) 0.5975(6) 0.6485(3) 0.071(2) Uani 1 1 d . . . H7A H 0.2969 0.5253 0.6619 0.086 Uiso 1 1 calc R . . H7B H 0.1917 0.6222 0.6886 0.086 Uiso 1 1 calc R . . C8 C 0.0339(6) 0.6258(5) 0.6008(3) 0.0432(16) Uani 1 1 d . . . C9 C -0.0439(5) 0.6336(5) 0.5398(3) 0.0461(16) Uani 1 1 d . . . C10 C -0.1642(6) 0.6366(5) 0.5531(4) 0.062(2) Uani 1 1 d . . . H10 H -0.1901 0.6336 0.5985 0.075 Uiso 1 1 calc R . . C11 C -0.2435(7) 0.6438(6) 0.5008(4) 0.080(2) Uani 1 1 d . . . H11 H -0.3222 0.6450 0.5103 0.096 Uiso 1 1 calc R . . C12 C -0.2048(7) 0.6493(6) 0.4342(4) 0.076(2) Uani 1 1 d . . . H12 H -0.2582 0.6542 0.3983 0.091 Uiso 1 1 calc R . . C13 C -0.0871(6) 0.6477(5) 0.4190(4) 0.065(2) Uani 1 1 d . . . H13 H -0.0628 0.6522 0.3733 0.078 Uiso 1 1 calc R . . C14 C -0.0076(6) 0.6394(5) 0.4718(3) 0.0514(18) Uani 1 1 d . . . C15 C 0.1587(7) 0.6304(7) 0.3953(4) 0.082(2) Uani 1 1 d . . . H15A H 0.1069 0.6878 0.3612 0.099 Uiso 1 1 calc R . . H15B H 0.1677 0.5649 0.3808 0.099 Uiso 1 1 calc R . . C16 C 0.2852(7) 0.6334(7) 0.4044(4) 0.088(3) Uani 1 1 d . . . H16A H 0.3298 0.6240 0.3616 0.106 Uiso 1 1 calc R . . H16B H 0.2754 0.7001 0.4174 0.106 Uiso 1 1 calc R . . C18 C 0.0955(7) 0.2265(7) 0.7895(4) 0.076(2) Uani 1 1 d . . . H18 H 0.1800 0.2131 0.7889 0.091 Uiso 1 1 calc R . . C19 C 0.0592(9) 0.1436(7) 0.8003(5) 0.098(3) Uani 1 1 d . . . H19 H 0.1184 0.0748 0.8071 0.118 Uiso 1 1 calc R . . C20 C -0.0618(12) 0.1646(9) 0.8005(5) 0.102(3) Uani 1 1 d . . . H20 H -0.0877 0.1099 0.8069 0.122 Uiso 1 1 calc R . . C21 C -0.1512(9) 0.2683(10) 0.7913(4) 0.099(3) Uani 1 1 d . . . H21 H -0.2359 0.2822 0.7923 0.119 Uiso 1 1 calc R . . C22 C -0.1132(7) 0.3489(7) 0.7809(4) 0.072(2) Uani 1 1 d . . . H22 H -0.1719 0.4179 0.7745 0.087 Uiso 1 1 calc R . . C23 C 0.0082(7) 0.3282(6) 0.7798(3) 0.0557(18) Uani 1 1 d . . . C24 C 0.0517(6) 0.4152(5) 0.7704(3) 0.063(2) Uani 1 1 d . . . H24A H 0.1230 0.3979 0.7408 0.076 Uiso 1 1 calc R . . H24B H -0.0144 0.4791 0.7484 0.076 Uiso 1 1 calc R . . C25 C 0.0668(6) 0.5208(6) 0.8574(3) 0.0480(17) Uani 1 1 d . . . C26 C 0.1110(5) 0.5217(5) 0.9275(3) 0.0452(16) Uani 1 1 d . . . C27 C 0.0829(6) 0.6180(5) 0.9489(3) 0.062(2) Uani 1 1 d . . . H27 H 0.0377 0.6780 0.9184 0.074 Uiso 1 1 calc R . . C28 C 0.1179(7) 0.6295(6) 1.0121(4) 0.073(2) Uani 1 1 d . . . H28 H 0.0941 0.6955 1.0253 0.088 Uiso 1 1 calc R . . C29 C 0.1888(7) 0.5413(7) 1.0553(4) 0.074(2) Uani 1 1 d . . . H29 H 0.2157 0.5477 1.0981 0.089 Uiso 1 1 calc R . . C30 C 0.2216(6) 0.4433(6) 1.0373(3) 0.069(2) Uani 1 1 d . . . H30 H 0.2709 0.3843 1.0675 0.083 Uiso 1 1 calc R . . C31 C 0.1811(6) 0.4324(5) 0.9741(3) 0.0503(17) Uani 1 1 d . . . C32 C 0.2589(7) 0.2453(5) 1.0070(3) 0.071(2) Uani 1 1 d . . . H32A H 0.2110 0.2576 1.0486 0.085 Uiso 1 1 calc R . . H32B H 0.3445 0.2320 1.0185 0.085 Uiso 1 1 calc R . . C33 C 0.2545(8) 0.1539(6) 0.9799(4) 0.087(3) Uani 1 1 d . . . H33A H 0.2688 0.0974 1.0177 0.104 Uiso 1 1 calc R . . H33B H 0.1725 0.1730 0.9593 0.104 Uiso 1 1 calc R . . C34 C 0.3779(9) 0.0121(7) 0.9261(5) 0.100(3) Uani 1 1 d . . . H34A H 0.3031 0.0003 0.9203 0.120 Uiso 1 1 calc R . . H34B H 0.4214 -0.0305 0.9685 0.120 Uiso 1 1 calc R . . C35 C 0.3627(9) 0.7385(8) 0.9284(5) 0.119(4) Uani 1 1 d . . . H35 H 0.4321 0.6922 0.9083 0.143 Uiso 1 1 calc R . . C36 C 0.3747(14) 0.7625(12) 0.9908(7) 0.151(5) Uani 1 1 d . . . H36 H 0.4532 0.7326 1.0127 0.181 Uiso 1 1 calc R . . C37 C 0.2807(17) 0.8265(13) 1.0228(7) 0.153(7) Uani 1 1 d . . . H37 H 0.2913 0.8382 1.0674 0.183 Uiso 1 1 calc R . . C38 C 0.1696(14) 0.8741(9) 0.9894(7) 0.132(4) Uani 1 1 d . . . H38 H 0.1033 0.9235 1.0095 0.159 Uiso 1 1 calc R . . C39 C 0.1525(10) 0.8498(8) 0.9241(7) 0.112(3) Uani 1 1 d . . . H39 H 0.0744 0.8809 0.9017 0.134 Uiso 1 1 calc R . . C40 C 0.2504(9) 0.7809(7) 0.8941(4) 0.081(3) Uani 1 1 d . . . C41 C 0.2365(8) 0.7484(6) 0.8249(4) 0.093(3) Uani 1 1 d . . . H41A H 0.3145 0.6934 0.8143 0.112 Uiso 1 1 calc R . . H41B H 0.1725 0.7211 0.8275 0.112 Uiso 1 1 calc R . . C42 C 0.1107(6) 0.8659(6) 0.7241(3) 0.0543(18) Uani 1 1 d . . . C43 C 0.0936(6) 0.9544(5) 0.6687(3) 0.0513(17) Uani 1 1 d . . . C44 C -0.0127(7) 0.9911(6) 0.6274(4) 0.079(2) Uani 1 1 d . . . H44 H -0.0722 0.9638 0.6384 0.095 Uiso 1 1 calc R . . C45 C -0.0344(9) 1.0658(7) 0.5710(5) 0.107(3) Uani 1 1 d . . . H45 H -0.1084 1.0903 0.5448 0.128 Uiso 1 1 calc R . . C46 C 0.0533(10) 1.1042(6) 0.5535(4) 0.099(3) Uani 1 1 d . . . H46 H 0.0415 1.1523 0.5137 0.119 Uiso 1 1 calc R . . C47 C 0.1582(8) 1.0726(6) 0.5940(4) 0.076(2) Uani 1 1 d . . . H47 H 0.2166 1.1006 0.5821 0.091 Uiso 1 1 calc R . . C48 C 0.1794(6) 0.9993(6) 0.6527(4) 0.0587(19) Uani 1 1 d . . . C49 C 0.3652(7) 1.0149(6) 0.6849(4) 0.081(2) Uani 1 1 d . . . H49A H 0.3210 1.0905 0.6792 0.097 Uiso 1 1 calc R . . H49B H 0.4116 0.9955 0.6435 0.097 Uiso 1 1 calc R . . C50 C 0.4522(7) 0.9776(6) 0.7472(4) 0.086(3) Uani 1 1 d . . . H50A H 0.4893 0.9017 0.7556 0.103 Uiso 1 1 calc R . . H50B H 0.5187 1.0018 0.7393 0.103 Uiso 1 1 calc R . . C51 C 0.4595(8) 0.9818(7) 0.8664(5) 0.101(3) Uani 1 1 d . . . H51A H 0.5201 1.0127 0.8643 0.121 Uiso 1 1 calc R . . H51B H 0.5043 0.9062 0.8716 0.121 Uiso 1 1 calc R . . C52 C 0.4707(6) 0.5458(5) 0.4734(4) 0.079(2) Uani 1 1 d . . . H52A H 0.4629 0.6092 0.4908 0.094 Uiso 1 1 calc R . . H52B H 0.5205 0.5384 0.4324 0.094 Uiso 1 1 calc R . . N1 N 0.1543(5) 0.6025(4) 0.5936(3) 0.0586(16) Uani 1 1 d . . . H1 H 0.1848 0.5895 0.5537 0.070 Uiso 1 1 calc R . . N2 N 0.0861(5) 0.4312(4) 0.8372(3) 0.0615(16) Uani 1 1 d . . . H2 H 0.1231 0.3759 0.8667 0.074 Uiso 1 1 calc R . . N3 N 0.2026(5) 0.8378(5) 0.7702(3) 0.0747(18) Uani 1 1 d . . . H3 H 0.2458 0.8750 0.7678 0.090 Uiso 1 1 calc R . . N4 N -0.3029(6) 0.6630(5) 0.7875(3) 0.0672(18) Uani 1 1 d . . . N5 N -0.1969(6) 0.9286(6) 0.8230(4) 0.0671(17) Uani 1 1 d . . . N6 N -0.2831(6) 0.8747(5) 0.6144(4) 0.0734(19) Uani 1 1 d . . . O1 O -0.0128(4) 0.6386(3) 0.6586(2) 0.0620(13) Uani 1 1 d . . . O2 O 0.1063(4) 0.6403(4) 0.4619(2) 0.0707(14) Uani 1 1 d . . . O3 O 0.3515(5) 0.5503(4) 0.4576(3) 0.0798(15) Uani 1 1 d . . . O4 O 0.0116(4) 0.6062(3) 0.8182(2) 0.0592(12) Uani 1 1 d . . . O5 O 0.2075(4) 0.3355(4) 0.9550(2) 0.0660(13) Uani 1 1 d . . . O6 O 0.3448(5) 0.1204(4) 0.9307(3) 0.0880(17) Uani 1 1 d . . . O7 O 0.0429(4) 0.8161(3) 0.7268(2) 0.0582(12) Uani 1 1 d . . . O8 O 0.2793(4) 0.9667(4) 0.6959(2) 0.0723(14) Uani 1 1 d . . . O9 O 0.3840(5) 1.0176(4) 0.8050(3) 0.0914(17) Uani 1 1 d . . . O10 O -0.2276(4) 0.6251(4) 0.7417(3) 0.0651(14) Uani 1 1 d . . . O11 O -0.3841(5) 0.6320(5) 0.8067(3) 0.098(2) Uani 1 1 d . . . O12 O -0.2929(4) 0.7373(4) 0.8139(2) 0.0660(13) Uani 1 1 d . . . O13 O -0.1265(5) 0.8341(4) 0.8485(2) 0.0694(14) Uani 1 1 d . . . O14 O -0.2246(6) 1.0007(5) 0.8570(3) 0.105(2) Uani 1 1 d . . . O15 O -0.2362(4) 0.9428(3) 0.7609(3) 0.0709(14) Uani 1 1 d . . . O16 O -0.3219(4) 0.8308(4) 0.6647(3) 0.0697(14) Uani 1 1 d . . . O17 O -0.3504(5) 0.9263(5) 0.5651(3) 0.119(2) Uani 1 1 d . . . O18 O -0.1691(4) 0.8602(4) 0.6177(2) 0.0740(15) 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 La1 0.0406(2) 0.0476(2) 0.0316(2) -0.00243(16) 0.00121(15) -0.02063(17) C1 0.060(5) 0.077(6) 0.088(6) -0.022(5) -0.004(5) -0.032(5) C2 0.082(6) 0.092(7) 0.116(8) -0.046(6) 0.003(6) -0.028(6) C3 0.104(8) 0.130(10) 0.117(9) -0.048(7) 0.009(7) -0.060(7) C4 0.065(6) 0.174(12) 0.103(8) -0.064(8) -0.001(6) -0.056(7) C5 0.061(5) 0.145(9) 0.069(6) -0.037(6) -0.003(4) -0.025(6) C6 0.045(4) 0.092(6) 0.056(5) -0.028(5) 0.006(4) -0.031(4) C7 0.070(5) 0.084(6) 0.048(4) -0.004(4) -0.012(4) -0.019(5) C8 0.053(4) 0.044(4) 0.040(4) -0.008(3) 0.011(3) -0.026(3) C9 0.041(4) 0.050(4) 0.052(4) -0.012(3) 0.003(3) -0.022(3) C10 0.066(5) 0.074(5) 0.060(5) -0.022(4) 0.011(4) -0.039(4) C11 0.068(5) 0.107(7) 0.083(6) -0.030(5) 0.008(5) -0.048(5) C12 0.066(5) 0.081(6) 0.089(6) -0.024(5) -0.023(5) -0.033(4) C13 0.067(5) 0.075(5) 0.051(4) -0.015(4) -0.004(4) -0.023(4) C14 0.051(4) 0.062(5) 0.048(4) -0.011(4) 0.002(4) -0.029(4) C15 0.072(5) 0.133(8) 0.047(5) -0.016(5) 0.014(4) -0.047(5) C16 0.076(6) 0.134(8) 0.057(5) -0.012(5) 0.030(5) -0.047(6) C18 0.066(5) 0.069(6) 0.097(6) -0.028(5) 0.007(5) -0.027(5) C19 0.091(7) 0.075(7) 0.139(9) -0.018(6) 0.003(6) -0.044(6) C20 0.140(10) 0.113(9) 0.092(7) -0.030(7) 0.019(7) -0.088(8) C21 0.079(7) 0.157(11) 0.074(6) -0.038(7) 0.009(5) -0.055(8) C22 0.071(6) 0.087(7) 0.060(5) -0.020(5) 0.002(4) -0.030(5) C23 0.062(5) 0.056(5) 0.050(4) -0.012(4) -0.004(4) -0.023(4) C24 0.085(5) 0.067(5) 0.041(4) -0.011(4) -0.009(4) -0.033(4) C25 0.060(4) 0.054(5) 0.037(4) -0.001(4) -0.001(3) -0.031(4) C26 0.048(4) 0.046(4) 0.041(4) -0.005(3) -0.002(3) -0.019(3) C27 0.082(5) 0.056(5) 0.051(4) -0.008(4) -0.004(4) -0.032(4) C28 0.110(6) 0.066(6) 0.055(5) -0.015(4) -0.012(5) -0.044(5) C29 0.099(6) 0.080(6) 0.055(5) -0.014(5) -0.010(5) -0.045(5) C30 0.088(5) 0.075(6) 0.032(4) 0.002(4) -0.007(4) -0.023(5) C31 0.060(4) 0.052(5) 0.037(4) -0.006(4) 0.002(3) -0.021(4) C32 0.093(6) 0.056(5) 0.050(5) 0.011(4) -0.002(4) -0.021(4) C33 0.108(7) 0.056(6) 0.087(7) -0.001(5) 0.018(6) -0.027(5) C34 0.121(8) 0.065(7) 0.101(7) -0.017(5) -0.006(6) -0.023(6) C35 0.100(7) 0.176(11) 0.071(6) -0.001(7) -0.021(6) -0.050(7) C36 0.159(13) 0.223(17) 0.096(11) -0.007(10) -0.037(9) -0.105(12) C37 0.23(2) 0.210(19) 0.073(10) 0.004(10) 0.001(11) -0.150(17) C38 0.189(14) 0.109(10) 0.122(11) -0.044(9) 0.052(10) -0.076(10) C39 0.112(9) 0.081(8) 0.146(11) -0.006(7) 0.004(8) -0.046(7) C40 0.092(7) 0.096(7) 0.064(6) 0.010(5) -0.016(5) -0.051(6) C41 0.130(7) 0.072(6) 0.072(6) 0.014(5) -0.028(5) -0.040(5) C42 0.055(4) 0.061(5) 0.049(4) -0.007(4) -0.001(4) -0.026(4) C43 0.063(5) 0.045(4) 0.047(4) -0.004(3) 0.001(4) -0.024(4) C44 0.081(5) 0.074(6) 0.094(6) 0.008(5) -0.025(5) -0.048(5) C45 0.136(8) 0.085(7) 0.102(7) 0.049(6) -0.059(6) -0.064(6) C46 0.151(9) 0.072(6) 0.084(6) 0.028(5) -0.031(6) -0.065(7) C47 0.108(7) 0.059(6) 0.075(6) 0.003(5) 0.005(5) -0.052(5) C48 0.060(5) 0.066(5) 0.061(5) -0.015(4) 0.007(4) -0.035(4) C49 0.070(5) 0.084(6) 0.100(6) -0.014(5) 0.014(5) -0.043(5) C50 0.056(5) 0.097(7) 0.112(7) -0.031(6) 0.013(5) -0.034(5) C51 0.079(6) 0.093(7) 0.107(7) -0.026(6) -0.018(6) -0.005(5) C52 0.066(5) 0.086(7) 0.101(7) -0.029(5) 0.017(5) -0.044(5) N1 0.048(3) 0.086(4) 0.041(3) -0.019(3) -0.001(3) -0.022(3) N2 0.094(4) 0.048(4) 0.042(3) -0.004(3) -0.021(3) -0.027(3) N3 0.089(4) 0.078(5) 0.067(4) 0.009(4) -0.022(4) -0.050(4) N4 0.063(5) 0.074(5) 0.061(5) 0.005(4) -0.005(4) -0.028(4) N5 0.073(5) 0.074(5) 0.068(5) -0.026(4) 0.025(4) -0.039(4) N6 0.068(5) 0.082(5) 0.069(5) 0.005(4) -0.023(4) -0.034(4) O1 0.068(3) 0.076(4) 0.045(3) -0.011(3) 0.013(2) -0.033(3) O2 0.061(3) 0.125(4) 0.039(3) -0.018(3) 0.009(2) -0.049(3) O3 0.068(3) 0.103(4) 0.083(4) -0.018(3) 0.010(3) -0.048(3) O4 0.078(3) 0.054(3) 0.042(3) -0.001(2) -0.012(2) -0.024(3) O5 0.089(3) 0.050(3) 0.047(3) -0.001(2) -0.007(3) -0.018(3) O6 0.100(4) 0.065(4) 0.093(4) -0.020(3) 0.021(3) -0.026(3) O7 0.061(3) 0.065(3) 0.060(3) -0.004(2) 0.006(2) -0.039(3) O8 0.065(3) 0.081(4) 0.088(4) -0.002(3) 0.000(3) -0.051(3) O9 0.062(3) 0.089(4) 0.108(5) -0.033(4) 0.004(3) -0.008(3) O10 0.060(3) 0.065(3) 0.074(4) -0.011(3) 0.009(3) -0.028(3) O11 0.086(4) 0.157(6) 0.083(4) 0.003(4) 0.008(3) -0.088(4) O12 0.069(3) 0.071(4) 0.055(3) -0.006(3) 0.014(3) -0.027(3) O13 0.083(4) 0.061(4) 0.061(3) -0.012(3) -0.002(3) -0.024(3) O14 0.143(5) 0.090(5) 0.096(4) -0.050(4) 0.033(4) -0.050(4) O15 0.076(3) 0.063(3) 0.063(3) -0.009(3) -0.003(3) -0.017(3) O16 0.062(3) 0.086(4) 0.061(3) 0.014(3) -0.006(3) -0.038(3) O17 0.103(4) 0.155(6) 0.093(4) 0.054(4) -0.050(4) -0.065(4) O18 0.072(3) 0.101(4) 0.061(3) 0.016(3) -0.018(3) -0.055(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag La1 O1 2.369(5) . ? La1 O4 2.402(4) . ? La1 O7 2.405(4) . ? La1 O12 2.533(5) . ? La1 O16 2.547(4) . ? La1 O15 2.552(5) . ? La1 O18 2.553(4) . ? La1 O13 2.553(5) . ? La1 O10 2.585(5) . ? La1 N6 2.977(6) . ? La1 N4 2.980(8) . ? La1 N5 2.981(7) . ? C1 C6 1.342(9) . ? C1 C2 1.393(10) . ? C1 H1A 0.9300 . ? C2 C3 1.377(11) . ? C2 H2A 0.9300 . ? C3 C4 1.344(12) . ? C3 H3A 0.9300 . ? C4 C5 1.456(12) . ? C4 H4 0.9300 . ? C5 C6 1.383(9) . ? C5 H5 0.9300 . ? C6 C7 1.495(9) . ? C7 N1 1.458(7) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 O1 1.244(6) . ? C8 N1 1.322(7) . ? C8 C9 1.485(8) . ? C9 C14 1.384(8) . ? C9 C10 1.411(8) . ? C10 C11 1.364(9) . ? C10 H10 0.9300 . ? C11 C12 1.366(9) . ? C11 H11 0.9300 . ? C12 C13 1.395(9) . ? C12 H12 0.9300 . ? C13 C14 1.370(8) . ? C13 H13 0.9300 . ? C14 O2 1.349(7) . ? C15 O2 1.422(7) . ? C15 C16 1.515(9) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 O3 1.421(8) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C18 C23 1.374(9) . ? C18 C19 1.385(10) . ? C18 H18 0.9300 . ? C19 C20 1.327(11) . ? C19 H19 0.9300 . ? C20 C21 1.402(11) . ? C20 H20 0.9300 . ? C21 C22 1.369(11) . ? C21 H21 0.9300 . ? C22 C23 1.332(9) . ? C22 H22 0.9300 . ? C23 C24 1.496(8) . ? C24 N2 1.450(7) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 O4 1.263(7) . ? C25 N2 1.307(7) . ? C25 C26 1.481(8) . ? C26 C27 1.385(8) . ? C26 C31 1.403(8) . ? C27 C28 1.362(8) . ? C27 H27 0.9300 . ? C28 C29 1.363(9) . ? C28 H28 0.9300 . ? C29 C30 1.372(9) . ? C29 H29 0.9300 . ? C30 C31 1.385(8) . ? C30 H30 0.9300 . ? C31 O5 1.378(7) . ? C32 O5 1.435(7) . ? C32 C33 1.480(9) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 O6 1.390(8) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 O6 1.432(8) . ? C34 C51 1.484(10) 1_545 ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.335(13) . ? C35 C40 1.356(10) . ? C35 H35 0.9300 . ? C36 C37 1.317(15) . ? C36 H36 0.9300 . ? C37 C38 1.337(15) . ? C37 H37 0.9300 . ? C38 C39 1.406(13) . ? C38 H38 0.9300 . ? C39 C40 1.351(11) . ? C39 H39 0.9300 . ? C40 C41 1.519(10) . ? C41 N3 1.459(8) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 O7 1.253(7) . ? C42 N3 1.316(7) . ? C42 C43 1.482(8) . ? C43 C44 1.373(8) . ? C43 C48 1.397(8) . ? C44 C45 1.365(9) . ? C44 H44 0.9300 . ? C45 C46 1.358(10) . ? C45 H45 0.9300 . ? C46 C47 1.359(10) . ? C46 H46 0.9300 . ? C47 C48 1.384(9) . ? C47 H47 0.9300 . ? C48 O8 1.344(7) . ? C49 O8 1.422(7) . ? C49 C50 1.500(9) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 O9 1.413(8) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C51 O9 1.415(8) . ? C51 C34 1.484(10) 1_565 ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C52 O3 1.413(8) . ? C52 C52 1.470(13) 2_666 ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? N1 H1 0.8600 . ? N2 H2 0.8600 . ? N3 H3 0.8600 . ? N4 O11 1.227(7) . ? N4 O10 1.253(7) . ? N4 O12 1.279(7) . ? N5 O14 1.221(7) . ? N5 O15 1.268(7) . ? N5 O13 1.285(7) . ? N6 O17 1.208(7) . ? N6 O16 1.260(7) . ? N6 O18 1.270(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 La1 O4 80.66(15) . . ? O1 La1 O7 86.95(15) . . ? O4 La1 O7 89.43(15) . . ? O1 La1 O12 124.56(16) . . ? O4 La1 O12 83.41(15) . . ? O7 La1 O12 145.61(16) . . ? O1 La1 O16 92.41(16) . . ? O4 La1 O16 144.67(16) . . ? O7 La1 O16 125.00(16) . . ? O12 La1 O16 72.13(16) . . ? O1 La1 O15 147.36(16) . . ? O4 La1 O15 127.56(15) . . ? O7 La1 O15 78.37(15) . . ? O12 La1 O15 79.62(16) . . ? O16 La1 O15 73.31(16) . . ? O1 La1 O18 72.60(16) . . ? O4 La1 O18 150.91(15) . . ? O7 La1 O18 78.10(14) . . ? O12 La1 O18 121.22(15) . . ? O16 La1 O18 49.89(14) . . ? O15 La1 O18 75.90(16) . . ? O1 La1 O13 151.49(15) . . ? O4 La1 O13 77.24(16) . . ? O7 La1 O13 75.12(15) . . ? O12 La1 O13 70.49(16) . . ? O16 La1 O13 116.00(16) . . ? O15 La1 O13 50.33(15) . . ? O18 La1 O13 123.30(17) . . ? O1 La1 O10 74.79(16) . . ? O4 La1 O10 77.08(15) . . ? O7 La1 O10 158.72(15) . . ? O12 La1 O10 49.90(16) . . ? O16 La1 O10 67.69(16) . . ? O15 La1 O10 122.90(16) . . ? O18 La1 O10 105.94(15) . . ? O13 La1 O10 116.78(16) . . ? O1 La1 N6 82.68(17) . . ? O4 La1 N6 159.52(16) . . ? O7 La1 N6 101.52(17) . . ? O12 La1 N6 96.43(18) . . ? O16 La1 N6 24.84(14) . . ? O15 La1 N6 72.12(17) . . ? O18 La1 N6 25.08(15) . . ? O13 La1 N6 122.13(17) . . ? O10 La1 N6 87.12(17) . . ? O1 La1 N4 99.52(18) . . ? O4 La1 N4 80.09(16) . . ? O7 La1 N4 166.55(15) . . ? O12 La1 N4 25.19(15) . . ? O16 La1 N4 66.86(16) . . ? O15 La1 N4 101.31(18) . . ? O18 La1 N4 115.02(15) . . ? O13 La1 N4 94.21(18) . . ? O10 La1 N4 24.75(14) . . ? N6 La1 N4 91.04(18) . . ? O1 La1 N5 161.21(15) . . ? O4 La1 N5 102.59(18) . . ? O7 La1 N5 74.66(15) . . ? O12 La1 N5 74.21(17) . . ? O16 La1 N5 94.98(18) . . ? O15 La1 N5 24.98(15) . . ? O18 La1 N5 99.31(19) . . ? O13 La1 N5 25.36(14) . . ? O10 La1 N5 124.00(17) . . ? N6 La1 N5 97.02(19) . . ? N4 La1 N5 99.27(19) . . ? C6 C1 C2 119.2(8) . . ? C6 C1 H1A 120.4 . . ? C2 C1 H1A 120.4 . . ? C3 C2 C1 123.2(9) . . ? C3 C2 H2A 118.4 . . ? C1 C2 H2A 118.4 . . ? C4 C3 C2 117.3(10) . . ? C4 C3 H3A 121.3 . . ? C2 C3 H3A 121.3 . . ? C3 C4 C5 121.5(9) . . ? C3 C4 H4 119.2 . . ? C5 C4 H4 119.2 . . ? C6 C5 C4 117.6(9) . . ? C6 C5 H5 121.2 . . ? C4 C5 H5 121.2 . . ? C1 C6 C5 121.2(8) . . ? C1 C6 C7 121.2(7) . . ? C5 C6 C7 117.6(8) . . ? N1 C7 C6 111.5(5) . . ? N1 C7 H7A 109.3 . . ? C6 C7 H7A 109.3 . . ? N1 C7 H7B 109.3 . . ? C6 C7 H7B 109.3 . . ? H7A C7 H7B 108.0 . . ? O1 C8 N1 120.1(6) . . ? O1 C8 C9 120.6(6) . . ? N1 C8 C9 119.3(6) . . ? C14 C9 C10 118.4(6) . . ? C14 C9 C8 124.9(6) . . ? C10 C9 C8 116.7(6) . . ? C11 C10 C9 121.6(7) . . ? C11 C10 H10 119.2 . . ? C9 C10 H10 119.2 . . ? C10 C11 C12 118.6(7) . . ? C10 C11 H11 120.7 . . ? C12 C11 H11 120.7 . . ? C11 C12 C13 121.5(7) . . ? C11 C12 H12 119.3 . . ? C13 C12 H12 119.3 . . ? C14 C13 C12 119.5(7) . . ? C14 C13 H13 120.2 . . ? C12 C13 H13 120.2 . . ? O2 C14 C13 123.7(6) . . ? O2 C14 C9 115.9(6) . . ? C13 C14 C9 120.4(6) . . ? O2 C15 C16 104.5(6) . . ? O2 C15 H15A 110.9 . . ? C16 C15 H15A 110.9 . . ? O2 C15 H15B 110.9 . . ? C16 C15 H15B 110.9 . . ? H15A C15 H15B 108.9 . . ? O3 C16 C15 106.8(6) . . ? O3 C16 H16A 110.4 . . ? C15 C16 H16A 110.4 . . ? O3 C16 H16B 110.4 . . ? C15 C16 H16B 110.4 . . ? H16A C16 H16B 108.6 . . ? C23 C18 C19 120.9(8) . . ? C23 C18 H18 119.6 . . ? C19 C18 H18 119.6 . . ? C20 C19 C18 118.5(9) . . ? C20 C19 H19 120.7 . . ? C18 C19 H19 120.7 . . ? C19 C20 C21 120.9(9) . . ? C19 C20 H20 119.6 . . ? C21 C20 H20 119.6 . . ? C22 C21 C20 119.6(9) . . ? C22 C21 H21 120.2 . . ? C20 C21 H21 120.2 . . ? C23 C22 C21 119.8(8) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C22 C23 C18 120.4(8) . . ? C22 C23 C24 120.6(7) . . ? C18 C23 C24 119.0(7) . . ? N2 C24 C23 109.5(5) . . ? N2 C24 H24A 109.8 . . ? C23 C24 H24A 109.8 . . ? N2 C24 H24B 109.8 . . ? C23 C24 H24B 109.8 . . ? H24A C24 H24B 108.2 . . ? O4 C25 N2 121.2(6) . . ? O4 C25 C26 119.6(6) . . ? N2 C25 C26 119.2(6) . . ? C27 C26 C31 117.0(6) . . ? C27 C26 C25 117.8(6) . . ? C31 C26 C25 125.2(6) . . ? C28 C27 C26 123.6(7) . . ? C28 C27 H27 118.2 . . ? C26 C27 H27 118.2 . . ? C27 C28 C29 117.9(7) . . ? C27 C28 H28 121.1 . . ? C29 C28 H28 121.1 . . ? C28 C29 C30 121.8(7) . . ? C28 C29 H29 119.1 . . ? C30 C29 H29 119.1 . . ? C29 C30 C31 119.8(7) . . ? C29 C30 H30 120.1 . . ? C31 C30 H30 120.1 . . ? O5 C31 C30 121.9(6) . . ? O5 C31 C26 118.3(5) . . ? C30 C31 C26 119.9(6) . . ? O5 C32 C33 108.8(6) . . ? O5 C32 H32A 109.9 . . ? C33 C32 H32A 109.9 . . ? O5 C32 H32B 109.9 . . ? C33 C32 H32B 109.9 . . ? H32A C32 H32B 108.3 . . ? O6 C33 C32 110.4(7) . . ? O6 C33 H33A 109.6 . . ? C32 C33 H33A 109.6 . . ? O6 C33 H33B 109.6 . . ? C32 C33 H33B 109.6 . . ? H33A C33 H33B 108.1 . . ? O6 C34 C51 109.6(8) . 1_545 ? O6 C34 H34A 109.7 . . ? C51 C34 H34A 109.7 1_545 . ? O6 C34 H34B 109.7 . . ? C51 C34 H34B 109.7 1_545 . ? H34A C34 H34B 108.2 . . ? C36 C35 C40 120.6(11) . . ? C36 C35 H35 119.7 . . ? C40 C35 H35 119.7 . . ? C37 C36 C35 123.2(15) . . ? C37 C36 H36 118.4 . . ? C35 C36 H36 118.4 . . ? C36 C37 C38 118.2(16) . . ? C36 C37 H37 120.9 . . ? C38 C37 H37 120.9 . . ? C37 C38 C39 120.3(14) . . ? C37 C38 H38 119.8 . . ? C39 C38 H38 119.8 . . ? C40 C39 C38 119.5(11) . . ? C40 C39 H39 120.2 . . ? C38 C39 H39 120.2 . . ? C39 C40 C35 118.0(9) . . ? C39 C40 C41 121.9(9) . . ? C35 C40 C41 120.1(10) . . ? N3 C41 C40 110.3(6) . . ? N3 C41 H41A 109.6 . . ? C40 C41 H41A 109.6 . . ? N3 C41 H41B 109.6 . . ? C40 C41 H41B 109.6 . . ? H41A C41 H41B 108.1 . . ? O7 C42 N3 119.8(6) . . ? O7 C42 C43 121.8(6) . . ? N3 C42 C43 118.4(6) . . ? C44 C43 C48 117.6(6) . . ? C44 C43 C42 116.8(6) . . ? C48 C43 C42 125.5(6) . . ? C45 C44 C43 122.5(7) . . ? C45 C44 H44 118.7 . . ? C43 C44 H44 118.7 . . ? C46 C45 C44 119.2(8) . . ? C46 C45 H45 120.4 . . ? C44 C45 H45 120.4 . . ? C45 C46 C47 120.2(8) . . ? C45 C46 H46 119.9 . . ? C47 C46 H46 119.9 . . ? C46 C47 C48 121.1(7) . . ? C46 C47 H47 119.5 . . ? C48 C47 H47 119.5 . . ? O8 C48 C47 124.1(7) . . ? O8 C48 C43 116.7(7) . . ? C47 C48 C43 119.1(7) . . ? O8 C49 C50 107.3(6) . . ? O8 C49 H49A 110.2 . . ? C50 C49 H49A 110.2 . . ? O8 C49 H49B 110.2 . . ? C50 C49 H49B 110.2 . . ? H49A C49 H49B 108.5 . . ? O9 C50 C49 108.8(6) . . ? O9 C50 H50A 109.9 . . ? C49 C50 H50A 109.9 . . ? O9 C50 H50B 109.9 . . ? C49 C50 H50B 109.9 . . ? H50A C50 H50B 108.3 . . ? O9 C51 C34 108.6(7) . 1_565 ? O9 C51 H51A 110.0 . . ? C34 C51 H51A 110.0 1_565 . ? O9 C51 H51B 110.0 . . ? C34 C51 H51B 110.0 1_565 . ? H51A C51 H51B 108.3 . . ? O3 C52 C52 106.7(8) . 2_666 ? O3 C52 H52A 110.4 . . ? C52 C52 H52A 110.4 2_666 . ? O3 C52 H52B 110.4 . . ? C52 C52 H52B 110.4 2_666 . ? H52A C52 H52B 108.6 . . ? C8 N1 C7 124.6(6) . . ? C8 N1 H1 117.7 . . ? C7 N1 H1 117.7 . . ? C25 N2 C24 126.8(6) . . ? C25 N2 H2 116.6 . . ? C24 N2 H2 116.6 . . ? C42 N3 C41 124.9(6) . . ? C42 N3 H3 117.6 . . ? C41 N3 H3 117.6 . . ? O11 N4 O10 122.7(7) . . ? O11 N4 O12 120.2(7) . . ? O10 N4 O12 117.1(7) . . ? O11 N4 La1 175.8(5) . . ? O10 N4 La1 59.7(4) . . ? O12 N4 La1 57.5(4) . . ? O14 N5 O15 121.9(7) . . ? O14 N5 O13 121.6(7) . . ? O15 N5 O13 116.5(6) . . ? O14 N5 La1 177.8(5) . . ? O15 N5 La1 58.2(3) . . ? O13 N5 La1 58.3(3) . . ? O17 N6 O16 121.7(6) . . ? O17 N6 O18 121.9(7) . . ? O16 N6 O18 116.4(6) . . ? O17 N6 La1 178.0(6) . . ? O16 N6 La1 58.1(3) . . ? O18 N6 La1 58.4(3) . . ? C8 O1 La1 149.0(4) . . ? C14 O2 C15 119.6(5) . . ? C52 O3 C16 113.1(6) . . ? C25 O4 La1 168.8(4) . . ? C31 O5 C32 118.0(5) . . ? C33 O6 C34 110.4(6) . . ? C42 O7 La1 167.9(4) . . ? C48 O8 C49 119.2(6) . . ? C50 O9 C51 111.8(6) . . ? N4 O10 La1 95.6(4) . . ? N4 O12 La1 97.3(4) . . ? N5 O13 La1 96.3(4) . . ? N5 O15 La1 96.8(4) . . ? N6 O16 La1 97.1(4) . . ? N6 O18 La1 96.5(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 C1 C2 C3 0.3(13) . . . . ? C1 C2 C3 C4 -1.3(14) . . . . ? C2 C3 C4 C5 1.8(14) . . . . ? C3 C4 C5 C6 -1.4(13) . . . . ? C2 C1 C6 C5 0.2(11) . . . . ? C2 C1 C6 C7 178.6(7) . . . . ? C4 C5 C6 C1 0.3(11) . . . . ? C4 C5 C6 C7 -178.2(7) . . . . ? C1 C6 C7 N1 29.5(10) . . . . ? C5 C6 C7 N1 -152.0(6) . . . . ? O1 C8 C9 C14 167.8(6) . . . . ? N1 C8 C9 C14 -13.8(10) . . . . ? O1 C8 C9 C10 -11.3(9) . . . . ? N1 C8 C9 C10 167.1(6) . . . . ? C14 C9 C10 C11 0.8(10) . . . . ? C8 C9 C10 C11 179.9(6) . . . . ? C9 C10 C11 C12 -0.7(12) . . . . ? C10 C11 C12 C13 0.0(12) . . . . ? C11 C12 C13 C14 0.7(11) . . . . ? C12 C13 C14 O2 -178.0(6) . . . . ? C12 C13 C14 C9 -0.5(10) . . . . ? C10 C9 C14 O2 177.5(6) . . . . ? C8 C9 C14 O2 -1.6(10) . . . . ? C10 C9 C14 C13 -0.2(10) . . . . ? C8 C9 C14 C13 -179.2(6) . . . . ? O2 C15 C16 O3 57.6(8) . . . . ? C23 C18 C19 C20 0.4(13) . . . . ? C18 C19 C20 C21 -1.0(14) . . . . ? C19 C20 C21 C22 1.0(14) . . . . ? C20 C21 C22 C23 -0.2(12) . . . . ? C21 C22 C23 C18 -0.3(11) . . . . ? C21 C22 C23 C24 -178.4(6) . . . . ? C19 C18 C23 C22 0.3(12) . . . . ? C19 C18 C23 C24 178.3(7) . . . . ? C22 C23 C24 N2 98.6(7) . . . . ? C18 C23 C24 N2 -79.5(8) . . . . ? O4 C25 C26 C27 3.8(9) . . . . ? N2 C25 C26 C27 -176.4(6) . . . . ? O4 C25 C26 C31 -175.2(6) . . . . ? N2 C25 C26 C31 4.6(10) . . . . ? C31 C26 C27 C28 -1.0(10) . . . . ? C25 C26 C27 C28 179.9(6) . . . . ? C26 C27 C28 C29 2.8(11) . . . . ? C27 C28 C29 C30 -1.9(12) . . . . ? C28 C29 C30 C31 -0.8(12) . . . . ? C29 C30 C31 O5 -177.4(6) . . . . ? C29 C30 C31 C26 2.6(11) . . . . ? C27 C26 C31 O5 178.2(6) . . . . ? C25 C26 C31 O5 -2.8(10) . . . . ? C27 C26 C31 C30 -1.7(10) . . . . ? C25 C26 C31 C30 177.3(6) . . . . ? O5 C32 C33 O6 73.5(8) . . . . ? C40 C35 C36 C37 1(2) . . . . ? C35 C36 C37 C38 -4(2) . . . . ? C36 C37 C38 C39 5(2) . . . . ? C37 C38 C39 C40 -2.5(17) . . . . ? C38 C39 C40 C35 -0.7(14) . . . . ? C38 C39 C40 C41 177.6(8) . . . . ? C36 C35 C40 C39 1.6(16) . . . . ? C36 C35 C40 C41 -176.7(10) . . . . ? C39 C40 C41 N3 65.1(11) . . . . ? C35 C40 C41 N3 -116.6(9) . . . . ? O7 C42 C43 C44 10.8(10) . . . . ? N3 C42 C43 C44 -171.2(6) . . . . ? O7 C42 C43 C48 -165.3(7) . . . . ? N3 C42 C43 C48 12.7(10) . . . . ? C48 C43 C44 C45 2.3(12) . . . . ? C42 C43 C44 C45 -174.1(8) . . . . ? C43 C44 C45 C46 1.7(14) . . . . ? C44 C45 C46 C47 -3.6(15) . . . . ? C45 C46 C47 C48 1.5(14) . . . . ? C46 C47 C48 O8 -178.2(7) . . . . ? C46 C47 C48 C43 2.5(12) . . . . ? C44 C43 C48 O8 176.3(6) . . . . ? C42 C43 C48 O8 -7.6(10) . . . . ? C44 C43 C48 C47 -4.3(10) . . . . ? C42 C43 C48 C47 171.8(6) . . . . ? O8 C49 C50 O9 -66.7(8) . . . . ? O1 C8 N1 C7 -4.6(10) . . . . ? C9 C8 N1 C7 177.0(6) . . . . ? C6 C7 N1 C8 -128.1(7) . . . . ? O4 C25 N2 C24 1.0(11) . . . . ? C26 C25 N2 C24 -178.8(6) . . . . ? C23 C24 N2 C25 -142.0(7) . . . . ? O7 C42 N3 C41 2.2(11) . . . . ? C43 C42 N3 C41 -175.8(6) . . . . ? C40 C41 N3 C42 -131.2(8) . . . . ? O1 La1 N4 O11 -128(7) . . . . ? O4 La1 N4 O11 153(7) . . . . ? O7 La1 N4 O11 114(7) . . . . ? O12 La1 N4 O11 58(7) . . . . ? O16 La1 N4 O11 -39(7) . . . . ? O15 La1 N4 O11 27(7) . . . . ? O18 La1 N4 O11 -53(7) . . . . ? O13 La1 N4 O11 77(7) . . . . ? O10 La1 N4 O11 -126(7) . . . . ? N6 La1 N4 O11 -45(7) . . . . ? N5 La1 N4 O11 52(7) . . . . ? O1 La1 N4 O10 -1.9(4) . . . . ? O4 La1 N4 O10 -80.6(4) . . . . ? O7 La1 N4 O10 -119.9(7) . . . . ? O12 La1 N4 O10 -176.2(6) . . . . ? O16 La1 N4 O10 86.6(4) . . . . ? O15 La1 N4 O10 152.8(3) . . . . ? O18 La1 N4 O10 73.2(4) . . . . ? O13 La1 N4 O10 -156.9(4) . . . . ? N6 La1 N4 O10 80.8(4) . . . . ? N5 La1 N4 O10 178.1(4) . . . . ? O1 La1 N4 O12 174.3(3) . . . . ? O4 La1 N4 O12 95.6(4) . . . . ? O7 La1 N4 O12 56.3(9) . . . . ? O16 La1 N4 O12 -97.2(4) . . . . ? O15 La1 N4 O12 -31.0(4) . . . . ? O18 La1 N4 O12 -110.6(4) . . . . ? O13 La1 N4 O12 19.4(4) . . . . ? O10 La1 N4 O12 176.2(6) . . . . ? N6 La1 N4 O12 -103.0(4) . . . . ? N5 La1 N4 O12 -5.7(4) . . . . ? O1 La1 N5 O14 -10(16) . . . . ? O4 La1 N5 O14 88(16) . . . . ? O7 La1 N5 O14 2(16) . . . . ? O12 La1 N5 O14 168(16) . . . . ? O16 La1 N5 O14 -123(16) . . . . ? O15 La1 N5 O14 -93(16) . . . . ? O18 La1 N5 O14 -73(16) . . . . ? O13 La1 N5 O14 90(16) . . . . ? O10 La1 N5 O14 171(16) . . . . ? N6 La1 N5 O14 -98(16) . . . . ? N4 La1 N5 O14 170(16) . . . . ? O1 La1 N5 O15 83.2(7) . . . . ? O4 La1 N5 O15 -178.7(4) . . . . ? O7 La1 N5 O15 95.4(4) . . . . ? O12 La1 N5 O15 -99.4(4) . . . . ? O16 La1 N5 O15 -29.6(4) . . . . ? O18 La1 N5 O15 20.5(4) . . . . ? O13 La1 N5 O15 -177.1(6) . . . . ? O10 La1 N5 O15 -96.0(4) . . . . ? N6 La1 N5 O15 -4.7(4) . . . . ? N4 La1 N5 O15 -96.9(4) . . . . ? O1 La1 N5 O13 -99.7(6) . . . . ? O4 La1 N5 O13 -1.7(4) . . . . ? O7 La1 N5 O13 -87.5(4) . . . . ? O12 La1 N5 O13 77.7(4) . . . . ? O16 La1 N5 O13 147.5(4) . . . . ? O15 La1 N5 O13 177.1(6) . . . . ? O18 La1 N5 O13 -162.4(4) . . . . ? O10 La1 N5 O13 81.1(4) . . . . ? N6 La1 N5 O13 172.4(4) . . . . ? N4 La1 N5 O13 80.2(4) . . . . ? O1 La1 N6 O17 -164(17) . . . . ? O4 La1 N6 O17 161(17) . . . . ? O7 La1 N6 O17 -78(17) . . . . ? O12 La1 N6 O17 72(17) . . . . ? O16 La1 N6 O17 84(17) . . . . ? O15 La1 N6 O17 -5(17) . . . . ? O18 La1 N6 O17 -100(17) . . . . ? O13 La1 N6 O17 1(17) . . . . ? O10 La1 N6 O17 121(17) . . . . ? N4 La1 N6 O17 97(17) . . . . ? N5 La1 N6 O17 -3(17) . . . . ? O1 La1 N6 O16 112.2(4) . . . . ? O4 La1 N6 O16 76.5(7) . . . . ? O7 La1 N6 O16 -162.4(4) . . . . ? O12 La1 N6 O16 -11.9(4) . . . . ? O15 La1 N6 O16 -88.8(4) . . . . ? O18 La1 N6 O16 176.3(7) . . . . ? O13 La1 N6 O16 -82.9(4) . . . . ? O10 La1 N6 O16 37.2(4) . . . . ? N4 La1 N6 O16 12.8(4) . . . . ? N5 La1 N6 O16 -86.7(4) . . . . ? O1 La1 N6 O18 -64.1(4) . . . . ? O4 La1 N6 O18 -99.9(6) . . . . ? O7 La1 N6 O18 21.3(4) . . . . ? O12 La1 N6 O18 171.8(4) . . . . ? O16 La1 N6 O18 -176.3(7) . . . . ? O15 La1 N6 O18 94.9(4) . . . . ? O13 La1 N6 O18 100.8(4) . . . . ? O10 La1 N6 O18 -139.1(4) . . . . ? N4 La1 N6 O18 -163.6(4) . . . . ? N5 La1 N6 O18 97.0(4) . . . . ? N1 C8 O1 La1 95.5(9) . . . . ? C9 C8 O1 La1 -86.1(9) . . . . ? O4 La1 O1 C8 -145.7(8) . . . . ? O7 La1 O1 C8 -55.8(8) . . . . ? O12 La1 O1 C8 139.1(8) . . . . ? O16 La1 O1 C8 69.2(8) . . . . ? O15 La1 O1 C8 7.0(9) . . . . ? O18 La1 O1 C8 22.7(8) . . . . ? O13 La1 O1 C8 -106.2(8) . . . . ? O10 La1 O1 C8 135.3(8) . . . . ? N6 La1 O1 C8 46.3(8) . . . . ? N4 La1 O1 C8 136.1(8) . . . . ? N5 La1 O1 C8 -44.0(11) . . . . ? C13 C14 O2 C15 -11.7(10) . . . . ? C9 C14 O2 C15 170.7(6) . . . . ? C16 C15 O2 C14 -179.4(6) . . . . ? C52 C52 O3 C16 -177.6(7) 2_666 . . . ? C15 C16 O3 C52 -177.9(6) . . . . ? N2 C25 O4 La1 43(3) . . . . ? C26 C25 O4 La1 -137.0(19) . . . . ? O1 La1 O4 C25 -74(2) . . . . ? O7 La1 O4 C25 -161(2) . . . . ? O12 La1 O4 C25 52(2) . . . . ? O16 La1 O4 C25 7(2) . . . . ? O15 La1 O4 C25 124(2) . . . . ? O18 La1 O4 C25 -98(2) . . . . ? O13 La1 O4 C25 124(2) . . . . ? O10 La1 O4 C25 2(2) . . . . ? N6 La1 O4 C25 -38(2) . . . . ? N4 La1 O4 C25 27(2) . . . . ? N5 La1 O4 C25 125(2) . . . . ? C30 C31 O5 C32 11.1(9) . . . . ? C26 C31 O5 C32 -168.9(6) . . . . ? C33 C32 O5 C31 168.0(6) . . . . ? C32 C33 O6 C34 155.5(6) . . . . ? C51 C34 O6 C33 171.5(7) 1_545 . . . ? N3 C42 O7 La1 112(2) . . . . ? C43 C42 O7 La1 -70(2) . . . . ? O1 La1 O7 C42 153(2) . . . . ? O4 La1 O7 C42 -126(2) . . . . ? O12 La1 O7 C42 -49(2) . . . . ? O16 La1 O7 C42 62(2) . . . . ? O15 La1 O7 C42 3(2) . . . . ? O18 La1 O7 C42 80(2) . . . . ? O13 La1 O7 C42 -49(2) . . . . ? O10 La1 O7 C42 -176.2(19) . . . . ? N6 La1 O7 C42 71(2) . . . . ? N4 La1 O7 C42 -87(2) . . . . ? N5 La1 O7 C42 -23(2) . . . . ? C47 C48 O8 C49 5.0(10) . . . . ? C43 C48 O8 C49 -175.6(6) . . . . ? C50 C49 O8 C48 169.8(6) . . . . ? C49 C50 O9 C51 177.5(6) . . . . ? C34 C51 O9 C50 -170.7(7) 1_565 . . . ? O11 N4 O10 La1 176.0(6) . . . . ? O12 N4 O10 La1 -3.6(6) . . . . ? O1 La1 O10 N4 178.0(4) . . . . ? O4 La1 O10 N4 94.4(4) . . . . ? O7 La1 O10 N4 146.3(4) . . . . ? O12 La1 O10 N4 2.1(3) . . . . ? O16 La1 O10 N4 -82.8(4) . . . . ? O15 La1 O10 N4 -32.3(4) . . . . ? O18 La1 O10 N4 -115.5(4) . . . . ? O13 La1 O10 N4 26.0(4) . . . . ? N6 La1 O10 N4 -98.8(4) . . . . ? N5 La1 O10 N4 -2.2(4) . . . . ? O11 N4 O12 La1 -175.9(5) . . . . ? O10 N4 O12 La1 3.7(6) . . . . ? O1 La1 O12 N4 -6.9(4) . . . . ? O4 La1 O12 N4 -80.7(4) . . . . ? O7 La1 O12 N4 -160.0(3) . . . . ? O16 La1 O12 N4 73.5(4) . . . . ? O15 La1 O12 N4 149.1(4) . . . . ? O18 La1 O12 N4 82.7(4) . . . . ? O13 La1 O12 N4 -159.5(4) . . . . ? O10 La1 O12 N4 -2.1(3) . . . . ? N6 La1 O12 N4 78.7(4) . . . . ? N5 La1 O12 N4 174.2(4) . . . . ? O14 N5 O13 La1 -177.5(6) . . . . ? O15 N5 O13 La1 2.8(6) . . . . ? O1 La1 O13 N5 138.3(4) . . . . ? O4 La1 O13 N5 178.3(4) . . . . ? O7 La1 O13 N5 85.5(4) . . . . ? O12 La1 O13 N5 -94.2(4) . . . . ? O16 La1 O13 N5 -36.6(4) . . . . ? O15 La1 O13 N5 -1.6(4) . . . . ? O18 La1 O13 N5 20.9(4) . . . . ? O10 La1 O13 N5 -113.4(4) . . . . ? N6 La1 O13 N5 -8.9(4) . . . . ? N4 La1 O13 N5 -102.8(4) . . . . ? O14 N5 O15 La1 177.5(6) . . . . ? O13 N5 O15 La1 -2.8(6) . . . . ? O1 La1 O15 N5 -143.6(4) . . . . ? O4 La1 O15 N5 1.6(4) . . . . ? O7 La1 O15 N5 -78.6(4) . . . . ? O12 La1 O15 N5 74.8(4) . . . . ? O16 La1 O15 N5 149.1(4) . . . . ? O18 La1 O15 N5 -159.1(4) . . . . ? O13 La1 O15 N5 1.6(4) . . . . ? O10 La1 O15 N5 100.9(4) . . . . ? N6 La1 O15 N5 175.1(4) . . . . ? N4 La1 O15 N5 87.7(4) . . . . ? O17 N6 O16 La1 -177.7(7) . . . . ? O18 N6 O16 La1 3.5(7) . . . . ? O1 La1 O16 N6 -66.8(4) . . . . ? O4 La1 O16 N6 -144.0(4) . . . . ? O7 La1 O16 N6 21.2(5) . . . . ? O12 La1 O16 N6 167.6(5) . . . . ? O15 La1 O16 N6 83.4(4) . . . . ? O18 La1 O16 N6 -2.0(4) . . . . ? O13 La1 O16 N6 110.8(4) . . . . ? O10 La1 O16 N6 -139.2(5) . . . . ? N4 La1 O16 N6 -166.1(5) . . . . ? N5 La1 O16 N6 96.0(4) . . . . ? O17 N6 O18 La1 177.7(7) . . . . ? O16 N6 O18 La1 -3.5(7) . . . . ? O1 La1 O18 N6 110.8(4) . . . . ? O4 La1 O18 N6 134.8(4) . . . . ? O7 La1 O18 N6 -158.7(4) . . . . ? O12 La1 O18 N6 -9.6(5) . . . . ? O16 La1 O18 N6 2.0(4) . . . . ? O15 La1 O18 N6 -77.9(4) . . . . ? O13 La1 O18 N6 -95.6(4) . . . . ? O10 La1 O18 N6 42.8(4) . . . . ? N4 La1 O18 N6 18.2(5) . . . . ? N5 La1 O18 N6 -86.7(4) . . . . ? _diffrn_measured_fraction_theta_max 0.917 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.917 _refine_diff_density_max 0.535 _refine_diff_density_min -0.400 _refine_diff_density_rms 0.089 #===END data_compound8 _database_code_depnum_ccdc_archive 'CCDC 817225' #TrackingRef '- 1-12.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H54 N6 O18 Pr' _chemical_formula_weight 1179.91 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.732(8) _cell_length_b 14.149(10) _cell_length_c 19.594(14) _cell_angle_alpha 81.871(7) _cell_angle_beta 88.384(7) _cell_angle_gamma 66.055(7) _cell_volume 2941(4) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 5524 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 22.26 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.332 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1210 _exptl_absorpt_coefficient_mu 0.899 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8065 _exptl_absorpt_correction_T_max 0.8477 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 21052 _diffrn_reflns_av_R_equivalents 0.0734 _diffrn_reflns_av_sigmaI/netI 0.1301 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 25.50 _reflns_number_total 10784 _reflns_number_gt 6701 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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. Diffuse electron densities resulting from residual disorder solvent moleculeswere removed from the data set using the SQUEEZE routine of PLATON andrefined further using the data generated. ; _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^)+(0.0592P)^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 10784 _refine_ls_number_parameters 673 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1058 _refine_ls_R_factor_gt 0.0644 _refine_ls_wR_factor_ref 0.1471 _refine_ls_wR_factor_gt 0.1355 _refine_ls_goodness_of_fit_ref 0.947 _refine_ls_restrained_S_all 0.947 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.500 0.000 450 72 ' ' _platon_squeeze_details ; ; 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 C35 C 0.3672(5) 0.7364(5) 0.9273(4) 0.099(3) Uani 1 1 d G . . H35 H 0.4364 0.6903 0.9072 0.118 Uiso 1 1 calc R . . C36 C 0.3785(7) 0.7599(7) 0.9926(4) 0.131(4) Uani 1 1 d G . . H36 H 0.4554 0.7294 1.0163 0.158 Uiso 1 1 calc R . . C37 C 0.2750(11) 0.8289(7) 1.0226(3) 0.128(5) Uani 1 1 d G . . H37 H 0.2826 0.8446 1.0663 0.154 Uiso 1 1 calc R . . C38 C 0.1602(9) 0.8744(5) 0.9872(5) 0.133(4) Uani 1 1 d G . . H38 H 0.0909 0.9206 1.0073 0.159 Uiso 1 1 calc R . . C39 C 0.1488(5) 0.8510(5) 0.9219(4) 0.099(3) Uani 1 1 d G . . H39 H 0.0720 0.8814 0.8982 0.119 Uiso 1 1 calc R . . C40 C 0.2523(6) 0.7820(5) 0.8919(3) 0.069(2) Uani 1 1 d G . . Pr1 Pr -0.12134(3) 0.75495(3) 0.738328(18) 0.04207(14) Uani 1 1 d . . . C1 C 0.0944(7) 0.2260(6) 0.7891(4) 0.068(2) Uani 1 1 d . . . H1 H 0.1789 0.2124 0.7874 0.081 Uiso 1 1 calc R . . C2 C 0.0593(9) 0.1436(7) 0.8003(5) 0.093(3) Uani 1 1 d . . . H2 H 0.1191 0.0752 0.8069 0.112 Uiso 1 1 calc R . . C3 C -0.0637(11) 0.1637(8) 0.8016(5) 0.095(3) Uani 1 1 d . . . H3 H -0.0883 0.1083 0.8087 0.113 Uiso 1 1 calc R . . C4 C -0.1524(8) 0.2640(9) 0.7927(4) 0.086(3) Uani 1 1 d . . . H4 H -0.2367 0.2769 0.7940 0.104 Uiso 1 1 calc R . . C5 C -0.1155(7) 0.3466(6) 0.7818(3) 0.0617(19) Uani 1 1 d . . . H5 H -0.1750 0.4152 0.7755 0.074 Uiso 1 1 calc R . . C6 C 0.0094(6) 0.3264(5) 0.7803(3) 0.0473(16) Uani 1 1 d . . . C7 C 0.0490(7) 0.4154(5) 0.7710(3) 0.0595(18) Uani 1 1 d . . . H7A H 0.1182 0.4008 0.7400 0.071 Uiso 1 1 calc R . . H7B H -0.0195 0.4787 0.7506 0.071 Uiso 1 1 calc R . . C8 C 0.0672(5) 0.5204(5) 0.8574(3) 0.0374(14) Uani 1 1 d . . . C9 C 0.1124(5) 0.5207(5) 0.9276(3) 0.0404(14) Uani 1 1 d . . . C10 C 0.0841(6) 0.6160(5) 0.9485(3) 0.0515(17) Uani 1 1 d . . . H10 H 0.0384 0.6761 0.9184 0.062 Uiso 1 1 calc R . . C11 C 0.1208(7) 0.6262(6) 1.0122(4) 0.0619(19) Uani 1 1 d . . . H11 H 0.0982 0.6921 1.0250 0.074 Uiso 1 1 calc R . . C12 C 0.1898(7) 0.5399(6) 1.0558(4) 0.066(2) Uani 1 1 d . . . H12 H 0.2160 0.5465 1.0985 0.080 Uiso 1 1 calc R . . C13 C 0.2216(6) 0.4423(6) 1.0377(3) 0.0594(19) Uani 1 1 d . . . H13 H 0.2702 0.3833 1.0679 0.071 Uiso 1 1 calc R . . C14 C 0.1810(6) 0.4313(5) 0.9739(3) 0.0454(15) Uani 1 1 d . . . C15 C 0.2560(7) 0.2446(5) 1.0075(4) 0.070(2) Uani 1 1 d . . . H15A H 0.2059 0.2575 1.0481 0.084 Uiso 1 1 calc R . . H15B H 0.3410 0.2310 1.0206 0.084 Uiso 1 1 calc R . . C16 C 0.2536(7) 0.1534(6) 0.9806(4) 0.074(2) Uani 1 1 d . . . H16A H 0.2697 0.0967 1.0183 0.089 Uiso 1 1 calc R . . H16B H 0.1713 0.1714 0.9608 0.089 Uiso 1 1 calc R . . C17 C 0.3767(8) 0.0145(6) 0.9237(5) 0.087(3) Uani 1 1 d . . . H17A H 0.3017 0.0032 0.9173 0.105 Uiso 1 1 calc R . . H17B H 0.4191 -0.0286 0.9660 0.105 Uiso 1 1 calc R . . C18 C 0.4298(6) 0.6324(7) 0.6557(4) 0.082(3) Uani 1 1 d . . . H18 H 0.4654 0.5726 0.6878 0.098 Uiso 1 1 calc R . . C19 C 0.4945(8) 0.6991(10) 0.6342(5) 0.102(4) Uani 1 1 d . . . H19 H 0.5718 0.6828 0.6549 0.122 Uiso 1 1 calc R . . C20 C 0.4487(9) 0.7825(9) 0.5863(5) 0.095(3) Uani 1 1 d . . . H20 H 0.4950 0.8214 0.5722 0.114 Uiso 1 1 calc R . . C21 C 0.3339(7) 0.8100(7) 0.5582(5) 0.082(2) Uani 1 1 d . . . H21 H 0.2999 0.8702 0.5262 0.099 Uiso 1 1 calc R . . C22 C 0.2641(6) 0.7494(6) 0.5763(4) 0.064(2) Uani 1 1 d . . . H22 H 0.1867 0.7685 0.5547 0.077 Uiso 1 1 calc R . . C23 C 0.3097(5) 0.6626(6) 0.6254(3) 0.0554(19) Uani 1 1 d . . . C24 C 0.2386(6) 0.5981(6) 0.6478(3) 0.0606(19) Uani 1 1 d . . . H24A H 0.2963 0.5261 0.6613 0.073 Uiso 1 1 calc R . . H24B H 0.1904 0.6229 0.6876 0.073 Uiso 1 1 calc R . . C25 C 0.0349(5) 0.6259(4) 0.5987(3) 0.0400(14) Uani 1 1 d . . . C26 C -0.0439(5) 0.6333(4) 0.5383(3) 0.0380(14) Uani 1 1 d . . . C27 C -0.1624(6) 0.6371(5) 0.5509(3) 0.0551(18) Uani 1 1 d . . . H27 H -0.1890 0.6343 0.5960 0.066 Uiso 1 1 calc R . . C28 C -0.2415(6) 0.6450(6) 0.4979(4) 0.073(2) Uani 1 1 d . . . H28 H -0.3203 0.6464 0.5072 0.088 Uiso 1 1 calc R . . C29 C -0.2047(6) 0.6507(6) 0.4329(4) 0.067(2) Uani 1 1 d . . . H29 H -0.2586 0.6563 0.3972 0.080 Uiso 1 1 calc R . . C30 C -0.0893(6) 0.6483(5) 0.4180(3) 0.0569(18) Uani 1 1 d . . . H30 H -0.0648 0.6525 0.3725 0.068 Uiso 1 1 calc R . . C31 C -0.0091(5) 0.6394(5) 0.4713(3) 0.0457(15) Uani 1 1 d . . . C32 C 0.1598(6) 0.6321(7) 0.3944(3) 0.072(2) Uani 1 1 d . . . H32A H 0.1095 0.6910 0.3609 0.087 Uiso 1 1 calc R . . H32B H 0.1675 0.5680 0.3784 0.087 Uiso 1 1 calc R . . C33 C 0.2853(7) 0.6322(7) 0.4056(4) 0.078(2) Uani 1 1 d . . . H33A H 0.3305 0.6241 0.3631 0.094 Uiso 1 1 calc R . . H33B H 0.2758 0.6981 0.4195 0.094 Uiso 1 1 calc R . . C34 C 0.4691(6) 0.5470(5) 0.4738(4) 0.068(2) Uani 1 1 d . . . H34A H 0.4592 0.6098 0.4924 0.082 Uiso 1 1 calc R . . H34B H 0.5189 0.5423 0.4330 0.082 Uiso 1 1 calc R . . C41 C 0.2429(8) 0.7486(6) 0.8235(4) 0.079(2) Uani 1 1 d . . . H41A H 0.3226 0.6953 0.8134 0.095 Uiso 1 1 calc R . . H41B H 0.1810 0.7193 0.8251 0.095 Uiso 1 1 calc R . . C42 C 0.1148(6) 0.8672(5) 0.7244(3) 0.0440(15) Uani 1 1 d . . . C43 C 0.0958(6) 0.9551(5) 0.6688(3) 0.0432(15) Uani 1 1 d . . . C44 C -0.0102(7) 0.9913(6) 0.6273(4) 0.068(2) Uani 1 1 d . . . H44 H -0.0693 0.9638 0.6383 0.082 Uiso 1 1 calc R . . C45 C -0.0324(8) 1.0648(6) 0.5715(4) 0.091(3) Uani 1 1 d . . . H45 H -0.1064 1.0887 0.5455 0.109 Uiso 1 1 calc R . . C46 C 0.0544(9) 1.1030(6) 0.5541(4) 0.083(3) Uani 1 1 d . . . H46 H 0.0422 1.1508 0.5143 0.099 Uiso 1 1 calc R . . C47 C 0.1593(7) 1.0722(5) 0.5941(4) 0.067(2) Uani 1 1 d . . . H47 H 0.2179 1.0996 0.5815 0.080 Uiso 1 1 calc R . . C48 C 0.1803(6) 1.0008(5) 0.6533(3) 0.0510(17) Uani 1 1 d . . . C49 C 0.3669(6) 1.0179(6) 0.6852(4) 0.072(2) Uani 1 1 d . . . H49A H 0.3218 1.0933 0.6798 0.087 Uiso 1 1 calc R . . H49B H 0.4141 0.9992 0.6441 0.087 Uiso 1 1 calc R . . C50 C 0.4519(6) 0.9800(6) 0.7477(4) 0.076(2) Uani 1 1 d . . . H50A H 0.4879 0.9043 0.7561 0.091 Uiso 1 1 calc R . . H50B H 0.5194 1.0030 0.7406 0.091 Uiso 1 1 calc R . . C51 C 0.4583(7) 0.9819(7) 0.8656(5) 0.087(3) Uani 1 1 d . . . H51A H 0.5214 1.0100 0.8640 0.104 Uiso 1 1 calc R . . H51B H 0.4999 0.9063 0.8708 0.104 Uiso 1 1 calc R . . N1 N 0.0868(5) 0.4302(4) 0.8376(2) 0.0516(14) Uani 1 1 d . . . H1A H 0.1253 0.3749 0.8666 0.062 Uiso 1 1 calc R . . N2 N 0.1548(4) 0.6033(4) 0.5924(2) 0.0503(14) Uani 1 1 d . . . H2A H 0.1860 0.5907 0.5528 0.060 Uiso 1 1 calc R . . N3 N 0.2080(5) 0.8378(5) 0.7700(3) 0.0671(17) Uani 1 1 d . . . H3A H 0.2512 0.8748 0.7677 0.080 Uiso 1 1 calc R . . N4 N -0.2848(6) 0.8782(5) 0.6129(3) 0.0609(15) Uani 1 1 d . . . N5 N -0.3061(5) 0.6632(5) 0.7869(3) 0.0528(14) Uani 1 1 d . . . N6 N -0.1970(5) 0.9295(5) 0.8242(3) 0.0550(15) Uani 1 1 d . . . O1 O 0.0133(4) 0.6048(3) 0.81848(19) 0.0480(10) Uani 1 1 d . . . O2 O 0.2080(4) 0.3342(3) 0.9557(2) 0.0556(12) Uani 1 1 d . . . O3 O 0.3429(5) 0.1203(4) 0.9304(3) 0.0729(14) Uani 1 1 d . . . O4 O -0.0126(4) 0.6389(3) 0.6569(2) 0.0515(11) Uani 1 1 d . . . O5 O 0.1064(4) 0.6401(4) 0.4608(2) 0.0622(13) Uani 1 1 d . . . O6 O 0.3516(4) 0.5499(4) 0.4570(3) 0.0689(13) Uani 1 1 d . . . O7 O 0.0455(4) 0.8172(3) 0.7274(2) 0.0510(11) Uani 1 1 d . . . O8 O 0.2816(4) 0.9676(3) 0.6960(2) 0.0618(12) Uani 1 1 d . . . O9 O 0.3840(4) 1.0198(4) 0.8045(3) 0.0757(15) Uani 1 1 d . . . O10 O -0.1711(4) 0.8634(4) 0.6161(2) 0.0682(14) Uani 1 1 d . . . O11 O -0.3507(6) 0.9281(6) 0.5635(3) 0.123(3) Uani 1 1 d . . . O12 O -0.3231(4) 0.8337(4) 0.6625(2) 0.0597(12) Uani 1 1 d . . . O13 O -0.2316(4) 0.6256(3) 0.7417(2) 0.0526(11) Uani 1 1 d . . . O14 O -0.3838(5) 0.6297(5) 0.8066(3) 0.0878(17) Uani 1 1 d . . . O15 O -0.2980(4) 0.7369(4) 0.8133(2) 0.0561(12) Uani 1 1 d . . . O16 O -0.1293(4) 0.8366(4) 0.8496(2) 0.0589(12) Uani 1 1 d . . . O17 O -0.2262(6) 1.0013(4) 0.8577(3) 0.0948(18) Uani 1 1 d . . . O18 O -0.2349(4) 0.9453(3) 0.7621(3) 0.0603(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 C35 0.088(7) 0.147(9) 0.072(6) 0.010(6) -0.021(5) -0.066(6) C36 0.146(11) 0.199(13) 0.090(8) 0.010(8) -0.024(8) -0.122(10) C37 0.226(15) 0.131(11) 0.082(7) 0.001(8) 0.002(10) -0.133(11) C38 0.189(14) 0.087(8) 0.144(12) -0.032(8) 0.046(10) -0.076(9) C39 0.097(7) 0.101(8) 0.118(9) -0.009(6) 0.000(6) -0.060(6) C40 0.074(5) 0.068(5) 0.075(6) 0.012(4) -0.009(5) -0.047(5) Pr1 0.0412(2) 0.0533(2) 0.0413(2) -0.00411(16) -0.00091(14) -0.02966(17) C1 0.061(5) 0.052(5) 0.100(6) -0.025(4) 0.008(4) -0.030(4) C2 0.098(7) 0.061(6) 0.127(8) -0.025(5) 0.002(6) -0.035(5) C3 0.127(9) 0.093(7) 0.104(7) -0.028(6) 0.016(6) -0.082(7) C4 0.076(6) 0.144(9) 0.067(5) -0.032(6) 0.011(5) -0.069(7) C5 0.064(5) 0.065(5) 0.056(4) -0.018(4) -0.001(4) -0.023(4) C6 0.059(4) 0.053(4) 0.041(4) -0.014(3) -0.001(3) -0.032(4) C7 0.086(5) 0.060(5) 0.043(4) -0.008(3) -0.015(4) -0.039(4) C8 0.039(3) 0.041(4) 0.040(4) -0.005(3) 0.002(3) -0.025(3) C9 0.050(4) 0.048(4) 0.034(3) -0.002(3) 0.000(3) -0.032(3) C10 0.065(4) 0.048(4) 0.052(4) -0.005(3) -0.006(3) -0.034(3) C11 0.089(5) 0.062(5) 0.051(4) -0.017(4) 0.000(4) -0.045(4) C12 0.093(6) 0.080(6) 0.045(4) -0.015(4) -0.009(4) -0.052(5) C13 0.075(5) 0.066(5) 0.036(4) 0.010(3) -0.020(3) -0.032(4) C14 0.058(4) 0.053(4) 0.031(3) -0.002(3) 0.000(3) -0.029(3) C15 0.093(6) 0.055(5) 0.052(4) 0.013(4) -0.008(4) -0.026(4) C16 0.089(6) 0.057(5) 0.079(6) 0.003(4) 0.010(5) -0.036(4) C17 0.088(6) 0.069(6) 0.104(7) -0.012(5) -0.020(5) -0.029(5) C18 0.043(4) 0.124(7) 0.070(5) -0.035(5) -0.010(4) -0.019(5) C19 0.047(5) 0.195(12) 0.096(7) -0.063(7) -0.002(5) -0.070(7) C20 0.074(7) 0.142(10) 0.108(8) -0.061(7) 0.009(6) -0.071(7) C21 0.074(6) 0.084(6) 0.109(7) -0.032(5) 0.008(5) -0.045(5) C22 0.049(4) 0.073(5) 0.080(5) -0.029(5) -0.003(4) -0.028(4) C23 0.031(3) 0.093(6) 0.051(4) -0.034(4) 0.000(3) -0.026(4) C24 0.043(4) 0.089(5) 0.052(4) -0.014(4) -0.006(3) -0.027(4) C25 0.044(4) 0.040(4) 0.044(4) -0.011(3) 0.009(3) -0.024(3) C26 0.039(3) 0.038(3) 0.048(4) -0.008(3) 0.000(3) -0.026(3) C27 0.049(4) 0.075(5) 0.060(4) -0.019(4) 0.008(3) -0.042(4) C28 0.045(4) 0.105(6) 0.089(6) -0.028(5) -0.002(4) -0.045(4) C29 0.054(4) 0.086(6) 0.073(5) -0.027(4) -0.013(4) -0.037(4) C30 0.064(5) 0.069(5) 0.049(4) -0.013(4) -0.004(3) -0.037(4) C31 0.045(4) 0.058(4) 0.046(4) -0.015(3) 0.000(3) -0.030(3) C32 0.063(5) 0.125(7) 0.045(4) -0.019(4) 0.013(4) -0.055(5) C33 0.070(5) 0.120(7) 0.064(5) -0.023(5) 0.029(4) -0.058(5) C34 0.042(4) 0.094(6) 0.089(6) -0.041(4) 0.021(4) -0.040(4) C41 0.106(6) 0.069(5) 0.064(5) 0.017(4) -0.038(5) -0.043(5) C42 0.050(4) 0.048(4) 0.047(4) -0.011(3) 0.006(3) -0.032(3) C43 0.053(4) 0.044(4) 0.043(4) -0.004(3) -0.003(3) -0.031(3) C44 0.067(5) 0.072(5) 0.081(5) 0.008(4) -0.020(4) -0.048(4) C45 0.113(7) 0.081(6) 0.093(6) 0.032(5) -0.050(5) -0.065(6) C46 0.137(8) 0.064(5) 0.063(5) 0.023(4) -0.026(5) -0.065(6) C47 0.092(6) 0.067(5) 0.067(5) 0.001(4) 0.004(4) -0.062(5) C48 0.063(4) 0.050(4) 0.059(4) -0.010(4) 0.008(4) -0.041(4) C49 0.052(4) 0.069(5) 0.115(7) -0.021(5) 0.024(5) -0.044(4) C50 0.045(4) 0.077(6) 0.121(7) -0.033(5) 0.002(5) -0.035(4) C51 0.062(5) 0.075(6) 0.114(7) -0.023(5) -0.007(5) -0.014(4) N1 0.076(4) 0.043(3) 0.039(3) 0.001(3) -0.017(3) -0.030(3) N2 0.040(3) 0.082(4) 0.038(3) -0.020(3) 0.004(2) -0.031(3) N3 0.076(4) 0.080(4) 0.065(4) 0.018(3) -0.030(3) -0.059(4) N4 0.066(4) 0.071(4) 0.051(4) 0.012(3) -0.022(3) -0.038(3) N5 0.044(3) 0.068(4) 0.053(4) 0.017(3) -0.009(3) -0.036(3) N6 0.060(4) 0.055(4) 0.070(4) -0.028(4) 0.024(3) -0.040(3) O1 0.070(3) 0.043(3) 0.035(2) 0.002(2) -0.017(2) -0.028(2) O2 0.075(3) 0.045(3) 0.041(3) 0.000(2) -0.011(2) -0.020(2) O3 0.089(4) 0.050(3) 0.084(4) -0.010(3) 0.010(3) -0.032(3) O4 0.048(2) 0.070(3) 0.045(3) -0.010(2) 0.007(2) -0.032(2) O5 0.047(3) 0.115(4) 0.042(3) -0.018(3) 0.006(2) -0.049(3) O6 0.049(3) 0.091(4) 0.083(4) -0.020(3) 0.010(3) -0.043(3) O7 0.048(2) 0.058(3) 0.061(3) 0.004(2) -0.005(2) -0.041(2) O8 0.051(3) 0.069(3) 0.085(3) -0.004(3) -0.006(2) -0.047(2) O9 0.048(3) 0.076(4) 0.096(4) -0.029(3) -0.002(3) -0.013(3) O10 0.060(3) 0.101(4) 0.060(3) 0.019(3) -0.014(2) -0.058(3) O11 0.097(4) 0.169(6) 0.104(5) 0.070(5) -0.063(4) -0.080(4) O12 0.043(2) 0.087(3) 0.054(3) 0.010(3) -0.006(2) -0.037(2) O13 0.043(2) 0.058(3) 0.068(3) -0.012(2) 0.008(2) -0.030(2) O14 0.071(3) 0.133(5) 0.087(4) 0.011(3) 0.005(3) -0.078(4) O15 0.052(3) 0.069(3) 0.050(3) -0.002(2) 0.008(2) -0.031(2) O16 0.073(3) 0.050(3) 0.060(3) -0.016(2) 0.002(2) -0.028(3) O17 0.125(5) 0.074(4) 0.103(4) -0.046(4) 0.025(4) -0.049(4) O18 0.064(3) 0.055(3) 0.061(3) -0.006(2) -0.009(2) -0.022(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 C35 C36 1.3900 . ? C35 C40 1.3900 . ? C35 H35 0.9300 . ? C36 C37 1.3900 . ? C36 H36 0.9300 . ? C37 C38 1.3900 . ? C37 H37 0.9300 . ? C38 C39 1.3900 . ? C38 H38 0.9300 . ? C39 C40 1.3900 . ? C39 H39 0.9300 . ? C40 C41 1.504(8) . ? Pr1 O4 2.407(4) . ? Pr1 O1 2.438(4) . ? Pr1 O7 2.445(4) . ? Pr1 O12 2.577(4) . ? Pr1 O18 2.580(5) . ? Pr1 O15 2.582(4) . ? Pr1 O16 2.591(4) . ? Pr1 O10 2.597(4) . ? Pr1 O13 2.628(4) . ? Pr1 N6 3.005(6) . ? Pr1 N4 3.017(6) . ? Pr1 N5 3.018(5) . ? C1 C6 1.355(9) . ? C1 C2 1.374(10) . ? C1 H1 0.9300 . ? C2 C3 1.354(12) . ? C2 H2 0.9300 . ? C3 C4 1.367(12) . ? C3 H3 0.9300 . ? C4 C5 1.391(11) . ? C4 H4 0.9300 . ? C5 C6 1.375(9) . ? C5 H5 0.9300 . ? C6 C7 1.496(8) . ? C7 N1 1.460(7) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 O1 1.251(7) . ? C8 N1 1.315(7) . ? C8 C9 1.490(8) . ? C9 C10 1.372(8) . ? C9 C14 1.400(8) . ? C10 C11 1.377(8) . ? C10 H10 0.9300 . ? C11 C12 1.349(9) . ? C11 H11 0.9300 . ? C12 C13 1.373(9) . ? C12 H12 0.9300 . ? C13 C14 1.400(8) . ? C13 H13 0.9300 . ? C14 O2 1.376(7) . ? C15 O2 1.429(7) . ? C15 C16 1.471(9) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 O3 1.401(8) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 O3 1.409(8) . ? C17 C51 1.468(11) 1_545 ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C23 1.417(9) . ? C18 C19 1.446(12) . ? C18 H18 0.9300 . ? C19 C20 1.328(13) . ? C19 H19 0.9300 . ? C20 C21 1.351(11) . ? C20 H20 0.9300 . ? C21 C22 1.414(10) . ? C21 H21 0.9300 . ? C22 C23 1.372(9) . ? C22 H22 0.9300 . ? C23 C24 1.485(9) . ? C24 N2 1.458(7) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 O4 1.259(6) . ? C25 N2 1.316(7) . ? C25 C26 1.488(8) . ? C26 C31 1.366(8) . ? C26 C27 1.386(7) . ? C27 C28 1.375(9) . ? C27 H27 0.9300 . ? C28 C29 1.334(9) . ? C28 H28 0.9300 . ? C29 C30 1.365(9) . ? C29 H29 0.9300 . ? C30 C31 1.384(8) . ? C30 H30 0.9300 . ? C31 O5 1.368(7) . ? C32 O5 1.428(7) . ? C32 C33 1.496(9) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 O6 1.397(9) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 O6 1.409(7) . ? C34 C34 1.491(14) 2_666 ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C41 N3 1.445(8) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 O7 1.272(6) . ? C42 N3 1.321(7) . ? C42 C43 1.480(8) . ? C43 C44 1.375(8) . ? C43 C48 1.393(8) . ? C44 C45 1.349(10) . ? C44 H44 0.9300 . ? C45 C46 1.350(10) . ? C45 H45 0.9300 . ? C46 C47 1.357(10) . ? C46 H46 0.9300 . ? C47 C48 1.382(9) . ? C47 H47 0.9300 . ? C48 O8 1.351(7) . ? C49 O8 1.442(7) . ? C49 C50 1.495(10) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 O9 1.397(8) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C51 O9 1.406(9) . ? C51 C17 1.468(11) 1_565 ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? N1 H1A 0.8600 . ? N2 H2A 0.8600 . ? N3 H3A 0.8600 . ? N4 O11 1.198(6) . ? N4 O12 1.256(6) . ? N4 O10 1.266(6) . ? N5 O14 1.218(6) . ? N5 O13 1.243(6) . ? N5 O15 1.266(7) . ? N6 O17 1.213(6) . ? N6 O16 1.264(7) . ? N6 O18 1.266(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C36 C35 C40 120.0 . . ? C36 C35 H35 120.0 . . ? C40 C35 H35 120.0 . . ? C35 C36 C37 120.0 . . ? C35 C36 H36 120.0 . . ? C37 C36 H36 120.0 . . ? C36 C37 C38 120.0 . . ? C36 C37 H37 120.0 . . ? C38 C37 H37 120.0 . . ? C37 C38 C39 120.0 . . ? C37 C38 H38 120.0 . . ? C39 C38 H38 120.0 . . ? C40 C39 C38 120.0 . . ? C40 C39 H39 120.0 . . ? C38 C39 H39 120.0 . . ? C39 C40 C35 120.0 . . ? C39 C40 C41 121.9(6) . . ? C35 C40 C41 118.0(6) . . ? O4 Pr1 O1 80.76(14) . . ? O4 Pr1 O7 87.06(14) . . ? O1 Pr1 O7 89.05(14) . . ? O4 Pr1 O12 91.63(15) . . ? O1 Pr1 O12 145.22(14) . . ? O7 Pr1 O12 124.64(14) . . ? O4 Pr1 O18 147.21(15) . . ? O1 Pr1 O18 127.17(14) . . ? O7 Pr1 O18 77.77(15) . . ? O12 Pr1 O18 74.22(15) . . ? O4 Pr1 O15 123.80(15) . . ? O1 Pr1 O15 83.85(14) . . ? O7 Pr1 O15 146.36(15) . . ? O12 Pr1 O15 72.33(15) . . ? O18 Pr1 O15 80.57(15) . . ? O4 Pr1 O16 152.25(15) . . ? O1 Pr1 O16 77.76(15) . . ? O7 Pr1 O16 75.29(14) . . ? O12 Pr1 O16 115.99(15) . . ? O18 Pr1 O16 49.43(15) . . ? O15 Pr1 O16 71.07(15) . . ? O4 Pr1 O10 72.37(16) . . ? O1 Pr1 O10 150.80(15) . . ? O7 Pr1 O10 78.54(13) . . ? O12 Pr1 O10 48.94(13) . . ? O18 Pr1 O10 76.18(16) . . ? O15 Pr1 O10 120.57(14) . . ? O16 Pr1 O10 123.11(16) . . ? O4 Pr1 O13 75.15(14) . . ? O1 Pr1 O13 77.31(14) . . ? O7 Pr1 O13 159.00(13) . . ? O12 Pr1 O13 67.94(14) . . ? O18 Pr1 O13 123.21(14) . . ? O15 Pr1 O13 48.74(14) . . ? O16 Pr1 O13 116.34(14) . . ? O10 Pr1 O13 105.83(14) . . ? O4 Pr1 N6 161.23(13) . . ? O1 Pr1 N6 102.45(17) . . ? O7 Pr1 N6 74.59(14) . . ? O12 Pr1 N6 95.54(17) . . ? O18 Pr1 N6 24.73(14) . . ? O15 Pr1 N6 74.95(15) . . ? O16 Pr1 N6 24.72(15) . . ? O10 Pr1 N6 99.58(18) . . ? O13 Pr1 N6 123.62(14) . . ? O4 Pr1 N4 82.33(16) . . ? O1 Pr1 N4 159.53(14) . . ? O7 Pr1 N4 101.52(15) . . ? O12 Pr1 N4 24.34(13) . . ? O18 Pr1 N4 72.68(16) . . ? O15 Pr1 N4 96.15(16) . . ? O16 Pr1 N4 121.70(16) . . ? O10 Pr1 N4 24.64(13) . . ? O13 Pr1 N4 87.28(15) . . ? N6 Pr1 N4 97.27(18) . . ? O4 Pr1 N5 99.32(17) . . ? O1 Pr1 N5 80.33(14) . . ? O7 Pr1 N5 166.50(14) . . ? O12 Pr1 N5 67.41(14) . . ? O18 Pr1 N5 102.01(17) . . ? O15 Pr1 N5 24.58(14) . . ? O16 Pr1 N5 94.19(16) . . ? O10 Pr1 N5 114.68(14) . . ? O13 Pr1 N5 24.18(14) . . ? N6 Pr1 N5 99.45(16) . . ? N4 Pr1 N5 91.16(15) . . ? C6 C1 C2 121.8(7) . . ? C6 C1 H1 119.1 . . ? C2 C1 H1 119.1 . . ? C3 C2 C1 119.0(8) . . ? C3 C2 H2 120.5 . . ? C1 C2 H2 120.5 . . ? C2 C3 C4 121.0(8) . . ? C2 C3 H3 119.5 . . ? C4 C3 H3 119.5 . . ? C3 C4 C5 119.4(8) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? C6 C5 C4 119.7(7) . . ? C6 C5 H5 120.2 . . ? C4 C5 H5 120.2 . . ? C1 C6 C5 119.1(6) . . ? C1 C6 C7 121.2(6) . . ? C5 C6 C7 119.6(6) . . ? N1 C7 C6 109.8(5) . . ? N1 C7 H7A 109.7 . . ? C6 C7 H7A 109.7 . . ? N1 C7 H7B 109.7 . . ? C6 C7 H7B 109.7 . . ? H7A C7 H7B 108.2 . . ? O1 C8 N1 121.6(5) . . ? O1 C8 C9 119.8(5) . . ? N1 C8 C9 118.6(5) . . ? C10 C9 C14 117.7(6) . . ? C10 C9 C8 117.3(5) . . ? C14 C9 C8 125.0(5) . . ? C9 C10 C11 122.6(6) . . ? C9 C10 H10 118.7 . . ? C11 C10 H10 118.7 . . ? C12 C11 C10 119.5(7) . . ? C12 C11 H11 120.3 . . ? C10 C11 H11 120.3 . . ? C11 C12 C13 120.6(6) . . ? C11 C12 H12 119.7 . . ? C13 C12 H12 119.7 . . ? C12 C13 C14 120.2(6) . . ? C12 C13 H13 119.9 . . ? C14 C13 H13 119.9 . . ? O2 C14 C9 119.4(5) . . ? O2 C14 C13 121.2(6) . . ? C9 C14 C13 119.4(6) . . ? O2 C15 C16 109.6(6) . . ? O2 C15 H15A 109.8 . . ? C16 C15 H15A 109.8 . . ? O2 C15 H15B 109.8 . . ? C16 C15 H15B 109.8 . . ? H15A C15 H15B 108.2 . . ? O3 C16 C15 111.3(6) . . ? O3 C16 H16A 109.4 . . ? C15 C16 H16A 109.4 . . ? O3 C16 H16B 109.4 . . ? C15 C16 H16B 109.4 . . ? H16A C16 H16B 108.0 . . ? O3 C17 C51 112.7(7) . 1_545 ? O3 C17 H17A 109.1 . . ? C51 C17 H17A 109.1 1_545 . ? O3 C17 H17B 109.1 . . ? C51 C17 H17B 109.1 1_545 . ? H17A C17 H17B 107.8 . . ? C23 C18 C19 116.9(8) . . ? C23 C18 H18 121.6 . . ? C19 C18 H18 121.6 . . ? C20 C19 C18 123.1(8) . . ? C20 C19 H19 118.5 . . ? C18 C19 H19 118.5 . . ? C19 C20 C21 119.0(9) . . ? C19 C20 H20 120.5 . . ? C21 C20 H20 120.5 . . ? C20 C21 C22 121.6(9) . . ? C20 C21 H21 119.2 . . ? C22 C21 H21 119.2 . . ? C23 C22 C21 120.4(7) . . ? C23 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? C22 C23 C18 118.9(7) . . ? C22 C23 C24 122.6(6) . . ? C18 C23 C24 118.5(7) . . ? N2 C24 C23 110.9(5) . . ? N2 C24 H24A 109.5 . . ? C23 C24 H24A 109.5 . . ? N2 C24 H24B 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 108.0 . . ? O4 C25 N2 119.4(5) . . ? O4 C25 C26 119.8(5) . . ? N2 C25 C26 120.7(5) . . ? C31 C26 C27 117.7(5) . . ? C31 C26 C25 124.6(5) . . ? C27 C26 C25 117.6(5) . . ? C28 C27 C26 121.2(6) . . ? C28 C27 H27 119.4 . . ? C26 C27 H27 119.4 . . ? C29 C28 C27 119.7(6) . . ? C29 C28 H28 120.1 . . ? C27 C28 H28 120.1 . . ? C28 C29 C30 121.2(7) . . ? C28 C29 H29 119.4 . . ? C30 C29 H29 119.4 . . ? C29 C30 C31 119.3(6) . . ? C29 C30 H30 120.4 . . ? C31 C30 H30 120.4 . . ? C26 C31 O5 115.9(5) . . ? C26 C31 C30 121.0(6) . . ? O5 C31 C30 123.1(6) . . ? O5 C32 C33 103.9(5) . . ? O5 C32 H32A 111.0 . . ? C33 C32 H32A 111.0 . . ? O5 C32 H32B 111.0 . . ? C33 C32 H32B 111.0 . . ? H32A C32 H32B 109.0 . . ? O6 C33 C32 109.0(6) . . ? O6 C33 H33A 109.9 . . ? C32 C33 H33A 109.9 . . ? O6 C33 H33B 109.9 . . ? C32 C33 H33B 109.9 . . ? H33A C33 H33B 108.3 . . ? O6 C34 C34 107.0(7) . 2_666 ? O6 C34 H34A 110.3 . . ? C34 C34 H34A 110.3 2_666 . ? O6 C34 H34B 110.3 . . ? C34 C34 H34B 110.3 2_666 . ? H34A C34 H34B 108.6 . . ? N3 C41 C40 109.5(6) . . ? N3 C41 H41A 109.8 . . ? C40 C41 H41A 109.8 . . ? N3 C41 H41B 109.8 . . ? C40 C41 H41B 109.8 . . ? H41A C41 H41B 108.2 . . ? O7 C42 N3 119.7(6) . . ? O7 C42 C43 120.8(6) . . ? N3 C42 C43 119.5(5) . . ? C44 C43 C48 117.5(6) . . ? C44 C43 C42 117.7(6) . . ? C48 C43 C42 124.7(6) . . ? C45 C44 C43 123.0(7) . . ? C45 C44 H44 118.5 . . ? C43 C44 H44 118.5 . . ? C44 C45 C46 118.9(8) . . ? C44 C45 H45 120.5 . . ? C46 C45 H45 120.5 . . ? C45 C46 C47 120.5(7) . . ? C45 C46 H46 119.7 . . ? C47 C46 H46 119.7 . . ? C46 C47 C48 121.1(6) . . ? C46 C47 H47 119.5 . . ? C48 C47 H47 119.5 . . ? O8 C48 C47 124.4(6) . . ? O8 C48 C43 116.9(6) . . ? C47 C48 C43 118.7(6) . . ? O8 C49 C50 106.0(6) . . ? O8 C49 H49A 110.5 . . ? C50 C49 H49A 110.5 . . ? O8 C49 H49B 110.5 . . ? C50 C49 H49B 110.5 . . ? H49A C49 H49B 108.7 . . ? O9 C50 C49 109.1(6) . . ? O9 C50 H50A 109.9 . . ? C49 C50 H50A 109.9 . . ? O9 C50 H50B 109.9 . . ? C49 C50 H50B 109.9 . . ? H50A C50 H50B 108.3 . . ? O9 C51 C17 108.0(6) . 1_565 ? O9 C51 H51A 110.1 . . ? C17 C51 H51A 110.1 1_565 . ? O9 C51 H51B 110.1 . . ? C17 C51 H51B 110.1 1_565 . ? H51A C51 H51B 108.4 . . ? C8 N1 C7 125.9(5) . . ? C8 N1 H1A 117.1 . . ? C7 N1 H1A 117.1 . . ? C25 N2 C24 124.8(5) . . ? C25 N2 H2A 117.6 . . ? C24 N2 H2A 117.6 . . ? C42 N3 C41 125.2(6) . . ? C42 N3 H3A 117.4 . . ? C41 N3 H3A 117.4 . . ? O11 N4 O12 121.9(6) . . ? O11 N4 O10 121.6(6) . . ? O12 N4 O10 116.4(5) . . ? O11 N4 Pr1 179.2(6) . . ? O12 N4 Pr1 57.8(3) . . ? O10 N4 Pr1 58.7(3) . . ? O14 N5 O13 121.7(6) . . ? O14 N5 O15 120.3(6) . . ? O13 N5 O15 118.0(5) . . ? O14 N5 Pr1 177.7(5) . . ? O13 N5 Pr1 60.0(3) . . ? O15 N5 Pr1 58.0(3) . . ? O17 N6 O16 121.9(7) . . ? O17 N6 O18 120.7(7) . . ? O16 N6 O18 117.4(5) . . ? O17 N6 Pr1 178.3(5) . . ? O16 N6 Pr1 59.0(3) . . ? O18 N6 Pr1 58.5(3) . . ? C8 O1 Pr1 168.6(4) . . ? C14 O2 C15 118.9(5) . . ? C16 O3 C17 111.9(6) . . ? C25 O4 Pr1 149.3(4) . . ? C31 O5 C32 120.9(5) . . ? C33 O6 C34 113.1(5) . . ? C42 O7 Pr1 168.1(4) . . ? C48 O8 C49 119.0(5) . . ? C50 O9 C51 111.4(6) . . ? N4 O10 Pr1 96.6(4) . . ? N4 O12 Pr1 97.9(3) . . ? N5 O13 Pr1 95.8(3) . . ? N5 O15 Pr1 97.4(3) . . ? N6 O16 Pr1 96.3(4) . . ? N6 O18 Pr1 96.8(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 C40 C35 C36 C37 0.0 . . . . ? C35 C36 C37 C38 0.0 . . . . ? C36 C37 C38 C39 0.0 . . . . ? C37 C38 C39 C40 0.0 . . . . ? C38 C39 C40 C35 0.0 . . . . ? C38 C39 C40 C41 175.8(5) . . . . ? C36 C35 C40 C39 0.0 . . . . ? C36 C35 C40 C41 -176.0(5) . . . . ? C6 C1 C2 C3 1.0(13) . . . . ? C1 C2 C3 C4 -0.7(14) . . . . ? C2 C3 C4 C5 0.4(14) . . . . ? C3 C4 C5 C6 -0.2(11) . . . . ? C2 C1 C6 C5 -0.9(11) . . . . ? C2 C1 C6 C7 177.5(7) . . . . ? C4 C5 C6 C1 0.5(10) . . . . ? C4 C5 C6 C7 -177.9(6) . . . . ? C1 C6 C7 N1 -78.2(8) . . . . ? C5 C6 C7 N1 100.2(7) . . . . ? O1 C8 C9 C10 4.6(8) . . . . ? N1 C8 C9 C10 -176.2(5) . . . . ? O1 C8 C9 C14 -175.6(5) . . . . ? N1 C8 C9 C14 3.7(8) . . . . ? C14 C9 C10 C11 0.2(9) . . . . ? C8 C9 C10 C11 -180.0(6) . . . . ? C9 C10 C11 C12 1.6(10) . . . . ? C10 C11 C12 C13 -1.2(11) . . . . ? C11 C12 C13 C14 -0.9(11) . . . . ? C10 C9 C14 O2 178.1(5) . . . . ? C8 C9 C14 O2 -1.7(9) . . . . ? C10 C9 C14 C13 -2.3(9) . . . . ? C8 C9 C14 C13 177.8(5) . . . . ? C12 C13 C14 O2 -177.7(6) . . . . ? C12 C13 C14 C9 2.7(10) . . . . ? O2 C15 C16 O3 70.6(8) . . . . ? C23 C18 C19 C20 -3.0(13) . . . . ? C18 C19 C20 C21 3.2(14) . . . . ? C19 C20 C21 C22 -3.0(13) . . . . ? C20 C21 C22 C23 2.7(11) . . . . ? C21 C22 C23 C18 -2.4(10) . . . . ? C21 C22 C23 C24 178.1(6) . . . . ? C19 C18 C23 C22 2.5(10) . . . . ? C19 C18 C23 C24 -178.0(6) . . . . ? C22 C23 C24 N2 28.4(9) . . . . ? C18 C23 C24 N2 -151.0(6) . . . . ? O4 C25 C26 C31 167.6(6) . . . . ? N2 C25 C26 C31 -14.1(9) . . . . ? O4 C25 C26 C27 -10.5(8) . . . . ? N2 C25 C26 C27 167.8(6) . . . . ? C31 C26 C27 C28 1.1(10) . . . . ? C25 C26 C27 C28 179.3(6) . . . . ? C26 C27 C28 C29 -1.0(11) . . . . ? C27 C28 C29 C30 0.3(12) . . . . ? C28 C29 C30 C31 0.3(11) . . . . ? C27 C26 C31 O5 177.2(5) . . . . ? C25 C26 C31 O5 -0.9(9) . . . . ? C27 C26 C31 C30 -0.5(9) . . . . ? C25 C26 C31 C30 -178.6(6) . . . . ? C29 C30 C31 C26 -0.1(10) . . . . ? C29 C30 C31 O5 -177.7(6) . . . . ? O5 C32 C33 O6 57.2(8) . . . . ? C39 C40 C41 N3 65.2(7) . . . . ? C35 C40 C41 N3 -118.9(6) . . . . ? O7 C42 C43 C44 10.1(9) . . . . ? N3 C42 C43 C44 -172.5(6) . . . . ? O7 C42 C43 C48 -166.7(6) . . . . ? N3 C42 C43 C48 10.6(9) . . . . ? C48 C43 C44 C45 2.8(11) . . . . ? C42 C43 C44 C45 -174.2(7) . . . . ? C43 C44 C45 C46 1.9(13) . . . . ? C44 C45 C46 C47 -3.5(14) . . . . ? C45 C46 C47 C48 0.4(13) . . . . ? C46 C47 C48 O8 -179.1(7) . . . . ? C46 C47 C48 C43 4.4(11) . . . . ? C44 C43 C48 O8 177.4(6) . . . . ? C42 C43 C48 O8 -5.8(9) . . . . ? C44 C43 C48 C47 -5.8(9) . . . . ? C42 C43 C48 C47 171.0(6) . . . . ? O8 C49 C50 O9 -68.0(7) . . . . ? O1 C8 N1 C7 -0.8(9) . . . . ? C9 C8 N1 C7 179.9(5) . . . . ? C6 C7 N1 C8 -143.4(6) . . . . ? O4 C25 N2 C24 -4.0(9) . . . . ? C26 C25 N2 C24 177.7(6) . . . . ? C23 C24 N2 C25 -128.5(6) . . . . ? O7 C42 N3 C41 2.5(10) . . . . ? C43 C42 N3 C41 -174.9(6) . . . . ? C40 C41 N3 C42 -128.6(7) . . . . ? O4 Pr1 N4 O11 178(100) . . . . ? O1 Pr1 N4 O11 143(39) . . . . ? O7 Pr1 N4 O11 -97(39) . . . . ? O12 Pr1 N4 O11 66(39) . . . . ? O18 Pr1 N4 O11 -24(39) . . . . ? O15 Pr1 N4 O11 54(39) . . . . ? O16 Pr1 N4 O11 -17(39) . . . . ? O10 Pr1 N4 O11 -118(39) . . . . ? O13 Pr1 N4 O11 102(39) . . . . ? N6 Pr1 N4 O11 -21(39) . . . . ? N5 Pr1 N4 O11 79(39) . . . . ? O4 Pr1 N4 O12 111.6(4) . . . . ? O1 Pr1 N4 O12 77.1(6) . . . . ? O7 Pr1 N4 O12 -163.1(4) . . . . ? O18 Pr1 N4 O12 -89.9(4) . . . . ? O15 Pr1 N4 O12 -11.8(4) . . . . ? O16 Pr1 N4 O12 -83.3(4) . . . . ? O10 Pr1 N4 O12 175.5(6) . . . . ? O13 Pr1 N4 O12 36.2(4) . . . . ? N6 Pr1 N4 O12 -87.4(4) . . . . ? N5 Pr1 N4 O12 12.3(4) . . . . ? O4 Pr1 N4 O10 -63.9(4) . . . . ? O1 Pr1 N4 O10 -98.4(5) . . . . ? O7 Pr1 N4 O10 21.4(4) . . . . ? O12 Pr1 N4 O10 -175.5(6) . . . . ? O18 Pr1 N4 O10 94.6(4) . . . . ? O15 Pr1 N4 O10 172.7(4) . . . . ? O16 Pr1 N4 O10 101.2(4) . . . . ? O13 Pr1 N4 O10 -139.3(4) . . . . ? N6 Pr1 N4 O10 97.1(4) . . . . ? N5 Pr1 N4 O10 -163.2(4) . . . . ? O4 Pr1 N5 O14 -142(11) . . . . ? O1 Pr1 N5 O14 139(11) . . . . ? O7 Pr1 N5 O14 101(11) . . . . ? O12 Pr1 N5 O14 -54(11) . . . . ? O18 Pr1 N5 O14 13(11) . . . . ? O15 Pr1 N5 O14 43(11) . . . . ? O16 Pr1 N5 O14 62(11) . . . . ? O10 Pr1 N5 O14 -67(11) . . . . ? O13 Pr1 N5 O14 -140(12) . . . . ? N6 Pr1 N5 O14 38(11) . . . . ? N4 Pr1 N5 O14 -60(11) . . . . ? O4 Pr1 N5 O13 -1.7(3) . . . . ? O1 Pr1 N5 O13 -80.5(3) . . . . ? O7 Pr1 N5 O13 -119.1(7) . . . . ? O12 Pr1 N5 O13 86.2(3) . . . . ? O18 Pr1 N5 O13 153.3(3) . . . . ? O15 Pr1 N5 O13 -177.0(5) . . . . ? O16 Pr1 N5 O13 -157.4(3) . . . . ? O10 Pr1 N5 O13 73.1(3) . . . . ? N6 Pr1 N5 O13 178.3(3) . . . . ? N4 Pr1 N5 O13 80.7(3) . . . . ? O4 Pr1 N5 O15 175.3(3) . . . . ? O1 Pr1 N5 O15 96.4(3) . . . . ? O7 Pr1 N5 O15 57.8(8) . . . . ? O12 Pr1 N5 O15 -96.9(3) . . . . ? O18 Pr1 N5 O15 -29.8(3) . . . . ? O16 Pr1 N5 O15 19.6(3) . . . . ? O10 Pr1 N5 O15 -109.9(3) . . . . ? O13 Pr1 N5 O15 177.0(5) . . . . ? N6 Pr1 N5 O15 -4.7(4) . . . . ? N4 Pr1 N5 O15 -102.3(3) . . . . ? O4 Pr1 N6 O17 21(20) . . . . ? O1 Pr1 N6 O17 119(20) . . . . ? O7 Pr1 N6 O17 33(20) . . . . ? O12 Pr1 N6 O17 -91(20) . . . . ? O18 Pr1 N6 O17 -61(20) . . . . ? O15 Pr1 N6 O17 -161(20) . . . . ? O16 Pr1 N6 O17 122(20) . . . . ? O10 Pr1 N6 O17 -42(20) . . . . ? O13 Pr1 N6 O17 -158(20) . . . . ? N4 Pr1 N6 O17 -67(20) . . . . ? N5 Pr1 N6 O17 -159(20) . . . . ? O4 Pr1 N6 O16 -100.7(6) . . . . ? O1 Pr1 N6 O16 -2.7(3) . . . . ? O7 Pr1 N6 O16 -88.2(3) . . . . ? O12 Pr1 N6 O16 147.3(3) . . . . ? O18 Pr1 N6 O16 177.6(5) . . . . ? O15 Pr1 N6 O16 77.3(3) . . . . ? O10 Pr1 N6 O16 -163.4(3) . . . . ? O13 Pr1 N6 O16 80.2(4) . . . . ? N4 Pr1 N6 O16 171.8(3) . . . . ? N5 Pr1 N6 O16 79.4(3) . . . . ? O4 Pr1 N6 O18 81.7(6) . . . . ? O1 Pr1 N6 O18 179.7(3) . . . . ? O7 Pr1 N6 O18 94.2(3) . . . . ? O12 Pr1 N6 O18 -30.3(3) . . . . ? O15 Pr1 N6 O18 -100.3(3) . . . . ? O16 Pr1 N6 O18 -177.6(5) . . . . ? O10 Pr1 N6 O18 19.0(3) . . . . ? O13 Pr1 N6 O18 -97.4(3) . . . . ? N4 Pr1 N6 O18 -5.8(3) . . . . ? N5 Pr1 N6 O18 -98.2(3) . . . . ? N1 C8 O1 Pr1 46(2) . . . . ? C9 C8 O1 Pr1 -134.6(17) . . . . ? O4 Pr1 O1 C8 -77.2(19) . . . . ? O7 Pr1 O1 C8 -164.3(19) . . . . ? O12 Pr1 O1 C8 2(2) . . . . ? O18 Pr1 O1 C8 121.8(19) . . . . ? O15 Pr1 O1 C8 48.6(19) . . . . ? O16 Pr1 O1 C8 120.5(19) . . . . ? O10 Pr1 O1 C8 -100.2(19) . . . . ? O13 Pr1 O1 C8 -0.4(19) . . . . ? N6 Pr1 O1 C8 121.7(19) . . . . ? N4 Pr1 O1 C8 -43(2) . . . . ? N5 Pr1 O1 C8 24.0(19) . . . . ? C9 C14 O2 C15 -167.9(6) . . . . ? C13 C14 O2 C15 12.5(9) . . . . ? C16 C15 O2 C14 168.4(6) . . . . ? C15 C16 O3 C17 156.8(6) . . . . ? C51 C17 O3 C16 172.9(7) 1_545 . . . ? N2 C25 O4 Pr1 94.3(8) . . . . ? C26 C25 O4 Pr1 -87.4(8) . . . . ? O1 Pr1 O4 C25 -144.9(7) . . . . ? O7 Pr1 O4 C25 -55.4(7) . . . . ? O12 Pr1 O4 C25 69.2(7) . . . . ? O18 Pr1 O4 C25 6.4(9) . . . . ? O15 Pr1 O4 C25 138.9(7) . . . . ? O16 Pr1 O4 C25 -105.3(8) . . . . ? O10 Pr1 O4 C25 23.5(7) . . . . ? O13 Pr1 O4 C25 135.8(8) . . . . ? N6 Pr1 O4 C25 -43.4(10) . . . . ? N4 Pr1 O4 C25 46.6(7) . . . . ? N5 Pr1 O4 C25 136.6(7) . . . . ? C26 C31 O5 C32 171.5(6) . . . . ? C30 C31 O5 C32 -10.8(10) . . . . ? C33 C32 O5 C31 -178.2(6) . . . . ? C32 C33 O6 C34 -176.9(6) . . . . ? C34 C34 O6 C33 -177.3(7) 2_666 . . . ? N3 C42 O7 Pr1 115.0(18) . . . . ? C43 C42 O7 Pr1 -68(2) . . . . ? O4 Pr1 O7 C42 150.6(19) . . . . ? O1 Pr1 O7 C42 -128.6(19) . . . . ? O12 Pr1 O7 C42 61(2) . . . . ? O18 Pr1 O7 C42 -0.2(19) . . . . ? O15 Pr1 O7 C42 -51(2) . . . . ? O16 Pr1 O7 C42 -51.0(19) . . . . ? O10 Pr1 O7 C42 78.0(19) . . . . ? O13 Pr1 O7 C42 -177.6(18) . . . . ? N6 Pr1 O7 C42 -25.4(19) . . . . ? N4 Pr1 O7 C42 69(2) . . . . ? N5 Pr1 O7 C42 -91(2) . . . . ? C47 C48 O8 C49 8.0(9) . . . . ? C43 C48 O8 C49 -175.4(6) . . . . ? C50 C49 O8 C48 168.7(6) . . . . ? C49 C50 O9 C51 176.8(6) . . . . ? C17 C51 O9 C50 -171.8(6) 1_565 . . . ? O11 N4 O10 Pr1 179.2(6) . . . . ? O12 N4 O10 Pr1 -4.2(6) . . . . ? O4 Pr1 O10 N4 110.9(4) . . . . ? O1 Pr1 O10 N4 134.8(4) . . . . ? O7 Pr1 O10 N4 -158.6(4) . . . . ? O12 Pr1 O10 N4 2.5(3) . . . . ? O18 Pr1 O10 N4 -78.5(4) . . . . ? O15 Pr1 O10 N4 -8.5(4) . . . . ? O16 Pr1 O10 N4 -94.8(4) . . . . ? O13 Pr1 O10 N4 42.6(4) . . . . ? N6 Pr1 O10 N4 -86.6(4) . . . . ? N5 Pr1 O10 N4 18.5(4) . . . . ? O11 N4 O12 Pr1 -179.2(6) . . . . ? O10 N4 O12 Pr1 4.3(6) . . . . ? O4 Pr1 O12 N4 -67.2(4) . . . . ? O1 Pr1 O12 N4 -143.3(4) . . . . ? O7 Pr1 O12 N4 20.3(4) . . . . ? O18 Pr1 O12 N4 82.7(4) . . . . ? O15 Pr1 O12 N4 167.7(4) . . . . ? O16 Pr1 O12 N4 109.9(4) . . . . ? O10 Pr1 O12 N4 -2.5(4) . . . . ? O13 Pr1 O12 N4 -140.5(4) . . . . ? N6 Pr1 O12 N4 95.4(4) . . . . ? N5 Pr1 O12 N4 -166.7(4) . . . . ? O14 N5 O13 Pr1 178.3(5) . . . . ? O15 N5 O13 Pr1 -2.9(5) . . . . ? O4 Pr1 O13 N5 178.3(3) . . . . ? O1 Pr1 O13 N5 94.6(3) . . . . ? O7 Pr1 O13 N5 145.3(4) . . . . ? O12 Pr1 O13 N5 -83.7(3) . . . . ? O18 Pr1 O13 N5 -31.7(4) . . . . ? O15 Pr1 O13 N5 1.7(3) . . . . ? O16 Pr1 O13 N5 25.4(4) . . . . ? O10 Pr1 O13 N5 -115.3(3) . . . . ? N6 Pr1 O13 N5 -2.0(4) . . . . ? N4 Pr1 O13 N5 -98.9(3) . . . . ? O14 N5 O15 Pr1 -178.2(5) . . . . ? O13 N5 O15 Pr1 3.0(5) . . . . ? O4 Pr1 O15 N5 -5.6(4) . . . . ? O1 Pr1 O15 N5 -80.2(3) . . . . ? O7 Pr1 O15 N5 -159.1(3) . . . . ? O12 Pr1 O15 N5 74.2(3) . . . . ? O18 Pr1 O15 N5 150.5(3) . . . . ? O16 Pr1 O15 N5 -159.3(4) . . . . ? O10 Pr1 O15 N5 82.8(4) . . . . ? O13 Pr1 O15 N5 -1.7(3) . . . . ? N6 Pr1 O15 N5 175.2(4) . . . . ? N4 Pr1 O15 N5 79.3(3) . . . . ? O17 N6 O16 Pr1 -178.3(5) . . . . ? O18 N6 O16 Pr1 2.3(5) . . . . ? O4 Pr1 O16 N6 137.2(4) . . . . ? O1 Pr1 O16 N6 177.3(3) . . . . ? O7 Pr1 O16 N6 85.0(3) . . . . ? O12 Pr1 O16 N6 -36.7(4) . . . . ? O18 Pr1 O16 N6 -1.3(3) . . . . ? O15 Pr1 O16 N6 -95.1(3) . . . . ? O10 Pr1 O16 N6 19.6(4) . . . . ? O13 Pr1 O16 N6 -113.7(3) . . . . ? N4 Pr1 O16 N6 -9.6(4) . . . . ? N5 Pr1 O16 N6 -103.6(3) . . . . ? O17 N6 O18 Pr1 178.3(5) . . . . ? O16 N6 O18 Pr1 -2.3(5) . . . . ? O4 Pr1 O18 N6 -144.0(3) . . . . ? O1 Pr1 O18 N6 -0.4(4) . . . . ? O7 Pr1 O18 N6 -79.7(3) . . . . ? O12 Pr1 O18 N6 148.6(4) . . . . ? O15 Pr1 O18 N6 74.4(3) . . . . ? O16 Pr1 O18 N6 1.3(3) . . . . ? O10 Pr1 O18 N6 -160.7(3) . . . . ? O13 Pr1 O18 N6 99.2(3) . . . . ? N4 Pr1 O18 N6 173.9(4) . . . . ? N5 Pr1 O18 N6 86.5(3) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.450 _refine_diff_density_min -1.365 _refine_diff_density_rms 0.107 #===END data_compound9 _database_code_depnum_ccdc_archive 'CCDC 817226' #TrackingRef '- 1-12.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H54 N6 Nd O18' _chemical_formula_weight 1183.25 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' Nd Nd -0.1943 3.0179 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.7509(8) _cell_length_b 14.0863(9) _cell_length_c 19.5636(14) _cell_angle_alpha 81.903(3) _cell_angle_beta 88.260(3) _cell_angle_gamma 66.215(3) _cell_volume 2932.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6238 _cell_measurement_theta_min 2.46 _cell_measurement_theta_max 25.03 _exptl_crystal_description block _exptl_crystal_colour light-purple _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.340 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1308 _exptl_absorpt_coefficient_mu 0.964 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8144 _exptl_absorpt_correction_T_max 0.8521 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 15991 _diffrn_reflns_av_R_equivalents 0.0212 _diffrn_reflns_av_sigmaI/netI 0.0430 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 25.50 _reflns_number_total 10800 _reflns_number_gt 9255 _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. Diffuse electron densities resulting from residual disorder solvent moleculeswere removed from the data set using the SQUEEZE routine of PLATON andrefined further using the data generated. ; # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.500 0.500 0.000 448.0 74.1 _platon_squeeze_details ; ; _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^)+(0.0150P)^2^+1.1205P] 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 10800 _refine_ls_number_parameters 685 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0392 _refine_ls_R_factor_gt 0.0315 _refine_ls_wR_factor_ref 0.0643 _refine_ls_wR_factor_gt 0.0620 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _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 Nd1 Nd -0.120598(13) 0.753399(11) 0.738842(7) 0.03935(5) Uani 1 1 d . . . C1 C -0.1136(3) 0.3460(3) 0.78120(16) 0.0646(9) Uani 1 1 d . . . H1 H -0.1730 0.4146 0.7748 0.077 Uiso 1 1 calc R . . C2 C -0.1504(4) 0.2645(4) 0.7919(2) 0.0870(12) Uani 1 1 d . . . H2 H -0.2347 0.2781 0.7925 0.104 Uiso 1 1 calc R . . C3 C -0.0638(5) 0.1631(4) 0.8019(2) 0.0961(14) Uani 1 1 d . . . H3 H -0.0892 0.1081 0.8097 0.115 Uiso 1 1 calc R . . C4 C 0.0599(4) 0.1431(3) 0.8004(2) 0.0925(13) Uani 1 1 d . . . H4 H 0.1190 0.0743 0.8070 0.111 Uiso 1 1 calc R . . C5 C 0.0968(3) 0.2247(2) 0.78908(18) 0.0684(9) Uani 1 1 d . . . H5 H 0.1811 0.2108 0.7876 0.082 Uiso 1 1 calc R . . C6 C 0.0107(3) 0.3267(2) 0.77990(14) 0.0502(7) Uani 1 1 d . . . C7 C 0.0516(3) 0.4153(2) 0.77009(15) 0.0577(8) Uani 1 1 d . . . H7A H 0.1216 0.3995 0.7396 0.069 Uiso 1 1 calc R . . H7B H -0.0157 0.4787 0.7489 0.069 Uiso 1 1 calc R . . C8 C 0.0673(2) 0.5215(2) 0.85697(13) 0.0416(6) Uani 1 1 d . . . C9 C 0.1106(2) 0.5225(2) 0.92765(13) 0.0399(6) Uani 1 1 d . . . C10 C 0.0802(3) 0.6192(2) 0.94898(15) 0.0552(8) Uani 1 1 d . . . H10 H 0.0328 0.6794 0.9194 0.066 Uiso 1 1 calc R . . C11 C 0.1179(3) 0.6295(3) 1.01270(17) 0.0666(9) Uani 1 1 d . . . H11 H 0.0943 0.6954 1.0262 0.080 Uiso 1 1 calc R . . C12 C 0.1898(3) 0.5420(3) 1.05534(16) 0.0694(9) Uani 1 1 d . . . H12 H 0.2178 0.5482 1.0978 0.083 Uiso 1 1 calc R . . C13 C 0.2216(3) 0.4446(3) 1.03660(15) 0.0623(8) Uani 1 1 d . . . H13 H 0.2708 0.3855 1.0665 0.075 Uiso 1 1 calc R . . C14 C 0.1815(3) 0.4331(2) 0.97362(14) 0.0478(7) Uani 1 1 d . . . C15 C 0.2600(3) 0.2465(2) 1.00684(16) 0.0684(9) Uani 1 1 d . . . H15A H 0.2119 0.2596 1.0483 0.082 Uiso 1 1 calc R . . H15B H 0.3452 0.2332 1.0184 0.082 Uiso 1 1 calc R . . C16 C 0.2558(4) 0.1545(3) 0.98082(19) 0.0779(10) Uani 1 1 d . . . H16A H 0.2715 0.0982 1.0188 0.094 Uiso 1 1 calc R . . H16B H 0.1736 0.1726 0.9613 0.094 Uiso 1 1 calc R . . C17 C 0.3776(4) 0.0123(3) 0.9247(2) 0.0898(12) Uani 1 1 d . . . H17A H 0.3025 0.0010 0.9189 0.108 Uiso 1 1 calc R . . H17B H 0.4206 -0.0307 0.9669 0.108 Uiso 1 1 calc R . . C18 C 0.4584(4) -0.0191(3) 0.8654(2) 0.0930(13) Uani 1 1 d . . . H18A H 0.5203 0.0104 0.8636 0.112 Uiso 1 1 calc R . . H18B H 0.5013 -0.0948 0.8707 0.112 Uiso 1 1 calc R . . C19 C 0.4529(3) 0.9764(3) 0.7458(2) 0.0796(11) Uani 1 1 d . . . H19A H 0.4874 0.9004 0.7538 0.096 Uiso 1 1 calc R . . H19B H 0.5209 0.9986 0.7382 0.096 Uiso 1 1 calc R . . C20 C 0.3674(3) 1.0155(3) 0.6846(2) 0.0742(10) Uani 1 1 d . . . H20A H 0.3236 1.0911 0.6799 0.089 Uiso 1 1 calc R . . H20B H 0.4132 0.9971 0.6429 0.089 Uiso 1 1 calc R . . C21 C 0.1795(3) 0.9988(2) 0.65296(16) 0.0531(7) Uani 1 1 d . . . C22 C 0.1597(4) 1.0722(2) 0.59394(18) 0.0698(9) Uani 1 1 d . . . H22 H 0.2183 1.1000 0.5818 0.084 Uiso 1 1 calc R . . C23 C 0.0550(4) 1.1030(3) 0.5543(2) 0.0888(12) Uani 1 1 d . . . H23 H 0.0437 1.1505 0.5143 0.107 Uiso 1 1 calc R . . C24 C -0.0349(4) 1.0656(3) 0.5720(2) 0.1002(14) Uani 1 1 d . . . H24 H -0.1089 1.0907 0.5462 0.120 Uiso 1 1 calc R . . C25 C -0.0130(3) 0.9902(2) 0.62853(18) 0.0733(10) Uani 1 1 d . . . H25 H -0.0724 0.9629 0.6397 0.088 Uiso 1 1 calc R . . C26 C 0.0930(3) 0.9537(2) 0.66923(14) 0.0462(7) Uani 1 1 d . . . C27 C 0.1112(3) 0.8649(2) 0.72458(15) 0.0457(7) Uani 1 1 d . . . C28 C 0.2365(4) 0.7480(3) 0.82539(18) 0.0798(11) Uani 1 1 d . . . H28A H 0.3141 0.6929 0.8147 0.096 Uiso 1 1 calc R . . H28B H 0.1726 0.7206 0.8281 0.096 Uiso 1 1 calc R . . C29 C 0.2510(4) 0.7788(3) 0.89422(19) 0.0715(10) Uani 1 1 d . . . C30 C 0.1538(4) 0.8498(3) 0.9238(3) 0.0968(13) Uani 1 1 d . . . H30 H 0.0770 0.8831 0.9006 0.116 Uiso 1 1 calc R . . C31 C 0.1691(6) 0.8732(4) 0.9899(3) 0.1221(18) Uani 1 1 d . . . H31 H 0.1030 0.9214 1.0107 0.146 Uiso 1 1 calc R . . C32 C 0.2805(8) 0.8245(6) 1.0217(3) 0.130(2) Uani 1 1 d . . . H32 H 0.2901 0.8380 1.0659 0.156 Uiso 1 1 calc R . . C33 C 0.3787(6) 0.7574(5) 0.9929(3) 0.135(2) Uani 1 1 d . . . H33 H 0.4560 0.7267 1.0156 0.161 Uiso 1 1 calc R . . C34 C 0.3631(4) 0.7344(4) 0.9287(2) 0.1031(14) Uani 1 1 d . . . H34 H 0.4310 0.6873 0.9083 0.124 Uiso 1 1 calc R . . C35 C 0.2663(3) 0.7501(3) 0.57726(19) 0.0662(9) Uani 1 1 d . . . H35 H 0.1878 0.7707 0.5571 0.079 Uiso 1 1 calc R . . C36 C 0.3364(3) 0.8076(3) 0.5578(2) 0.0818(11) Uani 1 1 d . . . H36 H 0.3048 0.8659 0.5240 0.098 Uiso 1 1 calc R . . C37 C 0.4515(4) 0.7804(4) 0.5873(3) 0.0957(14) Uani 1 1 d . . . H37 H 0.4977 0.8199 0.5741 0.115 Uiso 1 1 calc R . . C38 C 0.4968(4) 0.6944(5) 0.6363(2) 0.0999(15) Uani 1 1 d . . . H38 H 0.5746 0.6753 0.6569 0.120 Uiso 1 1 calc R . . C39 C 0.4285(3) 0.6347(3) 0.65614(19) 0.0832(12) Uani 1 1 d . . . H39 H 0.4611 0.5759 0.6895 0.100 Uiso 1 1 calc R . . C40 C 0.3119(3) 0.6628(3) 0.62612(16) 0.0583(8) Uani 1 1 d . . . C41 C 0.2387(3) 0.5980(3) 0.64869(16) 0.0638(9) Uani 1 1 d . . . H41A H 0.2958 0.5258 0.6623 0.077 Uiso 1 1 calc R . . H41B H 0.1911 0.6231 0.6887 0.077 Uiso 1 1 calc R . . C42 C 0.0348(3) 0.6260(2) 0.60122(14) 0.0425(6) Uani 1 1 d . . . C43 C -0.0439(2) 0.6339(2) 0.54079(14) 0.0419(6) Uani 1 1 d . . . C44 C -0.1619(3) 0.6372(2) 0.55320(17) 0.0588(8) Uani 1 1 d . . . H44 H -0.1884 0.6343 0.5984 0.071 Uiso 1 1 calc R . . C45 C -0.2411(3) 0.6448(3) 0.5004(2) 0.0712(10) Uani 1 1 d . . . H45 H -0.3197 0.6461 0.5101 0.085 Uiso 1 1 calc R . . C46 C -0.2036(3) 0.6503(3) 0.43379(19) 0.0683(9) Uani 1 1 d . . . H46 H -0.2571 0.6558 0.3979 0.082 Uiso 1 1 calc R . . C47 C -0.0879(3) 0.6478(2) 0.41949(16) 0.0595(8) Uani 1 1 d . . . H47 H -0.0631 0.6519 0.3740 0.071 Uiso 1 1 calc R . . C48 C -0.0075(3) 0.6392(2) 0.47256(15) 0.0479(7) Uani 1 1 d . . . C49 C 0.1593(3) 0.6320(3) 0.39503(16) 0.0722(10) Uani 1 1 d . . . H49A H 0.1091 0.6911 0.3617 0.087 Uiso 1 1 calc R . . H49B H 0.1664 0.5677 0.3791 0.087 Uiso 1 1 calc R . . C50 C 0.2863(3) 0.6320(3) 0.40554(19) 0.0790(11) Uani 1 1 d . . . H50A H 0.3312 0.6231 0.3628 0.095 Uiso 1 1 calc R . . H50B H 0.2776 0.6982 0.4191 0.095 Uiso 1 1 calc R . . C51 C 0.4700(3) 0.5465(3) 0.47319(18) 0.0719(10) Uani 1 1 d . . . H51A H 0.4611 0.6101 0.4907 0.086 Uiso 1 1 calc R . . H51B H 0.5199 0.5399 0.4323 0.086 Uiso 1 1 calc R . . N1 N 0.0877(2) 0.43152(17) 0.83688(12) 0.0522(6) Uani 1 1 d . . . H1A H 0.1263 0.3763 0.8659 0.063 Uiso 1 1 calc R . . N2 N 0.2030(2) 0.8367(2) 0.77036(13) 0.0673(8) Uani 1 1 d . . . H2A H 0.2466 0.8735 0.7675 0.081 Uiso 1 1 calc R . . N3 N 0.1545(2) 0.60276(19) 0.59417(12) 0.0520(6) Uani 1 1 d . . . H3A H 0.1851 0.5894 0.5544 0.062 Uiso 1 1 calc R . . N4 N -0.1954(2) 0.9273(2) 0.82285(15) 0.0577(7) Uani 1 1 d . . . N5 N -0.3016(2) 0.6627(2) 0.78821(14) 0.0570(7) Uani 1 1 d . . . N6 N -0.2818(3) 0.8743(2) 0.61540(14) 0.0629(7) Uani 1 1 d . . . O1 O 0.01171(18) 0.60648(14) 0.81836(9) 0.0516(5) Uani 1 1 d . . . O2 O 0.20960(19) 0.33656(14) 0.95457(10) 0.0585(5) Uani 1 1 d . . . O3 O 0.3453(2) 0.12020(17) 0.93011(13) 0.0770(7) Uani 1 1 d . . . O4 O 0.3852(2) 0.01727(19) 0.80397(14) 0.0812(7) Uani 1 1 d . . . O5 O 0.2808(2) 0.96627(16) 0.69565(12) 0.0666(6) Uani 1 1 d . . . O6 O 0.04149(17) 0.81644(14) 0.72682(10) 0.0528(5) Uani 1 1 d . . . O7 O -0.01240(18) 0.63899(15) 0.65928(10) 0.0542(5) Uani 1 1 d . . . O8 O 0.10660(19) 0.64019(18) 0.46186(10) 0.0644(6) Uani 1 1 d . . . O9 O 0.3517(2) 0.54961(19) 0.45715(13) 0.0743(6) Uani 1 1 d . . . O10 O -0.1253(2) 0.83420(16) 0.84823(10) 0.0612(5) Uani 1 1 d . . . O11 O -0.2234(3) 0.99866(19) 0.85674(14) 0.0925(8) Uani 1 1 d . . . O12 O -0.23389(19) 0.94077(15) 0.76115(12) 0.0632(6) Uani 1 1 d . . . O13 O -0.29141(19) 0.73648(17) 0.81445(10) 0.0601(5) Uani 1 1 d . . . O14 O -0.3797(2) 0.6292(2) 0.80688(13) 0.0890(8) Uani 1 1 d . . . O15 O -0.22566(18) 0.62475(15) 0.74191(11) 0.0567(5) Uani 1 1 d . . . O16 O -0.31958(18) 0.82932(17) 0.66544(11) 0.0610(6) Uani 1 1 d . . . O17 O -0.3492(3) 0.9267(2) 0.56686(14) 0.1127(11) Uani 1 1 d . . . O18 O -0.1688(2) 0.86034(17) 0.61922(11) 0.0665(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 Nd1 0.04084(9) 0.04486(9) 0.03348(8) -0.00228(6) 0.00090(6) -0.01947(7) C1 0.064(2) 0.077(2) 0.051(2) -0.0165(17) -0.0021(16) -0.0235(19) C2 0.077(3) 0.128(4) 0.074(3) -0.027(3) 0.015(2) -0.057(3) C3 0.129(4) 0.102(3) 0.095(3) -0.025(3) 0.020(3) -0.083(3) C4 0.109(3) 0.058(2) 0.116(4) -0.027(2) 0.014(3) -0.035(2) C5 0.066(2) 0.054(2) 0.087(3) -0.0211(18) 0.0064(19) -0.0227(18) C6 0.063(2) 0.0535(18) 0.0358(16) -0.0129(13) -0.0020(14) -0.0235(16) C7 0.080(2) 0.0532(18) 0.0405(17) -0.0073(14) -0.0097(15) -0.0263(17) C8 0.0427(16) 0.0461(16) 0.0368(15) -0.0023(13) 0.0001(12) -0.0195(13) C9 0.0425(15) 0.0467(15) 0.0330(15) -0.0057(12) 0.0011(12) -0.0204(13) C10 0.071(2) 0.0530(18) 0.0453(18) -0.0033(14) -0.0017(15) -0.0293(16) C11 0.093(3) 0.064(2) 0.052(2) -0.0179(17) 0.0012(18) -0.039(2) C12 0.093(3) 0.082(2) 0.0395(19) -0.0105(18) -0.0095(18) -0.041(2) C13 0.077(2) 0.062(2) 0.0385(18) -0.0024(15) -0.0093(16) -0.0191(18) C14 0.0558(18) 0.0527(17) 0.0334(15) -0.0034(13) 0.0005(13) -0.0211(15) C15 0.087(3) 0.0548(19) 0.0466(19) 0.0075(15) -0.0002(17) -0.0154(18) C16 0.097(3) 0.055(2) 0.075(3) 0.0054(18) 0.013(2) -0.029(2) C17 0.101(3) 0.057(2) 0.101(3) -0.008(2) -0.012(3) -0.020(2) C18 0.074(3) 0.079(3) 0.111(4) -0.029(3) -0.014(3) -0.009(2) C19 0.056(2) 0.081(2) 0.116(3) -0.038(2) 0.014(2) -0.0351(19) C20 0.064(2) 0.078(2) 0.100(3) -0.023(2) 0.020(2) -0.0466(19) C21 0.066(2) 0.0478(17) 0.0516(19) -0.0113(14) 0.0076(16) -0.0287(16) C22 0.097(3) 0.060(2) 0.066(2) -0.0046(17) 0.008(2) -0.047(2) C23 0.137(4) 0.064(2) 0.072(3) 0.0175(19) -0.016(3) -0.055(3) C24 0.124(4) 0.076(3) 0.106(3) 0.033(2) -0.056(3) -0.057(3) C25 0.087(3) 0.062(2) 0.079(3) 0.0142(18) -0.024(2) -0.0442(19) C26 0.0524(18) 0.0422(15) 0.0460(17) -0.0028(13) -0.0008(14) -0.0222(14) C27 0.0484(17) 0.0457(16) 0.0468(17) -0.0078(13) 0.0026(14) -0.0225(14) C28 0.098(3) 0.077(2) 0.064(2) 0.0149(19) -0.029(2) -0.040(2) C29 0.078(3) 0.080(2) 0.062(2) 0.0109(19) -0.015(2) -0.042(2) C30 0.104(4) 0.083(3) 0.108(4) -0.001(3) -0.006(3) -0.046(3) C31 0.158(6) 0.092(4) 0.127(5) -0.028(3) 0.032(4) -0.060(4) C32 0.196(7) 0.156(6) 0.082(4) -0.007(4) 0.006(5) -0.118(6) C33 0.132(5) 0.198(7) 0.086(4) 0.008(4) -0.035(3) -0.085(5) C34 0.088(3) 0.159(4) 0.067(3) -0.002(3) -0.011(2) -0.058(3) C35 0.0444(18) 0.072(2) 0.086(3) -0.026(2) -0.0010(18) -0.0227(17) C36 0.074(3) 0.079(2) 0.105(3) -0.038(2) 0.014(2) -0.037(2) C37 0.078(3) 0.131(4) 0.114(4) -0.065(3) 0.020(3) -0.063(3) C38 0.056(2) 0.173(5) 0.093(3) -0.057(3) 0.000(2) -0.056(3) C39 0.052(2) 0.136(4) 0.062(2) -0.034(2) -0.0006(17) -0.032(2) C40 0.0365(16) 0.088(2) 0.0505(19) -0.0329(18) 0.0021(14) -0.0179(17) C41 0.0512(19) 0.089(2) 0.0446(19) -0.0129(17) -0.0024(15) -0.0205(18) C42 0.0488(17) 0.0403(15) 0.0407(16) -0.0087(12) 0.0082(13) -0.0200(13) C43 0.0435(16) 0.0403(15) 0.0462(17) -0.0100(12) 0.0041(13) -0.0203(13) C44 0.0556(19) 0.075(2) 0.059(2) -0.0226(17) 0.0131(16) -0.0360(17) C45 0.053(2) 0.093(3) 0.083(3) -0.026(2) 0.0040(19) -0.0407(19) C46 0.060(2) 0.078(2) 0.073(3) -0.0219(19) -0.0153(18) -0.0291(18) C47 0.064(2) 0.068(2) 0.0481(19) -0.0105(15) -0.0045(16) -0.0265(17) C48 0.0478(17) 0.0526(17) 0.0476(18) -0.0086(14) -0.0002(14) -0.0240(14) C49 0.069(2) 0.112(3) 0.0410(19) -0.0147(19) 0.0124(16) -0.042(2) C50 0.075(3) 0.109(3) 0.060(2) -0.014(2) 0.0244(19) -0.045(2) C51 0.051(2) 0.087(3) 0.090(3) -0.035(2) 0.0255(19) -0.0351(19) N1 0.0743(17) 0.0409(13) 0.0388(14) -0.0025(10) -0.0133(12) -0.0205(12) N2 0.0809(19) 0.0730(18) 0.0612(18) 0.0135(14) -0.0207(15) -0.0505(16) N3 0.0440(14) 0.0774(17) 0.0383(14) -0.0168(12) 0.0032(11) -0.0256(13) N4 0.0637(17) 0.0554(17) 0.0629(19) -0.0170(15) 0.0134(15) -0.0311(15) N5 0.0498(16) 0.0714(18) 0.0489(16) 0.0150(14) -0.0067(13) -0.0307(14) N6 0.0644(18) 0.0698(18) 0.0548(17) 0.0124(14) -0.0187(14) -0.0330(15) O1 0.0670(13) 0.0440(11) 0.0406(11) 0.0001(9) -0.0112(10) -0.0201(10) O2 0.0799(15) 0.0432(11) 0.0399(12) 0.0003(9) -0.0068(10) -0.0132(11) O3 0.0907(18) 0.0534(13) 0.0837(18) -0.0121(12) 0.0145(14) -0.0257(13) O4 0.0558(14) 0.0795(16) 0.098(2) -0.0318(15) 0.0008(14) -0.0102(13) O5 0.0621(14) 0.0681(14) 0.0820(16) -0.0018(12) -0.0013(12) -0.0415(12) O6 0.0534(12) 0.0560(12) 0.0560(13) 0.0009(10) -0.0017(10) -0.0318(10) O7 0.0578(13) 0.0673(13) 0.0405(12) -0.0126(10) 0.0122(10) -0.0274(11) O8 0.0575(13) 0.1089(18) 0.0363(12) -0.0136(11) 0.0074(10) -0.0425(13) O9 0.0568(14) 0.0936(17) 0.0811(17) -0.0187(14) 0.0130(12) -0.0378(13) O10 0.0787(15) 0.0542(13) 0.0486(13) -0.0102(10) 0.0004(11) -0.0235(12) O11 0.126(2) 0.0680(16) 0.092(2) -0.0387(15) 0.0187(17) -0.0403(16) O12 0.0644(14) 0.0536(13) 0.0621(15) -0.0058(11) -0.0067(11) -0.0142(11) O13 0.0615(14) 0.0699(14) 0.0498(13) -0.0065(11) 0.0129(10) -0.0288(12) O14 0.0758(17) 0.133(2) 0.0794(18) 0.0087(16) 0.0077(13) -0.0721(17) O15 0.0529(13) 0.0576(12) 0.0638(14) -0.0085(11) 0.0084(11) -0.0270(10) O16 0.0518(13) 0.0793(14) 0.0528(13) 0.0103(11) -0.0057(10) -0.0333(11) O17 0.097(2) 0.143(2) 0.088(2) 0.0576(19) -0.0496(17) -0.0597(19) O18 0.0617(14) 0.0900(16) 0.0556(14) 0.0147(12) -0.0099(11) -0.0459(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd1 O7 2.3602(19) . ? Nd1 O6 2.3979(18) . ? Nd1 O1 2.4010(18) . ? Nd1 O13 2.5259(19) . ? Nd1 O12 2.527(2) . ? Nd1 O16 2.5352(19) . ? Nd1 O18 2.543(2) . ? Nd1 O10 2.551(2) . ? Nd1 O15 2.5654(19) . ? C1 C2 1.369(5) . ? C1 C6 1.374(4) . ? C1 H1 0.9300 . ? C2 C3 1.369(6) . ? C2 H2 0.9300 . ? C3 C4 1.365(5) . ? C3 H3 0.9300 . ? C4 C5 1.372(5) . ? C4 H4 0.9300 . ? C5 C6 1.373(4) . ? C5 H5 0.9300 . ? C6 C7 1.497(4) . ? C7 N1 1.461(3) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 O1 1.254(3) . ? C8 N1 1.307(3) . ? C8 C9 1.492(3) . ? C9 C10 1.385(4) . ? C9 C14 1.403(4) . ? C10 C11 1.381(4) . ? C10 H10 0.9300 . ? C11 C12 1.358(4) . ? C11 H11 0.9300 . ? C12 C13 1.369(4) . ? C12 H12 0.9300 . ? C13 C14 1.386(4) . ? C13 H13 0.9300 . ? C14 O2 1.367(3) . ? C15 O2 1.439(3) . ? C15 C16 1.477(4) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 O3 1.409(4) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 O3 1.429(4) . ? C17 C18 1.478(5) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 O4 1.408(4) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 O4 1.421(4) 1_565 ? C19 C20 1.479(5) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 O5 1.441(3) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 O5 1.356(3) . ? C21 C22 1.394(4) . ? C21 C26 1.408(4) . ? C22 C23 1.355(5) . ? C22 H22 0.9300 . ? C23 C24 1.374(5) . ? C23 H23 0.9300 . ? C24 C25 1.372(5) . ? C24 H24 0.9300 . ? C25 C26 1.371(4) . ? C25 H25 0.9300 . ? C26 C27 1.483(4) . ? C27 O6 1.257(3) . ? C27 N2 1.318(3) . ? C28 N2 1.457(4) . ? C28 C29 1.506(5) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C30 1.357(5) . ? C29 C34 1.361(5) . ? C30 C31 1.411(7) . ? C30 H30 0.9300 . ? C31 C32 1.333(7) . ? C31 H31 0.9300 . ? C32 C33 1.332(7) . ? C32 H32 0.9300 . ? C33 C34 1.375(6) . ? C33 H33 0.9300 . ? C34 H34 0.9300 . ? C35 C40 1.371(5) . ? C35 C36 1.383(5) . ? C35 H35 0.9300 . ? C36 C37 1.369(5) . ? C36 H36 0.9300 . ? C37 C38 1.363(6) . ? C37 H37 0.9300 . ? C38 C39 1.391(6) . ? C38 H38 0.9300 . ? C39 C40 1.387(4) . ? C39 H39 0.9300 . ? C40 C41 1.505(4) . ? C41 N3 1.453(3) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 O7 1.253(3) . ? C42 N3 1.318(3) . ? C42 C43 1.487(4) . ? C43 C44 1.384(4) . ? C43 C48 1.390(4) . ? C44 C45 1.375(4) . ? C44 H44 0.9300 . ? C45 C46 1.366(5) . ? C45 H45 0.9300 . ? C46 C47 1.368(4) . ? C46 H46 0.9300 . ? C47 C48 1.384(4) . ? C47 H47 0.9300 . ? C48 O8 1.357(3) . ? C49 O8 1.429(3) . ? C49 C50 1.512(4) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 O9 1.398(4) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C51 O9 1.416(4) . ? C51 C51 1.492(7) 2_666 ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? N1 H1A 0.8600 . ? N2 H2A 0.8600 . ? N3 H3A 0.8600 . ? N4 O11 1.211(3) . ? N4 O12 1.264(3) . ? N4 O10 1.270(3) . ? N5 O14 1.217(3) . ? N5 O15 1.267(3) . ? N5 O13 1.270(3) . ? N6 O17 1.204(3) . ? N6 O16 1.258(3) . ? N6 O18 1.265(3) . ? O4 C19 1.421(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 O7 Nd1 O6 86.62(7) . . ? O7 Nd1 O1 80.80(7) . . ? O6 Nd1 O1 89.34(6) . . ? O7 Nd1 O13 125.00(7) . . ? O6 Nd1 O13 145.50(7) . . ? O1 Nd1 O13 83.46(7) . . ? O7 Nd1 O12 147.06(7) . . ? O6 Nd1 O12 78.01(7) . . ? O1 Nd1 O12 127.32(7) . . ? O13 Nd1 O12 79.81(7) . . ? O7 Nd1 O16 92.36(7) . . ? O6 Nd1 O16 124.73(6) . . ? O1 Nd1 O16 144.99(7) . . ? O13 Nd1 O16 72.49(7) . . ? O12 Nd1 O16 73.64(7) . . ? O7 Nd1 O18 72.82(7) . . ? O6 Nd1 O18 77.78(6) . . ? O1 Nd1 O18 151.12(7) . . ? O13 Nd1 O18 121.33(7) . . ? O12 Nd1 O18 75.52(7) . . ? O16 Nd1 O18 49.76(6) . . ? O7 Nd1 O10 151.01(7) . . ? O6 Nd1 O10 74.72(7) . . ? O1 Nd1 O10 77.06(6) . . ? O13 Nd1 O10 70.78(7) . . ? O12 Nd1 O10 50.26(7) . . ? O16 Nd1 O10 116.46(7) . . ? O18 Nd1 O10 122.76(7) . . ? O7 Nd1 O15 74.92(7) . . ? O6 Nd1 O15 158.64(7) . . ? O1 Nd1 O15 77.35(6) . . ? O13 Nd1 O15 50.23(7) . . ? O12 Nd1 O15 123.34(7) . . ? O16 Nd1 O15 67.74(6) . . ? O18 Nd1 O15 106.12(7) . . ? O10 Nd1 O15 117.39(7) . . ? C2 C1 C6 120.3(3) . . ? C2 C1 H1 119.9 . . ? C6 C1 H1 119.9 . . ? C1 C2 C3 120.3(4) . . ? C1 C2 H2 119.8 . . ? C3 C2 H2 119.8 . . ? C4 C3 C2 119.9(4) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C3 C4 C5 119.8(4) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? C4 C5 C6 120.8(3) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? C5 C6 C1 118.9(3) . . ? C5 C6 C7 120.5(3) . . ? C1 C6 C7 120.6(3) . . ? N1 C7 C6 109.7(2) . . ? N1 C7 H7A 109.7 . . ? C6 C7 H7A 109.7 . . ? N1 C7 H7B 109.7 . . ? C6 C7 H7B 109.7 . . ? H7A C7 H7B 108.2 . . ? O1 C8 N1 121.5(2) . . ? O1 C8 C9 119.7(2) . . ? N1 C8 C9 118.8(2) . . ? C10 C9 C14 117.6(2) . . ? C10 C9 C8 117.3(2) . . ? C14 C9 C8 125.1(2) . . ? C11 C10 C9 122.3(3) . . ? C11 C10 H10 118.8 . . ? C9 C10 H10 118.8 . . ? C12 C11 C10 119.0(3) . . ? C12 C11 H11 120.5 . . ? C10 C11 H11 120.5 . . ? C11 C12 C13 120.7(3) . . ? C11 C12 H12 119.6 . . ? C13 C12 H12 119.6 . . ? C12 C13 C14 120.8(3) . . ? C12 C13 H13 119.6 . . ? C14 C13 H13 119.6 . . ? O2 C14 C13 121.8(3) . . ? O2 C14 C9 118.7(2) . . ? C13 C14 C9 119.5(3) . . ? O2 C15 C16 109.4(3) . . ? O2 C15 H15A 109.8 . . ? C16 C15 H15A 109.8 . . ? O2 C15 H15B 109.8 . . ? C16 C15 H15B 109.8 . . ? H15A C15 H15B 108.3 . . ? O3 C16 C15 110.9(3) . . ? O3 C16 H16A 109.5 . . ? C15 C16 H16A 109.5 . . ? O3 C16 H16B 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 108.1 . . ? O3 C17 C18 110.6(3) . . ? O3 C17 H17A 109.5 . . ? C18 C17 H17A 109.5 . . ? O3 C17 H17B 109.5 . . ? C18 C17 H17B 109.5 . . ? H17A C17 H17B 108.1 . . ? O4 C18 C17 109.3(3) . . ? O4 C18 H18A 109.8 . . ? C17 C18 H18A 109.8 . . ? O4 C18 H18B 109.8 . . ? C17 C18 H18B 109.8 . . ? H18A C18 H18B 108.3 . . ? O4 C19 C20 108.6(3) 1_565 . ? O4 C19 H19A 110.0 1_565 . ? C20 C19 H19A 110.0 . . ? O4 C19 H19B 110.0 1_565 . ? C20 C19 H19B 110.0 . . ? H19A C19 H19B 108.3 . . ? O5 C20 C19 106.3(3) . . ? O5 C20 H20A 110.5 . . ? C19 C20 H20A 110.5 . . ? O5 C20 H20B 110.5 . . ? C19 C20 H20B 110.5 . . ? H20A C20 H20B 108.7 . . ? O5 C21 C22 122.9(3) . . ? O5 C21 C26 117.4(3) . . ? C22 C21 C26 119.6(3) . . ? C23 C22 C21 119.9(3) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C22 C23 C24 121.4(3) . . ? C22 C23 H23 119.3 . . ? C24 C23 H23 119.3 . . ? C25 C24 C23 118.6(4) . . ? C25 C24 H24 120.7 . . ? C23 C24 H24 120.7 . . ? C26 C25 C24 122.5(3) . . ? C26 C25 H25 118.8 . . ? C24 C25 H25 118.8 . . ? C25 C26 C21 117.8(3) . . ? C25 C26 C27 117.1(3) . . ? C21 C26 C27 124.9(3) . . ? O6 C27 N2 120.8(3) . . ? O6 C27 C26 120.4(3) . . ? N2 C27 C26 118.8(2) . . ? N2 C28 C29 111.6(3) . . ? N2 C28 H28A 109.3 . . ? C29 C28 H28A 109.3 . . ? N2 C28 H28B 109.3 . . ? C29 C28 H28B 109.3 . . ? H28A C28 H28B 108.0 . . ? C30 C29 C34 118.3(4) . . ? C30 C29 C28 121.6(4) . . ? C34 C29 C28 120.1(4) . . ? C29 C30 C31 120.1(5) . . ? C29 C30 H30 120.0 . . ? C31 C30 H30 120.0 . . ? C32 C31 C30 118.5(6) . . ? C32 C31 H31 120.7 . . ? C30 C31 H31 120.7 . . ? C33 C32 C31 122.7(6) . . ? C33 C32 H32 118.7 . . ? C31 C32 H32 118.7 . . ? C32 C33 C34 118.5(6) . . ? C32 C33 H33 120.7 . . ? C34 C33 H33 120.7 . . ? C29 C34 C33 121.8(5) . . ? C29 C34 H34 119.1 . . ? C33 C34 H34 119.1 . . ? C40 C35 C36 120.4(3) . . ? C40 C35 H35 119.8 . . ? C36 C35 H35 119.8 . . ? C37 C36 C35 121.3(4) . . ? C37 C36 H36 119.3 . . ? C35 C36 H36 119.3 . . ? C38 C37 C36 118.6(4) . . ? C38 C37 H37 120.7 . . ? C36 C37 H37 120.7 . . ? C37 C38 C39 121.1(4) . . ? C37 C38 H38 119.4 . . ? C39 C38 H38 119.4 . . ? C40 C39 C38 119.9(4) . . ? C40 C39 H39 120.0 . . ? C38 C39 H39 120.0 . . ? C35 C40 C39 118.7(3) . . ? C35 C40 C41 122.0(3) . . ? C39 C40 C41 119.3(3) . . ? N3 C41 C40 111.9(3) . . ? N3 C41 H41A 109.2 . . ? C40 C41 H41A 109.2 . . ? N3 C41 H41B 109.2 . . ? C40 C41 H41B 109.2 . . ? H41A C41 H41B 107.9 . . ? O7 C42 N3 120.0(3) . . ? O7 C42 C43 119.9(2) . . ? N3 C42 C43 120.1(2) . . ? C44 C43 C48 117.7(3) . . ? C44 C43 C42 117.8(3) . . ? C48 C43 C42 124.5(2) . . ? C45 C44 C43 121.8(3) . . ? C45 C44 H44 119.1 . . ? C43 C44 H44 119.1 . . ? C46 C45 C44 119.6(3) . . ? C46 C45 H45 120.2 . . ? C44 C45 H45 120.2 . . ? C45 C46 C47 120.3(3) . . ? C45 C46 H46 119.8 . . ? C47 C46 H46 119.8 . . ? C46 C47 C48 120.2(3) . . ? C46 C47 H47 119.9 . . ? C48 C47 H47 119.9 . . ? O8 C48 C47 123.2(3) . . ? O8 C48 C43 116.2(2) . . ? C47 C48 C43 120.5(3) . . ? O8 C49 C50 104.1(3) . . ? O8 C49 H49A 110.9 . . ? C50 C49 H49A 110.9 . . ? O8 C49 H49B 110.9 . . ? C50 C49 H49B 110.9 . . ? H49A C49 H49B 108.9 . . ? O9 C50 C49 108.6(3) . . ? O9 C50 H50A 110.0 . . ? C49 C50 H50A 110.0 . . ? O9 C50 H50B 110.0 . . ? C49 C50 H50B 110.0 . . ? H50A C50 H50B 108.4 . . ? O9 C51 C51 106.7(3) . 2_666 ? O9 C51 H51A 110.4 . . ? C51 C51 H51A 110.4 2_666 . ? O9 C51 H51B 110.4 . . ? C51 C51 H51B 110.4 2_666 . ? H51A C51 H51B 108.6 . . ? C8 N1 C7 126.5(2) . . ? C8 N1 H1A 116.7 . . ? C7 N1 H1A 116.7 . . ? C27 N2 C28 125.2(3) . . ? C27 N2 H2A 117.4 . . ? C28 N2 H2A 117.4 . . ? C42 N3 C41 124.8(2) . . ? C42 N3 H3A 117.6 . . ? C41 N3 H3A 117.6 . . ? O11 N4 O12 122.4(3) . . ? O11 N4 O10 121.0(3) . . ? O12 N4 O10 116.6(2) . . ? O14 N5 O15 121.4(3) . . ? O14 N5 O13 121.8(3) . . ? O15 N5 O13 116.9(2) . . ? O17 N6 O16 121.9(3) . . ? O17 N6 O18 122.4(3) . . ? O16 N6 O18 115.7(2) . . ? C8 O1 Nd1 168.87(18) . . ? C14 O2 C15 117.9(2) . . ? C16 O3 C17 111.1(3) . . ? C18 O4 C19 112.6(3) . 1_545 ? C21 O5 C20 119.8(3) . . ? C27 O6 Nd1 169.00(19) . . ? C42 O7 Nd1 149.27(18) . . ? C48 O8 C49 120.6(2) . . ? C50 O9 C51 112.7(3) . . ? N4 O10 Nd1 95.86(17) . . ? N4 O12 Nd1 97.20(16) . . ? N5 O13 Nd1 97.30(16) . . ? N5 O15 Nd1 95.49(16) . . ? N6 O16 Nd1 97.47(16) . . ? N6 O18 Nd1 96.89(16) . . ? 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 0.4(6) . . . . ? C1 C2 C3 C4 -0.7(6) . . . . ? C2 C3 C4 C5 0.2(7) . . . . ? C3 C4 C5 C6 0.7(6) . . . . ? C4 C5 C6 C1 -1.0(5) . . . . ? C4 C5 C6 C7 177.8(3) . . . . ? C2 C1 C6 C5 0.4(5) . . . . ? C2 C1 C6 C7 -178.3(3) . . . . ? C5 C6 C7 N1 -79.0(4) . . . . ? C1 C6 C7 N1 99.7(3) . . . . ? O1 C8 C9 C10 3.8(4) . . . . ? N1 C8 C9 C10 -175.8(3) . . . . ? O1 C8 C9 C14 -175.0(3) . . . . ? N1 C8 C9 C14 5.4(4) . . . . ? C14 C9 C10 C11 0.4(4) . . . . ? C8 C9 C10 C11 -178.5(3) . . . . ? C9 C10 C11 C12 1.7(5) . . . . ? C10 C11 C12 C13 -2.0(5) . . . . ? C11 C12 C13 C14 0.2(5) . . . . ? C12 C13 C14 O2 -178.4(3) . . . . ? C12 C13 C14 C9 2.0(5) . . . . ? C10 C9 C14 O2 178.1(2) . . . . ? C8 C9 C14 O2 -3.1(4) . . . . ? C10 C9 C14 C13 -2.2(4) . . . . ? C8 C9 C14 C13 176.6(3) . . . . ? O2 C15 C16 O3 72.1(4) . . . . ? O3 C17 C18 O4 -78.0(4) . . . . ? O4 C19 C20 O5 -68.2(3) 1_565 . . . ? O5 C21 C22 C23 -178.6(3) . . . . ? C26 C21 C22 C23 2.8(5) . . . . ? C21 C22 C23 C24 1.8(6) . . . . ? C22 C23 C24 C25 -4.4(7) . . . . ? C23 C24 C25 C26 2.2(6) . . . . ? C24 C25 C26 C21 2.3(5) . . . . ? C24 C25 C26 C27 -174.1(3) . . . . ? O5 C21 C26 C25 176.5(3) . . . . ? C22 C21 C26 C25 -4.8(4) . . . . ? O5 C21 C26 C27 -7.4(4) . . . . ? C22 C21 C26 C27 171.2(3) . . . . ? C25 C26 C27 O6 10.1(4) . . . . ? C21 C26 C27 O6 -165.9(3) . . . . ? C25 C26 C27 N2 -171.1(3) . . . . ? C21 C26 C27 N2 12.8(4) . . . . ? N2 C28 C29 C30 63.3(5) . . . . ? N2 C28 C29 C34 -117.4(4) . . . . ? C34 C29 C30 C31 -2.3(6) . . . . ? C28 C29 C30 C31 176.9(4) . . . . ? C29 C30 C31 C32 0.4(7) . . . . ? C30 C31 C32 C33 2.1(9) . . . . ? C31 C32 C33 C34 -2.5(9) . . . . ? C30 C29 C34 C33 1.9(7) . . . . ? C28 C29 C34 C33 -177.3(4) . . . . ? C32 C33 C34 C29 0.4(8) . . . . ? C40 C35 C36 C37 -1.1(5) . . . . ? C35 C36 C37 C38 0.5(6) . . . . ? C36 C37 C38 C39 0.3(6) . . . . ? C37 C38 C39 C40 -0.4(6) . . . . ? C36 C35 C40 C39 1.0(5) . . . . ? C36 C35 C40 C41 -179.9(3) . . . . ? C38 C39 C40 C35 -0.2(5) . . . . ? C38 C39 C40 C41 -179.3(3) . . . . ? C35 C40 C41 N3 28.8(4) . . . . ? C39 C40 C41 N3 -152.1(3) . . . . ? O7 C42 C43 C44 -11.2(4) . . . . ? N3 C42 C43 C44 167.1(3) . . . . ? O7 C42 C43 C48 168.2(3) . . . . ? N3 C42 C43 C48 -13.4(4) . . . . ? C48 C43 C44 C45 0.4(4) . . . . ? C42 C43 C44 C45 179.9(3) . . . . ? C43 C44 C45 C46 -0.7(5) . . . . ? C44 C45 C46 C47 0.3(5) . . . . ? C45 C46 C47 C48 0.3(5) . . . . ? C46 C47 C48 O8 -177.5(3) . . . . ? C46 C47 C48 C43 -0.6(5) . . . . ? C44 C43 C48 O8 177.3(3) . . . . ? C42 C43 C48 O8 -2.1(4) . . . . ? C44 C43 C48 C47 0.2(4) . . . . ? C42 C43 C48 C47 -179.2(3) . . . . ? O8 C49 C50 O9 56.8(4) . . . . ? O1 C8 N1 C7 0.0(4) . . . . ? C9 C8 N1 C7 179.6(3) . . . . ? C6 C7 N1 C8 -142.1(3) . . . . ? O6 C27 N2 C28 2.0(5) . . . . ? C26 C27 N2 C28 -176.7(3) . . . . ? C29 C28 N2 C27 -130.8(3) . . . . ? O7 C42 N3 C41 -4.9(4) . . . . ? C43 C42 N3 C41 176.8(3) . . . . ? C40 C41 N3 C42 -128.2(3) . . . . ? N1 C8 O1 Nd1 41.3(11) . . . . ? C9 C8 O1 Nd1 -138.2(8) . . . . ? O7 Nd1 O1 C8 -72.5(10) . . . . ? O6 Nd1 O1 C8 -159.2(10) . . . . ? O13 Nd1 O1 C8 54.6(10) . . . . ? O12 Nd1 O1 C8 126.4(9) . . . . ? O16 Nd1 O1 C8 8.3(10) . . . . ? O18 Nd1 O1 C8 -96.6(10) . . . . ? O10 Nd1 O1 C8 126.3(10) . . . . ? O15 Nd1 O1 C8 3.9(10) . . . . ? C13 C14 O2 C15 12.6(4) . . . . ? C9 C14 O2 C15 -167.7(3) . . . . ? C16 C15 O2 C14 166.7(3) . . . . ? C15 C16 O3 C17 156.6(3) . . . . ? C18 C17 O3 C16 172.5(3) . . . . ? C17 C18 O4 C19 -170.7(3) . . . 1_545 ? C22 C21 O5 C20 6.2(4) . . . . ? C26 C21 O5 C20 -175.2(3) . . . . ? C19 C20 O5 C21 170.1(3) . . . . ? N2 C27 O6 Nd1 107.1(10) . . . . ? C26 C27 O6 Nd1 -74.2(11) . . . . ? O7 Nd1 O6 C27 158.0(10) . . . . ? O1 Nd1 O6 C27 -121.2(10) . . . . ? O13 Nd1 O6 C27 -43.7(10) . . . . ? O12 Nd1 O6 C27 7.3(10) . . . . ? O16 Nd1 O6 C27 67.5(10) . . . . ? O18 Nd1 O6 C27 84.9(10) . . . . ? O10 Nd1 O6 C27 -44.4(10) . . . . ? O15 Nd1 O6 C27 -172.0(9) . . . . ? N3 C42 O7 Nd1 96.0(4) . . . . ? C43 C42 O7 Nd1 -85.6(4) . . . . ? O6 Nd1 O7 C42 -55.9(4) . . . . ? O1 Nd1 O7 C42 -145.7(4) . . . . ? O13 Nd1 O7 C42 139.0(3) . . . . ? O12 Nd1 O7 C42 5.9(4) . . . . ? O16 Nd1 O7 C42 68.8(4) . . . . ? O18 Nd1 O7 C42 22.4(3) . . . . ? O10 Nd1 O7 C42 -105.2(4) . . . . ? O15 Nd1 O7 C42 135.0(4) . . . . ? C47 C48 O8 C49 -11.0(4) . . . . ? C43 C48 O8 C49 172.0(3) . . . . ? C50 C49 O8 C48 -177.9(3) . . . . ? C49 C50 O9 C51 -177.0(3) . . . . ? C51 C51 O9 C50 -178.2(3) 2_666 . . . ? O11 N4 O10 Nd1 -178.2(2) . . . . ? O12 N4 O10 Nd1 2.0(3) . . . . ? O7 Nd1 O10 N4 137.56(17) . . . . ? O6 Nd1 O10 N4 85.80(16) . . . . ? O1 Nd1 O10 N4 178.70(17) . . . . ? O13 Nd1 O10 N4 -93.81(17) . . . . ? O12 Nd1 O10 N4 -1.16(15) . . . . ? O16 Nd1 O10 N4 -35.78(18) . . . . ? O18 Nd1 O10 N4 21.69(19) . . . . ? O15 Nd1 O10 N4 -113.14(16) . . . . ? O11 N4 O12 Nd1 178.2(2) . . . . ? O10 N4 O12 Nd1 -2.0(3) . . . . ? O7 Nd1 O12 N4 -142.81(16) . . . . ? O6 Nd1 O12 N4 -78.82(16) . . . . ? O1 Nd1 O12 N4 1.0(2) . . . . ? O13 Nd1 O12 N4 74.58(17) . . . . ? O16 Nd1 O12 N4 149.16(18) . . . . ? O18 Nd1 O12 N4 -159.11(17) . . . . ? O10 Nd1 O12 N4 1.17(15) . . . . ? O15 Nd1 O12 N4 100.91(17) . . . . ? O14 N5 O13 Nd1 -176.8(2) . . . . ? O15 N5 O13 Nd1 3.8(2) . . . . ? O7 Nd1 O13 N5 -7.20(18) . . . . ? O6 Nd1 O13 N5 -160.33(14) . . . . ? O1 Nd1 O13 N5 -81.13(15) . . . . ? O12 Nd1 O13 N5 149.02(16) . . . . ? O16 Nd1 O13 N5 73.11(15) . . . . ? O18 Nd1 O13 N5 83.03(16) . . . . ? O10 Nd1 O13 N5 -159.67(17) . . . . ? O15 Nd1 O13 N5 -2.16(14) . . . . ? O14 N5 O15 Nd1 176.9(2) . . . . ? O13 N5 O15 Nd1 -3.7(2) . . . . ? O7 Nd1 O15 N5 177.88(16) . . . . ? O6 Nd1 O15 N5 146.82(17) . . . . ? O1 Nd1 O15 N5 94.15(16) . . . . ? O13 Nd1 O15 N5 2.16(14) . . . . ? O12 Nd1 O15 N5 -32.45(18) . . . . ? O16 Nd1 O15 N5 -83.12(15) . . . . ? O18 Nd1 O15 N5 -115.47(15) . . . . ? O10 Nd1 O15 N5 26.16(17) . . . . ? O17 N6 O16 Nd1 -176.9(3) . . . . ? O18 N6 O16 Nd1 3.5(3) . . . . ? O7 Nd1 O16 N6 -67.11(18) . . . . ? O6 Nd1 O16 N6 20.4(2) . . . . ? O1 Nd1 O16 N6 -144.39(17) . . . . ? O13 Nd1 O16 N6 166.81(19) . . . . ? O12 Nd1 O16 N6 82.59(18) . . . . ? O18 Nd1 O16 N6 -2.08(16) . . . . ? O10 Nd1 O16 N6 109.67(18) . . . . ? O15 Nd1 O16 N6 -139.75(19) . . . . ? O17 N6 O18 Nd1 176.9(3) . . . . ? O16 N6 O18 Nd1 -3.5(3) . . . . ? O7 Nd1 O18 N6 110.62(18) . . . . ? O6 Nd1 O18 N6 -159.16(18) . . . . ? O1 Nd1 O18 N6 135.49(17) . . . . ? O13 Nd1 O18 N6 -10.4(2) . . . . ? O12 Nd1 O18 N6 -78.57(18) . . . . ? O16 Nd1 O18 N6 2.07(16) . . . . ? O10 Nd1 O18 N6 -96.54(18) . . . . ? O15 Nd1 O18 N6 42.51(19) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.478 _refine_diff_density_min -0.435 _refine_diff_density_rms 0.054 #===END data_compound10 _database_code_depnum_ccdc_archive 'CCDC 817227' #TrackingRef '- 1-12.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H54 Eu N6 O18' _chemical_formula_weight 1190.96 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.4625(3) _cell_length_b 15.9942(4) _cell_length_c 17.5529(4) _cell_angle_alpha 78.5740(10) _cell_angle_beta 86.7910(10) _cell_angle_gamma 77.0770(10) _cell_volume 3074.14(13) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4386 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 20.75 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.287 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1218 _exptl_absorpt_coefficient_mu 1.088 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.823 _exptl_absorpt_correction_T_max 0.939 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 16732 _diffrn_reflns_av_R_equivalents 0.0253 _diffrn_reflns_av_sigmaI/netI 0.0590 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 25.50 _reflns_number_total 11304 _reflns_number_gt 8225 _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 ; The distance restrains were applied to the nitrate groups in the compound. 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. Diffuse electron densities resulting from residual disorder solvent moleculeswere removed from the data set using the SQUEEZE routine of PLATON andrefined further using the data generated. ; # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.001 0.500 691.3 92.0 _platon_squeeze_details ; ; _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^)+(0.0354P)^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 11304 _refine_ls_number_parameters 661 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0630 _refine_ls_R_factor_gt 0.0417 _refine_ls_wR_factor_ref 0.0926 _refine_ls_wR_factor_gt 0.0863 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _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 Eu1 Eu 0.342224(18) 0.801378(13) 0.247282(12) 0.05344(8) Uani 1 1 d . . . C1 C 0.0758(3) 0.8798(2) 0.0573(2) 0.0549(10) Uani 1 1 d . . . C2 C 0.0170(4) 0.8902(3) -0.0145(3) 0.0625(11) Uani 1 1 d . . . C3 C -0.1031(4) 0.8865(3) -0.0123(3) 0.0770(14) Uani 1 1 d . . . H3 H -0.1424 0.8925 -0.0586 0.092 Uiso 1 1 calc R . . C4 C -0.1640(4) 0.8745(3) 0.0555(3) 0.0818(14) Uani 1 1 d . . . H4 H -0.2444 0.8723 0.0551 0.098 Uiso 1 1 calc R . . C5 C -0.1095(4) 0.8656(3) 0.1241(3) 0.0801(14) Uani 1 1 d . . . H5 H -0.1526 0.8578 0.1704 0.096 Uiso 1 1 calc R . . C6 C 0.0087(4) 0.8681(3) 0.1253(3) 0.0666(12) Uani 1 1 d . . . H6 H 0.0450 0.8619 0.1727 0.080 Uiso 1 1 calc R . . C7 C 0.2038(4) 0.8819(2) 0.0654(2) 0.0569(10) Uani 1 1 d . . . C8 C 0.3917(4) 0.9098(4) 0.0041(3) 0.0923(16) Uani 1 1 d . . . H8A H 0.4198 0.8933 0.0572 0.111 Uiso 1 1 calc R . . H8B H 0.3879 0.9719 -0.0125 0.111 Uiso 1 1 calc R . . C9 C 0.4827(4) 0.8611(3) -0.0466(2) 0.0646(11) Uani 1 1 d . . . C10 C 0.5104(6) 0.7718(4) -0.0331(3) 0.1006(18) Uani 1 1 d . . . H10 H 0.4695 0.7406 0.0056 0.121 Uiso 1 1 calc R . . C11 C 0.5971(8) 0.7284(5) -0.0758(5) 0.138(3) Uani 1 1 d . . . H11 H 0.6156 0.6676 -0.0659 0.166 Uiso 1 1 calc R . . C12 C 0.6560(6) 0.7724(9) -0.1319(5) 0.150(4) Uani 1 1 d . . . H12 H 0.7147 0.7425 -0.1614 0.180 Uiso 1 1 calc R . . C13 C 0.6297(9) 0.8612(8) -0.1457(4) 0.154(4) Uani 1 1 d . . . H13 H 0.6722 0.8920 -0.1836 0.185 Uiso 1 1 calc R . . C14 C 0.5413(6) 0.9053(4) -0.1042(3) 0.1010(18) Uani 1 1 d . . . H14 H 0.5213 0.9660 -0.1155 0.121 Uiso 1 1 calc R . . C15 C 0.0288(4) 0.9143(3) -0.1526(3) 0.0828(14) Uani 1 1 d . . . H15A H -0.0364 0.9655 -0.1600 0.099 Uiso 1 1 calc R . . H15B H -0.0026 0.8636 -0.1555 0.099 Uiso 1 1 calc R . . C16 C 0.1247(5) 0.9252(3) -0.2133(3) 0.0902(16) Uani 1 1 d . . . H16A H 0.0901 0.9395 -0.2647 0.108 Uiso 1 1 calc R . . H16B H 0.1609 0.9726 -0.2068 0.108 Uiso 1 1 calc R . . C17 C 0.3078(5) 0.8560(4) -0.2572(3) 0.0949(16) Uani 1 1 d . . . H17A H 0.3426 0.9030 -0.2478 0.114 Uiso 1 1 calc R . . H17B H 0.2795 0.8707 -0.3102 0.114 Uiso 1 1 calc R . . C18 C 0.4001(5) 0.7723(4) -0.2459(3) 0.0879(15) Uani 1 1 d . . . H18A H 0.4752 0.7830 -0.2697 0.105 Uiso 1 1 calc R . . H18B H 0.4133 0.7502 -0.1908 0.105 Uiso 1 1 calc R . . C19 C 0.4517(4) 0.6310(3) -0.2749(3) 0.0827(14) Uani 1 1 d . . . H19A H 0.4676 0.6041 -0.2208 0.099 Uiso 1 1 calc R . . H19B H 0.5253 0.6440 -0.2992 0.099 Uiso 1 1 calc R . . C20 C 0.4082(5) 0.5702(3) -0.3154(2) 0.0830(14) Uani 1 1 d . . . H20A H 0.4658 0.5149 -0.3106 0.100 Uiso 1 1 calc R . . H20B H 0.3324 0.5593 -0.2931 0.100 Uiso 1 1 calc R . . C21 C 0.3628(2) 0.57093(18) -0.44811(13) 0.0612(11) Uani 1 1 d G . . C22 C 0.3541(3) 0.48393(18) -0.42932(14) 0.0810(14) Uani 1 1 d G . . H22 H 0.3678 0.4531 -0.3787 0.097 Uiso 1 1 calc R . . C23 C 0.3248(3) 0.44301(14) -0.4862(2) 0.0856(15) Uani 1 1 d G . . H23 H 0.3190 0.3848 -0.4736 0.103 Uiso 1 1 calc R . . C24 C 0.3043(3) 0.48910(19) -0.56186(18) 0.0809(14) Uani 1 1 d G . . H24 H 0.2847 0.4617 -0.5999 0.097 Uiso 1 1 calc R . . C25 C 0.3131(2) 0.57610(19) -0.58065(12) 0.0696(12) Uani 1 1 d G . . H25 H 0.2993 0.6069 -0.6313 0.083 Uiso 1 1 calc R . . C26 C 0.3423(2) 0.61702(14) -0.52377(15) 0.0546(10) Uani 1 1 d G . . C27 C 0.0131(3) 0.6933(3) 0.2845(2) 0.0597(11) Uani 1 1 d . . . C28 C -0.0927(4) 0.6761(3) 0.2630(3) 0.0657(11) Uani 1 1 d . . . C29 C -0.1985(4) 0.7018(3) 0.3017(3) 0.0762(13) Uani 1 1 d . . . H29 H -0.2685 0.6886 0.2878 0.091 Uiso 1 1 calc R . . C30 C -0.2004(5) 0.7461(4) 0.3596(3) 0.0961(17) Uani 1 1 d . . . H30 H -0.2721 0.7645 0.3850 0.115 Uiso 1 1 calc R . . C31 C -0.0970(5) 0.7644(4) 0.3814(3) 0.1079(19) Uani 1 1 d . . . H31 H -0.0990 0.7952 0.4213 0.130 Uiso 1 1 calc R . . C32 C 0.0091(4) 0.7373(3) 0.3444(3) 0.0855(15) Uani 1 1 d . . . H32 H 0.0790 0.7488 0.3602 0.103 Uiso 1 1 calc R . . C33 C 0.1316(4) 0.6658(3) 0.2460(2) 0.0565(10) Uani 1 1 d . . . C34 C 0.2601(4) 0.5590(3) 0.1785(3) 0.0802(14) Uani 1 1 d . . . H34A H 0.2750 0.4961 0.1952 0.096 Uiso 1 1 calc R . . H34B H 0.3243 0.5792 0.1979 0.096 Uiso 1 1 calc R . . C35 C 0.2625(4) 0.5805(3) 0.0906(3) 0.0741(13) Uani 1 1 d . . . C36 C 0.3369(5) 0.5249(4) 0.0518(4) 0.111(2) Uani 1 1 d . . . H36 H 0.3849 0.4742 0.0790 0.134 Uiso 1 1 calc R . . C37 C 0.3415(6) 0.5433(6) -0.0278(5) 0.132(3) Uani 1 1 d . . . H37 H 0.3930 0.5043 -0.0538 0.158 Uiso 1 1 calc R . . C38 C 0.2740(6) 0.6160(6) -0.0697(4) 0.112(2) Uani 1 1 d . . . H38 H 0.2767 0.6267 -0.1237 0.134 Uiso 1 1 calc R . . C39 C 0.2016(7) 0.6734(4) -0.0303(5) 0.134(2) Uani 1 1 d . . . H39 H 0.1556 0.7252 -0.0573 0.161 Uiso 1 1 calc R . . C40 C 0.1967(5) 0.6545(4) 0.0490(4) 0.1048(18) Uani 1 1 d . . . H40 H 0.1464 0.6940 0.0752 0.126 Uiso 1 1 calc R . . C41 C -0.1916(4) 0.6331(4) 0.1636(4) 0.1035(19) Uani 1 1 d . . . H41A H -0.2538 0.6848 0.1659 0.124 Uiso 1 1 calc R . . H41B H -0.2208 0.5821 0.1894 0.124 Uiso 1 1 calc R . . C42 C -0.1591(5) 0.6270(4) 0.0820(4) 0.117(2) Uani 1 1 d . . . H42A H -0.2304 0.6290 0.0538 0.141 Uiso 1 1 calc R . . H42B H -0.1255 0.6765 0.0578 0.141 Uiso 1 1 calc R . . C43 C -0.0459(4) 0.5410(3) 0.0007(4) 0.1041(18) Uani 1 1 d . . . H43A H -0.0148 0.5908 -0.0259 0.125 Uiso 1 1 calc R . . H43B H -0.1169 0.5397 -0.0262 0.125 Uiso 1 1 calc R . . C44 C 0.3494(3) 0.7096(3) 0.4496(2) 0.0600(11) Uani 1 1 d . . . C45 C 0.3790(5) 0.8467(3) 0.4812(3) 0.0926(16) Uani 1 1 d . . . H45A H 0.3020 0.8857 0.4859 0.111 Uiso 1 1 calc R . . H45B H 0.4065 0.8591 0.4277 0.111 Uiso 1 1 calc R . . C46 C 0.4670(4) 0.8628(3) 0.53398(18) 0.0838(15) Uani 1 1 d G . . C47 C 0.5789(4) 0.8067(2) 0.5449(3) 0.125(2) Uani 1 1 d G . . H47 H 0.5979 0.7583 0.5211 0.150 Uiso 1 1 calc R . . C48 C 0.6623(4) 0.8228(4) 0.5915(3) 0.184(4) Uani 1 1 d G . . H48 H 0.7372 0.7852 0.5988 0.221 Uiso 1 1 calc R . . C49 C 0.6339(5) 0.8952(4) 0.6271(2) 0.193(5) Uani 1 1 d G . . H49 H 0.6897 0.9060 0.6583 0.232 Uiso 1 1 calc R . . C50 C 0.5221(6) 0.9514(3) 0.6162(2) 0.156(4) Uani 1 1 d G . . H50 H 0.5031 0.9998 0.6401 0.188 Uiso 1 1 calc R . . C51 C 0.4386(4) 0.9352(2) 0.5696(2) 0.116(2) Uani 1 1 d G . . H51 H 0.3638 0.9728 0.5623 0.139 Uiso 1 1 calc R . . N1 N 0.1961(4) 0.9590(3) 0.2907(2) 0.0848(13) Uani 1 1 d D . . N2 N 0.5570(3) 0.8719(3) 0.2416(3) 0.0751(11) Uani 1 1 d D . . N3 N 0.4971(3) 0.6550(2) 0.1900(2) 0.0628(9) Uani 1 1 d D . . N4 N 0.2710(3) 0.8946(2) 0.0033(2) 0.0734(10) Uani 1 1 d . . . H4A H 0.2422 0.8939 -0.0408 0.088 Uiso 1 1 calc R . . N5 N 0.1483(3) 0.5977(2) 0.2121(2) 0.0730(10) Uani 1 1 d . . . H5A H 0.0881 0.5745 0.2098 0.088 Uiso 1 1 calc R . . N6 N 0.3656(3) 0.7562(2) 0.5010(2) 0.0770(11) Uani 1 1 d . . . H6A H 0.3684 0.7315 0.5493 0.092 Uiso 1 1 calc R . . O1 O 0.3014(3) 0.9527(2) 0.2681(2) 0.0983(12) Uani 1 1 d D . . O2 O 0.1537(3) 0.8924(2) 0.29416(18) 0.0821(9) Uani 1 1 d D . . O3 O 0.1370(3) 1.0260(3) 0.3067(3) 0.1361(18) Uani 1 1 d D . . O4 O 0.5072(3) 0.8656(2) 0.18064(19) 0.0843(9) Uani 1 1 d D . . O5 O 0.5191(3) 0.8338(2) 0.3051(2) 0.0814(9) Uani 1 1 d D . . O6 O 0.6360(3) 0.9120(2) 0.2384(2) 0.1032(12) Uani 1 1 d D . . O7 O 0.4272(3) 0.71473(19) 0.14633(16) 0.0706(8) Uani 1 1 d D . . O8 O 0.4998(2) 0.66268(18) 0.26029(17) 0.0731(8) Uani 1 1 d D . . O9 O 0.5559(3) 0.5909(2) 0.16648(19) 0.0849(10) Uani 1 1 d D . . O10 O 0.2445(2) 0.87434(18) 0.13128(16) 0.0694(8) Uani 1 1 d . . . O11 O 0.0836(2) 0.90350(19) -0.08012(16) 0.0694(8) Uani 1 1 d . . . O12 O 0.2125(3) 0.8467(2) -0.20577(17) 0.0824(9) Uani 1 1 d . . . O13 O 0.3624(3) 0.7085(2) -0.27997(16) 0.0777(9) Uani 1 1 d . . . O14 O 0.3941(3) 0.61238(18) -0.39565(15) 0.0737(8) Uani 1 1 d . . . O15 O 0.2135(2) 0.70543(18) 0.24935(15) 0.0621(7) Uani 1 1 d . . . O16 O -0.0863(2) 0.6378(2) 0.1998(2) 0.0992(12) Uani 1 1 d . . . O17 O -0.0754(3) 0.5491(2) 0.0780(2) 0.0950(10) Uani 1 1 d . . . O18 O 0.3391(3) 0.74449(18) 0.37927(16) 0.0701(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu1 0.05215(13) 0.05781(14) 0.05422(13) -0.01451(9) -0.01256(9) -0.01372(9) C1 0.054(3) 0.042(2) 0.064(3) -0.0127(19) -0.009(2) 0.0040(18) C2 0.067(3) 0.055(3) 0.064(3) -0.016(2) -0.018(2) 0.000(2) C3 0.064(3) 0.074(3) 0.091(4) -0.021(3) -0.025(3) 0.000(2) C4 0.059(3) 0.075(3) 0.106(4) -0.011(3) 0.000(3) -0.008(2) C5 0.075(4) 0.070(3) 0.084(4) -0.005(3) 0.010(3) -0.004(3) C6 0.068(3) 0.063(3) 0.059(3) -0.007(2) -0.002(2) 0.002(2) C7 0.070(3) 0.044(2) 0.055(3) -0.0150(19) -0.010(2) 0.000(2) C8 0.078(3) 0.112(4) 0.101(4) -0.041(3) -0.001(3) -0.033(3) C9 0.067(3) 0.077(3) 0.053(3) -0.004(2) -0.011(2) -0.027(3) C10 0.158(6) 0.075(4) 0.062(3) -0.003(3) -0.003(3) -0.019(4) C11 0.168(8) 0.115(6) 0.111(6) -0.040(5) -0.048(5) 0.037(5) C12 0.079(4) 0.280(13) 0.120(7) -0.112(9) 0.011(4) -0.040(7) C13 0.172(9) 0.253(11) 0.094(5) -0.053(7) 0.046(5) -0.156(9) C14 0.142(5) 0.102(4) 0.070(4) -0.007(3) 0.015(4) -0.062(4) C15 0.093(4) 0.095(4) 0.056(3) -0.021(2) -0.018(3) -0.001(3) C16 0.115(4) 0.085(4) 0.065(3) -0.019(3) -0.023(3) -0.002(3) C17 0.117(4) 0.098(4) 0.076(4) -0.030(3) 0.012(3) -0.028(4) C18 0.088(4) 0.117(4) 0.069(3) -0.027(3) 0.002(3) -0.035(3) C19 0.097(4) 0.090(4) 0.052(3) -0.011(2) -0.014(2) 0.001(3) C20 0.114(4) 0.071(3) 0.054(3) -0.008(2) -0.002(3) -0.001(3) C21 0.062(3) 0.064(3) 0.059(3) -0.019(2) 0.004(2) -0.012(2) C22 0.101(4) 0.066(3) 0.073(3) -0.010(3) 0.003(3) -0.018(3) C23 0.096(4) 0.062(3) 0.106(4) -0.024(3) 0.007(3) -0.026(3) C24 0.086(3) 0.078(4) 0.092(4) -0.037(3) -0.002(3) -0.027(3) C25 0.078(3) 0.071(3) 0.068(3) -0.022(2) -0.010(2) -0.024(2) C26 0.049(2) 0.065(3) 0.055(2) -0.018(2) -0.0049(19) -0.017(2) C27 0.050(2) 0.071(3) 0.058(3) -0.008(2) -0.002(2) -0.019(2) C28 0.054(3) 0.069(3) 0.079(3) -0.019(2) -0.005(2) -0.019(2) C29 0.052(3) 0.098(4) 0.081(3) -0.018(3) 0.004(2) -0.021(3) C30 0.071(4) 0.134(5) 0.079(4) -0.023(3) 0.015(3) -0.015(3) C31 0.094(4) 0.148(6) 0.096(4) -0.064(4) 0.013(3) -0.023(4) C32 0.073(3) 0.126(4) 0.071(3) -0.044(3) 0.004(3) -0.029(3) C33 0.053(3) 0.067(3) 0.052(2) -0.008(2) -0.011(2) -0.017(2) C34 0.059(3) 0.074(3) 0.112(4) -0.033(3) -0.001(3) -0.013(2) C35 0.061(3) 0.068(3) 0.108(4) -0.042(3) 0.002(3) -0.021(2) C36 0.087(4) 0.129(5) 0.127(6) -0.074(5) 0.004(4) 0.000(4) C37 0.096(5) 0.162(7) 0.158(7) -0.100(6) 0.017(5) -0.016(5) C38 0.094(5) 0.157(7) 0.102(5) -0.038(5) 0.014(4) -0.055(5) C39 0.186(7) 0.089(5) 0.120(6) -0.020(4) 0.013(5) -0.020(5) C40 0.130(5) 0.076(4) 0.105(5) -0.028(3) 0.014(4) -0.010(4) C41 0.062(3) 0.132(5) 0.138(5) -0.069(4) -0.020(3) -0.023(3) C42 0.096(4) 0.141(6) 0.124(5) -0.064(4) -0.036(4) -0.004(4) C43 0.093(4) 0.108(5) 0.129(5) -0.051(4) -0.013(4) -0.031(3) C44 0.061(3) 0.069(3) 0.056(3) -0.018(2) -0.015(2) -0.017(2) C45 0.138(5) 0.071(3) 0.077(3) -0.012(3) -0.026(3) -0.035(3) C46 0.140(5) 0.082(4) 0.050(3) -0.024(2) 0.014(3) -0.060(3) C47 0.130(5) 0.146(6) 0.118(5) -0.056(5) 0.001(4) -0.041(5) C48 0.128(6) 0.279(12) 0.173(9) -0.038(8) -0.029(6) -0.098(7) C49 0.295(13) 0.256(12) 0.094(6) -0.021(7) -0.026(7) -0.200(11) C50 0.293(12) 0.159(7) 0.069(4) -0.026(4) 0.008(6) -0.156(8) C51 0.210(7) 0.098(4) 0.067(4) -0.033(3) 0.034(4) -0.084(4) N1 0.075(3) 0.085(3) 0.100(3) -0.050(3) -0.037(3) 0.008(3) N2 0.057(3) 0.070(3) 0.105(4) -0.027(2) -0.011(2) -0.014(2) N3 0.050(2) 0.072(3) 0.071(3) -0.021(2) 0.0060(19) -0.0164(19) N4 0.062(2) 0.103(3) 0.063(2) -0.029(2) -0.0066(19) -0.022(2) N5 0.055(2) 0.077(3) 0.103(3) -0.045(2) 0.006(2) -0.0245(19) N6 0.119(3) 0.063(2) 0.057(2) -0.0115(18) -0.023(2) -0.031(2) O1 0.071(2) 0.076(2) 0.159(4) -0.051(2) -0.012(2) -0.0100(19) O2 0.076(2) 0.087(2) 0.091(2) -0.0380(19) 0.0014(17) -0.0152(19) O3 0.096(3) 0.113(3) 0.212(5) -0.105(3) -0.046(3) 0.027(2) O4 0.074(2) 0.103(3) 0.086(2) -0.0162(19) -0.0072(18) -0.0389(18) O5 0.062(2) 0.103(3) 0.087(2) -0.023(2) -0.0167(18) -0.0272(18) O6 0.068(2) 0.104(3) 0.155(4) -0.036(2) -0.006(2) -0.042(2) O7 0.080(2) 0.073(2) 0.0531(17) -0.0092(15) -0.0037(15) -0.0069(17) O8 0.075(2) 0.077(2) 0.065(2) -0.0206(16) -0.0204(16) 0.0012(15) O9 0.067(2) 0.088(2) 0.105(3) -0.045(2) 0.0096(18) -0.0083(18) O10 0.0729(19) 0.076(2) 0.0562(18) -0.0096(14) -0.0222(15) -0.0081(15) O11 0.0742(19) 0.086(2) 0.0486(17) -0.0180(14) -0.0114(15) -0.0125(16) O12 0.096(2) 0.085(2) 0.064(2) -0.0185(17) 0.0058(18) -0.013(2) O13 0.084(2) 0.092(2) 0.0604(19) -0.0231(17) -0.0119(16) -0.0157(19) O14 0.109(2) 0.071(2) 0.0436(16) -0.0105(14) -0.0078(16) -0.0225(17) O15 0.0557(17) 0.0757(19) 0.0662(18) -0.0234(14) -0.0053(13) -0.0280(15) O16 0.0530(18) 0.134(3) 0.135(3) -0.076(3) -0.0160(19) -0.0222(18) O17 0.089(2) 0.105(3) 0.106(3) -0.048(2) -0.010(2) -0.026(2) O18 0.093(2) 0.075(2) 0.0503(17) -0.0112(14) -0.0161(15) -0.0324(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 Eu1 O18 2.317(3) . ? Eu1 O10 2.343(3) . ? Eu1 O15 2.349(3) . ? Eu1 O1 2.456(3) . ? Eu1 O4 2.479(3) . ? Eu1 O7 2.487(3) . ? Eu1 O8 2.508(3) . ? Eu1 O5 2.513(3) . ? Eu1 O2 2.517(3) . ? C1 C6 1.386(5) . ? C1 C2 1.425(5) . ? C1 C7 1.491(5) . ? C2 O11 1.354(5) . ? C2 C3 1.389(6) . ? C3 C4 1.347(6) . ? C3 H3 0.9300 . ? C4 C5 1.356(6) . ? C4 H4 0.9300 . ? C5 C6 1.365(6) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 O10 1.244(4) . ? C7 N4 1.308(5) . ? C8 N4 1.459(5) . ? C8 C9 1.514(6) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C14 1.351(6) . ? C9 C10 1.366(6) . ? C10 C11 1.358(9) . ? C10 H10 0.9300 . ? C11 C12 1.337(10) . ? C11 H11 0.9300 . ? C12 C13 1.358(11) . ? C12 H12 0.9300 . ? C13 C14 1.362(10) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 O11 1.413(4) . ? C15 C16 1.502(6) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 O12 1.411(5) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 O12 1.392(5) . ? C17 C18 1.495(7) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 O13 1.434(5) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 O13 1.412(5) . ? C19 C20 1.493(6) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 O14 1.437(5) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 O14 1.342(3) . ? C21 C22 1.3900 . ? C21 C26 1.3900 . ? C22 C23 1.3900 . ? C22 H22 0.9300 . ? C23 C24 1.3900 . ? C23 H23 0.9300 . ? C24 C25 1.3900 . ? C24 H24 0.9300 . ? C25 C26 1.3900 . ? C25 H25 0.9300 . ? C26 C44 1.482(5) 1_554 ? C27 C32 1.370(6) . ? C27 C28 1.390(5) . ? C27 C33 1.497(5) . ? C28 O16 1.360(5) . ? C28 C29 1.377(6) . ? C29 C30 1.346(6) . ? C29 H29 0.9300 . ? C30 C31 1.373(7) . ? C30 H30 0.9300 . ? C31 C32 1.369(6) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 O15 1.255(4) . ? C33 N5 1.313(5) . ? C34 N5 1.442(5) . ? C34 C35 1.512(6) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.347(6) . ? C35 C40 1.351(7) . ? C36 C37 1.371(9) . ? C36 H36 0.9300 . ? C37 C38 1.347(8) . ? C37 H37 0.9300 . ? C38 C39 1.362(8) . ? C38 H38 0.9300 . ? C39 C40 1.365(8) . ? C39 H39 0.9300 . ? C40 H40 0.9300 . ? C41 O16 1.419(5) . ? C41 C42 1.475(7) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 O17 1.404(6) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 O17 1.404(6) . ? C43 C43 1.489(10) 2_565 ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 O18 1.249(4) . ? C44 N6 1.323(5) . ? C44 C26 1.48(3) 1_556 ? C45 N6 1.461(5) . ? C45 C46 1.503(5) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 C47 1.3900 . ? C46 C51 1.3900 . ? C47 C48 1.3900 . ? C47 H47 0.9300 . ? C48 C49 1.3900 . ? C48 H48 0.9300 . ? C49 C50 1.3900 . ? C49 H49 0.9300 . ? C50 C51 1.3900 . ? C50 H50 0.9300 . ? C51 H51 0.9300 . ? N1 O3 1.208(4) . ? N1 O1 1.239(5) . ? N1 O2 1.256(5) . ? N2 O6 1.213(4) . ? N2 O5 1.264(5) . ? N2 O4 1.273(4) . ? N3 O9 1.225(4) . ? N3 O7 1.257(4) . ? N3 O8 1.266(4) . ? N4 H4A 0.8600 . ? N5 H5A 0.8600 . ? N6 H6A 0.8600 . ? 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 O18 Eu1 O10 151.22(10) . . ? O18 Eu1 O15 80.01(9) . . ? O10 Eu1 O15 83.94(10) . . ? O18 Eu1 O1 92.83(11) . . ? O10 Eu1 O1 79.84(11) . . ? O15 Eu1 O1 130.84(11) . . ? O18 Eu1 O4 123.58(10) . . ? O10 Eu1 O4 81.38(10) . . ? O15 Eu1 O4 147.92(10) . . ? O1 Eu1 O4 74.04(12) . . ? O18 Eu1 O7 124.38(10) . . ? O10 Eu1 O7 73.55(9) . . ? O15 Eu1 O7 75.87(9) . . ? O1 Eu1 O7 139.81(12) . . ? O4 Eu1 O7 72.66(10) . . ? O18 Eu1 O8 77.00(10) . . ? O10 Eu1 O8 124.43(9) . . ? O15 Eu1 O8 82.59(9) . . ? O1 Eu1 O8 143.33(11) . . ? O4 Eu1 O8 82.50(10) . . ? O7 Eu1 O8 50.88(9) . . ? O18 Eu1 O5 72.97(11) . . ? O10 Eu1 O5 127.71(11) . . ? O15 Eu1 O5 147.89(11) . . ? O1 Eu1 O5 68.55(11) . . ? O4 Eu1 O5 50.95(10) . . ? O7 Eu1 O5 105.44(10) . . ? O8 Eu1 O5 74.80(10) . . ? O18 Eu1 O2 76.86(10) . . ? O10 Eu1 O2 77.14(10) . . ? O15 Eu1 O2 80.91(10) . . ? O1 Eu1 O2 50.34(11) . . ? O4 Eu1 O2 122.76(11) . . ? O7 Eu1 O2 144.11(10) . . ? O8 Eu1 O2 151.07(11) . . ? O5 Eu1 O2 108.76(11) . . ? C6 C1 C2 117.8(4) . . ? C6 C1 C7 117.0(4) . . ? C2 C1 C7 125.2(4) . . ? O11 C2 C3 125.0(4) . . ? O11 C2 C1 116.7(4) . . ? C3 C2 C1 118.3(4) . . ? C4 C3 C2 121.5(5) . . ? C4 C3 H3 119.2 . . ? C2 C3 H3 119.2 . . ? C3 C4 C5 120.7(5) . . ? C3 C4 H4 119.6 . . ? C5 C4 H4 119.6 . . ? C4 C5 C6 120.1(5) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C5 C6 C1 121.5(4) . . ? C5 C6 H6 119.2 . . ? C1 C6 H6 119.2 . . ? O10 C7 N4 120.8(4) . . ? O10 C7 C1 119.4(4) . . ? N4 C7 C1 119.7(4) . . ? N4 C8 C9 115.3(4) . . ? N4 C8 H8A 108.4 . . ? C9 C8 H8A 108.4 . . ? N4 C8 H8B 108.4 . . ? C9 C8 H8B 108.4 . . ? H8A C8 H8B 107.5 . . ? C14 C9 C10 118.8(5) . . ? C14 C9 C8 120.5(5) . . ? C10 C9 C8 120.7(5) . . ? C11 C10 C9 120.6(6) . . ? C11 C10 H10 119.7 . . ? C9 C10 H10 119.7 . . ? C12 C11 C10 120.4(8) . . ? C12 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? C11 C12 C13 119.7(8) . . ? C11 C12 H12 120.2 . . ? C13 C12 H12 120.2 . . ? C12 C13 C14 120.3(8) . . ? C12 C13 H13 119.8 . . ? C14 C13 H13 119.8 . . ? C9 C14 C13 120.3(6) . . ? C9 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? O11 C15 C16 106.2(4) . . ? O11 C15 H15A 110.5 . . ? C16 C15 H15A 110.5 . . ? O11 C15 H15B 110.5 . . ? C16 C15 H15B 110.5 . . ? H15A C15 H15B 108.7 . . ? O12 C16 C15 109.1(4) . . ? O12 C16 H16A 109.9 . . ? C15 C16 H16A 109.9 . . ? O12 C16 H16B 109.9 . . ? C15 C16 H16B 109.9 . . ? H16A C16 H16B 108.3 . . ? O12 C17 C18 109.4(4) . . ? O12 C17 H17A 109.8 . . ? C18 C17 H17A 109.8 . . ? O12 C17 H17B 109.8 . . ? C18 C17 H17B 109.8 . . ? H17A C17 H17B 108.2 . . ? O13 C18 C17 110.7(4) . . ? O13 C18 H18A 109.5 . . ? C17 C18 H18A 109.5 . . ? O13 C18 H18B 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 108.1 . . ? O13 C19 C20 108.3(4) . . ? O13 C19 H19A 110.0 . . ? C20 C19 H19A 110.0 . . ? O13 C19 H19B 110.0 . . ? C20 C19 H19B 110.0 . . ? H19A C19 H19B 108.4 . . ? O14 C20 C19 106.5(4) . . ? O14 C20 H20A 110.4 . . ? C19 C20 H20A 110.4 . . ? O14 C20 H20B 110.4 . . ? C19 C20 H20B 110.4 . . ? H20A C20 H20B 108.6 . . ? O14 C21 C22 122.1(2) . . ? O14 C21 C26 117.9(2) . . ? C22 C21 C26 120.0 . . ? C23 C22 C21 120.0 . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C24 C23 C22 120.0 . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? C23 C24 C25 120.0 . . ? C23 C24 H24 120.0 . . ? C25 C24 H24 120.0 . . ? C26 C25 C24 120.0 . . ? C26 C25 H25 120.0 . . ? C24 C25 H25 120.0 . . ? C25 C26 C21 120.0 . . ? C25 C26 C44 115.3(2) . 1_554 ? C21 C26 C44 124.7(2) . 1_554 ? C32 C27 C28 118.3(4) . . ? C32 C27 C33 118.2(4) . . ? C28 C27 C33 123.5(4) . . ? O16 C28 C29 122.8(4) . . ? O16 C28 C27 116.4(4) . . ? C29 C28 C27 120.7(4) . . ? C30 C29 C28 119.8(4) . . ? C30 C29 H29 120.1 . . ? C28 C29 H29 120.1 . . ? C29 C30 C31 120.4(5) . . ? C29 C30 H30 119.8 . . ? C31 C30 H30 119.8 . . ? C32 C31 C30 120.1(5) . . ? C32 C31 H31 119.9 . . ? C30 C31 H31 119.9 . . ? C31 C32 C27 120.6(5) . . ? C31 C32 H32 119.7 . . ? C27 C32 H32 119.7 . . ? O15 C33 N5 121.6(4) . . ? O15 C33 C27 119.9(4) . . ? N5 C33 C27 118.4(4) . . ? N5 C34 C35 113.4(4) . . ? N5 C34 H34A 108.9 . . ? C35 C34 H34A 108.9 . . ? N5 C34 H34B 108.9 . . ? C35 C34 H34B 108.9 . . ? H34A C34 H34B 107.7 . . ? C36 C35 C40 118.2(6) . . ? C36 C35 C34 118.7(5) . . ? C40 C35 C34 123.0(5) . . ? C35 C36 C37 119.8(6) . . ? C35 C36 H36 120.1 . . ? C37 C36 H36 120.1 . . ? C38 C37 C36 122.3(6) . . ? C38 C37 H37 118.9 . . ? C36 C37 H37 118.9 . . ? C37 C38 C39 117.8(7) . . ? C37 C38 H38 121.1 . . ? C39 C38 H38 121.1 . . ? C38 C39 C40 119.7(7) . . ? C38 C39 H39 120.2 . . ? C40 C39 H39 120.2 . . ? C35 C40 C39 122.2(6) . . ? C35 C40 H40 118.9 . . ? C39 C40 H40 118.9 . . ? O16 C41 C42 106.8(4) . . ? O16 C41 H41A 110.4 . . ? C42 C41 H41A 110.4 . . ? O16 C41 H41B 110.4 . . ? C42 C41 H41B 110.4 . . ? H41A C41 H41B 108.6 . . ? O17 C42 C41 110.7(5) . . ? O17 C42 H42A 109.5 . . ? C41 C42 H42A 109.5 . . ? O17 C42 H42B 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 108.1 . . ? O17 C43 C43 109.6(6) . 2_565 ? O17 C43 H43A 109.7 . . ? C43 C43 H43A 109.7 2_565 . ? O17 C43 H43B 109.7 . . ? C43 C43 H43B 109.7 2_565 . ? H43A C43 H43B 108.2 . . ? O18 C44 N6 119.7(4) . . ? O18 C44 C26 120.8(4) . 1_556 ? N6 C44 C26 119.5(4) . 1_556 ? N6 C45 C46 110.8(4) . . ? N6 C45 H45A 109.5 . . ? C46 C45 H45A 109.5 . . ? N6 C45 H45B 109.5 . . ? C46 C45 H45B 109.5 . . ? H45A C45 H45B 108.1 . . ? C47 C46 C51 120.0 . . ? C47 C46 C45 119.6(4) . . ? C51 C46 C45 120.3(4) . . ? C48 C47 C46 120.0 . . ? C48 C47 H47 120.0 . . ? C46 C47 H47 120.0 . . ? C47 C48 C49 120.0 . . ? C47 C48 H48 120.0 . . ? C49 C48 H48 120.0 . . ? C50 C49 C48 120.0 . . ? C50 C49 H49 120.0 . . ? C48 C49 H49 120.0 . . ? C49 C50 C51 120.0 . . ? C49 C50 H50 120.0 . . ? C51 C50 H50 120.0 . . ? C50 C51 C46 120.0 . . ? C50 C51 H51 120.0 . . ? C46 C51 H51 120.0 . . ? O3 N1 O1 121.8(5) . . ? O3 N1 O2 122.1(5) . . ? O1 N1 O2 116.0(4) . . ? O6 N2 O5 122.7(4) . . ? O6 N2 O4 121.6(5) . . ? O5 N2 O4 115.7(4) . . ? O9 N3 O7 121.6(4) . . ? O9 N3 O8 121.8(4) . . ? O7 N3 O8 116.5(3) . . ? C7 N4 C8 124.0(4) . . ? C7 N4 H4A 118.0 . . ? C8 N4 H4A 118.0 . . ? C33 N5 C34 124.9(4) . . ? C33 N5 H5A 117.6 . . ? C34 N5 H5A 117.6 . . ? C44 N6 C45 124.3(4) . . ? C44 N6 H6A 117.8 . . ? C45 N6 H6A 117.8 . . ? N1 O1 Eu1 98.5(3) . . ? N1 O2 Eu1 95.1(3) . . ? N2 O4 Eu1 96.8(3) . . ? N2 O5 Eu1 95.5(3) . . ? N3 O7 Eu1 96.9(2) . . ? N3 O8 Eu1 95.7(2) . . ? C7 O10 Eu1 156.6(3) . . ? C2 O11 C15 118.6(3) . . ? C17 O12 C16 111.0(4) . . ? C19 O13 C18 111.7(4) . . ? C21 O14 C20 120.4(3) . . ? C33 O15 Eu1 170.2(3) . . ? C28 O16 C41 121.0(4) . . ? C42 O17 C43 111.6(4) . . ? C44 O18 Eu1 173.5(3) . . ? 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 O11 178.5(3) . . . . ? C7 C1 C2 O11 -0.4(6) . . . . ? C6 C1 C2 C3 -1.1(6) . . . . ? C7 C1 C2 C3 180.0(4) . . . . ? O11 C2 C3 C4 -178.8(4) . . . . ? C1 C2 C3 C4 0.8(6) . . . . ? C2 C3 C4 C5 0.0(7) . . . . ? C3 C4 C5 C6 -0.5(7) . . . . ? C4 C5 C6 C1 0.0(7) . . . . ? C2 C1 C6 C5 0.7(6) . . . . ? C7 C1 C6 C5 179.7(4) . . . . ? C6 C1 C7 O10 -0.8(5) . . . . ? C2 C1 C7 O10 178.1(4) . . . . ? C6 C1 C7 N4 -178.6(4) . . . . ? C2 C1 C7 N4 0.3(6) . . . . ? N4 C8 C9 C14 121.0(5) . . . . ? N4 C8 C9 C10 -61.5(6) . . . . ? C14 C9 C10 C11 1.4(8) . . . . ? C8 C9 C10 C11 -176.1(5) . . . . ? C9 C10 C11 C12 -0.5(10) . . . . ? C10 C11 C12 C13 0.7(12) . . . . ? C11 C12 C13 C14 -2.0(13) . . . . ? C10 C9 C14 C13 -2.7(8) . . . . ? C8 C9 C14 C13 174.9(5) . . . . ? C12 C13 C14 C9 3.0(11) . . . . ? O11 C15 C16 O12 65.9(5) . . . . ? O12 C17 C18 O13 75.8(5) . . . . ? O13 C19 C20 O14 63.2(5) . . . . ? O14 C21 C22 C23 -178.1(3) . . . . ? C26 C21 C22 C23 0.0 . . . . ? C21 C22 C23 C24 0.0 . . . . ? C22 C23 C24 C25 0.0 . . . . ? C23 C24 C25 C26 0.0 . . . . ? C24 C25 C26 C21 0.0 . . . . ? C24 C25 C26 C44 179.8(3) . . . 1_554 ? O14 C21 C26 C25 178.2(3) . . . . ? C22 C21 C26 C25 0.0 . . . . ? O14 C21 C26 C44 -1.6(3) . . . 1_554 ? C22 C21 C26 C44 -179.8(3) . . . 1_554 ? C32 C27 C28 O16 175.6(4) . . . . ? C33 C27 C28 O16 -4.8(6) . . . . ? C32 C27 C28 C29 -0.8(7) . . . . ? C33 C27 C28 C29 178.7(4) . . . . ? O16 C28 C29 C30 -174.3(5) . . . . ? C27 C28 C29 C30 1.9(7) . . . . ? C28 C29 C30 C31 -1.3(8) . . . . ? C29 C30 C31 C32 -0.2(9) . . . . ? C30 C31 C32 C27 1.3(9) . . . . ? C28 C27 C32 C31 -0.8(8) . . . . ? C33 C27 C32 C31 179.7(5) . . . . ? C32 C27 C33 O15 -23.5(6) . . . . ? C28 C27 C33 O15 156.9(4) . . . . ? C32 C27 C33 N5 153.7(4) . . . . ? C28 C27 C33 N5 -25.8(6) . . . . ? N5 C34 C35 C36 -154.5(4) . . . . ? N5 C34 C35 C40 28.0(7) . . . . ? C40 C35 C36 C37 -1.7(8) . . . . ? C34 C35 C36 C37 -179.4(5) . . . . ? C35 C36 C37 C38 0.2(10) . . . . ? C36 C37 C38 C39 1.7(10) . . . . ? C37 C38 C39 C40 -2.1(10) . . . . ? C36 C35 C40 C39 1.4(9) . . . . ? C34 C35 C40 C39 178.9(6) . . . . ? C38 C39 C40 C35 0.6(10) . . . . ? O16 C41 C42 O17 64.3(6) . . . . ? N6 C45 C46 C47 50.5(5) . . . . ? N6 C45 C46 C51 -131.7(4) . . . . ? C51 C46 C47 C48 0.0 . . . . ? C45 C46 C47 C48 177.8(4) . . . . ? C46 C47 C48 C49 0.0 . . . . ? C47 C48 C49 C50 0.0 . . . . ? C48 C49 C50 C51 0.0 . . . . ? C49 C50 C51 C46 0.0 . . . . ? C47 C46 C51 C50 0.0 . . . . ? C45 C46 C51 C50 -177.8(4) . . . . ? O10 C7 N4 C8 -6.5(6) . . . . ? C1 C7 N4 C8 171.2(4) . . . . ? C9 C8 N4 C7 137.0(4) . . . . ? O15 C33 N5 C34 2.6(7) . . . . ? C27 C33 N5 C34 -174.6(4) . . . . ? C35 C34 N5 C33 -104.7(5) . . . . ? O18 C44 N6 C45 -3.5(7) . . . . ? C26 C44 N6 C45 177.3(13) 1_556 . . . ? C46 C45 N6 C44 -143.9(4) . . . . ? O3 N1 O1 Eu1 -178.4(4) . . . . ? O2 N1 O1 Eu1 0.0(4) . . . . ? O18 Eu1 O1 N1 -70.3(3) . . . . ? O10 Eu1 O1 N1 81.7(3) . . . . ? O15 Eu1 O1 N1 8.9(3) . . . . ? O4 Eu1 O1 N1 165.5(3) . . . . ? O7 Eu1 O1 N1 130.5(3) . . . . ? O8 Eu1 O1 N1 -142.2(2) . . . . ? O5 Eu1 O1 N1 -140.8(3) . . . . ? O2 Eu1 O1 N1 0.0(2) . . . . ? O3 N1 O2 Eu1 178.4(4) . . . . ? O1 N1 O2 Eu1 0.0(4) . . . . ? O18 Eu1 O2 N1 105.0(3) . . . . ? O10 Eu1 O2 N1 -87.4(3) . . . . ? O15 Eu1 O2 N1 -173.2(3) . . . . ? O1 Eu1 O2 N1 0.0(2) . . . . ? O4 Eu1 O2 N1 -16.6(3) . . . . ? O7 Eu1 O2 N1 -123.2(3) . . . . ? O8 Eu1 O2 N1 130.8(3) . . . . ? O5 Eu1 O2 N1 38.4(3) . . . . ? O6 N2 O4 Eu1 -169.8(3) . . . . ? O5 N2 O4 Eu1 10.4(4) . . . . ? O18 Eu1 O4 N2 -13.6(3) . . . . ? O10 Eu1 O4 N2 150.8(2) . . . . ? O15 Eu1 O4 N2 -145.4(2) . . . . ? O1 Eu1 O4 N2 69.0(2) . . . . ? O7 Eu1 O4 N2 -133.8(3) . . . . ? O8 Eu1 O4 N2 -82.5(2) . . . . ? O5 Eu1 O4 N2 -6.0(2) . . . . ? O2 Eu1 O4 N2 82.3(3) . . . . ? O6 N2 O5 Eu1 170.0(4) . . . . ? O4 N2 O5 Eu1 -10.2(4) . . . . ? O18 Eu1 O5 N2 179.5(3) . . . . ? O10 Eu1 O5 N2 -23.3(3) . . . . ? O15 Eu1 O5 N2 145.5(2) . . . . ? O1 Eu1 O5 N2 -80.4(3) . . . . ? O4 Eu1 O5 N2 6.1(2) . . . . ? O7 Eu1 O5 N2 57.6(3) . . . . ? O8 Eu1 O5 N2 98.7(3) . . . . ? O2 Eu1 O5 N2 -111.3(2) . . . . ? O9 N3 O7 Eu1 175.1(3) . . . . ? O8 N3 O7 Eu1 -2.0(3) . . . . ? O18 Eu1 O7 N3 -23.6(3) . . . . ? O10 Eu1 O7 N3 -178.5(2) . . . . ? O15 Eu1 O7 N3 -90.7(2) . . . . ? O1 Eu1 O7 N3 130.9(2) . . . . ? O4 Eu1 O7 N3 95.6(2) . . . . ? O8 Eu1 O7 N3 1.2(2) . . . . ? O5 Eu1 O7 N3 56.1(2) . . . . ? O2 Eu1 O7 N3 -142.0(2) . . . . ? O9 N3 O8 Eu1 -175.1(3) . . . . ? O7 N3 O8 Eu1 2.0(3) . . . . ? O18 Eu1 O8 N3 158.0(2) . . . . ? O10 Eu1 O8 N3 -0.8(3) . . . . ? O15 Eu1 O8 N3 76.6(2) . . . . ? O1 Eu1 O8 N3 -125.0(3) . . . . ? O4 Eu1 O8 N3 -74.9(2) . . . . ? O7 Eu1 O8 N3 -1.2(2) . . . . ? O5 Eu1 O8 N3 -126.4(2) . . . . ? O2 Eu1 O8 N3 132.2(3) . . . . ? N4 C7 O10 Eu1 -87.4(8) . . . . ? C1 C7 O10 Eu1 94.8(7) . . . . ? O18 Eu1 O10 C7 -106.2(7) . . . . ? O15 Eu1 O10 C7 -50.0(7) . . . . ? O1 Eu1 O10 C7 176.6(7) . . . . ? O4 Eu1 O10 C7 101.4(7) . . . . ? O7 Eu1 O10 C7 27.0(7) . . . . ? O8 Eu1 O10 C7 26.7(8) . . . . ? O5 Eu1 O10 C7 124.1(7) . . . . ? O2 Eu1 O10 C7 -132.0(7) . . . . ? C3 C2 O11 C15 -0.3(6) . . . . ? C1 C2 O11 C15 -179.9(3) . . . . ? C16 C15 O11 C2 -178.5(4) . . . . ? C18 C17 O12 C16 178.5(4) . . . . ? C15 C16 O12 C17 -175.5(4) . . . . ? C20 C19 O13 C18 -176.8(4) . . . . ? C17 C18 O13 C19 175.9(4) . . . . ? C22 C21 O14 C20 -6.2(4) . . . . ? C26 C21 O14 C20 175.6(3) . . . . ? C19 C20 O14 C21 175.8(3) . . . . ? N5 C33 O15 Eu1 129.8(14) . . . . ? C27 C33 O15 Eu1 -53.0(17) . . . . ? O18 Eu1 O15 C33 117.7(16) . . . . ? O10 Eu1 O15 C33 -38.4(16) . . . . ? O1 Eu1 O15 C33 32.6(16) . . . . ? O4 Eu1 O15 C33 -101.4(16) . . . . ? O7 Eu1 O15 C33 -112.9(16) . . . . ? O8 Eu1 O15 C33 -164.3(16) . . . . ? O5 Eu1 O15 C33 150.5(15) . . . . ? O2 Eu1 O15 C33 39.5(16) . . . . ? C29 C28 O16 C41 8.9(7) . . . . ? C27 C28 O16 C41 -167.4(5) . . . . ? C42 C41 O16 C28 154.6(5) . . . . ? C41 C42 O17 C43 178.3(4) . . . . ? C43 C43 O17 C42 178.2(5) 2_565 . . . ? N6 C44 O18 Eu1 101(2) . . . . ? C26 C44 O18 Eu1 -80(3) 1_556 . . . ? O10 Eu1 O18 C44 168(2) . . . . ? O15 Eu1 O18 C44 111(2) . . . . ? O1 Eu1 O18 C44 -118(2) . . . . ? O4 Eu1 O18 C44 -45(2) . . . . ? O7 Eu1 O18 C44 46(2) . . . . ? O8 Eu1 O18 C44 27(2) . . . . ? O5 Eu1 O18 C44 -51(2) . . . . ? O2 Eu1 O18 C44 -166(2) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.316 _refine_diff_density_min -0.443 _refine_diff_density_rms 0.063 #===END data_compound11 _database_code_depnum_ccdc_archive 'CCDC 817228' #TrackingRef '- 1-12.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H54 N6 O18 Tb' _chemical_formula_weight 1197.94 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' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.4447(7) _cell_length_b 15.9902(11) _cell_length_c 17.5724(12) _cell_angle_alpha 78.616(3) _cell_angle_beta 87.019(3) _cell_angle_gamma 76.896(3) _cell_volume 3070.4(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6609 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 24.17 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.296 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1354 _exptl_absorpt_coefficient_mu 1.230 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.771 _exptl_absorpt_correction_T_max 0.782 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 16705 _diffrn_reflns_av_R_equivalents 0.0187 _diffrn_reflns_av_sigmaI/netI 0.0404 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 25.50 _reflns_number_total 11282 _reflns_number_gt 9338 _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. Diffuse electron densities resulting from disorder residual solvent moleculeswere removed from the data set using the SQUEEZE routine of PLATON andrefined further using the data generated. ; _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^)+(0.0353P)^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 11282 _refine_ls_number_parameters 673 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0427 _refine_ls_R_factor_gt 0.0325 _refine_ls_wR_factor_ref 0.0731 _refine_ls_wR_factor_gt 0.0703 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _refine_ls_shift/su_max 0.004 _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 C29 C 0.46446(7) 0.36353(5) 0.03342(4) 0.0764(4) Uani 1 1 d G . . C30 C 0.43535(10) 0.43562(5) 0.06942(5) 0.1070(6) Uani 1 1 d G . . H30 H 0.3600 0.4730 0.0623 0.128 Uiso 1 1 calc R . . C31 C 0.51890(14) 0.45186(8) 0.11609(6) 0.1414(7) Uani 1 1 d G . . H31 H 0.4994 0.5001 0.1402 0.170 Uiso 1 1 calc R . . C32 C 0.63155(12) 0.39599(11) 0.12675(7) 0.1677(8) Uani 1 1 d G . . H32 H 0.6874 0.4069 0.1580 0.201 Uiso 1 1 calc R . . C33 C 0.66066(8) 0.32390(10) 0.09075(7) 0.1616(10) Uani 1 1 d G . . H33 H 0.7360 0.2865 0.0979 0.194 Uiso 1 1 calc R . . C34 C 0.57711(8) 0.30766(6) 0.04409(5) 0.1140(7) Uani 1 1 d G . . H34 H 0.5966 0.2594 0.0200 0.137 Uiso 1 1 calc R . . Tb1 Tb 0.340701(5) 0.300065(3) -0.251707(3) 0.04838(2) Uani 1 1 d . . . C1 C 0.51394(16) 0.27384(9) 0.46764(8) 0.0955(6) Uani 1 1 d . . . H1 H 0.4778 0.2400 0.5069 0.115 Uiso 1 1 calc R . . C2 C 0.60144(19) 0.23427(12) 0.42277(10) 0.1367(8) Uani 1 1 d . . . H2 H 0.6253 0.1736 0.4321 0.164 Uiso 1 1 calc R . . C3 C 0.65350(16) 0.28195(17) 0.36526(11) 0.1677(10) Uani 1 1 d . . . H3 H 0.7123 0.2543 0.3344 0.201 Uiso 1 1 calc R . . C4 C 0.62098(18) 0.36873(14) 0.35242(11) 0.1631(8) Uani 1 1 d . . . H4 H 0.6578 0.4019 0.3130 0.196 Uiso 1 1 calc R . . C5 C 0.53429(15) 0.40891(10) 0.39680(8) 0.0984(6) Uani 1 1 d . . . H5 H 0.5120 0.4697 0.3869 0.118 Uiso 1 1 calc R . . C6 C 0.47898(10) 0.36283(8) 0.45533(7) 0.0576(4) Uani 1 1 d . . . C7 C 0.39191(12) 0.40831(9) 0.50726(9) 0.0819(5) Uani 1 1 d . . . H7A H 0.4214 0.3892 0.5600 0.098 Uiso 1 1 calc R . . H7B H 0.3881 0.4706 0.4928 0.098 Uiso 1 1 calc R . . C8 C 0.20221(10) 0.38092(7) 0.56717(6) 0.0520(3) Uani 1 1 d . . . C9 C 0.07382(10) 0.37882(6) 0.55831(6) 0.0494(3) Uani 1 1 d . . . C10 C 0.00648(11) 0.36721(7) 0.62617(7) 0.0606(4) Uani 1 1 d . . . H10 H 0.0432 0.3609 0.6736 0.073 Uiso 1 1 calc R . . C11 C -0.11270(12) 0.36477(8) 0.62537(8) 0.0724(5) Uani 1 1 d . . . H11 H -0.1560 0.3572 0.6715 0.087 Uiso 1 1 calc R . . C12 C -0.16674(12) 0.37371(8) 0.55557(9) 0.0781(5) Uani 1 1 d . . . H12 H -0.2470 0.3710 0.5546 0.094 Uiso 1 1 calc R . . C13 C -0.10404(11) 0.38662(8) 0.48696(8) 0.0708(4) Uani 1 1 d . . . H13 H -0.1423 0.3934 0.4400 0.085 Uiso 1 1 calc R . . C14 C 0.01548(11) 0.38949(7) 0.48763(7) 0.0554(4) Uani 1 1 d . . . C15 C 0.02822(13) 0.41390(9) 0.34753(7) 0.0770(5) Uani 1 1 d . . . H15A H -0.0381 0.4646 0.3399 0.092 Uiso 1 1 calc R . . H15B H -0.0018 0.3628 0.3438 0.092 Uiso 1 1 calc R . . C16 C 0.12352(14) 0.42610(9) 0.28824(8) 0.0840(5) Uani 1 1 d . . . H16A H 0.0893 0.4417 0.2366 0.101 Uiso 1 1 calc R . . H16B H 0.1600 0.4728 0.2963 0.101 Uiso 1 1 calc R . . C17 C 0.30700(14) 0.35561(9) 0.24351(8) 0.0872(5) Uani 1 1 d . . . H17A H 0.3420 0.4026 0.2527 0.105 Uiso 1 1 calc R . . H17B H 0.2780 0.3704 0.1906 0.105 Uiso 1 1 calc R . . C18 C 0.39986(13) 0.27257(9) 0.25402(8) 0.0798(5) Uani 1 1 d . . . H18A H 0.4742 0.2834 0.2294 0.096 Uiso 1 1 calc R . . H18B H 0.4149 0.2503 0.3089 0.096 Uiso 1 1 calc R . . C19 C 0.44889(13) 0.13148(9) 0.22534(7) 0.0785(5) Uani 1 1 d . . . H19A H 0.4648 0.1043 0.2793 0.094 Uiso 1 1 calc R . . H19B H 0.5228 0.1443 0.2016 0.094 Uiso 1 1 calc R . . C20 C 0.40662(14) 0.07057(8) 0.18458(7) 0.0768(5) Uani 1 1 d . . . H20A H 0.4646 0.0152 0.1899 0.092 Uiso 1 1 calc R . . H20B H 0.3305 0.0597 0.2061 0.092 Uiso 1 1 calc R . . C21 C 0.36215(11) 0.07001(7) 0.05133(7) 0.0590(4) Uani 1 1 d . . . C22 C 0.35368(13) -0.01687(8) 0.06977(8) 0.0751(5) Uani 1 1 d . . . H22 H 0.3674 -0.0481 0.1202 0.090 Uiso 1 1 calc R . . C23 C 0.32459(13) -0.05651(8) 0.01241(9) 0.0841(5) Uani 1 1 d . . . H23 H 0.3178 -0.1145 0.0250 0.101 Uiso 1 1 calc R . . C24 C 0.30570(13) -0.01264(8) -0.06172(8) 0.0760(5) Uani 1 1 d . . . H24 H 0.2874 -0.0405 -0.0998 0.091 Uiso 1 1 calc R . . C25 C 0.31390(11) 0.07364(8) -0.07995(7) 0.0632(4) Uani 1 1 d . . . H25 H 0.3005 0.1038 -0.1308 0.076 Uiso 1 1 calc R . . C26 C 0.34165(10) 0.11696(7) -0.02443(6) 0.0507(3) Uani 1 1 d . . . C27 C 0.34828(10) 0.20996(7) -0.05129(6) 0.0534(3) Uani 1 1 d . . . C28 C 0.37785(14) 0.34752(8) -0.01981(8) 0.0821(5) Uani 1 1 d . . . H28A H 0.3005 0.3867 -0.0159 0.098 Uiso 1 1 calc R . . H28B H 0.4063 0.3595 -0.0730 0.098 Uiso 1 1 calc R . . C35 C 0.33498(15) 0.02248(10) -0.44846(10) 0.1056(6) Uani 1 1 d . . . H35 H 0.3806 -0.0294 -0.4211 0.127 Uiso 1 1 calc R . . C36 C 0.34156(17) 0.04010(12) -0.52841(11) 0.1273(7) Uani 1 1 d . . . H36 H 0.3907 -0.0001 -0.5545 0.153 Uiso 1 1 calc R . . C37 C 0.27643(16) 0.11604(12) -0.56919(10) 0.1164(7) Uani 1 1 d . . . H37 H 0.2807 0.1289 -0.6231 0.140 Uiso 1 1 calc R . . C38 C 0.2053(2) 0.17240(11) -0.52928(10) 0.1262(9) Uani 1 1 d . . . H38 H 0.1601 0.2247 -0.5563 0.151 Uiso 1 1 calc R . . C39 C 0.19828(17) 0.15444(9) -0.45078(9) 0.1000(6) Uani 1 1 d . . . H39 H 0.1479 0.1944 -0.4251 0.120 Uiso 1 1 calc R . . C40 C 0.26302(11) 0.07956(7) -0.40899(8) 0.0678(4) Uani 1 1 d . . . C41 C 0.26076(11) 0.05824(8) -0.32169(8) 0.0739(5) Uani 1 1 d . . . H41A H 0.2755 -0.0048 -0.3050 0.089 Uiso 1 1 calc R . . H41B H 0.3256 0.0779 -0.3023 0.089 Uiso 1 1 calc R . . C42 C 0.13138(10) 0.16623(7) -0.25396(6) 0.0513(3) Uani 1 1 d . . . C43 C 0.01309(10) 0.19353(7) -0.21567(6) 0.0533(4) Uani 1 1 d . . . C44 C 0.00942(13) 0.23778(9) -0.15564(8) 0.0808(5) Uani 1 1 d . . . H44 H 0.0796 0.2499 -0.1406 0.097 Uiso 1 1 calc R . . C45 C -0.09634(15) 0.26444(12) -0.11741(9) 0.1035(6) Uani 1 1 d . . . H45 H -0.0980 0.2951 -0.0774 0.124 Uiso 1 1 calc R . . C46 C -0.19901(14) 0.24523(10) -0.13890(8) 0.0903(6) Uani 1 1 d . . . H46 H -0.2705 0.2627 -0.1128 0.108 Uiso 1 1 calc R . . C47 C -0.19848(12) 0.20134(9) -0.19736(8) 0.0742(5) Uani 1 1 d . . . H47 H -0.2690 0.1884 -0.2109 0.089 Uiso 1 1 calc R . . C48 C -0.09309(11) 0.17577(8) -0.23697(7) 0.0608(4) Uani 1 1 d . . . C49 C -0.19171(12) 0.13253(10) -0.33638(9) 0.0976(5) Uani 1 1 d . . . H49A H -0.2535 0.1847 -0.3342 0.117 Uiso 1 1 calc R . . H49B H -0.2217 0.0820 -0.3107 0.117 Uiso 1 1 calc R . . C50 C -0.15940(15) 0.12612(11) -0.41811(10) 0.1105(6) Uani 1 1 d . . . H50A H -0.2309 0.1278 -0.4462 0.133 Uiso 1 1 calc R . . H50B H -0.1266 0.1758 -0.4425 0.133 Uiso 1 1 calc R . . C51 C -0.04439(15) 0.04110(9) -0.49982(9) 0.0950(6) Uani 1 1 d . . . H51A H -0.0112 0.0902 -0.5253 0.114 Uiso 1 1 calc R . . H51B H -0.1154 0.0414 -0.5278 0.114 Uiso 1 1 calc R . . N1 N 0.27023(9) 0.39352(7) 0.50564(6) 0.0669(3) Uani 1 1 d . . . H1A H 0.2418 0.3931 0.4614 0.080 Uiso 1 1 calc R . . N2 N 0.36463(10) 0.25646(6) 0.00025(6) 0.0698(4) Uani 1 1 d . . . H2A H 0.3677 0.2318 0.0485 0.084 Uiso 1 1 calc R . . N3 N 0.14870(9) 0.09749(6) -0.28729(6) 0.0687(3) Uani 1 1 d . . . H3A H 0.0886 0.0739 -0.2888 0.082 Uiso 1 1 calc R . . N4 N 0.49531(8) 0.15489(6) -0.30934(6) 0.0569(3) Uani 1 1 d . . . N5 N 0.55487(9) 0.36875(6) -0.25628(6) 0.0674(3) Uani 1 1 d . . . N6 N 0.19508(10) 0.45658(7) -0.20858(6) 0.0786(4) Uani 1 1 d . . . O1 O 0.24257(7) 0.37284(5) 0.63365(4) 0.0644(3) Uani 1 1 d . . . O2 O 0.08182(8) 0.40277(5) 0.42160(4) 0.0671(3) Uani 1 1 d . . . O3 O 0.21060(9) 0.34708(6) 0.29539(5) 0.0758(3) Uani 1 1 d . . . O4 O 0.36080(8) 0.20924(6) 0.22070(5) 0.0717(3) Uani 1 1 d . . . O5 O 0.39351(9) 0.11258(5) 0.10455(4) 0.0709(3) Uani 1 1 d . . . O6 O 0.33673(8) 0.24389(5) -0.12114(4) 0.0655(3) Uani 1 1 d . . . O7 O 0.21281(7) 0.20541(5) -0.25032(4) 0.0573(2) Uani 1 1 d . . . O8 O -0.08593(8) 0.13621(6) -0.29953(6) 0.0939(3) Uani 1 1 d . . . O9 O -0.07515(9) 0.04871(6) -0.42235(6) 0.0919(4) Uani 1 1 d . . . O10 O 0.49732(8) 0.16243(5) -0.23910(5) 0.0666(3) Uani 1 1 d . . . O11 O 0.55555(8) 0.09210(6) -0.33306(5) 0.0796(3) Uani 1 1 d . . . O12 O 0.42424(8) 0.21509(5) -0.35258(4) 0.0629(3) Uani 1 1 d . . . O13 O 0.50419(8) 0.36306(6) -0.31716(5) 0.0776(3) Uani 1 1 d . . . O14 O 0.63391(8) 0.40831(6) -0.25952(7) 0.0952(4) Uani 1 1 d . . . O15 O 0.51740(7) 0.33001(6) -0.19342(5) 0.0738(3) Uani 1 1 d . . . O16 O 0.30126(8) 0.44982(6) -0.23128(6) 0.0921(4) Uani 1 1 d . . . O17 O 0.13700(10) 0.52374(6) -0.19227(7) 0.1266(4) Uani 1 1 d . . . O18 O 0.15294(8) 0.39045(6) -0.20563(5) 0.0764(3) 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 C29 0.1221(10) 0.0771(7) 0.0469(6) -0.0209(5) 0.0129(7) -0.0520(6) C30 0.1994(15) 0.0829(8) 0.0605(8) -0.0234(6) 0.0285(10) -0.0743(8) C31 0.2730(17) 0.1317(9) 0.0657(9) -0.0238(8) 0.0093(11) -0.1379(9) C32 0.2524(16) 0.2181(14) 0.0887(12) -0.0218(11) -0.0158(12) -0.1705(11) C33 0.1213(13) 0.228(2) 0.1552(18) -0.0304(16) -0.0218(14) -0.0793(13) C34 0.1051(11) 0.1467(12) 0.1093(12) -0.0495(10) 0.0046(10) -0.0461(10) Tb1 0.04680(3) 0.05267(3) 0.04841(3) -0.01301(2) -0.00979(2) -0.01163(2) C1 0.1387(14) 0.0734(9) 0.0607(8) 0.0015(7) -0.0049(9) -0.0069(9) C2 0.1578(16) 0.1201(12) 0.1070(11) -0.0495(10) -0.0491(11) 0.0558(12) C3 0.0654(10) 0.339(2) 0.1298(13) -0.1236(13) 0.0101(10) -0.0420(13) C4 0.1884(13) 0.2677(17) 0.0957(12) -0.0646(12) 0.0621(11) -0.1667(11) C5 0.1395(12) 0.1034(9) 0.0660(9) -0.0046(8) 0.0070(9) -0.0666(8) C6 0.0546(6) 0.0678(7) 0.0496(6) 0.0008(6) -0.0103(5) -0.0198(5) C7 0.0675(8) 0.0969(8) 0.0928(9) -0.0333(7) -0.0031(7) -0.0285(7) C8 0.0571(7) 0.0442(5) 0.0524(6) -0.0149(5) -0.0116(5) 0.0009(5) C9 0.0548(6) 0.0373(5) 0.0521(6) -0.0087(5) -0.0056(5) -0.0007(5) C10 0.0617(7) 0.0504(6) 0.0621(7) -0.0073(6) -0.0060(6) 0.0013(6) C11 0.0680(8) 0.0586(7) 0.0794(9) -0.0032(7) 0.0060(7) -0.0009(7) C12 0.0521(7) 0.0675(7) 0.1101(11) -0.0123(8) -0.0042(8) -0.0066(6) C13 0.0635(7) 0.0664(7) 0.0806(8) -0.0151(6) -0.0216(7) -0.0051(6) C14 0.0570(7) 0.0508(6) 0.0574(6) -0.0143(5) -0.0087(6) -0.0048(5) C15 0.0819(9) 0.0874(8) 0.0572(7) -0.0209(6) -0.0241(6) 0.0018(7) C16 0.1027(11) 0.0873(9) 0.0552(7) -0.0190(7) -0.0122(8) 0.0000(8) C17 0.1108(11) 0.0818(8) 0.0760(9) -0.0245(7) 0.0144(9) -0.0308(8) C18 0.0858(9) 0.1028(9) 0.0614(7) -0.0269(7) 0.0015(7) -0.0332(7) C19 0.0886(10) 0.0929(9) 0.0453(7) -0.0112(7) -0.0124(7) -0.0012(8) C20 0.1005(10) 0.0713(8) 0.0460(7) 0.0003(6) 0.0000(7) -0.0033(8) C21 0.0590(7) 0.0574(6) 0.0616(7) -0.0161(5) 0.0039(6) -0.0115(6) C22 0.0968(10) 0.0569(7) 0.0683(8) -0.0079(6) 0.0104(8) -0.0161(7) C23 0.0971(10) 0.0561(7) 0.1034(11) -0.0203(7) 0.0124(9) -0.0244(7) C24 0.0899(9) 0.0706(7) 0.0819(8) -0.0298(6) 0.0049(7) -0.0357(6) C25 0.0627(7) 0.0714(7) 0.0616(7) -0.0155(6) -0.0085(6) -0.0230(6) C26 0.0475(6) 0.0548(6) 0.0520(6) -0.0124(5) -0.0031(5) -0.0132(5) C27 0.0517(6) 0.0601(6) 0.0523(6) -0.0135(5) -0.0084(5) -0.0161(5) C28 0.1240(11) 0.0585(7) 0.0696(8) -0.0110(6) -0.0162(8) -0.0300(7) C35 0.0899(11) 0.1100(10) 0.1197(11) -0.0601(8) 0.0064(10) 0.0031(9) C36 0.0946(12) 0.1662(14) 0.1390(13) -0.0891(10) 0.0224(11) -0.0188(11) C37 0.1201(12) 0.1564(13) 0.0952(11) -0.0406(10) 0.0203(10) -0.0668(10) C38 0.1896(19) 0.0862(10) 0.1019(12) -0.0217(9) -0.0014(13) -0.0251(12) C39 0.1380(14) 0.0670(8) 0.0930(10) -0.0306(7) 0.0125(10) -0.0082(9) C40 0.0524(6) 0.0612(6) 0.1036(9) -0.0405(6) 0.0070(7) -0.0214(5) C41 0.0556(7) 0.0658(7) 0.1066(10) -0.0335(7) 0.0050(7) -0.0130(6) C42 0.0510(6) 0.0575(6) 0.0476(6) -0.0086(5) -0.0085(5) -0.0158(5) C43 0.0526(6) 0.0568(6) 0.0511(6) -0.0089(5) -0.0040(5) -0.0139(5) C44 0.0662(8) 0.1199(9) 0.0682(8) -0.0390(7) 0.0075(7) -0.0283(7) C45 0.0889(10) 0.1562(12) 0.0794(8) -0.0608(8) 0.0154(8) -0.0263(10) C46 0.0695(9) 0.1218(11) 0.0741(9) -0.0209(9) 0.0173(8) -0.0118(9) C47 0.0524(7) 0.0812(8) 0.0857(9) -0.0054(7) 0.0002(7) -0.0178(6) C48 0.0529(7) 0.0640(7) 0.0643(7) -0.0092(6) -0.0023(6) -0.0128(6) C49 0.0572(8) 0.1260(10) 0.1260(11) -0.0576(8) -0.0175(8) -0.0210(7) C50 0.0903(11) 0.1229(11) 0.1258(11) -0.0524(9) -0.0338(9) -0.0069(9) C51 0.0906(10) 0.1013(9) 0.1051(10) -0.0410(8) -0.0083(9) -0.0255(8) N1 0.0580(6) 0.0894(6) 0.0576(5) -0.0231(5) -0.0054(5) -0.0162(5) N2 0.1074(8) 0.0577(5) 0.0499(5) -0.0097(4) -0.0174(5) -0.0262(5) N3 0.0527(5) 0.0711(5) 0.0963(7) -0.0356(5) 0.0082(5) -0.0276(4) N4 0.0446(5) 0.0613(5) 0.0696(6) -0.0205(5) 0.0074(5) -0.0163(4) N5 0.0468(5) 0.0646(5) 0.0957(7) -0.0265(5) -0.0076(5) -0.0115(4) N6 0.0671(6) 0.0798(6) 0.0931(6) -0.0465(5) -0.0317(5) 0.0083(5) O1 0.0652(5) 0.0685(5) 0.0545(4) -0.0080(4) -0.0176(4) -0.0038(4) O2 0.0685(5) 0.0824(5) 0.0505(4) -0.0167(4) -0.0147(4) -0.0104(4) O3 0.0893(6) 0.0761(5) 0.0599(5) -0.0166(4) 0.0060(5) -0.0122(5) O4 0.0741(5) 0.0797(5) 0.0612(5) -0.0210(4) -0.0102(4) -0.0082(4) O5 0.1067(6) 0.0614(4) 0.0447(4) -0.0086(4) -0.0088(4) -0.0183(4) O6 0.0880(5) 0.0693(4) 0.0462(4) -0.0080(4) -0.0145(4) -0.0309(4) O7 0.0497(4) 0.0723(4) 0.0592(4) -0.0216(3) -0.0044(3) -0.0238(3) O8 0.0476(4) 0.1302(6) 0.1266(6) -0.0733(5) -0.0096(5) -0.0222(4) O9 0.0846(6) 0.0939(5) 0.1097(7) -0.0437(5) -0.0129(6) -0.0220(5) O10 0.0684(5) 0.0670(5) 0.0611(5) -0.0182(4) -0.0146(4) 0.0002(4) O11 0.0578(5) 0.0818(5) 0.1035(6) -0.0452(4) 0.0076(5) -0.0025(4) O12 0.0707(5) 0.0648(4) 0.0501(4) -0.0099(4) -0.0014(4) -0.0098(4) O13 0.0726(5) 0.0953(5) 0.0744(5) -0.0175(5) -0.0083(5) -0.0349(4) O14 0.0611(5) 0.0937(6) 0.1422(8) -0.0252(6) -0.0106(6) -0.0362(4) O15 0.0568(5) 0.0945(5) 0.0752(5) -0.0191(4) -0.0113(4) -0.0224(4) O16 0.0661(5) 0.0722(5) 0.1485(8) -0.0469(5) -0.0125(6) -0.0119(4) O17 0.0905(7) 0.1054(6) 0.1943(9) -0.0953(5) -0.0408(7) 0.0237(6) O18 0.0724(5) 0.0821(5) 0.0812(5) -0.0344(4) 0.0004(5) -0.0140(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 C29 C30 1.3900 . ? C29 C34 1.3900 . ? C29 C28 1.4930(17) . ? C30 C31 1.3900 . ? C30 H30 0.9300 . ? C31 C32 1.3900 . ? C31 H31 0.9300 . ? C32 C33 1.3900 . ? C32 H32 0.9300 . ? C33 C34 1.3900 . ? C33 H33 0.9300 . ? C34 H34 0.9300 . ? Tb1 O6 2.2950(7) . ? Tb1 O1 2.3218(7) 1_554 ? Tb1 O7 2.3281(8) . ? Tb1 O16 2.4289(9) . ? Tb1 O13 2.4520(9) . ? Tb1 O12 2.4673(8) . ? Tb1 O10 2.4831(8) . ? Tb1 O15 2.4932(9) . ? Tb1 O18 2.4970(9) . ? C1 C2 1.361(2) . ? C1 C6 1.3642(18) . ? C1 H1 0.9300 . ? C2 C3 1.340(3) . ? C2 H2 0.9300 . ? C3 C4 1.329(3) . ? C3 H3 0.9300 . ? C4 C5 1.354(2) . ? C4 H4 0.9300 . ? C5 C6 1.3587(19) . ? C5 H5 0.9300 . ? C6 C7 1.4810(18) . ? C7 N1 1.4670(18) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 O1 1.2506(14) . ? C8 N1 1.3089(15) . ? C8 C9 1.4943(17) . ? C9 C10 1.3901(16) . ? C9 C14 1.4030(16) . ? C10 C11 1.3742(19) . ? C10 H10 0.9300 . ? C11 C12 1.370(2) . ? C11 H11 0.9300 . ? C12 C13 1.375(2) . ? C12 H12 0.9300 . ? C13 C14 1.3798(18) . ? C13 H13 0.9300 . ? C14 O2 1.3608(14) . ? C15 O2 1.4297(15) . ? C15 C16 1.487(2) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 O3 1.4088(16) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 O3 1.4077(18) . ? C17 C18 1.4868(19) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 O4 1.4264(18) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 O4 1.4032(15) . ? C19 C20 1.490(2) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 O5 1.4334(13) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 O5 1.3653(16) . ? C21 C22 1.3872(17) . ? C21 C26 1.3961(15) . ? C22 C23 1.383(2) . ? C22 H22 0.9300 . ? C23 C24 1.3548(19) . ? C23 H23 0.9300 . ? C24 C25 1.3770(18) . ? C24 H24 0.9300 . ? C25 C26 1.3897(18) . ? C25 H25 0.9300 . ? C26 C27 1.4867(15) . ? C27 O6 1.2409(13) . ? C27 N2 1.3247(16) . ? C28 N2 1.4693(16) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C35 C40 1.357(2) . ? C35 C36 1.379(2) . ? C35 H35 0.9300 . ? C36 C37 1.358(2) . ? C36 H36 0.9300 . ? C37 C38 1.351(3) . ? C37 H37 0.9300 . ? C38 C39 1.354(2) . ? C38 H38 0.9300 . ? C39 C40 1.3525(17) . ? C39 H39 0.9300 . ? C40 C41 1.5046(19) . ? C41 N3 1.4520(16) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 O7 1.2457(15) . ? C42 N3 1.3168(16) . ? C42 C43 1.4930(16) . ? C43 C44 1.3755(19) . ? C43 C48 1.3939(18) . ? C44 C45 1.376(2) . ? C44 H44 0.9300 . ? C45 C46 1.369(2) . ? C45 H45 0.9300 . ? C46 C47 1.353(2) . ? C46 H46 0.9300 . ? C47 C48 1.3813(18) . ? C47 H47 0.9300 . ? C48 O8 1.3626(17) . ? C49 O8 1.4204(18) . ? C49 C50 1.482(2) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 O9 1.3982(18) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C51 O9 1.4100(19) . ? C51 C51 1.469(3) 2_554 ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? N1 H1A 0.8600 . ? N2 H2A 0.8600 . ? N3 H3A 0.8600 . ? N4 O11 1.2159(12) . ? N4 O12 1.2594(11) . ? N4 O10 1.2655(13) . ? N5 O14 1.2088(14) . ? N5 O15 1.2604(13) . ? N5 O13 1.2713(15) . ? N6 O17 1.2064(14) . ? N6 O16 1.2468(14) . ? N6 O18 1.2492(15) . ? O1 Tb1 2.3218(7) 1_556 ? 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 C30 C29 C34 120.0 . . ? C30 C29 C28 120.64(7) . . ? C34 C29 C28 119.30(7) . . ? C29 C30 C31 120.0 . . ? C29 C30 H30 120.0 . . ? C31 C30 H30 120.0 . . ? C30 C31 C32 120.0 . . ? C30 C31 H31 120.0 . . ? C32 C31 H31 120.0 . . ? C31 C32 C33 120.0 . . ? C31 C32 H32 120.0 . . ? C33 C32 H32 120.0 . . ? C34 C33 C32 120.0 . . ? C34 C33 H33 120.0 . . ? C32 C33 H33 120.0 . . ? C33 C34 C29 120.0 . . ? C33 C34 H34 120.0 . . ? C29 C34 H34 120.0 . . ? O6 Tb1 O1 150.65(3) . 1_554 ? O6 Tb1 O7 79.96(3) . . ? O1 Tb1 O7 83.71(3) 1_554 . ? O6 Tb1 O16 92.81(3) . . ? O1 Tb1 O16 79.81(3) 1_554 . ? O7 Tb1 O16 131.11(3) . . ? O6 Tb1 O13 123.85(3) . . ? O1 Tb1 O13 81.60(3) 1_554 . ? O7 Tb1 O13 147.78(3) . . ? O16 Tb1 O13 73.84(3) . . ? O6 Tb1 O12 125.07(3) . . ? O1 Tb1 O12 73.25(3) 1_554 . ? O7 Tb1 O12 75.94(3) . . ? O16 Tb1 O12 139.22(3) . . ? O13 Tb1 O12 72.42(3) . . ? O6 Tb1 O10 77.44(3) . . ? O1 Tb1 O10 124.46(3) 1_554 . ? O7 Tb1 O10 82.68(3) . . ? O16 Tb1 O10 143.12(3) . . ? O13 Tb1 O10 82.30(3) . . ? O12 Tb1 O10 51.20(3) . . ? O6 Tb1 O15 72.87(3) . . ? O1 Tb1 O15 128.36(3) 1_554 . ? O7 Tb1 O15 147.43(3) . . ? O16 Tb1 O15 68.88(3) . . ? O13 Tb1 O15 51.24(3) . . ? O12 Tb1 O15 105.36(3) . . ? O10 Tb1 O15 74.27(3) . . ? O6 Tb1 O18 76.55(3) . . ? O1 Tb1 O18 76.86(3) 1_554 . ? O7 Tb1 O18 80.73(3) . . ? O16 Tb1 O18 50.80(3) . . ? O13 Tb1 O18 122.99(3) . . ? O12 Tb1 O18 143.66(3) . . ? O10 Tb1 O18 151.17(3) . . ? O15 Tb1 O18 109.28(3) . . ? C2 C1 C6 120.39(15) . . ? C2 C1 H1 119.8 . . ? C6 C1 H1 119.8 . . ? C3 C2 C1 120.61(18) . . ? C3 C2 H2 119.7 . . ? C1 C2 H2 119.7 . . ? C4 C3 C2 119.95(19) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C4 C5 120.01(18) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C4 C5 C6 121.77(15) . . ? C4 C5 H5 119.1 . . ? C6 C5 H5 119.1 . . ? C5 C6 C1 117.26(13) . . ? C5 C6 C7 120.69(12) . . ? C1 C6 C7 121.86(12) . . ? N1 C7 C6 114.54(12) . . ? N1 C7 H7A 108.6 . . ? C6 C7 H7A 108.6 . . ? N1 C7 H7B 108.6 . . ? C6 C7 H7B 108.6 . . ? H7A C7 H7B 107.6 . . ? O1 C8 N1 120.71(11) . . ? O1 C8 C9 119.27(10) . . ? N1 C8 C9 120.00(10) . . ? C10 C9 C14 117.67(11) . . ? C10 C9 C8 116.71(10) . . ? C14 C9 C8 125.60(10) . . ? C11 C10 C9 122.03(12) . . ? C11 C10 H10 119.0 . . ? C9 C10 H10 119.0 . . ? C12 C11 C10 119.00(13) . . ? C12 C11 H11 120.5 . . ? C10 C11 H11 120.5 . . ? C11 C12 C13 120.93(13) . . ? C11 C12 H12 119.5 . . ? C13 C12 H12 119.5 . . ? C12 C13 C14 120.15(13) . . ? C12 C13 H13 119.9 . . ? C14 C13 H13 119.9 . . ? O2 C14 C13 122.77(11) . . ? O2 C14 C9 117.03(11) . . ? C13 C14 C9 120.20(11) . . ? O2 C15 C16 106.71(12) . . ? O2 C15 H15A 110.4 . . ? C16 C15 H15A 110.4 . . ? O2 C15 H15B 110.4 . . ? C16 C15 H15B 110.4 . . ? H15A C15 H15B 108.6 . . ? O3 C16 C15 108.34(11) . . ? O3 C16 H16A 110.0 . . ? C15 C16 H16A 110.0 . . ? O3 C16 H16B 110.0 . . ? C15 C16 H16B 110.0 . . ? H16A C16 H16B 108.4 . . ? O3 C17 C18 110.35(11) . . ? O3 C17 H17A 109.6 . . ? C18 C17 H17A 109.6 . . ? O3 C17 H17B 109.6 . . ? C18 C17 H17B 109.6 . . ? H17A C17 H17B 108.1 . . ? O4 C18 C17 110.19(12) . . ? O4 C18 H18A 109.6 . . ? C17 C18 H18A 109.6 . . ? O4 C18 H18B 109.6 . . ? C17 C18 H18B 109.6 . . ? H18A C18 H18B 108.1 . . ? O4 C19 C20 109.53(12) . . ? O4 C19 H19A 109.8 . . ? C20 C19 H19A 109.8 . . ? O4 C19 H19B 109.8 . . ? C20 C19 H19B 109.8 . . ? H19A C19 H19B 108.2 . . ? O5 C20 C19 106.35(10) . . ? O5 C20 H20A 110.5 . . ? C19 C20 H20A 110.5 . . ? O5 C20 H20B 110.5 . . ? C19 C20 H20B 110.5 . . ? H20A C20 H20B 108.7 . . ? O5 C21 C22 122.48(11) . . ? O5 C21 C26 117.15(10) . . ? C22 C21 C26 120.35(12) . . ? C23 C22 C21 119.36(12) . . ? C23 C22 H22 120.3 . . ? C21 C22 H22 120.3 . . ? C24 C23 C22 121.39(13) . . ? C24 C23 H23 119.3 . . ? C22 C23 H23 119.3 . . ? C23 C24 C25 119.21(14) . . ? C23 C24 H24 120.4 . . ? C25 C24 H24 120.4 . . ? C24 C25 C26 121.80(11) . . ? C24 C25 H25 119.1 . . ? C26 C25 H25 119.1 . . ? C25 C26 C21 117.88(11) . . ? C25 C26 C27 116.77(10) . . ? C21 C26 C27 125.35(11) . . ? O6 C27 N2 120.48(10) . . ? O6 C27 C26 120.21(11) . . ? N2 C27 C26 119.30(10) . . ? N2 C28 C29 110.53(9) . . ? N2 C28 H28A 109.5 . . ? C29 C28 H28A 109.5 . . ? N2 C28 H28B 109.5 . . ? C29 C28 H28B 109.5 . . ? H28A C28 H28B 108.1 . . ? C40 C35 C36 121.14(14) . . ? C40 C35 H35 119.4 . . ? C36 C35 H35 119.4 . . ? C37 C36 C35 120.16(17) . . ? C37 C36 H36 119.9 . . ? C35 C36 H36 119.9 . . ? C38 C37 C36 118.16(17) . . ? C38 C37 H37 120.9 . . ? C36 C37 H37 120.9 . . ? C37 C38 C39 121.46(16) . . ? C37 C38 H38 119.3 . . ? C39 C38 H38 119.3 . . ? C40 C39 C38 121.37(15) . . ? C40 C39 H39 119.3 . . ? C38 C39 H39 119.3 . . ? C39 C40 C35 117.70(14) . . ? C39 C40 C41 123.11(12) . . ? C35 C40 C41 119.18(11) . . ? N3 C41 C40 113.99(10) . . ? N3 C41 H41A 108.8 . . ? C40 C41 H41A 108.8 . . ? N3 C41 H41B 108.8 . . ? C40 C41 H41B 108.8 . . ? H41A C41 H41B 107.7 . . ? O7 C42 N3 121.60(10) . . ? O7 C42 C43 119.95(11) . . ? N3 C42 C43 118.34(11) . . ? C44 C43 C48 118.48(11) . . ? C44 C43 C42 117.97(11) . . ? C48 C43 C42 123.55(11) . . ? C43 C44 C45 121.11(15) . . ? C43 C44 H44 119.4 . . ? C45 C44 H44 119.4 . . ? C46 C45 C44 119.20(16) . . ? C46 C45 H45 120.4 . . ? C44 C45 H45 120.4 . . ? C47 C46 C45 121.24(14) . . ? C47 C46 H46 119.4 . . ? C45 C46 H46 119.4 . . ? C46 C47 C48 119.90(14) . . ? C46 C47 H47 120.1 . . ? C48 C47 H47 120.1 . . ? O8 C48 C47 123.75(12) . . ? O8 C48 C43 116.13(10) . . ? C47 C48 C43 120.06(13) . . ? O8 C49 C50 107.11(12) . . ? O8 C49 H49A 110.3 . . ? C50 C49 H49A 110.3 . . ? O8 C49 H49B 110.3 . . ? C50 C49 H49B 110.3 . . ? H49A C49 H49B 108.5 . . ? O9 C50 C49 111.02(12) . . ? O9 C50 H50A 109.4 . . ? C49 C50 H50A 109.4 . . ? O9 C50 H50B 109.4 . . ? C49 C50 H50B 109.4 . . ? H50A C50 H50B 108.0 . . ? O9 C51 C51 109.02(15) . 2_554 ? O9 C51 H51A 109.9 . . ? C51 C51 H51A 109.9 2_554 . ? O9 C51 H51B 109.9 . . ? C51 C51 H51B 109.9 2_554 . ? H51A C51 H51B 108.3 . . ? C8 N1 C7 124.22(11) . . ? C8 N1 H1A 117.9 . . ? C7 N1 H1A 117.9 . . ? C27 N2 C28 124.10(10) . . ? C27 N2 H2A 118.0 . . ? C28 N2 H2A 118.0 . . ? C42 N3 C41 125.44(11) . . ? C42 N3 H3A 117.3 . . ? C41 N3 H3A 117.3 . . ? O11 N4 O12 122.07(10) . . ? O11 N4 O10 122.06(9) . . ? O12 N4 O10 115.83(9) . . ? O14 N5 O15 123.14(12) . . ? O14 N5 O13 121.56(11) . . ? O15 N5 O13 115.30(10) . . ? O17 N6 O16 121.45(12) . . ? O17 N6 O18 122.78(12) . . ? O16 N6 O18 115.75(10) . . ? C8 O1 Tb1 156.58(7) . 1_556 ? C14 O2 C15 120.03(10) . . ? C17 O3 C16 111.23(10) . . ? C19 O4 C18 112.01(10) . . ? C21 O5 C20 120.00(10) . . ? C27 O6 Tb1 172.84(8) . . ? C42 O7 Tb1 170.24(7) . . ? C48 O8 C49 120.51(10) . . ? C50 O9 C51 111.76(11) . . ? N4 O10 Tb1 96.01(5) . . ? N4 O12 Tb1 96.94(6) . . ? N5 O13 Tb1 96.98(7) . . ? N5 O15 Tb1 95.31(7) . . ? N6 O16 Tb1 98.43(7) . . ? N6 O18 Tb1 95.02(7) . . ? 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 C34 C29 C30 C31 0.0 . . . . ? C28 C29 C30 C31 -177.12(8) . . . . ? C29 C30 C31 C32 0.0 . . . . ? C30 C31 C32 C33 0.0 . . . . ? C31 C32 C33 C34 0.0 . . . . ? C32 C33 C34 C29 0.0 . . . . ? C30 C29 C34 C33 0.0 . . . . ? C28 C29 C34 C33 177.16(7) . . . . ? C6 C1 C2 C3 -0.8(3) . . . . ? C1 C2 C3 C4 1.0(3) . . . . ? C2 C3 C4 C5 -0.8(3) . . . . ? C3 C4 C5 C6 0.4(3) . . . . ? C4 C5 C6 C1 -0.3(2) . . . . ? C4 C5 C6 C7 174.76(16) . . . . ? C2 C1 C6 C5 0.5(2) . . . . ? C2 C1 C6 C7 -174.51(16) . . . . ? C5 C6 C7 N1 118.89(14) . . . . ? C1 C6 C7 N1 -66.31(17) . . . . ? O1 C8 C9 C10 -0.39(14) . . . . ? N1 C8 C9 C10 -178.53(10) . . . . ? O1 C8 C9 C14 178.09(10) . . . . ? N1 C8 C9 C14 -0.05(16) . . . . ? C14 C9 C10 C11 0.95(16) . . . . ? C8 C9 C10 C11 179.56(10) . . . . ? C9 C10 C11 C12 0.26(18) . . . . ? C10 C11 C12 C13 -1.22(19) . . . . ? C11 C12 C13 C14 0.94(19) . . . . ? C12 C13 C14 O2 -179.45(11) . . . . ? C12 C13 C14 C9 0.32(18) . . . . ? C10 C9 C14 O2 178.56(10) . . . . ? C8 C9 C14 O2 0.09(16) . . . . ? C10 C9 C14 C13 -1.23(16) . . . . ? C8 C9 C14 C13 -179.70(10) . . . . ? O2 C15 C16 O3 67.24(14) . . . . ? O3 C17 C18 O4 75.19(14) . . . . ? O4 C19 C20 O5 63.44(13) . . . . ? O5 C21 C22 C23 -178.26(12) . . . . ? C26 C21 C22 C23 -0.1(2) . . . . ? C21 C22 C23 C24 0.9(2) . . . . ? C22 C23 C24 C25 -1.0(2) . . . . ? C23 C24 C25 C26 0.3(2) . . . . ? C24 C25 C26 C21 0.44(18) . . . . ? C24 C25 C26 C27 179.81(11) . . . . ? O5 C21 C26 C25 177.72(10) . . . . ? C22 C21 C26 C25 -0.57(17) . . . . ? O5 C21 C26 C27 -1.58(17) . . . . ? C22 C21 C26 C27 -179.87(11) . . . . ? C25 C26 C27 O6 -4.39(16) . . . . ? C21 C26 C27 O6 174.92(11) . . . . ? C25 C26 C27 N2 174.50(11) . . . . ? C21 C26 C27 N2 -6.19(17) . . . . ? C30 C29 C28 N2 -131.13(8) . . . . ? C34 C29 C28 N2 51.73(12) . . . . ? C40 C35 C36 C37 0.7(3) . . . . ? C35 C36 C37 C38 -0.6(3) . . . . ? C36 C37 C38 C39 0.0(3) . . . . ? C37 C38 C39 C40 0.5(3) . . . . ? C38 C39 C40 C35 -0.4(3) . . . . ? C38 C39 C40 C41 178.12(17) . . . . ? C36 C35 C40 C39 -0.2(3) . . . . ? C36 C35 C40 C41 -178.78(16) . . . . ? C39 C40 C41 N3 28.7(2) . . . . ? C35 C40 C41 N3 -152.78(14) . . . . ? O7 C42 C43 C44 -23.04(15) . . . . ? N3 C42 C43 C44 153.23(11) . . . . ? O7 C42 C43 C48 157.66(10) . . . . ? N3 C42 C43 C48 -26.07(15) . . . . ? C48 C43 C44 C45 -0.27(19) . . . . ? C42 C43 C44 C45 -179.60(12) . . . . ? C43 C44 C45 C46 1.0(2) . . . . ? C44 C45 C46 C47 -0.6(2) . . . . ? C45 C46 C47 C48 -0.6(2) . . . . ? C46 C47 C48 O8 -175.79(12) . . . . ? C46 C47 C48 C43 1.37(18) . . . . ? C44 C43 C48 O8 176.43(10) . . . . ? C42 C43 C48 O8 -4.27(15) . . . . ? C44 C43 C48 C47 -0.94(17) . . . . ? C42 C43 C48 C47 178.36(10) . . . . ? O8 C49 C50 O9 63.24(17) . . . . ? O1 C8 N1 C7 -6.60(17) . . . . ? C9 C8 N1 C7 171.51(10) . . . . ? C6 C7 N1 C8 139.34(12) . . . . ? O6 C27 N2 C28 -3.91(18) . . . . ? C26 C27 N2 C28 177.21(11) . . . . ? C29 C28 N2 C27 -144.66(11) . . . . ? O7 C42 N3 C41 1.21(17) . . . . ? C43 C42 N3 C41 -174.99(10) . . . . ? C40 C41 N3 C42 -103.63(14) . . . . ? N1 C8 O1 Tb1 -85.7(2) . . . 1_556 ? C9 C8 O1 Tb1 96.2(2) . . . 1_556 ? C13 C14 O2 C15 -0.40(16) . . . . ? C9 C14 O2 C15 179.82(10) . . . . ? C16 C15 O2 C14 -179.52(10) . . . . ? C18 C17 O3 C16 177.92(12) . . . . ? C15 C16 O3 C17 -176.81(12) . . . . ? C20 C19 O4 C18 -175.84(10) . . . . ? C17 C18 O4 C19 176.51(11) . . . . ? C22 C21 O5 C20 -6.66(18) . . . . ? C26 C21 O5 C20 175.09(11) . . . . ? C19 C20 O5 C21 176.24(11) . . . . ? N2 C27 O6 Tb1 93.9(7) . . . . ? C26 C27 O6 Tb1 -87.2(7) . . . . ? O1 Tb1 O6 C27 175.9(6) 1_554 . . . ? O7 Tb1 O6 C27 118.7(7) . . . . ? O16 Tb1 O6 C27 -110.0(7) . . . . ? O13 Tb1 O6 C27 -37.6(7) . . . . ? O12 Tb1 O6 C27 53.9(7) . . . . ? O10 Tb1 O6 C27 34.0(7) . . . . ? O15 Tb1 O6 C27 -43.1(7) . . . . ? O18 Tb1 O6 C27 -158.5(7) . . . . ? N3 C42 O7 Tb1 130.5(4) . . . . ? C43 C42 O7 Tb1 -53.4(5) . . . . ? O6 Tb1 O7 C42 117.4(4) . . . . ? O1 Tb1 O7 C42 -38.1(4) 1_554 . . . ? O16 Tb1 O7 C42 32.5(5) . . . . ? O13 Tb1 O7 C42 -101.3(4) . . . . ? O12 Tb1 O7 C42 -112.3(4) . . . . ? O10 Tb1 O7 C42 -164.1(4) . . . . ? O15 Tb1 O7 C42 151.1(4) . . . . ? O18 Tb1 O7 C42 39.6(4) . . . . ? C47 C48 O8 C49 11.12(18) . . . . ? C43 C48 O8 C49 -166.14(11) . . . . ? C50 C49 O8 C48 153.78(12) . . . . ? C49 C50 O9 C51 179.33(14) . . . . ? C51 C51 O9 C50 179.79(17) 2_554 . . . ? O11 N4 O10 Tb1 -176.36(9) . . . . ? O12 N4 O10 Tb1 1.49(10) . . . . ? O6 Tb1 O10 N4 158.23(7) . . . . ? O1 Tb1 O10 N4 -0.23(8) 1_554 . . . ? O7 Tb1 O10 N4 76.94(6) . . . . ? O16 Tb1 O10 N4 -124.07(7) . . . . ? O13 Tb1 O10 N4 -74.48(7) . . . . ? O12 Tb1 O10 N4 -0.88(6) . . . . ? O15 Tb1 O10 N4 -126.29(7) . . . . ? O18 Tb1 O10 N4 132.19(7) . . . . ? O11 N4 O12 Tb1 176.35(9) . . . . ? O10 N4 O12 Tb1 -1.50(10) . . . . ? O6 Tb1 O12 N4 -24.29(8) . . . . ? O1 Tb1 O12 N4 -178.56(7) 1_554 . . . ? O7 Tb1 O12 N4 -91.00(7) . . . . ? O16 Tb1 O12 N4 130.63(7) . . . . ? O13 Tb1 O12 N4 95.14(7) . . . . ? O10 Tb1 O12 N4 0.88(6) . . . . ? O15 Tb1 O12 N4 55.32(7) . . . . ? O18 Tb1 O12 N4 -142.63(6) . . . . ? O14 N5 O13 Tb1 -169.73(9) . . . . ? O15 N5 O13 Tb1 10.75(9) . . . . ? O6 Tb1 O13 N5 -13.04(7) . . . . ? O1 Tb1 O13 N5 151.08(6) 1_554 . . . ? O7 Tb1 O13 N5 -145.14(6) . . . . ? O16 Tb1 O13 N5 69.33(6) . . . . ? O12 Tb1 O13 N5 -133.91(6) . . . . ? O10 Tb1 O13 N5 -82.26(6) . . . . ? O15 Tb1 O13 N5 -6.28(5) . . . . ? O18 Tb1 O13 N5 82.79(6) . . . . ? O14 N5 O15 Tb1 169.95(9) . . . . ? O13 N5 O15 Tb1 -10.54(9) . . . . ? O6 Tb1 O15 N5 -179.56(7) . . . . ? O1 Tb1 O15 N5 -22.75(8) 1_554 . . . ? O7 Tb1 O15 N5 145.65(6) . . . . ? O16 Tb1 O15 N5 -79.54(7) . . . . ? O13 Tb1 O15 N5 6.31(6) . . . . ? O12 Tb1 O15 N5 57.83(6) . . . . ? O10 Tb1 O15 N5 99.04(6) . . . . ? O18 Tb1 O15 N5 -111.01(6) . . . . ? O17 N6 O16 Tb1 -178.86(11) . . . . ? O18 N6 O16 Tb1 -0.37(11) . . . . ? O6 Tb1 O16 N6 -69.88(8) . . . . ? O1 Tb1 O16 N6 81.50(8) 1_554 . . . ? O7 Tb1 O16 N6 9.24(9) . . . . ? O13 Tb1 O16 N6 165.62(8) . . . . ? O12 Tb1 O16 N6 130.45(7) . . . . ? O10 Tb1 O16 N6 -142.59(7) . . . . ? O15 Tb1 O16 N6 -140.30(8) . . . . ? O18 Tb1 O16 N6 0.21(6) . . . . ? O17 N6 O18 Tb1 178.83(11) . . . . ? O16 N6 O18 Tb1 0.36(11) . . . . ? O6 Tb1 O18 N6 104.86(7) . . . . ? O1 Tb1 O18 N6 -87.69(7) 1_554 . . . ? O7 Tb1 O18 N6 -173.34(7) . . . . ? O16 Tb1 O18 N6 -0.21(6) . . . . ? O13 Tb1 O18 N6 -16.98(8) . . . . ? O12 Tb1 O18 N6 -122.93(7) . . . . ? O10 Tb1 O18 N6 131.00(7) . . . . ? O15 Tb1 O18 N6 38.72(7) . . . . ? # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 -0.006 0.000 612 126 ' ' _platon_squeeze_details ; C101 0.058 0.089 0.189 ! 2.98 eA-3 C102 0.031 0.482 0.009 ! 2.55 eA-3 C103 0.985 0.949 0.904 ! 2.35 eA-3 C104 1.000 0.907 0.941 ! 2.21 eA-3 C105 0.018 0.902 0.868 ! 2.03 eA-3 C106 0.989 0.076 0.161 ! 1.99 eA-3 C107 0.881 0.091 0.206 ! 1.84 eA-3 C108 0.030 0.175 0.283 ! 1.81 eA-3 C109 0.112 0.915 0.761 ! 1.75 eA-3 C110 0.016 0.372 0.050 ! 1.67 eA-3 C111 0.018 0.787 0.731 ! 1.50 eA-3 C112 1.001 0.119 0.283 ! 1.44 eA-3 C113 0.897 0.470 0.988 ! 0.79 eA-3 Q114 0.301 0.260 0.749 ! 0.73 eA-3 Q115 0.655 0.669 0.304 ! 0.67 eA-3 Q116 0.705 0.672 0.235 ! 0.59 eA-3 Q117 0.401 0.252 0.745 ! 0.59 eA-3 Q118 0.361 0.302 0.727 ! 0.58 eA-3 Q119 0.563 0.519 0.891 ! 0.57 eA-3 Q120 0.982 0.094 0.755 ! 0.53 eA-3 ; _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.550 _refine_diff_density_min -0.566 _refine_diff_density_rms 0.054