# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Wei-Sheng Liu' _publ_contact_author_address ; Lab of Applied Organic Chemistry Lanzhou university Lanzhou 730000 CHINA ; _publ_contact_author_email SONGXUEQIN001@163.COM _publ_section_title ; Tuning the self-assembly and luminescence properties of lanthanide coordination polymers by ligand design ; loop_ _publ_author_name 'Wei-Sheng Liu' 'Wei Dou' 'Xue-Qin Song' 'Xiao-Liang Tang' 'Ya-Wen Wang' 'Jiangrong Zheng' data_z060622songxq18_0m _database_code_depnum_ccdc_archive 'CCDC 672449' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H45 N3 O9' _chemical_formula_weight 807.87 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.9278(2) _cell_length_b 15.1760(4) _cell_length_c 31.0232(8) _cell_angle_alpha 90.00 _cell_angle_beta 95.2180(10) _cell_angle_gamma 90.00 _cell_volume 4185.86(18) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2991 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 20.28 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.282 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1704 _exptl_absorpt_coefficient_mu 0.089 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 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 22130 _diffrn_reflns_av_R_equivalents 0.0414 _diffrn_reflns_av_sigmaI/netI 0.0520 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 25.50 _reflns_number_total 7759 _reflns_number_gt 4118 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0716P)^2^+0.1838P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0022(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7759 _refine_ls_number_parameters 702 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1135 _refine_ls_R_factor_gt 0.0529 _refine_ls_wR_factor_ref 0.1578 _refine_ls_wR_factor_gt 0.1263 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.3510(4) 0.3727(3) -0.02281(12) 0.0781(10) Uani 1 1 d . . . C2 C -0.2378(5) 0.3860(3) 0.00630(12) 0.0837(10) Uani 1 1 d . . . C3 C -0.3644(3) 0.2815(2) -0.02818(11) 0.0646(9) Uani 1 1 d . . . C4 C -0.2616(3) 0.2423(2) -0.00190(9) 0.0595(7) Uani 1 1 d . . . C5 C -0.2226(3) 0.1492(2) 0.00673(14) 0.0715(9) Uani 1 1 d . . . C6 C -0.0417(3) 0.08721(17) -0.03967(9) 0.0528(7) Uani 1 1 d . . . C7 C 0.1201(3) 0.07369(15) -0.04735(8) 0.0455(6) Uani 1 1 d . . . C8 C 0.1484(4) 0.03531(18) -0.08670(9) 0.0614(8) Uani 1 1 d . . . C9 C 0.2924(4) 0.0232(2) -0.09836(11) 0.0697(8) Uani 1 1 d . . . C10 C 0.4120(4) 0.04764(19) -0.07039(10) 0.0655(8) Uani 1 1 d . . . C11 C 0.3893(3) 0.08494(18) -0.03116(9) 0.0561(7) Uani 1 1 d . . . C12 C 0.2446(3) 0.09944(15) -0.01967(8) 0.0461(6) Uani 1 1 d . . . C13 C 0.3408(3) 0.1826(2) 0.04390(9) 0.0533(7) Uani 1 1 d . . . C14 C 0.2757(2) 0.23486(17) 0.07882(8) 0.0463(6) Uani 1 1 d . . . C15 C 0.2265(2) 0.32149(18) 0.07014(8) 0.0493(6) Uani 1 1 d . . . C16 C 0.1768(2) 0.37241(17) 0.10372(8) 0.0489(6) Uani 1 1 d . . . C17 C 0.1679(3) 0.33511(17) 0.14486(8) 0.0514(7) Uani 1 1 d . . . C18 C 0.2155(3) 0.24835(17) 0.15297(8) 0.0501(6) Uani 1 1 d . . . C19 C 0.2698(3) 0.19773(17) 0.11997(8) 0.0491(6) Uani 1 1 d . . . C20 C 0.3206(5) 0.1033(2) 0.12824(14) 0.0752(9) Uani 1 1 d . . . C21 C 0.2287(5) 0.3594(3) 0.02519(11) 0.0738(9) Uani 1 1 d . . . C22 C 0.1057(5) 0.3886(3) 0.18031(12) 0.0753(10) Uani 1 1 d . . . C23 C 0.2051(4) 0.2109(2) 0.19737(9) 0.0642(8) Uani 1 1 d . . . C24 C 0.2784(3) 0.2634(2) 0.26953(8) 0.0610(7) Uani 1 1 d . . . C25 C 0.2003(4) 0.1967(3) 0.28845(11) 0.0839(10) Uani 1 1 d . . . C26 C 0.1652(5) 0.2062(4) 0.33084(13) 0.1055(13) Uani 1 1 d . . . C27 C 0.2061(5) 0.2814(4) 0.35374(13) 0.1050(13) Uani 1 1 d . . . C28 C 0.2846(4) 0.3461(3) 0.33510(11) 0.0862(11) Uani 1 1 d . . . C29 C 0.3239(3) 0.3397(2) 0.29280(9) 0.0646(8) Uani 1 1 d . . . C30 C 0.4070(3) 0.4155(2) 0.27602(10) 0.0685(8) Uani 1 1 d . . . C31 C 0.5707(4) 0.4719(3) 0.22316(13) 0.0854(10) Uani 1 1 d . . . C32 C 0.7285(5) 0.4741(3) 0.24239(15) 0.1014(13) Uani 1 1 d . . . C33 C 0.8063(6) 0.4302(4) 0.27359(19) 0.151(2) Uani 1 1 d . . . H33A H 0.7724 0.3841 0.2899 0.181 Uiso 1 1 calc R . . C34 C 0.9500(10) 0.4673(10) 0.2772(4) 0.267(9) Uani 1 1 d . . . H34A H 1.0290 0.4496 0.2969 0.321 Uiso 1 1 calc R . . C35 C 0.9571(13) 0.5287(10) 0.2495(5) 0.313(12) Uani 1 1 d . . . H35A H 1.0418 0.5622 0.2454 0.375 Uiso 1 1 calc R . . C36 C 0.1391(3) 0.46830(19) 0.09694(12) 0.0590(7) Uani 1 1 d . . . C37 C -0.0846(3) 0.55959(17) 0.09615(8) 0.0512(6) Uani 1 1 d . . . C38 C 0.0000(3) 0.63557(19) 0.09358(10) 0.0663(8) Uani 1 1 d . . . C39 C -0.0661(4) 0.7171(2) 0.09757(12) 0.0813(10) Uani 1 1 d . . . C40 C -0.2156(4) 0.7239(2) 0.10303(12) 0.0830(10) Uani 1 1 d . . . C41 C -0.2995(4) 0.6487(2) 0.10510(10) 0.0712(9) Uani 1 1 d . . . C42 C -0.2382(3) 0.56497(17) 0.10207(8) 0.0532(7) Uani 1 1 d . . . C43 C -0.3441(3) 0.48943(19) 0.10562(9) 0.0596(7) Uani 1 1 d . . . C44 C -0.3803(4) 0.3309(2) 0.11292(13) 0.0718(9) Uani 1 1 d . . . C45 C -0.3093(3) 0.2631(2) 0.14187(10) 0.0639(8) Uani 1 1 d . . . C46 C -0.2099(4) 0.2002(3) 0.13773(14) 0.1041(12) Uani 1 1 d . . . H46 H -0.1640 0.1866 0.1128 0.125 Uiso 1 1 calc R . . C47 C -0.1854(6) 0.1565(3) 0.17914(19) 0.1117(17) Uani 1 1 d . . . C48 C -0.2638(7) 0.2016(4) 0.20446(19) 0.149(2) Uani 1 1 d . . . H48 H -0.2649 0.1903 0.2339 0.179 Uiso 1 1 calc R . . H1 H 0.411(3) 0.1367(17) 0.0558(7) 0.056(7) Uiso 1 1 d . . . H2 H 0.389(3) 0.2211(17) 0.0245(8) 0.060(8) Uiso 1 1 d . . . H3 H 0.062(3) 0.0192(16) -0.1053(8) 0.057(7) Uiso 1 1 d . . . H4 H 0.182(3) 0.5033(19) 0.1232(9) 0.075(9) Uiso 1 1 d . . . H5 H 0.478(3) 0.1024(17) -0.0101(8) 0.069(8) Uiso 1 1 d . . . H6 H 0.229(3) 0.152(2) 0.2014(9) 0.082(11) Uiso 1 1 d . . . H7 H 0.042(4) 0.435(2) 0.1709(10) 0.101(12) Uiso 1 1 d . . . H8 H -0.400(3) 0.6510(19) 0.1092(9) 0.083(10) Uiso 1 1 d . . . H9 H 0.107(3) 0.223(2) 0.2076(9) 0.084(10) Uiso 1 1 d . . . H10 H -0.260(3) 0.782(2) 0.1084(9) 0.086(10) Uiso 1 1 d . . . H11 H -0.194(3) 0.4029(19) 0.1117(9) 0.074(9) Uiso 1 1 d . . . H12 H 0.108(3) 0.6299(16) 0.0899(8) 0.063(8) Uiso 1 1 d . . . H13 H 0.304(3) -0.0025(19) -0.1272(10) 0.083(9) Uiso 1 1 d . . . H14 H 0.000(3) 0.1438(19) 0.0157(9) 0.070(9) Uiso 1 1 d . . . H15 H -0.485(4) 0.348(2) 0.1226(9) 0.095(10) Uiso 1 1 d . . . H16 H 0.180(3) 0.4934(18) 0.0710(9) 0.072(9) Uiso 1 1 d . . . H17 H 0.518(3) 0.0372(18) -0.0775(8) 0.079(9) Uiso 1 1 d . . . H18 H 0.177(4) 0.289(2) 0.3854(12) 0.111(11) Uiso 1 1 d . . . H19 H 0.319(4) 0.391(2) 0.0201(11) 0.121(14) Uiso 1 1 d . . . H20 H 0.295(4) 0.070(3) 0.1030(13) 0.124(14) Uiso 1 1 d . . . H21 H 0.147(4) 0.400(2) 0.0181(10) 0.095(11) Uiso 1 1 d . . . H22 H -0.285(4) 0.114(2) -0.0126(10) 0.093(11) Uiso 1 1 d . . . H23 H 0.044(5) 0.350(3) 0.1983(15) 0.18(2) Uiso 1 1 d . . . H24 H -0.390(3) 0.306(2) 0.0851(11) 0.091(11) Uiso 1 1 d . . . H25 H 0.214(4) 0.314(3) 0.0029(13) 0.127(15) Uiso 1 1 d . . . H26 H 0.312(3) 0.400(2) 0.3505(11) 0.095(11) Uiso 1 1 d . . . H27 H -0.230(3) 0.134(2) 0.0385(11) 0.091(10) Uiso 1 1 d . . . H29 H -0.192(4) 0.440(3) 0.0179(12) 0.134(15) Uiso 1 1 d . . . H30 H 0.554(4) 0.463(2) 0.1887(12) 0.114(12) Uiso 1 1 d . . . H31 H 0.513(4) 0.531(3) 0.2290(11) 0.108(12) Uiso 1 1 d . . . H32 H -0.008(4) 0.767(2) 0.0970(10) 0.100(12) Uiso 1 1 d . . . H33 H 0.419(5) 0.100(2) 0.1391(12) 0.115(14) Uiso 1 1 d . . . H34 H 0.175(3) 0.143(2) 0.2713(10) 0.097(11) Uiso 1 1 d . . . H35 H -0.404(4) 0.414(2) -0.0385(11) 0.108(13) Uiso 1 1 d . . . H36 H 0.473(3) 0.350(2) 0.2292(10) 0.088(11) Uiso 1 1 d . . . H37 H -0.135(4) 0.109(3) 0.1870(13) 0.136(16) Uiso 1 1 d . . . H38 H 0.175(5) 0.412(3) 0.2014(15) 0.155(18) Uiso 1 1 d . . . H39 H 0.106(4) 0.158(3) 0.3419(11) 0.117(13) Uiso 1 1 d . . . H40 H 0.262(4) 0.075(3) 0.1480(14) 0.135(16) Uiso 1 1 d . . . H47 H -0.423(3) 0.2596(19) -0.0441(9) 0.062(10) Uiso 1 1 d . . . N1 N -0.0710(2) 0.12703(17) -0.00302(9) 0.0639(7) Uani 1 1 d . . . N2 N 0.4843(3) 0.4030(2) 0.24141(9) 0.0715(7) Uani 1 1 d . . . N3 N -0.2872(3) 0.40942(15) 0.11195(8) 0.0623(7) Uani 1 1 d . . . O1 O -0.1778(2) 0.30583(17) 0.02008(7) 0.0887(7) Uani 1 1 d . . . O2 O -0.1432(2) 0.06408(16) -0.06622(6) 0.0865(7) Uani 1 1 d . . . O3 O 0.21879(17) 0.13915(12) 0.01866(5) 0.0557(5) Uani 1 1 d . . . O4 O 0.31395(19) 0.25660(13) 0.22737(5) 0.0635(5) Uani 1 1 d . . . O5 O 0.4071(3) 0.48795(17) 0.29392(8) 0.1043(8) Uani 1 1 d . . . O6 O 0.8153(5) 0.5373(3) 0.22619(13) 0.1751(18) Uani 1 1 d . . . O7 O -0.02372(17) 0.47708(11) 0.09243(6) 0.0585(5) Uani 1 1 d . . . O8 O -0.4805(2) 0.50234(15) 0.10424(8) 0.0980(8) Uani 1 1 d . . . O9 O -0.3442(3) 0.2671(2) 0.18358(10) 0.1309(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.068(2) 0.088(3) 0.078(2) 0.018(2) 0.0069(18) 0.008(2) C2 0.104(3) 0.066(3) 0.080(2) 0.005(2) 0.008(2) -0.001(2) C3 0.0525(18) 0.075(3) 0.065(2) 0.0041(18) -0.0035(16) -0.0087(17) C4 0.0462(15) 0.067(2) 0.0665(18) -0.0029(16) 0.0126(14) -0.0066(14) C5 0.0450(16) 0.077(2) 0.094(3) 0.008(2) 0.0132(17) 0.0035(16) C6 0.0551(16) 0.0486(16) 0.0531(16) 0.0079(14) -0.0030(13) -0.0076(13) C7 0.0531(15) 0.0335(14) 0.0493(15) 0.0011(12) 0.0015(12) -0.0020(11) C8 0.075(2) 0.0517(18) 0.0556(18) -0.0060(14) -0.0033(16) -0.0055(15) C9 0.092(2) 0.0557(19) 0.064(2) -0.0144(16) 0.0198(18) 0.0005(16) C10 0.068(2) 0.0554(18) 0.076(2) -0.0092(16) 0.0242(17) 0.0083(15) C11 0.0501(15) 0.0542(17) 0.0652(18) -0.0108(15) 0.0120(14) 0.0033(13) C12 0.0525(15) 0.0365(14) 0.0497(15) -0.0050(12) 0.0077(12) 0.0022(11) C13 0.0427(14) 0.0603(19) 0.0567(17) -0.0115(15) 0.0030(13) -0.0019(14) C14 0.0365(13) 0.0492(16) 0.0529(16) -0.0112(13) 0.0025(11) -0.0025(11) C15 0.0368(13) 0.0565(17) 0.0543(16) -0.0026(14) 0.0033(11) -0.0047(12) C16 0.0374(13) 0.0479(16) 0.0612(17) -0.0031(14) 0.0035(11) -0.0014(11) C17 0.0445(14) 0.0537(17) 0.0558(16) -0.0142(14) 0.0044(12) -0.0004(12) C18 0.0502(14) 0.0487(17) 0.0513(15) -0.0065(13) 0.0034(12) -0.0067(12) C19 0.0482(14) 0.0449(16) 0.0532(16) -0.0077(13) -0.0001(12) -0.0030(12) C20 0.099(3) 0.057(2) 0.070(2) -0.0046(19) 0.008(2) 0.011(2) C21 0.081(2) 0.077(3) 0.064(2) 0.010(2) 0.0157(18) 0.005(2) C22 0.081(2) 0.076(3) 0.070(2) -0.022(2) 0.0115(19) 0.022(2) C23 0.076(2) 0.061(2) 0.0550(18) -0.0064(16) 0.0055(15) -0.0138(17) C24 0.0598(17) 0.077(2) 0.0472(16) -0.0023(16) 0.0093(13) 0.0011(15) C25 0.094(2) 0.096(3) 0.064(2) 0.004(2) 0.0176(18) -0.014(2) C26 0.109(3) 0.139(4) 0.072(3) 0.016(3) 0.028(2) -0.019(3) C27 0.110(3) 0.149(4) 0.059(2) 0.003(3) 0.023(2) 0.001(3) C28 0.093(2) 0.108(3) 0.057(2) -0.012(2) 0.0067(18) 0.008(2) C29 0.0635(17) 0.081(2) 0.0496(17) -0.0091(16) 0.0048(13) 0.0080(16) C30 0.0643(18) 0.074(2) 0.066(2) -0.0163(18) 0.0026(15) 0.0054(16) C31 0.091(3) 0.080(3) 0.086(3) -0.005(2) 0.010(2) -0.015(2) C32 0.084(3) 0.102(3) 0.123(3) -0.057(3) 0.034(3) -0.023(2) C33 0.102(4) 0.181(6) 0.163(5) -0.069(4) -0.028(3) 0.042(4) C34 0.081(6) 0.41(2) 0.304(14) -0.265(14) -0.038(7) 0.062(8) C35 0.115(6) 0.42(2) 0.43(2) -0.351(18) 0.133(10) -0.122(10) C36 0.0431(15) 0.0515(19) 0.083(2) 0.0018(17) 0.0071(15) 0.0009(13) C37 0.0536(15) 0.0416(16) 0.0579(16) 0.0047(13) 0.0019(12) 0.0038(13) C38 0.0602(19) 0.0471(19) 0.092(2) 0.0087(16) 0.0064(16) -0.0031(15) C39 0.083(2) 0.047(2) 0.113(3) 0.0140(19) 0.0025(19) -0.0014(19) C40 0.083(3) 0.050(2) 0.117(3) 0.0104(19) 0.0148(19) 0.0144(19) C41 0.063(2) 0.061(2) 0.091(2) 0.0145(17) 0.0168(17) 0.0148(17) C42 0.0531(15) 0.0460(17) 0.0605(16) 0.0086(13) 0.0045(12) 0.0041(13) C43 0.0502(16) 0.0596(19) 0.0687(18) 0.0136(15) 0.0033(13) 0.0071(14) C44 0.060(2) 0.062(2) 0.091(3) 0.007(2) -0.0010(18) -0.0149(16) C45 0.0607(17) 0.0542(19) 0.077(2) 0.0054(16) 0.0080(15) -0.0150(15) C46 0.107(3) 0.078(3) 0.122(3) -0.030(3) -0.022(2) 0.019(2) C47 0.114(3) 0.046(2) 0.164(5) 0.005(3) -0.045(3) 0.003(2) C48 0.185(5) 0.105(4) 0.157(5) 0.071(4) 0.014(4) 0.008(4) N1 0.0409(13) 0.0772(18) 0.0729(17) -0.0117(14) 0.0012(12) -0.0032(12) N2 0.0784(17) 0.0679(19) 0.0699(17) -0.0116(15) 0.0158(14) -0.0094(15) N3 0.0440(13) 0.0498(15) 0.0915(18) 0.0104(13) -0.0019(12) -0.0044(12) O1 0.0852(15) 0.0900(18) 0.0876(15) 0.0072(14) -0.0105(12) -0.0036(13) O2 0.0629(12) 0.1189(19) 0.0736(14) -0.0098(13) -0.0166(10) -0.0157(12) O3 0.0434(9) 0.0706(12) 0.0533(10) -0.0207(9) 0.0064(8) -0.0053(8) O4 0.0648(11) 0.0793(14) 0.0472(10) -0.0093(10) 0.0100(9) -0.0094(10) O5 0.126(2) 0.0815(18) 0.1094(19) -0.0374(15) 0.0348(15) -0.0079(14) O6 0.152(3) 0.180(3) 0.209(4) -0.112(3) 0.102(3) -0.083(3) O7 0.0450(10) 0.0434(11) 0.0870(13) -0.0041(9) 0.0049(8) 0.0008(8) O8 0.0499(12) 0.0838(16) 0.161(2) 0.0354(15) 0.0103(12) 0.0057(11) O9 0.135(2) 0.142(3) 0.122(2) 0.045(2) 0.0456(18) 0.030(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 1.308(5) . ? C1 C3 1.398(5) . ? C1 H35 0.90(3) . ? C2 O1 1.381(4) . ? C2 H29 0.97(4) . ? C3 C4 1.313(4) . ? C3 H47 0.76(3) . ? C4 O1 1.364(3) . ? C4 C5 1.474(4) . ? C5 N1 1.453(3) . ? C5 H22 0.94(3) . ? C5 H27 1.02(3) . ? C6 O2 1.219(3) . ? C6 N1 1.334(3) . ? C6 C7 1.499(3) . ? C7 C8 1.396(4) . ? C7 C12 1.397(3) . ? C8 C9 1.379(4) . ? C8 H3 0.95(2) . ? C9 C10 1.365(4) . ? C9 H13 0.99(3) . ? C10 C11 1.374(4) . ? C10 H17 1.00(3) . ? C11 C12 1.388(3) . ? C11 H5 1.02(3) . ? C12 O3 1.371(3) . ? C13 O3 1.442(3) . ? C13 C14 1.501(3) . ? C13 H1 0.99(2) . ? C13 H2 0.97(3) . ? C14 C19 1.401(3) . ? C14 C15 1.405(3) . ? C15 C16 1.401(3) . ? C15 C21 1.510(4) . ? C16 C17 1.405(3) . ? C16 C36 1.504(4) . ? C17 C18 1.399(3) . ? C17 C22 1.513(4) . ? C18 C19 1.401(3) . ? C18 C23 1.500(4) . ? C19 C20 1.518(4) . ? C20 H20 0.94(4) . ? C20 H33 0.91(4) . ? C20 H40 0.94(4) . ? C21 H19 0.96(4) . ? C21 H21 0.97(3) . ? C21 H25 0.98(4) . ? C22 H7 0.94(4) . ? C22 H23 1.01(5) . ? C22 H38 0.93(5) . ? C23 O4 1.458(3) . ? C23 H6 0.92(3) . ? C23 H9 0.97(3) . ? C24 O4 1.378(3) . ? C24 C25 1.390(4) . ? C24 C29 1.404(4) . ? C25 C26 1.387(5) . ? C25 H34 0.99(3) . ? C26 C27 1.376(6) . ? C26 H39 0.98(4) . ? C27 C28 1.365(5) . ? C27 H18 1.04(4) . ? C28 C29 1.392(4) . ? C28 H26 0.97(3) . ? C29 C30 1.489(4) . ? C30 O5 1.231(3) . ? C30 N2 1.342(4) . ? C31 N2 1.445(4) . ? C31 C32 1.479(5) . ? C31 H30 1.07(4) . ? C31 H31 1.06(4) . ? C32 C33 1.319(6) . ? C32 O6 1.358(5) . ? C33 C34 1.395(11) . ? C33 H33A 0.9300 . ? C34 C35 1.27(2) . ? C34 H34A 0.9300 . ? C35 O6 1.406(13) . ? C35 H35A 0.9300 . ? C36 O7 1.454(3) . ? C36 H4 1.02(3) . ? C36 H16 0.99(3) . ? C37 O7 1.374(3) . ? C37 C38 1.385(4) . ? C37 C42 1.402(3) . ? C38 C39 1.381(4) . ? C38 H12 0.98(3) . ? C39 C40 1.364(4) . ? C39 H32 0.92(3) . ? C40 C41 1.370(4) . ? C40 H10 0.98(3) . ? C41 C42 1.391(4) . ? C41 H8 0.92(3) . ? C42 C43 1.497(4) . ? C43 O8 1.230(3) . ? C43 N3 1.324(3) . ? C44 N3 1.455(4) . ? C44 C45 1.470(4) . ? C44 H15 1.04(3) . ? C44 H24 0.94(3) . ? C45 C46 1.317(4) . ? C45 O9 1.359(4) . ? C46 C47 1.445(6) . ? C46 H46 0.9300 . ? C47 C48 1.295(7) . ? C47 H37 0.87(4) . ? C48 O9 1.355(5) . ? C48 H48 0.9300 . ? N1 H14 0.85(3) . ? N2 H36 0.89(3) . ? N3 H11 0.84(3) . ? 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 C3 106.7(4) . . ? C2 C1 H35 127(2) . . ? C3 C1 H35 126(2) . . ? C1 C2 O1 109.3(4) . . ? C1 C2 H29 131(2) . . ? O1 C2 H29 119(2) . . ? C4 C3 C1 109.1(3) . . ? C4 C3 H47 127(2) . . ? C1 C3 H47 124(2) . . ? C3 C4 O1 108.1(3) . . ? C3 C4 C5 133.4(3) . . ? O1 C4 C5 118.5(3) . . ? N1 C5 C4 113.2(3) . . ? N1 C5 H22 104.1(19) . . ? C4 C5 H22 108.1(19) . . ? N1 C5 H27 106.8(17) . . ? C4 C5 H27 111.0(18) . . ? H22 C5 H27 114(3) . . ? O2 C6 N1 121.0(3) . . ? O2 C6 C7 121.4(3) . . ? N1 C6 C7 117.6(2) . . ? C8 C7 C12 117.2(2) . . ? C8 C7 C6 116.7(2) . . ? C12 C7 C6 126.0(2) . . ? C9 C8 C7 122.2(3) . . ? C9 C8 H3 122.1(14) . . ? C7 C8 H3 115.7(15) . . ? C10 C9 C8 119.4(3) . . ? C10 C9 H13 122.8(16) . . ? C8 C9 H13 117.7(16) . . ? C9 C10 C11 120.3(3) . . ? C9 C10 H17 121.1(16) . . ? C11 C10 H17 118.6(16) . . ? C10 C11 C12 120.6(3) . . ? C10 C11 H5 120.5(14) . . ? C12 C11 H5 118.9(14) . . ? O3 C12 C11 121.7(2) . . ? O3 C12 C7 118.0(2) . . ? C11 C12 C7 120.3(2) . . ? O3 C13 C14 108.11(19) . . ? O3 C13 H1 107.6(14) . . ? C14 C13 H1 112.2(14) . . ? O3 C13 H2 107.1(14) . . ? C14 C13 H2 110.7(15) . . ? H1 C13 H2 111(2) . . ? C19 C14 C15 120.9(2) . . ? C19 C14 C13 119.6(2) . . ? C15 C14 C13 119.4(2) . . ? C16 C15 C14 119.2(2) . . ? C16 C15 C21 120.5(3) . . ? C14 C15 C21 120.2(3) . . ? C15 C16 C17 120.1(2) . . ? C15 C16 C36 120.8(3) . . ? C17 C16 C36 119.1(2) . . ? C18 C17 C16 120.1(2) . . ? C18 C17 C22 120.0(3) . . ? C16 C17 C22 119.9(3) . . ? C17 C18 C19 120.3(2) . . ? C17 C18 C23 118.5(3) . . ? C19 C18 C23 121.2(3) . . ? C14 C19 C18 119.3(2) . . ? C14 C19 C20 119.9(3) . . ? C18 C19 C20 120.8(3) . . ? C19 C20 H20 108(2) . . ? C19 C20 H33 112(2) . . ? H20 C20 H33 116(3) . . ? C19 C20 H40 111(3) . . ? H20 C20 H40 101(3) . . ? H33 C20 H40 108(3) . . ? C15 C21 H19 115(2) . . ? C15 C21 H21 112.4(19) . . ? H19 C21 H21 106(3) . . ? C15 C21 H25 112(2) . . ? H19 C21 H25 107(3) . . ? H21 C21 H25 104(3) . . ? C17 C22 H7 116(2) . . ? C17 C22 H23 110(3) . . ? H7 C22 H23 105(3) . . ? C17 C22 H38 117(3) . . ? H7 C22 H38 106(3) . . ? H23 C22 H38 101(4) . . ? O4 C23 C18 108.2(2) . . ? O4 C23 H6 103.9(19) . . ? C18 C23 H6 117.1(19) . . ? O4 C23 H9 105.8(17) . . ? C18 C23 H9 111.4(17) . . ? H6 C23 H9 110(3) . . ? O4 C24 C25 120.9(3) . . ? O4 C24 C29 118.0(3) . . ? C25 C24 C29 121.1(3) . . ? C26 C25 C24 119.4(4) . . ? C26 C25 H34 122.6(19) . . ? C24 C25 H34 118.0(19) . . ? C27 C26 C25 120.2(4) . . ? C27 C26 H39 124(2) . . ? C25 C26 H39 115(2) . . ? C28 C27 C26 120.1(4) . . ? C28 C27 H18 120(2) . . ? C26 C27 H18 120(2) . . ? C27 C28 C29 122.1(4) . . ? C27 C28 H26 121(2) . . ? C29 C28 H26 117(2) . . ? C28 C29 C24 117.2(3) . . ? C28 C29 C30 116.8(3) . . ? C24 C29 C30 126.0(3) . . ? O5 C30 N2 120.5(3) . . ? O5 C30 C29 120.8(3) . . ? N2 C30 C29 118.6(3) . . ? N2 C31 C32 112.4(3) . . ? N2 C31 H30 106.0(19) . . ? C32 C31 H30 116.3(18) . . ? N2 C31 H31 104.8(19) . . ? C32 C31 H31 112.2(19) . . ? H30 C31 H31 104(3) . . ? C33 C32 O6 110.3(5) . . ? C33 C32 C31 134.7(5) . . ? O6 C32 C31 114.9(5) . . ? C32 C33 C34 105.9(8) . . ? C32 C33 H33A 127.0 . . ? C34 C33 H33A 127.0 . . ? C35 C34 C33 110.1(11) . . ? C35 C34 H34A 125.0 . . ? C33 C34 H34A 125.0 . . ? C34 C35 O6 108.5(10) . . ? C34 C35 H35A 125.8 . . ? O6 C35 H35A 125.8 . . ? O7 C36 C16 108.1(2) . . ? O7 C36 H4 109.0(15) . . ? C16 C36 H4 109.3(16) . . ? O7 C36 H16 109.1(15) . . ? C16 C36 H16 113.0(16) . . ? H4 C36 H16 108(2) . . ? O7 C37 C38 122.1(2) . . ? O7 C37 C42 117.6(2) . . ? C38 C37 C42 120.3(2) . . ? C39 C38 C37 120.0(3) . . ? C39 C38 H12 121.4(15) . . ? C37 C38 H12 118.6(15) . . ? C40 C39 C38 120.7(3) . . ? C40 C39 H32 120(2) . . ? C38 C39 H32 119(2) . . ? C39 C40 C41 119.2(3) . . ? C39 C40 H10 120.3(17) . . ? C41 C40 H10 120.2(17) . . ? C40 C41 C42 122.5(3) . . ? C40 C41 H8 121.4(19) . . ? C42 C41 H8 116.1(19) . . ? C41 C42 C37 117.2(3) . . ? C41 C42 C43 116.1(2) . . ? C37 C42 C43 126.7(2) . . ? O8 C43 N3 121.1(3) . . ? O8 C43 C42 120.4(3) . . ? N3 C43 C42 118.5(2) . . ? N3 C44 C45 111.8(2) . . ? N3 C44 H15 108.9(17) . . ? C45 C44 H15 110.5(17) . . ? N3 C44 H24 108(2) . . ? C45 C44 H24 106(2) . . ? H15 C44 H24 111(3) . . ? C46 C45 O9 109.8(3) . . ? C46 C45 C44 134.7(4) . . ? O9 C45 C44 115.3(3) . . ? C45 C46 C47 107.1(4) . . ? C45 C46 H46 126.4 . . ? C47 C46 H46 126.4 . . ? C48 C47 C46 104.5(4) . . ? C48 C47 H37 124(3) . . ? C46 C47 H37 131(3) . . ? C47 C48 O9 113.0(5) . . ? C47 C48 H48 123.5 . . ? O9 C48 H48 123.5 . . ? C6 N1 C5 122.8(3) . . ? C6 N1 H14 121.6(19) . . ? C5 N1 H14 115.6(19) . . ? C30 N2 C31 122.9(3) . . ? C30 N2 H36 115(2) . . ? C31 N2 H36 122(2) . . ? C43 N3 C44 122.8(3) . . ? C43 N3 H11 118(2) . . ? C44 N3 H11 118(2) . . ? C4 O1 C2 106.7(3) . . ? C12 O3 C13 119.61(18) . . ? C24 O4 C23 116.3(2) . . ? C32 O6 C35 105.2(7) . . ? C37 O7 C36 118.37(19) . . ? C48 O9 C45 105.4(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C3 C1 C2 O1 -0.3(4) . . . . ? C2 C1 C3 C4 1.1(4) . . . . ? C1 C3 C4 O1 -1.4(3) . . . . ? C1 C3 C4 C5 179.7(3) . . . . ? C3 C4 C5 N1 118.3(4) . . . . ? O1 C4 C5 N1 -60.5(4) . . . . ? O2 C6 C7 C8 1.5(4) . . . . ? N1 C6 C7 C8 -177.4(2) . . . . ? O2 C6 C7 C12 178.4(3) . . . . ? N1 C6 C7 C12 -0.4(4) . . . . ? C12 C7 C8 C9 -0.3(4) . . . . ? C6 C7 C8 C9 177.0(3) . . . . ? C7 C8 C9 C10 1.4(4) . . . . ? C8 C9 C10 C11 -0.8(5) . . . . ? C9 C10 C11 C12 -0.9(4) . . . . ? C10 C11 C12 O3 -177.9(2) . . . . ? C10 C11 C12 C7 2.0(4) . . . . ? C8 C7 C12 O3 178.5(2) . . . . ? C6 C7 C12 O3 1.5(4) . . . . ? C8 C7 C12 C11 -1.4(4) . . . . ? C6 C7 C12 C11 -178.3(2) . . . . ? O3 C13 C14 C19 94.7(3) . . . . ? O3 C13 C14 C15 -87.5(3) . . . . ? C19 C14 C15 C16 2.7(3) . . . . ? C13 C14 C15 C16 -175.1(2) . . . . ? C19 C14 C15 C21 -177.9(3) . . . . ? C13 C14 C15 C21 4.4(4) . . . . ? C14 C15 C16 C17 -3.8(3) . . . . ? C21 C15 C16 C17 176.8(3) . . . . ? C14 C15 C16 C36 173.3(2) . . . . ? C21 C15 C16 C36 -6.1(4) . . . . ? C15 C16 C17 C18 3.0(3) . . . . ? C36 C16 C17 C18 -174.2(2) . . . . ? C15 C16 C17 C22 -176.5(3) . . . . ? C36 C16 C17 C22 6.3(4) . . . . ? C16 C17 C18 C19 -1.1(3) . . . . ? C22 C17 C18 C19 178.4(3) . . . . ? C16 C17 C18 C23 179.7(2) . . . . ? C22 C17 C18 C23 -0.8(4) . . . . ? C15 C14 C19 C18 -0.7(3) . . . . ? C13 C14 C19 C18 177.0(2) . . . . ? C15 C14 C19 C20 178.7(3) . . . . ? C13 C14 C19 C20 -3.6(4) . . . . ? C17 C18 C19 C14 -0.1(3) . . . . ? C23 C18 C19 C14 179.1(2) . . . . ? C17 C18 C19 C20 -179.5(3) . . . . ? C23 C18 C19 C20 -0.3(4) . . . . ? C17 C18 C23 O4 -68.4(3) . . . . ? C19 C18 C23 O4 112.4(3) . . . . ? O4 C24 C25 C26 -179.4(3) . . . . ? C29 C24 C25 C26 0.8(5) . . . . ? C24 C25 C26 C27 0.7(6) . . . . ? C25 C26 C27 C28 -1.5(6) . . . . ? C26 C27 C28 C29 1.0(6) . . . . ? C27 C28 C29 C24 0.4(5) . . . . ? C27 C28 C29 C30 178.9(3) . . . . ? O4 C24 C29 C28 178.9(2) . . . . ? C25 C24 C29 C28 -1.3(4) . . . . ? O4 C24 C29 C30 0.6(4) . . . . ? C25 C24 C29 C30 -179.6(3) . . . . ? C28 C29 C30 O5 -17.9(4) . . . . ? C24 C29 C30 O5 160.4(3) . . . . ? C28 C29 C30 N2 160.9(3) . . . . ? C24 C29 C30 N2 -20.9(4) . . . . ? N2 C31 C32 C33 -3.6(7) . . . . ? N2 C31 C32 O6 179.6(3) . . . . ? O6 C32 C33 C34 -0.3(6) . . . . ? C31 C32 C33 C34 -177.3(6) . . . . ? C32 C33 C34 C35 -0.6(14) . . . . ? C33 C34 C35 O6 1.2(17) . . . . ? C15 C16 C36 O7 104.3(3) . . . . ? C17 C16 C36 O7 -78.5(3) . . . . ? O7 C37 C38 C39 -179.9(3) . . . . ? C42 C37 C38 C39 1.1(4) . . . . ? C37 C38 C39 C40 -1.6(5) . . . . ? C38 C39 C40 C41 0.8(6) . . . . ? C39 C40 C41 C42 0.3(5) . . . . ? C40 C41 C42 C37 -0.8(5) . . . . ? C40 C41 C42 C43 179.1(3) . . . . ? O7 C37 C42 C41 -179.0(2) . . . . ? C38 C37 C42 C41 0.1(4) . . . . ? O7 C37 C42 C43 1.2(4) . . . . ? C38 C37 C42 C43 -179.8(3) . . . . ? C41 C42 C43 O8 11.2(4) . . . . ? C37 C42 C43 O8 -169.0(3) . . . . ? C41 C42 C43 N3 -166.2(3) . . . . ? C37 C42 C43 N3 13.6(4) . . . . ? N3 C44 C45 C46 -84.7(5) . . . . ? N3 C44 C45 O9 90.4(4) . . . . ? O9 C45 C46 C47 3.8(4) . . . . ? C44 C45 C46 C47 179.1(3) . . . . ? C45 C46 C47 C48 -4.6(5) . . . . ? C46 C47 C48 O9 3.7(6) . . . . ? O2 C6 N1 C5 -3.1(4) . . . . ? C7 C6 N1 C5 175.7(2) . . . . ? C4 C5 N1 C6 -99.5(4) . . . . ? O5 C30 N2 C31 -0.1(5) . . . . ? C29 C30 N2 C31 -178.9(3) . . . . ? C32 C31 N2 C30 90.6(4) . . . . ? O8 C43 N3 C44 6.9(5) . . . . ? C42 C43 N3 C44 -175.7(3) . . . . ? C45 C44 N3 C43 -149.0(3) . . . . ? C3 C4 O1 C2 1.3(3) . . . . ? C5 C4 O1 C2 -179.7(3) . . . . ? C1 C2 O1 C4 -0.6(4) . . . . ? C11 C12 O3 C13 12.5(4) . . . . ? C7 C12 O3 C13 -167.4(2) . . . . ? C14 C13 O3 C12 168.9(2) . . . . ? C25 C24 O4 C23 34.2(4) . . . . ? C29 C24 O4 C23 -146.0(3) . . . . ? C18 C23 O4 C24 150.8(2) . . . . ? C33 C32 O6 C35 1.0(7) . . . . ? C31 C32 O6 C35 178.6(6) . . . . ? C34 C35 O6 C32 -1.4(14) . . . . ? C38 C37 O7 C36 15.8(4) . . . . ? C42 C37 O7 C36 -165.1(2) . . . . ? C16 C36 O7 C37 164.9(2) . . . . ? C47 C48 O9 C45 -1.5(6) . . . . ? C46 C45 O9 C48 -1.7(4) . . . . ? C44 C45 O9 C48 -178.0(3) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.322 _refine_diff_density_min -0.212 _refine_diff_density_rms 0.036 data_060912d _database_code_depnum_ccdc_archive 'CCDC 672450' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H47 N6 O19 Pr' _chemical_formula_weight 1152.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.395(2) _cell_length_b 17.708(3) _cell_length_c 24.171(4) _cell_angle_alpha 90.00 _cell_angle_beta 106.782(2) _cell_angle_gamma 90.00 _cell_volume 5898.9(17) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6019 _cell_measurement_theta_min 2.243 _cell_measurement_theta_max 25.278 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.29 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.298 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2352 _exptl_absorpt_coefficient_mu 0.896 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7385 _exptl_absorpt_correction_T_max 0.7811 _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 30035 _diffrn_reflns_av_R_equivalents 0.0660 _diffrn_reflns_av_sigmaI/netI 0.0883 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10300 _reflns_number_gt 5328 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1064P)^2^+9.0602P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10300 _refine_ls_number_parameters 712 _refine_ls_number_restraints 446 _refine_ls_R_factor_all 0.1431 _refine_ls_R_factor_gt 0.0660 _refine_ls_wR_factor_ref 0.2285 _refine_ls_wR_factor_gt 0.1674 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.056 _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 Pr1 Pr 0.29211(4) 0.77275(2) 0.01789(2) 0.0594(2) Uani 1 1 d . B . N1 N 0.3006(5) 0.5351(4) 0.0615(4) 0.073(2) Uani 1 1 d . . . H1 H 0.3139 0.4881 0.0685 0.088 Uiso 1 1 calc R A 1 N2 N 0.2710(7) 1.0052(4) 0.0748(3) 0.092(3) Uani 1 1 d . . . H2 H 0.2600 1.0530 0.0725 0.111 Uiso 1 1 calc R . . N3 N 0.5146(6) 0.7557(4) 0.1848(3) 0.071(2) Uani 1 1 d . . . H3 H 0.5710 0.7523 0.2096 0.085 Uiso 1 1 calc R . . N4 N 0.1347(7) 0.7400(4) 0.0714(5) 0.078(2) Uani 1 1 d . B . N5 N 0.4220(8) 0.8339(6) -0.0486(4) 0.093(3) Uani 1 1 d . B . N6 N 0.1744(7) 0.7194(6) -0.0996(5) 0.086(3) Uani 1 1 d . B . O1 O 0.4224(4) 0.4230(3) 0.0721(3) 0.0607(15) Uani 1 1 d . . . O2 O 0.3565(4) 0.6504(3) 0.0507(3) 0.0739(18) Uani 1 1 d . . . O3 O 0.1174(15) 0.4510(12) 0.0222(9) 0.110(5) Uani 0.450(12) 1 d PDU B 1 O3' O 0.1307(12) 0.4571(9) -0.0162(8) 0.116(6) Uani 0.550(12) 1 d PD B 2 O4 O 0.1605(4) 1.1201(3) 0.0318(2) 0.0615(15) Uani 1 1 d . . . O5 O 0.2300(5) 0.8936(3) 0.0346(3) 0.0731(18) Uani 1 1 d . . . O6 O 0.4170(10) 1.0132(8) 0.2259(5) 0.192(4) Uani 1 1 d DU . . O7 O 0.6957(4) 0.8054(4) 0.2267(3) 0.0709(17) Uani 1 1 d . . . O8 O 0.4291(5) 0.8021(3) 0.0996(3) 0.0654(16) Uani 1 1 d . . . O9 O 0.3432(9) 0.8164(8) 0.2185(5) 0.162(3) Uani 1 1 d DU . . O10 O 0.2205(6) 0.7492(4) 0.1015(3) 0.083(2) Uani 1 1 d . . . O11 O 0.1193(5) 0.7443(4) 0.0168(4) 0.084(2) Uani 1 1 d . . . O12 O 0.0677(6) 0.7250(5) 0.0923(4) 0.117(3) Uani 1 1 d . . . O13 O 0.3670(6) 0.8756(4) -0.0297(3) 0.087(2) Uani 1 1 d . . . O14 O 0.4181(6) 0.7642(4) -0.0367(4) 0.094(2) Uani 1 1 d . . . O15 O 0.4740(8) 0.8559(6) -0.0771(5) 0.150(4) Uani 1 1 d . . . O16 O 0.1806(6) 0.7891(4) -0.0863(3) 0.091(2) Uani 1 1 d . . . O17 O 0.2236(6) 0.6744(4) -0.0625(3) 0.094(2) Uani 1 1 d . . . O18 O 0.1209(7) 0.6982(6) -0.1455(4) 0.121(3) Uani 1 1 d . . . C1 C 0.3554(6) 0.3150(4) 0.1051(4) 0.051(2) Uani 1 1 d . . . C2 C 0.2925(6) 0.2688(4) 0.0653(3) 0.052(2) Uani 1 1 d . . . C3 C 0.2092(6) 0.2409(4) 0.0773(4) 0.055(2) Uani 1 1 d . . . C4 C 0.1925(6) 0.2551(5) 0.1308(4) 0.058(2) Uani 1 1 d . . . C5 C 0.2542(6) 0.3060(5) 0.1692(4) 0.058(2) Uani 1 1 d . . . C6 C 0.3343(6) 0.3365(4) 0.1556(4) 0.057(2) Uani 1 1 d . . . C7 C 0.4463(7) 0.3470(4) 0.0936(4) 0.065(2) Uani 1 1 d . . . H7A H 0.4998 0.3477 0.1289 0.078 Uiso 1 1 calc R . . H7B H 0.4649 0.3165 0.0651 0.078 Uiso 1 1 calc R . . C8 C 0.3111(9) 0.2483(6) 0.0084(5) 0.092(3) Uani 1 1 d . . . H8A H 0.2763 0.2824 -0.0212 0.138 Uiso 1 1 calc R . . H8B H 0.2896 0.1975 -0.0020 0.138 Uiso 1 1 calc R . . H8C H 0.3793 0.2519 0.0125 0.138 Uiso 1 1 calc R . . C9 C 0.1337(7) 1.1987(4) 0.0314(4) 0.072(3) Uani 1 1 d . . . H9A H 0.0710 1.2032 0.0387 0.086 Uiso 1 1 calc R . . H9B H 0.1285 1.2205 -0.0062 0.086 Uiso 1 1 calc R . . C10 C 0.1068(8) 0.2193(6) 0.1452(5) 0.095(3) Uani 1 1 d . . . H10A H 0.1222 0.2118 0.1862 0.143 Uiso 1 1 calc R . . H10B H 0.0923 0.1715 0.1259 0.143 Uiso 1 1 calc R . . H10C H 0.0514 0.2519 0.1327 0.143 Uiso 1 1 calc R . . C11 C 0.7688(7) 0.8320(6) 0.2774(4) 0.079(3) Uani 1 1 d . . . H11A H 0.7712 0.8868 0.2770 0.095 Uiso 1 1 calc R . . H11B H 0.8319 0.8129 0.2773 0.095 Uiso 1 1 calc R . . C12 C 0.3980(7) 0.3945(5) 0.1956(4) 0.077(3) Uani 1 1 d . . . H12A H 0.4601 0.3725 0.2142 0.115 Uiso 1 1 calc R . . H12B H 0.3676 0.4099 0.2243 0.115 Uiso 1 1 calc R . . H12C H 0.4064 0.4376 0.1735 0.115 Uiso 1 1 calc R . . C13 C 0.3724(6) 0.5812(4) 0.0590(4) 0.056(2) Uani 1 1 d . B . C14 C 0.4727(6) 0.5498(4) 0.0681(3) 0.051(2) Uani 1 1 d . . . C15 C 0.4968(6) 0.4729(4) 0.0739(3) 0.052(2) Uani 1 1 d . B . C16 C 0.5893(7) 0.4493(5) 0.0805(4) 0.067(3) Uani 1 1 d . . . H16 H 0.6038 0.3980 0.0831 0.081 Uiso 1 1 calc R B . C17 C 0.6614(8) 0.5017(6) 0.0835(5) 0.082(3) Uani 1 1 d . B . H17 H 0.7249 0.4856 0.0889 0.099 Uiso 1 1 calc R . . C18 C 0.6406(8) 0.5769(6) 0.0785(5) 0.083(3) Uani 1 1 d . . . H18A H 0.6896 0.6118 0.0801 0.100 Uiso 1 1 calc R B . C19 C 0.5472(7) 0.6010(5) 0.0711(4) 0.070(3) Uani 1 1 d . B . H19 H 0.5335 0.6525 0.0680 0.084 Uiso 1 1 calc R . . C20 C 0.2013(7) 0.5594(5) 0.0531(6) 0.094(4) Uani 0.450(12) 1 d PD B 1 H20A H 0.1726 0.5727 0.0129 0.113 Uiso 0.450(12) 1 calc PR B 1 H20B H 0.2010 0.6041 0.0762 0.113 Uiso 0.450(12) 1 calc PR B 1 C21 C 0.1428(19) 0.5003(12) 0.0693(11) 0.098(5) Uani 0.450(12) 1 d PDU B 1 C22 C 0.0902(19) 0.4805(13) 0.1090(9) 0.107(5) Uani 0.450(12) 1 d PDU B 1 H22 H 0.0907 0.5059 0.1427 0.128 Uiso 0.450(12) 1 calc PR B 1 C23 C 0.0354(17) 0.4124(12) 0.0858(10) 0.103(5) Uani 0.450(12) 1 d PDU B 1 H23 H -0.0034 0.3847 0.1032 0.124 Uiso 0.450(12) 1 calc PR B 1 C24 C 0.053(4) 0.396(2) 0.0307(15) 0.104(4) Uani 0.450(12) 1 d PDU B 1 H24 H 0.0261 0.3566 0.0058 0.125 Uiso 0.450(12) 1 calc PR B 1 C20' C 0.2013(7) 0.5594(5) 0.0531(6) 0.094(4) Uani 0.550(12) 1 d PD B 2 H20C H 0.1940 0.5824 0.0880 0.113 Uiso 0.550(12) 1 calc PR B 2 H20D H 0.1822 0.5956 0.0218 0.113 Uiso 0.550(12) 1 calc PR B 2 C21' C 0.1437(15) 0.4920(10) 0.0392(9) 0.088(4) Uani 0.550(12) 1 d PDU B 2 C22' C 0.0925(15) 0.4513(11) 0.0701(8) 0.099(4) Uani 0.550(12) 1 d PDU B 2 H22' H 0.0888 0.4635 0.1068 0.119 Uiso 0.550(12) 1 calc PR B 2 C23' C 0.047(3) 0.3890(19) 0.0372(12) 0.107(4) Uani 0.550(12) 1 d PDU B 2 H23' H 0.0104 0.3522 0.0485 0.129 Uiso 0.550(12) 1 calc PR B 2 C24' C 0.0685(15) 0.3926(10) -0.0168(8) 0.104(4) Uani 0.550(12) 1 d PDU B 2 H24' H 0.0462 0.3591 -0.0474 0.124 Uiso 0.550(12) 1 calc PR B 2 C25 C 0.2161(7) 0.9627(5) 0.0342(4) 0.056(2) Uani 1 1 d . B . C26 C 0.1367(6) 0.9992(4) -0.0112(3) 0.0459(19) Uani 1 1 d . . . C27 C 0.1078(6) 1.0748(4) -0.0130(4) 0.053(2) Uani 1 1 d . B . C28 C 0.0319(7) 1.1018(5) -0.0578(4) 0.063(2) Uani 1 1 d . . . H28 H 0.0128 1.1520 -0.0581 0.076 Uiso 1 1 calc R B . C29 C -0.0154(7) 1.0538(6) -0.1019(4) 0.074(3) Uani 1 1 d . B . H29 H -0.0661 1.0725 -0.1320 0.088 Uiso 1 1 calc R . . C30 C 0.0103(8) 0.9803(6) -0.1024(4) 0.075(3) Uani 1 1 d . . . H30 H -0.0221 0.9491 -0.1328 0.090 Uiso 1 1 calc R B . C31 C 0.0846(8) 0.9523(5) -0.0577(4) 0.067(3) Uani 1 1 d . B . H31 H 0.1012 0.9015 -0.0578 0.081 Uiso 1 1 calc R . . C32 C 0.3504(10) 0.9779(7) 0.1244(5) 0.112(4) Uani 1 1 d U . . H32A H 0.3450 0.9237 0.1282 0.134 Uiso 1 1 calc R . . H32B H 0.4124 0.9887 0.1178 0.134 Uiso 1 1 calc R . . C33 C 0.3457(12) 1.0142(10) 0.1764(6) 0.145(4) Uani 1 1 d DU . . C34 C 0.2681(14) 1.0327(12) 0.1949(7) 0.188(5) Uani 1 1 d DU . . H34 H 0.2037 1.0227 0.1750 0.226 Uiso 1 1 calc R . . C35 C 0.3004(15) 1.0696(11) 0.2491(7) 0.183(5) Uani 1 1 d DU . . H35 H 0.2641 1.1000 0.2664 0.219 Uiso 1 1 calc R . . C36 C 0.3927(15) 1.0517(12) 0.2697(7) 0.179(5) Uani 1 1 d DU . . H36 H 0.4335 1.0626 0.3063 0.215 Uiso 1 1 calc R . . C37 C 0.5061(7) 0.7985(4) 0.1385(4) 0.055(2) Uani 1 1 d . B . C38 C 0.5912(7) 0.8435(5) 0.1341(4) 0.059(2) Uani 1 1 d . . . C39 C 0.6820(7) 0.8467(6) 0.1763(4) 0.068(3) Uani 1 1 d . B . C40 C 0.7553(9) 0.8883(8) 0.1657(5) 0.103(4) Uani 1 1 d . . . H40 H 0.8165 0.8875 0.1924 0.123 Uiso 1 1 calc R B . C41 C 0.7403(11) 0.9311(8) 0.1163(6) 0.119(5) Uani 1 1 d . B . H41 H 0.7907 0.9602 0.1107 0.142 Uiso 1 1 calc R . . C42 C 0.6529(11) 0.9312(7) 0.0758(5) 0.103(4) Uani 1 1 d . . . H42 H 0.6431 0.9599 0.0423 0.124 Uiso 1 1 calc R B . C43 C 0.5780(8) 0.8879(6) 0.0847(4) 0.076(3) Uani 1 1 d . B . H43 H 0.5176 0.8885 0.0571 0.091 Uiso 1 1 calc R . . C44 C 0.4338(8) 0.7135(6) 0.1965(5) 0.084(3) Uani 1 1 d . . . H44A H 0.3835 0.7064 0.1603 0.101 Uiso 1 1 calc R . . H44B H 0.4572 0.6639 0.2111 0.101 Uiso 1 1 calc R . . C45 C 0.3915(12) 0.7488(10) 0.2369(6) 0.128(4) Uani 1 1 d DU . . C46 C 0.3909(12) 0.7305(10) 0.2920(6) 0.143(4) Uani 1 1 d DU . . H46 H 0.4226 0.6909 0.3151 0.172 Uiso 1 1 calc R . . C47 C 0.3319(13) 0.7849(11) 0.3047(8) 0.158(5) Uani 1 1 d DU . . H47 H 0.3128 0.7842 0.3383 0.189 Uiso 1 1 calc R . . C48 C 0.3035(13) 0.8409(12) 0.2630(7) 0.171(4) Uani 1 1 d DU . . H48 H 0.2673 0.8841 0.2640 0.205 Uiso 1 1 calc R . . O19 O 0.116(3) 0.193(3) 0.3223(19) 0.31(2) Uiso 0.50 1 d P . . O20 O 0.246(3) 0.564(2) 0.2297(17) 0.286(17) Uiso 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pr1 0.0649(4) 0.0388(3) 0.0736(4) 0.0006(2) 0.0187(3) 0.0110(2) N1 0.061(5) 0.042(4) 0.116(7) 0.020(4) 0.025(5) 0.015(4) N2 0.128(8) 0.054(5) 0.064(5) -0.010(4) -0.021(5) 0.044(5) N3 0.063(5) 0.072(5) 0.074(5) 0.020(4) 0.013(4) -0.013(4) N4 0.072(7) 0.051(5) 0.118(8) 0.001(5) 0.041(7) 0.018(4) N5 0.104(8) 0.095(8) 0.093(7) 0.013(6) 0.051(6) 0.012(6) N6 0.080(7) 0.083(7) 0.095(7) -0.017(6) 0.026(6) 0.009(5) O1 0.057(4) 0.039(3) 0.085(4) 0.010(3) 0.019(3) 0.007(3) O2 0.070(4) 0.039(3) 0.108(5) 0.010(3) 0.019(4) 0.013(3) O3 0.093(7) 0.092(7) 0.125(8) 0.007(7) 0.000(7) 0.021(6) O3' 0.099(12) 0.093(11) 0.147(16) 0.005(11) 0.023(12) 0.017(9) O4 0.065(4) 0.035(3) 0.072(4) -0.003(3) 0.001(3) 0.009(3) O5 0.088(5) 0.037(3) 0.095(5) -0.001(3) 0.028(4) 0.014(3) O6 0.196(8) 0.224(8) 0.126(7) -0.027(7) 0.000(7) 0.021(7) O7 0.062(4) 0.081(4) 0.066(4) 0.007(3) 0.013(3) -0.005(3) O8 0.065(4) 0.053(3) 0.071(4) 0.005(3) 0.009(3) 0.004(3) O9 0.152(7) 0.205(9) 0.127(6) -0.036(6) 0.038(6) -0.004(7) O10 0.073(5) 0.096(5) 0.081(5) 0.004(4) 0.024(4) 0.001(4) O11 0.070(5) 0.080(5) 0.102(6) -0.013(4) 0.026(4) 0.005(4) O12 0.093(6) 0.112(7) 0.167(8) 0.014(6) 0.073(6) 0.015(5) O13 0.106(6) 0.062(4) 0.099(5) 0.022(4) 0.040(5) 0.013(4) O14 0.108(6) 0.080(5) 0.117(6) -0.006(5) 0.068(5) 0.010(4) O15 0.172(10) 0.162(10) 0.154(9) 0.029(7) 0.108(8) -0.005(7) O16 0.107(6) 0.088(6) 0.070(4) -0.001(4) 0.009(4) 0.022(4) O17 0.111(6) 0.061(4) 0.102(5) -0.019(4) 0.017(5) 0.019(4) O18 0.110(7) 0.159(8) 0.082(5) -0.043(6) 0.006(5) -0.001(6) C1 0.058(5) 0.024(4) 0.071(5) 0.010(4) 0.020(5) 0.011(3) C2 0.064(6) 0.032(4) 0.056(5) 0.001(4) 0.008(4) 0.011(4) C3 0.058(5) 0.029(4) 0.069(6) 0.001(4) 0.003(5) 0.010(4) C4 0.056(5) 0.046(5) 0.066(6) 0.001(4) 0.009(5) 0.005(4) C5 0.054(5) 0.048(5) 0.069(6) -0.005(4) 0.013(5) 0.011(4) C6 0.052(5) 0.037(4) 0.074(6) -0.004(4) 0.007(5) 0.004(4) C7 0.079(7) 0.033(4) 0.083(6) 0.004(4) 0.026(5) 0.014(4) C8 0.119(10) 0.073(7) 0.090(8) -0.004(5) 0.038(7) -0.010(6) C9 0.075(7) 0.035(4) 0.092(7) -0.005(5) 0.004(6) 0.005(4) C10 0.075(7) 0.100(9) 0.111(9) 0.001(7) 0.026(7) -0.018(6) C11 0.064(6) 0.096(8) 0.075(7) 0.008(6) 0.018(6) -0.017(6) C12 0.065(6) 0.064(6) 0.092(7) -0.018(5) 0.008(5) -0.009(5) C13 0.061(6) 0.039(5) 0.064(5) 0.002(4) 0.011(5) 0.010(4) C14 0.061(6) 0.036(4) 0.054(5) 0.006(4) 0.016(4) 0.003(4) C15 0.058(6) 0.047(5) 0.054(5) 0.003(4) 0.019(4) 0.000(4) C16 0.065(6) 0.058(6) 0.087(7) 0.011(5) 0.034(5) 0.012(5) C17 0.069(7) 0.084(8) 0.102(8) 0.024(6) 0.038(6) 0.017(6) C18 0.062(7) 0.089(8) 0.099(8) 0.018(6) 0.024(6) -0.015(6) C19 0.081(8) 0.051(5) 0.079(6) 0.016(5) 0.026(6) -0.006(5) C20 0.063(7) 0.057(6) 0.171(12) 0.018(7) 0.045(7) 0.009(5) C21 0.091(7) 0.085(7) 0.110(7) 0.012(6) 0.016(6) 0.008(6) C22 0.100(7) 0.095(7) 0.115(7) 0.004(6) 0.017(6) 0.009(6) C23 0.092(7) 0.090(7) 0.116(7) 0.012(6) 0.013(6) 0.004(6) C24 0.092(6) 0.089(7) 0.121(7) 0.012(6) 0.015(6) 0.008(6) C20' 0.063(7) 0.057(6) 0.171(12) 0.018(7) 0.045(7) 0.009(5) C21' 0.081(6) 0.074(6) 0.103(7) -0.002(6) 0.016(6) 0.012(5) C22' 0.088(6) 0.090(6) 0.111(7) 0.008(6) 0.018(6) 0.008(6) C23' 0.093(6) 0.090(6) 0.125(7) 0.010(6) 0.010(6) 0.011(6) C24' 0.093(6) 0.085(6) 0.118(7) -0.003(6) 0.007(6) 0.011(6) C25 0.071(6) 0.043(5) 0.059(5) -0.008(4) 0.028(5) 0.009(4) C26 0.056(5) 0.037(4) 0.052(5) 0.001(4) 0.025(4) -0.002(4) C27 0.059(5) 0.036(4) 0.066(5) 0.000(4) 0.024(5) -0.003(4) C28 0.070(6) 0.043(5) 0.067(6) -0.002(4) 0.003(5) 0.009(4) C29 0.067(7) 0.074(7) 0.069(6) 0.007(5) 0.003(5) -0.003(5) C30 0.079(7) 0.068(7) 0.069(6) -0.006(5) 0.007(6) -0.013(5) C31 0.090(7) 0.047(5) 0.074(6) -0.008(5) 0.035(6) -0.007(5) C32 0.115(8) 0.094(7) 0.101(7) -0.020(6) -0.009(6) 0.045(6) C33 0.154(9) 0.180(9) 0.072(6) -0.040(7) -0.012(7) 0.053(8) C34 0.185(10) 0.239(10) 0.109(8) -0.048(8) -0.006(8) 0.052(9) C35 0.200(11) 0.224(11) 0.101(8) -0.041(8) 0.005(9) 0.069(10) C36 0.197(11) 0.223(11) 0.097(8) -0.048(8) 0.010(9) 0.021(10) C37 0.060(6) 0.042(4) 0.062(5) 0.009(4) 0.017(5) 0.003(4) C38 0.074(6) 0.050(5) 0.060(5) -0.001(4) 0.032(5) -0.001(4) C39 0.061(6) 0.084(7) 0.065(6) 0.003(5) 0.029(5) -0.003(5) C40 0.077(8) 0.148(12) 0.089(8) 0.007(8) 0.033(7) -0.028(8) C41 0.127(12) 0.156(13) 0.086(9) 0.011(9) 0.051(9) -0.061(10) C42 0.137(12) 0.112(10) 0.069(7) 0.006(7) 0.045(8) -0.042(9) C43 0.088(8) 0.072(6) 0.070(6) 0.009(5) 0.026(6) -0.006(6) C44 0.077(7) 0.084(7) 0.084(7) 0.031(6) 0.013(6) -0.023(6) C45 0.122(9) 0.182(10) 0.086(7) -0.005(8) 0.041(7) -0.048(8) C46 0.139(9) 0.195(11) 0.106(8) -0.017(8) 0.050(7) -0.037(8) C47 0.142(9) 0.216(12) 0.125(8) -0.025(8) 0.053(8) -0.045(9) C48 0.152(8) 0.219(10) 0.136(8) -0.041(8) 0.030(8) -0.007(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pr1 O5 2.398(5) . ? Pr1 O2 2.399(5) . ? Pr1 O8 2.410(6) . ? Pr1 O11 2.531(7) . ? Pr1 O14 2.536(7) . ? Pr1 O13 2.552(7) . ? Pr1 O10 2.555(7) . ? Pr1 O16 2.583(7) . ? Pr1 O17 2.584(7) . ? N1 C13 1.333(11) . ? N1 C20 1.449(12) . ? N1 H1 0.8600 . ? N2 C25 1.306(11) . ? N2 C32 1.477(13) . ? N2 H2 0.8600 . ? N3 C37 1.326(11) . ? N3 C44 1.477(12) . ? N3 H3 0.8600 . ? N4 O12 1.240(11) . ? N4 O10 1.250(11) . ? N4 O11 1.275(11) . ? N5 O15 1.218(11) . ? N5 O13 1.261(11) . ? N5 O14 1.272(11) . ? N6 O18 1.213(11) . ? N6 O17 1.254(11) . ? N6 O16 1.273(10) . ? O1 C15 1.379(9) . ? O1 C7 1.447(9) . ? O2 C13 1.252(9) . ? O3 C21 1.397(16) . ? O3 C24 1.403(16) . ? O3' C21' 1.438(15) . ? O3' C24' 1.449(15) . ? O4 C27 1.386(9) . ? O4 C9 1.444(9) . ? O5 C25 1.240(9) . ? O6 C33 1.333(12) . ? O6 C36 1.386(14) . ? O7 C39 1.384(10) . ? O7 C11 1.446(10) . ? O8 C37 1.231(9) . ? O9 C45 1.392(14) . ? O9 C48 1.424(14) . ? C1 C2 1.384(11) . ? C1 C6 1.394(11) . ? C1 C7 1.523(12) . ? C2 C3 1.403(12) . ? C2 C8 1.518(13) . ? C3 C4 1.406(12) . ? C3 C9 1.507(12) 1_545 ? C4 C5 1.410(12) . ? C4 C10 1.514(13) . ? C5 C6 1.394(12) . ? C5 C11 1.494(12) 2_645 ? C6 C12 1.523(11) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 C3 1.507(12) 1_565 ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C5 1.494(12) 2_655 ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.502(11) . ? C14 C19 1.390(12) . ? C14 C15 1.404(10) . ? C15 C16 1.359(12) . ? C16 C17 1.380(13) . ? C16 H16 0.9300 . ? C17 C18 1.361(14) . ? C17 H17 0.9300 . ? C18 C19 1.373(13) . ? C18 H18A 0.9300 . ? C19 H19 0.9300 . ? C20 C21 1.465(15) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.426(16) . ? C22 C23 1.461(16) . ? C22 H22 0.9300 . ? C23 C24 1.454(17) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C21' C22' 1.391(15) . ? C22' C23' 1.405(16) . ? C22' H22' 0.9300 . ? C23' C24' 1.425(16) . ? C23' H23' 0.9300 . ? C24' H24' 0.9300 . ? C25 C26 1.484(11) . ? C26 C27 1.398(10) . ? C26 C31 1.425(11) . ? C27 C28 1.382(11) . ? C28 C29 1.379(12) . ? C28 H28 0.9300 . ? C29 C30 1.354(13) . ? C29 H29 0.9300 . ? C30 C31 1.375(13) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C32 C33 1.430(17) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.357(16) . ? C34 C35 1.417(15) . ? C34 H34 0.9300 . ? C35 C36 1.316(15) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C37 C38 1.492(12) . ? C38 C43 1.395(12) . ? C38 C39 1.408(12) . ? C39 C40 1.371(13) . ? C40 C41 1.378(16) . ? C40 H40 0.9300 . ? C41 C42 1.353(17) . ? C41 H41 0.9300 . ? C42 C43 1.390(14) . ? C42 H42 0.9300 . ? C43 H43 0.9300 . ? C44 C45 1.435(18) . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C45 C46 1.373(14) . ? C46 C47 1.375(15) . ? C46 H46 0.9300 . ? C47 C48 1.388(15) . ? C47 H47 0.9300 . ? C48 H48 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Pr1 O2 151.3(2) . . ? O5 Pr1 O8 85.8(2) . . ? O2 Pr1 O8 77.1(2) . . ? O5 Pr1 O11 76.5(2) . . ? O2 Pr1 O11 96.2(2) . . ? O8 Pr1 O11 128.3(2) . . ? O5 Pr1 O14 119.9(2) . . ? O2 Pr1 O14 81.5(2) . . ? O8 Pr1 O14 84.3(2) . . ? O11 Pr1 O14 146.2(3) . . ? O5 Pr1 O13 70.5(2) . . ? O2 Pr1 O13 128.3(2) . . ? O8 Pr1 O13 82.2(2) . . ? O11 Pr1 O13 132.8(2) . . ? O14 Pr1 O13 49.5(2) . . ? O5 Pr1 O10 76.0(2) . . ? O2 Pr1 O10 78.2(2) . . ? O8 Pr1 O10 78.9(2) . . ? O11 Pr1 O10 49.9(3) . . ? O14 Pr1 O10 156.1(3) . . ? O13 Pr1 O10 142.4(2) . . ? O5 Pr1 O16 84.7(2) . . ? O2 Pr1 O16 119.7(2) . . ? O8 Pr1 O16 155.0(2) . . ? O11 Pr1 O16 71.3(3) . . ? O14 Pr1 O16 80.5(3) . . ? O13 Pr1 O16 72.8(2) . . ? O10 Pr1 O16 120.7(3) . . ? O5 Pr1 O17 130.4(2) . . ? O2 Pr1 O17 70.6(2) . . ? O8 Pr1 O17 143.7(2) . . ? O11 Pr1 O17 72.4(3) . . ? O14 Pr1 O17 75.1(3) . . ? O13 Pr1 O17 105.1(3) . . ? O10 Pr1 O17 109.3(3) . . ? O16 Pr1 O17 49.3(2) . . ? C13 N1 C20 123.9(7) . . ? C13 N1 H1 118.0 . . ? C20 N1 H1 118.0 . . ? C25 N2 C32 125.4(8) . . ? C25 N2 H2 117.3 . . ? C32 N2 H2 117.3 . . ? C37 N3 C44 124.3(8) . . ? C37 N3 H3 117.9 . . ? C44 N3 H3 117.9 . . ? O12 N4 O10 122.9(11) . . ? O12 N4 O11 120.7(11) . . ? O10 N4 O11 116.3(9) . . ? O15 N5 O13 124.8(11) . . ? O15 N5 O14 120.9(11) . . ? O13 N5 O14 114.4(9) . . ? O18 N6 O17 122.4(11) . . ? O18 N6 O16 120.7(10) . . ? O17 N6 O16 116.9(9) . . ? C15 O1 C7 118.8(6) . . ? C13 O2 Pr1 166.4(6) . . ? C21 O3 C24 110.0(11) . . ? C21' O3' C24' 105.1(9) . . ? C27 O4 C9 117.9(6) . . ? C25 O5 Pr1 161.3(6) . . ? C33 O6 C36 112.4(14) . . ? C39 O7 C11 117.2(7) . . ? C37 O8 Pr1 163.4(6) . . ? C45 O9 C48 107.0(14) . . ? N4 O10 Pr1 96.7(6) . . ? N4 O11 Pr1 97.1(6) . . ? N5 O13 Pr1 97.9(6) . . ? N5 O14 Pr1 98.3(6) . . ? N6 O16 Pr1 96.7(6) . . ? N6 O17 Pr1 97.1(6) . . ? C2 C1 C6 120.4(8) . . ? C2 C1 C7 121.2(8) . . ? C6 C1 C7 118.4(8) . . ? C1 C2 C3 119.5(8) . . ? C1 C2 C8 121.3(9) . . ? C3 C2 C8 119.2(8) . . ? C2 C3 C4 120.8(8) . . ? C2 C3 C9 120.0(8) . 1_545 ? C4 C3 C9 119.2(9) . 1_545 ? C3 C4 C5 118.5(8) . . ? C3 C4 C10 120.3(8) . . ? C5 C4 C10 121.2(9) . . ? C6 C5 C4 120.0(8) . . ? C6 C5 C11 119.2(8) . 2_645 ? C4 C5 C11 120.7(8) . 2_645 ? C1 C6 C5 120.3(8) . . ? C1 C6 C12 119.7(8) . . ? C5 C6 C12 119.9(8) . . ? O1 C7 C1 106.4(6) . . ? O1 C7 H7A 110.4 . . ? C1 C7 H7A 110.4 . . ? O1 C7 H7B 110.4 . . ? C1 C7 H7B 110.4 . . ? H7A C7 H7B 108.6 . . ? C2 C8 H8A 109.5 . . ? C2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O4 C9 C3 109.8(7) . 1_565 ? O4 C9 H9A 109.7 . . ? C3 C9 H9A 109.7 1_565 . ? O4 C9 H9B 109.7 . . ? C3 C9 H9B 109.7 1_565 . ? H9A C9 H9B 108.2 . . ? C4 C10 H10A 109.5 . . ? C4 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C4 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O7 C11 C5 110.1(7) . 2_655 ? O7 C11 H11A 109.6 . . ? C5 C11 H11A 109.6 2_655 . ? O7 C11 H11B 109.6 . . ? C5 C11 H11B 109.6 2_655 . ? H11A C11 H11B 108.2 . . ? C6 C12 H12A 109.5 . . ? C6 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C6 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O2 C13 N1 119.9(8) . . ? O2 C13 C14 120.6(8) . . ? N1 C13 C14 119.4(7) . . ? C19 C14 C15 117.6(8) . . ? C19 C14 C13 117.4(7) . . ? C15 C14 C13 125.0(7) . . ? C16 C15 O1 122.2(8) . . ? C16 C15 C14 121.0(8) . . ? O1 C15 C14 116.8(7) . . ? C15 C16 C17 119.8(9) . . ? C15 C16 H16 120.1 . . ? C17 C16 H16 120.1 . . ? C18 C17 C16 120.6(10) . . ? C18 C17 H17 119.7 . . ? C16 C17 H17 119.7 . . ? C17 C18 C19 119.9(10) . . ? C17 C18 H18A 120.0 . . ? C19 C18 H18A 120.0 . . ? C18 C19 C14 121.0(9) . . ? C18 C19 H19 119.5 . . ? C14 C19 H19 119.5 . . ? N1 C20 C21 111.7(14) . . ? N1 C20 H20A 109.3 . . ? C21 C20 H20A 109.3 . . ? N1 C20 H20B 109.3 . . ? C21 C20 H20B 109.3 . . ? H20A C20 H20B 107.9 . . ? O3 C21 C22 109.3(10) . . ? O3 C21 C20 105.3(17) . . ? C22 C21 C20 144.3(19) . . ? C21 C22 C23 106.2(10) . . ? C21 C22 H22 126.9 . . ? C23 C22 H22 126.9 . . ? C24 C23 C22 107.4(10) . . ? C24 C23 H23 126.3 . . ? C22 C23 H23 126.3 . . ? O3 C24 C23 107.0(11) . . ? O3 C24 H24 126.5 . . ? C23 C24 H24 126.5 . . ? C22' C21' O3' 109.4(10) . . ? C21' C22' C23' 109.4(11) . . ? C21' C22' H22' 125.3 . . ? C23' C22' H22' 125.3 . . ? C22' C23' C24' 107.3(10) . . ? C22' C23' H23' 126.4 . . ? C24' C23' H23' 126.4 . . ? C23' C24' O3' 108.7(10) . . ? C23' C24' H24' 125.6 . . ? O3' C24' H24' 125.6 . . ? O5 C25 N2 120.1(8) . . ? O5 C25 C26 121.6(8) . . ? N2 C25 C26 118.3(7) . . ? C27 C26 C31 116.7(8) . . ? C27 C26 C25 126.8(7) . . ? C31 C26 C25 116.6(7) . . ? C28 C27 O4 122.8(7) . . ? C28 C27 C26 121.1(8) . . ? O4 C27 C26 116.0(7) . . ? C29 C28 C27 119.6(8) . . ? C29 C28 H28 120.2 . . ? C27 C28 H28 120.2 . . ? C30 C29 C28 121.6(9) . . ? C30 C29 H29 119.2 . . ? C28 C29 H29 119.2 . . ? C29 C30 C31 119.5(9) . . ? C29 C30 H30 120.2 . . ? C31 C30 H30 120.2 . . ? C30 C31 C26 121.5(8) . . ? C30 C31 H31 119.3 . . ? C26 C31 H31 119.3 . . ? C33 C32 N2 110.1(10) . . ? C33 C32 H32A 109.6 . . ? N2 C32 H32A 109.6 . . ? C33 C32 H32B 109.6 . . ? N2 C32 H32B 109.6 . . ? H32A C32 H32B 108.1 . . ? O6 C33 C34 101.6(13) . . ? O6 C33 C32 124.3(14) . . ? C34 C33 C32 130.5(14) . . ? C33 C34 C35 109.5(16) . . ? C33 C34 H34 125.2 . . ? C35 C34 H34 125.2 . . ? C36 C35 C34 105.3(16) . . ? C36 C35 H35 127.3 . . ? C34 C35 H35 127.3 . . ? C35 C36 O6 106.2(15) . . ? C35 C36 H36 126.9 . . ? O6 C36 H36 126.9 . . ? O8 C37 N3 121.2(8) . . ? O8 C37 C38 119.6(8) . . ? N3 C37 C38 119.2(8) . . ? C43 C38 C39 117.8(9) . . ? C43 C38 C37 116.8(9) . . ? C39 C38 C37 125.3(8) . . ? C40 C39 O7 121.8(10) . . ? C40 C39 C38 119.2(9) . . ? O7 C39 C38 118.9(8) . . ? C39 C40 C41 121.5(12) . . ? C39 C40 H40 119.3 . . ? C41 C40 H40 119.3 . . ? C42 C41 C40 120.5(11) . . ? C42 C41 H41 119.7 . . ? C40 C41 H41 119.7 . . ? C41 C42 C43 119.2(11) . . ? C41 C42 H42 120.4 . . ? C43 C42 H42 120.4 . . ? C42 C43 C38 121.5(10) . . ? C42 C43 H43 119.2 . . ? C38 C43 H43 119.2 . . ? C45 C44 N3 115.0(10) . . ? C45 C44 H44A 108.5 . . ? N3 C44 H44A 108.5 . . ? C45 C44 H44B 108.5 . . ? N3 C44 H44B 108.5 . . ? H44A C44 H44B 107.5 . . ? C46 C45 O9 111.7(15) . . ? C46 C45 C44 132.9(16) . . ? O9 C45 C44 115.3(12) . . ? C45 C46 C47 103.2(16) . . ? C45 C46 H46 128.4 . . ? C47 C46 H46 128.4 . . ? C46 C47 C48 114.3(17) . . ? C46 C47 H47 122.9 . . ? C48 C47 H47 122.9 . . ? C47 C48 O9 103.4(16) . . ? C47 C48 H48 128.3 . . ? O9 C48 H48 128.3 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.006 _refine_diff_density_min -1.020 _refine_diff_density_rms 0.112 # Attachment '2.cif' data_060517f _database_code_depnum_ccdc_archive 'CCDC 672451' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42.50 H43 N6 Nd O18.50' _chemical_formula_weight 1078.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.657(7) _cell_length_b 16.373(7) _cell_length_c 18.370(9) _cell_angle_alpha 90.00 _cell_angle_beta 98.696(7) _cell_angle_gamma 90.00 _cell_volume 4952(4) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 4365 _cell_measurement_theta_min 2.474 _cell_measurement_theta_max 20.395 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.446 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2192 _exptl_absorpt_coefficient_mu 1.125 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7289 _exptl_absorpt_correction_T_max 0.7661 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 25588 _diffrn_reflns_av_R_equivalents 0.0901 _diffrn_reflns_av_sigmaI/netI 0.1010 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8712 _reflns_number_gt 3963 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1304P)^2^+0.9974P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8712 _refine_ls_number_parameters 619 _refine_ls_number_restraints 616 _refine_ls_R_factor_all 0.1548 _refine_ls_R_factor_gt 0.0702 _refine_ls_wR_factor_ref 0.2545 _refine_ls_wR_factor_gt 0.1880 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.029 _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 Nd1 Nd 0.21623(3) 0.00107(3) 0.18542(3) 0.0556(2) Uani 1 1 d . . . N1 N 0.2554(6) 0.2595(6) 0.1263(7) 0.100(4) Uani 1 1 d . . . H1 H 0.2501 0.3116 0.1293 0.120 Uiso 1 1 calc R . . N2 N 0.4757(7) 0.0384(8) 0.2336(7) 0.114(4) Uani 1 1 d . . . H2 H 0.5273 0.0332 0.2352 0.137 Uiso 1 1 calc R . . N3 N 0.1303(5) 0.4964(5) 0.4489(5) 0.063(2) Uani 1 1 d . . . H3 H 0.1157 0.5115 0.4040 0.076 Uiso 1 1 calc R . . N4 N 0.2661(8) 0.0317(11) 0.3410(9) 0.108(3) Uani 1 1 d U . . N5 N 0.0389(6) 0.0183(5) 0.1927(6) 0.066(2) Uani 1 1 d U . . N6 N 0.2281(10) -0.1755(8) 0.1926(7) 0.107(4) Uani 1 1 d U . . O1 O 0.1865(4) 0.3756(4) 0.2001(4) 0.063(2) Uani 1 1 d . . . O2 O 0.4023(5) 0.4626(5) 0.3175(5) 0.081(2) Uani 1 1 d . . . O3 O 0.2334(4) 0.5629(4) 0.3538(4) 0.0596(19) Uani 1 1 d . . . O4 O 0.2003(4) 0.1377(4) 0.1412(5) 0.069(2) Uani 1 1 d . . . O5 O 0.4360(9) 0.2680(9) 0.1858(10) 0.177(4) Uani 1 1 d U . . O6 O 0.3554(4) 0.0250(5) 0.1742(6) 0.091(3) Uani 1 1 d . . . O7 O 0.5548(9) 0.1727(9) 0.3291(9) 0.180(4) Uani 1 1 d U . . O8 O 0.2026(4) 0.5277(5) 0.5565(4) 0.063(2) Uani 1 1 d . . . O9 O 0.1963(7) 0.3238(6) 0.4322(6) 0.117(3) Uani 1 1 d U . . O10 O 0.2520(6) 0.0891(6) 0.2983(6) 0.101(3) Uani 1 1 d U . . O11 O 0.2623(6) -0.0389(7) 0.3178(6) 0.109(3) Uani 1 1 d U . . O12 O 0.2882(8) 0.0481(9) 0.4050(7) 0.158(4) Uani 1 1 d U . . O13 O 0.0926(5) 0.0215(5) 0.2497(5) 0.085(2) Uani 1 1 d U . . O14 O 0.0644(4) 0.0042(4) 0.1338(4) 0.0654(18) Uani 1 1 d U . . O15 O -0.0312(4) 0.0295(5) 0.1971(5) 0.081(2) Uani 1 1 d U . . O16 O 0.1597(6) -0.1395(6) 0.1906(5) 0.103(3) Uani 1 1 d U . . O17 O 0.2907(7) -0.1338(6) 0.1903(6) 0.109(3) Uani 1 1 d U . . O18 O 0.2297(9) -0.2522(6) 0.1907(6) 0.163(5) Uani 1 1 d U . . O19 O 1.0000 0.5000 0.0000 0.38(3) Uani 1 2 d SDU . . H19 H 1.0430 0.5085 -0.0152 0.569 Uiso 0.50 1 d PR . . C1 C 0.2689(6) 0.4847(5) 0.2524(6) 0.054(3) Uani 1 1 d . . . C2 C 0.3040(7) 0.4927(7) 0.1804(6) 0.069(3) Uani 1 1 d . . . H2A H 0.3225 0.4392 0.1673 0.083 Uiso 1 1 calc R . . H2B H 0.3512 0.5280 0.1892 0.083 Uiso 1 1 calc R . . C3 C 0.2458(10) 0.5265(11) 0.1142(9) 0.133(6) Uani 1 1 d . . . H3A H 0.2737 0.5302 0.0723 0.199 Uiso 1 1 calc R . . H3B H 0.2274 0.5798 0.1260 0.199 Uiso 1 1 calc R . . H3C H 0.1999 0.4907 0.1031 0.199 Uiso 1 1 calc R . . C4 C 0.1836(5) 0.4498(5) 0.2398(6) 0.051(3) Uani 1 1 d . . . H4A H 0.1651 0.4396 0.2865 0.061 Uiso 1 1 calc R . . H4B H 0.1465 0.4879 0.2118 0.061 Uiso 1 1 calc R . . C5 C 0.3194(6) 0.4308(7) 0.3078(6) 0.065(3) Uani 1 1 d . . . H5A H 0.2984 0.4318 0.3542 0.078 Uiso 1 1 calc R . . H5B H 0.3183 0.3749 0.2901 0.078 Uiso 1 1 calc R . . C6 C 0.2650(6) 0.5702(6) 0.2858(6) 0.062(3) Uani 1 1 d . . . H6A H 0.3189 0.5942 0.2946 0.074 Uiso 1 1 calc R . . H6B H 0.2302 0.6053 0.2521 0.074 Uiso 1 1 calc R . . C7 C 0.1154(6) 0.3345(6) 0.1826(6) 0.057(3) Uani 1 1 d . . . C8 C 0.0405(6) 0.3663(7) 0.1926(7) 0.071(3) Uani 1 1 d . . . H8 H 0.0367 0.4191 0.2105 0.085 Uiso 1 1 calc R . . C9 C -0.0286(6) 0.3187(7) 0.1758(7) 0.081(4) Uani 1 1 d . . . H9 H -0.0787 0.3398 0.1828 0.097 Uiso 1 1 calc R . . C10 C -0.0245(6) 0.2420(7) 0.1493(8) 0.083(4) Uani 1 1 d . . . H10 H -0.0716 0.2112 0.1379 0.100 Uiso 1 1 calc R . . C11 C 0.0485(6) 0.2099(7) 0.1393(7) 0.072(3) Uani 1 1 d . . . H11 H 0.0505 0.1569 0.1215 0.086 Uiso 1 1 calc R . . C12 C 0.1196(5) 0.2539(6) 0.1548(6) 0.054(3) Uani 1 1 d . . . C13 C 0.1969(6) 0.2123(7) 0.1420(7) 0.063(3) Uani 1 1 d . . . C14 C 0.3287(9) 0.2269(10) 0.1041(11) 0.134(4) Uani 1 1 d U . . H14A H 0.3401 0.1747 0.1285 0.161 Uiso 1 1 calc R . . H14B H 0.3180 0.2163 0.0516 0.161 Uiso 1 1 calc R . . C15 C 0.3982(11) 0.2746(12) 0.1182(13) 0.131(4) Uani 1 1 d U . . C16 C 0.4323(12) 0.3325(12) 0.0850(13) 0.153(5) Uani 1 1 d U . . H16 H 0.4141 0.3545 0.0388 0.183 Uiso 1 1 calc R . . C17 C 0.5030(12) 0.3551(12) 0.1342(14) 0.155(5) Uani 1 1 d U . . H17 H 0.5409 0.3940 0.1251 0.185 Uiso 1 1 calc R . . C18 C 0.5056(14) 0.3139(14) 0.1913(14) 0.171(5) Uani 1 1 d U . . H18 H 0.5475 0.3141 0.2310 0.205 Uiso 1 1 calc R . . C19 C 0.4571(7) 0.4349(8) 0.3742(7) 0.079(3) Uani 1 1 d U . . C20 C 0.4355(8) 0.3840(9) 0.4275(9) 0.104(4) Uani 1 1 d U . . H20 H 0.3826 0.3644 0.4225 0.125 Uiso 1 1 calc R . . C21 C 0.4919(8) 0.3603(10) 0.4904(8) 0.111(4) Uani 1 1 d U . . H21 H 0.4751 0.3300 0.5282 0.133 Uiso 1 1 calc R . . C22 C 0.5692(8) 0.3827(10) 0.4934(9) 0.115(4) Uani 1 1 d U . . H22 H 0.6080 0.3655 0.5322 0.138 Uiso 1 1 calc R . . C23 C 0.5913(8) 0.4324(9) 0.4377(8) 0.105(4) Uani 1 1 d U . . H23 H 0.6456 0.4473 0.4406 0.126 Uiso 1 1 calc R . . C24 C 0.5384(7) 0.4600(9) 0.3799(8) 0.086(3) Uani 1 1 d U . . C25 C 0.4297(8) 0.0079(7) 0.1769(8) 0.085(3) Uani 1 1 d U . . C26 C 0.4476(10) 0.0808(11) 0.2954(10) 0.132(3) Uani 1 1 d U . . H26A H 0.4121 0.1248 0.2753 0.159 Uiso 1 1 calc R . . H26B H 0.4148 0.0427 0.3187 0.159 Uiso 1 1 calc R . . C27 C 0.5049(11) 0.1133(12) 0.3496(11) 0.138(4) Uani 1 1 d DU . . C28 C 0.5328(12) 0.0905(13) 0.4199(12) 0.163(5) Uani 1 1 d DU . . H28 H 0.5167 0.0443 0.4435 0.195 Uiso 1 1 calc R . . C29 C 0.5880(11) 0.1462(12) 0.4501(12) 0.160(5) Uani 1 1 d DU . . H29 H 0.6111 0.1500 0.4993 0.192 Uiso 1 1 calc R . . C30 C 0.6029(12) 0.1954(13) 0.3941(12) 0.163(5) Uani 1 1 d DU . . H30 H 0.6401 0.2382 0.3987 0.196 Uiso 1 1 calc R . . C31 C 0.2270(6) 0.6323(6) 0.3945(6) 0.054(3) Uani 1 1 d . . . C32 C 0.2493(6) 0.7095(6) 0.3711(7) 0.067(3) Uani 1 1 d . . . H32 H 0.2696 0.7153 0.3269 0.080 Uiso 1 1 calc R . . C33 C 0.2407(8) 0.7771(7) 0.4151(8) 0.086(4) Uani 1 1 d . . . H33 H 0.2524 0.8289 0.3987 0.103 Uiso 1 1 calc R . . C34 C 0.2154(9) 0.7689(7) 0.4818(8) 0.091(4) Uani 1 1 d . . . H34 H 0.2121 0.8139 0.5122 0.109 Uiso 1 1 calc R . . C35 C 0.1947(8) 0.6911(7) 0.5032(7) 0.082(4) Uani 1 1 d . . . H35 H 0.1755 0.6851 0.5478 0.099 Uiso 1 1 calc R . . C36 C 0.2016(6) 0.6235(6) 0.4614(6) 0.053(3) Uani 1 1 d . . . C37 C 0.1784(6) 0.5444(6) 0.4921(7) 0.056(3) Uani 1 1 d . . . C38 C 0.0995(8) 0.4174(7) 0.4726(7) 0.081(3) Uani 1 1 d U . . H38A H 0.1235 0.4066 0.5232 0.098 Uiso 1 1 calc R . . H38B H 0.0411 0.4209 0.4709 0.098 Uiso 1 1 calc R . . C39 C 0.1185(10) 0.3492(8) 0.4256(9) 0.093(3) Uani 1 1 d U . . C40 C 0.0726(11) 0.3021(8) 0.3765(9) 0.112(4) Uani 1 1 d U . . H40 H 0.0170 0.3072 0.3612 0.134 Uiso 1 1 calc R . . C41 C 0.1252(11) 0.2423(9) 0.3520(9) 0.114(4) Uani 1 1 d U . . H41 H 0.1105 0.1999 0.3189 0.136 Uiso 1 1 calc R . . C42 C 0.1968(11) 0.2589(9) 0.3850(10) 0.115(4) Uani 1 1 d U . . H42 H 0.2433 0.2305 0.3777 0.138 Uiso 1 1 calc R . . C43 C 0.973(5) 0.566(3) 0.046(4) 0.34(3) Uani 0.50 1 d PDU . . H43A H 1.0099 0.5702 0.0915 0.517 Uiso 0.50 1 calc PR . . H43B H 0.9194 0.5542 0.0566 0.517 Uiso 0.50 1 calc PR . . H43C H 0.9721 0.6172 0.0202 0.517 Uiso 0.50 1 calc PR . . 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 0.0438(3) 0.0502(3) 0.0708(4) -0.0012(3) 0.0020(2) 0.0051(3) N1 0.067(7) 0.054(6) 0.191(14) -0.021(7) 0.058(8) -0.009(5) N2 0.065(7) 0.152(11) 0.122(11) -0.072(9) -0.001(7) 0.018(7) N3 0.063(5) 0.065(5) 0.058(5) -0.003(5) -0.001(4) -0.016(5) N4 0.098(7) 0.131(8) 0.092(8) -0.012(7) 0.002(7) 0.000(7) N5 0.052(5) 0.076(6) 0.069(6) 0.006(5) 0.002(5) -0.011(4) N6 0.162(10) 0.067(7) 0.094(7) 0.006(6) 0.023(8) 0.017(7) O1 0.037(4) 0.053(4) 0.097(6) -0.019(4) 0.008(4) -0.006(3) O2 0.054(5) 0.093(5) 0.094(7) 0.027(5) 0.001(4) -0.010(4) O3 0.052(4) 0.043(4) 0.085(6) -0.003(4) 0.017(4) -0.007(3) O4 0.051(4) 0.040(4) 0.113(7) -0.002(4) -0.004(4) 0.005(3) O5 0.141(7) 0.160(7) 0.227(9) -0.030(8) 0.020(7) -0.026(7) O6 0.032(4) 0.098(6) 0.140(8) 0.006(5) 0.001(4) 0.015(4) O7 0.150(7) 0.181(8) 0.201(8) -0.038(7) -0.006(7) -0.008(7) O8 0.060(5) 0.074(5) 0.055(5) 0.005(4) 0.005(4) -0.010(4) O9 0.125(7) 0.075(5) 0.152(7) -0.008(5) 0.028(6) 0.003(5) O10 0.088(5) 0.099(6) 0.112(6) -0.035(5) 0.007(5) 0.004(5) O11 0.118(6) 0.102(5) 0.102(6) 0.007(5) 0.001(5) 0.014(5) O12 0.165(10) 0.194(10) 0.107(9) -0.038(8) -0.001(8) 0.017(9) O13 0.064(4) 0.118(6) 0.074(5) -0.004(4) 0.010(4) 0.000(4) O14 0.056(4) 0.072(4) 0.068(5) 0.001(4) 0.011(4) -0.010(4) O15 0.040(4) 0.103(6) 0.102(7) 0.011(5) 0.015(4) -0.005(4) O16 0.121(6) 0.080(5) 0.110(6) 0.008(5) 0.026(5) -0.010(5) O17 0.120(7) 0.087(6) 0.116(7) -0.003(5) 0.008(6) 0.030(5) O18 0.308(14) 0.057(6) 0.127(9) 0.004(6) 0.042(10) 0.022(8) O19 0.46(6) 0.30(6) 0.43(7) 0.13(5) 0.24(4) 0.14(4) C1 0.046(5) 0.040(6) 0.076(8) -0.004(5) 0.011(5) -0.002(4) C2 0.059(6) 0.070(7) 0.082(8) -0.001(7) 0.022(6) 0.002(6) C3 0.126(14) 0.188(17) 0.086(12) 0.032(11) 0.021(10) -0.015(12) C4 0.045(6) 0.034(5) 0.076(8) -0.005(5) 0.011(5) -0.003(4) C5 0.038(6) 0.063(7) 0.094(9) -0.014(6) 0.015(6) -0.014(5) C6 0.047(6) 0.058(7) 0.081(8) -0.005(6) 0.013(6) -0.009(5) C7 0.037(5) 0.052(6) 0.081(8) -0.008(5) 0.006(5) -0.004(5) C8 0.039(6) 0.061(7) 0.111(10) -0.020(6) 0.007(6) 0.006(5) C9 0.031(6) 0.083(9) 0.127(12) -0.029(8) 0.004(6) 0.002(6) C10 0.039(6) 0.057(7) 0.151(13) -0.026(8) 0.007(7) -0.010(6) C11 0.055(7) 0.056(7) 0.101(10) -0.010(6) -0.003(6) -0.002(6) C12 0.038(5) 0.047(6) 0.076(8) -0.006(5) 0.009(5) -0.002(5) C13 0.045(6) 0.053(7) 0.089(9) -0.011(6) 0.005(6) -0.002(5) C14 0.087(8) 0.122(9) 0.205(11) -0.055(8) 0.058(8) -0.014(7) C15 0.094(8) 0.118(9) 0.188(11) -0.056(9) 0.049(8) -0.030(7) C16 0.118(9) 0.140(10) 0.207(11) -0.054(9) 0.047(9) -0.020(8) C17 0.115(8) 0.144(10) 0.215(12) -0.038(9) 0.061(9) -0.037(8) C18 0.131(8) 0.159(9) 0.219(11) -0.042(9) 0.019(9) -0.018(8) C19 0.054(6) 0.098(7) 0.084(7) 0.034(6) 0.006(5) 0.001(6) C20 0.064(6) 0.129(8) 0.118(8) 0.044(7) 0.007(6) -0.009(6) C21 0.075(7) 0.135(8) 0.118(8) 0.048(7) 0.006(7) -0.017(7) C22 0.072(6) 0.140(8) 0.127(8) 0.044(7) -0.003(6) -0.008(7) C23 0.071(7) 0.129(8) 0.110(8) 0.040(7) -0.003(6) -0.007(7) C24 0.054(6) 0.106(7) 0.093(7) 0.025(6) -0.001(6) 0.004(6) C25 0.064(7) 0.079(7) 0.104(8) -0.025(7) -0.013(6) 0.007(6) C26 0.101(6) 0.146(7) 0.145(7) -0.036(6) 0.004(6) -0.013(6) C27 0.102(8) 0.155(9) 0.152(9) -0.043(8) 0.002(8) -0.029(7) C28 0.134(9) 0.186(10) 0.163(10) -0.028(9) 0.006(9) -0.034(8) C29 0.133(9) 0.183(10) 0.158(10) -0.035(9) 0.006(9) -0.033(8) C30 0.132(8) 0.174(9) 0.173(9) -0.033(8) -0.011(8) -0.025(8) C31 0.045(6) 0.044(6) 0.068(8) 0.002(5) -0.005(5) -0.001(5) C32 0.066(7) 0.049(6) 0.081(9) -0.004(6) -0.001(6) -0.012(6) C33 0.099(10) 0.041(7) 0.105(12) 0.012(7) -0.020(9) 0.000(6) C34 0.139(13) 0.057(8) 0.070(10) -0.013(7) -0.009(9) 0.001(8) C35 0.118(11) 0.056(7) 0.069(9) 0.002(6) 0.001(8) 0.001(7) C36 0.061(7) 0.037(5) 0.057(7) -0.002(5) -0.005(5) -0.003(5) C37 0.043(6) 0.052(6) 0.070(8) -0.007(6) 0.004(6) 0.006(5) C38 0.092(7) 0.052(6) 0.104(8) -0.002(5) 0.028(6) -0.017(5) C39 0.106(8) 0.054(6) 0.121(8) 0.013(6) 0.017(7) -0.014(6) C40 0.143(9) 0.072(7) 0.123(8) 0.006(7) 0.024(8) -0.013(7) C41 0.142(8) 0.074(7) 0.126(8) -0.005(6) 0.024(7) -0.006(7) C42 0.134(8) 0.081(7) 0.134(8) -0.007(6) 0.032(7) 0.009(7) C43 0.41(6) 0.28(7) 0.39(8) 0.14(5) 0.22(5) 0.18(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 Nd1 O4 2.381(7) . ? Nd1 O6 2.391(8) . ? Nd1 O8 2.391(8) 4_565 ? Nd1 O16 2.494(9) . ? Nd1 O10 2.521(9) . ? Nd1 O11 2.523(10) . ? Nd1 O17 2.528(9) . ? Nd1 O13 2.546(8) . ? Nd1 O14 2.564(7) . ? N1 C13 1.310(12) . ? N1 C14 1.447(15) . ? N1 H1 0.8600 . ? N2 C25 1.297(15) . ? N2 C26 1.467(18) . ? N2 H2 0.8600 . ? N3 C37 1.302(13) . ? N3 C38 1.482(12) . ? N3 H3 0.8600 . ? N4 O12 1.209(16) . ? N4 O10 1.224(16) . ? N4 O11 1.231(18) . ? N5 O15 1.198(11) . ? N5 O14 1.242(12) . ? N5 O13 1.272(12) . ? N6 O17 1.251(15) . ? N6 O18 1.257(15) . ? N6 O16 1.280(15) . ? O1 C7 1.356(10) . ? O1 C4 1.422(10) . ? O2 C19 1.356(13) . ? O2 C5 1.461(11) . ? O3 C31 1.373(11) . ? O3 C6 1.433(12) . ? O4 C13 1.223(11) . ? O5 C15 1.31(2) . ? O5 C18 1.37(2) . ? O6 C25 1.263(14) . ? O7 C27 1.37(2) . ? O7 C30 1.38(2) . ? O8 C37 1.222(12) . ? O8 Nd1 2.391(8) 4_566 ? O9 C39 1.349(16) . ? O9 C42 1.372(17) . ? O19 C43 1.49(2) 3_765 ? O19 C43 1.49(2) . ? O19 H19 0.8200 . ? C1 C5 1.504(14) . ? C1 C4 1.515(12) . ? C1 C2 1.529(15) . ? C1 C6 1.534(13) . ? C2 C3 1.540(18) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.391(13) . ? C7 C12 1.420(13) . ? C8 C9 1.385(13) . ? C8 H8 0.9300 . ? C9 C10 1.351(14) . ? C9 H9 0.9300 . ? C10 C11 1.363(14) . ? C10 H10 0.9300 . ? C11 C12 1.379(13) . ? C11 H11 0.9300 . ? C12 C13 1.506(13) . ? C14 C15 1.388(19) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.30(2) . ? C16 C17 1.42(2) . ? C16 H16 0.9300 . ? C17 C18 1.24(3) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C20 1.376(16) . ? C19 C24 1.404(15) . ? C20 C21 1.428(17) . ? C20 H20 0.9300 . ? C21 C22 1.332(16) . ? C21 H21 0.9300 . ? C22 C23 1.402(18) . ? C22 H22 0.9300 . ? C23 C24 1.350(16) . ? C23 H23 0.9300 . ? C24 C25 1.467(18) 2_655 ? C25 C24 1.467(18) 2_645 ? C26 C27 1.38(2) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.357(16) . ? C28 C29 1.352(15) . ? C28 H28 0.9300 . ? C29 C30 1.359(16) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C36 1.366(14) . ? C31 C32 1.402(13) . ? C32 C33 1.392(16) . ? C32 H32 0.9300 . ? C33 C34 1.361(18) . ? C33 H33 0.9300 . ? C34 C35 1.391(16) . ? C34 H34 0.9300 . ? C35 C36 1.363(14) . ? C35 H35 0.9300 . ? C36 C37 1.486(14) . ? C38 C39 1.475(17) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 C40 1.336(18) . ? C40 C41 1.431(19) . ? C40 H40 0.9300 . ? C41 C42 1.282(19) . ? C41 H41 0.9300 . ? C42 H42 0.9300 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Nd1 O6 82.9(3) . . ? O4 Nd1 O8 81.9(3) . 4_565 ? O6 Nd1 O8 84.0(3) . 4_565 ? O4 Nd1 O16 148.9(3) . . ? O6 Nd1 O16 122.1(3) . . ? O8 Nd1 O16 82.9(3) 4_565 . ? O4 Nd1 O10 75.1(3) . . ? O6 Nd1 O10 82.3(3) . . ? O8 Nd1 O10 154.4(3) 4_565 . ? O16 Nd1 O10 122.7(4) . . ? O4 Nd1 O11 125.1(3) . . ? O6 Nd1 O11 88.2(3) . . ? O8 Nd1 O11 150.8(3) 4_565 . ? O16 Nd1 O11 77.6(4) . . ? O10 Nd1 O11 49.9(4) . . ? O4 Nd1 O17 149.5(3) . . ? O6 Nd1 O17 70.7(3) . . ? O8 Nd1 O17 80.5(3) 4_565 . ? O16 Nd1 O17 51.6(4) . . ? O10 Nd1 O17 114.6(3) . . ? O11 Nd1 O17 70.3(4) . . ? O4 Nd1 O13 88.8(3) . . ? O6 Nd1 O13 151.8(3) . . ? O8 Nd1 O13 121.5(3) 4_565 . ? O16 Nd1 O13 76.5(3) . . ? O10 Nd1 O13 69.6(3) . . ? O11 Nd1 O13 74.7(3) . . ? O17 Nd1 O13 121.7(3) . . ? O4 Nd1 O14 78.6(2) . . ? O6 Nd1 O14 151.6(3) . . ? O8 Nd1 O14 72.3(2) 4_565 . ? O16 Nd1 O14 71.1(3) . . ? O10 Nd1 O14 113.0(3) . . ? O11 Nd1 O14 120.1(3) . . ? O17 Nd1 O14 118.8(3) . . ? O13 Nd1 O14 49.3(3) . . ? C13 N1 C14 122.1(11) . . ? C13 N1 H1 118.9 . . ? C14 N1 H1 118.9 . . ? C25 N2 C26 125.9(12) . . ? C25 N2 H2 117.1 . . ? C26 N2 H2 117.1 . . ? C37 N3 C38 123.8(10) . . ? C37 N3 H3 118.1 . . ? C38 N3 H3 118.1 . . ? O12 N4 O10 117.0(18) . . ? O12 N4 O11 122.6(17) . . ? O10 N4 O11 120.3(15) . . ? O15 N5 O14 123.6(10) . . ? O15 N5 O13 120.6(11) . . ? O14 N5 O13 115.8(9) . . ? O17 N6 O18 121.5(16) . . ? O17 N6 O16 119.4(12) . . ? O18 N6 O16 118.8(16) . . ? C7 O1 C4 116.7(7) . . ? C19 O2 C5 119.3(9) . . ? C31 O3 C6 118.3(8) . . ? C13 O4 Nd1 159.7(8) . . ? C15 O5 C18 108(2) . . ? C25 O6 Nd1 156.7(9) . . ? C27 O7 C30 104.5(18) . . ? C37 O8 Nd1 166.2(7) . 4_566 ? C39 O9 C42 106.2(13) . . ? N4 O10 Nd1 95.0(10) . . ? N4 O11 Nd1 94.7(10) . . ? N5 O13 Nd1 97.5(7) . . ? N5 O14 Nd1 97.4(6) . . ? N6 O16 Nd1 94.9(8) . . ? N6 O17 Nd1 94.1(8) . . ? C43 O19 C43 180(4) 3_765 . ? C43 O19 H19 64.8 3_765 . ? C43 O19 H19 115.2 . . ? C5 C1 C4 107.3(8) . . ? C5 C1 C2 112.7(9) . . ? C4 C1 C2 111.9(9) . . ? C5 C1 C6 108.5(9) . . ? C4 C1 C6 108.1(8) . . ? C2 C1 C6 108.2(8) . . ? C1 C2 C3 115.9(10) . . ? C1 C2 H2A 108.3 . . ? C3 C2 H2A 108.3 . . ? C1 C2 H2B 108.3 . . ? C3 C2 H2B 108.3 . . ? H2A C2 H2B 107.4 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? O1 C4 C1 107.3(7) . . ? O1 C4 H4A 110.3 . . ? C1 C4 H4A 110.3 . . ? O1 C4 H4B 110.3 . . ? C1 C4 H4B 110.3 . . ? H4A C4 H4B 108.5 . . ? O2 C5 C1 107.2(9) . . ? O2 C5 H5A 110.3 . . ? C1 C5 H5A 110.3 . . ? O2 C5 H5B 110.3 . . ? C1 C5 H5B 110.3 . . ? H5A C5 H5B 108.5 . . ? O3 C6 C1 108.4(8) . . ? O3 C6 H6A 110.0 . . ? C1 C6 H6A 110.0 . . ? O3 C6 H6B 110.0 . . ? C1 C6 H6B 110.0 . . ? H6A C6 H6B 108.4 . . ? O1 C7 C8 123.5(9) . . ? O1 C7 C12 117.2(8) . . ? C8 C7 C12 119.3(9) . . ? C9 C8 C7 119.4(10) . . ? C9 C8 H8 120.3 . . ? C7 C8 H8 120.3 . . ? C10 C9 C8 121.2(10) . . ? C10 C9 H9 119.4 . . ? C8 C9 H9 119.4 . . ? C9 C10 C11 120.1(10) . . ? C9 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? C10 C11 C12 121.8(10) . . ? C10 C11 H11 119.1 . . ? C12 C11 H11 119.1 . . ? C11 C12 C7 118.2(9) . . ? C11 C12 C13 117.3(9) . . ? C7 C12 C13 124.5(9) . . ? O4 C13 N1 123.4(10) . . ? O4 C13 C12 119.7(10) . . ? N1 C13 C12 116.7(9) . . ? C15 C14 N1 117.1(13) . . ? C15 C14 H14A 108.0 . . ? N1 C14 H14A 108.0 . . ? C15 C14 H14B 108.0 . . ? N1 C14 H14B 108.0 . . ? H14A C14 H14B 107.3 . . ? C16 C15 O5 108.8(19) . . ? C16 C15 C14 137(3) . . ? O5 C15 C14 114(2) . . ? C15 C16 C17 106(2) . . ? C15 C16 H16 127.2 . . ? C17 C16 H16 127.2 . . ? C18 C17 C16 108(2) . . ? C18 C17 H17 125.8 . . ? C16 C17 H17 125.8 . . ? C17 C18 O5 108(2) . . ? C17 C18 H18 125.9 . . ? O5 C18 H18 125.9 . . ? O2 C19 C20 122.1(11) . . ? O2 C19 C24 119.4(11) . . ? C20 C19 C24 118.5(12) . . ? C19 C20 C21 122.0(12) . . ? C19 C20 H20 119.0 . . ? C21 C20 H20 119.0 . . ? C22 C21 C20 118.2(14) . . ? C22 C21 H21 120.9 . . ? C20 C21 H21 120.9 . . ? C21 C22 C23 119.3(14) . . ? C21 C22 H22 120.3 . . ? C23 C22 H22 120.3 . . ? C24 C23 C22 123.7(14) . . ? C24 C23 H23 118.1 . . ? C22 C23 H23 118.1 . . ? C23 C24 C19 118.0(13) . . ? C23 C24 C25 118.3(12) . 2_655 ? C19 C24 C25 123.4(11) . 2_655 ? O6 C25 N2 113.7(13) . . ? O6 C25 C24 123.2(11) . 2_645 ? N2 C25 C24 123.0(12) . 2_645 ? C27 C26 N2 118.3(15) . . ? C27 C26 H26A 107.7 . . ? N2 C26 H26A 107.7 . . ? C27 C26 H26B 107.7 . . ? N2 C26 H26B 107.7 . . ? H26A C26 H26B 107.1 . . ? C28 C27 O7 108.8(17) . . ? C28 C27 C26 133(2) . . ? O7 C27 C26 117(2) . . ? C29 C28 C27 109(2) . . ? C29 C28 H28 125.7 . . ? C27 C28 H28 125.7 . . ? C28 C29 C30 106(2) . . ? C28 C29 H29 126.8 . . ? C30 C29 H29 126.8 . . ? C29 C30 O7 110(2) . . ? C29 C30 H30 124.9 . . ? O7 C30 H30 124.9 . . ? C36 C31 O3 117.5(9) . . ? C36 C31 C32 120.3(10) . . ? O3 C31 C32 122.2(10) . . ? C33 C32 C31 118.8(12) . . ? C33 C32 H32 120.6 . . ? C31 C32 H32 120.6 . . ? C34 C33 C32 121.2(11) . . ? C34 C33 H33 119.4 . . ? C32 C33 H33 119.4 . . ? C33 C34 C35 117.9(12) . . ? C33 C34 H34 121.1 . . ? C35 C34 H34 121.1 . . ? C36 C35 C34 122.7(13) . . ? C36 C35 H35 118.7 . . ? C34 C35 H35 118.7 . . ? C35 C36 C31 118.9(10) . . ? C35 C36 C37 116.4(11) . . ? C31 C36 C37 124.6(9) . . ? O8 C37 N3 122.5(10) . . ? O8 C37 C36 119.8(10) . . ? N3 C37 C36 117.7(11) . . ? C39 C38 N3 112.0(10) . . ? C39 C38 H38A 109.2 . . ? N3 C38 H38A 109.2 . . ? C39 C38 H38B 109.2 . . ? N3 C38 H38B 109.2 . . ? H38A C38 H38B 107.9 . . ? C40 C39 O9 109.0(15) . . ? C40 C39 C38 132.9(16) . . ? O9 C39 C38 118.0(13) . . ? C39 C40 C41 107.0(16) . . ? C39 C40 H40 126.5 . . ? C41 C40 H40 126.5 . . ? C42 C41 C40 106.0(16) . . ? C42 C41 H41 127.0 . . ? C40 C41 H41 127.0 . . ? C41 C42 O9 111.7(16) . . ? C41 C42 H42 124.2 . . ? O9 C42 H42 124.2 . . ? O19 C43 H43A 109.5 . . ? O19 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? O19 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.678 _refine_diff_density_min -0.730 _refine_diff_density_rms 0.146 # Attachment '3.cif' data_p21c _database_code_depnum_ccdc_archive 'CCDC 672452' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety C42H41N3O9,N3O9,Sm _chemical_formula_sum 'C42 H41 N6 O18 Sm' _chemical_formula_weight 1068.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.6382(6) _cell_length_b 16.2654(5) _cell_length_c 18.6824(6) _cell_angle_alpha 90.00 _cell_angle_beta 98.911(2) _cell_angle_gamma 90.00 _cell_volume 4994.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 2517 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 17.62 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.420 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2164 _exptl_absorpt_coefficient_mu 1.250 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8346 _exptl_absorpt_correction_T_max 0.8852 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22725 _diffrn_reflns_av_R_equivalents 0.1010 _diffrn_reflns_av_sigmaI/netI 0.1831 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 25.05 _reflns_number_total 8209 _reflns_number_gt 2966 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0200P)^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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8209 _refine_ls_number_parameters 578 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1788 _refine_ls_R_factor_gt 0.0666 _refine_ls_wR_factor_ref 0.1413 _refine_ls_wR_factor_gt 0.1198 _refine_ls_goodness_of_fit_ref 0.964 _refine_ls_restrained_S_all 0.964 _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 C46 C 0.8830(7) 0.7164(9) 0.1007(11) 0.157(9) Uani 1 1 d G . . C50 C 0.9265(11) 0.6571(10) 0.0661(7) 0.226(13) Uani 1 1 d G . . H50 H 0.9111 0.6360 0.0197 0.271 Uiso 1 1 calc R . . C49 C 0.9976(9) 0.6355(7) 0.1148(11) 0.205(12) Uani 1 1 d G . . H49 H 1.0369 0.5979 0.1059 0.246 Uiso 1 1 calc R . . C48 C 0.9980(9) 0.6815(10) 0.1795(9) 0.213(13) Uani 1 1 d G . . H48 H 1.0377 0.6792 0.2204 0.255 Uiso 1 1 calc R . . O26 O 0.9272(12) 0.7314(7) 0.1707(10) 0.227(9) Uani 1 1 d G . . C39 C 0.9763(11) 0.3984(9) 0.0838(10) 0.233(14) Uani 1 1 d G . . H39 H 1.0029 0.4363 0.0585 0.279 Uiso 1 1 calc R . . C40 C 0.9099(10) 0.3478(12) 0.0540(7) 0.272(18) Uani 1 1 d G . . H40 H 0.8854 0.3468 0.0057 0.326 Uiso 1 1 calc R . . C41 C 0.8875(9) 0.2991(8) 0.1108(12) 0.238(15) Uani 1 1 d G . . H41 H 0.8457 0.2605 0.1063 0.285 Uiso 1 1 calc R . . O27 O 0.9400(11) 0.3195(10) 0.1757(8) 0.230(8) Uani 1 1 d G . . C38 C 0.9949(7) 0.3809(11) 0.1590(9) 0.141(7) Uani 1 1 d G . . C42 C 0.6153(7) 0.6476(5) 0.4261(5) 0.090(4) Uani 1 1 d G . . O25 O 0.6955(5) 0.6786(5) 0.4292(5) 0.125(4) Uani 1 1 d G . . C37 C 0.6930(7) 0.7445(5) 0.3791(6) 0.142(7) Uani 1 1 d G . . H37 H 0.7371 0.7758 0.3702 0.170 Uiso 1 1 calc R . . C36 C 0.6111(9) 0.7544(6) 0.3451(5) 0.173(9) Uani 1 1 d G . . H36 H 0.5922 0.7932 0.3100 0.207 Uiso 1 1 calc R . . C43 C 0.5631(5) 0.6945(7) 0.3741(6) 0.120(6) Uani 1 1 d G . . H43 H 0.5073 0.6872 0.3614 0.144 Uiso 1 1 calc R . . C1 C 0.6138(5) 0.6661(5) 0.1810(5) 0.046(3) Uani 1 1 d . . . C2 C 0.5391(7) 0.6338(6) 0.1923(6) 0.073(3) Uani 1 1 d . . . H2 H 0.5362 0.5811 0.2109 0.088 Uiso 1 1 calc R . . C3 C 0.4695(6) 0.6808(7) 0.1757(6) 0.085(4) Uani 1 1 d . . . H3 H 0.4198 0.6578 0.1818 0.102 Uiso 1 1 calc R . . C4 C 0.4708(6) 0.7603(7) 0.1506(6) 0.073(4) Uani 1 1 d . . . H4 H 0.4239 0.7921 0.1422 0.087 Uiso 1 1 calc R . . C5 C 0.5467(6) 0.7912(6) 0.1382(6) 0.070(4) Uani 1 1 d . . . H5 H 0.5491 0.8438 0.1191 0.083 Uiso 1 1 calc R . . C6 C 0.6184(6) 0.7455(6) 0.1537(5) 0.054(3) Uani 1 1 d . . . C7 C 0.6934(6) 0.7836(7) 0.1365(6) 0.063(3) Uani 1 1 d . . . C8 C 0.8229(8) 0.7706(9) 0.0942(12) 0.160(8) Uani 1 1 d . . . H8A H 0.8081 0.7853 0.0435 0.192 Uiso 1 1 calc R . . H8B H 0.8415 0.8200 0.1207 0.192 Uiso 1 1 calc R . . C11 C 0.6807(6) 0.5479(6) 0.2388(6) 0.064(3) Uani 1 1 d . . . H11A H 0.6453 0.5091 0.2096 0.076 Uiso 1 1 calc R . . H11B H 0.6595 0.5573 0.2837 0.076 Uiso 1 1 calc R . . C12 C 0.7684(6) 0.5136(6) 0.2549(5) 0.053(3) Uani 1 1 d . . . C13 C 0.8026(6) 0.5060(7) 0.1850(6) 0.079(3) Uani 1 1 d . . . H13A H 0.8523 0.4741 0.1949 0.095 Uiso 1 1 calc R . . H13B H 0.8176 0.5606 0.1711 0.095 Uiso 1 1 calc R . . C14 C 0.7459(8) 0.4646(8) 0.1148(7) 0.122(6) Uani 1 1 d . . . H14A H 0.7410 0.4066 0.1227 0.183 Uiso 1 1 calc R . . H14B H 0.7706 0.4734 0.0723 0.183 Uiso 1 1 calc R . . H14C H 0.6929 0.4894 0.1082 0.183 Uiso 1 1 calc R . . C15 C 0.8201(6) 0.5702(6) 0.3104(6) 0.065(3) Uani 1 1 d . . . H15A H 0.8190 0.6263 0.2925 0.078 Uiso 1 1 calc R . . H15B H 0.7996 0.5697 0.3562 0.078 Uiso 1 1 calc R . . C16 C 0.9558(7) 0.5661(6) 0.3751(6) 0.065(3) Uani 1 1 d . . . C17 C 0.9332(9) 0.6212(8) 0.4267(7) 0.105(5) Uani 1 1 d . . . H17 H 0.8800 0.6403 0.4219 0.126 Uiso 1 1 calc R . . C18 C 0.9904(9) 0.6473(9) 0.4846(7) 0.119(6) Uani 1 1 d . . . H18 H 0.9758 0.6844 0.5182 0.143 Uiso 1 1 calc R . . C19 C 1.0680(8) 0.6177(10) 0.4917(8) 0.109(5) Uani 1 1 d . . . H19 H 1.1063 0.6330 0.5310 0.131 Uiso 1 1 calc R . . C20 C 1.0885(8) 0.5661(7) 0.4412(7) 0.091(4) Uani 1 1 d . . . H20 H 1.1415 0.5462 0.4474 0.109 Uiso 1 1 calc R . . C21 C 1.0375(7) 0.5416(7) 0.3826(7) 0.072(3) Uani 1 1 d . . . C22 C 1.0692(7) 0.4904(7) 0.3263(7) 0.073(3) Uani 1 1 d . . . C23 C 1.0508(12) 0.4065(14) 0.2181(12) 0.279(17) Uani 1 1 d . . . H23A H 1.0932 0.4367 0.1993 0.334 Uiso 1 1 calc R . . H23B H 1.0759 0.3575 0.2413 0.334 Uiso 1 1 calc R . . C24 C 0.7655(6) 0.4296(6) 0.2866(6) 0.056(3) Uani 1 1 d . . . H24A H 0.7312 0.3940 0.2532 0.067 Uiso 1 1 calc R . . H24B H 0.8198 0.4061 0.2955 0.067 Uiso 1 1 calc R . . C25 C 0.7271(6) 0.3660(5) 0.3962(6) 0.055(3) Uani 1 1 d . . . C26 C 0.7502(6) 0.2878(5) 0.3708(6) 0.064(3) Uani 1 1 d . . . H26 H 0.7686 0.2812 0.3267 0.077 Uiso 1 1 calc R . . C27 C 0.7429(7) 0.2229(6) 0.4172(7) 0.075(4) Uani 1 1 d . . . H27 H 0.7541 0.1704 0.4018 0.090 Uiso 1 1 calc R . . C29 C 0.7207(8) 0.2309(7) 0.4835(7) 0.092(5) Uani 1 1 d . . . H29 H 0.7201 0.1855 0.5136 0.110 Uiso 1 1 calc R . . C31 C 0.6987(7) 0.3081(6) 0.5058(6) 0.073(4) Uani 1 1 d . . . H31 H 0.6809 0.3138 0.5503 0.088 Uiso 1 1 calc R . . C32 C 0.7026(6) 0.3758(6) 0.4633(6) 0.054(3) Uani 1 1 d . . . C33 C 0.6812(7) 0.4561(6) 0.4911(7) 0.060(3) Uani 1 1 d . . . C34 C 0.6002(7) 0.5838(5) 0.4720(6) 0.069(3) Uani 1 1 d . . . H34A H 0.5421 0.5790 0.4723 0.083 Uiso 1 1 calc R . . H34B H 0.6263 0.5956 0.5211 0.083 Uiso 1 1 calc R . . N1 N 0.5452(6) 0.9805(5) 0.1884(7) 0.072(3) Uani 1 1 d . . . N3 N 0.7280(13) 1.1765(8) 0.1908(7) 0.115(5) Uani 1 1 d . . . N4 N 0.7707(10) 0.9556(9) 0.3342(10) 0.131(7) Uani 1 1 d . . . N5 N 1.0240(7) 0.4570(7) 0.2744(7) 0.133(5) Uani 1 1 d . . . H5A H 0.9725 0.4646 0.2719 0.159 Uiso 1 1 calc R . . N6 N 0.7500(6) 0.7380(6) 0.1219(7) 0.106(4) Uani 1 1 d . . . H6 H 0.7463 0.6859 0.1283 0.127 Uiso 1 1 calc R . . N7 N 0.6315(5) 0.5066(4) 0.4476(4) 0.064(2) Uani 1 1 d . . . H7 H 0.6174 0.4927 0.4030 0.077 Uiso 1 1 calc R . . O1 O 0.5951(5) 0.9747(4) 0.2462(4) 0.079(2) Uani 1 1 d . . . O2 O 0.5660(4) 0.9951(5) 0.1282(4) 0.0665(18) Uani 1 1 d . . . O3 O 0.4708(4) 0.9719(4) 0.1941(4) 0.077(2) Uani 1 1 d . . . O4 O 1.1449(5) 0.4733(4) 0.3328(4) 0.087(3) Uani 1 1 d . . . O6 O 0.7645(6) 1.0318(7) 0.3126(5) 0.117(3) Uani 1 1 d . . . O10 O 0.7525(7) 0.9052(7) 0.2879(6) 0.111(4) Uani 1 1 d . . . O11 O 0.6600(7) 1.1392(6) 0.1875(5) 0.110(4) Uani 1 1 d . . . O12 O 0.7882(7) 1.1344(6) 0.1849(6) 0.108(4) Uani 1 1 d . . . O13 O 0.7005(4) 0.8606(4) 0.1401(4) 0.067(2) Uani 1 1 d . . . O14 O 0.7294(9) 1.2508(6) 0.1933(5) 0.180(6) Uani 1 1 d . . . O15 O 0.7039(4) 0.4733(4) 0.5565(4) 0.0621(19) Uani 1 1 d . . . O16 O 0.7942(9) 0.9506(8) 0.3996(6) 0.178(6) Uani 1 1 d . . . O17 O 0.9013(5) 0.5376(4) 0.3190(4) 0.079(2) Uani 1 1 d . . . O18 O 0.7335(4) 0.4359(4) 0.3530(4) 0.0638(19) Uani 1 1 d . . . O19 O 0.6848(4) 0.6256(3) 0.1994(4) 0.0567(18) Uani 1 1 d . . . Sm1 Sm 0.71784(3) 0.99703(3) 0.18085(3) 0.05952(19) 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 C46 0.15(2) 0.145(19) 0.20(2) 0.043(16) 0.105(17) -0.031(17) C50 0.14(2) 0.167(19) 0.40(4) 0.14(2) 0.14(2) 0.091(15) C49 0.12(2) 0.129(16) 0.40(4) 0.08(2) 0.14(2) 0.040(14) C48 0.16(3) 0.19(3) 0.29(3) 0.01(2) 0.00(2) -0.04(2) O26 0.144(14) 0.153(12) 0.38(3) 0.046(14) 0.042(16) 0.048(11) C39 0.33(4) 0.23(2) 0.14(2) -0.109(17) 0.03(2) -0.09(2) C40 0.14(2) 0.52(5) 0.17(2) -0.19(3) 0.063(17) -0.02(2) C41 0.26(3) 0.25(3) 0.19(2) -0.15(2) 0.01(3) -0.02(2) O27 0.146(14) 0.209(15) 0.33(3) -0.068(15) 0.024(15) 0.012(12) C38 0.054(10) 0.199(18) 0.172(19) -0.113(15) 0.025(11) 0.009(11) C42 0.083(11) 0.081(9) 0.105(12) -0.033(8) 0.013(9) 0.029(8) O25 0.156(10) 0.073(6) 0.151(10) 0.018(6) 0.041(8) -0.005(6) C37 0.21(2) 0.060(9) 0.190(19) -0.041(10) 0.130(15) -0.047(11) C36 0.22(2) 0.141(16) 0.159(18) -0.066(14) 0.03(2) 0.037(18) C43 0.186(17) 0.068(9) 0.114(12) 0.016(8) 0.044(12) -0.010(10) C1 0.031(6) 0.046(5) 0.058(7) 0.004(5) -0.001(5) 0.009(5) C2 0.050(8) 0.061(7) 0.107(10) 0.015(6) 0.007(7) 0.000(6) C3 0.030(7) 0.091(9) 0.130(11) 0.038(8) 0.002(6) -0.004(6) C4 0.036(7) 0.066(7) 0.114(10) 0.032(7) 0.005(6) 0.007(5) C5 0.058(8) 0.046(6) 0.099(9) 0.011(6) -0.006(7) 0.003(6) C6 0.034(6) 0.047(6) 0.080(8) 0.000(5) 0.003(5) -0.002(5) C7 0.041(7) 0.060(7) 0.084(9) 0.020(6) 0.000(6) 0.002(6) C8 0.090(12) 0.113(12) 0.30(2) 0.094(14) 0.103(13) 0.064(10) C11 0.037(7) 0.073(7) 0.083(8) 0.001(6) 0.017(6) -0.013(5) C12 0.048(6) 0.050(7) 0.061(6) -0.003(5) 0.014(5) 0.007(5) C13 0.051(6) 0.065(6) 0.124(10) 0.002(8) 0.018(6) -0.002(7) C14 0.101(12) 0.170(13) 0.084(10) -0.036(9) -0.019(9) 0.008(10) C15 0.034(7) 0.075(7) 0.083(8) 0.015(6) 0.000(6) 0.009(6) C16 0.068(8) 0.062(7) 0.066(8) -0.015(6) 0.008(6) 0.006(6) C17 0.096(11) 0.125(11) 0.096(11) -0.051(9) 0.024(9) 0.005(9) C18 0.091(13) 0.145(12) 0.110(14) -0.071(10) -0.019(10) 0.027(9) C19 0.040(8) 0.194(15) 0.088(11) -0.041(10) -0.008(7) 0.012(9) C20 0.065(9) 0.117(10) 0.083(10) -0.027(8) -0.012(8) 0.008(8) C21 0.040(7) 0.069(7) 0.104(10) -0.011(7) 0.006(7) 0.002(6) C22 0.050(7) 0.071(7) 0.093(9) -0.001(7) -0.005(6) -0.003(7) C23 0.117(16) 0.43(4) 0.26(3) -0.26(3) -0.072(17) 0.07(2) C24 0.039(6) 0.059(6) 0.071(8) 0.006(6) 0.013(5) 0.015(5) C25 0.036(6) 0.045(6) 0.075(8) 0.002(6) -0.017(6) -0.005(5) C26 0.047(7) 0.045(6) 0.095(9) 0.003(6) -0.006(6) 0.003(5) C27 0.084(9) 0.046(6) 0.085(10) 0.007(7) -0.017(8) 0.004(6) C29 0.130(12) 0.069(8) 0.070(10) 0.018(7) -0.004(9) -0.010(8) C31 0.106(10) 0.052(6) 0.057(7) 0.007(6) -0.004(7) -0.003(7) C32 0.061(7) 0.047(6) 0.052(7) -0.004(6) 0.002(6) 0.004(5) C33 0.054(7) 0.061(7) 0.068(8) -0.007(6) 0.013(6) -0.007(6) C34 0.089(9) 0.040(6) 0.079(9) 0.017(6) 0.015(7) 0.022(6) N1 0.049(7) 0.070(7) 0.092(9) -0.012(6) -0.003(6) 0.004(5) N3 0.21(2) 0.068(9) 0.068(8) -0.011(8) 0.038(11) -0.025(11) N4 0.120(13) 0.112(11) 0.151(18) 0.070(11) -0.013(12) 0.002(11) N5 0.061(8) 0.180(11) 0.149(11) -0.096(9) -0.011(8) 0.032(7) N6 0.095(9) 0.058(6) 0.182(12) 0.028(7) 0.078(8) 0.008(6) N7 0.082(6) 0.046(4) 0.062(5) 0.002(5) 0.001(4) 0.018(5) O1 0.060(5) 0.111(6) 0.065(5) 0.016(4) 0.005(4) -0.020(4) O2 0.063(5) 0.076(5) 0.062(5) -0.002(5) 0.012(4) 0.007(4) O3 0.046(5) 0.088(6) 0.097(6) -0.004(4) 0.011(4) 0.006(4) O4 0.055(5) 0.096(6) 0.108(7) -0.010(4) 0.000(4) 0.021(4) O6 0.102(8) 0.169(9) 0.074(6) -0.054(6) -0.001(6) -0.026(7) O10 0.093(8) 0.114(8) 0.118(10) 0.038(6) -0.010(7) -0.021(6) O11 0.155(10) 0.069(6) 0.111(8) -0.004(5) 0.036(7) 0.018(6) O12 0.117(9) 0.083(7) 0.119(9) 0.000(6) 0.007(7) -0.039(6) O13 0.041(4) 0.053(4) 0.104(6) 0.007(4) 0.001(4) -0.009(3) O14 0.375(19) 0.060(5) 0.112(8) -0.007(6) 0.057(10) -0.042(10) O15 0.049(4) 0.058(4) 0.078(5) 0.000(4) 0.005(4) 0.006(3) O16 0.195(14) 0.241(13) 0.082(8) 0.049(8) -0.031(9) -0.007(11) O17 0.061(5) 0.084(5) 0.090(6) -0.026(4) 0.001(4) 0.017(4) O18 0.053(5) 0.056(4) 0.083(6) 0.011(4) 0.012(4) 0.017(3) O19 0.037(4) 0.050(4) 0.084(5) 0.006(4) 0.015(3) 0.006(3) Sm1 0.0509(3) 0.0558(3) 0.0704(3) 0.0025(4) 0.0049(2) -0.0075(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 C46 C8 1.324(15) . ? C46 C50 1.4200 . ? C46 O26 1.4200 . ? C50 C49 1.4200 . ? C50 H50 0.9300 . ? C49 C48 1.4200 . ? C49 H49 0.9300 . ? C48 O26 1.4200 . ? C48 H48 0.9300 . ? C39 C40 1.4200 . ? C39 C38 1.4200 . ? C39 H39 0.9300 . ? C40 C41 1.4200 . ? C40 H40 0.9300 . ? C41 O27 1.4200 . ? C41 H41 0.9300 . ? O27 C38 1.4200 . ? C38 C23 1.392(16) . ? C42 C34 1.394(11) . ? C42 C43 1.4200 . ? C42 O25 1.4200 . ? O25 C37 1.4200 . ? C37 C36 1.4200 . ? C37 H37 0.9300 . ? C36 C43 1.4200 . ? C36 H36 0.9300 . ? C43 H43 0.9300 . ? C1 O19 1.349(9) . ? C1 C2 1.395(14) . ? C1 C6 1.396(12) . ? C2 C3 1.383(12) . ? C2 H2 0.9300 . ? C3 C4 1.377(13) . ? C3 H3 0.9300 . ? C4 C5 1.411(14) . ? C4 H4 0.9300 . ? C5 C6 1.396(12) . ? C5 H5 0.9300 . ? C6 C7 1.473(14) . ? C7 O13 1.259(11) . ? C7 N6 1.260(13) . ? C8 N6 1.490(16) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C11 O19 1.471(10) . ? C11 C12 1.547(12) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C24 1.494(12) . ? C12 C13 1.510(14) . ? C12 C15 1.544(12) . ? C13 C14 1.636(13) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 O17 1.437(11) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 O17 1.358(11) . ? C16 C21 1.403(14) . ? C16 C17 1.408(15) . ? C17 C18 1.392(13) . ? C17 H17 0.9300 . ? C18 C19 1.365(16) . ? C18 H18 0.9300 . ? C19 C20 1.346(16) . ? C19 H19 0.9300 . ? C20 C21 1.337(13) . ? C20 H20 0.9300 . ? C21 C22 1.501(17) . ? C22 N5 1.255(12) . ? C22 O4 1.277(12) . ? C23 N5 1.46(2) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 O18 1.428(11) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C32 1.386(14) . ? C25 O18 1.407(11) . ? C25 C26 1.431(12) . ? C26 C27 1.383(13) . ? C26 H26 0.9300 . ? C27 C29 1.352(16) . ? C27 H27 0.9300 . ? C29 C31 1.391(14) . ? C29 H29 0.9300 . ? C31 C32 1.363(13) . ? C31 H31 0.9300 . ? C32 C33 1.470(13) . ? C33 O15 1.253(11) . ? C33 N7 1.347(11) . ? C34 N7 1.458(11) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? N1 O2 1.250(12) . ? N1 O1 1.260(9) . ? N1 O3 1.266(11) . ? N3 O14 1.209(14) . ? N3 O12 1.233(16) . ? N3 O11 1.278(16) . ? N4 O10 1.196(16) . ? N4 O16 1.227(16) . ? N4 O6 1.303(14) . ? N5 H5A 0.8600 . ? N6 H6 0.8600 . ? N7 H7 0.8600 . ? O1 Sm1 2.562(8) . ? O2 Sm1 2.565(6) . ? O4 Sm1 2.369(9) 2_745 ? O6 Sm1 2.527(8) . ? O10 Sm1 2.491(10) . ? O11 Sm1 2.516(8) . ? O12 Sm1 2.519(9) . ? O13 Sm1 2.349(6) . ? O15 Sm1 2.348(8) 4_576 ? Sm1 O15 2.348(8) 4_575 ? Sm1 O4 2.369(9) 2_755 ? 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 C8 C46 C50 147(2) . . ? C8 C46 O26 104(2) . . ? C50 C46 O26 108.0 . . ? C46 C50 C49 108.0 . . ? C46 C50 H50 126.0 . . ? C49 C50 H50 126.0 . . ? C48 C49 C50 108.0 . . ? C48 C49 H49 126.0 . . ? C50 C49 H49 126.0 . . ? O26 C48 C49 108.0 . . ? O26 C48 H48 126.0 . . ? C49 C48 H48 126.0 . . ? C48 O26 C46 108.0 . . ? C40 C39 C38 108.0 . . ? C40 C39 H39 126.0 . . ? C38 C39 H39 126.0 . . ? C39 C40 C41 108.0 . . ? C39 C40 H40 126.0 . . ? C41 C40 H40 126.0 . . ? O27 C41 C40 108.0 . . ? O27 C41 H41 126.0 . . ? C40 C41 H41 126.0 . . ? C38 O27 C41 108.0 . . ? C23 C38 O27 114(2) . . ? C23 C38 C39 138(2) . . ? O27 C38 C39 108.0 . . ? C34 C42 C43 132.2(10) . . ? C34 C42 O25 119.8(10) . . ? C43 C42 O25 108.0 . . ? C37 O25 C42 108.0 . . ? O25 C37 C36 108.0 . . ? O25 C37 H37 126.0 . . ? C36 C37 H37 126.0 . . ? C37 C36 C43 108.0 . . ? C37 C36 H36 126.0 . . ? C43 C36 H36 126.0 . . ? C42 C43 C36 108.0 . . ? C42 C43 H43 126.0 . . ? C36 C43 H43 126.0 . . ? O19 C1 C2 122.9(8) . . ? O19 C1 C6 116.8(8) . . ? C2 C1 C6 120.2(9) . . ? C3 C2 C1 119.6(9) . . ? C3 C2 H2 120.2 . . ? C1 C2 H2 120.2 . . ? C4 C3 C2 122.5(10) . . ? C4 C3 H3 118.7 . . ? C2 C3 H3 118.7 . . ? C3 C4 C5 116.9(9) . . ? C3 C4 H4 121.6 . . ? C5 C4 H4 121.6 . . ? C6 C5 C4 122.3(9) . . ? C6 C5 H5 118.9 . . ? C4 C5 H5 118.9 . . ? C5 C6 C1 118.4(9) . . ? C5 C6 C7 117.2(9) . . ? C1 C6 C7 124.3(9) . . ? O13 C7 N6 122.0(11) . . ? O13 C7 C6 118.8(10) . . ? N6 C7 C6 119.1(10) . . ? C46 C8 N6 112.0(11) . . ? C46 C8 H8A 109.2 . . ? N6 C8 H8A 109.2 . . ? C46 C8 H8B 109.2 . . ? N6 C8 H8B 109.2 . . ? H8A C8 H8B 107.9 . . ? O19 C11 C12 106.9(7) . . ? O19 C11 H11A 110.3 . . ? C12 C11 H11A 110.3 . . ? O19 C11 H11B 110.3 . . ? C12 C11 H11B 110.3 . . ? H11A C11 H11B 108.6 . . ? C24 C12 C13 107.8(8) . . ? C24 C12 C15 109.2(8) . . ? C13 C12 C15 112.6(9) . . ? C24 C12 C11 108.7(8) . . ? C13 C12 C11 109.4(8) . . ? C15 C12 C11 109.1(8) . . ? C12 C13 C14 118.7(9) . . ? C12 C13 H13A 107.6 . . ? C14 C13 H13A 107.6 . . ? C12 C13 H13B 107.6 . . ? C14 C13 H13B 107.6 . . ? H13A C13 H13B 107.1 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O17 C15 C12 105.8(8) . . ? O17 C15 H15A 110.6 . . ? C12 C15 H15A 110.6 . . ? O17 C15 H15B 110.6 . . ? C12 C15 H15B 110.6 . . ? H15A C15 H15B 108.7 . . ? O17 C16 C21 120.1(11) . . ? O17 C16 C17 121.9(11) . . ? C21 C16 C17 118.0(11) . . ? C18 C17 C16 120.2(13) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C19 C18 C17 119.3(14) . . ? C19 C18 H18 120.4 . . ? C17 C18 H18 120.4 . . ? C20 C19 C18 119.4(12) . . ? C20 C19 H19 120.3 . . ? C18 C19 H19 120.3 . . ? C21 C20 C19 124.2(13) . . ? C21 C20 H20 117.9 . . ? C19 C20 H20 117.9 . . ? C20 C21 C16 118.6(13) . . ? C20 C21 C22 119.5(11) . . ? C16 C21 C22 121.9(10) . . ? N5 C22 O4 116.4(13) . . ? N5 C22 C21 123.2(12) . . ? O4 C22 C21 120.2(10) . . ? C38 C23 N5 120.0(16) . . ? C38 C23 H23A 107.3 . . ? N5 C23 H23A 107.3 . . ? C38 C23 H23B 107.3 . . ? N5 C23 H23B 107.3 . . ? H23A C23 H23B 106.9 . . ? O18 C24 C12 108.5(8) . . ? O18 C24 H24A 110.0 . . ? C12 C24 H24A 110.0 . . ? O18 C24 H24B 110.0 . . ? C12 C24 H24B 110.0 . . ? H24A C24 H24B 108.4 . . ? C32 C25 O18 119.0(9) . . ? C32 C25 C26 122.2(10) . . ? O18 C25 C26 118.7(11) . . ? C27 C26 C25 114.6(11) . . ? C27 C26 H26 122.7 . . ? C25 C26 H26 122.7 . . ? C29 C27 C26 124.3(11) . . ? C29 C27 H27 117.8 . . ? C26 C27 H27 117.8 . . ? C27 C29 C31 118.9(11) . . ? C27 C29 H29 120.6 . . ? C31 C29 H29 120.6 . . ? C32 C31 C29 121.1(12) . . ? C32 C31 H31 119.5 . . ? C29 C31 H31 119.5 . . ? C31 C32 C25 118.8(10) . . ? C31 C32 C33 118.4(11) . . ? C25 C32 C33 122.8(9) . . ? O15 C33 N7 121.1(9) . . ? O15 C33 C32 119.3(9) . . ? N7 C33 C32 119.3(9) . . ? C42 C34 N7 110.0(9) . . ? C42 C34 H34A 109.7 . . ? N7 C34 H34A 109.7 . . ? C42 C34 H34B 109.7 . . ? N7 C34 H34B 109.7 . . ? H34A C34 H34B 108.2 . . ? O2 N1 O1 123.2(10) . . ? O2 N1 O3 120.5(9) . . ? O1 N1 O3 116.3(12) . . ? O14 N3 O12 123.2(19) . . ? O14 N3 O11 119.2(19) . . ? O12 N3 O11 117.2(12) . . ? O10 N4 O16 132.9(15) . . ? O10 N4 O6 115.4(15) . . ? O16 N4 O6 111.7(17) . . ? C22 N5 C23 126.0(13) . . ? C22 N5 H5A 117.0 . . ? C23 N5 H5A 117.0 . . ? C7 N6 C8 122.8(10) . . ? C7 N6 H6 118.6 . . ? C8 N6 H6 118.6 . . ? C33 N7 C34 123.5(8) . . ? C33 N7 H7 118.2 . . ? C34 N7 H7 118.2 . . ? N1 O1 Sm1 92.8(7) . . ? N1 O2 Sm1 92.9(5) . . ? C22 O4 Sm1 155.1(8) . 2_745 ? N4 O6 Sm1 94.9(10) . . ? N4 O10 Sm1 99.8(10) . . ? N3 O11 Sm1 95.5(9) . . ? N3 O12 Sm1 96.6(9) . . ? C7 O13 Sm1 164.4(8) . . ? C33 O15 Sm1 168.1(7) . 4_576 ? C16 O17 C15 117.7(9) . . ? C25 O18 C24 120.8(8) . . ? C1 O19 C11 116.1(7) . . ? O15 Sm1 O13 83.4(2) 4_575 . ? O15 Sm1 O4 82.9(3) 4_575 2_755 ? O13 Sm1 O4 83.3(2) . 2_755 ? O15 Sm1 O10 153.2(3) 4_575 . ? O13 Sm1 O10 72.3(3) . . ? O4 Sm1 O10 83.2(3) 2_755 . ? O15 Sm1 O11 83.1(3) 4_575 . ? O13 Sm1 O11 148.8(3) . . ? O4 Sm1 O11 122.6(3) 2_755 . ? O10 Sm1 O11 123.7(4) . . ? O15 Sm1 O12 79.7(3) 4_575 . ? O13 Sm1 O12 151.8(4) . . ? O4 Sm1 O12 72.3(3) 2_755 . ? O10 Sm1 O12 117.3(3) . . ? O11 Sm1 O12 50.4(4) . . ? O15 Sm1 O6 152.3(3) 4_575 . ? O13 Sm1 O6 122.1(3) . . ? O4 Sm1 O6 89.2(3) 2_755 . ? O10 Sm1 O6 49.8(4) . . ? O11 Sm1 O6 79.0(3) . . ? O12 Sm1 O6 72.6(4) . . ? O15 Sm1 O1 122.5(2) 4_575 . ? O13 Sm1 O1 87.3(2) . . ? O4 Sm1 O1 151.8(2) 2_755 . ? O10 Sm1 O1 68.6(3) . . ? O11 Sm1 O1 76.6(3) . . ? O12 Sm1 O1 120.8(3) . . ? O6 Sm1 O1 73.4(3) . . ? O15 Sm1 O2 71.5(2) 4_575 . ? O13 Sm1 O2 78.5(2) . . ? O4 Sm1 O2 149.9(3) 2_755 . ? O10 Sm1 O2 113.1(3) . . ? O11 Sm1 O2 70.6(3) . . ? O12 Sm1 O2 116.6(3) . . ? O6 Sm1 O2 120.8(3) . . ? O1 Sm1 O2 51.0(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C8 C46 C50 C49 169(2) . . . . ? O26 C46 C50 C49 0.0 . . . . ? C46 C50 C49 C48 0.0 . . . . ? C50 C49 C48 O26 0.0 . . . . ? C49 C48 O26 C46 0.0 . . . . ? C8 C46 O26 C48 -174.0(11) . . . . ? C50 C46 O26 C48 0.0 . . . . ? C38 C39 C40 C41 0.0 . . . . ? C39 C40 C41 O27 0.0 . . . . ? C40 C41 O27 C38 0.0 . . . . ? C41 O27 C38 C23 -179.5(15) . . . . ? C41 O27 C38 C39 0.0 . . . . ? C40 C39 C38 C23 179(2) . . . . ? C40 C39 C38 O27 0.0 . . . . ? C34 C42 O25 C37 -177.9(10) . . . . ? C43 C42 O25 C37 0.0 . . . . ? C42 O25 C37 C36 0.0 . . . . ? O25 C37 C36 C43 0.0 . . . . ? C34 C42 C43 C36 177.5(11) . . . . ? O25 C42 C43 C36 0.0 . . . . ? C37 C36 C43 C42 0.0 . . . . ? O19 C1 C2 C3 176.5(10) . . . . ? C6 C1 C2 C3 0.5(17) . . . . ? C1 C2 C3 C4 -2.4(19) . . . . ? C2 C3 C4 C5 3.6(19) . . . . ? C3 C4 C5 C6 -3.0(18) . . . . ? C4 C5 C6 C1 1.2(16) . . . . ? C4 C5 C6 C7 178.3(11) . . . . ? O19 C1 C6 C5 -176.1(9) . . . . ? C2 C1 C6 C5 0.0(15) . . . . ? O19 C1 C6 C7 7.0(15) . . . . ? C2 C1 C6 C7 -176.8(11) . . . . ? C5 C6 C7 O13 31.0(15) . . . . ? C1 C6 C7 O13 -152.1(9) . . . . ? C5 C6 C7 N6 -152.3(12) . . . . ? C1 C6 C7 N6 24.6(18) . . . . ? C50 C46 C8 N6 102(2) . . . . ? O26 C46 C8 N6 -88.9(17) . . . . ? O19 C11 C12 C24 -172.9(8) . . . . ? O19 C11 C12 C13 -55.4(10) . . . . ? O19 C11 C12 C15 68.2(10) . . . . ? C24 C12 C13 C14 72.1(11) . . . . ? C15 C12 C13 C14 -167.4(9) . . . . ? C11 C12 C13 C14 -45.9(12) . . . . ? C24 C12 C15 O17 65.0(11) . . . . ? C13 C12 C15 O17 -54.8(10) . . . . ? C11 C12 C15 O17 -176.4(8) . . . . ? O17 C16 C17 C18 178.2(12) . . . . ? C21 C16 C17 C18 -2.6(19) . . . . ? C16 C17 C18 C19 -1(2) . . . . ? C17 C18 C19 C20 2(2) . . . . ? C18 C19 C20 C21 1(2) . . . . ? C19 C20 C21 C16 -5(2) . . . . ? C19 C20 C21 C22 174.2(14) . . . . ? O17 C16 C21 C20 -175.4(10) . . . . ? C17 C16 C21 C20 5.4(18) . . . . ? O17 C16 C21 C22 5.8(17) . . . . ? C17 C16 C21 C22 -173.4(11) . . . . ? C20 C21 C22 N5 171.3(12) . . . . ? C16 C21 C22 N5 -9.9(19) . . . . ? C20 C21 C22 O4 -2.9(18) . . . . ? C16 C21 C22 O4 175.9(11) . . . . ? O27 C38 C23 N5 -72(3) . . . . ? C39 C38 C23 N5 109(2) . . . . ? C13 C12 C24 O18 179.8(7) . . . . ? C15 C12 C24 O18 57.2(11) . . . . ? C11 C12 C24 O18 -61.7(9) . . . . ? C32 C25 C26 C27 2.5(13) . . . . ? O18 C25 C26 C27 179.1(8) . . . . ? C25 C26 C27 C29 -3.8(16) . . . . ? C26 C27 C29 C31 4.1(19) . . . . ? C27 C29 C31 C32 -2.9(17) . . . . ? C29 C31 C32 C25 1.7(15) . . . . ? C29 C31 C32 C33 -177.9(10) . . . . ? O18 C25 C32 C31 -178.2(8) . . . . ? C26 C25 C32 C31 -1.6(14) . . . . ? O18 C25 C32 C33 1.4(13) . . . . ? C26 C25 C32 C33 178.0(8) . . . . ? C31 C32 C33 O15 40.3(14) . . . . ? C25 C32 C33 O15 -139.3(10) . . . . ? C31 C32 C33 N7 -133.7(11) . . . . ? C25 C32 C33 N7 46.7(14) . . . . ? C43 C42 C34 N7 109.1(10) . . . . ? O25 C42 C34 N7 -73.6(10) . . . . ? O4 C22 N5 C23 -5(2) . . . . ? C21 C22 N5 C23 -179.9(18) . . . . ? C38 C23 N5 C22 -172.6(18) . . . . ? O13 C7 N6 C8 -12(2) . . . . ? C6 C7 N6 C8 171.4(14) . . . . ? C46 C8 N6 C7 163.5(17) . . . . ? O15 C33 N7 C34 -0.1(16) . . . . ? C32 C33 N7 C34 173.7(10) . . . . ? C42 C34 N7 C33 128.2(11) . . . . ? O2 N1 O1 Sm1 -1.9(10) . . . . ? O3 N1 O1 Sm1 179.2(7) . . . . ? O1 N1 O2 Sm1 1.9(10) . . . . ? O3 N1 O2 Sm1 -179.2(8) . . . . ? N5 C22 O4 Sm1 99(2) . . . 2_745 ? C21 C22 O4 Sm1 -87(2) . . . 2_745 ? O10 N4 O6 Sm1 -1.1(18) . . . . ? O16 N4 O6 Sm1 179.4(14) . . . . ? O16 N4 O10 Sm1 -180(2) . . . . ? O6 N4 O10 Sm1 1.1(18) . . . . ? O14 N3 O11 Sm1 178.4(12) . . . . ? O12 N3 O11 Sm1 4.7(16) . . . . ? O14 N3 O12 Sm1 -178.1(13) . . . . ? O11 N3 O12 Sm1 -4.7(16) . . . . ? N6 C7 O13 Sm1 -105(3) . . . . ? C6 C7 O13 Sm1 72(3) . . . . ? N7 C33 O15 Sm1 64(3) . . . 4_576 ? C32 C33 O15 Sm1 -110(3) . . . 4_576 ? C21 C16 O17 C15 -174.7(10) . . . . ? C17 C16 O17 C15 4.4(16) . . . . ? C12 C15 O17 C16 -167.4(9) . . . . ? C32 C25 O18 C24 174.3(8) . . . . ? C26 C25 O18 C24 -2.4(11) . . . . ? C12 C24 O18 C25 -177.5(7) . . . . ? C2 C1 O19 C11 -5.6(13) . . . . ? C6 C1 O19 C11 170.4(8) . . . . ? C12 C11 O19 C1 -179.1(7) . . . . ? C7 O13 Sm1 O15 180(100) . . . 4_575 ? C7 O13 Sm1 O4 96(3) . . . 2_755 ? C7 O13 Sm1 O10 11(3) . . . . ? C7 O13 Sm1 O11 -115(2) . . . . ? C7 O13 Sm1 O12 126(3) . . . . ? C7 O13 Sm1 O6 11(3) . . . . ? C7 O13 Sm1 O1 -57(3) . . . . ? C7 O13 Sm1 O2 -108(3) . . . . ? N4 O10 Sm1 O15 153.2(10) . . . 4_575 ? N4 O10 Sm1 O13 179.1(13) . . . . ? N4 O10 Sm1 O4 94.0(12) . . . 2_755 ? N4 O10 Sm1 O11 -30.9(14) . . . . ? N4 O10 Sm1 O12 28.0(14) . . . . ? N4 O10 Sm1 O6 -0.7(11) . . . . ? N4 O10 Sm1 O1 -86.7(12) . . . . ? N4 O10 Sm1 O2 -112.3(12) . . . . ? N3 O11 Sm1 O15 -85.0(9) . . . 4_575 ? N3 O11 Sm1 O13 -149.9(8) . . . . ? N3 O11 Sm1 O4 -8.0(10) . . . 2_755 ? N3 O11 Sm1 O10 96.9(10) . . . . ? N3 O11 Sm1 O12 -2.6(9) . . . . ? N3 O11 Sm1 O6 73.8(9) . . . . ? N3 O11 Sm1 O1 149.2(9) . . . . ? N3 O11 Sm1 O2 -157.8(10) . . . . ? N3 O12 Sm1 O15 92.2(10) . . . 4_575 ? N3 O12 Sm1 O13 146.5(9) . . . . ? N3 O12 Sm1 O4 177.9(11) . . . 2_755 ? N3 O12 Sm1 O10 -109.8(10) . . . . ? N3 O12 Sm1 O11 2.7(9) . . . . ? N3 O12 Sm1 O6 -87.2(10) . . . . ? N3 O12 Sm1 O1 -29.6(11) . . . . ? N3 O12 Sm1 O2 29.1(11) . . . . ? N4 O6 Sm1 O15 -154.1(9) . . . 4_575 ? N4 O6 Sm1 O13 0.4(11) . . . . ? N4 O6 Sm1 O4 -81.2(10) . . . 2_755 ? N4 O6 Sm1 O10 0.6(10) . . . . ? N4 O6 Sm1 O11 155.4(10) . . . . ? N4 O6 Sm1 O12 -152.9(10) . . . . ? N4 O6 Sm1 O1 76.3(10) . . . . ? N4 O6 Sm1 O2 96.0(10) . . . . ? N1 O1 Sm1 O15 4.1(6) . . . 4_575 ? N1 O1 Sm1 O13 -76.3(5) . . . . ? N1 O1 Sm1 O4 -146.8(6) . . . 2_755 ? N1 O1 Sm1 O10 -148.3(6) . . . . ? N1 O1 Sm1 O11 76.8(5) . . . . ? N1 O1 Sm1 O12 101.8(6) . . . . ? N1 O1 Sm1 O6 159.1(6) . . . . ? N1 O1 Sm1 O2 1.0(5) . . . . ? N1 O2 Sm1 O15 -178.2(6) . . . 4_575 ? N1 O2 Sm1 O13 95.0(6) . . . . ? N1 O2 Sm1 O4 148.8(6) . . . 2_755 ? N1 O2 Sm1 O10 30.1(7) . . . . ? N1 O2 Sm1 O11 -89.1(6) . . . . ? N1 O2 Sm1 O12 -110.4(7) . . . . ? N1 O2 Sm1 O6 -25.6(7) . . . . ? N1 O2 Sm1 O1 -1.0(5) . . . . ? _diffrn_measured_fraction_theta_max 0.927 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.927 _refine_diff_density_max 0.860 _refine_diff_density_min -0.750 _refine_diff_density_rms 0.095