Supplementary Material (ESI) for Chemical Communications This journal is (c) The Royal Society of Chemistry 2003 data_global _publ_contact_author_email DKPN@CUHK.EDU.HK _publ_contact_author_name 'Prof Dennis K. P. Ng' _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name D.K.P.Ng Y.Bian J.Jiang C.-H.Lee J.Wang R.Wang data_Sm(Pc)[Pc(OC5H11)4] _database_code_CSD 202238 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C85 H77 Cl3 N16 O6 Sm' _chemical_formula_weight 1675.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 21.058(7) _cell_length_b 17.615(6) _cell_length_c 21.066(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.000(5) _cell_angle_gamma 90.00 _cell_volume 7815(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.424 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3440 _exptl_absorpt_coefficient_mu 0.920 _exptl_absorpt_correction_type 'SEMI-EMPIRICAL FROM EQUIVALENTS' _exptl_absorpt_correction_T_min 0.6563 _exptl_absorpt_correction_T_max 0.7699 _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40268 _diffrn_reflns_av_R_equivalents 0.0513 _diffrn_reflns_av_sigmaI/netI 0.0694 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 25.04 _reflns_number_total 13761 _reflns_number_gt 9050 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SIEMENS SHELXTL' _computing_publication_material 'SIEMENS 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^)+(0.1015P)^2^+138.5656P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13761 _refine_ls_number_parameters 1018 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1430 _refine_ls_R_factor_gt 0.1056 _refine_ls_wR_factor_ref 0.3165 _refine_ls_wR_factor_gt 0.2931 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.085 _refine_ls_shift/su_max 0.150 _refine_ls_shift/su_mean 0.003 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 Sm1 Sm 0.473830(0) 0.305850(0) 0.615860(0) 0.04174(0) Uani 1 1 d . . . N1 N 0.528470(7) 0.220360(9) 0.541490(7) 0.05554(5) Uani 1 1 d . . . N2 N 0.455770(8) 0.216180(10) 0.455440(8) 0.06369(6) Uani 1 1 d . . . N3 N 0.396570(7) 0.231160(9) 0.553390(7) 0.05422(5) Uani 1 1 d . . . N4 N 0.309100(8) 0.227460(10) 0.626060(8) 0.06604(6) Uani 1 1 d . . . N5 N 0.407280(7) 0.226270(9) 0.685890(7) 0.05489(5) Uani 1 1 d . . . N6 N 0.479490(8) 0.202200(10) 0.772610(8) 0.06490(6) Uani 1 1 d . . . N7 N 0.540570(7) 0.214230(9) 0.674840(7) 0.05346(5) Uani 1 1 d . . . N8 N 0.626060(8) 0.196530(9) 0.602160(8) 0.06068(5) Uani 1 1 d . . . N9 N 0.490690(7) 0.378720(8) 0.712850(6) 0.04819(4) Uani 1 1 d . . . N10 N 0.380810(8) 0.400800(10) 0.745720(8) 0.06511(6) Uani 1 1 d . . . N11 N 0.385410(7) 0.393960(8) 0.630600(7) 0.04890(4) Uani 1 1 d . . . N12 N 0.352390(6) 0.409010(8) 0.520160(7) 0.04918(4) Uani 1 1 d . . . N13 N 0.466390(7) 0.392130(8) 0.525090(7) 0.04718(4) Uani 1 1 d . . . N14 N 0.575770(7) 0.398090(8) 0.492550(7) 0.05076(5) Uani 1 1 d . . . N15 N 0.571980(6) 0.377880(8) 0.605950(6) 0.04543(4) Uani 1 1 d . . . N16 N 0.606820(7) 0.381540(9) 0.716880(7) 0.05423(5) Uani 1 1 d . . . O1 O 0.729220(8) 0.165800(13) 0.508190(8) 0.11410(8) Uani 1 1 d . . . O2 O 0.360600(9) 0.207829(14) 0.351040(8) 0.12112(9) Uani 1 1 d . . . O3 O 0.203310(7) 0.209510(11) 0.717700(8) 0.09964(7) Uani 1 1 d . . . O4 O 0.571270(8) 0.160890(12) 0.875330(7) 0.10044(7) Uani 1 1 d . . . O5 O 0.294110(10) 0.304790(12) 0.333590(10) 0.11531(8) Uani 1 1 d . . . C1 C 0.594360(9) 0.204190(11) 0.548060(10) 0.05943(6) Uani 1 1 d . . . C2 C 0.620620(10) 0.189790(13) 0.484560(10) 0.06823(7) Uani 1 1 d . . . C3 C 0.680340(11) 0.168870(15) 0.461250(11) 0.07832(8) Uani 1 1 d . . . C4 C 0.688080(14) 0.157710(18) 0.397980(13) 0.10569(11) Uani 1 1 d . . . H4B H 0.7279 0.1446 0.3824 0.127 Uiso 1 1 calc R . . C5 C 0.636670(12) 0.165740(18) 0.355470(11) 0.10033(10) Uani 1 1 d . . . H5A H 0.6431 0.1577 0.3123 0.120 Uiso 1 1 calc R . . C6 C 0.577760(12) 0.185110(16) 0.376710(12) 0.08978(10) Uani 1 1 d . . . H6B H 0.5439 0.1907 0.3487 0.108 Uiso 1 1 calc R . . C7 C 0.569760(10) 0.196260(12) 0.441700(9) 0.06224(6) Uani 1 1 d . . . C8 C 0.513200(10) 0.212500(11) 0.479500(9) 0.05882(6) Uani 1 1 d . . . C9 C 0.402160(10) 0.222120(11) 0.487820(9) 0.06344(6) Uani 1 1 d . . . C10 C 0.340860(11) 0.214460(13) 0.459410(10) 0.07449(7) Uani 1 1 d . . . C11 C 0.316210(12) 0.209080(16) 0.396950(12) 0.08861(9) Uani 1 1 d . . . C12 C 0.248930(12) 0.205940(18) 0.390340(12) 0.10564(11) Uani 1 1 d . . . H12B H 0.2319 0.1990 0.3500 0.127 Uiso 1 1 calc R . . C13 C 0.208760(13) 0.212660(18) 0.440300(12) 0.10047(11) Uani 1 1 d . . . H13A H 0.1653 0.2151 0.4330 0.121 Uiso 1 1 calc R . . C14 C 0.230500(12) 0.215890(17) 0.499980(13) 0.09894(10) Uani 1 1 d . . . H14 H 0.2034 0.2149 0.5349 0.119 Uiso 1 1 calc R . . C15 C 0.296550(9) 0.220810(13) 0.506530(11) 0.07576(7) Uani 1 1 d . . . C16 C 0.334980(9) 0.226850(12) 0.569700(10) 0.06002(6) Uani 1 1 d . . . C17 C 0.341520(9) 0.221780(10) 0.680470(8) 0.05235(6) Uani 1 1 d . . . C18 C 0.314900(11) 0.209340(14) 0.740970(12) 0.08040(8) Uani 1 1 d . . . C19 C 0.250640(10) 0.196490(15) 0.760790(10) 0.07606(8) Uani 1 1 d . . . C20 C 0.242270(12) 0.179110(18) 0.824170(12) 0.10152(11) Uani 1 1 d . . . H20A H 0.2012 0.1707 0.8389 0.122 Uiso 1 1 calc R . . C21 C 0.291960(12) 0.173600(19) 0.866690(12) 0.10666(11) Uani 1 1 d . . . H21A H 0.2837 0.1650 0.9095 0.128 Uiso 1 1 calc R . . C22 C 0.354020(12) 0.180830(18) 0.845780(12) 0.10224(11) Uani 1 1 d . . . H22A H 0.3884 0.1729 0.8727 0.123 Uiso 1 1 calc R . . C23 C 0.361980(9) 0.200410(13) 0.782780(9) 0.06447(7) Uani 1 1 d . . . C24 C 0.424660(10) 0.211750(11) 0.747330(9) 0.05851(6) Uani 1 1 d . . . C25 C 0.534060(8) 0.200970(11) 0.741870(9) 0.05397(6) Uani 1 1 d . . . C26 C 0.596000(10) 0.178750(13) 0.765260(11) 0.07403(8) Uani 1 1 d . . . C27 C 0.613740(11) 0.158090(16) 0.827130(10) 0.08200(9) Uani 1 1 d . . . C28 C 0.677700(12) 0.132180(19) 0.833750(14) 0.10638(11) Uani 1 1 d . . . H28A H 0.6917 0.1133 0.8725 0.128 Uiso 1 1 calc R . . C29 C 0.719290(12) 0.13514(2) 0.782050(12) 0.11920(12) Uani 1 1 d . . . H29A H 0.7618 0.1233 0.7888 0.143 Uiso 1 1 calc R . . C30 C 0.700840(13) 0.15416(2) 0.723330(14) 0.11063(12) Uani 1 1 d . . . H30A H 0.7284 0.1513 0.6889 0.133 Uiso 1 1 calc R . . C31 C 0.637220(8) 0.178790(13) 0.716370(9) 0.06077(6) Uani 1 1 d . . . C32 C 0.601180(9) 0.198630(11) 0.659270(9) 0.06045(6) Uani 1 1 d . . . C33 C 0.788750(13) 0.126260(19) 0.497511(15) 0.12832(12) Uani 1 1 d . . . H33A H 0.8136 0.1478 0.4626 0.154 Uiso 1 1 calc R . . C34 C 0.77256(2) 0.04280(3) 0.48784(2) 0.2359(3) Uani 1 1 d . . . H34A H 0.7393 0.0372 0.4564 0.283 Uiso 1 1 calc R . . H34B H 0.8096 0.0148 0.4737 0.283 Uiso 1 1 calc R . . C35 C 0.75056(3) 0.01426(2) 0.55122(2) 0.2161(3) Uani 1 1 d . . . H35A H 0.7406 -0.0388 0.5481 0.324 Uiso 1 1 calc R . . H35B H 0.7134 0.0418 0.5641 0.324 Uiso 1 1 calc R . . H35C H 0.7836 0.0215 0.5820 0.324 Uiso 1 1 calc R . . C36 C 0.822930(19) 0.12857(4) 0.56019(2) 0.3001(3) Uani 1 1 d . . . H36A H 0.7926 0.1264 0.5948 0.360 Uiso 1 1 calc R . . H36B H 0.8514 0.0855 0.5638 0.360 Uiso 1 1 calc R . . C37 C 0.859609(15) 0.20046(2) 0.56332(2) 0.17581(17) Uani 1 1 d . . . H37A H 0.8821 0.2029 0.6029 0.264 Uiso 1 1 calc R . . H37B H 0.8310 0.2428 0.5603 0.264 Uiso 1 1 calc R . . H37C H 0.8894 0.2022 0.5288 0.264 Uiso 1 1 calc R . . C38 C 0.358197(17) 0.15813(2) 0.288610(13) 0.15260(15) Uani 1 1 d . . . H38A H 0.3163 0.1458 0.2713 0.183 Uiso 1 1 calc R . . C39 C 0.40038(4) 0.09024(4) 0.31317(4) 0.4728(5) Uani 1 1 d . . . H39A H 0.4405 0.0886 0.2906 0.567 Uiso 1 1 calc R . . H39B H 0.4088 0.0954 0.3582 0.567 Uiso 1 1 calc R . . C41 C 0.40671(3) 0.19531(4) 0.243420(19) 0.2823(4) Uani 1 1 d . . . H41A H 0.4451 0.2087 0.2663 0.339 Uiso 1 1 calc R . . H41B H 0.4178 0.1607 0.2094 0.339 Uiso 1 1 calc R . . C42 C 0.37575(3) 0.26442(3) 0.21739(3) 0.2851(3) Uani 1 1 d . . . H42A H 0.4049 0.2905 0.1900 0.428 Uiso 1 1 calc R . . H42B H 0.3636 0.2973 0.2517 0.428 Uiso 1 1 calc R . . H42C H 0.3387 0.2501 0.1937 0.428 Uiso 1 1 calc R . . C43 C 0.143260(12) 0.173441(18) 0.722351(15) 0.10394(11) Uani 1 1 d . . . H43A H 0.1278 0.1832 0.7655 0.125 Uiso 1 1 calc R . . C44 C 0.149381(15) 0.08829(2) 0.716190(16) 0.12610(14) Uani 1 1 d . . . H44A H 0.1716 0.0681 0.7528 0.151 Uiso 1 1 calc R . . H44B H 0.1075 0.0655 0.7147 0.151 Uiso 1 1 calc R . . C45 C 0.18521(2) 0.06883(2) 0.65694(3) 0.2307(3) Uani 1 1 d . . . H45A H 0.1902 0.0148 0.6541 0.346 Uiso 1 1 calc R . . H45B H 0.2263 0.0924 0.6581 0.346 Uiso 1 1 calc R . . H45C H 0.1621 0.0868 0.6206 0.346 Uiso 1 1 calc R . . C46 C 0.105540(11) 0.218489(14) 0.681260(12) 0.08143(8) Uani 1 1 d . . . H46A H 0.1126 0.2058 0.6390 0.098 Uiso 1 1 calc R . . C47 C 0.06708(4) 0.26837(6) 0.685721(18) 0.5324(7) Uani 1 1 d . . . H47A H 0.0511 0.2809 0.6443 0.799 Uiso 1 1 calc R . . H47B H 0.0866 0.3123 0.7042 0.799 Uiso 1 1 calc R . . H47C H 0.0326 0.2518 0.7122 0.799 Uiso 1 1 calc R . . C48 C 0.575370(14) 0.11399(2) 0.929290(13) 0.13449(14) Uani 1 1 d . . . H48A H 0.6175 0.1180 0.9487 0.161 Uiso 1 1 calc R . . C49 C 0.52502(3) 0.14029(4) 0.974870(19) 0.3080(3) Uani 1 1 d . . . H49A H 0.5235 0.1071 1.0116 0.370 Uiso 1 1 calc R . . H49B H 0.4837 0.1399 0.9545 0.370 Uiso 1 1 calc R . . C51 C 0.56121(4) 0.03303(3) 0.91200(2) 0.5720(4) Uani 1 1 d . . . H51A H 0.5554 0.0029 0.9501 0.686 Uiso 1 1 calc R . . H51B H 0.5962 0.0117 0.8879 0.686 Uiso 1 1 calc R . . C52 C 0.50142(2) 0.03250(3) 0.87279(3) 0.3191(4) Uani 1 1 d . . . H52A H 0.4912 -0.0188 0.8611 0.479 Uiso 1 1 calc R . . H52B H 0.5078 0.0623 0.8351 0.479 Uiso 1 1 calc R . . H52C H 0.4672 0.0537 0.8971 0.479 Uiso 1 1 calc R . . C53 C 0.547680(9) 0.383920(10) 0.742130(8) 0.05065(5) Uani 1 1 d . . . C54 C 0.536800(11) 0.397800(12) 0.810820(9) 0.06724(7) Uani 1 1 d . . . C55 C 0.579210(12) 0.411370(15) 0.859720(10) 0.08335(9) Uani 1 1 d . . . H55A H 0.6230 0.4113 0.8543 0.100 Uiso 1 1 calc R . . C56 C 0.548760(15) 0.42575(2) 0.920130(11) 0.12858(14) Uani 1 1 d . . . H56A H 0.5748 0.4324 0.9554 0.154 Uiso 1 1 calc R . . C57 C 0.488060(14) 0.43005(2) 0.928720(12) 0.14091(15) Uani 1 1 d . . . H57A H 0.4715 0.4425 0.9683 0.169 Uiso 1 1 calc R . . C58 C 0.448790(14) 0.415940(18) 0.878430(10) 0.10526(11) Uani 1 1 d . . . H58A H 0.4051 0.4154 0.8846 0.126 Uiso 1 1 calc R . . C59 C 0.473060(9) 0.402600(12) 0.818890(9) 0.06022(6) Uani 1 1 d . . . C60 C 0.443300(9) 0.393280(11) 0.756110(8) 0.05573(6) Uani 1 1 d . . . C61 C 0.354350(9) 0.402930(11) 0.686350(9) 0.05593(6) Uani 1 1 d . . . C62 C 0.288380(9) 0.421360(13) 0.675070(11) 0.06746(7) Uani 1 1 d . . . C63 C 0.237070(10) 0.437280(15) 0.716110(13) 0.08994(9) Uani 1 1 d . . . H63A H 0.2423 0.4369 0.7599 0.108 Uiso 1 1 calc R . . C64 C 0.181310(11) 0.452720(19) 0.690270(14) 0.11023(12) Uani 1 1 d . . . H64A H 0.1476 0.4649 0.7169 0.132 Uiso 1 1 calc R . . C65 C 0.170590(12) 0.451530(19) 0.623820(14) 0.11340(12) Uani 1 1 d . . . H65A H 0.1302 0.4606 0.6076 0.136 Uiso 1 1 calc R . . C66 C 0.221300(10) 0.436640(15) 0.583050(12) 0.08449(9) Uani 1 1 d . . . H66A H 0.2163 0.4359 0.5392 0.101 Uiso 1 1 calc R . . C67 C 0.279960(9) 0.422850(12) 0.611860(10) 0.06031(6) Uani 1 1 d . . . C68 C 0.342110(8) 0.407170(10) 0.583270(9) 0.05300(6) Uani 1 1 d . . . C69 C 0.409220(8) 0.404230(9) 0.494400(8) 0.04509(5) Uani 1 1 d . . . C70 C 0.420230(8) 0.415590(10) 0.427780(8) 0.04794(5) Uani 1 1 d . . . C71 C 0.380040(10) 0.428320(12) 0.375550(9) 0.06540(7) Uani 1 1 d . . . H71A H 0.3362 0.4301 0.3806 0.078 Uiso 1 1 calc R . . C72 C 0.406960(12) 0.437920(13) 0.317410(10) 0.08114(8) Uani 1 1 d . . . H72A H 0.3811 0.4464 0.2823 0.097 Uiso 1 1 calc R . . C73 C 0.474000(11) 0.435130(13) 0.309430(10) 0.07047(7) Uani 1 1 d . . . H73A H 0.4911 0.4394 0.2689 0.085 Uiso 1 1 calc R . . C74 C 0.513560(10) 0.426410(12) 0.359680(9) 0.06226(7) Uani 1 1 d . . . H74A H 0.5574 0.4284 0.3548 0.075 Uiso 1 1 calc R . . C75 C 0.485970(9) 0.414370(11) 0.418910(8) 0.05365(6) Uani 1 1 d . . . C76 C 0.513440(8) 0.398690(10) 0.481880(8) 0.04499(5) Uani 1 1 d . . . C77 C 0.601060(8) 0.391830(10) 0.549390(8) 0.04696(5) Uani 1 1 d . . . C78 C 0.670010(8) 0.400460(11) 0.560330(9) 0.05099(6) Uani 1 1 d . . . C79 C 0.720790(10) 0.414210(13) 0.520660(11) 0.07222(7) Uani 1 1 d . . . H79A H 0.7155 0.4178 0.4769 0.087 Uiso 1 1 calc R . . C80 C 0.779710(9) 0.422400(16) 0.548190(12) 0.09221(9) Uani 1 1 d . . . H80A H 0.8147 0.4315 0.5223 0.111 Uiso 1 1 calc R . . C81 C 0.788570(11) 0.417500(17) 0.613140(14) 0.10834(11) Uani 1 1 d . . . H81A H 0.8290 0.4244 0.6299 0.130 Uiso 1 1 calc R . . C82 C 0.738760(10) 0.402710(17) 0.653330(13) 0.09468(10) Uani 1 1 d . . . H82A H 0.7446 0.3991 0.6970 0.114 Uiso 1 1 calc R . . C83 C 0.679050(8) 0.393280(11) 0.625830(9) 0.05497(6) Uani 1 1 d . . . C84 C 0.616120(8) 0.382600(10) 0.654180(8) 0.04965(5) Uani 1 1 d . . . C85 C -0.54725(2) 0.06745(2) 0.616499(14) 0.15986(17) Uani 1 1 d . . . Cl1 Cl -0.490261(16) 0.017311(14) 0.57999(2) 0.3240(2) Uani 0.60 1 d P A 1 Cl2 Cl -0.549059(15) 0.025650(11) 0.690260(10) 0.23113(13) Uani 0.60 1 d P A 1 Cl1' Cl -0.54885(5) 0.02951(3) 0.561710(19) 0.6362(6) Uani 0.40 1 d P A 2 Cl2' Cl -0.61894(3) 0.04502(2) 0.67450(2) 1.1923(2) Uani 0.40 1 d P A 2 Cl3 Cl -0.614879(12) 0.033690(11) 0.58290(2) 0.5948(2) Uani 1 1 d . A . C40 C 0.36302(3) 0.02124(5) 0.30056(4) 0.4324(6) Uani 1 1 d . . . H40A H 0.3869 -0.0226 0.3133 0.649 Uiso 1 1 calc R . . H40B H 0.3537 0.0181 0.2560 0.649 Uiso 1 1 calc R . . H40C H 0.3240 0.0232 0.3241 0.649 Uiso 1 1 calc R . . C50 C 0.54244(2) 0.22036(5) 0.99489(3) 0.4055(4) Uani 1 1 d . . . H50A H 0.5101 0.2401 1.0224 0.608 Uiso 1 1 calc R . . H50B H 0.5460 0.2520 0.9580 0.608 Uiso 1 1 calc R . . H50C H 0.5823 0.2196 1.0170 0.608 Uiso 1 1 calc R . . O6 O 0.39839(2) 0.30218(2) 0.87607(2) 0.2487(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sm1 0.04178(0) 0.04315(0) 0.04030(0) 0.00125(0) -0.00230(0) -0.00128(0) N1 0.06236(9) 0.05617(9) 0.04809(8) -0.00892(7) -0.00038(7) 0.00139(8) N2 0.06661(10) 0.07127(10) 0.05318(9) -0.00883(8) -0.00034(8) -0.00696(9) N3 0.04633(8) 0.04839(8) 0.06794(9) -0.00260(8) -0.00836(7) -0.01269(7) N4 0.05846(9) 0.06352(10) 0.07614(10) 0.00889(9) -0.01165(8) -0.01446(8) N5 0.05616(8) 0.05375(8) 0.05477(8) 0.00050(7) 0.00463(7) -0.00653(7) N6 0.06310(9) 0.06928(10) 0.06231(9) 0.02066(8) 0.00429(8) 0.00331(8) N7 0.04926(8) 0.06210(9) 0.04901(8) 0.00882(7) -0.00500(7) 0.00050(7) N8 0.06545(9) 0.05768(9) 0.05891(9) -0.00473(8) -0.00286(8) 0.02187(8) N9 0.05327(8) 0.04779(8) 0.04351(7) -0.00203(7) -0.00718(7) -0.00469(7) N10 0.05586(9) 0.07668(11) 0.06279(9) -0.00558(9) 0.01052(8) 0.00845(8) N11 0.04307(7) 0.05274(8) 0.05089(8) 0.00339(7) -0.00101(6) -0.00104(7) N12 0.04186(7) 0.05275(8) 0.05294(8) 0.00762(7) -0.00966(6) -0.00121(7) N13 0.04605(7) 0.04489(8) 0.05061(8) 0.00741(7) -0.00470(6) -0.00320(6) N14 0.05468(8) 0.05296(8) 0.04464(7) 0.00750(7) 0.00417(7) -0.00721(7) N15 0.04228(7) 0.05496(8) 0.03904(7) 0.00431(7) -0.00317(6) -0.00183(7) N16 0.05300(8) 0.06162(9) 0.04807(8) -0.00074(7) -0.01675(7) -0.00988(7) O1 0.08105(10) 0.17823(17) 0.08302(11) -0.03320(12) -0.00528(9) 0.03827(11) O2 0.09355(12) 0.1964(2) 0.07342(10) -0.02890(12) -0.00700(10) -0.02190(13) O3 0.05394(8) 0.14640(15) 0.09859(11) 0.04198(10) 0.00751(8) -0.01321(9) O4 0.08299(10) 0.14862(15) 0.06971(9) 0.03301(10) -0.00860(8) 0.00597(11) O5 0.11054(14) 0.11688(15) 0.11851(14) -0.00886(12) -0.01737(12) 0.00091(12) C1 0.05740(10) 0.05353(11) 0.06735(11) -0.00149(9) 0.01705(9) 0.01135(9) C2 0.06662(12) 0.08341(14) 0.05466(11) -0.01248(11) 0.00540(10) 0.01074(11) C3 0.07273(13) 0.09911(17) 0.06312(12) -0.00490(13) 0.00380(11) 0.00245(13) C4 0.10560(19) 0.1200(2) 0.09144(17) -0.03279(16) 0.01272(15) 0.01510(17) C5 0.08903(16) 0.1544(2) 0.05758(12) -0.02971(14) 0.01224(12) 0.01846(17) C6 0.07903(15) 0.1183(2) 0.07203(14) -0.00973(15) -0.00425(12) 0.00180(15) C7 0.07493(12) 0.06365(11) 0.04815(9) -0.00917(9) 0.01707(9) 0.01073(10) C8 0.07135(12) 0.05195(11) 0.05316(10) -0.00396(9) 0.00422(9) -0.00789(9) C9 0.07806(12) 0.05195(10) 0.06032(11) -0.01515(9) -0.02192(10) -0.00842(10) C10 0.08060(13) 0.08915(14) 0.05372(11) -0.00944(11) 0.00009(10) -0.03391(11) C11 0.07730(14) 0.1168(2) 0.07178(14) -0.00418(14) -0.02025(12) -0.01827(14) C12 0.09758(16) 0.1438(2) 0.07553(14) 0.00996(15) -0.04678(11) -0.02554(16) C13 0.08235(15) 0.1349(2) 0.08417(16) 0.00292(16) -0.03065(13) 0.00123(16) C14 0.07508(14) 0.1183(2) 0.10339(18) 0.01146(16) -0.03122(13) -0.01503(15) C15 0.05911(10) 0.06702(12) 0.10114(14) 0.01844(11) -0.04450(9) -0.01496(10) C16 0.05520(10) 0.05638(11) 0.06849(12) -0.00140(10) -0.00393(9) -0.00947(9) C17 0.06293(10) 0.04478(9) 0.04935(9) 0.00204(8) 0.01540(8) -0.00956(8) C18 0.07432(14) 0.08471(15) 0.08218(14) 0.01902(12) -0.00584(12) -0.01063(12) C19 0.04730(10) 0.11588(18) 0.06500(12) 0.02339(12) 0.00628(9) -0.00259(12) C20 0.06901(14) 0.1634(3) 0.07212(14) 0.01837(17) 0.00314(12) -0.00815(17) C21 0.07681(15) 0.1693(3) 0.07392(14) 0.03099(16) 0.02047(12) 0.00779(17) C22 0.07736(15) 0.1555(3) 0.07390(14) 0.02381(16) 0.01133(13) -0.00287(17) C23 0.05704(11) 0.08623(14) 0.05015(10) 0.01437(10) -0.00510(9) -0.00748(11) C24 0.07719(12) 0.04946(10) 0.04889(10) 0.01167(8) -0.00204(9) 0.00549(9) C25 0.04514(9) 0.05698(10) 0.05980(10) 0.00689(9) -0.00671(8) 0.01645(8) C26 0.06339(12) 0.08143(15) 0.07728(13) 0.00977(12) -0.01716(11) 0.01120(11) C27 0.07571(14) 0.11702(18) 0.05328(11) 0.01460(13) -0.01265(11) -0.00229(14) C28 0.07512(15) 0.1463(2) 0.09770(18) 0.02661(18) -0.00137(14) 0.01670(17) C29 0.06663(13) 0.2090(3) 0.08197(15) 0.02725(18) -0.02321(12) 0.04502(16) C30 0.08179(17) 0.1509(3) 0.09921(19) 0.0063(2) -0.00812(15) -0.00010(19) C31 0.04141(9) 0.08708(14) 0.05383(10) 0.00133(10) -0.01166(8) 0.01080(9) C32 0.05992(11) 0.06174(11) 0.05970(11) -0.00242(10) -0.00147(9) 0.01745(9) C33 0.10838(16) 0.1452(2) 0.1313(2) 0.00975(19) 0.06704(14) 0.04868(16) C34 0.1787(4) 0.3080(6) 0.2209(5) -0.0842(4) 0.0120(4) 0.0737(4) C35 0.3157(6) 0.1189(3) 0.2136(5) 0.0288(3) 0.0293(5) 0.0356(4) C36 0.1942(3) 0.3016(6) 0.4044(5) -0.1213(5) -0.2197(2) 0.0926(3) C37 0.1205(2) 0.1595(3) 0.2474(3) -0.0577(3) 0.10288(19) -0.0077(2) C38 0.1799(3) 0.1933(3) 0.08457(15) -0.0169(2) -0.08185(14) 0.0046(3) C39 0.4523(8) 0.3968(7) 0.5693(12) -0.2163(8) -0.2152(8) 0.2963(5) C41 0.2670(6) 0.4969(11) 0.0829(3) 0.0314(4) -0.0183(3) 0.0735(6) C42 0.2973(6) 0.2690(5) 0.2889(5) -0.1438(4) -0.1026(5) 0.1384(4) C43 0.06520(14) 0.1261(2) 0.1205(2) 0.00693(19) -0.00764(15) -0.00239(15) C44 0.1053(2) 0.1268(3) 0.1461(3) 0.0085(2) -0.0177(2) -0.0115(2) C45 0.2000(4) 0.0918(2) 0.4003(7) 0.0533(4) 0.0230(5) -0.0253(3) C46 0.07406(14) 0.09073(16) 0.07949(14) -0.00540(13) -0.01344(12) -0.00572(13) C47 0.6454(12) 0.9148(17) 0.03704(18) -0.0484(5) 0.0605(4) 0.3069(11) C48 0.08263(17) 0.2225(3) 0.09829(18) 0.0613(2) -0.01530(15) 0.0170(2) C49 0.2796(6) 0.4924(7) 0.1521(2) 0.1994(3) 0.0455(3) -0.0287(5) C51 1.0555(9) 0.4099(4) 0.2506(4) 0.2408(3) 0.3669(5) 0.5388(4) C52 0.1320(3) 0.2596(5) 0.5657(9) 0.1928(5) -0.0834(5) -0.0607(4) C53 0.05590(10) 0.05148(10) 0.04457(9) 0.00493(8) -0.00811(8) -0.01085(8) C54 0.09278(14) 0.06933(13) 0.03960(9) -0.00084(9) -0.01147(10) -0.00096(12) C55 0.08006(14) 0.11411(19) 0.05588(12) -0.00121(13) -0.01379(11) -0.01079(14) C56 0.1448(2) 0.2059(3) 0.03512(11) -0.01641(17) -0.02699(13) 0.0114(2) C57 0.09565(19) 0.2691(4) 0.05799(13) -0.05559(18) -0.00390(14) 0.0157(2) C58 0.10675(18) 0.1650(3) 0.04404(11) -0.02983(14) -0.01255(12) 0.00360(19) C59 0.06056(11) 0.07156(12) 0.04853(10) -0.00831(10) -0.00035(9) -0.00462(10) C60 0.07601(12) 0.05097(10) 0.04020(9) -0.00924(8) 0.01554(8) -0.00258(9) C61 0.05120(10) 0.06147(11) 0.05511(10) -0.00226(9) 0.00814(8) 0.01172(9) C62 0.05022(10) 0.06659(12) 0.08557(14) -0.00020(12) 0.00716(10) -0.00090(10) C63 0.05835(11) 0.10883(18) 0.10263(16) -0.00442(15) 0.03144(11) 0.01752(13) C64 0.05937(13) 0.1449(3) 0.1265(2) -0.0008(2) 0.02819(14) 0.01357(16) C65 0.05929(13) 0.1614(3) 0.1195(2) 0.0234(2) 0.01149(14) 0.03065(16) C66 0.04883(11) 0.11424(18) 0.09040(15) 0.03387(14) 0.00665(11) 0.01191(12) C67 0.04707(9) 0.06320(11) 0.07066(12) 0.01618(10) 0.00581(9) 0.00365(9) C68 0.04109(9) 0.04923(10) 0.06869(11) 0.01141(9) -0.00191(8) 0.00682(8) C69 0.04867(9) 0.03924(8) 0.04736(9) 0.01297(7) -0.01043(7) -0.00284(7) C70 0.05609(9) 0.04230(9) 0.04543(9) 0.00285(8) -0.01364(8) 0.00528(8) C71 0.07215(12) 0.06469(12) 0.05935(11) 0.00774(10) -0.01091(10) -0.00121(11) C72 0.12401(18) 0.07159(14) 0.04781(10) 0.00644(10) -0.02586(11) 0.01015(13) C73 0.09040(14) 0.07113(13) 0.04989(11) 0.00399(10) -0.00737(11) -0.00065(12) C74 0.07527(12) 0.06655(12) 0.04495(9) 0.00427(9) -0.00135(9) -0.00995(11) C75 0.06753(11) 0.05279(10) 0.04062(9) 0.00166(8) -0.00556(8) -0.01250(9) C76 0.04651(9) 0.04479(9) 0.04367(9) 0.00911(8) -0.00318(7) -0.00437(8) C77 0.03812(8) 0.05551(10) 0.04725(9) -0.00443(8) 0.00353(7) -0.00205(8) C78 0.03956(8) 0.05386(10) 0.05956(10) 0.00295(9) 0.01160(8) -0.00440(8) C79 0.05791(11) 0.07832(14) 0.08042(14) 0.01248(12) 0.00734(11) 0.00685(11) C80 0.03476(9) 0.12707(19) 0.11479(17) 0.04814(15) 0.01016(11) -0.00559(12) C81 0.05282(12) 0.1336(2) 0.1386(2) 0.05420(17) -0.01790(14) -0.00844(14) C82 0.04289(10) 0.1378(2) 0.10335(16) 0.03009(16) -0.02294(11) -0.00774(13) C83 0.04308(9) 0.06243(11) 0.05940(10) 0.01069(9) -0.01086(8) -0.00887(8) C84 0.04493(9) 0.04975(9) 0.05426(10) 0.00862(8) -0.00781(8) -0.00534(8) C85 0.2532(4) 0.1506(3) 0.07577(18) -0.02599(19) -0.0060(2) 0.0813(3) Cl1 0.3085(3) 0.12780(16) 0.5358(5) 0.0260(3) 0.0863(4) 0.06602(18) Cl2 0.4124(3) 0.10349(11) 0.17749(16) -0.03434(11) 0.07773(19) -0.02516(17) Cl1' 1.5503(16) 0.1375(3) 0.2207(3) -0.0110(3) 0.3952(4) -0.0286(6) Cl2' 2.0000(4) 0.1105(2) 1.4665(3) 0.1341(2) 1.6374(2) 0.1655(3) Cl3 0.4564(2) 0.13812(13) 1.1899(6) 0.0320(3) -0.4165(3) -0.06833(15) C40 0.1756(4) 0.6169(12) 0.5046(11) -0.1780(9) -0.0638(5) -0.1446(5) C50 0.2186(3) 0.4579(10) 0.5399(7) 0.2098(7) 0.2566(3) 0.1167(5) O6 0.2781(4) 0.2244(4) 0.2436(4) -0.0150(3) -0.0107(3) 0.0153(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 Sm1 N15 2.4342(6) . ? Sm1 N9 2.4390(6) . ? Sm1 N11 2.4438(6) . ? Sm1 N13 2.4477(6) . ? Sm1 N1 2.4589(5) . ? Sm1 N5 2.4709(5) . ? Sm1 N3 2.4718(5) . ? Sm1 N7 2.4746(5) . ? N1 C8 1.3520(5) . ? N1 C1 1.4232(5) . ? N2 C8 1.3129(5) . ? N2 C9 1.3231(4) . ? N3 C16 1.3439(5) . ? N3 C9 1.3955(5) . ? N4 C16 1.3064(5) . ? N4 C17 1.3379(4) . ? N5 C24 1.3692(5) . ? N5 C17 1.3917(5) . ? N6 C24 1.2826(5) . ? N6 C25 1.3192(4) . ? N7 C32 1.3461(5) . ? N7 C25 1.4378(5) . ? N8 C32 1.3128(5) . ? N8 C1 1.3277(4) . ? N9 C53 1.3524(4) . ? N9 C60 1.3756(4) . ? N10 C60 1.3406(5) . ? N10 C61 1.3697(5) . ? N11 C61 1.3536(4) . ? N11 C68 1.3710(4) . ? N12 C69 1.3167(4) . ? N12 C68 1.3474(5) . ? N13 C76 1.3504(4) . ? N13 C69 1.3830(4) . ? N14 C77 1.3151(4) . ? N14 C76 1.3317(5) . ? N15 C77 1.3620(4) . ? N15 C84 1.3796(4) . ? N16 C84 1.3354(5) . ? N16 C53 1.3549(5) . ? O1 C3 1.4284(4) . ? O1 C33 1.4516(5) . ? O2 C11 1.3452(4) . ? O2 C38 1.5807(6) . ? O3 C19 1.3675(4) . ? O3 C43 1.4186(5) . ? O4 C27 1.3540(4) . ? O4 C48 1.4079(5) . ? C1 C2 1.4696(5) . ? C2 C3 1.3994(5) . ? C2 C7 1.4055(4) . ? C3 C4 1.3571(6) . ? C4 C5 1.4121(5) . ? C5 C6 1.3622(5) . ? C6 C7 1.3933(5) . ? C7 C8 1.4610(5) . ? C9 C10 1.4292(5) . ? C10 C15 1.3669(4) . ? C10 C11 1.4177(5) . ? C11 C12 1.4247(6) . ? C12 C13 1.3555(5) . ? C13 C14 1.3392(5) . ? C14 C15 1.4004(6) . ? C15 C16 1.5611(5) . ? C17 C18 1.4095(5) . ? C18 C23 1.3354(5) . ? C18 C19 1.4341(5) . ? C19 C20 1.3811(5) . ? C20 C21 1.3808(5) . ? C21 C22 1.3850(6) . ? C22 C23 1.3815(5) . ? C23 C24 1.5296(5) . ? C25 C26 1.4482(5) . ? C26 C31 1.3469(4) . ? C26 C27 1.4039(5) . ? C27 C28 1.4289(6) . ? C28 C29 1.3986(5) . ? C29 C30 1.3392(6) . ? C30 C31 1.4158(6) . ? C31 C32 1.4646(5) . ? C33 C36 1.5043(7) . ? C33 C34 1.5229(8) . ? C34 C35 1.4999(8) . ? C36 C37 1.4847(8) . ? C38 C41 1.5423(7) . ? C38 C39 1.5770(9) . ? C39 C40 1.4719(12) . ? C41 C42 1.4858(9) . ? C43 C46 1.4177(5) . ? C43 C44 1.5111(7) . ? C44 C45 1.4983(7) . ? C46 C47 1.1987(11) . ? C48 C51 1.5018(8) . ? C48 C49 1.5036(7) . ? C49 C50 1.5172(11) . ? C51 C52 1.5058(10) . ? C53 C54 1.4853(5) . ? C54 C59 1.3556(5) . ? C54 C55 1.3842(4) . ? C55 C56 1.4474(5) . ? C56 C57 1.2932(6) . ? C57 C58 1.3668(5) . ? C58 C59 1.3747(5) . ? C59 C60 1.4727(5) . ? C61 C62 1.4463(5) . ? C62 C67 1.3436(5) . ? C62 C63 1.4119(5) . ? C63 C64 1.3225(5) . ? C64 C65 1.4181(6) . ? C65 C66 1.3953(5) . ? C66 C67 1.3976(5) . ? C67 C68 1.4669(5) . ? C69 C70 1.4365(5) . ? C70 C75 1.3971(5) . ? C70 C71 1.4061(4) . ? C71 C72 1.3602(5) . ? C72 C73 1.4226(6) . ? C73 C74 1.3558(4) . ? C74 C75 1.3926(5) . ? C75 C76 1.4733(5) . ? C77 C78 1.4780(5) . ? C78 C79 1.3786(4) . ? C78 C83 1.3987(5) . ? C79 C80 1.3772(5) . ? C80 C81 1.3836(6) . ? C81 C82 1.3729(5) . ? C82 C83 1.3943(5) . ? C83 C84 1.4657(5) . ? C85 Cl1' 1.3341(6) . ? C85 Cl1 1.6768(6) . ? C85 Cl3 1.6979(7) . ? C85 Cl2 1.7199(6) . ? C85 Cl2' 1.9820(8) . ? Cl1' Cl3 1.4622(11) . ? Cl2' Cl3 1.9419(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N15 Sm1 N9 70.968(12) . . ? N15 Sm1 N11 109.07(3) . . ? N9 Sm1 N11 70.743(14) . . ? N15 Sm1 N13 70.347(13) . . ? N9 Sm1 N13 109.69(3) . . ? N11 Sm1 N13 69.887(15) . . ? N15 Sm1 N1 82.37(2) . . ? N9 Sm1 N1 141.997(14) . . ? N11 Sm1 N1 145.735(10) . . ? N13 Sm1 N1 84.98(2) . . ? N15 Sm1 N5 145.944(10) . . ? N9 Sm1 N5 83.16(2) . . ? N11 Sm1 N5 81.51(2) . . ? N13 Sm1 N5 141.482(13) . . ? N1 Sm1 N5 107.36(2) . . ? N15 Sm1 N3 142.246(13) . . ? N9 Sm1 N3 145.283(9) . . ? N11 Sm1 N3 84.50(2) . . ? N13 Sm1 N3 82.67(2) . . ? N1 Sm1 N3 69.07(2) . . ? N5 Sm1 N3 69.06(2) . . ? N15 Sm1 N7 84.31(2) . . ? N9 Sm1 N7 80.79(2) . . ? N11 Sm1 N7 141.547(14) . . ? N13 Sm1 N7 146.469(11) . . ? N1 Sm1 N7 69.80(2) . . ? N5 Sm1 N7 69.65(2) . . ? N3 Sm1 N7 107.10(2) . . ? C8 N1 C1 107.777(17) . . ? C8 N1 Sm1 124.531(19) . . ? C1 N1 Sm1 121.118(16) . . ? C8 N2 C9 126.21(3) . . ? C16 N3 C9 109.151(18) . . ? C16 N3 Sm1 121.95(2) . . ? C9 N3 Sm1 122.157(17) . . ? C16 N4 C17 124.41(3) . . ? C24 N5 C17 109.446(17) . . ? C24 N5 Sm1 121.25(2) . . ? C17 N5 Sm1 123.201(16) . . ? C24 N6 C25 125.63(3) . . ? C32 N7 C25 107.250(16) . . ? C32 N7 Sm1 123.317(18) . . ? C25 N7 Sm1 123.019(15) . . ? C32 N8 C1 125.67(3) . . ? C53 N9 C60 109.21(3) . . ? C53 N9 Sm1 123.154(14) . . ? C60 N9 Sm1 123.20(2) . . ? C60 N10 C61 123.443(17) . . ? C61 N11 C68 106.85(3) . . ? C61 N11 Sm1 123.542(15) . . ? C68 N11 Sm1 121.473(19) . . ? C69 N12 C68 123.446(16) . . ? C76 N13 C69 108.08(3) . . ? C76 N13 Sm1 122.194(18) . . ? C69 N13 Sm1 121.106(14) . . ? C77 N14 C76 123.605(16) . . ? C77 N15 C84 109.30(3) . . ? C77 N15 Sm1 123.424(14) . . ? C84 N15 Sm1 122.706(19) . . ? C84 N16 C53 121.513(17) . . ? C3 O1 C33 122.22(3) . . ? C11 O2 C38 125.80(3) . . ? C19 O3 C43 121.92(3) . . ? C27 O4 C48 122.93(3) . . ? N8 C1 N1 126.44(2) . . ? N8 C1 C2 125.08(3) . . ? N1 C1 C2 108.23(2) . . ? C3 C2 C7 118.73(3) . . ? C3 C2 C1 134.67(2) . . ? C7 C2 C1 106.50(3) . . ? C4 C3 C2 119.39(2) . . ? C4 C3 O1 126.01(3) . . ? C2 C3 O1 114.50(3) . . ? C3 C4 C5 121.08(3) . . ? C6 C5 C4 120.99(3) . . ? C5 C6 C7 117.92(2) . . ? C6 C7 C2 121.85(3) . . ? C6 C7 C8 131.43(2) . . ? C2 C7 C8 106.68(3) . . ? N2 C8 N1 125.939(19) . . ? N2 C8 C7 123.38(3) . . ? N1 C8 C7 110.65(3) . . ? N2 C9 N3 126.25(2) . . ? N2 C9 C10 123.18(3) . . ? N3 C9 C10 110.43(2) . . ? C15 C10 C11 115.44(3) . . ? C15 C10 C9 107.74(3) . . ? C11 C10 C9 136.53(2) . . ? O2 C11 C10 114.45(3) . . ? O2 C11 C12 128.32(3) . . ? C10 C11 C12 117.22(2) . . ? C13 C12 C11 122.77(3) . . ? C14 C13 C12 121.29(3) . . ? C13 C14 C15 115.76(3) . . ? C10 C15 C14 126.97(3) . . ? C10 C15 C16 105.71(3) . . ? C14 C15 C16 127.09(2) . . ? N4 C16 N3 129.382(19) . . ? N4 C16 C15 123.99(3) . . ? N3 C16 C15 106.63(3) . . ? N4 C17 N5 125.01(2) . . ? N4 C17 C18 125.69(3) . . ? N5 C17 C18 109.29(2) . . ? C23 C18 C17 108.63(3) . . ? C23 C18 C19 119.33(3) . . ? C17 C18 C19 131.53(2) . . ? O3 C19 C20 125.87(3) . . ? O3 C19 C18 117.90(3) . . ? C20 C19 C18 115.90(2) . . ? C21 C20 C19 123.09(3) . . ? C20 C21 C22 120.15(3) . . ? C23 C22 C21 116.30(2) . . ? C18 C23 C22 124.96(3) . . ? C18 C23 C24 107.65(3) . . ? C22 C23 C24 127.33(2) . . ? N6 C24 N5 131.12(2) . . ? N6 C24 C23 123.84(3) . . ? N5 C24 C23 104.79(2) . . ? N6 C25 N7 124.227(19) . . ? N6 C25 C26 128.46(3) . . ? N7 C25 C26 106.989(19) . . ? C31 C26 C27 122.59(3) . . ? C31 C26 C25 108.67(3) . . ? C27 C26 C25 128.73(2) . . ? O4 C27 C26 120.73(3) . . ? O4 C27 C28 124.13(3) . . ? C26 C27 C28 115.10(2) . . ? C29 C28 C27 120.16(3) . . ? C30 C29 C28 123.16(3) . . ? C29 C30 C31 116.54(3) . . ? C26 C31 C30 122.04(3) . . ? C26 C31 C32 107.11(3) . . ? C30 C31 C32 130.43(2) . . ? N8 C32 N7 127.406(19) . . ? N8 C32 C31 122.63(3) . . ? N7 C32 C31 109.87(2) . . ? O1 C33 C36 105.32(3) . . ? O1 C33 C34 106.89(3) . . ? C36 C33 C34 104.52(4) . . ? C35 C34 C33 105.88(4) . . ? C37 C36 C33 108.12(4) . . ? C41 C38 C39 98.71(5) . . ? C41 C38 O2 104.90(4) . . ? C39 C38 O2 97.41(4) . . ? C40 C39 C38 105.43(6) . . ? C42 C41 C38 106.56(5) . . ? C46 C43 O3 101.92(3) . . ? C46 C43 C44 123.43(3) . . ? O3 C43 C44 111.26(3) . . ? C45 C44 C43 109.98(3) . . ? C47 C46 C43 137.81(3) . . ? O4 C48 C51 110.44(3) . . ? O4 C48 C49 106.95(4) . . ? C51 C48 C49 107.91(4) . . ? C48 C49 C50 107.07(5) . . ? C48 C51 C52 107.76(5) . . ? N9 C53 N16 129.38(3) . . ? N9 C53 C54 108.58(2) . . ? N16 C53 C54 121.962(18) . . ? C59 C54 C55 122.33(3) . . ? C59 C54 C53 106.569(18) . . ? C55 C54 C53 130.84(3) . . ? C54 C55 C56 113.50(3) . . ? C57 C56 C55 124.83(3) . . ? C56 C57 C58 118.61(3) . . ? C57 C58 C59 120.89(3) . . ? C54 C59 C58 119.55(2) . . ? C54 C59 C60 107.56(2) . . ? C58 C59 C60 132.86(3) . . ? N10 C60 N9 128.49(2) . . ? N10 C60 C59 123.596(18) . . ? N9 C60 C59 107.88(3) . . ? N11 C61 N10 126.34(3) . . ? N11 C61 C62 110.35(2) . . ? N10 C61 C62 123.155(19) . . ? C67 C62 C63 120.13(3) . . ? C67 C62 C61 107.096(18) . . ? C63 C62 C61 132.77(3) . . ? C64 C63 C62 117.92(3) . . ? C63 C64 C65 123.00(3) . . ? C66 C65 C64 119.25(3) . . ? C65 C66 C67 116.22(3) . . ? C62 C67 C66 123.40(2) . . ? C62 C67 C68 106.59(2) . . ? C66 C67 C68 130.01(3) . . ? N12 C68 N11 127.94(2) . . ? N12 C68 C67 122.952(18) . . ? N11 C68 C67 109.07(3) . . ? N12 C69 N13 127.47(3) . . ? N12 C69 C70 122.714(17) . . ? N13 C69 C70 109.74(2) . . ? C75 C70 C71 119.62(2) . . ? C75 C70 C69 106.766(15) . . ? C71 C70 C69 133.60(2) . . ? C72 C71 C70 118.27(3) . . ? C71 C72 C73 121.05(2) . . ? C74 C73 C72 121.43(3) . . ? C73 C74 C75 117.42(3) . . ? C74 C75 C70 122.065(19) . . ? C74 C75 C76 132.18(3) . . ? C70 C75 C76 105.75(2) . . ? N14 C76 N13 127.49(2) . . ? N14 C76 C75 122.714(17) . . ? N13 C76 C75 109.57(3) . . ? N14 C77 N15 129.02(3) . . ? N14 C77 C78 122.084(17) . . ? N15 C77 C78 108.89(2) . . ? C79 C78 C83 120.56(2) . . ? C79 C78 C77 133.28(2) . . ? C83 C78 C77 106.156(15) . . ? C80 C79 C78 117.51(3) . . ? C79 C80 C81 122.10(2) . . ? C82 C81 C80 121.24(3) . . ? C81 C82 C83 117.09(3) . . ? C82 C83 C78 121.46(2) . . ? C82 C83 C84 131.40(3) . . ? C78 C83 C84 106.89(2) . . ? N16 C84 N15 128.96(2) . . ? N16 C84 C83 122.509(18) . . ? N15 C84 C83 108.47(3) . . ? Cl1' C85 Cl1 50.02(5) . . ? Cl1' C85 Cl3 56.13(5) . . ? Cl1 C85 Cl3 102.98(3) . . ? Cl1' C85 Cl2 124.52(4) . . ? Cl1 C85 Cl2 101.82(3) . . ? Cl3 C85 Cl2 102.01(3) . . ? Cl1' C85 Cl2' 114.47(5) . . ? Cl1 C85 Cl2' 136.30(3) . . ? Cl3 C85 Cl2' 63.15(3) . . ? Cl2 C85 Cl2' 48.76(2) . . ? C85 Cl1' Cl3 74.61(4) . . ? Cl3 Cl2' C85 51.27(2) . . ? Cl1' Cl3 C85 49.25(3) . . ? Cl1' Cl3 Cl2' 110.51(3) . . ? C85 Cl3 Cl2' 65.59(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 3.440 _refine_diff_density_min -3.499 _refine_diff_density_rms 0.155 data_Eu(Pc)[Pc(OC5H11)4] _database_code_CSD 202446 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety Eu(Pc)[Pc(OC5H11)4] _chemical_formula_sum 'C85 H73 Cl3 Eu N16 O4' _chemical_formula_weight 1640.90 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 21.0430(10) _cell_length_b 17.4463(8) _cell_length_c 21.0430(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.2620(10) _cell_angle_gamma 90.00 _cell_volume 7725.3(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.66 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.411 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3364 _exptl_absorpt_coefficient_mu 0.979 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.68577 _exptl_absorpt_correction_T_max 1.000 _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 'BRUKER SMART CCD DIFFRACTOMETER' _diffrn_measurement_method 'OMEGA SCAN' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 51900 _diffrn_reflns_av_R_equivalents 0.0847 _diffrn_reflns_av_sigmaI/netI 0.1245 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 28.06 _reflns_number_total 18666 _reflns_number_gt 8441 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART CCD DIFFRACTOMETER' _computing_cell_refinement 'BRUKER SMART CCD DIFFRACTOMETER' _computing_data_reduction 'BRUKER SMART CCD DIFFRACTOMETER' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SIEMENS SHELXTL' _computing_publication_material 'SIEMENS 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^)+(0.1158P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18666 _refine_ls_number_parameters 975 _refine_ls_number_restraints 52 _refine_ls_R_factor_all 0.1608 _refine_ls_R_factor_gt 0.0693 _refine_ls_wR_factor_ref 0.2264 _refine_ls_wR_factor_gt 0.1777 _refine_ls_goodness_of_fit_ref 0.947 _refine_ls_restrained_S_all 0.976 _refine_ls_shift/su_max 0.141 _refine_ls_shift/su_mean 0.007 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Eu1 Eu 0.616104(2) 0.194743(3) 0.973725(2) 0.04764(1) Uani 1 1 d . . . N1 N 0.55370(4) 0.26854(5) 0.89657(4) 0.0607(3) Uani 1 1 d . . . N2 N 0.68573(4) 0.27262(5) 0.90770(4) 0.0607(3) Uani 1 1 d . . . N2' N 0.77306(4) 0.29758(5) 0.97912(4) 0.0665(3) Uani 1 1 d . . . N3' N 0.60283(4) 0.30513(5) 1.12517(4) 0.0702(3) Uani 1 1 d . . . N3 N 0.67410(4) 0.28602(4) 1.04006(4) 0.0599(3) Uani 1 1 d . . . N4 N 0.54220(4) 0.28004(5) 1.02807(4) 0.0619(3) Uani 1 1 d . . . N4' N 0.45395(4) 0.28189(5) 0.95490(4) 0.0693(3) Uani 1 1 d . . . N5 N 0.63052(3) 0.10608(4) 0.88601(3) 0.0550(3) Uani 1 1 d . . . N5' N 0.62478(4) 0.27138(5) 0.80826(4) 0.0700(3) Uani 1 1 d . . . N6 N 0.71212(3) 0.12143(5) 0.99041(4) 0.0567(3) Uani 1 1 d . . . N7 N 0.60698(3) 0.12297(4) 1.07207(3) 0.0493(2) Uani 1 1 d . . . N8 N 0.52606(3) 0.10833(4) 0.96648(3) 0.0519(2) Uani 1 1 d . . . N9 N 0.74488(4) 0.09855(5) 0.88119(4) 0.0677(3) Uani 1 1 d . . . N10 N 0.71727(4) 0.11977(5) 1.10595(4) 0.0629(3) Uani 1 1 d . . . N11 N 0.49314(3) 0.10358(4) 1.07677(4) 0.0573(3) Uani 1 1 d . . . N12 N 0.52029(4) 0.09037(5) 0.85313(4) 0.0607(3) Uani 1 1 d . . . O1 O 0.34926(4) 0.29149(7) 0.85941(5) 0.1482(5) Uani 1 1 d . C . O2 O 0.71805(4) 0.28949(5) 0.70266(4) 0.1086(4) Uani 1 1 d . . . O3 O 0.87606(4) 0.33745(6) 1.07053(4) 0.1105(4) Uani 1 1 d . E . O4 O 0.50777(4) 0.33358(6) 1.22787(4) 0.1174(4) Uani 1 1 d . . . C1 C 0.48734(5) 0.27668(6) 0.90181(5) 0.0667(3) Uani 1 1 d . . . C2 C 0.46062(5) 0.28205(7) 0.83748(5) 0.0766(4) Uani 1 1 d . . . C3 C 0.39794(6) 0.28927(8) 0.81399(7) 0.1046(5) Uani 1 1 d . . . C4 C 0.38946(6) 0.29258(9) 0.74925(6) 0.1191(6) Uani 1 1 d . . . H4A H 0.3488 0.2993 0.7325 0.143 Uiso 1 1 calc R . . C5 C 0.43979(6) 0.28613(8) 0.70944(6) 0.1002(5) Uani 1 1 d . . . H5A H 0.4321 0.2860 0.6659 0.120 Uiso 1 1 calc R . . C6 C 0.50262(6) 0.27976(8) 0.73076(6) 0.1022(5) Uani 1 1 d . . . H6A H 0.5368 0.2778 0.7029 0.123 Uiso 1 1 calc R . . C7 C 0.51053(5) 0.27664(6) 0.79554(5) 0.0762(4) Uani 1 1 d . . . C8 C 0.56881(5) 0.27000(6) 0.83453(5) 0.0699(4) Uani 1 1 d . . . C9 C 0.67959(5) 0.27515(6) 0.84071(5) 0.0674(4) Uani 1 1 d . . . C10 C 0.74141(6) 0.28998(7) 0.81368(5) 0.0800(4) Uani 1 1 d . . . C11 C 0.76176(6) 0.30106(7) 0.75062(6) 0.0912(5) Uani 1 1 d . . . C12 C 0.82556(6) 0.32019(9) 0.74070(6) 0.1144(6) Uani 1 1 d . . . H12B H 0.8402 0.3294 0.6998 0.137 Uiso 1 1 calc R . . C13 C 0.86690(6) 0.32541(9) 0.79184(6) 0.1151(6) Uani 1 1 d . . . H13A H 0.9096 0.3354 0.7842 0.138 Uiso 1 1 calc R . . C14 C 0.84694(6) 0.31622(7) 0.85446(6) 0.0966(5) Uani 1 1 d . . . H14A H 0.8747 0.3212 0.8887 0.116 Uiso 1 1 calc R . . C15 C 0.78265(5) 0.29913(6) 0.86262(5) 0.0688(4) Uani 1 1 d . . . C16 C 0.74750(5) 0.28825(6) 0.92276(5) 0.0644(4) Uani 1 1 d . . . C17 C 0.74010(5) 0.30052(5) 1.03341(5) 0.0638(3) Uani 1 1 d . . . C18 C 0.76505(5) 0.32199(7) 1.09424(5) 0.0758(4) Uani 1 1 d . . . C19 C 0.82675(5) 0.34284(8) 1.11562(5) 0.0841(4) Uani 1 1 d . . . C20 C 0.83245(6) 0.36860(9) 1.17787(6) 0.1097(5) Uani 1 1 d . . . H20A H 0.8717 0.3865 1.1920 0.132 Uiso 1 1 calc R . . C21 C 0.78224(6) 0.36855(9) 1.21911(6) 0.1157(6) Uani 1 1 d . . . H21A H 0.7885 0.3833 1.2611 0.139 Uiso 1 1 calc R . . C22 C 0.72229(6) 0.34673(9) 1.19863(6) 0.0995(5) Uani 1 1 d . . . H22A H 0.6876 0.3475 1.2258 0.119 Uiso 1 1 calc R . . C23 C 0.71633(5) 0.32376(6) 1.13601(5) 0.0683(4) Uani 1 1 d . . . C24 C 0.65936(5) 0.30179(6) 1.09922(5) 0.0652(3) Uani 1 1 d . . . C25 C 0.54840(5) 0.29744(6) 1.09350(5) 0.0660(4) Uani 1 1 d . . . C26 C 0.48513(5) 0.31025(6) 1.11878(5) 0.0721(4) Uani 1 1 d . . . C27 C 0.46231(6) 0.32975(8) 1.17973(6) 0.0922(5) Uani 1 1 d . . . C28 C 0.39796(6) 0.34057(9) 1.18652(7) 0.1129(6) Uani 1 1 d . . . H28A H 0.3822 0.3528 1.2265 0.135 Uiso 1 1 calc R . . C29 C 0.35628(6) 0.33407(8) 1.13671(6) 0.1012(5) Uani 1 1 d . . . H29A H 0.3132 0.3429 1.1431 0.121 Uiso 1 1 calc R . . C30 C 0.37786(6) 0.31452(7) 1.07693(7) 0.0938(5) Uani 1 1 d . . . H30A H 0.3499 0.3081 1.0430 0.113 Uiso 1 1 calc R . . C31 C 0.44267(5) 0.30478(6) 1.06942(5) 0.0675(4) Uani 1 1 d . . . C32 C 0.48019(5) 0.28727(6) 1.01187(5) 0.0679(4) Uani 1 1 d . . . C33 C 0.58219(5) 0.09175(6) 0.84312(4) 0.0613(3) Uani 1 1 d . . . C34 C 0.61126(5) 0.07543(7) 0.78064(5) 0.0709(4) Uani 1 1 d . . . C35 C 0.58310(7) 0.05979(8) 0.72231(5) 0.1031(5) Uani 1 1 d . . . H35A H 0.5392 0.0584 0.7171 0.124 Uiso 1 1 calc R . . C36 C 0.62449(7) 0.04623(10) 0.67198(6) 0.1266(7) Uani 1 1 d . . . H36A H 0.6080 0.0378 0.6315 0.152 Uiso 1 1 calc R . . C37 C 0.68767(7) 0.04511(10) 0.68074(6) 0.1314(7) Uani 1 1 d . . . H37A H 0.7137 0.0322 0.6468 0.158 Uiso 1 1 calc R . . C38 C 0.71507(7) 0.06233(8) 0.73822(6) 0.1047(6) Uani 1 1 d . . . H38A H 0.7590 0.0632 0.7429 0.126 Uiso 1 1 calc R . . C39 C 0.67644(5) 0.07813(7) 0.78849(5) 0.0726(4) Uani 1 1 d . . . C40 C 0.68745(5) 0.09637(6) 0.85546(5) 0.0621(3) Uani 1 1 d . . . C41 C 0.75559(4) 0.10763(6) 0.94247(5) 0.0622(3) Uani 1 1 d . . . C42 C 0.81968(5) 0.09703(6) 0.97163(5) 0.0714(4) Uani 1 1 d . . . C43 C 0.87864(5) 0.08345(8) 0.94587(7) 0.1050(5) Uani 1 1 d . . . H43A H 0.8840 0.0791 0.9022 0.126 Uiso 1 1 calc R . . C44 C 0.92913(6) 0.07651(10) 0.98664(7) 0.1297(7) Uani 1 1 d . . . H44A H 0.9698 0.0700 0.9704 0.156 Uiso 1 1 calc R . . C45 C 0.92050(5) 0.07896(9) 1.05053(7) 0.1180(6) Uani 1 1 d . . . H45A H 0.9557 0.0710 1.0766 0.142 Uiso 1 1 calc R . . C46 C 0.86137(5) 0.09284(8) 1.07958(6) 0.0937(5) Uani 1 1 d . . . H46A H 0.8565 0.0948 1.1235 0.112 Uiso 1 1 calc R . . C47 C 0.81091(4) 0.10346(6) 1.03754(5) 0.0719(4) Uani 1 1 d . . . C48 C 0.74207(4) 0.11694(6) 1.04878(5) 0.0632(3) Uani 1 1 d . . . C49 C 0.65486(4) 0.12000(5) 1.11633(4) 0.0552(3) Uani 1 1 d . . . C50 C 0.62797(5) 0.10860(6) 1.17933(5) 0.0670(4) Uani 1 1 d . . . C51 C 0.65470(6) 0.09970(8) 1.23852(5) 0.0961(5) Uani 1 1 d . . . H51A H 0.6984 0.1032 1.2446 0.115 Uiso 1 1 calc R . . C52 C 0.61422(6) 0.08535(9) 1.28883(5) 0.1162(6) Uani 1 1 d . . . H52A H 0.6311 0.0805 1.3295 0.139 Uiso 1 1 calc R . . C53 C 0.55115(6) 0.07821(9) 1.28032(5) 0.1187(6) Uani 1 1 d . . . H53A H 0.5259 0.0672 1.3153 0.142 Uiso 1 1 calc R . . C54 C 0.52183(6) 0.08674(7) 1.22048(5) 0.0809(4) Uani 1 1 d . . . H54A H 0.4781 0.0823 1.2150 0.097 Uiso 1 1 calc R . . C55 C 0.56226(5) 0.10227(6) 1.17005(4) 0.0595(3) Uani 1 1 d . . . C56 C 0.55071(4) 0.11068(5) 1.10207(4) 0.0539(3) Uani 1 1 d . . . C57 C 0.48242(4) 0.10154(5) 1.01460(4) 0.0517(3) Uani 1 1 d . . . C58 C 0.41901(4) 0.08652(6) 0.98662(5) 0.0573(3) Uani 1 1 d . . . C59 C 0.36041(4) 0.07522(6) 1.01457(5) 0.0703(4) Uani 1 1 d . . . H59A H 0.3557 0.0745 1.0585 0.084 Uiso 1 1 calc R . . C60 C 0.30937(5) 0.06510(6) 0.97411(6) 0.0874(5) Uani 1 1 d . . . H60A H 0.2689 0.0595 0.9911 0.105 Uiso 1 1 calc R . . C61 C 0.31691(5) 0.06303(7) 0.90811(6) 0.0836(4) Uani 1 1 d . . . H61A H 0.2816 0.0550 0.8822 0.100 Uiso 1 1 calc R . . C62 C 0.37569(4) 0.07268(6) 0.88109(5) 0.0705(4) Uani 1 1 d . . . H62A H 0.3811 0.0712 0.8373 0.085 Uiso 1 1 calc R . . C63 C 0.42684(4) 0.08472(5) 0.92223(4) 0.0563(3) Uani 1 1 d . . . C64 C 0.49525(4) 0.09547(5) 0.91014(4) 0.0552(3) Uani 1 1 d . . . C65 C 0.29233(6) 0.33297(6) 0.85117(5) 0.1505(7) Uani 1 1 d D . . H65 H 0.2728 0.3403 0.8092 0.181 Uiso 1 1 calc R A 1 C66 C 0.72453(6) 0.32738(6) 0.64221(5) 0.1144(6) Uani 1 1 d D . . H66A H 0.7674 0.3185 0.6258 0.137 Uiso 1 1 calc R . . C67 C 0.95036(6) 0.37819(5) 1.05290(9) 0.3157(12) Uani 1 1 d D . . H67 H 0.9658 0.3741 1.0968 0.379 Uiso 1 1 calc R B 1 C68 C 0.49724(6) 0.37688(7) 1.28497(6) 0.1447(8) Uani 1 1 d D . . H68A H 0.4559 0.3619 1.3023 0.174 Uiso 1 1 calc R . . C69 C 0.25375(8) 0.31774(10) 0.90896(7) 0.496(4) Uani 1 1 d D C . H69A H 0.2231 0.3577 0.9184 0.596 Uiso 1 1 calc R . . H69B H 0.2789 0.3051 0.9462 0.596 Uiso 1 1 calc R . . C70 C 0.22556(9) 0.24942(9) 0.87636(9) 0.2969(17) Uani 1 1 d D . . H70A H 0.1959 0.2248 0.9043 0.445 Uiso 1 1 calc R C . H70B H 0.2588 0.2141 0.8655 0.445 Uiso 1 1 calc R . . H70C H 0.2039 0.2656 0.8384 0.445 Uiso 1 1 calc R . . C71 C 0.32203(14) 0.39838(7) 0.88767(9) 0.245(2) Uiso 0.50 1 d PD C 1 C72 C 0.3271(4) 0.47026(10) 0.84906(12) 0.400(5) Uiso 0.50 1 d PD C 1 C71' C 0.30711(18) 0.41478(7) 0.83389(9) 0.291(3) Uiso 0.50 1 d PD D 2 C72' C 0.2919(2) 0.46917(13) 0.88654(9) 0.287(3) Uiso 0.50 1 d PD D 2 C73 C 0.67735(6) 0.28345(7) 0.60262(6) 0.1775(10) Uani 1 1 d D . . H73A H 0.6388 0.2816 0.6277 0.213 Uiso 1 1 calc R . . H73B H 0.6679 0.3161 0.5665 0.213 Uiso 1 1 calc R . . C74 C 0.68514(16) 0.20460(8) 0.57589(14) 0.441(3) Uani 1 1 d D . . H74A H 0.6482 0.1914 0.5513 0.661 Uiso 1 1 calc R . . H74B H 0.6902 0.1686 0.6100 0.661 Uiso 1 1 calc R . . H74C H 0.7220 0.2032 0.5492 0.661 Uiso 1 1 calc R . . C75 C 0.71484(6) 0.41204(6) 0.65216(7) 0.1534(8) Uani 1 1 d D . . H75A H 0.7203 0.4379 0.6118 0.184 Uiso 1 1 calc R . . H75B H 0.7476 0.4307 0.6808 0.184 Uiso 1 1 calc R . . C76 C 0.65033(6) 0.43386(12) 0.67908(10) 0.2599(14) Uani 1 1 d D . . H76A H 0.6484 0.4884 0.6848 0.390 Uiso 1 1 calc R . . H76B H 0.6444 0.4088 0.7193 0.390 Uiso 1 1 calc R . . H76C H 0.6175 0.4181 0.6501 0.390 Uiso 1 1 calc R . . C77 C 0.99180(9) 0.31483(6) 1.02951(9) 0.256(3) Uiso 0.50 1 d PD E 1 C78 C 0.96154(12) 0.23751(7) 1.0211(3) 0.538(7) Uiso 0.50 1 d PD E 1 C77' C 0.99138(9) 0.31480(6) 1.02951(9) 0.203(2) Uiso 0.50 1 d PD F 2 C78' C 1.0074(2) 0.25013(8) 1.07371(8) 0.551(7) Uiso 0.50 1 d PD F 2 C79 C 0.91613(7) 0.45221(8) 1.06482(6) 0.3459(16) Uani 1 1 d D E . H79A H 0.9467 0.4918 1.0755 0.415 Uiso 1 1 calc R . . H79B H 0.8877 0.4460 1.1007 0.415 Uiso 1 1 calc R . . C80 C 0.87818(9) 0.47678(14) 1.00692(6) 0.2720(15) Uani 1 1 d D . . H80A H 0.8719 0.5313 1.0080 0.408 Uiso 1 1 calc R E . H80B H 0.8377 0.4515 1.0070 0.408 Uiso 1 1 calc R . . H80C H 0.9009 0.4632 0.9691 0.408 Uiso 1 1 calc R . . C81 C 0.54701(7) 0.35555(8) 1.33188(7) 0.2626(13) Uani 1 1 d D . . H81A H 0.5451 0.3878 1.3694 0.315 Uiso 1 1 calc R . . H81B H 0.5891 0.3590 1.3136 0.315 Uiso 1 1 calc R . . C82 C 0.53005(13) 0.27458(8) 1.34711(12) 0.321(2) Uani 1 1 d D . . H82A H 0.5604 0.2541 1.3767 0.482 Uiso 1 1 calc R . . H82B H 0.5304 0.2446 1.3089 0.482 Uiso 1 1 calc R . . H82C H 0.4884 0.2730 1.3655 0.482 Uiso 1 1 calc R . . C83 C 0.49674(6) 0.46208(7) 1.27491(10) 0.2551(13) Uani 1 1 d D . . H83A H 0.4643 0.4769 1.2445 0.306 Uiso 1 1 calc R . . H83B H 0.4897 0.4892 1.3145 0.306 Uiso 1 1 calc R . . C84 C 0.56134(6) 0.47722(16) 1.24989(12) 0.326(2) Uani 1 1 d D . . H84A H 0.5658 0.5309 1.2411 0.489 Uiso 1 1 calc R . . H84B H 0.5675 0.4485 1.2115 0.489 Uiso 1 1 calc R . . H84C H 0.5925 0.4621 1.2809 0.489 Uiso 1 1 calc R . . C85 C 0.61467(5) 0.43823(13) 0.94079(6) 0.2518(12) Uani 1 1 d D . . H85A H 0.6156 0.3823 0.9450 0.302 Uiso 0.50 1 calc PR G 1 Cl1 Cl 0.68491(6) 0.46952(12) 0.91522(7) 0.3082(9) Uiso 0.50 1 d PD H 1 Cl2 Cl 0.58792(6) 0.48117(8) 1.01512(5) 0.2094(5) Uiso 0.50 1 d PD H 1 Cl3 Cl 0.55184(5) 0.46566(7) 0.88853(5) 0.1818(4) Uiso 0.50 1 d PD H 1 Cl1' Cl 0.69283(4) 0.47712(7) 0.96482(5) 0.1753(4) Uiso 0.50 1 d PD H 2 Cl2' Cl 0.55286(6) 0.48442(13) 0.96887(8) 0.3695(12) Uiso 0.50 1 d PD H 2 Cl3' Cl 0.62471(7) 0.45593(10) 0.85517(6) 0.2723(8) Uiso 0.50 1 d PD H 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu1 0.04153(2) 0.05553(2) 0.04581(2) 0.00270(2) -0.00553(2) -0.00242(2) N1 0.0662(5) 0.0643(5) 0.0514(4) 0.0055(4) -0.0110(4) 0.0013(4) N2 0.0579(5) 0.0620(5) 0.0622(5) 0.0084(4) -0.0061(4) -0.0058(4) N2' 0.0572(5) 0.0745(5) 0.0677(5) 0.0007(4) -0.0028(4) -0.0104(4) N3' 0.0711(5) 0.0697(5) 0.0698(5) -0.0065(5) -0.0129(4) -0.0040(4) N3 0.0594(5) 0.0654(5) 0.0547(5) -0.0021(4) -0.0099(4) -0.0048(4) N4 0.0531(5) 0.0618(5) 0.0708(5) 0.0033(4) -0.0016(4) 0.0015(4) N4' 0.0539(5) 0.0741(5) 0.0797(6) 0.0054(5) -0.0074(4) 0.0076(4) N5 0.0555(4) 0.0639(5) 0.0456(4) 0.0000(4) -0.0033(3) -0.0051(4) N5' 0.0716(5) 0.0799(5) 0.0583(5) 0.0109(5) -0.0124(4) -0.0098(5) N6 0.0399(4) 0.0672(5) 0.0630(5) 0.0036(4) -0.0036(4) 0.0034(4) N7 0.0441(4) 0.0565(4) 0.0471(4) 0.0010(4) -0.0028(3) -0.0022(3) N8 0.0481(4) 0.0608(4) 0.0468(4) -0.0015(4) -0.0072(3) -0.0069(4) N9 0.0590(5) 0.0785(6) 0.0657(5) -0.0017(5) 0.0114(4) 0.0024(4) N10 0.0572(4) 0.0810(5) 0.0505(4) 0.0134(4) -0.0190(3) -0.0073(4) N11 0.0505(4) 0.0583(5) 0.0630(5) 0.0023(4) 0.0010(4) -0.0001(4) N12 0.0611(5) 0.0686(5) 0.0525(4) 0.0031(4) -0.0065(4) -0.0096(4) O1 0.0762(6) 0.2416(12) 0.1265(8) 0.0374(7) -0.0204(5) 0.0379(6) O2 0.1099(6) 0.1490(8) 0.0670(5) 0.0066(5) 0.0015(5) -0.0363(5) O3 0.0746(5) 0.1633(8) 0.0936(6) -0.0131(6) -0.0066(4) -0.0334(5) O4 0.0845(6) 0.1837(9) 0.0841(6) -0.0373(6) 0.0037(5) 0.0179(6) C1 0.0655(6) 0.0584(5) 0.0760(6) 0.0105(5) -0.0292(5) -0.0027(5) C2 0.0675(6) 0.0917(8) 0.0705(7) 0.0144(6) -0.0179(5) -0.0053(6) C3 0.0816(8) 0.1330(11) 0.0989(9) 0.0192(8) -0.0276(7) 0.0019(8) C4 0.0908(8) 0.1772(15) 0.0889(8) 0.0085(9) -0.0483(6) 0.0046(9) C5 0.0863(8) 0.1409(11) 0.0731(7) 0.0068(8) -0.0319(6) -0.0082(8) C6 0.1145(10) 0.1148(10) 0.0770(8) 0.0167(7) -0.0245(7) -0.0156(8) C7 0.0857(7) 0.0758(7) 0.0668(6) 0.0111(5) -0.0344(5) -0.0082(6) C8 0.0709(6) 0.0661(6) 0.0724(7) 0.0138(6) -0.0127(5) -0.0028(6) C9 0.0642(6) 0.0671(6) 0.0711(6) 0.0137(5) 0.0172(5) -0.0039(5) C10 0.0852(8) 0.0876(8) 0.0671(7) 0.0055(6) -0.0059(6) 0.0013(6) C11 0.0928(8) 0.1177(10) 0.0631(7) 0.0012(7) -0.0005(6) -0.0285(7) C12 0.0843(9) 0.1793(14) 0.0797(8) -0.0113(9) 0.0162(7) -0.0299(9) C13 0.0638(7) 0.1904(15) 0.0911(9) 0.0033(10) 0.0212(7) -0.0271(8) C14 0.0802(8) 0.1240(10) 0.0854(8) -0.0044(8) 0.0003(7) -0.0203(7) C15 0.0567(6) 0.0817(7) 0.0680(6) 0.0037(6) 0.0078(5) -0.0121(5) C16 0.0576(6) 0.0597(6) 0.0759(7) 0.0021(5) -0.0012(5) -0.0066(5) C17 0.0640(6) 0.0596(6) 0.0676(6) -0.0010(5) -0.0225(5) -0.0027(5) C18 0.0714(7) 0.0861(8) 0.0697(7) 0.0008(6) -0.0151(5) -0.0109(6) C19 0.0712(7) 0.1134(9) 0.0677(7) 0.0065(7) -0.0120(6) -0.0086(7) C20 0.0779(7) 0.1654(13) 0.0856(8) -0.0139(9) -0.0324(6) -0.0225(8) C21 0.0810(8) 0.1965(14) 0.0693(7) -0.0259(9) -0.0212(6) -0.0286(9) C22 0.0880(8) 0.1405(11) 0.0698(8) -0.0019(8) -0.0095(6) -0.0084(9) C23 0.0756(7) 0.0730(7) 0.0560(6) -0.0048(5) -0.0155(5) -0.0023(5) C24 0.0595(6) 0.0669(6) 0.0692(6) 0.0026(6) -0.0038(5) -0.0032(5) C25 0.0644(6) 0.0578(6) 0.0761(7) 0.0019(5) 0.0148(5) 0.0056(5) C26 0.0633(6) 0.0767(7) 0.0765(7) -0.0138(6) 0.0091(5) -0.0014(6) C27 0.0728(8) 0.1151(9) 0.0889(8) -0.0079(8) 0.0031(7) 0.0023(7) C28 0.0847(9) 0.1408(11) 0.1132(11) -0.0108(10) 0.0166(8) 0.0206(9) C29 0.0601(7) 0.1410(11) 0.1026(9) -0.0059(9) 0.0171(7) 0.0094(8) C30 0.0642(7) 0.1187(10) 0.0983(9) 0.0127(8) -0.0040(6) 0.0073(7) C31 0.0524(5) 0.0695(6) 0.0807(7) 0.0071(6) 0.0020(5) 0.0026(5) C32 0.0526(6) 0.0649(6) 0.0862(7) 0.0115(6) 0.0032(5) 0.0009(5) C33 0.0705(6) 0.0703(6) 0.0432(5) -0.0005(5) -0.0066(4) -0.0077(5) C34 0.0809(7) 0.0829(7) 0.0490(6) 0.0006(6) 0.0043(5) -0.0074(6) C35 0.1248(10) 0.1332(11) 0.0513(7) -0.0024(7) -0.0008(7) -0.0237(9) C36 0.1436(12) 0.1785(14) 0.0576(8) -0.0204(9) 0.0078(8) -0.0222(11) C37 0.1368(12) 0.1925(16) 0.0652(8) -0.0248(10) 0.0267(8) -0.0062(12) C38 0.1081(10) 0.1419(12) 0.0643(7) -0.0083(8) 0.0120(7) -0.0024(9) C39 0.0753(7) 0.0835(7) 0.0591(6) -0.0054(6) 0.0124(5) 0.0003(6) C40 0.0602(6) 0.0679(6) 0.0582(6) -0.0050(5) 0.0046(5) 0.0011(5) C41 0.0399(5) 0.0629(6) 0.0837(7) 0.0020(5) 0.0050(5) 0.0086(5) C42 0.0547(6) 0.0757(7) 0.0838(7) -0.0046(6) -0.0089(5) 0.0066(5) C43 0.0522(6) 0.1339(10) 0.1290(11) -0.0084(9) -0.0001(7) 0.0314(7) C44 0.0533(7) 0.2049(15) 0.1308(12) -0.0279(12) 0.0025(7) 0.0349(9) C45 0.0400(6) 0.1663(13) 0.1476(12) 0.0067(11) -0.0196(7) 0.0113(8) C46 0.0579(6) 0.1214(10) 0.1016(9) 0.0094(8) -0.0216(6) -0.0010(7) C47 0.0477(5) 0.0733(7) 0.0945(8) 0.0059(6) -0.0173(5) 0.0022(5) C48 0.0567(5) 0.0601(6) 0.0727(6) 0.0092(5) -0.0172(5) -0.0048(5) C49 0.0536(5) 0.0627(5) 0.0493(5) 0.0099(5) -0.0145(4) -0.0044(5) C50 0.0689(6) 0.0787(7) 0.0533(6) -0.0031(5) -0.0149(5) -0.0080(5) C51 0.1039(8) 0.1270(10) 0.0570(6) 0.0033(7) -0.0271(6) -0.0296(8) C52 0.1235(9) 0.1816(13) 0.0433(6) 0.0138(8) -0.0186(6) -0.0531(9) C53 0.1327(10) 0.1772(13) 0.0463(6) 0.0044(8) 0.0131(7) -0.0577(9) C54 0.0870(8) 0.0977(8) 0.0582(6) 0.0038(6) 0.0047(6) -0.0146(7) C55 0.0711(6) 0.0625(6) 0.0447(5) 0.0003(5) -0.0060(4) -0.0088(5) C56 0.0565(5) 0.0522(5) 0.0530(5) -0.0008(4) -0.0069(4) 0.0022(4) C57 0.0470(5) 0.0553(5) 0.0526(5) -0.0003(4) -0.0099(4) -0.0044(4) C58 0.0407(5) 0.0589(5) 0.0721(6) 0.0033(5) -0.0026(4) 0.0005(4) C59 0.0486(5) 0.0729(7) 0.0892(7) 0.0049(6) -0.0067(5) -0.0046(5) C60 0.0373(5) 0.0810(8) 0.1438(11) 0.0025(8) -0.0128(6) -0.0046(5) C61 0.0615(6) 0.0946(8) 0.0946(8) 0.0014(7) -0.0307(5) -0.0051(6) C62 0.0585(6) 0.0698(6) 0.0831(7) 0.0037(6) -0.0207(5) -0.0019(5) C63 0.0512(5) 0.0515(5) 0.0661(6) -0.0024(5) -0.0167(4) -0.0054(4) C64 0.0520(5) 0.0544(5) 0.0591(5) 0.0049(5) -0.0118(4) -0.0074(4) C65 0.1040(10) 0.1554(13) 0.1916(15) -0.0335(12) -0.0607(9) 0.0394(10) C66 0.1228(10) 0.1567(12) 0.0636(7) 0.0148(8) -0.0217(7) -0.0341(9) C67 0.2922(16) 0.1285(14) 0.524(3) 0.0726(17) -0.2772(14) -0.0991(12) C68 0.1007(11) 0.2334(18) 0.1001(10) -0.0454(12) 0.0037(9) 0.0225(12) C69 0.1102(17) 1.114(10) 0.266(3) -0.217(4) -0.0016(19) 0.149(3) C70 0.209(2) 0.467(4) 0.214(3) 0.033(3) -0.0276(19) 0.154(2) C73 0.1268(12) 0.293(2) 0.1125(11) 0.0520(13) -0.0491(9) -0.0150(14) C74 0.325(4) 0.225(3) 0.773(8) -0.097(4) 0.046(5) 0.112(2) C75 0.1969(16) 0.1090(11) 0.1541(15) 0.0265(11) -0.0284(13) -0.0320(12) C76 0.1811(18) 0.219(2) 0.380(3) 0.124(2) 0.0959(19) 0.0675(16) C79 0.1831(15) 0.699(4) 0.1561(14) -0.185(2) 0.1004(11) -0.2124(19) C80 0.427(3) 0.287(3) 0.1014(14) 0.0425(16) -0.0222(18) -0.167(2) C81 0.182(2) 0.411(3) 0.1949(17) -0.1665(17) 0.0038(15) -0.042(2) C82 0.394(4) 0.350(4) 0.219(3) 0.020(3) -0.054(3) 0.047(4) C83 0.298(3) 0.2123(19) 0.255(2) -0.1099(17) -0.076(2) 0.1092(18) C84 0.234(2) 0.234(3) 0.511(5) -0.044(3) 0.129(3) -0.071(2) C85 0.1536(14) 0.190(2) 0.414(3) 0.027(2) 0.1685(13) 0.0042(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu1 N6 2.4156(7) . ? Eu1 N8 2.4257(7) . ? Eu1 N7 2.4272(7) . ? Eu1 N5 2.4283(7) . ? Eu1 N2 2.4375(8) . ? Eu1 N4 2.4407(8) . ? Eu1 N3 2.4409(8) . ? Eu1 N1 2.4492(8) . ? N1 C8 1.3455(13) . ? N1 C1 1.4083(13) . ? N2 C16 1.3639(13) . ? N2 C9 1.4158(13) . ? N2' C16 1.3102(14) . ? N2' C17 1.3401(13) . ? N3' C24 1.3124(13) . ? N3' C25 1.3294(14) . ? N3 C24 1.3134(13) . ? N3 C17 1.4194(13) . ? N4 C32 1.3530(13) . ? N4 C25 1.4154(14) . ? N4' C32 1.3210(14) . ? N4' C1 1.3257(13) . ? N5 C40 1.3726(12) . ? N5 C33 1.3796(12) . ? N5' C8 1.3035(13) . ? N5' C9 1.3392(13) . ? N6 C48 1.3802(12) . ? N6 C41 1.3859(12) . ? N7 C56 1.3613(11) . ? N7 C49 1.3700(11) . ? N8 C64 1.3672(11) . ? N8 C57 1.3751(11) . ? N9 C41 1.3175(13) . ? N9 C40 1.3227(13) . ? N10 C48 1.3146(12) . ? N10 C49 1.3322(12) . ? N11 C56 1.3268(12) . ? N11 C57 1.3271(12) . ? N12 C64 1.3154(12) . ? N12 C33 1.3207(12) . ? O1 C3 1.4048(17) . ? O1 C65 1.4096(15) . ? O2 C11 1.3772(15) . ? O2 C66 1.4406(14) . ? O3 C19 1.4124(14) . ? O3 C67 1.7585(15) . ? O4 C27 1.3918(15) . ? O4 C68 1.4374(15) . ? C1 C2 1.4665(15) . ? C2 C7 1.3780(15) . ? C2 C3 1.4120(17) . ? C3 C4 1.3743(19) . ? C4 C5 1.3582(18) . ? C5 C6 1.3985(18) . ? C6 C7 1.3737(16) . ? C7 C8 1.4770(15) . ? C9 C10 1.4455(16) . ? C10 C15 1.3532(16) . ? C10 C11 1.4095(17) . ? C11 C12 1.4000(18) . ? C12 C13 1.3836(19) . ? C13 C14 1.3940(19) . ? C14 C15 1.3968(16) . ? C15 C16 1.4808(15) . ? C17 C18 1.4312(15) . ? C18 C23 1.3538(15) . ? C18 C19 1.4196(16) . ? C19 C20 1.3895(17) . ? C20 C21 1.3704(17) . ? C21 C22 1.3845(17) . ? C22 C23 1.3824(16) . ? C23 C24 1.4747(15) . ? C25 C26 1.4532(15) . ? C26 C31 1.3705(15) . ? C26 C27 1.4131(17) . ? C27 C28 1.3753(18) . ? C28 C29 1.3683(19) . ? C29 C30 1.3822(19) . ? C30 C31 1.3841(16) . ? C31 C32 1.4805(16) . ? C33 C34 1.4803(14) . ? C34 C39 1.3815(15) . ? C34 C35 1.3876(15) . ? C35 C36 1.3945(19) . ? C36 C37 1.341(2) . ? C37 C38 1.3710(18) . ? C38 C39 1.3651(16) . ? C39 C40 1.4622(14) . ? C41 C42 1.4907(14) . ? C42 C43 1.3767(15) . ? C42 C47 1.4044(16) . ? C43 C44 1.3679(18) . ? C44 C45 1.358(2) . ? C45 C46 1.4099(16) . ? C46 C47 1.3913(15) . ? C47 C48 1.4876(13) . ? C49 C50 1.4574(13) . ? C50 C51 1.3731(15) . ? C50 C55 1.4000(14) . ? C51 C52 1.3846(17) . ? C52 C53 1.3442(19) . ? C53 C54 1.4077(16) . ? C54 C55 1.3897(15) . ? C55 C56 1.4573(13) . ? C57 C58 1.4794(12) . ? C58 C63 1.3662(14) . ? C58 C59 1.3827(13) . ? C59 C60 1.3789(15) . ? C60 C61 1.3990(17) . ? C61 C62 1.3740(14) . ? C62 C63 1.3942(13) . ? C63 C64 1.4750(12) . ? C65 C69 1.4891(19) . ? C65 C71 1.509(2) . ? C66 C73 1.5032(17) . ? C66 C75 1.5057(15) . ? C67 C77 1.4929(19) . ? C67 C79 1.5003(18) . ? C68 C81 1.4832(19) . ? C68 C83 1.5015(17) . ? C69 C70 1.496(2) . ? C71 C72 1.498(3) . ? C71' C72' 1.495(3) . ? C73 C74 1.495(2) . ? C75 C76 1.5217(19) . ? C77 C78 1.502(2) . ? C77' C78' 1.500(2) . ? C79 C80 1.516(2) . ? C81 C82 1.492(2) . ? C83 C84 1.484(2) . ? C85 Cl2' 1.642(2) . ? C85 Cl1 1.6672(19) . ? C85 Cl3 1.7814(16) . ? C85 Cl2 1.8255(18) . ? C85 Cl3' 1.8412(17) . ? C85 Cl1' 1.8477(16) . ? 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 N6 Eu1 N8 109.43(3) . . ? N6 Eu1 N7 70.87(2) . . ? N8 Eu1 N7 70.61(2) . . ? N6 Eu1 N5 70.48(3) . . ? N8 Eu1 N5 69.92(2) . . ? N7 Eu1 N5 109.28(2) . . ? N6 Eu1 N2 82.73(3) . . ? N8 Eu1 N2 141.45(2) . . ? N7 Eu1 N2 145.45(2) . . ? N5 Eu1 N2 81.04(3) . . ? N6 Eu1 N4 142.10(3) . . ? N8 Eu1 N4 84.79(3) . . ? N7 Eu1 N4 82.07(3) . . ? N5 Eu1 N4 145.75(3) . . ? N2 Eu1 N4 108.25(3) . . ? N6 Eu1 N3 81.18(3) . . ? N8 Eu1 N3 146.07(3) . . ? N7 Eu1 N3 83.70(3) . . ? N5 Eu1 N3 141.85(3) . . ? N2 Eu1 N3 70.25(3) . . ? N4 Eu1 N3 69.65(3) . . ? N6 Eu1 N1 145.11(3) . . ? N8 Eu1 N1 82.46(3) . . ? N7 Eu1 N1 142.38(2) . . ? N5 Eu1 N1 84.23(3) . . ? N2 Eu1 N1 69.58(3) . . ? N4 Eu1 N1 69.46(3) . . ? N3 Eu1 N1 107.54(3) . . ? C8 N1 C1 108.23(8) . . ? C8 N1 Eu1 121.65(6) . . ? C1 N1 Eu1 122.01(6) . . ? C16 N2 C9 107.91(8) . . ? C16 N2 Eu1 123.62(6) . . ? C9 N2 Eu1 122.18(6) . . ? C16 N2' C17 124.37(9) . . ? C24 N3' C25 124.57(9) . . ? C24 N3 C17 106.95(8) . . ? C24 N3 Eu1 124.00(6) . . ? C17 N3 Eu1 123.15(6) . . ? C32 N4 C25 108.03(8) . . ? C32 N4 Eu1 123.69(7) . . ? C25 N4 Eu1 122.04(6) . . ? C32 N4' C1 123.28(9) . . ? C40 N5 C33 108.27(7) . . ? C40 N5 Eu1 123.16(6) . . ? C33 N5 Eu1 121.23(6) . . ? C8 N5' C9 124.22(9) . . ? C48 N6 C41 109.74(7) . . ? C48 N6 Eu1 122.52(6) . . ? C41 N6 Eu1 122.72(6) . . ? C56 N7 C49 108.51(7) . . ? C56 N7 Eu1 123.30(6) . . ? C49 N7 Eu1 122.56(6) . . ? C64 N8 C57 107.99(7) . . ? C64 N8 Eu1 121.57(6) . . ? C57 N8 Eu1 122.09(6) . . ? C41 N9 C40 123.78(8) . . ? C48 N10 C49 123.09(8) . . ? C56 N11 C57 123.29(8) . . ? C64 N12 C33 122.94(8) . . ? C3 O1 C65 123.54(11) . . ? C11 O2 C66 120.94(10) . . ? C19 O3 C67 140.48(10) . . ? C27 O4 C68 121.71(10) . . ? N4' C1 N1 127.05(9) . . ? N4' C1 C2 124.82(9) . . ? N1 C1 C2 108.08(8) . . ? C7 C2 C3 119.69(11) . . ? C7 C2 C1 107.26(9) . . ? C3 C2 C1 133.03(11) . . ? C4 C3 O1 125.54(12) . . ? C4 C3 C2 117.88(12) . . ? O1 C3 C2 116.57(11) . . ? C5 C4 C3 120.65(12) . . ? C4 C5 C6 123.19(12) . . ? C7 C6 C5 115.57(11) . . ? C6 C7 C2 122.93(11) . . ? C6 C7 C8 130.60(11) . . ? C2 C7 C8 106.44(9) . . ? N5' C8 N1 129.04(10) . . ? N5' C8 C7 120.84(10) . . ? N1 C8 C7 109.94(9) . . ? N5' C9 N2 125.50(9) . . ? N5' C9 C10 125.64(10) . . ? N2 C9 C10 108.61(9) . . ? C15 C10 C11 120.25(11) . . ? C15 C10 C9 107.26(10) . . ? C11 C10 C9 132.29(11) . . ? O2 C11 C12 124.29(11) . . ? O2 C11 C10 117.71(11) . . ? C12 C11 C10 117.96(11) . . ? C13 C12 C11 119.97(12) . . ? C12 C13 C14 122.45(12) . . ? C13 C14 C15 115.91(11) . . ? C10 C15 C14 123.34(11) . . ? C10 C15 C16 108.32(9) . . ? C14 C15 C16 128.34(10) . . ? N2' C16 N2 128.46(10) . . ? N2' C16 C15 123.58(9) . . ? N2 C16 C15 107.83(9) . . ? N2' C17 N3 126.00(9) . . ? N2' C17 C18 125.69(9) . . ? N3 C17 C18 108.27(9) . . ? C23 C18 C19 118.86(10) . . ? C23 C18 C17 108.12(9) . . ? C19 C18 C17 132.97(10) . . ? C20 C19 O3 126.46(10) . . ? C20 C19 C18 117.16(10) . . ? O3 C19 C18 116.35(10) . . ? C21 C20 C19 122.23(12) . . ? C20 C21 C22 120.48(12) . . ? C23 C22 C21 117.06(11) . . ? C18 C23 C22 124.04(10) . . ? C18 C23 C24 105.63(9) . . ? C22 C23 C24 130.22(10) . . ? N3' C24 N3 128.46(10) . . ? N3' C24 C23 120.41(9) . . ? N3 C24 C23 110.93(9) . . ? N3' C25 N4 125.79(9) . . ? N3' C25 C26 126.13(10) . . ? N4 C25 C26 107.97(9) . . ? C31 C26 C27 118.78(10) . . ? C31 C26 C25 107.89(10) . . ? C27 C26 C25 133.24(10) . . ? C28 C27 O4 126.27(12) . . ? C28 C27 C26 117.79(12) . . ? O4 C27 C26 115.90(10) . . ? C29 C28 C27 122.48(13) . . ? C28 C29 C30 120.37(12) . . ? C29 C30 C31 117.53(11) . . ? C26 C31 C30 122.98(11) . . ? C26 C31 C32 106.62(9) . . ? C30 C31 C32 130.40(11) . . ? N4' C32 N4 128.36(10) . . ? N4' C32 C31 122.32(9) . . ? N4 C32 C31 109.30(9) . . ? N12 C33 N5 128.58(8) . . ? N12 C33 C34 123.37(9) . . ? N5 C33 C34 108.03(8) . . ? C39 C34 C35 122.15(10) . . ? C39 C34 C33 107.54(9) . . ? C35 C34 C33 130.32(10) . . ? C34 C35 C36 116.07(12) . . ? C37 C36 C35 121.35(12) . . ? C36 C37 C38 122.04(13) . . ? C39 C38 C37 118.58(13) . . ? C38 C39 C34 119.67(10) . . ? C38 C39 C40 134.30(10) . . ? C34 C39 C40 105.99(9) . . ? N9 C40 N5 127.04(9) . . ? N9 C40 C39 122.78(9) . . ? N5 C40 C39 110.10(8) . . ? N9 C41 N6 128.52(8) . . ? N9 C41 C42 122.57(9) . . ? N6 C41 C42 108.71(9) . . ? C43 C42 C47 121.69(10) . . ? C43 C42 C41 132.42(11) . . ? C47 C42 C41 105.90(8) . . ? C44 C43 C42 117.84(13) . . ? C45 C44 C43 120.75(12) . . ? C44 C45 C46 123.83(12) . . ? C47 C46 C45 114.81(11) . . ? C46 C47 C42 120.93(9) . . ? C46 C47 C48 131.36(10) . . ? C42 C47 C48 107.58(9) . . ? N10 C48 N6 129.11(8) . . ? N10 C48 C47 122.85(9) . . ? N6 C48 C47 107.97(8) . . ? N10 C49 N7 127.68(8) . . ? N10 C49 C50 122.40(8) . . ? N7 C49 C50 109.64(8) . . ? C51 C50 C55 121.18(10) . . ? C51 C50 C49 132.95(10) . . ? C55 C50 C49 105.74(8) . . ? C50 C51 C52 117.58(11) . . ? C53 C52 C51 121.70(11) . . ? C52 C53 C54 122.53(11) . . ? C55 C54 C53 115.87(11) . . ? C54 C55 C50 121.11(9) . . ? C54 C55 C56 132.01(9) . . ? C50 C55 C56 106.80(8) . . ? N11 C56 N7 128.54(8) . . ? N11 C56 C55 122.17(8) . . ? N7 C56 C55 109.25(8) . . ? N11 C57 N8 127.77(8) . . ? N11 C57 C58 123.09(8) . . ? N8 C57 C58 109.05(8) . . ? C63 C58 C59 122.04(9) . . ? C63 C58 C57 106.62(8) . . ? C59 C58 C57 131.34(9) . . ? C60 C59 C58 116.70(10) . . ? C59 C60 C61 121.65(10) . . ? C62 C61 C60 120.93(10) . . ? C61 C62 C63 117.10(10) . . ? C58 C63 C62 121.53(9) . . ? C58 C63 C64 106.89(8) . . ? C62 C63 C64 131.57(9) . . ? N12 C64 N8 127.71(8) . . ? N12 C64 C63 122.96(8) . . ? N8 C64 C63 109.30(8) . . ? O1 C65 C69 105.91(10) . . ? O1 C65 C71 88.62(13) . . ? C69 C65 C71 86.87(12) . . ? O2 C66 C73 100.98(9) . . ? O2 C66 C75 108.29(10) . . ? C73 C66 C75 119.19(10) . . ? C77 C67 C79 166.92(15) . . ? C77 C67 O3 106.95(9) . . ? C79 C67 O3 83.38(9) . . ? O4 C68 C81 108.27(10) . . ? O4 C68 C83 113.79(12) . . ? C81 C68 C83 110.28(11) . . ? C65 C69 C70 89.09(12) . . ? C72 C71 C65 112.8(2) . . ? C74 C73 C66 127.17(16) . . ? C66 C75 C76 114.76(12) . . ? C67 C77 C78 117.14(18) . . ? C67 C79 C80 111.14(14) . . ? C68 C81 C82 102.21(14) . . ? C84 C83 C68 102.74(14) . . ? Cl2' C85 Cl1 131.32(18) . . ? Cl2' C85 Cl3 60.23(8) . . ? Cl1 C85 Cl3 111.68(11) . . ? Cl2' C85 Cl2 40.76(8) . . ? Cl1 C85 Cl2 114.80(12) . . ? Cl3 C85 Cl2 100.82(9) . . ? Cl2' C85 Cl3' 111.37(12) . . ? Cl1 C85 Cl3' 61.53(8) . . ? Cl3 C85 Cl3' 55.87(7) . . ? Cl2 C85 Cl3' 143.79(15) . . ? Cl2' C85 Cl1' 115.27(13) . . ? Cl1 C85 Cl1' 34.78(7) . . ? Cl3 C85 Cl1' 136.68(14) . . ? Cl2 C85 Cl1' 83.82(8) . . ? Cl3' C85 Cl1' 95.75(9) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.06 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.405 _refine_diff_density_min -0.706 _refine_diff_density_rms 0.121