# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Jing Xi Liu' _publ_contact_author_email jxliu411@ahut.edu.cn _publ_author_name 'Jing Xi Liu' # Attachment '- La.cif' data_p_La _database_code_depnum_ccdc_archive 'CCDC 883404' #TrackingRef '- La.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H103 Cl2 La N21 O34.50' _chemical_formula_weight 1760.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Fdd2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 36.256(4) _cell_length_b 54.989(5) _cell_length_c 16.0501(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 31999(5) _cell_formula_units_Z 16 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 9631 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.462 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 14672 _exptl_absorpt_coefficient_mu 0.696 _exptl_absorpt_correction_type 'multi scan' _exptl_absorpt_correction_T_min 0.7827 _exptl_absorpt_correction_T_max 0.8675 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 Apex CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 75499 _diffrn_reflns_av_R_equivalents 0.1038 _diffrn_reflns_av_sigmaI/netI 0.0560 _diffrn_reflns_limit_h_min -40 _diffrn_reflns_limit_h_max 42 _diffrn_reflns_limit_k_min -64 _diffrn_reflns_limit_k_max 64 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 24.72 _reflns_number_total 12650 _reflns_number_gt 12242 _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. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.004 0.000 0.103 12797 4479 ' ' 2 -0.028 0.152 0.614 46 10 ' ' 3 0.028 0.348 0.114 46 11 ' ' 4 -0.028 0.652 0.114 46 10 ' ' 5 0.028 0.848 0.614 46 11 ' ' 6 0.222 0.098 0.864 46 21 ' ' 7 0.222 0.598 0.364 46 21 ' ' 8 0.278 0.402 0.864 46 20 ' ' 9 0.278 0.902 0.364 46 20 ' ' 10 0.472 0.152 0.114 46 10 ' ' 11 0.472 0.652 0.614 46 10 ' ' 12 0.528 0.348 0.614 46 11 ' ' 13 0.528 0.848 0.114 46 11 ' ' 14 0.722 0.098 0.364 46 21 ' ' 15 0.722 0.598 0.864 46 21 ' ' 16 0.778 0.402 0.364 46 20 ' ' 17 0.778 0.902 0.864 46 20 ' ' _platon_squeeze_details ; ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1362P)^2^+507.3046P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(11) _refine_ls_number_reflns 12650 _refine_ls_number_parameters 776 _refine_ls_number_restraints 127 _refine_ls_R_factor_all 0.0759 _refine_ls_R_factor_gt 0.0744 _refine_ls_wR_factor_ref 0.1945 _refine_ls_wR_factor_gt 0.1931 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.043 _refine_ls_shift/su_mean 0.008 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group La1 La 0.134326(7) 0.091190(4) 0.272054(19) 0.02220(6) Uani 1 1 d . . . Cl1 Cl 0.12653(12) 0.12451(7) 0.1655(3) 0.1200(12) Uani 1 1 d . . . Cl2 Cl 0.18211(11) 0.06895(7) 0.3508(3) 0.1195(13) Uani 1 1 d . . . O1W O 0.14656(11) 0.06873(8) 0.1375(4) 0.0515(13) Uani 1 1 d . . . O3W O 0.10973(12) 0.08026(9) 0.4160(4) 0.0548(13) Uani 1 1 d . . . O2W O 0.11218(14) 0.04653(8) 0.2849(4) 0.0765(16) Uani 1 1 d U . . C1 C 0.03989(13) 0.08451(8) 0.1794(4) 0.0241(11) Uani 1 1 d U . . C2 C -0.01773(15) 0.07808(9) 0.1132(5) 0.0384(17) Uani 1 1 d . . . C3 C -0.02373(15) 0.08200(9) 0.2070(4) 0.0323(14) Uani 1 1 d . . . C4 C -0.05777(12) 0.11079(8) 0.1281(3) 0.0138(6) Uani 1 1 d U . . C5 C 0.02232(18) 0.08837(10) 0.3267(4) 0.0341(13) Uani 1 1 d U . . H5A H 0.0030 0.0800 0.3585 0.041 Uiso 1 1 calc R . . H5B H 0.0457 0.0801 0.3386 0.041 Uiso 1 1 calc R . . C6 C -0.06066(13) 0.11685(10) 0.2822(4) 0.0278(12) Uani 1 1 d U . . H6A H -0.0831 0.1260 0.2687 0.033 Uiso 1 1 calc R . . H6B H -0.0670 0.1044 0.3236 0.033 Uiso 1 1 calc R . . C7 C 0.05533(14) 0.12720(9) 0.3491(3) 0.0221(11) Uani 1 1 d U . . C8 C -0.00640(15) 0.12726(10) 0.3826(3) 0.0279(12) Uani 1 1 d U . . C9 C 0.01074(14) 0.15201(10) 0.4078(3) 0.0256(13) Uani 1 1 d . . . C10 C -0.03715(15) 0.15783(9) 0.3109(3) 0.0235(12) Uani 1 1 d . . . C11 C 0.07722(15) 0.16773(12) 0.3830(4) 0.0311(14) Uani 1 1 d . . . H11A H 0.1010 0.1593 0.3803 0.037 Uiso 1 1 calc R . . H11B H 0.0755 0.1758 0.4373 0.037 Uiso 1 1 calc R . . C12 C -0.00884(14) 0.19544(11) 0.3645(3) 0.0281(13) Uani 1 1 d . . . H12A H -0.0334 0.2025 0.3564 0.034 Uiso 1 1 calc R . . H12B H -0.0009 0.1998 0.4208 0.034 Uiso 1 1 calc R . . C13 C 0.09944(14) 0.18442(8) 0.2523(3) 0.0194(11) Uani 1 1 d . . . C14 C 0.05607(13) 0.20925(9) 0.3173(4) 0.0250(12) Uani 1 1 d . . . C15 C 0.06865(14) 0.22171(8) 0.2344(4) 0.0272(13) Uani 1 1 d . . . C16 C 0.00411(15) 0.21598(8) 0.2330(4) 0.0267(13) Uani 1 1 d . . . C17 C 0.11864(14) 0.20857(9) 0.1301(4) 0.0277(13) Uani 1 1 d . . . H17A H 0.1422 0.2002 0.1385 0.033 Uiso 1 1 calc R . . H17B H 0.1239 0.2259 0.1231 0.033 Uiso 1 1 calc R . . C18 C 0.03050(17) 0.23285(10) 0.1071(5) 0.0404(17) Uani 1 1 d . . . H18A H 0.0458 0.2475 0.1030 0.048 Uiso 1 1 calc R . . H18B H 0.0047 0.2379 0.1006 0.048 Uiso 1 1 calc R . . C19 C 0.11090(13) 0.17822(10) 0.0225(4) 0.0328(13) Uani 1 1 d . . . C20 C 0.07694(15) 0.21425(9) -0.0035(4) 0.0343(14) Uani 1 1 d . . . C21 C 0.06878(17) 0.19490(13) -0.0747(4) 0.0387(16) Uani 1 1 d . . . C22 C 0.01340(14) 0.20427(9) -0.0037(4) 0.0306(13) Uani 1 1 d . . . C23 C 0.09661(17) 0.15251(13) -0.1025(4) 0.0382(16) Uani 1 1 d . . . H23A H 0.0966 0.1568 -0.1617 0.046 Uiso 1 1 calc R . . H23B H 0.1208 0.1456 -0.0892 0.046 Uiso 1 1 calc R . . C24 C 0.00714(15) 0.17573(10) -0.1192(3) 0.0260(13) Uani 1 1 d . . . H24A H 0.0165 0.1770 -0.1763 0.031 Uiso 1 1 calc R . . H24B H -0.0180 0.1824 -0.1188 0.031 Uiso 1 1 calc R . . C25 C 0.07462(15) 0.11565(10) -0.0314(3) 0.0282(12) Uani 1 1 d U . . C26 C 0.03319(15) 0.13199(9) -0.1300(3) 0.0274(12) Uani 1 1 d U . . C27 C 0.01643(14) 0.10785(9) -0.0899(3) 0.0243(11) Uani 1 1 d U . . C28 C -0.02409(14) 0.13939(8) -0.0592(3) 0.0191(10) Uani 1 1 d U . . C29 C 0.04373(16) 0.08016(11) 0.0300(4) 0.0388(15) Uani 1 1 d . . . H29A H 0.0345 0.0662 -0.0017 0.047 Uiso 1 1 calc R . . H29B H 0.0691 0.0765 0.0467 0.047 Uiso 1 1 calc R . . C30 C -0.04556(16) 0.09898(10) -0.0163(4) 0.0343(14) Uani 1 1 d . . . H30A H -0.0703 0.1055 -0.0267 0.041 Uiso 1 1 calc R . . H30B H -0.0441 0.0831 -0.0436 0.041 Uiso 1 1 calc R . . C31 C -0.02734(17) 0.05177(10) 0.0835(5) 0.0394(14) Uani 1 1 d U . . H31A H -0.0232 0.0503 0.0233 0.047 Uiso 1 1 calc R . . H31B H -0.0115 0.0399 0.1119 0.047 Uiso 1 1 calc R . . C32 C -0.06749(17) 0.04671(11) 0.1035(5) 0.0418(15) Uani 1 1 d U . . H32A H -0.0832 0.0561 0.0654 0.050 Uiso 1 1 calc R . . H32B H -0.0726 0.0294 0.0944 0.050 Uiso 1 1 calc R . . C33 C -0.0768(2) 0.05310(13) 0.1900(5) 0.0533(17) Uani 1 1 d U . . H33A H -0.0891 0.0391 0.2155 0.064 Uiso 1 1 calc R . . H33B H -0.0947 0.0664 0.1886 0.064 Uiso 1 1 calc R . . C34 C -0.04498(16) 0.06066(10) 0.2465(5) 0.0503(19) Uani 1 1 d . . . H34A H -0.0283 0.0469 0.2547 0.060 Uiso 1 1 calc R . . H34B H -0.0546 0.0656 0.3010 0.060 Uiso 1 1 calc R . . C35 C -0.02602(17) 0.11450(14) 0.4595(4) 0.0466(17) Uani 1 1 d . . . H35A H -0.0394 0.1002 0.4395 0.056 Uiso 1 1 calc R . . H35B H -0.0071 0.1089 0.4986 0.056 Uiso 1 1 calc R . . C36 C -0.0504(2) 0.12951(15) 0.5015(5) 0.055(2) Uani 1 1 d . . . H36A H -0.0627 0.1203 0.5459 0.066 Uiso 1 1 calc R . . H36B H -0.0693 0.1355 0.4629 0.066 Uiso 1 1 calc R . . C37 C -0.0289(2) 0.15168(15) 0.5403(5) 0.061(2) Uani 1 1 d . . . H37A H -0.0433 0.1666 0.5318 0.073 Uiso 1 1 calc R . . H37B H -0.0263 0.1492 0.6005 0.073 Uiso 1 1 calc R . . C38 C 0.0096(2) 0.15504(17) 0.5020(5) 0.055(2) Uani 1 1 d . . . H38A H 0.0186 0.1713 0.5161 0.066 Uiso 1 1 calc R . . H38B H 0.0264 0.1432 0.5272 0.066 Uiso 1 1 calc R . . C39 C 0.06552(18) 0.22377(11) 0.3981(4) 0.0455(16) Uani 1 1 d . . . H39A H 0.0547 0.2155 0.4463 0.055 Uiso 1 1 calc R . . H39B H 0.0923 0.2241 0.4056 0.055 Uiso 1 1 calc R . . C40 C 0.0510(2) 0.24974(11) 0.3946(5) 0.054(2) Uani 1 1 d . . . H40A H 0.0631 0.2594 0.4380 0.065 Uiso 1 1 calc R . . H40B H 0.0245 0.2497 0.4061 0.065 Uiso 1 1 calc R . . C41 C 0.0581(2) 0.26194(12) 0.3073(6) 0.060(2) Uani 1 1 d U . . H41A H 0.0346 0.2637 0.2777 0.071 Uiso 1 1 calc R . . H41B H 0.0684 0.2782 0.3155 0.071 Uiso 1 1 calc R . . C42 C 0.08344(18) 0.24745(11) 0.2566(5) 0.0500(19) Uani 1 1 d . . . H42A H 0.1068 0.2457 0.2868 0.060 Uiso 1 1 calc R . . H42B H 0.0886 0.2563 0.2049 0.060 Uiso 1 1 calc R . . C43 C 0.09387(17) 0.23713(12) -0.0277(5) 0.0438(17) Uani 1 1 d . . . H43A H 0.1187 0.2342 -0.0498 0.053 Uiso 1 1 calc R . . H43B H 0.0959 0.2479 0.0208 0.053 Uiso 1 1 calc R . . C44 C 0.0693(2) 0.24917(13) -0.0954(5) 0.0526(17) Uani 1 1 d U . . H44A H 0.0822 0.2633 -0.1186 0.063 Uiso 1 1 calc R . . H44B H 0.0463 0.2549 -0.0700 0.063 Uiso 1 1 calc R . . C45 C 0.0598(3) 0.22991(17) -0.1704(6) 0.065(2) Uani 1 1 d U . . H45A H 0.0331 0.2274 -0.1729 0.078 Uiso 1 1 calc R . . H45B H 0.0677 0.2369 -0.2238 0.078 Uiso 1 1 calc R . . C46 C 0.0769(2) 0.20780(14) -0.1594(5) 0.0526(19) Uani 1 1 d . . . H46A H 0.1036 0.2102 -0.1642 0.063 Uiso 1 1 calc R . . H46B H 0.0693 0.1970 -0.2047 0.063 Uiso 1 1 calc R . . C47 C 0.0346(2) 0.13125(14) -0.2219(5) 0.0529(16) Uani 1 1 d U . . H47A H 0.0460 0.1462 -0.2426 0.063 Uiso 1 1 calc R . . H47B H 0.0095 0.1304 -0.2441 0.063 Uiso 1 1 calc R . . C48 C 0.0567(3) 0.1093(2) -0.2529(7) 0.094(3) Uani 1 1 d . . . H48A H 0.0831 0.1127 -0.2461 0.113 Uiso 1 1 calc R . . H48B H 0.0520 0.1071 -0.3125 0.113 Uiso 1 1 calc R . . C49 C 0.0465(2) 0.08426(17) -0.2035(5) 0.070(2) Uani 1 1 d . . . H49A H 0.0424 0.0711 -0.2437 0.084 Uiso 1 1 calc R . . H49B H 0.0670 0.0796 -0.1673 0.084 Uiso 1 1 calc R . . C50 C 0.01245(17) 0.08784(11) -0.1522(4) 0.0378(16) Uani 1 1 d . . . H50A H -0.0083 0.0916 -0.1892 0.045 Uiso 1 1 calc R . . H50B H 0.0067 0.0727 -0.1228 0.045 Uiso 1 1 calc R . . N1 N 0.02238(13) 0.08257(8) 0.1019(4) 0.0390(14) Uani 1 1 d . . . N2 N 0.01423(13) 0.08591(8) 0.2380(3) 0.0301(11) Uani 1 1 d U . . N3 N -0.04079(13) 0.09567(7) 0.0732(3) 0.0282(12) Uani 1 1 d . . . N4 N -0.04618(12) 0.10496(8) 0.2057(3) 0.0313(12) Uani 1 1 d . . . N5 N 0.02479(13) 0.11311(10) 0.3553(4) 0.0383(14) Uani 1 1 d . . . N6 N 0.04793(13) 0.15016(8) 0.3755(3) 0.0262(11) Uani 1 1 d . . . N7 N -0.03250(12) 0.13353(9) 0.3169(3) 0.0257(11) Uani 1 1 d . . . N8 N -0.01260(13) 0.16936(10) 0.3618(3) 0.0335(12) Uani 1 1 d . . . N9 N 0.07551(12) 0.18613(7) 0.3167(3) 0.0211(10) Uani 1 1 d . . . N10 N 0.09572(12) 0.20527(8) 0.2039(3) 0.0276(11) Uani 1 1 d . . . N11 N 0.01526(13) 0.20687(7) 0.3079(3) 0.0260(11) Uani 1 1 d . . . N12 N 0.03492(12) 0.22297(8) 0.1873(4) 0.0335(13) Uani 1 1 d . . . N13 N 0.10133(14) 0.19937(8) 0.0545(3) 0.0348(12) Uani 1 1 d . . . N14 N 0.09125(13) 0.17450(11) -0.0537(3) 0.0364(13) Uani 1 1 d . . . N15 N 0.04002(12) 0.21668(7) 0.0375(3) 0.0247(11) Uani 1 1 d . . . N16 N 0.02951(13) 0.19005(10) -0.0663(3) 0.0360(13) Uani 1 1 d . . . N17 N 0.06890(13) 0.13431(10) -0.0879(3) 0.0320(12) Uani 1 1 d . . . N18 N 0.04431(12) 0.10140(9) -0.0250(3) 0.0295(11) Uani 1 1 d U . . N19 N 0.00564(12) 0.15046(10) -0.0961(3) 0.0328(12) Uani 1 1 d . . . N20 N -0.01840(12) 0.11514(8) -0.0539(3) 0.0280(11) Uani 1 1 d . . . O4 O 0.07298(10) 0.08543(6) 0.1896(3) 0.0288(9) Uani 1 1 d . . . O1 O 0.08650(9) 0.12014(6) 0.3239(2) 0.0252(9) Uani 1 1 d . . . O3 O 0.12188(10) 0.16816(6) 0.2377(3) 0.0263(9) Uani 1 1 d . . . O2 O 0.13410(11) 0.16422(7) 0.0495(3) 0.0306(10) Uani 1 1 d . . . O5 O 0.10369(10) 0.11227(7) 0.0059(2) 0.0304(10) Uani 1 1 d . . . O8 O -0.08073(10) 0.12722(6) 0.1128(2) 0.0258(9) Uani 1 1 d . . . O10 O -0.05936(10) 0.16771(7) 0.2648(3) 0.0313(9) Uani 1 1 d U . . O6 O -0.02775(10) 0.21645(6) 0.2107(3) 0.0296(10) Uani 1 1 d . . . O9 O -0.02015(10) 0.20504(6) 0.0103(3) 0.0333(10) Uani 1 1 d . . . O7 O -0.05137(11) 0.15111(6) -0.0376(3) 0.0297(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 La1 0.02082(11) 0.01305(10) 0.03274(13) 0.00982(11) -0.01751(11) -0.00334(10) Cl1 0.149(3) 0.0893(19) 0.122(3) 0.0207(19) -0.033(2) -0.008(2) Cl2 0.112(2) 0.115(2) 0.131(3) -0.004(2) -0.024(2) 0.009(2) O1W 0.0247(19) 0.042(2) 0.088(4) -0.033(2) -0.022(2) 0.0106(18) O3W 0.028(2) 0.059(2) 0.078(3) 0.049(2) -0.004(2) 0.0073(19) O2W 0.073(3) 0.030(2) 0.126(4) 0.035(2) -0.066(3) -0.0180(19) C1 0.021(2) 0.0104(17) 0.041(2) 0.0019(17) -0.0152(19) 0.0009(16) C2 0.020(2) 0.013(2) 0.083(5) -0.001(3) -0.010(3) -0.0055(19) C3 0.026(3) 0.021(2) 0.050(3) 0.011(2) -0.024(2) 0.000(2) C4 0.0143(8) 0.0125(8) 0.0147(9) 0.0011(7) -0.0024(7) -0.0007(6) C5 0.041(2) 0.027(2) 0.035(2) 0.0203(19) -0.012(2) 0.0025(19) C6 0.0148(19) 0.034(2) 0.034(2) 0.0087(19) -0.0097(19) -0.0068(17) C7 0.026(2) 0.0234(19) 0.017(2) 0.0158(16) -0.0080(17) -0.0028(17) C8 0.026(2) 0.032(2) 0.026(2) 0.0061(19) -0.0147(19) 0.0001(18) C9 0.017(2) 0.037(3) 0.023(3) -0.008(2) -0.004(2) -0.003(2) C10 0.026(2) 0.034(3) 0.010(2) 0.0019(19) 0.004(2) 0.010(2) C11 0.023(3) 0.053(3) 0.018(3) 0.003(2) -0.012(2) -0.004(2) C12 0.024(2) 0.046(3) 0.014(2) -0.010(2) -0.011(2) 0.004(2) C13 0.034(2) 0.0139(19) 0.010(2) -0.0038(16) -0.0058(19) -0.0068(18) C14 0.015(2) 0.022(2) 0.038(3) -0.017(2) -0.012(2) -0.0015(18) C15 0.022(2) 0.013(2) 0.046(3) -0.016(2) -0.011(2) -0.0007(18) C16 0.037(3) 0.0068(19) 0.036(3) -0.0027(19) -0.002(2) 0.0095(19) C17 0.024(2) 0.020(2) 0.039(3) 0.002(2) -0.022(2) -0.0088(19) C18 0.035(3) 0.025(3) 0.062(4) 0.005(3) -0.022(3) -0.007(2) C19 0.012(2) 0.057(3) 0.029(3) 0.019(3) -0.003(2) -0.014(2) C20 0.030(2) 0.022(2) 0.051(3) 0.019(2) -0.028(2) -0.012(2) C21 0.040(3) 0.064(4) 0.012(3) 0.008(3) -0.013(2) 0.001(3) C22 0.028(3) 0.025(2) 0.038(3) 0.026(2) -0.015(2) -0.006(2) C23 0.032(3) 0.069(4) 0.014(3) -0.010(3) 0.007(2) 0.008(3) C24 0.029(3) 0.035(3) 0.014(2) 0.002(2) -0.012(2) 0.000(2) C25 0.029(2) 0.036(2) 0.019(2) -0.0134(18) -0.0057(18) 0.0028(19) C26 0.035(2) 0.027(2) 0.020(2) -0.0105(18) -0.0125(19) 0.0001(19) C27 0.023(2) 0.028(2) 0.022(2) -0.0147(17) -0.0119(17) -0.0015(18) C28 0.025(2) 0.0208(19) 0.011(2) -0.0065(16) -0.0068(16) 0.0043(17) C29 0.031(3) 0.040(3) 0.045(4) -0.010(3) -0.016(3) 0.015(2) C30 0.032(3) 0.027(2) 0.044(3) -0.020(2) -0.022(2) 0.011(2) C31 0.036(2) 0.024(2) 0.059(3) -0.005(2) -0.019(2) -0.0071(19) C32 0.039(2) 0.024(2) 0.061(3) -0.002(2) -0.021(2) -0.008(2) C33 0.045(3) 0.043(3) 0.072(3) 0.015(2) -0.008(3) -0.009(2) C34 0.026(3) 0.031(3) 0.094(5) 0.031(3) -0.028(3) -0.003(2) C35 0.027(3) 0.086(4) 0.027(3) 0.039(3) -0.002(2) -0.012(3) C36 0.052(4) 0.066(4) 0.046(4) -0.009(3) 0.012(3) 0.016(3) C37 0.081(5) 0.061(4) 0.041(5) -0.004(3) -0.007(4) 0.022(4) C38 0.037(3) 0.088(5) 0.040(5) -0.002(4) -0.009(3) -0.004(3) C39 0.039(3) 0.047(3) 0.051(4) -0.040(3) -0.022(3) 0.018(3) C40 0.072(5) 0.023(3) 0.069(5) -0.019(3) -0.012(4) 0.001(3) C41 0.048(3) 0.031(3) 0.100(5) -0.032(3) -0.018(3) 0.007(3) C42 0.046(3) 0.029(3) 0.075(5) -0.020(3) -0.015(3) -0.013(3) C43 0.030(3) 0.045(3) 0.056(4) 0.031(3) -0.010(3) -0.007(3) C44 0.058(3) 0.049(3) 0.051(3) 0.028(2) -0.005(2) -0.007(2) C45 0.066(3) 0.074(3) 0.056(3) 0.025(3) -0.004(3) -0.011(3) C46 0.043(3) 0.070(4) 0.045(4) 0.031(3) -0.016(3) -0.012(3) C47 0.059(3) 0.065(3) 0.034(3) -0.015(2) -0.003(2) 0.005(2) C48 0.079(6) 0.142(8) 0.061(6) -0.054(6) -0.004(5) -0.017(6) C49 0.055(4) 0.096(5) 0.060(5) -0.050(4) -0.023(3) 0.036(4) C50 0.034(3) 0.037(3) 0.042(4) -0.016(3) -0.012(3) 0.005(2) N1 0.026(2) 0.0115(18) 0.080(4) -0.008(2) -0.028(2) 0.0026(17) N2 0.038(2) 0.0135(16) 0.039(2) 0.0105(16) -0.0224(18) -0.0018(16) N3 0.026(2) 0.0102(17) 0.049(3) -0.0064(18) -0.013(2) 0.0011(16) N4 0.022(2) 0.031(2) 0.041(3) 0.006(2) -0.018(2) -0.0056(18) N5 0.020(2) 0.053(3) 0.041(3) 0.017(2) -0.002(2) -0.004(2) N6 0.034(2) 0.030(2) 0.015(2) 0.0108(17) -0.0107(18) -0.0007(19) N7 0.0173(19) 0.039(2) 0.020(2) -0.0011(19) -0.0108(17) -0.0038(18) N8 0.032(2) 0.054(3) 0.015(2) -0.010(2) -0.0148(18) 0.001(2) N9 0.025(2) 0.0217(19) 0.016(2) -0.0043(16) -0.0039(17) 0.0014(17) N10 0.025(2) 0.021(2) 0.036(3) 0.0033(19) -0.005(2) 0.0103(17) N11 0.037(2) 0.0128(17) 0.028(2) -0.0035(17) -0.007(2) 0.0047(18) N12 0.023(2) 0.0156(19) 0.062(3) 0.006(2) -0.024(2) 0.0021(17) N13 0.038(2) 0.027(2) 0.039(3) 0.014(2) -0.019(2) 0.000(2) N14 0.024(2) 0.067(3) 0.018(2) 0.011(2) -0.0115(18) 0.001(2) N15 0.025(2) 0.0215(18) 0.028(3) 0.0063(17) -0.0111(18) -0.0074(16) N16 0.032(2) 0.047(3) 0.030(3) 0.022(2) -0.010(2) 0.005(2) N17 0.034(2) 0.053(3) 0.009(2) -0.0105(19) -0.0049(18) 0.009(2) N18 0.0271(19) 0.038(2) 0.023(2) -0.0118(17) -0.0143(17) 0.0120(17) N19 0.016(2) 0.048(3) 0.035(3) 0.000(2) -0.0089(19) 0.0158(19) N20 0.025(2) 0.032(2) 0.027(2) -0.0168(18) -0.0168(19) 0.0061(18) O4 0.0272(18) 0.0217(16) 0.037(2) -0.0054(15) -0.0200(16) 0.0151(14) O1 0.0170(16) 0.0212(16) 0.038(2) 0.0094(15) -0.0100(15) -0.0032(14) O3 0.0214(16) 0.0212(17) 0.036(2) 0.0030(15) -0.0078(16) 0.0085(14) O2 0.035(2) 0.0335(19) 0.024(2) 0.0039(15) -0.0084(15) -0.0013(16) O5 0.0205(16) 0.051(2) 0.020(2) 0.0002(16) -0.0141(15) -0.0003(15) O8 0.0306(18) 0.0194(16) 0.027(2) -0.0103(14) -0.0081(15) 0.0052(14) O10 0.0282(16) 0.0402(17) 0.0257(17) -0.0149(15) -0.0182(15) 0.0071(14) O6 0.0199(17) 0.0192(16) 0.050(2) -0.0161(16) -0.0108(16) 0.0063(13) O9 0.0343(19) 0.0214(16) 0.044(2) 0.0139(17) -0.0088(18) 0.0034(14) O7 0.0356(19) 0.0147(15) 0.039(2) -0.0046(15) -0.0208(17) 0.0048(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag La1 Cl2 2.468(4) . ? La1 O1 2.497(4) . ? La1 Cl1 2.522(4) . ? La1 O1W 2.527(5) . ? La1 O3W 2.548(5) . ? La1 O7 2.556(4) 3 ? La1 O2W 2.592(4) . ? La1 O8 2.597(4) 3 ? La1 O4 2.607(4) . ? C1 O4 1.212(6) . ? C1 N2 1.325(8) . ? C1 N1 1.400(8) . ? C2 N3 1.430(7) . ? C2 N1 1.486(7) . ? C2 C3 1.537(10) . ? C2 C31 1.563(8) . ? C3 N2 1.479(7) . ? C3 N4 1.502(7) . ? C3 C34 1.540(8) . ? C4 O8 1.253(6) . ? C4 N4 1.354(7) . ? C4 N3 1.359(7) . ? C5 N5 1.439(8) . ? C5 N2 1.460(8) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N7 1.482(7) . ? C6 N4 1.486(8) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O1 1.262(6) . ? C7 N6 1.358(7) . ? C7 N5 1.355(7) . ? C8 N5 1.441(8) . ? C8 N7 1.458(7) . ? C8 C9 1.550(8) . ? C8 C35 1.588(8) . ? C9 N6 1.448(7) . ? C9 N8 1.473(7) . ? C9 C38 1.522(9) . ? C10 O10 1.221(7) . ? C10 N7 1.350(7) . ? C10 N8 1.364(7) . ? C11 N6 1.440(7) . ? C11 N9 1.469(7) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 N11 1.409(7) . ? C12 N8 1.441(8) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 O3 1.231(6) . ? C13 N9 1.353(7) . ? C13 N10 1.392(6) . ? C14 N9 1.454(6) . ? C14 N11 1.493(7) . ? C14 C15 1.565(8) . ? C14 C39 1.561(8) . ? C15 N10 1.421(7) . ? C15 N12 1.439(7) . ? C15 C42 1.555(7) . ? C16 O6 1.209(7) . ? C16 N11 1.364(7) . ? C16 N12 1.390(8) . ? C17 N10 1.459(8) . ? C17 N13 1.457(8) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 N12 1.407(9) . ? C18 N15 1.468(8) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 O2 1.220(7) . ? C19 N13 1.318(8) . ? C19 N14 1.429(8) . ? C20 C43 1.453(8) . ? C20 N15 1.497(7) . ? C20 N13 1.522(7) . ? C20 C21 1.590(9) . ? C21 N14 1.427(9) . ? C21 N16 1.455(8) . ? C21 C46 1.561(9) . ? C22 O9 1.238(7) . ? C22 N15 1.355(7) . ? C22 N16 1.401(8) . ? C23 N17 1.437(9) . ? C23 N14 1.454(9) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 N16 1.413(7) . ? C24 N19 1.440(7) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C25 O5 1.226(7) . ? C25 N18 1.354(7) . ? C25 N17 1.385(8) . ? C26 N17 1.466(7) . ? C26 C47 1.477(10) . ? C26 N19 1.524(7) . ? C26 C27 1.595(8) . ? C27 N20 1.445(7) . ? C27 N18 1.494(7) . ? C27 C50 1.493(8) . ? C28 O7 1.231(6) . ? C28 N20 1.352(7) . ? C28 N19 1.372(7) . ? C29 N1 1.396(9) . ? C29 N18 1.465(8) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C30 N3 1.458(8) . ? C30 N20 1.457(8) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C31 C32 1.516(9) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C32 C33 1.472(11) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C33 C34 1.526(10) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C35 C36 1.384(10) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C36 C37 1.576(12) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C37 C38 1.536(11) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C39 C40 1.523(9) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C40 C41 1.575(12) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C41 C42 1.464(10) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C43 C44 1.553(10) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C44 C45 1.640(12) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C45 C46 1.375(12) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C47 C48 1.530(14) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C48 C49 1.634(16) . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C49 C50 1.496(10) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? O8 La1 2.597(4) 11_454 ? O7 La1 2.556(4) 11_454 ? 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 Cl2 La1 O1 129.26(14) . . ? Cl2 La1 Cl1 141.78(14) . . ? O1 La1 Cl1 71.63(14) . . ? Cl2 La1 O1W 94.14(14) . . ? O1 La1 O1W 135.91(13) . . ? Cl1 La1 O1W 78.18(15) . . ? Cl2 La1 O3W 70.41(14) . . ? O1 La1 O3W 66.75(13) . . ? Cl1 La1 O3W 138.32(15) . . ? O1W La1 O3W 136.14(16) . . ? Cl2 La1 O7 68.50(13) . 3 ? O1 La1 O7 130.75(11) . 3 ? Cl1 La1 O7 74.22(13) . 3 ? O1W La1 O7 66.47(13) . 3 ? O3W La1 O7 134.25(14) . 3 ? Cl2 La1 O2W 72.98(14) . . ? O1 La1 O2W 111.25(15) . . ? Cl1 La1 O2W 135.03(16) . . ? O1W La1 O2W 70.09(19) . . ? O3W La1 O2W 66.2(2) . . ? O7 La1 O2W 117.99(15) 3 . ? Cl2 La1 O8 72.66(12) . 3 ? O1 La1 O8 74.06(11) . 3 ? Cl1 La1 O8 87.08(12) . 3 ? O1W La1 O8 136.10(13) . 3 ? O3W La1 O8 79.63(14) . 3 ? O7 La1 O8 69.77(12) 3 3 ? O2W La1 O8 137.76(16) . 3 ? Cl2 La1 O4 142.97(12) . . ? O1 La1 O4 69.77(12) . . ? Cl1 La1 O4 69.41(13) . . ? O1W La1 O4 69.91(13) . . ? O3W La1 O4 97.65(14) . . ? O7 La1 O4 127.46(13) 3 . ? O2W La1 O4 70.19(14) . . ? O8 La1 O4 141.45(11) 3 . ? O4 C1 N2 126.6(5) . . ? O4 C1 N1 124.9(5) . . ? N2 C1 N1 108.5(4) . . ? N3 C2 N1 113.9(5) . . ? N3 C2 C3 105.2(5) . . ? N1 C2 C3 103.5(5) . . ? N3 C2 C31 111.0(5) . . ? N1 C2 C31 109.6(5) . . ? C3 C2 C31 113.4(5) . . ? N2 C3 N4 112.7(4) . . ? N2 C3 C2 102.6(5) . . ? N4 C3 C2 100.4(4) . . ? N2 C3 C34 116.0(5) . . ? N4 C3 C34 112.0(5) . . ? C2 C3 C34 111.6(5) . . ? O8 C4 N4 123.9(4) . . ? O8 C4 N3 128.0(5) . . ? N4 C4 N3 108.1(4) . . ? N5 C5 N2 114.3(5) . . ? N5 C5 H5A 108.7 . . ? N2 C5 H5A 108.6 . . ? N5 C5 H5B 108.7 . . ? N2 C5 H5B 108.7 . . ? H5A C5 H5B 107.6 . . ? N7 C6 N4 109.9(4) . . ? N7 C6 H6A 109.7 . . ? N4 C6 H6A 109.7 . . ? N7 C6 H6B 109.7 . . ? N4 C6 H6B 109.7 . . ? H6A C6 H6B 108.2 . . ? O1 C7 N6 124.3(4) . . ? O1 C7 N5 125.4(5) . . ? N6 C7 N5 110.3(5) . . ? N5 C8 N7 114.7(5) . . ? N5 C8 C9 103.8(4) . . ? N7 C8 C9 103.9(4) . . ? N5 C8 C35 110.5(5) . . ? N7 C8 C35 112.1(4) . . ? C9 C8 C35 111.4(5) . . ? N6 C9 N8 113.7(5) . . ? N6 C9 C38 112.8(5) . . ? N8 C9 C38 114.3(5) . . ? N6 C9 C8 102.6(4) . . ? N8 C9 C8 102.0(4) . . ? C38 C9 C8 110.1(5) . . ? O10 C10 N7 124.5(5) . . ? O10 C10 N8 125.9(5) . . ? N7 C10 N8 109.6(5) . . ? N6 C11 N9 111.8(4) . . ? N6 C11 H11A 109.2 . . ? N9 C11 H11A 109.2 . . ? N6 C11 H11B 109.3 . . ? N9 C11 H11B 109.3 . . ? H11A C11 H11B 108.0 . . ? N11 C12 N8 118.9(5) . . ? N11 C12 H12A 107.6 . . ? N8 C12 H12A 107.6 . . ? N11 C12 H12B 107.6 . . ? N8 C12 H12B 107.6 . . ? H12A C12 H12B 107.0 . . ? O3 C13 N9 128.3(4) . . ? O3 C13 N10 123.8(5) . . ? N9 C13 N10 107.9(4) . . ? N9 C14 N11 113.8(4) . . ? N9 C14 C15 103.7(4) . . ? N11 C14 C15 103.9(4) . . ? N9 C14 C39 110.3(4) . . ? N11 C14 C39 110.3(4) . . ? C15 C14 C39 114.7(4) . . ? N10 C15 N12 115.9(5) . . ? N10 C15 C42 114.8(5) . . ? N12 C15 C42 111.7(4) . . ? N10 C15 C14 102.4(4) . . ? N12 C15 C14 102.7(4) . . ? C42 C15 C14 107.7(5) . . ? O6 C16 N11 123.4(5) . . ? O6 C16 N12 127.3(5) . . ? N11 C16 N12 109.2(5) . . ? N10 C17 N13 112.8(4) . . ? N10 C17 H17A 109.0 . . ? N13 C17 H17A 109.0 . . ? N10 C17 H17B 109.0 . . ? N13 C17 H17B 109.0 . . ? H17A C17 H17B 107.8 . . ? N12 C18 N15 115.8(5) . . ? N12 C18 H18A 108.3 . . ? N15 C18 H18A 108.3 . . ? N12 C18 H18B 108.3 . . ? N15 C18 H18B 108.3 . . ? H18A C18 H18B 107.4 . . ? O2 C19 N13 126.8(6) . . ? O2 C19 N14 123.9(6) . . ? N13 C19 N14 109.2(5) . . ? C43 C20 N15 114.7(5) . . ? C43 C20 N13 112.5(5) . . ? N15 C20 N13 107.4(5) . . ? C43 C20 C21 117.8(6) . . ? N15 C20 C21 102.1(4) . . ? N13 C20 C21 100.8(4) . . ? N14 C21 N16 113.1(5) . . ? N14 C21 C46 117.1(5) . . ? N16 C21 C46 110.4(5) . . ? N14 C21 C20 104.4(4) . . ? N16 C21 C20 103.8(5) . . ? C46 C21 C20 106.7(5) . . ? O9 C22 N15 126.4(5) . . ? O9 C22 N16 124.0(5) . . ? N15 C22 N16 109.5(5) . . ? N17 C23 N14 113.5(5) . . ? N17 C23 H23A 108.9 . . ? N14 C23 H23A 108.9 . . ? N17 C23 H23B 108.9 . . ? N14 C23 H23B 108.9 . . ? H23A C23 H23B 107.7 . . ? N16 C24 N19 113.9(4) . . ? N16 C24 H24A 108.8 . . ? N19 C24 H24A 108.8 . . ? N16 C24 H24B 108.8 . . ? N19 C24 H24B 108.7 . . ? H24A C24 H24B 107.7 . . ? O5 C25 N18 125.0(5) . . ? O5 C25 N17 124.1(5) . . ? N18 C25 N17 110.9(5) . . ? N17 C26 C47 115.5(5) . . ? N17 C26 N19 110.9(4) . . ? C47 C26 N19 113.5(5) . . ? N17 C26 C27 102.9(4) . . ? C47 C26 C27 113.2(5) . . ? N19 C26 C27 99.3(4) . . ? N20 C27 N18 112.3(4) . . ? N20 C27 C50 112.8(4) . . ? N18 C27 C50 110.9(4) . . ? N20 C27 C26 105.3(4) . . ? N18 C27 C26 102.8(4) . . ? C50 C27 C26 112.3(5) . . ? O7 C28 N20 128.4(5) . . ? O7 C28 N19 121.4(4) . . ? N20 C28 N19 110.2(4) . . ? N1 C29 N18 115.5(5) . . ? N1 C29 H29A 108.4 . . ? N18 C29 H29A 108.4 . . ? N1 C29 H29B 108.4 . . ? N18 C29 H29B 108.4 . . ? H29A C29 H29B 107.5 . . ? N3 C30 N20 113.8(4) . . ? N3 C30 H30A 108.8 . . ? N20 C30 H30A 108.8 . . ? N3 C30 H30B 108.8 . . ? N20 C30 H30B 108.8 . . ? H30A C30 H30B 107.7 . . ? C32 C31 C2 108.6(5) . . ? C32 C31 H31A 110.0 . . ? C2 C31 H31A 109.9 . . ? C32 C31 H31B 109.9 . . ? C2 C31 H31B 110.0 . . ? H31A C31 H31B 108.3 . . ? C33 C32 C31 112.1(6) . . ? C33 C32 H32A 109.2 . . ? C31 C32 H32A 109.1 . . ? C33 C32 H32B 109.2 . . ? C31 C32 H32B 109.1 . . ? H32A C32 H32B 107.9 . . ? C32 C33 C34 116.8(6) . . ? C32 C33 H33A 108.1 . . ? C34 C33 H33A 108.1 . . ? C32 C33 H33B 108.1 . . ? C34 C33 H33B 108.1 . . ? H33A C33 H33B 107.3 . . ? C33 C34 C3 110.0(6) . . ? C33 C34 H34A 109.6 . . ? C3 C34 H34A 109.7 . . ? C33 C34 H34B 109.7 . . ? C3 C34 H34B 109.6 . . ? H34A C34 H34B 108.2 . . ? C36 C35 C8 113.6(6) . . ? C36 C35 H35A 108.8 . . ? C8 C35 H35A 108.8 . . ? C36 C35 H35B 108.9 . . ? C8 C35 H35B 108.8 . . ? H35A C35 H35B 107.7 . . ? C35 C36 C37 109.8(6) . . ? C35 C36 H36A 109.7 . . ? C37 C36 H36A 109.7 . . ? C35 C36 H36B 109.7 . . ? C37 C36 H36B 109.7 . . ? H36A C36 H36B 108.2 . . ? C38 C37 C36 112.6(7) . . ? C38 C37 H37A 109.0 . . ? C36 C37 H37A 109.0 . . ? C38 C37 H37B 109.1 . . ? C36 C37 H37B 109.1 . . ? H37A C37 H37B 107.8 . . ? C9 C38 C37 114.2(6) . . ? C9 C38 H38A 108.7 . . ? C37 C38 H38A 108.7 . . ? C9 C38 H38B 108.7 . . ? C37 C38 H38B 108.7 . . ? H38A C38 H38B 107.6 . . ? C40 C39 C14 111.9(5) . . ? C40 C39 H39A 109.3 . . ? C14 C39 H39A 109.2 . . ? C40 C39 H39B 109.2 . . ? C14 C39 H39B 109.2 . . ? H39A C39 H39B 107.9 . . ? C39 C40 C41 112.1(6) . . ? C39 C40 H40A 109.2 . . ? C41 C40 H40A 109.2 . . ? C39 C40 H40B 109.1 . . ? C41 C40 H40B 109.2 . . ? H40A C40 H40B 107.9 . . ? C42 C41 C40 111.4(6) . . ? C42 C41 H41A 109.3 . . ? C40 C41 H41A 109.4 . . ? C42 C41 H41B 109.3 . . ? C40 C41 H41B 109.4 . . ? H41A C41 H41B 108.0 . . ? C41 C42 C15 114.0(6) . . ? C41 C42 H42A 108.7 . . ? C15 C42 H42A 108.7 . . ? C41 C42 H42B 108.8 . . ? C15 C42 H42B 108.8 . . ? H42A C42 H42B 107.7 . . ? C20 C43 C44 108.3(5) . . ? C20 C43 H43A 110.0 . . ? C44 C43 H43A 110.1 . . ? C20 C43 H43B 110.0 . . ? C44 C43 H43B 110.0 . . ? H43A C43 H43B 108.4 . . ? C43 C44 C45 111.0(6) . . ? C43 C44 H44A 109.4 . . ? C45 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? C45 C44 H44B 109.4 . . ? H44A C44 H44B 108.0 . . ? C46 C45 C44 112.4(7) . . ? C46 C45 H45A 109.1 . . ? C44 C45 H45A 109.1 . . ? C46 C45 H45B 109.1 . . ? C44 C45 H45B 109.1 . . ? H45A C45 H45B 107.8 . . ? C45 C46 C21 115.4(7) . . ? C45 C46 H46A 108.5 . . ? C21 C46 H46A 108.5 . . ? C45 C46 H46B 108.4 . . ? C21 C46 H46B 108.4 . . ? H46A C46 H46B 107.5 . . ? C26 C47 C48 111.5(7) . . ? C26 C47 H47A 109.3 . . ? C48 C47 H47A 109.3 . . ? C26 C47 H47B 109.4 . . ? C48 C47 H47B 109.4 . . ? H47A C47 H47B 108.0 . . ? C47 C48 C49 112.8(8) . . ? C47 C48 H48A 109.1 . . ? C49 C48 H48A 109.1 . . ? C47 C48 H48B 109.0 . . ? C49 C48 H48B 109.0 . . ? H48A C48 H48B 107.8 . . ? C50 C49 C48 110.1(7) . . ? C50 C49 H49A 109.6 . . ? C48 C49 H49A 109.7 . . ? C50 C49 H49B 109.6 . . ? C48 C49 H49B 109.6 . . ? H49A C49 H49B 108.2 . . ? C27 C50 C49 112.7(6) . . ? C27 C50 H50A 109.0 . . ? C49 C50 H50A 109.1 . . ? C27 C50 H50B 109.0 . . ? C49 C50 H50B 109.1 . . ? H50A C50 H50B 107.8 . . ? C1 N1 C29 119.3(5) . . ? C1 N1 C2 110.4(5) . . ? C29 N1 C2 128.8(5) . . ? C1 N2 C5 123.8(5) . . ? C1 N2 C3 113.9(5) . . ? C5 N2 C3 121.9(5) . . ? C4 N3 C2 112.8(5) . . ? C4 N3 C30 120.6(4) . . ? C2 N3 C30 126.6(5) . . ? C4 N4 C6 123.1(4) . . ? C4 N4 C3 112.3(5) . . ? C6 N4 C3 123.4(5) . . ? C7 N5 C8 110.8(5) . . ? C7 N5 C5 124.6(5) . . ? C8 N5 C5 124.0(5) . . ? C7 N6 C9 111.2(4) . . ? C7 N6 C11 120.2(5) . . ? C9 N6 C11 127.5(5) . . ? C10 N7 C8 111.5(4) . . ? C10 N7 C6 120.0(4) . . ? C8 N7 C6 125.0(4) . . ? C10 N8 C12 122.8(5) . . ? C10 N8 C9 111.9(5) . . ? C12 N8 C9 125.1(4) . . ? C13 N9 C14 112.1(4) . . ? C13 N9 C11 118.6(4) . . ? C14 N9 C11 128.2(4) . . ? C13 N10 C15 113.5(5) . . ? C13 N10 C17 120.0(4) . . ? C15 N10 C17 126.4(4) . . ? C16 N11 C12 123.3(5) . . ? C16 N11 C14 110.5(5) . . ? C12 N11 C14 126.0(4) . . ? C16 N12 C18 119.9(5) . . ? C16 N12 C15 113.1(5) . . ? C18 N12 C15 126.6(5) . . ? C19 N13 C17 121.2(5) . . ? C19 N13 C20 112.9(5) . . ? C17 N13 C20 125.0(4) . . ? C21 N14 C19 112.0(5) . . ? C21 N14 C23 127.1(5) . . ? C19 N14 C23 120.8(5) . . ? C22 N15 C18 120.6(5) . . ? C22 N15 C20 112.2(4) . . ? C18 N15 C20 126.7(4) . . ? C22 N16 C24 120.1(5) . . ? C22 N16 C21 111.9(5) . . ? C24 N16 C21 127.5(5) . . ? C25 N17 C23 121.2(5) . . ? C25 N17 C26 111.7(5) . . ? C23 N17 C26 127.1(5) . . ? C25 N18 C29 121.2(5) . . ? C25 N18 C27 111.1(5) . . ? C29 N18 C27 126.9(4) . . ? C28 N19 C24 124.7(4) . . ? C28 N19 C26 111.9(5) . . ? C24 N19 C26 121.8(5) . . ? C28 N20 C27 112.4(4) . . ? C28 N20 C30 121.6(4) . . ? C27 N20 C30 125.9(4) . . ? C1 O4 La1 156.6(4) . . ? C7 O1 La1 157.7(3) . . ? C4 O8 La1 156.4(3) . 11_454 ? C28 O7 La1 157.8(3) . 11_454 ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 24.72 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.324 _refine_diff_density_min -1.950 _refine_diff_density_rms 0.160 # Attachment '- Dy.cif' data_p_Dy _database_code_depnum_ccdc_archive 'CCDC 883405' #TrackingRef '- Dy.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C100 H117 Cl2 Dy4 N40 O36' _chemical_formula_weight 3176.24 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.7746(11) _cell_length_b 20.9988(14) _cell_length_c 26.1823(18) _cell_angle_alpha 100.806(3) _cell_angle_beta 98.196(3) _cell_angle_gamma 94.875(3) _cell_volume 7845.2(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6425 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 26.43 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.345 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3165 _exptl_absorpt_coefficient_mu 1.992 _exptl_absorpt_correction_type 'multi scan' _exptl_absorpt_correction_T_min 0.5772 _exptl_absorpt_correction_T_max 0.7282 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _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 Apex CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 88338 _diffrn_reflns_av_R_equivalents 0.0654 _diffrn_reflns_av_sigmaI/netI 0.0818 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 0.80 _diffrn_reflns_theta_max 26.00 _reflns_number_total 29870 _reflns_number_gt 20479 _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. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 -0.001 -0.007 2649 1264 ' ' _platon_squeeze_details ; ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0280P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 29870 _refine_ls_number_parameters 1693 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0670 _refine_ls_R_factor_gt 0.0440 _refine_ls_wR_factor_ref 0.0904 _refine_ls_wR_factor_gt 0.0855 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 0.426482(18) 0.573311(10) 0.302552(9) 0.02253(7) Uani 1 1 d . . . Dy2 Dy 0.71080(2) 0.295332(10) 0.159376(10) 0.02856(7) Uani 1 1 d . . . Dy3 Dy 0.422555(19) -0.087066(10) 0.682466(10) 0.02556(7) Uani 1 1 d . . . Dy4 Dy 0.700815(19) 0.238876(10) 0.878931(10) 0.02641(7) Uani 1 1 d . . . Cl1 Cl 0.49008(10) 0.46591(5) 0.25890(5) 0.0323(3) Uani 1 1 d . . . Cl2 Cl 0.48401(10) 0.03137(5) 0.73785(5) 0.0327(3) Uani 1 1 d . . . O1W O 0.3012(3) 0.63690(16) 0.30372(14) 0.0404(10) Uani 1 1 d . . . O2W O 0.4588(3) 0.66759(14) 0.37295(13) 0.0299(9) Uani 1 1 d . . . O3W O 0.5645(3) 0.26573(16) 0.17804(15) 0.0386(10) Uani 1 1 d . . . O4W O 0.7629(3) 0.19678(15) 0.12266(15) 0.0380(10) Uani 1 1 d . . . O5W O 0.7240(3) 0.23379(15) 0.22916(14) 0.0380(10) Uani 1 1 d . . . O6W O 0.6135(3) 0.25252(19) 0.07574(16) 0.0573(13) Uani 1 1 d . . . O7W O 0.7859(3) 0.34368(18) 0.09819(17) 0.0563(13) Uani 1 1 d . . . O8W O 0.8715(3) 0.30485(18) 0.19064(16) 0.0480(11) Uani 1 1 d . . . O9W O 0.2954(3) -0.17066(15) 0.65949(15) 0.0387(10) Uani 1 1 d . . . O10W O 0.4540(3) -0.17422(14) 0.61747(13) 0.0332(9) Uani 1 1 d . . . O11W O 0.6062(3) 0.26841(17) 0.94533(15) 0.0449(11) Uani 1 1 d . . . O12W O 0.5540(3) 0.24317(16) 0.83372(14) 0.0404(10) Uani 1 1 d . . . O13W O 0.8600(3) 0.25306(17) 0.87306(15) 0.0430(11) Uani 1 1 d . . . O14W O 0.7611(3) 0.34467(15) 0.92725(14) 0.0395(10) Uani 1 1 d . . . O15W O 0.7791(3) 0.20295(18) 0.95239(15) 0.0467(11) Uani 1 1 d . . . O16W O 0.7095(3) 0.30368(15) 0.81290(14) 0.0371(10) Uani 1 1 d . . . O1 O 0.4718(2) 0.53370(14) 0.38162(13) 0.0253(8) Uani 1 1 d . . . O2 O 0.3008(2) 0.49882(14) 0.31418(13) 0.0268(9) Uani 1 1 d . . . O3 O 0.3147(3) 0.54565(14) 0.22257(13) 0.0281(9) Uani 1 1 d . . . O4 O 0.4891(2) 0.61764(13) 0.23549(12) 0.0219(8) Uani 1 1 d . . . O5 O 0.5905(3) 0.60826(14) 0.33222(13) 0.0256(8) Uani 1 1 d . . . O6 O 0.6029(3) 0.28803(15) 0.29005(14) 0.0320(9) Uani 1 1 d . . . O7 O 0.4065(3) 0.24305(15) 0.21636(13) 0.0286(9) Uani 1 1 d . . . O8 O 0.4234(2) 0.29790(14) 0.11316(13) 0.0286(9) Uani 1 1 d . . . O9 O 0.6278(3) 0.38151(14) 0.13808(13) 0.0286(9) Uani 1 1 d . . . O10 O 0.7360(3) 0.37409(14) 0.23589(13) 0.0314(9) Uani 1 1 d . . . O11 O 0.3147(3) -0.07871(15) 0.74261(14) 0.0311(9) Uani 1 1 d . . . O12 O 0.2942(3) -0.03407(15) 0.64795(14) 0.0317(9) Uani 1 1 d . . . O13 O 0.4637(3) -0.03883(14) 0.61230(13) 0.0292(9) Uani 1 1 d . . . O14 O 0.5882(3) -0.09306(14) 0.68274(13) 0.0265(9) Uani 1 1 d . . . O15 O 0.4897(2) -0.12013(14) 0.76145(13) 0.0245(8) Uani 1 1 d . . . O16 O 0.4144(3) 0.18536(15) 0.87226(14) 0.0333(9) Uani 1 1 d . . . O17 O 0.3952(3) 0.23817(15) 0.76618(14) 0.0325(9) Uani 1 1 d . . . O18 O 0.5905(3) 0.22927(15) 0.72809(13) 0.0320(9) Uani 1 1 d . . . O19 O 0.7236(3) 0.16506(13) 0.80590(12) 0.0276(9) Uani 1 1 d . . . O20 O 0.6221(2) 0.13910(13) 0.88616(13) 0.0266(9) Uani 1 1 d . . . N1 N 0.5977(3) 0.47753(17) 0.39852(16) 0.0263(11) Uani 1 1 d . . . N2 N 0.4582(3) 0.42704(17) 0.39206(15) 0.0247(10) Uani 1 1 d . . . N3 N 0.6520(3) 0.37735(17) 0.35786(16) 0.0250(10) Uani 1 1 d . . . N4 N 0.5104(3) 0.32542(17) 0.34963(15) 0.0247(10) Uani 1 1 d . . . N5 N 0.3128(3) 0.39671(17) 0.33340(15) 0.0224(10) Uani 1 1 d . . . N6 N 0.2318(3) 0.40407(17) 0.25766(16) 0.0231(10) Uani 1 1 d . . . N7 N 0.3623(3) 0.29308(17) 0.29260(15) 0.0234(10) Uani 1 1 d . . . N8 N 0.2828(3) 0.30184(17) 0.21603(15) 0.0229(10) Uani 1 1 d . . . N9 N 0.2439(3) 0.44355(17) 0.17791(16) 0.0255(10) Uani 1 1 d . . . N10 N 0.3386(3) 0.50066(17) 0.13911(16) 0.0249(10) Uani 1 1 d . . . N11 N 0.2917(3) 0.34226(17) 0.13511(15) 0.0246(10) Uani 1 1 d . . . N12 N 0.3897(3) 0.39933(16) 0.09844(16) 0.0219(10) Uani 1 1 d . . . N13 N 0.4875(3) 0.56310(17) 0.14967(15) 0.0238(10) Uani 1 1 d . . . N14 N 0.6204(3) 0.58942(17) 0.20330(16) 0.0227(10) Uani 1 1 d . . . N15 N 0.5411(3) 0.45999(17) 0.11358(16) 0.0244(10) Uani 1 1 d . . . N16 N 0.6801(3) 0.49145(16) 0.16122(16) 0.0226(10) Uani 1 1 d . . . N17 N 0.7102(3) 0.58359(17) 0.28749(16) 0.0236(10) Uani 1 1 d . . . N18 N 0.7005(3) 0.54300(17) 0.35880(16) 0.0256(10) Uani 1 1 d . . . N19 N 0.7663(3) 0.48555(17) 0.24551(16) 0.0242(10) Uani 1 1 d . . . N20 N 0.7516(3) 0.44302(17) 0.31639(16) 0.0256(10) Uani 1 1 d . . . N21 N 0.3357(3) -0.03137(17) 0.83017(17) 0.0273(11) Uani 1 1 d . . . N22 N 0.2405(3) 0.00981(18) 0.77436(18) 0.0307(11) Uani 1 1 d . . . N23 N 0.3853(3) 0.07858(17) 0.88061(16) 0.0285(11) Uani 1 1 d . . . N24 N 0.2849(3) 0.11885(18) 0.82665(18) 0.0302(11) Uani 1 1 d . . . N25 N 0.2228(3) 0.04762(18) 0.69255(17) 0.0319(11) Uani 1 1 d . . . N26 N 0.2999(3) 0.06994(17) 0.63119(16) 0.0280(11) Uani 1 1 d . . . N27 N 0.2719(3) 0.15712(18) 0.74411(17) 0.0309(11) Uani 1 1 d . . . N28 N 0.3486(3) 0.18082(19) 0.68107(17) 0.0304(11) Uani 1 1 d . . . N29 N 0.4478(3) 0.06549(18) 0.60020(16) 0.0264(11) Uani 1 1 d . . . N30 N 0.5881(3) 0.03818(17) 0.61877(16) 0.0266(11) Uani 1 1 d . . . N31 N 0.4972(3) 0.17559(17) 0.65107(16) 0.0267(11) Uani 1 1 d . . . N32 N 0.6387(3) 0.14866(17) 0.66824(16) 0.0223(10) Uani 1 1 d . . . N33 N 0.6956(3) -0.00920(17) 0.67678(15) 0.0217(10) Uani 1 1 d . . . N34 N 0.7096(3) -0.04964(17) 0.74847(16) 0.0248(10) Uani 1 1 d . . . N35 N 0.7423(3) 0.09992(17) 0.72794(16) 0.0234(10) Uani 1 1 d . . . N36 N 0.7587(3) 0.05928(16) 0.80161(15) 0.0217(10) Uani 1 1 d . . . N37 N 0.6214(3) -0.06798(16) 0.81789(15) 0.0213(10) Uani 1 1 d . . . N38 N 0.4879(3) -0.06733(17) 0.84640(16) 0.0239(10) Uani 1 1 d . . . N39 N 0.6779(3) 0.03899(17) 0.87190(15) 0.0246(10) Uani 1 1 d . . . N40 N 0.5380(3) 0.04489(16) 0.89383(16) 0.0247(10) Uani 1 1 d . . . C1 C 0.5069(4) 0.4837(2) 0.38914(18) 0.0218(12) Uani 1 1 d . . . C2 C 0.6161(4) 0.4117(2) 0.40334(19) 0.0277(13) Uani 1 1 d . . . C3 C 0.5184(4) 0.3757(2) 0.39888(19) 0.0242(12) Uani 1 1 d . . . C4 C 0.5897(4) 0.3267(2) 0.32814(19) 0.0229(12) Uani 1 1 d . . . C5 C 0.3594(4) 0.4200(2) 0.38689(19) 0.0260(13) Uani 1 1 d . . . H5A H 0.3398 0.4620 0.4005 0.031 Uiso 1 1 calc R . . H5B H 0.3407 0.3899 0.4084 0.031 Uiso 1 1 calc R . . C6 C 0.4345(4) 0.2747(2) 0.32854(19) 0.0241(12) Uani 1 1 d . . . H6A H 0.4582 0.2366 0.3104 0.029 Uiso 1 1 calc R . . H6B H 0.4080 0.2624 0.3576 0.029 Uiso 1 1 calc R . . C7 C 0.2854(4) 0.4384(2) 0.3022(2) 0.0262(12) Uani 1 1 d . . . C8 C 0.2855(4) 0.3284(2) 0.30848(19) 0.0244(12) Uani 1 1 d . . . C9 C 0.2271(4) 0.33282(19) 0.25409(19) 0.0228(12) Uani 1 1 d . . . C10 C 0.3560(4) 0.2768(2) 0.23926(19) 0.0208(12) Uani 1 1 d . . . C11 C 0.1889(4) 0.4353(2) 0.21676(19) 0.0247(12) Uani 1 1 d . . . H11A H 0.1314 0.4093 0.1997 0.030 Uiso 1 1 calc R . . H11B H 0.1744 0.4778 0.2332 0.030 Uiso 1 1 calc R . . C12 C 0.2578(4) 0.2899(2) 0.15922(18) 0.0259(13) Uani 1 1 d . . . H12A H 0.1912 0.2829 0.1503 0.031 Uiso 1 1 calc R . . H12B H 0.2813 0.2501 0.1442 0.031 Uiso 1 1 calc R . . C13 C 0.3004(4) 0.5006(2) 0.18307(19) 0.0212(12) Uani 1 1 d . . . C14 C 0.2452(4) 0.3994(2) 0.1279(2) 0.0278(13) Uani 1 1 d . . . C15 C 0.3132(4) 0.4393(2) 0.10095(19) 0.0251(12) Uani 1 1 d . . . C16 C 0.3731(4) 0.3428(2) 0.11613(19) 0.0234(12) Uani 1 1 d . . . C17 C 0.3885(4) 0.5592(2) 0.1325(2) 0.0248(13) Uani 1 1 d . . . H17A H 0.3654 0.5964 0.1523 0.030 Uiso 1 1 calc R . . H17B H 0.3772 0.5618 0.0956 0.030 Uiso 1 1 calc R . . C18 C 0.4712(4) 0.4149(2) 0.07710(19) 0.0247(12) Uani 1 1 d . . . H18A H 0.4540 0.4335 0.0464 0.030 Uiso 1 1 calc R . . H18B H 0.4973 0.3748 0.0655 0.030 Uiso 1 1 calc R . . C19 C 0.5294(4) 0.5921(2) 0.1999(2) 0.0244(12) Uani 1 1 d . . . C20 C 0.5513(4) 0.5322(2) 0.11818(19) 0.0221(12) Uani 1 1 d . . . C21 C 0.6464(4) 0.5537(2) 0.15475(19) 0.0239(12) Uani 1 1 d . . . C22 C 0.6170(4) 0.4393(2) 0.13870(19) 0.0239(12) Uani 1 1 d . . . C23 C 0.6845(4) 0.6236(2) 0.24911(19) 0.0255(12) Uani 1 1 d . . . H23A H 0.6573 0.6606 0.2662 0.031 Uiso 1 1 calc R . . H23B H 0.7397 0.6403 0.2377 0.031 Uiso 1 1 calc R . . C24 C 0.7678(4) 0.4854(2) 0.1913(2) 0.0280(13) Uani 1 1 d . . . H24A H 0.7894 0.4451 0.1755 0.034 Uiso 1 1 calc R . . H24B H 0.8120 0.5211 0.1887 0.034 Uiso 1 1 calc R . . C25 C 0.6592(4) 0.5798(2) 0.3269(2) 0.0278(13) Uani 1 1 d . . . C26 C 0.7843(4) 0.5430(2) 0.2887(2) 0.0266(13) Uani 1 1 d . . . C27 C 0.7758(4) 0.5129(2) 0.3390(2) 0.0292(13) Uani 1 1 d . . . C28 C 0.7496(4) 0.4293(2) 0.2637(2) 0.0258(12) Uani 1 1 d . . . C29 C 0.6654(4) 0.5343(2) 0.40518(19) 0.0261(12) Uani 1 1 d . . . H29A H 0.6377 0.5730 0.4184 0.031 Uiso 1 1 calc R . . H29B H 0.7166 0.5307 0.4317 0.031 Uiso 1 1 calc R . . C30 C 0.7423(4) 0.3914(2) 0.3460(2) 0.0316(14) Uani 1 1 d . . . H30A H 0.7599 0.3519 0.3261 0.038 Uiso 1 1 calc R . . H30B H 0.7852 0.4036 0.3789 0.038 Uiso 1 1 calc R . . C31 C 0.6762(4) 0.4105(2) 0.4553(2) 0.0335(14) Uani 1 1 d . . . H31A H 0.6907 0.3663 0.4556 0.040 Uiso 1 1 calc R . . H31B H 0.7336 0.4381 0.4585 0.040 Uiso 1 1 calc R . . C32 C 0.6291(4) 0.4339(2) 0.5019(2) 0.0353(15) Uani 1 1 d . . . H32A H 0.6250 0.4803 0.5055 0.042 Uiso 1 1 calc R . . H32B H 0.6659 0.4272 0.5338 0.042 Uiso 1 1 calc R . . C33 C 0.5329(4) 0.3983(2) 0.4960(2) 0.0375(15) Uani 1 1 d . . . H33A H 0.5295 0.3777 0.5260 0.045 Uiso 1 1 calc R . . H33B H 0.4889 0.4301 0.4968 0.045 Uiso 1 1 calc R . . C34 C 0.5047(4) 0.3469(2) 0.44625(18) 0.0267(13) Uani 1 1 d . . . H34A H 0.5413 0.3108 0.4476 0.032 Uiso 1 1 calc R . . H34B H 0.4405 0.3302 0.4433 0.032 Uiso 1 1 calc R . . C35 C 0.2276(4) 0.2929(2) 0.3413(2) 0.0295(13) Uani 1 1 d . . . H35A H 0.2666 0.2879 0.3731 0.035 Uiso 1 1 calc R . . H35B H 0.1797 0.3190 0.3517 0.035 Uiso 1 1 calc R . . C36 C 0.1842(4) 0.2267(2) 0.3108(2) 0.0361(15) Uani 1 1 d . . . H36A H 0.1425 0.2080 0.3310 0.043 Uiso 1 1 calc R . . H36B H 0.2318 0.1981 0.3058 0.043 Uiso 1 1 calc R . . C37 C 0.1300(4) 0.2304(2) 0.2559(2) 0.0417(16) Uani 1 1 d . . . H37A H 0.1564 0.2039 0.2286 0.050 Uiso 1 1 calc R . . H37B H 0.0666 0.2120 0.2534 0.050 Uiso 1 1 calc R . . C38 C 0.1308(4) 0.2989(2) 0.2458(2) 0.0325(14) Uani 1 1 d . . . H38A H 0.1016 0.2974 0.2100 0.039 Uiso 1 1 calc R . . H38B H 0.0956 0.3238 0.2694 0.039 Uiso 1 1 calc R . . C39 C 0.1496(4) 0.3815(2) 0.0947(2) 0.0320(13) Uani 1 1 d . . . H39A H 0.1084 0.3631 0.1152 0.038 Uiso 1 1 d R . . C40 C 0.1109(8) 0.4404(5) 0.0778(4) 0.033(3) Uani 0.50 1 d P . . H40A H 0.1022 0.4714 0.1087 0.040 Uiso 0.50 1 calc PR . . H40B H 0.0514 0.4267 0.0557 0.040 Uiso 0.50 1 calc PR . . C40' C 0.1596(9) 0.3485(5) 0.0431(5) 0.048(4) Uani 0.50 1 d P . . H40C H 0.1001 0.3409 0.0206 0.058 Uiso 0.50 1 calc PR . . H40D H 0.1802 0.3063 0.0453 0.058 Uiso 0.50 1 calc PR . . C41 C 0.1777(8) 0.4747(5) 0.0463(4) 0.030(3) Uani 0.50 1 d P . . H41A H 0.1475 0.4704 0.0102 0.036 Uiso 0.50 1 calc PR . . H41B H 0.1898 0.5209 0.0620 0.036 Uiso 0.50 1 calc PR . . C41' C 0.2318(8) 0.3887(5) 0.0166(4) 0.038(3) Uani 0.50 1 d P . . H41C H 0.2815 0.3627 0.0096 0.045 Uiso 0.50 1 calc PR . . H41D H 0.2008 0.3953 -0.0169 0.045 Uiso 0.50 1 calc PR . . C42 C 0.2673(4) 0.4464(2) 0.0462(2) 0.0355(15) Uani 1 1 d . . . H42B H 0.3091 0.4745 0.0325 0.043 Uiso 1 1 d R . . C43 C 0.5467(4) 0.5534(2) 0.0659(2) 0.0289(13) Uani 1 1 d . . . H43A H 0.4846 0.5427 0.0464 0.035 Uiso 1 1 calc R . . H43B H 0.5878 0.5304 0.0452 0.035 Uiso 1 1 calc R . . C44 C 0.5743(4) 0.6267(2) 0.0749(2) 0.0306(14) Uani 1 1 d . . . H44A H 0.5813 0.6381 0.0413 0.037 Uiso 1 1 calc R . . H44B H 0.5249 0.6491 0.0878 0.037 Uiso 1 1 calc R . . C45 C 0.6624(4) 0.6509(2) 0.1132(2) 0.0342(14) Uani 1 1 d . . . H45A H 0.6486 0.6798 0.1439 0.041 Uiso 1 1 calc R . . H45B H 0.7038 0.6760 0.0967 0.041 Uiso 1 1 calc R . . C46 C 0.7102(4) 0.5954(2) 0.1306(2) 0.0280(13) Uani 1 1 d . . . H46A H 0.7293 0.5686 0.1005 0.034 Uiso 1 1 calc R . . H46B H 0.7648 0.6132 0.1563 0.034 Uiso 1 1 calc R . . C47 C 0.8791(4) 0.5817(2) 0.2923(2) 0.0366(15) Uani 1 1 d . . . H47A H 0.9254 0.5517 0.2894 0.044 Uiso 1 1 calc R . . H47B H 0.8780 0.6043 0.2631 0.044 Uiso 1 1 calc R . . C48 C 0.9046(5) 0.6307(3) 0.3437(2) 0.0497(18) Uani 1 1 d . . . H48A H 0.8647 0.6651 0.3435 0.060 Uiso 1 1 calc R . . H48B H 0.9673 0.6505 0.3464 0.060 Uiso 1 1 calc R . . C49 C 0.8966(5) 0.6005(3) 0.3924(2) 0.0489(17) Uani 1 1 d . . . H49A H 0.9561 0.6079 0.4150 0.059 Uiso 1 1 calc R . . H49B H 0.8535 0.6225 0.4121 0.059 Uiso 1 1 calc R . . C50 C 0.8645(4) 0.5269(2) 0.3785(2) 0.0339(14) Uani 1 1 d . . . H50A H 0.9118 0.5037 0.3637 0.041 Uiso 1 1 calc R . . H50B H 0.8545 0.5115 0.4102 0.041 Uiso 1 1 calc R . . C51 C 0.2991(4) -0.0364(2) 0.7795(2) 0.0297(13) Uani 1 1 d . . . C52 C 0.3092(4) 0.0257(2) 0.8640(2) 0.0328(14) Uani 1 1 d . . . C53 C 0.2400(4) 0.0535(2) 0.8246(2) 0.0299(13) Uani 1 1 d . . . C54 C 0.3663(4) 0.1326(2) 0.8602(2) 0.0324(15) Uani 1 1 d . . . C55 C 0.1828(4) 0.0084(2) 0.7252(2) 0.0365(15) Uani 1 1 d . . . H55A H 0.1248 0.0237 0.7322 0.044 Uiso 1 1 calc R . . H55B H 0.1697 -0.0364 0.7059 0.044 Uiso 1 1 calc R . . C56 C 0.2468(4) 0.1652(2) 0.7963(2) 0.0341(14) Uani 1 1 d . . . H56A H 0.1802 0.1596 0.7930 0.041 Uiso 1 1 calc R . . H56B H 0.2685 0.2093 0.8154 0.041 Uiso 1 1 calc R . . C57 C 0.2754(4) 0.0233(2) 0.6568(2) 0.0275(13) Uani 1 1 d . . . C58 C 0.2174(4) 0.1184(2) 0.6958(2) 0.0306(13) Uani 1 1 d . . . C59 C 0.2712(4) 0.1334(2) 0.6521(2) 0.0299(13) Uani 1 1 d . . . C60 C 0.3443(4) 0.1957(2) 0.7338(2) 0.0291(13) Uani 1 1 d . . . C61 C 0.3492(4) 0.0549(2) 0.5865(2) 0.0345(14) Uani 1 1 d . . . H61A H 0.3314 0.0095 0.5694 0.041 Uiso 1 1 calc R . . H61B H 0.3301 0.0815 0.5613 0.041 Uiso 1 1 calc R . . C62 C 0.4175(4) 0.2134(2) 0.6585(2) 0.0313(14) Uani 1 1 d . . . H62A H 0.4395 0.2555 0.6813 0.038 Uiso 1 1 calc R . . H62B H 0.3897 0.2211 0.6247 0.038 Uiso 1 1 calc R . . C63 C 0.4960(4) 0.0178(2) 0.61126(19) 0.0254(13) Uani 1 1 d . . . C64 C 0.5061(4) 0.1273(2) 0.6042(2) 0.0282(13) Uani 1 1 d . . . C65 C 0.6053(4) 0.1083(2) 0.6169(2) 0.0293(13) Uani 1 1 d . . . C66 C 0.5764(4) 0.1877(2) 0.6865(2) 0.0305(14) Uani 1 1 d . . . C67 C 0.6577(4) -0.0053(2) 0.62247(19) 0.0277(13) Uani 1 1 d . . . H67A H 0.7076 0.0088 0.6053 0.033 Uiso 1 1 calc R . . H67B H 0.6316 -0.0487 0.6034 0.033 Uiso 1 1 calc R . . C68 C 0.7303(4) 0.1503(2) 0.6966(2) 0.0293(13) Uani 1 1 d . . . H68A H 0.7470 0.1927 0.7199 0.035 Uiso 1 1 calc R . . H68B H 0.7728 0.1460 0.6715 0.035 Uiso 1 1 calc R . . C69 C 0.6557(4) -0.0534(2) 0.70067(19) 0.0237(13) Uani 1 1 d . . . C70 C 0.7697(4) 0.0352(2) 0.71045(19) 0.0221(12) Uani 1 1 d . . . C71 C 0.7808(4) 0.0060(2) 0.7616(2) 0.0262(13) Uani 1 1 d . . . C72 C 0.7395(4) 0.1122(2) 0.78006(19) 0.0209(11) Uani 1 1 d . . . C73 C 0.6839(4) -0.0918(2) 0.78326(18) 0.0228(12) Uani 1 1 d . . . H73A H 0.6562 -0.1336 0.7618 0.027 Uiso 1 1 calc R . . H73B H 0.7396 -0.0995 0.8046 0.027 Uiso 1 1 calc R . . C74 C 0.7633(4) 0.0595(2) 0.85616(19) 0.0267(13) Uani 1 1 d . . . H74A H 0.7853 0.1033 0.8758 0.032 Uiso 1 1 calc R . . H74B H 0.8083 0.0311 0.8660 0.032 Uiso 1 1 calc R . . C75 C 0.5283(4) -0.0876(2) 0.8042(2) 0.0258(13) Uani 1 1 d . . . C76 C 0.6454(4) -0.0296(2) 0.87151(19) 0.0243(12) Uani 1 1 d . . . C77 C 0.5509(4) -0.0249(2) 0.89011(18) 0.0230(12) Uani 1 1 d . . . C78 C 0.6119(4) 0.0792(2) 0.88358(18) 0.0254(13) Uani 1 1 d . . . C79 C 0.3900(4) -0.0809(2) 0.8465(2) 0.0292(14) Uani 1 1 d . . . H79A H 0.3807 -0.0849 0.8818 0.035 Uiso 1 1 calc R . . H79B H 0.3677 -0.1226 0.8231 0.035 Uiso 1 1 calc R . . C80 C 0.4672(4) 0.0778(2) 0.9172(2) 0.0296(14) Uani 1 1 d . . . H80A H 0.4508 0.0565 0.9450 0.035 Uiso 1 1 calc R . . H80B H 0.4921 0.1224 0.9333 0.035 Uiso 1 1 calc R . . C81 C 0.2654(4) 0.0088(2) 0.9098(2) 0.0386(15) Uani 1 1 d . . . H81A H 0.2183 -0.0310 0.8968 0.046 Uiso 1 1 d R . . H81B H 0.3127 -0.0007 0.9361 0.046 Uiso 1 1 d R . . C82 C 0.2182(6) 0.0626(3) 0.9341(3) 0.040(2) Uani 0.70 1 d P . . H82A H 0.2637 0.0993 0.9512 0.048 Uiso 0.70 1 calc PR . . H82B H 0.1871 0.0487 0.9611 0.048 Uiso 0.70 1 calc PR . . C83 C 0.1461(6) 0.0856(4) 0.8935(3) 0.044(2) Uani 0.70 1 d P . . H83A H 0.0851 0.0775 0.9023 0.053 Uiso 0.70 1 calc PR . . H83B H 0.1594 0.1323 0.8963 0.053 Uiso 0.70 1 calc PR . . C84 C 0.1462(4) 0.0530(3) 0.8403(2) 0.0391(15) Uani 1 1 d . . . H84A H 0.1074 0.0738 0.8167 0.047 Uiso 1 1 d R . . H84B H 0.1184 0.0068 0.8375 0.047 Uiso 1 1 d R . . C85 C 0.1178(4) 0.1342(3) 0.6864(2) 0.0438(16) Uani 1 1 d . . . H85A H 0.0860 0.1204 0.7131 0.053 Uiso 1 1 d R . . H85B H 0.1188 0.1817 0.6899 0.053 Uiso 1 1 d R . . C86 C 0.0667(8) 0.1047(6) 0.6359(5) 0.041(3) Uani 0.50 1 d P . . H86A H 0.0085 0.1228 0.6312 0.049 Uiso 0.50 1 calc PR . . H86B H 0.0537 0.0581 0.6337 0.049 Uiso 0.50 1 calc PR . . C86' C 0.1237(10) 0.2041(6) 0.6722(6) 0.061(4) Uani 0.50 1 d P . . H86C H 0.0609 0.2135 0.6636 0.073 Uiso 0.50 1 d PR . . H86D H 0.1510 0.2348 0.7043 0.073 Uiso 0.50 1 d PR . . C87 C 0.1222(9) 0.1172(5) 0.5915(4) 0.040(3) Uani 0.50 1 d P . . H87A H 0.1337 0.0753 0.5723 0.048 Uiso 0.50 1 calc PR . . H87B H 0.0840 0.1371 0.5671 0.048 Uiso 0.50 1 calc PR . . C87' C 0.1736(10) 0.2169(5) 0.6313(5) 0.049(4) Uani 0.50 1 d P . . H87C H 0.2220 0.2526 0.6456 0.059 Uiso 0.50 1 calc PR . . H87D H 0.1323 0.2298 0.6038 0.059 Uiso 0.50 1 calc PR . . C88 C 0.2132(4) 0.1597(2) 0.6095(2) 0.0400(15) Uani 1 1 d . . . H88B H 0.2458 0.1595 0.5798 0.048 Uiso 1 1 d R . . C89 C 0.4895(4) 0.1532(2) 0.5535(2) 0.0314(14) Uani 1 1 d . . . H89A H 0.4248 0.1585 0.5450 0.038 Uiso 1 1 calc R . . H89B H 0.5249 0.1956 0.5582 0.038 Uiso 1 1 calc R . . C90 C 0.5177(4) 0.1060(3) 0.5088(2) 0.0398(16) Uani 1 1 d . . . H90A H 0.5141 0.1258 0.4781 0.048 Uiso 1 1 calc R . . H90B H 0.4737 0.0670 0.5000 0.048 Uiso 1 1 calc R . . C91 C 0.6139(4) 0.0858(2) 0.5204(2) 0.0351(15) Uani 1 1 d . . . H91A H 0.6498 0.0972 0.4944 0.042 Uiso 1 1 calc R . . H91B H 0.6095 0.0389 0.5172 0.042 Uiso 1 1 calc R . . C92 C 0.6631(4) 0.1189(2) 0.5754(2) 0.0319(14) Uani 1 1 d . . . H92A H 0.7213 0.1015 0.5826 0.038 Uiso 1 1 calc R . . H92B H 0.6762 0.1654 0.5769 0.038 Uiso 1 1 calc R . . C93 C 0.8567(4) 0.0378(2) 0.6863(2) 0.0304(13) Uani 1 1 d . . . H93A H 0.9025 0.0711 0.7086 0.036 Uiso 1 1 calc R . . H93B H 0.8436 0.0498 0.6522 0.036 Uiso 1 1 calc R . . C94 C 0.8951(4) -0.0275(3) 0.6796(2) 0.0402(15) Uani 1 1 d . . . H94A H 0.9544 -0.0225 0.6682 0.048 Uiso 1 1 calc R . . H94B H 0.8542 -0.0585 0.6520 0.048 Uiso 1 1 calc R . . C95 C 0.9068(4) -0.0558(2) 0.7303(2) 0.0388(15) Uani 1 1 d . . . H95A H 0.8716 -0.0985 0.7232 0.047 Uiso 1 1 calc R . . H95B H 0.9711 -0.0613 0.7399 0.047 Uiso 1 1 calc R . . C96 C 0.8755(4) -0.0125(2) 0.7764(2) 0.0279(13) Uani 1 1 d . . . H96A H 0.8756 -0.0355 0.8053 0.033 Uiso 1 1 calc R . . H96B H 0.9186 0.0267 0.7884 0.033 Uiso 1 1 calc R . . C97 C 0.7118(4) -0.0604(2) 0.9062(2) 0.0293(13) Uani 1 1 d . . . H97A H 0.7312 -0.0309 0.9401 0.035 Uiso 1 1 calc R . . H97B H 0.7659 -0.0681 0.8900 0.035 Uiso 1 1 calc R . . C98 C 0.6661(4) -0.1247(2) 0.9144(2) 0.0360(15) Uani 1 1 d . . . H98A H 0.7090 -0.1432 0.9376 0.043 Uiso 1 1 calc R . . H98B H 0.6516 -0.1552 0.8808 0.043 Uiso 1 1 calc R . . C99 C 0.5767(4) -0.1162(2) 0.9384(2) 0.0348(15) Uani 1 1 d . . . H99A H 0.5271 -0.1473 0.9170 0.042 Uiso 1 1 calc R . . H99B H 0.5858 -0.1258 0.9735 0.042 Uiso 1 1 calc R . . C100 C 0.5487(4) -0.0469(2) 0.94170(19) 0.0273(13) Uani 1 1 d . . . H10A H 0.4871 -0.0461 0.9504 0.033 Uiso 1 1 calc R . . H10B H 0.5905 -0.0170 0.9695 0.033 Uiso 1 1 calc R . . C82' C 0.1754(17) -0.0304(9) 0.8914(11) 0.063(7) Uani 0.30 1 d P . . H82C H 0.1859 -0.0744 0.8762 0.076 Uiso 0.30 1 d PR . . H82D H 0.1449 -0.0327 0.9215 0.076 Uiso 0.30 1 d PR . . C83' C 0.1175(16) -0.0085(8) 0.8549(8) 0.045(6) Uani 0.30 1 d P . . H83C H 0.0596 -0.0043 0.8679 0.055 Uiso 0.30 1 d PR . . H83D H 0.1052 -0.0419 0.8230 0.055 Uiso 0.30 1 d 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 Dy1 0.03112(18) 0.01652(10) 0.02182(13) 0.00336(9) 0.00852(11) 0.00737(10) Dy2 0.03527(19) 0.01862(11) 0.03481(16) 0.00407(10) 0.01384(13) 0.00937(11) Dy3 0.03538(19) 0.01758(11) 0.02455(14) 0.00313(9) 0.00911(12) 0.00316(10) Dy4 0.03696(19) 0.01572(11) 0.02695(14) 0.00200(9) 0.00888(12) 0.00425(10) Cl1 0.0420(10) 0.0228(6) 0.0341(8) 0.0030(5) 0.0117(7) 0.0119(6) Cl2 0.0468(10) 0.0212(6) 0.0298(7) 0.0015(5) 0.0115(7) 0.0010(6) O1W 0.046(3) 0.0310(19) 0.040(2) -0.0036(17) 0.000(2) 0.0187(18) O2W 0.038(3) 0.0222(16) 0.026(2) -0.0024(14) 0.0014(18) 0.0052(16) O3W 0.039(3) 0.040(2) 0.041(2) 0.0135(18) 0.012(2) 0.0088(18) O4W 0.040(3) 0.0241(17) 0.050(3) -0.0027(16) 0.013(2) 0.0174(17) O5W 0.051(3) 0.0271(18) 0.040(2) 0.0099(16) 0.012(2) 0.0116(17) O6W 0.078(4) 0.053(2) 0.037(3) 0.003(2) -0.003(2) 0.024(2) O7W 0.069(4) 0.051(2) 0.066(3) 0.023(2) 0.043(3) 0.023(2) O8W 0.031(3) 0.053(2) 0.057(3) 0.001(2) 0.009(2) 0.000(2) O9W 0.038(3) 0.0275(18) 0.048(3) 0.0039(17) 0.008(2) -0.0032(17) O10W 0.049(3) 0.0205(16) 0.032(2) 0.0063(15) 0.0112(19) 0.0029(16) O11W 0.059(3) 0.041(2) 0.041(2) 0.0066(18) 0.031(2) 0.008(2) O12W 0.045(3) 0.037(2) 0.037(2) 0.0068(17) 0.002(2) 0.0010(18) O13W 0.037(3) 0.048(2) 0.037(2) -0.0088(18) 0.005(2) 0.0038(19) O14W 0.055(3) 0.0217(17) 0.040(2) -0.0065(16) 0.018(2) 0.0022(17) O15W 0.059(3) 0.047(2) 0.035(2) 0.0153(18) 0.000(2) 0.002(2) O16W 0.052(3) 0.0244(17) 0.036(2) 0.0074(16) 0.008(2) 0.0060(17) O1 0.032(2) 0.0198(16) 0.027(2) 0.0057(14) 0.0111(17) 0.0076(15) O2 0.033(3) 0.0191(16) 0.030(2) 0.0055(14) 0.0102(17) 0.0033(15) O3 0.044(3) 0.0204(16) 0.0212(19) 0.0027(14) 0.0106(18) 0.0046(16) O4 0.028(2) 0.0206(15) 0.0194(18) 0.0040(14) 0.0104(16) 0.0045(15) O5 0.031(3) 0.0187(16) 0.030(2) 0.0053(14) 0.0099(18) 0.0085(16) O6 0.039(3) 0.0234(17) 0.035(2) 0.0039(16) 0.0099(19) 0.0066(16) O7 0.037(3) 0.0269(17) 0.027(2) 0.0068(15) 0.0133(18) 0.0136(16) O8 0.030(2) 0.0248(17) 0.034(2) 0.0064(15) 0.0123(18) 0.0058(16) O9 0.043(3) 0.0172(16) 0.030(2) 0.0079(14) 0.0111(18) 0.0126(15) O10 0.045(3) 0.0172(16) 0.033(2) 0.0030(15) 0.0105(19) 0.0083(16) O11 0.040(3) 0.0232(17) 0.031(2) 0.0053(15) 0.0110(19) 0.0024(16) O12 0.036(3) 0.0252(18) 0.034(2) 0.0054(15) 0.0081(19) 0.0051(16) O13 0.042(3) 0.0212(16) 0.024(2) 0.0030(14) 0.0101(18) -0.0032(16) O14 0.034(3) 0.0194(16) 0.023(2) 0.0006(14) 0.0035(18) -0.0007(16) O15 0.035(3) 0.0181(15) 0.022(2) 0.0038(14) 0.0059(17) 0.0065(15) O16 0.039(3) 0.0251(18) 0.040(2) 0.0070(16) 0.0143(19) 0.0079(17) O17 0.042(3) 0.0198(16) 0.034(2) 0.0014(16) 0.0086(19) -0.0022(16) O18 0.043(3) 0.0249(17) 0.028(2) 0.0023(16) 0.0067(18) 0.0103(16) O19 0.046(3) 0.0141(15) 0.0223(19) 0.0013(13) 0.0066(18) 0.0043(15) O20 0.037(3) 0.0150(15) 0.029(2) 0.0038(14) 0.0084(18) 0.0095(15) N1 0.032(3) 0.021(2) 0.029(3) 0.0128(18) 0.006(2) 0.0077(19) N2 0.034(3) 0.0207(19) 0.024(2) 0.0107(17) 0.011(2) 0.0071(19) N3 0.030(3) 0.0207(19) 0.027(2) 0.0082(17) 0.007(2) 0.0075(19) N4 0.036(3) 0.0210(19) 0.019(2) 0.0048(17) 0.007(2) 0.0054(19) N5 0.029(3) 0.0190(19) 0.020(2) 0.0049(16) 0.006(2) 0.0037(18) N6 0.025(3) 0.024(2) 0.023(2) 0.0074(17) 0.006(2) 0.0044(18) N7 0.030(3) 0.026(2) 0.018(2) 0.0082(17) 0.008(2) 0.0092(19) N8 0.027(3) 0.024(2) 0.020(2) 0.0028(17) 0.007(2) 0.0084(18) N9 0.027(3) 0.023(2) 0.029(3) 0.0062(18) 0.013(2) 0.0035(18) N10 0.029(3) 0.0176(19) 0.029(3) 0.0036(17) 0.009(2) 0.0038(18) N11 0.036(3) 0.0174(18) 0.023(2) 0.0050(16) 0.011(2) 0.0036(18) N12 0.025(3) 0.0185(18) 0.029(2) 0.0107(17) 0.014(2) 0.0072(17) N13 0.031(3) 0.022(2) 0.019(2) 0.0044(17) 0.002(2) 0.0099(19) N14 0.021(3) 0.0220(19) 0.026(2) 0.0045(17) 0.011(2) 0.0010(18) N15 0.029(3) 0.0184(19) 0.024(2) 0.0018(17) 0.004(2) 0.0004(18) N16 0.021(3) 0.0167(18) 0.033(3) 0.0088(17) 0.008(2) 0.0073(17) N17 0.024(3) 0.0188(19) 0.032(3) 0.0093(17) 0.009(2) 0.0061(18) N18 0.031(3) 0.023(2) 0.024(2) 0.0051(17) 0.005(2) 0.0061(19) N19 0.026(3) 0.023(2) 0.026(2) 0.0073(17) 0.006(2) 0.0071(18) N20 0.031(3) 0.0218(19) 0.025(2) 0.0077(17) 0.003(2) 0.0062(18) N21 0.034(3) 0.021(2) 0.032(3) 0.0077(18) 0.017(2) 0.0070(19) N22 0.029(3) 0.025(2) 0.037(3) 0.0025(19) 0.008(2) 0.0018(19) N23 0.041(3) 0.019(2) 0.026(3) 0.0059(17) 0.005(2) 0.0053(19) N24 0.034(3) 0.022(2) 0.036(3) 0.0069(19) 0.008(2) 0.008(2) N25 0.035(3) 0.024(2) 0.037(3) 0.0046(19) 0.008(2) 0.007(2) N26 0.036(3) 0.021(2) 0.028(3) 0.0068(18) 0.008(2) 0.0010(19) N27 0.037(3) 0.027(2) 0.033(3) 0.0100(19) 0.013(2) 0.005(2) N28 0.033(3) 0.029(2) 0.031(3) 0.0061(19) 0.010(2) 0.004(2) N29 0.032(3) 0.025(2) 0.023(2) 0.0072(17) 0.002(2) 0.0049(19) N30 0.044(3) 0.0168(19) 0.024(2) 0.0091(17) 0.014(2) 0.004(2) N31 0.033(3) 0.023(2) 0.025(2) 0.0018(17) 0.007(2) 0.0104(19) N32 0.019(3) 0.0220(19) 0.024(2) 0.0021(17) -0.001(2) 0.0025(18) N33 0.024(3) 0.0200(19) 0.023(2) 0.0067(17) 0.011(2) -0.0009(18) N34 0.029(3) 0.0186(19) 0.028(3) 0.0043(17) 0.010(2) 0.0026(18) N35 0.027(3) 0.0205(19) 0.028(3) 0.0121(17) 0.011(2) 0.0086(18) N36 0.029(3) 0.0170(18) 0.021(2) 0.0076(16) 0.006(2) 0.0049(17) N37 0.029(3) 0.0176(18) 0.022(2) 0.0070(16) 0.015(2) 0.0029(18) N38 0.032(3) 0.0194(19) 0.024(2) 0.0079(17) 0.012(2) 0.0060(18) N39 0.033(3) 0.0188(19) 0.025(2) 0.0067(17) 0.011(2) 0.0051(19) N40 0.036(3) 0.0129(18) 0.028(2) 0.0046(17) 0.013(2) 0.0042(18) C1 0.030(4) 0.023(2) 0.010(3) 0.0019(19) 0.000(2) 0.000(2) C2 0.043(4) 0.018(2) 0.024(3) 0.005(2) 0.007(3) 0.010(2) C3 0.032(4) 0.020(2) 0.023(3) 0.008(2) 0.006(2) 0.004(2) C4 0.026(4) 0.022(2) 0.022(3) 0.006(2) 0.003(3) 0.006(2) C5 0.038(4) 0.019(2) 0.025(3) 0.002(2) 0.014(3) 0.013(2) C6 0.033(4) 0.017(2) 0.025(3) 0.005(2) 0.011(3) 0.010(2) C7 0.025(4) 0.035(3) 0.025(3) 0.012(2) 0.013(3) 0.011(2) C8 0.035(4) 0.018(2) 0.023(3) 0.005(2) 0.010(3) 0.001(2) C9 0.033(4) 0.012(2) 0.025(3) 0.0027(19) 0.011(3) 0.002(2) C10 0.029(4) 0.014(2) 0.022(3) 0.0068(19) 0.008(2) 0.005(2) C11 0.022(3) 0.031(3) 0.022(3) 0.006(2) 0.002(2) 0.007(2) C12 0.036(4) 0.018(2) 0.022(3) -0.001(2) 0.006(3) 0.002(2) C13 0.022(3) 0.022(2) 0.024(3) 0.010(2) 0.003(2) 0.011(2) C14 0.037(4) 0.022(2) 0.024(3) 0.001(2) 0.005(3) 0.007(2) C15 0.028(4) 0.028(2) 0.022(3) 0.004(2) 0.014(3) 0.006(2) C16 0.027(4) 0.024(2) 0.020(3) 0.004(2) 0.007(2) 0.008(2) C17 0.037(4) 0.016(2) 0.026(3) 0.007(2) 0.012(3) 0.009(2) C18 0.033(4) 0.016(2) 0.026(3) 0.000(2) 0.013(3) 0.006(2) C19 0.028(4) 0.014(2) 0.033(3) 0.008(2) 0.003(3) 0.001(2) C20 0.030(4) 0.014(2) 0.025(3) 0.0061(19) 0.006(2) 0.009(2) C21 0.034(4) 0.018(2) 0.023(3) 0.005(2) 0.013(3) 0.009(2) C22 0.030(4) 0.020(2) 0.025(3) 0.004(2) 0.013(3) 0.004(2) C23 0.033(4) 0.018(2) 0.027(3) 0.005(2) 0.006(3) 0.006(2) C24 0.021(4) 0.023(2) 0.039(3) 0.001(2) 0.007(3) 0.008(2) C25 0.041(4) 0.016(2) 0.024(3) -0.002(2) 0.008(3) -0.005(2) C26 0.028(4) 0.022(2) 0.028(3) 0.000(2) 0.005(3) 0.006(2) C27 0.030(4) 0.025(2) 0.033(3) 0.008(2) 0.004(3) 0.008(2) C28 0.017(3) 0.027(3) 0.035(3) 0.007(2) 0.005(3) 0.008(2) C29 0.026(4) 0.027(2) 0.024(3) 0.004(2) 0.002(2) 0.005(2) C30 0.032(4) 0.028(3) 0.038(3) 0.007(2) 0.010(3) 0.013(2) C31 0.047(4) 0.024(2) 0.031(3) 0.005(2) 0.005(3) 0.012(2) C32 0.051(5) 0.031(3) 0.024(3) 0.005(2) 0.002(3) 0.006(3) C33 0.053(5) 0.041(3) 0.022(3) 0.010(2) 0.008(3) 0.008(3) C34 0.034(4) 0.026(2) 0.023(3) 0.008(2) 0.008(3) 0.008(2) C35 0.036(4) 0.032(3) 0.027(3) 0.011(2) 0.017(3) 0.008(2) C36 0.045(4) 0.030(3) 0.039(4) 0.012(2) 0.020(3) 0.000(3) C37 0.050(5) 0.031(3) 0.043(4) 0.007(3) 0.012(3) -0.009(3) C38 0.033(4) 0.036(3) 0.029(3) 0.003(2) 0.011(3) 0.001(3) C39 0.029(4) 0.036(3) 0.031(3) 0.007(2) 0.007(3) 0.004(2) C40 0.019(7) 0.047(6) 0.025(6) -0.006(5) -0.004(5) 0.002(5) C40' 0.042(9) 0.037(6) 0.055(9) 0.013(6) -0.023(7) -0.007(6) C41 0.028(8) 0.027(5) 0.031(6) 0.005(4) -0.003(5) 0.003(5) C41' 0.044(9) 0.043(6) 0.026(6) 0.001(5) 0.010(6) 0.012(6) C42 0.050(5) 0.030(3) 0.032(3) 0.016(2) 0.010(3) 0.008(3) C43 0.038(4) 0.023(2) 0.027(3) 0.007(2) 0.007(3) 0.007(2) C44 0.049(4) 0.024(2) 0.026(3) 0.011(2) 0.019(3) 0.006(2) C45 0.047(4) 0.021(2) 0.035(3) 0.010(2) 0.008(3) -0.002(2) C46 0.035(4) 0.022(2) 0.028(3) 0.005(2) 0.009(3) 0.004(2) C47 0.038(4) 0.033(3) 0.043(4) 0.013(3) 0.011(3) 0.006(3) C48 0.044(5) 0.047(3) 0.048(4) 0.005(3) -0.008(3) -0.019(3) C49 0.042(5) 0.047(3) 0.048(4) 0.004(3) -0.009(3) -0.011(3) C50 0.025(4) 0.036(3) 0.039(4) 0.006(2) 0.000(3) 0.009(2) C51 0.038(4) 0.019(2) 0.035(3) 0.008(2) 0.015(3) 0.000(2) C52 0.045(4) 0.027(3) 0.029(3) 0.007(2) 0.012(3) 0.008(3) C53 0.028(4) 0.024(2) 0.042(3) 0.009(2) 0.016(3) 0.008(2) C54 0.049(5) 0.025(3) 0.032(3) 0.007(2) 0.023(3) 0.018(3) C55 0.037(4) 0.030(3) 0.046(4) 0.006(3) 0.017(3) 0.010(3) C56 0.038(4) 0.027(3) 0.040(4) 0.006(2) 0.014(3) 0.008(2) C57 0.022(4) 0.026(3) 0.031(3) 0.006(2) -0.004(3) -0.001(2) C58 0.032(4) 0.025(2) 0.035(3) 0.008(2) 0.004(3) 0.004(2) C59 0.029(4) 0.025(2) 0.038(3) 0.007(2) 0.011(3) 0.004(2) C60 0.037(4) 0.023(2) 0.033(3) 0.012(2) 0.013(3) 0.009(2) C61 0.042(4) 0.030(3) 0.031(3) 0.007(2) 0.004(3) 0.004(3) C62 0.041(4) 0.021(2) 0.035(3) 0.008(2) 0.011(3) 0.009(2) C63 0.036(4) 0.019(2) 0.023(3) 0.001(2) 0.013(3) 0.002(2) C64 0.042(4) 0.020(2) 0.025(3) 0.003(2) 0.011(3) 0.012(2) C65 0.044(4) 0.017(2) 0.028(3) 0.007(2) 0.005(3) 0.006(2) C66 0.043(4) 0.020(2) 0.030(3) 0.011(2) 0.008(3) 0.001(2) C67 0.043(4) 0.019(2) 0.020(3) 0.000(2) 0.009(3) 0.003(2) C68 0.033(4) 0.021(2) 0.031(3) 0.000(2) 0.006(3) 0.001(2) C69 0.035(4) 0.021(2) 0.018(3) 0.001(2) 0.008(3) 0.019(2) C70 0.029(4) 0.017(2) 0.022(3) 0.0014(19) 0.009(2) 0.007(2) C71 0.027(4) 0.021(2) 0.029(3) -0.001(2) 0.008(3) 0.001(2) C72 0.020(3) 0.022(2) 0.025(3) 0.009(2) 0.009(2) 0.006(2) C73 0.033(4) 0.020(2) 0.019(3) 0.0057(19) 0.007(2) 0.008(2) C74 0.032(4) 0.024(2) 0.026(3) 0.004(2) 0.007(3) 0.006(2) C75 0.037(4) 0.015(2) 0.031(3) 0.008(2) 0.016(3) 0.009(2) C76 0.035(4) 0.013(2) 0.026(3) 0.005(2) 0.008(3) 0.002(2) C77 0.038(4) 0.018(2) 0.016(3) 0.0064(19) 0.010(2) 0.004(2) C78 0.039(4) 0.021(2) 0.017(3) 0.002(2) 0.004(3) 0.009(2) C79 0.040(4) 0.016(2) 0.037(3) 0.008(2) 0.020(3) 0.006(2) C80 0.049(4) 0.017(2) 0.026(3) 0.002(2) 0.019(3) 0.009(2) C81 0.045(4) 0.035(3) 0.043(4) 0.013(3) 0.023(3) 0.006(3) C82 0.048(6) 0.034(4) 0.042(5) 0.000(4) 0.030(5) 0.009(4) C83 0.038(6) 0.044(5) 0.052(6) 0.000(4) 0.021(5) 0.013(4) C84 0.030(4) 0.037(3) 0.052(4) 0.009(3) 0.010(3) 0.010(3) C85 0.048(5) 0.035(3) 0.053(4) 0.017(3) 0.009(3) 0.003(3) C86 0.022(8) 0.055(7) 0.047(8) 0.011(6) 0.012(6) -0.003(6) C86' 0.051(11) 0.058(8) 0.090(12) 0.037(8) 0.016(9) 0.037(7) C87 0.045(9) 0.038(6) 0.036(7) 0.008(5) -0.007(6) 0.010(6) C87' 0.069(11) 0.047(7) 0.042(8) 0.030(6) 0.009(7) 0.024(7) C88 0.034(4) 0.040(3) 0.047(4) 0.013(3) 0.002(3) 0.008(3) C89 0.036(4) 0.030(3) 0.033(3) 0.012(2) 0.012(3) 0.004(2) C90 0.059(5) 0.038(3) 0.029(3) 0.015(2) 0.015(3) 0.013(3) C91 0.050(5) 0.037(3) 0.023(3) 0.012(2) 0.015(3) 0.005(3) C92 0.044(4) 0.020(2) 0.036(3) 0.008(2) 0.014(3) 0.006(2) C93 0.036(4) 0.032(3) 0.025(3) 0.005(2) 0.011(3) 0.003(2) C94 0.032(4) 0.043(3) 0.046(4) 0.003(3) 0.012(3) 0.007(3) C95 0.045(4) 0.025(3) 0.050(4) 0.003(2) 0.023(3) 0.009(3) C96 0.030(4) 0.023(2) 0.035(3) 0.008(2) 0.013(3) 0.008(2) C97 0.040(4) 0.029(3) 0.022(3) 0.005(2) 0.008(3) 0.009(2) C98 0.063(5) 0.023(2) 0.026(3) 0.011(2) 0.014(3) 0.009(3) C99 0.061(5) 0.020(2) 0.029(3) 0.011(2) 0.016(3) 0.008(3) C100 0.038(4) 0.020(2) 0.025(3) 0.001(2) 0.014(3) 0.006(2) C82' 0.060(19) 0.031(10) 0.11(2) 0.017(12) 0.041(16) 0.009(11) C83' 0.066(18) 0.016(8) 0.055(14) 0.007(8) 0.005(12) 0.019(9) _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 Dy1 O1W 2.373(4) . ? Dy1 O4 2.395(3) . ? Dy1 O2W 2.401(3) . ? Dy1 O1 2.402(3) . ? Dy1 O2 2.415(3) . ? Dy1 O3 2.418(4) . ? Dy1 O5 2.441(4) . ? Dy1 Cl1 2.6412(11) . ? Dy2 O10 2.308(3) . ? Dy2 O3W 2.341(4) . ? Dy2 O4W 2.353(3) . ? Dy2 O9 2.377(3) . ? Dy2 O8W 2.378(4) . ? Dy2 O7W 2.398(4) . ? Dy2 O6W 2.411(4) . ? Dy2 O5W 2.423(4) . ? Dy3 O10W 2.380(3) . ? Dy3 O13 2.384(3) . ? Dy3 O9W 2.386(4) . ? Dy3 O11 2.389(3) . ? Dy3 O15 2.411(3) . ? Dy3 O12 2.428(4) . ? Dy3 O14 2.461(4) . ? Dy3 Cl2 2.6459(12) . ? Dy4 O19 2.309(3) . ? Dy4 O12W 2.336(4) . ? Dy4 O20 2.361(3) . ? Dy4 O14W 2.370(3) . ? Dy4 O13W 2.376(4) . ? Dy4 O15W 2.380(4) . ? Dy4 O16W 2.403(3) . ? Dy4 O11W 2.408(4) . ? O1 C1 1.245(5) . ? O2 C7 1.242(5) . ? O3 C13 1.243(5) . ? O4 C19 1.239(6) . ? O5 C25 1.234(6) . ? O6 C4 1.213(5) . ? O7 C10 1.216(5) . ? O8 C16 1.246(5) . ? O9 C22 1.234(5) . ? O10 C28 1.231(5) . ? O11 C51 1.245(6) . ? O12 C57 1.245(5) . ? O13 C63 1.250(5) . ? O14 C69 1.218(6) . ? O15 C75 1.229(6) . ? O16 C54 1.227(6) . ? O17 C60 1.224(6) . ? O18 C66 1.242(6) . ? O19 C72 1.246(5) . ? O20 C78 1.242(5) . ? N1 C1 1.351(7) . ? N1 C2 1.456(5) . ? N1 C29 1.456(6) . ? N2 C1 1.358(6) . ? N2 C5 1.440(6) . ? N2 C3 1.475(6) . ? N3 C4 1.379(6) . ? N3 C30 1.432(7) . ? N3 C2 1.463(6) . ? N4 C4 1.370(6) . ? N4 C6 1.449(6) . ? N4 C3 1.488(6) . ? N5 C7 1.353(6) . ? N5 C5 1.444(6) . ? N5 C8 1.456(5) . ? N6 C7 1.353(6) . ? N6 C11 1.456(6) . ? N6 C9 1.476(5) . ? N7 C10 1.362(6) . ? N7 C6 1.446(6) . ? N7 C8 1.475(6) . ? N8 C10 1.357(6) . ? N8 C12 1.449(6) . ? N8 C9 1.476(6) . ? N9 C13 1.374(6) . ? N9 C11 1.415(6) . ? N9 C14 1.460(6) . ? N10 C13 1.353(6) . ? N10 C17 1.430(6) . ? N10 C15 1.459(6) . ? N11 C16 1.365(6) . ? N11 C12 1.455(6) . ? N11 C14 1.462(6) . ? N12 C16 1.369(6) . ? N12 C18 1.436(6) . ? N12 C15 1.465(6) . ? N13 C19 1.374(6) . ? N13 C20 1.455(6) . ? N13 C17 1.457(7) . ? N14 C19 1.341(6) . ? N14 C23 1.445(6) . ? N14 C21 1.469(6) . ? N15 C22 1.364(6) . ? N15 C18 1.445(6) . ? N15 C20 1.490(5) . ? N16 C22 1.358(6) . ? N16 C24 1.446(6) . ? N16 C21 1.469(5) . ? N17 C25 1.371(6) . ? N17 C26 1.444(6) . ? N17 C23 1.456(6) . ? N18 C25 1.357(6) . ? N18 C29 1.422(6) . ? N18 C27 1.438(6) . ? N19 C28 1.371(6) . ? N19 C24 1.423(6) . ? N19 C26 1.467(6) . ? N20 C28 1.350(6) . ? N20 C30 1.455(6) . ? N20 C27 1.469(6) . ? N21 C51 1.341(7) . ? N21 C79 1.457(6) . ? N21 C52 1.468(6) . ? N22 C51 1.367(7) . ? N22 C55 1.433(7) . ? N22 C53 1.457(6) . ? N23 C54 1.374(6) . ? N23 C80 1.436(7) . ? N23 C52 1.466(7) . ? N24 C54 1.358(7) . ? N24 C53 1.461(6) . ? N24 C56 1.468(6) . ? N25 C57 1.355(6) . ? N25 C55 1.443(7) . ? N25 C58 1.483(6) . ? N26 C57 1.341(6) . ? N26 C61 1.463(6) . ? N26 C59 1.465(6) . ? N27 C60 1.376(7) . ? N27 C56 1.449(6) . ? N27 C58 1.456(7) . ? N28 C60 1.369(6) . ? N28 C62 1.434(7) . ? N28 C59 1.467(7) . ? N29 C63 1.329(6) . ? N29 C61 1.437(7) . ? N29 C64 1.472(6) . ? N30 C63 1.367(7) . ? N30 C67 1.437(6) . ? N30 C65 1.484(5) . ? N31 C66 1.358(7) . ? N31 C64 1.468(6) . ? N31 C62 1.492(6) . ? N32 C66 1.360(6) . ? N32 C65 1.443(6) . ? N32 C68 1.443(7) . ? N33 C69 1.354(6) . ? N33 C70 1.445(6) . ? N33 C67 1.472(6) . ? N34 C69 1.369(6) . ? N34 C73 1.449(6) . ? N34 C71 1.459(6) . ? N35 C72 1.348(6) . ? N35 C70 1.460(5) . ? N35 C68 1.462(6) . ? N36 C72 1.370(6) . ? N36 C74 1.419(6) . ? N36 C71 1.474(6) . ? N37 C75 1.377(7) . ? N37 C73 1.440(6) . ? N37 C76 1.460(6) . ? N38 C75 1.346(6) . ? N38 C79 1.450(6) . ? N38 C77 1.464(6) . ? N39 C78 1.373(6) . ? N39 C74 1.439(6) . ? N39 C76 1.476(5) . ? N40 C78 1.344(6) . ? N40 C80 1.447(6) . ? N40 C77 1.480(5) . ? C2 C31 1.521(7) . ? C2 C3 1.550(7) . ? C3 C34 1.509(7) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C8 C35 1.540(7) . ? C8 C9 1.579(7) . ? C9 C38 1.502(7) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C14 C39 1.525(8) . ? C14 C15 1.578(7) . ? C15 C42 1.535(7) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C20 C43 1.513(7) . ? C20 C21 1.563(7) . ? C21 C46 1.513(7) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C26 C47 1.540(7) . ? C26 C27 1.580(7) . ? C27 C50 1.519(8) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C32 1.514(7) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 C33 1.522(8) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.508(7) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.506(7) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 C37 1.563(8) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 C38 1.510(7) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 C40' 1.432(13) . ? C39 C40 1.518(12) . ? C39 H39A 0.9700 . ? C40 C41 1.584(15) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C40' C41' 1.615(16) . ? C40' H40C 0.9700 . ? C40' H40D 0.9700 . ? C41 C42 1.496(12) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C41' C42 1.330(11) . ? C41' H41C 0.9700 . ? C41' H41D 0.9700 . ? C42 H42B 0.9700 . ? C43 C44 1.522(6) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 C45 1.512(8) . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C45 C46 1.522(7) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C47 C48 1.511(7) . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C48 C49 1.543(8) . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C49 C50 1.536(7) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C52 C81 1.525(7) . ? C52 C53 1.574(8) . ? C53 C84 1.499(7) . ? C55 H55A 0.9700 . ? C55 H55B 0.9700 . ? C56 H56A 0.9700 . ? C56 H56B 0.9700 . ? C58 C85 1.532(8) . ? C58 C59 1.546(7) . ? C59 C88 1.526(8) . ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? C62 H62A 0.9700 . ? C62 H62B 0.9700 . ? C64 C89 1.524(7) . ? C64 C65 1.558(8) . ? C65 C92 1.511(7) . ? C67 H67A 0.9700 . ? C67 H67B 0.9700 . ? C68 H68A 0.9700 . ? C68 H68B 0.9700 . ? C70 C93 1.514(7) . ? C70 C71 1.568(7) . ? C71 C96 1.501(7) . ? C73 H73A 0.9700 . ? C73 H73B 0.9700 . ? C74 H74A 0.9700 . ? C74 H74B 0.9700 . ? C76 C97 1.510(7) . ? C76 C77 1.548(7) . ? C77 C100 1.512(7) . ? C79 H79A 0.9700 . ? C79 H79B 0.9700 . ? C80 H80A 0.9700 . ? C80 H80B 0.9700 . ? C81 C82' 1.47(2) . ? C81 C82 1.469(8) . ? C81 H81A 1.0126 . ? C81 H81B 0.9700 . ? C82 C83 1.567(12) . ? C82 H82A 0.9700 . ? C82 H82B 0.9700 . ? C83 C84 1.434(9) . ? C83 H83A 0.9700 . ? C83 H83B 0.9700 . ? C84 C83' 1.462(18) . ? C84 H84A 0.9699 . ? C84 H84B 1.0068 . ? C85 C86 1.423(13) . ? C85 C86' 1.578(12) . ? C85 H85A 0.9699 . ? C85 H85B 0.9826 . ? C86 C87 1.563(16) . ? C86 H86A 0.9700 . ? C86 H86B 0.9700 . ? C86' C87' 1.436(17) . ? C86' H85B 0.7267 . ? C86' H86C 0.9701 . ? C86' H86D 0.9698 . ? C87 C88 1.512(13) . ? C87 H87A 0.9700 . ? C87 H87B 0.9700 . ? C87' C88 1.439(12) . ? C87' H87C 0.9700 . ? C87' H87D 0.9700 . ? C88 H88B 0.9701 . ? C89 C90 1.517(7) . ? C89 H89A 0.9700 . ? C89 H89B 0.9700 . ? C90 C91 1.522(8) . ? C90 H90A 0.9700 . ? C90 H90B 0.9700 . ? C91 C92 1.526(7) . ? C91 H91A 0.9700 . ? C91 H91B 0.9700 . ? C92 H92A 0.9700 . ? C92 H92B 0.9700 . ? C93 C94 1.518(7) . ? C93 H93A 0.9700 . ? C93 H93B 0.9700 . ? C94 C95 1.546(8) . ? C94 H94A 0.9700 . ? C94 H94B 0.9700 . ? C95 C96 1.523(7) . ? C95 H95A 0.9700 . ? C95 H95B 0.9700 . ? C96 H96A 0.9700 . ? C96 H96B 0.9700 . ? C97 C98 1.524(7) . ? C97 H97A 0.9700 . ? C97 H97B 0.9700 . ? C98 C99 1.552(8) . ? C98 H98A 0.9700 . ? C98 H98B 0.9700 . ? C99 C100 1.537(6) . ? C99 H99A 0.9700 . ? C99 H99B 0.9700 . ? C100 H10A 0.9700 . ? C100 H10B 0.9700 . ? C82' C83' 1.36(3) . ? C82' H81A 0.6325 . ? C82' H82C 0.9700 . ? C82' H82D 0.9700 . ? C83' H84B 0.6070 . ? C83' H83C 0.9701 . ? C83' H83D 0.9700 . ? 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 O1W Dy1 O4 95.20(12) . . ? O1W Dy1 O2W 68.52(12) . . ? O4 Dy1 O2W 99.40(11) . . ? O1W Dy1 O1 115.61(12) . . ? O4 Dy1 O1 141.74(12) . . ? O2W Dy1 O1 73.77(10) . . ? O1W Dy1 O2 76.45(12) . . ? O4 Dy1 O2 141.27(11) . . ? O2W Dy1 O2 111.77(11) . . ? O1 Dy1 O2 71.73(12) . . ? O1W Dy1 O3 66.41(11) . . ? O4 Dy1 O3 71.67(11) . . ? O2W Dy1 O3 132.76(11) . . ? O1 Dy1 O3 140.09(11) . . ? O2 Dy1 O3 70.35(11) . . ? O1W Dy1 O5 128.98(11) . . ? O4 Dy1 O5 70.81(11) . . ? O2W Dy1 O5 66.13(11) . . ? O1 Dy1 O5 72.16(11) . . ? O2 Dy1 O5 142.63(11) . . ? O3 Dy1 O5 140.49(11) . . ? O1W Dy1 Cl1 146.96(9) . . ? O4 Dy1 Cl1 83.43(7) . . ? O2W Dy1 Cl1 144.39(9) . . ? O1 Dy1 Cl1 82.19(7) . . ? O2 Dy1 Cl1 84.11(8) . . ? O3 Dy1 Cl1 82.06(8) . . ? O5 Dy1 Cl1 81.83(8) . . ? O10 Dy2 O3W 88.47(13) . . ? O10 Dy2 O4W 140.63(13) . . ? O3W Dy2 O4W 105.37(13) . . ? O10 Dy2 O9 75.13(12) . . ? O3W Dy2 O9 77.52(12) . . ? O4W Dy2 O9 143.31(12) . . ? O10 Dy2 O8W 74.54(13) . . ? O3W Dy2 O8W 144.46(14) . . ? O4W Dy2 O8W 73.14(13) . . ? O9 Dy2 O8W 125.43(13) . . ? O10 Dy2 O7W 104.89(13) . . ? O3W Dy2 O7W 141.85(15) . . ? O4W Dy2 O7W 86.84(13) . . ? O9 Dy2 O7W 71.97(13) . . ? O8W Dy2 O7W 73.52(15) . . ? O10 Dy2 O6W 146.38(13) . . ? O3W Dy2 O6W 73.47(15) . . ? O4W Dy2 O6W 72.60(13) . . ? O9 Dy2 O6W 73.42(12) . . ? O8W Dy2 O6W 134.95(14) . . ? O7W Dy2 O6W 76.25(16) . . ? O10 Dy2 O5W 75.77(11) . . ? O3W Dy2 O5W 70.15(13) . . ? O4W Dy2 O5W 74.86(12) . . ? O9 Dy2 O5W 136.55(12) . . ? O8W Dy2 O5W 75.44(14) . . ? O7W Dy2 O5W 147.42(14) . . ? O6W Dy2 O5W 121.47(14) . . ? O10W Dy3 O13 73.92(11) . . ? O10W Dy3 O9W 69.83(12) . . ? O13 Dy3 O9W 115.98(12) . . ? O10W Dy3 O11 133.18(11) . . ? O13 Dy3 O11 139.76(12) . . ? O9W Dy3 O11 65.65(12) . . ? O10W Dy3 O15 100.18(11) . . ? O13 Dy3 O15 141.55(12) . . ? O9W Dy3 O15 96.09(12) . . ? O11 Dy3 O15 71.48(12) . . ? O10W Dy3 O12 111.03(12) . . ? O13 Dy3 O12 71.07(12) . . ? O9W Dy3 O12 75.31(12) . . ? O11 Dy3 O12 70.95(12) . . ? O15 Dy3 O12 141.63(11) . . ? O10W Dy3 O14 66.90(12) . . ? O13 Dy3 O14 72.76(12) . . ? O9W Dy3 O14 130.79(11) . . ? O11 Dy3 O14 139.57(12) . . ? O15 Dy3 O14 70.18(11) . . ? O12 Dy3 O14 142.56(11) . . ? O10W Dy3 Cl2 144.70(9) . . ? O13 Dy3 Cl2 81.86(8) . . ? O9W Dy3 Cl2 145.25(9) . . ? O11 Dy3 Cl2 81.45(8) . . ? O15 Dy3 Cl2 83.08(8) . . ? O12 Dy3 Cl2 83.94(8) . . ? O14 Dy3 Cl2 81.73(8) . . ? O19 Dy4 O12W 87.25(13) . . ? O19 Dy4 O20 75.36(11) . . ? O12W Dy4 O20 78.22(12) . . ? O19 Dy4 O14W 139.51(12) . . ? O12W Dy4 O14W 109.12(13) . . ? O20 Dy4 O14W 142.99(12) . . ? O19 Dy4 O13W 72.64(12) . . ? O12W Dy4 O13W 143.09(14) . . ? O20 Dy4 O13W 123.54(12) . . ? O14W Dy4 O13W 72.61(12) . . ? O19 Dy4 O15W 105.12(12) . . ? O12W Dy4 O15W 142.52(14) . . ? O20 Dy4 O15W 71.30(13) . . ? O14W Dy4 O15W 84.39(13) . . ? O13W Dy4 O15W 73.86(14) . . ? O19 Dy4 O16W 76.23(11) . . ? O12W Dy4 O16W 69.55(13) . . ? O20 Dy4 O16W 137.57(12) . . ? O14W Dy4 O16W 75.60(12) . . ? O13W Dy4 O16W 75.65(14) . . ? O15W Dy4 O16W 147.35(14) . . ? O19 Dy4 O11W 147.61(13) . . ? O12W Dy4 O11W 73.83(14) . . ? O20 Dy4 O11W 75.18(11) . . ? O14W Dy4 O11W 72.57(13) . . ? O13W Dy4 O11W 136.54(14) . . ? O15W Dy4 O11W 77.64(14) . . ? O16W Dy4 O11W 118.99(12) . . ? C1 O1 Dy1 131.7(3) . . ? C7 O2 Dy1 131.6(3) . . ? C13 O3 Dy1 135.1(3) . . ? C19 O4 Dy1 130.9(3) . . ? C25 O5 Dy1 132.0(3) . . ? C22 O9 Dy2 154.3(4) . . ? C28 O10 Dy2 157.7(3) . . ? C51 O11 Dy3 136.1(3) . . ? C57 O12 Dy3 133.0(3) . . ? C63 O13 Dy3 131.8(3) . . ? C69 O14 Dy3 132.4(3) . . ? C75 O15 Dy3 130.8(3) . . ? C72 O19 Dy4 157.5(3) . . ? C78 O20 Dy4 155.0(3) . . ? C1 N1 C2 113.0(4) . . ? C1 N1 C29 120.1(4) . . ? C2 N1 C29 126.8(5) . . ? C1 N2 C5 121.9(4) . . ? C1 N2 C3 111.9(4) . . ? C5 N2 C3 126.2(4) . . ? C4 N3 C30 122.8(4) . . ? C4 N3 C2 112.1(4) . . ? C30 N3 C2 125.1(4) . . ? C4 N4 C6 121.3(4) . . ? C4 N4 C3 112.0(4) . . ? C6 N4 C3 126.2(4) . . ? C7 N5 C5 121.6(4) . . ? C7 N5 C8 113.1(4) . . ? C5 N5 C8 125.2(4) . . ? C7 N6 C11 122.4(4) . . ? C7 N6 C9 112.8(4) . . ? C11 N6 C9 124.6(4) . . ? C10 N7 C6 123.0(4) . . ? C10 N7 C8 112.0(4) . . ? C6 N7 C8 124.9(4) . . ? C10 N8 C12 121.3(4) . . ? C10 N8 C9 112.9(4) . . ? C12 N8 C9 125.2(4) . . ? C13 N9 C11 120.4(4) . . ? C13 N9 C14 111.5(4) . . ? C11 N9 C14 128.0(4) . . ? C13 N10 C17 119.7(4) . . ? C13 N10 C15 112.0(4) . . ? C17 N10 C15 128.0(4) . . ? C16 N11 C12 122.4(4) . . ? C16 N11 C14 112.0(4) . . ? C12 N11 C14 125.7(4) . . ? C16 N12 C18 122.8(4) . . ? C16 N12 C15 112.4(4) . . ? C18 N12 C15 124.6(4) . . ? C19 N13 C20 112.3(4) . . ? C19 N13 C17 122.7(4) . . ? C20 N13 C17 124.7(4) . . ? C19 N14 C23 121.8(4) . . ? C19 N14 C21 113.0(4) . . ? C23 N14 C21 124.9(4) . . ? C22 N15 C18 121.6(4) . . ? C22 N15 C20 112.0(4) . . ? C18 N15 C20 124.8(4) . . ? C22 N16 C24 122.7(4) . . ? C22 N16 C21 112.6(4) . . ? C24 N16 C21 124.6(4) . . ? C25 N17 C26 112.7(4) . . ? C25 N17 C23 119.9(4) . . ? C26 N17 C23 127.4(4) . . ? C25 N18 C29 120.4(4) . . ? C25 N18 C27 113.4(4) . . ? C29 N18 C27 126.1(4) . . ? C28 N19 C24 122.3(4) . . ? C28 N19 C26 111.5(4) . . ? C24 N19 C26 126.2(4) . . ? C28 N20 C30 121.3(4) . . ? C28 N20 C27 112.4(4) . . ? C30 N20 C27 125.8(4) . . ? C51 N21 C79 120.7(4) . . ? C51 N21 C52 111.7(4) . . ? C79 N21 C52 127.4(4) . . ? C51 N22 C55 121.0(4) . . ? C51 N22 C53 111.6(5) . . ? C55 N22 C53 127.2(4) . . ? C54 N23 C80 122.6(5) . . ? C54 N23 C52 111.9(5) . . ? C80 N23 C52 125.4(4) . . ? C54 N24 C53 112.6(4) . . ? C54 N24 C56 123.2(4) . . ? C53 N24 C56 124.1(5) . . ? C57 N25 C55 122.3(4) . . ? C57 N25 C58 112.1(4) . . ? C55 N25 C58 125.5(4) . . ? C57 N26 C61 120.4(4) . . ? C57 N26 C59 113.3(4) . . ? C61 N26 C59 126.3(4) . . ? C60 N27 C56 121.4(4) . . ? C60 N27 C58 111.6(4) . . ? C56 N27 C58 126.1(5) . . ? C60 N28 C62 121.9(4) . . ? C60 N28 C59 111.6(4) . . ? C62 N28 C59 126.3(4) . . ? C63 N29 C61 121.1(4) . . ? C63 N29 C64 112.8(5) . . ? C61 N29 C64 126.1(4) . . ? C63 N30 C67 123.1(4) . . ? C63 N30 C65 111.4(4) . . ? C67 N30 C65 125.2(5) . . ? C66 N31 C64 111.2(4) . . ? C66 N31 C62 122.0(4) . . ? C64 N31 C62 126.4(4) . . ? C66 N32 C65 113.3(4) . . ? C66 N32 C68 122.9(4) . . ? C65 N32 C68 123.8(4) . . ? C69 N33 C70 114.4(4) . . ? C69 N33 C67 120.1(4) . . ? C70 N33 C67 125.2(4) . . ? C69 N34 C73 119.9(4) . . ? C69 N34 C71 112.6(4) . . ? C73 N34 C71 126.7(4) . . ? C72 N35 C70 111.4(4) . . ? C72 N35 C68 121.6(4) . . ? C70 N35 C68 126.6(4) . . ? C72 N36 C74 123.0(4) . . ? C72 N36 C71 110.8(4) . . ? C74 N36 C71 126.0(4) . . ? C75 N37 C73 120.3(4) . . ? C75 N37 C76 112.2(4) . . ? C73 N37 C76 127.0(4) . . ? C75 N38 C79 123.2(4) . . ? C75 N38 C77 113.1(4) . . ? C79 N38 C77 123.4(4) . . ? C78 N39 C74 124.5(4) . . ? C78 N39 C76 111.2(4) . . ? C74 N39 C76 123.9(4) . . ? C78 N40 C80 120.7(4) . . ? C78 N40 C77 111.7(4) . . ? C80 N40 C77 126.1(4) . . ? O1 C1 N1 126.6(4) . . ? O1 C1 N2 124.3(5) . . ? N1 C1 N2 109.0(4) . . ? N1 C2 N3 112.5(4) . . ? N1 C2 C31 112.2(4) . . ? N3 C2 C31 112.4(4) . . ? N1 C2 C3 103.0(4) . . ? N3 C2 C3 104.2(4) . . ? C31 C2 C3 111.9(4) . . ? N2 C3 N4 111.7(4) . . ? N2 C3 C34 112.1(4) . . ? N4 C3 C34 113.0(4) . . ? N2 C3 C2 102.9(4) . . ? N4 C3 C2 102.7(4) . . ? C34 C3 C2 113.5(4) . . ? O6 C4 N4 124.8(5) . . ? O6 C4 N3 126.2(5) . . ? N4 C4 N3 108.9(4) . . ? N2 C5 N5 113.9(4) . . ? N2 C5 H5A 108.8 . . ? N5 C5 H5A 108.8 . . ? N2 C5 H5B 108.8 . . ? N5 C5 H5B 108.8 . . ? H5A C5 H5B 107.7 . . ? N7 C6 N4 114.3(4) . . ? N7 C6 H6A 108.7 . . ? N4 C6 H6A 108.7 . . ? N7 C6 H6B 108.7 . . ? N4 C6 H6B 108.7 . . ? H6A C6 H6B 107.6 . . ? O2 C7 N5 125.5(5) . . ? O2 C7 N6 125.2(5) . . ? N5 C7 N6 109.1(4) . . ? N5 C8 N7 113.9(4) . . ? N5 C8 C35 111.9(4) . . ? N7 C8 C35 112.9(4) . . ? N5 C8 C9 102.8(3) . . ? N7 C8 C9 103.2(4) . . ? C35 C8 C9 111.4(4) . . ? N8 C9 N6 112.1(4) . . ? N8 C9 C38 112.8(4) . . ? N6 C9 C38 114.1(4) . . ? N8 C9 C8 101.9(4) . . ? N6 C9 C8 101.8(4) . . ? C38 C9 C8 113.0(4) . . ? O7 C10 N8 125.7(4) . . ? O7 C10 N7 124.7(5) . . ? N8 C10 N7 109.6(4) . . ? N9 C11 N6 114.2(4) . . ? N9 C11 H11A 108.7 . . ? N6 C11 H11A 108.7 . . ? N9 C11 H11B 108.7 . . ? N6 C11 H11B 108.7 . . ? H11A C11 H11B 107.6 . . ? N8 C12 N11 114.4(4) . . ? N8 C12 H12A 108.7 . . ? N11 C12 H12A 108.7 . . ? N8 C12 H12B 108.7 . . ? N11 C12 H12B 108.7 . . ? H12A C12 H12B 107.6 . . ? O3 C13 N10 124.8(4) . . ? O3 C13 N9 124.9(4) . . ? N10 C13 N9 110.3(4) . . ? N9 C14 N11 112.0(4) . . ? N9 C14 C39 112.3(4) . . ? N11 C14 C39 112.9(4) . . ? N9 C14 C15 103.0(4) . . ? N11 C14 C15 103.5(4) . . ? C39 C14 C15 112.5(4) . . ? N10 C15 N12 112.1(4) . . ? N10 C15 C42 114.6(4) . . ? N12 C15 C42 112.5(4) . . ? N10 C15 C14 103.1(4) . . ? N12 C15 C14 102.4(4) . . ? C42 C15 C14 111.0(4) . . ? O8 C16 N11 125.8(4) . . ? O8 C16 N12 124.6(5) . . ? N11 C16 N12 109.5(4) . . ? N10 C17 N13 113.6(4) . . ? N10 C17 H17A 108.9 . . ? N13 C17 H17A 108.9 . . ? N10 C17 H17B 108.9 . . ? N13 C17 H17B 108.9 . . ? H17A C17 H17B 107.7 . . ? N12 C18 N15 114.3(4) . . ? N12 C18 H18A 108.7 . . ? N15 C18 H18A 108.7 . . ? N12 C18 H18B 108.7 . . ? N15 C18 H18B 108.7 . . ? H18A C18 H18B 107.6 . . ? O4 C19 N14 126.2(5) . . ? O4 C19 N13 125.0(5) . . ? N14 C19 N13 108.8(4) . . ? N13 C20 N15 111.8(4) . . ? N13 C20 C43 111.7(4) . . ? N15 C20 C43 113.9(4) . . ? N13 C20 C21 102.9(4) . . ? N15 C20 C21 102.4(4) . . ? C43 C20 C21 113.3(4) . . ? N14 C21 N16 112.4(4) . . ? N14 C21 C46 113.0(4) . . ? N16 C21 C46 113.2(4) . . ? N14 C21 C20 102.5(4) . . ? N16 C21 C20 103.2(4) . . ? C46 C21 C20 111.6(4) . . ? O9 C22 N16 125.9(5) . . ? O9 C22 N15 124.5(5) . . ? N16 C22 N15 109.5(4) . . ? N14 C23 N17 114.2(4) . . ? N14 C23 H23A 108.7 . . ? N17 C23 H23A 108.7 . . ? N14 C23 H23B 108.7 . . ? N17 C23 H23B 108.7 . . ? H23A C23 H23B 107.6 . . ? N19 C24 N16 114.7(4) . . ? N19 C24 H24A 108.6 . . ? N16 C24 H24A 108.6 . . ? N19 C24 H24B 108.6 . . ? N16 C24 H24B 108.6 . . ? H24A C24 H24B 107.6 . . ? O5 C25 N18 127.8(5) . . ? O5 C25 N17 123.9(5) . . ? N18 C25 N17 108.2(5) . . ? N17 C26 N19 112.2(4) . . ? N17 C26 C47 112.7(4) . . ? N19 C26 C47 112.8(4) . . ? N17 C26 C27 102.7(4) . . ? N19 C26 C27 103.2(4) . . ? C47 C26 C27 112.5(4) . . ? N18 C27 N20 112.6(4) . . ? N18 C27 C50 113.3(4) . . ? N20 C27 C50 112.6(4) . . ? N18 C27 C26 102.6(4) . . ? N20 C27 C26 102.6(4) . . ? C50 C27 C26 112.2(5) . . ? O10 C28 N20 125.1(4) . . ? O10 C28 N19 124.5(5) . . ? N20 C28 N19 110.4(4) . . ? N18 C29 N1 115.2(4) . . ? N18 C29 H29A 108.5 . . ? N1 C29 H29A 108.5 . . ? N18 C29 H29B 108.5 . . ? N1 C29 H29B 108.5 . . ? H29A C29 H29B 107.5 . . ? N3 C30 N20 114.9(4) . . ? N3 C30 H30A 108.5 . . ? N20 C30 H30A 108.5 . . ? N3 C30 H30B 108.5 . . ? N20 C30 H30B 108.5 . . ? H30A C30 H30B 107.5 . . ? C32 C31 C2 111.7(5) . . ? C32 C31 H31A 109.3 . . ? C2 C31 H31A 109.3 . . ? C32 C31 H31B 109.3 . . ? C2 C31 H31B 109.3 . . ? H31A C31 H31B 107.9 . . ? C31 C32 C33 112.0(4) . . ? C31 C32 H32A 109.2 . . ? C33 C32 H32A 109.2 . . ? C31 C32 H32B 109.2 . . ? C33 C32 H32B 109.2 . . ? H32A C32 H32B 107.9 . . ? C34 C33 C32 114.7(5) . . ? C34 C33 H33A 108.6 . . ? C32 C33 H33A 108.6 . . ? C34 C33 H33B 108.6 . . ? C32 C33 H33B 108.6 . . ? H33A C33 H33B 107.6 . . ? C3 C34 C33 110.0(4) . . ? C3 C34 H34A 109.7 . . ? C33 C34 H34A 109.7 . . ? C3 C34 H34B 109.7 . . ? C33 C34 H34B 109.7 . . ? H34A C34 H34B 108.2 . . ? C36 C35 C8 111.5(4) . . ? C36 C35 H35A 109.3 . . ? C8 C35 H35A 109.3 . . ? C36 C35 H35B 109.3 . . ? C8 C35 H35B 109.3 . . ? H35A C35 H35B 108.0 . . ? C35 C36 C37 111.9(4) . . ? C35 C36 H36A 109.2 . . ? C37 C36 H36A 109.2 . . ? C35 C36 H36B 109.2 . . ? C37 C36 H36B 109.2 . . ? H36A C36 H36B 107.9 . . ? C38 C37 C36 113.6(4) . . ? C38 C37 H37A 108.9 . . ? C36 C37 H37A 108.9 . . ? C38 C37 H37B 108.9 . . ? C36 C37 H37B 108.9 . . ? H37A C37 H37B 107.7 . . ? C9 C38 C37 111.7(5) . . ? C9 C38 H38A 109.3 . . ? C37 C38 H38A 109.3 . . ? C9 C38 H38B 109.3 . . ? C37 C38 H38B 109.3 . . ? H38A C38 H38B 107.9 . . ? C40' C39 C40 96.3(7) . . ? C40' C39 C14 108.3(7) . . ? C40 C39 C14 112.0(5) . . ? C40' C39 H39A 121.9 . . ? C40 C39 H39A 108.9 . . ? C14 C39 H39A 108.9 . . ? C39 C40 C41 111.2(8) . . ? C39 C40 H40A 109.4 . . ? C41 C40 H40A 109.4 . . ? C39 C40 H40B 109.4 . . ? C41 C40 H40B 109.4 . . ? H40A C40 H40B 108.0 . . ? C39 C40' C41' 113.0(8) . . ? C39 C40' H40C 109.0 . . ? C41' C40' H40C 109.0 . . ? C39 C40' H40D 109.0 . . ? C41' C40' H40D 109.0 . . ? H40C C40' H40D 107.8 . . ? C42 C41 C40 112.6(8) . . ? C42 C41 H41A 109.1 . . ? C40 C41 H41A 109.1 . . ? C42 C41 H41B 109.1 . . ? C40 C41 H41B 109.1 . . ? H41A C41 H41B 107.8 . . ? C42 C41' C40' 113.8(8) . . ? C42 C41' H41C 108.8 . . ? C40' C41' H41C 108.8 . . ? C42 C41' H41D 108.8 . . ? C40' C41' H41D 108.8 . . ? H41C C41' H41D 107.7 . . ? C41' C42 C41 95.7(7) . . ? C41' C42 C15 111.2(6) . . ? C41 C42 C15 113.8(6) . . ? C41' C42 H42B 119.0 . . ? C41 C42 H42B 108.4 . . ? C15 C42 H42B 108.4 . . ? C20 C43 C44 110.0(4) . . ? C20 C43 H43A 109.7 . . ? C44 C43 H43A 109.7 . . ? C20 C43 H43B 109.7 . . ? C44 C43 H43B 109.7 . . ? H43A C43 H43B 108.2 . . ? C45 C44 C43 114.4(4) . . ? C45 C44 H44A 108.7 . . ? C43 C44 H44A 108.7 . . ? C45 C44 H44B 108.7 . . ? C43 C44 H44B 108.7 . . ? H44A C44 H44B 107.6 . . ? C44 C45 C46 112.3(4) . . ? C44 C45 H45A 109.1 . . ? C46 C45 H45A 109.1 . . ? C44 C45 H45B 109.1 . . ? C46 C45 H45B 109.1 . . ? H45A C45 H45B 107.9 . . ? C21 C46 C45 110.6(4) . . ? C21 C46 H46A 109.5 . . ? C45 C46 H46A 109.5 . . ? C21 C46 H46B 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 108.1 . . ? C48 C47 C26 111.3(5) . . ? C48 C47 H47A 109.4 . . ? C26 C47 H47A 109.4 . . ? C48 C47 H47B 109.4 . . ? C26 C47 H47B 109.4 . . ? H47A C47 H47B 108.0 . . ? C47 C48 C49 113.2(5) . . ? C47 C48 H48A 108.9 . . ? C49 C48 H48A 108.9 . . ? C47 C48 H48B 108.9 . . ? C49 C48 H48B 108.9 . . ? H48A C48 H48B 107.8 . . ? C50 C49 C48 113.3(5) . . ? C50 C49 H49A 108.9 . . ? C48 C49 H49A 108.9 . . ? C50 C49 H49B 108.9 . . ? C48 C49 H49B 108.9 . . ? H49A C49 H49B 107.7 . . ? C27 C50 C49 110.3(4) . . ? C27 C50 H50A 109.6 . . ? C49 C50 H50A 109.6 . . ? C27 C50 H50B 109.6 . . ? C49 C50 H50B 109.6 . . ? H50A C50 H50B 108.1 . . ? O11 C51 N21 124.3(5) . . ? O11 C51 N22 125.1(5) . . ? N21 C51 N22 110.6(4) . . ? N23 C52 N21 111.8(4) . . ? N23 C52 C81 113.1(4) . . ? N21 C52 C81 113.2(4) . . ? N23 C52 C53 102.9(4) . . ? N21 C52 C53 102.9(4) . . ? C81 C52 C53 112.0(5) . . ? N22 C53 N24 112.1(4) . . ? N22 C53 C84 112.6(5) . . ? N24 C53 C84 113.8(4) . . ? N22 C53 C52 102.8(4) . . ? N24 C53 C52 103.0(4) . . ? C84 C53 C52 111.5(5) . . ? O16 C54 N24 125.9(5) . . ? O16 C54 N23 124.6(6) . . ? N24 C54 N23 109.4(5) . . ? N22 C55 N25 113.7(5) . . ? N22 C55 H55A 108.8 . . ? N25 C55 H55A 108.8 . . ? N22 C55 H55B 108.8 . . ? N25 C55 H55B 108.8 . . ? H55A C55 H55B 107.7 . . ? N27 C56 N24 113.0(4) . . ? N27 C56 H56A 109.0 . . ? N24 C56 H56A 109.0 . . ? N27 C56 H56B 109.0 . . ? N24 C56 H56B 109.0 . . ? H56A C56 H56B 107.8 . . ? O12 C57 N26 125.9(5) . . ? O12 C57 N25 125.1(5) . . ? N26 C57 N25 108.9(4) . . ? N27 C58 N25 111.6(4) . . ? N27 C58 C85 113.7(4) . . ? N25 C58 C85 112.2(4) . . ? N27 C58 C59 103.9(4) . . ? N25 C58 C59 102.6(4) . . ? C85 C58 C59 112.1(5) . . ? N26 C59 N28 112.7(4) . . ? N26 C59 C88 111.7(4) . . ? N28 C59 C88 112.4(4) . . ? N26 C59 C58 102.8(4) . . ? N28 C59 C58 103.5(4) . . ? C88 C59 C58 113.2(5) . . ? O17 C60 N28 125.2(5) . . ? O17 C60 N27 125.6(5) . . ? N28 C60 N27 109.2(5) . . ? N29 C61 N26 114.5(4) . . ? N29 C61 H61A 108.6 . . ? N26 C61 H61A 108.6 . . ? N29 C61 H61B 108.6 . . ? N26 C61 H61B 108.6 . . ? H61A C61 H61B 107.6 . . ? N28 C62 N31 113.0(4) . . ? N28 C62 H62A 109.0 . . ? N31 C62 H62A 109.0 . . ? N28 C62 H62B 109.0 . . ? N31 C62 H62B 109.0 . . ? H62A C62 H62B 107.8 . . ? O13 C63 N29 126.0(5) . . ? O13 C63 N30 123.8(5) . . ? N29 C63 N30 110.1(4) . . ? N31 C64 N29 111.9(4) . . ? N31 C64 C89 112.9(4) . . ? N29 C64 C89 111.5(4) . . ? N31 C64 C65 103.7(4) . . ? N29 C64 C65 102.9(4) . . ? C89 C64 C65 113.3(4) . . ? N32 C65 N30 112.5(4) . . ? N32 C65 C92 114.1(4) . . ? N30 C65 C92 111.9(4) . . ? N32 C65 C64 102.5(4) . . ? N30 C65 C64 102.6(4) . . ? C92 C65 C64 112.4(4) . . ? O18 C66 N31 125.1(5) . . ? O18 C66 N32 125.6(5) . . ? N31 C66 N32 109.3(4) . . ? N30 C67 N33 114.2(4) . . ? N30 C67 H67A 108.7 . . ? N33 C67 H67A 108.7 . . ? N30 C67 H67B 108.7 . . ? N33 C67 H67B 108.7 . . ? H67A C67 H67B 107.6 . . ? N32 C68 N35 115.3(4) . . ? N32 C68 H68A 108.5 . . ? N35 C68 H68A 108.5 . . ? N32 C68 H68B 108.5 . . ? N35 C68 H68B 108.5 . . ? H68A C68 H68B 107.5 . . ? O14 C69 N33 127.8(5) . . ? O14 C69 N34 124.8(5) . . ? N33 C69 N34 107.2(5) . . ? N33 C70 N35 112.5(4) . . ? N33 C70 C93 112.4(4) . . ? N35 C70 C93 112.5(4) . . ? N33 C70 C71 102.0(4) . . ? N35 C70 C71 103.8(4) . . ? C93 C70 C71 112.9(4) . . ? N34 C71 N36 112.2(4) . . ? N34 C71 C96 113.1(4) . . ? N36 C71 C96 111.9(4) . . ? N34 C71 C70 102.8(4) . . ? N36 C71 C70 102.7(3) . . ? C96 C71 C70 113.3(4) . . ? O19 C72 N35 124.9(4) . . ? O19 C72 N36 123.9(4) . . ? N35 C72 N36 111.2(4) . . ? N37 C73 N34 116.0(4) . . ? N37 C73 H73A 108.3 . . ? N34 C73 H73A 108.3 . . ? N37 C73 H73B 108.3 . . ? N34 C73 H73B 108.3 . . ? H73A C73 H73B 107.4 . . ? N36 C74 N39 115.3(4) . . ? N36 C74 H74A 108.5 . . ? N39 C74 H74A 108.5 . . ? N36 C74 H74B 108.5 . . ? N39 C74 H74B 108.5 . . ? H74A C74 H74B 107.5 . . ? O15 C75 N38 126.1(5) . . ? O15 C75 N37 125.6(5) . . ? N38 C75 N37 108.2(5) . . ? N37 C76 N39 111.6(4) . . ? N37 C76 C97 112.6(4) . . ? N39 C76 C97 112.5(4) . . ? N37 C76 C77 103.2(4) . . ? N39 C76 C77 103.1(3) . . ? C97 C76 C77 113.2(4) . . ? N38 C77 N40 112.4(4) . . ? N38 C77 C100 112.3(4) . . ? N40 C77 C100 112.9(4) . . ? N38 C77 C76 102.6(4) . . ? N40 C77 C76 103.4(4) . . ? C100 C77 C76 112.4(4) . . ? O20 C78 N40 125.8(5) . . ? O20 C78 N39 123.8(5) . . ? N40 C78 N39 110.3(4) . . ? N38 C79 N21 114.0(4) . . ? N38 C79 H79A 108.8 . . ? N21 C79 H79A 108.8 . . ? N38 C79 H79B 108.8 . . ? N21 C79 H79B 108.8 . . ? H79A C79 H79B 107.7 . . ? N23 C80 N40 114.1(4) . . ? N23 C80 H80A 108.7 . . ? N40 C80 H80A 108.7 . . ? N23 C80 H80B 108.7 . . ? N40 C80 H80B 108.7 . . ? H80A C80 H80B 107.6 . . ? C82' C81 C82 88.9(9) . . ? C82' C81 C52 111.6(11) . . ? C82 C81 C52 111.5(5) . . ? C82' C81 H81A 20.6 . . ? C82 C81 H81A 107.9 . . ? C52 C81 H81A 110.0 . . ? C82' C81 H81B 124.4 . . ? C82 C81 H81B 109.3 . . ? C52 C81 H81B 109.3 . . ? H81A C81 H81B 108.8 . . ? C81 C82 C83 113.0(6) . . ? C81 C82 H82A 109.0 . . ? C83 C82 H82A 109.0 . . ? C81 C82 H82B 109.0 . . ? C83 C82 H82B 109.0 . . ? H82A C82 H82B 107.8 . . ? C84 C83 C82 112.7(6) . . ? C84 C83 H83A 109.1 . . ? C82 C83 H83A 109.1 . . ? C84 C83 H83B 109.1 . . ? C82 C83 H83B 109.1 . . ? H83A C83 H83B 107.8 . . ? C83 C84 C83' 88.6(9) . . ? C83 C84 C53 114.0(6) . . ? C83' C84 C53 111.6(10) . . ? C83 C84 H84A 108.8 . . ? C83' C84 H84A 123.9 . . ? C53 C84 H84A 108.7 . . ? C83 C84 H84B 105.9 . . ? C83' C84 H84B 19.1 . . ? C53 C84 H84B 110.1 . . ? H84A C84 H84B 109.3 . . ? C86 C85 C58 115.2(7) . . ? C86 C85 C86' 92.3(8) . . ? C58 C85 C86' 105.5(7) . . ? C86 C85 H85A 108.4 . . ? C58 C85 H85A 108.6 . . ? C86' C85 H85A 126.5 . . ? C86 C85 H85B 107.3 . . ? C58 C85 H85B 108.2 . . ? C86' C85 H85B 19.3 . . ? H85A C85 H85B 109.0 . . ? C85 C86 C87 110.3(9) . . ? C85 C86 H86A 109.6 . . ? C87 C86 H86A 109.6 . . ? C85 C86 H86B 109.6 . . ? C87 C86 H86B 109.6 . . ? H86A C86 H86B 108.1 . . ? C87' C86' C85 119.9(10) . . ? C87' C86' H85B 142.3 . . ? C85 C86' H85B 26.5 . . ? C87' C86' H86C 108.7 . . ? C85 C86' H86C 106.6 . . ? H85B C86' H86C 101.8 . . ? C87' C86' H86D 107.4 . . ? C85 C86' H86D 106.7 . . ? H85B C86' H86D 83.7 . . ? H86C C86' H86D 106.7 . . ? C88 C87 C86 116.1(9) . . ? C88 C87 H87A 108.3 . . ? C86 C87 H87A 108.3 . . ? C88 C87 H87B 108.3 . . ? C86 C87 H87B 108.3 . . ? H87A C87 H87B 107.4 . . ? C86' C87' C88 110.3(9) . . ? C86' C87' H87C 109.6 . . ? C88 C87' H87C 109.6 . . ? C86' C87' H87D 109.6 . . ? C88 C87' H87D 109.6 . . ? H87C C87' H87D 108.1 . . ? C87' C88 C87 95.0(8) . . ? C87' C88 C59 111.7(6) . . ? C87 C88 C59 109.5(6) . . ? C87' C88 H88B 120.6 . . ? C87 C88 H88B 109.5 . . ? C59 C88 H88B 109.4 . . ? C90 C89 C64 109.7(4) . . ? C90 C89 H89A 109.7 . . ? C64 C89 H89A 109.7 . . ? C90 C89 H89B 109.7 . . ? C64 C89 H89B 109.7 . . ? H89A C89 H89B 108.2 . . ? C89 C90 C91 115.0(5) . . ? C89 C90 H90A 108.5 . . ? C91 C90 H90A 108.5 . . ? C89 C90 H90B 108.5 . . ? C91 C90 H90B 108.5 . . ? H90A C90 H90B 107.5 . . ? C90 C91 C92 112.0(4) . . ? C90 C91 H91A 109.2 . . ? C92 C91 H91A 109.2 . . ? C90 C91 H91B 109.2 . . ? C92 C91 H91B 109.2 . . ? H91A C91 H91B 107.9 . . ? C65 C92 C91 111.2(5) . . ? C65 C92 H92A 109.4 . . ? C91 C92 H92A 109.4 . . ? C65 C92 H92B 109.4 . . ? C91 C92 H92B 109.4 . . ? H92A C92 H92B 108.0 . . ? C70 C93 C94 111.3(4) . . ? C70 C93 H93A 109.4 . . ? C94 C93 H93A 109.4 . . ? C70 C93 H93B 109.4 . . ? C94 C93 H93B 109.4 . . ? H93A C93 H93B 108.0 . . ? C93 C94 C95 113.9(4) . . ? C93 C94 H94A 108.8 . . ? C95 C94 H94A 108.8 . . ? C93 C94 H94B 108.8 . . ? C95 C94 H94B 108.8 . . ? H94A C94 H94B 107.7 . . ? C96 C95 C94 112.8(4) . . ? C96 C95 H95A 109.0 . . ? C94 C95 H95A 109.0 . . ? C96 C95 H95B 109.0 . . ? C94 C95 H95B 109.0 . . ? H95A C95 H95B 107.8 . . ? C71 C96 C95 111.8(5) . . ? C71 C96 H96A 109.3 . . ? C95 C96 H96A 109.3 . . ? C71 C96 H96B 109.3 . . ? C95 C96 H96B 109.3 . . ? H96A C96 H96B 107.9 . . ? C76 C97 C98 110.2(5) . . ? C76 C97 H97A 109.6 . . ? C98 C97 H97A 109.6 . . ? C76 C97 H97B 109.6 . . ? C98 C97 H97B 109.6 . . ? H97A C97 H97B 108.1 . . ? C97 C98 C99 112.3(4) . . ? C97 C98 H98A 109.2 . . ? C99 C98 H98A 109.2 . . ? C97 C98 H98B 109.2 . . ? C99 C98 H98B 109.2 . . ? H98A C98 H98B 107.9 . . ? C100 C99 C98 112.4(4) . . ? C100 C99 H99A 109.1 . . ? C98 C99 H99A 109.1 . . ? C100 C99 H99B 109.1 . . ? C98 C99 H99B 109.1 . . ? H99A C99 H99B 107.9 . . ? C77 C100 C99 111.1(4) . . ? C77 C100 H10A 109.4 . . ? C99 C100 H10A 109.4 . . ? C77 C100 H10B 109.4 . . ? C99 C100 H10B 109.4 . . ? H10A C100 H10B 108.0 . . ? C83' C82' C81 115.7(17) . . ? C83' C82' H81A 136.4 . . ? C81 C82' H81A 34.3 . . ? C83' C82' H82C 108.1 . . ? C81 C82' H82C 108.1 . . ? H81A C82' H82C 74.8 . . ? C83' C82' H82D 108.5 . . ? C81 C82' H82D 108.7 . . ? H81A C82' H82D 111.8 . . ? H82C C82' H82D 107.5 . . ? C82' C83' C84 118.5(18) . . ? C82' C83' H84B 140.7 . . ? C84 C83' H84B 32.8 . . ? C82' C83' H83C 107.6 . . ? C84 C83' H83C 107.8 . . ? H84B C83' H83C 108.2 . . ? C82' C83' H83D 107.9 . . ? C84 C83' H83D 107.5 . . ? H84B C83' H83D 76.3 . . ? H83C C83' H83D 107.0 . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 1.215 _refine_diff_density_min -1.228 _refine_diff_density_rms 0.119 # Attachment '- Er.cif' data_p21c _database_code_depnum_ccdc_archive 'CCDC 883406' #TrackingRef '- Er.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H100 Cl6 Er2 N20 O30' _chemical_formula_weight 2008.72 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 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 26.288(11) _cell_length_b 28.856(12) _cell_length_c 20.917(9) _cell_angle_alpha 90.00 _cell_angle_beta 100.996(5) _cell_angle_gamma 90.00 _cell_volume 15576(12) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9921 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 26.62 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.744 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8304 _exptl_absorpt_coefficient_mu 2.442 _exptl_absorpt_correction_type 'multi scan' _exptl_absorpt_correction_T_min 0.4417 _exptl_absorpt_correction_T_max 0.6541 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 94381 _diffrn_reflns_av_R_equivalents 0.1040 _diffrn_reflns_av_sigmaI/netI 0.1502 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 27.57 _reflns_number_total 35670 _reflns_number_gt 17432 _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. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.038 0.000 -0.013 2711 1149 ' ' 2 0.018 0.500 0.781 2711 1143 ' ' _platon_squeeze_details ; ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0380P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 35670 _refine_ls_number_parameters 1603 _refine_ls_number_restraints 39 _refine_ls_R_factor_all 0.1220 _refine_ls_R_factor_gt 0.0679 _refine_ls_wR_factor_ref 0.1688 _refine_ls_wR_factor_gt 0.1533 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Er1 Er 0.645069(13) 0.789282(11) 0.379104(16) 0.02654(9) Uani 1 1 d . . . Er2 Er 0.815025(13) 0.646516(12) 0.679080(16) 0.02924(9) Uani 1 1 d . . . Er3 Er 0.096249(13) 0.645473(12) 0.736481(16) 0.02948(9) Uani 1 1 d . . . Er4 Er 0.265250(13) 0.784399(11) 1.038066(16) 0.02540(8) Uani 1 1 d . . . Cl1 Cl 0.69469(8) 0.75877(7) 0.49174(9) 0.0380(5) Uani 1 1 d . . . Cl2 Cl 0.57776(17) 0.77260(15) 0.28880(19) 0.1220(14) Uani 1 1 d . . . Cl3 Cl 0.33235(16) 0.76943(15) 1.1275(2) 0.1237(14) Uani 1 1 d . . . Cl4 Cl 0.21627(8) 0.75322(7) 0.92598(9) 0.0373(5) Uani 1 1 d . . . O1W O 0.6318(2) 0.85058(19) 0.3045(3) 0.0467(16) Uani 1 1 d . . . O2W O 0.8551(2) 0.61878(18) 0.7811(2) 0.0384(14) Uani 1 1 d . . . O3W O 0.7833(2) 0.71919(18) 0.6974(3) 0.0453(16) Uani 1 1 d . . . O4W O 0.7981(2) 0.56675(19) 0.6781(3) 0.0549(18) Uani 1 1 d . . . O5W O 0.8906(2) 0.6938(2) 0.7133(3) 0.0542(18) Uani 1 1 d . . . O6W O 0.8834(2) 0.6097(2) 0.6372(3) 0.0595(19) Uani 1 1 d . . . O7W O 0.7469(2) 0.63924(18) 0.7419(2) 0.0383(14) Uani 1 1 d . . . O8W O 0.2767(2) 0.8463(2) 1.1129(3) 0.0523(17) Uani 1 1 d . . . O9W O 0.0257(2) 0.6103(2) 0.7726(3) 0.067(2) Uani 1 1 d . . . O10W O 0.1124(2) 0.5654(2) 0.7413(3) 0.065(2) Uani 1 1 d . . . O11W O 0.1611(2) 0.6372(2) 0.6716(3) 0.0561(18) Uani 1 1 d . . . O12W O 0.1318(2) 0.71617(19) 0.7216(3) 0.0542(17) Uani 1 1 d . . . O13W O 0.0533(2) 0.61778(19) 0.6354(3) 0.0490(17) Uani 1 1 d . . . O14W O 0.0272(3) 0.6986(2) 0.7007(3) 0.0577(19) Uani 1 1 d . . . O1 O 0.71407(19) 0.84481(16) 0.3969(2) 0.0317(13) Uani 1 1 d . . . O2 O 0.71634(18) 0.75738(16) 0.3393(2) 0.0284(12) Uani 1 1 d . . . O3 O 0.63016(19) 0.70740(17) 0.3580(2) 0.0297(13) Uani 1 1 d . . . O4 O 0.57133(19) 0.76757(18) 0.4235(2) 0.0338(13) Uani 1 1 d . . . O5 O 0.6209(2) 0.85381(17) 0.4431(2) 0.0338(13) Uani 1 1 d . . . O6 O 0.74085(19) 0.63572(18) 0.6035(2) 0.0362(14) Uani 1 1 d . . . O7 O 0.82813(19) 0.68886(17) 0.5874(2) 0.0310(13) Uani 1 1 d . . . O8 O 0.7304(2) 0.80062(18) 0.7052(2) 0.0363(14) Uani 1 1 d . . . O9 O 0.6743(2) 0.70197(18) 0.6808(3) 0.0404(15) Uani 1 1 d . . . O10 O 0.8345(2) 0.79282(17) 0.6521(2) 0.0344(14) Uani 1 1 d . . . O11 O 0.28095(19) 0.70213(16) 1.0586(2) 0.0291(13) Uani 1 1 d . . . O12 O 0.33926(19) 0.76250(17) 0.9954(2) 0.0287(12) Uani 1 1 d U . . O13 O 0.28720(19) 0.84798(17) 0.9769(2) 0.0291(12) Uani 1 1 d . . . O14 O 0.1952(2) 0.83955(17) 1.0219(2) 0.0334(13) Uani 1 1 d . . . O15 O 0.2387(2) 0.69786(18) 0.7347(2) 0.0416(15) Uani 1 1 d . . . O16 O 0.1819(2) 0.79823(18) 0.7102(2) 0.0361(14) Uani 1 1 d . . . O17 O 0.0770(2) 0.78729(17) 0.7640(3) 0.0372(14) Uani 1 1 d . . . O18 O 0.17152(18) 0.63364(17) 0.8104(2) 0.0300(13) Uani 1 1 d . . . O19 O 0.0817(2) 0.68498(17) 0.8285(2) 0.0345(14) Uani 1 1 d . . . O20 O 0.19354(18) 0.75106(16) 1.0770(2) 0.0252(12) Uani 1 1 d . . . N1 N 0.7618(2) 0.6908(2) 0.3793(3) 0.0256(14) Uani 1 1 d . . . N2 N 0.8026(2) 0.7584(2) 0.3932(3) 0.0281(15) Uani 1 1 d . . . N3 N 0.7994(2) 0.83400(19) 0.4426(3) 0.0273(15) Uani 1 1 d . . . N4 N 0.7520(2) 0.8812(2) 0.4907(3) 0.0299(15) Uani 1 1 d . . . N5 N 0.6727(2) 0.8892(2) 0.5312(3) 0.0290(15) Uani 1 1 d . . . N6 N 0.8435(2) 0.8053(2) 0.5471(3) 0.0367(16) Uani 1 1 d U . . N7 N 0.6032(2) 0.8483(2) 0.5466(3) 0.0335(16) Uani 1 1 d . . . N8 N 0.5608(2) 0.7748(2) 0.5289(3) 0.0270(15) Uani 1 1 d . . . N9 N 0.5655(2) 0.7052(2) 0.4896(3) 0.0303(15) Uani 1 1 d . . . N10 N 0.6138(2) 0.6525(2) 0.4323(3) 0.0301(15) Uani 1 1 d . . . N11 N 0.6853(2) 0.6456(2) 0.3907(3) 0.0246(14) Uani 1 1 d . . . N12 N 0.8090(2) 0.6611(2) 0.4808(3) 0.0268(15) Uani 1 1 d . . . N13 N 0.8427(2) 0.73176(19) 0.5002(3) 0.0219(14) Uani 1 1 d . . . N14 N 0.8003(2) 0.8585(2) 0.5974(3) 0.0313(16) Uani 1 1 d . . . N15 N 0.7190(2) 0.8638(2) 0.6366(3) 0.0320(16) Uani 1 1 d . . . N16 N 0.6500(2) 0.8232(2) 0.6519(3) 0.0327(16) Uani 1 1 d . . . N17 N 0.6068(2) 0.74805(18) 0.6342(3) 0.0229(14) Uani 1 1 d . . . N18 N 0.6109(2) 0.6773(2) 0.5943(3) 0.0275(15) Uani 1 1 d . . . N19 N 0.6613(2) 0.6272(2) 0.5366(3) 0.0325(16) Uani 1 1 d . . . N20 N 0.7338(2) 0.6196(2) 0.4957(3) 0.0298(15) Uani 1 1 d . . . N21 N 0.0656(2) 0.7263(2) 0.9157(3) 0.0231(14) Uani 1 1 d . . . N22 N 0.1007(2) 0.6553(2) 0.9341(3) 0.0290(15) Uani 1 1 d . . . N23 N 0.1787(2) 0.61522(19) 0.9196(3) 0.0244(14) Uani 1 1 d . . . N24 N 0.3014(2) 0.6744(2) 0.8218(3) 0.0285(15) Uani 1 1 d . . . N25 N 0.3052(2) 0.7462(2) 0.7827(3) 0.0332(16) Uani 1 1 d . . . N26 N 0.2253(2) 0.64066(18) 1.0241(3) 0.0234(14) Uani 1 1 d . . . N27 N 0.2619(2) 0.8215(2) 0.7663(3) 0.0270(15) Uani 1 1 d . . . N28 N 0.1920(2) 0.8597(2) 0.7810(3) 0.0309(16) Uani 1 1 d . . . N29 N 0.1108(2) 0.8523(2) 0.8213(3) 0.0287(15) Uani 1 1 d U . . N30 N 0.0654(3) 0.8042(2) 0.8674(3) 0.0335(17) Uani 1 1 d . . . N31 N 0.1111(2) 0.8277(2) 0.9765(3) 0.0286(15) Uani 1 1 d U . . N32 N 0.1571(2) 0.8761(2) 0.9267(3) 0.0299(15) Uani 1 1 d . . . N33 N 0.2369(2) 0.8847(2) 0.8880(3) 0.0276(15) Uani 1 1 d . . . N34 N 0.3064(2) 0.8442(2) 0.8732(3) 0.0273(15) Uani 1 1 d . . . N35 N 0.3513(2) 0.7713(2) 0.8893(3) 0.0294(15) Uani 1 1 d . . . N36 N 0.3448(2) 0.7002(2) 0.9278(3) 0.0272(15) Uani 1 1 d . . . N37 N 0.2975(2) 0.64775(18) 0.9837(3) 0.0222(13) Uani 1 1 d . . . N38 N 0.2515(2) 0.62413(19) 0.8783(3) 0.0238(11) Uani 1 1 d U . . N39 N 0.1492(2) 0.68507(19) 1.0366(3) 0.0241(14) Uani 1 1 d . . . N40 N 0.1083(2) 0.7517(2) 1.0240(3) 0.0251(14) Uani 1 1 d . . . C1 C 0.6311(3) 0.8624(3) 0.5023(4) 0.035(2) Uani 1 1 d . . . C2 C 0.7527(3) 0.8516(2) 0.4402(4) 0.0273(18) Uani 1 1 d . . . C3 C 0.7562(3) 0.7374(3) 0.3677(3) 0.0273(18) Uani 1 1 d . . . C4 C 0.6418(3) 0.6721(3) 0.3924(4) 0.0292(18) Uani 1 1 d . . . C5 C 0.5670(3) 0.7505(3) 0.4774(4) 0.0279(18) Uani 1 1 d . . . C6 C 0.7025(3) 0.8261(3) 0.6683(4) 0.0301(19) Uani 1 1 d . . . C7 C 0.8269(3) 0.6944(3) 0.5278(4) 0.0273(18) Uani 1 1 d . . . C8 C 0.7135(3) 0.6282(2) 0.5495(4) 0.0290(18) Uani 1 1 d . . . C9 C 0.6299(3) 0.6318(3) 0.5889(3) 0.0325(19) Uani 1 1 d . . . H9A H 0.6008 0.6106 0.5798 0.039 Uiso 1 1 calc R . . H9B H 0.6511 0.6230 0.6303 0.039 Uiso 1 1 calc R . . C10 C 0.6349(3) 0.7090(3) 0.6395(4) 0.0325(19) Uani 1 1 d . . . C11 C 0.6212(3) 0.7879(2) 0.6784(3) 0.0299(18) Uani 1 1 d . . . H11A H 0.5899 0.8015 0.6883 0.036 Uiso 1 1 calc R . . H11B H 0.6418 0.7767 0.7189 0.036 Uiso 1 1 calc R . . C12 C 0.7740(3) 0.8764(3) 0.6465(4) 0.0288(18) Uani 1 1 d . . . H12A H 0.7769 0.9099 0.6472 0.035 Uiso 1 1 calc R . . H12B H 0.7912 0.8650 0.6887 0.035 Uiso 1 1 calc R . . C13 C 0.7875(3) 0.6178(3) 0.4939(4) 0.0330(19) Uani 1 1 d . . . H13A H 0.8061 0.6064 0.5355 0.040 Uiso 1 1 calc R . . H13B H 0.7928 0.5958 0.4607 0.040 Uiso 1 1 calc R . . C14 C 0.8750(3) 0.7677(3) 0.5387(4) 0.034(2) Uani 1 1 d U . . H14A H 0.8911 0.7552 0.5808 0.041 Uiso 1 1 calc R . . H14B H 0.9021 0.7776 0.5162 0.041 Uiso 1 1 calc R . . C15 C 0.7086(3) 0.9096(3) 0.4952(4) 0.0310(19) Uani 1 1 d . . . H15A H 0.6902 0.9166 0.4515 0.037 Uiso 1 1 calc R . . H15B H 0.7210 0.9386 0.5157 0.037 Uiso 1 1 calc R . . C16 C 0.8111(3) 0.8078(2) 0.3872(3) 0.0253(17) Uani 1 1 d . . . H16A H 0.7894 0.8191 0.3474 0.030 Uiso 1 1 calc R . . H16B H 0.8470 0.8131 0.3839 0.030 Uiso 1 1 calc R . . C17 C 0.7212(3) 0.6581(2) 0.3498(3) 0.0259(17) Uani 1 1 d . . . H17A H 0.7021 0.6717 0.3100 0.031 Uiso 1 1 calc R . . H17B H 0.7377 0.6302 0.3379 0.031 Uiso 1 1 calc R . . C18 C 0.5640(3) 0.6700(2) 0.4381(3) 0.0280(18) Uani 1 1 d . . . H18A H 0.5426 0.6443 0.4471 0.034 Uiso 1 1 calc R . . H18B H 0.5477 0.6835 0.3968 0.034 Uiso 1 1 calc R . . C19 C 0.5557(3) 0.8238(3) 0.5265(4) 0.033(2) Uani 1 1 d . . . H19A H 0.5317 0.8330 0.5541 0.040 Uiso 1 1 calc R . . H19B H 0.5408 0.8328 0.4822 0.040 Uiso 1 1 calc R . . C20 C 0.8261(3) 0.8174(2) 0.6005(4) 0.0316(19) Uani 1 1 d U . . C21 C 0.6258(3) 0.8622(3) 0.6116(4) 0.0495(14) Uani 1 1 d . . . C22 C 0.6754(3) 0.8915(2) 0.6011(4) 0.0278(18) Uani 1 1 d . . . C23 C 0.8016(3) 0.8814(2) 0.5352(3) 0.0254(17) Uani 1 1 d . . . C24 C 0.8367(2) 0.8462(3) 0.5022(3) 0.0265(17) Uani 1 1 d . . . C25 C 0.8404(2) 0.7263(2) 0.4295(3) 0.0224(16) Uani 1 1 d . . . C26 C 0.8128(3) 0.6778(2) 0.4164(3) 0.0252(17) Uani 1 1 d . . . C27 C 0.6915(3) 0.6091(3) 0.4393(4) 0.035(2) Uani 1 1 d . . . C28 C 0.6412(3) 0.6139(2) 0.4693(4) 0.0291(18) Uani 1 1 d . . . C29 C 0.5620(3) 0.6958(3) 0.5560(4) 0.0307(19) Uani 1 1 d . . . C30 C 0.5580(3) 0.7451(3) 0.5857(3) 0.0286(18) Uani 1 1 d . . . C31 C 0.5904(3) 0.8922(3) 0.6445(4) 0.0495(14) Uani 1 1 d U . . H31A H 0.5764 0.9171 0.6152 0.059 Uiso 1 1 calc R . . H31B H 0.5616 0.8735 0.6526 0.059 Uiso 1 1 calc R . . C32 C 0.6758(3) 0.9405(3) 0.6268(4) 0.047(2) Uani 1 1 d U . . H32A H 0.7093 0.9547 0.6269 0.056 Uiso 1 1 calc R . . H32B H 0.6495 0.9588 0.5991 0.056 Uiso 1 1 calc R . . C33 C 0.8259(3) 0.9294(3) 0.5413(4) 0.046(2) Uani 1 1 d . . . H33A H 0.8064 0.9494 0.5651 0.056 Uiso 1 1 calc R . . H33B H 0.8242 0.9425 0.4982 0.056 Uiso 1 1 calc R . . C34 C 0.8844(3) 0.8690(3) 0.4878(4) 0.036(2) Uani 1 1 d . . . H34A H 0.8746 0.8922 0.4542 0.043 Uiso 1 1 calc R . . H34B H 0.9058 0.8461 0.4718 0.043 Uiso 1 1 calc R . . C35 C 0.8922(3) 0.7284(3) 0.4075(3) 0.0279(18) Uani 1 1 d . . . H35A H 0.9166 0.7080 0.4344 0.034 Uiso 1 1 calc R . . H35B H 0.9057 0.7597 0.4129 0.034 Uiso 1 1 calc R . . C36 C 0.8430(3) 0.6464(3) 0.3798(4) 0.037(2) Uani 1 1 d . . . H36A H 0.8229 0.6186 0.3667 0.044 Uiso 1 1 calc R . . H36B H 0.8749 0.6372 0.4083 0.044 Uiso 1 1 calc R . . C37 C 0.6971(3) 0.5615(3) 0.4116(4) 0.043(2) Uani 1 1 d . . . H37A H 0.7026 0.5388 0.4465 0.052 Uiso 1 1 calc R . . H37B H 0.7270 0.5609 0.3907 0.052 Uiso 1 1 calc R . . C38 C 0.6090(3) 0.5693(2) 0.4645(4) 0.040(2) Uani 1 1 d . . . H38A H 0.6275 0.5456 0.4925 0.048 Uiso 1 1 calc R . . H38B H 0.5763 0.5751 0.4781 0.048 Uiso 1 1 calc R . . C39 C 0.5158(3) 0.6659(3) 0.5634(4) 0.036(2) Uani 1 1 d . . . H39A H 0.5177 0.6367 0.5410 0.044 Uiso 1 1 calc R . . H39B H 0.5174 0.6592 0.6092 0.044 Uiso 1 1 calc R . . C40 C 0.5104(3) 0.7523(3) 0.6138(4) 0.037(2) Uani 1 1 d . . . H40A H 0.5077 0.7847 0.6252 0.044 Uiso 1 1 calc R . . H40B H 0.5126 0.7340 0.6531 0.044 Uiso 1 1 calc R . . C41 C 0.4623(3) 0.7379(3) 0.5640(4) 0.042(2) Uani 1 1 d . . . H41A H 0.4322 0.7398 0.5845 0.050 Uiso 1 1 calc R . . H41B H 0.4572 0.7599 0.5282 0.050 Uiso 1 1 calc R . . C42 C 0.4649(3) 0.6893(3) 0.5363(4) 0.045(2) Uani 1 1 d . . . H42A H 0.4368 0.6708 0.5467 0.054 Uiso 1 1 calc R . . H42B H 0.4606 0.6911 0.4893 0.054 Uiso 1 1 calc R . . C43 C 0.5993(4) 0.5532(3) 0.3939(5) 0.068(3) Uani 1 1 d . . . H43A H 0.5755 0.5748 0.3681 0.082 Uiso 1 1 calc R . . H43B H 0.5824 0.5232 0.3913 0.082 Uiso 1 1 calc R . . C44 C 0.6489(4) 0.5491(3) 0.3625(5) 0.072(3) Uani 1 1 d . . . H44A H 0.6519 0.5176 0.3473 0.087 Uiso 1 1 calc R . . H44B H 0.6456 0.5697 0.3253 0.087 Uiso 1 1 calc R . . C45 C 0.8558(3) 0.6701(3) 0.3194(4) 0.038(2) Uani 1 1 d . . . H45A H 0.8754 0.6489 0.2975 0.045 Uiso 1 1 calc R . . H45B H 0.8238 0.6774 0.2896 0.045 Uiso 1 1 calc R . . C46 C 0.8865(3) 0.7140(3) 0.3360(3) 0.040(2) Uani 1 1 d . . . H46A H 0.8697 0.7389 0.3087 0.048 Uiso 1 1 calc R . . H46B H 0.9207 0.7097 0.3261 0.048 Uiso 1 1 calc R . . C47 C 0.9150(4) 0.8918(4) 0.5483(5) 0.072(3) Uani 1 1 d . . . H47A H 0.9453 0.9069 0.5376 0.086 Uiso 1 1 calc R . . H47B H 0.9269 0.8682 0.5808 0.086 Uiso 1 1 calc R . . C48 C 0.8823(4) 0.9276(4) 0.5767(5) 0.064(3) Uani 1 1 d . . . H48A H 0.8832 0.9203 0.6222 0.076 Uiso 1 1 calc R . . H48B H 0.8977 0.9580 0.5747 0.076 Uiso 1 1 calc R . . C49 C 0.6656(5) 0.9392(4) 0.6925(6) 0.090(4) Uani 1 1 d U . . H49A H 0.6624 0.9710 0.7064 0.108 Uiso 1 1 calc R . . H49B H 0.6959 0.9262 0.7205 0.108 Uiso 1 1 calc R . . C50 C 0.6170(3) 0.9119(3) 0.7054(4) 0.0495(14) Uani 1 1 d U . . H50A H 0.6278 0.8874 0.7369 0.059 Uiso 1 1 calc R . . H50B H 0.5940 0.9326 0.7228 0.059 Uiso 1 1 calc R . . C51 C 0.1575(3) 0.8476(3) 0.9768(4) 0.0281(18) Uani 1 1 d . . . C52 C 0.1990(3) 0.9046(2) 0.9224(4) 0.0328(19) Uani 1 1 d . . . H52A H 0.2164 0.9126 0.9662 0.039 Uiso 1 1 calc R . . H52B H 0.1859 0.9330 0.9006 0.039 Uiso 1 1 calc R . . C53 C 0.2776(3) 0.8574(2) 0.9156(4) 0.0311(19) Uani 1 1 d . . . C54 C 0.3556(3) 0.8218(2) 0.8916(4) 0.0280(18) Uani 1 1 d . . . H54A H 0.3714 0.8313 0.9354 0.034 Uiso 1 1 calc R . . H54B H 0.3782 0.8318 0.8625 0.034 Uiso 1 1 calc R . . C55 C 0.3440(3) 0.7468(3) 0.9423(4) 0.0270(17) Uani 1 1 d U . . C56 C 0.3466(3) 0.6657(2) 0.9781(3) 0.0251(17) Uani 1 1 d . . . H56A H 0.3684 0.6403 0.9692 0.030 Uiso 1 1 calc R . . H56B H 0.3626 0.6792 1.0195 0.030 Uiso 1 1 calc R . . C57 C 0.2694(3) 0.6679(2) 1.0253(3) 0.0229(17) Uani 1 1 d . . . C58 C 0.0997(3) 0.8018(2) 1.0288(4) 0.0282(18) Uani 1 1 d . . . H58A H 0.0637 0.8070 1.0315 0.034 Uiso 1 1 calc R . . H58B H 0.1209 0.8132 1.0688 0.034 Uiso 1 1 calc R . . C59 C 0.1531(3) 0.7320(2) 1.0481(3) 0.0238(17) Uani 1 1 d . . . C60 C 0.1883(3) 0.6534(2) 1.0658(3) 0.0249(17) Uani 1 1 d . . . H60A H 0.1718 0.6254 1.0775 0.030 Uiso 1 1 calc R . . H60B H 0.2074 0.6670 1.1057 0.030 Uiso 1 1 calc R . . C61 C 0.0828(3) 0.6896(2) 0.8876(4) 0.0244(17) Uani 1 1 d . . . C62 C 0.0355(3) 0.7623(2) 0.8766(4) 0.0257(17) Uani 1 1 d . . . H62A H 0.0069 0.7711 0.8972 0.031 Uiso 1 1 calc R . . H62B H 0.0209 0.7495 0.8341 0.031 Uiso 1 1 calc R . . C63 C 0.0842(3) 0.8125(3) 0.8120(4) 0.0284(18) Uani 1 1 d . . . C64 C 0.1370(3) 0.8705(3) 0.7712(4) 0.0309(19) Uani 1 1 d . . . H64A H 0.1201 0.8580 0.7294 0.037 Uiso 1 1 calc R . . H64B H 0.1328 0.9039 0.7693 0.037 Uiso 1 1 calc R . . C65 C 0.2098(3) 0.8228(3) 0.7488(4) 0.0305(19) Uani 1 1 d . . . C66 C 0.2912(3) 0.7847(2) 0.7392(4) 0.0323(19) Uani 1 1 d . . . H66A H 0.2703 0.7733 0.6989 0.039 Uiso 1 1 calc R . . H66B H 0.3224 0.7981 0.7288 0.039 Uiso 1 1 calc R . . C67 C 0.0322(4) 0.9077(3) 0.9648(4) 0.0561(15) Uani 1 1 d U . . H67A H 0.0485 0.9009 1.0095 0.067 Uiso 1 1 calc R . . H67B H -0.0006 0.9231 0.9652 0.067 Uiso 1 1 calc R . . C68 C 0.2778(3) 0.7056(2) 0.7758(3) 0.0262(17) Uani 1 1 d . . . C69 C 0.1984(3) 0.6258(2) 0.8649(3) 0.0250(17) Uani 1 1 d . . . C70 C 0.1230(3) 0.6129(3) 0.9207(4) 0.033(2) Uani 1 1 d . . . H70A H 0.1050 0.6017 0.8787 0.040 Uiso 1 1 calc R . . H70B H 0.1177 0.5904 0.9533 0.040 Uiso 1 1 calc R . . C71 C 0.0709(3) 0.7202(2) 0.9873(3) 0.0278(18) Uani 1 1 d . . . C72 C 0.0985(3) 0.6721(2) 1.0004(3) 0.0247(17) Uani 1 1 d . . . C73 C 0.2202(3) 0.6050(2) 0.9755(3) 0.0239(17) Uani 1 1 d . . . C74 C 0.2719(3) 0.6106(2) 0.9453(3) 0.0258(17) Uani 1 1 d U . . C75 C 0.3492(3) 0.6921(3) 0.8597(4) 0.0300(19) Uani 1 1 d . . . C76 C 0.3528(3) 0.7420(2) 0.8323(3) 0.0254(17) Uani 1 1 d . . . C77 C 0.2821(3) 0.8593(3) 0.8061(3) 0.0323(19) Uani 1 1 d . . . C78 C 0.2339(3) 0.8860(3) 0.8160(4) 0.0299(19) Uani 1 1 d . . . C79 C 0.1084(4) 0.8762(3) 0.8814(4) 0.0518(14) Uani 1 1 d U . . C80 C 0.0739(4) 0.8414(3) 0.9156(5) 0.0561(15) Uani 1 1 d U . . C81 C 0.0229(4) 0.8629(3) 0.9260(5) 0.0561(15) Uani 1 1 d . . . H81A H 0.0010 0.8692 0.8841 0.067 Uiso 1 1 calc R . . H81B H 0.0049 0.8410 0.9490 0.067 Uiso 1 1 calc R . . C82 C 0.0811(4) 0.9238(3) 0.8716(4) 0.0518(14) Uani 1 1 d . . . H82A H 0.1030 0.9454 0.8538 0.062 Uiso 1 1 calc R . . H82B H 0.0489 0.9206 0.8404 0.062 Uiso 1 1 calc R . . C83 C 0.2354(3) 0.9368(3) 0.7911(4) 0.044(2) Uani 1 1 d . . . H83A H 0.2026 0.9519 0.7921 0.053 Uiso 1 1 calc R . . H83B H 0.2626 0.9539 0.8192 0.053 Uiso 1 1 calc R . . C84 C 0.3219(3) 0.8876(3) 0.7779(4) 0.036(2) Uani 1 1 d . . . H84A H 0.3489 0.8674 0.7681 0.043 Uiso 1 1 calc R . . H84B H 0.3378 0.9105 0.8093 0.043 Uiso 1 1 calc R . . C85 C 0.4026(3) 0.7496(3) 0.8041(4) 0.0323(19) Uani 1 1 d . . . H85A H 0.4008 0.7312 0.7650 0.039 Uiso 1 1 calc R . . H85B H 0.4051 0.7820 0.7924 0.039 Uiso 1 1 calc R . . C86 C 0.3973(3) 0.6626(3) 0.8550(4) 0.034(2) Uani 1 1 d . . . H86A H 0.3959 0.6337 0.8783 0.041 Uiso 1 1 calc R . . H86B H 0.3971 0.6553 0.8097 0.041 Uiso 1 1 calc R . . C87 C 0.3024(3) 0.5655(3) 0.9492(4) 0.037(2) Uani 1 1 d . . . H87A H 0.3358 0.5710 0.9375 0.044 Uiso 1 1 calc R . . H87B H 0.2837 0.5431 0.9189 0.044 Uiso 1 1 calc R . . C88 C 0.2141(3) 0.5562(2) 1.0028(3) 0.0319(19) Uani 1 1 d . . . H88A H 0.1849 0.5561 1.0251 0.038 Uiso 1 1 calc R . . H88B H 0.2066 0.5343 0.9670 0.038 Uiso 1 1 calc R . . C89 C 0.0690(3) 0.6394(3) 1.0359(4) 0.037(2) Uani 1 1 d . . . H89A H 0.0895 0.6117 1.0478 0.044 Uiso 1 1 calc R . . H89B H 0.0371 0.6303 1.0071 0.044 Uiso 1 1 calc R . . C90 C 0.0179(3) 0.7213(3) 1.0085(4) 0.0327(19) Uani 1 1 d . . . H90A H -0.0060 0.7006 0.9813 0.039 Uiso 1 1 calc R . . H90B H 0.0036 0.7524 1.0034 0.039 Uiso 1 1 calc R . . C91 C 0.0248(3) 0.7063(3) 1.0806(4) 0.043(2) Uani 1 1 d . . . H91A H 0.0418 0.7310 1.1079 0.051 Uiso 1 1 calc R . . H91B H -0.0092 0.7019 1.0914 0.051 Uiso 1 1 calc R . . C92 C 0.0563(4) 0.6614(3) 1.0967(4) 0.050(3) Uani 1 1 d . . . H92A H 0.0882 0.6684 1.1269 0.060 Uiso 1 1 calc R . . H92B H 0.0366 0.6397 1.1177 0.060 Uiso 1 1 calc R . . C93 C 0.2618(3) 0.5410(3) 1.0490(4) 0.044(2) Uani 1 1 d . . . H93A H 0.2579 0.5088 1.0606 0.053 Uiso 1 1 calc R . . H93B H 0.2654 0.5593 1.0885 0.053 Uiso 1 1 calc R . . C94 C 0.3101(4) 0.5460(3) 1.0210(4) 0.050(3) Uani 1 1 d . . . H94A H 0.3265 0.5158 1.0219 0.060 Uiso 1 1 calc R . . H94B H 0.3338 0.5663 1.0492 0.060 Uiso 1 1 calc R . . C95 C 0.4466(3) 0.6880(3) 0.8832(4) 0.042(2) Uani 1 1 d . . . H95A H 0.4758 0.6693 0.8764 0.050 Uiso 1 1 calc R . . H95B H 0.4488 0.6910 0.9299 0.050 Uiso 1 1 calc R . . C96 C 0.4514(3) 0.7358(3) 0.8546(4) 0.051(3) Uani 1 1 d . . . H96A H 0.4814 0.7364 0.8338 0.062 Uiso 1 1 calc R . . H96B H 0.4570 0.7584 0.8896 0.062 Uiso 1 1 calc R . . C97 C 0.2935(4) 0.9120(3) 0.7146(4) 0.061(3) Uani 1 1 d . . . H97A H 0.3170 0.9341 0.7007 0.073 Uiso 1 1 calc R . . H97B H 0.2848 0.8890 0.6805 0.073 Uiso 1 1 calc R . . C98 C 0.2452(4) 0.9366(3) 0.7226(4) 0.050(3) Uani 1 1 d . . . H98A H 0.2160 0.9221 0.6944 0.060 Uiso 1 1 calc R . . H98B H 0.2472 0.9684 0.7083 0.060 Uiso 1 1 calc R . . C99 C 0.0703(4) 0.9419(3) 0.9309(4) 0.0518(14) Uani 1 1 d U . . H99A H 0.0539 0.9720 0.9225 0.062 Uiso 1 1 calc R . . H99B H 0.1028 0.9464 0.9614 0.062 Uiso 1 1 calc R . . C100 C 0.2801(3) 0.6274(2) 0.8285(4) 0.0320(19) Uani 1 1 d . . . H10A H 0.2580 0.6189 0.7876 0.038 Uiso 1 1 calc R . . H10B H 0.3085 0.6055 0.8369 0.038 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Er1 0.02179(17) 0.0375(2) 0.02040(18) 0.00449(15) 0.00427(14) 0.00093(14) Er2 0.02972(19) 0.0371(2) 0.02082(19) 0.00442(15) 0.00474(15) 0.00223(15) Er3 0.02821(18) 0.0385(2) 0.02112(19) -0.00376(15) 0.00309(15) -0.00013(15) Er4 0.02497(17) 0.03365(19) 0.01801(17) -0.00261(15) 0.00520(14) -0.00150(14) Cl1 0.0348(11) 0.0505(13) 0.0271(11) 0.0108(9) 0.0015(9) 0.0002(9) Cl2 0.115(3) 0.139(3) 0.108(3) -0.003(2) 0.009(2) -0.004(3) Cl3 0.101(3) 0.150(3) 0.121(3) -0.009(3) 0.025(2) 0.001(3) Cl4 0.0376(11) 0.0502(12) 0.0227(10) -0.0082(9) 0.0022(9) -0.0023(9) O1W 0.041(3) 0.056(4) 0.038(3) 0.018(3) -0.005(3) -0.011(3) O2W 0.043(3) 0.045(3) 0.023(3) 0.012(2) -0.002(3) -0.005(3) O3W 0.055(4) 0.035(3) 0.046(4) 0.003(3) 0.011(3) 0.008(3) O4W 0.051(4) 0.044(4) 0.064(4) -0.013(3) -0.001(3) -0.001(3) O5W 0.039(4) 0.064(4) 0.057(4) 0.008(3) 0.003(3) -0.017(3) O6W 0.049(4) 0.072(4) 0.061(4) 0.017(3) 0.020(3) 0.035(3) O7W 0.035(3) 0.047(3) 0.034(3) -0.001(3) 0.007(3) 0.009(3) O8W 0.046(4) 0.059(4) 0.048(4) -0.011(3) 0.000(3) 0.004(3) O9W 0.062(4) 0.063(4) 0.089(5) -0.022(4) 0.048(4) -0.020(3) O10W 0.054(4) 0.044(4) 0.085(5) -0.008(3) -0.014(4) 0.001(3) O11W 0.037(3) 0.093(5) 0.042(4) -0.010(3) 0.015(3) 0.000(3) O12W 0.060(4) 0.041(4) 0.067(4) -0.003(3) 0.024(3) -0.012(3) O13W 0.057(4) 0.050(4) 0.035(4) -0.010(3) -0.003(3) 0.013(3) O14W 0.064(4) 0.061(4) 0.045(4) 0.003(3) 0.002(3) 0.025(3) O1 0.031(3) 0.032(3) 0.033(3) 0.004(2) 0.006(2) 0.004(2) O2 0.020(3) 0.038(3) 0.025(3) 0.006(2) -0.001(2) -0.001(2) O3 0.027(3) 0.048(3) 0.015(3) 0.012(2) 0.005(2) 0.005(2) O4 0.031(3) 0.049(3) 0.023(3) 0.003(2) 0.007(2) -0.005(2) O5 0.031(3) 0.045(3) 0.025(3) 0.007(2) 0.005(2) -0.004(2) O6 0.025(3) 0.057(4) 0.026(3) 0.009(3) 0.003(2) -0.002(2) O7 0.034(3) 0.041(3) 0.022(3) 0.004(2) 0.015(2) 0.003(2) O8 0.036(3) 0.042(3) 0.031(3) 0.007(3) 0.006(3) 0.002(3) O9 0.026(3) 0.048(3) 0.042(4) -0.005(3) -0.005(3) 0.007(2) O10 0.044(3) 0.042(3) 0.019(3) -0.004(2) 0.011(2) -0.001(3) O11 0.029(3) 0.035(3) 0.024(3) -0.012(2) 0.006(2) -0.006(2) O12 0.029(3) 0.046(3) 0.013(3) 0.001(2) 0.011(2) 0.002(2) O13 0.032(3) 0.039(3) 0.018(3) -0.004(2) 0.007(2) -0.003(2) O14 0.033(3) 0.040(3) 0.027(3) -0.002(2) 0.004(2) 0.004(2) O15 0.045(4) 0.048(3) 0.026(3) 0.003(3) -0.007(3) -0.008(3) O16 0.029(3) 0.047(3) 0.030(3) -0.013(3) 0.002(2) -0.007(2) O17 0.046(3) 0.035(3) 0.033(3) -0.004(2) 0.015(3) -0.003(3) O18 0.023(3) 0.049(3) 0.019(3) 0.000(2) 0.005(2) 0.006(2) O19 0.047(3) 0.033(3) 0.023(3) 0.002(2) 0.005(3) 0.008(2) O20 0.023(3) 0.038(3) 0.015(3) -0.007(2) 0.004(2) -0.003(2) N1 0.027(3) 0.038(4) 0.014(3) 0.003(3) 0.007(3) -0.003(3) N2 0.030(3) 0.031(4) 0.022(3) 0.000(3) 0.001(3) 0.001(3) N3 0.032(3) 0.027(3) 0.026(4) -0.003(3) 0.013(3) -0.003(3) N4 0.031(3) 0.032(4) 0.028(4) 0.005(3) 0.009(3) 0.006(3) N5 0.032(4) 0.033(4) 0.024(3) 0.000(3) 0.008(3) -0.001(3) N6 0.039(3) 0.062(3) 0.009(3) 0.006(2) 0.004(2) 0.035(3) N7 0.034(4) 0.046(4) 0.022(4) 0.001(3) 0.012(3) -0.004(3) N8 0.030(3) 0.031(3) 0.022(3) 0.002(3) 0.010(3) 0.002(3) N9 0.029(3) 0.040(4) 0.026(4) -0.003(3) 0.016(3) -0.008(3) N10 0.026(3) 0.037(4) 0.027(4) -0.001(3) 0.004(3) 0.000(3) N11 0.016(3) 0.037(4) 0.024(3) 0.007(3) 0.014(2) 0.001(3) N12 0.032(3) 0.030(3) 0.017(3) 0.001(3) 0.002(3) -0.009(3) N13 0.022(3) 0.025(3) 0.019(3) 0.005(3) 0.003(2) -0.001(2) N14 0.028(3) 0.031(4) 0.036(4) 0.000(3) 0.007(3) 0.002(3) N15 0.017(3) 0.045(4) 0.036(4) -0.006(3) 0.008(3) 0.001(3) N16 0.029(3) 0.036(4) 0.033(4) -0.005(3) 0.005(3) -0.003(3) N17 0.024(3) 0.023(3) 0.023(3) 0.012(3) 0.006(3) -0.001(2) N18 0.018(3) 0.033(4) 0.032(4) 0.002(3) 0.004(3) 0.002(3) N19 0.037(4) 0.038(4) 0.023(4) -0.007(3) 0.006(3) -0.012(3) N20 0.027(3) 0.041(4) 0.023(4) -0.003(3) 0.008(3) 0.006(3) N21 0.024(3) 0.037(4) 0.010(3) 0.000(3) 0.007(2) 0.005(3) N22 0.038(4) 0.033(4) 0.016(3) -0.003(3) 0.005(3) 0.002(3) N23 0.023(3) 0.025(3) 0.024(3) -0.002(3) 0.002(3) 0.002(2) N24 0.034(4) 0.029(3) 0.023(3) 0.001(3) 0.006(3) -0.002(3) N25 0.032(4) 0.042(4) 0.024(4) 0.008(3) 0.002(3) -0.009(3) N26 0.040(4) 0.020(3) 0.009(3) -0.002(2) 0.001(3) -0.002(3) N27 0.028(3) 0.034(4) 0.019(3) -0.004(3) 0.005(3) -0.002(3) N28 0.029(3) 0.033(4) 0.030(4) -0.010(3) 0.005(3) 0.003(3) N29 0.032(3) 0.035(4) 0.024(3) 0.003(3) 0.016(3) 0.000(3) N30 0.051(4) 0.024(3) 0.026(4) 0.005(3) 0.009(3) -0.011(3) N31 0.025(3) 0.035(4) 0.024(3) 0.000(3) -0.003(3) 0.006(3) N32 0.023(3) 0.034(4) 0.031(4) 0.001(3) 0.002(3) -0.005(3) N33 0.033(4) 0.029(3) 0.022(3) 0.006(3) 0.010(3) 0.001(3) N34 0.022(3) 0.041(4) 0.019(3) 0.007(3) 0.007(3) 0.000(3) N35 0.024(3) 0.041(4) 0.025(4) -0.001(3) 0.007(3) 0.002(3) N36 0.021(3) 0.042(4) 0.021(3) -0.001(3) 0.009(3) 0.000(3) N37 0.017(3) 0.022(3) 0.028(3) 0.001(3) 0.005(3) -0.001(2) N38 0.0239(13) 0.0249(13) 0.0236(14) 0.0003(9) 0.0067(9) 0.0010(9) N39 0.016(3) 0.024(3) 0.030(4) 0.007(3) -0.001(3) -0.003(2) N40 0.028(3) 0.037(4) 0.012(3) -0.008(3) 0.008(3) -0.009(3) C1 0.040(5) 0.032(4) 0.030(5) 0.009(4) -0.001(4) 0.000(4) C2 0.020(4) 0.030(4) 0.033(4) 0.011(3) 0.007(3) -0.002(3) C3 0.036(4) 0.034(4) 0.015(4) -0.003(3) 0.014(3) -0.007(3) C4 0.030(4) 0.032(4) 0.026(4) -0.006(3) 0.005(3) -0.008(3) C5 0.022(4) 0.044(5) 0.019(4) 0.003(4) 0.008(3) 0.000(3) C6 0.040(5) 0.027(4) 0.025(4) -0.004(3) 0.012(4) -0.003(3) C7 0.029(4) 0.034(4) 0.022(4) 0.010(3) 0.015(3) 0.007(3) C8 0.027(4) 0.022(4) 0.038(5) 0.001(3) 0.005(4) -0.004(3) C9 0.023(4) 0.054(5) 0.023(4) 0.004(4) 0.010(3) 0.000(4) C10 0.032(4) 0.036(5) 0.031(5) 0.007(4) 0.010(4) -0.003(4) C11 0.031(4) 0.038(5) 0.021(4) 0.001(3) 0.007(3) -0.003(3) C12 0.023(4) 0.033(4) 0.030(4) -0.014(3) 0.004(3) -0.004(3) C13 0.031(4) 0.032(4) 0.041(5) 0.004(4) 0.018(4) 0.008(3) C14 0.033(4) 0.034(4) 0.033(5) -0.007(4) -0.002(4) -0.011(3) C15 0.030(4) 0.037(5) 0.030(4) 0.001(3) 0.016(3) 0.006(3) C16 0.025(4) 0.033(4) 0.022(4) 0.004(3) 0.012(3) -0.009(3) C17 0.029(4) 0.028(4) 0.021(4) -0.002(3) 0.006(3) 0.000(3) C18 0.032(4) 0.031(4) 0.021(4) -0.010(3) 0.005(3) -0.002(3) C19 0.026(4) 0.049(5) 0.025(4) 0.009(4) 0.006(3) -0.002(4) C20 0.032(4) 0.022(4) 0.043(5) -0.004(4) 0.011(4) -0.015(3) C21 0.043(3) 0.062(4) 0.045(3) -0.004(3) 0.014(3) 0.008(3) C22 0.026(4) 0.032(4) 0.027(4) -0.001(3) 0.009(3) 0.006(3) C23 0.019(4) 0.034(4) 0.023(4) 0.000(3) 0.004(3) -0.005(3) C24 0.009(3) 0.049(5) 0.025(4) -0.005(3) 0.010(3) 0.001(3) C25 0.014(3) 0.038(4) 0.015(4) 0.002(3) 0.003(3) -0.002(3) C26 0.021(4) 0.042(4) 0.013(4) 0.006(3) 0.005(3) 0.001(3) C27 0.033(4) 0.031(4) 0.038(5) -0.002(4) 0.003(4) -0.004(3) C28 0.028(4) 0.028(4) 0.029(4) -0.009(3) -0.001(3) 0.002(3) C29 0.020(4) 0.049(5) 0.023(4) -0.005(4) 0.007(3) -0.007(3) C30 0.024(4) 0.041(5) 0.020(4) -0.009(3) 0.002(3) -0.001(3) C31 0.043(3) 0.062(4) 0.045(3) -0.004(3) 0.014(3) 0.008(3) C32 0.041(5) 0.040(5) 0.061(6) -0.014(4) 0.017(4) 0.006(4) C33 0.038(5) 0.036(5) 0.070(6) 0.002(4) 0.023(4) -0.005(4) C34 0.023(4) 0.045(5) 0.046(5) -0.011(4) 0.023(4) -0.011(3) C35 0.019(4) 0.045(5) 0.021(4) 0.002(3) 0.006(3) 0.003(3) C36 0.037(4) 0.043(5) 0.036(5) -0.004(4) 0.020(4) 0.011(4) C37 0.037(5) 0.034(5) 0.060(6) -0.021(4) 0.016(4) -0.003(4) C38 0.045(5) 0.024(4) 0.055(6) -0.001(4) 0.018(4) -0.006(4) C39 0.029(4) 0.049(5) 0.030(5) 0.003(4) 0.002(4) -0.003(4) C40 0.025(4) 0.053(5) 0.036(5) -0.002(4) 0.015(4) -0.006(4) C41 0.025(4) 0.052(5) 0.052(6) 0.006(4) 0.019(4) -0.013(4) C42 0.026(4) 0.070(6) 0.044(5) 0.000(5) 0.018(4) -0.010(4) C43 0.060(7) 0.061(7) 0.079(8) -0.016(6) 0.003(6) -0.001(5) C44 0.087(8) 0.064(7) 0.071(7) -0.039(5) 0.027(6) -0.041(6) C45 0.023(4) 0.054(5) 0.043(5) 0.002(4) 0.024(4) 0.005(4) C46 0.038(5) 0.067(6) 0.016(4) 0.000(4) 0.011(3) -0.009(4) C47 0.039(6) 0.104(9) 0.077(8) -0.022(6) 0.023(5) -0.015(6) C48 0.047(6) 0.077(7) 0.068(7) -0.020(6) 0.015(5) -0.004(5) C49 0.100(10) 0.085(9) 0.086(7) -0.028(7) 0.021(7) -0.019(7) C50 0.043(3) 0.062(4) 0.045(3) -0.004(3) 0.014(3) 0.008(3) C51 0.024(4) 0.034(4) 0.029(4) -0.007(3) 0.009(3) 0.004(3) C52 0.047(5) 0.025(4) 0.029(4) 0.001(3) 0.014(4) 0.002(4) C53 0.028(4) 0.026(4) 0.039(5) -0.003(4) 0.007(4) -0.017(3) C54 0.021(4) 0.035(4) 0.032(4) 0.000(3) 0.014(3) -0.008(3) C55 0.009(3) 0.042(4) 0.032(4) 0.006(3) 0.009(3) -0.001(3) C56 0.015(3) 0.035(4) 0.025(4) 0.002(3) 0.005(3) 0.003(3) C57 0.017(3) 0.036(4) 0.015(4) 0.011(3) 0.001(3) -0.009(3) C58 0.027(4) 0.030(4) 0.031(4) -0.007(3) 0.012(3) -0.001(3) C59 0.031(4) 0.029(4) 0.013(4) 0.003(3) 0.007(3) 0.002(3) C60 0.029(4) 0.036(4) 0.011(4) 0.000(3) 0.010(3) 0.000(3) C61 0.024(4) 0.028(4) 0.020(4) -0.003(3) 0.002(3) -0.005(3) C62 0.015(3) 0.032(4) 0.031(4) -0.002(3) 0.006(3) -0.003(3) C63 0.031(4) 0.035(4) 0.019(4) -0.002(3) 0.006(3) 0.006(3) C64 0.027(4) 0.036(4) 0.031(5) 0.007(4) 0.010(3) 0.004(3) C65 0.024(4) 0.042(5) 0.027(4) 0.013(4) 0.009(3) 0.000(3) C66 0.037(4) 0.034(4) 0.029(4) 0.003(4) 0.015(4) -0.011(4) C67 0.052(4) 0.064(4) 0.051(4) -0.008(3) 0.006(3) 0.012(3) C68 0.033(4) 0.032(4) 0.015(4) -0.004(3) 0.011(3) -0.003(3) C69 0.029(4) 0.025(4) 0.021(4) -0.009(3) 0.002(3) -0.001(3) C70 0.044(5) 0.031(4) 0.027(4) -0.001(3) 0.011(4) 0.000(4) C71 0.031(4) 0.035(4) 0.023(4) -0.003(3) 0.019(3) -0.004(3) C72 0.025(4) 0.033(4) 0.018(4) -0.001(3) 0.008(3) 0.002(3) C73 0.024(4) 0.027(4) 0.021(4) 0.003(3) 0.003(3) 0.002(3) C74 0.016(3) 0.034(4) 0.029(4) -0.016(3) 0.011(3) 0.006(3) C75 0.029(4) 0.029(4) 0.031(5) -0.004(3) 0.003(3) -0.002(3) C76 0.023(4) 0.034(4) 0.018(4) 0.003(3) 0.000(3) -0.002(3) C77 0.048(5) 0.038(5) 0.015(4) -0.002(3) 0.017(3) 0.000(4) C78 0.030(4) 0.035(4) 0.023(4) 0.012(3) -0.001(3) -0.006(3) C79 0.060(3) 0.055(4) 0.039(3) 0.004(3) 0.008(3) 0.006(3) C80 0.052(4) 0.064(4) 0.051(4) -0.008(3) 0.006(3) 0.012(3) C81 0.052(4) 0.064(4) 0.051(4) -0.008(3) 0.006(3) 0.012(3) C82 0.060(3) 0.055(4) 0.039(3) 0.004(3) 0.008(3) 0.006(3) C83 0.045(5) 0.035(5) 0.049(6) 0.005(4) 0.002(4) -0.003(4) C84 0.036(4) 0.040(5) 0.037(5) 0.004(4) 0.019(4) -0.007(4) C85 0.024(4) 0.041(5) 0.032(5) -0.012(4) 0.007(3) -0.006(3) C86 0.037(4) 0.043(5) 0.026(4) -0.005(4) 0.014(4) 0.014(4) C87 0.039(5) 0.035(5) 0.037(5) 0.000(4) 0.009(4) 0.004(4) C88 0.051(5) 0.026(4) 0.021(4) -0.006(3) 0.013(4) -0.003(4) C89 0.039(5) 0.040(5) 0.035(5) -0.006(4) 0.016(4) -0.003(4) C90 0.023(4) 0.043(5) 0.034(5) -0.012(4) 0.009(3) -0.015(3) C91 0.042(5) 0.066(6) 0.028(5) -0.001(4) 0.025(4) -0.009(4) C92 0.077(7) 0.057(6) 0.026(5) 0.010(4) 0.033(5) 0.005(5) C93 0.048(5) 0.048(5) 0.037(5) 0.008(4) 0.010(4) 0.001(4) C94 0.066(6) 0.034(5) 0.051(6) 0.010(4) 0.016(5) 0.015(4) C95 0.021(4) 0.074(6) 0.027(5) 0.004(4) -0.005(3) 0.005(4) C96 0.033(5) 0.070(7) 0.051(6) 0.014(5) 0.008(4) 0.002(4) C97 0.078(7) 0.053(6) 0.055(6) 0.030(5) 0.022(5) 0.011(5) C98 0.058(6) 0.048(6) 0.043(6) 0.017(4) 0.008(5) -0.005(5) C99 0.060(3) 0.055(4) 0.039(3) 0.004(3) 0.008(3) 0.006(3) C100 0.037(4) 0.031(4) 0.033(5) 0.001(3) 0.020(4) -0.002(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 Er1 O1W 2.341(5) . ? Er1 O2 2.377(5) . ? Er1 Cl2 2.378(4) . ? Er1 O4 2.388(5) . ? Er1 O1 2.396(5) . ? Er1 O3 2.422(5) . ? Er1 O5 2.446(5) . ? Er1 Cl1 2.618(2) . ? Er2 O6 2.285(5) . ? Er2 O3W 2.316(5) . ? Er2 O2W 2.335(5) . ? Er2 O4W 2.344(6) . ? Er2 O7 2.354(5) . ? Er2 O6W 2.393(6) . ? Er2 O5W 2.402(6) . ? Er2 O7W 2.424(6) . ? Er3 O12W 2.290(6) . ? Er3 O18 2.293(5) . ? Er3 O19 2.331(5) . ? Er3 O13W 2.339(5) . ? Er3 O10W 2.348(6) . ? Er3 O9W 2.362(6) . ? Er3 O11W 2.384(6) . ? Er3 O14W 2.386(6) . ? Er4 Cl3 2.354(4) . ? Er4 O8W 2.357(6) . ? Er4 O13 2.370(5) . ? Er4 O12 2.375(5) . ? Er4 O20 2.394(5) . ? Er4 O14 2.409(5) . ? Er4 O11 2.434(5) . ? Er4 Cl4 2.610(2) . ? O1 C2 1.241(8) . ? O2 C3 1.242(8) . ? O3 C4 1.251(8) . ? O4 C5 1.255(8) . ? O5 C1 1.242(9) . ? O6 C8 1.237(8) . ? O7 C7 1.251(8) . ? O8 C6 1.208(8) . ? O9 C10 1.233(8) . ? O10 C20 1.275(9) . ? O11 C57 1.214(8) . ? O12 C55 1.229(8) . ? O13 C53 1.288(9) . ? O14 C51 1.252(8) . ? O15 C68 1.228(8) . ? O16 C65 1.212(9) . ? O17 C63 1.225(8) . ? O18 C69 1.241(8) . ? O19 C61 1.237(8) . ? O20 C59 1.246(8) . ? N1 C3 1.371(9) . ? N1 C26 1.463(8) . ? N1 C17 1.468(8) . ? N2 C3 1.376(9) . ? N2 C16 1.453(8) . ? N2 C25 1.461(8) . ? N3 C2 1.322(9) . ? N3 C16 1.463(9) . ? N3 C24 1.476(8) . ? N4 C2 1.362(9) . ? N4 C15 1.422(9) . ? N4 C23 1.450(8) . ? N5 C1 1.380(9) . ? N5 C15 1.440(9) . ? N5 C22 1.452(9) . ? N6 C20 1.332(10) . ? N6 C14 1.395(9) . ? N6 C24 1.497(10) . ? N7 C1 1.350(10) . ? N7 C19 1.426(9) . ? N7 C21 1.435(10) . ? N8 C5 1.319(9) . ? N8 C19 1.419(9) . ? N8 C30 1.479(9) . ? N9 C5 1.335(9) . ? N9 C29 1.435(9) . ? N9 C18 1.475(9) . ? N10 C4 1.338(9) . ? N10 C18 1.431(9) . ? N10 C28 1.465(9) . ? N11 C4 1.382(9) . ? N11 C17 1.437(9) . ? N11 C27 1.453(9) . ? N12 C7 1.390(9) . ? N12 C13 1.419(9) . ? N12 C26 1.452(9) . ? N13 C7 1.327(9) . ? N13 C14 1.477(8) . ? N13 C25 1.478(8) . ? N14 C20 1.360(9) . ? N14 C12 1.439(9) . ? N14 C23 1.466(9) . ? N15 C6 1.388(9) . ? N15 C12 1.466(9) . ? N15 C22 1.474(9) . ? N16 C6 1.360(9) . ? N16 C11 1.442(9) . ? N16 C21 1.473(10) . ? N17 C10 1.341(9) . ? N17 C30 1.478(8) . ? N17 C11 1.478(9) . ? N18 C10 1.377(9) . ? N18 C9 1.416(9) . ? N18 C29 1.479(9) . ? N19 C8 1.346(9) . ? N19 C28 1.457(9) . ? N19 C9 1.498(9) . ? N20 C8 1.357(10) . ? N20 C13 1.421(9) . ? N20 C27 1.491(9) . ? N21 C61 1.331(9) . ? N21 C62 1.459(8) . ? N21 C71 1.488(8) . ? N22 C61 1.405(9) . ? N22 C70 1.408(9) . ? N22 C72 1.481(9) . ? N23 C69 1.377(9) . ? N23 C73 1.469(8) . ? N23 C70 1.470(9) . ? N24 C68 1.376(9) . ? N24 C75 1.445(9) . ? N24 C100 1.484(9) . ? N25 C68 1.367(9) . ? N25 C66 1.439(9) . ? N25 C76 1.470(9) . ? N26 C57 1.398(8) . ? N26 C73 1.435(8) . ? N26 C60 1.470(9) . ? N27 C65 1.350(9) . ? N27 C77 1.413(9) . ? N27 C66 1.487(9) . ? N28 C65 1.388(9) . ? N28 C78 1.420(9) . ? N28 C64 1.455(9) . ? N29 C63 1.341(9) . ? N29 C79 1.446(10) . ? N29 C64 1.455(9) . ? N30 C63 1.365(9) . ? N30 C80 1.460(11) . ? N30 C62 1.476(9) . ? N31 C51 1.349(9) . ? N31 C58 1.402(9) . ? N31 C80 1.503(10) . ? N32 C51 1.330(9) . ? N32 C52 1.391(9) . ? N32 C79 1.440(10) . ? N33 C53 1.364(9) . ? N33 C52 1.453(9) . ? N33 C78 1.494(9) . ? N34 C53 1.327(10) . ? N34 C54 1.431(9) . ? N34 C77 1.492(9) . ? N35 C55 1.358(9) . ? N35 C54 1.461(9) . ? N35 C76 1.468(9) . ? N36 C55 1.380(9) . ? N36 C56 1.443(9) . ? N36 C75 1.470(9) . ? N37 C57 1.372(9) . ? N37 C56 1.417(8) . ? N37 C74 1.428(8) . ? N38 C69 1.372(9) . ? N38 C100 1.401(9) . ? N38 C74 1.455(9) . ? N39 C59 1.376(9) . ? N39 C60 1.423(8) . ? N39 C72 1.451(8) . ? N40 C59 1.318(9) . ? N40 C71 1.446(9) . ? N40 C58 1.471(9) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C21 C31 1.527(12) . ? C21 C22 1.605(11) . ? C22 C32 1.512(10) . ? C23 C33 1.521(10) . ? C23 C24 1.613(10) . ? C24 C34 1.497(9) . ? C25 C35 1.518(9) . ? C25 C26 1.577(10) . ? C26 C36 1.507(10) . ? C27 C37 1.511(10) . ? C27 C28 1.572(11) . ? C28 C38 1.534(10) . ? C29 C39 1.521(10) . ? C29 C30 1.565(10) . ? C30 C40 1.495(10) . ? C31 C50 1.447(11) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 C49 1.449(13) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C48 1.527(11) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C47 1.514(11) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C46 1.531(10) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 C45 1.529(10) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 C44 1.515(11) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 C43 1.521(12) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 C42 1.509(11) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 C41 1.535(10) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 C42 1.526(11) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 C44 1.571(14) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C45 C46 1.507(11) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C47 C48 1.534(13) . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C49 C50 1.568(14) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C54 H54A 0.9700 . ? C54 H54B 0.9700 . ? C56 H56A 0.9700 . ? C56 H56B 0.9700 . ? C58 H58A 0.9700 . ? C58 H58B 0.9700 . ? C60 H60A 0.9700 . ? C60 H60B 0.9700 . ? C62 H62A 0.9700 . ? C62 H62B 0.9700 . ? C64 H64A 0.9700 . ? C64 H64B 0.9700 . ? C66 H66A 0.9700 . ? C66 H66B 0.9700 . ? C67 C81 1.521(12) . ? C67 C99 1.660(13) . ? C67 H67A 0.9700 . ? C67 H67B 0.9700 . ? C70 H70A 0.9700 . ? C70 H70B 0.9700 . ? C71 C90 1.542(10) . ? C71 C72 1.568(10) . ? C72 C89 1.502(10) . ? C73 C88 1.540(9) . ? C73 C74 1.610(10) . ? C74 C87 1.523(10) . ? C75 C86 1.541(10) . ? C75 C76 1.560(10) . ? C76 C85 1.552(10) . ? C77 C84 1.531(10) . ? C77 C78 1.531(11) . ? C78 C83 1.559(10) . ? C79 C82 1.546(12) . ? C79 C80 1.608(14) . ? C80 C81 1.530(13) . ? C81 H81A 0.9700 . ? C81 H81B 0.9700 . ? C82 C99 1.424(11) . ? C82 H82A 0.9700 . ? C82 H82B 0.9700 . ? C83 C98 1.503(11) . ? C83 H83A 0.9700 . ? C83 H83B 0.9700 . ? C84 C97 1.558(11) . ? C84 H84A 0.9700 . ? C84 H84B 0.9700 . ? C85 C96 1.549(10) . ? C85 H85A 0.9700 . ? C85 H85B 0.9700 . ? C86 C95 1.508(10) . ? C86 H86A 0.9700 . ? C86 H86B 0.9700 . ? C87 C94 1.581(10) . ? C87 H87A 0.9700 . ? C87 H87B 0.9700 . ? C88 C93 1.496(10) . ? C88 H88A 0.9700 . ? C88 H88B 0.9700 . ? C89 C92 1.517(11) . ? C89 H89A 0.9700 . ? C89 H89B 0.9700 . ? C90 C91 1.548(10) . ? C90 H90A 0.9700 . ? C90 H90B 0.9700 . ? C91 C92 1.538(11) . ? C91 H91A 0.9700 . ? C91 H91B 0.9700 . ? C92 H92A 0.9700 . ? C92 H92B 0.9700 . ? C93 C94 1.503(12) . ? C93 H93A 0.9700 . ? C93 H93B 0.9700 . ? C94 H94A 0.9700 . ? C94 H94B 0.9700 . ? C95 C96 1.519(12) . ? C95 H95A 0.9700 . ? C95 H95B 0.9700 . ? C96 H96A 0.9700 . ? C96 H96B 0.9700 . ? C97 C98 1.492(13) . ? C97 H97A 0.9700 . ? C97 H97B 0.9700 . ? C98 H98A 0.9700 . ? C98 H98B 0.9700 . ? C99 H99A 0.9700 . ? C99 H99B 0.9700 . ? C100 H10A 0.9700 . ? C100 H10B 0.9700 . ? 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 O1W Er1 O2 94.91(19) . . ? O1W Er1 Cl2 68.28(16) . . ? O2 Er1 Cl2 99.20(16) . . ? O1W Er1 O4 115.44(19) . . ? O2 Er1 O4 141.98(17) . . ? Cl2 Er1 O4 73.73(16) . . ? O1W Er1 O1 67.03(17) . . ? O2 Er1 O1 71.89(17) . . ? Cl2 Er1 O1 133.25(16) . . ? O4 Er1 O1 139.65(17) . . ? O1W Er1 O3 128.12(17) . . ? O2 Er1 O3 70.68(16) . . ? Cl2 Er1 O3 65.65(15) . . ? O4 Er1 O3 72.53(17) . . ? O1 Er1 O3 140.55(17) . . ? O1W Er1 O5 76.62(19) . . ? O2 Er1 O5 142.26(16) . . ? Cl2 Er1 O5 110.93(16) . . ? O4 Er1 O5 70.87(17) . . ? O1 Er1 O5 70.96(17) . . ? O3 Er1 O5 142.42(17) . . ? O1W Er1 Cl1 147.07(14) . . ? O2 Er1 Cl1 83.95(12) . . ? Cl2 Er1 Cl1 144.50(11) . . ? O4 Er1 Cl1 82.16(13) . . ? O1 Er1 Cl1 81.54(12) . . ? O3 Er1 Cl1 82.62(11) . . ? O5 Er1 Cl1 84.29(12) . . ? O6 Er2 O3W 87.22(19) . . ? O6 Er2 O2W 139.71(18) . . ? O3W Er2 O2W 105.84(19) . . ? O6 Er2 O4W 74.04(19) . . ? O3W Er2 O4W 144.8(2) . . ? O2W Er2 O4W 73.91(19) . . ? O6 Er2 O7 75.24(18) . . ? O3W Er2 O7 77.19(19) . . ? O2W Er2 O7 144.31(18) . . ? O4W Er2 O7 124.04(19) . . ? O6 Er2 O6W 106.7(2) . . ? O3W Er2 O6W 141.5(2) . . ? O2W Er2 O6W 86.7(2) . . ? O4W Er2 O6W 73.4(2) . . ? O7 Er2 O6W 72.27(19) . . ? O6 Er2 O5W 146.20(19) . . ? O3W Er2 O5W 74.9(2) . . ? O2W Er2 O5W 73.68(19) . . ? O4W Er2 O5W 134.8(2) . . ? O7 Er2 O5W 72.96(18) . . ? O6W Er2 O5W 74.1(2) . . ? O6 Er2 O7W 75.05(18) . . ? O3W Er2 O7W 70.25(19) . . ? O2W Er2 O7W 74.11(18) . . ? O4W Er2 O7W 76.2(2) . . ? O7 Er2 O7W 136.43(17) . . ? O6W Er2 O7W 147.57(19) . . ? O5W Er2 O7W 122.8(2) . . ? O12W Er3 O18 84.4(2) . . ? O12W Er3 O19 79.2(2) . . ? O18 Er3 O19 76.83(17) . . ? O12W Er3 O13W 108.7(2) . . ? O18 Er3 O13W 139.88(18) . . ? O19 Er3 O13W 141.84(19) . . ? O12W Er3 O10W 143.8(2) . . ? O18 Er3 O10W 72.45(19) . . ? O19 Er3 O10W 120.2(2) . . ? O13W Er3 O10W 75.8(2) . . ? O12W Er3 O9W 142.4(2) . . ? O18 Er3 O9W 110.5(2) . . ? O19 Er3 O9W 71.5(2) . . ? O13W Er3 O9W 82.5(2) . . ? O10W Er3 O9W 73.2(2) . . ? O12W Er3 O11W 69.9(2) . . ? O18 Er3 O11W 75.55(19) . . ? O19 Er3 O11W 140.1(2) . . ? O13W Er3 O11W 74.1(2) . . ? O10W Er3 O11W 77.4(2) . . ? O9W Er3 O11W 146.1(2) . . ? O12W Er3 O14W 72.0(2) . . ? O18 Er3 O14W 144.54(19) . . ? O19 Er3 O14W 73.11(19) . . ? O13W Er3 O14W 74.3(2) . . ? O10W Er3 O14W 140.1(2) . . ? O9W Er3 O14W 77.3(2) . . ? O11W Er3 O14W 118.0(2) . . ? Cl3 Er4 O8W 68.28(17) . . ? Cl3 Er4 O13 110.39(16) . . ? O8W Er4 O13 76.01(19) . . ? Cl3 Er4 O12 72.91(15) . . ? O8W Er4 O12 116.18(19) . . ? O13 Er4 O12 72.67(17) . . ? Cl3 Er4 O20 100.08(15) . . ? O8W Er4 O20 95.03(19) . . ? O13 Er4 O20 141.59(16) . . ? O12 Er4 O20 140.86(16) . . ? Cl3 Er4 O14 132.05(16) . . ? O8W Er4 O14 65.76(18) . . ? O13 Er4 O14 70.82(18) . . ? O12 Er4 O14 141.49(17) . . ? O20 Er4 O14 71.47(17) . . ? Cl3 Er4 O11 66.69(15) . . ? O8W Er4 O11 128.78(18) . . ? O13 Er4 O11 143.12(17) . . ? O12 Er4 O11 71.54(17) . . ? O20 Er4 O11 70.48(16) . . ? O14 Er4 O11 140.22(17) . . ? Cl3 Er4 Cl4 144.81(11) . . ? O8W Er4 Cl4 146.78(14) . . ? O13 Er4 Cl4 84.90(12) . . ? O12 Er4 Cl4 82.54(12) . . ? O20 Er4 Cl4 83.21(11) . . ? O14 Er4 Cl4 82.46(13) . . ? O11 Er4 Cl4 81.98(12) . . ? C2 O1 Er1 135.1(5) . . ? C3 O2 Er1 131.3(5) . . ? C4 O3 Er1 132.5(4) . . ? C5 O4 Er1 132.3(5) . . ? C1 O5 Er1 132.0(5) . . ? C8 O6 Er2 157.9(5) . . ? C7 O7 Er2 153.9(5) . . ? C57 O11 Er4 132.6(4) . . ? C55 O12 Er4 132.1(4) . . ? C53 O13 Er4 132.8(4) . . ? C51 O14 Er4 134.5(5) . . ? C69 O18 Er3 155.9(5) . . ? C61 O19 Er3 154.3(5) . . ? C59 O20 Er4 131.8(4) . . ? C3 N1 C26 113.7(6) . . ? C3 N1 C17 120.7(6) . . ? C26 N1 C17 125.3(6) . . ? C3 N2 C16 122.5(6) . . ? C3 N2 C25 112.8(6) . . ? C16 N2 C25 124.5(6) . . ? C2 N3 C16 120.2(6) . . ? C2 N3 C24 113.8(6) . . ? C16 N3 C24 125.9(6) . . ? C2 N4 C15 122.7(6) . . ? C2 N4 C23 110.9(6) . . ? C15 N4 C23 126.3(6) . . ? C1 N5 C15 122.9(6) . . ? C1 N5 C22 110.5(6) . . ? C15 N5 C22 126.6(6) . . ? C20 N6 C14 128.0(6) . . ? C20 N6 C24 107.4(6) . . ? C14 N6 C24 122.5(6) . . ? C1 N7 C19 120.5(6) . . ? C1 N7 C21 112.7(7) . . ? C19 N7 C21 126.8(7) . . ? C5 N8 C19 121.7(6) . . ? C5 N8 C30 112.4(6) . . ? C19 N8 C30 125.9(6) . . ? C5 N9 C29 112.3(6) . . ? C5 N9 C18 122.2(6) . . ? C29 N9 C18 125.4(6) . . ? C4 N10 C18 121.6(6) . . ? C4 N10 C28 112.2(6) . . ? C18 N10 C28 126.1(6) . . ? C4 N11 C17 121.3(6) . . ? C4 N11 C27 111.4(6) . . ? C17 N11 C27 127.0(6) . . ? C7 N12 C13 124.4(6) . . ? C7 N12 C26 110.7(6) . . ? C13 N12 C26 124.8(6) . . ? C7 N13 C14 121.9(6) . . ? C7 N13 C25 113.1(6) . . ? C14 N13 C25 122.0(6) . . ? C20 N14 C12 125.6(7) . . ? C20 N14 C23 109.8(6) . . ? C12 N14 C23 124.6(6) . . ? C6 N15 C12 121.1(6) . . ? C6 N15 C22 112.4(6) . . ? C12 N15 C22 126.0(6) . . ? C6 N16 C11 121.8(6) . . ? C6 N16 C21 113.9(6) . . ? C11 N16 C21 123.9(7) . . ? C10 N17 C30 113.6(6) . . ? C10 N17 C11 122.1(6) . . ? C30 N17 C11 123.9(6) . . ? C10 N18 C9 123.2(6) . . ? C10 N18 C29 111.7(6) . . ? C9 N18 C29 125.0(6) . . ? C8 N19 C28 111.5(6) . . ? C8 N19 C9 122.3(6) . . ? C28 N19 C9 125.5(6) . . ? C8 N20 C13 125.4(6) . . ? C8 N20 C27 109.9(6) . . ? C13 N20 C27 124.6(6) . . ? C61 N21 C62 120.7(6) . . ? C61 N21 C71 112.2(6) . . ? C62 N21 C71 125.8(6) . . ? C61 N22 C70 124.9(6) . . ? C61 N22 C72 110.5(6) . . ? C70 N22 C72 124.3(6) . . ? C69 N23 C73 111.5(6) . . ? C69 N23 C70 123.7(6) . . ? C73 N23 C70 124.7(6) . . ? C68 N24 C75 112.4(6) . . ? C68 N24 C100 122.4(6) . . ? C75 N24 C100 125.1(6) . . ? C68 N25 C66 121.8(6) . . ? C68 N25 C76 111.5(6) . . ? C66 N25 C76 126.2(6) . . ? C57 N26 C73 112.3(6) . . ? C57 N26 C60 119.3(6) . . ? C73 N26 C60 128.1(6) . . ? C65 N27 C77 112.8(6) . . ? C65 N27 C66 119.3(6) . . ? C77 N27 C66 127.7(6) . . ? C65 N28 C78 111.1(6) . . ? C65 N28 C64 120.8(6) . . ? C78 N28 C64 127.7(6) . . ? C63 N29 C79 115.2(7) . . ? C63 N29 C64 120.6(6) . . ? C79 N29 C64 124.2(7) . . ? C63 N30 C80 115.2(7) . . ? C63 N30 C62 122.8(6) . . ? C80 N30 C62 121.8(7) . . ? C51 N31 C58 123.5(6) . . ? C51 N31 C80 109.4(7) . . ? C58 N31 C80 126.9(7) . . ? C51 N32 C52 121.9(6) . . ? C51 N32 C79 113.0(7) . . ? C52 N32 C79 124.9(7) . . ? C53 N33 C52 125.1(6) . . ? C53 N33 C78 109.0(6) . . ? C52 N33 C78 125.5(6) . . ? C53 N34 C54 123.6(6) . . ? C53 N34 C77 110.3(6) . . ? C54 N34 C77 126.0(6) . . ? C55 N35 C54 121.0(6) . . ? C55 N35 C76 113.1(6) . . ? C54 N35 C76 125.9(6) . . ? C55 N36 C56 120.8(6) . . ? C55 N36 C75 112.0(6) . . ? C56 N36 C75 126.8(6) . . ? C57 N37 C56 120.4(6) . . ? C57 N37 C74 114.9(6) . . ? C56 N37 C74 124.5(6) . . ? C69 N38 C100 121.0(6) . . ? C69 N38 C74 112.4(6) . . ? C100 N38 C74 125.7(6) . . ? C59 N39 C60 122.2(6) . . ? C59 N39 C72 112.1(5) . . ? C60 N39 C72 125.0(6) . . ? C59 N40 C71 113.6(6) . . ? C59 N40 C58 122.4(6) . . ? C71 N40 C58 123.7(6) . . ? O5 C1 N7 125.6(7) . . ? O5 C1 N5 123.4(8) . . ? N7 C1 N5 111.0(7) . . ? O1 C2 N3 126.2(7) . . ? O1 C2 N4 122.5(7) . . ? N3 C2 N4 111.2(6) . . ? O2 C3 N1 126.4(7) . . ? O2 C3 N2 125.9(7) . . ? N1 C3 N2 107.8(6) . . ? O3 C4 N10 126.9(7) . . ? O3 C4 N11 123.2(7) . . ? N10 C4 N11 109.8(6) . . ? O4 C5 N8 124.8(7) . . ? O4 C5 N9 124.5(7) . . ? N8 C5 N9 110.6(6) . . ? O8 C6 N16 126.1(7) . . ? O8 C6 N15 125.1(7) . . ? N16 C6 N15 108.8(6) . . ? O7 C7 N13 125.9(7) . . ? O7 C7 N12 123.9(7) . . ? N13 C7 N12 110.2(6) . . ? O6 C8 N19 125.5(7) . . ? O6 C8 N20 122.4(7) . . ? N19 C8 N20 112.2(7) . . ? N18 C9 N19 113.1(6) . . ? N18 C9 H9A 109.0 . . ? N19 C9 H9A 109.0 . . ? N18 C9 H9B 109.0 . . ? N19 C9 H9B 109.0 . . ? H9A C9 H9B 107.8 . . ? O9 C10 N17 124.8(7) . . ? O9 C10 N18 125.9(7) . . ? N17 C10 N18 109.1(6) . . ? N16 C11 N17 113.6(6) . . ? N16 C11 H11A 108.8 . . ? N17 C11 H11A 108.8 . . ? N16 C11 H11B 108.8 . . ? N17 C11 H11B 108.8 . . ? H11A C11 H11B 107.7 . . ? N14 C12 N15 113.8(6) . . ? N14 C12 H12A 108.8 . . ? N15 C12 H12A 108.8 . . ? N14 C12 H12B 108.8 . . ? N15 C12 H12B 108.8 . . ? H12A C12 H12B 107.7 . . ? N12 C13 N20 114.0(6) . . ? N12 C13 H13A 108.8 . . ? N20 C13 H13A 108.8 . . ? N12 C13 H13B 108.8 . . ? N20 C13 H13B 108.8 . . ? H13A C13 H13B 107.6 . . ? N6 C14 N13 108.7(6) . . ? N6 C14 H14A 109.9 . . ? N13 C14 H14A 109.9 . . ? N6 C14 H14B 109.9 . . ? N13 C14 H14B 109.9 . . ? H14A C14 H14B 108.3 . . ? N4 C15 N5 114.4(6) . . ? N4 C15 H15A 108.7 . . ? N5 C15 H15A 108.7 . . ? N4 C15 H15B 108.7 . . ? N5 C15 H15B 108.7 . . ? H15A C15 H15B 107.6 . . ? N2 C16 N3 112.3(6) . . ? N2 C16 H16A 109.2 . . ? N3 C16 H16A 109.2 . . ? N2 C16 H16B 109.2 . . ? N3 C16 H16B 109.2 . . ? H16A C16 H16B 107.9 . . ? N11 C17 N1 114.7(6) . . ? N11 C17 H17A 108.6 . . ? N1 C17 H17A 108.6 . . ? N11 C17 H17B 108.6 . . ? N1 C17 H17B 108.6 . . ? H17A C17 H17B 107.6 . . ? N10 C18 N9 114.1(6) . . ? N10 C18 H18A 108.7 . . ? N9 C18 H18A 108.7 . . ? N10 C18 H18B 108.7 . . ? N9 C18 H18B 108.7 . . ? H18A C18 H18B 107.6 . . ? N8 C19 N7 114.4(6) . . ? N8 C19 H19A 108.7 . . ? N7 C19 H19A 108.7 . . ? N8 C19 H19B 108.7 . . ? N7 C19 H19B 108.7 . . ? H19A C19 H19B 107.6 . . ? O10 C20 N6 122.1(7) . . ? O10 C20 N14 121.9(7) . . ? N6 C20 N14 115.9(7) . . ? N7 C21 N16 112.7(7) . . ? N7 C21 C31 114.1(7) . . ? N16 C21 C31 114.0(7) . . ? N7 C21 C22 102.6(7) . . ? N16 C21 C22 101.9(6) . . ? C31 C21 C22 110.1(7) . . ? N5 C22 N15 111.6(6) . . ? N5 C22 C32 113.3(6) . . ? N15 C22 C32 112.0(6) . . ? N5 C22 C21 103.2(6) . . ? N15 C22 C21 102.7(6) . . ? C32 C22 C21 113.2(7) . . ? N4 C23 N14 113.3(6) . . ? N4 C23 C33 111.6(6) . . ? N14 C23 C33 114.7(6) . . ? N4 C23 C24 104.0(5) . . ? N14 C23 C24 102.0(5) . . ? C33 C23 C24 110.2(6) . . ? N3 C24 C34 112.4(6) . . ? N3 C24 N6 108.9(6) . . ? C34 C24 N6 118.0(6) . . ? N3 C24 C23 99.8(5) . . ? C34 C24 C23 112.1(6) . . ? N6 C24 C23 103.8(5) . . ? N2 C25 N13 110.2(6) . . ? N2 C25 C35 112.2(6) . . ? N13 C25 C35 115.6(5) . . ? N2 C25 C26 103.1(5) . . ? N13 C25 C26 101.4(5) . . ? C35 C25 C26 113.2(6) . . ? N12 C26 N1 111.1(6) . . ? N12 C26 C36 114.1(6) . . ? N1 C26 C36 113.7(6) . . ? N12 C26 C25 104.1(5) . . ? N1 C26 C25 102.2(5) . . ? C36 C26 C25 110.6(6) . . ? N11 C27 N20 112.0(6) . . ? N11 C27 C37 113.4(7) . . ? N20 C27 C37 112.1(6) . . ? N11 C27 C28 103.0(6) . . ? N20 C27 C28 103.0(6) . . ? C37 C27 C28 112.7(6) . . ? N19 C28 N10 111.2(6) . . ? N19 C28 C38 112.2(6) . . ? N10 C28 C38 113.1(6) . . ? N19 C28 C27 103.3(6) . . ? N10 C28 C27 102.8(6) . . ? C38 C28 C27 113.3(6) . . ? N9 C29 N18 112.5(6) . . ? N9 C29 C39 114.0(6) . . ? N18 C29 C39 111.6(6) . . ? N9 C29 C30 103.6(6) . . ? N18 C29 C30 103.3(5) . . ? C39 C29 C30 111.1(6) . . ? N17 C30 N8 110.4(6) . . ? N17 C30 C40 113.9(6) . . ? N8 C30 C40 114.1(6) . . ? N17 C30 C29 102.1(5) . . ? N8 C30 C29 100.9(6) . . ? C40 C30 C29 114.0(6) . . ? C50 C31 C21 112.7(8) . . ? C50 C31 H31A 109.1 . . ? C21 C31 H31A 109.1 . . ? C50 C31 H31B 109.1 . . ? C21 C31 H31B 109.1 . . ? H31A C31 H31B 107.8 . . ? C49 C32 C22 108.9(8) . . ? C49 C32 H32A 109.9 . . ? C22 C32 H32A 109.9 . . ? C49 C32 H32B 109.9 . . ? C22 C32 H32B 109.9 . . ? H32A C32 H32B 108.3 . . ? C23 C33 C48 111.2(7) . . ? C23 C33 H33A 109.4 . . ? C48 C33 H33A 109.4 . . ? C23 C33 H33B 109.4 . . ? C48 C33 H33B 109.4 . . ? H33A C33 H33B 108.0 . . ? C24 C34 C47 110.8(7) . . ? C24 C34 H34A 109.5 . . ? C47 C34 H34A 109.5 . . ? C24 C34 H34B 109.5 . . ? C47 C34 H34B 109.5 . . ? H34A C34 H34B 108.1 . . ? C25 C35 C46 111.0(6) . . ? C25 C35 H35A 109.4 . . ? C46 C35 H35A 109.4 . . ? C25 C35 H35B 109.4 . . ? C46 C35 H35B 109.4 . . ? H35A C35 H35B 108.0 . . ? C26 C36 C45 111.8(6) . . ? C26 C36 H36A 109.3 . . ? C45 C36 H36A 109.3 . . ? C26 C36 H36B 109.3 . . ? C45 C36 H36B 109.3 . . ? H36A C36 H36B 107.9 . . ? C27 C37 C44 110.1(7) . . ? C27 C37 H37A 109.6 . . ? C44 C37 H37A 109.6 . . ? C27 C37 H37B 109.6 . . ? C44 C37 H37B 109.6 . . ? H37A C37 H37B 108.2 . . ? C43 C38 C28 107.9(7) . . ? C43 C38 H38A 110.1 . . ? C28 C38 H38A 110.1 . . ? C43 C38 H38B 110.1 . . ? C28 C38 H38B 110.1 . . ? H38A C38 H38B 108.4 . . ? C42 C39 C29 112.1(7) . . ? C42 C39 H39A 109.2 . . ? C29 C39 H39A 109.2 . . ? C42 C39 H39B 109.2 . . ? C29 C39 H39B 109.2 . . ? H39A C39 H39B 107.9 . . ? C30 C40 C41 109.8(6) . . ? C30 C40 H40A 109.7 . . ? C41 C40 H40A 109.7 . . ? C30 C40 H40B 109.7 . . ? C41 C40 H40B 109.7 . . ? H40A C40 H40B 108.2 . . ? C42 C41 C40 114.5(7) . . ? C42 C41 H41A 108.6 . . ? C40 C41 H41A 108.6 . . ? C42 C41 H41B 108.6 . . ? C40 C41 H41B 108.6 . . ? H41A C41 H41B 107.6 . . ? C39 C42 C41 111.7(7) . . ? C39 C42 H42A 109.3 . . ? C41 C42 H42A 109.3 . . ? C39 C42 H42B 109.3 . . ? C41 C42 H42B 109.3 . . ? H42A C42 H42B 107.9 . . ? C38 C43 C44 115.5(8) . . ? C38 C43 H43A 108.4 . . ? C44 C43 H43A 108.4 . . ? C38 C43 H43B 108.4 . . ? C44 C43 H43B 108.4 . . ? H43A C43 H43B 107.5 . . ? C37 C44 C43 110.6(8) . . ? C37 C44 H44A 109.5 . . ? C43 C44 H44A 109.5 . . ? C37 C44 H44B 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 108.1 . . ? C46 C45 C36 112.2(7) . . ? C46 C45 H45A 109.2 . . ? C36 C45 H45A 109.2 . . ? C46 C45 H45B 109.2 . . ? C36 C45 H45B 109.2 . . ? H45A C45 H45B 107.9 . . ? C45 C46 C35 113.7(6) . . ? C45 C46 H46A 108.8 . . ? C35 C46 H46A 108.8 . . ? C45 C46 H46B 108.8 . . ? C35 C46 H46B 108.8 . . ? H46A C46 H46B 107.7 . . ? C34 C47 C48 111.6(8) . . ? C34 C47 H47A 109.3 . . ? C48 C47 H47A 109.3 . . ? C34 C47 H47B 109.3 . . ? C48 C47 H47B 109.3 . . ? H47A C47 H47B 108.0 . . ? C33 C48 C47 113.6(8) . . ? C33 C48 H48A 108.9 . . ? C47 C48 H48A 108.9 . . ? C33 C48 H48B 108.9 . . ? C47 C48 H48B 108.9 . . ? H48A C48 H48B 107.7 . . ? C32 C49 C50 118.7(9) . . ? C32 C49 H49A 107.6 . . ? C50 C49 H49A 107.6 . . ? C32 C49 H49B 107.6 . . ? C50 C49 H49B 107.6 . . ? H49A C49 H49B 107.1 . . ? C31 C50 C49 108.6(8) . . ? C31 C50 H50A 110.0 . . ? C49 C50 H50A 110.0 . . ? C31 C50 H50B 110.0 . . ? C49 C50 H50B 110.0 . . ? H50A C50 H50B 108.4 . . ? O14 C51 N32 126.5(7) . . ? O14 C51 N31 120.5(7) . . ? N32 C51 N31 112.9(6) . . ? N32 C52 N33 115.1(6) . . ? N32 C52 H52A 108.5 . . ? N33 C52 H52A 108.5 . . ? N32 C52 H52B 108.5 . . ? N33 C52 H52B 108.5 . . ? H52A C52 H52B 107.5 . . ? O13 C53 N34 125.1(7) . . ? O13 C53 N33 122.1(7) . . ? N34 C53 N33 112.7(7) . . ? N34 C54 N35 112.4(6) . . ? N34 C54 H54A 109.1 . . ? N35 C54 H54A 109.1 . . ? N34 C54 H54B 109.1 . . ? N35 C54 H54B 109.1 . . ? H54A C54 H54B 107.9 . . ? O12 C55 N35 126.9(7) . . ? O12 C55 N36 124.4(7) . . ? N35 C55 N36 108.6(6) . . ? N37 C56 N36 114.1(5) . . ? N37 C56 H56A 108.7 . . ? N36 C56 H56A 108.7 . . ? N37 C56 H56B 108.7 . . ? N36 C56 H56B 108.7 . . ? H56A C56 H56B 107.6 . . ? O11 C57 N37 127.1(6) . . ? O11 C57 N26 125.6(7) . . ? N37 C57 N26 107.2(6) . . ? N31 C58 N40 114.3(6) . . ? N31 C58 H58A 108.7 . . ? N40 C58 H58A 108.7 . . ? N31 C58 H58B 108.7 . . ? N40 C58 H58B 108.7 . . ? H58A C58 H58B 107.6 . . ? O20 C59 N40 127.7(7) . . ? O20 C59 N39 123.2(6) . . ? N40 C59 N39 109.0(6) . . ? N39 C60 N26 114.3(5) . . ? N39 C60 H60A 108.7 . . ? N26 C60 H60A 108.7 . . ? N39 C60 H60B 108.7 . . ? N26 C60 H60B 108.7 . . ? H60A C60 H60B 107.6 . . ? O19 C61 N21 125.6(7) . . ? O19 C61 N22 123.8(7) . . ? N21 C61 N22 110.6(6) . . ? N21 C62 N30 114.3(6) . . ? N21 C62 H62A 108.7 . . ? N30 C62 H62A 108.7 . . ? N21 C62 H62B 108.7 . . ? N30 C62 H62B 108.7 . . ? H62A C62 H62B 107.6 . . ? O17 C63 N29 128.5(7) . . ? O17 C63 N30 124.6(7) . . ? N29 C63 N30 106.9(6) . . ? N28 C64 N29 114.5(6) . . ? N28 C64 H64A 108.6 . . ? N29 C64 H64A 108.6 . . ? N28 C64 H64B 108.6 . . ? N29 C64 H64B 108.6 . . ? H64A C64 H64B 107.6 . . ? O16 C65 N27 128.1(7) . . ? O16 C65 N28 123.8(7) . . ? N27 C65 N28 108.0(6) . . ? N25 C66 N27 113.5(6) . . ? N25 C66 H66A 108.9 . . ? N27 C66 H66A 108.9 . . ? N25 C66 H66B 108.9 . . ? N27 C66 H66B 108.9 . . ? H66A C66 H66B 107.7 . . ? C81 C67 C99 109.0(8) . . ? C81 C67 H67A 109.9 . . ? C99 C67 H67A 109.9 . . ? C81 C67 H67B 109.9 . . ? C99 C67 H67B 109.9 . . ? H67A C67 H67B 108.3 . . ? O15 C68 N25 125.7(7) . . ? O15 C68 N24 125.1(7) . . ? N25 C68 N24 109.1(6) . . ? O18 C69 N38 125.0(7) . . ? O18 C69 N23 124.4(7) . . ? N38 C69 N23 110.5(6) . . ? N22 C70 N23 114.7(6) . . ? N22 C70 H70A 108.6 . . ? N23 C70 H70A 108.6 . . ? N22 C70 H70B 108.6 . . ? N23 C70 H70B 108.6 . . ? H70A C70 H70B 107.6 . . ? N40 C71 N21 112.7(6) . . ? N40 C71 C90 113.2(6) . . ? N21 C71 C90 111.7(6) . . ? N40 C71 C72 102.6(6) . . ? N21 C71 C72 103.4(5) . . ? C90 C71 C72 112.4(6) . . ? N39 C72 N22 112.1(6) . . ? N39 C72 C89 114.5(6) . . ? N22 C72 C89 111.9(6) . . ? N39 C72 C71 102.1(5) . . ? N22 C72 C71 103.0(5) . . ? C89 C72 C71 112.2(6) . . ? N26 C73 N23 112.0(5) . . ? N26 C73 C88 113.3(6) . . ? N23 C73 C88 111.3(6) . . ? N26 C73 C74 103.6(5) . . ? N23 C73 C74 102.8(5) . . ? C88 C73 C74 113.2(6) . . ? N37 C74 N38 112.8(6) . . ? N37 C74 C87 115.1(6) . . ? N38 C74 C87 111.9(6) . . ? N37 C74 C73 101.4(5) . . ? N38 C74 C73 102.8(5) . . ? C87 C74 C73 111.6(6) . . ? N24 C75 N36 111.4(6) . . ? N24 C75 C86 114.1(6) . . ? N36 C75 C86 111.5(6) . . ? N24 C75 C76 103.4(5) . . ? N36 C75 C76 103.3(6) . . ? C86 C75 C76 112.3(6) . . ? N35 C76 N25 112.1(6) . . ? N35 C76 C85 112.5(6) . . ? N25 C76 C85 112.8(6) . . ? N35 C76 C75 102.8(6) . . ? N25 C76 C75 103.4(5) . . ? C85 C76 C75 112.5(6) . . ? N27 C77 N34 112.1(6) . . ? N27 C77 C84 113.1(6) . . ? N34 C77 C84 108.5(6) . . ? N27 C77 C78 103.9(6) . . ? N34 C77 C78 103.7(6) . . ? C84 C77 C78 115.3(6) . . ? N28 C78 N33 113.1(6) . . ? N28 C78 C77 104.0(6) . . ? N33 C78 C77 103.8(5) . . ? N28 C78 C83 113.3(6) . . ? N33 C78 C83 111.2(6) . . ? C77 C78 C83 110.7(7) . . ? N32 C79 N29 112.9(8) . . ? N32 C79 C82 114.9(7) . . ? N29 C79 C82 113.8(7) . . ? N32 C79 C80 102.3(7) . . ? N29 C79 C80 102.3(7) . . ? C82 C79 C80 109.1(8) . . ? N30 C80 N31 112.4(7) . . ? N30 C80 C81 112.0(8) . . ? N31 C80 C81 115.6(8) . . ? N30 C80 C79 100.1(7) . . ? N31 C80 C79 102.2(7) . . ? C81 C80 C79 113.2(8) . . ? C67 C81 C80 111.4(8) . . ? C67 C81 H81A 109.3 . . ? C80 C81 H81A 109.3 . . ? C67 C81 H81B 109.3 . . ? C80 C81 H81B 109.3 . . ? H81A C81 H81B 108.0 . . ? C99 C82 C79 112.0(7) . . ? C99 C82 H82A 109.2 . . ? C79 C82 H82A 109.2 . . ? C99 C82 H82B 109.2 . . ? C79 C82 H82B 109.2 . . ? H82A C82 H82B 107.9 . . ? C98 C83 C78 109.6(7) . . ? C98 C83 H83A 109.7 . . ? C78 C83 H83A 109.7 . . ? C98 C83 H83B 109.7 . . ? C78 C83 H83B 109.7 . . ? H83A C83 H83B 108.2 . . ? C77 C84 C97 108.5(7) . . ? C77 C84 H84A 110.0 . . ? C97 C84 H84A 110.0 . . ? C77 C84 H84B 110.0 . . ? C97 C84 H84B 110.0 . . ? H84A C84 H84B 108.4 . . ? C96 C85 C76 110.7(6) . . ? C96 C85 H85A 109.5 . . ? C76 C85 H85A 109.5 . . ? C96 C85 H85B 109.5 . . ? C76 C85 H85B 109.5 . . ? H85A C85 H85B 108.1 . . ? C95 C86 C75 111.2(6) . . ? C95 C86 H86A 109.4 . . ? C75 C86 H86A 109.4 . . ? C95 C86 H86B 109.4 . . ? C75 C86 H86B 109.4 . . ? H86A C86 H86B 108.0 . . ? C74 C87 C94 109.0(6) . . ? C74 C87 H87A 109.9 . . ? C94 C87 H87A 109.9 . . ? C74 C87 H87B 109.9 . . ? C94 C87 H87B 109.9 . . ? H87A C87 H87B 108.3 . . ? C93 C88 C73 111.8(6) . . ? C93 C88 H88A 109.3 . . ? C73 C88 H88A 109.3 . . ? C93 C88 H88B 109.3 . . ? C73 C88 H88B 109.3 . . ? H88A C88 H88B 107.9 . . ? C72 C89 C92 111.7(6) . . ? C72 C89 H89A 109.3 . . ? C92 C89 H89A 109.3 . . ? C72 C89 H89B 109.3 . . ? C92 C89 H89B 109.3 . . ? H89A C89 H89B 107.9 . . ? C71 C90 C91 109.3(6) . . ? C71 C90 H90A 109.8 . . ? C91 C90 H90A 109.8 . . ? C71 C90 H90B 109.8 . . ? C91 C90 H90B 109.8 . . ? H90A C90 H90B 108.3 . . ? C92 C91 C90 114.1(7) . . ? C92 C91 H91A 108.7 . . ? C90 C91 H91A 108.7 . . ? C92 C91 H91B 108.7 . . ? C90 C91 H91B 108.7 . . ? H91A C91 H91B 107.6 . . ? C89 C92 C91 111.4(7) . . ? C89 C92 H92A 109.4 . . ? C91 C92 H92A 109.4 . . ? C89 C92 H92B 109.4 . . ? C91 C92 H92B 109.4 . . ? H92A C92 H92B 108.0 . . ? C88 C93 C94 112.8(7) . . ? C88 C93 H93A 109.0 . . ? C94 C93 H93A 109.0 . . ? C88 C93 H93B 109.0 . . ? C94 C93 H93B 109.0 . . ? H93A C93 H93B 107.8 . . ? C93 C94 C87 116.1(7) . . ? C93 C94 H94A 108.3 . . ? C87 C94 H94A 108.3 . . ? C93 C94 H94B 108.3 . . ? C87 C94 H94B 108.3 . . ? H94A C94 H94B 107.4 . . ? C86 C95 C96 114.6(6) . . ? C86 C95 H95A 108.6 . . ? C96 C95 H95A 108.6 . . ? C86 C95 H95B 108.6 . . ? C96 C95 H95B 108.6 . . ? H95A C95 H95B 107.6 . . ? C95 C96 C85 112.5(7) . . ? C95 C96 H96A 109.1 . . ? C85 C96 H96A 109.1 . . ? C95 C96 H96B 109.1 . . ? C85 C96 H96B 109.1 . . ? H96A C96 H96B 107.8 . . ? C98 C97 C84 113.5(8) . . ? C98 C97 H97A 108.9 . . ? C84 C97 H97A 108.9 . . ? C98 C97 H97B 108.9 . . ? C84 C97 H97B 108.9 . . ? H97A C97 H97B 107.7 . . ? C97 C98 C83 114.5(7) . . ? C97 C98 H98A 108.6 . . ? C83 C98 H98A 108.6 . . ? C97 C98 H98B 108.6 . . ? C83 C98 H98B 108.6 . . ? H98A C98 H98B 107.6 . . ? C82 C99 C67 112.9(8) . . ? C82 C99 H99A 109.0 . . ? C67 C99 H99A 109.0 . . ? C82 C99 H99B 109.0 . . ? C67 C99 H99B 109.0 . . ? H99A C99 H99B 107.8 . . ? N38 C100 N24 113.5(6) . . ? N38 C100 H10A 108.9 . . ? N24 C100 H10A 108.9 . . ? N38 C100 H10B 108.9 . . ? N24 C100 H10B 108.9 . . ? H10A C100 H10B 107.7 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.57 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 3.708 _refine_diff_density_min -2.030 _refine_diff_density_rms 0.190 # Attachment '- Ho.cif' data_p _database_code_depnum_ccdc_archive 'CCDC 883407' #TrackingRef '- Ho.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H100 Cl6 Ho2 N20 O30' _chemical_formula_weight 2004.06 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ho Ho -0.2175 4.6783 '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)/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 26.324(7) _cell_length_b 28.868(7) _cell_length_c 20.957(5) _cell_angle_alpha 90.00 _cell_angle_beta 100.900(3) _cell_angle_gamma 90.00 _cell_volume 15638(7) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 7970 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 24.82 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.702 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8128 _exptl_absorpt_coefficient_mu 2.306 _exptl_absorpt_correction_type 'multi scan' _exptl_absorpt_correction_T_min 0.5544 _exptl_absorpt_correction_T_max 0.6817 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 75750 _diffrn_reflns_av_R_equivalents 0.1453 _diffrn_reflns_av_sigmaI/netI 0.1766 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 25.00 _reflns_number_total 26990 _reflns_number_gt 13395 _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. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.003 0.000 0.152 2732 1609 ' ' 2 -0.044 0.500 0.234 2732 1602 ' ' _platon_squeeze_details ; ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0250P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 26990 _refine_ls_number_parameters 1627 _refine_ls_number_restraints 47 _refine_ls_R_factor_all 0.1415 _refine_ls_R_factor_gt 0.0862 _refine_ls_wR_factor_ref 0.1857 _refine_ls_wR_factor_gt 0.1650 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.004 _refine_ls_shift/su_max 0.005 _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 Ho1 Ho 0.264989(17) 0.284534(19) 0.53874(2) 0.03116(14) Uani 1 1 d . . . Ho2 Ho 0.095878(18) 0.14476(2) 0.23666(2) 0.03415(15) Uani 1 1 d . . . Cl1 Cl 0.21566(10) 0.25284(11) 0.42592(14) 0.0440(7) Uani 1 1 d . . . Cl2 Cl 0.3334(2) 0.2696(3) 0.6308(3) 0.153(2) Uani 1 1 d . . . Ho3 Ho 0.644431(17) 0.290004(19) -0.12067(2) 0.03211(15) Uani 1 1 d . . . Ho4 Ho 0.814843(18) 0.14614(2) 0.17939(3) 0.03521(15) Uani 1 1 d . . . Cl3 Cl 0.69430(10) 0.25891(11) -0.00823(14) 0.0448(8) Uani 1 1 d . . . Cl4 Cl 0.5774(2) 0.2738(3) -0.2109(3) 0.150(2) Uani 1 1 d . . . O1W O 0.2767(3) 0.3472(3) 0.6146(4) 0.050(2) Uani 1 1 d . . . O2W O 0.0519(3) 0.1166(3) 0.1352(4) 0.055(2) Uani 1 1 d . . . O3W O 0.0252(4) 0.1089(3) 0.2724(5) 0.081(3) Uani 1 1 d . . . O4W O 0.1114(3) 0.0628(3) 0.2416(5) 0.073(3) Uani 1 1 d . . . O5W O 0.1310(4) 0.2183(3) 0.2186(5) 0.068(3) Uani 1 1 d . . . O6W O 0.0252(3) 0.1982(3) 0.2003(5) 0.070(3) Uani 1 1 d . . . O7W O 0.1608(3) 0.1370(3) 0.1708(4) 0.063(3) Uani 1 1 d . . . O8W O 0.6294(3) 0.3532(3) -0.1935(4) 0.055(2) Uani 1 1 d . . . O9W O 0.8897(3) 0.1931(4) 0.2144(5) 0.073(3) Uani 1 1 d . . . O10W O 0.8546(3) 0.1186(3) 0.2790(4) 0.056(2) Uani 1 1 d . . . O11W O 0.7838(3) 0.2184(3) 0.1992(4) 0.052(2) Uani 1 1 d . . . O12W O 0.7467(3) 0.1394(3) 0.2396(4) 0.056(2) Uani 1 1 d . . . O13W O 0.8825(3) 0.1085(4) 0.1378(5) 0.070(3) Uani 1 1 d . . . O14W O 0.7981(3) 0.0645(3) 0.1782(5) 0.068(3) Uani 1 1 d . . . O1 O 0.1931(3) 0.2515(2) 0.5780(3) 0.0330(18) Uani 1 1 d . . . O2 O 0.3400(2) 0.2631(3) 0.4951(3) 0.0314(17) Uani 1 1 d . . . O3 O 0.2801(3) 0.2007(3) 0.5589(4) 0.0336(18) Uani 1 1 d . . . O4 O 0.2869(3) 0.3483(3) 0.4753(4) 0.043(2) Uani 1 1 d . . . O5 O 0.1951(3) 0.3392(3) 0.5239(4) 0.043(2) Uani 1 1 d . . . O6 O 0.1709(3) 0.1329(3) 0.3112(4) 0.0393(19) Uani 1 1 d . . . O7 O 0.0823(3) 0.1845(3) 0.3294(4) 0.043(2) Uani 1 1 d . . . O8 O 0.1816(3) 0.2972(3) 0.2114(4) 0.045(2) Uani 1 1 d . . . O9 O 0.0773(3) 0.2877(3) 0.2667(4) 0.045(2) Uani 1 1 d . . . O10 O 0.2390(3) 0.1981(3) 0.2358(4) 0.046(2) Uani 1 1 d . . . O11 O 0.7173(2) 0.2582(3) -0.1598(3) 0.0359(18) Uani 1 1 d . . . O12 O 0.5709(2) 0.2684(3) -0.0766(3) 0.0357(18) Uani 1 1 d . . . O13 O 0.6309(3) 0.2088(3) -0.1412(4) 0.038(2) Uani 1 1 d . . . O14 O 0.6213(3) 0.3530(3) -0.0573(4) 0.0389(19) Uani 1 1 d . . . O15 O 0.7138(3) 0.3463(3) -0.1018(3) 0.0361(18) Uani 1 1 d . . . O16 O 0.7406(3) 0.1356(3) 0.1028(4) 0.0361(18) Uani 1 1 d . . . O17 O 0.8292(3) 0.1883(3) 0.0877(4) 0.042(2) Uani 1 1 d . . . O18 O 0.7304(3) 0.2997(3) 0.2059(4) 0.0369(19) Uani 1 1 d . . . O19 O 0.8345(3) 0.2924(3) 0.1533(4) 0.0390(19) Uani 1 1 d . . . O20 O 0.6741(3) 0.2016(3) 0.1807(4) 0.0403(19) Uani 1 1 d . . . N1 N 0.3056(3) 0.2451(4) 0.2827(4) 0.039(2) Uani 1 1 d . . . N2 N 0.0648(3) 0.3023(3) 0.3681(4) 0.037(2) Uani 1 1 d . . . N3 N 0.3509(3) 0.2706(3) 0.3893(4) 0.032(2) Uani 1 1 d . . . N4 N 0.1791(3) 0.1155(3) 0.4209(4) 0.029(2) Uani 1 1 d U . . N5 N 0.1007(3) 0.1552(3) 0.4331(4) 0.031(2) Uani 1 1 d . . . N6 N 0.2961(3) 0.1471(3) 0.4839(4) 0.035(2) Uani 1 1 d . . . N7 N 0.1066(3) 0.2513(3) 0.5235(4) 0.030(2) Uani 1 1 d . . . N8 N 0.1095(3) 0.3287(3) 0.4755(4) 0.034(2) Uani 1 1 d . . . N9 N 0.1110(3) 0.3522(3) 0.3196(4) 0.035(2) Uani 1 1 d . . . N10 N 0.2506(3) 0.1232(3) 0.3777(4) 0.032(2) Uani 1 1 d U . . N11 N 0.1921(3) 0.3604(3) 0.2816(4) 0.033(2) Uani 1 1 d . . . N12 N 0.3049(3) 0.3439(3) 0.3720(4) 0.033(2) Uani 1 1 d . . . N13 N 0.3457(3) 0.2008(3) 0.4286(4) 0.034(2) Uani 1 1 d . . . N14 N 0.3008(3) 0.1742(3) 0.3216(4) 0.033(2) Uani 1 1 d . . . N15 N 0.2249(3) 0.1402(3) 0.5250(4) 0.026(2) Uani 1 1 d . . . N16 N 0.2618(3) 0.3216(3) 0.2651(4) 0.036(2) Uani 1 1 d . . . N17 N 0.2380(3) 0.3837(3) 0.3879(4) 0.037(2) Uani 1 1 d . . . N18 N 0.1498(3) 0.1857(3) 0.5371(4) 0.028(2) Uani 1 1 d . . . N19 N 0.0654(3) 0.2256(3) 0.4160(4) 0.031(2) Uani 1 1 d . . . N20 N 0.1556(3) 0.3762(3) 0.4261(4) 0.036(2) Uani 1 1 d . . . N21 N 0.5654(3) 0.2058(3) -0.0107(4) 0.032(2) Uani 1 1 d . . . N22 N 0.7185(3) 0.3637(3) 0.1369(5) 0.037(2) Uani 1 1 d . . . N23 N 0.6026(3) 0.3494(3) 0.0457(4) 0.033(2) Uani 1 1 d . . . N24 N 0.5602(3) 0.2760(3) 0.0299(4) 0.033(2) Uani 1 1 d . . . N25 N 0.6613(3) 0.1271(3) 0.0366(4) 0.036(2) Uani 1 1 d . . . N26 N 0.8028(3) 0.2596(3) -0.1069(4) 0.029(2) Uani 1 1 d . . . N27 N 0.6070(3) 0.2490(3) 0.1336(4) 0.0221(18) Uani 1 1 d U . . N28 N 0.6502(3) 0.3231(3) 0.1527(4) 0.036(2) Uani 1 1 d . . . N29 N 0.8006(3) 0.3574(3) 0.0976(4) 0.033(2) Uani 1 1 d . . . N30 N 0.6846(3) 0.1469(3) -0.1096(4) 0.032(2) Uani 1 1 d . . . N31 N 0.8422(3) 0.2322(3) -0.0001(4) 0.031(2) Uani 1 1 d . . . N32 N 0.6141(3) 0.1527(3) -0.0681(4) 0.035(2) Uani 1 1 d . . . N33 N 0.7623(3) 0.1911(4) -0.1205(4) 0.040(3) Uani 1 1 d . . . N34 N 0.6715(4) 0.3883(4) 0.0314(4) 0.044(3) Uani 1 1 d . . . N35 N 0.6101(3) 0.1769(3) 0.0935(4) 0.032(2) Uani 1 1 d . . . N36 N 0.7326(3) 0.1195(3) -0.0045(4) 0.034(2) Uani 1 1 d . . . N37 N 0.8092(3) 0.1613(3) -0.0174(4) 0.026(2) Uani 1 1 d . . . N38 N 0.8461(3) 0.3087(4) 0.0500(5) 0.048(3) Uani 1 1 d . . . N39 N 0.7986(3) 0.3338(3) -0.0577(4) 0.037(2) Uani 1 1 d . . . N40 N 0.7507(3) 0.3822(3) -0.0076(4) 0.036(2) Uani 1 1 d . . . C1 C 0.3222(4) 0.3888(4) 0.2742(6) 0.044(3) Uani 1 1 d . . . H1A H 0.3401 0.4113 0.3048 0.053 Uiso 1 1 calc R . . H1B H 0.3478 0.3679 0.2624 0.053 Uiso 1 1 calc R . . C2 C 0.4501(4) 0.2333(5) 0.3555(7) 0.054(4) Uani 1 1 d . . . H2A H 0.4803 0.2353 0.3354 0.064 Uiso 1 1 calc R . . H2B H 0.4554 0.2548 0.3917 0.064 Uiso 1 1 calc R . . C3 C 0.0721(6) 0.4421(6) 0.4319(8) 0.090(5) Uani 1 1 d D . . H3A H 0.0533 0.4710 0.4231 0.108 Uiso 1 1 calc R . . H3B H 0.1041 0.4485 0.4619 0.108 Uiso 1 1 calc R . . C4 C 0.0571(5) 0.1612(4) 0.5964(6) 0.053(3) Uani 1 1 d U . . H4A H 0.0893 0.1686 0.6253 0.064 Uiso 1 1 calc R . . H4B H 0.0383 0.1397 0.6189 0.064 Uiso 1 1 calc R . . C5 C 0.1986(4) 0.4052(4) 0.4214(6) 0.045(3) Uani 1 1 d . . . H5A H 0.2154 0.4142 0.4649 0.054 Uiso 1 1 calc R . . H5B H 0.1857 0.4332 0.3982 0.054 Uiso 1 1 calc R . . C6 C 0.3095(5) 0.0453(5) 0.5210(6) 0.062(4) Uani 1 1 d . . . H6A H 0.3247 0.0148 0.5199 0.075 Uiso 1 1 calc R . . H6B H 0.3347 0.0645 0.5490 0.075 Uiso 1 1 calc R . . C7 C 0.0836(4) 0.4236(4) 0.3717(6) 0.048(3) Uani 1 1 d . . . H7A H 0.1079 0.4439 0.3558 0.057 Uiso 1 1 calc R . . H7B H 0.0522 0.4222 0.3391 0.057 Uiso 1 1 calc R . . C8 C 0.2676(4) 0.1672(4) 0.5259(5) 0.028(2) Uani 1 1 d . . . C9 C 0.0240(4) 0.2072(4) 0.5811(6) 0.043(3) Uani 1 1 d . . . H9A H -0.0099 0.2025 0.5916 0.051 Uiso 1 1 calc R . . H9B H 0.0408 0.2322 0.6080 0.051 Uiso 1 1 calc R . . C10 C 0.3018(4) 0.0654(4) 0.4527(5) 0.034(3) Uani 1 1 d . . . H10A H 0.2833 0.0432 0.4221 0.041 Uiso 1 1 calc R . . H10B H 0.3353 0.0709 0.4411 0.041 Uiso 1 1 calc R . . C11 C 0.2344(4) 0.3884(4) 0.3177(5) 0.034(3) Uani 1 1 d . . . C12 C 0.1221(3) 0.1130(4) 0.4192(5) 0.030(3) Uani 1 1 d . . . H12A H 0.1051 0.1027 0.3764 0.036 Uiso 1 1 calc R . . H12B H 0.1155 0.0900 0.4504 0.036 Uiso 1 1 calc R . . C13 C 0.2913(4) 0.2837(4) 0.2401(5) 0.028(2) Uani 1 1 d . . . H13A H 0.2707 0.2722 0.1999 0.033 Uiso 1 1 calc R . . H13B H 0.3226 0.2969 0.2296 0.033 Uiso 1 1 calc R . . C14 C 0.3503(4) 0.2412(4) 0.3334(5) 0.036(3) Uani 1 1 d . . . C15 C 0.4028(4) 0.2507(4) 0.3052(6) 0.039(3) Uani 1 1 d . . . H15A H 0.4012 0.2346 0.2642 0.047 Uiso 1 1 calc R . . H15B H 0.4063 0.2836 0.2975 0.047 Uiso 1 1 calc R . . C16 C 0.0353(3) 0.2628(4) 0.3768(5) 0.034(3) Uani 1 1 d . . . H16A H 0.0201 0.2504 0.3345 0.041 Uiso 1 1 calc R . . H16B H 0.0071 0.2721 0.3980 0.041 Uiso 1 1 calc R . . C17 C 0.4485(4) 0.1881(5) 0.3811(6) 0.046(3) Uani 1 1 d . . . H17A H 0.4531 0.1899 0.4281 0.055 Uiso 1 1 calc R . . H17B H 0.4769 0.1701 0.3705 0.055 Uiso 1 1 calc R . . C18 C 0.0745(5) 0.3413(5) 0.4134(7) 0.064(2) Uani 1 1 d D . . C19 C 0.3548(4) 0.3199(4) 0.3947(6) 0.041(3) Uani 1 1 d . . . H19A H 0.3797 0.3308 0.3694 0.050 Uiso 1 1 calc R . . H19B H 0.3676 0.3281 0.4397 0.050 Uiso 1 1 calc R . . C20 C 0.0690(4) 0.1379(4) 0.5364(6) 0.045(3) Uani 1 1 d . . . H20A H 0.0372 0.1281 0.5083 0.054 Uiso 1 1 calc R . . H20B H 0.0904 0.1108 0.5485 0.054 Uiso 1 1 calc R . . C21 C 0.1073(4) 0.3743(4) 0.3835(5) 0.030(2) Uani 1 1 d . . . C22 C 0.3472(3) 0.1666(4) 0.4780(5) 0.029(3) Uani 1 1 d . . . H22A H 0.3630 0.1801 0.5194 0.034 Uiso 1 1 calc R . . H22B H 0.3694 0.1414 0.4693 0.034 Uiso 1 1 calc R . . C23 C 0.1975(4) 0.1260(4) 0.3647(6) 0.035(3) Uani 1 1 d . . . C24 C 0.1557(4) 0.3479(4) 0.4763(6) 0.033(3) Uani 1 1 d . . . C25 C 0.1377(4) 0.3713(4) 0.2704(6) 0.040(3) Uani 1 1 d . . . H25A H 0.1215 0.3594 0.2281 0.048 Uiso 1 1 calc R . . H25B H 0.1336 0.4047 0.2694 0.048 Uiso 1 1 calc R . . C26 C 0.0839(3) 0.1891(4) 0.3891(5) 0.029(3) Uani 1 1 d . . . C27 C 0.0835(4) 0.3113(4) 0.3129(6) 0.033(3) Uani 1 1 d . . . C28 C 0.2342(5) 0.4351(4) 0.2900(6) 0.052(3) Uani 1 1 d . . . H28A H 0.2600 0.4536 0.3182 0.062 Uiso 1 1 calc R . . H28B H 0.2008 0.4491 0.2903 0.062 Uiso 1 1 calc R . . C29 C 0.3964(4) 0.1630(4) 0.3539(5) 0.036(3) Uani 1 1 d . . . H29A H 0.3951 0.1557 0.3085 0.044 Uiso 1 1 calc R . . H29B H 0.3953 0.1341 0.3771 0.044 Uiso 1 1 calc R . . C30 C 0.2139(4) 0.0557(4) 0.5014(6) 0.043(3) Uani 1 1 d . . . H30A H 0.2094 0.0345 0.4649 0.052 Uiso 1 1 calc R . . H30B H 0.1834 0.0537 0.5210 0.052 Uiso 1 1 calc R . . C31 C 0.0181(4) 0.2206(4) 0.5096(6) 0.047(3) Uani 1 1 d . . . H31A H 0.0045 0.2519 0.5036 0.056 Uiso 1 1 calc R . . H31B H -0.0065 0.2000 0.4835 0.056 Uiso 1 1 calc R . . C32 C 0.2191(3) 0.1057(4) 0.4767(5) 0.030(3) Uani 1 1 d . . . C33 C 0.2084(4) 0.3243(4) 0.2503(5) 0.033(3) Uani 1 1 d . . . C34 C 0.2778(4) 0.3566(4) 0.4168(5) 0.032(3) Uani 1 1 d . . . C35 C 0.0982(4) 0.1736(4) 0.5001(5) 0.030(3) Uani 1 1 d . . . C36 C 0.2774(4) 0.2050(4) 0.2768(5) 0.034(3) Uani 1 1 d . . . C37 C 0.2791(4) 0.1283(4) 0.3281(6) 0.046(3) Uani 1 1 d . . . H37A H 0.2569 0.1204 0.2871 0.055 Uiso 1 1 calc R . . H37B H 0.3073 0.1061 0.3354 0.055 Uiso 1 1 calc R . . C38 C 0.0988(4) 0.3013(4) 0.5280(6) 0.037(3) Uani 1 1 d . . . H38A H 0.0631 0.3066 0.5318 0.044 Uiso 1 1 calc R . . H38B H 0.1204 0.3123 0.5678 0.044 Uiso 1 1 calc R . . C39 C 0.0231(5) 0.3640(4) 0.4257(7) 0.064(2) Uani 1 1 d DU . . H39A H 0.0004 0.3713 0.3849 0.077 Uiso 1 1 calc R . . H39B H 0.0051 0.3432 0.4502 0.077 Uiso 1 1 calc R . . C40 C 0.2827(4) 0.3602(4) 0.3076(5) 0.044(3) Uani 1 1 d . . . C41 C 0.3431(3) 0.2475(4) 0.4408(5) 0.031(3) Uani 1 1 d . . . C42 C 0.2708(3) 0.1120(4) 0.4475(5) 0.033(3) Uani 1 1 d . . . C43 C 0.2625(4) 0.0408(5) 0.5524(6) 0.054(4) Uani 1 1 d . . . H43A H 0.2662 0.0606 0.5905 0.065 Uiso 1 1 calc R . . H43B H 0.2587 0.0091 0.5659 0.065 Uiso 1 1 calc R . . C44 C 0.2446(5) 0.4377(5) 0.2238(7) 0.058(4) Uani 1 1 d . . . H44A H 0.2466 0.4700 0.2119 0.069 Uiso 1 1 calc R . . H44B H 0.2157 0.4239 0.1942 0.069 Uiso 1 1 calc R . . C45 C 0.2949(4) 0.4132(4) 0.2151(6) 0.050(3) Uani 1 1 d . . . H45A H 0.2867 0.3909 0.1800 0.060 Uiso 1 1 calc R . . H45B H 0.3181 0.4360 0.2023 0.060 Uiso 1 1 calc R . . C46 C 0.0698(3) 0.2183(4) 0.4858(5) 0.031(3) Uani 1 1 d . . . C47 C 0.0391(5) 0.4073(4) 0.4636(7) 0.064(2) Uani 1 1 d DU . . H47A H 0.0588 0.3985 0.5058 0.077 Uiso 1 1 calc R . . H47B H 0.0082 0.4231 0.4708 0.077 Uiso 1 1 calc R . . C48 C 0.1526(4) 0.2301(4) 0.5460(5) 0.033(3) Uani 1 1 d . . . C49 C 0.1889(4) 0.1537(4) 0.5644(5) 0.038(3) Uani 1 1 d . . . H49A H 0.1720 0.1260 0.5763 0.046 Uiso 1 1 calc R . . H49B H 0.2081 0.1670 0.6041 0.046 Uiso 1 1 calc R . . C50 C 0.3482(3) 0.1920(4) 0.3600(5) 0.027(2) Uani 1 1 d . . . C51 C 0.6486(6) 0.0463(5) -0.1379(8) 0.080(5) Uani 1 1 d . . . H51A H 0.6516 0.0138 -0.1483 0.095 Uiso 1 1 calc R . . H51B H 0.6458 0.0641 -0.1777 0.095 Uiso 1 1 calc R . . C52 C 0.8813(5) 0.4271(5) 0.0813(7) 0.072(4) Uani 1 1 d . . . H52A H 0.8811 0.4173 0.1255 0.087 Uiso 1 1 calc R . . H52B H 0.8977 0.4573 0.0831 0.087 Uiso 1 1 calc R . . C53 C 0.8544(4) 0.1686(4) -0.1812(6) 0.048(3) Uani 1 1 d . . . H53A H 0.8225 0.1754 -0.2114 0.058 Uiso 1 1 calc R . . H53B H 0.8744 0.1472 -0.2022 0.058 Uiso 1 1 calc R . . C54 C 0.5885(5) 0.3913(4) 0.1443(7) 0.049(3) Uani 1 1 d . . . H54A H 0.5592 0.3731 0.1517 0.059 Uiso 1 1 calc R . . H54B H 0.5755 0.4162 0.1145 0.059 Uiso 1 1 calc R . . C55 C 0.6911(4) 0.1094(4) -0.0603(6) 0.044(3) Uani 1 1 d . . . C56 C 0.8273(4) 0.4309(4) 0.0451(6) 0.049(3) Uani 1 1 d . . . H56A H 0.8272 0.4451 0.0032 0.059 Uiso 1 1 calc R . . H56B H 0.8077 0.4506 0.0690 0.059 Uiso 1 1 calc R . . C57 C 0.6077(4) 0.0680(4) -0.0337(6) 0.043(3) Uani 1 1 d . . . H57A H 0.6264 0.0434 -0.0076 0.052 Uiso 1 1 calc R . . H57B H 0.5758 0.0740 -0.0184 0.052 Uiso 1 1 calc R . . C58 C 0.4619(4) 0.2393(5) 0.0620(7) 0.052(4) Uani 1 1 d . . . H58A H 0.4592 0.2613 0.0265 0.063 Uiso 1 1 calc R . . H58B H 0.4310 0.2424 0.0805 0.063 Uiso 1 1 calc R . . C59 C 0.6961(4) 0.0616(4) -0.0895(6) 0.040(3) Uani 1 1 d . . . H59A H 0.7256 0.0616 -0.1110 0.048 Uiso 1 1 calc R . . H59B H 0.7028 0.0391 -0.0546 0.048 Uiso 1 1 calc R . . C60 C 0.4639(4) 0.1871(5) 0.0330(6) 0.059(4) Uani 1 1 d . . . H60A H 0.4360 0.1687 0.0440 0.071 Uiso 1 1 calc R . . H60B H 0.4597 0.1883 -0.0140 0.071 Uiso 1 1 calc R . . C61 C 0.6289(4) 0.1323(4) 0.0868(5) 0.038(3) Uani 1 1 d . . . H61A H 0.5998 0.1114 0.0765 0.046 Uiso 1 1 calc R . . H61B H 0.6492 0.1228 0.1283 0.046 Uiso 1 1 calc R . . C62 C 0.7083(4) 0.4087(4) -0.0053(6) 0.041(3) Uani 1 1 d . . . H62A H 0.6903 0.4145 -0.0494 0.049 Uiso 1 1 calc R . . H62B H 0.7197 0.4384 0.0139 0.049 Uiso 1 1 calc R . . C63 C 0.5579(4) 0.2452(4) 0.0858(5) 0.038(3) Uani 1 1 d . . . C64 C 0.5965(5) 0.0546(6) -0.1054(8) 0.076(5) Uani 1 1 d . . . H64A H 0.5757 0.0788 -0.1297 0.091 Uiso 1 1 calc R . . H64B H 0.5761 0.0264 -0.1104 0.091 Uiso 1 1 calc R . . C65 C 0.6750(4) 0.4395(4) 0.1311(7) 0.053(3) Uani 1 1 d U . . H65A H 0.7077 0.4546 0.1303 0.064 Uiso 1 1 calc R . . H65B H 0.6479 0.4568 0.1033 0.064 Uiso 1 1 calc R . . C66 C 0.5097(4) 0.2522(4) 0.1148(6) 0.044(3) Uani 1 1 d . . . H66A H 0.5074 0.2841 0.1281 0.052 Uiso 1 1 calc R . . H66B H 0.5111 0.2325 0.1527 0.052 Uiso 1 1 calc R . . C67 C 0.6411(4) 0.1747(5) -0.1083(5) 0.040(3) Uani 1 1 d . . . C68 C 0.6763(4) 0.3915(4) 0.1065(5) 0.036(3) Uani 1 1 d . . . C69 C 0.5556(4) 0.3242(4) 0.0281(5) 0.037(3) Uani 1 1 d . . . H69A H 0.5326 0.3333 0.0570 0.044 Uiso 1 1 calc R . . H69B H 0.5393 0.3332 -0.0156 0.044 Uiso 1 1 calc R . . C70 C 0.7872(4) 0.1174(4) -0.0072(6) 0.037(3) Uani 1 1 d . . . H70A H 0.8058 0.1045 0.0333 0.044 Uiso 1 1 calc R . . H70B H 0.7919 0.0967 -0.0420 0.044 Uiso 1 1 calc R . . C71 C 0.8252(4) 0.3179(4) 0.1041(6) 0.032(3) Uani 1 1 d . . . C72 C 0.6652(8) 0.4390(7) 0.1981(7) 0.105(6) Uani 1 1 d U . . H72A H 0.6620 0.4710 0.2111 0.126 Uiso 1 1 calc R . . H72B H 0.6958 0.4265 0.2259 0.126 Uiso 1 1 calc R . . C73 C 0.8861(4) 0.2146(4) -0.1641(6) 0.045(3) Uani 1 1 d . . . H73A H 0.9202 0.2108 -0.1745 0.054 Uiso 1 1 calc R . . H73B H 0.8689 0.2396 -0.1907 0.054 Uiso 1 1 calc R . . C74 C 0.8845(4) 0.3695(4) -0.0108(5) 0.036(3) Uani 1 1 d . . . H74A H 0.9060 0.3464 -0.0262 0.043 Uiso 1 1 calc R . . H74B H 0.8755 0.3927 -0.0446 0.043 Uiso 1 1 calc R . . C75 C 0.5177(4) 0.1644(4) 0.0629(6) 0.042(3) Uani 1 1 d . . . H75A H 0.5187 0.1577 0.1085 0.050 Uiso 1 1 calc R . . H75B H 0.5212 0.1354 0.0410 0.050 Uiso 1 1 calc R . . C76 C 0.7209(4) 0.1582(4) -0.1517(5) 0.029(2) Uani 1 1 d . . . H76A H 0.7021 0.1719 -0.1915 0.035 Uiso 1 1 calc R . . H76B H 0.7369 0.1299 -0.1632 0.035 Uiso 1 1 calc R . . C77 C 0.8733(4) 0.2679(4) 0.0397(5) 0.029(2) Uani 1 1 d . . . H77A H 0.8878 0.2545 0.0816 0.035 Uiso 1 1 calc R . . H77B H 0.9019 0.2764 0.0189 0.035 Uiso 1 1 calc R . . C78 C 0.7502(4) 0.3517(4) -0.0618(6) 0.035(3) Uani 1 1 d . . . C79 C 0.6212(4) 0.2873(4) 0.1795(5) 0.032(3) Uani 1 1 d . . . H79A H 0.5900 0.3007 0.1900 0.039 Uiso 1 1 calc R . . H79B H 0.6419 0.2754 0.2193 0.039 Uiso 1 1 calc R . . C80 C 0.7732(4) 0.3762(4) 0.1474(5) 0.037(3) Uani 1 1 d . . . H80A H 0.7900 0.3649 0.1898 0.044 Uiso 1 1 calc R . . H80B H 0.7761 0.4097 0.1479 0.044 Uiso 1 1 calc R . . C81 C 0.7141(4) 0.1273(4) 0.0493(6) 0.035(3) Uani 1 1 d . . . C82 C 0.5633(3) 0.1706(4) -0.0625(5) 0.037(3) Uani 1 1 d . . . H82A H 0.5417 0.1451 -0.0537 0.044 Uiso 1 1 calc R . . H82B H 0.5472 0.1843 -0.1037 0.044 Uiso 1 1 calc R . . C83 C 0.8013(4) 0.3827(4) 0.0352(5) 0.033(3) Uani 1 1 d . . . C84 C 0.8275(4) 0.1932(4) 0.0267(6) 0.038(3) Uani 1 1 d . . . C85 C 0.8359(3) 0.3469(4) 0.0024(5) 0.033(3) Uani 1 1 d . . . C86 C 0.6307(4) 0.3627(4) 0.0026(6) 0.038(3) Uani 1 1 d . . . C87 C 0.8918(3) 0.2281(4) -0.0909(4) 0.029(3) Uani 1 1 d . . . H87A H 0.9147 0.2063 -0.0645 0.035 Uiso 1 1 calc R . . H87B H 0.9071 0.2587 -0.0841 0.035 Uiso 1 1 calc R . . C88 C 0.8106(4) 0.3081(4) -0.1120(5) 0.033(3) Uani 1 1 d . . . H88A H 0.7892 0.3194 -0.1517 0.040 Uiso 1 1 calc R . . H88B H 0.8465 0.3137 -0.1148 0.040 Uiso 1 1 calc R . . C89 C 0.6353(4) 0.2084(4) 0.1401(6) 0.046(3) Uani 1 1 d . . . C90 C 0.6188(7) 0.4128(6) 0.2125(12) 0.120(8) Uani 1 1 d . . . H90A H 0.5963 0.4335 0.2307 0.144 Uiso 1 1 calc R . . H90B H 0.6300 0.3881 0.2435 0.144 Uiso 1 1 calc R . . C91 C 0.6261(4) 0.3602(4) 0.1141(5) 0.029(2) Uani 1 1 d U . . C92 C 0.5614(3) 0.1952(4) 0.0566(5) 0.030(3) Uani 1 1 d . . . C93 C 0.8414(4) 0.1456(4) -0.1186(5) 0.040(3) Uani 1 1 d . . . H93A H 0.8218 0.1174 -0.1304 0.047 Uiso 1 1 calc R . . H93B H 0.8733 0.1374 -0.0894 0.047 Uiso 1 1 calc R . . C94 C 0.8398(3) 0.2281(3) -0.0696(5) 0.022(2) Uani 1 1 d . . . C95 C 0.5664(3) 0.2507(4) -0.0222(5) 0.027(2) Uani 1 1 d . . . C96 C 0.7562(4) 0.2383(4) -0.1299(5) 0.030(3) Uani 1 1 d . . . C97 C 0.7003(4) 0.3250(4) 0.1676(5) 0.030(3) Uani 1 1 d . . . C98 C 0.8111(4) 0.1774(4) -0.0850(5) 0.035(3) Uani 1 1 d . . . C99 C 0.6413(4) 0.1125(4) -0.0298(6) 0.042(3) Uani 1 1 d . . . C100 C 0.9136(4) 0.3915(5) 0.0484(7) 0.058(4) Uani 1 1 d . . . H10C H 0.9433 0.4074 0.0376 0.070 Uiso 1 1 calc R . . H10D H 0.9265 0.3675 0.0797 0.070 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ho1 0.0216(2) 0.0497(4) 0.0202(3) -0.0034(3) -0.0010(2) -0.0020(2) Ho2 0.0256(2) 0.0532(4) 0.0207(3) -0.0038(3) -0.0031(2) -0.0004(2) Cl1 0.0322(14) 0.067(2) 0.0281(16) -0.0097(15) -0.0057(12) -0.0040(13) Cl2 0.121(5) 0.190(7) 0.147(6) -0.004(5) 0.027(4) -0.016(4) Ho3 0.0197(2) 0.0532(4) 0.0207(3) 0.0048(3) -0.0032(2) 0.0013(2) Ho4 0.0277(3) 0.0522(4) 0.0232(3) 0.0057(3) -0.0018(2) 0.0020(2) Cl3 0.0363(15) 0.068(2) 0.0265(16) 0.0106(15) -0.0042(12) 0.0031(14) Cl4 0.120(5) 0.194(7) 0.140(5) 0.004(5) 0.036(4) -0.010(5) O1W 0.043(5) 0.072(6) 0.030(5) -0.013(4) -0.010(4) 0.009(4) O2W 0.035(4) 0.089(7) 0.034(5) -0.018(5) -0.011(4) 0.011(4) O3W 0.061(6) 0.075(7) 0.113(9) -0.021(7) 0.033(6) -0.015(5) O4W 0.057(6) 0.070(7) 0.078(7) -0.015(6) -0.022(5) 0.007(5) O5W 0.066(6) 0.066(7) 0.071(7) -0.001(6) 0.011(5) -0.008(5) O6W 0.058(6) 0.066(7) 0.075(7) 0.013(6) -0.010(5) 0.034(5) O7W 0.032(4) 0.114(8) 0.042(6) -0.011(5) 0.005(4) -0.002(5) O8W 0.048(5) 0.066(6) 0.048(6) 0.008(5) -0.003(4) -0.009(4) O9W 0.049(5) 0.097(8) 0.067(7) -0.004(6) -0.006(5) -0.019(5) O10W 0.051(5) 0.073(7) 0.037(5) 0.004(5) -0.009(4) -0.011(4) O11W 0.046(5) 0.053(5) 0.059(6) 0.006(5) 0.018(4) 0.009(4) O12W 0.041(5) 0.092(7) 0.036(5) 0.016(5) 0.009(4) 0.006(4) O13W 0.052(5) 0.097(8) 0.063(7) 0.023(6) 0.018(5) 0.022(5) O14W 0.074(6) 0.062(7) 0.068(7) -0.006(5) 0.013(5) -0.006(5) O1 0.035(4) 0.040(5) 0.024(4) -0.005(4) 0.003(3) -0.009(3) O2 0.033(4) 0.046(5) 0.012(4) -0.007(4) -0.001(3) -0.001(3) O3 0.042(4) 0.039(5) 0.020(4) -0.003(4) 0.006(3) 0.001(4) O4 0.029(4) 0.051(5) 0.048(6) -0.004(5) 0.004(4) -0.003(4) O5 0.032(4) 0.045(5) 0.048(5) -0.005(4) -0.002(4) 0.013(3) O6 0.027(4) 0.063(6) 0.021(4) 0.004(4) -0.013(3) 0.003(4) O7 0.034(4) 0.062(6) 0.030(5) -0.010(4) -0.001(4) 0.010(4) O8 0.039(4) 0.055(6) 0.036(5) -0.004(4) -0.006(4) -0.002(4) O9 0.052(5) 0.047(6) 0.035(5) -0.009(4) 0.006(4) -0.005(4) O10 0.042(5) 0.060(6) 0.029(5) -0.012(4) -0.009(4) -0.016(4) O11 0.024(4) 0.053(5) 0.031(5) 0.003(4) 0.007(3) 0.003(3) O12 0.025(4) 0.058(5) 0.021(4) 0.009(4) -0.002(3) -0.001(3) O13 0.038(4) 0.052(6) 0.025(5) 0.008(4) 0.006(4) 0.002(4) O14 0.031(4) 0.063(6) 0.021(5) -0.004(4) 0.000(3) -0.011(4) O15 0.024(4) 0.062(5) 0.020(4) 0.004(4) -0.003(3) 0.002(3) O16 0.032(4) 0.052(5) 0.023(4) -0.001(4) 0.003(3) 0.001(3) O17 0.042(4) 0.062(6) 0.021(5) 0.007(4) 0.005(4) 0.007(4) O18 0.028(4) 0.053(5) 0.026(5) -0.001(4) -0.003(3) -0.005(4) O19 0.035(4) 0.053(6) 0.029(5) -0.005(4) 0.006(4) 0.007(4) O20 0.034(4) 0.057(6) 0.027(5) -0.001(4) -0.001(4) -0.001(4) N1 0.022(4) 0.072(7) 0.024(5) -0.002(5) 0.004(4) -0.006(4) N2 0.038(5) 0.050(6) 0.023(5) 0.004(5) 0.005(4) -0.015(4) N3 0.027(4) 0.038(6) 0.033(6) -0.004(5) 0.008(4) -0.006(4) N4 0.020(3) 0.042(4) 0.024(4) 0.002(3) 0.000(3) -0.004(3) N5 0.033(5) 0.038(6) 0.017(5) 0.007(4) -0.005(4) 0.009(4) N6 0.020(4) 0.052(6) 0.031(6) -0.017(5) 0.001(4) -0.003(4) N7 0.020(4) 0.044(6) 0.023(5) -0.001(4) -0.002(4) 0.001(4) N8 0.019(4) 0.061(7) 0.021(5) -0.005(5) 0.003(4) -0.005(4) N9 0.028(5) 0.053(7) 0.022(5) -0.004(5) -0.001(4) 0.002(4) N10 0.032(3) 0.035(4) 0.024(4) -0.010(3) -0.004(3) 0.006(3) N11 0.026(4) 0.046(6) 0.021(5) -0.006(4) -0.014(4) 0.007(4) N12 0.024(4) 0.040(6) 0.032(6) -0.001(5) -0.001(4) 0.006(4) N13 0.018(4) 0.053(7) 0.033(6) -0.012(5) 0.011(4) 0.000(4) N14 0.024(4) 0.049(6) 0.022(5) 0.006(5) -0.005(4) -0.002(4) N15 0.024(4) 0.032(5) 0.021(5) -0.005(4) 0.003(4) 0.000(4) N16 0.028(5) 0.041(6) 0.042(6) -0.021(5) 0.012(4) -0.006(4) N17 0.035(5) 0.048(6) 0.030(6) -0.006(5) 0.012(4) -0.002(4) N18 0.026(4) 0.037(6) 0.019(5) 0.001(4) 0.000(4) -0.010(4) N19 0.015(4) 0.042(6) 0.035(6) -0.004(5) -0.003(4) -0.003(4) N20 0.022(4) 0.050(6) 0.034(6) 0.011(5) -0.001(4) -0.003(4) N21 0.028(4) 0.043(7) 0.025(5) -0.008(5) 0.004(4) -0.004(4) N22 0.034(5) 0.035(6) 0.040(6) -0.001(5) 0.004(4) -0.004(4) N23 0.021(4) 0.046(6) 0.034(6) 0.001(5) 0.007(4) 0.006(4) N24 0.028(5) 0.045(6) 0.028(6) 0.009(5) 0.008(4) 0.003(4) N25 0.027(4) 0.042(6) 0.040(6) -0.002(5) 0.011(4) -0.002(4) N26 0.018(4) 0.040(6) 0.027(5) 0.005(4) -0.004(4) -0.005(4) N27 0.023(3) 0.025(4) 0.015(4) 0.004(3) -0.005(3) -0.002(3) N28 0.031(5) 0.041(6) 0.038(6) -0.010(5) 0.012(4) -0.006(4) N29 0.035(5) 0.034(6) 0.030(6) 0.000(5) 0.009(4) -0.009(4) N30 0.035(5) 0.033(6) 0.024(5) -0.003(4) -0.004(4) 0.007(4) N31 0.028(4) 0.051(6) 0.016(5) 0.003(4) 0.007(4) -0.010(4) N32 0.025(4) 0.056(6) 0.021(5) -0.004(5) -0.004(4) 0.004(4) N33 0.015(4) 0.080(8) 0.022(5) -0.004(5) -0.003(4) -0.005(4) N34 0.051(6) 0.059(7) 0.021(5) 0.000(5) 0.006(5) -0.012(5) N35 0.024(4) 0.046(6) 0.020(5) 0.000(5) -0.008(4) 0.003(4) N36 0.020(4) 0.051(6) 0.030(5) -0.006(5) 0.002(4) -0.001(4) N37 0.030(4) 0.036(6) 0.016(5) 0.005(4) 0.010(4) 0.004(4) N38 0.025(5) 0.075(8) 0.044(7) 0.021(6) 0.007(5) 0.010(5) N39 0.020(4) 0.052(6) 0.037(6) -0.006(5) 0.001(4) -0.011(4) N40 0.027(4) 0.042(6) 0.037(6) 0.011(5) 0.004(4) 0.002(4) C1 0.025(5) 0.060(9) 0.046(8) 0.007(7) 0.003(5) -0.004(5) C2 0.015(5) 0.067(10) 0.078(10) 0.013(8) 0.008(6) 0.002(5) C3 0.097(12) 0.102(14) 0.074(12) -0.044(11) 0.022(10) -0.021(10) C4 0.060(5) 0.057(5) 0.047(5) 0.002(4) 0.019(4) -0.001(4) C5 0.047(7) 0.055(8) 0.029(7) -0.011(6) -0.001(6) -0.013(6) C6 0.083(10) 0.061(9) 0.047(9) 0.024(7) 0.024(8) 0.028(8) C7 0.045(7) 0.034(7) 0.065(9) 0.010(7) 0.009(6) 0.005(5) C8 0.025(5) 0.034(7) 0.025(6) 0.012(5) 0.005(5) 0.007(5) C9 0.044(7) 0.051(8) 0.037(8) 0.003(6) 0.017(6) 0.005(6) C10 0.033(6) 0.046(8) 0.021(6) -0.009(5) -0.001(5) 0.003(5) C11 0.034(6) 0.044(8) 0.022(6) 0.001(5) 0.002(5) -0.007(5) C12 0.023(5) 0.046(7) 0.019(6) 0.008(5) -0.002(4) 0.007(5) C13 0.033(5) 0.040(7) 0.011(5) 0.002(5) 0.009(4) -0.009(5) C14 0.023(5) 0.054(8) 0.032(7) 0.008(6) 0.006(5) 0.013(5) C15 0.024(5) 0.052(8) 0.044(8) -0.005(6) 0.012(5) 0.012(5) C16 0.017(5) 0.055(8) 0.026(6) -0.019(6) -0.009(4) 0.006(5) C17 0.019(5) 0.077(10) 0.036(8) 0.001(7) -0.010(5) 0.005(6) C18 0.064(2) 0.064(2) 0.064(2) -0.0004(10) 0.0123(11) 0.0002(10) C19 0.026(6) 0.052(8) 0.047(8) 0.001(7) 0.008(5) 0.007(5) C20 0.016(5) 0.078(10) 0.044(8) -0.007(7) 0.014(5) -0.010(5) C21 0.024(5) 0.026(6) 0.038(7) -0.012(5) 0.002(5) 0.002(4) C22 0.019(5) 0.039(7) 0.025(6) 0.010(5) -0.005(4) -0.004(4) C23 0.031(6) 0.032(7) 0.043(8) 0.001(6) 0.010(6) 0.001(5) C24 0.032(6) 0.031(7) 0.035(7) -0.015(6) 0.002(5) 0.009(5) C25 0.026(5) 0.056(8) 0.036(7) 0.013(6) -0.001(5) 0.016(5) C26 0.018(5) 0.052(8) 0.018(6) 0.005(6) 0.008(4) -0.012(5) C27 0.026(5) 0.044(8) 0.027(7) -0.003(6) 0.001(5) 0.004(5) C28 0.049(7) 0.045(8) 0.056(9) -0.009(7) 0.000(7) -0.009(6) C29 0.031(6) 0.049(8) 0.026(7) 0.005(6) -0.003(5) 0.005(5) C30 0.038(6) 0.024(7) 0.064(9) 0.014(6) 0.000(6) 0.013(5) C31 0.027(6) 0.062(8) 0.057(9) -0.019(7) 0.026(6) -0.020(5) C32 0.015(5) 0.035(7) 0.034(7) 0.000(5) -0.008(4) 0.008(4) C33 0.033(6) 0.037(7) 0.029(7) -0.002(6) 0.005(5) -0.008(5) C34 0.021(5) 0.050(8) 0.019(6) 0.000(6) -0.007(5) -0.003(5) C35 0.028(5) 0.055(8) 0.005(5) 0.003(5) 0.000(4) 0.004(5) C36 0.026(5) 0.048(8) 0.029(7) -0.016(6) 0.010(5) -0.005(5) C37 0.037(6) 0.073(10) 0.027(7) 0.001(6) 0.005(5) -0.008(6) C38 0.028(6) 0.048(8) 0.034(7) -0.006(6) 0.003(5) -0.002(5) C39 0.064(2) 0.064(2) 0.064(2) -0.0004(10) 0.0123(11) 0.0002(10) C40 0.039(6) 0.071(9) 0.021(7) -0.011(6) 0.006(5) 0.002(6) C41 0.013(5) 0.047(8) 0.028(7) 0.007(6) -0.010(5) 0.001(4) C42 0.013(4) 0.067(8) 0.016(6) -0.023(6) -0.002(4) -0.003(5) C43 0.045(7) 0.056(9) 0.058(9) 0.001(7) 0.003(7) 0.014(6) C44 0.059(8) 0.053(9) 0.062(10) 0.022(8) 0.011(7) -0.004(7) C45 0.054(7) 0.062(9) 0.037(8) 0.011(7) 0.017(6) -0.010(6) C46 0.019(5) 0.051(8) 0.022(6) 0.003(5) 0.003(4) 0.002(5) C47 0.064(2) 0.064(2) 0.064(2) -0.0004(10) 0.0123(11) 0.0002(10) C48 0.022(5) 0.056(9) 0.022(6) 0.010(6) 0.006(5) -0.001(5) C49 0.025(5) 0.054(8) 0.034(7) 0.002(6) 0.000(5) -0.002(5) C50 0.022(5) 0.036(7) 0.019(6) -0.003(5) -0.005(4) -0.005(4) C51 0.088(11) 0.061(10) 0.087(13) -0.002(9) 0.010(10) -0.023(8) C52 0.055(8) 0.087(12) 0.070(11) -0.011(9) 0.004(8) -0.003(8) C53 0.036(6) 0.056(9) 0.057(9) -0.002(7) 0.020(6) -0.004(6) C54 0.054(7) 0.023(7) 0.080(10) -0.010(7) 0.034(7) 0.014(5) C55 0.039(6) 0.051(8) 0.045(8) -0.003(7) 0.012(6) 0.001(6) C56 0.053(7) 0.055(9) 0.042(8) -0.001(7) 0.015(6) -0.007(6) C57 0.029(6) 0.031(7) 0.069(9) -0.010(7) 0.007(6) -0.004(5) C58 0.020(5) 0.070(10) 0.071(10) 0.006(8) 0.019(6) -0.005(5) C59 0.040(6) 0.041(7) 0.041(7) -0.005(6) 0.012(6) 0.002(5) C60 0.027(6) 0.101(12) 0.049(9) 0.021(9) 0.006(6) -0.009(7) C61 0.035(6) 0.054(8) 0.023(6) 0.000(6) -0.002(5) -0.002(5) C62 0.021(5) 0.061(8) 0.039(7) 0.009(6) 0.006(5) 0.001(5) C63 0.020(5) 0.063(9) 0.032(7) -0.006(6) 0.006(5) 0.001(5) C64 0.058(9) 0.085(12) 0.085(12) -0.008(10) 0.010(8) -0.011(8) C65 0.032(6) 0.057(9) 0.074(8) -0.010(8) 0.017(6) 0.008(6) C66 0.032(6) 0.053(8) 0.049(8) -0.004(7) 0.015(6) -0.007(5) C67 0.016(5) 0.085(10) 0.018(7) -0.020(7) -0.002(5) -0.008(6) C68 0.027(5) 0.042(8) 0.034(7) 0.002(6) -0.008(5) -0.009(5) C69 0.019(5) 0.064(9) 0.029(7) 0.006(6) 0.007(5) 0.001(5) C70 0.028(5) 0.038(7) 0.039(7) 0.009(6) -0.006(5) 0.006(5) C71 0.027(5) 0.028(7) 0.043(8) 0.005(6) 0.009(5) 0.000(5) C72 0.124(16) 0.136(17) 0.045(8) -0.008(11) -0.008(9) 0.019(14) C73 0.022(5) 0.079(10) 0.036(7) 0.004(7) 0.007(5) 0.006(6) C74 0.017(5) 0.054(8) 0.035(7) 0.008(6) 0.002(5) -0.005(5) C75 0.045(7) 0.052(8) 0.031(7) 0.007(6) 0.013(6) 0.000(6) C76 0.029(5) 0.051(7) 0.006(5) 0.000(5) -0.002(4) -0.001(5) C77 0.022(5) 0.042(7) 0.021(6) -0.005(5) -0.003(4) -0.002(5) C78 0.031(6) 0.037(7) 0.033(7) 0.005(6) -0.005(5) -0.004(5) C79 0.025(5) 0.051(8) 0.019(6) 0.005(5) 0.000(4) -0.010(5) C80 0.035(6) 0.049(8) 0.028(7) -0.008(6) 0.008(5) -0.014(5) C81 0.028(5) 0.040(7) 0.038(8) 0.004(6) 0.007(5) -0.002(5) C82 0.014(5) 0.054(8) 0.039(7) 0.002(6) -0.005(5) -0.017(5) C83 0.033(6) 0.030(7) 0.035(7) -0.007(5) 0.003(5) -0.003(5) C84 0.030(6) 0.042(8) 0.044(8) 0.010(7) 0.013(6) 0.009(5) C85 0.018(5) 0.067(8) 0.012(6) 0.001(5) -0.001(4) 0.001(5) C86 0.029(6) 0.034(7) 0.047(8) 0.006(6) -0.008(6) -0.010(5) C87 0.018(5) 0.059(8) 0.008(5) -0.010(5) -0.004(4) -0.007(5) C88 0.025(5) 0.053(8) 0.024(6) 0.015(6) 0.010(5) -0.003(5) C89 0.034(6) 0.063(9) 0.039(8) 0.003(7) 0.004(6) 0.002(6) C90 0.090(13) 0.078(13) 0.21(3) -0.043(15) 0.067(15) -0.019(10) C91 0.027(4) 0.037(4) 0.023(4) -0.012(4) 0.001(3) 0.009(3) C92 0.019(5) 0.048(7) 0.023(6) -0.004(5) 0.006(4) -0.011(5) C93 0.037(6) 0.048(8) 0.032(7) -0.002(6) 0.001(5) 0.008(5) C94 0.022(5) 0.028(6) 0.016(5) 0.002(5) 0.000(4) 0.004(4) C95 0.018(5) 0.046(8) 0.018(6) -0.001(5) 0.008(4) 0.005(4) C96 0.019(5) 0.044(8) 0.028(6) 0.002(6) 0.003(5) 0.004(5) C97 0.026(5) 0.052(8) 0.014(6) -0.002(5) 0.011(5) 0.002(5) C98 0.030(5) 0.040(7) 0.031(7) 0.013(6) -0.004(5) 0.002(5) C99 0.038(6) 0.047(8) 0.039(8) -0.027(6) 0.001(6) -0.021(6) C100 0.028(6) 0.068(10) 0.076(10) -0.007(8) 0.003(6) -0.012(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ho1 O1W 2.391(8) . ? Ho1 O5 2.398(7) . ? Ho1 O1 2.399(6) . ? Ho1 O4 2.403(8) . ? Ho1 O2 2.408(6) . ? Ho1 Cl2 2.417(7) . ? Ho1 O3 2.475(8) . ? Ho1 Cl1 2.637(3) . ? Ho2 O6 2.301(7) . ? Ho2 O7 2.342(7) . ? Ho2 O2W 2.364(8) . ? Ho2 O3W 2.370(9) . ? Ho2 O5W 2.373(9) . ? Ho2 O4W 2.400(9) . ? Ho2 O7W 2.403(8) . ? Ho2 O6W 2.425(8) . ? Ho3 O8W 2.363(8) . ? Ho3 Cl4 2.375(7) . ? Ho3 O12 2.380(6) . ? Ho3 O13 2.397(8) . ? Ho3 O14 2.398(8) . ? Ho3 O11 2.406(6) . ? Ho3 O15 2.419(7) . ? Ho3 Cl3 2.629(3) . ? Ho4 O10W 2.293(8) . ? Ho4 O16 2.304(7) . ? Ho4 O11W 2.308(8) . ? Ho4 O17 2.365(7) . ? Ho4 O13W 2.387(8) . ? Ho4 O12W 2.387(7) . ? Ho4 O9W 2.389(9) . ? Ho4 O14W 2.397(9) . ? O1 C48 1.303(12) . ? O2 C41 1.241(12) . ? O3 C8 1.200(12) . ? O4 C34 1.228(12) . ? O5 C24 1.321(13) . ? O6 C23 1.219(13) . ? O7 C26 1.251(12) . ? O8 C33 1.249(12) . ? O9 C27 1.169(12) . ? O10 C36 1.215(12) . ? O11 C96 1.238(12) . ? O12 C95 1.276(11) . ? O13 C67 1.203(14) . ? O14 C86 1.264(13) . ? O15 C78 1.159(12) . ? O16 C81 1.226(12) . ? O17 C84 1.279(13) . ? O18 C97 1.251(12) . ? O19 C71 1.254(12) . ? O20 C89 1.216(13) . ? N1 C36 1.369(14) . ? N1 C14 1.433(13) . ? N1 C13 1.434(13) . ? N2 C27 1.365(13) . ? N2 C16 1.411(13) . ? N2 C18 1.463(15) . ? N3 C41 1.316(13) . ? N3 C19 1.432(14) . ? N3 C14 1.445(13) . ? N4 C23 1.389(13) . ? N4 C32 1.445(12) . ? N4 C12 1.496(11) . ? N5 C26 1.360(13) . ? N5 C12 1.396(13) . ? N5 C35 1.515(12) . ? N6 C42 1.364(12) . ? N6 C8 1.386(13) . ? N6 C22 1.486(11) . ? N7 C48 1.360(12) . ? N7 C38 1.463(14) . ? N7 C46 1.476(13) . ? N8 C24 1.333(13) . ? N8 C38 1.427(13) . ? N8 C18 1.490(16) . ? N9 C27 1.378(14) . ? N9 C25 1.461(13) . ? N9 C21 1.503(13) . ? N10 C23 1.377(12) . ? N10 C37 1.401(13) . ? N10 C42 1.492(13) . ? N11 C33 1.344(13) . ? N11 C25 1.441(12) . ? N11 C11 1.466(13) . ? N12 C34 1.333(13) . ? N12 C40 1.444(14) . ? N12 C19 1.480(12) . ? N13 C41 1.376(14) . ? N13 C22 1.428(13) . ? N13 C50 1.473(13) . ? N14 C36 1.353(13) . ? N14 C50 1.446(12) . ? N14 C37 1.458(14) . ? N15 C8 1.366(12) . ? N15 C32 1.406(12) . ? N15 C49 1.424(12) . ? N16 C33 1.382(12) . ? N16 C40 1.466(14) . ? N16 C13 1.493(12) . ? N17 C34 1.356(13) . ? N17 C11 1.462(13) . ? N17 C5 1.494(13) . ? N18 C48 1.295(14) . ? N18 C49 1.420(13) . ? N18 C35 1.474(12) . ? N19 C26 1.331(13) . ? N19 C46 1.459(13) . ? N19 C16 1.487(13) . ? N20 C24 1.332(14) . ? N20 C21 1.410(12) . ? N20 C5 1.427(13) . ? N21 C95 1.320(13) . ? N21 C92 1.465(13) . ? N21 C82 1.479(13) . ? N22 C97 1.418(13) . ? N22 C68 1.420(13) . ? N22 C80 1.459(12) . ? N23 C86 1.328(13) . ? N23 C69 1.423(12) . ? N23 C91 1.483(13) . ? N24 C95 1.348(13) . ? N24 C69 1.396(14) . ? N24 C63 1.480(14) . ? N25 C81 1.364(12) . ? N25 C99 1.455(13) . ? N25 C61 1.482(12) . ? N26 C96 1.375(12) . ? N26 C88 1.421(13) . ? N26 C94 1.451(12) . ? N27 C89 1.380(14) . ? N27 C79 1.467(12) . ? N27 C63 1.480(12) . ? N28 C97 1.297(12) . ? N28 C91 1.417(13) . ? N28 C79 1.460(12) . ? N29 C71 1.307(13) . ? N29 C80 1.479(13) . ? N29 C83 1.501(13) . ? N30 C67 1.403(14) . ? N30 C76 1.456(12) . ? N30 C55 1.482(14) . ? N31 C84 1.348(14) . ? N31 C94 1.451(12) . ? N31 C77 1.472(12) . ? N32 C67 1.358(14) . ? N32 C82 1.460(12) . ? N32 C99 1.513(15) . ? N33 C96 1.381(14) . ? N33 C98 1.413(12) . ? N33 C76 1.499(13) . ? N34 C86 1.350(13) . ? N34 C62 1.469(13) . ? N34 C68 1.556(14) . ? N35 C61 1.396(14) . ? N35 C89 1.404(14) . ? N35 C92 1.465(12) . ? N36 C81 1.330(13) . ? N36 C70 1.448(12) . ? N36 C55 1.471(14) . ? N37 C84 1.329(14) . ? N37 C70 1.427(13) . ? N37 C98 1.499(13) . ? N38 C71 1.377(14) . ? N38 C77 1.415(14) . ? N38 C85 1.479(14) . ? N39 C78 1.361(13) . ? N39 C88 1.442(13) . ? N39 C85 1.493(13) . ? N40 C62 1.363(12) . ? N40 C78 1.436(14) . ? N40 C83 1.457(13) . ? C1 C45 1.486(15) . ? C1 C40 1.591(15) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C17 1.415(17) . ? C2 C15 1.555(15) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C7 1.454(18) . ? C3 C47 1.557(14) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C20 1.510(16) . ? C4 C9 1.586(16) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C43 1.514(16) . ? C6 C10 1.522(15) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C21 1.556(15) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C9 C31 1.528(16) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C42 1.567(15) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C28 1.466(16) . ? C11 C40 1.559(15) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C50 1.529(15) . ? C14 C15 1.626(13) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C29 1.561(14) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C21 1.498(17) . ? C18 C39 1.569(17) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C35 1.566(14) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C28 C44 1.466(17) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C50 1.544(13) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 C32 1.549(15) . ? C30 C43 1.563(15) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C46 1.536(12) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 C42 1.604(12) . ? C35 C46 1.492(14) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 C47 1.497(13) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 C45 1.543(16) . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C51 C59 1.517(17) . ? C51 C64 1.660(19) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C52 C56 1.484(16) . ? C52 C100 1.573(18) . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C53 C93 1.566(15) . ? C53 C73 1.572(16) . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C54 C91 1.557(13) . ? C54 C90 1.62(2) . ? C54 H54A 0.9700 . ? C54 H54B 0.9700 . ? C55 C59 1.525(16) . ? C55 C99 1.567(14) . ? C56 C83 1.549(15) . ? C56 H56A 0.9700 . ? C56 H56B 0.9700 . ? C57 C64 1.526(18) . ? C57 C99 1.554(14) . ? C57 H57A 0.9700 . ? C57 H57B 0.9700 . ? C58 C66 1.555(16) . ? C58 C60 1.630(18) . ? C58 H58A 0.9700 . ? C58 H58B 0.9700 . ? C59 H59A 0.9700 . ? C59 H59B 0.9700 . ? C60 C75 1.578(15) . ? C60 H60A 0.9700 . ? C60 H60B 0.9700 . ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? C62 H62A 0.9700 . ? C62 H62B 0.9700 . ? C63 C66 1.520(13) . ? C63 C92 1.577(16) . ? C64 H64A 0.9700 . ? C64 H64B 0.9700 . ? C65 C72 1.474(19) . ? C65 C68 1.480(16) . ? C65 H65A 0.9700 . ? C65 H65B 0.9700 . ? C66 H66A 0.9700 . ? C66 H66B 0.9700 . ? C68 C91 1.633(14) . ? C69 H69A 0.9700 . ? C69 H69B 0.9700 . ? C70 H70A 0.9700 . ? C70 H70B 0.9700 . ? C72 C90 1.52(2) . ? C72 H72A 0.9700 . ? C72 H72B 0.9700 . ? C73 C87 1.563(14) . ? C73 H73A 0.9700 . ? C73 H73B 0.9700 . ? C74 C100 1.475(16) . ? C74 C85 1.507(13) . ? C74 H74A 0.9700 . ? C74 H74B 0.9700 . ? C75 C92 1.480(14) . ? C75 H75A 0.9700 . ? C75 H75B 0.9700 . ? C76 H76A 0.9700 . ? C76 H76B 0.9700 . ? C77 H77A 0.9700 . ? C77 H77B 0.9700 . ? C79 H79A 0.9700 . ? C79 H79B 0.9700 . ? C80 H80A 0.9700 . ? C80 H80B 0.9700 . ? C82 H82A 0.9700 . ? C82 H82B 0.9700 . ? C83 C85 1.612(14) . ? C87 C94 1.516(12) . ? C87 H87A 0.9700 . ? C87 H87B 0.9700 . ? C88 H88A 0.9700 . ? C88 H88B 0.9700 . ? C90 H90A 0.9700 . ? C90 H90B 0.9700 . ? C93 C98 1.479(15) . ? C93 H93A 0.9700 . ? C93 H93B 0.9700 . ? C94 C98 1.649(14) . ? C100 H10C 0.9700 . ? C100 H10D 0.9700 . ? 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 O1W Ho1 O5 65.7(3) . . ? O1W Ho1 O1 94.8(3) . . ? O5 Ho1 O1 70.8(3) . . ? O1W Ho1 O4 76.9(3) . . ? O5 Ho1 O4 71.5(3) . . ? O1 Ho1 O4 141.4(2) . . ? O1W Ho1 O2 115.8(2) . . ? O5 Ho1 O2 141.6(3) . . ? O1 Ho1 O2 141.7(2) . . ? O4 Ho1 O2 71.8(2) . . ? O1W Ho1 Cl2 67.7(3) . . ? O5 Ho1 Cl2 131.2(3) . . ? O1 Ho1 Cl2 99.9(2) . . ? O4 Ho1 Cl2 110.9(2) . . ? O2 Ho1 Cl2 73.5(2) . . ? O1W Ho1 O3 129.0(3) . . ? O5 Ho1 O3 139.4(2) . . ? O1 Ho1 O3 70.4(2) . . ? O4 Ho1 O3 142.7(2) . . ? O2 Ho1 O3 72.3(2) . . ? Cl2 Ho1 O3 67.5(2) . . ? O1W Ho1 Cl1 147.1(2) . . ? O5 Ho1 Cl1 82.9(2) . . ? O1 Ho1 Cl1 83.28(18) . . ? O4 Ho1 Cl1 84.2(2) . . ? O2 Ho1 Cl1 82.57(17) . . ? Cl2 Ho1 Cl1 145.15(19) . . ? O3 Ho1 Cl1 81.38(19) . . ? O6 Ho2 O7 75.8(3) . . ? O6 Ho2 O2W 140.4(3) . . ? O7 Ho2 O2W 142.1(2) . . ? O6 Ho2 O3W 110.1(3) . . ? O7 Ho2 O3W 72.5(3) . . ? O2W Ho2 O3W 81.6(3) . . ? O6 Ho2 O5W 86.1(3) . . ? O7 Ho2 O5W 79.6(3) . . ? O2W Ho2 O5W 107.7(3) . . ? O3W Ho2 O5W 142.5(3) . . ? O6 Ho2 O4W 72.9(3) . . ? O7 Ho2 O4W 119.9(3) . . ? O2W Ho2 O4W 75.5(3) . . ? O3W Ho2 O4W 72.2(3) . . ? O5W Ho2 O4W 145.1(3) . . ? O6 Ho2 O7W 76.3(3) . . ? O7 Ho2 O7W 139.4(3) . . ? O2W Ho2 O7W 74.4(3) . . ? O3W Ho2 O7W 145.8(3) . . ? O5W Ho2 O7W 69.6(3) . . ? O4W Ho2 O7W 78.4(3) . . ? O6 Ho2 O6W 144.8(3) . . ? O7 Ho2 O6W 73.8(3) . . ? O2W Ho2 O6W 73.8(3) . . ? O3W Ho2 O6W 77.0(4) . . ? O5W Ho2 O6W 71.3(3) . . ? O4W Ho2 O6W 139.0(3) . . ? O7W Ho2 O6W 117.8(3) . . ? O8W Ho3 Cl4 68.2(3) . . ? O8W Ho3 O12 113.8(3) . . ? Cl4 Ho3 O12 73.9(2) . . ? O8W Ho3 O13 129.6(3) . . ? Cl4 Ho3 O13 66.6(3) . . ? O12 Ho3 O13 73.1(2) . . ? O8W Ho3 O14 75.1(3) . . ? Cl4 Ho3 O14 111.2(2) . . ? O12 Ho3 O14 70.9(2) . . ? O13 Ho3 O14 142.8(2) . . ? O8W Ho3 O11 97.0(3) . . ? Cl4 Ho3 O11 100.0(2) . . ? O12 Ho3 O11 142.3(3) . . ? O13 Ho3 O11 70.5(2) . . ? O14 Ho3 O11 141.3(2) . . ? O8W Ho3 O15 67.5(3) . . ? Cl4 Ho3 O15 133.3(2) . . ? O12 Ho3 O15 139.1(2) . . ? O13 Ho3 O15 140.1(2) . . ? O14 Ho3 O15 70.3(2) . . ? O11 Ho3 O15 71.7(2) . . ? O8W Ho3 Cl3 146.8(2) . . ? Cl4 Ho3 Cl3 144.69(19) . . ? O12 Ho3 Cl3 82.37(17) . . ? O13 Ho3 Cl3 81.9(2) . . ? O14 Ho3 Cl3 84.2(2) . . ? O11 Ho3 Cl3 83.09(18) . . ? O15 Ho3 Cl3 81.32(18) . . ? O10W Ho4 O16 140.3(3) . . ? O10W Ho4 O11W 105.4(3) . . ? O16 Ho4 O11W 87.8(3) . . ? O10W Ho4 O17 143.4(3) . . ? O16 Ho4 O17 75.3(3) . . ? O11W Ho4 O17 78.3(3) . . ? O10W Ho4 O13W 86.1(3) . . ? O16 Ho4 O13W 106.2(3) . . ? O11W Ho4 O13W 142.4(3) . . ? O17 Ho4 O13W 72.1(3) . . ? O10W Ho4 O12W 75.5(3) . . ? O16 Ho4 O12W 74.6(3) . . ? O11W Ho4 O12W 69.6(3) . . ? O17 Ho4 O12W 136.3(3) . . ? O13W Ho4 O12W 147.4(3) . . ? O10W Ho4 O9W 73.1(3) . . ? O16 Ho4 O9W 146.2(3) . . ? O11W Ho4 O9W 74.4(3) . . ? O17 Ho4 O9W 73.0(3) . . ? O13W Ho4 O9W 75.1(3) . . ? O12W Ho4 O9W 122.8(3) . . ? O10W Ho4 O14W 73.7(3) . . ? O16 Ho4 O14W 74.5(3) . . ? O11W Ho4 O14W 145.1(3) . . ? O17 Ho4 O14W 123.7(3) . . ? O13W Ho4 O14W 72.3(3) . . ? O12W Ho4 O14W 76.7(3) . . ? O9W Ho4 O14W 134.5(3) . . ? C48 O1 Ho1 129.3(6) . . ? C41 O2 Ho1 130.0(6) . . ? C8 O3 Ho1 132.2(7) . . ? C34 O4 Ho1 132.9(7) . . ? C24 O5 Ho1 134.2(6) . . ? C23 O6 Ho2 156.5(7) . . ? C26 O7 Ho2 154.3(8) . . ? C96 O11 Ho3 130.0(6) . . ? C95 O12 Ho3 132.3(6) . . ? C67 O13 Ho3 133.5(7) . . ? C86 O14 Ho3 134.0(7) . . ? C78 O15 Ho3 134.8(7) . . ? C81 O16 Ho4 157.4(7) . . ? C84 O17 Ho4 152.6(8) . . ? C36 N1 C14 110.8(10) . . ? C36 N1 C13 121.9(9) . . ? C14 N1 C13 127.3(9) . . ? C27 N2 C16 124.0(10) . . ? C27 N2 C18 110.9(10) . . ? C16 N2 C18 124.8(9) . . ? C41 N3 C19 117.3(10) . . ? C41 N3 C14 112.9(9) . . ? C19 N3 C14 129.6(9) . . ? C23 N4 C32 114.4(8) . . ? C23 N4 C12 119.8(8) . . ? C32 N4 C12 125.7(8) . . ? C26 N5 C12 125.4(9) . . ? C26 N5 C35 108.0(8) . . ? C12 N5 C35 126.2(8) . . ? C42 N6 C8 113.6(8) . . ? C42 N6 C22 126.0(8) . . ? C8 N6 C22 120.2(9) . . ? C48 N7 C38 123.2(9) . . ? C48 N7 C46 110.3(9) . . ? C38 N7 C46 125.8(8) . . ? C24 N8 C38 122.3(9) . . ? C24 N8 C18 108.7(10) . . ? C38 N8 C18 129.1(9) . . ? C27 N9 C25 124.4(9) . . ? C27 N9 C21 109.4(8) . . ? C25 N9 C21 126.1(9) . . ? C23 N10 C37 120.9(9) . . ? C23 N10 C42 111.5(8) . . ? C37 N10 C42 127.5(8) . . ? C33 N11 C25 119.3(9) . . ? C33 N11 C11 113.3(8) . . ? C25 N11 C11 126.8(9) . . ? C34 N12 C40 113.2(8) . . ? C34 N12 C19 117.6(9) . . ? C40 N12 C19 129.0(9) . . ? C41 N13 C22 122.6(9) . . ? C41 N13 C50 111.4(9) . . ? C22 N13 C50 126.0(9) . . ? C36 N14 C50 112.5(9) . . ? C36 N14 C37 121.7(9) . . ? C50 N14 C37 125.7(9) . . ? C8 N15 C32 113.0(8) . . ? C8 N15 C49 118.2(9) . . ? C32 N15 C49 128.2(8) . . ? C33 N16 C40 110.0(8) . . ? C33 N16 C13 122.5(9) . . ? C40 N16 C13 127.5(8) . . ? C34 N17 C11 113.7(9) . . ? C34 N17 C5 125.2(9) . . ? C11 N17 C5 121.0(9) . . ? C48 N18 C49 124.6(9) . . ? C48 N18 C35 109.5(9) . . ? C49 N18 C35 125.7(9) . . ? C26 N19 C46 110.1(9) . . ? C26 N19 C16 122.5(9) . . ? C46 N19 C16 126.2(8) . . ? C24 N20 C21 110.1(9) . . ? C24 N20 C5 122.1(9) . . ? C21 N20 C5 127.7(10) . . ? C95 N21 C92 112.8(9) . . ? C95 N21 C82 122.6(9) . . ? C92 N21 C82 124.4(9) . . ? C97 N22 C68 110.2(8) . . ? C97 N22 C80 122.3(9) . . ? C68 N22 C80 126.4(9) . . ? C86 N23 C69 122.7(9) . . ? C86 N23 C91 114.4(9) . . ? C69 N23 C91 122.8(8) . . ? C95 N24 C69 122.8(9) . . ? C95 N24 C63 110.1(9) . . ? C69 N24 C63 127.1(9) . . ? C81 N25 C99 111.0(9) . . ? C81 N25 C61 124.3(9) . . ? C99 N25 C61 123.8(8) . . ? C96 N26 C88 123.3(9) . . ? C96 N26 C94 111.7(8) . . ? C88 N26 C94 124.5(8) . . ? C89 N27 C79 120.6(9) . . ? C89 N27 C63 113.0(9) . . ? C79 N27 C63 125.4(8) . . ? C97 N28 C91 115.5(9) . . ? C97 N28 C79 121.3(10) . . ? C91 N28 C79 123.0(8) . . ? C71 N29 C80 123.0(9) . . ? C71 N29 C83 115.3(9) . . ? C80 N29 C83 121.7(9) . . ? C67 N30 C76 120.9(9) . . ? C67 N30 C55 113.1(9) . . ? C76 N30 C55 125.7(8) . . ? C84 N31 C94 112.9(9) . . ? C84 N31 C77 121.4(9) . . ? C94 N31 C77 122.7(8) . . ? C67 N32 C82 118.7(10) . . ? C67 N32 C99 115.9(9) . . ? C82 N32 C99 125.3(9) . . ? C96 N33 C98 114.8(9) . . ? C96 N33 C76 120.4(8) . . ? C98 N33 C76 124.5(10) . . ? C86 N34 C62 122.1(10) . . ? C86 N34 C68 113.0(9) . . ? C62 N34 C68 124.8(9) . . ? C61 N35 C89 122.5(9) . . ? C61 N35 C92 124.9(9) . . ? C89 N35 C92 112.6(9) . . ? C81 N36 C70 124.4(9) . . ? C81 N36 C55 111.8(8) . . ? C70 N36 C55 123.7(9) . . ? C84 N37 C70 127.9(9) . . ? C84 N37 C98 111.7(9) . . ? C70 N37 C98 120.3(9) . . ? C71 N38 C77 125.4(10) . . ? C71 N38 C85 111.1(9) . . ? C77 N38 C85 123.4(9) . . ? C78 N39 C88 119.2(9) . . ? C78 N39 C85 114.5(9) . . ? C88 N39 C85 126.1(8) . . ? C62 N40 C78 119.1(9) . . ? C62 N40 C83 129.3(10) . . ? C78 N40 C83 111.3(8) . . ? C45 C1 C40 111.1(9) . . ? C45 C1 H1A 109.4 . . ? C40 C1 H1A 109.4 . . ? C45 C1 H1B 109.4 . . ? C40 C1 H1B 109.4 . . ? H1A C1 H1B 108.0 . . ? C17 C2 C15 118.6(10) . . ? C17 C2 H2A 107.7 . . ? C15 C2 H2A 107.7 . . ? C17 C2 H2B 107.7 . . ? C15 C2 H2B 107.7 . . ? H2A C2 H2B 107.1 . . ? C7 C3 C47 110.9(12) . . ? C7 C3 H3A 109.5 . . ? C47 C3 H3A 109.4 . . ? C7 C3 H3B 109.5 . . ? C47 C3 H3B 109.5 . . ? H3A C3 H3B 108.0 . . ? C20 C4 C9 113.4(10) . . ? C20 C4 H4A 108.9 . . ? C9 C4 H4A 108.9 . . ? C20 C4 H4B 108.9 . . ? C9 C4 H4B 108.9 . . ? H4A C4 H4B 107.7 . . ? N20 C5 N17 114.8(9) . . ? N20 C5 H5A 108.6 . . ? N17 C5 H5A 108.6 . . ? N20 C5 H5B 108.6 . . ? N17 C5 H5B 108.6 . . ? H5A C5 H5B 107.5 . . ? C43 C6 C10 117.9(11) . . ? C43 C6 H6A 107.8 . . ? C10 C6 H6A 107.8 . . ? C43 C6 H6B 107.8 . . ? C10 C6 H6B 107.8 . . ? H6A C6 H6B 107.2 . . ? C3 C7 C21 110.0(11) . . ? C3 C7 H7A 109.7 . . ? C21 C7 H7A 109.7 . . ? C3 C7 H7B 109.7 . . ? C21 C7 H7B 109.7 . . ? H7A C7 H7B 108.2 . . ? O3 C8 N15 127.2(9) . . ? O3 C8 N6 125.5(9) . . ? N15 C8 N6 107.2(9) . . ? C31 C9 C4 111.2(9) . . ? C31 C9 H9A 109.4 . . ? C4 C9 H9A 109.4 . . ? C31 C9 H9B 109.4 . . ? C4 C9 H9B 109.4 . . ? H9A C9 H9B 108.0 . . ? C6 C10 C42 111.6(9) . . ? C6 C10 H10A 109.3 . . ? C42 C10 H10A 109.3 . . ? C6 C10 H10B 109.3 . . ? C42 C10 H10B 109.3 . . ? H10A C10 H10B 108.0 . . ? N17 C11 C28 118.6(10) . . ? N17 C11 N11 111.4(8) . . ? C28 C11 N11 111.0(9) . . ? N17 C11 C40 100.8(8) . . ? C28 C11 C40 111.7(9) . . ? N11 C11 C40 101.6(9) . . ? N5 C12 N4 113.4(9) . . ? N5 C12 H12A 108.9 . . ? N4 C12 H12A 108.9 . . ? N5 C12 H12B 108.9 . . ? N4 C12 H12B 108.9 . . ? H12A C12 H12B 107.7 . . ? N1 C13 N16 116.3(8) . . ? N1 C13 H13A 108.2 . . ? N16 C13 H13A 108.2 . . ? N1 C13 H13B 108.2 . . ? N16 C13 H13B 108.2 . . ? H13A C13 H13B 107.4 . . ? N1 C14 N3 115.7(8) . . ? N1 C14 C50 105.2(9) . . ? N3 C14 C50 104.1(8) . . ? N1 C14 C15 110.7(8) . . ? N3 C14 C15 108.5(9) . . ? C50 C14 C15 112.5(8) . . ? C2 C15 C14 108.9(9) . . ? C2 C15 H15A 109.9 . . ? C14 C15 H15A 109.9 . . ? C2 C15 H15B 109.9 . . ? C14 C15 H15B 109.9 . . ? H15A C15 H15B 108.3 . . ? N2 C16 N19 114.1(8) . . ? N2 C16 H16A 108.7 . . ? N19 C16 H16A 108.7 . . ? N2 C16 H16B 108.7 . . ? N19 C16 H16B 108.7 . . ? H16A C16 H16B 107.6 . . ? C2 C17 C29 112.1(9) . . ? C2 C17 H17A 109.2 . . ? C29 C17 H17A 109.2 . . ? C2 C17 H17B 109.2 . . ? C29 C17 H17B 109.2 . . ? H17A C17 H17B 107.9 . . ? N2 C18 N8 112.5(10) . . ? N2 C18 C21 105.2(10) . . ? N8 C18 C21 102.2(10) . . ? N2 C18 C39 112.1(11) . . ? N8 C18 C39 111.5(11) . . ? C21 C18 C39 112.7(11) . . ? N3 C19 N12 113.2(9) . . ? N3 C19 H19A 108.9 . . ? N12 C19 H19A 108.9 . . ? N3 C19 H19B 108.9 . . ? N12 C19 H19B 108.9 . . ? H19A C19 H19B 107.8 . . ? C4 C20 C35 108.0(10) . . ? C4 C20 H20A 110.1 . . ? C35 C20 H20A 110.1 . . ? C4 C20 H20B 110.1 . . ? C35 C20 H20B 110.1 . . ? H20A C20 H20B 108.4 . . ? N20 C21 C18 106.3(10) . . ? N20 C21 N9 112.3(8) . . ? C18 C21 N9 104.0(9) . . ? N20 C21 C7 110.4(9) . . ? C18 C21 C7 113.8(9) . . ? N9 C21 C7 109.8(9) . . ? N13 C22 N6 114.8(8) . . ? N13 C22 H22A 108.6 . . ? N6 C22 H22A 108.6 . . ? N13 C22 H22B 108.6 . . ? N6 C22 H22B 108.6 . . ? H22A C22 H22B 107.5 . . ? O6 C23 N10 125.2(10) . . ? O6 C23 N4 125.8(9) . . ? N10 C23 N4 108.7(10) . . ? O5 C24 N20 126.7(10) . . ? O5 C24 N8 121.0(11) . . ? N20 C24 N8 112.3(9) . . ? N11 C25 N9 113.5(9) . . ? N11 C25 H25A 108.9 . . ? N9 C25 H25A 108.9 . . ? N11 C25 H25B 108.9 . . ? N9 C25 H25B 108.9 . . ? H25A C25 H25B 107.7 . . ? O7 C26 N19 124.3(11) . . ? O7 C26 N5 123.1(11) . . ? N19 C26 N5 112.4(9) . . ? O9 C27 N2 125.2(11) . . ? O9 C27 N9 124.8(10) . . ? N2 C27 N9 110.0(10) . . ? C11 C28 C44 115.7(11) . . ? C11 C28 H28A 108.3 . . ? C44 C28 H28A 108.3 . . ? C11 C28 H28B 108.3 . . ? C44 C28 H28B 108.3 . . ? H28A C28 H28B 107.4 . . ? C50 C29 C17 113.4(9) . . ? C50 C29 H29A 108.9 . . ? C17 C29 H29A 108.9 . . ? C50 C29 H29B 108.9 . . ? C17 C29 H29B 108.9 . . ? H29A C29 H29B 107.7 . . ? C32 C30 C43 111.8(9) . . ? C32 C30 H30A 109.2 . . ? C43 C30 H30A 109.2 . . ? C32 C30 H30B 109.2 . . ? C43 C30 H30B 109.2 . . ? H30A C30 H30B 107.9 . . ? C9 C31 C46 112.0(10) . . ? C9 C31 H31A 109.2 . . ? C46 C31 H31A 109.2 . . ? C9 C31 H31B 109.2 . . ? C46 C31 H31B 109.2 . . ? H31A C31 H31B 107.9 . . ? N15 C32 N4 114.1(8) . . ? N15 C32 C30 115.0(9) . . ? N4 C32 C30 110.8(9) . . ? N15 C32 C42 102.2(7) . . ? N4 C32 C42 102.1(8) . . ? C30 C32 C42 111.6(8) . . ? O8 C33 N11 127.7(10) . . ? O8 C33 N16 122.3(10) . . ? N11 C33 N16 109.9(9) . . ? O4 C34 N12 128.3(10) . . ? O4 C34 N17 123.3(10) . . ? N12 C34 N17 108.4(9) . . ? N18 C35 C46 106.1(9) . . ? N18 C35 N5 112.0(7) . . ? C46 C35 N5 103.1(8) . . ? N18 C35 C20 112.8(8) . . ? C46 C35 C20 113.2(8) . . ? N5 C35 C20 109.3(9) . . ? O10 C36 N14 126.3(11) . . ? O10 C36 N1 124.6(11) . . ? N14 C36 N1 109.0(9) . . ? N10 C37 N14 116.0(10) . . ? N10 C37 H37A 108.3 . . ? N14 C37 H37A 108.3 . . ? N10 C37 H37B 108.3 . . ? N14 C37 H37B 108.3 . . ? H37A C37 H37B 107.4 . . ? N8 C38 N7 116.5(9) . . ? N8 C38 H38A 108.2 . . ? N7 C38 H38A 108.2 . . ? N8 C38 H38B 108.2 . . ? N7 C38 H38B 108.2 . . ? H38A C38 H38B 107.3 . . ? C47 C39 C18 105.7(10) . . ? C47 C39 H39A 110.6 . . ? C18 C39 H39A 110.6 . . ? C47 C39 H39B 110.6 . . ? C18 C39 H39B 110.6 . . ? H39A C39 H39B 108.7 . . ? N12 C40 N16 111.1(10) . . ? N12 C40 C11 103.9(8) . . ? N16 C40 C11 104.9(8) . . ? N12 C40 C1 113.5(9) . . ? N16 C40 C1 109.2(9) . . ? C11 C40 C1 113.9(10) . . ? O2 C41 N3 128.1(11) . . ? O2 C41 N13 122.7(10) . . ? N3 C41 N13 108.7(10) . . ? N6 C42 N10 115.7(10) . . ? N6 C42 C10 113.9(8) . . ? N10 C42 C10 109.7(8) . . ? N6 C42 C32 103.3(7) . . ? N10 C42 C32 103.2(7) . . ? C10 C42 C32 110.1(9) . . ? C6 C43 C30 108.0(11) . . ? C6 C43 H43A 110.1 . . ? C30 C43 H43A 110.1 . . ? C6 C43 H43B 110.1 . . ? C30 C43 H43B 110.1 . . ? H43A C43 H43B 108.4 . . ? C28 C44 C45 113.9(11) . . ? C28 C44 H44A 108.8 . . ? C45 C44 H44A 108.8 . . ? C28 C44 H44B 108.8 . . ? C45 C44 H44B 108.8 . . ? H44A C44 H44B 107.7 . . ? C1 C45 C44 114.2(10) . . ? C1 C45 H45A 108.7 . . ? C44 C45 H45A 108.7 . . ? C1 C45 H45B 108.7 . . ? C44 C45 H45B 108.7 . . ? H45A C45 H45B 107.6 . . ? N19 C46 N7 111.3(8) . . ? N19 C46 C35 105.6(8) . . ? N7 C46 C35 101.4(8) . . ? N19 C46 C31 114.2(8) . . ? N7 C46 C31 109.2(8) . . ? C35 C46 C31 114.4(9) . . ? C39 C47 C3 115.9(11) . . ? C39 C47 H47A 108.3 . . ? C3 C47 H47A 108.3 . . ? C39 C47 H47B 108.3 . . ? C3 C47 H47B 108.3 . . ? H47A C47 H47B 107.4 . . ? N18 C48 O1 124.2(10) . . ? N18 C48 N7 111.8(9) . . ? O1 C48 N7 123.7(11) . . ? N18 C49 N15 117.2(9) . . ? N18 C49 H49A 108.0 . . ? N15 C49 H49A 108.0 . . ? N18 C49 H49B 108.0 . . ? N15 C49 H49B 108.0 . . ? H49A C49 H49B 107.2 . . ? N14 C50 N13 114.2(8) . . ? N14 C50 C14 102.4(8) . . ? N13 C50 C14 101.9(8) . . ? N14 C50 C29 113.4(9) . . ? N13 C50 C29 111.4(8) . . ? C14 C50 C29 112.7(8) . . ? C59 C51 C64 108.9(12) . . ? C59 C51 H51A 109.9 . . ? C64 C51 H51A 109.9 . . ? C59 C51 H51B 109.9 . . ? C64 C51 H51B 109.9 . . ? H51A C51 H51B 108.3 . . ? C56 C52 C100 111.7(11) . . ? C56 C52 H52A 109.3 . . ? C100 C52 H52A 109.3 . . ? C56 C52 H52B 109.3 . . ? C100 C52 H52B 109.3 . . ? H52A C52 H52B 107.9 . . ? C93 C53 C73 110.9(10) . . ? C93 C53 H53A 109.5 . . ? C73 C53 H53A 109.5 . . ? C93 C53 H53B 109.5 . . ? C73 C53 H53B 109.5 . . ? H53A C53 H53B 108.0 . . ? C91 C54 C90 109.4(10) . . ? C91 C54 H54A 109.8 . . ? C90 C54 H54A 109.8 . . ? C91 C54 H54B 109.8 . . ? C90 C54 H54B 109.8 . . ? H54A C54 H54B 108.2 . . ? N36 C55 N30 112.4(9) . . ? N36 C55 C59 113.0(10) . . ? N30 C55 C59 112.9(10) . . ? N36 C55 C99 102.6(9) . . ? N30 C55 C99 104.3(9) . . ? C59 C55 C99 110.9(9) . . ? C52 C56 C83 111.1(11) . . ? C52 C56 H56A 109.4 . . ? C83 C56 H56A 109.4 . . ? C52 C56 H56B 109.4 . . ? C83 C56 H56B 109.4 . . ? H56A C56 H56B 108.0 . . ? C64 C57 C99 105.2(11) . . ? C64 C57 H57A 110.7 . . ? C99 C57 H57A 110.7 . . ? C64 C57 H57B 110.7 . . ? C99 C57 H57B 110.7 . . ? H57A C57 H57B 108.8 . . ? C66 C58 C60 114.0(10) . . ? C66 C58 H58A 108.8 . . ? C60 C58 H58A 108.8 . . ? C66 C58 H58B 108.8 . . ? C60 C58 H58B 108.8 . . ? H58A C58 H58B 107.7 . . ? C51 C59 C55 114.2(10) . . ? C51 C59 H59A 108.7 . . ? C55 C59 H59A 108.7 . . ? C51 C59 H59B 108.7 . . ? C55 C59 H59B 108.7 . . ? H59A C59 H59B 107.6 . . ? C75 C60 C58 109.0(10) . . ? C75 C60 H60A 109.9 . . ? C58 C60 H60A 109.9 . . ? C75 C60 H60B 109.9 . . ? C58 C60 H60B 109.9 . . ? H60A C60 H60B 108.3 . . ? N35 C61 N25 115.4(9) . . ? N35 C61 H61A 108.4 . . ? N25 C61 H61A 108.4 . . ? N35 C61 H61B 108.4 . . ? N25 C61 H61B 108.4 . . ? H61A C61 H61B 107.5 . . ? N40 C62 N34 114.8(10) . . ? N40 C62 H62A 108.6 . . ? N34 C62 H62A 108.6 . . ? N40 C62 H62B 108.6 . . ? N34 C62 H62B 108.6 . . ? H62A C62 H62B 107.5 . . ? N27 C63 N24 109.3(8) . . ? N27 C63 C66 114.1(9) . . ? N24 C63 C66 113.5(9) . . ? N27 C63 C92 102.8(8) . . ? N24 C63 C92 103.1(8) . . ? C66 C63 C92 113.0(9) . . ? C57 C64 C51 114.8(11) . . ? C57 C64 H64A 108.6 . . ? C51 C64 H64A 108.6 . . ? C57 C64 H64B 108.6 . . ? C51 C64 H64B 108.6 . . ? H64A C64 H64B 107.5 . . ? C72 C65 C68 110.1(13) . . ? C72 C65 H65A 109.6 . . ? C68 C65 H65A 109.6 . . ? C72 C65 H65B 109.6 . . ? C68 C65 H65B 109.6 . . ? H65A C65 H65B 108.2 . . ? C63 C66 C58 108.0(9) . . ? C63 C66 H66A 110.1 . . ? C58 C66 H66A 110.1 . . ? C63 C66 H66B 110.1 . . ? C58 C66 H66B 110.1 . . ? H66A C66 H66B 108.4 . . ? O13 C67 N32 130.7(10) . . ? O13 C67 N30 123.5(10) . . ? N32 C67 N30 105.6(11) . . ? N22 C68 C65 116.2(9) . . ? N22 C68 N34 109.1(9) . . ? C65 C68 N34 113.9(10) . . ? N22 C68 C91 102.8(8) . . ? C65 C68 C91 114.2(9) . . ? N34 C68 C91 98.9(8) . . ? N24 C69 N23 115.8(9) . . ? N24 C69 H69A 108.3 . . ? N23 C69 H69A 108.3 . . ? N24 C69 H69B 108.3 . . ? N23 C69 H69B 108.3 . . ? H69A C69 H69B 107.4 . . ? N37 C70 N36 113.8(8) . . ? N37 C70 H70A 108.8 . . ? N36 C70 H70A 108.8 . . ? N37 C70 H70B 108.8 . . ? N36 C70 H70B 108.8 . . ? H70A C70 H70B 107.7 . . ? O19 C71 N29 128.0(10) . . ? O19 C71 N38 121.1(10) . . ? N29 C71 N38 110.5(10) . . ? C65 C72 C90 119.1(16) . . ? C65 C72 H72A 107.5 . . ? C90 C72 H72A 107.5 . . ? C65 C72 H72B 107.5 . . ? C90 C72 H72B 107.5 . . ? H72A C72 H72B 107.0 . . ? C87 C73 C53 112.5(9) . . ? C87 C73 H73A 109.1 . . ? C53 C73 H73A 109.1 . . ? C87 C73 H73B 109.1 . . ? C53 C73 H73B 109.1 . . ? H73A C73 H73B 107.8 . . ? C100 C74 C85 110.8(9) . . ? C100 C74 H74A 109.5 . . ? C85 C74 H74A 109.5 . . ? C100 C74 H74B 109.5 . . ? C85 C74 H74B 109.5 . . ? H74A C74 H74B 108.1 . . ? C92 C75 C60 111.6(10) . . ? C92 C75 H75A 109.3 . . ? C60 C75 H75A 109.3 . . ? C92 C75 H75B 109.3 . . ? C60 C75 H75B 109.3 . . ? H75A C75 H75B 108.0 . . ? N30 C76 N33 112.6(8) . . ? N30 C76 H76A 109.1 . . ? N33 C76 H76A 109.1 . . ? N30 C76 H76B 109.1 . . ? N33 C76 H76B 109.1 . . ? H76A C76 H76B 107.8 . . ? N38 C77 N31 115.2(8) . . ? N38 C77 H77A 108.5 . . ? N31 C77 H77A 108.5 . . ? N38 C77 H77B 108.5 . . ? N31 C77 H77B 108.5 . . ? H77A C77 H77B 107.5 . . ? O15 C78 N39 129.2(11) . . ? O15 C78 N40 122.5(10) . . ? N39 C78 N40 108.3(9) . . ? N28 C79 N27 111.7(8) . . ? N28 C79 H79A 109.3 . . ? N27 C79 H79A 109.3 . . ? N28 C79 H79B 109.3 . . ? N27 C79 H79B 109.3 . . ? H79A C79 H79B 108.0 . . ? N22 C80 N29 113.6(8) . . ? N22 C80 H80A 108.8 . . ? N29 C80 H80A 108.8 . . ? N22 C80 H80B 108.8 . . ? N29 C80 H80B 108.8 . . ? H80A C80 H80B 107.7 . . ? O16 C81 N36 124.9(9) . . ? O16 C81 N25 124.1(10) . . ? N36 C81 N25 111.0(10) . . ? N32 C82 N21 113.2(8) . . ? N32 C82 H82A 108.9 . . ? N21 C82 H82A 108.9 . . ? N32 C82 H82B 108.9 . . ? N21 C82 H82B 108.9 . . ? H82A C82 H82B 107.7 . . ? N40 C83 N29 111.8(8) . . ? N40 C83 C56 114.9(9) . . ? N29 C83 C56 113.4(9) . . ? N40 C83 C85 104.8(8) . . ? N29 C83 C85 99.3(8) . . ? C56 C83 C85 111.2(8) . . ? O17 C84 N37 124.0(11) . . ? O17 C84 N31 123.4(12) . . ? N37 C84 N31 112.5(10) . . ? N38 C85 N39 112.8(9) . . ? N38 C85 C74 113.2(8) . . ? N39 C85 C74 113.5(8) . . ? N38 C85 C83 103.7(8) . . ? N39 C85 C83 100.8(7) . . ? C74 C85 C83 111.7(9) . . ? O14 C86 N23 125.6(10) . . ? O14 C86 N34 123.8(10) . . ? N23 C86 N34 110.6(11) . . ? C94 C87 C73 111.3(8) . . ? C94 C87 H87A 109.4 . . ? C73 C87 H87A 109.4 . . ? C94 C87 H87B 109.4 . . ? C73 C87 H87B 109.4 . . ? H87A C87 H87B 108.0 . . ? N26 C88 N39 113.1(8) . . ? N26 C88 H88A 109.0 . . ? N39 C88 H88A 109.0 . . ? N26 C88 H88B 109.0 . . ? N39 C88 H88B 109.0 . . ? H88A C88 H88B 107.8 . . ? O20 C89 N27 124.9(12) . . ? O20 C89 N35 127.2(11) . . ? N27 C89 N35 107.8(9) . . ? C72 C90 C54 107.2(16) . . ? C72 C90 H90A 110.3 . . ? C54 C90 H90A 110.3 . . ? C72 C90 H90B 110.3 . . ? C54 C90 H90B 110.3 . . ? H90A C90 H90B 108.5 . . ? N28 C91 N23 116.8(8) . . ? N28 C91 C54 117.1(9) . . ? N23 C91 C54 109.4(9) . . ? N28 C91 C68 101.0(8) . . ? N23 C91 C68 102.7(8) . . ? C54 C91 C68 108.1(9) . . ? N21 C92 N35 111.7(7) . . ? N21 C92 C75 114.1(9) . . ? N35 C92 C75 110.7(9) . . ? N21 C92 C63 101.8(9) . . ? N35 C92 C63 103.5(8) . . ? C75 C92 C63 114.3(8) . . ? C98 C93 C53 111.1(9) . . ? C98 C93 H93A 109.4 . . ? C53 C93 H93A 109.4 . . ? C98 C93 H93B 109.4 . . ? C53 C93 H93B 109.4 . . ? H93A C93 H93B 108.0 . . ? N31 C94 N26 112.6(8) . . ? N31 C94 C87 115.1(8) . . ? N26 C94 C87 113.2(8) . . ? N31 C94 C98 101.5(8) . . ? N26 C94 C98 102.4(7) . . ? C87 C94 C98 110.5(8) . . ? O12 C95 N21 124.5(10) . . ? O12 C95 N24 123.4(10) . . ? N21 C95 N24 112.0(9) . . ? O11 C96 N26 124.5(10) . . ? O11 C96 N33 126.4(10) . . ? N26 C96 N33 108.8(8) . . ? O18 C97 N28 128.4(10) . . ? O18 C97 N22 121.6(9) . . ? N28 C97 N22 109.8(10) . . ? N33 C98 C93 116.1(10) . . ? N33 C98 N37 113.3(8) . . ? C93 C98 N37 112.0(9) . . ? N33 C98 C94 101.1(8) . . ? C93 C98 C94 111.9(8) . . ? N37 C98 C94 100.8(8) . . ? N25 C99 N32 109.6(9) . . ? N25 C99 C57 112.8(10) . . ? N32 C99 C57 113.6(9) . . ? N25 C99 C55 103.2(8) . . ? N32 C99 C55 100.2(9) . . ? C57 C99 C55 116.3(9) . . ? C74 C100 C52 114.3(10) . . ? C74 C100 H10C 108.7 . . ? C52 C100 H10C 108.7 . . ? C74 C100 H10D 108.7 . . ? C52 C100 H10D 108.7 . . ? H10C C100 H10D 107.6 . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 1.845 _refine_diff_density_min -1.831 _refine_diff_density_rms 0.182 # Attachment '- Nd.cif' data_o _database_code_depnum_ccdc_archive 'CCDC 883409' #TrackingRef '- Nd.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H92 Cl2 N21 Nd O29' _chemical_formula_weight 1666.59 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' Cl Cl 0.1484 0.1585 '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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 26.971(4) _cell_length_b 18.358(3) _cell_length_c 30.331(7) _cell_angle_alpha 90.00 _cell_angle_beta 114.565(2) _cell_angle_gamma 90.00 _cell_volume 13659(4) _cell_formula_units_Z 8 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 7379 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 22.52 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.621 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6920 _exptl_absorpt_coefficient_mu 0.940 _exptl_absorpt_correction_type 'multi scan' _exptl_absorpt_correction_T_min 0.7406 _exptl_absorpt_correction_T_max 0.8271 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 Apex CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 57188 _diffrn_reflns_av_R_equivalents 0.0785 _diffrn_reflns_av_sigmaI/netI 0.0632 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 25.20 _reflns_number_total 12063 _reflns_number_gt 8994 _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. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.047 0.397 -0.061 4495 2015 ' ' 2 0.000 0.408 0.250 68 51 ' ' 3 0.000 0.604 0.250 5 0 ' ' 4 0.000 0.592 0.750 69 39 ' ' 5 0.000 0.396 0.750 5 0 ' ' 6 0.212 0.142 0.178 48 7 ' ' 7 0.212 0.858 0.678 48 9 ' ' 8 0.288 0.642 0.322 48 7 ' ' 9 0.288 0.358 0.822 48 7 ' ' 10 0.500 0.908 0.250 68 51 ' ' 11 0.500 0.092 0.750 69 39 ' ' 12 0.500 0.104 0.250 5 0 ' ' 13 0.500 0.896 0.750 5 0 ' ' 14 0.712 0.642 0.178 48 7 ' ' 15 0.712 0.358 0.678 48 9 ' ' 16 0.788 0.142 0.322 48 7 ' ' 17 0.788 0.858 0.822 48 7 ' ' _platon_squeeze_details ; ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1650P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12063 _refine_ls_number_parameters 766 _refine_ls_number_restraints 144 _refine_ls_R_factor_all 0.0931 _refine_ls_R_factor_gt 0.0762 _refine_ls_wR_factor_ref 0.2296 _refine_ls_wR_factor_gt 0.2158 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nd1 Nd 0.688753(10) 0.609021(14) 0.753150(10) 0.02923(9) Uani 1 1 d . . . Cl1 Cl 0.66917(11) 0.58488(17) 0.66940(10) 0.0999(8) Uani 1 1 d . . . Cl2 Cl 0.75441(11) 0.63377(17) 0.83370(9) 0.0981(8) Uani 1 1 d . . . O1W O 0.58788(13) 0.60020(18) 0.70365(12) 0.0269(8) Uani 1 1 d . . . O2W O 0.64124(15) 0.61578(18) 0.80803(13) 0.0339(9) Uani 1 1 d . . . O1 O 0.92068(13) 0.97256(16) 0.84407(11) 0.0225(7) Uani 1 1 d . . . O2 O 0.87226(12) 1.01398(17) 0.91944(11) 0.0222(7) Uani 1 1 d . . . O3 O 0.75193(11) 1.06153(15) 0.86059(10) 0.0165(7) Uani 1 1 d . . . O4 O 0.83123(10) 0.98717(14) 0.73476(10) 0.0122(6) Uani 1 1 d . . . O5 O 0.73397(10) 1.03564(14) 0.74566(9) 0.0103(6) Uani 1 1 d . . . O6 O 0.81173(12) 0.69796(16) 0.92574(11) 0.0224(7) Uani 1 1 d . . . O7 O 0.68892(12) 0.74435(16) 0.85661(11) 0.0212(7) Uani 1 1 d . . . O8 O 0.85979(11) 0.65689(15) 0.85466(10) 0.0148(6) Uani 1 1 d . . . O9 O 0.65531(10) 0.72952(15) 0.74255(10) 0.0131(6) Uani 1 1 d . . . O10 O 0.75755(10) 0.68420(14) 0.74209(9) 0.0120(6) Uani 1 1 d . . . N1 N 0.83341(13) 0.93860(19) 0.95698(12) 0.0141(8) Uani 1 1 d . . . N2 N 0.80740(13) 0.8115(2) 0.95547(12) 0.0164(8) Uani 1 1 d . . . N3 N 0.92651(12) 0.85826(18) 0.81423(11) 0.0095(6) Uani 1 1 d U . . N4 N 0.85899(11) 0.87024(17) 0.73084(10) 0.0058(6) Uani 1 1 d U . . N5 N 0.73884(13) 0.97127(18) 0.90786(12) 0.0132(8) Uani 1 1 d . . . N6 N 0.94545(13) 0.87055(19) 0.89184(12) 0.0137(8) Uani 1 1 d . . . N7 N 0.65022(13) 0.85751(18) 0.83129(11) 0.0104(7) Uani 1 1 d . . . N8 N 0.92283(13) 0.74378(19) 0.89673(12) 0.0143(8) Uani 1 1 d . . . N9 N 0.74357(12) 0.77666(17) 0.68665(10) 0.0066(6) Uani 1 1 d U . . N10 N 0.71352(13) 0.84468(18) 0.90553(12) 0.0134(8) Uani 1 1 d . . . N11 N 0.62901(12) 0.84779(16) 0.74518(11) 0.0066(7) Uani 1 1 d . . . N12 N 0.69153(11) 0.94238(17) 0.69178(10) 0.0057(6) Uani 1 1 d U . . N13 N 0.67932(12) 0.98248(18) 0.83198(11) 0.0090(6) Uani 1 1 d U . . N14 N 0.66055(12) 0.81885(17) 0.69084(11) 0.0076(6) Uani 1 1 d U . . N15 N 0.89841(12) 0.73413(17) 0.81816(11) 0.0070(6) Uani 1 1 d U . . N16 N 0.66035(12) 0.97144(17) 0.74641(11) 0.0075(7) Uani 1 1 d . . . N17 N 0.90785(14) 0.9009(2) 0.94899(12) 0.0172(9) Uani 1 1 d . . . N18 N 0.82820(12) 0.74729(17) 0.73627(11) 0.0064(6) Uani 1 1 d U . . N19 N 0.77359(12) 0.90042(16) 0.68525(11) 0.0064(6) Uani 1 1 d U . . N20 N 0.88557(13) 0.7746(2) 0.95537(12) 0.0161(8) Uani 1 1 d . . . C1 C 1.01907(17) 0.7772(3) 0.91862(15) 0.0226(11) Uani 1 1 d . . . H1A H 1.0416 0.8135 0.9125 0.027 Uiso 1 1 calc R . . H1B H 1.0266 0.7793 0.9528 0.027 Uiso 1 1 calc R . . C2 C 0.55799(18) 1.0018(3) 0.65901(16) 0.0232(11) Uani 1 1 d . . . H2A H 0.5197 1.0147 0.6424 0.028 Uiso 1 1 calc R . . H2B H 0.5774 1.0444 0.6768 0.028 Uiso 1 1 calc R . . C3 C 0.92179(16) 0.7273(2) 0.94367(13) 0.0125(9) Uani 1 1 d . . . H3A H 0.9103 0.6772 0.9434 0.015 Uiso 1 1 calc R . . H3B H 0.9585 0.7318 0.9689 0.015 Uiso 1 1 calc R . . C4 C 0.83287(16) 0.7550(2) 0.94353(13) 0.0148(9) Uani 1 1 d . . . C5 C 0.85171(18) 0.8764(3) 1.03435(15) 0.0203(7) Uani 1 1 d U . . H5A H 0.8185 0.8963 1.0345 0.024 Uiso 1 1 calc R . . H5B H 0.8573 0.8285 1.0491 0.024 Uiso 1 1 calc R . . C6 C 0.56390(15) 0.9407(2) 0.69518(14) 0.0116(7) Uani 1 1 d U . . H6A H 0.5532 0.9584 0.7201 0.014 Uiso 1 1 calc R . . H6B H 0.5401 0.9005 0.6786 0.014 Uiso 1 1 calc R . . C7 C 0.94703(19) 0.8417(3) 1.02882(15) 0.0244(11) Uani 1 1 d . . . H7A H 0.9426 0.8000 1.0465 0.029 Uiso 1 1 calc R . . H7B H 0.9807 0.8355 1.0250 0.029 Uiso 1 1 calc R . . C8 C 0.68420(15) 0.8084(2) 0.86307(13) 0.0127(9) Uani 1 1 d . . . C9 C 0.76373(16) 0.8164(2) 0.61827(13) 0.0119(9) Uani 1 1 d . . . H9A H 0.7855 0.8508 0.6097 0.014 Uiso 1 1 calc R . . H9B H 0.7256 0.8272 0.5988 0.014 Uiso 1 1 calc R . . C10 C 0.87083(17) 0.9566(2) 0.93949(14) 0.0173(10) Uani 1 1 d U . . C11 C 0.95385(17) 0.9080(2) 0.93643(14) 0.0168(10) Uani 1 1 d . . . H11A H 0.9861 0.8884 0.9626 0.020 Uiso 1 1 calc R . . H11B H 0.9603 0.9592 0.9331 0.020 Uiso 1 1 calc R . . C12 C 0.82148(14) 0.9241(2) 0.71815(13) 0.0087(8) Uani 1 1 d . . . C13 C 0.72634(14) 1.0103(2) 0.86568(13) 0.0094(7) Uani 1 1 d U . . C15 C 0.62252(14) 0.9145(2) 0.71836(13) 0.0074(6) Uani 1 1 d U . . C16 C 0.77505(14) 0.7315(2) 0.72368(12) 0.0057(8) Uani 1 1 d . . . C17 C 0.57918(18) 0.9825(2) 0.62183(16) 0.0218(11) Uani 1 1 d . . . H17A H 0.6074 1.0169 0.6240 0.026 Uiso 1 1 calc R . . H17B H 0.5498 0.9868 0.5897 0.026 Uiso 1 1 calc R . . C18 C 0.64936(14) 0.7931(2) 0.72769(13) 0.0080(8) Uani 1 1 d . . . C19 C 0.89923(15) 0.8452(2) 0.97891(13) 0.0129(9) Uani 1 1 d . . . C20 C 0.83360(16) 0.7146(2) 0.64083(14) 0.0153(9) Uani 1 1 d U . . H20A H 0.8527 0.7000 0.6213 0.018 Uiso 1 1 calc R . . H20B H 0.8311 0.6724 0.6590 0.018 Uiso 1 1 calc R . . C21 C 0.78887(16) 0.9877(2) 0.95096(14) 0.0153(10) Uani 1 1 d . . . H21A H 0.8000 1.0372 0.9486 0.018 Uiso 1 1 calc R . . H21B H 0.7812 0.9848 0.9795 0.018 Uiso 1 1 calc R . . C22 C 0.59914(15) 0.9559(2) 0.84936(14) 0.0132(9) Uani 1 1 d . . . H22A H 0.5825 0.9172 0.8603 0.016 Uiso 1 1 calc R . . H22B H 0.5748 0.9677 0.8162 0.016 Uiso 1 1 calc R . . C23 C 0.61095(14) 0.8347(2) 0.78364(13) 0.0099(8) Uani 1 1 d . . . H23A H 0.5770 0.8606 0.7759 0.012 Uiso 1 1 calc R . . H23B H 0.6037 0.7831 0.7846 0.012 Uiso 1 1 calc R . . C24 C 0.99094(14) 0.7582(2) 0.82267(13) 0.0092(8) Uani 1 1 d . . . H24A H 1.0184 0.7961 0.8306 0.011 Uiso 1 1 calc R . . H24B H 0.9783 0.7471 0.7885 0.011 Uiso 1 1 calc R . . C25 C 0.83614(13) 0.80214(19) 0.70516(12) 0.0042(6) Uani 1 1 d U . . C26 C 0.65424(14) 1.0161(2) 0.78357(12) 0.0068(6) Uani 1 1 d U . . H26A H 0.6158 1.0239 0.7749 0.008 Uiso 1 1 calc R . . H26B H 0.6709 1.0633 0.7846 0.008 Uiso 1 1 calc R . . C27 C 0.69758(15) 0.9206(2) 0.90528(14) 0.0132(9) Uani 1 1 d . . . C28 C 0.88992(14) 0.7071(2) 0.85656(13) 0.0093(6) Uani 1 1 d U . . C29 C 0.60245(15) 0.9052(2) 0.62852(14) 0.0102(9) Uani 1 1 d . . . H29A H 0.5732 0.8701 0.6215 0.012 Uiso 1 1 calc R . . H29B H 0.6190 0.8969 0.6060 0.012 Uiso 1 1 calc R . . C30 C 0.92966(16) 0.9064(2) 0.84936(14) 0.0156(10) Uani 1 1 d . . . C31 C 0.86683(15) 0.7735(2) 0.67645(14) 0.0114(9) Uani 1 1 d . . . H31A H 0.9016 0.7535 0.6986 0.014 Uiso 1 1 calc R . . H31B H 0.8739 0.8133 0.6588 0.014 Uiso 1 1 calc R . . C32 C 0.69892(14) 0.9869(2) 0.72945(12) 0.0056(6) Uani 1 1 d U . . C33 C 0.84494(16) 0.8691(2) 0.98189(13) 0.0136(9) Uani 1 1 d . . . C34 C 0.95893(14) 0.7949(2) 0.88836(14) 0.0111(9) Uani 1 1 d . . . C35 C 0.91536(14) 0.8811(2) 0.76516(13) 0.0066(8) Uani 1 1 d U . . H35A H 0.9390 0.8542 0.7540 0.008 Uiso 1 1 calc R . . H35B H 0.9243 0.9324 0.7656 0.008 Uiso 1 1 calc R . . C36 C 0.87147(15) 0.7019(2) 0.77063(13) 0.0081(6) Uani 1 1 d U . . H36A H 0.8561 0.6554 0.7737 0.010 Uiso 1 1 calc R . . H36B H 0.8983 0.6926 0.7578 0.010 Uiso 1 1 calc R . . C37 C 0.77582(13) 0.8246(2) 0.67118(12) 0.0052(8) Uani 1 1 d . . . C38 C 0.72576(14) 0.9467(2) 0.66509(13) 0.0071(6) Uani 1 1 d U . . H38A H 0.7043 0.9327 0.6317 0.009 Uiso 1 1 calc R . . H38B H 0.7373 0.9968 0.6652 0.009 Uiso 1 1 calc R . . C39 C 0.77635(17) 0.7389(2) 0.60733(15) 0.0188(10) Uani 1 1 d . . . H39A H 0.7502 0.7055 0.6106 0.023 Uiso 1 1 calc R . . H39B H 0.7723 0.7365 0.5740 0.023 Uiso 1 1 calc R . . C40 C 0.68472(14) 0.7739(2) 0.66590(13) 0.0072(8) Uani 1 1 d . . . H40A H 0.6708 0.7894 0.6323 0.009 Uiso 1 1 calc R . . H40B H 0.6734 0.7239 0.6663 0.009 Uiso 1 1 calc R . . C41 C 0.65316(15) 0.9296(2) 0.85100(13) 0.0084(8) Uani 1 1 d . . . C43 C 0.94340(14) 0.7858(2) 0.83267(13) 0.0095(9) Uani 1 1 d . . . C44 C 0.64458(14) 0.89451(19) 0.67970(13) 0.0054(8) Uani 1 1 d U . . C45 C 0.9504(2) 0.9096(3) 1.05720(18) 0.0356(14) Uani 1 1 d . . . H45A H 0.9578 0.9506 1.0406 0.043 Uiso 1 1 calc R . . H45B H 0.9807 0.9053 1.0887 0.043 Uiso 1 1 calc R . . C46 C 0.6485(2) 1.0111(3) 0.93360(17) 0.0349(13) Uani 1 1 d . . . H46A H 0.6771 1.0473 0.9416 0.042 Uiso 1 1 calc R . . H46B H 0.6309 1.0179 0.9554 0.042 Uiso 1 1 calc R . . C47 C 1.0339(2) 0.7021(3) 0.90675(17) 0.0355(13) Uani 1 1 d . . . H47A H 1.0168 0.6655 0.9189 0.043 Uiso 1 1 calc R . . H47B H 1.0731 0.6957 0.9233 0.043 Uiso 1 1 calc R . . C48 C 0.8992(2) 0.9251(3) 1.06418(17) 0.0346(13) Uani 1 1 d . . . H48A H 0.8888 0.9755 1.0556 0.042 Uiso 1 1 calc R . . H48B H 0.9070 0.9191 1.0982 0.042 Uiso 1 1 calc R . . C49 C 0.67402(18) 0.9359(3) 0.94168(15) 0.0213(10) Uani 1 1 d U . . H49A H 0.7026 0.9328 0.9742 0.026 Uiso 1 1 calc R . . H49B H 0.6466 0.8996 0.9385 0.026 Uiso 1 1 calc R . . C50 C 0.60671(18) 1.0235(3) 0.88154(16) 0.0222(10) Uani 1 1 d . . . H50A H 0.6184 1.0641 0.8677 0.027 Uiso 1 1 calc R . . H50B H 0.5720 1.0364 0.8818 0.027 Uiso 1 1 calc R . . C14 C 1.01623(17) 0.6902(2) 0.85242(15) 0.0191(10) Uani 1 1 d . . . H14A H 1.0477 0.6758 0.8467 0.023 Uiso 1 1 calc R . . H14B H 0.9900 0.6508 0.8416 0.023 Uiso 1 1 calc R . . C42 C 0.75097(15) 0.8065(2) 0.94810(14) 0.0134(9) Uani 1 1 d . . . H42A H 0.7475 0.8261 0.9764 0.016 Uiso 1 1 calc R . . H42B H 0.7406 0.7555 0.9454 0.016 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd1 0.03052(14) 0.02142(16) 0.03775(16) 0.00071(11) 0.01618(12) 0.00031(10) Cl1 0.0915(15) 0.1138(19) 0.0914(15) -0.0105(14) 0.0352(13) -0.0010(15) Cl2 0.0937(15) 0.1079(18) 0.0892(15) -0.0050(14) 0.0345(13) -0.0024(15) O1W 0.0191(15) 0.0256(18) 0.0327(17) -0.0017(14) 0.0075(13) 0.0041(13) O2W 0.0524(19) 0.0230(18) 0.0443(18) -0.0030(14) 0.0380(15) -0.0038(15) O1 0.0374(16) 0.0059(14) 0.0233(15) -0.0015(12) 0.0117(13) 0.0052(13) O2 0.0290(15) 0.0173(16) 0.0212(14) 0.0035(12) 0.0114(12) 0.0042(13) O3 0.0164(12) 0.0104(14) 0.0245(14) 0.0018(11) 0.0105(11) 0.0002(11) O4 0.0125(12) 0.0035(13) 0.0197(13) -0.0032(11) 0.0059(11) 0.0003(11) O5 0.0127(12) 0.0046(13) 0.0171(12) -0.0049(10) 0.0095(10) -0.0025(10) O6 0.0306(15) 0.0126(15) 0.0240(15) -0.0036(12) 0.0113(13) 0.0047(13) O7 0.0287(15) 0.0082(14) 0.0236(15) -0.0023(12) 0.0077(12) 0.0083(12) O8 0.0167(12) 0.0150(15) 0.0144(13) 0.0034(11) 0.0080(11) 0.0023(11) O9 0.0158(12) 0.0080(14) 0.0191(13) 0.0006(11) 0.0106(11) -0.0008(11) O10 0.0125(12) 0.0061(13) 0.0158(13) 0.0068(11) 0.0042(11) 0.0022(11) N1 0.0165(15) 0.0132(17) 0.0116(15) 0.0022(13) 0.0047(13) 0.0084(14) N2 0.0133(15) 0.0204(19) 0.0133(15) -0.0040(14) 0.0034(13) 0.0057(14) N3 0.0100(8) 0.0083(9) 0.0093(8) -0.0003(7) 0.0031(6) 0.0019(7) N4 0.0054(8) 0.0046(8) 0.0070(8) -0.0004(7) 0.0022(6) -0.0003(7) N5 0.0118(15) 0.0109(17) 0.0132(15) 0.0007(13) 0.0014(13) 0.0016(13) N6 0.0174(15) 0.0103(17) 0.0137(15) -0.0066(13) 0.0069(13) -0.0007(14) N7 0.0165(15) 0.0051(16) 0.0092(14) -0.0029(12) 0.0048(12) 0.0045(13) N8 0.0183(15) 0.0141(17) 0.0114(15) 0.0017(13) 0.0071(13) 0.0020(14) N9 0.0065(8) 0.0055(9) 0.0072(8) 0.0006(7) 0.0025(6) 0.0006(7) N10 0.0191(15) 0.0073(16) 0.0135(15) 0.0024(13) 0.0064(13) 0.0082(13) N11 0.0117(13) 0.0011(15) 0.0091(14) -0.0003(11) 0.0066(11) -0.0005(12) N12 0.0052(8) 0.0052(9) 0.0078(8) 0.0003(7) 0.0038(6) 0.0002(7) N13 0.0098(8) 0.0094(9) 0.0092(8) 0.0013(7) 0.0053(6) -0.0001(7) N14 0.0086(8) 0.0056(9) 0.0082(8) -0.0008(7) 0.0032(6) 0.0013(7) N15 0.0064(8) 0.0080(9) 0.0073(8) 0.0002(7) 0.0034(6) 0.0002(7) N16 0.0090(13) 0.0034(15) 0.0113(14) -0.0016(12) 0.0052(12) -0.0025(12) N17 0.0164(16) 0.0202(19) 0.0098(15) -0.0015(14) 0.0004(13) 0.0098(14) N18 0.0058(8) 0.0058(9) 0.0079(8) 0.0005(7) 0.0031(6) 0.0014(7) N19 0.0064(8) 0.0050(9) 0.0085(8) 0.0004(7) 0.0037(6) 0.0008(7) N20 0.0181(16) 0.0175(19) 0.0123(15) -0.0042(14) 0.0059(13) 0.0041(14) C1 0.0129(19) 0.035(3) 0.0130(19) -0.0028(19) -0.0018(16) 0.0107(19) C2 0.021(2) 0.017(2) 0.027(2) 0.0036(18) 0.0043(18) 0.0155(18) C3 0.0184(18) 0.015(2) 0.0062(16) 0.0064(15) 0.0069(14) 0.0112(16) C4 0.0156(18) 0.023(2) 0.0079(17) 0.0037(16) 0.0072(15) 0.0075(17) C5 0.0219(9) 0.0214(10) 0.0185(10) -0.0003(8) 0.0093(7) 0.0013(8) C6 0.0103(9) 0.0119(9) 0.0130(9) -0.0008(7) 0.0052(6) 0.0017(7) C7 0.025(2) 0.032(3) 0.0091(19) 0.0006(18) -0.0004(17) 0.009(2) C8 0.0180(17) 0.014(2) 0.0105(17) 0.0034(15) 0.0107(14) 0.0026(16) C9 0.0194(18) 0.013(2) 0.0027(16) 0.0002(14) 0.0040(14) 0.0070(16) C10 0.0183(17) 0.024(2) 0.0079(16) -0.0042(15) 0.0035(14) 0.0090(16) C11 0.0183(19) 0.018(2) 0.0136(18) -0.0097(17) 0.0065(16) -0.0005(17) C12 0.0137(16) 0.0061(19) 0.0119(16) 0.0029(14) 0.0108(14) 0.0009(15) C13 0.0102(9) 0.0088(9) 0.0097(9) -0.0012(7) 0.0045(6) 0.0015(7) C15 0.0077(9) 0.0064(9) 0.0081(9) -0.0008(7) 0.0032(6) 0.0002(7) C16 0.0062(15) 0.0056(18) 0.0057(15) -0.0014(14) 0.0028(13) -0.0007(14) C17 0.020(2) 0.019(2) 0.023(2) 0.0081(18) 0.0062(17) 0.0073(18) C18 0.0062(15) 0.0032(18) 0.0153(17) -0.0012(14) 0.0052(14) 0.0003(14) C19 0.0135(17) 0.015(2) 0.0087(17) -0.0020(15) 0.0030(15) 0.0079(16) C20 0.0192(17) 0.0144(19) 0.0135(16) -0.0056(15) 0.0080(14) 0.0051(15) C21 0.0154(18) 0.017(2) 0.0080(17) -0.0050(16) -0.0011(15) 0.0047(17) C22 0.0122(16) 0.015(2) 0.0175(18) 0.0013(16) 0.0111(15) 0.0060(16) C23 0.0085(15) 0.0124(19) 0.0111(17) 0.0016(15) 0.0062(14) -0.0033(15) C24 0.0063(15) 0.0072(18) 0.0136(17) 0.0029(15) 0.0037(14) 0.0032(14) C25 0.0044(8) 0.0034(9) 0.0049(8) -0.0003(7) 0.0021(6) -0.0003(7) C26 0.0080(9) 0.0067(9) 0.0068(9) -0.0003(7) 0.0042(6) 0.0014(7) C27 0.0146(17) 0.013(2) 0.0120(17) 0.0009(16) 0.0052(15) 0.0071(16) C28 0.0090(9) 0.0092(9) 0.0092(9) -0.0003(7) 0.0033(6) 0.0020(7) C29 0.0058(16) 0.0120(19) 0.0109(17) -0.0005(15) 0.0016(14) 0.0049(15) C30 0.0099(17) 0.020(2) 0.0150(19) -0.0035(17) 0.0031(15) -0.0015(17) C31 0.0134(16) 0.0100(19) 0.0169(18) 0.0012(15) 0.0125(14) 0.0044(15) C32 0.0060(8) 0.0048(9) 0.0057(9) 0.0003(7) 0.0021(6) 0.0008(7) C33 0.0210(19) 0.012(2) 0.0076(17) 0.0015(15) 0.0054(15) 0.0064(17) C34 0.0068(16) 0.012(2) 0.0133(17) -0.0006(15) 0.0029(14) 0.0029(15) C35 0.0054(14) 0.0059(17) 0.0089(15) 0.0015(13) 0.0033(12) -0.0021(13) C36 0.0081(9) 0.0061(9) 0.0084(9) -0.0004(7) 0.0017(6) 0.0010(7) C37 0.0037(15) 0.0052(17) 0.0058(16) 0.0015(14) 0.0011(13) 0.0028(14) C38 0.0073(9) 0.0067(9) 0.0072(9) 0.0015(7) 0.0029(6) 0.0006(7) C39 0.0214(19) 0.016(2) 0.023(2) -0.0057(17) 0.0136(17) 0.0057(17) C40 0.0032(15) 0.0077(18) 0.0083(16) -0.0017(14) 0.0001(13) 0.0016(14) C41 0.0144(16) 0.0060(18) 0.0069(16) 0.0015(14) 0.0065(14) -0.0001(15) C43 0.0032(15) 0.0113(19) 0.0104(17) 0.0005(15) -0.0006(14) 0.0025(15) C44 0.0052(14) 0.0058(17) 0.0083(15) 0.0014(13) 0.0059(12) -0.0002(13) C45 0.031(3) 0.052(3) 0.016(2) -0.010(2) 0.001(2) -0.005(2) C46 0.030(2) 0.046(3) 0.028(2) -0.012(2) 0.012(2) 0.020(2) C47 0.037(2) 0.048(3) 0.024(2) 0.015(2) 0.0156(19) 0.036(2) C48 0.050(3) 0.032(3) 0.017(2) -0.008(2) 0.010(2) 0.010(2) C49 0.0267(18) 0.030(2) 0.0158(17) -0.0017(16) 0.0170(15) 0.0062(17) C50 0.025(2) 0.019(2) 0.029(2) -0.0023(18) 0.0178(18) 0.0070(18) C14 0.0149(18) 0.014(2) 0.028(2) 0.0019(18) 0.0086(17) 0.0108(17) C42 0.0159(17) 0.014(2) 0.0142(18) 0.0072(15) 0.0105(15) 0.0067(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd1 O9 2.360(3) . ? Nd1 O4 2.365(3) 4_646 ? Nd1 Cl2 2.390(3) . ? Nd1 Cl1 2.411(3) . ? Nd1 O10 2.445(3) . ? Nd1 O5 2.469(3) 4_646 ? Nd1 O2W 2.490(4) . ? Nd1 O1W 2.507(3) . ? O1 C30 1.235(5) . ? O2 C10 1.225(6) . ? O3 C13 1.213(5) . ? O4 C12 1.246(5) . ? O4 Nd1 2.365(3) 4_656 ? O5 C32 1.245(4) . ? O5 Nd1 2.469(3) 4_656 ? O6 C4 1.208(5) . ? O7 C8 1.208(5) . ? O8 C28 1.214(5) . ? O9 C18 1.237(5) . ? O10 C16 1.228(5) . ? N1 C10 1.362(6) . ? N1 C33 1.449(5) . ? N1 C21 1.451(5) . ? N2 C4 1.373(6) . ? N2 C42 1.446(5) . ? N2 C33 1.453(5) . ? N3 C30 1.360(5) . ? N3 C43 1.442(5) . ? N3 C35 1.453(5) . ? N4 C12 1.352(5) . ? N4 C35 1.456(4) . ? N4 C25 1.466(5) . ? N5 C13 1.381(5) . ? N5 C27 1.427(6) . ? N5 C21 1.468(5) . ? N6 C30 1.349(5) . ? N6 C11 1.448(5) . ? N6 C34 1.451(5) . ? N7 C8 1.359(5) . ? N7 C41 1.441(5) . ? N7 C23 1.454(5) . ? N8 C28 1.352(5) . ? N8 C34 1.449(6) . ? N8 C3 1.467(5) . ? N9 C16 1.370(5) . ? N9 C40 1.445(4) . ? N9 C37 1.446(5) . ? N10 C8 1.371(5) . ? N10 C42 1.447(5) . ? N10 C27 1.457(5) . ? N11 C18 1.354(5) . ? N11 C15 1.441(5) . ? N11 C23 1.459(5) . ? N12 C32 1.350(5) . ? N12 C44 1.458(5) . ? N12 C38 1.461(5) . ? N13 C13 1.355(5) . ? N13 C41 1.453(5) . ? N13 C26 1.473(5) . ? N14 C18 1.358(5) . ? N14 C40 1.445(5) . ? N14 C44 1.452(5) . ? N15 C28 1.370(5) . ? N15 C36 1.444(5) . ? N15 C43 1.456(5) . ? N16 C32 1.368(5) . ? N16 C26 1.458(5) . ? N16 C15 1.461(5) . ? N17 C10 1.374(6) . ? N17 C11 1.447(6) . ? N17 C19 1.449(6) . ? N18 C16 1.353(5) . ? N18 C25 1.455(5) . ? N18 C36 1.460(4) . ? N19 C12 1.335(5) . ? N19 C38 1.451(5) . ? N19 C37 1.464(5) . ? N20 C4 1.362(5) . ? N20 C19 1.450(5) . ? N20 C3 1.458(5) . ? C1 C47 1.519(7) . ? C1 C34 1.530(5) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C17 1.503(7) . ? C2 C6 1.530(6) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C5 C48 1.515(7) . ? C5 C33 1.530(6) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C15 1.517(5) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C45 1.495(7) . ? C7 C19 1.528(5) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C9 C37 1.507(5) . ? C9 C39 1.531(6) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C15 C44 1.564(5) . ? C17 C29 1.531(6) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C19 C33 1.567(6) . ? C20 C39 1.520(5) . ? C20 C31 1.528(5) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C41 1.516(5) . ? C22 C50 1.540(6) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C43 1.522(6) . ? C24 C14 1.525(5) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C31 1.522(5) . ? C25 C37 1.577(4) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C49 1.512(6) . ? C27 C41 1.592(5) . ? C29 C44 1.508(5) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C34 C43 1.571(5) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C45 C48 1.508(8) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 C49 1.516(7) . ? C46 C50 1.529(6) . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C47 C14 1.529(7) . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O9 Nd1 O4 143.99(10) . 4_646 ? O9 Nd1 Cl2 92.29(10) . . ? O4 Nd1 Cl2 98.11(10) 4_646 . ? O9 Nd1 Cl1 97.17(10) . . ? O4 Nd1 Cl1 91.45(10) 4_646 . ? Cl2 Nd1 Cl1 148.94(10) . . ? O9 Nd1 O10 73.80(9) . . ? O4 Nd1 O10 142.20(9) 4_646 . ? Cl2 Nd1 O10 75.58(9) . . ? Cl1 Nd1 O10 78.79(10) . . ? O9 Nd1 O5 141.80(9) . 4_646 ? O4 Nd1 O5 74.17(9) 4_646 4_646 ? Cl2 Nd1 O5 80.02(9) . 4_646 ? Cl1 Nd1 O5 74.28(9) . 4_646 ? O10 Nd1 O5 68.03(9) . 4_646 ? O9 Nd1 O2W 76.75(11) . . ? O4 Nd1 O2W 74.32(11) 4_646 . ? Cl2 Nd1 O2W 71.08(11) . . ? Cl1 Nd1 O2W 139.92(11) . . ? O10 Nd1 O2W 133.97(10) . . ? O5 Nd1 O2W 133.09(10) 4_646 . ? O9 Nd1 O1W 73.79(10) . . ? O4 Nd1 O1W 76.77(10) 4_646 . ? Cl2 Nd1 O1W 141.50(11) . . ? Cl1 Nd1 O1W 69.47(11) . . ? O10 Nd1 O1W 130.60(10) . . ? O5 Nd1 O1W 132.28(10) 4_646 . ? O2W Nd1 O1W 70.84(12) . . ? C12 O4 Nd1 156.6(2) . 4_656 ? C32 O5 Nd1 153.6(3) . 4_656 ? C18 O9 Nd1 156.7(3) . . ? C16 O10 Nd1 156.7(2) . . ? C10 N1 C33 112.6(3) . . ? C10 N1 C21 120.6(4) . . ? C33 N1 C21 126.8(4) . . ? C4 N2 C42 121.4(4) . . ? C4 N2 C33 112.6(3) . . ? C42 N2 C33 125.4(3) . . ? C30 N3 C43 112.9(3) . . ? C30 N3 C35 122.3(3) . . ? C43 N3 C35 124.2(3) . . ? C12 N4 C35 122.6(3) . . ? C12 N4 C25 111.9(3) . . ? C35 N4 C25 125.5(3) . . ? C13 N5 C27 113.8(3) . . ? C13 N5 C21 119.9(3) . . ? C27 N5 C21 126.1(3) . . ? C30 N6 C11 121.7(4) . . ? C30 N6 C34 112.8(3) . . ? C11 N6 C34 125.1(3) . . ? C8 N7 C41 114.2(3) . . ? C8 N7 C23 120.8(3) . . ? C41 N7 C23 124.6(3) . . ? C28 N8 C34 113.7(3) . . ? C28 N8 C3 120.1(3) . . ? C34 N8 C3 126.1(3) . . ? C16 N9 C40 122.0(3) . . ? C16 N9 C37 112.5(3) . . ? C40 N9 C37 125.4(3) . . ? C8 N10 C42 121.3(3) . . ? C8 N10 C27 113.9(3) . . ? C42 N10 C27 124.2(3) . . ? C18 N11 C15 112.6(3) . . ? C18 N11 C23 121.1(3) . . ? C15 N11 C23 126.1(3) . . ? C32 N12 C44 112.6(3) . . ? C32 N12 C38 122.1(3) . . ? C44 N12 C38 125.2(3) . . ? C13 N13 C41 114.1(3) . . ? C13 N13 C26 119.5(3) . . ? C41 N13 C26 125.3(3) . . ? C18 N14 C40 122.3(3) . . ? C18 N14 C44 112.3(3) . . ? C40 N14 C44 125.4(3) . . ? C28 N15 C36 120.5(3) . . ? C28 N15 C43 113.1(3) . . ? C36 N15 C43 125.4(3) . . ? C32 N16 C26 121.5(3) . . ? C32 N16 C15 112.7(3) . . ? C26 N16 C15 125.2(3) . . ? C10 N17 C11 120.4(4) . . ? C10 N17 C19 111.4(4) . . ? C11 N17 C19 127.3(3) . . ? C16 N18 C25 112.9(3) . . ? C16 N18 C36 121.2(3) . . ? C25 N18 C36 124.6(3) . . ? C12 N19 C38 122.6(3) . . ? C12 N19 C37 112.6(3) . . ? C38 N19 C37 124.8(3) . . ? C4 N20 C19 112.9(3) . . ? C4 N20 C3 120.7(3) . . ? C19 N20 C3 126.4(3) . . ? C47 C1 C34 111.6(4) . . ? C47 C1 H1A 109.3 . . ? C34 C1 H1A 109.3 . . ? C47 C1 H1B 109.3 . . ? C34 C1 H1B 109.3 . . ? H1A C1 H1B 108.0 . . ? C17 C2 C6 113.9(4) . . ? C17 C2 H2A 108.8 . . ? C6 C2 H2A 108.8 . . ? C17 C2 H2B 108.8 . . ? C6 C2 H2B 108.8 . . ? H2A C2 H2B 107.7 . . ? N20 C3 N8 113.5(3) . . ? N20 C3 H3A 108.9 . . ? N8 C3 H3A 108.9 . . ? N20 C3 H3B 108.9 . . ? N8 C3 H3B 108.9 . . ? H3A C3 H3B 107.7 . . ? O6 C4 N20 126.5(4) . . ? O6 C4 N2 125.3(4) . . ? N20 C4 N2 108.2(4) . . ? C48 C5 C33 112.2(4) . . ? C48 C5 H5A 109.2 . . ? C33 C5 H5A 109.2 . . ? C48 C5 H5B 109.2 . . ? C33 C5 H5B 109.2 . . ? H5A C5 H5B 107.9 . . ? C15 C6 C2 110.0(3) . . ? C15 C6 H6A 109.7 . . ? C2 C6 H6A 109.7 . . ? C15 C6 H6B 109.7 . . ? C2 C6 H6B 109.7 . . ? H6A C6 H6B 108.2 . . ? C45 C7 C19 111.1(4) . . ? C45 C7 H7A 109.4 . . ? C19 C7 H7A 109.4 . . ? C45 C7 H7B 109.4 . . ? C19 C7 H7B 109.4 . . ? H7A C7 H7B 108.0 . . ? O7 C8 N7 128.0(4) . . ? O7 C8 N10 124.5(3) . . ? N7 C8 N10 107.5(3) . . ? C37 C9 C39 110.8(3) . . ? C37 C9 H9A 109.5 . . ? C39 C9 H9A 109.5 . . ? C37 C9 H9B 109.5 . . ? C39 C9 H9B 109.5 . . ? H9A C9 H9B 108.1 . . ? O2 C10 N1 125.7(4) . . ? O2 C10 N17 125.1(4) . . ? N1 C10 N17 109.2(4) . . ? N17 C11 N6 112.7(3) . . ? N17 C11 H11A 109.1 . . ? N6 C11 H11A 109.1 . . ? N17 C11 H11B 109.1 . . ? N6 C11 H11B 109.1 . . ? H11A C11 H11B 107.8 . . ? O4 C12 N19 125.6(3) . . ? O4 C12 N4 123.9(3) . . ? N19 C12 N4 110.5(3) . . ? O3 C13 N13 126.9(3) . . ? O3 C13 N5 126.0(3) . . ? N13 C13 N5 107.1(3) . . ? N11 C15 N16 112.8(3) . . ? N11 C15 C6 112.9(3) . . ? N16 C15 C6 112.6(3) . . ? N11 C15 C44 103.2(3) . . ? N16 C15 C44 102.3(3) . . ? C6 C15 C44 112.0(3) . . ? O10 C16 N18 125.9(3) . . ? O10 C16 N9 125.2(3) . . ? N18 C16 N9 108.9(3) . . ? C2 C17 C29 112.5(4) . . ? C2 C17 H17A 109.1 . . ? C29 C17 H17A 109.1 . . ? C2 C17 H17B 109.1 . . ? C29 C17 H17B 109.1 . . ? H17A C17 H17B 107.8 . . ? O9 C18 N11 124.7(4) . . ? O9 C18 N14 126.1(4) . . ? N11 C18 N14 109.2(3) . . ? N17 C19 N20 113.4(3) . . ? N17 C19 C7 111.1(4) . . ? N20 C19 C7 112.8(3) . . ? N17 C19 C33 103.6(3) . . ? N20 C19 C33 103.1(3) . . ? C7 C19 C33 112.2(3) . . ? C39 C20 C31 113.6(3) . . ? C39 C20 H20A 108.9 . . ? C31 C20 H20A 108.9 . . ? C39 C20 H20B 108.9 . . ? C31 C20 H20B 108.9 . . ? H20A C20 H20B 107.7 . . ? N1 C21 N5 113.0(3) . . ? N1 C21 H21A 109.0 . . ? N5 C21 H21A 109.0 . . ? N1 C21 H21B 109.0 . . ? N5 C21 H21B 109.0 . . ? H21A C21 H21B 107.8 . . ? C41 C22 C50 111.3(3) . . ? C41 C22 H22A 109.4 . . ? C50 C22 H22A 109.4 . . ? C41 C22 H22B 109.4 . . ? C50 C22 H22B 109.4 . . ? H22A C22 H22B 108.0 . . ? N7 C23 N11 113.6(3) . . ? N7 C23 H23A 108.8 . . ? N11 C23 H23A 108.8 . . ? N7 C23 H23B 108.8 . . ? N11 C23 H23B 108.8 . . ? H23A C23 H23B 107.7 . . ? C43 C24 C14 111.1(3) . . ? C43 C24 H24A 109.4 . . ? C14 C24 H24A 109.4 . . ? C43 C24 H24B 109.4 . . ? C14 C24 H24B 109.4 . . ? H24A C24 H24B 108.0 . . ? N18 C25 N4 112.8(3) . . ? N18 C25 C31 113.2(3) . . ? N4 C25 C31 112.9(3) . . ? N18 C25 C37 102.4(3) . . ? N4 C25 C37 102.4(3) . . ? C31 C25 C37 112.0(3) . . ? N16 C26 N13 112.5(3) . . ? N16 C26 H26A 109.1 . . ? N13 C26 H26A 109.1 . . ? N16 C26 H26B 109.1 . . ? N13 C26 H26B 109.1 . . ? H26A C26 H26B 107.8 . . ? N5 C27 N10 113.7(3) . . ? N5 C27 C49 113.2(4) . . ? N10 C27 C49 112.7(4) . . ? N5 C27 C41 102.9(3) . . ? N10 C27 C41 101.5(3) . . ? C49 C27 C41 111.8(3) . . ? O8 C28 N8 126.7(4) . . ? O8 C28 N15 125.5(3) . . ? N8 C28 N15 107.8(3) . . ? C44 C29 C17 110.4(3) . . ? C44 C29 H29A 109.6 . . ? C17 C29 H29A 109.6 . . ? C44 C29 H29B 109.6 . . ? C17 C29 H29B 109.6 . . ? H29A C29 H29B 108.1 . . ? O1 C30 N6 124.8(4) . . ? O1 C30 N3 126.3(4) . . ? N6 C30 N3 108.8(4) . . ? C25 C31 C20 110.5(3) . . ? C25 C31 H31A 109.6 . . ? C20 C31 H31A 109.6 . . ? C25 C31 H31B 109.6 . . ? C20 C31 H31B 109.6 . . ? H31A C31 H31B 108.1 . . ? O5 C32 N12 126.1(4) . . ? O5 C32 N16 124.8(3) . . ? N12 C32 N16 109.0(3) . . ? N1 C33 N2 113.8(3) . . ? N1 C33 C5 111.8(3) . . ? N2 C33 C5 113.1(4) . . ? N1 C33 C19 102.7(3) . . ? N2 C33 C19 102.6(3) . . ? C5 C33 C19 112.0(3) . . ? N8 C34 N6 113.6(3) . . ? N8 C34 C1 112.3(3) . . ? N6 C34 C1 113.3(3) . . ? N8 C34 C43 102.8(3) . . ? N6 C34 C43 102.6(3) . . ? C1 C34 C43 111.4(3) . . ? N3 C35 N4 113.8(3) . . ? N3 C35 H35A 108.8 . . ? N4 C35 H35A 108.8 . . ? N3 C35 H35B 108.8 . . ? N4 C35 H35B 108.8 . . ? H35A C35 H35B 107.7 . . ? N15 C36 N18 113.5(3) . . ? N15 C36 H36A 108.9 . . ? N18 C36 H36A 108.9 . . ? N15 C36 H36B 108.9 . . ? N18 C36 H36B 108.9 . . ? H36A C36 H36B 107.7 . . ? N9 C37 N19 112.4(3) . . ? N9 C37 C9 113.0(3) . . ? N19 C37 C9 112.9(3) . . ? N9 C37 C25 103.0(3) . . ? N19 C37 C25 102.4(3) . . ? C9 C37 C25 112.2(3) . . ? N19 C38 N12 113.0(3) . . ? N19 C38 H38A 109.0 . . ? N12 C38 H38A 109.0 . . ? N19 C38 H38B 109.0 . . ? N12 C38 H38B 109.0 . . ? H38A C38 H38B 107.8 . . ? C20 C39 C9 112.5(3) . . ? C20 C39 H39A 109.1 . . ? C9 C39 H39A 109.1 . . ? C20 C39 H39B 109.1 . . ? C9 C39 H39B 109.1 . . ? H39A C39 H39B 107.8 . . ? N14 C40 N9 113.9(3) . . ? N14 C40 H40A 108.8 . . ? N9 C40 H40A 108.8 . . ? N14 C40 H40B 108.8 . . ? N9 C40 H40B 108.8 . . ? H40A C40 H40B 107.7 . . ? N7 C41 N13 113.6(3) . . ? N7 C41 C22 113.1(3) . . ? N13 C41 C22 113.2(3) . . ? N7 C41 C27 102.8(3) . . ? N13 C41 C27 101.5(3) . . ? C22 C41 C27 111.5(3) . . ? N3 C43 N15 113.2(3) . . ? N3 C43 C24 112.7(3) . . ? N15 C43 C24 112.9(3) . . ? N3 C43 C34 102.6(3) . . ? N15 C43 C34 102.2(3) . . ? C24 C43 C34 112.3(3) . . ? N14 C44 N12 112.1(3) . . ? N14 C44 C29 112.8(3) . . ? N12 C44 C29 112.6(3) . . ? N14 C44 C15 102.7(3) . . ? N12 C44 C15 103.4(3) . . ? C29 C44 C15 112.5(3) . . ? C7 C45 C48 113.5(5) . . ? C7 C45 H45A 108.9 . . ? C48 C45 H45A 108.9 . . ? C7 C45 H45B 108.9 . . ? C48 C45 H45B 108.9 . . ? H45A C45 H45B 107.7 . . ? C49 C46 C50 113.2(4) . . ? C49 C46 H46A 108.9 . . ? C50 C46 H46A 108.9 . . ? C49 C46 H46B 108.9 . . ? C50 C46 H46B 108.9 . . ? H46A C46 H46B 107.8 . . ? C1 C47 C14 113.0(4) . . ? C1 C47 H47A 109.0 . . ? C14 C47 H47A 109.0 . . ? C1 C47 H47B 109.0 . . ? C14 C47 H47B 109.0 . . ? H47A C47 H47B 107.8 . . ? C45 C48 C5 113.6(4) . . ? C45 C48 H48A 108.8 . . ? C5 C48 H48A 108.8 . . ? C45 C48 H48B 108.8 . . ? C5 C48 H48B 108.8 . . ? H48A C48 H48B 107.7 . . ? C27 C49 C46 110.6(4) . . ? C27 C49 H49A 109.5 . . ? C46 C49 H49A 109.5 . . ? C27 C49 H49B 109.5 . . ? C46 C49 H49B 109.5 . . ? H49A C49 H49B 108.1 . . ? C46 C50 C22 112.4(4) . . ? C46 C50 H50A 109.1 . . ? C22 C50 H50A 109.1 . . ? C46 C50 H50B 109.1 . . ? C22 C50 H50B 109.1 . . ? H50A C50 H50B 107.9 . . ? C24 C14 C47 112.5(4) . . ? C24 C14 H14A 109.1 . . ? C47 C14 H14A 109.1 . . ? C24 C14 H14B 109.1 . . ? C47 C14 H14B 109.1 . . ? H14A C14 H14B 107.8 . . ? N2 C42 N10 114.0(3) . . ? N2 C42 H42A 108.8 . . ? N10 C42 H42A 108.8 . . ? N2 C42 H42B 108.8 . . ? N10 C42 H42B 108.8 . . ? H42A C42 H42B 107.7 . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.20 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.116 _refine_diff_density_min -0.894 _refine_diff_density_rms 0.191 # Attachment 'Pr.cif' data_Pr _database_code_depnum_ccdc_archive 'CCDC 883410' #TrackingRef 'Pr.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H103 Cl2 N21 O34.50 Pr' _chemical_formula_weight 1762.34 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' Cl Cl 0.1484 0.1585 '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 Orthorhombic _symmetry_space_group_name_H-M Fdd2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 35.890(8) _cell_length_b 55.191(12) _cell_length_c 16.106(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 31903(12) _cell_formula_units_Z 16 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.468 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 14712 _exptl_absorpt_coefficient_mu 0.774 _exptl_absorpt_correction_type 'multi scan' _exptl_absorpt_correction_T_min 0.7788 _exptl_absorpt_correction_T_max 0.8544 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 50431 _diffrn_reflns_av_R_equivalents 0.0974 _diffrn_reflns_av_sigmaI/netI 0.0776 _diffrn_reflns_limit_h_min -42 _diffrn_reflns_limit_h_max 42 _diffrn_reflns_limit_k_min -66 _diffrn_reflns_limit_k_max 62 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.35 _diffrn_reflns_theta_max 25.20 _reflns_number_total 14124 _reflns_number_gt 12448 _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. loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.010 0.000 0.118 12788 4845 ' ' 2 -0.026 0.153 0.644 46 18 ' ' 3 0.026 0.347 0.144 47 18 ' ' 4 -0.026 0.653 0.144 46 18 ' ' 5 0.026 0.847 0.644 47 18 ' ' 6 0.224 0.097 0.894 46 13 ' ' 7 0.224 0.597 0.394 46 13 ' ' 8 0.276 0.403 0.894 47 10 ' ' 9 0.276 0.903 0.394 47 10 ' ' 10 0.474 0.153 0.144 46 18 ' ' 11 0.474 0.653 0.644 46 18 ' ' 12 0.526 0.347 0.644 47 18 ' ' 13 0.526 0.847 0.144 47 18 ' ' 14 0.724 0.097 0.394 46 13 ' ' 15 0.724 0.597 0.894 46 13 ' ' 16 0.776 0.403 0.394 47 10 ' ' 17 0.776 0.903 0.894 47 10 ' ' _platon_squeeze_details ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1091P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.000(15) _refine_ls_number_reflns 14124 _refine_ls_number_parameters 776 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0647 _refine_ls_R_factor_gt 0.0593 _refine_ls_wR_factor_ref 0.1570 _refine_ls_wR_factor_gt 0.1528 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 0.015 _refine_ls_shift/su_mean 0.001 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 0.616316(4) 0.158069(3) 0.258372(11) 0.03032(4) Uani 1 1 d . . . Cl1 Cl 0.62341(7) 0.12537(5) 0.36197(16) 0.1309(8) Uani 1 1 d . . . Cl2 Cl 0.56956(7) 0.18084(5) 0.18178(15) 0.1321(8) Uani 1 1 d . . . O1W O 0.63995(11) 0.20180(6) 0.2430(3) 0.1010(13) Uani 1 1 d . . . O2W O 0.60331(7) 0.18163(5) 0.38762(19) 0.0574(8) Uani 1 1 d . . . O3W O 0.63968(8) 0.16796(6) 0.1140(2) 0.0678(9) Uani 1 1 d . . . O1 O 0.41466(6) 0.11989(4) -0.04298(15) 0.0406(6) Uani 1 1 d . . . O2 O 0.36377(6) 0.16448(5) 0.22942(15) 0.0399(6) Uani 1 1 d . . . O3 O 0.39431(6) 0.11330(5) 0.27121(16) 0.0469(7) Uani 1 1 d . . . O4 O 0.42635(6) 0.08631(5) 0.09181(15) 0.0419(7) Uani 1 1 d . . . O5 O 0.37849(7) 0.16804(5) 0.03915(16) 0.0425(7) Uani 1 1 d . . . O6 O 0.52920(6) 0.21651(5) 0.07190(16) 0.0474(7) Uani 1 1 d . . . O7 O 0.55157(6) 0.15084(4) 0.31827(15) 0.0352(6) Uani 1 1 d . . . O8 O 0.58110(6) 0.12670(4) 0.17261(15) 0.0365(6) Uani 1 1 d . . . O9 O 0.56157(7) 0.16751(5) 0.01713(16) 0.0476(7) Uani 1 1 d . . . O10 O 0.52008(6) 0.20546(4) 0.26699(17) 0.0424(6) Uani 1 1 d . . . N1 N 0.42508(8) 0.18589(5) -0.03725(18) 0.0370(7) Uani 1 1 d . . . N2 N 0.47716(8) 0.11324(5) -0.07396(18) 0.0372(7) Uani 1 1 d U . . N3 N 0.46948(8) 0.19027(6) 0.34212(18) 0.0397(8) Uani 1 1 d . . . N4 N 0.40692(9) 0.17474(6) 0.33073(19) 0.0452(8) Uani 1 1 d U . . N5 N 0.48544(8) 0.20587(5) -0.02599(18) 0.0387(7) Uani 1 1 d . . . N6 N 0.40426(8) 0.20487(5) 0.0739(2) 0.0410(8) Uani 1 1 d . . . N7 N 0.45343(8) 0.14938(5) -0.09622(17) 0.0358(7) Uani 1 1 d . . . N8 N 0.49290(8) 0.15076(6) 0.37610(17) 0.0382(8) Uani 1 1 d . . . N9 N 0.51443(8) 0.16855(5) -0.08067(17) 0.0371(7) Uani 1 1 d . . . N10 N 0.45422(8) 0.10240(6) 0.30532(18) 0.0395(7) Uani 1 1 d U . . N11 N 0.39722(9) 0.19957(6) 0.2226(2) 0.0444(8) Uani 1 1 d . . . N12 N 0.53514(7) 0.13295(5) -0.03518(17) 0.0335(7) Uani 1 1 d . . . N13 N 0.47708(8) 0.08306(5) 0.17871(18) 0.0358(7) Uani 1 1 d . . . N14 N 0.46580(8) 0.22291(5) 0.0907(2) 0.0425(8) Uani 1 1 d . . . N15 N 0.54704(8) 0.10464(5) 0.07653(19) 0.0388(7) Uani 1 1 d U . . N16 N 0.48683(7) 0.08526(5) 0.04317(18) 0.0338(7) Uani 1 1 d . . . N17 N 0.51763(8) 0.11531(5) 0.33529(16) 0.0336(7) Uani 1 1 d . . . N18 N 0.45913(8) 0.21746(5) 0.24126(19) 0.0402(8) Uani 1 1 d . . . N19 N 0.54167(7) 0.09560(5) 0.21033(18) 0.0336(7) Uani 1 1 d . . . N20 N 0.42927(8) 0.13462(6) 0.36613(18) 0.0405(8) Uani 1 1 d . . . C1 C 0.48251(10) 0.10851(6) 0.3712(2) 0.0369(9) Uani 1 1 d . . . C2 C 0.56723(12) 0.04585(8) 0.1765(3) 0.0603(12) Uani 1 1 d . . . H2A H 0.5836 0.0539 0.2156 0.072 Uiso 1 1 calc R . . H2B H 0.5708 0.0285 0.1828 0.072 Uiso 1 1 calc R . . C3 C 0.46394(12) 0.13138(9) 0.5012(2) 0.0591(12) Uani 1 1 d . . . H3A H 0.4889 0.1299 0.5236 0.071 Uiso 1 1 calc R . . H3B H 0.4531 0.1462 0.5226 0.071 Uiso 1 1 calc R . . C4 C 0.49349(14) 0.15573(9) -0.2218(2) 0.0579(11) Uani 1 1 d U . . H4A H 0.4841 0.1717 -0.2355 0.070 Uiso 1 1 calc R . . H4B H 0.4776 0.1439 -0.2486 0.070 Uiso 1 1 calc R . . C5 C 0.49122(10) 0.15217(7) -0.1273(2) 0.0351(9) Uani 1 1 d . . . C6 C 0.57765(13) 0.05307(9) 0.0906(3) 0.0669(14) Uani 1 1 d . . . H6A H 0.5904 0.0396 0.0644 0.080 Uiso 1 1 calc R . . H6B H 0.5951 0.0665 0.0937 0.080 Uiso 1 1 calc R . . C7 C 0.42934(13) 0.24888(8) 0.3756(3) 0.0681(13) Uani 1 1 d . . . H7A H 0.4523 0.2548 0.3513 0.082 Uiso 1 1 calc R . . H7B H 0.4162 0.2627 0.3987 0.082 Uiso 1 1 calc R . . C8 C 0.51707(10) 0.07836(6) 0.1720(2) 0.0394(9) Uani 1 1 d . . . C9 C 0.40533(11) 0.23753(7) 0.3069(3) 0.0541(12) Uani 1 1 d . . . H9A H 0.3804 0.2345 0.3279 0.065 Uiso 1 1 calc R . . H9B H 0.4034 0.2487 0.2605 0.065 Uiso 1 1 calc R . . C10 C 0.42089(12) 0.20653(8) 0.4376(3) 0.0590(12) Uani 1 1 d . . . H10A H 0.3941 0.2078 0.4438 0.071 Uiso 1 1 calc R . . H10B H 0.4303 0.1960 0.4809 0.071 Uiso 1 1 calc R . . C11 C 0.54575(10) 0.06043(6) 0.0368(3) 0.0465(10) Uani 1 1 d . . . H11A H 0.5289 0.0468 0.0299 0.056 Uiso 1 1 calc R . . H11B H 0.5550 0.0650 -0.0175 0.056 Uiso 1 1 calc R . . C12 C 0.45239(15) 0.24904(9) -0.1144(3) 0.0748(15) Uani 1 1 d . . . H12A H 0.4793 0.2482 -0.1196 0.090 Uiso 1 1 calc R . . H12B H 0.4429 0.2588 -0.1597 0.090 Uiso 1 1 calc R . . C14 C 0.49257(9) 0.17593(7) 0.3975(2) 0.0388(9) Uani 1 1 d . . . H14A H 0.5179 0.1821 0.3959 0.047 Uiso 1 1 calc R . . H14B H 0.4834 0.1777 0.4539 0.047 Uiso 1 1 calc R . . C15 C 0.43564(13) 0.22303(7) -0.1200(3) 0.0536(11) Uani 1 1 d . . . H15A H 0.4088 0.2240 -0.1255 0.064 Uiso 1 1 calc R . . H15B H 0.4454 0.2149 -0.1687 0.064 Uiso 1 1 calc R . . C16 C 0.43865(13) 0.23149(8) 0.4451(3) 0.0619(12) Uani 1 1 d . . . H16A H 0.4308 0.2387 0.4972 0.074 Uiso 1 1 calc R . . H16B H 0.4655 0.2295 0.4473 0.074 Uiso 1 1 calc R . . C17 C 0.40210(10) 0.15294(8) 0.3830(2) 0.0443(10) Uani 1 1 d . . . H17A H 0.4038 0.1576 0.4410 0.053 Uiso 1 1 calc R . . H17B H 0.3774 0.1463 0.3737 0.053 Uiso 1 1 calc R . . C18 C 0.42460(10) 0.16706(6) -0.10472(19) 0.0354(9) Uani 1 1 d . . . H18A H 0.4007 0.1589 -0.1042 0.042 Uiso 1 1 calc R . . H18B H 0.4272 0.1750 -0.1580 0.042 Uiso 1 1 calc R . . C19 C 0.44234(13) 0.26078(9) -0.0325(4) 0.0686(14) Uani 1 1 d . . . H19A H 0.4311 0.2764 -0.0437 0.082 Uiso 1 1 calc R . . H19B H 0.4651 0.2636 -0.0015 0.082 Uiso 1 1 calc R . . C20 C 0.40095(9) 0.18428(6) 0.02573(18) 0.0348(8) Uani 1 1 d . . . C21 C 0.46605(9) 0.13285(7) 0.4060(2) 0.0379(9) Uani 1 1 d . . . C22 C 0.41615(11) 0.24639(7) 0.0209(3) 0.0523(11) Uani 1 1 d . . . H22A H 0.3926 0.2444 -0.0079 0.063 Uiso 1 1 calc R . . H22B H 0.4114 0.2552 0.0720 0.063 Uiso 1 1 calc R . . C23 C 0.42350(10) 0.11640(7) 0.3098(2) 0.0425(10) Uani 1 1 d . . . C24 C 0.52368(8) 0.13985(6) 0.34024(19) 0.0298(8) Uani 1 1 d . . . C25 C 0.48618(13) 0.08820(8) 0.4342(2) 0.0529(11) Uani 1 1 d . . . H25A H 0.5065 0.0918 0.4719 0.064 Uiso 1 1 calc R . . H25B H 0.4920 0.0732 0.4057 0.064 Uiso 1 1 calc R . . C26 C 0.43206(10) 0.22150(7) 0.0415(2) 0.0427(10) Uani 1 1 d . . . C27 C 0.52420(9) 0.08214(6) 0.0761(2) 0.0322(8) Uani 1 1 d . . . C28 C 0.51228(11) 0.19471(7) -0.0826(2) 0.0428(10) Uani 1 1 d . . . H28A H 0.5061 0.1997 -0.1387 0.051 Uiso 1 1 calc R . . H28B H 0.5368 0.2011 -0.0700 0.051 Uiso 1 1 calc R . . C29 C 0.52810(11) 0.11400(9) -0.1773(3) 0.0558(12) Uani 1 1 d . . . H29A H 0.5422 0.1000 -0.1588 0.067 Uiso 1 1 calc R . . H29B H 0.5093 0.1085 -0.2161 0.067 Uiso 1 1 calc R . . C30 C 0.52687(11) 0.05222(6) 0.1972(3) 0.0494(11) Uani 1 1 d . . . H30A H 0.5229 0.0503 0.2564 0.059 Uiso 1 1 calc R . . H30B H 0.5104 0.0411 0.1685 0.059 Uiso 1 1 calc R . . C31 C 0.38119(10) 0.20841(7) 0.1458(3) 0.0435(10) Uani 1 1 d . . . H31A H 0.3576 0.2003 0.1367 0.052 Uiso 1 1 calc R . . H31B H 0.3761 0.2256 0.1517 0.052 Uiso 1 1 calc R . . C32 C 0.47828(10) 0.08768(6) -0.0453(2) 0.0354(9) Uani 1 1 d . . . H32A H 0.4543 0.0802 -0.0563 0.042 Uiso 1 1 calc R . . H32B H 0.4969 0.0790 -0.0771 0.042 Uiso 1 1 calc R . . C33 C 0.46853(11) 0.23297(7) 0.1726(2) 0.0443(10) Uani 1 1 d . . . H33A H 0.4525 0.2471 0.1750 0.053 Uiso 1 1 calc R . . H33B H 0.4939 0.2386 0.1805 0.053 Uiso 1 1 calc R . . C34 C 0.44574(9) 0.20841(6) -0.0412(2) 0.0365(9) Uani 1 1 d . . . C35 C 0.45481(9) 0.08057(6) 0.2524(2) 0.0391(7) Uani 1 1 d U . . H35A H 0.4643 0.0671 0.2847 0.047 Uiso 1 1 calc R . . H35B H 0.4295 0.0767 0.2363 0.047 Uiso 1 1 calc R . . C38 C 0.48604(10) 0.20435(6) 0.2814(2) 0.0395(9) Uani 1 1 d . . . C39 C 0.43049(10) 0.19591(7) 0.3511(2) 0.0439(10) Uani 1 1 d . . . C40 C 0.42266(9) 0.21375(6) 0.2776(2) 0.0377(9) Uani 1 1 d . . . C41 C 0.44587(9) 0.12647(7) -0.0688(2) 0.0355(8) Uani 1 1 d U . . C42 C 0.50911(9) 0.12600(6) -0.10219(19) 0.0334(8) Uani 1 1 d . . . C43 C 0.54543(9) 0.09942(6) 0.3006(2) 0.0326(8) Uani 1 1 d . . . H43A H 0.5439 0.0838 0.3283 0.039 Uiso 1 1 calc R . . H43B H 0.5699 0.1061 0.3118 0.039 Uiso 1 1 calc R . . C44 C 0.49715(10) 0.21535(6) 0.0486(2) 0.0372(9) Uani 1 1 d . . . C46 C 0.55849(9) 0.11089(6) 0.1558(2) 0.0298(8) Uani 1 1 d . . . C47 C 0.53915(9) 0.15690(6) -0.0276(2) 0.0335(9) Uani 1 1 d . . . C48 C 0.56148(8) 0.11653(7) 0.0051(2) 0.0402(8) Uani 1 1 d U . . H48A H 0.5692 0.1044 -0.0348 0.048 Uiso 1 1 calc R . . H48B H 0.5834 0.1257 0.0210 0.048 Uiso 1 1 calc R . . C49 C 0.38671(9) 0.17842(6) 0.2575(3) 0.0383(7) Uani 1 1 d U . . C50 C 0.46054(8) 0.08497(6) 0.10340(19) 0.0282(7) Uani 1 1 d . . . C51 C 0.55365(14) 0.13147(10) -0.2200(3) 0.0730(12) Uani 1 1 d U . . H51A H 0.5667 0.1231 -0.2642 0.088 Uiso 1 1 calc R . . H51B H 0.5721 0.1372 -0.1806 0.088 Uiso 1 1 calc R . . C52 C 0.44032(17) 0.10958(12) 0.5300(3) 0.0906(14) Uani 1 1 d U . . H52A H 0.4142 0.1133 0.5213 0.109 Uiso 1 1 calc R . . H52B H 0.4440 0.1073 0.5892 0.109 Uiso 1 1 calc R . . C53 C 0.44974(14) 0.08511(11) 0.4841(3) 0.0784(13) Uani 1 1 d U . . H53A H 0.4526 0.0722 0.5244 0.094 Uiso 1 1 calc R . . H53B H 0.4295 0.0808 0.4469 0.094 Uiso 1 1 calc R . . C54 C 0.53328(16) 0.15319(11) -0.2564(3) 0.0791(12) Uani 1 1 d U . . H54A H 0.5321 0.1515 -0.3163 0.095 Uiso 1 1 calc R . . H54B H 0.5472 0.1678 -0.2440 0.095 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pr1 0.02209(6) 0.03060(7) 0.03828(7) 0.00333(7) -0.00749(7) -0.00001(7) Cl1 0.1300(14) 0.1401(18) 0.1226(14) 0.0159(13) -0.0215(13) -0.0055(14) Cl2 0.1219(15) 0.1413(17) 0.1331(16) -0.0040(13) -0.0120(13) 0.0163(13) O1W 0.104(2) 0.0662(19) 0.133(3) 0.0442(19) -0.063(2) -0.0346(17) O2W 0.0338(13) 0.0637(17) 0.0748(17) -0.0256(14) -0.0096(13) 0.0067(13) O3W 0.0457(15) 0.089(2) 0.0690(17) 0.0398(15) 0.0173(13) 0.0204(15) O1 0.0287(11) 0.0424(13) 0.0508(13) 0.0008(11) -0.0023(10) -0.0107(10) O2 0.0331(12) 0.0493(14) 0.0371(12) -0.0002(10) -0.0056(9) 0.0003(11) O3 0.0293(11) 0.0618(15) 0.0496(14) -0.0096(13) -0.0028(11) -0.0100(11) O4 0.0315(12) 0.0513(14) 0.0429(12) -0.0011(11) -0.0140(10) -0.0044(11) O5 0.0396(12) 0.0345(13) 0.0535(14) 0.0036(11) -0.0078(11) -0.0116(11) O6 0.0280(11) 0.0565(15) 0.0576(15) 0.0035(12) -0.0128(11) -0.0085(11) O7 0.0295(11) 0.0335(11) 0.0428(12) 0.0029(10) -0.0037(10) 0.0010(10) O8 0.0258(10) 0.0327(12) 0.0510(13) 0.0009(10) -0.0033(10) -0.0060(10) O9 0.0426(12) 0.0514(13) 0.0487(13) 0.0024(12) -0.0195(11) -0.0086(12) O10 0.0317(11) 0.0350(11) 0.0604(14) -0.0086(12) 0.0016(11) -0.0041(10) N1 0.0340(14) 0.0313(14) 0.0457(15) 0.0007(12) -0.0054(12) -0.0039(12) N2 0.0326(11) 0.0389(15) 0.0400(14) 0.0004(12) -0.0031(12) -0.0038(9) N3 0.0262(13) 0.0540(17) 0.0390(14) -0.0085(13) 0.0000(12) -0.0006(13) N4 0.0423(15) 0.0431(16) 0.0503(12) -0.0039(13) -0.0055(11) -0.0026(14) N5 0.0324(14) 0.0438(16) 0.0400(13) 0.0094(13) -0.0086(12) -0.0032(13) N6 0.0370(15) 0.0304(14) 0.0557(16) -0.0011(13) -0.0071(14) -0.0010(13) N7 0.0330(14) 0.0385(15) 0.0360(13) 0.0053(12) -0.0092(12) -0.0103(12) N8 0.0298(14) 0.0521(16) 0.0327(13) -0.0026(13) 0.0004(11) -0.0065(13) N9 0.0367(14) 0.0368(15) 0.0379(14) 0.0061(12) -0.0062(12) -0.0049(13) N10 0.0313(14) 0.0455(12) 0.0419(14) 0.0088(10) -0.0083(12) -0.0052(13) N11 0.0347(14) 0.0428(17) 0.0556(16) -0.0007(14) -0.0098(14) -0.0003(14) N12 0.0270(13) 0.0389(15) 0.0347(13) -0.0065(12) -0.0062(11) 0.0029(12) N13 0.0293(13) 0.0354(14) 0.0428(14) 0.0039(12) -0.0053(12) -0.0024(12) N14 0.0276(13) 0.0373(15) 0.0626(18) 0.0007(14) -0.0123(13) 0.0017(12) N15 0.0275(13) 0.0416(15) 0.0472(12) -0.0063(11) -0.0021(11) -0.0078(12) N16 0.0248(12) 0.0356(14) 0.0411(13) -0.0015(12) -0.0066(11) 0.0000(12) N17 0.0336(14) 0.0363(14) 0.0309(13) 0.0098(11) -0.0049(11) -0.0037(12) N18 0.0322(14) 0.0318(14) 0.0566(18) -0.0053(13) -0.0047(13) -0.0006(12) N19 0.0242(13) 0.0345(14) 0.0420(14) 0.0055(12) -0.0099(12) -0.0008(11) N20 0.0365(15) 0.0474(16) 0.0376(14) 0.0023(13) -0.0047(12) -0.0072(14) C1 0.0371(17) 0.0369(18) 0.0366(16) 0.0089(14) -0.0044(14) -0.0071(15) C2 0.056(2) 0.045(2) 0.080(3) -0.005(2) -0.025(2) 0.0182(19) C3 0.053(2) 0.097(3) 0.0270(16) 0.004(2) 0.0039(18) -0.006(2) C4 0.0719(13) 0.075(3) 0.0266(19) 0.0056(17) 0.0013(13) -0.011(2) C5 0.0341(17) 0.0437(18) 0.0277(15) 0.0026(14) -0.0025(13) -0.0023(15) C6 0.053(2) 0.053(2) 0.095(3) -0.013(2) -0.008(2) 0.017(2) C7 0.053(2) 0.060(2) 0.091(3) -0.040(2) 0.005(2) 0.001(2) C8 0.0397(17) 0.0297(17) 0.0489(18) 0.0028(14) -0.0142(15) -0.0029(15) C9 0.0360(19) 0.041(2) 0.086(3) -0.0165(19) 0.0000(19) 0.0047(17) C10 0.040(2) 0.072(3) 0.065(2) -0.028(2) 0.0039(19) 0.011(2) C11 0.0360(18) 0.0279(17) 0.076(2) -0.0156(16) 0.0002(17) 0.0005(15) C12 0.070(3) 0.061(3) 0.094(3) 0.041(2) -0.014(3) -0.010(2) C14 0.0273(16) 0.050(2) 0.0389(17) -0.0036(15) -0.0049(14) 0.0015(16) C15 0.060(2) 0.045(2) 0.056(2) 0.0263(17) -0.0119(18) -0.0112(19) C16 0.050(2) 0.071(3) 0.064(2) -0.037(2) -0.0008(19) 0.012(2) C17 0.0257(16) 0.080(3) 0.0272(15) 0.0026(16) 0.0046(14) -0.0080(18) C18 0.0429(18) 0.0384(17) 0.0247(14) 0.0039(13) -0.0078(13) -0.0082(16) C19 0.050(2) 0.052(2) 0.105(3) 0.022(2) -0.015(2) -0.012(2) C20 0.0326(16) 0.0367(16) 0.0351(17) 0.0144(13) -0.0056(13) 0.0006(14) C21 0.0280(16) 0.053(2) 0.0325(15) 0.0052(15) -0.0009(13) 0.0015(16) C22 0.0374(18) 0.0424(19) 0.077(3) 0.008(2) -0.0042(19) 0.0029(16) C23 0.0309(17) 0.055(2) 0.0414(18) 0.0076(16) -0.0008(15) -0.0005(16) C24 0.0240(14) 0.0385(17) 0.0270(14) -0.0024(13) -0.0064(12) -0.0040(14) C25 0.061(2) 0.059(2) 0.0379(18) 0.0267(16) -0.0049(18) -0.0140(19) C26 0.0322(17) 0.0438(19) 0.0523(19) 0.0084(16) -0.0107(15) -0.0062(16) C27 0.0250(15) 0.0239(15) 0.0475(17) -0.0041(14) -0.0055(13) -0.0004(13) C28 0.0417(19) 0.045(2) 0.0414(17) 0.0119(15) -0.0025(15) -0.0030(16) C29 0.0378(19) 0.083(3) 0.047(2) -0.018(2) 0.0013(17) -0.005(2) C30 0.052(2) 0.0169(15) 0.080(3) 0.0037(16) -0.0197(19) -0.0013(15) C31 0.0288(17) 0.043(2) 0.059(2) 0.0005(18) -0.0095(16) 0.0013(15) C32 0.0337(17) 0.0309(16) 0.0415(17) -0.0073(14) -0.0048(14) -0.0040(14) C33 0.0428(19) 0.0307(17) 0.060(2) -0.0124(16) -0.0017(17) -0.0006(16) C34 0.0269(15) 0.0328(17) 0.0497(18) 0.0087(15) -0.0076(14) -0.0036(14) C35 0.0372(16) 0.0447(14) 0.0354(14) 0.0122(11) -0.0060(15) -0.0151(14) C38 0.0354(17) 0.0334(16) 0.050(2) -0.0152(14) -0.0064(14) 0.0037(15) C39 0.0302(17) 0.055(2) 0.0466(18) -0.0147(17) 0.0073(15) 0.0025(16) C40 0.0274(15) 0.0356(16) 0.050(2) -0.0155(14) -0.0016(14) 0.0060(14) C41 0.0323(13) 0.0424(18) 0.0319(15) 0.0009(14) -0.0068(13) -0.0051(11) C42 0.0312(15) 0.0389(17) 0.0302(15) -0.0041(14) -0.0097(13) -0.0085(14) C43 0.0354(16) 0.0242(15) 0.0383(16) 0.0089(13) -0.0126(14) -0.0038(14) C44 0.0342(17) 0.0251(16) 0.0521(18) 0.0095(14) -0.0065(15) -0.0046(14) C46 0.0225(14) 0.0245(15) 0.0423(16) 0.0007(13) -0.0080(13) 0.0054(13) C47 0.0249(15) 0.0464(19) 0.0292(15) 0.0040(14) 0.0035(13) -0.0061(14) C48 0.0224(13) 0.0575(19) 0.0407(13) -0.0002(14) -0.0022(13) 0.0048(14) C49 0.0298(14) 0.0402(16) 0.0447(12) -0.0085(18) 0.0054(11) 0.0068(14) C50 0.0246(14) 0.0241(14) 0.0360(15) -0.0011(13) -0.0087(13) -0.0036(13) C51 0.067(2) 0.0938(19) 0.058(2) 0.0066(18) 0.0213(19) -0.0075(17) C52 0.085(3) 0.1272(17) 0.060(3) 0.0361(15) 0.018(2) 0.000(3) C53 0.058(3) 0.103(2) 0.074(3) 0.0352(17) -0.010(2) -0.030(2) C54 0.0865(16) 0.090(2) 0.060(3) 0.013(2) 0.0237(17) -0.0088(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pr1 Cl2 2.433(2) . ? Pr1 O1 2.465(2) 3 ? Pr1 Cl1 2.471(3) . ? Pr1 O2W 2.499(3) . ? Pr1 O3W 2.531(3) . ? Pr1 O7 2.547(2) . ? Pr1 O8 2.550(2) . ? Pr1 O4 2.558(2) 3 ? Pr1 O1W 2.570(4) . ? O1 C41 1.249(4) . ? O1 Pr1 2.465(2) 11_454 ? O2 C49 1.214(4) . ? O3 C23 1.230(4) . ? O4 C50 1.244(4) . ? O4 Pr1 2.558(2) 11_454 ? O5 C20 1.225(4) . ? O6 C44 1.212(4) . ? O7 C24 1.223(4) . ? O8 C46 1.222(4) . ? O9 C47 1.228(4) . ? O10 C38 1.245(4) . ? N1 C20 1.337(4) . ? N1 C34 1.449(4) . ? N1 C18 1.504(4) . ? N2 C41 1.342(5) . ? N2 C42 1.420(4) . ? N2 C32 1.485(4) . ? N3 C38 1.383(5) . ? N3 C39 1.441(4) . ? N3 C14 1.453(5) . ? N4 C49 1.399(5) . ? N4 C17 1.479(5) . ? N4 C39 1.479(5) . ? N5 C44 1.376(5) . ? N5 C34 1.453(4) . ? N5 C28 1.462(5) . ? N6 C20 1.381(4) . ? N6 C31 1.437(5) . ? N6 C26 1.453(5) . ? N7 C41 1.367(5) . ? N7 C18 1.429(5) . ? N7 C5 1.454(4) . ? N8 C24 1.384(4) . ? N8 C14 1.431(5) . ? N8 C21 1.462(5) . ? N9 C47 1.390(4) . ? N9 C28 1.446(5) . ? N9 C5 1.441(4) . ? N10 C23 1.348(5) . ? N10 C35 1.476(5) . ? N10 C1 1.507(4) . ? N11 C49 1.349(5) . ? N11 C31 1.450(5) . ? N11 C40 1.493(5) . ? N12 C47 1.335(4) . ? N12 C48 1.461(4) . ? N12 C42 1.478(4) . ? N13 C50 1.354(4) . ? N13 C35 1.438(5) . ? N13 C8 1.463(5) . ? N14 C44 1.378(5) . ? N14 C33 1.435(5) . ? N14 C26 1.449(5) . ? N15 C46 1.385(4) . ? N15 C48 1.423(5) . ? N15 C27 1.488(4) . ? N16 C50 1.353(4) . ? N16 C27 1.452(4) . ? N16 C32 1.464(4) . ? N17 C24 1.374(4) . ? N17 C1 1.437(4) . ? N17 C43 1.441(4) . ? N18 C38 1.369(5) . ? N18 C33 1.439(5) . ? N18 C40 1.449(4) . ? N19 C46 1.359(4) . ? N19 C8 1.437(4) . ? N19 C43 1.475(4) . ? N20 C23 1.370(5) . ? N20 C17 1.431(5) . ? N20 C21 1.471(4) . ? C1 C25 1.517(5) . ? C1 C21 1.571(5) . ? C2 C6 1.488(7) . ? C2 C30 1.527(6) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C52 1.543(8) . ? C3 C21 1.536(5) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.536(5) . ? C4 C54 1.540(7) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C42 1.632(5) . ? C6 C11 1.492(6) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C16 1.511(7) . ? C7 C9 1.537(7) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C30 1.540(5) . ? C8 C27 1.580(5) . ? C9 C40 1.527(5) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C16 1.522(7) . ? C10 C39 1.550(6) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C27 1.560(5) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C19 1.513(8) . ? C12 C15 1.559(6) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C34 1.547(5) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C22 1.501(6) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C22 C26 1.524(5) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C25 C53 1.544(7) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C34 1.593(5) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C51 1.498(7) . ? C29 C42 1.538(5) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C39 C40 1.564(5) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C51 C54 1.522(8) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C52 C53 1.577(9) . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C54 H54A 0.9700 . ? C54 H54B 0.9700 . ? 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 Cl2 Pr1 O1 129.71(8) . 3 ? Cl2 Pr1 Cl1 142.26(8) . . ? O1 Pr1 Cl1 72.36(8) 3 . ? Cl2 Pr1 O2W 91.41(9) . . ? O1 Pr1 O2W 137.47(9) 3 . ? Cl1 Pr1 O2W 80.61(9) . . ? Cl2 Pr1 O3W 69.60(9) . . ? O1 Pr1 O3W 66.01(9) 3 . ? Cl1 Pr1 O3W 138.04(10) . . ? O2W Pr1 O3W 135.64(11) . . ? Cl2 Pr1 O7 69.13(8) . . ? O1 Pr1 O7 132.16(8) 3 . ? Cl1 Pr1 O7 73.97(8) . . ? O2W Pr1 O7 66.14(8) . . ? O3W Pr1 O7 133.15(8) . . ? Cl2 Pr1 O8 74.59(8) . . ? O1 Pr1 O8 75.05(8) 3 . ? Cl1 Pr1 O8 85.46(8) . . ? O2W Pr1 O8 135.40(8) . . ? O3W Pr1 O8 79.23(10) . . ? O7 Pr1 O8 69.31(7) . . ? Cl2 Pr1 O4 141.69(8) . 3 ? O1 Pr1 O4 70.09(8) 3 3 ? Cl1 Pr1 O4 69.34(8) . 3 ? O2W Pr1 O4 69.91(8) . 3 ? O3W Pr1 O4 100.21(9) . 3 ? O7 Pr1 O4 126.04(8) . 3 ? O8 Pr1 O4 141.66(8) . 3 ? Cl2 Pr1 O1W 72.15(10) . . ? O1 Pr1 O1W 108.86(11) 3 . ? Cl1 Pr1 O1W 135.81(11) . . ? O2W Pr1 O1W 69.71(12) . . ? O3W Pr1 O1W 66.40(13) . . ? O7 Pr1 O1W 118.98(11) . . ? O8 Pr1 O1W 138.49(11) . . ? O4 Pr1 O1W 70.05(10) 3 . ? C41 O1 Pr1 157.7(2) . 11_454 ? C50 O4 Pr1 156.5(2) . 11_454 ? C24 O7 Pr1 159.1(2) . . ? C46 O8 Pr1 159.0(2) . . ? C20 N1 C34 115.0(3) . . ? C20 N1 C18 119.7(3) . . ? C34 N1 C18 124.5(3) . . ? C41 N2 C42 115.2(3) . . ? C41 N2 C32 121.4(3) . . ? C42 N2 C32 123.3(3) . . ? C38 N3 C39 111.5(3) . . ? C38 N3 C14 119.7(3) . . ? C39 N3 C14 127.6(3) . . ? C49 N4 C17 122.5(3) . . ? C49 N4 C39 111.6(3) . . ? C17 N4 C39 125.7(3) . . ? C44 N5 C34 114.2(3) . . ? C44 N5 C28 120.2(3) . . ? C34 N5 C28 125.6(3) . . ? C20 N6 C31 121.0(3) . . ? C20 N6 C26 112.1(3) . . ? C31 N6 C26 126.8(3) . . ? C41 N7 C18 121.3(3) . . ? C41 N7 C5 113.2(3) . . ? C18 N7 C5 124.8(3) . . ? C24 N8 C14 121.9(3) . . ? C24 N8 C21 111.7(3) . . ? C14 N8 C21 124.8(3) . . ? C47 N9 C28 120.6(3) . . ? C47 N9 C5 113.6(3) . . ? C28 N9 C5 125.8(3) . . ? C23 N10 C35 120.7(3) . . ? C23 N10 C1 112.6(3) . . ? C35 N10 C1 125.4(3) . . ? C49 N11 C31 122.4(3) . . ? C49 N11 C40 112.2(3) . . ? C31 N11 C40 124.9(3) . . ? C47 N12 C48 120.2(3) . . ? C47 N12 C42 113.1(3) . . ? C48 N12 C42 124.9(3) . . ? C50 N13 C35 120.2(3) . . ? C50 N13 C8 112.2(3) . . ? C35 N13 C8 126.1(3) . . ? C44 N14 C33 120.9(3) . . ? C44 N14 C26 113.4(3) . . ? C33 N14 C26 125.5(3) . . ? C46 N15 C48 121.5(3) . . ? C46 N15 C27 112.1(3) . . ? C48 N15 C27 125.6(3) . . ? C50 N16 C27 112.4(3) . . ? C50 N16 C32 123.6(3) . . ? C27 N16 C32 124.0(3) . . ? C24 N17 C1 111.9(3) . . ? C24 N17 C43 120.8(3) . . ? C1 N17 C43 127.2(3) . . ? C38 N18 C33 120.8(3) . . ? C38 N18 C40 111.8(3) . . ? C33 N18 C40 127.4(3) . . ? C46 N19 C8 114.0(3) . . ? C46 N19 C43 120.5(3) . . ? C8 N19 C43 125.1(3) . . ? C23 N20 C17 122.8(3) . . ? C23 N20 C21 112.1(3) . . ? C17 N20 C21 125.1(3) . . ? N17 C1 N10 111.4(3) . . ? N17 C1 C25 112.7(3) . . ? N10 C1 C25 111.3(3) . . ? N17 C1 C21 104.5(3) . . ? N10 C1 C21 100.9(3) . . ? C25 C1 C21 115.2(3) . . ? C6 C2 C30 112.3(4) . . ? C6 C2 H2A 109.1 . . ? C30 C2 H2A 109.1 . . ? C6 C2 H2B 109.1 . . ? C30 C2 H2B 109.1 . . ? H2A C2 H2B 107.9 . . ? C52 C3 C21 111.6(4) . . ? C52 C3 H3A 109.3 . . ? C21 C3 H3A 109.3 . . ? C52 C3 H3B 109.3 . . ? C21 C3 H3B 109.3 . . ? H3A C3 H3B 107.9 . . ? C5 C4 C54 113.3(4) . . ? C5 C4 H4A 108.9 . . ? C54 C4 H4A 108.9 . . ? C5 C4 H4B 108.9 . . ? C54 C4 H4B 108.9 . . ? H4A C4 H4B 107.7 . . ? N9 C5 N7 115.2(3) . . ? N9 C5 C4 113.9(3) . . ? N7 C5 C4 113.9(3) . . ? N9 C5 C42 101.4(3) . . ? N7 C5 C42 100.8(3) . . ? C4 C5 C42 109.8(3) . . ? C2 C6 C11 114.8(4) . . ? C2 C6 H6A 108.6 . . ? C11 C6 H6A 108.6 . . ? C2 C6 H6B 108.6 . . ? C11 C6 H6B 108.6 . . ? H6A C6 H6B 107.5 . . ? C16 C7 C9 113.5(4) . . ? C16 C7 H7A 108.9 . . ? C9 C7 H7A 108.9 . . ? C16 C7 H7B 108.9 . . ? C9 C7 H7B 108.9 . . ? H7A C7 H7B 107.7 . . ? N19 C8 N13 117.0(3) . . ? N19 C8 C30 111.5(3) . . ? N13 C8 C30 111.8(3) . . ? N19 C8 C27 103.5(3) . . ? N13 C8 C27 102.0(3) . . ? C30 C8 C27 110.1(3) . . ? C40 C9 C7 110.1(3) . . ? C40 C9 H9A 109.6 . . ? C7 C9 H9A 109.6 . . ? C40 C9 H9B 109.6 . . ? C7 C9 H9B 109.6 . . ? H9A C9 H9B 108.1 . . ? C16 C10 C39 108.7(4) . . ? C16 C10 H10A 110.0 . . ? C39 C10 H10A 110.0 . . ? C16 C10 H10B 109.9 . . ? C39 C10 H10B 109.9 . . ? H10A C10 H10B 108.3 . . ? C6 C11 C27 110.8(3) . . ? C6 C11 H11A 109.5 . . ? C27 C11 H11A 109.5 . . ? C6 C11 H11B 109.5 . . ? C27 C11 H11B 109.5 . . ? H11A C11 H11B 108.1 . . ? C19 C12 C15 110.7(4) . . ? C19 C12 H12A 109.5 . . ? C15 C12 H12A 109.5 . . ? C19 C12 H12B 109.5 . . ? C15 C12 H12B 109.5 . . ? H12A C12 H12B 108.1 . . ? N8 C14 N3 112.7(3) . . ? N8 C14 H14A 109.1 . . ? N3 C14 H14A 109.1 . . ? N8 C14 H14B 109.1 . . ? N3 C14 H14B 109.1 . . ? H14A C14 H14B 107.8 . . ? C34 C15 C12 110.0(3) . . ? C34 C15 H15A 109.7 . . ? C12 C15 H15A 109.7 . . ? C34 C15 H15B 109.6 . . ? C12 C15 H15B 109.6 . . ? H15A C15 H15B 108.2 . . ? C7 C16 C10 115.0(4) . . ? C7 C16 H16A 108.5 . . ? C10 C16 H16A 108.5 . . ? C7 C16 H16B 108.5 . . ? C10 C16 H16B 108.5 . . ? H16A C16 H16B 107.5 . . ? N20 C17 N4 112.8(3) . . ? N20 C17 H17A 109.0 . . ? N4 C17 H17A 109.0 . . ? N20 C17 H17B 109.0 . . ? N4 C17 H17B 109.0 . . ? H17A C17 H17B 107.8 . . ? N7 C18 N1 113.2(3) . . ? N7 C18 H18A 108.9 . . ? N1 C18 H18A 108.9 . . ? N7 C18 H18B 108.9 . . ? N1 C18 H18B 108.9 . . ? H18A C18 H18B 107.7 . . ? C12 C19 C22 115.0(4) . . ? C12 C19 H19A 108.5 . . ? C22 C19 H19A 108.5 . . ? C12 C19 H19B 108.5 . . ? C22 C19 H19B 108.5 . . ? H19A C19 H19B 107.5 . . ? O5 C20 N1 127.5(3) . . ? O5 C20 N6 124.0(3) . . ? N1 C20 N6 108.4(3) . . ? N8 C21 N20 113.7(3) . . ? N8 C21 C3 113.4(3) . . ? N20 C21 C3 113.3(3) . . ? N8 C21 C1 102.3(3) . . ? N20 C21 C1 103.8(3) . . ? C3 C21 C1 109.2(3) . . ? C19 C22 C26 111.5(3) . . ? C19 C22 H22A 109.3 . . ? C26 C22 H22A 109.3 . . ? C19 C22 H22B 109.3 . . ? C26 C22 H22B 109.3 . . ? H22A C22 H22B 108.0 . . ? O3 C23 N10 126.1(4) . . ? O3 C23 N20 124.4(3) . . ? N10 C23 N20 109.4(3) . . ? O7 C24 N17 127.0(3) . . ? O7 C24 N8 123.9(3) . . ? N17 C24 N8 109.1(3) . . ? C1 C25 C53 110.9(4) . . ? C1 C25 H25A 109.5 . . ? C53 C25 H25A 109.5 . . ? C1 C25 H25B 109.5 . . ? C53 C25 H25B 109.5 . . ? H25A C25 H25B 108.1 . . ? N14 C26 N6 114.3(3) . . ? N14 C26 C22 112.6(3) . . ? N6 C26 C22 113.0(3) . . ? N14 C26 C34 102.9(3) . . ? N6 C26 C34 103.0(3) . . ? C22 C26 C34 110.0(3) . . ? N16 C27 N15 114.3(3) . . ? N16 C27 C11 113.6(3) . . ? N15 C27 C11 111.7(3) . . ? N16 C27 C8 102.9(3) . . ? N15 C27 C8 101.2(3) . . ? C11 C27 C8 112.0(3) . . ? N9 C28 N5 116.3(3) . . ? N9 C28 H28A 108.2 . . ? N5 C28 H28A 108.2 . . ? N9 C28 H28B 108.2 . . ? N5 C28 H28B 108.2 . . ? H28A C28 H28B 107.4 . . ? C51 C29 C42 110.8(4) . . ? C51 C29 H29A 109.5 . . ? C42 C29 H29A 109.5 . . ? C51 C29 H29B 109.5 . . ? C42 C29 H29B 109.5 . . ? H29A C29 H29B 108.1 . . ? C2 C30 C8 112.0(3) . . ? C2 C30 H30A 109.2 . . ? C8 C30 H30A 109.2 . . ? C2 C30 H30B 109.2 . . ? C8 C30 H30B 109.2 . . ? H30A C30 H30B 107.9 . . ? N6 C31 N11 114.4(3) . . ? N6 C31 H31A 108.7 . . ? N11 C31 H31A 108.6 . . ? N6 C31 H31B 108.7 . . ? N11 C31 H31B 108.7 . . ? H31A C31 H31B 107.6 . . ? N16 C32 N2 113.3(3) . . ? N16 C32 H32A 108.9 . . ? N2 C32 H32A 108.9 . . ? N16 C32 H32B 108.9 . . ? N2 C32 H32B 108.9 . . ? H32A C32 H32B 107.7 . . ? N14 C33 N18 117.4(3) . . ? N14 C33 H33A 108.0 . . ? N18 C33 H33A 107.9 . . ? N14 C33 H33B 107.9 . . ? N18 C33 H33B 107.9 . . ? H33A C33 H33B 107.2 . . ? N1 C34 N5 114.3(3) . . ? N1 C34 C15 111.3(3) . . ? N5 C34 C15 114.8(3) . . ? N1 C34 C26 101.2(3) . . ? N5 C34 C26 101.8(3) . . ? C15 C34 C26 112.2(3) . . ? N13 C35 N10 114.0(3) . . ? N13 C35 H35A 108.8 . . ? N10 C35 H35A 108.7 . . ? N13 C35 H35B 108.8 . . ? N10 C35 H35B 108.8 . . ? H35A C35 H35B 107.6 . . ? O10 C38 N18 125.3(3) . . ? O10 C38 N3 125.5(3) . . ? N18 C38 N3 109.1(3) . . ? N3 C39 N4 111.3(3) . . ? N3 C39 C10 112.8(3) . . ? N4 C39 C10 111.8(3) . . ? N3 C39 C40 103.6(3) . . ? N4 C39 C40 103.1(3) . . ? C10 C39 C40 113.7(3) . . ? N18 C40 N11 112.7(3) . . ? N18 C40 C9 111.8(3) . . ? N11 C40 C9 112.6(3) . . ? N18 C40 C39 103.4(3) . . ? N11 C40 C39 103.2(3) . . ? C9 C40 C39 112.4(3) . . ? O1 C41 N2 127.8(3) . . ? O1 C41 N7 123.7(3) . . ? N2 C41 N7 108.5(3) . . ? N2 C42 N12 113.9(3) . . ? N2 C42 C29 113.3(3) . . ? N12 C42 C29 113.9(3) . . ? N2 C42 C5 101.6(3) . . ? N12 C42 C5 101.6(3) . . ? C29 C42 C5 111.1(3) . . ? N17 C43 N19 113.9(3) . . ? N17 C43 H43A 108.8 . . ? N19 C43 H43A 108.8 . . ? N17 C43 H43B 108.8 . . ? N19 C43 H43B 108.8 . . ? H43A C43 H43B 107.7 . . ? O6 C44 N5 125.5(3) . . ? O6 C44 N14 127.4(3) . . ? N5 C44 N14 107.2(3) . . ? O8 C46 N19 126.6(3) . . ? O8 C46 N15 125.4(3) . . ? N19 C46 N15 108.0(3) . . ? O9 C47 N12 126.6(3) . . ? O9 C47 N9 123.9(3) . . ? N12 C47 N9 109.4(3) . . ? N15 C48 N12 114.2(3) . . ? N15 C48 H48A 108.7 . . ? N12 C48 H48A 108.7 . . ? N15 C48 H48B 108.7 . . ? N12 C48 H48B 108.7 . . ? H48A C48 H48B 107.6 . . ? O2 C49 N11 125.7(4) . . ? O2 C49 N4 125.0(3) . . ? N11 C49 N4 109.4(3) . . ? O4 C50 N16 125.4(3) . . ? O4 C50 N13 124.8(3) . . ? N16 C50 N13 109.7(3) . . ? C29 C51 C54 113.0(4) . . ? C29 C51 H51A 109.0 . . ? C54 C51 H51A 109.0 . . ? C29 C51 H51B 109.0 . . ? C54 C51 H51B 109.0 . . ? H51A C51 H51B 107.8 . . ? C3 C52 C53 114.1(4) . . ? C3 C52 H52A 108.7 . . ? C53 C52 H52A 108.7 . . ? C3 C52 H52B 108.7 . . ? C53 C52 H52B 108.7 . . ? H52A C52 H52B 107.6 . . ? C25 C53 C52 109.3(4) . . ? C25 C53 H53A 109.8 . . ? C52 C53 H53A 109.8 . . ? C25 C53 H53B 109.8 . . ? C52 C53 H53B 109.8 . . ? H53A C53 H53B 108.3 . . ? C51 C54 C4 112.2(4) . . ? C51 C54 H54A 109.2 . . ? C4 C54 H54A 109.2 . . ? C51 C54 H54B 109.2 . . ? C4 C54 H54B 109.2 . . ? H54A C54 H54B 107.9 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.20 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.255 _refine_diff_density_min -0.773 _refine_diff_density_rms 0.127 # Attachment 'Sm.cif' data_Sm _database_code_depnum_ccdc_archive 'CCDC 883411' #TrackingRef 'Sm.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H92 Cl2 N21 O29 Sm' _chemical_formula_weight 1671.91 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0030 0.0020 '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' Cl Cl 0.1480 0.1590 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sm Sm -0.1640 3.4420 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 27.1046(13) _cell_length_b 18.3417(9) _cell_length_c 30.4416(15) _cell_angle_alpha 90.00 _cell_angle_beta 114.564(2) _cell_angle_gamma 90.00 _cell_volume 13764.2(12) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 7393 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 21.36 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.614 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6934 _exptl_absorpt_coefficient_mu 1.031 _exptl_absorpt_correction_type 'multi scan' _exptl_absorpt_correction_T_min 0.7206 _exptl_absorpt_correction_T_max 0.7899 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 61730 _diffrn_reflns_av_R_equivalents 0.0792 _diffrn_reflns_av_sigmaI/netI 0.0698 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 26.00 _reflns_number_total 13357 _reflns_number_gt 9834 _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. loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.048 0.411 -0.062 3899 1625 ' ' 2 0.000 0.408 0.250 43 36 ' ' 3 0.000 0.592 0.750 43 36 ' ' 4 0.211 0.141 0.178 48 10 ' ' 5 0.211 0.859 0.678 48 10 ' ' 6 0.289 0.641 0.322 48 11 ' ' 7 0.289 0.359 0.822 48 10 ' ' 8 0.500 0.908 0.250 43 36 ' ' 9 0.500 0.092 0.750 43 36 ' ' 10 0.711 0.641 0.178 48 10 ' ' 11 0.711 0.359 0.678 48 10 ' ' 12 0.789 0.141 0.322 48 11 ' ' 13 0.789 0.859 0.822 48 10 ' ' _platon_squeeze_details ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0954P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13357 _refine_ls_number_parameters 766 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0704 _refine_ls_R_factor_gt 0.0533 _refine_ls_wR_factor_ref 0.1538 _refine_ls_wR_factor_gt 0.1452 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sm1 Sm 0.309561(9) 0.390303(12) 0.245671(8) 0.02205(10) Uani 1 1 d . . . Cl1 Cl 0.32881(13) 0.4180(2) 0.32815(11) 0.1321(10) Uani 1 1 d . . . Cl2 Cl 0.24310(14) 0.3624(2) 0.16694(11) 0.1293(10) Uani 1 1 d . . . O1W O 0.40800(13) 0.39832(18) 0.29339(13) 0.0351(8) Uani 1 1 d . . . O2W O 0.35313(17) 0.38452(19) 0.18951(14) 0.0418(9) Uani 1 1 d . . . O1 O 0.08156(14) 0.02590(17) 0.15778(11) 0.0325(8) Uani 1 1 d . . . O2 O 0.12810(14) -0.01649(19) 0.08276(11) 0.0321(8) Uani 1 1 d . . . O3 O 0.24888(12) -0.06384(17) 0.14181(11) 0.0248(7) Uani 1 1 d . . . O4 O 0.17042(12) 0.01252(16) 0.26659(11) 0.0220(7) Uani 1 1 d . . . O5 O 0.26733(12) -0.03615(16) 0.25695(10) 0.0205(6) Uani 1 1 d . . . O6 O 0.30950(13) 0.25437(17) 0.14396(11) 0.0297(8) Uani 1 1 d . . . O7 O 0.13898(13) 0.34278(17) 0.14592(11) 0.0268(7) Uani 1 1 d . . . O8 O 0.18809(14) 0.29963(18) 0.07528(11) 0.0314(8) Uani 1 1 d . . . O9 O 0.34220(12) 0.26976(16) 0.25705(11) 0.0236(7) Uani 1 1 d . . . O10 O 0.24213(11) 0.31587(16) 0.25857(10) 0.0206(7) Uani 1 1 d . . . N1 N 0.17198(13) 0.25252(18) 0.26466(11) 0.0150(7) Uani 1 1 d . . . N2 N 0.19170(15) 0.1858(2) 0.04472(13) 0.0261(9) Uani 1 1 d . . . N3 N 0.09206(15) 0.0950(2) 0.05202(13) 0.0251(9) Uani 1 1 d . . . N4 N 0.11418(15) 0.2220(2) 0.04624(13) 0.0261(9) Uani 1 1 d . . . N5 N 0.26046(14) 0.0259(2) 0.09385(12) 0.0206(8) Uani 1 1 d . . . N6 N 0.16642(15) 0.0588(2) 0.04473(12) 0.0242(8) Uani 1 1 d . . . N7 N 0.14233(14) 0.12883(19) 0.27011(12) 0.0171(7) Uani 1 1 d . . . N8 N 0.05540(15) 0.1271(2) 0.10948(13) 0.0235(8) Uani 1 1 d . . . N9 N 0.07434(14) 0.13964(19) 0.18731(12) 0.0195(8) Uani 1 1 d . . . N10 N 0.25683(13) 0.22394(19) 0.31446(12) 0.0169(7) Uani 1 1 d . . . N11 N 0.30944(13) 0.05691(18) 0.31021(11) 0.0150(7) Uani 1 1 d . . . N12 N 0.10173(13) 0.26467(19) 0.18275(11) 0.0167(7) Uani 1 1 d . . . N13 N 0.28519(15) 0.15373(19) 0.09497(12) 0.0213(8) Uani 1 1 d . . . N14 N 0.34906(15) 0.14193(19) 0.16964(12) 0.0196(8) Uani 1 1 d . . . N15 N 0.32137(14) 0.01575(19) 0.16978(12) 0.0170(7) Uani 1 1 d . . . N16 N 0.37013(14) 0.15271(18) 0.25503(12) 0.0163(7) Uani 1 1 d . . . N17 N 0.07654(15) 0.2545(2) 0.10361(12) 0.0217(8) Uani 1 1 d . . . N18 N 0.33987(14) 0.02747(18) 0.25495(12) 0.0157(7) Uani 1 1 d . . . N19 N 0.33879(14) 0.18163(18) 0.30960(12) 0.0165(7) Uani 1 1 d . . . N20 N 0.22737(14) 0.09911(17) 0.31616(12) 0.0164(7) Uani 1 1 d . . . C1 C 0.1017(2) 0.0721(3) -0.06255(19) 0.0477(15) Uani 1 1 d . . . H1A H 0.1124 0.0218 -0.0541 0.057 Uiso 1 1 calc R . . H1B H 0.0942 0.0785 -0.0964 0.057 Uiso 1 1 calc R . . C2 C 0.3516(2) -0.0141(3) 0.06812(19) 0.0441(14) Uani 1 1 d . . . H2A H 0.3693 -0.0207 0.0465 0.053 Uiso 1 1 calc R . . H2B H 0.3239 -0.0514 0.0606 0.053 Uiso 1 1 calc R . . C3 C 0.0491(2) 0.0869(3) -0.0559(2) 0.0487(15) Uani 1 1 d . . . H3A H 0.0189 0.0909 -0.0873 0.058 Uiso 1 1 calc R . . H3B H 0.0421 0.0461 -0.0391 0.058 Uiso 1 1 calc R . . C4 C -0.01868(19) 0.2193(3) 0.08244(17) 0.0362(13) Uani 1 1 d . . . H4A H -0.0407 0.1824 0.0885 0.043 Uiso 1 1 calc R . . H4B H -0.0259 0.2171 0.0485 0.043 Uiso 1 1 calc R . . C5 C 0.3246(2) 0.0606(3) 0.05913(16) 0.0324(12) Uani 1 1 d . . . H5A H 0.3509 0.0975 0.0606 0.039 Uiso 1 1 calc R . . H5B H 0.2953 0.0618 0.0270 0.039 Uiso 1 1 calc R . . C6 C 0.0530(2) 0.1564(3) -0.02747(16) 0.0360(13) Uani 1 1 d . . . H6A H 0.0195 0.1635 -0.0236 0.043 Uiso 1 1 calc R . . H6B H 0.0579 0.1978 -0.0451 0.043 Uiso 1 1 calc R . . C7 C 0.21167(18) 0.0099(3) 0.05123(15) 0.0241(10) Uani 1 1 d . . . H7A H 0.2007 -0.0399 0.0533 0.029 Uiso 1 1 calc R . . H7B H 0.2196 0.0132 0.0231 0.029 Uiso 1 1 calc R . . C8 C -0.0349(2) 0.2951(3) 0.09400(18) 0.0447(15) Uani 1 1 d . . . H8A H -0.0193 0.3323 0.0810 0.054 Uiso 1 1 calc R . . H8B H -0.0740 0.3000 0.0783 0.054 Uiso 1 1 calc R . . C9 C 0.4431(2) -0.0009(3) 0.34220(17) 0.0302(11) Uani 1 1 d . . . H9A H 0.4813 -0.0130 0.3585 0.036 Uiso 1 1 calc R . . H9B H 0.4241 -0.0440 0.3250 0.036 Uiso 1 1 calc R . . C10 C 0.07736(18) 0.2694(3) 0.05716(15) 0.0234(10) Uani 1 1 d . . . H10A H 0.0881 0.3197 0.0566 0.028 Uiso 1 1 calc R . . H10B H 0.0410 0.2636 0.0321 0.028 Uiso 1 1 calc R . . C11 C 0.04691(18) 0.0898(3) 0.06502(15) 0.0257(10) Uani 1 1 d . . . H11A H 0.0397 0.0387 0.0683 0.031 Uiso 1 1 calc R . . H11B H 0.0150 0.1100 0.0391 0.031 Uiso 1 1 calc R . . C12 C 0.04118(17) 0.2028(2) 0.11285(15) 0.0209(9) Uani 1 1 d . . . C13 C 0.10038(18) 0.1519(2) 0.02200(15) 0.0234(10) Uani 1 1 d . . . C14 C 0.38808(17) 0.1645(2) 0.21663(15) 0.0211(9) Uani 1 1 d . . . H14A H 0.3957 0.2160 0.2154 0.025 Uiso 1 1 calc R . . H14B H 0.4216 0.1380 0.2243 0.025 Uiso 1 1 calc R . . C15 C 0.3933(2) -0.0243(3) 0.12018(18) 0.0321(11) Uani 1 1 d . . . H15A H 0.4280 -0.0369 0.1199 0.039 Uiso 1 1 calc R . . H15B H 0.3822 -0.0648 0.1345 0.039 Uiso 1 1 calc R . . C16 C 0.1477(2) 0.1203(3) -0.03307(16) 0.0343(12) Uani 1 1 d . . . H16A H 0.1419 0.1683 -0.0477 0.041 Uiso 1 1 calc R . . H16B H 0.1809 0.1008 -0.0332 0.041 Uiso 1 1 calc R . . C17 C 0.30230(18) 0.0777(2) 0.09623(14) 0.0205(9) Uani 1 1 d . . . C18 C 0.15437(18) 0.1274(2) 0.01912(15) 0.0226(10) Uani 1 1 d . . . C19 C 0.24805(19) 0.1915(3) 0.05223(15) 0.0253(10) Uani 1 1 d . . . H19A H 0.2518 0.1717 0.0242 0.030 Uiso 1 1 calc R . . H19B H 0.2580 0.2426 0.0548 0.030 Uiso 1 1 calc R . . C20 C 0.13373(17) 0.2260(2) 0.32398(15) 0.0209(9) Uani 1 1 d . . . H20A H 0.1267 0.1865 0.3418 0.025 Uiso 1 1 calc R . . H20B H 0.0991 0.2455 0.3016 0.025 Uiso 1 1 calc R . . C21 C 0.12928(17) 0.2969(2) 0.23008(14) 0.0162(9) Uani 1 1 d . . . H21A H 0.1027 0.3071 0.2429 0.019 Uiso 1 1 calc R . . H21B H 0.1448 0.3431 0.2267 0.019 Uiso 1 1 calc R . . C22 C 0.43602(17) 0.0596(2) 0.30567(16) 0.0230(10) Uani 1 1 d . . . H22A H 0.4594 0.1003 0.3217 0.028 Uiso 1 1 calc R . . H22B H 0.4465 0.0418 0.2808 0.028 Uiso 1 1 calc R . . C23 C 0.16579(19) 0.2855(3) 0.35900(16) 0.0274(11) Uani 1 1 d . . . H23A H 0.1464 0.3003 0.3780 0.033 Uiso 1 1 calc R . . H23B H 0.1684 0.3276 0.3408 0.033 Uiso 1 1 calc R . . C24 C 0.31438(18) 0.1896(3) 0.13725(16) 0.0234(10) Uani 1 1 d . . . C25 C 0.16679(19) 0.2416(3) 0.05739(15) 0.0268(11) Uani 1 1 d . . . C26 C 0.4221(2) 0.0193(3) 0.38020(17) 0.0306(11) Uani 1 1 d . . . H26A H 0.3947 -0.0157 0.3789 0.037 Uiso 1 1 calc R . . H26B H 0.4517 0.0164 0.4121 0.037 Uiso 1 1 calc R . . C27 C 0.10911(17) 0.2923(2) 0.14442(15) 0.0200(9) Uani 1 1 d . . . C28 C 0.37727(16) 0.0849(2) 0.28275(14) 0.0163(9) Uani 1 1 d . . . C29 C 0.40072(17) 0.0434(3) 0.15169(16) 0.0237(10) Uani 1 1 d . . . H29A H 0.4249 0.0321 0.1848 0.028 Uiso 1 1 calc R . . H29B H 0.4171 0.0821 0.1405 0.028 Uiso 1 1 calc R . . C30 C 0.00974(17) 0.2399(2) 0.17869(16) 0.0211(9) Uani 1 1 d . . . H30A H 0.0225 0.2516 0.2127 0.025 Uiso 1 1 calc R . . H30B H -0.0174 0.2019 0.1712 0.025 Uiso 1 1 calc R . . C31 C 0.27380(17) -0.0125(2) 0.13589(14) 0.0198(9) Uani 1 1 d . . . C32 C 0.34936(16) 0.2070(2) 0.27247(14) 0.0171(9) Uani 1 1 d . . . C33 C 0.27564(17) 0.0542(2) 0.33649(14) 0.0171(9) Uani 1 1 d . . . H33A H 0.2970 0.0696 0.3695 0.021 Uiso 1 1 calc R . . H33B H 0.2648 0.0040 0.3375 0.021 Uiso 1 1 calc R . . C34 C 0.12913(19) 0.0403(3) 0.06232(15) 0.0262(11) Uani 1 1 d . . . C35 C 0.39799(18) 0.0952(2) 0.37270(15) 0.0231(10) Uani 1 1 d . . . H35A H 0.4266 0.1309 0.3794 0.028 Uiso 1 1 calc R . . H35B H 0.3816 0.1034 0.3952 0.028 Uiso 1 1 calc R . . C36 C 0.23692(18) 0.1839(2) 0.38266(14) 0.0209(9) Uani 1 1 d . . . H36A H 0.2751 0.1741 0.4018 0.025 Uiso 1 1 calc R . . H36B H 0.2160 0.1488 0.3917 0.025 Uiso 1 1 calc R . . C37 C -0.01581(19) 0.3078(3) 0.14844(16) 0.0280(11) Uani 1 1 d . . . H37A H 0.0105 0.3471 0.1585 0.034 Uiso 1 1 calc R . . H37B H -0.0466 0.3229 0.1547 0.034 Uiso 1 1 calc R . . C38 C 0.08570(16) 0.1164(2) 0.23616(14) 0.0167(9) Uani 1 1 d . . . H38A H 0.0776 0.0648 0.2358 0.020 Uiso 1 1 calc R . . H38B H 0.0620 0.1426 0.2474 0.020 Uiso 1 1 calc R . . C39 C 0.17958(16) 0.0744(2) 0.28265(14) 0.0157(9) Uani 1 1 d . . . C40 C 0.22516(17) 0.2683(2) 0.27713(14) 0.0163(9) Uani 1 1 d . . . C41 C 0.07136(17) 0.0906(3) 0.15219(15) 0.0232(10) Uani 1 1 d . . . C42 C 0.30199(16) 0.0122(2) 0.27238(14) 0.0137(8) Uani 1 1 d . . . C43 C 0.16456(16) 0.1969(2) 0.29599(14) 0.0141(8) Uani 1 1 d . . . C44 C 0.34605(18) -0.0162(2) 0.21760(14) 0.0177(9) Uani 1 1 d . . . H44A H 0.3844 -0.0233 0.2262 0.021 Uiso 1 1 calc R . . H44B H 0.3300 -0.0638 0.2167 0.021 Uiso 1 1 calc R . . C45 C 0.2234(2) 0.2609(3) 0.39326(16) 0.0287(11) Uani 1 1 d . . . H45A H 0.2495 0.2947 0.3905 0.034 Uiso 1 1 calc R . . H45B H 0.2268 0.2629 0.4263 0.034 Uiso 1 1 calc R . . C46 C 0.05706(16) 0.2123(2) 0.16844(14) 0.0185(9) Uani 1 1 d . . . C47 C 0.34616(17) 0.0691(2) 0.14962(14) 0.0185(9) Uani 1 1 d . . . C48 C 0.31553(16) 0.2273(2) 0.33522(14) 0.0168(9) Uani 1 1 d . . . H48A H 0.3296 0.2118 0.3687 0.020 Uiso 1 1 calc R . . H48B H 0.3267 0.2774 0.3346 0.020 Uiso 1 1 calc R . . C49 C 0.22433(16) 0.1751(2) 0.32952(14) 0.0149(8) Uani 1 1 d . . . C50 C 0.35552(16) 0.1056(2) 0.32147(14) 0.0153(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sm1 0.02323(15) 0.01369(15) 0.03099(14) 0.00070(9) 0.01302(10) 0.00028(9) Cl1 0.116(2) 0.167(3) 0.109(2) -0.019(2) 0.0422(17) 0.001(2) Cl2 0.122(2) 0.151(3) 0.111(2) -0.0075(19) 0.0446(18) -0.005(2) O1W 0.0220(18) 0.033(2) 0.046(2) -0.0017(16) 0.0106(15) 0.0047(15) O2W 0.054(2) 0.033(2) 0.055(2) -0.0096(17) 0.039(2) -0.0090(17) O1 0.045(2) 0.0152(19) 0.0345(17) 0.0009(14) 0.0133(16) 0.0062(15) O2 0.037(2) 0.029(2) 0.0316(17) 0.0030(15) 0.0152(15) 0.0058(16) O3 0.0263(17) 0.0207(18) 0.0290(16) -0.0022(13) 0.0130(14) -0.0036(14) O4 0.0213(16) 0.0112(17) 0.0340(16) -0.0013(13) 0.0120(13) -0.0001(12) O5 0.0237(17) 0.0158(16) 0.0268(15) -0.0052(13) 0.0153(13) -0.0040(13) O6 0.0323(19) 0.0191(19) 0.0322(17) -0.0019(14) 0.0079(14) 0.0062(14) O7 0.0308(18) 0.0212(18) 0.0301(16) 0.0041(14) 0.0143(14) 0.0002(14) O8 0.0353(19) 0.0223(19) 0.0343(17) -0.0040(15) 0.0123(15) 0.0038(15) O9 0.0286(18) 0.0108(17) 0.0348(16) 0.0038(13) 0.0164(14) 0.0036(13) O10 0.0197(16) 0.0154(16) 0.0275(15) 0.0054(13) 0.0105(13) -0.0020(12) N1 0.0114(17) 0.0142(19) 0.0186(16) 0.0027(14) 0.0053(14) 0.0012(14) N2 0.026(2) 0.026(2) 0.0261(19) -0.0023(16) 0.0111(16) 0.0072(17) N3 0.026(2) 0.027(2) 0.0208(17) -0.0017(16) 0.0076(16) 0.0032(17) N4 0.029(2) 0.024(2) 0.0246(18) -0.0067(16) 0.0102(16) 0.0032(17) N5 0.021(2) 0.017(2) 0.0215(17) -0.0004(15) 0.0070(15) 0.0009(15) N6 0.027(2) 0.024(2) 0.0218(17) 0.0016(16) 0.0104(16) 0.0090(17) N7 0.0180(19) 0.0109(18) 0.0232(17) -0.0017(14) 0.0093(15) -0.0005(14) N8 0.027(2) 0.020(2) 0.0248(18) -0.0045(15) 0.0112(16) -0.0013(16) N9 0.0210(19) 0.0147(19) 0.0199(17) 0.0010(15) 0.0058(15) 0.0078(15) N10 0.0147(18) 0.0159(19) 0.0212(17) 0.0039(14) 0.0084(14) 0.0044(14) N11 0.0146(17) 0.0109(18) 0.0207(16) -0.0017(14) 0.0086(14) 0.0005(14) N12 0.0137(18) 0.018(2) 0.0182(16) -0.0009(14) 0.0065(14) -0.0005(14) N13 0.025(2) 0.016(2) 0.0238(18) 0.0006(15) 0.0111(15) 0.0045(15) N14 0.025(2) 0.0132(19) 0.0203(17) 0.0013(15) 0.0093(15) 0.0043(15) N15 0.0181(18) 0.0146(19) 0.0194(16) 0.0006(14) 0.0089(14) 0.0011(14) N16 0.0191(18) 0.0092(19) 0.0238(17) 0.0011(14) 0.0120(14) 0.0008(14) N17 0.023(2) 0.019(2) 0.0238(18) 0.0020(15) 0.0106(15) 0.0009(16) N18 0.0191(19) 0.0078(18) 0.0223(17) -0.0046(14) 0.0108(15) -0.0045(14) N19 0.0205(18) 0.0076(18) 0.0241(17) -0.0021(14) 0.0119(15) 0.0016(14) N20 0.0183(18) 0.0065(18) 0.0249(17) 0.0013(14) 0.0094(15) 0.0029(14) C1 0.062(4) 0.045(4) 0.032(3) -0.011(3) 0.015(3) 0.005(3) C2 0.046(3) 0.050(4) 0.042(3) -0.012(3) 0.024(3) 0.012(3) C3 0.051(4) 0.047(4) 0.034(3) -0.015(3) 0.004(3) -0.006(3) C4 0.021(3) 0.053(4) 0.025(2) 0.001(2) 0.000(2) 0.006(2) C5 0.034(3) 0.041(3) 0.027(2) 0.000(2) 0.017(2) 0.011(2) C6 0.033(3) 0.042(3) 0.022(2) -0.002(2) 0.000(2) 0.010(2) C7 0.023(2) 0.025(3) 0.022(2) -0.0064(19) 0.0076(18) 0.0040(19) C8 0.033(3) 0.062(4) 0.038(3) 0.014(3) 0.013(2) 0.029(3) C9 0.025(3) 0.025(3) 0.035(2) 0.005(2) 0.006(2) 0.015(2) C10 0.024(2) 0.022(3) 0.024(2) 0.0063(19) 0.0108(18) 0.0118(19) C11 0.023(2) 0.028(3) 0.023(2) -0.0106(19) 0.0060(18) -0.005(2) C12 0.018(2) 0.021(3) 0.022(2) 0.0015(18) 0.0074(17) 0.0029(18) C13 0.025(2) 0.023(3) 0.021(2) -0.0006(18) 0.0091(18) 0.0062(19) C14 0.020(2) 0.017(2) 0.028(2) -0.0003(18) 0.0115(18) -0.0011(18) C15 0.032(3) 0.026(3) 0.046(3) 0.001(2) 0.023(2) 0.010(2) C16 0.041(3) 0.043(3) 0.021(2) 0.001(2) 0.015(2) 0.007(2) C17 0.023(2) 0.019(2) 0.021(2) 0.0035(18) 0.0115(18) 0.0071(19) C18 0.026(2) 0.019(2) 0.021(2) -0.0003(18) 0.0084(18) 0.0059(19) C19 0.034(3) 0.021(3) 0.023(2) 0.0072(18) 0.014(2) 0.006(2) C20 0.021(2) 0.019(2) 0.026(2) 0.0011(18) 0.0138(18) 0.0028(18) C21 0.021(2) 0.009(2) 0.0200(19) 0.0012(16) 0.0101(17) 0.0069(17) C22 0.015(2) 0.021(3) 0.031(2) -0.0073(19) 0.0073(18) 0.0025(18) C23 0.033(3) 0.025(3) 0.033(2) -0.006(2) 0.022(2) 0.002(2) C24 0.026(2) 0.021(3) 0.031(2) 0.001(2) 0.019(2) 0.0022(19) C25 0.029(3) 0.029(3) 0.022(2) 0.001(2) 0.0093(19) 0.009(2) C26 0.025(3) 0.028(3) 0.032(2) 0.006(2) 0.005(2) 0.006(2) C27 0.018(2) 0.014(2) 0.027(2) 0.0046(18) 0.0087(18) 0.0066(18) C28 0.016(2) 0.010(2) 0.023(2) -0.0004(17) 0.0077(17) 0.0010(17) C29 0.016(2) 0.028(3) 0.031(2) 0.000(2) 0.0133(19) 0.0041(19) C30 0.014(2) 0.020(2) 0.030(2) 0.0000(19) 0.0110(18) 0.0038(18) C31 0.022(2) 0.017(2) 0.021(2) -0.0031(18) 0.0099(18) 0.0045(19) C32 0.014(2) 0.012(2) 0.022(2) -0.0028(17) 0.0051(16) -0.0015(17) C33 0.019(2) 0.014(2) 0.023(2) 0.0051(17) 0.0131(17) 0.0052(17) C34 0.029(3) 0.027(3) 0.0147(19) -0.0020(19) 0.0020(18) 0.009(2) C35 0.018(2) 0.025(3) 0.021(2) -0.0004(18) 0.0029(17) 0.0035(19) C36 0.025(2) 0.019(2) 0.019(2) 0.0014(18) 0.0097(18) 0.0040(18) C37 0.020(2) 0.026(3) 0.037(2) 0.006(2) 0.010(2) 0.008(2) C38 0.012(2) 0.013(2) 0.025(2) 0.0020(17) 0.0069(17) 0.0003(16) C39 0.019(2) 0.013(2) 0.022(2) 0.0041(17) 0.0157(17) 0.0049(17) C40 0.019(2) 0.012(2) 0.0172(19) -0.0023(16) 0.0072(17) 0.0019(17) C41 0.017(2) 0.024(3) 0.026(2) 0.0019(19) 0.0058(18) 0.0022(19) C42 0.013(2) 0.007(2) 0.0220(19) 0.0017(16) 0.0077(16) 0.0017(16) C43 0.014(2) 0.010(2) 0.0205(19) 0.0000(16) 0.0097(16) -0.0016(16) C44 0.023(2) 0.012(2) 0.0208(19) 0.0009(17) 0.0126(17) 0.0024(17) C45 0.034(3) 0.026(3) 0.028(2) -0.009(2) 0.015(2) 0.000(2) C46 0.015(2) 0.015(2) 0.024(2) 0.0044(17) 0.0056(17) 0.0055(17) C47 0.022(2) 0.014(2) 0.022(2) -0.0011(17) 0.0119(18) 0.0015(17) C48 0.019(2) 0.013(2) 0.0192(19) -0.0017(17) 0.0082(17) 0.0023(17) C49 0.017(2) 0.008(2) 0.0191(19) 0.0003(16) 0.0068(16) 0.0018(16) C50 0.017(2) 0.009(2) 0.0204(19) -0.0001(16) 0.0078(17) 0.0014(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sm1 O9 2.353(3) . ? Sm1 O4 2.372(3) 4 ? Sm1 Cl2 2.379(3) . ? Sm1 Cl1 2.397(3) . ? Sm1 O10 2.440(3) . ? Sm1 O2W 2.451(4) . ? Sm1 O1W 2.455(3) . ? Sm1 O5 2.456(3) 4 ? O1 C41 1.214(5) . ? O2 C34 1.220(6) . ? O3 C31 1.215(5) . ? O4 C39 1.219(5) . ? O4 Sm1 2.372(3) 4_545 ? O5 C42 1.235(5) . ? O5 Sm1 2.456(3) 4_545 ? O6 C24 1.222(5) . ? O7 C27 1.218(5) . ? O8 C25 1.226(6) . ? O9 C32 1.228(5) . ? O10 C40 1.228(5) . ? N1 C40 1.360(5) . ? N1 C21 1.448(5) . ? N1 C43 1.467(5) . ? N2 C25 1.367(6) . ? N2 C19 1.451(6) . ? N2 C18 1.457(6) . ? N3 C34 1.361(6) . ? N3 C11 1.438(6) . ? N3 C13 1.465(6) . ? N4 C25 1.369(6) . ? N4 C13 1.452(6) . ? N4 C10 1.462(6) . ? N5 C31 1.371(5) . ? N5 C7 1.446(5) . ? N5 C17 1.459(6) . ? N6 C34 1.368(6) . ? N6 C18 1.445(6) . ? N6 C7 1.465(6) . ? N7 C39 1.358(5) . ? N7 C43 1.465(5) . ? N7 C38 1.469(5) . ? N8 C41 1.364(6) . ? N8 C11 1.447(5) . ? N8 C12 1.456(6) . ? N9 C41 1.374(6) . ? N9 C46 1.451(5) . ? N9 C38 1.452(5) . ? N10 C40 1.371(5) . ? N10 C48 1.449(5) . ? N10 C49 1.457(5) . ? N11 C42 1.358(5) . ? N11 C33 1.446(5) . ? N11 C50 1.456(5) . ? N12 C27 1.361(5) . ? N12 C21 1.445(5) . ? N12 C46 1.462(5) . ? N13 C24 1.367(6) . ? N13 C19 1.448(5) . ? N13 C17 1.465(6) . ? N14 C24 1.360(6) . ? N14 C14 1.442(5) . ? N14 C47 1.456(6) . ? N15 C31 1.375(5) . ? N15 C44 1.449(5) . ? N15 C47 1.460(5) . ? N16 C32 1.356(5) . ? N16 C14 1.457(5) . ? N16 C28 1.469(5) . ? N17 C27 1.375(6) . ? N17 C10 1.449(5) . ? N17 C12 1.457(6) . ? N18 C42 1.366(5) . ? N18 C44 1.456(5) . ? N18 C28 1.463(5) . ? N19 C32 1.358(5) . ? N19 C48 1.454(5) . ? N19 C50 1.464(5) . ? N20 C39 1.351(5) . ? N20 C33 1.450(5) . ? N20 C49 1.464(5) . ? C1 C16 1.487(8) . ? C1 C3 1.544(9) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C5 1.523(7) . ? C2 C15 1.529(7) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C6 1.518(7) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C12 1.527(6) . ? C4 C8 1.542(7) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C17 1.519(6) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C13 1.522(6) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C37 1.535(7) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C22 1.526(6) . ? C9 C26 1.533(7) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C46 1.573(6) . ? C13 C18 1.568(6) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C29 1.531(7) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C18 1.528(6) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C47 1.573(6) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C43 1.517(6) . ? C20 C23 1.520(6) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C28 1.521(6) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C45 1.541(7) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C26 C35 1.514(6) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C28 C50 1.568(6) . ? C29 C47 1.529(6) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 C46 1.527(6) . ? C30 C37 1.532(6) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C35 C50 1.517(5) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 C49 1.517(5) . ? C36 C45 1.527(6) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C43 C49 1.565(5) . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O9 Sm1 O4 144.54(10) . 4 ? O9 Sm1 Cl2 91.55(11) . . ? O4 Sm1 Cl2 99.89(11) 4 . ? O9 Sm1 Cl1 98.04(11) . . ? O4 Sm1 Cl1 90.03(12) 4 . ? Cl2 Sm1 Cl1 147.63(12) . . ? O9 Sm1 O10 73.23(10) . . ? O4 Sm1 O10 142.15(10) 4 . ? Cl2 Sm1 O10 74.79(10) . . ? Cl1 Sm1 O10 78.53(11) . . ? O9 Sm1 O2W 78.54(11) . . ? O4 Sm1 O2W 73.92(11) 4 . ? Cl2 Sm1 O2W 70.77(12) . . ? Cl1 Sm1 O2W 141.42(13) . . ? O10 Sm1 O2W 134.29(11) . . ? O9 Sm1 O1W 73.72(11) . . ? O4 Sm1 O1W 76.88(11) 4 . ? Cl2 Sm1 O1W 142.21(12) . . ? Cl1 Sm1 O1W 69.99(12) . . ? O10 Sm1 O1W 129.85(11) . . ? O2W Sm1 O1W 72.24(13) . . ? O9 Sm1 O5 141.53(10) . 4 ? O4 Sm1 O5 73.88(10) 4 4 ? Cl2 Sm1 O5 78.96(11) . 4 ? Cl1 Sm1 O5 74.33(10) . 4 ? O10 Sm1 O5 68.30(10) . 4 ? O2W Sm1 O5 130.51(11) . 4 ? O1W Sm1 O5 133.25(11) . 4 ? C39 O4 Sm1 157.0(3) . 4_545 ? C42 O5 Sm1 155.3(3) . 4_545 ? C32 O9 Sm1 158.0(3) . . ? C40 O10 Sm1 157.0(3) . . ? C40 N1 C21 121.1(3) . . ? C40 N1 C43 112.5(3) . . ? C21 N1 C43 125.4(3) . . ? C25 N2 C19 120.8(4) . . ? C25 N2 C18 112.8(4) . . ? C19 N2 C18 126.1(4) . . ? C34 N3 C11 121.3(4) . . ? C34 N3 C13 112.2(4) . . ? C11 N3 C13 126.1(4) . . ? C25 N4 C13 112.3(4) . . ? C25 N4 C10 121.8(4) . . ? C13 N4 C10 125.9(4) . . ? C31 N5 C7 121.4(4) . . ? C31 N5 C17 113.0(3) . . ? C7 N5 C17 125.4(3) . . ? C34 N6 C18 112.9(4) . . ? C34 N6 C7 120.6(4) . . ? C18 N6 C7 126.5(4) . . ? C39 N7 C43 112.6(3) . . ? C39 N7 C38 121.4(3) . . ? C43 N7 C38 125.9(3) . . ? C41 N8 C11 121.5(4) . . ? C41 N8 C12 113.0(4) . . ? C11 N8 C12 125.0(4) . . ? C41 N9 C46 112.9(3) . . ? C41 N9 C38 121.5(4) . . ? C46 N9 C38 124.9(3) . . ? C40 N10 C48 122.2(3) . . ? C40 N10 C49 111.9(3) . . ? C48 N10 C49 125.9(3) . . ? C42 N11 C33 122.9(3) . . ? C42 N11 C50 112.4(3) . . ? C33 N11 C50 124.7(3) . . ? C27 N12 C21 120.2(3) . . ? C27 N12 C46 112.8(3) . . ? C21 N12 C46 125.9(3) . . ? C24 N13 C19 122.0(4) . . ? C24 N13 C17 112.4(3) . . ? C19 N13 C17 125.0(3) . . ? C24 N14 C14 122.4(4) . . ? C24 N14 C47 112.7(3) . . ? C14 N14 C47 124.7(3) . . ? C31 N15 C44 119.9(4) . . ? C31 N15 C47 112.9(3) . . ? C44 N15 C47 126.4(3) . . ? C32 N16 C14 122.4(3) . . ? C32 N16 C28 111.9(3) . . ? C14 N16 C28 125.3(3) . . ? C27 N17 C10 121.5(4) . . ? C27 N17 C12 112.4(3) . . ? C10 N17 C12 126.1(4) . . ? C42 N18 C44 122.7(3) . . ? C42 N18 C28 112.0(3) . . ? C44 N18 C28 124.8(3) . . ? C32 N19 C48 122.5(3) . . ? C32 N19 C50 112.4(3) . . ? C48 N19 C50 125.1(3) . . ? C39 N20 C33 122.9(3) . . ? C39 N20 C49 112.5(3) . . ? C33 N20 C49 124.6(3) . . ? C16 C1 C3 113.9(4) . . ? C16 C1 H1A 108.8 . . ? C3 C1 H1A 108.8 . . ? C16 C1 H1B 108.8 . . ? C3 C1 H1B 108.8 . . ? H1A C1 H1B 107.7 . . ? C5 C2 C15 112.9(4) . . ? C5 C2 H2A 109.0 . . ? C15 C2 H2A 109.0 . . ? C5 C2 H2B 109.0 . . ? C15 C2 H2B 109.0 . . ? H2A C2 H2B 107.8 . . ? C6 C3 C1 111.9(5) . . ? C6 C3 H3A 109.2 . . ? C1 C3 H3A 109.2 . . ? C6 C3 H3B 109.2 . . ? C1 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? C12 C4 C8 111.8(4) . . ? C12 C4 H4A 109.3 . . ? C8 C4 H4A 109.3 . . ? C12 C4 H4B 109.3 . . ? C8 C4 H4B 109.3 . . ? H4A C4 H4B 107.9 . . ? C17 C5 C2 111.2(4) . . ? C17 C5 H5A 109.4 . . ? C2 C5 H5A 109.4 . . ? C17 C5 H5B 109.4 . . ? C2 C5 H5B 109.4 . . ? H5A C5 H5B 108.0 . . ? C3 C6 C13 110.4(4) . . ? C3 C6 H6A 109.6 . . ? C13 C6 H6A 109.6 . . ? C3 C6 H6B 109.6 . . ? C13 C6 H6B 109.6 . . ? H6A C6 H6B 108.1 . . ? N5 C7 N6 113.5(3) . . ? N5 C7 H7A 108.9 . . ? N6 C7 H7A 108.9 . . ? N5 C7 H7B 108.9 . . ? N6 C7 H7B 108.9 . . ? H7A C7 H7B 107.7 . . ? C37 C8 C4 112.5(4) . . ? C37 C8 H8A 109.1 . . ? C4 C8 H8A 109.1 . . ? C37 C8 H8B 109.1 . . ? C4 C8 H8B 109.1 . . ? H8A C8 H8B 107.8 . . ? C22 C9 C26 113.6(4) . . ? C22 C9 H9A 108.8 . . ? C26 C9 H9A 108.8 . . ? C22 C9 H9B 108.8 . . ? C26 C9 H9B 108.8 . . ? H9A C9 H9B 107.7 . . ? N17 C10 N4 113.5(3) . . ? N17 C10 H10A 108.9 . . ? N4 C10 H10A 108.9 . . ? N17 C10 H10B 108.9 . . ? N4 C10 H10B 108.9 . . ? H10A C10 H10B 107.7 . . ? N3 C11 N8 113.8(4) . . ? N3 C11 H11A 108.8 . . ? N8 C11 H11A 108.8 . . ? N3 C11 H11B 108.8 . . ? N8 C11 H11B 108.8 . . ? H11A C11 H11B 107.7 . . ? N8 C12 N17 113.1(4) . . ? N8 C12 C4 113.0(4) . . ? N17 C12 C4 111.9(4) . . ? N8 C12 C46 102.7(3) . . ? N17 C12 C46 103.2(3) . . ? C4 C12 C46 112.2(4) . . ? N4 C13 N3 112.8(3) . . ? N4 C13 C6 112.9(4) . . ? N3 C13 C6 111.7(4) . . ? N4 C13 C18 103.5(4) . . ? N3 C13 C18 102.7(3) . . ? C6 C13 C18 112.5(4) . . ? N14 C14 N16 113.7(3) . . ? N14 C14 H14A 108.8 . . ? N16 C14 H14A 108.8 . . ? N14 C14 H14B 108.8 . . ? N16 C14 H14B 108.8 . . ? H14A C14 H14B 107.7 . . ? C2 C15 C29 113.5(4) . . ? C2 C15 H15A 108.9 . . ? C29 C15 H15A 108.9 . . ? C2 C15 H15B 108.9 . . ? C29 C15 H15B 108.9 . . ? H15A C15 H15B 107.7 . . ? C1 C16 C18 112.6(4) . . ? C1 C16 H16A 109.1 . . ? C18 C16 H16A 109.1 . . ? C1 C16 H16B 109.1 . . ? C18 C16 H16B 109.1 . . ? H16A C16 H16B 107.8 . . ? N5 C17 N13 112.8(3) . . ? N5 C17 C5 111.7(4) . . ? N13 C17 C5 113.4(4) . . ? N5 C17 C47 102.9(3) . . ? N13 C17 C47 102.6(3) . . ? C5 C17 C47 112.6(4) . . ? N6 C18 N2 113.6(3) . . ? N6 C18 C16 112.9(4) . . ? N2 C18 C16 112.0(4) . . ? N6 C18 C13 103.1(4) . . ? N2 C18 C13 102.5(3) . . ? C16 C18 C13 111.9(4) . . ? N13 C19 N2 113.6(4) . . ? N13 C19 H19A 108.8 . . ? N2 C19 H19A 108.8 . . ? N13 C19 H19B 108.8 . . ? N2 C19 H19B 108.8 . . ? H19A C19 H19B 107.7 . . ? C43 C20 C23 111.0(3) . . ? C43 C20 H20A 109.4 . . ? C23 C20 H20A 109.4 . . ? C43 C20 H20B 109.4 . . ? C23 C20 H20B 109.4 . . ? H20A C20 H20B 108.0 . . ? N12 C21 N1 114.9(3) . . ? N12 C21 H21A 108.6 . . ? N1 C21 H21A 108.6 . . ? N12 C21 H21B 108.6 . . ? N1 C21 H21B 108.6 . . ? H21A C21 H21B 107.5 . . ? C28 C22 C9 110.3(4) . . ? C28 C22 H22A 109.6 . . ? C9 C22 H22A 109.6 . . ? C28 C22 H22B 109.6 . . ? C9 C22 H22B 109.6 . . ? H22A C22 H22B 108.1 . . ? C20 C23 C45 112.8(4) . . ? C20 C23 H23A 109.0 . . ? C45 C23 H23A 109.0 . . ? C20 C23 H23B 109.0 . . ? C45 C23 H23B 109.0 . . ? H23A C23 H23B 107.8 . . ? O6 C24 N14 126.5(4) . . ? O6 C24 N13 124.4(4) . . ? N14 C24 N13 109.2(4) . . ? O8 C25 N2 125.4(4) . . ? O8 C25 N4 126.0(4) . . ? N2 C25 N4 108.6(4) . . ? C35 C26 C9 112.4(4) . . ? C35 C26 H26A 109.1 . . ? C9 C26 H26A 109.1 . . ? C35 C26 H26B 109.1 . . ? C9 C26 H26B 109.1 . . ? H26A C26 H26B 107.9 . . ? O7 C27 N12 125.7(4) . . ? O7 C27 N17 125.7(4) . . ? N12 C27 N17 108.6(4) . . ? N18 C28 N16 112.5(3) . . ? N18 C28 C22 112.8(3) . . ? N16 C28 C22 112.6(3) . . ? N18 C28 C50 102.8(3) . . ? N16 C28 C50 103.1(3) . . ? C22 C28 C50 112.2(3) . . ? C47 C29 C15 110.7(4) . . ? C47 C29 H29A 109.5 . . ? C15 C29 H29A 109.5 . . ? C47 C29 H29B 109.5 . . ? C15 C29 H29B 109.5 . . ? H29A C29 H29B 108.1 . . ? C46 C30 C37 110.8(4) . . ? C46 C30 H30A 109.5 . . ? C37 C30 H30A 109.5 . . ? C46 C30 H30B 109.5 . . ? C37 C30 H30B 109.5 . . ? H30A C30 H30B 108.1 . . ? O3 C31 N5 126.1(4) . . ? O3 C31 N15 125.9(4) . . ? N5 C31 N15 107.9(4) . . ? O9 C32 N16 124.3(4) . . ? O9 C32 N19 125.8(4) . . ? N16 C32 N19 109.8(4) . . ? N11 C33 N20 114.3(3) . . ? N11 C33 H33A 108.7 . . ? N20 C33 H33A 108.7 . . ? N11 C33 H33B 108.7 . . ? N20 C33 H33B 108.7 . . ? H33A C33 H33B 107.6 . . ? O2 C34 N3 125.2(5) . . ? O2 C34 N6 126.0(4) . . ? N3 C34 N6 108.8(4) . . ? C26 C35 C50 111.5(4) . . ? C26 C35 H35A 109.3 . . ? C50 C35 H35A 109.3 . . ? C26 C35 H35B 109.3 . . ? C50 C35 H35B 109.3 . . ? H35A C35 H35B 108.0 . . ? C49 C36 C45 110.9(3) . . ? C49 C36 H36A 109.5 . . ? C45 C36 H36A 109.5 . . ? C49 C36 H36B 109.5 . . ? C45 C36 H36B 109.5 . . ? H36A C36 H36B 108.1 . . ? C30 C37 C8 113.0(4) . . ? C30 C37 H37A 109.0 . . ? C8 C37 H37A 109.0 . . ? C30 C37 H37B 109.0 . . ? C8 C37 H37B 109.0 . . ? H37A C37 H37B 107.8 . . ? N9 C38 N7 112.9(3) . . ? N9 C38 H38A 109.0 . . ? N7 C38 H38A 109.0 . . ? N9 C38 H38B 109.0 . . ? N7 C38 H38B 109.0 . . ? H38A C38 H38B 107.8 . . ? O4 C39 N20 125.9(4) . . ? O4 C39 N7 124.6(4) . . ? N20 C39 N7 109.4(4) . . ? O10 C40 N1 125.4(4) . . ? O10 C40 N10 125.3(4) . . ? N1 C40 N10 109.3(4) . . ? O1 C41 N8 125.3(4) . . ? O1 C41 N9 126.5(4) . . ? N8 C41 N9 108.2(4) . . ? O5 C42 N11 125.3(4) . . ? O5 C42 N18 125.1(4) . . ? N11 C42 N18 109.6(3) . . ? N7 C43 N1 112.3(3) . . ? N7 C43 C20 113.7(3) . . ? N1 C43 C20 112.1(3) . . ? N7 C43 C49 102.5(3) . . ? N1 C43 C49 102.5(3) . . ? C20 C43 C49 112.7(3) . . ? N15 C44 N18 114.0(3) . . ? N15 C44 H44A 108.7 . . ? N18 C44 H44A 108.7 . . ? N15 C44 H44B 108.7 . . ? N18 C44 H44B 108.7 . . ? H44A C44 H44B 107.6 . . ? C36 C45 C23 113.1(4) . . ? C36 C45 H45A 109.0 . . ? C23 C45 H45A 109.0 . . ? C36 C45 H45B 109.0 . . ? C23 C45 H45B 109.0 . . ? H45A C45 H45B 107.8 . . ? N9 C46 N12 113.2(3) . . ? N9 C46 C30 112.6(4) . . ? N12 C46 C30 112.6(3) . . ? N9 C46 C12 102.9(3) . . ? N12 C46 C12 102.5(3) . . ? C30 C46 C12 112.3(3) . . ? N14 C47 N15 113.2(3) . . ? N14 C47 C29 112.5(4) . . ? N15 C47 C29 112.4(3) . . ? N14 C47 C17 103.1(3) . . ? N15 C47 C17 102.7(3) . . ? C29 C47 C17 112.1(3) . . ? N10 C48 N19 112.6(3) . . ? N10 C48 H48A 109.1 . . ? N19 C48 H48A 109.1 . . ? N10 C48 H48B 109.1 . . ? N19 C48 H48B 109.1 . . ? H48A C48 H48B 107.8 . . ? N10 C49 N20 112.7(3) . . ? N10 C49 C36 111.9(3) . . ? N20 C49 C36 112.5(3) . . ? N10 C49 C43 103.6(3) . . ? N20 C49 C43 102.9(3) . . ? C36 C49 C43 112.4(3) . . ? N11 C50 N19 112.3(3) . . ? N11 C50 C35 112.0(3) . . ? N19 C50 C35 113.5(3) . . ? N11 C50 C28 103.2(3) . . ? N19 C50 C28 102.7(3) . . ? C35 C50 C28 112.4(3) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.705 _refine_diff_density_min -1.621 _refine_diff_density_rms 0.132 # Attachment '- Ce.cif' data_p_Ce _database_code_depnum_ccdc_archive 'CCDC 892021' #TrackingRef '- Ce.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H103 Ce Cl2 N21 O34.50' _chemical_formula_weight 1761.55 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Fdd2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 35.869(15) _cell_length_b 55.15(2) _cell_length_c 16.021(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 31691(21) _cell_formula_units_Z 16 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 5438 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 21.33 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.477 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 14688 _exptl_absorpt_coefficient_mu 0.739 _exptl_absorpt_correction_type 'multi scan' _exptl_absorpt_correction_T_min 0.7717 _exptl_absorpt_correction_T_max 0.8603 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 58601 _diffrn_reflns_av_R_equivalents 0.2460 _diffrn_reflns_av_sigmaI/netI 0.1538 _diffrn_reflns_limit_h_min -42 _diffrn_reflns_limit_h_max 42 _diffrn_reflns_limit_k_min -64 _diffrn_reflns_limit_k_max 65 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.35 _diffrn_reflns_theta_max 25.20 _reflns_number_total 12768 _reflns_number_gt 8819 _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. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.009 0.000 0.069 12717 6735 ' ' 2 -0.028 0.152 0.557 45 17 ' ' 3 0.028 0.348 0.057 45 14 ' ' 4 -0.028 0.652 0.057 45 17 ' ' 5 0.028 0.848 0.557 45 14 ' ' 6 0.222 0.098 0.807 45 23 ' ' 7 0.222 0.598 0.307 45 23 ' ' 8 0.278 0.402 0.807 45 25 ' ' 9 0.278 0.902 0.307 45 25 ' ' 10 0.472 0.152 0.057 45 17 ' ' 11 0.472 0.652 0.557 45 17 ' ' 12 0.528 0.348 0.557 45 14 ' ' 13 0.528 0.848 0.057 45 14 ' ' 14 0.722 0.098 0.307 45 23 ' ' 15 0.722 0.598 0.807 45 23 ' ' 16 0.778 0.402 0.307 45 25 ' ' 17 0.778 0.902 0.807 45 25 ' ' _platon_squeeze_details ; ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1090P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(6) _refine_ls_number_reflns 12768 _refine_ls_number_parameters 740 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.1090 _refine_ls_R_factor_gt 0.0793 _refine_ls_wR_factor_ref 0.2014 _refine_ls_wR_factor_gt 0.1874 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.143 _refine_ls_shift/su_mean 0.011 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 Ce1 Ce 0.366793(6) 0.091838(4) 0.92206(2) 0.04358(6) Uani 1 1 d . . . Cl1 Cl 0.37445(8) 0.12446(6) 1.0255(3) 0.1603(13) Uani 1 1 d . . . Cl2 Cl 0.31830(8) 0.06937(5) 0.8432(2) 0.1529(12) Uani 1 1 d . . . O2 O 0.11465(8) 0.08576(7) 0.8913(2) 0.0617(12) Uani 1 1 d . . . O1 O 0.16572(9) 0.13035(6) 0.6177(2) 0.0551(10) Uani 1 1 d . . . O3 O 0.12985(8) 0.08246(7) 0.6987(3) 0.0611(12) Uani 1 1 d . . . O4 O 0.17700(8) 0.16408(6) 0.7571(2) 0.0504(10) Uani 1 1 d . . . O5 O 0.14498(8) 0.13625(6) 0.9336(2) 0.0519(9) Uani 1 1 d . . . O6 O 0.31320(8) 0.08325(6) 0.6801(3) 0.0582(10) Uani 1 1 d . . . O9 O 0.27968(8) 0.03386(6) 0.7357(3) 0.0598(11) Uani 1 1 d . . . O7 O 0.30213(8) 0.09914(6) 0.9809(3) 0.0536(10) Uani 1 1 d . . . O8 O 0.33111(8) 0.12392(6) 0.8364(2) 0.0562(10) Uani 1 1 d . . . O10 O 0.27030(8) 0.04367(5) 0.9298(3) 0.0562(10) Uani 1 1 d . . . O1W O 0.35321(10) 0.06765(8) 1.0506(3) 0.0977(15) Uani 1 1 d . . . O2W O 0.38827(11) 0.08322(10) 0.7722(3) 0.0949(15) Uani 1 1 d . . . O3W O 0.39123(15) 0.04768(9) 0.9052(5) 0.148(2) Uani 1 1 d . . . N1 N 0.24315(11) 0.09823(9) 1.0399(3) 0.0588(13) Uani 1 1 d . . . N2 N 0.15793(11) 0.07516(10) 0.9938(3) 0.0676(15) Uani 1 1 d . . . N3 N 0.26808(10) 0.13443(7) 1.0001(3) 0.0454(11) Uani 1 1 d . . . N4 N 0.20391(10) 0.10049(7) 0.5672(3) 0.0508(11) Uani 1 1 d . . . N5 N 0.18061(10) 0.11523(8) 1.0307(3) 0.0497(11) Uani 1 1 d . . . N6 N 0.26594(10) 0.08256(7) 0.5829(3) 0.0452(11) Uani 1 1 d . . . N7 N 0.21997(10) 0.05907(8) 1.0060(3) 0.0540(13) Uani 1 1 d . . . N8 N 0.15529(10) 0.04522(6) 0.7371(3) 0.0421(11) Uani 1 1 d . . . N9 N 0.28555(10) 0.11740(8) 0.6274(3) 0.0517(12) Uani 1 1 d . . . N10 N 0.22679(10) 0.16656(7) 0.8446(3) 0.0470(11) Uani 1 1 d . . . N11 N 0.29745(9) 0.14563(6) 0.7431(3) 0.0479(12) Uani 1 1 d . . . N12 N 0.17638(11) 0.06472(7) 0.6229(3) 0.0531(12) Uani 1 1 d . . . N13 N 0.21020(10) 0.03177(7) 0.9027(3) 0.0514(12) Uani 1 1 d . . . N14 N 0.23708(11) 0.04451(8) 0.6357(3) 0.0588(13) Uani 1 1 d . . . N15 N 0.22840(10) 0.13736(7) 0.5909(3) 0.0452(11) Uani 1 1 d . . . N16 N 0.20421(10) 0.14703(8) 0.9704(3) 0.0478(11) Uani 1 1 d . . . N17 N 0.21701(10) 0.02704(7) 0.7536(3) 0.0471(12) Uani 1 1 d . . . N18 N 0.29166(10) 0.15400(7) 0.8775(3) 0.0480(12) Uani 1 1 d . . . N19 N 0.23713(9) 0.16564(7) 0.7087(3) 0.0394(10) Uani 1 1 d . . . N20 N 0.14835(10) 0.04972(6) 0.8830(3) 0.0505(12) Uani 1 1 d . . . C1 C 0.17631(13) 0.08438(9) 0.5588(4) 0.0531(15) Uani 1 1 d . . . C2 C 0.27545(11) 0.16841(8) 0.7429(3) 0.0365(11) Uani 1 1 d . . . C3 C 0.20241(18) 0.00114(10) 0.5504(6) 0.107(2) Uani 1 1 d . . . H3A H 0.1935 -0.0082 0.5030 0.128 Uiso 1 1 calc R . . H3B H 0.2294 0.0018 0.5470 0.128 Uiso 1 1 calc R . . C4 C 0.21572(19) 0.11758(13) 1.0724(4) 0.0792(12) Uani 1 1 d . . . C5 C 0.17523(14) 0.13348(10) 0.9767(3) 0.0505(15) Uani 1 1 d . . . C6 C 0.32795(17) 0.19729(12) 0.7629(5) 0.083(2) Uani 1 1 d . . . H6A H 0.3527 0.1972 0.7458 0.100 Uiso 1 1 calc R . . C7 C 0.17115(17) 0.04317(11) 1.1021(4) 0.0764(19) Uani 1 1 d . . . H7A H 0.1804 0.0539 1.1454 0.092 Uiso 1 1 calc R . . H7B H 0.1443 0.0419 1.1083 0.092 Uiso 1 1 calc R . . C8 C 0.15569(15) 0.01359(10) 0.9677(4) 0.0731(18) Uani 1 1 d . . . H8A H 0.1520 0.0028 0.9206 0.088 Uiso 1 1 calc R . . H8B H 0.1314 0.0174 0.9907 0.088 Uiso 1 1 calc R . . C9 C 0.18668(19) 0.02769(11) 0.5435(5) 0.082(2) Uani 1 1 d . . . H9A H 0.1968 0.0355 0.4943 0.098 Uiso 1 1 calc R . . H9B H 0.1598 0.0272 0.5379 0.098 Uiso 1 1 calc R . . C10 C 0.26281(13) 0.05631(10) 0.5799(4) 0.0527(14) Uani 1 1 d . . . H10A H 0.2560 0.0519 0.5234 0.063 Uiso 1 1 calc R . . H10B H 0.2874 0.0496 0.5903 0.063 Uiso 1 1 calc R . . C11 C 0.18271(12) 0.02917(8) 0.7001(4) 0.0534(16) Uani 1 1 d . . . C12 C 0.18809(19) 0.01918(12) 1.1113(4) 0.083(2) Uani 1 1 d . . . H12A H 0.1796 0.0123 1.1636 0.099 Uiso 1 1 calc R . . H12B H 0.2149 0.0213 1.1154 0.099 Uiso 1 1 calc R . . C13 C 0.23672(12) 0.04526(9) 0.9438(3) 0.0530(15) Uani 1 1 d . . . C14 C 0.25965(13) 0.12526(9) 0.5612(3) 0.0435(13) Uani 1 1 d . . . C15 C 0.1923(2) -0.01104(14) 0.6245(6) 0.094(2) Uani 1 1 d . . . H15A H 0.2145 -0.0150 0.6561 0.113 Uiso 1 1 calc R . . H15B H 0.1797 -0.0261 0.6106 0.113 Uiso 1 1 calc R . . C16 C 0.29581(12) 0.19021(9) 0.7062(4) 0.0549(15) Uani 1 1 d . . . H16A H 0.3052 0.1862 0.6512 0.066 Uiso 1 1 calc R . . H16B H 0.2787 0.2037 0.7007 0.066 Uiso 1 1 calc R . . C17 C 0.17290(12) 0.03595(9) 0.9381(4) 0.0603(17) Uani 1 1 d . . . C18 C 0.15235(14) 0.09691(10) 1.0467(4) 0.0582(16) Uani 1 1 d . . . H18A H 0.1279 0.1037 1.0356 0.070 Uiso 1 1 calc R . . H18B H 0.1533 0.0922 1.1050 0.070 Uiso 1 1 calc R . . C19 C 0.27694(14) 0.19804(9) 0.8641(5) 0.0700(19) Uani 1 1 d . . . H19A H 0.2609 0.2090 0.8333 0.084 Uiso 1 1 calc R . . H19B H 0.2717 0.2000 0.9231 0.084 Uiso 1 1 calc R . . C20 C 0.18094(14) 0.05435(11) 1.0115(4) 0.0665(18) Uani 1 1 d . . . C21 C 0.29538(13) 0.14997(10) 0.9621(3) 0.0504(14) Uani 1 1 d . . . H21A H 0.2946 0.1655 0.9902 0.060 Uiso 1 1 calc R . . H21B H 0.3198 0.1430 0.9720 0.060 Uiso 1 1 calc R . . C22 C 0.28943(11) 0.09438(9) 0.6356(3) 0.0441(13) Uani 1 1 d . . . C23 C 0.27377(12) 0.10992(9) 1.0041(3) 0.0454(13) Uani 1 1 d . . . C24 C 0.13235(12) 0.04156(9) 0.8056(4) 0.0508(15) Uani 1 1 d . . . H24A H 0.1268 0.0244 0.8101 0.061 Uiso 1 1 calc R . . H24B H 0.1090 0.0500 0.7965 0.061 Uiso 1 1 calc R . . C25 C 0.20555(12) 0.16939(9) 0.9183(4) 0.0605(15) Uani 1 1 d . . . H25A H 0.1803 0.1740 0.9032 0.073 Uiso 1 1 calc R . . H25B H 0.2161 0.1825 0.9511 0.073 Uiso 1 1 calc R . . C26 C 0.27850(15) 0.13727(11) 0.4879(4) 0.0657(18) Uani 1 1 d . . . H26A H 0.2924 0.1512 0.5081 0.079 Uiso 1 1 calc R . . H26B H 0.2595 0.1432 0.4502 0.079 Uiso 1 1 calc R . . C27 C 0.22977(13) 0.16238(8) 0.6213(3) 0.0441(13) Uani 1 1 d . . . H27A H 0.2489 0.1709 0.5902 0.053 Uiso 1 1 calc R . . H27B H 0.2061 0.1700 0.6086 0.053 Uiso 1 1 calc R . . C28 C 0.19714(12) 0.12422(8) 0.5950(3) 0.0428(13) Uani 1 1 d . . . C29 C 0.31623(17) 0.20435(10) 0.8479(5) 0.086(2) Uani 1 1 d . . . H29A H 0.3195 0.2217 0.8547 0.103 Uiso 1 1 calc R . . H29B H 0.3320 0.1962 0.8884 0.103 Uiso 1 1 calc R . . C30 C 0.19679(11) 0.04171(9) 0.6183(4) 0.0487(14) Uani 1 1 d . . . C31 C 0.21047(10) 0.16533(8) 0.7700(3) 0.0368(12) Uani 1 1 d . . . C32 C 0.30971(11) 0.14009(8) 0.8218(4) 0.0439(13) Uani 1 1 d . . . C33 C 0.15209(12) 0.06591(9) 0.6869(4) 0.0635(16) Uani 1 1 d . . . C34 C 0.16673(13) 0.00465(9) 0.6774(5) 0.074(2) Uani 1 1 d . . . H34A H 0.1436 0.0071 0.6473 0.088 Uiso 1 1 calc R . . H34B H 0.1609 -0.0040 0.7284 0.088 Uiso 1 1 calc R . . C35 C 0.24805(12) 0.03509(8) 0.7092(3) 0.0415(13) Uani 1 1 d . . . C36 C 0.13743(11) 0.07081(9) 0.9221(5) 0.0567(14) Uani 1 1 d . . . C37 C 0.31229(11) 0.13434(9) 0.6650(4) 0.0526(14) Uani 1 1 d . . . H37A H 0.3181 0.1470 0.6250 0.063 Uiso 1 1 calc R . . H37B H 0.3352 0.1258 0.6777 0.063 Uiso 1 1 calc R . . C47 C 0.2425(2) 0.09915(14) 0.5358(4) 0.0822(13) Uani 1 1 d . . . C46 C 0.21449(19) 0.11942(13) 1.1647(4) 0.0792(12) Uani 1 1 d . . . H46A H 0.2043 0.1045 1.1870 0.095 Uiso 1 1 calc R . . H46B H 0.2398 0.1210 1.1855 0.095 Uiso 1 1 calc R . . C45 C 0.21990(13) 0.01702(9) 0.8305(4) 0.0551(16) Uani 1 1 d . . . H45A H 0.2454 0.0116 0.8376 0.066 Uiso 1 1 calc R . . H45B H 0.2043 0.0027 0.8316 0.066 Uiso 1 1 calc R . . C44 C 0.23256(18) 0.14134(12) 1.0348(4) 0.0777(12) Uani 1 1 d . . . C43 C 0.24187(13) 0.07401(9) 1.0614(3) 0.0501(13) Uani 1 1 d U . . H43A H 0.2317 0.0726 1.1174 0.060 Uiso 1 1 calc R . . H43B H 0.2671 0.0677 1.0628 0.060 Uiso 1 1 calc R . . C42 C 0.23598(19) 0.16081(12) 1.1001(4) 0.0777(12) Uani 1 1 d . . . H42A H 0.2557 0.1566 1.1388 0.093 Uiso 1 1 calc R . . H42B H 0.2426 0.1760 1.0735 0.093 Uiso 1 1 calc R . . C41 C 0.28364(19) 0.09740(13) 0.4101(5) 0.0822(13) Uani 1 1 d . . . H41A H 0.2826 0.0972 0.3496 0.099 Uiso 1 1 calc R . . H41B H 0.2977 0.0833 0.4278 0.099 Uiso 1 1 calc R . . C40 C 0.26827(13) 0.17193(8) 0.8384(4) 0.0588(16) Uani 1 1 d . . . C39 C 0.17965(17) -0.00034(15) 1.0373(5) 0.093(3) Uani 1 1 d . . . H39A H 0.2028 -0.0063 1.0136 0.111 Uiso 1 1 calc R . . H39B H 0.1658 -0.0140 1.0591 0.111 Uiso 1 1 calc R . . C38 C 0.2463(2) 0.09583(14) 0.4429(4) 0.0822(13) Uani 1 1 d . . . H38A H 0.2361 0.0801 0.4283 0.099 Uiso 1 1 calc R . . H38B H 0.2311 0.1080 0.4154 0.099 Uiso 1 1 calc R . . C48 C 0.3047(2) 0.12105(15) 0.4397(5) 0.090(3) Uani 1 1 d . . . H48A H 0.3256 0.1166 0.4747 0.108 Uiso 1 1 calc R . . H48B H 0.3142 0.1297 0.3915 0.108 Uiso 1 1 calc R . . C49 C 0.20130(18) 0.16377(12) 1.1455(4) 0.0777(12) Uani 1 1 d . . . H49A H 0.1811 0.1672 1.1071 0.093 Uiso 1 1 calc R . . H49B H 0.2034 0.1772 1.1845 0.093 Uiso 1 1 calc R . . C50 C 0.1931(2) 0.13904(13) 1.1951(4) 0.0792(12) Uani 1 1 d . . . H50A H 0.1986 0.1414 1.2538 0.095 Uiso 1 1 calc R . . H50B H 0.1669 0.1351 1.1901 0.095 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ce1 0.03525(9) 0.03925(11) 0.05623(15) -0.00559(13) -0.01592(11) 0.00094(10) Cl1 0.1446(18) 0.135(2) 0.201(3) -0.005(2) -0.054(2) -0.0041(17) Cl2 0.1476(18) 0.153(2) 0.158(3) -0.005(2) -0.0232(18) -0.0483(16) O2 0.0483(16) 0.083(2) 0.054(3) 0.016(2) -0.0101(15) 0.0157(16) O1 0.0511(16) 0.0451(18) 0.069(3) -0.0046(18) -0.0087(17) 0.0056(15) O3 0.0491(15) 0.0500(19) 0.084(3) 0.006(2) -0.0048(17) 0.0183(14) O4 0.0474(15) 0.0566(18) 0.047(2) -0.0034(17) -0.0103(15) 0.0117(14) O5 0.0514(15) 0.0664(19) 0.038(2) 0.0053(18) -0.0068(16) 0.0005(14) O6 0.0586(16) 0.0499(17) 0.066(2) -0.006(2) -0.0215(18) 0.0039(15) O9 0.0413(14) 0.0472(18) 0.091(3) -0.0159(19) -0.0203(17) 0.0055(13) O7 0.0415(14) 0.0447(17) 0.075(3) -0.0080(18) -0.0132(16) 0.0023(14) O8 0.0436(15) 0.066(2) 0.059(2) 0.0036(19) -0.0135(16) 0.0152(15) O10 0.0462(14) 0.0440(16) 0.078(3) -0.009(2) -0.0019(18) -0.0030(13) O1W 0.0540(18) 0.096(2) 0.143(4) 0.082(2) -0.019(2) -0.0082(19) O2W 0.064(2) 0.134(3) 0.086(3) -0.067(3) 0.017(2) -0.016(2) O3W 0.147(3) 0.097(3) 0.199(6) -0.068(3) -0.101(4) 0.067(3) N1 0.051(2) 0.083(3) 0.043(3) 0.001(2) -0.0086(19) 0.023(2) N2 0.055(2) 0.113(4) 0.035(3) 0.017(3) -0.001(2) 0.011(2) N3 0.0468(18) 0.057(2) 0.033(2) -0.0043(19) -0.0088(17) 0.0114(17) N4 0.057(2) 0.052(2) 0.043(3) -0.0180(19) -0.0217(19) 0.0228(18) N5 0.0567(19) 0.066(2) 0.027(2) -0.0053(19) -0.0160(17) 0.0238(18) N6 0.0525(18) 0.044(2) 0.040(2) -0.0073(19) -0.0151(18) 0.0144(17) N7 0.0370(16) 0.074(3) 0.051(3) 0.012(2) 0.0014(18) 0.0032(18) N8 0.0554(19) 0.0322(18) 0.039(2) 0.0050(17) -0.0047(18) 0.0020(16) N9 0.0470(18) 0.059(2) 0.050(3) -0.012(2) -0.0123(18) -0.0041(18) N10 0.0456(17) 0.0356(19) 0.060(3) -0.009(2) -0.0116(19) 0.0041(16) N11 0.0421(16) 0.0306(18) 0.071(3) 0.0160(19) -0.0180(19) 0.0096(15) N12 0.059(2) 0.044(2) 0.056(3) 0.002(2) -0.011(2) 0.0031(18) N13 0.0443(17) 0.044(2) 0.066(3) 0.013(2) -0.0144(19) 0.0082(16) N14 0.0475(18) 0.054(2) 0.075(3) -0.018(2) 0.000(2) 0.0047(18) N15 0.0402(17) 0.046(2) 0.049(3) 0.0119(19) -0.0047(17) 0.0025(16) N16 0.0510(18) 0.065(2) 0.027(2) -0.0079(19) -0.0176(17) 0.0124(19) N17 0.0526(19) 0.0302(18) 0.059(3) -0.0011(19) -0.0126(19) 0.0000(16) N18 0.0432(17) 0.0367(19) 0.064(3) -0.0053(19) -0.0218(19) 0.0014(16) N19 0.0346(15) 0.0395(18) 0.044(2) 0.0101(17) -0.0137(15) 0.0024(15) N20 0.0486(18) 0.0328(19) 0.070(3) 0.0134(19) -0.0118(19) 0.0099(16) C1 0.050(2) 0.052(3) 0.057(4) 0.005(3) -0.016(2) -0.020(2) C2 0.0429(18) 0.038(2) 0.028(2) -0.0044(19) -0.0211(18) 0.0113(17) C3 0.085(4) 0.060(3) 0.175(7) -0.080(4) -0.041(4) 0.034(3) C4 0.096(2) 0.095(3) 0.047(2) -0.010(2) 0.009(2) 0.002(2) C5 0.055(2) 0.062(3) 0.034(3) -0.010(2) -0.006(2) -0.002(2) C6 0.070(3) 0.084(4) 0.095(5) 0.012(4) -0.001(4) -0.027(3) C7 0.074(3) 0.074(3) 0.082(4) 0.041(3) -0.001(3) -0.022(3) C8 0.059(3) 0.066(3) 0.094(4) 0.043(3) -0.022(3) 0.004(3) C9 0.089(4) 0.067(4) 0.090(5) -0.017(4) -0.024(4) 0.025(3) C10 0.053(2) 0.064(3) 0.041(3) -0.012(2) -0.018(2) 0.019(2) C11 0.050(2) 0.041(2) 0.069(4) -0.002(2) -0.025(2) 0.001(2) C12 0.086(4) 0.098(4) 0.065(4) 0.048(3) -0.004(3) -0.018(3) C13 0.043(2) 0.060(3) 0.056(4) 0.019(3) -0.001(2) -0.003(2) C14 0.045(2) 0.050(2) 0.035(3) -0.005(2) -0.0147(19) 0.0093(19) C15 0.103(4) 0.074(4) 0.106(6) 0.013(4) -0.002(4) 0.031(4) C16 0.041(2) 0.050(3) 0.074(4) 0.027(3) -0.017(2) -0.006(2) C17 0.038(2) 0.058(3) 0.085(5) 0.016(3) 0.010(2) -0.0101(19) C18 0.046(2) 0.076(3) 0.053(4) -0.017(3) 0.003(2) 0.005(2) C19 0.063(3) 0.032(2) 0.115(5) -0.006(3) -0.046(3) 0.006(2) C20 0.052(2) 0.080(4) 0.068(4) 0.007(3) 0.022(3) 0.007(3) C21 0.056(2) 0.052(3) 0.044(3) -0.004(2) -0.025(2) 0.003(2) C22 0.0305(17) 0.068(3) 0.033(3) 0.006(2) -0.0050(19) 0.0126(19) C23 0.048(2) 0.051(3) 0.037(3) -0.005(2) -0.010(2) 0.017(2) C24 0.040(2) 0.045(3) 0.067(4) -0.002(3) -0.010(2) 0.0030(19) C25 0.051(2) 0.052(2) 0.078(4) -0.040(3) -0.004(3) 0.018(2) C26 0.054(3) 0.059(3) 0.084(5) 0.000(3) 0.017(3) 0.006(2) C27 0.045(2) 0.035(2) 0.053(3) 0.018(2) 0.002(2) 0.0106(19) C28 0.054(2) 0.039(2) 0.035(3) -0.002(2) -0.019(2) 0.009(2) C29 0.081(3) 0.040(3) 0.138(7) 0.003(4) -0.039(4) -0.020(3) C30 0.0322(18) 0.058(3) 0.056(3) -0.013(3) -0.014(2) -0.002(2) C31 0.0344(18) 0.034(2) 0.042(3) -0.005(2) -0.0142(19) -0.0006(17) C32 0.0306(18) 0.034(2) 0.067(3) -0.014(2) -0.012(2) 0.0056(17) C33 0.040(2) 0.057(3) 0.093(4) -0.042(3) -0.016(2) -0.010(2) C34 0.053(2) 0.045(3) 0.123(5) -0.011(4) -0.020(3) -0.003(2) C35 0.044(2) 0.031(2) 0.050(3) -0.003(2) -0.014(2) 0.0024(18) C36 0.0330(18) 0.071(3) 0.066(3) 0.023(4) -0.001(2) -0.006(2) C37 0.0362(18) 0.054(3) 0.067(4) -0.021(3) 0.006(2) 0.0068(18) C47 0.105(2) 0.103(3) 0.038(2) 0.001(2) 0.005(2) 0.014(2) C46 0.096(2) 0.095(3) 0.047(2) -0.010(2) 0.009(2) 0.002(2) C45 0.046(2) 0.041(3) 0.078(4) 0.005(3) -0.011(3) 0.005(2) C44 0.092(2) 0.075(2) 0.066(3) -0.0207(19) -0.0254(19) 0.0254(18) C43 0.0487(19) 0.056(2) 0.045(2) -0.0038(19) 0.0020(18) -0.0073(18) C42 0.092(2) 0.075(2) 0.066(3) -0.0207(19) -0.0254(19) 0.0254(18) C41 0.105(2) 0.103(3) 0.038(2) 0.001(2) 0.005(2) 0.014(2) C40 0.050(2) 0.031(2) 0.095(4) -0.010(3) -0.035(3) 0.0062(19) C39 0.057(3) 0.130(6) 0.091(5) 0.037(5) 0.001(3) 0.001(4) C38 0.105(2) 0.103(3) 0.038(2) 0.001(2) 0.005(2) 0.014(2) C48 0.091(4) 0.121(6) 0.058(5) 0.013(4) -0.002(4) -0.009(4) C49 0.092(2) 0.075(2) 0.066(3) -0.0207(19) -0.0254(19) 0.0254(18) C50 0.096(2) 0.095(3) 0.047(2) -0.010(2) 0.009(2) 0.002(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 Ce1 Cl1 2.462(4) . ? Ce1 Cl2 2.482(3) . ? Ce1 O1 2.488(3) 3 ? Ce1 O1W 2.501(5) . ? Ce1 O7 2.536(3) . ? Ce1 O2W 2.565(5) . ? Ce1 O4 2.575(3) 3 ? Ce1 O8 2.579(3) . ? Ce1 O3W 2.602(5) . ? O2 C36 1.261(6) . ? O1 C28 1.231(6) . ? O1 Ce1 2.488(3) 11_454 ? O3 C33 1.227(6) . ? O4 C31 1.220(5) . ? O4 Ce1 2.575(3) 11_454 ? O5 C5 1.295(6) . ? O6 C22 1.270(6) . ? O9 C35 1.213(5) . ? O7 C23 1.235(5) . ? O8 C32 1.200(5) . ? O10 C13 1.228(5) . ? N1 C43 1.381(7) . ? N1 C23 1.397(6) . ? N1 C4 1.543(8) . ? N2 C36 1.386(8) . ? N2 C20 1.442(8) . ? N2 C18 1.482(8) . ? N3 C23 1.369(6) . ? N3 C21 1.437(6) . ? N3 C44 1.441(8) . ? N4 C1 1.337(6) . ? N4 C28 1.404(6) . ? N4 C47 1.474(8) . ? N5 C5 1.341(7) . ? N5 C4 1.432(8) . ? N5 C18 1.454(7) . ? N6 C22 1.360(6) . ? N6 C47 1.454(8) . ? N6 C10 1.453(7) . ? N7 C13 1.392(7) . ? N7 C20 1.427(6) . ? N7 C43 1.444(7) . ? N8 C24 1.387(7) . ? N8 C33 1.400(7) . ? N8 C11 1.450(6) . ? N9 C22 1.283(6) . ? N9 C37 1.468(6) . ? N9 C14 1.475(6) . ? N10 C31 1.333(6) . ? N10 C25 1.413(7) . ? N10 C40 1.520(6) . ? N11 C32 1.370(7) . ? N11 C2 1.484(5) . ? N11 C37 1.496(7) . ? N12 C33 1.348(7) . ? N12 C30 1.467(6) . ? N12 C1 1.493(7) . ? N13 C13 1.376(6) . ? N13 C45 1.456(7) . ? N13 C17 1.471(6) . ? N14 C35 1.345(7) . ? N14 C10 1.441(7) . ? N14 C30 1.480(6) . ? N15 C28 1.337(6) . ? N15 C14 1.389(6) . ? N15 C27 1.464(6) . ? N16 C5 1.284(6) . ? N16 C44 1.482(8) . ? N16 C25 1.490(7) . ? N17 C45 1.355(8) . ? N17 C35 1.394(6) . ? N17 C11 1.504(6) . ? N18 C32 1.343(6) . ? N18 C21 1.379(7) . ? N18 C40 1.440(6) . ? N19 C31 1.371(6) . ? N19 C27 1.435(7) . ? N19 C2 1.488(5) . ? N20 C36 1.378(7) . ? N20 C24 1.439(7) . ? N20 C17 1.460(7) . ? C2 C16 1.525(7) . ? C2 C40 1.563(8) . ? C3 C15 1.412(12) . ? C3 C9 1.573(8) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C46 1.482(10) . ? C4 C44 1.563(10) . ? C6 C29 1.476(11) . ? C6 C16 1.519(8) . ? C6 H6A 0.9300 . ? C7 C12 1.463(9) . ? C7 C20 1.615(9) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C17 1.458(7) . ? C8 C39 1.603(9) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C30 1.471(9) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C34 1.513(7) . ? C11 C30 1.566(8) . ? C12 C39 1.630(11) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C14 C26 1.508(8) . ? C14 C47 1.618(9) . ? C15 C34 1.518(10) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C20 1.580(9) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C29 1.475(8) . ? C19 C40 1.529(7) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C48 1.509(10) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C47 C38 1.506(9) . ? C46 C50 1.412(10) . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C44 C42 1.503(9) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C42 C49 1.451(9) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C41 C38 1.443(10) . ? C41 C48 1.580(10) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C49 C50 1.605(10) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? 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 Cl1 Ce1 Cl2 141.81(10) . . ? Cl1 Ce1 O1 72.93(12) . 3 ? Cl2 Ce1 O1 128.61(12) . 3 ? Cl1 Ce1 O1W 81.80(15) . . ? Cl2 Ce1 O1W 90.93(13) . . ? O1 Ce1 O1W 138.97(13) 3 . ? Cl1 Ce1 O7 74.67(11) . . ? Cl2 Ce1 O7 68.13(11) . . ? O1 Ce1 O7 132.64(11) 3 . ? O1W Ce1 O7 66.46(12) . . ? Cl1 Ce1 O2W 137.05(14) . . ? Cl2 Ce1 O2W 68.99(12) . . ? O1 Ce1 O2W 64.84(14) 3 . ? O1W Ce1 O2W 136.88(16) . . ? O7 Ce1 O2W 130.68(13) . . ? Cl1 Ce1 O4 69.06(11) . 3 ? Cl2 Ce1 O4 142.59(11) . 3 ? O1 Ce1 O4 70.84(11) 3 3 ? O1W Ce1 O4 70.12(12) . 3 ? O7 Ce1 O4 126.20(12) . 3 ? O2W Ce1 O4 102.71(12) . 3 ? Cl1 Ce1 O8 84.97(12) . . ? Cl2 Ce1 O8 73.96(11) . . ? O1 Ce1 O8 74.98(11) 3 . ? O1W Ce1 O8 135.01(12) . . ? O7 Ce1 O8 68.59(12) . . ? O2W Ce1 O8 77.18(14) . . ? O4 Ce1 O8 141.72(11) 3 . ? Cl1 Ce1 O3W 135.76(16) . . ? Cl2 Ce1 O3W 73.50(14) . . ? O1 Ce1 O3W 107.63(16) 3 . ? O1W Ce1 O3W 69.64(19) . . ? O7 Ce1 O3W 119.70(16) . . ? O2W Ce1 O3W 68.2(2) . . ? O4 Ce1 O3W 69.75(15) 3 . ? O8 Ce1 O3W 138.92(17) . . ? C28 O1 Ce1 156.6(3) . 11_454 ? C31 O4 Ce1 157.2(3) . 11_454 ? C23 O7 Ce1 160.3(3) . . ? C32 O8 Ce1 158.6(4) . . ? C43 N1 C23 125.1(4) . . ? C43 N1 C4 124.3(5) . . ? C23 N1 C4 108.7(5) . . ? C36 N2 C20 109.2(5) . . ? C36 N2 C18 122.9(4) . . ? C20 N2 C18 127.6(5) . . ? C23 N3 C21 120.5(4) . . ? C23 N3 C44 112.0(4) . . ? C21 N3 C44 127.5(4) . . ? C1 N4 C28 121.6(4) . . ? C1 N4 C47 128.9(5) . . ? C28 N4 C47 108.5(4) . . ? C5 N5 C4 111.1(5) . . ? C5 N5 C18 122.3(4) . . ? C4 N5 C18 126.5(5) . . ? C22 N6 C47 112.3(5) . . ? C22 N6 C10 123.1(4) . . ? C47 N6 C10 124.4(5) . . ? C13 N7 C20 111.6(4) . . ? C13 N7 C43 121.2(4) . . ? C20 N7 C43 126.9(5) . . ? C24 N8 C33 121.6(4) . . ? C24 N8 C11 129.6(4) . . ? C33 N8 C11 108.6(4) . . ? C22 N9 C37 121.1(4) . . ? C22 N9 C14 115.6(4) . . ? C37 N9 C14 121.3(4) . . ? C31 N10 C25 121.2(4) . . ? C31 N10 C40 112.4(4) . . ? C25 N10 C40 124.1(4) . . ? C32 N11 C2 111.2(4) . . ? C32 N11 C37 124.3(4) . . ? C2 N11 C37 122.7(4) . . ? C33 N12 C30 113.8(4) . . ? C33 N12 C1 119.1(4) . . ? C30 N12 C1 126.5(4) . . ? C13 N13 C45 121.1(4) . . ? C13 N13 C17 111.1(4) . . ? C45 N13 C17 127.7(4) . . ? C35 N14 C10 122.0(4) . . ? C35 N14 C30 114.2(4) . . ? C10 N14 C30 123.7(4) . . ? C28 N15 C14 115.7(4) . . ? C28 N15 C27 121.5(4) . . ? C14 N15 C27 122.7(4) . . ? C5 N16 C44 112.2(5) . . ? C5 N16 C25 123.5(4) . . ? C44 N16 C25 122.9(4) . . ? C45 N17 C35 122.2(4) . . ? C45 N17 C11 127.8(4) . . ? C35 N17 C11 109.7(4) . . ? C32 N18 C21 120.9(4) . . ? C32 N18 C40 112.6(5) . . ? C21 N18 C40 126.5(4) . . ? C31 N19 C27 124.7(4) . . ? C31 N19 C2 112.4(4) . . ? C27 N19 C2 122.8(4) . . ? C36 N20 C24 122.8(4) . . ? C36 N20 C17 109.7(5) . . ? C24 N20 C17 126.8(4) . . ? N4 C1 N12 114.4(4) . . ? N11 C2 N19 113.9(3) . . ? N11 C2 C16 114.4(3) . . ? N19 C2 C16 112.4(4) . . ? N11 C2 C40 101.0(4) . . ? N19 C2 C40 102.8(3) . . ? C16 C2 C40 111.0(4) . . ? C15 C3 C9 114.1(6) . . ? C15 C3 H3A 108.7 . . ? C9 C3 H3A 108.7 . . ? C15 C3 H3B 108.7 . . ? C9 C3 H3B 108.7 . . ? H3A C3 H3B 107.6 . . ? N5 C4 C46 116.5(6) . . ? N5 C4 N1 109.9(5) . . ? C46 C4 N1 113.8(6) . . ? N5 C4 C44 103.7(5) . . ? C46 C4 C44 109.8(6) . . ? N1 C4 C44 101.7(5) . . ? N16 C5 O5 124.6(5) . . ? N16 C5 N5 111.8(4) . . ? O5 C5 N5 123.6(4) . . ? C29 C6 C16 113.8(5) . . ? C29 C6 H6A 123.1 . . ? C16 C6 H6A 123.1 . . ? C12 C7 C20 110.2(5) . . ? C12 C7 H7A 109.6 . . ? C20 C7 H7A 109.6 . . ? C12 C7 H7B 109.6 . . ? C20 C7 H7B 109.6 . . ? H7A C7 H7B 108.1 . . ? C17 C8 C39 113.9(5) . . ? C17 C8 H8A 108.8 . . ? C39 C8 H8A 108.8 . . ? C17 C8 H8B 108.8 . . ? C39 C8 H8B 108.8 . . ? H8A C8 H8B 107.7 . . ? C30 C9 C3 110.1(6) . . ? C30 C9 H9A 109.6 . . ? C3 C9 H9A 109.6 . . ? C30 C9 H9B 109.6 . . ? C3 C9 H9B 109.6 . . ? H9A C9 H9B 108.1 . . ? N14 C10 N6 118.6(4) . . ? N14 C10 H10A 107.7 . . ? N6 C10 H10A 107.7 . . ? N14 C10 H10B 107.7 . . ? N6 C10 H10B 107.7 . . ? H10A C10 H10B 107.1 . . ? N8 C11 N17 111.7(4) . . ? N8 C11 C34 112.8(4) . . ? N17 C11 C34 112.1(4) . . ? N8 C11 C30 106.9(4) . . ? N17 C11 C30 104.3(4) . . ? C34 C11 C30 108.4(5) . . ? C7 C12 C39 116.5(6) . . ? C7 C12 H12A 108.2 . . ? C39 C12 H12A 108.2 . . ? C7 C12 H12B 108.2 . . ? C39 C12 H12B 108.2 . . ? H12A C12 H12B 107.3 . . ? O10 C13 N13 123.5(5) . . ? O10 C13 N7 126.4(5) . . ? N13 C13 N7 109.9(4) . . ? N15 C14 N9 113.7(4) . . ? N15 C14 C26 114.7(4) . . ? N9 C14 C26 114.0(4) . . ? N15 C14 C47 101.9(4) . . ? N9 C14 C47 99.2(4) . . ? C26 C14 C47 111.5(5) . . ? C3 C15 C34 110.7(6) . . ? C3 C15 H15A 109.5 . . ? C34 C15 H15A 109.5 . . ? C3 C15 H15B 109.5 . . ? C34 C15 H15B 109.5 . . ? H15A C15 H15B 108.1 . . ? C6 C16 C2 109.6(4) . . ? C6 C16 H16A 109.8 . . ? C2 C16 H16A 109.8 . . ? C6 C16 H16B 109.8 . . ? C2 C16 H16B 109.8 . . ? H16A C16 H16B 108.2 . . ? C8 C17 N20 112.4(4) . . ? C8 C17 N13 112.2(4) . . ? N20 C17 N13 113.4(5) . . ? C8 C17 C20 112.2(5) . . ? N20 C17 C20 103.0(4) . . ? N13 C17 C20 102.8(4) . . ? N5 C18 N2 111.6(4) . . ? N5 C18 H18A 109.3 . . ? N2 C18 H18A 109.3 . . ? N5 C18 H18B 109.3 . . ? N2 C18 H18B 109.3 . . ? H18A C18 H18B 108.0 . . ? C29 C19 C40 111.7(5) . . ? C29 C19 H19A 109.3 . . ? C40 C19 H19A 109.3 . . ? C29 C19 H19B 109.3 . . ? C40 C19 H19B 109.3 . . ? H19A C19 H19B 108.0 . . ? N7 C20 N2 113.8(5) . . ? N7 C20 C17 104.5(4) . . ? N2 C20 C17 105.1(5) . . ? N7 C20 C7 109.7(5) . . ? N2 C20 C7 110.8(5) . . ? C17 C20 C7 112.6(5) . . ? N18 C21 N3 116.6(4) . . ? N18 C21 H21A 108.1 . . ? N3 C21 H21A 108.1 . . ? N18 C21 H21B 108.2 . . ? N3 C21 H21B 108.2 . . ? H21A C21 H21B 107.3 . . ? O6 C22 N9 127.5(5) . . ? O6 C22 N6 122.2(4) . . ? N9 C22 N6 110.1(4) . . ? O7 C23 N3 125.7(4) . . ? O7 C23 N1 123.3(4) . . ? N3 C23 N1 111.0(4) . . ? N8 C24 N20 113.6(4) . . ? N8 C24 H24A 108.8 . . ? N20 C24 H24A 108.8 . . ? N8 C24 H24B 108.8 . . ? N20 C24 H24B 108.8 . . ? H24A C24 H24B 107.7 . . ? N10 C25 N16 113.2(4) . . ? N10 C25 H25A 108.9 . . ? N16 C25 H25A 108.9 . . ? N10 C25 H25B 108.9 . . ? N16 C25 H25B 108.9 . . ? H25A C25 H25B 107.7 . . ? C14 C26 C48 114.6(5) . . ? C14 C26 H26A 108.6 . . ? C48 C26 H26A 108.6 . . ? C14 C26 H26B 108.6 . . ? C48 C26 H26B 108.6 . . ? H26A C26 H26B 107.6 . . ? N19 C27 N15 116.7(4) . . ? N19 C27 H27A 108.1 . . ? N15 C27 H27A 108.1 . . ? N19 C27 H27B 108.1 . . ? N15 C27 H27B 108.1 . . ? H27A C27 H27B 107.3 . . ? O1 C28 N15 129.3(4) . . ? O1 C28 N4 120.5(4) . . ? N15 C28 N4 110.2(4) . . ? C6 C29 C19 111.8(6) . . ? C6 C29 H29A 109.2 . . ? C19 C29 H29A 109.2 . . ? C6 C29 H29B 109.2 . . ? C19 C29 H29B 109.2 . . ? H29A C29 H29B 107.9 . . ? N12 C30 C9 111.9(4) . . ? N12 C30 N14 112.8(4) . . ? C9 C30 N14 116.7(5) . . ? N12 C30 C11 100.3(4) . . ? C9 C30 C11 111.7(5) . . ? N14 C30 C11 101.7(4) . . ? O4 C31 N10 125.9(4) . . ? O4 C31 N19 124.5(4) . . ? N10 C31 N19 109.6(3) . . ? O8 C32 N18 127.2(5) . . ? O8 C32 N11 123.4(5) . . ? N18 C32 N11 109.2(4) . . ? O3 C33 N12 125.1(5) . . ? O3 C33 N8 124.8(5) . . ? N12 C33 N8 110.1(4) . . ? C11 C34 C15 114.5(5) . . ? C11 C34 H34A 108.6 . . ? C15 C34 H34A 108.6 . . ? C11 C34 H34B 108.6 . . ? C15 C34 H34B 108.6 . . ? H34A C34 H34B 107.6 . . ? O9 C35 N14 126.9(5) . . ? O9 C35 N17 123.4(5) . . ? N14 C35 N17 109.6(4) . . ? O2 C36 N20 124.0(6) . . ? O2 C36 N2 123.7(5) . . ? N20 C36 N2 111.9(4) . . ? N9 C37 N11 112.1(4) . . ? N9 C37 H37A 109.2 . . ? N11 C37 H37A 109.2 . . ? N9 C37 H37B 109.2 . . ? N11 C37 H37B 109.2 . . ? H37A C37 H37B 107.9 . . ? N6 C47 N4 113.4(5) . . ? N6 C47 C38 112.6(6) . . ? N4 C47 C38 115.4(6) . . ? N6 C47 C14 102.1(5) . . ? N4 C47 C14 103.1(5) . . ? C38 C47 C14 108.8(6) . . ? C50 C46 C4 114.3(6) . . ? C50 C46 H46A 108.7 . . ? C4 C46 H46A 108.7 . . ? C50 C46 H46B 108.7 . . ? C4 C46 H46B 108.7 . . ? H46A C46 H46B 107.6 . . ? N17 C45 N13 118.4(4) . . ? N17 C45 H45A 107.7 . . ? N13 C45 H45A 107.7 . . ? N17 C45 H45B 107.7 . . ? N13 C45 H45B 107.7 . . ? H45A C45 H45B 107.1 . . ? N3 C44 N16 113.2(5) . . ? N3 C44 C42 112.6(5) . . ? N16 C44 C42 112.9(5) . . ? N3 C44 C4 105.6(5) . . ? N16 C44 C4 100.4(5) . . ? C42 C44 C4 111.2(6) . . ? N1 C43 N7 114.6(4) . . ? N1 C43 H43A 108.6 . . ? N7 C43 H43A 108.6 . . ? N1 C43 H43B 108.6 . . ? N7 C43 H43B 108.6 . . ? H43A C43 H43B 107.6 . . ? C49 C42 C44 111.1(6) . . ? C49 C42 H42A 109.4 . . ? C44 C42 H42A 109.4 . . ? C49 C42 H42B 109.4 . . ? C44 C42 H42B 109.4 . . ? H42A C42 H42B 108.0 . . ? C38 C41 C48 112.5(6) . . ? C38 C41 H41A 109.1 . . ? C48 C41 H41A 109.1 . . ? C38 C41 H41B 109.1 . . ? C48 C41 H41B 109.1 . . ? H41A C41 H41B 107.8 . . ? N18 C40 N10 114.1(4) . . ? N18 C40 C19 114.2(4) . . ? N10 C40 C19 111.4(4) . . ? N18 C40 C2 104.2(4) . . ? N10 C40 C2 101.6(4) . . ? C19 C40 C2 110.3(5) . . ? C8 C39 C12 106.8(6) . . ? C8 C39 H39A 110.4 . . ? C12 C39 H39A 110.4 . . ? C8 C39 H39B 110.4 . . ? C12 C39 H39B 110.4 . . ? H39A C39 H39B 108.6 . . ? C41 C38 C47 115.9(6) . . ? C41 C38 H38A 108.3 . . ? C47 C38 H38A 108.3 . . ? C41 C38 H38B 108.3 . . ? C47 C38 H38B 108.3 . . ? H38A C38 H38B 107.4 . . ? C26 C48 C41 110.3(5) . . ? C26 C48 H48A 109.6 . . ? C41 C48 H48A 109.6 . . ? C26 C48 H48B 109.6 . . ? C41 C48 H48B 109.6 . . ? H48A C48 H48B 108.1 . . ? C42 C49 C50 108.0(5) . . ? C42 C49 H49A 110.1 . . ? C50 C49 H49A 110.1 . . ? C42 C49 H49B 110.1 . . ? C50 C49 H49B 110.1 . . ? H49A C49 H49B 108.4 . . ? C46 C50 C49 112.5(6) . . ? C46 C50 H50A 109.1 . . ? C49 C50 H50A 109.1 . . ? C46 C50 H50B 109.1 . . ? C49 C50 H50B 109.1 . . ? H50A C50 H50B 107.8 . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.20 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.737 _refine_diff_density_min -0.866 _refine_diff_density_rms 0.125