# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Kong, Xiang-Jian' _publ_contact_author_email xjkong@xmu.edu.cn _publ_section_title ; Series of Di-, Tri- and Tetranuclear Lanthanide Clusters with Slow Magnetic Relaxation for Dy2 and Dy4 ; loop_ _publ_author_name 'Xiang-Jian Kong' 'Jun-Bo Peng' 'Yan-Ping Ren' 'La-Sheng Long' ; Rongbin Huang ; 'Lansun Zheng' # Attachment '- compelx1.cif' data_complex1 _database_code_depnum_ccdc_archive 'CCDC 791391' #TrackingRef '- compelx1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C168 H364 Cl24 N24 Nd8 O74' _chemical_formula_weight 5909.55 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' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.2942(3) _cell_length_b 15.3925(4) _cell_length_c 50.4286(13) _cell_angle_alpha 90.00 _cell_angle_beta 96.817(2) _cell_angle_gamma 90.00 _cell_volume 12558.5(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 14114 _cell_measurement_theta_min 2.6591 _cell_measurement_theta_max 29.0666 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.563 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6040 _exptl_absorpt_coefficient_mu 1.957 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5913 _exptl_absorpt_correction_T_max 0.8283 _exptl_absorpt_process_details ? _exptl_special_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 57662 _diffrn_reflns_av_R_equivalents 0.0859 _diffrn_reflns_av_sigmaI/netI 0.1346 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 59 _diffrn_reflns_theta_min 2.74 _diffrn_reflns_theta_max 25.00 _reflns_number_total 22090 _reflns_number_gt 13835 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. Non-hydrogen atoms were refined anisotropically, except for 11 atoms (c9 c15 c22 c28 c50 c51 c53 c57 c61 c78 o9) were refined isotropically due to disorder ; _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^)+(0.0020P)^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 22090 _refine_ls_number_parameters 1342 _refine_ls_number_restraints 66 _refine_ls_R_factor_all 0.1024 _refine_ls_R_factor_gt 0.0574 _refine_ls_wR_factor_ref 0.0686 _refine_ls_wR_factor_gt 0.0634 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.003 _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 0.58034(2) 0.57648(2) 0.023693(8) 0.00976(9) Uani 1 1 d . . . Nd2 Nd 0.91879(2) 0.55766(2) 0.223696(7) 0.00971(9) Uani 1 1 d . . . Nd3 Nd 1.08522(3) 0.39642(2) 0.269849(7) 0.00961(9) Uani 1 1 d . . . Nd4 Nd 0.90178(2) 1.08907(2) -0.022584(8) 0.00955(9) Uani 1 1 d . . . Cl1 Cl 0.64583(12) 0.85297(10) -0.01120(4) 0.0205(4) Uani 1 1 d . . . Cl2 Cl 0.06591(12) 0.47063(10) 0.06977(4) 0.0215(4) Uani 1 1 d . . . Cl3 Cl 0.88576(12) 0.64553(11) 0.01356(3) 0.0210(4) Uani 1 1 d . . . Cl4 Cl 1.13129(12) 0.12437(10) 0.23431(4) 0.0211(4) Uani 1 1 d . . . Cl5 Cl 1.12832(12) 0.77515(10) 0.22933(3) 0.0201(4) Uani 1 1 d . . . Cl6 Cl 0.41443(12) 0.98376(10) -0.05370(4) 0.0282(5) Uani 1 1 d . . . Cl7 Cl 0.14668(12) 0.69817(10) -0.03977(4) 0.0217(5) Uani 1 1 d . . . Cl8 Cl 0.86807(12) 0.18323(11) 0.26035(4) 0.0219(5) Uani 1 1 d . . . Cl9 Cl 1.09259(12) -0.03673(10) 0.30675(4) 0.0227(4) Uani 1 1 d . . . Cl10 Cl 0.86126(12) 0.80064(10) 0.28512(4) 0.0219(5) Uani 1 1 d . . . Cl11 Cl 0.36707(12) 0.77802(10) 0.01263(3) 0.0182(4) Uani 1 1 d . . . Cl12 Cl 0.92534(12) 1.00126(10) 0.17822(4) 0.0222(5) Uani 1 1 d . . . O1 O 1.1838(3) 0.3793(3) 0.31131(9) 0.0211(12) Uani 1 1 d . . . O2 O 1.2318(3) 0.4554(3) 0.27953(9) 0.0138(11) Uani 1 1 d . . . O3 O 1.0631(3) 0.5352(3) 0.29063(9) 0.0128(12) Uani 1 1 d . . . O4 O 0.9892(3) 0.6259(3) 0.26250(9) 0.0152(12) Uani 1 1 d . . . O5 O 0.9678(3) 0.3729(3) 0.29533(9) 0.0155(12) Uani 1 1 d . . . O6 O 0.9250(3) 0.4472(3) 0.25935(9) 0.0140(11) Uani 1 1 d . . . O7 O 1.0176(3) 0.3253(2) 0.22941(9) 0.0162(12) Uani 1 1 d . . . O8 O 0.9380(3) 0.4186(3) 0.20370(9) 0.0178(12) Uani 1 1 d . . . O9 O 1.0937(3) 0.5009(3) 0.23480(9) 0.0136(11) Uani 1 1 d U . . O10 O 1.0414(3) 0.5715(3) 0.19902(9) 0.0182(11) Uani 1 1 d . . . O11 O 0.8080(3) 0.5675(3) 0.18594(9) 0.0219(12) Uani 1 1 d . . . O12 O 0.7693(3) 0.4965(3) 0.21991(9) 0.0135(11) Uani 1 1 d . . . O13 O 0.6729(3) 0.5837(3) 0.06641(9) 0.0174(12) Uani 1 1 d . . . O14 O 0.7212(3) 0.5061(3) 0.03479(9) 0.0142(12) Uani 1 1 d . . . O15 O 0.4709(3) 0.3516(3) 0.01779(9) 0.0157(12) Uani 1 1 d . . . O16 O 0.5512(3) 0.4396(3) 0.04508(8) 0.0136(11) Uani 1 1 d . . . O17 O 0.5803(3) 0.4622(2) -0.01060(8) 0.0115(11) Uani 1 1 d . . . O18 O 0.5397(3) 0.3946(3) -0.04833(8) 0.0143(11) Uani 1 1 d . . . O19 O 0.8827(3) 0.9684(3) 0.00588(9) 0.0157(12) Uani 1 1 d . . . O20 O 0.9583(3) 0.8775(3) 0.03310(9) 0.0165(12) Uani 1 1 d . . . O21 O 0.7424(4) 1.1416(3) -0.08116(10) 0.0424(16) Uani 1 1 d . . . O22 O 0.7626(3) 1.0642(3) -0.04364(9) 0.0168(11) Uani 1 1 d . . . O23 O 1.0573(3) 1.0420(3) 0.04416(9) 0.0165(12) Uani 1 1 d . . . O24 O 0.9751(3) 1.1356(3) 0.01929(9) 0.0182(12) Uani 1 1 d . . . O1W O 1.0645(3) 0.2372(3) 0.28044(9) 0.0198(13) Uani 1 1 d . . . O2W O 1.1920(3) 0.3150(3) 0.24608(8) 0.0170(12) Uani 1 1 d . . . O3W O 0.9443(3) 0.7068(3) 0.20680(9) 0.0196(13) Uani 1 1 d . . . O4W O 0.8210(3) 0.6602(3) 0.24270(9) 0.0201(12) Uani 1 1 d . . . O5W O 0.6948(3) 0.6638(3) 0.00715(9) 0.0181(12) Uani 1 1 d . . . O6W O 0.5621(3) 0.7368(3) 0.03463(9) 0.0169(12) Uani 1 1 d . . . O7W O 0.8994(3) 1.1528(3) -0.06793(8) 0.0164(11) Uani 1 1 d . . . O8W O 0.8810(3) 1.2515(2) -0.02018(9) 0.0217(13) Uani 1 1 d . . . O9W O 0.7955(3) 1.1331(2) 0.01035(8) 0.0143(11) Uani 1 1 d . . . O10W O 0.9941(4) 0.9769(3) 0.25132(10) 0.0397(15) Uani 1 1 d . . . O11W O 0.8901(3) 0.8693(3) 0.22013(9) 0.0192(12) Uani 1 1 d . . . O12W O 1.0360(3) 0.6755(3) 0.05792(9) 0.0260(13) Uani 1 1 d . . . O13W O 0.0978(3) 0.5401(3) 0.01333(9) 0.0270(13) Uani 1 1 d . . . C1 C 1.2404(5) 0.4218(4) 0.30247(13) 0.0123(17) Uani 1 1 d . . . C2 C 1.3216(4) 0.4366(4) 0.32108(13) 0.0137(16) Uani 1 1 d . . . C3 C 1.3433(5) 0.3601(4) 0.33958(13) 0.0205(18) Uani 1 1 d . . . H3A H 1.2945 0.3447 0.3486 0.025 Uiso 1 1 calc R . . H3B H 1.3569 0.3094 0.3288 0.025 Uiso 1 1 calc R . . C4 C 1.4157(5) 0.3786(4) 0.36056(14) 0.023(2) Uani 1 1 d . . . H4A H 1.4666 0.3846 0.3518 0.028 Uiso 1 1 calc R . . H4B H 1.4234 0.3289 0.3731 0.028 Uiso 1 1 calc R . . C5 C 1.4023(5) 0.4610(5) 0.37608(15) 0.032(2) Uani 1 1 d . . . H5A H 1.3553 0.4525 0.3866 0.038 Uiso 1 1 calc R . . H5B H 1.4522 0.4731 0.3887 0.038 Uiso 1 1 calc R . . C6 C 1.3847(5) 0.5379(4) 0.35744(13) 0.0199(18) Uani 1 1 d . . . H6A H 1.3729 0.5897 0.3680 0.024 Uiso 1 1 calc R . . H6B H 1.4343 0.5505 0.3485 0.024 Uiso 1 1 calc R . . C7 C 1.3124(4) 0.5209(4) 0.33659(13) 0.0146(17) Uani 1 1 d . . . H7A H 1.3066 0.5701 0.3239 0.018 Uiso 1 1 calc R . . H7B H 1.2613 0.5178 0.3454 0.018 Uiso 1 1 calc R . . C8 C 1.0412(4) 0.6089(4) 0.28220(13) 0.0118(16) Uani 1 1 d . . . C9 C 1.0831(4) 0.6853(4) 0.29790(12) 0.0068(15) Uani 1 1 d U . . C10 C 1.1754(4) 0.6786(4) 0.29586(13) 0.0097(16) Uani 1 1 d . . . H10A H 1.1952 0.6202 0.3019 0.012 Uiso 1 1 calc R . . H10B H 1.1850 0.6852 0.2769 0.012 Uiso 1 1 calc R . . C11 C 1.2246(5) 0.7469(4) 0.31249(13) 0.0180(18) Uani 1 1 d . . . H11A H 1.2106 0.8051 0.3048 0.022 Uiso 1 1 calc R . . H11B H 1.2843 0.7369 0.3118 0.022 Uiso 1 1 calc R . . C12 C 1.2067(6) 0.7450(4) 0.34153(14) 0.028(2) Uani 1 1 d . . . H12A H 1.2275 0.6899 0.3499 0.034 Uiso 1 1 calc R . . H12B H 1.2365 0.7934 0.3514 0.034 Uiso 1 1 calc R . . C13 C 1.1151(5) 0.7531(4) 0.34375(14) 0.0203(19) Uani 1 1 d . . . H13A H 1.0964 0.8122 0.3380 0.024 Uiso 1 1 calc R . . H13B H 1.1058 0.7459 0.3627 0.024 Uiso 1 1 calc R . . C14 C 1.0628(5) 0.6853(4) 0.32658(12) 0.0160(17) Uani 1 1 d . . . H14A H 1.0734 0.6268 0.3344 0.019 Uiso 1 1 calc R . . H14B H 1.0034 0.6985 0.3267 0.019 Uiso 1 1 calc R . . C15 C 0.9119(4) 0.4100(4) 0.28107(13) 0.0094(15) Uani 1 1 d U . . C16 C 0.8232(4) 0.4133(4) 0.28861(13) 0.0118(16) Uani 1 1 d . . . C17 C 0.7968(4) 0.5065(4) 0.29248(14) 0.0180(18) Uani 1 1 d . . . H17A H 0.7371 0.5084 0.2945 0.022 Uiso 1 1 calc R . . H17B H 0.8061 0.5415 0.2767 0.022 Uiso 1 1 calc R . . C18 C 0.8466(5) 0.5440(4) 0.31730(15) 0.034(2) Uani 1 1 d . . . H18A H 0.9063 0.5419 0.3153 0.041 Uiso 1 1 calc R . . H18B H 0.8310 0.6055 0.3195 0.041 Uiso 1 1 calc R . . C19 C 0.8304(6) 0.4927(5) 0.34153(15) 0.036(2) Uani 1 1 d . . . H19A H 0.7709 0.4964 0.3438 0.043 Uiso 1 1 calc R . . H19B H 0.8622 0.5181 0.3576 0.043 Uiso 1 1 calc R . . C20 C 0.8547(5) 0.3975(5) 0.33898(14) 0.031(2) Uani 1 1 d . . . H20A H 0.9154 0.3930 0.3392 0.037 Uiso 1 1 calc R . . H20B H 0.8387 0.3642 0.3544 0.037 Uiso 1 1 calc R . . C21 C 0.8131(5) 0.3597(4) 0.31359(13) 0.0163(18) Uani 1 1 d . . . H21A H 0.7534 0.3534 0.3151 0.020 Uiso 1 1 calc R . . H21B H 0.8357 0.3008 0.3113 0.020 Uiso 1 1 calc R . . C22 C 0.9654(4) 0.3438(4) 0.21021(13) 0.0108(16) Uani 1 1 d U . . C23 C 0.9323(4) 0.2716(4) 0.19137(13) 0.0089(16) Uani 1 1 d . . . C24 C 0.9777(5) 0.2736(4) 0.16660(12) 0.0146(17) Uani 1 1 d . . . H24A H 1.0364 0.2583 0.1718 0.018 Uiso 1 1 calc R . . H24B H 0.9759 0.3334 0.1594 0.018 Uiso 1 1 calc R . . C25 C 0.9409(5) 0.2108(4) 0.14443(14) 0.025(2) Uani 1 1 d . . . H25A H 0.9674 0.2215 0.1281 0.029 Uiso 1 1 calc R . . H25B H 0.9533 0.1502 0.1502 0.029 Uiso 1 1 calc R . . C26 C 0.8494(5) 0.2216(4) 0.13822(14) 0.026(2) Uani 1 1 d . . . H26A H 0.8278 0.1768 0.1251 0.031 Uiso 1 1 calc R . . H26B H 0.8375 0.2793 0.1300 0.031 Uiso 1 1 calc R . . C27 C 0.8058(5) 0.2139(4) 0.16291(14) 0.0215(19) Uani 1 1 d . . . H27A H 0.8129 0.1542 0.1701 0.026 Uiso 1 1 calc R . . H27B H 0.7459 0.2243 0.1581 0.026 Uiso 1 1 calc R . . C28 C 0.8394(4) 0.2786(4) 0.18430(13) 0.0140(16) Uani 1 1 d U . . H28A H 0.8255 0.3383 0.1779 0.017 Uiso 1 1 calc R . . H28B H 0.8122 0.2687 0.2006 0.017 Uiso 1 1 calc R . . C29 C 1.0991(5) 0.5341(4) 0.21234(13) 0.0134(17) Uani 1 1 d . . . C30 C 1.1805(4) 0.5250(4) 0.20023(13) 0.0106(16) Uani 1 1 d . . . C31 C 1.2081(5) 0.6048(4) 0.18602(14) 0.0223(19) Uani 1 1 d . . . H31A H 1.2045 0.6560 0.1977 0.027 Uiso 1 1 calc R . . H31B H 1.2669 0.5975 0.1833 0.027 Uiso 1 1 calc R . . C32 C 1.1585(5) 0.6229(4) 0.15936(15) 0.030(2) Uani 1 1 d . . . H32A H 1.1022 0.6420 0.1622 0.036 Uiso 1 1 calc R . . H32B H 1.1849 0.6706 0.1503 0.036 Uiso 1 1 calc R . . C33 C 1.1529(5) 0.5439(5) 0.14203(14) 0.035(2) Uani 1 1 d . . . H33A H 1.1165 0.5567 0.1253 0.042 Uiso 1 1 calc R . . H33B H 1.2085 0.5302 0.1372 0.042 Uiso 1 1 calc R . . C34 C 1.1204(5) 0.4669(5) 0.15495(14) 0.034(2) Uani 1 1 d . . . H34A H 1.1205 0.4161 0.1429 0.040 Uiso 1 1 calc R . . H34B H 1.0627 0.4778 0.1583 0.040 Uiso 1 1 calc R . . C35 C 1.1734(5) 0.4469(4) 0.18139(13) 0.0208(18) Uani 1 1 d . . . H35A H 1.1488 0.3975 0.1902 0.025 Uiso 1 1 calc R . . H35B H 1.2294 0.4294 0.1777 0.025 Uiso 1 1 calc R . . C36 C 0.7538(5) 0.5299(4) 0.19699(15) 0.0152(17) Uani 1 1 d . . . C37 C 0.6667(4) 0.5248(4) 0.18188(13) 0.0112(16) Uani 1 1 d . . . C38 C 0.6636(4) 0.4518(4) 0.16083(13) 0.0190(17) Uani 1 1 d . . . H38A H 0.7087 0.4609 0.1496 0.023 Uiso 1 1 calc R . . H38B H 0.6732 0.3953 0.1700 0.023 Uiso 1 1 calc R . . C39 C 0.5830(5) 0.4489(5) 0.14339(15) 0.034(2) Uani 1 1 d . . . H39A H 0.5391 0.4313 0.1543 0.041 Uiso 1 1 calc R . . H39B H 0.5860 0.4041 0.1294 0.041 Uiso 1 1 calc R . . C40 C 0.5594(6) 0.5355(5) 0.12999(16) 0.045(3) Uani 1 1 d . . . H40A H 0.6004 0.5511 0.1178 0.053 Uiso 1 1 calc R . . H40B H 0.5046 0.5304 0.1193 0.053 Uiso 1 1 calc R . . C41 C 0.5567(5) 0.6055(5) 0.15083(15) 0.031(2) Uani 1 1 d . . . H41A H 0.5117 0.5927 0.1618 0.037 Uiso 1 1 calc R . . H41B H 0.5448 0.6621 0.1419 0.037 Uiso 1 1 calc R . . C42 C 0.6392(5) 0.6109(4) 0.16890(14) 0.0225(19) Uani 1 1 d . . . H42A H 0.6824 0.6316 0.1582 0.027 Uiso 1 1 calc R . . H42B H 0.6340 0.6543 0.1831 0.027 Uiso 1 1 calc R . . C43 C 0.7295(4) 0.5404(4) 0.05773(13) 0.0112(16) Uani 1 1 d . . . C44 C 0.8118(4) 0.5333(4) 0.07589(13) 0.0121(17) Uani 1 1 d . . . C45 C 0.8398(5) 0.6225(4) 0.08639(13) 0.0126(17) Uani 1 1 d . . . H45A H 0.7934 0.6508 0.0941 0.015 Uiso 1 1 calc R . . H45B H 0.8533 0.6586 0.0712 0.015 Uiso 1 1 calc R . . C46 C 0.9149(5) 0.6199(4) 0.10763(14) 0.0227(19) Uani 1 1 d . . . H46A H 0.9634 0.5977 0.0997 0.027 Uiso 1 1 calc R . . H46B H 0.9278 0.6793 0.1144 0.027 Uiso 1 1 calc R . . C47 C 0.8974(5) 0.5620(5) 0.13031(14) 0.029(2) Uani 1 1 d . . . H47A H 0.9466 0.5601 0.1438 0.035 Uiso 1 1 calc R . . H47B H 0.8509 0.5864 0.1389 0.035 Uiso 1 1 calc R . . C48 C 0.8761(5) 0.4717(4) 0.12093(13) 0.0230(19) Uani 1 1 d . . . H48A H 0.8623 0.4365 0.1362 0.028 Uiso 1 1 calc R . . H48B H 0.9248 0.4451 0.1141 0.028 Uiso 1 1 calc R . . C49 C 0.8034(4) 0.4702(4) 0.09901(13) 0.0183(18) Uani 1 1 d . . . H49A H 0.7524 0.4846 0.1070 0.022 Uiso 1 1 calc R . . H49B H 0.7971 0.4105 0.0918 0.022 Uiso 1 1 calc R . . C50 C 0.5223(5) 0.3673(4) 0.03729(13) 0.0117(16) Uani 1 1 d U . . C51 C 0.5575(4) 0.2887(4) 0.05448(13) 0.0088(15) Uani 1 1 d U . . C52 C 0.6497(4) 0.2954(4) 0.06117(13) 0.0148(17) Uani 1 1 d . . . H52A H 0.6634 0.3522 0.0698 0.018 Uiso 1 1 calc R . . H52B H 0.6759 0.2933 0.0444 0.018 Uiso 1 1 calc R . . C53 C 0.6853(5) 0.2235(4) 0.07958(14) 0.0206(18) Uani 1 1 d U . . H53A H 0.6776 0.1671 0.0702 0.025 Uiso 1 1 calc R . . H53B H 0.7453 0.2331 0.0842 0.025 Uiso 1 1 calc R . . C54 C 0.6445(5) 0.2201(4) 0.10475(14) 0.029(2) Uani 1 1 d . . . H54A H 0.6577 0.2738 0.1152 0.035 Uiso 1 1 calc R . . H54B H 0.6669 0.1703 0.1157 0.035 Uiso 1 1 calc R . . C55 C 0.5506(5) 0.2109(4) 0.09886(14) 0.025(2) Uani 1 1 d . . . H55A H 0.5255 0.2152 0.1158 0.030 Uiso 1 1 calc R . . H55B H 0.5370 0.1529 0.0910 0.030 Uiso 1 1 calc R . . C56 C 0.5134(5) 0.2818(4) 0.07938(13) 0.0149(17) Uani 1 1 d . . . H56A H 0.4543 0.2687 0.0740 0.018 Uiso 1 1 calc R . . H56B H 0.5167 0.3385 0.0887 0.018 Uiso 1 1 calc R . . C57 C 0.5948(4) 0.4275(4) -0.03267(13) 0.0112(16) Uani 1 1 d U . . C58 C 0.6842(4) 0.4292(4) -0.03929(13) 0.0118(16) Uani 1 1 d . . . C59 C 0.7015(5) 0.5237(4) -0.04763(13) 0.0159(17) Uani 1 1 d . . . H59A H 0.6854 0.5643 -0.0339 0.019 Uiso 1 1 calc R . . H59B H 0.7614 0.5310 -0.0486 0.019 Uiso 1 1 calc R . . C60 C 0.6542(5) 0.5457(4) -0.07427(14) 0.0216(19) Uani 1 1 d . . . H60A H 0.6645 0.6070 -0.0788 0.026 Uiso 1 1 calc R . . H60B H 0.5942 0.5385 -0.0734 0.026 Uiso 1 1 calc R . . C61 C 0.6819(5) 0.4859(4) -0.09565(15) 0.030(2) Uani 1 1 d U . . H61A H 0.6515 0.5008 -0.1132 0.036 Uiso 1 1 calc R . . H61B H 0.7416 0.4943 -0.0967 0.036 Uiso 1 1 calc R . . C62 C 0.6656(5) 0.3912(4) -0.08910(13) 0.025(2) Uani 1 1 d . . . H62A H 0.6878 0.3532 -0.1024 0.030 Uiso 1 1 calc R . . H62B H 0.6053 0.3813 -0.0902 0.030 Uiso 1 1 calc R . . C63 C 0.7062(5) 0.3673(4) -0.06093(13) 0.0158(17) Uani 1 1 d . . . H63A H 0.6890 0.3078 -0.0566 0.019 Uiso 1 1 calc R . . H63B H 0.7670 0.3669 -0.0609 0.019 Uiso 1 1 calc R . . C64 C 0.8961(5) 0.9231(4) 0.02662(14) 0.0158(17) Uani 1 1 d . . . C65 C 0.8324(4) 0.9271(4) 0.04705(13) 0.0129(16) Uani 1 1 d . . . C66 C 0.8686(5) 0.9857(5) 0.07024(14) 0.027(2) Uani 1 1 d . . . H66A H 0.9241 0.9641 0.0773 0.032 Uiso 1 1 calc R . . H66B H 0.8750 1.0454 0.0634 0.032 Uiso 1 1 calc R . . C67 C 0.8142(6) 0.9884(5) 0.09285(15) 0.041(3) Uani 1 1 d . . . H67A H 0.8423 1.0218 0.1081 0.050 Uiso 1 1 calc R . . H67B H 0.7614 1.0178 0.0866 0.050 Uiso 1 1 calc R . . C68 C 0.7972(7) 0.8966(6) 0.10183(16) 0.057(3) Uani 1 1 d . . . H68A H 0.8501 0.8687 0.1089 0.069 Uiso 1 1 calc R . . H68B H 0.7618 0.8990 0.1164 0.069 Uiso 1 1 calc R . . C69 C 0.7558(6) 0.8435(5) 0.07951(17) 0.042(3) Uani 1 1 d . . . H69A H 0.7020 0.8702 0.0728 0.050 Uiso 1 1 calc R . . H69B H 0.7450 0.7844 0.0860 0.050 Uiso 1 1 calc R . . C70 C 0.8096(5) 0.8378(4) 0.05714(14) 0.022(2) Uani 1 1 d . . . H70A H 0.7800 0.8045 0.0421 0.027 Uiso 1 1 calc R . . H70B H 0.8608 0.8058 0.0635 0.027 Uiso 1 1 calc R . . C71 C 0.7187(5) 1.0911(4) -0.06430(14) 0.0184(17) Uani 1 1 d . . . C72 C 0.6299(4) 1.0569(4) -0.06925(13) 0.0146(16) Uani 1 1 d . . . C73 C 0.5693(5) 1.1213(4) -0.08441(13) 0.0204(18) Uani 1 1 d . . . H73A H 0.5795 1.1798 -0.0766 0.025 Uiso 1 1 calc R . . H73B H 0.5123 1.1042 -0.0818 0.025 Uiso 1 1 calc R . . C74 C 0.5756(5) 1.1265(5) -0.11485(14) 0.034(2) Uani 1 1 d . . . H74A H 0.5287 1.1609 -0.1236 0.041 Uiso 1 1 calc R . . H74B H 0.6274 1.1568 -0.1178 0.041 Uiso 1 1 calc R . . C75 C 0.5749(6) 1.0401(5) -0.12719(15) 0.039(2) Uani 1 1 d . . . H75A H 0.5851 1.0464 -0.1461 0.047 Uiso 1 1 calc R . . H75B H 0.5194 1.0141 -0.1270 0.047 Uiso 1 1 calc R . . C76 C 0.6395(5) 0.9789(5) -0.11296(14) 0.033(2) Uani 1 1 d . . . H76A H 0.6347 0.9210 -0.1215 0.039 Uiso 1 1 calc R . . H76B H 0.6956 1.0017 -0.1145 0.039 Uiso 1 1 calc R . . C77 C 0.6274(5) 0.9705(4) -0.08383(13) 0.0213(18) Uani 1 1 d . . . H77A H 0.6710 0.9323 -0.0749 0.026 Uiso 1 1 calc R . . H77B H 0.5734 0.9424 -0.0825 0.026 Uiso 1 1 calc R . . C78 C 1.0341(4) 1.1165(4) 0.03713(13) 0.0101(16) Uani 1 1 d U . . C79 C 1.0829(5) 1.1910(4) 0.05122(13) 0.0149(18) Uani 1 1 d . . . C80 C 1.0768(5) 1.1878(4) 0.08082(12) 0.0124(17) Uani 1 1 d . . . H80A H 1.0905 1.1283 0.0874 0.015 Uiso 1 1 calc R . . H80B H 1.0190 1.1999 0.0838 0.015 Uiso 1 1 calc R . . C81 C 1.1337(5) 1.2523(4) 0.09710(14) 0.0203(19) Uani 1 1 d . . . H81A H 1.1141 1.3123 0.0930 0.024 Uiso 1 1 calc R . . H81B H 1.1316 1.2419 0.1164 0.024 Uiso 1 1 calc R . . C82 C 1.2223(5) 1.2430(4) 0.09080(14) 0.025(2) Uani 1 1 d . . . H82A H 1.2439 1.1853 0.0968 0.030 Uiso 1 1 calc R . . H82B H 1.2572 1.2878 0.1007 0.030 Uiso 1 1 calc R . . C83 C 1.2276(5) 1.2528(4) 0.06091(13) 0.0191(18) Uani 1 1 d . . . H83A H 1.2097 1.3120 0.0551 0.023 Uiso 1 1 calc R . . H83B H 1.2855 1.2450 0.0573 0.023 Uiso 1 1 calc R . . C84 C 1.1731(4) 1.1861(4) 0.04527(13) 0.0110(16) Uani 1 1 d . . . H84A H 1.1950 1.1273 0.0497 0.013 Uiso 1 1 calc R . . H84B H 1.1750 1.1956 0.0259 0.013 Uiso 1 1 calc R . . N1 N 1.3863(4) 0.4498(3) 0.30287(10) 0.0145(14) Uani 1 1 d . . . H1A H 1.3722 0.4956 0.2919 0.022 Uiso 1 1 calc R . . H1B H 1.3905 0.4010 0.2929 0.022 Uiso 1 1 calc R . . H1C H 1.4358 0.4606 0.3127 0.022 Uiso 1 1 calc R . . N2 N 1.0508(3) 0.7680(3) 0.28403(10) 0.0092(13) Uani 1 1 d . . . H2A H 0.9956 0.7729 0.2851 0.014 Uiso 1 1 calc R . . H2B H 1.0600 0.7663 0.2666 0.014 Uiso 1 1 calc R . . H2C H 1.0775 0.8146 0.2921 0.014 Uiso 1 1 calc R . . N3 N 0.7696(4) 0.3734(3) 0.26493(10) 0.0155(14) Uani 1 1 d . . . H3C H 0.7159 0.3730 0.2683 0.023 Uiso 1 1 calc R . . H3D H 0.7865 0.3180 0.2624 0.023 Uiso 1 1 calc R . . H3E H 0.7743 0.4054 0.2500 0.023 Uiso 1 1 calc R . . N4 N 0.9521(4) 0.1864(3) 0.20625(10) 0.0133(14) Uani 1 1 d . . . H4C H 0.9338 0.1410 0.1956 0.020 Uiso 1 1 calc R . . H4D H 0.9266 0.1854 0.2213 0.020 Uiso 1 1 calc R . . H4E H 1.0077 0.1818 0.2107 0.020 Uiso 1 1 calc R . . N5 N 1.2466(4) 0.5018(4) 0.22294(11) 0.0249(16) Uani 1 1 d . . . H5C H 1.2961 0.4958 0.2165 0.037 Uiso 1 1 calc R . . H5D H 1.2330 0.4511 0.2306 0.037 Uiso 1 1 calc R . . H5E H 1.2503 0.5449 0.2354 0.037 Uiso 1 1 calc R . . N6 N 0.6100(4) 0.5011(3) 0.20191(10) 0.0146(14) Uani 1 1 d . . . H6C H 0.6111 0.5437 0.2145 0.022 Uiso 1 1 calc R . . H6D H 0.6268 0.4501 0.2099 0.022 Uiso 1 1 calc R . . H6E H 0.5577 0.4951 0.1936 0.022 Uiso 1 1 calc R . . N7 N 0.8731(4) 0.4971(3) 0.05932(10) 0.0130(14) Uani 1 1 d . . . H7C H 0.9229 0.4915 0.0695 0.019 Uiso 1 1 calc R . . H7D H 0.8784 0.5336 0.0454 0.019 Uiso 1 1 calc R . . H7E H 0.8558 0.4441 0.0529 0.019 Uiso 1 1 calc R . . N8 N 0.5358(4) 0.2086(3) 0.03785(10) 0.0142(14) Uani 1 1 d . . . H8A H 0.5539 0.1605 0.0473 0.021 Uiso 1 1 calc R . . H8B H 0.5604 0.2114 0.0226 0.021 Uiso 1 1 calc R . . H8C H 0.4800 0.2056 0.0336 0.021 Uiso 1 1 calc R . . N9 N 0.7377(3) 0.4087(3) -0.01381(10) 0.0163(14) Uani 1 1 d . . . H9A H 0.7281 0.3531 -0.0088 0.024 Uiso 1 1 calc R . . H9B H 0.7257 0.4459 -0.0008 0.024 Uiso 1 1 calc R . . H9C H 0.7918 0.4146 -0.0163 0.024 Uiso 1 1 calc R . . N10 N 0.7560(4) 0.9691(3) 0.03282(10) 0.0140(14) Uani 1 1 d . . . H10C H 0.7166 0.9728 0.0441 0.021 Uiso 1 1 calc R . . H10D H 0.7366 0.9364 0.0184 0.021 Uiso 1 1 calc R . . H10E H 0.7686 1.0232 0.0273 0.021 Uiso 1 1 calc R . . N11 N 0.6016(4) 1.0406(3) -0.04236(10) 0.0168(15) Uani 1 1 d . . . H11C H 0.6014 1.0915 -0.0332 0.025 Uiso 1 1 calc R . . H11D H 0.6365 1.0024 -0.0330 0.025 Uiso 1 1 calc R . . H11E H 0.5496 1.0181 -0.0446 0.025 Uiso 1 1 calc R . . N12 N 1.0454(4) 1.2760(3) 0.04011(10) 0.0136(14) Uani 1 1 d . . . H12C H 1.0495 1.2789 0.0223 0.020 Uiso 1 1 calc R . . H12D H 1.0731 1.3214 0.0485 0.020 Uiso 1 1 calc R . . H12E H 0.9913 1.2783 0.0428 0.020 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 0.0079(2) 0.00902(19) 0.0121(2) -0.00003(16) 0.00005(17) 0.00150(16) Nd2 0.0076(2) 0.00984(19) 0.0116(2) -0.00041(17) 0.00063(17) -0.00001(17) Nd3 0.0081(2) 0.00984(19) 0.0109(2) -0.00107(17) 0.00111(17) -0.00041(17) Nd4 0.0076(2) 0.00915(19) 0.0119(2) -0.00035(16) 0.00100(17) 0.00039(17) Cl1 0.0194(11) 0.0171(9) 0.0240(11) 0.0006(8) -0.0014(9) -0.0006(8) Cl2 0.0155(11) 0.0210(10) 0.0280(11) -0.0015(8) 0.0019(9) 0.0026(8) Cl3 0.0149(11) 0.0284(10) 0.0202(11) 0.0068(8) 0.0036(9) -0.0003(8) Cl4 0.0181(11) 0.0186(9) 0.0256(11) -0.0085(8) -0.0010(9) 0.0023(8) Cl5 0.0200(12) 0.0236(10) 0.0172(10) 0.0033(8) 0.0043(9) -0.0053(8) Cl6 0.0130(11) 0.0180(10) 0.0553(14) 0.0014(9) 0.0112(10) 0.0020(8) Cl7 0.0183(11) 0.0185(9) 0.0292(12) -0.0096(8) 0.0072(9) 0.0006(8) Cl8 0.0172(11) 0.0256(10) 0.0235(11) 0.0032(9) 0.0054(9) -0.0033(9) Cl9 0.0161(11) 0.0198(10) 0.0328(12) -0.0029(8) 0.0057(9) -0.0006(8) Cl10 0.0155(11) 0.0186(9) 0.0314(12) -0.0083(8) 0.0013(9) 0.0034(8) Cl11 0.0184(12) 0.0157(9) 0.0207(11) -0.0002(8) 0.0035(9) 0.0020(8) Cl12 0.0194(11) 0.0168(9) 0.0301(12) 0.0022(8) 0.0020(9) -0.0001(8) O1 0.014(3) 0.034(3) 0.014(3) 0.006(2) -0.002(2) -0.006(3) O2 0.010(3) 0.016(3) 0.014(3) 0.000(2) -0.004(2) -0.001(2) O3 0.021(3) 0.006(2) 0.011(3) -0.003(2) 0.002(2) 0.004(2) O4 0.018(3) 0.009(2) 0.017(3) -0.003(2) -0.006(2) 0.001(2) O5 0.013(3) 0.014(2) 0.020(3) 0.007(2) 0.005(2) 0.000(2) O6 0.015(3) 0.012(2) 0.015(3) -0.002(2) 0.002(2) -0.005(2) O7 0.018(3) 0.013(2) 0.016(3) -0.003(2) -0.006(2) 0.003(2) O8 0.022(3) 0.012(3) 0.018(3) -0.001(2) -0.003(2) 0.005(2) O9 0.0142(14) 0.0142(13) 0.0126(14) 0.0003(9) 0.0028(9) -0.0005(9) O10 0.015(3) 0.018(3) 0.023(3) 0.006(2) 0.006(2) 0.003(2) O11 0.006(3) 0.047(3) 0.013(3) 0.002(2) 0.001(2) -0.010(3) O12 0.012(3) 0.018(3) 0.010(3) 0.006(2) 0.001(2) -0.005(2) O13 0.011(3) 0.027(3) 0.014(3) -0.006(2) 0.002(2) 0.004(2) O14 0.015(3) 0.014(2) 0.013(3) -0.005(2) -0.003(2) 0.002(2) O15 0.017(3) 0.012(2) 0.016(3) 0.003(2) -0.006(2) -0.003(2) O16 0.016(3) 0.010(2) 0.014(3) 0.001(2) 0.002(2) -0.001(2) O17 0.015(3) 0.008(2) 0.013(3) 0.000(2) 0.003(2) -0.005(2) O18 0.016(3) 0.015(2) 0.013(3) -0.005(2) 0.006(2) -0.007(2) O19 0.023(3) 0.012(2) 0.013(3) 0.006(2) 0.007(2) 0.000(2) O20 0.011(3) 0.014(2) 0.024(3) 0.006(2) 0.001(2) 0.004(2) O21 0.026(4) 0.064(4) 0.034(4) 0.026(3) -0.009(3) -0.018(3) O22 0.014(3) 0.018(3) 0.017(3) 0.000(2) -0.004(2) -0.002(2) O23 0.026(3) 0.004(2) 0.019(3) 0.000(2) 0.002(2) 0.000(2) O24 0.009(3) 0.017(2) 0.028(3) -0.005(2) 0.000(2) 0.006(2) O1W 0.027(4) 0.015(2) 0.018(3) 0.003(2) 0.002(3) -0.001(2) O2W 0.015(3) 0.028(3) 0.010(3) -0.006(2) 0.006(2) -0.001(2) O3W 0.028(4) 0.013(2) 0.020(3) 0.009(2) 0.013(3) 0.002(2) O4W 0.014(3) 0.024(3) 0.023(3) -0.008(2) 0.005(2) 0.005(2) O5W 0.022(3) 0.020(3) 0.012(3) 0.002(2) 0.003(2) -0.001(2) O6W 0.028(4) 0.012(2) 0.011(3) -0.006(2) 0.004(2) -0.001(2) O7W 0.021(3) 0.018(2) 0.011(3) 0.004(2) 0.004(2) -0.001(2) O8W 0.029(4) 0.009(2) 0.028(3) -0.002(2) 0.006(3) 0.005(2) O9W 0.018(3) 0.012(2) 0.016(3) 0.001(2) 0.013(2) -0.001(2) O10W 0.046(4) 0.042(3) 0.030(3) 0.003(3) -0.002(3) -0.014(3) O11W 0.014(3) 0.021(2) 0.024(3) 0.001(2) 0.008(2) 0.004(2) O12W 0.039(4) 0.022(3) 0.020(3) -0.005(2) 0.013(3) -0.010(3) O13W 0.019(3) 0.030(3) 0.033(3) 0.006(2) 0.006(3) -0.006(2) C1 0.018(5) 0.008(4) 0.011(4) -0.001(3) 0.006(3) 0.008(3) C2 0.008(4) 0.020(4) 0.013(4) 0.008(3) 0.004(3) 0.005(3) C3 0.019(5) 0.022(4) 0.019(4) 0.002(3) -0.002(4) 0.003(3) C4 0.019(5) 0.028(4) 0.021(5) 0.013(4) -0.005(4) 0.006(4) C5 0.025(6) 0.046(5) 0.021(5) -0.002(4) -0.014(4) -0.003(4) C6 0.022(5) 0.019(4) 0.018(4) -0.009(3) 0.002(4) 0.001(3) C7 0.014(4) 0.011(4) 0.019(4) 0.001(3) 0.002(4) 0.001(3) C8 0.011(4) 0.014(4) 0.012(4) 0.000(3) 0.007(3) 0.005(3) C9 0.0068(17) 0.0070(17) 0.0068(17) 0.0006(10) 0.0007(10) 0.0004(10) C10 0.008(4) 0.009(3) 0.013(4) 0.004(3) 0.002(3) -0.003(3) C11 0.006(4) 0.022(4) 0.025(5) -0.003(3) -0.002(4) -0.002(3) C12 0.054(7) 0.017(4) 0.012(4) -0.001(3) -0.002(4) -0.011(4) C13 0.026(5) 0.026(4) 0.009(4) -0.006(3) 0.003(4) -0.008(4) C14 0.023(5) 0.015(4) 0.010(4) -0.001(3) 0.004(4) -0.005(3) C15 0.0098(18) 0.0089(17) 0.0096(17) -0.0002(10) 0.0013(10) 0.0003(10) C16 0.009(4) 0.010(4) 0.016(4) -0.005(3) 0.003(3) -0.002(3) C17 0.005(4) 0.027(4) 0.022(4) 0.005(3) 0.003(4) -0.004(3) C18 0.036(6) 0.024(4) 0.044(6) -0.021(4) 0.014(5) -0.008(4) C19 0.025(5) 0.055(6) 0.026(5) -0.033(4) 0.000(4) 0.002(4) C20 0.026(5) 0.051(5) 0.018(5) 0.001(4) 0.007(4) 0.002(4) C21 0.012(5) 0.017(4) 0.020(4) 0.008(3) 0.003(4) 0.005(3) C22 0.0109(18) 0.0114(18) 0.0104(18) -0.0004(10) 0.0022(10) 0.0001(10) C23 0.007(4) 0.009(3) 0.009(4) 0.001(3) -0.007(3) 0.000(3) C24 0.018(5) 0.016(4) 0.009(4) 0.004(3) -0.001(3) -0.001(3) C25 0.043(6) 0.019(4) 0.013(4) -0.002(3) 0.007(4) 0.004(4) C26 0.038(6) 0.021(4) 0.013(4) 0.002(3) -0.014(4) 0.005(4) C27 0.009(4) 0.019(4) 0.032(5) 0.009(4) -0.013(4) -0.002(3) C28 0.0130(19) 0.0145(18) 0.0144(18) -0.0001(10) 0.0019(10) 0.0001(10) C29 0.023(5) 0.005(3) 0.012(4) 0.000(3) 0.001(4) 0.001(3) C30 0.004(4) 0.014(4) 0.013(4) 0.001(3) -0.001(3) 0.000(3) C31 0.025(5) 0.015(4) 0.030(5) -0.002(4) 0.018(4) -0.001(4) C32 0.034(6) 0.028(5) 0.031(5) 0.016(4) 0.022(4) 0.011(4) C33 0.035(6) 0.057(6) 0.014(4) 0.012(4) 0.007(4) 0.012(5) C34 0.032(6) 0.041(5) 0.026(5) -0.021(4) -0.008(4) 0.008(4) C35 0.026(5) 0.011(4) 0.027(5) 0.001(3) 0.010(4) -0.004(3) C36 0.008(4) 0.014(4) 0.023(5) -0.002(3) 0.002(4) -0.002(3) C37 0.007(4) 0.013(4) 0.015(4) 0.006(3) 0.004(3) -0.005(3) C38 0.019(5) 0.023(4) 0.014(4) -0.008(3) 0.000(3) 0.006(3) C39 0.030(5) 0.044(5) 0.027(5) -0.024(4) -0.001(4) 0.001(4) C40 0.022(6) 0.080(7) 0.027(5) 0.002(5) -0.017(4) -0.002(5) C41 0.020(5) 0.038(5) 0.032(5) 0.009(4) -0.007(4) 0.011(4) C42 0.017(5) 0.025(4) 0.025(5) 0.009(4) -0.001(4) 0.003(4) C43 0.008(4) 0.017(4) 0.009(4) 0.001(3) 0.003(3) -0.006(3) C44 0.014(4) 0.011(4) 0.012(4) 0.000(3) 0.005(3) 0.006(3) C45 0.022(5) 0.007(3) 0.007(4) 0.002(3) -0.004(3) 0.004(3) C46 0.020(5) 0.025(4) 0.022(5) -0.012(4) 0.000(4) -0.004(4) C47 0.019(5) 0.052(5) 0.016(4) 0.002(4) 0.000(4) 0.005(4) C48 0.025(5) 0.033(4) 0.010(4) 0.013(3) 0.000(4) -0.001(4) C49 0.014(4) 0.025(4) 0.016(4) 0.009(3) 0.004(4) -0.002(3) C50 0.0115(18) 0.0125(18) 0.0114(18) 0.0001(10) 0.0023(10) 0.0006(10) C51 0.0087(18) 0.0087(17) 0.0090(18) 0.0000(10) 0.0006(10) -0.0007(10) C52 0.013(4) 0.014(4) 0.016(4) 0.002(3) -0.003(3) -0.001(3) C53 0.020(2) 0.021(2) 0.021(2) 0.0001(10) 0.0016(10) -0.0002(10) C54 0.040(6) 0.019(4) 0.024(5) 0.006(4) -0.009(4) 0.001(4) C55 0.027(5) 0.026(4) 0.022(5) 0.005(4) 0.002(4) 0.001(4) C56 0.016(5) 0.017(4) 0.011(4) 0.002(3) -0.002(3) 0.002(3) C57 0.0115(18) 0.0105(18) 0.0114(18) 0.0004(10) 0.0010(10) 0.0005(10) C58 0.014(4) 0.013(4) 0.008(4) 0.000(3) -0.002(3) 0.000(3) C59 0.011(4) 0.018(4) 0.020(4) -0.001(3) 0.006(4) -0.002(3) C60 0.025(5) 0.014(4) 0.025(5) 0.011(3) 0.000(4) -0.001(3) C61 0.030(2) 0.032(2) 0.029(2) 0.0007(10) 0.0042(10) -0.0003(10) C62 0.028(5) 0.033(5) 0.014(4) -0.012(4) -0.003(4) 0.004(4) C63 0.010(4) 0.018(4) 0.020(4) 0.002(3) 0.003(4) 0.005(3) C64 0.023(5) 0.009(4) 0.016(4) -0.009(3) 0.005(4) -0.007(3) C65 0.008(4) 0.011(4) 0.019(4) 0.001(3) -0.001(3) 0.000(3) C66 0.020(5) 0.038(5) 0.020(5) -0.002(4) -0.005(4) 0.008(4) C67 0.062(8) 0.047(5) 0.019(5) -0.007(4) 0.018(5) 0.018(5) C68 0.078(8) 0.076(7) 0.025(5) 0.030(5) 0.037(6) 0.042(6) C69 0.044(6) 0.031(5) 0.059(7) 0.029(5) 0.043(6) 0.015(4) C70 0.027(5) 0.010(4) 0.034(5) 0.012(3) 0.017(4) -0.002(3) C71 0.018(5) 0.020(4) 0.017(4) -0.007(4) 0.001(4) -0.003(4) C72 0.010(4) 0.024(4) 0.010(4) 0.003(3) 0.002(3) -0.004(3) C73 0.012(4) 0.018(4) 0.030(5) 0.001(3) 0.000(4) -0.003(3) C74 0.029(6) 0.048(5) 0.022(5) 0.013(4) -0.016(4) 0.000(4) C75 0.042(7) 0.059(6) 0.016(5) -0.007(4) -0.002(4) -0.007(5) C76 0.030(6) 0.045(5) 0.022(5) -0.011(4) -0.006(4) -0.001(4) C77 0.020(5) 0.021(4) 0.023(5) -0.011(3) 0.002(4) -0.002(3) C78 0.0102(18) 0.0106(18) 0.0096(18) -0.0006(10) 0.0013(10) 0.0008(10) C79 0.024(5) 0.007(3) 0.013(4) -0.004(3) 0.000(4) 0.003(3) C80 0.017(5) 0.009(3) 0.010(4) 0.003(3) -0.005(3) -0.001(3) C81 0.027(5) 0.022(4) 0.011(4) 0.006(3) -0.004(4) -0.003(4) C82 0.035(6) 0.020(4) 0.018(5) 0.003(3) -0.008(4) -0.012(4) C83 0.013(5) 0.026(4) 0.019(5) 0.001(3) 0.004(4) 0.001(4) C84 0.006(4) 0.009(3) 0.019(4) 0.000(3) 0.004(3) 0.006(3) N1 0.021(4) 0.013(3) 0.008(3) 0.003(3) -0.003(3) 0.003(3) N2 0.005(3) 0.009(3) 0.013(3) -0.002(2) -0.004(3) 0.003(2) N3 0.015(4) 0.019(3) 0.013(3) 0.007(3) 0.003(3) -0.004(3) N4 0.009(4) 0.018(3) 0.014(3) -0.002(3) 0.002(3) -0.003(3) N5 0.008(4) 0.041(4) 0.026(4) 0.001(3) -0.001(3) -0.002(3) N6 0.013(4) 0.012(3) 0.018(3) 0.003(3) -0.004(3) 0.000(3) N7 0.013(4) 0.012(3) 0.012(3) 0.000(2) -0.007(3) -0.001(3) N8 0.018(4) 0.013(3) 0.013(3) 0.006(3) 0.004(3) 0.003(3) N9 0.011(3) 0.020(3) 0.017(3) -0.007(3) 0.001(3) 0.008(3) N10 0.013(4) 0.013(3) 0.017(3) -0.001(3) 0.005(3) -0.002(3) N11 0.018(4) 0.011(3) 0.023(4) -0.006(3) 0.005(3) 0.002(3) N12 0.020(4) 0.009(3) 0.012(3) 0.000(2) 0.003(3) 0.003(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 Nd1 O15 2.426(4) 3_665 ? Nd1 O16 2.439(4) . ? Nd1 O17 2.467(4) . ? Nd1 O18 2.479(5) 3_665 ? Nd1 O13 2.482(5) . ? Nd1 O5W 2.520(5) . ? Nd1 O14 2.540(5) . ? Nd1 O6W 2.554(4) . ? Nd1 O17 2.689(5) 3_665 ? Nd1 C43 2.858(7) . ? Nd1 C57 2.942(7) 3_665 ? Nd1 Nd1 4.0772(7) 3_665 ? Nd2 O4 2.391(4) . ? Nd2 O8 2.402(4) . ? Nd2 O6 2.468(4) . ? Nd2 O11 2.468(5) . ? Nd2 O10 2.485(5) . ? Nd2 O3W 2.500(4) . ? Nd2 O4W 2.512(4) . ? Nd2 O12 2.598(5) . ? Nd2 C36 2.893(7) . ? Nd3 O9 2.406(4) . ? Nd3 O3 2.426(4) . ? Nd3 O5 2.455(5) . ? Nd3 O7 2.457(4) . ? Nd3 O1 2.495(5) . ? Nd3 O1W 2.540(4) . ? Nd3 O2 2.548(5) . ? Nd3 O2W 2.556(4) . ? Nd3 O6 2.717(5) . ? Nd3 C1 2.875(8) . ? Nd3 C15 2.952(7) . ? Nd4 O19 2.391(4) . ? Nd4 O24 2.408(5) . ? Nd4 O22 2.418(5) . ? Nd4 O23 2.423(4) 3_775 ? Nd4 O20 2.455(5) 3_775 ? Nd4 O7W 2.485(4) . ? Nd4 O8W 2.528(4) . ? Nd4 O9W 2.627(4) . ? O1 C1 1.254(8) . ? O2 C1 1.260(7) . ? O3 C8 1.248(7) . ? O4 C8 1.255(8) . ? O5 C15 1.232(8) . ? O6 C15 1.276(7) . ? O7 C22 1.244(8) . ? O8 C22 1.264(7) . ? O9 C29 1.254(7) . ? O10 C29 1.231(8) . ? O11 C36 1.242(8) . ? O12 C36 1.263(8) . ? O13 C43 1.257(8) . ? O14 C43 1.264(7) . ? O15 C50 1.237(8) . ? O15 Nd1 2.426(4) 3_665 ? O16 C50 1.253(7) . ? O17 C57 1.281(7) . ? O17 Nd1 2.689(5) 3_665 ? O18 C57 1.232(8) . ? O18 Nd1 2.479(5) 3_665 ? O19 C64 1.254(8) . ? O20 C64 1.245(8) . ? O20 Nd4 2.455(5) 3_775 ? O21 C71 1.247(8) . ? O22 C71 1.261(8) . ? O23 C78 1.246(7) . ? O23 Nd4 2.423(4) 3_775 ? O24 C78 1.271(8) . ? C1 C2 1.545(10) . ? C2 N1 1.493(8) . ? C2 C3 1.518(8) . ? C2 C7 1.531(8) . ? C3 C4 1.514(10) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.520(9) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.518(9) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.505(9) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.533(9) . ? C9 N2 1.516(7) . ? C9 C14 1.522(8) . ? C9 C10 1.523(9) . ? C10 C11 1.514(8) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.526(9) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.515(11) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.547(9) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.539(9) . ? C16 C17 1.517(8) . ? C16 N3 1.523(8) . ? C16 C21 1.531(9) . ? C17 C18 1.522(10) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.504(10) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.528(9) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.494(9) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.519(8) . ? C23 C28 1.516(9) . ? C23 C24 1.526(9) . ? C23 N4 1.526(7) . ? C24 C25 1.544(9) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.495(11) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.510(10) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.522(8) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.531(9) . ? C30 C31 1.518(8) . ? C30 N5 1.519(8) . ? C30 C35 1.528(8) . ? C31 C32 1.510(10) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.494(9) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.481(9) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.532(9) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.530(10) . ? C37 N6 1.492(8) . ? C37 C42 1.523(8) . ? C37 C38 1.542(8) . ? C38 C39 1.493(10) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.523(10) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.510(10) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.533(10) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.536(10) . ? C44 N7 1.485(8) . ? C44 C45 1.522(8) . ? C44 C49 1.536(8) . ? C45 C46 1.528(9) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 C47 1.503(9) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C48 1.495(9) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 C49 1.521(9) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 C51 1.558(9) . ? C51 C52 1.503(9) . ? C51 N8 1.510(7) . ? C51 C56 1.523(9) . ? C52 C53 1.515(8) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C54 1.501(10) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 C55 1.531(11) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C56 1.543(9) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 C58 1.533(9) . ? C57 Nd1 2.942(7) 3_665 ? C58 N9 1.498(8) . ? C58 C63 1.523(8) . ? C58 C59 1.549(8) . ? C59 C60 1.506(9) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 C61 1.526(9) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 C62 1.524(9) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 C63 1.539(9) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 C65 1.547(9) . ? C65 N10 1.507(8) . ? C65 C70 1.527(8) . ? C65 C66 1.537(9) . ? C66 C67 1.525(10) . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? C67 C68 1.518(10) . ? C67 H67A 0.9900 . ? C67 H67B 0.9900 . ? C68 C69 1.487(11) . ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? C69 C70 1.512(9) . ? C69 H69A 0.9900 . ? C69 H69B 0.9900 . ? C70 H70A 0.9900 . ? C70 H70B 0.9900 . ? C71 C72 1.532(10) . ? C72 N11 1.505(8) . ? C72 C77 1.517(8) . ? C72 C73 1.536(9) . ? C73 C74 1.553(9) . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C74 C75 1.467(10) . ? C74 H74A 0.9900 . ? C74 H74B 0.9900 . ? C75 C76 1.527(10) . ? C75 H75A 0.9900 . ? C75 H75B 0.9900 . ? C76 C77 1.511(9) . ? C76 H76A 0.9900 . ? C76 H76B 0.9900 . ? C77 H77A 0.9900 . ? C77 H77B 0.9900 . ? C78 C79 1.523(9) . ? C79 C80 1.508(9) . ? C79 N12 1.522(7) . ? C79 C84 1.536(10) . ? C80 C81 1.529(9) . ? C80 H80A 0.9900 . ? C80 H80B 0.9900 . ? C81 C82 1.523(11) . ? C81 H81A 0.9900 . ? C81 H81B 0.9900 . ? C82 C83 1.527(9) . ? C82 H82A 0.9900 . ? C82 H82B 0.9900 . ? C83 C84 1.516(9) . ? C83 H83A 0.9900 . ? C83 H83B 0.9900 . ? C84 H84A 0.9900 . ? C84 H84B 0.9900 . ? N1 H1A 0.9100 . ? N1 H1B 0.9100 . ? N1 H1C 0.9100 . ? N2 H2A 0.9100 . ? N2 H2B 0.9100 . ? N2 H2C 0.9100 . ? N3 H3C 0.9100 . ? N3 H3D 0.9100 . ? N3 H3E 0.9100 . ? N4 H4C 0.9100 . ? N4 H4D 0.9100 . ? N4 H4E 0.9100 . ? N5 H5C 0.9100 . ? N5 H5D 0.9100 . ? N5 H5E 0.9100 . ? N6 H6C 0.9100 . ? N6 H6D 0.9100 . ? N6 H6E 0.9100 . ? N7 H7C 0.9100 . ? N7 H7D 0.9100 . ? N7 H7E 0.9100 . ? N8 H8A 0.9100 . ? N8 H8B 0.9100 . ? N8 H8C 0.9100 . ? N9 H9A 0.9100 . ? N9 H9B 0.9100 . ? N9 H9C 0.9100 . ? N10 H10C 0.9100 . ? N10 H10D 0.9100 . ? N10 H10E 0.9100 . ? N11 H11C 0.9100 . ? N11 H11D 0.9100 . ? N11 H11E 0.9100 . ? N12 H12C 0.9100 . ? N12 H12D 0.9100 . ? N12 H12E 0.9100 . ? 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 O15 Nd1 O16 135.27(15) 3_665 . ? O15 Nd1 O17 75.51(14) 3_665 . ? O16 Nd1 O17 73.14(13) . . ? O15 Nd1 O18 97.96(16) 3_665 3_665 ? O16 Nd1 O18 74.16(14) . 3_665 ? O17 Nd1 O18 123.01(15) . 3_665 ? O15 Nd1 O13 147.10(14) 3_665 . ? O16 Nd1 O13 77.59(15) . . ? O17 Nd1 O13 126.17(15) . . ? O18 Nd1 O13 89.52(15) 3_665 . ? O15 Nd1 O5W 70.36(16) 3_665 . ? O16 Nd1 O5W 142.90(15) . . ? O17 Nd1 O5W 95.00(14) . . ? O18 Nd1 O5W 136.82(13) 3_665 . ? O13 Nd1 O5W 82.27(15) . . ? O15 Nd1 O14 126.48(16) 3_665 . ? O16 Nd1 O14 75.66(15) . . ? O17 Nd1 O14 77.01(15) . . ? O18 Nd1 O14 135.44(15) 3_665 . ? O13 Nd1 O14 52.23(14) . . ? O5W Nd1 O14 67.38(14) . . ? O15 Nd1 O6W 73.03(14) 3_665 . ? O16 Nd1 O6W 134.87(14) . . ? O17 Nd1 O6W 148.24(13) . . ? O18 Nd1 O6W 66.38(14) 3_665 . ? O13 Nd1 O6W 80.99(14) . . ? O5W Nd1 O6W 70.47(15) . . ? O14 Nd1 O6W 119.33(15) . . ? O15 Nd1 O17 70.35(14) 3_665 3_665 ? O16 Nd1 O17 71.49(14) . 3_665 ? O17 Nd1 O17 75.57(16) . 3_665 ? O18 Nd1 O17 50.19(13) 3_665 3_665 ? O13 Nd1 O17 134.18(14) . 3_665 ? O5W Nd1 O17 140.71(14) . 3_665 ? O14 Nd1 O17 141.96(12) . 3_665 ? O6W Nd1 O17 97.60(14) . 3_665 ? O15 Nd1 C43 141.98(17) 3_665 . ? O16 Nd1 C43 76.28(17) . . ? O17 Nd1 C43 102.24(17) . . ? O18 Nd1 C43 113.53(17) 3_665 . ? O13 Nd1 C43 26.03(16) . . ? O5W Nd1 C43 72.08(17) . . ? O14 Nd1 C43 26.25(15) . . ? O6W Nd1 C43 99.81(17) . . ? O17 Nd1 C43 146.91(15) 3_665 . ? O15 Nd1 C57 84.33(17) 3_665 3_665 ? O16 Nd1 C57 70.77(16) . 3_665 ? O17 Nd1 C57 99.98(17) . 3_665 ? O18 Nd1 C57 24.39(15) 3_665 3_665 ? O13 Nd1 C57 111.61(17) . 3_665 ? O5W Nd1 C57 146.25(16) . 3_665 ? O14 Nd1 C57 145.56(16) . 3_665 ? O6W Nd1 C57 81.21(17) . 3_665 ? O17 Nd1 C57 25.80(15) 3_665 3_665 ? C43 Nd1 C57 132.41(19) . 3_665 ? O15 Nd1 Nd1 68.09(10) 3_665 3_665 ? O16 Nd1 Nd1 67.37(11) . 3_665 ? O17 Nd1 Nd1 39.69(11) . 3_665 ? O18 Nd1 Nd1 84.69(10) 3_665 3_665 ? O13 Nd1 Nd1 144.76(10) . 3_665 ? O5W Nd1 Nd1 124.27(10) . 3_665 ? O14 Nd1 Nd1 112.54(10) . 3_665 ? O6W Nd1 Nd1 126.99(12) . 3_665 ? O17 Nd1 Nd1 35.88(9) 3_665 3_665 ? C43 Nd1 Nd1 132.90(13) . 3_665 ? C57 Nd1 Nd1 60.74(13) 3_665 3_665 ? O4 Nd2 O8 131.39(15) . . ? O4 Nd2 O6 74.48(14) . . ? O8 Nd2 O6 72.30(14) . . ? O4 Nd2 O11 147.20(15) . . ? O8 Nd2 O11 81.41(16) . . ? O6 Nd2 O11 124.55(15) . . ? O4 Nd2 O10 92.04(16) . . ? O8 Nd2 O10 73.34(15) . . ? O6 Nd2 O10 117.25(15) . . ? O11 Nd2 O10 99.59(15) . . ? O4 Nd2 O3W 78.01(15) . . ? O8 Nd2 O3W 129.77(14) . . ? O6 Nd2 O3W 152.45(15) . . ? O11 Nd2 O3W 79.45(16) . . ? O10 Nd2 O3W 64.84(14) . . ? O4 Nd2 O4W 71.11(16) . . ? O8 Nd2 O4W 147.15(16) . . ? O6 Nd2 O4W 97.33(14) . . ? O11 Nd2 O4W 79.45(16) . . ? O10 Nd2 O4W 136.17(14) . . ? O3W Nd2 O4W 72.06(15) . . ? O4 Nd2 O12 125.06(15) . . ? O8 Nd2 O12 79.31(15) . . ? O6 Nd2 O12 76.17(15) . . ? O11 Nd2 O12 51.07(14) . . ? O10 Nd2 O12 142.85(14) . . ? O3W Nd2 O12 119.99(15) . . ? O4W Nd2 O12 67.90(14) . . ? O4 Nd2 C36 140.83(18) . . ? O8 Nd2 C36 80.42(18) . . ? O6 Nd2 C36 101.13(18) . . ? O11 Nd2 C36 25.22(16) . . ? O10 Nd2 C36 122.53(18) . . ? O3W Nd2 C36 99.18(18) . . ? O4W Nd2 C36 70.95(17) . . ? O12 Nd2 C36 25.89(15) . . ? O9 Nd3 O3 75.71(14) . . ? O9 Nd3 O5 126.85(15) . . ? O3 Nd3 O5 74.86(15) . . ? O9 Nd3 O7 75.37(14) . . ? O3 Nd3 O7 132.53(15) . . ? O5 Nd3 O7 93.89(16) . . ? O9 Nd3 O1 126.77(16) . . ? O3 Nd3 O1 81.08(15) . . ? O5 Nd3 O1 90.59(16) . . ? O7 Nd3 O1 146.02(14) . . ? O9 Nd3 O1W 145.11(14) . . ? O3 Nd3 O1W 136.80(15) . . ? O5 Nd3 O1W 67.42(14) . . ? O7 Nd3 O1W 71.74(14) . . ? O1 Nd3 O1W 79.08(15) . . ? O9 Nd3 O2 76.59(15) . . ? O3 Nd3 O2 77.73(15) . . ? O5 Nd3 O2 136.35(14) . . ? O7 Nd3 O2 129.47(15) . . ? O1 Nd3 O2 51.77(14) . . ? O1W Nd3 O2 116.66(15) . . ? O9 Nd3 O2W 83.20(14) . . ? O3 Nd3 O2W 141.20(15) . . ? O5 Nd3 O2W 142.12(14) . . ? O7 Nd3 O2W 69.85(15) . . ? O1 Nd3 O2W 86.25(15) . . ? O1W Nd3 O2W 74.93(14) . . ? O2 Nd3 O2W 65.77(14) . . ? O9 Nd3 O6 78.60(14) . . ? O3 Nd3 O6 69.01(14) . . ? O5 Nd3 O6 49.75(14) . . ? O7 Nd3 O6 68.93(14) . . ? O1 Nd3 O6 134.60(14) . . ? O1W Nd3 O6 99.79(15) . . ? O2 Nd3 O6 142.40(12) . . ? O2W Nd3 O6 137.89(14) . . ? O9 Nd3 C1 101.90(18) . . ? O3 Nd3 C1 78.40(17) . . ? O5 Nd3 C1 114.06(18) . . ? O7 Nd3 C1 144.38(17) . . ? O1 Nd3 C1 25.79(16) . . ? O1W Nd3 C1 98.09(17) . . ? O2 Nd3 C1 25.99(15) . . ? O2W Nd3 C1 74.55(16) . . ? O6 Nd3 C1 146.31(15) . . ? O9 Nd3 C15 103.50(17) . . ? O3 Nd3 C15 70.14(17) . . ? O5 Nd3 C15 24.16(15) . . ? O7 Nd3 C15 81.11(17) . . ? O1 Nd3 C15 112.48(17) . . ? O1W Nd3 C15 82.75(17) . . ? O2 Nd3 C15 146.56(15) . . ? O2W Nd3 C15 147.61(16) . . ? O6 Nd3 C15 25.59(14) . . ? C1 Nd3 C15 132.61(18) . . ? O19 Nd4 O24 77.94(15) . . ? O19 Nd4 O22 87.63(16) . . ? O24 Nd4 O22 140.69(16) . . ? O19 Nd4 O23 71.62(14) . 3_775 ? O24 Nd4 O23 120.49(15) . 3_775 ? O22 Nd4 O23 87.98(16) . 3_775 ? O19 Nd4 O20 118.89(15) . 3_775 ? O24 Nd4 O20 75.57(16) . 3_775 ? O22 Nd4 O20 141.69(15) . 3_775 ? O23 Nd4 O20 76.47(15) 3_775 3_775 ? O19 Nd4 O7W 150.54(14) . . ? O24 Nd4 O7W 129.90(15) . . ? O22 Nd4 O7W 75.35(15) . . ? O23 Nd4 O7W 83.73(14) 3_775 . ? O20 Nd4 O7W 68.38(15) 3_775 . ? O19 Nd4 O8W 135.40(15) . . ? O24 Nd4 O8W 73.69(15) . . ? O22 Nd4 O8W 93.05(15) . . ? O23 Nd4 O8W 152.98(15) 3_775 . ? O20 Nd4 O8W 86.34(15) 3_775 . ? O7W Nd4 O8W 70.49(14) . . ? O19 Nd4 O9W 71.25(14) . . ? O24 Nd4 O9W 70.37(15) . . ? O22 Nd4 O9W 70.38(15) . . ? O23 Nd4 O9W 137.39(14) 3_775 . ? O20 Nd4 O9W 141.34(14) 3_775 . ? O7W Nd4 O9W 122.73(14) . . ? O8W Nd4 O9W 67.16(13) . . ? C1 O1 Nd3 94.3(4) . . ? C1 O2 Nd3 91.6(4) . . ? C8 O3 Nd3 134.8(4) . . ? C8 O4 Nd2 140.3(4) . . ? C15 O5 Nd3 101.2(4) . . ? C15 O6 Nd2 159.7(4) . . ? C15 O6 Nd3 87.6(4) . . ? Nd2 O6 Nd3 107.19(16) . . ? C22 O7 Nd3 137.9(4) . . ? C22 O8 Nd2 139.7(4) . . ? C29 O9 Nd3 162.1(4) . . ? C29 O10 Nd2 107.1(4) . . ? C36 O11 Nd2 96.9(4) . . ? C36 O12 Nd2 90.2(4) . . ? C43 O13 Nd1 94.0(4) . . ? C43 O14 Nd1 91.1(4) . . ? C50 O15 Nd1 136.6(4) . 3_665 ? C50 O16 Nd1 135.6(4) . . ? C57 O17 Nd1 157.1(4) . . ? C57 O17 Nd1 88.2(4) . 3_665 ? Nd1 O17 Nd1 104.43(16) . 3_665 ? C57 O18 Nd1 99.4(4) . 3_665 ? C64 O19 Nd4 155.5(5) . . ? C64 O20 Nd4 124.9(4) . 3_775 ? C71 O22 Nd4 136.2(4) . . ? C78 O23 Nd4 136.8(4) . 3_775 ? C78 O24 Nd4 143.8(4) . . ? O1 C1 O2 122.3(7) . . ? O1 C1 C2 118.2(6) . . ? O2 C1 C2 119.4(6) . . ? O1 C1 Nd3 59.9(4) . . ? O2 C1 Nd3 62.4(4) . . ? C2 C1 Nd3 177.4(5) . . ? N1 C2 C3 110.6(6) . . ? N1 C2 C7 108.5(5) . . ? C3 C2 C7 111.9(5) . . ? N1 C2 C1 105.3(5) . . ? C3 C2 C1 112.3(6) . . ? C7 C2 C1 107.9(5) . . ? C4 C3 C2 112.9(6) . . ? C4 C3 H3A 109.0 . . ? C2 C3 H3A 109.0 . . ? C4 C3 H3B 109.0 . . ? C2 C3 H3B 109.0 . . ? H3A C3 H3B 107.8 . . ? C3 C4 C5 111.7(6) . . ? C3 C4 H4A 109.3 . . ? C5 C4 H4A 109.3 . . ? C3 C4 H4B 109.3 . . ? C5 C4 H4B 109.3 . . ? H4A C4 H4B 107.9 . . ? C6 C5 C4 111.1(6) . . ? C6 C5 H5A 109.4 . . ? C4 C5 H5A 109.4 . . ? C6 C5 H5B 109.4 . . ? C4 C5 H5B 109.4 . . ? H5A C5 H5B 108.0 . . ? C7 C6 C5 111.8(6) . . ? C7 C6 H6A 109.3 . . ? C5 C6 H6A 109.3 . . ? C7 C6 H6B 109.3 . . ? C5 C6 H6B 109.3 . . ? H6A C6 H6B 107.9 . . ? C6 C7 C2 112.9(6) . . ? C6 C7 H7A 109.0 . . ? C2 C7 H7A 109.0 . . ? C6 C7 H7B 109.0 . . ? C2 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? O3 C8 O4 126.7(6) . . ? O3 C8 C9 115.5(6) . . ? O4 C8 C9 117.8(5) . . ? N2 C9 C14 109.6(5) . . ? N2 C9 C10 108.5(5) . . ? C14 C9 C10 113.1(6) . . ? N2 C9 C8 107.3(5) . . ? C14 C9 C8 110.9(5) . . ? C10 C9 C8 107.2(5) . . ? C11 C10 C9 112.1(5) . . ? C11 C10 H10A 109.2 . . ? C9 C10 H10A 109.2 . . ? C11 C10 H10B 109.2 . . ? C9 C10 H10B 109.2 . . ? H10A C10 H10B 107.9 . . ? C10 C11 C12 111.7(6) . . ? C10 C11 H11A 109.3 . . ? C12 C11 H11A 109.3 . . ? C10 C11 H11B 109.3 . . ? C12 C11 H11B 109.3 . . ? H11A C11 H11B 107.9 . . ? C13 C12 C11 111.8(7) . . ? C13 C12 H12A 109.3 . . ? C11 C12 H12A 109.3 . . ? C13 C12 H12B 109.3 . . ? C11 C12 H12B 109.3 . . ? H12A C12 H12B 107.9 . . ? C12 C13 C14 112.7(6) . . ? C12 C13 H13A 109.1 . . ? C14 C13 H13A 109.1 . . ? C12 C13 H13B 109.1 . . ? C14 C13 H13B 109.1 . . ? H13A C13 H13B 107.8 . . ? C9 C14 C13 111.3(6) . . ? C9 C14 H14A 109.4 . . ? C13 C14 H14A 109.4 . . ? C9 C14 H14B 109.4 . . ? C13 C14 H14B 109.4 . . ? H14A C14 H14B 108.0 . . ? O5 C15 O6 121.5(7) . . ? O5 C15 C16 121.5(6) . . ? O6 C15 C16 117.0(6) . . ? O5 C15 Nd3 54.6(4) . . ? O6 C15 Nd3 66.8(4) . . ? C16 C15 Nd3 176.1(5) . . ? C17 C16 N3 109.7(6) . . ? C17 C16 C21 110.1(5) . . ? N3 C16 C21 108.7(5) . . ? C17 C16 C15 110.6(5) . . ? N3 C16 C15 105.1(5) . . ? C21 C16 C15 112.4(6) . . ? C16 C17 C18 109.4(6) . . ? C16 C17 H17A 109.8 . . ? C18 C17 H17A 109.8 . . ? C16 C17 H17B 109.8 . . ? C18 C17 H17B 109.8 . . ? H17A C17 H17B 108.2 . . ? C19 C18 C17 109.9(6) . . ? C19 C18 H18A 109.7 . . ? C17 C18 H18A 109.7 . . ? C19 C18 H18B 109.7 . . ? C17 C18 H18B 109.7 . . ? H18A C18 H18B 108.2 . . ? C18 C19 C20 111.2(6) . . ? C18 C19 H19A 109.4 . . ? C20 C19 H19A 109.4 . . ? C18 C19 H19B 109.4 . . ? C20 C19 H19B 109.4 . . ? H19A C19 H19B 108.0 . . ? C21 C20 C19 110.5(6) . . ? C21 C20 H20A 109.6 . . ? C19 C20 H20A 109.6 . . ? C21 C20 H20B 109.6 . . ? C19 C20 H20B 109.6 . . ? H20A C20 H20B 108.1 . . ? C20 C21 C16 114.4(6) . . ? C20 C21 H21A 108.7 . . ? C16 C21 H21A 108.7 . . ? C20 C21 H21B 108.7 . . ? C16 C21 H21B 108.7 . . ? H21A C21 H21B 107.6 . . ? O7 C22 O8 126.7(6) . . ? O7 C22 C23 118.6(6) . . ? O8 C22 C23 114.6(6) . . ? C28 C23 C22 111.4(5) . . ? C28 C23 C24 111.9(5) . . ? C22 C23 C24 109.1(5) . . ? C28 C23 N4 108.9(5) . . ? C22 C23 N4 106.4(5) . . ? C24 C23 N4 108.9(5) . . ? C23 C24 C25 113.3(6) . . ? C23 C24 H24A 108.9 . . ? C25 C24 H24A 108.9 . . ? C23 C24 H24B 108.9 . . ? C25 C24 H24B 108.9 . . ? H24A C24 H24B 107.7 . . ? C26 C25 C24 111.9(6) . . ? C26 C25 H25A 109.2 . . ? C24 C25 H25A 109.2 . . ? C26 C25 H25B 109.2 . . ? C24 C25 H25B 109.2 . . ? H25A C25 H25B 107.9 . . ? C25 C26 C27 111.9(6) . . ? C25 C26 H26A 109.2 . . ? C27 C26 H26A 109.2 . . ? C25 C26 H26B 109.2 . . ? C27 C26 H26B 109.2 . . ? H26A C26 H26B 107.9 . . ? C26 C27 C28 111.6(6) . . ? C26 C27 H27A 109.3 . . ? C28 C27 H27A 109.3 . . ? C26 C27 H27B 109.3 . . ? C28 C27 H27B 109.3 . . ? H27A C27 H27B 108.0 . . ? C23 C28 C27 112.7(6) . . ? C23 C28 H28A 109.1 . . ? C27 C28 H28A 109.1 . . ? C23 C28 H28B 109.1 . . ? C27 C28 H28B 109.1 . . ? H28A C28 H28B 107.8 . . ? O10 C29 O9 123.6(7) . . ? O10 C29 C30 117.8(6) . . ? O9 C29 C30 118.6(6) . . ? C31 C30 N5 108.8(6) . . ? C31 C30 C35 110.4(5) . . ? N5 C30 C35 106.2(5) . . ? C31 C30 C29 115.8(5) . . ? N5 C30 C29 106.9(5) . . ? C35 C30 C29 108.4(6) . . ? C32 C31 C30 114.3(6) . . ? C32 C31 H31A 108.7 . . ? C30 C31 H31A 108.7 . . ? C32 C31 H31B 108.7 . . ? C30 C31 H31B 108.7 . . ? H31A C31 H31B 107.6 . . ? C33 C32 C31 111.1(6) . . ? C33 C32 H32A 109.4 . . ? C31 C32 H32A 109.4 . . ? C33 C32 H32B 109.4 . . ? C31 C32 H32B 109.4 . . ? H32A C32 H32B 108.0 . . ? C34 C33 C32 113.3(6) . . ? C34 C33 H33A 108.9 . . ? C32 C33 H33A 108.9 . . ? C34 C33 H33B 108.9 . . ? C32 C33 H33B 108.9 . . ? H33A C33 H33B 107.7 . . ? C33 C34 C35 110.4(6) . . ? C33 C34 H34A 109.6 . . ? C35 C34 H34A 109.6 . . ? C33 C34 H34B 109.6 . . ? C35 C34 H34B 109.6 . . ? H34A C34 H34B 108.1 . . ? C30 C35 C34 112.1(5) . . ? C30 C35 H35A 109.2 . . ? C34 C35 H35A 109.2 . . ? C30 C35 H35B 109.2 . . ? C34 C35 H35B 109.2 . . ? H35A C35 H35B 107.9 . . ? O11 C36 O12 121.6(7) . . ? O11 C36 C37 117.9(6) . . ? O12 C36 C37 120.5(6) . . ? O11 C36 Nd2 57.9(4) . . ? O12 C36 Nd2 63.9(4) . . ? C37 C36 Nd2 174.2(5) . . ? N6 C37 C42 109.2(5) . . ? N6 C37 C36 106.7(5) . . ? C42 C37 C36 112.1(5) . . ? N6 C37 C38 108.5(5) . . ? C42 C37 C38 110.7(5) . . ? C36 C37 C38 109.5(6) . . ? C39 C38 C37 112.5(6) . . ? C39 C38 H38A 109.1 . . ? C37 C38 H38A 109.1 . . ? C39 C38 H38B 109.1 . . ? C37 C38 H38B 109.1 . . ? H38A C38 H38B 107.8 . . ? C38 C39 C40 113.1(6) . . ? C38 C39 H39A 109.0 . . ? C40 C39 H39A 109.0 . . ? C38 C39 H39B 109.0 . . ? C40 C39 H39B 109.0 . . ? H39A C39 H39B 107.8 . . ? C41 C40 C39 110.0(6) . . ? C41 C40 H40A 109.7 . . ? C39 C40 H40A 109.7 . . ? C41 C40 H40B 109.7 . . ? C39 C40 H40B 109.7 . . ? H40A C40 H40B 108.2 . . ? C40 C41 C42 110.9(6) . . ? C40 C41 H41A 109.5 . . ? C42 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? C42 C41 H41B 109.5 . . ? H41A C41 H41B 108.0 . . ? C37 C42 C41 113.6(6) . . ? C37 C42 H42A 108.8 . . ? C41 C42 H42A 108.8 . . ? C37 C42 H42B 108.8 . . ? C41 C42 H42B 108.8 . . ? H42A C42 H42B 107.7 . . ? O13 C43 O14 122.5(7) . . ? O13 C43 C44 117.0(6) . . ? O14 C43 C44 120.4(6) . . ? O13 C43 Nd1 60.0(4) . . ? O14 C43 Nd1 62.7(4) . . ? C44 C43 Nd1 172.8(4) . . ? N7 C44 C45 109.9(6) . . ? N7 C44 C49 108.5(5) . . ? C45 C44 C49 110.9(5) . . ? N7 C44 C43 106.9(5) . . ? C45 C44 C43 110.3(5) . . ? C49 C44 C43 110.3(6) . . ? C44 C45 C46 113.7(5) . . ? C44 C45 H45A 108.8 . . ? C46 C45 H45A 108.8 . . ? C44 C45 H45B 108.8 . . ? C46 C45 H45B 108.8 . . ? H45A C45 H45B 107.7 . . ? C47 C46 C45 109.9(6) . . ? C47 C46 H46A 109.7 . . ? C45 C46 H46A 109.7 . . ? C47 C46 H46B 109.7 . . ? C45 C46 H46B 109.7 . . ? H46A C46 H46B 108.2 . . ? C48 C47 C46 111.6(6) . . ? C48 C47 H47A 109.3 . . ? C46 C47 H47A 109.3 . . ? C48 C47 H47B 109.3 . . ? C46 C47 H47B 109.3 . . ? H47A C47 H47B 108.0 . . ? C47 C48 C49 112.1(6) . . ? C47 C48 H48A 109.2 . . ? C49 C48 H48A 109.2 . . ? C47 C48 H48B 109.2 . . ? C49 C48 H48B 109.2 . . ? H48A C48 H48B 107.9 . . ? C48 C49 C44 114.2(6) . . ? C48 C49 H49A 108.7 . . ? C44 C49 H49A 108.7 . . ? C48 C49 H49B 108.7 . . ? C44 C49 H49B 108.7 . . ? H49A C49 H49B 107.6 . . ? O15 C50 O16 128.1(6) . . ? O15 C50 C51 117.3(6) . . ? O16 C50 C51 114.6(6) . . ? C52 C51 N8 110.1(5) . . ? C52 C51 C56 112.1(6) . . ? N8 C51 C56 107.3(5) . . ? C52 C51 C50 111.3(5) . . ? N8 C51 C50 106.2(5) . . ? C56 C51 C50 109.5(5) . . ? C51 C52 C53 112.7(6) . . ? C51 C52 H52A 109.0 . . ? C53 C52 H52A 109.0 . . ? C51 C52 H52B 109.0 . . ? C53 C52 H52B 109.0 . . ? H52A C52 H52B 107.8 . . ? C54 C53 C52 111.6(6) . . ? C54 C53 H53A 109.3 . . ? C52 C53 H53A 109.3 . . ? C54 C53 H53B 109.3 . . ? C52 C53 H53B 109.3 . . ? H53A C53 H53B 108.0 . . ? C53 C54 C55 111.8(6) . . ? C53 C54 H54A 109.3 . . ? C55 C54 H54A 109.3 . . ? C53 C54 H54B 109.3 . . ? C55 C54 H54B 109.3 . . ? H54A C54 H54B 107.9 . . ? C54 C55 C56 111.4(6) . . ? C54 C55 H55A 109.3 . . ? C56 C55 H55A 109.3 . . ? C54 C55 H55B 109.3 . . ? C56 C55 H55B 109.3 . . ? H55A C55 H55B 108.0 . . ? C51 C56 C55 112.7(6) . . ? C51 C56 H56A 109.0 . . ? C55 C56 H56A 109.0 . . ? C51 C56 H56B 109.0 . . ? C55 C56 H56B 109.0 . . ? H56A C56 H56B 107.8 . . ? O18 C57 O17 122.2(7) . . ? O18 C57 C58 120.4(6) . . ? O17 C57 C58 117.4(6) . . ? O18 C57 Nd1 56.2(4) . 3_665 ? O17 C57 Nd1 66.0(4) . 3_665 ? C58 C57 Nd1 176.3(5) . 3_665 ? N9 C58 C63 108.6(5) . . ? N9 C58 C57 106.3(5) . . ? C63 C58 C57 117.1(6) . . ? N9 C58 C59 109.0(5) . . ? C63 C58 C59 109.1(5) . . ? C57 C58 C59 106.5(5) . . ? C60 C59 C58 111.3(6) . . ? C60 C59 H59A 109.4 . . ? C58 C59 H59A 109.4 . . ? C60 C59 H59B 109.4 . . ? C58 C59 H59B 109.4 . . ? H59A C59 H59B 108.0 . . ? C59 C60 C61 109.4(6) . . ? C59 C60 H60A 109.8 . . ? C61 C60 H60A 109.8 . . ? C59 C60 H60B 109.8 . . ? C61 C60 H60B 109.8 . . ? H60A C60 H60B 108.2 . . ? C62 C61 C60 110.5(6) . . ? C62 C61 H61A 109.5 . . ? C60 C61 H61A 109.5 . . ? C62 C61 H61B 109.5 . . ? C60 C61 H61B 109.5 . . ? H61A C61 H61B 108.1 . . ? C61 C62 C63 111.2(6) . . ? C61 C62 H62A 109.4 . . ? C63 C62 H62A 109.4 . . ? C61 C62 H62B 109.4 . . ? C63 C62 H62B 109.4 . . ? H62A C62 H62B 108.0 . . ? C58 C63 C62 113.5(5) . . ? C58 C63 H63A 108.9 . . ? C62 C63 H63A 108.9 . . ? C58 C63 H63B 108.9 . . ? C62 C63 H63B 108.9 . . ? H63A C63 H63B 107.7 . . ? O20 C64 O19 126.0(7) . . ? O20 C64 C65 115.9(6) . . ? O19 C64 C65 118.0(6) . . ? N10 C65 C70 108.9(6) . . ? N10 C65 C66 109.3(5) . . ? C70 C65 C66 111.2(6) . . ? N10 C65 C64 106.3(5) . . ? C70 C65 C64 113.3(5) . . ? C66 C65 C64 107.7(6) . . ? C67 C66 C65 112.4(7) . . ? C67 C66 H66A 109.1 . . ? C65 C66 H66A 109.1 . . ? C67 C66 H66B 109.1 . . ? C65 C66 H66B 109.1 . . ? H66A C66 H66B 107.9 . . ? C68 C67 C66 109.9(6) . . ? C68 C67 H67A 109.7 . . ? C66 C67 H67A 109.7 . . ? C68 C67 H67B 109.7 . . ? C66 C67 H67B 109.7 . . ? H67A C67 H67B 108.2 . . ? C69 C68 C67 111.6(7) . . ? C69 C68 H68A 109.3 . . ? C67 C68 H68A 109.3 . . ? C69 C68 H68B 109.3 . . ? C67 C68 H68B 109.3 . . ? H68A C68 H68B 108.0 . . ? C68 C69 C70 110.2(7) . . ? C68 C69 H69A 109.6 . . ? C70 C69 H69A 109.6 . . ? C68 C69 H69B 109.6 . . ? C70 C69 H69B 109.6 . . ? H69A C69 H69B 108.1 . . ? C69 C70 C65 112.5(6) . . ? C69 C70 H70A 109.1 . . ? C65 C70 H70A 109.1 . . ? C69 C70 H70B 109.1 . . ? C65 C70 H70B 109.1 . . ? H70A C70 H70B 107.8 . . ? O21 C71 O22 125.2(7) . . ? O21 C71 C72 117.8(7) . . ? O22 C71 C72 117.0(6) . . ? N11 C72 C77 107.3(5) . . ? N11 C72 C71 107.2(6) . . ? C77 C72 C71 110.5(6) . . ? N11 C72 C73 107.9(5) . . ? C77 C72 C73 110.2(6) . . ? C71 C72 C73 113.5(6) . . ? C72 C73 C74 114.3(6) . . ? C72 C73 H73A 108.7 . . ? C74 C73 H73A 108.7 . . ? C72 C73 H73B 108.7 . . ? C74 C73 H73B 108.7 . . ? H73A C73 H73B 107.6 . . ? C75 C74 C73 111.9(6) . . ? C75 C74 H74A 109.2 . . ? C73 C74 H74A 109.2 . . ? C75 C74 H74B 109.2 . . ? C73 C74 H74B 109.2 . . ? H74A C74 H74B 107.9 . . ? C74 C75 C76 112.9(7) . . ? C74 C75 H75A 109.0 . . ? C76 C75 H75A 109.0 . . ? C74 C75 H75B 109.0 . . ? C76 C75 H75B 109.0 . . ? H75A C75 H75B 107.8 . . ? C77 C76 C75 110.3(7) . . ? C77 C76 H76A 109.6 . . ? C75 C76 H76A 109.6 . . ? C77 C76 H76B 109.6 . . ? C75 C76 H76B 109.6 . . ? H76A C76 H76B 108.1 . . ? C76 C77 C72 113.4(6) . . ? C76 C77 H77A 108.9 . . ? C72 C77 H77A 108.9 . . ? C76 C77 H77B 108.9 . . ? C72 C77 H77B 108.9 . . ? H77A C77 H77B 107.7 . . ? O23 C78 O24 126.4(6) . . ? O23 C78 C79 115.8(6) . . ? O24 C78 C79 117.8(6) . . ? C80 C79 N12 108.8(5) . . ? C80 C79 C78 110.2(6) . . ? N12 C79 C78 108.1(6) . . ? C80 C79 C84 111.7(6) . . ? N12 C79 C84 108.8(5) . . ? C78 C79 C84 109.3(5) . . ? C79 C80 C81 113.8(6) . . ? C79 C80 H80A 108.8 . . ? C81 C80 H80A 108.8 . . ? C79 C80 H80B 108.8 . . ? C81 C80 H80B 108.8 . . ? H80A C80 H80B 107.7 . . ? C82 C81 C80 110.9(6) . . ? C82 C81 H81A 109.5 . . ? C80 C81 H81A 109.5 . . ? C82 C81 H81B 109.5 . . ? C80 C81 H81B 109.5 . . ? H81A C81 H81B 108.1 . . ? C81 C82 C83 111.3(7) . . ? C81 C82 H82A 109.4 . . ? C83 C82 H82A 109.4 . . ? C81 C82 H82B 109.4 . . ? C83 C82 H82B 109.4 . . ? H82A C82 H82B 108.0 . . ? C84 C83 C82 110.4(6) . . ? C84 C83 H83A 109.6 . . ? C82 C83 H83A 109.6 . . ? C84 C83 H83B 109.6 . . ? C82 C83 H83B 109.6 . . ? H83A C83 H83B 108.1 . . ? C83 C84 C79 112.3(5) . . ? C83 C84 H84A 109.1 . . ? C79 C84 H84A 109.1 . . ? C83 C84 H84B 109.1 . . ? C79 C84 H84B 109.1 . . ? H84A C84 H84B 107.9 . . ? C2 N1 H1A 109.5 . . ? C2 N1 H1B 109.5 . . ? H1A N1 H1B 109.5 . . ? C2 N1 H1C 109.5 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? C9 N2 H2A 109.5 . . ? C9 N2 H2B 109.5 . . ? H2A N2 H2B 109.5 . . ? C9 N2 H2C 109.5 . . ? H2A N2 H2C 109.5 . . ? H2B N2 H2C 109.5 . . ? C16 N3 H3C 109.5 . . ? C16 N3 H3D 109.5 . . ? H3C N3 H3D 109.5 . . ? C16 N3 H3E 109.5 . . ? H3C N3 H3E 109.5 . . ? H3D N3 H3E 109.5 . . ? C23 N4 H4C 109.5 . . ? C23 N4 H4D 109.5 . . ? H4C N4 H4D 109.5 . . ? C23 N4 H4E 109.5 . . ? H4C N4 H4E 109.5 . . ? H4D N4 H4E 109.5 . . ? C30 N5 H5C 109.5 . . ? C30 N5 H5D 109.5 . . ? H5C N5 H5D 109.5 . . ? C30 N5 H5E 109.5 . . ? H5C N5 H5E 109.5 . . ? H5D N5 H5E 109.5 . . ? C37 N6 H6C 109.5 . . ? C37 N6 H6D 109.5 . . ? H6C N6 H6D 109.5 . . ? C37 N6 H6E 109.5 . . ? H6C N6 H6E 109.5 . . ? H6D N6 H6E 109.5 . . ? C44 N7 H7C 109.5 . . ? C44 N7 H7D 109.5 . . ? H7C N7 H7D 109.5 . . ? C44 N7 H7E 109.5 . . ? H7C N7 H7E 109.5 . . ? H7D N7 H7E 109.5 . . ? C51 N8 H8A 109.5 . . ? C51 N8 H8B 109.5 . . ? H8A N8 H8B 109.5 . . ? C51 N8 H8C 109.5 . . ? H8A N8 H8C 109.5 . . ? H8B N8 H8C 109.5 . . ? C58 N9 H9A 109.5 . . ? C58 N9 H9B 109.5 . . ? H9A N9 H9B 109.5 . . ? C58 N9 H9C 109.5 . . ? H9A N9 H9C 109.5 . . ? H9B N9 H9C 109.5 . . ? C65 N10 H10C 109.5 . . ? C65 N10 H10D 109.5 . . ? H10C N10 H10D 109.5 . . ? C65 N10 H10E 109.5 . . ? H10C N10 H10E 109.5 . . ? H10D N10 H10E 109.5 . . ? C72 N11 H11C 109.5 . . ? C72 N11 H11D 109.5 . . ? H11C N11 H11D 109.5 . . ? C72 N11 H11E 109.5 . . ? H11C N11 H11E 109.5 . . ? H11D N11 H11E 109.5 . . ? C79 N12 H12C 109.5 . . ? C79 N12 H12D 109.5 . . ? H12C N12 H12D 109.5 . . ? C79 N12 H12E 109.5 . . ? H12C N12 H12E 109.5 . . ? H12D N12 H12E 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.157 _refine_diff_density_min -2.224 _refine_diff_density_rms 0.150 # Attachment '- complex2.cif' data_complex2 _database_code_depnum_ccdc_archive 'CCDC 791392' #TrackingRef '- complex2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C168 H478 Cl36 Dy12 N24 O131' _chemical_formula_weight 8157.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M pa-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' '-z, -x, -y' '-z-1/2, x-1/2, y' 'z-1/2, x, -y-1/2' 'z, -x-1/2, y-1/2' '-y, -z, -x' 'y, -z-1/2, x-1/2' '-y-1/2, z-1/2, x' 'y-1/2, z, -x-1/2' _cell_length_a 41.1341(3) _cell_length_b 41.1341(3) _cell_length_c 41.1341(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 69599.5(9) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7066 _cell_measurement_theta_min 2.7032 _cell_measurement_theta_max 28.8676 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.557 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 32848 _exptl_absorpt_coefficient_mu 2.898 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4768 _exptl_absorpt_correction_T_max 0.5311 _exptl_absorpt_process_details ? _exptl_special_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.46 (release 27-08-2009 CrysAlis171 .NET) (compiled Aug 27 2009,17:19:36) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 94564 _diffrn_reflns_av_R_equivalents 0.1661 _diffrn_reflns_av_sigmaI/netI 0.3015 _diffrn_reflns_limit_h_min -46 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -40 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -48 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.71 _diffrn_reflns_theta_max 25.00 _reflns_number_total 20402 _reflns_number_gt 7815 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. Non-hydrogen atoms were refined anisotropically, except for 35 atoms (c1 c2 c3 c4 c7 c11 c15 c21 c22 c28 c31 c33 c35 c40 c41 c49 c50 c52 c53 n2 n5 o5 o7 o21w c25 c29 c26 c14 c12 o30w c18 c46 c48 c36 o22w)were refined isotropically due to disorder ; _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^)+(0.0011P)^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 20402 _refine_ls_number_parameters 1123 _refine_ls_number_restraints 210 _refine_ls_R_factor_all 0.1547 _refine_ls_R_factor_gt 0.0585 _refine_ls_wR_factor_ref 0.0959 _refine_ls_wR_factor_gt 0.0889 _refine_ls_goodness_of_fit_ref 0.962 _refine_ls_restrained_S_all 0.957 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 0.232756(16) 1.007481(16) 0.681684(15) 0.01824(17) Uani 1 1 d . . . Dy2 Dy 0.242389(17) 1.015872(16) 0.573953(16) 0.02483(19) Uani 1 1 d . . . Dy3 Dy 0.273615(16) 1.012284(16) 0.326214(15) 0.01935(17) Uani 1 1 d . . . Dy4 Dy 0.261284(17) 1.027445(16) 0.433721(16) 0.02356(18) Uani 1 1 d . . . Cl1 Cl 0.20604(8) 0.90228(8) 0.73691(9) 0.0302(10) Uani 1 1 d . . . Cl2 Cl 0.33055(9) 1.12730(9) 0.43817(9) 0.0356(10) Uani 1 1 d . . . Cl3 Cl 0.34968(9) 1.03766(10) 0.51058(10) 0.0463(12) Uani 1 1 d . . . Cl4 Cl 0.33876(8) 1.04304(9) 0.73320(9) 0.0378(11) Uani 1 1 d . . . Cl5 Cl 0.21672(9) 1.09484(8) 0.76412(9) 0.0378(11) Uani 1 1 d . . . Cl6 Cl 0.15600(9) 1.03777(10) 0.49282(10) 0.0471(12) Uani 1 1 d . . . Cl7 Cl 0.37860(9) 1.06634(10) 0.30556(10) 0.0474(12) Uani 1 1 d . . . Cl8 Cl 0.19752(10) 1.12884(10) 0.43164(13) 0.0656(16) Uani 1 1 d . . . Cl9 Cl 0.32224(11) 0.92840(9) 0.47580(10) 0.0569(13) Uani 1 1 d . . . Cl10 Cl 0.32918(9) 0.93011(10) 0.72030(9) 0.0488(12) Uani 1 1 d . . . Cl11 Cl 0.12318(13) 0.94958(18) 0.69090(18) 0.180(4) Uani 1 1 d . . . Cl12 Cl 0.19002(15) 0.91464(12) 0.53078(13) 0.104(2) Uani 1 1 d . . . C1 C 0.2444(3) 0.9129(3) 0.6244(3) 0.022(4) Uani 1 1 d U . . C2 C 0.2100(3) 0.8971(3) 0.6298(4) 0.037(4) Uani 1 1 d U . . H2A H 0.1955 0.9030 0.6115 0.045 Uiso 1 1 calc R . . H2B H 0.2003 0.9058 0.6500 0.045 Uiso 1 1 calc R . . C3 C 0.2128(4) 0.8586(4) 0.6322(4) 0.072(6) Uani 1 1 d U . . H3A H 0.1914 0.8488 0.6370 0.087 Uiso 1 1 calc R . . H3B H 0.2213 0.8494 0.6117 0.087 Uiso 1 1 calc R . . C4 C 0.2357(5) 0.8529(4) 0.6590(4) 0.076(6) Uani 1 1 d U . . H4A H 0.2377 0.8290 0.6617 0.091 Uiso 1 1 calc R . . H4B H 0.2254 0.8613 0.6791 0.091 Uiso 1 1 calc R . . C5 C 0.2710(4) 0.8672(4) 0.6574(4) 0.083(7) Uani 1 1 d . . . H5A H 0.2825 0.8632 0.6782 0.100 Uiso 1 1 calc R . . H5B H 0.2835 0.8567 0.6397 0.100 Uiso 1 1 calc R . . C6 C 0.2680(5) 0.9045(4) 0.6510(4) 0.094(7) Uani 1 1 d . . . H6A H 0.2609 0.9153 0.6713 0.113 Uiso 1 1 calc R . . H6B H 0.2896 0.9132 0.6453 0.113 Uiso 1 1 calc R . . C7 C 0.2369(4) 0.9500(4) 0.6193(4) 0.037(4) Uani 1 1 d U . . C8 C 0.3331(4) 1.0244(4) 0.6336(3) 0.045(5) Uani 1 1 d . . . C9 C 0.3317(4) 1.0614(3) 0.6362(4) 0.048(5) Uani 1 1 d . . . H9A H 0.3154 1.0695 0.6204 0.058 Uiso 1 1 calc R . . H9B H 0.3238 1.0671 0.6582 0.058 Uiso 1 1 calc R . . C10 C 0.3626(4) 1.0787(4) 0.6303(4) 0.058(6) Uani 1 1 d . . . H10A H 0.3590 1.1024 0.6308 0.069 Uiso 1 1 calc R . . H10B H 0.3785 1.0731 0.6475 0.069 Uiso 1 1 calc R . . C11 C 0.3748(5) 1.0689(4) 0.5990(5) 0.070(6) Uani 1 1 d U . . H11A H 0.3953 1.0807 0.5946 0.084 Uiso 1 1 calc R . . H11B H 0.3589 1.0754 0.5821 0.084 Uiso 1 1 calc R . . C12 C 0.3811(4) 1.0318(4) 0.5964(4) 0.051(5) Uani 1 1 d U . . H12A H 0.3893 1.0263 0.5745 0.062 Uiso 1 1 calc R . . H12B H 0.3975 1.0250 0.6127 0.062 Uiso 1 1 calc R . . C13 C 0.3484(3) 1.0142(4) 0.6028(4) 0.038(4) Uani 1 1 d . . . H13A H 0.3333 1.0188 0.5846 0.046 Uiso 1 1 calc R . . H13B H 0.3522 0.9905 0.6034 0.046 Uiso 1 1 calc R . . C14 C 0.2979(4) 1.0102(3) 0.6368(4) 0.022(4) Uani 1 1 d U . . C15 C 0.2354(3) 1.1101(3) 0.6383(3) 0.012(3) Uani 1 1 d U . . C16 C 0.2602(3) 1.1204(3) 0.6635(3) 0.027(4) Uani 1 1 d . . . H16A H 0.2588 1.1060 0.6827 0.032 Uiso 1 1 calc R . . H16B H 0.2824 1.1186 0.6543 0.032 Uiso 1 1 calc R . . C17 C 0.2536(4) 1.1546(4) 0.6732(4) 0.048(5) Uani 1 1 d . . . H17A H 0.2692 1.1614 0.6902 0.057 Uiso 1 1 calc R . . H17B H 0.2565 1.1691 0.6542 0.057 Uiso 1 1 calc R . . C18 C 0.2204(4) 1.1576(4) 0.6855(4) 0.052(5) Uani 1 1 d U . . H18A H 0.2169 1.1805 0.6921 0.062 Uiso 1 1 calc R . . H18B H 0.2185 1.1440 0.7052 0.062 Uiso 1 1 calc R . . C19 C 0.1941(3) 1.1484(3) 0.6631(3) 0.030(4) Uani 1 1 d . . . H19A H 0.1932 1.1641 0.6448 0.036 Uiso 1 1 calc R . . H19B H 0.1730 1.1494 0.6747 0.036 Uiso 1 1 calc R . . C20 C 0.1994(3) 1.1145(3) 0.6500(4) 0.033(4) Uani 1 1 d . . . H20A H 0.1844 1.1105 0.6316 0.040 Uiso 1 1 calc R . . H20B H 0.1945 1.0984 0.6672 0.040 Uiso 1 1 calc R . . C21 C 0.2403(3) 1.0732(3) 0.6294(3) 0.022(4) Uani 1 1 d U . . C22 C 0.1406(3) 1.0082(3) 0.6165(3) 0.018(3) Uani 1 1 d U . . C23 C 0.1283(3) 1.0347(3) 0.5938(3) 0.023(4) Uani 1 1 d . . . H23A H 0.1434 1.0369 0.5752 0.027 Uiso 1 1 calc R . . H23B H 0.1282 1.0557 0.6056 0.027 Uiso 1 1 calc R . . C24 C 0.0933(3) 1.0277(4) 0.5806(4) 0.041(5) Uani 1 1 d . . . H24A H 0.0774 1.0288 0.5986 0.049 Uiso 1 1 calc R . . H24B H 0.0873 1.0442 0.5642 0.049 Uiso 1 1 calc R . . C25 C 0.0931(4) 0.9945(4) 0.5657(4) 0.048(5) Uani 1 1 d U . . H25A H 0.1082 0.9944 0.5470 0.057 Uiso 1 1 calc R . . H25B H 0.0710 0.9900 0.5573 0.057 Uiso 1 1 calc R . . C26 C 0.1028(3) 0.9670(3) 0.5890(3) 0.038(4) Uani 1 1 d U . . H26A H 0.0877 0.9662 0.6078 0.045 Uiso 1 1 calc R . . H26B H 0.1020 0.9457 0.5777 0.045 Uiso 1 1 calc R . . C27 C 0.1370(4) 0.9742(3) 0.6004(4) 0.047(5) Uani 1 1 d . . . H27A H 0.1519 0.9729 0.5815 0.057 Uiso 1 1 calc R . . H27B H 0.1436 0.9573 0.6162 0.057 Uiso 1 1 calc R . . C28 C 0.1759(3) 1.0135(3) 0.6265(4) 0.031(4) Uani 1 1 d U . . C29 C 0.1731(3) 1.0292(3) 0.3696(3) 0.024(4) Uani 1 1 d U . . C30 C 0.1749(3) 1.0645(3) 0.3628(4) 0.038(4) Uani 1 1 d . . . H30A H 0.1845 1.0672 0.3409 0.046 Uiso 1 1 calc R . . H30B H 0.1904 1.0741 0.3785 0.046 Uiso 1 1 calc R . . C31 C 0.1438(5) 1.0848(5) 0.3640(5) 0.071(6) Uani 1 1 d U . . H31A H 0.1489 1.1083 0.3630 0.086 Uiso 1 1 calc R . . H31B H 0.1293 1.0792 0.3456 0.086 Uiso 1 1 calc R . . C32 C 0.1283(4) 1.0765(4) 0.3956(6) 0.094(8) Uani 1 1 d . . . H32A H 0.1420 1.0853 0.4132 0.113 Uiso 1 1 calc R . . H32B H 0.1071 1.0879 0.3967 0.113 Uiso 1 1 calc R . . C33 C 0.1228(5) 1.0435(5) 0.4019(5) 0.078(6) Uani 1 1 d U . . H33A H 0.1069 1.0347 0.3861 0.093 Uiso 1 1 calc R . . H33B H 0.1135 1.0409 0.4240 0.093 Uiso 1 1 calc R . . C34 C 0.1553(3) 1.0238(4) 0.3995(4) 0.053(5) Uani 1 1 d . . . H34A H 0.1694 1.0298 0.4181 0.064 Uiso 1 1 calc R . . H34B H 0.1503 1.0003 0.4014 0.064 Uiso 1 1 calc R . . C35 C 0.2073(3) 1.0155(3) 0.3683(4) 0.023(4) Uani 1 1 d U . . C36 C 0.2672(3) 1.1169(3) 0.3642(3) 0.030(4) Uani 1 1 d U . . C37 C 0.3017(3) 1.1217(4) 0.3485(4) 0.037(4) Uani 1 1 d . . . H37A H 0.3183 1.1179 0.3655 0.045 Uiso 1 1 calc R . . H37B H 0.3047 1.1047 0.3316 0.045 Uiso 1 1 calc R . . C38 C 0.3079(4) 1.1536(3) 0.3336(4) 0.037(4) Uani 1 1 d . . . H38A H 0.3284 1.1532 0.3210 0.044 Uiso 1 1 calc R . . H38B H 0.3096 1.1706 0.3506 0.044 Uiso 1 1 calc R . . C39 C 0.2791(4) 1.1606(4) 0.3112(4) 0.051(5) Uani 1 1 d . . . H39A H 0.2823 1.1824 0.3015 0.062 Uiso 1 1 calc R . . H39B H 0.2796 1.1446 0.2932 0.062 Uiso 1 1 calc R . . C40 C 0.2461(3) 1.1597(3) 0.3263(3) 0.029(4) Uani 1 1 d U . . H40A H 0.2444 1.1768 0.3432 0.035 Uiso 1 1 calc R . . H40B H 0.2294 1.1640 0.3095 0.035 Uiso 1 1 calc R . . C41 C 0.2405(3) 1.1272(3) 0.3412(3) 0.022(4) Uani 1 1 d U . . H41A H 0.2386 1.1108 0.3236 0.026 Uiso 1 1 calc R . . H41B H 0.2196 1.1276 0.3531 0.026 Uiso 1 1 calc R . . C42 C 0.2619(3) 1.0806(3) 0.3732(4) 0.023(4) Uani 1 1 d . . . C43 C 0.2702(3) 0.9220(3) 0.3907(3) 0.021(4) Uani 1 1 d . . . C44 C 0.3005(4) 0.9072(3) 0.3775(4) 0.047(5) Uani 1 1 d . . . H44A H 0.3190 0.9136 0.3914 0.057 Uiso 1 1 calc R . . H44B H 0.3044 0.9159 0.3554 0.057 Uiso 1 1 calc R . . C45 C 0.2991(3) 0.8692(3) 0.3756(3) 0.038(4) Uani 1 1 d . . . H45A H 0.3188 0.8606 0.3647 0.045 Uiso 1 1 calc R . . H45B H 0.2979 0.8597 0.3977 0.045 Uiso 1 1 calc R . . C46 C 0.2692(4) 0.8604(4) 0.3563(4) 0.059(5) Uani 1 1 d U . . H46A H 0.2678 0.8364 0.3554 0.071 Uiso 1 1 calc R . . H46B H 0.2724 0.8683 0.3338 0.071 Uiso 1 1 calc R . . C47 C 0.2368(4) 0.8733(4) 0.3683(4) 0.064(6) Uani 1 1 d . . . H47A H 0.2313 0.8635 0.3896 0.077 Uiso 1 1 calc R . . H47B H 0.2193 0.8676 0.3526 0.077 Uiso 1 1 calc R . . C48 C 0.2396(4) 0.9109(4) 0.3715(4) 0.052(5) Uani 1 1 d U . . H48A H 0.2402 0.9206 0.3495 0.063 Uiso 1 1 calc R . . H48B H 0.2200 0.9192 0.3827 0.063 Uiso 1 1 calc R . . C49 C 0.2721(4) 0.9586(4) 0.3917(4) 0.030(4) Uani 1 1 d U . . C50 C 0.3632(3) 1.0127(3) 0.3920(3) 0.017(3) Uani 1 1 d U . . C51 C 0.3623(3) 0.9792(3) 0.4091(3) 0.030(4) Uani 1 1 d . . . H51A H 0.3461 0.9800 0.4269 0.035 Uiso 1 1 calc R . . H51B H 0.3549 0.9626 0.3933 0.035 Uiso 1 1 calc R . . C52 C 0.3945(3) 0.9692(3) 0.4227(4) 0.038(4) Uani 1 1 d U . . H52A H 0.3916 0.9492 0.4358 0.046 Uiso 1 1 calc R . . H52B H 0.4094 0.9639 0.4045 0.046 Uiso 1 1 calc R . . C53 C 0.4098(4) 0.9943(4) 0.4433(4) 0.061(5) Uani 1 1 d U . . H53A H 0.4318 0.9869 0.4494 0.073 Uiso 1 1 calc R . . H53B H 0.3969 0.9964 0.4636 0.073 Uiso 1 1 calc R . . C54 C 0.4127(3) 1.0286(4) 0.4274(4) 0.055(6) Uani 1 1 d . . . H54A H 0.4205 1.0444 0.4438 0.066 Uiso 1 1 calc R . . H54B H 0.4289 1.0278 0.4096 0.066 Uiso 1 1 calc R . . C55 C 0.3793(3) 1.0401(3) 0.4137(3) 0.029(4) Uani 1 1 d . . . H55A H 0.3825 1.0599 0.4004 0.035 Uiso 1 1 calc R . . H55B H 0.3646 1.0456 0.4319 0.035 Uiso 1 1 calc R . . C56 C 0.3290(4) 1.0229(3) 0.3831(4) 0.033(4) Uani 1 1 d . . . N1 N 0.2574(3) 0.9028(3) 0.5906(3) 0.060(4) Uani 1 1 d . . . H1A H 0.2770 0.9124 0.5871 0.090 Uiso 1 1 calc R . . H1B H 0.2431 0.9092 0.5750 0.090 Uiso 1 1 calc R . . H1C H 0.2597 0.8808 0.5899 0.090 Uiso 1 1 calc R . . N2 N 0.3515(2) 1.0111(3) 0.6626(2) 0.028(3) Uani 1 1 d U . . H2C H 0.3538 0.9892 0.6605 0.043 Uiso 1 1 calc R . . H2D H 0.3402 1.0156 0.6811 0.043 Uiso 1 1 calc R . . H2E H 0.3714 1.0206 0.6636 0.043 Uiso 1 1 calc R . . N3 N 0.2395(3) 1.1293(2) 0.6079(2) 0.027(3) Uani 1 1 d . . . H3C H 0.2367 1.1508 0.6123 0.040 Uiso 1 1 calc R . . H3D H 0.2244 1.1229 0.5930 0.040 Uiso 1 1 calc R . . H3E H 0.2598 1.1260 0.5997 0.040 Uiso 1 1 calc R . . N4 N 0.1198(2) 1.0083(3) 0.6460(2) 0.026(3) Uani 1 1 d . . . H4C H 0.1212 1.0281 0.6559 0.038 Uiso 1 1 calc R . . H4D H 0.1268 0.9926 0.6600 0.038 Uiso 1 1 calc R . . H4E H 0.0989 1.0043 0.6403 0.038 Uiso 1 1 calc R . . N5 N 0.1549(2) 1.0131(3) 0.3423(2) 0.027(3) Uani 1 1 d U . . H5C H 0.1340 1.0205 0.3419 0.041 Uiso 1 1 calc R . . H5D H 0.1549 0.9912 0.3453 0.041 Uiso 1 1 calc R . . H5E H 0.1647 1.0180 0.3230 0.041 Uiso 1 1 calc R . . N6 N 0.2667(3) 1.1368(2) 0.3948(2) 0.027(3) Uani 1 1 d . . . H6C H 0.2468 1.1351 0.4044 0.040 Uiso 1 1 calc R . . H6D H 0.2707 1.1580 0.3899 0.040 Uiso 1 1 calc R . . H6E H 0.2822 1.1294 0.4087 0.040 Uiso 1 1 calc R . . N7 N 0.2656(3) 0.9112(2) 0.4265(2) 0.031(3) Uani 1 1 d . . . H7A H 0.2837 0.9164 0.4382 0.046 Uiso 1 1 calc R . . H7B H 0.2623 0.8893 0.4273 0.046 Uiso 1 1 calc R . . H7C H 0.2481 0.9215 0.4352 0.046 Uiso 1 1 calc R . . N8 N 0.3824(2) 1.0092(3) 0.3620(2) 0.030(3) Uani 1 1 d . . . H8A H 0.3733 0.9936 0.3492 0.045 Uiso 1 1 calc R . . H8B H 0.4031 1.0033 0.3671 0.045 Uiso 1 1 calc R . . H8C H 0.3827 1.0284 0.3511 0.045 Uiso 1 1 calc R . . O1 O 0.2329(2) 0.9652(2) 0.6458(2) 0.032(3) Uani 1 1 d . . . O2 O 0.2377(2) 0.9617(2) 0.5919(2) 0.038(3) Uani 1 1 d . . . O3 O 0.28810(19) 1.0051(2) 0.6655(2) 0.021(2) Uani 1 1 d . . . O4 O 0.2822(2) 1.0090(2) 0.6118(2) 0.032(3) Uani 1 1 d . . . O5 O 0.24461(19) 1.0669(2) 0.5987(2) 0.022(2) Uani 1 1 d U . . O6 O 0.2402(2) 1.05282(19) 0.65148(19) 0.020(2) Uani 1 1 d . . . O7 O 0.1955(2) 1.0175(2) 0.6031(2) 0.028(3) Uani 1 1 d U . . O8 O 0.18236(19) 1.0127(2) 0.6563(2) 0.024(2) Uani 1 1 d . . . O9 O 0.2186(2) 1.0061(2) 0.3433(2) 0.026(3) Uani 1 1 d . . . O10 O 0.2217(2) 1.0176(2) 0.3958(2) 0.043(3) Uani 1 1 d . . . O11 O 0.2596(2) 1.0754(2) 0.4050(2) 0.027(2) Uani 1 1 d . . . O12 O 0.2613(2) 1.0596(2) 0.3518(2) 0.023(2) Uani 1 1 d . . . O13 O 0.2681(2) 0.9732(2) 0.4193(2) 0.027(2) Uani 1 1 d . . . O14 O 0.2779(2) 0.9722(2) 0.3648(2) 0.023(2) Uani 1 1 d . . . O15 O 0.3097(2) 1.0276(2) 0.4063(2) 0.028(3) Uani 1 1 d . . . O16 O 0.3218(2) 1.0242(2) 0.3533(2) 0.030(3) Uani 1 1 d . . . O1W O 0.2636(2) 1.0405(3) 0.7199(2) 0.048(3) Uani 1 1 d . . . O2W O 0.1967(2) 1.0423(2) 0.7135(2) 0.029(3) Uani 1 1 d . . . O3W O 0.1954(2) 0.9724(2) 0.7083(2) 0.038(3) Uani 1 1 d . . . O4W O 0.2619(2) 0.9689(2) 0.7157(2) 0.048(3) Uani 1 1 d . . . O5W O 0.2762(3) 0.9840(2) 0.5402(3) 0.083(5) Uani 1 1 d . . . O6W O 0.2123(2) 1.0529(2) 0.5406(2) 0.042(3) Uani 1 1 d . . . O7W O 0.2846(2) 1.0495(2) 0.5488(2) 0.036(3) Uani 1 1 d . . . O8W O 0.2061(3) 0.9882(3) 0.5354(2) 0.082(4) Uani 1 1 d . . . O9W O 0.3059(2) 1.0475(2) 0.2930(2) 0.024(2) Uani 1 1 d . . . O10W O 0.3158(2) 0.9796(2) 0.2997(2) 0.025(2) Uani 1 1 d . . . O11W O 0.24983(19) 0.9668(2) 0.2963(2) 0.025(2) Uani 1 1 d . . . O12W O 0.2391(2) 1.03621(19) 0.2850(2) 0.026(2) Uani 1 1 d . . . O13W O 0.2959(2) 1.0012(2) 0.4737(2) 0.031(3) Uani 1 1 d . . . O14W O 0.2900(2) 1.0680(2) 0.4645(2) 0.031(3) Uani 1 1 d . . . O15W O 0.2196(2) 1.0618(2) 0.4571(2) 0.045(3) Uani 1 1 d . . . O16W O 0.2237(2) 0.9948(2) 0.4666(2) 0.044(3) Uani 1 1 d . . . O17W O 0.2244(2) 1.0983(2) 0.2665(2) 0.052(3) Uani 1 1 d . . . O18W O 0.1759(2) 1.0183(2) 0.2753(2) 0.047(3) Uani 1 1 d . . . O19W O 0.1498(2) 0.8502(2) 0.3502(2) 0.061(6) Uani 1 3 d S . . O20W O 0.3277(2) 0.9245(2) 0.5871(2) 0.052(3) Uani 1 1 d . . . O21W O 0.4141(6) 0.9542(6) 0.5394(6) 0.108(9) Uani 0.50 1 d PU . . O22W O 0.2620(5) 0.9205(4) 0.5249(4) 0.048(6) Uani 0.50 1 d PU . . O23W O 0.1555(3) 0.9149(4) 0.4127(3) 0.114(5) Uani 1 1 d . . . O24W O 0.1483(2) 0.9370(2) 0.3544(2) 0.042(3) Uani 1 1 d . . . O25W O 0.1935(2) 0.9315(2) 0.2978(2) 0.033(3) Uani 1 1 d . . . O26W O 0.3569(3) 0.9404(2) 0.6524(2) 0.065(4) Uani 1 1 d . . . O27W O 0.2052(3) 0.9317(3) 0.4555(3) 0.107(5) Uani 1 1 d . . . O28W O 0.3066(5) 1.3066(5) 0.3066(5) 0.160(13) Uani 1 3 d S . . O29W O 0.3682(3) 1.0023(3) 0.2603(3) 0.113(5) Uani 1 1 d . . . O30W O 0.2860(3) 1.2856(3) 0.3687(3) 0.077(4) Uani 1 1 d U . . 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 0.0191(4) 0.0196(4) 0.0160(4) 0.0019(3) 0.0027(3) 0.0016(3) Dy2 0.0332(5) 0.0250(4) 0.0163(4) -0.0051(3) 0.0071(4) -0.0080(4) Dy3 0.0217(4) 0.0210(4) 0.0154(4) 0.0024(3) 0.0007(3) -0.0005(3) Dy4 0.0247(4) 0.0317(5) 0.0142(4) 0.0027(3) 0.0015(3) -0.0048(4) Cl1 0.025(2) 0.026(2) 0.039(2) -0.004(2) 0.001(2) -0.0026(18) Cl2 0.039(3) 0.040(2) 0.028(2) 0.006(2) -0.007(2) -0.004(2) Cl3 0.044(3) 0.059(3) 0.036(3) -0.022(2) 0.009(2) -0.025(2) Cl4 0.027(2) 0.046(3) 0.040(3) -0.005(2) 0.009(2) -0.014(2) Cl5 0.043(3) 0.026(2) 0.045(3) -0.007(2) -0.013(2) 0.000(2) Cl6 0.034(3) 0.050(3) 0.057(3) 0.005(2) -0.001(2) 0.001(2) Cl7 0.023(2) 0.062(3) 0.057(3) 0.032(3) 0.007(2) -0.005(2) Cl8 0.048(3) 0.032(3) 0.116(4) -0.030(3) 0.052(3) -0.013(2) Cl9 0.095(4) 0.034(3) 0.042(3) 0.000(2) -0.003(3) 0.015(3) Cl10 0.039(3) 0.059(3) 0.048(3) -0.003(2) 0.001(2) 0.013(2) Cl11 0.043(3) 0.238(8) 0.258(8) 0.227(7) 0.026(5) 0.018(4) Cl12 0.160(6) 0.060(4) 0.091(4) -0.027(3) 0.056(4) -0.067(4) C1 0.022(4) 0.022(4) 0.022(4) -0.0005(10) 0.0004(10) 0.0001(10) C2 0.037(4) 0.037(4) 0.037(4) 0.0000(10) 0.0006(10) -0.0001(10) C3 0.073(6) 0.072(6) 0.072(6) -0.0002(10) 0.0004(10) -0.0002(10) C4 0.076(6) 0.075(6) 0.076(6) 0.0000(10) 0.0002(10) 0.0002(10) C5 0.121(19) 0.045(13) 0.083(15) -0.024(11) -0.055(14) 0.063(13) C6 0.133(19) 0.052(13) 0.097(16) -0.003(12) -0.076(15) 0.032(13) C7 0.037(4) 0.037(4) 0.037(4) -0.0001(10) 0.0002(10) 0.0002(10) C8 0.057(12) 0.071(14) 0.007(9) 0.005(9) -0.001(9) 0.018(11) C9 0.048(12) 0.015(10) 0.082(14) -0.002(10) -0.022(11) 0.005(9) C10 0.036(12) 0.037(11) 0.100(17) 0.015(11) -0.018(11) -0.009(10) C11 0.070(6) 0.070(6) 0.070(6) 0.0003(10) 0.0003(10) -0.0002(10) C12 0.051(5) 0.052(5) 0.051(5) 0.0004(10) 0.0002(10) 0.0002(10) C13 0.031(10) 0.049(11) 0.035(11) -0.002(9) -0.009(8) 0.029(9) C14 0.022(4) 0.023(4) 0.023(4) -0.0001(10) -0.0002(10) 0.0002(10) C15 0.013(3) 0.012(3) 0.012(3) 0.0003(10) 0.0002(10) 0.0001(10) C16 0.030(9) 0.017(9) 0.033(9) -0.004(7) -0.024(8) -0.005(8) C17 0.039(11) 0.063(13) 0.041(11) -0.036(10) 0.002(9) -0.015(9) C18 0.052(5) 0.052(5) 0.052(5) -0.0001(10) 0.0004(10) 0.0002(10) C19 0.033(10) 0.022(10) 0.036(10) 0.009(8) 0.016(8) 0.022(8) C20 0.018(9) 0.041(11) 0.041(11) 0.013(9) 0.017(8) -0.001(8) C21 0.022(4) 0.021(4) 0.022(4) -0.0004(10) 0.0001(10) -0.0002(10) C22 0.018(4) 0.018(4) 0.018(4) 0.0000(10) 0.0005(10) -0.0006(10) C23 0.031(10) 0.013(9) 0.024(9) 0.000(7) 0.016(8) 0.001(7) C24 0.007(9) 0.074(13) 0.041(11) 0.022(10) -0.004(8) 0.008(9) C25 0.047(5) 0.048(5) 0.048(5) -0.0002(10) -0.0004(10) -0.0005(10) C26 0.037(4) 0.037(4) 0.038(4) -0.0001(10) -0.0002(10) -0.0002(10) C27 0.044(11) 0.042(11) 0.056(12) -0.005(9) -0.033(9) 0.012(9) C28 0.032(4) 0.031(4) 0.031(4) -0.0002(10) 0.0001(10) -0.0001(10) C29 0.024(4) 0.024(4) 0.024(4) -0.0003(10) 0.0000(10) 0.0001(10) C30 0.013(9) 0.048(11) 0.052(11) -0.009(9) -0.011(8) 0.009(9) C31 0.071(6) 0.071(6) 0.072(6) -0.0003(10) -0.0002(10) 0.0000(10) C32 0.025(12) 0.064(15) 0.19(3) -0.035(16) -0.018(14) -0.005(11) C33 0.078(6) 0.078(6) 0.078(6) -0.0003(10) 0.0002(10) 0.0001(10) C34 0.030(11) 0.095(15) 0.035(11) -0.021(10) -0.003(9) 0.005(11) C35 0.023(4) 0.024(4) 0.023(4) 0.0000(10) -0.0003(10) -0.0001(10) C36 0.030(4) 0.030(4) 0.029(4) -0.0001(10) 0.0000(10) 0.0001(10) C37 0.019(10) 0.061(13) 0.032(10) -0.004(9) 0.004(8) -0.007(9) C38 0.053(12) 0.024(10) 0.033(10) 0.006(8) -0.003(9) -0.007(9) C39 0.088(15) 0.015(9) 0.051(12) 0.018(9) 0.027(11) 0.012(9) C40 0.029(4) 0.029(4) 0.029(4) 0.0003(10) 0.0002(10) 0.0002(10) C41 0.022(4) 0.022(4) 0.022(4) -0.0001(10) -0.0001(10) 0.0002(10) C42 0.019(9) 0.036(11) 0.015(9) 0.010(8) -0.004(8) 0.007(8) C43 0.009(8) 0.014(9) 0.039(10) -0.002(7) 0.003(7) 0.001(7) C44 0.075(14) 0.032(11) 0.034(11) -0.001(9) 0.016(10) -0.041(10) C45 0.042(11) 0.047(12) 0.024(10) 0.008(8) 0.016(8) 0.005(9) C46 0.059(5) 0.058(5) 0.059(5) 0.0000(10) 0.0001(10) -0.0002(10) C47 0.077(15) 0.069(13) 0.046(12) 0.033(10) -0.034(11) -0.049(12) C48 0.053(5) 0.052(5) 0.052(5) 0.0004(10) 0.0000(10) -0.0001(10) C49 0.029(4) 0.030(4) 0.030(4) 0.0002(10) -0.0002(10) -0.0001(10) C50 0.017(4) 0.018(4) 0.017(4) 0.0000(10) -0.0001(10) 0.0002(10) C51 0.031(10) 0.023(9) 0.034(10) 0.006(8) -0.012(8) -0.011(8) C52 0.038(4) 0.038(4) 0.038(4) 0.0001(10) 0.0000(10) 0.0005(10) C53 0.061(6) 0.061(6) 0.061(6) 0.0004(10) -0.0001(10) 0.0004(10) C54 0.014(9) 0.090(15) 0.062(13) -0.053(12) -0.004(9) -0.007(10) C55 0.051(11) 0.022(9) 0.013(9) -0.008(7) 0.004(8) -0.003(8) C56 0.055(13) 0.024(10) 0.021(10) 0.003(8) -0.008(10) -0.008(9) N1 0.080(11) 0.018(8) 0.082(11) -0.011(7) 0.052(9) 0.005(7) N2 0.028(3) 0.029(3) 0.029(3) 0.0002(10) -0.0001(10) -0.0007(10) N3 0.043(8) 0.010(6) 0.027(7) -0.004(6) 0.003(6) 0.001(6) N4 0.033(8) 0.035(8) 0.009(6) -0.001(6) -0.003(6) -0.005(6) N5 0.027(3) 0.027(3) 0.027(3) -0.0002(10) 0.0005(10) 0.0003(10) N6 0.032(8) 0.020(7) 0.028(7) 0.005(6) -0.019(6) -0.014(6) N7 0.039(8) 0.029(7) 0.025(7) 0.002(6) 0.002(7) -0.008(6) N8 0.026(7) 0.039(8) 0.025(8) 0.015(6) 0.000(6) -0.008(7) O1 0.041(7) 0.013(6) 0.043(7) -0.010(5) 0.014(6) -0.002(5) O2 0.057(7) 0.029(6) 0.026(6) -0.006(5) 0.016(6) 0.003(6) O3 0.007(5) 0.038(6) 0.018(6) 0.012(5) -0.003(4) 0.005(5) O4 0.040(7) 0.031(6) 0.026(6) -0.003(5) 0.014(5) 0.003(5) O5 0.021(2) 0.022(2) 0.022(2) 0.0003(10) 0.0000(10) -0.0008(10) O6 0.033(6) 0.019(5) 0.010(5) -0.005(4) 0.001(5) -0.009(5) O7 0.028(3) 0.029(3) 0.029(3) 0.0001(10) 0.0002(10) -0.0007(10) O8 0.023(6) 0.028(6) 0.022(6) -0.008(5) -0.001(5) 0.006(5) O9 0.017(6) 0.050(7) 0.010(5) -0.001(5) 0.005(4) 0.010(5) O10 0.026(6) 0.069(8) 0.034(7) 0.020(6) 0.005(5) -0.013(6) O11 0.031(6) 0.019(6) 0.032(6) -0.007(5) -0.004(5) 0.010(5) O12 0.024(6) 0.030(6) 0.016(6) -0.009(5) 0.002(5) 0.004(5) O13 0.028(6) 0.034(6) 0.019(6) 0.007(5) -0.009(5) -0.007(5) O14 0.031(6) 0.018(5) 0.019(6) 0.009(5) 0.007(5) -0.013(5) O15 0.007(6) 0.028(6) 0.049(7) -0.014(6) 0.005(5) -0.003(5) O16 0.023(6) 0.042(7) 0.024(6) 0.009(5) 0.000(5) -0.006(5) O1W 0.021(6) 0.090(9) 0.033(7) -0.032(6) -0.002(5) -0.008(6) O2W 0.028(6) 0.044(7) 0.014(6) -0.007(5) 0.006(5) 0.006(5) O3W 0.033(6) 0.036(6) 0.044(7) 0.009(5) 0.003(5) 0.007(5) O4W 0.052(7) 0.057(7) 0.036(7) 0.031(6) 0.022(6) 0.023(6) O5W 0.148(12) 0.024(7) 0.076(9) -0.017(6) 0.071(9) -0.009(8) O6W 0.031(6) 0.059(8) 0.035(7) 0.013(6) -0.017(5) -0.019(6) O7W 0.051(7) 0.023(6) 0.034(6) -0.007(5) 0.007(5) -0.015(5) O8W 0.152(12) 0.075(9) 0.020(7) 0.003(7) -0.018(7) -0.036(9) O9W 0.037(6) 0.017(6) 0.017(6) 0.004(5) 0.013(5) -0.002(5) O10W 0.022(6) 0.022(6) 0.031(6) -0.010(5) 0.004(5) -0.007(5) O11W 0.014(5) 0.041(6) 0.020(6) 0.015(5) 0.005(4) 0.006(5) O12W 0.033(6) 0.016(5) 0.028(6) 0.013(5) 0.004(5) 0.007(5) O13W 0.062(7) 0.020(6) 0.012(5) 0.002(4) 0.004(5) -0.009(5) O14W 0.051(7) 0.029(6) 0.013(5) -0.003(5) -0.007(5) -0.004(5) O15W 0.045(7) 0.062(8) 0.029(6) 0.000(6) 0.014(5) 0.001(6) O16W 0.067(8) 0.050(7) 0.017(6) 0.006(5) 0.012(6) -0.030(6) O17W 0.044(7) 0.051(7) 0.062(8) -0.013(6) 0.006(6) 0.004(6) O18W 0.032(6) 0.082(8) 0.027(6) 0.014(6) 0.006(5) -0.003(6) O19W 0.061(6) 0.061(6) 0.061(6) -0.013(6) 0.013(6) 0.013(6) O20W 0.068(8) 0.047(7) 0.041(7) -0.010(6) 0.032(6) -0.018(6) O21W 0.108(9) 0.108(9) 0.108(9) -0.0002(10) -0.0003(10) -0.0003(10) O22W 0.049(6) 0.048(6) 0.048(6) 0.0000(10) 0.0002(10) -0.0001(10) O23W 0.052(9) 0.177(15) 0.114(12) 0.064(11) 0.022(8) -0.026(10) O24W 0.027(6) 0.050(7) 0.048(7) -0.042(6) 0.000(5) 0.005(6) O25W 0.032(6) 0.028(6) 0.038(6) 0.011(5) -0.002(5) -0.005(5) O26W 0.103(10) 0.040(7) 0.053(8) 0.023(6) 0.000(7) -0.002(7) O27W 0.148(13) 0.057(9) 0.117(11) -0.009(8) 0.118(10) -0.029(9) O28W 0.160(13) 0.160(13) 0.160(13) 0.104(16) 0.104(16) 0.104(16) O29W 0.150(11) 0.046(8) 0.142(14) 0.018(9) 0.103(11) 0.008(9) O30W 0.077(4) 0.076(4) 0.077(4) 0.0001(10) 0.0000(10) 0.0014(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 O6 2.261(8) . ? Dy1 O1 2.281(9) . ? Dy1 O8 2.331(8) . ? Dy1 O3W 2.374(9) . ? Dy1 O3 2.374(8) . ? Dy1 O4W 2.433(9) . ? Dy1 O1W 2.434(9) . ? Dy1 O2W 2.441(8) . ? Dy2 O7 2.274(9) . ? Dy2 O4 2.275(10) . ? Dy2 O5 2.333(8) . ? Dy2 O2 2.355(9) . ? Dy2 O5W 2.363(10) . ? Dy2 O6W 2.397(9) . ? Dy2 O7W 2.448(9) . ? Dy2 O8W 2.457(11) . ? Dy3 O12 2.268(9) . ? Dy3 O14 2.297(8) . ? Dy3 O16 2.327(9) . ? Dy3 O9 2.383(8) . ? Dy3 O9W 2.394(8) . ? Dy3 O12W 2.418(8) . ? Dy3 O11W 2.443(9) . ? Dy3 O10W 2.451(8) . ? Dy4 O15 2.290(9) . ? Dy4 O10 2.291(10) . ? Dy4 O11 2.298(9) . ? Dy4 O13 2.327(9) . ? Dy4 O14W 2.404(8) . ? Dy4 O15W 2.420(9) . ? Dy4 O13W 2.427(9) . ? Dy4 O16W 2.456(9) . ? C1 C6 1.504(18) . ? C1 N1 1.543(15) . ? C1 C2 1.571(17) . ? C1 C7 1.573(18) . ? C2 C3 1.592(19) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.47(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.57(2) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.56(2) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 O2 1.225(16) . ? C7 O1 1.268(16) . ? C8 C13 1.474(18) . ? C8 N2 1.514(16) . ? C8 C9 1.526(19) . ? C8 C14 1.57(2) . ? C9 C10 1.477(18) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.44(2) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.55(2) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.549(19) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 O4 1.218(15) . ? C14 O3 1.263(15) . ? C15 N3 1.491(14) . ? C15 C16 1.513(15) . ? C15 C20 1.566(17) . ? C15 C21 1.578(16) . ? C16 C17 1.491(17) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.460(19) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.471(18) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.514(17) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 O6 1.236(14) . ? C21 O5 1.301(14) . ? C22 N4 1.486(14) . ? C22 C23 1.524(16) . ? C22 C28 1.524(17) . ? C22 C27 1.553(17) . ? C23 C24 1.562(17) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.500(18) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.536(18) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.511(17) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 O8 1.253(15) . ? C28 O7 1.267(15) . ? C29 C34 1.450(18) . ? C29 C30 1.480(18) . ? C29 N5 1.503(15) . ? C29 C35 1.517(18) . ? C30 C31 1.528(19) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.49(2) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.40(2) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.56(2) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 O9 1.195(15) . ? C35 O10 1.279(15) . ? C36 N6 1.504(15) . ? C36 C41 1.510(16) . ? C36 C42 1.554(18) . ? C36 C37 1.572(18) . ? C37 C38 1.472(18) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.525(19) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.493(18) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.489(16) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 O12 1.237(14) . ? C42 O11 1.331(15) . ? C43 C44 1.487(18) . ? C43 C49 1.511(18) . ? C43 N7 1.552(15) . ? C43 C48 1.554(18) . ? C44 C45 1.566(18) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.506(18) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 C47 1.52(2) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C48 1.557(19) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 O14 1.262(15) . ? C49 O13 1.295(15) . ? C50 N8 1.475(14) . ? C50 C56 1.514(19) . ? C50 C51 1.544(17) . ? C50 C55 1.583(16) . ? C51 C52 1.500(17) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C53 1.478(18) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C54 1.56(2) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 C55 1.558(18) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 O15 1.255(16) . ? C56 O16 1.260(15) . ? N1 H1A 0.9100 . ? N1 H1B 0.9100 . ? N1 H1C 0.9100 . ? N2 H2C 0.9100 . ? N2 H2D 0.9100 . ? N2 H2E 0.9100 . ? N3 H3C 0.9100 . ? N3 H3D 0.9100 . ? N3 H3E 0.9100 . ? N4 H4C 0.9100 . ? N4 H4D 0.9100 . ? N4 H4E 0.9100 . ? N5 H5C 0.9100 . ? N5 H5D 0.9100 . ? N5 H5E 0.9100 . ? N6 H6C 0.9100 . ? N6 H6D 0.9100 . ? N6 H6E 0.9100 . ? N7 H7A 0.9100 . ? N7 H7B 0.9100 . ? N7 H7C 0.9100 . ? N8 H8A 0.9100 . ? N8 H8B 0.9100 . ? N8 H8C 0.9100 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Dy1 O1 105.9(3) . . ? O6 Dy1 O8 78.4(3) . . ? O1 Dy1 O8 77.4(3) . . ? O6 Dy1 O3W 147.3(3) . . ? O1 Dy1 O3W 80.5(3) . . ? O8 Dy1 O3W 71.7(3) . . ? O6 Dy1 O3 75.5(3) . . ? O1 Dy1 O3 77.6(3) . . ? O8 Dy1 O3 137.0(3) . . ? O3W Dy1 O3 136.4(3) . . ? O6 Dy1 O4W 142.0(3) . . ? O1 Dy1 O4W 82.7(3) . . ? O8 Dy1 O4W 139.1(3) . . ? O3W Dy1 O4W 70.0(3) . . ? O3 Dy1 O4W 70.2(3) . . ? O6 Dy1 O1W 79.9(3) . . ? O1 Dy1 O1W 147.4(3) . . ? O8 Dy1 O1W 134.5(3) . . ? O3W Dy1 O1W 112.2(3) . . ? O3 Dy1 O1W 72.9(3) . . ? O4W Dy1 O1W 74.7(4) . . ? O6 Dy1 O2W 83.8(3) . . ? O1 Dy1 O2W 142.6(3) . . ? O8 Dy1 O2W 69.2(3) . . ? O3W Dy1 O2W 73.5(3) . . ? O3 Dy1 O2W 139.2(3) . . ? O4W Dy1 O2W 112.0(3) . . ? O1W Dy1 O2W 69.1(3) . . ? O7 Dy2 O4 104.7(3) . . ? O7 Dy2 O5 77.1(3) . . ? O4 Dy2 O5 77.6(3) . . ? O7 Dy2 O2 78.0(3) . . ? O4 Dy2 O2 74.2(3) . . ? O5 Dy2 O2 135.8(3) . . ? O7 Dy2 O5W 145.7(3) . . ? O4 Dy2 O5W 84.8(4) . . ? O5 Dy2 O5W 137.0(3) . . ? O2 Dy2 O5W 73.0(3) . . ? O7 Dy2 O6W 81.1(3) . . ? O4 Dy2 O6W 147.4(3) . . ? O5 Dy2 O6W 72.4(3) . . ? O2 Dy2 O6W 137.6(3) . . ? O5W Dy2 O6W 108.7(4) . . ? O7 Dy2 O7W 144.0(3) . . ? O4 Dy2 O7W 81.3(3) . . ? O5 Dy2 O7W 69.4(3) . . ? O2 Dy2 O7W 136.5(3) . . ? O5W Dy2 O7W 69.3(3) . . ? O6W Dy2 O7W 76.5(3) . . ? O7 Dy2 O8W 80.7(4) . . ? O4 Dy2 O8W 145.2(4) . . ? O5 Dy2 O8W 136.2(4) . . ? O2 Dy2 O8W 73.4(4) . . ? O5W Dy2 O8W 73.8(4) . . ? O6W Dy2 O8W 67.1(4) . . ? O7W Dy2 O8W 114.8(3) . . ? O12 Dy3 O14 108.3(3) . . ? O12 Dy3 O16 77.7(3) . . ? O14 Dy3 O16 75.8(3) . . ? O12 Dy3 O9 75.1(3) . . ? O14 Dy3 O9 78.0(3) . . ? O16 Dy3 O9 133.6(3) . . ? O12 Dy3 O9W 82.5(3) . . ? O14 Dy3 O9W 141.9(3) . . ? O16 Dy3 O9W 71.0(3) . . ? O9 Dy3 O9W 139.5(3) . . ? O12 Dy3 O12W 81.0(3) . . ? O14 Dy3 O12W 145.3(3) . . ? O16 Dy3 O12W 138.6(3) . . ? O9 Dy3 O12W 72.1(3) . . ? O9W Dy3 O12W 71.3(3) . . ? O12 Dy3 O11W 143.2(3) . . ? O14 Dy3 O11W 80.1(3) . . ? O16 Dy3 O11W 138.0(3) . . ? O9 Dy3 O11W 71.7(3) . . ? O9W Dy3 O11W 113.4(3) . . ? O12W Dy3 O11W 74.0(3) . . ? O12 Dy3 O10W 146.6(3) . . ? O14 Dy3 O10W 81.9(3) . . ? O16 Dy3 O10W 74.1(3) . . ? O9 Dy3 O10W 138.1(3) . . ? O9W Dy3 O10W 71.6(3) . . ? O12W Dy3 O10W 109.0(3) . . ? O11W Dy3 O10W 68.9(3) . . ? O15 Dy4 O10 106.4(3) . . ? O15 Dy4 O11 76.7(3) . . ? O10 Dy4 O11 77.3(3) . . ? O15 Dy4 O13 76.9(3) . . ? O10 Dy4 O13 75.1(3) . . ? O11 Dy4 O13 134.1(3) . . ? O15 Dy4 O14W 80.2(3) . . ? O10 Dy4 O14W 146.2(3) . . ? O11 Dy4 O14W 72.0(3) . . ? O13 Dy4 O14W 137.8(3) . . ? O15 Dy4 O15W 144.1(3) . . ? O10 Dy4 O15W 82.6(3) . . ? O11 Dy4 O15W 71.5(3) . . ? O13 Dy4 O15W 138.3(3) . . ? O14W Dy4 O15W 74.5(3) . . ? O15 Dy4 O13W 80.0(3) . . ? O10 Dy4 O13W 143.0(3) . . ? O11 Dy4 O13W 138.4(3) . . ? O13 Dy4 O13W 71.0(3) . . ? O14W Dy4 O13W 70.4(3) . . ? O15W Dy4 O13W 113.9(3) . . ? O15 Dy4 O16W 145.2(3) . . ? O10 Dy4 O16W 80.3(3) . . ? O11 Dy4 O16W 137.1(3) . . ? O13 Dy4 O16W 72.0(3) . . ? O14W Dy4 O16W 113.5(3) . . ? O15W Dy4 O16W 69.8(3) . . ? O13W Dy4 O16W 75.7(3) . . ? C6 C1 N1 111.7(13) . . ? C6 C1 C2 112.5(13) . . ? N1 C1 C2 109.2(11) . . ? C6 C1 C7 116.4(12) . . ? N1 C1 C7 102.1(11) . . ? C2 C1 C7 104.0(11) . . ? C1 C2 C3 110.6(12) . . ? C1 C2 H2A 109.5 . . ? C3 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? C3 C2 H2B 109.5 . . ? H2A C2 H2B 108.1 . . ? C4 C3 C2 104.8(14) . . ? C4 C3 H3A 110.8 . . ? C2 C3 H3A 110.8 . . ? C4 C3 H3B 110.8 . . ? C2 C3 H3B 110.8 . . ? H3A C3 H3B 108.9 . . ? C3 C4 C5 120.2(15) . . ? C3 C4 H4A 107.3 . . ? C5 C4 H4A 107.3 . . ? C3 C4 H4B 107.3 . . ? C5 C4 H4B 107.3 . . ? H4A C4 H4B 106.9 . . ? C6 C5 C4 107.4(14) . . ? C6 C5 H5A 110.2 . . ? C4 C5 H5A 110.2 . . ? C6 C5 H5B 110.2 . . ? C4 C5 H5B 110.2 . . ? H5A C5 H5B 108.5 . . ? C1 C6 C5 113.5(14) . . ? C1 C6 H6A 108.9 . . ? C5 C6 H6A 108.9 . . ? C1 C6 H6B 108.9 . . ? C5 C6 H6B 108.9 . . ? H6A C6 H6B 107.7 . . ? O2 C7 O1 127.0(15) . . ? O2 C7 C1 119.9(14) . . ? O1 C7 C1 112.9(13) . . ? C13 C8 N2 111.2(12) . . ? C13 C8 C9 111.1(14) . . ? N2 C8 C9 108.8(12) . . ? C13 C8 C14 111.2(13) . . ? N2 C8 C14 105.0(12) . . ? C9 C8 C14 109.3(13) . . ? C10 C9 C8 115.8(14) . . ? C10 C9 H9A 108.3 . . ? C8 C9 H9A 108.3 . . ? C10 C9 H9B 108.3 . . ? C8 C9 H9B 108.3 . . ? H9A C9 H9B 107.4 . . ? C11 C10 C9 108.2(16) . . ? C11 C10 H10A 110.1 . . ? C9 C10 H10A 110.1 . . ? C11 C10 H10B 110.1 . . ? C9 C10 H10B 110.1 . . ? H10A C10 H10B 108.4 . . ? C10 C11 C12 113.1(15) . . ? C10 C11 H11A 109.0 . . ? C12 C11 H11A 109.0 . . ? C10 C11 H11B 109.0 . . ? C12 C11 H11B 109.0 . . ? H11A C11 H11B 107.8 . . ? C13 C12 C11 107.6(13) . . ? C13 C12 H12A 110.2 . . ? C11 C12 H12A 110.2 . . ? C13 C12 H12B 110.2 . . ? C11 C12 H12B 110.2 . . ? H12A C12 H12B 108.5 . . ? C8 C13 C12 112.6(14) . . ? C8 C13 H13A 109.1 . . ? C12 C13 H13A 109.1 . . ? C8 C13 H13B 109.1 . . ? C12 C13 H13B 109.1 . . ? H13A C13 H13B 107.8 . . ? O4 C14 O3 128.0(14) . . ? O4 C14 C8 115.6(13) . . ? O3 C14 C8 115.8(13) . . ? N3 C15 C16 110.5(10) . . ? N3 C15 C20 107.7(10) . . ? C16 C15 C20 113.4(11) . . ? N3 C15 C21 107.4(10) . . ? C16 C15 C21 110.0(10) . . ? C20 C15 C21 107.6(11) . . ? C17 C16 C15 108.8(11) . . ? C17 C16 H16A 109.9 . . ? C15 C16 H16A 109.9 . . ? C17 C16 H16B 109.9 . . ? C15 C16 H16B 109.9 . . ? H16A C16 H16B 108.3 . . ? C18 C17 C16 110.1(14) . . ? C18 C17 H17A 109.6 . . ? C16 C17 H17A 109.6 . . ? C18 C17 H17B 109.6 . . ? C16 C17 H17B 109.6 . . ? H17A C17 H17B 108.2 . . ? C17 C18 C19 116.8(14) . . ? C17 C18 H18A 108.1 . . ? C19 C18 H18A 108.1 . . ? C17 C18 H18B 108.1 . . ? C19 C18 H18B 108.1 . . ? H18A C18 H18B 107.3 . . ? C18 C19 C20 110.6(12) . . ? C18 C19 H19A 109.5 . . ? C20 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? C20 C19 H19B 109.5 . . ? H19A C19 H19B 108.1 . . ? C19 C20 C15 110.6(11) . . ? C19 C20 H20A 109.5 . . ? C15 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 108.1 . . ? O6 C21 O5 125.5(12) . . ? O6 C21 C15 118.7(12) . . ? O5 C21 C15 115.9(12) . . ? N4 C22 C23 107.9(10) . . ? N4 C22 C28 108.9(11) . . ? C23 C22 C28 112.3(11) . . ? N4 C22 C27 107.2(11) . . ? C23 C22 C27 110.7(11) . . ? C28 C22 C27 109.7(11) . . ? C22 C23 C24 112.7(11) . . ? C22 C23 H23A 109.1 . . ? C24 C23 H23A 109.1 . . ? C22 C23 H23B 109.1 . . ? C24 C23 H23B 109.1 . . ? H23A C23 H23B 107.8 . . ? C25 C24 C23 108.4(12) . . ? C25 C24 H24A 110.0 . . ? C23 C24 H24A 110.0 . . ? C25 C24 H24B 110.0 . . ? C23 C24 H24B 110.0 . . ? H24A C24 H24B 108.4 . . ? C24 C25 C26 114.5(13) . . ? C24 C25 H25A 108.6 . . ? C26 C25 H25A 108.6 . . ? C24 C25 H25B 108.6 . . ? C26 C25 H25B 108.6 . . ? H25A C25 H25B 107.6 . . ? C27 C26 C25 106.8(12) . . ? C27 C26 H26A 110.4 . . ? C25 C26 H26A 110.4 . . ? C27 C26 H26B 110.4 . . ? C25 C26 H26B 110.4 . . ? H26A C26 H26B 108.6 . . ? C26 C27 C22 113.5(12) . . ? C26 C27 H27A 108.9 . . ? C22 C27 H27A 108.9 . . ? C26 C27 H27B 108.9 . . ? C22 C27 H27B 108.9 . . ? H27A C27 H27B 107.7 . . ? O8 C28 O7 127.6(13) . . ? O8 C28 C22 117.7(13) . . ? O7 C28 C22 114.7(13) . . ? C34 C29 C30 109.6(13) . . ? C34 C29 N5 108.4(11) . . ? C30 C29 N5 108.4(11) . . ? C34 C29 C35 116.1(13) . . ? C30 C29 C35 108.1(12) . . ? N5 C29 C35 105.8(11) . . ? C29 C30 C31 119.2(13) . . ? C29 C30 H30A 107.5 . . ? C31 C30 H30A 107.5 . . ? C29 C30 H30B 107.5 . . ? C31 C30 H30B 107.5 . . ? H30A C30 H30B 107.0 . . ? C32 C31 C30 105.2(15) . . ? C32 C31 H31A 110.7 . . ? C30 C31 H31A 110.7 . . ? C32 C31 H31B 110.7 . . ? C30 C31 H31B 110.7 . . ? H31A C31 H31B 108.8 . . ? C33 C32 C31 117.0(18) . . ? C33 C32 H32A 108.0 . . ? C31 C32 H32A 108.0 . . ? C33 C32 H32B 108.0 . . ? C31 C32 H32B 108.0 . . ? H32A C32 H32B 107.3 . . ? C32 C33 C34 110.7(16) . . ? C32 C33 H33A 109.5 . . ? C34 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? C34 C33 H33B 109.5 . . ? H33A C33 H33B 108.1 . . ? C29 C34 C33 113.9(15) . . ? C29 C34 H34A 108.8 . . ? C33 C34 H34A 108.8 . . ? C29 C34 H34B 108.8 . . ? C33 C34 H34B 108.8 . . ? H34A C34 H34B 107.7 . . ? O9 C35 O10 127.0(14) . . ? O9 C35 C29 120.8(14) . . ? O10 C35 C29 112.1(13) . . ? N6 C36 C41 111.4(11) . . ? N6 C36 C42 108.7(11) . . ? C41 C36 C42 108.5(11) . . ? N6 C36 C37 106.8(11) . . ? C41 C36 C37 111.4(11) . . ? C42 C36 C37 110.0(12) . . ? C38 C37 C36 115.9(13) . . ? C38 C37 H37A 108.3 . . ? C36 C37 H37A 108.3 . . ? C38 C37 H37B 108.3 . . ? C36 C37 H37B 108.3 . . ? H37A C37 H37B 107.4 . . ? C37 C38 C39 106.6(13) . . ? C37 C38 H38A 110.4 . . ? C39 C38 H38A 110.4 . . ? C37 C38 H38B 110.4 . . ? C39 C38 H38B 110.4 . . ? H38A C38 H38B 108.6 . . ? C40 C39 C38 116.7(13) . . ? C40 C39 H39A 108.1 . . ? C38 C39 H39A 108.1 . . ? C40 C39 H39B 108.1 . . ? C38 C39 H39B 108.1 . . ? H39A C39 H39B 107.3 . . ? C41 C40 C39 109.5(12) . . ? C41 C40 H40A 109.8 . . ? C39 C40 H40A 109.8 . . ? C41 C40 H40B 109.8 . . ? C39 C40 H40B 109.8 . . ? H40A C40 H40B 108.2 . . ? C40 C41 C36 113.3(11) . . ? C40 C41 H41A 108.9 . . ? C36 C41 H41A 108.9 . . ? C40 C41 H41B 108.9 . . ? C36 C41 H41B 108.9 . . ? H41A C41 H41B 107.7 . . ? O12 C42 O11 125.9(13) . . ? O12 C42 C36 120.4(13) . . ? O11 C42 C36 113.7(12) . . ? C44 C43 C49 112.1(12) . . ? C44 C43 N7 109.5(11) . . ? C49 C43 N7 105.4(11) . . ? C44 C43 C48 111.8(12) . . ? C49 C43 C48 110.5(12) . . ? N7 C43 C48 107.3(10) . . ? C43 C44 C45 113.4(11) . . ? C43 C44 H44A 108.9 . . ? C45 C44 H44A 108.9 . . ? C43 C44 H44B 108.9 . . ? C45 C44 H44B 108.9 . . ? H44A C44 H44B 107.7 . . ? C46 C45 C44 107.0(13) . . ? C46 C45 H45A 110.3 . . ? C44 C45 H45A 110.3 . . ? C46 C45 H45B 110.3 . . ? C44 C45 H45B 110.3 . . ? H45A C45 H45B 108.6 . . ? C45 C46 C47 117.7(14) . . ? C45 C46 H46A 107.9 . . ? C47 C46 H46A 107.9 . . ? C45 C46 H46B 107.9 . . ? C47 C46 H46B 107.9 . . ? H46A C46 H46B 107.2 . . ? C46 C47 C48 107.9(13) . . ? C46 C47 H47A 110.1 . . ? C48 C47 H47A 110.1 . . ? C46 C47 H47B 110.1 . . ? C48 C47 H47B 110.1 . . ? H47A C47 H47B 108.4 . . ? C43 C48 C47 113.4(13) . . ? C43 C48 H48A 108.9 . . ? C47 C48 H48A 108.9 . . ? C43 C48 H48B 108.9 . . ? C47 C48 H48B 108.9 . . ? H48A C48 H48B 107.7 . . ? O14 C49 O13 126.2(14) . . ? O14 C49 C43 115.2(13) . . ? O13 C49 C43 118.6(13) . . ? N8 C50 C56 108.8(11) . . ? N8 C50 C51 107.9(11) . . ? C56 C50 C51 109.5(11) . . ? N8 C50 C55 108.4(11) . . ? C56 C50 C55 109.1(11) . . ? C51 C50 C55 113.0(11) . . ? C52 C51 C50 113.2(11) . . ? C52 C51 H51A 108.9 . . ? C50 C51 H51A 108.9 . . ? C52 C51 H51B 108.9 . . ? C50 C51 H51B 108.9 . . ? H51A C51 H51B 107.8 . . ? C53 C52 C51 113.4(13) . . ? C53 C52 H52A 108.9 . . ? C51 C52 H52A 108.9 . . ? C53 C52 H52B 108.9 . . ? C51 C52 H52B 108.9 . . ? H52A C52 H52B 107.7 . . ? C52 C53 C54 115.2(14) . . ? C52 C53 H53A 108.5 . . ? C54 C53 H53A 108.5 . . ? C52 C53 H53B 108.5 . . ? C54 C53 H53B 108.5 . . ? H53A C53 H53B 107.5 . . ? C55 C54 C53 111.0(13) . . ? C55 C54 H54A 109.4 . . ? C53 C54 H54A 109.4 . . ? C55 C54 H54B 109.4 . . ? C53 C54 H54B 109.4 . . ? H54A C54 H54B 108.0 . . ? C54 C55 C50 110.9(11) . . ? C54 C55 H55A 109.5 . . ? C50 C55 H55A 109.5 . . ? C54 C55 H55B 109.5 . . ? C50 C55 H55B 109.5 . . ? H55A C55 H55B 108.0 . . ? O15 C56 O16 125.6(15) . . ? O15 C56 C50 116.5(13) . . ? O16 C56 C50 117.7(14) . . ? C1 N1 H1A 109.5 . . ? C1 N1 H1B 109.5 . . ? H1A N1 H1B 109.5 . . ? C1 N1 H1C 109.5 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? C8 N2 H2C 109.5 . . ? C8 N2 H2D 109.5 . . ? H2C N2 H2D 109.5 . . ? C8 N2 H2E 109.5 . . ? H2C N2 H2E 109.5 . . ? H2D N2 H2E 109.5 . . ? C15 N3 H3C 109.5 . . ? C15 N3 H3D 109.5 . . ? H3C N3 H3D 109.5 . . ? C15 N3 H3E 109.5 . . ? H3C N3 H3E 109.5 . . ? H3D N3 H3E 109.5 . . ? C22 N4 H4C 109.5 . . ? C22 N4 H4D 109.5 . . ? H4C N4 H4D 109.5 . . ? C22 N4 H4E 109.5 . . ? H4C N4 H4E 109.5 . . ? H4D N4 H4E 109.5 . . ? C29 N5 H5C 109.5 . . ? C29 N5 H5D 109.5 . . ? H5C N5 H5D 109.5 . . ? C29 N5 H5E 109.5 . . ? H5C N5 H5E 109.5 . . ? H5D N5 H5E 109.5 . . ? C36 N6 H6C 109.5 . . ? C36 N6 H6D 109.5 . . ? H6C N6 H6D 109.5 . . ? C36 N6 H6E 109.5 . . ? H6C N6 H6E 109.5 . . ? H6D N6 H6E 109.5 . . ? C43 N7 H7A 109.5 . . ? C43 N7 H7B 109.5 . . ? H7A N7 H7B 109.5 . . ? C43 N7 H7C 109.5 . . ? H7A N7 H7C 109.5 . . ? H7B N7 H7C 109.5 . . ? C50 N8 H8A 109.5 . . ? C50 N8 H8B 109.5 . . ? H8A N8 H8B 109.5 . . ? C50 N8 H8C 109.5 . . ? H8A N8 H8C 109.5 . . ? H8B N8 H8C 109.5 . . ? C7 O1 Dy1 158.8(10) . . ? C7 O2 Dy2 131.4(10) . . ? C14 O3 Dy1 124.1(9) . . ? C14 O4 Dy2 162.8(10) . . ? C21 O5 Dy2 126.6(8) . . ? C21 O6 Dy1 164.4(9) . . ? C28 O7 Dy2 159.7(9) . . ? C28 O8 Dy1 129.0(9) . . ? C35 O9 Dy3 126.1(9) . . ? C35 O10 Dy4 160.6(9) . . ? C42 O11 Dy4 130.0(8) . . ? C42 O12 Dy3 157.9(9) . . ? C49 O13 Dy4 133.0(9) . . ? C49 O14 Dy3 155.4(9) . . ? C56 O15 Dy4 157.5(9) . . ? C56 O16 Dy3 131.1(10) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.028 _refine_diff_density_min -2.162 _refine_diff_density_rms 0.160 # Attachment '- complex3.cif' data_complex3 _database_code_depnum_ccdc_archive 'CCDC 791393' #TrackingRef '- complex3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C70 H150 Cl9 La3 N10 O66' _chemical_formula_weight 2923.78 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' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M p2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.5606(3) _cell_length_b 27.2041(5) _cell_length_c 29.0262(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.814(2) _cell_angle_gamma 90.00 _cell_volume 11496.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 27746 _cell_measurement_theta_min 2.8883 _cell_measurement_theta_max 32.5647 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.689 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5968 _exptl_absorpt_coefficient_mu 1.411 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6381 _exptl_absorpt_correction_T_max 0.6770 _exptl_absorpt_process_details ? _exptl_special_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.46 (release 27-08-2009 CrysAlis171 .NET) (compiled Aug 27 2009,17:19:36) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 63518 _diffrn_reflns_av_R_equivalents 0.0409 _diffrn_reflns_av_sigmaI/netI 0.0627 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.90 _diffrn_reflns_theta_max 25.00 _reflns_number_total 20236 _reflns_number_gt 14666 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. Non-hydrogen atoms were refined anisotropically, except for o48 was refined isotropically due to disorder ; _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^)+(0.0356P)^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 20236 _refine_ls_number_parameters 1423 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0575 _refine_ls_R_factor_gt 0.0374 _refine_ls_wR_factor_ref 0.0846 _refine_ls_wR_factor_gt 0.0820 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.081 _refine_ls_shift/su_max 0.030 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group La1 La 0.285896(19) 0.429374(9) 0.392058(8) 0.01518(7) Uani 1 1 d . . . La2 La 0.298881(19) 0.567135(9) 0.097867(8) 0.01309(7) Uani 1 1 d . . . La3 La 0.278023(18) 0.496124(8) 0.247993(8) 0.01032(6) Uani 1 1 d . . . Cl1 Cl -0.01050(10) 0.75393(4) 0.64060(4) 0.0290(3) Uani 1 1 d . . . Cl2 Cl 0.16484(9) 0.44433(4) 0.56829(4) 0.0268(3) Uani 1 1 d . . . Cl3 Cl 0.10429(10) 1.01691(4) 0.43699(4) 0.0292(3) Uani 1 1 d . . . Cl4 Cl 0.00700(10) 0.66088(4) 0.01208(4) 0.0309(3) Uani 1 1 d . . . Cl5 Cl 0.62146(11) 0.87601(5) 0.47076(4) 0.0351(3) Uani 1 1 d . . . Cl6 Cl 0.40391(10) 0.66534(5) 0.66824(5) 0.0339(3) Uani 1 1 d . . . Cl7 Cl 0.34912(10) 0.15493(5) 0.34395(5) 0.0327(3) Uani 1 1 d . . . Cl8 Cl 0.44556(12) 0.59733(6) 0.47591(5) 0.0502(4) Uani 1 1 d . . . Cl9 Cl 0.13360(9) 0.63007(4) 0.53978(4) 0.0235(3) Uani 1 1 d . . . C1 C 0.2289(4) 0.31065(19) 0.42156(18) 0.0279(12) Uani 1 1 d . . . C2 C 0.2259(4) 0.28352(16) 0.46867(16) 0.0233(11) Uani 1 1 d . . . C3 C 0.3115(4) 0.2978(2) 0.49582(17) 0.0370(14) Uani 1 1 d . . . H3A H 0.3165 0.3341 0.4963 0.044 Uiso 1 1 calc R . . H3B H 0.3660 0.2848 0.4798 0.044 Uiso 1 1 calc R . . C4 C 0.3127(5) 0.2788(2) 0.5456(2) 0.0510(18) Uani 1 1 d . . . H4A H 0.3204 0.2426 0.5454 0.061 Uiso 1 1 calc R . . H4B H 0.3658 0.2932 0.5625 0.061 Uiso 1 1 calc R . . C5 C 0.2257(5) 0.2917(2) 0.56999(18) 0.0492(18) Uani 1 1 d . . . H5A H 0.2217 0.3279 0.5735 0.059 Uiso 1 1 calc R . . H5B H 0.2268 0.2770 0.6012 0.059 Uiso 1 1 calc R . . C6 C 0.1422(4) 0.2732(2) 0.54342(17) 0.0407(15) Uani 1 1 d . . . H6A H 0.1442 0.2369 0.5417 0.049 Uiso 1 1 calc R . . H6B H 0.0858 0.2827 0.5599 0.049 Uiso 1 1 calc R . . C7 C 0.1391(4) 0.29430(18) 0.49533(16) 0.0299(13) Uani 1 1 d . . . H7A H 0.1305 0.3303 0.4972 0.036 Uiso 1 1 calc R . . H7B H 0.0857 0.2804 0.4784 0.036 Uiso 1 1 calc R . . C8 C 0.1099(3) 0.43318(16) 0.30227(15) 0.0174(10) Uani 1 1 d . . . C9 C 0.0122(3) 0.41726(15) 0.31465(14) 0.0151(10) Uani 1 1 d . . . C10 C -0.0442(3) 0.46344(16) 0.32623(16) 0.0215(11) Uani 1 1 d . . . H10A H -0.0182 0.4789 0.3544 0.026 Uiso 1 1 calc R . . H10B H -0.0389 0.4874 0.3007 0.026 Uiso 1 1 calc R . . C11 C -0.1451(4) 0.45204(18) 0.33376(17) 0.0298(12) Uani 1 1 d . . . H11A H -0.1512 0.4325 0.3623 0.036 Uiso 1 1 calc R . . H11B H -0.1791 0.4832 0.3379 0.036 Uiso 1 1 calc R . . C12 C -0.1870(4) 0.42384(18) 0.29391(17) 0.0307(13) Uani 1 1 d . . . H12A H -0.1865 0.4445 0.2659 0.037 Uiso 1 1 calc R . . H12B H -0.2517 0.4158 0.3008 0.037 Uiso 1 1 calc R . . C13 C -0.1342(4) 0.37666(18) 0.28515(16) 0.0280(12) Uani 1 1 d . . . H13A H -0.1616 0.3593 0.2583 0.034 Uiso 1 1 calc R . . H13B H -0.1387 0.3548 0.3123 0.034 Uiso 1 1 calc R . . C14 C -0.0334(3) 0.38796(16) 0.27588(14) 0.0199(11) Uani 1 1 d . . . H14A H 0.0003 0.3567 0.2718 0.024 Uiso 1 1 calc R . . H14B H -0.0291 0.4068 0.2468 0.024 Uiso 1 1 calc R . . C15 C 0.3310(3) 0.37503(15) 0.28795(15) 0.0163(10) Uani 1 1 d . . . C16 C 0.3179(3) 0.32140(15) 0.27141(14) 0.0162(10) Uani 1 1 d . . . C17 C 0.2155(3) 0.31232(16) 0.26224(16) 0.0230(11) Uani 1 1 d . . . H17A H 0.1818 0.3164 0.2914 0.028 Uiso 1 1 calc R . . H17B H 0.1922 0.3372 0.2401 0.028 Uiso 1 1 calc R . . C18 C 0.1964(4) 0.26113(18) 0.24290(19) 0.0387(15) Uani 1 1 d . . . H18A H 0.2094 0.2363 0.2671 0.046 Uiso 1 1 calc R . . H18B H 0.1307 0.2585 0.2341 0.046 Uiso 1 1 calc R . . C19 C 0.2547(5) 0.25027(18) 0.20108(18) 0.0416(17) Uani 1 1 d . . . H19A H 0.2343 0.2716 0.1752 0.050 Uiso 1 1 calc R . . H19B H 0.2449 0.2157 0.1916 0.050 Uiso 1 1 calc R . . C20 C 0.3575(4) 0.25868(17) 0.21024(17) 0.0336(14) Uani 1 1 d . . . H20A H 0.3805 0.2340 0.2326 0.040 Uiso 1 1 calc R . . H20B H 0.3914 0.2543 0.1812 0.040 Uiso 1 1 calc R . . C21 C 0.3756(4) 0.31019(16) 0.22922(15) 0.0241(12) Uani 1 1 d . . . H21A H 0.4415 0.3133 0.2376 0.029 Uiso 1 1 calc R . . H21B H 0.3616 0.3347 0.2049 0.029 Uiso 1 1 calc R . . C22 C 0.4402(3) 0.49860(15) 0.34933(14) 0.0160(10) Uani 1 1 d . . . C23 C 0.5233(3) 0.53248(16) 0.34545(14) 0.0152(10) Uani 1 1 d . . . C24 C 0.5817(3) 0.51760(17) 0.30456(16) 0.0235(11) Uani 1 1 d . . . H24A H 0.5419 0.5154 0.2767 0.028 Uiso 1 1 calc R . . H24B H 0.6080 0.4846 0.3104 0.028 Uiso 1 1 calc R . . C25 C 0.6599(4) 0.55370(19) 0.2954(2) 0.0385(14) Uani 1 1 d . . . H25A H 0.7053 0.5522 0.3211 0.046 Uiso 1 1 calc R . . H25B H 0.6915 0.5441 0.2668 0.046 Uiso 1 1 calc R . . C26 C 0.6239(4) 0.60597(19) 0.2906(2) 0.0412(15) Uani 1 1 d . . . H26A H 0.5837 0.6082 0.2629 0.049 Uiso 1 1 calc R . . H26B H 0.6762 0.6287 0.2865 0.049 Uiso 1 1 calc R . . C27 C 0.5702(4) 0.62136(18) 0.33279(18) 0.0305(13) Uani 1 1 d . . . H27A H 0.5455 0.6549 0.3281 0.037 Uiso 1 1 calc R . . H27B H 0.6117 0.6220 0.3601 0.037 Uiso 1 1 calc R . . C28 C 0.4914(3) 0.58591(16) 0.34132(16) 0.0211(11) Uani 1 1 d . . . H28A H 0.4461 0.5886 0.3157 0.025 Uiso 1 1 calc R . . H28B H 0.4602 0.5955 0.3700 0.025 Uiso 1 1 calc R . . C29 C 0.2076(3) 0.54794(16) 0.35567(15) 0.0168(10) Uani 1 1 d . . . C30 C 0.1745(3) 0.59648(15) 0.37726(14) 0.0170(10) Uani 1 1 d . . . C31 C 0.0717(4) 0.60247(17) 0.36813(15) 0.0241(12) Uani 1 1 d . . . H31A H 0.0598 0.6001 0.3345 0.029 Uiso 1 1 calc R . . H31B H 0.0389 0.5750 0.3831 0.029 Uiso 1 1 calc R . . C32 C 0.0329(4) 0.65063(19) 0.38545(19) 0.0432(16) Uani 1 1 d . . . H32A H 0.0330 0.6504 0.4196 0.052 Uiso 1 1 calc R . . H32B H -0.0314 0.6542 0.3745 0.052 Uiso 1 1 calc R . . C33 C 0.0896(5) 0.6943(2) 0.3685(2) 0.056(2) Uani 1 1 d . . . H33A H 0.0805 0.6979 0.3348 0.067 Uiso 1 1 calc R . . H33B H 0.0673 0.7248 0.3833 0.067 Uiso 1 1 calc R . . C34 C 0.1910(5) 0.68834(18) 0.37902(18) 0.0438(17) Uani 1 1 d . . . H34A H 0.2011 0.6892 0.4128 0.053 Uiso 1 1 calc R . . H34B H 0.2249 0.7162 0.3655 0.053 Uiso 1 1 calc R . . C35 C 0.2287(4) 0.64060(16) 0.36013(15) 0.0248(12) Uani 1 1 d . . . H35A H 0.2939 0.6371 0.3697 0.030 Uiso 1 1 calc R . . H35B H 0.2259 0.6415 0.3260 0.030 Uiso 1 1 calc R . . C36 C 0.3501(3) 0.61014(16) 0.21307(15) 0.0169(10) Uani 1 1 d . . . C37 C 0.3500(3) 0.66599(15) 0.21886(14) 0.0160(10) Uani 1 1 d . . . C38 C 0.2496(3) 0.68182(16) 0.22004(16) 0.0220(11) Uani 1 1 d . . . H38A H 0.2181 0.6628 0.2442 0.026 Uiso 1 1 calc R . . H38B H 0.2200 0.6737 0.1901 0.026 Uiso 1 1 calc R . . C39 C 0.2368(4) 0.73655(17) 0.22949(17) 0.0306(13) Uani 1 1 d . . . H39A H 0.2593 0.7557 0.2029 0.037 Uiso 1 1 calc R . . H39B H 0.1706 0.7437 0.2330 0.037 Uiso 1 1 calc R . . C40 C 0.2880(4) 0.75200(18) 0.27235(18) 0.0375(15) Uani 1 1 d . . . H40A H 0.2590 0.7366 0.2994 0.045 Uiso 1 1 calc R . . H40B H 0.2830 0.7881 0.2759 0.045 Uiso 1 1 calc R . . C41 C 0.3884(4) 0.73780(16) 0.27148(17) 0.0294(13) Uani 1 1 d . . . H41A H 0.4196 0.7574 0.2476 0.035 Uiso 1 1 calc R . . H41B H 0.4174 0.7459 0.3016 0.035 Uiso 1 1 calc R . . C42 C 0.4022(3) 0.68370(15) 0.26167(14) 0.0200(11) Uani 1 1 d . . . H42A H 0.3819 0.6644 0.2886 0.024 Uiso 1 1 calc R . . H42B H 0.4686 0.6774 0.2576 0.024 Uiso 1 1 calc R . . C43 C 0.4469(3) 0.48635(15) 0.16120(15) 0.0174(10) Uani 1 1 d . . . C44 C 0.5330(3) 0.45577(15) 0.15193(14) 0.0155(10) Uani 1 1 d . . . C45 C 0.5162(4) 0.40211(16) 0.16565(17) 0.0239(12) Uani 1 1 d . . . H45A H 0.4972 0.4009 0.1982 0.029 Uiso 1 1 calc R . . H45B H 0.4654 0.3886 0.1465 0.029 Uiso 1 1 calc R . . C46 C 0.6018(4) 0.37011(18) 0.15966(19) 0.0362(14) Uani 1 1 d . . . H46A H 0.5896 0.3368 0.1719 0.043 Uiso 1 1 calc R . . H46B H 0.6150 0.3669 0.1264 0.043 Uiso 1 1 calc R . . C47 C 0.6851(4) 0.3918(2) 0.18445(18) 0.0375(14) Uani 1 1 d . . . H47A H 0.6755 0.3901 0.2181 0.045 Uiso 1 1 calc R . . H47B H 0.7398 0.3717 0.1773 0.045 Uiso 1 1 calc R . . C48 C 0.7034(4) 0.44489(19) 0.17096(17) 0.0315(13) Uani 1 1 d . . . H48A H 0.7223 0.4463 0.1384 0.038 Uiso 1 1 calc R . . H48B H 0.7542 0.4582 0.1902 0.038 Uiso 1 1 calc R . . C49 C 0.6168(3) 0.47649(17) 0.17739(15) 0.0226(11) Uani 1 1 d . . . H49A H 0.6034 0.4787 0.2107 0.027 Uiso 1 1 calc R . . H49B H 0.6290 0.5102 0.1661 0.027 Uiso 1 1 calc R . . C50 C 0.1994(3) 0.45605(16) 0.13487(15) 0.0178(11) Uani 1 1 d . . . C51 C 0.1293(3) 0.41637(15) 0.12173(14) 0.0158(10) Uani 1 1 d . . . C52 C 0.0413(3) 0.42576(16) 0.14894(16) 0.0220(11) Uani 1 1 d . . . H52A H 0.0579 0.4291 0.1820 0.026 Uiso 1 1 calc R . . H52B H 0.0145 0.4574 0.1387 0.026 Uiso 1 1 calc R . . C53 C -0.0312(4) 0.38626(18) 0.14394(18) 0.0306(13) Uani 1 1 d . . . H53A H -0.0566 0.3867 0.1121 0.037 Uiso 1 1 calc R . . H53B H -0.0820 0.3932 0.1653 0.037 Uiso 1 1 calc R . . C54 C 0.0082(4) 0.33572(19) 0.15427(18) 0.0391(15) Uani 1 1 d . . . H54A H 0.0281 0.3340 0.1870 0.047 Uiso 1 1 calc R . . H54B H -0.0398 0.3104 0.1490 0.047 Uiso 1 1 calc R . . C55 C 0.0889(4) 0.32558(16) 0.12366(17) 0.0318(14) Uani 1 1 d . . . H55A H 0.0677 0.3250 0.0911 0.038 Uiso 1 1 calc R . . H55B H 0.1145 0.2928 0.1312 0.038 Uiso 1 1 calc R . . C56 C 0.1649(4) 0.36459(15) 0.12951(16) 0.0243(12) Uani 1 1 d . . . H56A H 0.1916 0.3622 0.1610 0.029 Uiso 1 1 calc R . . H56B H 0.2144 0.3578 0.1074 0.029 Uiso 1 1 calc R . . C57 C 0.1219(3) 0.57315(15) 0.17698(15) 0.0155(10) Uani 1 1 d . . . C58 C 0.0241(3) 0.58920(15) 0.18914(14) 0.0155(10) Uani 1 1 d . . . C59 C -0.0348(3) 0.54505(16) 0.20364(16) 0.0220(11) Uani 1 1 d . . . H59A H -0.0457 0.5238 0.1765 0.026 Uiso 1 1 calc R . . H59B H -0.0001 0.5256 0.2268 0.026 Uiso 1 1 calc R . . C60 C -0.1270(4) 0.55927(18) 0.22366(18) 0.0306(13) Uani 1 1 d . . . H60A H -0.1589 0.5294 0.2345 0.037 Uiso 1 1 calc R . . H60B H -0.1658 0.5747 0.1994 0.037 Uiso 1 1 calc R . . C61 C -0.1142(4) 0.59501(19) 0.26365(18) 0.0359(14) Uani 1 1 d . . . H61A H -0.0787 0.5790 0.2888 0.043 Uiso 1 1 calc R . . H61B H -0.1749 0.6045 0.2758 0.043 Uiso 1 1 calc R . . C62 C -0.0632(4) 0.64074(17) 0.24713(17) 0.0288(12) Uani 1 1 d . . . H62A H -0.1006 0.6576 0.2232 0.035 Uiso 1 1 calc R . . H62B H -0.0545 0.6637 0.2733 0.035 Uiso 1 1 calc R . . C63 C 0.0294(3) 0.62765(16) 0.22763(15) 0.0208(11) Uani 1 1 d . . . H63A H 0.0693 0.6150 0.2528 0.025 Uiso 1 1 calc R . . H63B H 0.0582 0.6578 0.2155 0.025 Uiso 1 1 calc R . . C64 C 0.2871(3) 0.67016(16) 0.05728(15) 0.0177(10) Uani 1 1 d . . . C65 C 0.2723(4) 0.72248(16) 0.03856(16) 0.0226(11) Uani 1 1 d . . . C66 C 0.2621(5) 0.7253(2) -0.01389(17) 0.0437(17) Uani 1 1 d . . . H66A H 0.2363 0.7578 -0.0226 0.052 Uiso 1 1 calc R . . H66B H 0.2185 0.6997 -0.0246 0.052 Uiso 1 1 calc R . . C67 C 0.3543(6) 0.7181(2) -0.0379(2) 0.067(2) Uani 1 1 d . . . H67A H 0.3733 0.6833 -0.0347 0.081 Uiso 1 1 calc R . . H67B H 0.3462 0.7252 -0.0711 0.081 Uiso 1 1 calc R . . C68 C 0.4291(7) 0.7503(3) -0.0187(4) 0.105(4) Uani 1 1 d . . . H68A H 0.4152 0.7851 -0.0261 0.126 Uiso 1 1 calc R . . H68B H 0.4880 0.7417 -0.0332 0.126 Uiso 1 1 calc R . . C69 C 0.4385(5) 0.7445(3) 0.0334(4) 0.090(3) Uani 1 1 d . . . H69A H 0.4571 0.7104 0.0409 0.108 Uiso 1 1 calc R . . H69B H 0.4870 0.7669 0.0453 0.108 Uiso 1 1 calc R . . C70 C 0.3495(4) 0.75603(19) 0.0564(2) 0.0412(15) Uani 1 1 d . . . H70A H 0.3329 0.7908 0.0504 0.049 Uiso 1 1 calc R . . H70B H 0.3569 0.7517 0.0901 0.049 Uiso 1 1 calc R . . N1 N 0.2294(3) 0.22995(14) 0.45626(15) 0.0381(12) Uani 1 1 d . . . H1A H 0.2280 0.2115 0.4824 0.057 Uiso 1 1 calc R . . H1B H 0.2821 0.2236 0.4409 0.057 Uiso 1 1 calc R . . H1C H 0.1802 0.2223 0.4380 0.057 Uiso 1 1 calc R . . N2 N 0.0193(3) 0.38578(13) 0.35739(12) 0.0227(10) Uani 1 1 d . . . H2A H 0.0525 0.3583 0.3512 0.034 Uiso 1 1 calc R . . H2B H -0.0380 0.3770 0.3664 0.034 Uiso 1 1 calc R . . H2C H 0.0476 0.4031 0.3803 0.034 Uiso 1 1 calc R . . N3 N 0.3479(3) 0.28879(12) 0.31040(12) 0.0213(9) Uani 1 1 d . . . H3C H 0.3412 0.2568 0.3019 0.032 Uiso 1 1 calc R . . H3D H 0.3129 0.2950 0.3355 0.032 Uiso 1 1 calc R . . H3E H 0.4079 0.2948 0.3175 0.032 Uiso 1 1 calc R . . N4 N 0.5778(3) 0.52729(14) 0.38943(13) 0.0239(10) Uani 1 1 d . . . H4C H 0.5975 0.4957 0.3925 0.036 Uiso 1 1 calc R . . H4D H 0.5419 0.5353 0.4137 0.036 Uiso 1 1 calc R . . H4E H 0.6272 0.5478 0.3888 0.036 Uiso 1 1 calc R . . N5 N 0.1905(3) 0.59242(13) 0.42821(12) 0.0233(10) Uani 1 1 d . . . H5C H 0.1718 0.6206 0.4422 0.035 Uiso 1 1 calc R . . H5D H 0.2515 0.5877 0.4341 0.035 Uiso 1 1 calc R . . H5E H 0.1581 0.5665 0.4393 0.035 Uiso 1 1 calc R . . N6 N 0.3933(3) 0.68758(13) 0.17646(12) 0.0208(9) Uani 1 1 d . . . H6C H 0.3620 0.6772 0.1509 0.031 Uiso 1 1 calc R . . H6D H 0.4528 0.6776 0.1749 0.031 Uiso 1 1 calc R . . H6E H 0.3913 0.7210 0.1780 0.031 Uiso 1 1 calc R . . N7 N 0.5499(3) 0.45845(14) 0.10115(11) 0.0209(9) Uani 1 1 d . . . H7C H 0.6007 0.4405 0.0943 0.031 Uiso 1 1 calc R . . H7D H 0.5589 0.4903 0.0928 0.031 Uiso 1 1 calc R . . H7E H 0.5005 0.4461 0.0855 0.031 Uiso 1 1 calc R . . N8 N 0.1073(3) 0.42349(13) 0.07106(12) 0.0243(10) Uani 1 1 d . . . H8A H 0.0656 0.4005 0.0617 0.036 Uiso 1 1 calc R . . H8B H 0.1596 0.4201 0.0545 0.036 Uiso 1 1 calc R . . H8C H 0.0836 0.4541 0.0665 0.036 Uiso 1 1 calc R . . N9 N -0.0171(3) 0.61234(13) 0.14629(12) 0.0209(9) Uani 1 1 d . . . H9A H -0.0754 0.6223 0.1521 0.031 Uiso 1 1 calc R . . H9B H -0.0180 0.5899 0.1230 0.031 Uiso 1 1 calc R . . H9C H 0.0174 0.6387 0.1380 0.031 Uiso 1 1 calc R . . N10 N 0.1846(3) 0.74040(13) 0.06020(13) 0.0251(10) Uani 1 1 d . . . H10C H 0.1720 0.7714 0.0502 0.038 Uiso 1 1 calc R . . H10D H 0.1914 0.7405 0.0914 0.038 Uiso 1 1 calc R . . H10E H 0.1375 0.7201 0.0520 0.038 Uiso 1 1 calc R . . O1 O 0.2105(2) 0.35550(12) 0.42210(12) 0.0334(9) Uani 1 1 d . . . O1W O 0.1261(2) 0.44063(11) 0.43264(10) 0.0227(8) Uani 1 1 d . . . O2W O 0.3274(3) 0.46270(14) 0.47200(11) 0.0401(10) Uani 1 1 d . . . O3W O 0.4137(2) 0.37175(11) 0.42170(11) 0.0281(8) Uani 1 1 d . . . O4W O 0.1671(2) 0.56288(12) 0.03756(10) 0.0284(8) Uani 1 1 d . . . O5W O 0.3564(3) 0.52085(12) 0.02629(10) 0.0306(9) Uani 1 1 d . . . O6W O 0.4619(2) 0.60465(13) 0.08594(13) 0.0387(10) Uani 1 1 d . . . O7W O 0.6473(3) 0.54244(15) 0.07116(15) 0.0583(12) Uani 1 1 d . . . O8W O 0.6753(3) 0.44329(12) 0.39885(12) 0.0365(9) Uani 1 1 d . . . O9W O 0.2990(3) 0.58117(12) -0.04911(11) 0.0322(9) Uani 1 1 d . . . O2 O 0.2501(3) 0.28592(13) 0.38792(12) 0.0450(11) Uani 1 1 d . . . O3 O 0.1203(2) 0.45567(11) 0.26511(10) 0.0216(8) Uani 1 1 d . . . O4 O 0.1731(2) 0.42413(12) 0.33085(10) 0.0244(8) Uani 1 1 d . . . O5 O 0.3514(2) 0.38066(10) 0.32973(10) 0.0186(7) Uani 1 1 d . . . O6 O 0.3183(2) 0.40734(10) 0.25851(10) 0.0201(8) Uani 1 1 d . . . O7 O 0.4320(2) 0.47623(11) 0.38673(10) 0.0264(8) Uani 1 1 d . . . O8 O 0.3860(2) 0.49519(10) 0.31561(10) 0.0188(7) Uani 1 1 d . . . O9 O 0.2045(2) 0.54496(11) 0.31314(10) 0.0199(7) Uani 1 1 d . . . O10W O 0.0713(2) 0.52666(11) 0.47220(10) 0.0254(8) Uani 1 1 d . . . O10 O 0.2332(2) 0.51513(11) 0.38356(10) 0.0264(8) Uani 1 1 d . . . O11 O 0.3416(2) 0.58432(10) 0.24778(10) 0.0207(8) Uani 1 1 d . . . O12 O 0.3544(2) 0.59478(10) 0.17210(10) 0.0231(8) Uani 1 1 d . . . O13 O 0.4090(2) 0.50544(11) 0.12626(10) 0.0249(8) Uani 1 1 d . . . O14 O 0.4212(2) 0.48916(10) 0.20187(10) 0.0195(7) Uani 1 1 d . . . O15 O 0.2333(2) 0.45373(11) 0.17447(10) 0.0245(8) Uani 1 1 d . . . O16 O 0.2139(2) 0.48860(11) 0.10543(10) 0.0257(8) Uani 1 1 d . . . O17 O 0.1519(2) 0.58747(11) 0.13897(10) 0.0220(8) Uani 1 1 d . . . O18 O 0.1645(2) 0.54823(11) 0.20610(10) 0.0236(8) Uani 1 1 d . . . O19 O 0.2773(2) 0.66463(10) 0.09995(10) 0.0211(8) Uani 1 1 d . . . O20 O 0.3061(3) 0.63580(11) 0.03074(10) 0.0274(9) Uani 1 1 d . . . O21 O -0.0200(3) 0.71936(15) 0.67668(15) 0.0671(14) Uani 1 1 d . . . O22 O -0.0101(4) 0.72764(17) 0.59807(15) 0.0709(15) Uani 1 1 d . . . O23 O 0.0747(3) 0.78001(13) 0.64564(12) 0.0367(9) Uani 1 1 d . . . O24 O -0.0851(3) 0.78787(13) 0.64130(18) 0.0655(14) Uani 1 1 d . . . O25 O 0.1058(3) 0.41726(14) 0.53729(12) 0.0492(12) Uani 1 1 d . . . O26 O 0.1457(4) 0.49436(15) 0.56291(15) 0.089(2) Uani 1 1 d . . . O27 O 0.1512(3) 0.42951(15) 0.61465(12) 0.0550(12) Uani 1 1 d . . . O28 O 0.2571(3) 0.4341(2) 0.55716(14) 0.0754(15) Uani 1 1 d . . . O29 O 0.1263(3) 0.96690(13) 0.42742(13) 0.0470(11) Uani 1 1 d . . . O30 O 0.0075(3) 1.02410(14) 0.42851(14) 0.0526(11) Uani 1 1 d . . . O31 O 0.1525(3) 1.04872(15) 0.40688(13) 0.0558(12) Uani 1 1 d . . . O32 O 0.1282(4) 1.02752(14) 0.48324(12) 0.0578(13) Uani 1 1 d . . . O33 O 0.0531(3) 0.64975(14) 0.05471(12) 0.0477(11) Uani 1 1 d . . . O34 O -0.0900(3) 0.65669(14) 0.01536(16) 0.0577(12) Uani 1 1 d . . . O35 O 0.0393(3) 0.62696(13) -0.02197(12) 0.0419(10) Uani 1 1 d . . . O36 O 0.0308(3) 0.70962(13) -0.00129(13) 0.0468(11) Uani 1 1 d . . . O37 O 0.5884(6) 0.8503(3) 0.4335(2) 0.158(3) Uani 1 1 d . . . O38 O 0.7094(6) 0.8740(7) 0.4727(3) 0.333(10) Uani 1 1 d . . . O39 O 0.6032(8) 0.8583(4) 0.5111(2) 0.234(6) Uani 1 1 d . . . O40 O 0.5949(11) 0.9165(3) 0.4665(4) 0.363(11) Uani 1 1 d . . . O41 O 0.3106(3) 0.67578(17) 0.65949(18) 0.0747(15) Uani 1 1 d . . . O42 O 0.4359(3) 0.63275(16) 0.63443(18) 0.0772(17) Uani 1 1 d . . . O43 O 0.4161(5) 0.64566(19) 0.71227(16) 0.102(2) Uani 1 1 d . . . O44 O 0.4571(3) 0.71039(12) 0.66581(13) 0.0367(9) Uani 1 1 d . . . O45 O 0.4081(5) 0.1146(2) 0.33955(17) 0.125(3) Uani 1 1 d . . . O46 O 0.3468(6) 0.1754(4) 0.38477(19) 0.220(6) Uani 1 1 d . . . O47 O 0.2804(7) 0.1577(5) 0.3186(5) 0.337(10) Uani 1 1 d . . . O48 O 0.3959(7) 0.1854(3) 0.3174(3) 0.180(3) Uani 1 1 d U . . O49 O 0.4318(4) 0.61491(19) 0.52000(14) 0.0750(16) Uani 1 1 d . . . O50 O 0.5334(3) 0.6137(2) 0.45934(18) 0.0841(17) Uani 1 1 d . . . O51 O 0.4488(7) 0.5474(2) 0.4733(3) 0.180(4) Uani 1 1 d . . . O52 O 0.3780(4) 0.6136(3) 0.44599(16) 0.126(3) Uani 1 1 d . . . O53 O 0.0458(3) 0.60729(14) 0.54441(13) 0.0499(11) Uani 1 1 d . . . O54 O 0.1998(3) 0.59328(13) 0.52829(11) 0.0386(10) Uani 1 1 d . . . O55 O 0.1314(3) 0.66547(12) 0.50327(11) 0.0440(11) Uani 1 1 d . . . O56 O 0.1581(3) 0.65381(13) 0.58231(11) 0.0445(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 La1 0.01659(16) 0.01755(14) 0.01136(13) 0.00002(11) -0.00155(11) 0.00058(12) La2 0.01647(15) 0.01255(13) 0.01029(13) 0.00111(10) 0.00119(11) 0.00159(11) La3 0.01224(14) 0.01034(13) 0.00839(12) 0.00048(10) 0.00053(10) -0.00016(11) Cl1 0.0344(8) 0.0197(6) 0.0331(7) 0.0010(5) 0.0036(6) -0.0035(6) Cl2 0.0296(8) 0.0297(7) 0.0210(6) 0.0003(5) -0.0032(6) -0.0051(6) Cl3 0.0357(8) 0.0298(7) 0.0219(6) 0.0010(5) -0.0036(6) 0.0031(6) Cl4 0.0332(8) 0.0270(7) 0.0321(7) -0.0078(5) -0.0077(6) 0.0081(6) Cl5 0.0429(10) 0.0321(7) 0.0303(7) 0.0081(6) 0.0042(7) 0.0051(7) Cl6 0.0317(9) 0.0301(7) 0.0402(8) -0.0119(6) 0.0080(6) -0.0026(6) Cl7 0.0308(8) 0.0333(7) 0.0339(7) 0.0110(6) -0.0012(6) 0.0036(6) Cl8 0.0437(11) 0.0678(11) 0.0389(9) -0.0285(8) -0.0088(8) -0.0091(8) Cl9 0.0344(8) 0.0210(6) 0.0151(6) -0.0006(5) 0.0016(5) -0.0063(5) C1 0.021(3) 0.027(3) 0.035(3) 0.005(2) 0.003(2) -0.008(2) C2 0.026(3) 0.018(2) 0.026(3) 0.002(2) 0.007(2) -0.006(2) C3 0.035(4) 0.043(3) 0.033(3) 0.012(2) -0.004(3) -0.005(3) C4 0.054(5) 0.052(4) 0.047(4) 0.020(3) -0.021(3) -0.010(3) C5 0.086(6) 0.039(4) 0.022(3) 0.007(3) 0.000(3) -0.016(4) C6 0.053(4) 0.047(3) 0.023(3) 0.002(3) 0.017(3) -0.007(3) C7 0.032(3) 0.028(3) 0.030(3) 0.000(2) 0.005(3) -0.004(2) C8 0.017(3) 0.016(2) 0.020(2) -0.009(2) 0.001(2) 0.000(2) C9 0.019(3) 0.018(2) 0.008(2) 0.0054(17) -0.0014(19) -0.005(2) C10 0.023(3) 0.020(3) 0.022(3) -0.005(2) 0.003(2) 0.001(2) C11 0.024(3) 0.030(3) 0.036(3) -0.001(2) 0.005(3) 0.005(2) C12 0.016(3) 0.041(3) 0.035(3) 0.008(2) -0.004(2) -0.007(2) C13 0.028(3) 0.036(3) 0.021(3) -0.004(2) -0.002(2) -0.011(2) C14 0.024(3) 0.023(3) 0.012(2) -0.0052(19) 0.000(2) -0.005(2) C15 0.017(3) 0.013(2) 0.020(3) 0.0013(19) 0.003(2) 0.000(2) C16 0.024(3) 0.013(2) 0.012(2) 0.0017(17) 0.001(2) 0.004(2) C17 0.025(3) 0.019(2) 0.025(3) -0.002(2) -0.002(2) -0.002(2) C18 0.041(4) 0.026(3) 0.048(4) -0.004(2) -0.017(3) -0.011(3) C19 0.075(5) 0.018(3) 0.031(3) -0.009(2) -0.022(3) 0.003(3) C20 0.058(4) 0.020(3) 0.023(3) -0.001(2) 0.005(3) 0.012(3) C21 0.034(3) 0.018(2) 0.020(3) -0.0002(19) 0.006(2) 0.007(2) C22 0.015(3) 0.017(2) 0.016(2) -0.0021(19) -0.001(2) 0.002(2) C23 0.011(3) 0.024(2) 0.011(2) 0.0008(18) -0.0032(19) 0.001(2) C24 0.017(3) 0.028(3) 0.026(3) 0.002(2) 0.003(2) 0.004(2) C25 0.024(3) 0.044(3) 0.047(4) 0.004(3) 0.013(3) -0.004(3) C26 0.027(4) 0.040(3) 0.057(4) 0.019(3) 0.004(3) -0.011(3) C27 0.020(3) 0.031(3) 0.040(3) 0.009(2) -0.011(3) -0.007(2) C28 0.021(3) 0.020(2) 0.022(3) 0.0021(19) -0.006(2) 0.000(2) C29 0.016(3) 0.017(2) 0.017(3) 0.0014(19) 0.001(2) -0.002(2) C30 0.023(3) 0.018(2) 0.010(2) -0.0027(18) 0.004(2) -0.003(2) C31 0.026(3) 0.032(3) 0.014(2) -0.001(2) 0.003(2) 0.007(2) C32 0.050(4) 0.038(3) 0.042(3) -0.005(3) 0.006(3) 0.026(3) C33 0.097(6) 0.024(3) 0.046(4) 0.001(3) 0.015(4) 0.027(4) C34 0.086(6) 0.019(3) 0.027(3) 0.002(2) 0.014(3) -0.009(3) C35 0.038(4) 0.022(3) 0.015(2) -0.001(2) 0.004(2) -0.007(2) C36 0.012(3) 0.020(2) 0.018(3) 0.000(2) -0.004(2) 0.000(2) C37 0.019(3) 0.016(2) 0.013(2) 0.0028(18) 0.002(2) -0.006(2) C38 0.022(3) 0.023(3) 0.021(3) 0.003(2) -0.001(2) -0.006(2) C39 0.030(3) 0.023(3) 0.039(3) -0.002(2) 0.002(3) 0.004(2) C40 0.054(4) 0.025(3) 0.034(3) -0.007(2) 0.004(3) 0.000(3) C41 0.047(4) 0.017(3) 0.024(3) -0.001(2) -0.008(3) -0.007(2) C42 0.022(3) 0.021(2) 0.017(2) 0.0034(19) -0.006(2) -0.005(2) C43 0.018(3) 0.012(2) 0.022(3) -0.0007(19) 0.002(2) -0.004(2) C44 0.018(3) 0.020(2) 0.008(2) 0.0003(18) 0.0042(19) 0.003(2) C45 0.027(3) 0.018(3) 0.027(3) 0.003(2) 0.003(2) 0.001(2) C46 0.043(4) 0.023(3) 0.043(3) 0.007(2) 0.005(3) 0.013(3) C47 0.029(4) 0.051(4) 0.032(3) 0.006(3) 0.001(3) 0.019(3) C48 0.021(3) 0.049(3) 0.025(3) -0.002(2) 0.000(2) 0.001(3) C49 0.025(3) 0.027(3) 0.016(2) -0.003(2) -0.003(2) 0.002(2) C50 0.019(3) 0.016(2) 0.018(3) -0.0031(19) 0.002(2) 0.003(2) C51 0.023(3) 0.018(2) 0.006(2) -0.0006(17) -0.0006(19) 0.000(2) C52 0.023(3) 0.019(2) 0.024(3) -0.004(2) -0.001(2) -0.001(2) C53 0.025(3) 0.035(3) 0.032(3) -0.010(2) 0.006(3) -0.005(2) C54 0.051(4) 0.031(3) 0.035(3) 0.001(2) -0.002(3) -0.022(3) C55 0.051(4) 0.012(3) 0.031(3) 0.001(2) -0.013(3) 0.002(2) C56 0.037(3) 0.016(2) 0.020(3) -0.001(2) -0.004(2) 0.004(2) C57 0.020(3) 0.008(2) 0.019(2) -0.0034(18) -0.001(2) -0.001(2) C58 0.019(3) 0.015(2) 0.012(2) 0.0022(17) 0.001(2) 0.007(2) C59 0.023(3) 0.019(2) 0.024(3) -0.001(2) 0.002(2) 0.000(2) C60 0.020(3) 0.031(3) 0.040(3) -0.003(2) 0.007(3) -0.008(2) C61 0.024(3) 0.045(3) 0.040(3) -0.011(3) 0.016(3) -0.006(3) C62 0.027(3) 0.030(3) 0.030(3) -0.015(2) 0.007(2) 0.002(2) C63 0.020(3) 0.023(3) 0.019(2) -0.005(2) -0.001(2) -0.006(2) C64 0.019(3) 0.017(2) 0.017(3) 0.0020(19) 0.000(2) -0.001(2) C65 0.031(3) 0.013(2) 0.025(3) 0.001(2) 0.006(2) -0.002(2) C66 0.077(5) 0.030(3) 0.024(3) 0.014(2) 0.013(3) 0.023(3) C67 0.108(7) 0.038(4) 0.057(4) 0.017(3) 0.048(5) 0.015(4) C68 0.112(9) 0.052(5) 0.153(9) -0.003(5) 0.100(8) -0.023(5) C69 0.042(5) 0.054(5) 0.174(10) -0.018(5) 0.038(6) -0.026(4) C70 0.034(4) 0.025(3) 0.065(4) 0.001(3) 0.005(3) -0.009(3) N1 0.049(3) 0.027(2) 0.038(3) 0.002(2) 0.017(2) -0.003(2) N2 0.029(3) 0.027(2) 0.0127(19) 0.0045(16) 0.0004(18) -0.0049(19) N3 0.032(3) 0.014(2) 0.017(2) 0.0036(16) -0.0028(19) 0.0030(18) N4 0.021(3) 0.023(2) 0.027(2) 0.0001(17) -0.0112(19) -0.0013(18) N5 0.030(3) 0.024(2) 0.016(2) -0.0033(16) 0.0022(19) -0.0045(19) N6 0.025(3) 0.018(2) 0.020(2) 0.0015(16) -0.0017(18) -0.0043(18) N7 0.022(2) 0.028(2) 0.0124(19) -0.0003(16) 0.0011(17) 0.0044(18) N8 0.038(3) 0.021(2) 0.014(2) 0.0009(16) -0.0078(19) -0.0085(19) N9 0.022(3) 0.019(2) 0.021(2) -0.0011(16) -0.0067(18) 0.0059(18) N10 0.035(3) 0.014(2) 0.026(2) 0.0019(16) 0.000(2) 0.0031(19) O1 0.027(2) 0.029(2) 0.044(2) 0.0119(16) 0.0031(18) -0.0050(17) O1W 0.023(2) 0.0264(18) 0.0187(17) -0.0020(14) 0.0062(15) -0.0015(15) O2W 0.040(3) 0.063(3) 0.0172(18) -0.0074(17) -0.0023(17) -0.014(2) O3W 0.023(2) 0.0303(19) 0.0313(19) 0.0072(15) -0.0035(16) 0.0019(16) O4W 0.028(2) 0.033(2) 0.0231(18) 0.0025(15) -0.0093(16) 0.0017(17) O5W 0.041(2) 0.0322(19) 0.0189(18) -0.0052(15) 0.0060(17) 0.0086(17) O6W 0.019(2) 0.040(2) 0.057(2) 0.0192(18) 0.0040(19) -0.0034(17) O7W 0.050(3) 0.062(3) 0.063(3) 0.021(2) -0.001(2) -0.009(2) O8W 0.032(2) 0.030(2) 0.047(2) 0.0061(17) -0.0037(19) 0.0029(17) O9W 0.039(2) 0.036(2) 0.0215(18) -0.0031(15) 0.0087(17) 0.0022(18) O2 0.073(3) 0.036(2) 0.027(2) -0.0017(17) 0.022(2) -0.017(2) O3 0.021(2) 0.0281(18) 0.0157(17) 0.0068(14) 0.0039(15) -0.0053(15) O4 0.0166(19) 0.040(2) 0.0167(16) -0.0031(15) -0.0035(15) 0.0028(16) O5 0.026(2) 0.0148(16) 0.0147(17) -0.0009(12) -0.0002(15) 0.0040(14) O6 0.032(2) 0.0118(16) 0.0170(16) 0.0022(13) 0.0028(15) 0.0050(15) O7 0.026(2) 0.034(2) 0.0191(18) 0.0088(15) -0.0009(15) -0.0045(16) O8 0.0176(18) 0.0182(16) 0.0206(17) -0.0023(13) -0.0032(14) -0.0017(14) O9 0.024(2) 0.0230(17) 0.0131(17) -0.0052(13) 0.0030(14) 0.0049(15) O10W 0.031(2) 0.0244(18) 0.0209(17) -0.0019(14) 0.0055(16) -0.0043(16) O10 0.040(2) 0.0216(18) 0.0181(17) 0.0021(14) 0.0080(16) 0.0073(16) O11 0.030(2) 0.0165(16) 0.0152(16) 0.0046(13) -0.0041(15) -0.0074(15) O12 0.034(2) 0.0162(17) 0.0187(17) -0.0013(13) -0.0036(16) 0.0018(15) O13 0.028(2) 0.0302(19) 0.0163(17) 0.0056(14) 0.0001(15) 0.0145(16) O14 0.0189(19) 0.0229(17) 0.0169(17) 0.0010(13) 0.0087(14) 0.0018(14) O15 0.032(2) 0.0296(19) 0.0121(17) -0.0033(14) -0.0045(15) -0.0056(16) O16 0.033(2) 0.0210(17) 0.0231(18) 0.0054(14) -0.0062(16) -0.0062(16) O17 0.022(2) 0.0300(18) 0.0147(17) 0.0034(14) 0.0036(15) 0.0050(15) O18 0.018(2) 0.0271(18) 0.0255(18) 0.0081(14) -0.0019(15) 0.0062(15) O19 0.031(2) 0.0167(16) 0.0158(17) 0.0023(13) -0.0001(15) 0.0015(15) O20 0.051(3) 0.0131(17) 0.0185(17) 0.0012(14) 0.0037(17) 0.0049(16) O21 0.075(4) 0.057(3) 0.070(3) 0.037(2) 0.017(3) -0.010(3) O22 0.074(4) 0.081(3) 0.058(3) -0.038(2) 0.006(3) -0.035(3) O23 0.034(3) 0.040(2) 0.036(2) -0.0027(17) -0.0026(18) -0.0098(18) O24 0.036(3) 0.024(2) 0.136(4) -0.003(2) -0.007(3) 0.002(2) O25 0.065(3) 0.045(2) 0.037(2) -0.0037(18) -0.016(2) -0.023(2) O26 0.166(6) 0.041(3) 0.058(3) -0.008(2) -0.054(3) 0.021(3) O27 0.078(4) 0.066(3) 0.021(2) 0.0079(19) 0.001(2) -0.009(3) O28 0.029(3) 0.155(5) 0.042(3) 0.003(3) 0.004(2) -0.012(3) O29 0.054(3) 0.034(2) 0.053(3) -0.0121(18) -0.018(2) 0.012(2) O30 0.038(3) 0.056(3) 0.064(3) -0.004(2) -0.001(2) 0.016(2) O31 0.052(3) 0.069(3) 0.046(3) 0.033(2) -0.004(2) -0.010(2) O32 0.100(4) 0.050(3) 0.023(2) -0.0094(18) -0.012(2) -0.002(3) O33 0.070(3) 0.048(2) 0.024(2) -0.0054(17) -0.010(2) 0.009(2) O34 0.029(3) 0.046(3) 0.099(4) -0.016(2) 0.003(2) 0.009(2) O35 0.042(3) 0.049(2) 0.034(2) -0.0214(18) -0.0090(19) 0.011(2) O36 0.050(3) 0.028(2) 0.062(3) 0.0063(18) -0.018(2) 0.0019(19) O37 0.224(10) 0.162(7) 0.086(5) -0.056(4) -0.067(5) 0.027(6) O38 0.049(6) 0.84(3) 0.108(7) -0.008(12) 0.004(5) 0.001(11) O39 0.288(13) 0.342(13) 0.072(5) 0.064(6) -0.009(6) -0.173(11) O40 0.64(3) 0.064(5) 0.373(16) -0.059(7) -0.369(18) 0.118(9) O41 0.022(3) 0.078(3) 0.125(4) -0.038(3) 0.013(3) -0.001(2) O42 0.037(3) 0.072(3) 0.123(4) -0.071(3) 0.030(3) -0.016(2) O43 0.163(7) 0.088(4) 0.054(3) 0.036(3) -0.010(4) -0.058(4) O44 0.033(2) 0.0243(19) 0.053(2) 0.0017(17) 0.001(2) 0.0004(17) O45 0.194(8) 0.124(5) 0.058(3) -0.006(3) -0.017(4) 0.121(5) O46 0.256(11) 0.352(12) 0.051(4) -0.069(5) -0.040(5) 0.246(10) O47 0.159(9) 0.407(16) 0.439(17) -0.345(15) -0.196(11) 0.197(11) O48 0.181(4) 0.178(4) 0.180(4) 0.0014(10) 0.0052(10) 0.0005(10) O49 0.074(4) 0.118(4) 0.033(2) -0.027(3) -0.005(2) 0.008(3) O50 0.032(3) 0.132(5) 0.088(4) -0.029(3) 0.000(3) -0.012(3) O51 0.245(11) 0.079(5) 0.219(9) -0.078(5) 0.083(8) -0.076(6) O52 0.030(3) 0.301(9) 0.047(3) 0.012(4) -0.011(3) -0.002(4) O53 0.040(3) 0.057(3) 0.053(3) -0.014(2) 0.022(2) -0.022(2) O54 0.046(3) 0.040(2) 0.030(2) -0.0062(17) -0.0038(19) 0.012(2) O55 0.085(4) 0.025(2) 0.0225(19) 0.0095(15) 0.003(2) 0.000(2) O56 0.078(3) 0.035(2) 0.0205(19) -0.0069(16) -0.011(2) -0.006(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 La1 O4 2.406(3) . ? La1 O5 2.447(3) . ? La1 O1 2.456(3) . ? La1 O10 2.467(3) . ? La1 O7 2.487(3) . ? La1 O2W 2.556(3) . ? La1 O3W 2.572(3) . ? La1 O1W 2.640(3) . ? La2 O12 2.411(3) . ? La2 O13 2.455(3) . ? La2 O16 2.480(3) . ? La2 O17 2.526(3) . ? La2 O5W 2.579(3) . ? La2 O4W 2.581(3) . ? La2 O6W 2.611(4) . ? La2 O19 2.672(3) . ? La2 O20 2.702(3) . ? La2 C64 3.044(4) . ? La3 O18 2.483(3) . ? La3 O8 2.497(3) . ? La3 O14 2.501(3) . ? La3 O6 2.503(3) . ? La3 O15 2.504(3) . ? La3 O9 2.558(3) . ? La3 O11 2.572(3) . ? La3 O3 2.601(3) . ? Cl1 O21 1.416(4) . ? Cl1 O24 1.426(4) . ? Cl1 O22 1.427(4) . ? Cl1 O23 1.435(4) . ? Cl2 O26 1.398(4) . ? Cl2 O28 1.413(5) . ? Cl2 O27 1.421(4) . ? Cl2 O25 1.439(4) . ? Cl3 O32 1.412(4) . ? Cl3 O31 1.422(4) . ? Cl3 O29 1.426(4) . ? Cl3 O30 1.441(4) . ? Cl4 O34 1.421(4) . ? Cl4 O36 1.426(4) . ? Cl4 O33 1.432(4) . ? Cl4 O35 1.436(3) . ? Cl5 O40 1.173(7) . ? Cl5 O38 1.283(8) . ? Cl5 O39 1.297(6) . ? Cl5 O37 1.370(6) . ? Cl6 O43 1.394(4) . ? Cl6 O42 1.407(4) . ? Cl6 O41 1.408(5) . ? Cl6 O44 1.452(4) . ? Cl7 O47 1.235(8) . ? Cl7 O46 1.310(5) . ? Cl7 O48 1.327(9) . ? Cl7 O45 1.401(5) . ? Cl8 O51 1.360(6) . ? Cl8 O52 1.376(5) . ? Cl8 O49 1.383(4) . ? Cl8 O50 1.443(5) . ? Cl9 O53 1.428(4) . ? Cl9 O55 1.432(3) . ? Cl9 O54 1.432(4) . ? Cl9 O56 1.434(3) . ? C1 O2 1.229(6) . ? C1 O1 1.250(6) . ? C1 C2 1.555(7) . ? C2 N1 1.502(6) . ? C2 C3 1.516(7) . ? C2 C7 1.519(7) . ? C3 C4 1.534(7) . ? C4 C5 1.502(9) . ? C5 C6 1.516(8) . ? C6 C7 1.509(7) . ? C8 O3 1.251(5) . ? C8 O4 1.255(5) . ? C8 C9 1.534(6) . ? C9 N2 1.510(5) . ? C9 C14 1.524(6) . ? C9 C10 1.541(6) . ? C10 C11 1.520(7) . ? C11 C12 1.510(7) . ? C12 C13 1.520(7) . ? C13 C14 1.528(7) . ? C15 O6 1.238(5) . ? C15 O5 1.254(5) . ? C15 C16 1.547(6) . ? C16 N3 1.498(5) . ? C16 C21 1.526(6) . ? C16 C17 1.530(7) . ? C17 C18 1.526(6) . ? C18 C19 1.520(8) . ? C19 C20 1.533(8) . ? C20 C21 1.527(6) . ? C22 O7 1.252(5) . ? C22 O8 1.252(5) . ? C22 C23 1.527(6) . ? C23 N4 1.500(5) . ? C23 C24 1.525(6) . ? C23 C28 1.530(6) . ? C24 C25 1.530(7) . ? C25 C26 1.521(7) . ? C26 C27 1.521(7) . ? C27 C28 1.522(6) . ? C29 O9 1.237(5) . ? C29 O10 1.258(5) . ? C29 C30 1.542(6) . ? C30 N5 1.498(5) . ? C30 C35 1.523(6) . ? C30 C31 1.525(7) . ? C31 C32 1.515(6) . ? C32 C33 1.532(8) . ? C33 C34 1.512(9) . ? C34 C35 1.516(7) . ? C36 O11 1.236(5) . ? C36 O12 1.263(5) . ? C36 C37 1.528(6) . ? C37 N6 1.510(5) . ? C37 C38 1.525(7) . ? C37 C42 1.526(6) . ? C38 C39 1.526(6) . ? C39 C40 1.501(7) . ? C40 C41 1.514(8) . ? C41 C42 1.513(6) . ? C43 O14 1.246(5) . ? C43 O13 1.260(5) . ? C43 C44 1.532(6) . ? C44 N7 1.500(5) . ? C44 C49 1.526(6) . ? C44 C45 1.533(6) . ? C45 C46 1.532(7) . ? C46 C47 1.521(8) . ? C47 C48 1.521(7) . ? C48 C49 1.539(7) . ? C50 O15 1.246(5) . ? C50 O16 1.251(5) . ? C50 C51 1.530(6) . ? C51 N8 1.513(5) . ? C51 C56 1.517(6) . ? C51 C52 1.536(6) . ? C52 C53 1.511(6) . ? C53 C54 1.518(7) . ? C54 C55 1.509(8) . ? C55 C56 1.540(7) . ? C57 O18 1.242(5) . ? C57 O17 1.255(5) . ? C57 C58 1.535(6) . ? C58 N9 1.510(5) . ? C58 C63 1.532(6) . ? C58 C59 1.538(6) . ? C59 C60 1.521(7) . ? C60 C61 1.524(7) . ? C61 C62 1.530(7) . ? C62 C63 1.511(7) . ? C64 O20 1.245(5) . ? C64 O19 1.258(5) . ? C64 C65 1.538(6) . ? C65 N10 1.512(6) . ? C65 C66 1.530(6) . ? C65 C70 1.533(7) . ? C66 C67 1.534(9) . ? C67 C68 1.499(11) . ? C68 C69 1.525(12) . ? C69 C70 1.499(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 La1 O5 72.01(11) . . ? O4 La1 O1 84.82(11) . . ? O5 La1 O1 90.02(11) . . ? O4 La1 O10 76.95(11) . . ? O5 La1 O10 124.21(10) . . ? O1 La1 O10 131.99(12) . . ? O4 La1 O7 124.05(10) . . ? O5 La1 O7 83.61(11) . . ? O1 La1 O7 145.97(11) . . ? O10 La1 O7 76.97(11) . . ? O4 La1 O2W 147.31(12) . . ? O5 La1 O2W 140.68(12) . . ? O1 La1 O2W 93.97(12) . . ? O10 La1 O2W 79.90(11) . . ? O7 La1 O2W 71.52(11) . . ? O4 La1 O3W 133.92(10) . . ? O5 La1 O3W 68.24(10) . . ? O1 La1 O3W 73.01(11) . . ? O10 La1 O3W 146.34(11) . . ? O7 La1 O3W 73.59(11) . . ? O2W La1 O3W 75.63(12) . . ? O4 La1 O1W 74.93(10) . . ? O5 La1 O1W 138.41(10) . . ? O1 La1 O1W 62.30(11) . . ? O10 La1 O1W 70.12(10) . . ? O7 La1 O1W 136.74(10) . . ? O2W La1 O1W 75.66(11) . . ? O3W La1 O1W 124.02(10) . . ? O12 La2 O13 72.79(10) . . ? O12 La2 O16 110.55(10) . . ? O13 La2 O16 72.88(11) . . ? O12 La2 O17 77.59(11) . . ? O13 La2 O17 122.99(10) . . ? O16 La2 O17 73.72(11) . . ? O12 La2 O5W 139.78(12) . . ? O13 La2 O5W 73.66(10) . . ? O16 La2 O5W 79.57(11) . . ? O17 La2 O5W 140.74(11) . . ? O12 La2 O4W 148.94(11) . . ? O13 La2 O4W 132.25(10) . . ? O16 La2 O4W 69.79(10) . . ? O17 La2 O4W 72.76(10) . . ? O5W La2 O4W 71.25(11) . . ? O12 La2 O6W 72.70(12) . . ? O13 La2 O6W 73.82(11) . . ? O16 La2 O6W 143.52(11) . . ? O17 La2 O6W 139.00(11) . . ? O5W La2 O6W 77.16(12) . . ? O4W La2 O6W 126.57(11) . . ? O12 La2 O19 73.04(9) . . ? O13 La2 O19 138.39(10) . . ? O16 La2 O19 142.56(11) . . ? O17 La2 O19 70.80(10) . . ? O5W La2 O19 122.85(10) . . ? O4W La2 O19 88.46(10) . . ? O6W La2 O19 73.89(11) . . ? O12 La2 O20 114.37(10) . . ? O13 La2 O20 133.04(11) . . ? O16 La2 O20 133.15(10) . . ? O17 La2 O20 103.37(10) . . ? O5W La2 O20 74.94(10) . . ? O4W La2 O20 65.06(10) . . ? O6W La2 O20 65.75(11) . . ? O19 La2 O20 48.39(9) . . ? O12 La2 C64 94.30(11) . . ? O13 La2 C64 142.39(12) . . ? O16 La2 C64 143.32(12) . . ? O17 La2 C64 86.44(11) . . ? O5W La2 C64 98.91(11) . . ? O4W La2 C64 75.03(11) . . ? O6W La2 C64 68.59(12) . . ? O19 La2 C64 24.32(10) . . ? O20 La2 C64 24.09(10) . . ? O18 La3 O8 142.95(10) . . ? O18 La3 O14 109.59(10) . . ? O8 La3 O14 84.25(10) . . ? O18 La3 O6 139.81(10) . . ? O8 La3 O6 75.55(10) . . ? O14 La3 O6 78.26(10) . . ? O18 La3 O15 71.48(10) . . ? O8 La3 O15 144.91(10) . . ? O14 La3 O15 73.58(11) . . ? O6 La3 O15 73.57(10) . . ? O18 La3 O9 77.45(10) . . ? O8 La3 O9 71.93(10) . . ? O14 La3 O9 142.74(10) . . ? O6 La3 O9 120.71(9) . . ? O15 La3 O9 139.71(11) . . ? O18 La3 O11 72.75(10) . . ? O8 La3 O11 77.80(9) . . ? O14 La3 O11 76.49(10) . . ? O6 La3 O11 144.75(11) . . ? O15 La3 O11 121.13(9) . . ? O9 La3 O11 70.85(10) . . ? O18 La3 O3 75.62(10) . . ? O8 La3 O3 113.15(9) . . ? O14 La3 O3 144.62(10) . . ? O6 La3 O3 76.96(10) . . ? O15 La3 O3 75.43(10) . . ? O9 La3 O3 72.46(10) . . ? O11 La3 O3 135.58(10) . . ? O21 Cl1 O24 109.7(3) . . ? O21 Cl1 O22 108.0(3) . . ? O24 Cl1 O22 110.5(3) . . ? O21 Cl1 O23 110.3(3) . . ? O24 Cl1 O23 109.6(2) . . ? O22 Cl1 O23 108.7(3) . . ? O26 Cl2 O28 110.8(4) . . ? O26 Cl2 O27 110.6(3) . . ? O28 Cl2 O27 107.9(3) . . ? O26 Cl2 O25 108.2(3) . . ? O28 Cl2 O25 108.5(3) . . ? O27 Cl2 O25 110.9(2) . . ? O32 Cl3 O31 110.1(3) . . ? O32 Cl3 O29 109.1(2) . . ? O31 Cl3 O29 110.3(3) . . ? O32 Cl3 O30 111.2(3) . . ? O31 Cl3 O30 107.6(3) . . ? O29 Cl3 O30 108.6(2) . . ? O34 Cl4 O36 109.8(2) . . ? O34 Cl4 O33 112.3(3) . . ? O36 Cl4 O33 108.6(2) . . ? O34 Cl4 O35 109.3(2) . . ? O36 Cl4 O35 109.1(3) . . ? O33 Cl4 O35 107.8(2) . . ? O40 Cl5 O38 111.8(11) . . ? O40 Cl5 O39 111.7(9) . . ? O38 Cl5 O39 99.3(7) . . ? O40 Cl5 O37 106.6(5) . . ? O38 Cl5 O37 110.7(7) . . ? O39 Cl5 O37 116.7(5) . . ? O43 Cl6 O42 111.0(4) . . ? O43 Cl6 O41 110.6(4) . . ? O42 Cl6 O41 109.2(3) . . ? O43 Cl6 O44 107.9(3) . . ? O42 Cl6 O44 108.4(3) . . ? O41 Cl6 O44 109.6(3) . . ? O47 Cl7 O46 118.8(5) . . ? O47 Cl7 O48 91.9(9) . . ? O46 Cl7 O48 106.2(7) . . ? O47 Cl7 O45 119.1(5) . . ? O46 Cl7 O45 116.1(4) . . ? O48 Cl7 O45 96.7(5) . . ? O51 Cl8 O52 108.0(5) . . ? O51 Cl8 O49 113.8(4) . . ? O52 Cl8 O49 111.2(4) . . ? O51 Cl8 O50 104.9(4) . . ? O52 Cl8 O50 108.6(3) . . ? O49 Cl8 O50 110.0(3) . . ? O53 Cl9 O55 110.5(3) . . ? O53 Cl9 O54 108.9(2) . . ? O55 Cl9 O54 107.8(2) . . ? O53 Cl9 O56 109.1(2) . . ? O55 Cl9 O56 109.7(2) . . ? O54 Cl9 O56 110.8(2) . . ? O2 C1 O1 127.0(5) . . ? O2 C1 C2 116.7(4) . . ? O1 C1 C2 116.3(4) . . ? N1 C2 C3 110.1(4) . . ? N1 C2 C7 109.9(4) . . ? C3 C2 C7 111.7(4) . . ? N1 C2 C1 104.4(4) . . ? C3 C2 C1 107.6(4) . . ? C7 C2 C1 113.0(4) . . ? C2 C3 C4 113.7(5) . . ? C5 C4 C3 111.5(5) . . ? C4 C5 C6 110.9(5) . . ? C7 C6 C5 111.0(4) . . ? C6 C7 C2 112.6(5) . . ? O3 C8 O4 124.7(4) . . ? O3 C8 C9 117.7(4) . . ? O4 C8 C9 117.6(4) . . ? N2 C9 C14 109.5(3) . . ? N2 C9 C8 107.5(4) . . ? C14 C9 C8 111.7(4) . . ? N2 C9 C10 108.3(4) . . ? C14 C9 C10 111.1(4) . . ? C8 C9 C10 108.6(3) . . ? C11 C10 C9 112.6(4) . . ? C12 C11 C10 112.0(4) . . ? C11 C12 C13 110.9(4) . . ? C12 C13 C14 110.4(4) . . ? C9 C14 C13 112.6(4) . . ? O6 C15 O5 127.7(4) . . ? O6 C15 C16 116.0(4) . . ? O5 C15 C16 116.2(4) . . ? N3 C16 C21 109.3(4) . . ? N3 C16 C17 108.0(4) . . ? C21 C16 C17 112.0(4) . . ? N3 C16 C15 106.9(3) . . ? C21 C16 C15 111.7(4) . . ? C17 C16 C15 108.8(4) . . ? C18 C17 C16 112.5(4) . . ? C19 C18 C17 111.7(4) . . ? C18 C19 C20 112.8(4) . . ? C21 C20 C19 111.2(4) . . ? C16 C21 C20 112.3(4) . . ? O7 C22 O8 125.1(4) . . ? O7 C22 C23 116.3(4) . . ? O8 C22 C23 118.6(4) . . ? N4 C23 C24 110.1(4) . . ? N4 C23 C22 106.9(3) . . ? C24 C23 C22 110.4(4) . . ? N4 C23 C28 108.2(3) . . ? C24 C23 C28 111.3(4) . . ? C22 C23 C28 109.8(4) . . ? C23 C24 C25 112.9(4) . . ? C26 C25 C24 111.1(4) . . ? C25 C26 C27 111.4(4) . . ? C26 C27 C28 110.8(4) . . ? C27 C28 C23 112.7(4) . . ? O9 C29 O10 127.0(4) . . ? O9 C29 C30 117.0(4) . . ? O10 C29 C30 115.9(4) . . ? N5 C30 C35 107.8(4) . . ? N5 C30 C31 108.6(4) . . ? C35 C30 C31 111.8(4) . . ? N5 C30 C29 107.0(3) . . ? C35 C30 C29 112.1(4) . . ? C31 C30 C29 109.4(4) . . ? C32 C31 C30 113.8(4) . . ? C31 C32 C33 111.0(5) . . ? C34 C33 C32 112.4(5) . . ? C33 C34 C35 112.1(5) . . ? C34 C35 C30 111.4(4) . . ? O11 C36 O12 125.9(4) . . ? O11 C36 C37 118.4(4) . . ? O12 C36 C37 115.6(4) . . ? N6 C37 C38 108.7(4) . . ? N6 C37 C42 109.4(4) . . ? C38 C37 C42 111.1(4) . . ? N6 C37 C36 107.2(3) . . ? C38 C37 C36 106.6(4) . . ? C42 C37 C36 113.7(4) . . ? C37 C38 C39 113.5(4) . . ? C40 C39 C38 111.2(4) . . ? C39 C40 C41 112.5(4) . . ? C42 C41 C40 112.5(4) . . ? C41 C42 C37 113.2(4) . . ? O14 C43 O13 127.1(4) . . ? O14 C43 C44 117.2(4) . . ? O13 C43 C44 115.7(4) . . ? N7 C44 C49 108.5(4) . . ? N7 C44 C43 107.0(3) . . ? C49 C44 C43 111.4(4) . . ? N7 C44 C45 109.3(3) . . ? C49 C44 C45 110.8(4) . . ? C43 C44 C45 109.7(4) . . ? C46 C45 C44 112.2(4) . . ? C47 C46 C45 111.7(4) . . ? C48 C47 C46 112.8(4) . . ? C47 C48 C49 110.6(4) . . ? C44 C49 C48 112.7(4) . . ? O15 C50 O16 126.7(4) . . ? O15 C50 C51 116.7(4) . . ? O16 C50 C51 116.6(4) . . ? N8 C51 C56 109.3(3) . . ? N8 C51 C50 106.4(3) . . ? C56 C51 C50 113.1(4) . . ? N8 C51 C52 108.2(4) . . ? C56 C51 C52 111.3(4) . . ? C50 C51 C52 108.2(3) . . ? C53 C52 C51 114.7(4) . . ? C52 C53 C54 111.4(4) . . ? C55 C54 C53 110.1(4) . . ? C54 C55 C56 111.9(4) . . ? C51 C56 C55 112.3(4) . . ? O18 C57 O17 126.2(4) . . ? O18 C57 C58 117.0(4) . . ? O17 C57 C58 116.7(4) . . ? N9 C58 C63 109.4(3) . . ? N9 C58 C57 106.7(3) . . ? C63 C58 C57 109.0(4) . . ? N9 C58 C59 109.5(4) . . ? C63 C58 C59 110.8(4) . . ? C57 C58 C59 111.3(3) . . ? C60 C59 C58 113.9(4) . . ? C59 C60 C61 110.7(4) . . ? C60 C61 C62 109.6(4) . . ? C63 C62 C61 111.4(4) . . ? C62 C63 C58 113.5(4) . . ? O20 C64 O19 123.3(4) . . ? O20 C64 C65 120.5(4) . . ? O19 C64 C65 116.2(4) . . ? O20 C64 La2 62.4(2) . . ? O19 C64 La2 61.0(2) . . ? C65 C64 La2 174.8(3) . . ? N10 C65 C66 109.1(4) . . ? N10 C65 C70 106.7(4) . . ? C66 C65 C70 111.5(4) . . ? N10 C65 C64 105.5(4) . . ? C66 C65 C64 114.2(4) . . ? C70 C65 C64 109.5(4) . . ? C65 C66 C67 111.8(5) . . ? C68 C67 C66 113.1(6) . . ? C67 C68 C69 111.3(6) . . ? C70 C69 C68 110.7(7) . . ? C69 C70 C65 111.1(5) . . ? C1 O1 La1 134.2(3) . . ? C8 O3 La3 119.3(3) . . ? C8 O4 La1 164.4(3) . . ? C15 O5 La1 133.8(3) . . ? C15 O6 La3 143.3(3) . . ? C22 O7 La1 113.3(3) . . ? C22 O8 La3 175.2(3) . . ? C29 O9 La3 139.6(3) . . ? C29 O10 La1 145.5(3) . . ? C36 O11 La3 124.9(3) . . ? C36 O12 La2 157.6(3) . . ? C43 O13 La2 146.0(3) . . ? C43 O14 La3 140.9(3) . . ? C50 O15 La3 149.0(3) . . ? C50 O16 La2 139.4(3) . . ? C57 O17 La2 131.0(3) . . ? C57 O18 La3 165.3(3) . . ? C64 O19 La2 94.7(2) . . ? C64 O20 La2 93.5(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.382 _refine_diff_density_min -1.112 _refine_diff_density_rms 0.099 # Attachment '- complex4.cif' data_complex4 _database_code_depnum_ccdc_archive 'CCDC 791394' #TrackingRef '- complex4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C70 H150 Cl9 N10 Nd3 O66' _chemical_formula_weight 2939.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 p2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.5240(2) _cell_length_b 27.1221(5) _cell_length_c 28.9263(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.599(2) _cell_angle_gamma 90.00 _cell_volume 11394.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 32958 _cell_measurement_theta_min 2.7335 _cell_measurement_theta_max 29.0759 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.714 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6004 _exptl_absorpt_coefficient_mu 1.665 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6178 _exptl_absorpt_correction_T_max 0.7318 _exptl_absorpt_process_details ? _exptl_special_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.46 (release 27-08-2009 CrysAlis171 .NET) (compiled Aug 27 2009,17:19:36) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 173(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 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 97744 _diffrn_reflns_av_R_equivalents 0.0592 _diffrn_reflns_av_sigmaI/netI 0.0687 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.74 _diffrn_reflns_theta_max 25.00 _reflns_number_total 19979 _reflns_number_gt 15172 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. Non-hydrogen atoms were refined anisotropically, except for c51 was refined isotropically due to disorder ; _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^)+(0.0424P)^2^+448.2065P] 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 19979 _refine_ls_number_parameters 1423 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1096 _refine_ls_R_factor_gt 0.0874 _refine_ls_wR_factor_ref 0.2126 _refine_ls_wR_factor_gt 0.2051 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.049 _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 Nd1 Nd 0.28409(3) 0.429591(17) 0.392078(15) 0.01629(11) Uani 1 1 d . . . Nd2 Nd 0.29596(3) 0.567837(16) 0.099028(15) 0.01581(10) Uani 1 1 d . . . Nd3 Nd 0.27689(3) 0.497214(16) 0.247871(15) 0.01143(9) Uani 1 1 d . . . Cl1 Cl -0.01111(17) 0.75286(9) 0.63987(9) 0.0314(6) Uani 1 1 d . . . Cl2 Cl 0.16500(17) 0.44406(9) 0.56810(8) 0.0300(6) Uani 1 1 d . . . Cl3 Cl 0.10540(17) 1.01679(9) 0.43719(8) 0.0326(6) Uani 1 1 d . . . Cl4 Cl 0.00558(17) 0.66097(9) 0.01125(9) 0.0342(6) Uani 1 1 d . . . Cl5 Cl 0.62033(19) 0.87648(10) 0.47003(9) 0.0368(7) Uani 1 1 d . . . Cl6 Cl 0.40323(19) 0.66343(10) 0.66792(9) 0.0390(7) Uani 1 1 d . . . Cl7 Cl 0.35283(18) 0.15598(10) 0.34339(9) 0.0369(7) Uani 1 1 d . . . Cl8 Cl 0.4450(2) 0.59728(12) 0.47667(10) 0.0510(8) Uani 1 1 d . . . Cl9 Cl 0.13397(17) 0.62982(9) 0.53985(8) 0.0294(6) Uani 1 1 d . . . C1 C 0.2304(6) 0.3105(4) 0.4216(3) 0.028(2) Uani 1 1 d . . . C2 C 0.2282(6) 0.2837(3) 0.4685(3) 0.027(2) Uani 1 1 d . . . C3 C 0.3148(7) 0.2982(4) 0.4969(4) 0.043(3) Uani 1 1 d . . . H3A H 0.3698 0.2852 0.4811 0.052 Uiso 1 1 calc R . . H3B H 0.3198 0.3346 0.4975 0.052 Uiso 1 1 calc R . . C4 C 0.3151(9) 0.2796(4) 0.5455(4) 0.049(3) Uani 1 1 d . . . H4A H 0.3675 0.2945 0.5627 0.059 Uiso 1 1 calc R . . H4B H 0.3238 0.2434 0.5454 0.059 Uiso 1 1 calc R . . C5 C 0.2251(10) 0.2921(5) 0.5703(4) 0.058(4) Uani 1 1 d . . . H5A H 0.2258 0.2769 0.6014 0.069 Uiso 1 1 calc R . . H5B H 0.2206 0.3283 0.5743 0.069 Uiso 1 1 calc R . . C6 C 0.1436(8) 0.2742(4) 0.5440(3) 0.040(3) Uani 1 1 d . . . H6A H 0.0869 0.2840 0.5603 0.048 Uiso 1 1 calc R . . H6B H 0.1452 0.2377 0.5425 0.048 Uiso 1 1 calc R . . C7 C 0.1408(7) 0.2948(4) 0.4954(3) 0.029(2) Uani 1 1 d . . . H7A H 0.1320 0.3309 0.4970 0.035 Uiso 1 1 calc R . . H7B H 0.0873 0.2806 0.4786 0.035 Uiso 1 1 calc R . . C8 C 0.1118(5) 0.4334(3) 0.3032(3) 0.018(2) Uani 1 1 d . . . C9 C 0.0127(6) 0.4174(3) 0.3144(3) 0.017(2) Uani 1 1 d . . . C10 C -0.0435(6) 0.4645(3) 0.3252(3) 0.026(2) Uani 1 1 d . . . H10A H -0.0172 0.4806 0.3531 0.031 Uiso 1 1 calc R . . H10B H -0.0381 0.4879 0.2991 0.031 Uiso 1 1 calc R . . C11 C -0.1428(7) 0.4535(4) 0.3332(4) 0.034(3) Uani 1 1 d . . . H11A H -0.1768 0.4848 0.3375 0.040 Uiso 1 1 calc R . . H11B H -0.1490 0.4337 0.3617 0.040 Uiso 1 1 calc R . . C12 C -0.1850(7) 0.4253(4) 0.2923(4) 0.039(3) Uani 1 1 d . . . H12A H -0.2501 0.4174 0.2989 0.047 Uiso 1 1 calc R . . H12B H -0.1835 0.4461 0.2643 0.047 Uiso 1 1 calc R . . C13 C -0.1323(6) 0.3777(4) 0.2836(4) 0.033(3) Uani 1 1 d . . . H13A H -0.1378 0.3558 0.3108 0.039 Uiso 1 1 calc R . . H13B H -0.1593 0.3605 0.2565 0.039 Uiso 1 1 calc R . . C14 C -0.0331(6) 0.3883(4) 0.2750(3) 0.024(2) Uani 1 1 d . . . H14A H -0.0277 0.4072 0.2459 0.029 Uiso 1 1 calc R . . H14B H 0.0001 0.3567 0.2710 0.029 Uiso 1 1 calc R . . C15 C 0.3302(6) 0.3788(4) 0.2882(3) 0.025(2) Uani 1 1 d . . . C16 C 0.3189(7) 0.3240(3) 0.2718(3) 0.023(2) Uani 1 1 d . . . C17 C 0.2187(6) 0.3142(3) 0.2635(3) 0.025(2) Uani 1 1 d . . . H17A H 0.1941 0.3394 0.2419 0.030 Uiso 1 1 calc R . . H17B H 0.1857 0.3177 0.2930 0.030 Uiso 1 1 calc R . . C18 C 0.1988(8) 0.2625(4) 0.2432(4) 0.043(3) Uani 1 1 d . . . H18A H 0.2123 0.2373 0.2671 0.052 Uiso 1 1 calc R . . H18B H 0.1326 0.2601 0.2350 0.052 Uiso 1 1 calc R . . C19 C 0.2551(9) 0.2517(4) 0.2010(4) 0.049(3) Uani 1 1 d . . . H19A H 0.2342 0.2732 0.1753 0.059 Uiso 1 1 calc R . . H19B H 0.2451 0.2170 0.1916 0.059 Uiso 1 1 calc R . . C20 C 0.3575(8) 0.2601(3) 0.2099(4) 0.037(3) Uani 1 1 d . . . H20A H 0.3913 0.2554 0.1807 0.044 Uiso 1 1 calc R . . H20B H 0.3803 0.2353 0.2324 0.044 Uiso 1 1 calc R . . C21 C 0.3777(7) 0.3127(3) 0.2290(3) 0.027(2) Uani 1 1 d . . . H21A H 0.4438 0.3154 0.2374 0.032 Uiso 1 1 calc R . . H21B H 0.3643 0.3374 0.2046 0.032 Uiso 1 1 calc R . . C22 C 0.4353(6) 0.4996(3) 0.3477(3) 0.021(2) Uani 1 1 d . . . C23 C 0.5218(6) 0.5334(3) 0.3461(3) 0.018(2) Uani 1 1 d . . . C24 C 0.5830(6) 0.5188(3) 0.3055(3) 0.022(2) Uani 1 1 d . . . H24A H 0.6090 0.4856 0.3115 0.027 Uiso 1 1 calc R . . H24B H 0.5448 0.5168 0.2771 0.027 Uiso 1 1 calc R . . C25 C 0.6602(7) 0.5542(4) 0.2979(4) 0.040(3) Uani 1 1 d . . . H25A H 0.6933 0.5449 0.2694 0.048 Uiso 1 1 calc R . . H25B H 0.7043 0.5522 0.3242 0.048 Uiso 1 1 calc R . . C26 C 0.6243(8) 0.6084(4) 0.2932(4) 0.046(3) Uani 1 1 d . . . H26A H 0.6773 0.6310 0.2896 0.055 Uiso 1 1 calc R . . H26B H 0.5849 0.6112 0.2652 0.055 Uiso 1 1 calc R . . C27 C 0.5703(7) 0.6233(4) 0.3345(4) 0.034(3) Uani 1 1 d . . . H27A H 0.5465 0.6572 0.3302 0.041 Uiso 1 1 calc R . . H27B H 0.6107 0.6231 0.3623 0.041 Uiso 1 1 calc R . . C28 C 0.4906(6) 0.5881(3) 0.3414(4) 0.025(2) Uani 1 1 d . . . H28A H 0.4475 0.5910 0.3148 0.030 Uiso 1 1 calc R . . H28B H 0.4571 0.5977 0.3696 0.030 Uiso 1 1 calc R . . C29 C 0.2087(5) 0.5466(3) 0.3551(3) 0.0147(19) Uani 1 1 d . . . C30 C 0.1753(6) 0.5947(3) 0.3765(3) 0.022(2) Uani 1 1 d . . . C31 C 0.0729(6) 0.6014(4) 0.3677(3) 0.026(2) Uani 1 1 d . . . H31A H 0.0392 0.5741 0.3828 0.031 Uiso 1 1 calc R . . H31B H 0.0605 0.5994 0.3341 0.031 Uiso 1 1 calc R . . C32 C 0.0364(8) 0.6508(4) 0.3860(4) 0.051(3) Uani 1 1 d . . . H32A H -0.0286 0.6547 0.3761 0.062 Uiso 1 1 calc R . . H32B H 0.0380 0.6502 0.4202 0.062 Uiso 1 1 calc R . . C33 C 0.0909(9) 0.6943(5) 0.3693(5) 0.054(4) Uani 1 1 d . . . H33A H 0.0685 0.7246 0.3847 0.065 Uiso 1 1 calc R . . H33B H 0.0812 0.6982 0.3356 0.065 Uiso 1 1 calc R . . C34 C 0.1929(10) 0.6882(4) 0.3794(4) 0.050(4) Uani 1 1 d . . . H34A H 0.2038 0.6886 0.4132 0.060 Uiso 1 1 calc R . . H34B H 0.2271 0.7161 0.3658 0.060 Uiso 1 1 calc R . . C35 C 0.2286(8) 0.6398(4) 0.3593(4) 0.036(3) Uani 1 1 d . . . H35A H 0.2944 0.6359 0.3678 0.043 Uiso 1 1 calc R . . H35B H 0.2241 0.6412 0.3252 0.043 Uiso 1 1 calc R . . C36 C 0.3466(6) 0.6107(3) 0.2127(3) 0.022(2) Uani 1 1 d . . . C37 C 0.3482(6) 0.6662(3) 0.2193(3) 0.022(2) Uani 1 1 d . . . C38 C 0.2497(7) 0.6823(4) 0.2194(3) 0.030(3) Uani 1 1 d . . . H38A H 0.2166 0.6635 0.2434 0.037 Uiso 1 1 calc R . . H38B H 0.2214 0.6741 0.1891 0.037 Uiso 1 1 calc R . . C39 C 0.2373(7) 0.7378(4) 0.2286(4) 0.036(3) Uani 1 1 d . . . H39A H 0.1710 0.7452 0.2320 0.043 Uiso 1 1 calc R . . H39B H 0.2605 0.7568 0.2020 0.043 Uiso 1 1 calc R . . C40 C 0.2899(8) 0.7534(4) 0.2730(4) 0.044(3) Uani 1 1 d . . . H40A H 0.2858 0.7896 0.2765 0.052 Uiso 1 1 calc R . . H40B H 0.2604 0.7381 0.3001 0.052 Uiso 1 1 calc R . . C41 C 0.3902(8) 0.7383(4) 0.2719(4) 0.038(3) Uani 1 1 d . . . H41A H 0.4195 0.7459 0.3021 0.046 Uiso 1 1 calc R . . H41B H 0.4222 0.7577 0.2479 0.046 Uiso 1 1 calc R . . C42 C 0.4006(7) 0.6835(3) 0.2616(3) 0.028(2) Uani 1 1 d . . . H42A H 0.4668 0.6761 0.2574 0.033 Uiso 1 1 calc R . . H42B H 0.3793 0.6645 0.2886 0.033 Uiso 1 1 calc R . . C43 C 0.4430(5) 0.4888(3) 0.1615(3) 0.017(2) Uani 1 1 d . . . C44 C 0.5300(6) 0.4578(4) 0.1522(3) 0.023(2) Uani 1 1 d . . . C45 C 0.5139(6) 0.4043(4) 0.1645(4) 0.029(2) Uani 1 1 d . . . H45A H 0.4636 0.3912 0.1447 0.035 Uiso 1 1 calc R . . H45B H 0.4936 0.4023 0.1970 0.035 Uiso 1 1 calc R . . C46 C 0.5987(7) 0.3724(4) 0.1586(4) 0.039(3) Uani 1 1 d . . . H46A H 0.6123 0.3691 0.1253 0.047 Uiso 1 1 calc R . . H46B H 0.5865 0.3391 0.1711 0.047 Uiso 1 1 calc R . . C47 C 0.6828(7) 0.3946(4) 0.1837(4) 0.039(3) Uani 1 1 d . . . H47A H 0.6736 0.3926 0.2176 0.047 Uiso 1 1 calc R . . H47B H 0.7383 0.3751 0.1762 0.047 Uiso 1 1 calc R . . C48 C 0.6981(6) 0.4480(4) 0.1701(4) 0.034(3) Uani 1 1 d . . . H48A H 0.7498 0.4618 0.1885 0.041 Uiso 1 1 calc R . . H48B H 0.7148 0.4497 0.1370 0.041 Uiso 1 1 calc R . . C49 C 0.6131(6) 0.4783(3) 0.1780(3) 0.027(2) Uani 1 1 d . . . H49A H 0.6244 0.5125 0.1677 0.033 Uiso 1 1 calc R . . H49B H 0.5999 0.4791 0.2115 0.033 Uiso 1 1 calc R . . C50 C 0.2016(6) 0.4575(3) 0.1358(3) 0.021(2) Uani 1 1 d . . . C51 C 0.1298(5) 0.4176(3) 0.1224(3) 0.0140(7) Uani 1 1 d U . . C52 C 0.0407(6) 0.4266(4) 0.1497(3) 0.028(2) Uani 1 1 d . . . H52A H 0.0565 0.4288 0.1830 0.033 Uiso 1 1 calc R . . H52B H 0.0141 0.4586 0.1402 0.033 Uiso 1 1 calc R . . C53 C -0.0315(7) 0.3870(4) 0.1431(4) 0.036(3) Uani 1 1 d . . . H53A H -0.0547 0.3875 0.1108 0.043 Uiso 1 1 calc R . . H53B H -0.0840 0.3933 0.1638 0.043 Uiso 1 1 calc R . . C54 C 0.0116(8) 0.3352(4) 0.1542(4) 0.038(3) Uani 1 1 d . . . H54A H 0.0308 0.3340 0.1871 0.046 Uiso 1 1 calc R . . H54B H -0.0352 0.3092 0.1489 0.046 Uiso 1 1 calc R . . C55 C 0.0919(8) 0.3260(4) 0.1246(3) 0.035(3) Uani 1 1 d . . . H55A H 0.0713 0.3254 0.0919 0.042 Uiso 1 1 calc R . . H55B H 0.1178 0.2932 0.1322 0.042 Uiso 1 1 calc R . . C56 C 0.1673(7) 0.3647(3) 0.1302(3) 0.031(3) Uani 1 1 d . . . H56A H 0.2168 0.3581 0.1078 0.037 Uiso 1 1 calc R . . H56B H 0.1942 0.3624 0.1617 0.037 Uiso 1 1 calc R . . C57 C 0.1230(6) 0.5729(3) 0.1775(3) 0.023(2) Uani 1 1 d . . . C58 C 0.0246(6) 0.5893(3) 0.1894(3) 0.023(2) Uani 1 1 d . . . C59 C -0.0350(6) 0.5456(3) 0.2037(4) 0.028(2) Uani 1 1 d . . . H59A H -0.0467 0.5245 0.1763 0.033 Uiso 1 1 calc R . . H59B H -0.0007 0.5256 0.2268 0.033 Uiso 1 1 calc R . . C60 C -0.1271(6) 0.5608(4) 0.2242(4) 0.036(3) Uani 1 1 d . . . H60A H -0.1600 0.5309 0.2348 0.043 Uiso 1 1 calc R . . H60B H -0.1653 0.5766 0.1999 0.043 Uiso 1 1 calc R . . C61 C -0.1160(7) 0.5963(4) 0.2649(4) 0.044(3) Uani 1 1 d . . . H61A H -0.1773 0.6059 0.2766 0.053 Uiso 1 1 calc R . . H61B H -0.0813 0.5802 0.2903 0.053 Uiso 1 1 calc R . . C62 C -0.0645(7) 0.6417(4) 0.2485(4) 0.037(3) Uani 1 1 d . . . H62A H -0.0557 0.6647 0.2748 0.044 Uiso 1 1 calc R . . H62B H -0.1015 0.6588 0.2244 0.044 Uiso 1 1 calc R . . C63 C 0.0299(6) 0.6276(3) 0.2287(3) 0.025(2) Uani 1 1 d . . . H63A H 0.0601 0.6577 0.2169 0.029 Uiso 1 1 calc R . . H63B H 0.0691 0.6142 0.2540 0.029 Uiso 1 1 calc R . . C64 C 0.2850(6) 0.6690(3) 0.0572(3) 0.021(2) Uani 1 1 d . . . C65 C 0.2711(6) 0.7207(3) 0.0383(3) 0.025(2) Uani 1 1 d . . . C66 C 0.2646(10) 0.7244(5) -0.0135(4) 0.052(4) Uani 1 1 d . . . H66A H 0.2399 0.7572 -0.0219 0.063 Uiso 1 1 calc R . . H66B H 0.2207 0.6992 -0.0250 0.063 Uiso 1 1 calc R . . C67 C 0.3577(10) 0.7170(5) -0.0374(5) 0.071(4) Uani 1 1 d . . . H67A H 0.3757 0.6819 -0.0350 0.086 Uiso 1 1 calc R . . H67B H 0.3506 0.7250 -0.0707 0.086 Uiso 1 1 calc R . . C68 C 0.4320(11) 0.7479(6) -0.0172(7) 0.100(6) Uani 1 1 d . . . H68A H 0.4203 0.7828 -0.0254 0.120 Uiso 1 1 calc R . . H68B H 0.4914 0.7383 -0.0311 0.120 Uiso 1 1 calc R . . C69 C 0.4398(10) 0.7434(6) 0.0345(7) 0.093(6) Uani 1 1 d . . . H69A H 0.4878 0.7665 0.0459 0.112 Uiso 1 1 calc R . . H69B H 0.4597 0.7096 0.0425 0.112 Uiso 1 1 calc R . . C70 C 0.3488(9) 0.7547(4) 0.0588(5) 0.054(4) Uani 1 1 d . . . H70A H 0.3321 0.7898 0.0542 0.065 Uiso 1 1 calc R . . H70B H 0.3557 0.7487 0.0925 0.065 Uiso 1 1 calc R . . N1 N 0.2316(6) 0.2295(3) 0.4561(3) 0.041(2) Uani 1 1 d . . . H1A H 0.2302 0.2112 0.4824 0.061 Uiso 1 1 calc R . . H1B H 0.2845 0.2231 0.4406 0.061 Uiso 1 1 calc R . . H1C H 0.1823 0.2218 0.4379 0.061 Uiso 1 1 calc R . . N2 N 0.0181(5) 0.3857(3) 0.3572(3) 0.027(2) Uani 1 1 d . . . H2A H 0.0514 0.3581 0.3511 0.040 Uiso 1 1 calc R . . H2B H -0.0397 0.3770 0.3658 0.040 Uiso 1 1 calc R . . H2C H 0.0459 0.4029 0.3804 0.040 Uiso 1 1 calc R . . N3 N 0.3498(5) 0.2917(3) 0.3106(3) 0.026(2) Uani 1 1 d . . . H3C H 0.3432 0.2596 0.3022 0.039 Uiso 1 1 calc R . . H3D H 0.3152 0.2979 0.3359 0.039 Uiso 1 1 calc R . . H3E H 0.4101 0.2979 0.3173 0.039 Uiso 1 1 calc R . . N4 N 0.5710(5) 0.5276(3) 0.3909(3) 0.029(2) Uani 1 1 d . . . H4C H 0.5906 0.4959 0.3940 0.044 Uiso 1 1 calc R . . H4D H 0.5322 0.5351 0.4144 0.044 Uiso 1 1 calc R . . H4E H 0.6203 0.5483 0.3919 0.044 Uiso 1 1 calc R . . N5 N 0.1927(6) 0.5913(3) 0.4278(3) 0.030(2) Uani 1 1 d . . . H5C H 0.1738 0.6196 0.4417 0.045 Uiso 1 1 calc R . . H5D H 0.2540 0.5869 0.4333 0.045 Uiso 1 1 calc R . . H5E H 0.1609 0.5653 0.4395 0.045 Uiso 1 1 calc R . . N6 N 0.3947(6) 0.6876(3) 0.1760(3) 0.029(2) Uani 1 1 d . . . H6C H 0.3637 0.6774 0.1503 0.043 Uiso 1 1 calc R . . H6D H 0.4540 0.6769 0.1749 0.043 Uiso 1 1 calc R . . H6E H 0.3939 0.7211 0.1774 0.043 Uiso 1 1 calc R . . N7 N 0.5483(5) 0.4623(3) 0.1016(2) 0.0246(19) Uani 1 1 d . . . H7C H 0.5991 0.4444 0.0944 0.037 Uiso 1 1 calc R . . H7D H 0.5579 0.4946 0.0944 0.037 Uiso 1 1 calc R . . H7E H 0.4989 0.4508 0.0853 0.037 Uiso 1 1 calc R . . N8 N 0.1123(6) 0.4250(3) 0.0700(3) 0.033(2) Uani 1 1 d . . . H8A H 0.0705 0.4023 0.0598 0.050 Uiso 1 1 calc R . . H8B H 0.1660 0.4210 0.0546 0.050 Uiso 1 1 calc R . . H8C H 0.0900 0.4559 0.0649 0.050 Uiso 1 1 calc R . . N9 N -0.0150(5) 0.6127(3) 0.1463(3) 0.0234(19) Uani 1 1 d . . . H9A H -0.0735 0.6229 0.1518 0.035 Uiso 1 1 calc R . . H9B H -0.0153 0.5903 0.1229 0.035 Uiso 1 1 calc R . . H9C H 0.0201 0.6391 0.1382 0.035 Uiso 1 1 calc R . . N10 N 0.1844(6) 0.7398(3) 0.0587(3) 0.031(2) Uani 1 1 d . . . H10C H 0.1735 0.7709 0.0481 0.047 Uiso 1 1 calc R . . H10D H 0.1900 0.7404 0.0901 0.047 Uiso 1 1 calc R . . H10E H 0.1367 0.7199 0.0504 0.047 Uiso 1 1 calc R . . O1 O 0.2127(5) 0.3570(2) 0.4224(3) 0.0353(19) Uani 1 1 d . . . O1W O 0.1264(5) 0.4405(3) 0.4325(2) 0.0315(18) Uani 1 1 d . . . O2W O 0.3243(6) 0.4637(3) 0.4702(2) 0.047(2) Uani 1 1 d . . . O3W O 0.4110(4) 0.3746(2) 0.4212(2) 0.0317(18) Uani 1 1 d . . . O4W O 0.1661(5) 0.5637(3) 0.0403(2) 0.0337(18) Uani 1 1 d . . . O5W O 0.3511(5) 0.5221(3) 0.0294(2) 0.0321(18) Uani 1 1 d . . . O6W O 0.4566(5) 0.6040(3) 0.0859(3) 0.043(2) Uani 1 1 d . . . O7W O 0.6463(6) 0.5439(4) 0.0725(3) 0.063(3) Uani 1 1 d . . . O8W O 0.6753(5) 0.4446(3) 0.3981(3) 0.041(2) Uani 1 1 d . . . O9W O 0.2996(5) 0.5783(3) -0.0484(2) 0.038(2) Uani 1 1 d . . . O2 O 0.2514(6) 0.2872(3) 0.3874(2) 0.043(2) Uani 1 1 d . . . O3 O 0.1251(4) 0.4565(2) 0.2661(2) 0.0279(17) Uani 1 1 d . . . O4 O 0.1725(4) 0.4237(3) 0.3320(2) 0.0296(17) Uani 1 1 d . . . O5 O 0.3494(4) 0.3840(2) 0.3301(2) 0.0230(15) Uani 1 1 d . . . O6 O 0.3171(4) 0.4103(2) 0.2585(2) 0.0225(15) Uani 1 1 d . . . O7 O 0.4238(4) 0.4774(2) 0.3844(2) 0.0278(17) Uani 1 1 d . . . O8 O 0.3864(4) 0.4976(2) 0.3115(2) 0.0307(17) Uani 1 1 d . . . O9 O 0.2058(4) 0.5445(2) 0.3120(2) 0.0247(16) Uani 1 1 d . . . O10W O 0.0705(5) 0.5270(2) 0.4721(2) 0.0316(18) Uani 1 1 d . . . O10 O 0.2319(5) 0.5136(2) 0.3833(2) 0.0304(17) Uani 1 1 d . . . O11 O 0.3361(4) 0.5843(2) 0.2474(2) 0.0213(15) Uani 1 1 d . . . O12 O 0.3513(5) 0.5956(3) 0.1717(2) 0.0320(18) Uani 1 1 d . . . O13 O 0.4050(5) 0.5076(2) 0.1262(2) 0.0320(17) Uani 1 1 d . . . O14 O 0.4161(4) 0.4909(2) 0.2018(2) 0.0262(16) Uani 1 1 d . . . O15 O 0.2316(4) 0.4551(2) 0.1756(2) 0.0279(17) Uani 1 1 d . . . O16 O 0.2143(4) 0.4902(2) 0.1063(2) 0.0259(16) Uani 1 1 d . . . O17 O 0.1555(4) 0.5877(2) 0.1407(2) 0.0257(16) Uani 1 1 d . . . O18 O 0.1637(4) 0.5477(3) 0.2076(2) 0.0323(18) Uani 1 1 d . . . O19 O 0.2739(4) 0.6631(2) 0.0996(2) 0.0242(16) Uani 1 1 d . . . O20 O 0.3046(5) 0.6347(2) 0.0310(2) 0.0329(18) Uani 1 1 d . . . O21 O -0.0241(7) 0.7189(3) 0.6763(3) 0.069(3) Uani 1 1 d . . . O22 O -0.0115(7) 0.7276(4) 0.5973(3) 0.066(3) Uani 1 1 d . . . O23 O 0.0731(5) 0.7808(3) 0.6455(3) 0.043(2) Uani 1 1 d . . . O24 O -0.0863(6) 0.7869(3) 0.6396(4) 0.073(3) Uani 1 1 d . . . O25 O 0.1061(6) 0.4171(3) 0.5362(3) 0.051(2) Uani 1 1 d . . . O26 O 0.1415(9) 0.4955(4) 0.5639(3) 0.096(4) Uani 1 1 d . . . O27 O 0.1525(6) 0.4285(4) 0.6146(3) 0.057(3) Uani 1 1 d . . . O28 O 0.2594(5) 0.4348(4) 0.5566(3) 0.064(3) Uani 1 1 d . . . O29 O 0.1277(6) 0.9670(3) 0.4260(3) 0.055(2) Uani 1 1 d . . . O30 O 0.0089(6) 1.0250(3) 0.4295(3) 0.063(3) Uani 1 1 d . . . O31 O 0.1536(6) 1.0494(3) 0.4068(3) 0.066(3) Uani 1 1 d . . . O32 O 0.1309(7) 1.0277(3) 0.4835(3) 0.064(3) Uani 1 1 d . . . O33 O 0.0498(6) 0.6511(3) 0.0547(2) 0.054(2) Uani 1 1 d . . . O34 O -0.0931(5) 0.6573(3) 0.0137(3) 0.059(3) Uani 1 1 d . . . O35 O 0.0385(6) 0.6258(3) -0.0216(3) 0.050(2) Uani 1 1 d . . . O36 O 0.0303(6) 0.7097(3) -0.0036(3) 0.048(2) Uani 1 1 d . . . O37 O 0.5903(12) 0.8495(6) 0.4313(4) 0.144(6) Uani 1 1 d . . . O38 O 0.6867(14) 0.8978(15) 0.4612(8) 0.453(19) Uani 1 1 d . . . O39 O 0.623(2) 0.8531(9) 0.5080(6) 0.294(13) Uani 1 1 d . . . O40 O 0.5516(11) 0.9049(6) 0.4824(6) 0.154(6) Uani 1 1 d . . . O41 O 0.3109(6) 0.6714(4) 0.6603(4) 0.075(3) Uani 1 1 d . . . O42 O 0.4378(6) 0.6304(4) 0.6340(4) 0.103(4) Uani 1 1 d . . . O43 O 0.4164(11) 0.6438(5) 0.7120(4) 0.126(5) Uani 1 1 d . . . O44 O 0.4561(5) 0.7095(3) 0.6656(3) 0.045(2) Uani 1 1 d . . . O45 O 0.4207(7) 0.1191(4) 0.3387(4) 0.093(4) Uani 1 1 d . . . O46 O 0.3595(13) 0.1792(7) 0.3837(5) 0.228(7) Uani 1 1 d . . . O47 O 0.2741(10) 0.1357(9) 0.3429(12) 0.288(15) Uani 1 1 d . . . O48 O 0.3583(17) 0.1838(5) 0.3096(5) 0.237(10) Uani 1 1 d . . . O49 O 0.4310(8) 0.6138(5) 0.5215(3) 0.092(4) Uani 1 1 d . . . O50 O 0.5328(6) 0.6116(4) 0.4606(4) 0.079(3) Uani 1 1 d . . . O51 O 0.4362(12) 0.5503(5) 0.4661(6) 0.231(7) Uani 1 1 d . . . O52 O 0.3793(6) 0.6174(7) 0.4503(5) 0.153(7) Uani 1 1 d . . . O53 O 0.0455(6) 0.6093(4) 0.5432(3) 0.065(3) Uani 1 1 d . . . O54 O 0.2007(6) 0.5931(3) 0.5281(2) 0.043(2) Uani 1 1 d . . . O55 O 0.1303(7) 0.6652(3) 0.5037(3) 0.057(3) Uani 1 1 d . . . O56 O 0.1578(6) 0.6538(3) 0.5827(2) 0.047(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd1 0.0183(2) 0.0144(2) 0.0162(2) 0.00152(19) 0.00073(17) 0.00027(19) Nd2 0.0197(2) 0.0117(2) 0.0160(2) 0.00153(18) -0.00092(17) 0.00139(18) Nd3 0.01214(18) 0.00902(19) 0.01316(19) 0.00154(17) 0.00125(15) -0.00166(17) Cl1 0.0373(12) 0.0221(11) 0.0349(13) 0.0012(10) 0.0018(11) -0.0087(10) Cl2 0.0332(12) 0.0305(12) 0.0262(12) 0.0004(10) -0.0045(10) -0.0049(10) Cl3 0.0349(12) 0.0335(13) 0.0293(12) -0.0016(10) -0.0014(10) -0.0031(10) Cl4 0.0352(12) 0.0337(13) 0.0337(13) -0.0061(11) -0.0074(11) 0.0074(11) Cl5 0.0442(14) 0.0312(13) 0.0351(13) 0.0064(11) 0.0041(11) 0.0051(11) Cl6 0.0403(14) 0.0346(13) 0.0423(14) -0.0096(12) 0.0087(12) -0.0024(12) Cl7 0.0382(13) 0.0351(13) 0.0373(14) 0.0085(11) 0.0003(11) 0.0042(11) Cl8 0.0419(15) 0.0704(19) 0.0406(15) -0.0238(14) -0.0053(12) -0.0178(14) Cl9 0.0413(13) 0.0273(12) 0.0196(11) -0.0025(9) 0.0014(10) -0.0068(10) C1 0.017(4) 0.036(5) 0.030(5) 0.001(4) 0.002(4) -0.007(4) C2 0.025(5) 0.021(5) 0.035(5) 0.001(4) 0.005(4) 0.001(4) C3 0.035(6) 0.047(7) 0.047(7) 0.008(6) -0.011(5) -0.017(5) C4 0.064(8) 0.039(6) 0.045(7) 0.017(5) -0.009(6) 0.001(6) C5 0.106(10) 0.043(7) 0.025(6) -0.002(5) -0.013(6) -0.021(7) C6 0.050(6) 0.044(6) 0.026(5) 0.013(5) 0.008(5) -0.003(5) C7 0.039(5) 0.019(5) 0.028(5) 0.001(4) 0.009(4) -0.001(4) C8 0.014(4) 0.021(4) 0.018(4) -0.007(4) 0.000(3) 0.000(4) C9 0.018(4) 0.017(4) 0.015(4) 0.001(3) -0.005(3) -0.002(3) C10 0.031(5) 0.024(5) 0.022(5) -0.001(4) -0.003(4) 0.002(4) C11 0.031(5) 0.033(5) 0.037(6) 0.009(5) 0.014(4) 0.011(4) C12 0.035(5) 0.052(7) 0.031(5) 0.010(5) -0.010(5) -0.002(5) C13 0.026(5) 0.039(6) 0.033(5) 0.004(5) -0.004(4) -0.015(4) C14 0.023(4) 0.036(5) 0.013(4) -0.002(4) -0.003(4) -0.010(4) C15 0.016(4) 0.034(5) 0.024(5) 0.005(4) 0.000(4) 0.007(4) C16 0.040(5) 0.015(4) 0.015(4) 0.007(4) -0.002(4) 0.003(4) C17 0.032(5) 0.007(4) 0.035(5) 0.000(4) 0.004(4) -0.002(4) C18 0.056(7) 0.019(5) 0.055(7) -0.002(5) -0.012(6) -0.010(5) C19 0.084(8) 0.027(5) 0.036(6) -0.016(5) -0.021(6) 0.016(6) C20 0.066(7) 0.012(4) 0.033(5) 0.003(4) 0.012(5) 0.006(5) C21 0.042(5) 0.014(4) 0.025(5) 0.002(4) 0.007(4) 0.011(4) C22 0.022(4) 0.022(4) 0.020(4) -0.005(4) -0.010(3) 0.000(4) C23 0.019(4) 0.017(4) 0.017(4) 0.006(3) -0.004(3) 0.005(3) C24 0.011(4) 0.028(5) 0.028(5) 0.001(4) 0.004(4) 0.004(4) C25 0.024(5) 0.038(6) 0.058(7) -0.002(5) 0.007(5) -0.009(5) C26 0.040(6) 0.038(6) 0.061(7) 0.007(6) 0.016(6) -0.024(5) C27 0.030(5) 0.028(5) 0.044(6) 0.009(5) -0.011(5) -0.005(4) C28 0.018(4) 0.015(4) 0.041(6) -0.006(4) -0.002(4) -0.003(4) C29 0.011(4) 0.014(4) 0.019(4) 0.000(3) 0.004(3) 0.002(3) C30 0.024(4) 0.025(5) 0.016(4) -0.004(4) 0.001(4) 0.006(4) C31 0.017(4) 0.044(6) 0.016(4) -0.005(4) 0.004(4) 0.005(4) C32 0.054(7) 0.048(7) 0.052(7) -0.002(6) 0.010(6) 0.029(6) C33 0.063(8) 0.045(7) 0.056(8) -0.011(6) 0.008(6) 0.021(6) C34 0.097(10) 0.014(5) 0.038(6) -0.001(5) 0.011(6) -0.009(6) C35 0.056(6) 0.023(5) 0.029(5) -0.003(4) 0.010(5) -0.015(5) C36 0.021(4) 0.029(5) 0.017(4) -0.002(4) -0.002(4) -0.008(4) C37 0.035(5) 0.015(4) 0.017(4) 0.004(4) -0.002(4) -0.014(4) C38 0.040(5) 0.024(5) 0.027(5) 0.000(4) 0.000(4) -0.005(4) C39 0.039(6) 0.030(5) 0.039(6) -0.005(5) -0.004(5) 0.001(5) C40 0.064(7) 0.025(5) 0.042(6) -0.015(5) 0.000(6) -0.003(5) C41 0.065(7) 0.021(5) 0.028(5) -0.004(4) -0.012(5) -0.002(5) C42 0.040(5) 0.023(5) 0.020(5) 0.003(4) -0.008(4) -0.008(4) C43 0.010(4) 0.020(4) 0.021(4) -0.007(4) 0.006(3) -0.005(3) C44 0.023(4) 0.032(5) 0.013(4) 0.001(4) 0.003(4) -0.001(4) C45 0.024(5) 0.028(5) 0.035(5) -0.001(4) 0.005(4) 0.002(4) C46 0.046(6) 0.023(5) 0.047(6) 0.004(5) 0.004(5) 0.009(5) C47 0.033(5) 0.053(7) 0.032(6) 0.011(5) -0.008(5) 0.017(5) C48 0.010(4) 0.050(6) 0.041(6) -0.003(5) -0.010(4) 0.015(4) C49 0.033(5) 0.023(5) 0.026(5) 0.003(4) -0.001(4) -0.001(4) C50 0.023(4) 0.021(4) 0.017(4) -0.002(4) 0.005(4) 0.009(4) C51 0.0140(9) 0.0145(10) 0.0137(10) 0.0006(7) 0.0002(7) -0.0001(7) C52 0.030(5) 0.040(6) 0.013(4) 0.001(4) -0.002(4) 0.002(5) C53 0.028(5) 0.038(6) 0.043(6) -0.008(5) 0.005(5) -0.012(5) C54 0.056(7) 0.025(5) 0.034(6) 0.001(5) -0.005(5) -0.010(5) C55 0.061(7) 0.019(5) 0.025(5) -0.011(4) -0.004(5) -0.007(5) C56 0.043(6) 0.021(5) 0.028(5) -0.005(4) -0.005(4) 0.010(4) C57 0.037(5) 0.013(4) 0.019(4) -0.009(4) -0.004(4) 0.001(4) C58 0.027(5) 0.026(5) 0.017(4) 0.007(4) -0.001(4) 0.010(4) C59 0.018(4) 0.022(5) 0.043(6) 0.003(4) 0.010(4) -0.001(4) C60 0.017(4) 0.043(6) 0.048(6) -0.022(5) 0.000(4) 0.005(4) C61 0.022(5) 0.045(6) 0.066(7) -0.020(6) 0.020(5) 0.000(5) C62 0.031(5) 0.038(6) 0.041(6) -0.020(5) 0.009(5) -0.006(5) C63 0.029(5) 0.025(5) 0.019(4) -0.004(4) -0.005(4) -0.003(4) C64 0.018(4) 0.024(5) 0.022(5) 0.002(4) -0.004(4) -0.002(4) C65 0.028(5) 0.018(4) 0.029(5) 0.009(4) 0.004(4) 0.009(4) C66 0.086(9) 0.046(7) 0.026(6) 0.010(5) 0.007(6) 0.019(7) C67 0.100(10) 0.050(8) 0.066(8) 0.006(7) 0.047(8) -0.001(8) C68 0.089(10) 0.055(9) 0.158(15) -0.004(10) 0.085(10) -0.005(8) C69 0.056(9) 0.061(10) 0.163(18) -0.017(11) 0.036(10) -0.013(8) C70 0.062(8) 0.022(6) 0.079(9) 0.006(6) 0.007(7) -0.009(6) N1 0.049(5) 0.031(5) 0.042(5) 0.002(4) 0.012(4) -0.013(4) N2 0.030(4) 0.030(4) 0.021(4) 0.003(3) 0.005(3) -0.001(4) N3 0.031(4) 0.027(4) 0.020(4) 0.009(3) -0.001(3) 0.007(3) N4 0.028(4) 0.029(4) 0.031(4) -0.003(4) -0.014(3) -0.006(4) N5 0.043(5) 0.030(4) 0.017(4) 0.002(3) 0.006(4) -0.002(4) N6 0.034(4) 0.027(4) 0.026(4) 0.004(4) -0.003(4) -0.008(4) N7 0.023(4) 0.032(4) 0.019(4) 0.000(3) 0.004(3) 0.011(3) N8 0.052(5) 0.026(4) 0.021(4) -0.003(4) -0.007(4) -0.004(4) N9 0.032(4) 0.010(3) 0.028(4) -0.001(3) -0.008(3) 0.006(3) N10 0.042(5) 0.014(4) 0.038(5) 0.001(3) -0.002(4) 0.010(4) O1 0.038(4) 0.023(3) 0.045(4) 0.014(3) -0.001(3) -0.008(3) O1W 0.044(4) 0.041(4) 0.010(3) -0.012(3) 0.013(3) 0.001(3) O2W 0.055(5) 0.063(5) 0.022(4) -0.005(4) -0.003(3) -0.011(4) O3W 0.031(3) 0.030(4) 0.034(4) 0.010(3) -0.009(3) 0.010(3) O4W 0.034(4) 0.032(4) 0.035(4) 0.008(3) -0.014(3) 0.003(3) O5W 0.044(4) 0.035(4) 0.017(3) -0.004(3) 0.000(3) 0.008(3) O6W 0.031(4) 0.048(5) 0.051(5) 0.017(4) 0.008(3) -0.003(3) O7W 0.052(5) 0.071(6) 0.066(6) 0.035(5) 0.007(4) 0.001(5) O8W 0.026(4) 0.034(4) 0.063(5) 0.002(4) -0.007(4) 0.004(3) O9W 0.055(4) 0.040(4) 0.020(3) -0.009(3) 0.002(3) 0.008(4) O2 0.073(5) 0.033(4) 0.022(4) -0.001(3) 0.009(4) -0.003(4) O3 0.024(3) 0.036(4) 0.025(3) 0.005(3) 0.005(3) -0.010(3) O4 0.024(3) 0.038(4) 0.026(3) -0.005(3) -0.005(3) 0.001(3) O5 0.024(3) 0.028(3) 0.017(3) -0.004(3) -0.001(3) 0.000(3) O6 0.035(3) 0.013(3) 0.019(3) 0.000(3) 0.000(3) 0.010(3) O7 0.026(3) 0.037(4) 0.020(3) 0.001(3) 0.001(3) -0.009(3) O8 0.030(3) 0.028(3) 0.034(4) -0.004(3) -0.011(3) 0.004(3) O9 0.033(3) 0.022(3) 0.019(3) 0.000(3) 0.005(3) 0.007(3) O10W 0.037(4) 0.027(4) 0.030(4) -0.006(3) 0.007(3) -0.003(3) O10 0.046(4) 0.017(3) 0.028(3) 0.004(3) 0.007(3) 0.009(3) O11 0.028(3) 0.016(3) 0.020(3) 0.002(3) 0.001(3) -0.006(3) O12 0.035(4) 0.030(4) 0.030(4) -0.002(3) -0.004(3) 0.003(3) O13 0.042(4) 0.030(4) 0.023(3) -0.002(3) 0.001(3) 0.015(3) O14 0.027(3) 0.017(3) 0.035(4) -0.003(3) 0.013(3) -0.003(3) O15 0.035(4) 0.025(3) 0.024(3) -0.005(3) -0.008(3) -0.001(3) O16 0.033(3) 0.012(3) 0.033(3) 0.006(3) -0.003(3) -0.010(3) O17 0.030(3) 0.024(3) 0.024(3) -0.008(3) 0.006(3) -0.007(3) O18 0.027(3) 0.033(4) 0.036(4) -0.001(3) -0.008(3) 0.012(3) O19 0.028(3) 0.018(3) 0.027(3) 0.002(3) 0.002(3) -0.002(3) O20 0.059(4) 0.020(3) 0.020(3) 0.001(3) 0.006(3) 0.011(3) O21 0.082(6) 0.055(5) 0.069(6) 0.034(5) 0.018(5) -0.008(5) O22 0.075(6) 0.075(6) 0.048(5) -0.020(5) -0.004(5) -0.027(5) O23 0.038(4) 0.046(5) 0.045(4) 0.001(4) -0.004(4) -0.011(4) O24 0.040(5) 0.040(5) 0.141(9) 0.011(6) -0.007(6) 0.003(4) O25 0.057(5) 0.060(5) 0.034(4) -0.007(4) -0.019(4) -0.019(4) O26 0.159(10) 0.075(7) 0.054(6) -0.016(5) -0.049(6) 0.012(7) O27 0.064(5) 0.077(6) 0.030(4) 0.007(4) 0.003(4) -0.019(5) O28 0.037(4) 0.122(8) 0.032(4) 0.019(5) -0.005(4) -0.011(5) O29 0.063(5) 0.054(5) 0.049(5) -0.023(4) -0.018(4) 0.014(4) O30 0.045(5) 0.059(6) 0.084(7) -0.015(5) 0.001(5) 0.017(4) O31 0.063(6) 0.067(6) 0.068(6) 0.036(5) -0.005(5) -0.016(5) O32 0.110(7) 0.058(5) 0.024(4) -0.022(4) -0.001(4) 0.002(5) O33 0.074(6) 0.066(6) 0.021(4) -0.008(4) -0.012(4) 0.014(5) O34 0.035(4) 0.046(5) 0.096(7) -0.022(5) -0.003(4) 0.007(4) O35 0.061(5) 0.055(5) 0.035(4) -0.023(4) -0.009(4) 0.019(4) O36 0.054(5) 0.031(4) 0.061(5) 0.009(4) -0.012(4) -0.006(4) O37 0.236(16) 0.128(12) 0.066(7) -0.022(8) -0.066(9) 0.031(12) O38 0.230(14) 0.91(6) 0.221(17) -0.25(3) 0.171(13) -0.34(2) O39 0.54(3) 0.23(2) 0.108(11) 0.080(12) -0.168(16) -0.14(2) O40 0.165(12) 0.126(11) 0.171(15) -0.038(11) 0.011(12) 0.084(10) O41 0.039(5) 0.068(6) 0.119(9) -0.021(6) -0.002(5) -0.013(5) O42 0.053(5) 0.088(6) 0.170(9) -0.091(6) 0.048(6) -0.026(5) O43 0.211(13) 0.105(8) 0.061(7) 0.028(6) -0.025(8) -0.085(9) O44 0.033(4) 0.033(4) 0.070(5) 0.005(4) -0.002(4) 0.003(3) O45 0.099(7) 0.118(8) 0.063(6) -0.006(6) -0.001(6) 0.076(6) O46 0.275(15) 0.296(16) 0.112(9) -0.135(10) -0.113(9) 0.205(13) O47 0.044(8) 0.23(2) 0.59(4) -0.13(3) 0.072(15) -0.014(11) O48 0.53(3) 0.045(7) 0.138(10) 0.023(7) 0.189(14) 0.063(12) O49 0.077(7) 0.151(11) 0.049(6) -0.022(7) -0.006(5) 0.002(7) O50 0.044(5) 0.096(8) 0.097(7) -0.039(6) 0.001(5) -0.010(5) O51 0.323(15) 0.117(8) 0.258(15) -0.116(9) 0.206(12) -0.159(9) O52 0.014(4) 0.29(2) 0.151(11) 0.080(13) -0.020(6) 0.009(8) O53 0.057(5) 0.079(6) 0.058(5) -0.026(5) 0.029(4) -0.025(5) O54 0.063(5) 0.040(4) 0.025(4) 0.000(3) 0.002(4) 0.018(4) O55 0.107(7) 0.037(4) 0.028(4) 0.011(4) 0.004(4) 0.012(5) O56 0.082(6) 0.032(4) 0.026(4) -0.012(3) -0.010(4) -0.002(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd1 O4 2.369(6) . ? Nd1 O5 2.384(6) . ? Nd1 O1 2.397(7) . ? Nd1 O10 2.415(6) . ? Nd1 O7 2.421(6) . ? Nd1 O2W 2.506(7) . ? Nd1 O3W 2.510(6) . ? Nd1 O1W 2.599(7) . ? Nd2 O12 2.365(7) . ? Nd2 O13 2.401(7) . ? Nd2 O16 2.428(6) . ? Nd2 O17 2.440(6) . ? Nd2 O5W 2.504(6) . ? Nd2 O4W 2.528(7) . ? Nd2 O6W 2.563(7) . ? Nd2 O19 2.603(6) . ? Nd2 O20 2.680(6) . ? Nd2 C64 3.003(9) . ? Nd3 O8 2.421(6) . ? Nd3 O18 2.428(6) . ? Nd3 O14 2.440(6) . ? Nd3 O6 2.447(6) . ? Nd3 O15 2.464(6) . ? Nd3 O9 2.488(6) . ? Nd3 O11 2.514(6) . ? Nd3 O3 2.527(6) . ? Cl1 O22 1.410(9) . ? Cl1 O21 1.414(9) . ? Cl1 O24 1.431(9) . ? Cl1 O23 1.448(8) . ? Cl2 O27 1.424(8) . ? Cl2 O28 1.436(9) . ? Cl2 O26 1.442(12) . ? Cl2 O25 1.450(8) . ? Cl3 O32 1.418(8) . ? Cl3 O29 1.426(9) . ? Cl3 O30 1.434(9) . ? Cl3 O31 1.435(9) . ? Cl4 O33 1.430(8) . ? Cl4 O35 1.431(8) . ? Cl4 O36 1.435(8) . ? Cl4 O34 1.439(8) . ? Cl5 O38 1.15(2) . ? Cl5 O39 1.268(18) . ? Cl5 O40 1.314(14) . ? Cl5 O37 1.405(13) . ? Cl6 O41 1.374(9) . ? Cl6 O43 1.394(12) . ? Cl6 O42 1.424(10) . ? Cl6 O44 1.468(8) . ? Cl7 O48 1.237(14) . ? Cl7 O47 1.269(16) . ? Cl7 O46 1.329(14) . ? Cl7 O45 1.411(10) . ? Cl8 O51 1.317(14) . ? Cl8 O52 1.332(12) . ? Cl8 O49 1.390(11) . ? Cl8 O50 1.416(10) . ? Cl9 O53 1.405(9) . ? Cl9 O55 1.420(8) . ? Cl9 O54 1.433(8) . ? Cl9 O56 1.438(7) . ? C1 O2 1.216(12) . ? C1 O1 1.285(12) . ? C1 C2 1.540(14) . ? C2 N1 1.514(12) . ? C2 C7 1.526(13) . ? C2 C3 1.546(14) . ? C3 C4 1.493(16) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.535(19) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.484(17) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.511(13) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 O4 1.234(10) . ? C8 O3 1.260(10) . ? C8 C9 1.541(11) . ? C9 N2 1.508(11) . ? C9 C14 1.532(12) . ? C9 C10 1.549(12) . ? C10 C11 1.494(13) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.531(15) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.522(15) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.492(13) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 O6 1.225(11) . ? C15 O5 1.248(11) . ? C15 C16 1.567(13) . ? C16 N3 1.488(11) . ? C16 C17 1.497(13) . ? C16 C21 1.541(13) . ? C17 C18 1.546(13) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.505(17) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.523(17) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.557(13) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 O7 1.236(11) . ? C22 O8 1.258(10) . ? C22 C23 1.556(12) . ? C23 N4 1.482(11) . ? C23 C24 1.532(12) . ? C23 C28 1.555(12) . ? C24 C25 1.495(13) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.565(16) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.492(16) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.516(13) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 O9 1.248(10) . ? C29 O10 1.253(10) . ? C29 C30 1.527(12) . ? C30 N5 1.505(11) . ? C30 C31 1.516(12) . ? C30 C35 1.532(13) . ? C31 C32 1.537(15) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.504(18) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.516(18) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.528(15) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 O11 1.244(11) . ? C36 O12 1.258(11) . ? C36 C37 1.518(12) . ? C37 C38 1.495(14) . ? C37 C42 1.507(12) . ? C37 N6 1.542(11) . ? C38 C39 1.539(14) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.546(15) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.513(16) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.525(13) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 O14 1.234(10) . ? C43 O13 1.262(11) . ? C43 C44 1.544(12) . ? C44 N7 1.494(11) . ? C44 C45 1.512(13) . ? C44 C49 1.517(13) . ? C45 C46 1.517(14) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 C47 1.537(15) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C48 1.519(15) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 C49 1.501(13) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 O15 1.229(11) . ? C50 O16 1.245(11) . ? C50 C51 1.550(12) . ? C51 C52 1.543(12) . ? C51 N8 1.546(11) . ? C51 C56 1.550(12) . ? C52 C53 1.511(14) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C54 1.569(15) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 C55 1.476(15) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C56 1.524(14) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 O17 1.235(11) . ? C57 O18 1.252(11) . ? C57 C58 1.538(13) . ? C58 N9 1.508(11) . ? C58 C59 1.528(13) . ? C58 C63 1.540(13) . ? C59 C60 1.525(13) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 C61 1.528(15) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 C62 1.518(15) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 C63 1.541(13) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 O20 1.235(11) . ? C64 O19 1.248(11) . ? C64 C65 1.518(12) . ? C65 N10 1.489(12) . ? C65 C66 1.503(14) . ? C65 C70 1.569(15) . ? C66 C67 1.539(19) . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? C67 C68 1.48(2) . ? C67 H67A 0.9900 . ? C67 H67B 0.9900 . ? C68 C69 1.50(3) . ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? C69 C70 1.54(2) . ? C69 H69A 0.9900 . ? C69 H69B 0.9900 . ? C70 H70A 0.9900 . ? C70 H70B 0.9900 . ? N1 H1A 0.9100 . ? N1 H1B 0.9100 . ? N1 H1C 0.9100 . ? N2 H2A 0.9100 . ? N2 H2B 0.9100 . ? N2 H2C 0.9100 . ? N3 H3C 0.9100 . ? N3 H3D 0.9100 . ? N3 H3E 0.9100 . ? N4 H4C 0.9100 . ? N4 H4D 0.9100 . ? N4 H4E 0.9100 . ? N5 H5C 0.9100 . ? N5 H5D 0.9100 . ? N5 H5E 0.9100 . ? N6 H6C 0.9100 . ? N6 H6D 0.9100 . ? N6 H6E 0.9100 . ? N7 H7C 0.9100 . ? N7 H7D 0.9100 . ? N7 H7E 0.9100 . ? N8 H8A 0.9100 . ? N8 H8B 0.9100 . ? N8 H8C 0.9100 . ? N9 H9A 0.9100 . ? N9 H9B 0.9100 . ? N9 H9C 0.9100 . ? N10 H10C 0.9100 . ? N10 H10D 0.9100 . ? N10 H10E 0.9100 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Nd1 O5 71.8(2) . . ? O4 Nd1 O1 85.3(2) . . ? O5 Nd1 O1 91.5(2) . . ? O4 Nd1 O10 76.9(2) . . ? O5 Nd1 O10 122.5(2) . . ? O1 Nd1 O10 132.7(2) . . ? O4 Nd1 O7 122.5(2) . . ? O5 Nd1 O7 82.5(2) . . ? O1 Nd1 O7 147.2(2) . . ? O10 Nd1 O7 75.4(2) . . ? O4 Nd1 O2W 146.9(2) . . ? O5 Nd1 O2W 141.2(2) . . ? O1 Nd1 O2W 94.1(3) . . ? O10 Nd1 O2W 79.4(3) . . ? O7 Nd1 O2W 72.3(2) . . ? O4 Nd1 O3W 134.5(2) . . ? O5 Nd1 O3W 69.3(2) . . ? O1 Nd1 O3W 73.0(2) . . ? O10 Nd1 O3W 145.6(2) . . ? O7 Nd1 O3W 74.7(2) . . ? O2W Nd1 O3W 75.7(2) . . ? O4 Nd1 O1W 74.8(2) . . ? O5 Nd1 O1W 139.2(2) . . ? O1 Nd1 O1W 62.8(2) . . ? O10 Nd1 O1W 70.3(2) . . ? O7 Nd1 O1W 136.3(2) . . ? O2W Nd1 O1W 75.5(2) . . ? O3W Nd1 O1W 124.4(2) . . ? O12 Nd2 O13 73.1(2) . . ? O12 Nd2 O16 111.2(2) . . ? O13 Nd2 O16 72.7(2) . . ? O12 Nd2 O17 76.7(2) . . ? O13 Nd2 O17 122.7(2) . . ? O16 Nd2 O17 74.7(2) . . ? O12 Nd2 O5W 139.8(2) . . ? O13 Nd2 O5W 73.2(2) . . ? O16 Nd2 O5W 78.5(2) . . ? O17 Nd2 O5W 141.5(2) . . ? O12 Nd2 O4W 148.8(2) . . ? O13 Nd2 O4W 132.5(2) . . ? O16 Nd2 O4W 70.0(2) . . ? O17 Nd2 O4W 73.7(2) . . ? O5W Nd2 O4W 71.3(2) . . ? O12 Nd2 O6W 73.1(2) . . ? O13 Nd2 O6W 73.2(2) . . ? O16 Nd2 O6W 142.3(2) . . ? O17 Nd2 O6W 139.1(2) . . ? O5W Nd2 O6W 76.8(2) . . ? O4W Nd2 O6W 126.2(2) . . ? O12 Nd2 O19 73.7(2) . . ? O13 Nd2 O19 138.9(2) . . ? O16 Nd2 O19 143.1(2) . . ? O17 Nd2 O19 71.0(2) . . ? O5W Nd2 O19 122.5(2) . . ? O4W Nd2 O19 87.5(2) . . ? O6W Nd2 O19 74.6(2) . . ? O12 Nd2 O20 114.7(2) . . ? O13 Nd2 O20 131.7(2) . . ? O16 Nd2 O20 132.7(2) . . ? O17 Nd2 O20 105.0(2) . . ? O5W Nd2 O20 74.2(2) . . ? O4W Nd2 O20 64.9(2) . . ? O6W Nd2 O20 65.3(2) . . ? O19 Nd2 O20 48.66(19) . . ? O12 Nd2 C64 94.7(2) . . ? O13 Nd2 C64 141.8(2) . . ? O16 Nd2 C64 143.5(2) . . ? O17 Nd2 C64 87.5(2) . . ? O5W Nd2 C64 98.4(2) . . ? O4W Nd2 C64 74.5(2) . . ? O6W Nd2 C64 68.6(2) . . ? O19 Nd2 C64 24.4(2) . . ? O20 Nd2 C64 24.3(2) . . ? O8 Nd3 O18 143.0(2) . . ? O8 Nd3 O14 82.8(2) . . ? O18 Nd3 O14 109.8(2) . . ? O8 Nd3 O6 75.8(2) . . ? O18 Nd3 O6 139.7(2) . . ? O14 Nd3 O6 78.6(2) . . ? O8 Nd3 O15 144.5(2) . . ? O18 Nd3 O15 71.4(2) . . ? O14 Nd3 O15 73.7(2) . . ? O6 Nd3 O15 73.8(2) . . ? O8 Nd3 O9 72.9(2) . . ? O18 Nd3 O9 77.4(2) . . ? O14 Nd3 O9 142.8(2) . . ? O6 Nd3 O9 120.2(2) . . ? O15 Nd3 O9 139.6(2) . . ? O8 Nd3 O11 77.2(2) . . ? O18 Nd3 O11 72.4(2) . . ? O14 Nd3 O11 77.1(2) . . ? O6 Nd3 O11 145.5(2) . . ? O15 Nd3 O11 121.2(2) . . ? O9 Nd3 O11 70.4(2) . . ? O8 Nd3 O3 114.3(2) . . ? O18 Nd3 O3 76.0(2) . . ? O14 Nd3 O3 144.4(2) . . ? O6 Nd3 O3 76.1(2) . . ? O15 Nd3 O3 75.4(2) . . ? O9 Nd3 O3 72.6(2) . . ? O11 Nd3 O3 135.4(2) . . ? O22 Cl1 O21 109.5(6) . . ? O22 Cl1 O24 108.3(6) . . ? O21 Cl1 O24 108.5(6) . . ? O22 Cl1 O23 110.5(5) . . ? O21 Cl1 O23 112.1(5) . . ? O24 Cl1 O23 107.8(5) . . ? O27 Cl2 O28 107.4(5) . . ? O27 Cl2 O26 109.5(6) . . ? O28 Cl2 O26 112.0(7) . . ? O27 Cl2 O25 111.8(5) . . ? O28 Cl2 O25 108.8(5) . . ? O26 Cl2 O25 107.3(6) . . ? O32 Cl3 O29 110.7(5) . . ? O32 Cl3 O30 111.1(6) . . ? O29 Cl3 O30 109.7(5) . . ? O32 Cl3 O31 109.1(6) . . ? O29 Cl3 O31 109.3(6) . . ? O30 Cl3 O31 106.9(6) . . ? O33 Cl4 O35 108.0(5) . . ? O33 Cl4 O36 108.9(5) . . ? O35 Cl4 O36 109.1(5) . . ? O33 Cl4 O34 112.5(6) . . ? O35 Cl4 O34 109.0(5) . . ? O36 Cl4 O34 109.3(5) . . ? O38 Cl5 O39 114.9(19) . . ? O38 Cl5 O40 114(2) . . ? O39 Cl5 O40 94.4(15) . . ? O38 Cl5 O37 109.6(14) . . ? O39 Cl5 O37 116.0(12) . . ? O40 Cl5 O37 107.0(11) . . ? O41 Cl6 O43 109.3(8) . . ? O41 Cl6 O42 109.8(6) . . ? O43 Cl6 O42 110.1(8) . . ? O41 Cl6 O44 111.7(5) . . ? O43 Cl6 O44 107.5(6) . . ? O42 Cl6 O44 108.4(6) . . ? O48 Cl7 O47 108.7(18) . . ? O48 Cl7 O46 113.5(11) . . ? O47 Cl7 O46 105.9(16) . . ? O48 Cl7 O45 107.8(10) . . ? O47 Cl7 O45 108.7(11) . . ? O46 Cl7 O45 112.1(8) . . ? O51 Cl8 O52 101.3(12) . . ? O51 Cl8 O49 121.0(10) . . ? O52 Cl8 O49 106.9(9) . . ? O51 Cl8 O50 105.9(9) . . ? O52 Cl8 O50 110.0(8) . . ? O49 Cl8 O50 111.1(7) . . ? O53 Cl9 O55 106.9(6) . . ? O53 Cl9 O54 111.3(5) . . ? O55 Cl9 O54 108.4(5) . . ? O53 Cl9 O56 109.4(5) . . ? O55 Cl9 O56 109.5(5) . . ? O54 Cl9 O56 111.2(5) . . ? O2 C1 O1 125.2(9) . . ? O2 C1 C2 118.6(9) . . ? O1 C1 C2 116.1(8) . . ? N1 C2 C7 109.9(8) . . ? N1 C2 C1 104.4(8) . . ? C7 C2 C1 112.5(8) . . ? N1 C2 C3 110.0(8) . . ? C7 C2 C3 110.8(8) . . ? C1 C2 C3 108.9(8) . . ? C4 C3 C2 114.2(9) . . ? C4 C3 H3A 108.7 . . ? C2 C3 H3A 108.7 . . ? C4 C3 H3B 108.7 . . ? C2 C3 H3B 108.7 . . ? H3A C3 H3B 107.6 . . ? C3 C4 C5 111.8(10) . . ? C3 C4 H4A 109.3 . . ? C5 C4 H4A 109.3 . . ? C3 C4 H4B 109.3 . . ? C5 C4 H4B 109.3 . . ? H4A C4 H4B 107.9 . . ? C6 C5 C4 111.5(10) . . ? C6 C5 H5A 109.3 . . ? C4 C5 H5A 109.3 . . ? C6 C5 H5B 109.3 . . ? C4 C5 H5B 109.3 . . ? H5A C5 H5B 108.0 . . ? C5 C6 C7 111.7(9) . . ? C5 C6 H6A 109.3 . . ? C7 C6 H6A 109.3 . . ? C5 C6 H6B 109.3 . . ? C7 C6 H6B 109.3 . . ? H6A C6 H6B 107.9 . . ? C6 C7 C2 112.8(8) . . ? C6 C7 H7A 109.0 . . ? C2 C7 H7A 109.0 . . ? C6 C7 H7B 109.0 . . ? C2 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? O4 C8 O3 124.5(8) . . ? O4 C8 C9 117.5(7) . . ? O3 C8 C9 118.0(7) . . ? N2 C9 C14 109.5(7) . . ? N2 C9 C8 106.9(7) . . ? C14 C9 C8 112.8(7) . . ? N2 C9 C10 109.1(7) . . ? C14 C9 C10 110.6(7) . . ? C8 C9 C10 107.8(7) . . ? C11 C10 C9 112.2(8) . . ? C11 C10 H10A 109.2 . . ? C9 C10 H10A 109.2 . . ? C11 C10 H10B 109.2 . . ? C9 C10 H10B 109.2 . . ? H10A C10 H10B 107.9 . . ? C10 C11 C12 111.2(8) . . ? C10 C11 H11A 109.4 . . ? C12 C11 H11A 109.4 . . ? C10 C11 H11B 109.4 . . ? C12 C11 H11B 109.4 . . ? H11A C11 H11B 108.0 . . ? C13 C12 C11 110.7(8) . . ? C13 C12 H12A 109.5 . . ? C11 C12 H12A 109.5 . . ? C13 C12 H12B 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 108.1 . . ? C14 C13 C12 110.7(8) . . ? C14 C13 H13A 109.5 . . ? C12 C13 H13A 109.5 . . ? C14 C13 H13B 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 108.1 . . ? C13 C14 C9 112.8(8) . . ? C13 C14 H14A 109.0 . . ? C9 C14 H14A 109.0 . . ? C13 C14 H14B 109.0 . . ? C9 C14 H14B 109.0 . . ? H14A C14 H14B 107.8 . . ? O6 C15 O5 129.3(9) . . ? O6 C15 C16 115.8(8) . . ? O5 C15 C16 114.9(8) . . ? N3 C16 C17 107.6(7) . . ? N3 C16 C21 108.8(7) . . ? C17 C16 C21 112.4(8) . . ? N3 C16 C15 107.5(7) . . ? C17 C16 C15 108.4(7) . . ? C21 C16 C15 112.0(7) . . ? C16 C17 C18 113.6(8) . . ? C16 C17 H17A 108.8 . . ? C18 C17 H17A 108.8 . . ? C16 C17 H17B 108.8 . . ? C18 C17 H17B 108.8 . . ? H17A C17 H17B 107.7 . . ? C19 C18 C17 112.5(9) . . ? C19 C18 H18A 109.1 . . ? C17 C18 H18A 109.1 . . ? C19 C18 H18B 109.1 . . ? C17 C18 H18B 109.1 . . ? H18A C18 H18B 107.8 . . ? C18 C19 C20 111.8(9) . . ? C18 C19 H19A 109.3 . . ? C20 C19 H19A 109.3 . . ? C18 C19 H19B 109.3 . . ? C20 C19 H19B 109.3 . . ? H19A C19 H19B 107.9 . . ? C19 C20 C21 112.2(9) . . ? C19 C20 H20A 109.2 . . ? C21 C20 H20A 109.2 . . ? C19 C20 H20B 109.2 . . ? C21 C20 H20B 109.2 . . ? H20A C20 H20B 107.9 . . ? C16 C21 C20 111.3(8) . . ? C16 C21 H21A 109.4 . . ? C20 C21 H21A 109.4 . . ? C16 C21 H21B 109.4 . . ? C20 C21 H21B 109.4 . . ? H21A C21 H21B 108.0 . . ? O7 C22 O8 127.8(8) . . ? O7 C22 C23 115.4(7) . . ? O8 C22 C23 116.8(8) . . ? N4 C23 C24 111.4(7) . . ? N4 C23 C28 108.3(7) . . ? C24 C23 C28 110.6(7) . . ? N4 C23 C22 107.1(7) . . ? C24 C23 C22 110.2(7) . . ? C28 C23 C22 109.2(7) . . ? C25 C24 C23 112.8(8) . . ? C25 C24 H24A 109.0 . . ? C23 C24 H24A 109.0 . . ? C25 C24 H24B 109.0 . . ? C23 C24 H24B 109.0 . . ? H24A C24 H24B 107.8 . . ? C24 C25 C26 111.5(8) . . ? C24 C25 H25A 109.3 . . ? C26 C25 H25A 109.3 . . ? C24 C25 H25B 109.3 . . ? C26 C25 H25B 109.3 . . ? H25A C25 H25B 108.0 . . ? C27 C26 C25 111.3(9) . . ? C27 C26 H26A 109.4 . . ? C25 C26 H26A 109.4 . . ? C27 C26 H26B 109.4 . . ? C25 C26 H26B 109.4 . . ? H26A C26 H26B 108.0 . . ? C26 C27 C28 110.0(9) . . ? C26 C27 H27A 109.7 . . ? C28 C27 H27A 109.7 . . ? C26 C27 H27B 109.7 . . ? C28 C27 H27B 109.7 . . ? H27A C27 H27B 108.2 . . ? C27 C28 C23 113.0(7) . . ? C27 C28 H28A 109.0 . . ? C23 C28 H28A 109.0 . . ? C27 C28 H28B 109.0 . . ? C23 C28 H28B 109.0 . . ? H28A C28 H28B 107.8 . . ? O9 C29 O10 128.6(8) . . ? O9 C29 C30 115.9(7) . . ? O10 C29 C30 115.4(7) . . ? N5 C30 C31 109.1(7) . . ? N5 C30 C29 107.3(7) . . ? C31 C30 C29 110.4(7) . . ? N5 C30 C35 106.8(7) . . ? C31 C30 C35 110.4(8) . . ? C29 C30 C35 112.7(7) . . ? C30 C31 C32 112.8(8) . . ? C30 C31 H31A 109.0 . . ? C32 C31 H31A 109.0 . . ? C30 C31 H31B 109.0 . . ? C32 C31 H31B 109.0 . . ? H31A C31 H31B 107.8 . . ? C33 C32 C31 112.9(10) . . ? C33 C32 H32A 109.0 . . ? C31 C32 H32A 109.0 . . ? C33 C32 H32B 109.0 . . ? C31 C32 H32B 109.0 . . ? H32A C32 H32B 107.8 . . ? C32 C33 C34 111.7(10) . . ? C32 C33 H33A 109.3 . . ? C34 C33 H33A 109.3 . . ? C32 C33 H33B 109.3 . . ? C34 C33 H33B 109.3 . . ? H33A C33 H33B 107.9 . . ? C33 C34 C35 110.9(10) . . ? C33 C34 H34A 109.5 . . ? C35 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? C35 C34 H34B 109.5 . . ? H34A C34 H34B 108.1 . . ? C34 C35 C30 112.8(9) . . ? C34 C35 H35A 109.0 . . ? C30 C35 H35A 109.0 . . ? C34 C35 H35B 109.0 . . ? C30 C35 H35B 109.0 . . ? H35A C35 H35B 107.8 . . ? O11 C36 O12 125.5(9) . . ? O11 C36 C37 118.1(8) . . ? O12 C36 C37 116.2(8) . . ? C38 C37 C42 112.6(8) . . ? C38 C37 C36 106.0(7) . . ? C42 C37 C36 114.7(7) . . ? C38 C37 N6 108.6(7) . . ? C42 C37 N6 108.6(7) . . ? C36 C37 N6 106.0(7) . . ? C37 C38 C39 113.5(8) . . ? C37 C38 H38A 108.9 . . ? C39 C38 H38A 108.9 . . ? C37 C38 H38B 108.9 . . ? C39 C38 H38B 108.9 . . ? H38A C38 H38B 107.7 . . ? C38 C39 C40 110.7(9) . . ? C38 C39 H39A 109.5 . . ? C40 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? C40 C39 H39B 109.5 . . ? H39A C39 H39B 108.1 . . ? C41 C40 C39 112.1(9) . . ? C41 C40 H40A 109.2 . . ? C39 C40 H40A 109.2 . . ? C41 C40 H40B 109.2 . . ? C39 C40 H40B 109.2 . . ? H40A C40 H40B 107.9 . . ? C40 C41 C42 111.4(9) . . ? C40 C41 H41A 109.4 . . ? C42 C41 H41A 109.4 . . ? C40 C41 H41B 109.4 . . ? C42 C41 H41B 109.4 . . ? H41A C41 H41B 108.0 . . ? C37 C42 C41 114.3(8) . . ? C37 C42 H42A 108.7 . . ? C41 C42 H42A 108.7 . . ? C37 C42 H42B 108.7 . . ? C41 C42 H42B 108.7 . . ? H42A C42 H42B 107.6 . . ? O14 C43 O13 127.1(8) . . ? O14 C43 C44 117.2(7) . . ? O13 C43 C44 115.6(7) . . ? N7 C44 C45 109.8(8) . . ? N7 C44 C49 107.6(7) . . ? C45 C44 C49 111.1(8) . . ? N7 C44 C43 106.2(7) . . ? C45 C44 C43 110.7(7) . . ? C49 C44 C43 111.3(7) . . ? C44 C45 C46 113.2(8) . . ? C44 C45 H45A 108.9 . . ? C46 C45 H45A 108.9 . . ? C44 C45 H45B 108.9 . . ? C46 C45 H45B 108.9 . . ? H45A C45 H45B 107.8 . . ? C45 C46 C47 111.4(9) . . ? C45 C46 H46A 109.3 . . ? C47 C46 H46A 109.3 . . ? C45 C46 H46B 109.3 . . ? C47 C46 H46B 109.3 . . ? H46A C46 H46B 108.0 . . ? C48 C47 C46 111.6(8) . . ? C48 C47 H47A 109.3 . . ? C46 C47 H47A 109.3 . . ? C48 C47 H47B 109.3 . . ? C46 C47 H47B 109.3 . . ? H47A C47 H47B 108.0 . . ? C49 C48 C47 111.0(8) . . ? C49 C48 H48A 109.4 . . ? C47 C48 H48A 109.4 . . ? C49 C48 H48B 109.4 . . ? C47 C48 H48B 109.4 . . ? H48A C48 H48B 108.0 . . ? C48 C49 C44 112.1(8) . . ? C48 C49 H49A 109.2 . . ? C44 C49 H49A 109.2 . . ? C48 C49 H49B 109.2 . . ? C44 C49 H49B 109.2 . . ? H49A C49 H49B 107.9 . . ? O15 C50 O16 128.8(9) . . ? O15 C50 C51 115.4(8) . . ? O16 C50 C51 115.4(7) . . ? C52 C51 N8 110.6(7) . . ? C52 C51 C50 109.1(7) . . ? N8 C51 C50 105.0(6) . . ? C52 C51 C56 111.4(7) . . ? N8 C51 C56 108.4(7) . . ? C50 C51 C56 112.1(7) . . ? C53 C52 C51 114.1(8) . . ? C53 C52 H52A 108.7 . . ? C51 C52 H52A 108.7 . . ? C53 C52 H52B 108.7 . . ? C51 C52 H52B 108.7 . . ? H52A C52 H52B 107.6 . . ? C52 C53 C54 109.6(8) . . ? C52 C53 H53A 109.8 . . ? C54 C53 H53A 109.8 . . ? C52 C53 H53B 109.8 . . ? C54 C53 H53B 109.8 . . ? H53A C53 H53B 108.2 . . ? C55 C54 C53 110.3(9) . . ? C55 C54 H54A 109.6 . . ? C53 C54 H54A 109.6 . . ? C55 C54 H54B 109.6 . . ? C53 C54 H54B 109.6 . . ? H54A C54 H54B 108.1 . . ? C54 C55 C56 113.2(8) . . ? C54 C55 H55A 108.9 . . ? C56 C55 H55A 108.9 . . ? C54 C55 H55B 108.9 . . ? C56 C55 H55B 108.9 . . ? H55A C55 H55B 107.8 . . ? C55 C56 C51 111.8(8) . . ? C55 C56 H56A 109.3 . . ? C51 C56 H56A 109.3 . . ? C55 C56 H56B 109.3 . . ? C51 C56 H56B 109.3 . . ? H56A C56 H56B 107.9 . . ? O17 C57 O18 126.5(9) . . ? O17 C57 C58 117.7(8) . . ? O18 C57 C58 115.7(8) . . ? N9 C58 C59 109.8(7) . . ? N9 C58 C57 106.4(7) . . ? C59 C58 C57 111.6(7) . . ? N9 C58 C63 110.0(7) . . ? C59 C58 C63 110.3(7) . . ? C57 C58 C63 108.7(7) . . ? C60 C59 C58 113.5(8) . . ? C60 C59 H59A 108.9 . . ? C58 C59 H59A 108.9 . . ? C60 C59 H59B 108.9 . . ? C58 C59 H59B 108.9 . . ? H59A C59 H59B 107.7 . . ? C59 C60 C61 112.6(8) . . ? C59 C60 H60A 109.1 . . ? C61 C60 H60A 109.1 . . ? C59 C60 H60B 109.1 . . ? C61 C60 H60B 109.1 . . ? H60A C60 H60B 107.8 . . ? C62 C61 C60 108.7(9) . . ? C62 C61 H61A 110.0 . . ? C60 C61 H61A 110.0 . . ? C62 C61 H61B 110.0 . . ? C60 C61 H61B 110.0 . . ? H61A C61 H61B 108.3 . . ? C61 C62 C63 111.0(8) . . ? C61 C62 H62A 109.4 . . ? C63 C62 H62A 109.4 . . ? C61 C62 H62B 109.4 . . ? C63 C62 H62B 109.4 . . ? H62A C62 H62B 108.0 . . ? C58 C63 C62 113.8(8) . . ? C58 C63 H63A 108.8 . . ? C62 C63 H63A 108.8 . . ? C58 C63 H63B 108.8 . . ? C62 C63 H63B 108.8 . . ? H63A C63 H63B 107.7 . . ? O20 C64 O19 122.5(8) . . ? O20 C64 C65 120.4(8) . . ? O19 C64 C65 117.1(8) . . ? O20 C64 Nd2 63.0(5) . . ? O19 C64 Nd2 59.5(5) . . ? C65 C64 Nd2 174.8(6) . . ? N10 C65 C66 109.1(8) . . ? N10 C65 C64 106.8(7) . . ? C66 C65 C64 115.3(8) . . ? N10 C65 C70 104.7(8) . . ? C66 C65 C70 112.0(9) . . ? C64 C65 C70 108.3(8) . . ? C65 C66 C67 113.2(11) . . ? C65 C66 H66A 108.9 . . ? C67 C66 H66A 108.9 . . ? C65 C66 H66B 108.9 . . ? C67 C66 H66B 108.9 . . ? H66A C66 H66B 107.7 . . ? C68 C67 C66 112.8(12) . . ? C68 C67 H67A 109.0 . . ? C66 C67 H67A 109.0 . . ? C68 C67 H67B 109.0 . . ? C66 C67 H67B 109.0 . . ? H67A C67 H67B 107.8 . . ? C67 C68 C69 113.2(13) . . ? C67 C68 H68A 108.9 . . ? C69 C68 H68A 108.9 . . ? C67 C68 H68B 108.9 . . ? C69 C68 H68B 108.9 . . ? H68A C68 H68B 107.8 . . ? C68 C69 C70 112.6(14) . . ? C68 C69 H69A 109.1 . . ? C70 C69 H69A 109.1 . . ? C68 C69 H69B 109.1 . . ? C70 C69 H69B 109.1 . . ? H69A C69 H69B 107.8 . . ? C69 C70 C65 109.2(11) . . ? C69 C70 H70A 109.8 . . ? C65 C70 H70A 109.8 . . ? C69 C70 H70B 109.8 . . ? C65 C70 H70B 109.8 . . ? H70A C70 H70B 108.3 . . ? C2 N1 H1A 109.5 . . ? C2 N1 H1B 109.5 . . ? H1A N1 H1B 109.5 . . ? C2 N1 H1C 109.5 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? C9 N2 H2A 109.5 . . ? C9 N2 H2B 109.5 . . ? H2A N2 H2B 109.5 . . ? C9 N2 H2C 109.5 . . ? H2A N2 H2C 109.5 . . ? H2B N2 H2C 109.5 . . ? C16 N3 H3C 109.5 . . ? C16 N3 H3D 109.5 . . ? H3C N3 H3D 109.5 . . ? C16 N3 H3E 109.5 . . ? H3C N3 H3E 109.5 . . ? H3D N3 H3E 109.5 . . ? C23 N4 H4C 109.5 . . ? C23 N4 H4D 109.5 . . ? H4C N4 H4D 109.5 . . ? C23 N4 H4E 109.5 . . ? H4C N4 H4E 109.5 . . ? H4D N4 H4E 109.5 . . ? C30 N5 H5C 109.5 . . ? C30 N5 H5D 109.5 . . ? H5C N5 H5D 109.5 . . ? C30 N5 H5E 109.5 . . ? H5C N5 H5E 109.5 . . ? H5D N5 H5E 109.5 . . ? C37 N6 H6C 109.5 . . ? C37 N6 H6D 109.5 . . ? H6C N6 H6D 109.5 . . ? C37 N6 H6E 109.5 . . ? H6C N6 H6E 109.5 . . ? H6D N6 H6E 109.5 . . ? C44 N7 H7C 109.5 . . ? C44 N7 H7D 109.5 . . ? H7C N7 H7D 109.5 . . ? C44 N7 H7E 109.5 . . ? H7C N7 H7E 109.5 . . ? H7D N7 H7E 109.5 . . ? C51 N8 H8A 109.5 . . ? C51 N8 H8B 109.5 . . ? H8A N8 H8B 109.5 . . ? C51 N8 H8C 109.5 . . ? H8A N8 H8C 109.5 . . ? H8B N8 H8C 109.5 . . ? C58 N9 H9A 109.5 . . ? C58 N9 H9B 109.5 . . ? H9A N9 H9B 109.5 . . ? C58 N9 H9C 109.5 . . ? H9A N9 H9C 109.5 . . ? H9B N9 H9C 109.5 . . ? C65 N10 H10C 109.5 . . ? C65 N10 H10D 109.5 . . ? H10C N10 H10D 109.5 . . ? C65 N10 H10E 109.5 . . ? H10C N10 H10E 109.5 . . ? H10D N10 H10E 109.5 . . ? C1 O1 Nd1 135.3(6) . . ? C8 O3 Nd3 122.4(5) . . ? C8 O4 Nd1 163.5(6) . . ? C15 O5 Nd1 134.5(6) . . ? C15 O6 Nd3 142.7(6) . . ? C22 O7 Nd1 117.4(5) . . ? C22 O8 Nd3 172.9(6) . . ? C29 O9 Nd3 139.3(5) . . ? C29 O10 Nd1 145.4(6) . . ? C36 O11 Nd3 126.2(6) . . ? C36 O12 Nd2 157.0(6) . . ? C43 O13 Nd2 145.2(6) . . ? C43 O14 Nd3 142.4(6) . . ? C50 O15 Nd3 149.2(6) . . ? C50 O16 Nd2 138.8(6) . . ? C57 O17 Nd2 133.1(6) . . ? C57 O18 Nd3 162.7(6) . . ? C64 O19 Nd2 96.1(5) . . ? C64 O20 Nd2 92.7(5) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 3.344 _refine_diff_density_min -2.398 _refine_diff_density_rms 0.211 # Attachment '- complex5.cif' data_complex5 _database_code_depnum_ccdc_archive 'CCDC 791395' #TrackingRef '- complex5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H118 Cl8 Dy4 N6 O66' _chemical_formula_weight 2697.02 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' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M p2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 13.1386(2) _cell_length_b 26.5893(6) _cell_length_c 26.6992(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9327.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 11149 _cell_measurement_theta_min 2.7530 _cell_measurement_theta_max 29.0781 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.921 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5360 _exptl_absorpt_coefficient_mu 3.510 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3997 _exptl_absorpt_correction_T_max 0.4863 _exptl_absorpt_process_details ? _exptl_special_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 173(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 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30956 _diffrn_reflns_av_R_equivalents 0.0516 _diffrn_reflns_av_sigmaI/netI 0.1262 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.76 _diffrn_reflns_theta_max 25.00 _reflns_number_total 15266 _reflns_number_gt 11444 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. Non-hydrogen atoms were refined anisotropically, except for 22 atoms(o13 o14 c9 c15 c22 c26 c27 c28 c30 c33 n4 c23 c35 c37 o7 n3 c7 c31 o25 o26 c13)were refined isotropically due to disorder ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.008(6) _refine_ls_number_reflns 15266 _refine_ls_number_parameters 1135 _refine_ls_number_restraints 132 _refine_ls_R_factor_all 0.0574 _refine_ls_R_factor_gt 0.0382 _refine_ls_wR_factor_ref 0.0503 _refine_ls_wR_factor_gt 0.0481 _refine_ls_goodness_of_fit_ref 0.825 _refine_ls_restrained_S_all 0.822 _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 Dy1 Dy 0.02022(3) 0.466765(15) 0.840453(14) 0.01084(9) Uani 1 1 d . . . Dy2 Dy -0.21157(3) 0.497571(17) 0.757624(13) 0.01115(10) Uani 1 1 d . . . Dy3 Dy 0.04733(3) 0.488157(16) 0.699372(14) 0.01126(10) Uani 1 1 d . . . Dy4 Dy -0.01388(3) 0.596998(15) 0.784885(14) 0.01096(10) Uani 1 1 d . . . Cl1 Cl -0.15404(15) 0.50654(10) 0.95341(8) 0.0220(6) Uani 1 1 d . . . Cl2 Cl -0.32906(19) 0.69653(10) 0.67701(11) 0.0361(7) Uani 1 1 d . . . Cl3 Cl -0.0413(2) 0.76073(13) 0.92238(15) 0.0736(12) Uani 1 1 d . . . Cl4 Cl 0.49881(16) 0.53674(10) 1.00107(8) 0.0247(6) Uani 1 1 d . . . Cl5 Cl -0.03728(18) 0.29813(9) 0.79755(10) 0.0296(6) Uani 1 1 d . . . Cl6 Cl 0.44018(18) 0.47156(11) 0.61803(9) 0.0322(7) Uani 1 1 d . . . Cl7 Cl 0.39038(15) 0.50190(10) 0.84423(8) 0.0235(5) Uani 1 1 d . . . Cl8 Cl 0.2579(2) 0.27733(11) 1.02002(11) 0.0388(7) Uani 1 1 d . . . C1 C -0.1613(6) 0.4247(3) 0.6592(4) 0.022(2) Uani 1 1 d . . . C2 C -0.2007(6) 0.3833(3) 0.6265(3) 0.015(2) Uani 1 1 d . . . C3 C -0.2859(6) 0.4011(4) 0.5938(3) 0.023(2) Uani 1 1 d . . . H3A H -0.2590 0.4264 0.5699 0.027 Uiso 1 1 calc R . . H3B H -0.3375 0.4180 0.6149 0.027 Uiso 1 1 calc R . . C4 C -0.3372(7) 0.3591(4) 0.5643(3) 0.027(3) Uani 1 1 d . . . H4A H -0.3962 0.3729 0.5457 0.032 Uiso 1 1 calc R . . H4B H -0.2886 0.3453 0.5395 0.032 Uiso 1 1 calc R . . C5 C -0.3720(7) 0.3184(4) 0.5976(4) 0.034(3) Uani 1 1 d . . . H5A H -0.4034 0.2914 0.5772 0.041 Uiso 1 1 calc R . . H5B H -0.4248 0.3317 0.6205 0.041 Uiso 1 1 calc R . . C6 C -0.2832(8) 0.2959(4) 0.6290(4) 0.053(3) Uani 1 1 d . . . H6A H -0.3094 0.2699 0.6522 0.064 Uiso 1 1 calc R . . H6B H -0.2323 0.2801 0.6066 0.064 Uiso 1 1 calc R . . C7 C -0.2351(7) 0.3384(4) 0.6580(4) 0.033(3) Uani 1 1 d U . . H7A H -0.1754 0.3250 0.6763 0.040 Uiso 1 1 calc R . . H7B H -0.2846 0.3504 0.6833 0.040 Uiso 1 1 calc R . . C8 C 0.1868(5) 0.4084(4) 0.7666(3) 0.015(2) Uani 1 1 d . . . C9 C 0.2578(5) 0.3636(3) 0.7590(3) 0.011(2) Uani 1 1 d U . . C10 C 0.3661(6) 0.3818(3) 0.7484(3) 0.022(2) Uani 1 1 d . . . H10A H 0.3637 0.4074 0.7215 0.026 Uiso 1 1 calc R . . H10B H 0.3931 0.3983 0.7789 0.026 Uiso 1 1 calc R . . C11 C 0.4389(6) 0.3401(3) 0.7328(4) 0.030(3) Uani 1 1 d . . . H11A H 0.5045 0.3550 0.7222 0.035 Uiso 1 1 calc R . . H11B H 0.4522 0.3178 0.7618 0.035 Uiso 1 1 calc R . . C12 C 0.3952(7) 0.3106(4) 0.6913(4) 0.041(3) Uani 1 1 d . . . H12A H 0.4413 0.2820 0.6841 0.049 Uiso 1 1 calc R . . H12B H 0.3931 0.3321 0.6610 0.049 Uiso 1 1 calc R . . C13 C 0.2912(6) 0.2903(3) 0.7004(3) 0.024(2) Uani 1 1 d U . . H13A H 0.2659 0.2737 0.6696 0.029 Uiso 1 1 calc R . . H13B H 0.2938 0.2649 0.7274 0.029 Uiso 1 1 calc R . . C14 C 0.2207(7) 0.3314(3) 0.7148(3) 0.031(3) Uani 1 1 d . . . H14A H 0.1540 0.3165 0.7237 0.038 Uiso 1 1 calc R . . H14B H 0.2100 0.3535 0.6855 0.038 Uiso 1 1 calc R . . C15 C -0.2119(6) 0.4141(3) 0.8492(3) 0.014(2) Uani 1 1 d U . . C16 C -0.2811(6) 0.3733(3) 0.8729(3) 0.014(2) Uani 1 1 d . . . C17 C -0.3315(6) 0.3421(3) 0.8334(4) 0.026(3) Uani 1 1 d . . . H17A H -0.2787 0.3233 0.8147 0.031 Uiso 1 1 calc R . . H17B H -0.3666 0.3646 0.8094 0.031 Uiso 1 1 calc R . . C18 C -0.4088(6) 0.3047(3) 0.8549(3) 0.024(3) Uani 1 1 d . . . H18A H -0.4412 0.2859 0.8271 0.029 Uiso 1 1 calc R . . H18B H -0.3729 0.2801 0.8765 0.029 Uiso 1 1 calc R . . C19 C -0.4880(7) 0.3304(4) 0.8845(3) 0.032(3) Uani 1 1 d . . . H19A H -0.5345 0.3050 0.8990 0.038 Uiso 1 1 calc R . . H19B H -0.5285 0.3524 0.8621 0.038 Uiso 1 1 calc R . . C20 C -0.4431(7) 0.3613(4) 0.9256(3) 0.032(3) Uani 1 1 d . . . H20A H -0.4119 0.3387 0.9507 0.039 Uiso 1 1 calc R . . H20B H -0.4979 0.3805 0.9424 0.039 Uiso 1 1 calc R . . C21 C -0.3610(6) 0.3987(3) 0.9061(3) 0.019(2) Uani 1 1 d . . . H21A H -0.3948 0.4257 0.8868 0.022 Uiso 1 1 calc R . . H21B H -0.3266 0.4145 0.9351 0.022 Uiso 1 1 calc R . . C22 C -0.2587(6) 0.6025(3) 0.8206(3) 0.014(2) Uani 1 1 d U . . C23 C -0.3255(6) 0.6244(3) 0.8627(3) 0.010(2) Uani 1 1 d U . . C24 C -0.2640(5) 0.6490(3) 0.9044(3) 0.015(2) Uani 1 1 d . . . H24A H -0.2228 0.6229 0.9213 0.018 Uiso 1 1 calc R . . H24B H -0.2166 0.6737 0.8894 0.018 Uiso 1 1 calc R . . C25 C -0.3289(6) 0.6752(3) 0.9427(3) 0.019(2) Uani 1 1 d U . . H25A H -0.3670 0.6497 0.9621 0.022 Uiso 1 1 calc R . . H25B H -0.2842 0.6936 0.9662 0.022 Uiso 1 1 calc R . . C26 C -0.4019(6) 0.7110(4) 0.9202(3) 0.020(2) Uani 1 1 d U . . H26A H -0.3636 0.7393 0.9054 0.024 Uiso 1 1 calc R . . H26B H -0.4458 0.7247 0.9471 0.024 Uiso 1 1 calc R . . C27 C -0.4695(6) 0.6878(3) 0.8799(3) 0.015(2) Uani 1 1 d U . . H27A H -0.5109 0.7144 0.8639 0.018 Uiso 1 1 calc R . . H27B H -0.5165 0.6631 0.8953 0.018 Uiso 1 1 calc R . . C28 C -0.4026(6) 0.6609(3) 0.8393(3) 0.017(2) Uani 1 1 d U . . H28A H -0.4474 0.6421 0.8161 0.021 Uiso 1 1 calc R . . H28B H -0.3656 0.6866 0.8196 0.021 Uiso 1 1 calc R . . C29 C 0.1126(6) 0.5705(4) 0.8903(3) 0.014(2) Uani 1 1 d . . . C30 C 0.1693(6) 0.5980(3) 0.9329(3) 0.012(2) Uani 1 1 d U . . C31 C 0.0924(6) 0.6117(3) 0.9747(3) 0.017(2) Uani 1 1 d U . . H31A H 0.0355 0.6311 0.9600 0.020 Uiso 1 1 calc R . . H31B H 0.0640 0.5804 0.9892 0.020 Uiso 1 1 calc R . . C32 C 0.1425(7) 0.6424(5) 1.0158(3) 0.048(4) Uani 1 1 d . . . H32A H 0.0895 0.6534 1.0398 0.057 Uiso 1 1 calc R . . H32B H 0.1909 0.6207 1.0342 0.057 Uiso 1 1 calc R . . C33 C 0.1963(7) 0.6862(4) 0.9975(4) 0.034(3) Uani 1 1 d U . . H33A H 0.2295 0.7036 1.0259 0.040 Uiso 1 1 calc R . . H33B H 0.1471 0.7099 0.9821 0.040 Uiso 1 1 calc R . . C34 C 0.2779(7) 0.6716(4) 0.9583(3) 0.031(3) Uani 1 1 d . . . H34A H 0.3099 0.7024 0.9445 0.037 Uiso 1 1 calc R . . H34B H 0.3316 0.6511 0.9743 0.037 Uiso 1 1 calc R . . C35 C 0.2295(6) 0.6425(4) 0.9172(3) 0.021(2) Uani 1 1 d . . . H35A H 0.1842 0.6654 0.8982 0.026 Uiso 1 1 calc R . . H35B H 0.2835 0.6311 0.8940 0.026 Uiso 1 1 calc R . . C36 C 0.1825(5) 0.5940(3) 0.7016(3) 0.0108(19) Uani 1 1 d U . . C37 C 0.2841(6) 0.6190(3) 0.6860(3) 0.018(2) Uani 1 1 d U . . C38 C 0.2792(7) 0.6756(3) 0.6811(3) 0.027(3) Uani 1 1 d . . . H38A H 0.2169 0.6849 0.6624 0.032 Uiso 1 1 calc R . . H38B H 0.3386 0.6874 0.6615 0.032 Uiso 1 1 calc R . . C39 C 0.2784(7) 0.7025(4) 0.7321(4) 0.037(3) Uani 1 1 d . . . H39A H 0.2858 0.7391 0.7264 0.045 Uiso 1 1 calc R . . H39B H 0.2115 0.6969 0.7482 0.045 Uiso 1 1 calc R . . C40 C 0.3600(7) 0.6856(4) 0.7670(4) 0.037(3) Uani 1 1 d . . . H40A H 0.3507 0.7015 0.8002 0.045 Uiso 1 1 calc R . . H40B H 0.4275 0.6955 0.7539 0.045 Uiso 1 1 calc R . . C41 C 0.3540(7) 0.6279(4) 0.7721(3) 0.034(3) Uani 1 1 d . . . H41A H 0.4083 0.6161 0.7949 0.041 Uiso 1 1 calc R . . H41B H 0.2876 0.6185 0.7869 0.041 Uiso 1 1 calc R . . C42 C 0.3658(5) 0.6025(4) 0.7216(3) 0.025(3) Uani 1 1 d . . . H42A H 0.4333 0.6109 0.7074 0.030 Uiso 1 1 calc R . . H42B H 0.3624 0.5656 0.7260 0.030 Uiso 1 1 calc R . . O1 O -0.2225(4) 0.4466(2) 0.6873(2) 0.0280(17) Uani 1 1 d . . . O1W O 0.0777(4) 0.4146(2) 0.9093(2) 0.0155(15) Uani 1 1 d . . . O2 O -0.0656(4) 0.4344(2) 0.6555(2) 0.0280(17) Uani 1 1 d . . . O2W O -0.2837(4) 0.5546(2) 0.6929(2) 0.0255(16) Uani 1 1 d . . . O3 O 0.1687(4) 0.4344(2) 0.7281(2) 0.0223(16) Uani 1 1 d . . . O3W O -0.3909(3) 0.4724(2) 0.7464(2) 0.0239(16) Uani 1 1 d . . . O4 O 0.1507(4) 0.4162(2) 0.8093(2) 0.0204(16) Uani 1 1 d . . . O4W O -0.0018(4) 0.5369(2) 0.62393(17) 0.0249(15) Uani 1 1 d . . . O5 O -0.1190(4) 0.4151(2) 0.86356(19) 0.0150(15) Uani 1 1 d . . . O5W O 0.1415(4) 0.4528(3) 0.6289(2) 0.0282(18) Uani 1 1 d . . . O6 O -0.2543(4) 0.4420(2) 0.8183(2) 0.0190(16) Uani 1 1 d . . . O6W O -0.0778(4) 0.6497(2) 0.7179(2) 0.0196(15) Uani 1 1 d . . . O7 O -0.1779(4) 0.6239(2) 0.8109(2) 0.0194(15) Uani 1 1 d U . . O7W O 0.0232(4) 0.6832(2) 0.8076(2) 0.0269(15) Uani 1 1 d . . . O8W O 0.1607(4) 0.5776(2) 0.4840(2) 0.0304(18) Uani 1 1 d . . . O8 O -0.2939(4) 0.5636(2) 0.79932(19) 0.0137(13) Uani 1 1 d . . . O9 O 0.1244(4) 0.5242(2) 0.8862(2) 0.0155(15) Uani 1 1 d . . . O9W O 0.3507(4) 0.5290(2) 0.4959(2) 0.0245(16) Uani 1 1 d . . . O10 O 0.0609(4) 0.5981(2) 0.8624(2) 0.0249(16) Uani 1 1 d . . . O10W O 0.1194(4) 0.6080(3) 0.5821(2) 0.0299(18) Uani 1 1 d . . . O11 O 0.1700(4) 0.5496(2) 0.6857(2) 0.0195(16) Uani 1 1 d . . . O11W O 0.0086(5) 0.6833(2) 0.6277(2) 0.0346(17) Uani 1 1 d . . . O12W O -0.3359(5) 0.5453(3) 0.5967(2) 0.040(2) Uani 1 1 d . . . O12 O 0.1245(4) 0.6171(2) 0.7305(2) 0.0183(15) Uani 1 1 d . . . O13W O -0.1591(5) 0.6746(3) 0.5622(2) 0.050(2) Uani 1 1 d . . . O13 O 0.0863(3) 0.5222(2) 0.78057(18) 0.0125(14) Uani 1 1 d U . . H13C H 0.1606 0.5288 0.7853 0.015 Uiso 1 1 calc R . . O14W O -0.0664(5) 0.3703(3) 0.9737(2) 0.046(2) Uani 1 1 d . . . O14 O -0.0799(3) 0.5445(2) 0.72398(19) 0.0089(13) Uani 1 1 d U . . H14C H -0.1044 0.5645 0.6946 0.011 Uiso 1 1 calc R . . O15W O 0.4960(5) 0.6164(3) 0.5908(2) 0.054(2) Uani 1 1 d . . . O15 O -0.0542(3) 0.44785(19) 0.76161(18) 0.0083(13) Uani 1 1 d . . . H15A H -0.0645 0.4111 0.7556 0.010 Uiso 1 1 calc R . . O16W O 0.2577(4) 0.3623(3) 0.9068(2) 0.0266(18) Uani 1 1 d . . . O16 O -0.0985(3) 0.5272(2) 0.82323(19) 0.0159(15) Uani 1 1 d . . . H16A H -0.1368 0.5376 0.8539 0.019 Uiso 1 1 calc R . . O17W O -0.1486(5) 0.5675(3) 0.5531(2) 0.046(2) Uani 1 1 d . . . O17 O -0.0549(4) 0.4974(2) 0.93209(18) 0.0233(15) Uani 1 1 d . . . O18W O 0.4800(6) 0.2079(3) 0.9645(3) 0.064(2) Uani 1 1 d . . . O18 O -0.2251(4) 0.5152(2) 0.91346(18) 0.0234(16) Uani 1 1 d . . . O19 O -0.1857(4) 0.4637(3) 0.9820(2) 0.047(2) Uani 1 1 d . . . O20 O -0.1524(5) 0.5492(3) 0.9838(3) 0.049(2) Uani 1 1 d . . . O21 O -0.3296(6) 0.6769(3) 0.6281(3) 0.069(3) Uani 1 1 d . . . O22 O -0.2324(5) 0.7181(3) 0.6883(3) 0.067(3) Uani 1 1 d . . . O23 O -0.3467(6) 0.6575(3) 0.7120(3) 0.070(3) Uani 1 1 d . . . O24 O -0.4018(5) 0.7360(3) 0.6810(3) 0.068(3) Uani 1 1 d . . . O25 O -0.1350(9) 0.7626(5) 0.9157(5) 0.149(5) Uani 1 1 d U . . O26 O -0.0368(14) 0.7939(8) 0.8680(7) 0.292(9) Uani 1 1 d U . . O27 O 0.0070(8) 0.7879(3) 0.9559(3) 0.109(4) Uani 1 1 d . . . O28 O 0.0148(8) 0.7232(4) 0.9029(3) 0.141(5) Uani 1 1 d . . . O29 O 0.5752(4) 0.5422(3) 1.0388(2) 0.044(2) Uani 1 1 d . . . O30 O 0.4859(5) 0.5821(2) 0.9738(2) 0.0388(18) Uani 1 1 d . . . O31 O 0.5276(5) 0.4964(3) 0.9683(2) 0.0466(19) Uani 1 1 d . . . O32 O 0.4025(4) 0.5251(3) 1.0245(2) 0.039(2) Uani 1 1 d . . . O33 O 0.0056(6) 0.2621(3) 0.7664(2) 0.062(2) Uani 1 1 d . . . O34 O -0.1011(4) 0.2751(2) 0.8332(3) 0.041(2) Uani 1 1 d . . . O35 O 0.0412(5) 0.3237(3) 0.8229(3) 0.073(3) Uani 1 1 d . . . O36 O -0.0923(5) 0.3327(3) 0.7685(3) 0.056(2) Uani 1 1 d . . . O37 O 0.3413(5) 0.4875(3) 0.6104(3) 0.072(3) Uani 1 1 d . . . O38 O 0.4924(5) 0.4820(3) 0.5726(2) 0.058(2) Uani 1 1 d . . . O39 O 0.4843(5) 0.4995(3) 0.6566(2) 0.068(2) Uani 1 1 d . . . O40 O 0.4401(7) 0.4216(3) 0.6296(3) 0.096(3) Uani 1 1 d . . . O41 O 0.3682(5) 0.4597(3) 0.8737(3) 0.057(2) Uani 1 1 d . . . O42 O 0.3791(5) 0.5461(3) 0.8735(2) 0.042(2) Uani 1 1 d . . . O43 O 0.3250(4) 0.5033(3) 0.8012(2) 0.0388(18) Uani 1 1 d . . . O44 O 0.4940(4) 0.5018(3) 0.8280(2) 0.060(2) Uani 1 1 d . . . O45 O 0.2057(6) 0.3227(3) 1.0288(3) 0.060(2) Uani 1 1 d . . . O46 O 0.1825(5) 0.2373(3) 1.0243(3) 0.053(2) Uani 1 1 d . . . O47 O 0.3019(5) 0.2769(3) 0.9713(3) 0.061(3) Uani 1 1 d . . . O48 O 0.3344(6) 0.2672(3) 1.0566(3) 0.075(3) Uani 1 1 d . . . N1 N -0.1155(5) 0.3667(3) 0.5929(3) 0.028(2) Uani 1 1 d . . . H1A H -0.0624 0.3557 0.6118 0.042 Uiso 1 1 calc R . . H1B H -0.0949 0.3931 0.5736 0.042 Uiso 1 1 calc R . . H1C H -0.1376 0.3413 0.5728 0.042 Uiso 1 1 calc R . . N2 N 0.2559(5) 0.3331(3) 0.8050(3) 0.023(2) Uani 1 1 d . . . H2A H 0.2791 0.3518 0.8311 0.035 Uiso 1 1 calc R . . H2B H 0.2963 0.3056 0.8009 0.035 Uiso 1 1 calc R . . H2C H 0.1909 0.3231 0.8113 0.035 Uiso 1 1 calc R . . N3 N -0.2168(5) 0.3396(3) 0.9037(3) 0.0187(18) Uani 1 1 d U . . H3C H -0.1693 0.3246 0.8839 0.028 Uiso 1 1 calc R . . H3D H -0.2564 0.3157 0.9182 0.028 Uiso 1 1 calc R . . H3E H -0.1850 0.3579 0.9279 0.028 Uiso 1 1 calc R . . N4 N -0.3855(5) 0.5793(3) 0.8836(2) 0.0165(18) Uani 1 1 d U . . H4C H -0.4223 0.5649 0.8585 0.025 Uiso 1 1 calc R . . H4D H -0.4283 0.5900 0.9081 0.025 Uiso 1 1 calc R . . H4E H -0.3413 0.5563 0.8964 0.025 Uiso 1 1 calc R . . N5 N 0.2432(5) 0.5580(3) 0.9550(3) 0.027(2) Uani 1 1 d . . . H5C H 0.2776 0.5715 0.9813 0.041 Uiso 1 1 calc R . . H5D H 0.2882 0.5483 0.9310 0.041 Uiso 1 1 calc R . . H5E H 0.2069 0.5308 0.9655 0.041 Uiso 1 1 calc R . . N6 N 0.3075(5) 0.5968(3) 0.6357(2) 0.0213(19) Uani 1 1 d . . . H6C H 0.3096 0.5627 0.6381 0.032 Uiso 1 1 calc R . . H6D H 0.3689 0.6084 0.6248 0.032 Uiso 1 1 calc R . . H6E H 0.2583 0.6059 0.6135 0.032 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 Dy1 0.0107(2) 0.0120(2) 0.0098(2) 0.0013(2) -0.00004(17) 0.00088(19) Dy2 0.01000(19) 0.0132(2) 0.0102(2) -0.0009(2) 0.00012(16) 0.0000(2) Dy3 0.0111(2) 0.0132(2) 0.0094(2) -0.0006(2) 0.00066(16) -0.00015(17) Dy4 0.0105(2) 0.0114(2) 0.0110(2) 0.0005(2) 0.00053(16) -0.00001(18) Cl1 0.0236(13) 0.0268(16) 0.0155(12) -0.0005(14) 0.0007(9) 0.0045(12) Cl2 0.0351(16) 0.0299(17) 0.0432(19) -0.0040(17) -0.0087(13) 0.0124(13) Cl3 0.0258(19) 0.063(2) 0.132(3) -0.060(3) 0.0018(19) -0.0003(17) Cl4 0.0224(14) 0.0362(15) 0.0154(11) 0.0025(13) -0.0031(10) -0.0019(12) Cl5 0.0281(15) 0.0241(14) 0.0367(16) -0.0061(14) 0.0091(12) -0.0044(11) Cl6 0.0320(15) 0.0348(17) 0.0297(15) 0.0003(16) 0.0017(11) 0.0084(13) Cl7 0.0224(12) 0.0236(14) 0.0246(13) -0.0048(15) 0.0027(10) -0.0023(12) Cl8 0.0422(18) 0.0307(17) 0.0434(19) 0.0056(17) -0.0026(14) -0.0094(14) C1 0.021(6) 0.015(6) 0.028(6) 0.007(6) -0.010(5) 0.000(4) C2 0.022(5) 0.005(5) 0.017(5) -0.004(5) -0.005(4) -0.005(4) C3 0.028(5) 0.030(6) 0.010(5) -0.003(5) -0.002(4) -0.012(5) C4 0.032(6) 0.027(6) 0.020(6) -0.010(6) -0.013(4) -0.011(5) C5 0.043(7) 0.025(6) 0.035(7) -0.003(6) -0.006(5) -0.021(5) C6 0.050(8) 0.024(6) 0.084(10) -0.015(8) -0.012(7) -0.010(6) C7 0.033(3) 0.033(3) 0.033(3) 0.0009(10) -0.0001(10) -0.0002(10) C8 0.010(5) 0.018(6) 0.017(5) -0.005(5) 0.005(4) 0.005(4) C9 0.012(2) 0.011(2) 0.011(2) 0.0004(10) -0.0004(10) 0.0001(10) C10 0.022(5) 0.014(5) 0.029(6) -0.012(6) 0.001(4) 0.006(4) C11 0.024(6) 0.026(6) 0.039(6) -0.005(6) 0.005(5) 0.011(5) C12 0.056(7) 0.025(6) 0.041(8) 0.004(7) 0.011(6) 0.022(6) C13 0.025(2) 0.024(2) 0.024(2) -0.0002(10) 0.0006(10) 0.0000(10) C14 0.046(6) 0.023(6) 0.025(6) 0.011(6) 0.006(5) 0.010(5) C15 0.014(2) 0.014(2) 0.014(2) -0.0004(10) 0.0007(10) -0.0003(10) C16 0.005(4) 0.024(6) 0.012(5) 0.002(5) 0.001(4) 0.001(4) C17 0.017(5) 0.017(6) 0.043(7) -0.002(6) -0.005(5) 0.000(4) C18 0.012(5) 0.024(6) 0.036(7) -0.011(6) -0.002(4) -0.005(4) C19 0.020(6) 0.030(6) 0.045(7) 0.020(6) -0.003(5) -0.009(5) C20 0.028(6) 0.036(7) 0.032(6) 0.014(6) 0.013(5) 0.019(5) C21 0.022(5) 0.014(5) 0.020(5) -0.003(5) 0.002(4) -0.004(4) C22 0.013(2) 0.014(2) 0.014(2) 0.0004(10) -0.0006(10) 0.0005(10) C23 0.010(2) 0.010(2) 0.010(2) -0.0004(10) 0.0005(10) 0.0000(10) C24 0.010(5) 0.019(6) 0.015(5) 0.002(5) -0.003(4) 0.000(4) C25 0.019(2) 0.019(2) 0.018(2) 0.0003(10) -0.0006(10) 0.0000(10) C26 0.020(2) 0.020(2) 0.021(2) -0.0006(10) 0.0013(10) 0.0004(10) C27 0.015(2) 0.015(2) 0.015(2) 0.0002(10) 0.0002(10) 0.0010(10) C28 0.017(2) 0.017(2) 0.017(2) 0.0004(10) 0.0008(10) -0.0004(10) C29 0.007(5) 0.017(6) 0.018(6) 0.001(6) 0.008(4) 0.005(4) C30 0.012(2) 0.012(2) 0.011(2) -0.0006(10) -0.0004(10) -0.0002(10) C31 0.017(2) 0.017(2) 0.017(2) 0.0000(10) 0.0002(10) 0.0003(10) C32 0.027(6) 0.089(10) 0.027(7) -0.016(8) 0.013(5) 0.022(7) C33 0.034(3) 0.033(3) 0.034(3) -0.0008(10) -0.0006(10) -0.0002(10) C34 0.024(6) 0.029(6) 0.040(7) -0.002(6) -0.002(5) 0.001(5) C35 0.017(5) 0.022(6) 0.025(6) -0.001(6) 0.002(4) 0.006(5) C36 0.011(2) 0.011(2) 0.010(2) -0.0002(10) 0.0002(10) 0.0003(10) C37 0.019(2) 0.018(2) 0.018(2) -0.0005(10) 0.0003(10) 0.0005(10) C38 0.018(5) 0.024(6) 0.038(7) -0.008(6) 0.004(4) -0.010(5) C39 0.034(6) 0.029(6) 0.049(8) 0.019(7) 0.003(5) -0.001(5) C40 0.036(6) 0.036(7) 0.039(7) 0.004(7) -0.009(5) -0.012(5) C41 0.037(6) 0.040(7) 0.025(6) 0.013(6) -0.008(5) 0.013(5) C42 0.004(4) 0.034(6) 0.037(6) -0.006(6) 0.000(4) -0.003(4) O1 0.023(4) 0.031(4) 0.030(4) -0.016(4) -0.007(3) 0.002(3) O1W 0.018(3) 0.014(4) 0.015(3) 0.003(3) -0.003(2) 0.005(3) O2 0.031(4) 0.039(4) 0.014(4) -0.008(4) 0.010(3) -0.015(3) O2W 0.023(3) 0.037(4) 0.017(3) -0.006(4) -0.010(3) 0.012(3) O3 0.027(4) 0.026(4) 0.014(4) -0.005(4) 0.001(3) 0.004(3) O3W 0.009(3) 0.033(4) 0.029(4) 0.003(4) -0.002(2) -0.006(3) O4 0.026(4) 0.020(4) 0.015(4) 0.005(3) 0.001(3) 0.010(3) O4W 0.036(4) 0.027(4) 0.012(3) -0.007(3) 0.002(3) 0.004(3) O5 0.018(3) 0.014(4) 0.013(3) 0.010(3) -0.003(2) 0.005(3) O5W 0.026(4) 0.037(5) 0.022(4) -0.006(4) 0.007(3) 0.001(3) O6 0.015(3) 0.023(4) 0.019(4) 0.012(3) -0.002(2) -0.002(3) O6W 0.033(4) 0.017(4) 0.008(3) 0.009(3) -0.005(3) 0.002(3) O7 0.0197(17) 0.0195(17) 0.0190(17) 0.0004(10) 0.0012(10) -0.0005(10) O7W 0.026(4) 0.018(3) 0.036(4) 0.005(3) 0.000(3) -0.001(3) O8W 0.030(4) 0.036(5) 0.025(4) 0.007(4) -0.002(3) -0.002(3) O8 0.018(3) 0.015(3) 0.008(3) -0.008(3) 0.001(3) 0.004(3) O9 0.022(3) 0.013(4) 0.011(3) 0.002(3) -0.004(2) -0.002(3) O9W 0.020(3) 0.031(4) 0.023(4) 0.003(4) 0.002(3) -0.005(3) O10 0.028(4) 0.020(4) 0.027(4) -0.008(4) -0.006(3) 0.004(3) O10W 0.019(4) 0.042(5) 0.029(4) 0.013(4) 0.000(3) -0.011(3) O11 0.023(3) 0.021(4) 0.014(4) -0.001(3) -0.004(3) -0.005(3) O11W 0.041(4) 0.040(4) 0.023(4) 0.004(4) 0.010(3) -0.011(4) O12W 0.056(5) 0.045(5) 0.018(4) 0.004(4) -0.002(3) -0.002(4) O12 0.014(3) 0.016(4) 0.024(4) 0.001(3) -0.001(3) 0.000(3) O13W 0.073(5) 0.054(6) 0.023(4) 0.008(4) 0.007(4) 0.023(5) O13 0.0117(16) 0.0134(16) 0.0124(16) -0.0002(10) 0.0011(9) -0.0007(10) O14W 0.048(5) 0.066(6) 0.023(4) 0.010(4) 0.004(3) -0.023(4) O14 0.0092(15) 0.0089(16) 0.0087(16) 0.0015(10) -0.0011(9) 0.0005(10) O15W 0.040(5) 0.063(5) 0.060(5) 0.019(5) 0.005(4) -0.003(4) O15 0.013(3) 0.004(3) 0.008(3) 0.002(3) 0.000(2) -0.005(2) O16W 0.021(4) 0.038(5) 0.021(4) -0.008(4) -0.002(3) 0.006(3) O16 0.009(3) 0.017(3) 0.022(4) -0.004(3) 0.005(2) 0.002(3) O17W 0.035(4) 0.070(6) 0.031(4) -0.003(5) 0.001(3) 0.004(4) O17 0.012(3) 0.031(4) 0.027(3) 0.004(4) 0.004(2) 0.009(3) O18W 0.057(5) 0.065(5) 0.071(6) 0.009(5) -0.005(4) -0.002(5) O18 0.023(3) 0.030(4) 0.017(3) 0.000(4) -0.006(3) 0.010(3) O19 0.039(5) 0.064(6) 0.037(5) 0.035(5) 0.010(3) 0.009(4) O20 0.052(5) 0.057(6) 0.038(5) -0.034(5) -0.001(4) -0.004(4) O21 0.074(6) 0.099(8) 0.033(5) -0.037(5) 0.010(4) -0.034(5) O22 0.026(5) 0.053(6) 0.122(8) -0.024(6) -0.014(4) 0.006(4) O23 0.116(7) 0.037(5) 0.058(6) 0.007(6) 0.017(5) 0.024(5) O24 0.050(5) 0.053(5) 0.101(8) 0.007(6) -0.016(4) 0.036(4) O25 0.149(5) 0.150(5) 0.150(5) -0.0008(10) 0.0001(10) 0.0000(10) O26 0.292(9) 0.292(9) 0.292(9) 0.0000(10) -0.0003(10) -0.0003(10) O27 0.218(11) 0.069(6) 0.041(5) -0.008(5) -0.050(7) -0.069(8) O28 0.189(11) 0.175(12) 0.060(6) -0.030(7) -0.038(7) 0.150(10) O29 0.022(4) 0.071(6) 0.040(5) -0.002(5) -0.013(3) -0.009(4) O30 0.050(5) 0.028(4) 0.039(4) -0.005(4) 0.006(4) 0.011(4) O31 0.053(4) 0.053(5) 0.033(4) -0.016(4) 0.003(3) 0.014(5) O32 0.021(4) 0.068(6) 0.028(4) 0.013(4) 0.003(3) -0.012(4) O33 0.076(5) 0.049(5) 0.060(5) -0.025(5) 0.041(5) 0.005(5) O34 0.035(4) 0.041(5) 0.048(5) 0.013(5) 0.019(3) 0.000(4) O35 0.028(5) 0.088(6) 0.103(7) -0.049(6) 0.002(4) -0.004(5) O36 0.096(6) 0.035(5) 0.039(5) 0.023(5) -0.012(4) 0.018(5) O37 0.021(4) 0.079(7) 0.116(7) -0.030(7) -0.014(4) 0.013(5) O38 0.047(5) 0.096(7) 0.030(4) -0.010(5) 0.008(3) -0.009(5) O39 0.067(5) 0.093(6) 0.045(4) -0.043(5) -0.002(4) 0.011(6) O40 0.168(10) 0.042(6) 0.079(7) 0.007(6) 0.000(6) 0.005(7) O41 0.078(6) 0.029(5) 0.063(6) 0.026(5) -0.014(4) -0.025(5) O42 0.050(5) 0.041(5) 0.034(5) -0.026(4) 0.013(3) 0.006(4) O43 0.041(4) 0.045(5) 0.031(4) 0.005(5) -0.016(3) -0.013(4) O44 0.010(3) 0.111(6) 0.058(4) -0.047(5) 0.015(3) -0.011(4) O45 0.069(6) 0.028(5) 0.084(7) -0.016(5) -0.002(5) -0.001(5) O46 0.081(6) 0.030(5) 0.049(6) 0.009(5) -0.004(4) -0.032(5) O47 0.061(5) 0.073(7) 0.049(5) 0.036(5) 0.026(4) 0.026(5) O48 0.109(7) 0.057(6) 0.060(6) 0.029(5) -0.060(5) -0.020(5) N1 0.024(5) 0.028(5) 0.032(5) -0.017(5) -0.003(4) 0.002(4) N2 0.032(5) 0.017(5) 0.021(5) -0.005(4) 0.004(4) 0.008(4) N3 0.019(2) 0.019(2) 0.019(2) 0.0010(10) 0.0007(10) -0.0004(10) N4 0.016(2) 0.017(2) 0.016(2) 0.0001(10) 0.0014(10) 0.0008(10) N5 0.022(4) 0.026(5) 0.034(5) -0.019(5) -0.008(3) 0.007(4) N6 0.022(4) 0.023(5) 0.018(4) -0.015(4) 0.008(3) 0.002(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 O16 2.287(5) . ? Dy1 O4 2.332(6) . ? Dy1 O13 2.342(5) . ? Dy1 O5 2.369(5) . ? Dy1 O15 2.375(5) . ? Dy1 O9 2.386(6) . ? Dy1 O1W 2.423(5) . ? Dy1 O17 2.761(5) . ? Dy1 Dy4 3.7938(6) . ? Dy1 Dy3 3.8260(5) . ? Dy1 Dy2 3.8518(5) . ? Dy2 O6 2.262(5) . ? Dy2 O14 2.314(5) . ? Dy2 O1 2.319(6) . ? Dy2 O8 2.343(5) . ? Dy2 O16 2.428(5) . ? Dy2 O15 2.457(5) . ? Dy2 O3W 2.468(4) . ? Dy2 O2W 2.486(6) . ? Dy2 Dy3 3.7486(5) . ? Dy2 Dy4 3.7769(6) . ? Dy3 O3 2.275(6) . ? Dy3 O11 2.324(5) . ? Dy3 O14 2.339(5) . ? Dy3 O2 2.370(6) . ? Dy3 O15 2.385(5) . ? Dy3 O13 2.404(5) . ? Dy3 O5W 2.440(6) . ? Dy3 O4W 2.481(5) . ? Dy3 Dy4 3.7729(6) . ? Dy4 O10 2.291(6) . ? Dy4 O14 2.313(5) . ? Dy4 O7 2.375(5) . ? Dy4 O12 2.387(5) . ? Dy4 O13 2.388(5) . ? Dy4 O16 2.393(5) . ? Dy4 O7W 2.420(5) . ? Dy4 O6W 2.422(5) . ? Cl1 O20 1.394(7) . ? Cl1 O19 1.433(7) . ? Cl1 O18 1.436(5) . ? Cl1 O17 1.442(5) . ? Cl2 O21 1.407(7) . ? Cl2 O23 1.416(8) . ? Cl2 O24 1.424(7) . ? Cl2 O22 1.426(7) . ? Cl3 O25 1.246(12) . ? Cl3 O27 1.314(7) . ? Cl3 O28 1.346(9) . ? Cl3 O26 1.700(19) . ? Cl4 O30 1.420(6) . ? Cl4 O29 1.429(6) . ? Cl4 O31 1.435(7) . ? Cl4 O32 1.446(5) . ? Cl5 O33 1.388(6) . ? Cl5 O36 1.404(7) . ? Cl5 O35 1.407(7) . ? Cl5 O34 1.408(6) . ? Cl6 O40 1.365(9) . ? Cl6 O37 1.382(6) . ? Cl6 O39 1.396(7) . ? Cl6 O38 1.419(6) . ? Cl7 O41 1.401(7) . ? Cl7 O42 1.419(7) . ? Cl7 O44 1.429(5) . ? Cl7 O43 1.434(5) . ? Cl8 O45 1.407(8) . ? Cl8 O47 1.423(7) . ? Cl8 O48 1.427(7) . ? Cl8 O46 1.459(7) . ? C1 O1 1.245(10) . ? C1 O2 1.287(9) . ? C1 C2 1.497(11) . ? C2 C3 1.496(10) . ? C2 N1 1.501(10) . ? C2 C7 1.531(12) . ? C3 C4 1.526(11) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.473(12) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.556(12) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.509(12) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 O4 1.253(9) . ? C8 O3 1.259(9) . ? C8 C9 1.527(11) . ? C9 N2 1.472(10) . ? C9 C10 1.528(10) . ? C9 C14 1.537(11) . ? C10 C11 1.522(10) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.476(12) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.489(11) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.483(11) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 O6 1.241(9) . ? C15 O5 1.280(9) . ? C15 C16 1.550(11) . ? C16 N3 1.481(10) . ? C16 C17 1.498(11) . ? C16 C21 1.531(11) . ? C17 C18 1.533(11) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.475(11) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.494(12) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.556(11) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 O7 1.232(8) . ? C22 O8 1.269(9) . ? C22 C23 1.540(10) . ? C23 C24 1.523(10) . ? C23 C28 1.535(10) . ? C23 N4 1.540(10) . ? C24 C25 1.503(10) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.478(11) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.526(10) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.568(10) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 O10 1.247(10) . ? C29 O9 1.246(10) . ? C29 C30 1.545(11) . ? C30 C35 1.484(11) . ? C30 C31 1.548(10) . ? C30 N5 1.555(10) . ? C31 C32 1.519(12) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.449(13) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.548(11) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.486(11) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 O12 1.247(9) . ? C36 O11 1.267(9) . ? C36 C37 1.548(10) . ? C37 N6 1.499(9) . ? C37 C42 1.500(10) . ? C37 C38 1.513(11) . ? C38 C39 1.538(12) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.490(11) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.541(13) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.516(11) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? O13 H13C 1.0000 . ? O14 H14C 1.0000 . ? O15 H15A 1.0000 . ? O16 H16A 1.0000 . ? N1 H1A 0.9100 . ? N1 H1B 0.9100 . ? N1 H1C 0.9100 . ? N2 H2A 0.9100 . ? N2 H2B 0.9100 . ? N2 H2C 0.9100 . ? N3 H3C 0.9100 . ? N3 H3D 0.9100 . ? N3 H3E 0.9100 . ? N4 H4C 0.9100 . ? N4 H4D 0.9100 . ? N4 H4E 0.9100 . ? N5 H5C 0.9100 . ? N5 H5D 0.9100 . ? N5 H5E 0.9100 . ? N6 H6C 0.9100 . ? N6 H6D 0.9100 . ? N6 H6E 0.9100 . ? 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 O16 Dy1 O4 146.63(19) . . ? O16 Dy1 O13 70.92(17) . . ? O4 Dy1 O13 81.18(19) . . ? O16 Dy1 O5 86.16(18) . . ? O4 Dy1 O5 109.1(2) . . ? O13 Dy1 O5 145.99(18) . . ? O16 Dy1 O15 71.94(17) . . ? O4 Dy1 O15 82.23(18) . . ? O13 Dy1 O15 71.38(17) . . ? O5 Dy1 O15 77.89(17) . . ? O16 Dy1 O9 92.55(18) . . ? O4 Dy1 O9 97.41(19) . . ? O13 Dy1 O9 74.57(18) . . ? O5 Dy1 O9 132.89(18) . . ? O15 Dy1 O9 145.59(18) . . ? O16 Dy1 O1W 140.13(18) . . ? O4 Dy1 O1W 73.21(19) . . ? O13 Dy1 O1W 139.68(17) . . ? O5 Dy1 O1W 73.25(18) . . ? O15 Dy1 O1W 132.81(18) . . ? O9 Dy1 O1W 78.41(19) . . ? O16 Dy1 O17 74.13(17) . . ? O4 Dy1 O17 138.49(17) . . ? O13 Dy1 O17 123.48(18) . . ? O5 Dy1 O17 70.39(17) . . ? O15 Dy1 O17 134.49(15) . . ? O9 Dy1 O17 64.08(17) . . ? O1W Dy1 O17 66.95(17) . . ? O16 Dy1 Dy4 36.78(12) . . ? O4 Dy1 Dy4 118.26(14) . . ? O13 Dy1 Dy4 37.08(12) . . ? O5 Dy1 Dy4 122.65(13) . . ? O15 Dy1 Dy4 78.35(12) . . ? O9 Dy1 Dy4 71.58(14) . . ? O1W Dy1 Dy4 148.84(14) . . ? O17 Dy1 Dy4 91.98(13) . . ? O16 Dy1 Dy3 76.18(13) . . ? O4 Dy1 Dy3 70.51(14) . . ? O13 Dy1 Dy3 36.84(12) . . ? O5 Dy1 Dy3 114.48(13) . . ? O15 Dy1 Dy3 36.59(11) . . ? O9 Dy1 Dy3 110.80(13) . . ? O1W Dy1 Dy3 143.39(13) . . ? O17 Dy1 Dy3 149.50(12) . . ? Dy4 Dy1 Dy3 59.356(10) . . ? O16 Dy1 Dy2 36.46(13) . . ? O4 Dy1 Dy2 119.96(14) . . ? O13 Dy1 Dy2 76.55(11) . . ? O5 Dy1 Dy2 70.25(12) . . ? O15 Dy1 Dy2 37.88(11) . . ? O9 Dy1 Dy2 127.68(14) . . ? O1W Dy1 Dy2 143.49(12) . . ? O17 Dy1 Dy2 99.40(10) . . ? Dy4 Dy1 Dy2 59.202(10) . . ? Dy3 Dy1 Dy2 58.449(9) . . ? O6 Dy2 O14 144.61(18) . . ? O6 Dy2 O1 100.5(2) . . ? O14 Dy2 O1 92.68(19) . . ? O6 Dy2 O8 91.97(19) . . ? O14 Dy2 O8 97.23(18) . . ? O1 Dy2 O8 142.51(19) . . ? O6 Dy2 O16 81.23(18) . . ? O14 Dy2 O16 69.37(17) . . ? O1 Dy2 O16 144.23(18) . . ? O8 Dy2 O16 72.32(17) . . ? O6 Dy2 O15 80.01(17) . . ? O14 Dy2 O15 71.19(16) . . ? O1 Dy2 O15 76.88(18) . . ? O8 Dy2 O15 140.45(17) . . ? O16 Dy2 O15 68.20(16) . . ? O6 Dy2 O3W 70.91(18) . . ? O14 Dy2 O3W 144.37(18) . . ? O1 Dy2 O3W 71.60(19) . . ? O8 Dy2 O3W 79.63(19) . . ? O16 Dy2 O3W 139.44(17) . . ? O15 Dy2 O3W 131.54(18) . . ? O6 Dy2 O2W 143.20(18) . . ? O14 Dy2 O2W 71.74(18) . . ? O1 Dy2 O2W 76.7(2) . . ? O8 Dy2 O2W 72.38(18) . . ? O16 Dy2 O2W 122.43(19) . . ? O15 Dy2 O2W 132.79(17) . . ? O3W Dy2 O2W 73.56(19) . . ? O6 Dy2 Dy3 118.59(13) . . ? O14 Dy2 Dy3 36.55(13) . . ? O1 Dy2 Dy3 71.42(14) . . ? O8 Dy2 Dy3 131.76(13) . . ? O16 Dy2 Dy3 76.46(11) . . ? O15 Dy2 Dy3 38.57(11) . . ? O3W Dy2 Dy3 142.94(13) . . ? O2W Dy2 Dy3 95.66(13) . . ? O6 Dy2 Dy4 119.31(14) . . ? O14 Dy2 Dy4 35.26(13) . . ? O1 Dy2 Dy4 127.39(15) . . ? O8 Dy2 Dy4 72.64(13) . . ? O16 Dy2 Dy4 38.09(13) . . ? O15 Dy2 Dy4 77.84(12) . . ? O3W Dy2 Dy4 150.44(14) . . ? O2W Dy2 Dy4 88.24(14) . . ? Dy3 Dy2 Dy4 60.176(10) . . ? O6 Dy2 Dy1 69.29(13) . . ? O14 Dy2 Dy1 75.32(12) . . ? O1 Dy2 Dy1 112.92(14) . . ? O8 Dy2 Dy1 104.57(12) . . ? O16 Dy2 Dy1 34.03(13) . . ? O15 Dy2 Dy1 36.40(11) . . ? O3W Dy2 Dy1 140.08(13) . . ? O2W Dy2 Dy1 146.11(13) . . ? Dy3 Dy2 Dy1 60.432(10) . . ? Dy4 Dy2 Dy1 59.634(10) . . ? O3 Dy3 O11 90.5(2) . . ? O3 Dy3 O14 144.0(2) . . ? O11 Dy3 O14 95.19(18) . . ? O3 Dy3 O2 103.1(2) . . ? O11 Dy3 O2 141.29(19) . . ? O14 Dy3 O2 94.44(19) . . ? O3 Dy3 O15 82.76(18) . . ? O11 Dy3 O15 144.42(18) . . ? O14 Dy3 O15 72.07(17) . . ? O2 Dy3 O15 73.95(18) . . ? O3 Dy3 O13 77.47(18) . . ? O11 Dy3 O13 74.31(18) . . ? O14 Dy3 O13 70.00(16) . . ? O2 Dy3 O13 143.73(18) . . ? O15 Dy3 O13 70.13(17) . . ? O3 Dy3 O5W 70.3(2) . . ? O11 Dy3 O5W 78.3(2) . . ? O14 Dy3 O5W 145.68(19) . . ? O2 Dy3 O5W 72.78(19) . . ? O15 Dy3 O5W 130.36(19) . . ? O13 Dy3 O5W 137.05(17) . . ? O3 Dy3 O4W 141.71(19) . . ? O11 Dy3 O4W 71.65(18) . . ? O14 Dy3 O4W 72.99(17) . . ? O2 Dy3 O4W 75.6(2) . . ? O15 Dy3 O4W 130.93(17) . . ? O13 Dy3 O4W 126.20(18) . . ? O5W Dy3 O4W 73.00(19) . . ? O3 Dy3 Dy2 122.52(14) . . ? O11 Dy3 Dy2 130.39(14) . . ? O14 Dy3 Dy2 36.09(12) . . ? O2 Dy3 Dy2 71.18(13) . . ? O15 Dy3 Dy2 39.96(11) . . ? O13 Dy3 Dy2 78.12(11) . . ? O5W Dy3 Dy2 143.69(13) . . ? O4W Dy3 Dy2 93.78(12) . . ? O3 Dy3 Dy4 115.30(14) . . ? O11 Dy3 Dy4 72.79(14) . . ? O14 Dy3 Dy4 35.56(12) . . ? O2 Dy3 Dy4 128.93(14) . . ? O15 Dy3 Dy4 78.69(12) . . ? O13 Dy3 Dy4 37.92(12) . . ? O5W Dy3 Dy4 150.48(15) . . ? O4W Dy3 Dy4 91.99(12) . . ? Dy2 Dy3 Dy4 60.283(10) . . ? O3 Dy3 Dy1 68.86(14) . . ? O11 Dy3 Dy1 108.90(13) . . ? O14 Dy3 Dy1 75.64(13) . . ? O2 Dy3 Dy1 109.81(14) . . ? O15 Dy3 Dy1 36.41(12) . . ? O13 Dy3 Dy1 35.72(12) . . ? O5W Dy3 Dy1 138.49(15) . . ? O4W Dy3 Dy1 148.51(12) . . ? Dy2 Dy3 Dy1 61.119(9) . . ? Dy4 Dy3 Dy1 59.897(10) . . ? O10 Dy4 O14 143.5(2) . . ? O10 Dy4 O7 96.95(19) . . ? O14 Dy4 O7 92.72(17) . . ? O10 Dy4 O12 102.7(2) . . ? O14 Dy4 O12 89.64(18) . . ? O7 Dy4 O12 143.28(19) . . ? O10 Dy4 O13 79.50(19) . . ? O14 Dy4 O13 70.73(17) . . ? O7 Dy4 O13 139.95(18) . . ? O12 Dy4 O13 74.78(18) . . ? O10 Dy4 O16 79.8(2) . . ? O14 Dy4 O16 70.02(17) . . ? O7 Dy4 O16 71.75(18) . . ? O12 Dy4 O16 141.98(18) . . ? O13 Dy4 O16 68.35(16) . . ? O10 Dy4 O7W 71.0(2) . . ? O14 Dy4 O7W 145.46(19) . . ? O7 Dy4 O7W 79.86(19) . . ? O12 Dy4 O7W 77.68(19) . . ? O13 Dy4 O7W 133.60(18) . . ? O16 Dy4 O7W 136.09(18) . . ? O10 Dy4 O6W 143.9(2) . . ? O14 Dy4 O6W 72.54(18) . . ? O7 Dy4 O6W 74.15(19) . . ? O12 Dy4 O6W 71.69(18) . . ? O13 Dy4 O6W 129.60(18) . . ? O16 Dy4 O6W 127.08(17) . . ? O7W Dy4 O6W 72.98(18) . . ? O10 Dy4 Dy3 117.71(15) . . ? O14 Dy4 Dy3 36.03(11) . . ? O7 Dy4 Dy3 127.00(14) . . ? O12 Dy4 Dy3 69.00(14) . . ? O13 Dy4 Dy3 38.22(12) . . ? O16 Dy4 Dy3 76.31(13) . . ? O7W Dy4 Dy3 146.62(13) . . ? O6W Dy4 Dy3 94.06(14) . . ? O10 Dy4 Dy2 118.56(15) . . ? O14 Dy4 Dy2 35.28(12) . . ? O7 Dy4 Dy2 69.11(14) . . ? O12 Dy4 Dy2 124.30(14) . . ? O13 Dy4 Dy2 77.69(12) . . ? O16 Dy4 Dy2 38.77(12) . . ? O7W Dy4 Dy2 148.18(13) . . ? O6W Dy4 Dy2 91.37(13) . . ? Dy3 Dy4 Dy2 59.540(10) . . ? O10 Dy4 Dy1 66.91(16) . . ? O14 Dy4 Dy1 76.59(13) . . ? O7 Dy4 Dy1 105.54(14) . . ? O12 Dy4 Dy1 110.63(14) . . ? O13 Dy4 Dy1 36.25(12) . . ? O16 Dy4 Dy1 34.91(12) . . ? O7W Dy4 Dy1 137.94(13) . . ? O6W Dy4 Dy1 149.05(14) . . ? Dy3 Dy4 Dy1 60.747(10) . . ? Dy2 Dy4 Dy1 61.164(10) . . ? O20 Cl1 O19 110.0(4) . . ? O20 Cl1 O18 108.2(4) . . ? O19 Cl1 O18 109.5(4) . . ? O20 Cl1 O17 110.6(4) . . ? O19 Cl1 O17 109.8(4) . . ? O18 Cl1 O17 108.7(3) . . ? O21 Cl2 O23 109.8(5) . . ? O21 Cl2 O24 109.9(5) . . ? O23 Cl2 O24 112.4(5) . . ? O21 Cl2 O22 110.5(5) . . ? O23 Cl2 O22 107.6(5) . . ? O24 Cl2 O22 106.6(5) . . ? O25 Cl3 O27 123.5(8) . . ? O25 Cl3 O28 121.1(8) . . ? O27 Cl3 O28 114.1(7) . . ? O25 Cl3 O26 83.7(8) . . ? O27 Cl3 O26 106.2(8) . . ? O28 Cl3 O26 92.1(8) . . ? O30 Cl4 O29 111.0(5) . . ? O30 Cl4 O31 110.8(4) . . ? O29 Cl4 O31 108.7(4) . . ? O30 Cl4 O32 107.4(4) . . ? O29 Cl4 O32 109.4(4) . . ? O31 Cl4 O32 109.6(4) . . ? O33 Cl5 O36 109.3(5) . . ? O33 Cl5 O35 108.9(5) . . ? O36 Cl5 O35 109.0(5) . . ? O33 Cl5 O34 110.3(4) . . ? O36 Cl5 O34 110.6(4) . . ? O35 Cl5 O34 108.7(5) . . ? O40 Cl6 O37 109.4(6) . . ? O40 Cl6 O39 110.6(5) . . ? O37 Cl6 O39 109.7(4) . . ? O40 Cl6 O38 112.6(6) . . ? O37 Cl6 O38 105.6(5) . . ? O39 Cl6 O38 109.0(4) . . ? O41 Cl7 O42 109.4(4) . . ? O41 Cl7 O44 111.5(5) . . ? O42 Cl7 O44 105.5(4) . . ? O41 Cl7 O43 110.2(4) . . ? O42 Cl7 O43 110.9(4) . . ? O44 Cl7 O43 109.2(4) . . ? O45 Cl8 O47 110.9(5) . . ? O45 Cl8 O48 113.0(5) . . ? O47 Cl8 O48 109.8(5) . . ? O45 Cl8 O46 106.4(5) . . ? O47 Cl8 O46 109.9(5) . . ? O48 Cl8 O46 106.6(5) . . ? O1 C1 O2 125.7(9) . . ? O1 C1 C2 118.2(8) . . ? O2 C1 C2 116.1(8) . . ? C1 C2 C3 111.5(7) . . ? C1 C2 N1 107.9(7) . . ? C3 C2 N1 107.5(7) . . ? C1 C2 C7 110.9(7) . . ? C3 C2 C7 110.3(7) . . ? N1 C2 C7 108.7(7) . . ? C2 C3 C4 113.6(8) . . ? C2 C3 H3A 108.8 . . ? C4 C3 H3A 108.8 . . ? C2 C3 H3B 108.8 . . ? C4 C3 H3B 108.8 . . ? H3A C3 H3B 107.7 . . ? C5 C4 C3 111.3(7) . . ? C5 C4 H4A 109.4 . . ? C3 C4 H4A 109.4 . . ? C5 C4 H4B 109.4 . . ? C3 C4 H4B 109.4 . . ? H4A C4 H4B 108.0 . . ? C4 C5 C6 112.0(8) . . ? C4 C5 H5A 109.2 . . ? C6 C5 H5A 109.2 . . ? C4 C5 H5B 109.2 . . ? C6 C5 H5B 109.2 . . ? H5A C5 H5B 107.9 . . ? C7 C6 C5 107.6(8) . . ? C7 C6 H6A 110.2 . . ? C5 C6 H6A 110.2 . . ? C7 C6 H6B 110.2 . . ? C5 C6 H6B 110.2 . . ? H6A C6 H6B 108.5 . . ? C6 C7 C2 115.2(8) . . ? C6 C7 H7A 108.5 . . ? C2 C7 H7A 108.5 . . ? C6 C7 H7B 108.5 . . ? C2 C7 H7B 108.5 . . ? H7A C7 H7B 107.5 . . ? O4 C8 O3 125.5(8) . . ? O4 C8 C9 118.8(8) . . ? O3 C8 C9 115.7(7) . . ? N2 C9 C10 110.2(7) . . ? N2 C9 C8 107.9(6) . . ? C10 C9 C8 110.3(7) . . ? N2 C9 C14 109.1(7) . . ? C10 C9 C14 109.3(7) . . ? C8 C9 C14 110.1(7) . . ? C11 C10 C9 114.0(7) . . ? C11 C10 H10A 108.8 . . ? C9 C10 H10A 108.8 . . ? C11 C10 H10B 108.8 . . ? C9 C10 H10B 108.8 . . ? H10A C10 H10B 107.7 . . ? C12 C11 C10 110.4(7) . . ? C12 C11 H11A 109.6 . . ? C10 C11 H11A 109.6 . . ? C12 C11 H11B 109.6 . . ? C10 C11 H11B 109.6 . . ? H11A C11 H11B 108.1 . . ? C11 C12 C13 115.3(8) . . ? C11 C12 H12A 108.5 . . ? C13 C12 H12A 108.5 . . ? C11 C12 H12B 108.5 . . ? C13 C12 H12B 108.5 . . ? H12A C12 H12B 107.5 . . ? C14 C13 C12 110.5(8) . . ? C14 C13 H13A 109.6 . . ? C12 C13 H13A 109.6 . . ? C14 C13 H13B 109.6 . . ? C12 C13 H13B 109.6 . . ? H13A C13 H13B 108.1 . . ? C13 C14 C9 114.3(7) . . ? C13 C14 H14A 108.7 . . ? C9 C14 H14A 108.7 . . ? C13 C14 H14B 108.7 . . ? C9 C14 H14B 108.7 . . ? H14A C14 H14B 107.6 . . ? O6 C15 O5 127.9(8) . . ? O6 C15 C16 115.3(7) . . ? O5 C15 C16 116.8(7) . . ? N3 C16 C17 107.9(7) . . ? N3 C16 C21 109.7(7) . . ? C17 C16 C21 110.4(7) . . ? N3 C16 C15 108.4(6) . . ? C17 C16 C15 111.0(7) . . ? C21 C16 C15 109.3(7) . . ? C16 C17 C18 112.9(8) . . ? C16 C17 H17A 109.0 . . ? C18 C17 H17A 109.0 . . ? C16 C17 H17B 109.0 . . ? C18 C17 H17B 109.0 . . ? H17A C17 H17B 107.8 . . ? C19 C18 C17 111.5(8) . . ? C19 C18 H18A 109.3 . . ? C17 C18 H18A 109.3 . . ? C19 C18 H18B 109.3 . . ? C17 C18 H18B 109.3 . . ? H18A C18 H18B 108.0 . . ? C18 C19 C20 111.7(7) . . ? C18 C19 H19A 109.3 . . ? C20 C19 H19A 109.3 . . ? C18 C19 H19B 109.3 . . ? C20 C19 H19B 109.3 . . ? H19A C19 H19B 107.9 . . ? C19 C20 C21 112.3(7) . . ? C19 C20 H20A 109.1 . . ? C21 C20 H20A 109.1 . . ? C19 C20 H20B 109.1 . . ? C21 C20 H20B 109.1 . . ? H20A C20 H20B 107.9 . . ? C16 C21 C20 112.8(7) . . ? C16 C21 H21A 109.0 . . ? C20 C21 H21A 109.0 . . ? C16 C21 H21B 109.0 . . ? C20 C21 H21B 109.0 . . ? H21A C21 H21B 107.8 . . ? O7 C22 O8 126.6(8) . . ? O7 C22 C23 118.1(8) . . ? O8 C22 C23 115.3(7) . . ? C24 C23 C28 112.1(7) . . ? C24 C23 C22 113.1(6) . . ? C28 C23 C22 108.5(7) . . ? C24 C23 N4 110.0(7) . . ? C28 C23 N4 107.6(6) . . ? C22 C23 N4 105.2(6) . . ? C25 C24 C23 113.3(6) . . ? C25 C24 H24A 108.9 . . ? C23 C24 H24A 108.9 . . ? C25 C24 H24B 108.9 . . ? C23 C24 H24B 108.9 . . ? H24A C24 H24B 107.7 . . ? C26 C25 C24 113.0(7) . . ? C26 C25 H25A 109.0 . . ? C24 C25 H25A 109.0 . . ? C26 C25 H25B 109.0 . . ? C24 C25 H25B 109.0 . . ? H25A C25 H25B 107.8 . . ? C25 C26 C27 113.9(8) . . ? C25 C26 H26A 108.8 . . ? C27 C26 H26A 108.8 . . ? C25 C26 H26B 108.8 . . ? C27 C26 H26B 108.8 . . ? H26A C26 H26B 107.7 . . ? C26 C27 C28 110.2(7) . . ? C26 C27 H27A 109.6 . . ? C28 C27 H27A 109.6 . . ? C26 C27 H27B 109.6 . . ? C28 C27 H27B 109.6 . . ? H27A C27 H27B 108.1 . . ? C23 C28 C27 112.1(7) . . ? C23 C28 H28A 109.2 . . ? C27 C28 H28A 109.2 . . ? C23 C28 H28B 109.2 . . ? C27 C28 H28B 109.2 . . ? H28A C28 H28B 107.9 . . ? O10 C29 O9 126.7(9) . . ? O10 C29 C30 115.1(8) . . ? O9 C29 C30 118.2(8) . . ? C35 C30 C29 115.2(7) . . ? C35 C30 C31 111.4(7) . . ? C29 C30 C31 109.1(6) . . ? C35 C30 N5 108.7(6) . . ? C29 C30 N5 104.8(7) . . ? C31 C30 N5 107.2(7) . . ? C32 C31 C30 111.4(7) . . ? C32 C31 H31A 109.4 . . ? C30 C31 H31A 109.4 . . ? C32 C31 H31B 109.4 . . ? C30 C31 H31B 109.4 . . ? H31A C31 H31B 108.0 . . ? C33 C32 C31 113.6(8) . . ? C33 C32 H32A 108.8 . . ? C31 C32 H32A 108.8 . . ? C33 C32 H32B 108.8 . . ? C31 C32 H32B 108.8 . . ? H32A C32 H32B 107.7 . . ? C32 C33 C34 111.4(9) . . ? C32 C33 H33A 109.3 . . ? C34 C33 H33A 109.3 . . ? C32 C33 H33B 109.3 . . ? C34 C33 H33B 109.3 . . ? H33A C33 H33B 108.0 . . ? C35 C34 C33 109.5(8) . . ? C35 C34 H34A 109.8 . . ? C33 C34 H34A 109.8 . . ? C35 C34 H34B 109.8 . . ? C33 C34 H34B 109.8 . . ? H34A C34 H34B 108.2 . . ? C30 C35 C34 115.7(8) . . ? C30 C35 H35A 108.3 . . ? C34 C35 H35A 108.3 . . ? C30 C35 H35B 108.3 . . ? C34 C35 H35B 108.3 . . ? H35A C35 H35B 107.4 . . ? O12 C36 O11 126.0(7) . . ? O12 C36 C37 118.9(8) . . ? O11 C36 C37 114.9(7) . . ? N6 C37 C42 107.8(7) . . ? N6 C37 C38 108.8(7) . . ? C42 C37 C38 112.1(8) . . ? N6 C37 C36 104.5(7) . . ? C42 C37 C36 108.7(7) . . ? C38 C37 C36 114.4(7) . . ? C37 C38 C39 112.7(8) . . ? C37 C38 H38A 109.0 . . ? C39 C38 H38A 109.0 . . ? C37 C38 H38B 109.0 . . ? C39 C38 H38B 109.0 . . ? H38A C38 H38B 107.8 . . ? C40 C39 C38 114.2(8) . . ? C40 C39 H39A 108.7 . . ? C38 C39 H39A 108.7 . . ? C40 C39 H39B 108.7 . . ? C38 C39 H39B 108.7 . . ? H39A C39 H39B 107.6 . . ? C39 C40 C41 108.5(8) . . ? C39 C40 H40A 110.0 . . ? C41 C40 H40A 110.0 . . ? C39 C40 H40B 110.0 . . ? C41 C40 H40B 110.0 . . ? H40A C40 H40B 108.4 . . ? C42 C41 C40 111.2(8) . . ? C42 C41 H41A 109.4 . . ? C40 C41 H41A 109.4 . . ? C42 C41 H41B 109.4 . . ? C40 C41 H41B 109.4 . . ? H41A C41 H41B 108.0 . . ? C37 C42 C41 111.1(7) . . ? C37 C42 H42A 109.4 . . ? C41 C42 H42A 109.4 . . ? C37 C42 H42B 109.4 . . ? C41 C42 H42B 109.4 . . ? H42A C42 H42B 108.0 . . ? C1 O1 Dy2 136.2(6) . . ? C1 O2 Dy3 134.0(6) . . ? C8 O3 Dy3 138.8(5) . . ? C8 O4 Dy1 134.3(5) . . ? C15 O5 Dy1 132.1(5) . . ? C15 O6 Dy2 139.0(5) . . ? C22 O7 Dy4 134.8(6) . . ? C22 O8 Dy2 131.0(5) . . ? C29 O9 Dy1 127.3(6) . . ? C29 O10 Dy4 140.0(6) . . ? C36 O11 Dy3 133.8(5) . . ? C36 O12 Dy4 137.0(5) . . ? Dy1 O13 Dy4 106.67(18) . . ? Dy1 O13 Dy3 107.4(2) . . ? Dy4 O13 Dy3 103.86(18) . . ? Dy1 O13 H13C 112.8 . . ? Dy4 O13 H13C 112.8 . . ? Dy3 O13 H13C 112.8 . . ? Dy2 O14 Dy4 109.5(2) . . ? Dy2 O14 Dy3 107.4(2) . . ? Dy4 O14 Dy3 108.41(18) . . ? Dy2 O14 H14C 110.5 . . ? Dy4 O14 H14C 110.5 . . ? Dy3 O14 H14C 110.5 . . ? Dy1 O15 Dy3 107.00(18) . . ? Dy1 O15 Dy2 105.72(18) . . ? Dy3 O15 Dy2 101.46(18) . . ? Dy1 O15 H15A 113.9 . . ? Dy3 O15 H15A 113.9 . . ? Dy2 O15 H15A 113.9 . . ? Dy1 O16 Dy4 108.31(18) . . ? Dy1 O16 Dy2 109.5(2) . . ? Dy4 O16 Dy2 103.14(19) . . ? Dy1 O16 H16A 111.8 . . ? Dy4 O16 H16A 111.8 . . ? Dy2 O16 H16A 111.8 . . ? Cl1 O17 Dy1 136.2(3) . . ? C2 N1 H1A 109.5 . . ? C2 N1 H1B 109.5 . . ? H1A N1 H1B 109.5 . . ? C2 N1 H1C 109.5 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? C9 N2 H2A 109.5 . . ? C9 N2 H2B 109.5 . . ? H2A N2 H2B 109.5 . . ? C9 N2 H2C 109.5 . . ? H2A N2 H2C 109.5 . . ? H2B N2 H2C 109.5 . . ? C16 N3 H3C 109.5 . . ? C16 N3 H3D 109.5 . . ? H3C N3 H3D 109.5 . . ? C16 N3 H3E 109.5 . . ? H3C N3 H3E 109.5 . . ? H3D N3 H3E 109.5 . . ? C23 N4 H4C 109.5 . . ? C23 N4 H4D 109.5 . . ? H4C N4 H4D 109.5 . . ? C23 N4 H4E 109.5 . . ? H4C N4 H4E 109.5 . . ? H4D N4 H4E 109.5 . . ? C30 N5 H5C 109.5 . . ? C30 N5 H5D 109.5 . . ? H5C N5 H5D 109.5 . . ? C30 N5 H5E 109.5 . . ? H5C N5 H5E 109.5 . . ? H5D N5 H5E 109.5 . . ? C37 N6 H6C 109.5 . . ? C37 N6 H6D 109.5 . . ? H6C N6 H6D 109.5 . . ? C37 N6 H6E 109.5 . . ? H6C N6 H6E 109.5 . . ? H6D N6 H6E 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.118 _refine_diff_density_min -0.982 _refine_diff_density_rms 0.142 # Attachment '- complex6.cif' data_complex6 _database_code_depnum_ccdc_archive 'CCDC 791396' #TrackingRef '- complex6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H118 Cl8 N6 O66 Yb4' _chemical_formula_weight 2739.18 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' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M p2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 13.0726(2) _cell_length_b 26.5154(4) _cell_length_c 26.5492(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9202.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 23749 _cell_measurement_theta_min 2.7715 _cell_measurement_theta_max 29.1018 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.36 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.977 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5424 _exptl_absorpt_coefficient_mu 4.375 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2736 _exptl_absorpt_correction_T_max 0.3019 _exptl_absorpt_process_details ? _exptl_special_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.46 (release 27-08-2009 CrysAlis171 .NET) (compiled Aug 27 2009,17:19:36) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 173(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 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42080 _diffrn_reflns_av_R_equivalents 0.0429 _diffrn_reflns_av_sigmaI/netI 0.0656 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.78 _diffrn_reflns_theta_max 26.00 _reflns_number_total 17260 _reflns_number_gt 15037 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. Non-hydrogen atoms were refined anisotropically, except for o13 and c22 were refined isotropically due to disorder ; _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^)+(0.0113P)^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 -0.004(4) _refine_ls_number_reflns 17260 _refine_ls_number_parameters 1135 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0359 _refine_ls_R_factor_gt 0.0286 _refine_ls_wR_factor_ref 0.0471 _refine_ls_wR_factor_gt 0.0462 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.004 _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 Yb1 Yb 0.020563(19) 0.466698(9) 0.838694(9) 0.00994(6) Uani 1 1 d . . . Yb2 Yb -0.208120(18) 0.497593(10) 0.757525(9) 0.00987(6) Uani 1 1 d . . . Yb3 Yb 0.047209(18) 0.488377(9) 0.699767(9) 0.00987(6) Uani 1 1 d . . . Yb4 Yb -0.013639(19) 0.594949(9) 0.784391(9) 0.00983(6) Uani 1 1 d . . . Cl1 Cl -0.15673(11) 0.50580(6) 0.95420(5) 0.0204(4) Uani 1 1 d . . . Cl2 Cl -0.33137(15) 0.69647(7) 0.67822(7) 0.0334(5) Uani 1 1 d . . . Cl3 Cl -0.04059(16) 0.76203(8) 0.91740(9) 0.0482(6) Uani 1 1 d . . . Cl4 Cl 0.49778(11) 0.53592(6) 1.00116(5) 0.0211(4) Uani 1 1 d . . . Cl5 Cl -0.03417(13) 0.29619(6) 0.79849(7) 0.0255(4) Uani 1 1 d . . . Cl6 Cl 0.44409(13) 0.47246(7) 0.61799(6) 0.0285(4) Uani 1 1 d . . . Cl7 Cl 0.39017(11) 0.50078(6) 0.84332(6) 0.0208(3) Uani 1 1 d . . . Cl8 Cl 0.25906(15) 0.27693(7) 1.02047(7) 0.0375(5) Uani 1 1 d . . . C1 C -0.1552(5) 0.4259(2) 0.6600(2) 0.0171(14) Uani 1 1 d . . . C2 C -0.1975(5) 0.3836(2) 0.6277(2) 0.0128(14) Uani 1 1 d . . . C3 C -0.2853(5) 0.4014(2) 0.5944(2) 0.0179(14) Uani 1 1 d . . . H3A H -0.3374 0.4181 0.6157 0.021 Uiso 1 1 calc R . . H3B H -0.2590 0.4268 0.5703 0.021 Uiso 1 1 calc R . . C4 C -0.3361(5) 0.3592(3) 0.5651(2) 0.0273(17) Uani 1 1 d . . . H4A H -0.3965 0.3726 0.5471 0.033 Uiso 1 1 calc R . . H4B H -0.2876 0.3460 0.5396 0.033 Uiso 1 1 calc R . . C5 C -0.3687(6) 0.3171(3) 0.5990(3) 0.043(2) Uani 1 1 d . . . H5A H -0.3980 0.2894 0.5785 0.051 Uiso 1 1 calc R . . H5B H -0.4227 0.3294 0.6222 0.051 Uiso 1 1 calc R . . C6 C -0.2797(6) 0.2970(3) 0.6296(3) 0.042(2) Uani 1 1 d . . . H6A H -0.3044 0.2704 0.6527 0.050 Uiso 1 1 calc R . . H6B H -0.2286 0.2818 0.6067 0.050 Uiso 1 1 calc R . . C7 C -0.2304(5) 0.3384(2) 0.6595(3) 0.0269(17) Uani 1 1 d . . . H7A H -0.1696 0.3246 0.6770 0.032 Uiso 1 1 calc R . . H7B H -0.2790 0.3501 0.6856 0.032 Uiso 1 1 calc R . . C8 C 0.1838(4) 0.4090(2) 0.7652(2) 0.0142(14) Uani 1 1 d . . . C9 C 0.2561(4) 0.3647(2) 0.7571(2) 0.0116(13) Uani 1 1 d . . . C10 C 0.3646(4) 0.3826(2) 0.7463(2) 0.0212(16) Uani 1 1 d . . . H10A H 0.3921 0.3992 0.7768 0.025 Uiso 1 1 calc R . . H10B H 0.3622 0.4082 0.7191 0.025 Uiso 1 1 calc R . . C11 C 0.4376(5) 0.3406(2) 0.7306(3) 0.0277(18) Uani 1 1 d . . . H11A H 0.5042 0.3554 0.7206 0.033 Uiso 1 1 calc R . . H11B H 0.4497 0.3178 0.7595 0.033 Uiso 1 1 calc R . . C12 C 0.3946(5) 0.3108(3) 0.6873(3) 0.0295(18) Uani 1 1 d . . . H12A H 0.4410 0.2824 0.6796 0.035 Uiso 1 1 calc R . . H12B H 0.3911 0.3327 0.6571 0.035 Uiso 1 1 calc R . . C13 C 0.2895(5) 0.2905(2) 0.6986(2) 0.0242(16) Uani 1 1 d . . . H13A H 0.2936 0.2661 0.7267 0.029 Uiso 1 1 calc R . . H13B H 0.2628 0.2726 0.6686 0.029 Uiso 1 1 calc R . . C14 C 0.2170(5) 0.3329(2) 0.7127(2) 0.0224(15) Uani 1 1 d . . . H14A H 0.1496 0.3184 0.7216 0.027 Uiso 1 1 calc R . . H14B H 0.2071 0.3551 0.6831 0.027 Uiso 1 1 calc R . . C15 C -0.2072(5) 0.4143(2) 0.8483(2) 0.0149(14) Uani 1 1 d . . . C16 C -0.2782(5) 0.3739(2) 0.8716(2) 0.0142(14) Uani 1 1 d . . . C17 C -0.3294(5) 0.3429(2) 0.8302(2) 0.0201(16) Uani 1 1 d . . . H17A H -0.2763 0.3246 0.8109 0.024 Uiso 1 1 calc R . . H17B H -0.3652 0.3659 0.8067 0.024 Uiso 1 1 calc R . . C18 C -0.4068(5) 0.3046(2) 0.8516(3) 0.0272(17) Uani 1 1 d . . . H18A H -0.4397 0.2860 0.8237 0.033 Uiso 1 1 calc R . . H18B H -0.3706 0.2799 0.8732 0.033 Uiso 1 1 calc R . . C19 C -0.4870(5) 0.3314(2) 0.8820(3) 0.0307(18) Uani 1 1 d . . . H19A H -0.5346 0.3063 0.8966 0.037 Uiso 1 1 calc R . . H19B H -0.5269 0.3539 0.8597 0.037 Uiso 1 1 calc R . . C20 C -0.4398(5) 0.3624(2) 0.9242(3) 0.0264(17) Uani 1 1 d . . . H20A H -0.4073 0.3395 0.9489 0.032 Uiso 1 1 calc R . . H20B H -0.4943 0.3814 0.9418 0.032 Uiso 1 1 calc R . . C21 C -0.3600(5) 0.3992(2) 0.9040(2) 0.0221(16) Uani 1 1 d . . . H21A H -0.3265 0.4162 0.9328 0.026 Uiso 1 1 calc R . . H21B H -0.3949 0.4254 0.8837 0.026 Uiso 1 1 calc R . . C22 C -0.2557(4) 0.6008(2) 0.8204(2) 0.0109(13) Uani 1 1 d U . . C23 C -0.3242(4) 0.6229(2) 0.8618(2) 0.0113(14) Uani 1 1 d . . . C24 C -0.2612(5) 0.6482(2) 0.9042(2) 0.0141(14) Uani 1 1 d . . . H24A H -0.2184 0.6224 0.9210 0.017 Uiso 1 1 calc R . . H24B H -0.2150 0.6737 0.8892 0.017 Uiso 1 1 calc R . . C25 C -0.3298(5) 0.6738(2) 0.9436(2) 0.0176(15) Uani 1 1 d . . . H25A H -0.3688 0.6477 0.9620 0.021 Uiso 1 1 calc R . . H25B H -0.2863 0.6918 0.9682 0.021 Uiso 1 1 calc R . . C26 C -0.4035(5) 0.7106(2) 0.9204(2) 0.0216(16) Uani 1 1 d . . . H26A H -0.3650 0.7393 0.9060 0.026 Uiso 1 1 calc R . . H26B H -0.4497 0.7239 0.9468 0.026 Uiso 1 1 calc R . . C27 C -0.4686(5) 0.6849(2) 0.8780(2) 0.0194(15) Uani 1 1 d . . . H27A H -0.5137 0.6590 0.8931 0.023 Uiso 1 1 calc R . . H27B H -0.5124 0.7105 0.8615 0.023 Uiso 1 1 calc R . . C28 C -0.4007(4) 0.6607(2) 0.8393(2) 0.0151(14) Uani 1 1 d . . . H28A H -0.3623 0.6874 0.8213 0.018 Uiso 1 1 calc R . . H28B H -0.4439 0.6430 0.8142 0.018 Uiso 1 1 calc R . . C29 C 0.1119(4) 0.5696(2) 0.8887(2) 0.0126(14) Uani 1 1 d . . . C30 C 0.1664(4) 0.5955(2) 0.9330(2) 0.0157(14) Uani 1 1 d . . . C31 C 0.0895(5) 0.6105(2) 0.9728(2) 0.0208(16) Uani 1 1 d . . . H31A H 0.0570 0.5797 0.9866 0.025 Uiso 1 1 calc R . . H31B H 0.0353 0.6312 0.9571 0.025 Uiso 1 1 calc R . . C32 C 0.1377(5) 0.6401(3) 1.0159(3) 0.035(2) Uani 1 1 d . . . H32A H 0.0833 0.6513 1.0393 0.042 Uiso 1 1 calc R . . H32B H 0.1849 0.6178 1.0347 0.042 Uiso 1 1 calc R . . C33 C 0.1949(6) 0.6849(3) 0.9977(3) 0.038(2) Uani 1 1 d . . . H33A H 0.2287 0.7017 1.0265 0.046 Uiso 1 1 calc R . . H33B H 0.1463 0.7092 0.9825 0.046 Uiso 1 1 calc R . . C34 C 0.2751(5) 0.6706(2) 0.9588(3) 0.0253(17) Uani 1 1 d . . . H34A H 0.3286 0.6496 0.9749 0.030 Uiso 1 1 calc R . . H34B H 0.3082 0.7015 0.9456 0.030 Uiso 1 1 calc R . . C35 C 0.2268(5) 0.6412(2) 0.9151(3) 0.0220(16) Uani 1 1 d . . . H35A H 0.1807 0.6639 0.8961 0.026 Uiso 1 1 calc R . . H35B H 0.2815 0.6299 0.8919 0.026 Uiso 1 1 calc R . . C36 C 0.1809(4) 0.5920(2) 0.7024(2) 0.0133(13) Uani 1 1 d . . . C37 C 0.2815(5) 0.6176(2) 0.6863(2) 0.0157(14) Uani 1 1 d . . . C38 C 0.2780(5) 0.6750(2) 0.6811(2) 0.0217(16) Uani 1 1 d . . . H38A H 0.2167 0.6846 0.6614 0.026 Uiso 1 1 calc R . . H38B H 0.3391 0.6865 0.6623 0.026 Uiso 1 1 calc R . . C39 C 0.2747(5) 0.7019(2) 0.7328(3) 0.0294(18) Uani 1 1 d . . . H39A H 0.2820 0.7387 0.7276 0.035 Uiso 1 1 calc R . . H39B H 0.2075 0.6958 0.7488 0.035 Uiso 1 1 calc R . . C40 C 0.3577(5) 0.6840(3) 0.7673(3) 0.0292(18) Uani 1 1 d . . . H40A H 0.3494 0.6999 0.8008 0.035 Uiso 1 1 calc R . . H40B H 0.4251 0.6942 0.7536 0.035 Uiso 1 1 calc R . . C41 C 0.3544(5) 0.6270(3) 0.7728(3) 0.0296(18) Uani 1 1 d . . . H41A H 0.4104 0.6160 0.7954 0.036 Uiso 1 1 calc R . . H41B H 0.2887 0.6171 0.7884 0.036 Uiso 1 1 calc R . . C42 C 0.3653(4) 0.6015(2) 0.7232(2) 0.0188(15) Uani 1 1 d . . . H42A H 0.3619 0.5645 0.7281 0.023 Uiso 1 1 calc R . . H42B H 0.4330 0.6096 0.7087 0.023 Uiso 1 1 calc R . . O1 O -0.2180(3) 0.44722(16) 0.68851(15) 0.0235(11) Uani 1 1 d . . . O1W O 0.0766(3) 0.41609(15) 0.90663(15) 0.0155(10) Uani 1 1 d . . . O2 O -0.0612(3) 0.43521(15) 0.65645(16) 0.0218(11) Uani 1 1 d . . . O2W O -0.2793(3) 0.55295(15) 0.69405(15) 0.0187(10) Uani 1 1 d . . . O3 O 0.1670(3) 0.43550(15) 0.72743(15) 0.0192(11) Uani 1 1 d . . . O3W O -0.3847(3) 0.47335(16) 0.74634(15) 0.0225(11) Uani 1 1 d . . . O4 O 0.1493(3) 0.41633(15) 0.80913(15) 0.0176(10) Uani 1 1 d . . . O4W O -0.0025(3) 0.53511(15) 0.62583(13) 0.0193(10) Uani 1 1 d . . . O5 O -0.1152(3) 0.41547(15) 0.86237(14) 0.0145(10) Uani 1 1 d . . . O5W O 0.1398(3) 0.45395(16) 0.62997(15) 0.0213(11) Uani 1 1 d . . . O6 O -0.2500(3) 0.44259(15) 0.81683(14) 0.0150(10) Uani 1 1 d . . . O6W O -0.0787(3) 0.64608(15) 0.71734(15) 0.0204(10) Uani 1 1 d . . . O7 O -0.1736(3) 0.62258(15) 0.81060(15) 0.0179(10) Uani 1 1 d . . . O7W O 0.0230(3) 0.67945(14) 0.80609(15) 0.0218(10) Uani 1 1 d . . . O8W O 0.1631(3) 0.57910(16) 0.48347(16) 0.0285(12) Uani 1 1 d . . . O8 O -0.2905(3) 0.56169(15) 0.79961(15) 0.0173(10) Uani 1 1 d . . . O9 O 0.1207(3) 0.52227(15) 0.88532(14) 0.0153(10) Uani 1 1 d . . . O9W O 0.3535(3) 0.53023(17) 0.49517(16) 0.0283(12) Uani 1 1 d . . . O10 O 0.0590(3) 0.59702(15) 0.86157(14) 0.0170(10) Uani 1 1 d . . . O10W O 0.1198(3) 0.60690(17) 0.58330(16) 0.0281(12) Uani 1 1 d . . . O11 O 0.1684(3) 0.54860(15) 0.68602(14) 0.0166(10) Uani 1 1 d . . . O11W O 0.0057(4) 0.68230(16) 0.62756(15) 0.0294(12) Uani 1 1 d . . . O12W O -0.3328(4) 0.5460(2) 0.59722(18) 0.0514(16) Uani 1 1 d . . . O12 O 0.1218(3) 0.61575(15) 0.73158(15) 0.0165(10) Uani 1 1 d . . . O13W O -0.1624(4) 0.6744(2) 0.56418(19) 0.0477(16) Uani 1 1 d . . . O13 O 0.0855(3) 0.52129(13) 0.78007(13) 0.0097(9) Uani 1 1 d U . . H13C H 0.1602 0.5279 0.7848 0.012 Uiso 1 1 calc R . . O14W O -0.0639(4) 0.3715(2) 0.97292(17) 0.0462(15) Uani 1 1 d . . . O14 O -0.0782(3) 0.54293(14) 0.72376(14) 0.0126(9) Uani 1 1 d . . . H14C H -0.1029 0.5630 0.6942 0.015 Uiso 1 1 calc R . . O15W O 0.4958(4) 0.61540(19) 0.58983(19) 0.0505(15) Uani 1 1 d . . . O15 O -0.0528(3) 0.44872(14) 0.76172(13) 0.0103(9) Uani 1 1 d . . . H15A H -0.0633 0.4119 0.7557 0.012 Uiso 1 1 calc R . . O16W O 0.2554(3) 0.36135(16) 0.90653(16) 0.0217(11) Uani 1 1 d . . . O16 O -0.0978(3) 0.52592(13) 0.82307(14) 0.0096(9) Uani 1 1 d . . . H16A H -0.1361 0.5361 0.8540 0.012 Uiso 1 1 calc R . . O17W O -0.1454(4) 0.5689(2) 0.5531(2) 0.0511(16) Uani 1 1 d . . . O17 O -0.0556(3) 0.49905(17) 0.93376(15) 0.0278(11) Uani 1 1 d . . . O18W O 0.4801(5) 0.2082(2) 0.9646(2) 0.0739(19) Uani 1 1 d . . . O18 O -0.2268(3) 0.51300(17) 0.91296(15) 0.0249(11) Uani 1 1 d . . . O19 O -0.1872(4) 0.4620(2) 0.98191(19) 0.0421(14) Uani 1 1 d . . . O20 O -0.1577(4) 0.5493(2) 0.98489(19) 0.0461(15) Uani 1 1 d . . . O21 O -0.3344(5) 0.6777(3) 0.6277(2) 0.072(2) Uani 1 1 d . . . O22 O -0.2309(4) 0.7160(2) 0.6882(2) 0.068(2) Uani 1 1 d . . . O23 O -0.3516(5) 0.6566(2) 0.7117(2) 0.0661(19) Uani 1 1 d . . . O24 O -0.4014(4) 0.7366(2) 0.6855(2) 0.070(2) Uani 1 1 d . . . O25 O -0.1312(9) 0.7552(4) 0.9289(5) 0.283(10) Uani 1 1 d . . . O26 O -0.0377(8) 0.7941(3) 0.8734(4) 0.186(6) Uani 1 1 d . . . O27 O 0.0153(7) 0.7852(2) 0.9543(2) 0.097(3) Uani 1 1 d . . . O28 O -0.0002(7) 0.7174(3) 0.9021(2) 0.112(3) Uani 1 1 d . . . O29 O 0.5738(3) 0.5411(2) 1.03911(18) 0.0398(14) Uani 1 1 d . . . O30 O 0.4873(4) 0.58207(16) 0.97403(16) 0.0356(13) Uani 1 1 d . . . O31 O 0.5252(4) 0.49636(18) 0.96754(16) 0.0453(13) Uani 1 1 d . . . O32 O 0.4010(3) 0.52446(18) 1.02452(17) 0.0344(13) Uani 1 1 d . . . O33 O 0.0067(4) 0.25973(18) 0.76562(18) 0.0553(17) Uani 1 1 d . . . O34 O -0.1047(3) 0.27342(16) 0.83325(19) 0.0343(12) Uani 1 1 d . . . O35 O 0.0456(4) 0.3191(2) 0.8267(2) 0.0654(19) Uani 1 1 d . . . O36 O -0.0853(4) 0.33417(18) 0.7705(2) 0.0550(17) Uani 1 1 d . . . O37 O 0.3417(4) 0.4863(2) 0.6120(2) 0.0565(17) Uani 1 1 d . . . O38 O 0.4962(4) 0.4844(2) 0.57194(16) 0.0485(15) Uani 1 1 d . . . O39 O 0.4888(4) 0.5013(2) 0.65783(16) 0.0552(15) Uani 1 1 d . . . O40 O 0.4516(5) 0.4212(2) 0.6292(2) 0.072(2) Uani 1 1 d . . . O41 O 0.3717(5) 0.45649(19) 0.8714(2) 0.0577(18) Uani 1 1 d . . . O42 O 0.3773(3) 0.54389(18) 0.87431(17) 0.0332(13) Uani 1 1 d . . . O43 O 0.3239(3) 0.50303(18) 0.80055(17) 0.0345(12) Uani 1 1 d . . . O44 O 0.4948(3) 0.5014(2) 0.82705(17) 0.0530(15) Uani 1 1 d . . . O45 O 0.2091(5) 0.3233(2) 1.0296(2) 0.0679(19) Uani 1 1 d . . . O46 O 0.1862(4) 0.23606(18) 1.02469(19) 0.0484(16) Uani 1 1 d . . . O47 O 0.3019(5) 0.2756(2) 0.9707(2) 0.0571(18) Uani 1 1 d . . . O48 O 0.3374(5) 0.2681(2) 1.0570(2) 0.073(2) Uani 1 1 d . . . N1 N -0.1114(4) 0.3681(2) 0.5930(2) 0.0275(15) Uani 1 1 d . . . H1A H -0.0575 0.3569 0.6116 0.041 Uiso 1 1 calc R . . H1B H -0.0916 0.3951 0.5741 0.041 Uiso 1 1 calc R . . H1C H -0.1334 0.3430 0.5723 0.041 Uiso 1 1 calc R . . N2 N 0.2569(4) 0.33315(18) 0.80436(18) 0.0196(13) Uani 1 1 d . . . H2A H 0.2803 0.3520 0.8306 0.029 Uiso 1 1 calc R . . H2B H 0.2985 0.3060 0.7999 0.029 Uiso 1 1 calc R . . H2C H 0.1922 0.3224 0.8112 0.029 Uiso 1 1 calc R . . N3 N -0.2140(4) 0.34019(18) 0.90310(19) 0.0193(13) Uani 1 1 d . . . H3C H -0.1661 0.3250 0.8834 0.029 Uiso 1 1 calc R . . H3D H -0.2542 0.3163 0.9177 0.029 Uiso 1 1 calc R . . H3E H -0.1823 0.3586 0.9274 0.029 Uiso 1 1 calc R . . N4 N -0.3845(4) 0.57885(17) 0.88294(18) 0.0150(12) Uani 1 1 d . . . H4C H -0.4216 0.5643 0.8578 0.023 Uiso 1 1 calc R . . H4D H -0.4275 0.5901 0.9074 0.023 Uiso 1 1 calc R . . H4E H -0.3406 0.5558 0.8962 0.023 Uiso 1 1 calc R . . N5 N 0.2395(4) 0.55756(18) 0.95492(18) 0.0193(13) Uani 1 1 d . . . H5C H 0.2734 0.5716 0.9813 0.029 Uiso 1 1 calc R . . H5D H 0.2852 0.5480 0.9309 0.029 Uiso 1 1 calc R . . H5E H 0.2040 0.5301 0.9658 0.029 Uiso 1 1 calc R . . N6 N 0.3062(4) 0.59562(19) 0.63597(18) 0.0215(13) Uani 1 1 d . . . H6C H 0.3083 0.5614 0.6384 0.032 Uiso 1 1 calc R . . H6D H 0.3681 0.6073 0.6255 0.032 Uiso 1 1 calc R . . H6E H 0.2573 0.6048 0.6134 0.032 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 Yb1 0.01022(13) 0.01006(13) 0.00955(13) 0.00118(11) -0.00080(11) 0.00055(11) Yb2 0.00979(12) 0.01023(14) 0.00960(13) -0.00071(12) -0.00030(10) 0.00020(11) Yb3 0.01041(13) 0.01053(13) 0.00867(13) -0.00027(11) 0.00021(10) -0.00002(10) Yb4 0.01003(13) 0.00875(13) 0.01072(13) -0.00001(11) 0.00027(11) -0.00004(11) Cl1 0.0203(8) 0.0246(10) 0.0163(8) 0.0005(8) -0.0008(6) 0.0023(8) Cl2 0.0377(11) 0.0249(11) 0.0377(12) -0.0052(9) -0.0078(9) 0.0101(9) Cl3 0.0332(12) 0.0303(11) 0.0811(17) -0.0204(11) 0.0123(12) -0.0090(10) Cl4 0.0206(9) 0.0253(9) 0.0176(8) 0.0002(7) -0.0007(7) -0.0030(7) Cl5 0.0258(10) 0.0188(8) 0.0318(10) -0.0048(7) 0.0050(8) -0.0034(7) Cl6 0.0267(9) 0.0332(11) 0.0256(10) 0.0008(8) 0.0037(7) 0.0103(8) Cl7 0.0180(8) 0.0221(9) 0.0224(9) -0.0027(8) 0.0026(6) -0.0029(7) Cl8 0.0469(13) 0.0292(11) 0.0364(12) 0.0070(9) -0.0013(9) -0.0104(9) C1 0.025(4) 0.017(4) 0.010(3) 0.000(3) -0.003(3) 0.001(3) C2 0.015(3) 0.006(3) 0.017(4) -0.004(3) 0.004(3) -0.008(3) C3 0.019(3) 0.018(4) 0.016(4) -0.002(3) -0.004(3) -0.001(3) C4 0.025(4) 0.035(5) 0.022(4) -0.009(3) -0.004(3) -0.012(3) C5 0.041(5) 0.029(5) 0.059(6) -0.012(4) -0.006(4) -0.015(4) C6 0.051(6) 0.013(4) 0.061(6) 0.001(4) -0.006(5) -0.010(4) C7 0.038(5) 0.019(4) 0.024(4) 0.006(3) 0.003(3) -0.003(3) C8 0.007(3) 0.017(4) 0.018(4) -0.004(3) 0.002(3) 0.001(3) C9 0.014(3) 0.008(3) 0.013(3) 0.004(3) 0.002(3) 0.005(2) C10 0.015(3) 0.029(4) 0.020(4) -0.006(3) 0.001(3) 0.001(3) C11 0.017(4) 0.023(4) 0.043(5) 0.000(3) 0.013(3) 0.006(3) C12 0.027(4) 0.024(4) 0.037(5) -0.003(3) 0.013(3) 0.010(3) C13 0.039(4) 0.013(3) 0.020(4) -0.006(3) 0.006(3) 0.008(3) C14 0.026(4) 0.020(4) 0.021(4) 0.001(3) -0.003(3) 0.002(3) C15 0.016(3) 0.008(3) 0.021(4) -0.001(3) 0.008(3) 0.000(3) C16 0.013(3) 0.016(3) 0.014(3) 0.002(3) 0.002(3) 0.004(3) C17 0.014(3) 0.017(4) 0.028(4) -0.001(3) -0.003(3) 0.000(3) C18 0.021(4) 0.028(4) 0.033(5) -0.003(3) -0.009(3) -0.009(3) C19 0.017(4) 0.023(4) 0.053(5) 0.009(3) 0.005(4) -0.007(3) C20 0.010(3) 0.032(4) 0.038(5) 0.014(3) 0.014(3) 0.007(3) C21 0.018(4) 0.016(4) 0.032(4) -0.004(3) 0.003(3) 0.001(3) C22 0.0107(15) 0.0107(16) 0.0113(16) 0.0002(10) -0.0009(10) 0.0010(10) C23 0.013(3) 0.014(3) 0.006(3) 0.000(3) 0.005(2) 0.002(3) C24 0.019(4) 0.015(4) 0.009(3) -0.004(3) -0.003(3) -0.002(3) C25 0.024(4) 0.020(4) 0.010(4) 0.000(3) -0.005(3) -0.003(3) C26 0.023(4) 0.017(4) 0.025(4) -0.007(3) 0.012(3) 0.001(3) C27 0.020(4) 0.019(4) 0.020(4) 0.001(3) 0.002(3) 0.007(3) C28 0.013(3) 0.014(3) 0.018(4) 0.000(3) 0.006(3) -0.001(3) C29 0.013(3) 0.013(4) 0.011(3) -0.001(3) 0.007(3) -0.001(3) C30 0.011(3) 0.021(4) 0.015(4) -0.002(3) -0.005(3) 0.002(3) C31 0.017(4) 0.030(4) 0.016(4) -0.013(3) 0.001(3) 0.005(3) C32 0.021(4) 0.054(5) 0.030(5) -0.018(4) 0.005(3) 0.007(4) C33 0.036(5) 0.031(5) 0.047(5) -0.031(4) -0.013(4) 0.001(4) C34 0.017(4) 0.019(4) 0.041(5) -0.010(3) -0.006(3) -0.003(3) C35 0.015(4) 0.017(4) 0.034(4) 0.001(3) 0.002(3) 0.000(3) C36 0.019(3) 0.013(3) 0.008(3) 0.006(3) -0.001(3) 0.004(3) C37 0.017(3) 0.014(3) 0.016(4) -0.006(3) 0.005(3) -0.001(3) C38 0.022(4) 0.019(4) 0.024(4) -0.001(3) 0.003(3) -0.009(3) C39 0.028(4) 0.011(4) 0.049(5) -0.001(3) 0.012(4) -0.003(3) C40 0.034(4) 0.029(4) 0.024(4) -0.002(3) -0.007(3) -0.007(3) C41 0.028(4) 0.037(5) 0.023(4) 0.002(3) -0.011(3) 0.007(4) C42 0.012(3) 0.015(4) 0.029(4) 0.007(3) 0.006(3) -0.004(3) O1 0.022(3) 0.033(3) 0.016(3) -0.014(2) -0.004(2) 0.002(2) O1W 0.017(2) 0.018(3) 0.011(2) 0.0048(19) 0.0000(18) 0.0012(19) O2 0.019(2) 0.024(3) 0.022(3) -0.004(2) 0.004(2) -0.007(2) O2W 0.019(2) 0.021(2) 0.017(2) 0.001(2) -0.007(2) 0.005(2) O3 0.029(3) 0.016(3) 0.013(3) 0.0075(19) 0.0028(19) 0.008(2) O3W 0.013(2) 0.037(3) 0.018(3) -0.006(2) -0.0013(18) -0.003(2) O4 0.018(2) 0.019(3) 0.016(3) 0.000(2) -0.0022(19) 0.0109(19) O4W 0.025(3) 0.025(2) 0.008(2) 0.0030(18) -0.0054(19) 0.001(2) O5 0.012(2) 0.014(2) 0.017(2) -0.0016(19) -0.0021(18) -0.0023(19) O5W 0.022(3) 0.027(3) 0.015(3) -0.002(2) -0.0010(19) 0.000(2) O6 0.017(2) 0.015(2) 0.013(2) 0.0029(19) -0.0017(18) -0.0018(19) O6W 0.026(3) 0.018(2) 0.017(3) 0.006(2) -0.003(2) 0.000(2) O7 0.017(2) 0.012(2) 0.025(3) 0.0054(19) 0.0055(19) 0.0015(18) O7W 0.029(3) 0.011(2) 0.025(3) 0.0022(18) -0.001(2) 0.002(2) O8W 0.035(3) 0.022(3) 0.029(3) 0.000(2) 0.004(2) -0.002(2) O8 0.017(2) 0.019(2) 0.016(2) -0.006(2) 0.003(2) 0.0020(19) O9 0.016(2) 0.019(3) 0.011(2) -0.0025(18) -0.0048(18) 0.0029(19) O9W 0.033(3) 0.027(3) 0.025(3) -0.001(2) 0.002(2) 0.001(2) O10 0.024(2) 0.014(2) 0.013(2) -0.0002(19) -0.0038(19) 0.002(2) O10W 0.028(3) 0.030(3) 0.026(3) 0.009(2) 0.004(2) -0.002(2) O11 0.017(2) 0.016(3) 0.016(3) -0.0061(19) -0.0036(18) -0.0044(19) O11W 0.035(3) 0.027(3) 0.026(3) -0.002(2) 0.011(2) -0.004(2) O12W 0.070(4) 0.057(4) 0.026(3) -0.004(3) -0.002(3) -0.001(3) O12 0.016(2) 0.015(2) 0.019(3) 0.0044(19) 0.0031(19) -0.0053(19) O13W 0.062(4) 0.048(4) 0.033(3) 0.000(3) -0.002(3) 0.024(3) O13 0.0091(12) 0.0101(12) 0.0100(12) 0.0006(9) 0.0010(9) -0.0022(9) O14W 0.057(4) 0.057(4) 0.025(3) 0.006(3) -0.002(3) -0.026(3) O14 0.014(2) 0.012(2) 0.011(2) 0.0058(18) -0.0013(17) 0.0009(18) O15W 0.035(3) 0.058(4) 0.058(4) 0.012(3) 0.000(3) -0.011(3) O15 0.008(2) 0.015(2) 0.007(2) 0.0020(17) 0.0015(16) 0.0001(17) O16W 0.023(3) 0.024(3) 0.017(3) -0.003(2) -0.004(2) 0.007(2) O16 0.008(2) 0.009(2) 0.011(2) 0.0010(17) 0.0014(16) 0.0024(17) O17W 0.042(4) 0.069(4) 0.042(4) -0.006(3) -0.012(3) 0.010(3) O17 0.011(2) 0.035(3) 0.037(3) 0.001(2) 0.0018(19) -0.003(2) O18W 0.073(5) 0.070(4) 0.079(5) 0.011(4) -0.008(4) 0.004(4) O18 0.024(3) 0.036(3) 0.015(2) -0.002(2) -0.0027(19) 0.006(2) O19 0.039(3) 0.051(4) 0.036(3) 0.026(3) 0.003(2) -0.007(3) O20 0.051(4) 0.058(4) 0.030(3) -0.025(3) -0.002(3) 0.004(3) O21 0.086(5) 0.103(5) 0.027(4) -0.019(4) 0.001(3) -0.028(4) O22 0.038(4) 0.060(4) 0.107(6) -0.026(4) -0.016(3) 0.010(3) O23 0.110(6) 0.037(4) 0.051(4) 0.014(3) 0.020(4) 0.021(3) O24 0.045(4) 0.051(4) 0.113(6) 0.005(4) -0.012(3) 0.030(3) O25 0.206(12) 0.216(12) 0.427(19) -0.245(13) 0.254(13) -0.167(10) O26 0.226(13) 0.109(7) 0.221(11) 0.065(8) -0.182(10) -0.060(8) O27 0.183(8) 0.055(4) 0.052(4) 0.012(3) -0.030(5) -0.065(5) O28 0.154(8) 0.120(6) 0.063(5) -0.037(4) -0.020(5) 0.082(6) O29 0.021(3) 0.062(4) 0.036(3) -0.008(3) -0.020(2) -0.011(3) O30 0.045(3) 0.026(3) 0.036(3) 0.011(2) 0.013(3) 0.003(2) O31 0.058(4) 0.041(3) 0.037(3) -0.012(3) 0.006(3) 0.013(3) O32 0.020(3) 0.055(4) 0.029(3) 0.009(3) 0.003(2) -0.010(2) O33 0.072(4) 0.038(3) 0.055(4) -0.026(3) 0.037(3) -0.009(3) O34 0.029(3) 0.023(3) 0.050(4) 0.009(3) 0.014(3) 0.002(2) O35 0.037(4) 0.093(5) 0.066(4) -0.037(4) 0.005(3) -0.022(3) O36 0.078(4) 0.029(3) 0.059(4) 0.019(3) 0.014(3) 0.018(3) O37 0.020(3) 0.056(4) 0.093(5) -0.012(4) -0.005(3) 0.009(3) O38 0.044(3) 0.080(4) 0.022(3) -0.001(3) 0.003(2) -0.010(3) O39 0.064(4) 0.075(4) 0.027(3) -0.010(3) -0.007(3) 0.009(4) O40 0.086(5) 0.034(4) 0.097(5) 0.013(3) 0.011(4) 0.011(4) O41 0.091(5) 0.028(3) 0.054(4) 0.023(3) -0.024(3) -0.021(3) O42 0.032(3) 0.036(3) 0.031(3) -0.021(2) 0.008(2) 0.006(2) O43 0.034(3) 0.031(3) 0.038(3) 0.002(3) -0.017(2) -0.006(2) O44 0.018(3) 0.091(4) 0.050(3) -0.034(3) 0.013(2) -0.010(3) O45 0.085(5) 0.032(4) 0.087(5) -0.011(3) 0.002(4) 0.004(4) O46 0.069(4) 0.030(3) 0.046(4) 0.011(3) -0.007(3) -0.027(3) O47 0.053(4) 0.063(4) 0.055(4) 0.022(3) 0.018(3) 0.016(3) O48 0.085(5) 0.065(4) 0.068(5) 0.016(4) -0.050(4) -0.010(4) N1 0.021(3) 0.025(3) 0.036(4) -0.018(3) 0.001(3) 0.000(3) N2 0.020(3) 0.016(3) 0.023(3) -0.002(2) 0.000(2) 0.006(2) N3 0.021(3) 0.013(3) 0.024(3) 0.009(2) 0.008(3) 0.000(2) N4 0.014(3) 0.011(3) 0.021(3) 0.000(2) 0.001(2) 0.000(2) N5 0.020(3) 0.020(3) 0.018(3) -0.004(2) -0.006(2) 0.002(2) N6 0.017(3) 0.019(3) 0.028(3) 0.002(3) 0.004(2) -0.004(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 Yb1 O16 2.243(4) . ? Yb1 O4 2.287(4) . ? Yb1 O13 2.289(4) . ? Yb1 O15 2.307(4) . ? Yb1 O5 2.322(4) . ? Yb1 O9 2.328(4) . ? Yb1 O1W 2.365(4) . ? Yb1 O17 2.846(4) . ? Yb1 Yb4 3.7206(3) . ? Yb1 Yb3 3.7491(3) . ? Yb1 Yb2 3.7752(3) . ? Yb2 O6 2.215(4) . ? Yb2 O14 2.265(4) . ? Yb2 O1 2.271(4) . ? Yb2 O8 2.301(4) . ? Yb2 O16 2.382(4) . ? Yb2 O15 2.411(3) . ? Yb2 O3W 2.414(4) . ? Yb2 O2W 2.421(4) . ? Yb2 Yb3 3.6813(3) . ? Yb2 Yb4 3.6927(4) . ? Yb3 O3 2.227(4) . ? Yb3 O14 2.277(4) . ? Yb3 O11 2.279(4) . ? Yb3 O2 2.306(4) . ? Yb3 O15 2.350(4) . ? Yb3 O13 2.357(4) . ? Yb3 O5W 2.394(4) . ? Yb3 O4W 2.410(4) . ? Yb3 Yb4 3.6967(3) . ? Yb4 O10 2.259(4) . ? Yb4 O14 2.282(4) . ? Yb4 O7 2.323(4) . ? Yb4 O12 2.325(4) . ? Yb4 O13 2.347(3) . ? Yb4 O7W 2.363(4) . ? Yb4 O16 2.369(4) . ? Yb4 O6W 2.394(4) . ? Cl1 O20 1.412(5) . ? Cl1 O19 1.432(5) . ? Cl1 O18 1.440(4) . ? Cl1 O17 1.440(4) . ? Cl2 O23 1.406(5) . ? Cl2 O24 1.417(5) . ? Cl2 O21 1.430(5) . ? Cl2 O22 1.437(6) . ? Cl3 O25 1.237(9) . ? Cl3 O28 1.357(6) . ? Cl3 O27 1.367(6) . ? Cl3 O26 1.446(9) . ? Cl4 O29 1.422(4) . ? Cl4 O31 1.423(5) . ? Cl4 O30 1.426(4) . ? Cl4 O32 1.442(4) . ? Cl5 O33 1.408(5) . ? Cl5 O36 1.419(5) . ? Cl5 O35 1.420(5) . ? Cl5 O34 1.438(5) . ? Cl6 O40 1.396(5) . ? Cl6 O37 1.397(5) . ? Cl6 O39 1.430(5) . ? Cl6 O38 1.435(5) . ? Cl7 O41 1.411(5) . ? Cl7 O42 1.418(4) . ? Cl7 O43 1.429(4) . ? Cl7 O44 1.435(4) . ? Cl8 O45 1.413(6) . ? Cl8 O48 1.429(5) . ? Cl8 O47 1.437(6) . ? Cl8 O46 1.448(5) . ? C1 O1 1.251(7) . ? C1 O2 1.257(7) . ? C1 C2 1.515(8) . ? C2 N1 1.512(7) . ? C2 C3 1.525(8) . ? C2 C7 1.528(8) . ? C3 C4 1.516(8) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.497(9) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.515(10) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.502(9) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 O3 1.244(7) . ? C8 O4 1.264(6) . ? C8 C9 1.525(7) . ? C9 N2 1.508(7) . ? C9 C10 1.523(8) . ? C9 C14 1.536(8) . ? C10 C11 1.525(8) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.503(9) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.506(9) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.517(8) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 O6 1.255(7) . ? C15 O5 1.259(7) . ? C15 C16 1.546(8) . ? C16 N3 1.483(7) . ? C16 C21 1.527(8) . ? C16 C17 1.529(8) . ? C17 C18 1.542(8) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.502(9) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.518(9) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.526(8) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 O7 1.246(6) . ? C22 O8 1.259(7) . ? C22 C23 1.534(8) . ? C23 N4 1.518(7) . ? C23 C28 1.536(8) . ? C23 C24 1.547(8) . ? C24 C25 1.536(8) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.501(8) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.568(8) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.502(8) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 O10 1.236(7) . ? C29 O9 1.262(7) . ? C29 C30 1.538(8) . ? C30 N5 1.504(7) . ? C30 C31 1.511(8) . ? C30 C35 1.523(8) . ? C31 C32 1.524(8) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.484(10) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.520(9) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.533(8) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 O11 1.242(7) . ? C36 O12 1.261(7) . ? C36 C37 1.541(8) . ? C37 N6 1.493(7) . ? C37 C38 1.528(8) . ? C37 C42 1.531(8) . ? C38 C39 1.547(8) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.498(9) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.517(9) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.489(8) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? O13 H13C 1.0000 . ? O14 H14C 1.0000 . ? O15 H15A 1.0000 . ? O16 H16A 1.0000 . ? N1 H1A 0.9100 . ? N1 H1B 0.9100 . ? N1 H1C 0.9100 . ? N2 H2A 0.9100 . ? N2 H2B 0.9100 . ? N2 H2C 0.9100 . ? N3 H3C 0.9100 . ? N3 H3D 0.9100 . ? N3 H3E 0.9100 . ? N4 H4C 0.9100 . ? N4 H4D 0.9100 . ? N4 H4E 0.9100 . ? N5 H5C 0.9100 . ? N5 H5D 0.9100 . ? N5 H5E 0.9100 . ? N6 H6C 0.9100 . ? N6 H6D 0.9100 . ? N6 H6E 0.9100 . ? 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 O16 Yb1 O4 148.50(14) . . ? O16 Yb1 O13 71.76(13) . . ? O4 Yb1 O13 82.13(14) . . ? O16 Yb1 O15 72.19(13) . . ? O4 Yb1 O15 83.17(13) . . ? O13 Yb1 O15 71.48(13) . . ? O16 Yb1 O5 86.13(13) . . ? O4 Yb1 O5 108.28(14) . . ? O13 Yb1 O5 146.89(14) . . ? O15 Yb1 O5 78.53(13) . . ? O16 Yb1 O9 92.46(13) . . ? O4 Yb1 O9 97.96(14) . . ? O13 Yb1 O9 75.69(13) . . ? O15 Yb1 O9 146.69(13) . . ? O5 Yb1 O9 131.02(13) . . ? O16 Yb1 O1W 138.77(13) . . ? O4 Yb1 O1W 72.69(14) . . ? O13 Yb1 O1W 139.72(13) . . ? O15 Yb1 O1W 133.41(13) . . ? O5 Yb1 O1W 72.44(14) . . ? O9 Yb1 O1W 77.25(13) . . ? O16 Yb1 O17 73.24(13) . . ? O4 Yb1 O17 137.55(13) . . ? O13 Yb1 O17 122.84(13) . . ? O15 Yb1 O17 134.62(12) . . ? O5 Yb1 O17 70.65(13) . . ? O9 Yb1 O17 62.24(13) . . ? O1W Yb1 O17 66.60(13) . . ? O16 Yb1 Yb4 37.39(9) . . ? O4 Yb1 Yb4 119.28(10) . . ? O13 Yb1 Yb4 37.15(9) . . ? O15 Yb1 Yb4 78.21(9) . . ? O5 Yb1 Yb4 123.22(10) . . ? O9 Yb1 Yb4 72.25(9) . . ? O1W Yb1 Yb4 148.38(10) . . ? O17 Yb1 Yb4 91.50(9) . . ? O16 Yb1 Yb3 76.98(9) . . ? O4 Yb1 Yb3 71.55(10) . . ? O13 Yb1 Yb3 36.82(9) . . ? O15 Yb1 Yb3 36.77(9) . . ? O5 Yb1 Yb3 115.29(10) . . ? O9 Yb1 Yb3 111.96(10) . . ? O1W Yb1 Yb3 143.97(10) . . ? O17 Yb1 Yb3 149.19(9) . . ? Yb4 Yb1 Yb3 59.324(6) . . ? O16 Yb1 Yb2 36.52(9) . . ? O4 Yb1 Yb2 120.89(10) . . ? O13 Yb1 Yb2 76.59(9) . . ? O15 Yb1 Yb2 37.82(9) . . ? O5 Yb1 Yb2 71.11(10) . . ? O9 Yb1 Yb2 127.71(9) . . ? O1W Yb1 Yb2 143.51(9) . . ? O17 Yb1 Yb2 99.43(8) . . ? Yb4 Yb1 Yb2 59.023(7) . . ? Yb3 Yb1 Yb2 58.582(6) . . ? O6 Yb2 O14 144.67(14) . . ? O6 Yb2 O1 99.92(15) . . ? O14 Yb2 O1 92.02(15) . . ? O6 Yb2 O8 91.47(14) . . ? O14 Yb2 O8 98.68(14) . . ? O1 Yb2 O8 143.08(14) . . ? O6 Yb2 O16 80.67(13) . . ? O14 Yb2 O16 70.60(13) . . ? O1 Yb2 O16 144.02(14) . . ? O8 Yb2 O16 72.29(13) . . ? O6 Yb2 O15 79.70(13) . . ? O14 Yb2 O15 70.87(13) . . ? O1 Yb2 O15 76.65(14) . . ? O8 Yb2 O15 140.21(13) . . ? O16 Yb2 O15 68.02(12) . . ? O6 Yb2 O3W 71.10(14) . . ? O14 Yb2 O3W 144.02(14) . . ? O1 Yb2 O3W 71.93(14) . . ? O8 Yb2 O3W 79.00(14) . . ? O16 Yb2 O3W 138.84(13) . . ? O15 Yb2 O3W 131.88(13) . . ? O6 Yb2 O2W 143.05(14) . . ? O14 Yb2 O2W 72.01(14) . . ? O1 Yb2 O2W 76.88(14) . . ? O8 Yb2 O2W 73.16(14) . . ? O16 Yb2 O2W 123.38(13) . . ? O15 Yb2 O2W 132.99(13) . . ? O3W Yb2 O2W 73.03(14) . . ? O6 Yb2 Yb3 118.44(10) . . ? O14 Yb2 Yb3 35.98(9) . . ? O1 Yb2 Yb3 71.12(11) . . ? O8 Yb2 Yb3 132.48(10) . . ? O16 Yb2 Yb3 77.06(9) . . ? O15 Yb2 Yb3 38.75(8) . . ? O3W Yb2 Yb3 142.93(9) . . ? O2W Yb2 Yb3 95.68(10) . . ? O6 Yb2 Yb4 119.54(10) . . ? O14 Yb2 Yb4 35.85(10) . . ? O1 Yb2 Yb4 127.30(11) . . ? O8 Yb2 Yb4 73.26(10) . . ? O16 Yb2 Yb4 38.87(9) . . ? O15 Yb2 Yb4 77.70(9) . . ? O3W Yb2 Yb4 150.24(10) . . ? O2W Yb2 Yb4 88.59(10) . . ? Yb3 Yb2 Yb4 60.173(7) . . ? O6 Yb2 Yb1 69.32(10) . . ? O14 Yb2 Yb1 75.37(10) . . ? O1 Yb2 Yb1 112.21(11) . . ? O8 Yb2 Yb1 104.69(10) . . ? O16 Yb2 Yb1 34.08(9) . . ? O15 Yb2 Yb1 35.92(9) . . ? O3W Yb2 Yb1 140.31(10) . . ? O2W Yb2 Yb1 146.45(10) . . ? Yb3 Yb2 Yb1 60.355(7) . . ? Yb4 Yb2 Yb1 59.751(6) . . ? O3 Yb3 O14 144.50(14) . . ? O3 Yb3 O11 90.28(15) . . ? O14 Yb3 O11 95.76(14) . . ? O3 Yb3 O2 102.25(15) . . ? O14 Yb3 O2 94.88(14) . . ? O11 Yb3 O2 140.87(14) . . ? O3 Yb3 O15 83.03(13) . . ? O14 Yb3 O15 71.81(13) . . ? O11 Yb3 O15 144.35(13) . . ? O2 Yb3 O15 74.55(14) . . ? O3 Yb3 O13 77.61(14) . . ? O14 Yb3 O13 70.41(13) . . ? O11 Yb3 O13 74.81(13) . . ? O2 Yb3 O13 143.87(14) . . ? O15 Yb3 O13 69.55(13) . . ? O3 Yb3 O5W 70.09(14) . . ? O14 Yb3 O5W 145.35(14) . . ? O11 Yb3 O5W 77.97(14) . . ? O2 Yb3 O5W 72.06(14) . . ? O15 Yb3 O5W 130.74(14) . . ? O13 Yb3 O5W 137.20(13) . . ? O3 Yb3 O4W 141.42(14) . . ? O14 Yb3 O4W 72.98(13) . . ? O11 Yb3 O4W 72.34(14) . . ? O2 Yb3 O4W 75.08(14) . . ? O15 Yb3 O4W 130.56(13) . . ? O13 Yb3 O4W 127.11(13) . . ? O5W Yb3 O4W 72.66(14) . . ? O3 Yb3 Yb2 122.83(10) . . ? O14 Yb3 Yb2 35.76(9) . . ? O11 Yb3 Yb2 130.58(10) . . ? O2 Yb3 Yb2 72.00(10) . . ? O15 Yb3 Yb2 39.97(9) . . ? O13 Yb3 Yb2 77.94(9) . . ? O5W Yb3 Yb2 143.73(10) . . ? O4W Yb3 Yb2 93.49(10) . . ? O3 Yb3 Yb4 115.60(11) . . ? O14 Yb3 Yb4 35.87(9) . . ? O11 Yb3 Yb4 73.22(10) . . ? O2 Yb3 Yb4 129.64(10) . . ? O15 Yb3 Yb4 78.28(9) . . ? O13 Yb3 Yb4 38.09(8) . . ? O5W Yb3 Yb4 150.52(10) . . ? O4W Yb3 Yb4 92.52(9) . . ? Yb2 Yb3 Yb4 60.066(7) . . ? O3 Yb3 Yb1 69.16(10) . . ? O14 Yb3 Yb1 75.84(10) . . ? O11 Yb3 Yb1 109.25(10) . . ? O2 Yb3 Yb1 109.86(11) . . ? O15 Yb3 Yb1 36.00(9) . . ? O13 Yb3 Yb1 35.59(9) . . ? O5W Yb3 Yb1 138.58(10) . . ? O4W Yb3 Yb1 148.75(9) . . ? Yb2 Yb3 Yb1 61.062(6) . . ? Yb4 Yb3 Yb1 59.953(6) . . ? O10 Yb4 O14 144.11(14) . . ? O10 Yb4 O7 95.69(14) . . ? O14 Yb4 O7 93.95(14) . . ? O10 Yb4 O12 102.77(14) . . ? O14 Yb4 O12 89.99(13) . . ? O7 Yb4 O12 142.34(14) . . ? O10 Yb4 O13 80.36(13) . . ? O14 Yb4 O13 70.53(13) . . ? O7 Yb4 O13 140.75(13) . . ? O12 Yb4 O13 75.37(13) . . ? O10 Yb4 O7W 70.77(14) . . ? O14 Yb4 O7W 145.12(13) . . ? O7 Yb4 O7W 79.06(14) . . ? O12 Yb4 O7W 76.57(14) . . ? O13 Yb4 O7W 133.58(14) . . ? O10 Yb4 O16 79.68(14) . . ? O14 Yb4 O16 70.55(13) . . ? O7 Yb4 O16 72.30(13) . . ? O12 Yb4 O16 142.95(13) . . ? O13 Yb4 O16 68.56(12) . . ? O7W Yb4 O16 136.14(13) . . ? O10 Yb4 O6W 144.11(14) . . ? O14 Yb4 O6W 71.72(13) . . ? O7 Yb4 O6W 73.98(14) . . ? O12 Yb4 O6W 71.82(14) . . ? O13 Yb4 O6W 129.14(13) . . ? O7W Yb4 O6W 73.51(14) . . ? O16 Yb4 O6W 126.50(13) . . ? O10 Yb4 Yb2 118.79(10) . . ? O14 Yb4 Yb2 35.55(9) . . ? O7 Yb4 Yb2 70.03(10) . . ? O12 Yb4 Yb2 125.01(10) . . ? O13 Yb4 Yb2 77.81(9) . . ? O7W Yb4 Yb2 148.17(11) . . ? O16 Yb4 Yb2 39.12(9) . . ? O6W Yb4 Yb2 90.44(10) . . ? O10 Yb4 Yb3 118.64(10) . . ? O14 Yb4 Yb3 35.78(9) . . ? O7 Yb4 Yb3 128.09(10) . . ? O12 Yb4 Yb3 69.57(10) . . ? O13 Yb4 Yb3 38.30(9) . . ? O7W Yb4 Yb3 146.06(10) . . ? O16 Yb4 Yb3 76.87(9) . . ? O6W Yb4 Yb3 93.30(10) . . ? Yb2 Yb4 Yb3 59.760(6) . . ? O10 Yb4 Yb1 67.68(10) . . ? O14 Yb4 Yb1 76.43(9) . . ? O7 Yb4 Yb1 106.28(10) . . ? O12 Yb4 Yb1 111.04(10) . . ? O13 Yb4 Yb1 36.09(9) . . ? O7W Yb4 Yb1 138.42(10) . . ? O16 Yb4 Yb1 35.09(9) . . ? O6W Yb4 Yb1 148.05(10) . . ? Yb2 Yb4 Yb1 61.226(7) . . ? Yb3 Yb4 Yb1 60.723(7) . . ? O20 Cl1 O19 111.3(3) . . ? O20 Cl1 O18 108.9(3) . . ? O19 Cl1 O18 108.7(3) . . ? O20 Cl1 O17 109.1(3) . . ? O19 Cl1 O17 110.4(3) . . ? O18 Cl1 O17 108.3(3) . . ? O23 Cl2 O24 110.9(4) . . ? O23 Cl2 O21 109.0(4) . . ? O24 Cl2 O21 111.8(4) . . ? O23 Cl2 O22 109.0(4) . . ? O24 Cl2 O22 107.1(4) . . ? O21 Cl2 O22 108.9(4) . . ? O25 Cl3 O28 108.6(6) . . ? O25 Cl3 O27 113.6(7) . . ? O28 Cl3 O27 113.5(5) . . ? O25 Cl3 O26 108.1(9) . . ? O28 Cl3 O26 105.1(6) . . ? O27 Cl3 O26 107.5(4) . . ? O29 Cl4 O31 109.9(3) . . ? O29 Cl4 O30 110.0(3) . . ? O31 Cl4 O30 109.9(3) . . ? O29 Cl4 O32 109.2(3) . . ? O31 Cl4 O32 109.6(3) . . ? O30 Cl4 O32 108.3(3) . . ? O33 Cl5 O36 109.9(3) . . ? O33 Cl5 O35 110.0(4) . . ? O36 Cl5 O35 108.6(4) . . ? O33 Cl5 O34 110.7(3) . . ? O36 Cl5 O34 109.4(3) . . ? O35 Cl5 O34 108.2(3) . . ? O40 Cl6 O37 110.3(4) . . ? O40 Cl6 O39 109.5(4) . . ? O37 Cl6 O39 109.7(3) . . ? O40 Cl6 O38 111.3(4) . . ? O37 Cl6 O38 107.5(3) . . ? O39 Cl6 O38 108.5(3) . . ? O41 Cl7 O42 110.1(3) . . ? O41 Cl7 O43 110.5(3) . . ? O42 Cl7 O43 110.8(3) . . ? O41 Cl7 O44 109.4(4) . . ? O42 Cl7 O44 106.2(3) . . ? O43 Cl7 O44 109.8(3) . . ? O45 Cl8 O48 110.9(4) . . ? O45 Cl8 O47 111.0(4) . . ? O48 Cl8 O47 110.0(4) . . ? O45 Cl8 O46 109.5(4) . . ? O48 Cl8 O46 107.3(4) . . ? O47 Cl8 O46 108.1(4) . . ? O1 C1 O2 126.7(6) . . ? O1 C1 C2 115.9(5) . . ? O2 C1 C2 117.3(5) . . ? N1 C2 C1 106.0(5) . . ? N1 C2 C3 106.9(5) . . ? C1 C2 C3 112.0(5) . . ? N1 C2 C7 109.5(5) . . ? C1 C2 C7 111.7(5) . . ? C3 C2 C7 110.6(5) . . ? C4 C3 C2 113.5(5) . . ? C4 C3 H3A 108.9 . . ? C2 C3 H3A 108.9 . . ? C4 C3 H3B 108.9 . . ? C2 C3 H3B 108.9 . . ? H3A C3 H3B 107.7 . . ? C5 C4 C3 111.5(6) . . ? C5 C4 H4A 109.3 . . ? C3 C4 H4A 109.3 . . ? C5 C4 H4B 109.3 . . ? C3 C4 H4B 109.3 . . ? H4A C4 H4B 108.0 . . ? C4 C5 C6 111.4(6) . . ? C4 C5 H5A 109.3 . . ? C6 C5 H5A 109.3 . . ? C4 C5 H5B 109.3 . . ? C6 C5 H5B 109.3 . . ? H5A C5 H5B 108.0 . . ? C7 C6 C5 110.9(6) . . ? C7 C6 H6A 109.5 . . ? C5 C6 H6A 109.5 . . ? C7 C6 H6B 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 108.1 . . ? C6 C7 C2 113.7(6) . . ? C6 C7 H7A 108.8 . . ? C2 C7 H7A 108.8 . . ? C6 C7 H7B 108.8 . . ? C2 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? O3 C8 O4 126.5(5) . . ? O3 C8 C9 115.4(5) . . ? O4 C8 C9 118.1(5) . . ? N2 C9 C10 108.9(5) . . ? N2 C9 C8 108.3(5) . . ? C10 C9 C8 111.3(5) . . ? N2 C9 C14 109.7(5) . . ? C10 C9 C14 109.7(5) . . ? C8 C9 C14 109.0(5) . . ? C9 C10 C11 114.0(5) . . ? C9 C10 H10A 108.8 . . ? C11 C10 H10A 108.8 . . ? C9 C10 H10B 108.8 . . ? C11 C10 H10B 108.8 . . ? H10A C10 H10B 107.7 . . ? C12 C11 C10 111.0(5) . . ? C12 C11 H11A 109.4 . . ? C10 C11 H11A 109.4 . . ? C12 C11 H11B 109.4 . . ? C10 C11 H11B 109.4 . . ? H11A C11 H11B 108.0 . . ? C11 C12 C13 112.2(5) . . ? C11 C12 H12A 109.2 . . ? C13 C12 H12A 109.2 . . ? C11 C12 H12B 109.2 . . ? C13 C12 H12B 109.2 . . ? H12A C12 H12B 107.9 . . ? C12 C13 C14 110.7(5) . . ? C12 C13 H13A 109.5 . . ? C14 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 108.1 . . ? C13 C14 C9 112.8(5) . . ? C13 C14 H14A 109.0 . . ? C9 C14 H14A 109.0 . . ? C13 C14 H14B 109.0 . . ? C9 C14 H14B 109.0 . . ? H14A C14 H14B 107.8 . . ? O6 C15 O5 127.4(5) . . ? O6 C15 C16 114.4(5) . . ? O5 C15 C16 118.2(5) . . ? N3 C16 C21 110.1(5) . . ? N3 C16 C17 109.2(5) . . ? C21 C16 C17 109.5(5) . . ? N3 C16 C15 107.7(5) . . ? C21 C16 C15 110.0(5) . . ? C17 C16 C15 110.3(5) . . ? C16 C17 C18 112.1(5) . . ? C16 C17 H17A 109.2 . . ? C18 C17 H17A 109.2 . . ? C16 C17 H17B 109.2 . . ? C18 C17 H17B 109.2 . . ? H17A C17 H17B 107.9 . . ? C19 C18 C17 110.1(5) . . ? C19 C18 H18A 109.6 . . ? C17 C18 H18A 109.6 . . ? C19 C18 H18B 109.6 . . ? C17 C18 H18B 109.6 . . ? H18A C18 H18B 108.1 . . ? C18 C19 C20 111.7(6) . . ? C18 C19 H19A 109.3 . . ? C20 C19 H19A 109.3 . . ? C18 C19 H19B 109.3 . . ? C20 C19 H19B 109.3 . . ? H19A C19 H19B 107.9 . . ? C19 C20 C21 111.4(5) . . ? C19 C20 H20A 109.4 . . ? C21 C20 H20A 109.3 . . ? C19 C20 H20B 109.4 . . ? C21 C20 H20B 109.4 . . ? H20A C20 H20B 108.0 . . ? C20 C21 C16 113.3(5) . . ? C20 C21 H21A 108.9 . . ? C16 C21 H21A 108.9 . . ? C20 C21 H21B 108.9 . . ? C16 C21 H21B 108.9 . . ? H21A C21 H21B 107.7 . . ? O7 C22 O8 126.9(6) . . ? O7 C22 C23 118.3(5) . . ? O8 C22 C23 114.7(5) . . ? N4 C23 C22 105.8(5) . . ? N4 C23 C28 107.9(5) . . ? C22 C23 C28 110.5(5) . . ? N4 C23 C24 110.0(5) . . ? C22 C23 C24 112.1(5) . . ? C28 C23 C24 110.3(5) . . ? C25 C24 C23 112.1(5) . . ? C25 C24 H24A 109.2 . . ? C23 C24 H24A 109.2 . . ? C25 C24 H24B 109.2 . . ? C23 C24 H24B 109.2 . . ? H24A C24 H24B 107.9 . . ? C26 C25 C24 112.4(5) . . ? C26 C25 H25A 109.1 . . ? C24 C25 H25A 109.1 . . ? C26 C25 H25B 109.1 . . ? C24 C25 H25B 109.1 . . ? H25A C25 H25B 107.8 . . ? C25 C26 C27 111.2(5) . . ? C25 C26 H26A 109.4 . . ? C27 C26 H26A 109.4 . . ? C25 C26 H26B 109.4 . . ? C27 C26 H26B 109.4 . . ? H26A C26 H26B 108.0 . . ? C28 C27 C26 110.9(5) . . ? C28 C27 H27A 109.5 . . ? C26 C27 H27A 109.5 . . ? C28 C27 H27B 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 108.1 . . ? C27 C28 C23 113.4(5) . . ? C27 C28 H28A 108.9 . . ? C23 C28 H28A 108.9 . . ? C27 C28 H28B 108.9 . . ? C23 C28 H28B 108.9 . . ? H28A C28 H28B 107.7 . . ? O10 C29 O9 126.5(6) . . ? O10 C29 C30 116.2(5) . . ? O9 C29 C30 117.2(5) . . ? N5 C30 C31 109.1(5) . . ? N5 C30 C35 108.9(5) . . ? C31 C30 C35 110.7(5) . . ? N5 C30 C29 106.9(5) . . ? C31 C30 C29 110.2(5) . . ? C35 C30 C29 111.0(5) . . ? C30 C31 C32 112.7(5) . . ? C30 C31 H31A 109.1 . . ? C32 C31 H31A 109.1 . . ? C30 C31 H31B 109.1 . . ? C32 C31 H31B 109.1 . . ? H31A C31 H31B 107.8 . . ? C33 C32 C31 112.1(6) . . ? C33 C32 H32A 109.2 . . ? C31 C32 H32A 109.2 . . ? C33 C32 H32B 109.2 . . ? C31 C32 H32B 109.2 . . ? H32A C32 H32B 107.9 . . ? C32 C33 C34 111.6(6) . . ? C32 C33 H33A 109.3 . . ? C34 C33 H33A 109.3 . . ? C32 C33 H33B 109.3 . . ? C34 C33 H33B 109.3 . . ? H33A C33 H33B 108.0 . . ? C33 C34 C35 110.9(6) . . ? C33 C34 H34A 109.5 . . ? C35 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? C35 C34 H34B 109.5 . . ? H34A C34 H34B 108.1 . . ? C30 C35 C34 112.5(5) . . ? C30 C35 H35A 109.1 . . ? C34 C35 H35A 109.1 . . ? C30 C35 H35B 109.1 . . ? C34 C35 H35B 109.1 . . ? H35A C35 H35B 107.8 . . ? O11 C36 O12 126.7(6) . . ? O11 C36 C37 115.0(5) . . ? O12 C36 C37 118.3(5) . . ? N6 C37 C38 108.4(5) . . ? N6 C37 C42 108.0(5) . . ? C38 C37 C42 111.0(5) . . ? N6 C37 C36 105.2(5) . . ? C38 C37 C36 115.9(5) . . ? C42 C37 C36 108.0(5) . . ? C37 C38 C39 112.4(5) . . ? C37 C38 H38A 109.1 . . ? C39 C38 H38A 109.1 . . ? C37 C38 H38B 109.1 . . ? C39 C38 H38B 109.1 . . ? H38A C38 H38B 107.9 . . ? C40 C39 C38 112.1(6) . . ? C40 C39 H39A 109.2 . . ? C38 C39 H39A 109.2 . . ? C40 C39 H39B 109.2 . . ? C38 C39 H39B 109.2 . . ? H39A C39 H39B 107.9 . . ? C39 C40 C41 110.8(6) . . ? C39 C40 H40A 109.5 . . ? C41 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? C41 C40 H40B 109.5 . . ? H40A C40 H40B 108.1 . . ? C42 C41 C40 111.4(6) . . ? C42 C41 H41A 109.4 . . ? C40 C41 H41A 109.4 . . ? C42 C41 H41B 109.4 . . ? C40 C41 H41B 109.4 . . ? H41A C41 H41B 108.0 . . ? C41 C42 C37 111.8(5) . . ? C41 C42 H42A 109.3 . . ? C37 C42 H42A 109.3 . . ? C41 C42 H42B 109.3 . . ? C37 C42 H42B 109.3 . . ? H42A C42 H42B 107.9 . . ? C1 O1 Yb2 135.8(4) . . ? C1 O2 Yb3 133.1(4) . . ? C8 O3 Yb3 138.2(4) . . ? C8 O4 Yb1 131.9(4) . . ? C15 O5 Yb1 131.6(4) . . ? C15 O6 Yb2 139.2(4) . . ? C22 O7 Yb4 133.7(4) . . ? C22 O8 Yb2 130.7(4) . . ? C29 O9 Yb1 128.0(4) . . ? C29 O10 Yb4 138.6(4) . . ? C36 O11 Yb3 133.2(4) . . ? C36 O12 Yb4 135.9(4) . . ? Yb1 O13 Yb4 106.76(14) . . ? Yb1 O13 Yb3 107.59(14) . . ? Yb4 O13 Yb3 103.61(14) . . ? Yb1 O13 H13C 112.8 . . ? Yb4 O13 H13C 112.8 . . ? Yb3 O13 H13C 112.8 . . ? Yb2 O14 Yb3 108.26(15) . . ? Yb2 O14 Yb4 108.59(15) . . ? Yb3 O14 Yb4 108.35(15) . . ? Yb2 O14 H14C 110.5 . . ? Yb3 O14 H14C 110.5 . . ? Yb4 O14 H14C 110.5 . . ? Yb1 O15 Yb3 107.24(14) . . ? Yb1 O15 Yb2 106.26(14) . . ? Yb3 O15 Yb2 101.28(13) . . ? Yb1 O15 H15A 113.7 . . ? Yb3 O15 H15A 113.7 . . ? Yb2 O15 H15A 113.7 . . ? Yb1 O16 Yb4 107.52(14) . . ? Yb1 O16 Yb2 109.39(15) . . ? Yb4 O16 Yb2 102.01(14) . . ? Yb1 O16 H16A 112.4 . . ? Yb4 O16 H16A 112.4 . . ? Yb2 O16 H16A 112.4 . . ? Cl1 O17 Yb1 133.9(2) . . ? C2 N1 H1A 109.5 . . ? C2 N1 H1B 109.5 . . ? H1A N1 H1B 109.5 . . ? C2 N1 H1C 109.5 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? C9 N2 H2A 109.5 . . ? C9 N2 H2B 109.5 . . ? H2A N2 H2B 109.5 . . ? C9 N2 H2C 109.5 . . ? H2A N2 H2C 109.5 . . ? H2B N2 H2C 109.5 . . ? C16 N3 H3C 109.5 . . ? C16 N3 H3D 109.5 . . ? H3C N3 H3D 109.5 . . ? C16 N3 H3E 109.5 . . ? H3C N3 H3E 109.5 . . ? H3D N3 H3E 109.5 . . ? C23 N4 H4C 109.5 . . ? C23 N4 H4D 109.5 . . ? H4C N4 H4D 109.5 . . ? C23 N4 H4E 109.5 . . ? H4C N4 H4E 109.5 . . ? H4D N4 H4E 109.5 . . ? C30 N5 H5C 109.5 . . ? C30 N5 H5D 109.5 . . ? H5C N5 H5D 109.5 . . ? C30 N5 H5E 109.5 . . ? H5C N5 H5E 109.5 . . ? H5D N5 H5E 109.5 . . ? C37 N6 H6C 109.5 . . ? C37 N6 H6D 109.5 . . ? H6C N6 H6D 109.5 . . ? C37 N6 H6E 109.5 . . ? H6C N6 H6E 109.5 . . ? H6D N6 H6E 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.006 _refine_diff_density_min -0.912 _refine_diff_density_rms 0.127