# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1 _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C122 H103 Dy5 N4 O25, 3(C H2 Cl2)' _chemical_formula_sum 'C125 H109 Cl6 Dy5 N4 O25' _chemical_formula_weight 3092.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_H-M_alt 'P 21 21 21' _space_group_name_Hall 'P 2ac 2ab' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_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 18.2305(5) _cell_length_b 18.9609(4) _cell_length_c 33.7647(6) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 11671.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 55860 _cell_measurement_theta_min 1.55 _cell_measurement_theta_max 27.30 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.760 _exptl_crystal_F_000 6076 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.450 _exptl_crystal_size_mid 0.370 _exptl_crystal_size_min 0.280 _exptl_absorpt_coefficient_mu 3.375 _shelx_estimated_absorpt_T_min 0.312 _shelx_estimated_absorpt_T_max 0.452 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.2628 _exptl_absorpt_correction_T_max 0.6540 _exptl_absorpt_process_details 'STOE X-RED & X-SHAPE' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean 6.667 _diffrn_reflns_number 51121 _diffrn_reflns_av_unetI/netI 0.0638 _diffrn_reflns_av_R_equivalents 0.0651 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 1.550 _diffrn_reflns_theta_max 25.248 _diffrn_reflns_theta_full 25.250 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_point_group_measured_fraction_full 0.999 _reflns_number_total 21132 _reflns_number_gt 18429 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.846 _reflns_Friedel_fraction_max 0.999 _reflns_Friedel_fraction_full 0.999 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA, PLATON (A.L.Spek, 2005)' _computing_data_reduction 'STOE X-RED, PLATON (A.L.Spek, 2005)' _computing_structure_solution 'SHELXS-2013 (Sheldrick, 2013)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _refine_special_details ; Two lattice CH2Cl2 per formula unit were badly disordered and were handled using the SQUEEZE option in PLATON (see below). One phenyl ring was twofold (70:30) disordered, and was refined with partial occupancy anisotropic (major component) or isotropic (minor component) carbon atoms, constrained to rigid hexagons. The thermal parameters of the carbons of the major component, and those of the carbons in three other rings which exhibited strong thermal motion, were refined using rigid-body restraints (SIMU). ; # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.245 0.877 0.177 246 81 '2(CH2Cl2) = 84 e' 2 0.254 0.123 0.677 246 81 '2(CH2Cl2) = 84 e' 3 0.745 0.623 0.823 246 81 '2(CH2Cl2) = 84 e' 4 0.754 0.377 0.323 246 81 '2(CH2Cl2) = 84 e' _platon_squeeze_details ; Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13 ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0253P)^2^] 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 x determined using 7763 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons and Flack (2004), Acta Cryst. A60, s61). ; _refine_ls_abs_structure_Flack -0.034(7) _chemical_absolute_configuration rmad _refine_ls_number_reflns 21132 _refine_ls_number_parameters 1408 _refine_ls_number_restraints 63 _refine_ls_R_factor_all 0.0352 _refine_ls_R_factor_gt 0.0287 _refine_ls_wR_factor_ref 0.0619 _refine_ls_wR_factor_gt 0.0603 _refine_ls_goodness_of_fit_ref 0.951 _refine_ls_restrained_S_all 0.951 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 0.34175(2) 0.42661(2) 0.55769(2) 0.02245(8) Uani 1 1 d . . . . . Dy2 Dy 0.42451(2) 0.61260(2) 0.55551(2) 0.02035(8) Uani 1 1 d . . . . . Dy3 Dy 0.28048(2) 0.56991(2) 0.48629(2) 0.02153(8) Uani 1 1 d . . . . . Dy4 Dy 0.16162(2) 0.52963(2) 0.56843(2) 0.02186(8) Uani 1 1 d . . . . . Dy5 Dy 0.30676(2) 0.56495(2) 0.63702(2) 0.02175(8) Uani 1 1 d . . . . . O21 O 0.2519(3) 0.4720(3) 0.60362(14) 0.0226(12) Uani 1 1 d D . . . . H21 H 0.2320 0.4350 0.6218 0.027 Uiso 1 1 calc DR U . . . O22 O 0.2359(3) 0.4762(3) 0.52171(15) 0.0214(12) Uani 1 1 d D . . . . H22 H 0.2095 0.4408 0.5050 0.026 Uiso 1 1 calc DR U . . . O23 O 0.3843(3) 0.5213(3) 0.51623(15) 0.0232(12) Uani 1 1 d D . . . . H23 H 0.4220 0.5057 0.4966 0.028 Uiso 1 1 calc DR U . . . O24 O 0.3956(3) 0.5178(3) 0.59786(15) 0.0219(12) Uani 1 1 d D . . . . H24 H 0.4389 0.5008 0.6133 0.026 Uiso 1 1 calc DR U . . . O25 O 0.2844(3) 0.5924(2) 0.56293(15) 0.0212(11) Uani 1 1 d D . . . . H25 H 0.2681 0.6383 0.5645 0.025 Uiso 1 1 calc DR U . . . O1 O 0.3861(3) 0.3657(3) 0.61222(17) 0.0290(13) Uani 1 1 d . . . . . O2 O 0.4635(3) 0.4027(3) 0.54534(18) 0.0337(14) Uani 1 1 d . . . . . O3 O 0.2598(4) 0.3364(3) 0.56722(18) 0.0337(15) Uani 1 1 d . . . . . O4 O 0.3341(4) 0.3666(3) 0.49781(16) 0.0285(13) Uani 1 1 d . . . . . O5 O 0.5277(3) 0.5736(3) 0.58733(15) 0.0265(12) Uani 1 1 d . . . . . O6 O 0.5200(3) 0.6234(3) 0.51145(16) 0.0270(12) Uani 1 1 d . . . . . O7 O 0.3789(3) 0.6651(3) 0.61455(17) 0.0263(13) Uani 1 1 d . . . . . O8 O 0.3745(4) 0.7507(3) 0.6603(2) 0.051(2) Uani 1 1 d . . . . . O9 O 0.3703(3) 0.5526(3) 0.43975(17) 0.0333(14) Uani 1 1 d . . . . . O10 O 0.2246(3) 0.5172(3) 0.43393(17) 0.0325(13) Uani 1 1 d . . . . . O11 O 0.3513(3) 0.6689(3) 0.50405(16) 0.0241(12) Uani 1 1 d . . . . . O12 O 0.3831(5) 0.7805(3) 0.4981(2) 0.052(2) Uani 1 1 d . . . . . O13 O 0.0907(3) 0.4488(3) 0.53608(17) 0.0297(14) Uani 1 1 d . . . . . O14 O 0.0869(3) 0.4820(3) 0.61615(15) 0.0287(13) Uani 1 1 d . . . . . O15 O 0.1620(3) 0.6072(3) 0.51292(15) 0.0234(11) Uani 1 1 d . . . . . O16 O 0.1086(3) 0.6889(3) 0.47424(18) 0.0326(14) Uani 1 1 d . . . . . O17 O 0.2551(3) 0.4908(3) 0.68268(16) 0.0294(14) Uani 1 1 d . . . . . O18 O 0.3940(3) 0.5495(3) 0.68520(16) 0.0298(14) Uani 1 1 d . . . . . O19 O 0.1884(3) 0.6082(3) 0.62385(15) 0.0244(12) Uani 1 1 d . . . . . O20 O 0.0838(4) 0.6590(4) 0.64163(18) 0.0409(16) Uani 1 1 d . . . . . N1 N 0.4673(4) 0.7372(3) 0.5662(2) 0.0254(15) Uani 1 1 d . . . . . H1A H 0.5206 0.7390 0.5606 0.031 Uiso 1 1 calc R U . . . H1B H 0.4427 0.7676 0.5464 0.031 Uiso 1 1 calc R U . . . N2 N 0.2558(4) 0.6722(3) 0.4426(2) 0.0289(16) Uani 1 1 d . . . . . H2A H 0.2662 0.6579 0.4150 0.035 Uiso 1 1 calc R U . . . H2B H 0.2028 0.6833 0.4442 0.035 Uiso 1 1 calc R U . . . N3 N 0.0496(4) 0.6033(4) 0.5632(2) 0.0380(18) Uani 1 1 d . . . . . H3A H 0.0069 0.5740 0.5709 0.046 Uiso 1 1 calc R U . . . H3B H 0.0534 0.6421 0.5828 0.046 Uiso 1 1 calc R U . . . N4 N 0.2619(4) 0.6518(4) 0.6876(2) 0.0287(16) Uani 1 1 d . . . . . H4A H 0.2661 0.6295 0.7140 0.034 Uiso 1 1 calc R U . . . H4B H 0.2957 0.6927 0.6873 0.034 Uiso 1 1 calc R U . . . C1 C 0.3878(7) 0.3296(5) 0.6909(3) 0.045(3) Uani 1 1 d . . . . . H1 H 0.3445 0.3488 0.6796 0.054 Uiso 1 1 calc R U . . . C2 C 0.3862(7) 0.3036(6) 0.7284(3) 0.055(3) Uani 1 1 d . . . . . H2 H 0.3413 0.3034 0.7428 0.066 Uiso 1 1 calc R U . . . C3 C 0.4493(7) 0.2774(5) 0.7460(3) 0.048(3) Uani 1 1 d . . . . . H3 H 0.4485 0.2608 0.7726 0.058 Uiso 1 1 calc R U . . . C4 C 0.5138(7) 0.2759(5) 0.7240(3) 0.053(3) Uani 1 1 d . . . . . H4 H 0.5576 0.2578 0.7353 0.064 Uiso 1 1 calc R U . . . C5 C 0.5135(7) 0.3009(5) 0.6858(3) 0.048(3) Uani 1 1 d . . . . . H5 H 0.5575 0.2986 0.6707 0.058 Uiso 1 1 calc R U . . . C6 C 0.4525(6) 0.3285(4) 0.6689(3) 0.035(2) Uani 1 1 d . . . . . C7 C 0.4485(6) 0.3571(4) 0.6280(3) 0.036(2) Uani 1 1 d . . . . . C8 C 0.5141(6) 0.3722(5) 0.6072(3) 0.040(2) Uani 1 1 d . . . . . H8 H 0.5586 0.3692 0.6218 0.048 Uiso 1 1 calc R U . . . C9 C 0.5196(5) 0.3909(4) 0.5676(3) 0.033(2) Uani 1 1 d . . . . . C10 C 0.5927(5) 0.3950(4) 0.5473(3) 0.038(2) Uani 1 1 d . . . . . C11 C 0.6541(6) 0.3631(5) 0.5631(4) 0.051(3) Uani 1 1 d . . . . . H11 H 0.6515 0.3392 0.5878 0.061 Uiso 1 1 calc R U . . . C12 C 0.7198(7) 0.3667(6) 0.5423(4) 0.067(4) Uani 1 1 d . . . . . H12 H 0.7617 0.3433 0.5527 0.081 Uiso 1 1 calc R U . . . C13 C 0.7262(6) 0.4022(5) 0.5079(4) 0.060(3) Uani 1 1 d . . . . . H13 H 0.7716 0.4038 0.4942 0.072 Uiso 1 1 calc R U . . . C14 C 0.6652(8) 0.4363(6) 0.4931(4) 0.072(4) Uani 1 1 d . . . . . H14 H 0.6687 0.4618 0.4689 0.087 Uiso 1 1 calc R U . . . C15 C 0.5985(6) 0.4335(6) 0.5132(4) 0.061(3) Uani 1 1 d . . . . . H15 H 0.5571 0.4583 0.5033 0.073 Uiso 1 1 calc R U . . . C16 C 0.1434(5) 0.2783(4) 0.6045(2) 0.066(3) Uani 1 1 d G U . . . H16 H 0.1734 0.3116 0.6180 0.080 Uiso 1 1 calc R U . . . C17 C 0.0908(6) 0.2402(6) 0.6253(2) 0.095(5) Uani 1 1 d G U . . . H17 H 0.0849 0.2474 0.6530 0.114 Uiso 1 1 calc R U . . . C18 C 0.0470(6) 0.1916(6) 0.6056(3) 0.138(9) Uani 1 1 d G U . . . H18 H 0.0111 0.1655 0.6198 0.166 Uiso 1 1 calc R U . . . C19 C 0.0557(5) 0.1811(6) 0.5651(3) 0.119(7) Uani 1 1 d G U . . . H19 H 0.0257 0.1478 0.5517 0.142 Uiso 1 1 calc R U . . . C20 C 0.1082(5) 0.2192(5) 0.54435(19) 0.073(4) Uani 1 1 d G U . . . H20 H 0.1141 0.2120 0.5167 0.087 Uiso 1 1 calc R U . . . C21 C 0.1521(4) 0.2678(4) 0.5640(2) 0.048(2) Uani 1 1 d G U . . . C22 C 0.2149(6) 0.3061(4) 0.5445(3) 0.036(2) Uani 1 1 d . U . . . C23 C 0.2211(6) 0.3051(5) 0.5029(3) 0.036(2) Uani 1 1 d . . . . . H23A H 0.1826 0.2847 0.4877 0.043 Uiso 1 1 calc R U . . . C24 C 0.2822(6) 0.3332(5) 0.4828(3) 0.038(2) Uani 1 1 d D U . . . C25A C 0.2882(6) 0.3158(6) 0.4394(2) 0.038(5) Uani 0.7 1 d DG U P A 1 C26A C 0.2263(5) 0.3033(8) 0.4163(3) 0.039(3) Uani 0.7 1 d G U P A 1 H26A H 0.1788 0.3083 0.4275 0.047 Uiso 0.7 1 calc R U P A 1 C27A C 0.2340(6) 0.2836(7) 0.3769(3) 0.053(5) Uani 0.7 1 d G U P A 1 H27A H 0.1917 0.2750 0.3612 0.064 Uiso 0.7 1 calc R U P A 1 C28A C 0.3035(7) 0.2763(7) 0.3605(2) 0.062(5) Uani 0.7 1 d G U P A 1 H28A H 0.3088 0.2627 0.3336 0.074 Uiso 0.7 1 calc R U P A 1 C29A C 0.3654(6) 0.2887(7) 0.3836(3) 0.073(5) Uani 0.7 1 d G U P A 1 H29A H 0.4129 0.2837 0.3724 0.088 Uiso 0.7 1 calc R U P A 1 C30A C 0.3577(5) 0.3085(6) 0.4230(3) 0.045(3) Uani 0.7 1 d G U P A 1 H30A H 0.4000 0.3170 0.4387 0.054 Uiso 0.7 1 calc R U P A 1 C25B C 0.287(2) 0.3249(19) 0.4375(6) 0.055(17) Uiso 0.3 1 d DG . P A 2 C26B C 0.2371(18) 0.285(2) 0.4158(10) 0.065(18) Uiso 0.3 1 d G . P A 2 H26B H 0.1964 0.2634 0.4287 0.078 Uiso 0.3 1 calc R U P A 2 C27B C 0.2469(19) 0.2759(19) 0.3753(9) 0.070(19) Uiso 0.3 1 d G . P A 2 H27B H 0.2130 0.2485 0.3605 0.084 Uiso 0.3 1 calc R U P A 2 C28B C 0.306(2) 0.3072(17) 0.3565(5) 0.068(15) Uiso 0.3 1 d G . P A 2 H28B H 0.3131 0.3011 0.3288 0.081 Uiso 0.3 1 calc R U P A 2 C29B C 0.3560(15) 0.3473(14) 0.3781(7) 0.053(9) Uiso 0.3 1 d G . P A 2 H29B H 0.3966 0.3687 0.3652 0.064 Uiso 0.3 1 calc R U P A 2 C30B C 0.3462(16) 0.3562(15) 0.4186(7) 0.053(9) Uiso 0.3 1 d G . P A 2 H30B H 0.3801 0.3836 0.4334 0.063 Uiso 0.3 1 calc R U P A 2 C31 C -0.0130(5) 0.5026(5) 0.6783(3) 0.036(2) Uani 1 1 d . . . . . H31 H 0.0198 0.5404 0.6731 0.043 Uiso 1 1 calc R U . . . C32 C -0.0550(6) 0.5035(6) 0.7121(3) 0.047(3) Uani 1 1 d . . . . . H32 H -0.0528 0.5427 0.7296 0.056 Uiso 1 1 calc R U . . . C33 C -0.1006(6) 0.4472(7) 0.7205(3) 0.053(3) Uani 1 1 d . . . . . H33 H -0.1292 0.4474 0.7440 0.063 Uiso 1 1 calc R U . . . C34 C -0.1046(5) 0.3919(6) 0.6953(3) 0.041(2) Uani 1 1 d . . . . . H34 H -0.1360 0.3535 0.7014 0.049 Uiso 1 1 calc R U . . . C35 C -0.0641(5) 0.3905(5) 0.6613(3) 0.038(2) Uani 1 1 d . . . . . H35 H -0.0672 0.3509 0.6442 0.046 Uiso 1 1 calc R U . . . C36 C -0.0181(5) 0.4469(4) 0.6515(2) 0.029(2) Uani 1 1 d . . . . . C37 C 0.0256(5) 0.4504(4) 0.6144(2) 0.0241(18) Uani 1 1 d . . . . . C38 C -0.0041(5) 0.4196(4) 0.5801(2) 0.0293(19) Uani 1 1 d . . . . . H38 H -0.0517 0.3995 0.5821 0.035 Uiso 1 1 calc R U . . . C39 C 0.0304(5) 0.4164(4) 0.5437(2) 0.0268(19) Uani 1 1 d . . . . . C40 C -0.0008(5) 0.3720(4) 0.5114(3) 0.0285(19) Uani 1 1 d . . . . . C41 C -0.0703(6) 0.3410(5) 0.5138(3) 0.046(2) Uani 1 1 d . . . . . H41 H -0.1008 0.3505 0.5360 0.055 Uiso 1 1 calc R U . . . C42 C -0.0951(7) 0.2971(6) 0.4843(3) 0.057(3) Uani 1 1 d . . . . . H42 H -0.1423 0.2763 0.4864 0.069 Uiso 1 1 calc R U . . . C43 C -0.0525(6) 0.2829(5) 0.4517(3) 0.047(3) Uani 1 1 d . . . . . H43 H -0.0693 0.2510 0.4320 0.056 Uiso 1 1 calc R U . . . C44 C 0.0145(7) 0.3153(5) 0.4477(3) 0.053(3) Uani 1 1 d . . . . . H44 H 0.0438 0.3072 0.4249 0.064 Uiso 1 1 calc R U . . . C45 C 0.0392(6) 0.3604(5) 0.4778(3) 0.044(2) Uani 1 1 d . . . . . H45 H 0.0851 0.3836 0.4748 0.053 Uiso 1 1 calc R U . . . C46 C 0.1140(6) 0.4588(6) 0.3902(3) 0.049(3) Uani 1 1 d . U . . . H46 H 0.1037 0.4775 0.4157 0.059 Uiso 1 1 calc R U . . . C47 C 0.0588(7) 0.4240(7) 0.3690(4) 0.067(3) Uani 1 1 d . U . . . H47 H 0.0109 0.4203 0.3800 0.080 Uiso 1 1 calc R U . . . C48 C 0.0730(8) 0.3956(6) 0.3332(3) 0.060(3) Uani 1 1 d . U . . . H48 H 0.0357 0.3706 0.3195 0.072 Uiso 1 1 calc R U . . . C49 C 0.1413(7) 0.4026(5) 0.3164(3) 0.051(3) Uani 1 1 d . U . . . H49 H 0.1509 0.3830 0.2911 0.062 Uiso 1 1 calc R U . . . C50 C 0.1966(6) 0.4385(5) 0.3368(3) 0.048(2) Uani 1 1 d . U . . . H50 H 0.2436 0.4441 0.3250 0.057 Uiso 1 1 calc R U . . . C51 C 0.1831(6) 0.4660(5) 0.3742(3) 0.036(2) Uani 1 1 d . U . . . C52 C 0.2417(6) 0.5007(5) 0.3986(3) 0.042(3) Uani 1 1 d . . . . . C53 C 0.3123(7) 0.5107(6) 0.3826(3) 0.052(3) Uani 1 1 d . . . . . H53 H 0.3186 0.5018 0.3551 0.062 Uiso 1 1 calc R U . . . C54 C 0.3740(5) 0.5329(5) 0.4040(3) 0.033(2) Uani 1 1 d . U . . . C55 C 0.4487(3) 0.5337(4) 0.38569(18) 0.042(2) Uani 1 1 d G U . . . C56 C 0.4579(4) 0.5339(5) 0.34483(17) 0.085(5) Uani 1 1 d G U . . . H56A H 0.4163 0.5335 0.3279 0.102 Uiso 1 1 calc R U . . . C57 C 0.5280(4) 0.5349(5) 0.32872(15) 0.094(5) Uani 1 1 d G U . . . H57A H 0.5344 0.5351 0.3008 0.113 Uiso 1 1 calc R U . . . C58 C 0.5890(3) 0.5355(5) 0.3535(2) 0.073(4) Uani 1 1 d G U . . . H58A H 0.6369 0.5361 0.3425 0.088 Uiso 1 1 calc R U . . . C59 C 0.5797(3) 0.5352(5) 0.3943(2) 0.071(3) Uani 1 1 d G U . . . H59A H 0.6214 0.5357 0.4112 0.085 Uiso 1 1 calc R U . . . C60 C 0.5096(4) 0.5343(4) 0.41044(14) 0.062(3) Uani 1 1 d G U . . . H60A H 0.5033 0.5341 0.4384 0.074 Uiso 1 1 calc R U . . . C61 C 0.5937(6) 0.6858(5) 0.4495(3) 0.042(2) Uani 1 1 d . . . . . H61 H 0.5423 0.6926 0.4519 0.051 Uiso 1 1 calc R U . . . C62 C 0.6298(7) 0.7120(6) 0.4171(3) 0.058(3) Uani 1 1 d . . . . . H62 H 0.6033 0.7390 0.3982 0.069 Uiso 1 1 calc R U . . . C63 C 0.7047(7) 0.7001(7) 0.4111(4) 0.063(3) Uani 1 1 d . . . . . H63 H 0.7285 0.7161 0.3878 0.075 Uiso 1 1 calc R U . . . C64 C 0.7438(6) 0.6638(6) 0.4405(3) 0.052(3) Uani 1 1 d . . . . . H64 H 0.7951 0.6564 0.4380 0.062 Uiso 1 1 calc R U . . . C65 C 0.7060(5) 0.6390(6) 0.4734(3) 0.045(3) Uani 1 1 d . . . . . H65 H 0.7324 0.6136 0.4931 0.054 Uiso 1 1 calc R U . . . C66 C 0.6312(5) 0.6497(4) 0.4789(2) 0.0288(19) Uani 1 1 d . . . . . C67 C 0.5901(5) 0.6238(4) 0.5140(2) 0.0265(18) Uani 1 1 d . . . . . C68 C 0.6295(5) 0.6012(4) 0.5477(2) 0.0284(19) Uani 1 1 d . . . . . H68 H 0.6813 0.6062 0.5477 0.034 Uiso 1 1 calc R U . . . C69 C 0.5965(4) 0.5722(4) 0.5809(2) 0.0250(17) Uani 1 1 d . . . . . C70 C 0.6415(5) 0.5370(4) 0.6125(2) 0.0281(19) Uani 1 1 d . . . . . C71 C 0.6079(5) 0.5209(5) 0.6479(3) 0.037(2) Uani 1 1 d . . . . . H71 H 0.5585 0.5346 0.6523 0.044 Uiso 1 1 calc R U . . . C72 C 0.6458(6) 0.4847(5) 0.6771(3) 0.042(2) Uani 1 1 d . . . . . H72 H 0.6218 0.4727 0.7011 0.050 Uiso 1 1 calc R U . . . C73 C 0.7175(6) 0.4661(6) 0.6715(3) 0.049(3) Uani 1 1 d . . . . . H73 H 0.7435 0.4424 0.6919 0.059 Uiso 1 1 calc R U . . . C74 C 0.7519(6) 0.4816(6) 0.6367(3) 0.052(3) Uani 1 1 d . . . . . H74 H 0.8016 0.4684 0.6328 0.062 Uiso 1 1 calc R U . . . C75 C 0.7142(5) 0.5166(5) 0.6070(3) 0.040(2) Uani 1 1 d . . . . . H75 H 0.7381 0.5268 0.5827 0.048 Uiso 1 1 calc R U . . . C76 C 0.1498(5) 0.4079(5) 0.7145(3) 0.037(2) Uani 1 1 d . . . . . H76 H 0.1449 0.4249 0.6882 0.045 Uiso 1 1 calc R U . . . C77 C 0.0945(6) 0.3664(6) 0.7308(3) 0.054(3) Uani 1 1 d . . . . . H77 H 0.0524 0.3552 0.7155 0.065 Uiso 1 1 calc R U . . . C78 C 0.1004(7) 0.3416(7) 0.7686(4) 0.069(4) Uani 1 1 d . . . . . H78 H 0.0628 0.3128 0.7795 0.083 Uiso 1 1 calc R U . . . C79 C 0.1629(7) 0.3591(8) 0.7918(4) 0.075(4) Uani 1 1 d . . . . . H79 H 0.1669 0.3435 0.8184 0.090 Uiso 1 1 calc R U . . . C80 C 0.2175(6) 0.3991(7) 0.7749(3) 0.056(3) Uani 1 1 d . . . . . H80 H 0.2601 0.4094 0.7900 0.067 Uiso 1 1 calc R U . . . C81 C 0.2128(5) 0.4250(5) 0.7364(2) 0.034(2) Uani 1 1 d . . . . . C82 C 0.2710(5) 0.4687(4) 0.7171(2) 0.0287(19) Uani 1 1 d . . . . . C83 C 0.3364(5) 0.4826(5) 0.7361(2) 0.033(2) Uani 1 1 d . . . . . H83 H 0.3418 0.4668 0.7627 0.040 Uiso 1 1 calc R U . . . C84 C 0.3961(5) 0.5189(4) 0.7187(2) 0.0277(19) Uani 1 1 d . . . . . C85 C 0.4665(5) 0.5240(5) 0.7407(2) 0.033(2) Uani 1 1 d . . . . . C86 C 0.5120(5) 0.5825(5) 0.7362(3) 0.039(2) Uani 1 1 d . . . . . H86 H 0.4984 0.6186 0.7182 0.047 Uiso 1 1 calc R U . . . C87 C 0.5759(6) 0.5891(6) 0.7571(3) 0.050(3) Uani 1 1 d . . . . . H87 H 0.6061 0.6293 0.7533 0.060 Uiso 1 1 calc R U . . . C88 C 0.5968(6) 0.5370(6) 0.7840(3) 0.052(3) Uani 1 1 d . . . . . H88 H 0.6413 0.5413 0.7984 0.062 Uiso 1 1 calc R U . . . C89 C 0.5520(6) 0.4791(6) 0.7895(3) 0.045(2) Uani 1 1 d . . . . . H89 H 0.5654 0.4439 0.8081 0.053 Uiso 1 1 calc R U . . . C90 C 0.4879(5) 0.4719(5) 0.7681(3) 0.039(2) Uani 1 1 d . . . . . H90 H 0.4579 0.4314 0.7719 0.047 Uiso 1 1 calc R U . . . C91 C 0.1481(5) 0.6463(4) 0.6472(2) 0.030(2) Uani 1 1 d . . . . . C92 C 0.1868(5) 0.6788(4) 0.6834(2) 0.0293(19) Uani 1 1 d . . . . . H92 H 0.1902 0.7308 0.6789 0.035 Uiso 1 1 calc R U . . . C93 C 0.1400(5) 0.6673(5) 0.7193(3) 0.032(2) Uani 1 1 d . . . . . C94 C 0.1321(6) 0.5986(5) 0.7343(3) 0.043(2) Uani 1 1 d . . . . . H94 H 0.1570 0.5607 0.7218 0.051 Uiso 1 1 calc R U . . . C95 C 0.0889(7) 0.5855(6) 0.7666(3) 0.056(3) Uani 1 1 d . . . . . H95 H 0.0850 0.5390 0.7768 0.068 Uiso 1 1 calc R U . . . C96 C 0.0509(7) 0.6402(7) 0.7844(3) 0.065(4) Uani 1 1 d . . . . . H96 H 0.0208 0.6312 0.8068 0.078 Uiso 1 1 calc R U . . . C97 C 0.0569(8) 0.7076(7) 0.7696(4) 0.071(4) Uani 1 1 d . . . . . H97 H 0.0299 0.7450 0.7814 0.086 Uiso 1 1 calc R U . . . C98 C 0.1023(6) 0.7205(5) 0.7376(3) 0.045(3) Uani 1 1 d . . . . . H98 H 0.1075 0.7674 0.7281 0.054 Uiso 1 1 calc R U . . . C99 C 0.1066(5) 0.6462(4) 0.5014(3) 0.0273(19) Uani 1 1 d . . . . . C100 C 0.0345(5) 0.6345(4) 0.5239(3) 0.031(2) Uani 1 1 d . . . . . H100 H 0.0109 0.6816 0.5281 0.037 Uiso 1 1 calc R U . . . C101 C -0.0181(5) 0.5889(4) 0.5006(3) 0.033(2) Uani 1 1 d . . . . . C102 C -0.0066(6) 0.5686(5) 0.4624(3) 0.044(2) Uani 1 1 d . . . . . H102 H 0.0377 0.5810 0.4493 0.053 Uiso 1 1 calc R U . . . C103 C -0.0589(6) 0.5303(5) 0.4427(4) 0.058(3) Uani 1 1 d . . . . . H103 H -0.0501 0.5176 0.4159 0.069 Uiso 1 1 calc R U . . . C104 C -0.1225(7) 0.5098(6) 0.4599(5) 0.065(4) Uani 1 1 d . . . . . H104 H -0.1576 0.4830 0.4455 0.078 Uiso 1 1 calc R U . . . C105 C -0.1349(6) 0.5283(6) 0.4980(4) 0.058(3) Uani 1 1 d . . . . . H105 H -0.1790 0.5142 0.5107 0.070 Uiso 1 1 calc R U . . . C106 C -0.0831(6) 0.5679(5) 0.5189(3) 0.049(3) Uani 1 1 d . . . . . H106 H -0.0923 0.5806 0.5457 0.059 Uiso 1 1 calc R U . . . C107 C 0.3485(5) 0.7295(4) 0.4866(3) 0.0296(19) Uani 1 1 d . . . . . C108 C 0.2971(5) 0.7373(4) 0.4509(2) 0.0292(19) Uani 1 1 d . . . . . H108 H 0.2607 0.7751 0.4574 0.035 Uiso 1 1 calc R U . . . C109 C 0.3402(5) 0.7615(4) 0.4153(3) 0.0315(19) Uani 1 1 d . . . . . C110 C 0.4015(5) 0.7240(5) 0.4022(3) 0.036(2) Uani 1 1 d . . . . . H110 H 0.4165 0.6830 0.4162 0.043 Uiso 1 1 calc R U . . . C111 C 0.4403(6) 0.7451(5) 0.3696(3) 0.044(2) Uani 1 1 d . . . . . H111 H 0.4818 0.7188 0.3611 0.053 Uiso 1 1 calc R U . . . C112 C 0.4192(6) 0.8046(6) 0.3490(3) 0.051(3) Uani 1 1 d . . . . . H112 H 0.4462 0.8200 0.3265 0.061 Uiso 1 1 calc R U . . . C113 C 0.3583(7) 0.8411(6) 0.3615(3) 0.052(3) Uani 1 1 d . . . . . H113 H 0.3432 0.8817 0.3472 0.063 Uiso 1 1 calc R U . . . C114 C 0.3188(6) 0.8206(5) 0.3941(3) 0.047(3) Uani 1 1 d . . . . . H114 H 0.2769 0.8468 0.4021 0.056 Uiso 1 1 calc R U . . . C115 C 0.3979(5) 0.7268(4) 0.6295(3) 0.030(2) Uani 1 1 d . . . . . C116 C 0.4550(5) 0.7683(4) 0.6058(3) 0.030(2) Uani 1 1 d . . . . . H116 H 0.4358 0.8173 0.6019 0.036 Uiso 1 1 calc R U . . . C117 C 0.5266(5) 0.7735(4) 0.6282(3) 0.031(2) Uani 1 1 d . . . . . C118 C 0.5625(6) 0.7130(5) 0.6418(3) 0.039(2) Uani 1 1 d . . . . . H118 H 0.5387 0.6686 0.6397 0.047 Uiso 1 1 calc R U . . . C119 C 0.6319(7) 0.7162(6) 0.6584(3) 0.054(3) Uani 1 1 d . . . . . H119 H 0.6559 0.6743 0.6669 0.064 Uiso 1 1 calc R U . . . C120 C 0.6659(7) 0.7809(7) 0.6624(3) 0.057(3) Uani 1 1 d . . . . . H120 H 0.7136 0.7836 0.6736 0.069 Uiso 1 1 calc R U . . . C121 C 0.6314(7) 0.8401(6) 0.6505(3) 0.054(3) Uani 1 1 d . . . . . H121 H 0.6548 0.8845 0.6541 0.064 Uiso 1 1 calc R U . . . C122 C 0.5623(6) 0.8375(5) 0.6332(3) 0.042(2) Uani 1 1 d . . . . . H122 H 0.5394 0.8799 0.6246 0.050 Uiso 1 1 calc R U . . . C123 C 0.6801(7) 0.3459(6) 0.7682(3) 0.063(3) Uani 1 1 d . . . . . H12A H 0.6532 0.3831 0.7537 0.075 Uiso 1 1 calc R U . . . H12B H 0.6448 0.3214 0.7857 0.075 Uiso 1 1 calc R U . . . Cl1 Cl 0.7166(2) 0.28564(17) 0.73440(10) 0.0707(9) Uani 1 1 d . . . . . Cl2 Cl 0.7481(3) 0.3841(2) 0.79658(14) 0.1035(14) 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 Dy1 0.02354(19) 0.02173(15) 0.02207(18) 0.00024(16) 0.00018(17) -0.00003(16) Dy2 0.01873(19) 0.02369(16) 0.01864(18) -0.00001(15) -0.00024(16) -0.00172(15) Dy3 0.02029(18) 0.02570(17) 0.01862(18) 0.00231(16) -0.00064(15) -0.00349(17) Dy4 0.01844(19) 0.02718(17) 0.01995(18) 0.00235(15) 0.00028(16) -0.00133(16) Dy5 0.01966(18) 0.02671(18) 0.01889(18) 0.00011(16) 0.00103(16) -0.00071(16) O21 0.028(3) 0.027(3) 0.013(3) 0.002(2) 0.005(2) 0.004(3) O22 0.020(3) 0.021(2) 0.023(3) 0.000(2) -0.003(2) -0.004(2) O23 0.027(3) 0.025(3) 0.017(3) 0.001(2) -0.003(2) 0.000(2) O24 0.025(3) 0.025(3) 0.015(3) 0.006(2) 0.004(2) 0.001(2) O25 0.024(3) 0.023(2) 0.016(3) 0.002(2) -0.002(2) -0.001(2) O1 0.029(4) 0.033(3) 0.025(3) 0.005(3) -0.003(3) 0.005(3) O2 0.029(4) 0.031(3) 0.041(4) 0.000(3) 0.007(3) 0.005(3) O3 0.046(4) 0.022(2) 0.033(3) 0.002(3) -0.006(3) -0.013(3) O4 0.034(3) 0.027(3) 0.024(3) -0.009(2) 0.000(3) -0.003(3) O5 0.023(3) 0.033(3) 0.024(3) 0.006(3) -0.001(2) 0.000(3) O6 0.021(3) 0.036(3) 0.024(3) -0.002(3) 0.001(3) 0.000(2) O7 0.021(3) 0.027(3) 0.031(3) -0.003(2) 0.004(3) -0.003(2) O8 0.058(5) 0.046(4) 0.048(4) -0.023(3) 0.027(4) -0.023(4) O9 0.033(3) 0.045(3) 0.022(3) -0.004(3) 0.004(3) -0.002(3) O10 0.032(3) 0.038(3) 0.027(3) -0.001(3) 0.000(3) -0.010(3) O11 0.021(3) 0.024(3) 0.027(3) 0.003(2) -0.003(3) -0.002(2) O12 0.072(6) 0.034(3) 0.049(4) 0.020(3) -0.027(4) -0.024(4) O13 0.020(3) 0.038(3) 0.031(3) -0.003(3) 0.002(3) -0.007(2) O14 0.028(3) 0.039(3) 0.018(3) 0.005(3) 0.002(3) -0.008(3) O15 0.021(3) 0.027(2) 0.022(3) 0.005(2) -0.002(3) 0.002(3) O16 0.024(3) 0.036(3) 0.037(4) 0.016(3) -0.003(3) 0.003(3) O17 0.022(3) 0.044(3) 0.022(3) 0.006(3) -0.002(3) -0.005(3) O18 0.028(3) 0.043(3) 0.019(3) 0.000(2) -0.004(3) -0.001(3) O19 0.019(3) 0.030(3) 0.024(3) -0.001(2) -0.002(2) 0.001(3) O20 0.032(4) 0.065(4) 0.026(3) -0.003(3) -0.007(3) 0.019(3) N1 0.026(4) 0.025(3) 0.026(4) 0.000(3) -0.001(3) -0.003(3) N2 0.022(4) 0.038(3) 0.027(4) 0.011(3) -0.010(3) -0.010(3) N3 0.024(4) 0.061(4) 0.029(4) 0.009(4) 0.002(3) 0.007(4) N4 0.028(4) 0.037(4) 0.021(4) 0.000(3) 0.006(3) -0.002(3) C1 0.053(7) 0.044(5) 0.038(6) -0.001(5) -0.005(5) 0.009(5) C2 0.056(8) 0.061(7) 0.047(7) 0.011(5) 0.009(6) 0.008(6) C3 0.074(9) 0.042(5) 0.028(5) 0.001(4) -0.007(6) -0.001(6) C4 0.057(8) 0.052(6) 0.052(7) 0.015(5) -0.014(6) 0.012(6) C5 0.051(7) 0.046(5) 0.048(6) 0.004(5) -0.003(6) 0.006(5) C6 0.055(7) 0.022(4) 0.029(5) 0.003(4) -0.012(5) 0.002(4) C7 0.045(6) 0.026(4) 0.037(5) -0.003(4) -0.007(5) 0.004(4) C8 0.033(6) 0.040(5) 0.046(6) -0.005(4) -0.005(5) 0.003(4) C9 0.026(5) 0.029(4) 0.042(5) -0.002(4) -0.006(4) -0.003(4) C10 0.043(6) 0.027(4) 0.044(6) 0.000(4) 0.001(5) -0.005(4) C11 0.034(6) 0.054(5) 0.065(7) -0.002(5) 0.011(6) 0.009(5) C12 0.044(7) 0.055(7) 0.104(11) -0.019(7) 0.010(7) 0.002(6) C13 0.040(6) 0.031(5) 0.110(10) 0.007(6) 0.025(7) -0.003(5) C14 0.067(8) 0.059(6) 0.092(9) 0.026(7) 0.027(8) 0.008(7) C15 0.051(7) 0.052(6) 0.079(8) 0.022(7) 0.020(6) 0.015(6) C16 0.064(9) 0.065(7) 0.070(7) -0.003(6) 0.023(7) -0.010(6) C17 0.085(12) 0.132(13) 0.069(9) 0.009(8) 0.024(8) -0.034(9) C18 0.104(15) 0.22(2) 0.093(10) -0.006(13) 0.032(11) -0.100(15) C19 0.097(14) 0.166(16) 0.092(10) -0.006(11) 0.019(10) -0.084(12) C20 0.058(8) 0.086(8) 0.075(8) 0.012(7) -0.004(6) -0.037(7) C21 0.052(7) 0.038(5) 0.053(6) 0.004(5) -0.004(5) -0.003(4) C22 0.042(6) 0.023(4) 0.044(5) -0.002(4) -0.005(5) 0.000(4) C23 0.035(5) 0.038(5) 0.036(5) 0.000(4) -0.008(4) -0.007(4) C24 0.039(6) 0.034(4) 0.040(5) -0.018(4) -0.004(5) 0.006(4) C25A 0.040(8) 0.036(8) 0.039(8) -0.021(7) -0.002(6) 0.004(6) C26A 0.048(8) 0.032(8) 0.038(7) 0.000(6) -0.008(6) 0.011(8) C27A 0.066(10) 0.054(10) 0.040(9) -0.007(7) -0.021(8) 0.005(9) C28A 0.082(11) 0.067(12) 0.036(8) -0.021(8) 0.000(7) 0.002(11) C29A 0.065(10) 0.109(14) 0.046(9) -0.039(10) 0.013(8) -0.004(11) C30A 0.051(8) 0.055(8) 0.028(6) -0.007(6) -0.004(6) -0.006(7) C31 0.025(5) 0.055(5) 0.028(5) 0.002(4) 0.004(4) -0.008(4) C32 0.031(6) 0.074(7) 0.036(6) -0.004(5) 0.004(5) -0.005(5) C33 0.030(6) 0.104(9) 0.023(5) 0.015(6) 0.005(4) 0.006(6) C34 0.026(5) 0.063(6) 0.033(5) 0.019(5) -0.006(4) -0.008(5) C35 0.026(5) 0.048(5) 0.042(5) 0.014(5) 0.002(4) -0.004(4) C36 0.024(4) 0.040(5) 0.023(4) 0.011(4) 0.004(4) 0.000(4) C37 0.024(4) 0.026(4) 0.023(4) 0.007(3) 0.000(4) -0.003(3) C38 0.021(4) 0.038(5) 0.029(4) 0.009(4) 0.004(4) -0.004(4) C39 0.025(5) 0.028(4) 0.027(4) 0.003(3) -0.001(4) -0.001(3) C40 0.029(5) 0.026(4) 0.030(5) 0.005(4) -0.003(4) -0.003(3) C41 0.040(6) 0.052(5) 0.046(6) -0.009(5) 0.006(5) -0.016(5) C42 0.053(8) 0.068(7) 0.052(7) -0.003(6) 0.007(6) -0.030(6) C43 0.053(7) 0.036(5) 0.051(7) -0.005(5) -0.009(6) -0.010(5) C44 0.053(7) 0.060(6) 0.047(6) -0.026(5) 0.005(6) -0.005(5) C45 0.030(5) 0.063(6) 0.039(6) -0.004(5) 0.002(5) -0.013(5) C46 0.044(6) 0.061(6) 0.042(6) -0.011(5) -0.001(5) -0.015(5) C47 0.048(7) 0.085(8) 0.066(7) -0.012(7) -0.011(6) -0.019(7) C48 0.072(7) 0.056(6) 0.052(6) -0.005(5) -0.027(6) -0.019(7) C49 0.083(8) 0.046(5) 0.025(5) -0.011(4) -0.023(5) -0.009(6) C50 0.054(6) 0.051(6) 0.038(5) -0.009(5) -0.006(5) -0.007(5) C51 0.046(6) 0.035(4) 0.028(4) 0.002(4) -0.007(4) -0.010(4) C52 0.048(7) 0.040(5) 0.036(6) 0.003(4) -0.010(5) -0.014(5) C53 0.061(8) 0.069(7) 0.025(5) -0.013(5) 0.006(5) -0.022(6) C54 0.036(5) 0.041(5) 0.023(4) -0.001(4) 0.003(4) -0.004(4) C55 0.048(6) 0.048(5) 0.028(5) -0.007(4) 0.012(4) -0.010(5) C56 0.057(7) 0.161(14) 0.037(6) -0.040(8) 0.018(5) -0.030(9) C57 0.072(8) 0.173(15) 0.037(6) -0.035(8) 0.027(5) -0.045(10) C58 0.053(7) 0.110(10) 0.057(7) -0.023(7) 0.027(5) -0.010(7) C59 0.048(6) 0.105(9) 0.060(6) -0.004(7) 0.005(6) -0.007(8) C60 0.042(6) 0.100(9) 0.043(6) -0.003(6) 0.008(5) -0.004(7) C61 0.031(6) 0.049(5) 0.047(6) 0.018(5) 0.001(5) 0.007(4) C62 0.045(7) 0.069(7) 0.058(7) 0.040(6) 0.001(6) -0.003(6) C63 0.045(8) 0.084(8) 0.059(7) 0.028(7) 0.014(6) -0.004(6) C64 0.027(6) 0.082(7) 0.046(6) 0.004(6) 0.012(5) -0.002(5) C65 0.031(6) 0.068(7) 0.035(5) 0.012(5) 0.007(4) 0.009(5) C66 0.033(5) 0.030(4) 0.023(5) 0.001(4) -0.002(4) -0.001(4) C67 0.029(5) 0.027(4) 0.024(4) -0.007(4) 0.004(4) 0.000(3) C68 0.018(4) 0.039(4) 0.028(5) 0.004(4) -0.002(4) 0.002(4) C69 0.027(4) 0.026(4) 0.022(4) -0.004(4) -0.002(3) -0.001(4) C70 0.027(5) 0.026(4) 0.031(5) -0.003(4) -0.006(4) 0.001(4) C71 0.029(5) 0.050(5) 0.031(5) 0.002(4) 0.000(4) 0.006(4) C72 0.039(6) 0.053(6) 0.033(5) 0.011(4) 0.001(5) 0.007(5) C73 0.045(6) 0.058(6) 0.045(6) 0.018(5) -0.007(5) 0.013(5) C74 0.034(6) 0.066(7) 0.056(7) 0.011(6) -0.009(5) 0.016(5) C75 0.029(5) 0.053(5) 0.039(5) 0.012(4) -0.001(4) 0.008(5) C76 0.034(6) 0.048(5) 0.030(5) 0.010(4) -0.002(4) -0.008(4) C77 0.040(7) 0.069(7) 0.054(7) 0.028(6) -0.010(5) -0.010(5) C78 0.040(7) 0.103(10) 0.064(8) 0.050(8) -0.005(6) -0.014(7) C79 0.035(6) 0.137(12) 0.054(7) 0.056(8) -0.004(6) -0.016(8) C80 0.035(6) 0.103(9) 0.031(5) 0.033(6) -0.009(5) -0.005(6) C81 0.023(5) 0.049(5) 0.029(4) 0.013(4) 0.001(4) -0.005(4) C82 0.032(5) 0.034(4) 0.020(4) 0.004(4) 0.002(4) 0.002(4) C83 0.031(5) 0.045(5) 0.023(4) 0.001(4) -0.003(4) -0.001(4) C84 0.035(5) 0.029(4) 0.019(4) -0.003(4) -0.002(4) 0.003(4) C85 0.033(5) 0.042(5) 0.025(4) -0.006(4) -0.008(4) 0.004(4) C86 0.029(5) 0.046(5) 0.043(6) -0.008(4) -0.004(4) -0.001(4) C87 0.039(6) 0.058(6) 0.055(7) -0.010(5) -0.007(6) -0.002(5) C88 0.042(6) 0.071(7) 0.044(6) -0.015(6) -0.023(5) 0.011(6) C89 0.041(6) 0.057(6) 0.036(5) -0.007(5) -0.012(5) 0.005(5) C90 0.034(5) 0.043(5) 0.039(5) 0.000(5) -0.005(4) 0.005(5) C91 0.034(6) 0.030(4) 0.026(4) 0.005(3) 0.008(4) 0.005(4) C92 0.037(5) 0.031(4) 0.020(4) -0.001(3) 0.008(4) 0.004(4) C93 0.021(5) 0.048(5) 0.027(5) -0.006(4) 0.007(4) -0.006(4) C94 0.038(6) 0.045(5) 0.045(6) 0.002(5) 0.015(5) 0.006(4) C95 0.054(8) 0.067(7) 0.048(6) -0.001(6) 0.011(6) -0.012(6) C96 0.059(8) 0.103(10) 0.032(6) -0.010(6) 0.018(6) -0.021(7) C97 0.068(10) 0.077(8) 0.069(8) -0.021(7) 0.040(7) -0.005(7) C98 0.042(6) 0.045(5) 0.049(6) -0.014(5) 0.010(5) 0.002(5) C99 0.028(5) 0.026(4) 0.028(5) -0.006(4) -0.009(4) -0.003(4) C100 0.023(5) 0.036(4) 0.035(5) 0.001(4) 0.000(4) 0.003(4) C101 0.026(5) 0.022(4) 0.050(6) 0.014(4) -0.011(4) 0.000(3) C102 0.043(6) 0.052(5) 0.038(5) 0.012(5) -0.007(5) -0.007(5) C103 0.059(8) 0.059(6) 0.055(7) 0.007(6) -0.019(6) -0.026(6) C104 0.047(8) 0.044(6) 0.105(11) 0.009(7) -0.021(7) -0.013(5) C105 0.036(6) 0.045(6) 0.094(10) 0.007(6) 0.008(6) -0.009(5) C106 0.039(6) 0.035(5) 0.074(7) 0.007(5) 0.002(6) 0.004(5) C107 0.027(5) 0.028(4) 0.034(5) 0.005(4) -0.002(4) -0.003(4) C108 0.025(5) 0.033(4) 0.029(5) 0.011(4) -0.004(4) -0.004(4) C109 0.030(5) 0.035(4) 0.030(5) 0.004(4) -0.006(4) -0.004(4) C110 0.020(5) 0.044(5) 0.044(6) 0.007(4) -0.006(4) -0.005(4) C111 0.032(6) 0.057(6) 0.043(6) -0.011(5) 0.005(5) -0.008(5) C112 0.041(7) 0.068(7) 0.044(6) 0.008(5) -0.002(5) -0.028(6) C113 0.056(8) 0.057(6) 0.044(6) 0.027(5) -0.002(6) -0.011(6) C114 0.053(7) 0.043(5) 0.046(6) 0.016(5) -0.001(5) 0.001(5) C115 0.026(5) 0.033(4) 0.031(5) -0.012(4) 0.001(4) -0.004(4) C116 0.030(5) 0.023(4) 0.038(5) 0.005(4) 0.001(4) -0.002(4) C117 0.031(5) 0.035(4) 0.027(5) -0.001(4) 0.005(4) -0.001(4) C118 0.040(6) 0.036(5) 0.040(5) -0.006(4) -0.007(5) -0.001(4) C119 0.052(7) 0.065(7) 0.044(6) -0.021(5) -0.019(6) 0.005(6) C120 0.033(6) 0.098(9) 0.041(6) -0.006(6) -0.016(5) -0.007(6) C121 0.065(8) 0.066(7) 0.031(6) 0.004(5) -0.009(5) -0.033(6) C122 0.049(7) 0.042(5) 0.033(5) 0.006(4) -0.011(5) -0.013(5) C123 0.062(9) 0.067(7) 0.058(7) 0.026(6) 0.007(6) 0.009(6) Cl1 0.063(2) 0.0733(18) 0.076(2) 0.0193(17) 0.0230(18) 0.0185(17) Cl2 0.087(3) 0.097(3) 0.126(4) -0.015(3) 0.016(3) -0.028(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 Dy1 O3 2.294(5) . ? Dy1 O2 2.303(6) . ? Dy1 O1 2.319(5) . ? Dy1 O4 2.325(5) . ? Dy1 O23 2.406(5) . ? Dy1 O24 2.406(5) . ? Dy1 O21 2.415(5) . ? Dy1 O22 2.467(5) . ? Dy2 O5 2.288(5) . ? Dy2 O6 2.299(6) . ? Dy2 O23 2.300(5) . ? Dy2 O24 2.357(5) . ? Dy2 O7 2.378(5) . ? Dy2 O11 2.438(5) . ? Dy2 N1 2.515(6) . ? Dy2 O25 2.595(5) . ? Dy3 O10 2.272(6) . ? Dy3 O22 2.291(5) . ? Dy3 O9 2.293(6) . ? Dy3 O23 2.336(5) . ? Dy3 O11 2.356(5) . ? Dy3 O15 2.445(6) . ? Dy3 N2 2.478(6) . ? Dy3 O25 2.624(5) . ? Dy4 O13 2.284(5) . ? Dy4 O14 2.295(5) . ? Dy4 O21 2.305(5) . ? Dy4 O22 2.312(5) . ? Dy4 O15 2.383(5) . ? Dy4 O19 2.442(5) . ? Dy4 N3 2.481(7) . ? Dy4 O25 2.542(5) . ? Dy5 O24 2.274(5) . ? Dy5 O17 2.289(6) . ? Dy5 O18 2.294(6) . ? Dy5 O21 2.319(5) . ? Dy5 O19 2.351(6) . ? Dy5 O7 2.431(5) . ? Dy5 N4 2.509(7) . ? Dy5 O25 2.588(5) . ? O21 H21 1.0000 . ? O22 H22 1.0000 . ? O23 H23 1.0000 . ? O24 H24 1.0000 . ? O25 H25 0.9200 . ? O1 C7 1.267(11) . ? O2 C9 1.290(11) . ? O3 C22 1.260(11) . ? O4 C24 1.245(11) . ? O5 C69 1.275(10) . ? O6 C67 1.281(10) . ? O7 C115 1.320(10) . ? O8 C115 1.213(10) . ? O9 C54 1.265(10) . ? O10 C52 1.272(11) . ? O11 C107 1.292(9) . ? O12 C107 1.220(10) . ? O13 C39 1.285(10) . ? O14 C37 1.270(10) . ? O15 C99 1.311(10) . ? O16 C99 1.223(10) . ? O17 C82 1.270(10) . ? O18 C84 1.272(10) . ? O19 C91 1.297(10) . ? O20 C91 1.212(11) . ? N1 C116 1.477(11) . ? N1 H1A 0.9900 . ? N1 H1B 0.9900 . ? N2 C108 1.472(10) . ? N2 H2A 0.9900 . ? N2 H2B 0.9900 . ? N3 C100 1.479(11) . ? N3 H3A 0.9900 . ? N3 H3B 0.9900 . ? N4 C92 1.468(12) . ? N4 H4A 0.9900 . ? N4 H4B 0.9900 . ? C1 C2 1.360(14) . ? C1 C6 1.393(15) . ? C1 H1 0.9500 . ? C2 C3 1.388(16) . ? C2 H2 0.9500 . ? C3 C4 1.390(17) . ? C3 H3 0.9500 . ? C4 C5 1.376(15) . ? C4 H4 0.9500 . ? C5 C6 1.355(14) . ? C5 H5 0.9500 . ? C6 C7 1.486(13) . ? C7 C8 1.415(14) . ? C8 C9 1.389(13) . ? C8 H8 0.9500 . ? C9 C10 1.500(13) . ? C10 C15 1.365(14) . ? C10 C11 1.381(14) . ? C11 C12 1.391(16) . ? C11 H11 0.9500 . ? C12 C13 1.346(17) . ? C12 H12 0.9500 . ? C13 C14 1.380(17) . ? C13 H13 0.9500 . ? C14 C15 1.395(16) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C17 1.3900 . ? C16 C21 1.3900 . ? C16 H16 0.9500 . ? C17 C18 1.3900 . ? C17 H17 0.9500 . ? C18 C19 1.3900 . ? C18 H18 0.9500 . ? C19 C20 1.3900 . ? C19 H19 0.9500 . ? C20 C21 1.3900 . ? C20 H20 0.9500 . ? C21 C22 1.507(11) . ? C22 C23 1.412(13) . ? C23 C24 1.408(14) . ? C23 H23A 0.9500 . ? C24 C25A 1.508(11) . ? C24 C25B 1.54(2) . ? C25A C26A 1.3900 . ? C25A C30A 1.3900 . ? C26A C27A 1.3900 . ? C26A H26A 0.9500 . ? C27A C28A 1.3900 . ? C27A H27A 0.9500 . ? C28A C29A 1.3900 . ? C28A H28A 0.9500 . ? C29A C30A 1.3900 . ? C29A H29A 0.9500 . ? C30A H30A 0.9500 . ? C25B C26B 1.3900 . ? C25B C30B 1.3900 . ? C26B C27B 1.3900 . ? C26B H26B 0.9500 . ? C27B C28B 1.3900 . ? C27B H27B 0.9500 . ? C28B C29B 1.3900 . ? C28B H28B 0.9500 . ? C29B C30B 1.3900 . ? C29B H29B 0.9500 . ? C30B H30B 0.9500 . ? C31 C32 1.374(13) . ? C31 C36 1.394(12) . ? C31 H31 0.9500 . ? C32 C33 1.381(15) . ? C32 H32 0.9500 . ? C33 C34 1.351(15) . ? C33 H33 0.9500 . ? C34 C35 1.364(13) . ? C34 H34 0.9500 . ? C35 C36 1.399(12) . ? C35 H35 0.9500 . ? C36 C37 1.485(11) . ? C37 C38 1.404(11) . ? C38 C39 1.382(11) . ? C38 H38 0.9500 . ? C39 C40 1.491(12) . ? C40 C45 1.365(13) . ? C40 C41 1.400(13) . ? C41 C42 1.375(15) . ? C41 H41 0.9500 . ? C42 C43 1.373(16) . ? C42 H42 0.9500 . ? C43 C44 1.373(15) . ? C43 H43 0.9500 . ? C44 C45 1.403(14) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46 C51 1.378(15) . ? C46 C47 1.399(15) . ? C46 H46 0.9500 . ? C47 C48 1.349(17) . ? C47 H47 0.9500 . ? C48 C49 1.374(18) . ? C48 H48 0.9500 . ? C49 C50 1.397(14) . ? C49 H49 0.9500 . ? C50 C51 1.388(13) . ? C50 H50 0.9500 . ? C51 C52 1.501(13) . ? C52 C53 1.409(16) . ? C53 C54 1.403(14) . ? C53 H53 0.9500 . ? C54 C55 1.495(10) . ? C55 C56 1.3900 . ? C55 C60 1.3900 . ? C56 C57 1.3900 . ? C56 H56A 0.9500 . ? C57 C58 1.3900 . ? C57 H57A 0.9500 . ? C58 C59 1.3900 . ? C58 H58A 0.9500 . ? C59 C60 1.3900 . ? C59 H59A 0.9500 . ? C60 H60A 0.9500 . ? C61 C62 1.370(14) . ? C61 C66 1.385(12) . ? C61 H61 0.9500 . ? C62 C63 1.400(16) . ? C62 H62 0.9500 . ? C63 C64 1.401(16) . ? C63 H63 0.9500 . ? C64 C65 1.389(14) . ? C64 H64 0.9500 . ? C65 C66 1.391(13) . ? C65 H65 0.9500 . ? C66 C67 1.486(12) . ? C67 C68 1.413(11) . ? C68 C69 1.384(11) . ? C68 H68 0.9500 . ? C69 C70 1.503(11) . ? C70 C71 1.376(12) . ? C70 C75 1.392(13) . ? C71 C72 1.386(13) . ? C71 H71 0.9500 . ? C72 C73 1.367(15) . ? C72 H72 0.9500 . ? C73 C74 1.363(15) . ? C73 H73 0.9500 . ? C74 C75 1.386(13) . ? C74 H74 0.9500 . ? C75 H75 0.9500 . ? C76 C77 1.393(14) . ? C76 C81 1.404(13) . ? C76 H76 0.9500 . ? C77 C78 1.365(15) . ? C77 H77 0.9500 . ? C78 C79 1.422(17) . ? C78 H78 0.9500 . ? C79 C80 1.375(16) . ? C79 H79 0.9500 . ? C80 C81 1.390(12) . ? C80 H80 0.9500 . ? C81 C82 1.494(12) . ? C82 C83 1.381(13) . ? C83 C84 1.415(13) . ? C83 H83 0.9500 . ? C84 C85 1.486(12) . ? C85 C86 1.393(13) . ? C85 C90 1.409(13) . ? C86 C87 1.367(14) . ? C86 H86 0.9500 . ? C87 C88 1.395(15) . ? C87 H87 0.9500 . ? C88 C89 1.381(15) . ? C88 H88 0.9500 . ? C89 C90 1.381(14) . ? C89 H89 0.9500 . ? C90 H90 0.9500 . ? C91 C92 1.539(12) . ? C92 C93 1.499(12) . ? C92 H92 1.0000 . ? C93 C98 1.368(13) . ? C93 C94 1.405(13) . ? C94 C95 1.366(14) . ? C94 H94 0.9500 . ? C95 C96 1.384(17) . ? C95 H95 0.9500 . ? C96 C97 1.376(17) . ? C96 H96 0.9500 . ? C97 C98 1.384(16) . ? C97 H97 0.9500 . ? C98 H98 0.9500 . ? C99 C100 1.535(13) . ? C100 C101 1.514(12) . ? C100 H100 1.0000 . ? C101 C102 1.363(13) . ? C101 C106 1.395(14) . ? C102 C103 1.369(14) . ? C102 H102 0.9500 . ? C103 C104 1.354(17) . ? C103 H103 0.9500 . ? C104 C105 1.353(18) . ? C104 H104 0.9500 . ? C105 C106 1.397(16) . ? C105 H105 0.9500 . ? C106 H106 0.9500 . ? C107 C108 1.532(12) . ? C108 C109 1.510(12) . ? C108 H108 1.0000 . ? C109 C114 1.386(12) . ? C109 C110 1.395(13) . ? C110 C111 1.369(14) . ? C110 H110 0.9500 . ? C111 C112 1.380(15) . ? C111 H111 0.9500 . ? C112 C113 1.374(16) . ? C112 H112 0.9500 . ? C113 C114 1.371(15) . ? C113 H113 0.9500 . ? C114 H114 0.9500 . ? C115 C116 1.531(12) . ? C116 C117 1.511(13) . ? C116 H116 1.0000 . ? C117 C122 1.389(12) . ? C117 C118 1.398(13) . ? C118 C119 1.385(15) . ? C118 H118 0.9500 . ? C119 C120 1.380(16) . ? C119 H119 0.9500 . ? C120 C121 1.348(16) . ? C120 H120 0.9500 . ? C121 C122 1.391(15) . ? C121 H121 0.9500 . ? C122 H122 0.9500 . ? C123 Cl2 1.727(14) . ? C123 Cl1 1.747(13) . ? C123 H12A 0.9900 . ? C123 H12B 0.9900 . ? 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 O3 Dy1 O2 120.4(2) . . ? O3 Dy1 O1 75.2(2) . . ? O2 Dy1 O1 73.1(2) . . ? O3 Dy1 O4 73.6(2) . . ? O2 Dy1 O4 78.7(2) . . ? O1 Dy1 O4 117.89(19) . . ? O3 Dy1 O23 148.0(2) . . ? O2 Dy1 O23 74.36(19) . . ? O1 Dy1 O23 136.1(2) . . ? O4 Dy1 O23 83.04(18) . . ? O3 Dy1 O24 136.23(19) . . ? O2 Dy1 O24 81.4(2) . . ? O1 Dy1 O24 76.57(19) . . ? O4 Dy1 O24 150.06(19) . . ? O23 Dy1 O24 70.13(16) . . ? O3 Dy1 O21 74.6(2) . . ? O2 Dy1 O21 147.2(2) . . ? O1 Dy1 O21 84.50(19) . . ? O4 Dy1 O21 133.8(2) . . ? O23 Dy1 O21 109.06(18) . . ? O24 Dy1 O21 70.03(19) . . ? O3 Dy1 O22 81.01(19) . . ? O2 Dy1 O22 137.71(19) . . ? O1 Dy1 O22 148.6(2) . . ? O4 Dy1 O22 73.2(2) . . ? O23 Dy1 O22 71.42(18) . . ? O24 Dy1 O22 108.82(17) . . ? O21 Dy1 O22 69.47(17) . . ? O5 Dy2 O6 73.16(19) . . ? O5 Dy2 O23 106.8(2) . . ? O6 Dy2 O23 86.27(19) . . ? O5 Dy2 O24 69.70(19) . . ? O6 Dy2 O24 129.06(19) . . ? O23 Dy2 O24 72.82(17) . . ? O5 Dy2 O7 91.7(2) . . ? O6 Dy2 O7 140.35(19) . . ? O23 Dy2 O7 133.38(19) . . ? O24 Dy2 O7 74.48(18) . . ? O5 Dy2 O11 157.85(19) . . ? O6 Dy2 O11 85.09(19) . . ? O23 Dy2 O11 75.17(17) . . ? O24 Dy2 O11 130.08(19) . . ? O7 Dy2 O11 102.87(19) . . ? O5 Dy2 N1 88.9(2) . . ? O6 Dy2 N1 77.0(2) . . ? O23 Dy2 N1 152.7(2) . . ? O24 Dy2 N1 134.4(2) . . ? O7 Dy2 N1 66.1(2) . . ? O11 Dy2 N1 82.0(2) . . ? O5 Dy2 O25 135.73(17) . . ? O6 Dy2 O25 145.17(18) . . ? O23 Dy2 O25 68.37(18) . . ? O24 Dy2 O25 66.96(17) . . ? O7 Dy2 O25 68.69(18) . . ? O11 Dy2 O25 66.06(17) . . ? N1 Dy2 O25 115.48(19) . . ? O10 Dy3 O22 84.61(19) . . ? O10 Dy3 O9 74.0(2) . . ? O22 Dy3 O9 120.01(19) . . ? O10 Dy3 O23 121.8(2) . . ? O22 Dy3 O23 75.87(18) . . ? O9 Dy3 O23 70.2(2) . . ? O10 Dy3 O11 142.58(19) . . ? O22 Dy3 O11 132.80(18) . . ? O9 Dy3 O11 84.1(2) . . ? O23 Dy3 O11 76.12(18) . . ? O10 Dy3 O15 91.0(2) . . ? O22 Dy3 O15 73.67(18) . . ? O9 Dy3 O15 157.60(19) . . ? O23 Dy3 O15 132.16(18) . . ? O11 Dy3 O15 99.18(18) . . ? O10 Dy3 N2 78.5(2) . . ? O22 Dy3 N2 148.6(2) . . ? O9 Dy3 N2 80.5(2) . . ? O23 Dy3 N2 135.5(2) . . ? O11 Dy3 N2 68.1(2) . . ? O15 Dy3 N2 80.3(2) . . ? O10 Dy3 O25 148.36(19) . . ? O22 Dy3 O25 67.72(16) . . ? O9 Dy3 O25 132.82(19) . . ? O23 Dy3 O25 67.37(17) . . ? O11 Dy3 O25 66.68(17) . . ? O15 Dy3 O25 67.30(17) . . ? N2 Dy3 O25 117.7(2) . . ? O13 Dy4 O14 74.7(2) . . ? O13 Dy4 O21 109.4(2) . . ? O14 Dy4 O21 82.8(2) . . ? O13 Dy4 O22 73.22(19) . . ? O14 Dy4 O22 130.85(19) . . ? O21 Dy4 O22 74.11(17) . . ? O13 Dy4 O15 92.28(19) . . ? O14 Dy4 O15 142.8(2) . . ? O21 Dy4 O15 134.12(19) . . ? O22 Dy4 O15 74.47(18) . . ? O13 Dy4 O19 152.81(19) . . ? O14 Dy4 O19 79.67(19) . . ? O21 Dy4 O19 75.61(18) . . ? O22 Dy4 O19 132.31(18) . . ? O15 Dy4 O19 103.02(17) . . ? O13 Dy4 N3 83.0(2) . . ? O14 Dy4 N3 77.4(2) . . ? O21 Dy4 N3 153.0(2) . . ? O22 Dy4 N3 132.9(2) . . ? O15 Dy4 N3 66.4(2) . . ? O19 Dy4 N3 82.8(2) . . ? O13 Dy4 O25 141.09(18) . . ? O14 Dy4 O25 139.30(18) . . ? O21 Dy4 O25 68.36(18) . . ? O22 Dy4 O25 68.89(17) . . ? O15 Dy4 O25 69.56(17) . . ? O19 Dy4 O25 66.05(17) . . ? N3 Dy4 O25 117.1(2) . . ? O24 Dy5 O17 116.3(2) . . ? O24 Dy5 O18 82.5(2) . . ? O17 Dy5 O18 74.3(2) . . ? O24 Dy5 O21 74.08(19) . . ? O17 Dy5 O21 71.52(19) . . ? O18 Dy5 O21 123.15(19) . . ? O24 Dy5 O19 132.91(18) . . ? O17 Dy5 O19 88.0(2) . . ? O18 Dy5 O19 144.59(19) . . ? O21 Dy5 O19 77.12(18) . . ? O24 Dy5 O7 74.96(18) . . ? O17 Dy5 O7 155.8(2) . . ? O18 Dy5 O7 86.9(2) . . ? O21 Dy5 O7 132.47(18) . . ? O19 Dy5 O7 99.49(19) . . ? O24 Dy5 N4 152.4(2) . . ? O17 Dy5 N4 79.1(2) . . ? O18 Dy5 N4 80.1(2) . . ? O21 Dy5 N4 133.6(2) . . ? O19 Dy5 N4 66.4(2) . . ? O7 Dy5 N4 82.9(2) . . ? O24 Dy5 O25 68.23(18) . . ? O17 Dy5 O25 135.23(18) . . ? O18 Dy5 O25 145.15(19) . . ? O21 Dy5 O25 67.36(16) . . ? O19 Dy5 O25 66.57(17) . . ? O7 Dy5 O25 68.05(17) . . ? N4 Dy5 O25 118.30(19) . . ? Dy4 O21 Dy5 101.5(2) . . ? Dy4 O21 Dy1 108.80(19) . . ? Dy5 O21 Dy1 106.9(2) . . ? Dy4 O21 H21 113.0 . . ? Dy5 O21 H21 113.0 . . ? Dy1 O21 H21 113.0 . . ? Dy3 O22 Dy4 102.96(19) . . ? Dy3 O22 Dy1 106.0(2) . . ? Dy4 O22 Dy1 106.8(2) . . ? Dy3 O22 H22 113.4 . . ? Dy4 O22 H22 113.4 . . ? Dy1 O22 H22 113.4 . . ? Dy2 O23 Dy3 102.2(2) . . ? Dy2 O23 Dy1 109.2(2) . . ? Dy3 O23 Dy1 106.5(2) . . ? Dy2 O23 H23 112.7 . . ? Dy3 O23 H23 112.7 . . ? Dy1 O23 H23 112.7 . . ? Dy5 O24 Dy2 102.2(2) . . ? Dy5 O24 Dy1 108.7(2) . . ? Dy2 O24 Dy1 107.3(2) . . ? Dy5 O24 H24 112.7 . . ? Dy2 O24 H24 112.7 . . ? Dy1 O24 H24 112.7 . . ? Dy4 O25 Dy5 88.49(16) . . ? Dy4 O25 Dy2 160.5(2) . . ? Dy5 O25 Dy2 88.17(16) . . ? Dy4 O25 Dy3 88.38(16) . . ? Dy5 O25 Dy3 157.7(2) . . ? Dy2 O25 Dy3 87.46(16) . . ? Dy4 O25 H25 98.9 . . ? Dy5 O25 H25 100.6 . . ? Dy2 O25 H25 100.6 . . ? Dy3 O25 H25 101.7 . . ? C7 O1 Dy1 135.4(6) . . ? C9 O2 Dy1 133.9(6) . . ? C22 O3 Dy1 132.7(6) . . ? C24 O4 Dy1 130.4(6) . . ? C69 O5 Dy2 137.4(5) . . ? C67 O6 Dy2 135.4(5) . . ? C115 O7 Dy2 126.8(5) . . ? C115 O7 Dy5 135.6(5) . . ? Dy2 O7 Dy5 97.12(19) . . ? C54 O9 Dy3 137.3(6) . . ? C52 O10 Dy3 136.7(6) . . ? C107 O11 Dy3 124.8(5) . . ? C107 O11 Dy2 137.4(5) . . ? Dy3 O11 Dy2 97.62(18) . . ? C39 O13 Dy4 135.2(5) . . ? C37 O14 Dy4 132.5(5) . . ? C99 O15 Dy4 125.5(5) . . ? C99 O15 Dy3 137.3(5) . . ? Dy4 O15 Dy3 96.49(18) . . ? C82 O17 Dy5 136.6(6) . . ? C84 O18 Dy5 135.3(6) . . ? C91 O19 Dy5 126.8(5) . . ? C91 O19 Dy4 133.8(5) . . ? Dy5 O19 Dy4 96.63(19) . . ? C116 N1 Dy2 117.2(5) . . ? C116 N1 H1A 108.0 . . ? Dy2 N1 H1A 108.0 . . ? C116 N1 H1B 108.0 . . ? Dy2 N1 H1B 108.0 . . ? H1A N1 H1B 107.2 . . ? C108 N2 Dy3 116.7(5) . . ? C108 N2 H2A 108.1 . . ? Dy3 N2 H2A 108.1 . . ? C108 N2 H2B 108.1 . . ? Dy3 N2 H2B 108.1 . . ? H2A N2 H2B 107.3 . . ? C100 N3 Dy4 116.2(5) . . ? C100 N3 H3A 108.2 . . ? Dy4 N3 H3A 108.2 . . ? C100 N3 H3B 108.2 . . ? Dy4 N3 H3B 108.2 . . ? H3A N3 H3B 107.4 . . ? C92 N4 Dy5 117.9(5) . . ? C92 N4 H4A 107.8 . . ? Dy5 N4 H4A 107.8 . . ? C92 N4 H4B 107.8 . . ? Dy5 N4 H4B 107.8 . . ? H4A N4 H4B 107.2 . . ? C2 C1 C6 120.6(10) . . ? C2 C1 H1 119.7 . . ? C6 C1 H1 119.7 . . ? C1 C2 C3 120.7(12) . . ? C1 C2 H2 119.7 . . ? C3 C2 H2 119.7 . . ? C2 C3 C4 118.7(10) . . ? C2 C3 H3 120.7 . . ? C4 C3 H3 120.7 . . ? C5 C4 C3 119.4(11) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? C6 C5 C4 122.0(11) . . ? C6 C5 H5 119.0 . . ? C4 C5 H5 119.0 . . ? C5 C6 C1 118.5(9) . . ? C5 C6 C7 124.8(10) . . ? C1 C6 C7 116.6(9) . . ? O1 C7 C8 121.6(9) . . ? O1 C7 C6 118.8(9) . . ? C8 C7 C6 119.6(9) . . ? C9 C8 C7 126.2(9) . . ? C9 C8 H8 116.9 . . ? C7 C8 H8 116.9 . . ? O2 C9 C8 123.3(9) . . ? O2 C9 C10 115.4(8) . . ? C8 C9 C10 121.3(9) . . ? C15 C10 C11 119.8(10) . . ? C15 C10 C9 118.8(9) . . ? C11 C10 C9 121.3(9) . . ? C10 C11 C12 118.8(11) . . ? C10 C11 H11 120.6 . . ? C12 C11 H11 120.6 . . ? C13 C12 C11 122.3(13) . . ? C13 C12 H12 118.9 . . ? C11 C12 H12 118.9 . . ? C12 C13 C14 118.6(11) . . ? C12 C13 H13 120.7 . . ? C14 C13 H13 120.7 . . ? C13 C14 C15 120.5(11) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C10 C15 C14 119.9(11) . . ? C10 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C17 C16 C21 120.0 . . ? C17 C16 H16 120.0 . . ? C21 C16 H16 120.0 . . ? C18 C17 C16 120.0 . . ? C18 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? C17 C18 C19 120.0 . . ? C17 C18 H18 120.0 . . ? C19 C18 H18 120.0 . . ? C20 C19 C18 120.0 . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C21 C20 C19 120.0 . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C20 C21 C16 120.0 . . ? C20 C21 C22 123.2(6) . . ? C16 C21 C22 116.6(6) . . ? O3 C22 C23 124.0(9) . . ? O3 C22 C21 116.6(8) . . ? C23 C22 C21 119.4(8) . . ? C24 C23 C22 122.6(9) . . ? C24 C23 H23A 118.7 . . ? C22 C23 H23A 118.7 . . ? O4 C24 C23 126.7(9) . . ? O4 C24 C25A 116.9(9) . . ? C23 C24 C25A 116.2(9) . . ? O4 C24 C25B 114.6(16) . . ? C23 C24 C25B 118.7(15) . . ? C26A C25A C30A 120.0 . . ? C26A C25A C24 121.6(8) . . ? C30A C25A C24 118.3(8) . . ? C27A C26A C25A 120.0 . . ? C27A C26A H26A 120.0 . . ? C25A C26A H26A 120.0 . . ? C26A C27A C28A 120.0 . . ? C26A C27A H27A 120.0 . . ? C28A C27A H27A 120.0 . . ? C29A C28A C27A 120.0 . . ? C29A C28A H28A 120.0 . . ? C27A C28A H28A 120.0 . . ? C28A C29A C30A 120.0 . . ? C28A C29A H29A 120.0 . . ? C30A C29A H29A 120.0 . . ? C29A C30A C25A 120.0 . . ? C29A C30A H30A 120.0 . . ? C25A C30A H30A 120.0 . . ? C26B C25B C30B 120.0 . . ? C26B C25B C24 123(2) . . ? C30B C25B C24 117(2) . . ? C27B C26B C25B 120.0 . . ? C27B C26B H26B 120.0 . . ? C25B C26B H26B 120.0 . . ? C26B C27B C28B 120.0 . . ? C26B C27B H27B 120.0 . . ? C28B C27B H27B 120.0 . . ? C27B C28B C29B 120.0 . . ? C27B C28B H28B 120.0 . . ? C29B C28B H28B 120.0 . . ? C30B C29B C28B 120.0 . . ? C30B C29B H29B 120.0 . . ? C28B C29B H29B 120.0 . . ? C29B C30B C25B 120.0 . . ? C29B C30B H30B 120.0 . . ? C25B C30B H30B 120.0 . . ? C32 C31 C36 120.8(9) . . ? C32 C31 H31 119.6 . . ? C36 C31 H31 119.6 . . ? C31 C32 C33 119.7(10) . . ? C31 C32 H32 120.1 . . ? C33 C32 H32 120.1 . . ? C34 C33 C32 120.2(9) . . ? C34 C33 H33 119.9 . . ? C32 C33 H33 119.9 . . ? C33 C34 C35 121.0(10) . . ? C33 C34 H34 119.5 . . ? C35 C34 H34 119.5 . . ? C34 C35 C36 120.5(10) . . ? C34 C35 H35 119.7 . . ? C36 C35 H35 119.7 . . ? C31 C36 C35 117.7(8) . . ? C31 C36 C37 118.5(7) . . ? C35 C36 C37 123.7(8) . . ? O14 C37 C38 125.0(7) . . ? O14 C37 C36 117.0(7) . . ? C38 C37 C36 118.0(7) . . ? C39 C38 C37 125.2(8) . . ? C39 C38 H38 117.4 . . ? C37 C38 H38 117.4 . . ? O13 C39 C38 123.1(8) . . ? O13 C39 C40 116.6(7) . . ? C38 C39 C40 120.2(8) . . ? C45 C40 C41 117.6(9) . . ? C45 C40 C39 119.7(8) . . ? C41 C40 C39 122.7(8) . . ? C42 C41 C40 120.6(10) . . ? C42 C41 H41 119.7 . . ? C40 C41 H41 119.7 . . ? C43 C42 C41 120.9(10) . . ? C43 C42 H42 119.5 . . ? C41 C42 H42 119.5 . . ? C42 C43 C44 119.5(10) . . ? C42 C43 H43 120.2 . . ? C44 C43 H43 120.2 . . ? C43 C44 C45 119.2(10) . . ? C43 C44 H44 120.4 . . ? C45 C44 H44 120.4 . . ? C40 C45 C44 121.9(10) . . ? C40 C45 H45 119.1 . . ? C44 C45 H45 119.1 . . ? C51 C46 C47 120.3(10) . . ? C51 C46 H46 119.9 . . ? C47 C46 H46 119.9 . . ? C48 C47 C46 120.5(12) . . ? C48 C47 H47 119.8 . . ? C46 C47 H47 119.8 . . ? C47 C48 C49 120.4(11) . . ? C47 C48 H48 119.8 . . ? C49 C48 H48 119.8 . . ? C48 C49 C50 119.9(10) . . ? C48 C49 H49 120.1 . . ? C50 C49 H49 120.1 . . ? C51 C50 C49 120.2(11) . . ? C51 C50 H50 119.9 . . ? C49 C50 H50 119.9 . . ? C46 C51 C50 118.8(9) . . ? C46 C51 C52 118.6(9) . . ? C50 C51 C52 122.6(10) . . ? O10 C52 C53 123.4(9) . . ? O10 C52 C51 116.7(9) . . ? C53 C52 C51 119.9(9) . . ? C54 C53 C52 125.1(9) . . ? C54 C53 H53 117.4 . . ? C52 C53 H53 117.4 . . ? O9 C54 C53 122.5(9) . . ? O9 C54 C55 116.2(8) . . ? C53 C54 C55 121.3(8) . . ? C56 C55 C60 120.0 . . ? C56 C55 C54 121.4(5) . . ? C60 C55 C54 118.6(5) . . ? C57 C56 C55 120.0 . . ? C57 C56 H56A 120.0 . . ? C55 C56 H56A 120.0 . . ? C56 C57 C58 120.0 . . ? C56 C57 H57A 120.0 . . ? C58 C57 H57A 120.0 . . ? C59 C58 C57 120.0 . . ? C59 C58 H58A 120.0 . . ? C57 C58 H58A 120.0 . . ? C60 C59 C58 120.0 . . ? C60 C59 H59A 120.0 . . ? C58 C59 H59A 120.0 . . ? C59 C60 C55 120.0 . . ? C59 C60 H60A 120.0 . . ? C55 C60 H60A 120.0 . . ? C62 C61 C66 120.9(10) . . ? C62 C61 H61 119.5 . . ? C66 C61 H61 119.5 . . ? C61 C62 C63 121.7(11) . . ? C61 C62 H62 119.2 . . ? C63 C62 H62 119.2 . . ? C62 C63 C64 118.2(10) . . ? C62 C63 H63 120.9 . . ? C64 C63 H63 120.9 . . ? C65 C64 C63 118.7(10) . . ? C65 C64 H64 120.6 . . ? C63 C64 H64 120.6 . . ? C64 C65 C66 122.9(9) . . ? C64 C65 H65 118.6 . . ? C66 C65 H65 118.6 . . ? C61 C66 C65 117.5(9) . . ? C61 C66 C67 119.1(8) . . ? C65 C66 C67 123.4(8) . . ? O6 C67 C68 124.0(8) . . ? O6 C67 C66 116.8(8) . . ? C68 C67 C66 119.2(8) . . ? C69 C68 C67 123.5(8) . . ? C69 C68 H68 118.2 . . ? C67 C68 H68 118.2 . . ? O5 C69 C68 123.8(8) . . ? O5 C69 C70 115.2(7) . . ? C68 C69 C70 121.0(7) . . ? C71 C70 C75 118.6(8) . . ? C71 C70 C69 118.2(8) . . ? C75 C70 C69 123.1(8) . . ? C70 C71 C72 120.4(9) . . ? C70 C71 H71 119.8 . . ? C72 C71 H71 119.8 . . ? C73 C72 C71 120.4(9) . . ? C73 C72 H72 119.8 . . ? C71 C72 H72 119.8 . . ? C74 C73 C72 120.1(9) . . ? C74 C73 H73 119.9 . . ? C72 C73 H73 119.9 . . ? C73 C74 C75 120.0(10) . . ? C73 C74 H74 120.0 . . ? C75 C74 H74 120.0 . . ? C74 C75 C70 120.5(9) . . ? C74 C75 H75 119.8 . . ? C70 C75 H75 119.8 . . ? C77 C76 C81 121.0(9) . . ? C77 C76 H76 119.5 . . ? C81 C76 H76 119.5 . . ? C78 C77 C76 120.4(11) . . ? C78 C77 H77 119.8 . . ? C76 C77 H77 119.8 . . ? C77 C78 C79 119.8(11) . . ? C77 C78 H78 120.1 . . ? C79 C78 H78 120.1 . . ? C80 C79 C78 118.7(10) . . ? C80 C79 H79 120.6 . . ? C78 C79 H79 120.6 . . ? C79 C80 C81 122.5(10) . . ? C79 C80 H80 118.7 . . ? C81 C80 H80 118.7 . . ? C80 C81 C76 117.5(9) . . ? C80 C81 C82 124.0(9) . . ? C76 C81 C82 118.6(7) . . ? O17 C82 C83 124.0(8) . . ? O17 C82 C81 114.9(8) . . ? C83 C82 C81 121.1(7) . . ? C82 C83 C84 124.4(8) . . ? C82 C83 H83 117.8 . . ? C84 C83 H83 117.8 . . ? O18 C84 C83 124.6(8) . . ? O18 C84 C85 116.2(8) . . ? C83 C84 C85 119.2(7) . . ? C86 C85 C90 117.8(9) . . ? C86 C85 C84 120.8(8) . . ? C90 C85 C84 121.4(9) . . ? C87 C86 C85 121.6(10) . . ? C87 C86 H86 119.2 . . ? C85 C86 H86 119.2 . . ? C86 C87 C88 120.3(10) . . ? C86 C87 H87 119.8 . . ? C88 C87 H87 119.8 . . ? C89 C88 C87 119.2(10) . . ? C89 C88 H88 120.4 . . ? C87 C88 H88 120.4 . . ? C88 C89 C90 120.7(10) . . ? C88 C89 H89 119.7 . . ? C90 C89 H89 119.7 . . ? C89 C90 C85 120.5(10) . . ? C89 C90 H90 119.8 . . ? C85 C90 H90 119.8 . . ? O20 C91 O19 124.3(8) . . ? O20 C91 C92 119.2(8) . . ? O19 C91 C92 116.5(8) . . ? N4 C92 C93 113.8(7) . . ? N4 C92 C91 111.3(7) . . ? C93 C92 C91 108.9(7) . . ? N4 C92 H92 107.5 . . ? C93 C92 H92 107.5 . . ? C91 C92 H92 107.5 . . ? C98 C93 C94 118.0(9) . . ? C98 C93 C92 123.0(9) . . ? C94 C93 C92 119.0(8) . . ? C95 C94 C93 121.0(9) . . ? C95 C94 H94 119.5 . . ? C93 C94 H94 119.5 . . ? C94 C95 C96 119.9(11) . . ? C94 C95 H95 120.0 . . ? C96 C95 H95 120.0 . . ? C97 C96 C95 119.9(11) . . ? C97 C96 H96 120.1 . . ? C95 C96 H96 120.1 . . ? C96 C97 C98 119.7(11) . . ? C96 C97 H97 120.2 . . ? C98 C97 H97 120.2 . . ? C93 C98 C97 121.5(10) . . ? C93 C98 H98 119.3 . . ? C97 C98 H98 119.3 . . ? O16 C99 O15 125.0(8) . . ? O16 C99 C100 119.5(8) . . ? O15 C99 C100 115.5(7) . . ? N3 C100 C101 110.8(7) . . ? N3 C100 C99 110.1(7) . . ? C101 C100 C99 111.5(7) . . ? N3 C100 H100 108.1 . . ? C101 C100 H100 108.1 . . ? C99 C100 H100 108.1 . . ? C102 C101 C106 118.1(9) . . ? C102 C101 C100 123.8(9) . . ? C106 C101 C100 118.1(9) . . ? C101 C102 C103 120.2(10) . . ? C101 C102 H102 119.9 . . ? C103 C102 H102 119.9 . . ? C104 C103 C102 122.6(12) . . ? C104 C103 H103 118.7 . . ? C102 C103 H103 118.7 . . ? C105 C104 C103 118.5(11) . . ? C105 C104 H104 120.8 . . ? C103 C104 H104 120.8 . . ? C104 C105 C106 120.5(11) . . ? C104 C105 H105 119.8 . . ? C106 C105 H105 119.8 . . ? C101 C106 C105 120.2(11) . . ? C101 C106 H106 119.9 . . ? C105 C106 H106 119.9 . . ? O12 C107 O11 122.6(8) . . ? O12 C107 C108 119.3(7) . . ? O11 C107 C108 118.0(7) . . ? N2 C108 C109 111.7(7) . . ? N2 C108 C107 112.4(6) . . ? C109 C108 C107 109.7(7) . . ? N2 C108 H108 107.6 . . ? C109 C108 H108 107.6 . . ? C107 C108 H108 107.6 . . ? C114 C109 C110 118.4(9) . . ? C114 C109 C108 120.7(9) . . ? C110 C109 C108 120.9(8) . . ? C111 C110 C109 121.2(9) . . ? C111 C110 H110 119.4 . . ? C109 C110 H110 119.4 . . ? C110 C111 C112 120.1(10) . . ? C110 C111 H111 120.0 . . ? C112 C111 H111 120.0 . . ? C113 C112 C111 118.8(10) . . ? C113 C112 H112 120.6 . . ? C111 C112 H112 120.6 . . ? C114 C113 C112 121.9(10) . . ? C114 C113 H113 119.0 . . ? C112 C113 H113 119.0 . . ? C113 C114 C109 119.7(11) . . ? C113 C114 H114 120.2 . . ? C109 C114 H114 120.2 . . ? O8 C115 O7 124.5(8) . . ? O8 C115 C116 119.7(7) . . ? O7 C115 C116 115.7(7) . . ? N1 C116 C117 110.3(7) . . ? N1 C116 C115 111.8(7) . . ? C117 C116 C115 111.0(7) . . ? N1 C116 H116 107.9 . . ? C117 C116 H116 107.9 . . ? C115 C116 H116 107.9 . . ? C122 C117 C118 117.2(9) . . ? C122 C117 C116 121.5(8) . . ? C118 C117 C116 121.1(8) . . ? C119 C118 C117 121.7(9) . . ? C119 C118 H118 119.1 . . ? C117 C118 H118 119.1 . . ? C120 C119 C118 119.2(11) . . ? C120 C119 H119 120.4 . . ? C118 C119 H119 120.4 . . ? C121 C120 C119 120.2(11) . . ? C121 C120 H120 119.9 . . ? C119 C120 H120 119.9 . . ? C120 C121 C122 121.2(10) . . ? C120 C121 H121 119.4 . . ? C122 C121 H121 119.4 . . ? C117 C122 C121 120.5(10) . . ? C117 C122 H122 119.8 . . ? C121 C122 H122 119.8 . . ? Cl2 C123 Cl1 111.3(8) . . ? Cl2 C123 H12A 109.4 . . ? Cl1 C123 H12A 109.4 . . ? Cl2 C123 H12B 109.4 . . ? Cl1 C123 H12B 109.4 . . ? H12A C123 H12B 108.0 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A O16 0.99 2.41 3.234(9) 139.8 4_566 N1 H1B O12 0.99 1.98 2.885(9) 151.5 . N2 H2B O16 0.99 2.00 2.905(10) 151.4 . N3 H3B O20 0.99 2.09 2.917(10) 140.0 . N4 H4B O8 0.99 2.03 2.928(10) 150.4 . _refine_diff_density_max 0.592 _refine_diff_density_min -0.693 _refine_diff_density_rms 0.094 _database_code_depnum_ccdc_archive 'CCDC 915211' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2 _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C134 H115 Dy5 N8 O25, 5(C H2 Cl2)' _chemical_formula_sum 'C139 H125 Cl10 Dy5 N8 O25' _chemical_formula_weight 3474.46 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' Dy Dy -0.1892 4.4098 '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' _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_H-M_alt 'P 21 21 21' _space_group_name_Hall 'P 2ac 2ab' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 19.2234(3) _cell_length_b 23.2783(4) _cell_length_c 30.4077(7) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 13607.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 127693 _cell_measurement_theta_min 1.34 _cell_measurement_theta_max 27.18 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.696 _exptl_crystal_F_000 6860 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.480 _exptl_crystal_size_mid 0.350 _exptl_crystal_size_min 0.070 _exptl_absorpt_coefficient_mu 2.982 _shelx_estimated_absorpt_T_min 0.329 _shelx_estimated_absorpt_T_max 0.818 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.2338 _exptl_absorpt_correction_T_max 0.8207 _exptl_absorpt_process_details 'STOE X-RED & X-SHAPE' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Stoe IPDS II' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean 6.667 _diffrn_reflns_number 294120 _diffrn_reflns_av_unetI/netI 0.0874 _diffrn_reflns_av_R_equivalents 0.1159 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.873 _diffrn_reflns_theta_max 25.350 _diffrn_reflns_theta_full 25.250 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_point_group_measured_fraction_full 0.999 _reflns_number_total 24906 _reflns_number_gt 18470 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.856 _reflns_Friedel_fraction_max 1.000 _reflns_Friedel_fraction_full 1.000 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA, PLATON (A.L.Spek, 2005)' _computing_data_reduction 'STOE X-RED, PLATON (A.L.Spek, 2005)' _computing_structure_solution 'SHELXS-2013 (Sheldrick, 2013)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _refine_special_details ; As a result of unresolved twinning of the crystal, it was only possible to refine the Dy atoms with anisotropic thermal parameters. However, the final structure is quite sufficient to demonstrate that the molecule is isostructural with its analogues. Five lattice dichloromethane molecules per Dy5 cluster were badly disordered, and were handled using SQUEEZE (see below). ; # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.401 0.462 0.092 548 244 '5 CH2Cl2 (= 210 e)' 2 0.401 -0.038 0.408 548 245 '5 CH2Cl2 (= 210 e)' 3 -0.099 0.538 0.592 548 244 '5 CH2Cl2 (= 210 e)' 4 0.099 0.038 0.908 548 244 '5 CH2Cl2 (= 210 e)' 5 0.083 0.742 0.032 7 2 ' ' 6 0.094 0.908 0.199 7 2 ' ' 7 0.406 0.092 0.699 7 2 ' ' 8 0.417 0.258 0.532 7 2 ' ' 9 0.583 0.758 0.968 7 2 ' ' 10 0.594 0.592 0.801 7 2 ' ' 11 0.906 0.408 0.301 7 2 ' ' 12 0.917 0.242 0.468 7 2 ' ' _platon_squeeze_details ; Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13 ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.1343P)^2^+21.3540P] 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 x determined using 6873 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons and Flack (2004), Acta Cryst. A60, s61). ; _refine_ls_abs_structure_Flack 0.070(5) _chemical_absolute_configuration rmad _refine_ls_number_reflns 24906 _refine_ls_number_parameters 546 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1072 _refine_ls_R_factor_gt 0.0837 _refine_ls_wR_factor_ref 0.2409 _refine_ls_wR_factor_gt 0.2322 _refine_ls_goodness_of_fit_ref 1.122 _refine_ls_restrained_S_all 1.122 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 0.19289(6) 0.69917(6) 0.32154(4) 0.0447(3) Uani 1 1 d . . . . . Dy2 Dy 0.35736(6) 0.69901(5) 0.25228(4) 0.0414(3) Uani 1 1 d . . . . . Dy3 Dy 0.33263(6) 0.58373(5) 0.32825(4) 0.0425(3) Uani 1 1 d . . . . . Dy4 Dy 0.16918(6) 0.54809(6) 0.27730(4) 0.0472(3) Uani 1 1 d . . . . . Dy5 Dy 0.19749(6) 0.66292(6) 0.19937(4) 0.0467(3) Uani 1 1 d . . . . . O21 O 0.3159(7) 0.6814(6) 0.3221(5) 0.035(3) Uiso 1 1 d . . . . . H21 H 0.3390 0.7020 0.3434 0.042 Uiso 1 1 calc R U . . . O22 O 0.2158(8) 0.5963(7) 0.3347(5) 0.041(4) Uiso 1 1 d . . . . . H22 H 0.1989 0.5839 0.3613 0.049 Uiso 1 1 calc R U . . . O23 O 0.1392(7) 0.6416(6) 0.2634(5) 0.032(3) Uiso 1 1 d . . . . . H23A H 0.0920 0.6471 0.2613 0.038 Uiso 1 1 calc R U . . . O24 O 0.2412(8) 0.7277(7) 0.2495(6) 0.041(4) Uiso 1 1 d . . . . . H24 H 0.2345 0.7657 0.2422 0.050 Uiso 1 1 calc R U . . . O25 O 0.2758(8) 0.6111(7) 0.2546(6) 0.048(4) Uiso 1 1 d . . . . . H25 H 0.2982 0.5862 0.2359 0.058 Uiso 1 1 calc R U . . . C1 C 0.0140(8) 0.8001(10) 0.2319(7) 0.066(8) Uiso 1 1 d G . . . . H1 H 0.0615 0.7937 0.2248 0.080 Uiso 1 1 calc R U . . . C2 C -0.0281(10) 0.8313(10) 0.2035(6) 0.081(10) Uiso 1 1 d G . . . . H2 H -0.0094 0.8463 0.1769 0.098 Uiso 1 1 calc R U . . . C3 C -0.0976(9) 0.8407(9) 0.2139(6) 0.062(8) Uiso 1 1 d G . . . . H3 H -0.1264 0.8620 0.1944 0.075 Uiso 1 1 calc R U . . . C4 C -0.1250(8) 0.8187(10) 0.2527(7) 0.079(9) Uiso 1 1 d G . . . . H4 H -0.1725 0.8251 0.2598 0.095 Uiso 1 1 calc R U . . . C5 C -0.0829(10) 0.7875(10) 0.2811(6) 0.078(10) Uiso 1 1 d G . . . . H5 H -0.1016 0.7725 0.3077 0.093 Uiso 1 1 calc R U . . . C6 C -0.0134(9) 0.7781(9) 0.2707(6) 0.057(7) Uiso 1 1 d G . . . . C7 C 0.0310(15) 0.7366(14) 0.3017(11) 0.062(7) Uiso 1 1 d . . . . . C8 C -0.0018(13) 0.6997(12) 0.3284(9) 0.049(6) Uiso 1 1 d . . . . . H8 H -0.0497 0.6915 0.3238 0.058 Uiso 1 1 calc R U . . . C9 C 0.0342(14) 0.6729(12) 0.3632(9) 0.056(7) Uiso 1 1 d D . . . . C10 C -0.0032(9) 0.6320(8) 0.3957(6) 0.043(6) Uiso 1 1 d DG . . . . C11 C 0.0370(7) 0.6024(10) 0.4261(7) 0.072(9) Uiso 1 1 d G . . . . H11 H 0.0863 0.6051 0.4251 0.087 Uiso 1 1 calc R U . . . C12 C 0.0051(11) 0.5688(10) 0.4581(7) 0.084(11) Uiso 1 1 d G . . . . H12 H 0.0326 0.5485 0.4789 0.101 Uiso 1 1 calc R U . . . C13 C -0.0670(12) 0.5648(10) 0.4595(7) 0.091(11) Uiso 1 1 d G . . . . H13 H -0.0888 0.5418 0.4813 0.109 Uiso 1 1 calc R U . . . C14 C -0.1072(8) 0.5944(11) 0.4290(8) 0.093(12) Uiso 1 1 d G . . . . H14 H -0.1565 0.5917 0.4300 0.112 Uiso 1 1 calc R U . . . C15 C -0.0753(9) 0.6280(9) 0.3971(7) 0.070(9) Uiso 1 1 d G . . . . H15 H -0.1028 0.6483 0.3763 0.084 Uiso 1 1 calc R U . . . C21B C 0.2807(18) 0.7484(16) 0.4579(8) 0.036(9) Uiso 0.6 1 d G . P A 2 C16B C 0.3361(18) 0.7771(15) 0.4774(13) 0.060(12) Uiso 0.6 1 d G . P A 2 H16B H 0.3643 0.8022 0.4604 0.072 Uiso 0.6 1 calc R U P A 2 C17B C 0.3502(18) 0.769(2) 0.5218(13) 0.081(18) Uiso 0.6 1 d G . P A 2 H17B H 0.3881 0.7887 0.5351 0.098 Uiso 0.6 1 calc R U P A 2 C18B C 0.309(2) 0.732(2) 0.5467(8) 0.10(2) Uiso 0.6 1 d G . P A 2 H18B H 0.3187 0.7269 0.5771 0.117 Uiso 0.6 1 calc R U P A 2 C19B C 0.254(2) 0.7037(17) 0.5272(12) 0.082(17) Uiso 0.6 1 d G . P A 2 H19B H 0.2254 0.6786 0.5442 0.099 Uiso 0.6 1 calc R U P A 2 C20B C 0.2395(14) 0.7117(16) 0.4828(12) 0.047(11) Uiso 0.6 1 d G . P A 2 H20B H 0.2016 0.6920 0.4695 0.056 Uiso 0.6 1 calc R U P A 2 C22 C 0.2596(18) 0.7631(16) 0.4097(12) 0.073(9) Uiso 1 1 d . . . . . C23 C 0.2796(19) 0.8123(16) 0.3907(12) 0.079(10) Uiso 1 1 d . . . . . H23 H 0.3137 0.8350 0.4051 0.095 Uiso 1 1 calc R U . . . C24 C 0.2545(17) 0.8306(16) 0.3534(12) 0.072(9) Uiso 1 1 d . . . . . C25A C 0.247(5) 0.902(3) 0.3331(19) 0.19(9) Uiso 0.4 1 d G . P B 2 C26A C 0.261(3) 0.897(2) 0.2884(18) 0.040(18) Uiso 0.4 1 d G . P B 2 H26A H 0.2503 0.8626 0.2735 0.047 Uiso 0.4 1 calc R U P B 2 C27A C 0.289(3) 0.943(3) 0.2656(15) 0.09(3) Uiso 0.4 1 d G . P B 2 H27A H 0.2987 0.9399 0.2350 0.105 Uiso 0.4 1 calc R U P B 2 C28A C 0.304(4) 0.994(2) 0.287(2) 0.10(3) Uiso 0.4 1 d G . P B 2 H28A H 0.3239 1.0257 0.2718 0.124 Uiso 0.4 1 calc R U P B 2 C29A C 0.290(3) 0.999(2) 0.332(2) 0.07(2) Uiso 0.4 1 d G . P B 2 H29A H 0.3005 1.0342 0.3471 0.078 Uiso 0.4 1 calc R U P B 2 C30A C 0.262(5) 0.953(3) 0.3550(16) 0.9(8) Uiso 0.4 1 d G . P B 2 H30A H 0.2521 0.9569 0.3855 1.100 Uiso 0.4 1 calc R U P B 2 C31 C -0.0765(9) 0.5986(10) 0.2686(7) 0.059(7) Uiso 1 1 d G . . . . H31 H -0.0364 0.6136 0.2544 0.070 Uiso 1 1 calc R U . . . C32 C -0.1407(11) 0.6251(8) 0.2627(7) 0.094(12) Uiso 1 1 d G . . . . H32 H -0.1443 0.6582 0.2446 0.112 Uiso 1 1 calc R U . . . C33 C -0.1994(9) 0.6033(9) 0.2834(7) 0.057(7) Uiso 1 1 d G . . . . H33 H -0.2433 0.6214 0.2794 0.069 Uiso 1 1 calc R U . . . C34 C -0.1941(10) 0.5548(10) 0.3099(8) 0.103(13) Uiso 1 1 d G . . . . H34 H -0.2343 0.5399 0.3241 0.124 Uiso 1 1 calc R U . . . C35 C -0.1300(12) 0.5283(9) 0.3158(8) 0.089(11) Uiso 1 1 d G . . . . H35 H -0.1263 0.4952 0.3339 0.107 Uiso 1 1 calc R U . . . C36 C -0.0712(9) 0.5502(10) 0.2951(8) 0.085(10) Uiso 1 1 d G . . . . C37 C 0.0027(12) 0.5288(10) 0.3067(8) 0.041(6) Uiso 1 1 d . . . . . C38 C 0.0173(15) 0.4897(13) 0.3401(10) 0.058(7) Uiso 1 1 d . . . . . H38 H -0.0198 0.4746 0.3572 0.069 Uiso 1 1 calc R U . . . C39 C 0.0821(13) 0.4730(11) 0.3486(9) 0.046(6) Uiso 1 1 d . . . . . C40 C 0.0895(10) 0.4281(8) 0.3884(6) 0.049(6) Uiso 1 1 d G . . . . C41 C 0.1498(9) 0.3951(9) 0.3882(6) 0.061(8) Uiso 1 1 d G . . . . H41 H 0.1838 0.4008 0.3660 0.073 Uiso 1 1 calc R U . . . C42 C 0.1602(10) 0.3537(9) 0.4205(8) 0.087(11) Uiso 1 1 d G . . . . H42 H 0.2014 0.3312 0.4204 0.104 Uiso 1 1 calc R U . . . C43 C 0.1104(12) 0.3453(9) 0.4530(7) 0.088(11) Uiso 1 1 d G . . . . H43 H 0.1175 0.3171 0.4751 0.106 Uiso 1 1 calc R U . . . C44 C 0.0501(11) 0.3783(11) 0.4532(7) 0.079(10) Uiso 1 1 d G . . . . H44 H 0.0161 0.3726 0.4754 0.095 Uiso 1 1 calc R U . . . C45 C 0.0397(9) 0.4197(9) 0.4209(7) 0.083(10) Uiso 1 1 d G . . . . H45 H -0.0015 0.4422 0.4211 0.100 Uiso 1 1 calc R U . . . C46 C 0.3035(10) 0.5561(9) 0.5161(7) 0.061(7) Uiso 1 1 d G . . . . H46 H 0.3442 0.5774 0.5229 0.073 Uiso 1 1 calc R U . . . C47 C 0.2613(13) 0.5355(12) 0.5497(5) 0.134(19) Uiso 1 1 d G . . . . H47 H 0.2732 0.5428 0.5795 0.161 Uiso 1 1 calc R U . . . C48 C 0.2018(12) 0.5042(11) 0.5397(6) 0.094(12) Uiso 1 1 d G . . . . H48 H 0.1730 0.4901 0.5627 0.113 Uiso 1 1 calc R U . . . C49 C 0.1844(9) 0.4936(9) 0.4961(7) 0.061(7) Uiso 1 1 d G . . . . H49 H 0.1437 0.4722 0.4893 0.073 Uiso 1 1 calc R U . . . C50 C 0.2266(10) 0.5142(9) 0.4625(5) 0.062(8) Uiso 1 1 d G . . . . H50 H 0.2147 0.5069 0.4327 0.074 Uiso 1 1 calc R U . . . C51 C 0.2861(9) 0.5454(9) 0.4725(6) 0.055(7) Uiso 1 1 d G . . . . C52 C 0.3319(13) 0.5682(10) 0.4376(8) 0.043(5) Uiso 1 1 d . . . . . C53 C 0.3965(15) 0.5910(13) 0.4404(11) 0.059(7) Uiso 1 1 d . . . . . H53 H 0.4120 0.5972 0.4697 0.070 Uiso 1 1 calc R U . . . C54 C 0.4433(14) 0.6068(13) 0.4091(10) 0.054(7) Uiso 1 1 d . . . . . C55 C 0.5156(8) 0.6244(9) 0.4206(6) 0.075(9) Uiso 1 1 d G . . . . C56 C 0.5652(10) 0.6158(9) 0.3880(5) 0.052(7) Uiso 1 1 d G . . . . H56 H 0.5519 0.6001 0.3604 0.063 Uiso 1 1 calc R U . . . C57 C 0.6344(9) 0.6300(11) 0.3958(6) 0.112(15) Uiso 1 1 d G . . . . H57 H 0.6683 0.6241 0.3736 0.135 Uiso 1 1 calc R U . . . C58 C 0.6539(8) 0.6529(11) 0.4362(7) 0.078(10) Uiso 1 1 d G . . . . H58 H 0.7011 0.6626 0.4416 0.094 Uiso 1 1 calc R U . . . C59 C 0.6042(10) 0.6615(9) 0.4688(6) 0.069(8) Uiso 1 1 d G . . . . H59 H 0.6176 0.6771 0.4964 0.083 Uiso 1 1 calc R U . . . C60 C 0.5351(9) 0.6472(10) 0.4610(6) 0.061(8) Uiso 1 1 d G . . . . H60 H 0.5012 0.6531 0.4833 0.073 Uiso 1 1 calc R U . . . C61 C 0.4598(15) 0.8820(10) 0.3617(10) 0.133(18) Uiso 1 1 d G . . . . H61 H 0.4370 0.9109 0.3450 0.160 Uiso 1 1 calc R U . . . C62 C 0.4882(17) 0.8951(9) 0.4025(10) 0.16(2) Uiso 1 1 d G . . . . H62 H 0.4848 0.9331 0.4137 0.197 Uiso 1 1 calc R U . . . C63 C 0.5215(14) 0.8528(13) 0.4269(7) 0.081(10) Uiso 1 1 d G . . . . H63 H 0.5409 0.8618 0.4547 0.097 Uiso 1 1 calc R U . . . C64 C 0.5264(13) 0.7972(11) 0.4104(8) 0.117(15) Uiso 1 1 d G . . . . H64 H 0.5492 0.7682 0.4270 0.140 Uiso 1 1 calc R U . . . C65 C 0.4980(13) 0.7840(8) 0.3696(8) 0.074(9) Uiso 1 1 d G . . . . H65 H 0.5014 0.7461 0.3583 0.088 Uiso 1 1 calc R U . . . C66 C 0.4647(12) 0.8264(11) 0.3452(7) 0.062(8) Uiso 1 1 d G . . . . C67 C 0.4351(15) 0.8006(15) 0.3037(11) 0.063(7) Uiso 1 1 d . . . . . C68 C 0.4292(19) 0.8464(18) 0.2679(13) 0.085(11) Uiso 1 1 d . . . . . H68 H 0.4409 0.8851 0.2743 0.102 Uiso 1 1 calc R U . . . C69 C 0.4068(11) 0.8315(10) 0.2262(8) 0.038(5) Uiso 1 1 d . . . . . C70 C 0.4048(11) 0.8736(8) 0.1900(5) 0.061(8) Uiso 1 1 d G . . . . C71 C 0.4019(9) 0.8549(7) 0.1466(6) 0.042(6) Uiso 1 1 d G . . . . H71 H 0.3971 0.8151 0.1404 0.051 Uiso 1 1 calc R U . . . C72 C 0.4062(12) 0.8943(9) 0.1124(5) 0.075(9) Uiso 1 1 d G . . . . H72 H 0.4042 0.8815 0.0828 0.090 Uiso 1 1 calc R U . . . C73 C 0.4133(13) 0.9525(8) 0.1215(7) 0.139(19) Uiso 1 1 d G . . . . H73 H 0.4162 0.9795 0.0981 0.167 Uiso 1 1 calc R U . . . C74 C 0.4162(12) 0.9713(6) 0.1649(8) 0.066(8) Uiso 1 1 d G . . . . H74 H 0.4211 1.0111 0.1711 0.079 Uiso 1 1 calc R U . . . C75 C 0.4120(11) 0.9318(8) 0.1991(6) 0.083(10) Uiso 1 1 d G . . . . H75 H 0.4139 0.9447 0.2287 0.100 Uiso 1 1 calc R U . . . C76 C 0.1280(9) 0.8600(8) 0.0918(6) 0.072(9) Uiso 1 1 d G . . . . H76 H 0.0911 0.8411 0.0769 0.086 Uiso 1 1 calc R U . . . C77 C 0.1487(11) 0.9146(8) 0.0786(6) 0.089(11) Uiso 1 1 d G . . . . H77 H 0.1260 0.9330 0.0547 0.107 Uiso 1 1 calc R U . . . C78 C 0.2027(10) 0.9423(7) 0.1005(7) 0.056(7) Uiso 1 1 d G . . . . H78 H 0.2169 0.9796 0.0915 0.068 Uiso 1 1 calc R U . . . C79 C 0.2359(9) 0.9154(8) 0.1355(7) 0.078(9) Uiso 1 1 d G . . . . H79 H 0.2728 0.9343 0.1504 0.094 Uiso 1 1 calc R U . . . C80 C 0.2152(10) 0.8608(8) 0.1486(6) 0.067(8) Uiso 1 1 d G . . . . H80 H 0.2379 0.8424 0.1725 0.081 Uiso 1 1 calc R U . . . C81 C 0.1612(9) 0.8331(6) 0.1268(6) 0.046(6) Uiso 1 1 d G . . . . C82 C 0.1413(16) 0.7771(14) 0.1423(11) 0.063(8) Uiso 1 1 d . . . . . C83 C 0.0807(15) 0.7451(13) 0.1287(11) 0.059(7) Uiso 1 1 d . . . . . H83 H 0.0539 0.7622 0.1060 0.071 Uiso 1 1 calc R U . . . C84 C 0.0581(14) 0.6974(13) 0.1428(9) 0.054(6) Uiso 1 1 d . . . . . C85 C -0.0118(10) 0.6698(8) 0.1257(7) 0.070(8) Uiso 1 1 d G . . . . C86 C -0.0414(12) 0.6879(8) 0.0863(7) 0.087(11) Uiso 1 1 d G . . . . H86 H -0.0245 0.7214 0.0721 0.104 Uiso 1 1 calc R U . . . C87 C -0.0957(12) 0.6568(10) 0.0678(6) 0.093(12) Uiso 1 1 d G . . . . H87 H -0.1159 0.6691 0.0409 0.112 Uiso 1 1 calc R U . . . C88 C -0.1205(10) 0.6077(9) 0.0886(7) 0.069(9) Uiso 1 1 d G . . . . H88 H -0.1576 0.5865 0.0759 0.083 Uiso 1 1 calc R U . . . C89 C -0.0909(10) 0.5897(7) 0.1279(7) 0.066(8) Uiso 1 1 d G . . . . H89 H -0.1078 0.5561 0.1421 0.079 Uiso 1 1 calc R U . . . C90 C -0.0366(9) 0.6207(8) 0.1465(6) 0.052(7) Uiso 1 1 d G . . . . H90 H -0.0164 0.6084 0.1734 0.062 Uiso 1 1 calc R U . . . C91 C 0.3052(19) 0.4468(16) 0.2966(13) 0.080(9) Uiso 1 1 d . . . . . C92 C 0.3598(13) 0.4369(11) 0.3225(9) 0.044(5) Uiso 1 1 d . . . . . H92 H 0.3900 0.4071 0.3084 0.053 Uiso 1 1 calc R U . . . C93 C 0.3323(15) 0.4131(13) 0.3664(9) 0.058(7) Uiso 1 1 d . . . . . H93A H 0.2996 0.4417 0.3789 0.069 Uiso 1 1 calc R U . . . H93B H 0.3051 0.3780 0.3600 0.069 Uiso 1 1 calc R U . . . C94 C 0.3834(14) 0.3989(13) 0.4003(10) 0.056(7) Uiso 1 1 d . . . . . C95 C 0.4226(10) 0.3449(7) 0.4036(7) 0.059(7) Uiso 1 1 d G . . . . C96 C 0.4266(10) 0.2970(9) 0.3764(5) 0.078(9) Uiso 1 1 d G . . . . H96 H 0.4025 0.2966 0.3491 0.093 Uiso 1 1 calc R U . . . C97 C 0.4659(10) 0.2497(7) 0.3891(6) 0.050(6) Uiso 1 1 d G . . . . H97 H 0.4686 0.2169 0.3705 0.060 Uiso 1 1 calc R U . . . C98 C 0.5011(10) 0.2502(8) 0.4290(7) 0.076(9) Uiso 1 1 d G . . . . H98 H 0.5279 0.2179 0.4377 0.092 Uiso 1 1 calc R U . . . C99 C 0.4971(11) 0.2981(10) 0.4562(6) 0.099(12) Uiso 1 1 d G . . . . H99 H 0.5212 0.2984 0.4835 0.118 Uiso 1 1 calc R U . . . C100 C 0.4579(11) 0.3454(8) 0.4435(6) 0.062(8) Uiso 1 1 d G . . . . C101 C 0.398(2) 0.423(2) 0.4395(15) 0.094(12) Uiso 1 1 d . . . . . H101 H 0.3798 0.4592 0.4477 0.113 Uiso 1 1 calc R U . . . C102 C 0.4763(14) 0.5971(12) 0.2602(9) 0.051(7) Uiso 1 1 d . . . . . C103 C 0.5158(12) 0.6443(10) 0.2359(8) 0.040(6) Uiso 1 1 d . . . . . H103 H 0.5435 0.6257 0.2120 0.048 Uiso 1 1 calc R U . . . C104 C 0.5714(15) 0.6776(13) 0.2694(10) 0.057(7) Uiso 1 1 d . . . . . H10A H 0.5447 0.6969 0.2930 0.068 Uiso 1 1 calc R U . . . H10B H 0.6017 0.6485 0.2834 0.068 Uiso 1 1 calc R U . . . C105 C 0.6096(14) 0.7149(12) 0.2503(10) 0.056(7) Uiso 1 1 d . . . . . C106 C 0.6680(8) 0.7069(7) 0.2154(5) 0.042(5) Uiso 1 1 d G . . . . C107 C 0.6907(10) 0.6576(6) 0.1940(7) 0.073(9) Uiso 1 1 d G . . . . H107 H 0.6688 0.6218 0.1997 0.088 Uiso 1 1 calc R U . . . C108 C 0.7454(10) 0.6607(7) 0.1642(7) 0.071(9) Uiso 1 1 d G . . . . H108 H 0.7609 0.6270 0.1496 0.086 Uiso 1 1 calc R U . . . C109 C 0.7774(9) 0.7131(8) 0.1559(6) 0.070(9) Uiso 1 1 d G . . . . H109 H 0.8149 0.7153 0.1355 0.084 Uiso 1 1 calc R U . . . C110 C 0.7547(9) 0.7624(6) 0.1773(7) 0.060(7) Uiso 1 1 d G . . . . H110 H 0.7766 0.7982 0.1716 0.072 Uiso 1 1 calc R U . . . C111 C 0.7000(9) 0.7593(6) 0.2071(6) 0.057(7) Uiso 1 1 d G . . . . C112 C 0.6178(17) 0.7710(15) 0.2526(12) 0.071(8) Uiso 1 1 d . . . . . H112 H 0.5849 0.7929 0.2688 0.085 Uiso 1 1 calc R U . . . C113 C 0.3397(12) 0.6598(11) 0.1433(8) 0.042(5) Uiso 1 1 d . . . . . C114 C 0.2946(17) 0.6559(15) 0.1075(11) 0.069(8) Uiso 1 1 d . . . . . H114 H 0.3105 0.6244 0.0874 0.082 Uiso 1 1 calc R U . . . C115 C 0.2970(14) 0.7145(11) 0.0826(9) 0.049(6) Uiso 1 1 d . . . . . H11A H 0.2793 0.7443 0.1029 0.058 Uiso 1 1 calc R U . . . H11B H 0.3466 0.7236 0.0769 0.058 Uiso 1 1 calc R U . . . C116 C 0.2600(14) 0.7211(12) 0.0412(9) 0.050(6) Uiso 1 1 d . . . . . C117 C 0.2471(12) 0.7738(9) 0.0162(7) 0.091(11) Uiso 1 1 d G . . . . C118 C 0.2635(11) 0.8309(10) 0.0244(6) 0.075(9) Uiso 1 1 d G . . . . H118 H 0.2888 0.8410 0.0502 0.090 Uiso 1 1 calc R U . . . C119 C 0.2430(13) 0.8733(7) -0.0050(8) 0.085(11) Uiso 1 1 d G . . . . H119 H 0.2543 0.9124 0.0006 0.102 Uiso 1 1 calc R U . . . C120 C 0.2060(13) 0.8586(9) -0.0426(7) 0.095(12) Uiso 1 1 d G . . . . H120 H 0.1920 0.8876 -0.0628 0.114 Uiso 1 1 calc R U . . . C121 C 0.1896(11) 0.8014(10) -0.0508(6) 0.075(9) Uiso 1 1 d G . . . . H121 H 0.1643 0.7914 -0.0765 0.090 Uiso 1 1 calc R U . . . C122 C 0.2101(12) 0.7590(7) -0.0214(8) 0.065(8) Uiso 1 1 d G . . . . C123 C 0.233(2) 0.6833(19) 0.0159(14) 0.089(11) Uiso 1 1 d . . . . . H123 H 0.2386 0.6433 0.0212 0.107 Uiso 1 1 calc R U . . . C124 C 0.172(2) 0.5179(19) 0.1737(16) 0.099(12) Uiso 1 1 d . . . . . C125 C 0.1255(17) 0.4751(15) 0.1873(11) 0.071(9) Uiso 1 1 d . . . . . H125 H 0.1395 0.4392 0.1716 0.085 Uiso 1 1 calc R U . . . C126 C 0.039(3) 0.485(3) 0.177(2) 0.135(18) Uiso 1 1 d . . . . . H12A H 0.0183 0.5073 0.2012 0.162 Uiso 1 1 calc R U . . . H12B H 0.0339 0.5076 0.1496 0.162 Uiso 1 1 calc R U . . . C127 C 0.0020(18) 0.4348(16) 0.1723(13) 0.078(9) Uiso 1 1 d . . . . . C128 C 0.0046(10) 0.3968(8) 0.1361(6) 0.075(9) Uiso 1 1 d G . . . . C129 C 0.0497(9) 0.3925(8) 0.1006(7) 0.065(8) Uiso 1 1 d G . . . . H129 H 0.0875 0.4186 0.0978 0.078 Uiso 1 1 calc R U . . . C130 C 0.0397(10) 0.3500(9) 0.0691(6) 0.072(9) Uiso 1 1 d G . . . . H130 H 0.0706 0.3471 0.0448 0.087 Uiso 1 1 calc R U . . . C131 C -0.0155(10) 0.3118(8) 0.0731(6) 0.067(8) Uiso 1 1 d G . . . . H131 H -0.0223 0.2828 0.0516 0.081 Uiso 1 1 calc R U . . . C132 C -0.0606(9) 0.3161(8) 0.1087(6) 0.069(9) Uiso 1 1 d G . . . . H132 H -0.0984 0.2900 0.1114 0.083 Uiso 1 1 calc R U . . . C133 C -0.0506(9) 0.3586(8) 0.1402(5) 0.043(6) Uiso 1 1 d G . . . . C134 C -0.0568(16) 0.4213(15) 0.1970(12) 0.068(8) Uiso 1 1 d . . . . . H134 H -0.0745 0.4409 0.2220 0.082 Uiso 1 1 calc R U . . . N1 N 0.4742(11) 0.6859(10) 0.2165(8) 0.051(5) Uiso 1 1 d . . . . . H1A H 0.4670 0.6757 0.1853 0.062 Uiso 1 1 calc R U . . . H1B H 0.4993 0.7231 0.2173 0.062 Uiso 1 1 calc R U . . . N2 N 0.4030(10) 0.4877(8) 0.3334(7) 0.040(5) Uiso 1 1 d . . . . . H2A H 0.4430 0.4895 0.3129 0.048 Uiso 1 1 calc R U . . . H2B H 0.4216 0.4834 0.3636 0.048 Uiso 1 1 calc R U . . . N3 N 0.1380(13) 0.4648(11) 0.2337(8) 0.062(6) Uiso 1 1 d . . . . . H3A H 0.1758 0.4361 0.2364 0.075 Uiso 1 1 calc R U . . . H3B H 0.0955 0.4476 0.2465 0.075 Uiso 1 1 calc R U . . . N4 N 0.2210(14) 0.6460(13) 0.1201(10) 0.074(8) Uiso 1 1 d . . . . . H4A H 0.2082 0.6059 0.1127 0.089 Uiso 1 1 calc R U . . . H4B H 0.1909 0.6718 0.1025 0.089 Uiso 1 1 calc R U . . . N5 N 0.6698(12) 0.7980(11) 0.2332(8) 0.059(6) Uiso 1 1 d . . . . . H5A H 0.6821 0.8341 0.2368 0.071 Uiso 1 1 calc R U . . . N6 N 0.4411(15) 0.3927(14) 0.4671(11) 0.083(9) Uiso 1 1 d . . . . . H6 H 0.4545 0.4019 0.4939 0.099 Uiso 1 1 calc R U . . . N7 N -0.0855(12) 0.3691(10) 0.1755(8) 0.056(6) Uiso 1 1 d . . . . . H7 H -0.1207 0.3486 0.1853 0.068 Uiso 1 1 calc R U . . . N8 N 0.1970(17) 0.7031(15) -0.0187(11) 0.091(9) Uiso 1 1 d . . . . . H8A H 0.1699 0.6829 -0.0361 0.110 Uiso 1 1 calc R U . . . O1 O 0.0965(8) 0.7447(7) 0.2987(6) 0.046(4) Uiso 1 1 d . . . . . O2 O 0.1022(11) 0.6686(9) 0.3650(7) 0.066(5) Uiso 1 1 d . . . . . O3 O 0.2194(9) 0.7927(8) 0.3228(7) 0.057(5) Uiso 1 1 d . . . . . O4 O 0.2244(9) 0.7221(8) 0.3915(6) 0.053(4) Uiso 1 1 d . . . . . O5 O 0.3716(8) 0.7861(7) 0.2189(6) 0.045(4) Uiso 1 1 d . . . . . O6 O 0.4198(8) 0.7536(8) 0.2988(6) 0.047(4) Uiso 1 1 d . . . . . O7 O 0.3181(8) 0.6647(7) 0.1810(5) 0.044(4) Uiso 1 1 d . . . . . O8 O 0.4051(10) 0.6537(9) 0.1357(7) 0.065(5) Uiso 1 1 d . . . . . O9 O 0.4265(9) 0.6120(8) 0.3700(6) 0.052(4) Uiso 1 1 d . . . . . O10 O 0.3052(10) 0.5660(8) 0.3994(6) 0.057(5) Uiso 1 1 d . . . . . O11 O 0.4157(7) 0.6119(7) 0.2730(5) 0.034(3) Uiso 1 1 d . . . . . O12 O 0.5052(16) 0.5573(14) 0.2734(11) 0.113(10) Uiso 1 1 d . . . . . O13 O 0.1342(10) 0.4875(8) 0.3314(7) 0.057(5) Uiso 1 1 d . . . . . O14 O 0.0506(9) 0.5533(8) 0.2829(6) 0.049(4) Uiso 1 1 d . . . . . O15 O 0.2801(9) 0.5059(8) 0.2925(6) 0.049(4) Uiso 1 1 d . . . . . O16 O 0.2757(10) 0.4090(9) 0.2723(7) 0.063(5) Uiso 1 1 d . . . . . O17 O 0.0890(11) 0.6639(10) 0.1691(8) 0.071(6) Uiso 1 1 d . . . . . O18 O 0.1821(9) 0.7528(8) 0.1732(6) 0.053(4) Uiso 1 1 d . . . . . O19 O 0.1813(8) 0.5610(7) 0.1966(6) 0.049(4) Uiso 1 1 d . . . . . O20 O 0.1678(13) 0.5314(11) 0.1303(8) 0.083(7) Uiso 1 1 d . . . . . C21A C 0.303(6) 0.772(4) 0.465(2) 0.11(4) Uiso 0.4 1 d G . P A 1 C16A C 0.349(5) 0.783(4) 0.499(4) 0.24(11) Uiso 0.4 1 d G . P A 1 H16A H 0.3827 0.8121 0.4964 0.287 Uiso 0.4 1 calc R U P A 1 C17A C 0.345(4) 0.750(4) 0.538(3) 0.07(2) Uiso 0.4 1 d G . P A 1 H17A H 0.3761 0.7579 0.5611 0.088 Uiso 0.4 1 calc R U P A 1 C18A C 0.295(5) 0.707(4) 0.542(2) 0.11(4) Uiso 0.4 1 d G . P A 1 H18A H 0.2926 0.6853 0.5678 0.133 Uiso 0.4 1 calc R U P A 1 C19A C 0.250(4) 0.696(4) 0.507(4) 0.35(19) Uiso 0.4 1 d G . P A 1 H19A H 0.2157 0.6669 0.5098 0.424 Uiso 0.4 1 calc R U P A 1 C20A C 0.254(5) 0.729(4) 0.469(3) 0.07(2) Uiso 0.4 1 d G . P A 1 H20A H 0.2223 0.7210 0.4451 0.089 Uiso 0.4 1 calc R U P A 1 C25B C 0.269(2) 0.8913(11) 0.3322(12) 0.060(13) Uiso 0.6 1 d G . P B 1 C26B C 0.265(2) 0.9049(13) 0.2878(11) 0.18(7) Uiso 0.6 1 d G . P B 1 H26B H 0.2676 0.8753 0.2663 0.217 Uiso 0.6 1 calc R U P B 1 C27B C 0.257(2) 0.9617(15) 0.2748(8) 0.059(12) Uiso 0.6 1 d G . P B 1 H27B H 0.2537 0.9710 0.2445 0.071 Uiso 0.6 1 calc R U P B 1 C28B C 0.2530(17) 1.0050(11) 0.3063(10) 0.057(12) Uiso 0.6 1 d G . P B 1 H28B H 0.2473 1.0438 0.2974 0.069 Uiso 0.6 1 calc R U P B 1 C29B C 0.2574(18) 0.9913(12) 0.3507(9) 0.059(12) Uiso 0.6 1 d G . P B 1 H29B H 0.2548 1.0209 0.3722 0.070 Uiso 0.6 1 calc R U P B 1 C30B C 0.2657(18) 0.9345(14) 0.3636(9) 0.067(14) Uiso 0.6 1 d G . P B 1 H30B H 0.2687 0.9252 0.3940 0.080 Uiso 0.6 1 calc R U P B 1 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 0.0487(6) 0.0484(7) 0.0369(6) -0.0003(6) -0.0012(5) 0.0040(6) Dy2 0.0450(6) 0.0436(6) 0.0355(6) 0.0033(6) -0.0038(5) -0.0013(5) Dy3 0.0468(6) 0.0438(6) 0.0368(6) 0.0036(5) -0.0029(5) -0.0001(5) Dy4 0.0469(6) 0.0483(7) 0.0463(7) -0.0023(6) -0.0019(6) -0.0041(6) Dy5 0.0443(6) 0.0614(8) 0.0344(6) -0.0005(6) -0.0030(5) -0.0037(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 O3 2.236(19) . ? Dy1 O1 2.245(17) . ? Dy1 O4 2.275(19) . ? Dy1 O2 2.30(2) . ? Dy1 O21 2.401(14) . ? Dy1 O23 2.445(14) . ? Dy1 O22 2.467(16) . ? Dy1 O24 2.470(17) . ? Dy2 O6 2.250(18) . ? Dy2 O5 2.285(17) . ? Dy2 O21 2.303(15) . ? Dy2 O24 2.331(15) . ? Dy2 O11 2.402(15) . ? Dy2 O7 2.431(16) . ? Dy2 N1 2.51(2) . ? Dy2 O25 2.579(17) . ? Dy3 O10 2.266(19) . ? Dy3 O22 2.274(15) . ? Dy3 O9 2.303(18) . ? Dy3 O21 2.303(14) . ? Dy3 O15 2.343(18) . ? Dy3 O11 2.408(15) . ? Dy3 O25 2.571(18) . ? Dy3 N2 2.618(19) . ? Dy4 O22 2.259(16) . ? Dy4 O13 2.27(2) . ? Dy4 O14 2.290(17) . ? Dy4 O23 2.291(14) . ? Dy4 O15 2.393(17) . ? Dy4 N3 2.42(3) . ? Dy4 O19 2.483(18) . ? Dy4 O25 2.612(17) . ? Dy5 O18 2.260(18) . ? Dy5 O17 2.28(2) . ? Dy5 O23 2.301(14) . ? Dy5 O24 2.303(17) . ? Dy5 O7 2.385(15) . ? Dy5 O19 2.395(17) . ? Dy5 N4 2.48(3) . ? Dy5 O25 2.558(18) . ? O21 H21 0.9200 . ? O22 H22 0.9200 . ? O23 H23A 0.9200 . ? O24 H24 0.9200 . ? O25 H25 0.9200 . ? C1 C2 1.3900 . ? C1 C6 1.3900 . ? C1 H1 0.9500 . ? C2 C3 1.3900 . ? C2 H2 0.9500 . ? C3 C4 1.3900 . ? C3 H3 0.9500 . ? C4 C5 1.3900 . ? C4 H4 0.9500 . ? C5 C6 1.3900 . ? C5 H5 0.9500 . ? C6 C7 1.60(3) . ? C7 O1 1.28(3) . ? C7 C8 1.34(4) . ? C8 C9 1.41(4) . ? C8 H8 0.9500 . ? C9 O2 1.31(3) . ? C9 C10 1.55(2) . ? C10 C11 1.3900 . ? C10 C15 1.3900 . ? C11 C12 1.3900 . ? C11 H11 0.9500 . ? C12 C13 1.3900 . ? C12 H12 0.9500 . ? C13 C14 1.3900 . ? C13 H13 0.9500 . ? C14 C15 1.3900 . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C21B C16B 1.3900 . ? C21B C20B 1.3900 . ? C21B C22 1.56(4) . ? C16B C17B 1.3900 . ? C16B H16B 0.9500 . ? C17B C18B 1.3900 . ? C17B H17B 0.9500 . ? C18B C19B 1.3900 . ? C18B H18B 0.9500 . ? C19B C20B 1.3900 . ? C19B H19B 0.9500 . ? C20B H20B 0.9500 . ? C22 O4 1.29(4) . ? C22 C23 1.34(5) . ? C22 C21A 1.88(10) . ? C22 C20A 1.97(11) . ? C23 C24 1.30(5) . ? C23 H23 0.9500 . ? C24 O3 1.45(4) . ? C24 C25B 1.58(4) . ? C24 C25A 1.79(7) . ? C25A C26A 1.3900 . ? C25A C30A 1.3900 . ? C26A C27A 1.3900 . ? C26A H26A 0.9500 . ? C27A C28A 1.3900 . ? C27A H27A 0.9500 . ? C28A C29A 1.3900 . ? C28A H28A 0.9500 . ? C29A C30A 1.3900 . ? C29A H29A 0.9500 . ? C30A H30A 0.9500 . ? C31 C32 1.3900 . ? C31 C36 1.3900 . ? C31 H31 0.9500 . ? C32 C33 1.3900 . ? C32 H32 0.9500 . ? C33 C34 1.3900 . ? C33 H33 0.9500 . ? C34 C35 1.3900 . ? C34 H34 0.9500 . ? C35 C36 1.3900 . ? C35 H35 0.9500 . ? C36 C37 1.55(3) . ? C37 O14 1.30(3) . ? C37 C38 1.39(4) . ? C38 C39 1.33(4) . ? C38 H38 0.9500 . ? C39 O13 1.18(3) . ? C39 C40 1.61(3) . ? C40 C41 1.3900 . ? C40 C45 1.3900 . ? C41 C42 1.3900 . ? C41 H41 0.9500 . ? C42 C43 1.3900 . ? C42 H42 0.9500 . ? C43 C44 1.3900 . ? C43 H43 0.9500 . ? C44 C45 1.3900 . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46 C47 1.3900 . ? C46 C51 1.3900 . ? C46 H46 0.9500 . ? C47 C48 1.3900 . ? C47 H47 0.9500 . ? C48 C49 1.3900 . ? C48 H48 0.9500 . ? C49 C50 1.3900 . ? C49 H49 0.9500 . ? C50 C51 1.3900 . ? C50 H50 0.9500 . ? C51 C52 1.48(3) . ? C52 O10 1.27(3) . ? C52 C53 1.35(4) . ? C53 C54 1.36(4) . ? C53 H53 0.9500 . ? C54 O9 1.24(3) . ? C54 C55 1.49(3) . ? C55 C56 1.3900 . ? C55 C60 1.3900 . ? C56 C57 1.3900 . ? C56 H56 0.9500 . ? C57 C58 1.3900 . ? C57 H57 0.9500 . ? C58 C59 1.3900 . ? C58 H58 0.9500 . ? C59 C60 1.3900 . ? C59 H59 0.9500 . ? C60 H60 0.9500 . ? C61 C62 1.3900 . ? C61 C66 1.3900 . ? C61 H61 0.9500 . ? C62 C63 1.3900 . ? C62 H62 0.9500 . ? C63 C64 1.3900 . ? C63 H63 0.9500 . ? C64 C65 1.3900 . ? C64 H64 0.9500 . ? C65 C66 1.3900 . ? C65 H65 0.9500 . ? C66 C67 1.51(4) . ? C67 O6 1.14(3) . ? C67 C68 1.53(5) . ? C68 C69 1.38(5) . ? C68 H68 0.9500 . ? C69 O5 1.27(3) . ? C69 C70 1.48(3) . ? C70 C71 1.3900 . ? C70 C75 1.3900 . ? C71 C72 1.3900 . ? C71 H71 0.9500 . ? C72 C73 1.3900 . ? C72 H72 0.9500 . ? C73 C74 1.3900 . ? C73 H73 0.9500 . ? C74 C75 1.3900 . ? C74 H74 0.9500 . ? C75 H75 0.9500 . ? C76 C77 1.3900 . ? C76 C81 1.3900 . ? C76 H76 0.9500 . ? C77 C78 1.3900 . ? C77 H77 0.9500 . ? C78 C79 1.3900 . ? C78 H78 0.9500 . ? C79 C80 1.3900 . ? C79 H79 0.9500 . ? C80 C81 1.3900 . ? C80 H80 0.9500 . ? C81 C82 1.44(3) . ? C82 O18 1.35(4) . ? C82 C83 1.44(4) . ? C83 C84 1.27(4) . ? C83 H83 0.9500 . ? C84 O17 1.26(3) . ? C84 C85 1.58(3) . ? C85 C86 1.3900 . ? C85 C90 1.3900 . ? C86 C87 1.3900 . ? C86 H86 0.9500 . ? C87 C88 1.3900 . ? C87 H87 0.9500 . ? C88 C89 1.3900 . ? C88 H88 0.9500 . ? C89 C90 1.3900 . ? C89 H89 0.9500 . ? C90 H90 0.9500 . ? C91 O16 1.28(4) . ? C91 C92 1.33(4) . ? C91 O15 1.46(4) . ? C92 N2 1.48(3) . ? C92 C93 1.54(4) . ? C92 H92 1.0000 . ? C93 C94 1.46(4) . ? C93 H93A 0.9900 . ? C93 H93B 0.9900 . ? C94 C101 1.35(5) . ? C94 C95 1.47(3) . ? C95 C96 1.3900 . ? C95 C100 1.3900 . ? C96 C97 1.3900 . ? C96 H96 0.9500 . ? C97 C98 1.3900 . ? C97 H97 0.9500 . ? C98 C99 1.3900 . ? C98 H98 0.9500 . ? C99 C100 1.3900 . ? C99 H99 0.9500 . ? C100 N6 1.35(3) . ? C101 N6 1.37(5) . ? C101 H101 0.9500 . ? C102 O12 1.15(4) . ? C102 O11 1.28(3) . ? C102 C103 1.53(4) . ? C103 N1 1.39(3) . ? C103 C104 1.67(4) . ? C103 H103 1.0000 . ? C104 C105 1.28(4) . ? C104 H10A 0.9900 . ? C104 H10B 0.9900 . ? C105 C112 1.32(4) . ? C105 C106 1.56(3) . ? C106 C107 1.3900 . ? C106 C111 1.3900 . ? C107 C108 1.3900 . ? C107 H107 0.9500 . ? C108 C109 1.3900 . ? C108 H108 0.9500 . ? C109 C110 1.3900 . ? C109 H109 0.9500 . ? C110 C111 1.3900 . ? C110 H110 0.9500 . ? C111 N5 1.33(3) . ? C112 N5 1.32(4) . ? C112 H112 0.9500 . ? C113 O7 1.22(3) . ? C113 O8 1.29(3) . ? C113 C114 1.39(4) . ? C114 N4 1.48(4) . ? C114 C115 1.56(4) . ? C114 H114 1.0000 . ? C115 C116 1.45(4) . ? C115 H11A 0.9900 . ? C115 H11B 0.9900 . ? C116 C123 1.28(5) . ? C116 C117 1.46(3) . ? C117 C118 1.3900 . ? C117 C122 1.3900 . ? C118 C119 1.3900 . ? C118 H118 0.9500 . ? C119 C120 1.3900 . ? C119 H119 0.9500 . ? C120 C121 1.3900 . ? C120 H120 0.9500 . ? C121 C122 1.3900 . ? C121 H121 0.9500 . ? C122 N8 1.33(4) . ? C123 N8 1.34(5) . ? C123 H123 0.9500 . ? C124 O19 1.24(5) . ? C124 O20 1.36(5) . ? C124 C125 1.40(5) . ? C125 N3 1.45(4) . ? C125 C126 1.71(6) . ? C125 H125 1.0000 . ? C126 C127 1.37(6) . ? C126 H12A 0.9900 . ? C126 H12B 0.9900 . ? C127 C134 1.39(5) . ? C127 C128 1.41(4) . ? C128 C129 1.3900 . ? C128 C133 1.3900 . ? C129 C130 1.3900 . ? C129 H129 0.9500 . ? C130 C131 1.3900 . ? C130 H130 0.9500 . ? C131 C132 1.3900 . ? C131 H131 0.9500 . ? C132 C133 1.3900 . ? C132 H132 0.9500 . ? C133 N7 1.29(3) . ? C134 N7 1.49(4) . ? C134 H134 0.9500 . ? N1 H1A 0.9900 . ? N1 H1B 0.9900 . ? N2 H2A 0.9900 . ? N2 H2B 0.9900 . ? N3 H3A 0.9900 . ? N3 H3B 0.9900 . ? N4 H4A 0.9900 . ? N4 H4B 0.9900 . ? N5 H5A 0.8800 . ? N6 H6 0.8800 . ? N7 H7 0.8800 . ? N8 H8A 0.8800 . ? C21A C16A 1.3900 . ? C21A C20A 1.3900 . ? C16A C17A 1.3900 . ? C16A H16A 0.9500 . ? C17A C18A 1.3900 . ? C17A H17A 0.9500 . ? C18A C19A 1.3900 . ? C18A H18A 0.9500 . ? C19A C20A 1.3900 . ? C19A H19A 0.9500 . ? C20A H20A 0.9500 . ? C25B C26B 1.3900 . ? C25B C30B 1.3900 . ? C26B C27B 1.3900 . ? C26B H26B 0.9500 . ? C27B C28B 1.3900 . ? C27B H27B 0.9500 . ? C28B C29B 1.3900 . ? C28B H28B 0.9500 . ? C29B C30B 1.3900 . ? C29B H29B 0.9500 . ? C30B H30B 0.9500 . ? 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 O3 Dy1 O1 74.6(6) . . ? O3 Dy1 O4 72.2(7) . . ? O1 Dy1 O4 113.5(7) . . ? O3 Dy1 O2 117.7(7) . . ? O1 Dy1 O2 72.5(7) . . ? O4 Dy1 O2 74.8(7) . . ? O3 Dy1 O21 86.7(6) . . ? O1 Dy1 O21 153.7(6) . . ? O4 Dy1 O21 76.8(6) . . ? O2 Dy1 O21 133.5(6) . . ? O3 Dy1 O23 129.9(6) . . ? O1 Dy1 O23 71.7(6) . . ? O4 Dy1 O23 156.4(6) . . ? O2 Dy1 O23 85.8(6) . . ? O21 Dy1 O23 109.0(5) . . ? O3 Dy1 O22 154.3(6) . . ? O1 Dy1 O22 130.9(6) . . ? O4 Dy1 O22 91.7(6) . . ? O2 Dy1 O22 75.0(7) . . ? O21 Dy1 O22 69.9(5) . . ? O23 Dy1 O22 70.1(5) . . ? O3 Dy1 O24 70.6(6) . . ? O1 Dy1 O24 84.8(6) . . ? O4 Dy1 O24 131.7(6) . . ? O2 Dy1 O24 151.4(6) . . ? O21 Dy1 O24 71.4(5) . . ? O23 Dy1 O24 70.5(5) . . ? O22 Dy1 O24 109.7(5) . . ? O6 Dy2 O5 73.4(6) . . ? O6 Dy2 O21 72.9(6) . . ? O5 Dy2 O21 127.5(6) . . ? O6 Dy2 O24 111.8(6) . . ? O5 Dy2 O24 81.0(6) . . ? O21 Dy2 O24 75.7(5) . . ? O6 Dy2 O11 93.6(6) . . ? O5 Dy2 O11 144.2(5) . . ? O21 Dy2 O11 76.7(5) . . ? O24 Dy2 O11 134.3(5) . . ? O6 Dy2 O7 155.9(6) . . ? O5 Dy2 O7 86.1(6) . . ? O21 Dy2 O7 131.0(5) . . ? O24 Dy2 O7 76.4(5) . . ? O11 Dy2 O7 95.8(5) . . ? O6 Dy2 N1 82.2(7) . . ? O5 Dy2 N1 79.0(7) . . ? O21 Dy2 N1 133.3(6) . . ? O24 Dy2 N1 151.0(7) . . ? O11 Dy2 N1 66.0(6) . . ? O7 Dy2 N1 81.5(6) . . ? O6 Dy2 O25 139.1(6) . . ? O5 Dy2 O25 142.1(6) . . ? O21 Dy2 O25 67.8(5) . . ? O24 Dy2 O25 69.3(6) . . ? O11 Dy2 O25 66.8(5) . . ? O7 Dy2 O25 64.9(6) . . ? N1 Dy2 O25 117.3(6) . . ? O10 Dy3 O22 73.2(6) . . ? O10 Dy3 O9 73.0(7) . . ? O22 Dy3 O9 133.7(6) . . ? O10 Dy3 O21 103.0(6) . . ? O22 Dy3 O21 75.1(5) . . ? O9 Dy3 O21 82.7(6) . . ? O10 Dy3 O15 101.7(7) . . ? O22 Dy3 O15 73.3(6) . . ? O9 Dy3 O15 144.6(6) . . ? O21 Dy3 O15 131.7(6) . . ? O10 Dy3 O11 150.5(6) . . ? O22 Dy3 O11 132.8(5) . . ? O9 Dy3 O11 77.7(6) . . ? O21 Dy3 O11 76.5(5) . . ? O15 Dy3 O11 99.9(6) . . ? O10 Dy3 O25 141.1(6) . . ? O22 Dy3 O25 67.8(6) . . ? O9 Dy3 O25 137.9(6) . . ? O21 Dy3 O25 68.0(5) . . ? O15 Dy3 O25 66.7(6) . . ? O11 Dy3 O25 66.9(5) . . ? O10 Dy3 N2 84.7(7) . . ? O22 Dy3 N2 128.0(6) . . ? O9 Dy3 N2 78.8(6) . . ? O21 Dy3 N2 156.9(5) . . ? O15 Dy3 N2 65.8(6) . . ? O11 Dy3 N2 86.1(6) . . ? O25 Dy3 N2 118.9(6) . . ? O22 Dy4 O13 82.3(7) . . ? O22 Dy4 O14 108.1(6) . . ? O13 Dy4 O14 71.6(7) . . ? O22 Dy4 O23 76.7(5) . . ? O13 Dy4 O23 130.5(6) . . ? O14 Dy4 O23 73.3(6) . . ? O22 Dy4 O15 72.7(6) . . ? O13 Dy4 O15 82.5(6) . . ? O14 Dy4 O15 153.5(6) . . ? O23 Dy4 O15 130.5(6) . . ? O22 Dy4 N3 156.6(7) . . ? O13 Dy4 N3 80.0(8) . . ? O14 Dy4 N3 80.6(8) . . ? O23 Dy4 N3 126.7(7) . . ? O15 Dy4 N3 89.8(7) . . ? O22 Dy4 O19 131.7(6) . . ? O13 Dy4 O19 145.0(6) . . ? O14 Dy4 O19 99.3(6) . . ? O23 Dy4 O19 74.2(5) . . ? O15 Dy4 O19 99.0(6) . . ? N3 Dy4 O19 65.1(7) . . ? O22 Dy4 O25 67.3(6) . . ? O13 Dy4 O25 140.6(6) . . ? O14 Dy4 O25 140.4(6) . . ? O23 Dy4 O25 67.4(5) . . ? O15 Dy4 O25 65.3(6) . . ? N3 Dy4 O25 119.9(7) . . ? O19 Dy4 O25 66.3(6) . . ? O18 Dy5 O17 74.3(7) . . ? O18 Dy5 O23 115.8(6) . . ? O17 Dy5 O23 84.2(7) . . ? O18 Dy5 O24 71.0(6) . . ? O17 Dy5 O24 126.5(7) . . ? O23 Dy5 O24 76.0(5) . . ? O18 Dy5 O7 91.6(6) . . ? O17 Dy5 O7 142.6(7) . . ? O23 Dy5 O7 132.5(5) . . ? O24 Dy5 O7 77.8(6) . . ? O18 Dy5 O19 152.7(6) . . ? O17 Dy5 O19 82.9(7) . . ? O23 Dy5 O19 75.7(5) . . ? O24 Dy5 O19 136.0(6) . . ? O7 Dy5 O19 97.8(6) . . ? O18 Dy5 N4 80.1(8) . . ? O17 Dy5 N4 77.0(9) . . ? O23 Dy5 N4 151.2(7) . . ? O24 Dy5 N4 132.8(8) . . ? O7 Dy5 N4 66.3(7) . . ? O19 Dy5 N4 80.4(8) . . ? O18 Dy5 O25 138.2(6) . . ? O17 Dy5 O25 143.9(7) . . ? O23 Dy5 O25 68.2(5) . . ? O24 Dy5 O25 70.1(6) . . ? O7 Dy5 O25 65.8(5) . . ? O19 Dy5 O25 68.4(6) . . ? N4 Dy5 O25 117.1(8) . . ? Dy2 O21 Dy3 101.7(6) . . ? Dy2 O21 Dy1 107.7(6) . . ? Dy3 O21 Dy1 108.0(6) . . ? Dy2 O21 H21 112.9 . . ? Dy3 O21 H21 112.9 . . ? Dy1 O21 H21 112.9 . . ? Dy4 O22 Dy3 105.2(6) . . ? Dy4 O22 Dy1 106.6(6) . . ? Dy3 O22 Dy1 106.7(6) . . ? Dy4 O22 H22 112.6 . . ? Dy3 O22 H22 112.6 . . ? Dy1 O22 H22 112.6 . . ? Dy4 O23 Dy5 103.8(6) . . ? Dy4 O23 Dy1 106.4(6) . . ? Dy5 O23 Dy1 106.8(5) . . ? Dy4 O23 H23A 113.1 . . ? Dy5 O23 H23A 113.1 . . ? Dy1 O23 H23A 113.1 . . ? Dy5 O24 Dy2 100.7(6) . . ? Dy5 O24 Dy1 105.9(6) . . ? Dy2 O24 Dy1 104.6(6) . . ? Dy5 O24 H24 114.7 . . ? Dy2 O24 H24 114.7 . . ? Dy1 O24 H24 114.7 . . ? Dy5 O25 Dy3 159.8(8) . . ? Dy5 O25 Dy2 88.0(5) . . ? Dy3 O25 Dy2 87.8(5) . . ? Dy5 O25 Dy4 88.7(5) . . ? Dy3 O25 Dy4 88.0(6) . . ? Dy2 O25 Dy4 158.4(8) . . ? Dy5 O25 H25 99.5 . . ? Dy3 O25 H25 100.7 . . ? Dy2 O25 H25 101.4 . . ? Dy4 O25 H25 100.3 . . ? C2 C1 C6 120.0 . . ? C2 C1 H1 120.0 . . ? C6 C1 H1 120.0 . . ? C3 C2 C1 120.0 . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C4 C3 C2 120.0 . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C4 C5 120.0 . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C4 C5 C6 120.0 . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C5 C6 C1 120.0 . . ? C5 C6 C7 118.3(16) . . ? C1 C6 C7 121.4(16) . . ? O1 C7 C8 127(3) . . ? O1 C7 C6 113(2) . . ? C8 C7 C6 120(2) . . ? C7 C8 C9 120(2) . . ? C7 C8 H8 119.8 . . ? C9 C8 H8 119.8 . . ? O2 C9 C8 124(2) . . ? O2 C9 C10 113(2) . . ? C8 C9 C10 121(2) . . ? C11 C10 C15 120.0 . . ? C11 C10 C9 118.2(16) . . ? C15 C10 C9 121.6(16) . . ? C12 C11 C10 120.0 . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C11 C12 C13 120.0 . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? C12 C13 C14 120.0 . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? C15 C14 C13 120.0 . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C14 C15 C10 120.0 . . ? C14 C15 H15 120.0 . . ? C10 C15 H15 120.0 . . ? C16B C21B C20B 120.0 . . ? C16B C21B C22 120(3) . . ? C20B C21B C22 120(3) . . ? C21B C16B C17B 120.0 . . ? C21B C16B H16B 120.0 . . ? C17B C16B H16B 120.0 . . ? C18B C17B C16B 120.0 . . ? C18B C17B H17B 120.0 . . ? C16B C17B H17B 120.0 . . ? C17B C18B C19B 120.0 . . ? C17B C18B H18B 120.0 . . ? C19B C18B H18B 120.0 . . ? C20B C19B C18B 120.0 . . ? C20B C19B H19B 120.0 . . ? C18B C19B H19B 120.0 . . ? C19B C20B C21B 120.0 . . ? C19B C20B H20B 120.0 . . ? C21B C20B H20B 120.0 . . ? O4 C22 C23 127(3) . . ? O4 C22 C21B 112(3) . . ? C23 C22 C21B 121(3) . . ? O4 C22 C21A 134(4) . . ? C23 C22 C21A 100(4) . . ? O4 C22 C20A 93(3) . . ? C23 C22 C20A 139(4) . . ? C21A C22 C20A 42.3(15) . . ? C24 C23 C22 123(4) . . ? C24 C23 H23 118.4 . . ? C22 C23 H23 118.4 . . ? C23 C24 O3 122(3) . . ? C23 C24 C25B 125(3) . . ? O3 C24 C25B 112(3) . . ? C23 C24 C25A 129(4) . . ? O3 C24 C25A 108(3) . . ? C26A C25A C30A 120.0 . . ? C26A C25A C24 104(4) . . ? C30A C25A C24 128(4) . . ? C27A C26A C25A 120.0 . . ? C27A C26A H26A 120.0 . . ? C25A C26A H26A 120.0 . . ? C26A C27A C28A 120.0 . . ? C26A C27A H27A 120.0 . . ? C28A C27A H27A 120.0 . . ? C27A C28A C29A 120.0 . . ? C27A C28A H28A 120.0 . . ? C29A C28A H28A 120.0 . . ? C30A C29A C28A 120.0 . . ? C30A C29A H29A 120.0 . . ? C28A C29A H29A 120.0 . . ? C29A C30A C25A 120.0 . . ? C29A C30A H30A 120.0 . . ? C25A C30A H30A 120.0 . . ? C32 C31 C36 120.0 . . ? C32 C31 H31 120.0 . . ? C36 C31 H31 120.0 . . ? C31 C32 C33 120.0 . . ? C31 C32 H32 120.0 . . ? C33 C32 H32 120.0 . . ? C34 C33 C32 120.0 . . ? C34 C33 H33 120.0 . . ? C32 C33 H33 120.0 . . ? C33 C34 C35 120.0 . . ? C33 C34 H34 120.0 . . ? C35 C34 H34 120.0 . . ? C36 C35 C34 120.0 . . ? C36 C35 H35 120.0 . . ? C34 C35 H35 120.0 . . ? C35 C36 C31 120.0 . . ? C35 C36 C37 121.7(17) . . ? C31 C36 C37 117.5(17) . . ? O14 C37 C38 123(2) . . ? O14 C37 C36 113(2) . . ? C38 C37 C36 124(2) . . ? C39 C38 C37 121(3) . . ? C39 C38 H38 119.3 . . ? C37 C38 H38 119.3 . . ? O13 C39 C38 129(3) . . ? O13 C39 C40 116(2) . . ? C38 C39 C40 115(2) . . ? C41 C40 C45 120.0 . . ? C41 C40 C39 115.5(15) . . ? C45 C40 C39 124.5(15) . . ? C42 C41 C40 120.0 . . ? C42 C41 H41 120.0 . . ? C40 C41 H41 120.0 . . ? C41 C42 C43 120.0 . . ? C41 C42 H42 120.0 . . ? C43 C42 H42 120.0 . . ? C44 C43 C42 120.0 . . ? C44 C43 H43 120.0 . . ? C42 C43 H43 120.0 . . ? C43 C44 C45 120.0 . . ? C43 C44 H44 120.0 . . ? C45 C44 H44 120.0 . . ? C44 C45 C40 120.0 . . ? C44 C45 H45 120.0 . . ? C40 C45 H45 120.0 . . ? C47 C46 C51 120.0 . . ? C47 C46 H46 120.0 . . ? C51 C46 H46 120.0 . . ? C46 C47 C48 120.0 . . ? C46 C47 H47 120.0 . . ? C48 C47 H47 120.0 . . ? C49 C48 C47 120.0 . . ? C49 C48 H48 120.0 . . ? C47 C48 H48 120.0 . . ? C50 C49 C48 120.0 . . ? C50 C49 H49 120.0 . . ? C48 C49 H49 120.0 . . ? C49 C50 C51 120.0 . . ? C49 C50 H50 120.0 . . ? C51 C50 H50 120.0 . . ? C50 C51 C46 120.0 . . ? C50 C51 C52 121.4(16) . . ? C46 C51 C52 118.6(16) . . ? O10 C52 C53 116(2) . . ? O10 C52 C51 114(2) . . ? C53 C52 C51 130(2) . . ? C52 C53 C54 132(3) . . ? C52 C53 H53 114.1 . . ? C54 C53 H53 114.1 . . ? O9 C54 C53 122(3) . . ? O9 C54 C55 116(2) . . ? C53 C54 C55 122(3) . . ? C56 C55 C60 120.0 . . ? C56 C55 C54 115.6(17) . . ? C60 C55 C54 124.4(17) . . ? C55 C56 C57 120.0 . . ? C55 C56 H56 120.0 . . ? C57 C56 H56 120.0 . . ? C58 C57 C56 120.0 . . ? C58 C57 H57 120.0 . . ? C56 C57 H57 120.0 . . ? C57 C58 C59 120.0 . . ? C57 C58 H58 120.0 . . ? C59 C58 H58 120.0 . . ? C58 C59 C60 120.0 . . ? C58 C59 H59 120.0 . . ? C60 C59 H59 120.0 . . ? C59 C60 C55 120.0 . . ? C59 C60 H60 120.0 . . ? C55 C60 H60 120.0 . . ? C62 C61 C66 120.0 . . ? C62 C61 H61 120.0 . . ? C66 C61 H61 120.0 . . ? C61 C62 C63 120.0 . . ? C61 C62 H62 120.0 . . ? C63 C62 H62 120.0 . . ? C64 C63 C62 120.0 . . ? C64 C63 H63 120.0 . . ? C62 C63 H63 120.0 . . ? C65 C64 C63 120.0 . . ? C65 C64 H64 120.0 . . ? C63 C64 H64 120.0 . . ? C64 C65 C66 120.0 . . ? C64 C65 H65 120.0 . . ? C66 C65 H65 120.0 . . ? C65 C66 C61 120.0 . . ? C65 C66 C67 110(2) . . ? C61 C66 C67 130(2) . . ? O6 C67 C66 126(3) . . ? O6 C67 C68 124(3) . . ? C66 C67 C68 110(3) . . ? C69 C68 C67 120(3) . . ? C69 C68 H68 119.9 . . ? C67 C68 H68 119.9 . . ? O5 C69 C68 122(3) . . ? O5 C69 C70 114(2) . . ? C68 C69 C70 122(3) . . ? C71 C70 C75 120.0 . . ? C71 C70 C69 120.0(16) . . ? C75 C70 C69 119.8(16) . . ? C72 C71 C70 120.0 . . ? C72 C71 H71 120.0 . . ? C70 C71 H71 120.0 . . ? C71 C72 C73 120.0 . . ? C71 C72 H72 120.0 . . ? C73 C72 H72 120.0 . . ? C74 C73 C72 120.0 . . ? C74 C73 H73 120.0 . . ? C72 C73 H73 120.0 . . ? C73 C74 C75 120.0 . . ? C73 C74 H74 120.0 . . ? C75 C74 H74 120.0 . . ? C74 C75 C70 120.0 . . ? C74 C75 H75 120.0 . . ? C70 C75 H75 120.0 . . ? C77 C76 C81 120.0 . . ? C77 C76 H76 120.0 . . ? C81 C76 H76 120.0 . . ? C78 C77 C76 120.0 . . ? C78 C77 H77 120.0 . . ? C76 C77 H77 120.0 . . ? C77 C78 C79 120.0 . . ? C77 C78 H78 120.0 . . ? C79 C78 H78 120.0 . . ? C80 C79 C78 120.0 . . ? C80 C79 H79 120.0 . . ? C78 C79 H79 120.0 . . ? C79 C80 C81 120.0 . . ? C79 C80 H80 120.0 . . ? C81 C80 H80 120.0 . . ? C80 C81 C76 120.0 . . ? C80 C81 C82 117.5(17) . . ? C76 C81 C82 122.5(17) . . ? O18 C82 C81 117(2) . . ? O18 C82 C83 117(3) . . ? C81 C82 C83 126(3) . . ? C84 C83 C82 129(3) . . ? C84 C83 H83 115.4 . . ? C82 C83 H83 115.4 . . ? O17 C84 C83 126(3) . . ? O17 C84 C85 111(2) . . ? C83 C84 C85 122(3) . . ? C86 C85 C90 120.0 . . ? C86 C85 C84 120.7(16) . . ? C90 C85 C84 118.4(17) . . ? C85 C86 C87 120.0 . . ? C85 C86 H86 120.0 . . ? C87 C86 H86 120.0 . . ? C86 C87 C88 120.0 . . ? C86 C87 H87 120.0 . . ? C88 C87 H87 120.0 . . ? C89 C88 C87 120.0 . . ? C89 C88 H88 120.0 . . ? C87 C88 H88 120.0 . . ? C88 C89 C90 120.0 . . ? C88 C89 H89 120.0 . . ? C90 C89 H89 120.0 . . ? C89 C90 C85 120.0 . . ? C89 C90 H90 120.0 . . ? C85 C90 H90 120.0 . . ? O16 C91 C92 125(3) . . ? O16 C91 O15 117(3) . . ? C92 C91 O15 118(3) . . ? C91 C92 N2 116(3) . . ? C91 C92 C93 108(2) . . ? N2 C92 C93 107(2) . . ? C91 C92 H92 108.8 . . ? N2 C92 H92 108.8 . . ? C93 C92 H92 108.8 . . ? C94 C93 C92 117(2) . . ? C94 C93 H93A 107.9 . . ? C92 C93 H93A 107.9 . . ? C94 C93 H93B 107.9 . . ? C92 C93 H93B 107.9 . . ? H93A C93 H93B 107.2 . . ? C101 C94 C93 132(3) . . ? C101 C94 C95 101(3) . . ? C93 C94 C95 126(3) . . ? C96 C95 C100 120.0 . . ? C96 C95 C94 132.3(17) . . ? C100 C95 C94 107.6(17) . . ? C97 C96 C95 120.0 . . ? C97 C96 H96 120.0 . . ? C95 C96 H96 120.0 . . ? C96 C97 C98 120.0 . . ? C96 C97 H97 120.0 . . ? C98 C97 H97 120.0 . . ? C99 C98 C97 120.0 . . ? C99 C98 H98 120.0 . . ? C97 C98 H98 120.0 . . ? C98 C99 C100 120.0 . . ? C98 C99 H99 120.0 . . ? C100 C99 H99 120.0 . . ? N6 C100 C99 129(2) . . ? N6 C100 C95 111(2) . . ? C99 C100 C95 120.0 . . ? C94 C101 N6 117(4) . . ? C94 C101 H101 121.4 . . ? N6 C101 H101 121.4 . . ? O12 C102 O11 123(3) . . ? O12 C102 C103 121(3) . . ? O11 C102 C103 114(2) . . ? N1 C103 C102 115(2) . . ? N1 C103 C104 108(2) . . ? C102 C103 C104 111(2) . . ? N1 C103 H103 107.7 . . ? C102 C103 H103 107.7 . . ? C104 C103 H103 107.7 . . ? C105 C104 C103 114(3) . . ? C105 C104 H10A 108.8 . . ? C103 C104 H10A 108.8 . . ? C105 C104 H10B 108.8 . . ? C103 C104 H10B 108.8 . . ? H10A C104 H10B 107.7 . . ? C104 C105 C112 136(3) . . ? C104 C105 C106 130(3) . . ? C112 C105 C106 94(2) . . ? C107 C106 C111 120.0 . . ? C107 C106 C105 130.2(15) . . ? C111 C106 C105 109.8(15) . . ? C106 C107 C108 120.0 . . ? C106 C107 H107 120.0 . . ? C108 C107 H107 120.0 . . ? C109 C108 C107 120.0 . . ? C109 C108 H108 120.0 . . ? C107 C108 H108 120.0 . . ? C108 C109 C110 120.0 . . ? C108 C109 H109 120.0 . . ? C110 C109 H109 120.0 . . ? C111 C110 C109 120.0 . . ? C111 C110 H110 120.0 . . ? C109 C110 H110 120.0 . . ? N5 C111 C110 133.0(16) . . ? N5 C111 C106 106.9(16) . . ? C110 C111 C106 120.0 . . ? C105 C112 N5 123(3) . . ? C105 C112 H112 118.7 . . ? N5 C112 H112 118.7 . . ? O7 C113 O8 121(2) . . ? O7 C113 C114 122(2) . . ? O8 C113 C114 117(2) . . ? C113 C114 N4 114(3) . . ? C113 C114 C115 108(3) . . ? N4 C114 C115 107(3) . . ? C113 C114 H114 109.5 . . ? N4 C114 H114 109.5 . . ? C115 C114 H114 109.5 . . ? C116 C115 C114 120(2) . . ? C116 C115 H11A 107.4 . . ? C114 C115 H11A 107.4 . . ? C116 C115 H11B 107.4 . . ? C114 C115 H11B 107.4 . . ? H11A C115 H11B 106.9 . . ? C123 C116 C115 130(3) . . ? C123 C116 C117 101(3) . . ? C115 C116 C117 128(2) . . ? C118 C117 C122 120.0 . . ? C118 C117 C116 132.1(19) . . ? C122 C117 C116 107.9(19) . . ? C119 C118 C117 120.0 . . ? C119 C118 H118 120.0 . . ? C117 C118 H118 120.0 . . ? C120 C119 C118 120.0 . . ? C120 C119 H119 120.0 . . ? C118 C119 H119 120.0 . . ? C119 C120 C121 120.0 . . ? C119 C120 H120 120.0 . . ? C121 C120 H120 120.0 . . ? C122 C121 C120 120.0 . . ? C122 C121 H121 120.0 . . ? C120 C121 H121 120.0 . . ? N8 C122 C121 133(2) . . ? N8 C122 C117 107(2) . . ? C121 C122 C117 120.0 . . ? C116 C123 N8 116(4) . . ? C116 C123 H123 121.8 . . ? N8 C123 H123 121.8 . . ? O19 C124 O20 112(4) . . ? O19 C124 C125 120(4) . . ? O20 C124 C125 115(4) . . ? C124 C125 N3 108(3) . . ? C124 C125 C126 118(4) . . ? N3 C125 C126 111(3) . . ? C124 C125 H125 106.5 . . ? N3 C125 H125 106.5 . . ? C126 C125 H125 106.5 . . ? C127 C126 C125 114(4) . . ? C127 C126 H12A 108.7 . . ? C125 C126 H12A 108.7 . . ? C127 C126 H12B 108.7 . . ? C125 C126 H12B 108.7 . . ? H12A C126 H12B 107.6 . . ? C126 C127 C134 124(4) . . ? C126 C127 C128 126(4) . . ? C134 C127 C128 108(3) . . ? C129 C128 C133 120.0 . . ? C129 C128 C127 132.2(19) . . ? C133 C128 C127 107.8(19) . . ? C130 C129 C128 120.0 . . ? C130 C129 H129 120.0 . . ? C128 C129 H129 120.0 . . ? C129 C130 C131 120.0 . . ? C129 C130 H130 120.0 . . ? C131 C130 H130 120.0 . . ? C130 C131 C132 120.0 . . ? C130 C131 H131 120.0 . . ? C132 C131 H131 120.0 . . ? C133 C132 C131 120.0 . . ? C133 C132 H132 120.0 . . ? C131 C132 H132 120.0 . . ? N7 C133 C132 129.6(16) . . ? N7 C133 C128 110.4(16) . . ? C132 C133 C128 120.0 . . ? C127 C134 N7 104(3) . . ? C127 C134 H134 127.8 . . ? N7 C134 H134 127.8 . . ? C103 N1 Dy2 114.6(16) . . ? C103 N1 H1A 108.6 . . ? Dy2 N1 H1A 108.6 . . ? C103 N1 H1B 108.6 . . ? Dy2 N1 H1B 108.6 . . ? H1A N1 H1B 107.6 . . ? C92 N2 Dy3 112.3(13) . . ? C92 N2 H2A 109.2 . . ? Dy3 N2 H2A 109.2 . . ? C92 N2 H2B 109.2 . . ? Dy3 N2 H2B 109.2 . . ? H2A N2 H2B 107.9 . . ? C125 N3 Dy4 116(2) . . ? C125 N3 H3A 108.2 . . ? Dy4 N3 H3A 108.2 . . ? C125 N3 H3B 108.2 . . ? Dy4 N3 H3B 108.2 . . ? H3A N3 H3B 107.4 . . ? C114 N4 Dy5 113(2) . . ? C114 N4 H4A 108.9 . . ? Dy5 N4 H4A 108.9 . . ? C114 N4 H4B 108.9 . . ? Dy5 N4 H4B 108.9 . . ? H4A N4 H4B 107.7 . . ? C112 N5 C111 106(2) . . ? C112 N5 H5A 127.1 . . ? C111 N5 H5A 127.1 . . ? C100 N6 C101 104(3) . . ? C100 N6 H6 128.2 . . ? C101 N6 H6 128.2 . . ? C133 N7 C134 109(2) . . ? C133 N7 H7 125.4 . . ? C134 N7 H7 125.4 . . ? C122 N8 C123 107(3) . . ? C122 N8 H8A 126.7 . . ? C123 N8 H8A 126.7 . . ? C7 O1 Dy1 136.3(19) . . ? C9 O2 Dy1 134.8(17) . . ? C24 O3 Dy1 135.3(19) . . ? C22 O4 Dy1 135(2) . . ? C69 O5 Dy2 136.2(16) . . ? C67 O6 Dy2 140(2) . . ? C113 O7 Dy5 123.2(15) . . ? C113 O7 Dy2 139.5(15) . . ? Dy5 O7 Dy2 95.6(6) . . ? C54 O9 Dy3 134.9(18) . . ? C52 O10 Dy3 140.4(17) . . ? C102 O11 Dy2 125.0(16) . . ? C102 O11 Dy3 138.2(16) . . ? Dy2 O11 Dy3 95.9(5) . . ? C39 O13 Dy4 138.7(19) . . ? C37 O14 Dy4 136.3(16) . . ? C91 O15 Dy3 123.0(18) . . ? C91 O15 Dy4 134.2(18) . . ? Dy3 O15 Dy4 99.0(7) . . ? C84 O17 Dy5 133.7(19) . . ? C82 O18 Dy5 135.3(17) . . ? C124 O19 Dy5 147(3) . . ? C124 O19 Dy4 116(2) . . ? Dy5 O19 Dy4 95.6(6) . . ? C16A C21A C20A 120.0 . . ? C16A C21A C22 166(6) . . ? C20A C21A C22 72(7) . . ? C17A C16A C21A 120.00(7) . . ? C17A C16A H16A 120.0 . . ? C21A C16A H16A 120.0 . . ? C16A C17A C18A 120.00(5) . . ? C16A C17A H17A 120.0 . . ? C18A C17A H17A 120.0 . . ? C19A C18A C17A 120.0 . . ? C19A C18A H18A 120.0 . . ? C17A C18A H18A 120.0 . . ? C18A C19A C20A 120.0 . . ? C18A C19A H19A 120.0 . . ? C20A C19A H19A 120.0 . . ? C19A C20A C21A 120.0 . . ? C19A C20A C22 172(5) . . ? C21A C20A C22 65(6) . . ? C19A C20A H20A 120.0 . . ? C21A C20A H20A 120.0 . . ? C22 C20A H20A 55.0 . . ? C26B C25B C30B 120.0 . . ? C26B C25B C24 126(3) . . ? C30B C25B C24 111(3) . . ? C27B C26B C25B 120.0 . . ? C27B C26B H26B 120.0 . . ? C25B C26B H26B 120.0 . . ? C26B C27B C28B 120.0 . . ? C26B C27B H27B 120.0 . . ? C28B C27B H27B 120.0 . . ? C29B C28B C27B 120.0 . . ? C29B C28B H28B 120.0 . . ? C27B C28B H28B 120.0 . . ? C28B C29B C30B 120.0 . . ? C28B C29B H29B 120.0 . . ? C30B C29B H29B 120.0 . . ? C29B C30B C25B 120.0 . . ? C29B C30B H30B 120.0 . . ? C25B C30B H30B 120.0 . . ? _refine_diff_density_max 1.840 _refine_diff_density_min -1.980 _refine_diff_density_rms 0.213 _database_code_depnum_ccdc_archive 'CCDC 915212' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_3 _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C110 H103 Dy5 N4 O25, 3(C H2 Cl2), C H4 O' _chemical_formula_sum 'C114 H113 Cl6 Dy5 N4 O26' _chemical_formula_weight 2980.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_H-M_alt 'P 21 21 21' _space_group_name_Hall 'P 2ac 2ab' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 17.1242(6) _cell_length_b 20.0781(4) _cell_length_c 32.8693(7) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 11301.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 81777 _cell_measurement_theta_min 1.19 _cell_measurement_theta_max 25.23 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.752 _exptl_crystal_F_000 5860 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.490 _exptl_crystal_size_mid 0.480 _exptl_crystal_size_min 0.440 _exptl_absorpt_coefficient_mu 3.482 _shelx_estimated_absorpt_T_min 0.280 _shelx_estimated_absorpt_T_max 0.310 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.221 _exptl_absorpt_correction_T_max 0.385 _exptl_absorpt_process_details 'STOE X-RED & X-SHAPE' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean 6.667 _diffrn_reflns_number 83418 _diffrn_reflns_av_unetI/netI 0.0645 _diffrn_reflns_av_R_equivalents 0.0938 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 1.188 _diffrn_reflns_theta_max 25.070 _diffrn_reflns_theta_full 25.250 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measured_fraction_theta_full 0.976 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_Laue_measured_fraction_full 0.976 _diffrn_reflns_point_group_measured_fraction_max 0.992 _diffrn_reflns_point_group_measured_fraction_full 0.973 _reflns_number_total 19908 _reflns_number_gt 17006 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.838 _reflns_Friedel_fraction_max 0.989 _reflns_Friedel_fraction_full 0.969 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA, PLATON (A.L.Spek, 2005)' _computing_data_reduction 'STOE X-RED, PLATON (A.L.Spek, 2005)' _computing_structure_solution 'SHELXS-2013 (Sheldrick, 2013)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _refine_special_details ; One of the three lattice CH2Cl2 per formula unit was badly disordered and was handled using the SQUEEZE option in PLATON (see below). The carbon atoms of one Ph2acac ligand (and one phenyl ring in particular) refined with strongly anisotropic thermal parameters. Attempts to refine this ligand using split carbon atoms were unsatisfactory, and it seems that this ligand is better described as undergoing high thermal motion, rather than being disordered over two positions. The carbons were refined using rigid-body and similarity restraints on their anisotropic thermal parameters. ; # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.148 0.627 0.271 155 46 'CH2Cl2 (= 42 e)' 2 0.148 0.127 0.229 155 46 'CH2Cl2 (= 42 e)' 3 0.352 0.873 0.729 155 46 'CH2Cl2 (= 42 e)' 4 0.648 0.373 0.771 155 46 'CH2Cl2 (= 42 e)' _platon_squeeze_details ; Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13 ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0484P)^2^] 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 x determined using 7035 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons and Flack (2004), Acta Cryst. A60, s61). ; _refine_ls_abs_structure_Flack 0.005(7) _chemical_absolute_configuration rmad _refine_ls_number_reflns 19908 _refine_ls_number_parameters 1371 _refine_ls_number_restraints 139 _refine_ls_R_factor_all 0.0465 _refine_ls_R_factor_gt 0.0390 _refine_ls_wR_factor_ref 0.0901 _refine_ls_wR_factor_gt 0.0876 _refine_ls_goodness_of_fit_ref 0.966 _refine_ls_restrained_S_all 0.964 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 0.37695(3) 0.43151(2) 0.44085(2) 0.03493(13) Uani 1 1 d . . . . . Dy2 Dy 0.18178(3) 0.52212(2) 0.43232(2) 0.03143(12) Uani 1 1 d . . . . . Dy3 Dy 0.31699(3) 0.57560(2) 0.50939(2) 0.03249(12) Uani 1 1 d . . . . . Dy4 Dy 0.46300(3) 0.60716(3) 0.43312(2) 0.03319(12) Uani 1 1 d . . . . . Dy5 Dy 0.32779(3) 0.55279(3) 0.35541(2) 0.03732(13) Uani 1 1 d . . . . . O21 O 0.2777(4) 0.4677(4) 0.3941(2) 0.0328(17) Uani 1 1 d . . . . . H21 H 0.2562 0.4305 0.3773 0.039 Uiso 1 1 calc R U . . . O22 O 0.4311(4) 0.5149(4) 0.3948(2) 0.0348(17) Uani 1 1 d . . . . . H22 H 0.4758 0.4978 0.3782 0.042 Uiso 1 1 calc R U . . . O23 O 0.4257(4) 0.5258(4) 0.4791(2) 0.0339(17) Uani 1 1 d . . . . . H23 H 0.4677 0.5137 0.4989 0.041 Uiso 1 1 calc R U . . . O24 O 0.2683(4) 0.4799(3) 0.4796(2) 0.0295(16) Uani 1 1 d . . . . . H24 H 0.2439 0.4483 0.4993 0.035 Uiso 1 1 calc R U . . . O25 O 0.3132(4) 0.5838(3) 0.4314(2) 0.0317(15) Uani 1 1 d . . . . . H25 H 0.2926 0.6302 0.4283 0.038 Uiso 1 1 calc R U . . . O1 O 0.4148(5) 0.3707(4) 0.3836(3) 0.046(2) Uani 1 1 d . . . . . O2 O 0.5086(5) 0.4074(4) 0.4487(3) 0.048(2) Uani 1 1 d . . . . . O3 O 0.3737(5) 0.3772(4) 0.5036(2) 0.0430(19) Uani 1 1 d . . . . . O4 O 0.2896(4) 0.3437(4) 0.4342(3) 0.0447(19) Uani 1 1 d . . . . . O5 O 0.1130(4) 0.4434(4) 0.4667(2) 0.0362(17) Uani 1 1 d . . . . . O6 O 0.1088(5) 0.4658(4) 0.3855(2) 0.0421(19) Uani 1 1 d . . . . . O7 O 0.1996(4) 0.5924(4) 0.3730(2) 0.0330(17) Uani 1 1 d . . . . . O8 O 0.0896(5) 0.6486(5) 0.3622(3) 0.049(2) Uani 1 1 d . . . . . O9 O 0.4010(4) 0.5471(4) 0.5604(2) 0.0425(19) Uani 1 1 d . . . . . O10 O 0.2416(4) 0.5363(4) 0.5614(2) 0.0393(18) Uani 1 1 d . . . . . O11 O 0.1888(4) 0.6060(3) 0.4839(2) 0.0315(15) Uani 1 1 d . . . . . O12 O 0.1344(5) 0.6749(5) 0.5292(3) 0.054(2) Uani 1 1 d . . . . . O13 O 0.5773(4) 0.5687(4) 0.4057(2) 0.0420(19) Uani 1 1 d . . . . . O14 O 0.5582(4) 0.6257(4) 0.4808(2) 0.0402(19) Uani 1 1 d . . . . . O15 O 0.3888(4) 0.6668(3) 0.4824(2) 0.0334(17) Uani 1 1 d . . . . . O16 O 0.4281(5) 0.7732(4) 0.4828(3) 0.049(2) Uani 1 1 d . . . . . O17 O 0.2856(6) 0.4734(5) 0.3110(2) 0.059(2) Uani 1 1 d . U . . . O18 O 0.4247(5) 0.5406(6) 0.3067(3) 0.061(3) Uani 1 1 d . U . . . O19 O 0.3997(5) 0.6521(4) 0.3734(2) 0.0429(19) Uani 1 1 d . . . . . O20 O 0.3742(6) 0.7323(5) 0.3297(3) 0.065(3) Uani 1 1 d . . . . . N1 N 0.0557(5) 0.5874(4) 0.4412(3) 0.037(2) Uani 1 1 d . . . . . H1 H 0.0570 0.6237 0.4204 0.044 Uiso 1 1 calc R U . . . N2 N 0.2957(6) 0.6807(5) 0.5486(3) 0.040(2) Uani 1 1 d . . . . . H2 H 0.2377 0.6869 0.5486 0.048 Uiso 1 1 calc R U . . . N3 N 0.5136(5) 0.7205(4) 0.4117(3) 0.038(2) Uani 1 1 d . . . . . H3 H 0.5209 0.7468 0.4373 0.046 Uiso 1 1 calc R U . . . N4 N 0.2668(6) 0.6311(5) 0.3021(3) 0.043(2) Uani 1 1 d . . . . . H4 H 0.2993 0.6725 0.3030 0.052 Uiso 1 1 calc R U . . . C1 C 0.5364(12) 0.2989(10) 0.3051(6) 0.096(6) Uani 1 1 d . . . . . H1A H 0.5878 0.3097 0.3137 0.115 Uiso 1 1 calc R U . . . C2 C 0.5233(16) 0.2613(12) 0.2682(6) 0.112(8) Uani 1 1 d . . . . . H2A H 0.5668 0.2452 0.2532 0.135 Uiso 1 1 calc R U . . . C3 C 0.4464(14) 0.2480(9) 0.2539(6) 0.090(6) Uani 1 1 d . . . . . H3A H 0.4382 0.2238 0.2295 0.108 Uiso 1 1 calc R U . . . C4 C 0.3873(13) 0.2698(8) 0.2751(6) 0.088(5) Uani 1 1 d . . . . . H4A H 0.3358 0.2641 0.2651 0.105 Uiso 1 1 calc R U . . . C5 C 0.3992(12) 0.3017(9) 0.3127(5) 0.090(6) Uani 1 1 d . . . . . H5 H 0.3549 0.3121 0.3289 0.108 Uiso 1 1 calc R U . . . C6 C 0.4727(9) 0.3185(6) 0.3273(4) 0.056(4) Uani 1 1 d . . . . . C7 C 0.4803(8) 0.3553(6) 0.3671(4) 0.049(3) Uani 1 1 d . . . . . C8 C 0.5511(10) 0.3685(7) 0.3842(4) 0.059(4) Uani 1 1 d . . . . . H8 H 0.5958 0.3632 0.3674 0.070 Uiso 1 1 calc R U . . . C9 C 0.5635(7) 0.3890(6) 0.4240(4) 0.051(3) Uani 1 1 d . . . . . C10 C 0.6436(8) 0.3905(7) 0.4424(5) 0.061(4) Uani 1 1 d . . . . . C11 C 0.6591(8) 0.4298(7) 0.4759(5) 0.063(4) Uani 1 1 d . . . . . H11 H 0.6182 0.4553 0.4877 0.076 Uiso 1 1 calc R U . . . C12 C 0.7329(10) 0.4327(8) 0.4927(6) 0.081(5) Uani 1 1 d . . . . . H12 H 0.7434 0.4621 0.5147 0.097 Uiso 1 1 calc R U . . . C13 C 0.7919(8) 0.3921(8) 0.4772(6) 0.077(5) Uani 1 1 d . . . . . H13 H 0.8422 0.3920 0.4893 0.092 Uiso 1 1 calc R U . . . C14 C 0.7768(11) 0.3532(9) 0.4448(7) 0.092(6) Uani 1 1 d . . . . . H14 H 0.8174 0.3261 0.4342 0.110 Uiso 1 1 calc R U . . . C15 C 0.7027(8) 0.3513(8) 0.4263(6) 0.079(5) Uani 1 1 d . . . . . H15 H 0.6934 0.3238 0.4033 0.095 Uiso 1 1 calc R U . . . C16 C 0.2645(9) 0.3180(7) 0.5896(4) 0.061(4) Uani 1 1 d . . . . . H16 H 0.2145 0.3149 0.5772 0.073 Uiso 1 1 calc R U . . . C17 C 0.2717(12) 0.3074(9) 0.6317(5) 0.081(5) Uani 1 1 d . . . . . H17 H 0.2265 0.2992 0.6476 0.097 Uiso 1 1 calc R U . . . C18 C 0.3421(12) 0.3088(9) 0.6494(5) 0.086(5) Uani 1 1 d . . . . . H18 H 0.3480 0.2995 0.6775 0.103 Uiso 1 1 calc R U . . . C19 C 0.4058(12) 0.3241(10) 0.6256(5) 0.086(6) Uani 1 1 d . . . . . H19 H 0.4560 0.3255 0.6379 0.103 Uiso 1 1 calc R U . . . C20 C 0.3998(9) 0.3375(7) 0.5846(4) 0.058(4) Uani 1 1 d . . . . . H20 H 0.4446 0.3500 0.5694 0.069 Uiso 1 1 calc R U . . . C21 C 0.3282(9) 0.3326(6) 0.5660(5) 0.058(3) Uani 1 1 d . . . . . C22 C 0.3202(8) 0.3414(6) 0.5204(4) 0.049(3) Uani 1 1 d . . . . . C23 C 0.2629(8) 0.3068(6) 0.5009(4) 0.052(3) Uani 1 1 d . . . . . H23A H 0.2273 0.2816 0.5168 0.063 Uiso 1 1 calc R U . . . C24 C 0.2538(7) 0.3065(6) 0.4584(4) 0.046(3) Uani 1 1 d . . . . . C25 C 0.2006(7) 0.2574(6) 0.4390(5) 0.053(3) Uani 1 1 d . . . . . C26 C 0.1988(9) 0.2526(7) 0.3974(5) 0.062(4) Uani 1 1 d . . . . . H26 H 0.2296 0.2824 0.3817 0.075 Uiso 1 1 calc R U . . . C27 C 0.1527(10) 0.2049(9) 0.3772(6) 0.084(5) Uani 1 1 d . . . . . H27 H 0.1502 0.2037 0.3484 0.101 Uiso 1 1 calc R U . . . C28 C 0.1121(10) 0.1606(8) 0.3999(7) 0.082(6) Uani 1 1 d . . . . . H28 H 0.0859 0.1249 0.3867 0.099 Uiso 1 1 calc R U . . . C29 C 0.1076(10) 0.1656(8) 0.4415(6) 0.081(5) Uani 1 1 d . . . . . H29 H 0.0731 0.1377 0.4563 0.097 Uiso 1 1 calc R U . . . C30 C 0.1540(9) 0.2120(7) 0.4619(5) 0.065(4) Uani 1 1 d . . . . . H30 H 0.1545 0.2134 0.4908 0.079 Uiso 1 1 calc R U . . . C31 C 0.0633(8) 0.3756(6) 0.5338(4) 0.049(3) Uani 1 1 d . . . . . H31 H 0.0970 0.4129 0.5368 0.059 Uiso 1 1 calc R U . . . C32 C 0.0389(9) 0.3404(7) 0.5678(5) 0.063(4) Uani 1 1 d . . . . . H32 H 0.0540 0.3551 0.5941 0.075 Uiso 1 1 calc R U . . . C33 C -0.0069(8) 0.2844(6) 0.5639(4) 0.055(3) Uani 1 1 d . . . . . H33 H -0.0210 0.2590 0.5872 0.066 Uiso 1 1 calc R U . . . C34 C -0.0322(10) 0.2655(8) 0.5257(5) 0.074(5) Uani 1 1 d . . . . . H34 H -0.0659 0.2283 0.5226 0.089 Uiso 1 1 calc R U . . . C35 C -0.0085(8) 0.3008(7) 0.4924(4) 0.055(4) Uani 1 1 d . . . . . H35 H -0.0251 0.2862 0.4663 0.066 Uiso 1 1 calc R U . . . C36 C 0.0382(7) 0.3563(5) 0.4947(3) 0.037(2) Uani 1 1 d . . . . . C37 C 0.0668(6) 0.3957(5) 0.4586(3) 0.034(2) Uani 1 1 d . . . . . C38 C 0.0408(7) 0.3793(6) 0.4199(3) 0.042(3) Uani 1 1 d . . . . . H38 H 0.0075 0.3417 0.4169 0.050 Uiso 1 1 calc R U . . . C39 C 0.0615(6) 0.4158(6) 0.3849(3) 0.039(3) Uani 1 1 d . . . . . C40 C 0.0281(7) 0.4001(7) 0.3440(4) 0.047(3) Uani 1 1 d . . . . . C41 C 0.0341(9) 0.4484(9) 0.3135(4) 0.071(4) Uani 1 1 d . . . . . H41 H 0.0604 0.4890 0.3192 0.086 Uiso 1 1 calc R U . . . C42 C 0.0029(11) 0.4388(11) 0.2754(5) 0.091(6) Uani 1 1 d . . . . . H42 H 0.0072 0.4720 0.2549 0.109 Uiso 1 1 calc R U . . . C43 C -0.0354(10) 0.3785(13) 0.2678(5) 0.095(7) Uani 1 1 d . . . . . H43 H -0.0563 0.3701 0.2415 0.114 Uiso 1 1 calc R U . . . C44 C -0.0433(13) 0.3310(13) 0.2977(6) 0.114(9) Uani 1 1 d . . . . . H44 H -0.0702 0.2908 0.2919 0.136 Uiso 1 1 calc R U . . . C45 C -0.0125(9) 0.3411(10) 0.3366(5) 0.081(5) Uani 1 1 d . . . . . H45 H -0.0190 0.3087 0.3574 0.097 Uiso 1 1 calc R U . . . C46 C 0.2449(18) 0.3891(12) 0.2183(6) 0.143(9) Uani 1 1 d . U . . . H46A H 0.2777 0.4156 0.2015 0.172 Uiso 1 1 calc R U . . . C47 C 0.1950(18) 0.3441(14) 0.2010(7) 0.150(9) Uani 1 1 d . U . . . H47A H 0.1907 0.3410 0.1722 0.180 Uiso 1 1 calc R U . . . C48 C 0.149(2) 0.3011(17) 0.2271(9) 0.185(12) Uani 1 1 d . U . . . H48A H 0.1182 0.2662 0.2157 0.222 Uiso 1 1 calc R U . . . C49 C 0.1492(15) 0.3121(14) 0.2695(8) 0.143(9) Uani 1 1 d . U . . . H49A H 0.1140 0.2892 0.2869 0.172 Uiso 1 1 calc R U . . . C50 C 0.2036(13) 0.3577(11) 0.2853(6) 0.107(6) Uani 1 1 d . U . . . H50A H 0.2095 0.3614 0.3139 0.128 Uiso 1 1 calc R U . . . C51 C 0.2475(12) 0.3963(9) 0.2610(5) 0.088(5) Uani 1 1 d D U . . . C52 C 0.3086(10) 0.4452(8) 0.2796(5) 0.073(4) Uani 1 1 d D U . . . C53 C 0.3781(10) 0.4560(10) 0.2625(5) 0.092(5) Uani 1 1 d D U . . . H53A H 0.3900 0.4315 0.2386 0.110 Uiso 1 1 calc R U . . . C54 C 0.4336(9) 0.4988(8) 0.2763(5) 0.068(4) Uani 1 1 d D U . . . C55 C 0.5145(10) 0.5032(9) 0.2559(5) 0.080(4) Uani 1 1 d D U . . . C56 C 0.5520(9) 0.5614(9) 0.2612(5) 0.072(4) Uani 1 1 d . U . . . H56A H 0.5311 0.5948 0.2785 0.086 Uiso 1 1 calc R U . . . C57 C 0.6266(12) 0.5723(12) 0.2395(7) 0.109(6) Uani 1 1 d . U . . . H57A H 0.6547 0.6129 0.2418 0.131 Uiso 1 1 calc R U . . . C58 C 0.6519(11) 0.5233(11) 0.2168(7) 0.109(7) Uani 1 1 d . U . . . H58A H 0.7009 0.5295 0.2038 0.131 Uiso 1 1 calc R U . . . C59 C 0.6145(15) 0.4638(13) 0.2101(7) 0.129(8) Uani 1 1 d . U . . . H59A H 0.6369 0.4303 0.1934 0.155 Uiso 1 1 calc R U . . . C60 C 0.5388(13) 0.4540(10) 0.2297(6) 0.101(6) Uani 1 1 d . U . . . H60A H 0.5079 0.4156 0.2246 0.121 Uiso 1 1 calc R U . . . C61 C 0.7797(7) 0.5137(7) 0.3952(4) 0.053(3) Uani 1 1 d . . . . . H61 H 0.8021 0.5278 0.4202 0.064 Uiso 1 1 calc R U . . . C62 C 0.8234(9) 0.4776(8) 0.3685(5) 0.076(5) Uani 1 1 d . . . . . H62 H 0.8756 0.4660 0.3752 0.091 Uiso 1 1 calc R U . . . C63 C 0.7920(8) 0.4577(8) 0.3320(5) 0.074(5) Uani 1 1 d . . . . . H63 H 0.8234 0.4336 0.3133 0.088 Uiso 1 1 calc R U . . . C64 C 0.7156(9) 0.4724(9) 0.3221(5) 0.074(5) Uani 1 1 d . . . . . H64 H 0.6943 0.4582 0.2969 0.089 Uiso 1 1 calc R U . . . C65 C 0.6711(8) 0.5076(7) 0.3491(4) 0.057(3) Uani 1 1 d . . . . . H65 H 0.6181 0.5168 0.3427 0.068 Uiso 1 1 calc R U . . . C66 C 0.7016(6) 0.5303(6) 0.3861(4) 0.041(3) Uani 1 1 d . . . . . C67 C 0.6498(6) 0.5660(6) 0.4154(4) 0.041(3) Uani 1 1 d . . . . . C68 C 0.6778(7) 0.5936(6) 0.4518(3) 0.042(3) Uani 1 1 d . . . . . H68 H 0.7327 0.5936 0.4558 0.051 Uiso 1 1 calc R U . . . C69 C 0.6323(7) 0.6207(5) 0.4822(3) 0.038(3) Uani 1 1 d . . . . . C70 C 0.6690(7) 0.6482(5) 0.5202(3) 0.039(3) Uani 1 1 d . . . . . C71 C 0.6318(8) 0.6979(7) 0.5407(4) 0.050(3) Uani 1 1 d . . . . . H71 H 0.5822 0.7131 0.5317 0.060 Uiso 1 1 calc R U . . . C72 C 0.6663(9) 0.7261(7) 0.5745(5) 0.065(4) Uani 1 1 d . . . . . H72 H 0.6409 0.7618 0.5881 0.078 Uiso 1 1 calc R U . . . C73 C 0.7380(8) 0.7030(8) 0.5891(4) 0.060(4) Uani 1 1 d . . . . . H73 H 0.7615 0.7226 0.6124 0.072 Uiso 1 1 calc R U . . . C74 C 0.7728(8) 0.6527(7) 0.5695(5) 0.059(3) Uani 1 1 d . . . . . H74 H 0.8212 0.6366 0.5795 0.070 Uiso 1 1 calc R U . . . C75 C 0.7413(7) 0.6237(7) 0.5357(4) 0.046(3) Uani 1 1 d . . . . . H75 H 0.7672 0.5877 0.5227 0.055 Uiso 1 1 calc R U . . . C76 C 0.4786(8) 0.4866(8) 0.6567(4) 0.062(4) Uani 1 1 d . . . . . H76 H 0.4334 0.4701 0.6701 0.075 Uiso 1 1 calc R U . . . C77 C 0.5516(10) 0.4815(10) 0.6746(4) 0.080(5) Uani 1 1 d . . . . . H77 H 0.5561 0.4614 0.7007 0.096 Uiso 1 1 calc R U . . . C78 C 0.6184(9) 0.5053(9) 0.6554(5) 0.076(5) Uani 1 1 d . . . . . H78 H 0.6682 0.5007 0.6678 0.091 Uiso 1 1 calc R U . . . C79 C 0.6110(9) 0.5348(9) 0.6190(5) 0.075(5) Uani 1 1 d . . . . . H79 H 0.6562 0.5523 0.6062 0.089 Uiso 1 1 calc R U . . . C80 C 0.5387(8) 0.5405(7) 0.5995(4) 0.056(3) Uani 1 1 d . . . . . H80 H 0.5351 0.5608 0.5734 0.067 Uiso 1 1 calc R U . . . C81 C 0.4732(7) 0.5166(6) 0.6184(4) 0.046(3) Uani 1 1 d . . . . . C82 C 0.3954(7) 0.5235(6) 0.5965(3) 0.041(3) Uani 1 1 d . . . . . C83 C 0.3265(7) 0.5086(6) 0.6157(3) 0.042(3) Uani 1 1 d . . . . . H83 H 0.3287 0.4940 0.6432 0.051 Uiso 1 1 calc R U . . . C84 C 0.2520(7) 0.5135(6) 0.5970(3) 0.036(3) Uani 1 1 d . . . . . C85 C 0.1785(7) 0.4939(5) 0.6197(3) 0.038(3) Uani 1 1 d . . . . . C86 C 0.1085(7) 0.5177(6) 0.6058(4) 0.041(3) Uani 1 1 d . . . . . H86 H 0.1076 0.5479 0.5835 0.049 Uiso 1 1 calc R U . . . C87 C 0.0398(8) 0.4984(7) 0.6236(4) 0.054(3) Uani 1 1 d . . . . . H87 H -0.0082 0.5150 0.6132 0.065 Uiso 1 1 calc R U . . . C88 C 0.0389(8) 0.4557(7) 0.6561(4) 0.058(4) Uani 1 1 d . . . . . H88 H -0.0089 0.4436 0.6687 0.070 Uiso 1 1 calc R U . . . C89 C 0.1105(9) 0.4302(9) 0.6704(4) 0.069(4) Uani 1 1 d . . . . . H89 H 0.1118 0.3994 0.6923 0.083 Uiso 1 1 calc R U . . . C90 C 0.1782(8) 0.4508(7) 0.6520(4) 0.054(3) Uani 1 1 d . . . . . H90 H 0.2267 0.4346 0.6620 0.065 Uiso 1 1 calc R U . . . C91 C 0.1308(7) 0.6365(6) 0.5006(3) 0.039(3) Uani 1 1 d . . . . . C92 C 0.0511(6) 0.6212(6) 0.4816(3) 0.037(3) Uani 1 1 d . . . . . H92 H 0.0212 0.6638 0.4785 0.045 Uiso 1 1 calc R U . . . C93 C 0.0032(7) 0.5726(6) 0.5074(4) 0.043(3) Uani 1 1 d . . . . . H93A H 0.0360 0.5356 0.5175 0.052 Uiso 1 1 calc R U . . . H93B H -0.0212 0.5955 0.5308 0.052 Uiso 1 1 calc R U . . . C94 C -0.0576(7) 0.5478(7) 0.4782(4) 0.053(3) Uani 1 1 d . . . . . H94A H -0.1053 0.5755 0.4799 0.064 Uiso 1 1 calc R U . . . H94B H -0.0715 0.5011 0.4844 0.064 Uiso 1 1 calc R U . . . C95 C -0.0216(7) 0.5530(6) 0.4361(4) 0.048(3) Uani 1 1 d . . . . . H95A H -0.0141 0.5082 0.4242 0.058 Uiso 1 1 calc R U . . . H95B H -0.0559 0.5791 0.4178 0.058 Uiso 1 1 calc R U . . . C96 C 0.1549(7) 0.6291(6) 0.3517(4) 0.042(3) Uani 1 1 d . . . . . C97 C 0.1859(7) 0.6533(7) 0.3112(4) 0.052(3) Uani 1 1 d . . . . . H97 H 0.1868 0.7030 0.3123 0.062 Uiso 1 1 calc R U . . . C98 C 0.1382(9) 0.6347(12) 0.2758(5) 0.092(6) Uani 1 1 d . . . . . H98A H 0.1270 0.6744 0.2590 0.111 Uiso 1 1 calc R U . . . H98B H 0.0879 0.6153 0.2849 0.111 Uiso 1 1 calc R U . . . C99 C 0.1829(10) 0.5853(8) 0.2522(5) 0.084(6) Uani 1 1 d . . . . . H99A H 0.1687 0.5864 0.2230 0.101 Uiso 1 1 calc R U . . . H99B H 0.1755 0.5397 0.2629 0.101 Uiso 1 1 calc R U . . . C100 C 0.2665(9) 0.6105(9) 0.2592(4) 0.070(4) Uani 1 1 d . . . . . H10A H 0.3050 0.5746 0.2544 0.084 Uiso 1 1 calc R U . . . H10B H 0.2786 0.6485 0.2412 0.084 Uiso 1 1 calc R U . . . C101 C 0.4060(7) 0.7128(6) 0.3608(4) 0.040(3) Uani 1 1 d . . . . . C102 C 0.4578(8) 0.7587(6) 0.3859(4) 0.045(3) Uani 1 1 d . . . . . H102 H 0.4232 0.7849 0.4045 0.054 Uiso 1 1 calc R U . . . C103 C 0.5039(9) 0.8084(7) 0.3598(5) 0.063(4) Uani 1 1 d . . . . . H10C H 0.4891 0.8548 0.3665 0.076 Uiso 1 1 calc R U . . . H10D H 0.4946 0.8005 0.3305 0.076 Uiso 1 1 calc R U . . . C104 C 0.5901(9) 0.7950(7) 0.3710(5) 0.062(4) Uani 1 1 d . . . . . H10E H 0.6239 0.7963 0.3465 0.075 Uiso 1 1 calc R U . . . H10F H 0.6095 0.8278 0.3911 0.075 Uiso 1 1 calc R U . . . C105 C 0.5872(7) 0.7245(7) 0.3893(4) 0.050(3) Uani 1 1 d . . . . . H10G H 0.5889 0.6905 0.3675 0.060 Uiso 1 1 calc R U . . . H10H H 0.6321 0.7172 0.4078 0.060 Uiso 1 1 calc R U . . . C106 C 0.3877(7) 0.7277(5) 0.4959(3) 0.037(3) Uani 1 1 d . . . . . C107 C 0.3267(8) 0.7428(5) 0.5287(4) 0.045(3) Uani 1 1 d . . . . . H107 H 0.2823 0.7677 0.5161 0.053 Uiso 1 1 calc R U . . . C108 C 0.3610(10) 0.7851(7) 0.5642(4) 0.072(5) Uani 1 1 d . . . . . H10I H 0.4187 0.7820 0.5645 0.087 Uiso 1 1 calc R U . . . H10J H 0.3460 0.8324 0.5612 0.087 Uiso 1 1 calc R U . . . C109 C 0.3276(11) 0.7569(6) 0.6026(4) 0.060(4) Uani 1 1 d . . . . . H10K H 0.3638 0.7627 0.6258 0.073 Uiso 1 1 calc R U . . . H10L H 0.2767 0.7776 0.6093 0.073 Uiso 1 1 calc R U . . . C110 C 0.3183(11) 0.6855(7) 0.5919(4) 0.068(4) Uani 1 1 d . . . . . H11A H 0.3680 0.6615 0.5966 0.082 Uiso 1 1 calc R U . . . H11B H 0.2775 0.6649 0.6092 0.082 Uiso 1 1 calc R U . . . C111 C 0.3299(13) 0.1121(9) 0.4096(6) 0.095(6) Uani 1 1 d . . . . . H11H H 0.3694 0.1240 0.4304 0.114 Uiso 1 1 calc R U . . . H11I H 0.2787 0.1295 0.4187 0.114 Uiso 1 1 calc R U . . . C112 C 0.7063(12) 0.3335(11) 0.2342(6) 0.100(6) Uani 1 1 d . . . . . H11F H 0.6697 0.3045 0.2190 0.120 Uiso 1 1 calc R U . . . H11G H 0.6763 0.3720 0.2447 0.120 Uiso 1 1 calc R U . . . C114 C 0.0170(13) 0.8033(10) 0.3416(7) 0.102(7) Uani 1 1 d . . . . . H11C H 0.0738 0.8086 0.3401 0.153 Uiso 1 1 calc R U . . . H11D H 0.0003 0.8055 0.3701 0.153 Uiso 1 1 calc R U . . . H11E H -0.0084 0.8390 0.3261 0.153 Uiso 1 1 calc R U . . . O26 O -0.0046(9) 0.7403(8) 0.3248(5) 0.110(5) Uani 1 1 d . . . . . H26A H -0.0032 0.7111 0.3431 0.164 Uiso 1 1 calc R U . . . Cl1 Cl 0.3250(3) 0.0255(3) 0.4048(2) 0.116(2) Uani 1 1 d . . . . . Cl2 Cl 0.3559(3) 0.1493(3) 0.36153(17) 0.1009(16) Uani 1 1 d . . . . . Cl3 Cl 0.7459(4) 0.2889(3) 0.2752(2) 0.135(2) Uani 1 1 d . . . . . Cl4 Cl 0.7772(4) 0.3615(4) 0.2019(3) 0.159(3) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.0415(3) 0.0306(3) 0.0327(3) -0.0013(2) 0.0026(2) 0.0016(2) Dy2 0.0362(3) 0.0317(2) 0.0263(2) -0.0008(2) 0.0006(2) -0.0013(2) Dy3 0.0367(3) 0.0356(3) 0.0252(2) -0.0008(2) 0.0009(2) -0.0009(2) Dy4 0.0355(3) 0.0340(3) 0.0300(3) 0.0007(2) 0.0024(2) -0.0001(2) Dy5 0.0401(3) 0.0445(3) 0.0273(3) 0.0025(2) 0.0015(2) -0.0031(2) O21 0.045(4) 0.031(4) 0.023(4) -0.009(3) -0.002(3) 0.002(3) O22 0.048(5) 0.030(4) 0.026(4) 0.004(3) 0.006(3) 0.000(3) O23 0.042(4) 0.030(4) 0.029(4) -0.005(3) -0.003(3) 0.007(3) O24 0.036(4) 0.031(4) 0.022(4) 0.003(3) 0.007(3) -0.001(3) O25 0.030(4) 0.030(4) 0.034(4) 0.001(3) 0.002(3) -0.003(3) O1 0.053(5) 0.038(5) 0.045(5) -0.009(4) 0.009(4) 0.004(4) O2 0.043(5) 0.040(5) 0.059(6) 0.003(4) 0.004(4) 0.005(4) O3 0.050(5) 0.043(4) 0.036(4) 0.009(4) 0.002(4) -0.002(4) O4 0.047(5) 0.037(4) 0.050(5) 0.004(4) 0.011(4) -0.010(4) O5 0.041(4) 0.035(4) 0.033(4) -0.002(3) 0.002(3) -0.008(4) O6 0.041(5) 0.048(5) 0.037(4) -0.004(4) 0.001(3) -0.004(4) O7 0.027(4) 0.042(4) 0.030(4) 0.007(3) -0.002(3) -0.004(3) O8 0.040(5) 0.065(6) 0.043(5) 0.001(4) -0.001(4) 0.006(4) O9 0.037(4) 0.069(5) 0.021(4) 0.007(4) -0.005(3) 0.005(4) O10 0.045(4) 0.049(5) 0.025(4) 0.004(4) 0.006(3) -0.003(4) O11 0.030(4) 0.036(4) 0.029(4) -0.001(3) 0.000(3) 0.008(3) O12 0.045(5) 0.066(6) 0.051(5) -0.027(5) 0.002(4) -0.009(4) O13 0.038(5) 0.053(5) 0.034(4) -0.007(4) 0.000(3) 0.003(4) O14 0.040(5) 0.045(5) 0.036(5) -0.003(4) -0.006(3) -0.002(4) O15 0.037(4) 0.030(4) 0.033(4) -0.004(3) 0.005(3) 0.002(3) O16 0.067(6) 0.040(5) 0.042(5) -0.008(4) 0.005(4) -0.013(4) O17 0.078(6) 0.067(6) 0.031(5) -0.013(4) -0.009(4) 0.000(5) O18 0.056(6) 0.090(7) 0.038(5) 0.009(4) 0.019(4) 0.008(5) O19 0.042(5) 0.045(5) 0.042(5) 0.008(4) 0.001(4) -0.009(4) O20 0.074(7) 0.054(6) 0.066(6) 0.026(5) -0.030(5) -0.015(5) N1 0.028(5) 0.038(5) 0.044(6) -0.005(4) -0.005(4) 0.000(4) N2 0.043(6) 0.045(6) 0.031(5) -0.010(4) 0.009(4) -0.011(4) N3 0.045(6) 0.031(5) 0.038(5) 0.001(4) 0.007(4) -0.007(4) N4 0.037(5) 0.052(6) 0.040(6) 0.009(5) -0.001(4) -0.004(5) C1 0.094(14) 0.111(15) 0.083(13) -0.026(12) 0.034(11) 0.003(12) C2 0.14(2) 0.126(18) 0.071(13) -0.013(12) 0.065(14) 0.039(16) C3 0.124(18) 0.062(11) 0.083(13) -0.012(9) 0.029(13) 0.013(11) C4 0.116(16) 0.065(10) 0.083(13) -0.025(10) 0.004(12) -0.003(10) C5 0.109(15) 0.086(13) 0.074(12) -0.043(10) 0.040(11) -0.033(11) C6 0.074(10) 0.041(7) 0.052(8) 0.001(6) 0.027(7) 0.009(7) C7 0.049(8) 0.026(6) 0.071(9) 0.000(6) 0.015(7) -0.001(5) C8 0.081(11) 0.047(8) 0.047(8) -0.002(6) 0.019(7) 0.003(7) C9 0.037(7) 0.039(7) 0.078(10) 0.003(7) 0.005(6) 0.004(6) C10 0.049(8) 0.045(7) 0.088(11) 0.016(8) 0.005(7) 0.003(6) C11 0.045(8) 0.055(8) 0.091(12) 0.015(8) -0.006(7) 0.008(7) C12 0.081(11) 0.051(9) 0.111(14) 0.022(9) -0.033(10) -0.017(8) C13 0.035(8) 0.054(9) 0.141(17) 0.026(11) 0.000(9) 0.007(7) C14 0.071(12) 0.065(11) 0.138(19) 0.016(13) 0.017(12) 0.013(9) C15 0.042(8) 0.062(9) 0.134(17) 0.019(10) 0.009(9) 0.014(7) C16 0.072(10) 0.058(9) 0.053(9) 0.014(7) 0.009(7) 0.003(7) C17 0.101(14) 0.088(13) 0.052(10) 0.018(9) 0.017(9) 0.011(11) C18 0.116(16) 0.092(13) 0.050(10) 0.022(9) -0.013(10) 0.006(11) C19 0.108(14) 0.093(14) 0.056(11) 0.021(9) -0.005(10) 0.028(11) C20 0.062(9) 0.065(9) 0.046(8) 0.016(7) -0.003(7) -0.008(7) C21 0.075(10) 0.046(7) 0.051(8) 0.013(6) 0.008(8) 0.004(7) C22 0.063(8) 0.032(6) 0.053(8) 0.000(5) 0.003(7) 0.015(7) C23 0.067(9) 0.044(7) 0.046(8) 0.010(6) 0.009(6) 0.005(6) C24 0.034(7) 0.032(6) 0.072(9) -0.006(6) 0.007(6) -0.001(5) C25 0.051(8) 0.045(7) 0.063(9) 0.001(7) 0.008(7) 0.004(6) C26 0.060(9) 0.046(8) 0.081(11) -0.016(7) 0.007(7) -0.014(7) C27 0.082(12) 0.077(12) 0.092(14) -0.030(10) -0.017(10) 0.000(10) C28 0.077(12) 0.046(9) 0.125(17) -0.001(10) -0.031(11) -0.016(8) C29 0.083(12) 0.062(10) 0.098(14) 0.007(10) -0.013(10) -0.031(9) C30 0.060(9) 0.056(9) 0.081(11) 0.009(8) -0.005(8) -0.006(7) C31 0.074(9) 0.036(7) 0.036(7) 0.003(5) 0.002(6) -0.014(6) C32 0.084(10) 0.061(9) 0.043(8) 0.002(7) 0.011(8) -0.014(8) C33 0.064(8) 0.050(8) 0.051(8) 0.021(7) 0.008(7) -0.008(6) C34 0.084(11) 0.062(9) 0.076(11) 0.023(8) -0.012(9) -0.029(9) C35 0.069(9) 0.052(8) 0.044(8) -0.005(6) -0.015(7) -0.027(7) C36 0.041(6) 0.030(5) 0.038(6) 0.001(5) -0.003(5) 0.001(5) C37 0.038(6) 0.030(6) 0.036(6) -0.004(5) -0.002(5) -0.007(5) C38 0.043(7) 0.045(7) 0.036(7) -0.013(5) 0.001(5) -0.010(6) C39 0.037(6) 0.046(7) 0.035(6) -0.012(5) 0.001(5) 0.008(5) C40 0.043(7) 0.067(8) 0.031(6) -0.016(6) -0.009(5) 0.000(6) C41 0.081(11) 0.093(12) 0.041(8) -0.015(8) -0.004(7) -0.021(9) C42 0.096(14) 0.125(17) 0.050(10) -0.014(11) -0.022(9) 0.017(12) C43 0.052(10) 0.18(2) 0.055(11) -0.027(13) -0.015(8) 0.001(12) C44 0.108(16) 0.15(2) 0.078(14) -0.066(15) 0.013(12) -0.064(15) C45 0.078(11) 0.121(15) 0.043(9) -0.031(9) -0.006(7) -0.025(11) C46 0.26(3) 0.113(16) 0.056(9) -0.020(11) -0.040(13) -0.043(15) C47 0.23(3) 0.14(2) 0.080(13) -0.041(12) -0.065(14) -0.026(16) C48 0.26(3) 0.18(2) 0.114(16) -0.043(17) -0.057(19) -0.079(19) C49 0.143(19) 0.17(2) 0.117(14) -0.061(15) -0.022(14) -0.070(14) C50 0.132(17) 0.106(14) 0.082(11) -0.032(10) -0.017(10) -0.043(11) C51 0.151(14) 0.064(10) 0.049(8) -0.021(7) -0.020(9) -0.010(9) C52 0.093(10) 0.077(10) 0.049(8) -0.018(7) 0.003(7) 0.000(8) C53 0.129(12) 0.090(12) 0.057(10) -0.012(8) 0.027(9) -0.010(10) C54 0.091(9) 0.060(8) 0.052(8) 0.007(6) 0.038(7) 0.011(7) C55 0.105(10) 0.064(9) 0.071(10) 0.011(7) 0.035(8) 0.014(7) C56 0.062(8) 0.084(10) 0.070(10) -0.009(8) 0.008(7) 0.017(7) C57 0.097(12) 0.103(12) 0.127(16) 0.025(11) 0.038(12) 0.009(10) C58 0.078(11) 0.100(12) 0.149(17) 0.043(12) 0.069(11) 0.044(9) C59 0.150(18) 0.117(14) 0.120(16) 0.010(13) 0.076(14) 0.026(13) C60 0.136(14) 0.084(10) 0.083(12) -0.002(9) 0.062(11) 0.018(10) C61 0.046(7) 0.057(9) 0.057(8) -0.014(7) 0.006(6) 0.002(6) C62 0.055(9) 0.077(10) 0.095(12) -0.034(9) 0.001(9) 0.002(9) C63 0.055(9) 0.083(11) 0.082(11) -0.049(9) 0.016(8) 0.010(8) C64 0.067(10) 0.091(12) 0.065(10) -0.039(9) -0.003(8) 0.012(9) C65 0.042(7) 0.072(9) 0.056(8) -0.024(7) 0.007(6) 0.008(7) C66 0.025(6) 0.044(7) 0.053(7) -0.004(6) 0.003(5) 0.002(5) C67 0.033(6) 0.040(7) 0.050(7) -0.001(6) 0.003(5) 0.011(5) C68 0.038(6) 0.043(6) 0.045(7) 0.000(5) 0.007(5) 0.003(5) C69 0.035(6) 0.036(6) 0.043(7) 0.004(5) -0.011(5) -0.011(5) C70 0.055(7) 0.028(5) 0.035(6) 0.000(5) 0.004(5) -0.011(5) C71 0.052(8) 0.058(8) 0.039(7) -0.013(6) -0.005(6) 0.000(6) C72 0.073(10) 0.056(8) 0.067(10) -0.027(7) 0.014(8) -0.003(8) C73 0.050(9) 0.078(10) 0.052(9) -0.002(8) -0.009(7) -0.015(8) C74 0.053(8) 0.058(8) 0.065(9) -0.003(8) -0.011(7) -0.009(7) C75 0.037(7) 0.056(8) 0.045(7) 0.003(6) -0.005(5) -0.008(6) C76 0.051(8) 0.094(12) 0.041(8) -0.001(7) -0.009(6) 0.016(8) C77 0.072(11) 0.129(16) 0.040(8) 0.005(9) -0.018(7) 0.031(11) C78 0.052(9) 0.094(12) 0.081(12) -0.008(10) -0.027(9) 0.008(9) C79 0.055(9) 0.083(12) 0.086(12) 0.007(10) -0.013(8) 0.003(8) C80 0.054(8) 0.060(9) 0.053(8) 0.014(7) -0.010(6) -0.009(7) C81 0.054(8) 0.051(7) 0.034(6) 0.000(6) -0.014(6) 0.008(6) C82 0.047(7) 0.045(7) 0.032(6) -0.001(5) -0.001(5) 0.000(6) C83 0.042(7) 0.053(7) 0.031(6) 0.006(5) -0.007(5) 0.006(6) C84 0.042(6) 0.047(7) 0.018(5) 0.002(5) 0.004(4) -0.002(5) C85 0.045(7) 0.038(6) 0.033(6) -0.005(5) -0.003(5) -0.003(6) C86 0.050(7) 0.033(6) 0.039(7) 0.004(5) -0.003(5) -0.004(5) C87 0.055(8) 0.056(8) 0.050(8) -0.001(6) 0.000(6) -0.008(7) C88 0.059(8) 0.078(10) 0.037(7) -0.006(7) 0.012(6) -0.018(8) C89 0.064(10) 0.103(12) 0.042(8) 0.026(8) -0.007(7) -0.026(9) C90 0.051(8) 0.067(8) 0.044(7) 0.011(6) -0.003(6) 0.005(7) C91 0.035(6) 0.048(7) 0.033(6) 0.004(5) 0.003(5) -0.002(5) C92 0.032(6) 0.040(6) 0.040(7) -0.008(5) -0.003(5) -0.002(5) C93 0.050(7) 0.032(6) 0.047(7) -0.002(6) 0.006(5) 0.009(5) C94 0.042(7) 0.067(9) 0.051(8) 0.011(7) -0.002(6) -0.018(6) C95 0.045(7) 0.038(6) 0.061(8) -0.013(6) -0.006(6) 0.002(5) C96 0.057(8) 0.037(6) 0.032(6) 0.005(5) -0.005(6) -0.004(6) C97 0.049(7) 0.069(8) 0.037(7) 0.021(6) 0.003(6) 0.007(7) C98 0.058(10) 0.17(2) 0.046(9) -0.005(11) -0.008(7) -0.009(11) C99 0.099(13) 0.072(10) 0.081(12) -0.023(9) -0.055(10) 0.025(10) C100 0.084(11) 0.091(12) 0.034(7) 0.010(8) 0.005(7) 0.035(9) C101 0.044(7) 0.031(6) 0.045(7) 0.011(5) 0.000(5) -0.004(5) C102 0.057(8) 0.035(6) 0.042(7) 0.008(5) -0.002(6) 0.002(6) C103 0.084(11) 0.047(8) 0.059(9) 0.015(7) -0.013(8) -0.024(7) C104 0.068(10) 0.055(9) 0.064(10) 0.008(7) 0.016(7) -0.014(7) C105 0.039(7) 0.061(9) 0.051(8) 0.002(6) 0.010(6) 0.003(6) C106 0.059(8) 0.029(6) 0.023(6) -0.001(4) -0.003(5) -0.003(5) C107 0.060(8) 0.032(6) 0.042(7) 0.002(5) -0.002(6) 0.005(6) C108 0.119(13) 0.050(8) 0.048(8) -0.025(7) 0.025(9) -0.036(8) C109 0.100(12) 0.041(7) 0.040(7) -0.009(6) -0.004(8) -0.014(8) C110 0.111(13) 0.055(8) 0.039(8) -0.002(6) -0.011(8) -0.015(9) C111 0.105(15) 0.076(11) 0.104(15) -0.004(11) 0.025(12) -0.001(11) C112 0.115(16) 0.093(14) 0.090(14) -0.013(11) 0.012(12) -0.027(12) C114 0.107(16) 0.089(15) 0.109(17) 0.023(13) -0.002(12) 0.019(12) O26 0.099(10) 0.107(11) 0.123(13) -0.005(10) -0.036(9) 0.031(9) Cl1 0.093(4) 0.078(3) 0.178(6) -0.006(3) 0.048(4) 0.002(3) Cl2 0.098(4) 0.114(4) 0.090(3) 0.006(3) 0.018(3) 0.027(3) Cl3 0.120(5) 0.113(5) 0.174(7) 0.007(5) -0.011(4) 0.016(4) Cl4 0.127(5) 0.175(7) 0.175(7) 0.013(6) 0.050(5) 0.014(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 O2 2.320(8) . ? Dy1 O4 2.322(7) . ? Dy1 O3 2.334(8) . ? Dy1 O1 2.334(8) . ? Dy1 O21 2.403(7) . ? Dy1 O23 2.421(7) . ? Dy1 O22 2.441(7) . ? Dy1 O24 2.454(7) . ? Dy2 O5 2.272(7) . ? Dy2 O6 2.283(8) . ? Dy2 O24 2.308(7) . ? Dy2 O21 2.338(7) . ? Dy2 O11 2.393(7) . ? Dy2 O7 2.427(7) . ? Dy2 N1 2.543(8) . ? Dy2 O25 2.569(6) . ? Dy3 O9 2.282(7) . ? Dy3 O10 2.283(7) . ? Dy3 O24 2.313(7) . ? Dy3 O23 2.337(7) . ? Dy3 O15 2.378(7) . ? Dy3 O11 2.428(7) . ? Dy3 N2 2.499(9) . ? Dy3 O25 2.571(7) . ? Dy4 O13 2.289(8) . ? Dy4 O14 2.291(7) . ? Dy4 O22 2.306(7) . ? Dy4 O23 2.316(8) . ? Dy4 O15 2.383(7) . ? Dy4 O19 2.418(8) . ? Dy4 N3 2.534(9) . ? Dy4 O25 2.609(6) . ? Dy5 O17 2.278(9) . ? Dy5 O21 2.296(7) . ? Dy5 O18 2.319(8) . ? Dy5 O22 2.320(7) . ? Dy5 O7 2.406(7) . ? Dy5 O19 2.417(8) . ? Dy5 N4 2.575(10) . ? Dy5 O25 2.585(7) . ? O21 H21 1.0000 . ? O22 H22 1.0000 . ? O23 H23 1.0000 . ? O24 H24 1.0000 . ? O25 H25 1.0001 . ? O1 C7 1.286(14) . ? O2 C9 1.297(15) . ? O3 C22 1.288(15) . ? O4 C24 1.253(14) . ? O5 C37 1.271(12) . ? O6 C39 1.291(14) . ? O7 C96 1.271(13) . ? O8 C96 1.234(14) . ? O9 C82 1.280(13) . ? O10 C84 1.269(12) . ? O11 C91 1.289(13) . ? O12 C91 1.217(14) . ? O13 C67 1.282(13) . ? O14 C69 1.275(13) . ? O15 C106 1.300(12) . ? O16 C106 1.224(13) . ? O17 C52 1.242(16) . ? O18 C54 1.313(17) . ? O19 C101 1.291(13) . ? O20 C101 1.224(14) . ? N1 C92 1.492(14) . ? N1 C95 1.501(14) . ? N1 H1 1.0000 . ? N2 C110 1.481(16) . ? N2 C107 1.504(15) . ? N2 H2 1.0000 . ? N3 C105 1.463(15) . ? N3 C102 1.491(15) . ? N3 H3 1.0000 . ? N4 C100 1.468(17) . ? N4 C97 1.487(16) . ? N4 H4 1.0000 . ? C1 C6 1.37(2) . ? C1 C2 1.45(3) . ? C1 H1A 0.9500 . ? C2 C3 1.42(3) . ? C2 H2A 0.9500 . ? C3 C4 1.30(3) . ? C3 H3A 0.9500 . ? C4 C5 1.41(2) . ? C4 H4A 0.9500 . ? C5 C6 1.39(2) . ? C5 H5 0.9500 . ? C6 C7 1.507(19) . ? C7 C8 1.36(2) . ? C8 C9 1.388(19) . ? C8 H8 0.9500 . ? C9 C10 1.499(19) . ? C10 C11 1.38(2) . ? C10 C15 1.39(2) . ? C11 C12 1.38(2) . ? C11 H11 0.9500 . ? C12 C13 1.39(2) . ? C12 H12 0.9500 . ? C13 C14 1.34(3) . ? C13 H13 0.9500 . ? C14 C15 1.41(2) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C21 1.369(19) . ? C16 C17 1.41(2) . ? C16 H16 0.9500 . ? C17 C18 1.34(2) . ? C17 H17 0.9500 . ? C18 C19 1.38(2) . ? C18 H18 0.9500 . ? C19 C20 1.37(2) . ? C19 H19 0.9500 . ? C20 C21 1.38(2) . ? C20 H20 0.9500 . ? C21 C22 1.516(19) . ? C22 C23 1.362(19) . ? C23 C24 1.404(19) . ? C23 H23A 0.9500 . ? C24 C25 1.486(18) . ? C25 C26 1.37(2) . ? C25 C30 1.427(19) . ? C26 C27 1.41(2) . ? C26 H26 0.9500 . ? C27 C28 1.35(3) . ? C27 H27 0.9500 . ? C28 C29 1.37(3) . ? C28 H28 0.9500 . ? C29 C30 1.40(2) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.388(18) . ? C31 C36 1.409(16) . ? C31 H31 0.9500 . ? C32 C33 1.377(19) . ? C32 H32 0.9500 . ? C33 C34 1.38(2) . ? C33 H33 0.9500 . ? C34 C35 1.365(19) . ? C34 H34 0.9500 . ? C35 C36 1.374(16) . ? C35 H35 0.9500 . ? C36 C37 1.508(15) . ? C37 C38 1.386(15) . ? C38 C39 1.412(16) . ? C38 H38 0.9500 . ? C39 C40 1.494(15) . ? C40 C45 1.39(2) . ? C40 C41 1.40(2) . ? C41 C42 1.37(2) . ? C41 H41 0.9500 . ? C42 C43 1.40(3) . ? C42 H42 0.9500 . ? C43 C44 1.38(3) . ? C43 H43 0.9500 . ? C44 C45 1.40(2) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46 C47 1.37(3) . ? C46 C51 1.41(2) . ? C46 H46A 0.9500 . ? C47 C48 1.45(4) . ? C47 H47A 0.9500 . ? C48 C49 1.41(3) . ? C48 H48A 0.9500 . ? C49 C50 1.41(3) . ? C49 H49A 0.9500 . ? C50 C51 1.34(3) . ? C50 H50A 0.9500 . ? C51 C52 1.56(2) . ? C52 C53 1.335(18) . ? C53 C54 1.359(18) . ? C53 H53A 0.9500 . ? C54 C55 1.541(18) . ? C55 C56 1.34(2) . ? C55 C60 1.37(2) . ? C56 C57 1.48(2) . ? C56 H56A 0.9500 . ? C57 C58 1.31(3) . ? C57 H57A 0.9500 . ? C58 C59 1.37(3) . ? C58 H58A 0.9500 . ? C59 C60 1.46(3) . ? C59 H59A 0.9500 . ? C60 H60A 0.9500 . ? C61 C62 1.361(19) . ? C61 C66 1.411(17) . ? C61 H61 0.9500 . ? C62 C63 1.37(2) . ? C62 H62 0.9500 . ? C63 C64 1.38(2) . ? C63 H63 0.9500 . ? C64 C65 1.368(18) . ? C64 H64 0.9500 . ? C65 C66 1.397(17) . ? C65 H65 0.9500 . ? C66 C67 1.495(16) . ? C67 C68 1.401(16) . ? C68 C69 1.380(16) . ? C68 H68 0.9500 . ? C69 C70 1.501(15) . ? C70 C71 1.362(17) . ? C70 C75 1.426(17) . ? C71 C72 1.381(18) . ? C71 H71 0.9500 . ? C72 C73 1.40(2) . ? C72 H72 0.9500 . ? C73 C74 1.34(2) . ? C73 H73 0.9500 . ? C74 C75 1.367(18) . ? C74 H74 0.9500 . ? C75 H75 0.9500 . ? C76 C77 1.386(19) . ? C76 C81 1.399(18) . ? C76 H76 0.9500 . ? C77 C78 1.39(2) . ? C77 H77 0.9500 . ? C78 C79 1.34(2) . ? C78 H78 0.9500 . ? C79 C80 1.40(2) . ? C79 H79 0.9500 . ? C80 C81 1.370(19) . ? C80 H80 0.9500 . ? C81 C82 1.521(16) . ? C82 C83 1.372(16) . ? C83 C84 1.419(16) . ? C83 H83 0.9500 . ? C84 C85 1.517(16) . ? C85 C90 1.369(16) . ? C85 C86 1.369(16) . ? C86 C87 1.371(18) . ? C86 H86 0.9500 . ? C87 C88 1.369(19) . ? C87 H87 0.9500 . ? C88 C89 1.41(2) . ? C88 H88 0.9500 . ? C89 C90 1.371(19) . ? C89 H89 0.9500 . ? C90 H90 0.9500 . ? C91 C92 1.533(15) . ? C92 C93 1.532(16) . ? C92 H92 1.0000 . ? C93 C94 1.499(17) . ? C93 H93A 0.9900 . ? C93 H93B 0.9900 . ? C94 C95 1.519(18) . ? C94 H94A 0.9900 . ? C94 H94B 0.9900 . ? C95 H95A 0.9900 . ? C95 H95B 0.9900 . ? C96 C97 1.515(16) . ? C97 C98 1.468(19) . ? C97 H97 1.0000 . ? C98 C99 1.47(2) . ? C98 H98A 0.9900 . ? C98 H98B 0.9900 . ? C99 C100 1.54(2) . ? C99 H99A 0.9900 . ? C99 H99B 0.9900 . ? C100 H10A 0.9900 . ? C100 H10B 0.9900 . ? C101 C102 1.521(17) . ? C102 C103 1.535(17) . ? C102 H102 1.0000 . ? C103 C104 1.54(2) . ? C103 H10C 0.9900 . ? C103 H10D 0.9900 . ? C104 C105 1.539(19) . ? C104 H10E 0.9900 . ? C104 H10F 0.9900 . ? C105 H10G 0.9900 . ? C105 H10H 0.9900 . ? C106 C107 1.530(17) . ? C107 C108 1.558(17) . ? C107 H107 1.0000 . ? C108 C109 1.498(19) . ? C108 H10I 0.9900 . ? C108 H10J 0.9900 . ? C109 C110 1.485(18) . ? C109 H10K 0.9900 . ? C109 H10L 0.9900 . ? C110 H11A 0.9900 . ? C110 H11B 0.9900 . ? C111 Cl1 1.747(18) . ? C111 Cl2 1.804(19) . ? C111 H11H 0.9900 . ? C111 H11I 0.9900 . ? C112 Cl4 1.71(2) . ? C112 Cl3 1.76(2) . ? C112 H11F 0.9900 . ? C112 H11G 0.9900 . ? C114 O26 1.43(2) . ? C114 H11C 0.9800 . ? C114 H11D 0.9800 . ? C114 H11E 0.9800 . ? O26 H26A 0.8400 . ? 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 O2 Dy1 O4 118.6(3) . . ? O2 Dy1 O3 80.1(3) . . ? O4 Dy1 O3 73.4(3) . . ? O2 Dy1 O1 73.2(3) . . ? O4 Dy1 O1 72.9(3) . . ? O3 Dy1 O1 118.3(3) . . ? O2 Dy1 O21 145.2(3) . . ? O4 Dy1 O21 73.4(3) . . ? O3 Dy1 O21 133.6(3) . . ? O1 Dy1 O21 80.8(3) . . ? O2 Dy1 O23 76.7(3) . . ? O4 Dy1 O23 149.9(3) . . ? O3 Dy1 O23 85.1(3) . . ? O1 Dy1 O23 137.0(3) . . ? O21 Dy1 O23 109.8(2) . . ? O2 Dy1 O22 81.0(3) . . ? O4 Dy1 O22 135.0(3) . . ? O3 Dy1 O22 151.4(3) . . ? O1 Dy1 O22 75.8(3) . . ? O21 Dy1 O22 70.4(3) . . ? O23 Dy1 O22 69.8(2) . . ? O2 Dy1 O24 139.6(3) . . ? O4 Dy1 O24 82.0(3) . . ? O3 Dy1 O24 73.1(3) . . ? O1 Dy1 O24 146.6(3) . . ? O21 Dy1 O24 71.1(2) . . ? O23 Dy1 O24 71.5(2) . . ? O22 Dy1 O24 109.7(2) . . ? O5 Dy2 O6 73.0(3) . . ? O5 Dy2 O24 75.1(3) . . ? O6 Dy2 O24 128.6(3) . . ? O5 Dy2 O21 107.9(3) . . ? O6 Dy2 O21 77.9(3) . . ? O24 Dy2 O21 74.8(2) . . ? O5 Dy2 O11 99.4(2) . . ? O6 Dy2 O11 148.6(3) . . ? O24 Dy2 O11 75.5(2) . . ? O21 Dy2 O11 132.4(2) . . ? O5 Dy2 O7 150.4(2) . . ? O6 Dy2 O7 79.3(3) . . ? O24 Dy2 O7 132.4(2) . . ? O21 Dy2 O7 75.7(2) . . ? O11 Dy2 O7 98.8(2) . . ? O5 Dy2 N1 82.0(3) . . ? O6 Dy2 N1 82.4(3) . . ? O24 Dy2 N1 131.1(3) . . ? O21 Dy2 N1 154.1(3) . . ? O11 Dy2 N1 66.3(3) . . ? O7 Dy2 N1 84.2(3) . . ? O5 Dy2 O25 142.7(2) . . ? O6 Dy2 O25 135.2(2) . . ? O24 Dy2 O25 67.8(2) . . ? O21 Dy2 O25 66.6(2) . . ? O11 Dy2 O25 68.0(2) . . ? O7 Dy2 O25 66.4(2) . . ? N1 Dy2 O25 119.8(2) . . ? O9 Dy3 O10 73.7(3) . . ? O9 Dy3 O24 109.3(3) . . ? O10 Dy3 O24 80.0(3) . . ? O9 Dy3 O23 72.7(3) . . ? O10 Dy3 O23 128.5(3) . . ? O24 Dy3 O23 75.6(2) . . ? O9 Dy3 O15 98.1(3) . . ? O10 Dy3 O15 146.9(3) . . ? O24 Dy3 O15 132.0(2) . . ? O23 Dy3 O15 76.0(3) . . ? O9 Dy3 O11 152.5(2) . . ? O10 Dy3 O11 80.5(2) . . ? O24 Dy3 O11 74.7(2) . . ? O23 Dy3 O11 132.9(2) . . ? O15 Dy3 O11 98.3(2) . . ? O9 Dy3 N2 85.7(3) . . ? O10 Dy3 N2 79.8(3) . . ? O24 Dy3 N2 150.2(3) . . ? O23 Dy3 N2 134.2(3) . . ? O15 Dy3 N2 67.5(3) . . ? O11 Dy3 N2 80.4(3) . . ? O9 Dy3 O25 139.9(2) . . ? O10 Dy3 O25 139.0(2) . . ? O24 Dy3 O25 67.7(2) . . ? O23 Dy3 O25 67.8(2) . . ? O15 Dy3 O25 65.9(2) . . ? O11 Dy3 O25 67.4(2) . . ? N2 Dy3 O25 117.1(3) . . ? O13 Dy4 O14 73.5(3) . . ? O13 Dy4 O22 73.6(3) . . ? O14 Dy4 O22 132.3(3) . . ? O13 Dy4 O23 104.8(3) . . ? O14 Dy4 O23 82.2(3) . . ? O22 Dy4 O23 74.0(2) . . ? O13 Dy4 O15 153.3(3) . . ? O14 Dy4 O15 80.3(3) . . ? O22 Dy4 O15 130.5(3) . . ? O23 Dy4 O15 76.3(2) . . ? O13 Dy4 O19 101.0(3) . . ? O14 Dy4 O19 144.4(3) . . ? O22 Dy4 O19 75.5(3) . . ? O23 Dy4 O19 132.1(3) . . ? O15 Dy4 O19 97.2(3) . . ? O13 Dy4 N3 84.3(3) . . ? O14 Dy4 N3 78.5(3) . . ? O22 Dy4 N3 130.6(3) . . ? O23 Dy4 N3 155.4(3) . . ? O15 Dy4 N3 85.4(3) . . ? O19 Dy4 N3 66.0(3) . . ? O13 Dy4 O25 140.5(3) . . ? O14 Dy4 O25 138.1(3) . . ? O22 Dy4 O25 67.1(2) . . ? O23 Dy4 O25 67.5(2) . . ? O15 Dy4 O25 65.2(2) . . ? O19 Dy4 O25 66.9(2) . . ? N3 Dy4 O25 119.4(3) . . ? O17 Dy5 O21 73.5(3) . . ? O17 Dy5 O18 73.2(4) . . ? O21 Dy5 O18 124.8(3) . . ? O17 Dy5 O22 111.7(3) . . ? O21 Dy5 O22 74.4(3) . . ? O18 Dy5 O22 78.7(3) . . ? O17 Dy5 O7 95.5(3) . . ? O21 Dy5 O7 76.8(2) . . ? O18 Dy5 O7 148.7(3) . . ? O22 Dy5 O7 132.1(2) . . ? O17 Dy5 O19 153.6(3) . . ? O21 Dy5 O19 131.9(3) . . ? O18 Dy5 O19 83.8(3) . . ? O22 Dy5 O19 75.3(3) . . ? O7 Dy5 O19 97.6(3) . . ? O17 Dy5 N4 82.2(3) . . ? O21 Dy5 N4 132.8(3) . . ? O18 Dy5 N4 83.4(3) . . ? O22 Dy5 N4 152.7(3) . . ? O7 Dy5 N4 65.9(3) . . ? O19 Dy5 N4 82.5(3) . . ? O17 Dy5 O25 139.1(3) . . ? O21 Dy5 O25 66.9(2) . . ? O18 Dy5 O25 139.6(3) . . ? O22 Dy5 O25 67.3(2) . . ? O7 Dy5 O25 66.4(2) . . ? O19 Dy5 O25 67.3(2) . . ? N4 Dy5 O25 118.1(3) . . ? Dy5 O21 Dy2 102.3(3) . . ? Dy5 O21 Dy1 108.4(3) . . ? Dy2 O21 Dy1 107.2(3) . . ? Dy5 O21 H21 112.8 . . ? Dy2 O21 H21 112.8 . . ? Dy1 O21 H21 112.8 . . ? Dy4 O22 Dy5 102.9(3) . . ? Dy4 O22 Dy1 107.6(3) . . ? Dy5 O22 Dy1 106.3(3) . . ? Dy4 O22 H22 113.1 . . ? Dy5 O22 H22 113.1 . . ? Dy1 O22 H22 113.1 . . ? Dy4 O23 Dy3 101.3(3) . . ? Dy4 O23 Dy1 107.9(3) . . ? Dy3 O23 Dy1 106.3(3) . . ? Dy4 O23 H23 113.5 . . ? Dy3 O23 H23 113.5 . . ? Dy1 O23 H23 113.5 . . ? Dy2 O24 Dy3 102.2(3) . . ? Dy2 O24 Dy1 106.5(3) . . ? Dy3 O24 Dy1 106.0(3) . . ? Dy2 O24 H24 113.7 . . ? Dy3 O24 H24 113.7 . . ? Dy1 O24 H24 113.7 . . ? Dy2 O25 Dy3 88.8(2) . . ? Dy2 O25 Dy5 88.9(2) . . ? Dy3 O25 Dy5 161.0(3) . . ? Dy2 O25 Dy4 161.4(3) . . ? Dy3 O25 Dy4 88.0(2) . . ? Dy5 O25 Dy4 88.2(2) . . ? Dy2 O25 H25 98.2 . . ? Dy3 O25 H25 99.8 . . ? Dy5 O25 H25 99.2 . . ? Dy4 O25 H25 100.4 . . ? C7 O1 Dy1 135.2(8) . . ? C9 O2 Dy1 134.0(8) . . ? C22 O3 Dy1 130.9(8) . . ? C24 O4 Dy1 135.0(9) . . ? C37 O5 Dy2 138.0(7) . . ? C39 O6 Dy2 137.6(7) . . ? C96 O7 Dy5 127.5(7) . . ? C96 O7 Dy2 134.7(7) . . ? Dy5 O7 Dy2 96.6(2) . . ? C82 O9 Dy3 136.5(7) . . ? C84 O10 Dy3 137.3(7) . . ? C91 O11 Dy2 126.7(7) . . ? C91 O11 Dy3 131.9(7) . . ? Dy2 O11 Dy3 96.5(2) . . ? C67 O13 Dy4 138.1(7) . . ? C69 O14 Dy4 136.2(7) . . ? C106 O15 Dy3 126.1(7) . . ? C106 O15 Dy4 135.5(7) . . ? Dy3 O15 Dy4 98.2(2) . . ? C52 O17 Dy5 138.7(10) . . ? C54 O18 Dy5 132.5(9) . . ? C101 O19 Dy5 138.0(8) . . ? C101 O19 Dy4 125.1(8) . . ? Dy5 O19 Dy4 96.8(3) . . ? C92 N1 C95 105.3(9) . . ? C92 N1 Dy2 112.4(6) . . ? C95 N1 Dy2 119.9(7) . . ? C92 N1 H1 106.1 . . ? C95 N1 H1 106.1 . . ? Dy2 N1 H1 106.1 . . ? C110 N2 C107 105.8(9) . . ? C110 N2 Dy3 120.8(8) . . ? C107 N2 Dy3 115.1(6) . . ? C110 N2 H2 104.5 . . ? C107 N2 H2 104.5 . . ? Dy3 N2 H2 104.5 . . ? C105 N3 C102 103.7(9) . . ? C105 N3 Dy4 119.0(7) . . ? C102 N3 Dy4 113.6(7) . . ? C105 N3 H3 106.6 . . ? C102 N3 H3 106.6 . . ? Dy4 N3 H3 106.6 . . ? C100 N4 C97 105.8(10) . . ? C100 N4 Dy5 118.8(8) . . ? C97 N4 Dy5 115.2(7) . . ? C100 N4 H4 105.3 . . ? C97 N4 H4 105.3 . . ? Dy5 N4 H4 105.3 . . ? C6 C1 C2 118(2) . . ? C6 C1 H1A 120.9 . . ? C2 C1 H1A 120.9 . . ? C3 C2 C1 121.2(17) . . ? C3 C2 H2A 119.4 . . ? C1 C2 H2A 119.4 . . ? C4 C3 C2 118.6(19) . . ? C4 C3 H3A 120.7 . . ? C2 C3 H3A 120.7 . . ? C3 C4 C5 121(2) . . ? C3 C4 H4A 119.6 . . ? C5 C4 H4A 119.6 . . ? C6 C5 C4 123.0(17) . . ? C6 C5 H5 118.5 . . ? C4 C5 H5 118.5 . . ? C1 C6 C5 117.9(16) . . ? C1 C6 C7 122.3(16) . . ? C5 C6 C7 119.8(12) . . ? O1 C7 C8 123.7(13) . . ? O1 C7 C6 114.2(12) . . ? C8 C7 C6 122.0(12) . . ? C7 C8 C9 125.7(13) . . ? C7 C8 H8 117.1 . . ? C9 C8 H8 117.1 . . ? O2 C9 C8 124.3(12) . . ? O2 C9 C10 113.8(13) . . ? C8 C9 C10 121.8(13) . . ? C11 C10 C15 119.2(14) . . ? C11 C10 C9 120.7(12) . . ? C15 C10 C9 120.1(15) . . ? C12 C11 C10 121.3(15) . . ? C12 C11 H11 119.4 . . ? C10 C11 H11 119.4 . . ? C11 C12 C13 119.5(17) . . ? C11 C12 H12 120.2 . . ? C13 C12 H12 120.2 . . ? C14 C13 C12 119.3(16) . . ? C14 C13 H13 120.3 . . ? C12 C13 H13 120.3 . . ? C13 C14 C15 122.1(17) . . ? C13 C14 H14 119.0 . . ? C15 C14 H14 119.0 . . ? C10 C15 C14 118.5(19) . . ? C10 C15 H15 120.8 . . ? C14 C15 H15 120.8 . . ? C21 C16 C17 121.4(16) . . ? C21 C16 H16 119.3 . . ? C17 C16 H16 119.3 . . ? C18 C17 C16 120.2(17) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C17 C18 C19 118.1(16) . . ? C17 C18 H18 120.9 . . ? C19 C18 H18 120.9 . . ? C20 C19 C18 122.6(18) . . ? C20 C19 H19 118.7 . . ? C18 C19 H19 118.7 . . ? C21 C20 C19 119.3(15) . . ? C21 C20 H20 120.3 . . ? C19 C20 H20 120.3 . . ? C16 C21 C20 118.2(14) . . ? C16 C21 C22 120.9(14) . . ? C20 C21 C22 120.9(13) . . ? O3 C22 C23 126.6(12) . . ? O3 C22 C21 115.1(12) . . ? C23 C22 C21 118.0(12) . . ? C22 C23 C24 123.4(13) . . ? C22 C23 H23A 118.3 . . ? C24 C23 H23A 118.3 . . ? O4 C24 C23 125.1(12) . . ? O4 C24 C25 114.9(12) . . ? C23 C24 C25 119.9(12) . . ? C26 C25 C30 117.9(13) . . ? C26 C25 C24 119.3(12) . . ? C30 C25 C24 122.7(14) . . ? C25 C26 C27 122.1(16) . . ? C25 C26 H26 119.0 . . ? C27 C26 H26 119.0 . . ? C28 C27 C26 118.4(18) . . ? C28 C27 H27 120.8 . . ? C26 C27 H27 120.8 . . ? C27 C28 C29 122.0(16) . . ? C27 C28 H28 119.0 . . ? C29 C28 H28 119.0 . . ? C28 C29 C30 119.7(16) . . ? C28 C29 H29 120.1 . . ? C30 C29 H29 120.1 . . ? C29 C30 C25 119.5(16) . . ? C29 C30 H30 120.3 . . ? C25 C30 H30 120.3 . . ? C32 C31 C36 120.1(12) . . ? C32 C31 H31 119.9 . . ? C36 C31 H31 119.9 . . ? C33 C32 C31 120.9(14) . . ? C33 C32 H32 119.6 . . ? C31 C32 H32 119.6 . . ? C32 C33 C34 119.2(13) . . ? C32 C33 H33 120.4 . . ? C34 C33 H33 120.4 . . ? C35 C34 C33 119.5(13) . . ? C35 C34 H34 120.2 . . ? C33 C34 H34 120.2 . . ? C34 C35 C36 123.4(13) . . ? C34 C35 H35 118.3 . . ? C36 C35 H35 118.3 . . ? C35 C36 C31 116.8(11) . . ? C35 C36 C37 124.9(11) . . ? C31 C36 C37 118.2(10) . . ? O5 C37 C38 124.9(10) . . ? O5 C37 C36 115.7(9) . . ? C38 C37 C36 119.4(10) . . ? C37 C38 C39 122.9(11) . . ? C37 C38 H38 118.5 . . ? C39 C38 H38 118.5 . . ? O6 C39 C38 123.4(10) . . ? O6 C39 C40 114.7(11) . . ? C38 C39 C40 121.9(11) . . ? C45 C40 C41 119.9(12) . . ? C45 C40 C39 121.8(13) . . ? C41 C40 C39 118.1(12) . . ? C42 C41 C40 121.9(16) . . ? C42 C41 H41 119.1 . . ? C40 C41 H41 119.1 . . ? C41 C42 C43 117.8(19) . . ? C41 C42 H42 121.1 . . ? C43 C42 H42 121.1 . . ? C44 C43 C42 121.1(16) . . ? C44 C43 H43 119.4 . . ? C42 C43 H43 119.4 . . ? C43 C44 C45 121.1(19) . . ? C43 C44 H44 119.5 . . ? C45 C44 H44 119.5 . . ? C40 C45 C44 118.1(18) . . ? C40 C45 H45 120.9 . . ? C44 C45 H45 120.9 . . ? C47 C46 C51 120(3) . . ? C47 C46 H46A 120.0 . . ? C51 C46 H46A 120.0 . . ? C46 C47 C48 119(2) . . ? C46 C47 H47A 120.3 . . ? C48 C47 H47A 120.3 . . ? C49 C48 C47 119(2) . . ? C49 C48 H48A 120.5 . . ? C47 C48 H48A 120.5 . . ? C50 C49 C48 118(3) . . ? C50 C49 H49A 120.9 . . ? C48 C49 H49A 120.9 . . ? C51 C50 C49 122(2) . . ? C51 C50 H50A 119.1 . . ? C49 C50 H50A 119.1 . . ? C50 C51 C46 121.0(18) . . ? C50 C51 C52 120.4(15) . . ? C46 C51 C52 118.4(19) . . ? O17 C52 C53 124.0(15) . . ? O17 C52 C51 113.7(14) . . ? C53 C52 C51 122.4(15) . . ? C52 C53 C54 125.9(16) . . ? C52 C53 H53A 117.1 . . ? C54 C53 H53A 117.1 . . ? O18 C54 C53 125.2(13) . . ? O18 C54 C55 113.5(14) . . ? C53 C54 C55 121.3(15) . . ? C56 C55 C60 124.1(16) . . ? C56 C55 C54 115.1(14) . . ? C60 C55 C54 120.2(18) . . ? C55 C56 C57 118.6(17) . . ? C55 C56 H56A 120.7 . . ? C57 C56 H56A 120.7 . . ? C58 C57 C56 117(2) . . ? C58 C57 H57A 121.6 . . ? C56 C57 H57A 121.6 . . ? C57 C58 C59 126.2(19) . . ? C57 C58 H58A 116.9 . . ? C59 C58 H58A 116.9 . . ? C58 C59 C60 117(2) . . ? C58 C59 H59A 121.3 . . ? C60 C59 H59A 121.3 . . ? C55 C60 C59 117(2) . . ? C55 C60 H60A 121.7 . . ? C59 C60 H60A 121.7 . . ? C62 C61 C66 120.6(13) . . ? C62 C61 H61 119.7 . . ? C66 C61 H61 119.7 . . ? C61 C62 C63 120.2(15) . . ? C61 C62 H62 119.9 . . ? C63 C62 H62 119.9 . . ? C62 C63 C64 121.0(13) . . ? C62 C63 H63 119.5 . . ? C64 C63 H63 119.5 . . ? C65 C64 C63 119.0(14) . . ? C65 C64 H64 120.5 . . ? C63 C64 H64 120.5 . . ? C64 C65 C66 121.6(13) . . ? C64 C65 H65 119.2 . . ? C66 C65 H65 119.2 . . ? C65 C66 C61 117.6(11) . . ? C65 C66 C67 119.7(10) . . ? C61 C66 C67 122.6(11) . . ? O13 C67 C68 121.8(10) . . ? O13 C67 C66 115.7(10) . . ? C68 C67 C66 122.5(10) . . ? C69 C68 C67 125.5(11) . . ? C69 C68 H68 117.2 . . ? C67 C68 H68 117.2 . . ? O14 C69 C68 124.4(10) . . ? O14 C69 C70 114.8(10) . . ? C68 C69 C70 120.8(10) . . ? C71 C70 C75 118.8(11) . . ? C71 C70 C69 119.0(11) . . ? C75 C70 C69 122.2(11) . . ? C70 C71 C72 120.0(13) . . ? C70 C71 H71 120.0 . . ? C72 C71 H71 120.0 . . ? C71 C72 C73 121.1(13) . . ? C71 C72 H72 119.4 . . ? C73 C72 H72 119.4 . . ? C74 C73 C72 118.4(14) . . ? C74 C73 H73 120.8 . . ? C72 C73 H73 120.8 . . ? C73 C74 C75 122.6(14) . . ? C73 C74 H74 118.7 . . ? C75 C74 H74 118.7 . . ? C74 C75 C70 119.1(12) . . ? C74 C75 H75 120.5 . . ? C70 C75 H75 120.5 . . ? C77 C76 C81 118.4(15) . . ? C77 C76 H76 120.8 . . ? C81 C76 H76 120.8 . . ? C76 C77 C78 121.5(15) . . ? C76 C77 H77 119.2 . . ? C78 C77 H77 119.2 . . ? C79 C78 C77 118.7(14) . . ? C79 C78 H78 120.7 . . ? C77 C78 H78 120.7 . . ? C78 C79 C80 122.0(16) . . ? C78 C79 H79 119.0 . . ? C80 C79 H79 119.0 . . ? C81 C80 C79 119.1(13) . . ? C81 C80 H80 120.4 . . ? C79 C80 H80 120.4 . . ? C80 C81 C76 120.3(12) . . ? C80 C81 C82 118.0(11) . . ? C76 C81 C82 121.7(12) . . ? O9 C82 C83 125.0(11) . . ? O9 C82 C81 114.0(10) . . ? C83 C82 C81 121.0(10) . . ? C82 C83 C84 123.9(10) . . ? C82 C83 H83 118.1 . . ? C84 C83 H83 118.1 . . ? O10 C84 C83 123.5(10) . . ? O10 C84 C85 115.5(10) . . ? C83 C84 C85 120.9(10) . . ? C90 C85 C86 118.5(11) . . ? C90 C85 C84 123.3(11) . . ? C86 C85 C84 118.1(10) . . ? C85 C86 C87 120.6(12) . . ? C85 C86 H86 119.7 . . ? C87 C86 H86 119.7 . . ? C88 C87 C86 121.3(13) . . ? C88 C87 H87 119.4 . . ? C86 C87 H87 119.4 . . ? C87 C88 C89 118.6(13) . . ? C87 C88 H88 120.7 . . ? C89 C88 H88 120.7 . . ? C90 C89 C88 118.6(13) . . ? C90 C89 H89 120.7 . . ? C88 C89 H89 120.7 . . ? C85 C90 C89 122.4(13) . . ? C85 C90 H90 118.8 . . ? C89 C90 H90 118.8 . . ? O12 C91 O11 126.3(11) . . ? O12 C91 C92 119.1(10) . . ? O11 C91 C92 114.6(10) . . ? N1 C92 C93 103.3(9) . . ? N1 C92 C91 114.0(9) . . ? C93 C92 C91 112.2(10) . . ? N1 C92 H92 109.0 . . ? C93 C92 H92 109.0 . . ? C91 C92 H92 109.0 . . ? C94 C93 C92 103.2(10) . . ? C94 C93 H93A 111.1 . . ? C92 C93 H93A 111.1 . . ? C94 C93 H93B 111.1 . . ? C92 C93 H93B 111.1 . . ? H93A C93 H93B 109.1 . . ? C93 C94 C95 106.2(10) . . ? C93 C94 H94A 110.5 . . ? C95 C94 H94A 110.5 . . ? C93 C94 H94B 110.5 . . ? C95 C94 H94B 110.5 . . ? H94A C94 H94B 108.7 . . ? N1 C95 C94 106.6(10) . . ? N1 C95 H95A 110.4 . . ? C94 C95 H95A 110.4 . . ? N1 C95 H95B 110.4 . . ? C94 C95 H95B 110.4 . . ? H95A C95 H95B 108.6 . . ? O8 C96 O7 125.2(11) . . ? O8 C96 C97 117.4(11) . . ? O7 C96 C97 117.3(11) . . ? C98 C97 N4 106.5(12) . . ? C98 C97 C96 114.8(12) . . ? N4 C97 C96 114.0(10) . . ? C98 C97 H97 107.0 . . ? N4 C97 H97 107.0 . . ? C96 C97 H97 107.0 . . ? C97 C98 C99 107.4(13) . . ? C97 C98 H98A 110.2 . . ? C99 C98 H98A 110.2 . . ? C97 C98 H98B 110.2 . . ? C99 C98 H98B 110.2 . . ? H98A C98 H98B 108.5 . . ? C98 C99 C100 100.6(13) . . ? C98 C99 H99A 111.7 . . ? C100 C99 H99A 111.7 . . ? C98 C99 H99B 111.7 . . ? C100 C99 H99B 111.7 . . ? H99A C99 H99B 109.4 . . ? N4 C100 C99 104.0(12) . . ? N4 C100 H10A 111.0 . . ? C99 C100 H10A 111.0 . . ? N4 C100 H10B 111.0 . . ? C99 C100 H10B 111.0 . . ? H10A C100 H10B 109.0 . . ? O20 C101 O19 122.1(11) . . ? O20 C101 C102 121.2(10) . . ? O19 C101 C102 116.6(10) . . ? N3 C102 C101 111.7(9) . . ? N3 C102 C103 108.9(11) . . ? C101 C102 C103 113.0(11) . . ? N3 C102 H102 107.7 . . ? C101 C102 H102 107.7 . . ? C103 C102 H102 107.7 . . ? C102 C103 C104 104.2(11) . . ? C102 C103 H10C 110.9 . . ? C104 C103 H10C 110.9 . . ? C102 C103 H10D 110.9 . . ? C104 C103 H10D 110.9 . . ? H10C C103 H10D 108.9 . . ? C105 C104 C103 102.9(11) . . ? C105 C104 H10E 111.2 . . ? C103 C104 H10E 111.2 . . ? C105 C104 H10F 111.2 . . ? C103 C104 H10F 111.2 . . ? H10E C104 H10F 109.1 . . ? N3 C105 C104 106.0(10) . . ? N3 C105 H10G 110.5 . . ? C104 C105 H10G 110.5 . . ? N3 C105 H10H 110.5 . . ? C104 C105 H10H 110.5 . . ? H10G C105 H10H 108.7 . . ? O16 C106 O15 124.9(11) . . ? O16 C106 C107 119.1(10) . . ? O15 C106 C107 115.9(10) . . ? N2 C107 C106 112.5(9) . . ? N2 C107 C108 105.1(9) . . ? C106 C107 C108 112.2(11) . . ? N2 C107 H107 109.0 . . ? C106 C107 H107 109.0 . . ? C108 C107 H107 109.0 . . ? C109 C108 C107 106.3(10) . . ? C109 C108 H10I 110.5 . . ? C107 C108 H10I 110.5 . . ? C109 C108 H10J 110.5 . . ? C107 C108 H10J 110.5 . . ? H10I C108 H10J 108.7 . . ? C110 C109 C108 101.9(11) . . ? C110 C109 H10K 111.4 . . ? C108 C109 H10K 111.4 . . ? C110 C109 H10L 111.4 . . ? C108 C109 H10L 111.4 . . ? H10K C109 H10L 109.3 . . ? N2 C110 C109 108.6(11) . . ? N2 C110 H11A 110.0 . . ? C109 C110 H11A 110.0 . . ? N2 C110 H11B 110.0 . . ? C109 C110 H11B 110.0 . . ? H11A C110 H11B 108.4 . . ? Cl1 C111 Cl2 110.1(10) . . ? Cl1 C111 H11H 109.6 . . ? Cl2 C111 H11H 109.6 . . ? Cl1 C111 H11I 109.6 . . ? Cl2 C111 H11I 109.6 . . ? H11H C111 H11I 108.1 . . ? Cl4 C112 Cl3 111.7(13) . . ? Cl4 C112 H11F 109.3 . . ? Cl3 C112 H11F 109.3 . . ? Cl4 C112 H11G 109.3 . . ? Cl3 C112 H11G 109.3 . . ? H11F C112 H11G 107.9 . . ? O26 C114 H11C 109.5 . . ? O26 C114 H11D 109.5 . . ? H11C C114 H11D 109.5 . . ? O26 C114 H11E 109.5 . . ? H11C C114 H11E 109.5 . . ? H11D C114 H11E 109.5 . . ? C114 O26 H26A 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 O8 1.00 2.06 2.932(13) 145.2 . N2 H2 O12 1.00 1.90 2.837(13) 155.5 . N3 H3 O16 1.00 2.25 2.953(13) 126.5 . N4 H4 O20 1.00 1.97 2.887(14) 152.0 . O26 H26A O8 0.84 2.12 2.737(16) 130.2 . _refine_diff_density_max 0.682 _refine_diff_density_min -1.662 _refine_diff_density_rms 0.115 _database_code_depnum_ccdc_archive 'CCDC 915213' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_4 _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C146 H119 Dy5 N4 O25, 5(C7 H8), 0.5(H2 O)' _chemical_formula_sum 'C181 H160 Dy5 N4 O25.5' _chemical_formula_weight 3611.62 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' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 16.8080(11) _cell_length_b 18.5842(11) _cell_length_c 26.0343(15) _cell_angle_alpha 83.712(5) _cell_angle_beta 74.534(5) _cell_angle_gamma 75.964(5) _cell_volume 7594.9(8) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 10822 _cell_measurement_theta_min 1.29 _cell_measurement_theta_max 25.10 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.579 _exptl_crystal_F_000 3616 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.110 _exptl_crystal_size_mid 0.050 _exptl_crystal_size_min 0.030 _exptl_absorpt_coefficient_mu 2.504 _shelx_estimated_absorpt_T_min 0.770 _shelx_estimated_absorpt_T_max 0.929 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.533 _exptl_absorpt_correction_T_max 0.717 _exptl_absorpt_process_details 'STOE X-RED & X-SHAPE' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean 6.667 _diffrn_reflns_number 38778 _diffrn_reflns_av_unetI/netI 0.2411 _diffrn_reflns_av_R_equivalents 0.1255 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.887 _diffrn_reflns_theta_max 20.816 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measured_fraction_theta_full 0.577 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_Laue_measured_fraction_full 0.577 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_point_group_measured_fraction_full 0.577 _reflns_number_total 15870 _reflns_number_gt 6790 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. The small crystal was weakly diffracting, and also appeared to be twinned, preventing a full refinement of the structure. However, the structure obtained was sufficient to show that the compound was isostructural to its analogues. The data were truncated at 0.90 Ang, as there was no significant intensity at higher angles. ; _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA, PLATON (A.L.Spek, 2005)' _computing_data_reduction 'STOE X-RED, PLATON (A.L.Spek, 2005)' _computing_structure_solution 'SHELXS-2013 (Sheldrick, 2013)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _refine_special_details ; Many of the phenyl rings were disordered and could be split into two partial- occupancy rings, which were refined as rigid hexagons. Other ligands showed unresolved disorder or high thermal motion, and could be refined using rigid- bond restraints on the thermal parameters. Four lattice toluenes per cluster were badly disordered, and were handled using SQUEEZE (see below) to keep the data:parameter ration from becoming too low. ; # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 -0.004 0.500 1159 402 '8 toluene (= 400 e)' 2 0.144 0.234 0.900 17 4 ' ' 3 0.856 0.766 0.100 17 3 ' ' _platon_squeeze_details ; Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13 ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0116P)^2^] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 15870 _refine_ls_number_parameters 1407 _refine_ls_number_restraints 138 _refine_ls_R_factor_all 0.1304 _refine_ls_R_factor_gt 0.0519 _refine_ls_wR_factor_ref 0.1008 _refine_ls_wR_factor_gt 0.0833 _refine_ls_goodness_of_fit_ref 0.663 _refine_ls_restrained_S_all 0.662 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 0.63401(5) 0.39274(4) 0.14385(3) 0.0437(2) Uani 1 1 d . . . . . Dy2 Dy 0.49379(5) 0.26556(4) 0.22221(4) 0.0424(2) Uani 1 1 d . U . . . Dy3 Dy 0.71302(5) 0.18263(4) 0.16731(4) 0.0434(2) Uani 1 1 d . U . . . Dy4 Dy 0.77252(5) 0.30499(4) 0.24011(3) 0.0423(2) Uani 1 1 d . U . . . Dy5 Dy 0.55303(5) 0.38925(4) 0.29556(3) 0.0426(2) Uani 1 1 d . U . . . O21 O 0.6663(3) 0.4066(2) 0.22680(18) 0.043(3) Uani 1 1 d . . . . . H21 H 0.6817 0.4551 0.2278 0.052 Uiso 1 1 calc R U . . . O22 O 0.5148(3) 0.3868(2) 0.21664(18) 0.037(3) Uani 1 1 d R . . . . H22 H 0.4633 0.4257 0.2136 0.044 Uiso 1 1 calc R U . . . O23 O 0.6008(3) 0.2721(2) 0.14653(18) 0.045(3) Uani 1 1 d R . . . . H23 H 0.5868 0.2624 0.1133 0.054 Uiso 1 1 calc R U . . . O24 O 0.7557(3) 0.2930(2) 0.15737(18) 0.043(3) Uani 1 1 d R . . . . H24 H 0.8084 0.2931 0.1283 0.052 Uiso 1 1 calc R U . . . O25 O 0.6309(3) 0.2672(2) 0.24574(18) 0.037(2) Uani 1 1 d R U . . . H25 H 0.6275 0.2296 0.2764 0.044 Uiso 1 1 calc R U . . . O1 O 0.5381(7) 0.4032(6) 0.0924(5) 0.062(3) Uani 1 1 d . U . . . O2 O 0.5574(7) 0.5132(5) 0.1506(4) 0.052(3) Uani 1 1 d . . . . . O3 O 0.7122(8) 0.3636(6) 0.0591(4) 0.053(3) Uani 1 1 d . . . . . O4 O 0.7332(8) 0.4619(7) 0.1226(5) 0.061(4) Uani 1 1 d . . . . . O5 O 0.3728(7) 0.3503(6) 0.2158(4) 0.052(3) Uani 1 1 d . . . . . O6 O 0.4417(7) 0.2178(5) 0.1669(4) 0.049(3) Uani 1 1 d . . . . . O7 O 0.4676(6) 0.2975(5) 0.3123(4) 0.039(3) Uani 1 1 d . . . . . O8 O 0.3864(7) 0.3106(7) 0.3975(5) 0.068(4) Uani 1 1 d . . . . . O9 O 0.6900(7) 0.1464(6) 0.0923(5) 0.055(3) Uani 1 1 d . . . . . O10 O 0.8466(6) 0.1430(5) 0.1099(5) 0.043(3) Uani 1 1 d . U . . . O11 O 0.5916(6) 0.1428(5) 0.2174(4) 0.045(3) Uani 1 1 d . . . . . O12 O 0.5100(7) 0.0623(6) 0.2249(5) 0.064(4) Uani 1 1 d . . . . . O13 O 0.8990(7) 0.3133(6) 0.1772(4) 0.057(3) Uani 1 1 d . . . . . O14 O 0.8245(7) 0.3912(6) 0.2692(4) 0.052(3) Uani 1 1 d . . . . . O15 O 0.7917(6) 0.1766(5) 0.2332(4) 0.043(3) Uani 1 1 d . . . . . O16 O 0.8775(9) 0.0640(7) 0.2272(6) 0.088(5) Uani 1 1 d . . . . . O17 O 0.5827(7) 0.4980(6) 0.3069(5) 0.064(4) Uani 1 1 d . U . . . O18 O 0.4244(6) 0.4721(6) 0.3171(4) 0.049(3) Uani 1 1 d . . . . . O19 O 0.6711(6) 0.3222(5) 0.3269(4) 0.041(3) Uani 1 1 d . . . . . O20 O 0.7483(7) 0.2996(7) 0.3871(4) 0.072(4) Uani 1 1 d . . . . . N1 N 0.4174(4) 0.1868(3) 0.2932(2) 0.065(4) Uani 1 1 d . . . . . H11 H 0.3804 0.1662 0.2776 0.078 Uiso 1 1 calc R U . . . H12 H 0.4599 0.1443 0.3031 0.078 Uiso 1 1 calc R U . . . N2 N 0.7359(4) 0.0430(3) 0.1856(2) 0.051(4) Uani 1 1 d R . . . . H221 H 0.7623 0.0189 0.1512 0.061 Uiso 1 1 calc R U . . . H231 H 0.7770 0.0278 0.2080 0.061 Uiso 1 1 calc R U . . . N3 N 0.8714(4) 0.2262(3) 0.2929(2) 0.049(4) Uani 1 1 d R . . . . H31 H 0.9225 0.2470 0.2852 0.059 Uiso 1 1 calc R U . . . H32 H 0.8433 0.2326 0.3312 0.059 Uiso 1 1 calc R U . . . N4 N 0.5268(4) 0.3793(3) 0.3946(2) 0.049(4) Uani 1 1 d R . . . . H41 H 0.5041 0.4302 0.4076 0.059 Uiso 1 1 calc R U . . . H42 H 0.4814 0.3517 0.4086 0.059 Uiso 1 1 calc R U . . . C1 C 0.3771(4) 0.4773(3) 0.0243(2) 0.068(6) Uani 1 1 d R . . . . H1 H 0.3620 0.5277 0.0336 0.082 Uiso 1 1 calc R U . . . C2 C 0.3380(12) 0.4564(11) -0.0108(8) 0.078(6) Uani 1 1 d . . . . . H2 H 0.2912 0.4894 -0.0209 0.094 Uiso 1 1 calc R U . . . C3 C 0.3695(14) 0.3857(11) -0.0307(7) 0.073(6) Uani 1 1 d . . . . . H3 H 0.3473 0.3697 -0.0563 0.087 Uiso 1 1 calc R U . . . C4 C 0.4312(17) 0.3422(12) -0.0126(9) 0.093(8) Uani 1 1 d . . . . . H4 H 0.4549 0.2944 -0.0266 0.112 Uiso 1 1 calc R U . . . C5 C 0.4630(14) 0.3626(10) 0.0256(9) 0.084(7) Uani 1 1 d . . . . . H5 H 0.5060 0.3280 0.0383 0.101 Uiso 1 1 calc R U . . . C6 C 0.4347(12) 0.4301(11) 0.0453(7) 0.060(5) Uani 1 1 d . U . . . C7 C 0.4742(12) 0.4509(10) 0.0835(7) 0.053(4) Uani 1 1 d . U . . . C8 C 0.4449(12) 0.5217(10) 0.1081(8) 0.070(6) Uani 1 1 d . U . . . H8 H 0.3940 0.5532 0.1024 0.084 Uiso 1 1 calc R U . . . C9 C 0.4885(12) 0.5475(12) 0.1409(7) 0.065(6) Uani 1 1 d . . . . . C10 C 0.4468(15) 0.6223(9) 0.1660(9) 0.078(6) Uani 1 1 d . U . . . C11 C 0.4967(14) 0.6622(10) 0.1773(8) 0.076(6) Uani 1 1 d . U . . . H11A H 0.5549 0.6390 0.1730 0.091 Uiso 1 1 calc R U . . . C12 C 0.4712(19) 0.7321(12) 0.1941(10) 0.110(8) Uani 1 1 d . U . . . H12A H 0.5101 0.7602 0.1968 0.133 Uiso 1 1 calc R U . . . C13 C 0.382(2) 0.7608(11) 0.2076(10) 0.123(10) Uani 1 1 d . U . . . H13 H 0.3580 0.8083 0.2220 0.148 Uiso 1 1 calc R U . . . C14 C 0.3317(19) 0.7182(17) 0.1993(11) 0.146(11) Uani 1 1 d . U . . . H14 H 0.2718 0.7344 0.2096 0.175 Uiso 1 1 calc R U . . . C15 C 0.3670(16) 0.6538(13) 0.1766(10) 0.102(7) Uani 1 1 d . U . . . H15 H 0.3305 0.6286 0.1672 0.122 Uiso 1 1 calc R U . . . C16 C 0.7695(17) 0.3115(11) -0.0363(12) 0.088(8) Uani 1 1 d . . . . . H16 H 0.7125 0.3244 -0.0158 0.105 Uiso 1 1 calc R U . . . C17 C 0.784(2) 0.2809(13) -0.0824(16) 0.106(9) Uani 1 1 d . . . . . H17 H 0.7382 0.2757 -0.0956 0.127 Uiso 1 1 calc R U . . . C18 C 0.866(3) 0.2569(13) -0.1109(10) 0.115(11) Uani 1 1 d . . . . . H18 H 0.8780 0.2380 -0.1452 0.137 Uiso 1 1 calc R U . . . C19 C 0.9283(17) 0.2600(13) -0.0904(11) 0.096(8) Uani 1 1 d . . . . . H19 H 0.9853 0.2379 -0.1072 0.115 Uiso 1 1 calc R U . . . C20 C 0.9085(14) 0.2965(10) -0.0437(9) 0.071(6) Uani 1 1 d . . . . . H20 H 0.9532 0.3020 -0.0295 0.085 Uiso 1 1 calc R U . . . C21 C 0.8268(16) 0.3250(10) -0.0172(7) 0.060(6) Uani 1 1 d . . . . . C22 C 0.7888(15) 0.3627(10) 0.0341(10) 0.075(7) Uani 1 1 d . . . . . C23 C 0.8385(13) 0.4056(11) 0.0475(8) 0.075(6) Uani 1 1 d . . . . . H23A H 0.8947 0.4034 0.0266 0.090 Uiso 1 1 calc R U . . . C24 C 0.8047(17) 0.4536(10) 0.0935(10) 0.075(7) Uani 1 1 d . . . . . C25 C 0.8602(13) 0.5072(10) 0.1013(8) 0.057(5) Uani 1 1 d . . . . . C26 C 0.9406(16) 0.5098(15) 0.0706(8) 0.103(8) Uani 1 1 d . . . . . H26 H 0.9665 0.4819 0.0396 0.123 Uiso 1 1 calc R U . . . C27 C 0.9807(17) 0.5559(15) 0.0879(11) 0.116(10) Uani 1 1 d . . . . . H27 H 1.0376 0.5553 0.0688 0.139 Uiso 1 1 calc R U . . . C28 C 0.9487(15) 0.6001(14) 0.1276(12) 0.093(8) Uani 1 1 d . . . . . H28 H 0.9800 0.6322 0.1352 0.112 Uiso 1 1 calc R U . . . C29 C 0.870(2) 0.5988(12) 0.1577(10) 0.116(9) Uani 1 1 d . . . . . H29 H 0.8445 0.6281 0.1880 0.139 Uiso 1 1 calc R U . . . C30 C 0.8232(14) 0.5488(13) 0.1410(11) 0.105(8) Uani 1 1 d . . . . . H30 H 0.7665 0.5481 0.1598 0.126 Uiso 1 1 calc R U . . . C31 C 0.8633(12) 0.4555(11) 0.3466(8) 0.072(6) Uani 1 1 d . . . . . H31A H 0.8197 0.4285 0.3568 0.086 Uiso 1 1 calc R U . . . C32 C 0.8783(14) 0.4954(13) 0.3860(9) 0.101(8) Uani 1 1 d . . . . . H32A H 0.8508 0.4893 0.4226 0.121 Uiso 1 1 calc R U . . . C33 C 0.9337(15) 0.5432(13) 0.3698(14) 0.122(11) Uani 1 1 d . . . . . H33 H 0.9399 0.5754 0.3937 0.146 Uiso 1 1 calc R U . . . C34 C 0.9781(14) 0.5413(14) 0.3182(11) 0.105(9) Uani 1 1 d . . . . . H34 H 1.0207 0.5692 0.3077 0.126 Uiso 1 1 calc R U . . . C35 C 0.9673(11) 0.5025(9) 0.2792(8) 0.063(5) Uani 1 1 d . . . . . H35 H 0.9974 0.5075 0.2430 0.076 Uiso 1 1 calc R U . . . C36 C 0.9098(11) 0.4551(10) 0.2951(9) 0.063(6) Uani 1 1 d . . . . . C37 C 0.8985(12) 0.4094(8) 0.2557(9) 0.063(6) Uani 1 1 d . . . . . C38 C 0.9651(11) 0.3869(9) 0.2104(7) 0.059(5) Uani 1 1 d . . . . . H38 H 1.0159 0.4034 0.2062 0.071 Uiso 1 1 calc R U . . . C39 C 0.9627(10) 0.3434(8) 0.1720(7) 0.043(4) Uani 1 1 d . . . . . C40 C 1.0255(10) 0.3273(11) 0.1191(8) 0.060(5) Uani 1 1 d . . . . . C41 C 1.0857(12) 0.3705(12) 0.1050(8) 0.083(6) Uani 1 1 d . . . . . H41A H 1.0868 0.4053 0.1287 0.100 Uiso 1 1 calc R U . . . C42 C 1.1462(13) 0.3618(11) 0.0540(9) 0.082(7) Uani 1 1 d . . . . . H42A H 1.1887 0.3899 0.0431 0.099 Uiso 1 1 calc R U . . . C43 C 1.1395(12) 0.3128(12) 0.0232(9) 0.078(6) Uani 1 1 d . . . . . H43 H 1.1800 0.3062 -0.0102 0.094 Uiso 1 1 calc R U . . . C44 C 1.0806(11) 0.2709(11) 0.0343(7) 0.067(6) Uani 1 1 d . . . . . H44 H 1.0796 0.2373 0.0097 0.080 Uiso 1 1 calc R U . . . C45 C 1.0222(11) 0.2793(10) 0.0830(10) 0.075(6) Uani 1 1 d . . . . . H45 H 0.9792 0.2517 0.0919 0.089 Uiso 1 1 calc R U . . . C46 C 1.0177(12) 0.0807(8) 0.0765(8) 0.062(5) Uani 1 1 d . . . . . H46 H 0.9907 0.0820 0.1135 0.075 Uiso 1 1 calc R U . . . C47 C 1.1047(13) 0.0597(10) 0.0623(10) 0.075(6) Uani 1 1 d . . . . . H47 H 1.1376 0.0462 0.0878 0.090 Uiso 1 1 calc R U . . . C48 C 1.1389(14) 0.0598(10) 0.0097(10) 0.072(6) Uani 1 1 d . . . . . H48 H 1.1987 0.0433 -0.0019 0.086 Uiso 1 1 calc R U . . . C49 C 1.0966(11) 0.0810(9) -0.0275(8) 0.060(5) Uani 1 1 d . . . . . H49 H 1.1259 0.0828 -0.0641 0.072 Uiso 1 1 calc R U . . . C50 C 1.0057(11) 0.1011(9) -0.0118(8) 0.066(5) Uani 1 1 d . . . . . H50 H 0.9738 0.1149 -0.0378 0.079 Uiso 1 1 calc R U . . . C51 C 0.9662(11) 0.1001(8) 0.0414(7) 0.044(4) Uani 1 1 d . U . . . C52 C 0.8696(10) 0.1229(7) 0.0625(7) 0.038(4) Uani 1 1 d . U . . . C53 C 0.8200(11) 0.1207(8) 0.0298(7) 0.054(5) Uani 1 1 d . U . . . H53 H 0.8464 0.1100 -0.0065 0.065 Uiso 1 1 calc R U . . . C54 C 0.7331(11) 0.1332(8) 0.0464(8) 0.042(4) Uani 1 1 d . . . . . C55 C 0.6827(9) 0.1285(7) 0.0066(7) 0.046(4) Uani 1 1 d . U . . . C56 C 0.7148(11) 0.1221(8) -0.0490(7) 0.055(4) Uani 1 1 d . U . . . H56 H 0.7742 0.1148 -0.0634 0.065 Uiso 1 1 calc R U . . . C57 C 0.6641(12) 0.1261(9) -0.0834(8) 0.064(5) Uani 1 1 d . U . . . H57 H 0.6881 0.1210 -0.1206 0.077 Uiso 1 1 calc R U . . . C58 C 0.5798(11) 0.1371(9) -0.0632(7) 0.059(5) Uani 1 1 d . U . . . H58 H 0.5447 0.1414 -0.0871 0.071 Uiso 1 1 calc R U . . . C59 C 0.5442(11) 0.1423(9) -0.0123(7) 0.062(5) Uani 1 1 d . U . . . H59 H 0.4846 0.1485 0.0006 0.074 Uiso 1 1 calc R U . . . C60 C 0.5951(10) 0.1387(8) 0.0232(7) 0.052(4) Uani 1 1 d . U . . . H60 H 0.5686 0.1435 0.0602 0.063 Uiso 1 1 calc R U . . . C61 C 0.4029(11) 0.1087(9) 0.1234(8) 0.059(5) Uani 1 1 d . U . . . H61 H 0.4371 0.0962 0.1482 0.071 Uiso 1 1 calc R U . . . C62 C 0.3931(12) 0.0532(9) 0.0940(8) 0.060(5) Uani 1 1 d . . . . . H62 H 0.4234 0.0035 0.0979 0.073 Uiso 1 1 calc R U . . . C63 C 0.3414(12) 0.0693(11) 0.0603(8) 0.069(6) Uani 1 1 d . . . . . H63 H 0.3353 0.0306 0.0416 0.083 Uiso 1 1 calc R U . . . C64 C 0.2983(12) 0.1398(11) 0.0528(8) 0.074(6) Uani 1 1 d . . . . . H64 H 0.2594 0.1502 0.0309 0.089 Uiso 1 1 calc R U . . . C65 C 0.3118(10) 0.1968(9) 0.0777(7) 0.053(4) Uani 1 1 d . U . . . H65 H 0.2873 0.2470 0.0693 0.063 Uiso 1 1 calc R U . . . C66 C 0.3621(9) 0.1809(9) 0.1156(6) 0.047(4) Uani 1 1 d . U . . . C67 C 0.3765(11) 0.2378(8) 0.1458(7) 0.049(4) Uani 1 1 d . U . . . C68 C 0.3166(10) 0.3048(8) 0.1535(6) 0.046(4) Uani 1 1 d . U . . . H68 H 0.2721 0.3147 0.1359 0.056 Uiso 1 1 calc R U . . . C69 C 0.3204(11) 0.3599(8) 0.1878(6) 0.048(4) Uani 1 1 d . U . . . C70 C 0.2630(8) 0.4341(8) 0.1862(6) 0.038(4) Uani 1 1 d . U . . . C71 C 0.2464(10) 0.4789(9) 0.2296(7) 0.058(5) Uani 1 1 d . U . . . H71 H 0.2717 0.4591 0.2581 0.070 Uiso 1 1 calc R U . . . C72 C 0.1973(13) 0.5478(10) 0.2335(8) 0.076(7) Uani 1 1 d . . . . . H72 H 0.1904 0.5763 0.2632 0.091 Uiso 1 1 calc R U . . . C73 C 0.1582(11) 0.5756(9) 0.1944(8) 0.061(5) Uani 1 1 d . . . . . H73 H 0.1191 0.6224 0.1982 0.073 Uiso 1 1 calc R U . . . C74 C 0.1740(11) 0.5369(10) 0.1484(8) 0.064(6) Uani 1 1 d . . . . . H74 H 0.1504 0.5597 0.1197 0.077 Uiso 1 1 calc R U . . . C75 C 0.2238(11) 0.4659(10) 0.1444(7) 0.060(5) Uani 1 1 d . U . . . H75 H 0.2319 0.4385 0.1140 0.072 Uiso 1 1 calc R U . . . C76 C 0.2556(10) 0.5221(10) 0.3619(6) 0.050(4) Uani 1 1 d . U . . . H76 H 0.2783 0.4701 0.3647 0.060 Uiso 1 1 calc R U . . . C77 C 0.1648(12) 0.5535(13) 0.3798(9) 0.084(6) Uani 1 1 d . U . . . H77 H 0.1265 0.5218 0.3933 0.101 Uiso 1 1 calc R U . . . C78 C 0.1372(16) 0.6239(15) 0.3770(11) 0.114(9) Uani 1 1 d . U . . . H78 H 0.0790 0.6423 0.3934 0.136 Uiso 1 1 calc R U . . . C79 C 0.1808(15) 0.6730(13) 0.3540(11) 0.108(8) Uani 1 1 d . U . . . H79 H 0.1544 0.7237 0.3491 0.129 Uiso 1 1 calc R U . . . C80 C 0.2717(12) 0.6463(10) 0.3363(9) 0.084(6) Uani 1 1 d . U . . . H80 H 0.3071 0.6801 0.3215 0.101 Uiso 1 1 calc R U . . . C81 C 0.3064(10) 0.5708(10) 0.3411(6) 0.051(4) Uani 1 1 d . U . . . C82 C 0.4028(10) 0.5439(11) 0.3244(7) 0.054(5) Uani 1 1 d . . . . . C83 C 0.4545(10) 0.5907(8) 0.3246(6) 0.046(4) Uani 1 1 d . U . . . H83 H 0.4301 0.6413 0.3325 0.055 Uiso 1 1 calc R U . . . C84 C 0.5463(10) 0.5641(9) 0.3129(7) 0.046(4) Uani 1 1 d . U . . . C85 C 0.5943(11) 0.6207(10) 0.3128(7) 0.059(5) Uani 1 1 d . U . . . C86 C 0.5709(15) 0.6963(10) 0.3131(10) 0.098(8) Uani 1 1 d . . . . . H86 H 0.5132 0.7169 0.3136 0.117 Uiso 1 1 calc R U . . . C87 C 0.6163(16) 0.7450(13) 0.3129(11) 0.114(10) Uani 1 1 d . . . . . H87 H 0.5908 0.7964 0.3158 0.137 Uiso 1 1 calc R U . . . C88 C 0.7029(16) 0.7190(12) 0.3082(9) 0.101(8) Uani 1 1 d . . . . . H88 H 0.7387 0.7523 0.3056 0.121 Uiso 1 1 calc R U . . . C89 C 0.7356(14) 0.6413(13) 0.3075(10) 0.104(8) Uani 1 1 d . . . . . H89 H 0.7936 0.6207 0.3060 0.125 Uiso 1 1 calc R U . . . C90 C 0.6823(12) 0.5980(11) 0.3089(9) 0.093(8) Uani 1 1 d . . . . . H90 H 0.7060 0.5461 0.3070 0.111 Uiso 1 1 calc R U . . . C91 C 0.8541(13) 0.1258(12) 0.2456(7) 0.058(5) Uani 1 1 d . . . . . C92 C 0.9007(11) 0.1442(8) 0.2849(7) 0.059(5) Uani 1 1 d D . . . . C93A C 0.9982(8) 0.1339(11) 0.2550(8) 0.051(11) Uiso 0.68 1 d DG U P A 1 C94A C 1.0269(11) 0.1483(12) 0.2005(8) 0.076(11) Uiso 0.68 1 d G U P A 1 H94A H 0.9882 0.1596 0.1785 0.091 Uiso 0.68 1 calc R U P A 1 C95A C 1.1123(13) 0.1463(11) 0.1783(7) 0.080(13) Uiso 0.68 1 d G U P A 1 H95A H 1.1320 0.1561 0.1410 0.096 Uiso 0.68 1 calc R U P A 1 C96A C 1.1690(8) 0.1298(11) 0.2105(10) 0.107(11) Uiso 0.68 1 d G . P A 1 H96A H 1.2273 0.1284 0.1953 0.128 Uiso 0.68 1 calc R U P A 1 C97A C 1.1402(12) 0.1154(11) 0.2650(9) 0.136(14) Uiso 0.68 1 d G . P A 1 H97A H 1.1789 0.1042 0.2870 0.163 Uiso 0.68 1 calc R U P A 1 C98A C 1.0548(13) 0.1175(10) 0.2873(7) 0.085(9) Uiso 0.68 1 d G . P A 1 H98A H 1.0352 0.1077 0.3245 0.102 Uiso 0.68 1 calc R U P A 1 C93B C 0.9987(12) 0.123(2) 0.2571(16) 0.06(2) Uiso 0.32 1 d DG U P A 2 C94B C 1.0312(18) 0.164(2) 0.2114(17) 0.060(17) Uiso 0.32 1 d G U P A 2 H94B H 0.9955 0.2058 0.1987 0.072 Uiso 0.32 1 calc R U P A 2 C95B C 1.1157(19) 0.1422(19) 0.1841(13) 0.08(3) Uiso 0.32 1 d G U P A 2 H95B H 1.1379 0.1697 0.1529 0.095 Uiso 0.32 1 calc R U P A 2 C96B C 1.1679(12) 0.0804(18) 0.2026(13) 0.024(10) Uiso 0.32 1 d G . P A 2 H96B H 1.2257 0.0658 0.1839 0.029 Uiso 0.32 1 calc R U P A 2 C97B C 1.1354(19) 0.0400(17) 0.2483(14) 0.16(4) Uiso 0.32 1 d G . P A 2 H97B H 1.1710 -0.0022 0.2609 0.190 Uiso 0.32 1 calc R U P A 2 C98B C 1.051(2) 0.061(2) 0.2755(12) 0.054(14) Uiso 0.32 1 d G . P A 2 H98B H 1.0287 0.0339 0.3067 0.064 Uiso 0.32 1 calc R U P A 2 C99 C 0.8920(12) 0.0918(9) 0.3330(8) 0.049(7) Uiso 0.68 1 d G U P A 1 C100 C 0.9274(12) 0.0171(11) 0.3243(7) 0.072(8) Uiso 0.68 1 d G . P A 1 H100 H 0.9582 0.0019 0.2895 0.086 Uiso 0.68 1 calc R U P A 1 C101 C 0.9177(14) -0.0355(8) 0.3664(10) 0.138(14) Uiso 0.68 1 d G . P A 1 H101 H 0.9419 -0.0866 0.3604 0.166 Uiso 0.68 1 calc R U P A 1 C102 C 0.8726(15) -0.0134(12) 0.4173(8) 0.125(13) Uiso 0.68 1 d G . P A 1 H102 H 0.8660 -0.0493 0.4461 0.150 Uiso 0.68 1 calc R U P A 1 C103 C 0.8372(13) 0.0614(13) 0.4261(7) 0.102(12) Uiso 0.68 1 d G . P A 1 H103 H 0.8064 0.0765 0.4608 0.122 Uiso 0.68 1 calc R U P A 1 C104 C 0.8469(12) 0.1140(9) 0.3839(9) 0.084(10) Uiso 0.68 1 d G . P A 1 H104 H 0.8227 0.1651 0.3899 0.101 Uiso 0.68 1 calc R U P A 1 C199 C 0.872(2) 0.112(2) 0.3456(13) 0.063(17) Uiso 0.32 1 d G U P A 2 C200 C 0.830(3) 0.054(2) 0.3568(17) 0.065(17) Uiso 0.32 1 d G . P A 2 H200 H 0.8151 0.0350 0.3291 0.078 Uiso 0.32 1 calc R U P A 2 C201 C 0.811(3) 0.023(2) 0.408(2) 0.11(3) Uiso 0.32 1 d G . P A 2 H201 H 0.7829 -0.0169 0.4161 0.130 Uiso 0.32 1 calc R U P A 2 C202 C 0.834(3) 0.050(3) 0.4489(15) 0.18(5) Uiso 0.32 1 d G . P A 2 H202 H 0.8205 0.0292 0.4843 0.217 Uiso 0.32 1 calc R U P A 2 C203 C 0.875(3) 0.109(2) 0.4377(14) 0.08(2) Uiso 0.32 1 d G . P A 2 H203 H 0.8903 0.1273 0.4654 0.100 Uiso 0.32 1 calc R U P A 2 C204 C 0.894(2) 0.1394(18) 0.3861(16) 0.046(13) Uiso 0.32 1 d G . P A 2 H204 H 0.9225 0.1792 0.3784 0.055 Uiso 0.32 1 calc R U P A 2 C105 C 0.5824(14) 0.0750(10) 0.2151(8) 0.067(6) Uani 1 1 d . . . . . C106 C 0.6583(10) 0.0129(8) 0.2128(7) 0.050(5) Uani 1 1 d D . . . . C107 C 0.6537(9) -0.0480(9) 0.1784(8) 0.050(5) Uani 1 1 d . . . . . C108 C 0.6322(10) -0.0296(10) 0.1302(8) 0.058(5) Uani 1 1 d . . . . . H108 H 0.6178 0.0215 0.1196 0.069 Uiso 1 1 calc R U . . . C109 C 0.6304(14) -0.0812(15) 0.0969(9) 0.093(7) Uani 1 1 d . . . . . H109 H 0.6140 -0.0668 0.0644 0.112 Uiso 1 1 calc R U . . . C110 C 0.6536(16) -0.1546(13) 0.1127(12) 0.104(9) Uani 1 1 d . . . . . H110 H 0.6533 -0.1923 0.0909 0.125 Uiso 1 1 calc R U . . . C111 C 0.676(2) -0.1725(14) 0.1568(13) 0.145(14) Uani 1 1 d . . . . . H111 H 0.6937 -0.2238 0.1654 0.174 Uiso 1 1 calc R U . . . C112 C 0.6750(16) -0.1220(11) 0.1929(10) 0.108(9) Uani 1 1 d . . . . . H112 H 0.6888 -0.1382 0.2261 0.130 Uiso 1 1 calc R U . . . C113 C 0.6599(16) -0.0159(11) 0.2713(6) 0.043(18) Uiso 0.57 1 d DG U P B 1 C114 C 0.7365(13) -0.0537(12) 0.2819(8) 0.067(10) Uiso 0.57 1 d G . P B 1 H114 H 0.7874 -0.0580 0.2544 0.081 Uiso 0.57 1 calc R U P B 1 C115 C 0.7385(14) -0.0850(12) 0.3326(10) 0.081(11) Uiso 0.57 1 d G . P B 1 H115 H 0.7908 -0.1108 0.3399 0.097 Uiso 0.57 1 calc R U P B 1 C116 C 0.6639(18) -0.0787(14) 0.3727(7) 0.097(17) Uiso 0.57 1 d G . P B 1 H116 H 0.6653 -0.1002 0.4074 0.117 Uiso 0.57 1 calc R U P B 1 C117 C 0.5874(14) -0.0410(15) 0.3621(8) 0.100(15) Uiso 0.57 1 d G . P B 1 H117 H 0.5365 -0.0366 0.3896 0.120 Uiso 0.57 1 calc R U P B 1 C118 C 0.5854(12) -0.0096(12) 0.3114(10) 0.095(13) Uiso 0.57 1 d G . P B 1 H118 H 0.5331 0.0162 0.3042 0.114 Uiso 0.57 1 calc R U P B 1 C213 C 0.6606(19) -0.0188(14) 0.2700(7) 0.04(2) Uiso 0.43 1 d DG U P B 2 C214 C 0.7208(16) -0.0069(14) 0.2939(10) 0.064(13) Uiso 0.43 1 d G . P B 2 H214 H 0.7657 0.0149 0.2736 0.077 Uiso 0.43 1 calc R U P B 2 C215 C 0.7152(17) -0.0270(16) 0.3475(10) 0.075(13) Uiso 0.43 1 d G . P B 2 H215 H 0.7563 -0.0189 0.3639 0.091 Uiso 0.43 1 calc R U P B 2 C216 C 0.650(2) -0.0590(18) 0.3773(6) 0.10(2) Uiso 0.43 1 d G . P B 2 H216 H 0.6457 -0.0727 0.4139 0.115 Uiso 0.43 1 calc R U P B 2 C217 C 0.5894(16) -0.0709(16) 0.3533(10) 0.072(14) Uiso 0.43 1 d G . P B 2 H217 H 0.5445 -0.0927 0.3736 0.086 Uiso 0.43 1 calc R U P B 2 C218 C 0.5950(16) -0.0508(14) 0.2997(10) 0.056(11) Uiso 0.43 1 d G . P B 2 H218 H 0.5539 -0.0589 0.2833 0.068 Uiso 0.43 1 calc R U P B 2 C119 C 0.4085(12) 0.2819(10) 0.3530(10) 0.060(5) Uani 1 1 d . . . . . C120 C 0.3642(10) 0.2235(8) 0.3433(6) 0.043(4) Uani 1 1 d D . . . . C121 C 0.2767(12) 0.2614(11) 0.3360(9) 0.064(14) Uiso 0.62 1 d G U P C 1 C122 C 0.2199(16) 0.3052(13) 0.3759(8) 0.079(10) Uiso 0.62 1 d G U P C 1 H122 H 0.2354 0.3101 0.4077 0.095 Uiso 0.62 1 calc R U P C 1 C123 C 0.1404(14) 0.3418(12) 0.3693(9) 0.124(14) Uiso 0.62 1 d G . P C 1 H123 H 0.1016 0.3718 0.3966 0.149 Uiso 0.62 1 calc R U P C 1 C124 C 0.1178(12) 0.3346(12) 0.3229(10) 0.094(11) Uiso 0.62 1 d G U P C 1 H124 H 0.0635 0.3597 0.3184 0.112 Uiso 0.62 1 calc R U P C 1 C125 C 0.1746(15) 0.2908(13) 0.2830(8) 0.095(11) Uiso 0.62 1 d G . P C 1 H125 H 0.1591 0.2859 0.2513 0.115 Uiso 0.62 1 calc R U P C 1 C126 C 0.2540(14) 0.2542(11) 0.2896(8) 0.091(11) Uiso 0.62 1 d G . P C 1 H126 H 0.2928 0.2242 0.2623 0.110 Uiso 0.62 1 calc R U P C 1 C221 C 0.2769(18) 0.2547(15) 0.3318(13) 0.07(2) Uiso 0.38 1 d G U P C 2 C222 C 0.2371(18) 0.3295(14) 0.3352(12) 0.026(9) Uiso 0.38 1 d G U P C 2 H222 H 0.2629 0.3632 0.3464 0.031 Uiso 0.38 1 calc R U P C 2 C223 C 0.1597(19) 0.3550(15) 0.3223(16) 0.081(17) Uiso 0.38 1 d G . P C 2 H223 H 0.1325 0.4061 0.3246 0.098 Uiso 0.38 1 calc R U P C 2 C224 C 0.122(2) 0.306(2) 0.3059(19) 0.16(3) Uiso 0.38 1 d G U P C 2 H224 H 0.0691 0.3231 0.2971 0.198 Uiso 0.38 1 calc R U P C 2 C225 C 0.162(3) 0.231(2) 0.3025(18) 0.17(3) Uiso 0.38 1 d G . P C 2 H225 H 0.1361 0.1971 0.2913 0.200 Uiso 0.38 1 calc R U P C 2 C226 C 0.239(3) 0.2054(13) 0.3154(16) 0.066(15) Uiso 0.38 1 d G . P C 2 H226 H 0.2665 0.1542 0.3131 0.080 Uiso 0.38 1 calc R U P C 2 C127 C 0.3573(16) 0.1641(11) 0.3896(8) 0.063(11) Uiso 0.57 1 d DG U P C 1 C128 C 0.4099(14) 0.1462(12) 0.4244(10) 0.088(10) Uiso 0.57 1 d G U P C 1 H128 H 0.4477 0.1767 0.4246 0.106 Uiso 0.57 1 calc R U P C 1 C129 C 0.4072(16) 0.0838(14) 0.4589(9) 0.095(10) Uiso 0.57 1 d G U P C 1 H129 H 0.4431 0.0716 0.4827 0.114 Uiso 0.57 1 calc R U P C 1 C130 C 0.3518(19) 0.0391(11) 0.4586(10) 0.135(13) Uiso 0.57 1 d G U P C 1 H130 H 0.3500 -0.0035 0.4822 0.162 Uiso 0.57 1 calc R U P C 1 C131 C 0.2992(17) 0.0570(14) 0.4238(12) 0.141(13) Uiso 0.57 1 d G U P C 1 H131 H 0.2614 0.0265 0.4236 0.169 Uiso 0.57 1 calc R U P C 1 C132 C 0.3019(16) 0.1195(15) 0.3893(10) 0.117(12) Uiso 0.57 1 d G U P C 1 H132 H 0.2660 0.1317 0.3655 0.140 Uiso 0.57 1 calc R U P C 1 C227 C 0.349(2) 0.1629(15) 0.3879(10) 0.080(15) Uiso 0.43 1 d DG U P C 2 C228 C 0.4035(19) 0.0932(18) 0.3851(11) 0.088(12) Uiso 0.43 1 d G U P C 2 H228 H 0.4469 0.0802 0.3535 0.105 Uiso 0.43 1 calc R U P C 2 C229 C 0.394(2) 0.0423(13) 0.4284(14) 0.113(13) Uiso 0.43 1 d G U P C 2 H229 H 0.4317 -0.0054 0.4264 0.136 Uiso 0.43 1 calc R U P C 2 C230 C 0.331(2) 0.0612(17) 0.4745(11) 0.107(14) Uiso 0.43 1 d G U P C 2 H230 H 0.3248 0.0264 0.5041 0.128 Uiso 0.43 1 calc R U P C 2 C231 C 0.2766(19) 0.1309(19) 0.4774(10) 0.130(15) Uiso 0.43 1 d G U P C 2 H23B H 0.2332 0.1438 0.5089 0.157 Uiso 0.43 1 calc R U P C 2 C232 C 0.2856(19) 0.1818(13) 0.4341(13) 0.078(11) Uiso 0.43 1 d G U P C 2 H232 H 0.2484 0.2294 0.4360 0.093 Uiso 0.43 1 calc R U P C 2 C133 C 0.6802(11) 0.3202(9) 0.3721(8) 0.052(5) Uani 1 1 d . . . . . C134 C 0.5980(11) 0.3437(8) 0.4198(6) 0.054(5) Uani 1 1 d D . . . . C135 C 0.629(2) 0.4082(15) 0.4467(15) 0.060(12) Uiso 0.5 1 d G U P D 1 C136 C 0.6355(19) 0.4774(17) 0.4219(10) 0.100(17) Uiso 0.5 1 d G . P D 1 H136 H 0.6321 0.4873 0.3859 0.120 Uiso 0.5 1 calc R U P D 1 C137 C 0.6470(19) 0.5321(13) 0.4498(12) 0.075(13) Uiso 0.5 1 d G . P D 1 H137 H 0.6515 0.5794 0.4328 0.090 Uiso 0.5 1 calc R U P D 1 C138 C 0.652(2) 0.5177(16) 0.5025(12) 0.071(11) Uiso 0.5 1 d G . P D 1 H138 H 0.6599 0.5551 0.5215 0.085 Uiso 0.5 1 calc R U P D 1 C139 C 0.645(3) 0.448(2) 0.5273(11) 0.121(19) Uiso 0.5 1 d G . P D 1 H139 H 0.6488 0.4386 0.5633 0.146 Uiso 0.5 1 calc R U P D 1 C140 C 0.634(3) 0.3938(15) 0.4994(16) 0.17(3) Uiso 0.5 1 d G . P D 1 H140 H 0.6294 0.3465 0.5164 0.202 Uiso 0.5 1 calc R U P D 1 C235 C 0.6082(17) 0.3913(12) 0.4575(11) 0.035(9) Uiso 0.5 1 d G U P D 2 C236 C 0.6092(17) 0.4647(13) 0.4404(10) 0.052(10) Uiso 0.5 1 d G . P D 2 H236 H 0.5924 0.4844 0.4086 0.063 Uiso 0.5 1 calc R U P D 2 C237 C 0.635(2) 0.5092(12) 0.4696(13) 0.090(15) Uiso 0.5 1 d G . P D 2 H237 H 0.6353 0.5593 0.4579 0.108 Uiso 0.5 1 calc R U P D 2 C238 C 0.659(2) 0.4804(18) 0.5160(14) 0.088(14) Uiso 0.5 1 d G . P D 2 H238 H 0.6765 0.5108 0.5360 0.106 Uiso 0.5 1 calc R U P D 2 C239 C 0.658(3) 0.4070(19) 0.5332(12) 0.19(3) Uiso 0.5 1 d G . P D 2 H239 H 0.6749 0.3873 0.5649 0.227 Uiso 0.5 1 calc R U P D 2 C240 C 0.633(2) 0.3625(13) 0.5039(12) 0.071(12) Uiso 0.5 1 d G . P D 2 H240 H 0.6320 0.3123 0.5156 0.086 Uiso 0.5 1 calc R U P D 2 C141 C 0.581(2) 0.2836(14) 0.4649(11) 0.078(13) Uiso 0.5 1 d DG U P D 1 C142 C 0.5081(19) 0.2928(12) 0.5063(12) 0.13(2) Uiso 0.5 1 d G . P D 1 H142 H 0.4731 0.3410 0.5132 0.156 Uiso 0.5 1 calc R U P D 1 C143 C 0.4863(16) 0.2316(17) 0.5377(10) 0.085(14) Uiso 0.5 1 d G . P D 1 H143 H 0.4364 0.2380 0.5660 0.102 Uiso 0.5 1 calc R U P D 1 C144 C 0.5375(19) 0.1612(13) 0.5275(11) 0.091(13) Uiso 0.5 1 d G . P D 1 H144 H 0.5226 0.1194 0.5490 0.109 Uiso 0.5 1 calc R U P D 1 C145 C 0.6105(18) 0.1520(12) 0.4861(13) 0.16(2) Uiso 0.5 1 d G . P D 1 H145 H 0.6456 0.1038 0.4792 0.189 Uiso 0.5 1 calc R U P D 1 C146 C 0.6324(16) 0.2131(17) 0.4548(10) 0.086(13) Uiso 0.5 1 d G . P D 1 H146 H 0.6823 0.2068 0.4265 0.104 Uiso 0.5 1 calc R U P D 1 C241 C 0.5695(14) 0.2702(10) 0.4491(9) 0.029(8) Uiso 0.5 1 d DG U P D 2 C242 C 0.5033(15) 0.2747(12) 0.4948(10) 0.066(13) Uiso 0.5 1 d G . P D 2 H242 H 0.4756 0.3215 0.5096 0.079 Uiso 0.5 1 calc R U P D 2 C243 C 0.4776(16) 0.2108(17) 0.5188(10) 0.116(19) Uiso 0.5 1 d G . P D 2 H243 H 0.4324 0.2138 0.5501 0.139 Uiso 0.5 1 calc R U P D 2 C244 C 0.518(2) 0.1423(13) 0.4972(13) 0.116(17) Uiso 0.5 1 d G . P D 2 H244 H 0.5006 0.0986 0.5136 0.139 Uiso 0.5 1 calc R U P D 2 C245 C 0.584(2) 0.1378(10) 0.4515(13) 0.14(2) Uiso 0.5 1 d G . P D 2 H245 H 0.6121 0.0910 0.4366 0.166 Uiso 0.5 1 calc R U P D 2 C246 C 0.6101(16) 0.2018(14) 0.4274(9) 0.084(13) Uiso 0.5 1 d G . P D 2 H246 H 0.6553 0.1987 0.3962 0.101 Uiso 0.5 1 calc R U P D 2 C151 C 1.031(2) -0.1207(15) 0.2239(14) 0.243(19) Uiso 1 1 d G . . . . C152 C 0.967(2) -0.1239(14) 0.2001(9) 0.203(15) Uiso 1 1 d G . . . . H152 H 0.9541 -0.0879 0.1729 0.244 Uiso 1 1 calc R U . . . C153 C 0.9223(15) -0.1797(19) 0.2160(12) 0.27(2) Uiso 1 1 d G . . . . H153 H 0.8787 -0.1819 0.1997 0.322 Uiso 1 1 calc R U . . . C154 C 0.9413(19) -0.2323(13) 0.2557(12) 0.200(15) Uiso 1 1 d G . . . . H154 H 0.9107 -0.2704 0.2666 0.240 Uiso 1 1 calc R U . . . C155 C 1.005(2) -0.2291(16) 0.2796(10) 0.27(2) Uiso 1 1 d G . . . . H155 H 1.0180 -0.2651 0.3068 0.325 Uiso 1 1 calc R U . . . C156 C 1.0498(17) -0.173(2) 0.2637(14) 0.28(2) Uiso 1 1 d G . . . . H156 H 1.0934 -0.1711 0.2800 0.342 Uiso 1 1 calc R U . . . C157 C 1.093(3) -0.067(3) 0.200(2) 0.33(3) Uiso 1 1 d . . . . . H157 H 1.1325 -0.0706 0.2221 0.493 Uiso 1 1 calc R U . . . H158 H 1.0602 -0.0156 0.1984 0.493 Uiso 1 1 calc R U . . . H160 H 1.1249 -0.0810 0.1635 0.493 Uiso 1 1 calc R U . . . O99 O 0.606(2) 0.1496(19) 0.3428(15) 0.142(13) Uiso 0.5 1 d . . P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.0429(5) 0.0481(5) 0.0431(6) 0.0011(4) -0.0121(4) -0.0160(4) Dy2 0.0376(5) 0.0443(5) 0.0473(7) -0.0027(5) -0.0102(5) -0.0130(4) Dy3 0.0382(5) 0.0475(5) 0.0465(6) -0.0045(5) -0.0094(5) -0.0135(4) Dy4 0.0372(5) 0.0483(5) 0.0430(6) -0.0059(5) -0.0101(5) -0.0107(4) Dy5 0.0387(5) 0.0450(5) 0.0456(6) -0.0051(5) -0.0114(5) -0.0098(4) O21 0.031(6) 0.073(8) 0.027(7) -0.003(6) 0.005(5) -0.026(6) O22 0.033(6) 0.031(6) 0.058(8) -0.002(5) -0.022(6) -0.017(5) O23 0.031(6) 0.035(6) 0.077(9) -0.011(6) -0.025(6) -0.003(5) O24 0.016(6) 0.059(7) 0.052(8) -0.022(6) 0.001(5) -0.008(5) O25 0.031(5) 0.054(6) 0.035(7) -0.001(5) -0.013(5) -0.021(5) O1 0.040(7) 0.061(7) 0.092(10) 0.016(7) -0.029(7) -0.020(5) O2 0.047(8) 0.046(7) 0.069(9) 0.022(6) -0.033(7) -0.011(6) O3 0.055(8) 0.063(8) 0.040(8) 0.014(6) -0.009(6) -0.024(7) O4 0.050(8) 0.091(9) 0.045(8) 0.006(7) 0.007(7) -0.046(7) O5 0.046(7) 0.072(8) 0.054(8) -0.009(6) -0.035(7) -0.015(6) O6 0.064(8) 0.048(7) 0.035(7) -0.009(6) 0.001(6) -0.020(6) O7 0.022(6) 0.044(6) 0.049(8) 0.006(6) -0.002(6) -0.013(5) O8 0.052(8) 0.079(9) 0.059(9) -0.018(8) 0.016(7) -0.014(7) O9 0.047(7) 0.076(8) 0.043(8) -0.010(7) 0.018(6) -0.041(6) O10 0.033(6) 0.054(7) 0.053(7) -0.014(6) -0.011(5) -0.023(5) O11 0.035(7) 0.032(6) 0.066(9) 0.011(6) -0.014(6) -0.010(5) O12 0.038(8) 0.068(8) 0.082(10) 0.007(7) -0.011(7) -0.014(7) O13 0.059(8) 0.078(8) 0.033(8) -0.013(7) -0.007(6) -0.013(7) O14 0.057(8) 0.061(7) 0.044(8) 0.004(6) -0.024(6) -0.014(6) O15 0.022(6) 0.048(6) 0.068(9) 0.002(6) -0.024(6) -0.013(5) O16 0.099(11) 0.069(9) 0.118(13) -0.028(9) -0.060(10) -0.014(8) O17 0.043(7) 0.056(6) 0.094(10) -0.024(7) -0.020(7) 0.002(5) O18 0.040(7) 0.052(7) 0.062(9) -0.011(6) -0.023(6) -0.008(6) O19 0.043(7) 0.043(6) 0.025(7) 0.004(6) 0.002(6) 0.000(5) O20 0.044(8) 0.119(10) 0.047(8) -0.022(7) -0.019(7) 0.011(7) N1 0.058(10) 0.083(10) 0.057(11) -0.019(9) 0.002(8) -0.031(8) N2 0.042(9) 0.048(8) 0.062(10) -0.015(8) -0.014(8) -0.004(7) N3 0.039(8) 0.082(10) 0.033(9) -0.001(8) -0.014(7) -0.019(7) N4 0.053(9) 0.054(8) 0.040(9) -0.002(7) -0.018(7) -0.003(7) C1 0.087(15) 0.058(12) 0.078(16) -0.018(11) -0.046(13) -0.018(11) C2 0.050(13) 0.084(15) 0.085(17) 0.016(13) -0.018(12) 0.008(11) C3 0.101(17) 0.079(15) 0.049(14) 0.015(12) -0.053(13) -0.011(13) C4 0.15(2) 0.076(15) 0.060(16) -0.014(13) -0.033(16) -0.020(16) C5 0.119(19) 0.050(13) 0.080(17) -0.006(12) -0.045(15) 0.010(12) C6 0.063(12) 0.072(13) 0.049(13) 0.013(10) -0.020(9) -0.022(10) C7 0.061(12) 0.058(10) 0.043(12) 0.029(8) -0.012(9) -0.031(8) C8 0.050(12) 0.071(11) 0.091(17) -0.005(10) -0.019(12) -0.016(9) C9 0.058(13) 0.118(17) 0.027(12) 0.007(11) -0.004(10) -0.047(13) C10 0.112(14) 0.023(10) 0.093(17) -0.006(10) -0.023(14) -0.007(9) C11 0.105(13) 0.067(11) 0.063(15) -0.004(11) -0.049(12) 0.002(10) C12 0.19(2) 0.064(12) 0.10(2) -0.004(13) -0.07(2) -0.043(13) C13 0.21(2) 0.041(12) 0.10(2) -0.036(13) -0.08(2) 0.054(13) C14 0.124(17) 0.17(3) 0.13(3) -0.08(2) -0.061(19) 0.055(15) C15 0.100(13) 0.099(16) 0.11(2) -0.021(14) -0.022(16) -0.020(12) C16 0.11(2) 0.053(14) 0.09(2) -0.007(14) 0.013(17) -0.034(14) C17 0.12(2) 0.065(16) 0.15(3) 0.013(18) -0.03(2) -0.060(17) C18 0.23(4) 0.087(18) 0.050(18) -0.011(14) -0.04(2) -0.06(2) C19 0.10(2) 0.099(19) 0.052(18) 0.035(16) 0.018(16) -0.022(16) C20 0.071(16) 0.069(13) 0.056(16) 0.012(12) -0.004(13) -0.006(12) C21 0.101(19) 0.059(12) 0.037(13) -0.016(10) -0.022(13) -0.037(13) C22 0.082(17) 0.064(13) 0.11(2) -0.026(13) -0.064(16) -0.016(13) C23 0.066(14) 0.088(14) 0.053(14) -0.026(12) -0.004(11) 0.015(12) C24 0.105(19) 0.043(12) 0.10(2) 0.009(13) -0.071(17) -0.019(13) C25 0.078(15) 0.052(12) 0.029(12) -0.014(10) 0.003(11) -0.006(11) C26 0.11(2) 0.15(2) 0.029(13) -0.015(14) 0.018(13) -0.022(18) C27 0.10(2) 0.13(2) 0.11(2) -0.055(19) -0.021(18) 0.009(17) C28 0.069(16) 0.12(2) 0.12(2) 0.018(18) -0.040(16) -0.077(16) C29 0.19(3) 0.082(16) 0.09(2) -0.013(14) -0.02(2) -0.070(19) C30 0.067(16) 0.13(2) 0.13(2) 0.002(19) -0.001(16) -0.073(15) C31 0.061(13) 0.106(16) 0.049(14) -0.034(13) 0.004(11) -0.028(12) C32 0.081(16) 0.16(2) 0.086(18) -0.076(17) -0.027(14) -0.032(16) C33 0.055(16) 0.12(2) 0.22(4) -0.10(2) -0.042(19) -0.010(15) C34 0.054(15) 0.14(2) 0.12(2) -0.079(19) 0.016(15) -0.030(14) C35 0.061(13) 0.047(11) 0.082(16) -0.005(11) -0.022(12) -0.008(10) C36 0.037(11) 0.079(13) 0.087(17) -0.046(13) -0.014(11) -0.020(10) C37 0.045(13) 0.021(9) 0.112(19) 0.000(11) -0.014(13) 0.007(9) C38 0.049(12) 0.076(13) 0.054(13) -0.032(11) 0.001(10) -0.023(10) C39 0.035(11) 0.027(9) 0.069(15) 0.011(9) -0.013(10) -0.016(8) C40 0.029(11) 0.075(14) 0.075(16) 0.043(13) -0.021(11) -0.021(10) C41 0.056(14) 0.128(18) 0.058(15) -0.027(14) 0.008(12) -0.020(14) C42 0.093(17) 0.097(16) 0.081(18) -0.007(14) -0.016(14) -0.071(14) C43 0.039(12) 0.125(18) 0.072(16) 0.016(15) -0.005(11) -0.039(13) C44 0.036(11) 0.108(16) 0.031(12) 0.003(11) 0.011(10) 0.005(12) C45 0.034(12) 0.072(13) 0.12(2) -0.003(14) -0.020(14) -0.027(10) C46 0.066(15) 0.048(11) 0.062(14) -0.018(10) -0.002(11) 0.000(10) C47 0.049(15) 0.077(14) 0.10(2) -0.013(14) -0.035(14) 0.014(11) C48 0.069(15) 0.062(13) 0.074(18) -0.035(13) -0.008(15) 0.007(11) C49 0.044(12) 0.072(13) 0.055(14) -0.003(11) 0.012(11) -0.022(10) C50 0.050(13) 0.062(12) 0.080(17) -0.027(12) -0.007(11) -0.001(10) C51 0.052(8) 0.050(10) 0.037(11) -0.016(9) -0.012(8) -0.017(9) C52 0.042(8) 0.027(8) 0.060(10) -0.005(8) -0.022(7) -0.023(7) C53 0.058(11) 0.066(11) 0.045(11) -0.028(10) -0.010(9) -0.021(10) C54 0.040(11) 0.041(10) 0.056(13) 0.009(9) -0.020(10) -0.028(8) C55 0.038(7) 0.028(8) 0.064(9) -0.017(9) 0.002(8) 0.000(8) C56 0.052(9) 0.057(10) 0.064(10) -0.019(10) -0.011(7) -0.025(9) C57 0.073(10) 0.068(11) 0.069(11) 0.008(10) -0.019(8) -0.052(11) C58 0.067(9) 0.083(12) 0.054(9) -0.010(11) -0.031(8) -0.043(11) C59 0.058(10) 0.072(11) 0.054(10) -0.023(11) -0.026(7) 0.008(10) C60 0.051(8) 0.077(11) 0.033(9) 0.010(9) -0.006(7) -0.034(10) C61 0.063(13) 0.049(8) 0.086(15) -0.026(10) -0.032(11) -0.025(8) C62 0.082(14) 0.032(10) 0.071(15) -0.016(10) -0.005(12) -0.030(10) C63 0.062(14) 0.091(16) 0.073(16) -0.012(12) -0.032(12) -0.031(12) C64 0.067(14) 0.090(15) 0.062(15) -0.006(13) -0.025(12) -0.003(13) C65 0.047(11) 0.064(11) 0.058(13) -0.023(9) -0.018(8) -0.017(9) C66 0.018(9) 0.075(9) 0.043(11) -0.037(9) -0.003(7) 0.007(8) C67 0.061(12) 0.042(8) 0.057(13) -0.005(8) -0.029(10) -0.018(7) C68 0.054(11) 0.047(8) 0.041(11) 0.004(7) -0.019(9) -0.012(7) C69 0.062(12) 0.047(8) 0.028(11) 0.003(7) 0.007(8) -0.022(7) C70 0.022(8) 0.050(8) 0.056(10) -0.004(7) -0.013(7) -0.026(6) C71 0.056(12) 0.051(10) 0.079(13) -0.012(9) -0.041(11) -0.004(9) C72 0.096(16) 0.071(13) 0.075(16) -0.009(11) -0.068(14) 0.011(12) C73 0.066(13) 0.039(10) 0.088(16) -0.016(11) -0.017(12) -0.030(9) C74 0.059(13) 0.052(12) 0.084(17) 0.023(12) -0.035(11) -0.007(10) C75 0.074(13) 0.071(12) 0.054(12) 0.013(10) -0.032(10) -0.036(10) C76 0.044(8) 0.075(10) 0.039(11) -0.034(9) -0.008(8) -0.019(7) C77 0.034(8) 0.130(15) 0.098(18) -0.042(15) -0.011(11) -0.023(10) C78 0.064(13) 0.129(16) 0.13(3) -0.08(2) 0.005(14) 0.008(10) C79 0.072(12) 0.090(14) 0.16(3) -0.038(15) -0.054(16) 0.023(9) C80 0.062(10) 0.064(9) 0.14(2) -0.025(12) -0.055(12) -0.004(9) C81 0.034(9) 0.079(10) 0.039(11) -0.002(9) -0.014(8) -0.003(7) C82 0.028(10) 0.072(13) 0.054(13) 0.011(11) -0.012(9) 0.000(10) C83 0.045(7) 0.037(9) 0.051(12) -0.004(8) -0.001(9) -0.009(7) C84 0.037(8) 0.061(8) 0.053(12) 0.007(9) -0.031(9) -0.017(7) C85 0.060(11) 0.066(10) 0.064(14) -0.009(10) -0.026(10) -0.026(9) C86 0.101(18) 0.042(13) 0.14(2) 0.016(13) -0.023(16) -0.014(13) C87 0.080(19) 0.094(17) 0.19(3) -0.026(18) -0.012(18) -0.066(16) C88 0.092(19) 0.072(16) 0.13(2) 0.018(14) 0.011(15) -0.050(14) C89 0.082(16) 0.092(17) 0.16(3) -0.001(16) -0.040(16) -0.061(15) C90 0.057(14) 0.071(13) 0.16(2) -0.063(14) -0.029(14) -0.011(12) C91 0.075(15) 0.092(16) 0.032(12) -0.009(11) -0.016(10) -0.063(13) C92 0.074(13) 0.027(9) 0.066(14) 0.002(9) -0.010(11) -0.002(9) C105 0.066(15) 0.054(13) 0.069(16) -0.006(11) -0.007(12) 0.000(12) C106 0.055(12) 0.039(10) 0.058(13) -0.016(9) -0.003(9) -0.019(9) C107 0.022(9) 0.054(12) 0.077(15) -0.008(11) -0.023(10) 0.003(8) C108 0.026(10) 0.061(12) 0.074(15) -0.029(12) 0.013(10) -0.002(9) C109 0.101(18) 0.13(2) 0.083(18) -0.043(17) -0.024(14) -0.067(16) C110 0.13(2) 0.063(16) 0.13(3) -0.047(17) -0.002(18) -0.047(15) C111 0.23(4) 0.11(2) 0.14(3) -0.04(2) -0.13(3) -0.01(2) C112 0.19(3) 0.064(14) 0.13(2) -0.005(15) -0.13(2) -0.043(15) C119 0.052(13) 0.056(12) 0.084(18) 0.009(13) -0.043(14) -0.013(11) C120 0.048(10) 0.044(9) 0.027(10) 0.007(8) 0.006(8) -0.013(8) C133 0.037(12) 0.072(13) 0.030(12) -0.018(10) 0.011(10) 0.009(9) C134 0.077(13) 0.059(11) 0.040(12) -0.012(9) -0.038(10) -0.012(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 O4 2.265(11) . ? Dy1 O3 2.294(12) . ? Dy1 O2 2.295(10) . ? Dy1 O1 2.318(11) . ? Dy1 O22 2.378(4) . ? Dy1 O21 2.417(4) . ? Dy1 O23 2.429(4) . ? Dy1 O24 2.478(4) . ? Dy2 O6 2.227(11) . ? Dy2 O5 2.283(10) . ? Dy2 O23 2.301(5) . ? Dy2 O22 2.347(4) . ? Dy2 O7 2.383(11) . ? Dy2 O11 2.461(9) . ? Dy2 N1 2.503(6) . ? Dy2 O25 2.545(4) . ? Dy3 O9 2.287(12) . ? Dy3 O24 2.299(4) . ? Dy3 O23 2.333(4) . ? Dy3 O10 2.338(10) . ? Dy3 O11 2.349(10) . ? Dy3 O15 2.409(10) . ? Dy3 N2 2.540(6) . ? Dy3 O25 2.587(4) . ? Dy4 O14 2.281(11) . ? Dy4 O24 2.287(4) . ? Dy4 O21 2.329(4) . ? Dy4 O13 2.339(12) . ? Dy4 O15 2.350(10) . ? Dy4 O19 2.440(10) . ? Dy4 N3 2.529(6) . ? Dy4 O25 2.605(4) . ? Dy5 O17 2.262(11) . ? Dy5 O18 2.299(10) . ? Dy5 O21 2.300(4) . ? Dy5 O22 2.319(4) . ? Dy5 O19 2.366(10) . ? Dy5 O7 2.418(10) . ? Dy5 N4 2.492(6) . ? Dy5 O25 2.615(4) . ? O21 H21 1.0000 . ? O22 H22 1.0000 . ? O23 H23 1.0000 . ? O24 H24 1.0000 . ? O25 H25 1.0001 . ? O1 C7 1.273(18) . ? O2 C9 1.256(19) . ? O3 C22 1.28(2) . ? O4 C24 1.22(3) . ? O5 C69 1.256(18) . ? O6 C67 1.311(17) . ? O7 C119 1.31(2) . ? O8 C119 1.25(2) . ? O9 C54 1.237(18) . ? O10 C52 1.261(17) . ? O11 C105 1.31(2) . ? O12 C105 1.25(2) . ? O13 C39 1.293(17) . ? O14 C37 1.32(2) . ? O15 C91 1.31(2) . ? O16 C91 1.23(2) . ? O17 C84 1.239(16) . ? O18 C82 1.316(19) . ? O19 C133 1.223(18) . ? O20 C133 1.266(19) . ? N1 C120 1.498(16) . ? N1 H11 0.9900 . ? N1 H12 0.9900 . ? N2 C106 1.513(17) . ? N2 H221 0.9900 . ? N2 H231 0.9900 . ? N3 C92 1.502(15) . ? N3 H31 0.9900 . ? N3 H32 0.9900 . ? N4 C134 1.496(16) . ? N4 H41 0.9900 . ? N4 H42 0.9900 . ? C1 C6 1.331(18) . ? C1 C2 1.39(2) . ? C1 H1 0.9500 . ? C2 C3 1.39(2) . ? C2 H2 0.9500 . ? C3 C4 1.31(2) . ? C3 H3 0.9500 . ? C4 C5 1.37(3) . ? C4 H4 0.9500 . ? C5 C6 1.34(2) . ? C5 H5 0.9500 . ? C6 C7 1.46(2) . ? C7 C8 1.44(2) . ? C8 C9 1.44(2) . ? C8 H8 0.9500 . ? C9 C10 1.53(3) . ? C10 C15 1.29(3) . ? C10 C11 1.35(3) . ? C11 C12 1.35(3) . ? C11 H11A 0.9500 . ? C12 C13 1.43(3) . ? C12 H12A 0.9500 . ? C13 C14 1.36(4) . ? C13 H13 0.9500 . ? C14 C15 1.33(3) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C21 1.28(3) . ? C16 C17 1.32(3) . ? C16 H16 0.9500 . ? C17 C18 1.37(3) . ? C17 H17 0.9500 . ? C18 C19 1.31(3) . ? C18 H18 0.9500 . ? C19 C20 1.38(3) . ? C19 H19 0.9500 . ? C20 C21 1.36(2) . ? C20 H20 0.9500 . ? C21 C22 1.49(3) . ? C22 C23 1.41(3) . ? C23 C24 1.47(3) . ? C23 H23A 0.9500 . ? C24 C25 1.58(3) . ? C25 C30 1.28(3) . ? C25 C26 1.38(3) . ? C26 C27 1.39(3) . ? C26 H26 0.9500 . ? C27 C28 1.31(3) . ? C27 H27 0.9500 . ? C28 C29 1.36(3) . ? C28 H28 0.9500 . ? C29 C30 1.51(3) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C36 1.36(2) . ? C31 C32 1.44(2) . ? C31 H31A 0.9500 . ? C32 C33 1.40(3) . ? C32 H32A 0.9500 . ? C33 C34 1.35(3) . ? C33 H33 0.9500 . ? C34 C35 1.38(3) . ? C34 H34 0.9500 . ? C35 C36 1.42(2) . ? C35 H35 0.9500 . ? C36 C37 1.48(2) . ? C37 C38 1.41(2) . ? C38 C39 1.37(2) . ? C38 H38 0.9500 . ? C39 C40 1.50(2) . ? C40 C45 1.38(2) . ? C40 C41 1.39(3) . ? C41 C42 1.44(3) . ? C41 H41A 0.9500 . ? C42 C43 1.32(2) . ? C42 H42A 0.9500 . ? C43 C44 1.36(3) . ? C43 H43 0.9500 . ? C44 C45 1.38(2) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46 C47 1.38(2) . ? C46 C51 1.38(2) . ? C46 H46 0.9500 . ? C47 C48 1.34(3) . ? C47 H47 0.9500 . ? C48 C49 1.32(2) . ? C48 H48 0.9500 . ? C49 C50 1.44(2) . ? C49 H49 0.9500 . ? C50 C51 1.37(2) . ? C50 H50 0.9500 . ? C51 C52 1.54(2) . ? C52 C53 1.35(2) . ? C53 C54 1.38(2) . ? C53 H53 0.9500 . ? C54 C55 1.53(2) . ? C55 C60 1.39(2) . ? C55 C56 1.41(2) . ? C56 C57 1.38(2) . ? C56 H56 0.9500 . ? C57 C58 1.34(2) . ? C57 H57 0.9500 . ? C58 C59 1.30(2) . ? C58 H58 0.9500 . ? C59 C60 1.41(2) . ? C59 H59 0.9500 . ? C60 H60 0.9500 . ? C61 C66 1.37(2) . ? C61 C62 1.42(2) . ? C61 H61 0.9500 . ? C62 C63 1.36(2) . ? C62 H62 0.9500 . ? C63 C64 1.36(2) . ? C63 H63 0.9500 . ? C64 C65 1.39(2) . ? C64 H64 0.9500 . ? C65 C66 1.43(2) . ? C65 H65 0.9500 . ? C66 C67 1.48(2) . ? C67 C68 1.39(2) . ? C68 C69 1.45(2) . ? C68 H68 0.9500 . ? C69 C70 1.48(2) . ? C70 C71 1.40(2) . ? C70 C75 1.42(2) . ? C71 C72 1.34(2) . ? C71 H71 0.9500 . ? C72 C73 1.35(2) . ? C72 H72 0.9500 . ? C73 C74 1.40(2) . ? C73 H73 0.9500 . ? C74 C75 1.38(2) . ? C74 H74 0.9500 . ? C75 H75 0.9500 . ? C76 C81 1.37(2) . ? C76 C77 1.46(2) . ? C76 H76 0.9500 . ? C77 C78 1.28(3) . ? C77 H77 0.9500 . ? C78 C79 1.30(3) . ? C78 H78 0.9500 . ? C79 C80 1.45(3) . ? C79 H79 0.9500 . ? C80 C81 1.39(2) . ? C80 H80 0.9500 . ? C81 C82 1.53(2) . ? C82 C83 1.37(2) . ? C83 C84 1.46(2) . ? C83 H83 0.9500 . ? C84 C85 1.47(2) . ? C85 C86 1.36(2) . ? C85 C90 1.41(2) . ? C86 C87 1.32(3) . ? C86 H86 0.9500 . ? C87 C88 1.39(3) . ? C87 H87 0.9500 . ? C88 C89 1.42(3) . ? C88 H88 0.9500 . ? C89 C90 1.33(2) . ? C89 H89 0.9500 . ? C90 H90 0.9500 . ? C91 C92 1.55(2) . ? C92 C99 1.50(2) . ? C92 C93B 1.58(2) . ? C92 C93A 1.59(2) . ? C92 C199 1.62(4) . ? C93A C94A 1.3900 . ? C93A C98A 1.3900 . ? C94A C95A 1.3900 . ? C94A H94A 0.9500 . ? C95A C96A 1.3900 . ? C95A H95A 0.9500 . ? C96A C97A 1.3900 . ? C96A H96A 0.9500 . ? C97A C98A 1.3900 . ? C97A H97A 0.9500 . ? C98A H98A 0.9500 . ? C93B C94B 1.3900 . ? C93B C98B 1.3900 . ? C94B C95B 1.3900 . ? C94B H94B 0.9500 . ? C95B C96B 1.3900 . ? C95B H95B 0.9500 . ? C96B C97B 1.3900 . ? C96B H96B 0.9500 . ? C97B C98B 1.3900 . ? C97B H97B 0.9500 . ? C98B H98B 0.9500 . ? C99 C100 1.3900 . ? C99 C104 1.3900 . ? C100 C101 1.3900 . ? C100 H100 0.9500 . ? C101 C102 1.3900 . ? C101 H101 0.9500 . ? C102 C103 1.3900 . ? C102 H102 0.9500 . ? C103 C104 1.3900 . ? C103 H103 0.9500 . ? C104 H104 0.9500 . ? C199 C200 1.3900 . ? C199 C204 1.3900 . ? C200 C201 1.3900 . ? C200 H200 0.9500 . ? C201 C202 1.3900 . ? C201 H201 0.9500 . ? C202 C203 1.3900 . ? C202 H202 0.9500 . ? C203 C204 1.3900 . ? C203 H203 0.9500 . ? C204 H204 0.9500 . ? C105 C106 1.49(2) . ? C106 C107 1.55(2) . ? C106 C213 1.55(2) . ? C106 C113 1.56(2) . ? C107 C112 1.37(2) . ? C107 C108 1.38(2) . ? C108 C109 1.37(2) . ? C108 H108 0.9500 . ? C109 C110 1.37(3) . ? C109 H109 0.9500 . ? C110 C111 1.29(3) . ? C110 H110 0.9500 . ? C111 C112 1.40(3) . ? C111 H111 0.9500 . ? C112 H112 0.9500 . ? C113 C114 1.3900 . ? C113 C118 1.3900 . ? C114 C115 1.3900 . ? C114 H114 0.9500 . ? C115 C116 1.3900 . ? C115 H115 0.9500 . ? C116 C117 1.3900 . ? C116 H116 0.9500 . ? C117 C118 1.3900 . ? C117 H117 0.9500 . ? C118 H118 0.9500 . ? C213 C214 1.3900 . ? C213 C218 1.3900 . ? C214 C215 1.3900 . ? C214 H214 0.9500 . ? C215 C216 1.3900 . ? C215 H215 0.9500 . ? C216 C217 1.3900 . ? C216 H216 0.9500 . ? C217 C218 1.3900 . ? C217 H217 0.9500 . ? C218 H218 0.9500 . ? C119 C120 1.53(2) . ? C120 C121 1.52(2) . ? C120 C221 1.54(3) . ? C120 C227 1.54(2) . ? C120 C127 1.54(2) . ? C121 C122 1.3900 . ? C121 C126 1.3900 . ? C122 C123 1.3900 . ? C122 H122 0.9500 . ? C123 C124 1.3900 . ? C123 H123 0.9500 . ? C124 C125 1.3900 . ? C124 H124 0.9500 . ? C125 C126 1.3900 . ? C125 H125 0.9500 . ? C126 H126 0.9500 . ? C221 C222 1.3900 . ? C221 C226 1.3900 . ? C222 C223 1.3900 . ? C222 H222 0.9500 . ? C223 C224 1.3900 . ? C223 H223 0.9500 . ? C224 C225 1.3900 . ? C224 H224 0.9500 . ? C225 C226 1.3900 . ? C225 H225 0.9500 . ? C226 H226 0.9500 . ? C127 C128 1.3900 . ? C127 C132 1.3900 . ? C128 C129 1.3900 . ? C128 H128 0.9500 . ? C129 C130 1.3900 . ? C129 H129 0.9500 . ? C130 C131 1.3900 . ? C130 H130 0.9500 . ? C131 C132 1.3900 . ? C131 H131 0.9500 . ? C132 H132 0.9500 . ? C227 C228 1.3900 . ? C227 C232 1.3900 . ? C228 C229 1.3900 . ? C228 H228 0.9500 . ? C229 C230 1.3900 . ? C229 H229 0.9500 . ? C230 C231 1.3900 . ? C230 H230 0.9500 . ? C231 C232 1.3900 . ? C231 H23B 0.9500 . ? C232 H232 0.9500 . ? C133 C134 1.60(2) . ? C134 C235 1.46(3) . ? C134 C141 1.55(2) . ? C134 C241 1.60(2) . ? C134 C135 1.70(3) . ? C135 C136 1.3900 . ? C135 C140 1.3900 . ? C136 C137 1.3900 . ? C136 H136 0.9500 . ? C137 C138 1.3900 . ? C137 H137 0.9500 . ? C138 C139 1.3900 . ? C138 H138 0.9500 . ? C139 C140 1.3900 . ? C139 H139 0.9500 . ? C140 H140 0.9500 . ? C235 C236 1.3900 . ? C235 C240 1.3900 . ? C236 C237 1.3900 . ? C236 H236 0.9500 . ? C237 C238 1.3900 . ? C237 H237 0.9500 . ? C238 C239 1.3900 . ? C238 H238 0.9500 . ? C239 C240 1.3900 . ? C239 H239 0.9500 . ? C240 H240 0.9500 . ? C141 C142 1.3900 . ? C141 C146 1.3900 . ? C142 C143 1.3900 . ? C142 H142 0.9500 . ? C143 C144 1.3900 . ? C143 H143 0.9500 . ? C144 C145 1.3900 . ? C144 H144 0.9500 . ? C145 C146 1.3900 . ? C145 H145 0.9500 . ? C146 H146 0.9500 . ? C241 C242 1.3900 . ? C241 C246 1.3900 . ? C242 C243 1.3900 . ? C242 H242 0.9500 . ? C243 C244 1.3900 . ? C243 H243 0.9500 . ? C244 C245 1.3900 . ? C244 H244 0.9500 . ? C245 C246 1.3900 . ? C245 H245 0.9500 . ? C246 H246 0.9500 . ? C151 C152 1.3900 . ? C151 C156 1.3900 . ? C151 C157 1.58(5) . ? C152 C153 1.3900 . ? C152 H152 0.9500 . ? C153 C154 1.3900 . ? C153 H153 0.9500 . ? C154 C155 1.3900 . ? C154 H154 0.9500 . ? C155 C156 1.3900 . ? C155 H155 0.9500 . ? C156 H156 0.9500 . ? C157 H157 0.9800 . ? C157 H158 0.9800 . ? C157 H160 0.9800 . ? 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 Dy1 O3 73.7(4) . . ? O4 Dy1 O2 75.6(4) . . ? O3 Dy1 O2 114.0(4) . . ? O4 Dy1 O1 120.6(4) . . ? O3 Dy1 O1 73.4(4) . . ? O2 Dy1 O1 74.7(4) . . ? O4 Dy1 O22 134.7(3) . . ? O3 Dy1 O22 151.0(3) . . ? O2 Dy1 O22 75.9(3) . . ? O1 Dy1 O22 84.0(3) . . ? O4 Dy1 O21 74.3(3) . . ? O3 Dy1 O21 135.2(3) . . ? O2 Dy1 O21 87.0(3) . . ? O1 Dy1 O21 151.2(3) . . ? O22 Dy1 O21 69.81(13) . . ? O4 Dy1 O23 148.2(3) . . ? O3 Dy1 O23 84.0(3) . . ? O2 Dy1 O23 135.4(3) . . ? O1 Dy1 O23 72.2(3) . . ? O22 Dy1 O23 71.63(12) . . ? O21 Dy1 O23 108.91(17) . . ? O4 Dy1 O24 82.5(3) . . ? O3 Dy1 O24 75.7(3) . . ? O2 Dy1 O24 151.6(3) . . ? O1 Dy1 O24 132.9(3) . . ? O22 Dy1 O24 109.03(17) . . ? O21 Dy1 O24 69.71(11) . . ? O23 Dy1 O24 69.97(11) . . ? O6 Dy2 O5 75.0(4) . . ? O6 Dy2 O23 82.3(3) . . ? O5 Dy2 O23 110.8(3) . . ? O6 Dy2 O22 126.3(3) . . ? O5 Dy2 O22 69.6(3) . . ? O23 Dy2 O22 74.49(13) . . ? O6 Dy2 O7 143.3(4) . . ? O5 Dy2 O7 88.7(4) . . ? O23 Dy2 O7 134.4(3) . . ? O22 Dy2 O7 74.9(3) . . ? O6 Dy2 O11 83.0(4) . . ? O5 Dy2 O11 156.3(3) . . ? O23 Dy2 O11 74.1(3) . . ? O22 Dy2 O11 132.6(3) . . ? O7 Dy2 O11 104.3(3) . . ? O6 Dy2 N1 85.2(3) . . ? O5 Dy2 N1 93.7(3) . . ? O23 Dy2 N1 148.38(17) . . ? O22 Dy2 N1 134.88(18) . . ? O7 Dy2 N1 62.8(3) . . ? O11 Dy2 N1 75.6(3) . . ? O6 Dy2 O25 143.0(3) . . ? O5 Dy2 O25 136.4(3) . . ? O23 Dy2 O25 68.93(11) . . ? O22 Dy2 O25 68.63(11) . . ? O7 Dy2 O25 68.9(2) . . ? O11 Dy2 O25 67.3(3) . . ? N1 Dy2 O25 107.04(17) . . ? O9 Dy3 O24 115.1(3) . . ? O9 Dy3 O23 73.2(3) . . ? O24 Dy3 O23 74.81(12) . . ? O9 Dy3 O10 73.7(4) . . ? O24 Dy3 O10 82.3(3) . . ? O23 Dy3 O10 126.1(3) . . ? O9 Dy3 O11 88.5(4) . . ? O24 Dy3 O11 134.1(3) . . ? O23 Dy3 O11 75.7(2) . . ? O10 Dy3 O11 143.5(3) . . ? O9 Dy3 O15 154.2(4) . . ? O24 Dy3 O15 73.9(3) . . ? O23 Dy3 O15 132.0(3) . . ? O10 Dy3 O15 84.2(4) . . ? O11 Dy3 O15 102.1(4) . . ? O9 Dy3 N2 78.9(3) . . ? O24 Dy3 N2 152.61(17) . . ? O23 Dy3 N2 132.58(17) . . ? O10 Dy3 N2 79.3(3) . . ? O11 Dy3 N2 65.9(3) . . ? O15 Dy3 N2 84.1(3) . . ? O9 Dy3 O25 138.2(3) . . ? O24 Dy3 O25 68.36(11) . . ? O23 Dy3 O25 67.72(11) . . ? O10 Dy3 O25 143.4(3) . . ? O11 Dy3 O25 68.2(3) . . ? O15 Dy3 O25 67.3(3) . . ? N2 Dy3 O25 118.02(17) . . ? O14 Dy4 O24 129.9(3) . . ? O14 Dy4 O21 83.9(3) . . ? O24 Dy4 O21 74.62(13) . . ? O14 Dy4 O13 73.7(4) . . ? O24 Dy4 O13 71.8(3) . . ? O21 Dy4 O13 109.2(3) . . ? O14 Dy4 O15 142.8(3) . . ? O24 Dy4 O15 75.3(3) . . ? O21 Dy4 O15 133.0(3) . . ? O13 Dy4 O15 94.5(4) . . ? O14 Dy4 O19 82.3(4) . . ? O24 Dy4 O19 131.6(3) . . ? O21 Dy4 O19 74.9(2) . . ? O13 Dy4 O19 154.9(4) . . ? O15 Dy4 O19 100.3(3) . . ? O14 Dy4 N3 77.4(3) . . ? O24 Dy4 N3 131.62(17) . . ? O21 Dy4 N3 153.75(18) . . ? O13 Dy4 N3 83.2(3) . . ? O15 Dy4 N3 66.0(3) . . ? O19 Dy4 N3 84.4(3) . . ? O14 Dy4 O25 141.5(3) . . ? O24 Dy4 O25 68.22(11) . . ? O21 Dy4 O25 67.79(11) . . ? O13 Dy4 O25 139.2(3) . . ? O15 Dy4 O25 67.9(2) . . ? O19 Dy4 O25 65.9(3) . . ? N3 Dy4 O25 118.12(17) . . ? O17 Dy5 O18 74.3(4) . . ? O17 Dy5 O21 72.4(3) . . ? O18 Dy5 O21 125.2(3) . . ? O17 Dy5 O22 113.8(3) . . ? O18 Dy5 O22 82.6(3) . . ? O21 Dy5 O22 72.90(14) . . ? O17 Dy5 O19 90.6(4) . . ? O18 Dy5 O19 145.2(4) . . ? O21 Dy5 O19 76.9(3) . . ? O22 Dy5 O19 132.0(3) . . ? O17 Dy5 O7 154.9(4) . . ? O18 Dy5 O7 84.0(3) . . ? O21 Dy5 O7 131.8(3) . . ? O22 Dy5 O7 74.7(3) . . ? O19 Dy5 O7 100.6(3) . . ? O17 Dy5 N4 81.8(4) . . ? O18 Dy5 N4 80.8(3) . . ? O21 Dy5 N4 134.10(18) . . ? O22 Dy5 N4 152.96(18) . . ? O19 Dy5 N4 65.9(3) . . ? O7 Dy5 N4 82.5(3) . . ? O17 Dy5 O25 137.7(3) . . ? O18 Dy5 O25 142.7(3) . . ? O21 Dy5 O25 68.00(11) . . ? O22 Dy5 O25 67.80(11) . . ? O19 Dy5 O25 66.7(3) . . ? O7 Dy5 O25 67.2(3) . . ? N4 Dy5 O25 116.25(17) . . ? Dy5 O21 Dy4 102.31(17) . . ? Dy5 O21 Dy1 108.06(16) . . ? Dy4 O21 Dy1 107.95(16) . . ? Dy5 O21 H21 112.6 . . ? Dy4 O21 H21 112.6 . . ? Dy1 O21 H21 112.6 . . ? Dy5 O22 Dy2 101.27(17) . . ? Dy5 O22 Dy1 108.77(16) . . ? Dy2 O22 Dy1 106.80(16) . . ? Dy5 O22 H22 113.1 . . ? Dy2 O22 H22 113.1 . . ? Dy1 O22 H22 113.1 . . ? Dy2 O23 Dy3 101.72(17) . . ? Dy2 O23 Dy1 106.60(16) . . ? Dy3 O23 Dy1 107.66(16) . . ? Dy2 O23 H23 113.3 . . ? Dy3 O23 H23 113.3 . . ? Dy1 O23 H23 113.3 . . ? Dy4 O24 Dy3 102.65(18) . . ? Dy4 O24 Dy1 107.25(16) . . ? Dy3 O24 Dy1 107.10(16) . . ? Dy4 O24 H24 113.0 . . ? Dy3 O24 H24 113.0 . . ? Dy1 O24 H24 113.0 . . ? Dy2 O25 Dy3 88.89(13) . . ? Dy2 O25 Dy4 158.64(19) . . ? Dy3 O25 Dy4 87.21(13) . . ? Dy2 O25 Dy5 88.69(13) . . ? Dy3 O25 Dy5 158.69(19) . . ? Dy4 O25 Dy5 87.38(12) . . ? Dy2 O25 H25 98.6 . . ? Dy3 O25 H25 100.6 . . ? Dy4 O25 H25 102.7 . . ? Dy5 O25 H25 100.7 . . ? C7 O1 Dy1 137.2(12) . . ? C9 O2 Dy1 134.8(12) . . ? C22 O3 Dy1 133.7(12) . . ? C24 O4 Dy1 134.1(13) . . ? C69 O5 Dy2 136.4(10) . . ? C67 O6 Dy2 136.7(10) . . ? C119 O7 Dy2 127.3(11) . . ? C119 O7 Dy5 133.3(11) . . ? Dy2 O7 Dy5 97.4(4) . . ? C54 O9 Dy3 135.2(10) . . ? C52 O10 Dy3 132.3(9) . . ? C105 O11 Dy3 121.8(11) . . ? C105 O11 Dy2 133.4(11) . . ? Dy3 O11 Dy2 96.7(3) . . ? C39 O13 Dy4 138.5(11) . . ? C37 O14 Dy4 133.2(11) . . ? C91 O15 Dy4 124.8(9) . . ? C91 O15 Dy3 132.2(10) . . ? Dy4 O15 Dy3 97.6(4) . . ? C84 O17 Dy5 139.2(10) . . ? C82 O18 Dy5 133.0(10) . . ? C133 O19 Dy5 126.9(10) . . ? C133 O19 Dy4 132.3(10) . . ? Dy5 O19 Dy4 97.2(4) . . ? C120 N1 Dy2 117.1(6) . . ? C120 N1 H11 108.0 . . ? Dy2 N1 H11 108.0 . . ? C120 N1 H12 108.0 . . ? Dy2 N1 H12 108.0 . . ? H11 N1 H12 107.3 . . ? C106 N2 Dy3 116.8(7) . . ? C106 N2 H221 108.1 . . ? Dy3 N2 H221 108.1 . . ? C106 N2 H231 108.1 . . ? Dy3 N2 H231 108.1 . . ? H221 N2 H231 107.3 . . ? C92 N3 Dy4 119.4(8) . . ? C92 N3 H31 107.5 . . ? Dy4 N3 H31 107.5 . . ? C92 N3 H32 107.5 . . ? Dy4 N3 H32 107.5 . . ? H31 N3 H32 107.0 . . ? C134 N4 Dy5 119.7(7) . . ? C134 N4 H41 107.4 . . ? Dy5 N4 H41 107.4 . . ? C134 N4 H42 107.4 . . ? Dy5 N4 H42 107.4 . . ? H41 N4 H42 106.9 . . ? C6 C1 C2 123.2(13) . . ? C6 C1 H1 118.4 . . ? C2 C1 H1 118.4 . . ? C3 C2 C1 117.9(14) . . ? C3 C2 H2 121.0 . . ? C1 C2 H2 121.0 . . ? C4 C3 C2 117.2(18) . . ? C4 C3 H3 121.4 . . ? C2 C3 H3 121.4 . . ? C3 C4 C5 123(2) . . ? C3 C4 H4 118.5 . . ? C5 C4 H4 118.5 . . ? C6 C5 C4 121.4(19) . . ? C6 C5 H5 119.3 . . ? C4 C5 H5 119.3 . . ? C1 C6 C5 116.5(17) . . ? C1 C6 C7 123.7(17) . . ? C5 C6 C7 119.4(18) . . ? O1 C7 C8 122.0(17) . . ? O1 C7 C6 115.4(17) . . ? C8 C7 C6 122.6(17) . . ? C7 C8 C9 123.9(18) . . ? C7 C8 H8 118.0 . . ? C9 C8 H8 118.0 . . ? O2 C9 C8 125.2(19) . . ? O2 C9 C10 117.6(17) . . ? C8 C9 C10 117.2(18) . . ? C15 C10 C11 114.8(19) . . ? C15 C10 C9 127(2) . . ? C11 C10 C9 118(2) . . ? C12 C11 C10 126(2) . . ? C12 C11 H11A 117.1 . . ? C10 C11 H11A 117.1 . . ? C11 C12 C13 115(2) . . ? C11 C12 H12A 122.4 . . ? C13 C12 H12A 122.4 . . ? C14 C13 C12 118(2) . . ? C14 C13 H13 120.9 . . ? C12 C13 H13 120.9 . . ? C15 C14 C13 119(3) . . ? C15 C14 H14 120.3 . . ? C13 C14 H14 120.3 . . ? C10 C15 C14 126(3) . . ? C10 C15 H15 117.0 . . ? C14 C15 H15 117.0 . . ? C21 C16 C17 125(2) . . ? C21 C16 H16 117.7 . . ? C17 C16 H16 117.7 . . ? C16 C17 C18 119(3) . . ? C16 C17 H17 120.6 . . ? C18 C17 H17 120.6 . . ? C19 C18 C17 120(3) . . ? C19 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? C18 C19 C20 118(3) . . ? C18 C19 H19 121.0 . . ? C20 C19 H19 121.0 . . ? C21 C20 C19 122(2) . . ? C21 C20 H20 119.0 . . ? C19 C20 H20 119.0 . . ? C16 C21 C20 116.1(19) . . ? C16 C21 C22 111(2) . . ? C20 C21 C22 133(2) . . ? O3 C22 C23 123.7(19) . . ? O3 C22 C21 120.5(17) . . ? C23 C22 C21 115(2) . . ? C22 C23 C24 121(2) . . ? C22 C23 H23A 119.4 . . ? C24 C23 H23A 119.4 . . ? O4 C24 C23 125.3(19) . . ? O4 C24 C25 116.3(19) . . ? C23 C24 C25 118(2) . . ? C30 C25 C26 122(2) . . ? C30 C25 C24 112(2) . . ? C26 C25 C24 125(2) . . ? C25 C26 C27 116(2) . . ? C25 C26 H26 122.2 . . ? C27 C26 H26 122.2 . . ? C28 C27 C26 127(3) . . ? C28 C27 H27 116.5 . . ? C26 C27 H27 116.5 . . ? C27 C28 C29 118(2) . . ? C27 C28 H28 121.0 . . ? C29 C28 H28 121.0 . . ? C28 C29 C30 117(2) . . ? C28 C29 H29 121.4 . . ? C30 C29 H29 121.4 . . ? C25 C30 C29 120(2) . . ? C25 C30 H30 120.0 . . ? C29 C30 H30 120.0 . . ? C36 C31 C32 122(2) . . ? C36 C31 H31A 119.1 . . ? C32 C31 H31A 119.1 . . ? C33 C32 C31 119(2) . . ? C33 C32 H32A 120.4 . . ? C31 C32 H32A 120.4 . . ? C34 C33 C32 116(2) . . ? C34 C33 H33 121.9 . . ? C32 C33 H33 121.9 . . ? C33 C34 C35 126(2) . . ? C33 C34 H34 116.9 . . ? C35 C34 H34 116.9 . . ? C34 C35 C36 118(2) . . ? C34 C35 H35 121.2 . . ? C36 C35 H35 121.2 . . ? C31 C36 C35 118.2(17) . . ? C31 C36 C37 121.6(18) . . ? C35 C36 C37 120(2) . . ? O14 C37 C38 126.6(18) . . ? O14 C37 C36 113.0(17) . . ? C38 C37 C36 120.3(18) . . ? C39 C38 C37 125.5(17) . . ? C39 C38 H38 117.3 . . ? C37 C38 H38 117.3 . . ? O13 C39 C38 120.9(17) . . ? O13 C39 C40 111.2(15) . . ? C38 C39 C40 127.7(17) . . ? C45 C40 C41 119.7(19) . . ? C45 C40 C39 125.1(17) . . ? C41 C40 C39 115(2) . . ? C40 C41 C42 119(2) . . ? C40 C41 H41A 120.4 . . ? C42 C41 H41A 120.4 . . ? C43 C42 C41 116.4(19) . . ? C43 C42 H42A 121.8 . . ? C41 C42 H42A 121.8 . . ? C42 C43 C44 127(2) . . ? C42 C43 H43 116.7 . . ? C44 C43 H43 116.7 . . ? C43 C44 C45 117(2) . . ? C43 C44 H44 121.4 . . ? C45 C44 H44 121.4 . . ? C44 C45 C40 120.7(19) . . ? C44 C45 H45 119.6 . . ? C40 C45 H45 119.6 . . ? C47 C46 C51 126(2) . . ? C47 C46 H46 117.2 . . ? C51 C46 H46 117.2 . . ? C48 C47 C46 114(2) . . ? C48 C47 H47 122.8 . . ? C46 C47 H47 122.8 . . ? C49 C48 C47 125(2) . . ? C49 C48 H48 117.3 . . ? C47 C48 H48 117.3 . . ? C48 C49 C50 119.1(19) . . ? C48 C49 H49 120.5 . . ? C50 C49 H49 120.5 . . ? C51 C50 C49 118.6(18) . . ? C51 C50 H50 120.7 . . ? C49 C50 H50 120.7 . . ? C50 C51 C46 116.7(17) . . ? C50 C51 C52 122.7(16) . . ? C46 C51 C52 120.5(17) . . ? O10 C52 C53 127.8(15) . . ? O10 C52 C51 113.2(13) . . ? C53 C52 C51 119.0(16) . . ? C52 C53 C54 123.2(16) . . ? C52 C53 H53 118.4 . . ? C54 C53 H53 118.4 . . ? O9 C54 C53 125.9(15) . . ? O9 C54 C55 114.7(14) . . ? C53 C54 C55 119.3(16) . . ? C60 C55 C56 113.5(15) . . ? C60 C55 C54 119.9(15) . . ? C56 C55 C54 126.2(15) . . ? C57 C56 C55 123.2(17) . . ? C57 C56 H56 118.4 . . ? C55 C56 H56 118.4 . . ? C58 C57 C56 118.6(19) . . ? C58 C57 H57 120.7 . . ? C56 C57 H57 120.7 . . ? C59 C58 C57 122.9(17) . . ? C59 C58 H58 118.6 . . ? C57 C58 H58 118.6 . . ? C58 C59 C60 119.1(17) . . ? C58 C59 H59 120.4 . . ? C60 C59 H59 120.4 . . ? C55 C60 C59 122.8(16) . . ? C55 C60 H60 118.6 . . ? C59 C60 H60 118.6 . . ? C66 C61 C62 118.9(17) . . ? C66 C61 H61 120.5 . . ? C62 C61 H61 120.5 . . ? C63 C62 C61 121.5(17) . . ? C63 C62 H62 119.3 . . ? C61 C62 H62 119.3 . . ? C64 C63 C62 121.0(18) . . ? C64 C63 H63 119.5 . . ? C62 C63 H63 119.5 . . ? C63 C64 C65 119.1(18) . . ? C63 C64 H64 120.5 . . ? C65 C64 H64 120.5 . . ? C64 C65 C66 120.8(16) . . ? C64 C65 H65 119.6 . . ? C66 C65 H65 119.6 . . ? C61 C66 C65 118.3(14) . . ? C61 C66 C67 117.2(14) . . ? C65 C66 C67 124.4(15) . . ? O6 C67 C68 125.2(14) . . ? O6 C67 C66 116.3(14) . . ? C68 C67 C66 118.3(15) . . ? C67 C68 C69 121.9(15) . . ? C67 C68 H68 119.1 . . ? C69 C68 H68 119.1 . . ? O5 C69 C68 124.2(15) . . ? O5 C69 C70 118.1(14) . . ? C68 C69 C70 117.5(15) . . ? C71 C70 C75 115.9(14) . . ? C71 C70 C69 117.5(14) . . ? C75 C70 C69 126.6(15) . . ? C72 C71 C70 124.7(16) . . ? C72 C71 H71 117.7 . . ? C70 C71 H71 117.7 . . ? C71 C72 C73 118.4(18) . . ? C71 C72 H72 120.8 . . ? C73 C72 H72 120.8 . . ? C72 C73 C74 121.1(17) . . ? C72 C73 H73 119.5 . . ? C74 C73 H73 119.5 . . ? C75 C74 C73 120.4(17) . . ? C75 C74 H74 119.8 . . ? C73 C74 H74 119.8 . . ? C74 C75 C70 119.3(17) . . ? C74 C75 H75 120.4 . . ? C70 C75 H75 120.4 . . ? C81 C76 C77 116.9(17) . . ? C81 C76 H76 121.6 . . ? C77 C76 H76 121.6 . . ? C78 C77 C76 120(2) . . ? C78 C77 H77 120.2 . . ? C76 C77 H77 120.2 . . ? C77 C78 C79 127(3) . . ? C77 C78 H78 116.7 . . ? C79 C78 H78 116.7 . . ? C78 C79 C80 117(2) . . ? C78 C79 H79 121.7 . . ? C80 C79 H79 121.7 . . ? C81 C80 C79 119(2) . . ? C81 C80 H80 120.4 . . ? C79 C80 H80 120.4 . . ? C76 C81 C80 120.5(16) . . ? C76 C81 C82 120.8(16) . . ? C80 C81 C82 118.6(17) . . ? O18 C82 C83 128.0(14) . . ? O18 C82 C81 111.0(15) . . ? C83 C82 C81 120.5(16) . . ? C82 C83 C84 121.0(14) . . ? C82 C83 H83 119.5 . . ? C84 C83 H83 119.5 . . ? O17 C84 C83 123.6(14) . . ? O17 C84 C85 120.8(14) . . ? C83 C84 C85 115.4(15) . . ? C86 C85 C90 109.2(17) . . ? C86 C85 C84 131.8(18) . . ? C90 C85 C84 119.0(16) . . ? C87 C86 C85 130(2) . . ? C87 C86 H86 115.2 . . ? C85 C86 H86 115.2 . . ? C86 C87 C88 118(2) . . ? C86 C87 H87 120.9 . . ? C88 C87 H87 120.9 . . ? C87 C88 C89 118(2) . . ? C87 C88 H88 121.1 . . ? C89 C88 H88 121.1 . . ? C90 C89 C88 118(2) . . ? C90 C89 H89 121.1 . . ? C88 C89 H89 121.1 . . ? C89 C90 C85 127.2(19) . . ? C89 C90 H90 116.4 . . ? C85 C90 H90 116.4 . . ? O16 C91 O15 122.7(15) . . ? O16 C91 C92 118.1(18) . . ? O15 C91 C92 119.2(16) . . ? C99 C92 N3 118.5(14) . . ? C99 C92 C91 110.0(14) . . ? N3 C92 C91 107.1(13) . . ? N3 C92 C93B 111(2) . . ? C91 C92 C93B 107(2) . . ? C99 C92 C93A 108.9(15) . . ? N3 C92 C93A 103.9(13) . . ? C91 C92 C93A 107.9(15) . . ? N3 C92 C199 100.3(17) . . ? C91 C92 C199 115.2(19) . . ? C93B C92 C199 116(2) . . ? C94A C93A C98A 120.0 . . ? C94A C93A C92 123.3(16) . . ? C98A C93A C92 116.3(16) . . ? C95A C94A C93A 120.0 . . ? C95A C94A H94A 120.0 . . ? C93A C94A H94A 120.0 . . ? C94A C95A C96A 120.0 . . ? C94A C95A H95A 120.0 . . ? C96A C95A H95A 120.0 . . ? C97A C96A C95A 120.0 . . ? C97A C96A H96A 120.0 . . ? C95A C96A H96A 120.0 . . ? C96A C97A C98A 120.0 . . ? C96A C97A H97A 120.0 . . ? C98A C97A H97A 120.0 . . ? C97A C98A C93A 120.0 . . ? C97A C98A H98A 120.0 . . ? C93A C98A H98A 120.0 . . ? C94B C93B C98B 120.0 . . ? C94B C93B C92 119(3) . . ? C98B C93B C92 120(3) . . ? C93B C94B C95B 120.0 . . ? C93B C94B H94B 120.0 . . ? C95B C94B H94B 120.0 . . ? C94B C95B C96B 120.0 . . ? C94B C95B H95B 120.0 . . ? C96B C95B H95B 120.0 . . ? C95B C96B C97B 120.0 . . ? C95B C96B H96B 120.0 . . ? C97B C96B H96B 120.0 . . ? C98B C97B C96B 120.0 . . ? C98B C97B H97B 120.0 . . ? C96B C97B H97B 120.0 . . ? C97B C98B C93B 120.0 . . ? C97B C98B H98B 120.0 . . ? C93B C98B H98B 120.0 . . ? C100 C99 C104 120.0 . . ? C100 C99 C92 116.5(15) . . ? C104 C99 C92 123.4(15) . . ? C99 C100 C101 120.0 . . ? C99 C100 H100 120.0 . . ? C101 C100 H100 120.0 . . ? C102 C101 C100 120.0 . . ? C102 C101 H101 120.0 . . ? C100 C101 H101 120.0 . . ? C103 C102 C101 120.0 . . ? C103 C102 H102 120.0 . . ? C101 C102 H102 120.0 . . ? C104 C103 C102 120.0 . . ? C104 C103 H103 120.0 . . ? C102 C103 H103 120.0 . . ? C103 C104 C99 120.0 . . ? C103 C104 H104 120.0 . . ? C99 C104 H104 120.0 . . ? C200 C199 C204 120.0 . . ? C200 C199 C92 120(3) . . ? C204 C199 C92 119(3) . . ? C199 C200 C201 120.0 . . ? C199 C200 H200 120.0 . . ? C201 C200 H200 120.0 . . ? C202 C201 C200 120.0 . . ? C202 C201 H201 120.0 . . ? C200 C201 H201 120.0 . . ? C201 C202 C203 120.0 . . ? C201 C202 H202 120.0 . . ? C203 C202 H202 120.0 . . ? C204 C203 C202 120.0 . . ? C204 C203 H203 120.0 . . ? C202 C203 H203 120.0 . . ? C203 C204 C199 120.0 . . ? C203 C204 H204 120.0 . . ? C199 C204 H204 120.0 . . ? O12 C105 O11 120.2(16) . . ? O12 C105 C106 120.7(17) . . ? O11 C105 C106 117.7(18) . . ? C105 C106 N2 107.9(13) . . ? C105 C106 C107 109.0(14) . . ? N2 C106 C107 108.3(12) . . ? C105 C106 C213 109.5(16) . . ? N2 C106 C213 111.7(16) . . ? C107 C106 C213 110.4(16) . . ? C105 C106 C113 107.9(15) . . ? N2 C106 C113 111.0(13) . . ? C107 C106 C113 112.6(14) . . ? C112 C107 C108 117.5(17) . . ? C112 C107 C106 121.6(17) . . ? C108 C107 C106 120.8(15) . . ? C109 C108 C107 123.6(19) . . ? C109 C108 H108 118.2 . . ? C107 C108 H108 118.2 . . ? C108 C109 C110 117(2) . . ? C108 C109 H109 121.6 . . ? C110 C109 H109 121.6 . . ? C111 C110 C109 120(2) . . ? C111 C110 H110 119.9 . . ? C109 C110 H110 119.9 . . ? C110 C111 C112 125(2) . . ? C110 C111 H111 117.6 . . ? C112 C111 H111 117.6 . . ? C107 C112 C111 117(2) . . ? C107 C112 H112 121.6 . . ? C111 C112 H112 121.6 . . ? C114 C113 C118 120.0 . . ? C114 C113 C106 118.9(17) . . ? C118 C113 C106 120.9(17) . . ? C113 C114 C115 120.0 . . ? C113 C114 H114 120.0 . . ? C115 C114 H114 120.0 . . ? C114 C115 C116 120.0 . . ? C114 C115 H115 120.0 . . ? C116 C115 H115 120.0 . . ? C115 C116 C117 120.0 . . ? C115 C116 H116 120.0 . . ? C117 C116 H116 120.0 . . ? C118 C117 C116 120.0 . . ? C118 C117 H117 120.0 . . ? C116 C117 H117 120.0 . . ? C117 C118 C113 120.0 . . ? C117 C118 H118 120.0 . . ? C113 C118 H118 120.0 . . ? C214 C213 C218 120.0 . . ? C214 C213 C106 121(2) . . ? C218 C213 C106 119(2) . . ? C215 C214 C213 120.0 . . ? C215 C214 H214 120.0 . . ? C213 C214 H214 120.0 . . ? C214 C215 C216 120.0 . . ? C214 C215 H215 120.0 . . ? C216 C215 H215 120.0 . . ? C217 C216 C215 120.0 . . ? C217 C216 H216 120.0 . . ? C215 C216 H216 120.0 . . ? C216 C217 C218 120.0 . . ? C216 C217 H217 120.0 . . ? C218 C217 H217 120.0 . . ? C217 C218 C213 120.0 . . ? C217 C218 H218 120.0 . . ? C213 C218 H218 120.0 . . ? O8 C119 O7 125.5(16) . . ? O8 C119 C120 119.6(19) . . ? O7 C119 C120 114.9(18) . . ? N1 C120 C121 109.8(14) . . ? N1 C120 C119 106.8(14) . . ? C121 C120 C119 109.5(14) . . ? N1 C120 C221 104.3(15) . . ? C119 C120 C221 115.1(16) . . ? N1 C120 C227 108.6(16) . . ? C119 C120 C227 116.9(18) . . ? C221 C120 C227 104.4(19) . . ? N1 C120 C127 108.9(12) . . ? C121 C120 C127 110.3(16) . . ? C119 C120 C127 111.5(16) . . ? C122 C121 C126 120.0 . . ? C122 C121 C120 119.2(17) . . ? C126 C121 C120 120.8(17) . . ? C123 C122 C121 120.0 . . ? C123 C122 H122 120.0 . . ? C121 C122 H122 120.0 . . ? C122 C123 C124 120.0 . . ? C122 C123 H123 120.0 . . ? C124 C123 H123 120.0 . . ? C123 C124 C125 120.0 . . ? C123 C124 H124 120.0 . . ? C125 C124 H124 120.0 . . ? C126 C125 C124 120.0 . . ? C126 C125 H125 120.0 . . ? C124 C125 H125 120.0 . . ? C125 C126 C121 120.0 . . ? C125 C126 H126 120.0 . . ? C121 C126 H126 120.0 . . ? C222 C221 C226 120.0 . . ? C222 C221 C120 123(2) . . ? C226 C221 C120 117(2) . . ? C223 C222 C221 120.0 . . ? C223 C222 H222 120.0 . . ? C221 C222 H222 120.0 . . ? C222 C223 C224 120.0 . . ? C222 C223 H223 120.0 . . ? C224 C223 H223 120.0 . . ? C225 C224 C223 120.0 . . ? C225 C224 H224 120.0 . . ? C223 C224 H224 120.0 . . ? C226 C225 C224 120.0 . . ? C226 C225 H225 120.0 . . ? C224 C225 H225 120.0 . . ? C225 C226 C221 120.0 . . ? C225 C226 H226 120.0 . . ? C221 C226 H226 120.0 . . ? C128 C127 C132 120.0 . . ? C128 C127 C120 125.0(19) . . ? C132 C127 C120 114.2(19) . . ? C127 C128 C129 120.0 . . ? C127 C128 H128 120.0 . . ? C129 C128 H128 120.0 . . ? C130 C129 C128 120.0 . . ? C130 C129 H129 120.0 . . ? C128 C129 H129 120.0 . . ? C129 C130 C131 120.0 . . ? C129 C130 H130 120.0 . . ? C131 C130 H130 120.0 . . ? C130 C131 C132 120.0 . . ? C130 C131 H131 120.0 . . ? C132 C131 H131 120.0 . . ? C131 C132 C127 120.0 . . ? C131 C132 H132 120.0 . . ? C127 C132 H132 120.0 . . ? C228 C227 C232 120.0 . . ? C228 C227 C120 121(2) . . ? C232 C227 C120 119(2) . . ? C229 C228 C227 120.0 . . ? C229 C228 H228 120.0 . . ? C227 C228 H228 120.0 . . ? C230 C229 C228 120.0 . . ? C230 C229 H229 120.0 . . ? C228 C229 H229 120.0 . . ? C229 C230 C231 120.0 . . ? C229 C230 H230 120.0 . . ? C231 C230 H230 120.0 . . ? C230 C231 C232 120.0 . . ? C230 C231 H23B 120.0 . . ? C232 C231 H23B 120.0 . . ? C231 C232 C227 120.0 . . ? C231 C232 H232 120.0 . . ? C227 C232 H232 120.0 . . ? O19 C133 O20 127.8(15) . . ? O19 C133 C134 118.5(15) . . ? O20 C133 C134 113.7(16) . . ? C235 C134 N4 112.2(14) . . ? N4 C134 C141 117.0(17) . . ? C235 C134 C133 114.1(17) . . ? N4 C134 C133 106.7(12) . . ? C141 C134 C133 116.0(17) . . ? C235 C134 C241 111.7(18) . . ? N4 C134 C241 102.5(13) . . ? C133 C134 C241 108.9(14) . . ? N4 C134 C135 110.8(15) . . ? C141 C134 C135 105.6(19) . . ? C133 C134 C135 99.3(17) . . ? C136 C135 C140 120.0 . . ? C136 C135 C134 123(2) . . ? C140 C135 C134 116(2) . . ? C137 C136 C135 120.0 . . ? C137 C136 H136 120.0 . . ? C135 C136 H136 120.0 . . ? C136 C137 C138 120.0 . . ? C136 C137 H137 120.0 . . ? C138 C137 H137 120.0 . . ? C137 C138 C139 120.0 . . ? C137 C138 H138 120.0 . . ? C139 C138 H138 120.0 . . ? C138 C139 C140 120.0 . . ? C138 C139 H139 120.0 . . ? C140 C139 H139 120.0 . . ? C139 C140 C135 120.0 . . ? C139 C140 H140 120.0 . . ? C135 C140 H140 120.0 . . ? C236 C235 C240 120.0 . . ? C236 C235 C134 116.9(18) . . ? C240 C235 C134 121.9(18) . . ? C235 C236 C237 120.0 . . ? C235 C236 H236 120.0 . . ? C237 C236 H236 120.0 . . ? C236 C237 C238 120.0 . . ? C236 C237 H237 120.0 . . ? C238 C237 H237 120.0 . . ? C239 C238 C237 120.0 . . ? C239 C238 H238 120.0 . . ? C237 C238 H238 120.0 . . ? C240 C239 C238 120.0 . . ? C240 C239 H239 120.0 . . ? C238 C239 H239 120.0 . . ? C239 C240 C235 120.0 . . ? C239 C240 H240 120.0 . . ? C235 C240 H240 120.0 . . ? C142 C141 C146 120.0 . . ? C142 C141 C134 123(2) . . ? C146 C141 C134 115(2) . . ? C143 C142 C141 120.0 . . ? C143 C142 H142 120.0 . . ? C141 C142 H142 120.0 . . ? C142 C143 C144 120.0 . . ? C142 C143 H143 120.0 . . ? C144 C143 H143 120.0 . . ? C145 C144 C143 120.0 . . ? C145 C144 H144 120.0 . . ? C143 C144 H144 120.0 . . ? C144 C145 C146 120.0 . . ? C144 C145 H145 120.0 . . ? C146 C145 H145 120.0 . . ? C145 C146 C141 120.0 . . ? C145 C146 H146 120.0 . . ? C141 C146 H146 120.0 . . ? C242 C241 C246 120.0 . . ? C242 C241 C134 120.6(17) . . ? C246 C241 C134 119.3(17) . . ? C243 C242 C241 120.0 . . ? C243 C242 H242 120.0 . . ? C241 C242 H242 120.0 . . ? C244 C243 C242 120.0 . . ? C244 C243 H243 120.0 . . ? C242 C243 H243 120.0 . . ? C243 C244 C245 120.0 . . ? C243 C244 H244 120.0 . . ? C245 C244 H244 120.0 . . ? C246 C245 C244 120.0 . . ? C246 C245 H245 120.0 . . ? C244 C245 H245 120.0 . . ? C245 C246 C241 120.0 . . ? C245 C246 H246 120.0 . . ? C241 C246 H246 120.0 . . ? C152 C151 C156 120.0 . . ? C152 C151 C157 121(3) . . ? C156 C151 C157 119(3) . . ? C151 C152 C153 120.0 . . ? C151 C152 H152 120.0 . . ? C153 C152 H152 120.0 . . ? C152 C153 C154 120.0 . . ? C152 C153 H153 120.0 . . ? C154 C153 H153 120.0 . . ? C153 C154 C155 120.0 . . ? C153 C154 H154 120.0 . . ? C155 C154 H154 120.0 . . ? C156 C155 C154 120.0 . . ? C156 C155 H155 120.0 . . ? C154 C155 H155 120.0 . . ? C155 C156 C151 120.0 . . ? C155 C156 H156 120.0 . . ? C151 C156 H156 120.0 . . ? C151 C157 H157 109.5 . . ? C151 C157 H158 109.5 . . ? H157 C157 H158 109.5 . . ? C151 C157 H160 109.5 . . ? H157 C157 H160 109.5 . . ? H158 C157 H160 109.5 . . ? _refine_diff_density_max 0.820 _refine_diff_density_min -0.496 _refine_diff_density_rms 0.104 #END=========================================================================== #-- _database_code_depnum_ccdc_archive 'CCDC 915214'