# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_publication_text _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author_name 'Xuelan Mei' _publ_contact_author_address ; Department of Chemistry Nankai University Tianjin 300071, P.R. China ; _publ_contact_author_email daluhuashu@126.com loop_ _publ_author_name _publ_author_address 'Xue-Lan Mei' ;Department of Chemistry Nankai University Tianjin 300071, P.R. China ; 'Li-Cun Li' ; Department of Chemistry Nankai University Tianjin 300071, P.R. China ; data_1 _database_code_depnum_ccdc_archive 'CCDC 832559' #TrackingRef 'CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H45 Gd N4.5 O9' _chemical_formula_weight 805.98 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' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M c2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 24.180(5) _cell_length_b 15.012(3) _cell_length_c 19.798(4) _cell_angle_alpha 90.00 _cell_angle_beta 100.55(3) _cell_angle_gamma 90.00 _cell_volume 7065(2) _cell_formula_units_Z 8 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 10066 _cell_measurement_theta_min 1.6044 _cell_measurement_theta_max 27.8784 _exptl_crystal_description sheet _exptl_crystal_colour purpleblue _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.516 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3284 _exptl_absorpt_coefficient_mu 1.935 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.6982 _exptl_absorpt_correction_T_max 0.8927 _exptl_absorpt_process_details CrystalClear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn CCD area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 34605 _diffrn_reflns_av_R_equivalents 0.1078 _diffrn_reflns_av_sigmaI/netI 0.0762 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 25.02 _reflns_number_total 6228 _reflns_number_gt 4595 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'CrystalStructure 3.8' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0467P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00028(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6228 _refine_ls_number_parameters 443 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0734 _refine_ls_R_factor_gt 0.0501 _refine_ls_wR_factor_ref 0.1151 _refine_ls_wR_factor_gt 0.1053 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd1 Gd 0.170939(6) -0.002656(11) 0.100253(8) 0.01970(5) Uani 1 1 d . . . O1 O 0.13321(10) -0.14798(16) 0.09480(12) 0.0266(7) Uani 1 1 d . . . O2 O 0.09132(10) -0.00314(15) 0.01554(13) 0.0266(7) Uani 1 1 d . . . O3 O 0.25569(10) -0.07598(16) 0.13986(12) 0.0270(7) Uani 1 1 d . . . O4 O 0.20639(10) -0.05182(16) 0.00335(12) 0.0269(7) Uani 1 1 d . . . O5 O 0.16611(10) -0.03590(16) 0.21558(12) 0.0256(7) Uani 1 1 d . . . O6 O 0.11164(9) 0.10585(15) 0.13909(12) 0.0237(7) Uani 1 1 d . . . O7 O 0.18852(10) 0.12734(15) 0.03245(12) 0.0275(7) Uani 1 1 d . . . O8 O 0.16771(11) 0.38844(17) 0.15051(13) 0.0372(8) Uani 1 1 d . . . O9 O 0.48358(13) 0.12122(18) 0.13128(13) 0.0494(10) Uani 1 1 d . . . N1 N 0.23510(11) 0.12419(18) 0.17294(14) 0.0211(8) Uani 1 1 d . . . N2 N 0.17461(12) 0.20753(18) 0.04691(14) 0.0208(8) Uani 1 1 d . . . N3 N 0.16511(12) 0.33069(19) 0.10212(14) 0.0238(8) Uani 1 1 d . . . N4 N 0.53421(14) 0.2859(2) 0.21159(17) 0.0410(10) Uani 1 1 d . . . N5 N 0.49311(13) 0.09614(19) 0.19385(15) 0.0300(9) Uani 1 1 d . . . C1 C 0.09647(18) -0.2905(2) 0.0595(2) 0.0405(13) Uani 1 1 d . . . H1A H 0.1327 -0.3135 0.0801 0.061 Uiso 1 1 calc R . . H1B H 0.0836 -0.3199 0.0165 0.061 Uiso 1 1 calc R . . H1C H 0.0702 -0.3009 0.0896 0.061 Uiso 1 1 calc R . . C2 C 0.10110(15) -0.1910(2) 0.04744(19) 0.0261(10) Uani 1 1 d . . . C3 C 0.07055(16) -0.1539(2) -0.01130(19) 0.0314(11) Uani 1 1 d . . . H3 H 0.0520 -0.1924 -0.0448 0.038 Uiso 1 1 calc R . . C4 C 0.06530(14) -0.0611(3) -0.02444(18) 0.0253(10) Uani 1 1 d . . . C5 C 0.02619(16) -0.0293(3) -0.0868(2) 0.0340(11) Uani 1 1 d . . . H5A H 0.0245 0.0346 -0.0862 0.051 Uiso 1 1 calc R . . H5B H -0.0107 -0.0533 -0.0871 0.051 Uiso 1 1 calc R . . H5C H 0.0395 -0.0486 -0.1271 0.051 Uiso 1 1 calc R . . C6 C 0.33086(14) -0.1778(2) 0.16417(18) 0.0298(11) Uani 1 1 d . . . H6A H 0.3464 -0.1381 0.2008 0.045 Uiso 1 1 calc R . . H6B H 0.3602 -0.1981 0.1412 0.045 Uiso 1 1 calc R . . H6C H 0.3140 -0.2280 0.1827 0.045 Uiso 1 1 calc R . . C7 C 0.28684(15) -0.1296(2) 0.11370(18) 0.0261(10) Uani 1 1 d . . . C8 C 0.28206(16) -0.1471(2) 0.04407(18) 0.0282(10) Uani 1 1 d . . . H8A H 0.3066 -0.1885 0.0307 0.034 Uiso 1 1 calc R . . C9 C 0.24284(16) -0.1065(2) -0.00733(18) 0.0276(10) Uani 1 1 d . . . C10 C 0.24475(18) -0.1282(2) -0.08131(18) 0.0373(12) Uani 1 1 d . . . H10A H 0.2072 -0.1371 -0.1062 0.056 Uiso 1 1 calc R . . H10B H 0.2663 -0.1815 -0.0833 0.056 Uiso 1 1 calc R . . H10C H 0.2620 -0.0798 -0.1015 0.056 Uiso 1 1 calc R . . C11 C 0.15861(17) -0.0455(3) 0.33273(18) 0.0359(12) Uani 1 1 d . . . H11A H 0.1395 -0.1018 0.3279 0.054 Uiso 1 1 calc R . . H11B H 0.1445 -0.0100 0.3662 0.054 Uiso 1 1 calc R . . H11C H 0.1982 -0.0552 0.3476 0.054 Uiso 1 1 calc R . . C12 C 0.14866(14) 0.0019(2) 0.26502(18) 0.0218(9) Uani 1 1 d . . . C13 C 0.11899(15) 0.0834(2) 0.25801(19) 0.0277(10) Uani 1 1 d . . . H13 H 0.1101 0.1086 0.2976 0.033 Uiso 1 1 calc R . . C14 C 0.10215(14) 0.1289(2) 0.19674(18) 0.0222(9) Uani 1 1 d . . . C15 C 0.06760(15) 0.2133(2) 0.19857(19) 0.0290(11) Uani 1 1 d . . . H15A H 0.0901 0.2642 0.1921 0.043 Uiso 1 1 calc R . . H15B H 0.0558 0.2177 0.2422 0.043 Uiso 1 1 calc R . . H15C H 0.0351 0.2112 0.1626 0.043 Uiso 1 1 calc R . . C16 C 0.27386(15) 0.0939(2) 0.22442(18) 0.0270(10) Uani 1 1 d . . . H16 H 0.2793 0.0327 0.2287 0.032 Uiso 1 1 calc R . . C17 C 0.30621(15) 0.1487(2) 0.27149(18) 0.0258(10) Uani 1 1 d . . . H17 H 0.3331 0.1243 0.3061 0.031 Uiso 1 1 calc R . . C18 C 0.29879(15) 0.2397(2) 0.26741(18) 0.0280(10) Uani 1 1 d . . . H18 H 0.3202 0.2777 0.2990 0.034 Uiso 1 1 calc R . . C19 C 0.25827(15) 0.2729(2) 0.21451(18) 0.0261(10) Uani 1 1 d . . . H19 H 0.2514 0.3338 0.2103 0.031 Uiso 1 1 calc R . . C20 C 0.22828(14) 0.2138(2) 0.16820(17) 0.0205(9) Uani 1 1 d . . . C21 C 0.18914(14) 0.2479(2) 0.10785(17) 0.0209(9) Uani 1 1 d . . . C22 C 0.13550(17) 0.3516(3) 0.03103(19) 0.0346(11) Uani 1 1 d . . . C23 C 0.13731(16) 0.2617(2) -0.00610(19) 0.0293(11) Uani 1 1 d . . . C24 C 0.1701(3) 0.4254(3) 0.0052(2) 0.105(2) Uani 1 1 d . . . H24A H 0.1520 0.4439 -0.0398 0.157 Uiso 1 1 calc R . . H24B H 0.2071 0.4032 0.0032 0.157 Uiso 1 1 calc R . . H24C H 0.1731 0.4752 0.0361 0.157 Uiso 1 1 calc R . . C25 C 0.0791(2) 0.3890(4) 0.0339(2) 0.108(2) Uani 1 1 d . . . H25A H 0.0573 0.3456 0.0531 0.162 Uiso 1 1 calc R . . H25B H 0.0603 0.4041 -0.0117 0.162 Uiso 1 1 calc R . . H25C H 0.0833 0.4415 0.0621 0.162 Uiso 1 1 calc R . . C26 C 0.08152(19) 0.2135(3) -0.0223(3) 0.091(2) Uani 1 1 d . . . H26A H 0.0866 0.1573 -0.0435 0.136 Uiso 1 1 calc R . . H26B H 0.0550 0.2490 -0.0530 0.136 Uiso 1 1 calc R . . H26C H 0.0676 0.2035 0.0195 0.136 Uiso 1 1 calc R . . C27 C 0.1639(2) 0.2655(3) -0.0691(2) 0.0698(18) Uani 1 1 d . . . H27A H 0.2007 0.2914 -0.0574 0.105 Uiso 1 1 calc R . . H27B H 0.1410 0.3012 -0.1036 0.105 Uiso 1 1 calc R . . H27C H 0.1669 0.2063 -0.0864 0.105 Uiso 1 1 calc R . . C28 C 0.53282(17) 0.3776(3) 0.2129(2) 0.0397(12) Uani 1 1 d . . . H28 H 0.5551 0.4092 0.1875 0.048 Uiso 1 1 calc R . . C29 C 0.5000 0.4243(4) 0.2500 0.0420(19) Uani 1 2 d S . . H29 H 0.5000 0.4862 0.2500 0.050 Uiso 1 2 calc SR . . C32 C 0.5000 0.2450(3) 0.2500 0.0245(14) Uani 1 2 d S . . C33 C 0.5000 0.1466(3) 0.2500 0.0261(14) Uani 1 2 d S . . C34 C 0.50376(17) -0.0002(2) 0.21142(18) 0.0272(10) Uani 1 1 d . . . C36 C 0.56893(16) -0.0132(2) 0.2106(2) 0.0405(12) Uani 1 1 d . . . H36A H 0.5761 0.0000 0.1655 0.061 Uiso 1 1 calc R . . H36B H 0.5795 -0.0737 0.2222 0.061 Uiso 1 1 calc R . . H36C H 0.5905 0.0263 0.2434 0.061 Uiso 1 1 calc R . . C37 C 0.46991(17) -0.0618(3) 0.1623(2) 0.0403(13) Uani 1 1 d . . . H37A H 0.4308 -0.0465 0.1574 0.060 Uiso 1 1 calc R . . H37B H 0.4755 -0.1218 0.1791 0.060 Uiso 1 1 calc R . . H37C H 0.4814 -0.0573 0.1185 0.060 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.02179(10) 0.02058(9) 0.01600(10) -0.00049(8) 0.00151(8) 0.00054(9) O1 0.0265(14) 0.0292(14) 0.0229(14) -0.0005(11) 0.0014(11) -0.0012(12) O2 0.0257(13) 0.0293(14) 0.0239(14) -0.0028(11) 0.0023(11) -0.0026(12) O3 0.0274(14) 0.0292(14) 0.0242(14) -0.0052(11) 0.0041(11) 0.0027(12) O4 0.0298(14) 0.0279(14) 0.0252(14) -0.0009(11) 0.0106(11) 0.0049(12) O5 0.0285(14) 0.0272(13) 0.0214(14) 0.0013(11) 0.0053(11) 0.0022(12) O6 0.0218(13) 0.0243(13) 0.0251(14) -0.0019(11) 0.0049(11) -0.0013(11) O7 0.0369(15) 0.0189(12) 0.0278(14) 0.0011(11) 0.0089(12) 0.0024(12) O8 0.0383(16) 0.0325(15) 0.0404(16) -0.0107(13) 0.0058(13) 0.0085(13) O9 0.082(2) 0.0357(16) 0.0291(17) 0.0007(13) 0.0075(16) -0.0003(16) N1 0.0190(15) 0.0261(16) 0.0190(16) -0.0028(13) 0.0054(13) -0.0026(13) N2 0.0205(16) 0.0204(15) 0.0226(16) 0.0048(13) 0.0066(13) 0.0005(13) N3 0.0234(16) 0.0224(16) 0.0279(18) -0.0004(13) 0.0110(14) -0.0001(13) N4 0.038(2) 0.046(2) 0.040(2) 0.0037(17) 0.0108(17) -0.0052(18) N5 0.041(2) 0.0251(17) 0.0240(17) 0.0018(15) 0.0070(15) 0.0017(15) C1 0.049(3) 0.026(2) 0.044(3) 0.0059(19) 0.001(2) -0.011(2) C2 0.0188(19) 0.028(2) 0.031(2) 0.0010(17) 0.0035(17) -0.0086(17) C3 0.037(2) 0.025(2) 0.028(2) 0.0005(17) -0.0048(19) -0.0064(18) C4 0.0182(19) 0.038(2) 0.020(2) -0.0026(17) 0.0055(16) -0.0043(17) C5 0.033(2) 0.042(2) 0.024(2) 0.0031(19) -0.0015(18) -0.0055(19) C6 0.026(2) 0.030(2) 0.032(2) -0.0033(18) 0.0029(18) 0.0028(17) C7 0.029(2) 0.0208(18) 0.027(2) -0.0004(16) 0.0008(17) -0.0031(17) C8 0.038(2) 0.0247(19) 0.025(2) 0.0009(16) 0.0136(17) 0.0028(18) C9 0.035(2) 0.0222(19) 0.026(2) -0.0007(17) 0.0070(18) -0.0034(18) C10 0.051(3) 0.029(2) 0.032(2) -0.0019(18) 0.010(2) 0.007(2) C11 0.053(3) 0.031(2) 0.024(2) 0.0042(18) 0.0066(19) 0.000(2) C12 0.0244(17) 0.0269(18) 0.0149(18) -0.0020(16) 0.0055(15) -0.0097(17) C13 0.031(2) 0.025(2) 0.029(2) -0.0023(17) 0.0105(17) -0.0005(17) C14 0.0161(18) 0.0255(19) 0.025(2) -0.0077(16) 0.0052(16) -0.0090(16) C15 0.022(2) 0.032(2) 0.033(2) -0.0019(18) 0.0045(17) 0.0002(17) C16 0.030(2) 0.029(2) 0.023(2) 0.0011(17) 0.0077(17) 0.0040(17) C17 0.021(2) 0.034(2) 0.021(2) -0.0076(17) 0.0025(16) 0.0039(17) C18 0.024(2) 0.036(2) 0.023(2) -0.0084(17) 0.0025(17) 0.0003(18) C19 0.031(2) 0.0228(19) 0.025(2) -0.0060(16) 0.0059(17) -0.0051(17) C20 0.0156(18) 0.0272(19) 0.0209(19) -0.0010(16) 0.0094(15) -0.0017(16) C21 0.0186(18) 0.0217(18) 0.024(2) 0.0012(15) 0.0089(15) -0.0004(16) C22 0.051(3) 0.031(2) 0.023(2) 0.0079(18) 0.0106(19) 0.013(2) C23 0.031(2) 0.028(2) 0.027(2) 0.0063(18) -0.0016(18) -0.0022(18) C24 0.246(7) 0.036(3) 0.041(3) -0.005(2) 0.050(4) -0.051(4) C25 0.087(4) 0.180(5) 0.045(3) -0.044(3) -0.021(3) 0.098(4) C26 0.048(3) 0.049(3) 0.150(5) 0.044(3) -0.051(3) -0.019(3) C27 0.145(5) 0.046(3) 0.026(2) 0.008(2) 0.033(3) 0.038(3) C28 0.033(2) 0.044(2) 0.039(3) 0.016(2) 0.001(2) -0.014(2) C29 0.056(4) 0.023(3) 0.042(4) 0.000 -0.005(3) 0.000 C32 0.033(3) 0.018(3) 0.023(3) 0.000 0.008(2) 0.000 C33 0.033(3) 0.028(3) 0.019(3) 0.000 0.012(2) 0.000 C34 0.050(2) 0.0180(17) 0.019(2) -0.0021(15) 0.0220(17) -0.0061(18) C36 0.040(2) 0.036(2) 0.050(3) -0.005(2) 0.022(2) -0.001(2) C37 0.047(3) 0.028(2) 0.045(3) -0.007(2) 0.006(2) -0.001(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 Gd1 O2 2.310(2) . ? Gd1 O3 2.332(2) . ? Gd1 O4 2.358(2) . ? Gd1 O1 2.359(2) . ? Gd1 O5 2.361(2) . ? Gd1 O6 2.388(2) . ? Gd1 O7 2.450(2) . ? Gd1 N1 2.699(3) . ? O1 C2 1.278(4) . ? O2 C4 1.263(4) . ? O3 C7 1.275(4) . ? O4 C9 1.251(4) . ? O5 C12 1.269(4) . ? O6 C14 1.254(4) . ? O7 N2 1.296(3) . ? O8 N3 1.285(4) . ? O9 N5 1.275(4) . ? N1 C16 1.332(4) . ? N1 C20 1.357(4) . ? N2 C21 1.339(4) . ? N2 C23 1.493(4) . ? N3 C21 1.367(4) . ? N3 C22 1.491(4) . ? N4 C32 1.368(4) . ? N4 C28 1.378(5) . ? N5 C33 1.331(4) . ? N5 C34 1.499(4) . ? C1 C2 1.519(5) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.376(5) . ? C3 C4 1.419(5) . ? C3 H3 0.9300 . ? C4 C5 1.489(5) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 C7 1.506(5) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 C8 1.387(5) . ? C8 C9 1.397(5) . ? C8 H8A 0.9300 . ? C9 C10 1.509(5) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C12 1.498(5) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C13 1.412(5) . ? C13 C14 1.387(5) . ? C13 H13 0.9300 . ? C14 C15 1.521(5) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 C17 1.374(5) . ? C16 H16 0.9300 . ? C17 C18 1.379(5) . ? C17 H17 0.9300 . ? C18 C19 1.389(5) . ? C18 H18 0.9300 . ? C19 C20 1.382(5) . ? C19 H19 0.9300 . ? C20 C21 1.474(4) . ? C22 C25 1.485(6) . ? C22 C24 1.531(6) . ? C22 C23 1.541(5) . ? C23 C27 1.505(6) . ? C23 C26 1.513(6) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 C29 1.369(5) . ? C28 H28 0.9300 . ? C29 C28 1.369(5) 2_655 ? C29 H29 0.9300 . ? C32 N4 1.368(4) 2_655 ? C32 C33 1.476(7) . ? C33 N5 1.331(4) 2_655 ? C34 C37 1.476(5) . ? C34 C34 1.571(7) 2_655 ? C34 C36 1.591(5) . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Gd1 O3 143.79(8) . . ? O2 Gd1 O4 77.72(9) . . ? O3 Gd1 O4 72.41(8) . . ? O2 Gd1 O1 72.54(8) . . ? O3 Gd1 O1 83.54(8) . . ? O4 Gd1 O1 82.45(9) . . ? O2 Gd1 O5 121.28(9) . . ? O3 Gd1 O5 76.77(9) . . ? O4 Gd1 O5 144.12(8) . . ? O1 Gd1 O5 76.21(8) . . ? O2 Gd1 O6 76.48(8) . . ? O3 Gd1 O6 139.13(8) . . ? O4 Gd1 O6 143.55(8) . . ? O1 Gd1 O6 113.29(8) . . ? O5 Gd1 O6 72.17(8) . . ? O2 Gd1 O7 79.04(8) . . ? O3 Gd1 O7 109.29(8) . . ? O4 Gd1 O7 71.22(8) . . ? O1 Gd1 O7 144.69(8) . . ? O5 Gd1 O7 137.96(8) . . ? O6 Gd1 O7 78.92(8) . . ? O2 Gd1 N1 135.28(8) . . ? O3 Gd1 N1 76.69(8) . . ? O4 Gd1 N1 113.29(9) . . ? O1 Gd1 N1 148.90(8) . . ? O5 Gd1 N1 76.05(9) . . ? O6 Gd1 N1 70.59(8) . . ? O7 Gd1 N1 65.78(8) . . ? C2 O1 Gd1 132.8(2) . . ? C4 O2 Gd1 135.3(2) . . ? C7 O3 Gd1 135.2(2) . . ? C9 O4 Gd1 135.7(2) . . ? C12 O5 Gd1 137.2(2) . . ? C14 O6 Gd1 134.6(2) . . ? N2 O7 Gd1 122.7(2) . . ? C16 N1 C20 116.8(3) . . ? C16 N1 Gd1 115.0(2) . . ? C20 N1 Gd1 127.7(2) . . ? O7 N2 C21 125.7(3) . . ? O7 N2 C23 119.9(3) . . ? C21 N2 C23 114.3(3) . . ? O8 N3 C21 126.1(3) . . ? O8 N3 C22 120.7(3) . . ? C21 N3 C22 113.2(3) . . ? C32 N4 C28 114.8(4) . . ? O9 N5 C33 128.0(3) . . ? O9 N5 C34 120.2(3) . . ? C33 N5 C34 111.5(3) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C3 125.1(3) . . ? O1 C2 C1 115.7(3) . . ? C3 C2 C1 119.2(3) . . ? C2 C3 C4 124.7(3) . . ? C2 C3 H3 117.7 . . ? C4 C3 H3 117.7 . . ? O2 C4 C3 122.9(3) . . ? O2 C4 C5 117.8(3) . . ? C3 C4 C5 119.3(3) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 H6A 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C7 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O3 C7 C8 125.1(3) . . ? O3 C7 C6 115.6(3) . . ? C8 C7 C6 119.2(3) . . ? C7 C8 C9 124.3(4) . . ? C7 C8 H8A 117.9 . . ? C9 C8 H8A 117.9 . . ? O4 C9 C8 124.6(3) . . ? O4 C9 C10 117.0(3) . . ? C8 C9 C10 118.4(3) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C12 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? O5 C12 C13 123.1(3) . . ? O5 C12 C11 117.1(3) . . ? C13 C12 C11 119.7(3) . . ? C14 C13 C12 125.1(4) . . ? C14 C13 H13 117.4 . . ? C12 C13 H13 117.4 . . ? O6 C14 C13 125.9(3) . . ? O6 C14 C15 116.4(3) . . ? C13 C14 C15 117.6(3) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N1 C16 C17 123.2(3) . . ? N1 C16 H16 118.4 . . ? C17 C16 H16 118.4 . . ? C16 C17 C18 120.1(3) . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C17 C18 C19 117.8(3) . . ? C17 C18 H18 121.1 . . ? C19 C18 H18 121.1 . . ? C20 C19 C18 118.8(3) . . ? C20 C19 H19 120.6 . . ? C18 C19 H19 120.6 . . ? N1 C20 C19 123.3(3) . . ? N1 C20 C21 116.9(3) . . ? C19 C20 C21 119.7(3) . . ? N2 C21 N3 107.4(3) . . ? N2 C21 C20 126.7(3) . . ? N3 C21 C20 125.7(3) . . ? C25 C22 N3 109.2(3) . . ? C25 C22 C24 107.6(4) . . ? N3 C22 C24 105.7(3) . . ? C25 C22 C23 117.1(4) . . ? N3 C22 C23 102.4(3) . . ? C24 C22 C23 114.1(4) . . ? N2 C23 C27 108.0(3) . . ? N2 C23 C26 106.7(3) . . ? C27 C23 C26 110.0(4) . . ? N2 C23 C22 102.0(3) . . ? C27 C23 C22 114.6(3) . . ? C26 C23 C22 114.7(4) . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C27 H27A 109.5 . . ? C23 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C23 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 N4 122.6(4) . . ? C29 C28 H28 118.7 . . ? N4 C28 H28 118.7 . . ? C28 C29 C28 118.5(5) 2_655 . ? C28 C29 H29 120.7 2_655 . ? C28 C29 H29 120.7 . . ? N4 C32 N4 126.6(5) 2_655 . ? N4 C32 C33 116.7(2) 2_655 . ? N4 C32 C33 116.7(2) . . ? N5 C33 N5 110.5(5) . 2_655 ? N5 C33 C32 124.7(2) . . ? N5 C33 C32 124.7(2) 2_655 . ? C37 C34 N5 113.6(3) . . ? C37 C34 C34 119.4(3) . 2_655 ? N5 C34 C34 100.4(2) . 2_655 ? C37 C34 C36 110.3(3) . . ? N5 C34 C36 104.1(3) . . ? C34 C34 C36 107.6(4) 2_655 . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C34 C37 H37A 109.5 . . ? C34 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C34 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Gd1 O1 C2 23.1(3) . . . . ? O3 Gd1 O1 C2 -129.4(3) . . . . ? O4 Gd1 O1 C2 -56.3(3) . . . . ? O5 Gd1 O1 C2 152.7(3) . . . . ? O6 Gd1 O1 C2 89.4(3) . . . . ? O7 Gd1 O1 C2 -14.8(4) . . . . ? N1 Gd1 O1 C2 -179.9(3) . . . . ? O3 Gd1 O2 C4 23.6(4) . . . . ? O4 Gd1 O2 C4 58.4(3) . . . . ? O1 Gd1 O2 C4 -27.4(3) . . . . ? O5 Gd1 O2 C4 -88.5(3) . . . . ? O6 Gd1 O2 C4 -147.6(3) . . . . ? O7 Gd1 O2 C4 131.3(3) . . . . ? N1 Gd1 O2 C4 169.2(3) . . . . ? O2 Gd1 O3 C7 19.1(4) . . . . ? O4 Gd1 O3 C7 -16.8(3) . . . . ? O1 Gd1 O3 C7 67.3(3) . . . . ? O5 Gd1 O3 C7 144.6(3) . . . . ? O6 Gd1 O3 C7 -174.2(3) . . . . ? O7 Gd1 O3 C7 -78.8(3) . . . . ? N1 Gd1 O3 C7 -136.8(3) . . . . ? O2 Gd1 O4 C9 -143.2(3) . . . . ? O3 Gd1 O4 C9 16.1(3) . . . . ? O1 Gd1 O4 C9 -69.5(3) . . . . ? O5 Gd1 O4 C9 -15.9(4) . . . . ? O6 Gd1 O4 C9 171.0(3) . . . . ? O7 Gd1 O4 C9 134.3(3) . . . . ? N1 Gd1 O4 C9 82.5(3) . . . . ? O2 Gd1 O5 C12 -73.0(3) . . . . ? O3 Gd1 O5 C12 141.3(3) . . . . ? O4 Gd1 O5 C12 172.5(3) . . . . ? O1 Gd1 O5 C12 -132.3(3) . . . . ? O6 Gd1 O5 C12 -11.8(3) . . . . ? O7 Gd1 O5 C12 37.0(4) . . . . ? N1 Gd1 O5 C12 61.9(3) . . . . ? O2 Gd1 O6 C14 143.9(3) . . . . ? O3 Gd1 O6 C14 -28.2(4) . . . . ? O4 Gd1 O6 C14 -170.1(3) . . . . ? O1 Gd1 O6 C14 79.9(3) . . . . ? O5 Gd1 O6 C14 14.2(3) . . . . ? O7 Gd1 O6 C14 -134.9(3) . . . . ? N1 Gd1 O6 C14 -66.9(3) . . . . ? O2 Gd1 O7 N2 93.5(2) . . . . ? O3 Gd1 O7 N2 -123.1(2) . . . . ? O4 Gd1 O7 N2 174.1(2) . . . . ? O1 Gd1 O7 N2 130.2(2) . . . . ? O5 Gd1 O7 N2 -31.6(3) . . . . ? O6 Gd1 O7 N2 15.3(2) . . . . ? N1 Gd1 O7 N2 -58.2(2) . . . . ? O2 Gd1 N1 C16 171.3(2) . . . . ? O3 Gd1 N1 C16 -28.8(2) . . . . ? O4 Gd1 N1 C16 -92.7(3) . . . . ? O1 Gd1 N1 C16 23.2(3) . . . . ? O5 Gd1 N1 C16 50.6(2) . . . . ? O6 Gd1 N1 C16 126.3(3) . . . . ? O7 Gd1 N1 C16 -147.4(3) . . . . ? O2 Gd1 N1 C20 -0.5(3) . . . . ? O3 Gd1 N1 C20 159.4(3) . . . . ? O4 Gd1 N1 C20 95.5(3) . . . . ? O1 Gd1 N1 C20 -148.6(3) . . . . ? O5 Gd1 N1 C20 -121.2(3) . . . . ? O6 Gd1 N1 C20 -45.5(3) . . . . ? O7 Gd1 N1 C20 40.8(3) . . . . ? Gd1 O7 N2 C21 53.6(4) . . . . ? Gd1 O7 N2 C23 -123.9(3) . . . . ? Gd1 O1 C2 C3 -13.8(6) . . . . ? Gd1 O1 C2 C1 167.5(3) . . . . ? O1 C2 C3 C4 -7.3(7) . . . . ? C1 C2 C3 C4 171.3(4) . . . . ? Gd1 O2 C4 C3 21.3(6) . . . . ? Gd1 O2 C4 C5 -160.7(3) . . . . ? C2 C3 C4 O2 4.3(6) . . . . ? C2 C3 C4 C5 -173.7(4) . . . . ? Gd1 O3 C7 C8 13.3(6) . . . . ? Gd1 O3 C7 C6 -165.2(2) . . . . ? O3 C7 C8 C9 1.4(6) . . . . ? C6 C7 C8 C9 179.9(3) . . . . ? Gd1 O4 C9 C8 -11.5(6) . . . . ? Gd1 O4 C9 C10 169.7(2) . . . . ? C7 C8 C9 O4 -2.2(6) . . . . ? C7 C8 C9 C10 176.5(4) . . . . ? Gd1 O5 C12 C13 6.6(5) . . . . ? Gd1 O5 C12 C11 -175.9(2) . . . . ? O5 C12 C13 C14 4.4(6) . . . . ? C11 C12 C13 C14 -173.0(3) . . . . ? Gd1 O6 C14 C13 -11.8(5) . . . . ? Gd1 O6 C14 C15 170.0(2) . . . . ? C12 C13 C14 O6 -1.6(6) . . . . ? C12 C13 C14 C15 176.6(3) . . . . ? C20 N1 C16 C17 0.0(5) . . . . ? Gd1 N1 C16 C17 -172.7(3) . . . . ? N1 C16 C17 C18 1.0(6) . . . . ? C16 C17 C18 C19 -0.4(6) . . . . ? C17 C18 C19 C20 -1.1(5) . . . . ? C16 N1 C20 C19 -1.6(5) . . . . ? Gd1 N1 C20 C19 170.1(3) . . . . ? C16 N1 C20 C21 174.7(3) . . . . ? Gd1 N1 C20 C21 -13.7(4) . . . . ? C18 C19 C20 N1 2.2(6) . . . . ? C18 C19 C20 C21 -174.0(3) . . . . ? O7 N2 C21 N3 -178.7(3) . . . . ? C23 N2 C21 N3 -1.1(4) . . . . ? O7 N2 C21 C20 6.8(6) . . . . ? C23 N2 C21 C20 -175.6(3) . . . . ? O8 N3 C21 N2 177.4(3) . . . . ? C22 N3 C21 N2 -4.6(4) . . . . ? O8 N3 C21 C20 -8.1(6) . . . . ? C22 N3 C21 C20 169.9(3) . . . . ? N1 C20 C21 N2 -24.9(5) . . . . ? C19 C20 C21 N2 151.5(4) . . . . ? N1 C20 C21 N3 161.6(3) . . . . ? C19 C20 C21 N3 -22.0(5) . . . . ? O8 N3 C22 C25 -49.1(5) . . . . ? C21 N3 C22 C25 132.8(4) . . . . ? O8 N3 C22 C24 66.4(4) . . . . ? C21 N3 C22 C24 -111.7(4) . . . . ? O8 N3 C22 C23 -173.9(3) . . . . ? C21 N3 C22 C23 8.0(4) . . . . ? O7 N2 C23 C27 -55.3(4) . . . . ? C21 N2 C23 C27 127.0(3) . . . . ? O7 N2 C23 C26 62.9(4) . . . . ? C21 N2 C23 C26 -114.8(4) . . . . ? O7 N2 C23 C22 -176.4(3) . . . . ? C21 N2 C23 C22 5.9(4) . . . . ? C25 C22 C23 N2 -127.0(4) . . . . ? N3 C22 C23 N2 -7.6(4) . . . . ? C24 C22 C23 N2 106.0(4) . . . . ? C25 C22 C23 C27 116.6(4) . . . . ? N3 C22 C23 C27 -124.0(4) . . . . ? C24 C22 C23 C27 -10.3(5) . . . . ? C25 C22 C23 C26 -12.1(5) . . . . ? N3 C22 C23 C26 107.3(4) . . . . ? C24 C22 C23 C26 -139.0(4) . . . . ? C32 N4 C28 C29 0.3(5) . . . . ? N4 C28 C29 C28 -0.2(3) . . . 2_655 ? C28 N4 C32 N4 -0.2(2) . . . 2_655 ? C28 N4 C32 C33 179.8(2) . . . . ? O9 N5 C33 N5 177.5(4) . . . 2_655 ? C34 N5 C33 N5 -8.47(19) . . . 2_655 ? O9 N5 C33 C32 -2.5(4) . . . . ? C34 N5 C33 C32 171.54(19) . . . . ? N4 C32 C33 N5 129.7(2) 2_655 . . . ? N4 C32 C33 N5 -50.3(2) . . . . ? N4 C32 C33 N5 -50.3(2) 2_655 . . 2_655 ? N4 C32 C33 N5 129.7(2) . . . 2_655 ? O9 N5 C34 C37 -36.5(5) . . . . ? C33 N5 C34 C37 148.9(3) . . . . ? O9 N5 C34 C34 -165.2(4) . . . 2_655 ? C33 N5 C34 C34 20.2(4) . . . 2_655 ? O9 N5 C34 C36 83.5(4) . . . . ? C33 N5 C34 C36 -91.1(3) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.415 _refine_diff_density_min -1.553 _refine_diff_density_rms 0.133 #===end data_2 _database_code_depnum_ccdc_archive 'CCDC 832560' #TrackingRef 'CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H45 Dy N4.5 O9' _chemical_formula_weight 811.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Dy Dy -0.1892 4.4098 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 24.306(5) _cell_length_b 14.939(3) _cell_length_c 19.812(4) _cell_angle_alpha 90.00 _cell_angle_beta 100.50(3) _cell_angle_gamma 90.00 _cell_volume 7073(2) _cell_formula_units_Z 8 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 9637 _cell_measurement_theta_min 1.6076 _cell_measurement_theta_max 27.8944 _exptl_crystal_description sheet _exptl_crystal_colour purpleblue _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 1.34 _exptl_crystal_density_diffrn 1.524 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3300 _exptl_absorpt_coefficient_mu 2.171 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.6707 _exptl_absorpt_correction_T_max 0.8808 _exptl_absorpt_process_details CrystalClear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn CCD area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 23536 _diffrn_reflns_av_R_equivalents 0.0464 _diffrn_reflns_av_sigmaI/netI 0.0416 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 25.01 _reflns_number_total 6228 _reflns_number_gt 4937 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'CrystalStructure 3.8' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0439P)^2^+4.4898P] 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 SHELXL _refine_ls_extinction_coef 0.00098(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6228 _refine_ls_number_parameters 443 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0475 _refine_ls_R_factor_gt 0.0353 _refine_ls_wR_factor_ref 0.0897 _refine_ls_wR_factor_gt 0.0835 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 0.170488(7) -0.001909(11) 0.100682(9) 0.02365(10) Uani 1 1 d . . . O1 O 0.13385(11) -0.14609(17) 0.09542(14) 0.0322(6) Uani 1 1 d . . . O2 O 0.09120(12) -0.00085(15) 0.01616(15) 0.0333(7) Uani 1 1 d . . . O3 O 0.25390(10) -0.07430(16) 0.13988(14) 0.0305(6) Uani 1 1 d . . . O4 O 0.20420(11) -0.04986(17) 0.00425(14) 0.0321(7) Uani 1 1 d . . . O5 O 0.16569(11) -0.03638(17) 0.21470(13) 0.0300(6) Uani 1 1 d . . . O6 O 0.11228(10) 0.10502(16) 0.13813(14) 0.0288(6) Uani 1 1 d . . . O7 O 0.18830(11) 0.12694(16) 0.03332(13) 0.0301(6) Uani 1 1 d . . . O8 O 0.16822(12) 0.38856(18) 0.15115(16) 0.0423(8) Uani 1 1 d . . . O9 O 0.48447(16) 0.1213(2) 0.13093(17) 0.0640(10) Uani 1 1 d . . . N1 N 0.23424(12) 0.12364(19) 0.17349(16) 0.0252(7) Uani 1 1 d . . . N2 N 0.17463(13) 0.2075(2) 0.04766(17) 0.0283(8) Uani 1 1 d . . . N3 N 0.16567(12) 0.3311(2) 0.10237(16) 0.0284(8) Uani 1 1 d . . . N4 N 0.53333(16) 0.2865(3) 0.2115(2) 0.0499(10) Uani 1 1 d . . . N5 N 0.49303(16) 0.0955(2) 0.19455(19) 0.0415(9) Uani 1 1 d . . . C1 C 0.0979(2) -0.2895(3) 0.0599(3) 0.0516(13) Uani 1 1 d . . . H1A H 0.1348 -0.3138 0.0745 0.077 Uiso 1 1 calc R . . H1B H 0.0805 -0.3177 0.0180 0.077 Uiso 1 1 calc R . . H1C H 0.0759 -0.3002 0.0947 0.077 Uiso 1 1 calc R . . C2 C 0.10215(17) -0.1894(3) 0.0484(2) 0.0337(10) Uani 1 1 d . . . C3 C 0.07106(18) -0.1520(3) -0.0107(2) 0.0401(11) Uani 1 1 d . . . H3 H 0.0525 -0.1905 -0.0442 0.048 Uiso 1 1 calc R . . C4 C 0.06599(16) -0.0603(3) -0.0228(2) 0.0336(10) Uani 1 1 d . . . C5 C 0.02619(18) -0.0283(3) -0.0854(2) 0.0409(11) Uani 1 1 d . . . H5A H 0.0249 0.0359 -0.0854 0.061 Uiso 1 1 calc R . . H5B H -0.0105 -0.0517 -0.0848 0.061 Uiso 1 1 calc R . . H5C H 0.0388 -0.0487 -0.1259 0.061 Uiso 1 1 calc R . . C6 C 0.32998(16) -0.1744(3) 0.1643(2) 0.0355(10) Uani 1 1 d . . . H6A H 0.3465 -0.1329 0.1992 0.053 Uiso 1 1 calc R . . H6B H 0.3582 -0.1967 0.1406 0.053 Uiso 1 1 calc R . . H6C H 0.3137 -0.2234 0.1851 0.053 Uiso 1 1 calc R . . C7 C 0.28496(16) -0.1273(2) 0.1139(2) 0.0271(9) Uani 1 1 d . . . C8 C 0.28002(17) -0.1452(3) 0.0443(2) 0.0334(10) Uani 1 1 d . . . H8 H 0.3045 -0.1865 0.0308 0.040 Uiso 1 1 calc R . . C9 C 0.24044(18) -0.1051(2) -0.0066(2) 0.0325(10) Uani 1 1 d . . . C10 C 0.2417(2) -0.1267(3) -0.0811(2) 0.0485(12) Uani 1 1 d . . . H10A H 0.2042 -0.1355 -0.1055 0.073 Uiso 1 1 calc R . . H10B H 0.2631 -0.1803 -0.0835 0.073 Uiso 1 1 calc R . . H10C H 0.2587 -0.0780 -0.1014 0.073 Uiso 1 1 calc R . . C11 C 0.15774(19) -0.0467(3) 0.3316(2) 0.0400(11) Uani 1 1 d . . . H11A H 0.1406 -0.1048 0.3259 0.060 Uiso 1 1 calc R . . H11B H 0.1416 -0.0130 0.3644 0.060 Uiso 1 1 calc R . . H11C H 0.1972 -0.0532 0.3478 0.060 Uiso 1 1 calc R . . C12 C 0.14783(17) 0.0019(2) 0.2635(2) 0.0278(9) Uani 1 1 d . . . C13 C 0.11855(16) 0.0833(2) 0.2576(2) 0.0309(9) Uani 1 1 d . . . H13 H 0.1099 0.1085 0.2973 0.037 Uiso 1 1 calc R . . C14 C 0.10184(15) 0.1285(2) 0.1963(2) 0.0274(9) Uani 1 1 d . . . C15 C 0.06825(16) 0.2130(2) 0.1973(2) 0.0359(10) Uani 1 1 d . . . H15A H 0.0903 0.2635 0.1882 0.054 Uiso 1 1 calc R . . H15B H 0.0581 0.2200 0.2417 0.054 Uiso 1 1 calc R . . H15C H 0.0350 0.2096 0.1628 0.054 Uiso 1 1 calc R . . C16 C 0.27243(16) 0.0939(3) 0.2254(2) 0.0292(9) Uani 1 1 d . . . H16 H 0.2773 0.0323 0.2299 0.035 Uiso 1 1 calc R . . C17 C 0.30525(16) 0.1473(3) 0.2729(2) 0.0334(10) Uani 1 1 d . . . H17 H 0.3318 0.1223 0.3075 0.040 Uiso 1 1 calc R . . C18 C 0.29813(16) 0.2389(3) 0.2683(2) 0.0332(10) Uani 1 1 d . . . H18 H 0.3196 0.2771 0.2997 0.040 Uiso 1 1 calc R . . C19 C 0.25798(15) 0.2722(3) 0.2153(2) 0.0304(9) Uani 1 1 d . . . H19 H 0.2515 0.3335 0.2114 0.037 Uiso 1 1 calc R . . C20 C 0.22760(15) 0.2137(2) 0.1683(2) 0.0257(9) Uani 1 1 d . . . C21 C 0.18895(16) 0.2480(2) 0.10857(19) 0.0242(8) Uani 1 1 d . . . C22 C 0.13683(19) 0.3526(3) 0.0311(2) 0.0394(11) Uani 1 1 d . . . C23 C 0.13794(17) 0.2625(3) -0.0057(2) 0.0339(10) Uani 1 1 d . . . C24 C 0.1723(3) 0.4255(3) 0.0056(3) 0.107(3) Uani 1 1 d . . . H24A H 0.1755 0.4758 0.0362 0.161 Uiso 1 1 calc R . . H24B H 0.1549 0.4440 -0.0396 0.161 Uiso 1 1 calc R . . H24C H 0.2090 0.4023 0.0043 0.161 Uiso 1 1 calc R . . C25 C 0.0802(2) 0.3901(5) 0.0336(3) 0.114(3) Uani 1 1 d . . . H25A H 0.0583 0.3460 0.0520 0.171 Uiso 1 1 calc R . . H25B H 0.0619 0.4060 -0.0119 0.171 Uiso 1 1 calc R . . H25C H 0.0841 0.4423 0.0623 0.171 Uiso 1 1 calc R . . C26 C 0.0820(2) 0.2149(3) -0.0217(4) 0.104(3) Uani 1 1 d . . . H26A H 0.0873 0.1558 -0.0383 0.156 Uiso 1 1 calc R . . H26B H 0.0571 0.2478 -0.0561 0.156 Uiso 1 1 calc R . . H26C H 0.0662 0.2111 0.0192 0.156 Uiso 1 1 calc R . . C27 C 0.1657(3) 0.2663(3) -0.0685(2) 0.0720(18) Uani 1 1 d . . . H27A H 0.2012 0.2959 -0.0568 0.108 Uiso 1 1 calc R . . H27B H 0.1422 0.2987 -0.1044 0.108 Uiso 1 1 calc R . . H27C H 0.1712 0.2065 -0.0838 0.108 Uiso 1 1 calc R . . C28 C 0.53238(19) 0.3780(3) 0.2123(2) 0.0468(12) Uani 1 1 d . . . H28 H 0.5543 0.4094 0.1865 0.056 Uiso 1 1 calc R . . C29 C 0.5000 0.4248(4) 0.2500 0.0472(17) Uani 1 2 d S . . H29 H 0.5000 0.4870 0.2500 0.057 Uiso 1 2 calc SR . . C32 C 0.5000 0.2462(3) 0.2500 0.0281(13) Uani 1 2 d S . . C33 C 0.5000 0.1480(4) 0.2500 0.0341(14) Uani 1 2 d S . . C34 C 0.5032(2) -0.0004(2) 0.2113(3) 0.0384(12) Uani 1 1 d . . . C36 C 0.5689(2) -0.0140(3) 0.2124(3) 0.0485(13) Uani 1 1 d . . . H36A H 0.5784 -0.0760 0.2201 0.073 Uiso 1 1 calc R . . H36B H 0.5899 0.0215 0.2485 0.073 Uiso 1 1 calc R . . H36C H 0.5776 0.0045 0.1691 0.073 Uiso 1 1 calc R . . C37 C 0.47027(18) -0.0614(3) 0.1624(2) 0.0449(12) Uani 1 1 d . . . H37A H 0.4314 -0.0458 0.1569 0.067 Uiso 1 1 calc R . . H37B H 0.4756 -0.1216 0.1791 0.067 Uiso 1 1 calc R . . H37C H 0.4822 -0.0568 0.1189 0.067 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.02618(14) 0.02529(14) 0.01781(13) 0.00087(8) -0.00043(8) -0.00018(7) O1 0.0367(16) 0.0353(15) 0.0219(16) 0.0034(13) -0.0020(13) -0.0060(13) O2 0.0315(16) 0.0380(17) 0.0265(17) -0.0005(13) -0.0053(13) -0.0029(12) O3 0.0315(15) 0.0320(15) 0.0267(17) -0.0023(12) 0.0022(13) 0.0041(12) O4 0.0404(17) 0.0297(15) 0.0261(17) 0.0024(13) 0.0059(13) 0.0049(13) O5 0.0385(16) 0.0282(14) 0.0233(16) 0.0017(13) 0.0055(13) 0.0005(13) O6 0.0281(15) 0.0310(14) 0.0260(16) 0.0016(12) 0.0013(13) 0.0000(11) O7 0.0398(16) 0.0253(14) 0.0255(16) -0.0003(12) 0.0068(13) 0.0054(12) O8 0.0527(19) 0.0352(16) 0.0374(19) -0.0082(15) 0.0042(15) 0.0076(14) O9 0.105(3) 0.052(2) 0.032(2) 0.0063(17) 0.002(2) -0.0010(19) N1 0.0274(17) 0.0276(17) 0.0202(18) -0.0020(14) 0.0031(15) -0.0010(14) N2 0.0311(19) 0.0286(18) 0.025(2) 0.0049(15) 0.0055(15) 0.0025(14) N3 0.0316(19) 0.0272(18) 0.026(2) -0.0009(15) 0.0052(16) -0.0020(14) N4 0.048(2) 0.059(3) 0.042(3) 0.004(2) 0.004(2) -0.005(2) N5 0.065(3) 0.032(2) 0.025(2) 0.0010(17) 0.0010(19) -0.0022(18) C1 0.056(3) 0.039(3) 0.056(4) 0.006(2) -0.002(3) -0.011(2) C2 0.038(2) 0.033(2) 0.030(3) -0.001(2) 0.005(2) -0.0110(19) C3 0.048(3) 0.038(3) 0.028(3) -0.001(2) -0.007(2) -0.007(2) C4 0.027(2) 0.048(3) 0.025(2) -0.004(2) 0.0003(18) -0.0072(19) C5 0.037(3) 0.050(3) 0.030(3) 0.004(2) -0.008(2) -0.007(2) C6 0.035(2) 0.038(2) 0.033(3) -0.003(2) 0.005(2) 0.0036(18) C7 0.029(2) 0.0218(19) 0.030(2) 0.0016(17) 0.0031(18) -0.0038(16) C8 0.042(2) 0.030(2) 0.027(2) -0.0040(19) 0.004(2) 0.0095(19) C9 0.046(3) 0.025(2) 0.027(2) -0.0001(18) 0.007(2) -0.0043(19) C10 0.065(3) 0.051(3) 0.030(3) -0.004(2) 0.008(2) 0.013(2) C11 0.060(3) 0.038(3) 0.022(2) 0.004(2) 0.006(2) 0.001(2) C12 0.031(2) 0.030(2) 0.023(2) 0.0002(17) 0.0041(18) -0.0070(16) C13 0.036(2) 0.028(2) 0.030(3) -0.0043(18) 0.008(2) -0.0035(17) C14 0.0186(19) 0.029(2) 0.033(3) -0.0031(18) 0.0015(18) -0.0083(16) C15 0.032(2) 0.033(2) 0.041(3) -0.001(2) 0.002(2) 0.0030(18) C16 0.030(2) 0.029(2) 0.028(2) -0.0010(18) 0.0035(19) 0.0032(17) C17 0.027(2) 0.045(3) 0.025(2) -0.003(2) -0.0005(18) 0.0048(19) C18 0.031(2) 0.038(2) 0.030(3) -0.0115(19) 0.0046(19) -0.0040(19) C19 0.030(2) 0.031(2) 0.031(2) -0.0022(19) 0.0084(19) 0.0010(18) C20 0.024(2) 0.029(2) 0.026(2) -0.0037(17) 0.0093(18) -0.0026(16) C21 0.028(2) 0.0230(19) 0.022(2) -0.0004(17) 0.0074(17) -0.0034(16) C22 0.057(3) 0.036(2) 0.027(3) 0.006(2) 0.012(2) 0.013(2) C23 0.039(2) 0.030(2) 0.028(3) 0.0069(19) -0.0039(19) -0.0018(18) C24 0.240(9) 0.039(3) 0.051(4) 0.000(3) 0.048(5) -0.046(4) C25 0.096(5) 0.195(8) 0.039(4) -0.031(4) -0.023(3) 0.102(5) C26 0.063(4) 0.049(3) 0.166(8) 0.050(4) -0.068(4) -0.018(3) C27 0.145(6) 0.051(3) 0.022(3) 0.008(2) 0.020(3) 0.036(3) C28 0.043(3) 0.052(3) 0.043(3) 0.008(2) -0.001(2) -0.019(2) C29 0.065(5) 0.026(3) 0.041(4) 0.000 -0.015(4) 0.000 C32 0.033(3) 0.027(3) 0.023(3) 0.000 -0.001(3) 0.000 C33 0.050(4) 0.029(3) 0.023(3) 0.000 0.006(3) 0.000 C34 0.064(3) 0.017(2) 0.042(3) -0.0008(18) 0.028(3) 0.0011(18) C36 0.041(3) 0.046(3) 0.061(4) -0.007(2) 0.015(3) -0.001(2) C37 0.045(3) 0.041(3) 0.046(3) -0.011(2) 0.003(2) -0.013(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 2.304(3) . ? Dy1 O2 2.311(3) . ? Dy1 O4 2.325(3) . ? Dy1 O1 2.326(3) . ? Dy1 O5 2.340(3) . ? Dy1 O6 2.342(2) . ? Dy1 O7 2.426(2) . ? Dy1 N1 2.680(3) . ? O1 C2 1.273(5) . ? O2 C4 1.261(5) . ? O3 C7 1.266(4) . ? O4 C9 1.254(4) . ? O5 C12 1.266(4) . ? O6 C14 1.274(4) . ? O7 N2 1.293(4) . ? O8 N3 1.286(4) . ? O9 N5 1.298(4) . ? N1 C16 1.330(5) . ? N1 C20 1.357(4) . ? N2 C21 1.338(5) . ? N2 C23 1.498(5) . ? N3 C21 1.360(5) . ? N3 C22 1.492(5) . ? N4 C32 1.352(4) . ? N4 C28 1.367(5) . ? N5 C33 1.336(4) . ? N5 C34 1.480(5) . ? C1 C2 1.519(5) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.390(6) . ? C3 C4 1.392(6) . ? C3 H3 0.9300 . ? C4 C5 1.505(6) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 C7 1.513(5) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 C8 1.388(5) . ? C8 C9 1.397(6) . ? C8 H8 0.9300 . ? C9 C10 1.516(5) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C12 1.512(5) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C13 1.404(5) . ? C13 C14 1.384(5) . ? C13 H13 0.9300 . ? C14 C15 1.506(5) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 C17 1.373(5) . ? C16 H16 0.9300 . ? C17 C18 1.380(5) . ? C17 H17 0.9300 . ? C18 C19 1.389(6) . ? C18 H18 0.9300 . ? C19 C20 1.389(5) . ? C19 H19 0.9300 . ? C20 C21 1.463(5) . ? C22 C25 1.495(6) . ? C22 C24 1.531(6) . ? C22 C23 1.534(6) . ? C23 C26 1.515(6) . ? C23 C27 1.520(6) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 C29 1.371(5) . ? C28 H28 0.9300 . ? C29 C28 1.371(5) 2_655 ? C29 H29 0.9300 . ? C32 N4 1.352(4) 2_655 ? C32 C33 1.467(7) . ? C33 N5 1.336(4) 2_655 ? C34 C37 1.458(6) . ? C34 C34 1.568(9) 2_655 ? C34 C36 1.606(7) . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Dy1 O2 144.45(9) . . ? O3 Dy1 O4 73.27(9) . . ? O2 Dy1 O4 77.23(10) . . ? O3 Dy1 O1 83.49(9) . . ? O2 Dy1 O1 73.26(9) . . ? O4 Dy1 O1 82.37(9) . . ? O3 Dy1 O5 76.53(9) . . ? O2 Dy1 O5 121.28(10) . . ? O4 Dy1 O5 144.33(9) . . ? O1 Dy1 O5 75.73(9) . . ? O3 Dy1 O6 139.33(9) . . ? O2 Dy1 O6 75.69(9) . . ? O4 Dy1 O6 142.57(9) . . ? O1 Dy1 O6 113.41(8) . . ? O5 Dy1 O6 72.85(9) . . ? O3 Dy1 O7 108.87(9) . . ? O2 Dy1 O7 78.74(9) . . ? O4 Dy1 O7 70.57(8) . . ? O1 Dy1 O7 144.63(9) . . ? O5 Dy1 O7 138.67(9) . . ? O6 Dy1 O7 79.15(8) . . ? O3 Dy1 N1 76.12(9) . . ? O2 Dy1 N1 135.16(9) . . ? O4 Dy1 N1 113.71(9) . . ? O1 Dy1 N1 148.34(10) . . ? O5 Dy1 N1 76.12(9) . . ? O6 Dy1 N1 71.08(9) . . ? O7 Dy1 N1 66.25(9) . . ? C2 O1 Dy1 132.8(3) . . ? C4 O2 Dy1 133.4(3) . . ? C7 O3 Dy1 135.2(3) . . ? C9 O4 Dy1 135.1(3) . . ? C12 O5 Dy1 136.2(2) . . ? C14 O6 Dy1 134.9(3) . . ? N2 O7 Dy1 122.57(19) . . ? C16 N1 C20 116.5(3) . . ? C16 N1 Dy1 115.8(2) . . ? C20 N1 Dy1 127.1(3) . . ? O7 N2 C21 125.7(3) . . ? O7 N2 C23 119.9(3) . . ? C21 N2 C23 114.3(3) . . ? O8 N3 C21 125.4(3) . . ? O8 N3 C22 121.1(3) . . ? C21 N3 C22 113.5(3) . . ? C32 N4 C28 115.2(4) . . ? O9 N5 C33 126.7(4) . . ? O9 N5 C34 119.7(3) . . ? C33 N5 C34 113.1(4) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C3 125.2(4) . . ? O1 C2 C1 116.0(4) . . ? C3 C2 C1 118.8(4) . . ? C2 C3 C4 123.9(4) . . ? C2 C3 H3 118.0 . . ? C4 C3 H3 118.0 . . ? O2 C4 C3 124.8(4) . . ? O2 C4 C5 116.6(4) . . ? C3 C4 C5 118.6(4) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 H6A 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C7 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O3 C7 C8 125.0(4) . . ? O3 C7 C6 115.8(3) . . ? C8 C7 C6 119.2(3) . . ? C7 C8 C9 124.0(3) . . ? C7 C8 H8 118.0 . . ? C9 C8 H8 118.0 . . ? O4 C9 C8 124.8(4) . . ? O4 C9 C10 116.6(4) . . ? C8 C9 C10 118.6(4) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C12 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? O5 C12 C13 124.5(4) . . ? O5 C12 C11 116.4(3) . . ? C13 C12 C11 119.1(3) . . ? C14 C13 C12 124.0(4) . . ? C14 C13 H13 118.0 . . ? C12 C13 H13 118.0 . . ? O6 C14 C13 125.8(4) . . ? O6 C14 C15 116.2(4) . . ? C13 C14 C15 118.1(3) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N1 C16 C17 124.9(4) . . ? N1 C16 H16 117.6 . . ? C17 C16 H16 117.6 . . ? C16 C17 C18 118.7(4) . . ? C16 C17 H17 120.6 . . ? C18 C17 H17 120.6 . . ? C17 C18 C19 117.9(4) . . ? C17 C18 H18 121.0 . . ? C19 C18 H18 121.0 . . ? C18 C19 C20 119.7(4) . . ? C18 C19 H19 120.1 . . ? C20 C19 H19 120.1 . . ? N1 C20 C19 122.1(4) . . ? N1 C20 C21 117.3(3) . . ? C19 C20 C21 120.5(3) . . ? N2 C21 N3 107.2(3) . . ? N2 C21 C20 126.5(3) . . ? N3 C21 C20 126.0(3) . . ? N3 C22 C25 109.0(3) . . ? N3 C22 C24 105.6(4) . . ? C25 C22 C24 108.8(5) . . ? N3 C22 C23 102.4(3) . . ? C25 C22 C23 116.1(4) . . ? C24 C22 C23 114.0(4) . . ? N2 C23 C26 106.6(3) . . ? N2 C23 C27 107.6(3) . . ? C26 C23 C27 111.2(5) . . ? N2 C23 C22 101.9(3) . . ? C26 C23 C22 114.7(4) . . ? C27 C23 C22 113.9(3) . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C27 H27A 109.5 . . ? C23 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C23 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N4 C28 C29 121.9(4) . . ? N4 C28 H28 119.0 . . ? C29 C28 H28 119.0 . . ? C28 C29 C28 118.7(6) 2_655 . ? C28 C29 H29 120.6 2_655 . ? C28 C29 H29 120.6 . . ? N4 C32 N4 127.1(5) 2_655 . ? N4 C32 C33 116.4(3) 2_655 . ? N4 C32 C33 116.4(3) . . ? N5 C33 N5 108.0(5) . 2_655 ? N5 C33 C32 126.0(2) . . ? N5 C33 C32 126.0(2) 2_655 . ? C37 C34 N5 114.0(4) . . ? C37 C34 C34 120.7(4) . 2_655 ? N5 C34 C34 100.2(2) . 2_655 ? C37 C34 C36 110.7(3) . . ? N5 C34 C36 104.4(3) . . ? C34 C34 C36 105.2(6) 2_655 . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C34 C37 H37A 109.5 . . ? C34 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C34 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Dy1 O1 C2 -129.5(3) . . . . ? O2 Dy1 O1 C2 23.3(3) . . . . ? O4 Dy1 O1 C2 -55.6(3) . . . . ? O5 Dy1 O1 C2 152.8(3) . . . . ? O6 Dy1 O1 C2 89.0(3) . . . . ? O7 Dy1 O1 C2 -15.8(4) . . . . ? N1 Dy1 O1 C2 -179.3(3) . . . . ? O3 Dy1 O2 C4 24.7(4) . . . . ? O4 Dy1 O2 C4 59.1(3) . . . . ? O1 Dy1 O2 C4 -26.7(3) . . . . ? O5 Dy1 O2 C4 -87.7(4) . . . . ? O6 Dy1 O2 C4 -147.0(4) . . . . ? O7 Dy1 O2 C4 131.5(4) . . . . ? N1 Dy1 O2 C4 170.0(3) . . . . ? O2 Dy1 O3 C7 18.9(4) . . . . ? O4 Dy1 O3 C7 -16.3(3) . . . . ? O1 Dy1 O3 C7 67.7(3) . . . . ? O5 Dy1 O3 C7 144.5(3) . . . . ? O6 Dy1 O3 C7 -173.6(3) . . . . ? O7 Dy1 O3 C7 -78.2(3) . . . . ? N1 Dy1 O3 C7 -136.7(3) . . . . ? O3 Dy1 O4 C9 16.2(3) . . . . ? O2 Dy1 O4 C9 -143.8(4) . . . . ? O1 Dy1 O4 C9 -69.3(4) . . . . ? O5 Dy1 O4 C9 -17.1(4) . . . . ? O6 Dy1 O4 C9 171.7(3) . . . . ? O7 Dy1 O4 C9 133.8(4) . . . . ? N1 Dy1 O4 C9 82.2(4) . . . . ? O3 Dy1 O5 C12 141.4(4) . . . . ? O2 Dy1 O5 C12 -72.1(4) . . . . ? O4 Dy1 O5 C12 174.1(3) . . . . ? O1 Dy1 O5 C12 -132.0(4) . . . . ? O6 Dy1 O5 C12 -11.5(4) . . . . ? O7 Dy1 O5 C12 38.0(4) . . . . ? N1 Dy1 O5 C12 62.6(4) . . . . ? O3 Dy1 O6 C14 -29.2(4) . . . . ? O2 Dy1 O6 C14 143.4(3) . . . . ? O4 Dy1 O6 C14 -171.7(3) . . . . ? O1 Dy1 O6 C14 79.1(3) . . . . ? O5 Dy1 O6 C14 13.6(3) . . . . ? O7 Dy1 O6 C14 -135.6(3) . . . . ? N1 Dy1 O6 C14 -67.2(3) . . . . ? O3 Dy1 O7 N2 -123.0(3) . . . . ? O2 Dy1 O7 N2 93.1(3) . . . . ? O4 Dy1 O7 N2 173.3(3) . . . . ? O1 Dy1 O7 N2 131.1(2) . . . . ? O5 Dy1 O7 N2 -32.1(3) . . . . ? O6 Dy1 O7 N2 15.7(3) . . . . ? N1 Dy1 O7 N2 -58.3(3) . . . . ? O3 Dy1 N1 C16 -29.6(2) . . . . ? O2 Dy1 N1 C16 170.4(2) . . . . ? O4 Dy1 N1 C16 -93.9(2) . . . . ? O1 Dy1 N1 C16 21.9(3) . . . . ? O5 Dy1 N1 C16 49.7(2) . . . . ? O6 Dy1 N1 C16 126.0(3) . . . . ? O7 Dy1 N1 C16 -147.8(3) . . . . ? O3 Dy1 N1 C20 158.7(3) . . . . ? O2 Dy1 N1 C20 -1.4(3) . . . . ? O4 Dy1 N1 C20 94.3(3) . . . . ? O1 Dy1 N1 C20 -149.8(2) . . . . ? O5 Dy1 N1 C20 -122.0(3) . . . . ? O6 Dy1 N1 C20 -45.7(3) . . . . ? O7 Dy1 N1 C20 40.5(2) . . . . ? Dy1 O7 N2 C21 53.3(4) . . . . ? Dy1 O7 N2 C23 -124.3(3) . . . . ? Dy1 O1 C2 C3 -14.2(6) . . . . ? Dy1 O1 C2 C1 167.1(3) . . . . ? O1 C2 C3 C4 -7.0(7) . . . . ? C1 C2 C3 C4 171.6(4) . . . . ? Dy1 O2 C4 C3 20.5(6) . . . . ? Dy1 O2 C4 C5 -161.8(3) . . . . ? C2 C3 C4 O2 4.1(7) . . . . ? C2 C3 C4 C5 -173.6(4) . . . . ? Dy1 O3 C7 C8 12.5(6) . . . . ? Dy1 O3 C7 C6 -166.8(2) . . . . ? O3 C7 C8 C9 1.4(6) . . . . ? C6 C7 C8 C9 -179.3(4) . . . . ? Dy1 O4 C9 C8 -12.2(6) . . . . ? Dy1 O4 C9 C10 169.7(3) . . . . ? C7 C8 C9 O4 -1.5(6) . . . . ? C7 C8 C9 C10 176.6(4) . . . . ? Dy1 O5 C12 C13 6.0(6) . . . . ? Dy1 O5 C12 C11 -176.1(3) . . . . ? O5 C12 C13 C14 5.2(6) . . . . ? C11 C12 C13 C14 -172.7(4) . . . . ? Dy1 O6 C14 C13 -10.6(6) . . . . ? Dy1 O6 C14 C15 169.5(2) . . . . ? C12 C13 C14 O6 -2.9(6) . . . . ? C12 C13 C14 C15 177.1(3) . . . . ? C20 N1 C16 C17 -0.5(5) . . . . ? Dy1 N1 C16 C17 -173.1(3) . . . . ? N1 C16 C17 C18 1.3(6) . . . . ? C16 C17 C18 C19 -0.2(5) . . . . ? C17 C18 C19 C20 -1.6(5) . . . . ? C16 N1 C20 C19 -1.4(5) . . . . ? Dy1 N1 C20 C19 170.3(2) . . . . ? C16 N1 C20 C21 175.4(3) . . . . ? Dy1 N1 C20 C21 -12.9(4) . . . . ? C18 C19 C20 N1 2.5(5) . . . . ? C18 C19 C20 C21 -174.2(3) . . . . ? O7 N2 C21 N3 -179.2(3) . . . . ? C23 N2 C21 N3 -1.4(4) . . . . ? O7 N2 C21 C20 7.3(5) . . . . ? C23 N2 C21 C20 -174.9(3) . . . . ? O8 N3 C21 N2 176.9(3) . . . . ? C22 N3 C21 N2 -4.7(4) . . . . ? O8 N3 C21 C20 -9.5(5) . . . . ? C22 N3 C21 C20 168.9(3) . . . . ? N1 C20 C21 N2 -25.6(5) . . . . ? C19 C20 C21 N2 151.3(3) . . . . ? N1 C20 C21 N3 162.0(3) . . . . ? C19 C20 C21 N3 -21.1(5) . . . . ? O8 N3 C22 C25 -49.6(5) . . . . ? C21 N3 C22 C25 131.9(4) . . . . ? O8 N3 C22 C24 67.2(4) . . . . ? C21 N3 C22 C24 -111.3(4) . . . . ? O8 N3 C22 C23 -173.1(3) . . . . ? C21 N3 C22 C23 8.3(4) . . . . ? O7 N2 C23 C26 63.7(5) . . . . ? C21 N2 C23 C26 -114.3(4) . . . . ? O7 N2 C23 C27 -55.7(4) . . . . ? C21 N2 C23 C27 126.4(4) . . . . ? O7 N2 C23 C22 -175.7(3) . . . . ? C21 N2 C23 C22 6.3(4) . . . . ? N3 C22 C23 N2 -8.0(4) . . . . ? C25 C22 C23 N2 -126.7(4) . . . . ? C24 C22 C23 N2 105.6(5) . . . . ? N3 C22 C23 C26 106.8(4) . . . . ? C25 C22 C23 C26 -11.9(6) . . . . ? C24 C22 C23 C26 -139.7(5) . . . . ? N3 C22 C23 C27 -123.5(4) . . . . ? C25 C22 C23 C27 117.8(5) . . . . ? C24 C22 C23 C27 -9.9(6) . . . . ? C32 N4 C28 C29 0.3(6) . . . . ? N4 C28 C29 C28 -0.2(3) . . . 2_655 ? C28 N4 C32 N4 -0.2(3) . . . 2_655 ? C28 N4 C32 C33 179.8(3) . . . . ? O9 N5 C33 N5 179.2(5) . . . 2_655 ? C34 N5 C33 N5 -8.2(2) . . . 2_655 ? O9 N5 C33 C32 -0.8(5) . . . . ? C34 N5 C33 C32 171.8(2) . . . . ? N4 C32 C33 N5 130.0(3) 2_655 . . . ? N4 C32 C33 N5 -50.0(3) . . . . ? N4 C32 C33 N5 -50.0(3) 2_655 . . 2_655 ? N4 C32 C33 N5 130.0(3) . . . 2_655 ? O9 N5 C34 C37 -37.1(6) . . . . ? C33 N5 C34 C37 149.8(3) . . . . ? O9 N5 C34 C34 -167.5(5) . . . 2_655 ? C33 N5 C34 C34 19.4(6) . . . 2_655 ? O9 N5 C34 C36 83.8(5) . . . . ? C33 N5 C34 C36 -89.3(4) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.699 _refine_diff_density_min -0.802 _refine_diff_density_rms 0.102 #===end data_3 _database_code_depnum_ccdc_archive 'CCDC 832561' #TrackingRef 'CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30.5 H36 Dy F9 N3 O8' _chemical_formula_weight 906.1132 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' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 30.036(6) _cell_length_b 12.799(3) _cell_length_c 19.800(4) _cell_angle_alpha 90.00 _cell_angle_beta 102.40(3) _cell_angle_gamma 90.00 _cell_volume 7434(3) _cell_formula_units_Z 8 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 10638 _cell_measurement_theta_min 1.7360 _cell_measurement_theta_max 27.8824 _exptl_crystal_description bar-type _exptl_crystal_colour purple _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.617 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3598 _exptl_absorpt_coefficient_mu 2.104 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.6321 _exptl_absorpt_correction_T_max 0.7032 _exptl_absorpt_process_details CrystalClear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn CCD area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 24503 _diffrn_reflns_av_R_equivalents 0.0395 _diffrn_reflns_av_sigmaI/netI 0.0363 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 25.02 _reflns_number_total 6558 _reflns_number_gt 5631 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'CrystalStructure 3.8' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0535P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment CONSTR _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6558 _refine_ls_number_parameters 559 _refine_ls_number_restraints 117 _refine_ls_R_factor_all 0.0415 _refine_ls_R_factor_gt 0.0338 _refine_ls_wR_factor_ref 0.0873 _refine_ls_wR_factor_gt 0.0823 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.109 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 0.344553(5) 0.771326(13) 0.387146(8) 0.02464(8) Uani 1 1 d . . . F1 F 0.47876(9) 0.7297(3) 0.5729(2) 0.0830(11) Uani 1 1 d . . . F2 F 0.42767(9) 0.6609(2) 0.61800(14) 0.0637(8) Uani 1 1 d . . . F3 F 0.45645(11) 0.8077(3) 0.65566(16) 0.0831(11) Uani 1 1 d . . . F4 F 0.31104(11) 0.4576(2) 0.51890(16) 0.0735(9) Uani 1 1 d . . . F5 F 0.24029(10) 0.4430(2) 0.4758(2) 0.0746(9) Uani 1 1 d . . . F6 F 0.28913(11) 0.4084(2) 0.41451(17) 0.0726(9) Uani 1 1 d . . . F7 F 0.47577(15) 1.0403(4) 0.4263(3) 0.0782(18) Uani 0.609(4) 1 d PDU A 1 F8 F 0.49394(15) 1.0038(4) 0.3307(3) 0.086(2) Uani 0.609(4) 1 d PDU A 1 F9 F 0.50207(13) 0.8902(4) 0.4107(3) 0.086(2) Uani 0.609(4) 1 d PDU A 1 F7' F 0.3626(5) 1.0767(16) 0.1905(10) 0.096(8) Uani 0.216(12) 1 d PDU A 2 F8' F 0.2977(6) 1.0585(17) 0.2211(10) 0.098(8) Uani 0.216(12) 1 d PDU A 2 F9' F 0.3225(8) 0.9370(11) 0.1620(8) 0.102(9) Uani 0.216(12) 1 d PDU A 2 F7" F 0.3386(10) 1.1115(9) 0.2230(12) 0.126(17) Uani 0.175(12) 1 d PD A 3 F9" F 0.3513(8) 0.982(2) 0.1588(8) 0.090(11) Uani 0.175(12) 1 d PD A 3 F8" F 0.2891(4) 0.987(2) 0.1977(11) 0.095(10) Uani 0.175(12) 1 d PD A 3 O1 O 0.34174(8) 0.9288(2) 0.44848(14) 0.0348(6) Uani 1 1 d . . . O2 O 0.38644(9) 0.7426(2) 0.49740(14) 0.0327(6) Uani 1 1 d . . . O3 O 0.26783(8) 0.7979(2) 0.38728(14) 0.0313(6) Uani 1 1 d . . . O4 O 0.31792(8) 0.6141(2) 0.42430(13) 0.0301(6) Uani 1 1 d . . . O5 O 0.33344(9) 0.8850(2) 0.29578(14) 0.0371(7) Uani 1 1 d . . . O6 O 0.41509(8) 0.8526(2) 0.38885(15) 0.0361(7) Uani 1 1 d . . . O7 O 0.39439(8) 0.6513(2) 0.35421(13) 0.0300(6) Uani 1 1 d . . . O8 O 0.32638(9) 0.3317(2) 0.28779(15) 0.0421(7) Uani 1 1 d . . . N1 N 0.38656(9) 0.5520(2) 0.34581(16) 0.0271(7) Uani 1 1 d . . . N2 N 0.35513(10) 0.4013(2) 0.31356(16) 0.0316(7) Uani 1 1 d . . . N3 N 0.30362(10) 0.6629(2) 0.27852(16) 0.0298(7) Uani 1 1 d . . . C1 C 0.36456(15) 1.0853(3) 0.5103(2) 0.0469(11) Uani 1 1 d . . . H1A H 0.3463 1.1169 0.4683 0.070 Uiso 1 1 calc R . . H1B H 0.3952 1.1157 0.5199 0.070 Uiso 1 1 calc R . . H1C H 0.3501 1.0988 0.5493 0.070 Uiso 1 1 calc R . . C2 C 0.36777(12) 0.9689(3) 0.5000(2) 0.0317(9) Uani 1 1 d . . . C3 C 0.40006(12) 0.9116(3) 0.5491(2) 0.0355(10) Uani 1 1 d . . . H3 H 0.4181 0.9480 0.5872 0.043 Uiso 1 1 calc R . . C4 C 0.40621(12) 0.8063(3) 0.5438(2) 0.0326(9) Uani 1 1 d . . . C5 C 0.44208(16) 0.7516(4) 0.5986(3) 0.0478(12) Uani 1 1 d . . . C6 C 0.19052(13) 0.8000(4) 0.3969(2) 0.0431(11) Uani 1 1 d . . . H6A H 0.1947 0.8760 0.3995 0.065 Uiso 1 1 calc R . . H6B H 0.1756 0.7769 0.4338 0.065 Uiso 1 1 calc R . . H6C H 0.1715 0.7813 0.3519 0.065 Uiso 1 1 calc R . . C7 C 0.23643(13) 0.7474(3) 0.4055(2) 0.0296(9) Uani 1 1 d . . . C8 C 0.24081(12) 0.6448(3) 0.4319(2) 0.0347(9) Uani 1 1 d . . . H8A H 0.2156 0.6145 0.4466 0.042 Uiso 1 1 calc R . . C9 C 0.27988(13) 0.5867(3) 0.43738(19) 0.0305(9) Uani 1 1 d . . . C10 C 0.27944(15) 0.4732(4) 0.4614(2) 0.0452(11) Uani 1 1 d . . . C11 C 0.47665(18) 0.9629(4) 0.3828(3) 0.0694(16) Uani 1 1 d D . . H11A H 0.4908 0.9210 0.4218 0.104 Uiso 0.609(4) 1 d PR A 2 H11B H 0.4934 0.9558 0.3469 0.104 Uiso 0.609(4) 1 d PR A 2 H11C H 0.4767 1.0348 0.3966 0.104 Uiso 0.609(4) 1 d PR A 2 C12 C 0.42738(14) 0.9265(4) 0.3559(3) 0.0439(11) Uani 1 1 d . A . C13 C 0.40148(16) 0.9779(4) 0.2994(3) 0.0537(13) Uani 1 1 d . . . H13 H 0.4153 1.0322 0.2784 0.064 Uiso 1 1 calc R A . C14 C 0.35659(16) 0.9540(3) 0.2724(2) 0.0456(11) Uani 1 1 d . A . C15 C 0.3322(2) 1.0114(5) 0.2082(3) 0.0657(16) Uani 1 1 d D . . C16 C 0.34930(12) 0.5061(3) 0.30895(19) 0.0272(8) Uani 1 1 d . . . C17 C 0.40346(12) 0.3726(3) 0.3471(2) 0.0347(9) Uani 1 1 d . . . C18 C 0.42036(12) 0.4755(3) 0.3856(2) 0.0340(9) Uani 1 1 d . . . C19 C 0.40292(15) 0.2777(3) 0.3935(3) 0.0474(12) Uani 1 1 d . . . H19A H 0.3833 0.2920 0.4261 0.071 Uiso 1 1 calc R . . H19B H 0.4340 0.2631 0.4192 0.071 Uiso 1 1 calc R . . H19C H 0.3911 0.2171 0.3650 0.071 Uiso 1 1 calc R . . C20 C 0.42606(14) 0.3456(4) 0.2874(2) 0.0515(12) Uani 1 1 d . . . H20A H 0.4101 0.2865 0.2615 0.077 Uiso 1 1 calc R . . H20B H 0.4580 0.3269 0.3057 0.077 Uiso 1 1 calc R . . H20C H 0.4246 0.4062 0.2567 0.077 Uiso 1 1 calc R . . C21 C 0.41509(15) 0.4804(4) 0.4607(2) 0.0471(12) Uani 1 1 d . . . H21A H 0.4201 0.5522 0.4778 0.071 Uiso 1 1 calc R . . H21B H 0.4375 0.4340 0.4892 0.071 Uiso 1 1 calc R . . H21C H 0.3843 0.4580 0.4632 0.071 Uiso 1 1 calc R . . C22 C 0.46829(12) 0.5101(4) 0.3803(3) 0.0519(13) Uani 1 1 d . . . H22A H 0.4701 0.5138 0.3316 0.078 Uiso 1 1 calc R . . H22B H 0.4907 0.4596 0.4044 0.078 Uiso 1 1 calc R . . H22C H 0.4747 0.5791 0.4017 0.078 Uiso 1 1 calc R . . C23 C 0.30996(11) 0.5603(3) 0.26548(19) 0.0269(8) Uani 1 1 d . . . C24 C 0.28192(12) 0.5069(3) 0.2117(2) 0.0334(9) Uani 1 1 d . . . H24 H 0.2864 0.4344 0.2053 0.040 Uiso 1 1 calc R . . C25 C 0.24732(13) 0.5599(3) 0.1674(2) 0.0385(10) Uani 1 1 d . . . H25 H 0.2283 0.5251 0.1296 0.046 Uiso 1 1 calc R . . C26 C 0.24127(13) 0.6635(3) 0.1794(2) 0.0403(11) Uani 1 1 d . . . H26 H 0.2179 0.7020 0.1498 0.048 Uiso 1 1 calc R . . C27 C 0.26944(13) 0.7118(3) 0.2353(2) 0.0347(10) Uani 1 1 d . . . H27 H 0.2643 0.7836 0.2434 0.042 Uiso 1 1 calc R . . C28 C 0.3755(4) 0.3225(15) 0.6323(8) 0.074(5) Uani 0.50 1 d PDU . . H28A H 0.3459 0.2905 0.6247 0.111 Uiso 0.50 1 d PR . . H28B H 0.3734 0.3938 0.6464 0.111 Uiso 0.50 1 d PR . . H28C H 0.3865 0.3207 0.5902 0.111 Uiso 0.50 1 d PR . . C29 C 0.4082(3) 0.2613(9) 0.6887(6) 0.062(3) Uani 0.50 1 d PDU . . H29A H 0.4101 0.1898 0.6749 0.075 Uiso 0.50 1 d PR . . H29B H 0.3971 0.2623 0.7307 0.075 Uiso 0.50 1 d PR . . C30 C 0.4558(3) 0.3109(11) 0.7021(6) 0.049(3) Uani 0.50 1 d PDU . . H30A H 0.4533 0.3839 0.7117 0.059 Uiso 0.50 1 d PR . . H30B H 0.4679 0.3046 0.6611 0.059 Uiso 0.50 1 d PR . . C31 C 0.4883(2) 0.2592(7) 0.7631(5) 0.057(3) Uani 0.50 1 d PDU . . H31A H 0.4906 0.1859 0.7541 0.069 Uiso 0.50 1 d PR . . H31B H 0.4768 0.2669 0.8045 0.069 Uiso 0.50 1 d PR . . C32 C 0.5362(3) 0.3079(13) 0.7730(6) 0.059(4) Uani 0.50 1 d PDU . . H32A H 0.5337 0.3815 0.7807 0.071 Uiso 0.50 1 d PR . . H32B H 0.5479 0.2987 0.7319 0.071 Uiso 0.50 1 d PR . . C33 C 0.5688(3) 0.2628(9) 0.8369(6) 0.067(3) Uani 0.50 1 d PDU . . H33A H 0.5718 0.1894 0.8289 0.080 Uiso 0.50 1 d PR . . H33B H 0.5568 0.2708 0.8779 0.080 Uiso 0.50 1 d PR . . C34 C 0.6165(4) 0.3113(18) 0.8453(9) 0.087(5) Uani 0.50 1 d PDU . . H34A H 0.6368 0.2799 0.8841 0.131 Uiso 0.50 1 d PR . . H34B H 0.6286 0.3024 0.8046 0.131 Uiso 0.50 1 d PR . . H34C H 0.6134 0.3844 0.8540 0.131 Uiso 0.50 1 d PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.02000(11) 0.02315(13) 0.02874(12) 0.00232(7) 0.00073(8) -0.00292(6) F1 0.0326(16) 0.116(3) 0.096(3) 0.039(2) 0.0054(17) 0.0222(15) F2 0.0669(18) 0.0588(19) 0.0543(17) 0.0245(14) -0.0119(14) -0.0063(14) F3 0.093(2) 0.072(2) 0.0588(19) 0.0003(17) -0.0403(18) -0.0001(18) F4 0.088(2) 0.0529(19) 0.071(2) 0.0286(16) 0.0004(18) -0.0008(16) F5 0.0636(17) 0.0503(18) 0.123(3) 0.0213(18) 0.0479(18) -0.0140(14) F6 0.110(2) 0.0348(17) 0.087(2) -0.0107(16) 0.0502(19) -0.0156(16) F7 0.057(3) 0.086(4) 0.083(4) -0.032(3) -0.003(3) -0.029(3) F8 0.054(3) 0.124(5) 0.085(4) 0.004(3) 0.025(3) -0.055(3) F9 0.025(2) 0.070(4) 0.153(5) 0.023(4) -0.002(3) -0.008(2) F7' 0.125(13) 0.091(15) 0.077(13) 0.054(11) 0.030(10) 0.013(11) F8' 0.117(14) 0.110(17) 0.068(12) 0.039(11) 0.019(11) 0.045(12) F9' 0.114(16) 0.110(13) 0.068(11) 0.036(10) -0.013(10) 0.006(11) F7" 0.21(4) 0.064(16) 0.069(17) 0.006(12) -0.05(2) 0.058(19) F9" 0.12(2) 0.13(3) 0.019(8) 0.013(11) 0.024(11) 0.051(19) F8" 0.101(17) 0.13(3) 0.052(14) 0.046(15) 0.020(12) 0.062(15) O1 0.0289(14) 0.0324(16) 0.0390(15) -0.0046(12) -0.0020(12) 0.0004(11) O2 0.0303(15) 0.0329(16) 0.0317(15) 0.0047(12) -0.0006(13) -0.0016(11) O3 0.0237(13) 0.0344(16) 0.0350(15) 0.0004(12) 0.0049(12) -0.0025(11) O4 0.0256(13) 0.0286(15) 0.0359(14) 0.0028(11) 0.0061(12) -0.0052(10) O5 0.0388(15) 0.0351(17) 0.0355(15) 0.0058(13) 0.0038(13) -0.0033(12) O6 0.0267(13) 0.0325(16) 0.0481(17) 0.0029(13) 0.0062(13) -0.0075(11) O7 0.0240(12) 0.0234(14) 0.0397(15) -0.0005(11) 0.0004(11) -0.0022(10) O8 0.0347(15) 0.0283(16) 0.0572(19) -0.0026(13) -0.0035(14) -0.0068(12) N1 0.0198(15) 0.0271(19) 0.0332(17) 0.0046(14) 0.0028(13) 0.0009(12) N2 0.0282(16) 0.0270(19) 0.0374(18) 0.0015(14) 0.0019(14) 0.0012(13) N3 0.0232(15) 0.0280(19) 0.0346(17) 0.0010(14) -0.0018(14) 0.0006(12) C1 0.048(3) 0.032(3) 0.057(3) -0.002(2) 0.002(2) -0.0054(19) C2 0.0256(19) 0.031(2) 0.038(2) -0.0046(17) 0.0075(17) -0.0060(15) C3 0.0267(19) 0.038(3) 0.038(2) -0.0042(18) -0.0016(17) -0.0075(16) C4 0.0198(18) 0.045(3) 0.031(2) 0.0064(19) 0.0018(16) -0.0025(17) C5 0.037(3) 0.054(3) 0.045(3) 0.007(2) -0.007(2) -0.007(2) C6 0.028(2) 0.058(3) 0.042(2) 0.007(2) 0.0055(19) -0.0002(19) C7 0.025(2) 0.043(2) 0.0202(18) -0.0060(16) 0.0036(16) -0.0109(16) C8 0.030(2) 0.042(2) 0.032(2) 0.0012(18) 0.0069(17) -0.0111(17) C9 0.035(2) 0.031(2) 0.0244(18) 0.0010(16) 0.0032(17) -0.0134(16) C10 0.050(3) 0.036(3) 0.051(3) 0.003(2) 0.015(2) -0.009(2) C11 0.061(3) 0.071(4) 0.080(4) -0.002(3) 0.024(3) -0.035(3) C12 0.039(2) 0.035(3) 0.062(3) -0.007(2) 0.021(2) -0.0160(19) C13 0.054(3) 0.042(3) 0.068(3) 0.014(2) 0.019(3) -0.014(2) C14 0.064(3) 0.034(3) 0.044(3) 0.007(2) 0.024(2) 0.000(2) C15 0.085(4) 0.060(4) 0.052(3) 0.028(3) 0.013(3) -0.003(3) C16 0.0244(18) 0.025(2) 0.032(2) 0.0012(16) 0.0047(16) -0.0017(14) C17 0.028(2) 0.034(2) 0.038(2) 0.0048(18) 0.0013(18) 0.0037(16) C18 0.0246(19) 0.030(2) 0.043(2) 0.0050(18) -0.0034(18) 0.0057(15) C19 0.045(3) 0.030(2) 0.060(3) 0.011(2) -0.005(2) 0.0025(18) C20 0.041(2) 0.061(3) 0.050(3) -0.007(2) 0.005(2) 0.015(2) C21 0.056(3) 0.042(3) 0.035(2) 0.003(2) -0.008(2) 0.011(2) C22 0.020(2) 0.044(3) 0.084(4) 0.011(2) -0.005(2) 0.0010(17) C23 0.0217(17) 0.029(2) 0.0298(19) 0.0006(16) 0.0049(16) 0.0010(14) C24 0.031(2) 0.030(2) 0.037(2) -0.0056(17) 0.0033(18) -0.0016(16) C25 0.030(2) 0.041(3) 0.038(2) -0.0056(19) -0.0057(18) 0.0006(17) C26 0.030(2) 0.044(3) 0.039(2) -0.0010(19) -0.0093(19) 0.0050(18) C27 0.029(2) 0.033(2) 0.038(2) 0.0015(17) -0.0015(18) 0.0040(16) C28 0.075(7) 0.074(8) 0.066(8) 0.003(7) 0.000(6) 0.024(6) C29 0.068(7) 0.071(7) 0.048(6) -0.006(5) 0.013(5) -0.005(5) C30 0.061(6) 0.050(6) 0.038(7) -0.003(5) 0.013(5) -0.005(5) C31 0.064(7) 0.051(5) 0.058(6) 0.002(5) 0.015(5) 0.001(4) C32 0.069(7) 0.065(7) 0.044(8) 0.002(6) 0.011(6) 0.006(6) C33 0.068(7) 0.068(7) 0.068(7) 0.013(5) 0.023(6) 0.002(5) C34 0.079(8) 0.096(9) 0.083(10) 0.009(8) 0.011(7) -0.015(7) _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 O5 2.289(3) . ? Dy1 O2 2.303(3) . ? Dy1 O3 2.330(2) . ? Dy1 O7 2.333(3) . ? Dy1 O4 2.342(3) . ? Dy1 O6 2.354(3) . ? Dy1 O1 2.364(3) . ? Dy1 N3 2.632(3) . ? F1 C5 1.339(6) . ? F2 C5 1.324(5) . ? F3 C5 1.329(6) . ? F4 C10 1.332(5) . ? F5 C10 1.326(5) . ? F6 C10 1.323(5) . ? F7 C11 1.317(6) . ? F7 H11C 0.5985 . ? F8 C11 1.357(6) . ? F8 H11B 0.6941 . ? F9 C11 1.254(6) . ? F9 H11A 0.5940 . ? F7' C15 1.338(9) . ? F8' C15 1.272(9) . ? F9' C15 1.309(9) . ? F7" C15 1.319(9) . ? F9" C15 1.293(9) . ? F8" C15 1.306(9) . ? O1 C2 1.253(4) . ? O2 C4 1.276(5) . ? O3 C7 1.258(5) . ? O4 C9 1.274(4) . ? O5 C14 1.271(5) . ? O6 C12 1.249(5) . ? O7 N1 1.297(4) . ? O8 N2 1.269(4) . ? N1 C16 1.334(4) . ? N1 C18 1.505(4) . ? N2 C16 1.354(5) . ? N2 C17 1.506(4) . ? N3 C27 1.343(5) . ? N3 C23 1.359(5) . ? C1 C2 1.510(6) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.421(5) . ? C3 C4 1.368(6) . ? C3 H3 0.9500 . ? C4 C5 1.525(6) . ? C6 C7 1.511(6) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.410(6) . ? C8 C9 1.373(5) . ? C8 H8A 0.9500 . ? C9 C10 1.529(6) . ? C11 C12 1.534(6) . ? C11 H11A 0.9601 . ? C11 H11B 0.9600 . ? C11 H11C 0.9599 . ? C12 C13 1.385(6) . ? C13 C14 1.374(6) . ? C13 H13 0.9500 . ? C14 C15 1.514(6) . ? C16 C23 1.477(5) . ? C17 C20 1.524(6) . ? C17 C19 1.524(6) . ? C17 C18 1.552(6) . ? C18 C21 1.529(6) . ? C18 C22 1.531(5) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.388(5) . ? C24 C25 1.385(5) . ? C24 H24 0.9500 . ? C25 C26 1.366(6) . ? C25 H25 0.9500 . ? C26 C27 1.385(5) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 C34 0.48(2) 2_656 ? C28 C29 1.535(9) . ? C28 C33 1.823(17) 2_656 ? C28 H28A 0.9600 . ? C28 H28B 0.9601 . ? C28 H28C 0.9599 . ? C29 C33 0.943(15) 2_656 ? C29 C34 1.094(19) 2_656 ? C29 C30 1.537(9) . ? C29 C32 1.784(16) 2_656 ? C29 H29A 0.9600 . ? C29 H29B 0.9601 . ? C30 C32 0.501(15) 2_656 ? C30 C33 1.131(16) 2_656 ? C30 C31 1.531(8) . ? C30 C31 1.796(15) 2_656 ? C30 H30A 0.9599 . ? C30 H30B 0.9600 . ? C31 C31 0.958(19) 2_656 ? C31 C32 1.103(15) 2_656 ? C31 C32 1.539(9) . ? C31 C30 1.796(15) 2_656 ? C31 H31A 0.9601 . ? C31 H31B 0.9600 . ? C32 C30 0.501(15) 2_656 ? C32 C31 1.103(15) 2_656 ? C32 C33 1.537(9) . ? C32 C29 1.784(16) 2_656 ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C33 C29 0.943(15) 2_656 ? C33 C30 1.131(16) 2_656 ? C33 C34 1.538(9) . ? C33 C28 1.823(17) 2_656 ? C33 H33A 0.9601 . ? C33 H33B 0.9600 . ? C34 C28 0.48(2) 2_656 ? C34 C29 1.094(19) 2_656 ? C34 H34A 0.9601 . ? C34 H34B 0.9598 . ? C34 H34C 0.9599 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Dy1 O2 143.88(9) . . ? O5 Dy1 O3 86.07(10) . . ? O2 Dy1 O3 111.18(10) . . ? O5 Dy1 O7 101.01(10) . . ? O2 Dy1 O7 84.67(10) . . ? O3 Dy1 O7 142.24(9) . . ? O5 Dy1 O4 142.43(9) . . ? O2 Dy1 O4 73.67(9) . . ? O3 Dy1 O4 73.78(9) . . ? O7 Dy1 O4 78.75(9) . . ? O5 Dy1 O6 73.06(10) . . ? O2 Dy1 O6 75.53(10) . . ? O3 Dy1 O6 145.36(9) . . ? O7 Dy1 O6 70.45(10) . . ? O4 Dy1 O6 137.93(9) . . ? O5 Dy1 O1 81.31(10) . . ? O2 Dy1 O1 73.84(9) . . ? O3 Dy1 O1 74.36(9) . . ? O7 Dy1 O1 143.19(8) . . ? O4 Dy1 O1 121.27(10) . . ? O6 Dy1 O1 75.36(10) . . ? O5 Dy1 N3 74.11(10) . . ? O2 Dy1 N3 138.99(9) . . ? O3 Dy1 N3 77.85(10) . . ? O7 Dy1 N3 68.88(9) . . ? O4 Dy1 N3 70.87(9) . . ? O6 Dy1 N3 120.38(10) . . ? O1 Dy1 N3 143.84(9) . . ? C11 F7 H11C 42.1 . . ? C11 F8 H11B 41.9 . . ? C11 F9 H11A 47.7 . . ? C2 O1 Dy1 133.0(2) . . ? C4 O2 Dy1 131.0(3) . . ? C7 O3 Dy1 136.7(3) . . ? C9 O4 Dy1 133.0(2) . . ? C14 O5 Dy1 137.0(3) . . ? C12 O6 Dy1 133.9(3) . . ? N1 O7 Dy1 124.9(2) . . ? O7 N1 C16 127.5(3) . . ? O7 N1 C18 119.1(3) . . ? C16 N1 C18 113.1(3) . . ? O8 N2 C16 127.0(3) . . ? O8 N2 C17 121.0(3) . . ? C16 N2 C17 111.7(3) . . ? C27 N3 C23 116.7(3) . . ? C27 N3 Dy1 115.7(3) . . ? C23 N3 Dy1 127.2(2) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C3 124.1(4) . . ? O1 C2 C1 117.8(3) . . ? C3 C2 C1 118.0(3) . . ? C4 C3 C2 122.6(3) . . ? C4 C3 H3 118.7 . . ? C2 C3 H3 118.7 . . ? O2 C4 C3 129.5(4) . . ? O2 C4 C5 111.6(4) . . ? C3 C4 C5 118.9(4) . . ? F2 C5 F3 107.1(4) . . ? F2 C5 F1 105.8(4) . . ? F3 C5 F1 107.0(4) . . ? F2 C5 C4 112.5(3) . . ? F3 C5 C4 114.1(4) . . ? F1 C5 C4 109.8(4) . . ? C7 C6 H6A 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C7 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O3 C7 C8 124.7(4) . . ? O3 C7 C6 117.4(4) . . ? C8 C7 C6 117.8(4) . . ? C9 C8 C7 122.9(4) . . ? C9 C8 H8A 118.5 . . ? C7 C8 H8A 118.5 . . ? O4 C9 C8 128.6(4) . . ? O4 C9 C10 113.1(3) . . ? C8 C9 C10 118.3(4) . . ? F6 C10 F5 107.8(4) . . ? F6 C10 F4 106.4(4) . . ? F5 C10 F4 105.9(4) . . ? F6 C10 C9 111.1(4) . . ? F5 C10 C9 114.3(4) . . ? F4 C10 C9 110.9(3) . . ? F9 C11 F7 111.6(5) . . ? F9 C11 F8 108.9(5) . . ? F7 C11 F8 105.8(5) . . ? F9 C11 C12 112.2(4) . . ? F7 C11 C12 107.6(5) . . ? F8 C11 C12 110.6(5) . . ? F9 C11 H11A 27.2 . . ? F7 C11 H11A 87.8 . . ? F8 C11 H11A 130.7 . . ? C12 C11 H11A 109.6 . . ? F9 C11 H11B 83.7 . . ? F7 C11 H11B 130.1 . . ? F8 C11 H11B 28.9 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? F9 C11 H11C 128.6 . . ? F7 C11 H11C 24.7 . . ? F8 C11 H11C 82.5 . . ? C12 C11 H11C 109.3 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? O6 C12 C13 127.2(4) . . ? O6 C12 C11 114.9(4) . . ? C13 C12 C11 118.0(4) . . ? C14 C13 C12 122.9(4) . . ? C14 C13 H13 118.6 . . ? C12 C13 H13 118.6 . . ? O5 C14 C13 125.5(4) . . ? O5 C14 C15 116.0(4) . . ? C13 C14 C15 118.4(4) . . ? F8' C15 F9" 143.5(13) . . ? F8' C15 F8" 47.4(9) . . ? F9" C15 F8" 113.3(8) . . ? F8' C15 F9' 114.6(8) . . ? F9" C15 F9' 47.7(9) . . ? F8" C15 F9' 69.4(9) . . ? F8' C15 F7" 65.2(10) . . ? F9" C15 F7" 112.6(8) . . ? F8" C15 F7" 111.2(8) . . ? F9' C15 F7" 149.5(12) . . ? F8' C15 F7' 112.8(8) . . ? F9" C15 F7' 62.9(10) . . ? F8" C15 F7' 144.9(12) . . ? F9' C15 F7' 109.5(7) . . ? F7" C15 F7' 51.5(10) . . ? F8' C15 C14 109.3(10) . . ? F9" C15 C14 106.3(9) . . ? F8" C15 C14 107.5(9) . . ? F9' C15 C14 103.2(9) . . ? F7" C15 C14 105.3(9) . . ? F7' C15 C14 106.8(8) . . ? N1 C16 N2 108.6(3) . . ? N1 C16 C23 125.7(3) . . ? N2 C16 C23 125.5(3) . . ? N2 C17 C20 105.1(3) . . ? N2 C17 C19 109.0(3) . . ? C20 C17 C19 110.5(4) . . ? N2 C17 C18 101.1(3) . . ? C20 C17 C18 114.8(4) . . ? C19 C17 C18 115.2(3) . . ? N1 C18 C21 106.5(3) . . ? N1 C18 C22 108.4(3) . . ? C21 C18 C22 110.5(4) . . ? N1 C18 C17 100.5(3) . . ? C21 C18 C17 114.8(4) . . ? C22 C18 C17 115.2(4) . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C18 C22 H22A 109.5 . . ? C18 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C18 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N3 C23 C24 122.4(3) . . ? N3 C23 C16 118.1(3) . . ? C24 C23 C16 119.5(3) . . ? C25 C24 C23 119.6(4) . . ? C25 C24 H24 120.2 . . ? C23 C24 H24 120.2 . . ? C26 C25 C24 118.3(4) . . ? C26 C25 H25 120.8 . . ? C24 C25 H25 120.8 . . ? C25 C26 C27 119.5(4) . . ? C25 C26 H26 120.3 . . ? C27 C26 H26 120.3 . . ? N3 C27 C26 123.5(4) . . ? N3 C27 H27 118.2 . . ? C26 C27 H27 118.2 . . ? C34 C28 C29 19(3) 2_656 . ? C34 C28 C33 47(3) 2_656 2_656 ? C29 C28 C33 31.2(6) . 2_656 ? C34 C28 H28A 106.3 2_656 . ? C29 C28 H28A 108.8 . . ? C33 C28 H28A 128.8 2_656 . ? C34 C28 H28B 93.8 2_656 . ? C29 C28 H28B 110.1 . . ? C33 C28 H28B 114.5 2_656 . ? H28A C28 H28B 109.5 . . ? C34 C28 H28C 126.7 2_656 . ? C29 C28 H28C 109.5 . . ? C33 C28 H28C 79.5 2_656 . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C33 C29 C34 97.7(15) 2_656 2_656 ? C33 C29 C28 91.5(13) 2_656 . ? C34 C29 C28 8.3(15) 2_656 . ? C33 C29 C30 47.1(9) 2_656 . ? C34 C29 C30 110.3(16) 2_656 . ? C28 C29 C30 110.0(8) . . ? C33 C29 C32 59.5(9) 2_656 2_656 ? C34 C29 C32 121.0(17) 2_656 2_656 ? C28 C29 C32 122.2(10) . 2_656 ? C30 C29 C32 15.1(7) . 2_656 ? C33 C29 H29A 76.7 2_656 . ? C34 C29 H29A 117.1 2_656 . ? C28 C29 H29A 110.3 . . ? C30 C29 H29A 109.4 . . ? C32 C29 H29A 109.4 2_656 . ? C33 C29 H29B 153.9 2_656 . ? C34 C29 H29B 102.2 2_656 . ? C28 C29 H29B 109.7 . . ? C30 C29 H29B 109.2 . . ? C32 C29 H29B 95.5 2_656 . ? H29A C29 H29B 108.2 . . ? C32 C30 C33 137(3) 2_656 2_656 ? C32 C30 C31 26(2) 2_656 . ? C33 C30 C31 121.1(13) 2_656 . ? C32 C30 C29 112(3) 2_656 . ? C33 C30 C29 37.7(7) 2_656 . ? C31 C30 C29 111.7(8) . . ? C32 C30 C31 52(2) 2_656 2_656 ? C33 C30 C31 118.7(13) 2_656 2_656 ? C31 C30 C31 32.2(7) . 2_656 ? C29 C30 C31 132.3(9) . 2_656 ? C32 C30 H30A 85.5 2_656 . ? C33 C30 H30A 126.7 2_656 . ? C31 C30 H30A 109.2 . . ? C29 C30 H30A 109.1 . . ? C31 C30 H30A 112.9 2_656 . ? C32 C30 H30B 129.6 2_656 . ? C33 C30 H30B 71.6 2_656 . ? C31 C30 H30B 109.8 . . ? C29 C30 H30B 109.0 . . ? C31 C30 H30B 78.7 2_656 . ? H30A C30 H30B 108.0 . . ? C31 C31 C32 96.4(13) 2_656 2_656 ? C31 C31 C30 89.3(12) 2_656 . ? C32 C31 C30 11.5(10) 2_656 . ? C31 C31 C32 45.4(8) 2_656 . ? C32 C31 C32 109.2(14) 2_656 . ? C30 C31 C32 110.2(7) . . ? C31 C31 C30 58.5(8) 2_656 2_656 ? C32 C31 C30 118.6(10) 2_656 2_656 ? C30 C31 C30 121.8(9) . 2_656 ? C32 C31 C30 14.9(7) . 2_656 ? C31 C31 H31A 79.0 2_656 . ? C32 C31 H31A 119.6 2_656 . ? C30 C31 H31A 109.5 . . ? C32 C31 H31A 108.6 . . ? C30 C31 H31A 109.6 2_656 . ? C31 C31 H31B 154.5 2_656 . ? C32 C31 H31B 100.6 2_656 . ? C30 C31 H31B 110.1 . . ? C32 C31 H31B 110.4 . . ? C30 C31 H31B 96.5 2_656 . ? H31A C31 H31B 108.1 . . ? C30 C32 C31 143(3) 2_656 2_656 ? C30 C32 C33 30(3) 2_656 . ? C31 C32 C33 122.7(13) 2_656 . ? C30 C32 C31 113(3) 2_656 . ? C31 C32 C31 38.2(10) 2_656 . ? C33 C32 C31 111.4(8) . . ? C30 C32 C29 53(2) 2_656 2_656 ? C31 C32 C29 121.4(14) 2_656 2_656 ? C33 C32 C29 31.9(6) . 2_656 ? C31 C32 C29 133.0(11) . 2_656 ? C30 C32 H32A 78.8 2_656 . ? C31 C32 H32A 126.4 2_656 . ? C33 C32 H32A 107.2 . . ? C31 C32 H32A 108.4 . . ? C29 C32 H32A 111.0 2_656 . ? C30 C32 H32B 131.1 2_656 . ? C31 C32 H32B 72.3 2_656 . ? C33 C32 H32B 111.6 . . ? C31 C32 H32B 110.2 . . ? C29 C32 H32B 80.7 2_656 . ? H32A C32 H32B 108.0 . . ? C29 C33 C30 95.2(12) 2_656 2_656 ? C29 C33 C32 88.6(12) 2_656 . ? C30 C33 C32 12.8(10) 2_656 . ? C29 C33 C34 44.8(11) 2_656 . ? C30 C33 C34 108.1(12) 2_656 . ? C32 C33 C34 110.6(8) . . ? C29 C33 C28 57.3(10) 2_656 2_656 ? C30 C33 C28 114.8(13) 2_656 2_656 ? C32 C33 C28 119.7(10) . 2_656 ? C34 C33 C28 13.2(11) . 2_656 ? C29 C33 H33A 77.5 2_656 . ? C30 C33 H33A 119.4 2_656 . ? C32 C33 H33A 107.3 . . ? C34 C33 H33A 107.0 . . ? C28 C33 H33A 110.6 2_656 . ? C29 C33 H33B 155.2 2_656 . ? C30 C33 H33B 102.3 2_656 . ? C32 C33 H33B 111.7 . . ? C34 C33 H33B 112.0 . . ? C28 C33 H33B 99.0 2_656 . ? H33A C33 H33B 108.1 . . ? C28 C34 C29 152(5) 2_656 2_656 ? C28 C34 C33 120(4) 2_656 . ? C29 C34 C33 37.4(8) 2_656 . ? C28 C34 H34A 43.8 2_656 . ? C29 C34 H34A 118.5 2_656 . ? C33 C34 H34A 109.6 . . ? C28 C34 H34B 127.4 2_656 . ? C29 C34 H34B 75.0 2_656 . ? C33 C34 H34B 111.9 . . ? H34A C34 H34B 109.5 . . ? C28 C34 H34C 65.8 2_656 . ? C29 C34 H34C 127.1 2_656 . ? C33 C34 H34C 106.9 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O5 Dy1 O1 C2 -128.0(4) . . . . ? O2 Dy1 O1 C2 25.5(3) . . . . ? O3 Dy1 O1 C2 143.6(4) . . . . ? O7 Dy1 O1 C2 -31.3(4) . . . . ? O4 Dy1 O1 C2 84.3(4) . . . . ? O6 Dy1 O1 C2 -53.4(3) . . . . ? N3 Dy1 O1 C2 -175.3(3) . . . . ? O5 Dy1 O2 C4 25.9(4) . . . . ? O3 Dy1 O2 C4 -88.1(3) . . . . ? O7 Dy1 O2 C4 127.3(3) . . . . ? O4 Dy1 O2 C4 -152.9(4) . . . . ? O6 Dy1 O2 C4 56.2(3) . . . . ? O1 Dy1 O2 C4 -22.5(3) . . . . ? N3 Dy1 O2 C4 176.1(3) . . . . ? O5 Dy1 O3 C7 153.3(4) . . . . ? O2 Dy1 O3 C7 -59.4(4) . . . . ? O7 Dy1 O3 C7 50.3(4) . . . . ? O4 Dy1 O3 C7 5.3(3) . . . . ? O6 Dy1 O3 C7 -154.6(3) . . . . ? O1 Dy1 O3 C7 -124.7(4) . . . . ? N3 Dy1 O3 C7 78.7(4) . . . . ? O5 Dy1 O4 C9 -64.8(4) . . . . ? O2 Dy1 O4 C9 114.1(3) . . . . ? O3 Dy1 O4 C9 -4.4(3) . . . . ? O7 Dy1 O4 C9 -158.2(3) . . . . ? O6 Dy1 O4 C9 158.6(3) . . . . ? O1 Dy1 O4 C9 55.2(3) . . . . ? N3 Dy1 O4 C9 -86.9(3) . . . . ? O2 Dy1 O5 C14 25.1(5) . . . . ? O3 Dy1 O5 C14 146.4(4) . . . . ? O7 Dy1 O5 C14 -71.0(4) . . . . ? O4 Dy1 O5 C14 -156.8(4) . . . . ? O6 Dy1 O5 C14 -5.6(4) . . . . ? O1 Dy1 O5 C14 71.7(4) . . . . ? N3 Dy1 O5 C14 -135.1(4) . . . . ? O5 Dy1 O6 C12 8.1(4) . . . . ? O2 Dy1 O6 C12 -153.8(4) . . . . ? O3 Dy1 O6 C12 -47.4(5) . . . . ? O7 Dy1 O6 C12 116.8(4) . . . . ? O4 Dy1 O6 C12 162.1(4) . . . . ? O1 Dy1 O6 C12 -77.1(4) . . . . ? N3 Dy1 O6 C12 67.4(4) . . . . ? O5 Dy1 O7 N1 -121.5(3) . . . . ? O2 Dy1 O7 N1 94.6(3) . . . . ? O3 Dy1 O7 N1 -23.6(3) . . . . ? O4 Dy1 O7 N1 20.2(2) . . . . ? O6 Dy1 O7 N1 171.1(3) . . . . ? O1 Dy1 O7 N1 148.3(2) . . . . ? N3 Dy1 O7 N1 -53.5(2) . . . . ? Dy1 O7 N1 C16 49.9(5) . . . . ? Dy1 O7 N1 C18 -124.4(3) . . . . ? O5 Dy1 N3 C27 -42.0(3) . . . . ? O2 Dy1 N3 C27 155.7(3) . . . . ? O3 Dy1 N3 C27 47.3(3) . . . . ? O7 Dy1 N3 C27 -150.9(3) . . . . ? O4 Dy1 N3 C27 124.2(3) . . . . ? O6 Dy1 N3 C27 -100.8(3) . . . . ? O1 Dy1 N3 C27 7.0(4) . . . . ? O5 Dy1 N3 C23 145.6(3) . . . . ? O2 Dy1 N3 C23 -16.7(4) . . . . ? O3 Dy1 N3 C23 -125.1(3) . . . . ? O7 Dy1 N3 C23 36.7(3) . . . . ? O4 Dy1 N3 C23 -48.3(3) . . . . ? O6 Dy1 N3 C23 86.8(3) . . . . ? O1 Dy1 N3 C23 -165.4(3) . . . . ? Dy1 O1 C2 C3 -21.2(6) . . . . ? Dy1 O1 C2 C1 158.8(3) . . . . ? O1 C2 C3 C4 1.2(7) . . . . ? C1 C2 C3 C4 -178.8(4) . . . . ? Dy1 O2 C4 C3 17.2(6) . . . . ? Dy1 O2 C4 C5 -161.3(3) . . . . ? C2 C3 C4 O2 0.8(7) . . . . ? C2 C3 C4 C5 179.3(4) . . . . ? O2 C4 C5 F2 -43.5(6) . . . . ? C3 C4 C5 F2 137.8(4) . . . . ? O2 C4 C5 F3 -165.8(4) . . . . ? C3 C4 C5 F3 15.5(6) . . . . ? O2 C4 C5 F1 74.1(5) . . . . ? C3 C4 C5 F1 -104.6(5) . . . . ? Dy1 O3 C7 C8 -2.9(6) . . . . ? Dy1 O3 C7 C6 178.4(3) . . . . ? O3 C7 C8 C9 -3.4(6) . . . . ? C6 C7 C8 C9 175.3(4) . . . . ? Dy1 O4 C9 C8 1.4(6) . . . . ? Dy1 O4 C9 C10 -179.3(2) . . . . ? C7 C8 C9 O4 4.1(6) . . . . ? C7 C8 C9 C10 -175.1(4) . . . . ? O4 C9 C10 F6 -58.1(5) . . . . ? C8 C9 C10 F6 121.3(4) . . . . ? O4 C9 C10 F5 179.6(4) . . . . ? C8 C9 C10 F5 -1.0(6) . . . . ? O4 C9 C10 F4 60.0(5) . . . . ? C8 C9 C10 F4 -120.7(4) . . . . ? Dy1 O6 C12 C13 -8.3(8) . . . . ? Dy1 O6 C12 C11 171.2(3) . . . . ? F9 C11 C12 O6 29.6(7) . . . . ? F7 C11 C12 O6 -93.5(5) . . . . ? F8 C11 C12 O6 151.4(5) . . . . ? F9 C11 C12 C13 -150.9(5) . . . . ? F7 C11 C12 C13 86.1(6) . . . . ? F8 C11 C12 C13 -29.0(7) . . . . ? O6 C12 C13 C14 1.5(8) . . . . ? C11 C12 C13 C14 -177.9(5) . . . . ? Dy1 O5 C14 C13 2.9(8) . . . . ? Dy1 O5 C14 C15 -178.9(3) . . . . ? C12 C13 C14 O5 1.3(8) . . . . ? C12 C13 C14 C15 -176.9(5) . . . . ? O5 C14 C15 F8' 60.2(13) . . . . ? C13 C14 C15 F8' -121.4(13) . . . . ? O5 C14 C15 F9" -111.5(15) . . . . ? C13 C14 C15 F9" 66.9(15) . . . . ? O5 C14 C15 F8" 10.1(15) . . . . ? C13 C14 C15 F8" -171.5(14) . . . . ? O5 C14 C15 F9' -62.1(13) . . . . ? C13 C14 C15 F9' 116.2(13) . . . . ? O5 C14 C15 F7" 128.8(16) . . . . ? C13 C14 C15 F7" -52.8(16) . . . . ? O5 C14 C15 F7' -177.5(12) . . . . ? C13 C14 C15 F7' 0.9(12) . . . . ? O7 N1 C16 N2 179.7(4) . . . . ? C18 N1 C16 N2 -5.7(5) . . . . ? O7 N1 C16 C23 4.6(6) . . . . ? C18 N1 C16 C23 179.2(4) . . . . ? O8 N2 C16 N1 176.9(4) . . . . ? C17 N2 C16 N1 -9.9(4) . . . . ? O8 N2 C16 C23 -7.9(7) . . . . ? C17 N2 C16 C23 165.2(4) . . . . ? O8 N2 C17 C20 74.1(5) . . . . ? C16 N2 C17 C20 -99.5(4) . . . . ? O8 N2 C17 C19 -44.4(5) . . . . ? C16 N2 C17 C19 142.0(4) . . . . ? O8 N2 C17 C18 -166.2(3) . . . . ? C16 N2 C17 C18 20.2(4) . . . . ? O7 N1 C18 C21 72.7(4) . . . . ? C16 N1 C18 C21 -102.3(4) . . . . ? O7 N1 C18 C22 -46.1(5) . . . . ? C16 N1 C18 C22 138.8(4) . . . . ? O7 N1 C18 C17 -167.2(3) . . . . ? C16 N1 C18 C17 17.7(4) . . . . ? N2 C17 C18 N1 -20.8(4) . . . . ? C20 C17 C18 N1 91.8(4) . . . . ? C19 C17 C18 N1 -138.1(3) . . . . ? N2 C17 C18 C21 93.0(4) . . . . ? C20 C17 C18 C21 -154.5(3) . . . . ? C19 C17 C18 C21 -24.3(5) . . . . ? N2 C17 C18 C22 -136.9(3) . . . . ? C20 C17 C18 C22 -24.4(5) . . . . ? C19 C17 C18 C22 105.7(4) . . . . ? C27 N3 C23 C24 -2.0(6) . . . . ? Dy1 N3 C23 C24 170.4(3) . . . . ? C27 N3 C23 C16 175.6(4) . . . . ? Dy1 N3 C23 C16 -12.0(5) . . . . ? N1 C16 C23 N3 -21.0(6) . . . . ? N2 C16 C23 N3 164.6(4) . . . . ? N1 C16 C23 C24 156.7(4) . . . . ? N2 C16 C23 C24 -17.7(6) . . . . ? N3 C23 C24 C25 2.9(6) . . . . ? C16 C23 C24 C25 -174.7(4) . . . . ? C23 C24 C25 C26 -1.6(6) . . . . ? C24 C25 C26 C27 -0.4(7) . . . . ? C23 N3 C27 C26 -0.1(6) . . . . ? Dy1 N3 C27 C26 -173.4(3) . . . . ? C25 C26 C27 N3 1.3(7) . . . . ? C34 C28 C29 C33 -138(12) 2_656 . . 2_656 ? C33 C28 C29 C34 138(12) 2_656 . . 2_656 ? C34 C28 C29 C30 -94(12) 2_656 . . . ? C33 C28 C29 C30 44.4(11) 2_656 . . . ? C34 C28 C29 C32 -84(12) 2_656 . . 2_656 ? C33 C28 C29 C32 54.3(11) 2_656 . . 2_656 ? C33 C29 C30 C32 -141(4) 2_656 . . 2_656 ? C34 C29 C30 C32 137(3) 2_656 . . 2_656 ? C28 C29 C30 C32 146(3) . . . 2_656 ? C34 C29 C30 C33 -81.5(17) 2_656 . . 2_656 ? C28 C29 C30 C33 -72.6(17) . . . 2_656 ? C32 C29 C30 C33 141(4) 2_656 . . 2_656 ? C33 C29 C30 C31 -113.2(18) 2_656 . . . ? C34 C29 C30 C31 165.3(15) 2_656 . . . ? C28 C29 C30 C31 174.2(12) . . . . ? C32 C29 C30 C31 28(3) 2_656 . . . ? C33 C29 C30 C31 -83.4(18) 2_656 . . 2_656 ? C34 C29 C30 C31 -164.9(15) 2_656 . . 2_656 ? C28 C29 C30 C31 -156.0(13) . . . 2_656 ? C32 C29 C30 C31 58(3) 2_656 . . 2_656 ? C32 C30 C31 C31 -128(6) 2_656 . . 2_656 ? C33 C30 C31 C31 95.4(13) 2_656 . . 2_656 ? C29 C30 C31 C31 136.5(10) . . . 2_656 ? C33 C30 C31 C32 -136(6) 2_656 . . 2_656 ? C29 C30 C31 C32 -95(6) . . . 2_656 ? C31 C30 C31 C32 128(6) 2_656 . . 2_656 ? C32 C30 C31 C32 -87(6) 2_656 . . . ? C33 C30 C31 C32 136.6(13) 2_656 . . . ? C29 C30 C31 C32 177.6(12) . . . . ? C31 C30 C31 C32 41.2(8) 2_656 . . . ? C32 C30 C31 C30 -77(6) 2_656 . . 2_656 ? C33 C30 C31 C30 146.9(14) 2_656 . . 2_656 ? C29 C30 C31 C30 -172.1(10) . . . 2_656 ? C31 C30 C31 C30 51.5(7) 2_656 . . 2_656 ? C31 C31 C32 C30 -149(4) 2_656 . . 2_656 ? C32 C31 C32 C30 132(3) 2_656 . . 2_656 ? C30 C31 C32 C30 144(4) . . . 2_656 ? C32 C31 C32 C31 -79.8(17) 2_656 . . 2_656 ? C30 C31 C32 C31 -67.6(15) . . . 2_656 ? C30 C31 C32 C31 149(4) 2_656 . . 2_656 ? C31 C31 C32 C33 -116.2(18) 2_656 . . . ? C32 C31 C32 C33 164.0(13) 2_656 . . . ? C30 C31 C32 C33 176.1(13) . . . . ? C30 C31 C32 C33 32(3) 2_656 . . . ? C31 C31 C32 C29 -88.1(19) 2_656 . . 2_656 ? C32 C31 C32 C29 -167.9(15) 2_656 . . 2_656 ? C30 C31 C32 C29 -155.7(14) . . . 2_656 ? C30 C31 C32 C29 60(3) 2_656 . . 2_656 ? C30 C32 C33 C29 -121(5) 2_656 . . 2_656 ? C31 C32 C33 C29 98.0(17) 2_656 . . 2_656 ? C31 C32 C33 C29 139.3(14) . . . 2_656 ? C31 C32 C33 C30 -141(5) 2_656 . . 2_656 ? C31 C32 C33 C30 -100(5) . . . 2_656 ? C29 C32 C33 C30 121(5) 2_656 . . 2_656 ? C30 C32 C33 C34 -81(5) 2_656 . . . ? C31 C32 C33 C34 138.0(16) 2_656 . . . ? C31 C32 C33 C34 179.2(13) . . . . ? C29 C32 C33 C34 39.9(14) 2_656 . . . ? C30 C32 C33 C28 -71(5) 2_656 . . 2_656 ? C31 C32 C33 C28 148.6(15) 2_656 . . 2_656 ? C31 C32 C33 C28 -170.1(12) . . . 2_656 ? C29 C32 C33 C28 50.6(11) 2_656 . . 2_656 ? C29 C33 C34 C28 -159(7) 2_656 . . 2_656 ? C30 C33 C34 C28 122(6) 2_656 . . 2_656 ? C32 C33 C34 C28 136(5) . . . 2_656 ? C30 C33 C34 C29 -78.8(17) 2_656 . . 2_656 ? C32 C33 C34 C29 -65.5(19) . . . 2_656 ? C28 C33 C34 C29 159(7) 2_656 . . 2_656 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.839 _refine_diff_density_min -1.580 _refine_diff_density_rms 0.176 #===end