# Electronic Supplementary Material (ESI) for RSC Advances # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'RSC Advances' _journal_coden_cambridge 1500 _journal_year ? _journal_volume ? _journal_page_first ? _publ_author_name 'Jing Xin Liu' _publ_contact_author_name 'Jing Xin Liu' _publ_contact_author_email jxliu411@ahut.edu.cn # Attachment 'compound2a.cif' data_2a _database_code_depnum_ccdc_archive 'CCDC 820005' #TrackingRef 'compound2a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common compound2a _chemical_melting_point 'not measured' _chemical_formula_moiety 'C30 H38 Dy N20 O14, C6 H6 O2,3(N O3), 7(H2 O)' _chemical_formula_sum 'C36 H58 Dy N23 O32' _chemical_formula_weight 1487.55 _chemical_absolute_configuration ' R ' 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' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M P6(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y, x-y, z+1/3' '-x+y, -x, z+2/3' 'x-y, x, z+1/6' 'y, -x+y, z+5/6' _cell_length_a 14.4478(18) _cell_length_b 14.4478(18) _cell_length_c 46.109(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 8335(3) _cell_formula_units_Z 6 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 8785 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 25.73 _exptl_crystal_description block _exptl_crystal_colour 'red brown' _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.778 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4542 _exptl_absorpt_coefficient_mu 1.464 _exptl_absorpt_correction_type 'multi scan' _exptl_absorpt_correction_T_min 0.7294 _exptl_absorpt_correction_T_max 0.8213 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 58125 _diffrn_reflns_av_R_equivalents 0.0470 _diffrn_reflns_av_sigmaI/netI 0.0457 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -56 _diffrn_reflns_limit_l_max 56 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 26.00 _reflns_number_total 10420 _reflns_number_gt 9527 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0782P)^2^+20.1941P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.001(10) _refine_ls_number_reflns 10420 _refine_ls_number_parameters 809 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.0510 _refine_ls_R_factor_gt 0.0448 _refine_ls_wR_factor_ref 0.1223 _refine_ls_wR_factor_gt 0.1191 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.079 _refine_ls_shift/su_mean 0.012 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 0.331105(10) 0.540121(11) 0.597170(4) 0.01911(3) Uani 1 1 d . . . O1W O 0.31084(18) 0.68304(18) 0.58032(6) 0.0320(7) Uani 1 1 d . . . H1WA H 0.2639 0.6900 0.5897 0.038 Uiso 1 1 d R . . H1WB H 0.3453 0.7374 0.5695 0.038 Uiso 1 1 d R . . O2W O 0.15005(17) 0.48820(17) 0.59671(7) 0.0331(7) Uani 1 1 d . . . H2WA H 0.1393 0.5363 0.6039 0.040 Uiso 1 1 d R . . H2WB H 0.0998 0.4274 0.6021 0.040 Uiso 1 1 d R . . O3W O 0.44315(17) 0.46692(18) 0.59960(6) 0.0332(7) Uani 1 1 d . . . H3WA H 0.4235 0.4026 0.5952 0.040 Uiso 1 1 d R . . H3WB H 0.4999 0.5080 0.5903 0.040 Uiso 1 1 d R . . O4W O 0.50590(19) 0.6790(2) 0.60771(6) 0.0359(8) Uani 1 1 d . . . H4WA H 0.5545 0.6779 0.5976 0.043 Uiso 1 1 d R . . H4WB H 0.5308 0.7407 0.6152 0.043 Uiso 1 1 d R . . O5W O 1.0420(3) 0.4844(4) 0.46316(17) 0.135(2) Uani 1 1 d D . . H5WA H 1.0114 0.5161 0.4559 0.162 Uiso 1 1 d RD . . H5WB H 1.0907 0.5281 0.4745 0.162 Uiso 1 1 d R . . O6W O -0.0354(4) -0.0533(4) 0.51983(10) 0.104(2) Uani 1 1 d . . . H6WA H -0.0631 -0.0189 0.5124 0.124 Uiso 1 1 d R . . H6WB H -0.0678 -0.0824 0.5355 0.124 Uiso 1 1 d R . . O7W O 1.0166(3) 0.5877(4) 0.54115(13) 0.102(2) Uani 1 1 d . . . H7WA H 1.0172 0.5540 0.5562 0.122 Uiso 1 1 d R . . H7WB H 1.0773 0.6147 0.5329 0.122 Uiso 1 1 d R . . O8W O 0.6836(6) 0.9470(4) 0.46923(16) 0.148(3) Uani 1 1 d . . . H8WA H 0.6712 0.9599 0.4521 0.178 Uiso 1 1 d R . . H8WB H 0.6979 0.8967 0.4684 0.178 Uiso 1 1 d R . . O9W O 0.4366(3) 0.8347(3) 0.54375(10) 0.0773(14) Uani 1 1 d . . . H9WA H 0.4023 0.8505 0.5316 0.093 Uiso 1 1 d R . . H9WB H 0.4903 0.8923 0.5496 0.093 Uiso 1 1 d R . . O10W O 0.9541(4) 0.2130(8) 0.54971(14) 0.201(5) Uani 1 1 d . . . H10A H 0.9706 0.2386 0.5667 0.242 Uiso 1 1 d R . . H10B H 0.9491 0.2580 0.5389 0.242 Uiso 1 1 d R . . O11W O 0.0171(4) 0.4029(4) 0.39654(16) 0.144(3) Uani 1 1 d . . . H11C H 0.0232 0.4412 0.4112 0.172 Uiso 1 1 d R . . H11D H 0.0171 0.3473 0.4026 0.172 Uiso 1 1 d R . . C31 C -0.0454(4) 0.7342(4) 0.44130(16) 0.082(2) Uani 1 1 d . . . C32 C -0.0200(4) 0.8309(4) 0.45385(15) 0.0655(18) Uani 1 1 d . . . H32 H 0.0274 0.8578 0.4696 0.079 Uiso 1 1 calc R . . C33 C -0.0666(4) 0.8882(4) 0.44255(13) 0.0636(18) Uani 1 1 d . . . H33 H -0.0518 0.9528 0.4514 0.076 Uiso 1 1 calc R . . C34 C -0.1347(4) 0.8517(4) 0.41843(13) 0.0610(18) Uani 1 1 d . . . C35 C -0.1583(4) 0.7554(5) 0.40659(15) 0.085(2) Uani 1 1 d . . . H35 H -0.2040 0.7289 0.3904 0.102 Uiso 1 1 calc R . . C36 C -0.1143(4) 0.6954(4) 0.41857(15) 0.087(2) Uani 1 1 d . . . H36 H -0.1330 0.6282 0.4107 0.105 Uiso 1 1 calc R . . O11 O -0.0060(4) 0.6729(4) 0.45147(15) 0.137(2) Uani 1 1 d . . . H11 H 0.0343 0.7034 0.4654 0.205 Uiso 1 1 calc R . . O12 O -0.1796(3) 0.9062(3) 0.40654(10) 0.0749(14) Uani 1 1 d . . . H12 H -0.1588 0.9632 0.4154 0.112 Uiso 1 1 calc R . . C1 C 0.4158(2) 0.6176(2) 0.52686(7) 0.0207(8) Uani 1 1 d . . . C2 C 0.4817(2) 0.7005(2) 0.48227(8) 0.0199(8) Uani 1 1 d . . . H2A H 0.5026 0.7759 0.4784 0.024 Uiso 1 1 calc R . . C3 C 0.3565(2) 0.6237(2) 0.47969(8) 0.0224(8) Uani 1 1 d . . . H3A H 0.3192 0.6625 0.4739 0.027 Uiso 1 1 calc R . . C4 C 0.4445(2) 0.5678(2) 0.44689(7) 0.0214(8) Uani 1 1 d . . . C5 C 0.2226(2) 0.5134(2) 0.51978(8) 0.0217(8) Uani 1 1 d . . . H5A H 0.1731 0.5227 0.5072 0.026 Uiso 1 1 calc R . . H5B H 0.2163 0.5359 0.5394 0.026 Uiso 1 1 calc R . . C6 C 0.2497(2) 0.4496(2) 0.45110(7) 0.0209(8) Uani 1 1 d . . . H6A H 0.2557 0.4276 0.4314 0.025 Uiso 1 1 calc R . . H6B H 0.1904 0.4643 0.4512 0.025 Uiso 1 1 calc R . . C7 C 0.2083(2) 0.3508(2) 0.54270(8) 0.0212(8) Uani 1 1 d . . . C8 C 0.1480(2) 0.3325(2) 0.49472(8) 0.0223(9) Uani 1 1 d . . . H8A H 0.0796 0.3259 0.4883 0.027 Uiso 1 1 calc R . . C9 C 0.1332(2) 0.2256(3) 0.50560(8) 0.0242(9) Uani 1 1 d . . . H9A H 0.0566 0.1702 0.5063 0.029 Uiso 1 1 calc R . . C10 C 0.2369(2) 0.2789(3) 0.46352(7) 0.0217(9) Uani 1 1 d . . . C11 C 0.1704(3) 0.1688(3) 0.55487(8) 0.0273(10) Uani 1 1 d . . . H11A H 0.1669 0.1920 0.5746 0.033 Uiso 1 1 calc R . . H11B H 0.1034 0.1023 0.5511 0.033 Uiso 1 1 calc R . . C12 C 0.1986(3) 0.1056(3) 0.48381(8) 0.0249(9) Uani 1 1 d . . . H12A H 0.1300 0.0445 0.4897 0.030 Uiso 1 1 calc R . . H12B H 0.2129 0.0929 0.4639 0.030 Uiso 1 1 calc R . . C13 C 0.3441(3) 0.1961(3) 0.57116(8) 0.0255(9) Uani 1 1 d . . . C14 C 0.2659(2) 0.0755(2) 0.53197(8) 0.0226(9) Uani 1 1 d . . . H14A H 0.2056 0.0014 0.5340 0.027 Uiso 1 1 calc R . . C15 C 0.3731(3) 0.0838(3) 0.54091(8) 0.0287(10) Uani 1 1 d . . . H15A H 0.3625 0.0150 0.5485 0.034 Uiso 1 1 calc R . . C16 C 0.3759(2) 0.1251(2) 0.49161(8) 0.0219(9) Uani 1 1 d . . . C17 C 0.5087(3) 0.1920(3) 0.58019(9) 0.0303(10) Uani 1 1 d . . . H17A H 0.5173 0.1289 0.5814 0.036 Uiso 1 1 calc R . . H17B H 0.4968 0.2094 0.5999 0.036 Uiso 1 1 calc R . . C18 C 0.5376(2) 0.1280(2) 0.51138(9) 0.0269(9) Uani 1 1 d . . . H18A H 0.5448 0.0793 0.5248 0.032 Uiso 1 1 calc R . . H18B H 0.5488 0.1103 0.4916 0.032 Uiso 1 1 calc R . . C19 C 0.6431(2) 0.3845(3) 0.57642(7) 0.0216(8) Uani 1 1 d . . . C20 C 0.6717(2) 0.2731(2) 0.54570(7) 0.0220(8) Uani 1 1 d . . . H20A H 0.7055 0.2314 0.5520 0.026 Uiso 1 1 calc R . . C21 C 0.7567(2) 0.3918(2) 0.53928(7) 0.0208(8) Uani 1 1 d . . . H21A H 0.8303 0.4048 0.5420 0.025 Uiso 1 1 calc R . . C22 C 0.6565(2) 0.3141(2) 0.49747(7) 0.0191(8) Uani 1 1 d . . . C23 C 0.7843(2) 0.5651(3) 0.56154(7) 0.0217(9) Uani 1 1 d . . . H23A H 0.8608 0.5940 0.5581 0.026 Uiso 1 1 calc R . . H23B H 0.7761 0.5866 0.5811 0.026 Uiso 1 1 calc R . . C24 C 0.8035(2) 0.4966(2) 0.49153(8) 0.0243(9) Uani 1 1 d . . . H24A H 0.8034 0.4720 0.4717 0.029 Uiso 1 1 calc R . . H24B H 0.8768 0.5289 0.4989 0.029 Uiso 1 1 calc R . . C25 C 0.6810(2) 0.6523(2) 0.54911(8) 0.0207(8) Uani 1 1 d . . . C26 C 0.7968(2) 0.6557(3) 0.51295(8) 0.0232(9) Uani 1 1 d . . . H26A H 0.8748 0.7031 0.5153 0.028 Uiso 1 1 calc R . . C27 C 0.7419(2) 0.7185(2) 0.50220(7) 0.0200(8) Uani 1 1 d . . . H27A H 0.7949 0.7928 0.4968 0.024 Uiso 1 1 calc R . . C28 C 0.7042(2) 0.5795(2) 0.46986(7) 0.0170(8) Uani 1 1 d . . . C29 C 0.6060(2) 0.7551(2) 0.52621(8) 0.0206(9) Uani 1 1 d . . . H29A H 0.6410 0.8246 0.5164 0.025 Uiso 1 1 calc R . . H29B H 0.5907 0.7666 0.5462 0.025 Uiso 1 1 calc R . . C30 C 0.6338(2) 0.6952(2) 0.45591(8) 0.0222(8) Uani 1 1 d . . . H30A H 0.6729 0.7735 0.4567 0.027 Uiso 1 1 calc R . . H30B H 0.6439 0.6743 0.4365 0.027 Uiso 1 1 calc R . . N1 N 0.5057(2) 0.6856(2) 0.51161(6) 0.0223(7) Uani 1 1 d . . . N2 N 0.32884(19) 0.5809(2) 0.50963(6) 0.0206(7) Uani 1 1 d . . . N3 N 0.52183(19) 0.6579(2) 0.46003(6) 0.0206(7) Uani 1 1 d . . . N4 N 0.3472(2) 0.5471(2) 0.45800(7) 0.0247(8) Uani 1 1 d . . . N5 N 0.19109(19) 0.4013(2) 0.52044(6) 0.0209(7) Uani 1 1 d . . . N6 N 0.1798(2) 0.2498(2) 0.53455(6) 0.0236(8) Uani 1 1 d . . . N7 N 0.2243(2) 0.3620(2) 0.47072(7) 0.0249(8) Uani 1 1 d . . . N8 N 0.1897(2) 0.2004(2) 0.48433(7) 0.0273(8) Uani 1 1 d . . . N9 N 0.2570(2) 0.1481(2) 0.55314(7) 0.0267(8) Uani 1 1 d . . . N10 N 0.4166(2) 0.1664(2) 0.56270(7) 0.0275(8) Uani 1 1 d . . . N11 N 0.2805(2) 0.1104(2) 0.50223(6) 0.0226(8) Uani 1 1 d . . . N12 N 0.4308(2) 0.1125(2) 0.51368(6) 0.0238(7) Uani 1 1 d . . . N13 N 0.6075(2) 0.2819(2) 0.56871(7) 0.0274(8) Uani 1 1 d . . . N14 N 0.7313(2) 0.4502(2) 0.56034(6) 0.0227(7) Uani 1 1 d . . . N15 N 0.6171(2) 0.2350(2) 0.51788(7) 0.0256(8) Uani 1 1 d . . . N16 N 0.7365(2) 0.4072(2) 0.50893(6) 0.0217(7) Uani 1 1 d . . . N17 N 0.74449(19) 0.61193(19) 0.54075(6) 0.0184(7) Uani 1 1 d . . . N18 N 0.67874(19) 0.71492(18) 0.52697(6) 0.0184(7) Uani 1 1 d . . . N19 N 0.77247(19) 0.57808(19) 0.49059(6) 0.0194(7) Uani 1 1 d . . . N20 N 0.67966(19) 0.65549(19) 0.47683(6) 0.0199(7) Uani 1 1 d . . . O1 O 0.41626(16) 0.59403(18) 0.55265(5) 0.0231(6) Uani 1 1 d . . . O2 O 0.24236(17) 0.38844(18) 0.56729(5) 0.0255(6) Uani 1 1 d . . . O3 O 0.35346(18) 0.25369(18) 0.59167(6) 0.0308(7) Uani 1 1 d . . . O4 O 0.60695(17) 0.41398(18) 0.59604(6) 0.0310(7) Uani 1 1 d . . . O5 O 0.63650(17) 0.63713(18) 0.57249(5) 0.0262(6) Uani 1 1 d . . . O7 O 0.45729(16) 0.51787(17) 0.42831(6) 0.0285(6) Uani 1 1 d . . . O8 O 0.28155(17) 0.27182(18) 0.44136(6) 0.0279(7) Uani 1 1 d . . . O9 O 0.40454(17) 0.14560(17) 0.46637(5) 0.0229(6) Uani 1 1 d . . . O10 O 0.62606(17) 0.30370(17) 0.47200(5) 0.0257(6) Uani 1 1 d . . . O6 O 0.67103(17) 0.52194(18) 0.44821(5) 0.0255(7) Uani 1 1 d . . . N21 N -0.0552(3) 0.1568(3) 0.44092(8) 0.0770(17) Uani 1 1 d D . . O13 O -0.1209(4) 0.1072(4) 0.42095(10) 0.130(2) Uani 1 1 d D . . O14 O 0.0242(3) 0.2478(4) 0.43743(15) 0.134(3) Uani 1 1 d D . . O15 O -0.0765(5) 0.1170(5) 0.46611(10) 0.160(3) Uani 1 1 d D . . N22 N 0.8623(3) 0.2823(4) 0.49467(9) 0.129(2) Uani 1 1 d D . . O16 O 0.8606(4) 0.3109(4) 0.46845(11) 0.175(3) Uani 1 1 d D . . O17 O 0.9348(4) 0.3413(4) 0.51193(15) 0.176(4) Uani 1 1 d D . . O18 O 0.7854(5) 0.1882(5) 0.50328(19) 0.215(5) Uani 1 1 d D . . O19 O 0.1907(5) 0.7080(3) 0.4976(2) 0.170(3) Uiso 1 1 d D . . N23 N 0.2194(3) 0.8051(4) 0.5044(3) 0.196(8) Uiso 1 1 d D . . O20 O 0.1416(4) 0.8203(5) 0.5007(3) 0.213(5) Uiso 1 1 d D . . O21 O 0.3186(4) 0.8761(7) 0.5005(4) 0.219(8) Uiso 1 1 d 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 0.02111(5) 0.02342(5) 0.01246(6) -0.00123(5) 0.00287(5) 0.01088(4) O1W 0.0373(10) 0.0344(10) 0.0309(14) 0.0092(9) 0.0154(10) 0.0229(7) O2W 0.0266(9) 0.0230(9) 0.0469(15) -0.0058(11) 0.0020(12) 0.0104(7) O3W 0.0284(9) 0.0359(10) 0.0374(15) -0.0017(11) 0.0063(11) 0.0177(7) O4W 0.0245(10) 0.0395(12) 0.0354(15) -0.0125(11) 0.0030(10) 0.0097(9) O5W 0.109(2) 0.180(3) 0.166(6) -0.039(4) -0.023(3) 0.1106(18) O6W 0.108(3) 0.080(3) 0.053(3) 0.004(2) -0.006(3) -0.005(3) O7W 0.056(2) 0.118(3) 0.113(4) -0.004(3) 0.006(2) 0.031(2) O8W 0.236(6) 0.085(3) 0.116(5) 0.026(3) 0.009(5) 0.074(3) O9W 0.0681(19) 0.0630(18) 0.092(3) 0.0335(19) 0.011(2) 0.0263(15) O10W 0.079(3) 0.372(10) 0.067(4) -0.068(5) -0.007(3) 0.048(5) O11W 0.071(3) 0.102(3) 0.219(6) 0.093(3) 0.008(3) 0.014(2) C31 0.053(2) 0.054(2) 0.133(5) 0.039(3) 0.052(3) 0.0234(19) C32 0.050(2) 0.053(2) 0.085(4) 0.009(3) 0.019(3) 0.0189(19) C33 0.057(3) 0.051(2) 0.063(3) -0.002(2) 0.013(3) 0.012(2) C34 0.032(2) 0.059(3) 0.061(3) -0.009(2) 0.018(2) 0.000(2) C35 0.036(2) 0.071(3) 0.094(4) -0.036(3) 0.034(2) -0.014(2) C36 0.067(2) 0.046(3) 0.122(4) 0.000(3) 0.070(3) 0.008(2) O11 0.116(2) 0.096(2) 0.217(5) 0.089(3) 0.113(3) 0.0676(18) O12 0.0549(17) 0.089(2) 0.077(3) -0.017(2) -0.0068(18) 0.0333(15) C1 0.0279(12) 0.0209(11) 0.0167(16) -0.0014(11) 0.0071(12) 0.0147(9) C2 0.0226(11) 0.0202(11) 0.0203(17) 0.0019(11) 0.0048(11) 0.0132(9) C3 0.0246(11) 0.0272(12) 0.0206(17) 0.0024(12) -0.0019(12) 0.0170(9) C4 0.0279(12) 0.0230(12) 0.0164(16) 0.0060(11) -0.0021(12) 0.0152(9) C5 0.0211(11) 0.0253(12) 0.0198(17) -0.0007(12) 0.0003(12) 0.0124(9) C6 0.0227(12) 0.0270(13) 0.0107(15) 0.0009(11) -0.0016(11) 0.0106(10) C7 0.0186(11) 0.0215(12) 0.0204(16) -0.0012(12) 0.0087(12) 0.0078(9) C8 0.0154(11) 0.0257(13) 0.0222(17) -0.0013(12) -0.0018(12) 0.0075(10) C9 0.0188(12) 0.0251(13) 0.0223(18) -0.0053(12) -0.0009(12) 0.0062(10) C10 0.0144(11) 0.0274(13) 0.0178(17) -0.0040(12) -0.0065(12) 0.0063(10) C11 0.0330(14) 0.0227(13) 0.0243(19) 0.0014(13) 0.0034(14) 0.0126(11) C12 0.0305(14) 0.0216(13) 0.0153(17) -0.0032(12) 0.0011(13) 0.0076(11) C13 0.0336(14) 0.0241(13) 0.0155(17) 0.0036(12) 0.0027(13) 0.0119(11) C14 0.0271(13) 0.0150(12) 0.0204(17) 0.0015(11) 0.0040(13) 0.0066(10) C15 0.0391(15) 0.0222(13) 0.0253(19) 0.0096(13) 0.0084(14) 0.0157(11) C16 0.0278(13) 0.0151(12) 0.0200(17) -0.0027(11) -0.0025(12) 0.0086(10) C17 0.0387(15) 0.0379(15) 0.0157(18) 0.0038(13) -0.0032(14) 0.0202(12) C18 0.0353(14) 0.0191(12) 0.0285(19) 0.0002(12) 0.0034(14) 0.0153(10) C19 0.0192(11) 0.0379(14) 0.0121(16) -0.0020(12) -0.0072(11) 0.0175(9) C20 0.0302(12) 0.0321(12) 0.0132(16) 0.0034(11) 0.0013(12) 0.0226(9) C21 0.0196(11) 0.0265(12) 0.0201(17) -0.0081(12) -0.0066(11) 0.0143(9) C22 0.0315(12) 0.0244(11) 0.0091(15) -0.0030(10) 0.0013(11) 0.0197(9) C23 0.0200(12) 0.0328(14) 0.0123(15) -0.0059(12) -0.0074(11) 0.0132(10) C24 0.0241(11) 0.0298(12) 0.0260(18) -0.0056(12) -0.0003(12) 0.0188(9) C25 0.0166(11) 0.0233(13) 0.0205(17) -0.0066(12) -0.0072(12) 0.0087(9) C26 0.0168(11) 0.0268(13) 0.0233(18) -0.0030(13) -0.0002(12) 0.0088(10) C27 0.0212(12) 0.0205(12) 0.0169(16) 0.0006(11) 0.0024(12) 0.0094(9) C28 0.0146(11) 0.0208(12) 0.0096(14) 0.0010(11) 0.0030(11) 0.0044(9) C29 0.0177(12) 0.0191(12) 0.0195(17) -0.0057(12) -0.0020(12) 0.0051(10) C30 0.0249(12) 0.0238(12) 0.0205(17) 0.0050(12) 0.0057(12) 0.0142(9) N1 0.0215(10) 0.0282(11) 0.0150(14) 0.0027(10) 0.0030(10) 0.0108(8) N2 0.0191(9) 0.0245(10) 0.0207(15) 0.0041(10) 0.0032(10) 0.0127(8) N3 0.0252(10) 0.0246(10) 0.0158(14) 0.0020(10) 0.0015(10) 0.0153(8) N4 0.0225(11) 0.0247(11) 0.0247(17) -0.0009(11) 0.0018(11) 0.0101(9) N5 0.0249(10) 0.0253(11) 0.0130(14) -0.0023(10) -0.0005(10) 0.0128(8) N6 0.0257(11) 0.0195(11) 0.0180(14) -0.0026(10) -0.0009(11) 0.0056(9) N7 0.0260(11) 0.0281(11) 0.0219(15) 0.0001(11) 0.0019(11) 0.0147(9) N8 0.0234(11) 0.0288(12) 0.0285(17) -0.0036(11) -0.0010(11) 0.0122(9) N9 0.0297(12) 0.0274(12) 0.0224(16) -0.0022(11) -0.0005(11) 0.0137(9) N10 0.0308(12) 0.0316(12) 0.0176(15) 0.0004(11) -0.0034(11) 0.0138(9) N11 0.0244(11) 0.0255(11) 0.0163(14) -0.0022(10) 0.0017(10) 0.0113(8) N12 0.0316(11) 0.0279(11) 0.0173(14) -0.0031(10) 0.0012(11) 0.0189(8) N13 0.0319(12) 0.0309(12) 0.0196(15) -0.0040(11) 0.0036(11) 0.0159(9) N14 0.0283(11) 0.0334(11) 0.0109(13) -0.0027(10) -0.0013(10) 0.0188(8) N15 0.0360(12) 0.0202(11) 0.0186(15) -0.0009(10) -0.0045(11) 0.0127(9) N16 0.0239(11) 0.0248(11) 0.0138(14) -0.0058(10) -0.0024(10) 0.0102(8) N17 0.0223(10) 0.0231(10) 0.0119(13) -0.0027(9) -0.0045(10) 0.0130(8) N18 0.0199(10) 0.0157(9) 0.0196(14) -0.0009(9) 0.0006(10) 0.0090(7) N19 0.0256(10) 0.0216(10) 0.0140(13) -0.0020(9) -0.0010(10) 0.0140(8) N20 0.0213(10) 0.0207(10) 0.0167(14) 0.0014(10) 0.0013(10) 0.0099(8) O1 0.0212(8) 0.0326(10) 0.0143(12) -0.0010(8) 0.0049(8) 0.0126(7) O2 0.0288(9) 0.0336(10) 0.0143(12) -0.0023(9) 0.0030(9) 0.0158(7) O3 0.0356(10) 0.0339(10) 0.0226(14) -0.0061(9) -0.0020(10) 0.0171(8) O4 0.0346(9) 0.0382(10) 0.0250(13) -0.0060(10) -0.0026(11) 0.0218(7) O5 0.0312(9) 0.0319(9) 0.0206(13) -0.0006(9) 0.0057(9) 0.0196(7) O7 0.0321(9) 0.0314(9) 0.0271(13) -0.0043(10) 0.0000(10) 0.0198(7) O8 0.0288(9) 0.0320(10) 0.0241(13) -0.0005(9) 0.0029(9) 0.0161(7) O9 0.0264(9) 0.0298(9) 0.0116(11) -0.0007(8) 0.0005(8) 0.0133(7) O10 0.0332(10) 0.0239(9) 0.0193(12) -0.0021(9) -0.0016(9) 0.0137(7) O6 0.0259(9) 0.0280(10) 0.0198(13) -0.0032(9) -0.0014(9) 0.0114(7) N21 0.072(2) 0.082(2) 0.082(4) -0.018(2) -0.027(2) 0.0422(18) O13 0.103(3) 0.132(4) 0.139(4) -0.063(3) -0.080(3) 0.045(3) O14 0.068(2) 0.097(3) 0.205(7) -0.041(4) -0.053(3) 0.018(2) O15 0.177(4) 0.164(4) 0.164(6) -0.024(4) -0.084(4) 0.104(3) N22 0.0787(19) 0.269(5) 0.084(4) -0.063(4) -0.043(2) 0.120(2) O16 0.098(3) 0.131(3) 0.324(9) -0.112(4) -0.060(4) 0.077(2) O17 0.097(3) 0.130(3) 0.325(12) -0.096(5) -0.037(5) 0.075(3) O18 0.069(3) 0.330(11) 0.195(9) 0.073(8) 0.034(4) 0.061(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 O10 2.318(2) 5 ? Dy1 O1 2.318(2) . ? Dy1 O2W 2.333(2) . ? Dy1 O3W 2.337(3) . ? Dy1 O2 2.353(2) . ? Dy1 O1W 2.357(3) . ? Dy1 O4W 2.361(2) . ? Dy1 O9 2.370(2) 5 ? O1W H1WA 0.8500 . ? O1W H1WB 0.8499 . ? O2W H2WA 0.8502 . ? O2W H2WB 0.8500 . ? O3W H3WA 0.8499 . ? O3W H3WB 0.8498 . ? O4W H4WA 0.8499 . ? O4W H4WB 0.8500 . ? O5W H5WA 0.8499 . ? O5W H5WB 0.8500 . ? O6W H6WA 0.8499 . ? O6W H6WB 0.8501 . ? O7W H7WA 0.8498 . ? O7W H7WB 0.8504 . ? O8W H8WA 0.8496 . ? O8W H8WB 0.8500 . ? O9W H9WA 0.8503 . ? O9W H9WB 0.8499 . ? O10W H10A 0.8499 . ? O10W H10B 0.8499 . ? O11W H11C 0.8500 . ? O11W H11D 0.8502 . ? C31 O11 1.353(9) . ? C31 C36 1.359(9) . ? C31 C32 1.382(9) . ? C32 C33 1.402(10) . ? C32 H32 0.9400 . ? C33 C34 1.401(8) . ? C33 H33 0.9400 . ? C34 O12 1.361(8) . ? C34 C35 1.370(9) . ? C35 C36 1.418(10) . ? C35 H35 0.9400 . ? C36 H36 0.9400 . ? O11 H11 0.8300 . ? O12 H12 0.8300 . ? C1 O1 1.238(4) . ? C1 N2 1.350(4) . ? C1 N1 1.368(4) . ? C2 N1 1.439(5) . ? C2 N3 1.457(5) . ? C2 C3 1.584(4) . ? C2 H2A 0.9900 . ? C3 N4 1.447(5) . ? C3 N2 1.483(4) . ? C3 H3A 0.9900 . ? C4 O7 1.193(5) . ? C4 N3 1.362(4) . ? C4 N4 1.381(5) . ? C5 N2 1.425(4) . ? C5 N5 1.447(4) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N4 1.443(4) . ? C6 N7 1.446(5) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O2 1.247(4) . ? C7 N5 1.352(5) . ? C7 N6 1.357(4) . ? C8 N7 1.467(4) . ? C8 N5 1.470(4) . ? C8 C9 1.533(5) . ? C8 H8A 0.9900 . ? C9 N8 1.435(5) . ? C9 N6 1.457(5) . ? C9 H9A 0.9900 . ? C10 O8 1.239(4) . ? C10 N7 1.343(5) . ? C10 N8 1.378(4) . ? C11 N9 1.426(5) . ? C11 N6 1.452(5) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 N11 1.429(5) . ? C12 N8 1.439(5) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 O3 1.222(4) . ? C13 N10 1.371(6) . ? C13 N9 1.372(4) . ? C14 N11 1.440(5) . ? C14 N9 1.485(5) . ? C14 C15 1.549(5) . ? C14 H14A 0.9900 . ? C15 N10 1.442(5) . ? C15 N12 1.448(5) . ? C15 H15A 0.9900 . ? C16 O9 1.221(4) . ? C16 N12 1.358(5) . ? C16 N11 1.375(5) . ? C17 N10 1.438(5) . ? C17 N13 1.466(4) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 N15 1.423(4) . ? C18 N12 1.448(5) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 O4 1.222(5) . ? C19 N13 1.352(5) . ? C19 N14 1.365(4) . ? C20 N13 1.456(5) . ? C20 N15 1.462(4) . ? C20 C21 1.559(4) . ? C20 H20A 0.9900 . ? C21 N14 1.450(5) . ? C21 N16 1.469(5) . ? C21 H21A 0.9900 . ? C22 O10 1.236(4) . ? C22 N15 1.365(4) . ? C22 N16 1.367(4) . ? C23 N14 1.440(4) . ? C23 N17 1.448(5) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 N16 1.414(4) . ? C24 N19 1.455(5) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C25 O5 1.217(4) . ? C25 N17 1.366(5) . ? C25 N18 1.374(5) . ? C26 N19 1.431(4) . ? C26 N17 1.462(4) . ? C26 C27 1.555(5) . ? C26 H26A 0.9900 . ? C27 N18 1.447(4) . ? C27 N20 1.479(4) . ? C27 H27A 0.9900 . ? C28 O6 1.233(4) . ? C28 N20 1.350(5) . ? C28 N19 1.381(4) . ? C29 N18 1.432(5) . ? C29 N1 1.452(4) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C30 N3 1.439(4) . ? C30 N20 1.442(5) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? O9 Dy1 2.370(2) 6_554 ? O10 Dy1 2.318(2) 6_554 ? N21 O14 1.250(5) . ? N21 O13 1.258(5) . ? N21 O15 1.264(5) . ? N22 O17 1.251(6) . ? N22 O16 1.282(6) . ? N22 O18 1.315(6) . ? O19 N23 1.287(7) . ? N23 O20 1.259(7) . ? N23 O21 1.292(6) . ? 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 O10 Dy1 O1 135.44(8) 5 . ? O10 Dy1 O2W 80.05(10) 5 . ? O1 Dy1 O2W 114.91(10) . . ? O10 Dy1 O3W 115.99(9) 5 . ? O1 Dy1 O3W 79.82(10) . . ? O2W Dy1 O3W 140.69(8) . . ? O10 Dy1 O2 146.30(9) 5 . ? O1 Dy1 O2 75.22(8) . . ? O2W Dy1 O2 72.18(9) . . ? O3W Dy1 O2 77.57(9) . . ? O10 Dy1 O1W 74.87(9) 5 . ? O1 Dy1 O1W 72.03(9) . . ? O2W Dy1 O1W 70.63(8) . . ? O3W Dy1 O1W 146.05(8) . . ? O2 Dy1 O1W 111.99(9) . . ? O10 Dy1 O4W 72.34(10) 5 . ? O1 Dy1 O4W 74.59(8) . . ? O2W Dy1 O4W 145.71(10) . . ? O3W Dy1 O4W 71.70(10) . . ? O2 Dy1 O4W 139.94(10) . . ? O1W Dy1 O4W 82.65(10) . . ? O10 Dy1 O9 75.37(8) 5 5 ? O1 Dy1 O9 146.69(8) . 5 ? O2W Dy1 O9 77.38(10) . 5 ? O3W Dy1 O9 73.18(9) . 5 ? O2 Dy1 O9 80.16(8) . 5 ? O1W Dy1 O9 139.28(8) . 5 ? O4W Dy1 O9 113.60(10) . 5 ? Dy1 O1W H1WA 113.1 . . ? Dy1 O1W H1WB 137.0 . . ? H1WA O1W H1WB 108.7 . . ? Dy1 O2W H2WA 111.5 . . ? Dy1 O2W H2WB 124.8 . . ? H2WA O2W H2WB 108.7 . . ? Dy1 O3W H3WA 123.7 . . ? Dy1 O3W H3WB 107.7 . . ? H3WA O3W H3WB 108.7 . . ? Dy1 O4W H4WA 114.4 . . ? Dy1 O4W H4WB 133.4 . . ? H4WA O4W H4WB 108.7 . . ? H5WA O5W H5WB 107.6 . . ? H6WA O6W H6WB 109.0 . . ? H7WA O7W H7WB 109.0 . . ? H8WA O8W H8WB 108.5 . . ? H9WA O9W H9WB 108.4 . . ? H10A O10W H10B 108.6 . . ? H11C O11W H11D 107.7 . . ? O11 C31 C36 117.3(6) . . ? O11 C31 C32 122.1(6) . . ? C36 C31 C32 120.6(7) . . ? C31 C32 C33 118.6(6) . . ? C31 C32 H32 120.7 . . ? C33 C32 H32 120.7 . . ? C34 C33 C32 121.8(6) . . ? C34 C33 H33 119.1 . . ? C32 C33 H33 119.1 . . ? O12 C34 C35 118.5(5) . . ? O12 C34 C33 123.4(5) . . ? C35 C34 C33 118.0(6) . . ? C34 C35 C36 120.4(6) . . ? C34 C35 H35 119.8 . . ? C36 C35 H35 119.8 . . ? C31 C36 C35 120.6(6) . . ? C31 C36 H36 119.7 . . ? C35 C36 H36 119.7 . . ? C31 O11 H11 109.5 . . ? C34 O12 H12 109.5 . . ? O1 C1 N2 126.1(3) . . ? O1 C1 N1 123.9(3) . . ? N2 C1 N1 110.0(3) . . ? N1 C2 N3 114.9(3) . . ? N1 C2 C3 104.0(2) . . ? N3 C2 C3 101.9(2) . . ? N1 C2 H2A 111.8 . . ? N3 C2 H2A 111.8 . . ? C3 C2 H2A 111.8 . . ? N4 C3 N2 115.0(3) . . ? N4 C3 C2 103.0(3) . . ? N2 C3 C2 101.4(2) . . ? N4 C3 H3A 112.2 . . ? N2 C3 H3A 112.2 . . ? C2 C3 H3A 112.2 . . ? O7 C4 N3 126.6(3) . . ? O7 C4 N4 125.7(3) . . ? N3 C4 N4 107.6(3) . . ? N2 C5 N5 113.7(3) . . ? N2 C5 H5A 108.8 . . ? N5 C5 H5A 108.8 . . ? N2 C5 H5B 108.8 . . ? N5 C5 H5B 108.8 . . ? H5A C5 H5B 107.7 . . ? N4 C6 N7 114.4(3) . . ? N4 C6 H6A 108.7 . . ? N7 C6 H6A 108.7 . . ? N4 C6 H6B 108.7 . . ? N7 C6 H6B 108.7 . . ? H6A C6 H6B 107.6 . . ? O2 C7 N5 126.5(3) . . ? O2 C7 N6 124.2(3) . . ? N5 C7 N6 109.3(3) . . ? N7 C8 N5 114.2(2) . . ? N7 C8 C9 104.2(3) . . ? N5 C8 C9 102.4(3) . . ? N7 C8 H8A 111.8 . . ? N5 C8 H8A 111.8 . . ? C9 C8 H8A 111.8 . . ? N8 C9 N6 115.7(3) . . ? N8 C9 C8 102.8(3) . . ? N6 C9 C8 104.1(3) . . ? N8 C9 H9A 111.2 . . ? N6 C9 H9A 111.2 . . ? C8 C9 H9A 111.2 . . ? O8 C10 N7 125.9(3) . . ? O8 C10 N8 124.7(4) . . ? N7 C10 N8 109.4(3) . . ? N9 C11 N6 113.2(3) . . ? N9 C11 H11A 108.9 . . ? N6 C11 H11A 108.9 . . ? N9 C11 H11B 108.9 . . ? N6 C11 H11B 108.9 . . ? H11A C11 H11B 107.7 . . ? N11 C12 N8 114.2(3) . . ? N11 C12 H12A 108.7 . . ? N8 C12 H12A 108.7 . . ? N11 C12 H12B 108.7 . . ? N8 C12 H12B 108.7 . . ? H12A C12 H12B 107.6 . . ? O3 C13 N10 126.2(3) . . ? O3 C13 N9 125.0(4) . . ? N10 C13 N9 108.7(3) . . ? N11 C14 N9 115.3(3) . . ? N11 C14 C15 105.1(3) . . ? N9 C14 C15 102.0(3) . . ? N11 C14 H14A 111.3 . . ? N9 C14 H14A 111.3 . . ? C15 C14 H14A 111.3 . . ? N10 C15 N12 114.6(2) . . ? N10 C15 C14 104.7(3) . . ? N12 C15 C14 101.7(3) . . ? N10 C15 H15A 111.7 . . ? N12 C15 H15A 111.7 . . ? C14 C15 H15A 111.7 . . ? O9 C16 N12 126.7(3) . . ? O9 C16 N11 124.7(3) . . ? N12 C16 N11 108.7(3) . . ? N10 C17 N13 113.0(3) . . ? N10 C17 H17A 109.0 . . ? N13 C17 H17A 109.0 . . ? N10 C17 H17B 109.0 . . ? N13 C17 H17B 109.0 . . ? H17A C17 H17B 107.8 . . ? N15 C18 N12 111.7(3) . . ? N15 C18 H18A 109.3 . . ? N12 C18 H18A 109.3 . . ? N15 C18 H18B 109.3 . . ? N12 C18 H18B 109.3 . . ? H18A C18 H18B 107.9 . . ? O4 C19 N13 125.6(3) . . ? O4 C19 N14 124.9(3) . . ? N13 C19 N14 109.3(3) . . ? N13 C20 N15 115.1(3) . . ? N13 C20 C21 103.2(3) . . ? N15 C20 C21 103.1(3) . . ? N13 C20 H20A 111.6 . . ? N15 C20 H20A 111.6 . . ? C21 C20 H20A 111.6 . . ? N14 C21 N16 114.9(3) . . ? N14 C21 C20 102.9(3) . . ? N16 C21 C20 103.9(2) . . ? N14 C21 H21A 111.5 . . ? N16 C21 H21A 111.5 . . ? C20 C21 H21A 111.5 . . ? O10 C22 N15 125.4(3) . . ? O10 C22 N16 124.1(3) . . ? N15 C22 N16 110.5(3) . . ? N14 C23 N17 114.0(2) . . ? N14 C23 H23A 108.8 . . ? N17 C23 H23A 108.8 . . ? N14 C23 H23B 108.8 . . ? N17 C23 H23B 108.8 . . ? H23A C23 H23B 107.7 . . ? N16 C24 N19 114.1(3) . . ? N16 C24 H24A 108.7 . . ? N19 C24 H24A 108.7 . . ? N16 C24 H24B 108.7 . . ? N19 C24 H24B 108.7 . . ? H24A C24 H24B 107.6 . . ? O5 C25 N17 125.4(3) . . ? O5 C25 N18 126.3(4) . . ? N17 C25 N18 108.3(3) . . ? N19 C26 N17 114.9(2) . . ? N19 C26 C27 103.3(3) . . ? N17 C26 C27 103.2(3) . . ? N19 C26 H26A 111.6 . . ? N17 C26 H26A 111.6 . . ? C27 C26 H26A 111.6 . . ? N18 C27 N20 115.1(2) . . ? N18 C27 C26 102.9(3) . . ? N20 C27 C26 102.9(3) . . ? N18 C27 H27A 111.7 . . ? N20 C27 H27A 111.7 . . ? C26 C27 H27A 111.7 . . ? O6 C28 N20 124.7(3) . . ? O6 C28 N19 126.1(3) . . ? N20 C28 N19 109.1(3) . . ? N18 C29 N1 114.3(3) . . ? N18 C29 H29A 108.7 . . ? N1 C29 H29A 108.7 . . ? N18 C29 H29B 108.7 . . ? N1 C29 H29B 108.7 . . ? H29A C29 H29B 107.6 . . ? N3 C30 N20 114.6(3) . . ? N3 C30 H30A 108.6 . . ? N20 C30 H30A 108.6 . . ? N3 C30 H30B 108.6 . . ? N20 C30 H30B 108.6 . . ? H30A C30 H30B 107.6 . . ? C1 N1 C2 112.2(3) . . ? C1 N1 C29 121.3(3) . . ? C2 N1 C29 124.3(2) . . ? C1 N2 C5 123.2(3) . . ? C1 N2 C3 112.3(2) . . ? C5 N2 C3 124.4(3) . . ? C4 N3 C30 122.1(3) . . ? C4 N3 C2 114.0(3) . . ? C30 N3 C2 123.0(2) . . ? C4 N4 C6 121.4(3) . . ? C4 N4 C3 113.3(2) . . ? C6 N4 C3 124.8(3) . . ? C7 N5 C5 125.4(3) . . ? C7 N5 C8 112.2(3) . . ? C5 N5 C8 122.0(3) . . ? C7 N6 C11 123.0(3) . . ? C7 N6 C9 111.5(3) . . ? C11 N6 C9 123.5(3) . . ? C10 N7 C6 122.6(3) . . ? C10 N7 C8 110.2(3) . . ? C6 N7 C8 123.5(3) . . ? C10 N8 C9 112.1(3) . . ? C10 N8 C12 121.9(3) . . ? C9 N8 C12 125.9(3) . . ? C13 N9 C11 122.7(3) . . ? C13 N9 C14 111.9(3) . . ? C11 N9 C14 125.4(3) . . ? C13 N10 C17 120.9(3) . . ? C13 N10 C15 111.9(3) . . ? C17 N10 C15 124.6(4) . . ? C16 N11 C12 122.5(3) . . ? C16 N11 C14 110.7(3) . . ? C12 N11 C14 125.2(3) . . ? C16 N12 C18 125.0(3) . . ? C16 N12 C15 113.4(3) . . ? C18 N12 C15 121.6(3) . . ? C19 N13 C20 112.2(2) . . ? C19 N13 C17 123.0(3) . . ? C20 N13 C17 124.5(3) . . ? C19 N14 C23 123.7(3) . . ? C19 N14 C21 112.3(3) . . ? C23 N14 C21 123.6(3) . . ? C22 N15 C18 122.4(3) . . ? C22 N15 C20 111.7(2) . . ? C18 N15 C20 125.7(3) . . ? C22 N16 C24 122.4(3) . . ? C22 N16 C21 110.7(2) . . ? C24 N16 C21 125.5(2) . . ? C25 N17 C23 121.4(3) . . ? C25 N17 C26 112.0(3) . . ? C23 N17 C26 122.9(3) . . ? C25 N18 C29 123.2(3) . . ? C25 N18 C27 112.8(3) . . ? C29 N18 C27 122.9(3) . . ? C28 N19 C26 112.6(3) . . ? C28 N19 C24 123.0(3) . . ? C26 N19 C24 123.9(3) . . ? C28 N20 C30 121.6(3) . . ? C28 N20 C27 111.3(3) . . ? C30 N20 C27 122.9(3) . . ? C1 O1 Dy1 150.2(2) . . ? C7 O2 Dy1 148.3(2) . . ? C16 O9 Dy1 150.8(2) . 6_554 ? C22 O10 Dy1 155.3(2) . 6_554 ? O14 N21 O13 122.6(5) . . ? O14 N21 O15 118.9(5) . . ? O13 N21 O15 118.1(4) . . ? O17 N22 O16 121.7(5) . . ? O17 N22 O18 120.0(6) . . ? O16 N22 O18 118.4(5) . . ? O20 N23 O19 109.3(6) . . ? O20 N23 O21 125.1(8) . . ? O19 N23 O21 117.1(8) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.664 _refine_diff_density_min -0.747 _refine_diff_density_rms 0.134 # Attachment 'compound1.cif' data_k _database_code_depnum_ccdc_archive 'CCDC 820006' #TrackingRef 'compound1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common compound1 _chemical_melting_point 'not measured' _chemical_formula_moiety 'C30 H38 Dy N20 O14 2(N O3) Cl 7(H2O)' _chemical_formula_sum 'C30 H52 Cl Dy N22 O27' _chemical_formula_weight 1350.89 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.473(2) _cell_length_b 22.512(3) _cell_length_c 16.595(3) _cell_angle_alpha 90.00 _cell_angle_beta 101.605(4) _cell_angle_gamma 90.00 _cell_volume 5296.5(14) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 8892 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 26.31 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.694 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2740 _exptl_absorpt_coefficient_mu 1.568 _exptl_absorpt_correction_type 'multi scan' _exptl_absorpt_correction_T_min 0.6257 _exptl_absorpt_correction_T_max 0.7143 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 43820 _diffrn_reflns_av_R_equivalents 0.0800 _diffrn_reflns_av_sigmaI/netI 0.0775 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 26.00 _reflns_number_total 10146 _reflns_number_gt 6803 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.1329P)^2^+27.5997P] 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 10146 _refine_ls_number_parameters 739 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.1183 _refine_ls_R_factor_gt 0.0776 _refine_ls_wR_factor_ref 0.2412 _refine_ls_wR_factor_gt 0.2123 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 0.067 _refine_ls_shift/su_mean 0.005 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 0.810665(18) 0.169033(12) 0.664638(15) 0.03467(7) Uani 1 1 d . . . O1W O 0.7546(3) 0.0752(2) 0.6925(3) 0.0595(14) Uani 1 1 d . . . H1WA H 0.7119 0.0683 0.7197 0.071 Uiso 1 1 d R . . H1WB H 0.7959 0.0480 0.7034 0.071 Uiso 1 1 d R . . O2W O 0.9420(3) 0.22951(19) 0.6754(3) 0.0482(12) Uani 1 1 d . . . H2WA H 0.9368 0.2658 0.6878 0.058 Uiso 1 1 d R . . H2WB H 0.9972 0.2177 0.6970 0.058 Uiso 1 1 d R . . O3W O 0.6458(3) 0.17590(19) 0.6533(3) 0.0487(12) Uani 1 1 d . . . H3WA H 0.6205 0.2100 0.6452 0.058 Uiso 1 1 d R . . H3WB H 0.6115 0.1510 0.6224 0.058 Uiso 1 1 d R . . O4W O 0.9261(3) 0.1091(2) 0.6211(3) 0.0598(14) Uani 1 1 d . . . H4WA H 0.9243 0.0937 0.5741 0.072 Uiso 1 1 d R . . H4WB H 0.9152 0.0818 0.6535 0.072 Uiso 1 1 d R . . O5W O 0.7028(5) -0.0610(2) 0.2604(5) 0.155(3) Uani 1 1 d D . . H5WA H 0.7223 -0.0995 0.2856 0.186 Uiso 1 1 calc R . . H5WB H 0.7369 -0.0268 0.2885 0.186 Uiso 1 1 calc R . . O6W O 0.1357(4) 0.4606(3) 0.2871(5) 0.181(3) Uani 1 1 d . . . H6WA H 0.1978 0.4689 0.3215 0.217 Uiso 1 1 calc R . . H6WB H 0.0826 0.4825 0.3011 0.217 Uiso 1 1 calc R . . O7W O 0.1055(6) 0.1985(6) 0.5554(4) 0.204(5) Uani 1 1 d . . . H7WA H 0.1651 0.1927 0.5949 0.245 Uiso 1 1 calc R . . H7WB H 0.0527 0.2168 0.5750 0.245 Uiso 1 1 calc R . . Cl1 Cl 0.9149(8) 0.0456(5) 0.4744(7) 0.220(5) Uani 0.50 1 d P . . Cl1' Cl 0.8554(7) -0.0042(5) 0.5345(9) 0.257(6) Uani 0.50 1 d P . . O8W O 0.0600(4) 0.3077(5) 0.3692(5) 0.181(5) Uani 1 1 d D . . H8WA H 0.1207 0.3142 0.4067 0.217 Uiso 1 1 calc R . . H8WB H 0.0038 0.3237 0.3859 0.217 Uiso 1 1 calc R . . O9W O 0.5240(6) 0.2994(5) 0.7988(4) 0.160(4) Uani 1 1 d . . . H9WA H 0.5758 0.2787 0.8351 0.191 Uiso 1 1 calc R . . H9WB H 0.4957 0.3337 0.8210 0.191 Uiso 1 1 calc R . . O10W O 0.4528(6) 0.1167(4) 0.7541(6) 0.269(9) Uani 1 1 d D . . H10C H 0.4873 0.0853 0.7885 0.323 Uiso 1 1 calc R . . H10D H 0.4409 0.1541 0.7805 0.323 Uiso 1 1 calc R . . O11W O 1.0084(12) 0.6403(8) 0.4786(7) 0.287(8) Uani 1 1 d . . . H11B H 1.0704 0.6272 0.5086 0.344 Uiso 1 1 calc R . . H11C H 0.9869 0.6791 0.4940 0.344 Uiso 1 1 calc R . . O1 O 0.7502(3) 0.13494(18) 0.5318(2) 0.0439(12) Uani 1 1 d . . . O2 O 0.7704(3) 0.25435(16) 0.5818(2) 0.0360(10) Uani 1 1 d . . . O3 O 0.5803(3) 0.29852(18) 0.6417(2) 0.0423(11) Uani 1 1 d . . . O4 O 0.4419(3) 0.19081(19) 0.6199(2) 0.0494(13) Uani 1 1 d . . . O5 O 0.5489(3) 0.08120(17) 0.5589(2) 0.0496(13) Uani 1 1 d . . . O6 O 0.3970(3) 0.15452(19) 0.2018(2) 0.0491(13) Uani 1 1 d . . . O7 O 0.6015(3) 0.1924(2) 0.1728(2) 0.0505(13) Uani 1 1 d . . . O8 O 0.6097(3) 0.32468(17) 0.2335(2) 0.0408(11) Uani 1 1 d . . . O9 O 0.4156(3) 0.36514(17) 0.2858(2) 0.0400(11) Uani 1 1 d . . . O10 O 0.2834(3) 0.26550(18) 0.2677(2) 0.0438(11) Uani 1 1 d D . . N1 N 0.6995(3) 0.0913(2) 0.4047(3) 0.0389(13) Uani 1 1 d . . . N2 N 0.8041(3) 0.1652(2) 0.4173(3) 0.0392(13) Uani 1 1 d . . . N3 N 0.8217(3) 0.2675(2) 0.4578(3) 0.0424(14) Uani 1 1 d . . . N4 N 0.7376(3) 0.3377(2) 0.5015(3) 0.0378(13) Uani 1 1 d . . . N5 N 0.5921(3) 0.3672(2) 0.5417(3) 0.0360(13) Uani 1 1 d . . . N6 N 0.4492(3) 0.3411(2) 0.5574(3) 0.0372(13) Uani 1 1 d . . . N7 N 0.3404(3) 0.2586(2) 0.5439(3) 0.0407(14) Uani 1 1 d . . . N8 N 0.3329(4) 0.1646(2) 0.5033(3) 0.0455(15) Uani 1 1 d . . . N9 N 0.4147(4) 0.0811(2) 0.4583(3) 0.0461(15) Uani 1 1 d . . . N10 N 0.5480(4) 0.0544(2) 0.4247(3) 0.0452(15) Uani 1 1 d . . . N11 N 0.4880(4) 0.0847(2) 0.2810(3) 0.0476(15) Uani 1 1 d . . . N12 N 0.3542(4) 0.1124(2) 0.3151(3) 0.0441(14) Uani 1 1 d . . . N13 N 0.2705(3) 0.1943(2) 0.3615(3) 0.0387(13) Uani 1 1 d . . . N14 N 0.2750(3) 0.2886(2) 0.3999(3) 0.0381(13) Uani 1 1 d . . . N15 N 0.3822(3) 0.3706(2) 0.4157(3) 0.0361(13) Uani 1 1 d . . . N16 N 0.5250(3) 0.39490(19) 0.3980(3) 0.0337(12) Uani 1 1 d . . . N17 N 0.6695(3) 0.3664(2) 0.3596(3) 0.0368(13) Uani 1 1 d . . . N18 N 0.7485(3) 0.2925(2) 0.3153(3) 0.0373(13) Uani 1 1 d . . . N19 N 0.7396(4) 0.1903(2) 0.2713(3) 0.0429(14) Uani 1 1 d . . . N20 N 0.6405(3) 0.1133(2) 0.2580(3) 0.0410(13) Uani 1 1 d . . . N21 N 0.9076(6) -0.0224(3) 0.8144(4) 0.090(3) Uani 1 1 d . . . N22 N 0.7736(4) 0.5592(4) 0.4070(4) 0.229(2) Uani 1 1 d D . . O11 O 0.8779(8) -0.0175(4) 0.7390(6) 0.165(4) Uani 1 1 d . . . O12 O 0.9830(6) -0.0415(4) 0.8415(6) 0.191(4) Uani 1 1 d . . . O13 O 0.8632(6) -0.0020(3) 0.8646(5) 0.124(3) Uani 1 1 d . . . O14 O 0.7070(5) 0.5585(4) 0.3461(4) 0.228(6) Uani 1 1 d D . . O15 O 0.7670(7) 0.5309(4) 0.4697(4) 0.249(8) Uani 1 1 d D . . O16 O 0.8403(6) 0.5938(5) 0.4072(12) 0.240(17) Uani 1 1 d D . . C1 C 0.7517(4) 0.1311(3) 0.4571(4) 0.0429(16) Uani 1 1 d . . . C2 C 0.8668(4) 0.2107(3) 0.4560(4) 0.0451(17) Uani 1 1 d . . . H2A H 0.9187 0.2148 0.4265 0.054 Uiso 1 1 calc R . . H2B H 0.8939 0.1986 0.5125 0.054 Uiso 1 1 calc R . . C3 C 0.7748(4) 0.2836(3) 0.5191(3) 0.0370(15) Uani 1 1 d . . . C4 C 0.6934(4) 0.3718(2) 0.5588(3) 0.0345(14) Uani 1 1 d . . . H4A H 0.7180 0.3578 0.6149 0.041 Uiso 1 1 calc R . . H4B H 0.7110 0.4137 0.5562 0.041 Uiso 1 1 calc R . . C5 C 0.5444(4) 0.3316(2) 0.5858(3) 0.0344(14) Uani 1 1 d . . . C6 C 0.3770(4) 0.3100(3) 0.5895(3) 0.0408(16) Uani 1 1 d . . . H6A H 0.4031 0.2982 0.6463 0.049 Uiso 1 1 calc R . . H6B H 0.3248 0.3376 0.5907 0.049 Uiso 1 1 calc R . . C7 C 0.3780(4) 0.2025(3) 0.5603(4) 0.0422(16) Uani 1 1 d . . . C8 C 0.3496(5) 0.1015(3) 0.5096(4) 0.0474(18) Uani 1 1 d . . . H8A H 0.2893 0.0806 0.4931 0.057 Uiso 1 1 calc R . . H8B H 0.3756 0.0913 0.5671 0.057 Uiso 1 1 calc R . . C9 C 0.5077(5) 0.0736(2) 0.4869(4) 0.0440(17) Uani 1 1 d . . . C10 C 0.6496(5) 0.0442(3) 0.4334(4) 0.0516(19) Uani 1 1 d . . . H10A H 0.6769 0.0373 0.4916 0.062 Uiso 1 1 calc R . . H10B H 0.6590 0.0080 0.4032 0.062 Uiso 1 1 calc R . . C11 C 0.4788(5) 0.0450(2) 0.3488(3) 0.0436(17) Uani 1 1 d . . . H11A H 0.4770 0.0028 0.3315 0.052 Uiso 1 1 calc R . . C12 C 0.3846(5) 0.0641(3) 0.3702(3) 0.0484(18) Uani 1 1 d . . . H12A H 0.3381 0.0313 0.3627 0.058 Uiso 1 1 calc R . . C13 C 0.2554(4) 0.1914(3) 0.4456(3) 0.0437(16) Uani 1 1 d . . . H13A H 0.1939 0.1732 0.4487 0.052 Uiso 1 1 calc R . . C14 C 0.2616(4) 0.2573(3) 0.4733(3) 0.0395(16) Uani 1 1 d . . . H14A H 0.2024 0.2700 0.4895 0.047 Uiso 1 1 calc R . . C15 C 0.4303(4) 0.3887(2) 0.4990(3) 0.0344(14) Uani 1 1 d . . . H15A H 0.3979 0.4224 0.5199 0.041 Uiso 1 1 calc R . . C16 C 0.5302(4) 0.4062(2) 0.4859(3) 0.0347(14) Uani 1 1 d . . . H16A H 0.5442 0.4485 0.4997 0.042 Uiso 1 1 calc R . . C17 C 0.7543(4) 0.3610(3) 0.4243(3) 0.0379(15) Uani 1 1 d . . . H17A H 0.7906 0.3985 0.4323 0.046 Uiso 1 1 calc R . . C18 C 0.8099(4) 0.3111(3) 0.3929(4) 0.0388(16) Uani 1 1 d . . . H18A H 0.8716 0.3255 0.3837 0.047 Uiso 1 1 calc R . . C19 C 0.7916(4) 0.1477(3) 0.3302(3) 0.0425(16) Uani 1 1 d . . . H19A H 0.8520 0.1359 0.3156 0.051 Uiso 1 1 calc R . . C20 C 0.7215(5) 0.0940(2) 0.3246(3) 0.0453(17) Uani 1 1 d D . . H20A H 0.7503 0.0566 0.3102 0.054 Uiso 1 1 calc R . . C21 C 0.6555(4) 0.1673(3) 0.2301(3) 0.0412(16) Uani 1 1 d . . . C22 C 0.5603(4) 0.0779(3) 0.2313(3) 0.0462(18) Uani 1 1 d . . . H22A H 0.5797 0.0361 0.2326 0.055 Uiso 1 1 calc R . . H22B H 0.5327 0.0880 0.1741 0.055 Uiso 1 1 calc R . . C23 C 0.4126(4) 0.1213(3) 0.2607(3) 0.0418(16) Uani 1 1 d . . . C24 C 0.2645(4) 0.1436(3) 0.3080(4) 0.0446(17) Uani 1 1 d . . . H24A H 0.2430 0.1566 0.2510 0.053 Uiso 1 1 calc R . . H24B H 0.2173 0.1159 0.3211 0.053 Uiso 1 1 calc R . . C25 C 0.2852(4) 0.3506(2) 0.3942(4) 0.0368(15) Uani 1 1 d . . . H25A H 0.2489 0.3700 0.4307 0.044 Uiso 1 1 calc R . . H25B H 0.2584 0.3631 0.3378 0.044 Uiso 1 1 calc R . . C26 C 0.5975(4) 0.4110(2) 0.3563(3) 0.0361(15) Uani 1 1 d . . . H26A H 0.6270 0.4478 0.3804 0.043 Uiso 1 1 calc R . . H26B H 0.5693 0.4191 0.2986 0.043 Uiso 1 1 calc R . . C27 C 0.4397(4) 0.3754(2) 0.3606(3) 0.0329(14) Uani 1 1 d . . . C28 C 0.2772(4) 0.2511(2) 0.3367(3) 0.0326(14) Uani 1 1 d . . . C29 C 0.6700(4) 0.3271(2) 0.2970(3) 0.0333(14) Uani 1 1 d . . . C30 C 0.7716(4) 0.2494(3) 0.2580(4) 0.0429(17) Uani 1 1 d . . . H30A H 0.7432 0.2618 0.2019 0.051 Uiso 1 1 calc R . . H30B H 0.8402 0.2486 0.2628 0.051 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 0.03393(12) 0.03673(14) 0.02746(12) -0.00547(11) -0.00787(10) 0.00197(12) O1W 0.061(3) 0.046(2) 0.064(3) -0.003(2) -0.005(2) -0.015(2) O2W 0.0314(19) 0.048(2) 0.056(2) 0.005(2) -0.0117(19) -0.0004(18) O3W 0.038(2) 0.058(3) 0.045(2) -0.009(2) -0.0048(19) -0.004(2) O4W 0.065(3) 0.073(3) 0.037(2) -0.009(2) 0.000(2) 0.030(2) O5W 0.147(6) 0.062(3) 0.255(8) -0.077(4) 0.040(6) 0.036(4) O6W 0.220(6) 0.231(7) 0.104(5) 0.073(5) 0.065(5) 0.168(5) O7W 0.138(5) 0.398(13) 0.098(4) -0.110(6) 0.075(4) -0.097(7) Cl1 0.217(9) 0.206(9) 0.226(10) -0.037(8) 0.015(8) 0.064(8) Cl1' 0.133(6) 0.177(8) 0.407(15) -0.106(9) -0.069(8) 0.020(6) O8W 0.101(6) 0.255(11) 0.170(9) 0.010(9) -0.010(6) 0.051(7) O9W 0.107(5) 0.298(12) 0.073(4) 0.025(6) 0.017(4) 0.002(7) O10W 0.52(2) 0.179(10) 0.099(6) 0.052(6) 0.044(10) 0.056(13) O11W 0.295(15) 0.41(2) 0.110(7) 0.055(11) -0.068(9) -0.003(16) O1 0.049(2) 0.049(2) 0.0271(18) -0.0043(17) -0.0084(18) -0.004(2) O2 0.0404(19) 0.034(2) 0.0286(18) -0.0009(16) -0.0040(16) 0.0046(17) O3 0.046(2) 0.042(2) 0.036(2) -0.0002(18) 0.0008(18) 0.0014(19) O4 0.062(3) 0.041(2) 0.039(2) 0.0091(18) -0.005(2) -0.002(2) O5 0.081(3) 0.030(2) 0.0307(19) 0.0013(17) -0.004(2) -0.009(2) O6 0.060(3) 0.046(2) 0.036(2) 0.0079(18) -0.002(2) -0.001(2) O7 0.058(3) 0.048(2) 0.038(2) 0.0056(19) -0.010(2) 0.006(2) O8 0.041(2) 0.044(2) 0.0350(19) 0.0022(17) 0.0034(17) -0.0023(18) O9 0.044(2) 0.040(2) 0.0321(19) -0.0003(17) -0.0016(17) -0.0007(18) O10 0.045(2) 0.046(2) 0.035(2) 0.0063(18) -0.0071(18) -0.0073(19) N1 0.056(3) 0.029(2) 0.024(2) -0.0019(19) -0.010(2) -0.004(2) N2 0.040(2) 0.043(3) 0.029(2) -0.002(2) -0.008(2) 0.006(2) N3 0.046(3) 0.047(3) 0.033(2) 0.005(2) 0.007(2) 0.008(2) N4 0.040(2) 0.040(3) 0.030(2) 0.002(2) -0.003(2) 0.003(2) N5 0.040(2) 0.032(2) 0.033(2) -0.0012(19) 0.002(2) -0.002(2) N6 0.042(2) 0.039(3) 0.028(2) 0.0023(19) 0.002(2) 0.001(2) N7 0.035(2) 0.038(3) 0.043(3) 0.006(2) -0.004(2) -0.002(2) N8 0.060(3) 0.035(3) 0.038(3) 0.006(2) 0.000(2) -0.006(2) N9 0.062(3) 0.040(3) 0.029(2) -0.001(2) -0.007(2) -0.007(2) N10 0.065(3) 0.032(3) 0.031(2) -0.001(2) -0.007(2) -0.006(2) N11 0.066(3) 0.035(3) 0.037(3) 0.004(2) -0.002(2) -0.002(2) N12 0.059(3) 0.038(3) 0.031(2) 0.009(2) -0.001(2) -0.009(2) N13 0.036(2) 0.044(3) 0.031(2) 0.002(2) -0.005(2) -0.008(2) N14 0.037(2) 0.040(3) 0.037(2) 0.005(2) 0.007(2) -0.003(2) N15 0.032(2) 0.041(3) 0.031(2) 0.008(2) -0.0032(19) -0.002(2) N16 0.036(2) 0.028(2) 0.034(2) -0.0037(19) -0.0001(19) -0.0008(19) N17 0.033(2) 0.034(3) 0.042(2) 0.000(2) 0.005(2) 0.000(2) N18 0.038(2) 0.034(2) 0.039(2) -0.004(2) 0.006(2) 0.002(2) N19 0.048(3) 0.038(3) 0.034(2) -0.004(2) -0.011(2) 0.009(2) N20 0.045(3) 0.035(3) 0.033(2) -0.004(2) -0.013(2) 0.007(2) N21 0.110(5) 0.068(4) 0.081(4) 0.045(3) -0.006(4) 0.000(4) N22 0.148(14) 0.34(2) 0.178(23) 0.127(14) 0.012(11) -0.024(14) O11 0.255(10) 0.095(5) 0.125(6) 0.018(5) -0.008(7) 0.059(6) O12 0.117(6) 0.213(7) 0.222(7) 0.154(6) -0.015(6) -0.025(6) O13 0.157(7) 0.091(5) 0.119(5) 0.038(4) 0.014(5) -0.001(5) O14 0.285(12) 0.215(14) 0.240(12) -0.073(10) 0.187(8) -0.077(11) O15 0.204(10) 0.170(11) 0.41(2) -0.087(13) 0.117(12) 0.033(9) O16 0.26(3) 0.22(2) 0.217(4) -0.06(2) -0.03(3) -0.01(2) C1 0.043(3) 0.034(3) 0.041(3) -0.011(2) -0.018(3) 0.015(3) C2 0.029(3) 0.059(4) 0.043(3) -0.006(3) -0.003(2) 0.011(3) C3 0.026(2) 0.036(3) 0.042(3) -0.011(2) -0.011(2) 0.000(2) C4 0.030(2) 0.035(3) 0.034(3) -0.011(2) -0.006(2) -0.006(2) C5 0.038(3) 0.030(3) 0.029(3) -0.005(2) -0.009(2) 0.001(2) C6 0.049(3) 0.046(3) 0.029(3) -0.003(2) 0.011(2) 0.003(3) C7 0.054(3) 0.034(3) 0.039(3) 0.006(2) 0.011(3) -0.010(3) C8 0.063(4) 0.036(3) 0.039(3) 0.012(3) 0.002(3) -0.011(3) C9 0.065(4) 0.016(2) 0.043(3) 0.002(2) -0.008(3) -0.019(3) C10 0.079(4) 0.027(3) 0.037(3) -0.002(3) -0.015(3) 0.009(3) C11 0.070(4) 0.021(3) 0.032(3) -0.005(2) -0.008(3) -0.013(3) C12 0.073(4) 0.036(3) 0.031(3) 0.005(2) -0.001(3) -0.014(3) C13 0.041(3) 0.054(3) 0.035(3) 0.013(3) 0.005(2) -0.010(3) C14 0.037(3) 0.047(3) 0.033(3) 0.010(2) 0.004(2) -0.002(3) C15 0.043(3) 0.024(3) 0.034(3) -0.001(2) -0.001(2) 0.005(2) C16 0.046(3) 0.027(3) 0.029(3) -0.003(2) 0.003(2) -0.003(2) C17 0.040(3) 0.035(3) 0.036(3) 0.002(2) 0.002(2) -0.007(3) C18 0.034(3) 0.040(3) 0.039(3) 0.004(3) 0.000(2) -0.004(2) C19 0.050(3) 0.040(3) 0.033(3) -0.008(2) 0.000(3) 0.008(3) C20 0.060(3) 0.036(3) 0.035(3) -0.004(2) -0.002(3) 0.017(3) C21 0.050(3) 0.042(3) 0.029(3) 0.001(2) 0.003(2) 0.020(3) C22 0.060(4) 0.049(3) 0.021(3) -0.008(2) -0.011(3) 0.003(3) C23 0.053(3) 0.033(3) 0.033(3) -0.003(2) -0.006(3) -0.007(3) C24 0.046(3) 0.045(3) 0.038(3) 0.000(3) -0.003(3) -0.022(3) C25 0.032(3) 0.034(3) 0.045(3) 0.012(2) 0.007(2) 0.015(2) C26 0.043(3) 0.026(3) 0.037(3) -0.001(2) 0.004(2) -0.011(2) C27 0.033(3) 0.026(3) 0.035(3) -0.002(2) -0.004(2) -0.002(2) C28 0.028(2) 0.036(3) 0.030(3) 0.009(2) -0.001(2) -0.004(2) C29 0.034(2) 0.034(3) 0.030(2) 0.008(2) 0.005(2) -0.010(2) C30 0.033(3) 0.059(4) 0.038(3) -0.002(3) 0.010(2) 0.004(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 O2W 2.315(4) . ? Dy1 O1 2.332(4) . ? Dy1 O1W 2.341(5) . ? Dy1 O10 2.350(4) 4_666 ? Dy1 O3W 2.360(4) . ? Dy1 O2 2.366(4) . ? Dy1 O4W 2.371(5) . ? Dy1 O9 2.389(3) 4_666 ? Dy1 H4WB 2.5082 . ? O1W H1WA 0.8501 . ? O1W H1WB 0.8501 . ? O2W H2WA 0.8498 . ? O2W H2WB 0.8501 . ? O3W H3WA 0.8500 . ? O3W H3WB 0.8501 . ? O4W H4WA 0.8499 . ? O4W H4WB 0.8502 . ? O5W H5WA 0.9800 . ? O5W H5WB 0.9800 . ? O6W H6WA 0.9800 . ? O6W H6WB 0.9800 . ? O7W H7WA 0.9800 . ? O7W H7WB 0.9800 . ? Cl1 Cl1' 1.826(18) . ? O8W H8WA 0.9800 . ? O8W H8WB 0.9800 . ? O9W H9WA 0.9800 . ? O9W H9WB 0.9800 . ? O10W H10C 0.9800 . ? O10W H10D 0.9800 . ? O11W H11B 0.9800 . ? O11W H11C 0.9800 . ? O1 C1 1.248(7) . ? O2 C3 1.242(7) . ? O3 C5 1.221(6) . ? O4 C7 1.238(7) . ? O5 C9 1.236(7) . ? O6 C23 1.216(7) . ? O7 C21 1.239(7) . ? O8 C29 1.227(6) . ? O9 C27 1.243(6) . ? O9 Dy1 2.389(3) 4_565 ? O10 C28 1.212(6) . ? O10 Dy1 2.350(4) 4_565 ? N1 C1 1.366(7) . ? N1 C10 1.417(8) . ? N1 C20 1.428(8) . ? N2 C1 1.342(8) . ? N2 C2 1.432(7) . ? N2 C19 1.474(7) . ? N3 C3 1.381(8) . ? N3 C2 1.439(8) . ? N3 C18 1.441(7) . ? N4 C3 1.340(7) . ? N4 C17 1.449(7) . ? N4 C4 1.466(7) . ? N5 C5 1.363(7) . ? N5 C4 1.439(7) . ? N5 C16 1.449(7) . ? N6 C5 1.380(7) . ? N6 C15 1.435(7) . ? N6 C6 1.445(8) . ? N7 C7 1.382(8) . ? N7 C6 1.426(7) . ? N7 C14 1.461(7) . ? N8 C7 1.341(7) . ? N8 C8 1.442(8) . ? N8 C13 1.452(7) . ? N9 C9 1.346(8) . ? N9 C8 1.465(9) . ? N9 C12 1.489(7) . ? N10 C9 1.355(8) . ? N10 C11 1.459(7) . ? N10 C10 1.466(9) . ? N11 C23 1.354(8) . ? N11 C22 1.464(9) . ? N11 C11 1.465(8) . ? N12 C23 1.371(8) . ? N12 C12 1.431(7) . ? N12 C24 1.460(8) . ? N13 C28 1.351(7) . ? N13 C24 1.439(8) . ? N13 C13 1.456(8) . ? N14 C28 1.353(7) . ? N14 C25 1.408(7) . ? N14 C14 1.454(7) . ? N15 C27 1.358(7) . ? N15 C25 1.449(7) . ? N15 C15 1.474(7) . ? N16 C27 1.340(7) . ? N16 C26 1.416(7) . ? N16 C16 1.468(7) . ? N17 C29 1.364(7) . ? N17 C26 1.441(7) . ? N17 C17 1.464(7) . ? N18 C29 1.360(7) . ? N18 C30 1.444(8) . ? N18 C18 1.471(7) . ? N19 C21 1.372(8) . ? N19 C30 1.439(8) . ? N19 C19 1.465(7) . ? N20 C21 1.333(8) . ? N20 C22 1.405(8) . ? N20 C20 1.505(7) . ? N21 O12 1.175(11) . ? N21 O13 1.238(12) . ? N21 O11 1.243(11) . ? N22 O15 1.240(8) . ? N22 O16 1.241(8) . ? N22 O14 1.249(7) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C11 C12 1.538(10) . ? C11 H11A 0.9900 . ? C12 H12A 0.9900 . ? C13 C14 1.551(9) . ? C13 H13A 0.9900 . ? C14 H14A 0.9900 . ? C15 C16 1.555(8) . ? C15 H15A 0.9900 . ? C16 H16A 0.9900 . ? C17 C18 1.534(9) . ? C17 H17A 0.9900 . ? C18 H18A 0.9900 . ? C19 C20 1.568(8) . ? C19 H19A 0.9900 . ? C20 H20A 0.9900 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 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 O2W Dy1 O1 114.38(15) . . ? O2W Dy1 O1W 145.76(15) . . ? O1 Dy1 O1W 79.10(15) . . ? O2W Dy1 O10 80.24(14) . 4_666 ? O1 Dy1 O10 143.90(13) . 4_666 ? O1W Dy1 O10 107.84(16) . 4_666 ? O2W Dy1 O3W 140.22(15) . . ? O1 Dy1 O3W 76.41(15) . . ? O1W Dy1 O3W 71.94(16) . . ? O10 Dy1 O3W 72.64(13) 4_666 . ? O2W Dy1 O2 70.73(13) . . ? O1 Dy1 O2 73.50(13) . . ? O1W Dy1 O2 142.41(14) . . ? O10 Dy1 O2 81.72(13) 4_666 . ? O3W Dy1 O2 76.92(14) . . ? O2W Dy1 O4W 74.97(16) . . ? O1 Dy1 O4W 71.23(14) . . ? O1W Dy1 O4W 80.79(17) . . ? O10 Dy1 O4W 144.16(13) 4_666 . ? O3W Dy1 O4W 140.89(15) . . ? O2 Dy1 O4W 113.04(15) . . ? O2W Dy1 O9 75.61(14) . 4_666 ? O1 Dy1 O9 138.03(14) . 4_666 ? O1W Dy1 O9 74.35(14) . 4_666 ? O10 Dy1 O9 76.19(13) 4_666 4_666 ? O3W Dy1 O9 123.30(14) . 4_666 ? O2 Dy1 O9 142.27(13) . 4_666 ? O4W Dy1 O9 72.88(14) . 4_666 ? O2W Dy1 H4WB 88.1 . . ? O1 Dy1 H4WB 77.9 . . ? O1W Dy1 H4WB 63.1 . . ? O10 Dy1 H4WB 137.5 4_666 . ? O3W Dy1 H4WB 131.4 . . ? O2 Dy1 H4WB 132.4 . . ? O4W Dy1 H4WB 19.8 . . ? O9 Dy1 H4WB 61.3 4_666 . ? Dy1 O1W H1WA 126.0 . . ? Dy1 O1W H1WB 115.8 . . ? H1WA O1W H1WB 108.2 . . ? Dy1 O2W H2WA 118.2 . . ? Dy1 O2W H2WB 122.4 . . ? H2WA O2W H2WB 108.7 . . ? Dy1 O3W H3WA 117.9 . . ? Dy1 O3W H3WB 117.6 . . ? H3WA O3W H3WB 108.6 . . ? Dy1 O4W H4WA 128.3 . . ? Dy1 O4W H4WB 89.3 . . ? H4WA O4W H4WB 108.1 . . ? H5WA O5W H5WB 114.7 . . ? H6WA O6W H6WB 115.8 . . ? H7WA O7W H7WB 118.3 . . ? H8WA O8W H8WB 117.1 . . ? H9WA O9W H9WB 118.0 . . ? H10C O10W H10D 118.3 . . ? H11B O11W H11C 116.2 . . ? C1 O1 Dy1 152.1(4) . . ? C3 O2 Dy1 150.2(4) . . ? C27 O9 Dy1 154.7(4) . 4_565 ? C28 O10 Dy1 155.7(4) . 4_565 ? C1 N1 C10 122.1(5) . . ? C1 N1 C20 111.4(5) . . ? C10 N1 C20 124.6(4) . . ? C1 N2 C2 124.0(5) . . ? C1 N2 C19 111.0(5) . . ? C2 N2 C19 124.9(5) . . ? C3 N3 C2 122.7(5) . . ? C3 N3 C18 111.8(5) . . ? C2 N3 C18 125.1(5) . . ? C3 N4 C17 113.0(5) . . ? C3 N4 C4 122.9(5) . . ? C17 N4 C4 123.7(5) . . ? C5 N5 C4 122.9(4) . . ? C5 N5 C16 112.6(4) . . ? C4 N5 C16 123.8(5) . . ? C5 N6 C15 112.8(5) . . ? C5 N6 C6 123.1(5) . . ? C15 N6 C6 123.8(5) . . ? C7 N7 C6 123.3(5) . . ? C7 N7 C14 110.6(5) . . ? C6 N7 C14 126.1(5) . . ? C7 N8 C8 121.7(5) . . ? C7 N8 C13 113.8(5) . . ? C8 N8 C13 123.5(5) . . ? C9 N9 C8 123.3(5) . . ? C9 N9 C12 112.8(5) . . ? C8 N9 C12 123.8(5) . . ? C9 N10 C11 112.2(5) . . ? C9 N10 C10 123.5(5) . . ? C11 N10 C10 124.3(5) . . ? C23 N11 C22 123.7(5) . . ? C23 N11 C11 111.6(5) . . ? C22 N11 C11 123.7(5) . . ? C23 N12 C12 112.3(5) . . ? C23 N12 C24 122.3(5) . . ? C12 N12 C24 124.8(5) . . ? C28 N13 C24 124.2(5) . . ? C28 N13 C13 111.6(5) . . ? C24 N13 C13 123.5(5) . . ? C28 N14 C25 123.3(5) . . ? C28 N14 C14 111.9(5) . . ? C25 N14 C14 124.8(5) . . ? C27 N15 C25 123.6(4) . . ? C27 N15 C15 111.8(4) . . ? C25 N15 C15 124.6(5) . . ? C27 N16 C26 124.2(5) . . ? C27 N16 C16 112.0(5) . . ? C26 N16 C16 123.2(4) . . ? C29 N17 C26 122.5(4) . . ? C29 N17 C17 111.9(4) . . ? C26 N17 C17 125.3(5) . . ? C29 N18 C30 122.2(4) . . ? C29 N18 C18 111.2(5) . . ? C30 N18 C18 126.0(4) . . ? C21 N19 C30 123.6(5) . . ? C21 N19 C19 111.7(5) . . ? C30 N19 C19 124.7(5) . . ? C21 N20 C22 126.1(5) . . ? C21 N20 C20 111.2(4) . . ? C22 N20 C20 122.7(5) . . ? O12 N21 O13 116.5(9) . . ? O12 N21 O11 121.6(10) . . ? O13 N21 O11 121.5(9) . . ? O15 N22 O16 120.8(10) . . ? O15 N22 O14 119.7(8) . . ? O16 N22 O14 118.9(9) . . ? O1 C1 N2 125.0(5) . . ? O1 C1 N1 124.0(6) . . ? N2 C1 N1 111.0(5) . . ? N2 C2 N3 113.4(5) . . ? N2 C2 H2A 108.9 . . ? N3 C2 H2A 108.9 . . ? N2 C2 H2B 108.9 . . ? N3 C2 H2B 108.9 . . ? H2A C2 H2B 107.7 . . ? O2 C3 N4 125.3(5) . . ? O2 C3 N3 126.5(5) . . ? N4 C3 N3 108.2(5) . . ? N5 C4 N4 113.2(4) . . ? N5 C4 H4A 108.9 . . ? N4 C4 H4A 108.9 . . ? N5 C4 H4B 108.9 . . ? N4 C4 H4B 108.9 . . ? H4A C4 H4B 107.8 . . ? O3 C5 N5 125.5(5) . . ? O3 C5 N6 126.7(5) . . ? N5 C5 N6 107.8(4) . . ? N7 C6 N6 114.6(5) . . ? N7 C6 H6A 108.6 . . ? N6 C6 H6A 108.6 . . ? N7 C6 H6B 108.6 . . ? N6 C6 H6B 108.6 . . ? H6A C6 H6B 107.6 . . ? O4 C7 N8 127.4(6) . . ? O4 C7 N7 123.6(5) . . ? N8 C7 N7 109.0(5) . . ? N8 C8 N9 112.6(5) . . ? N8 C8 H8A 109.1 . . ? N9 C8 H8A 109.1 . . ? N8 C8 H8B 109.1 . . ? N9 C8 H8B 109.1 . . ? H8A C8 H8B 107.8 . . ? O5 C9 N9 125.3(6) . . ? O5 C9 N10 125.7(6) . . ? N9 C9 N10 109.0(5) . . ? N1 C10 N10 114.7(5) . . ? N1 C10 H10A 108.6 . . ? N10 C10 H10A 108.6 . . ? N1 C10 H10B 108.6 . . ? N10 C10 H10B 108.6 . . ? H10A C10 H10B 107.6 . . ? N10 C11 N11 114.9(5) . . ? N10 C11 C12 104.3(5) . . ? N11 C11 C12 103.2(5) . . ? N10 C11 H11A 111.3 . . ? N11 C11 H11A 111.3 . . ? C12 C11 H11A 111.3 . . ? N12 C12 N9 115.1(5) . . ? N12 C12 C11 103.8(5) . . ? N9 C12 C11 101.6(5) . . ? N12 C12 H12A 111.9 . . ? N9 C12 H12A 111.9 . . ? C11 C12 H12A 111.9 . . ? N8 C13 N13 114.0(5) . . ? N8 C13 C14 102.1(4) . . ? N13 C13 C14 103.3(5) . . ? N8 C13 H13A 112.2 . . ? N13 C13 H13A 112.2 . . ? C14 C13 H13A 112.2 . . ? N14 C14 N7 116.6(5) . . ? N14 C14 C13 103.0(5) . . ? N7 C14 C13 104.3(4) . . ? N14 C14 H14A 110.8 . . ? N7 C14 H14A 110.8 . . ? C13 C14 H14A 110.8 . . ? N6 C15 N15 114.6(4) . . ? N6 C15 C16 103.1(4) . . ? N15 C15 C16 102.5(4) . . ? N6 C15 H15A 111.9 . . ? N15 C15 H15A 111.9 . . ? C16 C15 H15A 111.9 . . ? N5 C16 N16 115.5(5) . . ? N5 C16 C15 103.3(4) . . ? N16 C16 C15 103.4(4) . . ? N5 C16 H16A 111.3 . . ? N16 C16 H16A 111.3 . . ? C15 C16 H16A 111.3 . . ? N4 C17 N17 114.5(5) . . ? N4 C17 C18 103.1(5) . . ? N17 C17 C18 103.3(4) . . ? N4 C17 H17A 111.7 . . ? N17 C17 H17A 111.7 . . ? C18 C17 H17A 111.7 . . ? N3 C18 N18 114.9(5) . . ? N3 C18 C17 103.6(5) . . ? N18 C18 C17 103.9(4) . . ? N3 C18 H18A 111.3 . . ? N18 C18 H18A 111.3 . . ? C17 C18 H18A 111.3 . . ? N19 C19 N2 115.2(5) . . ? N19 C19 C20 103.0(4) . . ? N2 C19 C20 102.4(5) . . ? N19 C19 H19A 111.8 . . ? N2 C19 H19A 111.8 . . ? C20 C19 H19A 111.8 . . ? N1 C20 N20 114.2(5) . . ? N1 C20 C19 103.9(4) . . ? N20 C20 C19 102.7(4) . . ? N1 C20 H20A 111.8 . . ? N20 C20 H20A 111.8 . . ? C19 C20 H20A 111.8 . . ? O7 C21 N20 124.1(5) . . ? O7 C21 N19 124.7(6) . . ? N20 C21 N19 111.2(5) . . ? N20 C22 N11 113.7(5) . . ? N20 C22 H22A 108.8 . . ? N11 C22 H22A 108.8 . . ? N20 C22 H22B 108.8 . . ? N11 C22 H22B 108.8 . . ? H22A C22 H22B 107.7 . . ? O6 C23 N11 125.7(6) . . ? O6 C23 N12 125.5(6) . . ? N11 C23 N12 108.7(5) . . ? N13 C24 N12 112.9(4) . . ? N13 C24 H24A 109.0 . . ? N12 C24 H24A 109.0 . . ? N13 C24 H24B 109.0 . . ? N12 C24 H24B 109.0 . . ? H24A C24 H24B 107.8 . . ? N14 C25 N15 113.6(4) . . ? N14 C25 H25A 108.8 . . ? N15 C25 H25A 108.8 . . ? N14 C25 H25B 108.8 . . ? N15 C25 H25B 108.8 . . ? H25A C25 H25B 107.7 . . ? N16 C26 N17 113.9(4) . . ? N16 C26 H26A 108.8 . . ? N17 C26 H26A 108.8 . . ? N16 C26 H26B 108.8 . . ? N17 C26 H26B 108.8 . . ? H26A C26 H26B 107.7 . . ? O9 C27 N16 124.8(5) . . ? O9 C27 N15 124.8(5) . . ? N16 C27 N15 110.3(5) . . ? O10 C28 N13 124.4(5) . . ? O10 C28 N14 125.7(5) . . ? N13 C28 N14 110.0(5) . . ? O8 C29 N18 125.7(5) . . ? O8 C29 N17 124.8(5) . . ? N18 C29 N17 109.5(4) . . ? N19 C30 N18 113.4(5) . . ? N19 C30 H30A 108.9 . . ? N18 C30 H30A 108.9 . . ? N19 C30 H30B 108.9 . . ? N18 C30 H30B 108.9 . . ? H30A C30 H30B 107.7 . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 2.498 _refine_diff_density_min -1.093 _refine_diff_density_rms 0.194 data_p _database_code_depnum_ccdc_archive 'CCDC 844326' #TrackingRef 'compound 2b.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common compound2b _chemical_melting_point 'not measured' _chemical_formula_moiety 'C30 H38 Dy N20 O14, C6 H6 O2,3(N O3), 7(H2 O)' _chemical_formula_sum 'C36 H58 Dy N23 O32' _chemical_formula_weight 1487.55 _chemical_absolute_configuration ' S ' 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' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M P6(5) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+2/3' '-x+y, -x, z+1/3' '-x, -y, z+1/2' 'y, -x+y, z+1/6' 'x-y, x, z+5/6' _cell_length_a 14.5310(10) _cell_length_b 14.5310(10) _cell_length_c 46.070(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 8424.5(15) _cell_formula_units_Z 6 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 7265 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 22.97 _exptl_crystal_description block _exptl_crystal_colour 'red brown' _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.759 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4542 _exptl_absorpt_coefficient_mu 1.449 _exptl_absorpt_correction_type 'multi scan' _exptl_absorpt_correction_T_min 0.7045 _exptl_absorpt_correction_T_max 0.8120 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 57360 _diffrn_reflns_av_R_equivalents 0.0812 _diffrn_reflns_av_sigmaI/netI 0.0615 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -56 _diffrn_reflns_limit_l_max 54 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 26.00 _reflns_number_total 10436 _reflns_number_gt 9255 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 1.000 0.023 1206 239 ' ' 2 0.058 0.594 0.174 45 6 ' ' 3 -0.058 0.405 0.674 45 7 ' ' 4 0.104 0.805 0.309 8 2 ' ' 5 0.194 0.298 0.976 8 1 ' ' 6 0.299 0.104 0.143 9 3 ' ' 7 0.405 0.463 0.840 46 5 ' ' 8 0.463 0.058 0.007 46 12 ' ' 9 0.536 0.942 0.507 46 12 ' ' 10 0.594 0.536 0.340 46 5 ' ' 11 0.701 0.896 0.643 9 4 ' ' 12 0.805 0.701 0.476 8 1 ' ' 13 0.896 0.194 0.809 8 1 ' ' _platon_squeeze_details ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0839P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.020(18) _refine_ls_number_reflns 10436 _refine_ls_number_parameters 709 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.0583 _refine_ls_R_factor_gt 0.0517 _refine_ls_wR_factor_ref 0.1328 _refine_ls_wR_factor_gt 0.1298 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.818 _refine_ls_shift/su_max 0.059 _refine_ls_shift/su_mean 0.016 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 0.32330(2) 0.78623(2) 0.090163(8) 0.03024(7) Uani 1 1 d . . . O1 O 0.3137(3) 0.6956(3) 0.13185(10) 0.0392(13) Uani 1 1 d . . . O2 O 0.2505(3) 0.8507(3) 0.12452(10) 0.0393(13) Uani 1 1 d . . . O3 O -0.0006(4) 0.7180(4) 0.10029(11) 0.0458(14) Uani 1 1 d . . . O4 O 0.1411(3) 0.4739(3) 0.10862(10) 0.0363(12) Uani 1 1 d . . . O5 O -0.0660(3) 0.4783(3) 0.08933(11) 0.0393(12) Uani 1 1 d . . . O6 O -0.1523(3) 0.6107(3) 0.22601(10) 0.0394(13) Uani 1 1 d . . . O7 O -0.1848(3) 0.4039(3) 0.21349(10) 0.0391(13) Uani 1 1 d . . . O8 O 0.0924(4) 0.7499(4) 0.25003(11) 0.0486(15) Uani 1 1 d . . . O9 O -0.0038(3) 0.3661(4) 0.23401(11) 0.0448(14) Uani 1 1 d . . . O10 O 0.1872(3) 0.5920(4) 0.25574(12) 0.0466(14) Uani 1 1 d . . . O11 O -0.1015(6) 0.0751(8) 0.0656(2) 0.220(7) Uani 1 1 d D . . O12 O 0.3033(6) 0.3375(8) 0.1041(3) 0.227(6) Uani 1 1 d D . . N1 N 0.3753(4) 0.7657(4) 0.17689(12) 0.0394(16) Uani 1 1 d . . . N2 N 0.3100(4) 0.8904(4) 0.17254(12) 0.0374(16) Uani 1 1 d . . . N3 N 0.2417(5) 0.8359(5) 0.22162(14) 0.051(2) Uani 1 1 d . . . N4 N 0.3181(5) 0.7240(4) 0.22778(13) 0.0439(18) Uani 1 1 d . . . N5 N -0.0400(4) 0.2862(4) 0.18829(12) 0.0364(16) Uani 1 1 d . . . N6 N 0.1273(4) 0.3906(4) 0.20184(12) 0.0352(15) Uani 1 1 d . . . N7 N 0.3223(4) 0.5966(4) 0.16887(12) 0.0341(15) Uani 1 1 d . . . N8 N -0.1502(4) 0.6317(5) 0.12919(13) 0.0422(17) Uani 1 1 d . . . N9 N 0.0192(4) 0.3418(4) 0.13815(12) 0.0343(15) Uani 1 1 d . . . N10 N 0.1002(4) 0.8506(4) 0.21065(14) 0.0418(17) Uani 1 1 d . . . N11 N 0.1600(4) 0.8855(4) 0.16030(13) 0.0403(17) Uani 1 1 d . . . N12 N -0.0191(4) 0.7920(4) 0.14289(14) 0.0437(17) Uani 1 1 d . . . N13 N -0.1860(4) 0.3116(4) 0.17309(12) 0.0320(14) Uani 1 1 d . . . N14 N -0.2595(4) 0.4136(4) 0.17009(12) 0.0343(15) Uani 1 1 d . . . N15 N -0.2048(4) 0.4494(5) 0.11916(15) 0.0429(18) Uani 1 1 d . . . N16 N -0.2144(4) 0.5933(4) 0.17943(12) 0.0346(15) Uani 1 1 d . . . N17 N -0.1412(4) 0.3378(4) 0.12139(12) 0.0359(15) Uani 1 1 d . . . N18 N -0.0787(4) 0.7475(4) 0.19296(13) 0.0397(16) Uani 1 1 d . . . N19 N 0.1888(4) 0.4265(4) 0.15157(12) 0.0303(14) Uani 1 1 d . . . N20 N 0.2744(4) 0.5551(4) 0.22069(12) 0.0356(15) Uani 1 1 d . . . O1W O 0.3053(4) 0.6243(4) 0.07412(12) 0.0492(15) Uani 1 1 d . . . O2W O 0.4967(4) 0.8251(4) 0.10177(12) 0.0527(17) Uani 1 1 d . . . O3W O 0.4340(4) 0.9712(4) 0.09150(13) 0.0485(15) Uani 1 1 d . . . O4W O 0.1452(3) 0.6590(3) 0.09022(13) 0.0460(14) Uani 1 1 d . . . O5W O 0.6022(6) 0.9790(6) 0.2309(2) 0.106(3) Uani 1 1 d . . . O6W O 0.4250(6) 0.5856(6) 0.0355(2) 0.129(3) Uani 1 1 d D . . O7W O 0.4268(10) 0.3254(10) 0.1495(3) 0.184(5) Uani 1 1 d . . . O8W O -0.0160(10) 0.0425(6) 0.1810(2) 0.192(4) Uani 1 1 d . . . O9W O -0.4606(6) 0.5154(10) 0.1251(2) 0.163(5) Uani 1 1 d . . . C1 C 0.3919(5) 0.7296(5) 0.20511(14) 0.0378(19) Uani 1 1 d . . . H1A H 0.4668 0.7718 0.2115 0.045 Uiso 1 1 calc R . . C2 C 0.2805(5) 0.9187(5) 0.19854(15) 0.041(2) Uani 1 1 d . . . H2A H 0.3368 0.9885 0.2058 0.049 Uiso 1 1 calc R . . C3 C -0.2104(5) 0.5410(5) 0.11027(15) 0.0383(18) Uani 1 1 d . . . H3A H -0.2849 0.5234 0.1101 0.046 Uiso 1 1 calc R . . H3B H -0.1830 0.5602 0.0904 0.046 Uiso 1 1 calc R . . C4 C 0.1785(6) 0.9208(6) 0.19039(16) 0.043(2) Uani 1 1 d . . . H4A H 0.1896 0.9936 0.1921 0.051 Uiso 1 1 calc R . . C5 C -0.2242(4) 0.2968(5) 0.14359(14) 0.0314(17) Uani 1 1 d . . . H5A H -0.2789 0.2220 0.1398 0.038 Uiso 1 1 calc R . . C6 C -0.1929(5) 0.6600(5) 0.15370(15) 0.0369(17) Uani 1 1 d . . . H6A H -0.2567 0.6638 0.1480 0.044 Uiso 1 1 calc R . . C8 C -0.0494(5) 0.7150(5) 0.12191(17) 0.044(2) Uani 1 1 d . . . C9 C 0.2163(5) 0.4431(5) 0.22252(15) 0.0405(19) Uani 1 1 d . . . H9A H 0.1882 0.4231 0.2423 0.049 Uiso 1 1 calc R . . H9B H 0.2652 0.4160 0.2193 0.049 Uiso 1 1 calc R . . C10 C 0.4010(5) 0.8737(5) 0.16991(18) 0.044(2) Uani 1 1 d . . . H10A H 0.4282 0.8901 0.1500 0.052 Uiso 1 1 calc R . . H10B H 0.4576 0.9231 0.1829 0.052 Uiso 1 1 calc R . . C11 C 0.0843(6) 0.8900(5) 0.14090(18) 0.045(2) Uani 1 1 d . . . H11A H 0.1107 0.8996 0.1209 0.054 Uiso 1 1 calc R . . H11B H 0.0761 0.9511 0.1460 0.054 Uiso 1 1 calc R . . C12 C 0.3098(6) 0.8113(6) 0.23854(17) 0.046(2) Uani 1 1 d . . . H12A H 0.3809 0.8742 0.2392 0.055 Uiso 1 1 calc R . . H12B H 0.2827 0.7956 0.2585 0.055 Uiso 1 1 calc R . . C13 C -0.1022(5) 0.7702(5) 0.16334(16) 0.0417(19) Uani 1 1 d . . . H13A H -0.1235 0.8251 0.1632 0.050 Uiso 1 1 calc R . . C14 C 0.3011(5) 0.5061(5) 0.15211(15) 0.0369(17) Uani 1 1 d . . . H14A H 0.3412 0.4743 0.1601 0.044 Uiso 1 1 calc R . . H14B H 0.3257 0.5285 0.1322 0.044 Uiso 1 1 calc R . . C15 C 0.2524(5) 0.6208(6) 0.23634(14) 0.0385(19) Uani 1 1 d . . . C16 C 0.0202(5) 0.2833(5) 0.16331(14) 0.0326(16) Uani 1 1 d . . . H16A H 0.0011 0.2096 0.1583 0.039 Uiso 1 1 calc R . . C17 C 0.1195(5) 0.4214(4) 0.13036(14) 0.0297(16) Uani 1 1 d . . . C18 C 0.1385(5) 0.8049(5) 0.22933(14) 0.0359(18) Uani 1 1 d . . . C19 C 0.2417(5) 0.8719(5) 0.15020(16) 0.0375(19) Uani 1 1 d . . . C20 C -0.1277(5) 0.4279(5) 0.10761(15) 0.0352(18) Uani 1 1 d . . . C21 C -0.1499(5) 0.6460(5) 0.20122(15) 0.0344(16) Uani 1 1 d . . . C22 C -0.0086(5) 0.8281(6) 0.21314(17) 0.047(2) Uani 1 1 d . . . H22A H -0.0107 0.8935 0.2096 0.057 Uiso 1 1 calc R . . H22B H -0.0339 0.8045 0.2330 0.057 Uiso 1 1 calc R . . C23 C 0.3595(5) 0.6138(6) 0.19961(16) 0.044(2) Uani 1 1 d . . . H23A H 0.4197 0.6010 0.2024 0.053 Uiso 1 1 calc R . . C24 C -0.1520(5) 0.2459(5) 0.18784(15) 0.0359(18) Uani 1 1 d . . . H24A H -0.1775 0.2356 0.2079 0.043 Uiso 1 1 calc R . . H24B H -0.1863 0.1759 0.1785 0.043 Uiso 1 1 calc R . . C25 C 0.0272(5) 0.3522(5) 0.21032(15) 0.0385(19) Uani 1 1 d . . . C26 C -0.2698(5) 0.3726(5) 0.14026(15) 0.0346(19) Uani 1 1 d . . . H26A H -0.3451 0.3335 0.1340 0.042 Uiso 1 1 calc R . . C27 C 0.1348(5) 0.3475(5) 0.17438(15) 0.0364(17) Uani 1 1 d . . . H27A H 0.1668 0.3016 0.1767 0.044 Uiso 1 1 calc R . . C28 C -0.0654(5) 0.3008(5) 0.11726(15) 0.0355(18) Uani 1 1 d . . . H28A H -0.1037 0.2230 0.1182 0.043 Uiso 1 1 calc R . . H28B H -0.0346 0.3214 0.0978 0.043 Uiso 1 1 calc R . . C29 C -0.2077(5) 0.3790(6) 0.18722(15) 0.0376(19) Uani 1 1 d . . . C30 C 0.3356(4) 0.6875(5) 0.15784(14) 0.0312(17) Uani 1 1 d . . . C7 C -0.2959(5) 0.4847(5) 0.17941(16) 0.0405(19) Uani 1 1 d . . . H7A H -0.3533 0.4762 0.1666 0.049 Uiso 1 1 calc R . . H7B H -0.3251 0.4648 0.1991 0.049 Uiso 1 1 calc R . . C36 C -0.0030(4) 0.1336(5) 0.07702(18) 0.757(5) Uani 1 1 d GDU . . C35 C 0.0609(5) 0.2276(5) 0.0621(2) 0.163(6) Uani 1 1 d GD . . H35A H 0.0342 0.2450 0.0457 0.196 Uiso 1 1 calc R . . C34 C 0.1642(5) 0.2958(5) 0.0715(3) 0.162(7) Uani 1 1 d GD . . H34A H 0.2073 0.3594 0.0614 0.194 Uiso 1 1 calc R . . C33 C 0.2036(5) 0.2700(7) 0.0957(3) 0.278(6) Uani 1 1 d GD . . C32 C 0.1397(6) 0.1760(8) 0.1106(2) 0.243(13) Uani 1 1 d GD . . H32A H 0.1663 0.1585 0.1270 0.292 Uiso 1 1 calc R . . C31 C 0.0364(6) 0.1078(6) 0.10128(19) 0.169(8) Uani 1 1 d GD . . H31A H -0.0068 0.0442 0.1114 0.202 Uiso 1 1 calc R . . O10W O 0.4474(9) 0.4317(9) 0.2020(3) 0.162(4) Uani 1 1 d . . . O11W O 0.3716(9) 0.4951(10) -0.0149(3) 0.182(5) Uani 1 1 d 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 0.03463(11) 0.03557(11) 0.01734(11) 0.00502(11) 0.00450(11) 0.01515(9) O1 0.052(2) 0.039(2) 0.024(2) 0.0036(17) 0.0029(19) 0.0202(16) O2 0.045(2) 0.045(2) 0.027(2) 0.0008(18) 0.0049(18) 0.0220(16) O3 0.051(2) 0.061(2) 0.029(2) -0.0009(19) 0.0029(19) 0.0305(17) O4 0.0413(18) 0.0405(19) 0.027(2) 0.0083(17) 0.0011(18) 0.0206(15) O5 0.0389(17) 0.0450(19) 0.034(2) 0.001(2) 0.012(2) 0.0211(14) O6 0.049(2) 0.045(2) 0.028(2) 0.0032(18) 0.0074(19) 0.0266(16) O7 0.051(2) 0.048(2) 0.023(2) -0.0055(17) -0.0049(18) 0.0285(16) O8 0.054(2) 0.050(2) 0.039(3) 0.005(2) 0.007(2) 0.0245(18) O9 0.052(2) 0.058(2) 0.031(3) 0.0036(19) 0.004(2) 0.0331(17) O10 0.0470(19) 0.061(2) 0.035(3) 0.004(2) 0.004(2) 0.0289(16) O11 0.218(10) 0.281(13) 0.192(14) -0.083(11) -0.061(10) 0.148(9) O12 0.156(7) 0.242(9) 0.264(12) -0.134(8) 0.046(8) 0.086(7) N1 0.046(3) 0.041(3) 0.026(3) 0.006(2) -0.002(2) 0.018(2) N2 0.041(2) 0.038(2) 0.028(3) -0.002(2) 0.000(2) 0.0161(19) N3 0.065(3) 0.050(3) 0.033(3) -0.002(3) 0.001(3) 0.026(2) N4 0.054(3) 0.039(3) 0.030(3) -0.006(2) -0.006(2) 0.017(2) N5 0.034(2) 0.040(3) 0.025(3) -0.004(2) 0.001(2) 0.011(2) N6 0.042(2) 0.045(2) 0.025(3) 0.004(2) 0.000(2) 0.0264(18) N7 0.034(2) 0.042(2) 0.024(3) 0.006(2) 0.001(2) 0.0178(18) N8 0.041(2) 0.055(3) 0.029(3) 0.007(2) 0.003(2) 0.023(2) N9 0.036(2) 0.035(2) 0.029(3) 0.007(2) 0.005(2) 0.0151(18) N10 0.054(3) 0.033(2) 0.041(3) 0.002(2) 0.003(3) 0.0230(19) N11 0.045(2) 0.042(2) 0.033(3) -0.005(2) 0.004(2) 0.021(2) N12 0.048(2) 0.050(2) 0.044(4) 0.005(2) 0.004(2) 0.0325(19) N13 0.037(2) 0.035(2) 0.026(3) -0.004(2) 0.001(2) 0.0192(17) N14 0.041(2) 0.043(2) 0.025(3) -0.005(2) -0.004(2) 0.0252(18) N15 0.040(2) 0.055(3) 0.033(3) 0.001(2) -0.003(2) 0.024(2) N16 0.036(2) 0.040(2) 0.023(3) 0.002(2) 0.001(2) 0.0154(19) N17 0.043(2) 0.049(2) 0.021(3) -0.008(2) 0.003(2) 0.0274(18) N18 0.055(3) 0.042(2) 0.026(3) 0.002(2) 0.001(2) 0.0268(19) N19 0.033(2) 0.029(2) 0.025(3) 0.0053(19) 0.004(2) 0.0121(17) N20 0.039(2) 0.050(2) 0.025(3) 0.004(2) 0.001(2) 0.0280(18) O1W 0.059(2) 0.044(2) 0.042(3) 0.011(2) 0.022(2) 0.0237(18) O2W 0.052(2) 0.052(3) 0.047(3) 0.006(2) 0.000(2) 0.021(2) O3W 0.045(2) 0.043(2) 0.045(3) 0.004(2) 0.003(2) 0.0126(17) O4W 0.039(2) 0.0360(19) 0.054(3) 0.009(2) 0.000(2) 0.0124(16) O5W 0.098(5) 0.045(3) 0.125(7) 0.000(4) -0.023(5) 0.000(4) O6W 0.120(4) 0.137(5) 0.168(7) 0.073(5) 0.089(4) 0.093(3) O7W 0.220(8) 0.241(9) 0.138(9) -0.072(8) -0.090(7) 0.151(6) O8W 0.439(9) 0.128(4) 0.094(8) 0.017(4) 0.009(7) 0.205(4) O9W 0.080(4) 0.303(10) 0.120(8) -0.073(7) -0.024(5) 0.107(5) C1 0.039(3) 0.047(3) 0.025(3) -0.003(3) -0.002(3) 0.019(2) C2 0.047(3) 0.040(3) 0.030(4) -0.008(3) 0.004(3) 0.017(2) C3 0.040(3) 0.057(3) 0.022(3) 0.005(3) -0.003(2) 0.027(2) C4 0.055(3) 0.041(3) 0.027(3) -0.001(3) 0.005(3) 0.021(3) C5 0.025(2) 0.038(3) 0.023(3) -0.005(2) -0.003(2) 0.010(2) C6 0.039(2) 0.053(3) 0.031(3) 0.006(3) 0.001(2) 0.033(2) C8 0.057(3) 0.050(3) 0.040(4) 0.006(3) 0.001(3) 0.038(2) C9 0.044(3) 0.066(3) 0.022(3) 0.011(3) 0.004(2) 0.035(2) C10 0.036(3) 0.032(3) 0.046(4) -0.005(3) -0.006(3) 0.004(3) C11 0.061(4) 0.022(2) 0.048(4) 0.010(3) 0.001(3) 0.018(2) C12 0.043(3) 0.058(4) 0.025(4) -0.014(3) -0.007(3) 0.016(3) C13 0.051(3) 0.046(3) 0.037(4) 0.005(3) 0.011(3) 0.030(2) C14 0.042(2) 0.057(3) 0.026(3) -0.001(2) 0.001(2) 0.035(2) C15 0.034(3) 0.062(4) 0.017(3) -0.002(3) -0.007(2) 0.022(2) C16 0.046(3) 0.031(2) 0.029(3) 0.007(2) 0.007(2) 0.0265(19) C17 0.036(2) 0.026(2) 0.029(3) -0.004(2) 0.001(2) 0.0170(19) C18 0.056(3) 0.042(3) 0.013(3) 0.000(2) 0.004(3) 0.027(2) C19 0.039(3) 0.030(3) 0.034(4) 0.004(3) 0.004(3) 0.011(2) C20 0.030(2) 0.044(3) 0.031(3) -0.002(3) -0.006(2) 0.019(2) C21 0.044(2) 0.045(3) 0.027(3) 0.002(2) 0.009(2) 0.0322(19) C22 0.065(3) 0.060(3) 0.033(4) -0.011(3) 0.004(3) 0.043(2) C23 0.027(3) 0.069(4) 0.033(4) 0.012(3) -0.004(3) 0.022(2) C24 0.039(3) 0.035(3) 0.030(3) 0.006(3) 0.008(3) 0.016(2) C25 0.045(3) 0.047(3) 0.025(3) 0.000(3) -0.001(3) 0.024(2) C26 0.029(3) 0.035(3) 0.032(4) 0.000(3) 0.000(2) 0.010(2) C27 0.049(3) 0.042(3) 0.027(3) 0.006(2) 0.007(3) 0.030(2) C28 0.040(3) 0.033(3) 0.028(3) -0.008(2) -0.002(3) 0.015(2) C29 0.031(3) 0.046(3) 0.025(3) 0.000(3) 0.011(2) 0.011(2) C30 0.024(2) 0.037(3) 0.025(3) 0.001(2) 0.004(2) 0.010(2) C7 0.042(3) 0.058(3) 0.028(4) 0.007(3) 0.010(3) 0.029(2) C36 0.956(6) 1.128(6) 0.749(7) -0.004(5) 0.002(5) 0.942(4) C35 0.163(8) 0.164(8) 0.186(13) -0.058(8) 0.056(9) 0.098(7) C34 0.099(8) 0.208(11) 0.139(10) -0.110(8) 0.009(8) 0.047(8) C33 0.118(6) 0.396(9) 0.362(14) -0.327(8) -0.098(9) 0.159(7) C32 0.196(13) 0.092(7) 0.44(4) -0.084(13) 0.062(18) 0.073(8) C31 0.160(11) 0.130(8) 0.208(17) -0.081(9) 0.021(12) 0.067(8) O10W 0.217(6) 0.227(7) 0.121(9) -0.042(6) -0.043(7) 0.169(5) O11W 0.263(7) 0.221(7) 0.149(9) 0.058(7) 0.087(7) 0.186(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 O1 2.293(5) . ? Dy1 O7 2.293(5) 6_664 ? Dy1 O4W 2.309(4) . ? Dy1 O3W 2.343(4) . ? Dy1 O2 2.344(5) . ? Dy1 O6 2.346(5) 6_664 ? Dy1 O1W 2.353(5) . ? Dy1 O2W 2.352(6) . ? O1 C30 1.260(8) . ? O2 C19 1.245(9) . ? O3 C8 1.211(9) . ? O4 C17 1.202(8) . ? O5 C20 1.180(8) . ? O6 C21 1.246(8) . ? O6 Dy1 2.346(5) 5_455 ? O7 C29 1.259(8) . ? O7 Dy1 2.293(5) 5_455 ? O8 C18 1.209(8) . ? O9 C25 1.236(9) . ? O10 C15 1.215(8) . ? O11 C36 1.354(9) . ? O12 C33 1.338(8) . ? N1 C30 1.319(8) . ? N1 C10 1.455(10) . ? N1 C1 1.466(9) . ? N2 C19 1.360(9) . ? N2 C2 1.402(10) . ? N2 C10 1.463(10) . ? N3 C18 1.378(10) . ? N3 C12 1.438(12) . ? N3 C2 1.489(10) . ? N4 C15 1.373(9) . ? N4 C12 1.423(12) . ? N4 C1 1.469(10) . ? N5 C25 1.403(8) . ? N5 C24 1.429(8) . ? N5 C16 1.459(9) . ? N6 C25 1.329(8) . ? N6 C27 1.441(9) . ? N6 C9 1.476(8) . ? N7 C30 1.336(9) . ? N7 C14 1.419(9) . ? N7 C23 1.492(9) . ? N8 C8 1.396(8) . ? N8 C6 1.444(10) . ? N8 C3 1.452(9) . ? N9 C17 1.380(7) . ? N9 C28 1.436(8) . ? N9 C16 1.442(9) . ? N10 C18 1.364(10) . ? N10 C4 1.430(9) . ? N10 C22 1.451(10) . ? N11 C19 1.379(10) . ? N11 C11 1.444(10) . ? N11 C4 1.456(9) . ? N12 C8 1.374(10) . ? N12 C13 1.436(9) . ? N12 C11 1.469(8) . ? N13 C29 1.338(10) . ? N13 C5 1.443(8) . ? N13 C24 1.445(10) . ? N14 C29 1.350(10) . ? N14 C7 1.441(10) . ? N14 C26 1.476(9) . ? N15 C20 1.410(10) . ? N15 C26 1.424(9) . ? N15 C3 1.433(11) . ? N16 C21 1.325(8) . ? N16 C7 1.423(8) . ? N16 C6 1.463(9) . ? N17 C20 1.377(9) . ? N17 C5 1.462(8) . ? N17 C28 1.460(10) . ? N18 C21 1.365(8) . ? N18 C22 1.442(9) . ? N18 C13 1.483(10) . ? N19 C17 1.379(9) . ? N19 C14 1.453(7) . ? N19 C27 1.462(8) . ? N20 C15 1.355(10) . ? N20 C9 1.413(8) . ? N20 C23 1.465(8) . ? C1 C23 1.525(11) . ? C1 H1A 0.9900 . ? C2 C4 1.544(12) . ? C2 H2A 0.9900 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C4 H4A 0.9900 . ? C5 C26 1.551(11) . ? C5 H5A 0.9900 . ? C6 C13 1.545(8) . ? C6 H6A 0.9900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 H13A 0.9900 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C16 C27 1.533(9) . ? C16 H16A 0.9900 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C23 H23A 0.9900 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C26 H26A 0.9900 . ? C27 H27A 0.9900 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C36 C35 1.3900 . ? C36 C31 1.3900 . ? C35 C34 1.3900 . ? C35 H35A 0.9400 . ? C34 C33 1.3900 . ? C34 H34A 0.9400 . ? C33 C32 1.3900 . ? C32 C31 1.3900 . ? C32 H32A 0.9400 . ? C31 H31A 0.9400 . ? 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 O1 Dy1 O7 134.64(17) . 6_664 ? O1 Dy1 O4W 79.48(18) . . ? O7 Dy1 O4W 116.5(2) 6_664 . ? O1 Dy1 O3W 116.50(18) . . ? O7 Dy1 O3W 79.20(18) 6_664 . ? O4W Dy1 O3W 140.35(19) . . ? O1 Dy1 O2 75.77(18) . . ? O7 Dy1 O2 146.73(15) 6_664 . ? O4W Dy1 O2 76.69(17) . . ? O3W Dy1 O2 73.26(17) . . ? O1 Dy1 O6 146.60(18) . 6_664 ? O7 Dy1 O6 76.01(17) 6_664 6_664 ? O4W Dy1 O6 72.96(19) . 6_664 ? O3W Dy1 O6 76.73(18) . 6_664 ? O2 Dy1 O6 79.77(17) . 6_664 ? O1 Dy1 O1W 75.19(18) . . ? O7 Dy1 O1W 71.51(15) 6_664 . ? O4W Dy1 O1W 71.37(18) . . ? O3W Dy1 O1W 145.53(18) . . ? O2 Dy1 O1W 139.94(15) . . ? O6 Dy1 O1W 112.17(18) 6_664 . ? O1 Dy1 O2W 72.39(17) . . ? O7 Dy1 O2W 73.86(19) 6_664 . ? O4W Dy1 O2W 146.05(19) . . ? O3W Dy1 O2W 71.33(19) . . ? O2 Dy1 O2W 113.21(18) . . ? O6 Dy1 O2W 139.32(18) 6_664 . ? O1W Dy1 O2W 83.18(19) . . ? C30 O1 Dy1 154.7(4) . . ? C19 O2 Dy1 149.6(5) . . ? C21 O6 Dy1 148.4(4) . 5_455 ? C29 O7 Dy1 150.8(5) . 5_455 ? C30 N1 C10 123.2(6) . . ? C30 N1 C1 111.1(6) . . ? C10 N1 C1 125.6(6) . . ? C19 N2 C2 113.8(6) . . ? C19 N2 C10 122.3(6) . . ? C2 N2 C10 123.7(6) . . ? C18 N3 C12 123.3(6) . . ? C18 N3 C2 111.1(7) . . ? C12 N3 C2 123.9(6) . . ? C15 N4 C12 123.4(6) . . ? C15 N4 C1 110.8(6) . . ? C12 N4 C1 125.7(6) . . ? C25 N5 C24 123.5(6) . . ? C25 N5 C16 111.6(5) . . ? C24 N5 C16 123.6(5) . . ? C25 N6 C27 112.4(5) . . ? C25 N6 C9 121.3(6) . . ? C27 N6 C9 123.6(6) . . ? C30 N7 C14 124.5(6) . . ? C30 N7 C23 109.5(6) . . ? C14 N7 C23 124.3(6) . . ? C8 N8 C6 110.8(6) . . ? C8 N8 C3 122.5(6) . . ? C6 N8 C3 125.4(5) . . ? C17 N9 C28 120.0(5) . . ? C17 N9 C16 112.7(5) . . ? C28 N9 C16 123.6(5) . . ? C18 N10 C4 112.8(6) . . ? C18 N10 C22 120.3(6) . . ? C4 N10 C22 126.9(7) . . ? C19 N11 C11 121.9(6) . . ? C19 N11 C4 110.6(6) . . ? C11 N11 C4 125.7(7) . . ? C8 N12 C13 113.0(5) . . ? C8 N12 C11 120.1(6) . . ? C13 N12 C11 126.5(6) . . ? C29 N13 C5 110.7(6) . . ? C29 N13 C24 122.6(6) . . ? C5 N13 C24 125.3(6) . . ? C29 N14 C7 124.5(6) . . ? C29 N14 C26 110.9(6) . . ? C7 N14 C26 124.5(6) . . ? C20 N15 C26 111.9(6) . . ? C20 N15 C3 121.2(6) . . ? C26 N15 C3 126.9(7) . . ? C21 N16 C7 126.7(6) . . ? C21 N16 C6 112.1(5) . . ? C7 N16 C6 121.2(5) . . ? C20 N17 C5 114.0(6) . . ? C20 N17 C28 121.0(5) . . ? C5 N17 C28 124.2(6) . . ? C21 N18 C22 122.9(6) . . ? C21 N18 C13 111.2(5) . . ? C22 N18 C13 124.1(6) . . ? C17 N19 C14 123.7(5) . . ? C17 N19 C27 112.1(5) . . ? C14 N19 C27 124.1(5) . . ? C15 N20 C9 124.3(5) . . ? C15 N20 C23 111.8(6) . . ? C9 N20 C23 123.7(6) . . ? N1 C1 N4 113.9(6) . . ? N1 C1 C23 103.4(5) . . ? N4 C1 C23 104.1(5) . . ? N1 C1 H1A 111.6 . . ? N4 C1 H1A 111.6 . . ? C23 C1 H1A 111.6 . . ? N2 C2 N3 114.9(6) . . ? N2 C2 C4 103.7(6) . . ? N3 C2 C4 102.1(5) . . ? N2 C2 H2A 111.8 . . ? N3 C2 H2A 111.8 . . ? C4 C2 H2A 111.8 . . ? N15 C3 N8 112.5(6) . . ? N15 C3 H3A 109.1 . . ? N8 C3 H3A 109.1 . . ? N15 C3 H3B 109.1 . . ? N8 C3 H3B 109.1 . . ? H3A C3 H3B 107.8 . . ? N10 C4 N11 115.4(5) . . ? N10 C4 C2 104.8(6) . . ? N11 C4 C2 103.5(6) . . ? N10 C4 H4A 110.9 . . ? N11 C4 H4A 110.9 . . ? C2 C4 H4A 110.9 . . ? N13 C5 N17 114.9(5) . . ? N13 C5 C26 104.9(6) . . ? N17 C5 C26 101.5(5) . . ? N13 C5 H5A 111.6 . . ? N17 C5 H5A 111.6 . . ? C26 C5 H5A 111.6 . . ? N8 C6 N16 115.1(6) . . ? N8 C6 C13 104.7(5) . . ? N16 C6 C13 104.0(5) . . ? N8 C6 H6A 110.9 . . ? N16 C6 H6A 110.9 . . ? C13 C6 H6A 110.9 . . ? O3 C8 N12 127.3(6) . . ? O3 C8 N8 124.8(6) . . ? N12 C8 N8 107.9(6) . . ? N20 C9 N6 114.9(6) . . ? N20 C9 H9A 108.5 . . ? N6 C9 H9A 108.5 . . ? N20 C9 H9B 108.5 . . ? N6 C9 H9B 108.5 . . ? H9A C9 H9B 107.5 . . ? N1 C10 N2 113.2(5) . . ? N1 C10 H10A 108.9 . . ? N2 C10 H10A 108.9 . . ? N1 C10 H10B 108.9 . . ? N2 C10 H10B 108.9 . . ? H10A C10 H10B 107.8 . . ? N11 C11 N12 110.5(6) . . ? N11 C11 H11A 109.5 . . ? N12 C11 H11A 109.5 . . ? N11 C11 H11B 109.6 . . ? N12 C11 H11B 109.5 . . ? H11A C11 H11B 108.1 . . ? N4 C12 N3 114.1(6) . . ? N4 C12 H12A 108.7 . . ? N3 C12 H12A 108.7 . . ? N4 C12 H12B 108.7 . . ? N3 C12 H12B 108.7 . . ? H12A C12 H12B 107.6 . . ? N12 C13 N18 113.1(6) . . ? N12 C13 C6 103.2(6) . . ? N18 C13 C6 101.9(5) . . ? N12 C13 H13A 112.6 . . ? N18 C13 H13A 112.6 . . ? C6 C13 H13A 112.6 . . ? N7 C14 N19 112.6(6) . . ? N7 C14 H14A 109.1 . . ? N19 C14 H14A 109.1 . . ? N7 C14 H14B 109.1 . . ? N19 C14 H14B 109.1 . . ? H14A C14 H14B 107.8 . . ? O10 C15 N20 124.6(6) . . ? O10 C15 N4 125.7(7) . . ? N20 C15 N4 109.6(6) . . ? N9 C16 N5 115.7(6) . . ? N9 C16 C27 103.7(5) . . ? N5 C16 C27 101.8(5) . . ? N9 C16 H16A 111.6 . . ? N5 C16 H16A 111.6 . . ? C27 C16 H16A 111.6 . . ? O4 C17 N9 125.4(6) . . ? O4 C17 N19 127.2(5) . . ? N9 C17 N19 107.3(5) . . ? O8 C18 N10 126.3(7) . . ? O8 C18 N3 125.0(7) . . ? N10 C18 N3 108.6(6) . . ? O2 C19 N2 127.8(7) . . ? O2 C19 N11 123.9(7) . . ? N2 C19 N11 108.2(6) . . ? O5 C20 N17 128.4(7) . . ? O5 C20 N15 125.0(7) . . ? N17 C20 N15 106.6(5) . . ? O6 C21 N16 126.2(5) . . ? O6 C21 N18 123.4(6) . . ? N16 C21 N18 110.4(6) . . ? N10 C22 N18 112.3(6) . . ? N10 C22 H22A 109.1 . . ? N18 C22 H22A 109.1 . . ? N10 C22 H22B 109.1 . . ? N18 C22 H22B 109.1 . . ? H22A C22 H22B 107.9 . . ? N20 C23 N7 113.7(5) . . ? N20 C23 C1 103.7(6) . . ? N7 C23 C1 103.2(6) . . ? N20 C23 H23A 111.9 . . ? N7 C23 H23A 111.9 . . ? C1 C23 H23A 111.9 . . ? N5 C24 N13 115.5(5) . . ? N5 C24 H24A 108.4 . . ? N13 C24 H24A 108.4 . . ? N5 C24 H24B 108.4 . . ? N13 C24 H24B 108.4 . . ? H24A C24 H24B 107.5 . . ? O9 C25 N6 127.1(6) . . ? O9 C25 N5 124.4(6) . . ? N6 C25 N5 108.4(6) . . ? N15 C26 N14 115.2(5) . . ? N15 C26 C5 105.8(6) . . ? N14 C26 C5 101.6(5) . . ? N15 C26 H26A 111.2 . . ? N14 C26 H26A 111.2 . . ? C5 C26 H26A 111.2 . . ? N6 C27 N19 114.7(5) . . ? N6 C27 C16 105.1(5) . . ? N19 C27 C16 103.4(5) . . ? N6 C27 H27A 111.1 . . ? N19 C27 H27A 111.1 . . ? C16 C27 H27A 111.1 . . ? N9 C28 N17 114.1(6) . . ? N9 C28 H28A 108.7 . . ? N17 C28 H28A 108.7 . . ? N9 C28 H28B 108.7 . . ? N17 C28 H28B 108.8 . . ? H28A C28 H28B 107.6 . . ? O7 C29 N13 123.6(7) . . ? O7 C29 N14 124.8(7) . . ? N13 C29 N14 111.6(6) . . ? O1 C30 N1 125.0(6) . . ? O1 C30 N7 122.4(6) . . ? N1 C30 N7 112.6(6) . . ? N16 C7 N14 113.3(5) . . ? N16 C7 H7A 108.9 . . ? N14 C7 H7A 108.9 . . ? N16 C7 H7B 108.9 . . ? N14 C7 H7B 108.9 . . ? H7A C7 H7B 107.7 . . ? O11 C36 C35 113.7(6) . . ? O11 C36 C31 126.3(6) . . ? C35 C36 C31 120.0 . . ? C34 C35 C36 120.0 . . ? C34 C35 H35A 120.0 . . ? C36 C35 H35A 120.0 . . ? C35 C34 C33 120.0 . . ? C35 C34 H34A 120.0 . . ? C33 C34 H34A 120.0 . . ? O12 C33 C32 121.6(9) . . ? O12 C33 C34 118.4(9) . . ? C32 C33 C34 120.0 . . ? C31 C32 C33 120.0 . . ? C31 C32 H32A 120.0 . . ? C33 C32 H32A 120.0 . . ? C32 C31 C36 120.0 . . ? C32 C31 H31A 120.0 . . ? C36 C31 H31A 120.0 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.123 _refine_diff_density_min -0.821 _refine_diff_density_rms 0.145