# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2004 data_global _journal_coden_Cambridge 182 # PART1: TITLE&AUTHORS (manual editing) _publ_contact_author_name 'Hermann, Petr' _publ_contact_author_address ; Dept. of Inorganic Chemistry, Faculty of Science, Charles University Hlavova 2030 128 40 Prague 2 Czech Republic ; _publ_contact_author_email petrh@natur.cuni.cz _publ_requested_journal Chem.Commun _publ_section_title ; Lanthanide(III) complexes of a pyridine N-oxide analogue of DOTA: exclusive M isomer formation induced by six-membered chelate ring ; loop_ _publ_author_name _publ_author_address 'Polasek, Miloslav' ; Dept. of Inorganic Chemistry, Charles University Hlavova 2030 128 40 Prague 2 Czech Republic ; 'Rudovsky, Jakub' ; Dept. of Inorganic Chemistry, Charles University Hlavova 2030 128 40 Prague 2 Czech Republic ; 'Hermann, Petr' ; Dept. of Inorganic Chemistry, Charles University Hlavova 2030 128 40 Prague 2 Czech Republic ; 'Lukes, Ivan' ; Dept. of Inorganic Chemistry, Charles University Hlavova 2030 128 40 Prague 2 Czech Republic ; 'Vander Elst, Luce' ; Dept. of Organic Chemistry, University of Mons-Hainaut Avenue du champ de Mars 24 B-7000 Mons Belgium ; 'Muller, Robert N.' ; Dept. of Organic Chemistry, University of Mons-Hainaut Avenue du champ de Mars 24 B-7000 Mons Belgium ; _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, p. 435. Coppens, P. (1970). Crystallographic Computing, edited by F.R. Ahmed, S.R.Hall & C.P. Huber, pp. 255-270, Copenhagen, Munksgaard. Hooft, R.W. (1998). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods Enzymol. 276, 307--326. Sheldrick, G. M. (1997). SHELXL97. University of G\"ottingen, Germany. Spek, A.L. (1999). PLATON. Version 1999. Utrecht University, The Netherlands. ; data_dypol _database_code_depnum_ccdc_archive 'CCDC 244292' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H28 Dy N5 O7, 3(H2O)' _chemical_formula_sum 'C20 H34 Dy N5 O10' _chemical_formula_weight 667.02 _chemical_compound_source 'synthesized by the authors' 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 triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.29510(10) _cell_length_b 10.7100(2) _cell_length_c 15.7375(3) _cell_angle_alpha 82.0772(12) _cell_angle_beta 86.8978(12) _cell_angle_gamma 90.0588(10) _cell_volume 1216.03(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 16569 _cell_measurement_theta_min 1 _cell_measurement_theta_max 27.5 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.822 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 670 _exptl_absorpt_coefficient_mu 3.137 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.246 _exptl_absorpt_correction_T_max 0.537 _exptl_absorpt_process_details ; Gaussian integration (Coppens, 1970) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius KappaCCD area detector' _diffrn_measurement_method '\f and \w scans to fill the Ewald sphere' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21215 _diffrn_reflns_av_R_equivalents 0.0404 _diffrn_reflns_av_sigmaI/netI 0.0277 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 27.53 _reflns_number_total 5585 _reflns_number_gt 5478 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)' _computing_cell_refinement 'COLLECT and DENZO' _computing_data_reduction 'COLLECT and DENZO' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0182P)^2^+1.2995P] where P==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5585 _refine_ls_number_parameters 471 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0192 _refine_ls_R_factor_gt 0.0181 _refine_ls_wR_factor_ref 0.0463 _refine_ls_wR_factor_gt 0.0460 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.088 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 0.463236(11) 0.153074(8) 0.699536(5) 0.01132(4) Uani 1 1 d . . . N1 N 0.7622(2) 0.03662(16) 0.74499(12) 0.0152(3) Uani 1 1 d . . . C2 C 0.7961(3) 0.0631(2) 0.83335(14) 0.0183(4) Uani 1 1 d . . . H21 H 0.915(4) 0.042(3) 0.8465(18) 0.022(7) Uiso 1 1 d . . . H22 H 0.716(3) 0.011(2) 0.8728(17) 0.015(6) Uiso 1 1 d . . . C3 C 0.7665(3) 0.2003(2) 0.84371(15) 0.0185(4) Uani 1 1 d . . . H31 H 0.802(4) 0.212(2) 0.8981(19) 0.020(7) Uiso 1 1 d . . . H32 H 0.845(4) 0.253(3) 0.8072(18) 0.017(6) Uiso 1 1 d . . . N4 N 0.5734(2) 0.24066(16) 0.83246(11) 0.0147(3) Uani 1 1 d . . . C5 C 0.5627(3) 0.38072(19) 0.82046(14) 0.0163(4) Uani 1 1 d . . . H51 H 0.635(4) 0.414(2) 0.8642(18) 0.018(6) Uiso 1 1 d . . . H52 H 0.437(4) 0.403(2) 0.8305(17) 0.014(6) Uiso 1 1 d . . . C6 C 0.6326(3) 0.4388(2) 0.73088(14) 0.0163(4) Uani 1 1 d . . . H61 H 0.624(4) 0.530(3) 0.7242(18) 0.021(7) Uiso 1 1 d . . . H62 H 0.759(3) 0.422(2) 0.7231(16) 0.012(6) Uiso 1 1 d . . . N7 N 0.5327(2) 0.39156(16) 0.66190(11) 0.0142(3) Uani 1 1 d . . . C8 C 0.6453(3) 0.4172(2) 0.57973(14) 0.0167(4) Uani 1 1 d . . . H81 H 0.706(4) 0.503(3) 0.5722(18) 0.022(7) Uiso 1 1 d . . . H82 H 0.569(3) 0.416(2) 0.5325(17) 0.014(6) Uiso 1 1 d . . . C9 C 0.7945(3) 0.3202(2) 0.57428(14) 0.0173(4) Uani 1 1 d . . . H91 H 0.869(4) 0.340(3) 0.5206(19) 0.023(7) Uiso 1 1 d . . . H92 H 0.872(4) 0.322(2) 0.6210(19) 0.019(7) Uiso 1 1 d . . . N10 N 0.7170(2) 0.19058(17) 0.57810(11) 0.0147(3) Uani 1 1 d . . . C11 C 0.8682(3) 0.0982(2) 0.59220(15) 0.0179(4) Uani 1 1 d . . . H111 H 0.970(4) 0.124(3) 0.557(2) 0.027(7) Uiso 1 1 d . . . H112 H 0.825(4) 0.017(3) 0.5771(19) 0.023(7) Uiso 1 1 d . . . C12 C 0.9200(3) 0.0832(2) 0.68497(15) 0.0177(4) Uani 1 1 d . . . H121 H 1.022(4) 0.021(3) 0.6946(18) 0.020(7) Uiso 1 1 d . . . H122 H 0.961(3) 0.159(2) 0.6989(14) 0.009(6) Uiso 1 1 d . . . C20 C 0.7551(3) -0.1027(2) 0.74515(15) 0.0187(4) Uani 1 1 d . . . H201 H 0.853(3) -0.141(2) 0.7759(17) 0.014(6) Uiso 1 1 d . . . H202 H 0.771(4) -0.114(2) 0.6853(18) 0.017(6) Uiso 1 1 d . . . C21 C 0.5805(3) -0.1692(2) 0.77826(15) 0.0190(4) Uani 1 1 d . . . N22 N 0.4305(3) -0.14574(17) 0.73122(12) 0.0175(4) Uani 1 1 d . . . O22N O 0.4343(2) -0.05018(14) 0.66650(10) 0.0180(3) Uani 1 1 d . . . C23 C 0.2744(3) -0.2139(2) 0.74908(17) 0.0232(5) Uani 1 1 d . . . H231 H 0.188(4) -0.192(3) 0.714(2) 0.032(8) Uiso 1 1 d . . . C24 C 0.2597(4) -0.3058(2) 0.81931(18) 0.0296(6) Uani 1 1 d . . . H241 H 0.156(4) -0.351(3) 0.828(2) 0.034(8) Uiso 1 1 d . . . C25 C 0.4061(4) -0.3286(2) 0.87154(18) 0.0309(6) Uani 1 1 d . . . H251 H 0.393(4) -0.383(3) 0.921(2) 0.039(9) Uiso 1 1 d . . . C26 C 0.5676(4) -0.2609(2) 0.84966(17) 0.0254(5) Uani 1 1 d . . . H261 H 0.662(4) -0.273(3) 0.874(2) 0.025(8) Uiso 1 1 d . . . C30 C 0.4548(3) 0.1880(2) 0.90880(15) 0.0201(4) Uani 1 1 d . . . H301 H 0.376(4) 0.246(3) 0.9218(19) 0.025(7) Uiso 1 1 d . . . H302 H 0.521(4) 0.170(3) 0.957(2) 0.027(7) Uiso 1 1 d . . . C31 C 0.3474(3) 0.0701(2) 0.89752(14) 0.0171(4) Uani 1 1 d . . . O311 O 0.3524(2) 0.03583(14) 0.82348(10) 0.0183(3) Uani 1 1 d . . . O312 O 0.2586(2) 0.01529(16) 0.96174(11) 0.0239(3) Uani 1 1 d . . . C40 C 0.3527(3) 0.4547(2) 0.65275(16) 0.0188(4) Uani 1 1 d . . . H401 H 0.306(4) 0.449(3) 0.590(2) 0.029(8) Uiso 1 1 d . . . H402 H 0.361(4) 0.545(3) 0.6567(18) 0.023(7) Uiso 1 1 d . . . C41 C 0.2027(3) 0.3904(2) 0.71433(15) 0.0186(4) Uani 1 1 d . . . O411 O 0.2231(2) 0.27445(14) 0.74220(10) 0.0178(3) Uani 1 1 d . . . O412 O 0.0663(2) 0.45389(16) 0.73150(15) 0.0369(5) Uani 1 1 d . . . C50 C 0.6306(3) 0.1777(2) 0.49647(14) 0.0181(4) Uani 1 1 d . . . H501 H 0.633(4) 0.086(3) 0.4894(18) 0.021(7) Uiso 1 1 d . . . H502 H 0.693(4) 0.220(3) 0.452(2) 0.032(8) Uiso 1 1 d . . . C51 C 0.4285(3) 0.2166(2) 0.49617(14) 0.0168(4) Uani 1 1 d . . . O511 O 0.3389(2) 0.19964(15) 0.56913(10) 0.0193(3) Uani 1 1 d . . . O512 O 0.3654(2) 0.25948(16) 0.42707(11) 0.0247(4) Uani 1 1 d . . . O1W O 0.0110(3) 0.3085(2) 0.37044(15) 0.0313(4) Uani 1 1 d . . . H1W1 H 0.004(4) 0.375(3) 0.347(2) 0.034(9) Uiso 1 1 d . . . H1W2 H 0.110(6) 0.305(4) 0.387(3) 0.051(11) Uiso 1 1 d . . . O2W O 0.0153(3) 0.17596(18) 1.03917(13) 0.0289(4) Uani 1 1 d . . . H2W1 H 0.079(6) 0.135(4) 1.021(3) 0.053(12) Uiso 1 1 d . . . H2W2 H -0.083(5) 0.129(3) 1.051(2) 0.039(9) Uiso 1 1 d . . . O3WA O 0.0789(6) 0.4085(4) 0.9305(3) 0.0347(10) Uani 0.45 1 d P . . O3WB O 0.1589(7) 0.4182(5) 0.9994(4) 0.0463(12) Uani 0.45 1 d P . . O3WC O -0.093(2) 0.5097(16) 0.8753(11) 0.023(3) Uani 0.10 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.01180(5) 0.01241(6) 0.00964(6) -0.00103(4) -0.00084(4) 0.00187(3) N1 0.0163(8) 0.0150(8) 0.0150(9) -0.0038(7) -0.0026(7) 0.0032(7) C2 0.0213(10) 0.0201(11) 0.0138(10) -0.0010(8) -0.0068(8) 0.0050(8) C3 0.0215(10) 0.0195(10) 0.0156(11) -0.0042(8) -0.0063(9) 0.0028(8) N4 0.0177(8) 0.0139(8) 0.0124(8) -0.0008(6) -0.0008(7) 0.0019(6) C5 0.0209(10) 0.0141(10) 0.0145(10) -0.0036(8) -0.0014(8) 0.0017(8) C6 0.0176(10) 0.0143(10) 0.0171(10) -0.0025(8) -0.0020(8) -0.0003(8) N7 0.0127(8) 0.0160(8) 0.0134(9) -0.0003(7) -0.0004(6) 0.0015(6) C8 0.0198(10) 0.0160(10) 0.0134(10) 0.0005(8) -0.0003(8) -0.0011(8) C9 0.0172(10) 0.0203(10) 0.0144(10) -0.0030(8) 0.0011(8) -0.0033(8) N10 0.0145(8) 0.0176(8) 0.0128(8) -0.0044(7) -0.0023(6) 0.0013(7) C11 0.0149(9) 0.0225(11) 0.0169(11) -0.0053(8) 0.0001(8) 0.0044(8) C12 0.0125(9) 0.0219(11) 0.0195(11) -0.0047(9) -0.0041(8) 0.0038(8) C20 0.0203(10) 0.0157(10) 0.0211(11) -0.0049(8) -0.0042(9) 0.0070(8) C21 0.0254(11) 0.0143(10) 0.0189(11) -0.0075(8) -0.0028(9) 0.0064(8) N22 0.0240(9) 0.0129(8) 0.0165(9) -0.0051(7) -0.0016(7) 0.0037(7) O22N 0.0257(8) 0.0145(7) 0.0146(8) -0.0036(6) -0.0050(6) 0.0035(6) C23 0.0240(11) 0.0190(11) 0.0279(13) -0.0093(9) 0.0006(10) 0.0016(9) C24 0.0347(13) 0.0200(11) 0.0341(14) -0.0078(10) 0.0076(11) -0.0029(10) C25 0.0480(16) 0.0176(11) 0.0254(13) -0.0005(10) 0.0069(12) 0.0030(10) C26 0.0353(13) 0.0190(11) 0.0227(12) -0.0046(9) -0.0049(10) 0.0072(10) C30 0.0300(12) 0.0189(11) 0.0112(10) -0.0025(8) 0.0019(9) 0.0007(9) C31 0.0195(10) 0.0154(10) 0.0158(10) 0.0000(8) 0.0004(8) 0.0049(8) O311 0.0262(8) 0.0149(7) 0.0136(7) -0.0029(6) 0.0027(6) 0.0003(6) O312 0.0301(9) 0.0241(8) 0.0161(8) 0.0000(6) 0.0059(7) -0.0018(7) C40 0.0162(10) 0.0150(10) 0.0241(12) 0.0023(8) -0.0026(9) 0.0040(8) C41 0.0126(9) 0.0190(10) 0.0250(12) -0.0046(9) -0.0036(8) 0.0006(8) O411 0.0152(7) 0.0146(7) 0.0234(8) -0.0028(6) 0.0015(6) 0.0018(5) O412 0.0151(8) 0.0190(8) 0.0746(15) -0.0039(9) 0.0078(9) 0.0046(6) C50 0.0196(10) 0.0239(11) 0.0111(10) -0.0030(8) -0.0019(8) 0.0006(8) C51 0.0209(10) 0.0154(10) 0.0153(10) -0.0037(8) -0.0069(8) 0.0014(8) O511 0.0174(7) 0.0258(8) 0.0144(8) -0.0002(6) -0.0043(6) 0.0001(6) O512 0.0320(9) 0.0279(9) 0.0153(8) -0.0027(6) -0.0097(7) 0.0087(7) O1W 0.0219(9) 0.0296(11) 0.0417(12) -0.0013(9) -0.0053(8) -0.0020(8) O2W 0.0316(10) 0.0224(9) 0.0326(10) -0.0036(8) -0.0004(8) 0.0048(8) O3WA 0.048(3) 0.0161(18) 0.038(3) -0.0006(17) 0.005(2) -0.0061(17) O3WB 0.042(3) 0.034(2) 0.062(3) -0.007(2) 0.009(2) 0.006(2) O3WC 0.021(8) 0.024(8) 0.026(9) -0.009(7) -0.006(7) -0.010(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 O311 2.2777(15) . ? Dy1 O511 2.2810(15) . ? Dy1 O411 2.3080(14) . ? Dy1 O22N 2.3188(15) . ? Dy1 N4 2.5735(18) . ? Dy1 N10 2.5776(17) . ? Dy1 N7 2.5845(18) . ? Dy1 N1 2.5983(17) . ? N1 C12 1.489(3) . ? N1 C2 1.490(3) . ? N1 C20 1.492(3) . ? C2 C3 1.515(3) . ? C2 H21 0.92(3) . ? C2 H22 0.95(3) . ? C3 N4 1.487(3) . ? C3 H31 0.93(3) . ? C3 H32 0.92(3) . ? N4 C30 1.486(3) . ? N4 C5 1.489(3) . ? C5 C6 1.522(3) . ? C5 H51 0.99(3) . ? C5 H52 0.96(3) . ? C6 N7 1.484(3) . ? C6 H61 0.97(3) . ? C6 H62 0.95(3) . ? N7 C40 1.483(3) . ? N7 C8 1.486(3) . ? C8 C9 1.512(3) . ? C8 H81 1.01(3) . ? C8 H82 0.95(3) . ? C9 N10 1.491(3) . ? C9 H91 0.98(3) . ? C9 H92 0.95(3) . ? N10 C50 1.484(3) . ? N10 C11 1.488(3) . ? C11 C12 1.515(3) . ? C11 H111 0.92(3) . ? C11 H112 0.98(3) . ? C12 H121 1.01(3) . ? C12 H122 0.92(2) . ? C20 C21 1.492(3) . ? C20 H201 0.95(3) . ? C20 H202 0.97(3) . ? C21 N22 1.358(3) . ? C21 C26 1.385(3) . ? N22 O22N 1.340(2) . ? N22 C23 1.348(3) . ? C23 C24 1.374(4) . ? C23 H231 0.87(3) . ? C24 C25 1.385(4) . ? C24 H241 0.89(3) . ? C25 C26 1.384(4) . ? C25 H251 0.91(3) . ? C26 H261 0.81(3) . ? C30 C31 1.521(3) . ? C30 H301 0.89(3) . ? C30 H302 0.92(3) . ? C31 O312 1.245(3) . ? C31 O311 1.268(3) . ? C40 C41 1.520(3) . ? C40 H401 1.07(3) . ? C40 H402 0.98(3) . ? C41 O412 1.245(3) . ? C41 O411 1.270(3) . ? C50 C51 1.533(3) . ? C50 H501 1.00(3) . ? C50 H502 0.89(3) . ? C51 O512 1.234(3) . ? C51 O511 1.280(3) . ? O1W H1W1 0.76(4) . ? O1W H1W2 0.78(4) . ? O2W H2W1 0.72(4) . ? O2W H2W2 0.87(4) . ? O3WA O3WB 1.275(7) . ? 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 O311 Dy1 O511 131.08(6) . . ? O311 Dy1 O411 77.79(5) . . ? O511 Dy1 O411 82.35(6) . . ? O311 Dy1 O22N 74.71(5) . . ? O511 Dy1 O22N 81.30(6) . . ? O411 Dy1 O22N 124.95(5) . . ? O311 Dy1 N4 68.61(6) . . ? O511 Dy1 N4 146.00(6) . . ? O411 Dy1 N4 75.27(6) . . ? O22N Dy1 N4 132.60(5) . . ? O311 Dy1 N10 148.56(6) . . ? O511 Dy1 N10 69.21(5) . . ? O411 Dy1 N10 133.06(5) . . ? O22N Dy1 N10 87.63(6) . . ? N4 Dy1 N10 108.83(6) . . ? O311 Dy1 N7 131.50(5) . . ? O511 Dy1 N7 77.85(6) . . ? O411 Dy1 N7 67.91(5) . . ? O22N Dy1 N7 153.66(6) . . ? N4 Dy1 N7 70.20(6) . . ? N10 Dy1 N7 70.04(5) . . ? O311 Dy1 N1 80.87(6) . . ? O511 Dy1 N1 131.73(6) . . ? O411 Dy1 N1 145.49(6) . . ? O22N Dy1 N1 73.69(5) . . ? N4 Dy1 N1 71.80(6) . . ? N10 Dy1 N1 69.15(6) . . ? N7 Dy1 N1 109.17(6) . . ? C12 N1 C2 109.90(17) . . ? C12 N1 C20 105.84(16) . . ? C2 N1 C20 108.94(17) . . ? C12 N1 Dy1 110.55(12) . . ? C2 N1 Dy1 107.16(12) . . ? C20 N1 Dy1 114.43(13) . . ? N1 C2 C3 112.49(18) . . ? N1 C2 H21 110.0(18) . . ? C3 C2 H21 108.3(18) . . ? N1 C2 H22 108.0(16) . . ? C3 C2 H22 110.2(15) . . ? H21 C2 H22 108(2) . . ? N4 C3 C2 112.90(18) . . ? N4 C3 H31 110.2(16) . . ? C2 C3 H31 108.0(16) . . ? N4 C3 H32 109.9(16) . . ? C2 C3 H32 111.9(17) . . ? H31 C3 H32 103(2) . . ? C30 N4 C3 110.21(17) . . ? C30 N4 C5 109.47(16) . . ? C3 N4 C5 110.11(17) . . ? C30 N4 Dy1 108.88(13) . . ? C3 N4 Dy1 107.67(13) . . ? C5 N4 Dy1 110.47(12) . . ? N4 C5 C6 112.12(17) . . ? N4 C5 H51 109.0(15) . . ? C6 C5 H51 110.0(15) . . ? N4 C5 H52 107.8(15) . . ? C6 C5 H52 110.0(15) . . ? H51 C5 H52 108(2) . . ? N7 C6 C5 112.81(17) . . ? N7 C6 H61 108.8(17) . . ? C5 C6 H61 110.9(16) . . ? N7 C6 H62 109.2(16) . . ? C5 C6 H62 109.6(15) . . ? H61 C6 H62 105(2) . . ? C40 N7 C6 110.28(17) . . ? C40 N7 C8 109.83(17) . . ? C6 N7 C8 109.03(16) . . ? C40 N7 Dy1 106.39(12) . . ? C6 N7 Dy1 110.85(12) . . ? C8 N7 Dy1 110.43(12) . . ? N7 C8 C9 111.46(17) . . ? N7 C8 H81 112.0(16) . . ? C9 C8 H81 107.9(16) . . ? N7 C8 H82 109.8(15) . . ? C9 C8 H82 108.7(15) . . ? H81 C8 H82 107(2) . . ? N10 C9 C8 111.77(17) . . ? N10 C9 H91 108.3(16) . . ? C8 C9 H91 110.5(16) . . ? N10 C9 H92 108.8(16) . . ? C8 C9 H92 109.1(16) . . ? H91 C9 H92 108(2) . . ? C50 N10 C11 110.07(17) . . ? C50 N10 C9 109.86(17) . . ? C11 N10 C9 108.65(17) . . ? C50 N10 Dy1 107.28(12) . . ? C11 N10 Dy1 111.47(13) . . ? C9 N10 Dy1 109.50(12) . . ? N10 C11 C12 110.48(17) . . ? N10 C11 H111 110.6(18) . . ? C12 C11 H111 109.3(19) . . ? N10 C11 H112 107.8(16) . . ? C12 C11 H112 110.5(17) . . ? H111 C11 H112 108(2) . . ? N1 C12 C11 111.65(18) . . ? N1 C12 H121 107.4(15) . . ? C11 C12 H121 110.6(16) . . ? N1 C12 H122 109.0(14) . . ? C11 C12 H122 110.4(14) . . ? H121 C12 H122 108(2) . . ? N1 C20 C21 117.26(17) . . ? N1 C20 H201 109.8(16) . . ? C21 C20 H201 108.9(15) . . ? N1 C20 H202 105.0(16) . . ? C21 C20 H202 105.9(16) . . ? H201 C20 H202 110(2) . . ? N22 C21 C26 118.6(2) . . ? N22 C21 C20 117.6(2) . . ? C26 C21 C20 123.6(2) . . ? O22N N22 C23 118.38(19) . . ? O22N N22 C21 119.72(18) . . ? C23 N22 C21 121.9(2) . . ? N22 O22N Dy1 118.04(12) . . ? N22 C23 C24 120.2(2) . . ? N22 C23 H231 114(2) . . ? C24 C23 H231 126(2) . . ? C23 C24 C25 119.8(3) . . ? C23 C24 H241 117(2) . . ? C25 C24 H241 123(2) . . ? C26 C25 C24 118.8(2) . . ? C26 C25 H251 121(2) . . ? C24 C25 H251 120(2) . . ? C25 C26 C21 120.6(3) . . ? C25 C26 H261 125(2) . . ? C21 C26 H261 114(2) . . ? N4 C30 C31 114.48(18) . . ? N4 C30 H301 109.2(19) . . ? C31 C30 H301 108.4(19) . . ? N4 C30 H302 112.2(18) . . ? C31 C30 H302 107.9(18) . . ? H301 C30 H302 104(3) . . ? O312 C31 O311 124.7(2) . . ? O312 C31 C30 117.4(2) . . ? O311 C31 C30 117.92(19) . . ? C31 O311 Dy1 125.65(14) . . ? N7 C40 C41 112.85(17) . . ? N7 C40 H401 109.6(16) . . ? C41 C40 H401 104.7(16) . . ? N7 C40 H402 112.0(16) . . ? C41 C40 H402 111.7(16) . . ? H401 C40 H402 105(2) . . ? O412 C41 O411 124.8(2) . . ? O412 C41 C40 117.7(2) . . ? O411 C41 C40 117.47(18) . . ? C41 O411 Dy1 124.37(14) . . ? N10 C50 C51 113.48(18) . . ? N10 C50 H501 107.5(16) . . ? C51 C50 H501 106.1(16) . . ? N10 C50 H502 112(2) . . ? C51 C50 H502 110(2) . . ? H501 C50 H502 108(3) . . ? O512 C51 O511 125.7(2) . . ? O512 C51 C50 118.4(2) . . ? O511 C51 C50 115.87(18) . . ? C51 O511 Dy1 125.80(13) . . ? H1W1 O1W H1W2 105(4) . . ? H2W1 O2W H2W2 103(4) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.635 _refine_diff_density_min -1.435 _refine_diff_density_rms 0.107 #======END