Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 loop_ _publ_author_name 'Christine Tedeschi' 'Joelle Azema' 'Heinz Gornitzka' 'Pierre Tisnes' 'Claude Picard' _publ_contact_author_name 'Dr Claude Picard' _publ_contact_author_address ; Universite Paul Sabatier Laboratoire de synthese et de physicochimie de molecules d'interet biologique-UM 118, route de Narbonne TOULOUSE cedex4 31062 FRANCE ; _publ_contact_author_email PICARD@CHIMIE.UPS-TLSE.FR _publ_section_title ; A solid-state study of eight-co-ordinate lanthanide (III) complexes (Ln == Eu, Gd, Tb, Dy) with 1-hydroxy-2-pyridinone ; data_1 _database_code_CSD 200686 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H50 Eu2 N8 Na2 O25' _chemical_formula_weight 1392.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 14.1076(5) _cell_length_b 19.1111(7) _cell_length_c 19.2936(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5201.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 6676 _cell_measurement_theta_min 2.77 _cell_measurement_theta_max 33.67 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.6 _exptl_crystal_size_min 0.7 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.778 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2776 _exptl_absorpt_coefficient_mu 2.499 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 '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_% ? _diffrn_reflns_number 71439 _diffrn_reflns_av_R_equivalents 0.0582 _diffrn_reflns_av_sigmaI/netI 0.0410 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 33.14 _reflns_number_total 19598 _reflns_number_gt 16970 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0348P)^2^+1.3063P] 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 mixed _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 -0.021(6) _refine_ls_number_reflns 19598 _refine_ls_number_parameters 748 _refine_ls_number_restraints 102 _refine_ls_R_factor_all 0.0403 _refine_ls_R_factor_gt 0.0315 _refine_ls_wR_factor_ref 0.0713 _refine_ls_wR_factor_gt 0.0670 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.005 _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 Eu1 Eu 0.812752(9) 0.672921(6) 0.266817(6) 0.01606(3) Uani 1 1 d . . . Eu2 Eu 0.315922(9) 0.668142(6) 0.229546(6) 0.01607(3) Uani 1 1 d . . . Na1 Na 0.57911(7) 0.72225(6) 0.23101(7) 0.0234(2) Uani 1 1 d . . . Na2 Na 0.05533(8) 0.63154(6) 0.18724(6) 0.0268(2) Uani 1 1 d . . . O1 O 0.88220(15) 0.77075(11) 0.32544(12) 0.0253(4) Uani 1 1 d . . . O2 O 0.70036(14) 0.75601(10) 0.31182(11) 0.0238(4) Uani 1 1 d . . . N1 N 0.82546(17) 0.82302(12) 0.34617(12) 0.0235(4) Uani 1 1 d . . . C1 C 0.7295(2) 0.81427(15) 0.33723(14) 0.0207(5) Uani 1 1 d . . . C2 C 0.6710(2) 0.87086(16) 0.35570(17) 0.0303(6) Uani 1 1 d . . . H2 H 0.6043 0.8672 0.3501 0.036 Uiso 1 1 calc R . . C3 C 0.7096(3) 0.93147(18) 0.3819(2) 0.0388(8) Uani 1 1 d . . . H3 H 0.6696 0.9701 0.3923 0.047 Uiso 1 1 calc R . . C4 C 0.8074(3) 0.93667(18) 0.3933(2) 0.0409(8) Uani 1 1 d . . . H4 H 0.8340 0.9775 0.4136 0.049 Uiso 1 1 calc R . . C5 C 0.8635(3) 0.88173(17) 0.37472(18) 0.0334(7) Uani 1 1 d . . . H5 H 0.9300 0.8845 0.3818 0.040 Uiso 1 1 calc R . . O3 O 0.91293(14) 0.69933(11) 0.17181(10) 0.0213(4) Uani 1 1 d . . . O4 O 0.73070(14) 0.71947(12) 0.16785(11) 0.0243(4) Uani 1 1 d . . . C6 C 0.87149(18) 0.71416(13) 0.11075(13) 0.0142(4) Uani 1 1 d . . . N2 N 0.7761(2) 0.72528(14) 0.11011(14) 0.0268(5) Uani 1 1 d . . . C7 C 0.7333(2) 0.74309(16) 0.04686(16) 0.0253(6) Uani 1 1 d . . . H7 H 0.6673 0.7532 0.0455 0.030 Uiso 1 1 calc R . . C8 C 0.7855(3) 0.74612(17) -0.01302(15) 0.0293(7) Uani 1 1 d . . . H8 H 0.7561 0.7576 -0.0558 0.035 Uiso 1 1 calc R . . C9 C 0.8830(3) 0.73200(19) -0.01024(18) 0.0321(7) Uani 1 1 d . . . H9 H 0.9196 0.7320 -0.0516 0.039 Uiso 1 1 calc R . . C10 C 0.9249(2) 0.71826(16) 0.05155(16) 0.0265(6) Uani 1 1 d . . . H10 H 0.9915 0.7114 0.0538 0.032 Uiso 1 1 calc R . . O5 O 0.80022(15) 0.56550(11) 0.20291(13) 0.0315(5) Uani 1 1 d . . . O6 O 0.66091(13) 0.61785(10) 0.27409(11) 0.0236(4) Uani 1 1 d . . . N3 N 0.64882(17) 0.55627(13) 0.24260(13) 0.0244(5) Uani 1 1 d . . . C11 C 0.7232(2) 0.52913(15) 0.20507(16) 0.0245(6) Uani 1 1 d . . . C12 C 0.7095(3) 0.46472(17) 0.1727(2) 0.0372(8) Uani 1 1 d . . . H12 H 0.7591 0.4452 0.1455 0.045 Uiso 1 1 calc R . . C13 C 0.6257(3) 0.4290(2) 0.1793(2) 0.0482(10) Uani 1 1 d . . . H13 H 0.6180 0.3847 0.1577 0.058 Uiso 1 1 calc R . . C14 C 0.5524(3) 0.4576(2) 0.2176(2) 0.0459(9) Uani 1 1 d . . . H14 H 0.4942 0.4330 0.2226 0.055 Uiso 1 1 calc R . . C15 C 0.5644(2) 0.52150(19) 0.24819(17) 0.0327(7) Uani 1 1 d . . . H15 H 0.5137 0.5419 0.2735 0.039 Uiso 1 1 calc R . . O7 O 0.82411(15) 0.61125(11) 0.37427(10) 0.0242(4) Uani 1 1 d . . . O8 O 0.97004(14) 0.63691(11) 0.29608(11) 0.0238(4) Uani 1 1 d . . . C16 C 0.90882(19) 0.60330(14) 0.40190(14) 0.0180(5) Uani 1 1 d . . . N4 N 0.98579(18) 0.61724(14) 0.36055(13) 0.0254(5) Uani 1 1 d . . . C17 C 1.0762(2) 0.61260(17) 0.38787(17) 0.0277(6) Uani 1 1 d . . . H17 H 1.1295 0.6230 0.3596 0.033 Uiso 1 1 calc R . . C18 C 1.0892(3) 0.59302(19) 0.45557(19) 0.0352(7) Uani 1 1 d . . . H18 H 1.1514 0.5903 0.4742 0.042 Uiso 1 1 calc R . . C19 C 1.0112(3) 0.57717(19) 0.49696(18) 0.0356(8) Uani 1 1 d . . . H19 H 1.0198 0.5632 0.5438 0.043 Uiso 1 1 calc R . . C20 C 0.9222(2) 0.58194(17) 0.46926(16) 0.0300(6) Uani 1 1 d . . . H20 H 0.8688 0.5703 0.4970 0.036 Uiso 1 1 calc R . . O9 O 0.46570(14) 0.65056(11) 0.17435(10) 0.0217(4) Uani 1 1 d . . . O10 O 0.30778(15) 0.61538(11) 0.11607(10) 0.0234(4) Uani 1 1 d . . . C21 C 0.38465(19) 0.61115(14) 0.07866(14) 0.0189(5) Uani 1 1 d . . . N5 N 0.46860(19) 0.62842(13) 0.11004(14) 0.0259(5) Uani 1 1 d . . . C22 C 0.5528(2) 0.62354(17) 0.07337(18) 0.0302(6) Uani 1 1 d . . . H22 H 0.6111 0.6334 0.0960 0.036 Uiso 1 1 calc R . . C23 C 0.5529(3) 0.6047(2) 0.00518(19) 0.0394(8) Uani 1 1 d . . . H23 H 0.6107 0.6025 -0.0199 0.047 Uiso 1 1 calc R . . C24 C 0.4670(3) 0.5887(2) -0.02743(18) 0.0400(8) Uani 1 1 d . . . H24 H 0.4660 0.5759 -0.0750 0.048 Uiso 1 1 calc R . . C25 C 0.3843(3) 0.59151(17) 0.00975(16) 0.0299(6) Uani 1 1 d . . . H25 H 0.3261 0.5799 -0.0121 0.036 Uiso 1 1 calc R . . O11 O 0.33373(14) 0.77992(11) 0.17665(11) 0.0231(4) Uani 1 1 d . . . O12 O 0.16972(14) 0.72519(11) 0.20290(12) 0.0254(4) Uani 1 1 d . . . C26 C 0.20868(18) 0.52469(13) 0.27103(15) 0.0194(4) Uani 1 1 d . . . N6 N 0.29452(18) 0.51515(14) 0.30125(15) 0.0283(5) Uani 1 1 d . . . C27 C 0.3187(3) 0.45208(17) 0.3300(2) 0.0377(8) Uani 1 1 d . . . H27 H 0.3795 0.4465 0.3505 0.045 Uiso 1 1 calc R . . C28 C 0.2571(3) 0.39735(19) 0.3297(2) 0.0407(8) Uani 1 1 d . . . H28 H 0.2752 0.3534 0.3486 0.049 Uiso 1 1 calc R . . C29 C 0.1687(3) 0.40633(17) 0.3019(2) 0.0366(7) Uani 1 1 d . . . H29 H 0.1242 0.3690 0.3032 0.044 Uiso 1 1 calc R . . C30 C 0.1439(2) 0.46904(16) 0.27192(18) 0.0306(6) Uani 1 1 d . . . H30 H 0.0829 0.4746 0.2518 0.037 Uiso 1 1 calc R . . O13 O 0.19088(14) 0.58482(10) 0.24197(10) 0.0234(4) Uani 1 1 d . . . O14 O 0.35451(15) 0.56914(11) 0.30116(13) 0.0289(5) Uani 1 1 d . . . C31 C 0.17243(18) 0.79191(14) 0.19105(14) 0.0201(5) Uani 1 1 d . . . N7 N 0.25875(18) 0.82172(14) 0.17598(12) 0.0238(5) Uani 1 1 d . . . C32 C 0.2662(2) 0.89112(17) 0.16039(19) 0.0311(6) Uani 1 1 d . . . H32 H 0.3260 0.9099 0.1476 0.037 Uiso 1 1 calc R . . C33 C 0.1879(3) 0.93437(17) 0.1629(2) 0.0386(8) Uani 1 1 d . . . H33 H 0.1935 0.9828 0.1526 0.046 Uiso 1 1 calc R . . C34 C 0.1016(3) 0.9059(2) 0.18063(18) 0.0379(8) Uani 1 1 d . . . H34 H 0.0475 0.9352 0.1837 0.046 Uiso 1 1 calc R . . C35 C 0.0928(2) 0.83588(19) 0.19391(17) 0.0332(7) Uani 1 1 d . . . H35 H 0.0325 0.8169 0.2051 0.040 Uiso 1 1 calc R . . O15 O 0.26372(16) 0.72142(13) 0.33370(12) 0.0297(5) Uani 1 1 d . . . O16 O 0.44176(14) 0.71022(11) 0.30178(11) 0.0249(4) Uani 1 1 d . . . C36 C 0.3269(2) 0.73064(14) 0.38357(13) 0.0210(5) Uani 1 1 d . . . N8 N 0.4211(2) 0.72433(14) 0.36615(14) 0.0292(5) Uani 1 1 d . . . C37 C 0.4888(3) 0.73262(18) 0.41732(19) 0.0366(8) Uani 1 1 d . . . H37 H 0.5541 0.7288 0.4060 0.044 Uiso 1 1 calc R . . C38 C 0.4620(4) 0.7464(2) 0.48453(19) 0.0522(13) Uani 1 1 d . . . H38 H 0.5089 0.7516 0.5195 0.063 Uiso 1 1 calc R . . C39 C 0.3668(5) 0.7528(2) 0.5014(2) 0.0545(14) Uani 1 1 d . . . H39 H 0.3484 0.7625 0.5478 0.065 Uiso 1 1 calc R . . C40 C 0.3001(3) 0.74511(19) 0.45118(18) 0.0424(9) Uani 1 1 d . . . H40 H 0.2348 0.7497 0.4625 0.051 Uiso 1 1 calc R . . O17 O 0.52006(17) 0.81918(14) 0.16780(17) 0.0428(6) Uani 1 1 d D . . H17A H 0.4669(17) 0.813(2) 0.176(2) 0.051 Uiso 1 1 d D . . H17B H 0.525(3) 0.843(2) 0.1360(17) 0.051 Uiso 1 1 d D . . O18 O -0.0258(2) 0.52236(17) 0.1607(2) 0.0572(9) Uani 1 1 d D . . H18A H -0.073(2) 0.536(3) 0.177(2) 0.069 Uiso 1 1 d D . . H18B H -0.039(4) 0.505(3) 0.1253(16) 0.069 Uiso 1 1 d D . . O19 O 0.11986(18) 0.62761(17) 0.07386(14) 0.0411(6) Uani 1 1 d D . . H19A H 0.105(3) 0.616(2) 0.0370(14) 0.049 Uiso 1 1 d D . . H19B H 0.1734(15) 0.623(2) 0.079(2) 0.049 Uiso 1 1 d D . . O20 O 0.08426(19) 0.78448(16) 0.36513(14) 0.0395(6) Uani 1 1 d D . . H20A H 0.037(2) 0.779(3) 0.348(2) 0.047 Uiso 1 1 d D . . H20B H 0.127(2) 0.772(3) 0.348(3) 0.047 Uiso 1 1 d D . . O21 O 0.6628(2) 0.5677(2) 0.4397(2) 0.0692(10) Uani 1 1 d D . . H21A H 0.604(2) 0.575(3) 0.418(3) 0.083 Uiso 1 1 d D . . H21B H 0.678(4) 0.6107(19) 0.418(3) 0.083 Uiso 1 1 d D . . O22 O 0.4587(3) 0.55988(18) 0.4218(2) 0.0646(9) Uani 1 1 d D . . H22A H 0.400(2) 0.559(3) 0.445(2) 0.078 Uiso 1 1 d D . . H22B H 0.420(3) 0.566(3) 0.3817(16) 0.078 Uiso 1 1 d D . . O23 O 0.9138(3) 0.41206(16) 0.0706(2) 0.0572(9) Uani 1 1 d D . . H23A H 0.878(3) 0.404(3) 0.0311(16) 0.069 Uiso 1 1 d D . . H23B H 0.878(3) 0.378(2) 0.092(2) 0.069 Uiso 1 1 d D . . O24 O 0.4885(2) 0.41901(17) 0.45490(17) 0.0496(7) Uani 1 1 d D . . H24A H 0.4253(19) 0.402(2) 0.449(3) 0.060 Uiso 1 1 d D . . H24B H 0.463(3) 0.4636(12) 0.449(3) 0.060 Uiso 1 1 d D . . O25 O 0.6704(4) 0.4360(2) 0.5189(3) 0.0973(15) Uani 1 1 d D . . H25A H 0.681(6) 0.4834(18) 0.502(3) 0.117 Uiso 1 1 d D . . H25B H 0.650(5) 0.462(3) 0.560(2) 0.117 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 Eu1 0.01264(5) 0.01705(5) 0.01849(5) -0.00048(5) -0.00032(5) 0.00014(4) Eu2 0.01212(5) 0.01806(5) 0.01803(5) 0.00201(5) -0.00037(5) -0.00025(5) Na1 0.0158(5) 0.0235(5) 0.0308(5) -0.0027(5) -0.0021(4) 0.0001(4) Na2 0.0170(5) 0.0331(6) 0.0304(6) 0.0049(5) 0.0004(5) 0.0008(5) O1 0.0186(9) 0.0213(10) 0.0358(11) -0.0091(8) -0.0026(8) 0.0010(7) O2 0.0187(9) 0.0233(9) 0.0295(10) -0.0067(8) -0.0007(7) 0.0007(7) N1 0.0232(11) 0.0196(10) 0.0278(10) -0.0037(9) 0.0001(9) -0.0009(9) C1 0.0210(12) 0.0195(12) 0.0217(11) -0.0014(9) 0.0008(9) 0.0013(9) C2 0.0298(16) 0.0238(14) 0.0373(15) -0.0015(11) 0.0060(12) 0.0052(11) C3 0.049(2) 0.0219(15) 0.0458(19) -0.0048(13) 0.0192(16) 0.0023(14) C4 0.049(2) 0.0266(15) 0.0475(19) -0.0134(14) 0.0108(17) -0.0082(16) C5 0.0340(17) 0.0241(15) 0.0419(17) -0.0086(13) 0.0007(13) -0.0104(12) O3 0.0163(9) 0.0265(10) 0.0212(9) 0.0052(8) -0.0016(7) 0.0005(7) O4 0.0170(9) 0.0337(11) 0.0222(9) 0.0023(8) 0.0010(7) 0.0044(8) C6 0.0130(10) 0.0131(10) 0.0164(10) 0.0014(8) 0.0008(8) 0.0001(8) N2 0.0295(13) 0.0247(12) 0.0261(12) -0.0015(10) 0.0000(10) 0.0027(10) C7 0.0237(14) 0.0251(14) 0.0271(14) 0.0012(11) -0.0063(10) 0.0022(11) C8 0.0399(18) 0.0261(15) 0.0218(13) 0.0007(11) -0.0053(11) 0.0028(12) C9 0.0423(19) 0.0279(16) 0.0261(15) 0.0021(12) 0.0084(13) 0.0033(14) C10 0.0269(14) 0.0232(13) 0.0294(14) 0.0019(11) 0.0079(11) 0.0044(11) O5 0.0224(10) 0.0257(10) 0.0464(13) -0.0111(9) 0.0071(9) -0.0037(8) O6 0.0173(8) 0.0202(9) 0.0332(10) -0.0021(8) -0.0010(8) -0.0025(6) N3 0.0199(11) 0.0227(11) 0.0307(12) -0.0019(9) -0.0015(9) -0.0023(9) C11 0.0224(13) 0.0212(13) 0.0297(14) -0.0040(11) 0.0001(10) -0.0021(10) C12 0.043(2) 0.0234(15) 0.0452(19) -0.0134(13) -0.0005(15) -0.0014(13) C13 0.058(3) 0.0310(18) 0.056(2) -0.0119(17) -0.007(2) -0.0123(17) C14 0.041(2) 0.041(2) 0.056(2) -0.0070(17) -0.0061(17) -0.0225(16) C15 0.0222(14) 0.0339(17) 0.0420(17) 0.0037(12) -0.0026(12) -0.0072(12) O7 0.0194(10) 0.0264(10) 0.0267(9) 0.0056(8) 0.0003(8) -0.0002(8) O8 0.0173(9) 0.0318(11) 0.0224(9) 0.0032(8) 0.0006(7) 0.0055(7) C16 0.0177(12) 0.0147(11) 0.0215(11) 0.0007(9) -0.0006(9) -0.0021(9) N4 0.0240(12) 0.0236(12) 0.0286(12) 0.0015(10) -0.0022(9) 0.0000(9) C17 0.0202(13) 0.0298(15) 0.0330(15) -0.0009(12) -0.0011(11) 0.0039(11) C18 0.0342(17) 0.0333(17) 0.0382(17) 0.0012(14) -0.0137(14) 0.0064(14) C19 0.046(2) 0.0332(18) 0.0272(15) 0.0077(13) -0.0079(14) 0.0042(15) C20 0.0332(16) 0.0310(16) 0.0257(14) 0.0045(12) 0.0015(12) -0.0002(12) O9 0.0178(9) 0.0247(10) 0.0227(9) -0.0039(7) -0.0012(7) -0.0005(7) O10 0.0167(9) 0.0285(10) 0.0249(9) -0.0020(8) 0.0001(8) -0.0013(8) C21 0.0189(12) 0.0169(11) 0.0208(11) -0.0009(9) -0.0014(9) 0.0004(9) N5 0.0265(12) 0.0232(12) 0.0280(12) -0.0015(10) 0.0028(9) 0.0002(9) C22 0.0243(14) 0.0299(15) 0.0363(15) -0.0035(12) 0.0083(12) -0.0021(12) C23 0.0372(18) 0.042(2) 0.0393(18) -0.0084(15) 0.0171(15) -0.0032(16) C24 0.054(2) 0.039(2) 0.0269(15) -0.0113(14) 0.0101(15) -0.0047(16) C25 0.0361(17) 0.0291(15) 0.0244(14) -0.0065(12) -0.0019(12) -0.0042(13) O11 0.0159(9) 0.0217(9) 0.0316(10) 0.0057(8) 0.0017(7) 0.0034(7) O12 0.0158(9) 0.0252(10) 0.0352(11) 0.0055(8) -0.0018(8) 0.0014(7) C26 0.0173(11) 0.0176(11) 0.0232(11) -0.0024(10) 0.0037(9) -0.0009(8) N6 0.0233(12) 0.0247(12) 0.0370(13) 0.0067(11) 0.0023(10) -0.0001(9) C27 0.0317(16) 0.0255(14) 0.056(2) 0.0131(14) -0.0083(16) 0.0033(14) C28 0.045(2) 0.0229(15) 0.055(2) 0.0098(15) -0.0010(17) -0.0033(14) C29 0.0385(18) 0.0224(14) 0.0488(19) 0.0037(13) 0.0054(15) -0.0103(12) C30 0.0276(14) 0.0260(14) 0.0382(16) -0.0023(13) 0.0039(13) -0.0053(11) O13 0.0157(8) 0.0241(9) 0.0305(9) 0.0071(7) -0.0009(8) -0.0015(7) O14 0.0231(10) 0.0239(10) 0.0397(12) 0.0103(9) -0.0078(9) -0.0055(8) C31 0.0170(11) 0.0229(12) 0.0205(11) -0.0007(9) -0.0019(9) 0.0047(9) N7 0.0249(11) 0.0231(12) 0.0234(10) 0.0010(9) -0.0022(8) 0.0035(9) C32 0.0330(16) 0.0207(14) 0.0396(17) 0.0033(12) -0.0055(13) -0.0002(12) C33 0.052(2) 0.0202(13) 0.0441(18) -0.0003(12) -0.0180(18) 0.0106(15) C34 0.0392(19) 0.0398(19) 0.0348(17) -0.0050(14) -0.0078(14) 0.0218(15) C35 0.0218(13) 0.0450(19) 0.0329(14) 0.0013(15) 0.0001(11) 0.0122(13) O15 0.0253(11) 0.0388(13) 0.0251(10) -0.0079(9) 0.0051(8) -0.0014(9) O16 0.0187(9) 0.0317(11) 0.0243(9) -0.0038(8) -0.0010(8) 0.0000(8) C36 0.0238(14) 0.0208(12) 0.0185(11) -0.0023(9) 0.0025(10) -0.0042(10) N8 0.0356(14) 0.0224(12) 0.0296(13) 0.0005(10) -0.0066(11) -0.0013(10) C37 0.046(2) 0.0257(15) 0.0382(17) 0.0051(13) -0.0205(15) -0.0066(14) C38 0.091(4) 0.034(2) 0.0313(18) 0.0028(15) -0.028(2) -0.016(2) C39 0.103(4) 0.037(2) 0.0233(15) -0.0061(14) 0.008(2) -0.024(2) C40 0.064(3) 0.0347(18) 0.0287(16) -0.0071(13) 0.0178(16) -0.0123(18) O17 0.0212(11) 0.0355(14) 0.0717(19) 0.0160(13) -0.0031(11) -0.0042(10) O18 0.0270(13) 0.0475(17) 0.097(3) -0.0343(17) 0.0139(15) -0.0063(12) O19 0.0239(11) 0.0654(19) 0.0339(12) -0.0097(12) -0.0036(10) 0.0043(12) O20 0.0284(12) 0.0486(16) 0.0415(14) -0.0112(12) 0.0034(10) 0.0014(12) O21 0.053(2) 0.091(3) 0.063(2) -0.0033(19) 0.0224(17) -0.0242(19) O22 0.087(3) 0.0463(18) 0.060(2) 0.0032(16) -0.0209(19) 0.0071(19) O23 0.069(2) 0.0309(15) 0.071(2) -0.0068(14) -0.0285(18) 0.0017(14) O24 0.0516(18) 0.0468(17) 0.0504(16) 0.0054(14) -0.0013(14) 0.0038(14) O25 0.099(4) 0.067(3) 0.126(4) -0.019(3) 0.013(3) -0.007(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 Eu1 O3 2.369(2) . ? Eu1 O7 2.390(2) . ? Eu1 O6 2.3908(19) . ? Eu1 O8 2.3909(19) . ? Eu1 O1 2.395(2) . ? Eu1 O5 2.401(2) . ? Eu1 O4 2.404(2) . ? Eu1 O2 2.406(2) . ? Eu1 C6 3.221(2) . ? Eu1 C16 3.225(3) . ? Eu1 C1 3.244(3) . ? Eu1 C11 3.251(3) . ? Eu2 O15 2.370(2) . ? Eu2 O11 2.381(2) . ? Eu2 O13 2.3885(19) . ? Eu2 O12 2.3889(19) . ? Eu2 O9 2.3900(19) . ? Eu2 O16 2.396(2) . ? Eu2 O14 2.405(2) . ? Eu2 O10 2.413(2) . ? Eu2 C31 3.201(3) . ? Eu2 C36 3.206(3) . ? Eu2 C26 3.232(3) . ? Eu2 C21 3.256(3) . ? Na1 O17 2.369(3) . ? Na1 O9 2.373(2) . ? Na1 O16 2.381(2) . ? Na1 O2 2.403(2) . ? Na1 O6 2.450(2) . ? Na1 O4 2.462(2) . ? Na2 O13 2.360(2) . ? Na2 O19 2.371(3) . ? Na2 O3 2.409(2) 1_455 ? Na2 O8 2.422(2) 1_455 ? Na2 O12 2.429(2) . ? Na2 O18 2.434(3) . ? Na2 Eu1 3.8333(12) 1_455 ? O1 N1 1.341(3) . ? O2 C1 1.284(3) . ? N1 C5 1.360(4) . ? N1 C1 1.375(4) . ? C1 C2 1.406(4) . ? C2 C3 1.376(5) . ? C3 C4 1.400(6) . ? C4 C5 1.363(5) . ? O3 C6 1.345(3) . ? O3 Na2 2.409(2) 1_655 ? O4 N2 1.290(3) . ? C6 N2 1.363(4) . ? C6 C10 1.371(4) . ? N2 C7 1.404(4) . ? C7 C8 1.372(5) . ? C8 C9 1.402(5) . ? C9 C10 1.356(5) . ? O5 C11 1.290(4) . ? O6 N3 1.336(3) . ? N3 C15 1.368(4) . ? N3 C11 1.377(4) . ? C11 C12 1.394(4) . ? C12 C13 1.372(6) . ? C13 C14 1.383(6) . ? C14 C15 1.367(5) . ? O7 C16 1.317(3) . ? O8 N4 1.318(3) . ? O8 Na2 2.422(2) 1_655 ? C16 N4 1.373(4) . ? C16 C20 1.375(4) . ? N4 C17 1.383(4) . ? C17 C18 1.371(5) . ? C18 C19 1.392(5) . ? C19 C20 1.368(5) . ? O9 N5 1.312(3) . ? O10 C21 1.305(3) . ? C21 N5 1.370(4) . ? C21 C25 1.381(4) . ? N5 C22 1.385(4) . ? C22 C23 1.364(5) . ? C23 C24 1.399(6) . ? C24 C25 1.370(5) . ? O11 N7 1.326(3) . ? O12 C31 1.296(3) . ? C26 O13 1.303(3) . ? C26 N6 1.356(4) . ? C26 C30 1.402(4) . ? N6 O14 1.334(3) . ? N6 C27 1.371(4) . ? C27 C28 1.360(5) . ? C28 C29 1.369(5) . ? C29 C30 1.376(5) . ? C31 N7 1.376(4) . ? C31 C35 1.404(4) . ? N7 C32 1.364(4) . ? C32 C33 1.380(5) . ? C33 C34 1.377(6) . ? C34 C35 1.368(5) . ? O15 C36 1.323(4) . ? O16 N8 1.304(3) . ? C36 N8 1.376(4) . ? C36 C40 1.386(4) . ? N8 C37 1.383(4) . ? C37 C38 1.376(6) . ? C38 C39 1.387(8) . ? C39 C40 1.359(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 O3 Eu1 O7 137.41(7) . . ? O3 Eu1 O6 132.36(7) . . ? O7 Eu1 O6 78.00(7) . . ? O3 Eu1 O8 71.96(7) . . ? O7 Eu1 O8 65.86(7) . . ? O6 Eu1 O8 133.71(7) . . ? O3 Eu1 O1 87.42(7) . . ? O7 Eu1 O1 87.01(8) . . ? O6 Eu1 O1 133.04(7) . . ? O8 Eu1 O1 74.55(7) . . ? O3 Eu1 O5 80.14(8) . . ? O7 Eu1 O5 91.65(8) . . ? O6 Eu1 O5 65.66(7) . . ? O8 Eu1 O5 86.76(8) . . ? O1 Eu1 O5 160.07(7) . . ? O3 Eu1 O4 66.04(7) . . ? O7 Eu1 O4 154.66(7) . . ? O6 Eu1 O4 77.18(7) . . ? O8 Eu1 O4 137.83(7) . . ? O1 Eu1 O4 106.46(8) . . ? O5 Eu1 O4 82.71(8) . . ? O3 Eu1 O2 122.13(7) . . ? O7 Eu1 O2 93.24(7) . . ? O6 Eu1 O2 71.27(7) . . ? O8 Eu1 O2 135.75(7) . . ? O1 Eu1 O2 65.41(7) . . ? O5 Eu1 O2 134.50(7) . . ? O4 Eu1 O2 74.04(7) . . ? O3 Eu1 C6 21.73(6) . . ? O7 Eu1 C6 156.11(7) . . ? O6 Eu1 C6 113.15(7) . . ? O8 Eu1 C6 93.01(7) . . ? O1 Eu1 C6 98.35(7) . . ? O5 Eu1 C6 75.41(7) . . ? O4 Eu1 C6 44.82(6) . . ? O2 Eu1 C6 110.21(7) . . ? O3 Eu1 C16 117.55(7) . . ? O7 Eu1 C16 21.16(7) . . ? O6 Eu1 C16 98.48(7) . . ? O8 Eu1 C16 45.60(7) . . ? O1 Eu1 C16 76.61(7) . . ? O5 Eu1 C16 95.35(8) . . ? O4 Eu1 C16 175.65(7) . . ? O2 Eu1 C16 104.93(7) . . ? C6 Eu1 C16 138.45(7) . . ? O3 Eu1 C1 111.26(7) . . ? O7 Eu1 C1 94.11(7) . . ? O6 Eu1 C1 91.01(7) . . ? O8 Eu1 C1 118.48(7) . . ? O1 Eu1 C1 45.58(7) . . ? O5 Eu1 C1 154.21(7) . . ? O4 Eu1 C1 81.38(7) . . ? O2 Eu1 C1 20.07(7) . . ? C6 Eu1 C1 106.31(7) . . ? C16 Eu1 C1 99.05(7) . . ? O3 Eu1 C11 97.38(7) . . ? O7 Eu1 C11 85.82(8) . . ? O6 Eu1 C11 45.67(7) . . ? O8 Eu1 C11 101.76(7) . . ? O1 Eu1 C11 172.79(8) . . ? O5 Eu1 C11 20.02(7) . . ? O4 Eu1 C11 80.48(8) . . ? O2 Eu1 C11 115.73(7) . . ? C6 Eu1 C11 87.95(7) . . ? C16 Eu1 C11 96.36(7) . . ? C1 Eu1 C11 135.80(7) . . ? O15 Eu2 O11 90.62(8) . . ? O15 Eu2 O13 88.39(8) . . ? O11 Eu2 O13 135.98(7) . . ? O15 Eu2 O12 73.63(8) . . ? O11 Eu2 O12 65.76(7) . . ? O13 Eu2 O12 71.83(7) . . ? O15 Eu2 O9 135.47(7) . . ? O11 Eu2 O9 80.90(7) . . ? O13 Eu2 O9 127.15(7) . . ? O12 Eu2 O9 137.02(7) . . ? O15 Eu2 O16 65.98(7) . . ? O11 Eu2 O16 82.53(7) . . ? O13 Eu2 O16 135.45(7) . . ? O12 Eu2 O16 127.71(7) . . ? O9 Eu2 O16 69.59(7) . . ? O15 Eu2 O14 85.48(9) . . ? O11 Eu2 O14 158.16(7) . . ? O13 Eu2 O14 65.48(7) . . ? O12 Eu2 O14 132.69(7) . . ? O9 Eu2 O14 86.86(7) . . ? O16 Eu2 O14 76.24(7) . . ? O15 Eu2 O10 159.06(8) . . ? O11 Eu2 O10 89.48(7) . . ? O13 Eu2 O10 77.13(7) . . ? O12 Eu2 O10 87.38(8) . . ? O9 Eu2 O10 65.11(7) . . ? O16 Eu2 O10 134.69(7) . . ? O14 Eu2 O10 101.73(8) . . ? O15 Eu2 C31 71.50(8) . . ? O11 Eu2 C31 45.91(7) . . ? O13 Eu2 C31 92.80(7) . . ? O12 Eu2 C31 21.05(7) . . ? O9 Eu2 C31 124.03(7) . . ? O16 Eu2 C31 110.83(7) . . ? O14 Eu2 C31 149.07(7) . . ? O10 Eu2 C31 93.91(7) . . ? O15 Eu2 C36 21.44(8) . . ? O11 Eu2 C36 93.33(7) . . ? O13 Eu2 C36 101.01(7) . . ? O12 Eu2 C36 94.08(8) . . ? O9 Eu2 C36 115.00(7) . . ? O16 Eu2 C36 45.58(7) . . ? O14 Eu2 C36 75.51(8) . . ? O10 Eu2 C36 177.17(7) . . ? C31 Eu2 C36 88.30(7) . . ? O15 Eu2 C26 90.51(8) . . ? O11 Eu2 C26 156.45(7) . . ? O13 Eu2 C26 20.59(7) . . ? O12 Eu2 C26 92.08(7) . . ? O9 Eu2 C26 113.89(7) . . ? O16 Eu2 C26 119.18(7) . . ? O14 Eu2 C26 45.28(7) . . ? O10 Eu2 C26 81.26(7) . . ? C31 Eu2 C26 112.85(7) . . ? C36 Eu2 C26 96.26(7) . . ? O15 Eu2 C21 173.89(8) . . ? O11 Eu2 C21 83.42(7) . . ? O13 Eu2 C21 94.97(7) . . ? O12 Eu2 C21 102.55(7) . . ? O9 Eu2 C21 44.87(7) . . ? O16 Eu2 C21 114.31(7) . . ? O14 Eu2 C21 100.55(8) . . ? O10 Eu2 C21 20.48(7) . . ? C31 Eu2 C21 103.18(7) . . ? C36 Eu2 C21 159.86(7) . . ? C26 Eu2 C21 94.42(7) . . ? O17 Na1 O9 88.69(9) . . ? O17 Na1 O16 94.85(9) . . ? O9 Na1 O16 70.11(8) . . ? O17 Na1 O2 111.99(10) . . ? O9 Na1 O2 159.05(9) . . ? O16 Na1 O2 103.48(8) . . ? O17 Na1 O6 167.67(11) . . ? O9 Na1 O6 90.21(8) . . ? O16 Na1 O6 96.32(8) . . ? O2 Na1 O6 70.32(7) . . ? O17 Na1 O4 93.87(9) . . ? O9 Na1 O4 110.19(8) . . ? O16 Na1 O4 171.28(9) . . ? O2 Na1 O4 73.06(8) . . ? O6 Na1 O4 75.00(8) . . ? O17 Na1 Eu1 130.08(7) . . ? O9 Na1 Eu1 124.80(6) . . ? O16 Na1 Eu1 128.87(7) . . ? O2 Na1 Eu1 43.38(5) . . ? O6 Na1 Eu1 43.08(5) . . ? O4 Na1 Eu1 43.39(5) . . ? O17 Na1 Eu2 82.37(6) . . ? O9 Na1 Eu2 36.13(5) . . ? O16 Na1 Eu2 36.34(5) . . ? O2 Na1 Eu2 139.69(7) . . ? O6 Na1 Eu2 103.75(6) . . ? O4 Na1 Eu2 145.83(7) . . ? Eu1 Na1 Eu2 146.83(3) . . ? O13 Na2 O19 95.14(9) . . ? O13 Na2 O3 159.16(9) . 1_455 ? O19 Na2 O3 102.90(9) . 1_455 ? O13 Na2 O8 91.76(8) . 1_455 ? O19 Na2 O8 172.76(9) . 1_455 ? O3 Na2 O8 70.74(7) 1_455 1_455 ? O13 Na2 O12 71.62(7) . . ? O19 Na2 O12 83.28(10) . . ? O3 Na2 O12 99.97(8) 1_455 . ? O8 Na2 O12 101.01(9) 1_455 . ? O13 Na2 O18 98.67(11) . . ? O19 Na2 O18 87.67(12) . . ? O3 Na2 O18 92.47(10) 1_455 . ? O8 Na2 O18 89.15(11) 1_455 . ? O12 Na2 O18 165.97(10) . . ? O13 Na2 Eu2 36.48(5) . . ? O19 Na2 Eu2 80.43(7) . . ? O3 Na2 Eu2 136.76(7) 1_455 . ? O8 Na2 Eu2 106.52(6) 1_455 . ? O12 Na2 Eu2 36.98(5) . . ? O18 Na2 Eu2 130.73(8) . . ? O13 Na2 Eu1 128.49(6) . 1_455 ? O19 Na2 Eu1 135.97(8) . 1_455 ? O3 Na2 Eu1 36.30(5) 1_455 1_455 ? O8 Na2 Eu1 36.93(5) 1_455 1_455 ? O12 Na2 Eu1 113.04(6) . 1_455 ? O18 Na2 Eu1 80.88(7) . 1_455 ? Eu2 Na2 Eu1 137.21(4) . 1_455 ? N1 O1 Eu1 118.57(15) . . ? C1 O2 Na1 135.11(18) . . ? C1 O2 Eu1 119.92(17) . . ? Na1 O2 Eu1 93.31(7) . . ? O1 N1 C5 120.0(2) . . ? O1 N1 C1 117.4(2) . . ? C5 N1 C1 122.6(3) . . ? O2 C1 N1 118.0(2) . . ? O2 C1 C2 125.1(3) . . ? N1 C1 C2 116.9(3) . . ? O2 C1 Eu1 40.01(13) . . ? N1 C1 Eu1 78.31(15) . . ? C2 C1 Eu1 163.5(2) . . ? C3 C2 C1 120.6(3) . . ? C2 C3 C4 120.5(3) . . ? C5 C4 C3 118.4(3) . . ? N1 C5 C4 120.9(3) . . ? C6 O3 Eu1 117.59(15) . . ? C6 O3 Na2 125.73(16) . 1_655 ? Eu1 O3 Na2 106.70(8) . 1_655 ? N2 O4 Eu1 118.61(17) . . ? N2 O4 Na1 148.98(18) . . ? Eu1 O4 Na1 91.90(8) . . ? O3 C6 N2 118.0(2) . . ? O3 C6 C10 120.2(2) . . ? N2 C6 C10 121.8(3) . . ? O3 C6 Eu1 40.68(11) . . ? N2 C6 Eu1 78.03(16) . . ? C10 C6 Eu1 159.1(2) . . ? O4 N2 C6 118.0(3) . . ? O4 N2 C7 123.9(3) . . ? C6 N2 C7 118.1(3) . . ? C8 C7 N2 120.7(3) . . ? C7 C8 C9 119.1(3) . . ? C10 C9 C8 119.9(3) . . ? C9 C10 C6 120.2(3) . . ? C11 O5 Eu1 120.39(19) . . ? N3 O6 Eu1 118.40(16) . . ? N3 O6 Na1 120.21(16) . . ? Eu1 O6 Na1 92.50(7) . . ? O6 N3 C15 120.2(3) . . ? O6 N3 C11 118.3(2) . . ? C15 N3 C11 121.5(3) . . ? O5 C11 N3 117.1(3) . . ? O5 C11 C12 125.3(3) . . ? N3 C11 C12 117.6(3) . . ? O5 C11 Eu1 39.58(14) . . ? N3 C11 Eu1 77.58(16) . . ? C12 C11 Eu1 164.7(2) . . ? C13 C12 C11 121.1(4) . . ? C12 C13 C14 119.9(3) . . ? C15 C14 C13 119.4(3) . . ? C14 C15 N3 120.5(3) . . ? C16 O7 Eu1 117.94(17) . . ? N4 O8 Eu1 117.47(16) . . ? N4 O8 Na2 136.23(17) . 1_655 ? Eu1 O8 Na2 105.57(8) . 1_655 ? O7 C16 N4 117.4(2) . . ? O7 C16 C20 122.8(3) . . ? N4 C16 C20 119.9(3) . . ? O7 C16 Eu1 40.90(12) . . ? N4 C16 Eu1 77.46(15) . . ? C20 C16 Eu1 160.7(2) . . ? O8 N4 C16 118.0(2) . . ? O8 N4 C17 122.2(3) . . ? C16 N4 C17 119.7(3) . . ? C18 C17 N4 120.3(3) . . ? C17 C18 C19 120.0(3) . . ? C20 C19 C18 119.1(3) . . ? C19 C20 C16 121.0(3) . . ? N5 O9 Na1 126.95(17) . . ? N5 O9 Eu2 119.63(16) . . ? Na1 O9 Eu2 108.04(8) . . ? C21 O10 Eu2 119.21(17) . . ? O10 C21 N5 117.3(2) . . ? O10 C21 C25 123.1(3) . . ? N5 C21 C25 119.6(3) . . ? O10 C21 Eu2 40.31(12) . . ? N5 C21 Eu2 77.40(15) . . ? C25 C21 Eu2 161.8(2) . . ? O9 N5 C21 118.0(2) . . ? O9 N5 C22 122.1(3) . . ? C21 N5 C22 119.9(3) . . ? C23 C22 N5 120.8(3) . . ? C22 C23 C24 119.4(3) . . ? C25 C24 C23 119.5(3) . . ? C24 C25 C21 120.8(3) . . ? N7 O11 Eu2 117.43(16) . . ? C31 O12 Eu2 117.49(16) . . ? C31 O12 Na2 136.27(17) . . ? Eu2 O12 Na2 105.31(8) . . ? O13 C26 N6 118.4(2) . . ? O13 C26 C30 123.3(3) . . ? N6 C26 C30 118.3(3) . . ? O13 C26 Eu2 40.14(12) . . ? N6 C26 Eu2 78.61(15) . . ? C30 C26 Eu2 162.1(2) . . ? O14 N6 C26 117.5(2) . . ? O14 N6 C27 121.5(3) . . ? C26 N6 C27 121.0(3) . . ? C28 C27 N6 121.0(3) . . ? C27 C28 C29 119.2(3) . . ? C28 C29 C30 120.4(3) . . ? C29 C30 C26 120.0(3) . . ? C26 O13 Na2 133.02(17) . . ? C26 O13 Eu2 119.26(16) . . ? Na2 O13 Eu2 107.54(8) . . ? N6 O14 Eu2 117.74(17) . . ? O12 C31 N7 118.1(2) . . ? O12 C31 C35 123.9(3) . . ? N7 C31 C35 118.0(3) . . ? O12 C31 Eu2 41.46(12) . . ? N7 C31 Eu2 78.18(15) . . ? C35 C31 Eu2 159.9(2) . . ? O11 N7 C32 121.8(3) . . ? O11 N7 C31 117.1(2) . . ? C32 N7 C31 121.1(3) . . ? N7 C32 C33 120.9(3) . . ? C34 C33 C32 118.6(3) . . ? C35 C34 C33 120.9(3) . . ? C34 C35 C31 120.3(3) . . ? C36 O15 Eu2 117.67(18) . . ? N8 O16 Na1 135.08(19) . . ? N8 O16 Eu2 117.24(18) . . ? Na1 O16 Eu2 107.57(8) . . ? O15 C36 N8 117.5(2) . . ? O15 C36 C40 121.8(3) . . ? N8 C36 C40 120.7(3) . . ? O15 C36 Eu2 40.89(13) . . ? N8 C36 Eu2 77.74(16) . . ? C40 C36 Eu2 159.0(2) . . ? O16 N8 C36 117.8(2) . . ? O16 N8 C37 123.3(3) . . ? C36 N8 C37 118.9(3) . . ? C38 C37 N8 120.3(4) . . ? C37 C38 C39 120.2(4) . . ? C40 C39 C38 119.6(4) . . ? C39 C40 C36 120.2(4) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 33.14 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.928 _refine_diff_density_min -1.181 _refine_diff_density_rms 0.122 #======END data_2 _database_code_CSD 200687 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H25 Gd N4 Na O12.50' _chemical_formula_weight 701.68 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' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 14.1145(6) _cell_length_b 19.1011(7) _cell_length_c 19.2734(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5196.2(3) _cell_formula_units_Z 8 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 5472 _cell_measurement_theta_min 2.559 _cell_measurement_theta_max 31.002 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.4 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.794 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2784 _exptl_absorpt_coefficient_mu 2.640 _exptl_absorpt_correction_type semi-empirical _exptl_absorpt_correction_T_min 0.748330 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS (Bruker-AXS)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 '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_% ? _diffrn_reflns_number 38047 _diffrn_reflns_av_R_equivalents 0.0397 _diffrn_reflns_av_sigmaI/netI 0.0565 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 28.28 _reflns_number_total 12904 _reflns_number_gt 9857 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0219P)^2^+0.5168P] 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 mixed _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 -0.031(8) _refine_ls_number_reflns 12904 _refine_ls_number_parameters 748 _refine_ls_number_restraints 191 _refine_ls_R_factor_all 0.0512 _refine_ls_R_factor_gt 0.0316 _refine_ls_wR_factor_ref 0.0626 _refine_ls_wR_factor_gt 0.0553 _refine_ls_goodness_of_fit_ref 0.962 _refine_ls_restrained_S_all 0.971 _refine_ls_shift/su_max 0.015 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd1 Gd 0.811964(18) 0.672479(12) 0.266646(13) 0.01750(6) Uani 1 1 d . . . Gd2 Gd 0.315298(18) 0.667701(12) 0.229809(13) 0.01728(6) Uani 1 1 d . . . Na1 Na 0.57859(12) 0.72182(10) 0.23154(11) 0.0248(4) Uani 1 1 d . . . Na2 Na 0.05505(13) 0.63109(10) 0.18771(11) 0.0291(5) Uani 1 1 d . . . O1 O 0.8820(2) 0.76954(18) 0.32532(18) 0.0265(8) Uani 1 1 d . . . O2 O 0.6996(2) 0.75506(17) 0.31243(17) 0.0232(8) Uani 1 1 d . . . N1 N 0.8253(3) 0.8217(2) 0.3461(2) 0.0241(9) Uani 1 1 d . . . C1 C 0.7286(4) 0.8123(3) 0.3376(3) 0.0213(11) Uani 1 1 d . . . C2 C 0.6711(4) 0.8686(3) 0.3572(3) 0.0327(13) Uani 1 1 d . . . H2 H 0.6043 0.8645 0.3532 0.039 Uiso 1 1 calc R . . C3 C 0.7093(5) 0.9294(3) 0.3820(3) 0.0394(16) Uani 1 1 d . . . H3 H 0.6692 0.9681 0.3919 0.047 Uiso 1 1 calc R . . C4 C 0.8067(5) 0.9350(3) 0.3931(3) 0.0402(14) Uani 1 1 d . . . H4 H 0.8330 0.9761 0.4132 0.048 Uiso 1 1 calc R . . C5 C 0.8637(4) 0.8802(3) 0.3742(3) 0.0340(14) Uani 1 1 d . . . H5 H 0.9303 0.8832 0.3809 0.041 Uiso 1 1 calc R . . O3 O 0.9117(2) 0.69858(18) 0.17252(19) 0.0232(8) Uani 1 1 d . . . O4 O 0.7292(2) 0.7185(2) 0.16903(19) 0.0241(9) Uani 1 1 d . . . C6 C 0.8708(3) 0.7133(2) 0.1116(2) 0.0099(9) Uani 1 1 d . . . N2 N 0.7759(3) 0.7250(2) 0.1110(3) 0.0328(12) Uani 1 1 d . . . C7 C 0.7322(4) 0.7426(3) 0.0473(3) 0.0266(12) Uani 1 1 d . . . H7 H 0.6661 0.7520 0.0458 0.032 Uiso 1 1 calc R . . C8 C 0.7849(4) 0.7460(3) -0.0123(3) 0.0297(13) Uani 1 1 d . . . H8 H 0.7552 0.7572 -0.0551 0.036 Uiso 1 1 calc R . . C9 C 0.8829(4) 0.7328(3) -0.0102(3) 0.0295(14) Uani 1 1 d . . . H9 H 0.9196 0.7341 -0.0515 0.035 Uiso 1 1 calc R . . C10 C 0.9244(4) 0.7182(3) 0.0523(3) 0.0291(12) Uani 1 1 d . . . H10 H 0.9910 0.7114 0.0547 0.035 Uiso 1 1 calc R . . O5 O 0.8007(3) 0.56470(17) 0.20348(19) 0.0315(9) Uani 1 1 d . . . O6 O 0.6609(2) 0.61760(16) 0.27454(18) 0.0240(8) Uani 1 1 d . . . N3 N 0.6491(3) 0.5558(2) 0.2425(2) 0.0262(10) Uani 1 1 d . . . C11 C 0.7234(4) 0.5284(3) 0.2056(3) 0.0234(13) Uani 1 1 d . . . C12 C 0.7103(4) 0.4634(3) 0.1719(3) 0.0376(15) Uani 1 1 d . . . H12 H 0.7600 0.4447 0.1443 0.045 Uiso 1 1 calc R . . C13 C 0.6269(5) 0.4269(3) 0.1784(4) 0.0472(18) Uani 1 1 d . . . H13 H 0.6196 0.3823 0.1574 0.057 Uiso 1 1 calc R . . C14 C 0.5525(5) 0.4569(3) 0.2168(3) 0.0448(16) Uani 1 1 d . . . H14 H 0.4938 0.4329 0.2214 0.054 Uiso 1 1 calc R . . C15 C 0.5654(4) 0.5209(3) 0.2474(3) 0.0334(13) Uani 1 1 d . . . H15 H 0.5147 0.5413 0.2728 0.040 Uiso 1 1 calc R . . O7 O 0.8219(3) 0.61124(19) 0.37411(18) 0.0251(8) Uani 1 1 d . . . O8 O 0.9685(2) 0.63624(18) 0.29584(18) 0.0247(9) Uani 1 1 d . . . C16 C 0.9065(3) 0.6033(2) 0.4027(3) 0.0146(11) Uani 1 1 d . . . N4 N 0.9834(3) 0.6176(2) 0.3603(2) 0.0281(11) Uani 1 1 d . . . C17 C 1.0747(4) 0.6130(3) 0.3887(3) 0.0302(13) Uani 1 1 d . . . H17 H 1.1283 0.6234 0.3607 0.036 Uiso 1 1 calc R . . C18 C 1.0867(4) 0.5939(3) 0.4555(3) 0.0371(15) Uani 1 1 d . . . H18 H 1.1489 0.5912 0.4743 0.045 Uiso 1 1 calc R . . C19 C 1.0097(5) 0.5783(3) 0.4968(3) 0.0348(15) Uani 1 1 d . . . H19 H 1.0184 0.5648 0.5438 0.042 Uiso 1 1 calc R . . C20 C 0.9204(4) 0.5825(3) 0.4691(3) 0.0318(14) Uani 1 1 d . . . H20 H 0.8673 0.5707 0.4971 0.038 Uiso 1 1 calc R . . O9 O 0.4645(2) 0.64999(17) 0.17548(17) 0.0212(8) Uani 1 1 d . . . O10 O 0.3067(3) 0.61479(19) 0.11703(18) 0.0253(8) Uani 1 1 d . . . C21 C 0.3837(3) 0.6104(3) 0.0794(3) 0.0155(11) Uani 1 1 d . . . N5 N 0.4666(3) 0.6279(2) 0.1104(2) 0.0315(12) Uani 1 1 d . . . C22 C 0.5514(4) 0.6226(3) 0.0741(3) 0.0281(12) Uani 1 1 d . . . H22 H 0.6092 0.6323 0.0974 0.034 Uiso 1 1 calc R . . C23 C 0.5535(4) 0.6038(3) 0.0067(3) 0.0380(15) Uani 1 1 d . . . H23 H 0.6115 0.6017 -0.0182 0.046 Uiso 1 1 calc R . . C24 C 0.4663(5) 0.5875(3) -0.0258(3) 0.0422(16) Uani 1 1 d . . . H24 H 0.4653 0.5748 -0.0734 0.051 Uiso 1 1 calc R . . C25 C 0.3835(4) 0.5900(3) 0.0110(3) 0.0304(14) Uani 1 1 d . . . H25 H 0.3255 0.5775 -0.0109 0.036 Uiso 1 1 calc R . . O11 O 0.3335(2) 0.77911(18) 0.17759(18) 0.0240(8) Uani 1 1 d . . . O12 O 0.1699(2) 0.72428(17) 0.20318(18) 0.0267(8) Uani 1 1 d . . . C26 C 0.2083(3) 0.5245(2) 0.2719(3) 0.0177(10) Uani 1 1 d . . . N6 N 0.2954(3) 0.5152(2) 0.3016(2) 0.0338(11) Uani 1 1 d . . . C27 C 0.3188(5) 0.4522(3) 0.3297(3) 0.0374(14) Uani 1 1 d . . . H27 H 0.3794 0.4465 0.3503 0.045 Uiso 1 1 calc R . . C28 C 0.2582(4) 0.3977(3) 0.3291(3) 0.0406(15) Uani 1 1 d . . . H28 H 0.2766 0.3537 0.3475 0.049 Uiso 1 1 calc R . . C29 C 0.1680(4) 0.4070(3) 0.3010(3) 0.0345(14) Uani 1 1 d . . . H29 H 0.1235 0.3697 0.3018 0.041 Uiso 1 1 calc R . . C30 C 0.1443(4) 0.4691(3) 0.2728(3) 0.0310(12) Uani 1 1 d . . . H30 H 0.0831 0.4752 0.2533 0.037 Uiso 1 1 calc R . . O13 O 0.1909(2) 0.58498(16) 0.24268(17) 0.0248(8) Uani 1 1 d . . . O14 O 0.3549(2) 0.56949(17) 0.30098(19) 0.0290(9) Uani 1 1 d . . . C31 C 0.1729(3) 0.7914(2) 0.1918(2) 0.0192(10) Uani 1 1 d . . . N7 N 0.2582(3) 0.8213(2) 0.1761(2) 0.0268(11) Uani 1 1 d . . . C32 C 0.2659(4) 0.8913(3) 0.1610(3) 0.0314(13) Uani 1 1 d . . . H32 H 0.3260 0.9104 0.1493 0.038 Uiso 1 1 calc R . . C33 C 0.1883(5) 0.9337(3) 0.1626(3) 0.0381(14) Uani 1 1 d . . . H33 H 0.1935 0.9820 0.1513 0.046 Uiso 1 1 calc R . . C34 C 0.1015(4) 0.9052(3) 0.1810(3) 0.0369(15) Uani 1 1 d . . . H34 H 0.0474 0.9345 0.1847 0.044 Uiso 1 1 calc R . . C35 C 0.0933(3) 0.8352(3) 0.1939(3) 0.0316(12) Uani 1 1 d . . . H35 H 0.0330 0.8159 0.2044 0.038 Uiso 1 1 calc R . . O15 O 0.2623(3) 0.7212(2) 0.3343(2) 0.0293(10) Uani 1 1 d . . . O16 O 0.4411(2) 0.70983(18) 0.3026(2) 0.0268(9) Uani 1 1 d . . . C36 C 0.3258(4) 0.7306(2) 0.3844(2) 0.0182(11) Uani 1 1 d . . . N8 N 0.4185(4) 0.7241(2) 0.3672(3) 0.0350(12) Uani 1 1 d . . . C37 C 0.4882(4) 0.7320(3) 0.4177(3) 0.0377(15) Uani 1 1 d . . . H37 H 0.5534 0.7276 0.4063 0.045 Uiso 1 1 calc R . . C38 C 0.4607(6) 0.7461(3) 0.4840(3) 0.055(2) Uani 1 1 d . . . H38 H 0.5073 0.7513 0.5192 0.065 Uiso 1 1 calc R . . C39 C 0.3649(6) 0.7530(3) 0.5009(3) 0.049(2) Uani 1 1 d . . . H39 H 0.3464 0.7638 0.5471 0.059 Uiso 1 1 calc R . . C40 C 0.2989(5) 0.7441(3) 0.4510(3) 0.0416(16) Uani 1 1 d . . . H40 H 0.2335 0.7474 0.4624 0.050 Uiso 1 1 calc R . . O17 O 0.5193(3) 0.8185(2) 0.1667(2) 0.0399(10) Uani 1 1 d D . . H17A H 0.529(3) 0.829(3) 0.2172(10) 0.060 Uiso 1 1 d D . . H17B H 0.4503(17) 0.809(3) 0.183(2) 0.060 Uiso 1 1 d D . . O18 O -0.0261(3) 0.5219(2) 0.1614(3) 0.0523(12) Uani 1 1 d D . . H18A H -0.094(2) 0.504(3) 0.174(3) 0.079 Uiso 1 1 d D . . H18B H -0.038(4) 0.483(3) 0.124(2) 0.079 Uiso 1 1 d D . . O19 O 0.1202(3) 0.6279(2) 0.0735(2) 0.0396(10) Uani 1 1 d D . . H19A H 0.101(4) 0.599(2) 0.0307(17) 0.059 Uiso 1 1 d D . . H19B H 0.105(4) 0.5803(18) 0.098(2) 0.059 Uiso 1 1 d D . . O20 O 0.0822(3) 0.7829(2) 0.36343(19) 0.0373(10) Uani 1 1 d D . . H20A H 0.147(2) 0.796(3) 0.384(2) 0.056 Uiso 1 1 d D . . H20B H 0.075(4) 0.763(3) 0.4139(14) 0.056 Uiso 1 1 d D . . O21 O 0.6610(3) 0.5676(3) 0.4392(3) 0.0612(14) Uani 1 1 d D . . H21A H 0.627(4) 0.616(2) 0.434(4) 0.092 Uiso 1 1 d D . . H21B H 0.713(3) 0.598(3) 0.414(3) 0.092 Uiso 1 1 d D . . O22 O 0.4570(4) 0.5601(2) 0.4213(3) 0.0664(15) Uani 1 1 d D . . H22A H 0.390(3) 0.570(4) 0.443(4) 0.100 Uiso 1 1 d D . . H22B H 0.466(5) 0.6109(18) 0.443(4) 0.100 Uiso 1 1 d D . . O23 O 0.9134(4) 0.4113(2) 0.0703(3) 0.0569(14) Uani 1 1 d D . . H23A H 0.877(4) 0.389(3) 0.030(2) 0.085 Uiso 1 1 d D . . H23B H 0.895(5) 0.363(2) 0.092(3) 0.085 Uiso 1 1 d D . . O24 O 0.4891(3) 0.4179(2) 0.4548(2) 0.0469(12) Uani 1 1 d D . . H24A H 0.512(4) 0.4703(15) 0.463(3) 0.070 Uiso 1 1 d D . . H24B H 0.439(3) 0.448(3) 0.428(3) 0.070 Uiso 1 1 d D . . O25 O 0.6706(5) 0.4373(3) 0.5194(4) 0.099(2) Uani 1 1 d D . . H25A H 0.679(7) 0.490(2) 0.497(4) 0.148 Uiso 1 1 d D . . H25B H 0.637(6) 0.474(4) 0.555(3) 0.148 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 Gd1 0.01379(12) 0.01951(12) 0.01922(13) -0.00029(12) 0.00002(12) 0.00021(11) Gd2 0.01331(12) 0.02016(12) 0.01839(13) 0.00193(12) -0.00014(12) -0.00041(11) Na1 0.0158(9) 0.0276(10) 0.0311(11) -0.0037(10) -0.0031(9) 0.0002(8) Na2 0.0180(10) 0.0369(12) 0.0323(12) 0.0065(10) -0.0007(9) -0.0002(9) O1 0.021(2) 0.0236(19) 0.035(2) -0.0091(17) -0.0028(17) 0.0011(16) O2 0.019(2) 0.0242(19) 0.0265(19) -0.0052(16) -0.0020(15) -0.0006(15) N1 0.023(2) 0.023(2) 0.026(2) -0.0011(18) 0.0001(18) -0.004(2) C1 0.024(3) 0.025(3) 0.015(3) 0.003(2) 0.001(2) 0.003(2) C2 0.027(3) 0.031(3) 0.040(3) 0.000(2) 0.006(2) 0.006(2) C3 0.053(4) 0.024(3) 0.041(4) -0.004(3) 0.020(3) 0.007(3) C4 0.042(4) 0.030(3) 0.049(4) -0.013(3) 0.005(3) -0.010(3) C5 0.033(3) 0.026(3) 0.043(4) -0.006(3) -0.001(3) -0.016(3) O3 0.0161(18) 0.029(2) 0.024(2) 0.0025(17) -0.0010(15) 0.0021(15) O4 0.0179(19) 0.034(2) 0.020(2) 0.0049(17) 0.0061(15) 0.0016(16) C6 0.012(2) 0.007(2) 0.011(2) 0.0005(17) -0.0038(18) -0.0007(18) N2 0.042(3) 0.022(2) 0.034(3) -0.002(2) -0.005(2) 0.002(2) C7 0.026(3) 0.029(3) 0.024(3) 0.004(2) -0.007(2) 0.001(2) C8 0.039(3) 0.025(3) 0.025(3) 0.000(2) -0.011(3) 0.004(3) C9 0.039(4) 0.027(3) 0.023(3) 0.005(3) 0.010(3) 0.004(3) C10 0.030(3) 0.024(3) 0.033(3) 0.004(2) 0.004(2) 0.006(2) O5 0.020(2) 0.0258(19) 0.049(2) -0.0061(17) 0.0072(17) -0.0028(17) O6 0.0186(18) 0.0206(16) 0.033(2) -0.0022(17) 0.0016(15) -0.0024(13) N3 0.025(2) 0.024(2) 0.030(3) 0.0026(19) -0.0020(19) -0.0067(18) C11 0.025(3) 0.019(3) 0.026(3) -0.002(2) 0.002(2) -0.003(2) C12 0.041(4) 0.028(3) 0.044(4) -0.014(3) -0.002(3) -0.002(2) C13 0.053(4) 0.030(3) 0.059(5) -0.009(3) -0.007(4) -0.015(3) C14 0.050(4) 0.038(3) 0.047(4) -0.003(3) -0.008(3) -0.023(3) C15 0.018(2) 0.044(3) 0.038(4) 0.008(3) 0.000(2) -0.002(3) O7 0.0166(19) 0.0303(19) 0.028(2) 0.0072(17) -0.0004(17) -0.0007(18) O8 0.0234(19) 0.034(2) 0.0165(19) 0.0024(16) 0.0023(15) 0.0075(16) C16 0.014(2) 0.012(2) 0.018(3) 0.000(2) 0.003(2) -0.0034(19) N4 0.027(3) 0.025(2) 0.032(3) -0.002(2) -0.003(2) -0.002(2) C17 0.021(3) 0.034(3) 0.035(3) -0.003(3) 0.001(2) 0.001(2) C18 0.032(3) 0.044(4) 0.035(4) -0.001(3) -0.012(3) 0.009(3) C19 0.046(4) 0.041(4) 0.017(3) 0.009(3) -0.006(3) 0.003(3) C20 0.035(3) 0.032(3) 0.028(3) 0.001(3) 0.007(3) -0.008(3) O9 0.0172(17) 0.0274(19) 0.0189(19) -0.0059(16) 0.0001(15) 0.0003(14) O10 0.0182(19) 0.032(2) 0.025(2) -0.0006(17) 0.0013(17) -0.0024(19) C21 0.017(3) 0.014(2) 0.016(3) -0.002(2) -0.003(2) 0.0009(19) N5 0.041(3) 0.021(2) 0.033(3) 0.002(2) 0.011(2) 0.005(2) C22 0.022(3) 0.029(3) 0.034(3) -0.005(3) 0.000(2) -0.005(2) C23 0.031(4) 0.039(4) 0.044(4) -0.008(3) 0.017(3) -0.001(3) C24 0.052(4) 0.043(4) 0.032(4) -0.013(3) 0.009(3) -0.004(3) C25 0.036(4) 0.028(3) 0.027(3) -0.009(3) -0.004(3) -0.004(3) O11 0.017(2) 0.0226(18) 0.033(2) 0.0054(16) 0.0022(15) 0.0053(15) O12 0.020(2) 0.0242(18) 0.036(2) 0.0045(16) -0.0041(16) -0.0013(15) C26 0.014(2) 0.019(2) 0.020(3) 0.001(2) 0.004(2) 0.0000(17) N6 0.032(3) 0.032(2) 0.038(3) 0.007(2) 0.002(2) 0.001(2) C27 0.030(3) 0.028(3) 0.054(4) 0.011(3) -0.008(3) 0.004(3) C28 0.046(4) 0.021(3) 0.055(4) 0.009(3) 0.003(3) 0.000(3) C29 0.034(4) 0.029(3) 0.041(3) 0.002(3) 0.003(3) -0.009(2) C30 0.026(3) 0.029(3) 0.038(3) 0.004(3) 0.001(3) -0.004(2) O13 0.0174(16) 0.0259(17) 0.031(2) 0.0075(15) -0.0004(16) -0.0033(16) O14 0.023(2) 0.0247(19) 0.039(2) 0.0104(17) -0.0075(17) -0.0087(16) C31 0.016(3) 0.025(3) 0.016(2) 0.000(2) -0.002(2) 0.001(2) N7 0.030(3) 0.027(3) 0.023(2) -0.002(2) -0.0072(19) 0.003(2) C32 0.029(3) 0.025(3) 0.041(4) 0.002(3) -0.005(3) -0.002(2) C33 0.054(4) 0.024(3) 0.037(3) -0.001(2) -0.018(3) 0.009(3) C34 0.041(4) 0.040(4) 0.030(3) -0.009(3) -0.011(3) 0.020(3) C35 0.021(3) 0.048(4) 0.025(3) 0.003(3) 0.001(2) 0.011(3) O15 0.023(2) 0.041(2) 0.023(2) -0.0050(18) 0.0060(17) 0.0038(18) O16 0.020(2) 0.034(2) 0.027(2) -0.0049(18) -0.0028(16) -0.0037(16) C36 0.020(3) 0.017(2) 0.017(2) -0.0050(19) 0.008(2) 0.001(2) N8 0.052(3) 0.023(2) 0.030(3) 0.001(2) -0.010(3) -0.004(2) C37 0.046(4) 0.028(3) 0.039(4) 0.002(3) -0.023(3) -0.007(3) C38 0.098(7) 0.034(4) 0.031(4) 0.006(3) -0.032(4) -0.016(4) C39 0.096(7) 0.032(4) 0.018(3) -0.007(3) 0.007(4) -0.017(4) C40 0.063(5) 0.033(3) 0.029(3) -0.003(3) 0.012(3) -0.010(3) O17 0.0199(19) 0.044(3) 0.056(3) 0.007(2) -0.0053(18) -0.0031(19) O18 0.030(2) 0.046(3) 0.081(4) -0.022(2) 0.010(2) -0.011(2) O19 0.029(2) 0.057(3) 0.033(2) -0.009(2) -0.0016(18) 0.005(2) O20 0.036(2) 0.046(2) 0.030(2) -0.0052(19) 0.0038(18) -0.004(2) O21 0.053(3) 0.068(3) 0.062(3) -0.001(3) 0.023(3) -0.015(3) O22 0.094(4) 0.037(3) 0.069(4) -0.003(3) -0.017(3) 0.009(3) O23 0.066(3) 0.030(2) 0.074(4) -0.015(2) -0.034(3) 0.005(2) O24 0.054(3) 0.038(3) 0.048(3) 0.007(2) 0.004(2) 0.005(2) O25 0.105(6) 0.067(4) 0.124(6) -0.012(4) 0.016(4) -0.005(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 O3 2.350(4) . ? Gd1 O6 2.381(3) . ? Gd1 O4 2.383(4) . ? Gd1 O8 2.383(3) . ? Gd1 O7 2.383(3) . ? Gd1 O1 2.386(3) . ? Gd1 O5 2.397(3) . ? Gd1 O2 2.405(3) . ? Gd1 Na1 3.4923(17) . ? Gd1 Na2 3.835(2) 1_655 ? Gd2 O11 2.368(3) . ? Gd2 O12 2.375(3) . ? Gd2 O13 2.375(3) . ? Gd2 O9 2.377(3) . ? Gd2 O15 2.379(4) . ? Gd2 O14 2.390(3) . ? Gd2 O10 2.400(4) . ? Gd2 O16 2.401(3) . ? Gd2 Na2 3.8263(19) . ? Gd2 Na1 3.8574(17) . ? Na1 O9 2.375(4) . ? Na1 O17 2.383(4) . ? Na1 O16 2.386(4) . ? Na1 O2 2.398(4) . ? Na1 O4 2.444(4) . ? Na1 O6 2.449(4) . ? Na2 O13 2.361(4) . ? Na2 O19 2.387(5) . ? Na2 O3 2.416(4) 1_455 ? Na2 O8 2.418(4) 1_455 ? Na2 O12 2.426(4) . ? Na2 O18 2.432(4) . ? Na2 Gd1 3.835(2) 1_455 ? O1 N1 1.339(5) . ? O2 C1 1.263(6) . ? N1 C5 1.356(6) . ? N1 C1 1.386(6) . ? C1 C2 1.400(7) . ? C2 C3 1.366(7) . ? C3 C4 1.396(9) . ? C4 C5 1.369(8) . ? O3 C6 1.339(5) . ? O3 Na2 2.416(4) 1_655 ? O4 N2 1.304(6) . ? C6 N2 1.358(6) . ? C6 C10 1.373(7) . ? N2 C7 1.414(7) . ? C7 C8 1.371(7) . ? C8 C9 1.406(8) . ? C9 C10 1.368(8) . ? O5 C11 1.294(6) . ? O6 N3 1.342(5) . ? N3 C15 1.360(6) . ? N3 C11 1.371(6) . ? C11 C12 1.414(7) . ? C12 C13 1.374(8) . ? C13 C14 1.406(9) . ? C14 C15 1.370(8) . ? O7 C16 1.322(6) . ? O8 N4 1.309(5) . ? O8 Na2 2.418(4) 1_655 ? C16 C20 1.355(7) . ? C16 N4 1.386(6) . ? N4 C17 1.403(7) . ? C17 C18 1.349(7) . ? C18 C19 1.380(8) . ? C19 C20 1.370(8) . ? O9 N5 1.324(5) . ? O10 C21 1.309(6) . ? C21 N5 1.355(6) . ? C21 C25 1.376(7) . ? N5 C22 1.389(7) . ? C22 C23 1.349(8) . ? C23 C24 1.416(8) . ? C24 C25 1.367(8) . ? O11 N7 1.335(5) . ? O12 C31 1.302(5) . ? C26 O13 1.310(5) . ? C26 N6 1.367(6) . ? C26 C30 1.390(6) . ? N6 O14 1.335(5) . ? N6 C27 1.360(6) . ? C27 C28 1.347(7) . ? C28 C29 1.394(8) . ? C29 C30 1.347(7) . ? C31 N7 1.365(6) . ? C31 C35 1.401(6) . ? N7 C32 1.374(7) . ? C32 C33 1.363(8) . ? C33 C34 1.387(8) . ? C34 C35 1.364(7) . ? O15 C36 1.328(6) . ? O16 N8 1.315(6) . ? C36 N8 1.356(7) . ? C36 C40 1.365(7) . ? N8 C37 1.392(7) . ? C37 C38 1.362(8) . ? C38 C39 1.397(10) . ? C39 C40 1.349(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Gd1 O6 132.79(12) . . ? O3 Gd1 O4 66.79(11) . . ? O6 Gd1 O4 76.93(12) . . ? O3 Gd1 O8 71.84(12) . . ? O6 Gd1 O8 133.43(11) . . ? O4 Gd1 O8 138.44(12) . . ? O3 Gd1 O7 137.71(13) . . ? O6 Gd1 O7 77.37(13) . . ? O4 Gd1 O7 153.70(13) . . ? O8 Gd1 O7 66.25(13) . . ? O3 Gd1 O1 87.30(12) . . ? O6 Gd1 O1 133.06(12) . . ? O4 Gd1 O1 106.89(13) . . ? O8 Gd1 O1 74.33(12) . . ? O7 Gd1 O1 86.85(13) . . ? O3 Gd1 O5 80.20(12) . . ? O6 Gd1 O5 66.11(12) . . ? O4 Gd1 O5 83.31(13) . . ? O8 Gd1 O5 86.09(12) . . ? O7 Gd1 O5 91.36(13) . . ? O1 Gd1 O5 159.32(12) . . ? O3 Gd1 O2 122.64(11) . . ? O6 Gd1 O2 71.01(11) . . ? O4 Gd1 O2 74.00(12) . . ? O8 Gd1 O2 135.69(12) . . ? O7 Gd1 O2 92.41(12) . . ? O1 Gd1 O2 65.76(12) . . ? O5 Gd1 O2 134.92(12) . . ? O3 Gd1 Na1 111.00(9) . . ? O6 Gd1 Na1 44.47(8) . . ? O4 Gd1 Na1 44.36(9) . . ? O8 Gd1 Na1 177.15(9) . . ? O7 Gd1 Na1 110.90(10) . . ? O1 Gd1 Na1 105.83(9) . . ? O5 Gd1 Na1 94.07(9) . . ? O2 Gd1 Na1 43.28(9) . . ? O3 Gd1 Na2 37.01(9) . 1_655 ? O6 Gd1 Na2 137.37(9) . 1_655 ? O4 Gd1 Na2 101.62(9) . 1_655 ? O8 Gd1 Na2 37.28(9) . 1_655 ? O7 Gd1 Na2 100.99(10) . 1_655 ? O1 Gd1 Na2 88.72(9) . 1_655 ? O5 Gd1 Na2 71.38(9) . 1_655 ? O2 Gd1 Na2 150.55(9) . 1_655 ? Na1 Gd1 Na2 145.34(5) . 1_655 ? O11 Gd2 O12 66.00(11) . . ? O11 Gd2 O13 136.26(11) . . ? O12 Gd2 O13 71.73(11) . . ? O11 Gd2 O9 81.04(11) . . ? O12 Gd2 O9 137.33(12) . . ? O13 Gd2 O9 127.35(11) . . ? O11 Gd2 O15 90.48(13) . . ? O12 Gd2 O15 73.51(12) . . ? O13 Gd2 O15 87.97(12) . . ? O9 Gd2 O15 135.46(12) . . ? O11 Gd2 O14 157.47(11) . . ? O12 Gd2 O14 133.10(12) . . ? O13 Gd2 O14 65.87(11) . . ? O9 Gd2 O14 86.19(12) . . ? O15 Gd2 O14 85.67(13) . . ? O11 Gd2 O10 89.95(12) . . ? O12 Gd2 O10 87.25(13) . . ? O13 Gd2 O10 77.12(12) . . ? O9 Gd2 O10 65.54(12) . . ? O15 Gd2 O10 158.69(13) . . ? O14 Gd2 O10 101.60(13) . . ? O11 Gd2 O16 82.33(12) . . ? O12 Gd2 O16 127.76(12) . . ? O13 Gd2 O16 135.12(12) . . ? O9 Gd2 O16 69.49(12) . . ? O15 Gd2 O16 66.05(12) . . ? O14 Gd2 O16 75.81(12) . . ? O10 Gd2 O16 135.03(13) . . ? O11 Gd2 Na2 100.29(8) . . ? O12 Gd2 Na2 37.63(8) . . ? O13 Gd2 Na2 35.98(8) . . ? O9 Gd2 Na2 137.01(9) . . ? O15 Gd2 Na2 87.49(9) . . ? O14 Gd2 Na2 101.71(9) . . ? O10 Gd2 Na2 71.48(10) . . ? O16 Gd2 Na2 153.49(9) . . ? O11 Gd2 Na1 70.01(8) . . ? O12 Gd2 Na1 135.41(9) . . ? O13 Gd2 Na1 152.83(9) . . ? O9 Gd2 Na1 35.71(8) . . ? O15 Gd2 Na1 100.40(9) . . ? O14 Gd2 Na1 88.84(9) . . ? O10 Gd2 Na1 99.76(10) . . ? O16 Gd2 Na1 36.18(9) . . ? Na2 Gd2 Na1 167.34(4) . . ? O9 Na1 O17 88.35(14) . . ? O9 Na1 O16 69.77(13) . . ? O17 Na1 O16 95.14(14) . . ? O9 Na1 O2 158.66(14) . . ? O17 Na1 O2 112.70(14) . . ? O16 Na1 O2 103.41(14) . . ? O9 Na1 O4 110.51(14) . . ? O17 Na1 O4 93.83(14) . . ? O16 Na1 O4 171.02(15) . . ? O2 Na1 O4 73.01(13) . . ? O9 Na1 O6 90.33(12) . . ? O17 Na1 O6 167.01(16) . . ? O16 Na1 O6 96.52(13) . . ? O2 Na1 O6 69.97(12) . . ? O4 Na1 O6 74.54(13) . . ? O9 Na1 Gd1 124.86(10) . . ? O17 Na1 Gd1 129.96(11) . . ? O16 Na1 Gd1 129.07(11) . . ? O2 Na1 Gd1 43.42(9) . . ? O4 Na1 Gd1 42.96(9) . . ? O6 Na1 Gd1 42.94(7) . . ? O9 Na1 Gd2 35.74(8) . . ? O17 Na1 Gd2 82.23(10) . . ? O16 Na1 Gd2 36.44(9) . . ? O2 Na1 Gd2 139.71(11) . . ? O4 Na1 Gd2 145.76(11) . . ? O6 Na1 Gd2 104.00(9) . . ? Gd1 Na1 Gd2 146.93(6) . . ? O13 Na2 O19 95.25(14) . . ? O13 Na2 O3 158.93(15) . 1_455 ? O19 Na2 O3 102.97(15) . 1_455 ? O13 Na2 O8 92.21(13) . 1_455 ? O19 Na2 O8 172.26(15) . 1_455 ? O3 Na2 O8 70.11(13) 1_455 1_455 ? O13 Na2 O12 71.09(12) . . ? O19 Na2 O12 82.78(14) . . ? O3 Na2 O12 100.54(13) 1_455 . ? O8 Na2 O12 101.65(14) 1_455 . ? O13 Na2 O18 98.99(15) . . ? O19 Na2 O18 88.12(17) . . ? O3 Na2 O18 92.17(15) 1_455 . ? O8 Na2 O18 88.68(15) 1_455 . ? O12 Na2 O18 165.74(16) . . ? O13 Na2 Gd2 36.24(8) . . ? O19 Na2 Gd2 80.22(11) . . ? O3 Na2 Gd2 137.04(11) 1_455 . ? O8 Na2 Gd2 107.15(10) 1_455 . ? O12 Na2 Gd2 36.70(8) . . ? O18 Na2 Gd2 130.76(12) . . ? O13 Na2 Gd1 128.70(11) . 1_455 ? O19 Na2 Gd1 135.71(12) . 1_455 ? O3 Na2 Gd1 35.84(9) 1_455 1_455 ? O8 Na2 Gd1 36.65(9) 1_455 1_455 ? O12 Na2 Gd1 113.45(10) . 1_455 ? O18 Na2 Gd1 80.69(11) . 1_455 ? Gd2 Na2 Gd1 137.48(6) . 1_455 ? N1 O1 Gd1 118.2(3) . . ? C1 O2 Na1 135.2(3) . . ? C1 O2 Gd1 119.6(3) . . ? Na1 O2 Gd1 93.29(12) . . ? O1 N1 C5 119.6(4) . . ? O1 N1 C1 117.1(4) . . ? C5 N1 C1 123.3(5) . . ? O2 C1 N1 118.5(5) . . ? O2 C1 C2 125.5(5) . . ? N1 C1 C2 116.0(5) . . ? C3 C2 C1 121.3(5) . . ? C2 C3 C4 120.5(5) . . ? C5 C4 C3 118.7(5) . . ? N1 C5 C4 120.1(5) . . ? C6 O3 Gd1 117.6(3) . . ? C6 O3 Na2 125.4(3) . 1_655 ? Gd1 O3 Na2 107.15(15) . 1_655 ? N2 O4 Gd1 117.7(3) . . ? N2 O4 Na1 149.3(3) . . ? Gd1 O4 Na1 92.67(13) . . ? O3 C6 N2 117.9(5) . . ? O3 C6 C10 120.5(5) . . ? N2 C6 C10 121.7(5) . . ? O4 N2 C6 118.4(5) . . ? O4 N2 C7 123.1(5) . . ? C6 N2 C7 118.5(5) . . ? C8 C7 N2 120.2(5) . . ? C7 C8 C9 120.0(5) . . ? C10 C9 C8 118.9(6) . . ? C9 C10 C6 120.7(5) . . ? C11 O5 Gd1 120.0(3) . . ? N3 O6 Gd1 117.9(3) . . ? N3 O6 Na1 120.0(3) . . ? Gd1 O6 Na1 92.59(12) . . ? O6 N3 C15 120.5(4) . . ? O6 N3 C11 118.6(4) . . ? C15 N3 C11 120.9(4) . . ? O5 C11 N3 117.3(4) . . ? O5 C11 C12 124.4(5) . . ? N3 C11 C12 118.3(5) . . ? C13 C12 C11 121.0(6) . . ? C12 C13 C14 118.8(6) . . ? C15 C14 C13 119.4(6) . . ? N3 C15 C14 121.6(5) . . ? C16 O7 Gd1 118.1(3) . . ? N4 O8 Gd1 116.9(3) . . ? N4 O8 Na2 136.5(3) . 1_655 ? Gd1 O8 Na2 106.07(14) . 1_655 ? O7 C16 C20 123.9(5) . . ? O7 C16 N4 116.0(4) . . ? C20 C16 N4 120.1(5) . . ? O8 N4 C16 119.1(4) . . ? O8 N4 C17 122.3(5) . . ? C16 N4 C17 118.5(5) . . ? C18 C17 N4 120.4(5) . . ? C17 C18 C19 120.6(6) . . ? C20 C19 C18 119.2(5) . . ? C16 C20 C19 121.2(5) . . ? N5 O9 Na1 126.9(3) . . ? N5 O9 Gd2 118.8(3) . . ? Na1 O9 Gd2 108.54(14) . . ? C21 O10 Gd2 119.1(3) . . ? O10 C21 N5 117.2(4) . . ? O10 C21 C25 123.2(5) . . ? N5 C21 C25 119.6(5) . . ? O9 N5 C21 118.5(4) . . ? O9 N5 C22 121.2(5) . . ? C21 N5 C22 120.3(5) . . ? C23 C22 N5 121.5(5) . . ? C22 C23 C24 117.7(5) . . ? C25 C24 C23 120.4(6) . . ? C24 C25 C21 120.3(6) . . ? N7 O11 Gd2 117.7(3) . . ? C31 O12 Gd2 117.2(3) . . ? C31 O12 Na2 136.4(3) . . ? Gd2 O12 Na2 105.67(13) . . ? O13 C26 N6 117.6(4) . . ? O13 C26 C30 123.7(4) . . ? N6 C26 C30 118.7(5) . . ? O14 N6 C27 122.5(5) . . ? O14 N6 C26 117.5(4) . . ? C27 N6 C26 120.0(5) . . ? C28 C27 N6 121.7(6) . . ? C27 C28 C29 119.0(5) . . ? C30 C29 C28 119.7(5) . . ? C29 C30 C26 120.9(5) . . ? C26 O13 Na2 132.5(3) . . ? C26 O13 Gd2 119.6(3) . . ? Na2 O13 Gd2 107.78(13) . . ? N6 O14 Gd2 117.9(3) . . ? O12 C31 N7 118.5(4) . . ? O12 C31 C35 123.9(4) . . ? N7 C31 C35 117.6(4) . . ? O11 N7 C31 116.5(4) . . ? O11 N7 C32 121.9(4) . . ? C31 N7 C32 121.6(4) . . ? C33 C32 N7 120.7(5) . . ? C32 C33 C34 118.8(5) . . ? C35 C34 C33 120.5(5) . . ? C34 C35 C31 120.8(5) . . ? C36 O15 Gd2 117.4(3) . . ? N8 O16 Na1 136.1(3) . . ? N8 O16 Gd2 116.4(3) . . ? Na1 O16 Gd2 107.37(15) . . ? O15 C36 N8 117.5(4) . . ? O15 C36 C40 121.4(5) . . ? N8 C36 C40 121.0(6) . . ? O16 N8 C36 118.9(5) . . ? O16 N8 C37 120.9(5) . . ? C36 N8 C37 120.1(5) . . ? C38 C37 N8 118.4(6) . . ? C37 C38 C39 120.9(6) . . ? C40 C39 C38 119.4(6) . . ? C39 C40 C36 120.2(7) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.756 _refine_diff_density_min -0.431 _refine_diff_density_rms 0.098 #======END data_4 _database_code_CSD 200688 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H18 Dy N3 O9' _chemical_formula_weight 546.82 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 6.3254(2) _cell_length_b 11.7520(4) _cell_length_c 13.6109(5) _cell_angle_alpha 103.7060(10) _cell_angle_beta 100.7370(10) _cell_angle_gamma 104.5080(10) _cell_volume 918.59(5) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 6392 _cell_measurement_theta_min 2.801 _cell_measurement_theta_max 32.371 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.977 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 534 _exptl_absorpt_coefficient_mu 4.123 _exptl_absorpt_correction_type semi-empirical _exptl_absorpt_correction_T_min 0.783318 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS (Bruker-AXS)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 '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_% ? _diffrn_reflns_number 15602 _diffrn_reflns_av_R_equivalents 0.0193 _diffrn_reflns_av_sigmaI/netI 0.0197 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 32.45 _reflns_number_total 6182 _reflns_number_gt 5839 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0310P)^2^+0.0116P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6182 _refine_ls_number_parameters 277 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0192 _refine_ls_R_factor_gt 0.0175 _refine_ls_wR_factor_ref 0.0453 _refine_ls_wR_factor_gt 0.0447 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 0.176957(11) 0.274881(6) 0.350775(5) 0.01524(3) Uani 1 1 d . . . O1 O 0.5253(2) 0.30741(11) 0.47613(10) 0.0207(2) Uani 1 1 d . . . O2 O 0.1458(2) 0.15267(16) 0.46098(13) 0.0382(4) Uani 1 1 d . . . N1 N 0.5277(3) 0.23274(15) 0.53534(13) 0.0243(3) Uani 1 1 d . . . C1 C 0.3233(3) 0.15110(16) 0.52738(14) 0.0236(3) Uani 1 1 d . . . C2 C 0.3142(4) 0.0692(2) 0.58574(19) 0.0435(6) Uani 1 1 d . . . H2 H 0.1730 0.0124 0.5803 0.052 Uiso 1 1 calc R . . C3 C 0.5061(5) 0.0693(2) 0.6510(2) 0.0544(8) Uani 1 1 d . . . H3 H 0.4980 0.0131 0.6911 0.065 Uiso 1 1 calc R . . C4 C 0.7142(5) 0.1517(3) 0.6588(2) 0.0551(8) Uani 1 1 d . . . H4 H 0.8484 0.1520 0.7040 0.066 Uiso 1 1 calc R . . C5 C 0.7229(4) 0.2325(2) 0.6005(2) 0.0380(5) Uani 1 1 d . . . H5 H 0.8641 0.2887 0.6050 0.046 Uiso 1 1 calc R . . O3 O 0.4739(2) 0.43520(11) 0.33848(10) 0.0221(2) Uani 1 1 d . . . O4 O 0.0606(2) 0.38065(13) 0.23309(11) 0.0291(3) Uani 1 1 d . . . N2 N 0.4311(3) 0.49263(14) 0.26711(12) 0.0243(3) Uani 1 1 d . . . C6 C 0.2096(3) 0.46254(16) 0.21155(14) 0.0243(3) Uani 1 1 d . . . C7 C 0.1630(5) 0.5213(2) 0.1357(2) 0.0440(6) Uani 1 1 d . . . H7 H 0.0112 0.5037 0.0969 0.053 Uiso 1 1 calc R . . C8 C 0.3347(6) 0.6045(3) 0.1165(2) 0.0598(9) Uani 1 1 d . . . H8 H 0.3014 0.6433 0.0644 0.072 Uiso 1 1 calc R . . C9 C 0.5572(5) 0.6314(3) 0.1738(2) 0.0564(8) Uani 1 1 d . . . H9 H 0.6764 0.6888 0.1610 0.068 Uiso 1 1 calc R . . C10 C 0.6028(4) 0.5751(2) 0.2483(2) 0.0406(5) Uani 1 1 d . . . H10 H 0.7544 0.5930 0.2874 0.049 Uiso 1 1 calc R . . O5 O 0.3544(2) 0.16915(11) 0.23808(10) 0.0220(2) Uani 1 1 d . . . O6 O -0.0742(2) 0.09300(11) 0.22362(10) 0.0233(2) Uani 1 1 d . . . N3 N 0.2292(2) 0.05791(13) 0.16958(11) 0.0189(3) Uani 1 1 d . . . C11 C 0.0022(3) 0.02068(15) 0.16432(13) 0.0189(3) Uani 1 1 d . . . C12 C -0.1259(3) -0.09591(16) 0.09233(15) 0.0254(3) Uani 1 1 d . . . H12 H -0.2830 -0.1268 0.0865 0.030 Uiso 1 1 calc R . . C13 C -0.0265(4) -0.16505(18) 0.03090(16) 0.0292(4) Uani 1 1 d . . . H13 H -0.1158 -0.2426 -0.0176 0.035 Uiso 1 1 calc R . . C14 C 0.2063(4) -0.12208(18) 0.03913(15) 0.0281(4) Uani 1 1 d . . . H14 H 0.2759 -0.1698 -0.0030 0.034 Uiso 1 1 calc R . . C15 C 0.3305(3) -0.00961(17) 0.10946(14) 0.0236(3) Uani 1 1 d . . . H15 H 0.4881 0.0213 0.1163 0.028 Uiso 1 1 calc R . . O7 O -0.1998(2) 0.25495(14) 0.35505(11) 0.0254(3) Uani 1 1 d . . . O8 O 0.1788(3) 0.44473(17) 0.49334(13) 0.0369(4) Uani 1 1 d . . . O9 O 0.5950(3) 0.30320(16) 0.11584(13) 0.0320(3) Uani 1 1 d . . . H8A H 0.282(5) 0.474(2) 0.543(2) 0.031(7) Uiso 1 1 d . . . H7A H -0.293(5) 0.219(3) 0.306(2) 0.038(7) Uiso 1 1 d . . . H7B H -0.265(5) 0.277(2) 0.398(2) 0.036(7) Uiso 1 1 d . . . H9A H 0.537(6) 0.281(3) 0.144(3) 0.055(11) Uiso 1 1 d . . . H9B H 0.741(6) 0.323(3) 0.163(3) 0.064(10) Uiso 1 1 d . . . H8B H 0.103(7) 0.465(4) 0.496(4) 0.079(15) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.01168(4) 0.01606(4) 0.01749(4) 0.00476(3) 0.00366(3) 0.00378(3) O1 0.0171(5) 0.0223(6) 0.0246(6) 0.0109(5) 0.0051(4) 0.0057(4) O2 0.0186(6) 0.0478(9) 0.0467(9) 0.0343(8) -0.0028(6) -0.0033(6) N1 0.0216(7) 0.0244(7) 0.0244(7) 0.0085(6) 0.0026(6) 0.0042(6) C1 0.0184(7) 0.0239(8) 0.0247(8) 0.0132(6) -0.0004(6) -0.0012(6) C2 0.0393(12) 0.0396(12) 0.0396(12) 0.0266(10) -0.0068(9) -0.0100(9) C3 0.0590(16) 0.0409(12) 0.0473(14) 0.0296(11) -0.0189(12) -0.0040(11) C4 0.0470(14) 0.0516(15) 0.0541(16) 0.0298(13) -0.0200(12) 0.0044(12) C5 0.0241(9) 0.0386(11) 0.0432(12) 0.0184(10) -0.0072(8) 0.0015(8) O3 0.0186(5) 0.0228(6) 0.0227(6) 0.0098(5) 0.0026(4) 0.0021(4) O4 0.0208(6) 0.0335(7) 0.0327(7) 0.0189(6) 0.0006(5) 0.0040(5) N2 0.0258(7) 0.0204(7) 0.0243(7) 0.0084(5) 0.0045(6) 0.0028(6) C6 0.0265(8) 0.0195(7) 0.0233(8) 0.0084(6) 0.0001(6) 0.0034(6) C7 0.0479(14) 0.0382(12) 0.0400(12) 0.0226(10) -0.0054(10) 0.0054(10) C8 0.075(2) 0.0457(14) 0.0527(16) 0.0361(13) 0.0001(14) 0.0006(14) C9 0.0619(18) 0.0411(13) 0.0559(16) 0.0304(12) 0.0079(13) -0.0116(12) C10 0.0344(11) 0.0354(11) 0.0439(12) 0.0184(10) 0.0058(9) -0.0063(9) O5 0.0158(5) 0.0205(5) 0.0233(6) -0.0017(4) 0.0048(4) 0.0027(4) O6 0.0155(5) 0.0211(6) 0.0288(6) 0.0007(5) 0.0056(5) 0.0041(4) N3 0.0170(6) 0.0186(6) 0.0190(6) 0.0032(5) 0.0025(5) 0.0058(5) C11 0.0162(7) 0.0183(7) 0.0207(7) 0.0062(6) 0.0019(5) 0.0048(5) C12 0.0207(8) 0.0200(7) 0.0287(9) 0.0038(6) -0.0012(6) 0.0035(6) C13 0.0345(10) 0.0201(8) 0.0252(8) 0.0009(7) -0.0019(7) 0.0080(7) C14 0.0368(10) 0.0253(8) 0.0238(8) 0.0048(7) 0.0069(7) 0.0156(8) C15 0.0250(8) 0.0275(8) 0.0215(8) 0.0068(6) 0.0076(6) 0.0128(7) O7 0.0127(5) 0.0328(7) 0.0246(6) -0.0005(5) 0.0040(5) 0.0057(5) O8 0.0231(7) 0.0479(9) 0.0271(7) -0.0124(6) -0.0052(6) 0.0201(7) O9 0.0278(7) 0.0390(8) 0.0284(7) 0.0095(6) 0.0079(6) 0.0091(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 O2 2.3110(14) . ? Dy1 O7 2.3483(13) . ? Dy1 O5 2.3652(12) . ? Dy1 O3 2.3663(12) . ? Dy1 O6 2.3682(12) . ? Dy1 O4 2.3696(13) . ? Dy1 O1 2.4044(12) . ? Dy1 O8 2.4277(15) . ? O1 N1 1.3256(19) . ? O2 C1 1.311(2) . ? N1 C1 1.371(2) . ? N1 C5 1.380(3) . ? C1 C2 1.383(3) . ? C2 C3 1.363(3) . ? C3 C4 1.394(4) . ? C4 C5 1.372(3) . ? O3 N2 1.3330(19) . ? O4 C6 1.297(2) . ? N2 C10 1.371(3) . ? N2 C6 1.375(2) . ? C6 C7 1.399(3) . ? C7 C8 1.377(4) . ? C8 C9 1.393(4) . ? C9 C10 1.361(4) . ? O5 N3 1.3542(18) . ? O6 C11 1.278(2) . ? N3 C15 1.361(2) . ? N3 C11 1.375(2) . ? C11 C12 1.416(2) . ? C12 C13 1.372(3) . ? C13 C14 1.405(3) . ? C14 C15 1.371(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Dy1 O7 81.57(5) . . ? O2 Dy1 O5 98.90(6) . . ? O7 Dy1 O5 134.74(5) . . ? O2 Dy1 O3 134.25(5) . . ? O7 Dy1 O3 133.45(5) . . ? O5 Dy1 O3 76.71(4) . . ? O2 Dy1 O6 83.06(5) . . ? O7 Dy1 O6 68.94(5) . . ? O5 Dy1 O6 66.25(4) . . ? O3 Dy1 O6 131.61(4) . . ? O2 Dy1 O4 158.25(5) . . ? O7 Dy1 O4 76.93(5) . . ? O5 Dy1 O4 93.96(5) . . ? O3 Dy1 O4 65.87(4) . . ? O6 Dy1 O4 86.20(5) . . ? O2 Dy1 O1 65.79(5) . . ? O7 Dy1 O1 135.99(5) . . ? O5 Dy1 O1 81.16(4) . . ? O3 Dy1 O1 68.57(4) . . ? O6 Dy1 O1 130.55(4) . . ? O4 Dy1 O1 134.04(4) . . ? O2 Dy1 O8 88.33(7) . . ? O7 Dy1 O8 72.11(5) . . ? O5 Dy1 O8 152.79(5) . . ? O3 Dy1 O8 79.49(6) . . ? O6 Dy1 O8 140.93(5) . . ? O4 Dy1 O8 88.17(6) . . ? O1 Dy1 O8 78.00(5) . . ? N1 O1 Dy1 118.11(10) . . ? C1 O2 Dy1 121.82(11) . . ? O1 N1 C1 116.44(14) . . ? O1 N1 C5 123.26(16) . . ? C1 N1 C5 120.28(17) . . ? O2 C1 N1 117.25(15) . . ? O2 C1 C2 123.28(18) . . ? N1 C1 C2 119.43(18) . . ? C3 C2 C1 120.6(2) . . ? C2 C3 C4 120.1(2) . . ? C5 C4 C3 119.2(2) . . ? C4 C5 N1 120.4(2) . . ? N2 O3 Dy1 118.97(10) . . ? C6 O4 Dy1 120.26(11) . . ? O3 N2 C10 120.91(17) . . ? O3 N2 C6 117.14(14) . . ? C10 N2 C6 121.91(17) . . ? O4 C6 N2 117.15(15) . . ? O4 C6 C7 125.21(19) . . ? N2 C6 C7 117.64(18) . . ? C8 C7 C6 120.7(2) . . ? C7 C8 C9 119.8(2) . . ? C10 C9 C8 119.6(2) . . ? C9 C10 N2 120.3(2) . . ? N3 O5 Dy1 118.04(9) . . ? C11 O6 Dy1 120.30(10) . . ? O5 N3 C15 119.47(14) . . ? O5 N3 C11 116.82(13) . . ? C15 N3 C11 123.70(15) . . ? O6 C11 N3 117.97(14) . . ? O6 C11 C12 126.05(16) . . ? N3 C11 C12 115.98(15) . . ? C13 C12 C11 121.07(17) . . ? C12 C13 C14 120.51(17) . . ? C15 C14 C13 118.39(17) . . ? N3 C15 C14 120.33(17) . . ? _diffrn_measured_fraction_theta_max 0.932 _diffrn_reflns_theta_full 32.45 _diffrn_measured_fraction_theta_full 0.932 _refine_diff_density_max 1.322 _refine_diff_density_min -0.767 _refine_diff_density_rms 0.091 #======END