data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author ; 'Annie K. Powell' ; _publ_contact_author_email annie.powell@kit.edu _publ_contact_author_phone '+49 721 608 2135' _publ_section_title ; Heterometallic 20-Membered {Fe16Ln4} (Ln = Sm, Eu, Gd, Tb, Dy, Ho) Metallo-Ring Aggregates ; loop_ _publ_author_name _publ_author_address 'Amer Baniodeh' ; Institut f\"ur Anorganische Chemie Karlsruhe Institute of Technology Engesserstr. 15 D-76131 Karlsruhe Germany ; 'Ian J. Hewitt' ; Institut f\"ur Anorganische Chemie Karlsruhe Institute of Technology Engesserstr. 15 D-76131 Karlsruhe Germany ; 'Valeriu Mereacre' ; Institut f\"ur Anorganische Chemie Karlsruhe Institute of Technology Engesserstr. 15 D-76131 Karlsruhe Germany ; 'Ghenadie Novitchi' ; Institut f\"ur Anorganische Chemie Karlsruhe Institute of Technology Engesserstr. 15 D-76131 Karlsruhe Germany ; 'Yanhua Lan' ; Institut f\"ur Anorganische Chemie Karlsruhe Institute of Technology Engesserstr. 15 D-76131 Karlsruhe Germany ; 'Christopher E. Anson' ; Institut f\"ur Anorganische Chemie Karlsruhe Institute of Technology Engesserstr. 15 D-76131 Karlsruhe Germany ; ; A.K.Powell ; ; Institut f\"ur Anorganische Chemie Karlsruhe Institute of Technology Engesserstr. 15 D-76131 Karlsruhe Germany ; _publ_contact_author_name 'Annie K. Powell' ########################################################################### data_amac16gds _database_code_depnum_ccdc_archive 'CCDC 780083' #TrackingRef '- amer_fe16ln4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C136 H276 Fe16 Gd4 N20 O76, 4(N O3), 10(C2 H3 N), 16(H2 O) ' _chemical_formula_sum 'C156 H338 Fe16 Gd4 N34 O104' _chemical_formula_weight 5877.20 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' Fe Fe 0.3463 0.8444 '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 'C c c a' _symmetry_space_group_name_Hall '-C 2b 2bc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' '-x, y, -z+1/2' 'x+1/2, -y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1, -y+1/2, z' '-x+1/2, y+1/2, -z+1/2' 'x+1, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' 'x, -y, z-1/2' '-x-1/2, y, z-1/2' '-x+1/2, -y+1/2, -z' 'x, y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' '-x, y+1/2, z-1/2' _cell_length_a 27.7908(14) _cell_length_b 27.9903(15) _cell_length_c 31.269(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 24324(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 40160 _cell_measurement_theta_min 1.46 _cell_measurement_theta_max 27.98 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.605 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 12064 _exptl_absorpt_coefficient_mu 2.090 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.391 _exptl_absorpt_correction_T_max 0.572 _exptl_absorpt_process_details ; XPREP in SHELXTL 6.14 (BrukerAXS Inc., 2003) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS II' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean 6.667 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 77829 _diffrn_reflns_av_R_equivalents 0.0611 _diffrn_reflns_av_sigmaI/netI 0.0372 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 26.73 _reflns_number_total 12913 _reflns_number_gt 8197 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'WinXpose 1.6.8 (Stoe & Cie GmbH, 2004)' _computing_cell_refinement 'X-Area 1.38 (Stoe & Cie GmbH, 2006)' _computing_data_reduction 'X-Area 1.38 (Stoe & Cie GmbH, 2006)' _computing_structure_solution 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_structure_refinement 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_molecular_graphics 'Diamond 2.1 (Crystal Impact, 1998)' _computing_publication_material 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _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. One lattice MeCN in the asymmetric unit (four per Fe16Gd4) could be refined anisotropically. The nitrates, waters and remaining MeCN were more badly disordered, and could not be refined satisfactorily; they were treated using SQUEEZE. The data were corrected for 1604 electrons per unit cell, or 401 per Fe16Gd4 unit (calc. for 4 nitrates, 4MeCN and 10H2O: 420 electrons - c.f. the Fe16Dy4 analogue). ; # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.250 0.000 -0.004 6170 1604 ' ' _platon_squeeze_details ; A.L.Spek, J.Appl.Cryst. 2003, 36, 7-13 ; _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^)+(0.0709P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12913 _refine_ls_number_parameters 613 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0697 _refine_ls_R_factor_gt 0.0505 _refine_ls_wR_factor_ref 0.1212 _refine_ls_wR_factor_gt 0.1172 _refine_ls_goodness_of_fit_ref 0.991 _refine_ls_restrained_S_all 0.991 _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 Gd1 Gd 0.359076(8) 0.344084(7) 0.678292(9) 0.04737(8) Uani 1 1 d . . . Fe1 Fe 0.46314(2) 0.40095(2) 0.71318(3) 0.04858(18) Uani 1 1 d . . . Fe2 Fe 0.35870(2) 0.31985(2) 0.57189(3) 0.04926(18) Uani 1 1 d . . . Fe3 Fe 0.41371(2) 0.35677(2) 0.48837(3) 0.05299(19) Uani 1 1 d . . . Fe4 Fe 0.47236(3) 0.30165(2) 0.41235(3) 0.0561(2) Uani 1 1 d . . . N1 N 0.49654(14) 0.41037(12) 0.64805(15) 0.0504(10) Uani 1 1 d . . . C1 C 0.54721(17) 0.42449(17) 0.65805(19) 0.0535(12) Uani 1 1 d . . . H1A H 0.5478 0.4580 0.6683 0.064 Uiso 1 1 calc R . . H1B H 0.5670 0.4225 0.6318 0.064 Uiso 1 1 calc R . . C2 C 0.56827(17) 0.39210(17) 0.69195(18) 0.0542(13) Uani 1 1 d . . . H2A H 0.5764 0.3607 0.6793 0.065 Uiso 1 1 calc R . . H2B H 0.5981 0.4064 0.7037 0.065 Uiso 1 1 calc R . . O1 O 0.53364(11) 0.38617(11) 0.72511(12) 0.0521(8) Uani 1 1 d . . . C3 C 0.49288(17) 0.36305(15) 0.62656(18) 0.0512(12) Uani 1 1 d . . . H3A H 0.5237 0.3555 0.6122 0.061 Uiso 1 1 calc R . . H3B H 0.4674 0.3643 0.6044 0.061 Uiso 1 1 calc R . . C4 C 0.48109(16) 0.32407(15) 0.65874(18) 0.0490(12) Uani 1 1 d . . . H4A H 0.4705 0.2948 0.6437 0.059 Uiso 1 1 calc R . . H4B H 0.5100 0.3162 0.6759 0.059 Uiso 1 1 calc R . . O2 O 0.44353(10) 0.34123(10) 0.68595(11) 0.0473(8) Uani 1 1 d . . . C5 C 0.47055(19) 0.44884(16) 0.62460(19) 0.0571(13) Uani 1 1 d . . . H5A H 0.4630 0.4747 0.6452 0.069 Uiso 1 1 calc R . . H5B H 0.4396 0.4357 0.6143 0.069 Uiso 1 1 calc R . . C6 C 0.4966(2) 0.47090(17) 0.58660(18) 0.0587(13) Uani 1 1 d . . . H6A H 0.4753 0.4952 0.5735 0.070 Uiso 1 1 calc R . . H6B H 0.5257 0.4876 0.5972 0.070 Uiso 1 1 calc R . . O3 O 0.51057(12) 0.43810(12) 0.55478(13) 0.0592(9) Uani 1 1 d . . . H3 H 0.4867 0.4314 0.5394 0.089 Uiso 1 1 calc R . . N2 N 0.30316(15) 0.42039(15) 0.67130(16) 0.0585(11) Uani 1 1 d . . . C7 C 0.3290(2) 0.46339(18) 0.6886(2) 0.0653(16) Uani 1 1 d . . . H7A H 0.3453 0.4801 0.6647 0.078 Uiso 1 1 calc R . . H7B H 0.3051 0.4857 0.7010 0.078 Uiso 1 1 calc R . . C8 C 0.36575(18) 0.45125(18) 0.7222(2) 0.0624(15) Uani 1 1 d . . . H8A H 0.3862 0.4794 0.7281 0.075 Uiso 1 1 calc R . . H8B H 0.3494 0.4420 0.7490 0.075 Uiso 1 1 calc R . . O4 O 0.39458(11) 0.41289(10) 0.70718(13) 0.0553(9) Uani 1 1 d . . . C9 C 0.29339(18) 0.42731(17) 0.6250(2) 0.0620(15) Uani 1 1 d . . . H9A H 0.2805 0.4599 0.6203 0.074 Uiso 1 1 calc R . . H9B H 0.2686 0.4041 0.6156 0.074 Uiso 1 1 calc R . . C10 C 0.33846(18) 0.42063(16) 0.5983(2) 0.0588(14) Uani 1 1 d . . . H10A H 0.3301 0.4211 0.5676 0.071 Uiso 1 1 calc R . . H10B H 0.3612 0.4471 0.6039 0.071 Uiso 1 1 calc R . . O5 O 0.36067(11) 0.37615(10) 0.60885(12) 0.0530(8) Uani 1 1 d . . . C11 C 0.2583(2) 0.4111(2) 0.6946(2) 0.0691(16) Uani 1 1 d . . . H11A H 0.2397 0.3863 0.6791 0.083 Uiso 1 1 calc R . . H11B H 0.2387 0.4406 0.6950 0.083 Uiso 1 1 calc R . . C12 C 0.2666(2) 0.3949(2) 0.7392(2) 0.0741(18) Uani 1 1 d . . . H12A H 0.2771 0.4222 0.7571 0.089 Uiso 1 1 calc R . . H12B H 0.2366 0.3818 0.7514 0.089 Uiso 1 1 calc R . . O6 O 0.30355(14) 0.35852(13) 0.73849(14) 0.0672(11) Uani 1 1 d D . . H6 H 0.309(2) 0.351(2) 0.7678(12) 0.081 Uiso 1 1 d D . . N3 N 0.36388(13) 0.24331(13) 0.54968(14) 0.0501(10) Uani 1 1 d . . . C13 C 0.35624(18) 0.21593(16) 0.58965(17) 0.0522(12) Uani 1 1 d . . . H13A H 0.3668 0.1825 0.5854 0.063 Uiso 1 1 calc R . . H13B H 0.3215 0.2156 0.5968 0.063 Uiso 1 1 calc R . . C14 C 0.38427(18) 0.23796(14) 0.62622(18) 0.0523(12) Uani 1 1 d . . . H14A H 0.3717 0.2258 0.6538 0.063 Uiso 1 1 calc R . . H14B H 0.4186 0.2287 0.6240 0.063 Uiso 1 1 calc R . . O7 O 0.38018(11) 0.28836(10) 0.62515(11) 0.0463(8) Uani 1 1 d . . . C15 C 0.41352(17) 0.23774(16) 0.53140(19) 0.0539(12) Uani 1 1 d . . . H15A H 0.4115 0.2379 0.4998 0.065 Uiso 1 1 calc R . . H15B H 0.4269 0.2065 0.5403 0.065 Uiso 1 1 calc R . . C16 C 0.44742(16) 0.27762(15) 0.54607(19) 0.0529(13) Uani 1 1 d . . . H16A H 0.4578 0.2715 0.5759 0.063 Uiso 1 1 calc R . . H16B H 0.4764 0.2781 0.5277 0.063 Uiso 1 1 calc R . . O8 O 0.42358(11) 0.32253(11) 0.54372(12) 0.0523(8) Uani 1 1 d . . . C17 C 0.32591(18) 0.23244(17) 0.51726(19) 0.0577(13) Uani 1 1 d . . . H17A H 0.3350 0.2481 0.4901 0.069 Uiso 1 1 calc R . . H17B H 0.2954 0.2472 0.5270 0.069 Uiso 1 1 calc R . . C18 C 0.31640(19) 0.18001(18) 0.5081(2) 0.0603(14) Uani 1 1 d . . . H18A H 0.3080 0.1637 0.5352 0.072 Uiso 1 1 calc R . . H18B H 0.2885 0.1773 0.4886 0.072 Uiso 1 1 calc R . . O9 O 0.35695(14) 0.15656(13) 0.48923(15) 0.0702(11) Uani 1 1 d . . . H9 H 0.3651 0.1332 0.5045 0.105 Uiso 1 1 calc R . . N4 N 0.36553(15) 0.40357(15) 0.44749(16) 0.0609(12) Uani 1 1 d . . . C19 C 0.31955(19) 0.4107(2) 0.4704(2) 0.0691(16) Uani 1 1 d . . . H19A H 0.2941 0.4191 0.4496 0.083 Uiso 1 1 calc R . . H19B H 0.3230 0.4377 0.4906 0.083 Uiso 1 1 calc R . . C20 C 0.30453(18) 0.3664(2) 0.4949(2) 0.0647(15) Uani 1 1 d . . . H20A H 0.2800 0.3746 0.5167 0.078 Uiso 1 1 calc R . . H20B H 0.2906 0.3424 0.4751 0.078 Uiso 1 1 calc R . . O10 O 0.34659(11) 0.34750(11) 0.51511(12) 0.0541(9) Uani 1 1 d . . . C21 C 0.3593(2) 0.3796(2) 0.4050(2) 0.0690(16) Uani 1 1 d . . . H21A H 0.3847 0.3903 0.3851 0.083 Uiso 1 1 calc R . . H21B H 0.3276 0.3881 0.3927 0.083 Uiso 1 1 calc R . . C22 C 0.3625(2) 0.3252(2) 0.4114(2) 0.0685(16) Uani 1 1 d . . . H22A H 0.3331 0.3134 0.4259 0.082 Uiso 1 1 calc R . . H22B H 0.3652 0.3090 0.3834 0.082 Uiso 1 1 calc R . . O11 O 0.40375(12) 0.31521(12) 0.43688(13) 0.0595(9) Uani 1 1 d . . . C23 C 0.3931(2) 0.44903(18) 0.4441(2) 0.0654(16) Uani 1 1 d . . . H23A H 0.3715 0.4752 0.4349 0.079 Uiso 1 1 calc R . . H23B H 0.4191 0.4457 0.4227 0.079 Uiso 1 1 calc R . . C24 C 0.4145(2) 0.46048(18) 0.4880(2) 0.0682(16) Uani 1 1 d . . . H24A H 0.4394 0.4856 0.4851 0.082 Uiso 1 1 calc R . . H24B H 0.3889 0.4726 0.5072 0.082 Uiso 1 1 calc R . . O12 O 0.43522(12) 0.41844(11) 0.50554(13) 0.0593(9) Uani 1 1 d . . . N5 N 0.52557(17) 0.36061(15) 0.39639(17) 0.0643(12) Uani 1 1 d . . . C25 C 0.5356(2) 0.38805(18) 0.4358(2) 0.0695(16) Uani 1 1 d . . . H25A H 0.5154 0.4172 0.4364 0.083 Uiso 1 1 calc R . . H25B H 0.5698 0.3981 0.4361 0.083 Uiso 1 1 calc R . . C26 C 0.52512(17) 0.35782(19) 0.4748(2) 0.0630(15) Uani 1 1 d . . . H26A H 0.5507 0.3335 0.4787 0.076 Uiso 1 1 calc R . . H26B H 0.5240 0.3781 0.5007 0.076 Uiso 1 1 calc R . . O13 O 0.47938(12) 0.33487(12) 0.46831(13) 0.0572(9) Uani 1 1 d . . . C27 C 0.5692(2) 0.33621(19) 0.3786(2) 0.0697(16) Uani 1 1 d . . . H27A H 0.5966 0.3588 0.3783 0.084 Uiso 1 1 calc R . . H27B H 0.5628 0.3263 0.3487 0.084 Uiso 1 1 calc R . . C28 C 0.58216(18) 0.29267(18) 0.40520(19) 0.0582(13) Uani 1 1 d . . . H28A H 0.6041 0.2715 0.3890 0.070 Uiso 1 1 calc R . . H28B H 0.5985 0.3026 0.4319 0.070 Uiso 1 1 calc R . . O14 O 0.53850(12) 0.26812(11) 0.41499(13) 0.0586(9) Uani 1 1 d . . . C29 C 0.4992(3) 0.3894(2) 0.3640(2) 0.0805(19) Uani 1 1 d . . . H29A H 0.5219 0.4103 0.3483 0.097 Uiso 1 1 calc R . . H29B H 0.4748 0.4097 0.3781 0.097 Uiso 1 1 calc R . . C30 C 0.4748(3) 0.3543(2) 0.3329(3) 0.090(2) Uani 1 1 d . . . H30A H 0.4490 0.3711 0.3170 0.108 Uiso 1 1 calc R . . H30B H 0.4987 0.3427 0.3119 0.108 Uiso 1 1 calc R . . O15 O 0.45498(17) 0.31526(15) 0.35495(14) 0.0776(12) Uani 1 1 d . . . O16 O 0.28324(11) 0.31240(12) 0.65246(13) 0.0554(9) Uani 1 1 d . . . O17 O 0.28666(11) 0.30897(11) 0.58059(13) 0.0528(9) Uani 1 1 d . . . C31 C 0.26512(18) 0.30529(17) 0.6161(2) 0.0579(14) Uani 1 1 d . . . C32 C 0.2122(2) 0.2917(3) 0.6131(2) 0.087(2) Uani 1 1 d . . . H32A H 0.2022 0.2762 0.6398 0.131 Uiso 1 1 calc R . . H32B H 0.2075 0.2696 0.5891 0.131 Uiso 1 1 calc R . . H32C H 0.1929 0.3205 0.6085 0.131 Uiso 1 1 calc R . . O18 O 0.47409(12) 0.47265(11) 0.72230(12) 0.0551(9) Uani 1 1 d . . . C33 C 0.5000 0.4934(2) 0.7500 0.0484(16) Uani 1 2 d S . . C34 C 0.5000 0.5466(2) 0.7500 0.063(2) Uani 1 2 d S . . H34A H 0.4818 0.5583 0.7748 0.095 Uiso 0.50 1 calc PR . . H34B H 0.4850 0.5583 0.7237 0.095 Uiso 0.50 1 calc PR . . H34C H 0.5332 0.5583 0.7516 0.095 Uiso 0.50 1 calc PR . . O19 O 0.35777(12) 0.27785(11) 0.72453(13) 0.0571(9) Uani 1 1 d . . . C35 C 0.3798(3) 0.2500 0.7500 0.0506(17) Uani 1 2 d S . . C36 C 0.4338(3) 0.2500 0.7500 0.079(3) Uani 1 2 d S . . H36A H 0.4455 0.2753 0.7310 0.118 Uiso 0.50 1 calc PR . . H36B H 0.4455 0.2190 0.7399 0.118 Uiso 0.50 1 calc PR . . H36C H 0.4455 0.2557 0.7791 0.118 Uiso 0.50 1 calc PR . . O41 O 0.39355(18) 0.0908(2) 0.5479(2) 0.118(2) Uani 1 1 d . . . N51 N 0.3999(5) 0.4652(4) 0.3255(4) 0.155(4) Uani 1 1 d U . . C51 C 0.3616(6) 0.4680(6) 0.3195(5) 0.167(6) Uani 1 1 d U . . C52 C 0.3158(6) 0.4719(6) 0.3128(6) 0.235(9) Uani 1 1 d U . . H52A H 0.3047 0.5032 0.3229 0.352 Uiso 1 1 calc R . . H52B H 0.2988 0.4466 0.3284 0.352 Uiso 1 1 calc R . . H52C H 0.3093 0.4689 0.2822 0.352 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.02616(11) 0.02893(11) 0.08702(18) 0.00025(11) -0.00321(11) 0.00406(8) Fe1 0.0295(3) 0.0281(3) 0.0881(5) -0.0016(3) -0.0044(3) 0.0015(2) Fe2 0.0277(3) 0.0325(3) 0.0876(5) 0.0043(3) -0.0037(3) 0.0022(3) Fe3 0.0320(3) 0.0352(3) 0.0917(6) 0.0076(3) -0.0034(3) -0.0011(3) Fe4 0.0386(4) 0.0390(4) 0.0908(6) -0.0004(3) -0.0002(4) -0.0022(3) N1 0.032(2) 0.0290(18) 0.090(3) 0.0013(18) -0.0081(19) -0.0016(15) C1 0.033(2) 0.039(2) 0.089(4) 0.000(2) -0.001(2) -0.0031(19) C2 0.029(2) 0.044(3) 0.090(4) -0.001(2) 0.001(2) -0.0036(19) O1 0.0320(17) 0.0383(16) 0.086(2) 0.0006(16) -0.0003(16) 0.0006(13) C3 0.037(3) 0.031(2) 0.086(4) -0.001(2) 0.000(2) -0.0025(19) C4 0.027(2) 0.032(2) 0.088(4) -0.004(2) 0.003(2) 0.0014(17) O2 0.0221(14) 0.0312(14) 0.089(2) 0.0001(15) -0.0004(14) 0.0029(12) C5 0.047(3) 0.032(2) 0.092(4) 0.001(2) -0.006(3) 0.002(2) C6 0.055(3) 0.040(2) 0.082(4) 0.005(2) -0.004(3) -0.007(2) O3 0.0374(18) 0.0492(19) 0.091(3) -0.0016(18) 0.0016(18) -0.0073(15) N2 0.038(2) 0.042(2) 0.096(4) -0.001(2) -0.002(2) 0.0044(18) C7 0.048(3) 0.039(3) 0.108(5) -0.008(3) -0.007(3) 0.014(2) C8 0.039(3) 0.041(3) 0.107(4) -0.014(3) -0.009(3) 0.016(2) O4 0.0345(17) 0.0264(14) 0.105(3) -0.0111(16) -0.0098(17) 0.0077(12) C9 0.038(3) 0.036(2) 0.112(5) 0.001(3) -0.006(3) 0.011(2) C10 0.042(3) 0.028(2) 0.106(4) 0.009(2) -0.003(3) 0.008(2) O5 0.0320(16) 0.0296(14) 0.097(3) 0.0059(15) -0.0052(17) 0.0085(13) C11 0.042(3) 0.052(3) 0.114(5) 0.004(3) 0.001(3) 0.012(2) C12 0.045(3) 0.062(3) 0.115(5) 0.000(3) 0.007(3) 0.019(3) O6 0.046(2) 0.056(2) 0.099(3) 0.004(2) 0.011(2) 0.0188(17) N3 0.033(2) 0.0338(18) 0.084(3) -0.0009(18) -0.0039(19) 0.0019(15) C13 0.041(3) 0.033(2) 0.083(4) 0.001(2) -0.005(2) -0.002(2) C14 0.039(3) 0.027(2) 0.091(4) 0.004(2) -0.008(2) 0.0039(18) O7 0.0303(16) 0.0255(13) 0.083(2) -0.0020(14) -0.0032(15) 0.0034(12) C15 0.036(3) 0.036(2) 0.090(4) -0.003(2) 0.000(2) 0.0038(19) C16 0.029(2) 0.032(2) 0.097(4) 0.005(2) 0.001(2) 0.0056(18) O8 0.0283(16) 0.0352(16) 0.093(3) 0.0051(16) -0.0039(16) 0.0048(13) C17 0.036(3) 0.047(3) 0.090(4) -0.003(3) -0.009(3) -0.002(2) C18 0.042(3) 0.050(3) 0.089(4) -0.007(3) -0.002(3) -0.003(2) O9 0.054(2) 0.047(2) 0.109(3) -0.003(2) 0.006(2) -0.0037(17) N4 0.040(2) 0.042(2) 0.101(4) 0.015(2) -0.004(2) 0.0011(18) C19 0.041(3) 0.053(3) 0.114(5) 0.023(3) -0.005(3) 0.009(2) C20 0.035(3) 0.058(3) 0.101(4) 0.022(3) -0.011(3) 0.004(2) O10 0.0240(15) 0.0450(18) 0.093(3) 0.0129(17) -0.0025(15) 0.0027(13) C21 0.059(4) 0.053(3) 0.095(4) 0.008(3) -0.016(3) -0.003(3) C22 0.047(3) 0.050(3) 0.108(5) 0.006(3) -0.020(3) -0.001(2) O11 0.0372(18) 0.0451(18) 0.096(3) 0.0090(18) -0.0091(18) 0.0007(15) C23 0.053(3) 0.038(2) 0.106(5) 0.017(3) -0.007(3) -0.008(2) C24 0.055(3) 0.041(3) 0.109(5) 0.018(3) 0.003(3) 0.005(2) O12 0.0406(19) 0.0362(16) 0.101(3) 0.0093(17) -0.0076(18) -0.0016(14) N5 0.052(3) 0.044(2) 0.096(4) 0.012(2) 0.004(2) -0.002(2) C25 0.054(3) 0.040(3) 0.114(5) 0.006(3) 0.002(3) -0.005(2) C26 0.029(2) 0.057(3) 0.103(4) -0.008(3) 0.002(3) -0.007(2) O13 0.0345(18) 0.0459(18) 0.091(3) -0.0022(17) 0.0003(17) -0.0049(14) C27 0.054(3) 0.048(3) 0.107(5) 0.007(3) 0.012(3) -0.004(2) C28 0.040(3) 0.047(3) 0.087(4) 0.000(3) 0.007(3) -0.010(2) O14 0.0394(19) 0.0404(17) 0.096(3) 0.0013(17) 0.0051(18) -0.0044(15) C29 0.078(4) 0.059(3) 0.105(5) 0.023(3) -0.017(4) -0.008(3) C30 0.090(5) 0.073(4) 0.106(5) 0.028(4) -0.007(4) 0.000(4) O15 0.076(3) 0.062(2) 0.095(3) 0.008(2) -0.002(2) -0.012(2) O16 0.0249(16) 0.0488(19) 0.093(3) 0.0027(18) -0.0069(17) -0.0014(14) O17 0.0264(16) 0.0399(16) 0.092(3) 0.0045(17) -0.0033(17) 0.0027(13) C31 0.031(3) 0.042(3) 0.102(5) 0.010(3) -0.002(3) -0.001(2) C32 0.033(3) 0.121(6) 0.109(5) -0.001(4) -0.002(3) -0.023(3) O18 0.048(2) 0.0296(15) 0.087(3) -0.0022(15) -0.0111(18) 0.0005(14) C33 0.039(4) 0.028(3) 0.078(5) 0.000 0.007(3) 0.000 C34 0.072(5) 0.028(3) 0.089(6) 0.000 -0.010(4) 0.000 O19 0.0383(18) 0.0392(17) 0.094(3) 0.0128(17) -0.0010(18) 0.0022(15) C35 0.041(4) 0.029(3) 0.082(5) -0.005(3) 0.000 0.000 C36 0.033(4) 0.061(5) 0.143(8) 0.037(5) 0.000 0.000 O41 0.064(3) 0.104(4) 0.187(6) 0.043(4) 0.016(3) 0.020(3) N51 0.188(10) 0.094(6) 0.182(10) 0.034(6) -0.001(9) -0.025(8) C51 0.170(11) 0.180(13) 0.151(10) 0.078(9) -0.048(12) -0.063(13) C52 0.184(11) 0.208(15) 0.31(2) 0.094(14) -0.106(15) -0.115(12) _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 O4 2.345(3) . ? Gd1 O5 2.350(4) . ? Gd1 O19 2.351(3) . ? Gd1 O7 2.353(3) . ? Gd1 O2 2.361(3) . ? Gd1 O16 2.425(3) . ? Gd1 O6 2.467(4) . ? Gd1 N2 2.650(4) . ? Fe1 O4 1.944(3) . ? Fe1 O2 1.954(3) . ? Fe1 O1 1.976(4) 3_656 ? Fe1 O1 2.037(3) . ? Fe1 O18 2.050(3) . ? Fe1 N1 2.253(5) . ? Fe2 O5 1.955(3) . ? Fe2 O10 1.966(4) . ? Fe2 O7 1.977(3) . ? Fe2 O8 2.008(3) . ? Fe2 O17 2.043(3) . ? Fe2 N3 2.257(4) . ? Fe3 O12 1.904(3) . ? Fe3 O8 1.997(4) . ? Fe3 O11 2.006(4) . ? Fe3 O13 2.025(3) . ? Fe3 O10 2.060(3) . ? Fe3 N4 2.268(4) . ? Fe4 O15 1.897(4) . ? Fe4 O14 1.978(3) 6 ? Fe4 O13 1.991(4) . ? Fe4 O14 2.066(3) . ? Fe4 O11 2.090(4) . ? Fe4 N5 2.272(4) . ? N1 C3 1.489(6) . ? N1 C5 1.490(6) . ? N1 C1 1.496(6) . ? C1 C2 1.513(7) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 O1 1.424(6) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? O1 Fe1 1.976(4) 3_656 ? C3 C4 1.520(7) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 O2 1.430(6) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.522(8) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 O3 1.409(6) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? O3 H3 0.8400 . ? N2 C11 1.468(7) . ? N2 C9 1.487(7) . ? N2 C7 1.503(7) . ? C7 C8 1.502(8) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 O4 1.419(5) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.516(8) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 O5 1.428(5) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.485(9) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 O6 1.446(6) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? O6 H6 0.95(3) . ? N3 C13 1.481(7) . ? N3 C17 1.495(6) . ? N3 C15 1.501(6) . ? C13 C14 1.515(7) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 O7 1.416(5) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.531(6) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 O8 1.423(5) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.518(7) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 O9 1.431(6) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? O9 H9 0.8400 . ? N4 C19 1.479(7) . ? N4 C23 1.489(6) . ? N4 C21 1.497(8) . ? C19 C20 1.517(7) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 O10 1.430(6) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.538(8) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 O11 1.424(6) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.529(9) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 O12 1.421(6) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? N5 C25 1.479(8) . ? N5 C29 1.486(8) . ? N5 C27 1.500(7) . ? C25 C26 1.513(8) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 O13 1.439(6) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.519(8) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 O14 1.428(6) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? O14 Fe4 1.978(3) 6 ? C29 C30 1.540(10) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 O15 1.404(8) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? O16 C31 1.260(7) . ? O17 C31 1.265(7) . ? C31 C32 1.521(7) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? O18 C33 1.268(4) . ? C33 O18 1.268(4) 3_656 ? C33 C34 1.489(8) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? O19 C35 1.272(5) . ? C35 O19 1.272(5) 8_456 ? C35 C36 1.499(10) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? N51 C51 1.085(16) . ? C51 C52 1.293(19) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Gd1 O5 91.97(12) . . ? O4 Gd1 O19 114.66(13) . . ? O5 Gd1 O19 150.41(12) . . ? O4 Gd1 O7 135.36(12) . . ? O5 Gd1 O7 66.17(11) . . ? O19 Gd1 O7 85.15(12) . . ? O4 Gd1 O2 64.56(10) . . ? O5 Gd1 O2 95.04(11) . . ? O19 Gd1 O2 85.78(11) . . ? O7 Gd1 O2 78.54(11) . . ? O4 Gd1 O16 142.59(11) . . ? O5 Gd1 O16 81.28(12) . . ? O19 Gd1 O16 84.43(12) . . ? O7 Gd1 O16 74.87(11) . . ? O2 Gd1 O16 152.31(11) . . ? O4 Gd1 O6 80.49(13) . . ? O5 Gd1 O6 130.86(12) . . ? O19 Gd1 O6 69.53(13) . . ? O7 Gd1 O6 143.43(12) . . ? O2 Gd1 O6 123.37(13) . . ? O16 Gd1 O6 76.73(14) . . ? O4 Gd1 N2 67.45(12) . . ? O5 Gd1 N2 68.10(13) . . ? O19 Gd1 N2 132.61(13) . . ? O7 Gd1 N2 128.47(13) . . ? O2 Gd1 N2 128.21(12) . . ? O16 Gd1 N2 75.98(12) . . ? O6 Gd1 N2 64.17(14) . . ? O4 Fe1 O2 80.30(12) . . ? O4 Fe1 O1 100.05(15) . 3_656 ? O2 Fe1 O1 105.02(14) . 3_656 ? O4 Fe1 O1 174.61(16) . . ? O2 Fe1 O1 100.05(13) . . ? O1 Fe1 O1 74.63(16) 3_656 . ? O4 Fe1 O18 89.46(13) . . ? O2 Fe1 O18 160.03(14) . . ? O1 Fe1 O18 93.57(14) 3_656 . ? O1 Fe1 O18 91.75(13) . . ? O4 Fe1 N1 107.24(16) . . ? O2 Fe1 N1 79.70(14) . . ? O1 Fe1 N1 152.70(14) 3_656 . ? O1 Fe1 N1 78.06(14) . . ? O18 Fe1 N1 87.14(14) . . ? O5 Fe2 O10 102.79(15) . . ? O5 Fe2 O7 81.53(13) . . ? O10 Fe2 O7 171.21(13) . . ? O5 Fe2 O8 101.77(14) . . ? O10 Fe2 O8 75.10(14) . . ? O7 Fe2 O8 96.61(14) . . ? O5 Fe2 O17 93.95(14) . . ? O10 Fe2 O17 90.64(14) . . ? O7 Fe2 O17 96.73(14) . . ? O8 Fe2 O17 160.69(15) . . ? O5 Fe2 N3 160.96(16) . . ? O10 Fe2 N3 96.14(15) . . ? O7 Fe2 N3 79.43(14) . . ? O8 Fe2 N3 80.99(13) . . ? O17 Fe2 N3 87.82(13) . . ? O12 Fe3 O8 98.48(15) . . ? O12 Fe3 O11 142.71(16) . . ? O8 Fe3 O11 115.87(14) . . ? O12 Fe3 O13 94.52(15) . . ? O8 Fe3 O13 89.96(14) . . ? O11 Fe3 O13 72.55(14) . . ? O12 Fe3 O10 106.49(15) . . ? O8 Fe3 O10 73.28(13) . . ? O11 Fe3 O10 97.35(15) . . ? O13 Fe3 O10 154.62(13) . . ? O12 Fe3 N4 79.66(15) . . ? O8 Fe3 N4 147.86(16) . . ? O11 Fe3 N4 78.52(16) . . ? O13 Fe3 N4 122.17(17) . . ? O10 Fe3 N4 76.53(15) . . ? O15 Fe4 O14 101.47(17) . 6 ? O15 Fe4 O13 139.69(17) . . ? O14 Fe4 O13 116.06(16) 6 . ? O15 Fe4 O14 110.83(18) . . ? O14 Fe4 O14 71.67(15) 6 . ? O13 Fe4 O14 95.16(15) . . ? O15 Fe4 O11 94.50(18) . . ? O14 Fe4 O11 91.42(14) 6 . ? O13 Fe4 O11 71.46(14) . . ? O14 Fe4 O11 151.61(15) . . ? O15 Fe4 N5 79.16(18) . . ? O14 Fe4 N5 145.68(16) 6 . ? O13 Fe4 N5 77.88(17) . . ? O14 Fe4 N5 76.09(15) . . ? O11 Fe4 N5 122.86(15) . . ? C3 N1 C5 112.8(4) . . ? C3 N1 C1 113.2(4) . . ? C5 N1 C1 111.6(4) . . ? C3 N1 Fe1 106.0(3) . . ? C5 N1 Fe1 109.3(3) . . ? C1 N1 Fe1 103.3(3) . . ? N1 C1 C2 110.6(4) . . ? N1 C1 H1A 109.5 . . ? C2 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 108.1 . . ? O1 C2 C1 108.6(4) . . ? O1 C2 H2A 110.0 . . ? C1 C2 H2A 110.0 . . ? O1 C2 H2B 110.0 . . ? C1 C2 H2B 110.0 . . ? H2A C2 H2B 108.4 . . ? C2 O1 Fe1 131.0(3) . 3_656 ? C2 O1 Fe1 119.5(3) . . ? Fe1 O1 Fe1 100.37(15) 3_656 . ? N1 C3 C4 110.8(4) . . ? N1 C3 H3A 109.5 . . ? C4 C3 H3A 109.5 . . ? N1 C3 H3B 109.5 . . ? C4 C3 H3B 109.5 . . ? H3A C3 H3B 108.1 . . ? O2 C4 C3 108.1(4) . . ? O2 C4 H4A 110.1 . . ? C3 C4 H4A 110.1 . . ? O2 C4 H4B 110.1 . . ? C3 C4 H4B 110.1 . . ? H4A C4 H4B 108.4 . . ? C4 O2 Fe1 110.1(2) . . ? C4 O2 Gd1 132.6(3) . . ? Fe1 O2 Gd1 107.01(12) . . ? N1 C5 C6 116.5(4) . . ? N1 C5 H5A 108.2 . . ? C6 C5 H5A 108.2 . . ? N1 C5 H5B 108.2 . . ? C6 C5 H5B 108.2 . . ? H5A C5 H5B 107.3 . . ? O3 C6 C5 114.7(4) . . ? O3 C6 H6A 108.6 . . ? C5 C6 H6A 108.6 . . ? O3 C6 H6B 108.6 . . ? C5 C6 H6B 108.6 . . ? H6A C6 H6B 107.6 . . ? C6 O3 H3 109.5 . . ? C11 N2 C9 110.5(4) . . ? C11 N2 C7 111.8(4) . . ? C9 N2 C7 109.5(4) . . ? C11 N2 Gd1 108.3(3) . . ? C9 N2 Gd1 107.0(3) . . ? C7 N2 Gd1 109.6(3) . . ? C8 C7 N2 113.3(4) . . ? C8 C7 H7A 108.9 . . ? N2 C7 H7A 108.9 . . ? C8 C7 H7B 108.9 . . ? N2 C7 H7B 108.9 . . ? H7A C7 H7B 107.7 . . ? O4 C8 C7 108.9(5) . . ? O4 C8 H8A 109.9 . . ? C7 C8 H8A 109.9 . . ? O4 C8 H8B 109.9 . . ? C7 C8 H8B 109.9 . . ? H8A C8 H8B 108.3 . . ? C8 O4 Fe1 130.7(3) . . ? C8 O4 Gd1 120.7(3) . . ? Fe1 O4 Gd1 107.97(12) . . ? N2 C9 C10 111.6(4) . . ? N2 C9 H9A 109.3 . . ? C10 C9 H9A 109.3 . . ? N2 C9 H9B 109.3 . . ? C10 C9 H9B 109.3 . . ? H9A C9 H9B 108.0 . . ? O5 C10 C9 109.8(4) . . ? O5 C10 H10A 109.7 . . ? C9 C10 H10A 109.7 . . ? O5 C10 H10B 109.7 . . ? C9 C10 H10B 109.7 . . ? H10A C10 H10B 108.2 . . ? C10 O5 Fe2 123.7(3) . . ? C10 O5 Gd1 122.5(3) . . ? Fe2 O5 Gd1 103.77(13) . . ? N2 C11 C12 112.7(5) . . ? N2 C11 H11A 109.0 . . ? C12 C11 H11A 109.0 . . ? N2 C11 H11B 109.0 . . ? C12 C11 H11B 109.0 . . ? H11A C11 H11B 107.8 . . ? O6 C12 C11 108.2(5) . . ? O6 C12 H12A 110.1 . . ? C11 C12 H12A 110.1 . . ? O6 C12 H12B 110.1 . . ? C11 C12 H12B 110.1 . . ? H12A C12 H12B 108.4 . . ? C12 O6 Gd1 124.8(4) . . ? C12 O6 H6 105(4) . . ? Gd1 O6 H6 127(4) . . ? C13 N3 C17 111.5(4) . . ? C13 N3 C15 113.5(4) . . ? C17 N3 C15 111.7(4) . . ? C13 N3 Fe2 102.9(3) . . ? C17 N3 Fe2 110.9(3) . . ? C15 N3 Fe2 105.9(3) . . ? N3 C13 C14 110.6(4) . . ? N3 C13 H13A 109.5 . . ? C14 C13 H13A 109.5 . . ? N3 C13 H13B 109.5 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 108.1 . . ? O7 C14 C13 110.3(4) . . ? O7 C14 H14A 109.6 . . ? C13 C14 H14A 109.6 . . ? O7 C14 H14B 109.6 . . ? C13 C14 H14B 109.6 . . ? H14A C14 H14B 108.1 . . ? C14 O7 Fe2 119.2(3) . . ? C14 O7 Gd1 131.6(3) . . ? Fe2 O7 Gd1 102.95(11) . . ? N3 C15 C16 112.1(4) . . ? N3 C15 H15A 109.2 . . ? C16 C15 H15A 109.2 . . ? N3 C15 H15B 109.2 . . ? C16 C15 H15B 109.2 . . ? H15A C15 H15B 107.9 . . ? O8 C16 C15 110.0(4) . . ? O8 C16 H16A 109.7 . . ? C15 C16 H16A 109.7 . . ? O8 C16 H16B 109.7 . . ? C15 C16 H16B 109.7 . . ? H16A C16 H16B 108.2 . . ? C16 O8 Fe3 122.2(3) . . ? C16 O8 Fe2 111.2(3) . . ? Fe3 O8 Fe2 105.94(14) . . ? N3 C17 C18 116.6(4) . . ? N3 C17 H17A 108.1 . . ? C18 C17 H17A 108.1 . . ? N3 C17 H17B 108.1 . . ? C18 C17 H17B 108.1 . . ? H17A C17 H17B 107.3 . . ? O9 C18 C17 112.6(4) . . ? O9 C18 H18A 109.1 . . ? C17 C18 H18A 109.1 . . ? O9 C18 H18B 109.1 . . ? C17 C18 H18B 109.1 . . ? H18A C18 H18B 107.8 . . ? C18 O9 H9 109.5 . . ? C19 N4 C23 111.3(4) . . ? C19 N4 C21 112.9(5) . . ? C23 N4 C21 112.3(5) . . ? C19 N4 Fe3 108.4(3) . . ? C23 N4 Fe3 103.3(3) . . ? C21 N4 Fe3 108.0(3) . . ? N4 C19 C20 111.9(4) . . ? N4 C19 H19A 109.2 . . ? C20 C19 H19A 109.2 . . ? N4 C19 H19B 109.2 . . ? C20 C19 H19B 109.2 . . ? H19A C19 H19B 107.9 . . ? O10 C20 C19 107.5(4) . . ? O10 C20 H20A 110.2 . . ? C19 C20 H20A 110.2 . . ? O10 C20 H20B 110.2 . . ? C19 C20 H20B 110.2 . . ? H20A C20 H20B 108.5 . . ? C20 O10 Fe2 133.2(3) . . ? C20 O10 Fe3 121.0(3) . . ? Fe2 O10 Fe3 105.14(14) . . ? N4 C21 C22 108.8(5) . . ? N4 C21 H21A 109.9 . . ? C22 C21 H21A 109.9 . . ? N4 C21 H21B 109.9 . . ? C22 C21 H21B 109.9 . . ? H21A C21 H21B 108.3 . . ? O11 C22 C21 108.2(4) . . ? O11 C22 H22A 110.1 . . ? C21 C22 H22A 110.1 . . ? O11 C22 H22B 110.1 . . ? C21 C22 H22B 110.1 . . ? H22A C22 H22B 108.4 . . ? C22 O11 Fe3 116.5(3) . . ? C22 O11 Fe4 124.4(4) . . ? Fe3 O11 Fe4 105.91(16) . . ? N4 C23 C24 108.4(5) . . ? N4 C23 H23A 110.0 . . ? C24 C23 H23A 110.0 . . ? N4 C23 H23B 110.0 . . ? C24 C23 H23B 110.0 . . ? H23A C23 H23B 108.4 . . ? O12 C24 C23 109.4(5) . . ? O12 C24 H24A 109.8 . . ? C23 C24 H24A 109.8 . . ? O12 C24 H24B 109.8 . . ? C23 C24 H24B 109.8 . . ? H24A C24 H24B 108.3 . . ? C24 O12 Fe3 120.9(3) . . ? C25 N5 C29 112.3(5) . . ? C25 N5 C27 113.2(5) . . ? C29 N5 C27 113.1(5) . . ? C25 N5 Fe4 108.5(3) . . ? C29 N5 Fe4 102.8(4) . . ? C27 N5 Fe4 106.1(3) . . ? N5 C25 C26 110.2(4) . . ? N5 C25 H25A 109.6 . . ? C26 C25 H25A 109.6 . . ? N5 C25 H25B 109.6 . . ? C26 C25 H25B 109.6 . . ? H25A C25 H25B 108.1 . . ? O13 C26 C25 107.8(5) . . ? O13 C26 H26A 110.1 . . ? C25 C26 H26A 110.1 . . ? O13 C26 H26B 110.1 . . ? C25 C26 H26B 110.1 . . ? H26A C26 H26B 108.5 . . ? C26 O13 Fe4 114.8(3) . . ? C26 O13 Fe3 128.1(3) . . ? Fe4 O13 Fe3 108.99(16) . . ? N5 C27 C28 110.7(5) . . ? N5 C27 H27A 109.5 . . ? C28 C27 H27A 109.5 . . ? N5 C27 H27B 109.5 . . ? C28 C27 H27B 109.5 . . ? H27A C27 H27B 108.1 . . ? O14 C28 C27 107.6(4) . . ? O14 C28 H28A 110.2 . . ? C27 C28 H28A 110.2 . . ? O14 C28 H28B 110.2 . . ? C27 C28 H28B 110.2 . . ? H28A C28 H28B 108.5 . . ? C28 O14 Fe4 126.6(3) . 6 ? C28 O14 Fe4 121.9(3) . . ? Fe4 O14 Fe4 108.13(15) 6 . ? N5 C29 C30 107.6(5) . . ? N5 C29 H29A 110.2 . . ? C30 C29 H29A 110.2 . . ? N5 C29 H29B 110.2 . . ? C30 C29 H29B 110.2 . . ? H29A C29 H29B 108.5 . . ? O15 C30 C29 111.0(6) . . ? O15 C30 H30A 109.4 . . ? C29 C30 H30A 109.4 . . ? O15 C30 H30B 109.4 . . ? C29 C30 H30B 109.4 . . ? H30A C30 H30B 108.0 . . ? C30 O15 Fe4 121.4(4) . . ? C31 O16 Gd1 134.9(3) . . ? C31 O17 Fe2 126.3(3) . . ? O16 C31 O17 126.2(5) . . ? O16 C31 C32 118.7(6) . . ? O17 C31 C32 115.1(6) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C33 O18 Fe1 129.0(3) . . ? O18 C33 O18 125.4(6) 3_656 . ? O18 C33 C34 117.3(3) 3_656 . ? O18 C33 C34 117.3(3) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C35 O19 Gd1 149.4(3) . . ? O19 C35 O19 122.3(6) 8_456 . ? O19 C35 C36 118.8(3) 8_456 . ? O19 C35 C36 118.8(3) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N51 C51 C52 179(3) . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3 O12 0.84 1.82 2.657(5) 178.5 . _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.526 _refine_diff_density_min -2.281 _refine_diff_density_rms 0.127 ############################################################################### data_amac16dy _database_code_depnum_ccdc_archive 'CCDC 780084' #TrackingRef '- amer_fe16ln4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C136 H276 Dy4 Fe16 N20 O76, 4(N O3), 10(C2 H3 N), 16(H2 O) ' _chemical_formula_sum 'C156 H338 Dy4 Fe16 N34 O104' _chemical_formula_weight 5898.20 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' Fe Fe 0.3463 0.8444 '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 orthorhombic _symmetry_space_group_name_H-M 'C c c a' _symmetry_space_group_name_Hall '-C 2b 2bc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' '-x, y, -z+1/2' 'x+1/2, -y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1, -y+1/2, z' '-x+1/2, y+1/2, -z+1/2' 'x+1, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' 'x, -y, z-1/2' '-x-1/2, y, z-1/2' '-x+1/2, -y+1/2, -z' 'x, y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' '-x, y+1/2, z-1/2' _cell_length_a 27.7714(11) _cell_length_b 28.0818(11) _cell_length_c 30.6492(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 23902.4(17) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 14042 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 28.03 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.639 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 12096 _exptl_absorpt_coefficient_mu 2.267 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5128 _exptl_absorpt_correction_T_max 0.6010 _exptl_absorpt_process_details 'SADABS 2.10 (Bruker AXS Inc., 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART Apex' _diffrn_measurement_method 'CCD area detector' _diffrn_detector_area_resol_mean 8.333 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 70812 _diffrn_reflns_av_R_equivalents 0.0332 _diffrn_reflns_av_sigmaI/netI 0.0240 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 28.13 _reflns_number_total 13682 _reflns_number_gt 11770 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT 5.6 (Bruker AXS Inc., 2005)' _computing_cell_refinement 'SMART-NT 5.6 (Bruker AXS Inc., 2005)' _computing_data_reduction 'SAINT+ 6.45 (Bruker AXS Inc., 2003)' _computing_structure_solution 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_structure_refinement 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_molecular_graphics 'Diamond 2.1 (Crystal Impact, 1998)' _computing_publication_material 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _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. one lattice MeCN per asymmetric unit (i.e. 4 per Fe16Dy4) was ordered and could be refined anisotropically. However, the nitrate counterion, the lattice waters and the remaining lattice MeCN were disordered, and were refined using two sets of half-occupancy atoms with geometrical restraints. ; _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^)+(0.1356P)^2^+16.1386P] 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 13682 _refine_ls_number_parameters 704 _refine_ls_number_restraints 41 _refine_ls_R_factor_all 0.0598 _refine_ls_R_factor_gt 0.0508 _refine_ls_wR_factor_ref 0.1858 _refine_ls_wR_factor_gt 0.1713 _refine_ls_goodness_of_fit_ref 1.115 _refine_ls_restrained_S_all 1.115 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 0.359110(7) 0.344092(7) 0.677854(6) 0.02258(10) Uani 1 1 d . . . Fe1 Fe 0.46295(2) 0.39994(2) 0.71268(2) 0.02309(15) Uani 1 1 d . . . Fe2 Fe 0.35844(2) 0.31927(2) 0.57027(2) 0.02371(15) Uani 1 1 d . . . Fe3 Fe 0.41336(2) 0.35582(2) 0.48489(2) 0.02856(16) Uani 1 1 d . . . Fe4 Fe 0.47250(3) 0.30141(3) 0.40755(2) 0.03348(17) Uani 1 1 d . . . N1 N 0.49639(13) 0.40969(12) 0.64661(12) 0.0245(7) Uani 1 1 d . . . C1 C 0.54693(16) 0.42343(16) 0.65607(14) 0.0294(9) Uani 1 1 d . . . H1A H 0.5480 0.4568 0.6664 0.035 Uiso 1 1 calc R . . H1B H 0.5664 0.4213 0.6291 0.035 Uiso 1 1 calc R . . C2 C 0.56807(17) 0.39075(17) 0.69069(15) 0.0310(9) Uani 1 1 d . . . H2A H 0.5762 0.3595 0.6777 0.037 Uiso 1 1 calc R . . H2B H 0.5979 0.4049 0.7028 0.037 Uiso 1 1 calc R . . O1 O 0.53328(11) 0.38459(11) 0.72469(10) 0.0266(6) Uani 1 1 d . . . C3 C 0.49255(17) 0.36232(14) 0.62435(14) 0.0273(8) Uani 1 1 d . . . H3A H 0.5235 0.3545 0.6101 0.033 Uiso 1 1 calc R . . H3B H 0.4674 0.3638 0.6015 0.033 Uiso 1 1 calc R . . C4 C 0.47996(15) 0.32357(14) 0.65739(14) 0.0241(8) Uani 1 1 d . . . H4A H 0.4691 0.2945 0.6420 0.029 Uiso 1 1 calc R . . H4B H 0.5087 0.3154 0.6750 0.029 Uiso 1 1 calc R . . O2 O 0.44280(12) 0.34065(9) 0.68493(10) 0.0228(6) Uani 1 1 d . . . C5 C 0.46986(17) 0.44828(15) 0.62270(15) 0.0284(9) Uani 1 1 d . . . H5A H 0.4619 0.4738 0.6438 0.034 Uiso 1 1 calc R . . H5B H 0.4391 0.4349 0.6119 0.034 Uiso 1 1 calc R . . C6 C 0.4961(2) 0.47082(16) 0.58426(15) 0.0351(10) Uani 1 1 d . . . H6A H 0.4749 0.4951 0.5709 0.042 Uiso 1 1 calc R . . H6B H 0.5251 0.4874 0.5953 0.042 Uiso 1 1 calc R . . O3 O 0.51027(12) 0.43791(12) 0.55149(11) 0.0340(7) Uani 1 1 d . . . H3 H 0.4864 0.4312 0.5358 0.051 Uiso 1 1 calc R . . N2 N 0.30325(15) 0.42025(15) 0.67037(14) 0.0337(9) Uani 1 1 d . . . C7 C 0.32903(19) 0.46294(17) 0.68753(18) 0.0382(11) Uani 1 1 d . . . H7A H 0.3052 0.4853 0.7000 0.046 Uiso 1 1 calc R . . H7B H 0.3454 0.4793 0.6631 0.046 Uiso 1 1 calc R . . C8 C 0.36605(18) 0.45041(17) 0.72234(18) 0.0366(11) Uani 1 1 d . . . H8A H 0.3869 0.4782 0.7282 0.044 Uiso 1 1 calc R . . H8B H 0.3496 0.4415 0.7498 0.044 Uiso 1 1 calc R . . O4 O 0.39426(12) 0.41174(11) 0.70724(11) 0.0301(7) Uani 1 1 d . . . C9 C 0.29308(18) 0.42685(17) 0.62300(16) 0.0344(10) Uani 1 1 d . . . H9A H 0.2803 0.4593 0.6179 0.041 Uiso 1 1 calc R . . H9B H 0.2684 0.4036 0.6135 0.041 Uiso 1 1 calc R . . C10 C 0.33907(18) 0.41977(16) 0.59630(16) 0.0324(10) Uani 1 1 d . . . H10A H 0.3312 0.4200 0.5648 0.039 Uiso 1 1 calc R . . H10B H 0.3617 0.4462 0.6021 0.039 Uiso 1 1 calc R . . O5 O 0.36103(10) 0.37558(11) 0.60765(11) 0.0273(7) Uani 1 1 d . . . C11 C 0.25769(19) 0.4109(2) 0.69456(19) 0.0417(12) Uani 1 1 d . . . H11A H 0.2390 0.3861 0.6790 0.050 Uiso 1 1 calc R . . H11B H 0.2381 0.4403 0.6952 0.050 Uiso 1 1 calc R . . C12 C 0.2670(2) 0.3949(2) 0.74016(19) 0.0452(13) Uani 1 1 d . . . H12A H 0.2777 0.4222 0.7582 0.054 Uiso 1 1 calc R . . H12B H 0.2372 0.3817 0.7531 0.054 Uiso 1 1 calc R . . O6 O 0.30399(14) 0.35879(14) 0.73914(12) 0.0399(8) Uani 1 1 d D . . H6 H 0.300(2) 0.347(2) 0.7647(14) 0.048 Uiso 1 1 d D . . N3 N 0.36354(14) 0.24313(14) 0.54804(12) 0.0276(8) Uani 1 1 d . . . C13 C 0.35584(16) 0.21559(16) 0.58923(15) 0.0268(9) Uani 1 1 d . . . H13A H 0.3665 0.1823 0.5851 0.032 Uiso 1 1 calc R . . H13B H 0.3211 0.2152 0.5966 0.032 Uiso 1 1 calc R . . C14 C 0.38442(16) 0.23843(14) 0.62663(14) 0.0257(8) Uani 1 1 d . . . H14A H 0.3722 0.2266 0.6550 0.031 Uiso 1 1 calc R . . H14B H 0.4188 0.2296 0.6242 0.031 Uiso 1 1 calc R . . O7 O 0.37954(11) 0.28836(10) 0.62474(9) 0.0247(6) Uani 1 1 d . . . C15 C 0.41246(16) 0.23722(16) 0.52953(14) 0.0286(9) Uani 1 1 d . . . H15A H 0.4104 0.2372 0.4973 0.034 Uiso 1 1 calc R . . H15B H 0.4257 0.2061 0.5388 0.034 Uiso 1 1 calc R . . C16 C 0.44682(16) 0.27711(15) 0.54420(14) 0.0272(8) Uani 1 1 d . . . H16A H 0.4573 0.2713 0.5746 0.033 Uiso 1 1 calc R . . H16B H 0.4757 0.2773 0.5253 0.033 Uiso 1 1 calc R . . O8 O 0.42334(11) 0.32137(11) 0.54156(10) 0.0262(6) Uani 1 1 d . . . C17 C 0.32532(18) 0.23172(16) 0.51596(15) 0.0322(10) Uani 1 1 d . . . H17A H 0.3332 0.2482 0.4883 0.039 Uiso 1 1 calc R . . H17B H 0.2948 0.2455 0.5268 0.039 Uiso 1 1 calc R . . C18 C 0.31638(19) 0.17955(17) 0.50547(16) 0.0352(10) Uani 1 1 d . . . H18A H 0.3075 0.1627 0.5327 0.042 Uiso 1 1 calc R . . H18B H 0.2887 0.1772 0.4852 0.042 Uiso 1 1 calc R . . O9 O 0.35631(14) 0.15642(13) 0.48655(14) 0.0410(9) Uani 1 1 d . . . H9 H 0.3759 0.1486 0.5062 0.061 Uiso 1 1 calc R . . N4 N 0.36500(16) 0.40266(16) 0.44303(15) 0.0371(9) Uani 1 1 d . . . C19 C 0.31869(19) 0.4098(2) 0.46578(19) 0.0443(13) Uani 1 1 d . . . H19A H 0.2933 0.4174 0.4442 0.053 Uiso 1 1 calc R . . H19B H 0.3215 0.4370 0.4862 0.053 Uiso 1 1 calc R . . C20 C 0.30459(18) 0.36458(19) 0.49137(17) 0.0376(11) Uani 1 1 d . . . H20A H 0.2797 0.3723 0.5134 0.045 Uiso 1 1 calc R . . H20B H 0.2913 0.3403 0.4712 0.045 Uiso 1 1 calc R . . O10 O 0.34644(12) 0.34692(11) 0.51209(11) 0.0299(7) Uani 1 1 d . . . C21 C 0.3591(2) 0.3785(2) 0.40007(19) 0.0437(13) Uani 1 1 d . . . H21A H 0.3844 0.3895 0.3797 0.052 Uiso 1 1 calc R . . H21B H 0.3274 0.3867 0.3874 0.052 Uiso 1 1 calc R . . C22 C 0.3629(2) 0.3246(2) 0.40638(19) 0.0422(13) Uani 1 1 d . . . H22A H 0.3336 0.3125 0.4211 0.051 Uiso 1 1 calc R . . H22B H 0.3657 0.3086 0.3777 0.051 Uiso 1 1 calc R . . O11 O 0.40417(13) 0.31455(13) 0.43219(11) 0.0363(7) Uani 1 1 d . . . C23 C 0.3914(2) 0.44857(18) 0.44064(17) 0.0397(11) Uani 1 1 d . . . H23A H 0.3691 0.4744 0.4322 0.048 Uiso 1 1 calc R . . H23B H 0.4171 0.4465 0.4183 0.048 Uiso 1 1 calc R . . C24 C 0.41352(19) 0.45938(18) 0.48495(16) 0.0366(10) Uani 1 1 d . . . H24A H 0.4383 0.4845 0.4819 0.044 Uiso 1 1 calc R . . H24B H 0.3883 0.4712 0.5051 0.044 Uiso 1 1 calc R . . O12 O 0.43479(13) 0.41720(12) 0.50245(11) 0.0353(7) Uani 1 1 d . . . N5 N 0.52625(17) 0.36039(16) 0.39196(14) 0.0390(10) Uani 1 1 d . . . C25 C 0.5357(2) 0.38789(19) 0.43291(18) 0.0402(11) Uani 1 1 d . . . H25A H 0.5152 0.4168 0.4337 0.048 Uiso 1 1 calc R . . H25B H 0.5698 0.3980 0.4340 0.048 Uiso 1 1 calc R . . C26 C 0.52425(19) 0.35617(19) 0.47176(16) 0.0352(10) Uani 1 1 d . . . H26A H 0.5496 0.3316 0.4751 0.042 Uiso 1 1 calc R . . H26B H 0.5233 0.3755 0.4988 0.042 Uiso 1 1 calc R . . O13 O 0.47944(12) 0.33430(13) 0.46488(11) 0.0335(7) Uani 1 1 d . . . C27 C 0.5701(2) 0.3371(2) 0.37418(18) 0.0453(13) Uani 1 1 d . . . H27A H 0.5975 0.3597 0.3752 0.054 Uiso 1 1 calc R . . H27B H 0.5646 0.3281 0.3434 0.054 Uiso 1 1 calc R . . C28 C 0.5823(2) 0.29275(18) 0.40080(17) 0.0383(11) Uani 1 1 d . . . H28A H 0.6041 0.2718 0.3840 0.046 Uiso 1 1 calc R . . H28B H 0.5986 0.3019 0.4283 0.046 Uiso 1 1 calc R . . O14 O 0.53841(12) 0.26846(12) 0.41018(11) 0.0353(7) Uani 1 1 d . . . C29 C 0.5012(3) 0.3885(2) 0.3587(2) 0.0543(15) Uani 1 1 d . . . H29A H 0.5245 0.4088 0.3428 0.065 Uiso 1 1 calc R . . H29B H 0.4770 0.4095 0.3727 0.065 Uiso 1 1 calc R . . C30 C 0.4762(3) 0.3546(3) 0.3266(2) 0.0572(17) Uani 1 1 d . . . H30A H 0.4509 0.3720 0.3104 0.069 Uiso 1 1 calc R . . H30B H 0.4999 0.3424 0.3053 0.069 Uiso 1 1 calc R . . O15 O 0.45538(16) 0.31612(15) 0.34940(12) 0.0479(10) Uani 1 1 d . . . O16 O 0.28394(11) 0.31241(11) 0.65265(10) 0.0311(7) Uani 1 1 d . . . O17 O 0.28665(11) 0.30885(11) 0.57970(10) 0.0280(6) Uani 1 1 d . . . C31 C 0.26513(16) 0.30512(16) 0.61576(16) 0.0307(9) Uani 1 1 d . . . C32 C 0.2122(2) 0.2919(3) 0.6136(2) 0.0544(16) Uani 1 1 d . . . H32A H 0.2078 0.2593 0.6244 0.082 Uiso 1 1 calc R . . H32B H 0.2010 0.2938 0.5834 0.082 Uiso 1 1 calc R . . H32C H 0.1935 0.3139 0.6317 0.082 Uiso 1 1 calc R . . O18 O 0.47416(12) 0.47105(10) 0.72214(10) 0.0288(6) Uani 1 1 d . . . C33 C 0.5000 0.4927(2) 0.7500 0.0272(12) Uani 1 2 d S . . C34 C 0.5000 0.5457(2) 0.7500 0.0457(19) Uani 1 2 d S . . H34A H 0.4816 0.5574 0.7751 0.069 Uiso 0.50 1 calc PR . . H34B H 0.4852 0.5574 0.7230 0.069 Uiso 0.50 1 calc PR . . H34C H 0.5332 0.5574 0.7519 0.069 Uiso 0.50 1 calc PR . . O19 O 0.35773(11) 0.27868(12) 0.72569(11) 0.0309(7) Uani 1 1 d . . . C35 C 0.3799(2) 0.2500 0.7500 0.0257(12) Uani 1 2 d S . . C36 C 0.4338(3) 0.2500 0.7500 0.0439(18) Uani 1 2 d S . . H36A H 0.4456 0.2755 0.7309 0.066 Uiso 0.50 1 calc PR . . H36B H 0.4456 0.2192 0.7393 0.066 Uiso 0.50 1 calc PR . . H36C H 0.4456 0.2553 0.7798 0.066 Uiso 0.50 1 calc PR . . N31A N 0.2717(12) 0.3455(8) 0.8431(8) 0.157(5) Uiso 0.50 1 d PD A 1 O31A O 0.2888(5) 0.3146(5) 0.8146(4) 0.090(4) Uiso 0.50 1 d PD A 1 O32A O 0.2494(7) 0.3301(7) 0.8773(6) 0.144(7) Uiso 0.50 1 d PD A 1 O33A O 0.2910(10) 0.3884(7) 0.8443(8) 0.202(10) Uiso 0.50 1 d PD A 1 N31B N 0.2676(8) 0.3464(11) 0.8466(8) 0.157(5) Uiso 0.50 1 d PD B 2 O31B O 0.3091(6) 0.3466(5) 0.8256(4) 0.097(5) Uiso 0.50 1 d PD B 2 O32B O 0.2321(7) 0.3204(9) 0.8326(7) 0.188(10) Uiso 0.50 1 d PD B 2 O33B O 0.2662(5) 0.3646(6) 0.8854(4) 0.104(4) Uiso 0.50 1 d PD B 2 O41 O 0.39357(18) 0.0916(2) 0.5454(2) 0.088(2) Uani 1 1 d . . . O42B O 0.2658(3) 0.2372(3) 0.7833(3) 0.052(2) Uiso 0.50 1 d P C -2 O43A O 0.3144(7) 0.0492(7) 0.5835(7) 0.138(6) Uiso 0.50 1 d P . 1 O43B O 0.3299(6) 0.0671(6) 0.6107(6) 0.111(5) Uiso 0.50 1 d P D -2 O44A O 0.2340(10) -0.0137(10) 0.5692(7) 0.181(9) Uiso 0.50 1 d P . 1 O45A O 0.5312(11) 0.2591(12) 0.2913(9) 0.209(12) Uiso 0.50 1 d P E -3 O45B O 0.5770(12) 0.2476(12) 0.2889(10) 0.221(12) Uiso 0.50 1 d P E -3 N51 N 0.4016(5) 0.4673(3) 0.3225(3) 0.119(4) Uani 1 1 d D . . C51 C 0.3612(4) 0.4699(4) 0.3193(3) 0.079(3) Uani 1 1 d D . . C52 C 0.3157(5) 0.4755(5) 0.3148(5) 0.155(7) Uani 1 1 d D . . H52A H 0.3059 0.5055 0.3284 0.232 Uiso 1 1 calc R . . H52B H 0.2988 0.4489 0.3287 0.232 Uiso 1 1 calc R . . H52C H 0.3077 0.4763 0.2836 0.232 Uiso 1 1 calc R . . N52A N 0.2803(10) 0.0558(11) 0.4847(8) 0.179(11) Uiso 0.50 1 d PD F 1 C53A C 0.3064(4) 0.0490(4) 0.4574(4) 0.042(2) Uiso 0.50 1 d PD F 1 C54A C 0.3330(8) 0.0498(9) 0.4243(7) 0.100(6) Uiso 0.50 1 d PD F 1 N52B N 0.3274(11) 0.0760(11) 0.4284(8) 0.161(11) Uiso 0.50 1 d PD G 2 C53B C 0.3428(8) 0.0606(7) 0.3955(7) 0.087(5) Uiso 0.50 1 d PD G 2 C54B C 0.3790(13) 0.0436(15) 0.3742(12) 0.189(15) Uiso 0.50 1 d PD G 2 N53A N 0.1310(7) 0.0939(7) 0.7874(6) 0.103(5) Uiso 0.50 1 d P H 1 C55A C 0.1342(8) 0.1263(9) 0.7647(8) 0.104(7) Uiso 0.50 1 d PD H 1 C56A C 0.1526(15) 0.1773(12) 0.7735(15) 0.192(15) Uiso 0.50 1 d PD H 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.01816(15) 0.01824(15) 0.03133(15) 0.00027(6) -0.00236(7) 0.00295(6) Fe1 0.0219(3) 0.0166(3) 0.0308(3) -0.0014(2) -0.0035(2) 0.0015(2) Fe2 0.0203(3) 0.0206(3) 0.0302(3) 0.0027(2) -0.0037(2) 0.0005(2) Fe3 0.0258(3) 0.0279(3) 0.0320(3) 0.0052(2) -0.0032(2) -0.0039(3) Fe4 0.0314(4) 0.0335(4) 0.0356(4) -0.0028(3) 0.0026(3) -0.0065(3) N1 0.0212(18) 0.0194(16) 0.0329(17) -0.0014(13) -0.0022(14) -0.0003(13) C1 0.025(2) 0.031(2) 0.033(2) -0.0006(17) 0.0013(17) -0.0078(17) C2 0.022(2) 0.035(2) 0.036(2) -0.0026(18) -0.0010(17) -0.0021(18) O1 0.0203(15) 0.0252(15) 0.0343(15) 0.0013(12) -0.0015(12) -0.0011(11) C3 0.027(2) 0.0199(19) 0.035(2) -0.0010(16) -0.0003(17) -0.0029(16) C4 0.021(2) 0.0184(18) 0.033(2) -0.0005(15) -0.0011(16) 0.0024(15) O2 0.0194(16) 0.0175(14) 0.0314(14) -0.0012(10) -0.0008(12) 0.0008(11) C5 0.030(2) 0.0203(19) 0.035(2) 0.0036(16) -0.0045(17) 0.0000(16) C6 0.041(3) 0.026(2) 0.038(2) 0.0035(18) -0.001(2) -0.004(2) O3 0.0298(18) 0.0326(17) 0.0394(17) 0.0019(13) -0.0033(14) -0.0055(14) N2 0.024(2) 0.033(2) 0.045(2) 0.0003(16) -0.0034(16) 0.0101(16) C7 0.035(3) 0.026(2) 0.054(3) -0.005(2) -0.009(2) 0.014(2) C8 0.032(3) 0.026(2) 0.052(3) -0.011(2) -0.007(2) 0.0110(19) O4 0.0281(17) 0.0216(14) 0.0407(17) -0.0080(12) -0.0044(13) 0.0073(12) C9 0.027(2) 0.029(2) 0.047(3) 0.0030(19) -0.0059(19) 0.0101(18) C10 0.030(2) 0.025(2) 0.042(2) 0.0088(18) -0.0052(19) 0.0031(18) O5 0.0229(16) 0.0181(14) 0.0407(17) 0.0019(12) -0.0039(12) 0.0029(11) C11 0.027(3) 0.040(3) 0.058(3) -0.007(2) 0.001(2) 0.012(2) C12 0.032(3) 0.045(3) 0.058(3) -0.006(2) 0.010(2) 0.015(2) O6 0.038(2) 0.045(2) 0.0364(18) 0.0008(15) 0.0049(15) 0.0149(16) N3 0.030(2) 0.0230(18) 0.0294(18) -0.0014(14) -0.0064(14) -0.0006(14) C13 0.029(2) 0.022(2) 0.029(2) 0.0004(16) -0.0034(16) -0.0016(16) C14 0.030(2) 0.0163(18) 0.031(2) -0.0028(15) -0.0024(17) 0.0008(15) O7 0.0253(16) 0.0180(13) 0.0308(14) 0.0009(11) -0.0004(12) 0.0026(11) C15 0.026(2) 0.029(2) 0.030(2) -0.0019(16) -0.0014(17) 0.0014(17) C16 0.025(2) 0.025(2) 0.032(2) 0.0018(16) 0.0015(17) 0.0033(16) O8 0.0216(15) 0.0253(15) 0.0316(15) 0.0026(11) -0.0008(12) 0.0014(11) C17 0.033(3) 0.028(2) 0.036(2) 0.0004(17) -0.0094(19) -0.0036(18) C18 0.033(3) 0.036(2) 0.037(2) -0.0046(18) -0.0037(19) -0.010(2) O9 0.041(2) 0.032(2) 0.050(2) -0.0090(15) -0.0016(16) -0.0071(14) N4 0.037(2) 0.033(2) 0.041(2) 0.0102(17) -0.0068(17) -0.0053(17) C19 0.031(3) 0.046(3) 0.056(3) 0.024(2) -0.007(2) 0.001(2) C20 0.027(2) 0.045(3) 0.042(3) 0.014(2) -0.0082(19) -0.001(2) O10 0.0210(16) 0.0328(17) 0.0359(17) 0.0093(12) -0.0046(13) 0.0015(12) C21 0.044(3) 0.045(3) 0.041(3) 0.009(2) -0.012(2) -0.010(2) C22 0.041(3) 0.045(3) 0.041(3) 0.007(2) -0.012(2) -0.006(2) O11 0.0347(19) 0.0396(18) 0.0345(17) 0.0030(14) -0.0064(14) -0.0075(15) C23 0.047(3) 0.033(2) 0.039(2) 0.0104(19) -0.005(2) -0.005(2) C24 0.036(3) 0.033(2) 0.041(2) 0.0067(19) -0.005(2) -0.002(2) O12 0.0345(19) 0.0273(15) 0.0441(18) 0.0059(13) -0.0074(14) -0.0033(14) N5 0.044(3) 0.034(2) 0.039(2) 0.0097(17) 0.0052(18) -0.0012(18) C25 0.034(3) 0.035(3) 0.052(3) 0.004(2) 0.002(2) -0.006(2) C26 0.030(3) 0.038(3) 0.037(2) -0.0017(19) -0.0038(19) -0.004(2) O13 0.0267(17) 0.0385(17) 0.0353(17) 0.0001(13) 0.0022(13) -0.0069(14) C27 0.045(3) 0.050(3) 0.040(3) 0.005(2) 0.014(2) -0.001(2) C28 0.037(3) 0.034(2) 0.044(3) -0.001(2) 0.005(2) -0.007(2) O14 0.0303(18) 0.0336(18) 0.0421(18) 0.0008(14) 0.0013(14) -0.0068(14) C29 0.049(4) 0.056(4) 0.057(3) 0.024(3) -0.005(3) -0.007(3) C30 0.062(4) 0.066(4) 0.044(3) 0.020(3) -0.007(3) -0.003(3) O15 0.054(3) 0.057(2) 0.0328(18) 0.0114(16) -0.0107(16) -0.0088(19) O16 0.0217(16) 0.0352(17) 0.0363(16) 0.0039(13) -0.0005(13) 0.0004(13) O17 0.0208(15) 0.0283(15) 0.0348(15) 0.0029(12) -0.0035(12) -0.0003(12) C31 0.019(2) 0.029(2) 0.044(2) 0.0043(18) -0.0050(18) -0.0023(17) C32 0.022(3) 0.092(5) 0.049(3) -0.002(3) 0.002(2) -0.017(3) O18 0.0330(17) 0.0183(14) 0.0351(16) 0.0013(11) -0.0062(13) 0.0001(12) C33 0.029(3) 0.028(3) 0.025(3) 0.000 0.000(2) 0.000 C34 0.071(6) 0.027(3) 0.039(4) 0.000 -0.018(4) 0.000 O19 0.0289(18) 0.0298(17) 0.0339(17) 0.0050(13) 0.0011(12) 0.0029(12) C35 0.034(3) 0.018(3) 0.025(3) 0.002(2) 0.000 0.000 C36 0.023(3) 0.043(4) 0.066(5) 0.025(4) 0.000 0.000 O41 0.042(3) 0.085(4) 0.136(5) 0.045(4) 0.004(3) 0.014(3) N51 0.186(13) 0.065(5) 0.106(7) 0.024(4) 0.021(7) -0.022(7) C51 0.089(8) 0.074(6) 0.076(6) 0.028(4) -0.012(5) -0.018(5) C52 0.133(12) 0.124(11) 0.208(15) 0.082(10) -0.083(11) -0.048(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 O4 2.318(3) . ? Dy1 O5 2.327(3) . ? Dy1 O7 2.328(3) . ? Dy1 O2 2.336(3) . ? Dy1 O19 2.351(3) . ? Dy1 O16 2.397(3) . ? Dy1 O6 2.458(4) . ? Dy1 N2 2.652(4) . ? Fe1 O4 1.943(3) . ? Fe1 O2 1.952(3) . ? Fe1 O1 1.970(3) 3_656 ? Fe1 O1 2.034(3) . ? Fe1 O18 2.042(3) . ? Fe1 N1 2.244(4) . ? Fe2 O5 1.954(3) . ? Fe2 O7 1.971(3) . ? Fe2 O10 1.973(3) . ? Fe2 O8 2.007(3) . ? Fe2 O17 2.036(3) . ? Fe2 N3 2.249(4) . ? Fe3 O12 1.901(3) . ? Fe3 O11 2.004(3) . ? Fe3 O8 2.007(3) . ? Fe3 O13 2.027(4) . ? Fe3 O10 2.052(4) . ? Fe3 N4 2.276(4) . ? Fe4 O15 1.890(4) . ? Fe4 O14 1.987(3) 6 ? Fe4 O13 1.995(3) . ? Fe4 O14 2.053(4) . ? Fe4 O11 2.075(4) . ? Fe4 N5 2.280(4) . ? N1 C1 1.484(6) . ? N1 C3 1.499(5) . ? N1 C5 1.501(5) . ? C1 C2 1.521(7) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 O1 1.432(5) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? O1 Fe1 1.970(3) 3_656 ? C3 C4 1.527(6) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 O2 1.417(5) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.523(6) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 O3 1.420(6) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? O3 H3 0.8400 . ? N2 C11 1.490(7) . ? N2 C9 1.490(6) . ? N2 C7 1.492(7) . ? C7 C8 1.523(7) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 O4 1.417(5) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.530(7) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 O5 1.426(5) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.491(8) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 O6 1.443(6) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? O6 H6 0.86(4) . ? N3 C15 1.482(6) . ? N3 C17 1.482(6) . ? N3 C13 1.496(6) . ? C13 C14 1.535(6) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 O7 1.410(5) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.539(6) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 O8 1.406(5) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.520(6) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 O9 1.410(6) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? O9 H9 0.8400 . ? N4 C19 1.477(7) . ? N4 C23 1.485(6) . ? N4 C21 1.490(8) . ? C19 C20 1.543(7) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 O10 1.414(6) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.530(8) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 O11 1.422(6) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.521(7) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 O12 1.428(6) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? N5 C29 1.466(7) . ? N5 C27 1.485(7) . ? N5 C25 1.497(7) . ? C25 C26 1.520(7) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 O13 1.404(6) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.527(8) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 O14 1.426(6) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? O14 Fe4 1.987(3) 6 ? C29 C30 1.534(10) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 O15 1.410(8) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? O16 C31 1.262(6) . ? O17 C31 1.261(6) . ? C31 C32 1.519(7) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? O18 C33 1.270(4) . ? C33 O18 1.270(4) 3_656 ? C33 C34 1.490(9) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? O19 C35 1.259(4) . ? C35 O19 1.258(4) 8_456 ? C35 C36 1.496(9) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? N31A O32A 1.291(15) . ? N31A O31A 1.319(15) . ? N31A O33A 1.320(14) . ? N31B O33B 1.295(14) . ? N31B O32B 1.300(14) . ? N31B O31B 1.318(14) . ? N51 C51 1.130(13) . ? C51 C52 1.279(14) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? N52A C53A 1.122(18) . ? C53A C54A 1.258(18) . ? N52B C53B 1.178(19) . ? C53B C54B 1.29(2) . ? N53A C55A 1.15(3) . ? C55A C56A 1.54(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 O4 Dy1 O5 92.19(11) . . ? O4 Dy1 O7 136.05(11) . . ? O5 Dy1 O7 66.63(10) . . ? O4 Dy1 O2 65.09(10) . . ? O5 Dy1 O2 94.51(10) . . ? O7 Dy1 O2 78.15(10) . . ? O4 Dy1 O19 113.89(12) . . ? O5 Dy1 O19 150.94(11) . . ? O7 Dy1 O19 85.11(11) . . ? O2 Dy1 O19 85.75(10) . . ? O4 Dy1 O16 142.76(11) . . ? O5 Dy1 O16 82.13(10) . . ? O7 Dy1 O16 74.78(11) . . ? O2 Dy1 O16 151.75(10) . . ? O19 Dy1 O16 84.08(11) . . ? O4 Dy1 O6 80.08(13) . . ? O5 Dy1 O6 131.08(11) . . ? O7 Dy1 O6 143.02(12) . . ? O2 Dy1 O6 123.75(12) . . ? O19 Dy1 O6 69.17(12) . . ? O16 Dy1 O6 76.48(12) . . ? O4 Dy1 N2 67.61(12) . . ? O5 Dy1 N2 68.10(12) . . ? O7 Dy1 N2 128.62(12) . . ? O2 Dy1 N2 128.56(12) . . ? O19 Dy1 N2 132.43(12) . . ? O16 Dy1 N2 76.23(12) . . ? O6 Dy1 N2 64.30(13) . . ? O4 Fe1 O2 80.01(13) . . ? O4 Fe1 O1 99.96(13) . 3_656 ? O2 Fe1 O1 104.67(13) . 3_656 ? O4 Fe1 O1 173.92(14) . . ? O2 Fe1 O1 99.99(13) . . ? O1 Fe1 O1 74.11(14) 3_656 . ? O4 Fe1 O18 89.72(13) . . ? O2 Fe1 O18 160.06(13) . . ? O1 Fe1 O18 93.87(13) 3_656 . ? O1 Fe1 O18 92.02(13) . . ? O4 Fe1 N1 107.94(14) . . ? O2 Fe1 N1 80.19(13) . . ? O1 Fe1 N1 152.09(13) 3_656 . ? O1 Fe1 N1 77.99(13) . . ? O18 Fe1 N1 86.89(13) . . ? O5 Fe2 O7 81.30(13) . . ? O5 Fe2 O10 102.57(14) . . ? O7 Fe2 O10 171.52(14) . . ? O5 Fe2 O8 101.55(13) . . ? O7 Fe2 O8 96.74(12) . . ? O10 Fe2 O8 75.16(13) . . ? O5 Fe2 O17 93.97(13) . . ? O7 Fe2 O17 96.17(13) . . ? O10 Fe2 O17 91.11(14) . . ? O8 Fe2 O17 161.11(13) . . ? O5 Fe2 N3 160.88(13) . . ? O7 Fe2 N3 79.58(13) . . ? O10 Fe2 N3 96.37(14) . . ? O8 Fe2 N3 80.70(13) . . ? O17 Fe2 N3 88.17(13) . . ? O12 Fe3 O11 142.38(15) . . ? O12 Fe3 O8 98.56(14) . . ? O11 Fe3 O8 115.87(13) . . ? O12 Fe3 O13 94.15(15) . . ? O11 Fe3 O13 72.49(14) . . ? O8 Fe3 O13 89.61(13) . . ? O12 Fe3 O10 106.19(15) . . ? O11 Fe3 O10 98.15(14) . . ? O8 Fe3 O10 73.44(12) . . ? O13 Fe3 O10 155.03(14) . . ? O12 Fe3 N4 79.65(15) . . ? O11 Fe3 N4 78.74(16) . . ? O8 Fe3 N4 147.97(15) . . ? O13 Fe3 N4 122.40(16) . . ? O10 Fe3 N4 76.40(14) . . ? O15 Fe4 O14 102.46(17) . 6 ? O15 Fe4 O13 138.91(17) . . ? O14 Fe4 O13 115.87(15) 6 . ? O15 Fe4 O14 111.09(17) . . ? O14 Fe4 O14 71.89(15) 6 . ? O13 Fe4 O14 95.05(14) . . ? O15 Fe4 O11 94.26(17) . . ? O14 Fe4 O11 91.23(14) 6 . ? O13 Fe4 O11 71.66(14) . . ? O14 Fe4 O11 151.78(14) . . ? O15 Fe4 N5 78.95(17) . . ? O14 Fe4 N5 145.64(16) 6 . ? O13 Fe4 N5 77.58(15) . . ? O14 Fe4 N5 75.63(15) . . ? O11 Fe4 N5 123.07(15) . . ? C1 N1 C3 112.8(3) . . ? C1 N1 C5 111.8(3) . . ? C3 N1 C5 112.5(3) . . ? C1 N1 Fe1 104.3(3) . . ? C3 N1 Fe1 105.8(2) . . ? C5 N1 Fe1 109.0(3) . . ? N1 C1 C2 110.1(3) . . ? N1 C1 H1A 109.6 . . ? C2 C1 H1A 109.6 . . ? N1 C1 H1B 109.6 . . ? C2 C1 H1B 109.6 . . ? H1A C1 H1B 108.1 . . ? O1 C2 C1 108.7(4) . . ? O1 C2 H2A 110.0 . . ? C1 C2 H2A 110.0 . . ? O1 C2 H2B 110.0 . . ? C1 C2 H2B 110.0 . . ? H2A C2 H2B 108.3 . . ? C2 O1 Fe1 130.3(3) . 3_656 ? C2 O1 Fe1 119.4(3) . . ? Fe1 O1 Fe1 100.43(14) 3_656 . ? N1 C3 C4 110.3(3) . . ? N1 C3 H3A 109.6 . . ? C4 C3 H3A 109.6 . . ? N1 C3 H3B 109.6 . . ? C4 C3 H3B 109.6 . . ? H3A C3 H3B 108.1 . . ? O2 C4 C3 108.7(3) . . ? O2 C4 H4A 109.9 . . ? C3 C4 H4A 109.9 . . ? O2 C4 H4B 109.9 . . ? C3 C4 H4B 109.9 . . ? H4A C4 H4B 108.3 . . ? C4 O2 Fe1 109.8(2) . . ? C4 O2 Dy1 133.1(2) . . ? Fe1 O2 Dy1 106.88(13) . . ? N1 C5 C6 116.3(4) . . ? N1 C5 H5A 108.2 . . ? C6 C5 H5A 108.2 . . ? N1 C5 H5B 108.2 . . ? C6 C5 H5B 108.2 . . ? H5A C5 H5B 107.4 . . ? O3 C6 C5 114.1(4) . . ? O3 C6 H6A 108.7 . . ? C5 C6 H6A 108.7 . . ? O3 C6 H6B 108.7 . . ? C5 C6 H6B 108.7 . . ? H6A C6 H6B 107.6 . . ? C6 O3 H3 109.5 . . ? C11 N2 C9 110.2(4) . . ? C11 N2 C7 112.0(4) . . ? C9 N2 C7 109.5(4) . . ? C11 N2 Dy1 108.1(3) . . ? C9 N2 Dy1 107.2(3) . . ? C7 N2 Dy1 109.7(3) . . ? N2 C7 C8 112.7(4) . . ? N2 C7 H7A 109.1 . . ? C8 C7 H7A 109.1 . . ? N2 C7 H7B 109.1 . . ? C8 C7 H7B 109.1 . . ? H7A C7 H7B 107.8 . . ? O4 C8 C7 108.8(4) . . ? O4 C8 H8A 109.9 . . ? C7 C8 H8A 109.9 . . ? O4 C8 H8B 109.9 . . ? C7 C8 H8B 109.9 . . ? H8A C8 H8B 108.3 . . ? C8 O4 Fe1 130.2(3) . . ? C8 O4 Dy1 121.5(3) . . ? Fe1 O4 Dy1 107.88(13) . . ? N2 C9 C10 110.3(4) . . ? N2 C9 H9A 109.6 . . ? C10 C9 H9A 109.6 . . ? N2 C9 H9B 109.6 . . ? C10 C9 H9B 109.6 . . ? H9A C9 H9B 108.1 . . ? O5 C10 C9 109.9(4) . . ? O5 C10 H10A 109.7 . . ? C9 C10 H10A 109.7 . . ? O5 C10 H10B 109.7 . . ? C9 C10 H10B 109.7 . . ? H10A C10 H10B 108.2 . . ? C10 O5 Fe2 123.1(3) . . ? C10 O5 Dy1 123.1(3) . . ? Fe2 O5 Dy1 103.52(13) . . ? N2 C11 C12 111.8(4) . . ? N2 C11 H11A 109.3 . . ? C12 C11 H11A 109.3 . . ? N2 C11 H11B 109.3 . . ? C12 C11 H11B 109.3 . . ? H11A C11 H11B 107.9 . . ? O6 C12 C11 108.4(4) . . ? O6 C12 H12A 110.0 . . ? C11 C12 H12A 110.0 . . ? O6 C12 H12B 110.0 . . ? C11 C12 H12B 110.0 . . ? H12A C12 H12B 108.4 . . ? C12 O6 Dy1 125.3(3) . . ? C12 O6 H6 99(4) . . ? Dy1 O6 H6 135(4) . . ? C15 N3 C17 112.2(4) . . ? C15 N3 C13 113.4(3) . . ? C17 N3 C13 110.2(3) . . ? C15 N3 Fe2 106.3(3) . . ? C17 N3 Fe2 111.2(3) . . ? C13 N3 Fe2 103.1(3) . . ? N3 C13 C14 109.9(3) . . ? N3 C13 H13A 109.7 . . ? C14 C13 H13A 109.7 . . ? N3 C13 H13B 109.7 . . ? C14 C13 H13B 109.7 . . ? H13A C13 H13B 108.2 . . ? O7 C14 C13 109.6(3) . . ? O7 C14 H14A 109.8 . . ? C13 C14 H14A 109.8 . . ? O7 C14 H14B 109.8 . . ? C13 C14 H14B 109.8 . . ? H14A C14 H14B 108.2 . . ? C14 O7 Fe2 120.1(2) . . ? C14 O7 Dy1 131.5(2) . . ? Fe2 O7 Dy1 102.93(12) . . ? N3 C15 C16 112.0(3) . . ? N3 C15 H15A 109.2 . . ? C16 C15 H15A 109.2 . . ? N3 C15 H15B 109.2 . . ? C16 C15 H15B 109.2 . . ? H15A C15 H15B 107.9 . . ? O8 C16 C15 109.8(4) . . ? O8 C16 H16A 109.7 . . ? C15 C16 H16A 109.7 . . ? O8 C16 H16B 109.7 . . ? C15 C16 H16B 109.7 . . ? H16A C16 H16B 108.2 . . ? C16 O8 Fe2 111.4(3) . . ? C16 O8 Fe3 122.7(3) . . ? Fe2 O8 Fe3 105.64(14) . . ? N3 C17 C18 117.8(4) . . ? N3 C17 H17A 107.9 . . ? C18 C17 H17A 107.9 . . ? N3 C17 H17B 107.9 . . ? C18 C17 H17B 107.9 . . ? H17A C17 H17B 107.2 . . ? O9 C18 C17 113.7(4) . . ? O9 C18 H18A 108.8 . . ? C17 C18 H18A 108.8 . . ? O9 C18 H18B 108.8 . . ? C17 C18 H18B 108.8 . . ? H18A C18 H18B 107.7 . . ? C18 O9 H9 109.5 . . ? C19 N4 C23 109.6(4) . . ? C19 N4 C21 112.6(4) . . ? C23 N4 C21 113.9(4) . . ? C19 N4 Fe3 109.0(3) . . ? C23 N4 Fe3 103.8(3) . . ? C21 N4 Fe3 107.5(3) . . ? N4 C19 C20 110.4(4) . . ? N4 C19 H19A 109.6 . . ? C20 C19 H19A 109.6 . . ? N4 C19 H19B 109.6 . . ? C20 C19 H19B 109.6 . . ? H19A C19 H19B 108.1 . . ? O10 C20 C19 107.9(4) . . ? O10 C20 H20A 110.1 . . ? C19 C20 H20A 110.1 . . ? O10 C20 H20B 110.1 . . ? C19 C20 H20B 110.1 . . ? H20A C20 H20B 108.4 . . ? C20 O10 Fe2 133.0(3) . . ? C20 O10 Fe3 121.3(3) . . ? Fe2 O10 Fe3 105.19(15) . . ? N4 C21 C22 109.3(4) . . ? N4 C21 H21A 109.8 . . ? C22 C21 H21A 109.8 . . ? N4 C21 H21B 109.8 . . ? C22 C21 H21B 109.8 . . ? H21A C21 H21B 108.3 . . ? O11 C22 C21 108.7(4) . . ? O11 C22 H22A 109.9 . . ? C21 C22 H22A 109.9 . . ? O11 C22 H22B 109.9 . . ? C21 C22 H22B 109.9 . . ? H22A C22 H22B 108.3 . . ? C22 O11 Fe3 115.9(3) . . ? C22 O11 Fe4 124.8(3) . . ? Fe3 O11 Fe4 106.25(15) . . ? N4 C23 C24 109.2(4) . . ? N4 C23 H23A 109.8 . . ? C24 C23 H23A 109.8 . . ? N4 C23 H23B 109.8 . . ? C24 C23 H23B 109.8 . . ? H23A C23 H23B 108.3 . . ? O12 C24 C23 109.7(4) . . ? O12 C24 H24A 109.7 . . ? C23 C24 H24A 109.7 . . ? O12 C24 H24B 109.7 . . ? C23 C24 H24B 109.7 . . ? H24A C24 H24B 108.2 . . ? C24 O12 Fe3 121.1(3) . . ? C29 N5 C27 111.8(5) . . ? C29 N5 C25 112.9(5) . . ? C27 N5 C25 113.1(5) . . ? C29 N5 Fe4 103.1(4) . . ? C27 N5 Fe4 107.1(3) . . ? C25 N5 Fe4 108.3(3) . . ? N5 C25 C26 108.5(4) . . ? N5 C25 H25A 110.0 . . ? C26 C25 H25A 110.0 . . ? N5 C25 H25B 110.0 . . ? C26 C25 H25B 110.0 . . ? H25A C25 H25B 108.4 . . ? O13 C26 C25 108.9(4) . . ? O13 C26 H26A 109.9 . . ? C25 C26 H26A 109.9 . . ? O13 C26 H26B 109.9 . . ? C25 C26 H26B 109.9 . . ? H26A C26 H26B 108.3 . . ? C26 O13 Fe4 114.9(3) . . ? C26 O13 Fe3 128.8(3) . . ? Fe4 O13 Fe3 108.49(16) . . ? N5 C27 C28 110.2(4) . . ? N5 C27 H27A 109.6 . . ? C28 C27 H27A 109.6 . . ? N5 C27 H27B 109.6 . . ? C28 C27 H27B 109.6 . . ? H27A C27 H27B 108.1 . . ? O14 C28 C27 108.0(5) . . ? O14 C28 H28A 110.1 . . ? C27 C28 H28A 110.1 . . ? O14 C28 H28B 110.1 . . ? C27 C28 H28B 110.1 . . ? H28A C28 H28B 108.4 . . ? C28 O14 Fe4 126.5(3) . 6 ? C28 O14 Fe4 122.6(3) . . ? Fe4 O14 Fe4 107.92(15) 6 . ? N5 C29 C30 109.0(5) . . ? N5 C29 H29A 109.9 . . ? C30 C29 H29A 109.9 . . ? N5 C29 H29B 109.9 . . ? C30 C29 H29B 109.9 . . ? H29A C29 H29B 108.3 . . ? O15 C30 C29 110.1(5) . . ? O15 C30 H30A 109.6 . . ? C29 C30 H30A 109.6 . . ? O15 C30 H30B 109.6 . . ? C29 C30 H30B 109.6 . . ? H30A C30 H30B 108.2 . . ? C30 O15 Fe4 122.1(4) . . ? C31 O16 Dy1 135.2(3) . . ? C31 O17 Fe2 126.9(3) . . ? O17 C31 O16 125.1(4) . . ? O17 C31 C32 116.2(4) . . ? O16 C31 C32 118.6(4) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C33 O18 Fe1 130.5(3) . . ? O18 C33 O18 122.9(6) 3_656 . ? O18 C33 C34 118.5(3) 3_656 . ? O18 C33 C34 118.5(3) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C35 O19 Dy1 149.5(3) . . ? O19 C35 O19 121.3(6) 8_456 . ? O19 C35 C36 119.3(3) 8_456 . ? O19 C35 C36 119.3(3) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? O32A N31A O31A 119.4(15) . . ? O32A N31A O33A 118.7(14) . . ? O31A N31A O33A 118.1(14) . . ? O33B N31B O32B 120.1(13) . . ? O33B N31B O31B 118.3(14) . . ? O32B N31B O31B 120.2(13) . . ? O44A O44A O43A 164.7(15) 2 2 ? N51 C51 C52 176.3(13) . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? N52A C53A C54A 168(2) . . ? N52B C53B C54B 148(3) . . ? N53A C55A C56A 131(3) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3 O12 0.84 1.80 2.644(5) 179.3 . O6 H6 O31A 0.86(4) 1.81(4) 2.658(13) 172(6) . O6 H6 O31B 0.86(4) 1.88(5) 2.677(14) 153(6) . O9 H9 O41 0.84 2.06 2.764(7) 140.7 . _diffrn_measured_fraction_theta_max 0.934 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 4.175 _refine_diff_density_min -1.103 _refine_diff_density_rms 0.159 data_amac16eu _database_code_depnum_ccdc_archive 'CCDC 804182' #TrackingRef '- amer_fe16ln4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C136 H276 Eu4 Fe16 N20 O76, 4(N O3), 11(C2 H3 N), 16(H2 O) ' _chemical_formula_sum 'C158 H341 Eu4 Fe16 N35 O104' _chemical_formula_weight 5897.10 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' Fe Fe 0.3463 0.8444 '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 'C c c a' _symmetry_space_group_name_Hall '-C 2b 2bc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' '-x, y, -z+1/2' 'x+1/2, -y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1, -y+1/2, z' '-x+1/2, y+1/2, -z+1/2' 'x+1, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' 'x, -y, z-1/2' '-x-1/2, y, z-1/2' '-x+1/2, -y+1/2, -z' 'x, y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' '-x, y+1/2, z-1/2' _cell_length_a 27.7369(19) _cell_length_b 28.1589(19) _cell_length_c 30.573(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 23879(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 11623 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 27.72 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.640 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 12136 _exptl_absorpt_coefficient_mu 2.069 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.542 _exptl_absorpt_correction_T_max 0.682 _exptl_absorpt_process_details 'SADABS 2.10 (Bruker AXS Inc., 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART Apex' _diffrn_measurement_method 'CCD area detector' _diffrn_detector_area_resol_mean 8.333 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 84676 _diffrn_reflns_av_R_equivalents 0.0506 _diffrn_reflns_av_sigmaI/netI 0.0296 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 26.73 _reflns_number_total 12669 _reflns_number_gt 10454 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT 5.6 (Bruker AXS Inc., 2005)' _computing_cell_refinement 'SMART-NT 5.6 (Bruker AXS Inc., 2005)' _computing_data_reduction 'SAINT+ 6.45 (Bruker AXS Inc., 2003)' _computing_structure_solution 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_structure_refinement 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_molecular_graphics 'Diamond 2.1 (Crystal Impact, 1998)' _computing_publication_material 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _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. Within the asymmetric unit, one lattice water and one MeCN were ordered, and a further water was disordered across a twofold axis; these could be refined anisotropically. The nitrate anion is disordered between two positions: in one it is disordered with 75% occupancy against a lattice water (25%), in the other it is disordered (together with a lattice water) with 25% occupancy against a MeCN (75%). The remaining lattice waters and MeCN are also disordered. ; _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^)+(0.0956P)^2^+17.5123P] 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 12669 _refine_ls_number_parameters 724 _refine_ls_number_restraints 104 _refine_ls_R_factor_all 0.0628 _refine_ls_R_factor_gt 0.0496 _refine_ls_wR_factor_ref 0.1586 _refine_ls_wR_factor_gt 0.1500 _refine_ls_goodness_of_fit_ref 1.201 _refine_ls_restrained_S_all 1.220 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Eu1 Eu 0.358998(8) 0.345128(8) 0.677979(8) 0.02220(10) Uani 1 1 d . . . Fe1 Fe 0.46321(2) 0.40241(2) 0.71245(2) 0.02199(16) Uani 1 1 d . . . Fe2 Fe 0.35835(2) 0.31929(2) 0.56938(2) 0.02317(16) Uani 1 1 d . . . Fe3 Fe 0.41309(3) 0.35548(3) 0.48374(2) 0.02670(17) Uani 1 1 d . . . Fe4 Fe 0.47252(3) 0.30095(3) 0.40692(2) 0.02998(18) Uani 1 1 d . . . N1 N 0.49646(14) 0.41147(13) 0.64613(13) 0.0233(8) Uani 1 1 d . . . C1 C 0.54679(17) 0.42601(18) 0.65575(16) 0.0273(10) Uani 1 1 d . . . H1A H 0.5472 0.4594 0.6660 0.033 Uiso 1 1 calc R . . H1B H 0.5664 0.4240 0.6288 0.033 Uiso 1 1 calc R . . C2 C 0.56824(17) 0.39396(18) 0.69074(17) 0.0285(11) Uani 1 1 d . . . H2A H 0.5769 0.3628 0.6779 0.034 Uiso 1 1 calc R . . H2B H 0.5979 0.4085 0.7028 0.034 Uiso 1 1 calc R . . O1 O 0.53379(11) 0.38750(12) 0.72475(11) 0.0246(7) Uani 1 1 d . . . C3 C 0.49343(18) 0.36388(16) 0.62402(16) 0.0247(10) Uani 1 1 d . . . H3A H 0.5246 0.3565 0.6097 0.030 Uiso 1 1 calc R . . H3B H 0.4681 0.3646 0.6012 0.030 Uiso 1 1 calc R . . C4 C 0.48150(17) 0.32546(16) 0.65798(15) 0.0234(10) Uani 1 1 d . . . H4A H 0.4712 0.2960 0.6430 0.028 Uiso 1 1 calc R . . H4B H 0.5104 0.3182 0.6757 0.028 Uiso 1 1 calc R . . O2 O 0.44383(12) 0.34236(10) 0.68542(11) 0.0219(7) Uani 1 1 d . . . C5 C 0.46980(19) 0.44915(17) 0.62197(17) 0.0284(11) Uani 1 1 d . . . H5A H 0.4618 0.4748 0.6429 0.034 Uiso 1 1 calc R . . H5B H 0.4389 0.4355 0.6117 0.034 Uiso 1 1 calc R . . C6 C 0.4951(2) 0.47153(18) 0.58281(16) 0.0321(11) Uani 1 1 d . . . H6A H 0.4730 0.4950 0.5693 0.039 Uiso 1 1 calc R . . H6B H 0.5238 0.4889 0.5933 0.039 Uiso 1 1 calc R . . O3 O 0.50977(13) 0.43866(13) 0.55020(11) 0.0310(8) Uani 1 1 d . . . H3 H 0.4860 0.4316 0.5344 0.047 Uiso 1 1 calc R . . N2 N 0.30303(16) 0.42182(16) 0.66949(15) 0.0349(10) Uani 1 1 d . . . C7 C 0.3285(2) 0.46416(19) 0.68632(19) 0.0370(13) Uani 1 1 d . . . H7A H 0.3044 0.4864 0.6988 0.044 Uiso 1 1 calc R . . H7B H 0.3445 0.4805 0.6616 0.044 Uiso 1 1 calc R . . C8 C 0.3658(2) 0.4530(2) 0.7209(2) 0.0372(13) Uani 1 1 d . . . H8A H 0.3862 0.4812 0.7263 0.045 Uiso 1 1 calc R . . H8B H 0.3497 0.4443 0.7487 0.045 Uiso 1 1 calc R . . O4 O 0.39481(12) 0.41449(12) 0.70597(11) 0.0286(8) Uani 1 1 d . . . C9 C 0.2925(2) 0.42679(19) 0.62181(18) 0.0351(12) Uani 1 1 d . . . H9A H 0.2791 0.4588 0.6160 0.042 Uiso 1 1 calc R . . H9B H 0.2680 0.4030 0.6131 0.042 Uiso 1 1 calc R . . C10 C 0.33722(19) 0.41979(17) 0.59505(18) 0.0313(11) Uani 1 1 d . . . H10A H 0.3288 0.4197 0.5636 0.038 Uiso 1 1 calc R . . H10B H 0.3598 0.4464 0.6004 0.038 Uiso 1 1 calc R . . O5 O 0.36002(11) 0.37585(11) 0.60621(11) 0.0252(7) Uani 1 1 d . . . C11 C 0.2576(2) 0.4125(2) 0.6938(2) 0.0435(14) Uani 1 1 d . . . H11A H 0.2394 0.3871 0.6786 0.052 Uiso 1 1 calc R . . H11B H 0.2375 0.4415 0.6935 0.052 Uiso 1 1 calc R . . C12 C 0.2663(2) 0.3978(2) 0.7400(2) 0.0455(15) Uani 1 1 d . . . H12A H 0.2771 0.4255 0.7575 0.055 Uiso 1 1 calc R . . H12B H 0.2363 0.3853 0.7531 0.055 Uiso 1 1 calc R . . O6 O 0.30319(14) 0.36149(15) 0.74003(13) 0.0411(9) Uani 1 1 d D . . H6 H 0.300(3) 0.347(2) 0.7643(15) 0.049 Uiso 1 1 d D . . N3 N 0.36399(14) 0.24328(15) 0.54738(13) 0.0269(9) Uani 1 1 d . . . C13 C 0.35653(18) 0.21571(17) 0.58884(16) 0.0257(10) Uani 1 1 d . . . H13A H 0.3676 0.1826 0.5847 0.031 Uiso 1 1 calc R . . H13B H 0.3218 0.2151 0.5963 0.031 Uiso 1 1 calc R . . C14 C 0.38494(18) 0.23892(16) 0.62614(16) 0.0253(10) Uani 1 1 d . . . H14A H 0.3728 0.2272 0.6546 0.030 Uiso 1 1 calc R . . H14B H 0.4194 0.2303 0.6237 0.030 Uiso 1 1 calc R . . O7 O 0.37989(11) 0.28877(11) 0.62413(11) 0.0229(7) Uani 1 1 d . . . C15 C 0.41368(18) 0.23772(17) 0.52917(17) 0.0280(10) Uani 1 1 d . . . H15A H 0.4119 0.2372 0.4968 0.034 Uiso 1 1 calc R . . H15B H 0.4272 0.2069 0.5389 0.034 Uiso 1 1 calc R . . C16 C 0.44723(18) 0.27777(16) 0.54362(16) 0.0269(10) Uani 1 1 d . . . H16A H 0.4578 0.2722 0.5741 0.032 Uiso 1 1 calc R . . H16B H 0.4762 0.2782 0.5247 0.032 Uiso 1 1 calc R . . O8 O 0.42317(11) 0.32208(11) 0.54085(10) 0.0227(7) Uani 1 1 d . . . C17 C 0.32557(19) 0.23113(18) 0.51493(17) 0.0315(11) Uani 1 1 d . . . H17A H 0.3337 0.2469 0.4870 0.038 Uiso 1 1 calc R . . H17B H 0.2949 0.2451 0.5254 0.038 Uiso 1 1 calc R . . C18 C 0.3168(2) 0.17962(19) 0.50557(18) 0.0346(12) Uani 1 1 d . . . H18A H 0.3083 0.1633 0.5332 0.042 Uiso 1 1 calc R . . H18B H 0.2890 0.1767 0.4854 0.042 Uiso 1 1 calc R . . O9 O 0.35746(14) 0.15668(14) 0.48658(15) 0.0397(10) Uani 1 1 d . . . H9 H 0.3705 0.1389 0.5052 0.060 Uiso 1 1 calc R . . N4 N 0.36461(16) 0.40188(17) 0.44144(16) 0.0344(10) Uani 1 1 d . . . C19 C 0.3182(2) 0.4077(2) 0.46417(19) 0.0400(13) Uani 1 1 d . . . H19A H 0.2929 0.4148 0.4424 0.048 Uiso 1 1 calc R . . H19B H 0.3205 0.4351 0.4843 0.048 Uiso 1 1 calc R . . C20 C 0.30361(19) 0.36373(19) 0.49010(18) 0.0339(12) Uani 1 1 d . . . H20A H 0.2790 0.3721 0.5122 0.041 Uiso 1 1 calc R . . H20B H 0.2900 0.3393 0.4703 0.041 Uiso 1 1 calc R . . O10 O 0.34598(12) 0.34616(12) 0.51089(12) 0.0278(8) Uani 1 1 d . . . C21 C 0.3594(2) 0.3774(2) 0.3988(2) 0.0425(15) Uani 1 1 d . . . H21A H 0.3850 0.3882 0.3786 0.051 Uiso 1 1 calc R . . H21B H 0.3278 0.3855 0.3857 0.051 Uiso 1 1 calc R . . C22 C 0.3629(2) 0.3246(2) 0.40475(19) 0.0385(13) Uani 1 1 d . . . H22A H 0.3334 0.3126 0.4192 0.046 Uiso 1 1 calc R . . H22B H 0.3659 0.3089 0.3759 0.046 Uiso 1 1 calc R . . O11 O 0.40384(13) 0.31420(13) 0.43082(11) 0.0330(8) Uani 1 1 d . . . C23 C 0.3908(2) 0.4474(2) 0.43923(19) 0.0373(13) Uani 1 1 d . . . H23A H 0.3684 0.4731 0.4306 0.045 Uiso 1 1 calc R . . H23B H 0.4167 0.4454 0.4170 0.045 Uiso 1 1 calc R . . C24 C 0.4124(2) 0.45813(19) 0.48394(18) 0.0363(12) Uani 1 1 d . . . H24A H 0.4367 0.4838 0.4812 0.044 Uiso 1 1 calc R . . H24B H 0.3868 0.4692 0.5040 0.044 Uiso 1 1 calc R . . O12 O 0.43428(13) 0.41722(12) 0.50109(12) 0.0318(8) Uani 1 1 d . . . N5 N 0.52623(17) 0.36028(17) 0.39145(15) 0.0366(10) Uani 1 1 d . . . C25 C 0.5356(2) 0.38687(19) 0.43190(18) 0.0376(13) Uani 1 1 d . . . H25A H 0.5153 0.4158 0.4326 0.045 Uiso 1 1 calc R . . H25B H 0.5698 0.3968 0.4328 0.045 Uiso 1 1 calc R . . C26 C 0.52435(18) 0.35599(19) 0.47116(17) 0.0312(11) Uani 1 1 d . . . H26A H 0.5498 0.3316 0.4749 0.037 Uiso 1 1 calc R . . H26B H 0.5232 0.3757 0.4980 0.037 Uiso 1 1 calc R . . O13 O 0.47874(13) 0.33357(13) 0.46428(11) 0.0305(8) Uani 1 1 d . . . C27 C 0.5693(2) 0.3369(2) 0.3731(2) 0.0424(14) Uani 1 1 d . . . H27A H 0.5968 0.3593 0.3733 0.051 Uiso 1 1 calc R . . H27B H 0.5630 0.3275 0.3424 0.051 Uiso 1 1 calc R . . C28 C 0.5817(2) 0.2927(2) 0.40041(18) 0.0370(12) Uani 1 1 d . . . H28A H 0.6041 0.2719 0.3840 0.044 Uiso 1 1 calc R . . H28B H 0.5975 0.3023 0.4281 0.044 Uiso 1 1 calc R . . O14 O 0.53838(13) 0.26813(13) 0.40949(12) 0.0322(8) Uani 1 1 d . . . C29 C 0.5005(3) 0.3879(2) 0.3576(2) 0.0535(17) Uani 1 1 d . . . H29A H 0.5236 0.4086 0.3420 0.064 Uiso 1 1 calc R . . H29B H 0.4760 0.4084 0.3716 0.064 Uiso 1 1 calc R . . C30 C 0.4763(3) 0.3547(3) 0.3254(2) 0.0534(18) Uani 1 1 d . . . H30A H 0.4509 0.3720 0.3092 0.064 Uiso 1 1 calc R . . H30B H 0.5004 0.3430 0.3040 0.064 Uiso 1 1 calc R . . O15 O 0.45569(16) 0.31582(15) 0.34782(12) 0.0447(10) Uani 1 1 d . . . O16 O 0.28248(12) 0.31276(13) 0.65179(11) 0.0317(8) Uani 1 1 d . . . O17 O 0.28628(12) 0.30819(12) 0.57847(11) 0.0275(7) Uani 1 1 d . . . C31 C 0.26432(18) 0.30521(18) 0.61488(18) 0.0313(11) Uani 1 1 d . . . C32 C 0.2113(2) 0.2930(3) 0.6120(2) 0.0528(17) Uani 1 1 d . . . H32A H 0.1987 0.2869 0.6415 0.079 Uiso 1 1 calc R . . H32B H 0.2071 0.2646 0.5939 0.079 Uiso 1 1 calc R . . H32C H 0.1937 0.3196 0.5989 0.079 Uiso 1 1 calc R . . O18 O 0.47444(13) 0.47353(11) 0.72142(11) 0.0281(8) Uani 1 1 d . . . C33 C 0.5000 0.4941(2) 0.7500 0.0255(14) Uani 1 2 d S . . C34 C 0.5000 0.5473(3) 0.7500 0.045(2) Uani 1 2 d S . . H34A H 0.4815 0.5589 0.7752 0.067 Uiso 0.50 1 calc PR . . H34B H 0.4852 0.5589 0.7229 0.067 Uiso 0.50 1 calc PR . . H34C H 0.5332 0.5589 0.7519 0.067 Uiso 0.50 1 calc PR . . O19 O 0.35748(12) 0.27994(13) 0.72649(12) 0.0324(8) Uani 1 1 d . . . C35 C 0.3795(3) 0.2500 0.7500 0.0261(14) Uani 1 2 d S . . C36 C 0.4331(3) 0.2500 0.7500 0.041(2) Uani 1 2 d S . . H36A H 0.4449 0.2755 0.7309 0.062 Uiso 0.50 1 calc PR . . H36B H 0.4449 0.2193 0.7392 0.062 Uiso 0.50 1 calc PR . . H36C H 0.4449 0.2552 0.7798 0.062 Uiso 0.50 1 calc PR . . O41 O 0.39440(18) 0.0918(2) 0.5451(2) 0.087(2) Uani 1 1 d . . . O42 O 0.2625(4) 0.2604(3) 0.7165(2) 0.053(3) Uani 0.50 1 d P A -1 O43A O 0.3143(6) 0.5510(6) 0.4172(6) 0.122(5) Uiso 0.50 1 d P B 1 O43B O 0.3291(5) 0.5656(5) 0.3903(5) 0.096(4) Uiso 0.50 1 d P C 2 O44B O 0.2500 0.5000 0.4353(7) 0.116(7) Uiso 0.50 2 d SP D 2 O45A O 0.5544(7) 0.2560(7) 0.2874(6) 0.148(7) Uiso 0.50 1 d P E 1 O45B O 0.5000 0.2500 0.2956(10) 0.152(10) Uiso 0.50 2 d SP F 2 N51 N 0.4014(5) 0.4641(4) 0.3207(3) 0.114(3) Uani 1 1 d DU . . C51 C 0.3593(5) 0.4695(4) 0.3169(4) 0.095(3) Uani 1 1 d DU . . C52 C 0.3111(5) 0.4764(5) 0.3145(5) 0.164(7) Uani 1 1 d DU . . H52A H 0.2944 0.4477 0.3245 0.245 Uiso 1 1 calc R . . H52B H 0.3020 0.4832 0.2842 0.245 Uiso 1 1 calc R . . H52C H 0.3020 0.5033 0.3332 0.245 Uiso 1 1 calc R . . N52A N 0.3677(6) 0.4042(7) 0.2154(6) 0.095(5) Uiso 0.50 1 d PDU G 1 C53A C 0.368(2) 0.3714(12) 0.2426(14) 0.184(10) Uiso 0.50 1 d PDU G 1 C54A C 0.3689(12) 0.3280(10) 0.2606(11) 0.154(11) Uiso 0.50 1 d PDU G 1 N52B N 0.311(2) 0.2865(18) 0.230(2) 0.44(4) Uiso 0.50 1 d PDU H 2 C53B C 0.3442(12) 0.3168(12) 0.2245(11) 0.139(10) Uiso 0.50 1 d PDU H 2 C54B C 0.361(2) 0.3610(14) 0.2312(18) 0.184(10) Uiso 0.50 1 d PDU H 2 N53A N 0.1955(8) 0.4526(5) 0.5381(6) 0.112(3) Uiso 0.75 1 d PD I 1 C81A C 0.1692(6) 0.4467(6) 0.5728(5) 0.113(5) Uiso 0.75 1 d PD I 1 C82A C 0.1547(7) 0.4364(6) 0.6110(5) 0.118(5) Uiso 0.75 1 d PD I 1 N31B N 0.193(2) 0.4460(8) 0.5438(15) 0.112(3) Uiso 0.25 1 d PD J 2 O31B O 0.1722(7) 0.4146(6) 0.5673(6) 0.055(5) Uiso 0.25 1 d PD J 2 O32B O 0.1973(6) 0.4890(5) 0.5573(5) 0.053(4) Uiso 0.25 1 d PD J 2 O33B O 0.2216(7) 0.4330(6) 0.5129(5) 0.061(5) Uiso 0.25 1 d PD J 2 O34B O 0.1138(10) 0.4559(9) 0.6343(8) 0.089(7) Uiso 0.25 1 d P K 2 N31A N 0.2701(4) 0.3449(4) 0.8457(3) 0.093(3) Uiso 0.40 1 d PD L 1 O31A O 0.3102(5) 0.3539(6) 0.8285(4) 0.071(4) Uiso 0.40 1 d PD L 1 O32A O 0.2644(5) 0.3601(5) 0.8859(4) 0.069(4) Uiso 0.40 1 d PD L 1 O33A O 0.2349(6) 0.3243(8) 0.8288(6) 0.132(8) Uiso 0.40 1 d PD L 1 N31C N 0.2701(4) 0.3449(4) 0.8457(3) 0.093(3) Uiso 0.35 1 d PD M 3 O31C O 0.2805(8) 0.3166(6) 0.8121(5) 0.088(6) Uiso 0.35 1 d PD M 3 O32C O 0.2833(10) 0.3878(6) 0.8434(7) 0.142(9) Uiso 0.35 1 d PD M 3 O33C O 0.2496(6) 0.3264(6) 0.8772(5) 0.082(5) Uiso 0.35 1 d PD M 3 O46B O 0.3005(8) 0.3274(8) 0.8203(6) 0.048(5) Uiso 0.25 1 d P N 2 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 0.01745(14) 0.01968(15) 0.02946(16) -0.00034(9) -0.00285(9) 0.00360(8) Fe1 0.0200(3) 0.0182(3) 0.0277(4) -0.0014(3) -0.0036(3) 0.0015(2) Fe2 0.0200(3) 0.0216(4) 0.0278(4) 0.0025(3) -0.0048(3) 0.0007(2) Fe3 0.0245(4) 0.0262(4) 0.0294(4) 0.0043(3) -0.0043(3) -0.0033(3) Fe4 0.0321(4) 0.0304(4) 0.0275(4) 0.0022(3) -0.0018(3) -0.0057(3) N1 0.023(2) 0.0209(19) 0.026(2) -0.0007(15) -0.0053(16) -0.0006(16) C1 0.022(2) 0.030(3) 0.030(3) 0.000(2) -0.0017(19) -0.008(2) C2 0.019(2) 0.031(3) 0.035(3) 0.000(2) -0.002(2) -0.0039(19) O1 0.0202(16) 0.0254(17) 0.0283(17) -0.0018(13) -0.0004(13) -0.0013(13) C3 0.025(2) 0.019(2) 0.030(2) -0.0035(18) -0.0024(19) -0.0010(18) C4 0.021(2) 0.019(2) 0.030(3) -0.0036(18) -0.0019(19) 0.0038(18) O2 0.0201(17) 0.0172(16) 0.0284(17) -0.0022(12) 0.0018(13) 0.0032(12) C5 0.033(3) 0.020(2) 0.032(3) 0.0027(19) -0.002(2) 0.002(2) C6 0.038(3) 0.026(3) 0.032(3) 0.004(2) -0.001(2) -0.005(2) O3 0.0273(19) 0.034(2) 0.0316(19) 0.0009(15) -0.0027(15) -0.0051(15) N2 0.030(2) 0.032(2) 0.043(3) 0.0002(19) -0.0053(19) 0.0101(19) C7 0.037(3) 0.022(3) 0.052(3) -0.004(2) -0.005(2) 0.016(2) C8 0.037(3) 0.027(3) 0.048(3) -0.013(2) -0.011(2) 0.015(2) O4 0.0260(18) 0.0236(17) 0.0362(19) -0.0088(14) -0.0061(14) 0.0063(14) C9 0.032(3) 0.026(3) 0.048(3) 0.000(2) -0.011(2) 0.010(2) C10 0.028(3) 0.023(2) 0.043(3) 0.004(2) -0.006(2) 0.007(2) O5 0.0208(17) 0.0173(16) 0.0374(19) 0.0018(14) -0.0044(13) 0.0016(12) C11 0.030(3) 0.043(3) 0.058(4) -0.011(3) 0.001(3) 0.016(3) C12 0.033(3) 0.048(4) 0.055(4) 0.000(3) 0.007(3) 0.020(3) O6 0.035(2) 0.052(2) 0.037(2) -0.0016(18) 0.0038(17) 0.0213(19) N3 0.027(2) 0.027(2) 0.028(2) -0.0008(17) -0.0066(16) -0.0013(16) C13 0.028(3) 0.020(2) 0.030(3) -0.0008(19) -0.0051(19) -0.0029(18) C14 0.027(2) 0.019(2) 0.030(3) -0.0027(18) -0.003(2) 0.0015(18) O7 0.0196(16) 0.0180(16) 0.0311(18) 0.0014(13) -0.0026(13) 0.0022(12) C15 0.028(3) 0.025(2) 0.030(3) -0.0031(19) -0.002(2) 0.003(2) C16 0.025(2) 0.025(2) 0.031(3) 0.0017(19) -0.002(2) 0.0057(19) O8 0.0198(16) 0.0222(16) 0.0262(17) 0.0020(13) -0.0027(13) 0.0006(12) C17 0.032(3) 0.031(3) 0.031(3) 0.002(2) -0.007(2) -0.003(2) C18 0.033(3) 0.037(3) 0.033(3) -0.004(2) -0.002(2) -0.006(2) O9 0.039(2) 0.033(2) 0.047(2) -0.0044(17) -0.0035(18) -0.0044(16) N4 0.033(2) 0.032(2) 0.038(3) 0.0087(19) -0.0088(19) -0.0069(19) C19 0.035(3) 0.041(3) 0.044(3) 0.018(3) -0.009(2) 0.003(2) C20 0.027(3) 0.038(3) 0.037(3) 0.012(2) -0.009(2) 0.000(2) O10 0.0178(16) 0.034(2) 0.0315(19) 0.0075(14) -0.0068(14) 0.0022(13) C21 0.042(3) 0.047(4) 0.038(3) 0.011(3) -0.018(2) -0.008(3) C22 0.035(3) 0.046(3) 0.035(3) 0.005(2) -0.013(2) -0.012(2) O11 0.032(2) 0.034(2) 0.033(2) 0.0020(15) -0.0088(15) -0.0049(16) C23 0.037(3) 0.033(3) 0.042(3) 0.012(2) -0.006(2) -0.003(2) C24 0.040(3) 0.027(3) 0.042(3) 0.008(2) -0.002(2) -0.001(2) O12 0.0286(19) 0.0268(18) 0.040(2) -0.0003(15) -0.0080(15) -0.0022(15) N5 0.036(3) 0.036(3) 0.038(3) 0.011(2) -0.001(2) -0.006(2) C25 0.038(3) 0.028(3) 0.047(3) 0.004(2) -0.003(2) -0.004(2) C26 0.021(2) 0.039(3) 0.034(3) -0.004(2) -0.002(2) -0.005(2) O13 0.0260(18) 0.0355(19) 0.0300(19) -0.0009(15) 0.0004(14) -0.0061(15) C27 0.038(3) 0.046(3) 0.043(3) 0.001(3) 0.011(3) -0.009(3) C28 0.034(3) 0.040(3) 0.037(3) -0.002(2) 0.007(2) -0.008(2) O14 0.031(2) 0.0297(19) 0.036(2) -0.0001(15) 0.0030(15) -0.0051(15) C29 0.057(4) 0.047(4) 0.056(4) 0.022(3) -0.007(3) -0.014(3) C30 0.057(4) 0.063(4) 0.040(4) 0.023(3) -0.010(3) -0.007(3) O15 0.054(3) 0.050(3) 0.030(2) 0.0103(18) -0.0060(18) -0.013(2) O16 0.0224(18) 0.041(2) 0.0316(19) 0.0006(15) -0.0019(15) -0.0035(15) O17 0.0228(17) 0.0268(17) 0.0328(19) 0.0016(14) -0.0015(14) 0.0001(14) C31 0.024(3) 0.027(3) 0.043(3) 0.005(2) -0.008(2) -0.001(2) C32 0.026(3) 0.090(5) 0.043(3) -0.001(3) -0.001(2) -0.019(3) O18 0.0356(19) 0.0184(16) 0.0304(19) -0.0010(13) -0.0066(15) 0.0013(14) C33 0.027(3) 0.025(3) 0.025(3) 0.000 0.001(3) 0.000 C34 0.076(6) 0.023(4) 0.036(4) 0.000 -0.020(4) 0.000 O19 0.0285(19) 0.033(2) 0.035(2) 0.0071(16) 0.0029(15) 0.0043(15) C35 0.035(4) 0.021(3) 0.023(3) 0.004(3) 0.000 0.000 C36 0.021(4) 0.040(4) 0.063(5) 0.027(4) 0.000 0.000 O41 0.039(3) 0.096(5) 0.126(5) 0.043(4) 0.007(3) 0.015(3) O42 0.109(8) 0.036(5) 0.014(3) 0.005(3) 0.000(4) 0.013(5) N51 0.159(8) 0.069(6) 0.112(7) 0.009(5) 0.013(8) -0.013(7) C51 0.146(9) 0.056(6) 0.084(7) 0.030(5) 0.005(8) -0.011(7) C52 0.126(8) 0.110(11) 0.255(18) 0.067(11) -0.069(12) -0.061(8) _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 O4 2.352(3) . ? Eu1 O5 2.359(3) . ? Eu1 O7 2.359(3) . ? Eu1 O19 2.360(4) . ? Eu1 O2 2.365(3) . ? Eu1 O16 2.445(3) . ? Eu1 O6 2.492(4) . ? Eu1 N2 2.672(4) . ? Fe1 O4 1.937(3) . ? Fe1 O2 1.957(3) . ? Fe1 O1 1.967(3) 3_656 ? Fe1 O1 2.037(3) . ? Fe1 O18 2.045(3) . ? Fe1 N1 2.242(4) . ? Fe2 O5 1.951(3) . ? Fe2 O10 1.972(3) . ? Fe2 O7 1.974(3) . ? Fe2 O8 2.000(3) . ? Fe2 O17 2.042(3) . ? Fe2 N3 2.249(4) . ? Fe3 O12 1.910(4) . ? Fe3 O8 2.003(3) . ? Fe3 O11 2.009(4) . ? Fe3 O13 2.013(4) . ? Fe3 O10 2.055(4) . ? Fe3 N4 2.278(5) . ? Fe4 O15 1.913(4) . ? Fe4 O14 1.970(4) 6 ? Fe4 O13 1.987(4) . ? Fe4 O14 2.049(4) . ? Fe4 O11 2.074(4) . ? Fe4 N5 2.288(5) . ? N1 C1 1.484(6) . ? N1 C5 1.489(6) . ? N1 C3 1.503(6) . ? C1 C2 1.521(7) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 O1 1.424(6) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? O1 Fe1 1.967(3) 3_656 ? C3 C4 1.536(7) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 O2 1.422(6) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.524(7) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 O3 1.420(6) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? O3 H3 0.8400 . ? N2 C7 1.478(7) . ? N2 C11 1.487(8) . ? N2 C9 1.493(7) . ? C7 C8 1.513(7) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 O4 1.426(6) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.498(8) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 O5 1.431(6) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.493(9) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 O6 1.446(6) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? O6 H6 0.85(4) . ? N3 C15 1.495(6) . ? N3 C17 1.496(6) . ? N3 C13 1.501(6) . ? C13 C14 1.532(6) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 O7 1.412(5) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.527(7) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 O8 1.418(5) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.498(7) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 O9 1.424(7) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? O9 H9 0.8400 . ? N4 C19 1.472(7) . ? N4 C23 1.475(7) . ? N4 C21 1.481(8) . ? C19 C20 1.525(7) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 O10 1.425(6) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.500(9) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 O11 1.419(6) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.523(8) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 O12 1.404(6) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? N5 C25 1.469(7) . ? N5 C27 1.475(8) . ? N5 C29 1.477(8) . ? C25 C26 1.515(8) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 O13 1.429(6) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.539(8) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 O14 1.414(6) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? O14 Fe4 1.970(4) 6 ? C29 C30 1.515(10) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 O15 1.412(7) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? O16 C31 1.254(6) . ? O17 C31 1.272(6) . ? C31 C32 1.513(7) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? O18 C33 1.266(5) . ? C33 O18 1.266(5) 3_656 ? C33 C34 1.497(10) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? O19 C35 1.266(5) . ? C35 O19 1.266(5) 8_456 ? C35 C36 1.486(10) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? N51 C51 1.182(11) . ? C51 C52 1.354(12) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? N52A C53A 1.243(18) . ? C53A C54A 1.339(18) . ? N52B C53B 1.259(19) . ? C53B C54B 1.349(19) . ? N53A C81A 1.298(14) . ? C81A C82A 1.267(15) . ? N31B O33B 1.280(15) . ? N31B O31B 1.281(15) . ? N31B O32B 1.282(15) . ? N31A O33A 1.247(12) . ? N31A O31A 1.257(11) . ? N31A O32A 1.311(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Eu1 O5 91.65(12) . . ? O4 Eu1 O7 135.13(11) . . ? O5 Eu1 O7 66.08(11) . . ? O4 Eu1 O19 115.13(13) . . ? O5 Eu1 O19 150.46(12) . . ? O7 Eu1 O19 85.40(12) . . ? O4 Eu1 O2 64.68(11) . . ? O5 Eu1 O2 95.15(11) . . ? O7 Eu1 O2 78.50(11) . . ? O19 Eu1 O2 86.08(11) . . ? O4 Eu1 O16 142.69(12) . . ? O5 Eu1 O16 80.94(11) . . ? O7 Eu1 O16 74.57(12) . . ? O19 Eu1 O16 84.28(12) . . ? O2 Eu1 O16 151.99(11) . . ? O4 Eu1 O6 80.32(14) . . ? O5 Eu1 O6 130.39(12) . . ? O7 Eu1 O6 143.95(13) . . ? O19 Eu1 O6 69.77(13) . . ? O2 Eu1 O6 123.43(12) . . ? O16 Eu1 O6 77.23(13) . . ? O4 Eu1 N2 67.02(13) . . ? O5 Eu1 N2 67.68(13) . . ? O7 Eu1 N2 128.21(12) . . ? O19 Eu1 N2 132.78(13) . . ? O2 Eu1 N2 127.87(13) . . ? O16 Eu1 N2 76.42(13) . . ? O6 Eu1 N2 64.13(14) . . ? O4 Fe1 O2 80.77(14) . . ? O4 Fe1 O1 100.30(14) . 3_656 ? O2 Fe1 O1 103.84(14) . 3_656 ? O4 Fe1 O1 174.86(15) . . ? O2 Fe1 O1 99.42(14) . . ? O1 Fe1 O1 74.64(15) 3_656 . ? O4 Fe1 O18 89.49(14) . . ? O2 Fe1 O18 160.81(14) . . ? O1 Fe1 O18 94.11(14) 3_656 . ? O1 Fe1 O18 91.76(14) . . ? O4 Fe1 N1 106.88(15) . . ? O2 Fe1 N1 80.18(14) . . ? O1 Fe1 N1 152.81(14) 3_656 . ? O1 Fe1 N1 78.17(14) . . ? O18 Fe1 N1 86.97(14) . . ? O5 Fe2 O10 102.38(14) . . ? O5 Fe2 O7 81.88(14) . . ? O10 Fe2 O7 171.36(14) . . ? O5 Fe2 O8 101.44(13) . . ? O10 Fe2 O8 75.28(13) . . ? O7 Fe2 O8 96.59(13) . . ? O5 Fe2 O17 93.99(13) . . ? O10 Fe2 O17 90.68(14) . . ? O7 Fe2 O17 96.56(14) . . ? O8 Fe2 O17 160.97(14) . . ? O5 Fe2 N3 161.41(15) . . ? O10 Fe2 N3 96.09(15) . . ? O7 Fe2 N3 79.53(14) . . ? O8 Fe2 N3 81.05(14) . . ? O17 Fe2 N3 87.89(14) . . ? O12 Fe3 O8 98.18(14) . . ? O12 Fe3 O11 142.15(16) . . ? O8 Fe3 O11 116.63(14) . . ? O12 Fe3 O13 94.75(15) . . ? O8 Fe3 O13 89.28(14) . . ? O11 Fe3 O13 72.54(14) . . ? O12 Fe3 O10 106.42(15) . . ? O8 Fe3 O10 73.40(13) . . ? O11 Fe3 O10 97.80(15) . . ? O13 Fe3 O10 154.14(14) . . ? O12 Fe3 N4 79.47(16) . . ? O8 Fe3 N4 147.86(16) . . ? O11 Fe3 N4 78.42(16) . . ? O13 Fe3 N4 122.83(16) . . ? O10 Fe3 N4 76.58(15) . . ? O15 Fe4 O14 102.49(17) . 6 ? O15 Fe4 O13 138.91(18) . . ? O14 Fe4 O13 115.76(15) 6 . ? O15 Fe4 O14 110.64(18) . . ? O14 Fe4 O14 71.94(16) 6 . ? O13 Fe4 O14 95.58(15) . . ? O15 Fe4 O11 93.97(17) . . ? O14 Fe4 O11 91.30(15) 6 . ? O13 Fe4 O11 71.68(14) . . ? O14 Fe4 O11 152.45(14) . . ? O15 Fe4 N5 78.68(17) . . ? O14 Fe4 N5 146.02(17) 6 . ? O13 Fe4 N5 77.78(16) . . ? O14 Fe4 N5 75.92(16) . . ? O11 Fe4 N5 122.65(17) . . ? C1 N1 C5 111.6(4) . . ? C1 N1 C3 112.8(4) . . ? C5 N1 C3 112.6(4) . . ? C1 N1 Fe1 103.8(3) . . ? C5 N1 Fe1 109.0(3) . . ? C3 N1 Fe1 106.4(3) . . ? N1 C1 C2 110.1(4) . . ? N1 C1 H1A 109.6 . . ? C2 C1 H1A 109.6 . . ? N1 C1 H1B 109.6 . . ? C2 C1 H1B 109.6 . . ? H1A C1 H1B 108.2 . . ? O1 C2 C1 109.1(4) . . ? O1 C2 H2A 109.9 . . ? C1 C2 H2A 109.9 . . ? O1 C2 H2B 109.9 . . ? C1 C2 H2B 109.9 . . ? H2A C2 H2B 108.3 . . ? C2 O1 Fe1 131.1(3) . 3_656 ? C2 O1 Fe1 118.9(3) . . ? Fe1 O1 Fe1 100.18(14) 3_656 . ? N1 C3 C4 109.6(4) . . ? N1 C3 H3A 109.7 . . ? C4 C3 H3A 109.7 . . ? N1 C3 H3B 109.7 . . ? C4 C3 H3B 109.7 . . ? H3A C3 H3B 108.2 . . ? O2 C4 C3 108.8(4) . . ? O2 C4 H4A 109.9 . . ? C3 C4 H4A 109.9 . . ? O2 C4 H4B 109.9 . . ? C3 C4 H4B 109.9 . . ? H4A C4 H4B 108.3 . . ? C4 O2 Fe1 109.7(3) . . ? C4 O2 Eu1 133.3(3) . . ? Fe1 O2 Eu1 106.57(13) . . ? N1 C5 C6 117.1(4) . . ? N1 C5 H5A 108.0 . . ? C6 C5 H5A 108.0 . . ? N1 C5 H5B 108.0 . . ? C6 C5 H5B 108.0 . . ? H5A C5 H5B 107.3 . . ? O3 C6 C5 114.5(4) . . ? O3 C6 H6A 108.6 . . ? C5 C6 H6A 108.6 . . ? O3 C6 H6B 108.6 . . ? C5 C6 H6B 108.6 . . ? H6A C6 H6B 107.6 . . ? C6 O3 H3 109.5 . . ? C7 N2 C11 111.9(4) . . ? C7 N2 C9 110.9(4) . . ? C11 N2 C9 109.8(4) . . ? C7 N2 Eu1 109.9(3) . . ? C11 N2 Eu1 107.5(3) . . ? C9 N2 Eu1 106.5(3) . . ? N2 C7 C8 113.7(4) . . ? N2 C7 H7A 108.8 . . ? C8 C7 H7A 108.8 . . ? N2 C7 H7B 108.8 . . ? C8 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? O4 C8 C7 108.7(4) . . ? O4 C8 H8A 110.0 . . ? C7 C8 H8A 110.0 . . ? O4 C8 H8B 110.0 . . ? C7 C8 H8B 110.0 . . ? H8A C8 H8B 108.3 . . ? C8 O4 Fe1 130.8(3) . . ? C8 O4 Eu1 120.6(3) . . ? Fe1 O4 Eu1 107.76(14) . . ? N2 C9 C10 111.1(4) . . ? N2 C9 H9A 109.4 . . ? C10 C9 H9A 109.4 . . ? N2 C9 H9B 109.4 . . ? C10 C9 H9B 109.4 . . ? H9A C9 H9B 108.0 . . ? O5 C10 C9 110.4(4) . . ? O5 C10 H10A 109.6 . . ? C9 C10 H10A 109.6 . . ? O5 C10 H10B 109.6 . . ? C9 C10 H10B 109.6 . . ? H10A C10 H10B 108.1 . . ? C10 O5 Fe2 123.9(3) . . ? C10 O5 Eu1 122.3(3) . . ? Fe2 O5 Eu1 103.72(14) . . ? N2 C11 C12 112.5(5) . . ? N2 C11 H11A 109.1 . . ? C12 C11 H11A 109.1 . . ? N2 C11 H11B 109.1 . . ? C12 C11 H11B 109.1 . . ? H11A C11 H11B 107.8 . . ? O6 C12 C11 108.1(5) . . ? O6 C12 H12A 110.1 . . ? C11 C12 H12A 110.1 . . ? O6 C12 H12B 110.1 . . ? C11 C12 H12B 110.1 . . ? H12A C12 H12B 108.4 . . ? C12 O6 Eu1 124.7(3) . . ? C12 O6 H6 105(5) . . ? Eu1 O6 H6 130(5) . . ? C15 N3 C17 112.7(4) . . ? C15 N3 C13 112.8(4) . . ? C17 N3 C13 110.1(4) . . ? C15 N3 Fe2 106.0(3) . . ? C17 N3 Fe2 111.5(3) . . ? C13 N3 Fe2 103.3(3) . . ? N3 C13 C14 109.7(4) . . ? N3 C13 H13A 109.7 . . ? C14 C13 H13A 109.7 . . ? N3 C13 H13B 109.7 . . ? C14 C13 H13B 109.7 . . ? H13A C13 H13B 108.2 . . ? O7 C14 C13 109.9(4) . . ? O7 C14 H14A 109.7 . . ? C13 C14 H14A 109.7 . . ? O7 C14 H14B 109.7 . . ? C13 C14 H14B 109.7 . . ? H14A C14 H14B 108.2 . . ? C14 O7 Fe2 120.0(3) . . ? C14 O7 Eu1 131.5(3) . . ? Fe2 O7 Eu1 102.98(13) . . ? N3 C15 C16 112.1(4) . . ? N3 C15 H15A 109.2 . . ? C16 C15 H15A 109.2 . . ? N3 C15 H15B 109.2 . . ? C16 C15 H15B 109.2 . . ? H15A C15 H15B 107.9 . . ? O8 C16 C15 110.2(4) . . ? O8 C16 H16A 109.6 . . ? C15 C16 H16A 109.6 . . ? O8 C16 H16B 109.6 . . ? C15 C16 H16B 109.6 . . ? H16A C16 H16B 108.1 . . ? C16 O8 Fe2 111.3(3) . . ? C16 O8 Fe3 122.1(3) . . ? Fe2 O8 Fe3 105.85(14) . . ? N3 C17 C18 117.7(4) . . ? N3 C17 H17A 107.9 . . ? C18 C17 H17A 107.9 . . ? N3 C17 H17B 107.9 . . ? C18 C17 H17B 107.9 . . ? H17A C17 H17B 107.2 . . ? O9 C18 C17 112.8(4) . . ? O9 C18 H18A 109.0 . . ? C17 C18 H18A 109.0 . . ? O9 C18 H18B 109.0 . . ? C17 C18 H18B 109.0 . . ? H18A C18 H18B 107.8 . . ? C18 O9 H9 109.5 . . ? C19 N4 C23 110.8(5) . . ? C19 N4 C21 112.4(4) . . ? C23 N4 C21 114.4(5) . . ? C19 N4 Fe3 108.2(3) . . ? C23 N4 Fe3 103.5(3) . . ? C21 N4 Fe3 106.9(3) . . ? N4 C19 C20 112.8(5) . . ? N4 C19 H19A 109.0 . . ? C20 C19 H19A 109.0 . . ? N4 C19 H19B 109.0 . . ? C20 C19 H19B 109.0 . . ? H19A C19 H19B 107.8 . . ? O10 C20 C19 107.1(4) . . ? O10 C20 H20A 110.3 . . ? C19 C20 H20A 110.3 . . ? O10 C20 H20B 110.3 . . ? C19 C20 H20B 110.3 . . ? H20A C20 H20B 108.5 . . ? C20 O10 Fe2 133.0(3) . . ? C20 O10 Fe3 121.5(3) . . ? Fe2 O10 Fe3 104.94(15) . . ? N4 C21 C22 110.4(4) . . ? N4 C21 H21A 109.6 . . ? C22 C21 H21A 109.6 . . ? N4 C21 H21B 109.6 . . ? C22 C21 H21B 109.6 . . ? H21A C21 H21B 108.1 . . ? O11 C22 C21 108.9(4) . . ? O11 C22 H22A 109.9 . . ? C21 C22 H22A 109.9 . . ? O11 C22 H22B 109.9 . . ? C21 C22 H22B 109.9 . . ? H22A C22 H22B 108.3 . . ? C22 O11 Fe3 115.8(3) . . ? C22 O11 Fe4 125.1(3) . . ? Fe3 O11 Fe4 105.70(16) . . ? N4 C23 C24 109.0(4) . . ? N4 C23 H23A 109.9 . . ? C24 C23 H23A 109.9 . . ? N4 C23 H23B 109.9 . . ? C24 C23 H23B 109.9 . . ? H23A C23 H23B 108.3 . . ? O12 C24 C23 110.0(4) . . ? O12 C24 H24A 109.7 . . ? C23 C24 H24A 109.7 . . ? O12 C24 H24B 109.7 . . ? C23 C24 H24B 109.7 . . ? H24A C24 H24B 108.2 . . ? C24 O12 Fe3 120.7(3) . . ? C25 N5 C27 113.9(5) . . ? C25 N5 C29 114.0(5) . . ? C27 N5 C29 111.0(5) . . ? C25 N5 Fe4 108.3(3) . . ? C27 N5 Fe4 106.3(3) . . ? C29 N5 Fe4 102.4(4) . . ? N5 C25 C26 109.8(4) . . ? N5 C25 H25A 109.7 . . ? C26 C25 H25A 109.7 . . ? N5 C25 H25B 109.7 . . ? C26 C25 H25B 109.7 . . ? H25A C25 H25B 108.2 . . ? O13 C26 C25 108.6(4) . . ? O13 C26 H26A 110.0 . . ? C25 C26 H26A 110.0 . . ? O13 C26 H26B 110.0 . . ? C25 C26 H26B 110.0 . . ? H26A C26 H26B 108.3 . . ? C26 O13 Fe4 114.3(3) . . ? C26 O13 Fe3 128.4(3) . . ? Fe4 O13 Fe3 108.91(16) . . ? N5 C27 C28 109.6(4) . . ? N5 C27 H27A 109.8 . . ? C28 C27 H27A 109.8 . . ? N5 C27 H27B 109.8 . . ? C28 C27 H27B 109.8 . . ? H27A C27 H27B 108.2 . . ? O14 C28 C27 108.2(5) . . ? O14 C28 H28A 110.1 . . ? C27 C28 H28A 110.1 . . ? O14 C28 H28B 110.1 . . ? C27 C28 H28B 110.1 . . ? H28A C28 H28B 108.4 . . ? C28 O14 Fe4 127.3(3) . 6 ? C28 O14 Fe4 122.0(3) . . ? Fe4 O14 Fe4 107.88(16) 6 . ? N5 C29 C30 110.1(5) . . ? N5 C29 H29A 109.6 . . ? C30 C29 H29A 109.6 . . ? N5 C29 H29B 109.6 . . ? C30 C29 H29B 109.6 . . ? H29A C29 H29B 108.1 . . ? O15 C30 C29 110.0(5) . . ? O15 C30 H30A 109.7 . . ? C29 C30 H30A 109.7 . . ? O15 C30 H30B 109.7 . . ? C29 C30 H30B 109.7 . . ? H30A C30 H30B 108.2 . . ? C30 O15 Fe4 121.9(4) . . ? C31 O16 Eu1 135.0(3) . . ? C31 O17 Fe2 126.7(3) . . ? O16 C31 O17 125.7(5) . . ? O16 C31 C32 118.7(5) . . ? O17 C31 C32 115.5(5) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C33 O18 Fe1 128.8(4) . . ? O18 C33 O18 125.5(6) 3_656 . ? O18 C33 C34 117.3(3) 3_656 . ? O18 C33 C34 117.3(3) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C35 O19 Eu1 150.0(4) . . ? O19 C35 O19 122.2(7) . 8_456 ? O19 C35 C36 118.9(3) . . ? O19 C35 C36 118.9(3) 8_456 . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N51 C51 C52 177.4(17) . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? N52A C53A C54A 162(5) . . ? N52B C53B C54B 150(4) . . ? C82A C81A N53A 164(2) . . ? O33B N31B O31B 119.7(17) . . ? O33B N31B O32B 117.0(16) . . ? O31B N31B O32B 120.7(17) . . ? O33A N31A O31A 127.9(11) . . ? O33A N31A O32A 116.5(10) . . ? O31A N31A O32A 115.6(10) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3 O12 0.84 1.81 2.646(5) 178.8 . O6 H6 O31A 0.85(4) 1.99(5) 2.721(14) 143(6) . O6 H6 O31C 0.85(4) 1.78(4) 2.617(18) 168(7) . O6 H6 O46B 0.85(4) 1.80(4) 2.635(19) 167(7) . O9 H9 O41 0.84 1.92 2.755(7) 172.3 . _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.581 _refine_diff_density_min -0.746 _refine_diff_density_rms 0.129